Isolation and Characterization of a Trinuclear Cobalt Complex Containing Trigonal-Prismatic Cobalt in Secondary Alcohol Aerobic Oxidation
Karthikeyan, I.; Alamsetti, S. K.; Sekar, G.; Organometallics 33 (2014) 1665–; doi:10.1021/om500003d

data_4082944
_publ_section_title
;
 Isolation and Characterization of a Trinuclear Cobalt Complex Containing
 Trigonal-Prismatic Cobalt in Secondary Alcohol Aerobic Oxidation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1665
_journal_paper_doi               10.1021/om500003d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C76 H72 Co3 N6 O15'
_chemical_formula_weight         1486.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.096(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.163(2)
_cell_length_b                   17.1312(12)
_cell_length_c                   18.0064(13)
_cell_measurement_reflns_used    8344
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.3
_cell_volume                     7621.0(9)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21884
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,1999)
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.333
_refine_ls_extinction_coef       0.0051(5)
_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_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5519
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1490P)^2^+27.7316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2275
_refine_ls_wR_factor_ref         0.2604
_reflns_number_gt                4032
_reflns_number_total             5519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500003d_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 4082944.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4082944