#------------------------------------------------------------------------------
#$Date: 2024-12-07 04:53:36 +0200 (Sat, 07 Dec 2024) $
#$Revision: 296737 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/34/1573422.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_1573422
loop_
_publ_author_name
'Fujisaki, Masahiro'
'Naito, Ryoya'
'Shirahata, Takashi'
'Kawasugi, Yoshitaka'
'Tajima, Naoya'
'Misaki, Yohji'
_publ_section_title
;
 Molecular Conductors Based on Dimethylcyclohexene-Fused
 Tetrathiafulvalene
;
_journal_issue                   6
_journal_name_full               Chemistry
_journal_page_first              1509
_journal_page_last               1522
_journal_paper_doi               10.3390/chemistry6060091
_journal_volume                  6
_journal_year                    2024
_chemical_formula_moiety         'Cl O4, 2(C14 H16 S6)'
_chemical_formula_sum            'C28 H32 Cl O4 S12'
_chemical_formula_weight         852.70
_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             2024-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                93.731(3)
_cell_angle_beta                 92.451(2)
_cell_angle_gamma                99.953(3)
_cell_formula_units_Z            2
_cell_length_a                   6.6158(2)
_cell_length_b                   8.0542(3)
_cell_length_c                   32.5826(7)
_cell_measurement_reflns_used    12904
_cell_measurement_temperature    446.15
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      1.8870
_cell_volume                     1703.83(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      446.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_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  ω   -110.00  69.00   0.50    4.69    --  -20.40  38.00  30.00  358
  2  ω    -65.00  69.00   0.50    4.69    --  -20.40  56.00 113.80  268
  3  ω    -68.00  69.00   0.50    4.69    --  -20.40  76.00 -90.00  274
  4  ω    -68.00  69.00   0.50    4.69    --  -20.40  76.00  30.00  274
  5  ω    -64.00  69.00   0.50    4.69    --  -20.40  57.00-150.00  266
  6  ω    -68.00  69.00   0.50    4.69    --  -20.40  76.00 150.00  274
  7  ω    -38.00  94.00   0.50    4.69    --    5.00  57.00  90.00  264
  8  ω   -110.00  69.00   0.50    4.69    --  -20.40  -1.00 120.00  358
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0076446000
_diffrn_orient_matrix_UB_12      0.0083838000
_diffrn_orient_matrix_UB_13      0.0218427000
_diffrn_orient_matrix_UB_21      -0.1068002000
_diffrn_orient_matrix_UB_22      -0.0315380000
_diffrn_orient_matrix_UB_23      0.0003985000
_diffrn_orient_matrix_UB_31      0.0204847000
_diffrn_orient_matrix_UB_32      -0.0835050000
_diffrn_orient_matrix_UB_33      0.0003149000
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            38064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       plate
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7831
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0419
_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)+(0.0248P)²+1.2184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6436
_reflns_number_total             7831
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            rac-DMCh-EDT-TTF_ClO4_100K.cif
_cod_data_source_block           exp_1
_cod_database_code               1573422
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C28H32S12ClO4
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O4A \\sim Cl1-O4B
 with sigma of 0.02
 O3A-O4B \\sim O3B-O4B
 with sigma of 0.02
 Cl1-O3A \\sim Cl1-O3B
 with sigma of 0.02
 C17-C18A \\sim C17A-C18A
 with sigma of 0.02
 C15-C17 \\sim C15-C17A
 with sigma of 0.02
 C20-C18 \\sim C20-C18A
 with sigma of 0.02
 C16-C18 \\sim C16-C18A
 with sigma of 0.02
 C18-C17 \\sim C18A-C17
 with sigma of 0.02
 C19-C17 \\sim C19-C17A
 with sigma of 0.02
 C18-C17 \\sim C18-C17A
 with sigma of 0.02
 C2-C4 \\sim C2-C4A
 with sigma of 0.02
 C6-C4 \\sim C6-C4A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3
 with sigma of 0.02
 C4-C3A \\sim C4A-C3A
 with sigma of 0.02
 C5-C3 \\sim C5-C3A
 with sigma of 0.02
 C1-C3 \\sim C1-C3A
 with sigma of 0.02
 C4-C3 \\sim C4-C3A
 with sigma of 0.02
 Cl1-O2A \\sim Cl1-O2B
 with sigma of 0.02
3. Others
 Sof(O2B)=Sof(O3B)=Sof(O4B)=1-FVAR(1)
 Sof(O2A)=Sof(O3A)=Sof(O4A)=FVAR(1)
 Sof(H19C)=Sof(H19D)=Sof(H20C)=Sof(H20D)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=1-FVAR(2)
 Sof(H19A)=Sof(H19B)=Sof(H20A)=Sof(H20B)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=
 FVAR(2)
 Sof(H5BC)=Sof(H5BD)=Sof(H6BC)=Sof(H6BD)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=1-
 FVAR(3)
 Sof(H5AA)=Sof(H5AB)=Sof(H6AA)=Sof(H6AB)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C3A(H3A), C4A(H4A), C17(H17), C18(H18), C17A(H17A), C18A(H18A)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6AA,H6AB), C6(H6BC,H6BD), C13(H13A,H13B),
 C14(H14A,H14B), C19(H19A,H19B), C19(H19C,H19D), C20(H20A,H20B), C20(H20C,H20D),
  C27(H27A,H27B), C28(H28A,H28B)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_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 4.008
_oxdiff_exptl_absorpt_empirical_full_min 0.291
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
Cl1 Cl 0.77078(15) 0.48185(9) 0.69206(2) 0.0425(2) Uani 1 1 d D . . . .
