#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:53:06 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714778.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714778
loop_
_publ_author_name
'Sumida, Akifumi'
'Onishi, Tomoharu'
'Imoto, Hiroaki'
'Naka, Kensuke'
_publ_section_title
;
 Synthesis, structures, and photophysical properties of π-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         'C23 H20 As B S2'
_chemical_formula_sum            'C23 H20 As B S2'
_chemical_formula_weight         446.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-31
_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                90
_cell_angle_beta                 107.164(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0407(15)
_cell_length_b                   20.1117(16)
_cell_length_c                   8.6242(9)
_cell_measurement_reflns_used    2059
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.9480
_cell_measurement_theta_min      3.1620
_cell_volume                     2161.1(4)
_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-ac5-024 (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      298
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00 114.00   0.50    1.25    --   30.00  54.00-150.00  362
  2  ω    -25.00   2.00   0.50    1.25    --   30.00  54.00   0.00   54
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0247180000
_diffrn_orient_matrix_UB_12      -0.0302853000
_diffrn_orient_matrix_UB_13      -0.0113294000
_diffrn_orient_matrix_UB_21      0.0502585000
_diffrn_orient_matrix_UB_22      0.0122281000
_diffrn_orient_matrix_UB_23      0.0484985000
_diffrn_orient_matrix_UB_31      -0.0100971000
_diffrn_orient_matrix_UB_32      -0.0132748000
_diffrn_orient_matrix_UB_33      0.0702814000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7974
_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         26.366
_diffrn_reflns_theta_min         2.671
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.466
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.249
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0363
_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/[σ²(Fo²)+(0.0159P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2943
_reflns_number_total             4409
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3e@298K
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_database_code               7714778
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AsAuClCH
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.462
_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:
 C5(H5), C10(H10), C14(H14), C7(H7), C6(H6), C11(H11), C13(H13), C12(H12),
 C19(H19), C17(H17), C8(H8)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_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 1.668
_oxdiff_exptl_absorpt_empirical_full_min 0.796
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.41475(3) 0.41446(2) 0.87242(4) 0.04074(11) Uani 1 1 d . . . . .
S1 S 0.44951(8) 0.60658(4) 0.63603(10) 0.0555(2) Uani 1 1 d . . . . .
S2 S 0.13178(8) 0.52363(4) 0.92723(12) 0.0636(3) Uani 1 1 d . . . . .
C4 C 0.2847(2) 0.44784(13) 0.9075(3) 0.0393(7) Uani 1 1 d . . . . .
C9 C 0.3502(2) 0.36152(13) 0.6745(3) 0.0374(7) Uani 1 1 d . . . . .
C1 C 0.4512(2) 0.49236(13) 0.7667(3) 0.0372(7) Uani 1 1 d . . . . .
C3 C 0.2417(2) 0.51021(14) 0.8575(3) 0.0408(7) Uani 1 1 d . . . . .
C2 C 0.3863(2) 0.54848(14) 0.7242(3) 0.0416(8) Uani 1 1 d . . . . .
C5 C 0.5494(3) 0.49840(15) 0.7282(3) 0.0463(8) Uani 1 1 d . . . . .
H5 H 0.601888 0.465535 0.749042 0.056 Uiso 1 1 calc R U . . .
C10 C 0.4138(3) 0.31323(14) 0.6351(4) 0.0519(9) Uani 1 1 d . . . . .
H10 H 0.483641 0.306708 0.701355 0.062 Uiso 1 1 calc R U . . .
C14 C 0.2469(3) 0.37022(15) 0.5749(4) 0.0512(9) Uani 1 1 d . . . . .
H14 H 0.203066 0.402408 0.600025 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2277(3) 0.41320(15) 0.9978(4) 0.0511(8) Uani 1 1 d . . . . .
H7 H 0.245697 0.370605 1.038791 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5579(3) 0.55746(16) 0.6576(4) 0.0555(9) Uani 1 1 d . . . . .
