#------------------------------------------------------------------------------
#$Date: 2024-10-23 01:10:20 +0300 (Wed, 23 Oct 2024) $
#$Revision: 295581 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572924.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_1572924
loop_
_publ_author_name
'Adachi, Yohei'
'Yamada, Kohei'
'Ohshita, Joji'
_publ_section_title
;
 Controlling the thermodynamic stability of conformational isomers of
 bistricyclic aromatic enes by introducing boron and silicon atoms
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D4SC06150K
_journal_year                    2024
_chemical_formula_moiety         'C53 H45 B S4 Si'
_chemical_formula_sum            'C53 H45 B S4 Si'
_chemical_formula_weight         849.03
_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             2023-09-01
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-09-03 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                98.872(2)
_cell_angle_beta                 94.418(2)
_cell_angle_gamma                102.867(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0376(2)
_cell_length_b                   15.9768(4)
_cell_length_c                   15.9911(3)
_cell_measurement_reflns_used    26910
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9040
_cell_measurement_theta_min      2.3170
_cell_volume                     2209.16(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.27a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  45.00   0.50    1.00    --   10.15 -99.00 150.00  124
  2  ω    -65.00  26.00   0.50    1.00    --   10.15 -35.00  79.00  182
  3  ω     -5.00  45.00   0.50    1.00    --   10.15 -99.00   0.00  100
  4  ω     -6.00  23.00   0.50    1.00    --   10.15 -99.00-180.00   58
  5  ω    -83.00  -3.00   0.50    1.00    --   -9.53 -57.00-150.00  160
  6  ω    -83.00   8.00   0.50    1.00    --   -9.53 -57.00 -30.00  182
  7  ω    -13.00  17.00   0.50    1.00    --   10.15  77.00-150.00   60
  8  ω      0.00  27.00   0.50    1.00    --   10.15  35.00-122.00   54
  9  ω     46.00  72.00   0.50    1.00    --   10.15  35.00-122.00   52
 10  ω     52.00  78.00   0.50    1.00    --   10.15  77.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0725190000
_diffrn_orient_matrix_UB_12      0.0020228000
_diffrn_orient_matrix_UB_13      -0.0188075000
_diffrn_orient_matrix_UB_21      0.0233875000
_diffrn_orient_matrix_UB_22      0.0461961000
_diffrn_orient_matrix_UB_23      0.0075102000
_diffrn_orient_matrix_UB_31      0.0276200000
_diffrn_orient_matrix_UB_32      -0.0014794000
_diffrn_orient_matrix_UB_33      -0.0404051000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.962
_diffrn_reflns_theta_min         2.014
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.27a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         12614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0353
_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)+(0.0419P)²+0.7560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10617
_reflns_number_total             12614
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc06150k2.cif
_cod_data_source_block           exp_2694
_cod_original_cell_volume        2209.15(9)
_cod_database_code               1572924
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C53H45B1S4Si1
_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   0.978
_shelx_estimated_absorpt_t_min   0.939
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C21(H21), C22(H22), C23(H23), C24(H24), C30(H30), C31(H31),
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42),
  C43(H43), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_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 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.840
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
S1 S 0.46646(3) 0.41532(2) 0.36581(2) 0.01666(7) Uani 1 1 d . . . . .
S2 S 0.83226(4) 0.19500(2) 0.23351(2) 0.01502(7) Uani 1 1 d . . . . .
S3 S 0.83804(4) 0.74573(2) 0.18839(2) 0.01917(7) Uani 1 1 d . . . . .
S4 S 1.27513(3) 0.55228(2) 0.08282(2) 0.01610(7) Uani 1 1 d . . . . .
Si1 Si 1.14303(4) 0.67257(2) 0.22885(2) 0.01194(7) Uani 1 1 d . . . . .
C1 C -0.02667(16) -0.00440(10) 0.31165(9) 0.0252(3) Uani 1 1 d . . . . .
H1A H -0.067702 0.047640 0.313873 0.038 Uiso 1 1 calc R U . . .
H1B H 0.039922 0.000434 0.364390 0.038 Uiso 1 1 calc R U . . .
H1C H -0.111118 -0.056276 0.305408 0.038 Uiso 1 1 calc R U . . .
C2 C 0.06570(14) -0.01225(8) 0.23525(8) 0.0165(2) Uani 1 1 d . . . . .