O1 O 0.6635(4) 0.4009(3) 0.65663(7) 0.0492(7) Uani 1 1 d . . . . .
O2A O 0.8900(19) 0.6317(15) 0.6817(5) 0.059(4) Uani 0.520(4) 1 d D . P A 1
O3A O 0.7779(7) 0.3656(5) 0.72357(12) 0.0370(12) Uani 0.520(4) 1 d D . P A 1
O4A O 0.5754(7) 0.5614(6) 0.70584(13) 0.0447(14) Uani 0.520(4) 1 d D . P A 1
O2B O 0.934(2) 0.6160(17) 0.6884(5) 0.049(4) Uani 0.480(4) 1 d D . P A 2
O3B O 0.9525(7) 0.3740(5) 0.69109(13) 0.0330(12) Uani 0.480(4) 1 d D . P A 2
O4B O 0.7267(8) 0.5009(9) 0.73105(14) 0.0577(19) Uani 0.480(4) 1 d D . P A 2
S1 S 1.22531(9) 0.29682(8) 1.01423(2) 0.01878(14) Uani 1 1 d . . . . .
S2 S 0.78204(9) 0.22962(8) 0.99129(2) 0.01846(14) Uani 1 1 d . . . . .
S3 S 1.32457(9) 0.44055(8) 0.92686(2) 0.01810(14) Uani 1 1 d . . . . .
S4 S 0.88445(9) 0.37386(8) 0.90100(2) 0.01807(14) Uani 1 1 d . . . . .
S5 S 1.47531(10) 0.49018(9) 0.84457(2) 0.02232(15) Uani 1 1 d . . . . .
S6 S 0.94829(10) 0.41129(9) 0.81212(2) 0.02108(15) Uani 1 1 d . . . . .
C1 C 1.0831(4) 0.0840(4) 1.16148(8) 0.0296(6) Uani 1 1 d D . . . .
H1A H 0.992101 0.092088 1.183419 0.044 Uiso 1 1 calc R U . B 1
H1B H 1.214255 0.153125 1.169116 0.044 Uiso 1 1 calc R U . B 1
H1C H 1.099880 -0.031417 1.156405 0.044 Uiso 1 1 calc R U . B 1
C2 C 0.6319(4) -0.0084(4) 1.13693(8) 0.0273(6) Uani 1 1 d D . . . .
H2A H 0.684733 -0.059283 1.159990 0.041 Uiso 1 1 calc R U . C 1
H2B H 0.512399 -0.082279 1.124501 0.041 Uiso 1 1 calc R U . C 1
H2C H 0.595505 0.097605 1.146155 0.041 Uiso 1 1 calc R U . C 1
C5 C 1.1513(4) 0.1568(3) 1.08970(7) 0.0189(5) Uani 1 1 d D . . . .
H5AA H 1.267369 0.244568 1.098677 0.023 Uiso 0.751(13) 1 calc R U P D 1
H5AB H 1.200901 0.050438 1.086387 0.023 Uiso 0.751(13) 1 calc R U P D 1
H5BC H 1.209291 0.261794 1.105475 0.023 Uiso 0.249(13) 1 calc R U P D 2
H5BD H 1.261911 0.094276 1.084802 0.023 Uiso 0.249(13) 1 calc R U P D 2
C6 C 0.7002(4) 0.0887(3) 1.06689(8) 0.0194(5) Uani 1 1 d D . . . .
H6AA H 0.607442 -0.003408 1.051693 0.023 Uiso 0.751(13) 1 calc R U P D 1
H6AB H 0.620461 0.173343 1.075921 0.023 Uiso 0.751(13) 1 calc R U P D 1
H6BC H 0.650597 -0.028465 1.057350 0.023 Uiso 0.249(13) 1 calc R U P D 2
H6BD H 0.584826 0.148259 1.065525 0.023 Uiso 0.249(13) 1 calc R U P D 2
C7 C 1.0614(4) 0.1959(3) 1.04919(7) 0.0171(5) Uani 1 1 d . . . . .
