# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_1010b
#[NbCl4{o-C6H4(PMe2)2}2] Cl.CH3CN

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 Cl4 Nb P4, C2 H3 N, Cl'
_chemical_formula_sum            'C22 H35 Cl5 N Nb P4'
_chemical_formula_weight         707.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.764(6)
_cell_length_b                   10.178(2)
_cell_length_c                   14.770(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.431(9)
_cell_angle_gamma                90
_cell_volume                     3085.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5934
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      34.6

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.044
_shelx_estimated_absorpt_T_min   0.885
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            9182
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.845
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3191
_reflns_number_gt                2992
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 2013)'

_refine_special_details          
;
The acetonitrile is disordered and lies very nearly in a mirror plane. 
It was modelled in 2 parts with adp?s for all atoms constrained to be 
the same and the geometry of the 2 parts restrained to be the same 
(shelx default esd). 

All hydrogens were placed in calculated positions and refined using a 
riding model. ADPS were set at 1.2 (CHar), 1.5(CH3) that of the parent 
atoms. CH3 torsion angles were allowed to refine.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+4.0161P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3191
_refine_ls_number_parameters     180
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0663
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001

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
Nb1 Nb 0.58546(2) 0.0000 0.28880(2) 0.01233(6) Uani 1 2 d S T P . .
Cl1 Cl 0.53644(3) 0.0000 0.41460(5) 0.01829(16) Uani 1 2 d S T P . .
Cl2 Cl 0.56508(3) 0.0000 0.11590(5) 0.01672(15) Uani 1 2 d S T P . .
Cl3 Cl 0.62027(2) -0.22844(5) 0.31212(3) 0.01690(11) Uani 1 1 d . . . . .
Cl4 Cl 0.14320(3) 0.0000 -0.13259(5) 0.01762(16) Uani 1 2 d S T P . .
P1 P 0.67920(4) 0.0000 0.46148(5) 0.01454(16) Uani 1 2 d S T P . .
P2 P 0.70000(4) 0.0000 0.25685(5) 0.01332(16) Uani 1 2 d S T P . .
P3 P 0.48078(2) 0.15555(5) 0.21859(4) 0.01477(12) Uani 1 1 d . . . . .
C1 C 0.67883(10) -0.1401(2) 0.53814(14) 0.0206(5) Uani 1 1 d . . . . .
H1A H 0.6871 -0.2208 0.5079 0.031 Uiso 1 1 calc R U . . .
H1B H 0.6363 -0.1462 0.5471 0.031 Uiso 1 1 calc R U . . .
H1C H 0.7129 -0.1286 0.6006 0.031 Uiso 1 1 calc R U . . .
C2 C 0.76148(13) 0.0000 0.4555(2) 0.0138(6) Uani 1 2 d S T P . .
C3 C 0.81537(14) 0.0000 0.5397(2) 0.0178(7) Uani 1 2 d S T P . .
H3 H 0.8093 0.0000 0.6004 0.021 Uiso 1 2 calc R U P . .
C4 C 0.87792(15) 0.0000 0.5343(2) 0.0193(7) Uani 1 2 d S T P . .
H4 H 0.9146 0.0000 0.5915 0.023 Uiso 1 2 calc R U P . .
C5 C 0.88688(15) 0.0000 0.4460(2) 0.0221(7) Uani 1 2 d S T P . .
H5 H 0.9298 0.0000 0.4429 0.027 Uiso 1 2 calc R U P . .
C6 C 0.83370(14) 0.0000 0.3617(2) 0.0206(7) Uani 1 2 d S T P . .
H6 H 0.8402 0.0000 0.3012 0.025 Uiso 1 2 calc R U P . .
C7 C 0.77048(14) 0.0000 0.3665(2) 0.0149(6) Uani 1 2 d S T P . .
C8 C 0.71468(10) -0.1395(2) 0.19013(15) 0.0184(5) Uani 1 1 d . . . . .
H8A H 0.7549 -0.1250 0.1755 0.028 Uiso 1 1 calc R U . . .
H8B H 0.6781 -0.1493 0.1301 0.028 Uiso 1 1 calc R U . . .
H8C H 0.7190 -0.2195 0.2287 0.028 Uiso 1 1 calc R U . . .
C9 C 0.46234(10) 0.2602(2) 0.30632(15) 0.0218(5) Uani 1 1 d . . . . .
H9A H 0.5020 0.3058 0.3452 0.033 Uiso 1 1 calc R U . . .
H9B H 0.4458 0.2062 0.3481 0.033 Uiso 1 1 calc R U . . .
H9C H 0.4293 0.3250 0.2729 0.033 Uiso 1 1 calc R U . . .
C10 C 0.48487(10) 0.2705(2) 0.12668(15) 0.0232(5) Uani 1 1 d . . . . .
H10A H 0.4801 0.2227 0.0672 0.035 Uiso 1 1 calc R U . . .
H10B H 0.5270 0.3158 0.1482 0.035 Uiso 1 1 calc R U . . .
H10C H 0.4497 0.3351 0.1151 0.035 Uiso 1 1 calc R U . . .
C11 C 0.40508(9) 0.06875(19) 0.16032(13) 0.0158(5) Uani 1 1 d . . . . .
C12 C 0.34746(10) 0.1379(2) 0.11360(15) 0.0216(5) Uani 1 1 d . . . . .
H12 H 0.3470 0.2312 0.1145 0.026 Uiso 1 1 calc R U . . .
C13 C 0.29114(10) 0.0680(2) 0.06601(15) 0.0232(5) Uani 1 1 d . . . . .
H13 H 0.2521 0.1141 0.0331 0.028 Uiso 1 1 calc R U . . .
N1A N 0.7767(3) 0.006(3) 0.7515(5) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
C14A C 0.8204(4) 0.009(2) 0.8182(6) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
C15A C 0.8782(4) 0.0230(11) 0.9083(6) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
H15A H 0.8926 0.1148 0.9161 0.039 Uiso 0.220(5) 1 calc R U P A -1
H15B H 0.9137 -0.0330 0.9038 0.039 Uiso 0.220(5) 1 calc R U P A -1
H15C H 0.8659 -0.0039 0.9636 0.039 Uiso 0.220(5) 1 calc R U P A -1
N1B N 0.7933(3) 0.0150(10) 0.7561(4) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
C14B C 0.8326(3) 0.002(5) 0.8268(4) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
C15B C 0.8816(4) -0.0495(8) 0.9167(6) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
H15D H 0.8889 -0.1432 0.9091 0.039 Uiso 0.280(5) 1 calc R U P A -2
H15E H 0.8654 -0.0372 0.9706 0.039 Uiso 0.280(5) 1 calc R U P A -2
H15F H 0.9227 -0.0016 0.9294 0.039 Uiso 0.280(5) 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
Nb1 Cl1 2.4309(9) . ?
Nb1 Cl3 2.4341(6) . ?
Nb1 Cl3 2.4341(6) 6 ?
Nb1 Cl2 2.4424(10) . ?
Nb1 P3 2.6833(7) 6 ?
Nb1 P3 2.6833(7) . ?
Nb1 P1 2.6843(10) . ?
Nb1 P2 2.6869(10) . ?
P1 C1 1.822(2) 6 ?
P1 C1 1.822(2) . ?
P1 C2 1.822(3) . ?
P2 C8 1.816(2) . ?
P2 C8 1.816(2) 6 ?
P2 C7 1.823(3) . ?
P3 C11 1.815(2) . ?
P3 C10 1.817(2) . ?
P3 C9 1.822(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.392(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.389(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.401(4) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C11 1.400(4) 6 ?
C11 C12 1.403(3) . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 C13 1.384(4) 6 ?
C13 H13 0.9500 . ?
N1A C14A 1.120(8) . ?
C14A C15A 1.502(10) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
N1B C14B 1.116(8) . ?
C14B C15B 1.493(16) . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 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
Cl1 Nb1 Cl3 94.989(16) . . ?
Cl1 Nb1 Cl3 94.989(16) . 6 ?
Cl3 Nb1 Cl3 145.57(3) . 6 ?
Cl1 Nb1 Cl2 145.69(3) . . ?
Cl3 Nb1 Cl2 95.029(14) . . ?
Cl3 Nb1 Cl2 95.028(14) 6 . ?
Cl1 Nb1 P3 76.31(2) . 6 ?
Cl3 Nb1 P3 71.06(2) . 6 ?
Cl3 Nb1 P3 143.373(18) 6 6 ?
Cl2 Nb1 P3 76.14(2) . 6 ?
Cl1 Nb1 P3 76.31(2) . . ?
Cl3 Nb1 P3 143.376(18) . . ?
Cl3 Nb1 P3 71.06(2) 6 . ?
Cl2 Nb1 P3 76.14(2) . . ?
P3 Nb1 P3 72.32(3) 6 . ?
Cl1 Nb1 P1 70.24(3) . . ?
Cl3 Nb1 P1 76.299(14) . . ?
Cl3 Nb1 P1 76.300(14) 6 . ?
Cl2 Nb1 P1 144.08(3) . . ?
P3 Nb1 P1 130.272(19) 6 . ?
P3 Nb1 P1 130.272(19) . . ?
Cl1 Nb1 P2 143.41(3) . . ?
Cl3 Nb1 P2 76.203(15) . . ?
Cl3 Nb1 P2 76.205(15) 6 . ?
Cl2 Nb1 P2 70.90(3) . . ?
P3 Nb1 P2 130.55(2) 6 . ?
P3 Nb1 P2 130.55(2) . . ?
P1 Nb1 P2 73.18(3) . . ?
C1 P1 C1 102.96(14) 6 . ?
C1 P1 C2 103.76(9) 6 . ?
C1 P1 C2 103.76(9) . . ?
C1 P1 Nb1 115.55(7) 6 . ?
C1 P1 Nb1 115.55(7) . . ?
C2 P1 Nb1 113.72(9) . . ?
C8 P2 C8 102.84(14) . 6 ?
C8 P2 C7 103.53(9) . . ?
C8 P2 C7 103.53(9) 6 . ?
C8 P2 Nb1 115.87(7) . . ?
C8 P2 Nb1 115.86(7) 6 . ?
C7 P2 Nb1 113.58(10) . . ?
C11 P3 C10 102.80(9) . . ?
C11 P3 C9 104.00(10) . . ?
C10 P3 C9 103.41(10) . . ?
C11 P3 Nb1 114.60(7) . . ?
C10 P3 Nb1 114.99(7) . . ?
C9 P3 Nb1 115.44(7) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 120.0(3) . . ?
C7 C2 P1 119.7(2) . . ?
C3 C2 P1 120.3(2) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.6(3) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C2 C7 C6 119.8(3) . . ?
C2 C7 P2 119.8(2) . . ?
C6 C7 P2 120.4(2) . . ?
P2 C8 H8A 109.5 . . ?
P2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P3 C10 H10A 109.5 . . ?
P3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 C11 C12 120.10(12) 6 . ?
C11 C11 P3 119.13(6) 6 . ?
C12 C11 P3 120.75(16) . . ?
C13 C12 C11 119.1(2) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C13 C13 C12 120.80(13) 6 . ?
C13 C13 H13 119.6 6 . ?
C12 C13 H13 119.6 . . ?
N1A C14A C15A 176(2) . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
N1B C14B C15B 166(4) . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?

_refine_diff_density_max         0.473
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 993845'
#######################################################################
#
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#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_2011kwl0108


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 As4 Cl4 Nb, C2 H5 Cl5 Nb O'
_chemical_formula_sum            'C22 H37 As4 Cl9 Nb2 O'
_chemical_formula_weight         1122.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.144(2)
_cell_length_b                   12.638(3)
_cell_length_c                   14.139(3)
_cell_angle_alpha                108.806(2)
_cell_angle_beta                 108.034(2)
_cell_angle_gamma                102.051(2)
_cell_volume                     1834.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4757
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      31.6

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.878
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_process_details   
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            15852
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.619
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7172
_reflns_number_gt                5780
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 2013)'

