Bis(dinitrogen)cobalt(-I) Complexes with NHC Ligation: Synthesis, Characterization and Their Dinitrogen Functionalization Reactions Affording Side-On Bound Diazene Complexes.
Gao, Yafei; Li, Guangyu; Deng, Liang; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b11660

data_4127118
_publ_section_title
;
 Bis(dinitrogen)cobalt(-I) Complexes with NHC Ligation: Synthesis,
 Characterization and Their Dinitrogen Functionalization Reactions
 Affording Side-On Bound Diazene Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11660
_journal_year                    2018
_chemical_formula_moiety         'C45 H72 Cl Co N6'
_chemical_formula_sum            'C45 H72 Cl Co N6'
_chemical_formula_weight         791.46
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.610(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.844(3)
_cell_length_b                   20.328(5)
_cell_length_c                   36.842(9)
_cell_measurement_reflns_used    5544
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.25
_cell_volume                     8867(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_av_unetI/netI     0.1304
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            62074
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.492
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1231 before and 0.0947 after correction.
The Ratio of minimum to maximum transmission is 0.6171.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         17260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0857P)^2^+1.6877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10562
_reflns_number_total             17260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11660_si_001.cif
_cod_data_source_block           (ICy)3CoCl
_cod_database_code               4127118
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C15(H15), C23(H23), C29(H29), C37(H37), C43(H43), C51(H51), C57(H57),
 C65(H65), C71(H71), C79(H79), C85(H85)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C66(H66A,H66B), C67(H67A,H67B),
  C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C80(H80A,H80B),
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C86(H86A,H86B),
  C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C21(H21), C22(H22), C35(H35), C36(H36), C49(H49), C50(H50),
 C63(H63), C64(H64), C77(H77), C78(H78)
;
_shelx_res_checksum              17638
_shelx_hkl_checksum              81072
_olex2_submission_special_instructions 'No special instructions were received'