#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:29:35 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298156 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573224.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1573224
loop_
_publ_author_name
'Sumida, Akifumi'
'Saeki, Akinori'
'Matsuo, Kyohei'
'Naka, Kensuke'
'Imoto, Hiroaki'
_publ_section_title
;
 Dithienoarsinines: stable and planar π-extended arsabenzenes.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1126
_journal_page_last               1135
_journal_paper_doi               10.1039/d4sc06590e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C9 H5 As S2'
_chemical_formula_sum            'C9 H5 As S2'
_chemical_formula_weight         252.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-07
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.093(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5045(11)
_cell_length_b                   6.2032(5)
_cell_length_c                   13.9819(13)
_cell_measurement_reflns_used    1511
_cell_measurement_temperature    197.15
_cell_measurement_theta_max      30.8270
_cell_measurement_theta_min      3.0180
_cell_volume                     890.86(15)
_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)'
_diffrn_ambient_temperature      197.15
_diffrn_detector                 'CCD plate'
_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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.848
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.128
_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_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0363
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1607
_reflns_number_total             1822
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc06590e2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 1573224--1573235.cif.'
_cod_database_code               1573224
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C9H5AsS2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.124
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . .
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'
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
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) . . ?
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_
_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