_refine_special_details          
;
 All hydrogens were placed in calculated positions and refined using a 
 riding model. ADPS were set at 1.2 (CHar, CH2), 1.5(CH3) that of the 
 parent atoms. CH3 torsion angles were allowed to refine.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7172
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0795
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.958
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.25282(4) 0.38707(3) 0.14615(3) 0.01553(9) Uani 1 1 d . . . . .
As1 As 0.48781(4) 0.39371(4) 0.24397(4) 0.01661(10) Uani 1 1 d . . . . .
As2 As 0.40843(4) 0.59517(4) 0.17052(4) 0.02008(11) Uani 1 1 d . . . . .
As3 As 0.05621(4) 0.33992(4) 0.20219(4) 0.01751(10) Uani 1 1 d . . . . .
As4 As 0.05760(4) 0.21529(4) -0.03751(4) 0.01866(11) Uani 1 1 d . . . . .
Cl1 Cl 0.31675(10) 0.32597(9) -0.00441(9) 0.0226(2) Uani 1 1 d . . . . .
Cl2 Cl 0.31428(10) 0.51760(9) 0.33597(8) 0.0200(2) Uani 1 1 d . . . . .
Cl3 Cl 0.13250(10) 0.49686(9) 0.07612(9) 0.0226(2) Uani 1 1 d . . . . .
Cl4 Cl 0.24784(10) 0.20703(8) 0.17654(9) 0.0201(2) Uani 1 1 d . . . . .
C1 C 0.5288(4) 0.2625(3) 0.1646(4) 0.0201(9) Uani 1 1 d . . . . .
H1A H 0.5971 0.2523 0.2157 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5533 0.2794 0.1096 0.030 Uiso 1 1 calc R U . . .
H1C H 0.4567 0.1894 0.1282 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5336(4) 0.3981(4) 0.3885(4) 0.0251(10) Uani 1 1 d . . . . .
H2A H 0.5508 0.4787 0.4411 0.038 Uiso 1 1 calc R U . . .
H2B H 0.6075 0.3760 0.4078 0.038 Uiso 1 1 calc R U . . .
H2C H 0.4659 0.3419 0.3902 0.038 Uiso 1 1 calc R U . . .
C3 C 0.6158(4) 0.5339(4) 0.2706(4) 0.0205(10) Uani 1 1 d . . . . .
C4 C 0.7399(4) 0.5512(4) 0.3252(4) 0.0248(10) Uani 1 1 d . . . . .
H4 H 0.7626 0.4921 0.3463 0.030 Uiso 1 1 calc R U . . .
C5 C 0.8297(4) 0.6548(4) 0.3485(4) 0.0274(11) Uani 1 1 d . . . . .
H5 H 0.9142 0.6676 0.3867 0.033 Uiso 1 1 calc R U . . .
C6 C 0.7960(5) 0.7397(4) 0.3159(4) 0.0272(11) Uani 1 1 d . . . . .
H6 H 0.8581 0.8109 0.3326 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6737(4) 0.7229(4) 0.2596(4) 0.0231(10) Uani 1 1 d . . . . .
H7 H 0.6519 0.7804 0.2352 0.028 Uiso 1 1 calc R U . . .
C8 C 0.5819(4) 0.6192(4) 0.2388(4) 0.0217(10) Uani 1 1 d . . . . .
C9 C 0.3897(5) 0.6168(4) 0.0370(4) 0.0319(12) Uani 1 1 d . . . . .
H9A H 0.4078 0.5542 -0.0114 0.048 Uiso 1 1 calc R U . . .
H9B H 0.4469 0.6948 0.0552 0.048 Uiso 1 1 calc R U . . .
H9C H 0.3049 0.6123 0.0000 0.048 Uiso 1 1 calc R U . . .
C10 C 0.3925(5) 0.7396(4) 0.2580(4) 0.0318(12) Uani 1 1 d . . . . .
H10A H 0.4583 0.8086 0.2697 0.048 Uiso 1 1 calc R U . . .
H10B H 0.3988 0.7395 0.3287 0.048 Uiso 1 1 calc R U . . .
H10C H 0.3122 0.7439 0.2198 0.048 Uiso 1 1 calc R U . . .
C11 C 0.0780(5) 0.0636(4) -0.0990(4) 0.0273(11) Uani 1 1 d . . . . .
H11A H 0.0006 0.0070 -0.1602 0.041 Uiso 1 1 calc R U . . .
H11B H 0.1000 0.0332 -0.0427 0.041 Uiso 1 1 calc R U . . .
H11C H 0.1436 0.0739 -0.1252 0.041 Uiso 1 1 calc R U . . .
C12 C 0.0097(4) 0.2559(4) -0.1610(4) 0.0267(10) Uani 1 1 d . . . . .
H12A H -0.0338 0.3127 -0.1485 0.040 Uiso 1 1 calc R U . . .
H12B H -0.0447 0.1838 -0.2274 0.040 Uiso 1 1 calc R U . . .
H12C H 0.0834 0.2918 -0.1700 0.040 Uiso 1 1 calc R U . . .
C13 C -0.0964(4) 0.1717(4) -0.0203(4) 0.0202(9) Uani 1 1 d . . . . .
C14 C -0.2064(4) 0.0939(4) -0.1100(4) 0.0253(10) Uani 1 1 d . . . . .
H14 H -0.2074 0.0618 -0.1811 0.030 Uiso 1 1 calc R U . . .
C15 C -0.3133(4) 0.0640(4) -0.0944(4) 0.0259(10) Uani 1 1 d . . . . .
H15 H -0.3887 0.0129 -0.1553 0.031 Uiso 1 1 calc R U . . .
C16 C -0.3112(4) 0.1083(4) 0.0096(4) 0.0265(10) Uani 1 1 d . . . . .
H16 H -0.3845 0.0851 0.0202 0.032 Uiso 1 1 calc R U . . .
C17 C -0.2026(4) 0.1865(4) 0.0985(4) 0.0245(10) Uani 1 1 d . . . . .
H17 H -0.2018 0.2171 0.1696 0.029 Uiso 1 1 calc R U . . .
C18 C -0.0947(4) 0.2202(3) 0.0835(4) 0.0202(9) Uani 1 1 d . . . . .
C19 C -0.0016(5) 0.4701(4) 0.2516(4) 0.0314(12) Uani 1 1 d . . . . .
H19A H -0.0682 0.4445 0.2733 0.047 Uiso 1 1 calc R U . . .
H19B H -0.0325 0.4945 0.1922 0.047 Uiso 1 1 calc R U . . .
H19C H 0.0665 0.5375 0.3144 0.047 Uiso 1 1 calc R U . . .
C20 C 0.0824(4) 0.2888(4) 0.3197(4) 0.0263(10) Uani 1 1 d . . . . .
H20A H 0.0071 0.2731 0.3327 0.039 Uiso 1 1 calc R U . . .
H20B H 0.1503 0.3514 0.3863 0.039 Uiso 1 1 calc R U . . .
H20C H 0.1029 0.2160 0.2996 0.039 Uiso 1 1 calc R U . . .
Nb2 Nb 0.25813(4) -0.09883(3) 0.59928(3) 0.01887(10) Uani 1 1 d . . . . .
Cl5 Cl 0.19361(11) -0.28671(9) 0.61354(10) 0.0251(2) Uani 1 1 d . . . . .
Cl6 Cl 0.34432(11) 0.01085(10) 0.79261(9) 0.0272(3) Uani 1 1 d . . . . .
Cl7 Cl 0.45391(11) -0.12262(10) 0.62152(10) 0.0293(3) Uani 1 1 d . . . . .
Cl8 Cl 0.17674(13) -0.22113(10) 0.40906(10) 0.0352(3) Uani 1 1 d . . . . .
Cl9 Cl 0.06918(11) -0.07577(10) 0.59363(10) 0.0296(3) Uani 1 1 d . . . . .
O1 O 0.3045(3) 0.0235(3) 0.5620(2) 0.0253(7) Uani 1 1 d . . . . .
C21 C 0.3391(5) 0.0575(5) 0.4843(4) 0.0345(12) Uani 1 1 d . . . . .
H21A H 0.3221 -0.0152 0.4200 0.041 Uiso 1 1 calc R U . . .
H21B H 0.4288 0.1019 0.5183 0.041 Uiso 1 1 calc R U . . .
C22 C 0.2735(7) 0.1307(7) 0.4481(6) 0.063(2) Uani 1 1 d . . . . .
H22A H 0.3002 0.2082 0.5093 0.095 Uiso 1 1 calc R U . . .
H22B H 0.1847 0.0912 0.4223 0.095 Uiso 1 1 calc R U . . .
H22C H 0.2915 0.1420 0.3884 0.095 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
Nb1 Cl2 2.4232(11) . ?
Nb1 Cl3 2.4242(12) . ?
Nb1 Cl1 2.4382(12) . ?
Nb1 Cl4 2.4402(11) . ?
Nb1 As1 2.7286(8) . ?
Nb1 As4 2.7352(7) . ?
Nb1 As2 2.7466(7) . ?
Nb1 As3 2.7505(7) . ?
As1 C2 1.923(4) . ?
As1 C1 1.936(4) . ?
As1 C3 1.938(4) . ?
As2 C10 1.934(4) . ?
As2 C8 1.936(5) . ?
As2 C9 1.945(5) . ?
As3 C20 1.931(4) . ?
As3 C19 1.933(4) . ?
As3 C18 1.940(4) . ?
As4 C12 1.931(4) . ?
As4 C11 1.936(4) . ?
As4 C13 1.949(4) . ?
C3 C8 1.384(6) . ?
C3 C4 1.396(6) . ?
C4 C5 1.385(6) . ?
C5 C6 1.384(7) . ?
C6 C7 1.383(7) . ?
C7 C8 1.409(6) . ?
C13 C18 1.387(6) . ?
C13 C14 1.399(6) . ?
C14 C15 1.380(7) . ?
C15 C16 1.385(7) . ?
C16 C17 1.387(6) . ?
C17 C18 1.393(6) . ?
Nb2 O1 1.824(3) . ?
Nb2 Cl9 2.3533(13) . ?
Nb2 Cl8 2.3738(13) . ?
Nb2 Cl6 2.3808(12) . ?
Nb2 Cl7 2.3956(13) . ?
Nb2 Cl5 2.4334(11) . ?
O1 C21 1.444(5) . ?
C21 C22 1.454(7) . ?

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
Cl2 Nb1 Cl3 93.94(4) . . ?
Cl2 Nb1 Cl1 146.16(4) . . ?
Cl3 Nb1 Cl1 95.61(4) . . ?
Cl2 Nb1 Cl4 95.62(4) . . ?
Cl3 Nb1 Cl4 146.16(4) . . ?
Cl1 Nb1 Cl4 94.27(4) . . ?
Cl2 Nb1 As1 77.02(3) . . ?
Cl3 Nb1 As1 143.47(3) . . ?
Cl1 Nb1 As1 76.05(3) . . ?
Cl4 Nb1 As1 70.37(3) . . ?
Cl2 Nb1 As4 143.62(3) . . ?
Cl3 Nb1 As4 75.91(3) . . ?
Cl1 Nb1 As4 70.20(3) . . ?
Cl4 Nb1 As4 77.22(3) . . ?
As1 Nb1 As4 130.60(2) . . ?
Cl2 Nb1 As2 76.93(3) . . ?
Cl3 Nb1 As2 70.51(3) . . ?
Cl1 Nb1 As2 75.87(3) . . ?
Cl4 Nb1 As2 143.33(3) . . ?
As1 Nb1 As2 72.970(19) . . ?
As4 Nb1 As2 128.84(2) . . ?
Cl2 Nb1 As3 70.99(3) . . ?
Cl3 Nb1 As3 77.27(3) . . ?
Cl1 Nb1 As3 142.83(3) . . ?
Cl4 Nb1 As3 75.37(3) . . ?
As1 Nb1 As3 129.81(2) . . ?
As4 Nb1 As3 72.70(2) . . ?
As2 Nb1 As3 132.20(2) . . ?
C2 As1 C1 104.49(19) . . ?
C2 As1 C3 101.02(19) . . ?
C1 As1 C3 104.04(18) . . ?
C2 As1 Nb1 115.42(14) . . ?
C1 As1 Nb1 115.28(14) . . ?
C3 As1 Nb1 114.86(14) . . ?
C10 As2 C8 103.7(2) . . ?
C10 As2 C9 101.0(2) . . ?
C8 As2 C9 104.2(2) . . ?
C10 As2 Nb1 115.57(14) . . ?
C8 As2 Nb1 114.37(12) . . ?
C9 As2 Nb1 116.15(15) . . ?
C20 As3 C19 101.9(2) . . ?
C20 As3 C18 105.00(18) . . ?
C19 As3 C18 100.9(2) . . ?
C20 As3 Nb1 115.59(14) . . ?
C19 As3 Nb1 116.67(14) . . ?
C18 As3 Nb1 114.81(13) . . ?
C12 As4 C11 102.8(2) . . ?
C12 As4 C13 102.4(2) . . ?
C11 As4 C13 103.24(19) . . ?
C12 As4 Nb1 115.19(14) . . ?
C11 As4 Nb1 116.27(15) . . ?
C13 As4 Nb1 115.10(13) . . ?
C8 C3 C4 120.5(4) . . ?
C8 C3 As1 118.9(3) . . ?
C4 C3 As1 120.6(3) . . ?
C5 C4 C3 119.7(4) . . ?
C4 C5 C6 119.8(4) . . ?
C7 C6 C5 121.2(4) . . ?
C6 C7 C8 119.0(4) . . ?
C3 C8 C7 119.7(4) . . ?
C3 C8 As2 118.9(3) . . ?
C7 C8 As2 121.4(3) . . ?
C18 C13 C14 120.5(4) . . ?
C18 C13 As4 118.3(3) . . ?
C14 C13 As4 121.1(3) . . ?
C15 C14 C13 119.5(4) . . ?
C14 C15 C16 120.2(4) . . ?
C15 C16 C17 120.4(4) . . ?
C16 C17 C18 120.0(4) . . ?
C13 C18 C17 119.3(4) . . ?
C13 C18 As3 118.8(3) . . ?
C17 C18 As3 121.8(3) . . ?
O1 Nb2 Cl9 94.85(11) . . ?
O1 Nb2 Cl8 85.28(10) . . ?
Cl9 Nb2 Cl8 93.80(5) . . ?
O1 Nb2 Cl6 98.48(10) . . ?
Cl9 Nb2 Cl6 88.66(5) . . ?
Cl8 Nb2 Cl6 175.33(4) . . ?
O1 Nb2 Cl7 88.68(11) . . ?
Cl9 Nb2 Cl7 174.61(5) . . ?
Cl8 Nb2 Cl7 90.55(5) . . ?
Cl6 Nb2 Cl7 86.79(4) . . ?
O1 Nb2 Cl5 168.59(10) . . ?
Cl9 Nb2 Cl5 89.56(4) . . ?
Cl8 Nb2 Cl5 83.94(4) . . ?
Cl6 Nb2 Cl5 92.12(4) . . ?
Cl7 Nb2 Cl5 87.72(4) . . ?
C21 O1 Nb2 145.6(3) . . ?
O1 C21 C22 112.7(4) . . ?

_refine_diff_density_max         0.843
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.130

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 993846'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2013rwz711a

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C20 H32 Cl4 Nb P4, C2 H3 Cl4 N Nb O, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.50 H36 Cl9 N Nb2 O P4'
_chemical_formula_weight         965.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.733(2)
_cell_length_b                   14.914(2)
_cell_length_c                   32.080(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7527.2(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15304
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      34.7

_exptl_crystal_description       Fragment
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_F_000             3848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.439
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            29471
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.986
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7372
_reflns_number_gt                5695
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?

