# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_1905
_database_code_depnum_ccdc_archive 'CCDC 2381482'
loop_
_audit_author_name
_audit_author_address
'Kohei Yamada'
;University
Japan
;
_audit_update_record             
;
2024-09-03 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_audit_creation_date             2023-01-19
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H37 B S4 Si'
_chemical_formula_sum            'C35 H37 B S4 Si'
_chemical_formula_weight         624.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         C35H37B1S4Si1
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8040(2)
_cell_length_b                   21.4141(4)
_cell_length_c                   11.1906(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.056(2)
_cell_angle_gamma                90
_cell_volume                     3289.48(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26551
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.8400
_cell_measurement_theta_min      2.4000
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.943
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99142
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -2 1 0.0432
0 2 -1 0.0265
2 -1 1 0.0819
-2 1 -1 0.0752
0 -1 0 0.0596
0 1 0 0.0411
1 0 0 0.0828
-1 0 0 0.0697
1 -2 -2 0.0404
-1 2 2 0.0797
11 19 7 0.0800
-13 -13 10 0.0586
12 11 -12 0.0621
2 3 15 0.0704
-14 9 11 0.0726
0 1 16 0.0574
11 1 12 0.0799
12 24 -2 0.0696

_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.07
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
-0.0001 -1.9986 0.9995 0.0865 0.0255 -0.0177
0.0001 1.9986 -0.9995 -0.0865 -0.0255 0.0177
1.9989 -1.0001 0.9996 0.0760 0.0704 0.0806
-1.9989 1.0001 -0.9996 -0.0760 -0.0704 -0.0806
0.0000 -0.9994 -0.0000 0.0148 0.0221 -0.0197
-0.0000 0.9994 0.0000 -0.0148 -0.0221 0.0197
0.9995 -0.0004 0.0000 0.0021 0.0335 0.0393
-0.9995 0.0004 -0.0000 -0.0021 -0.0335 -0.0393
1.0001 -1.9995 -1.9991 -0.0821 0.1152 -0.0434
-1.0001 1.9995 1.9991 0.0821 -0.1152 0.0434
11.4029 19.0185 7.0221 0.1430 -0.1708 0.9749
-13.4394 -13.0033 10.2596 0.7477 -0.3541 -0.5617
12.1764 11.0434 -11.8468 -0.8118 0.3850 0.4391
1.6379 2.8688 15.4215 0.8392 -0.2974 0.4553
-13.6647 9.2446 11.2544 0.4749 -0.8730 -0.1111
-0.1444 0.5746 15.6973 0.8850 -0.3114 0.3461
11.1179 0.8495 11.9162 0.6898 0.1304 0.7122
12.1247 23.5645 -1.8214 -0.4262 -0.0818 0.9009

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39668
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.656
_diffrn_reflns_theta_min         2.412
_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 0.999
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  30.00   0.50    1.00    --   -7.02 -99.00  30.00   82
  2  ω    -26.00  64.00   0.50    1.00    --   -7.02  38.00   0.00  180
  3  ω    -75.00 -49.00   0.50    1.00    --   -7.02 -57.00-150.00   52
  4  ω    -42.00  12.00   0.50    1.00    --   -7.02 -57.00-150.00  108
  5  ω     -6.00  21.00   0.50    1.00    --   -7.02 -99.00-180.00   54
  6  ω    -66.00  31.00   0.50    1.00    --    8.27 -57.00-180.00  194
  7  ω     -3.00  24.00   0.50    1.00    --    8.27 -99.00 -30.00   54
  8  ω     -5.00  58.00   0.50    1.00    --    8.27  57.00 120.00  126
;
_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      0.0021421000
_diffrn_orient_matrix_UB_12      -0.0147873000
_diffrn_orient_matrix_UB_13      0.0569413000
_diffrn_orient_matrix_UB_21      0.0334864000
_diffrn_orient_matrix_UB_22      -0.0221469000
_diffrn_orient_matrix_UB_23      -0.0187208000
_diffrn_orient_matrix_UB_31      0.0393097000
_diffrn_orient_matrix_UB_32      0.0196826000
_diffrn_orient_matrix_UB_33      0.0216866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6733
_reflns_number_total             7853
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_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     378
_refine_ls_number_reflns         7853
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.046
_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)+(0.0348P)²+1.3859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0778
_refine_special_details          ?
_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)
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), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.34555(2) 0.76252(2) 0.81943(3) 0.01494(8) Uani 1 1 d . . . . .
S2 S 0.43807(2) 0.51667(2) 0.70208(3) 0.01938(8) Uani 1 1 d . . . . .
S3 S 0.74265(2) 0.87387(2) 0.56795(3) 0.01975(8) Uani 1 1 d . . . . .
S4 S 0.86297(2) 0.61986(2) 0.48622(3) 0.01535(8) Uani 1 1 d . . . . .
Si1 Si 0.84372(3) 0.74164(2) 0.65678(3) 0.01540(9) Uani 1 1 d . . . . .
C1 C -0.08735(10) 0.54429(7) 0.81077(14) 0.0242(3) Uani 1 1 d . . . . .
H1A H -0.146015 0.518540 0.811099 0.036 Uiso 1 1 calc R U . . .
