Neutral Bis(α-iminopyridine)metal Complexes of the First-Row Transition Ions (Cr, Mn, Fe, Co, Ni, Zn) and Their Monocationic Analogues: Mixed Valency Involving a Redox Noninnocent Ligand System
Connie C. Lu; Eckhard Bill; Thomas Weyhermüller; Eberhard Bothe; Karl Wieghardt; Journal of the American Chemical Society 130 (2008) 3181–3197; doi:10.1021/ja710663n

data_4107523
_publ_section_title
;
 Neutral Bis(\a-iminopyridine)metal Complexes of the First-Row Transition
 Ions (Cr, Mn, Fe, Co, Ni, Zn) and Their Monocationic Analogues: Mixed
 Valency Involving a Redox Noninnocent Ligand System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3181
_journal_page_last               3197
_journal_paper_doi               10.1021/ja710663n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C36 H44 Co N4'
_chemical_formula_weight         591.68
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.704(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3884(3)
_cell_length_b                   18.4602(6)
_cell_length_c                   18.3906(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3131.85(18)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'747 images at 1.0 deg. stepwise rotation in omega and phi, 92 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70888
_diffrn_reflns_theta_full        33.17
_diffrn_reflns_theta_max         33.17
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7696
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         23746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0377P)^2^+0.4349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                20802
_reflns_number_total             23746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710663n-file003_04.cif
_cod_data_source_block           complex4
_cod_database_code               4107523