# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_s6098r
_database_code_depnum_ccdc_archive 'CCDC 2202018'
loop_
_audit_author_name
_audit_author_address
'Inigo Vitorica-yrezabal'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2022-07-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H75 As11 Ge5'
_chemical_formula_sum            'C30 H75 As11 Ge5'
_chemical_formula_weight         1622.97
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6695(3)
_cell_length_b                   14.0092(6)
_cell_length_c                   24.6674(7)
_cell_angle_alpha                85.802(3)
_cell_angle_beta                 84.724(3)
_cell_angle_gamma                82.011(3)
_cell_volume                     2608.60(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7278
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.9940
_cell_measurement_theta_min      1.7920
_shelx_estimated_absorpt_T_max   0.468
_shelx_estimated_absorpt_T_min   0.347
_exptl_absorpt_coefficient_mu    11.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.363
_diffrn_reflns_theta_min         1.802
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  45.00   1.00    3.00    --  -44.41  76.00 150.00   26
  2  ω    -73.00 -33.00   1.00    3.00    --  -44.41  76.00 150.00   40
  3  ω    -56.00  19.00   1.00    3.00    --  -44.41  57.00 -60.00   75
  4  ω    -78.00 -15.00   1.00    3.00    --  -46.39  57.00 120.00   63
  5  ω    -76.00  15.00   1.00    3.00    --  -46.39  76.00 -30.00   91
  6  ω   -131.00 -12.00   1.00    3.00    --  -46.39 -38.00 150.00  119
  7  ω    -56.00 -25.00   1.00   10.00    -- -107.20  76.00 -30.00   31
  8  ω   -195.00 -69.00   1.00   10.00    -- -107.20 -38.00   0.00  126
  9  ω   -145.00 -43.00   1.00   10.00    -- -107.20  76.00 -60.00  102
 10  ω   -192.00-114.00   1.00   10.00    -- -107.20 -38.00  30.00   78
 11  ω   -189.00 -72.00   1.00   10.00    -- -107.20 -38.00 -90.00  117
 12  ω   -123.00 -96.00   1.00   10.00    -- -107.20  76.00  60.00   27
 13  ω   -120.00 -62.00   1.00   10.00    -- -107.20  76.00 -30.00   58
 14  ω   -135.00 -85.00   1.00   10.00    -- -107.20  76.00 120.00   50
 15  ω   -122.00 -20.00   1.00   10.00    -- -107.20  76.00-120.00  102
 16  ω   -119.00 -85.00   1.00   10.00    -- -107.20  76.00-180.00   34
 17  ω   -116.00 -90.00   1.00   10.00    -- -107.20  57.00 150.00   26
 18  ω    -87.00 -18.00   1.00   10.00    -- -107.20  57.00 150.00   69
 19  ω   -131.00-102.00   1.00   10.00    -- -107.20  76.00 -90.00   29
 20  ω    -74.00 -47.00   1.00   10.00    -- -107.20  76.00 -90.00   27
 21  ω   -197.00-142.00   1.00   10.00    -- -107.20 -57.00  90.00   55
 22  ω   -105.00 -65.00   1.00   10.00    -- -107.20  76.00  30.00   40
 23  ω   -142.00 -26.00   1.00   10.00    -- -107.20  76.00  90.00  116
 24  ω   -188.00-104.00   1.00   10.00    -- -107.20 -38.00 -60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0700180000
_diffrn_orient_matrix_UB_12      0.0610634000
_diffrn_orient_matrix_UB_13      -0.0498615000
_diffrn_orient_matrix_UB_21      -0.0307975000
_diffrn_orient_matrix_UB_22      -0.0925952000
_diffrn_orient_matrix_UB_23      -0.0257043000
_diffrn_orient_matrix_UB_31      -0.1886219000
_diffrn_orient_matrix_UB_32      0.0084179000
_diffrn_orient_matrix_UB_33      0.0282994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7389
_reflns_number_total             10433
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10433
_refine_ls_number_restraints     203
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0853P)²+4.8257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1672
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C33
 1.5 with sigma of 0.02
 C33-C15
 1.5 with sigma of 0.02
 Ge2-C8 \\sim Ge2-C8A
 with sigma of 0.02
 C8-C38 \\sim C8A-C38A
 with sigma of 0.02
 Ge2-C38 \\sim Ge2-C38A
 with sigma of 0.04
 Ge4-C35 \\sim Ge4-C35A
 with sigma of 0.02
 C35-C43 \\sim C35A-C43A
 with sigma of 0.02
 Ge5-C45 \\sim Ge5-C45A
 with sigma of 0.02
 Ge4-C43 \\sim Ge4-C43A
 with sigma of 0.04
 Ge1-C19 \\sim Ge1-C19A
 with sigma of 0.02
 C19-C42 \\sim C19A-C42A
 with sigma of 0.02
 C24-C45 \\sim C24A-C45A
 with sigma of 0.02
 Ge1-C42 \\sim Ge1-C42A
 with sigma of 0.04
 Ge5-C24 \\sim Ge5-C24A
 with sigma of 0.04
 Ge5-C15 \\sim Ge5-C15A
 with sigma of 0.02
 C15-C33 \\sim C15A-C33A
 with sigma of 0.02
 Ge5-C33 \\sim Ge5-C33A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C45A \\sim C45 \\sim C24 \\sim C24A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C15A \\sim C15 \\sim C33A \\sim C33: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C43 \\sim C35 \\sim C35A \\sim C43A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C19A \\sim C19 \\sim C42A \\sim C42: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C8A \\sim C8: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C8) = Uanis(C8A)
4. Rigid body (RIGU) restrains
 C19A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24A, C45A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15A, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(2)
 Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(3)
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(4)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(4)
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(5)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C45)=Sof(H45A)=Sof(H45B)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C13(H13A,H13B), C15(H15A,H15B),
 C18(H18A,H18B), C19(H19A,H19B), C35(H35A,H35B), C45(H45A,H45B), C8A(H8AA,H8AB),
  C35A(H35C,H35D), C19A(H19C,H19D), C15A(H15C,H15D), C45A(H45C,H45D)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C38A(H38D,H38E,H38F), C43A(H43D,H43E,H43F), C42A(H42D,H42E,H42F),
 C33A(H33D,H33E,H33F), C24A(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 1.07412(12) 0.36026(7) 0.26812(4) 0.0492(2) Uani 1 1 d . . . . .
As2 As 0.82463(12) 0.21004(7) 0.19540(4) 0.0493(2) Uani 1 1 d . . . . .
As3 As 0.49243(12) 0.20403(7) 0.32135(4) 0.0504(2) Uani 1 1 d . . . . .
As4 As 0.52052(12) 0.27657(7) 0.22844(4) 0.0498(2) Uani 1 1 d . . . . .
As5 As 0.80148(12) 0.20293(7) 0.33856(4) 0.0495(2) Uani 1 1 d . . . . .
As6 As 0.80030(12) 0.37957(7) 0.32661(4) 0.0497(2) Uani 1 1 d . . . . .
As7 As 0.57002(12) 0.42655(7) 0.26300(4) 0.0493(2) Uani 1 1 d . . . . .
As8 As 0.72918(13) 0.47576(7) 0.17892(4) 0.0536(2) Uani 1 1 d . . . . .
As9 As 0.98216(13) 0.34941(7) 0.17781(4) 0.0523(2) Uani 1 1 d . . . . .
As10 As 1.13647(13) 0.52381(7) 0.24345(4) 0.0531(2) Uani 1 1 d . . . . .
As11 As 0.84861(14) 0.60582(7) 0.21640(4) 0.0558(2) Uani 1 1 d . . . . .
Ge1 Ge 0.48371(16) 0.04151(8) 0.29148(5) 0.0628(3) Uani 1 1 d D . . . .
Ge2 Ge 0.96400(16) 0.67086(9) 0.12890(4) 0.0620(3) Uani 1 1 d D . . . .
Ge3 Ge 0.73615(15) 0.20208(9) 0.43745(4) 0.0632(3) Uani 1 1 d . . . . .
Ge4 Ge 0.76237(18) 0.20275(9) 0.10073(4) 0.0666(3) Uani 1 1 d D . . . .
Ge5 Ge 1.11710(18) 0.58613(10) 0.33473(5) 0.0704(3) Uani 1 1 d D . . . .
C1 C 0.4034(14) -0.0405(8) 0.3544(4) 0.066(3) Uani 1 1 d . . . . .
H1A H 0.398195 -0.105821 0.342300 0.079 Uiso 1 1 calc R U . . .
H1B H 0.491375 -0.046872 0.381872 0.079 Uiso 1 1 calc R U . . .
C2 C 0.6378(16) 0.0815(10) 0.4609(4) 0.084(4) Uani 1 1 d . . . . .
H2A H 0.610484 0.079249 0.500994 0.101 Uiso 1 1 calc R U . . .
H2B H 0.525648 0.081892 0.443967 0.101 Uiso 1 1 calc R U . . .
C3 C 0.5737(15) 0.3126(9) 0.4617(4) 0.076(3) Uani 1 1 d . . . . .
H3A H 0.633713 0.371153 0.455693 0.091 Uiso 1 1 calc R U . . .
H3B H 0.471221 0.322141 0.439303 0.091 Uiso 1 1 calc R U . . .
C4 C 0.9594(18) 0.1966(12) 0.4712(5) 0.097(4) Uani 1 1 d . . . . .
H4A H 0.932019 0.203056 0.510906 0.117 Uiso 1 1 calc R U . . .
H4B H 1.027590 0.131938 0.466357 0.117 Uiso 1 1 calc R U . . .
C5 C 1.2142(19) 0.4883(11) 0.3874(4) 0.093(4) Uani 1 1 d . . . . .
H5A H 1.151036 0.431310 0.387016 0.112 Uiso 1 1 calc R U . . .
H5B H 1.339498 0.467889 0.375105 0.112 Uiso 1 1 calc R U . . .
C6 C 1.0971(19) 0.7758(9) 0.1446(5) 0.084(3) Uani 1 1 d . . . . .
H6A H 1.026813 0.816080 0.172313 0.101 Uiso 1 1 calc R U . . .
H6B H 1.208953 0.747293 0.159901 0.101 Uiso 1 1 calc R U . . .
C7 C 0.7513(16) 0.7259(10) 0.0894(5) 0.087(4) Uani 1 1 d . . . . .
H7A H 0.790959 0.757371 0.054062 0.104 Uiso 1 1 calc R U . . .
H7B H 0.686753 0.672596 0.081708 0.104 Uiso 1 1 calc R U . . .
C8 C 1.109(5) 0.587(2) 0.0803(11) 0.076(5) Uani 0.56(2) 1 d D U P A 1
H8A H 1.058507 0.525396 0.081243 0.092 Uiso 0.56(2) 1 calc R U P A 1
H8B H 1.104483 0.616666 0.042722 0.092 Uiso 0.56(2) 1 calc R U P A 1
C9 C 0.7597(17) -0.0072(9) 0.4463(6) 0.090(4) Uani 1 1 d . . . . .
H9A H 0.703765 -0.064514 0.458950 0.136 Uiso 1 1 calc R U . . .
H9B H 0.785135 -0.006332 0.406589 0.136 Uiso 1 1 calc R U . . .
H9C H 0.870030 -0.008977 0.463656 0.136 Uiso 1 1 calc R U . . .
C10 C 0.677(2) 0.0788(11) 0.0973(5) 0.096(4) Uani 1 1 d . . . . .
H10A H 0.752164 0.028875 0.118433 0.116 Uiso 1 1 calc R U . . .
H10B H 0.555295 0.082797 0.114647 0.116 Uiso 1 1 calc R U . . .
C11 C 0.2257(17) -0.0024(11) 0.3809(5) 0.095(4) Uani 1 1 d . . . . .
H11A H 0.193783 -0.046439 0.411806 0.142 Uiso 1 1 calc R U . . .
H11B H 0.230300 0.061593 0.393913 0.142 Uiso 1 1 calc R U . . .
H11C H 0.137026 0.002585 0.354302 0.142 Uiso 1 1 calc R U . . .
C12 C 1.0684(18) 0.2671(13) 0.4510(6) 0.107(5) Uani 1 1 d . . . . .
H12A H 1.175864 0.258134 0.470432 0.160 Uiso 1 1 calc R U . . .
H12B H 1.100218 0.260334 0.411950 0.160 Uiso 1 1 calc R U . . .
H12C H 1.004378 0.331653 0.456625 0.160 Uiso 1 1 calc R U . . .
C13 C 0.301(2) 0.0619(9) 0.2404(5) 0.101(5) Uani 1 1 d . . . . .
H13A H 0.191260 0.094906 0.258895 0.121 Uiso 1 1 calc R U . . .
H13B H 0.338475 0.105524 0.209419 0.121 Uiso 1 1 calc R U . . .
C14 C 1.1380(18) 0.8387(9) 0.0940(5) 0.084(3) Uani 1 1 d . . . . .
H14A H 1.203701 0.889638 0.103255 0.126 Uiso 1 1 calc R U . . .
H14B H 1.209490 0.799243 0.066738 0.126 Uiso 1 1 calc R U . . .
H14C H 1.027459 0.867990 0.079142 0.126 Uiso 1 1 calc R U . . .
C15 C 0.898(3) 0.657(2) 0.3583(15) 0.110(10) Uani 0.50(3) 1 d D U P B 1
H15A H 0.839181 0.685411 0.325697 0.132 Uiso 0.50(3) 1 calc R U P B 1
H15B H 0.822745 0.611696 0.377837 0.132 Uiso 0.50(3) 1 calc R U P B 1
C16 C 0.5079(17) 0.3013(12) 0.5213(5) 0.099(4) Uani 1 1 d . . . . .
H16A H 0.426765 0.358854 0.531347 0.148 Uiso 1 1 calc R U . . .
H16B H 0.445934 0.244303 0.527396 0.148 Uiso 1 1 calc R U . . .
H16C H 0.608487 0.293333 0.543792 0.148 Uiso 1 1 calc R U . . .
C17 C 1.206(2) 0.5162(13) 0.4448(5) 0.114(5) Uani 1 1 d . . . . .
H17A H 1.258260 0.461473 0.467641 0.171 Uiso 1 1 calc R U . . .
H17B H 1.271273 0.571100 0.446262 0.171 Uiso 1 1 calc R U . . .
H17C H 1.082175 0.534397 0.458213 0.171 Uiso 1 1 calc R U . . .
C18 C 0.986(3) 0.2015(13) 0.0577(5) 0.120(7) Uani 1 1 d . . . . .
H18A H 0.969114 0.190524 0.019461 0.144 Uiso 1 1 calc R U . . .
H18B H 1.026117 0.265771 0.057945 0.144 Uiso 1 1 calc R U . . .
C19 C 0.684(3) -0.0264(16) 0.2480(7) 0.067(6) Uani 0.58(2) 1 d D U P C 1
H19A H 0.650174 -0.087233 0.236698 0.081 Uiso 0.58(2) 1 calc R U P C 1
H19B H 0.711686 0.014184 0.214622 0.081 Uiso 0.58(2) 1 calc R U P C 1
C20 C 0.679(2) 0.0480(12) 0.0394(5) 0.114(6) Uani 1 1 d . . . . .
H20A H 0.635411 -0.014582 0.040279 0.172 Uiso 1 1 calc R U . . .
H20B H 0.603385 0.096321 0.018399 0.172 Uiso 1 1 calc R U . . .
H20C H 0.800384 0.042364 0.022189 0.172 Uiso 1 1 calc R U . . .
C21 C 0.632(2) 0.7957(12) 0.1202(6) 0.113(5) Uani 1 1 d . . . . .
H21A H 0.530841 0.820208 0.099172 0.170 Uiso 1 1 calc R U . . .
H21B H 0.589869 0.764707 0.154926 0.170 Uiso 1 1 calc R U . . .
H21C H 0.694111 0.849511 0.127270 0.170 Uiso 1 1 calc R U . . .
C22 C 1.128(3) 0.1266(17) 0.0772(8) 0.142(7) Uani 1 1 d . . . . .
H22A H 1.237315 0.130225 0.053572 0.213 Uiso 1 1 calc R U . . .
H22B H 1.148778 0.137828 0.114698 0.213 Uiso 1 1 calc R U . . .
H22C H 1.091701 0.062485 0.076164 0.213 Uiso 1 1 calc R U . . .
C23 C 0.259(3) -0.0308(12) 0.2179(7) 0.130(6) Uani 1 1 d . . . . .
H23A H 0.166499 -0.014685 0.192693 0.195 Uiso 1 1 calc R U . . .
H23B H 0.365945 -0.063234 0.198610 0.195 Uiso 1 1 calc R U . . .
H23C H 0.218501 -0.073868 0.248163 0.195 Uiso 1 1 calc R U . . .
C24 C 1.383(3) 0.7010(17) 0.2914(13) 0.143(10) Uani 0.75(2) 1 d D U P B 1
H24A H 1.429138 0.763328 0.287165 0.214 Uiso 0.75(2) 1 calc R U P B 1
H24B H 1.468309 0.652816 0.309243 0.214 Uiso 0.75(2) 1 calc R U P B 1
H24C H 1.365456 0.680339 0.255504 0.214 Uiso 0.75(2) 1 calc R U P B 1
C33 C 0.909(6) 0.737(2) 0.3949(14) 0.134(13) Uani 0.50(3) 1 d D U P B 1
H33A H 0.790397 0.769455 0.404928 0.202 Uiso 0.50(3) 1 calc R U P B 1
H33B H 0.964422 0.709980 0.428013 0.202 Uiso 0.50(3) 1 calc R U P B 1
H33C H 0.980899 0.783878 0.375745 0.202 Uiso 0.50(3) 1 calc R U P B 1
C35 C 0.570(4) 0.306(2) 0.0838(12) 0.121(10) Uani 0.54(3) 1 d D U P D 1
H35A H 0.565253 0.344464 0.116042 0.145 Uiso 0.54(3) 1 calc R U P D 1
H35B H 0.630921 0.343284 0.054196 0.145 Uiso 0.54(3) 1 calc R U P D 1
C38 C 1.308(3) 0.563(2) 0.0926(10) 0.115(10) Uani 0.56(2) 1 d D . P A 1
H38A H 1.371202 0.519458 0.065683 0.173 Uiso 0.56(2) 1 calc R U P A 1
H38B H 1.361699 0.622526 0.090621 0.173 Uiso 0.56(2) 1 calc R U P A 1
H38C H 1.315604 0.531020 0.129241 0.173 Uiso 0.56(2) 1 calc R U P A 1
C42 C 0.839(3) -0.0481(19) 0.2781(10) 0.093(7) Uani 0.58(2) 1 d D U P C 1
H42A H 0.935549 -0.081924 0.255169 0.139 Uiso 0.58(2) 1 calc R U P C 1
H42B H 0.873682 0.012060 0.288807 0.139 Uiso 0.58(2) 1 calc R U P C 1
H42C H 0.812199 -0.089309 0.310873 0.139 Uiso 0.58(2) 1 calc R U P C 1
C43 C 0.434(4) 0.324(3) 0.0731(12) 0.151(13) Uani 0.54(3) 1 d D U P D 1
H43A H 0.403800 0.394123 0.069265 0.226 Uiso 0.54(3) 1 calc R U P D 1
H43B H 0.421246 0.296090 0.038542 0.226 Uiso 0.54(3) 1 calc R U P D 1
H43C H 0.353989 0.297298 0.101885 0.226 Uiso 0.54(3) 1 calc R U P D 1
C45 C 1.226(2) 0.7103(12) 0.3227(9) 0.093(5) Uani 0.75(2) 1 d D U P B 1
H45A H 1.142482 0.760334 0.304846 0.111 Uiso 0.75(2) 1 calc R U P B 1
H45B H 1.245247 0.732835 0.358539 0.111 Uiso 0.75(2) 1 calc R U P B 1
C38A C 1.028(4) 0.528(2) 0.0450(9) 0.084(9) Uani 0.44(2) 1 d D . P A 2
H38D H 1.112744 0.478359 0.027935 0.127 Uiso 0.44(2) 1 calc R U P A 2
H38E H 0.922869 0.500182 0.060633 0.127 Uiso 0.44(2) 1 calc R U P A 2
H38F H 0.993114 0.579953 0.017456 0.127 Uiso 0.44(2) 1 calc R U P A 2
C8A C 1.114(7) 0.571(3) 0.0913(14) 0.076(5) Uani 0.44(2) 1 d D U P A 2
H8AA H 1.221883 0.597829 0.075085 0.092 Uiso 0.44(2) 1 calc R U P A 2
H8AB H 1.151767 0.518205 0.118183 0.092 Uiso 0.44(2) 1 calc R U P A 2
C35A C 0.623(5) 0.309(2) 0.0587(12) 0.113(10) Uani 0.46(3) 1 d D U P D 2
H35C H 0.563218 0.351243 0.087122 0.135 Uiso 0.46(3) 1 calc R U P D 2
H35D H 0.714573 0.345486 0.039324 0.135 Uiso 0.46(3) 1 calc R U P D 2
C43A C 0.521(5) 0.311(3) 0.0279(11) 0.124(12) Uani 0.46(3) 1 d D U P D 2
H43D H 0.481739 0.378063 0.015950 0.185 Uiso 0.46(3) 1 calc R U P D 2
H43E H 0.573421 0.275205 -0.003600 0.185 Uiso 0.46(3) 1 calc R U P D 2
H43F H 0.419624 0.281055 0.044970 0.185 Uiso 0.46(3) 1 calc R U P D 2
C19A C 0.727(3) -0.018(2) 0.2708(18) 0.096(12) Uani 0.42(2) 1 d D U P C 2
H19C H 0.767412 0.017189 0.236602 0.116 Uiso 0.42(2) 1 calc R U P C 2
H19D H 0.801107 -0.003615 0.299251 0.116 Uiso 0.42(2) 1 calc R U P C 2
C42A C 0.766(4) -0.1187(18) 0.2627(18) 0.103(11) Uani 0.42(2) 1 d D U P C 2
H42D H 0.892594 -0.135006 0.252682 0.154 Uiso 0.42(2) 1 calc R U P C 2
H42E H 0.732834 -0.155662 0.296469 0.154 Uiso 0.42(2) 1 calc R U P C 2
H42F H 0.698909 -0.134716 0.233393 0.154 Uiso 0.42(2) 1 calc R U P C 2
C15A C 0.877(3) 0.6214(15) 0.3620(13) 0.079(7) Uani 0.50(3) 1 d D U P B 2
H15C H 0.802721 0.583995 0.343345 0.094 Uiso 0.50(3) 1 calc R U P B 2
H15D H 0.866559 0.600099 0.401229 0.094 Uiso 0.50(3) 1 calc R U P B 2
C33A C 0.799(4) 0.7264(15) 0.3568(13) 0.097(10) Uani 0.50(3) 1 d D U P B 2
H33D H 0.675805 0.733605 0.372422 0.145 Uiso 0.50(3) 1 calc R U P B 2
H33E H 0.866866 0.764993 0.376324 0.145 Uiso 0.50(3) 1 calc R U P B 2
H33F H 0.802711 0.748809 0.318152 0.145 Uiso 0.50(3) 1 calc R U P B 2
C45A C 1.343(3) 0.653(2) 0.3262(11) 0.049(9) Uani 0.25(2) 1 d D U P B 2
H45C H 1.338519 0.698767 0.293664 0.059 Uiso 0.25(2) 1 calc R U P B 2
H45D H 1.345692 0.690772 0.358459 0.059 Uiso 0.25(2) 1 calc R U P B 2
C24A C 1.493(5) 0.590(4) 0.321(4) 0.16(2) Uani 0.25(2) 1 d D U P B 2
H24D H 1.595363 0.625662 0.317171 0.235 Uiso 0.25(2) 1 calc R U P B 2
H24E H 1.499959 0.545498 0.353524 0.235 Uiso 0.25(2) 1 calc R U P B 2
H24F H 1.492782 0.553497 0.288696 0.235 Uiso 0.25(2) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 As6 2.4304(13) . ?