H1B H -0.104336 0.584108 0.770759 0.036 Uiso 1 1 calc R U . . .
H1C H -0.059648 0.552165 0.893663 0.036 Uiso 1 1 calc R U . . .
C2 C -0.01259(9) 0.51006(6) 0.74337(12) 0.0159(3) Uani 1 1 d . . . . .
H2 H -0.042183 0.504063 0.658673 0.019 Uiso 1 1 calc R U . . .
C3 C 0.00864(10) 0.44519(7) 0.79738(14) 0.0219(3) Uani 1 1 d . . . . .
H3A H 0.036518 0.449434 0.881218 0.033 Uiso 1 1 calc R U . . .
H3B H 0.055031 0.423419 0.751503 0.033 Uiso 1 1 calc R U . . .
H3C H -0.052038 0.421193 0.793993 0.033 Uiso 1 1 calc R U . . .
C4 C 0.08032(9) 0.54770(6) 0.73907(12) 0.0140(3) Uani 1 1 d . . . . .
C5 C 0.14251(9) 0.56030(6) 0.84240(12) 0.0169(3) Uani 1 1 d . . . . .
H5 H 0.125003 0.546538 0.917922 0.020 Uiso 1 1 calc R U . . .
C6 C 0.22982(9) 0.59258(6) 0.83807(12) 0.0156(3) Uani 1 1 d . . . . .
C7 C 0.25616(9) 0.61384(6) 0.72675(12) 0.0126(2) Uani 1 1 d . . . . .
C8 C 0.19210(9) 0.60362(6) 0.62246(12) 0.0131(2) Uani 1 1 d . . . . .
C9 C 0.10593(9) 0.57037(6) 0.63017(12) 0.0142(3) Uani 1 1 d . . . . .
H9 H 0.063573 0.563022 0.559006 0.017 Uiso 1 1 calc R U . . .
C10 C 0.29658(10) 0.60395(7) 0.95288(13) 0.0221(3) Uani 1 1 d . . . . .
H10 H 0.353661 0.628406 0.930435 0.026 Uiso 1 1 calc R U . . .
C11 C 0.33618(12) 0.54286(8) 1.00935(15) 0.0324(4) Uani 1 1 d . . . . .
H11A H 0.282500 0.518630 1.036772 0.049 Uiso 1 1 calc R U . . .
H11B H 0.384207 0.552121 1.077917 0.049 Uiso 1 1 calc R U . . .
H11C H 0.367214 0.518656 0.949548 0.049 Uiso 1 1 calc R U . . .
C12 C 0.24733(14) 0.64317(9) 1.04271(15) 0.0367(4) Uani 1 1 d . . . . .
H12A H 0.223932 0.682314 1.004537 0.055 Uiso 1 1 calc R U . . .
H12B H 0.294242 0.652440 1.112402 0.055 Uiso 1 1 calc R U . . .
H12C H 0.192153 0.619973 1.068961 0.055 Uiso 1 1 calc R U . . .
C13 C 0.21699(9) 0.62750(6) 0.50119(12) 0.0150(3) Uani 1 1 d . . . . .
H13 H 0.276057 0.654552 0.516418 0.018 Uiso 1 1 calc R U . . .
C14 C 0.13531(10) 0.66784(7) 0.43841(13) 0.0225(3) Uani 1 1 d . . . . .
H14A H 0.075555 0.642996 0.424535 0.034 Uiso 1 1 calc R U . . .
H14B H 0.154263 0.682545 0.361280 0.034 Uiso 1 1 calc R U . . .
H14C H 0.123818 0.703788 0.489242 0.034 Uiso 1 1 calc R U . . .
C15 C 0.24283(10) 0.57393(7) 0.42041(13) 0.0219(3) Uani 1 1 d . . . . .
H15A H 0.299373 0.551344 0.459243 0.033 Uiso 1 1 calc R U . . .
H15B H 0.258378 0.590694 0.343219 0.033 Uiso 1 1 calc R U . . .
H15C H 0.187318 0.545335 0.406904 0.033 Uiso 1 1 calc R U . . .
C16 C 0.40088(9) 0.70664(6) 0.73933(11) 0.0121(2) Uani 1 1 d . . . . .
C17 C 0.49437(9) 0.72546(6) 0.71896(11) 0.0120(2) Uani 1 1 d . . . . .
C18 C 0.55957(8) 0.68285(6) 0.65926(11) 0.0116(2) Uani 1 1 d . . . . .
C19 C 0.53843(9) 0.61561(6) 0.67327(12) 0.0129(2) Uani 1 1 d . . . . .
C20 C 0.44419(9) 0.59676(6) 0.68884(12) 0.0143(3) Uani 1 1 d . . . . .
C21 C 0.44600(9) 0.80969(6) 0.82856(12) 0.0160(3) Uani 1 1 d . . . . .
H21 H 0.450247 0.848694 0.869221 0.019 Uiso 1 1 calc R U . . .
C22 C 0.51936(9) 0.78496(6) 0.77081(12) 0.0144(3) Uani 1 1 d . . . . .
H22 H 0.580141 0.805062 0.765697 0.017 Uiso 1 1 calc R U . . .
C23 C 0.56004(10) 0.50853(6) 0.69175(13) 0.0195(3) Uani 1 1 d . . . . .
