Cobalt-Catalyzed C(sp2)–C(sp3) Suzuki–Miyaura Cross-Coupling Enabled by Well-Defined Precatalysts with L,X-Type Ligands
Mills, L. Reginald; Gygi, David; Ludwig, Jacob R.; Simmons, Eric M.; Wisniewski, Steven R.; Kim, Junho; Chirik, Paul J.; ACS Catalysis  (2022) 1905–1918; doi:10.1021/acscatal.1c05586

data_4519286
_publ_section_title
;
 Cobalt-Catalyzed C(sp2)--C(sp3) Suzuki--Miyaura Cross-Coupling Enabled by
 Well-Defined Precatalysts with L,X-Type Ligands
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              1905
_journal_page_last               1918
_journal_paper_doi               10.1021/acscatal.1c05586
_journal_year                    2022
_chemical_formula_sum            'C58 H56 Cl8 Co2 N4 O8'
_chemical_formula_weight         1338.52
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 103.7380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9281(2)
_cell_length_b                   19.0648(4)
_cell_length_c                   16.0575(3)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.37
_cell_volume                     2952.37(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(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  0.0546
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            93498
_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         28.731
_diffrn_reflns_theta_min         2.112
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+2.5866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6682
_reflns_number_total             7666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c05586_si_004.cif
_cod_data_source_block           RM5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4519286
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.7101
_shelx_estimated_absorpt_t_max   0.7458
_shelx_res_checksum              81374
_shelx_hkl_checksum              20014