Synthesis, structure, spectral and electrochemical properties, and catalytic use of cobalt(III)-oxo cubane clusters.
Chakrabarty, Rajesh; Bora, Sanchay J.; Das, Birinchi K.; Inorganic chemistry 46 (2007) 9450–9462; doi:10.1021/ic7011759

data_4338947
_publ_section_title
;
 Synthesis, structure, spectral and electrochemical properties, and
 catalytic use of cobalt(III)-oxo cubane clusters.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9450
_journal_page_last               9462
_journal_paper_doi               10.1021/ic7011759
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C28 H32 Cl Co4 N4 Na O19.50'
_chemical_formula_sum            'C28 H32 Cl Co4 N4 Na O19.5'
_chemical_formula_weight         1037.22
_chemical_name_systematic
;
tetrakis(m\3-oxo)tetrakis(\m-acetato)tetrakispyridine tetracobalt(III) NaClO~4~ 3.5H~2~O
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.398(4)
_cell_length_b                   12.398(4)
_cell_length_c                   53.97(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.5
_cell_volume                     8296(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1999)'
_computing_publication_material  'WindowsXP Professional, Wordpad'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Ditrect, 'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS CCD'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            28930
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  0.7699
_exptl_absorpt_correction_T_min  0.5916
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+4.1580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                3575
_reflns_number_total             3684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011759.cif
_cod_data_source_block           1a-NaClO4
_cod_original_cell_volume        8295(5)
_cod_original_sg_symbol_H-M      I-42d
_cod_original_formula_sum        'C28 H32 Cl Co4 N4 Na O19.50'
_cod_database_code               4338947