#------------------------------------------------------------------------------
#$Date: 2024-03-04 22:42:16 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/97/7159773.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7159773
loop_
_publ_author_name
'Agrawal, Abhijeet R.'
'Shiouki, Israa'
'Deree, Yinon'
'Bogoslavsky, Benny'
'Gidron, Ori'
_publ_section_title
;
 Controlling helicene's pitch by molecular tethering
;
_journal_issue                   7
_journal_name_full               'Organic & Biomolecular Chemistry'
_journal_page_first              1365
_journal_page_last               1368
_journal_paper_doi               10.1039/D3OB02075D
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C46 H40 O2, C0.667 Cl2'
_chemical_formula_sum            'C46.67 H40 Cl2 O2'
_chemical_formula_weight         703.66
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-23
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2024-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                92.762(3)
_cell_angle_beta                 99.839(3)
_cell_angle_gamma                103.088(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2461(3)
_cell_length_b                   11.4386(4)
_cell_length_c                   15.5025(5)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.0330
_cell_measurement_theta_min      2.2950
_cell_volume                     1906.00(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  40.00   0.50  195.00    --    8.37 -99.00-120.00   52
  2  ω    -17.00  25.00   0.50  195.00    --    8.37 -99.00-180.00   84
  3  ω    -10.00  16.00   0.50  195.00    --    8.37 -99.00  60.00   52
  4  ω    -47.00  36.00   0.50  195.00    --   -9.62   0.00 -60.00  166
  5  ω    -82.00  -2.00   0.50  195.00    --   -9.62 -57.00  90.00  160
  6  ω    -81.00   4.00   0.50  195.00    --   -9.62 -57.00 -30.00  170
  7  ω    -82.00   9.00   0.50  195.00    --   -9.62 -77.00-120.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0140027000
_diffrn_orient_matrix_UB_12      0.0637838000
_diffrn_orient_matrix_UB_13      0.0012027000
_diffrn_orient_matrix_UB_21      -0.0190353000
_diffrn_orient_matrix_UB_22      -0.0042276000
_diffrn_orient_matrix_UB_23      -0.0463141000
_diffrn_orient_matrix_UB_31      -0.0615320000
_diffrn_orient_matrix_UB_32      -0.0005064000
_diffrn_orient_matrix_UB_33      0.0052680000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25907
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.301
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0667
_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)+(0.0904P)²+1.1547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6383
_reflns_number_total             8311
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ob02075d2.cif
_cod_data_source_block           origi114
_cod_depositor_comments
'Adding full bibliography for 7159772--7159774.cif.'
_cod_database_code               7159773
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H44 O2 Cl2'
_chemical_oxdiff_usercomment     Hep_C4
_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.
;
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.2) Cl3S(0.6) Cl4S(0.25) Cl5S(0.35) Cl6S(0.1)
 C1S(0.66667)
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C18(H18),
 C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26)
3.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.765
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
O1 O 0.29243(15) 0.11354(13) 0.59232(10) 0.0304(4) Uani 1 1 d . . . . .
O2 O 0.31276(14) -0.03048(13) 0.33888(10) 0.0301(4) Uani 1 1 d . . . . .
C1 C 0.35131(18) 0.21371(17) 0.33583(13) 0.0214(4) Uani 1 1 d . . . . .
C2 C 0.42527(18) 0.27815(17) 0.41396(13) 0.0203(4) Uani 1 1 d . . . . .
C3 C 0.55324(18) 0.33928(17) 0.41894(14) 0.0227(4) Uani 1 1 d . . . . .
H3 H 0.591856 0.332745 0.369574 0.027 Uiso 1 1 calc R U . . .
C4 C 0.61914(18) 0.40608(18) 0.49346(14) 0.0246(4) Uani 1 1 d . . . . .
H4 H 0.698805 0.456205 0.492788 0.029 Uiso 1 1 calc R U . . .
C5 C 0.57089(18) 0.40252(17) 0.57326(14) 0.0235(4) Uani 1 1 d . . . . .
C6 C 0.6407(2) 0.46996(19) 0.65293(15) 0.0295(5) Uani 1 1 d . . . . .
