# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

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

data_pos-1100k
_database_code_depnum_ccdc_archive 'CCDC 1865475'
_audit_update_record             
;
2018-09-01 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_audit_creation_date             2018-08-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C25 H16 O12 S4), 32(H2 O), 8(C8 H12 N4)'
_chemical_formula_sum            'C164 H224 N32 O80 S16'
_chemical_formula_weight         4436.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1212 0.1207 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.7276(5)
_cell_length_b                   25.7276(5)
_cell_length_c                   7.7202(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5110.1(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    12827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2830
_cell_measurement_theta_min      2.1970
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.733
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.022
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24962
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.939
_diffrn_reflns_theta_min         2.205
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ      0.00 360.00   0.30    0.50   0.00   0.00   0.00    --  1200
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0074110000
_diffrn_orient_matrix_UB_12      0.0262150000
_diffrn_orient_matrix_UB_13      -0.0001164000
_diffrn_orient_matrix_UB_21      -0.0201599000
_diffrn_orient_matrix_UB_22      0.0055886000
_diffrn_orient_matrix_UB_23      0.0576307000
_diffrn_orient_matrix_UB_31      0.0166955000
_diffrn_orient_matrix_UB_32      -0.0046794000
_diffrn_orient_matrix_UB_33      0.0700128000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2436
_reflns_number_total             2609
_reflns_odcompleteness_completeness 90.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.59
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0860P)²+6.1650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1429
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups, All N(H,H) groups
2.a Free rotating group:
 O005(O006)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00D(H00D), C00F(H00H), C00I(H00I)
2.c X=CH2 refined with riding coordinates:
 N007(H00C,H00E), N008(H00F,H00G)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S001 S 0.39514(2) 0.61363(2) 0.57648(6) 0.01905(19) Uani 1 1 d . . . . .
O002 O 0.43170(5) 0.57139(5) 0.54182(18) 0.0229(3) Uani 1 1 d . . . . .
O003 O 0.34451(5) 0.59408(5) 0.64127(19) 0.0278(3) Uani 1 1 d . . . . .
O004 O 0.38826(5) 0.64930(5) 0.43145(18) 0.0267(3) Uani 1 1 d . . . . .
O005 O 0.27068(6) 0.54885(6) 0.42848(17) 0.0317(4) Uani 1 1 d . . . . .
O006 O 0.35423(6) 0.54488(6) 0.95940(17) 0.0349(4) Uani 1 1 d G . . . .
N007 N 0.28282(6) 0.66080(6) -0.1108(2) 0.0231(4) Uani 1 1 d . . . . .
H00C H 0.297435 0.636597 -0.174934 0.028 Uiso 1 1 calc R . . . .
H00E H 0.256909 0.679284 -0.152506 0.028 Uiso 1 1 calc R . . . .
N008 N 0.33832(6) 0.64258(6) 0.1147(2) 0.0239(4) Uani 1 1 d . . . . .
H00F H 0.353526 0.618187 0.052938 0.029 Uiso 1 1 calc R . . . .
H00G H 0.348972 0.648977 0.220928 0.029 Uiso 1 1 calc R . . . .
C009 C 0.41252(7) 0.70497(7) 0.7519(2) 0.0210(4) Uani 1 1 d . . . . .
H009 H 0.389699 0.720530 0.670281 0.025 Uiso 1 1 calc R . . . .
C00A C 0.45507(7) 0.62837(6) 0.8685(2) 0.0197(4) Uani 1 1 d . . . . .
H00A H 0.461211 0.591968 0.865643 0.024 Uiso 1 1 calc R . . . .
C00B C 0.43641(7) 0.73503(6) 0.8782(2) 0.0195(4) Uani 1 1 d . . . . .
H00B H 0.429778 0.771343 0.881781 0.023 Uiso 1 1 calc R . . . .
C00C C 0.47029(6) 0.71286(6) 1.0012(2) 0.0162(4) Uani 1 1 d . . . . .
C00D C 0.47866(6) 0.65910(6) 0.9952(2) 0.0194(4) Uani 1 1 d . . . . .
H00D H 0.500717 0.643292 1.078664 0.023 Uiso 1 1 calc R . . . .
C00E C 0.42242(6) 0.65138(6) 0.7461(2) 0.0178(4) Uani 1 1 d . . . . .
