# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 2385300'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-01-07
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 As S2'
_chemical_formula_sum            'C9 H5 As S2'
_chemical_formula_weight         252.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         C9H5AsS2
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'
As As 0.0499 2.0058 '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'

_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                   10.5045(11)
_cell_length_b                   6.2032(5)
_cell_length_c                   13.9819(13)
_cell_angle_alpha                90
_cell_angle_beta                 102.093(10)
_cell_angle_gamma                90
_cell_volume                     890.86(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    197.15
_cell_measurement_theta_max      30.8270
_cell_measurement_theta_min      3.0180
_shelx_estimated_absorpt_T_max   0.501
_shelx_estimated_absorpt_T_min   0.124
_exptl_absorpt_coefficient_mu    4.216
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 2 0.1257
-1 0 -2 0.1092
0 -1 0 0.3986
0 1 0 0.4491
1 1 2 0.2334
-1 -2 -2 0.3667
1 -1 2 0.2917
1 0 -1 0.1303
-1 0 1 0.0619

_exptl_crystal_size_max          0.848
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.192
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
0.9999 0.0001 1.9997 -0.0542 0.1186 -0.0394
-0.9986 0.0049 -2.0000 0.0540 -0.1185 0.0399
-0.0018 -1.0015 -0.0014 0.0181 -0.0286 -0.1094
0.0018 1.0015 0.0014 -0.0181 0.0286 0.1094
1.0003 0.9966 2.0014 -0.0721 0.1470 0.0695
-1.0021 -1.9982 -2.0029 0.0902 -0.1756 -0.1789
0.9968 -1.0065 1.9986 -0.0359 0.0899 -0.1494
1.0003 0.0008 -1.0009 -0.0701 -0.0320 -0.0032
-1.0003 -0.0008 1.0009 0.0701 0.0320 0.0032

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3148
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.980
_diffrn_ambient_temperature      197.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00 117.80   0.30    2.50    --   30.00  54.00  30.00  606
  2  ω    -69.00 -44.70   0.30    2.50    --   30.00  54.00 150.00   81
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0648103000
_diffrn_orient_matrix_UB_12      -0.0179741000
_diffrn_orient_matrix_UB_13      0.0053023000
_diffrn_orient_matrix_UB_21      0.0182321000
_diffrn_orient_matrix_UB_22      0.0284146000
_diffrn_orient_matrix_UB_23      0.0502031000
_diffrn_orient_matrix_UB_31      -0.0153254000
_diffrn_orient_matrix_UB_32      0.1092992000
_diffrn_orient_matrix_UB_33      -0.0120500000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                1607
_reflns_number_total             1822
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0363
_refine_ls_restrained_S_all      1.079
_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)+(0.0620P)²+0.3054P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C6(H6), C8(H8)
;
_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
As1 As 0.52132(3) 0.17840(5) 0.60274(2) 0.02838(16) Uani 1 1 d . . . . .
S2 S 0.71722(10) 0.28256(16) 0.46579(7) 0.0341(2) Uani 1 1 d . . . . .
S1 S 0.38566(10) 0.31073(14) 0.77382(7) 0.0346(2) Uani 1 1 d . . . . .
C4 C 0.6993(3) 0.5470(5) 0.6065(2) 0.0254(7) Uani 1 1 d . . . . .
C3 C 0.6604(3) 0.6450(5) 0.6865(2) 0.0264(7) Uani 1 1 d . . . . .
H3 H 0.701047 0.776331 0.711106 0.032 Uiso 1 1 calc R U . . .
C1 C 0.4987(3) 0.3622(5) 0.7030(2) 0.0252(7) Uani 1 1 d . . . . .
C2 C 0.5653(3) 0.5590(5) 0.7314(2) 0.0257(7) Uani 1 1 d . . . . .
C5 C 0.6473(3) 0.3486(5) 0.5641(2) 0.0259(7) Uani 1 1 d . . . . .
C7 C 0.5203(4) 0.6583(6) 0.8119(3) 0.0354(8) Uani 1 1 d . . . . .
H7 H 0.553695 0.790579 0.841045 0.042 Uiso 1 1 calc R U . . .
C9 C 0.7945(3) 0.6361(6) 0.5560(2) 0.0314(8) Uani 1 1 d . . . . .
H9 H 0.838866 0.768372 0.573465 0.038 Uiso 1 1 calc R U . . .
C6 C 0.4268(4) 0.5451(6) 0.8411(3) 0.0387(8) Uani 1 1 d . . . . .
H6 H 0.387192 0.588494 0.893108 0.046 Uiso 1 1 calc R U . . .
C8 C 0.8133(3) 0.5110(6) 0.4816(3) 0.0355(8) Uani 1 1 d . . . . .
H8 H 0.873435 0.544954 0.441733 0.043 Uiso 1 1 calc R U . . .


_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
As1 C1 1.860(3) . ?
As1 C5 1.859(3) . ?
S2 C5 1.737(3) . ?
S2 C8 1.727(4) . ?
S1 C1 1.728(3) . ?
S1 C6 1.736(4) . ?
C4 C3 1.407(5) . ?
C4 C5 1.425(5) . ?
C4 C9 1.450(5) . ?
C3 C2 1.393(5) . ?
C1 C2 1.422(4) . ?
C2 C7 1.446(5) . ?
C7 C6 1.338(5) . ?
C9 C8 1.344(5) . ?

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
C5 As1 C1 94.72(15) . . ?
C8 S2 C5 92.17(17) . . ?
C1 S1 C6 91.87(18) . . ?
C3 C4 C5 123.7(3) . . ?
C3 C4 C9 124.6(3) . . ?
C5 C4 C9 111.7(3) . . ?
C2 C3 C4 123.2(3) . . ?
S1 C1 As1 122.04(18) . . ?
C2 C1 As1 127.1(3) . . ?
C2 C1 S1 110.8(2) . . ?
C3 C2 C1 124.1(3) . . ?
C3 C2 C7 124.7(3) . . ?
C1 C2 C7 111.2(3) . . ?
S2 C5 As1 122.74(19) . . ?
C4 C5 As1 127.1(3) . . ?
C4 C5 S2 110.1(2) . . ?
C6 C7 C2 113.2(3) . . ?
C8 C9 C4 112.6(3) . . ?
C7 C6 S1 112.9(3) . . ?
C9 C8 S2 113.4(3) . . ?


_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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.701
####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 2385302'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2023-05-23
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H9 As S2'
_chemical_formula_sum            'C17 H9 As S2'
_chemical_formula_weight         352.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C17H9S2As
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'
As As 0.0499 2.0058 '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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.4892(12)
_cell_length_b                   8.5408(7)
_cell_length_c                   23.219(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.422(9)
_cell_angle_gamma                90
_cell_volume                     2652.6(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1154
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.0140
_cell_measurement_theta_min      2.8570
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.321
_exptl_absorpt_coefficient_mu    2.861
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 2 0.1454
-1 -2 -2 0.1928
0 0 1 0.0248
0 0 -1 0.0732
-2 -2 1 0.1718
1 0 0 0.1870
-1 0 0 0.2150
1 -1 -1 0.2286
-1 1 1 0.2388

_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.098
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0022 2.0035 1.9990 0.0356 0.0364 0.1805
-1.0022 -2.0035 -1.9990 -0.0356 -0.0364 -0.1805
-0.0026 0.0003 1.0023 -0.0196 0.0209 0.0114
0.0026 -0.0003 -1.0023 0.0196 -0.0209 -0.0114
-2.0106 -2.0023 1.0037 -0.0660 0.0595 -0.1767
1.0006 -0.0002 0.0041 -0.0284 -0.0330 0.0303
-1.0006 0.0002 -0.0041 0.0284 0.0330 -0.0303
0.9999 -1.0020 -0.9934 -0.0604 -0.0677 -0.0448
-0.9999 1.0020 0.9934 0.0604 0.0677 0.0448

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            5607
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.830
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00 105.00   1.00    4.00    --   30.00  54.00   0.00   89
  2  ω    -49.00 111.00   1.00    4.00    --   30.00  54.00 120.00  160
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283140000
_diffrn_orient_matrix_UB_12      0.0515340000
_diffrn_orient_matrix_UB_13      -0.0196683000
_diffrn_orient_matrix_UB_21      -0.0331016000
_diffrn_orient_matrix_UB_22      0.0139534000
_diffrn_orient_matrix_UB_23      0.0207992000
_diffrn_orient_matrix_UB_31      0.0302511000
_diffrn_orient_matrix_UB_32      0.0635990000
_diffrn_orient_matrix_UB_33      0.0113946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1868
_reflns_number_total             2691
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      0.993
_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)+(0.0192P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.1027
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C16(H16), C14(H14), C11(H11), C10(H10), C15(H15), C8(H8),
 C9(H9)
;
_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
As1 As 0.91844(4) 0.40625(6) 0.54168(2) 0.02022(17) Uani 1 1 d . . . . .
S1 S 0.93846(9) 0.55771(16) 0.66589(6) 0.0206(3) Uani 1 1 d . . . . .
S2 S 0.80121(9) 0.34997(16) 0.41723(6) 0.0221(3) Uani 1 1 d . . . . .
C12 C 0.6448(3) 0.5095(6) 0.4412(2) 0.0149(11) Uani 1 1 d . . . . .
C6 C 0.7641(3) 0.6953(6) 0.6456(2) 0.0155(11) Uani 1 1 d . . . . .
C2 C 0.7749(3) 0.6076(6) 0.5933(2) 0.0163(11) Uani 1 1 d . . . . .
C1 C 0.8688(3) 0.5279(6) 0.5975(2) 0.0167(11) Uani 1 1 d . . . . .
C3 C 0.7051(3) 0.6020(6) 0.5433(2) 0.0167(11) Uani 1 1 d . . . . .
H3 H 0.644353 0.658264 0.543259 0.020 Uiso 1 1 calc R U . . .
C5 C 0.8074(3) 0.4342(6) 0.4860(2) 0.0180(11) Uani 1 1 d . . . . .
C13 C 0.5479(3) 0.5703(6) 0.4323(2) 0.0192(12) Uani 1 1 d . . . . .
H13 H 0.522689 0.629431 0.461816 0.023 Uiso 1 1 calc R U . . .
C16 C 0.6202(4) 0.3924(6) 0.3438(2) 0.0214(12) Uani 1 1 d . . . . .
H16 H 0.644915 0.333356 0.314048 0.026 Uiso 1 1 calc R U . . .
C14 C 0.4891(4) 0.5433(6) 0.3798(2) 0.0198(12) Uani 1 1 d . . . . .
H14 H 0.423715 0.586560 0.373292 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7193(3) 0.5189(6) 0.4935(2) 0.0165(11) Uani 1 1 d . . . . .
C17 C 0.6791(3) 0.4208(6) 0.3967(2) 0.0179(11) Uani 1 1 d . . . . .
C7 C 0.8467(3) 0.6807(6) 0.6887(2) 0.0152(11) Uani 1 1 d . . . . .
C11 C 0.6828(3) 0.7871(6) 0.6578(2) 0.0158(11) Uani 1 1 d . . . . .
H11 H 0.625344 0.797106 0.629729 0.019 Uiso 1 1 calc R U . . .
C10 C 0.6867(3) 0.8623(6) 0.7104(2) 0.0205(12) Uani 1 1 d . . . . .
H10 H 0.631784 0.924729 0.718359 0.025 Uiso 1 1 calc R U . . .
C15 C 0.5237(3) 0.4539(6) 0.3362(2) 0.0210(12) Uani 1 1 d . . . . .
H15 H 0.481105 0.434712 0.301068 0.025 Uiso 1 1 calc R U . . .
C8 C 0.8511(3) 0.7570(6) 0.7417(2) 0.0201(12) Uani 1 1 d . . . . .
H8 H 0.908111 0.747238 0.770157 0.024 Uiso 1 1 calc R U . . .
C9 C 0.7700(3) 0.8481(6) 0.7521(2) 0.0218(12) Uani 1 1 d . . . . .
H9 H 0.771422 0.901286 0.788149 0.026 Uiso 1 1 calc R U . . .


_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
As1 C1 1.853(5) . ?
As1 C5 1.864(5) . ?
S1 C1 1.757(5) . ?
S1 C7 1.756(5) . ?
S2 C5 1.743(5) . ?
S2 C17 1.761(5) . ?
C12 C13 1.397(6) . ?
C12 C4 1.474(6) . ?
C12 C17 1.408(7) . ?
C6 C2 1.449(7) . ?
C6 C7 1.403(6) . ?
C6 C11 1.405(6) . ?
C2 C1 1.430(6) . ?
C2 C3 1.399(6) . ?
C3 C4 1.390(7) . ?
C5 C4 1.421(6) . ?
C13 C14 1.385(7) . ?
C16 C17 1.395(7) . ?
C16 C15 1.393(7) . ?
C14 C15 1.395(7) . ?
C7 C8 1.388(7) . ?
C11 C10 1.375(7) . ?
C10 C9 1.391(6) . ?
C8 C9 1.389(7) . ?

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
C1 As1 C5 94.8(2) . . ?
C7 S1 C1 92.5(2) . . ?
C5 S2 C17 92.2(2) . . ?
C13 C12 C4 128.9(5) . . ?
C13 C12 C17 118.7(4) . . ?
C17 C12 C4 112.4(4) . . ?
C7 C6 C2 113.2(4) . . ?
C7 C6 C11 118.4(5) . . ?
C11 C6 C2 128.4(4) . . ?
C1 C2 C6 111.9(4) . . ?
C3 C2 C6 125.8(4) . . ?
C3 C2 C1 122.3(5) . . ?
S1 C1 As1 120.9(3) . . ?
C2 C1 As1 128.1(4) . . ?
C2 C1 S1 111.0(4) . . ?
C4 C3 C2 123.9(4) . . ?
S2 C5 As1 121.5(3) . . ?
C4 C5 As1 126.1(4) . . ?
C4 C5 S2 112.4(4) . . ?
C14 C13 C12 119.2(5) . . ?
C15 C16 C17 117.6(5) . . ?
C13 C14 C15 121.4(5) . . ?
C3 C4 C12 124.0(4) . . ?
C3 C4 C5 124.7(4) . . ?
C5 C4 C12 111.3(5) . . ?
C12 C17 S2 111.7(4) . . ?
C16 C17 S2 125.8(4) . . ?
C16 C17 C12 122.4(4) . . ?
C6 C7 S1 111.4(4) . . ?
C8 C7 S1 126.7(4) . . ?
C8 C7 C6 122.0(4) . . ?
C10 C11 C6 119.9(4) . . ?
C11 C10 C9 120.8(5) . . ?
C16 C15 C14 120.6(5) . . ?
C7 C8 C9 118.2(4) . . ?
C8 C9 C10 120.8(5) . . ?

_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 1.162
_oxdiff_exptl_absorpt_empirical_full_min 0.854
####################################################################### 
# 
# 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_3d-plate
_database_code_depnum_ccdc_archive 'CCDC 2385303'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2023-01-09
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C17 H9 As S2)'
_chemical_formula_sum            'C17 H9 As S2'
_chemical_formula_weight         352.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C17H9S2As
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'
As As 0.0499 2.0058 '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'

_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                   13.1348(11)
_cell_length_b                   8.5422(5)
_cell_length_c                   12.1986(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.983(8)
_cell_angle_gamma                90
_cell_volume                     1365.38(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1242
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.8440
_cell_measurement_theta_min      2.8370
_shelx_estimated_absorpt_T_max   0.814
_shelx_estimated_absorpt_T_min   0.446
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.1034
0 1 1 0.0860
1 -1 2 0.0743
-1 1 -2 0.2419
1 0 0 0.0498
-1 0 0 0.0268

_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.077
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
-0.0013 -1.0005 -1.0006 -0.0746 -0.0486 0.0486
-0.0017 0.9977 1.0013 0.0744 0.0487 -0.0484
0.5006 -1.0045 2.0021 0.0592 0.0385 0.1296
-0.5025 1.0011 -2.0013 -0.0593 -0.0385 -0.1293
0.5003 -0.0003 -0.0001 0.0178 -0.0198 0.0052
-0.5003 0.0003 0.0001 -0.0178 0.0198 -0.0052

