#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:53:06 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714772.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_7714772
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             2022-10-29
_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                 106.771(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0015(8)
_cell_length_b                   20.0469(10)
_cell_length_c                   8.4791(6)
_cell_measurement_reflns_used    3250
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.5060
_cell_measurement_theta_min      3.2090
_cell_volume                     2116.0(2)
_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      173.15
_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    -14.00  29.00   0.50    1.00    --   30.00  54.00 -30.00   86
  2  ω    -68.00 114.00   0.50    1.00    --   30.00  54.00-120.00  364
;
_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      0.0253958000
_diffrn_orient_matrix_UB_12      -0.0313967000
_diffrn_orient_matrix_UB_13      0.0010848000
_diffrn_orient_matrix_UB_21      0.0492261000
_diffrn_orient_matrix_UB_22      0.0163215000
_diffrn_orient_matrix_UB_23      0.0050205000
_diffrn_orient_matrix_UB_31      0.0133727000
_diffrn_orient_matrix_UB_32      -0.0005536000
_diffrn_orient_matrix_UB_33      0.0872186000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0574
_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       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8427
_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         26.371
_diffrn_reflns_theta_min         2.609
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.809
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.848
_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    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.584
_exptl_crystal_size_mid          0.438
_exptl_crystal_size_min          0.283
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0306
_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/[σ²(Fo²)+(0.0253P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3406
_reflns_number_total             4324
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           3e@173k
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_database_code               7714772
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHSAsB
_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   0.631
_shelx_estimated_absorpt_t_min   0.420
_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:
 C7(H7), C10(H10), C14(H14), C5(H5), C8(H8), C11(H11), C13(H13), C6(H6),
 C12(H12), C18(H18), C17(H17)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.813
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 0.58446(2) 0.58596(2) 0.12554(3) 0.02133(8) Uani 1 1 d . . . . .
S2 S 0.55082(5) 0.39245(3) 0.36641(8) 0.02975(16) Uani 1 1 d . . . . .
S1 S 0.86773(5) 0.47623(3) 0.06450(9) 0.03443(18) Uani 1 1 d . . . . .
C9 C 0.64921(18) 0.63889(11) 0.3258(3) 0.0211(5) Uani 1 1 d . . . . .
C4 C 0.54833(19) 0.50736(11) 0.2334(3) 0.0206(5) Uani 1 1 d . . . . .
C1 C 0.71501(18) 0.55262(11) 0.0880(3) 0.0216(5) Uani 1 1 d . . . . .
C2 C 0.75850(19) 0.48991(11) 0.1387(3) 0.0232(5) Uani 1 1 d . . . . .
C7 C 0.44960(19) 0.50108(12) 0.2721(3) 0.0249(6) Uani 1 1 d . . . . .
H7 H 0.395865 0.534722 0.250314 0.030 Uiso 1 1 calc R U . . .
C10 C 0.5848(2) 0.68746(11) 0.3675(3) 0.0273(6) Uani 1 1 d . . . . .
H10 H 0.513237 0.693898 0.300138 0.033 Uiso 1 1 calc R U . . .
C3 C 0.61394(19) 0.45127(11) 0.2770(3) 0.0226(5) Uani 1 1 d . . . . .
C14 C 0.7541(2) 0.63064(12) 0.4257(3) 0.0278(6) Uani 1 1 d . . . . .
H14 H 0.798984 0.597836 0.398668 0.033 Uiso 1 1 calc R U . . .
C5 C 0.7710(2) 0.58778(11) -0.0058(3) 0.0275(6) Uani 1 1 d . . . . .
H5 H 0.752078 0.631367 -0.048155 0.033 Uiso 1 1 calc R U . . .
C8 C 0.44045(19) 0.44145(12) 0.3441(3) 0.0287(6) Uani 1 1 d . . . . .
H8 H 0.379671 0.428696 0.377883 0.034 Uiso 1 1 calc R U . . .
C11 C 0.6249(2) 0.72645(12) 0.5071(3) 0.0351(7) Uani 1 1 d . . . . .
H11 H 0.580337 0.759272 0.534924 0.042 Uiso 1 1 calc R U . . .
C15 C 0.79081(19) 0.37339(11) 0.3094(3) 0.0262(6) Uani 1 1 d . . . . .
C19 C 0.7710(2) 0.31229(11) 0.2244(3) 0.0288(6) Uani 1 1 d . . . . .
C13 C 0.7935(2) 0.67021(12) 0.5647(3) 0.0334(6) Uani 1 1 d . . . . .
H13 H 0.865279 0.664463 0.631986 0.040 Uiso 1 1 calc R U . . .
C6 C 0.8554(2) 0.55250(13) -0.0290(4) 0.0356(7) Uani 1 1 d . . . . .
H6 H 0.901439 0.568401 -0.089709 0.043 Uiso 1 1 calc R U . . .
C12 C 0.7286(2) 0.71790(12) 0.6056(3) 0.0368(7) Uani 1 1 d . . . . .
H12 H 0.755548 0.744636 0.701128 0.044 Uiso 1 1 calc R U . . .
C23 C 0.9212(2) 0.26136(14) 0.4292(4) 0.0378(7) Uani 1 1 d . . . . .
C18 C 0.8360(2) 0.25730(12) 0.2872(4) 0.0346(7) Uani 1 1 d . . . . .
H18 H 0.821162 0.215887 0.230735 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8761(2) 0.37743(13) 0.4558(3) 0.0332(6) Uani 1 1 d . . . . .
C17 C 0.9408(2) 0.32173(14) 0.5108(4) 0.0379(7) Uani 1 1 d . . . . .