H6 H 0.719010 0.522799 0.652419 0.035 Uiso 1 1 calc R U . . .
C7 C 0.5973(2) 0.4599(2) 0.72922(15) 0.0333(5) Uani 1 1 d . . . . .
H7 H 0.639184 0.513755 0.779361 0.040 Uiso 1 1 calc R U . . .
C8 C 0.4893(2) 0.3694(2) 0.73491(14) 0.0299(5) Uani 1 1 d . . . . .
C9 C 0.4557(2) 0.3418(2) 0.81724(16) 0.0387(6) Uani 1 1 d . . . . .
H9 H 0.497153 0.392726 0.868907 0.046 Uiso 1 1 calc R U . . .
C10 C 0.3643(3) 0.2429(3) 0.82240(16) 0.0417(6) Uani 1 1 d . . . . .
H10 H 0.340119 0.227534 0.877341 0.050 Uiso 1 1 calc R U . . .
C11 C 0.3052(2) 0.1632(2) 0.74758(16) 0.0367(5) Uani 1 1 d . . . . .
H11 H 0.245320 0.091750 0.752718 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3345(2) 0.1893(2) 0.66680(14) 0.0286(5) Uani 1 1 d . . . . .
C13 C 0.42031(19) 0.29865(18) 0.65722(14) 0.0247(4) Uani 1 1 d . . . . .
C14 C 0.45258(18) 0.32977(17) 0.57373(13) 0.0218(4) Uani 1 1 d . . . . .
C15 C 0.37063(18) 0.28854(16) 0.48953(13) 0.0202(4) Uani 1 1 d . . . . .
C16 C 0.24032(18) 0.27370(17) 0.47615(13) 0.0207(4) Uani 1 1 d . . . . .
C17 C 0.16664(18) 0.22335(17) 0.39374(13) 0.0212(4) Uani 1 1 d . . . . .
C18 C 0.03868(18) 0.22732(18) 0.37019(14) 0.0249(4) Uani 1 1 d . . . . .
H18 H 0.000546 0.263090 0.411175 0.030 Uiso 1 1 calc R U . . .
C19 C -0.02798(19) 0.1805(2) 0.29013(14) 0.0275(5) Uani 1 1 d . . . . .
H19 H -0.107250 0.196538 0.271549 0.033 Uiso 1 1 calc R U . . .
C20 C 0.01825(19) 0.1074(2) 0.23281(14) 0.0268(5) Uani 1 1 d . . . . .
C21 C -0.0570(2) 0.0469(2) 0.15310(15) 0.0346(5) Uani 1 1 d . . . . .
H21 H -0.137997 0.059392 0.135393 0.042 Uiso 1 1 calc R U . . .
C22 C -0.0153(2) -0.0284(2) 0.10184(16) 0.0371(6) Uani 1 1 d . . . . .
H22 H -0.063594 -0.060955 0.045872 0.044 Uiso 1 1 calc R U . . .
C23 C 0.1001(2) -0.0596(2) 0.13072(15) 0.0337(5) Uani 1 1 d . . . . .
C24 C 0.1357(2) -0.1503(2) 0.08327(18) 0.0432(6) Uani 1 1 d . . . . .
H24 H 0.090993 -0.180708 0.025922 0.052 Uiso 1 1 calc R U . . .
C25 C 0.2343(3) -0.1945(2) 0.11955(18) 0.0452(6) Uani 1 1 d . . . . .
H25 H 0.260359 -0.252570 0.086101 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2970(2) -0.1549(2) 0.20566(17) 0.0384(6) Uani 1 1 d . . . . .
H26 H 0.361062 -0.190580 0.232138 0.046 Uiso 1 1 calc R U . . .
C27 C 0.2658(2) -0.06420(19) 0.25188(15) 0.0293(5) Uani 1 1 d . . . . .
C28 C 0.1735(2) -0.00548(19) 0.21250(14) 0.0275(5) Uani 1 1 d . . . . .
C29 C 0.13948(19) 0.09196(18) 0.25750(14) 0.0245(4) Uani 1 1 d . . . . .
C30 C 0.22163(18) 0.17228(17) 0.32969(13) 0.0212(4) Uani 1 1 d . . . . .
