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_1573235
_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         'C23 H15 As O4 S2'
_chemical_formula_sum            'C23 H15 As O4 S2'
_chemical_formula_weight         494.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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)
;
_audit_update_record
;
2024-09-20 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8326(12)
_cell_length_b                   7.7360(6)
_cell_length_c                   30.2340(15)
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.1420
_cell_measurement_theta_min      2.8960
_cell_volume                     4170.9(5)
_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      100.00
_diffrn_detector                 'CCD plate'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00  66.00   0.20    1.75    --   30.00  54.00-180.00  700
  2  \w     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       '\w 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_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.083
_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_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_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0990
_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_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06590e2.cif
_cod_data_source_block           3c-DMAD
_cod_depositor_comments
'Adding full bibliography for 1573224--1573235.cif.'
_cod_database_code               1573235
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOAsS
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.430
_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)
;
_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