H23 H 0.592982 0.469514 0.695819 0.023 Uiso 1 1 calc R U . . .
C24 C 0.60470(9) 0.56430(6) 0.67703(12) 0.0161(3) Uani 1 1 d . . . . .
H24 H 0.672374 0.568571 0.670048 0.019 Uiso 1 1 calc R U . . .
C25 C 0.63056(9) 0.70402(6) 0.59386(12) 0.0127(2) Uani 1 1 d . . . . .
C26 C 0.64977(9) 0.77146(6) 0.57466(12) 0.0141(3) Uani 1 1 d . . . . .
C27 C 0.74213(9) 0.79569(6) 0.60279(12) 0.0152(3) Uani 1 1 d . . . . .
C28 C 0.70079(9) 0.66272(6) 0.53858(11) 0.0125(2) Uani 1 1 d . . . . .
C29 C 0.79965(9) 0.67285(6) 0.56337(12) 0.0136(2) Uani 1 1 d . . . . .
C30 C 0.58106(10) 0.81598(6) 0.52265(13) 0.0175(3) Uani 1 1 d . . . . .
H30 H 0.514704 0.806654 0.497794 0.021 Uiso 1 1 calc R U . . .
C31 C 0.62166(10) 0.87341(6) 0.51275(14) 0.0214(3) Uani 1 1 d . . . . .
H31 H 0.587355 0.908869 0.479445 0.026 Uiso 1 1 calc R U . . .
C32 C 0.67781(9) 0.61335(6) 0.45486(12) 0.0142(3) Uani 1 1 d . . . . .
H32 H 0.613185 0.600928 0.427528 0.017 Uiso 1 1 calc R U . . .
C33 C 0.75869(9) 0.58599(6) 0.41845(12) 0.0154(3) Uani 1 1 d . . . . .
H33 H 0.757549 0.552465 0.362710 0.019 Uiso 1 1 calc R U . . .
C34 C 0.96728(10) 0.76898(7) 0.63083(16) 0.0264(3) Uani 1 1 d . . . . .
H34A H 0.968354 0.779546 0.545777 0.040 Uiso 1 1 calc R U . . .
H34B H 1.014742 0.735808 0.652849 0.040 Uiso 1 1 calc R U . . .
H34C H 0.984022 0.806018 0.680163 0.040 Uiso 1 1 calc R U . . .
C35 C 0.83707(14) 0.72293(8) 0.81741(14) 0.0320(4) Uani 1 1 d . . . . .
H35A H 0.846656 0.761138 0.865406 0.048 Uiso 1 1 calc R U . . .
H35B H 0.887981 0.692644 0.844283 0.048 Uiso 1 1 calc R U . . .
H35C H 0.773042 0.705111 0.827490 0.048 Uiso 1 1 calc R U . . .
B1 B 0.36131(10) 0.64051(7) 0.71502(13) 0.0130(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.7213(13) . ?
S1 C21 1.7098(13) . ?
S2 C20 1.7241(13) . ?
S2 C23 1.7087(14) . ?
S3 C27 1.7190(13) . ?
S3 C31 1.7185(15) . ?
S4 C29 1.7193(13) . ?
S4 C33 1.7156(13) . ?
Si1 C27 1.8688(14) . ?
Si1 C29 1.8705(13) . ?
Si1 C34 1.8549(15) . ?
Si1 C35 1.8534(16) . ?
C1 C2 1.5282(19) . ?
C2 C3 1.5308(19) . ?
C2 C4 1.5198(17) . ?
C4 C5 1.3920(18) . ?
C4 C9 1.3917(18) . ?
C5 C6 1.3947(18) . ?
C6 C7 1.4096(18) . ?
C6 C10 1.5197(19) . ?
C7 C8 1.4050(18) . ?
C7 B1 1.5781(18) . ?
C8 C9 1.3969(17) . ?
C8 C13 1.5230(18) . ?
C10 C11 1.529(2) . ?
C10 C12 1.524(2) . ?
C13 C14 1.5310(18) . ?
C13 C15 1.5259(19) . ?
C16 C17 1.3936(17) . ?
C16 B1 1.5317(19) . ?
C17 C18 1.4886(17) . ?
C17 C22 1.4273(17) . ?
C18 C19 1.4807(17) . ?
C18 C25 1.3611(18) . ?
C19 C20 1.3905(17) . ?
C19 C24 1.4276(17) . ?
C20 B1 1.5309(19) . ?
C21 C22 1.3644(18) . ?
C23 C24 1.3619(19) . ?
C25 C26 1.4881(17) . ?
C25 C28 1.4937(17) . ?
C26 C27 1.3818(18) . ?
C26 C30 1.4250(18) . ?
C28 C29 1.3808(17) . ?
C28 C32 1.4260(18) . ?
C30 C31 1.3609(19) . ?
C32 C33 1.3608(18) . ?

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 92.31(6) . . ?
C23 S2 C20 92.18(6) . . ?
C31 S3 C27 92.80(7) . . ?
C33 S4 C29 93.08(6) . . ?
C27 Si1 C29 96.80(6) . . ?
C34 Si1 C27 115.15(7) . . ?