C00F C 0.25972(7) 0.75780(7) 0.0731(3) 0.0229(4) Uani 1 1 d . . . . .
H00H H 0.266392 0.763020 -0.046675 0.027 Uiso 1 1 calc R . . . .
C00G C 0.27451(6) 0.71119(7) 0.1534(2) 0.0202(4) Uani 1 1 d . . . . .
C00H C 0.29982(7) 0.66940(7) 0.0485(3) 0.0209(4) Uani 1 1 d . . . . .
C00I C 0.23513(7) 0.79653(7) 0.1701(3) 0.0232(4) Uani 1 1 d . . . . .
H00I H 0.224952 0.828112 0.116085 0.028 Uiso 1 1 calc R . . . .
C00J C 0.500000 0.750000 1.125000 0.0164(7) Uani 1 4 d S T P . .
H00L H 0.3441(8) 0.5488(8) 0.840(3) 0.020 Uiso 1 1 d R . . . .
H00M H 0.3312(8) 0.5195(8) 1.013(3) 0.020 Uiso 1 1 d R . . . .
H00J H 0.2955(9) 0.5623(8) 0.483(3) 0.020 Uiso 1 1 d R . . . .
H00K H 0.2516(9) 0.5362(8) 0.510(3) 0.020 Uiso 1 1 d R . . . .


_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
S001 O002 1.4620(13) . ?
S001 O003 1.4833(13) . ?
S001 O004 1.4585(14) . ?
S001 C00E 1.7748(17) . ?
O005 H00J 0.84(2) . ?
O005 H00K 0.86(2) . ?
O006 H00L 0.96(2) . ?
O006 H00M 0.97(2) . ?
N007 H00C 0.8800 . ?
N007 H00E 0.8800 . ?
N007 C00H 1.324(3) . ?
N008 H00F 0.8800 . ?
N008 H00G 0.8800 . ?
N008 C00H 1.311(2) . ?
C009 H009 0.9500 . ?
C009 C00B 1.388(3) . ?
C009 C00E 1.403(2) . ?
C00A H00A 0.9500 . ?
C00A C00D 1.397(3) . ?
C00A C00E 1.396(2) . ?
C00B H00B 0.9500 . ?
C00B C00C 1.410(2) . ?
C00C C00D 1.400(2) . ?
C00C C00J 1.5526(16) . ?
C00D H00D 0.9500 . ?
C00F H00H 0.9500 . ?
C00F C00G 1.403(3) . ?
C00F C00I 1.398(3) . ?
C00G C00H 1.495(2) . ?
C00G C00I 1.399(3) 13_565 ?
C00I H00I 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
O002 S001 O003 112.00(8) . . ?
O002 S001 C00E 106.70(8) . . ?
O003 S001 C00E 106.50(8) . . ?
O004 S001 O002 113.92(8) . . ?
O004 S001 O003 111.45(8) . . ?
O004 S001 C00E 105.67(8) . . ?
H00J O005 H00K 103(2) . . ?
H00L O006 H00M 108.0(18) . . ?
H00C N007 H00E 120.0 . . ?
C00H N007 H00C 120.0 . . ?
C00H N007 H00E 120.0 . . ?
H00F N008 H00G 120.0 . . ?
C00H N008 H00F 120.0 . . ?
C00H N008 H00G 120.0 . . ?
C00B C009 H009 120.3 . . ?
C00B C009 C00E 119.35(16) . . ?
C00E C009 H009 120.3 . . ?
C00D C00A H00A 120.1 . . ?
C00E C00A H00A 120.1 . . ?
C00E C00A C00D 119.71(15) . . ?
C009 C00B H00B 119.3 . . ?
C009 C00B C00C 121.43(15) . . ?
C00C C00B H00B 119.3 . . ?
C00B C00C C00J 118.04(13) . . ?
C00D C00C C00B 118.19(15) . . ?
C00D C00C C00J 123.54(14) . . ?
C00A C00D C00C 121.03(16) . . ?
C00A C00D H00D 119.5 . . ?
C00C C00D H00D 119.5 . . ?
C009 C00E S001 119.33(13) . . ?
C00A C00E S001 120.36(13) . . ?
C00A C00E C009 120.27(16) . . ?
C00G C00F H00H 120.1 . . ?
C00I C00F H00H 120.1 . . ?
C00I C00F C00G 119.71(18) . . ?