_computing_publication_material  'WINGX (Farrugia, 2013)'

_refine_special_details          
;
All hydrogens were placed in calculated positions and refined using a 
riding model. ADPS were set at 1.2 (CHar), 1.5(CH3, CH2)that of the parent 
atoms. CH3 torsion angles were allowed to refine.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0180P)²+9.9885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7372
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.1111
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.37919(3) 0.50462(4) 0.39046(2) 0.01373(14) Uani 1 1 d . . . . .
Cl1 Cl 0.27076(10) 0.39014(10) 0.40250(5) 0.0200(4) Uani 1 1 d . . . . .
Cl2 Cl 0.49858(9) 0.55119(10) 0.34714(5) 0.0195(4) Uani 1 1 d . . . . .
Cl3 Cl 0.28041(10) 0.61647(10) 0.36343(5) 0.0208(4) Uani 1 1 d . . . . .
Cl4 Cl 0.47170(10) 0.46282(10) 0.44827(5) 0.0191(4) Uani 1 1 d . . . . .
P1 P 0.33019(10) 0.45561(11) 0.31368(5) 0.0175(4) Uani 1 1 d . . . . .
P2 P 0.45287(10) 0.34604(11) 0.37371(6) 0.0166(4) Uani 1 1 d . . . . .
P3 P 0.43801(10) 0.66233(11) 0.41920(5) 0.0164(4) Uani 1 1 d . . . . .
P4 P 0.28617(10) 0.54766(11) 0.45742(5) 0.0173(4) Uani 1 1 d . . . . .
C1 C 0.3614(4) 0.5299(4) 0.2717(2) 0.0282(18) Uani 1 1 d . . . . .
H1A H 0.4230 0.5261 0.2676 0.042 Uiso 1 1 calc R U . . .
H1B H 0.3458 0.5916 0.2788 0.042 Uiso 1 1 calc R U . . .
H1C H 0.3322 0.5121 0.2460 0.042 Uiso 1 1 calc R U . . .
C2 C 0.2158(4) 0.4465(5) 0.3067(2) 0.0280(18) Uani 1 1 d . . . . .
H2A H 0.2035 0.4267 0.2782 0.042 Uiso 1 1 calc R U . . .
H2B H 0.1894 0.5051 0.3116 0.042 Uiso 1 1 calc R U . . .
H2C H 0.1929 0.4029 0.3266 0.042 Uiso 1 1 calc R U . . .
C3 C 0.3666(4) 0.3444(4) 0.2976(2) 0.0196(16) Uani 1 1 d . . . . .
C4 C 0.3425(4) 0.3070(5) 0.2596(2) 0.0320(19) Uani 1 1 d . . . . .
H4 H 0.3100 0.3412 0.2404 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3658(5) 0.2201(5) 0.2497(3) 0.038(2) Uani 1 1 d . . . . .
H5 H 0.3506 0.1950 0.2235 0.045 Uiso 1 1 calc R U . . .
C6 C 0.4109(4) 0.1705(5) 0.2780(2) 0.0329(19) Uani 1 1 d . . . . .
H6 H 0.4246 0.1100 0.2716 0.040 Uiso 1 1 calc R U . . .
C7 C 0.4368(4) 0.2061(4) 0.3154(2) 0.0244(17) Uani 1 1 d . . . . .
H7 H 0.4691 0.1708 0.3343 0.029 Uiso 1 1 calc R U . . .
C8 C 0.4157(4) 0.2940(4) 0.3255(2) 0.0175(15) Uani 1 1 d . . . . .
C9 C 0.4374(4) 0.2601(4) 0.4129(2) 0.0278(18) Uani 1 1 d . . . . .
H9A H 0.3769 0.2448 0.4146 0.042 Uiso 1 1 calc R U . . .
H9B H 0.4570 0.2823 0.4400 0.042 Uiso 1 1 calc R U . . .
H9C H 0.4700 0.2065 0.4052 0.042 Uiso 1 1 calc R U . . .
C10 C 0.5676(4) 0.3470(4) 0.3672(2) 0.0265(17) Uani 1 1 d . . . . .
H10A H 0.5943 0.3699 0.3926 0.040 Uiso 1 1 calc R U . . .
H10B H 0.5826 0.3858 0.3436 0.040 Uiso 1 1 calc R U . . .
H10C H 0.5877 0.2860 0.3617 0.040 Uiso 1 1 calc R U . . .
C11 C 0.4321(4) 0.7552(4) 0.3827(2) 0.0242(17) Uani 1 1 d . . . . .
H11A H 0.3726 0.7721 0.3785 0.036 Uiso 1 1 calc R U . . .
H11B H 0.4571 0.7371 0.3560 0.036 Uiso 1 1 calc R U . . .
H11C H 0.4636 0.8065 0.3939 0.036 Uiso 1 1 calc R U . . .
C12 C 0.5486(4) 0.6621(4) 0.4367(2) 0.0220(16) Uani 1 1 d . . . . .
H12A H 0.5685 0.7240 0.4398 0.033 Uiso 1 1 calc R U . . .
H12B H 0.5839 0.6310 0.4161 0.033 Uiso 1 1 calc R U . . .
H12C H 0.5527 0.6312 0.4636 0.033 Uiso 1 1 calc R U . . .
C13 C 0.3819(4) 0.7040(4) 0.46468(19) 0.0153(14) Uani 1 1 d . . . . .
C14 C 0.4078(4) 0.7827(4) 0.4849(2) 0.0238(16) Uani 1 1 d . . . . .
H14 H 0.4533 0.8169 0.4737 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3678(4) 0.8111(4) 0.5209(2) 0.0264(17) Uani 1 1 d . . . . .
H15 H 0.3855 0.8650 0.5341 0.032 Uiso 1 1 calc R U . . .
C16 C 0.3018(4) 0.7611(5) 0.5379(2) 0.0287(18) Uani 1 1 d . . . . .
H16 H 0.2752 0.7804 0.5629 0.034 Uiso 1 1 calc R U . . .
C17 C 0.2746(4) 0.6835(4) 0.5185(2) 0.0235(16) Uani 1 1 d . . . . .
H17 H 0.2287 0.6501 0.5299 0.028 Uiso 1 1 calc R U . . .
C18 C 0.3152(4) 0.6541(4) 0.4819(2) 0.0183(15) Uani 1 1 d . . . . .
C19 C 0.1720(4) 0.5554(4) 0.4486(2) 0.0254(17) Uani 1 1 d . . . . .
H19A H 0.1487 0.4951 0.4442 0.038 Uiso 1 1 calc R U . . .
H19B H 0.1612 0.5922 0.4238 0.038 Uiso 1 1 calc R U . . .
H19C H 0.1448 0.5829 0.4729 0.038 Uiso 1 1 calc R U . . .
C20 C 0.2951(4) 0.4688(4) 0.5005(2) 0.0234(16) Uani 1 1 d . . . . .
H20A H 0.2478 0.4779 0.5199 0.035 Uiso 1 1 calc R U . . .
H20B H 0.3490 0.4786 0.5151 0.035 Uiso 1 1 calc R U . . .
H20C H 0.2934 0.4074 0.4897 0.035 Uiso 1 1 calc R U . . .
Nb2 Nb 0.37987(3) 0.99599(4) 0.62812(2) 0.01466(14) Uani 1 1 d . . . . .
Cl5 Cl 0.33272(12) 0.99178(12) 0.69954(5) 0.0293(4) Uani 1 1 d . . . . .
Cl6 Cl 0.23474(10) 1.00848(12) 0.60698(5) 0.0278(4) Uani 1 1 d . . . . .
Cl7 Cl 0.42317(10) 1.04917(11) 0.56039(5) 0.0234(4) Uani 1 1 d . . . . .
Cl8 Cl 0.52009(10) 1.02545(11) 0.65271(6) 0.0294(4) Uani 1 1 d . . . . .
O1 O 0.3901(3) 0.8837(3) 0.62071(14) 0.0223(11) Uani 1 1 d . . . . .
N1 N 0.3590(3) 1.1576(4) 0.64179(18) 0.0254(14) Uani 1 1 d . . . . .
C21 C 0.3384(4) 1.2260(5) 0.6534(2) 0.0224(16) Uani 1 1 d . . . . .
C22 C 0.3085(5) 1.3136(4) 0.6682(3) 0.038(2) Uani 1 1 d . . . . .
H22A H 0.2505 1.3240 0.6581 0.057 Uiso 1 1 calc R U . . .
H22B H 0.3461 1.3608 0.6575 0.057 Uiso 1 1 calc R U . . .
H22C H 0.3089 1.3146 0.6987 0.057 Uiso 1 1 calc R U . . .
Cl9 Cl 0.41228(19) 1.22778(18) 0.76302(9) 0.0808(9) Uani 1 1 d . . . . .
C23 C 0.5000 1.1570(8) 0.7500 0.059(4) Uani 1 2 d S T P . .
H23A H 0.4852 1.1183 0.7260 0.070 Uiso 0.5 1 calc R U P . .
H23B H 0.5148 1.1183 0.7740 0.070 Uiso 0.5 1 calc R U P . .


_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
Nb1 Cl2 2.4375(16) . ?
Nb1 Cl4 2.4385(16) . ?
Nb1 Cl3 2.4392(16) . ?
Nb1 Cl1 2.4444(16) . ?
Nb1 P4 2.6773(18) . ?
Nb1 P1 2.6824(19) . ?
Nb1 P2 2.6882(18) . ?
Nb1 P3 2.6904(18) . ?
P1 C1 1.812(6) . ?
P1 C2 1.818(6) . ?
P1 C3 1.829(7) . ?
P2 C9 1.812(6) . ?
P2 C10 1.817(6) . ?
P2 C8 1.826(6) . ?
P3 C13 1.815(6) . ?
P3 C11 1.817(6) . ?
P3 C12 1.828(6) . ?
P4 C20 1.820(6) . ?
P4 C19 1.822(6) . ?
P4 C18 1.829(7) . ?
C3 C4 1.394(9) . ?
C3 C8 1.401(9) . ?
C4 C5 1.384(9) . ?
C5 C6 1.368(10) . ?
C6 C7 1.375(9) . ?
C7 C8 1.391(8) . ?
C13 C18 1.400(8) . ?
C13 C14 1.402(8) . ?
C14 C15 1.380(9) . ?
C15 C16 1.391(9) . ?
C16 C17 1.381(9) . ?
C17 C18 1.407(9) . ?
Nb2 O1 1.700(4) . ?
Nb2 Cl8 2.3837(17) . ?
Nb2 Cl6 2.3892(17) . ?
Nb2 Cl5 2.4091(17) . ?
Nb2 Cl7 2.4112(17) . ?
Nb2 N1 2.472(6) . ?
N1 C21 1.133(8) . ?
C21 C22 1.467(9) . ?
Cl9 C23 1.787(8) . ?
C23 Cl9 1.787(8) 3_656 ?

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
Cl2 Nb1 Cl4 92.67(6) . . ?
Cl2 Nb1 Cl3 95.37(6) . . ?
Cl4 Nb1 Cl3 145.63(6) . . ?
Cl2 Nb1 Cl1 145.79(6) . . ?
Cl4 Nb1 Cl1 96.76(6) . . ?
Cl3 Nb1 Cl1 95.12(6) . . ?
Cl2 Nb1 P4 144.13(6) . . ?
Cl4 Nb1 P4 77.13(6) . . ?
Cl3 Nb1 P4 76.88(5) . . ?
Cl1 Nb1 P4 70.07(5) . . ?
Cl2 Nb1 P1 77.04(5) . . ?
Cl4 Nb1 P1 143.15(6) . . ?
Cl3 Nb1 P1 71.15(5) . . ?
Cl1 Nb1 P1 75.77(5) . . ?
P4 Nb1 P1 130.16(6) . . ?
Cl2 Nb1 P2 78.72(5) . . ?
Cl4 Nb1 P2 70.71(5) . . ?
Cl3 Nb1 P2 143.65(6) . . ?
Cl1 Nb1 P2 73.62(5) . . ?
P4 Nb1 P2 127.37(6) . . ?
P1 Nb1 P2 72.58(5) . . ?
Cl2 Nb1 P3 71.41(5) . . ?
Cl4 Nb1 P3 75.97(5) . . ?
Cl3 Nb1 P3 75.11(6) . . ?
Cl1 Nb1 P3 142.80(6) . . ?
P4 Nb1 P3 72.75(5) . . ?
P1 Nb1 P3 130.68(6) . . ?
P2 Nb1 P3 133.58(5) . . ?
C1 P1 C2 102.8(3) . . ?
C1 P1 C3 105.1(3) . . ?
C2 P1 C3 102.0(3) . . ?
C1 P1 Nb1 116.0(2) . . ?
C2 P1 Nb1 114.7(2) . . ?
C3 P1 Nb1 114.6(2) . . ?
C9 P2 C10 102.7(3) . . ?
C9 P2 C8 104.1(3) . . ?
C10 P2 C8 103.0(3) . . ?
C9 P2 Nb1 115.2(2) . . ?
C10 P2 Nb1 116.4(2) . . ?
C8 P2 Nb1 113.9(2) . . ?
C13 P3 C11 103.5(3) . . ?
C13 P3 C12 102.5(3) . . ?
C11 P3 C12 104.3(3) . . ?
C13 P3 Nb1 114.1(2) . . ?
C11 P3 Nb1 115.3(2) . . ?
C12 P3 Nb1 115.5(2) . . ?
C20 P4 C19 103.6(3) . . ?
C20 P4 C18 102.4(3) . . ?
C19 P4 C18 105.0(3) . . ?
C20 P4 Nb1 114.3(2) . . ?
C19 P4 Nb1 115.4(2) . . ?
C18 P4 Nb1 114.6(2) . . ?
C4 C3 C8 119.7(6) . . ?
C4 C3 P1 121.7(5) . . ?
C8 C3 P1 118.6(5) . . ?
C5 C4 C3 120.3(7) . . ?
C6 C5 C4 119.4(7) . . ?
C5 C6 C7 121.6(7) . . ?
C6 C7 C8 119.8(6) . . ?
C7 C8 C3 119.2(6) . . ?
C7 C8 P2 121.4(5) . . ?
C3 C8 P2 119.4(5) . . ?
C18 C13 C14 118.7(6) . . ?
C18 C13 P3 120.0(5) . . ?
C14 C13 P3 121.2(5) . . ?
C15 C14 C13 120.8(6) . . ?
C14 C15 C16 120.2(6) . . ?
C17 C16 C15 120.3(7) . . ?
C16 C17 C18 119.7(6) . . ?
C13 C18 C17 120.3(6) . . ?
C13 C18 P4 118.6(5) . . ?
C17 C18 P4 121.0(5) . . ?
O1 Nb2 Cl8 98.06(15) . . ?
O1 Nb2 Cl6 97.34(15) . . ?
Cl8 Nb2 Cl6 164.59(7) . . ?
O1 Nb2 Cl5 97.84(15) . . ?
Cl8 Nb2 Cl5 88.57(7) . . ?
Cl6 Nb2 Cl5 88.72(6) . . ?
O1 Nb2 Cl7 99.87(15) . . ?
Cl8 Nb2 Cl7 88.63(6) . . ?
Cl6 Nb2 Cl7 89.35(6) . . ?
Cl5 Nb2 Cl7 162.28(6) . . ?
O1 Nb2 N1 176.9(2) . . ?
Cl8 Nb2 N1 83.37(13) . . ?
Cl6 Nb2 N1 81.22(14) . . ?
Cl5 Nb2 N1 79.39(14) . . ?
Cl7 Nb2 N1 82.91(14) . . ?
C21 N1 Nb2 166.9(5) . . ?
N1 C21 C22 177.8(8) . . ?
Cl9 C23 Cl9 107.6(7) . 3_656 ?