C34 Si1 C29 114.28(6) . . ?
C35 Si1 C27 109.59(7) . . ?
C35 Si1 C29 108.98(7) . . ?
C35 Si1 C34 111.13(8) . . ?
C1 C2 C3 110.58(11) . . ?
C4 C2 C1 112.17(11) . . ?
C4 C2 C3 111.51(11) . . ?
C5 C4 C2 121.67(12) . . ?
C9 C4 C2 120.39(12) . . ?
C9 C4 C5 117.94(12) . . ?
C4 C5 C6 121.78(12) . . ?
C5 C6 C7 119.69(12) . . ?
C5 C6 C10 119.95(12) . . ?
C7 C6 C10 120.36(11) . . ?
C6 C7 B1 121.05(11) . . ?
C8 C7 C6 119.04(11) . . ?
C8 C7 B1 119.41(11) . . ?
C7 C8 C13 120.43(11) . . ?
C9 C8 C7 119.57(12) . . ?
C9 C8 C13 119.99(11) . . ?
C4 C9 C8 121.91(12) . . ?
C6 C10 C11 111.77(12) . . ?
C6 C10 C12 111.90(13) . . ?
C12 C10 C11 111.34(13) . . ?
C8 C13 C14 111.95(10) . . ?
C8 C13 C15 111.36(11) . . ?
C15 C13 C14 111.05(12) . . ?
C17 C16 S1 110.70(9) . . ?
C17 C16 B1 123.87(11) . . ?
B1 C16 S1 124.45(9) . . ?
C16 C17 C18 120.69(11) . . ?
C16 C17 C22 112.33(11) . . ?
C22 C17 C18 126.73(11) . . ?
C19 C18 C17 114.41(11) . . ?
C25 C18 C17 122.74(11) . . ?
C25 C18 C19 122.81(11) . . ?
C20 C19 C18 119.54(11) . . ?
C20 C19 C24 112.20(11) . . ?
C24 C19 C18 128.23(11) . . ?
C19 C20 S2 110.77(9) . . ?
C19 C20 B1 125.04(11) . . ?
B1 C20 S2 123.23(10) . . ?
C22 C21 S1 112.35(10) . . ?
C21 C22 C17 112.29(11) . . ?
C24 C23 S2 112.37(10) . . ?
C23 C24 C19 112.44(12) . . ?
C18 C25 C26 123.38(11) . . ?
C18 C25 C28 124.13(11) . . ?
C26 C25 C28 112.43(10) . . ?
C27 C26 C25 120.38(11) . . ?
C27 C26 C30 113.59(12) . . ?
C30 C26 C25 125.95(12) . . ?
S3 C27 Si1 130.96(8) . . ?
C26 C27 S3 109.86(10) . . ?
C26 C27 Si1 118.94(10) . . ?
C29 C28 C25 119.65(11) . . ?
C29 C28 C32 113.27(11) . . ?
C32 C28 C25 127.01(11) . . ?
S4 C29 Si1 130.38(7) . . ?
C28 C29 S4 109.85(10) . . ?
C28 C29 Si1 119.49(9) . . ?
C31 C30 C26 112.07(12) . . ?
C30 C31 S3 111.64(11) . . ?
C33 C32 C28 112.54(11) . . ?
C32 C33 S4 111.24(10) . . ?
C16 B1 C7 129.32(12) . . ?
C20 B1 C7 120.45(11) . . ?
C20 B1 C16 109.89(11) . . ?

_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 1.107
_oxdiff_exptl_absorpt_empirical_full_min 0.939
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_1911
_database_code_depnum_ccdc_archive 'CCDC 2381483'
loop_
_audit_author_name
_audit_author_address
'Kohei Yamada'
;University
Japan
;
_audit_update_record             
;
2024-09-03 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_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)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H41 B S4 Si'
_chemical_formula_sum            'C45 H41 B S4 Si'
_chemical_formula_weight         748.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         C45H41B1S2Si1
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   8.9658(2)
_cell_length_b                   24.7394(5)
_cell_length_c                   17.7919(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.333(2)
_cell_angle_gamma                90
_cell_volume                     3904.73(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24006
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4970
_cell_measurement_theta_min      2.4310
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.939
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98858
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.1053
1 0 0 0.1160
-1 0 0 0.0917
0 1 -1 0.0334
0 -1 1 0.0408
0 1 0 0.0612
0 -1 0 0.0260
1 -1 -2 0.0866
0 1 2 0.0519
-1 -1 2 0.0733
2 1 -1 0.1069
-1 1 0 0.0937
-1 2 0 0.0853
2 2 -1 0.1004
1 2 0 0.0934
0 2 1 0.0574
5 -20 -19 0.0630

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.074
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
0.9993 0.9995 0.0001 -0.0335 0.0104 0.0773
0.9993 0.0003 0.0002 -0.0105 -0.0066 0.0789
-0.9993 -0.0003 -0.0002 0.0105 0.0066 -0.0789
-0.0000 0.9993 -0.9993 0.0009 0.0494 -0.0016
0.0000 -0.9993 0.9993 -0.0009 -0.0494 0.0016
0.0000 0.9992 -0.0002 -0.0230 0.0170 -0.0016
-0.0000 -0.9992 0.0002 0.0230 -0.0170 0.0016
0.9991 -0.9988 -1.9979 0.0602 0.0412 0.0805