As1 As9 2.4190(12) . ?
As1 As10 2.4281(13) . ?
As2 As4 2.4759(14) . ?
As2 As9 2.4280(13) . ?
As2 Ge4 2.4383(13) . ?
As3 As4 2.4414(13) . ?
As3 As5 2.4439(12) . ?
As3 Ge1 2.4551(15) . ?
As4 As7 2.4143(14) . ?
As5 As6 2.4695(14) . ?
As5 Ge3 2.4441(14) . ?
As6 As7 2.4595(12) . ?
As7 As8 2.4137(13) . ?
As8 As9 2.4374(15) . ?
As8 As11 2.4248(14) . ?
As10 As11 2.4685(14) . ?
As10 Ge5 2.4584(15) . ?
As11 Ge2 2.4202(15) . ?
Ge1 C1 1.967(9) . ?
Ge1 C13 1.949(13) . ?
Ge1 C19 1.962(16) . ?
Ge1 C19A 1.97(2) . ?
Ge2 C6 1.982(11) . ?
Ge2 C7 2.009(11) . ?
Ge2 C8 1.915(17) . ?
Ge2 C8A 1.919(19) . ?
Ge3 C2 1.972(12) . ?
Ge3 C3 1.942(12) . ?
Ge3 C4 1.962(11) . ?
Ge4 C10 1.947(12) . ?
Ge4 C18 1.934(17) . ?
Ge4 C35 1.97(2) . ?
Ge4 C35A 1.99(2) . ?
Ge5 C5 1.938(13) . ?
Ge5 C15 1.89(2) . ?
Ge5 C45 2.025(16) . ?
Ge5 C15A 1.91(2) . ?
Ge5 C45A 2.07(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C11 1.502(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C9 1.493(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C16 1.515(16) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C12 1.415(19) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C17 1.490(17) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C14 1.508(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C21 1.45(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C38 1.57(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C20 1.520(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C23 1.533(17) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C33 1.507(13) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C22 1.49(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C42 1.44(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 C45 1.36(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C43 1.09(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
C38A C8A 1.57(5) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C35A C43A 1.14(3) . ?
C43A H43D 0.9800 . ?
C43A H43E 0.9800 . ?
C43A H43F 0.9800 . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C19A C42A 1.43(3) . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C15A C33A 1.51(2) . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
C45A H45C 0.9900 . ?
C45A H45D 0.9900 . ?
C45A C24A 1.35(3) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
As9 As1 As6 104.58(4) . . ?
As9 As1 As10 89.90(4) . . ?
As10 As1 As6 104.75(5) . . ?
As9 As2 As4 105.02(5) . . ?
As9 As2 Ge4 94.66(5) . . ?
Ge4 As2 As4 95.84(5) . . ?
As4 As3 As5 95.78(4) . . ?
As4 As3 Ge1 93.74(5) . . ?
As5 As3 Ge1 103.68(5) . . ?
As3 As4 As2 102.54(4) . . ?
As7 As4 As2 101.24(4) . . ?
As7 As4 As3 90.27(4) . . ?
As3 As5 As6 96.12(5) . . ?
As3 As5 Ge3 93.40(5) . . ?
Ge3 As5 As6 94.40(5) . . ?
As1 As6 As5 91.41(5) . . ?
As1 As6 As7 104.26(4) . . ?
As7 As6 As5 101.88(4) . . ?
As4 As7 As6 104.63(5) . . ?
As8 As7 As4 92.79(5) . . ?
As8 As7 As6 104.40(5) . . ?
As7 As8 As9 99.63(5) . . ?
As7 As8 As11 95.42(5) . . ?
As11 As8 As9 101.40(5) . . ?
As1 As9 As2 99.13(4) . . ?
As1 As9 As8 99.89(5) . . ?
As2 As9 As8 98.74(5) . . ?
As1 As10 As11 102.40(5) . . ?
As1 As10 Ge5 99.80(5) . . ?
Ge5 As10 As11 97.24(6) . . ?
As8 As11 As10 101.70(5) . . ?
Ge2 As11 As8 94.72(5) . . ?
Ge2 As11 As10 95.31(5) . . ?
C1 Ge1 As3 108.8(3) . . ?
C1 Ge1 C19A 104.5(13) . . ?
C13 Ge1 As3 103.4(4) . . ?
C13 Ge1 C1 108.4(5) . . ?
C13 Ge1 C19 102.1(8) . . ?
C13 Ge1 C19A 122.4(14) . . ?
C19 Ge1 As3 121.4(8) . . ?
C19 Ge1 C1 111.6(7) . . ?
C19A Ge1 As3 108.8(9) . . ?
C6 Ge2 As11 106.2(3) . . ?
C6 Ge2 C7 110.0(6) . . ?
C7 Ge2 As11 105.6(4) . . ?
C8 Ge2 As11 119.5(10) . . ?
C8 Ge2 C6 109.0(15) . . ?
C8 Ge2 C7 106.3(12) . . ?
C8A Ge2 As11 109.9(14) . . ?
C8A Ge2 C6 111.3(19) . . ?
C8A Ge2 C7 113.4(15) . . ?
C2 Ge3 As5 107.3(3) . . ?
C3 Ge3 As5 114.0(3) . . ?
C3 Ge3 C2 110.1(5) . . ?
C3 Ge3 C4 109.7(6) . . ?
C4 Ge3 As5 108.3(4) . . ?
C4 Ge3 C2 107.2(6) . . ?
C10 Ge4 As2 105.3(4) . . ?
C10 Ge4 C35 108.3(12) . . ?
C10 Ge4 C35A 112.6(11) . . ?
C18 Ge4 As2 106.3(4) . . ?
C18 Ge4 C10 109.0(7) . . ?
C18 Ge4 C35 118.3(14) . . ?
C18 Ge4 C35A 98.5(13) . . ?
C35 Ge4 As2 108.8(7) . . ?
C35A Ge4 As2 124.1(9) . . ?
C5 Ge5 As10 111.3(4) . . ?
C5 Ge5 C45 118.2(8) . . ?
C5 Ge5 C45A 92.8(9) . . ?
C15 Ge5 As10 116.1(10) . . ?
C15 Ge5 C5 115.2(14) . . ?
C15 Ge5 C45 89.9(12) . . ?
C45 Ge5 As10 104.4(6) . . ?
C15A Ge5 As10 111.5(9) . . ?
C15A Ge5 C5 105.1(10) . . ?
C15A Ge5 C45A 135.2(11) . . ?
C45A Ge5 As10 98.8(8) . . ?
Ge1 C1 H1A 108.8 . . ?
Ge1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C11 C1 Ge1 113.7(8) . . ?
C11 C1 H1A 108.8 . . ?
C11 C1 H1B 108.8 . . ?
Ge3 C2 H2A 108.9 . . ?
Ge3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C9 C2 Ge3 113.3(8) . . ?
C9 C2 H2A 108.9 . . ?
C9 C2 H2B 108.9 . . ?
Ge3 C3 H3A 109.0 . . ?
Ge3 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C16 C3 Ge3 112.9(9) . . ?
C16 C3 H3A 109.0 . . ?
C16 C3 H3B 109.0 . . ?
Ge3 C4 H4A 108.3 . . ?
Ge3 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C12 C4 Ge3 115.9(10) . . ?
C12 C4 H4A 108.3 . . ?
C12 C4 H4B 108.3 . . ?
Ge5 C5 H5A 108.1 . . ?
Ge5 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C17 C5 Ge5 116.6(11) . . ?
C17 C5 H5A 108.1 . . ?
C17 C5 H5B 108.1 . . ?
Ge2 C6 H6A 109.3 . . ?
Ge2 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C14 C6 Ge2 111.7(8) . . ?
C14 C6 H6A 109.3 . . ?
C14 C6 H6B 109.3 . . ?
Ge2 C7 H7A 109.0 . . ?
Ge2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C21 C7 Ge2 112.8(9) . . ?
C21 C7 H7A 109.0 . . ?
C21 C7 H7B 109.0 . . ?
Ge2 C8 H8A 108.4 . . ?
Ge2 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C38 C8 Ge2 116(2) . . ?
C38 C8 H8A 108.4 . . ?
C38 C8 H8B 108.4 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Ge4 C10 H10A 108.9 . . ?
Ge4 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C20 C10 Ge4 113.2(9) . . ?
C20 C10 H10A 108.9 . . ?
C20 C10 H10B 108.9 . . ?
C1 C11 H11A 109.5 . . ?
C1 C11 H11B 109.5 . . ?
C1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 C12 H12A 109.5 . . ?
C4 C12 H12B 109.5 . . ?
C4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Ge1 C13 H13A 108.7 . . ?
Ge1 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C23 C13 Ge1 114.3(11) . . ?
C23 C13 H13A 108.7 . . ?
C23 C13 H13B 108.7 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Ge5 C15 H15A 108.4 . . ?
Ge5 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C33 C15 Ge5 115(2) . . ?
C33 C15 H15A 108.4 . . ?
C33 C15 H15B 108.4 . . ?
C3 C16 H16A 109.5 . . ?
C3 C16 H16B 109.5 . . ?
C3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C5 C17 H17A 109.5 . . ?
C5 C17 H17B 109.5 . . ?
C5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Ge4 C18 H18A 108.8 . . ?
Ge4 C18 H18B 108.8 . . ?
H18A C18 H18B 107.6 . . ?
C22 C18 Ge4 114.0(10) . . ?
C22 C18 H18A 108.8 . . ?
C22 C18 H18B 108.8 . . ?
Ge1 C19 H19A 109.2 . . ?
Ge1 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C42 C19 Ge1 111.8(15) . . ?
C42 C19 H19A 109.2 . . ?
C42 C19 H19B 109.2 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C21 H21A 109.5 . . ?
C7 C21 H21B 109.5 . . ?
C7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C13 C23 H23A 109.5 . . ?
C13 C23 H23B 109.5 . . ?
C13 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C45 C24 H24A 109.5 . . ?
C45 C24 H24B 109.5 . . ?
C45 C24 H24C 109.5 . . ?
C15 C33 H33A 109.5 . . ?
C15 C33 H33B 109.5 . . ?
C15 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Ge4 C35 H35A 100.1 . . ?
Ge4 C35 H35B 100.1 . . ?
H35A C35 H35B 104.2 . . ?
C43 C35 Ge4 147(4) . . ?
C43 C35 H35A 100.1 . . ?
C43 C35 H35B 100.1 . . ?
C8 C38 H38A 109.5 . . ?
C8 C38 H38B 109.5 . . ?
C8 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C19 C42 H42A 109.5 . . ?
C19 C42 H42B 109.5 . . ?
C19 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C35 C43 H43A 109.5 . . ?
C35 C43 H43B 109.5 . . ?
C35 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Ge5 C45 H45A 108.9 . . ?
Ge5 C45 H45B 108.9 . . ?
C24 C45 Ge5 113.5(13) . . ?
C24 C45 H45A 108.9 . . ?
C24 C45 H45B 108.9 . . ?
H45A C45 H45B 107.7 . . ?
H38D C38A H38E 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
C8A C38A H38D 109.5 . . ?
C8A C38A H38E 109.5 . . ?
C8A C38A H38F 109.5 . . ?
Ge2 C8A H8AA 108.6 . . ?
Ge2 C8A H8AB 108.6 . . ?
C38A C8A Ge2 115(3) . . ?
C38A C8A H8AA 108.6 . . ?
C38A C8A H8AB 108.6 . . ?
H8AA C8A H8AB 107.6 . . ?
Ge4 C35A H35C 103.8 . . ?
Ge4 C35A H35D 103.8 . . ?
H35C C35A H35D 105.4 . . ?
C43A C35A Ge4 134(3) . . ?
C43A C35A H35C 103.8 . . ?
C43A C35A H35D 103.8 . . ?
C35A C43A H43D 109.5 . . ?
C35A C43A H43E 109.5 . . ?
C35A C43A H43F 109.5 . . ?
H43D C43A H43E 109.5 . . ?
H43D C43A H43F 109.5 . . ?
H43E C43A H43F 109.5 . . ?
Ge1 C19A H19C 107.1 . . ?
Ge1 C19A H19D 107.1 . . ?
H19C C19A H19D 106.8 . . ?
C42A C19A Ge1 121(2) . . ?
C42A C19A H19C 107.1 . . ?
C42A C19A H19D 107.1 . . ?
C19A C42A H42D 109.5 . . ?
C19A C42A H42E 109.5 . . ?
C19A C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
Ge5 C15A H15C 107.7 . . ?
Ge5 C15A H15D 107.7 . . ?
H15C C15A H15D 107.1 . . ?
C33A C15A Ge5 118.6(18) . . ?
C33A C15A H15C 107.7 . . ?
C33A C15A H15D 107.7 . . ?
C15A C33A H33D 109.5 . . ?
C15A C33A H33E 109.5 . . ?
C15A C33A H33F 109.5 . . ?
H33D C33A H33E 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
Ge5 C45A H45C 109.0 . . ?
Ge5 C45A H45D 109.0 . . ?
H45C C45A H45D 107.8 . . ?
C24A C45A Ge5 113(3) . . ?
C24A C45A H45C 109.0 . . ?
C24A C45A H45D 109.0 . . ?
C45A C24A H24D 109.5 . . ?
C45A C24A H24E 109.5 . . ?
C45A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
As10 Ge5 C15 C33 -148(3) . . . . ?
C5 Ge5 C15 C33 80(3) . . . . ?
C45 Ge5 C15 C33 -42(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.433
_oxdiff_exptl_absorpt_empirical_full_min 0.552
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_s5961r
_database_code_depnum_ccdc_archive 'CCDC 2202019'
loop_
_audit_author_name
_audit_author_address
'Inigo Vitorica-yrezabal'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2021-11-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H42 Ge3 N3 O3 P7, C2.5 H2.5 N0.5'
_chemical_formula_sum            'C32.50 H44.50 Ge3 N3.50 O3 P7'
_chemical_formula_weight         966.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H P N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.93920(10)
_cell_length_b                   20.9710(2)
_cell_length_c                   18.2317(2)
_cell_angle_alpha                90
_cell_angle_beta                 89.9510(10)
_cell_angle_gamma                90
_cell_volume                     4182.46(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13788
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4370
_cell_measurement_theta_min      3.1720
_shelx_estimated_absorpt_T_max   0.739
_shelx_estimated_absorpt_T_min   0.435
_exptl_absorpt_coefficient_mu    5.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19585
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.884
_diffrn_reflns_theta_min         3.212
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  44.00   1.00    1.00    --  -43.99  34.00  89.00   42
  2  ω    -92.00 -67.00   1.00    1.00    --  -43.99 -34.00 -68.00   25
  3  ω    -60.00  -4.00   1.00    1.00    --  -43.99  34.00  89.00   56
  4  ω   -115.00 -70.00   1.00    1.00    --  -46.21 -34.00 -68.00   45
  5  ω    -89.00 -62.00   1.00    1.00    -- -107.20  34.00  89.00   27
  6  ω   -168.00 -70.00   1.00    1.00    -- -107.20 -34.00 -68.00   98
  7  ω      5.00  30.00   1.00    1.00    --    5.00  34.00  89.00   25
  8  ω   -132.00 -12.00   1.00    1.00    --  -43.99 -57.00-150.00  120
  9  ω   -148.00 -23.00   1.00    1.00    -- -107.20  37.00 -60.00  125
 10  ω   -103.00 -22.00   1.00    1.00    -- -107.20  57.00  30.00   81
 11  ω   -108.00 -79.00   1.00    1.00    -- -107.20  57.00-120.00   29
 12  ω   -129.00 -30.00   1.00    1.00    -- -107.20  57.00 -60.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1260860000
_diffrn_orient_matrix_UB_12      0.0061916000
_diffrn_orient_matrix_UB_13      -0.0367102000
_diffrn_orient_matrix_UB_21      -0.0184034000
_diffrn_orient_matrix_UB_22      0.0726141000
_diffrn_orient_matrix_UB_23      -0.0065331000
_diffrn_orient_matrix_UB_31      0.0596904000
_diffrn_orient_matrix_UB_32      0.0093437000
_diffrn_orient_matrix_UB_33      0.0758919000
_diffrn_oxdiff_digest_frames     
;
01852a298a5c9f582c02d593b74a51bfb700772ff84
;
_diffrn_oxdiff_digest_hkl        
;
010413becc803543a55eb050db4a97f940b589
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7327
_reflns_number_total             7766
_reflns_odcompleteness_completeness 93.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²+5.6226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0829
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N4, C32}
3. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(C32)
4. Others
 Fixed Sof: C32(0.5) H32(0.5) H31(0.5) H31A(0.5) H33(0.5) H33A(0.5) N4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C16(H16), C28(H28), C10(H10), C17(H17), C9(H9), C26(H26),
 C20(H20), C7(H7), C19(H19), C8(H8), C6(H6), C18(H18), C27(H27), C32(H32),
 C31(H31), C31(H31A), C33(H33), C33(H33A)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C2(H2A,H2B,H2C),
  C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge3 Ge 0.97347(2) 0.34220(2) 0.47806(2) 0.02054(8) Uani 1 1 d . . . . .
Ge2 Ge 0.60716(3) 0.55120(2) 0.14221(2) 0.02107(8) Uani 1 1 d . . . . .
Ge1 Ge 0.32749(2) 0.16675(2) 0.29807(2) 0.02162(8) Uani 1 1 d . . . . .
P4 P 0.84936(5) 0.37840(3) 0.24127(3) 0.01836(13) Uani 1 1 d . . . . .
P3 P 0.59703(6) 0.33377(3) 0.15610(3) 0.01963(13) Uani 1 1 d . . . . .
P6 P 0.75441(6) 0.29270(3) 0.09602(3) 0.02182(13) Uani 1 1 d . . . . .
P7 P 0.91995(5) 0.30656(3) 0.16357(3) 0.02119(13) Uani 1 1 d . . . . .
P1 P 0.66650(5) 0.34228(3) 0.26844(3) 0.01722(12) Uani 1 1 d . . . . .
