#------------------------------------------------------------------------------
#$Date: 2024-12-07 04:53:23 +0200 (Sat, 07 Dec 2024) $
#$Revision: 296736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/34/1573421.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_1573421
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         '2(Cl O4), 4(C14 H16 S6)'
_chemical_formula_sum            'C56 H64 Cl2 O8 S24'
_chemical_formula_weight         1705.41
_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             2024-10-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                93.919(4)
_cell_angle_beta                 92.093(3)
_cell_angle_gamma                100.116(4)
_cell_formula_units_Z            1
_cell_length_a                   6.6663(3)
_cell_length_b                   8.2020(4)
_cell_length_c                   32.6647(13)
_cell_measurement_reflns_used    7594
_cell_measurement_temperature    263.15
_cell_measurement_theta_max      28.4650
_cell_measurement_theta_min      2.4960
_cell_volume                     1751.99(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      263.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -33.00  93.00   0.40    9.18    --    5.00  57.00-120.00  315
  2  ω    -62.00  72.00   0.40    9.18    --  -17.80  76.00-180.00  335
  3  ω    -56.00  72.00   0.40    9.18    --  -17.80  57.00 -60.00  320
  4  ω    -62.00  72.00   0.40    9.18    --  -17.80  76.00  90.00  335
  5  ω    -62.00  72.00   0.40    9.18    --  -17.80  76.00-150.00  335
  6  ω    -62.00  65.20   0.40    9.18    --  -17.80  76.00 -30.00  318
  7  ω    -46.00  29.20   0.40    9.18    --  -17.80  76.00  60.00  188
;
_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      0.0027126000
_diffrn_orient_matrix_UB_12      0.0039105000
_diffrn_orient_matrix_UB_13      0.0217772000
_diffrn_orient_matrix_UB_21      -0.1063982000
_diffrn_orient_matrix_UB_22      -0.0310422000
_diffrn_orient_matrix_UB_23      -0.0006318000
_diffrn_orient_matrix_UB_31      0.0195497000
_diffrn_orient_matrix_UB_32      -0.0823569000
_diffrn_orient_matrix_UB_33      -0.0004993000
_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  0.1018
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            31755
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.503
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8044
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0463P)²+1.1172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5769
_reflns_number_total             8044
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            rac-DMCh-EDT-TTF_ClO4_263K.cif
_cod_data_source_block           exp_1_263k_autored
_cod_database_code               1573421
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C28H3Cl1O42S12
_chemical_oxdiff_usercomment     deltaomega_0.4deg
_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   0.958
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O1A = Cl1-O2A = Cl1-O4A = Cl1-O3A
 1.5 with sigma of 0.02
 Cl1-O1A \\sim Cl1-O2A \\sim Cl1-O4A \\sim Cl1-O3A
 with sigma of 0.02
 O1A-O4A \\sim O2A-O3A \\sim O1A-O3A \\sim O2A-O4A \\sim O1A-O2A \\sim O4A-O3A
 with sigma of 0.04
 Cl1-O3A \\sim Cl1-O3B
 with sigma of 0.02
 Cl1-O1A \\sim Cl1-O1B
 with sigma of 0.02
 O1A-O3B \\sim O1B-O3B
 with sigma of 0.02
 Cl1-O2A \\sim Cl1-O2B
 with sigma of 0.02
 Cl1-O4A \\sim Cl1-O4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O1A \\sim O2A \\sim O3A \\sim O4A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl1, O1A, O2A, O3A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C17(H17), C18(H18)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C5(H5A,H5B), C6(H6A,H6B), C27(H27A,H27B),
 C28(H28A,H28B), C19(H19A,H19B), C20(H20A,H20B)
6.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 4.313
_oxdiff_exptl_absorpt_empirical_full_min 0.213
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 0.2270(2) 0.51294(14) 0.30713(3) 0.0639(3) Uani 1 1 d D U . . .
