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_4074824
_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         'C29 H36 Co N5 O4'
_chemical_formula_sum            'C29 H36 Co N5 O4'
_chemical_formula_weight         577.56
_chemical_name_common            Oct-Co(gH)(dpgH)Py
_chemical_name_systematic
;
 trans-(glyoximato)(diphenylglyoximato)-octyl-(pyridine)-cobalt(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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.697(5)
_cell_angle_beta                 71.207(5)
_cell_angle_gamma                64.859(5)
_cell_formula_units_Z            2
_cell_length_a                   11.076(5)
_cell_length_b                   12.299(5)
_cell_length_c                   12.299(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     1435.2(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5136
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        <0.05
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.9387
_exptl_absorpt_correction_T_min  0.9387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XCAD-4
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0020(15)
_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   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.4275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                2635
_reflns_number_total             4849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050919xsi20051118_115145.cif
_cod_data_source_block           12b
_cod_original_cell_volume        1435.2(10)
_cod_database_code               4074824