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_4310833
_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_formula_sum            'C9 H25 Cl Co N7 O4'
_chemical_formula_weight         389.74
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 146.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.145(2)
_cell_length_b                   22.277(3)
_cell_length_c                   13.070(2)
_cell_measurement_temperature    122(2)
_cell_volume                     1628.2(14)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.031
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51968
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.011
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.951
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_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          0.2037
_refine_ls_wR_factor_ref         0.2235
_reflns_number_gt                3459
_reflns_number_total             3744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302682_s1_3.cif
_cod_data_source_block           shelxlpk64
_cod_original_cell_volume        1628.3(13)
_cod_database_code               4310833