Synthesis and Structure of [Fe13O4F24(OMe)12]5-: The First Open-Shell Keggin Ion
Avi Bino; Michael Ardon; Dongwhan Lee; Bernhard Spingler; Stephen J. Lippard; Journal of the American Chemical Society 124 (2002) 4578–4579; doi:10.1021/ja025590a

data_4114765
_publ_section_title
;
 Synthesis and Structure of [Fe13O4F24(OMe)12]5-: The First Open-Shell
 Keggin Ion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4578
_journal_page_last               4579
_journal_paper_doi               10.1021/ja025590a
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         (PyH)5[Fe13O4(OMe)12F24]*MeOH*4H2O
_chemical_formula_sum            'C38 H78 F24 Fe13 N5 O21'
_chemical_formula_weight         2123.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4853(7)
_cell_length_b                   19.4853(7)
_cell_length_c                   19.4853(7)
_cell_measurement_temperature    188(2)
_cell_volume                     7398.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0104
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11749
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.779720
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      1.863
_exptl_crystal_density_method    flotation
_exptl_crystal_description       diamond
_exptl_crystal_F_000             4252
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         931
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+36.8306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                926
_reflns_number_total             931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja025590a.cif
_cod_data_source_block           global
_cod_database_code               4114765