Evaluation of Cobalt Complexes Bearing Tridentate Pincer Ligands for Catalytic C‒H Borylation
Schaefer, Brian A.; Margulieux, Grant W.; Small, Brooke L.; Chirik, Paul J.; Organometallics 34 (2015) 1307–; doi:10.1021/acs.organomet.5b00044

data_4087386
_publ_section_title
;
 Evaluation of Cobalt Complexes Bearing Tridentate Pincer Ligands for
 Catalytic C--H Borylation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1307
_journal_paper_doi               10.1021/acs.organomet.5b00044
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C44 H105 B2 Co2 N2 P4'
_chemical_formula_weight         925.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5055(4)
_cell_length_b                   33.6528(9)
_cell_length_c                   10.8926(3)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      3.32
_cell_volume                     5317.2(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 'ACTA 50'
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26522
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.783
_diffrn_reflns_theta_min         2.626
_exptl_absorpt_coefficient_mu    6.227
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.212(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+49.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2116
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                7537
_reflns_number_total             8772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00044_si_003.cif
_cod_data_source_block           bs36
_cod_database_code               4087386
_shelxl_version_number           2014-3
_shelx_res_checksum              55232
_shelx_hkl_checksum              32537