C31 C 0.40748(18) 0.20130(18) 0.26076(14) 0.0243(4) Uani 1 1 d . . . . .
C32 C 0.45480(19) 0.1987(2) 0.19733(14) 0.0278(5) Uani 1 1 d . . . . .
C33 C 0.5085(2) 0.1918(2) 0.11729(15) 0.0322(5) Uani 1 1 d . . . . .
C34 C 0.6286(3) 0.1480(3) 0.13951(19) 0.0567(8) Uani 1 1 d . . . . .
H34A H 0.688082 0.204869 0.184704 0.085 Uiso 1 1 calc R U . . .
H34B H 0.664465 0.142978 0.086526 0.085 Uiso 1 1 calc R U . . .
H34C H 0.609780 0.068259 0.161487 0.085 Uiso 1 1 calc R U . . .
C35 C 0.5375(3) 0.3175(3) 0.08383(18) 0.0505(7) Uani 1 1 d . . . . .
H35A H 0.460653 0.345004 0.069631 0.076 Uiso 1 1 calc R U . . .
H35B H 0.574000 0.313522 0.031006 0.076 Uiso 1 1 calc R U . . .
H35C H 0.596479 0.374005 0.129501 0.076 Uiso 1 1 calc R U . . .
C36 C 0.4144(3) 0.1031(3) 0.04683(17) 0.0431(6) Uani 1 1 d . . . . .
H36A H 0.397550 0.022763 0.068106 0.065 Uiso 1 1 calc R U . . .
H36B H 0.448651 0.099728 -0.007044 0.065 Uiso 1 1 calc R U . . .
H36C H 0.337015 0.130053 0.034413 0.065 Uiso 1 1 calc R U . . .
C37 C 0.18107(18) 0.31459(18) 0.54253(13) 0.0227(4) Uani 1 1 d . . . . .
C38 C 0.12896(19) 0.34866(19) 0.59663(14) 0.0262(4) Uani 1 1 d . . . . .
C39 C 0.0700(2) 0.3936(2) 0.66546(16) 0.0340(5) Uani 1 1 d . . . . .
C40 C 0.0255(3) 0.2906(3) 0.7210(2) 0.0560(8) Uani 1 1 d . . . . .
H40A H -0.031772 0.223322 0.682683 0.084 Uiso 1 1 calc R U . . .
H40B H -0.017201 0.319170 0.764767 0.084 Uiso 1 1 calc R U . . .
H40C H 0.097253 0.263520 0.750868 0.084 Uiso 1 1 calc R U . . .
C41 C -0.0424(2) 0.4379(3) 0.62141(18) 0.0431(6) Uani 1 1 d . . . . .
H41A H -0.015042 0.502314 0.584630 0.065 Uiso 1 1 calc R U . . .
H41B H -0.081361 0.468839 0.666644 0.065 Uiso 1 1 calc R U . . .
H41C H -0.102615 0.370873 0.584790 0.065 Uiso 1 1 calc R U . . .
C42 C 0.1653(3) 0.4969(3) 0.7224(2) 0.0684(10) Uani 1 1 d . . . . .
H42A H 0.127877 0.527416 0.768675 0.103 Uiso 1 1 calc R U . . .
H42B H 0.191990 0.561841 0.685828 0.103 Uiso 1 1 calc R U . . .
H42C H 0.237360 0.467769 0.749148 0.103 Uiso 1 1 calc R U . . .
C43 C 0.2246(3) -0.0071(2) 0.59502(18) 0.0440(6) Uani 1 1 d . . . . .
H43A H 0.140417 -0.008446 0.606644 0.053 Uiso 1 1 calc R U . . .
H43B H 0.268107 -0.046571 0.641819 0.053 Uiso 1 1 calc R U . . .
C44 C 0.2165(3) -0.0709(2) 0.50572(18) 0.0417(6) Uani 1 1 d . . . . .
H44A H 0.174274 -0.029111 0.459866 0.050 Uiso 1 1 calc R U . . .
H44B H 0.165798 -0.154424 0.502991 0.050 Uiso 1 1 calc R U . . .
C45 C 0.3450(2) -0.0743(2) 0.48674(16) 0.0369(5) Uani 1 1 d . . . . .
