#------------------------------------------------------------------------------
#$Date: 2024-09-02 12:36:32 +0300 (Mon, 02 Sep 2024) $
#$Revision: 294326 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244375.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_7244375
loop_
_publ_author_name
'zigon, nicolas'
'Avarvari, Narcis'
_publ_section_title
;
 [4]Helicene based anions in electrocrystallization with
 tetrachalcogenafulvalene donors
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00091A
_journal_year                    2022
_chemical_formula_moiety         'C18 H11 O3 S, C10 H12 S4'
_chemical_formula_sum            'C28 H23 O3 S5'
_chemical_formula_weight         567.76
_chemical_name_systematic        ([4]heliceneSO3)2(TMTTF)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-01-17 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.089(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5199(9)
_cell_length_b                   21.0758(15)
_cell_length_c                   19.3165(10)
_cell_measurement_reflns_used    2545
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.6810
_cell_measurement_theta_min      3.8460
_cell_volume                     4984.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00   4.00   1.00   16.50    --   41.11 -19.00-180.00   42
  2  ω     38.00  79.00   1.00   16.50    --   41.11-125.00  30.00   41
  3  ω    -30.00  26.00   1.00   16.50    --   41.11 -19.00 -60.00   56
  4  ω    -27.00  64.00   1.00   16.50    --   41.11 -57.00  60.00   91
  5  ω     22.00 106.00   1.00   66.00    --  103.45 -94.00 -60.00   84
  6  ω     38.00  67.00   1.00   66.00    --  103.45 -61.00 -30.00   29
  7  ω     52.00 158.00   1.00   66.00    --  103.45  15.00 -90.00  106
  8  ω     78.00 152.00   1.00   66.00    --  103.45  45.00 150.00   74
  9  ω     35.00  71.00   1.00   66.00    --  103.45 -61.00-150.00   36
 10  ω     27.00 105.00   1.00   66.00    --  103.45 -77.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1014154000
_diffrn_orient_matrix_UB_12      -0.0092726000
_diffrn_orient_matrix_UB_13      -0.0323833000
_diffrn_orient_matrix_UB_21      0.0743003000
_diffrn_orient_matrix_UB_22      0.0182806000
_diffrn_orient_matrix_UB_23      0.0713094000
_diffrn_orient_matrix_UB_31      0.0059428000
_diffrn_orient_matrix_UB_32      -0.0701352000
_diffrn_orient_matrix_UB_33      0.0228307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18501
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.108
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.542
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_preparation       electrocrystallization
_exptl_crystal_recrystallization_method electrocrystallization
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9372
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0952
_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)+(0.1130P)²+34.8087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6052
_reflns_number_total             9372
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00091a2.cif
_cod_data_source_block           exp_1570
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H46 O6 S10'
_cod_original_formula_weight         1135.53
_cod_original_formula_moiety         '2(C18 H11 O3 S), 2(C10 H12 S4)'
_cod_original_formula_units_Z            4
_cod_database_code               7244375
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H32 O6 S6'
_chemical_oxdiff_usercomment     'purple platelets'
_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.
;
_diffrn_oxdiff_digest_frames
;
0187f8fa3ad90dc5f3ae776562d3b379bb006658a05
;
_diffrn_oxdiff_digest_hkl
;
01f2c9a12142968b6e73b80de6e1caa6fa00ce
;
_reflns_odcompleteness_completeness 98.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9251(15)
 0.0749(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C22) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C6, C5, C4, C3, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C11(H11), C3(H3), C4(H4), C7(H7), C8(H8), C18(H18),
 C17(H17), C2(H2), C1(H1), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
 C26(H26), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C)
;
_ins_header
;
TITL exp_1570 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  12.519922  21.075814  19.316516  90.0000 102.0890  90.0000
ZERR    5.00   0.000946   0.001454   0.001037   0.0000   0.0062   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O S
UNIT 230.00 160.00 30.00 30.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection 2020-09-23
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_1570
_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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.874
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.0814(6) 0.7444(3) 0.2533(3) 0.0400(16) Uani 1 1 d . . . . .
