Hindered Rotation Leading to Nonequivalence in 2-Substituted Benzyl Cobaloximes: Structure−Property Relationship†
Mandal, Debaprasad; Gupta, B. D.; Organometallics 26 (2007) 658–; doi:10.1021/om060940d

data_4072676
_publ_section_title
;
 Hindered Rotation Leading to Nonequivalence in 2-Substituted Benzyl
 Cobaloximes:&#x00A0; Structure&#x2212;Property Relationship&#x2020;
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              658
_journal_paper_doi               10.1021/om060940d
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C21 H28 Co N5 O4'
_chemical_formula_sum            'C21 H28 Co N5 O4'
_chemical_formula_weight         473.41
_chemical_name_common            (2-Me)C6H4CH2Co(dmgH)2Py
_chemical_name_systematic
;
  trans-bis(dimethylglyoximato)-ortho-methyl-benzyl-(pyridine)-cobalt(III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                77.278(5)
_cell_angle_beta                 76.152(5)
_cell_angle_gamma                70.892(5)
_cell_formula_units_Z            2
_cell_length_a                   8.147(5)
_cell_length_b                   10.658(5)
_cell_length_c                   13.759(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                     1082.9(9)
_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 0.576
_diffrn_measured_fraction_theta_max 0.576
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 Mach2'
_diffrn_measurement_method       'theta-2theta 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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2367
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        <0.05
_diffrn_standards_interval_time  1h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.8649
_exptl_absorpt_correction_T_min  0.8068
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   XCAD4
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                1381
_reflns_number_total             2194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060940dsi20061012_013251.cif
_cod_data_source_block           2a
_cod_database_code               4072676