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_4327257
_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            'C35 H42 Co N5 O4 Pb'
_chemical_formula_weight         862.86
_chemical_name_common            (4-t-BuPy)Co(DH)2(PbPh3)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.348(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0104(7)
_cell_length_b                   15.7693(8)
_cell_length_c                   16.6230(8)
_cell_measurement_reflns_used    7941
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.58
_cell_volume                     3584.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25077
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.196
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method
'diethylether layered over methylene chloride'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.0993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                6663
_reflns_number_total             8169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0702512B2B-file002_3.cif
_cod_data_source_block           as309ccd
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4327257