P2 P 0.72050(5) 0.24252(3) 0.28230(3) 0.01740(12) Uani 1 1 d . . . . .
P5 P 0.80878(5) 0.21953(3) 0.17635(3) 0.01968(13) Uani 1 1 d . . . . .
O2 O 0.69627(17) 0.43238(9) 0.07961(10) 0.0268(4) Uani 1 1 d . . . . .
O1 O 0.54917(16) 0.17506(8) 0.20604(10) 0.0240(4) Uani 1 1 d . . . . .
O3 O 1.00759(16) 0.30555(8) 0.32210(10) 0.0252(4) Uani 1 1 d . . . . .
N3 N 0.90348(18) 0.37760(9) 0.39056(11) 0.0196(4) Uani 1 1 d . . . . .
N2 N 0.55346(18) 0.46546(10) 0.16091(11) 0.0211(4) Uani 1 1 d . . . . .
N1 N 0.48147(18) 0.20776(10) 0.31707(11) 0.0205(4) Uani 1 1 d . . . . .
C29 C 0.8038(3) 0.54614(12) 0.36732(14) 0.0269(5) Uani 1 1 d . . . . .
H29 H 0.833849 0.584856 0.347172 0.032 Uiso 1 1 calc R . . . .
C30 C 0.8748(2) 0.49116(12) 0.36495(13) 0.0222(5) Uani 1 1 d . . . . .
H30 H 0.954491 0.492690 0.344237 0.027 Uiso 1 1 calc R . . . .
C16 C 0.4442(2) 0.46509(13) 0.27796(15) 0.0260(5) Uani 1 1 d . . . . .
H16 H 0.512023 0.485648 0.300312 0.031 Uiso 1 1 calc R . . . .
C28 C 0.6887(2) 0.54409(13) 0.39927(14) 0.0267(5) Uani 1 1 d . . . . .
H28 H 0.640228 0.581617 0.401630 0.032 Uiso 1 1 calc R . . . .
C3 C 0.3623(3) 0.07837(13) 0.27496(17) 0.0318(6) Uani 1 1 d . . . . .
H3A H 0.383827 0.074659 0.222946 0.048 Uiso 1 1 calc GR . . . .
H3B H 0.289869 0.052316 0.285172 0.048 Uiso 1 1 calc GR . . . .
H3C H 0.430719 0.063457 0.305063 0.048 Uiso 1 1 calc GR . . . .
C4 C 0.2499(3) 0.21438(15) 0.21987(17) 0.0353(6) Uani 1 1 d . . . . .
H4A H 0.215593 0.253960 0.239694 0.053 Uiso 1 1 calc GR . . . .
H4B H 0.184347 0.188684 0.198286 0.053 Uiso 1 1 calc GR . . . .
H4C H 0.310602 0.224589 0.182079 0.053 Uiso 1 1 calc GR . . . .
C10 C 0.5755(2) 0.21104(13) 0.43874(15) 0.0270(5) Uani 1 1 d . . . . .
H10 H 0.612412 0.170773 0.429720 0.032 Uiso 1 1 calc R . . . .
C17 C 0.3409(3) 0.45048(14) 0.31955(16) 0.0323(6) Uani 1 1 d . . . . .
H17 H 0.337723 0.461927 0.369928 0.039 Uiso 1 1 calc R . . . .
C21 C 0.9317(2) 0.34871(12) 0.32609(13) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.5927(2) 0.24172(15) 0.50558(15) 0.0320(6) Uani 1 1 d . . . . .
H9 H 0.642549 0.222612 0.542142 0.038 Uiso 1 1 calc R . . . .
C26 C 0.7142(2) 0.43221(12) 0.42446(13) 0.0210(5) Uani 1 1 d . . . . .
H26 H 0.683172 0.393377 0.443783 0.025 Uiso 1 1 calc R . . . .
C20 C 0.3486(2) 0.41954(13) 0.17164(16) 0.0293(6) Uani 1 1 d . . . . .
H20 H 0.349890 0.409672 0.120792 0.035 Uiso 1 1 calc R . . . .
C7 C 0.4657(2) 0.32811(13) 0.46588(15) 0.0273(6) Uani 1 1 d . . . . .
H7 H 0.427459 0.367983 0.475172 0.033 Uiso 1 1 calc R . . . .
C19 C 0.2468(3) 0.40394(15) 0.21426(19) 0.0390(7) Uani 1 1 d . . . . .
H19 H 0.179572 0.382496 0.192444 0.047 Uiso 1 1 calc R . . . .
C23 C 1.1475(2) 0.35809(14) 0.47298(15) 0.0281(6) Uani 1 1 d . . . . .
H23A H 1.181614 0.336720 0.429760 0.042 Uiso 1 1 calc GR . . . .
H23B H 1.186970 0.341519 0.517302 0.042 Uiso 1 1 calc GR . . . .
H23C H 1.162155 0.404087 0.469319 0.042 Uiso 1 1 calc GR . . . .
C22 C 0.8978(3) 0.38877(15) 0.55750(14) 0.0314(6) Uani 1 1 d . . . . .
H22A H 0.908873 0.434637 0.549627 0.047 Uiso 1 1 calc GR . . . .
H22B H 0.935811 0.376431 0.604030 0.047 Uiso 1 1 calc GR . . . .
H22C H 0.810266 0.378866 0.559119 0.047 Uiso 1 1 calc GR . . . .
C25 C 0.8301(2) 0.43418(11) 0.39261(12) 0.0177(4) Uani 1 1 d . . . . .
C14 C 0.7804(2) 0.55433(13) 0.16460(16) 0.0291(6) Uani 1 1 d . . . . .
H14A H 0.798559 0.524469 0.204480 0.044 Uiso 1 1 calc GR . . . .
H14B H 0.802637 0.597646 0.179699 0.044 Uiso 1 1 calc GR . . . .
H14C H 0.827475 0.542445 0.120941 0.044 Uiso 1 1 calc GR . . . .
C11 C 0.6205(2) 0.41982(12) 0.12702(13) 0.0214(5) Uani 1 1 d . . . . .
C24 C 0.9329(3) 0.25242(13) 0.48002(16) 0.0309(6) Uani 1 1 d . . . . .
H24A H 0.849824 0.246320 0.461264 0.046 Uiso 1 1 calc GR . . . .
H24B H 0.937630 0.236666 0.530544 0.046 Uiso 1 1 calc GR . . . .
H24C H 0.990813 0.228805 0.449247 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.5041(2) 0.23979(12) 0.38544(13) 0.0201(5) Uani 1 1 d . . . . .
C8 C 0.5375(2) 0.30012(15) 0.51909(15) 0.0314(6) Uani 1 1 d . . . . .
H8 H 0.549060 0.320808 0.564921 0.038 Uiso 1 1 calc R . . . .
C15 C 0.4482(2) 0.44970(11) 0.20422(14) 0.0216(5) Uani 1 1 d . . . . .
C13 C 0.5700(3) 0.57170(13) 0.04149(15) 0.0331(6) Uani 1 1 d . . . . .
H13A H 0.610723 0.541104 0.009005 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.599014 0.614858 0.030423 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.481432 0.569551 0.033895 0.050 Uiso 1 1 calc GR . . . .
C6 C 0.4492(2) 0.29803(12) 0.39873(14) 0.0240(5) Uani 1 1 d . . . . .
H6 H 0.400258 0.317463 0.361968 0.029 Uiso 1 1 calc R . . . .
C2 C 0.2418(3) 0.17519(17) 0.39060(17) 0.0390(7) Uani 1 1 d . . . . .
H2A H 0.296961 0.163968 0.430909 0.059 Uiso 1 1 calc GR . . . .
H2B H 0.171016 0.146545 0.391065 0.059 Uiso 1 1 calc GR . . . .
H2C H 0.214072 0.219315 0.396624 0.059 Uiso 1 1 calc GR . . . .
C1 C 0.5673(2) 0.20375(11) 0.26357(13) 0.0185(5) Uani 1 1 d . . . . .
C18 C 0.2431(3) 0.41932(14) 0.28747(18) 0.0365(7) Uani 1 1 d . . . . .
H18 H 0.173380 0.408582 0.316049 0.044 Uiso 1 1 calc R . . . .
C12 C 0.5146(2) 0.60391(13) 0.20979(15) 0.0282(6) Uani 1 1 d . . . . .
H12A H 0.428603 0.590778 0.209197 0.042 Uiso 1 1 calc GR . . . .
H12B H 0.520851 0.648691 0.194872 0.042 Uiso 1 1 calc GR . . . .
H12C H 0.547487 0.598900 0.259430 0.042 Uiso 1 1 calc GR . . . .
C27 C 0.6446(2) 0.48748(13) 0.42767(14) 0.0256(5) Uani 1 1 d . . . . .
H27 H 0.565871 0.486387 0.449615 0.031 Uiso 1 1 calc R . . . .
C32 C 0.9350(5) 0.5490(2) -0.0424(3) 0.0897(15) Uani 0.5 1 d . . P A 1
H32 H 0.895931 0.580740 -0.071189 0.108 Uiso 0.5 1 calc R . P A 1
C31 C 0.8886(5) 0.4907(3) -0.0327(3) 0.0860(17) Uani 1 1 d . . . . .
H31 H 0.810329 0.480570 -0.052072 0.103 Uiso 0.5 1 calc R . P A 1
H31A H 0.810329 0.480570 -0.052072 0.103 Uiso 0.5 1 calc R . P A 2
C33 C 1.0410(6) 0.5586(2) -0.0083(5) 0.110(2) Uani 1 1 d . . . . .
H33 H 1.074497 0.600378 -0.010257 0.132 Uiso 0.5 1 calc R . P A 1
H33A H 1.074497 0.600378 -0.010257 0.132 Uiso 0.5 1 calc R . P A 2
N4 N 0.9350(5) 0.5490(2) -0.0424(3) 0.0897(15) Uani 0.5 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge3 N3 1.919(2) . ?
Ge3 C23 1.935(3) . ?
Ge3 C22 1.933(3) . ?
Ge3 C24 1.935(3) . ?
Ge2 N2 1.922(2) . ?
Ge2 C14 1.940(3) . ?
Ge2 C13 1.930(3) . ?
Ge2 C12 1.940(3) . ?
Ge1 N1 1.923(2) . ?
Ge1 C3 1.938(3) . ?
Ge1 C4 1.937(3) . ?
Ge1 C2 1.937(3) . ?
P4 P7 2.2071(8) . ?
P4 P1 2.1951(8) . ?
P4 C21 1.895(3) . ?
P3 P6 2.2141(8) . ?
P3 P1 2.1925(9) . ?
P3 C11 1.898(3) . ?
P6 P7 2.2101(9) . ?
P6 P5 2.2035(9) . ?
P7 P5 2.2055(9) . ?
P1 P2 2.1886(8) . ?
P2 P5 2.2121(8) . ?
P2 C1 1.894(2) . ?
O2 C11 1.226(3) . ?
O1 C1 1.225(3) . ?
O3 C21 1.231(3) . ?
N3 C21 1.358(3) . ?
N3 C25 1.433(3) . ?
N2 C11 1.354(3) . ?
N2 C15 1.434(3) . ?
N1 C5 1.438(3) . ?
N1 C1 1.356(3) . ?
C29 C30 1.391(4) . ?
C29 C28 1.387(4) . ?
C30 C25 1.386(3) . ?
C16 C17 1.394(4) . ?
C16 C15 1.383(4) . ?
C28 C27 1.382(4) . ?
C10 C9 1.391(4) . ?
C10 C5 1.385(4) . ?
C17 C18 1.384(4) . ?
C9 C8 1.388(4) . ?
C26 C25 1.395(3) . ?
C26 C27 1.388(4) . ?
C20 C19 1.396(4) . ?
C20 C15 1.394(4) . ?
C7 C8 1.380(4) . ?
C7 C6 1.389(4) . ?
C19 C18 1.374(5) . ?
C5 C6 1.382(4) . ?
C32 C31 1.335(7) . ?
C32 C33 1.332(8) . ?
C31 C33 1.491(9) 3_765 ?
C31 N4 1.335(7) . ?
C33 N4 1.332(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ge3 C23 106.66(10) . . ?
N3 Ge3 C22 104.86(10) . . ?
N3 Ge3 C24 107.47(11) . . ?
C22 Ge3 C23 111.70(12) . . ?
C22 Ge3 C24 112.33(13) . . ?
C24 Ge3 C23 113.20(12) . . ?
N2 Ge2 C14 107.03(10) . . ?
N2 Ge2 C13 108.22(11) . . ?
N2 Ge2 C12 105.14(10) . . ?
C14 Ge2 C12 110.89(12) . . ?
C13 Ge2 C14 113.53(13) . . ?
C13 Ge2 C12 111.54(12) . . ?
N1 Ge1 C3 107.16(10) . . ?
N1 Ge1 C4 106.63(11) . . ?
N1 Ge1 C2 103.04(10) . . ?
C4 Ge1 C3 114.78(13) . . ?
C4 Ge1 C2 112.45(14) . . ?
C2 Ge1 C3 111.80(14) . . ?
P1 P4 P7 103.15(3) . . ?
C21 P4 P7 97.66(8) . . ?
C21 P4 P1 97.81(7) . . ?
P1 P3 P6 102.94(3) . . ?
C11 P3 P6 97.29(8) . . ?
C11 P3 P1 97.86(8) . . ?
P7 P6 P3 108.08(3) . . ?
P5 P6 P3 98.75(3) . . ?
P5 P6 P7 59.96(3) . . ?
P4 P7 P6 99.27(3) . . ?
P5 P7 P4 107.73(3) . . ?
P5 P7 P6 59.87(3) . . ?
P3 P1 P4 97.69(3) . . ?
P2 P1 P4 96.31(3) . . ?
P2 P1 P3 97.12(3) . . ?
P1 P2 P5 103.01(3) . . ?
C1 P2 P1 98.66(8) . . ?
C1 P2 P5 97.74(8) . . ?
P6 P5 P7 60.17(3) . . ?
P6 P5 P2 108.11(3) . . ?
P7 P5 P2 98.75(3) . . ?
C21 N3 Ge3 117.16(16) . . ?
C21 N3 C25 121.3(2) . . ?
C25 N3 Ge3 121.49(15) . . ?
C11 N2 Ge2 114.52(16) . . ?
C11 N2 C15 121.5(2) . . ?
C15 N2 Ge2 123.95(16) . . ?
C5 N1 Ge1 121.12(14) . . ?
C1 N1 Ge1 116.66(16) . . ?
C1 N1 C5 122.2(2) . . ?
C28 C29 C30 119.6(2) . . ?
C25 C30 C29 120.4(2) . . ?
C15 C16 C17 120.1(3) . . ?
C27 C28 C29 120.0(2) . . ?
C5 C10 C9 119.3(3) . . ?
C18 C17 C16 120.0(3) . . ?
O3 C21 P4 120.96(19) . . ?
O3 C21 N3 122.2(2) . . ?
N3 C21 P4 116.88(18) . . ?
C8 C9 C10 120.3(3) . . ?
C27 C26 C25 119.4(2) . . ?
C15 C20 C19 119.5(3) . . ?
C8 C7 C6 120.1(3) . . ?
C18 C19 C20 120.6(3) . . ?
C30 C25 N3 120.5(2) . . ?
C30 C25 C26 119.8(2) . . ?
C26 C25 N3 119.7(2) . . ?
O2 C11 P3 119.49(19) . . ?
O2 C11 N2 122.4(2) . . ?
N2 C11 P3 118.13(18) . . ?
C10 C5 N1 120.2(2) . . ?
C6 C5 N1 119.3(2) . . ?
C6 C5 C10 120.5(2) . . ?
C7 C8 C9 119.9(2) . . ?
C16 C15 N2 120.4(2) . . ?
C16 C15 C20 119.7(2) . . ?
C20 C15 N2 119.8(2) . . ?
C5 C6 C7 119.9(3) . . ?
O1 C1 P2 120.59(17) . . ?
O1 C1 N1 122.3(2) . . ?
N1 C1 P2 117.13(18) . . ?
C19 C18 C17 119.9(3) . . ?
C28 C27 C26 120.7(2) . . ?
C33 C32 C31 114.1(6) . . ?
C32 C31 C33 120.3(5) . 3_765 ?
N4 C31 C33 120.3(5) . 3_765 ?
C32 C33 C31 125.4(5) . 3_765 ?
C33 N4 C31 114.1(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.779
_vrf_PLAT029_s5961r              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Why?  
RESPONSE: Crystal is metrically orthorhombic but has a monoclinic space-group.
The experimental strategy assumed an orthorhombic spacegroup, resulting in 
not enough data being collected for the monoclinic spacegroup. Due to the
sensitivity of these crystals, another experiment could not be performed to
extend the data collection strategy and collect the additional data for 
completeness.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_s5953l
_database_code_depnum_ccdc_archive 'CCDC 2202020'
loop_
_audit_author_name
_audit_author_address
'Inigo Vitorica-yrezabal'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2021-10-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H60 Ge3 N3 O3 P7'
_chemical_formula_sum            'C39 H60 Ge3 N3 O3 P7'
_chemical_formula_weight         1053.46
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.6729(2)
_cell_length_b                   20.5725(3)
_cell_length_c                   15.8849(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.2470(10)
_cell_angle_gamma                90
_cell_volume                     4781.82(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19305
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.7200
_cell_measurement_theta_min      2.0720
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.482
_exptl_absorpt_coefficient_mu    4.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29680
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.240
_diffrn_reflns_theta_min         3.521
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00 133.00   1.00    1.00    --   43.34  20.00-120.00  178
  2  ω     24.00 104.00   1.00    1.00    --   45.86  40.00-180.00   80
  3  ω     67.00 134.00   1.00    1.00    --   45.86  50.00-150.00   67
  4  ω    -23.00   3.00   1.00    1.00    --   45.86  40.00-180.00   26
  5  ω     33.00  60.00   1.00    1.00    --  108.20  50.00 120.00   27
  6  ω     21.00  46.00   1.00    1.00    --  108.20  30.00 150.00   25
  7  ω     20.00 142.00   1.00    1.00    --  108.20  50.00 150.00  122
  8  ω     89.00 137.00   1.00    1.00    --  108.20  50.00-180.00   48
  9  ω     94.00 196.00   1.00    1.00    --  108.20  30.00 150.00  102
 10  ω    152.00 195.00   1.00    1.00    --  108.20  50.00-180.00   43
 11  ω    150.00 198.00   1.00    1.00    --  108.20  50.00 150.00   48
 12  ω    135.00 191.00   1.00    1.00    --  108.20  50.00 120.00   56
 13  ω     84.00 198.00   1.00    1.00    --  108.20  20.00 -30.00  114
 14  ω    154.00 179.00   1.00    1.00    --  108.20  30.00-150.00   25
 15  ω     19.00  74.00   1.00    1.00    --  108.20  20.00 -30.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0930511000
_diffrn_orient_matrix_UB_12      -0.0345560000
_diffrn_orient_matrix_UB_13      0.0133234000
_diffrn_orient_matrix_UB_21      -0.0444917000
_diffrn_orient_matrix_UB_22      -0.0639337000
_diffrn_orient_matrix_UB_23      -0.0326634000
_diffrn_orient_matrix_UB_31      0.0213436000
_diffrn_orient_matrix_UB_32      0.0179474000
_diffrn_orient_matrix_UB_33      -0.0906233000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9318
_reflns_number_total             9613
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9613
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0475
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+12.5994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1094
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ge3-N6 \\sim Ge3A-N6
 with sigma of 0.02
 C38A-C2 \\sim C38-C2A
 with sigma of 0.002
 C1-C2 \\sim C1A-C2A
 with sigma of 0.04
 Ge3-C2 \\sim Ge3A-C2A
 with sigma of 0.04
 Ge3-C1 \\sim Ge3A-C1A
 with sigma of 0.02
 N6-C2 \\sim N6-C2A
 with sigma of 0.04
 C1-C37 \\sim C1A-C37A
 with sigma of 0.02
 Ge3-C37 \\sim Ge3A-C37A
 with sigma of 0.04
 N6-C1 \\sim N6-C1A
 with sigma of 0.04
 C36-C3 \\sim C3A-C36A
 with sigma of 0.002
 Ge3-C3 \\sim Ge3A-C3A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C38A \\sim C2A \\sim C2 \\sim C38: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C4A \\sim C39A \\sim C39: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C4A \\sim C39 \\sim C39A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C4 \\sim C39 \\sim C39A \\sim C4A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C3 \\sim C36 \\sim C3A \\sim C36A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Ge3A \\sim Ge3: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Rigid body (RIGU) restrains
 Ge3, C1, C2, C36, C37, C38, Ge3A, C38A, C2A, C1A, C37A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C36A, C3, C36, C3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(Ge3A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
 Sof(Ge3)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=FVAR(2)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B), C9(H9A,H9B), C4(H4A,
 H4B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C4A(H4AA,H4AB), C2A(H2AA,H2AB),
 C1A(H1AA,H1AB), C3A(H3AA,H3AB)
6.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C29(H29A,H29B,
 H29C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F), C38A(H38D,H38E,H38F),
 C37A(H37D,H37E,H37F), C36A(H36D,H36E,H36F)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23),
 C27(H27), C28(H28), C30(H30), C32(H32), C33(H33), C21(H21), C22(H22), C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.98098(3) 0.00492(2) 0.68400(2) 0.02510(10) Uani 1 1 d . . . . .
