Substrate Redox Non-innocence Inducing Stepwise Oxidative Addition Reaction: Nitrosoarene C-N Bond Cleavage on Low-Coordinate Cobalt(0) Species.
Wang, Dongyang; Leng, Xuebing; Ye, Shengfa; Deng, Liang; Journal of the American Chemical Society 141 (2019) 7731–7735; doi:10.1021/jacs.9b03726

data_4127228
_publ_section_title
;
 Substrate Redox Non-innocence Inducing Stepwise Oxidative Addition
 Reaction: Nitrosoarene C-N Bond Cleavage on Low-Coordinate Cobalt(0)
 Species.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7731
_journal_page_last               7735
_journal_paper_doi               10.1021/jacs.9b03726
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C63 H94 Co N4 O2'
_chemical_formula_sum            'C63 H94 Co N4 O2'
_chemical_formula_weight         998.35
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.489(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.8430(7)
_cell_length_b                   11.3664(2)
_cell_length_c                   20.0835(5)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      53.359
_cell_measurement_theta_min      3.875
_cell_volume                     6452.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.085
_diffrn_reflns_theta_min         3.874
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1143 before and 0.0718 after correction. The Ratio of minimum to maximum transmission is 0.6670. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         12283
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+1.4730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8523
_reflns_number_total             12283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03726_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4127227--4127228.cif.'
_cod_database_code               4127228
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C25 \\sim C27 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C32(H32), C48(H48), C50(H50)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C)
;
_shelx_res_checksum              70283
_shelx_hkl_checksum              77630
_shelx_fab_checksum              18209
_olex2_submission_special_instructions 'No special instructions were received'