C8 C 0.8611(4) 0.1651(3) 1.03902(7) 0.0180(5) Uani 1 1 d . . . . .
C9 C 1.0310(4) 0.3058(3) 0.97699(7) 0.0163(5) Uani 1 1 d . . . . .
C10 C 1.0727(4) 0.3677(3) 0.93986(7) 0.0167(5) Uani 1 1 d . . . . .
C11 C 1.2606(4) 0.4415(3) 0.87389(7) 0.0168(5) Uani 1 1 d . . . . .
C12 C 1.0593(4) 0.4111(3) 0.86203(7) 0.0164(5) Uani 1 1 d . . . . .
C13 C 1.3595(4) 0.4555(4) 0.79298(8) 0.0256(6) Uani 1 1 d . . . . .
H13A H 1.457775 0.506356 0.774160 0.031 Uiso 1 1 calc R U . . .
H13B H 1.329174 0.334906 0.785479 0.031 Uiso 1 1 calc R U . . .
C14 C 1.1638(4) 0.5274(4) 0.78771(8) 0.0259(6) Uani 1 1 d . . . . .
H14A H 1.128182 0.527543 0.758527 0.031 Uiso 1 1 calc R U . . .
H14B H 1.188955 0.643736 0.799168 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9919(5) 0.1451(7) 1.12236(12) 0.0168(10) Uani 0.751(13) 1 d D . P D 1
H3 H 0.956780 0.257022 1.128615 0.020 Uiso 0.751(13) 1 calc R U P D 1
C4 C 0.7982(7) 0.0217(8) 1.10489(14) 0.0179(10) Uani 0.751(13) 1 d D . P D 1
H4 H 0.837709 -0.086840 1.096555 0.021 Uiso 0.751(13) 1 calc R U P D 1
C3A C 0.9901(17) 0.053(3) 1.1150(3) 0.024(4) Uani 0.249(13) 1 d D . P D 2
H3A H 0.980033 -0.067419 1.106231 0.028 Uiso 0.249(13) 1 calc R U P D 2
C4A C 0.783(2) 0.097(3) 1.1110(4) 0.024(4) Uani 0.249(13) 1 d D . P D 2
H4A H 0.795818 0.215202 1.121941 0.028 Uiso 0.249(13) 1 calc R U P D 2
S7 S 0.69806(9) 0.04588(8) 0.59383(2) 0.01694(14) Uani 1 1 d . . . . .
S8 S 0.28838(9) 0.12391(7) 0.57991(2) 0.01529(13) Uani 1 1 d . . . . .
S9 S 0.82813(9) 0.18276(7) 0.50662(2) 0.01550(13) Uani 1 1 d . . . . .
S10 S 0.41940(9) 0.26940(7) 0.49235(2) 0.01464(13) Uani 1 1 d . . . . .
S11 S 0.99808(9) 0.32137(8) 0.43151(2) 0.01821(14) Uani 1 1 d . . . . .
S12 S 0.50483(9) 0.42161(7) 0.41382(2) 0.01574(13) Uani 1 1 d . . . . .
C15 C 0.5491(5) -0.0667(5) 0.74826(9) 0.0415(8) Uani 1 1 d D . . . .
H15A H 0.619572 0.046397 0.755810 0.062 Uiso 1 1 calc R U . E 1
H15B H 0.646188 -0.142506 0.747912 0.062 Uiso 1 1 calc R U . E 1
H15C H 0.448421 -0.099500 0.767931 0.062 Uiso 1 1 calc R U . E 1
C16 C 0.1317(5) 0.0244(5) 0.73483(8) 0.0362(7) Uani 1 1 d D . . . .
H16A H 0.052977 -0.087146 0.729123 0.054 Uiso 1 1 calc R U . F 1
H16B H 0.042489 0.106169 0.733045 0.054 Uiso 1 1 calc R U . F 1
H16C H 0.196162 0.034019 0.762044 0.054 Uiso 1 1 calc R U . F 1
C19 C 0.6130(4) -0.0337(4) 0.67421(8) 0.0245(6) Uani 1 1 d D . . . .
H19A H 0.717325 0.057748 0.686478 0.029 Uiso 0.758(10) 1 calc R U P G 1
H19B H 0.677030 -0.132308 0.669393 0.029 Uiso 0.758(10) 1 calc R U P G 1
H19C H 0.757578 0.014861 0.678750 0.029 Uiso 0.242(10) 1 calc R U P G 2
H19D H 0.599541 -0.155697 0.673556 0.029 Uiso 0.242(10) 1 calc R U P G 2
C20 C 0.1883(4) 0.0408(3) 0.65987(7) 0.0191(5) Uani 1 1 d D . . . .