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5484
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.847
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.05   0.15    5.00    --   30.00  54.00  90.00 1227
  2  ω     71.00 118.10   0.15    5.00    --   30.00  54.00   0.00  314
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0355425000
_diffrn_orient_matrix_UB_12      0.0358650000
_diffrn_orient_matrix_UB_13      0.0386655000
_diffrn_orient_matrix_UB_21      -0.0395285000
_diffrn_orient_matrix_UB_22      0.0129808000
_diffrn_orient_matrix_UB_23      0.0356360000
_diffrn_orient_matrix_UB_31      0.0103177000
_diffrn_orient_matrix_UB_32      -0.0737445000
_diffrn_orient_matrix_UB_33      0.0251387000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                1619
_reflns_number_total             2805
_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 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         2805
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.088
_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)+(0.0529P)²+0.0847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1643
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 As1A-C5A \\sim As1B-C5B
 with sigma of 0.02
 C17A-C4A \\sim C17B-C4B
 with sigma of 0.04
 S1A-C2A \\sim S1B-C2B
 with sigma of 0.02
 S2A-C4A \\sim S2B-C4B
 with sigma of 0.02
 C5A-C4A \\sim C5B-C4B
 with sigma of 0.02
 C1A-C2A \\sim C1B-C2B
 with sigma of 0.02
 C12A-C4A \\sim C12B-C4B
 with sigma of 0.04
 C6A-C2A \\sim C6B-C2B
 with sigma of 0.04
 As1A-C4A \\sim As1B-C4B
 with sigma of 0.04
 As1A-C2A \\sim As1B-C2B
 with sigma of 0.04
 C12A-C14A \\sim C12B-C14B
 with sigma of 0.04
 C2A-C11A \\sim C2B-C11B
 with sigma of 0.04
 As1A-C1A \\sim As1B-C1B
 with sigma of 0.02
 C9A-C7A \\sim C9B-C7B
 with sigma of 0.04
 C16A-C13A \\sim C16B-C13B
 with sigma of 0.04
 S2A-C13A \\sim S2B-C13B
 with sigma of 0.04
 S1A-C11A \\sim S1B-C11B
 with sigma of 0.02
 C6A-C8A \\sim C6B-C8B
 with sigma of 0.04
 S2A-C12A \\sim S2B-C12B
 with sigma of 0.04
 C5A-C17A \\sim C5B-C17B
 with sigma of 0.02
 C5A-C12A \\sim C5B-C12B
 with sigma of 0.04
 C17A-C13A \\sim C17B-C13B
 with sigma of 0.04
 C1A-C6A \\sim C1B-C6B
 with sigma of 0.02
 C12A-C15A \\sim C12B-C15B
 with sigma of 0.04
 C17A-C12A \\sim C17B-C12B
 with sigma of 0.02
 C17A-C16A \\sim C17B-C16B
 with sigma of 0.02
 C11A-C9A \\sim C11B-C9B
 with sigma of 0.04
 C12A-C13A \\sim C12B-C13B
 with sigma of 0.02
 C6A-C11A \\sim C6B-C11B
 with sigma of 0.02
 S2A-C16A \\sim S2B-C16B
 with sigma of 0.04
 C6A-C7A \\sim C6B-C7B
 with sigma of 0.02
 C5A-C1A \\sim C5B-C1B
 with sigma of 0.04
 C15A-C16A \\sim C15B-C16B
 with sigma of 0.02
 C5A-C16A \\sim C5B-C16B
 with sigma of 0.04
 C15A-C13A \\sim C15B-C13B
 with sigma of 0.02
 C1A-C11A \\sim C1B-C11B
 with sigma of 0.04
 C13A-C14A \\sim C13B-C14B
 with sigma of 0.02
 C10A-C11A \\sim C10B-C11B
 with sigma of 0.02
 C1A-C7A \\sim C1B-C7B
 with sigma of 0.04
 C10A-C9A \\sim C10B-C9B
 with sigma of 0.02
 C17A-C15A \\sim C17B-C15B
 with sigma of 0.04
 C9A-C8A \\sim C9B-C8B
 with sigma of 0.02
 C8A-C7A \\sim C8B-C7B
 with sigma of 0.02
 As1A-C17A \\sim As1B-C17B
 with sigma of 0.04
 C12A-C16A \\sim C12B-C16B
 with sigma of 0.04
 As1A-C6A \\sim As1B-C6B
 with sigma of 0.04
 C6A-C10A \\sim C6B-C10B
 with sigma of 0.04
 C15A-C14A \\sim C15B-C14B
 with sigma of 0.04
 C16A-C14A \\sim C16B-C14B
 with sigma of 0.04
 S1A-C1A \\sim S1B-C1B
 with sigma of 0.04
 C10A-C8A \\sim C10B-C8B
 with sigma of 0.04
 S1A-C6A \\sim S1B-C6B
 with sigma of 0.04
 C11A-C7A \\sim C11B-C7B
 with sigma of 0.04
 S1A-C10A \\sim S1B-C10B
 with sigma of 0.04
 S2A-C5A \\sim S2B-C5B
 with sigma of 0.04
 S2A-C17A \\sim S2B-C17B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 As1B, C5B, C4B, C3B, C2B, C1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C17A, C12A, C13A, C14A, C15A, C16A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7B, C6B, C11B, C10B, C8B, C9B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(As1B)=Sof(S1B)=Sof(S2B)=Sof(C5B)=Sof(C1B)=Sof(C17B)=Sof(C16B)=Sof(H16B)=
 Sof(C15B)=Sof(H15B)=Sof(C14B)=Sof(H14B)=Sof(C13B)=Sof(H13B)=Sof(C12B)=Sof(C6B)=
 Sof(C2B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(C9B)=Sof(H9B)=Sof(C8B)=Sof(H8B)=
 Sof(C4B)=Sof(C7B)=Sof(H7B)=Sof(C3B)=Sof(H3B)=1-FVAR(1)
 Sof(As1A)=Sof(S1A)=Sof(S2A)=Sof(C5A)=Sof(C1A)=Sof(C12A)=Sof(C13A)=Sof(H00F)=
 Sof(C14A)=Sof(H00K)=Sof(C15A)=Sof(H00C)=Sof(C16A)=Sof(H00E)=Sof(C17A)=Sof(C6A)=
 Sof(C2A)=Sof(C10A)=Sof(H00H)=Sof(C11A)=Sof(C9A)=Sof(H00J)=Sof(C8A)=Sof(H00L)=
 Sof(C4A)=Sof(C7A)=Sof(H5)=Sof(C3A)=Sof(H15)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C13A(H00F), C14A(H00K), C15A(H00C), C16A(H00E), C10A(H00H), C9A(H00J),
 C8A(H00L), C7A(H5), C16B(H16B), C15B(H15B), C14B(H14B), C13B(H13B), C10B(H10B),
  C9B(H9B), C8B(H8B), C7B(H7B), C3A(H15), C3B(H3B)
5.b Fitted hexagon refined as free rotating group:
 C12A(C13A,C14A,C15A,C16A,C17A)
;
_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
As1A As 0.47630(12) 0.54011(13) 0.30929(13) 0.0511(5) Uani 0.5269(18) 1 d D . P
A 1
S1A S 0.2148(4) 0.8027(7) 0.4332(6) 0.0598(13) Uani 0.5269(18) 1 d D . P A 1
S2A S 0.6170(2) 0.8237(3) 0.5864(2) 0.0579(9) Uani 0.5269(18) 1 d D . P A 1
C5A C 0.5559(9) 0.642(3) 0.423(2) 0.039(4) Uani 0.5269(18) 1 d D . P A 1
C1A C 0.3523(9) 0.628(2) 0.341(2) 0.049(5) Uani 0.5269(18) 1 d D . P A 1
C12A C 0.7063(8) 0.7149(13) 0.5248(9) 0.066(5) Uani 0.5269(18) 1 d DG . P A 1
C13A C 0.8104(9) 0.7113(18) 0.5547(10) 0.110(6) Uani 0.5269(18) 1 d DG . P A 1
H00F H 0.837451 0.771893 0.615184 0.132 Uiso 0.5269(18) 1 calc R U P A 1
C14A C 0.8748(6) 0.619(2) 0.4962(12) 0.125(9) Uani 0.5269(18) 1 d DG . P A 1
H00K H 0.945878 0.616336 0.516681 0.150 Uiso 0.5269(18) 1 calc R U P A 1
C15A C 0.8352(8) 0.5301(17) 0.4077(11) 0.129(8) Uani 0.5269(18) 1 d DG . P A 1
H00C H 0.879186 0.466965 0.367734 0.155 Uiso 0.5269(18) 1 calc R U P A 1
C16A C 0.7311(8) 0.5338(14) 0.3778(9) 0.081(5) Uani 0.5269(18) 1 d DG . P A 1
H00E H 0.704067 0.473149 0.317290 0.097 Uiso 0.5269(18) 1 calc R U P A 1
C17A C 0.6667(6) 0.6262(13) 0.4363(10) 0.063(4) Uani 0.5269(18) 1 d DG . P A 1
C6A C 0.2562(9) 0.5945(16) 0.2818(11) 0.050(3) Uani 0.5269(18) 1 d D . P A 1
C2A C 0.3416(8) 0.7435(10) 0.4259(9) 0.051(3) Uani 0.5269(18) 1 d D . P A 1
C10A C 0.0746(11) 0.661(2) 0.2787(11) 0.074(5) Uani 0.5269(18) 1 d D . P A 1
H00H H 0.019961 0.718399 0.306543 0.089 Uiso 0.5269(18) 1 calc R U P A 1
C11A C 0.1754(9) 0.6794(14) 0.3225(9) 0.060(3) Uani 0.5269(18) 1 d D . P A 1
C9A C 0.0579(11) 0.5531(18) 0.1910(11) 0.087(5) Uani 0.5269(18) 1 d D . P A 1
H00J H -0.009146 0.540129 0.157647 0.104 Uiso 0.5269(18) 1 calc R U P A 1
C8A C 0.1354(10) 0.4679(15) 0.1536(10) 0.074(4) Uani 0.5269(18) 1 d D . P A 1
H00L H 0.122186 0.391348 0.097959 0.089 Uiso 0.5269(18) 1 calc R U P A 1
C4A C 0.5228(10) 0.7534(12) 0.4925(10) 0.048(3) Uani 0.5269(18) 1 d D . P A 1
C7A C 0.2316(11) 0.4928(18) 0.1963(12) 0.070(5) Uani 0.5269(18) 1 d D . P A 1
H5 H 0.285445 0.437109 0.165724 0.083 Uiso 0.5269(18) 1 calc R U P A 1
As1B As 0.46078(14) 0.75926(16) 0.46670(12) 0.0428(5) Uani 0.4731(18) 1 d D . P
A 2
S1B S 0.2921(4) 0.4985(6) 0.1939(3) 0.0670(12) Uani 0.4731(18) 1 d D . P A 2
S2B S 0.7008(3) 0.4756(4) 0.3189(3) 0.0562(10) Uani 0.4731(18) 1 d D . P A 2
C5B C 0.5794(10) 0.666(3) 0.415(2) 0.033(5) Uani 0.4731(18) 1 d D . P A 2
C1B C 0.3707(10) 0.669(2) 0.358(2) 0.040(4) Uani 0.4731(18) 1 d D . P A 2
C17B C 0.6785(9) 0.6758(17) 0.4760(12) 0.046(4) Uani 0.4731(18) 1 d D . P A 2
C16B C 0.7068(11) 0.7704(15) 0.5665(11) 0.046(3) Uani 0.4731(18) 1 d D . P A 2
H16B H 0.658492 0.834157 0.600082 0.055 Uiso 0.4731(18) 1 calc R U P A 2
C15B C 0.8113(10) 0.7670(19) 0.6063(12) 0.068(4) Uani 0.4731(18) 1 d D . P A 2
H15B H 0.833065 0.832244 0.666450 0.081 Uiso 0.4731(18) 1 calc R U P A 2
C14B C 0.8820(11) 0.672(2) 0.5605(13) 0.079(5) Uani 0.4731(18) 1 d D . P A 2
H14B H 0.950499 0.671023 0.591010 0.095 Uiso 0.4731(18) 1 calc R U P A 2
C13B C 0.8537(10) 0.578(2) 0.4693(13) 0.075(5) Uani 0.4731(18) 1 d D . P A 2
H13B H 0.901954 0.513929 0.436307 0.090 Uiso 0.4731(18) 1 calc R U P A 2
C12B C 0.7516(9) 0.5831(16) 0.4291(10) 0.056(4) Uani 0.4731(18) 1 d D . P A 2
C6B C 0.2629(9) 0.7048(17) 0.3488(10) 0.066(3) Uani 0.4731(18) 1 d D . P A 2
C2B C 0.4007(9) 0.5583(11) 0.2767(8) 0.034(2) Uani 0.4731(18) 1 d D . P A 2
C10B C 0.1038(11) 0.637(3) 0.2380(14) 0.089(6) Uani 0.4731(18) 1 d D . P A 2
H10B H 0.069523 0.576915 0.180969 0.107 Uiso 0.4731(18) 1 calc R U P A 2
C11B C 0.2104(11) 0.625(2) 0.2611(13) 0.070(5) Uani 0.4731(18) 1 d D . P A 2
C9B C 0.0501(13) 0.741(3) 0.3037(16) 0.102(7) Uani 0.4731(18) 1 d D . P A 2
H9B H -0.020757 0.759223 0.287446 0.122 Uiso 0.4731(18) 1 calc R U P A 2
C8B C 0.1006(10) 0.816(2) 0.3903(13) 0.109(6) Uani 0.4731(18) 1 d D . P A 2
H8B H 0.063338 0.877018 0.439044 0.131 Uiso 0.4731(18) 1 calc R U P A 2
C4B C 0.5807(8) 0.5520(10) 0.3345(8) 0.038(2) Uani 0.4731(18) 1 d D . P A 2
C7B C 0.2040(17) 0.805(4) 0.407(2) 0.083(10) Uani 0.4731(18) 1 d D . P A 2
H7B H 0.237477 0.868725 0.462276 0.100 Uiso 0.4731(18) 1 calc R U P A 2
C3A C 0.4153(10) 0.7992(13) 0.4993(10) 0.052(4) Uani 0.5269(18) 1 d . . P A 1
H15 H 0.397319 0.868563 0.555717 0.062 Uiso 0.5269(18) 1 calc R U P A 1
C3B C 0.4970(11) 0.5106(17) 0.2619(13) 0.054(3) Uani 0.4731(18) 1 d . . P A 2
H3B H 0.508599 0.446719 0.200240 0.064 Uiso 0.4731(18) 1 calc R U P A 2


_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
As1A C5A 1.89(2) . ?
As1A C1A 1.857(14) . ?
S1A C2A 1.748(11) . ?
S1A C11A 1.762(12) . ?
S2A C12A 1.711(8) . ?
S2A C4A 1.735(12) . ?
C5A C17A 1.460(12) . ?
C5A C4A 1.36(3) . ?
C1A C6A 1.437(14) . ?
C1A C2A 1.45(2) . ?
C12A C13A 1.3900 . ?
C12A C17A 1.3900 . ?
C13A C14A 1.3900 . ?
C14A C15A 1.3900 . ?
C15A C16A 1.3900 . ?
C16A C17A 1.3900 . ?
C6A C11A 1.405(13) . ?
C6A C7A 1.378(18) . ?
C2A C3A 1.358(15) . ?
C10A C11A 1.402(15) . ?
C10A C9A 1.419(16) . ?
C9A C8A 1.357(15) . ?
C8A C7A 1.350(16) . ?
C4A C3A 1.473(18) . ?
As1B C5B 1.90(2) . ?
As1B C1B 1.875(15) . ?
S1B C2B 1.765(11) . ?
S1B C11B 1.765(14) . ?
S2B C12B 1.724(12) . ?
S2B C4B 1.731(10) . ?
C5B C17B 1.454(14) . ?
C5B C4B 1.38(3) . ?
C1B C6B 1.445(15) . ?
C1B C2B 1.45(2) . ?
C17B C16B 1.399(13) . ?
C17B C12B 1.398(13) . ?
C16B C15B 1.424(13) . ?
C15B C14B 1.378(16) . ?
C14B C13B 1.401(15) . ?
C13B C12B 1.395(14) . ?
C6B C11B 1.408(15) . ?
C6B C7B 1.38(2) . ?
C2B C3B 1.35(2) . ?
C10B C11B 1.412(17) . ?
C10B C9B 1.421(19) . ?
C9B C8B 1.367(18) . ?
C8B C7B 1.36(2) . ?
C4B C3B 1.408(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
C1A As1A C5A 96.4(8) . . ?
C2A S1A C11A 91.0(5) . . ?
C12A S2A C4A 90.1(5) . . ?
C17A C5A As1A 122.3(17) . . ?
C4A C5A As1A 126.4(10) . . ?
C4A C5A C17A 110.8(16) . . ?
C6A C1A As1A 124.7(12) . . ?
C6A C1A C2A 111.6(11) . . ?
C2A C1A As1A 123.6(9) . . ?
C13A C12A S2A 126.0(7) . . ?
C13A C12A C17A 120.0 . . ?
C17A C12A S2A 114.0(7) . . ?
C14A C13A C12A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C14A C15A C16A 120.0 . . ?
C15A C16A C17A 120.0 . . ?
C12A C17A C5A 110.6(13) . . ?
C16A C17A C5A 129.3(13) . . ?
C16A C17A C12A 120.0 . . ?
C11A C6A C1A 112.4(11) . . ?
C7A C6A C1A 130.9(12) . . ?
C7A C6A C11A 116.7(11) . . ?
C1A C2A S1A 112.0(8) . . ?
C3A C2A S1A 120.2(9) . . ?
C3A C2A C1A 127.7(11) . . ?
C11A C10A C9A 116.9(12) . . ?
C6A C11A S1A 113.0(8) . . ?
C10A C11A S1A 125.3(9) . . ?
C10A C11A C6A 121.7(10) . . ?
C8A C9A C10A 121.5(13) . . ?
C7A C8A C9A 119.4(12) . . ?
C5A C4A S2A 114.1(9) . . ?
C5A C4A C3A 124.6(11) . . ?
C3A C4A S2A 120.9(8) . . ?
C8A C7A C6A 123.7(12) . . ?
C1B As1B C5B 95.0(9) . . ?
C2B S1B C11B 92.9(6) . . ?
C12B S2B C4B 91.1(5) . . ?
C17B C5B As1B 122.2(18) . . ?
C4B C5B As1B 125.6(10) . . ?
C4B C5B C17B 110.5(16) . . ?
C6B C1B As1B 122.5(13) . . ?
C6B C1B C2B 113.1(12) . . ?
C2B C1B As1B 124.4(9) . . ?
C16B C17B C5B 128.0(15) . . ?
C12B C17B C5B 112.0(15) . . ?
C12B C17B C16B 119.8(10) . . ?
C17B C16B C15B 117.0(10) . . ?
C14B C15B C16B 122.3(11) . . ?
C15B C14B C13B 120.6(13) . . ?
C12B C13B C14B 117.2(11) . . ?
C17B C12B S2B 112.4(9) . . ?
C13B C12B S2B 124.7(9) . . ?
C13B C12B C17B 123.0(11) . . ?
C11B C6B C1B 112.7(12) . . ?
C7B C6B C1B 131.9(15) . . ?
C7B C6B C11B 115.3(14) . . ?
C1B C2B S1B 109.6(9) . . ?
C3B C2B S1B 124.2(9) . . ?
C3B C2B C1B 126.1(11) . . ?
C11B C10B C9B 117.1(16) . . ?
C6B C11B S1B 111.5(10) . . ?
C6B C11B C10B 123.0(13) . . ?
C10B C11B S1B 125.2(12) . . ?
C8B C9B C10B 119.8(16) . . ?
C7B C8B C9B 120.5(15) . . ?
C5B C4B S2B 113.5(8) . . ?
C5B C4B C3B 125.2(11) . . ?
C3B C4B S2B 120.9(9) . . ?
C8B C7B C6B 123.7(19) . . ?
C2A C3A C4A 120.8(10) . . ?
C2B C3B C4B 122.5(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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.751
####################################################################### 
# 
# 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_3c-P
_database_code_depnum_ccdc_archive 'CCDC 2385305'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2023-10-06
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H9 P S2'
_chemical_formula_sum            'C17 H9 P S2'
_chemical_formula_weight         308.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHSP
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'
P P 0.1023 0.0942 '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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.2423(8)
_cell_length_b                   8.4253(6)
_cell_length_c                   23.5820(15)
_cell_angle_alpha                90
_cell_angle_beta                 97.092(6)
_cell_angle_gamma                90
_cell_volume                     2610.9(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2686
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.5270
_cell_measurement_theta_min      3.0230
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.769
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 1 0.1306
2 0 -1 0.1436
0 1 -1 0.2285
0 -1 1 0.2475
0 0 1 0.0629
0 0 -1 0.0278

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.091
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9921 -0.0033 1.0011 0.0770 -0.0002 -0.0757
1.9921 0.0033 -1.0011 -0.0770 0.0002 0.0757
0.0007 0.9989 -0.9961 0.0591 -0.0016 0.0671
-0.0007 -0.9989 0.9961 -0.0591 0.0016 -0.0671
-0.0000 -0.0007 1.0004 -0.0033 0.0284 -0.0102
0.0000 0.0007 -1.0004 0.0033 -0.0284 0.0102

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            5291
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.056
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  37.10   0.15    2.50    --   30.00  54.00 120.00  734
  2  ω    -68.00  58.90   0.15    2.50    --   30.00  54.00-120.00  846
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403806000
_diffrn_orient_matrix_UB_12      0.0559303000
_diffrn_orient_matrix_UB_13      -0.0032404000
_diffrn_orient_matrix_UB_21      0.0143416000
_diffrn_orient_matrix_UB_22      0.0267444000
_diffrn_orient_matrix_UB_23      0.0283911000
_diffrn_orient_matrix_UB_31      0.0328063000
_diffrn_orient_matrix_UB_32      0.0570395000
_diffrn_orient_matrix_UB_33      -0.0101188000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                2296
_reflns_number_total             2672
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2672
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.096
_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)+(0.0462P)²+2.8341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0963
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C15(H15), C16(H16), C9(H9), C13(H13), C7(H7), C14(H14),
 C8(H8)
;
_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
S2 S 0.06063(4) 0.44133(6) 0.33627(2) 0.01936(15) Uani 1 1 d . . . . .
S1 S 0.18977(4) 0.64454(6) 0.57609(2) 0.02088(15) Uani 1 1 d . . . . .
P1 P 0.08578(4) 0.57931(7) 0.45597(2) 0.01897(15) Uani 1 1 d . . . . .
C4 C 0.22789(15) 0.3887(2) 0.40629(8) 0.0153(4) Uani 1 1 d . . . . .
C11 C 0.35343(15) 0.4895(2) 0.55582(8) 0.0163(4) Uani 1 1 d . . . . .
C10 C 0.45186(16) 0.4287(2) 0.56708(9) 0.0183(4) Uani 1 1 d . . . . .
H10 H 0.480170 0.368117 0.538955 0.022 Uiso 1 1 calc R U . . .
C17 C 0.23862(15) 0.3036(2) 0.35352(8) 0.0153(4) Uani 1 1 d . . . . .
C2 C 0.28179(15) 0.4767(2) 0.50392(8) 0.0160(4) Uani 1 1 d . . . . .
C6 C 0.31345(16) 0.5781(2) 0.59855(9) 0.0180(4) Uani 1 1 d . . . . .
C3 C 0.29883(15) 0.3941(2) 0.45473(8) 0.0159(4) Uani 1 1 d . . . . .
H3 H 0.361472 0.339325 0.454392 0.019 Uiso 1 1 calc R U . . .
C15 C 0.31545(16) 0.1386(3) 0.28781(9) 0.0195(4) Uani 1 1 d . . . . .
H15 H 0.371504 0.077415 0.278684 0.023 Uiso 1 1 calc R U . . .
C16 C 0.32115(14) 0.2121(2) 0.34048(8) 0.0170(4) Uani 1 1 d . . . . .
H16 H 0.380167 0.200774 0.367487 0.020 Uiso 1 1 calc R U . . .
C9 C 0.50791(16) 0.4575(3) 0.61956(9) 0.0206(4) Uani 1 1 d . . . . .
H9 H 0.574903 0.416052 0.627277 0.025 Uiso 1 1 calc R U . . .
C13 C 0.14719(15) 0.2440(3) 0.25942(8) 0.0187(4) Uani 1 1 d . . . . .
H13 H 0.088608 0.255310 0.232107 0.022 Uiso 1 1 calc R U . . .
C1 C 0.18967(16) 0.5588(2) 0.50828(8) 0.0173(4) Uani 1 1 d . . . . .
C7 C 0.36960(17) 0.6067(3) 0.65148(9) 0.0214(4) Uani 1 1 d . . . . .
H7 H 0.341414 0.665895 0.680010 0.026 Uiso 1 1 calc R U . . .
C5 C 0.13317(15) 0.4684(2) 0.40290(8) 0.0174(4) Uani 1 1 d . . . . .
C14 C 0.22883(16) 0.1524(3) 0.24761(9) 0.0201(4) Uani 1 1 d . . . . .
H14 H 0.226058 0.098594 0.212049 0.024 Uiso 1 1 calc R U . . .
C12 C 0.15308(15) 0.3193(2) 0.31243(9) 0.0173(4) Uani 1 1 d . . . . .
C8 C 0.46751(17) 0.5468(3) 0.66145(9) 0.0218(5) Uani 1 1 d . . . . .
H8 H 0.507595 0.566416 0.697010 0.026 Uiso 1 1 calc R U . . .


