Ligand Redox Non-Innocence in [Co<sup>III</sup>(TAML)]<sup>0/‒</sup> Complexes Affects Nitrene Formation.
van Leest, Nicolaas P.; Tepaske, Martijn A.; Oudsen, Jean-Pierre H; Venderbosch, Bas; Rietdijk, Niels R.; Siegler, Maxime A.; Tromp, Moniek; van der Vlugt, Jarl Ivar; de Bruin, Bas; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11715

data_4133875
_publ_section_title
;
 Ligand Redox Non-Innocence in [Co<sup>III</sup>(TAML)]<sup>0/--</sup>
 Complexes Affects Nitrene Formation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11715
_journal_year                    2019
_chemical_formula_sum            'C47 H48 Cl2 Co N4 O5 P'
_chemical_formula_weight         909.69
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6681(9)
_cell_length_b                   15.5580(10)
_cell_length_c                   19.0036(12)
_cell_measurement_reflns_used    197
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5474
_cell_measurement_theta_min      2.8711
_cell_volume                     4273.9(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            138208
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.143
_diffrn_reflns_theta_min         2.324
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'metallic dark brown-red'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.136
_exptl_transmission_factor_max   0.7460
_exptl_transmission_factor_min   0.7047
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         12575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0394
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9036
_reflns_number_total             12575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11715_si_002.cif
_cod_data_source_block           KvL_NR012_B_0m_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133875
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.921
_shelx_res_checksum              21377
_shelx_hkl_checksum              67291