0.0001 0.9990 1.9981 -0.0707 -0.0479 -0.0016
-0.9992 -0.9997 1.9982 -0.0142 -0.0752 -0.0773
1.9985 0.9999 -0.9989 -0.0202 0.0361 0.1562
-0.9992 0.9989 -0.0004 -0.0125 0.0236 -0.0806
-0.9992 1.9982 -0.0006 -0.0355 0.0406 -0.0822
1.9985 1.9991 -0.9990 -0.0432 0.0531 0.1546
0.9993 1.9987 -0.0001 -0.0565 0.0273 0.0757
0.0001 1.9983 0.9988 -0.0699 0.0016 -0.0032
5.4535 -19.5092 -19.1578 0.8495 0.2538 0.4625

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46377
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.809
_diffrn_reflns_theta_min         2.314
_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 0.838
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      4.00  43.00   0.50    0.50    --    8.40 -99.00  30.00   78
  2  ω    -17.00  23.00   0.50    0.50    --   -6.92 -99.00-180.00   80
  3  ω    -75.00  16.00   0.50    0.50    --   -6.92 -57.00-150.00  182
  4  ω    -83.00  43.00   0.50    0.50    --   -6.92   0.00-150.00  252
  5  ω     -3.00  31.00   0.50    0.50    --   -6.92  19.00-180.00   68
  6  ω    -29.00  57.00   0.50    0.50    --   -6.92  57.00  30.00  172
;
_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      -0.0105176000
_diffrn_orient_matrix_UB_12      -0.0230224000
_diffrn_orient_matrix_UB_13      -0.0238931000
_diffrn_orient_matrix_UB_21      -0.0066346000
_diffrn_orient_matrix_UB_22      0.0169958000
_diffrn_orient_matrix_UB_23      -0.0324448000
_diffrn_orient_matrix_UB_31      0.0790045000
_diffrn_orient_matrix_UB_32      -0.0016315000
_diffrn_orient_matrix_UB_33      0.0000112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7543
_reflns_number_total             9394
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         9394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      1.057
_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)+(0.0378P)²+1.5848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0961
_refine_special_details          ?
_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), C11(H11), 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), C38(H38), C39(H39), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.76422(5) 0.50615(2) 0.29455(2) 0.02132(10) Uani 1 1 d . . . . .
S2 S 0.26350(5) 0.36547(2) 0.27023(3) 0.02441(11) Uani 1 1 d . . . . .
S3 S 1.18320(4) 0.31748(2) 0.53604(2) 0.02018(10) Uani 1 1 d . . . . .
S4 S 0.65546(5) 0.18934(2) 0.52474(3) 0.02076(10) Uani 1 1 d . . . . .
Si1 Si 0.96206(5) 0.22495(2) 0.46096(3) 0.01435(10) Uani 1 1 d . . . . .
C1 C -0.0848(2) 0.59646(12) 0.14467(16) 0.0630(9) Uani 1 1 d . . . . .
H1A H -0.133362 0.570353 0.174758 0.095 Uiso 1 1 calc R U . . .
H1B H -0.049558 0.577849 0.101911 0.095 Uiso 1 1 calc R U . . .
H1C H -0.157530 0.624524 0.125331 0.095 Uiso 1 1 calc R U . . .
C2 C 0.0503(2) 0.62262(9) 0.19500(14) 0.0431(6) Uani 1 1 d . . . . .
H2 H 0.099422 0.647784 0.162044 0.052 Uiso 1 1 calc R U . . .
C3 C -0.0036(3) 0.65644(11) 0.25706(17) 0.0650(9) Uani 1 1 d . . . . .
H3A H -0.078715 0.682631 0.234122 0.097 Uiso 1 1 calc R U . . .
H3B H 0.082180 0.675712 0.285397 0.097 Uiso 1 1 calc R U . . .
H3C H -0.048998 0.632801 0.291700 0.097 Uiso 1 1 calc R U . . .
C4 C 0.16703(19) 0.57982(7) 0.22473(11) 0.0255(4) Uani 1 1 d . . . . .
C5 C 0.22730(19) 0.54691(7) 0.17350(11) 0.0242(4) Uani 1 1 d . . . . .
H5 H 0.197425 0.552618 0.120657 0.029 Uiso 1 1 calc R U . . .
C6 C 0.33001(19) 0.50580(7) 0.19676(10) 0.0215(4) Uani 1 1 d . . . . .
C7 C 0.37797(18) 0.49745(6) 0.27496(10) 0.0174(3) Uani 1 1 d . . . . .
C8 C 0.32282(18) 0.53184(6) 0.32736(10) 0.0178(3) Uani 1 1 d . . . . .
C9 C 0.21661(19) 0.57182(7) 0.30157(11) 0.0231(4) Uani 1 1 d . . . . .
H9 H 0.177516 0.594029 0.337667 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4170(2) 0.57861(7) 0.45149(11) 0.0249(4) Uani 1 1 d . . . . .
H10A H 0.496772 0.596143 0.428027 0.037 Uiso 1 1 calc R U . . .
H10B H 0.452949 0.572080 0.505409 0.037 Uiso 1 1 calc R U . . .