H2 H 0.106785 -0.065397 0.235442 0.020 Uiso 1 1 calc R U . . .
C3 C -0.04156(16) -0.02766(9) 0.15314(9) 0.0240(3) Uani 1 1 d . . . . .
H3A H -0.131380 -0.074570 0.154877 0.036 Uiso 1 1 calc R U . . .
H3B H 0.011739 -0.044254 0.104416 0.036 Uiso 1 1 calc R U . . .
H3C H -0.074022 0.025946 0.147319 0.036 Uiso 1 1 calc R U . . .
C4 C 0.20229(13) 0.06534(8) 0.24214(8) 0.0135(2) Uani 1 1 d . . . . .
C5 C 0.24027(13) 0.10529(8) 0.17231(8) 0.0135(2) Uani 1 1 d . . . . .
H5 H 0.177951 0.083954 0.119349 0.016 Uiso 1 1 calc R U . . .
C6 C 0.36641(13) 0.17539(8) 0.17752(7) 0.0124(2) Uani 1 1 d . . . . .
C7 C 0.45967(13) 0.20794(8) 0.25618(7) 0.0125(2) Uani 1 1 d . . . . .
C8 C 0.42535(14) 0.16698(8) 0.32652(8) 0.0142(2) Uani 1 1 d . . . . .
C9 C 0.29843(14) 0.09671(8) 0.31846(8) 0.0156(2) Uani 1 1 d . . . . .
H9 H 0.276889 0.069441 0.366356 0.019 Uiso 1 1 calc R U . . .
C10 C 0.40485(14) 0.21823(8) 0.10025(8) 0.0160(2) Uani 1 1 d . . . . .
H10 H 0.518447 0.231719 0.100810 0.019 Uiso 1 1 calc R U . . .
C11 C 0.35599(18) 0.30479(9) 0.10508(9) 0.0254(3) Uani 1 1 d . . . . .
H11A H 0.392020 0.333354 0.057940 0.038 Uiso 1 1 calc R U . . .
H11B H 0.400455 0.342861 0.159401 0.038 Uiso 1 1 calc R U . . .
H11C H 0.244313 0.293388 0.100986 0.038 Uiso 1 1 calc R U . . .
C12 C 0.33554(17) 0.16071(9) 0.01459(8) 0.0232(3) Uani 1 1 d . . . . .
H12A H 0.224584 0.153981 0.008172 0.035 Uiso 1 1 calc R U . . .
H12B H 0.358292 0.103277 0.012316 0.035 Uiso 1 1 calc R U . . .
H12C H 0.379309 0.187988 -0.031629 0.035 Uiso 1 1 calc R U . . .
C13 C 0.52970(15) 0.19658(8) 0.41019(8) 0.0179(2) Uani 1 1 d . . . . .
H13 H 0.611955 0.247449 0.402924 0.022 Uiso 1 1 calc R U . . .
C14 C 0.60769(16) 0.12494(10) 0.43089(9) 0.0247(3) Uani 1 1 d . . . . .
H14A H 0.678942 0.147061 0.483052 0.037 Uiso 1 1 calc R U . . .
H14B H 0.663780 0.107794 0.383618 0.037 Uiso 1 1 calc R U . . .
H14C H 0.530117 0.074215 0.439204 0.037 Uiso 1 1 calc R U . . .
C15 C 0.44700(17) 0.22737(10) 0.48481(8) 0.0243(3) Uani 1 1 d . . . . .
H15A H 0.374631 0.177285 0.498610 0.036 Uiso 1 1 calc R U . . .
H15B H 0.391558 0.269848 0.468998 0.036 Uiso 1 1 calc R U . . .
H15C H 0.521878 0.254694 0.534593 0.036 Uiso 1 1 calc R U . . .
C16 C 0.59527(13) 0.38359(8) 0.30110(7) 0.0130(2) Uani 1 1 d . . . . .
C17 C 0.70847(13) 0.45568(8) 0.29275(7) 0.0125(2) Uani 1 1 d . . . . .
C18 C 0.83180(13) 0.44462(7) 0.23909(7) 0.0111(2) Uani 1 1 d . . . . .
C19 C 0.87216(13) 0.35933(8) 0.23511(7) 0.0120(2) Uani 1 1 d . . . . .