H45A H 0.399288 0.008098 0.499384 0.044 Uiso 1 1 calc R U . . .
H45B H 0.381319 -0.126272 0.527657 0.044 Uiso 1 1 calc R U . . .
C46 C 0.3464(2) -0.1197(2) 0.39406(16) 0.0345(5) Uani 1 1 d . . . . .
H46A H 0.430117 -0.129578 0.388821 0.041 Uiso 1 1 calc R U . . .
H46B H 0.285984 -0.198373 0.377120 0.041 Uiso 1 1 calc R U . . .
Cl1S Cl 0.76522(16) 0.51995(17) 0.01167(11) 0.0670(5) Uani 0.5 1 d . . P A 1
Cl2S Cl 0.7828(4) 0.6269(5) -0.0045(3) 0.0732(12) Uani 0.2 1 d . . P A -2
Cl3S Cl 0.82172(13) 0.71328(12) -0.09547(9) 0.0630(4) Uani 0.6 1 d . . P A 1
Cl4S Cl 0.9223(4) 0.6018(4) -0.1409(3) 0.0765(10) Uani 0.25 1 d . . P A 2
Cl5S Cl 0.9207(3) 0.5124(3) -0.11275(19) 0.0710(8) Uani 0.35 1 d . . P A 1
Cl6S Cl 0.9822(10) 0.5392(10) -0.0682(9) 0.080(3) Uani 0.1 1 d . . P A -1
C1S C 0.8792(5) 0.6059(5) -0.0393(4) 0.0706(15) Uani 0.6667 1 d . . P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0244
0 0 -1 0.0056
2 1 -1 0.0550
-1 2 0 0.1037
1 -2 0 0.0510
-2 -1 1 0.0498
-16 4 6 0.0543
15 0 0 0.0379
-3 5 20 0.0473
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
C12 O1 C43 120.80(18) . . ?
C27 O2 C46 118.50(17) . . ?
C2 C1 C30 120.04(18) . . ?
C2 C1 C31 119.10(17) . . ?
C30 C1 C31 120.59(18) . . ?
C1 C2 C3 122.19(18) . . ?
C1 C2 C15 119.41(17) . . ?
C15 C2 C3 118.33(18) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.50(19) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C5 121.17(18) . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 121.79(19) . . ?
C14 C5 C4 119.29(19) . . ?
C14 C5 C6 118.92(19) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(2) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 121.5(2) . . ?
C13 C8 C7 118.9(2) . . ?
C13 C8 C9 119.4(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(2) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 H11 120.2 . . ?
O1 C12 C11 124.4(2) . . ?
O1 C12 C13 114.54(18) . . ?
C11 C12 C13 121.0(2) . . ?
C8 C13 C12 117.66(19) . . ?
C8 C13 C14 119.00(19) . . ?
C12 C13 C14 122.64(19) . . ?
C5 C14 C13 118.34(18) . . ?
C5 C14 C15 117.68(18) . . ?
C13 C14 C15 123.97(18) . . ?
C2 C15 C14 118.23(17) . . ?
C16 C15 C2 117.66(18) . . ?
C16 C15 C14 123.54(18) . . ?
C15 C16 C37 121.58(18) . . ?
C17 C16 C15 119.62(18) . . ?
C17 C16 C37 118.71(17) . . ?
C16 C17 C18 122.17(18) . . ?
C16 C17 C30 119.58(17) . . ?
C30 C17 C18 118.18(18) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.45(19) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.38(19) . . ?
C20 C19 H19 119.3 . . ?
C21 C20 C19 121.48(19) . . ?
C29 C20 C19 119.10(19) . . ?
C29 C20 C21 119.4(2) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.1(2) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 119.5 . . ?
C21 C22 C23 121.0(2) . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 121.1(2) . . ?
C24 C23 C28 120.1(2) . . ?
C28 C23 C22 118.6(2) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(2) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 119.9(2) . . ?
C27 C26 H26 120.0 . . ?
O2 C27 C26 123.0(2) . . ?
O2 C27 C28 115.56(18) . . ?
C26 C27 C28 121.2(2) . . ?
C23 C28 C27 116.6(2) . . ?
