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_4134787
_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         'C73 H110 Br0.195 Co2 N10.298, C6 H14'
_chemical_formula_sum            'C79 H124 Br0.19 Co2 N10.3'
_chemical_formula_weight         1351.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.437(2)
_cell_length_b                   16.9734(11)
_cell_length_c                   15.1227(11)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    99.96
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.83
_cell_volume                     7812.7(9)
_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      99.96
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59999
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         2.339
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 5837 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_coef       0.0027(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   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         17434
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0609P)^2^+3.0970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                14631
_reflns_number_total             17434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00291_si_005.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C79 H124 Br0.19 Co2 N10.30'
_cod_database_code               4134787
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C46(H46), C10(H10), C23(H23), C62(H62), C7(H7), C59(H59), C20(H20), C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C77(H77A,H77B), C76(H76A,H76B), C78(H78A,H78B), C75(H75A,H75B)
2.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C18(H18), C17(H17), C16(H16), C35(H35), C57(H57), C55(H55), C44(H44),
 C36(H36), C39(H39), C56(H56), C38(H38), C43(H43), C3(H3), C37(H37), C5(H5),
 C4(H4A), C42(H42)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C63(H63A,H63B,
 H63C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C60(H60A,H60B,H60C), C50(H50A,
 H50B,H50C), C30(H30A,H30B,H30C), C73(H73A,H73B,H73C), C29(H29A,H29B,H29C),
 C47(H47A,H47B,H47C), C67(H67A,H67B,H67C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C64(H64A,H64B,H64C), C11(H11A,H11B,H11C), C51(H51A,H51B,H51C), C68(H68A,H68B,
 H68C), C12(H12A,H12B,H12C), C48(H48A,H48B,H48C), C21(H21A,H21B,H21C), C24(H24A,
 H24B,H24C), C69(H69A,H69B,H69C), C79(H79A,H79B,H79C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C22(H22A,H22B,H22C), C61(H61A,H61B,H61C), C74(H74A,H74B,
 H74C)
;
_shelx_res_checksum              73978
_shelx_hkl_checksum              16530
_olex2_submission_special_instructions 'No special instructions were received'