(Benzenethiolato-<i>S</i>)(4-<i>tert</i>-butylpyridine-<i>N</i>)bis(dimethylglyoximato-<i>N</i>,<i>N</i>')cobalt(III) and (4-<i>tert</i>-Butylpyridine-<i>N</i>)bis(dimethylglyoximato-<i>N</i>,<i>N</i>')(4-methoxybenzenethiolato-<i>S</i>)cobalt(III)
Inouye, Yoshinobu; Kambe, Tohru; Tada, Masaru; Acta Crystallographica Section C 54 (1998) 945–947; doi:10.1107/S0108270198001693

data_2007464
_publ_section_title
;(Benzenethiolato-<i>S</i>)(4-<i>tert</i>-butylpyridine-<i>N</i>)bis(dimethylglyoximato-<i>N</i>,<i>N</i>')cobalt(III)
 and
 (4-<i>tert</i>-Butylpyridine-<i>N</i>)bis(dimethylglyoximato-<i>N</i>,<i>N</i>')(4-methoxybenzenethiolato-<i>S</i>)cobalt(III)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              945
_journal_page_last               947
_journal_paper_doi               10.1107/S0108270198001693
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Co (C4 H7 N2 O2)2 (C9 H13 N) (C6 H5 S)]'
_chemical_formula_sum            'C23 H32 Co N5 O4 S'
_chemical_formula_weight         533.53
_chemical_melting_point          204.5(5)
_chemical_name_common            Co(DH)~2~(4-^t^Bu-Py)(PhS)
_chemical_name_systematic
; Bis(dimethylglyoximato)(benzenethiolato)(4-tert-
butylpyridine)Cobalt(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.630(6)
_cell_length_b                   10.9850(10)
_cell_length_c                   9.779(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.85
_cell_measurement_theta_min      11.56
_cell_volume                     2538.0(10)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_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  0.018
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4588
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of independent and constrained refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_obs          .034
_refine_ls_shift/esd_max         -0.025
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.0976P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.090
_refine_ls_wR_factor_obs         .084
_reflns_number_observed          3615
_reflns_number_total             4469
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            oa1029.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '204--205' was changed to '204.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '204--205' was changed to '204.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.0976P] 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^)+(0.0433P)^2^+1.0976P] 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 /a'
_cod_original_formula_sum        'C23 H32 Co1 N5 O4 S1'
_cod_database_code               2007464