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_4333639
_publ_contact_author_email       tmeade@northwestern.edu
_publ_contact_author_name        'Thomas J. Meade'
_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_absolute_configuration ad
_chemical_formula_moiety         'Br, C22 H28 Co N4 O2, 2(C H4 O)'
_chemical_formula_sum            'C24 H36 Br Co N4 O4'
_chemical_formula_weight         583.41
_chemical_name_systematic
;
 trans-bis(pyridine)-(N,N'-ethylene-bis(acetylacetoniminato))
-cobalt(iii) bromide ethanol solvate 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-05
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.538(5)
_cell_length_b                   14.372(3)
_cell_length_c                   15.616(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5282.7(19)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.14
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6300
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.597253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0692 before and 0.0471 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1002 before and 0.0519 after correction.
 The Ratio of minimum to maximum transmission is 0.80.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.188
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.109(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         6300
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0180P)^2^+15.7602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                6153
_reflns_number_total             6300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302379j_si_002_3.cif
_cod_data_source_block           Co(acacen)(Py)2
_cod_original_cell_volume        5282.6(18)
_cod_database_code               4333639