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_7109042
_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            'C52 H104 Co Li N4 O8'
_chemical_formula_weight         979.26
_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   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.668(2)
_cell_angle_beta                 74.519(2)
_cell_angle_gamma                89.944(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5073(4)
_cell_length_b                   13.5432(4)
_cell_length_c                   16.3252(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2877.23(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31151
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9336
_exptl_absorpt_correction_T_min  0.9027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         14294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                11106
_reflns_number_total             14294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40461g.txt
_cod_data_source_block           Complex_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109042