O1A O 0.2586(15) 0.4784(16) 0.2666(2) 0.140(4) Uani 0.560(8) 1 d D U P A 1
O2A O 0.3811(17) 0.5743(18) 0.3360(4) 0.131(5) Uani 0.560(8) 1 d D U P A 1
O3A O 0.0708(10) 0.6191(8) 0.3107(2) 0.088(3) Uani 0.560(8) 1 d D U P A 1
O4A O 0.1290(16) 0.3591(9) 0.3229(3) 0.089(3) Uani 0.560(8) 1 d D U P A 1
O1B O 0.2332(18) 0.6228(12) 0.2759(3) 0.106(4) Uani 0.440(8) 1 d D . P A 2
O2B O 0.3153(17) 0.6035(16) 0.3446(3) 0.076(4) Uani 0.440(8) 1 d D . P A 2
O3B O 0.4207(17) 0.4552(17) 0.2955(4) 0.140(5) Uani 0.440(8) 1 d D . P A 2
O4B O 0.073(2) 0.3834(16) 0.3071(4) 0.116(6) Uani 0.440(8) 1 d D . P A 2
S1 S 0.69385(12) 0.04997(11) 0.59404(2) 0.0348(2) Uani 1 1 d . . . . .
S2 S 0.82637(12) 0.18350(10) 0.50707(2) 0.0339(2) Uani 1 1 d . . . . .
S3 S 0.28851(13) 0.12666(10) 0.58019(2) 0.0340(2) Uani 1 1 d . . . . .
S4 S 0.42150(12) 0.26719(10) 0.49279(2) 0.0328(2) Uani 1 1 d . . . . .
S5 S 0.99846(13) 0.32098(12) 0.43257(3) 0.0446(2) Uani 1 1 d . . . . .
S6 S 0.50953(13) 0.41630(11) 0.41466(3) 0.0363(2) Uani 1 1 d . . . . .
C9 C 0.5276(5) 0.1252(4) 0.56165(9) 0.0279(6) Uani 1 1 d . . . . .
C10 C 0.5840(5) 0.1820(4) 0.52430(9) 0.0282(6) Uani 1 1 d . . . . .
C7 C 0.5284(5) 0.0209(4) 0.63405(10) 0.0328(7) Uani 1 1 d . . . . .
C11 C 0.7870(5) 0.2838(4) 0.46279(9) 0.0321(7) Uani 1 1 d . . . . .
C8 C 0.3426(5) 0.0567(4) 0.62788(9) 0.0315(7) Uani 1 1 d . . . . .
C12 C 0.6006(5) 0.3212(4) 0.45579(9) 0.0293(7) Uani 1 1 d . . . . .
C13 C 0.9297(5) 0.4881(4) 0.40558(11) 0.0404(8) Uani 1 1 d . . . . .
H13A H 0.924491 0.581626 0.425122 0.049 Uiso 1 1 calc R U . . .
H13B H 1.034013 0.523401 0.386513 0.049 Uiso 1 1 calc R U . . .
C14 C 0.7267(5) 0.4392(5) 0.38228(10) 0.0398(8) Uani 1 1 d . . . . .
H14A H 0.724894 0.334943 0.366244 0.048 Uiso 1 1 calc R U . . .
H14B H 0.712497 0.522665 0.363230 0.048 Uiso 1 1 calc R U . . .
C5 C 0.6047(5) -0.0296(5) 0.67399(10) 0.0439(9) Uani 1 1 d . . . . .
H5A H 0.716266 0.055452 0.685408 0.053 Uiso 1 1 calc R U . . .
H5B H 0.657382 -0.131807 0.669095 0.053 Uiso 1 1 calc R U . . .
C6 C 0.1861(5) 0.0462(5) 0.66006(10) 0.0394(8) Uani 1 1 d . . . . .
H6A H 0.086721 -0.055242 0.654518 0.047 Uiso 1 1 calc R U . . .
H6B H 0.114932 0.139404 0.659011 0.047 Uiso 1 1 calc R U . . .
C3 C 0.4399(7) -0.0556(7) 0.70497(12) 0.0679(13) Uani 1 1 d . . . . .
H3 H 0.365579 -0.168448 0.697568 0.082 Uiso 1 1 calc R U . . .
C4 C 0.2863(7) 0.0480(7) 0.70218(12) 0.0680(13) Uani 1 1 d . . . . .
