Four-coordinate triarylborane synthesis <i>via</i> cascade B-Cl/C-B cross-metathesis and C-H bond borylation.
Yang, Kai; Zhang, Guan; Song, Qiuling; Chemical science 9 (2018) 7666–7672; doi:10.1039/c8sc02281j

data_1549782
_publ_section_title
;
 Four-coordinate triarylborane synthesis <i>via</i> cascade B-Cl/C-B
 cross-metathesis and C-H bond borylation.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              7666
_journal_page_last               7672
_journal_paper_doi               10.1039/c8sc02281j
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C23 H19 B N2'
_chemical_formula_sum            'C23 H19 B N2'
_chemical_formula_weight         334.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc1ywxwm
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
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_audit_update_record
;
2018-01-02 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                115.915(13)
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_cell_length_b                   10.1909(12)
_cell_length_c                   10.8774(16)
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_cell_measurement_temperature    294.29(18)
_cell_measurement_theta_max      27.0320
_cell_measurement_theta_min      3.4200
_cell_volume                     905.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      294.29(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1213
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_diffrn_measured_fraction_theta_full 0.9984
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_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0729373000
_diffrn_orient_matrix_UB_12      0.0161726000
_diffrn_orient_matrix_UB_13      -0.0070460000
_diffrn_orient_matrix_UB_21      0.0253277000
_diffrn_orient_matrix_UB_22      0.0743022000
_diffrn_orient_matrix_UB_23      0.0200210000
_diffrn_orient_matrix_UB_31      -0.0120113000
_diffrn_orient_matrix_UB_32      -0.0186017000
_diffrn_orient_matrix_UB_33      -0.0734787000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
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_exptl_absorpt_correction_T_min  0.63015
_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.2264
_exptl_crystal_description       block
_exptl_crystal_F_000             352.1254
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_refine_diff_density_min         -0.4756
_refine_diff_density_rms         0.0651
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_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              10
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                1860
_reflns_number_total             3178
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8sc02281j2.cif
_cod_data_source_block           exp_4444
_cod_depositor_comments
'Adding full bibliography for 1549782--1549783.cif.'
_cod_database_code               1549782
_reflns_odcompleteness_completeness 99.84
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C3, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C3 \\sim C16: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
4.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.670
_oxdiff_exptl_absorpt_empirical_full_min 0.365