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_7711064
_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         'C8 H4 As I S2'
_chemical_formula_sum            'C8 H4 As I S2'
_chemical_formula_weight         366.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-24
_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                 91.379(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2923(10)
_cell_length_b                   4.9794(4)
_cell_length_c                   28.3920(17)
_cell_measurement_reflns_used    2127
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      31.6960
_cell_measurement_theta_min      3.9870
_cell_volume                     2020.0(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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   2.00   0.50    3.50    --   30.00  54.00 -90.00  146
  2  \w     21.00 111.00   0.50    3.50    --   30.00  54.00 -90.00  180
  3  \w    -14.00  69.00   0.50    3.50    --   30.00  54.00-150.00  166
;
_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      -0.0481594000
_diffrn_orient_matrix_UB_12      -0.0043452000
_diffrn_orient_matrix_UB_13      0.0054231000
_diffrn_orient_matrix_UB_21      -0.0119576000
_diffrn_orient_matrix_UB_22      0.0320208000
_diffrn_orient_matrix_UB_23      -0.0237327000
_diffrn_orient_matrix_UB_31      -0.0012646000
_diffrn_orient_matrix_UB_32      -0.1387382000
_diffrn_orient_matrix_UB_33      -0.0056477000
_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  0.0167
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            4142
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.776
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.848
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.638
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+4.4617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1753
_reflns_number_total             2059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02051c2.cif
_cod_data_source_block           01-3_DTA-I
_cod_database_code               7711064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOAsS
_shelx_estimated_absorpt_t_max   0.434
_shelx_estimated_absorpt_t_min   0.098
_reflns_odcompleteness_completeness 99.83
_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:
 C2(H2), C3(H3), C7(H7), C6(H6)
;
_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 2.024
_oxdiff_exptl_absorpt_empirical_full_min 0.665