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_7714779
_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, 0.5(C H4 O)'
_chemical_formula_sum            'C27.5 H26 As B O0.5 S'
_chemical_formula_weight         482.27
_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             2023-02-11
_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                86.683(4)
_cell_angle_beta                 81.031(4)
_cell_angle_gamma                75.640(5)
_cell_formula_units_Z            4
_cell_length_a                   9.3729(6)
_cell_length_b                   14.9082(10)
_cell_length_c                   17.5035(8)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.0320
_cell_measurement_theta_min      2.7720
_cell_volume                     2340.0(2)
_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      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_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    -72.00  31.00   0.25    1.75    --   30.00  54.00-120.00  412
  2  \w    -71.00 -45.00   0.25    1.75    --   30.00  54.00   0.00  104
  3  \w     18.00  44.00   0.25    1.75    --   30.00  54.00   0.00  104
  4  \w    -74.00 109.00   0.25    1.75    --   30.00  54.00 120.00  732
;
_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      -0.0315093000
_diffrn_orient_matrix_UB_12      0.0052838000
_diffrn_orient_matrix_UB_13      0.0395248000
_diffrn_orient_matrix_UB_21      -0.0653360000
_diffrn_orient_matrix_UB_22      0.0301821000
_diffrn_orient_matrix_UB_23      -0.0108357000
_diffrn_orient_matrix_UB_31      -0.0312111000
_diffrn_orient_matrix_UB_32      -0.0383942000
_diffrn_orient_matrix_UB_33      -0.0020253000
_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  0.0714
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14207
_diffrn_reflns_point_group_measured_fraction_full 0.999
_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         2.704
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.831
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.761
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6751
_reflns_number_total             9569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3a-S_hexane
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_original_formula_sum        'C27.50 H26 As B O0.50 S'
_cod_database_code               7714779
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHBAsSO
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.384
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C35(H35), C34(H34), C33(H33), C5(H5), C9(H9), C11(H11), C27(H27),
 C50(H50), C6(H6), C36(H36), C24(H24), C39(H39), C51(H51), C12(H12), C10(H10),
 C25(H25), C23(H23), C8(H8), C42(H42), C7(H7), C52(H52), C38(H38), C44(H44),
 C15(H15), C26(H26), C54(H54), C53(H53), C37(H37), C17(H17)
2.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C55(H55A,H55B,H55C), C20(H20A,H20B,H20C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              84875
_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 1.811
_oxdiff_exptl_absorpt_empirical_full_min 0.555