Synthesis, structures, and photophysical properties of π-extended arsaborins.
Sumida, Akifumi; Onishi, Tomoharu; Imoto, Hiroaki; Naka, Kensuke; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1706–1713; doi:10.1039/d3dt03798c

data_7714783
_publ_section_title
;
 Synthesis, structures, and photophysical properties of &#x3c0;-extended
 arsaborins.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1706
_journal_page_last               1713
_journal_paper_doi               10.1039/d3dt03798c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H24 As B S'
_chemical_formula_sum            'C27 H24 As B S'
_chemical_formula_weight         466.25
_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             2023-03-14
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.766(4)
_cell_angle_beta                 78.127(5)
_cell_angle_gamma                77.208(5)
_cell_formula_units_Z            4
_cell_length_a                   9.5976(7)
_cell_length_b                   11.9622(6)
_cell_length_c                   20.8108(11)
_cell_measurement_reflns_used    3675
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.0080
_cell_measurement_theta_min      2.9220
_cell_volume                     2278.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (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 0.999
_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    -72.00  33.00   0.10    2.50    --   30.00  54.00-180.00 1050
  2  \w     18.00  44.00   0.10    2.50    --   30.00  54.00 -60.00  260
  3  \w    -58.00 -32.00   0.10    2.50    --   30.00  54.00 -90.00  260
  4  \w    -73.00 110.00   0.10    2.50    --   30.00  54.00  60.00 1830
;
_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      0.0121350000
_diffrn_orient_matrix_UB_12      -0.0105929000
_diffrn_orient_matrix_UB_13      0.0321846000
_diffrn_orient_matrix_UB_21      0.0249561000
_diffrn_orient_matrix_UB_22      -0.0594514000
_diffrn_orient_matrix_UB_23      -0.0085959000
_diffrn_orient_matrix_UB_31      0.0723765000
_diffrn_orient_matrix_UB_32      0.0075833000
_diffrn_orient_matrix_UB_33      -0.0102749000
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13851
_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         26.371
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (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    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.513
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.182
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6241
_reflns_number_total             9271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3a-S_methanol
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_database_code               7714783
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H24 As B S'
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C48(H48), C11(H11), C13(H13), C39(H39), C21(H21), C41(H41),
 C37(H37), C7(H7), C23(H23), C15(H15), C9(H9), C36(H36), C38(H38), C12(H12),
 C14(H14), C50(H50), C34(H34), C19(H19), C40(H40), C35(H35), C8(H8), C16(H16),
 C17(H17), C18(H18), C42(H42), C44(H44), C45(H45), C46(H46), C43(H43)
2.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C53(H53A,H53B,
 H53C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              31985
_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 2.000
_oxdiff_exptl_absorpt_empirical_full_min 0.606