_refine_diff_density_max         1.076
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.132

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 993847'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2013rwz727
#[{{Me2P(CH2)2PMe2}NbOCl3}2-\m-{Me2P(CH2)2PMe2}]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H48 Cl6 Nb2 O2 P6'
_chemical_formula_sum            'C18 H48 Cl6 Nb2 O2 P6'
_chemical_formula_weight         880.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.096(5)
_cell_length_b                   10.987(6)
_cell_length_c                   18.064(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.158(15)
_cell_angle_gamma                90.00
_cell_volume                     1805.3(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5514
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      34.6

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8255
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3444
_reflns_number_gt                2977
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular 
structures program for Mac and Windows. CrystalMaker Software Ltd, 
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 2013)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.


All hydrogens were placed in calculated positions and refined using a 
riding model. ADPS were set at 1.2 (CH2), 1.5(CH3) that of the parent 
atoms. CH3 torsion angles were allowed to refine.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0529P)²+7.7765P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3444
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1442
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.25884(6) 0.32807(5) 0.11047(3) 0.01368(18) Uani 1 1 d . . .
Cl1 Cl 0.52907(17) 0.28763(15) 0.12190(9) 0.0211(4) Uani 1 1 d . . .
Cl2 Cl 0.01065(17) 0.23876(14) 0.08119(9) 0.0202(4) Uani 1 1 d . . .
Cl3 Cl 0.23666(17) 0.24006(14) 0.24388(8) 0.0194(4) Uani 1 1 d . . .
P1 P 0.05527(18) 0.47399(15) 0.16926(9) 0.0147(4) Uani 1 1 d . . .
P2 P 0.39273(18) 0.51675(15) 0.17580(9) 0.0149(4) Uani 1 1 d . . .
P3 P 0.30021(18) 0.10986(15) 0.03776(9) 0.0159(4) Uani 1 1 d . . .
O1 O 0.2667(5) 0.4156(4) 0.0314(2) 0.0199(10) Uani 1 1 d . . .
C1 C -0.1015(7) 0.4094(6) 0.2189(4) 0.0222(15) Uani 1 1 d . . .
H1A H -0.1588 0.4751 0.2414 0.033 Uiso 1 1 calc R . .
H1B H -0.0659 0.3543 0.2577 0.033 Uiso 1 1 calc R . .
H1C H -0.1638 0.3641 0.1842 0.033 Uiso 1 1 calc R . .
C2 C -0.0258(7) 0.5704(6) 0.0982(3) 0.0239(15) Uani 1 1 d . . .
H2A H -0.0871 0.5207 0.0653 0.036 Uiso 1 1 calc R . .
H2B H 0.0525 0.6091 0.0695 0.036 Uiso 1 1 calc R . .
H2C H -0.0864 0.6332 0.1216 0.036 Uiso 1 1 calc R . .
C3 C 0.1291(7) 0.5803(6) 0.2382(3) 0.0164(13) Uani 1 1 d . . .
H3A H 0.0550 0.6433 0.2500 0.020 Uiso 1 1 calc R . .
H3B H 0.1541 0.5362 0.2844 0.020 Uiso 1 1 calc R . .
C4 C 0.2679(7) 0.6400(6) 0.2057(4) 0.0186(14) Uani 1 1 d . . .
H4A H 0.3166 0.6914 0.2435 0.022 Uiso 1 1 calc R . .
H4B H 0.2412 0.6921 0.1630 0.022 Uiso 1 1 calc R . .
C5 C 0.5207(7) 0.5926(6) 0.1134(4) 0.0228(15) Uani 1 1 d . . .
H5A H 0.5585 0.6666 0.1370 0.034 Uiso 1 1 calc R . .
H5B H 0.4697 0.6143 0.0674 0.034 Uiso 1 1 calc R . .
H5C H 0.6027 0.5378 0.1022 0.034 Uiso 1 1 calc R . .
C6 C 0.4914(7) 0.4819(6) 0.2609(3) 0.0200(14) Uani 1 1 d . . .
H6A H 0.5405 0.5555 0.2791 0.030 Uiso 1 1 calc R . .
H6B H 0.5650 0.4188 0.2511 0.030 Uiso 1 1 calc R . .
H6C H 0.4220 0.4526 0.2982 0.030 Uiso 1 1 calc R . .
C7 C 0.2160(7) 0.1108(6) -0.0537(3) 0.0211(14) Uani 1 1 d . . .
H7A H 0.2789 0.1557 -0.0881 0.032 Uiso 1 1 calc R . .
H7B H 0.1195 0.1502 -0.0510 0.032 Uiso 1 1 calc R . .
H7C H 0.2041 0.0269 -0.0711 0.032 Uiso 1 1 calc R . .
C8 C 0.2158(7) -0.0220(6) 0.0822(4) 0.0205(14) Uani 1 1 d . . .
H8A H 0.2113 -0.0898 0.0470 0.031 Uiso 1 1 calc R . .
H8B H 0.1161 -0.0011 0.0982 0.031 Uiso 1 1 calc R . .
H8C H 0.2746 -0.0460 0.1253 0.031 Uiso 1 1 calc R . .
C9 C 0.4908(7) 0.0617(5) 0.0207(3) 0.0183(14) Uani 1 1 d . . .
H9A H 0.5404 0.1260 -0.0084 0.022 Uiso 1 1 calc R . .
H9B H 0.5423 0.0559 0.0690 0.022 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Nb1 O1 1.724(4) . ?
Nb1 Cl1 2.506(2) . ?
Nb1 Cl2 2.517(2) . ?
Nb1 Cl3 2.605(2) . ?
Nb1 P1 2.6716(19) . ?
Nb1 P2 2.677(2) . ?
Nb1 P3 2.760(2) . ?
P1 C2 1.818(6) . ?
P1 C1 1.830(6) . ?
P1 C3 1.833(6) . ?
P2 C6 1.818(6) . ?
P2 C5 1.825(6) . ?
P2 C4 1.849(6) . ?
P3 C7 1.819(6) . ?
P3 C8 1.827(6) . ?
P3 C9 1.839(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.541(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C9 1.559(11) 3_655 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?

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 Nb1 Cl1 97.14(15) . . ?
O1 Nb1 Cl2 94.74(15) . . ?
Cl1 Nb1 Cl2 145.83(6) . . ?
O1 Nb1 Cl3 167.75(15) . . ?
Cl1 Nb1 Cl3 86.36(6) . . ?
Cl2 Nb1 Cl3 88.74(6) . . ?
O1 Nb1 P1 91.43(15) . . ?
Cl1 Nb1 P1 138.98(6) . . ?
Cl2 Nb1 P1 72.25(6) . . ?
Cl3 Nb1 P1 78.43(6) . . ?
O1 Nb1 P2 85.03(15) . . ?
Cl1 Nb1 P2 69.88(6) . . ?
Cl2 Nb1 P2 143.27(5) . . ?
Cl3 Nb1 P2 85.18(6) . . ?
P1 Nb1 P2 71.04(6) . . ?
O1 Nb1 P3 94.84(15) . . ?
Cl1 Nb1 P3 75.53(5) . . ?
Cl2 Nb1 P3 71.62(6) . . ?
Cl3 Nb1 P3 97.40(6) . . ?
P1 Nb1 P3 143.70(6) . . ?
P2 Nb1 P3 145.09(6) . . ?
C2 P1 C1 104.9(3) . . ?
C2 P1 C3 104.8(3) . . ?
C1 P1 C3 101.5(3) . . ?
C2 P1 Nb1 110.4(2) . . ?
C1 P1 Nb1 120.3(2) . . ?
C3 P1 Nb1 113.5(2) . . ?
C6 P2 C5 107.7(3) . . ?
C6 P2 C4 102.1(3) . . ?
C5 P2 C4 103.8(3) . . ?
C6 P2 Nb1 115.6(2) . . ?
C5 P2 Nb1 111.8(2) . . ?
C4 P2 Nb1 114.6(2) . . ?
C7 P3 C8 103.1(3) . . ?
C7 P3 C9 104.2(3) . . ?
C8 P3 C9 104.1(3) . . ?
C7 P3 Nb1 111.7(2) . . ?
C8 P3 Nb1 115.0(2) . . ?
C9 P3 Nb1 117.3(2) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 P1 108.1(4) . . ?
C4 C3 H3A 110.1 . . ?
P1 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
P1 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C3 C4 P2 107.7(4) . . ?
C3 C4 H4A 110.2 . . ?
P2 C4 H4A 110.2 . . ?
C3 C4 H4B 110.2 . . ?
P2 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P3 C7 H7A 109.5 . . ?
P3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C9 P3 115.7(6) 3_655 . ?
C9 C9 H9A 108.4 3_655 . ?
P3 C9 H9A 108.4 . . ?
C9 C9 H9B 108.4 3_655 . ?
P3 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.680
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.154
_database_code_depnum_ccdc_archive 'CCDC 993848'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2013rwz912b_ml
#[{o-C6H4(PMe2)2}NbOCl3-\m-O-NbCl3(CH3CN){o-C6H4(PMe2)2}]

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H35 Cl6 N Nb2 O2 P4'
_chemical_formula_sum            'C22 H35 Cl6 N Nb2 O2 P4'
_chemical_formula_weight         867.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.845(8)
_cell_length_b                   33.518(19)
_cell_length_c                   8.596(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.35(3)
_cell_angle_gamma                90
_cell_volume                     3410(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9110
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      34.6

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.352
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9606
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            17515
_diffrn_reflns_av_unetI/netI     0.2289
_diffrn_reflns_av_R_equivalents  0.1619
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.936
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6683
_reflns_number_gt                3128
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 2013)'

_refine_special_details          
;
The terminal oxygen O2 and chloride Cl6 are disordered (ca. 82:18) 
with respect to the side of the molecule they are on. These were 
modelled as  2 fractionally occupied ion both possible sites 
using distance restraints (Nb-O = 1.8 & Nb-Cl = 2.47, default 
Shelx esd) and the ADPs of Cl and O pairs were constrained to 
be equal.

All hydrogens were placed in calculated positions and refined 
using a riding model. ADPS were set at 1.2 (CHar), 1.5(CH3) 
that of the parent atoms. CH3 torsion angles were allowed to 
refine.

The crystal quality was poor and the measured diffraction 
images were weak (ca. 47obs) and rather messy. The 
residual electron density peaks (Q1-Q4) are located ca. 1A 
either side of the 2 Nb sites.

The structure contains solvent accessible voids of ca. 
75Ang3, and these do contain residual electron density peaks 
that could conceivably be disordered acetonitrile - although 
this is by no means certain. In view of the generally poor 
data quality no attempt was made to refine the possible 
solvent molecule. 