S1 S 0.10217(19) 0.70763(13) 0.31809(12) 0.0362(5) Uani 1 1 d . . . . .
O2 O 0.0038(6) 0.6858(4) 0.3382(4) 0.056(2) Uani 1 1 d . . . . .
S2 S -0.03311(19) 0.37309(11) 0.33959(11) 0.0325(5) Uani 1 1 d . . . . .
S3 S 0.07689(17) 0.76439(11) -0.10535(10) 0.0299(5) Uani 1 1 d . . . . .
O3 O 0.1776(6) 0.7411(4) 0.3733(4) 0.052(2) Uani 1 1 d . . . . .
C6 C 0.4295(8) 0.5249(5) 0.1742(5) 0.036(2) Uani 1 1 d . U . . .
C12 C 0.3120(8) 0.6960(5) 0.2539(5) 0.037(2) Uani 1 1 d . . . . .
H12 H 0.286634 0.734062 0.268733 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3906(7) 0.5809(4) 0.2065(5) 0.0304(19) Uani 1 1 d . . . . .
C13 C 0.2630(7) 0.6380(4) 0.2670(4) 0.0275(17) Uani 1 1 d . U . . .
C15 C 0.1712(8) 0.6369(5) 0.3009(5) 0.038(2) Uani 1 1 d . U . . .
C16 C 0.1298(10) 0.5799(5) 0.3187(6) 0.049(3) Uani 1 1 d . U . . .
H16 H 0.066659 0.578694 0.336824 0.059 Uiso 1 1 calc R . . . .
C11 C 0.3964(8) 0.6959(4) 0.2194(5) 0.034(2) Uani 1 1 d . . . . .
H11 H 0.429108 0.734302 0.212181 0.041 Uiso 1 1 calc R . . . .
C14 C 0.3090(8) 0.5790(4) 0.2488(5) 0.0335(19) Uani 1 1 d . U . . .
C9 C 0.4355(8) 0.6399(5) 0.1945(5) 0.036(2) Uani 1 1 d . . . . .
C3 C 0.5029(13) 0.4186(7) 0.1061(11) 0.089(5) Uani 1 1 d . U . . .
H3 H 0.527771 0.383551 0.084896 0.107 Uiso 1 1 calc R . . . .
C4 C 0.5459(16) 0.4797(7) 0.1005(12) 0.107(7) Uani 1 1 d . U . . .
H4 H 0.597596 0.485287 0.072778 0.129 Uiso 1 1 calc R . . . .
C5 C 0.5135(12) 0.5325(6) 0.1354(9) 0.073(4) Uani 1 1 d . U . . .
C7 C 0.5574(15) 0.5934(7) 0.1287(11) 0.098(7) Uani 1 1 d . . . . .
H7 H 0.612916 0.598139 0.103802 0.118 Uiso 1 1 calc R . . . .
C8 C 0.5219(9) 0.6417(5) 0.1562(6) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.554142 0.680738 0.151192 0.058 Uiso 1 1 calc R . . . .
C18 C 0.2697(14) 0.5236(6) 0.2751(9) 0.078(5) Uani 1 1 d . U . . .
H18 H 0.303045 0.485152 0.269101 0.093 Uiso 1 1 calc R . . . .
C17 C 0.1847(14) 0.5239(6) 0.3089(9) 0.079(5) Uani 1 1 d . U . . .
H17 H 0.162593 0.485924 0.325964 0.095 Uiso 1 1 calc R . . . .
C2 C 0.4245(14) 0.4136(6) 0.1434(12) 0.101(7) Uani 1 1 d . U . . .
H2 H 0.395960 0.373814 0.149763 0.121 Uiso 1 1 calc R . . . .
C1 C 0.3855(12) 0.4651(6) 0.1723(10) 0.087(6) Uani 1 1 d . U . . .
H1 H 0.324716 0.459496 0.192241 0.105 Uiso 1 1 calc R . . . .
