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_4323442
_publ_contact_author             'Dr. Pauli Kofod'
_publ_contact_author_email       paulik@virgil.ruc.dk
_publ_section_title
;
 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(NH3)5(CH3) S2O6'
_chemical_formula_sum            'C H18 Co N5 O6 S2'
_chemical_formula_weight         319.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.280(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4856(9)
_cell_length_b                   18.0720(11)
_cell_length_c                   9.7854(14)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    122.0(5)
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      18.28
_cell_volume                     1135.0(2)
_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)'
_computing_publication_material
;
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
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13575
_diffrn_reflns_theta_max         39.99
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       rod
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.763
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         -0.039
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.6270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_obs         0.0728
_reflns_number_observed          5331
_reflns_number_total             6948
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961264i_1.cif
_cod_data_source_block           pauli2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.6270P] where P=(Fo^2^+2Fc^2^)/3' 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^)+(0.0226P)^2^+0.6270P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4323442