_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
S2 C5 1.752(2) . ?
S2 C12 1.744(2) . ?
S1 C6 1.750(2) . ?
S1 C1 1.754(2) . ?
P1 C1 1.739(2) . ?
P1 C5 1.740(2) . ?
C4 C17 1.458(3) . ?
C4 C3 1.387(3) . ?
C4 C5 1.416(3) . ?
C11 C10 1.395(3) . ?
C11 C2 1.457(3) . ?
C11 C6 1.409(3) . ?
C10 C9 1.384(3) . ?
C17 C16 1.402(3) . ?
C17 C12 1.403(3) . ?
C2 C3 1.395(3) . ?
C2 C1 1.417(3) . ?
C6 C7 1.393(3) . ?
C15 C16 1.381(3) . ?
C15 C14 1.400(3) . ?
C9 C8 1.399(3) . ?
C13 C14 1.384(3) . ?
C13 C12 1.395(3) . ?
C7 C8 1.384(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
C12 S2 C5 92.11(10) . . ?
C6 S1 C1 92.26(10) . . ?
C1 P1 C5 97.63(9) . . ?
C3 C4 C17 126.25(18) . . ?
C3 C4 C5 122.41(18) . . ?
C5 C4 C17 111.34(17) . . ?
C10 C11 C2 128.98(18) . . ?
C10 C11 C6 118.88(19) . . ?
C6 C11 C2 112.14(18) . . ?
C9 C10 C11 119.43(19) . . ?
C16 C17 C4 128.18(18) . . ?
C16 C17 C12 119.00(18) . . ?
C12 C17 C4 112.81(17) . . ?
C3 C2 C11 125.45(18) . . ?
C3 C2 C1 122.21(18) . . ?
C1 C2 C11 112.34(17) . . ?
C11 C6 S1 111.91(15) . . ?
C7 C6 S1 126.29(16) . . ?
C7 C6 C11 121.79(19) . . ?
C4 C3 C2 122.58(18) . . ?
C16 C15 C14 121.40(19) . . ?
C15 C16 C17 119.08(18) . . ?
C10 C9 C8 121.1(2) . . ?
C14 C13 C12 118.36(18) . . ?
P1 C1 S1 121.13(12) . . ?
C2 C1 S1 111.31(15) . . ?
C2 C1 P1 127.57(16) . . ?
C8 C7 C6 118.30(19) . . ?
P1 C5 S2 120.54(12) . . ?
C4 C5 S2 111.88(15) . . ?
C4 C5 P1 127.57(16) . . ?
C13 C14 C15 120.34(19) . . ?
C17 C12 S2 111.82(15) . . ?
C13 C12 S2 126.37(16) . . ?
C13 C12 C17 121.81(18) . . ?
C7 C8 C9 120.5(2) . . ?

_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 1.719
_oxdiff_exptl_absorpt_empirical_full_min 0.813
####################################################################### 
# 
# 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_3d-P'
_database_code_depnum_ccdc_archive 'CCDC 2385311'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-07-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H20 O3 P2 S4'
_chemical_formula_sum            'C34 H20 O3 P2 S4'
_chemical_formula_weight         666.68
_chemical_melting_point          ?
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'
P P 0.2955 0.4335 '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'

_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                   7.4187(3)
_cell_length_b                   13.2453(5)
_cell_length_c                   17.9755(7)
_cell_angle_alpha                77.315(3)
_cell_angle_beta                 81.898(4)
_cell_angle_gamma                76.885(4)
_cell_volume                     1670.53(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7438
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      75.0930
_cell_measurement_theta_min      3.4570
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.281
_exptl_absorpt_coefficient_mu    3.786
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1309
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16675
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.383
_diffrn_reflns_theta_min         3.493
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5015
_reflns_number_total             6406
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     369
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.1064
_refine_ls_restrained_S_all      1.020
_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)+(0.1790P)²+8.1046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2880
_refine_ls_wR_factor_ref         0.3047
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C25(H25), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C42(H42), C43(H43), C44(H44),
  C45(H45)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
S3 S 0.8166(2) 0.41331(14) 0.55220(9) 0.0321(4) Uani 1 1 d . . . A 1
S4 S 0.7302(2) 0.75169(14) 0.69942(10) 0.0364(4) Uani 1 1 d . . . A 1
S5 S 0.9924(2) 0.30121(14) 0.76605(9) 0.0328(4) Uani 1 1 d . . . A 1
S6 S 0.6901(2) 0.63453(13) 0.91465(9) 0.0314(4) Uani 1 1 d . . . A 1
P7 P 0.3398(2) 0.56803(13) 0.67903(9) 0.0268(4) Uani 1 1 d . . . A 1
P8 P 0.4219(2) 0.42878(13) 0.83476(9) 0.0258(4) Uani 1 1 d . . . A 1
O9 O 0.1571(6) 0.6114(4) 0.6510(3) 0.0319(10) Uani 1 1 d . . . A 1
O10 O 0.3102(6) 0.4941(3) 0.7620(2) 0.0306(9) Uani 1 1 d . . . A 1
O11 O 0.3019(6) 0.3617(4) 0.8837(3) 0.0323(10) Uani 1 1 d . . . A 1
C12 C 0.6263(8) 0.3554(5) 0.5519(3) 0.0268(12) Uani 1 1 d . . . A 1
C13 C 0.6316(10) 0.2696(6) 0.5197(4) 0.0360(14) Uani 1 1 d . . . A 1
H13 H 0.743684 0.236111 0.494843 0.043 Uiso 1 1 calc R U . A 1
C14 C 0.4657(10) 0.2330(6) 0.5249(4) 0.0358(14) Uani 1 1 d . . . A 1
H14 H 0.463081 0.175397 0.501782 0.043 Uiso 1 1 calc R U . A 1
C15 C 0.3046(10) 0.2817(6) 0.5642(4) 0.0357(15) Uani 1 1 d . . . A 1
H15 H 0.193423 0.255748 0.568640 0.043 Uiso 1 1 calc R U . A 1
C16 C 0.3048(9) 0.3672(5) 0.5966(4) 0.0297(13) Uani 1 1 d . . . A 1
H16 H 0.193850 0.400702 0.622102 0.036 Uiso 1 1 calc R U . A 1
C17 C 0.4673(9) 0.4036(5) 0.5917(3) 0.0256(12) Uani 1 1 d . . . A 1
C18 C 0.5019(9) 0.4903(5) 0.6219(4) 0.0291(12) Uani 1 1 d . . . A 1
C19 C 0.6829(9) 0.5028(5) 0.6057(3) 0.0308(13) Uani 1 1 d . . . A 1
C20 C 0.7713(9) 0.5809(6) 0.6254(4) 0.0328(14) Uani 1 1 d . . . A 1
H20A H 0.821571 0.622462 0.577358 0.039 Uiso 1 1 calc R U . A 1
H20B H 0.877612 0.542862 0.655022 0.039 Uiso 1 1 calc R U . A 1
C21 C 0.6453(9) 0.6557(5) 0.6707(4) 0.0302(13) Uani 1 1 d . . . A 1
C22 C 0.4602(9) 0.6603(5) 0.6936(4) 0.0288(12) Uani 1 1 d . . . A 1
C23 C 0.3810(10) 0.7448(5) 0.7361(3) 0.0307(13) Uani 1 1 d . . . A 1
C24 C 0.5140(10) 0.7997(5) 0.7430(4) 0.0333(14) Uani 1 1 d . . . A 1
C25 C 0.4701(11) 0.8823(5) 0.7846(5) 0.0416(16) Uani 1 1 d . . . A 1
H25 H 0.562876 0.917431 0.791686 0.050 Uiso 1 1 calc R U . A 1
C26 C 0.2877(12) 0.9106(6) 0.8149(5) 0.0434(17) Uani 1 1 d . . . A 1
H26 H 0.254510 0.967113 0.842029 0.052 Uiso 1 1 calc R U . A 1
C27 C 0.1524(11) 0.8579(6) 0.8062(4) 0.0406(15) Uani 1 1 d . . . A 1
H27 H 0.028039 0.879003 0.827239 0.049 Uiso 1 1 calc R U . A 1
C28 C 0.1970(11) 0.7747(5) 0.7673(4) 0.0348(14) Uani 1 1 d . . . A 1
H28 H 0.104424 0.738438 0.761697 0.042 Uiso 1 1 calc R U . A 1
C29 C 0.8506(9) 0.2275(5) 0.7437(4) 0.0311(13) Uani 1 1 d . . . A 1
C30 C 0.9045(10) 0.1385(6) 0.7100(4) 0.0377(15) Uani 1 1 d . . . A 1
H30 H 1.032294 0.110803 0.697450 0.045 Uiso 1 1 calc R U . A 1
C31 C 0.7691(10) 0.0918(6) 0.6955(4) 0.0377(15) Uani 1 1 d . . . A 1
H31 H 0.803402 0.031455 0.672251 0.045 Uiso 1 1 calc R U . A 1
C32 C 0.5814(10) 0.1324(5) 0.7145(4) 0.0348(14) Uani 1 1 d . . . A 1
H32 H 0.490003 0.099217 0.703442 0.042 Uiso 1 1 calc R U . A 1
C33 C 0.5251(10) 0.2194(5) 0.7490(3) 0.0305(13) Uani 1 1 d . . . A 1
H33 H 0.397036 0.245347 0.762383 0.037 Uiso 1 1 calc R U . A 1
C34 C 0.6591(9) 0.2678(5) 0.7634(4) 0.0295(12) Uani 1 1 d . . . A 1
C35 C 0.6372(9) 0.3625(5) 0.7968(3) 0.0266(12) Uani 1 1 d . . . A 1
C36 C 0.8015(9) 0.3877(5) 0.8005(3) 0.0285(12) Uani 1 1 d . . . A 1
C37 C 0.8394(9) 0.4779(5) 0.8310(4) 0.0326(14) Uani 1 1 d . . . A 1
H37A H 0.933235 0.449634 0.868402 0.039 Uiso 1 1 calc R U . A 1
H37B H 0.891329 0.527412 0.788231 0.039 Uiso 1 1 calc R U . A 1
C38 C 0.6653(9) 0.5368(5) 0.8692(3) 0.0261(12) Uani 1 1 d . . . A 1
C39 C 0.4849(9) 0.5231(5) 0.8770(3) 0.0281(12) Uani 1 1 d . . . A 1
C40 C 0.3609(9) 0.5921(5) 0.9218(3) 0.0272(12) Uani 1 1 d . . . A 1
C41 C 0.4548(9) 0.6588(5) 0.9461(4) 0.0278(12) Uani 1 1 d . . . A 1
C42 C 0.3660(11) 0.7317(5) 0.9914(4) 0.0358(14) Uani 1 1 d . . . A 1
H42 H 0.432086 0.776332 1.006433 0.043 Uiso 1 1 calc R U . A 1
C43 C 0.1819(10) 0.7372(5) 1.0134(4) 0.0337(14) Uani 1 1 d . . . A 1
H43 H 0.118819 0.785742 1.044854 0.040 Uiso 1 1 calc R U . A 1
C44 C 0.0822(10) 0.6718(5) 0.9902(4) 0.0330(14) Uani 1 1 d . . . A 1
H44 H -0.046599 0.677147 1.006505 0.040 Uiso 1 1 calc R U . A 1
C45 C 0.1691(9) 0.6004(5) 0.9445(4) 0.0301(13) Uani 1 1 d . . . A 1
H45 H 0.100964 0.557550 0.928583 0.036 Uiso 1 1 calc R U . A 1


_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
S3 C12 1.754(7) . ?
S3 C19 1.735(7) . ?
S4 C21 1.739(7) . ?
S4 C24 1.730(7) . ?
S5 C29 1.726(7) . ?
S5 C36 1.741(6) . ?
S6 C38 1.729(6) . ?
S6 C41 1.737(7) . ?
P7 O9 1.461(5) . ?
P7 O10 1.611(5) . ?
P7 C18 1.764(7) . ?
P7 C22 1.750(7) . ?
P8 O10 1.622(5) . ?
P8 O11 1.467(5) . ?
P8 C35 1.762(6) . ?
P8 C39 1.771(7) . ?
C12 C13 1.374(10) . ?
C12 C17 1.389(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.406(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.399(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(9) . ?
C17 C18 1.459(9) . ?
C18 C19 1.373(9) . ?
C19 C20 1.470(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.496(9) . ?
C21 C22 1.368(9) . ?
C22 C23 1.459(9) . ?
C23 C24 1.385(10) . ?
C23 C28 1.404(10) . ?
C24 C25 1.411(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.389(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.387(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.395(10) . ?
C29 C34 1.423(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.374(11) . ?
C31 H31 0.9500 . ?
C31 C32 1.397(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.382(9) . ?
C33 H33 0.9500 . ?
C33 C34 1.379(10) . ?
C34 C35 1.474(9) . ?
C35 C36 1.349(9) . ?
C36 C37 1.513(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.509(9) . ?
C38 C39 1.375(9) . ?
C39 C40 1.437(9) . ?
C40 C41 1.411(9) . ?
C40 C45 1.410(9) . ?
C41 C42 1.391(9) . ?
C42 H42 0.9500 . ?
C42 C43 1.357(10) . ?
C43 H43 0.9500 . ?
C43 C44 1.417(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.378(9) . ?
C45 H45 0.9500 . ?

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
C19 S3 C12 91.4(3) . . ?
C24 S4 C21 91.4(3) . . ?
C29 S5 C36 91.6(3) . . ?
C38 S6 C41 91.7(3) . . ?
O9 P7 O10 107.7(3) . . ?
O9 P7 C18 116.1(3) . . ?
O9 P7 C22 115.9(3) . . ?
O10 P7 C18 107.1(3) . . ?
O10 P7 C22 105.2(3) . . ?
C22 P7 C18 104.0(3) . . ?
O10 P8 C35 106.3(3) . . ?
O10 P8 C39 106.9(3) . . ?
O11 P8 O10 107.2(3) . . ?
O11 P8 C35 116.2(3) . . ?
O11 P8 C39 116.2(3) . . ?
C35 P8 C39 103.3(3) . . ?
P7 O10 P8 141.5(3) . . ?
C13 C12 S3 125.2(5) . . ?
C13 C12 C17 122.8(6) . . ?
C17 C12 S3 111.9(5) . . ?
C12 C13 H13 121.1 . . ?
C12 C13 C14 117.8(6) . . ?
C14 C13 H13 121.1 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.7(7) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 120.9(7) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.6(6) . . ?
C17 C16 H16 120.2 . . ?
C12 C17 C18 111.5(6) . . ?
C16 C17 C12 119.1(6) . . ?
C16 C17 C18 129.5(6) . . ?
C17 C18 P7 125.8(5) . . ?
C19 C18 P7 121.3(5) . . ?
C19 C18 C17 112.7(6) . . ?
C18 C19 S3 112.5(5) . . ?
C18 C19 C20 129.2(6) . . ?
C20 C19 S3 118.3(5) . . ?
C19 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
C19 C20 C21 114.7(5) . . ?
H20A C20 H20B 107.6 . . ?
C21 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
C20 C21 S4 120.1(5) . . ?
C22 C21 S4 112.3(5) . . ?
C22 C21 C20 127.5(6) . . ?
C21 C22 P7 122.8(5) . . ?
C21 C22 C23 112.5(6) . . ?
C23 C22 P7 124.6(5) . . ?
C24 C23 C22 111.2(6) . . ?
C24 C23 C28 120.0(6) . . ?
C28 C23 C22 128.8(6) . . ?
C23 C24 S4 112.6(5) . . ?
C23 C24 C25 121.0(7) . . ?
C25 C24 S4 126.3(5) . . ?
C24 C25 H25 121.0 . . ?
C26 C25 C24 118.0(7) . . ?
C26 C25 H25 121.0 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.2(7) . . ?
C27 C26 H26 119.4 . . ?
C26 C27 H27 119.7 . . ?
C28 C27 C26 120.6(7) . . ?
C28 C27 H27 119.7 . . ?
C23 C28 H28 120.5 . . ?
C27 C28 C23 119.1(7) . . ?
C27 C28 H28 120.5 . . ?
C30 C29 S5 127.5(6) . . ?
C30 C29 C34 120.4(7) . . ?
C34 C29 S5 112.1(5) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 C29 118.6(7) . . ?
C31 C30 H30 120.7 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(6) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 119.1 . . ?
C33 C32 C31 121.7(7) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 120.8 . . ?
C34 C33 C32 118.5(6) . . ?
C34 C33 H33 120.8 . . ?
C29 C34 C35 110.3(6) . . ?
C33 C34 C29 120.2(6) . . ?
C33 C34 C35 129.5(6) . . ?
C34 C35 P8 123.6(5) . . ?
C36 C35 P8 123.8(5) . . ?
C36 C35 C34 112.4(6) . . ?
C35 C36 S5 113.6(5) . . ?
C35 C36 C37 129.0(6) . . ?
C37 C36 S5 117.5(5) . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C38 C37 C36 111.8(5) . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
C37 C38 S6 117.2(5) . . ?
C39 C38 S6 112.5(5) . . ?
C39 C38 C37 130.2(6) . . ?
C38 C39 P8 121.5(5) . . ?
C38 C39 C40 112.7(6) . . ?
C40 C39 P8 125.8(5) . . ?
C41 C40 C39 111.6(6) . . ?
C45 C40 C39 130.2(6) . . ?
C45 C40 C41 118.2(6) . . ?
C40 C41 S6 111.4(5) . . ?
C42 C41 S6 125.9(5) . . ?
C42 C41 C40 122.7(6) . . ?
C41 C42 H42 121.0 . . ?
C43 C42 C41 118.0(7) . . ?
C43 C42 H42 121.0 . . ?
C42 C43 H43 119.4 . . ?
C42 C43 C44 121.3(6) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 H44 119.5 . . ?
C45 C44 C43 121.0(6) . . ?
C45 C44 H44 119.5 . . ?
C40 C45 H45 120.6 . . ?
C44 C45 C40 118.9(6) . . ?
C44 C45 H45 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S3 C12 C13 C14 179.8(5) . . . . ?
S3 C12 C17 C16 179.8(5) . . . . ?
S3 C12 C17 C18 0.8(7) . . . . ?
S3 C19 C20 C21 179.2(5) . . . . ?
S4 C21 C22 P7 -175.4(4) . . . . ?
S4 C21 C22 C23 0.2(7) . . . . ?
S4 C24 C25 C26 179.3(6) . . . . ?
S5 C29 C30 C31 -178.8(5) . . . . ?
S5 C29 C34 C33 179.3(5) . . . . ?
S5 C29 C34 C35 0.7(7) . . . . ?
S5 C36 C37 C38 -171.8(4) . . . . ?
S6 C38 C39 P8 179.3(3) . . . . ?
S6 C38 C39 C40 -0.7(7) . . . . ?
S6 C41 C42 C43 -177.2(5) . . . . ?
P7 C18 C19 S3 177.3(4) . . . . ?
P7 C18 C19 C20 -4.6(10) . . . . ?
P7 C22 C23 C24 175.3(5) . . . . ?
P7 C22 C23 C28 -5.8(10) . . . . ?
P8 C35 C36 S5 174.5(3) . . . . ?
P8 C35 C36 C37 -4.6(10) . . . . ?
P8 C39 C40 C41 -179.1(5) . . . . ?
P8 C39 C40 C45 2.0(10) . . . . ?
O9 P7 O10 P8 -171.4(4) . . . . ?
O9 P7 C18 C17 -49.3(7) . . . . ?
O9 P7 C18 C19 135.2(5) . . . . ?
O9 P7 C22 C21 -135.7(5) . . . . ?
O9 P7 C22 C23 49.3(6) . . . . ?
O10 P7 C18 C17 71.0(6) . . . . ?
O10 P7 C18 C19 -104.5(6) . . . . ?
O10 P7 C22 C21 105.4(6) . . . . ?
O10 P7 C22 C23 -69.6(6) . . . . ?
O10 P8 C35 C34 -75.1(5) . . . . ?
O10 P8 C35 C36 110.4(6) . . . . ?
O10 P8 C39 C38 -106.3(5) . . . . ?
O10 P8 C39 C40 73.7(6) . . . . ?
O11 P8 O10 P7 -168.6(4) . . . . ?
O11 P8 C35 C34 44.1(6) . . . . ?
O11 P8 C35 C36 -130.4(5) . . . . ?
O11 P8 C39 C38 134.0(5) . . . . ?
O11 P8 C39 C40 -46.0(6) . . . . ?
C12 S3 C19 C18 -0.7(5) . . . . ?
C12 S3 C19 C20 -179.0(5) . . . . ?
C12 C13 C14 C15 -2.2(10) . . . . ?
C12 C17 C18 P7 -177.2(5) . . . . ?
C12 C17 C18 C19 -1.4(8) . . . . ?
C13 C12 C17 C16 -2.9(10) . . . . ?
C13 C12 C17 C18 178.1(6) . . . . ?
C13 C14 C15 C16 1.5(11) . . . . ?
C14 C15 C16 C17 -1.5(11) . . . . ?
C15 C16 C17 C12 2.1(10) . . . . ?
C15 C16 C17 C18 -179.1(7) . . . . ?
C16 C17 C18 P7 3.9(10) . . . . ?
C16 C17 C18 C19 179.7(6) . . . . ?
C17 C12 C13 C14 2.9(10) . . . . ?
C17 C18 C19 S3 1.3(7) . . . . ?
C17 C18 C19 C20 179.3(6) . . . . ?
C18 P7 O10 P8 63.1(5) . . . . ?
C18 P7 C22 C21 -7.0(6) . . . . ?
C18 P7 C22 C23 178.0(5) . . . . ?
C18 C19 C20 C21 1.3(10) . . . . ?
C19 S3 C12 C13 -177.3(6) . . . . ?
C19 S3 C12 C17 -0.1(5) . . . . ?
C19 C20 C21 S4 179.1(5) . . . . ?
C19 C20 C21 C22 -1.6(10) . . . . ?
C20 C21 C22 P7 5.3(10) . . . . ?
C20 C21 C22 C23 -179.1(6) . . . . ?
C21 S4 C24 C23 0.0(5) . . . . ?
C21 S4 C24 C25 177.5(7) . . . . ?
C21 C22 C23 C24 -0.2(8) . . . . ?
C21 C22 C23 C28 178.8(6) . . . . ?
C22 P7 O10 P8 -47.2(5) . . . . ?
C22 P7 C18 C17 -177.9(5) . . . . ?
C22 P7 C18 C19 6.6(6) . . . . ?
C22 C23 C24 S4 0.1(7) . . . . ?
C22 C23 C24 C25 -177.5(6) . . . . ?
C22 C23 C28 C27 179.7(6) . . . . ?
C23 C24 C25 C26 -3.4(11) . . . . ?
C24 S4 C21 C20 179.3(6) . . . . ?
C24 S4 C21 C22 -0.1(5) . . . . ?
C24 C23 C28 C27 -1.5(10) . . . . ?
C24 C25 C26 C27 1.5(12) . . . . ?
C25 C26 C27 C28 0.4(12) . . . . ?
C26 C27 C28 C23 -0.4(10) . . . . ?
C28 C23 C24 S4 -179.0(5) . . . . ?
C28 C23 C24 C25 3.5(10) . . . . ?
C29 S5 C36 C35 0.8(5) . . . . ?
C29 S5 C36 C37 -180.0(5) . . . . ?
C29 C30 C31 C32 -0.4(11) . . . . ?
C29 C34 C35 P8 -175.1(4) . . . . ?
C29 C34 C35 C36 0.0(7) . . . . ?
C30 C29 C34 C33 -0.4(9) . . . . ?
C30 C29 C34 C35 -179.1(6) . . . . ?
C30 C31 C32 C33 -0.6(11) . . . . ?
C31 C32 C33 C34 1.1(10) . . . . ?
C32 C33 C34 C29 -0.6(9) . . . . ?
C32 C33 C34 C35 177.8(6) . . . . ?
C33 C34 C35 P8 6.4(10) . . . . ?
C33 C34 C35 C36 -178.6(6) . . . . ?
C34 C29 C30 C31 0.9(10) . . . . ?
C34 C35 C36 S5 -0.6(7) . . . . ?
C34 C35 C36 C37 -179.6(6) . . . . ?
C35 P8 O10 P7 -43.7(5) . . . . ?
C35 P8 C39 C38 5.6(6) . . . . ?
C35 P8 C39 C40 -174.4(5) . . . . ?
C35 C36 C37 C38 7.2(9) . . . . ?
C36 S5 C29 C30 178.9(6) . . . . ?
C36 S5 C29 C34 -0.9(5) . . . . ?
C36 C37 C38 S6 174.2(4) . . . . ?
C36 C37 C38 C39 -2.8(9) . . . . ?
C37 C38 C39 P8 -3.6(10) . . . . ?
C37 C38 C39 C40 176.4(6) . . . . ?
C38 S6 C41 C40 0.2(5) . . . . ?
C38 S6 C41 C42 178.4(6) . . . . ?
C38 C39 C40 C41 0.9(8) . . . . ?
C38 C39 C40 C45 -178.0(6) . . . . ?
C39 P8 O10 P7 66.1(5) . . . . ?
C39 P8 C35 C34 172.6(5) . . . . ?
C39 P8 C35 C36 -2.0(6) . . . . ?
C39 C40 C41 S6 -0.6(7) . . . . ?
C39 C40 C41 C42 -178.9(6) . . . . ?
C39 C40 C45 C44 177.8(6) . . . . ?
C40 C41 C42 C43 0.8(10) . . . . ?
C41 S6 C38 C37 -177.2(5) . . . . ?
C41 S6 C38 C39 0.3(5) . . . . ?
C41 C40 C45 C44 -1.0(9) . . . . ?
C41 C42 C43 C44 -0.8(10) . . . . ?
C42 C43 C44 C45 -0.1(10) . . . . ?
C43 C44 C45 C40 1.0(10) . . . . ?
C45 C40 C41 S6 178.4(5) . . . . ?
C45 C40 C41 C42 0.1(9) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.397 0.000 0.000 197.7 54.8 ?
2 -0.449 0.000 0.500 187.8 54.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3d'
_database_code_depnum_ccdc_archive 'CCDC 2385310'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2023-01-23
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H16 As2 S4'
_chemical_formula_sum            'C34 H16 As2 S4'
_chemical_formula_weight         702.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHSAs
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'
As As 0.0499 2.0058 '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'

