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_4324758
_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, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C25 H51 F3 Fe N12 O3 S'
_chemical_formula_weight         712.69
_chemical_name_common            09003m
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.293(11)
_cell_angle_beta                 86.561(11)
_cell_angle_gamma                87.038(19)
_cell_formula_units_Z            2
_cell_length_a                   11.031(2)
_cell_length_b                   12.5778(16)
_cell_length_c                   12.811(2)
_cell_measurement_reflns_used    3795
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.38
_cell_volume                     1770.2(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21227
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       Plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0439P)^2^+0.6850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6989
_reflns_number_total             8021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102094d_si_002_2.cif
_cod_data_source_block           09003m
_cod_original_cell_volume        1770.1(5)
_cod_database_code               4324758