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_7714770
_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'
_chemical_formula_sum            'C27 H24 As B'
_chemical_formula_weight         434.19
_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             2021-12-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2023-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                114.397(15)
_cell_angle_beta                 91.526(11)
_cell_angle_gamma                112.134(11)
_cell_formula_units_Z            2
_cell_length_a                   9.0332(9)
_cell_length_b                   11.5594(15)
_cell_length_c                   12.589(2)
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.4480
_cell_measurement_theta_min      2.7970
_cell_volume                     1082.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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      93.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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  35.00   1.00    2.50    --   30.00  54.00 150.00  107
  2  \w    -71.00 -45.00   1.00    2.50    --   30.00  54.00 -90.00   26
  3  \w      6.00  33.00   1.00    2.50    --   30.00  54.00 -90.00   27
  4  \w    -69.00 115.00   1.00    2.50    --   30.00  54.00  30.00  184
  5  \w     33.00  60.00   1.00    2.50    --   30.00  54.00-120.00   27
  6  \w    -56.00 -30.00   1.00    2.50    --   30.00  54.00-120.00   26
;
_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      -0.0708195000
_diffrn_orient_matrix_UB_12      -0.0056575000
_diffrn_orient_matrix_UB_13      -0.0313643000
_diffrn_orient_matrix_UB_21      -0.0304796000
_diffrn_orient_matrix_UB_22      0.0173420000
_diffrn_orient_matrix_UB_23      0.0530729000
_diffrn_orient_matrix_UB_31      0.0399141000
_diffrn_orient_matrix_UB_32      0.0722030000
_diffrn_orient_matrix_UB_33      0.0146586000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5914
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.0
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.687
_exptl_crystal_size_mid          0.441
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4242
_reflns_number_total             5914
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9989\% 
around [-0.00 0.00 1.00] (reciprocal) or [0.25 0.46 0.85] (direct)
;
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_database_code               7714770
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHBAs
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5306(8)
 0.4694(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C5(H5), C18(H18), C8(H8), C12(H12), C11(H11), C7(H7),
 C9(H9), C14(H14), C21(H21), C23(H23), C10(H10), C15(H15), C16(H16)
3.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C)
;
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.776
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2