#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:53:06 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714782.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_7714782
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         'C27 H24 B P'
_chemical_formula_sum            'C27 H24 B P'
_chemical_formula_weight         390.24
_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             2023-05-08
_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                91.366(4)
_cell_angle_beta                 104.231(4)
_cell_angle_gamma                105.148(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1146(4)
_cell_length_b                   10.9100(6)
_cell_length_c                   11.5623(5)
_cell_measurement_reflns_used    3132
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      32.4710
_cell_measurement_theta_min      2.9540
_cell_volume                     1070.97(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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      100.05
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     61.00 101.00   0.50    1.00    --   30.00  54.00-180.00   80
  2  ω    -73.00  30.00   0.50    1.00    --   30.00  54.00  60.00  206
  3  ω    -72.00  31.00   0.50    1.00    --   30.00  54.00 -60.00  206
  4  ω    -73.00  33.00   0.50    1.00    --   30.00  54.00-180.00  212
;
_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      0.0236948000
_diffrn_orient_matrix_UB_12      -0.0520793000
_diffrn_orient_matrix_UB_13      -0.0196348000
_diffrn_orient_matrix_UB_21      -0.0414702000
_diffrn_orient_matrix_UB_22      0.0037537000
_diffrn_orient_matrix_UB_23      -0.0597671000
_diffrn_orient_matrix_UB_31      0.0685166000
_diffrn_orient_matrix_UB_32      0.0430207000
_diffrn_orient_matrix_UB_33      -0.0091424000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          1.007
_exptl_crystal_size_mid          0.704
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0468
_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)+(0.0628P)²+0.4079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3711
_reflns_number_total             4371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03798c2.cif
_cod_data_source_block           phosphaborin@100k
_cod_depositor_comments
'Adding full bibliography for 7714770--7714783.cif.'
_cod_database_code               7714782
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHBP
_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   0.974
_shelx_estimated_absorpt_t_min   0.873
_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:
 C8(H8), C9(H9), C12(H12), C7(H7), C10(H10), C5(H5), C14(H14), C18(H18),
 C23(H23), C11(H11), C6(H6), C15(H15), C17(H17), C21(H21), C16(H16)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), 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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.843
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
P1 P 0.68820(5) 0.77239(4) 0.91031(4) 0.01776(15) Uani 1 1 d . . . . .
C3 C 0.88388(19) 0.67378(16) 0.79683(14) 0.0159(4) Uani 1 1 d . . . . .
C4 C 0.8539(2) 0.78130(17) 0.84678(15) 0.0169(4) Uani 1 1 d . . . . .
C2 C 0.5989(2) 0.51872(17) 0.79797(15) 0.0167(4) Uani 1 1 d . . . . .
C19 C 0.80647(19) 0.42525(16) 0.71455(15) 0.0164(4) Uani 1 1 d . . . . .
C24 C 0.85441(19) 0.33259(17) 0.78495(15) 0.0172(4) Uani 1 1 d . . . . .
C8 C 0.4862(2) 0.39895(17) 0.76491(15) 0.0198(4) Uani 1 1 d . . . . .
H8 H 0.512443 0.332599 0.726792 0.024 Uiso 1 1 calc R U . . .
C9 C 0.9622(2) 0.90148(17) 0.85936(16) 0.0201(4) Uani 1 1 d . . . . .
H9 H 0.940102 0.973429 0.891757 0.024 Uiso 1 1 calc R U . . .
C12 C 1.0284(2) 0.69268(17) 0.76571(15) 0.0181(4) Uani 1 1 d . . . . .
H12 H 1.052545 0.621509 0.733915 0.022 Uiso 1 1 calc R U . . .
C1 C 0.5552(2) 0.61566(17) 0.85315(15) 0.0173(4) Uani 1 1 d . . . . .
C20 C 0.8034(2) 0.41631(17) 0.59196(15) 0.0196(4) Uani 1 1 d . . . . .
C7 C 0.3389(2) 0.37480(18) 0.78608(17) 0.0226(4) Uani 1 1 d . . . . .
H7 H 0.265901 0.292892 0.763449 0.027 Uiso 1 1 calc R U . . .
C10 C 1.1004(2) 0.91721(18) 0.82548(16) 0.0214(4) Uani 1 1 d . . . . .