H4 H 0.360024 0.161921 0.708240 0.082 Uiso 1 1 calc R U . . .
C1 C 0.5379(7) -0.0650(6) 0.74741(12) 0.0671(13) Uani 1 1 d . . . . .
H1A H 0.634518 -0.139027 0.745541 0.101 Uiso 1 1 calc R U . . .
H1B H 0.434351 -0.105612 0.765708 0.101 Uiso 1 1 calc R U . . .
H1C H 0.606711 0.043594 0.757717 0.101 Uiso 1 1 calc R U . . .
C2 C 0.1225(7) 0.0243(6) 0.73380(12) 0.0655(13) Uani 1 1 d . . . . .
H2A H 0.030941 0.100818 0.730012 0.098 Uiso 1 1 calc R U . . .
H2B H 0.185966 0.044620 0.760968 0.098 Uiso 1 1 calc R U . . .
H2C H 0.047784 -0.087356 0.730305 0.098 Uiso 1 1 calc R U . . .
S7 S -0.22259(13) 0.70143(12) -0.01435(3) 0.0403(2) Uani 1 1 d . . . . .
S8 S -0.32635(13) 0.56233(12) 0.07307(3) 0.0389(2) Uani 1 1 d . . . . .
S9 S 0.21492(13) 0.76974(12) 0.00926(3) 0.0400(2) Uani 1 1 d . . . . .
S10 S 0.10919(13) 0.63017(12) 0.09889(2) 0.0382(2) Uani 1 1 d . . . . .
S11 S -0.47701(14) 0.51136(14) 0.15516(3) 0.0517(3) Uani 1 1 d . . . . .
S12 S 0.04376(14) 0.59241(13) 0.18716(3) 0.0476(3) Uani 1 1 d . . . . .
C23 C -0.0329(5) 0.6953(4) 0.02316(10) 0.0341(7) Uani 1 1 d . . . . .
C24 C -0.0763(5) 0.6348(4) 0.06018(10) 0.0341(7) Uani 1 1 d . . . . .
C21 C -0.0590(5) 0.8002(4) -0.04916(10) 0.0362(8) Uani 1 1 d . . . . .
C25 C -0.2638(5) 0.5600(4) 0.12586(10) 0.0359(7) Uani 1 1 d . . . . .
C22 C 0.1402(5) 0.8318(4) -0.03836(10) 0.0351(7) Uani 1 1 d . . . . .
C26 C -0.0657(5) 0.5913(4) 0.13762(10) 0.0348(7) Uani 1 1 d . . . . .
C27 C -0.3644(7) 0.5460(7) 0.20596(13) 0.0742(14) Uani 1 1 d . . . . .
H27A H -0.340642 0.664441 0.213623 0.089 Uiso 1 1 calc R U . . .
H27B H -0.461635 0.492934 0.224468 0.089 Uiso 1 1 calc R U . . .
C28 C -0.1708(7) 0.4856(7) 0.21230(13) 0.0710(14) Uani 1 1 d . . . . .
H28A H -0.192195 0.368887 0.202792 0.085 Uiso 1 1 calc R U . . .
H28B H -0.136527 0.493690 0.241571 0.085 Uiso 1 1 calc R U . . .
C19 C -0.1440(5) 0.8383(5) -0.08950(10) 0.0398(8) Uani 1 1 d . . . . .
H19A H -0.203419 0.937757 -0.085758 0.048 Uiso 1 1 calc R U . . .
H19B H -0.251589 0.747531 -0.099687 0.048 Uiso 1 1 calc R U . . .
C20 C 0.3004(5) 0.9074(5) -0.06604(11) 0.0416(8) Uani 1 1 d . . . . .
H20A H 0.385227 0.826446 -0.073617 0.050 Uiso 1 1 calc R U . . .
H20B H 0.386961 1.001910 -0.051165 0.050 Uiso 1 1 calc R U . . .
C17 C 0.0165(7) 0.8640(6) -0.12064(12) 0.0642(12) Uani 1 1 d . . . . .
H17 H 0.047274 0.753085 -0.127488 0.077 Uiso 1 1 calc R U . . .