_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                   8.0954(6)
_cell_length_b                   11.3660(7)
_cell_length_c                   15.4655(8)
_cell_angle_alpha                87.822(5)
_cell_angle_beta                 85.309(5)
_cell_angle_gamma                80.114(6)
_cell_volume                     1396.77(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3347
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.3340
_cell_measurement_theta_min      2.8670
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.288
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             700
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 1 0.0195
0 -2 -1 0.0360
0 0 -1 0.0163
0 0 1 0.0879
-1 0 0 0.3122
1 0 0 0.2731

_exptl_crystal_size_max          0.608
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.055
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 2.0000 1.0000 0.0188 0.1322 0.0073
0.0000 -2.0000 -1.0000 -0.0188 -0.1322 -0.0073
0.0000 0.0000 -1.0000 -0.0452 -0.0086 0.0010
-0.0000 -0.0000 1.0000 0.0452 0.0086 -0.0010
-1.0000 0.0000 -0.0000 0.0068 0.0110 0.0883
1.0000 -0.0000 0.0000 -0.0068 -0.0110 -0.0883

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8439
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.791
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -46.00   0.10    7.00    --   30.00  54.00 120.00  270
  2  ω      8.00  34.00   0.10    7.00    --   30.00  54.00 120.00  260
  3  ω    -71.00  34.00   0.10    7.00    --   30.00  54.00   0.00 1050
  4  ω    -74.00 110.00   0.10    7.00    --   30.00  54.00-120.00 1840
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067839000
_diffrn_orient_matrix_UB_12      -0.0132236000
_diffrn_orient_matrix_UB_13      0.0452128000
_diffrn_orient_matrix_UB_21      -0.0109842000
_diffrn_orient_matrix_UB_22      0.0618299000
_diffrn_orient_matrix_UB_23      0.0085846000
_diffrn_orient_matrix_UB_31      -0.0882605000
_diffrn_orient_matrix_UB_32      0.0041619000
_diffrn_orient_matrix_UB_33      -0.0009874000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                4442
_reflns_number_total             5695
_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 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.016
_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)+(0.0477P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1076
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C10(H10), C33(H33), C30(H30), C25(H25), C26(H26),
 C32(H32), C7(H7), C31(H31), C16(H16), C8(H8), C15(H15), C9(H9), C13(H13),
 C14(H14)
;
_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
As1 As 0.27084(5) 0.58314(3) 0.49709(2) 0.02374(12) Uani 1 1 d . . . . .
As2 As 0.42314(5) 0.19194(3) 0.05775(2) 0.02212(12) Uani 1 1 d . . . . .
S3 S 0.02907(13) 0.45315(9) 0.19765(6) 0.0237(2) Uani 1 1 d . . . . .
S4 S 0.67583(13) 0.28864(9) 0.28332(6) 0.0254(2) Uani 1 1 d . . . . .
S1 S 0.43213(13) 0.62448(9) 0.21747(6) 0.0257(2) Uani 1 1 d . . . . .
S2 S 0.23592(14) 0.23292(9) 0.38908(6) 0.0286(2) Uani 1 1 d . . . . .
C3 C 0.3276(5) 0.4362(3) 0.3122(2) 0.0199(8) Uani 1 1 d . . . . .
C34 C 0.7311(5) 0.1448(3) 0.1513(2) 0.0207(8) Uani 1 1 d . . . . .
C18 C 0.2363(5) 0.3012(3) 0.0983(2) 0.0184(8) Uani 1 1 d . . . . .
C1 C 0.3452(5) 0.6255(3) 0.3851(2) 0.0206(8) Uani 1 1 d . . . . .
C22 C 0.5618(5) 0.2101(3) 0.1453(2) 0.0201(8) Uani 1 1 d . . . . .
C20 C 0.3584(5) 0.3639(3) 0.2305(2) 0.0207(8) Uani 1 1 d . . . . .
C2 C 0.3614(5) 0.5520(3) 0.3126(2) 0.0213(8) Uani 1 1 d . . . . .
C4 C 0.2715(5) 0.3811(3) 0.3890(2) 0.0225(8) Uani 1 1 d . . . . .
C11 C 0.3950(5) 0.7412(3) 0.3627(2) 0.0236(9) Uani 1 1 d . . . . .
C28 C 0.0800(5) 0.3260(3) 0.0572(2) 0.0200(8) Uani 1 1 d . . . . .
C19 C 0.2288(5) 0.3658(3) 0.1755(2) 0.0192(8) Uani 1 1 d . . . . .
C29 C 0.8084(5) 0.1792(3) 0.2222(2) 0.0222(8) Uani 1 1 d . . . . .
C21 C 0.5135(5) 0.2908(3) 0.2139(2) 0.0218(8) Uani 1 1 d . . . . .
C5 C 0.2404(5) 0.4307(3) 0.4720(2) 0.0205(8) Uani 1 1 d . . . . .
C17 C 0.1832(5) 0.3456(4) 0.5354(2) 0.0240(9) Uani 1 1 d . . . . .
C27 C 0.0390(5) 0.2817(3) -0.0208(2) 0.0225(8) Uani 1 1 d . . . . .
H27 H 0.120004 0.227175 -0.053677 0.027 Uiso 1 1 calc R U . . .
C24 C -0.2041(5) 0.4447(3) 0.0743(3) 0.0259(9) Uani 1 1 d . . . . .
H24 H -0.286171 0.499838 0.106068 0.031 Uiso 1 1 calc R U . . .
C23 C -0.0438(5) 0.4078(3) 0.1035(2) 0.0207(8) Uani 1 1 d . . . . .
C10 C 0.4018(5) 0.8353(3) 0.4171(3) 0.0299(10) Uani 1 1 d . . . . .
H10 H 0.370183 0.828703 0.477363 0.036 Uiso 1 1 calc R U . . .
C33 C 0.8213(5) 0.0538(3) 0.0986(2) 0.0249(9) Uani 1 1 d . . . . .
H33 H 0.771449 0.027547 0.050889 0.030 Uiso 1 1 calc R U . . .
C30 C 0.9718(5) 0.1287(4) 0.2388(3) 0.0273(9) Uani 1 1 d . . . . .
H30 H 1.023311 0.154446 0.286128 0.033 Uiso 1 1 calc R U . . .
C25 C -0.2395(5) 0.3986(3) -0.0021(2) 0.0249(9) Uani 1 1 d . . . . .
H25 H -0.347592 0.422132 -0.023110 0.030 Uiso 1 1 calc R U . . .
C26 C -0.1190(5) 0.3179(3) -0.0490(2) 0.0261(9) Uani 1 1 d . . . . .
H26 H -0.146509 0.287483 -0.101388 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4436(5) 0.7531(3) 0.2738(2) 0.0246(9) Uani 1 1 d . . . . .
C12 C 0.1717(5) 0.2363(4) 0.4996(2) 0.0271(9) Uani 1 1 d . . . . .
C32 C 0.9820(5) 0.0031(4) 0.1163(3) 0.0284(9) Uani 1 1 d . . . . .
H32 H 1.042194 -0.058773 0.080716 0.034 Uiso 1 1 calc R U . . .
C7 C 0.4973(5) 0.8569(4) 0.2392(3) 0.0320(10) Uani 1 1 d . . . . .
H7 H 0.530612 0.863820 0.179141 0.038 Uiso 1 1 calc R U . . .
C31 C 1.0580(5) 0.0405(4) 0.1853(3) 0.0303(10) Uani 1 1 d . . . . .
H31 H 1.169958 0.005129 0.195783 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1387(5) 0.3615(4) 0.6247(2) 0.0292(10) Uani 1 1 d . . . . .
H16 H 0.146817 0.434443 0.650753 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5007(6) 0.9491(4) 0.2944(3) 0.0363(11) Uani 1 1 d . . . . .
H8 H 0.534790 1.020883 0.272010 0.044 Uiso 1 1 calc R U . . .
C15 C 0.0829(6) 0.2700(4) 0.6744(3) 0.0395(12) Uani 1 1 d . . . . .
H15 H 0.053030 0.280216 0.734638 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4542(6) 0.9373(4) 0.3835(3) 0.0367(11) Uani 1 1 d . . . . .
H9 H 0.459196 1.000784 0.420874 0.044 Uiso 1 1 calc R U . . .
C13 C 0.1152(6) 0.1439(4) 0.5494(3) 0.0369(11) Uani 1 1 d . . . . .
H13 H 0.107861 0.070196 0.524197 0.044 Uiso 1 1 calc R U . . .
C14 C 0.0704(6) 0.1629(4) 0.6364(3) 0.0417(12) Uani 1 1 d . . . . .
H14 H 0.030023 0.101661 0.671178 0.050 Uiso 1 1 calc R U . . .


_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
As1 C1 1.860(4) . ?
As1 C5 1.852(4) . ?
As2 C18 1.866(4) . ?
As2 C22 1.868(4) . ?
S3 C19 1.761(4) . ?
S3 C23 1.742(4) . ?
S4 C29 1.748(4) . ?
S4 C21 1.761(4) . ?
S1 C2 1.762(4) . ?
S1 C6 1.750(4) . ?
S2 C4 1.757(4) . ?
S2 C12 1.745(4) . ?
C3 C20 1.514(5) . ?
C3 C2 1.390(5) . ?
C3 C4 1.400(5) . ?
C34 C22 1.450(5) . ?
C34 C29 1.405(5) . ?
C34 C33 1.406(5) . ?
C18 C28 1.443(5) . ?
C18 C19 1.418(5) . ?
C1 C2 1.407(5) . ?
C1 C11 1.462(5) . ?
C22 C21 1.414(5) . ?
C20 C19 1.400(5) . ?
C20 C21 1.392(5) . ?
C4 C5 1.407(5) . ?
C11 C10 1.397(5) . ?
C11 C6 1.407(5) . ?
C28 C27 1.409(5) . ?
C28 C23 1.413(5) . ?
C29 C30 1.389(6) . ?
C5 C17 1.455(5) . ?
C17 C12 1.399(6) . ?
C17 C16 1.410(5) . ?
C27 C26 1.376(6) . ?
C24 C23 1.400(6) . ?
C24 C25 1.381(5) . ?
C10 C9 1.371(5) . ?
C33 C32 1.374(6) . ?
C30 C31 1.380(6) . ?
C25 C26 1.394(5) . ?
C6 C7 1.399(5) . ?
C12 C13 1.398(5) . ?
C32 C31 1.390(6) . ?
C7 C8 1.382(6) . ?
C16 C15 1.385(6) . ?
C8 C9 1.406(6) . ?
C15 C14 1.394(7) . ?
C13 C14 1.379(6) . ?

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
C5 As1 C1 96.44(16) . . ?
C18 As2 C22 97.38(16) . . ?
C23 S3 C19 91.88(18) . . ?
C29 S4 C21 91.54(18) . . ?
C6 S1 C2 91.98(18) . . ?
C12 S2 C4 91.60(18) . . ?
C2 C3 C20 121.4(3) . . ?
C2 C3 C4 120.5(3) . . ?
C4 C3 C20 118.1(3) . . ?
C29 C34 C22 112.4(3) . . ?
C29 C34 C33 118.3(4) . . ?
C33 C34 C22 129.3(4) . . ?
C28 C18 As2 124.2(3) . . ?
C19 C18 As2 123.8(3) . . ?
C19 C18 C28 111.9(3) . . ?
C2 C1 As1 125.1(3) . . ?
C2 C1 C11 112.0(3) . . ?
C11 C1 As1 122.9(3) . . ?
C34 C22 As2 124.6(3) . . ?
C21 C22 As2 123.5(3) . . ?
C21 C22 C34 111.9(3) . . ?
C19 C20 C3 120.0(3) . . ?
C21 C20 C3 119.0(3) . . ?
C21 C20 C19 120.9(3) . . ?
C3 C2 S1 121.9(3) . . ?
C3 C2 C1 126.4(3) . . ?
C1 C2 S1 111.7(3) . . ?
C3 C4 S2 120.4(3) . . ?
C3 C4 C5 127.2(3) . . ?
C5 C4 S2 112.4(3) . . ?
C10 C11 C1 128.8(4) . . ?
C10 C11 C6 118.8(3) . . ?
C6 C11 C1 112.4(3) . . ?
C27 C28 C18 129.0(3) . . ?
C27 C28 C23 118.3(4) . . ?
C23 C28 C18 112.7(3) . . ?
C18 C19 S3 111.5(3) . . ?
C20 C19 S3 121.6(3) . . ?
C20 C19 C18 126.8(3) . . ?
C34 C29 S4 112.3(3) . . ?
C30 C29 S4 126.1(3) . . ?
C30 C29 C34 121.6(4) . . ?
C22 C21 S4 111.8(3) . . ?
C20 C21 S4 120.7(3) . . ?
C20 C21 C22 127.5(4) . . ?
C4 C5 As1 124.4(3) . . ?
C4 C5 C17 111.0(3) . . ?
C17 C5 As1 124.6(3) . . ?
C12 C17 C5 113.2(3) . . ?
C12 C17 C16 118.6(4) . . ?
C16 C17 C5 128.2(4) . . ?
C26 C27 C28 119.6(4) . . ?
C25 C24 C23 118.0(4) . . ?
C28 C23 S3 111.9(3) . . ?
C24 C23 S3 126.2(3) . . ?
C24 C23 C28 121.8(4) . . ?
C9 C10 C11 120.0(4) . . ?
C32 C33 C34 119.7(4) . . ?
C31 C30 C29 118.8(4) . . ?
C24 C25 C26 121.1(4) . . ?
C27 C26 C25 121.2(4) . . ?
C11 C6 S1 111.9(3) . . ?
C7 C6 S1 126.7(3) . . ?
C7 C6 C11 121.4(4) . . ?
C17 C12 S2 111.8(3) . . ?
C13 C12 S2 126.2(3) . . ?
C13 C12 C17 122.0(4) . . ?
C33 C32 C31 121.2(4) . . ?
C8 C7 C6 118.4(4) . . ?
C30 C31 C32 120.4(4) . . ?
C15 C16 C17 119.6(4) . . ?
C7 C8 C9 120.5(4) . . ?
C16 C15 C14 120.4(4) . . ?
C10 C9 C8 120.9(4) . . ?
C14 C13 C12 117.9(4) . . ?
C13 C14 C15 121.6(4) . . ?