H10 H 1.171660 0.999717 0.832964 0.026 Uiso 1 1 calc R U . . .
C13 C 0.5899(2) 0.87599(17) 0.81689(16) 0.0179(4) Uani 1 1 d . . . . .
C5 C 0.4057(2) 0.59031(18) 0.87500(17) 0.0223(4) Uani 1 1 d . . . . .
H5 H 0.377906 0.655418 0.913628 0.027 Uiso 1 1 calc R U . . .
C14 C 0.5772(2) 0.98668(17) 0.87178(17) 0.0209(4) Uani 1 1 d . . . . .
H14 H 0.618350 1.006196 0.955970 0.025 Uiso 1 1 calc R U . . .
C18 C 0.5286(2) 0.84915(18) 0.69323(16) 0.0221(4) Uani 1 1 d . . . . .
H18 H 0.536090 0.774014 0.654620 0.026 Uiso 1 1 calc R U . . .
C23 C 0.9016(2) 0.23672(17) 0.73461(16) 0.0210(4) Uani 1 1 d . . . . .
H23 H 0.933789 0.174875 0.783630 0.025 Uiso 1 1 calc R U . . .
C11 C 1.1354(2) 0.81159(18) 0.78017(16) 0.0219(4) Uani 1 1 d . . . . .
H11 H 1.232174 0.821379 0.759419 0.026 Uiso 1 1 calc R U . . .
C22 C 0.9028(2) 0.22927(18) 0.61494(17) 0.0240(4) Uani 1 1 d . . . . .
C6 C 0.2986(2) 0.47177(19) 0.84094(17) 0.0248(4) Uani 1 1 d . . . . .
H6 H 0.197198 0.456271 0.854952 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5046(2) 1.06869(18) 0.80424(18) 0.0259(4) Uani 1 1 d . . . . .
H15 H 0.495856 1.143600 0.842382 0.031 Uiso 1 1 calc R U . . .
C27 C 0.8600(2) 0.33672(18) 0.91660(16) 0.0224(4) Uani 1 1 d . . . . .
H27A H 0.962829 0.390472 0.963017 0.034 Uiso 1 1 calc R U . . .
H27B H 0.844051 0.250158 0.941834 0.034 Uiso 1 1 calc R U . . .
H27C H 0.776850 0.372224 0.930428 0.034 Uiso 1 1 calc R U . . .
C17 C 0.4569(2) 0.93119(19) 0.62624(17) 0.0257(4) Uani 1 1 d . . . . .
H17 H 0.415509 0.912219 0.542015 0.031 Uiso 1 1 calc R U . . .
C21 C 0.8520(2) 0.31971(18) 0.54469(16) 0.0237(4) Uani 1 1 d . . . . .
H21 H 0.850404 0.315415 0.462219 0.028 Uiso 1 1 calc R U . . .
C25 C 0.7465(2) 0.50996(19) 0.51053(16) 0.0265(4) Uani 1 1 d . . . . .
H25A H 0.660029 0.532345 0.534386 0.040 Uiso 1 1 calc R U . . .
H25B H 0.709171 0.471170 0.427546 0.040 Uiso 1 1 calc R U . . .
H25C H 0.833244 0.587121 0.516837 0.040 Uiso 1 1 calc R U . . .
C16 C 0.4453(2) 1.04118(19) 0.68207(18) 0.0269(4) Uani 1 1 d . . . . .
H16 H 0.396528 1.097519 0.635894 0.032 Uiso 1 1 calc R U . . .
B1 B 0.7628(2) 0.53952(19) 0.77087(16) 0.0158(4) Uani 1 1 d . . . . .
C26 C 0.9570(3) 0.1263(2) 0.5623(2) 0.0379(5) Uani 1 1 d . . . . .
H26A H 1.070724 0.156346 0.571146 0.057 Uiso 1 1 calc R U . . .
H26B H 0.901788 0.106056 0.477108 0.057 Uiso 1 1 calc R U . . .
H26C H 0.933814 0.049621 0.604543 0.057 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
0 -1 0 0.1109
0 1 0 0.0809
0 1 -1 0.1374
0 -1 1 0.2332
1 0 0 0.4652
-1 0 0 0.2547
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 P1 C13 100.58(8) . . ?