H20A H 0.094100 -0.066227 0.655877 0.023 Uiso 0.758(10) 1 calc R U P G 1
H20B H 0.109409 0.130958 0.657508 0.023 Uiso 0.758(10) 1 calc R U P G 1
H20C H 0.060215 -0.028157 0.648838 0.023 Uiso 0.242(10) 1 calc R U P G 2
H20D H 0.161897 0.153282 0.667361 0.023 Uiso 0.242(10) 1 calc R U P G 2
C21 C 0.5335(4) 0.0154(3) 0.63402(7) 0.0170(5) Uani 1 1 d . . . . .
C22 C 0.3433(4) 0.0505(3) 0.62748(7) 0.0154(5) Uani 1 1 d . . . . .
C23 C 0.5290(4) 0.1225(3) 0.56128(7) 0.0136(5) Uani 1 1 d . . . . .
C24 C 0.5836(4) 0.1815(3) 0.52397(7) 0.0137(5) Uani 1 1 d . . . . .
C25 C 0.7863(4) 0.2841(3) 0.46207(7) 0.0146(5) Uani 1 1 d . . . . .
C26 C 0.5984(4) 0.3233(3) 0.45498(7) 0.0141(5) Uani 1 1 d . . . . .
C27 C 0.9287(4) 0.4941(3) 0.40493(8) 0.0183(5) Uani 1 1 d . . . . .
H27A H 0.924130 0.588315 0.424787 0.022 Uiso 1 1 calc R U . . .
H27B H 1.033465 0.530798 0.385924 0.022 Uiso 1 1 calc R U . . .
C28 C 0.7224(4) 0.4461(3) 0.38132(7) 0.0177(5) Uani 1 1 d . . . . .
H28A H 0.719930 0.340780 0.364929 0.021 Uiso 1 1 calc R U . . .
H28B H 0.707833 0.532405 0.362520 0.021 Uiso 1 1 calc R U . . .
C17 C 0.4404(6) -0.0738(6) 0.70472(10) 0.0188(10) Uani 0.758(10) 1 d D . P G 1
H17 H 0.361373 -0.187297 0.697544 0.023 Uiso 0.758(10) 1 calc R U P G 1
C18 C 0.2980(6) 0.0569(7) 0.70313(11) 0.0189(10) Uani 0.758(10) 1 d D . P G 1
H18 H 0.378366 0.170953 0.708736 0.023 Uiso 0.758(10) 1 calc R U P G 1
C17A C 0.490(2) 0.030(2) 0.7104(3) 0.027(4) Uani 0.242(10) 1 d D . P G 2
H17A H 0.519799 0.153481 0.715907 0.033 Uiso 0.242(10) 1 calc R U P G 2
C18A C 0.2656(19) -0.037(2) 0.6991(3) 0.018(3) Uani 0.242(10) 1 d D . P G 2
H18A H 0.240766 -0.160408 0.695264 0.022 Uiso 0.242(10) 1 calc R U P G 2
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'
S S 0.1246 0.1234 '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
-2 -10 5 0.0612
9 -2 -2 0.0404
1 11 -4 0.0866
-9 1 3 0.0670
3 -11 -7 0.0786
0 0 46 0.0045
0 -1 -46 0.0390
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 Cl1 O2A 108.5(7) . . ?
O1 Cl1 O3A 110.8(2) . . ?
O1 Cl1 O4A 91.8(2) . . ?
O1 Cl1 O2B 119.2(7) . . ?
O1 Cl1 O3B 95.9(2) . . ?
O2A Cl1 O3A 136.7(7) . . ?
O2A Cl1 O4A 97.0(7) . . ?
O3A Cl1 O4A 99.3(3) . . ?
O2B Cl1 O3B 82.2(7) . . ?
O4B Cl1 O1 134.3(3) . . ?
O4B Cl1 O2B 103.2(8) . . ?
O4B Cl1 O3B 106.3(3) . . ?
C9 S1 C7 95.22(12) . . ?
C9 S2 C8 94.96(12) . . ?
C10 S3 C11 94.69(12) . . ?
C10 S4 C12 94.85(12) . . ?
C11 S5 C13 101.44(12) . . ?
C12 S6 C14 99.78(12) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H5AA C5 H5AB 108.0 . . ?
H5BC C5 H5BD 107.9 . . ?
C7 C5 H5AA 109.4 . . ?
C7 C5 H5AB 109.4 . . ?