H10C H 0.328122 0.602096 0.446545 0.037 Uiso 1 1 calc R U . . .
C11 C 0.37524(19) 0.52480(7) 0.41173(10) 0.0198(4) Uani 1 1 d . . . . .
H11 H 0.469049 0.502409 0.417014 0.024 Uiso 1 1 calc R U . . .
C12 C 0.2588(2) 0.49313(7) 0.44926(10) 0.0242(4) Uani 1 1 d . . . . .
H12A H 0.160254 0.510781 0.437925 0.036 Uiso 1 1 calc R U . . .
H12B H 0.289974 0.492275 0.504363 0.036 Uiso 1 1 calc R U . . .
H12C H 0.251784 0.456113 0.429467 0.036 Uiso 1 1 calc R U . . .
C13 C 0.3971(2) 0.47242(8) 0.13803(10) 0.0301(4) Uani 1 1 d . . . . .
H13 H 0.451409 0.441224 0.165335 0.036 Uiso 1 1 calc R U . . .
C14 C 0.5132(2) 0.50533(8) 0.10282(11) 0.0328(5) Uani 1 1 d . . . . .
H14A H 0.462721 0.535299 0.073379 0.049 Uiso 1 1 calc R U . . .
H14B H 0.562749 0.482094 0.069284 0.049 Uiso 1 1 calc R U . . .
H14C H 0.588765 0.519728 0.143183 0.049 Uiso 1 1 calc R U . . .
C15 C 0.2782(3) 0.44913(9) 0.07618(13) 0.0484(6) Uani 1 1 d . . . . .
H15A H 0.202183 0.429522 0.099817 0.073 Uiso 1 1 calc R U . . .
H15B H 0.326594 0.424316 0.044172 0.073 Uiso 1 1 calc R U . . .
H15C H 0.229805 0.478615 0.044905 0.073 Uiso 1 1 calc R U . . .
C16 C 0.65937(18) 0.45309(6) 0.32180(9) 0.0164(3) Uani 1 1 d . . . . .
C17 C 0.75359(17) 0.40992(6) 0.34767(9) 0.0147(3) Uani 1 1 d . . . . .
C18 C 0.68810(17) 0.35998(6) 0.37513(9) 0.0138(3) Uani 1 1 d . . . . .
C19 C 0.53155(17) 0.34862(7) 0.33883(9) 0.0158(3) Uani 1 1 d . . . . .
C20 C 0.43572(17) 0.39089(7) 0.31096(9) 0.0171(3) Uani 1 1 d . . . . .
C21 C 0.92864(19) 0.47059(7) 0.31292(10) 0.0222(4) Uani 1 1 d . . . . .
H21 H 1.023798 0.484239 0.304392 0.027 Uiso 1 1 calc R U . . .
C22 C 0.90787(18) 0.42048(7) 0.34119(9) 0.0187(3) Uani 1 1 d . . . . .
H22 H 0.987126 0.395313 0.355056 0.022 Uiso 1 1 calc R U . . .
C23 C 0.3210(2) 0.30010(7) 0.28691(11) 0.0256(4) Uani 1 1 d . . . . .
H23 H 0.259658 0.269514 0.272136 0.031 Uiso 1 1 calc R U . . .
C24 C 0.46448(18) 0.29690(7) 0.32367(10) 0.0202(4) Uani 1 1 d . . . . .
H24 H 0.514527 0.263781 0.337719 0.024 Uiso 1 1 calc R U . . .
C25 C 0.76119(17) 0.32859(6) 0.43169(9) 0.0142(3) Uani 1 1 d . . . . .
C26 C 0.69018(17) 0.28160(6) 0.46524(9) 0.0146(3) Uani 1 1 d . . . . .
C27 C 0.76489(17) 0.23315(6) 0.48161(9) 0.0161(3) Uani 1 1 d . . . . .
C28 C 0.91859(17) 0.33853(6) 0.46999(9) 0.0145(3) Uani 1 1 d . . . . .
C29 C 1.01876(17) 0.29616(7) 0.48274(9) 0.0152(3) Uani 1 1 d . . . . .
C30 C 0.97674(18) 0.38785(7) 0.50325(9) 0.0173(3) Uani 1 1 d . . . . .
H30 H 0.922610 0.420982 0.499226 0.021 Uiso 1 1 calc R U . . .
C31 C 1.11857(19) 0.38223(7) 0.54147(10) 0.0207(4) Uani 1 1 d . . . . .
H31 H 1.174788 0.410701 0.567888 0.025 Uiso 1 1 calc R U . . .
C32 C 0.54489(18) 0.28248(7) 0.48956(10) 0.0180(3) Uani 1 1 d . . . . .
H32 H 0.478758 0.312669 0.483234 0.022 Uiso 1 1 calc R U . . .
C33 C 0.51218(18) 0.23542(7) 0.52265(10) 0.0199(4) Uani 1 1 d . . . . .
H33 H 0.420856 0.228783 0.542295 0.024 Uiso 1 1 calc R U . . .
C34 C 0.96337(17) 0.20898(7) 0.35848(9) 0.0159(3) Uani 1 1 d . . . . .
