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_4134785
_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         'C68 H104 Co2 N12, 2(C4 O)'
_chemical_formula_sum            'C76 H104 Co2 N12 O2'
_chemical_formula_weight         1335.57
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.993(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7543(14)
_cell_length_b                   21.2404(15)
_cell_length_c                   10.2959(9)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.23
_cell_volume                     3880.3(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            53267
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.404
_diffrn_reflns_theta_min         2.488
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1697 before and 0.0959 after correction.
The Ratio of minimum to maximum transmission is 0.7334.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9639
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0658P)^2^+4.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7604
_reflns_number_total             9639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00291_si_004.cif
_cod_data_source_block           3b
_cod_database_code               4134785
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.870
_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
Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.05
3. Others
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(2)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(3)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C10(H10), C7(H7), C23(H23)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C4(H4), C18(H18), C17(H17)
4.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C11(H11A,H11B,
 H11C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C29(H29A,
 H29B,H29C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C),
 C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              4903
_shelx_hkl_checksum              30527
_olex2_submission_special_instructions 'No special instructions were received'