Ge2 Ge 0.50625(3) -0.19962(2) 0.94555(3) 0.03053(11) Uani 1 1 d . . . . .
Ge3 Ge 1.05541(17) -0.40467(15) 0.86533(18) 0.0340(4) Uani 0.536(7) 1 d D U P A
1
P4 P 0.77812(6) -0.31029(4) 0.79801(5) 0.02760(18) Uani 1 1 d . . . . .
P5 P 0.70880(5) -0.16239(4) 0.74276(5) 0.02554(17) Uani 1 1 d . . . . .
P6 P 0.91291(5) -0.21271(4) 0.70379(5) 0.02548(17) Uani 1 1 d . . . . .
P7 P 0.82688(5) -0.20937(4) 0.81035(5) 0.02444(17) Uani 1 1 d . . . . .
P8 P 0.74236(6) -0.32009(4) 0.66054(6) 0.0318(2) Uani 1 1 d . . . . .
P9 P 0.67637(6) -0.22614(5) 0.63310(6) 0.03092(19) Uani 1 1 d . . . . .
P10 P 0.81614(6) -0.24316(4) 0.59644(6) 0.03055(19) Uani 1 1 d . . . . .
O1 O 0.90207(16) -0.10982(12) 0.59779(15) 0.0307(5) Uani 1 1 d . . . . .
O2 O 0.90811(17) -0.38416(13) 0.73045(16) 0.0348(6) Uani 1 1 d . . . . .
N3 N 0.96395(17) -0.08162(12) 0.72727(16) 0.0204(5) Uani 1 1 d . . . . .
O4 O 0.55517(17) -0.22956(14) 0.77341(16) 0.0400(6) Uani 1 1 d . . . . .
N5 N 0.60783(18) -0.16891(13) 0.88643(17) 0.0248(6) Uani 1 1 d . . . . .
N6 N 0.94736(19) -0.35664(13) 0.86704(18) 0.0288(6) Uani 1 1 d D . . . .
C7 C 0.6120(2) -0.19167(17) 0.8062(2) 0.0288(7) Uani 1 1 d . . . . .
C8 C 0.8900(2) -0.35582(16) 0.7956(2) 0.0293(7) Uani 1 1 d . . . . .
C10 C 0.9252(2) -0.12494(15) 0.6713(2) 0.0242(6) Uani 1 1 d . . . . .
C11 C 0.9619(3) -0.07679(18) 0.8800(2) 0.0344(8) Uani 1 1 d . . . . .
H11 H 0.906657 -0.052606 0.872999 0.041 Uiso 1 1 calc R U . . .
C12 C 0.8612(3) -0.3659(2) 0.9929(3) 0.0410(9) Uani 1 1 d . . . . .
H12 H 0.833844 -0.405036 0.971788 0.049 Uiso 1 1 calc R U . . .
C13 C 1.0022(2) -0.09920(16) 0.8098(2) 0.0291(7) Uani 1 1 d . . . . .
C15 C 0.9599(3) -0.27437(19) 0.9759(2) 0.0370(8) Uani 1 1 d . . . . .
H15 H 1.000241 -0.250555 0.943356 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6672(3) -0.11844(17) 0.9187(2) 0.0336(8) Uani 1 1 d . . . . .
C18 C 1.0804(3) -0.1243(2) 0.9709(3) 0.0547(13) Uani 1 1 d . . . . .
H18 H 1.107420 -0.132274 1.026172 0.066 Uiso 1 1 calc R U . . .
C19 C 1.0005(3) -0.0890(2) 0.9602(3) 0.0450(10) Uani 1 1 d . . . . .
H19 H 0.972210 -0.073030 1.008002 0.054 Uiso 1 1 calc R U . . .
C20 C 0.8814(3) -0.2858(2) 1.1020(3) 0.0458(10) Uani 1 1 d . . . . .
H20 H 0.868486 -0.270272 1.156150 0.055 Uiso 1 1 calc R U . . .
C23 C 0.7263(3) -0.1324(2) 0.9889(3) 0.0436(9) Uani 1 1 d . . . . .
H23 H 0.731119 -0.175477 1.010131 0.052 Uiso 1 1 calc R U . . .
C25 C 0.9213(2) -0.33171(18) 0.9450(2) 0.0335(8) Uani 1 1 d . . . . .
C27 C 0.8416(3) -0.3427(2) 1.0712(3) 0.0471(10) Uani 1 1 d . . . . .
H27 H 0.800713 -0.365832 1.103821 0.057 Uiso 1 1 calc R U . . .
C28 C 0.9397(3) -0.2518(2) 1.0545(3) 0.0414(9) Uani 1 1 d . . . . .
H28 H 0.966360 -0.212415 1.075726 0.050 Uiso 1 1 calc R U . . .
C30 C 1.1209(3) -0.1481(2) 0.9021(4) 0.0562(14) Uani 1 1 d . . . . .
H30 H 1.175341 -0.173119 0.909953 0.067 Uiso 1 1 calc R U . . .
C32 C 0.7780(4) -0.0831(3) 1.0276(3) 0.0699(17) Uani 1 1 d . . . . .
H32 H 0.817484 -0.092516 1.076157 0.084 Uiso 1 1 calc R U . . .
C33 C 0.6613(3) -0.0556(2) 0.8866(3) 0.0486(11) Uani 1 1 d . . . . .
H33 H 0.620814 -0.045867 0.838790 0.058 Uiso 1 1 calc R U . . .
C14 C 0.8625(2) 0.03685(17) 0.6394(2) 0.0305(7) Uani 1 1 d . . . . .
H14A H 0.866021 0.084488 0.631520 0.037 Uiso 1 1 calc R U . . .
H14B H 0.846982 0.016920 0.583478 0.037 Uiso 1 1 calc R U . . .
C5 C 1.0733(2) -0.00218(19) 0.6024(3) 0.0367(8) Uani 1 1 d . . . . .
H5A H 1.051005 -0.032007 0.556502 0.044 Uiso 1 1 calc R U . . .
H5B H 1.082815 0.041057 0.577133 0.044 Uiso 1 1 calc R U . . .
C6 C 0.5259(3) -0.29271(17) 0.9613(2) 0.0355(8) Uani 1 1 d . . . . .
H6A H 0.470738 -0.311965 0.983576 0.043 Uiso 1 1 calc R U . . .
H6B H 0.533654 -0.312816 0.905631 0.043 Uiso 1 1 calc R U . . .
C17 C 1.0289(3) 0.05442(18) 0.7827(2) 0.0421(9) Uani 1 1 d . . . . .
H17A H 0.982533 0.055828 0.824859 0.051 Uiso 1 1 calc R U . . .
H17B H 1.083997 0.032485 0.808863 0.051 Uiso 1 1 calc R U . . .
C9 C 0.5177(3) -0.15307(19) 1.0527(3) 0.0413(9) Uani 1 1 d . . . . .
H9A H 0.476074 -0.173458 1.091310 0.050 Uiso 1 1 calc R U . . .
H9B H 0.580857 -0.158680 1.078080 0.050 Uiso 1 1 calc R U . . .
C4 C 0.394(2) -0.1708(12) 0.8875(17) 0.0505(18) Uani 0.404(9) 1 d . U P B 1
H4A H 0.354638 -0.151282 0.928846 0.061 Uiso 0.404(9) 1 calc R U P B 1
H4B H 0.407524 -0.136682 0.846338 0.061 Uiso 0.404(9) 1 calc R U P B 1
C3 C 1.1178(4) -0.3888(3) 0.9726(4) 0.0483(17) Uani 0.817(12) 1 d D U P A 1
H3A H 1.133643 -0.342079 0.976679 0.058 Uiso 0.817(12) 1 calc R U P A 1
H3B H 1.075768 -0.398366 1.016993 0.058 Uiso 0.817(12) 1 calc R U P A 1
C21 C 0.7162(5) -0.0070(2) 0.9257(4) 0.0730(19) Uani 1 1 d . . . . .
H21 H 0.714172 0.035893 0.903349 0.088 Uiso 1 1 calc R U . . .
C22 C 0.7732(5) -0.0209(3) 0.9968(4) 0.082(2) Uani 1 1 d . . . . .
H22 H 0.808926 0.012609 1.024049 0.099 Uiso 1 1 calc R U . . .
C1 C 1.0153(10) -0.4996(5) 0.8582(8) 0.068(3) Uani 0.536(7) 1 d D . P A 1
H1A H 1.040075 -0.521918 0.910124 0.082 Uiso 0.536(7) 1 calc R U P A 1
H1B H 0.947822 -0.500916 0.857753 0.082 Uiso 0.536(7) 1 calc R U P A 1
C2 C 1.1267(6) -0.3809(5) 0.7714(7) 0.066(3) Uani 0.536(7) 1 d D U P A 1
H2A H 1.181263 -0.409279 0.772239 0.080 Uiso 0.536(7) 1 calc R U P A 1
H2B H 1.089519 -0.389318 0.717875 0.080 Uiso 0.536(7) 1 calc R U P A 1
C31 C 0.7870(3) 0.02160(18) 0.6973(3) 0.0370(8) Uani 1 1 d . . . . .
H31A H 0.728725 0.038583 0.672316 0.055 Uiso 1 1 calc R U . . .
H31B H 0.782317 -0.025570 0.704434 0.055 Uiso 1 1 calc R U . . .
H31C H 0.801356 0.041998 0.752476 0.055 Uiso 1 1 calc R U . . .
C24 C 1.0822(3) -0.13568(19) 0.8203(3) 0.0419(9) Uani 1 1 d . . . . .
H24 H 1.110281 -0.151941 0.772586 0.050 Uiso 1 1 calc R U . . .
C26 C 0.6071(3) -0.3091(2) 1.0198(3) 0.0567(12) Uani 1 1 d . . . . .
H26A H 0.612744 -0.356470 1.024687 0.085 Uiso 1 1 calc R U . . .
H26B H 0.662336 -0.291279 0.997511 0.085 Uiso 1 1 calc R U . . .
H26C H 0.599344 -0.290426 1.075551 0.085 Uiso 1 1 calc R U . . .
C35 C 1.1649(3) -0.0275(3) 0.6427(3) 0.0565(12) Uani 1 1 d . . . . .
H35A H 1.209131 -0.030268 0.599568 0.085 Uiso 1 1 calc R U . . .
H35B H 1.187850 0.002388 0.687425 0.085 Uiso 1 1 calc R U . . .
H35C H 1.156045 -0.070663 0.666798 0.085 Uiso 1 1 calc R U . . .
C29 C 0.4966(5) -0.0805(2) 1.0476(3) 0.0709(17) Uani 1 1 d . . . . .
H29A H 0.504168 -0.061448 1.104251 0.106 Uiso 1 1 calc R U . . .
H29B H 0.538563 -0.059264 1.011012 0.106 Uiso 1 1 calc R U . . .
H29C H 0.433517 -0.074078 1.024275 0.106 Uiso 1 1 calc R U . . .
C34 C 1.0533(5) 0.1235(2) 0.7580(3) 0.079(2) Uani 1 1 d . . . . .
H34A H 1.077105 0.147349 0.808275 0.118 Uiso 1 1 calc R U . . .
H34B H 1.099882 0.122109 0.716877 0.118 Uiso 1 1 calc R U . . .
H34C H 0.998548 0.145422 0.732852 0.118 Uiso 1 1 calc R U . . .
C36 C 1.2038(5) -0.4281(3) 0.9901(4) 0.065(2) Uani 0.817(12) 1 d D U P A 1
H36A H 1.231766 -0.417215 1.046263 0.097 Uiso 0.817(12) 1 calc R U P A 1
H36B H 1.188793 -0.474525 0.987882 0.097 Uiso 0.817(12) 1 calc R U P A 1
H36C H 1.246764 -0.418146 0.947502 0.097 Uiso 0.817(12) 1 calc R U P A 1
C37 C 1.0430(12) -0.5370(6) 0.7844(8) 0.109(5) Uani 0.536(7) 1 d D . P A 1
H37A H 1.020206 -0.581663 0.787384 0.164 Uiso 0.536(7) 1 calc R U P A 1
H37B H 1.017257 -0.516509 0.732208 0.164 Uiso 0.536(7) 1 calc R U P A 1
H37C H 1.109815 -0.537581 0.784752 0.164 Uiso 0.536(7) 1 calc R U P A 1
C38 C 1.2036(7) -0.3599(6) 0.7384(9) 0.070(3) Uani 0.464(7) 1 d D U P A 2
H38A H 1.229134 -0.326741 0.702496 0.104 Uiso 0.464(7) 1 calc R U P A 2
H38B H 1.250070 -0.372931 0.782664 0.104 Uiso 0.464(7) 1 calc R U P A 2
H38C H 1.184843 -0.397780 0.704014 0.104 Uiso 0.464(7) 1 calc R U P A 2
C39 C 0.3904(5) -0.1237(4) 0.8214(5) 0.0538(17) Uani 0.596(9) 1 d . U P B 2
H39A H 0.330837 -0.120519 0.789501 0.081 Uiso 0.596(9) 1 calc R U P B 2
H39B H 0.400221 -0.085122 0.857200 0.081 Uiso 0.596(9) 1 calc R U P B 2
H39C H 0.438710 -0.126342 0.782098 0.081 Uiso 0.596(9) 1 calc R U P B 2
C4A C 0.3928(13) -0.1828(8) 0.8751(11) 0.0505(17) Uani 0.596(9) 1 d . U P B 2
H4AA H 0.380434 -0.220869 0.837940 0.061 Uiso 0.596(9) 1 calc R U P B 2
H4AB H 0.342087 -0.179801 0.912766 0.061 Uiso 0.596(9) 1 calc R U P B 2
C39A C 0.3430(7) -0.2248(6) 0.8421(7) 0.0506(19) Uani 0.404(9) 1 d . U P B 1
H39D H 0.286415 -0.207800 0.813645 0.076 Uiso 0.404(9) 1 calc R U P B 1
H39E H 0.380996 -0.243726 0.800262 0.076 Uiso 0.404(9) 1 calc R U P B 1
H39F H 0.328107 -0.258327 0.882775 0.076 Uiso 0.404(9) 1 calc R U P B 1
Ge3A Ge 1.0708(3) -0.3947(2) 0.8479(3) 0.0508(7) Uani 0.464(7) 1 d D U P A 2
C38A C 1.1575(10) -0.3107(5) 0.7725(12) 0.095(5) Uani 0.536(7) 1 d D U P A 1
H38D H 1.192778 -0.302367 0.723567 0.143 Uiso 0.536(7) 1 calc R U P A 1
H38E H 1.103893 -0.282181 0.770043 0.143 Uiso 0.536(7) 1 calc R U P A 1
H38F H 1.195758 -0.302168 0.824478 0.143 Uiso 0.536(7) 1 calc R U P A 1
C2A C 1.1216(6) -0.3322(6) 0.7784(8) 0.050(3) Uani 0.464(7) 1 d D U P A 2
H2AA H 1.075041 -0.318432 0.733740 0.060 Uiso 0.464(7) 1 calc R U P A 2
H2AB H 1.140366 -0.293545 0.812508 0.060 Uiso 0.464(7) 1 calc R U P A 2
C1A C 1.0545(6) -0.4828(4) 0.8114(5) 0.0354(19) Uani 0.464(7) 1 d D . P A 2
H1AA H 1.034406 -0.482480 0.750482 0.042 Uiso 0.464(7) 1 calc R U P A 2
H1AB H 1.114679 -0.504767 0.817486 0.042 Uiso 0.464(7) 1 calc R U P A 2
C37A C 0.9868(7) -0.5233(5) 0.8572(8) 0.044(3) Uani 0.464(7) 1 d D . P A 2
H37D H 0.983818 -0.567255 0.833493 0.065 Uiso 0.464(7) 1 calc R U P A 2
H37E H 1.006693 -0.525453 0.917367 0.065 Uiso 0.464(7) 1 calc R U P A 2
H37F H 0.926163 -0.503094 0.850148 0.065 Uiso 0.464(7) 1 calc R U P A 2
C3A C 1.1608(13) -0.3790(11) 0.9382(10) 0.043(6) Uani 0.183(12) 1 d D U P A 2
H3AA H 1.222258 -0.387486 0.918797 0.052 Uiso 0.183(12) 1 calc R U P A 2
H3AB H 1.158209 -0.332809 0.955406 0.052 Uiso 0.183(12) 1 calc R U P A 2
C36A C 1.1454(19) -0.4219(12) 1.0127(14) 0.049(7) Uani 0.183(12) 1 d D U P A 2
H36D H 1.192442 -0.412945 1.058306 0.074 Uiso 0.183(12) 1 calc R U P A 2
H36E H 1.084942 -0.412960 1.032415 0.074 Uiso 0.183(12) 1 calc R U P A 2
H36F H 1.148909 -0.467567 0.995853 0.074 Uiso 0.183(12) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N3 1.931(2) . ?
Ge1 C14 1.942(3) . ?
Ge1 C5 1.948(4) . ?
Ge1 C17 1.956(4) . ?
Ge2 N5 1.926(3) . ?
Ge2 C6 1.950(4) . ?
Ge2 C9 1.949(4) . ?
Ge2 C4 1.92(3) . ?
Ge2 C4A 1.966(19) . ?
Ge3 N6 1.870(4) . ?
Ge3 C3 1.902(5) . ?
Ge3 C1 2.040(11) . ?
Ge3 C2 1.947(11) . ?
P4 P7 2.1999(11) . ?
P4 P8 2.2169(12) . ?
P4 C8 1.893(4) . ?
P5 P7 2.1939(11) . ?
P5 P9 2.2042(13) . ?
P5 C7 1.899(3) . ?
P6 P7 2.1862(12) . ?
P6 P10 2.2266(12) . ?
P6 C10 1.890(3) . ?
P8 P9 2.1909(13) . ?
P8 P10 2.2084(13) . ?
P9 P10 2.2009(13) . ?
O1 C10 1.231(4) . ?
O2 C8 1.234(4) . ?
N3 C10 1.355(4) . ?
N3 C13 1.433(4) . ?
O4 C7 1.229(4) . ?
N5 C7 1.363(4) . ?
N5 C16 1.426(4) . ?
N6 C8 1.362(4) . ?
N6 C25 1.418(5) . ?
N6 Ge3A 2.017(5) . ?
C11 H11 0.9500 . ?
C11 C13 1.380(5) . ?
C11 C19 1.379(5) . ?
C12 H12 0.9500 . ?
C12 C25 1.397(6) . ?
C12 C27 1.382(6) . ?
C13 C24 1.394(5) . ?
C15 H15 0.9500 . ?
C15 C25 1.383(5) . ?
C15 C28 1.384(6) . ?
C16 C23 1.390(6) . ?
C16 C33 1.390(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.379(7) . ?
C18 C30 1.373(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C20 C27 1.380(6) . ?
C20 C28 1.374(6) . ?
C23 H23 0.9500 . ?
C23 C32 1.383(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C30 H30 0.9500 . ?
C30 C24 1.403(6) . ?
C32 H32 0.9500 . ?
C32 C22 1.371(9) . ?
C33 H33 0.9500 . ?
C33 C21 1.401(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C31 1.524(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C35 1.535(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C26 1.494(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C34 1.524(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C29 1.526(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C39A 1.49(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C36 1.507(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(10) . ?
C22 H22 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C37 1.485(14) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C38A 1.513(10) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 C2A 1.513(10) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 C4A 1.485(19) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C39A H39D 0.9800 . ?
C39A H39E 0.9800 . ?
C39A H39F 0.9800 . ?
Ge3A C2A 1.883(14) . ?
Ge3A C1A 1.913(8) . ?
Ge3A C3A 1.902(6) . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C37A 1.523(12) . ?
C37A H37D 0.9800 . ?
C37A H37E 0.9800 . ?
C37A H37F 0.9800 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C36A 1.507(7) . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ge1 C14 107.79(13) . . ?
N3 Ge1 C5 106.40(14) . . ?
N3 Ge1 C17 104.06(14) . . ?
C14 Ge1 C5 115.50(16) . . ?
C14 Ge1 C17 112.03(17) . . ?
C5 Ge1 C17 110.23(18) . . ?
N5 Ge2 C6 105.79(14) . . ?
N5 Ge2 C9 104.18(14) . . ?
N5 Ge2 C4A 108.5(6) . . ?
C6 Ge2 C4A 110.9(5) . . ?
C9 Ge2 C6 111.62(17) . . ?
C9 Ge2 C4A 115.1(5) . . ?
C4 Ge2 N5 109.4(9) . . ?
