Isolation of a Bimetallic Cobalt(III) Nitride and Examination of Its Hydrogen Atom Abstraction Chemistry and Reactivity Towards H2.
Sengupta, Debabrata; Sandoval-Pauker, Christian; Schueller, Emily C.; Encerrado-Manriquez, Angela M; Metta-Magana, Alejandro J; Lee, Wen-Yee; Seshadri, Ram; Pintér, Balázs; Fortier, Skye; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00291

data_4134784
_publ_section_title
;
 Isolation of a Bimetallic Cobalt(III) Nitride and Examination of Its
 Hydrogen Atom Abstraction Chemistry and Reactivity Towards H2.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00291
_journal_year                    2020
_chemical_formula_moiety         'C38 H60 Br Co N3 O'
_chemical_formula_sum            'C38 H60 Br Co N3 O'
_chemical_formula_weight         713.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.604(2)
_cell_length_b                   12.1480(6)
_cell_length_c                   15.6435(10)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.96
_cell_volume                     7526.2(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2689
_diffrn_reflns_av_unetI/netI     0.1732
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65294
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00012(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.1980
_refine_ls_R_factor_gt           0.1156
_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^)+70.8376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             7556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00291_si_003.cif
_cod_data_source_block           2
_cod_database_code               4134784
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C20(H20), C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C35(H35A,H35B), C37(H37A,H37B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C5(H5), C4(H4), C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              29554
_shelx_hkl_checksum              80691
_olex2_submission_special_instructions 'No special instructions were received'