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
w=1/[σ²(Fo²)+(0.1245P)²+17.2850P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6683
_refine_ls_number_parameters     342
_refine_ls_number_restraints     332
_refine_ls_R_factor_all          0.2117
_refine_ls_R_factor_gt           0.1030
_refine_ls_wR_factor_ref         0.2966
_refine_ls_wR_factor_gt          0.2254
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C -0.0241(13) -0.8916(5) 0.1077(18) 0.033(3) Uani 1 1 d . U . . .
H1A H -0.0479 -0.8648 0.0743 0.050 Uiso 1 1 calc R U . . .
H1B H -0.0506 -0.8968 0.2123 0.050 Uiso 1 1 calc R U . . .
H1C H -0.0564 -0.9114 0.0349 0.050 Uiso 1 1 calc R U . . .
C2 C 0.1749(14) -0.8636(4) 0.2757(17) 0.029(3) Uani 1 1 d . U . . .
H2A H 0.1640 -0.8354 0.2479 0.043 Uiso 1 1 calc R U . . .
H2B H 0.2549 -0.8684 0.3026 0.043 Uiso 1 1 calc R U . . .
H2C H 0.1296 -0.8701 0.3652 0.043 Uiso 1 1 calc R U . . .
C3 C 0.1546(14) -0.9458(4) 0.1746(17) 0.0310(15) Uani 1 1 d . U . . .
C4 C 0.1126(14) -0.9606(5) 0.3130(17) 0.0334(19) Uani 1 1 d . U . . .
H4 H 0.0785 -0.9430 0.3838 0.040 Uiso 1 1 calc R U . . .
C5 C 0.1210(14) -1.0012(5) 0.3467(19) 0.036(2) Uani 1 1 d . U . . .
H5 H 0.0877 -1.0113 0.4372 0.044 Uiso 1 1 calc R U . . .
C6 C 0.1776(15) -1.0272(5) 0.2495(18) 0.037(2) Uani 1 1 d . U . . .
H6 H 0.1863 -1.0545 0.2760 0.044 Uiso 1 1 calc R U . . .
C7 C 0.2213(14) -1.0120(5) 0.1119(18) 0.0348(19) Uani 1 1 d . U . . .
H7 H 0.2611 -1.0291 0.0450 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2059(14) -0.9720(4) 0.0743(16) 0.0309(15) Uani 1 1 d . U . . .
C9 C 0.1752(15) -0.9830(5) -0.2493(18) 0.036(3) Uani 1 1 d . U . . .
H9A H 0.0954 -0.9753 -0.2519 0.053 Uiso 1 1 calc R U . . .
H9B H 0.1825 -1.0110 -0.2185 0.053 Uiso 1 1 calc R U . . .
H9C H 0.2053 -0.9794 -0.3529 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3984(13) -0.9692(5) -0.1208(17) 0.030(2) Uani 1 1 d . U . . .
H10A H 0.4300 -0.9597 -0.2177 0.045 Uiso 1 1 calc R U . . .
H10B H 0.4002 -0.9984 -0.1185 0.045 Uiso 1 1 calc R U . . .
H10C H 0.4433 -0.9587 -0.0317 0.045 Uiso 1 1 calc R U . . .
C11 C 0.2758(14) -0.7991(5) -0.4057(18) 0.034(2) Uani 1 1 d . U . . .
C12 C 0.3212(15) -0.7680(5) -0.501(2) 0.044(3) Uani 1 1 d . U . . .
H12A H 0.3579 -0.7800 -0.5901 0.066 Uiso 1 1 calc R U . . .
H12B H 0.3766 -0.7523 -0.4396 0.066 Uiso 1 1 calc R U . . .
H12C H 0.2598 -0.7505 -0.5396 0.066 Uiso 1 1 calc R U . . .
C13 C 0.5808(14) -0.8601(5) 0.4989(16) 0.034(3) Uani 1 1 d . U . . .
H13A H 0.5116 -0.8761 0.4996 0.052 Uiso 1 1 calc R U . . .
H13B H 0.5619 -0.8318 0.5118 0.052 Uiso 1 1 calc R U . . .
H13C H 0.6324 -0.8685 0.5846 0.052 Uiso 1 1 calc R U . . .
C14 C 0.7078(14) -0.9163(5) 0.3198(18) 0.036(3) Uani 1 1 d . U . . .
H14A H 0.7464 -0.9213 0.2230 0.055 Uiso 1 1 calc R U . . .
H14B H 0.6474 -0.9360 0.3305 0.055 Uiso 1 1 calc R U . . .
H14C H 0.7621 -0.9186 0.4085 0.055 Uiso 1 1 calc R U . . .
C15 C 0.7746(13) -0.8349(4) 0.3380(15) 0.0271(15) Uani 1 1 d . U . . .
C16 C 0.8500(13) -0.8379(4) 0.4674(16) 0.0271(19) Uani 1 1 d . U . . .
H16 H 0.8361 -0.8568 0.5468 0.033 Uiso 1 1 calc R U . . .
C17 C 0.9442(13) -0.8138(4) 0.4808(16) 0.029(2) Uani 1 1 d . U . . .
H17 H 0.9958 -0.8165 0.5678 0.035 Uiso 1 1 calc R U . . .
C18 C 0.9635(13) -0.7855(4) 0.3663(16) 0.029(2) Uani 1 1 d . U . . .
H18 H 1.0258 -0.7678 0.3788 0.035 Uiso 1 1 calc R U . . .
C19 C 0.8926(13) -0.7829(4) 0.2342(16) 0.0282(19) Uani 1 1 d . U . . .
H19 H 0.9083 -0.7644 0.1544 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7960(13) -0.8082(4) 0.2189(16) 0.0269(15) Uani 1 1 d . U . . .
C21 C 0.7813(13) -0.8138(5) -0.1129(15) 0.030(3) Uani 1 1 d . U . . .
H21A H 0.8029 -0.8420 -0.1157 0.044 Uiso 1 1 calc R U . . .
H21B H 0.8495 -0.7973 -0.1038 0.044 Uiso 1 1 calc R U . . .
H21C H 0.7382 -0.8070 -0.2090 0.044 Uiso 1 1 calc R U . . .
C22 C 0.6625(13) -0.7514(4) 0.0460(17) 0.031(3) Uani 1 1 d . U . . .
H22A H 0.6156 -0.7443 0.1332 0.047 Uiso 1 1 calc R U . . .
H22B H 0.6216 -0.7452 -0.0525 0.047 Uiso 1 1 calc R U . . .
H22C H 0.7331 -0.7361 0.0531 0.047 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3111(4) -0.90427(12) -0.3811(4) 0.0360(9) Uani 1 1 d . U . . .
Cl2 Cl 0.0363(3) -0.89589(12) -0.2790(5) 0.0354(9) Uani 1 1 d . U . . .
Cl3 Cl 0.1177(4) -0.81575(12) -0.0559(5) 0.0380(9) Uani 1 1 d . U . . .
Cl4 Cl 0.4376(3) -0.90860(11) 0.2113(4) 0.0320(9) Uani 1 1 d . U . . .
Cl5 Cl 0.4991(3) -0.80844(11) -0.1693(4) 0.0301(8) Uani 1 1 d . U . . .
N1 N 0.2416(11) -0.8245(4) -0.3311(15) 0.0345(19) Uani 1 1 d . U . . .
Nb1 Nb 0.22215(12) -0.87447(4) -0.15633(15) 0.0276(4) Uani 1 1 d . U . . .
Nb2 Nb 0.51191(13) -0.85027(5) 0.06837(16) 0.0343(4) Uani 1 1 d D U . . .
O1 O 0.3498(9) -0.8644(3) -0.0526(11) 0.0297(13) Uani 1 1 d . U . . .
P1 P 0.1306(4) -0.89485(12) 0.1108(4) 0.0293(8) Uani 1 1 d . U . . .
P2 P 0.2536(4) -0.95219(12) -0.1107(4) 0.0294(8) Uani 1 1 d . U . . .
P3 P 0.6484(4) -0.86705(12) 0.3147(4) 0.0279(8) Uani 1 1 d . U . . .
P4 P 0.6946(4) -0.80489(12) 0.0538(4) 0.0262(8) Uani 1 1 d . U . . .
Cl6A Cl 0.6343(5) -0.89752(15) -0.0689(5) 0.0337(10) Uani 0.813(10) 1 d D U P A
1
O2A O 0.4597(12) -0.8114(4) 0.1990(15) 0.0287(13) Uani 0.813(10) 1 d D U P A 1
O2B O 0.608(4) -0.8836(15) -0.025(6) 0.0287(13) Uani 0.187(10) 1 d D U P A 2
Cl6B Cl 0.449(2) -0.8007(6) 0.239(2) 0.0337(10) Uani 0.187(10) 1 d D 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
C1 P1 1.835(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 P1 1.822(15) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C8 1.39(2) . ?
C3 C4 1.40(2) . ?
C3 P1 1.814(16) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.40(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.41(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.39(2) . ?
C7 H7 0.9500 . ?
C8 P2 1.834(16) . ?
C9 P2 1.805(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 P2 1.813(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N1 1.150(19) . ?
C11 C12 1.45(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 P3 1.819(16) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 P3 1.795(16) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.39(2) . ?
C15 C16 1.401(19) . ?
C15 P3 1.846(16) . ?
C16 C17 1.38(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.39(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.387(19) . ?
C18 H18 0.9500 . ?
C19 C20 1.43(2) . ?
C19 H19 0.9500 . ?
C20 P4 1.824(14) . ?
C21 P4 1.822(15) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 P4 1.834(15) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl1 Nb1 2.451(4) . ?
Cl2 Nb1 2.507(4) . ?
Cl3 Nb1 2.497(4) . ?
Cl4 Nb2 2.489(4) . ?
Cl5 Nb2 2.478(4) . ?
N1 Nb1 2.268(13) . ?
Nb1 O1 1.757(10) . ?
Nb1 P2 2.658(4) . ?
Nb1 P1 2.668(5) . ?
Nb2 O2B 1.80(2) . ?
Nb2 O2A 1.843(13) . ?
Nb2 O1 2.197(10) . ?
Nb2 Cl6B 2.357(15) . ?
Nb2 Cl6A 2.479(5) . ?
Nb2 P4 2.652(5) . ?
Nb2 P3 2.671(4) . ?

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
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 C3 C4 119.0(14) . . ?
C8 C3 P1 118.3(12) . . ?
C4 C3 P1 122.3(12) . . ?
C5 C4 C3 119.9(15) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.1(16) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 118.7(15) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C8 C7 C6 119.6(15) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C3 C8 C7 121.4(14) . . ?
C3 C8 P2 118.0(11) . . ?
C7 C8 P2 120.6(12) . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 178(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P3 C13 H13A 109.5 . . ?
P3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P3 C14 H14A 109.5 . . ?
P3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 120.0(14) . . ?
C20 C15 P3 117.8(10) . . ?
C16 C15 P3 122.1(11) . . ?
C17 C16 C15 120.8(14) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 119.7(13) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.7(14) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.7(14) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 119.0(13) . . ?
C15 C20 P4 118.5(11) . . ?
C19 C20 P4 122.4(11) . . ?
P4 C21 H21A 109.5 . . ?
P4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
P4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P4 C22 H22A 109.5 . . ?
P4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
P4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C11 N1 Nb1 164.6(12) . . ?
O1 Nb1 N1 94.9(5) . . ?
O1 Nb1 Cl1 95.1(4) . . ?
N1 Nb1 Cl1 73.7(4) . . ?
O1 Nb1 Cl3 95.8(4) . . ?
N1 Nb1 Cl3 73.3(4) . . ?
Cl1 Nb1 Cl3 145.96(14) . . ?
O1 Nb1 Cl2 172.5(3) . . ?
N1 Nb1 Cl2 92.5(3) . . ?
Cl1 Nb1 Cl2 87.13(15) . . ?
Cl3 Nb1 Cl2 86.12(15) . . ?
O1 Nb1 P2 90.0(3) . . ?
N1 Nb1 P2 143.5(4) . . ?
Cl1 Nb1 P2 69.81(14) . . ?
Cl3 Nb1 P2 142.16(15) . . ?
Cl2 Nb1 P2 84.08(13) . . ?
O1 Nb1 P1 89.1(3) . . ?
N1 Nb1 P1 144.6(4) . . ?
Cl1 Nb1 P1 141.00(15) . . ?
Cl3 Nb1 P1 71.32(14) . . ?
Cl2 Nb1 P1 84.73(14) . . ?
P2 Nb1 P1 71.43(13) . . ?
O2B Nb2 O1 102.1(19) . . ?
O2A Nb2 O1 97.6(5) . . ?
O2B Nb2 Cl6B 159(2) . . ?
O1 Nb2 Cl6B 98.7(7) . . ?
O2B Nb2 Cl5 90.1(18) . . ?
O2A Nb2 Cl5 95.3(4) . . ?
O1 Nb2 Cl5 73.1(3) . . ?
Cl6B Nb2 Cl5 95.9(6) . . ?
O2A Nb2 Cl6A 163.6(5) . . ?
O1 Nb2 Cl6A 98.9(3) . . ?
Cl5 Nb2 Cl6A 89.21(16) . . ?
O2B Nb2 Cl4 88.5(19) . . ?
O2A Nb2 Cl4 96.9(5) . . ?
O1 Nb2 Cl4 75.2(3) . . ?
Cl6B Nb2 Cl4 96.8(6) . . ?
Cl5 Nb2 Cl4 147.23(13) . . ?
Cl6A Nb2 Cl4 87.62(17) . . ?
O2B Nb2 P4 79(2) . . ?
O2A Nb2 P4 85.3(5) . . ?
O1 Nb2 P4 143.2(3) . . ?
Cl6B Nb2 P4 84.6(7) . . ?
Cl5 Nb2 P4 70.06(13) . . ?
Cl6A Nb2 P4 81.35(17) . . ?
Cl4 Nb2 P4 141.20(13) . . ?
O2B Nb2 P3 81.4(17) . . ?
O2A Nb2 P3 82.7(4) . . ?
O1 Nb2 P3 144.9(3) . . ?
Cl6B Nb2 P3 81.6(6) . . ?
Cl5 Nb2 P3 141.96(14) . . ?
Cl6A Nb2 P3 84.02(15) . . ?
Cl4 Nb2 P3 69.99(13) . . ?
P4 Nb2 P3 71.92(13) . . ?
Nb1 O1 Nb2 177.5(6) . . ?
C3 P1 C2 105.7(7) . . ?
C3 P1 C1 101.8(8) . . ?
C2 P1 C1 103.5(7) . . ?
C3 P1 Nb1 115.9(5) . . ?
C2 P1 Nb1 114.1(5) . . ?
C1 P1 Nb1 114.4(5) . . ?
C9 P2 C10 104.5(8) . . ?
C9 P2 C8 101.4(7) . . ?
C10 P2 C8 104.7(7) . . ?
C9 P2 Nb1 113.4(5) . . ?
C10 P2 Nb1 115.4(5) . . ?
C8 P2 Nb1 115.9(5) . . ?
C14 P3 C13 106.5(8) . . ?
C14 P3 C15 102.7(8) . . ?
C13 P3 C15 102.4(7) . . ?
C14 P3 Nb2 115.9(5) . . ?
C13 P3 Nb2 112.9(5) . . ?
C15 P3 Nb2 115.1(5) . . ?
C21 P4 C20 103.2(7) . . ?
C21 P4 C22 104.8(7) . . ?
C20 P4 C22 102.5(7) . . ?
C21 P4 Nb2 115.5(5) . . ?
C20 P4 Nb2 116.2(5) . . ?
C22 P4 Nb2 113.2(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
C8 C3 C4 C5 -1(2) . . . . ?
P1 C3 C4 C5 171.9(12) . . . . ?
C3 C4 C5 C6 4(2) . . . . ?
C4 C5 C6 C7 -3(2) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C4 C3 C8 C7 -3(2) . . . . ?
P1 C3 C8 C7 -176.4(12) . . . . ?
C4 C3 C8 P2 176.9(12) . . . . ?
P1 C3 C8 P2 3.6(18) . . . . ?
C6 C7 C8 C3 4(2) . . . . ?
C6 C7 C8 P2 -175.8(12) . . . . ?
C20 C15 C16 C17 2(2) . . . . ?
P3 C15 C16 C17 179.3(12) . . . . ?
C15 C16 C17 C18 1(2) . . . . ?
C16 C17 C18 C19 -4(2) . . . . ?
C17 C18 C19 C20 3(2) . . . . ?
C16 C15 C20 C19 -3(2) . . . . ?
P3 C15 C20 C19 179.7(11) . . . . ?
C16 C15 C20 P4 -179.3(11) . . . . ?
P3 C15 C20 P4 3.1(17) . . . . ?
C18 C19 C20 C15 0(2) . . . . ?
C18 C19 C20 P4 176.8(11) . . . . ?
C8 C3 P1 C2 -134.9(13) . . . . ?
C4 C3 P1 C2 52.0(15) . . . . ?
C8 C3 P1 C1 117.3(13) . . . . ?
C4 C3 P1 C1 -55.8(14) . . . . ?
C8 C3 P1 Nb1 -7.5(15) . . . . ?
C4 C3 P1 Nb1 179.4(11) . . . . ?
C3 C8 P2 C9 -121.5(13) . . . . ?
C7 C8 P2 C9 58.6(14) . . . . ?
C3 C8 P2 C10 130.0(13) . . . . ?
C7 C8 P2 C10 -49.9(14) . . . . ?
C3 C8 P2 Nb1 1.8(14) . . . . ?
C7 C8 P2 Nb1 -178.2(11) . . . . ?
C20 C15 P3 C14 119.5(13) . . . . ?
C16 C15 P3 C14 -58.0(14) . . . . ?
C20 C15 P3 C13 -130.2(13) . . . . ?
C16 C15 P3 C13 52.3(14) . . . . ?
C20 C15 P3 Nb2 -7.3(14) . . . . ?
C16 C15 P3 Nb2 175.1(11) . . . . ?
C15 C20 P4 C21 -124.9(13) . . . . ?
C19 C20 P4 C21 58.6(14) . . . . ?
C15 C20 P4 C22 126.5(13) . . . . ?
C19 C20 P4 C22 -50.0(14) . . . . ?
C15 C20 P4 Nb2 2.5(14) . . . . ?
C19 C20 P4 Nb2 -174.0(11) . . . . ?