_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 1.671
_oxdiff_exptl_absorpt_empirical_full_min 0.656
####################################################################### 
# 
# 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_3d-needle
_database_code_depnum_ccdc_archive 'CCDC 2385304'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-04-30
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H9 As S2'
_chemical_formula_sum            'C17 H9 As S2'
_chemical_formula_weight         352.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHSAs
_chemical_oxdiff_usercomment     ' '
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'
As As 0.0499 2.0058 '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'

_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                   14.5703(9)
_cell_length_b                   3.9421(3)
_cell_length_c                   23.8017(18)
_cell_angle_alpha                90
_cell_angle_beta                 99.317(7)
_cell_angle_gamma                90
_cell_volume                     1349.08(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.4370
_cell_measurement_theta_min      2.9060
_shelx_estimated_absorpt_T_max   0.901
_shelx_estimated_absorpt_T_min   0.353
_exptl_absorpt_coefficient_mu    2.812
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.0300
1 0 -1 0.0134
-1 1 -2 0.1939
1 -1 2 0.2040
0 0 1 0.0175
0 0 -1 0.0206
2 0 1 0.0190
-2 0 -1 0.0437

_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.038
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0010 -0.0004 0.9988 0.0127 0.0507 0.0117
1.0010 0.0004 -0.9988 -0.0127 -0.0507 -0.0117
-1.0038 1.0017 -1.9902 -0.0168 -0.0243 0.1966
1.0038 -1.0017 1.9902 0.0168 0.0243 -0.1966
-0.0006 -0.0003 1.0009 -0.0200 0.0205 -0.0097
0.0006 0.0003 -1.0009 0.0200 -0.0205 0.0097
2.0004 -0.0001 1.0051 -0.0853 -0.0399 -0.0525
-2.0004 0.0001 -1.0051 0.0853 0.0399 0.0525

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4939
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.074
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     15.00  42.00   0.15   15.00    --   30.00  54.00 -90.00  180
  2  ω    -66.00 -39.00   0.15   15.00    --   30.00  54.00   0.00  180
  3  ω    -65.00 110.05   0.15   15.00    --   30.00  54.00  30.00 1167
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0325814000
_diffrn_orient_matrix_UB_12      -0.0891523000
_diffrn_orient_matrix_UB_13      -0.0200149000
_diffrn_orient_matrix_UB_21      -0.0302175000
_diffrn_orient_matrix_UB_22      -0.0139382000
_diffrn_orient_matrix_UB_23      0.0204526000
_diffrn_orient_matrix_UB_31      -0.0214097000
_diffrn_orient_matrix_UB_32      0.1556868000
_diffrn_orient_matrix_UB_33      -0.0096449000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                2141
_reflns_number_total             2741
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.418
_refine_diff_density_min         -2.132
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.053
_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)+(0.0839P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1369
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C11(H11), C10(H10), C9(H9), C8(H8), C15(H15), C17(H17),
 C16(H16)
;
_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
As1 As 0.32922(3) 0.44672(13) 0.46628(2) 0.01851(19) Uani 1 1 d . . . . .
S2 S 0.04342(8) 0.8676(3) 0.42105(5) 0.0217(3) Uani 1 1 d . . . . .
S1 S 0.20890(8) 0.3231(3) 0.62529(5) 0.0218(3) Uani 1 1 d . . . . .
C1 C 0.2997(3) 0.3588(11) 0.53790(19) 0.0161(9) Uani 1 1 d . . . . .
C3 C 0.1369(3) 0.5922(12) 0.5201(2) 0.0204(10) Uani 1 1 d . . . . .
H3 H 0.082206 0.637265 0.535786 0.025 Uiso 1 1 calc R U . . .
C4 C 0.1399(3) 0.6785(12) 0.4639(2) 0.0191(10) Uani 1 1 d . . . . .
C14 C 0.0706(3) 1.0503(12) 0.3110(2) 0.0235(11) Uani 1 1 d . . . . .
H14 H 0.009398 1.140615 0.302994 0.028 Uiso 1 1 calc R U . . .
C2 C 0.2127(3) 0.4409(12) 0.55398(19) 0.0175(9) Uani 1 1 d . . . . .
C11 C 0.4527(3) 0.0821(12) 0.5838(2) 0.0222(11) Uani 1 1 d . . . . .
H11 H 0.480330 0.102710 0.550413 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5021(3) -0.0651(13) 0.6325(2) 0.0258(11) Uani 1 1 d . . . . .
H10 H 0.563279 -0.148090 0.632365 0.031 Uiso 1 1 calc R U . . .
C5 C 0.2159(3) 0.6359(12) 0.43432(19) 0.0180(10) Uani 1 1 d . . . . .
C12 C 0.1947(3) 0.7671(12) 0.37651(19) 0.0191(10) Uani 1 1 d . . . . .
C13 C 0.1039(3) 0.9043(12) 0.3639(2) 0.0201(10) Uani 1 1 d . . . . .
C6 C 0.3624(3) 0.1996(12) 0.58393(19) 0.0190(10) Uani 1 1 d . . . . .
C9 C 0.4617(4) -0.0911(13) 0.6818(2) 0.0259(11) Uani 1 1 d . . . . .
H9 H 0.496294 -0.190050 0.714976 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3230(3) 0.1683(13) 0.6339(2) 0.0203(10) Uani 1 1 d . . . . .
C8 C 0.3727(3) 0.0236(13) 0.6832(2) 0.0233(11) Uani 1 1 d . . . . .
H8 H 0.345925 0.004775 0.716919 0.028 Uiso 1 1 calc R U . . .
C15 C 0.1284(4) 1.0600(13) 0.2707(2) 0.0257(11) Uani 1 1 d . . . . .
H15 H 0.106937 1.159466 0.234650 0.031 Uiso 1 1 calc R U . . .
C17 C 0.2519(3) 0.7829(13) 0.3345(2) 0.0223(10) Uani 1 1 d . . . . .
H17 H 0.313417 0.695586 0.342097 0.027 Uiso 1 1 calc R U . . .
C16 C 0.2189(4) 0.9250(13) 0.2822(2) 0.0246(11) Uani 1 1 d . . . . .
H16 H 0.257494 0.931708 0.253637 0.029 Uiso 1 1 calc R U . . .


_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
As1 C1 1.857(5) . ?
As1 C5 1.859(5) . ?
S2 C4 1.762(5) . ?
S2 C13 1.742(5) . ?
S1 C2 1.769(5) . ?
S1 C7 1.752(5) . ?
C1 C2 1.419(6) . ?
C1 C6 1.451(6) . ?
C3 C4 1.389(7) . ?
C3 C2 1.391(7) . ?
C4 C5 1.415(6) . ?
C14 C13 1.400(7) . ?
C14 C15 1.374(7) . ?
C11 C10 1.389(7) . ?
C11 C6 1.395(7) . ?
C10 C9 1.399(7) . ?
C5 C12 1.456(6) . ?
C12 C13 1.414(6) . ?
C12 C17 1.403(6) . ?
C6 C7 1.407(6) . ?
C9 C8 1.378(7) . ?
C7 C8 1.398(7) . ?
C15 C16 1.406(7) . ?
C17 C16 1.379(7) . ?

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
C1 As1 C5 97.4(2) . . ?
C13 S2 C4 91.7(2) . . ?
C7 S1 C2 91.5(2) . . ?
C2 C1 As1 123.7(3) . . ?
C2 C1 C6 112.1(4) . . ?
C6 C1 As1 124.2(3) . . ?
C4 C3 C2 121.2(4) . . ?
C3 C4 S2 121.0(4) . . ?
C3 C4 C5 126.8(4) . . ?
C5 C4 S2 112.2(4) . . ?
C15 C14 C13 118.4(5) . . ?
C1 C2 S1 111.5(3) . . ?
C3 C2 S1 121.5(4) . . ?
C3 C2 C1 126.9(4) . . ?
C10 C11 C6 119.9(5) . . ?
C11 C10 C9 119.9(5) . . ?
C4 C5 As1 124.0(4) . . ?
C4 C5 C12 111.4(4) . . ?
C12 C5 As1 124.6(3) . . ?
C13 C12 C5 112.6(4) . . ?
C17 C12 C5 129.0(4) . . ?
C17 C12 C13 118.4(4) . . ?
C14 C13 S2 126.2(4) . . ?
C14 C13 C12 121.6(4) . . ?
C12 C13 S2 112.1(4) . . ?
C11 C6 C1 128.4(4) . . ?
C11 C6 C7 119.2(4) . . ?
C7 C6 C1 112.5(4) . . ?
C8 C9 C10 121.5(5) . . ?
C6 C7 S1 112.4(4) . . ?
C8 C7 S1 126.4(4) . . ?
C8 C7 C6 121.2(4) . . ?
C9 C8 C7 118.3(5) . . ?
C14 C15 C16 121.0(5) . . ?
C16 C17 C12 120.1(5) . . ?
C17 C16 C15 120.5(5) . . ?


_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 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.738
####################################################################### 
# 
# 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_3b-DMAD
_database_code_depnum_ccdc_archive 'CCDC 2385306'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-07-21
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H11 As O4 S2'
_chemical_formula_sum            'C15 H11 As O4 S2'
_chemical_formula_weight         394.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H10 N O'
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.4030(4)
_cell_length_b                   14.0494(5)
_cell_length_c                   10.7101(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.246(3)
_cell_angle_gamma                90
_cell_volume                     1545.01(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4592
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.7370
_cell_measurement_theta_min      2.9460
_shelx_estimated_absorpt_T_max   0.727
_shelx_estimated_absorpt_T_min   0.362
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_T_max  0.095
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             792
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0371
1 0 0 0.1003
0 -1 0 0.1111
0 1 0 0.0380
0 0 -1 0.2520
0 0 1 0.2330

_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.137
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0000 -0.0002 -0.0012 0.0525 0.0420 0.0158
1.0000 0.0002 0.0012 -0.0525 -0.0420 -0.0158
0.0011 -1.0005 -0.0006 0.0312 -0.0291 -0.0271
-0.0011 1.0005 0.0006 -0.0312 0.0291 0.0271
-0.0004 -0.0004 -1.0010 0.0212 -0.0298 0.0563
0.0004 0.0004 1.0010 -0.0212 0.0298 -0.0563

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.900
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  17.00   0.10    1.75    --   30.00  54.00 -90.00  360
  2  ω    -71.00 110.00   0.10    1.75    --   30.00  54.00 120.00 1810
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525057000
_diffrn_orient_matrix_UB_12      -0.0311893000
_diffrn_orient_matrix_UB_13      -0.0211359000
_diffrn_orient_matrix_UB_21      -0.0420297000
_diffrn_orient_matrix_UB_22      0.0289798000
_diffrn_orient_matrix_UB_23      0.0298236000
_diffrn_orient_matrix_UB_31      -0.0157886000
_diffrn_orient_matrix_UB_32      0.0270977000
_diffrn_orient_matrix_UB_33      -0.0562946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                2871
_reflns_number_total             3150
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.034
_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)+(0.0624P)²+0.2026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0931
_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:
 C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C8(H8), C7(H7)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C)
;
_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
As1 As 0.29231(2) 0.44049(2) 0.17372(2) 0.01763(11) Uani 1 1 d . . . . .
S1 S 0.63435(6) 0.25518(5) 0.27954(6) 0.02442(16) Uani 1 1 d . . . . .
S2 S 0.37517(6) 0.40608(5) 0.58807(5) 0.02223(16) Uani 1 1 d . . . . .
O4 O 0.09830(15) 0.13934(12) 0.25835(15) 0.0225(4) Uani 1 1 d . . . . .
O3 O 0.28625(17) 0.10542(12) 0.38622(16) 0.0248(4) Uani 1 1 d . . . . .
O2 O 0.09625(16) 0.23379(13) 0.01428(14) 0.0228(4) Uani 1 1 d . . . . .
O1 O -0.01886(16) 0.33317(14) 0.11899(16) 0.0285(4) Uani 1 1 d . . . . .
C10 C 0.2071(2) 0.31307(16) 0.1927(2) 0.0172(4) Uani 1 1 d . . . . .
C3 C 0.3910(2) 0.28902(17) 0.3690(2) 0.0189(5) Uani 1 1 d . . . . .
H3 H 0.425162 0.240263 0.433967 0.023 Uiso 1 1 calc R U . . .
C5 C 0.3126(2) 0.45803(17) 0.3570(2) 0.0189(5) Uani 1 1 d . . . . .
C1 C 0.4621(2) 0.37659(17) 0.1865(2) 0.0197(5) Uani 1 1 d . . . . .
C11 C 0.2637(2) 0.25606(16) 0.2855(2) 0.0170(4) Uani 1 1 d . . . . .
C14 C 0.2193(2) 0.15969(18) 0.31592(19) 0.0194(5) Uani 1 1 d . . . . .
C6 C 0.5643(2) 0.38513(18) 0.1132(2) 0.0227(5) Uani 1 1 d . . . . .
H6 H 0.563000 0.428314 0.044763 0.027 Uiso 1 1 calc R U . . .
C9 C 0.3138(2) 0.51848(18) 0.5587(2) 0.0242(5) Uani 1 1 d . . . . .
H9 H 0.301120 0.562390 0.623081 0.029 Uiso 1 1 calc R U . . .
C12 C 0.0824(2) 0.29452(17) 0.1072(2) 0.0198(5) Uani 1 1 d . . . . .
C4 C 0.3610(2) 0.38262(17) 0.4290(2) 0.0185(5) Uani 1 1 d . . . . .
C8 C 0.2851(2) 0.53794(18) 0.4315(2) 0.0217(5) Uani 1 1 d . . . . .
H8 H 0.251273 0.596892 0.397290 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4873(2) 0.31001(17) 0.2800(2) 0.0191(5) Uani 1 1 d . . . . .
C7 C 0.6647(2) 0.3238(2) 0.1531(2) 0.0277(6) Uani 1 1 d . . . . .
H7 H 0.741535 0.319339 0.116052 0.033 Uiso 1 1 calc R U . . .
C15 C 0.0540(3) 0.04422(19) 0.2842(3) 0.0310(6) Uani 1 1 d . . . . .
H15A H -0.031557 0.032663 0.233148 0.046 Uiso 1 1 calc R U . . .
H15B H 0.047247 0.038779 0.374113 0.046 Uiso 1 1 calc R U . . .
H15C H 0.116371 -0.002876 0.262632 0.046 Uiso 1 1 calc R U . . .
C13 C -0.0233(3) 0.2052(2) -0.0651(2) 0.0348(7) Uani 1 1 d . . . . .
H13A H -0.003358 0.160503 -0.129645 0.052 Uiso 1 1 calc R U . . .
H13B H -0.066910 0.261388 -0.106382 0.052 Uiso 1 1 calc R U . . .
H13C H -0.080592 0.174255 -0.013173 0.052 Uiso 1 1 calc R U . . .


_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
As1 C10 2.022(2) . ?
As1 C5 1.956(2) . ?
As1 C1 1.967(2) . ?
S1 C2 1.714(2) . ?
S1 C7 1.732(3) . ?
S2 C9 1.713(3) . ?
S2 C4 1.718(2) . ?
O4 C14 1.341(3) . ?
O4 C15 1.455(3) . ?
O3 C14 1.210(3) . ?
O2 C12 1.336(3) . ?
O2 C13 1.446(3) . ?
O1 C12 1.209(3) . ?
C10 C11 1.338(3) . ?
C10 C12 1.486(3) . ?
C3 C11 1.545(3) . ?
C3 C4 1.518(3) . ?
C3 C2 1.518(3) . ?
C5 C4 1.359(3) . ?
C5 C8 1.433(3) . ?
C1 C6 1.424(3) . ?
C1 C2 1.365(3) . ?
C11 C14 1.483(3) . ?
C6 C7 1.368(4) . ?
C9 C8 1.375(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
C5 As1 C10 89.39(9) . . ?
C5 As1 C1 92.10(10) . . ?
C1 As1 C10 89.55(9) . . ?
C2 S1 C7 91.57(12) . . ?
C9 S2 C4 91.43(12) . . ?
C14 O4 C15 114.29(19) . . ?
C12 O2 C13 115.5(2) . . ?
C11 C10 As1 117.20(16) . . ?
C11 C10 C12 126.1(2) . . ?
C12 C10 As1 116.55(16) . . ?
C4 C3 C11 106.83(18) . . ?
C4 C3 C2 107.37(19) . . ?
C2 C3 C11 106.60(17) . . ?
C4 C5 As1 116.24(18) . . ?
C4 C5 C8 112.6(2) . . ?
C8 C5 As1 131.19(19) . . ?
C6 C1 As1 131.69(18) . . ?
C2 C1 As1 115.33(17) . . ?
C2 C1 C6 113.0(2) . . ?
C10 C11 C3 119.0(2) . . ?
C10 C11 C14 126.5(2) . . ?
C14 C11 C3 114.49(19) . . ?
O4 C14 C11 113.33(19) . . ?
O3 C14 O4 123.8(2) . . ?
O3 C14 C11 122.9(2) . . ?
C7 C6 C1 112.0(2) . . ?
C8 C9 S2 112.36(19) . . ?
O2 C12 C10 112.49(19) . . ?
O1 C12 O2 124.4(2) . . ?
O1 C12 C10 123.1(2) . . ?
C3 C4 S2 126.54(17) . . ?
C5 C4 S2 112.22(18) . . ?
C5 C4 C3 121.2(2) . . ?
C9 C8 C5 111.4(2) . . ?
C3 C2 S1 126.45(17) . . ?
C1 C2 S1 111.81(18) . . ?
C1 C2 C3 121.7(2) . . ?
C6 C7 S1 111.66(18) . . ?


_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 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.479
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 2385301'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-03-29
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C9 H5 As S2)'
_chemical_formula_sum            'C9 H5 As S2'
_chemical_formula_weight         252.17
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHSAs
_chemical_oxdiff_usercomment     ' '
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'
As As 0.0499 2.0058 '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'

_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           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   6.1248(3)
_cell_length_b                   11.3296(6)
_cell_length_c                   12.9122(7)
_cell_angle_alpha                90
_cell_angle_beta                 95.535(6)
_cell_angle_gamma                90
_cell_volume                     891.82(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.8040
_cell_measurement_theta_min      3.1600
_shelx_estimated_absorpt_T_max   0.376
_shelx_estimated_absorpt_T_min   0.125
_exptl_absorpt_coefficient_mu    4.212
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.2813
0 -1 -1 0.2493
2 2 -1 0.1822
-2 -2 1 0.1065
1 -2 1 0.1878
-1 2 -1 0.2276

_exptl_crystal_size_max          0.848
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.289
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
0.0011 1.0018 0.9997 -0.0704 -0.0288 -0.0344
-0.0011 -1.0018 -0.9997 0.0704 0.0288 0.0344
2.0037 2.0018 -1.0038 -0.1211 0.2117 -0.1059
-2.0037 -2.0018 1.0038 0.1211 -0.2117 0.1059
1.0014 -2.0022 0.9995 -0.0512 0.0892 0.1517
-1.0014 2.0022 -0.9995 0.0512 -0.0892 -0.1517