C4 Ge2 C6 118.5(7) . . ?
C4 Ge2 C9 106.4(7) . . ?
N6 Ge3 C3 104.4(2) . . ?
N6 Ge3 C1 105.4(4) . . ?
N6 Ge3 C2 112.5(3) . . ?
C3 Ge3 C1 109.4(4) . . ?
C3 Ge3 C2 113.2(4) . . ?
C2 Ge3 C1 111.5(5) . . ?
P7 P4 P8 103.02(5) . . ?
C8 P4 P7 101.06(11) . . ?
C8 P4 P8 94.44(11) . . ?
P7 P5 P9 103.94(5) . . ?
C7 P5 P7 101.24(11) . . ?
C7 P5 P9 95.99(11) . . ?
P7 P6 P10 103.28(5) . . ?
C10 P6 P7 104.70(10) . . ?
C10 P6 P10 97.33(11) . . ?
P5 P7 P4 97.61(4) . . ?
P6 P7 P4 95.97(5) . . ?
P6 P7 P5 96.62(4) . . ?
P9 P8 P4 100.64(5) . . ?
P9 P8 P10 60.04(4) . . ?
P10 P8 P4 107.50(5) . . ?
P8 P9 P5 107.54(5) . . ?
P8 P9 P10 60.38(4) . . ?
P10 P9 P5 98.80(5) . . ?
P8 P10 P6 98.92(5) . . ?
P9 P10 P6 107.85(5) . . ?
P9 P10 P8 59.59(4) . . ?
C10 N3 Ge1 115.6(2) . . ?
C10 N3 C13 123.5(3) . . ?
C13 N3 Ge1 120.4(2) . . ?
C7 N5 Ge2 115.7(2) . . ?
C7 N5 C16 121.2(3) . . ?
C16 N5 Ge2 122.5(2) . . ?
C8 N6 Ge3 117.8(3) . . ?
C8 N6 C25 122.2(3) . . ?
C8 N6 Ge3A 112.7(3) . . ?
C25 N6 Ge3 119.2(2) . . ?
C25 N6 Ge3A 125.1(2) . . ?
O4 C7 P5 119.2(3) . . ?
O4 C7 N5 122.5(3) . . ?
N5 C7 P5 118.3(2) . . ?
O2 C8 P4 119.4(3) . . ?
O2 C8 N6 122.4(3) . . ?
N6 C8 P4 118.2(3) . . ?
O1 C10 P6 118.4(2) . . ?
O1 C10 N3 122.0(3) . . ?
N3 C10 P6 119.5(2) . . ?
C13 C11 H11 119.5 . . ?
C19 C11 H11 119.5 . . ?
C19 C11 C13 121.0(4) . . ?
C25 C12 H12 120.1 . . ?
C27 C12 H12 120.1 . . ?
C27 C12 C25 119.9(4) . . ?
C11 C13 N3 119.5(3) . . ?
C11 C13 C24 119.4(3) . . ?
C24 C13 N3 121.0(3) . . ?
C25 C15 H15 120.1 . . ?
C25 C15 C28 119.8(4) . . ?
C28 C15 H15 120.1 . . ?
C23 C16 N5 117.8(3) . . ?
C33 C16 N5 121.7(4) . . ?
C33 C16 C23 120.3(4) . . ?
C19 C18 H18 119.9 . . ?
C30 C18 H18 119.9 . . ?
C30 C18 C19 120.3(4) . . ?
C11 C19 C18 119.8(5) . . ?
C11 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C27 C20 H20 120.0 . . ?
C28 C20 H20 120.0 . . ?
C28 C20 C27 120.1(4) . . ?
C16 C23 H23 120.2 . . ?
C32 C23 C16 119.6(5) . . ?
C32 C23 H23 120.2 . . ?
C12 C25 N6 121.1(3) . . ?
C15 C25 N6 119.3(4) . . ?
C15 C25 C12 119.6(4) . . ?
C12 C27 H27 119.9 . . ?
C20 C27 C12 120.1(4) . . ?
C20 C27 H27 119.9 . . ?
C15 C28 H28 119.8 . . ?
C20 C28 C15 120.5(4) . . ?
C20 C28 H28 119.8 . . ?
C18 C30 H30 119.9 . . ?
C18 C30 C24 120.2(4) . . ?
C24 C30 H30 119.9 . . ?
C23 C32 H32 119.5 . . ?
C22 C32 C23 120.9(6) . . ?
C22 C32 H32 119.5 . . ?
C16 C33 H33 120.5 . . ?
C16 C33 C21 118.9(5) . . ?
C21 C33 H33 120.5 . . ?
Ge1 C14 H14A 109.1 . . ?
Ge1 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C31 C14 Ge1 112.4(2) . . ?
C31 C14 H14A 109.1 . . ?
C31 C14 H14B 109.1 . . ?
Ge1 C5 H5A 109.2 . . ?
Ge1 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C35 C5 Ge1 112.2(3) . . ?
C35 C5 H5A 109.2 . . ?
C35 C5 H5B 109.2 . . ?
Ge2 C6 H6A 108.8 . . ?
Ge2 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C26 C6 Ge2 113.9(3) . . ?
C26 C6 H6A 108.8 . . ?
C26 C6 H6B 108.8 . . ?
Ge1 C17 H17A 109.5 . . ?
Ge1 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C34 C17 Ge1 110.9(3) . . ?
C34 C17 H17A 109.5 . . ?
C34 C17 H17B 109.5 . . ?
Ge2 C9 H9A 108.4 . . ?
Ge2 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C29 C9 Ge2 115.5(3) . . ?
C29 C9 H9A 108.4 . . ?
C29 C9 H9B 108.4 . . ?
Ge2 C4 H4A 109.1 . . ?
Ge2 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C39A C4 Ge2 112.5(15) . . ?
C39A C4 H4A 109.1 . . ?
C39A C4 H4B 109.1 . . ?
Ge3 C3 H3A 108.6 . . ?
Ge3 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C36 C3 Ge3 114.4(4) . . ?
C36 C3 H3A 108.6 . . ?
C36 C3 H3B 108.6 . . ?
C33 C21 H21 119.8 . . ?
C22 C21 C33 120.5(5) . . ?
C22 C21 H21 119.8 . . ?
C32 C22 C21 119.7(5) . . ?
C32 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
Ge3 C1 H1A 108.2 . . ?
Ge3 C1 H1B 108.2 . . ?
H1A C1 H1B 107.3 . . ?
C37 C1 Ge3 116.5(10) . . ?
C37 C1 H1A 108.2 . . ?
C37 C1 H1B 108.2 . . ?
Ge3 C2 H2A 108.7 . . ?
Ge3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C38A C2 Ge3 114.0(9) . . ?
C38A C2 H2A 108.7 . . ?
C38A C2 H2B 108.7 . . ?
C14 C31 H31A 109.5 . . ?
C14 C31 H31B 109.5 . . ?
C14 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 C24 C30 119.3(4) . . ?
C13 C24 H24 120.4 . . ?
C30 C24 H24 120.4 . . ?
C6 C26 H26A 109.5 . . ?
C6 C26 H26B 109.5 . . ?
C6 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C5 C35 H35A 109.5 . . ?
C5 C35 H35B 109.5 . . ?
C5 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C9 C29 H29A 109.5 . . ?
C9 C29 H29B 109.5 . . ?
C9 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C17 C34 H34A 109.5 . . ?
C17 C34 H34B 109.5 . . ?
C17 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C3 C36 H36A 109.5 . . ?
C3 C36 H36B 109.5 . . ?
C3 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C1 C37 H37A 109.5 . . ?
C1 C37 H37B 109.5 . . ?
C1 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C2A C38 H38A 109.5 . . ?
C2A C38 H38B 109.5 . . ?
C2A C38 H38C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C4A C39 H39A 109.5 . . ?
C4A C39 H39B 109.5 . . ?
C4A C39 H39C 109.5 . . ?
Ge2 C4A H4AA 108.0 . . ?
Ge2 C4A H4AB 108.0 . . ?
C39 C4A Ge2 117.0(11) . . ?
C39 C4A H4AA 108.0 . . ?
C39 C4A H4AB 108.0 . . ?
H4AA C4A H4AB 107.3 . . ?
C4 C39A H39D 109.5 . . ?
C4 C39A H39E 109.5 . . ?
C4 C39A H39F 109.5 . . ?
H39D C39A H39E 109.5 . . ?
H39D C39A H39F 109.5 . . ?
H39E C39A H39F 109.5 . . ?
C2A Ge3A N6 102.8(3) . . ?
C2A Ge3A C1A 121.0(5) . . ?
C2A Ge3A C3A 92.5(7) . . ?
C1A Ge3A N6 108.7(3) . . ?
C3A Ge3A N6 113.7(8) . . ?
C3A Ge3A C1A 117.0(8) . . ?
C2 C38A H38D 109.5 . . ?
C2 C38A H38E 109.5 . . ?
C2 C38A H38F 109.5 . . ?
H38D C38A H38E 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
C38 C2A Ge3A 110.6(9) . . ?
C38 C2A H2AA 109.5 . . ?
C38 C2A H2AB 109.5 . . ?
Ge3A C2A H2AA 109.5 . . ?
Ge3A C2A H2AB 109.5 . . ?
H2AA C2A H2AB 108.1 . . ?
Ge3A C1A H1AA 108.2 . . ?
Ge3A C1A H1AB 108.2 . . ?
H1AA C1A H1AB 107.3 . . ?
C37A C1A Ge3A 116.4(6) . . ?
C37A C1A H1AA 108.2 . . ?
C37A C1A H1AB 108.2 . . ?
C1A C37A H37D 109.5 . . ?
C1A C37A H37E 109.5 . . ?
C1A C37A H37F 109.5 . . ?
H37D C37A H37E 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
Ge3A C3A H3AA 109.5 . . ?
Ge3A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 108.0 . . ?
C36A C3A Ge3A 110.9(14) . . ?
C36A C3A H3AA 109.5 . . ?
C36A C3A H3AB 109.5 . . ?
C3A C36A H36D 109.5 . . ?
C3A C36A H36E 109.5 . . ?
C3A C36A H36F 109.5 . . ?
H36D C36A H36E 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 N3 C10 P6 175.52(14) . . . . ?
Ge1 N3 C10 O1 -0.3(4) . . . . ?
Ge1 N3 C13 C11 74.9(4) . . . . ?
Ge1 N3 C13 C24 -101.6(3) . . . . ?
Ge2 N5 C7 P5 178.78(15) . . . . ?
Ge2 N5 C7 O4 -0.3(4) . . . . ?
Ge2 N5 C16 C23 70.5(4) . . . . ?
Ge2 N5 C16 C33 -104.0(4) . . . . ?
Ge3 N6 C8 P4 177.48(19) . . . . ?
Ge3 N6 C8 O2 -1.6(5) . . . . ?
Ge3 N6 C25 C12 -94.6(4) . . . . ?
Ge3 N6 C25 C15 81.8(4) . . . . ?
P7 P4 C8 O2 -113.3(3) . . . . ?
P7 P4 C8 N6 67.6(3) . . . . ?
P7 P5 C7 O4 -111.9(3) . . . . ?
P7 P5 C7 N5 69.0(3) . . . . ?
P7 P6 C10 O1 -123.6(2) . . . . ?
P7 P6 C10 N3 60.4(2) . . . . ?
P8 P4 C8 O2 -9.1(3) . . . . ?
P8 P4 C8 N6 171.8(3) . . . . ?
P9 P5 C7 O4 -6.4(3) . . . . ?
P9 P5 C7 N5 174.5(2) . . . . ?
P10 P6 C10 O1 -17.8(3) . . . . ?
P10 P6 C10 N3 166.3(2) . . . . ?
N3 C13 C24 C30 175.7(3) . . . . ?
N5 C16 C23 C32 -173.3(4) . . . . ?
N5 C16 C33 C21 174.6(4) . . . . ?
N6 Ge3A C2A C38 -165.1(8) . . . . ?
C7 N5 C16 C23 -119.1(4) . . . . ?
C7 N5 C16 C33 66.4(5) . . . . ?
C8 N6 C25 C12 74.8(5) . . . . ?
C8 N6 C25 C15 -108.7(4) . . . . ?
C10 N3 C13 C11 -113.9(4) . . . . ?
C10 N3 C13 C24 69.5(4) . . . . ?
C11 C13 C24 C30 -0.9(5) . . . . ?
C13 N3 C10 P6 4.0(4) . . . . ?
C13 N3 C10 O1 -171.8(3) . . . . ?
C13 C11 C19 C18 -0.4(6) . . . . ?
C16 N5 C7 P5 7.7(4) . . . . ?
C16 N5 C7 O4 -171.4(3) . . . . ?
C16 C23 C32 C22 -1.3(7) . . . . ?
C16 C33 C21 C22 -1.9(7) . . . . ?
C18 C30 C24 C13 -0.3(6) . . . . ?
C19 C11 C13 N3 -175.4(3) . . . . ?
C19 C11 C13 C24 1.2(5) . . . . ?
C19 C18 C30 C24 1.1(6) . . . . ?
C23 C16 C33 C21 0.3(6) . . . . ?
C23 C32 C22 C21 -0.3(8) . . . . ?
C25 N6 C8 P4 7.9(4) . . . . ?
C25 N6 C8 O2 -171.2(3) . . . . ?
C25 C12 C27 C20 -0.1(6) . . . . ?
C25 C15 C28 C20 -0.1(6) . . . . ?
C27 C12 C25 N6 175.7(3) . . . . ?
C27 C12 C25 C15 -0.7(6) . . . . ?
C27 C20 C28 C15 -0.8(6) . . . . ?
C28 C15 C25 N6 -175.7(3) . . . . ?
C28 C15 C25 C12 0.8(6) . . . . ?
C28 C20 C27 C12 0.8(7) . . . . ?
C30 C18 C19 C11 -0.8(6) . . . . ?
C33 C16 C23 C32 1.3(6) . . . . ?
C33 C21 C22 C32 1.9(8) . . . . ?
C3 Ge3 N6 C8 176.5(3) . . . . ?
C3 Ge3 N6 C25 -13.5(4) . . . . ?
C1 Ge3 N6 C8 -68.3(5) . . . . ?
C1 Ge3 N6 C25 101.7(5) . . . . ?
C2 Ge3 N6 C8 53.4(5) . . . . ?
C2 Ge3 N6 C25 -136.7(4) . . . . ?
Ge3A N6 C8 P4 -170.9(2) . . . . ?
Ge3A N6 C8 O2 10.0(4) . . . . ?
Ge3A N6 C25 C12 -106.6(4) . . . . ?
Ge3A N6 C25 C15 69.9(4) . . . . ?
C1A Ge3A C2A C38 -43.8(10) . . . . ?
C3A Ge3A C2A C38 79.9(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.410
_oxdiff_exptl_absorpt_empirical_full_min 0.661
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_s5950l
_database_code_depnum_ccdc_archive 'CCDC 2202022'
loop_
_audit_author_name
_audit_author_address
'Inigo Vitorica-yrezabal'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2022-08-17 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2021-10-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H48 Ge3 N3 O9 P7 S3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C35 H53 Ge3 N3 O9.50 P7 S3'
_chemical_formula_weight         1198.54
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.2603(3)
_cell_length_b                   13.7420(3)
_cell_length_c                   14.7414(3)
_cell_angle_alpha                73.987(2)
_cell_angle_beta                 87.041(2)
_cell_angle_gamma                89.564(2)
_cell_volume                     2578.49(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23456
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.8810
_cell_measurement_theta_min      3.0520
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.320
_exptl_absorpt_coefficient_mu    5.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32445
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.409
_diffrn_reflns_theta_min         3.123
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     41.00 107.00   1.00    1.00    --   43.53  50.00 -30.00   66
  2  ω    -45.00   6.00   1.00    1.00    --   43.53  60.00-150.00   51
  3  ω     93.00 133.00   1.00    1.00    --   43.53  60.00-150.00   40
  4  ω    -44.00 133.00   1.00    1.00    --   43.53  60.00  90.00  177
  5  ω      9.00  51.00   1.00    1.00    --   46.07  60.00 -60.00   42
  6  ω    -43.00 135.00   1.00    1.00    --   46.07  60.00  30.00  178
  7  ω     96.00 134.00   1.00    1.00    --   46.07  60.00 -60.00   38
  8  ω    -42.00  -7.00   1.00    1.00    --   46.07  60.00 -60.00   35
  9  ω     19.00  92.00   1.00    1.00    --  108.20  50.00-150.00   73
 10  ω    120.00 198.00   1.00    1.00    --  108.20  50.00-120.00   78
 11  ω    148.00 197.00   1.00    1.00    --  108.20  50.00  90.00   49
 12  ω    120.00 198.00   1.00    1.00    --  108.20  50.00   0.00   78
 13  ω     44.00  87.00   1.00    1.00    --  108.20  50.00 -60.00   43
 14  ω    103.00 128.00   1.00    1.00    --  108.20  50.00 -60.00   25
 15  ω    106.00 132.00   1.00    1.00    --  108.20  50.00  90.00   26
 16  ω     53.00  91.00   1.00    1.00    --  108.20  50.00  90.00   38
 17  ω     70.00  96.00   1.00    1.00    --  108.20  50.00   0.00   26
 18  ω     20.00 187.00   1.00    1.00    --  108.20  50.00  60.00  167
 19  ω    136.00 197.00   1.00    1.00    --  108.20  50.00 -60.00   61
 20  ω     19.00 198.00   1.00    1.00    --  108.20  50.00 150.00  179
 21  ω     24.00 191.00   1.00    1.00    --  108.20  10.00 -30.00  167
 22  ω     83.00 113.00   1.00    1.00    --  108.20  50.00-120.00   30
 23  ω    103.00 197.00   1.00    1.00    --  108.20  50.00-150.00   94
 24  ω    140.00 167.00   1.00    1.00    --  108.20  50.00 120.00   27
 25  ω     22.00  47.00   1.00    1.00    --  108.20  50.00   0.00   25
 26  ω    126.00 169.00   1.00    1.00    --  108.20  50.00 -90.00   43
 27  ω    142.00 168.00   1.00    1.00    --  108.20  50.00 -30.00   26
 28  ω    145.00 170.00   1.00    1.00    --  108.20  50.00  30.00   25
 29  ω     31.00  57.00   1.00    1.00    --  108.20  50.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0207985000
_diffrn_orient_matrix_UB_12      0.1112925000
_diffrn_orient_matrix_UB_13      -0.0031149000
_diffrn_orient_matrix_UB_21      -0.0584793000
_diffrn_orient_matrix_UB_22      -0.0346776000
_diffrn_orient_matrix_UB_23      0.0965960000
_diffrn_orient_matrix_UB_31      0.0983958000
_diffrn_orient_matrix_UB_32      0.0038675000
_diffrn_orient_matrix_UB_33      0.0501190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9771
_reflns_number_total             10226
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.131
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10226
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+3.1773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0774
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O14-C1B
 1.41 with sigma of 0.02
 C1C-C1D
 1.5 with sigma of 0.02
 O14-C1C
 1.42 with sigma of 0.02
 C1A-C1B
 1.48 with sigma of 0.02
 O14-C1A = O14-C1D
 2.37 with sigma of 0.04
 C17-C22 \\sim C17-C22A
 with sigma of 0.02
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20
 with sigma of 0.02
 C17-C21 \\sim C17-C21A
 with sigma of 0.04
 C20-C21 \\sim C20-C21A
 with sigma of 0.02
 C20-C22 \\sim C20-C22A
 with sigma of 0.04
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C22 \\sim C23 \\sim C21 \\sim C18A
\\sim C22A \\sim C21A \\sim C19A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
C19 \\sim C19A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
4. Rigid body (RIGU) restrains
 C1B, O14, C1C, C1A, C1D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C18A)=Sof(H18A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=Sof(C19A)=
 Sof(H19A)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C22)=Sof(H22)=Sof(C21)=Sof(H21)=FVAR(1)
 Fixed Sof: O14(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB)
6.b Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C28(H28), C7(H7), C18(H18), C29(H29), C11(H11), C19(H19),
 C8(H8), C10(H10), C22(H22), C21(H21), C18A(H18A), C22A(H22A), C21A(H21A),
 C19A(H19A)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C14(H14A,H14B,H14C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.59194(2) 0.33376(2) 0.09762(2) 0.02173(7) Uani 1 1 d . . . . .
Ge3 Ge 0.00372(2) 0.38986(2) 0.19659(2) 0.02692(7) Uani 1 1 d . . . . .
Ge2 Ge 0.36145(2) 0.74711(2) 0.47852(2) 0.02679(7) Uani 1 1 d . . . . .
S10 S 0.35118(5) 0.12665(4) 0.27570(4) 0.02870(12) Uani 1 1 d . . . . .
S9 S 0.14950(4) 0.70492(4) 0.06868(4) 0.02579(12) Uani 1 1 d . . . . .
P6 P 0.36433(4) 0.52840(4) 0.22177(4) 0.01841(11) Uani 1 1 d . . . . .