C35 C 0.95381(19) 0.25049(7) 0.30453(10) 0.0212(4) Uani 1 1 d . . . . .
H35 H 0.947524 0.286931 0.320595 0.025 Uiso 1 1 calc R U . . .
C36 C 0.9533(2) 0.23944(8) 0.22812(10) 0.0254(4) Uani 1 1 d . . . . .
H36 H 0.944552 0.268118 0.192248 0.031 Uiso 1 1 calc R U . . .
C37 C 0.96571(19) 0.18653(8) 0.20404(10) 0.0245(4) Uani 1 1 d . . . . .
H37 H 0.969596 0.179012 0.151996 0.029 Uiso 1 1 calc R U . . .
C38 C 0.97237(19) 0.14477(7) 0.25604(10) 0.0240(4) Uani 1 1 d . . . . .
H38 H 0.978733 0.108426 0.239582 0.029 Uiso 1 1 calc R U . . .
C39 C 0.96978(18) 0.15589(7) 0.33211(10) 0.0199(4) Uani 1 1 d . . . . .
H39 H 0.972415 0.126824 0.367166 0.024 Uiso 1 1 calc R U . . .
C40 C 1.08196(18) 0.17797(7) 0.52578(10) 0.0182(3) Uani 1 1 d . . . . .
C41 C 1.19460(18) 0.14604(7) 0.50119(10) 0.0203(4) Uani 1 1 d . . . . .
H41 H 1.205138 0.145670 0.448822 0.024 Uiso 1 1 calc R U . . .
C42 C 1.2914(2) 0.11486(7) 0.55199(11) 0.0264(4) Uani 1 1 d . . . . .
H42 H 1.366156 0.093114 0.534103 0.032 Uiso 1 1 calc R U . . .
C43 C 1.2786(2) 0.11556(8) 0.62863(11) 0.0313(4) Uani 1 1 d . . . . .
H43 H 1.344483 0.094338 0.663446 0.038 Uiso 1 1 calc R U . . .
C44 C 1.1697(2) 0.14719(9) 0.65411(11) 0.0332(5) Uani 1 1 d . . . . .
H44 H 1.161633 0.148019 0.706758 0.040 Uiso 1 1 calc R U . . .
C45 C 1.0717(2) 0.17784(8) 0.60364(10) 0.0269(4) Uani 1 1 d . . . . .
H45 H 0.996513 0.199053 0.622125 0.032 Uiso 1 1 calc R U . . .
B1 B 0.4873(2) 0.44946(8) 0.30416(10) 0.0166(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.7246(16) . ?
S1 C21 1.7070(18) . ?
S2 C20 1.7264(16) . ?
S2 C23 1.7103(19) . ?
S3 C29 1.7164(16) . ?
S3 C31 1.7110(18) . ?
S4 C27 1.7160(16) . ?
S4 C33 1.7139(17) . ?
Si1 C27 1.8680(16) . ?
Si1 C29 1.8586(17) . ?
Si1 C34 1.8675(17) . ?
Si1 C40 1.8647(17) . ?
C1 C2 1.541(4) . ?
C2 C3 1.519(4) . ?
C2 C4 1.528(3) . ?
C4 C5 1.389(3) . ?
C4 C9 1.389(3) . ?
C5 C6 1.394(2) . ?
C6 C7 1.411(2) . ?
C6 C13 1.523(3) . ?
C7 C8 1.404(2) . ?
C7 B1 1.579(2) . ?
C8 C9 1.403(2) . ?
C8 C11 1.517(2) . ?
C10 C11 1.528(2) . ?
C11 C12 1.533(2) . ?
C13 C14 1.526(3) . ?
C13 C15 1.529(3) . ?
C16 C17 1.398(2) . ?
C16 B1 1.532(2) . ?
C17 C18 1.481(2) . ?
C17 C22 1.429(2) . ?
C18 C19 1.484(2) . ?
C18 C25 1.362(2) . ?
C19 C20 1.398(2) . ?
C19 C24 1.423(2) . ?
C20 B1 1.531(2) . ?
C21 C22 1.361(2) . ?
C23 C24 1.358(2) . ?
C25 C26 1.491(2) . ?
C25 C28 1.496(2) . ?
C26 C27 1.383(2) . ?
C26 C32 1.431(2) . ?
C28 C29 1.378(2) . ?
C28 C30 1.422(2) . ?
C30 C31 1.359(2) . ?
C32 C33 1.356(2) . ?
C34 C35 1.400(2) . ?
C34 C39 1.398(2) . ?
C35 C36 1.386(2) . ?
C36 C37 1.387(3) . ?
C37 C38 1.382(3) . ?
C38 C39 1.385(2) . ?
C40 C41 1.401(2) . ?
C40 C45 1.401(2) . ?
C41 C42 1.392(2) . ?
C42 C43 1.385(3) . ?
C43 C44 1.378(3) . ?
C44 C45 1.387(3) . ?

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 92.56(8) . . ?
C23 S2 C20 92.45(8) . . ?
C31 S3 C29 92.76(8) . . ?
C33 S4 C27 92.60(8) . . ?
C29 Si1 C27 95.40(7) . . ?
C29 Si1 C34 111.34(7) . . ?
C29 Si1 C40 110.25(7) . . ?
