Utilization of crown ethers to stabilize the dinuclear μ-oxo bridged iron(III) aqua ion, [(H2O)5Fe(μ-O)Fe(OH2)5]4+
Peter C. Junk; Brian J. McCool; Boujemaa Moubaraki; Keith S. Murray; Leone Spiccia; John D. Cashion; Jonathan W. Steed; J. Chem. Soc., Dalton Trans.  (2002) 1024–1029; doi:10.1039/b105691n

data_7010934
_publ_section_title
;
 Utilization of crown ethers to stabilize the dinuclear \m-oxo bridged
 iron(III) aqua ion, [(H2O)5Fe(\m-O)Fe(OH2)5]4+
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1024
_journal_page_last               1029
_journal_paper_doi               10.1039/b105691n
_journal_year                    2002
_chemical_formula_sum            'C20 H68 Fe2 N5 O39.5'
_chemical_formula_weight         1122.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 110.860(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7399(7)
_cell_length_b                   14.7129(4)
_cell_length_c                   22.0035(10)
_cell_measurement_temperature    123(2)
_cell_volume                     4761.6(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16428
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.8990
_exptl_absorpt_correction_T_min  0.5946
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0501P)^2^+6.4788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                7432
_reflns_number_total             8780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105691n.txt
_cod_data_source_block           feno315
_cod_original_cell_volume        4761.5(3)
_cod_original_sg_symbol_H-M      P21/a
_cod_original_formula_sum        'C20 H68 Fe2 N5 O39.50'
_cod_database_code               7010934