C23 C28 C29 119.2(2) . . ?
C27 C28 C29 123.37(19) . . ?
C20 C29 C28 118.37(19) . . ?
C20 C29 C30 117.72(19) . . ?
C28 C29 C30 123.85(19) . . ?
C1 C30 C17 117.21(18) . . ?
C1 C30 C29 124.50(18) . . ?
C17 C30 C29 117.92(17) . . ?
C32 C31 C1 175.7(2) . . ?
C31 C32 C33 177.6(2) . . ?
C32 C33 C34 109.13(19) . . ?
C32 C33 C35 109.1(2) . . ?
C32 C33 C36 109.08(19) . . ?
C34 C33 C35 109.7(2) . . ?
C36 C33 C34 109.9(2) . . ?
C36 C33 C35 109.9(2) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C16 178.4(2) . . ?
C37 C38 C39 177.5(2) . . ?
C38 C39 C40 109.4(2) . . ?
C38 C39 C41 109.0(2) . . ?
C38 C39 C42 108.4(2) . . ?
C41 C39 C40 109.0(2) . . ?
C42 C39 C40 110.8(3) . . ?
C42 C39 C41 110.3(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O1 C43 H43A 110.5 . . ?
O1 C43 H43B 110.5 . . ?
O1 C43 C44 106.00(18) . . ?
H43A C43 H43B 108.7 . . ?
C44 C43 H43A 110.5 . . ?
C44 C43 H43B 110.5 . . ?
C43 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C43 C44 C45 112.0(2) . . ?
H44A C44 H44B 107.9 . . ?
C45 C44 H44A 109.2 . . ?
C45 C44 H44B 109.2 . . ?
C44 C45 H45A 108.5 . . ?
C44 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C46 C45 C44 115.1(2) . . ?
C46 C45 H45A 108.5 . . ?
C46 C45 H45B 108.5 . . ?
O2 C46 C45 106.21(17) . . ?
O2 C46 H46A 110.5 . . ?
O2 C46 H46B 110.5 . . ?
C45 C46 H46A 110.5 . . ?
C45 C46 H46B 110.5 . . ?
H46A C46 H46B 108.7 . . ?
Cl6S Cl5S C1S 69.6(7) . . ?
Cl5S Cl6S C1S 80.2(8) . . ?
Cl2S C1S Cl4S 138.2(5) . . ?
Cl3S C1S Cl1S 110.3(3) . . ?
Cl3S C1S Cl5S 108.6(3) . . ?
Cl5S C1S Cl1S 108.9(3) . . ?
Cl6S C1S Cl1S 116.9(5) . . ?
Cl6S C1S Cl3S 125.0(6) . . ?
Cl6S C1S Cl5S 30.2(4) . . ?
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
O1 C12 1.356(3) . ?
O1 C43 1.424(3) . ?
O2 C27 1.364(3) . ?
O2 C46 1.437(3) . ?
C1 C2 1.412(3) . ?
C1 C30 1.413(3) . ?
C1 C31 1.432(3) . ?
C2 C3 1.438(3) . ?
C2 C15 1.425(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.354(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.432(3) . ?
C5 C6 1.428(3) . ?
C5 C14 1.402(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.355(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.425(3) . ?
C8 C9 1.422(3) . ?
C8 C13 1.418(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.361(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.407(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.378(3) . ?
C12 C13 1.427(3) . ?
C13 C14 1.442(3) . ?
C14 C15 1.452(3) . ?
C15 C16 1.414(3) . ?
C16 C17 1.415(3) . ?
C16 C37 1.432(3) . ?
C17 C18 1.435(3) . ?
C17 C30 1.424(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.351(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.429(3) . ?
C20 C21 1.420(3) . ?
C20 C29 1.405(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.356(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.428(3) . ?
C23 C24 1.412(3) . ?
C23 C28 1.417(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.367(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.400(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(3) . ?
C27 C28 1.428(3) . ?
C28 C29 1.444(3) . ?
C29 C30 1.454(3) . ?
C31 C32 1.198(3) . ?
C32 C33 1.476(3) . ?
C33 C34 1.535(3) . ?
C33 C35 1.536(4) . ?
