Axial Ligand Exchange of N-heterocyclic Cobalt(III) Schiff Base Complexes: Molecular Structure and NMR Solution Dynamics
Lisa M. Manus; Robert J. Holbrook; Tulay A. Atesin; Marie C. Heffern; Allison S. Harney; Amanda L. Eckermann; Thomas J. Meade; Inorganic Chemistry 52 (2013) 1069–1076; doi:10.1021/ic302379j

data_4333640
_publ_section_title
;
 Axial Ligand Exchange of N-heterocyclic Cobalt(III) Schiff Base
 Complexes: Molecular Structure and NMR Solution Dynamics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1069
_journal_page_last               1076
_journal_paper_doi               10.1021/ic302379j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C20 H30 Co N6 O2, C24 H20 B, 2(C2 H6 O) '
_chemical_formula_sum            'C48 H62 B Co N6 O4'
_chemical_formula_weight         856.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                90.00
_cell_angle_beta                 97.6470(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9254(5)
_cell_length_b                   18.0542(6)
_cell_length_c                   17.8151(6)
_cell_measurement_reflns_used    9722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.26
_cell_volume                     4439.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76376
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         12872
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                9315
_reflns_number_total             12872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302379j_si_002_4.cif
_cod_data_source_block           Co(acacen)(NMeIm)2
_cod_database_code               4333640