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_4134786
_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         '3(C68 H106 Co2 N8), 6.833(C4.552)'
_chemical_formula_sum            'C235.11 H318 Co6 N24'
_chemical_formula_weight         3834.02
_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             2020-01-02
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                78.769(2)
_cell_angle_beta                 73.599(2)
_cell_angle_gamma                68.813(2)
_cell_formula_units_Z            1
_cell_length_a                   15.7471(7)
_cell_length_b                   18.5697(7)
_cell_length_c                   23.0557(10)
_cell_measurement_reflns_used    9631
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.24
_cell_volume                     5997.9(4)
_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  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0603
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            216026
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.057
_diffrn_reflns_theta_min         2.059
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.9316.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             2059
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         31911
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+5.3951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23858
_reflns_number_total             31911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00291_si_006.cif
_cod_data_source_block           6
_cod_database_code               4134786
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C117-C118 \\sim C116-C117
 with sigma of 0.02
3. Others
 Fixed Sof: C116(0.5) C4AA(0.5) C115(0.5) C5BA(0.5) C6BA(0.5) C114(0.5)
 C2BA(0.5) C113(0.5)
4.a Ternary CH refined with riding coordinates:
 C23(H23), C7(H7), C10(H10), C57(H57), C88(H88), C20(H20), C54(H54), C41(H41),
 C75(H75), C91(H91), C78(H78), C44(H44)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N12(H12), N8(H8), C16(H16), C18(H18), C84(H84), C17(H17), C51(H51),
 C85(H85), C86(H86), C52(H52), C50(H50), C3(H3), C5(H5), C4(H4A), C71(H71),
 C73(H73), C72(H72), C37(H37), C39(H39), C38(H38)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C62(H62A,H62B,
 H62C), C22(H22A,H22B,H22C), C64(H64A,H64B,H64C), C90(H90A,H90B,H90C), C56(H56A,
 H56B,H56C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C25(H25A,H25B,H25C),
 C63(H63A,H63B,H63C), C29(H29A,H29B,H29C), C42(H42A,H42B,H42C), C11(H11A,H11B,
 H11C), C21(H21A,H21B,H21C), C89(H89A,H89B,H89C), C55(H55A,H55B,H55C), C67(H67A,
 H67B,H67C), C59(H59A,H59B,H59C), C101(H10A,H10B,H10C), C66(H66A,H66B,H66C),
 C58(H58A,H58B,H58C), C43(H43A,H43B,H43C), C33(H33A,H33B,H33C), C68(H68A,H68B,
 H68C), C30(H30A,H30B,H30C), C79(H79A,H79B,H79C), C32(H32A,H32B,H32C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C34(H34A,H34B,H34C), C45(H45A,H45B,H45C),
 C102(H10D,H10E,H10F), C76(H76A,H76B,H76C), C80(H80A,H80B,H80C), C97(H97A,H97B,
 H97C), C46(H46A,H46B,H46C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C77(H77A,
 H77B,H77C), C100(H10G,H10H,H10I)
;
_shelx_res_checksum              25906
_shelx_hkl_checksum              84602
_olex2_submission_special_instructions 'No special instructions were received'