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_4134788
_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         'C84 H130 Co2 N13 Na O4, C6'
_chemical_formula_sum            'C90 H130 Co2 N13 Na O4'
_chemical_formula_weight         1598.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-09
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                70.454(4)
_cell_angle_beta                 72.443(3)
_cell_angle_gamma                70.308(4)
_cell_formula_units_Z            1
_cell_length_a                   12.4567(9)
_cell_length_b                   12.6505(10)
_cell_length_c                   16.5318(12)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.976
_cell_measurement_theta_min      2.68
_cell_volume                     2258.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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  0.1183
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            85809
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.976
_diffrn_reflns_theta_min         1.922
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         11738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0632P)^2^+3.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9441
_reflns_number_total             11738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00291_si_002.cif
_cod_data_source_block           1
_cod_database_code               4134788
_shelx_shelxl_version_number     2017/1
_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), C7(H7), C20(H20), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C42(H42A,H42B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C18(H18), C16(H16), C17(H17), C40(H40), C35(H35),
 C36(H36)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C9(H9A,H9B,H9C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C),
 C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C22(H22A,H22B,
 H22C), C11(H11A,H11B,H11C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C32(H32A,
 H32B,H32C), C12(H12A,H12B,H12C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              56031
_shelx_hkl_checksum              65581
_olex2_submission_special_instructions 'No special instructions were received'