C18 C 0.2100(6) 0.9633(6) -0.10450(12) 0.0626(12) Uani 1 1 d . . . . .
H18 H 0.174525 1.070686 -0.095581 0.075 Uiso 1 1 calc R U . . .
C15 C -0.0712(7) 0.9136(6) -0.16029(12) 0.0604(11) Uani 1 1 d . . . . .
H15A H -0.198650 0.841417 -0.167837 0.091 Uiso 1 1 calc R U . . .
H15B H 0.022503 0.904788 -0.181619 0.091 Uiso 1 1 calc R U . . .
H15C H -0.093034 1.026184 -0.156581 0.091 Uiso 1 1 calc R U . . .
C16 C 0.3764(6) 1.0071(6) -0.13491(13) 0.0588(11) Uani 1 1 d . . . . .
H16A H 0.493854 1.074978 -0.120785 0.088 Uiso 1 1 calc R U . . .
H16B H 0.326377 1.066788 -0.156195 0.088 Uiso 1 1 calc R U . . .
H16C H 0.413428 0.906963 -0.146839 0.088 Uiso 1 1 calc R U . . .
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
-1 -11 2 0.0530
-9 0 1 0.0533
0 11 -2 0.1034
6 8 -2 0.0890
9 0 -1 0.0683
3 -11 18 0.0936
-1 2 45 0.0441
1 -2 -45 0.0091
0 0 -46 0.0015
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
O1A Cl1 O2A 123.5(7) . . ?
O1A Cl1 O3A 109.6(5) . . ?
O1A Cl1 O4A 107.3(6) . . ?
O2A Cl1 O3A 107.8(6) . . ?
O2A Cl1 O4A 103.6(7) . . ?
O4A Cl1 O3A 103.2(5) . . ?
O1B Cl1 O2B 109.0(7) . . ?
O1B Cl1 O3B 94.0(7) . . ?
O2B Cl1 O3B 94.4(7) . . ?
O4B Cl1 O1B 120.0(7) . . ?
O4B Cl1 O2B 121.8(8) . . ?
O4B Cl1 O3B 110.6(10) . . ?
C9 S1 C7 95.67(15) . . ?
C10 S2 C11 95.32(14) . . ?
C9 S3 C8 95.84(14) . . ?
C10 S4 C12 95.36(14) . . ?
C11 S5 C13 98.56(15) . . ?
C12 S6 C14 101.53(15) . . ?
S1 C9 S3 114.73(16) . . ?
C10 C9 S1 122.1(2) . . ?
C10 C9 S3 123.1(2) . . ?
S2 C10 S4 115.56(16) . . ?
C9 C10 S2 122.1(2) . . ?
C9 C10 S4 122.2(2) . . ?
C8 C7 S1 117.1(2) . . ?
C8 C7 C5 123.5(3) . . ?
C5 C7 S1 119.2(2) . . ?
S5 C11 S2 114.61(18) . . ?
C12 C11 S2 117.3(2) . . ?
C12 C11 S5 128.1(2) . . ?
C7 C8 S3 116.5(2) . . ?
C7 C8 C6 123.5(3) . . ?
C6 C8 S3 119.9(2) . . ?
S6 C12 S4 114.48(18) . . ?
C11 C12 S4 116.4(2) . . ?
C11 C12 S6 129.1(2) . . ?
S5 C13 H13A 109.1 . . ?
S5 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 S5 112.3(3) . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
S6 C14 H14A 108.7 . . ?
S6 C14 H14B 108.7 . . ?
C13 C14 S6 114.1(2) . . ?
C13 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C7 C5 H5A 109.1 . . ?
C7 C5 H5B 109.1 . . ?
C7 C5 C3 112.6(3) . . ?
H5A C5 H5B 107.8 . . ?
C3 C5 H5A 109.1 . . ?
C3 C5 H5B 109.1 . . ?
C8 C6 H6A 109.5 . . ?
C8 C6 H6B 109.5 . . ?
C8 C6 C4 110.6(3) . . ?
H6A C6 H6B 108.1 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C5 C3 H3 104.4 . . ?
C5 C3 C1 109.4(4) . . ?
