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_4107528
_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_moiety         '[C40 H52 Fe N4 O]+, (C32 H12 B F24)-'
_chemical_formula_sum            'C72 H64 B F24 Fe N4 O'
_chemical_formula_weight         1523.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.431(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7624(2)
_cell_length_b                   29.4794(4)
_cell_length_c                   18.9134(3)
_cell_measurement_temperature    120(2)
_cell_volume                     7083.81(19)
_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      120(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
'2000 images at 0.5 deg. stepwise rotation in omega and phi, 90 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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            149135
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         16234
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0615P)^2^+8.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                14313
_reflns_number_total             16234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710663n-file003_09.cif
_cod_data_source_block           complex3oxTHF-120K
_cod_original_cell_volume        7083.81(18)
_cod_database_code               4107528