Dithienoarsinines: stable and planar π-extended arsabenzenes.
Sumida, Akifumi; Saeki, Akinori; Matsuo, Kyohei; Naka, Kensuke; Imoto, Hiroaki; Chemical science 16 (2025) 1126–1135; doi:10.1039/d4sc06590e

data_1573224
_publ_section_title
;
 Dithienoarsinines: stable and planar &#x3c0;-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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -64.00 117.80   0.30    2.50    --   30.00  54.00  30.00  606
  2  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0620P)^2^+0.3054P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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