P7 P 0.45835(4) 0.50135(4) 0.34528(4) 0.02055(11) Uani 1 1 d . . . . .
P1 P 0.30442(4) 0.37491(4) 0.24847(4) 0.01973(11) Uani 1 1 d . . . . .
P5 P 0.22925(4) 0.58362(4) 0.28551(4) 0.02023(11) Uani 1 1 d . . . . .
S8 S 0.58542(4) 0.71579(4) 0.23298(4) 0.02392(11) Uani 1 1 d . . . . .
P3 P 0.35205(4) 0.42760(4) 0.46523(4) 0.02353(12) Uani 1 1 d . . . . .
P2 P 0.27193(4) 0.32263(4) 0.40397(4) 0.02318(12) Uani 1 1 d . . . . .
P4 P 0.19786(4) 0.46292(4) 0.41973(4) 0.02293(11) Uani 1 1 d . . . . .
O6 O 0.08096(11) 0.46426(11) 0.25897(11) 0.0237(3) Uani 1 1 d . . . . .
O1 O 0.49135(11) 0.37400(11) 0.17632(11) 0.0230(3) Uani 1 1 d . . . . .
O2 O 0.39908(12) 0.63077(12) 0.44251(11) 0.0252(3) Uani 1 1 d . . . . .
O4 O 0.58168(12) 0.62575(13) 0.20147(11) 0.0292(3) Uani 1 1 d . . . . .
O8 O 0.25603(12) 0.70726(13) 0.08227(13) 0.0343(4) Uani 1 1 d . . . . .
O9 O 0.11845(13) 0.71516(13) -0.02522(11) 0.0326(4) Uani 1 1 d . . . . .
O11 O 0.25440(13) 0.16875(13) 0.29333(14) 0.0360(4) Uani 1 1 d . . . . .
O5 O 0.57122(14) 0.81154(13) 0.16623(12) 0.0343(4) Uani 1 1 d . . . . .
O12 O 0.39204(16) 0.04868(13) 0.35038(13) 0.0388(4) Uani 1 1 d . . . . .
N3 N 0.50557(14) 0.71071(15) 0.32170(13) 0.0253(4) Uani 1 1 d . . . . .
N7 N 0.09685(14) 0.59955(15) 0.13282(14) 0.0257(4) Uani 1 1 d . . . . .
N10 N 0.43804(14) 0.21341(14) 0.23759(14) 0.0251(4) Uani 1 1 d . . . . .
C1 C 0.42198(16) 0.30959(16) 0.22282(15) 0.0218(4) Uani 1 1 d . . . . .
C13 C 0.12727(16) 0.54865(16) 0.21464(15) 0.0218(4) Uani 1 1 d . . . . .
C2 C 0.45659(16) 0.63025(16) 0.36747(15) 0.0219(4) Uani 1 1 d . . . . .
C31 C 0.64559(17) 0.46750(18) 0.03824(17) 0.0274(5) Uani 1 1 d . . . . .
H31A H 0.599445 0.504564 -0.008889 0.041 Uiso 1 1 calc R U . . .
H31B H 0.711748 0.462122 0.007219 0.041 Uiso 1 1 calc R U . . .
H31C H 0.652850 0.503799 0.086208 0.041 Uiso 1 1 calc R U . . .
C14 C -0.12362(19) 0.4575(2) 0.17336(19) 0.0346(5) Uani 1 1 d . . . . .
H14A H -0.162909 0.448279 0.233327 0.052 Uiso 1 1 calc R U . . .
H14B H -0.161071 0.428875 0.131087 0.052 Uiso 1 1 calc R U . . .
H14C H -0.111815 0.529935 0.143837 0.052 Uiso 1 1 calc R U . . .
C25 C 0.39925(18) -0.00042(17) 0.16640(18) 0.0290(5) Uani 1 1 d . . . . .
H25 H 0.443096 -0.033280 0.214271 0.035 Uiso 1 1 calc R U . . .
C24 C 0.34218(18) 0.08180(17) 0.17536(17) 0.0275(5) Uani 1 1 d . . . . .
C32 C 0.51677(18) 0.27516(18) 0.01684(17) 0.0275(5) Uani 1 1 d . . . . .
H32A H 0.497068 0.205610 0.051049 0.041 Uiso 1 1 calc R U . . .
H32B H 0.558944 0.274753 -0.039639 0.041 Uiso 1 1 calc R U . . .
H32C H 0.456121 0.315369 -0.001922 0.041 Uiso 1 1 calc R U . . .
C33 C 0.68042(18) 0.24434(19) 0.18236(17) 0.0304(5) Uani 1 1 d . . . . .
H33A H 0.695892 0.273750 0.233550 0.046 Uiso 1 1 calc R U . . .
H33B H 0.743172 0.235411 0.147506 0.046 Uiso 1 1 calc R U . . .
H33C H 0.647113 0.178492 0.209013 0.046 Uiso 1 1 calc R U . . .
C26 C 0.39126(19) -0.03385(18) 0.08652(18) 0.0301(5) Uani 1 1 d . . . . .
H26 H 0.429262 -0.090807 0.080465 0.036 Uiso 1 1 calc R U . . .
C17 C 0.09192(18) 0.80176(18) 0.10931(17) 0.0280(5) Uani 1 1 d D U . . .
C6 C 0.70269(18) 0.71710(19) 0.28355(16) 0.0279(5) Uani 1 1 d . . . . .
C27 C 0.32854(18) 0.01447(18) 0.01492(18) 0.0301(5) Uani 1 1 d . . . . .
C15 C 0.0841(2) 0.3818(2) 0.08622(19) 0.0389(6) Uani 1 1 d . . . . .
H15A H 0.083598 0.447341 0.038263 0.058 Uiso 1 1 calc R U . . .
H15B H 0.055874 0.329656 0.060774 0.058 Uiso 1 1 calc R U . . .
H15C H 0.153626 0.364237 0.103482 0.058 Uiso 1 1 calc R U . . .
C28 C 0.2750(2) 0.0992(2) 0.0242(2) 0.0351(5) Uani 1 1 d . . . . .
H28 H 0.234017 0.134622 -0.025127 0.042 Uiso 1 1 calc R U . . .
C7 C 0.7671(2) 0.6360(2) 0.29079(19) 0.0391(6) Uani 1 1 d . . . . .
H7 H 0.747429 0.579892 0.269659 0.047 Uiso 1 1 calc R U . . .
C18 C 0.1404(12) 0.8417(13) 0.1718(13) 0.025(3) Uani 0.454(15) 1 d D U P A 1
H18 H 0.202288 0.813823 0.196618 0.030 Uiso 0.454(15) 1 calc R U P A 1
C29 C 0.28081(19) 0.13257(18) 0.1042(2) 0.0333(5) Uani 1 1 d . . . . .
H29 H 0.243109 0.189674 0.110320 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4795(2) 0.8144(2) 0.5031(2) 0.0413(6) Uani 1 1 d . . . . .
H3A H 0.487972 0.796518 0.571386 0.062 Uiso 1 1 calc R U . . .
H3B H 0.471459 0.887801 0.478975 0.062 Uiso 1 1 calc R U . . .
H3C H 0.539049 0.793048 0.471578 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2789(2) 0.6758(2) 0.5888(2) 0.0438(7) Uani 1 1 d . . . . .
H4A H 0.230056 0.632415 0.570664 0.066 Uiso 1 1 calc R U . . .
H4B H 0.242865 0.724974 0.615461 0.066 Uiso 1 1 calc R U . . .
H4C H 0.322181 0.634121 0.636203 0.066 Uiso 1 1 calc R U . . .
C11 C 0.7303(2) 0.7986(2) 0.3150(2) 0.0422(6) Uani 1 1 d . . . . .
H11 H 0.686050 0.854168 0.310548 0.051 Uiso 1 1 calc R U . . .
C5 C 0.2818(2) 0.82189(19) 0.3772(2) 0.0362(6) Uani 1 1 d . . . . .
H5A H 0.321084 0.833047 0.317018 0.054 Uiso 1 1 calc R U . . .
H5B H 0.263341 0.887328 0.387559 0.054 Uiso 1 1 calc R U . . .
H5C H 0.220375 0.783386 0.375404 0.054 Uiso 1 1 calc R U . . .
C19 C 0.0977(14) 0.923(2) 0.198(2) 0.035(2) Uani 0.454(15) 1 d D U P A 1
H19 H 0.132513 0.951921 0.238701 0.042 Uiso 0.454(15) 1 calc R U P A 1
C30 C 0.3185(2) -0.0249(2) -0.0699(2) 0.0365(6) Uani 1 1 d . . . . .
H30A H 0.385224 -0.043958 -0.090994 0.055 Uiso 1 1 calc R U . . .
H30B H 0.290001 0.027836 -0.120962 0.055 Uiso 1 1 calc R U . . .
H30C H 0.273832 -0.084390 -0.052847 0.055 Uiso 1 1 calc R U . . .
C16 C -0.0045(2) 0.2666(2) 0.2981(2) 0.0402(6) Uani 1 1 d . . . . .
H16A H 0.060791 0.232091 0.301994 0.060 Uiso 1 1 calc R U . . .
H16B H -0.056756 0.222349 0.286054 0.060 Uiso 1 1 calc R U . . .
H16C H -0.021560 0.282580 0.357794 0.060 Uiso 1 1 calc R U . . .
C8 C 0.8603(2) 0.6367(3) 0.3290(2) 0.0479(7) Uani 1 1 d . . . . .
H8 H 0.904309 0.580946 0.333354 0.057 Uiso 1 1 calc R U . . .
C20 C 0.0076(3) 0.9619(2) 0.1665(2) 0.0471(7) Uani 1 1 d D U . . .
C9 C 0.8901(2) 0.7163(3) 0.3605(2) 0.0481(8) Uani 1 1 d . . . . .
C10 C 0.8248(3) 0.7976(3) 0.3534(2) 0.0534(8) Uani 1 1 d . . . . .
H10 H 0.844645 0.853266 0.374935 0.064 Uiso 1 1 calc R U . . .
C12 C 0.9913(2) 0.7157(3) 0.4035(3) 0.0663(11) Uani 1 1 d . . . . .
H12A H 0.994164 0.657966 0.459829 0.100 Uiso 1 1 calc R U . . .
H12B H 1.000003 0.778741 0.421130 0.100 Uiso 1 1 calc R U . . .
H12C H 1.045338 0.710027 0.357315 0.100 Uiso 1 1 calc R U . . .
C22 C -0.0122(6) 0.8132(8) 0.1050(8) 0.0369(19) Uani 0.454(15) 1 d D U P A 1
H22 H -0.052208 0.769532 0.081356 0.044 Uiso 0.454(15) 1 calc R U P A 1
C23 C -0.0381(3) 1.0506(3) 0.1957(3) 0.0683(11) Uani 1 1 d . U . . .
H23A H -0.091840 1.026135 0.244733 0.103 Uiso 1 1 calc R U . . .
H23B H -0.066321 1.098301 0.140735 0.103 Uiso 1 1 calc R U . . .
H23C H 0.014250 1.084690 0.220405 0.103 Uiso 1 1 calc R U . . .
C21 C -0.0552(7) 0.8908(8) 0.1367(8) 0.048(2) Uani 0.454(15) 1 d D U P A 1
H21 H -0.126592 0.897774 0.139138 0.058 Uiso 0.454(15) 1 calc R U P A 1
O14 O 0.8824(6) 0.0017(4) 0.4393(4) 0.103(2) Uani 0.5 1 d D . P B -1
C1A C 1.0566(14) -0.0183(12) 0.4738(11) 0.158(5) Uani 0.5 1 d D . P B -1
H1AA H 1.099030 -0.045408 0.527413 0.237 Uiso 0.5 1 calc R U P B -1
H1AB H 1.070923 -0.054173 0.425668 0.237 Uiso 0.5 1 calc R U P B -1
H1AC H 1.071008 0.054013 0.446715 0.237 Uiso 0.5 1 calc R U P B -1
C1B C 0.9505(15) -0.0323(11) 0.5060(10) 0.154(5) Uani 0.5 1 d D . P B -1
H1BA H 0.938045 -0.105492 0.535168 0.185 Uiso 0.5 1 calc R U P B -1
H1BB H 0.938129 0.002360 0.556150 0.185 Uiso 0.5 1 calc R U P B -1
C1C C 0.7722(9) -0.0104(7) 0.4635(7) 0.136(4) Uani 0.5 1 d D . P B -1
H1CA H 0.756009 -0.083539 0.486804 0.163 Uiso 0.5 1 calc R U P B -1
H1CB H 0.755369 0.020312 0.515672 0.163 Uiso 0.5 1 calc R U P B -1
C1D C 0.7093(9) 0.0345(7) 0.3862(8) 0.122(3) Uani 0.5 1 d D . P B -1
H1DA H 0.638098 0.023329 0.407773 0.182 Uiso 0.5 1 calc R U P B -1
H1DB H 0.723178 0.107410 0.363564 0.182 Uiso 0.5 1 calc R U P B -1
H1DC H 0.723819 0.003382 0.334646 0.182 Uiso 0.5 1 calc R U P B -1
C18A C 0.1481(11) 0.8549(11) 0.1564(11) 0.032(3) Uani 0.546(15) 1 d D U P A 2
H18A H 0.216816 0.838146 0.167738 0.038 Uiso 0.546(15) 1 calc R U P A 2
C22A C 0.0039(5) 0.8479(6) 0.0678(7) 0.0342(16) Uani 0.546(15) 1 d D U P A 2
H22A H -0.026866 0.823475 0.021503 0.041 Uiso 0.546(15) 1 calc R U P A 2
C21A C -0.0372(5) 0.9288(6) 0.0948(7) 0.0390(17) Uani 0.546(15) 1 d D U P A 2
H21A H -0.095107 0.962069 0.065609 0.047 Uiso 0.546(15) 1 calc R U P A 2
C19A C 0.1039(12) 0.9321(16) 0.1869(18) 0.035(2) Uani 0.546(15) 1 d D U P A 2
H19A H 0.141495 0.965331 0.222939 0.042 Uiso 0.546(15) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O1 1.9010(15) . ?
Ge1 C31 1.928(2) . ?
Ge1 C32 1.930(2) . ?
Ge1 C33 1.931(2) . ?
Ge3 O6 1.8899(15) . ?
Ge3 C14 1.922(2) . ?
Ge3 C15 1.927(3) . ?
Ge3 C16 1.925(3) . ?
Ge2 O2 1.8750(15) . ?
Ge2 C3 1.924(3) . ?
Ge2 C4 1.938(3) . ?
Ge2 C5 1.924(3) . ?
S10 O11 1.4444(18) . ?
S10 O12 1.4337(19) . ?
S10 N10 1.6273(19) . ?
S10 C24 1.762(2) . ?
S9 O8 1.4387(17) . ?
S9 O9 1.4338(17) . ?
S9 N7 1.634(2) . ?
S9 C17 1.758(2) . ?
P6 P7 2.2049(7) . ?
P6 P1 2.1840(7) . ?
P6 P5 2.2059(7) . ?
P7 P3 2.2174(8) . ?
P7 C2 1.888(2) . ?
P1 P2 2.2251(7) . ?
P1 C1 1.866(2) . ?
P5 P4 2.2258(8) . ?
P5 C13 1.893(2) . ?
S8 O4 1.4386(17) . ?
S8 O5 1.4269(17) . ?
S8 N3 1.6261(19) . ?
S8 C6 1.761(2) . ?
P3 P2 2.2058(8) . ?
P3 P4 2.1938(8) . ?
P2 P4 2.2203(8) . ?
O6 C13 1.304(3) . ?
O1 C1 1.308(3) . ?
O2 C2 1.312(3) . ?
N3 C2 1.286(3) . ?
N7 C13 1.299(3) . ?
N10 C1 1.297(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C24 1.388(3) . ?
C25 C26 1.386(3) . ?
C24 C29 1.388(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.394(4) . ?
C17 C18 1.382(11) . ?
C17 C22 1.391(8) . ?
C17 C18A 1.382(10) . ?
C17 C22A 1.409(6) . ?
C6 C7 1.383(4) . ?
C6 C11 1.383(4) . ?
C27 C28 1.395(3) . ?
C27 C30 1.505(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C28 H28 0.9500 . ?
C28 C29 1.383(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(11) . ?
C29 H29 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C11 H11 0.9500 . ?
C11 C10 1.399(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C19 H19 0.9500 . ?
C19 C20 1.356(12) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C9 1.369(5) . ?
C20 C23 1.513(4) . ?
C20 C21 1.459(9) . ?
C20 C21A 1.418(7) . ?
C20 C19A 1.361(10) . ?
C9 C10 1.393(5) . ?
C9 C12 1.512(4) . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C21 1.385(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C21 H21 0.9500 . ?
O14 C1B 1.355(14) . ?
O14 C1C 1.485(12) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1A C1B 1.457(14) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C1C C1D 1.441(13) . ?
C1D H1DA 0.9800 . ?
C1D H1DB 0.9800 . ?
C1D H1DC 0.9800 . ?
C18A H18A 0.9500 . ?
C18A C19A 1.378(10) . ?
C22A H22A 0.9500 . ?
C22A C21A 1.380(7) . ?
C21A H21A 0.9500 . ?
C19A H19A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ge1 C31 96.36(8) . . ?
O1 Ge1 C32 104.37(8) . . ?
O1 Ge1 C33 105.75(9) . . ?
C31 Ge1 C32 115.01(10) . . ?
C31 Ge1 C33 115.18(11) . . ?
C32 Ge1 C33 116.72(10) . . ?
O6 Ge3 C14 106.94(9) . . ?
O6 Ge3 C15 106.49(9) . . ?
O6 Ge3 C16 96.55(10) . . ?
C14 Ge3 C15 115.95(12) . . ?
C14 Ge3 C16 113.37(12) . . ?
C16 Ge3 C15 115.01(13) . . ?
O2 Ge2 C3 110.01(10) . . ?
O2 Ge2 C4 95.31(10) . . ?
O2 Ge2 C5 103.82(10) . . ?
C3 Ge2 C4 115.74(14) . . ?
C3 Ge2 C5 116.62(12) . . ?
C5 Ge2 C4 112.39(13) . . ?
O11 S10 N10 112.32(10) . . ?
O11 S10 C24 107.52(11) . . ?
O12 S10 O11 118.34(12) . . ?
O12 S10 N10 107.42(11) . . ?
O12 S10 C24 109.23(11) . . ?
N10 S10 C24 100.51(10) . . ?
O8 S9 N7 111.69(10) . . ?
O8 S9 C17 108.13(12) . . ?
O9 S9 O8 117.82(11) . . ?
O9 S9 N7 104.89(11) . . ?
O9 S9 C17 107.92(11) . . ?
N7 S9 C17 105.70(11) . . ?
P7 P6 P5 97.27(3) . . ?
P1 P6 P7 97.83(3) . . ?
P1 P6 P5 93.85(3) . . ?
P6 P7 P3 103.29(3) . . ?
C2 P7 P6 101.08(7) . . ?
C2 P7 P3 96.25(7) . . ?
P6 P1 P2 104.98(3) . . ?
C1 P1 P6 99.27(7) . . ?
C1 P1 P2 106.78(7) . . ?
P6 P5 P4 103.51(3) . . ?
C13 P5 P6 100.52(7) . . ?
C13 P5 P4 98.03(7) . . ?
O4 S8 N3 111.94(10) . . ?
O4 S8 C6 107.36(11) . . ?
O5 S8 O4 118.71(11) . . ?
O5 S8 N3 106.40(11) . . ?
O5 S8 C6 108.75(11) . . ?
N3 S8 C6 102.45(10) . . ?
P2 P3 P7 100.65(3) . . ?
P4 P3 P7 107.97(3) . . ?
P4 P3 P2 60.62(3) . . ?
P3 P2 P1 106.63(3) . . ?
P3 P2 P4 59.42(3) . . ?
P4 P2 P1 97.23(3) . . ?
P3 P4 P5 100.38(3) . . ?
P3 P4 P2 59.96(3) . . ?
P2 P4 P5 107.45(3) . . ?
C13 O6 Ge3 122.71(14) . . ?
C1 O1 Ge1 120.35(13) . . ?
C2 O2 Ge2 124.94(14) . . ?
C2 N3 S8 123.82(17) . . ?
C13 N7 S9 123.87(17) . . ?
C1 N10 S10 123.98(17) . . ?
O1 C1 P1 111.80(15) . . ?
N10 C1 P1 128.79(17) . . ?
N10 C1 O1 119.10(19) . . ?
O6 C13 P5 112.74(15) . . ?
N7 C13 P5 128.42(17) . . ?
N7 C13 O6 118.8(2) . . ?
O2 C2 P7 111.52(15) . . ?
N3 C2 P7 128.56(17) . . ?
N3 C2 O2 119.9(2) . . ?
Ge1 C31 H31A 109.5 . . ?
Ge1 C31 H31B 109.5 . . ?
