Synthesis of a cobalt(IV) ketimide with a squashed tetrahedral geometry
Richard A. Lewis; Stephen P. George; Alon Chapovetsky; Guang Wu; Joshua S. Figueroa; Trevor W. Hayton; Chem.Commun. 49 (2013) 2888–; doi:10.1039/c3cc40461g

data_7109043
_publ_section_title
;
 Synthesis of a cobalt(IV) ketimide with a squashed tetrahedral geometry
;
_journal_name_full               Chem.Commun.
_journal_page_first              2888
_journal_paper_doi               10.1039/c3cc40461g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C36 H72 Co N4'
_chemical_formula_weight         619.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.220(3)
_cell_angle_beta                 78.481(3)
_cell_angle_gamma                73.509(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3082(9)
_cell_length_b                   11.5753(10)
_cell_length_c                   16.4021(14)
_cell_measurement_temperature    100(2)
_cell_volume                     1924.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31564
_diffrn_reflns_theta_full        25.26
_diffrn_reflns_theta_max         25.26
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+4.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                5459
_reflns_number_total             6849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40461g.txt
_cod_data_source_block           ac_1_84_0m
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109043