Unprecedented Stabilization of Cobalt(II) in a Tetrahedral S2O2 Environment: The Use of a Redox-Noninnocent Ligand
Núria Duran; William Clegg; Lourdes Cucurull-Sánchez; Robert A. Coxall; Hermas R. Jiménez; José-María Moratal; Francesc Lloret; Pilar González-Duarte; Inorganic Chemistry 39 (2000) 4821–4832; doi:10.1021/ic000223q

data_4321433
_publ_section_title
;
 Unprecedented Stabilization of Cobalt(II) in a Tetrahedral S2O2
 Environment: The Use of a Redox-Noninnocent Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4821
_journal_page_last               4832
_journal_paper_doi               10.1021/ic000223q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C72 H108 Co2 N3 Na3 O18 S6'
_chemical_formula_weight         1682.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.3925(13)
_cell_length_b                   16.3925(13)
_cell_length_c                   58.502(5)
_cell_measurement_reflns_used    10256
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.26
_cell_volume                     13614.2(19)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1053
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            26309
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.173
_refine_ls_goodness_of_fit_obs   1.152
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.198
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+45.3756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1573
_refine_ls_wR_factor_obs         0.1278
_reflns_number_observed          2649
_reflns_number_total             3658
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000223q_3.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+45.3756P] 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^)+(0.0512P)^2^+45.3756P] 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      'R -3 c'
_cod_database_code               4321433