S4 S 0.22396(17) 0.76742(12) 0.03177(11) 0.0317(5) Uani 1 1 d . . . . .
O4 O 0.0532(6) 0.3646(5) 0.4021(4) 0.057(2) Uani 1 1 d . . . . .
S5 S -0.12788(16) 0.75163(10) -0.03131(10) 0.0252(4) Uani 1 1 d . . . . .
O5 O -0.1073(6) 0.3195(4) 0.3268(4) 0.0494(19) Uani 1 1 d . . . . .
S6 S 0.01662(17) 0.75176(11) 0.10727(10) 0.0282(5) Uani 1 1 d . . . . .
O6 O -0.0871(7) 0.4335(4) 0.3390(4) 0.053(2) Uani 1 1 d . . . . .
S7 S 0.58715(19) 0.57724(11) 0.37396(12) 0.0340(5) Uani 1 1 d . . . . .
S8 S 0.73774(18) 0.57604(11) 0.51052(11) 0.0316(5) Uani 1 1 d . . . . .
S9 S 0.38370(18) 0.58918(11) 0.45305(11) 0.0314(5) Uani 1 1 d . . . . .
S10 S 0.53402(18) 0.58464(12) 0.58976(11) 0.0340(5) Uani 1 1 d . . . . .
C19 C 0.1430(13) 0.4357(6) 0.0204(7) 0.063(4) Uani 1 1 d . . . . .
H19 H 0.183740 0.442755 0.065799 0.075 Uiso 1 1 calc R . . . .
C20 C 0.1904(14) 0.4469(6) -0.0373(7) 0.070(4) Uani 1 1 d . . . . .
H20 H 0.262620 0.460310 -0.030341 0.084 Uiso 1 1 calc R . . . .
C21 C 0.1290(18) 0.4380(7) -0.1060(8) 0.083(5) Uani 1 1 d . . . . .
H21 H 0.161440 0.442645 -0.144790 0.099 Uiso 1 1 calc R . . . .
C22 C 0.0228(19) 0.4228(7) -0.1153(7) 0.087(6) Uani 1 1 d . U . . .
H22 H -0.017441 0.420503 -0.161517 0.104 Uiso 1 1 calc R . . . .
C23 C -0.0274(13) 0.4110(6) -0.0652(7) 0.063(4) Uani 1 1 d . . . . .
C24 C 0.0343(14) 0.4140(5) 0.0118(6) 0.066(4) Uani 1 1 d . . . . .
C25 C -0.1403(14) 0.3991(6) -0.0714(7) 0.069(4) Uani 1 1 d . . . . .
H25 H -0.179411 0.390081 -0.116784 0.083 Uiso 1 1 calc R . . . .
C26 C -0.2010(14) 0.3989(7) -0.0180(6) 0.077(5) Uani 1 1 d . . . . .
H26 H -0.276967 0.399763 -0.027122 0.093 Uiso 1 1 calc R . . . .
C27 C -0.1323(10) 0.3974(5) 0.0539(5) 0.046(3) Uani 1 1 d . . . . .
C28 C -0.0200(9) 0.4002(5) 0.0694(5) 0.040(2) Uani 1 1 d . . . . .
C29 C -0.1888(9) 0.3956(5) 0.1106(6) 0.045(3) Uani 1 1 d . . . . .
H29 H -0.264802 0.395575 0.099513 0.055 Uiso 1 1 calc R . . . .
C30 C -0.1387(8) 0.3939(4) 0.1788(6) 0.037(2) Uani 1 1 d . . . . .
H30 H -0.178526 0.397087 0.214217 0.045 Uiso 1 1 calc R . . . .
C31 C -0.0201(7) 0.3871(4) 0.1965(5) 0.0305(19) Uani 1 1 d . . . . .
C32 C 0.0381(8) 0.3880(4) 0.1410(5) 0.0314(19) Uani 1 1 d . . . . .
C33 C 0.0349(7) 0.3746(4) 0.2678(5) 0.0301(19) Uani 1 1 d . . . . .
