Syntheses and Characterization of Organo-Group 14 Cobaloxime Compounds
Alan M. Stolzenberg; Sarah R. Workman; Jessica E. Gutshall; Jeffrey L. Petersen; Novruz Akhmedov; Inorganic Chemistry 46 (2007) 6744–6754; doi:10.1021/ic070251+

data_4327255
_publ_contact_author_address
;Department of Chemistry
West Virginia University
PO Box 6045
Morgantown, WV 26506-6045
;
_publ_contact_author_email       astolzen@wvu.edu
_publ_contact_author_fax         '304 293-4904'
_publ_contact_author_name        'Alan M. Stolzenberg'
_publ_contact_author_phone       '304 293-3435 x6437'
_publ_section_title
;
 Syntheses and Characterization of Organo-Group 14 Cobaloxime Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6744
_journal_page_last               6754
_journal_paper_doi               10.1021/ic070251+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C17 H27 Co N5 O4'
_chemical_formula_weight         424.37
_chemical_name_common            Co(DH)2(4-t-BuPy)
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9821(11)
_cell_length_b                   9.7449(6)
_cell_length_c                   22.7374(15)
_cell_measurement_reflns_used    6703
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.26
_cell_volume                     3984.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24743
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4557
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0612P)^2^+0.8382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                3560
_reflns_number_total             4557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0702512B2B-file002_1.cif
_cod_data_source_block           as9ccd
_cod_database_code               4327255