NMR Spectroscopic and X-ray Crystallographic Study of Methylcobalt(III) Compounds with Saturated Amine Ligands
Pauli Kofod; Pernille Harris; Inorganic Chemistry 43 (2004) 2680–2688; doi:10.1021/ic0302682

data_4310834
_publ_section_title
;
 NMR Spectroscopic and X-ray Crystallographic Study of Methylcobalt(III)
 Compounds with Saturated Amine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2680
_journal_page_last               2688
_journal_paper_doi               10.1021/ic0302682
_journal_volume                  43
_journal_year                    2004
_chemical_absolute_configuration 'racemic twin'
_chemical_formula_sum            'C5 H22 Cl4 Co N5 Zn'
_chemical_formula_weight         418.38
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   7.654(2)
_cell_length_b                   13.368(2)
_cell_length_c                   14.662(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1500.2(5)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
EvalCCD (Duisenberg, 1998) and DREAD (Blessing, 1987)
;
_computing_molecular_graphics    'Ortep II (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD'
_diffrn_measurement_method       '\q and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            91306
_diffrn_reflns_theta_full        45.01
_diffrn_reflns_theta_max         45.01
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    3.400
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.296
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.492(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         12359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0306
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                11668
_reflns_number_total             12359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302682_s1_4.cif
_cod_data_source_block           shelxlpk65
_cod_database_code               4310834