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_1573229
_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         'C34 H16 As2 S4'
_chemical_formula_sum            'C34 H16 As2 S4'
_chemical_formula_weight         702.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-23
_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                87.822(5)
_cell_angle_beta                 85.309(5)
_cell_angle_gamma                80.114(6)
_cell_formula_units_Z            2
_cell_length_a                   8.0954(6)
_cell_length_b                   11.3660(7)
_cell_length_c                   15.4655(8)
_cell_measurement_reflns_used    3347
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.3340
_cell_measurement_theta_min      2.8670
_cell_volume                     1396.77(16)
_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)'
_diffrn_ambient_temperature      100.00
_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    -73.00 -46.00   0.10    7.00    --   30.00  54.00 120.00  270
  2  \w      8.00  34.00   0.10    7.00    --   30.00  54.00 120.00  260
  3  \w    -71.00  34.00   0.10    7.00    --   30.00  54.00   0.00 1050
  4  \w    -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       '\w 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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       needle
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.608
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.125
_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_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0421
_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/[\s^2^(Fo^2^)+(0.0477P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4442
_reflns_number_total             5695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06590e2.cif
_cod_data_source_block           3d'
_cod_depositor_comments
'Adding full bibliography for 1573224--1573235.cif.'
_cod_database_code               1573229
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHSAs
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.288
_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)
;
_shelx_res_checksum              94489
_shelx_hkl_checksum              12754
_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