N,B-Bidentate Boryl Ligand-Supported Iridium Catalyst for Efficient Functional-Group-Directed C-H Borylation.
Wang, Guanghui; Liu, Li; Wang, Hong; Ding, You-Song; Zhou, Jing; Mao, Shuai; Li, Pengfei; Journal of the American Chemical Society 139 (2017) 91–94; doi:10.1021/jacs.6b11867

data_4125396
_publ_section_title
;
 N,B-Bidentate Boryl Ligand-Supported Iridium Catalyst for Efficient
 Functional-Group-Directed C-H Borylation.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              91
_journal_page_last               94
_journal_paper_doi               10.1021/jacs.6b11867
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C27 H27 B Cl Ir N3 Si'
_chemical_formula_weight         660.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.047(7)
_cell_length_b                   11.047(7)
_cell_length_c                   42.43(3)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.34
_cell_volume                     5178(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            68674
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        24.830
_diffrn_reflns_theta_max         24.830
_diffrn_reflns_theta_min         1.905
_exptl_absorpt_coefficient_mu    5.327
_exptl_absorpt_correction_T_max  0.0637
_exptl_absorpt_correction_T_min  0.0306
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.258
_refine_diff_density_max         0.475
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.019(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0236
_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/[\s^2^(Fo^2^)+(0.0092P)^2^+12.6533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                4275
_reflns_number_total             4326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11867_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4125395--4125396.cif.'
_cod_original_cell_volume        5178(8)
_cod_database_code               4125396
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.182
_shelx_estimated_absorpt_t_max   0.340
_shelx_res_checksum              70928
_shelx_hkl_checksum              93648