C20 C 0.75892(14) 0.28608(8) 0.24084(7) 0.0128(2) Uani 1 1 d . . . . .
C21 C 0.56709(15) 0.52222(8) 0.38525(8) 0.0169(2) Uani 1 1 d . . . . .
H21 H 0.538802 0.567376 0.421791 0.020 Uiso 1 1 calc R U . . .
C22 C 0.69270(14) 0.53491(8) 0.34206(8) 0.0145(2) Uani 1 1 d . . . . .
H22 H 0.761345 0.589966 0.344583 0.017 Uiso 1 1 calc R U . . .
C23 C 1.01302(14) 0.25372(8) 0.22687(8) 0.0165(2) Uani 1 1 d . . . . .
H23 H 1.099441 0.229244 0.223160 0.020 Uiso 1 1 calc R U . . .
C24 C 1.01815(14) 0.34019(8) 0.22753(7) 0.0139(2) Uani 1 1 d . . . . .
H24 H 1.108341 0.382519 0.223420 0.017 Uiso 1 1 calc R U . . .
C25 C 0.89239(13) 0.50602(7) 0.19299(7) 0.0114(2) Uani 1 1 d . . . . .
C26 C 0.93578(14) 0.66720(8) 0.20116(7) 0.0129(2) Uani 1 1 d . . . . .
C27 C 0.83563(13) 0.58620(8) 0.18946(7) 0.0119(2) Uani 1 1 d . . . . .
C28 C 1.02300(13) 0.50172(7) 0.14222(7) 0.0114(2) Uani 1 1 d . . . . .
C29 C 1.14770(13) 0.57230(8) 0.15342(7) 0.0129(2) Uani 1 1 d . . . . .
C30 C 0.66468(15) 0.67128(9) 0.16598(9) 0.0193(3) Uani 1 1 d . . . . .
H30 H 0.570150 0.685823 0.153068 0.023 Uiso 1 1 calc R U . . .
C31 C 0.67965(14) 0.58842(8) 0.16904(8) 0.0151(2) Uani 1 1 d . . . . .
H31 H 0.596581 0.538403 0.158840 0.018 Uiso 1 1 calc R U . . .
C32 C 1.16230(15) 0.45160(8) 0.03829(8) 0.0164(2) Uani 1 1 d . . . . .
H32 H 1.187792 0.413574 -0.007170 0.020 Uiso 1 1 calc R U . . .
C33 C 1.03167(14) 0.43272(8) 0.07599(7) 0.0138(2) Uani 1 1 d . . . . .
H33 H 0.955302 0.379812 0.060040 0.017 Uiso 1 1 calc R U . . .
C34 C 1.28112(14) 0.77494(8) 0.21782(8) 0.0142(2) Uani 1 1 d . . . . .
C35 C 1.38914(15) 0.81580(9) 0.28628(8) 0.0200(3) Uani 1 1 d . . . . .
H35 H 1.392460 0.789485 0.335547 0.024 Uiso 1 1 calc R U . . .
C36 C 1.49475(16) 0.89533(9) 0.28546(9) 0.0249(3) Uani 1 1 d . . . . .
H36 H 1.568780 0.921070 0.333254 0.030 Uiso 1 1 calc R U . . .
C37 C 1.49059(16) 0.93532(9) 0.21603(9) 0.0229(3) Uani 1 1 d . . . . .
H37 H 1.560353 0.989515 0.216311 0.028 Uiso 1 1 calc R U . . .
C38 C 1.38288(14) 0.89654(8) 0.14352(8) 0.0165(2) Uani 1 1 d . . . . .
C39 C 1.27840(14) 0.81525(8) 0.14360(8) 0.0142(2) Uani 1 1 d . . . . .
C40 C 1.17362(15) 0.77741(8) 0.06970(8) 0.0179(2) Uani 1 1 d . . . . .
H40 H 1.103360 0.723163 0.068471 0.022 Uiso 1 1 calc R U . . .
C41 C 1.17185(16) 0.81771(9) -0.00010(8) 0.0223(3) Uani 1 1 d . . . . .
H41 H 1.101460 0.790915 -0.049196 0.027 Uiso 1 1 calc R U . . .
C42 C 1.27431(17) 0.89890(9) 0.00078(9) 0.0228(3) Uani 1 1 d . . . . .
H42 H 1.271949 0.926852 -0.047441 0.027 Uiso 1 1 calc R U . . .