_refine_diff_density_max         3.438
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.238

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 993849'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_14rwz213
#[NbF4{o-C6H4(AsMe2)2}2]  [NbF6]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 As4 F10 Nb2'
_chemical_formula_weight         947.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'F d d d'
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   12.989(4)
_cell_length_b                   21.329(6)
_cell_length_c                   22.051(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6109(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5669
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      34.7

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3648
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7838
_exptl_absorpt_correction_T_max  0.8615
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  ?
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '

_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'

_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5513
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.99
_reflns_number_total             1510
_reflns_number_gt                1399
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  ?




_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 All hydrogens were placed in calculated positions and refined using a 
 riding model. ADPS were set at 1.2 (CHar), 1.5(CH3) that of the parent 
 atoms. CH3 torsion angles were allowed to refine.

 The diffraction images show significant areas of localised diffuse 
 scattering - these are most likely associated with the disordered NbF6.
 The F thermal parameters were restrained using default shelx (SIM/DELU)
 instructions.

 There are residual electron density peaks associated with the disordered 
 NbF6 but the largest is 0.9 angstroms from F1 - this is difficult to 
 explain unless it is due to a very minor component of  a disorder
 involving the heavy atom positions. Modelling as partially occupied
 -C=O was attempted but proved unsuccessful.


 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1510
_refine_ls_number_parameters     99
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1708
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_restrained_S_all      1.331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.20310(5) 0.56692(3) 0.02351(3) 0.0384(3) Uani 1 1 d . . .
Nb1 Nb 0.1250 0.6250 0.1250 0.0357(4) Uani 1 4 d S . .
Nb2 Nb 0.6250 0.6250 0.1250 0.0308(4) Uani 1 4 d S . .
F1 F 0.0194(3) 0.56229(18) 0.10036(18) 0.0482(9) Uani 1 1 d . . .
C1 C 0.3521(6) 0.5626(3) 0.0177(4) 0.0499(18) Uani 1 1 d . . .
H1A H 0.3796 0.5407 0.0533 0.075 Uiso 1 1 calc R . .
H1B H 0.3804 0.6051 0.0160 0.075 Uiso 1 1 calc R . .
H1C H 0.3714 0.5397 -0.0191 0.075 Uiso 1 1 calc R . .
C2 C 0.1617(7) 0.4799(3) 0.0197(4) 0.0504(17) Uani 1 1 d . . .
H2A H 0.0864 0.4772 0.0206 0.076 Uiso 1 1 calc R . .
H2B H 0.1903 0.4573 0.0545 0.076 Uiso 1 1 calc R . .
H2C H 0.1874 0.4611 -0.0179 0.076 Uiso 1 1 calc R . .
C3 C 0.1596(6) 0.6003(3) -0.0550(3) 0.0438(14) Uani 1 1 d . . .
C4 C 0.1920(6) 0.5752(4) -0.1103(4) 0.0547(19) Uani 1 1 d . . .
H4 H 0.2373 0.5402 -0.1108 0.066 Uiso 1 1 calc R . .
C5 C 0.1594(7) 0.6003(4) -0.1632(3) 0.0536(18) Uani 1 1 d . . .
H5 H 0.1838 0.5838 -0.2005 0.064 Uiso 1 1 calc R . .
F2 F 0.4858(8) 0.6467(6) 0.1139(8) 0.131(5) Uani 0.70 1 d PU . .
F3 F 0.5961(16) 0.6794(11) 0.0699(9) 0.113(7) Uani 0.40 1 d PU . .
F4 F 0.6507(12) 0.6918(8) 0.0649(7) 0.074(4) Uani 0.40 1 d PU . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.935(7) . ?
As1 C1 1.941(7) . ?
As1 C3 1.954(7) . ?
As1 Nb1 2.7518(8) . ?
Nb1 F1 1.991(4) . ?
Nb1 F1 1.991(4) 11_454 ?
Nb1 F1 1.991(4) 14_455 ?
Nb1 F1 1.991(4) 8_554 ?
Nb1 As1 2.7518(8) 8_554 ?
Nb1 As1 2.7518(8) 11_454 ?
Nb1 As1 2.7518(8) 14_455 ?
Nb2 F3 1.721(15) 11_554 ?
Nb2 F3 1.721(15) 8_554 ?
Nb2 F3 1.721(15) 14 ?
Nb2 F3 1.721(15) . ?
Nb2 F2 1.882(10) 11_554 ?
Nb2 F2 1.882(10) 14 ?
Nb2 F2 1.882(10) 8_554 ?
Nb2 F2 1.882(10) . ?
Nb2 F4 1.975(11) 8_554 ?
Nb2 F4 1.975(11) 14 ?
Nb2 F4 1.975(11) 11_554 ?
Nb2 F4 1.975(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C3 1.385(14) 14_455 ?
C3 C4 1.398(10) . ?
C4 C5 1.350(11) . ?
C4 H4 0.9500 . ?
C5 C5 1.382(17) 14_455 ?
C5 H5 0.9500 . ?
F2 F2 1.05(2) 8_554 ?
F3 F4 0.764(18) . ?

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
C2 As1 C1 103.2(3) . . ?
C2 As1 C3 103.3(3) . . ?
C1 As1 C3 104.3(3) . . ?
C2 As1 Nb1 111.4(2) . . ?
C1 As1 Nb1 116.3(2) . . ?
C3 As1 Nb1 116.7(2) . . ?
F1 Nb1 F1 95.6(2) . 11_454 ?
F1 Nb1 F1 148.3(2) . 14_455 ?
F1 Nb1 F1 92.9(2) 11_454 14_455 ?
F1 Nb1 F1 92.9(2) . 8_554 ?
F1 Nb1 F1 148.3(2) 11_454 8_554 ?
F1 Nb1 F1 95.6(2) 14_455 8_554 ?
F1 Nb1 As1 141.10(12) . 8_554 ?
F1 Nb1 As1 80.02(11) 11_454 8_554 ?
F1 Nb1 As1 70.46(12) 14_455 8_554 ?
F1 Nb1 As1 74.31(12) 8_554 8_554 ?
F1 Nb1 As1 74.31(12) . . ?
F1 Nb1 As1 70.46(12) 11_454 . ?
F1 Nb1 As1 80.02(11) 14_455 . ?
F1 Nb1 As1 141.10(12) 8_554 . ?
As1 Nb1 As1 136.74(3) 8_554 . ?
F1 Nb1 As1 70.46(12) . 11_454 ?
F1 Nb1 As1 74.31(12) 11_454 11_454 ?
F1 Nb1 As1 141.10(12) 14_455 11_454 ?
F1 Nb1 As1 80.02(11) 8_554 11_454 ?
As1 Nb1 As1 71.17(3) 8_554 11_454 ?
As1 Nb1 As1 126.49(3) . 11_454 ?
F1 Nb1 As1 80.02(11) . 14_455 ?
F1 Nb1 As1 141.10(12) 11_454 14_455 ?
F1 Nb1 As1 74.31(12) 14_455 14_455 ?
F1 Nb1 As1 70.46(12) 8_554 14_455 ?
As1 Nb1 As1 126.49(3) 8_554 14_455 ?
As1 Nb1 As1 71.17(3) . 14_455 ?
As1 Nb1 As1 136.74(3) 11_454 14_455 ?
F3 Nb2 F3 90.2(18) 11_554 8_554 ?
F3 Nb2 F3 154.8(13) 11_554 14 ?
F3 Nb2 F3 95.3(18) 8_554 14 ?
F3 Nb2 F3 95.3(18) 11_554 . ?
F3 Nb2 F3 154.8(13) 8_554 . ?
F3 Nb2 F3 90.2(18) 14 . ?
F3 Nb2 F2 62.2(8) 11_554 11_554 ?
F3 Nb2 F2 106.4(9) 8_554 11_554 ?
F3 Nb2 F2 92.8(7) 14 11_554 ?
F3 Nb2 F2 97.8(9) . 11_554 ?
F3 Nb2 F2 92.8(7) 11_554 14 ?
F3 Nb2 F2 97.8(9) 8_554 14 ?
F3 Nb2 F2 62.2(8) 14 14 ?
F3 Nb2 F2 106.4(9) . 14 ?
F2 Nb2 F2 32.3(7) 11_554 14 ?
F3 Nb2 F2 106.4(9) 11_554 8_554 ?
F3 Nb2 F2 62.2(8) 8_554 8_554 ?
F3 Nb2 F2 97.8(9) 14 8_554 ?
F3 Nb2 F2 92.8(7) . 8_554 ?
F2 Nb2 F2 165.0(10) 11_554 8_554 ?
F2 Nb2 F2 151.6(9) 14 8_554 ?
F3 Nb2 F2 97.8(9) 11_554 . ?
F3 Nb2 F2 92.8(7) 8_554 . ?
F3 Nb2 F2 106.4(9) 14 . ?
F3 Nb2 F2 62.2(8) . . ?
F2 Nb2 F2 151.6(9) 11_554 . ?
F2 Nb2 F2 165.0(10) 14 . ?
F2 Nb2 F2 32.3(7) 8_554 . ?
F3 Nb2 F4 88.6(9) 11_554 8_554 ?
F3 Nb2 F4 22.6(7) 8_554 8_554 ?
F3 Nb2 F4 87.2(9) 14 8_554 ?
F3 Nb2 F4 175.6(11) . 8_554 ?
F2 Nb2 F4 85.9(7) 11_554 8_554 ?
F2 Nb2 F4 75.4(7) 14 8_554 ?
F2 Nb2 F4 84.1(6) 8_554 8_554 ?
F2 Nb2 F4 115.3(6) . 8_554 ?
F3 Nb2 F4 175.6(11) 11_554 14 ?
F3 Nb2 F4 87.2(9) 8_554 14 ?
F3 Nb2 F4 22.6(7) 14 14 ?
F3 Nb2 F4 88.6(9) . 14 ?
F2 Nb2 F4 115.3(6) 11_554 14 ?
F2 Nb2 F4 84.1(6) 14 14 ?
F2 Nb2 F4 75.4(7) 8_554 14 ?
F2 Nb2 F4 85.9(7) . 14 ?
F4 Nb2 F4 87.5(11) 8_554 14 ?
F3 Nb2 F4 22.6(7) 11_554 11_554 ?
F3 Nb2 F4 88.6(9) 8_554 11_554 ?
F3 Nb2 F4 175.6(11) 14 11_554 ?
F3 Nb2 F4 87.2(9) . 11_554 ?
F2 Nb2 F4 84.1(6) 11_554 11_554 ?
F2 Nb2 F4 115.3(6) 14 11_554 ?
F2 Nb2 F4 85.9(7) 8_554 11_554 ?
F2 Nb2 F4 75.4(7) . 11_554 ?
F4 Nb2 F4 95.7(12) 8_554 11_554 ?
F4 Nb2 F4 160.6(9) 14 11_554 ?
F3 Nb2 F4 87.2(9) 11_554 . ?
F3 Nb2 F4 175.6(11) 8_554 . ?
F3 Nb2 F4 88.6(9) 14 . ?
F3 Nb2 F4 22.6(7) . . ?
F2 Nb2 F4 75.4(7) 11_554 . ?
F2 Nb2 F4 85.9(7) 14 . ?
F2 Nb2 F4 115.3(6) 8_554 . ?
F2 Nb2 F4 84.1(6) . . ?
F4 Nb2 F4 160.6(9) 8_554 . ?
F4 Nb2 F4 95.7(12) 14 . ?
F4 Nb2 F4 87.5(11) 11_554 . ?
As1 C1 H1A 109.5 . . ?
As1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
As1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
As1 C2 H2A 109.5 . . ?
As1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
As1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C3 C4 119.1(5) 14_455 . ?
C3 C3 As1 117.7(2) 14_455 . ?
C4 C3 As1 123.1(6) . . ?
C5 C4 C3 120.5(8) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C5 120.3(5) . 14_455 ?
C4 C5 H5 119.8 . . ?
C5 C5 H5 119.8 14_455 . ?
F2 F2 Nb2 73.9(3) 8_554 . ?
F4 F3 Nb2 98(2) . . ?
F3 F4 Nb2 59.7(15) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.427
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.241
_database_code_depnum_ccdc_archive 'CCDC 993851'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2014wz130a_ml
#[NbF4{o-C6H4(PMe2)2}2]  [NbF6]

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 F10 Nb2 P4'
_chemical_formula_weight         772.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.246(4)
_cell_length_b                   12.325(4)
_cell_length_c                   12.458(4)
_cell_angle_alpha                114.100(3)
_cell_angle_beta                 111.026(2)
_cell_angle_gamma                101.266(2)
_cell_volume                     1467.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4396
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.072
_shelx_estimated_absorpt_T_min   0.830
_shelx_estimated_absorpt_T_max   0.864
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            12736
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.915
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             5703
_reflns_number_gt                4947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 2013)'