C00F C00G C00H 119.58(17) . . ?
C00I C00G C00F 120.25(17) 13_565 . ?
C00I C00G C00H 120.16(17) 13_565 . ?
N007 C00H C00G 118.64(16) . . ?
N008 C00H N007 121.58(17) . . ?
N008 C00H C00G 119.77(17) . . ?
C00F C00I C00G 120.05(18) . 13_565 ?
C00F C00I H00I 120.0 . . ?
C00G C00I H00I 120.0 13_565 . ?
C00C C00J C00C 112.27(6) 16_657 . ?
C00C C00J C00C 112.26(7) 16_657 3_665 ?
C00C C00J C00C 104.02(12) 16_657 14_567 ?
C00C C00J C00C 112.26(6) 3_665 14_567 ?
C00C C00J C00C 104.02(12) 3_665 . ?
C00C C00J C00C 112.26(7) 14_567 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.728
_oxdiff_exptl_absorpt_empirical_full_min 0.700
# start Validation Reply Form
_vrf_PLAT029_ALERT_3_A           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.907
RESPONSE: The crystals are extremely this and difficult to work 
with. Furthermore, upon cooling CPOS-5 undergoes a unit-cell 
expansion which further deteriorates the crystal and thus 
made it difficult to obtain high angle reflexions.
;
_vrf_PLAT245_ALERT_2_C           
;
PROBLEM: U(iso) H00M Smaller than U(eq) O006 by 0.015 Ang**2
RESPONSE: Hydrogen atoms are not refined anisotropically
;
_vrf_PLAT245_pos-1100k           
;
PROBLEM: U(iso) H00J      Smaller than U(eq) O005      by      0.012 Ang**2
RESPONSE: Hydrogen atoms are not refined anisotropically
;
_vrf_PLAT790_ALERT_4_C           
;
PROBLEM: Centre of Gravity not Within Unit Cell: Resd. # 1 Note C25 H16 O12 S4
RESPONSE: The unit-cell c-axis is very small and some part of the molecule 
lies outside to visualize complete molecules instead of fragments.
;
_vrf_PLAT790_cpos-5100k          
;
PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note  
RESPONSE: The molecular fragment is large and the cross the short 
unit-cell c-axis. 
;
_vrf_PLAT911_ALERT_3_C           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 3 Report
RESPONSE: The crystals grow as very thin needles. This resulted in 
difficulty obtaining high angle reflections. 
;
_vrf_PLAT911_cpos-5100k          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 3 Report
RESPONSE: The crystals grow as very thin needles. This resulted in 
difficulty obtaining high angle reflections. 
;
_vrf_PLAT977_ALERT_2_C           
;
PROBLEM: Check Negative Difference Density on H00J -0.33 eA-3
RESPONSE: The negative density is very low and the hydrogen 
atoms are not refined anisotropically and the afix commands 
are correct. Additionally, the crystal are very thin needles 
which limited the high angle reflections and thus the 
resolution.
;
_vrf_PLAT977_cpos-5100k          
;
PROBLEM: Check Negative Difference Density on H00J             -0.33 eA-3  
RESPONSE: The negative density is very low, and the hydrogen atoms are 
not refined anisotropically and the afix commands hare correct. 
Additionally, the crystal are very thin needles which limited the high 
angle reflections and thus the resolution.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pos-1273k
_database_code_depnum_ccdc_archive 'CCDC 1865476'
_audit_update_record             
;
2018-09-01 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_audit_creation_date             2018-08-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6

_chemical_name_common            ?
