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_4333641
_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
'2(C20 H28 N6 O2 Co), 2Cl, 1.75(H2 O), 0.6(C2 H6 O)'
_chemical_formula_sum            'C41.2 H63.1 Cl2 Co2 N12 O6.35'
_chemical_formula_weight         1016.90
_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                 100.328(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.8162(9)
_cell_length_b                   11.6873(4)
_cell_length_c                   16.9470(6)
_cell_measurement_reflns_used    4635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.20
_cell_volume                     4835.6(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1431
_diffrn_reflns_av_sigmaI/netI    0.1293
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41559
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         0.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.9699
_exptl_absorpt_correction_T_min  0.7070
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         10981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                5642
_reflns_number_total             10981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302379j_si_002_5.cif
_cod_data_source_block           Co(acacen)(2MeIm)2
_cod_original_formula_sum        'C41.20 H63.10 Cl2 Co2 N12 O6.35'
_cod_database_code               4333641