C34 C 0.1451(7) 0.3612(4) 0.2816(5) 0.0289(18) Uani 1 1 d . . . . .
H34 H 0.182050 0.354557 0.328102 0.035 Uiso 1 1 calc R . . . .
C35 C 0.2024(7) 0.3574(4) 0.2266(5) 0.0310(19) Uani 1 1 d . . . . .
H35 H 0.276271 0.346993 0.236606 0.037 Uiso 1 1 calc R . . . .
C36 C 0.1501(8) 0.3689(4) 0.1586(5) 0.033(2) Uani 1 1 d . . . . .
H36 H 0.188330 0.364208 0.122459 0.040 Uiso 1 1 calc R . . . .
C37 C 0.2455(9) 0.7625(5) -0.1768(5) 0.041(2) Uani 1 1 d . . . . .
H37A H 0.205204 0.794607 -0.206545 0.062 Uiso 1 1 calc GR . . . .
H37B H 0.228325 0.721611 -0.198066 0.062 Uiso 1 1 calc GR . . . .
H37C H 0.322378 0.770423 -0.171264 0.062 Uiso 1 1 calc GR . . . .
C38 C 0.2154(7) 0.7639(4) -0.1056(5) 0.0300(19) Uani 1 1 d . . . . .
C39 C 0.2842(7) 0.7633(4) -0.0421(5) 0.0304(19) Uani 1 1 d . . . . .
C40 C 0.4060(8) 0.7584(5) -0.0258(5) 0.040(2) Uani 1 1 d . . . . .
H40A H 0.427331 0.717522 -0.005724 0.060 Uiso 1 1 calc GR . . . .
H40B H 0.436157 0.790917 0.007408 0.060 Uiso 1 1 calc GR . . . .
H40C H 0.432615 0.763680 -0.068560 0.060 Uiso 1 1 calc GR . . . .
C41 C 0.0925(7) 0.7636(4) -0.0147(5) 0.0304(19) Uani 1 1 d . . . . .
C42 C 0.0002(7) 0.7563(4) 0.0171(4) 0.0255(17) Uani 1 1 d . . . . .
C43 C -0.1878(7) 0.7409(4) 0.0413(5) 0.0316(19) Uani 1 1 d . . . . .
C44 C -0.1202(7) 0.7417(5) 0.1055(5) 0.033(2) Uani 1 1 d . . . . .
C45 C -0.1585(9) 0.7289(6) 0.1733(5) 0.044(2) Uani 1 1 d . . . . .
H45A H -0.105171 0.744436 0.212765 0.066 Uiso 1 1 calc GR . . . .
H45B H -0.167985 0.684095 0.178407 0.066 Uiso 1 1 calc GR . . . .
H45C H -0.226853 0.750140 0.171744 0.066 Uiso 1 1 calc GR . . . .
C46 C -0.3087(7) 0.7271(5) 0.0287(5) 0.040(2) Uani 1 1 d . . . . .
H46A H -0.319857 0.682129 0.031155 0.060 Uiso 1 1 calc GR . . . .
H46B H -0.343760 0.742337 -0.017274 0.060 Uiso 1 1 calc GR . . . .
H46C H -0.339375 0.747963 0.064198 0.060 Uiso 1 1 calc GR . . . .
C47 C 0.7590(10) 0.5642(5) 0.3028(6) 0.047(3) Uani 1 1 d . . . . .
H47A H 0.774551 0.520483 0.294905 0.071 Uiso 1 1 calc GR . . . .
H47B H 0.822995 0.589319 0.303190 0.071 Uiso 1 1 calc GR . . . .
H47C H 0.700630 0.578623 0.265698 0.071 Uiso 1 1 calc GR . . . .
C48 C 0.7254(8) 0.5706(5) 0.3733(5) 0.037(2) Uani 1 1 d . . . . .
C49 C 0.7948(8) 0.5706(5) 0.4366(5) 0.035(2) Uani 1 1 d . . . . .