C7 C5 H5BC 109.2 . . ?
C7 C5 H5BD 109.2 . . ?
C7 C5 C3 111.0(2) . . ?
C7 C5 C3A 112.2(4) . . ?
C3 C5 H5AA 109.4 . . ?
C3 C5 H5AB 109.4 . . ?
C3A C5 H5BC 109.2 . . ?
C3A C5 H5BD 109.2 . . ?
H6AA C6 H6AB 108.0 . . ?
H6BC C6 H6BD 107.9 . . ?
C8 C6 H6AA 109.3 . . ?
C8 C6 H6AB 109.3 . . ?
C8 C6 H6BC 109.2 . . ?
C8 C6 H6BD 109.2 . . ?
C8 C6 C4 111.4(2) . . ?
C8 C6 C4A 111.9(5) . . ?
C4 C6 H6AA 109.3 . . ?
C4 C6 H6AB 109.3 . . ?
C4A C6 H6BC 109.2 . . ?
C4A C6 H6BD 109.2 . . ?
C5 C7 S1 118.85(18) . . ?
C8 C7 S1 117.65(19) . . ?
C8 C7 C5 123.4(2) . . ?
C6 C8 S2 118.89(19) . . ?
C7 C8 S2 117.19(19) . . ?
C7 C8 C6 123.8(2) . . ?
S1 C9 S2 114.85(13) . . ?
C10 C9 S1 121.81(19) . . ?
C10 C9 S2 123.3(2) . . ?
S4 C10 S3 114.81(13) . . ?
C9 C10 S3 121.57(19) . . ?
C9 C10 S4 123.57(19) . . ?
S5 C11 S3 113.13(14) . . ?
C12 C11 S3 117.10(18) . . ?
C12 C11 S5 129.73(19) . . ?
S6 C12 S4 115.42(14) . . ?
C11 C12 S4 116.88(18) . . ?
C11 C12 S6 127.66(19) . . ?
S5 C13 H13A 108.8 . . ?
S5 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 S5 113.64(19) . . ?
C14 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
S6 C14 H14A 108.9 . . ?
S6 C14 H14B 108.9 . . ?
C13 C14 S6 113.56(19) . . ?
C13 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C1 C3 H3 109.4 . . ?
C1 C3 C4 111.5(4) . . ?
C5 C3 C1 108.9(3) . . ?
C5 C3 H3 109.4 . . ?
C5 C3 C4 108.2(4) . . ?
C4 C3 H3 109.4 . . ?
C2 C4 H4 108.6 . . ?
C6 C4 C2 107.5(3) . . ?
C6 C4 H4 108.6 . . ?
C3 C4 C2 112.2(4) . . ?
C3 C4 C6 111.3(4) . . ?
C3 C4 H4 108.6 . . ?
C1 C3A H3A 108.7 . . ?
C5 C3A C1 104.9(8) . . ?
C5 C3A H3A 108.7 . . ?
C4A C3A C1 111.6(13) . . ?
C4A C3A C5 114.2(12) . . ?
C4A C3A H3A 108.7 . . ?
C2 C4A H4A 106.9 . . ?
C6 C4A C2 110.8(8) . . ?
C6 C4A H4A 106.9 . . ?
C3A C4A C2 111.6(14) . . ?
C3A C4A C6 113.2(13) . . ?
C3A C4A H4A 106.9 . . ?
C23 S7 C21 95.94(12) . . ?
C23 S8 C22 95.93(11) . . ?
C24 S9 C25 95.27(11) . . ?
C24 S10 C26 95.50(11) . . ?
C25 S11 C27 98.47(11) . . ?
C26 S12 C28 101.58(12) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C15 H15A 109.5 . . ?
C17 C15 H15B 109.5 . . ?
C17 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C16 H16A 109.5 . . ?
C18 C16 H16B 109.5 . . ?
C18 C16 H16C 109.5 . . ?
H19A C19 H19B 107.9 . . ?
H19C C19 H19D 108.1 . . ?
C21 C19 H19A 109.2 . . ?
C21 C19 H19B 109.2 . . ?
C21 C19 H19C 109.6 . . ?
C21 C19 H19D 109.6 . . ?
C21 C19 C17 112.2(2) . . ?
C21 C19 C17A 110.4(4) . . ?
C17 C19 H19A 109.2 . . ?
C17 C19 H19B 109.2 . . ?
C17A C19 H19C 109.6 . . ?
C17A C19 H19D 109.6 . . ?
H20A C20 H20B 108.2 . . ?
H20C C20 H20D 108.0 . . ?
C22 C20 H20A 109.7 . . ?
C22 C20 H20B 109.7 . . ?