_chemical_name_systematic        'POS-1 273K'
_chemical_formula_moiety         '4(C25 H16 O12 S4), 8(C8 H12 N4)'
_chemical_formula_sum            'C164 H160 N32 O48 S16'
_chemical_formula_weight         3860.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.1179(7)
_cell_length_b                   25.1179(7)
_cell_length_c                   7.6702(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4839.2(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3468
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.78
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.831
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.733
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.022
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6929
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         2.293
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1413
_reflns_number_total             2116
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2116
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0936
_refine_ls_restrained_S_all      1.322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2728
_refine_ls_wR_factor_ref         0.3100
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C3-H3
 1.08 with sigma of 0.01
 C4-H4
 1.08 with sigma of 0.01
 C6-H6
 1.08 with sigma of 0.01
 C7-H7
 1.08 with sigma of 0.01
 C8-H8
 1.08 with sigma of 0.01
 C10-H10
 1.08 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10)
3.b X=CH2 refined with riding coordinates:
 N1(H1a,H1b), N2(H2a,H2b)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.11019(6) 0.38935(5) 0.08407(19) 0.0459(6) Uani 1 1 d . . . A 1
O1 O 0.1250(2) 0.35333(19) -0.0531(7) 0.0837(17) Uani 1 1 d . . . A 1
O2 O 0.15459(19) 0.4150(2) 0.1686(8) 0.0897(18) Uani 1 1 d . . . A 1
O3 O 0.07128(16) 0.42791(15) 0.0279(5) 0.0495(10) Uani 1 1 d . . . A 1
C1 C 0.000000 0.250000 0.625000 0.033(2) Uani 1 4 d S T P A 1
C2 C 0.03052(19) 0.28767(18) 0.4996(6) 0.0318(11) Uani 1 1 d . . . A 1
C3 C 0.0668(2) 0.2658(2) 0.3839(6) 0.0388(12) Uani 1 1 d D . . A 1
H3 H 0.074199 0.229559 0.390514 0.047 Uiso 1 1 calc DR . . A 1
C4 C 0.0920(2) 0.2959(2) 0.2598(6) 0.0415(13) Uani 1 1 d D . . A 1
H4 H 0.1200(16) 0.2782(19) 0.171(6) 0.050 Uiso 1 1 d DR . . B 1
C5 C 0.07889(19) 0.35036(19) 0.2459(6) 0.0354(12) Uani 1 1 d . . . A 1
C6 C 0.0433(2) 0.3725(2) 0.3581(7) 0.0405(13) Uani 1 1 d D . . A 1
H6 H 0.0270(19) 0.4116(9) 0.344(7) 0.049 Uiso 1 1 d DR . . C 1
C7 C 0.0185(2) 0.3412(2) 0.4846(7) 0.0393(13) Uani 1 1 d D . . A 1
H7 H -0.0134(15) 0.3615(19) 0.550(7) 0.047 Uiso 1 1 d DR . . D 1
N1 N 0.1658(2) 0.3643(2) -0.3813(7) 0.0629(15) Uani 1 1 d . . . E 1
H1A H 0.151649 0.389424 -0.441463 0.076 Uiso 1 1 calc R . . E 1
H1B H 0.155817 0.358930 -0.275462 0.076 Uiso 1 1 calc R . . E 1
N2 N 0.21771(19) 0.3422(2) -0.6112(7) 0.0596(14) Uani 1 1 d . . . E 1
H2A H 0.203818 0.367276 -0.672680 0.072 Uiso 1 1 calc R . . E 1
H2B H 0.241917 0.322134 -0.655491 0.072 Uiso 1 1 calc R . . E 1
C8 C 0.2428(2) 0.2996(2) -0.1748(7) 0.0469(14) Uani 1 1 d D . . E 1
H8 H 0.238556 0.333028 -0.124750 0.056 Uiso 1 1 calc DR . . E 1
C9 C 0.22627(19) 0.2909(2) -0.3453(6) 0.0391(12) Uani 1 1 d . . . E 1
C10 C 0.2344(2) 0.2410(2) -0.4209(7) 0.0451(14) Uani 1 1 d D . . E 1
H10 H 0.224535 0.235092 -0.536116 0.054 Uiso 1 1 calc DR . . E 1
C11 C 0.2019(2) 0.3346(2) -0.4493(8) 0.0491(14) Uani 1 1 d . . . E 1


_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
S1 O1 1.437(5) . ?
S1 O2 1.442(5) . ?
S1 O3 1.442(4) . ?
S1 C5 1.766(5) . ?
C1 C2 1.552(5) 3 ?
C1 C2 1.552(5) . ?
C1 C2 1.552(5) 14_556 ?
C1 C2 1.552(5) 16_556 ?
C2 C3 1.385(7) . ?
C2 C7 1.382(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.372(7) . ?
C4 H4 1.075(10) . ?
C4 C5 1.410(7) . ?
C5 C6 1.359(7) . ?
C6 H6 1.071(10) . ?
C6 C7 1.395(7) . ?
C7 H7 1.075(10) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C11 1.283(7) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C11 1.318(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(7) . ?