C33 C36 1.535(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.200(3) . ?
C38 C39 1.479(3) . ?
C39 C40 1.535(4) . ?
C39 C41 1.532(3) . ?
C39 C42 1.525(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.512(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.532(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.508(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
Cl1S C1S 1.756(5) . ?
Cl2S C1S 1.352(7) . ?
Cl3S C1S 1.719(5) . ?
Cl4S C1S 1.727(7) . ?
Cl5S Cl6S 0.878(11) . ?
Cl5S C1S 1.718(7) . ?
Cl6S C1S 1.634(12) . ?
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
O1 C12 C13 C8 -166.06(18) . . . . ?
O1 C12 C13 C14 4.3(3) . . . . ?
O1 C43 C44 C45 62.1(3) . . . . ?
O2 C27 C28 C23 -163.74(19) . . . . ?
O2 C27 C28 C29 6.1(3) . . . . ?
C1 C2 C3 C4 176.07(18) . . . . ?
C1 C2 C15 C14 165.87(17) . . . . ?
C1 C2 C15 C16 -22.5(3) . . . . ?
C2 C1 C30 C17 15.8(3) . . . . ?
C2 C1 C30 C29 -171.42(18) . . . . ?
C2 C3 C4 C5 10.1(3) . . . . ?
C2 C15 C16 C17 14.2(3) . . . . ?
C2 C15 C16 C37 -162.31(18) . . . . ?
C3 C2 C15 C14 -17.2(3) . . . . ?
C3 C2 C15 C16 154.50(17) . . . . ?
C3 C4 C5 C6 178.28(19) . . . . ?
C3 C4 C5 C14 -0.9(3) . . . . ?
C4 C5 C6 C7 -175.78(19) . . . . ?
C4 C5 C14 C13 161.83(17) . . . . ?
C4 C5 C14 C15 -17.1(3) . . . . ?
C5 C6 C7 C8 9.0(3) . . . . ?
C5 C14 C15 C2 26.1(3) . . . . ?
C5 C14 C15 C16 -145.10(19) . . . . ?
C6 C5 C14 C13 -17.4(3) . . . . ?
C6 C5 C14 C15 163.71(17) . . . . ?
C6 C7 C8 C9 167.8(2) . . . . ?
C6 C7 C8 C13 -6.9(3) . . . . ?
C7 C8 C9 C10 -169.5(2) . . . . ?
C7 C8 C13 C12 163.41(19) . . . . ?
C7 C8 C13 C14 -7.3(3) . . . . ?
C8 C9 C10 C11 2.8(4) . . . . ?
C8 C13 C14 C5 19.3(3) . . . . ?
C8 C13 C14 C15 -161.84(18) . . . . ?
C9 C8 C13 C12 -11.4(3) . . . . ?
C9 C8 C13 C14 177.95(19) . . . . ?
C9 C10 C11 C12 -4.1(4) . . . . ?
C10 C11 C12 O1 173.3(2) . . . . ?
C10 C11 C12 C13 -2.7(3) . . . . ?
C11 C12 C13 C8 10.3(3) . . . . ?
C11 C12 C13 C14 -179.4(2) . . . . ?
C12 O1 C43 C44 -168.6(2) . . . . ?
C12 C13 C14 C5 -150.9(2) . . . . ?
C12 C13 C14 C15 28.0(3) . . . . ?
C13 C8 C9 C10 5.1(3) . . . . ?
C13 C14 C15 C2 -152.80(18) . . . . ?
C13 C14 C15 C16 36.0(3) . . . . ?
C14 C5 C6 C7 3.4(3) . . . . ?
C14 C15 C16 C17 -174.64(17) . . . . ?
C14 C15 C16 C37 8.9(3) . . . . ?
C15 C2 C3 C4 -0.8(3) . . . . ?
C15 C16 C17 C18 -167.61(18) . . . . ?
C15 C16 C17 C30 9.1(3) . . . . ?
C16 C17 C18 C19 178.58(19) . . . . ?
C16 C17 C30 C1 -24.1(3) . . . . ?
C16 C17 C30 C29 162.63(17) . . . . ?
C17 C18 C19 C20 11.3(3) . . . . ?