_refine_special_details          
;
All hydrogens were placed in calculated positions and refined 
using a riding model. ADPS were set at 1.2 (CHar), 1.5(CH3) that 
of the parent atoms. CH3 torsion angles were allowed to refine.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0611P)²+16.9674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5703
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1862
_refine_ls_wR_factor_gt          0.1839
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.24100(6) 0.11469(6) 0.36403(6) 0.01707(19) Uani 1 1 d . . . . .
P1 P 0.45025(19) 0.25289(19) 0.60133(19) 0.0194(4) Uani 1 1 d . . . . .
P2 P 0.43396(19) 0.2083(2) 0.33279(19) 0.0206(4) Uani 1 1 d . . . . .
P3 P 0.06188(19) -0.11785(19) 0.25127(19) 0.0203(4) Uani 1 1 d . . . . .
P4 P 0.01546(19) 0.12715(19) 0.27761(19) 0.0197(4) Uani 1 1 d . . . . .
F1 F 0.2601(4) 0.2922(4) 0.4131(4) 0.0216(9) Uani 1 1 d . . . . .
F2 F 0.3201(4) -0.0083(4) 0.3647(4) 0.0230(9) Uani 1 1 d . . . . .
F3 F 0.2012(4) 0.1255(4) 0.5054(4) 0.0242(10) Uani 1 1 d . . . . .
F4 F 0.1832(4) 0.0494(4) 0.1724(4) 0.0223(9) Uani 1 1 d . . . . .
C1 C 0.4830(8) 0.1547(8) 0.6743(8) 0.0256(17) Uani 1 1 d . . . . .
H1A H 0.5545 0.2101 0.7668 0.038 Uiso 1 1 calc R U . . .
H1B H 0.5053 0.0886 0.6204 0.038 Uiso 1 1 calc R U . . .
H1C H 0.4071 0.1123 0.6752 0.038 Uiso 1 1 calc R U . . .
C2 C 0.4313(8) 0.3834(8) 0.7193(8) 0.0264(17) Uani 1 1 d . . . . .
H2A H 0.5090 0.4318 0.8075 0.040 Uiso 1 1 calc R U . . .
H2B H 0.3584 0.3475 0.7282 0.040 Uiso 1 1 calc R U . . .
H2C H 0.4161 0.4419 0.6864 0.040 Uiso 1 1 calc R U . . .
C3 C 0.5960(7) 0.3273(8) 0.6056(8) 0.0212(16) Uani 1 1 d . . . . .
C4 C 0.7138(8) 0.4015(8) 0.7247(8) 0.0277(18) Uani 1 1 d . . . . .
H4 H 0.7197 0.4155 0.8078 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8212(8) 0.4539(8) 0.7204(9) 0.0300(19) Uani 1 1 d . . . . .
H5 H 0.9013 0.5027 0.8011 0.036 Uiso 1 1 calc R U . . .
C6 C 0.8150(8) 0.4369(9) 0.6009(10) 0.034(2) Uani 1 1 d . . . . .
H6 H 0.8897 0.4747 0.5998 0.041 Uiso 1 1 calc R U . . .
C7 C 0.6983(8) 0.3641(9) 0.4832(9) 0.0300(19) Uani 1 1 d . . . . .
H7 H 0.6933 0.3528 0.4012 0.036 Uiso 1 1 calc R U . . .
C8 C 0.5893(8) 0.3076(8) 0.4830(8) 0.0259(17) Uani 1 1 d . . . . .
C9 C 0.4592(8) 0.0846(9) 0.2134(9) 0.0303(19) Uani 1 1 d . . . . .
H9A H 0.4950 0.0370 0.2530 0.045 Uiso 1 1 calc R U . . .
H9B H 0.5187 0.1257 0.1923 0.045 Uiso 1 1 calc R U . . .
H9C H 0.3775 0.0243 0.1306 0.045 Uiso 1 1 calc R U . . .
C10 C 0.3996(8) 0.3087(9) 0.2626(9) 0.0283(18) Uani 1 1 d . . . . .
H10A H 0.4678 0.3383 0.2449 0.042 Uiso 1 1 calc R U . . .
H10B H 0.3943 0.3839 0.3269 0.042 Uiso 1 1 calc R U . . .
H10C H 0.3180 0.2579 0.1781 0.042 Uiso 1 1 calc R U . . .
C11 C 0.0860(8) -0.1659(8) 0.3748(8) 0.0271(18) Uani 1 1 d . . . . .
H11A H 0.0239 -0.2545 0.3312 0.041 Uiso 1 1 calc R U . . .
H11B H 0.0745 -0.1065 0.4471 0.041 Uiso 1 1 calc R U . . .
H11C H 0.1727 -0.1627 0.4128 0.041 Uiso 1 1 calc R U . . .
C12 C 0.0660(8) -0.2451(8) 0.1171(8) 0.0287(18) Uani 1 1 d . . . . .
H12A H 0.0098 -0.3293 0.0932 0.043 Uiso 1 1 calc R U . . .
H12B H 0.1535 -0.2398 0.1464 0.043 Uiso 1 1 calc R U . . .
H12C H 0.0367 -0.2358 0.0384 0.043 Uiso 1 1 calc R U . . .
C13 C -0.1025(8) -0.1331(8) 0.1837(8) 0.0234(16) Uani 1 1 d . . . . .
C14 C -0.2058(8) -0.2484(8) 0.1235(8) 0.0281(18) Uani 1 1 d . . . . .
H14 H -0.1922 -0.3244 0.1134 0.034 Uiso 1 1 calc R U . . .
C15 C -0.3295(8) -0.2529(9) 0.0778(8) 0.032(2) Uani 1 1 d . . . . .
H15 H -0.3997 -0.3324 0.0358 0.038 Uiso 1 1 calc R U . . .
C16 C -0.3511(8) -0.1423(10) 0.0932(9) 0.033(2) Uani 1 1 d . . . . .
H16 H -0.4353 -0.1453 0.0631 0.040 Uiso 1 1 calc R U . . .
C17 C -0.2457(8) -0.0249(9) 0.1544(8) 0.0301(19) Uani 1 1 d . . . . .
H17 H -0.2593 0.0512 0.1646 0.036 Uiso 1 1 calc R U . . .
C18 C -0.1236(8) -0.0204(8) 0.1992(8) 0.0270(17) Uani 1 1 d . . . . .
C19 C 0.0072(8) 0.2518(8) 0.4121(8) 0.0254(17) Uani 1 1 d . . . . .
H19A H 0.0228 0.2334 0.4845 0.038 Uiso 1 1 calc R U . . .
H19B H -0.0777 0.2533 0.3774 0.038 Uiso 1 1 calc R U . . .
H19C H 0.0720 0.3363 0.4475 0.038 Uiso 1 1 calc R U . . .
C20 C -0.0125(8) 0.1695(8) 0.1506(8) 0.0253(17) Uani 1 1 d . . . . .
H20A H -0.0931 0.1809 0.1248 0.038 Uiso 1 1 calc R U . . .
H20B H -0.0174 0.1001 0.0712 0.038 Uiso 1 1 calc R U . . .
H20C H 0.0577 0.2506 0.1866 0.038 Uiso 1 1 calc R U . . .
Nb2 Nb 0.75512(6) 0.40270(7) 0.13319(7) 0.0202(2) Uani 1 1 d . . . . .
F5 F 0.6294(5) 0.4249(5) 0.0116(5) 0.0364(12) Uani 1 1 d . . . . .
F6 F 0.7007(6) 0.2300(5) -0.0017(6) 0.0460(14) Uani 1 1 d . . . . .
F7 F 0.8677(5) 0.4567(6) 0.0763(6) 0.0426(14) Uani 1 1 d . . . . .
F8 F 0.8149(5) 0.5772(5) 0.2673(5) 0.0321(11) Uani 1 1 d . . . . .
F9 F 0.6382(5) 0.3490(6) 0.1845(5) 0.0398(13) Uani 1 1 d . . . . .
F10 F 0.8807(5) 0.3846(6) 0.2568(6) 0.0444(14) Uani 1 1 d . . . . .


_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
Nb1 F3 1.952(4) . ?
Nb1 F2 1.952(5) . ?
Nb1 F1 1.955(4) . ?
Nb1 F4 1.960(4) . ?
Nb1 P1 2.637(2) . ?
Nb1 P4 2.642(2) . ?
Nb1 P2 2.651(2) . ?
Nb1 P3 2.654(2) . ?
P1 C2 1.806(8) . ?
P1 C1 1.811(8) . ?
P1 C3 1.811(8) . ?
P2 C8 1.813(8) . ?
P2 C10 1.815(8) . ?
P2 C9 1.815(9) . ?
P3 C12 1.790(8) . ?
P3 C11 1.815(8) . ?
P3 C13 1.817(8) . ?
P4 C20 1.803(8) . ?
P4 C19 1.805(8) . ?
P4 C18 1.818(9) . ?
C3 C4 1.400(11) . ?
C3 C8 1.414(12) . ?
C4 C5 1.377(12) . ?
C5 C6 1.388(13) . ?
C6 C7 1.385(12) . ?
C7 C8 1.379(12) . ?
C13 C14 1.388(11) . ?
C13 C18 1.412(12) . ?
C14 C15 1.394(12) . ?
C15 C16 1.389(14) . ?
C16 C17 1.416(13) . ?
C17 C18 1.375(12) . ?
Nb2 F10 1.872(5) . ?
Nb2 F6 1.877(5) . ?
Nb2 F8 1.877(5) . ?
Nb2 F9 1.879(5) . ?
Nb2 F5 1.889(5) . ?
Nb2 F7 1.890(5) . ?

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
F3 Nb1 F2 95.29(19) . . ?
F3 Nb1 F1 92.86(19) . . ?
F2 Nb1 F1 148.99(19) . . ?
F3 Nb1 F4 149.22(19) . . ?
F2 Nb1 F4 92.78(19) . . ?
F1 Nb1 F4 95.35(19) . . ?
F3 Nb1 P1 69.61(14) . . ?
F2 Nb1 P1 77.10(14) . . ?
F1 Nb1 P1 77.86(13) . . ?
F4 Nb1 P1 141.16(14) . . ?
F3 Nb1 P4 78.11(14) . . ?
F2 Nb1 P4 141.70(14) . . ?
F1 Nb1 P4 69.29(14) . . ?
F4 Nb1 P4 77.21(14) . . ?
P1 Nb1 P4 132.14(7) . . ?
F3 Nb1 P2 140.73(14) . . ?
F2 Nb1 P2 79.97(14) . . ?
F1 Nb1 P2 74.89(14) . . ?
F4 Nb1 P2 69.97(14) . . ?
P1 Nb1 P2 71.35(7) . . ?
P4 Nb1 P2 128.08(7) . . ?
F3 Nb1 P3 75.75(14) . . ?
F2 Nb1 P3 70.44(14) . . ?
F1 Nb1 P3 140.52(14) . . ?
F4 Nb1 P3 79.13(14) . . ?
P1 Nb1 P3 129.33(7) . . ?
P4 Nb1 P3 71.38(7) . . ?
P2 Nb1 P3 135.70(7) . . ?
C2 P1 C1 105.8(4) . . ?
C2 P1 C3 106.0(4) . . ?
C1 P1 C3 105.9(4) . . ?
C2 P1 Nb1 110.8(3) . . ?
C1 P1 Nb1 110.8(3) . . ?
C3 P1 Nb1 116.8(3) . . ?
C8 P2 C10 106.1(4) . . ?
C8 P2 C9 105.0(4) . . ?
C10 P2 C9 104.7(4) . . ?
C8 P2 Nb1 116.9(3) . . ?
C10 P2 Nb1 109.3(3) . . ?
C9 P2 Nb1 113.9(3) . . ?
C12 P3 C11 104.3(4) . . ?
C12 P3 C13 105.6(4) . . ?
C11 P3 C13 105.6(4) . . ?
C12 P3 Nb1 114.1(3) . . ?
C11 P3 Nb1 109.7(3) . . ?
C13 P3 Nb1 116.6(3) . . ?
C20 P4 C19 106.4(4) . . ?
C20 P4 C18 104.5(4) . . ?
C19 P4 C18 106.6(4) . . ?
C20 P4 Nb1 110.3(3) . . ?
C19 P4 Nb1 111.3(3) . . ?
C18 P4 Nb1 117.0(3) . . ?
C4 C3 C8 119.4(7) . . ?
C4 C3 P1 122.5(6) . . ?
C8 C3 P1 118.1(6) . . ?
C5 C4 C3 119.4(8) . . ?
C4 C5 C6 121.5(8) . . ?
C7 C6 C5 119.1(8) . . ?
C8 C7 C6 121.1(9) . . ?
C7 C8 C3 119.5(8) . . ?
C7 C8 P2 123.7(7) . . ?
C3 C8 P2 116.8(6) . . ?
C14 C13 C18 119.5(8) . . ?
C14 C13 P3 122.9(7) . . ?
C18 C13 P3 117.6(6) . . ?
C13 C14 C15 120.3(8) . . ?
C16 C15 C14 120.6(8) . . ?
C15 C16 C17 119.0(8) . . ?
C18 C17 C16 120.4(9) . . ?
C17 C18 C13 120.2(8) . . ?
C17 C18 P4 122.4(7) . . ?
C13 C18 P4 117.4(6) . . ?
F10 Nb2 F6 90.7(3) . . ?
F10 Nb2 F8 88.7(2) . . ?
F6 Nb2 F8 177.9(3) . . ?
F10 Nb2 F9 90.3(3) . . ?
F6 Nb2 F9 90.0(3) . . ?
F8 Nb2 F9 92.0(2) . . ?
F10 Nb2 F5 178.7(3) . . ?
F6 Nb2 F5 90.6(3) . . ?
F8 Nb2 F5 90.0(2) . . ?
F9 Nb2 F5 89.6(2) . . ?
F10 Nb2 F7 91.8(3) . . ?
F6 Nb2 F7 89.7(3) . . ?
F8 Nb2 F7 88.2(2) . . ?
F9 Nb2 F7 177.8(3) . . ?
F5 Nb2 F7 88.3(3) . . ?

_refine_diff_density_max         2.195
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.188

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 993852'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2014wz227b_ml
#[TaF4{o-C6H4(PMe2)2}2] [TaF6]

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H32 F4 P4 Ta, F6 Ta'
_chemical_formula_sum            'C20 H32 F10 P4 Ta2'
_chemical_formula_weight         948.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.253(2)
_cell_length_b                   12.348(2)
_cell_length_c                   12.481(2)
_cell_angle_alpha                114.629(2)
_cell_angle_beta                 110.486(3)
_cell_angle_gamma                101.38(3)
_cell_volume                     1471.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4018
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      27.5

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    7.720
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;



_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14828
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5150
_reflns_number_gt                4574
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 All hydrogens were placed in calculated positions and refined using a 
riding model. ADPS were set at 1.2 (CHar), 1.5(CH3) that of the parent 
atoms. CH3 torsion angles were allowed to refine.