C8 C10 1.380(8) 13_554 ?
C9 C10 1.397(7) . ?
C9 C11 1.489(8) . ?
C10 H10 0.9300 . ?

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 S1 O2 114.2(4) . . ?
O1 S1 O3 112.3(3) . . ?
O1 S1 C5 106.3(2) . . ?
O2 S1 C5 106.0(3) . . ?
O3 S1 O2 111.0(3) . . ?
O3 S1 C5 106.3(2) . . ?
C2 C1 C2 103.4(3) 14_556 16_556 ?
C2 C1 C2 103.4(3) 3 . ?
C2 C1 C2 112.59(17) 16_556 . ?
C2 C1 C2 112.59(17) 3 16_556 ?
C2 C1 C2 112.59(17) 3 14_556 ?
C2 C1 C2 112.59(17) 14_556 . ?
C3 C2 C1 118.7(4) . . ?
C7 C2 C1 122.5(4) . . ?
C7 C2 C3 118.4(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 121.9(5) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 121(3) . . ?
C3 C4 C5 118.7(5) . . ?
C5 C4 H4 120(3) . . ?
C4 C5 S1 119.2(4) . . ?
C6 C5 S1 120.8(4) . . ?
C6 C5 C4 120.1(4) . . ?
C5 C6 H6 124(3) . . ?
C5 C6 C7 120.3(5) . . ?
C7 C6 H6 115(3) . . ?
C2 C7 C6 120.6(5) . . ?
C2 C7 H7 126(3) . . ?
C6 C7 H7 113(3) . . ?
H1A N1 H1B 120.0 . . ?
C11 N1 H1A 120.0 . . ?
C11 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C11 N2 H2A 120.0 . . ?
C11 N2 H2B 120.0 . . ?
C9 C8 H8 119.7 . . ?
C10 C8 H8 119.7 13_554 . ?
C10 C8 C9 120.6(5) 13_554 . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 C11 120.8(5) . . ?
C10 C9 C11 120.0(5) . . ?
C8 C10 C9 120.2(5) 13_554 . ?
C8 C10 H10 119.9 13_554 . ?
C9 C10 H10 119.9 . . ?
N1 C11 N2 120.8(6) . . ?
N1 C11 C9 120.0(5) . . ?
N2 C11 C9 119.2(5) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.000 -0.573 193.7 37.5 3.75Water
2 0.250 0.500 -0.960 193.7 37.5 3.75Water
3 0.750 0.000 -0.471 193.7 37.5 3.75Water
4 0.750 0.500 -0.517 193.7 37.5 3.75Water



_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT084_pos-1273k           
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.31 Report
RESPONSE: The crystals of CPOS-5 are very thin needles which resulted in 
difficulty obtain high resolution reflection data and affected the data 
quality.
;
_vrf_PLAT242_cpos-5273k          
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         S1 Check 
RESPONSE: The surrounding oxygen atoms attached to S1 can oscillate around 
S1 thus increasing their Ueq.
;
_vrf_PLAT340_cpos-5273k          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00643 Ang.  
RESPONSE: The crystals of CPOS-5 are very thin needles which resulted in 
difficulty obtain high resolution reflection data and affected the data 
quality.
;
_vrf_PLAT420_cpos-5273k          
;
PROBLEM: D-H Without Acceptor       N1       --H1A            Please Check 
RESPONSE: This D-H does not form a hydrogen bond within the structure 
and is directed in towards the channel.
;
_vrf_PLAT905_cpos-5273k          
;
PROBLEM: Negative K value in the Analysis of Variance ...     -0.372 Report
RESPONSE: The crystals of CPOS-5 are very thin needles which resulted in 
difficulty obtain good diffraction. Problems were found with the scaling 
procedure and could not be performed. Thus, the GOOF and Analysis 
of Variance are adversely affected.
;
_vrf_PLAT911_cpos-5273k          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595         22 Report
RESPONSE: The crystals of CPOS-5 are very thin needles which resulted in 
difficulty obtain high resolution reflection data and affected the data 
quality.
;
_vrf_PLAT918_cpos-5273k          
;
PROBLEM: Reflection(s) with I(obs) much Smaller I(calc) .          1 Check 
RESPONSE: The error/ESD for the refelctions where not large enough to 
justify omission.
;

# end Validation Reply Form
