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#$Date: 2023-10-21 02:03:11 +0300 (Sat, 21 Oct 2023) $
#$Revision: 287064 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/42/7714259.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_7714259
loop_
_publ_author_name
'Sokolnicki, Tomasz'
'Alharbi, Mashael'
'van Ingen, Yara'
'Rahim, Shahnaz'
'Pramanik, Milan'
'Roldan, Alberto'
'Walkowiak, Jedrzej'
'Melen, Rebecca'
_publ_section_title
;
 Reactivity of a series of triaryl borates, B(OArx)3, in hydroboration
 catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03333C
_journal_year                    2023
_chemical_formula_moiety         'C18 H9 B Cl6 O3'
_chemical_formula_sum            'C18 H9 B Cl6 O3'
_chemical_formula_weight         496.76
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-12 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.3506(7)
_cell_length_b                   13.3506(7)
_cell_length_c                   21.3882(14)
_cell_measurement_reflns_used    1465
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.1570
_cell_measurement_theta_min      4.1600
_cell_volume                     3301.5(3)
_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    'shelxle, Mercury, ORTEP, CorelDraw'
_computing_publication_material  publCIF
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'w/ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            2890
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.774
_diffrn_reflns_theta_min         3.651
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.218
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0917P)²+12.1021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1346
_reflns_number_total             1738
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03333c2.cif
_cod_data_source_block           rm2318_a_sq
_cod_original_cell_volume        3301.5(4)
_cod_database_code               7714259
_shelx_shelxl_version_number     2018/3
_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_min   0.827
_shelx_estimated_absorpt_t_max   0.845
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
B1 B 0.666667 0.333333 0.5216(2) 0.0301(9) Uani 1 3 d S T P . .
Cl2 Cl 0.85675(10) 0.47582(10) 0.39537(4) 0.0721(4) Uani 1 1 d . . . . .
Cl02 Cl 0.84120(12) 0.49189(11) 0.64518(5) 0.0884(5) Uani 1 1 d . . . . .
O003 O 0.78331(16) 0.37994(16) 0.52189(10) 0.0406(5) Uani 1 1 d . . . . .
C005 C 0.8604(2) 0.4970(2) 0.52041(14) 0.0386(6) Uani 1 1 d . . . . .
C006 C 0.9072(3) 0.5524(3) 0.46425(16) 0.0444(7) Uani 1 1 d . . . . .
C008 C 0.9946(3) 0.6662(3) 0.4628(2) 0.0576(10) Uani 1 1 d . . . . .
H008 H 1.027272 0.702565 0.424007 0.069 Uiso 1 1 calc R U . . .
C009 C 0.8991(3) 0.5598(3) 0.57483(17) 0.0543(8) Uani 1 1 d . . . . .
C00A C 0.9866(3) 0.6761(3) 0.5737(2) 0.0682(11) Uani 1 1 d . . . . .
H00A H 1.012671 0.719463 0.611327 0.082 Uiso 1 1 calc R U . . .
C00B C 1.0339(3) 0.7263(3) 0.5173(2) 0.0677(12) Uani 1 1 d . . . . .
H00B H 1.095106 0.804285 0.516257 0.081 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O003 B1 O003 119.998(5) 3_665 2_655 ?
O003 B1 O003 119.999(5) 3_665 . ?
O003 B1 O003 119.997(5) 2_655 . ?
B1 O003 C005 123.76(18) . . ?
C009 C005 O003 120.8(3) . . ?
C009 C005 C006 118.4(3) . . ?
O003 C005 C006 120.6(3) . . ?
C008 C006 C005 121.1(3) . . ?
C008 C006 Cl2 119.9(3) . . ?
C005 C006 Cl2 119.0(2) . . ?
C00B C008 C006 119.6(4) . . ?
C005 C009 C00A 120.8(4) . . ?
C005 C009 Cl02 118.9(2) . . ?
C00A C009 Cl02 120.2(3) . . ?
C00B C00A C009 118.8(4) . . ?
C008 C00B C00A 121.2(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
B1 O003 1.3577(19) 3_665 ?
B1 O003 1.3577(19) 2_655 ?
B1 O003 1.3577(19) . ?
Cl2 C006 1.727(4) . ?
Cl02 C009 1.727(4) . ?
O003 C005 1.376(3) . ?
C005 C009 1.376(5) . ?
C005 C006 1.385(4) . ?
C006 C008 1.377(5) . ?
C008 C00B 1.364(6) . ?
C009 C00A 1.401(5) . ?
C00A C00B 1.370(6) . ?