H6 H 0.617042 0.569653 0.624549 0.067 Uiso 1 1 calc R U . . .
C20 C 0.2284(3) 0.68651(15) 0.7739(4) 0.0508(8) Uani 1 1 d . . . . .
C15 C 0.2103(3) 0.62607(14) 0.6901(4) 0.0460(8) Uani 1 1 d . . . . .
C11 C 0.3740(3) 0.27448(15) 0.4973(4) 0.0647(11) Uani 1 1 d . . . . .
H11 H 0.417377 0.242175 0.471534 0.078 Uiso 1 1 calc R U . . .
C13 C 0.2077(3) 0.33095(16) 0.4366(4) 0.0635(10) Uani 1 1 d . . . . .
H13 H 0.137972 0.337026 0.369671 0.076 Uiso 1 1 calc R U . . .
C12 C 0.2720(3) 0.28343(17) 0.3996(4) 0.0655(11) Uani 1 1 d . . . . .
H12 H 0.245875 0.257247 0.307454 0.079 Uiso 1 1 calc R U . . .
C19 C 0.1636(3) 0.74130(15) 0.7111(4) 0.0619(10) Uani 1 1 d . . . . .
H19 H 0.177343 0.781527 0.766538 0.074 Uiso 1 1 calc R U . . .
C16 C 0.1261(3) 0.62271(16) 0.5440(4) 0.0576(9) Uani 1 1 d . . . . .
C18 C 0.0804(3) 0.73767(18) 0.5706(5) 0.0666(11) Uani 1 1 d . . . . .
C17 C 0.0617(3) 0.67792(19) 0.4883(4) 0.0678(11) Uani 1 1 d . . . . .
H17 H 0.004796 0.674535 0.393582 0.081 Uiso 1 1 calc R U . . .
C8 C 0.1445(3) 0.44796(16) 1.0190(4) 0.0658(10) Uani 1 1 d . . . . .
H8 H 0.099400 0.432437 1.076861 0.079 Uiso 1 1 calc R U . . .
B1 B 0.2797(3) 0.56200(16) 0.7556(4) 0.0416(9) Uani 1 1 d . . . . .
C23 C 0.3169(3) 0.69335(16) 0.9325(4) 0.0792(12) Uani 1 1 d . . . . .
H23A H 0.302469 0.664355 1.012012 0.119 Uiso 1 1 calc R U . . .
H23B H 0.319891 0.738499 0.969660 0.119 Uiso 1 1 calc R U . . .
H23C H 0.384313 0.681521 0.916404 0.119 Uiso 1 1 calc R U . . .
C21 C 0.1070(3) 0.55928(17) 0.4447(4) 0.0931(15) Uani 1 1 d . . . . .
H21A H 0.163676 0.553366 0.395783 0.140 Uiso 1 1 calc R U . . .
H21B H 0.039509 0.562173 0.361331 0.140 Uiso 1 1 calc R U . . .
H21C H 0.105802 0.522119 0.513975 0.140 Uiso 1 1 calc R U . . .
C22 C 0.0109(3) 0.79778(18) 0.5039(5) 0.1026(16) Uani 1 1 d . . . . .
H22A H -0.063230 0.786561 0.486311 0.154 Uiso 1 1 calc R U . . .
H22B H 0.021788 0.811066 0.403049 0.154 Uiso 1 1 calc R U . . .
H22C H 0.030184 0.833714 0.580307 0.154 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.1750
-1 0 0 0.1520
-1 -1 1 0.1386
1 2 -2 0.2104
1 2 0 0.1137
-1 -2 0 0.1355
0 1 0 0.1330
0 -1 0 0.1300
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 As1 C9 98.78(12) . . ?
C4 As1 C1 98.13(12) . . ?
C1 As1 C9 97.47(11) . . ?
C6 S1 C2 92.78(16) . . ?