C50 C 0.9172(7) 0.5651(5) 0.4461(5) 0.035(2) Uani 1 1 d . . . . .
H50A H 0.950116 0.565864 0.495716 0.052 Uiso 1 1 calc GR . . . .
H50B H 0.944386 0.599951 0.422896 0.052 Uiso 1 1 calc GR . . . .
H50C H 0.935047 0.525870 0.425913 0.052 Uiso 1 1 calc GR . . . .
C51 C 0.6037(7) 0.5780(4) 0.4645(5) 0.0310(19) Uani 1 1 d . . . . .
C52 C 0.5171(8) 0.5838(4) 0.4990(5) 0.0309(19) Uani 1 1 d . . . . .
C53 C 0.3260(7) 0.5936(4) 0.5280(5) 0.032(2) Uani 1 1 d . . . . .
C54 C 0.3951(8) 0.5920(5) 0.5911(5) 0.036(2) Uani 1 1 d . . . . .
C55 C 0.3687(9) 0.5969(6) 0.6634(5) 0.046(3) Uani 1 1 d . . . . .
H55A H 0.389182 0.558211 0.689010 0.069 Uiso 1 1 calc GR . . . .
H55B H 0.291765 0.603863 0.658652 0.069 Uiso 1 1 calc GR . . . .
H55C H 0.408398 0.631700 0.688629 0.069 Uiso 1 1 calc GR . . . .
C56 C 0.2036(8) 0.6000(5) 0.5123(5) 0.040(2) Uani 1 1 d . . . . .
H56A H 0.181798 0.632524 0.477377 0.059 Uiso 1 1 calc GR . . . .
H56B H 0.179957 0.611253 0.554886 0.059 Uiso 1 1 calc GR . . . .
H56C H 0.170871 0.560438 0.494666 0.059 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 12 -5 0.0433
-1 -13 4 0.0325
-7 4 7 0.0269
7 -5 -6 0.0235
-2 2 -11 0.0587
3 1 11 0.0634
-1 -13 -1 0.0315
1 14 0 0.0385
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 O3 110.3(5) . . ?
O1 S1 C15 106.9(4) . . ?
O2 S1 O1 113.3(4) . . ?
O2 S1 O3 114.7(5) . . ?
O2 S1 C15 104.9(5) . . ?
O3 S1 C15 106.0(5) . . ?
O4 S2 C33 104.9(4) . . ?
O5 S2 O4 112.6(5) . . ?
O5 S2 C33 106.0(4) . . ?
O6 S2 O4 112.4(5) . . ?
O6 S2 O5 113.8(5) . . ?
O6 S2 C33 106.3(4) . . ?
C41 S3 C38 95.9(4) . . ?
C5 C6 C10 118.8(9) . . ?
C1 C6 C10 125.7(9) . . ?
C1 C6 C5 115.3(10) . . ?
C11 C12 C13 119.8(9) . . ?
C14 C10 C6 124.0(8) . . ?
C9 C10 C6 117.6(8) . . ?
C9 C10 C14 118.4(8) . . ?
C12 C13 C15 120.9(9) . . ?
C12 C13 C14 119.5(8) . . ?
C15 C13 C14 119.6(8) . . ?
C13 C15 S1 122.3(8) . . ?
C16 C15 S1 117.3(8) . . ?
C16 C15 C13 120.3(9) . . ?
C15 C16 C17 118.7(10) . . ?
C12 C11 C9 122.1(9) . . ?
C10 C14 C13 118.7(8) . . ?
C18 C14 C10 125.1(9) . . ?
C18 C14 C13 116.2(9) . . ?
C10 C9 C8 118.6(9) . . ?
C11 C9 C10 120.6(8) . . ?
C11 C9 C8 120.7(9) . . ?
C2 C3 C4 116.7(13) . . ?
C5 C4 C3 122.3(13) . . ?
C4 C5 C6 118.9(12) . . ?
C4 C5 C7 121.3(12) . . ?
C7 C5 C6 119.7(11) . . ?