C18 C17 C30 C1 152.76(18) . . . . ?
C18 C17 C30 C29 -20.6(3) . . . . ?
C18 C19 C20 C21 172.7(2) . . . . ?
C18 C19 C20 C29 -5.1(3) . . . . ?
C19 C20 C21 C22 -175.7(2) . . . . ?
C19 C20 C29 C28 163.61(19) . . . . ?
C19 C20 C29 C30 -13.8(3) . . . . ?
C20 C21 C22 C23 6.8(4) . . . . ?
C20 C29 C30 C1 -146.3(2) . . . . ?
C20 C29 C30 C17 26.5(3) . . . . ?
C21 C20 C29 C28 -14.2(3) . . . . ?
C21 C20 C29 C30 168.35(19) . . . . ?
C21 C22 C23 C24 171.2(2) . . . . ?
C21 C22 C23 C28 -3.1(4) . . . . ?
C22 C23 C24 C25 -168.0(3) . . . . ?
C22 C23 C28 C27 161.0(2) . . . . ?
C22 C23 C28 C29 -9.2(3) . . . . ?
C23 C24 C25 C26 3.2(4) . . . . ?
C23 C28 C29 C20 17.8(3) . . . . ?
C23 C28 C29 C30 -164.9(2) . . . . ?
C24 C23 C28 C27 -13.3(3) . . . . ?
C24 C23 C28 C29 176.4(2) . . . . ?
C24 C25 C26 C27 -5.0(4) . . . . ?
C25 C26 C27 O2 172.4(2) . . . . ?
C25 C26 C27 C28 -2.7(4) . . . . ?
C26 C27 C28 C23 11.6(3) . . . . ?
C26 C27 C28 C29 -178.5(2) . . . . ?
C27 O2 C46 C45 -157.93(19) . . . . ?
C27 C28 C29 C20 -151.8(2) . . . . ?
C27 C28 C29 C30 25.5(3) . . . . ?
C28 C23 C24 C25 6.2(4) . . . . ?
C28 C29 C30 C1 36.4(3) . . . . ?
C28 C29 C30 C17 -150.79(19) . . . . ?
C29 C20 C21 C22 2.1(3) . . . . ?
C30 C1 C2 C3 -169.46(18) . . . . ?
C30 C1 C2 C15 7.4(3) . . . . ?
C30 C17 C18 C19 1.8(3) . . . . ?
C31 C1 C2 C3 4.6(3) . . . . ?
C31 C1 C2 C15 -178.59(17) . . . . ?
C31 C1 C30 C17 -158.20(18) . . . . ?
C31 C1 C30 C29 14.6(3) . . . . ?
C37 C16 C17 C18 9.0(3) . . . . ?
C37 C16 C17 C30 -174.36(17) . . . . ?
C43 O1 C12 C11 -7.5(3) . . . . ?
C43 O1 C12 C13 168.6(2) . . . . ?
C43 C44 C45 C46 -171.3(2) . . . . ?
C44 C45 C46 O2 67.7(2) . . . . ?
C46 O2 C27 C26 -29.7(3) . . . . ?
C46 O2 C27 C28 145.6(2) . . . . ?
Cl5S Cl6S C1S Cl1S 81.5(10) . . . . ?
Cl5S Cl6S C1S Cl3S -64.6(10) . . . . ?
Cl6S Cl5S C1S Cl1S -111.2(10) . . . . ?
Cl6S Cl5S C1S Cl3S 128.6(10) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0012 -0.0031 0.9998 0.0010 -0.0463 0.0052
-0.0012 0.0031 -0.9998 -0.0010 0.0463 -0.0052
1.9989 1.0034 -0.9970 0.0908 0.0039 -0.1288
-1.0018 1.9984 0.0125 0.1135 0.0100 0.0607
1.0018 -1.9984 -0.0125 -0.1135 -0.0100 -0.0607
-1.9989 -1.0034 0.9970 -0.0908 -0.0039 0.1288
-15.7566 3.7408 6.0813 0.0253 0.0025 0.9997
15.1831 0.0459 -0.1730 0.2153 -0.2812 -0.9352
-3.3119 5.3233 20.2417 0.3175 -0.8969 0.3077