C8 S2 C3 92.60(16) . . ?
C3 C4 As1 123.9(2) . . ?
C3 C4 C7 112.8(3) . . ?
C7 C4 As1 123.1(2) . . ?
C10 C9 As1 117.2(2) . . ?
C14 C9 As1 123.9(2) . . ?
C14 C9 C10 118.9(3) . . ?
C2 C1 As1 124.3(2) . . ?
C2 C1 C5 112.9(3) . . ?
C5 C1 As1 122.8(2) . . ?
C4 C3 S2 109.4(2) . . ?
C4 C3 B1 128.4(3) . . ?
B1 C3 S2 122.2(2) . . ?
C1 C2 S1 109.4(2) . . ?
C1 C2 B1 128.0(3) . . ?
B1 C2 S1 122.5(2) . . ?
C6 C5 C1 112.3(3) . . ?
C9 C10 C11 120.3(3) . . ?
C9 C14 C13 120.3(3) . . ?
C8 C7 C4 113.3(3) . . ?
C5 C6 S1 112.7(3) . . ?
C15 C20 C23 120.9(3) . . ?
C19 C20 C15 119.7(3) . . ?
C19 C20 C23 119.4(3) . . ?
C20 C15 C16 118.2(3) . . ?
C20 C15 B1 122.2(3) . . ?
C16 C15 B1 119.6(3) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C13 C14 119.9(3) . . ?
C11 C12 C13 120.1(3) . . ?
C18 C19 C20 122.1(3) . . ?
C15 C16 C21 120.1(3) . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 C21 119.7(3) . . ?
C19 C18 C17 118.4(3) . . ?
C19 C18 C22 121.4(4) . . ?
C17 C18 C22 120.2(4) . . ?
C18 C17 C16 121.4(3) . . ?
C7 C8 S2 111.9(3) . . ?
C3 B1 C15 120.7(3) . . ?
C2 B1 C3 116.6(3) . . ?
C2 B1 C15 122.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 C4 1.929(3) . ?
As1 C9 1.977(3) . ?
As1 C1 1.941(3) . ?
S1 C2 1.730(3) . ?
S1 C6 1.690(3) . ?
S2 C3 1.732(3) . ?
S2 C8 1.701(3) . ?
C4 C3 1.389(4) . ?
C4 C7 1.410(4) . ?
C9 C10 1.383(4) . ?
C9 C14 1.379(4) . ?
C1 C2 1.394(4) . ?
C1 C5 1.420(4) . ?
C3 B1 1.535(4) . ?
C2 B1 1.518(5) . ?
C5 C6 1.354(4) . ?
C10 C11 1.388(4) . ?
C14 C13 1.396(4) . ?
C7 C8 1.348(4) . ?
C20 C15 1.398(4) . ?
C20 C19 1.397(4) . ?
C20 C23 1.513(4) . ?
C15 C16 1.408(4) . ?
C15 B1 1.580(4) . ?
C11 C12 1.361(5) . ?
C13 C12 1.370(4) . ?
C19 C18 1.369(5) . ?
C16 C17 1.389(4) . ?
C16 C21 1.516(4) . ?
C18 C17 1.380(5) . ?
C18 C22 1.518(4) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0013 -0.0003 0.0003 0.0248 0.0503 -0.0101
-1.0013 0.0003 -0.0003 -0.0248 -0.0503 0.0101
-1.0011 -1.0029 1.0005 -0.0057 -0.0141 0.0937
1.0008 2.0061 -2.0012 -0.0133 -0.0222 -0.1774
1.0033 2.0035 -0.0000 -0.0359 0.0749 -0.0367
-1.0033 -2.0035 0.0000 0.0359 -0.0749 0.0367
0.0010 1.0019 -0.0002 -0.0303 0.0123 -0.0133
-0.0010 -1.0019 0.0002 0.0303 -0.0123 0.0133
