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_7714780
_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 Au B Cl, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H25 As Au B Cl2'
_chemical_formula_weight         709.07
_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             2022-07-19
_audit_creation_method
;
Olex2 1.5-ac5-023
(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                68.133(3)
_cell_angle_beta                 88.064(2)
_cell_angle_gamma                83.955(3)
_cell_formula_units_Z            4
_cell_length_a                   9.0967(3)
_cell_length_b                   15.1687(7)
_cell_length_c                   20.2163(5)
_cell_measurement_reflns_used    8919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7450
_cell_measurement_theta_min      2.8090
_cell_volume                     2574.40(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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 -45.00   0.15    5.00    --   30.00  54.00 -30.00  180
  2  \w      8.00  34.10   0.15    5.00    --   30.00  54.00 -30.00  174
  3  \w    -72.00  33.00   0.15    5.00    --   30.00  54.00-150.00  700
  4  \w    -74.00 108.10   0.15    5.00    --   30.00  54.00  90.00 1214
;
_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      0.0435545000
_diffrn_orient_matrix_UB_12      0.0244135000
_diffrn_orient_matrix_UB_13      0.0146944000
_diffrn_orient_matrix_UB_21      0.0632279000
_diffrn_orient_matrix_UB_22      -0.0123525000
_diffrn_orient_matrix_UB_23      -0.0174450000
_diffrn_orient_matrix_UB_31      -0.0159351000
_diffrn_orient_matrix_UB_32      0.0426159000
_diffrn_orient_matrix_UB_33      -0.0301488000
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         2.562
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.212
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (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    1.829
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.839
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8579
_reflns_number_total             10513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3a-AuCl
_cod_depositor_comments
;
Adding full bibliography for 7714770--7714783.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C55 H50 As2 Au2 B2 Cl4'
_cod_original_formula_weight         1418.14
_cod_original_formula_moiety         'C54 H48 As2 Au2 B2 Cl2, C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_database_code               7714780
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHBAsClAu
_shelx_estimated_absorpt_t_max   0.374
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C01Q(H01z,H)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00S(H00S), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C012(H012), C013(H013), C015(H015), C01A(H01d), C01B(H01e), C01C(H01f),
 C01D(H01g), C01F(H01h), C01G(H01i), C01H(H01j), C01K(H01K), C01M(H01M)
2.c Idealised Me refined as rotating group:
 C018(H01a,H01b,H01c), C01O(H01l,H01n,H01o), C01P(H01p,H01q,H01r), C01R(H01s,
 H01t,H01u), C01S(H01v,H01w,H01x), C01T(H01y,Ha,Hb)
;
_shelx_res_checksum              39398
_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 2.062
_oxdiff_exptl_absorpt_empirical_full_min 0.702