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_4127122
_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         'C60 H96 Co2 Cs2 N16, C4 H10 O'
_chemical_formula_sum            'C64 H106 Co2 Cs2 N16 O'
_chemical_formula_weight         1499.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                72.988(3)
_cell_angle_beta                 88.920(3)
_cell_angle_gamma                63.187(3)
_cell_formula_units_Z            2
_cell_length_a                   16.342(3)
_cell_length_b                   16.350(3)
_cell_length_c                   16.365(3)
_cell_measurement_reflns_used    3656
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.44
_cell_measurement_theta_min      2.16
_cell_volume                     3698.8(12)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.0644
_diffrn_reflns_av_unetI/netI     0.1304
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30102
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.604
_diffrn_reflns_theta_min         1.631
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0880 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.6927.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         16970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9217
_reflns_number_total             16970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11660_si_001.cif
_cod_data_source_block           2c
_cod_original_cell_volume        3699.0(10)
_cod_database_code               4127122
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.810
_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:
 C7(H7), C13(H13), C21(H21), C27(H27), C34(H34), C35(H35), C41(H41), C49(H49),
 C55(H55)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
  C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C19(H19), C20(H20), C33(H33), C47(H47), C48(H48)
2.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              79163
_shelx_hkl_checksum              45054
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'