C22 C20 H20C 109.4 . . ?
C22 C20 H20D 109.4 . . ?
C22 C20 C18 110.0(2) . . ?
C22 C20 C18A 111.4(4) . . ?
C18 C20 H20A 109.7 . . ?
C18 C20 H20B 109.7 . . ?
C18A C20 H20C 109.4 . . ?
C18A C20 H20D 109.4 . . ?
C19 C21 S7 119.36(18) . . ?
C22 C21 S7 116.69(18) . . ?
C22 C21 C19 123.8(2) . . ?
C20 C22 S8 120.13(18) . . ?
C21 C22 S8 116.62(18) . . ?
C21 C22 C20 123.1(2) . . ?
S7 C23 S8 114.73(13) . . ?
C24 C23 S7 122.44(18) . . ?
C24 C23 S8 122.82(19) . . ?
S10 C24 S9 115.44(13) . . ?
C23 C24 S9 121.74(19) . . ?
C23 C24 S10 122.74(18) . . ?
S9 C25 S11 114.71(14) . . ?
C26 C25 S9 117.56(17) . . ?
C26 C25 S11 127.73(18) . . ?
S12 C26 S10 114.35(14) . . ?
C25 C26 S10 116.22(17) . . ?
C25 C26 S12 129.43(18) . . ?
S11 C27 H27A 109.1 . . ?
S11 C27 H27B 109.1 . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 S11 112.31(17) . . ?
C28 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
S12 C28 H28A 108.8 . . ?
S12 C28 H28B 108.8 . . ?
C27 C28 S12 113.94(17) . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C15 C17 H17 109.8 . . ?
C19 C17 C15 106.5(3) . . ?
C19 C17 H17 109.8 . . ?
C18 C17 C15 110.9(3) . . ?
C18 C17 C19 109.9(3) . . ?
C18 C17 H17 109.8 . . ?
C16 C18 C20 107.9(3) . . ?
C16 C18 H18 109.8 . . ?
C20 C18 H18 109.8 . . ?
C17 C18 C16 110.6(4) . . ?
C17 C18 C20 108.9(4) . . ?
C17 C18 H18 109.8 . . ?
C15 C17A H17A 112.9 . . ?
C19 C17A C15 104.8(8) . . ?
C19 C17A H17A 112.9 . . ?
C18A C17A C15 106.2(11) . . ?
C18A C17A C19 106.4(11) . . ?
C18A C17A H17A 112.9 . . ?
C16 C18A H18A 110.5 . . ?
C20 C18A C16 104.3(7) . . ?
C20 C18A H18A 110.5 . . ?
C17A C18A C16 108.8(11) . . ?
C17A C18A C20 112.0(10) . . ?
C17A C18A H18A 110.5 . . ?
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
Cl1 O1 1.391(2) . ?
Cl1 O2A 1.393(10) . ?
Cl1 O3A 1.439(4) . ?
Cl1 O4A 1.607(4) . ?
Cl1 O2B 1.406(9) . ?
Cl1 O3B 1.601(4) . ?
Cl1 O4B 1.321(4) . ?
S1 C7 1.748(2) . ?
S1 C9 1.744(3) . ?
S2 C8 1.758(2) . ?
S2 C9 1.749(2) . ?
S3 C10 1.748(2) . ?
S3 C11 1.760(2) . ?
S4 C10 1.747(3) . ?
S4 C12 1.759(2) . ?
S5 C11 1.748(2) . ?
S5 C13 1.802(3) . ?
S6 C12 1.756(2) . ?
S6 C14 1.809(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C3 1.532(4) . ?
C1 C3A 1.597(11) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 C4 1.549(5) . ?
C2 C4A 1.521(12) . ?
C5 H5AA 0.9700 . ?
C5 H5AB 0.9700 . ?
C5 H5BC 0.9700 . ?
C5 H5BD 0.9700 . ?
C5 C7 1.499(3) . ?
C5 C3 1.526(4) . ?
C5 C3A 1.542(11) . ?
C6 H6AA 0.9700 . ?
C6 H6AB 0.9700 . ?
C6 H6BC 0.9700 . ?
C6 H6BD 0.9700 . ?
C6 C8 1.505(3) . ?
C6 C4 1.544(5) . ?
C6 C4A 1.509(11) . ?
C7 C8 1.329(4) . ?
C9 C10 1.360(3) . ?
C11 C12 1.347(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.514(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C3 H3 0.9800 . ?
C3 C4 1.542(8) . ?
C4 H4 0.9800 . ?
C3A H3A 0.9800 . ?
C3A C4A 1.48(3) . ?
C4A H4A 0.9800 . ?
S7 C21 1.741(2) . ?
S7 C23 1.726(2) . ?