C43 C 1.37660(16) 0.93713(9) 0.07087(9) 0.0203(3) Uani 1 1 d . . . . .
H43 H 1.444736 0.991837 0.071014 0.024 Uiso 1 1 calc R U . . .
C44 C 1.16058(13) 0.64873(8) 0.33997(7) 0.0135(2) Uani 1 1 d . . . . .
C45 C 1.21260(14) 0.57657(8) 0.35444(8) 0.0156(2) Uani 1 1 d . . . . .
H45 H 1.254309 0.545950 0.310006 0.019 Uiso 1 1 calc R U . . .
C46 C 1.20575(15) 0.54679(9) 0.43331(8) 0.0181(2) Uani 1 1 d . . . . .
H46 H 1.244361 0.497650 0.441583 0.022 Uiso 1 1 calc R U . . .
C47 C 1.14353(14) 0.58885(9) 0.49746(8) 0.0178(2) Uani 1 1 d . . . . .
H47 H 1.138076 0.568275 0.550068 0.021 Uiso 1 1 calc R U . . .
C48 C 1.08695(14) 0.66288(8) 0.48646(8) 0.0156(2) Uani 1 1 d . . . . .
C49 C 1.01745(15) 0.70487(9) 0.55148(8) 0.0208(3) Uani 1 1 d . . . . .
H49 H 1.008575 0.683148 0.603385 0.025 Uiso 1 1 calc R U . . .
C50 C 0.96282(16) 0.77619(10) 0.54091(9) 0.0242(3) Uani 1 1 d . . . . .
H50 H 0.914431 0.802961 0.584699 0.029 Uiso 1 1 calc R U . . .
C51 C 0.97860(16) 0.80991(9) 0.46464(9) 0.0227(3) Uani 1 1 d . . . . .
H51 H 0.942779 0.860312 0.457894 0.027 Uiso 1 1 calc R U . . .
C52 C 1.04500(15) 0.77071(8) 0.40027(8) 0.0180(2) Uani 1 1 d . . . . .
H52 H 1.055257 0.794600 0.349587 0.022 Uiso 1 1 calc R U . . .
C53 C 1.09890(13) 0.69477(8) 0.40808(8) 0.0145(2) Uani 1 1 d . . . . .
B1 B 0.59811(15) 0.28921(9) 0.26459(8) 0.0127(2) Uani 1 1 d . . . . .
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'
B B 0.0013 0.0007 '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'
Si Si 0.0817 0.0704 '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 -1 0 0.0370
0 1 0 0.0407
0 1 1 0.0915
0 -1 -1 0.0982
1 1 0 0.0692
-1 -1 0 0.0616
-1 -1 -1 0.0466
0 0 -1 0.1060
1 0 0 0.0633
-1 0 0 0.0510
0 0 1 0.1102
-1 0 -1 0.0561
1 -1 0 0.0475
1 0 -2 0.0826
-2 1 0 0.0499
2 -1 0 0.0340
-1 1 -2 0.0737
-1 1 -1 0.0561
-1 2 -1 0.0577
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
C21 S1 C16 92.47(6) . . ?
C23 S2 C20 92.61(6) . . ?
C26 S3 C30 92.95(6) . . ?
C32 S4 C29 92.79(6) . . ?
C26 Si1 C44 105.66(5) . . ?
C29 Si1 C26 96.15(5) . . ?
C29 Si1 C34 116.48(5) . . ?
C29 Si1 C44 108.17(5) . . ?
C34 Si1 C26 116.70(5) . . ?
C34 Si1 C44 112.12(5) . . ?
C3 C2 C1 109.09(11) . . ?
C3 C2 C4 113.38(10) . . ?
C4 C2 C1 112.29(10) . . ?
C5 C4 C2 121.93(11) . . ?
C9 C4 C2 120.63(11) . . ?
C9 C4 C5 117.39(11) . . ?
C6 C5 C4 122.42(11) . . ?
C5 C6 C7 119.27(10) . . ?
C5 C6 C10 121.35(10) . . ?
C7 C6 C10 119.38(10) . . ?
C6 C7 B1 120.20(10) . . ?
C8 C7 C6 119.01(11) . . ?
C8 C7 B1 120.79(10) . . ?
C7 C8 C13 120.18(11) . . ?
