Catalytic Properties of Cobalt(III)-Oxo Cubanes in the TBHP Oxidation of Benzylic Alcohols
Rajesh Chakrabarty; Purabi Sarmah; Bapan Saha; Stutee Chakravorty; Birinchi K. Das; Inorganic Chemistry 48 (2009) 6371–6379; doi:10.1021/ic802115n

data_4302600
_publ_contact_author_address
; Department of Chemistry
  Gauhati University
  Guwahati - 781 014
  India
;
_publ_contact_author_email       das_bk@rediffmail.com
_publ_contact_author_fax         '91 361 2700311'
_publ_contact_author_name        'Prof. Birinchi K. Das'
_publ_contact_author_phone       '91 361 2570535'
_publ_section_title
;
Catalytic Properties of Cobalt(III)-Oxo Cubanes in the TBHP Oxidation of
Benzylic Alcohols
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6371
_journal_page_last               6379
_journal_paper_doi               10.1021/ic802115n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C52 H48 Co4 N4 O12, 5(H2 O), 3.5(C1 H4 O)'
_chemical_formula_sum            'C55.5 H72 Co4 N4 O20.5'
_chemical_formula_weight         1359.03
_chemical_name_systematic
;
 tetrakis(\m-oxo)tetrakis(\m-benzoato)tetrakis-4-methylpyridine tetracobalt(III)
3.5MeOH 5H~2~O
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 123.2980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.7305(7)
_cell_length_b                   15.1874(5)
_cell_length_c                   20.7240(7)
_cell_measurement_reflns_used    3286
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      1.2
_cell_volume                     6242.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1015
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.8339
_exptl_absorpt_correction_T_min  0.8006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            olive-green
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
contributions.  Total electron count found = 244/unit cell.
Calculated for 3.5 methanol (the reaction solvent)
= 244/unit cell.  The intensive properties (density, F(000), etc.)
reflect these contributions
;
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0919P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                3379
_reflns_number_total             5734
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic802115n_si_001_2.cif
_cod_data_source_block           cobzmepy
_cod_original_cell_volume        6242.8(3)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4302600