 The residual electron density peaks (Q1-Q4) are located ca. 1A either
 side of the 2 Nb sites.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0505P)²+68.9328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5150
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1857
_refine_ls_wR_factor_gt          0.1840
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta2 Ta -0.24413(6) -0.59694(6) 0.13304(7) 0.0194(2) Uani 1 1 d . . .
F10 F -0.1172(11) -0.6109(12) 0.2566(11) 0.044(3) Uani 1 1 d . . .
F9 F -0.3596(10) -0.6545(11) 0.1843(11) 0.037(3) Uani 1 1 d . . .
F8 F -0.1866(10) -0.4215(9) 0.2690(10) 0.031(2) Uani 1 1 d . . .
F7 F -0.1318(11) -0.5411(11) 0.0758(11) 0.040(3) Uani 1 1 d . . .
F6 F -0.2971(12) -0.7717(11) -0.0048(12) 0.045(3) Uani 1 1 d . . .
F5 F -0.3706(10) -0.5750(11) 0.0133(11) 0.038(3) Uani 1 1 d . . .
Ta1 Ta -1.24062(6) -1.11554(6) -0.36498(6) 0.0165(2) Uani 1 1 d . . .
P4 P -1.0157(4) -1.1299(4) -0.2786(4) 0.0193(8) Uani 1 1 d . . .
P3 P -1.0602(4) -0.8827(4) -0.2514(4) 0.0191(8) Uani 1 1 d . . .
P2 P -1.4345(4) -1.2085(4) -0.3330(4) 0.0193(8) Uani 1 1 d . . .
P1 P -1.4496(4) -1.2516(4) -0.6022(4) 0.0179(8) Uani 1 1 d . . .
F1 F -1.2632(9) -1.2946(9) -0.4168(9) 0.022(2) Uani 1 1 d . . .
F2 F -1.3192(8) -0.9935(9) -0.3656(9) 0.024(2) Uani 1 1 d . . .
F3 F -1.1973(9) -1.1259(9) -0.5042(9) 0.025(2) Uani 1 1 d . . .
F4 F -1.1829(8) -1.0483(9) -0.1724(9) 0.0205(19) Uani 1 1 d . . .
C18 C -0.8779(16) -0.9822(17) -0.1997(16) 0.023(4) Uani 1 1 d . . .
C3 C -1.5949(15) -1.3258(16) -0.6066(17) 0.021(3) Uani 1 1 d . . .
C12 C -1.0638(17) -0.7516(16) -0.1160(17) 0.025(4) Uani 1 1 d . . .
H12A H -0.9998 -0.6685 -0.0855 0.038 Uiso 1 1 calc R . .
H12B H -1.0452 -0.7653 -0.0408 0.038 Uiso 1 1 calc R . .
H12C H -1.1484 -0.7499 -0.1485 0.038 Uiso 1 1 calc R . .
C1 C -1.4819(17) -1.1537(18) -0.6743(18) 0.027(4) Uani 1 1 d . . .
H1A H -1.5511 -1.2099 -0.7676 0.041 Uiso 1 1 calc R . .
H1B H -1.4052 -1.1090 -0.6727 0.041 Uiso 1 1 calc R . .
H1C H -1.5068 -1.0891 -0.6217 0.041 Uiso 1 1 calc R . .
C8 C -1.5889(16) -1.3074(15) -0.4832(19) 0.027(4) Uani 1 1 d . . .
C13 C -0.8974(16) -0.8687(15) -0.1841(16) 0.021(3) Uani 1 1 d . . .
C2 C -1.4343(16) -1.3837(16) -0.7243(16) 0.023(3) Uani 1 1 d . . .
H2A H -1.5129 -1.4316 -0.8110 0.034 Uiso 1 1 calc R . .
H2B H -1.4189 -1.4427 -0.6929 0.034 Uiso 1 1 calc R . .
H2C H -1.3627 -1.3485 -0.7353 0.034 Uiso 1 1 calc R . .
C19 C -1.0044(16) -1.2557(16) -0.4119(16) 0.024(4) Uani 1 1 d . . .
H19A H -1.0180 -1.2379 -0.4840 0.035 Uiso 1 1 calc R . .
H19B H -1.0694 -1.3405 -0.4481 0.035 Uiso 1 1 calc R . .
H19C H -0.9198 -1.2566 -0.3756 0.035 Uiso 1 1 calc R . .
C9 C -1.4604(17) -1.0850(18) -0.2133(19) 0.030(4) Uani 1 1 d . . .
H9A H -1.4972 -1.0385 -0.2528 0.045 Uiso 1 1 calc R . .
H9B H -1.3790 -1.0234 -0.1310 0.045 Uiso 1 1 calc R . .
H9C H -1.5189 -1.1263 -0.1913 0.045 Uiso 1 1 calc R . .
C20 C -0.9899(17) -1.1729(17) -0.1528(17) 0.024(4) Uani 1 1 d . . .
H20A H -0.9090 -1.1830 -0.1260 0.036 Uiso 1 1 calc R . .
H20B H -1.0596 -1.2551 -0.1902 0.036 Uiso 1 1 calc R . .
H20C H -0.9870 -1.1041 -0.0739 0.036 Uiso 1 1 calc R . .
C15 C -0.6697(17) -0.7500(18) -0.0784(19) 0.032(4) Uani 1 1 d . . .
H15 H -0.5991 -0.6715 -0.0389 0.038 Uiso 1 1 calc R . .
C14 C -0.7929(16) -0.7546(18) -0.1230(18) 0.029(4) Uani 1 1 d . . .
H14 H -0.8054 -0.6777 -0.1113 0.035 Uiso 1 1 calc R . .
C11 C -1.0799(17) -0.8327(17) -0.3718(16) 0.025(4) Uani 1 1 d . . .
H11A H -1.0158 -0.7445 -0.3267 0.037 Uiso 1 1 calc R . .
H11B H -1.1652 -0.8335 -0.4088 0.037 Uiso 1 1 calc R . .
H11C H -1.0693 -0.8929 -0.4450 0.037 Uiso 1 1 calc R . .
C10 C -1.4045(17) -1.3104(18) -0.2672(19) 0.028(4) Uani 1 1 d . . .
H10A H -1.4700 -1.3344 -0.2438 0.042 Uiso 1 1 calc R . .
H10B H -1.3206 -1.2630 -0.1865 0.042 Uiso 1 1 calc R . .
H10C H -1.4064 -1.3893 -0.3354 0.042 Uiso 1 1 calc R . .
C5 C -1.8205(17) -1.4518(17) -0.7212(19) 0.029(4) Uani 1 1 d . . .
H5 H -1.9004 -1.5002 -0.8014 0.035 Uiso 1 1 calc R . .
C6 C -1.8137(17) -1.4344(19) -0.5991(19) 0.031(4) Uani 1 1 d . . .
H6 H -1.8878 -1.4718 -0.5967 0.037 Uiso 1 1 calc R . .
C17 C -0.7562(17) -0.9768(18) -0.1528(18) 0.028(4) Uani 1 1 d . . .
H17 H -0.7430 -1.0527 -0.1617 0.034 Uiso 1 1 calc R . .
C16 C -0.6515(17) -0.8612(19) -0.0923(17) 0.031(4) Uani 1 1 d . . .
H16 H -0.5679 -0.8590 -0.0608 0.037 Uiso 1 1 calc R . .
C7 C -1.6980(17) -1.3623(17) -0.4848(19) 0.030(4) Uani 1 1 d . . .
H7 H -1.6933 -1.3499 -0.4027 0.036 Uiso 1 1 calc R . .
C4 C -1.7119(16) -1.3991(16) -0.7250(18) 0.025(4) Uani 1 1 d . . .
H4 H -1.7172 -1.4129 -0.8078 0.030 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Ta2 F10 1.864(11) . ?
Ta2 F9 1.879(10) . ?
Ta2 F8 1.888(9) . ?
Ta2 F5 1.895(10) . ?
Ta2 F7 1.898(11) . ?
Ta2 F6 1.900(11) . ?
Ta1 F2 1.944(9) . ?
Ta1 F3 1.950(10) . ?
Ta1 F1 1.955(9) . ?
Ta1 F4 1.970(9) . ?
Ta1 P1 2.645(4) . ?
Ta1 P4 2.657(4) . ?
Ta1 P3 2.658(4) . ?
Ta1 P2 2.664(4) . ?
P4 C20 1.806(17) . ?
P4 C18 1.809(17) . ?
P4 C19 1.814(16) . ?
P3 C11 1.810(16) . ?
P3 C12 1.811(17) . ?
P3 C13 1.812(18) . ?
P2 C10 1.795(17) . ?
P2 C9 1.811(19) . ?
P2 C8 1.812(18) . ?
P1 C3 1.804(17) . ?
P1 C2 1.809(15) . ?
P1 C1 1.809(17) . ?
C18 C17 1.37(2) . ?
C18 C13 1.41(2) . ?
C3 C4 1.40(2) . ?
C3 C8 1.43(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C8 C7 1.36(3) . ?
C13 C14 1.38(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C15 C16 1.38(3) . ?
C15 C14 1.39(3) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 C4 1.39(3) . ?
C5 C6 1.42(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.37(3) . ?
C6 H6 0.9500 . ?
C17 C16 1.40(3) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C7 H7 0.9500 . ?
C4 H4 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
F10 Ta2 F9 90.1(5) . . ?
F10 Ta2 F8 88.0(5) . . ?
F9 Ta2 F8 92.3(5) . . ?
F10 Ta2 F5 177.5(5) . . ?
F9 Ta2 F5 90.1(5) . . ?
F8 Ta2 F5 89.5(5) . . ?
F10 Ta2 F7 91.5(6) . . ?
F9 Ta2 F7 178.2(5) . . ?
F8 Ta2 F7 88.7(5) . . ?
F5 Ta2 F7 88.4(5) . . ?
F10 Ta2 F6 91.6(5) . . ?
F9 Ta2 F6 89.7(5) . . ?
F8 Ta2 F6 178.0(5) . . ?
F5 Ta2 F6 90.9(5) . . ?
F7 Ta2 F6 89.3(5) . . ?
F2 Ta1 F3 95.5(4) . . ?
F2 Ta1 F1 147.9(4) . . ?
F3 Ta1 F1 93.0(4) . . ?
F2 Ta1 F4 92.9(4) . . ?
F3 Ta1 F4 148.1(4) . . ?
F1 Ta1 F4 96.0(4) . . ?
F2 Ta1 P1 75.9(3) . . ?
F3 Ta1 P1 70.4(3) . . ?
F1 Ta1 P1 77.9(3) . . ?
F4 Ta1 P1 141.4(3) . . ?
F2 Ta1 P4 142.4(3) . . ?
F3 Ta1 P4 77.7(3) . . ?
F1 Ta1 P4 69.7(3) . . ?
F4 Ta1 P4 76.9(3) . . ?
P1 Ta1 P4 132.74(13) . . ?
F2 Ta1 P3 71.0(3) . . ?
F3 Ta1 P3 75.1(3) . . ?
F1 Ta1 P3 141.1(3) . . ?
F4 Ta1 P3 78.8(3) . . ?
P1 Ta1 P3 128.77(13) . . ?
P4 Ta1 P3 71.53(13) . . ?
F2 Ta1 P2 79.8(3) . . ?
F3 Ta1 P2 141.7(3) . . ?
F1 Ta1 P2 74.4(3) . . ?
F4 Ta1 P2 70.1(3) . . ?
P1 Ta1 P2 71.61(13) . . ?
P4 Ta1 P2 127.58(13) . . ?
P3 Ta1 P2 135.74(13) . . ?
C20 P4 C18 104.8(8) . . ?
C20 P4 C19 105.5(8) . . ?
C18 P4 C19 106.5(8) . . ?
C20 P4 Ta1 110.5(6) . . ?
C18 P4 Ta1 116.3(6) . . ?
C19 P4 Ta1 112.4(6) . . ?
C11 P3 C12 103.2(8) . . ?
C11 P3 C13 105.2(8) . . ?
C12 P3 C13 105.6(8) . . ?
C11 P3 Ta1 110.7(6) . . ?
C12 P3 Ta1 114.6(6) . . ?
C13 P3 Ta1 116.4(5) . . ?
C10 P2 C9 105.0(9) . . ?
C10 P2 C8 105.4(8) . . ?
C9 P2 C8 104.8(9) . . ?
C10 P2 Ta1 109.9(6) . . ?
C9 P2 Ta1 114.3(6) . . ?
C8 P2 Ta1 116.5(7) . . ?
C3 P1 C2 105.3(8) . . ?
C3 P1 C1 105.8(8) . . ?
C2 P1 C1 104.9(8) . . ?
C3 P1 Ta1 116.7(6) . . ?
C2 P1 Ta1 111.6(6) . . ?
C1 P1 Ta1 111.7(6) . . ?
C17 C18 C13 119.6(16) . . ?
C17 C18 P4 122.2(14) . . ?
C13 C18 P4 118.2(13) . . ?
C4 C3 C8 119.3(15) . . ?
C4 C3 P1 122.5(13) . . ?
C8 C3 P1 118.2(12) . . ?
P3 C12 H12A 109.5 . . ?
P3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C8 C3 118.9(16) . . ?
C7 C8 P2 124.2(16) . . ?
C3 C8 P2 116.9(13) . . ?
C14 C13 C18 119.0(16) . . ?
C14 C13 P3 123.4(13) . . ?
C18 C13 P3 117.6(12) . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P4 C19 H19A 109.5 . . ?
P4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P4 C20 H20A 109.5 . . ?
P4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C15 C14 119.2(17) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C13 C14 C15 121.4(18) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
P3 C11 H11A 109.5 . . ?
P3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C5 C6 120.8(16) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 118.3(16) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C18 C17 C16 120.9(18) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C15 C16 C17 119.9(17) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C8 C7 C6 123.1(18) . . ?
C8 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
C5 C4 C3 119.6(17) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         4.914
_refine_diff_density_min         -2.264
_refine_diff_density_rms         0.349
_database_code_depnum_ccdc_archive 'CCDC 993853'