Ge1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Ge3 C14 H14A 109.5 . . ?
Ge3 C14 H14B 109.5 . . ?
Ge3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C26 C25 C24 119.0(2) . . ?
C25 C24 S10 120.1(2) . . ?
C29 C24 S10 118.98(18) . . ?
C29 C24 C25 120.9(2) . . ?
Ge1 C32 H32A 109.5 . . ?
Ge1 C32 H32B 109.5 . . ?
Ge1 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Ge1 C33 H33A 109.5 . . ?
Ge1 C33 H33B 109.5 . . ?
Ge1 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.3(2) . . ?
C27 C26 H26 119.4 . . ?
C18 C17 S9 119.8(6) . . ?
C18 C17 C22 118.0(8) . . ?
C22 C17 S9 118.7(4) . . ?
C18A C17 S9 119.4(6) . . ?
C18A C17 C22A 117.5(7) . . ?
C22A C17 S9 119.5(3) . . ?
C7 C6 S8 119.2(2) . . ?
C11 C6 S8 120.4(2) . . ?
C11 C6 C7 120.4(2) . . ?
C26 C27 C30 120.4(2) . . ?
C28 C27 C26 118.5(2) . . ?
C28 C27 C30 121.1(2) . . ?
Ge3 C15 H15A 109.5 . . ?
Ge3 C15 H15B 109.5 . . ?
Ge3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C27 C28 H28 119.5 . . ?
C29 C28 C27 120.9(2) . . ?
C29 C28 H28 119.5 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.8(3) . . ?
C8 C7 H7 120.1 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.1(13) . . ?
C19 C18 H18 120.4 . . ?
C24 C29 H29 120.3 . . ?
C28 C29 C24 119.4(2) . . ?
C28 C29 H29 120.3 . . ?
Ge2 C3 H3A 109.5 . . ?
Ge2 C3 H3B 109.5 . . ?
Ge2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Ge2 C4 H4A 109.5 . . ?
Ge2 C4 H4B 109.5 . . ?
Ge2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C11 H11 120.6 . . ?
C6 C11 C10 118.7(3) . . ?
C10 C11 H11 120.6 . . ?
Ge2 C5 H5A 109.5 . . ?
Ge2 C5 H5B 109.5 . . ?
Ge2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C18 C19 H19 119.0 . . ?
C20 C19 C18 121.9(14) . . ?
C20 C19 H19 119.0 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Ge3 C16 H16A 109.5 . . ?
Ge3 C16 H16B 109.5 . . ?
Ge3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.4 . . ?
C19 C20 C23 121.2(7) . . ?
C19 C20 C21 113.4(10) . . ?
C21 C20 C23 121.3(4) . . ?
C21A C20 C23 119.0(4) . . ?
C19A C20 C23 120.9(6) . . ?
C19A C20 C21A 117.5(7) . . ?
C8 C9 C10 118.6(3) . . ?
C8 C9 C12 120.9(3) . . ?
C10 C9 C12 120.5(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 C11 121.1(3) . . ?
C9 C10 H10 119.4 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C17 C22 H22 121.3 . . ?
C21 C22 C17 117.3(7) . . ?
C21 C22 H22 121.3 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C21 H21 119.6 . . ?
C22 C21 C20 120.8(7) . . ?
C22 C21 H21 119.6 . . ?
C1B O14 C1C 121.0(9) . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C1B C1A H1AA 109.5 . . ?
C1B C1A H1AB 109.5 . . ?
C1B C1A H1AC 109.5 . . ?
O14 C1B C1A 116.2(12) . . ?
O14 C1B H1BA 108.2 . . ?
O14 C1B H1BB 108.2 . . ?
C1A C1B H1BA 108.2 . . ?
C1A C1B H1BB 108.2 . . ?
H1BA C1B H1BB 107.4 . . ?
O14 C1C H1CA 108.6 . . ?
O14 C1C H1CB 108.6 . . ?
H1CA C1C H1CB 107.6 . . ?
C1D C1C O14 114.5(7) . . ?
C1D C1C H1CA 108.6 . . ?
C1D C1C H1CB 108.6 . . ?
C1C C1D H1DA 109.5 . . ?
C1C C1D H1DB 109.5 . . ?
C1C C1D H1DC 109.5 . . ?
H1DA C1D H1DB 109.5 . . ?
H1DA C1D H1DC 109.5 . . ?
H1DB C1D H1DC 109.5 . . ?
C17 C18A H18A 120.1 . . ?
C19A C18A C17 119.7(12) . . ?
C19A C18A H18A 120.1 . . ?
C17 C22A H22A 120.2 . . ?
C21A C22A C17 119.6(5) . . ?
C21A C22A H22A 120.2 . . ?
C20 C21A H21A 120.3 . . ?
C22A C21A C20 119.4(5) . . ?
C22A C21A H21A 120.3 . . ?
C20 C19A C18A 121.4(12) . . ?
C20 C19A H19A 119.3 . . ?
C18A C19A H19A 119.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 O1 C1 P1 -154.14(10) . . . . ?
Ge1 O1 C1 N10 20.1(3) . . . . ?
Ge3 O6 C13 P5 -161.97(9) . . . . ?
Ge3 O6 C13 N7 21.2(3) . . . . ?
Ge2 O2 C2 P7 -170.38(9) . . . . ?
Ge2 O2 C2 N3 12.0(3) . . . . ?
S10 N10 C1 P1 5.4(3) . . . . ?
S10 N10 C1 O1 -167.66(16) . . . . ?
S10 C24 C29 C28 178.6(2) . . . . ?
S9 N7 C13 P5 5.1(3) . . . . ?
S9 N7 C13 O6 -178.59(15) . . . . ?
S9 C17 C18 C19 175.3(17) . . . . ?
S9 C17 C22 C21 -179.4(6) . . . . ?
S9 C17 C18A C19A 178.8(14) . . . . ?
S9 C17 C22A C21A -175.3(5) . . . . ?
P6 P7 C2 O2 106.46(14) . . . . ?
P6 P7 C2 N3 -76.2(2) . . . . ?
P6 P1 C1 O1 -16.04(16) . . . . ?
P6 P1 C1 N10 170.5(2) . . . . ?
P6 P5 C13 O6 98.58(14) . . . . ?
P6 P5 C13 N7 -84.9(2) . . . . ?
S8 N3 C2 P7 -2.1(3) . . . . ?
S8 N3 C2 O2 175.07(15) . . . . ?
S8 C6 C7 C8 178.9(2) . . . . ?
S8 C6 C11 C10 -179.0(2) . . . . ?
P3 P7 C2 O2 1.55(15) . . . . ?
P3 P7 C2 N3 178.9(2) . . . . ?
P2 P1 C1 O1 -124.87(14) . . . . ?
P2 P1 C1 N10 61.6(2) . . . . ?
P4 P5 C13 O6 -6.85(15) . . . . ?
P4 P5 C13 N7 169.66(19) . . . . ?
O4 S8 N3 C2 10.1(2) . . . . ?
O4 S8 C6 C7 -3.6(2) . . . . ?
O4 S8 C6 C11 176.0(2) . . . . ?
O8 S9 N7 C13 31.4(2) . . . . ?
O8 S9 C17 C18 -20.4(11) . . . . ?
O8 S9 C17 C22 -178.8(6) . . . . ?
O8 S9 C17 C18A -7.8(9) . . . . ?
O8 S9 C17 C22A 150.5(5) . . . . ?
O9 S9 N7 C13 160.11(18) . . . . ?
O9 S9 C17 C18 -148.9(11) . . . . ?
O9 S9 C17 C22 52.8(6) . . . . ?
O9 S9 C17 C18A -136.3(9) . . . . ?
O9 S9 C17 C22A 22.1(5) . . . . ?
O11 S10 N10 C1 -1.3(2) . . . . ?
O11 S10 C24 C25 -149.51(19) . . . . ?
O11 S10 C24 C29 33.2(2) . . . . ?
O5 S8 N3 C2 141.32(19) . . . . ?
O5 S8 C6 C7 -133.2(2) . . . . ?
O5 S8 C6 C11 46.3(2) . . . . ?
O12 S10 N10 C1 -133.1(2) . . . . ?
O12 S10 C24 C25 -19.9(2) . . . . ?
O12 S10 C24 C29 162.8(2) . . . . ?
N3 S8 C6 C7 114.5(2) . . . . ?
N3 S8 C6 C11 -66.0(2) . . . . ?
N7 S9 C17 C18 99.3(11) . . . . ?
N7 S9 C17 C22 -59.0(6) . . . . ?
N7 S9 C17 C18A 111.9(9) . . . . ?
N7 S9 C17 C22A -89.7(5) . . . . ?
N10 S10 C24 C25 92.9(2) . . . . ?
N10 S10 C24 C29 -84.4(2) . . . . ?
C14 Ge3 O6 C13 -78.03(18) . . . . ?
C25 C24 C29 C28 1.3(4) . . . . ?
C25 C26 C27 C28 1.3(4) . . . . ?
C25 C26 C27 C30 -178.1(2) . . . . ?
C24 S10 N10 C1 112.7(2) . . . . ?
C24 C25 C26 C27 1.0(4) . . . . ?
C26 C25 C24 S10 -179.61(18) . . . . ?
C26 C25 C24 C29 -2.4(4) . . . . ?
C26 C27 C28 C29 -2.5(4) . . . . ?
C17 S9 N7 C13 -86.0(2) . . . . ?
C17 C18 C19 C20 3(4) . . . . ?
C17 C22 C21 C20 4.5(12) . . . . ?
C17 C18A C19A C20 -4(3) . . . . ?
C17 C22A C21A C20 -2.3(10) . . . . ?
C6 S8 N3 C2 -104.6(2) . . . . ?
C6 C7 C8 C9 0.4(4) . . . . ?
C6 C11 C10 C9 -0.2(5) . . . . ?
C27 C28 C29 C24 1.1(4) . . . . ?
C15 Ge3 O6 C13 46.52(19) . . . . ?
C7 C6 C11 C10 0.5(4) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C7 C8 C9 C12 179.0(3) . . . . ?
C18 C17 C22 C21 21.8(14) . . . . ?
C18 C19 C20 C23 179.9(18) . . . . ?
C18 C19 C20 C21 23(3) . . . . ?
C3 Ge2 O2 C2 -61.5(2) . . . . ?
C4 Ge2 O2 C2 178.62(19) . . . . ?
C11 C6 C7 C8 -0.6(4) . . . . ?
C5 Ge2 O2 C2 63.99(19) . . . . ?
C19 C20 C21 C22 -26.3(19) . . . . ?
C30 C27 C28 C29 177.0(2) . . . . ?
C16 Ge3 O6 C13 165.06(17) . . . . ?
C8 C9 C10 C11 0.0(5) . . . . ?
C12 C9 C10 C11 -179.1(3) . . . . ?
C22 C17 C18 C19 -26(2) . . . . ?
C23 C20 C21 C22 176.3(6) . . . . ?
C23 C20 C21A C22A -179.9(5) . . . . ?
C23 C20 C19A C18A -176.6(14) . . . . ?
C1B O14 C1C C1D 176.7(10) . . . . ?
C1C O14 C1B C1A 178.7(12) . . . . ?
C18A C17 C22A C21A -16.6(13) . . . . ?
C22A C17 C18A C19A 20.0(19) . . . . ?
C21A C20 C19A C18A -15(3) . . . . ?
C19A C20 C21A C22A 18.0(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.732
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_s5984r
_database_code_depnum_ccdc_archive 'CCDC 2202021'
loop_
_audit_author_name
_audit_author_address
'George Whitehead'
;University of Manchester
United Kingdom
;
_audit_update_record             
;
2023-01-19 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_audit_creation_date             2021-11-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H48 As7 N3 O9 S3 Si3'
_chemical_formula_sum            'C33 H48 As7 N3 O9 S3 Si3'
_chemical_formula_weight         1335.63
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.0823(3)
_cell_length_b                   13.5652(3)
_cell_length_c                   14.0438(3)
_cell_angle_alpha                94.859(2)
_cell_angle_beta                 93.493(2)
_cell_angle_gamma                91.697(2)
_cell_volume                     2477.18(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24418
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.5150
_cell_measurement_theta_min      3.1570
_shelx_estimated_absorpt_T_max   0.837
_shelx_estimated_absorpt_T_min   0.539
_exptl_absorpt_coefficient_mu    7.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.024
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32941
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.832
_diffrn_reflns_theta_min         3.165
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00   6.00   1.00    1.00    --    5.00 -34.00 167.00   25
  2  ω    -46.00  -5.00   1.00    1.00    --  -44.02  34.00 -34.00   41
  3  ω    -69.00 -38.00   1.00    1.00    --  -44.02 -34.00 167.00   31
  4  ω   -125.00 -95.00   1.00    1.00    --  -44.02 -34.00 167.00   30
  5  ω    -99.00 -44.00   1.00    1.00    -- -107.20  34.00 -34.00   55
  6  ω   -191.00-164.00   1.00    1.00    -- -107.20 -34.00 167.00   27
  7  ω   -105.00 -67.00   1.00    1.00    -- -107.20 -34.00 167.00   38
  8  ω   -143.00-110.00   1.00    1.00    -- -107.20 -34.00 167.00   33
  9  ω    -11.00  79.00   1.00    1.00    --    5.00  34.00 -34.00   90
 10  ω    -84.00  44.00   1.00    1.00    --  -44.02  37.00  90.00  128
 11  ω    -75.00  44.00   1.00    1.00    --  -44.02  57.00 -60.00  119
 12  ω    -87.00  43.00   1.00    1.00    --  -46.18  76.00 120.00  130
 13  ω    -95.00 -70.00   1.00    1.00    --  -46.18 -34.00 167.00   25
 14  ω    -47.00 -22.00   1.00    1.00    --  -46.18  34.00 -34.00   25
 15  ω   -141.00-109.00   1.00    1.00    -- -107.20  76.00  30.00   32
 16  ω   -148.00 -19.00   1.00    1.00    -- -107.20  76.00 -60.00  129
 17  ω   -197.00 -68.00   1.00    1.00    -- -107.20 -37.00 -60.00  129
 18  ω   -144.00 -18.00   1.00    1.00    -- -107.20  37.00 150.00  126
 19  ω   -110.00 -19.00   1.00    1.00    -- -107.20  76.00 120.00   91
 20  ω   -196.00 -71.00   1.00    1.00    -- -107.20 -37.00-150.00  125
 21  ω   -135.00 -28.00   1.00    1.00    -- -107.20  76.00   0.00  107
 22  ω   -126.00-100.00   1.00    1.00    -- -107.20  76.00-180.00   26
 23  ω   -130.00-103.00   1.00    1.00    -- -107.20  76.00 -90.00   27
 24  ω    -43.00 -18.00   1.00    1.00    -- -107.20  76.00 150.00   25
 25  ω   -186.00-161.00   1.00    1.00    -- -107.20   0.00-150.00   25
 26  ω   -116.00 -90.00   1.00    1.00    -- -107.20  76.00  60.00   26
 27  ω   -155.00-130.00   1.00    1.00    -- -107.20   0.00-150.00   25
 28  ω    -74.00 -37.00   1.00    1.00    -- -107.20   0.00-150.00   37
 29  ω   -126.00 -46.00   1.00    1.00    -- -107.20  76.00-150.00   80
 30  ω   -101.00 -59.00   1.00    1.00    -- -107.20  76.00-120.00   42
 31  ω    -91.00 -54.00   1.00    1.00    -- -107.20  76.00-180.00   37
 32  ω   -107.00 -20.00   1.00    1.00    -- -107.20  76.00  30.00   87
 33  ω   -133.00 -74.00   1.00    1.00    -- -107.20  76.00 150.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0746153000
_diffrn_orient_matrix_UB_12      -0.0905128000
_diffrn_orient_matrix_UB_13      -0.0189840000
_diffrn_orient_matrix_UB_21      -0.0813088000
_diffrn_orient_matrix_UB_22      0.0655566000
_diffrn_orient_matrix_UB_23      -0.0440099000
_diffrn_orient_matrix_UB_31      0.0419216000
_diffrn_orient_matrix_UB_32      -0.0227234000
_diffrn_orient_matrix_UB_33      -0.0993605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9436
_reflns_number_total             9935
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         9935
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0216
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+1.6776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0581
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C6(H6), C20(H20), C17(H17), C28(H28), C10(H10), C32(H32), C31(H31),
 C18(H18), C29(H29), C9(H9), C7(H7)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C13(H13A,H13B,
 H13C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C), C15(H15A,
 H15B,H15C), C22(H22A,H22B,H22C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C3(H3A,H3B,
 H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As4 As 0.20810(2) 0.68326(2) 0.28561(2) 0.01614(5) Uani 1 1 d . . . . .
As7 As 0.35099(2) 0.76816(2) 0.38099(2) 0.01626(5) Uani 1 1 d . . . . .
As5 As 0.26285(2) 0.76945(2) 0.52707(2) 0.01733(5) Uani 1 1 d . . . . .
As6 As 0.45359(2) 0.62395(2) 0.39897(2) 0.01932(5) Uani 1 1 d . . . . .
As1 As 0.15880(2) 0.54791(2) 0.38079(2) 0.01978(5) Uani 1 1 d . . . . .
As3 As 0.32748(2) 0.49731(2) 0.43545(2) 0.02204(6) Uani 1 1 d . . . . .
As2 As 0.22403(2) 0.59438(2) 0.54511(2) 0.02165(6) Uani 1 1 d . . . . .
S2 S 0.30680(4) 0.75023(3) 0.76782(3) 0.01943(9) Uani 1 1 d . . . . .
S1 S 0.14765(4) 0.91033(4) 0.21419(4) 0.02222(10) Uani 1 1 d . . . . .
S3 S 0.58726(4) 0.71294(4) 0.21771(4) 0.02303(10) Uani 1 1 d . . . . .
Si2 Si 0.57326(4) 0.89043(4) 0.62945(4) 0.01867(10) Uani 1 1 d . . . . .
Si3 Si 0.34473(4) 0.46304(4) 0.11531(4) 0.01790(10) Uani 1 1 d . . . . .
Si1 Si -0.06533(4) 0.79545(4) 0.43711(4) 0.02488(12) Uani 1 1 d . . . . .
O4 O 0.46639(10) 0.82967(10) 0.57026(9) 0.0199(3) Uani 1 1 d . . . . .
O7 O 0.37945(10) 0.51457(10) 0.22962(10) 0.0199(3) Uani 1 1 d . . . . .
O5 O 0.20869(11) 0.75267(11) 0.71449(10) 0.0252(3) Uani 1 1 d . . . . .
O6 O 0.33209(12) 0.66095(11) 0.81004(11) 0.0269(3) Uani 1 1 d . . . . .
O2 O 0.25172(11) 0.87792(12) 0.22050(11) 0.0274(3) Uani 1 1 d . . . . .
O1 O 0.03476(11) 0.73892(10) 0.38223(10) 0.0222(3) Uani 1 1 d . . . . .
O8 O 0.59379(12) 0.74616(11) 0.31837(11) 0.0299(3) Uani 1 1 d . . . . .
O9 O 0.56815(12) 0.78430(11) 0.14993(12) 0.0316(3) Uani 1 1 d . . . . .
O3 O 0.13120(13) 1.01459(11) 0.22559(12) 0.0314(3) Uani 1 1 d . . . . .
N2 N 0.40194(12) 0.78094(12) 0.70419(12) 0.0196(3) Uani 1 1 d . . . . .
N1 N 0.07837(13) 0.86172(13) 0.29331(13) 0.0221(3) Uani 1 1 d . . . . .
N3 N 0.50180(13) 0.62176(13) 0.19225(12) 0.0220(3) Uani 1 1 d . . . . .
C12 C 0.38944(14) 0.79271(14) 0.61454(14) 0.0180(4) Uani 1 1 d . . . . .
C16 C 0.31503(15) 0.84947(14) 0.85643(14) 0.0191(4) Uani 1 1 d . . . . .
C21 C 0.37514(15) 0.84296(15) 0.94079(14) 0.0203(4) Uani 1 1 d . . . . .
H21 H 0.410219 0.784194 0.951556 0.024 Uiso 1 1 calc R U . . .
C6 C 0.14229(16) 0.79105(15) 0.04773(15) 0.0240(4) Uani 1 1 d . . . . .
H6 H 0.204112 0.765405 0.072886 0.029 Uiso 1 1 calc R U . . .
C1 C 0.09727(14) 0.77662(14) 0.32337(14) 0.0186(4) Uani 1 1 d . . . . .
C30 C 0.89022(15) 0.57109(15) 0.15830(14) 0.0224(4) Uani 1 1 d . . . . .
C20 C 0.38306(15) 0.92354(15) 1.00893(14) 0.0214(4) Uani 1 1 d . . . . .
H20 H 0.424003 0.919693 1.066643 0.026 Uiso 1 1 calc R U . . .
C23 C 0.44836(15) 0.58643(14) 0.25626(14) 0.0198(4) Uani 1 1 d . . . . .