C4 C3 C5 115.7(3) . . ?
C4 C3 H3 104.4 . . ?
C4 C3 C1 117.0(4) . . ?
C1 C3 H3 104.4 . . ?
C6 C4 H4 105.2 . . ?
C6 C4 C2 109.4(3) . . ?
C3 C4 C6 115.0(4) . . ?
C3 C4 H4 105.2 . . ?
C3 C4 C2 115.8(4) . . ?
C2 C4 H4 105.2 . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C23 S7 C21 95.55(16) . . ?
C24 S8 C25 94.65(16) . . ?
C23 S9 C22 95.00(16) . . ?
C24 S10 C26 94.85(15) . . ?
C25 S11 C27 101.47(19) . . ?
C26 S12 C28 100.09(19) . . ?
S7 C23 S9 114.86(18) . . ?
C24 C23 S7 121.9(3) . . ?
C24 C23 S9 123.2(3) . . ?
S10 C24 S8 114.85(18) . . ?
C23 C24 S8 121.9(3) . . ?
C23 C24 S10 123.3(3) . . ?
C22 C21 S7 117.0(3) . . ?
C22 C21 C19 123.4(3) . . ?
C19 C21 S7 119.5(2) . . ?
S11 C25 S8 113.2(2) . . ?
C26 C25 S8 117.2(2) . . ?
C26 C25 S11 129.6(3) . . ?
C21 C22 S9 117.4(2) . . ?
C21 C22 C20 123.2(3) . . ?
C20 C22 S9 119.4(3) . . ?
S12 C26 S10 115.13(19) . . ?
C25 C26 S10 117.0(3) . . ?
C25 C26 S12 127.8(3) . . ?
S11 C27 H27A 108.3 . . ?
S11 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C28 C27 S11 115.8(3) . . ?
C28 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
S12 C28 H28A 108.3 . . ?
S12 C28 H28B 108.3 . . ?
C27 C28 S12 115.8(3) . . ?
C27 C28 H28A 108.3 . . ?
C27 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C21 C19 H19A 109.2 . . ?
C21 C19 H19B 109.2 . . ?
C21 C19 C17 111.9(3) . . ?
H19A C19 H19B 107.9 . . ?
C17 C19 H19A 109.2 . . ?
C17 C19 H19B 109.2 . . ?
C22 C20 H20A 109.1 . . ?
C22 C20 H20B 109.1 . . ?
C22 C20 C18 112.5(3) . . ?
H20A C20 H20B 107.8 . . ?
C18 C20 H20A 109.1 . . ?
C18 C20 H20B 109.1 . . ?
C19 C17 H17 104.8 . . ?
C19 C17 C15 110.6(3) . . ?
C18 C17 C19 114.0(4) . . ?
C18 C17 H17 104.8 . . ?
C18 C17 C15 116.5(4) . . ?
C15 C17 H17 104.8 . . ?
C20 C18 H18 103.9 . . ?
C20 C18 C16 109.9(3) . . ?
C17 C18 C20 115.9(3) . . ?
C17 C18 H18 103.9 . . ?
C17 C18 C16 117.5(4) . . ?
C16 C18 H18 103.9 . . ?
C17 C15 H15A 109.5 . . ?
C17 C15 H15B 109.5 . . ?
C17 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 H16A 109.5 . . ?
C18 C16 H16B 109.5 . . ?
C18 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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 O1A 1.368(6) . ?
Cl1 O2A 1.371(8) . ?
Cl1 O3A 1.473(5) . ?
Cl1 O4A 1.452(7) . ?
Cl1 O1B 1.404(7) . ?
Cl1 O2B 1.437(8) . ?
Cl1 O3B 1.504(9) . ?
Cl1 O4B 1.343(10) . ?
S1 C9 1.724(3) . ?
S1 C7 1.743(3) . ?
S2 C10 1.729(3) . ?
S2 C11 1.746(3) . ?
S3 C9 1.728(3) . ?
S3 C8 1.743(3) . ?
S4 C10 1.733(3) . ?
S4 C12 1.754(3) . ?
S5 C11 1.745(3) . ?
S5 C13 1.795(3) . ?