S8 C22 1.740(2) . ?
S8 C23 1.729(2) . ?
S9 C24 1.735(2) . ?
S9 C25 1.746(2) . ?
S10 C24 1.734(2) . ?
S10 C26 1.757(2) . ?
S11 C25 1.748(2) . ?
S11 C27 1.800(2) . ?
S12 C26 1.745(2) . ?
S12 C28 1.814(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C17 1.556(4) . ?
C15 C17A 1.573(11) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 C18 1.542(4) . ?
C16 C18A 1.595(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C19 H19D 0.9700 . ?
C19 C21 1.493(3) . ?
C19 C17 1.551(4) . ?
C19 C17A 1.570(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C20 H20D 0.9700 . ?
C20 C22 1.499(3) . ?
C20 C18 1.545(4) . ?
C20 C18A 1.564(10) . ?
C21 C22 1.348(3) . ?
C23 C24 1.374(3) . ?
C25 C26 1.349(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.514(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C17 H17 0.9800 . ?
C17 C18 1.532(7) . ?
C18 H18 0.9800 . ?
C17A H17A 0.9800 . ?
C17A C18A 1.51(2) . ?
C18A H18A 0.9800 . ?
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
S1 C7 C8 S2 0.0(3) . . . . ?
S1 C7 C8 C6 -176.25(19) . . . . ?
S1 C9 C10 S3 0.6(3) . . . . ?
S1 C9 C10 S4 178.11(14) . . . . ?
S2 C9 C10 S3 -179.39(13) . . . . ?
S2 C9 C10 S4 -1.9(3) . . . . ?
S3 C11 C12 S4 0.0(3) . . . . ?
S3 C11 C12 S6 177.47(14) . . . . ?
S5 C11 C12 S4 -177.59(15) . . . . ?
S5 C11 C12 S6 -0.1(4) . . . . ?
S5 C13 C14 S6 -71.6(2) . . . . ?
C1 C3 C4 C2 56.3(6) . . . . ?
C1 C3 C4 C6 176.9(3) . . . . ?
C1 C3A C4A C2 -61(2) . . . . ?
C1 C3A C4A C6 173.4(7) . . . . ?
C5 C7 C8 S2 176.67(19) . . . . ?
C5 C7 C8 C6 0.4(4) . . . . ?
C5 C3 C4 C2 176.1(3) . . . . ?
C5 C3 C4 C6 -63.4(6) . . . . ?
C5 C3A C4A C2 -179.5(7) . . . . ?
C5 C3A C4A C6 55(2) . . . . ?
C7 S1 C9 S2 3.60(16) . . . . ?
C7 S1 C9 C10 -176.4(2) . . . . ?
C7 C5 C3 C1 173.2(3) . . . . ?
C7 C5 C3 C4 51.8(5) . . . . ?
C7 C5 C3A C1 -158.7(7) . . . . ?
C7 C5 C3A C4A -36.2(19) . . . . ?
C8 S2 C9 S1 -3.59(16) . . . . ?
C8 S2 C9 C10 176.4(2) . . . . ?
C8 C6 C4 C2 164.8(3) . . . . ?
C8 C6 C4 C3 41.5(5) . . . . ?
C8 C6 C4A C2 -169.5(9) . . . . ?
C8 C6 C4A C3A -43.2(19) . . . . ?
C9 S1 C7 C5 -179.0(2) . . . . ?
C9 S1 C7 C8 -2.2(2) . . . . ?
C9 S2 C8 C6 178.6(2) . . . . ?
C9 S2 C8 C7 2.2(2) . . . . ?
C10 S3 C11 S5 -174.46(14) . . . . ?
C10 S3 C11 C12 7.6(2) . . . . ?
C10 S4 C12 S6 174.65(14) . . . . ?
C10 S4 C12 C11 -7.5(2) . . . . ?
C11 S3 C10 S4 -12.56(16) . . . . ?
C11 S3 C10 C9 165.1(2) . . . . ?
C11 S5 C13 C14 43.8(2) . . . . ?
C12 S4 C10 S3 12.56(16) . . . . ?
C12 S4 C10 C9 -165.1(2) . . . . ?
C12 S6 C14 C13 52.8(2) . . . . ?
C13 S5 C11 S3 173.44(15) . . . . ?
C13 S5 C11 C12 -8.9(3) . . . . ?
C14 S6 C12 S4 159.66(15) . . . . ?
C14 S6 C12 C11 -17.9(3) . . . . ?
C3 C5 C7 S1 154.5(3) . . . . ?
C3 C5 C7 C8 -22.1(4) . . . . ?
C4 C6 C8 S2 173.5(3) . . . . ?
