Direct Manipulation of Metal Imido Geometry: Key Principles to Enhance C-H Amination Efficacy.
Baek, Yunjung; Hennessy, Elisabeth T.; Betley, Theodore A.; Journal of the American Chemical Society 141 (2019) 16944–16953; doi:10.1021/jacs.9b09015

data_4127963
_publ_section_title
;
 Direct Manipulation of Metal Imido Geometry: Key Principles to Enhance
 C-H Amination Efficacy.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16944
_journal_page_last               16953
_journal_paper_doi               10.1021/jacs.9b09015
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C68 H57 Co N2'
_chemical_formula_weight         961.08
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.266(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.870(3)
_cell_length_b                   16.390(3)
_cell_length_c                   18.057(3)
_cell_measurement_reflns_used    2616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.49
_cell_volume                     4988.8(15)
_computing_cell_refinement       'SAINT 8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT 8.37A (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29814
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.116
_diffrn_reflns_theta_max         25.116
_diffrn_reflns_theta_min         1.208
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0461P)^2^+1.4897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5312
_reflns_number_total             8840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09015_si_002.cif
_cod_data_source_block           (TrL)Co
_cod_original_cell_volume        4988.8(16)
_cod_database_code               4127963
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              9878
_shelx_hkl_checksum              21758