S6 C12 1.741(3) . ?
S6 C14 1.815(3) . ?
C9 C10 1.377(4) . ?
C7 C8 1.334(4) . ?
C7 C5 1.494(4) . ?
C11 C12 1.346(4) . ?
C8 C6 1.503(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.505(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C3 1.518(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C4 1.505(5) . ?
C3 H3 0.9800 . ?
C3 C4 1.445(6) . ?
C3 C1 1.523(5) . ?
C4 H4 0.9800 . ?
C4 C2 1.527(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
S7 C23 1.738(3) . ?
S7 C21 1.745(3) . ?
S8 C24 1.745(3) . ?
S8 C25 1.761(3) . ?
S9 C23 1.745(3) . ?
S9 C22 1.751(3) . ?
S10 C24 1.743(3) . ?
S10 C26 1.759(3) . ?
S11 C25 1.746(3) . ?
S11 C27 1.780(5) . ?
S12 C26 1.750(3) . ?
S12 C28 1.798(4) . ?
C23 C24 1.360(4) . ?
C21 C22 1.337(5) . ?
C21 C19 1.490(4) . ?
C25 C26 1.337(5) . ?
C22 C20 1.502(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.474(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C17 1.501(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C18 1.508(5) . ?
C17 H17 0.9800 . ?
C17 C18 1.459(6) . ?
C17 C15 1.511(5) . ?
C18 H18 0.9800 . ?
C18 C16 1.528(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
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 C9 C10 S2 -0.4(4) . . . . ?
S1 C9 C10 S4 -176.75(18) . . . . ?
S1 C7 C8 S3 0.5(4) . . . . ?
S1 C7 C8 C6 -176.9(3) . . . . ?
S1 C7 C5 C3 -178.0(3) . . . . ?
S2 C11 C12 S4 1.1(4) . . . . ?
S2 C11 C12 S6 -178.68(19) . . . . ?
S3 C9 C10 S2 178.47(17) . . . . ?
S3 C9 C10 S4 2.1(4) . . . . ?
S3 C8 C6 C4 -158.3(3) . . . . ?
S5 C11 C12 S4 -179.7(2) . . . . ?
S5 C11 C12 S6 0.6(5) . . . . ?
S5 C13 C14 S6 72.3(3) . . . . ?
C9 S1 C7 C8 1.7(3) . . . . ?
C9 S1 C7 C5 -173.7(3) . . . . ?
C9 S3 C8 C7 -2.5(3) . . . . ?
C9 S3 C8 C6 175.1(3) . . . . ?
C10 S2 C11 S5 179.17(19) . . . . ?
C10 S2 C11 C12 -1.5(3) . . . . ?
C10 S4 C12 S6 179.74(18) . . . . ?
C10 S4 C12 C11 -0.1(3) . . . . ?
C7 S1 C9 S3 -3.4(2) . . . . ?
C7 S1 C9 C10 175.6(3) . . . . ?
C7 C8 C6 C4 19.1(5) . . . . ?
C7 C5 C3 C4 -31.7(6) . . . . ?
C7 C5 C3 C1 -166.4(4) . . . . ?
C11 S2 C10 S4 1.4(2) . . . . ?
C11 S2 C10 C9 -175.2(3) . . . . ?
C11 S5 C13 C14 -57.9(3) . . . . ?
C8 S3 C9 S1 3.6(2) . . . . ?
C8 S3 C9 C10 -175.3(3) . . . . ?
C8 C7 C5 C3 6.9(6) . . . . ?
C8 C6 C4 C3 -43.5(5) . . . . ?
C8 C6 C4 C2 -175.9(4) . . . . ?
C12 S4 C10 S2 -1.0(2) . . . . ?
C12 S4 C10 C9 175.6(3) . . . . ?
C12 S6 C14 C13 -39.5(3) . . . . ?
C13 S5 C11 S2 -157.9(2) . . . . ?
C13 S5 C11 C12 22.9(4) . . . . ?
C14 S6 C12 S4 -176.28(18) . . . . ?
C14 S6 C12 C11 3.5(4) . . . . ?
C5 C7 C8 S3 175.8(3) . . . . ?