H17 H 0.999933 0.325433 0.607222 0.046 Uiso 1 1 calc R U . . .
C22 C 0.6818(2) 0.30534(13) 0.0656(4) 0.0443(8) Uani 1 1 d . . . . .
H22A H 0.612927 0.316079 0.085163 0.066 Uiso 1 1 calc R U . . .
H22B H 0.679908 0.259414 0.025336 0.066 Uiso 1 1 calc R U . . .
H22C H 0.694545 0.336023 -0.016713 0.066 Uiso 1 1 calc R U . . .
B1 B 0.7208(2) 0.43778(13) 0.2430(3) 0.0238(6) Uani 1 1 d . . . . .
C20 C 0.8960(3) 0.44104(14) 0.5561(4) 0.0506(9) Uani 1 1 d . . . . .
H20A H 0.896571 0.479017 0.483557 0.076 Uiso 1 1 calc R U . . .
H20B H 0.965430 0.438129 0.640741 0.076 Uiso 1 1 calc R U . . .
H20C H 0.838768 0.447193 0.608845 0.076 Uiso 1 1 calc R U . . .
C21 C 0.9907(3) 0.20058(14) 0.4955(4) 0.0551(9) Uani 1 1 d . . . . .
H21A H 0.981305 0.187599 0.601907 0.083 Uiso 1 1 calc R U . . .
H21B H 1.066349 0.211514 0.509780 0.083 Uiso 1 1 calc R U . . .
H21C H 0.969246 0.163540 0.417482 0.083 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
2 1 0 0.1240
-2 -1 0 0.2109
-2 -1 2 0.1771
0 0 -1 0.2641
0 1 0 0.1108
0 -1 0 0.1726
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 97.58(9) . . ?
C1 As1 C9 98.67(9) . . ?
C1 As1 C4 98.04(10) . . ?
C8 S2 C3 92.82(12) . . ?
C6 S1 C2 92.86(12) . . ?
C10 C9 As1 117.09(17) . . ?
C14 C9 As1 124.02(18) . . ?
C14 C9 C10 118.9(2) . . ?
C7 C4 As1 122.51(17) . . ?
C3 C4 As1 124.41(19) . . ?
C3 C4 C7 113.1(2) . . ?
C2 C1 As1 123.88(18) . . ?
C2 C1 C5 113.2(2) . . ?
C5 C1 As1 122.69(17) . . ?
C1 C2 S1 109.40(18) . . ?
C1 C2 B1 128.5(2) . . ?
B1 C2 S1 122.14(17) . . ?
C8 C7 C4 112.5(2) . . ?
C11 C10 C9 120.3(2) . . ?
C4 C3 S2 109.52(18) . . ?
C4 C3 B1 127.9(2) . . ?
B1 C3 S2 122.39(17) . . ?
C13 C14 C9 120.3(2) . . ?
C6 C5 C1 112.9(2) . . ?
C7 C8 S2 112.07(19) . . ?
C12 C11 C10 120.5(2) . . ?
C19 C15 C16 118.9(2) . . ?
C19 C15 B1 121.7(2) . . ?
C16 C15 B1 119.4(2) . . ?
C15 C19 C22 121.2(2) . . ?
C18 C19 C15 119.4(2) . . ?
C18 C19 C22 119.5(2) . . ?
C12 C13 C14 120.3(2) . . ?
C5 C6 S1 111.6(2) . . ?
C11 C12 C13 119.7(2) . . ?
C18 C23 C21 121.0(3) . . ?
C17 C23 C18 118.2(2) . . ?
C17 C23 C21 120.8(3) . . ?
C23 C18 C19 122.0(3) . . ?
C15 C16 C20 120.5(2) . . ?
C17 C16 C15 119.6(2) . . ?
C17 C16 C20 119.9(2) . . ?
C23 C17 C16 121.9(3) . . ?
C2 B1 C15 120.8(2) . . ?
C3 B1 C2 116.6(2) . . ?
C3 B1 C15 122.6(2) . . ?
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 C9 1.973(2) . ?
As1 C4 1.946(2) . ?
As1 C1 1.934(2) . ?
S2 C3 1.731(2) . ?
S2 C8 1.704(3) . ?
S1 C2 1.733(3) . ?
S1 C6 1.709(3) . ?
C9 C10 1.395(3) . ?
C9 C14 1.392(3) . ?
C4 C7 1.419(3) . ?
C4 C3 1.395(3) . ?
C1 C2 1.395(3) . ?
C1 C5 1.411(3) . ?
C2 B1 1.538(4) . ?
C7 C8 1.363(3) . ?
C10 C11 1.388(3) . ?
C3 B1 1.522(4) . ?
C14 C13 1.390(3) . ?
C5 C6 1.366(4) . ?
C11 C12 1.377(4) . ?
C15 C19 1.407(3) . ?
C15 C16 1.408(3) . ?
C15 B1 1.586(3) . ?
C19 C18 1.398(3) . ?
C19 C22 1.509(4) . ?
C13 C12 1.383(4) . ?
C23 C18 1.384(4) . ?
C23 C17 1.381(4) . ?
C23 C21 1.525(3) . ?
C16 C17 1.395(3) . ?
C16 C20 1.513(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
1.9999 1.0001 -0.0002 0.0194 0.1148 0.0262
-1.9999 -1.0001 0.0002 -0.0194 -0.1148 -0.0262
-1.9997 -0.9996 2.0003 -0.0172 -0.1047 0.1483
-0.0001 -0.0002 -1.0000 -0.0011 -0.0050 -0.0872
-0.0001 1.0000 -0.0001 -0.0314 0.0163 -0.0006
0.0001 -1.0000 0.0001 0.0314 -0.0163 0.0006