C8 C7 C5 120.9(11) . . ?
C7 C8 C9 124.2(10) . . ?
C17 C18 C14 122.6(12) . . ?
C18 C17 C16 121.7(12) . . ?
C3 C2 C1 121.7(13) . . ?
C2 C1 C6 124.6(12) . . ?
C41 S4 C39 95.8(4) . . ?
C42 S5 C43 94.7(4) . . ?
C42 S6 C44 94.6(4) . . ?
C51 S7 C48 95.7(4) . . ?
C51 S8 C49 95.8(5) . . ?
C52 S9 C53 95.8(4) . . ?
C52 S10 C54 96.0(4) . . ?
C20 C19 C24 121.6(14) . . ?
C19 C20 C21 119.7(16) . . ?
C22 C21 C20 119.4(14) . . ?
C23 C22 C21 124.9(15) . . ?
C22 C23 C24 119.9(16) . . ?
C22 C23 C25 127.5(16) . . ?
C25 C23 C24 112.4(12) . . ?
C19 C24 C23 114.0(11) . . ?
C19 C24 C28 124.8(13) . . ?
C28 C24 C23 121.1(14) . . ?
C26 C25 C23 128.6(12) . . ?
C25 C26 C27 113.1(14) . . ?
C28 C27 C26 125.0(12) . . ?
C28 C27 C29 118.9(9) . . ?
C29 C27 C26 116.1(12) . . ?
C27 C28 C24 117.6(11) . . ?
C27 C28 C32 119.2(9) . . ?
C32 C28 C24 123.2(11) . . ?
C30 C29 C27 123.5(10) . . ?
C29 C30 C31 118.6(10) . . ?
C32 C31 C30 118.7(9) . . ?
C32 C31 C33 120.7(8) . . ?
C33 C31 C30 120.4(9) . . ?
C31 C32 C28 119.4(9) . . ?
C31 C32 C36 116.9(8) . . ?
C36 C32 C28 123.3(9) . . ?
C31 C33 S2 122.9(7) . . ?
C34 C33 S2 118.1(7) . . ?
C34 C33 C31 119.0(8) . . ?
C33 C34 C35 121.0(8) . . ?
C36 C35 C34 120.1(8) . . ?
C35 C36 C32 121.9(8) . . ?
C37 C38 S3 116.5(7) . . ?
C39 C38 S3 116.6(7) . . ?
C39 C38 C37 126.9(9) . . ?
C38 C39 S4 116.2(7) . . ?
C38 C39 C40 128.6(8) . . ?
C40 C39 S4 115.2(7) . . ?
S4 C41 S3 115.3(5) . . ?
C42 C41 S3 120.6(7) . . ?
C42 C41 S4 124.0(7) . . ?
S5 C42 S6 117.4(5) . . ?
C41 C42 S5 122.1(6) . . ?
C41 C42 S6 120.5(7) . . ?
C44 C43 S5 116.5(7) . . ?
C44 C43 C46 124.5(8) . . ?
C46 C43 S5 118.8(7) . . ?
C43 C44 S6 116.8(7) . . ?
C43 C44 C45 122.9(8) . . ?
C45 C44 S6 120.1(7) . . ?
C47 C48 S7 118.5(8) . . ?
C49 C48 S7 116.7(7) . . ?
C49 C48 C47 124.8(9) . . ?
C48 C49 S8 116.8(7) . . ?
C48 C49 C50 124.0(8) . . ?
C50 C49 S8 119.2(7) . . ?
S7 C51 S8 114.9(5) . . ?
C52 C51 S7 123.3(7) . . ?
C52 C51 S8 121.7(7) . . ?
S10 C52 S9 115.1(5) . . ?
C51 C52 S9 121.8(7) . . ?
C51 C52 S10 123.1(7) . . ?
C54 C53 S9 116.9(7) . . ?
C54 C53 C56 128.4(9) . . ?
C56 C53 S9 114.7(7) . . ?
C53 C54 S10 116.2(7) . . ?
C53 C54 C55 128.2(9) . . ?
