Cobalt-Catalyzed C(sp(2))-H Borylation: Mechanistic Insights Inspire Catalyst Design.
Obligacion, Jennifer V.; Semproni, Scott P.; Pappas, Iraklis; Chirik, Paul J.; Journal of the American Chemical Society 138 (2016) 10645–10653; doi:10.1021/jacs.6b06144

data_4130726
_publ_section_title
;
 Cobalt-Catalyzed C(sp(2))-H Borylation: Mechanistic Insights Inspire
 Catalyst Design.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10645
_journal_page_last               10653
_journal_paper_doi               10.1021/jacs.6b06144
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C29 H56 B Ir N2 O2 P2'
_chemical_formula_weight         729.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 114.9260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5000(3)
_cell_length_b                   17.9686(6)
_cell_length_c                   10.8015(4)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.37
_cell_volume                     1672.09(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31391
_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         27.518
_diffrn_reflns_theta_min         2.364
_exptl_absorpt_coefficient_mu    4.115
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.034
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.352(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         7699
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0256P)^2^+0.1120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7512
_reflns_number_total             7699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06144_si_002.cif
_cod_data_source_block           jvo13
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4130726
_shelxl_version_number           2014-3
_shelx_res_checksum              92625
_shelx_hkl_checksum              65570