Cobalt-Catalyzed C(sp2)–H Borylation with an Air-Stable, Readily Prepared Terpyridine Cobalt(II) Bis(acetate) Precatalyst
Léonard, Nadia G.; Bezdek, Máté J.; Chirik, Paul J.; Organometallics 36 (2017) 142–; doi:10.1021/acs.organomet.6b00630

data_4086757
_publ_section_title
;
 Cobalt-Catalyzed C(sp2)--H Borylation with an Air-Stable, Readily
 Prepared Terpyridine Cobalt(II) Bis(acetate) Precatalyst
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              142
_journal_paper_doi               10.1021/acs.organomet.6b00630
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C20 H36 B2 Co O12'
_chemical_formula_weight         549.04
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-06-17 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   30.5500(14)
_cell_length_b                   30.5500(14)
_cell_length_c                   8.2057(4)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.31
_cell_volume                     6632.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP 3 (Farraguia, 1997)'
_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 0.981
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            24080
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         2.309
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             2601
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0669P)^2^+16.9070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3140
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00630_si_002.cif
_cod_data_source_block           nl9
_cod_depositor_comments
'Adding full bibliography for 4086756--4086757.cif.'
_cod_original_cell_volume        6632.4(7)
_cod_database_code               4086757
_shelxl_version_number           2014-3
_shelx_res_checksum              78487
_shelx_hkl_checksum              1366
_shelx_fab_checksum              90020