NMR Spectroscopic Characterization of Methylcobalt(III) Compounds with Classical Ligands. Crystal Structures of [Co(NH3)5(CH3)]S2O6, trans-[Co(en)2(NH3)(CH3)]S2O6 (en = 1,2-Ethanediamine), and [Co(NH3)6]-mer,trans-[Co(NO2)3(NH3)2(CH3)]2-trans-[Co(NO2)4(NH3)2]
Pauli Kofod; Pernille Harris; Sine Larsen; Inorganic Chemistry 36 (1997) 2258–2266; doi:10.1021/ic961264i

data_4323443
_publ_contact_author             'Dr. Pauli Kofod'
_publ_contact_author_email       paulik@virgil.ruc.dk
_publ_section_title
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 NMR Spectroscopic Characterization of Methylcobalt(III) Compounds with
 Classical Ligands. Crystal Structures of [Co(NH3)5(CH3)]S2O6,
 trans-[Co(en)2(NH3)(CH3)]S2O6 (en = 1,2-Ethanediamine), and
 [Co(NH3)6]-mer,trans-[Co(NO2)3(NH3)2(CH3)]2-trans-[Co(NO2)4(NH3)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2258
_journal_page_last               2266
_journal_paper_doi               10.1021/ic961264i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         Co(C4H8)2(NH3)(CH3)S2O6
_chemical_formula_sum            'C5 H22 Co N5 O6 S2'
_chemical_formula_weight         371.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 90.000(3)
_cell_angle_gamma                90.000(3)
_cell_formula_units_Z            4
_cell_length_a                   12.211(3)
_cell_length_b                   10.107(3)
_cell_length_c                   11.514(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    122.0(5)
_cell_measurement_theta_max      22.53
_cell_measurement_theta_min      22.10
_cell_volume                     1421.0(7)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'DREADD (Blessing, 1987)'
_computing_molecular_graphics    'OrtepII (Johnson, 1976)'
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;
SHELXL-93 (Sheldrick, 1993) and PLATON (Spek, 1990) 
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122.0(5)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_number            8854
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_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.841
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_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
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_exptl_crystal_description       rod
_exptl_crystal_F_000             776
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_refine_diff_density_max         0.290
_refine_diff_density_min         -0.477
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
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_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.556
_refine_ls_restrained_S_obs      1.580
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_obs          0.0173
_refine_ls_shift/esd_max         0.159
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)]
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_obs         0.0500
_reflns_number_observed          2205
_reflns_number_total             2501
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_cod_data_source_block           pk21
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323443