Two oxo complexes with tetranuclear [Fe~4~(μ~3~-O)~2~]^8+^ and trinuclear [Fe~3~(μ~3~-O)]^7+^ units
Piedad Cortés; Ana María Atria; María Teresa Garland; Ricardo Baggio; Acta Crystallographica Section C 62 (2006) m297–m302; doi:10.1107/S0108270106020087

data_2015422
_publ_section_title
;
 Two oxo complexes with tetranuclear [Fe~4~(\m~3~-O)~2~]^8+^ and
 trinuclear [Fe~3~(\m~3~-O)]^7+^ units
;
_journal_coeditor_code           FA3019
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m297
_journal_page_last               m302
_journal_paper_doi               10.1107/S0108270106020087
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Fe4 (C2 H3 O2)7 O2 (C10 H9 N3)2 (H2 O)] Cl, 1.25C2 H6 O, H2 O'
_chemical_formula_moiety
'C34 H41 Fe4 N6 O17 +, Cl -, 1.25C2 H6 O, H2 O'
_chemical_formula_sum            'C36.5 H50.5 Cl Fe4 N6 O19.25'
_chemical_formula_weight         1140.18
_chemical_name_systematic
;
hexa-\m~2~-acetato-acetatoaqua(di-3-pyridylamine)di-\m~3~-oxo-tetrairon(III)
chloride monohydrate ethanol 1.25-solvate
;
_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                 91.571(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.044(4)
_cell_length_b                   17.619(4)
_cell_length_c                   17.942(5)
_cell_measurement_reflns_used    3678
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.34
_cell_volume                     5070(2)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL-NT (Bruker, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.072
_diffrn_reflns_av_sigmaI/netI    0.1191
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8964
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2346
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.495
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                4931
_reflns_number_total             8964
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3019.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C36.50 H50.5 Cl Fe4 N6 O19.25'
_cod_database_code               2015422
_cod_database_fobs_code          2015422