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6527
_diffrn_reflns_point_group_measured_fraction_full 0.749
_diffrn_reflns_point_group_measured_fraction_max 0.729
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         3.170
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  -4.00   0.40    0.60    --   30.00  54.00  30.00  175
  2  ω    -48.00 112.00   0.40    0.60    --   30.00  54.00-180.00  400
  3  ω    -59.00  93.00   0.40    0.60    --   30.00  54.00 -90.00  380
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0573826000
_diffrn_orient_matrix_UB_12      -0.0255137000
_diffrn_orient_matrix_UB_13      -0.0448179000
_diffrn_orient_matrix_UB_21      0.1000903000
_diffrn_orient_matrix_UB_22      -0.0059346000
_diffrn_orient_matrix_UB_23      -0.0229354000
_diffrn_orient_matrix_UB_31      0.0152480000
_diffrn_orient_matrix_UB_32      -0.0568659000
_diffrn_orient_matrix_UB_33      0.0225795000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.455
_reflns_Friedel_fraction_full    0.497
_reflns_Friedel_fraction_max     0.457
_reflns_number_gt                2775
_reflns_number_total             2998
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         2998
_refine_ls_number_restraints     270
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      0.998
_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)+(0.0435P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0737
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.502(15)
 0.498(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 As1A-C1A \\sim As1B-C5B
 with sigma of 0.02
 C15A-C16A \\sim C17B-C18B
 with sigma of 0.02
 As1A-C5A \\sim As1B-C1B
 with sigma of 0.02
 C11A-C13A \\sim C13B-C11B
 with sigma of 0.02
 S2A-C2A \\sim S2B-C4B
 with sigma of 0.02
 C10A-C11A \\sim C14B-C13B
 with sigma of 0.02
 S2A-C7A \\sim S2B-C9B
 with sigma of 0.02
 C18A-C13A \\sim C16B-C11B
 with sigma of 0.02
 S1A-C4A \\sim S1B-C2B
 with sigma of 0.02
 S1A-C9A \\sim S1B-C7B
 with sigma of 0.02
 C17A-C13A \\sim C15B-C11B
 with sigma of 0.02
 C3A-C2A \\sim C3B-C4B
 with sigma of 0.02
 C3A-C4A \\sim C3B-C2B
 with sigma of 0.02
 S4A-C16A \\sim S4B-C18B
 with sigma of 0.02
 C8A-C5A \\sim C6B-C1B
 with sigma of 0.02
 C8A-C9A \\sim C6B-C7B
 with sigma of 0.02
 C6A-C1A \\sim C8B-C5B
 with sigma of 0.02
 As2A-C13A \\sim As2B-C11B
 with sigma of 0.02
 C6A-C7A \\sim C8B-C9B
 with sigma of 0.02
 C12A-S4A \\sim C12B-S4B
 with sigma of 0.02
 S3A-C14A \\sim S3B-C10B
 with sigma of 0.02
 C1A-C2A \\sim C5B-C4B
 with sigma of 0.02
 C5A-C4A \\sim C1B-C2B
 with sigma of 0.02
 C17A-C18A \\sim C15B-C16B
 with sigma of 0.02
 As2A-C17A \\sim As2B-C15B
 with sigma of 0.02
 As1A-C8A \\sim As1B-C6B
 with sigma of 0.02
 As1A-C6A \\sim As1B-C8B
 with sigma of 0.02
 As1A-C2A \\sim As1B-C4B
 with sigma of 0.02
 C12A-C14A \\sim C12B-C10B
 with sigma of 0.02
 As1A-C4A \\sim As1B-C2B
 with sigma of 0.02
 S4A-C15A \\sim S4B-C17B
 with sigma of 0.02
 S2A-C3A \\sim S2B-C3B
 with sigma of 0.02
 S2A-C6A \\sim S2B-C8B
 with sigma of 0.02
 S2A-C1A \\sim S2B-C5B
 with sigma of 0.02
 C10A-C16A \\sim C14B-C18B
 with sigma of 0.02
 S1A-C3A \\sim S1B-C3B
 with sigma of 0.02
 S1A-C8A \\sim S1B-C6B
 with sigma of 0.02
 S1A-C5A \\sim S1B-C1B
 with sigma of 0.02
 C15A-C10A \\sim C17B-C14B
 with sigma of 0.02
 C3A-C1A \\sim C3B-C5B
 with sigma of 0.02
 C3A-C5A \\sim C3B-C1B
 with sigma of 0.02
 C17A-C14A \\sim C15B-C10B
 with sigma of 0.02
 C8A-C4A \\sim C6B-C2B
 with sigma of 0.02
 C6A-C2A \\sim C8B-C4B
 with sigma of 0.02
 C14A-C13A \\sim C10B-C11B
 with sigma of 0.02
 As2A-C15A \\sim As2B-C17B
 with sigma of 0.02
 C1A-C5A \\sim C5B-C1B
 with sigma of 0.02
 As2A-C11A \\sim As2B-C13B
 with sigma of 0.02
 C1A-C7A \\sim C5B-C9B
 with sigma of 0.02
 C12A-S3A \\sim C12B-S3B
 with sigma of 0.02
 C2A-C4A \\sim C4B-C2B
 with sigma of 0.02
 C12A-C10A \\sim C12B-C14B
 with sigma of 0.02
 C2A-C7A \\sim C4B-C9B
 with sigma of 0.02
 S3A-C17A \\sim S3B-C15B
 with sigma of 0.02
 C5A-C9A \\sim C1B-C7B
 with sigma of 0.02
 S4A-C10A \\sim S4B-C14B
 with sigma of 0.02
 C15A-C11A \\sim C17B-C13B
 with sigma of 0.02
 C4A-C9A \\sim C2B-C7B
 with sigma of 0.02
 C18A-C14A \\sim C16B-C10B
 with sigma of 0.02
 C10A-C14A \\sim C14B-C10B
 with sigma of 0.02
 C11A-C16A \\sim C13B-C18B
 with sigma of 0.02
 As2A-C10A \\sim As2B-C14B
 with sigma of 0.02
 As2A-C14A \\sim As2B-C10B
 with sigma of 0.02
 C12A-C11A \\sim C12B-C13B
 with sigma of 0.02
 C12A-C13A \\sim C12B-C11B
 with sigma of 0.02
 S3A-C18A \\sim S3B-C16B
 with sigma of 0.02
 S3A-C13A \\sim S3B-C11B
 with sigma of 0.02
 S4A-C11A \\sim S4B-C13B
 with sigma of 0.02
4. Restrained planarity
 As2B, C14B, C10B, C17B, C13B, C15B, C11B, H17B, C18B, C12B, S4B, H15B, C16B,
 S3B, H18B, H12B, H16B
 with sigma of 0.1
 As1B, C5B, C1B, C8B, C4B, C6B, C2B, H8B, C9B, S2B, C3B, H6B, C7B, S1B, H9B,
 H3B, H7B
 with sigma of 0.1
5. Rigid body (RIGU) restrains
 As2A, C12A, S4A, C15A, C10A, C11A, C14A, C16A, C13A, S3A, C17A, C18A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 As2B, C12B, S4B, C17B, C14B, C13B, C10B, C11B, C18B, S3B, C15B, C16B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 As1B, S2B, S1B, C3B, C6B, C8B, C5B, C4B, C1B, C2B, C9B, C7B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 As1A, S2A, C3A, C6A, C1A, C2A, C5A, C4A, C7A, S1A, C8A, C9A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(As1B)=Sof(S2B)=Sof(S1B)=Sof(C3B)=Sof(H3B)=Sof(C6B)=Sof(H6B)=Sof(C8B)=
 Sof(H8B)=Sof(C5B)=Sof(C4B)=Sof(C1B)=Sof(C2B)=Sof(C7B)=Sof(H7B)=Sof(C9B)=
 Sof(H9B)=1-FVAR(1)
 Sof(As1A)=Sof(S2A)=Sof(S1A)=Sof(C3A)=Sof(H3A)=Sof(C8A)=Sof(H8A)=Sof(C6A)=
 Sof(H6A)=Sof(C1A)=Sof(C2A)=Sof(C5A)=Sof(C4A)=Sof(C9A)=Sof(H9A)=Sof(C7A)=
 Sof(H7A)=FVAR(1)
 Sof(As2B)=Sof(C12B)=Sof(H12B)=Sof(S3B)=Sof(S4B)=Sof(C17B)=Sof(H17B)=Sof(C15B)=
 Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C14B)=Sof(C13B)=Sof(C10B)=Sof(C11B)=
 Sof(C18B)=Sof(H18B)=1-FVAR(2)
 Sof(As2A)=Sof(C12A)=Sof(H12A)=Sof(S3A)=Sof(S4A)=Sof(C15A)=Sof(H15A)=Sof(C17A)=
 Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C10A)=Sof(C11A)=Sof(C14A)=Sof(C16A)=
 Sof(H16A)=Sof(C13A)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C12A(H12A), C3A(H3A), C15A(H15A), C17A(H17A), C8A(H8A), C6A(H6A), C18A(H18A),
 C16A(H16A), C9A(H9A), C7A(H7A), C3B(H3B), C6B(H6B), C8B(H8B), C7B(H7B),
 C9B(H9B), C12B(H12B), C17B(H17B), C15B(H15B), C16B(H16B), C18B(H18B)
;
_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
As1A As 1.21711(10) 0.90659(6) 0.31837(6) 0.01835(19) Uani 0.737(2) 1 d D . P A
1
As2A As 1.33821(11) 0.70627(6) 0.58626(6) 0.0194(2) Uani 0.699(2) 1 d D . P B 1
S2A S 0.8213(4) 0.94151(17) 0.58613(16) 0.0188(3) Uani 0.737(2) 1 d D . P A 1
C12A C 0.8863(16) 0.6067(7) 0.6731(7) 0.0266(15) Uani 0.699(2) 1 d D . P B 1
H12A H 0.757998 0.575626 0.698868 0.032 Uiso 0.699(2) 1 calc R U P B 1
S3A S 0.7786(5) 0.4695(2) 0.49763(19) 0.0233(5) Uani 0.699(2) 1 d D . P B 1
S1A S 0.6515(4) 0.67131(17) 0.23310(17) 0.0228(4) Uani 0.737(2) 1 d D . P A 1
S4A S 0.9341(4) 0.74169(19) 0.85084(16) 0.0229(4) Uani 0.699(2) 1 d D . P B 1
C3A C 0.7650(15) 0.8114(7) 0.4053(6) 0.0280(15) Uani 0.737(2) 1 d D . P A 1
H3A H 0.634633 0.783140 0.431134 0.034 Uiso 0.737(2) 1 calc R U P A 1
C15A C 1.2908(16) 0.8204(8) 0.7875(8) 0.0261(19) Uani 0.699(2) 1 d D . P B 1
H15A H 1.422240 0.863720 0.782663 0.031 Uiso 0.699(2) 1 calc R U P B 1
C17A C 1.134(2) 0.5437(9) 0.4281(8) 0.023(2) Uani 0.699(2) 1 d D . P B 1
H17A H 1.247765 0.554984 0.384176 0.028 Uiso 0.699(2) 1 calc R U P B 1
C8A C 1.0051(16) 0.7428(7) 0.1621(7) 0.0241(18) Uani 0.737(2) 1 d D . P A 1
H8A H 1.117385 0.754626 0.117294 0.029 Uiso 0.737(2) 1 calc R U P A 1
C6A C 1.1729(18) 1.0197(8) 0.5217(8) 0.027(2) Uani 0.737(2) 1 d D . P A 1
H6A H 1.304104 1.063484 0.517682 0.032 Uiso 0.737(2) 1 calc R U P A 1
C1A C 1.0859(19) 0.9408(12) 0.4403(12) 0.018(3) Uani 0.737(2) 1 d D . P A 1
C18A C 0.960(4) 0.4718(15) 0.4038(12) 0.028(5) Uani 0.699(2) 1 d D . P B 1
H18A H 0.939806 0.427170 0.341378 0.033 Uiso 0.699(2) 1 calc R U P B 1
C10A C 1.207(2) 0.7381(12) 0.7075(13) 0.018(3) Uani 0.699(2) 1 d D . P B 1
C2A C 0.8883(16) 0.8895(9) 0.4652(10) 0.019(3) Uani 0.737(2) 1 d D . P A 1
C11A C 1.0073(17) 0.6867(11) 0.7319(12) 0.019(3) Uani 0.699(2) 1 d D . P B 1
C14A C 1.1279(19) 0.6010(12) 0.5266(12) 0.019(3) Uani 0.699(2) 1 d D . P B 1
C5A C 1.0018(19) 0.8013(12) 0.2615(11) 0.019(3) Uani 0.737(2) 1 d D . P A 1
C16A C 1.179(4) 0.8311(15) 0.8640(11) 0.032(3) Uani 0.699(2) 1 d D . P B 1
H16A H 1.218947 0.880768 0.921996 0.039 Uiso 0.699(2) 1 calc R U P B 1
C4A C 0.8136(16) 0.7702(9) 0.3107(12) 0.019(3) Uani 0.737(2) 1 d D . P A 1
C9A C 0.836(3) 0.6708(13) 0.1394(10) 0.029(5) Uani 0.737(2) 1 d D . P A 1
H9A H 0.817420 0.623934 0.078194 0.035 Uiso 0.737(2) 1 calc R U P A 1
C7A C 1.058(3) 1.0264(13) 0.6012(10) 0.028(4) Uani 0.737(2) 1 d D . P A 1
H7A H 1.099271 1.072831 0.661134 0.034 Uiso 0.737(2) 1 calc R U P A 1
C13A C 0.9414(18) 0.5684(9) 0.5771(10) 0.021(2) Uani 0.699(2) 1 d D . P B 1
As1B As 0.6718(4) 0.7938(2) 0.41713(19) 0.0244(7) Uiso 0.263(2) 1 d D . P A 2
S2B S 1.2296(12) 1.0301(7) 0.5064(6) 0.0251(18) Uiso 0.263(2) 1 d D . P A 2
S1B S 1.0729(12) 0.7573(7) 0.1537(6) 0.0280(18) Uiso 0.263(2) 1 d D . P A 2
C3B C 1.125(4) 0.892(2) 0.3328(15) 0.057(11) Uiso 0.263(2) 1 d D . P A 2
H3B H 1.255286 0.921714 0.307587 0.069 Uiso 0.263(2) 1 calc R U P A 2
C6B C 0.714(3) 0.681(2) 0.2146(16) 0.037(10) Uiso 0.263(2) 1 d D . P A 2
H6B H 0.581184 0.638500 0.217644 0.044 Uiso 0.263(2) 1 calc R U P A 2
C8B C 0.879(4) 0.960(2) 0.5735(17) 0.066(16) Uiso 0.263(2) 1 d D . P A 2
H8B H 0.764171 0.948692 0.616799 0.079 Uiso 0.263(2) 1 calc R U P A 2
C5B C 0.884(3) 0.8999(14) 0.4749(18) 0.016(9) Uiso 0.263(2) 1 d D . P A 2
C4B C 1.074(4) 0.931(3) 0.4269(19) 0.017(11) Uiso 0.263(2) 1 d D . P A 2
C1B C 0.802(4) 0.7611(16) 0.2959(14) 0.024(12) Uiso 0.263(2) 1 d D . P A 2
C2B C 1.002(5) 0.813(3) 0.272(2) 0.017(11) Uiso 0.263(2) 1 d D . P A 2
C7B C 0.837(6) 0.672(3) 0.136(2) 0.020(12) Uiso 0.263(2) 1 d D . P A 2
H7B H 0.799659 0.624992 0.076278 0.024 Uiso 0.263(2) 1 calc R U P A 2
C9B C 1.043(6) 1.030(3) 0.599(2) 0.016(10) Uiso 0.263(2) 1 d D . P A 2
H9B H 1.059063 1.075211 0.660841 0.020 Uiso 0.263(2) 1 calc R U P A 2
As2B As 0.7930(3) 0.59262(18) 0.68590(16) 0.0249(6) Uiso 0.301(2) 1 d D . P B 2
C12B C 1.248(3) 0.6910(16) 0.5999(13) 0.040(7) Uiso 0.301(2) 1 d D . P B 2
H12B H 1.379048 0.719397 0.574497 0.047 Uiso 0.301(2) 1 calc R U P B 2
S3B S 1.1869(12) 0.5593(7) 0.4189(6) 0.0282(18) Uiso 0.301(2) 1 d D . P B 2
S4B S 1.3567(10) 0.8282(6) 0.7721(5) 0.0280(16) Uiso 0.301(2) 1 d D . P B 2
C17B C 1.001(3) 0.7560(17) 0.8433(15) 0.029(8) Uiso 0.301(2) 1 d D . P B 2
H17B H 0.886575 0.743315 0.886463 0.035 Uiso 0.301(2) 1 calc R U P B 2
C15B C 0.830(3) 0.481(2) 0.4831(16) 0.043(12) Uiso 0.301(2) 1 d D . P B 2
H15B H 0.696773 0.438570 0.485929 0.052 Uiso 0.301(2) 1 calc R U P B 2
C16B C 0.955(7) 0.474(3) 0.402(2) 0.021(11) Uiso 0.301(2) 1 d D . P B 2
H16B H 0.918884 0.425710 0.342734 0.025 Uiso 0.301(2) 1 calc R U P B 2
C14B C 1.006(3) 0.6975(14) 0.7431(18) 0.022(10) Uiso 0.301(2) 1 d D . P B 2
C13B C 1.195(4) 0.730(3) 0.6935(19) 0.022(11) Uiso 0.301(2) 1 d D . P B 2
C10B C 0.918(3) 0.5594(14) 0.5635(13) 0.011(6) Uiso 0.301(2) 1 d D . P B 2
C11B C 1.119(4) 0.611(3) 0.5398(18) 0.018(9) Uiso 0.301(2) 1 d D . P B 2
C18B C 1.158(6) 0.824(3) 0.8688(17) 0.015(7) Uiso 0.301(2) 1 d D . P B 2
H18B H 1.171922 0.868358 0.931432 0.019 Uiso 0.301(2) 1 calc R U P B 2


_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
As1A C1A 1.875(13) . ?
As1A C5A 1.874(13) . ?
As2A C10A 1.863(15) . ?
As2A C14A 1.867(13) . ?
S2A C2A 1.754(14) . ?
S2A C7A 1.734(19) . ?
C12A C11A 1.356(18) . ?
C12A C13A 1.386(15) . ?
S3A C18A 1.72(2) . ?
S3A C13A 1.762(13) . ?
S1A C4A 1.747(15) . ?
S1A C9A 1.731(19) . ?
S4A C11A 1.755(17) . ?
S4A C16A 1.80(2) . ?
C3A C2A 1.356(15) . ?
C3A C4A 1.367(17) . ?
C15A C10A 1.45(2) . ?
C15A C16A 1.26(2) . ?
C17A C18A 1.35(2) . ?
C17A C14A 1.432(18) . ?
C8A C5A 1.447(17) . ?
C8A C9A 1.33(2) . ?
C6A C1A 1.443(18) . ?
C6A C7A 1.30(2) . ?
C1A C2A 1.408(9) . ?
C10A C11A 1.416(10) . ?
C14A C13A 1.418(11) . ?
C5A C4A 1.414(9) . ?
As1B C5B 1.87(2) . ?
As1B C1B 1.86(2) . ?
S2B C4B 1.74(2) . ?
S2B C9B 1.73(3) . ?
S1B C2B 1.74(2) . ?
S1B C7B 1.73(4) . ?
C3B C4B 1.36(2) . ?
C3B C2B 1.37(2) . ?
C6B C1B 1.45(2) . ?
C6B C7B 1.32(3) . ?
C8B C5B 1.45(3) . ?
C8B C9B 1.29(3) . ?
C5B C4B 1.415(17) . ?
C1B C2B 1.418(17) . ?
As2B C14B 1.86(2) . ?
As2B C10B 1.859(19) . ?
C12B C13B 1.36(2) . ?
C12B C11B 1.39(2) . ?
S3B C16B 1.72(4) . ?
S3B C11B 1.754(19) . ?
S4B C13B 1.75(2) . ?
S4B C18B 1.83(3) . ?
C17B C14B 1.46(3) . ?
C17B C18B 1.25(3) . ?
C15B C16B 1.36(4) . ?
C15B C10B 1.43(2) . ?
C14B C13B 1.423(16) . ?
C10B C11B 1.425(16) . ?

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
C5A As1A C1A 96.8(6) . . ?
C10A As2A C14A 97.7(7) . . ?
C7A S2A C2A 91.2(6) . . ?
C11A C12A C13A 122.9(11) . . ?
C18A S3A C13A 91.9(7) . . ?
C9A S1A C4A 91.8(6) . . ?
C11A S4A C16A 90.1(6) . . ?
C2A C3A C4A 125.1(10) . . ?
C16A C15A C10A 116.0(11) . . ?
C18A C17A C14A 113.1(13) . . ?
C9A C8A C5A 113.5(11) . . ?
C7A C6A C1A 114.9(11) . . ?
C6A C1A As1A 125.6(8) . . ?
C2A C1A As1A 123.6(15) . . ?
C2A C1A C6A 110.7(13) . . ?
C17A C18A S3A 113.2(7) . . ?
C15A C10A As2A 124.9(9) . . ?
C11A C10A As2A 124.0(17) . . ?
C11A C10A C15A 111.2(16) . . ?
C3A C2A S2A 124.2(8) . . ?
C3A C2A C1A 125.7(15) . . ?
C1A C2A S2A 110.2(13) . . ?
C12A C11A S4A 123.7(9) . . ?
C12A C11A C10A 126.0(18) . . ?
C10A C11A S4A 110.3(16) . . ?
C17A C14A As2A 125.5(9) . . ?
C13A C14A As2A 122.1(14) . . ?
C13A C14A C17A 112.4(13) . . ?
C8A C5A As1A 124.7(8) . . ?
C4A C5A As1A 123.8(15) . . ?
C4A C5A C8A 111.5(14) . . ?
C15A C16A S4A 112.5(8) . . ?
C3A C4A S1A 124.8(8) . . ?
C3A C4A C5A 125.0(16) . . ?
C5A C4A S1A 110.2(14) . . ?
C8A C9A S1A 113.0(7) . . ?
C6A C7A S2A 112.9(7) . . ?
C12A C13A S3A 123.2(9) . . ?
C12A C13A C14A 127.3(14) . . ?
C14A C13A S3A 109.5(12) . . ?
C1B As1B C5B 97.2(11) . . ?
C9B S2B C4B 92.5(11) . . ?
C7B S1B C2B 92.3(11) . . ?
C4B C3B C2B 124.5(18) . . ?
C7B C6B C1B 113.6(17) . . ?
C9B C8B C5B 115.4(19) . . ?
C8B C5B As1B 125.6(17) . . ?
C4B C5B As1B 124(2) . . ?
C4B C5B C8B 110.7(19) . . ?
C3B C4B S2B 125.2(17) . . ?
C3B C4B C5B 125(2) . . ?
C5B C4B S2B 109.4(18) . . ?
C6B C1B As1B 124.9(16) . . ?
C2B C1B As1B 124(2) . . ?
C2B C1B C6B 111.5(19) . . ?
C3B C2B S1B 124.8(16) . . ?
C3B C2B C1B 125(2) . . ?
C1B C2B S1B 109.7(18) . . ?
C6B C7B S1B 112.8(12) . . ?
C8B C9B S2B 112.0(13) . . ?
C10B As2B C14B 97.8(11) . . ?
C13B C12B C11B 122.5(17) . . ?
C16B S3B C11B 92.1(11) . . ?
C13B S4B C18B 90.1(10) . . ?
C18B C17B C14B 115.8(18) . . ?
C16B C15B C10B 113.2(19) . . ?
C15B C16B S3B 113.1(12) . . ?
C17B C14B As2B 124.7(16) . . ?
C13B C14B As2B 124(2) . . ?
C13B C14B C17B 112(2) . . ?
C12B C13B S4B 123.5(16) . . ?
C12B C13B C14B 126(2) . . ?
C14B C13B S4B 110.1(19) . . ?
C15B C10B As2B 125.8(15) . . ?
C11B C10B As2B 122.4(17) . . ?
C11B C10B C15B 111.8(18) . . ?
C12B C11B S3B 123.0(15) . . ?
C12B C11B C10B 127.3(19) . . ?
C10B C11B S3B 109.7(17) . . ?
C17B C18B S4B 112.4(12) . . ?


