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_4338949
_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         'C32 H40 Co4 N4 O15'
_chemical_formula_sum            'C32 H34 Co4 N4 O15'
_chemical_formula_weight         961.72
_chemical_name_systematic
;
tetrakis(m\-oxo)tetrakis(m\-acetato)tetrakis(4-methylpyridine) tetracobalt(III) 3H~2~O
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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            4
_cell_length_a                   16.733(2)
_cell_length_b                   17.510(2)
_cell_length_c                   13.1904(18)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      1.7
_cell_volume                     3864.7(8)
_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 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21687
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                2569
_reflns_number_total             4653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011759.cif
_cod_data_source_block           1b-3H2O
_cod_original_cell_volume        3864.7(9)
_cod_original_sg_symbol_H-M      Pnnm
_cod_database_code               4338949