C55 C54 S10 115.6(7) . . ?
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 S1 1.448(7) . ?
S1 O2 1.443(7) . ?
S1 O3 1.452(8) . ?
S1 C15 1.788(11) . ?
S2 O4 1.452(8) . ?
S2 O5 1.449(7) . ?
S2 O6 1.441(8) . ?
S2 C33 1.773(9) . ?
S3 C38 1.736(9) . ?
S3 C41 1.721(9) . ?
C6 C10 1.465(13) . ?
C6 C5 1.423(15) . ?
C6 C1 1.372(16) . ?
C12 C13 1.414(13) . ?
C12 C11 1.362(13) . ?
C10 C14 1.437(13) . ?
C10 C9 1.405(13) . ?
C13 C15 1.438(13) . ?
C13 C14 1.444(13) . ?
C15 C16 1.381(15) . ?
C16 C17 1.397(18) . ?
C11 C9 1.401(13) . ?
C14 C18 1.401(15) . ?
C9 C8 1.433(13) . ?
C3 C4 1.41(2) . ?
C3 C2 1.34(2) . ?
C4 C5 1.404(18) . ?
C5 C7 1.412(19) . ?
C7 C8 1.272(17) . ?
C18 C17 1.360(18) . ?
C2 C1 1.356(17) . ?
S4 C39 1.751(9) . ?
S4 C41 1.704(9) . ?
S5 C42 1.681(9) . ?
S5 C43 1.739(9) . ?
S6 C42 1.714(8) . ?
S6 C44 1.719(9) . ?
S7 C48 1.739(10) . ?
S7 C51 1.717(9) . ?
S8 C49 1.730(9) . ?
S8 C51 1.727(9) . ?
S9 C52 1.723(10) . ?
S9 C53 1.750(9) . ?
S10 C52 1.721(9) . ?
S10 C54 1.752(10) . ?
C19 C20 1.388(17) . ?
C19 C24 1.41(2) . ?
C20 C21 1.40(2) . ?
C21 C22 1.34(2) . ?
C22 C23 1.28(2) . ?
C23 C24 1.53(2) . ?
C23 C25 1.42(2) . ?
C24 C28 1.451(14) . ?
C25 C26 1.40(2) . ?
C26 C27 1.473(14) . ?
C27 C28 1.375(16) . ?
C27 C29 1.424(16) . ?
C28 C32 1.446(13) . ?
C29 C30 1.336(15) . ?
C30 C31 1.459(13) . ?
C31 C32 1.417(13) . ?
C31 C33 1.430(13) . ?
C32 C36 1.429(14) . ?
C33 C34 1.379(13) . ?
C34 C35 1.404(12) . ?
C35 C36 1.362(14) . ?
C37 C38 1.500(12) . ?
C38 C39 1.343(13) . ?
C39 C40 1.494(13) . ?
C41 C42 1.426(11) . ?
C43 C44 1.347(13) . ?
C43 C46 1.510(12) . ?
C44 C45 1.509(12) . ?
C47 C48 1.513(13) . ?
C48 C49 1.342(14) . ?
C49 C50 1.510(12) . ?
C51 C52 1.393(12) . ?
C53 C54 1.340(14) . ?
C53 C56 1.506(13) . ?
C54 C55 1.504(13) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9251(15)
2 0.0749(15)
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
2.0020 12.0025 -5.0035 0.2538 0.0114 -0.9441
-1.0017 -13.0025 4.0063 -0.1108 -0.0264 0.9974
-7.0022 3.9981 6.9826 -0.9733 0.0507 -0.1626
7.0014 -4.9968 -5.9824 0.9501 0.0023 0.2555
-1.9895 1.9765 -10.9970 0.1360 -0.8959 -0.4015
2.9886 1.0275 10.9960 -0.0625 1.0250 0.1967
-0.9973 -13.0115 -0.9904 0.0516 -0.3826 0.8840
0.9981 14.0102 -0.0097 -0.0284 0.3296 -0.9769