C4 C6 C8 C7 -10.3(4) . . . . ?
C3A C5 C7 S1 -174.4(8) . . . . ?
C3A C5 C7 C8 9.0(9) . . . . ?
C4A C6 C8 S2 -159.8(10) . . . . ?
C4A C6 C8 C7 16.3(10) . . . . ?
S7 C21 C22 S8 -0.7(3) . . . . ?
S7 C21 C22 C20 -176.18(19) . . . . ?
S7 C23 C24 S9 0.2(3) . . . . ?
S7 C23 C24 S10 -176.36(13) . . . . ?
S8 C23 C24 S9 178.55(13) . . . . ?
S8 C23 C24 S10 1.9(3) . . . . ?
S9 C25 C26 S10 0.9(3) . . . . ?
S9 C25 C26 S12 -179.37(14) . . . . ?
S11 C25 C26 S10 -179.51(14) . . . . ?
S11 C25 C26 S12 0.2(4) . . . . ?
S11 C27 C28 S12 72.2(2) . . . . ?
C15 C17 C18 C16 -59.6(5) . . . . ?
C15 C17 C18 C20 -178.1(3) . . . . ?
C15 C17A C18A C16 68.8(14) . . . . ?
C15 C17A C18A C20 -176.4(7) . . . . ?
C19 C21 C22 S8 174.3(2) . . . . ?
C19 C21 C22 C20 -1.2(4) . . . . ?
C19 C17 C18 C16 -177.2(3) . . . . ?
C19 C17 C18 C20 64.4(5) . . . . ?
C19 C17A C18A C16 -179.9(6) . . . . ?
C19 C17A C18A C20 -65.1(15) . . . . ?
C21 S7 C23 S8 -3.19(16) . . . . ?
C21 S7 C23 C24 175.2(2) . . . . ?
C21 C19 C17 C15 -162.6(3) . . . . ?
C21 C19 C17 C18 -42.4(5) . . . . ?
C21 C19 C17A C15 166.3(6) . . . . ?
C21 C19 C17A C18A 54.0(13) . . . . ?
C22 S8 C23 S7 2.90(16) . . . . ?
C22 S8 C23 C24 -175.5(2) . . . . ?
C22 C20 C18 C16 -173.2(3) . . . . ?
C22 C20 C18 C17 -53.0(4) . . . . ?
C22 C20 C18A C16 159.4(6) . . . . ?
C22 C20 C18A C17A 41.9(14) . . . . ?
C23 S7 C21 C19 -172.9(2) . . . . ?
C23 S7 C21 C22 2.3(2) . . . . ?
C23 S8 C22 C20 174.3(2) . . . . ?
C23 S8 C22 C21 -1.3(2) . . . . ?
C24 S9 C25 S11 179.28(14) . . . . ?
C24 S9 C25 C26 -1.1(2) . . . . ?
C24 S10 C26 S12 -179.98(14) . . . . ?
C24 S10 C26 C25 -0.2(2) . . . . ?
C25 S9 C24 S10 0.92(16) . . . . ?
C25 S9 C24 C23 -175.9(2) . . . . ?
C25 S11 C27 C28 -58.45(19) . . . . ?
C26 S10 C24 S9 -0.53(16) . . . . ?
C26 S10 C24 C23 176.3(2) . . . . ?
C26 S12 C28 C27 -39.0(2) . . . . ?
C27 S11 C25 S9 -156.85(14) . . . . ?
C27 S11 C25 C26 23.6(3) . . . . ?
C28 S12 C26 S10 -177.01(13) . . . . ?
C28 S12 C26 C25 3.3(3) . . . . ?
C17 C19 C21 S7 -173.9(3) . . . . ?
C17 C19 C21 C22 11.2(4) . . . . ?
C18 C20 C22 S8 -153.0(3) . . . . ?
C18 C20 C22 C21 22.4(4) . . . . ?
C17A C19 C21 S7 152.1(7) . . . . ?
C17A C19 C21 C22 -22.8(8) . . . . ?
C18A C20 C22 S8 177.2(7) . . . . ?
C18A C20 C22 C21 -7.4(8) . . . . ?
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
-2.4571 -10.2699 4.6742 -0.0028 0.5882 0.8087
9.3251 -2.1691 -2.4061 0.0005 -0.9285 0.3714
1.1600 10.8514 -4.4437 0.0028 -0.4679 -0.8838
-9.2889 0.9511 2.8475 -0.0008 0.9632 -0.2688
3.2036 -10.8961 -7.4770 -0.2302 -0.0015 0.9731
0.1020 0.1832 45.6758 1.0000 0.0015 0.0012
0.0254 -0.6117 -45.5242 -0.9993 -0.0016 0.0373
