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_4072679
_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         'C16 H17 Br Co N5 O4'
_chemical_formula_sum            'C16 H17 Br Co N5 O4'
_chemical_formula_weight         482.19
_chemical_name_common            2-Br-C6H4CH2-Co(gH)2Py
_chemical_name_systematic
;
 trans-bis(glyoximato)-2-bromo-benzyl-(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                 110.657(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9460(15)
_cell_length_b                   26.5150(4)
_cell_length_c                   8.1980(13)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      +28
_cell_measurement_theta_min      -28
_cell_volume                     1819.6(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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11844
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        <0.05
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.5990
_exptl_absorpt_correction_T_min  0.4703
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.243
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1435
_reflns_number_gt                3243
_reflns_number_total             4434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060940dsi20061012_013251.cif
_cod_data_source_block           4c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072679