Low-Valent Chemistry of Cobalt Amide. Synthesis and Structural Characterization of Cobalt(II) Amido, Aryloxide, and Thiolate Compounds
Hung Kay Lee; Chung Hei Lam; Song-Lin Li; Ze-Ying Zhang; Thomas C. W. Mak; Inorganic Chemistry 40 (2001) 4691–4695; doi:10.1021/ic0102945

data_4320198
_publ_section_title
;
 Low-Valent Chemistry of Cobalt Amide. Synthesis and Structural
 Characterization of Cobalt(II) Amido, Aryloxide, and Thiolate Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4691
_journal_page_last               4695
_journal_paper_doi               10.1021/ic0102945
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C42 H74 Co N2 S2'
_chemical_formula_weight         730.08
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.177(5)
_cell_length_b                   11.056(2)
_cell_length_c                   17.263(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4423.6(16)
_computing_cell_refinement       'Biotex Rigaku'
_computing_data_collection       'Raxis-IIc Rigaku'
_computing_data_reduction        'Biotex Rigaku'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SIemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Raxis-IIc Rigaku'
_diffrn_measurement_method       IP
_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  0.1509
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10495
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  1.263
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1266P)^2^+0.4512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                3222
_reflns_number_total             3857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0102945.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4423.6(15)
_cod_database_code               4320198