C9 C8 C7 119.86(11) . . ?
C9 C8 C13 119.91(11) . . ?
C4 C9 C8 122.00(11) . . ?
C6 C10 C11 111.73(10) . . ?
C12 C10 C6 114.23(11) . . ?
C12 C10 C11 108.31(10) . . ?
C8 C13 C14 111.28(11) . . ?
C8 C13 C15 112.77(11) . . ?
C15 C13 C14 110.49(11) . . ?
C17 C16 S1 110.24(9) . . ?
C17 C16 B1 123.38(10) . . ?
B1 C16 S1 126.08(9) . . ?
C16 C17 C18 120.08(10) . . ?
C16 C17 C22 113.07(10) . . ?
C22 C17 C18 126.82(11) . . ?
C19 C18 C17 114.26(10) . . ?
C25 C18 C17 121.59(10) . . ?
C25 C18 C19 123.96(10) . . ?
C20 C19 C18 119.02(10) . . ?
C20 C19 C24 112.63(10) . . ?
C24 C19 C18 128.34(11) . . ?
C19 C20 S2 110.54(9) . . ?
C19 C20 B1 124.17(10) . . ?
B1 C20 S2 124.63(9) . . ?
C22 C21 S1 112.17(9) . . ?
C21 C22 C17 111.98(11) . . ?
C24 C23 S2 111.98(9) . . ?
C23 C24 C19 112.19(11) . . ?
C18 C25 C27 122.90(10) . . ?
C18 C25 C28 124.33(10) . . ?
C27 C25 C28 112.76(9) . . ?
S3 C26 Si1 132.48(7) . . ?
C27 C26 S3 110.24(9) . . ?
C27 C26 Si1 117.27(9) . . ?
C26 C27 C25 120.97(10) . . ?
C26 C27 C31 113.39(10) . . ?
C31 C27 C25 125.53(11) . . ?
C29 C28 C25 119.81(10) . . ?
C29 C28 C33 113.35(10) . . ?
C33 C28 C25 126.70(10) . . ?
S4 C29 Si1 131.22(7) . . ?
C28 C29 S4 110.00(9) . . ?
C28 C29 Si1 118.41(9) . . ?
C31 C30 S3 111.59(9) . . ?
C30 C31 C27 111.83(11) . . ?
C33 C32 S4 111.80(9) . . ?
C32 C33 C28 112.06(11) . . ?
C35 C34 Si1 117.90(9) . . ?
C35 C34 C39 118.19(11) . . ?
C39 C34 Si1 123.87(9) . . ?
C34 C35 C36 122.20(12) . . ?
C37 C36 C35 120.06(12) . . ?
C36 C37 C38 120.50(12) . . ?
C37 C38 C39 119.44(11) . . ?
C43 C38 C37 121.33(12) . . ?
C43 C38 C39 119.23(12) . . ?
C38 C39 C34 119.58(11) . . ?
C40 C39 C34 122.26(11) . . ?
C40 C39 C38 118.16(11) . . ?
C41 C40 C39 121.22(12) . . ?
C40 C41 C42 120.28(13) . . ?
C43 C42 C41 120.02(12) . . ?
C42 C43 C38 121.08(12) . . ?
C45 C44 Si1 119.27(9) . . ?
C45 C44 C53 118.24(11) . . ?
C53 C44 Si1 121.73(9) . . ?
C44 C45 C46 122.16(11) . . ?
C47 C46 C45 119.86(12) . . ?
C46 C47 C48 120.76(11) . . ?
C47 C48 C53 119.36(11) . . ?
C49 C48 C47 121.07(11) . . ?
C49 C48 C53 119.57(12) . . ?
C50 C49 C48 121.11(12) . . ?
C49 C50 C51 119.71(12) . . ?
C52 C51 C50 120.69(13) . . ?
C51 C52 C53 121.08(12) . . ?
C48 C53 C44 119.54(11) . . ?
C52 C53 C44 122.66(11) . . ?
C52 C53 C48 117.78(11) . . ?
C16 B1 C7 125.07(11) . . ?
C16 B1 C20 109.65(10) . . ?
C20 B1 C7 125.23(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C16 1.7232(12) . ?
S1 C21 1.7151(13) . ?
S2 C20 1.7203(12) . ?
S2 C23 1.7132(13) . ?
S3 C26 1.7150(12) . ?