C19 C 0.33186(16) 1.00998(15) 0.99390(15) 0.0223(4) Uani 1 1 d . . . . .
C27 C 0.70221(15) 0.65406(15) 0.19136(14) 0.0213(4) Uani 1 1 d . . . . .
C17 C 0.26259(16) 0.93459(15) 0.83993(15) 0.0235(4) Uani 1 1 d . . . . .
H17 H 0.221261 0.938208 0.782407 0.028 Uiso 1 1 calc R U . . .
C8 C 0.01262(16) 0.79700(15) -0.08274(16) 0.0244(4) Uani 1 1 d . . . . .
C26 C 0.23666(15) 0.37984(15) 0.14124(15) 0.0232(4) Uani 1 1 d . . . . .
H26A H 0.260424 0.334907 0.188342 0.035 Uiso 1 1 calc R U . . .
H26B H 0.210858 0.341180 0.082092 0.035 Uiso 1 1 calc R U . . .
H26C H 0.181604 0.419504 0.166962 0.035 Uiso 1 1 calc R U . . .
C28 C 0.73032(17) 0.57057(16) 0.23606(16) 0.0263(4) Uani 1 1 d . . . . .
H28 H 0.686080 0.542215 0.278311 0.032 Uiso 1 1 calc R U . . .
C10 C -0.00127(15) 0.89773(15) 0.06701(16) 0.0241(4) Uani 1 1 d . . . . .
H10 H -0.037599 0.943965 0.105466 0.029 Uiso 1 1 calc R U . . .
C32 C 0.76653(16) 0.69633(15) 0.13022(15) 0.0242(4) Uani 1 1 d . . . . .
H32 H 0.746443 0.752863 0.099132 0.029 Uiso 1 1 calc R U . . .
C14 C 0.65162(17) 0.79769(16) 0.68641(16) 0.0271(4) Uani 1 1 d . . . . .
H14A H 0.616196 0.773829 0.739978 0.041 Uiso 1 1 calc R U . . .
H14B H 0.718196 0.828147 0.710157 0.041 Uiso 1 1 calc R U . . .
H14C H 0.661997 0.741961 0.639274 0.041 Uiso 1 1 calc R U . . .
C5 C 0.09095(15) 0.86145(15) 0.10232(15) 0.0213(4) Uani 1 1 d . . . . .
C25 C 0.29980(16) 0.56108(15) 0.04009(15) 0.0234(4) Uani 1 1 d . . . . .
H25A H 0.234887 0.585686 0.062199 0.035 Uiso 1 1 calc R U . . .
H25B H 0.289615 0.533704 -0.026782 0.035 Uiso 1 1 calc R U . . .
H25C H 0.351160 0.615653 0.045106 0.035 Uiso 1 1 calc R U . . .
C31 C 0.86076(16) 0.65519(16) 0.11480(15) 0.0244(4) Uani 1 1 d . . . . .
H31 H 0.905727 0.684864 0.073999 0.029 Uiso 1 1 calc R U . . .
C13 C 0.52719(16) 0.99045(15) 0.71178(15) 0.0230(4) Uani 1 1 d . . . . .
H13A H 0.483719 1.033576 0.675481 0.035 Uiso 1 1 calc R U . . .
H13B H 0.585950 1.029270 0.743423 0.035 Uiso 1 1 calc R U . . .
H13C H 0.487457 0.961606 0.760128 0.035 Uiso 1 1 calc R U . . .
C18 C 0.27176(16) 1.01401(15) 0.90893(15) 0.0250(4) Uani 1 1 d . . . . .
H18 H 0.236311 1.072573 0.898172 0.030 Uiso 1 1 calc R U . . .
C24 C 0.45467(17) 0.39373(16) 0.07258(16) 0.0279(4) Uani 1 1 d . . . . .
H24A H 0.513631 0.439485 0.069997 0.042 Uiso 1 1 calc R U . . .
H24B H 0.436633 0.361314 0.008477 0.042 Uiso 1 1 calc R U . . .
H24C H 0.472166 0.343555 0.116568 0.042 Uiso 1 1 calc R U . . .
C29 C 0.82347(17) 0.52910(16) 0.21843(16) 0.0271(4) Uani 1 1 d . . . . .
H29 H 0.842180 0.471117 0.247779 0.032 Uiso 1 1 calc R U . . .
C9 C -0.03912(16) 0.86526(15) -0.02514(16) 0.0256(4) Uani 1 1 d . . . . .
H9 H -0.101687 0.890076 -0.049549 0.031 Uiso 1 1 calc R U . . .
C7 C 0.10264(16) 0.75832(16) -0.04400(16) 0.0247(4) Uani 1 1 d . . . . .
H7 H 0.136981 0.709134 -0.080864 0.030 Uiso 1 1 calc R U . . .
C11 C -0.02364(17) 0.76972(18) -0.18521(16) 0.0302(5) Uani 1 1 d . . . . .
H11A H -0.093948 0.791153 -0.196182 0.045 Uiso 1 1 calc R U . . .
H11B H -0.021884 0.697791 -0.199160 0.045 Uiso 1 1 calc R U . . .
H11C H 0.021209 0.802381 -0.227259 0.045 Uiso 1 1 calc R U . . .
C33 C 0.99062(16) 0.52430(17) 0.13872(17) 0.0291(5) Uani 1 1 d . . . . .
H33A H 0.978987 0.468964 0.089304 0.044 Uiso 1 1 calc R U . . .
H33B H 1.020396 0.499872 0.197615 0.044 Uiso 1 1 calc R U . . .
H33C H 1.037819 0.573611 0.116510 0.044 Uiso 1 1 calc R U . . .
C15 C 0.63901(17) 0.93819(17) 0.52868(16) 0.0281(4) Uani 1 1 d . . . . .
H15A H 0.642033 0.885168 0.477114 0.042 Uiso 1 1 calc R U . . .
H15B H 0.708727 0.961477 0.550895 0.042 Uiso 1 1 calc R U . . .
H15C H 0.601058 0.993198 0.504749 0.042 Uiso 1 1 calc R U . . .
C22 C 0.34076(18) 1.09725(16) 1.06803(17) 0.0299(5) Uani 1 1 d . . . . .
H22A H 0.296175 1.085348 1.119780 0.045 Uiso 1 1 calc R U . . .
H22B H 0.319961 1.156993 1.038403 0.045 Uiso 1 1 calc R U . . .
H22C H 0.411930 1.106197 1.094151 0.045 Uiso 1 1 calc R U . . .
C2 C -0.14398(17) 0.8633(2) 0.35191(18) 0.0348(5) Uani 1 1 d . . . . .
H2A H -0.111306 0.928320 0.346186 0.052 Uiso 1 1 calc R U . . .
H2B H -0.212435 0.872035 0.375403 0.052 Uiso 1 1 calc R U . . .
H2C H -0.149823 0.825538 0.289064 0.052 Uiso 1 1 calc R U . . .
C4 C -0.0058(2) 0.87388(18) 0.54132(17) 0.0349(5) Uani 1 1 d . . . . .
H4A H 0.031741 0.832288 0.584228 0.052 Uiso 1 1 calc R U . . .
H4B H -0.059305 0.907920 0.575808 0.052 Uiso 1 1 calc R U . . .
H4C H 0.041682 0.922927 0.519092 0.052 Uiso 1 1 calc R U . . .
C3 C -0.1362(2) 0.6869(2) 0.4749(2) 0.0485(7) Uani 1 1 d . . . . .
H3A H -0.162674 0.644685 0.418114 0.073 Uiso 1 1 calc R U . . .
H3B H -0.193477 0.709375 0.512013 0.073 Uiso 1 1 calc R U . . .
H3C H -0.090077 0.649231 0.514424 0.073 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As4 As7 2.4334(3) . ?
As4 As1 2.4545(3) . ?
As4 C1 2.0189(19) . ?
As7 As5 2.4129(3) . ?
As7 As6 2.4271(3) . ?
As5 As2 2.4512(3) . ?
As5 C12 2.0016(19) . ?
As6 As3 2.4535(3) . ?
As6 C23 2.022(2) . ?
As1 As3 2.4294(3) . ?
As1 As2 2.4357(3) . ?
As3 As2 2.4399(3) . ?
S2 O5 1.4488(15) . ?
S2 O6 1.4316(15) . ?
S2 N2 1.6399(17) . ?
S2 C16 1.750(2) . ?
S1 O2 1.4429(15) . ?
S1 O3 1.4339(16) . ?
S1 N1 1.6439(18) . ?
S1 C5 1.764(2) . ?
S3 O8 1.4435(16) . ?
S3 O9 1.4309(17) . ?
S3 N3 1.6438(17) . ?
S3 C27 1.768(2) . ?
Si2 O4 1.7317(14) . ?
Si2 C14 1.849(2) . ?
Si2 C13 1.846(2) . ?
Si2 C15 1.853(2) . ?
Si3 O7 1.7246(14) . ?
Si3 C26 1.856(2) . ?
Si3 C25 1.854(2) . ?
Si3 C24 1.845(2) . ?
Si1 O1 1.7260(15) . ?
Si1 C2 1.852(3) . ?
Si1 C4 1.852(2) . ?
Si1 C3 1.849(3) . ?
O4 C12 1.323(2) . ?
O7 C23 1.322(2) . ?
O1 C1 1.320(2) . ?
N2 C12 1.284(3) . ?
N1 C1 1.288(3) . ?
N3 C23 1.287(3) . ?
C16 C21 1.392(3) . ?
C16 C17 1.389(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.388(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.388(3) . ?
C6 C7 1.391(3) . ?
C30 C31 1.392(3) . ?
C30 C29 1.394(3) . ?
C30 C33 1.506(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.393(3) . ?
C19 C18 1.394(3) . ?
C19 C22 1.506(3) . ?
C27 C28 1.389(3) . ?
C27 C32 1.384(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(3) . ?
C8 C9 1.395(3) . ?
C8 C7 1.402(3) . ?
C8 C11 1.500(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28 0.9500 . ?
C28 C29 1.384(3) . ?
C10 H10 0.9500 . ?
C10 C5 1.395(3) . ?
C10 C9 1.388(3) . ?
C32 H32 0.9500 . ?
C32 C31 1.390(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C31 H31 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C18 H18 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C29 H29 0.9500 . ?
C9 H9 0.9500 . ?
C7 H7 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
As7 As4 As1 103.828(10) . . ?
C1 As4 As7 98.18(5) . . ?
C1 As4 As1 97.63(6) . . ?
As5 As7 As4 93.023(10) . . ?
As5 As7 As6 99.256(10) . . ?
As6 As7 As4 96.962(10) . . ?
As7 As5 As2 104.458(11) . . ?
C12 As5 As7 95.33(6) . . ?
C12 As5 As2 100.63(5) . . ?
As7 As6 As3 103.133(11) . . ?
C23 As6 As7 93.01(5) . . ?
C23 As6 As3 96.21(6) . . ?
As3 As1 As4 99.826(11) . . ?
As3 As1 As2 60.201(9) . . ?
As2 As1 As4 106.964(10) . . ?
As1 As3 As6 107.981(11) . . ?
As1 As3 As2 60.028(9) . . ?
As2 As3 As6 100.779(10) . . ?
As1 As2 As5 97.385(10) . . ?
As1 As2 As3 59.771(9) . . ?
As3 As2 As5 107.262(11) . . ?
O5 S2 N2 111.84(9) . . ?
O5 S2 C16 108.16(9) . . ?
O6 S2 O5 117.95(9) . . ?
O6 S2 N2 107.90(9) . . ?
O6 S2 C16 109.47(9) . . ?
N2 S2 C16 100.00(9) . . ?
O2 S1 N1 111.56(9) . . ?
O2 S1 C5 107.37(10) . . ?
O3 S1 O2 118.18(10) . . ?
O3 S1 N1 105.42(9) . . ?
O3 S1 C5 108.89(9) . . ?
N1 S1 C5 104.59(9) . . ?
O8 S3 N3 111.78(9) . . ?
O8 S3 C27 108.05(10) . . ?
O9 S3 O8 118.42(10) . . ?
O9 S3 N3 107.19(9) . . ?
O9 S3 C27 108.40(10) . . ?
N3 S3 C27 101.67(9) . . ?
O4 Si2 C14 108.22(9) . . ?
O4 Si2 C13 107.31(8) . . ?
O4 Si2 C15 101.55(9) . . ?
C14 Si2 C15 110.52(11) . . ?
C13 Si2 C14 115.60(10) . . ?
C13 Si2 C15 112.55(10) . . ?
O7 Si3 C26 99.75(8) . . ?
O7 Si3 C25 109.56(8) . . ?
O7 Si3 C24 107.28(9) . . ?
C25 Si3 C26 111.09(9) . . ?
C24 Si3 C26 112.22(10) . . ?
C24 Si3 C25 115.65(10) . . ?
O1 Si1 C2 111.29(9) . . ?
O1 Si1 C4 105.67(10) . . ?
O1 Si1 C3 100.94(10) . . ?
C4 Si1 C2 114.45(12) . . ?
C3 Si1 C2 111.94(14) . . ?
C3 Si1 C4 111.54(14) . . ?
C12 O4 Si2 123.61(12) . . ?
C23 O7 Si3 128.08(13) . . ?
C1 O1 Si1 127.87(13) . . ?
C12 N2 S2 122.38(14) . . ?
C1 N1 S1 121.90(15) . . ?
C23 N3 S3 122.52(15) . . ?
O4 C12 As5 111.70(13) . . ?
N2 C12 As5 129.00(15) . . ?
N2 C12 O4 119.21(17) . . ?
C21 C16 S2 119.93(15) . . ?
C17 C16 S2 118.87(15) . . ?
C17 C16 C21 121.19(18) . . ?
C16 C21 H21 120.5 . . ?
C20 C21 C16 119.03(18) . . ?
C20 C21 H21 120.5 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.57(19) . . ?
C7 C6 H6 120.2 . . ?
O1 C1 As4 112.47(13) . . ?
N1 C1 As4 128.53(15) . . ?
N1 C1 O1 118.86(18) . . ?
C31 C30 C29 118.64(19) . . ?
C31 C30 C33 120.93(19) . . ?
C29 C30 C33 120.40(19) . . ?
C21 C20 H20 119.5 . . ?
C21 C20 C19 120.94(18) . . ?
C19 C20 H20 119.5 . . ?
O7 C23 As6 111.93(14) . . ?
N3 C23 As6 129.22(15) . . ?
N3 C23 O7 118.84(18) . . ?
C20 C19 C18 118.67(18) . . ?
C20 C19 C22 120.74(19) . . ?
C18 C19 C22 120.59(19) . . ?
C28 C27 S3 120.39(16) . . ?
C32 C27 S3 118.75(16) . . ?
C32 C27 C28 120.74(19) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.71(19) . . ?
C18 C17 H17 120.6 . . ?
C9 C8 C7 118.3(2) . . ?
C9 C8 C11 121.01(19) . . ?
C7 C8 C11 120.6(2) . . ?
Si3 C26 H26A 109.5 . . ?
Si3 C26 H26B 109.5 . . ?
Si3 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.34(19) . . ?
C29 C28 H28 120.3 . . ?
C5 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C5 119.0(2) . . ?
C27 C32 H32 120.3 . . ?
C27 C32 C31 119.31(19) . . ?
C31 C32 H32 120.3 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C5 S1 119.10(15) . . ?
C6 C5 C10 120.7(2) . . ?
C10 C5 S1 120.11(17) . . ?
Si3 C25 H25A 109.5 . . ?
Si3 C25 H25B 109.5 . . ?
Si3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 120.93(19) . . ?
C32 C31 H31 119.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C18 H18 119.3 . . ?
C17 C18 C19 121.46(19) . . ?
C17 C18 H18 119.3 . . ?
Si3 C24 H24A 109.5 . . ?
Si3 C24 H24B 109.5 . . ?
Si3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C29 H29 119.5 . . ?
C28 C29 C30 121.0(2) . . ?
C28 C29 H29 119.5 . . ?
C8 C9 H9 119.2 . . ?
C10 C9 C8 121.51(19) . . ?
C10 C9 H9 119.2 . . ?
C6 C7 C8 120.8(2) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 N2 C12 As5 -4.9(3) . . . . ?
S2 N2 C12 O4 171.41(13) . . . . ?
S2 C16 C21 C20 178.11(15) . . . . ?
S2 C16 C17 C18 -178.08(16) . . . . ?
S1 N1 C1 As4 -0.4(3) . . . . ?
S1 N1 C1 O1 -175.67(14) . . . . ?
S3 N3 C23 As6 -2.2(3) . . . . ?
S3 N3 C23 O7 178.45(13) . . . . ?
S3 C27 C28 C29 -176.31(17) . . . . ?
S3 C27 C32 C31 175.00(16) . . . . ?
Si2 O4 C12 As5 161.06(9) . . . . ?
Si2 O4 C12 N2 -15.8(2) . . . . ?
Si3 O7 C23 As6 176.86(9) . . . . ?
Si3 O7 C23 N3 -3.7(3) . . . . ?
Si1 O1 C1 As4 176.09(9) . . . . ?
Si1 O1 C1 N1 -7.9(3) . . . . ?
O5 S2 N2 C12 -8.30(19) . . . . ?
O5 S2 C16 C21 152.29(16) . . . . ?
O5 S2 C16 C17 -29.05(19) . . . . ?
O6 S2 N2 C12 123.02(16) . . . . ?
O6 S2 C16 C21 22.56(19) . . . . ?
O6 S2 C16 C17 -158.79(16) . . . . ?
O2 S1 N1 C1 -29.2(2) . . . . ?
O2 S1 C5 C6 10.39(18) . . . . ?
O2 S1 C5 C10 -165.76(16) . . . . ?
O8 S3 N3 C23 0.2(2) . . . . ?
O8 S3 C27 C28 60.99(19) . . . . ?
O8 S3 C27 C32 -114.93(17) . . . . ?
O9 S3 N3 C23 -131.10(17) . . . . ?
O9 S3 C27 C28 -169.53(17) . . . . ?
O9 S3 C27 C32 14.56(19) . . . . ?
O3 S1 N1 C1 -158.72(17) . . . . ?
O3 S1 C5 C6 139.45(16) . . . . ?
O3 S1 C5 C10 -36.70(19) . . . . ?
N2 S2 C16 C21 -90.61(17) . . . . ?
N2 S2 C16 C17 88.04(17) . . . . ?
N1 S1 C5 C6 -108.25(16) . . . . ?
N1 S1 C5 C10 75.60(18) . . . . ?
N3 S3 C27 C28 -56.77(19) . . . . ?
N3 S3 C27 C32 127.31(17) . . . . ?
C16 S2 N2 C12 -122.61(17) . . . . ?
C16 C21 C20 C19 0.1(3) . . . . ?
C16 C17 C18 C19 -0.2(3) . . . . ?
C21 C16 C17 C18 0.6(3) . . . . ?
C21 C20 C19 C18 0.3(3) . . . . ?
C21 C20 C19 C22 -180.0(2) . . . . ?
C20 C19 C18 C17 -0.3(3) . . . . ?
C27 S3 N3 C23 115.25(17) . . . . ?
C27 C28 C29 C30 1.4(3) . . . . ?
C27 C32 C31 C30 1.4(3) . . . . ?
C17 C16 C21 C20 -0.5(3) . . . . ?
C26 Si3 O7 C23 -174.21(16) . . . . ?
C28 C27 C32 C31 -0.9(3) . . . . ?
C32 C27 C28 C29 -0.5(3) . . . . ?
C14 Si2 O4 C12 71.70(17) . . . . ?
C5 S1 N1 C1 86.52(18) . . . . ?
C5 C6 C7 C8 1.3(3) . . . . ?
C5 C10 C9 C8 0.3(3) . . . . ?
C25 Si3 O7 C23 -57.56(17) . . . . ?
C31 C30 C29 C28 -1.0(3) . . . . ?
C13 Si2 O4 C12 -53.67(17) . . . . ?
C24 Si3 O7 C23 68.71(18) . . . . ?
C29 C30 C31 C32 -0.5(3) . . . . ?
C9 C8 C7 C6 -3.4(3) . . . . ?
C9 C10 C5 S1 173.62(15) . . . . ?
C9 C10 C5 C6 -2.5(3) . . . . ?
C7 C6 C5 S1 -174.47(15) . . . . ?
C7 C6 C5 C10 1.7(3) . . . . ?
C7 C8 C9 C10 2.5(3) . . . . ?
C11 C8 C9 C10 -174.17(19) . . . . ?
C11 C8 C7 C6 173.35(19) . . . . ?
C33 C30 C31 C32 177.71(19) . . . . ?
C33 C30 C29 C28 -179.1(2) . . . . ?
C15 Si2 O4 C12 -171.94(16) . . . . ?
C22 C19 C18 C17 180.0(2) . . . . ?
C2 Si1 O1 C1 44.59(19) . . . . ?
C4 Si1 O1 C1 -80.20(18) . . . . ?
C3 Si1 O1 C1 163.53(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.755
