Stabilization of a cobalt-cobalt bond by two cyclic alkyl amino carbenes.
Mondal, Kartik Chandra; Samuel, Prinson P.; Roesky, Herbert W.; Carl, Elena; Herbst-Irmer, Regine; Stalke, Dietmar; Schwederski, Brigitte; Kaim, Wolfgang; Ungur, Liviu; Chibotaru, Liviu F.; Hermann, Markus; Frenking, Gernot; Journal of the American Chemical Society 136 (2014) 1770–1773; doi:10.1021/ja4123285

data_4120565
_publ_section_title
;
 Stabilization of a cobalt-cobalt bond by two cyclic alkyl amino carbenes.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1770
_journal_page_last               1773
_journal_paper_doi               10.1021/ja4123285
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C40 H62 Cl6 Co2 Li N2, C20 H32 N, C4 H8 O'
_chemical_formula_sum            'C64 H102 Cl6 Co2 Li N3 O'
_chemical_formula_weight         1266.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.322(2)
_cell_length_b                   25.322(2)
_cell_length_c                   10.553(2)
_cell_measurement_reflns_used    8924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.278
_cell_measurement_theta_min      2.24
_cell_volume                     6766.6(15)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            101142
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_min         1.137
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       needle
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 4532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         12397
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0201P)^2^+1.8688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10659
_reflns_number_total             12397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4123285_si_002.cif
_cod_data_source_block           sad_a
_cod_original_cell_volume        6766.6(17)
_cod_database_code               4120565
_shelxl_version_number           2013-4
_shelx_res_checksum              16999
_shelx_hkl_checksum              86652