_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 1.401
_oxdiff_exptl_absorpt_empirical_full_min 0.721
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.502(15)
2 0.498(15)

####################################################################### 
# 
# 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_3a-W(CO)5
_database_code_depnum_ccdc_archive 'CCDC 2385309'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-04-10
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H5 As O5 S2 W'
_chemical_formula_sum            'C14 H5 As O5 S2 W'
_chemical_formula_weight         576.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H5O5AsS2W
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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                   7.3120(5)
_cell_length_b                   10.1653(8)
_cell_length_c                   11.2954(8)
_cell_angle_alpha                92.355(6)
_cell_angle_beta                 106.909(6)
_cell_angle_gamma                100.480(6)
_cell_volume                     785.92(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2534
_cell_measurement_temperature    256.00
_cell_measurement_theta_max      32.7370
_cell_measurement_theta_min      3.1370
_shelx_estimated_absorpt_T_max   0.323
_shelx_estimated_absorpt_T_min   0.039
_exptl_absorpt_coefficient_mu    9.724
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1794
0 0 -1 0.2688
0 1 0 0.0629
0 -1 0 0.0835
-1 1 0 0.2156
1 -1 0 0.4137

_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.15
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
-0.0006 0.0014 0.9983 0.0647 0.0012 0.0120
0.0006 -0.0014 -0.9983 -0.0647 -0.0012 -0.0120
0.0018 0.9958 -0.0001 0.0017 0.0669 0.0238
-0.0018 -0.9958 0.0001 -0.0017 -0.0669 -0.0238
-0.9951 0.9947 0.0014 -0.0436 0.0176 0.1023
0.9951 -0.9947 -0.0014 0.0436 -0.0176 -0.1023

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4555
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.925
_diffrn_ambient_temperature      256.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00 -48.00   0.10    0.50    --   30.00  54.00 -90.00  250
  2  ω      5.00  32.00   0.10    0.50    --   30.00  54.00 -90.00  270
  3  ω    -70.00  31.00   0.10    0.50    --   30.00  54.00 150.00 1010
  4  ω    -74.00 110.00   0.10    0.50    --   30.00  54.00  30.00 1840
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0455688000
_diffrn_orient_matrix_UB_12      0.0016118000
_diffrn_orient_matrix_UB_13      0.0648637000
_diffrn_orient_matrix_UB_21      0.0494456000
_diffrn_orient_matrix_UB_22      0.0671154000
_diffrn_orient_matrix_UB_23      0.0011660000
_diffrn_orient_matrix_UB_31      -0.0787330000
_diffrn_orient_matrix_UB_32      0.0240645000
_diffrn_orient_matrix_UB_33      0.0119345000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                2385
_reflns_number_total             3210
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         6.699
_refine_diff_density_min         -5.056
_refine_diff_density_rms         0.533
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0985
_refine_ls_restrained_S_all      1.104
_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)+(0.1871P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2985
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C009 \\sim O007: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O008 \\sim C00B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C00D \\sim O006: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00N(H00N)
;
_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
W001 W 0.70010(10) 0.20133(7) 0.77907(7) 0.0308(4) Uani 1 1 d . . . . .
S003 S 0.5397(8) 0.2435(6) 0.3670(5) 0.0381(11) Uani 1 1 d . . . . .
S004 S 0.9273(7) 0.6440(6) 0.8256(5) 0.0412(12) Uani 1 1 d . . . . .
O005 O 0.237(2) 0.0962(15) 0.6901(16) 0.043(4) Uani 1 1 d . . . . .
O006 O 1.164(2) 0.2903(16) 0.8920(15) 0.042(3) Uani 1 1 d . U . . .
O007 O 0.756(2) 0.0227(14) 0.5593(14) 0.037(3) Uani 1 1 d . U . . .
O008 O 0.629(2) 0.4010(16) 0.9745(12) 0.039(3) Uani 1 1 d . U . . .
C009 C 0.727(3) 0.0832(18) 0.634(2) 0.034(3) Uani 1 1 d . U . . .
O00A O 0.723(3) -0.0298(17) 0.9505(18) 0.058(5) Uani 1 1 d . . . . .
C00B C 0.663(3) 0.330(2) 0.9156(19) 0.038(3) Uani 1 1 d . U . . .
C00C C 0.401(3) 0.1351(18) 0.719(2) 0.033(4) Uani 1 1 d . . . . .
C00D C 0.995(3) 0.263(2) 0.851(2) 0.041(3) Uani 1 1 d . U . . .
C00E C 0.662(3) 0.379(2) 0.467(2) 0.038(5) Uani 1 1 d . . . . .
C00F C 0.883(3) 0.657(2) 0.590(2) 0.045(5) Uani 1 1 d . . . . .
C00G C 0.827(3) 0.618(2) 0.464(2) 0.038(5) Uani 1 1 d . . . . .
H00G H 0.859687 0.682976 0.413428 0.045 Uiso 1 1 calc R U . . .
C00H C 0.991(3) 0.786(2) 0.655(2) 0.044(5) Uani 1 1 d . . . . .
H00H H 1.035758 0.857447 0.614664 0.053 Uiso 1 1 calc R U . . .
C00I C 0.710(3) 0.052(3) 0.888(2) 0.050(7) Uani 1 1 d . . . . .
C00J C 0.725(3) 0.492(2) 0.404(2) 0.040(5) Uani 1 1 d . . . . .
C00K C 0.568(3) 0.325(2) 0.241(2) 0.043(5) Uani 1 1 d . . . . .
H00K H 0.525033 0.283582 0.160334 0.052 Uiso 1 1 calc R U . . .
C00L C 0.655(3) 0.449(2) 0.270(2) 0.038(5) Uani 1 1 d . . . . .
H00L H 0.672906 0.507285 0.211044 0.046 Uiso 1 1 calc R U . . .
C00M C 0.842(3) 0.566(2) 0.677(2) 0.037(5) Uani 1 1 d . . . . .
C00N C 1.018(3) 0.793(2) 0.774(2) 0.039(5) Uani 1 1 d . . . . .
H00N H 1.081466 0.870831 0.826684 0.047 Uiso 1 1 calc R U . . .
As As 0.7062(3) 0.3928(2) 0.6380(2) 0.0357(6) 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
W001 C009 2.07(2) . ?
W001 C00B 2.09(2) . ?
W001 C00C 2.07(2) . ?
W001 C00D 2.04(2) . ?
W001 C00I 1.98(3) . ?
W001 As 2.568(2) . ?
S003 C00E 1.68(2) . ?
S003 C00K 1.72(2) . ?
S004 C00M 1.71(2) . ?
S004 C00N 1.74(2) . ?
O005 C00C 1.13(3) . ?
O006 C00D 1.16(3) . ?
O007 C009 1.11(2) . ?
O008 C00B 1.07(2) . ?
O00A C00I 1.12(3) . ?
C00E C00J 1.44(3) . ?
C00E As 1.86(2) . ?
C00F C00G 1.38(3) . ?
C00F C00H 1.44(3) . ?
C00F C00M 1.43(3) . ?
C00G C00J 1.40(3) . ?
C00H C00N 1.30(3) . ?
C00J C00L 1.47(3) . ?
C00K C00L 1.29(3) . ?
C00M As 1.83(2) . ?

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
C009 W001 C00B 175.6(7) . . ?
C009 W001 As 85.8(5) . . ?
C00B W001 As 90.3(6) . . ?
C00C W001 C009 90.6(8) . . ?
C00C W001 C00B 87.8(8) . . ?
C00C W001 As 95.8(5) . . ?
C00D W001 C009 92.0(8) . . ?
C00D W001 C00B 89.8(9) . . ?
C00D W001 C00C 175.9(8) . . ?
C00D W001 As 87.6(7) . . ?
C00I W001 C009 92.6(8) . . ?
C00I W001 C00B 91.4(8) . . ?
C00I W001 C00C 87.0(9) . . ?
C00I W001 C00D 89.7(10) . . ?
C00I W001 As 176.7(6) . . ?
C00E S003 C00K 92.3(11) . . ?
C00M S004 C00N 91.1(11) . . ?
O007 C009 W001 174.9(19) . . ?
O008 C00B W001 171.5(18) . . ?
O005 C00C W001 177.1(19) . . ?
O006 C00D W001 175.9(19) . . ?
S003 C00E As 126.0(12) . . ?
C00J C00E S003 112.1(16) . . ?
C00J C00E As 121.9(17) . . ?
C00G C00F C00H 128(2) . . ?
C00G C00F C00M 122(2) . . ?
C00M C00F C00H 110(2) . . ?
C00F C00G C00J 126(2) . . ?
C00N C00H C00F 114(2) . . ?
O00A C00I W001 177(2) . . ?
C00E C00J C00L 108(2) . . ?
C00G C00J C00E 125(2) . . ?
C00G C00J C00L 127.6(18) . . ?
C00L C00K S003 113.3(18) . . ?
C00K C00L C00J 114.4(19) . . ?
S004 C00M As 123.1(12) . . ?
C00F C00M S004 111.1(17) . . ?
C00F C00M As 125.7(18) . . ?
C00H C00N S004 114.1(19) . . ?
C00E As W001 127.9(6) . . ?
C00M As W001 128.9(7) . . ?
C00M As C00E 99.3(10) . . ?


_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 2.306
_oxdiff_exptl_absorpt_empirical_full_min 0.343
####################################################################### 
# 
# 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_3c-benzyne
_database_code_depnum_ccdc_archive 'CCDC 2385308'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-06-23
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H13 As S2'
_chemical_formula_sum            'C23 H13 As S2'
_chemical_formula_weight         428.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHAsS
_chemical_oxdiff_usercomment     ' '
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'
As As 0.0499 2.0058 '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'

_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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   16.1897(5)
_cell_length_b                   7.1373(3)
_cell_length_c                   31.4478(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.732(3)
_cell_angle_gamma                90
_cell_volume                     3633.5(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.8100
_cell_measurement_theta_min      2.8810
_shelx_estimated_absorpt_T_max   0.743
_shelx_estimated_absorpt_T_min   0.396
_exptl_absorpt_coefficient_mu    2.104
_exptl_absorpt_correction_T_max  0.122
_exptl_absorpt_correction_T_min  0.015
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 1 0.1514
-2 0 -1 0.1277
0 -2 1 0.2824
0 2 -1 0.2370
0 0 1 0.0781
0 0 -1 0.0716

_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
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
1.9989 0.0001 1.0016 0.0830 0.0210 -0.0299
-1.9989 -0.0001 -1.0016 -0.0830 -0.0210 0.0299
-0.0015 -1.9997 0.9981 0.0670 0.0246 0.1870
0.0015 1.9997 -0.9981 -0.0670 -0.0246 -0.1870
-0.0005 0.0001 1.0001 0.0006 0.0225 -0.0005
0.0005 -0.0001 -1.0001 -0.0006 -0.0225 0.0005

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            8410
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.591
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 114.00   0.10    1.75    --   30.00  54.00-180.00 1820
  2  ω     41.00  79.00   0.10    1.75    --   30.00  54.00  90.00  380
  3  ω    -17.00  19.00   0.10    1.75    --   30.00  54.00 120.00  360
  4  ω     41.00  66.00   0.10    1.75    --   30.00  54.00  30.00  250
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0412406000
_diffrn_orient_matrix_UB_12      -0.0332215000
_diffrn_orient_matrix_UB_13      0.0006042000
_diffrn_orient_matrix_UB_21      -0.0008111000
_diffrn_orient_matrix_UB_22      -0.0010570000
_diffrn_orient_matrix_UB_23      0.0225387000
_diffrn_orient_matrix_UB_31      -0.0146949000
_diffrn_orient_matrix_UB_32      -0.0937458000
_diffrn_orient_matrix_UB_33      -0.0004696000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                3540
_reflns_number_total             3705
_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 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3705
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0345
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+7.1908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0919
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C8, C1, C7, C4, C6, C5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C23(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C19(H19), C20(H20), C15(H15), C7(H7), C4(H4), C14(H14),
 C12(H12), C13(H13), C6(H6), C5(H5)
;
_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
As1 As 0.31432(2) 0.72264(4) 0.65793(2) 0.02663(11) Uani 1 1 d . . . . .
S2 S 0.19966(4) 0.55330(9) 0.73578(2) 0.02241(15) Uani 1 1 d . . . . .
S1 S 0.21471(4) 0.85504(9) 0.56959(2) 0.02960(16) Uani 1 1 d . . . . .
C22 C 0.13722(14) 0.0813(3) 0.67808(7) 0.0200(5) Uani 1 1 d . . . . .
H22 H 0.148601 0.025962 0.651313 0.024 Uiso 1 1 calc R U . . .
C17 C 0.17173(13) 0.2563(3) 0.68890(7) 0.0178(5) Uani 1 1 d . . . . .
C16 C 0.22392(13) 0.3789(3) 0.66506(7) 0.0179(4) Uani 1 1 d . . . . .
C9 C 0.23118(14) 0.5101(3) 0.59267(7) 0.0193(5) Uani 1 1 d . . . . .
C3 C 0.24295(14) 0.5403(3) 0.68586(7) 0.0213(5) Uani 1 1 d . . . . .
C23 C 0.25863(13) 0.3479(3) 0.62086(7) 0.0180(4) Uani 1 1 d . . . . .
H23 H 0.239465 0.225505 0.608804 0.022 Uiso 1 1 calc R U . . .
C18 C 0.15326(13) 0.3344(3) 0.72903(7) 0.0191(4) Uani 1 1 d . . . . .
C21 C 0.08670(14) -0.0095(4) 0.70658(8) 0.0235(5) Uani 1 1 d . . . . .
H21 H 0.063096 -0.127041 0.699159 0.028 Uiso 1 1 calc R U . . .
C19 C 0.10290(14) 0.2421(4) 0.75817(8) 0.0215(5) Uani 1 1 d . . . . .
H19 H 0.091713 0.295552 0.785151 0.026 Uiso 1 1 calc R U . . .
C20 C 0.06984(14) 0.0703(4) 0.74650(8) 0.0237(5) Uani 1 1 d . . . . .
H20 H 0.035257 0.005381 0.765719 0.028 Uiso 1 1 calc R U . . .
C10 C 0.18450(14) 0.5022(4) 0.55352(7) 0.0213(5) Uani 1 1 d . . . . .
C8 C 0.35318(14) 0.3543(4) 0.62421(7) 0.0225(5) Uani 1 1 d . . . . .
C15 C 0.15312(15) 0.3474(4) 0.53130(8) 0.0249(5) Uani 1 1 d . . . . .
H15 H 0.162125 0.224195 0.541802 0.030 Uiso 1 1 calc R U . . .
C2 C 0.25063(16) 0.6877(4) 0.60502(8) 0.0240(5) Uani 1 1 d . . . . .
C1 C 0.38872(15) 0.5180(4) 0.64054(7) 0.0267(5) Uani 1 1 d . . . . .
C7 C 0.40281(15) 0.2069(4) 0.61140(8) 0.0278(5) Uani 1 1 d . . . . .
H7 H 0.378503 0.095192 0.600625 0.033 Uiso 1 1 calc R U . . .
C4 C 0.47513(15) 0.5373(5) 0.64333(8) 0.0310(6) Uani 1 1 d . . . . .
H4 H 0.499710 0.649843 0.653514 0.037 Uiso 1 1 calc R U . . .
C11 C 0.17041(16) 0.6839(4) 0.53701(8) 0.0268(5) Uani 1 1 d . . . . .
C14 C 0.10888(16) 0.3753(4) 0.49392(8) 0.0314(6) Uani 1 1 d . . . . .
H14 H 0.087298 0.270467 0.478827 0.038 Uiso 1 1 calc R U . . .
C12 C 0.12559(17) 0.7117(4) 0.49919(9) 0.0324(6) Uani 1 1 d . . . . .
H12 H 0.116131 0.834211 0.488398 0.039 Uiso 1 1 calc R U . . .
C13 C 0.09555(16) 0.5565(5) 0.47804(8) 0.0347(6) Uani 1 1 d . . . . .
H13 H 0.065241 0.572579 0.452234 0.042 Uiso 1 1 calc R U . . .
C6 C 0.48893(17) 0.2234(5) 0.61442(9) 0.0388(7) Uani 1 1 d . . . . .
H6 H 0.523167 0.123341 0.605340 0.047 Uiso 1 1 calc R U . . .
C5 C 0.52394(16) 0.3850(5) 0.63057(9) 0.0416(7) Uani 1 1 d . . . . .
H5 H 0.582353 0.393496 0.633137 0.050 Uiso 1 1 calc R U . . .


_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
As1 C3 1.956(2) . ?
As1 C2 1.962(2) . ?
As1 C1 1.975(3) . ?
S2 C3 1.730(2) . ?
S2 C18 1.746(3) . ?
S1 C2 1.729(3) . ?
S1 C11 1.743(3) . ?
C22 C17 1.408(3) . ?
C22 C21 1.383(3) . ?
C17 C16 1.434(3) . ?
C17 C18 1.415(3) . ?
C16 C3 1.358(3) . ?
C16 C23 1.522(3) . ?
C9 C23 1.521(3) . ?
C9 C10 1.438(3) . ?
C9 C2 1.362(4) . ?
C23 C8 1.534(3) . ?
C18 C19 1.399(3) . ?
C21 C20 1.408(3) . ?
C19 C20 1.385(4) . ?
C10 C15 1.399(4) . ?
C10 C11 1.414(4) . ?
C8 C1 1.397(4) . ?
C8 C7 1.387(4) . ?
C15 C14 1.383(3) . ?
C1 C4 1.407(3) . ?
C7 C6 1.401(4) . ?
C4 C5 1.406(5) . ?
C11 C12 1.399(4) . ?
C14 C13 1.402(4) . ?
C12 C13 1.377(4) . ?
C6 C5 1.379(5) . ?

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
C3 As1 C2 89.39(10) . . ?
C3 As1 C1 89.91(10) . . ?
C2 As1 C1 89.26(10) . . ?
C3 S2 C18 91.17(11) . . ?
C2 S1 C11 91.57(13) . . ?
C21 C22 C17 119.7(2) . . ?
C22 C17 C16 130.5(2) . . ?
C22 C17 C18 118.5(2) . . ?
C18 C17 C16 111.0(2) . . ?
C17 C16 C23 128.0(2) . . ?
C3 C16 C17 113.4(2) . . ?
C3 C16 C23 118.6(2) . . ?
C10 C9 C23 128.0(2) . . ?
C2 C9 C23 118.5(2) . . ?
C2 C9 C10 113.4(2) . . ?
S2 C3 As1 128.35(14) . . ?
C16 C3 As1 118.67(17) . . ?
C16 C3 S2 112.98(18) . . ?
C16 C23 C8 108.23(18) . . ?
C9 C23 C16 108.23(19) . . ?
C9 C23 C8 107.52(18) . . ?
C17 C18 S2 111.43(17) . . ?
C19 C18 S2 126.54(19) . . ?
C19 C18 C17 122.0(2) . . ?
C22 C21 C20 120.8(2) . . ?
C20 C19 C18 118.0(2) . . ?
C19 C20 C21 121.0(2) . . ?
C15 C10 C9 130.0(2) . . ?
C15 C10 C11 119.0(2) . . ?
C11 C10 C9 111.0(2) . . ?
C1 C8 C23 117.2(2) . . ?
C7 C8 C23 122.6(2) . . ?
C7 C8 C1 120.3(2) . . ?
C14 C15 C10 119.5(3) . . ?
S1 C2 As1 128.88(15) . . ?
C9 C2 As1 118.49(18) . . ?
C9 C2 S1 112.62(18) . . ?
C8 C1 As1 118.06(18) . . ?
C8 C1 C4 120.6(3) . . ?
C4 C1 As1 121.3(2) . . ?
C8 C7 C6 119.8(3) . . ?
C5 C4 C1 117.9(3) . . ?
C10 C11 S1 111.32(18) . . ?
C12 C11 S1 127.3(2) . . ?
C12 C11 C10 121.4(3) . . ?
C15 C14 C13 120.7(3) . . ?
C13 C12 C11 118.2(3) . . ?
C12 C13 C14 121.2(2) . . ?
C5 C6 C7 119.9(3) . . ?
C6 C5 C4 121.5(2) . . ?