S3 C30 1.7176(14) . ?
S4 C29 1.7193(12) . ?
S4 C32 1.7143(13) . ?
Si1 C26 1.8709(12) . ?
Si1 C29 1.8615(12) . ?
Si1 C34 1.8648(12) . ?
Si1 C44 1.8763(12) . ?
C1 C2 1.5367(19) . ?
C2 C3 1.5239(18) . ?
C2 C4 1.5258(16) . ?
C4 C5 1.3977(17) . ?
C4 C9 1.3963(17) . ?
C5 C6 1.3961(16) . ?
C6 C7 1.4152(16) . ?
C6 C10 1.5286(16) . ?
C7 C8 1.4072(16) . ?
C7 B1 1.5704(17) . ?
C8 C9 1.3970(16) . ?
C8 C13 1.5216(16) . ?
C10 C11 1.5355(18) . ?
C10 C12 1.5285(18) . ?
C13 C14 1.5351(19) . ?
C13 C15 1.5313(19) . ?
C16 C17 1.3910(16) . ?
C16 B1 1.5374(18) . ?
C17 C18 1.4826(16) . ?
C17 C22 1.4262(16) . ?
C18 C19 1.4806(16) . ?
C18 C25 1.3607(16) . ?
C19 C20 1.3927(16) . ?
C19 C24 1.4290(16) . ?
C20 B1 1.5396(17) . ?
C21 C22 1.3668(17) . ?
C23 C24 1.3702(17) . ?
C25 C27 1.4892(16) . ?
C25 C28 1.4913(16) . ?
C26 C27 1.3807(16) . ?
C27 C31 1.4319(16) . ?
C28 C29 1.3836(16) . ?
C28 C33 1.4263(16) . ?
C30 C31 1.3681(17) . ?
C32 C33 1.3621(17) . ?
C34 C35 1.3816(17) . ?
C34 C39 1.4360(16) . ?
C35 C36 1.4117(18) . ?
C36 C37 1.366(2) . ?
C37 C38 1.4185(18) . ?
C38 C39 1.4258(17) . ?
C38 C43 1.4185(18) . ?
C39 C40 1.4182(17) . ?
C40 C41 1.3725(18) . ?
C41 C42 1.4134(19) . ?
C42 C43 1.364(2) . ?
C44 C45 1.3822(17) . ?
C44 C53 1.4377(17) . ?
C45 C46 1.4160(17) . ?
C46 C47 1.3655(18) . ?
C47 C48 1.4181(18) . ?
C48 C49 1.4138(18) . ?
C48 C53 1.4268(17) . ?
C49 C50 1.367(2) . ?
C50 C51 1.412(2) . ?
C51 C52 1.3694(19) . ?
C52 C53 1.4232(17) . ?
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
-0.0000 -1.0000 0.0002 -0.0020 -0.0462 0.0015
0.0000 1.0000 -0.0002 0.0020 0.0462 -0.0015
0.0001 0.9999 0.9991 -0.0168 0.0537 -0.0418
-0.0001 -0.9999 -0.9991 0.0168 -0.0537 0.0418
0.9997 1.0006 -0.0001 -0.0705 0.0696 0.0261
-0.9997 -1.0006 0.0001 0.0705 -0.0696 -0.0261
-0.9998 -1.0005 -0.9992 0.0893 -0.0771 0.0142
-0.0001 0.0001 -0.9994 0.0188 -0.0075 0.0404
0.9997 0.0006 0.0001 -0.0725 0.0234 0.0276
-0.9997 -0.0006 -0.0001 0.0725 -0.0234 -0.0276
0.0001 -0.0001 0.9994 -0.0188 0.0075 -0.0404
-0.9998 -0.0005 -0.9995 0.0913 -0.0309 0.0128
0.9997 -0.9994 0.0004 -0.0745 -0.0228 0.0291
0.9995 0.0007 -1.9986 -0.0349 0.0084 0.1084
-1.9993 0.9989 -0.0005 0.1470 -0.0006 -0.0567
1.9993 -0.9989 0.0005 -0.1470 0.0006 0.0567
-0.9998 0.9996 -1.9991 0.1121 0.0078 0.0517
-0.9998 0.9995 -0.9997 0.0933 0.0153 0.0113
-0.9997 1.9995 -1.0000 0.0954 0.0615 0.0098
