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_2015423
_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
'(C4 H7 N2) [Fe3 (C2 H3 O2)7 O (H2 O)2] Cl, 2H2O'
_chemical_formula_moiety         'C14 H25 Fe3 O17, C4 H7 N2 +, Cl -, 2H2 O'
_chemical_formula_sum            'C18 H36 Cl Fe3 N2 O19'
_chemical_formula_weight         787.49
_chemical_name_systematic
;
2-methylimidazolium
hexa-\m~2~-acetato-acetatodiaqua-\m~3~-oxo-triiron(III) chloride dihydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   32.147(6)
_cell_length_b                   12.048(2)
_cell_length_c                   8.0652(16)
_cell_measurement_reflns_used    1322
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.89
_cell_volume                     3123.7(10)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.079
_diffrn_reflns_av_sigmaI/netI    0.1277
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5673
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.794
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+17.3868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                1584
_reflns_number_total             2877
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3019.cif
_cod_data_source_block           II
_cod_depositor_comments
;
 Removing incorrectly marked comments that were interpreted as '_geom_hbond'
 loop values.

 Antanas Vaitkus,
 2017-03-07
;
_cod_original_cell_volume        3123.6(11)
_cod_database_code               2015423
_cod_database_fobs_code          2015423