_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 1.826
_oxdiff_exptl_absorpt_empirical_full_min 0.510
####################################################################### 
# 
# 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_3c-DMAD
_database_code_depnum_ccdc_archive 'CCDC 2385307'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Imoto'
;Kyoto Institute of Technology
Japan
;
_audit_update_record             
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_audit_creation_date             2024-06-23
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H15 As O4 S2'
_chemical_formula_sum            'C23 H15 As O4 S2'
_chemical_formula_weight         494.39
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOAsS
_chemical_oxdiff_usercomment     ' '
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.8326(12)
_cell_length_b                   7.7360(6)
_cell_length_c                   30.2340(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4170.9(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.1420
_cell_measurement_theta_min      2.8960
_shelx_estimated_absorpt_T_max   0.861
_shelx_estimated_absorpt_T_min   0.430
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 2 0.2120
2 -1 0 0.0380
-2 1 0 0.0452
-2 1 2 0.2050
2 -1 -2 0.2727
0 1 0 0.1363
0 -1 0 0.1134
-1 2 1 0.1785

_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.083
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
-0.9994 -0.0058 2.0011 0.1188 -0.0429 0.1390
2.0013 -1.0007 -0.0011 0.0445 0.0543 -0.0442
-2.0013 1.0007 0.0011 -0.0445 -0.0543 0.0442
-1.9998 0.9939 2.0019 0.0902 -0.0637 0.1686
1.9998 -0.9939 -2.0019 -0.0902 0.0637 -0.1686
0.0005 0.9987 0.0004 -0.0128 0.0127 0.0149
-0.0005 -0.9987 -0.0004 0.0128 -0.0127 -0.0149
-0.9992 1.9950 1.0016 0.0258 -0.0129 0.1067

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11351
_diffrn_reflns_point_group_measured_fraction_full 0.650
_diffrn_reflns_point_group_measured_fraction_max 0.643
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.652
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  66.00   0.20    1.75    --   30.00  54.00-180.00  700
  2  ω     21.00  46.00   0.20    1.75    --   30.00  54.00  60.00  125
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0158450000
_diffrn_orient_matrix_UB_12      -0.0128898000
_diffrn_orient_matrix_UB_13      0.0672668000
_diffrn_orient_matrix_UB_21      0.0334320000
_diffrn_orient_matrix_UB_22      0.0126526000
_diffrn_orient_matrix_UB_23      -0.0046846000
_diffrn_orient_matrix_UB_31      -0.0145993000
_diffrn_orient_matrix_UB_32      0.0149421000
_diffrn_orient_matrix_UB_33      0.0622249000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.264
_reflns_Friedel_fraction_full    0.287
_reflns_Friedel_fraction_max     0.274
_reflns_number_gt                4866
_reflns_number_total             5488
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.027(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         5488
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      1.051
_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)+(0.0496P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0990
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.973(19)
 0.027(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C31, O008, O00D, C30, C27
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O007, O00E, C28, C24, C30, C27, O008, O00D, C31, C29
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Ternary CH refined with riding coordinates:
 C46(H46), C23(H23)
4.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C19(H19), C13(H13), C40(H40), C10(H10), C41(H41),
 C18(H18), C36(H36), C20(H20), C11(H11), C33(H33), C12(H12), C35(H35), C34(H34),
  C21(H21)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C)
;
_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
As1 As 0.40238(3) 0.52614(8) 0.65372(2) 0.01793(16) Uani 1 1 d . . . . .
As2 As 0.33670(3) -0.54154(8) 0.84305(2) 0.01706(15) Uani 1 1 d . . . . .
S1 S 0.28666(9) 0.3880(2) 0.73253(6) 0.0212(4) Uani 1 1 d . . . . .
S4 S 0.45149(9) -0.3932(2) 0.76485(5) 0.0203(4) Uani 1 1 d . . . . .
S3 S 0.16253(8) -0.3867(2) 0.84551(6) 0.0214(4) Uani 1 1 d . . . . .
S2 S 0.57672(8) 0.3717(2) 0.65242(6) 0.0215(3) Uani 1 1 d . . . . .
O007 O 0.4584(3) -0.5641(6) 0.95993(15) 0.0254(11) Uani 1 1 d . . . . .
O008 O 0.3820(3) -0.2515(7) 0.98401(16) 0.0295(12) Uani 1 1 d . . . . .
O009 O 0.2577(3) 0.1121(7) 0.55129(16) 0.0291(12) Uani 1 1 d . . . . .
O00A O 0.3574(3) 0.7322(7) 0.56697(18) 0.0322(12) Uani 1 1 d . . . . .
O00B O 0.3589(3) 0.2172(8) 0.51453(15) 0.0295(12) Uani 1 1 d . . . . .
O00C O 0.2787(3) 0.5344(7) 0.53800(15) 0.0269(11) Uani 1 1 d . . . . .
O00D O 0.4819(3) -0.1407(7) 0.94832(16) 0.0310(12) Uani 1 1 d . . . . .
O00E O 0.3821(3) -0.7579(7) 0.92781(18) 0.0308(11) Uani 1 1 d . . . . .
C9 C 0.2540(4) 0.1739(9) 0.7302(2) 0.0208(14) Uani 1 1 d . . . . .
C44 C 0.4537(3) -0.0958(8) 0.8059(2) 0.0149(13) Uani 1 1 d . . . . .
C16 C 0.4598(3) 0.1897(9) 0.6333(2) 0.0185(14) Uani 1 1 d . . . . .
C17 C 0.5214(3) 0.0738(9) 0.6267(2) 0.0195(14) Uani 1 1 d . . . . .
C42 C 0.5227(4) 0.1587(9) 0.7858(2) 0.0248(15) Uani 1 1 d . . . . .
H42 H 0.537188 0.274762 0.791454 0.030 Uiso 1 1 calc R U . . .
C25 C 0.2591(3) -0.3660(9) 0.8520(2) 0.0207(14) Uani 1 1 d . . . . .
C39 C 0.4826(3) -0.1764(9) 0.7683(2) 0.0193(14) Uani 1 1 d . . . . .
C14 C 0.2850(3) 0.0850(9) 0.6934(2) 0.0191(14) Uani 1 1 d . . . . .
C43 C 0.4741(3) 0.0772(9) 0.8145(2) 0.0179(14) Uani 1 1 d . . . . .
H43 H 0.454671 0.136421 0.839542 0.021 Uiso 1 1 calc R U . . .
C28 C 0.4054(3) -0.6138(10) 0.9304(2) 0.0195(13) Uani 1 1 d . . . . .
C15 C 0.3350(3) 0.1958(10) 0.6685(2) 0.0161(14) Uani 1 1 d . . . . .
C7 C 0.3148(4) 0.1946(10) 0.5498(2) 0.0212(15) Uani 1 1 d . . . . .
C38 C 0.2796(3) -0.2054(9) 0.8658(2) 0.0177(14) Uani 1 1 d . . . . .
C2 C 0.3405(3) 0.3581(10) 0.6852(2) 0.0181(15) Uani 1 1 d . . . . .
C46 C 0.3629(3) -0.1708(9) 0.87324(19) 0.0156(13) Uani 1 1 d . . . . .
H46 H 0.371554 -0.049128 0.883146 0.019 Uiso 1 1 calc R U . . .
C19 C 0.5902(4) -0.1842(10) 0.6084(2) 0.0265(16) Uani 1 1 d . . . . .
H19 H 0.591217 -0.301028 0.598753 0.032 Uiso 1 1 calc R U . . .
C13 C 0.2637(3) -0.0879(9) 0.6864(2) 0.0211(14) Uani 1 1 d . . . . .
H13 H 0.283574 -0.150346 0.662006 0.025 Uiso 1 1 calc R U . . .
C40 C 0.5314(4) -0.0961(10) 0.7394(2) 0.0236(15) Uani 1 1 d . . . . .
H40 H 0.550864 -0.154856 0.714259 0.028 Uiso 1 1 calc R U . . .
C45 C 0.4045(3) -0.2082(9) 0.8304(2) 0.0164(14) Uani 1 1 d . . . . .
C10 C 0.2047(4) 0.0945(10) 0.7594(2) 0.0238(15) Uani 1 1 d . . . . .
H10 H 0.185165 0.155139 0.784134 0.029 Uiso 1 1 calc R U . . .
C22 C 0.5906(3) 0.1545(9) 0.6374(2) 0.0193(15) Uani 1 1 d . . . . .
C41 C 0.5510(4) 0.0743(9) 0.7485(2) 0.0241(15) Uani 1 1 d . . . . .
H41 H 0.584102 0.134006 0.729200 0.029 Uiso 1 1 calc R U . . .
C24 C 0.3843(3) -0.4707(9) 0.9008(2) 0.0181(12) Uani 1 1 d . . . . .
C4 C 0.3492(3) 0.2788(10) 0.5904(2) 0.0204(14) Uani 1 1 d . . . . .
C23 C 0.3762(3) 0.1532(9) 0.62601(19) 0.0176(14) Uani 1 1 d . . . . .
H23 H 0.367597 0.030476 0.616979 0.021 Uiso 1 1 calc R U . . .
C26 C 0.3982(3) -0.3691(9) 0.8123(2) 0.0185(14) Uani 1 1 d . . . . .
C30 C 0.4244(4) -0.2230(10) 0.9485(2) 0.0210(13) Uani 1 1 d . . . . .
C18 C 0.5231(3) -0.1006(9) 0.6116(2) 0.0191(14) Uani 1 1 d . . . . .
H18 H 0.477881 -0.158038 0.603822 0.023 Uiso 1 1 calc R U . . .
C36 C 0.2173(3) 0.0825(9) 0.8866(2) 0.0204(14) Uani 1 1 d . . . . .
H36 H 0.263069 0.139577 0.893447 0.024 Uiso 1 1 calc R U . . .
C5 C 0.3324(3) 0.5884(10) 0.5660(2) 0.0210(15) Uani 1 1 d . . . . .
C1 C 0.3551(3) 0.4480(9) 0.5969(2) 0.0179(14) Uani 1 1 d . . . . .
C3 C 0.4808(3) 0.3490(9) 0.6463(2) 0.0203(14) Uani 1 1 d . . . . .
C20 C 0.6584(4) -0.1005(10) 0.6193(2) 0.0257(16) Uani 1 1 d . . . . .
H20 H 0.704265 -0.162518 0.617076 0.031 Uiso 1 1 calc R U . . .
C11 C 0.1849(4) -0.0758(10) 0.7512(2) 0.0272(16) Uani 1 1 d . . . . .
H11 H 0.150937 -0.132270 0.770678 0.033 Uiso 1 1 calc R U . . .
C27 C 0.3905(3) -0.3005(10) 0.9082(2) 0.0187(12) Uani 1 1 d . . . . .
C33 C 0.0809(4) -0.0839(10) 0.8656(2) 0.0240(16) Uani 1 1 d . . . . .
H33 H 0.034947 -0.139774 0.858726 0.029 Uiso 1 1 calc R U . . .
C12 C 0.2139(3) -0.1666(10) 0.7148(2) 0.0240(15) Uani 1 1 d . . . . .
H12 H 0.199171 -0.283007 0.709798 0.029 Uiso 1 1 calc R U . . .
C32 C 0.1492(3) -0.1727(10) 0.8623(2) 0.0205(14) Uani 1 1 d . . . . .
C29 C 0.4838(5) -0.6989(12) 0.9895(3) 0.042(2) Uani 1 1 d . . . . .
H29A H 0.501347 -0.797999 0.972090 0.063 Uiso 1 1 calc R U . . .
H29B H 0.442356 -0.735089 1.008587 0.063 Uiso 1 1 calc R U . . .
H29C H 0.525095 -0.655049 1.007695 0.063 Uiso 1 1 calc R U . . .
C37 C 0.2176(3) -0.0908(9) 0.8728(2) 0.0201(14) Uani 1 1 d . . . . .
C35 C 0.1497(4) 0.1691(10) 0.8902(2) 0.0253(15) Uani 1 1 d . . . . .
H35 H 0.148786 0.285302 0.900435 0.030 Uiso 1 1 calc R U . . .
C34 C 0.0820(4) 0.0854(10) 0.8788(2) 0.0261(16) Uani 1 1 d . . . . .
H34 H 0.036253 0.147881 0.880391 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2525(4) 0.6654(12) 0.5070(2) 0.038(2) Uani 1 1 d . . . . .
H6A H 0.293811 0.699035 0.487421 0.058 Uiso 1 1 calc R U . . .
H6B H 0.235002 0.766831 0.523444 0.058 Uiso 1 1 calc R U . . .
H6C H 0.211231 0.618401 0.489345 0.058 Uiso 1 1 calc R U . . .
C8 C 0.3305(4) 0.1420(13) 0.4739(2) 0.042(2) Uani 1 1 d . . . . .
H8A H 0.362964 0.175482 0.449209 0.063 Uiso 1 1 calc R U . . .
H8B H 0.279474 0.184042 0.468496 0.063 Uiso 1 1 calc R U . . .
H8C H 0.329853 0.015816 0.476619 0.063 Uiso 1 1 calc R U . . .
C31 C 0.4132(5) -0.1958(13) 1.0263(2) 0.044(2) Uani 1 1 d . . . . .
H31A H 0.419458 -0.069942 1.026188 0.067 Uiso 1 1 calc R U . . .
H31B H 0.461988 -0.251163 1.030918 0.067 Uiso 1 1 calc R U . . .
H31C H 0.379015 -0.228854 1.050259 0.067 Uiso 1 1 calc R U . . .
C21 C 0.6595(4) 0.0702(10) 0.6332(2) 0.0249(16) Uani 1 1 d . . . . .
H21 H 0.705327 0.127690 0.639560 0.030 Uiso 1 1 calc R U . . .


_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
As1 C2 1.953(7) . ?
As1 C1 2.007(6) . ?
As1 C3 1.971(6) . ?
As2 C25 1.958(7) . ?
As2 C24 2.016(6) . ?
As2 C26 1.960(7) . ?
S1 C9 1.756(7) . ?
S1 C2 1.739(6) . ?
S4 C39 1.770(7) . ?
S4 C26 1.732(6) . ?
S3 C25 1.740(6) . ?
S3 C32 1.749(8) . ?
S2 C22 1.759(8) . ?
S2 C3 1.729(6) . ?
O007 C28 1.355(8) . ?
O007 C29 1.446(9) . ?
O008 C30 1.332(8) . ?
O008 C31 1.460(8) . ?
O009 C7 1.204(8) . ?
O00A C5 1.199(9) . ?
O00B C7 1.336(8) . ?
O00B C8 1.450(9) . ?
O00C C5 1.345(8) . ?
O00C C6 1.457(8) . ?
O00D C30 1.208(8) . ?
O00E C28 1.192(9) . ?
C9 C14 1.420(9) . ?
C9 C10 1.388(9) . ?
C44 C39 1.396(9) . ?
C44 C43 1.411(9) . ?
C44 C45 1.439(9) . ?
C16 C17 1.433(9) . ?
C16 C23 1.532(8) . ?
C16 C3 1.347(10) . ?
C17 C22 1.419(9) . ?
C17 C18 1.424(10) . ?
C42 C43 1.380(9) . ?
C42 C41 1.396(10) . ?
C25 C38 1.361(10) . ?
C39 C40 1.382(9) . ?
C14 C15 1.449(9) . ?
C14 C13 1.406(10) . ?
C28 C24 1.473(10) . ?
C15 C2 1.357(10) . ?
C15 C23 1.515(8) . ?
C7 C4 1.519(9) . ?
C38 C46 1.526(8) . ?
C38 C37 1.433(9) . ?
C46 C45 1.520(8) . ?
C46 C27 1.538(9) . ?
C19 C18 1.364(9) . ?
C19 C20 1.417(10) . ?
C13 C12 1.378(9) . ?
C40 C41 1.392(10) . ?
C45 C26 1.365(9) . ?
C10 C11 1.387(11) . ?
C22 C21 1.398(9) . ?
C24 C27 1.341(10) . ?
C4 C23 1.527(9) . ?
C4 C1 1.328(10) . ?
C30 C27 1.485(9) . ?
C36 C37 1.404(10) . ?
C36 C35 1.385(9) . ?
C5 C1 1.488(9) . ?
C20 C21 1.385(11) . ?
C11 C12 1.405(10) . ?
C33 C32 1.401(9) . ?
C33 C34 1.370(11) . ?
C32 C37 1.412(9) . ?
C35 C34 1.412(10) . ?

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
C2 As1 C1 88.8(3) . . ?
C2 As1 C3 89.6(3) . . ?
C3 As1 C1 89.5(3) . . ?
C25 As2 C24 89.4(3) . . ?
C25 As2 C26 89.3(3) . . ?
C26 As2 C24 89.4(3) . . ?
C2 S1 C9 91.4(3) . . ?
C26 S4 C39 91.2(3) . . ?
C25 S3 C32 90.8(3) . . ?
C3 S2 C22 90.8(3) . . ?
C28 O007 C29 114.9(6) . . ?
C30 O008 C31 116.2(6) . . ?
C7 O00B C8 114.7(5) . . ?
C5 O00C C6 114.6(6) . . ?
C14 C9 S1 111.1(5) . . ?
C10 C9 S1 127.0(5) . . ?
C10 C9 C14 122.0(7) . . ?
C39 C44 C43 118.6(6) . . ?
C39 C44 C45 112.0(6) . . ?
C43 C44 C45 129.5(6) . . ?
C17 C16 C23 127.7(6) . . ?
C3 C16 C17 113.5(6) . . ?
C3 C16 C23 118.7(6) . . ?
C22 C17 C16 111.1(6) . . ?
C22 C17 C18 118.2(6) . . ?
C18 C17 C16 130.8(6) . . ?
C43 C42 C41 121.4(7) . . ?
S3 C25 As2 128.3(4) . . ?
C38 C25 As2 119.0(5) . . ?
C38 C25 S3 112.7(5) . . ?
C44 C39 S4 110.8(5) . . ?
C40 C39 S4 125.9(5) . . ?
C40 C39 C44 123.2(7) . . ?
C9 C14 C15 111.1(6) . . ?
C13 C14 C9 118.3(6) . . ?
C13 C14 C15 130.6(6) . . ?
C42 C43 C44 118.7(6) . . ?
O007 C28 C24 111.4(6) . . ?
O00E C28 O007 123.5(7) . . ?
O00E C28 C24 125.0(6) . . ?
C14 C15 C23 127.6(6) . . ?
C2 C15 C14 113.4(6) . . ?
C2 C15 C23 118.8(6) . . ?
O009 C7 O00B 126.7(6) . . ?
O009 C7 C4 122.6(6) . . ?
O00B C7 C4 110.6(5) . . ?
C25 C38 C46 117.8(6) . . ?
C25 C38 C37 113.7(5) . . ?
C37 C38 C46 128.4(6) . . ?
S1 C2 As1 128.6(4) . . ?
C15 C2 As1 118.4(5) . . ?
C15 C2 S1 113.0(5) . . ?
C38 C46 C27 107.3(5) . . ?
C45 C46 C38 108.5(5) . . ?
C45 C46 C27 107.8(5) . . ?
C18 C19 C20 121.4(7) . . ?
C12 C13 C14 120.0(6) . . ?
C39 C40 C41 117.2(6) . . ?
C44 C45 C46 128.3(6) . . ?
C26 C45 C44 113.3(6) . . ?
C26 C45 C46 118.3(6) . . ?
C11 C10 C9 118.0(6) . . ?
C17 C22 S2 111.0(5) . . ?
C21 C22 S2 126.3(5) . . ?
C21 C22 C17 122.6(7) . . ?
C40 C41 C42 120.8(6) . . ?
C28 C24 As2 115.5(5) . . ?
C27 C24 As2 116.5(5) . . ?
C27 C24 C28 128.0(6) . . ?
C7 C4 C23 115.1(6) . . ?
C1 C4 C7 125.0(6) . . ?
C1 C4 C23 119.9(6) . . ?
C15 C23 C16 108.1(5) . . ?
C15 C23 C4 107.8(5) . . ?
C4 C23 C16 106.9(5) . . ?
S4 C26 As2 128.8(4) . . ?
C45 C26 As2 118.5(5) . . ?
C45 C26 S4 112.6(5) . . ?
O008 C30 C27 111.3(6) . . ?
O00D C30 O008 124.9(6) . . ?
O00D C30 C27 123.7(6) . . ?
C19 C18 C17 119.3(6) . . ?
C35 C36 C37 119.3(6) . . ?
O00A C5 O00C 124.6(7) . . ?
O00A C5 C1 124.1(6) . . ?
O00C C5 C1 111.2(6) . . ?
C4 C1 As1 117.1(5) . . ?
C4 C1 C5 127.3(6) . . ?
C5 C1 As1 115.6(5) . . ?
S2 C3 As1 128.2(4) . . ?
C16 C3 As1 118.2(5) . . ?
C16 C3 S2 113.6(5) . . ?
C21 C20 C19 121.2(6) . . ?
C10 C11 C12 121.3(6) . . ?
C24 C27 C46 119.9(6) . . ?
C24 C27 C30 124.6(6) . . ?
C30 C27 C46 115.5(6) . . ?
C34 C33 C32 118.5(6) . . ?
C13 C12 C11 120.4(7) . . ?
C33 C32 S3 127.1(5) . . ?
C33 C32 C37 121.0(7) . . ?
C37 C32 S3 111.9(5) . . ?
C36 C37 C38 129.6(6) . . ?
C36 C37 C32 119.5(6) . . ?
C32 C37 C38 110.9(6) . . ?
C36 C35 C34 120.2(7) . . ?
C33 C34 C35 121.5(6) . . ?
C20 C21 C22 117.4(7) . . ?


_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 1.993
_oxdiff_exptl_absorpt_empirical_full_min 0.728
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.973(19)
2 0.027(19)