C1 P1 C4 104.18(8) . . ?
C1 P1 C13 101.59(8) . . ?
C4 C3 C12 117.35(15) . . ?
C4 C3 B1 122.78(15) . . ?
C12 C3 B1 119.83(15) . . ?
C3 C4 P1 123.66(13) . . ?
C9 C4 P1 116.01(13) . . ?
C9 C4 C3 120.09(15) . . ?
C8 C2 C1 117.33(15) . . ?
C8 C2 B1 119.56(15) . . ?
C1 C2 B1 123.10(16) . . ?
C24 C19 C20 118.26(16) . . ?
C24 C19 B1 121.33(14) . . ?
C20 C19 B1 120.38(15) . . ?
C19 C24 C27 120.84(15) . . ?
C23 C24 C19 120.27(15) . . ?
C23 C24 C27 118.88(16) . . ?
C7 C8 C2 122.27(17) . . ?
C10 C9 C4 121.09(16) . . ?
C11 C12 C3 122.00(16) . . ?
C2 C1 P1 123.62(13) . . ?
C5 C1 P1 116.08(13) . . ?
C5 C1 C2 120.12(16) . . ?
C19 C20 C25 120.71(16) . . ?
C21 C20 C19 119.97(17) . . ?
C21 C20 C25 119.32(15) . . ?
C8 C7 C6 119.37(17) . . ?
C9 C10 C11 119.86(17) . . ?
C14 C13 P1 118.58(14) . . ?
C18 C13 P1 122.65(14) . . ?
C18 C13 C14 118.77(17) . . ?
C6 C5 C1 120.72(17) . . ?
C15 C14 C13 120.57(17) . . ?
C17 C18 C13 120.51(18) . . ?
C22 C23 C24 121.78(17) . . ?
C12 C11 C10 119.55(16) . . ?
C23 C22 C21 117.83(16) . . ?
C23 C22 C26 121.14(18) . . ?
C21 C22 C26 121.03(17) . . ?
C5 C6 C7 120.18(16) . . ?
C16 C15 C14 119.95(18) . . ?
C18 C17 C16 120.09(18) . . ?
C22 C21 C20 121.85(16) . . ?
C15 C16 C17 120.11(18) . . ?
C3 B1 C2 120.50(15) . . ?
C3 B1 C19 119.16(15) . . ?
C2 B1 C19 120.33(15) . . ?
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
P1 C4 1.8173(17) . ?
P1 C1 1.8165(19) . ?
P1 C13 1.8324(18) . ?
C3 C4 1.413(2) . ?
C3 C12 1.414(2) . ?
C3 B1 1.557(3) . ?
C4 C9 1.399(2) . ?
C2 C8 1.411(2) . ?
C2 C1 1.413(2) . ?
C2 B1 1.561(2) . ?
C19 C24 1.404(2) . ?
C19 C20 1.411(2) . ?
C19 B1 1.576(2) . ?
C24 C23 1.395(2) . ?
C24 C27 1.510(2) . ?
C8 C7 1.382(2) . ?
C9 C10 1.380(2) . ?
C12 C11 1.382(3) . ?
C1 C5 1.404(2) . ?
C20 C21 1.393(2) . ?
C20 C25 1.511(3) . ?
C7 C6 1.394(3) . ?
C10 C11 1.396(3) . ?
C13 C14 1.396(2) . ?
C13 C18 1.394(3) . ?
C5 C6 1.381(3) . ?
C14 C15 1.392(3) . ?
C18 C17 1.385(3) . ?
C23 C22 1.387(3) . ?
C22 C21 1.393(3) . ?
C22 C26 1.511(3) . ?
C15 C16 1.377(3) . ?
C17 C16 1.389(3) . ?
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
0.0003 -1.0004 0.0010 0.0521 -0.0038 -0.0430
-0.0003 1.0004 -0.0010 -0.0521 0.0038 0.0430
-0.0001 0.9973 -1.0001 -0.0323 0.0635 0.0520
0.0001 -0.9973 1.0001 0.0323 -0.0635 -0.0520
1.0017 -0.0000 -0.0009 0.0238 -0.0415 0.0686
-1.0017 0.0000 0.0009 -0.0238 0.0415 -0.0686
