Cobaloximes with Mixed Dioximes of Glyoxime and Diphenylglyoxime: Synthesis, Characterization, CV, X-ray Studies, and Crystal Packing
Gupta, B. D.; Yamuna, R.; Mandal, Debaprasad; Organometallics 25 (2006) 706–; doi:10.1021/om050919x

data_4074823
_publ_section_title
;
 Cobaloximes with Mixed Dioximes of Glyoxime and Diphenylglyoxime:&#x00A0;
 Synthesis, Characterization, CV, X-ray Studies, and Crystal Packing
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              706
_journal_paper_doi               10.1021/om050919x
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C46 H48 Co2 N10 O8'
_chemical_formula_sum            'C23 H24 Co N5 O4'
_chemical_formula_weight         986.80
_chemical_name_common            CH3CH2Co(gH)(dpgH)Py
_chemical_name_systematic
;
 trans-(glyoximato)(diphenylglyoximato)-ethyl-(pyridine)-cobalt(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
_cell_angle_beta                 101.1360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9461(13)
_cell_length_b                   11.6249(6)
_cell_length_c                   15.6026(8)
_cell_measurement_reflns_used    8219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      +28.0
_cell_measurement_theta_min      -28.0
_cell_volume                     4439.5(4)
_computing_cell_refinement       'SMART 5.628 (BRUKER, 2003)'
_computing_data_collection       'SMART 5.628 (BRUKER, 2003)'
_computing_data_reduction        'SAINT+ 6.45 (BRUKER, 2003)'
_computing_molecular_graphics    'Diamond 2.1'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \f/\w
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28839
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        <0.005
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.8673
_exptl_absorpt_correction_T_min  0.7982
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+3.2928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                9099
_reflns_number_total             10946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050919xsi20051118_115145.cif
_cod_data_source_block           6b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4074823