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_4130724
_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 H54 B Co N4 O2 P2'
_chemical_formula_weight         622.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.647(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9557(4)
_cell_length_b                   16.1170(6)
_cell_length_c                   20.4822(9)
_cell_measurement_reflns_used    9209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.79
_cell_measurement_theta_min      2.43
_cell_volume                     3249.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR 92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.796
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         12887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0391P)^2^+1.6028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8586
_reflns_number_total             12887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06144_si_002.cif
_cod_data_source_block           jvo5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130724
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2014-3
_shelx_res_checksum              7274
_shelx_hkl_checksum              8470