Hexanuclear Iron(III) Salicylaldoximato Complexes Presenting the [Fe6(μ3-O)2(μ2-OR)2]12+Core: Syntheses, Crystal Structures, and Spectroscopic and Magnetic Characterization
Raptopoulou, Catherine P.; Boudalis, Athanassios K.; Sanakis, Yiannis; Psycharis, Vassilis; Clemente-Juan, Juan Modesto; Fardis, Michael; Diamantopoulos, George; Papavassiliou, George; Inorganic Chemistry 45 (2006) 2317–2326; doi:10.1021/ic051945q

data_4331970
_publ_section_title
;
 Hexanuclear Iron(III) Salicylaldoximato Complexes Presenting the
 [Fe6(\m3-O)2(\m2-OR)2]12+Core: Syntheses, Crystal Structures, and
 Spectroscopic and Magnetic Characterization
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2317
_journal_page_last               2326
_journal_paper_doi               10.1021/ic051945q
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C100 H88 Fe6 N10 O28'
_chemical_formula_weight         2212.90
_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                105.79(2)
_cell_angle_beta                 96.72(2)
_cell_angle_gamma                116.69(2)
_cell_formula_units_Z            1
_cell_length_a                   13.210(8)
_cell_length_b                   13.87(1)
_cell_length_c                   17.04(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.5
_cell_volume                     2578(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.774
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       \q/2\q
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5494
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      1.41
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1236P)^2^+10.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.2161
_reflns_number_gt                3922
_reflns_number_total             5212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051945qsup1.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        2578.17(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331970