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_7714774
_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         'C35 H28 As B, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C35.5 H29 As B Cl'
_chemical_formula_weight         576.77
_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             2023-02-02
_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                86.788(4)
_cell_angle_beta                 75.613(4)
_cell_angle_gamma                74.804(4)
_cell_formula_units_Z            4
_cell_length_a                   11.0750(5)
_cell_length_b                   16.3776(7)
_cell_length_c                   16.4079(8)
_cell_measurement_reflns_used    7504
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.0800
_cell_measurement_theta_min      2.7550
_cell_volume                     2781.8(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 0.998
_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    -74.00 107.00   0.10    4.50    --   30.00  54.00-180.00 1810
  2  \w     36.00  76.00   0.10    4.50    --   30.00  54.00  90.00  400
  3  \w     38.00 108.00   0.10    4.50    --   30.00  54.00  30.00  700
  4  \w     38.00  92.00   0.10    4.50    --   30.00  54.00-120.00  540
  5  \w    -48.00 -22.00   0.10    4.50    --   30.00  54.00-150.00  260
  6  \w    -74.00 -32.00   0.10    4.50    --   30.00  54.00  30.00  420
;
_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      0.0531899000
_diffrn_orient_matrix_UB_12      -0.0067974000
_diffrn_orient_matrix_UB_13      -0.0356280000
_diffrn_orient_matrix_UB_21      0.0007910000
_diffrn_orient_matrix_UB_22      -0.0434162000
_diffrn_orient_matrix_UB_23      -0.0005032000
_diffrn_orient_matrix_UB_31      -0.0430020000
_diffrn_orient_matrix_UB_32      0.0091112000
_diffrn_orient_matrix_UB_33      -0.0268686000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20553
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.563
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.930
_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    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.91
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         11366
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.7530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8569
_reflns_number_total             11366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_original_formula_sum        'C35.50 H29 As B Cl'
_cod_database_code               7714774
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHBAsCl
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B2) = Uanis(C63)
Uanis(C21) = Uanis(As1)
3. Rigid body (RIGU) restrains
 As2, C36, C48, B2, C38, C39
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(H72C)=Sof(H72D)=1-FVAR(1)
 Sof(H72A)=Sof(H72B)=Sof(Cl2B)=Sof(Cl1B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C72(H72C,H72D), C72(H72A,H72B)
5.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C40(H40), C22(H22), C47(H47), C5(H5), C49(H49), C58(H58), C62(H62),
 C51(H51), C13(H13), C67(H67), C45(H45), C12(H12), C53(H53), C54(H54), C59(H59),
  C20(H20), C60(H60), C65(H65), C61(H61), C26(H26), C52(H52), C7(H7), C44(H44),
 C42(H42), C23(H23), C16(H16), C10(H10), C25(H25), C15(H15), C18(H18), C43(H43),
  C9(H9), C8(H8), C24(H24), C17(H17), C31(H31), C29(H29)
5.c Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C70(H70A,H70B,H70C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              67583
_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 1.346
_oxdiff_exptl_absorpt_empirical_full_min 0.648