C34 Si1 C27 110.80(7) . . ?
C40 Si1 C27 115.04(7) . . ?
C40 Si1 C34 112.79(7) . . ?
C3 C2 C1 110.3(2) . . ?
C3 C2 C4 113.83(19) . . ?
C4 C2 C1 110.6(2) . . ?
C5 C4 C2 119.40(18) . . ?
C5 C4 C9 117.58(16) . . ?
C9 C4 C2 123.01(18) . . ?
C4 C5 C6 122.41(17) . . ?
C5 C6 C7 119.57(16) . . ?
C5 C6 C13 120.12(16) . . ?
C7 C6 C13 120.21(15) . . ?
C6 C7 B1 121.38(15) . . ?
C8 C7 C6 118.67(15) . . ?
C8 C7 B1 119.92(15) . . ?
C7 C8 C11 119.94(15) . . ?
C9 C8 C7 119.85(16) . . ?
C9 C8 C11 120.20(15) . . ?
C4 C9 C8 121.83(17) . . ?
C8 C11 C10 112.21(14) . . ?
C8 C11 C12 110.91(14) . . ?
C10 C11 C12 112.33(14) . . ?
C6 C13 C14 110.69(15) . . ?
C6 C13 C15 113.25(18) . . ?
C14 C13 C15 110.57(17) . . ?
C17 C16 S1 110.25(12) . . ?
C17 C16 B1 124.44(14) . . ?
B1 C16 S1 124.11(12) . . ?
C16 C17 C18 119.77(14) . . ?
C16 C17 C22 112.33(14) . . ?
C22 C17 C18 127.87(14) . . ?
C17 C18 C19 114.18(13) . . ?
C25 C18 C17 123.24(14) . . ?
C25 C18 C19 122.48(14) . . ?
C20 C19 C18 120.44(14) . . ?
C20 C19 C24 112.60(14) . . ?
C24 C19 C18 126.85(15) . . ?
C19 C20 S2 110.05(12) . . ?
C19 C20 B1 123.97(14) . . ?
B1 C20 S2 125.01(12) . . ?
C22 C21 S1 112.31(13) . . ?
C21 C22 C17 112.47(15) . . ?
C24 C23 S2 112.30(13) . . ?
C23 C24 C19 112.55(16) . . ?
C18 C25 C26 123.56(14) . . ?
C18 C25 C28 124.34(14) . . ?
C26 C25 C28 112.04(13) . . ?
C27 C26 C25 122.55(14) . . ?
C27 C26 C32 112.57(14) . . ?
C32 C26 C25 124.70(14) . . ?
S4 C27 Si1 129.65(10) . . ?
C26 C27 S4 110.53(11) . . ?
C26 C27 Si1 119.73(12) . . ?
C29 C28 C25 119.96(14) . . ?
C29 C28 C30 113.17(14) . . ?
C30 C28 C25 126.55(14) . . ?
S3 C29 Si1 126.41(9) . . ?
C28 C29 S3 110.15(12) . . ?
C28 C29 Si1 122.33(12) . . ?
C31 C30 C28 112.36(15) . . ?
C30 C31 S3 111.56(13) . . ?
C33 C32 C26 112.44(15) . . ?
C32 C33 S4 111.84(12) . . ?
C35 C34 Si1 120.39(13) . . ?
C39 C34 Si1 122.19(13) . . ?
C39 C34 C35 117.40(15) . . ?
C36 C35 C34 121.27(16) . . ?
C35 C36 C37 120.01(17) . . ?
C38 C37 C36 119.75(17) . . ?
C37 C38 C39 120.04(17) . . ?
C38 C39 C34 121.45(16) . . ?
C41 C40 Si1 122.36(13) . . ?
C41 C40 C45 117.44(16) . . ?
C45 C40 Si1 119.89(13) . . ?
C42 C41 C40 121.28(17) . . ?
C43 C42 C41 119.99(17) . . ?
C44 C43 C42 119.64(17) . . ?
C43 C44 C45 120.64(18) . . ?
C44 C45 C40 121.01(18) . . ?
C16 B1 C7 125.62(15) . . ?
C20 B1 C7 123.86(15) . . ?
C20 B1 C16 110.25(14) . . ?

_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 1.067
_oxdiff_exptl_absorpt_empirical_full_min 0.913
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_2694
_database_code_depnum_ccdc_archive 'CCDC 2381484'
loop_
_audit_author_name
_audit_author_address
'Kohei Yamada'
;University
Japan
;
_audit_update_record             
;
2024-09-03 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_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)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C53 H45 B S4 Si'
_chemical_formula_sum            'C53 H45 B S4 Si'
_chemical_formula_weight         849.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         C53H45B1S4Si1
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0376(2)
_cell_length_b                   15.9768(4)
_cell_length_c                   15.9911(3)
_cell_angle_alpha                98.872(2)
_cell_angle_beta                 94.418(2)
_cell_angle_gamma                102.867(2)
_cell_volume                     2209.15(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26910
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.9040
_cell_measurement_theta_min      2.3170
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.939
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             892
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

_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.078
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

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10617
_reflns_number_total             12614
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0353
_refine_ls_restrained_S_all      1.046
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_
_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) . . ?

_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
