4-Aryldithieno[3,2-b:2′,3′-d]arsoles: effects of the As-substituent on the structure, photophysical properties, and stability
Takahara, Chisa; Iwasaki, Suzuka; Kihara, Hyota; Miyake, Yusuke; Imoto, Hiroaki; Naka, Kensuke; Dalton Transactions  (2022) –; doi:10.1039/D2DT02051C

data_7711069
_publ_section_title
;
 4-Aryldithieno[3,2-b:2&#x2032;,3&#x2032;-d]arsoles: effects of the
 As-substituent on the structure, photophysical properties, and stability
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02051C
_journal_year                    2022
_chemical_formula_moiety         'C14 H9 As S2'
_chemical_formula_sum            'C14 H9 As S2'
_chemical_formula_weight         316.25
_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             2021-10-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.6354(8)
_cell_length_b                   5.8417(7)
_cell_length_c                   33.241(3)
_cell_measurement_reflns_used    2725
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      29.9110
_cell_measurement_theta_min      3.2060
_cell_volume                     2453.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_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    -71.00  72.00   0.25    5.00    --   30.00  54.00-180.00  572
  2  \w     78.00 103.00   0.25    5.00    --   30.00  54.00-180.00  100
  3  \w    -15.00  10.00   0.25    5.00    --   30.00  54.00 -30.00  100
;
_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      0.0368837000
_diffrn_orient_matrix_UB_12      -0.0146815000
_diffrn_orient_matrix_UB_13      0.0374241000
_diffrn_orient_matrix_UB_21      -0.0417212000
_diffrn_orient_matrix_UB_22      -0.0140438000
_diffrn_orient_matrix_UB_23      0.0143135000
_diffrn_orient_matrix_UB_31      0.0069413000
_diffrn_orient_matrix_UB_32      -0.0065251000
_diffrn_orient_matrix_UB_33      -0.1146524000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            7545
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.081
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 1142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.226(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_full    0.677
_reflns_Friedel_fraction_max     0.673
_reflns_number_gt                3562
_reflns_number_total             4214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02051c2.cif
_cod_data_source_block           02_DTA-H
_cod_database_code               7711069
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHAsS
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.355
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C6(H6), C14(H14), C28(H28), C5(H5), C8(H8), C19(H19), C21(H21),
 C12(H12), C13(H13), C22(H22), C24(H24), C7(H7), C25(H25), C26(H26), C10(H10),
 C27(H27), C11(H11)
;
_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 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.316