Characterization of a Tricationic trigonal Bipyramidal Iron(IV) Cyanide Complex, with a Very High Reduction Potential, and Its Iron(II) and Iron(III) Congeners
Jason England; Erik R. Farquhar; Yisong Guo; Matthew A. Cranswick; Kallol Ray; Eckard Münck; Lawrence Que; Inorganic Chemistry 50 (2011) 2885–2896; doi:10.1021/ic102094d

data_4324757
_publ_contact_author_address
;Department of Chemistry and Center for Metals in Biocatalysis
University of Minnesota
207 Pleasant St. SE
Minneapolis
MN 55455
USA
;
_publ_contact_author_email       larryque@umn.edu
_publ_contact_author_fax         +1(612)6247029
_publ_contact_author_name        'Professor Lawrence Que, Jr.'
_publ_contact_author_phone       +1(612)6250389
_publ_section_title
;
 Characterization of a Tricationic trigonal Bipyramidal Iron(IV) Cyanide
 Complex, with a Very High Reduction Potential, and Its Iron(II) and
 Iron(III) Congeners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2885
_journal_page_last               2896
_journal_paper_doi               10.1021/ic102094d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C22 H48 Fe N11, 0.91(C F3 O3 S), 1.09(F6 Sb), C2 H3 N'
_chemical_formula_sum            'C24.91 H51 F9.28 Fe N12 O2.72 S0.91 Sb1.09'
_chemical_formula_weight         956.46
_chemical_name_common            10093a
_chemical_name_systematic
;
  ?
;
_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                 98.969(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0565(13)
_cell_length_b                   22.044(3)
_cell_length_c                   20.036(3)
_cell_measurement_reflns_used    2906
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.77
_cell_volume                     3951.1(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            46455
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldick, 2008)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8996
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0051P)^2^+9.9383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                6619
_reflns_number_total             8996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102094d_si_002_1.cif
_cod_data_source_block           10093a
_cod_original_cell_volume        3951.2(10)
_cod_database_code               4324757