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_4338948
_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 Co4 N4  O12 . 0.5NaNO3 . 8H2O'
_chemical_formula_sum            'C28 H36 Co4 N4.5 Na0.5 O21.5'
_chemical_formula_weight         1026.83
_chemical_name_common
'tetraoxotetracobalt(III)acetate tetrapyridine adduct'
_chemical_name_systematic
;
 tetrakis[(mu3-oxo)(mu-acetato)(pyridine)]tetracobalt(III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                92.187(2)
_cell_angle_beta                 91.111(2)
_cell_angle_gamma                103.145(2)
_cell_formula_units_Z            4
_cell_length_a                   10.122(1)
_cell_length_b                   11.177(1)
_cell_length_c                   36.620(4)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.22
_cell_volume                     4029.8(7)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            41472
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.9043
_exptl_absorpt_correction_T_min  0.6192
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         15780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+65.3776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                12046
_reflns_number_total             15780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011759.cif
_cod_data_source_block           1a-NaNO3
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C28 H36 Co4 N4.50 Na0.50 O21.50'
_cod_database_code               4338948