C5 C7 C8 C6 -1.7(5) . . . . ?
C5 C3 C4 C6 51.9(6) . . . . ?
C5 C3 C4 C2 -178.9(4) . . . . ?
C1 C3 C4 C6 -176.9(4) . . . . ?
C1 C3 C4 C2 -47.7(7) . . . . ?
S7 C23 C24 S8 -1.2(4) . . . . ?
S7 C23 C24 S10 -178.76(18) . . . . ?
S7 C21 C22 S9 0.4(4) . . . . ?
S7 C21 C22 C20 176.5(3) . . . . ?
S7 C21 C19 C17 -159.3(3) . . . . ?
S8 C25 C26 S10 -0.3(4) . . . . ?
S8 C25 C26 S12 -178.14(19) . . . . ?
S9 C23 C24 S8 179.67(18) . . . . ?
S9 C23 C24 S10 2.1(5) . . . . ?
S9 C22 C20 C18 -176.5(3) . . . . ?
S11 C25 C26 S10 178.1(2) . . . . ?
S11 C25 C26 S12 0.3(5) . . . . ?
S11 C27 C28 S12 67.8(5) . . . . ?
C23 S7 C21 C22 2.2(3) . . . . ?
C23 S7 C21 C19 179.7(3) . . . . ?
C23 S9 C22 C21 -2.7(3) . . . . ?
C23 S9 C22 C20 -179.0(3) . . . . ?
C24 S8 C25 S11 174.34(19) . . . . ?
C24 S8 C25 C26 -7.0(3) . . . . ?
C24 S10 C26 S12 -174.5(2) . . . . ?
C24 S10 C26 C25 7.4(3) . . . . ?
C21 S7 C23 S9 -4.0(2) . . . . ?
C21 S7 C23 C24 176.8(3) . . . . ?
C21 C22 C20 C18 7.5(5) . . . . ?
C21 C19 C17 C18 -42.6(5) . . . . ?
C21 C19 C17 C15 -176.2(4) . . . . ?
C25 S8 C24 S10 11.9(2) . . . . ?
C25 S8 C24 C23 -165.8(3) . . . . ?
C25 S11 C27 C28 -41.9(4) . . . . ?
C22 S9 C23 S7 4.1(2) . . . . ?
C22 S9 C23 C24 -176.7(3) . . . . ?
C22 C21 C19 C17 18.0(5) . . . . ?
C22 C20 C18 C17 -32.9(5) . . . . ?
C22 C20 C18 C16 -169.0(3) . . . . ?
C26 S10 C24 S8 -12.0(2) . . . . ?
C26 S10 C24 C23 165.7(3) . . . . ?
C26 S12 C28 C27 -48.9(4) . . . . ?
C27 S11 C25 S8 -172.8(2) . . . . ?
C27 S11 C25 C26 8.7(4) . . . . ?
C28 S12 C26 S10 -162.3(2) . . . . ?
C28 S12 C26 C25 15.6(4) . . . . ?
C19 C21 C22 S9 -177.0(3) . . . . ?
C19 C21 C22 C20 -0.8(6) . . . . ?
C19 C17 C18 C20 52.0(6) . . . . ?
C19 C17 C18 C16 -175.3(4) . . . . ?
C15 C17 C18 C20 -177.2(4) . . . . ?
C15 C17 C18 C16 -44.5(6) . . . . ?
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
-1.3297 -10.9749 2.1027 -0.0007 0.4808 0.8768
-9.2276 -0.1455 1.1066 -0.0015 0.9856 -0.1690
-0.1834 11.4154 -2.0037 0.0005 -0.3336 -0.9427
5.6256 7.8932 -2.0592 0.0013 -0.8423 -0.5391
9.1991 0.3242 -1.1349 0.0015 -0.9881 0.1537
3.0140 -10.6886 18.4211 0.3675 -0.0005 0.9300
-0.7498 1.5978 45.0674 0.9857 0.0017 -0.1688
0.7317 -1.5349 -45.1191 -0.9866 -0.0017 0.1632
0.1889 0.3379 -46.0037 -1.0000 -0.0015 -0.0012
