#------------------------------------------------------------------------------
#$Date: 2017-03-07 17:24:47 +0200 (Tue, 07 Mar 2017) $
#$Revision: 194047 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/54/2015423.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2015423
loop_
_publ_author_name
'Piedad Cortés'
'Ana María Atria'
'María Teresa Garland'
'Ricardo Baggio'
_publ_section_title
;
 Two oxo complexes with tetranuclear [Fe₄(μ₃-O)₂]⁸⁺ and
 trinuclear [Fe₃(μ₃-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-μ₂-acetato-acetatodiaqua-μ₃-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       'φ and ω 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/[σ²(Fo²)+(0.0993P)²+17.3868P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Fe Fe1 0.15105(3) 0.61315(8) 1.08730(11) 0.0245(2) Uani d . 1
Fe Fe2 0.07772(4) 0.7500 0.88154(16) 0.0244(3) Uani d S 1
O O1 0.12758(17) 0.7500 1.0192(8) 0.0263(16) Uani d S 1
O O1W 0.18246(13) 0.4661(4) 1.1581(6) 0.0343(13) Uani d . 1
O O11 0.10002(14) 0.6286(4) 0.7317(6) 0.0381(13) Uani d . 1
O O21 0.14458(15) 0.5287(4) 0.8741(6) 0.0401(13) Uani d . 1
C C11 0.1241(2) 0.5475(5) 0.7467(7) 0.0290(17) Uani d . 1
C C21 0.1296(3) 0.4716(6) 0.6037(8) 0.052(2) Uani d . 1
H H21A 0.1412 0.5120 0.5120 0.079 Uiso calc R 1
H H21B 0.1032 0.4413 0.5724 0.079 Uiso calc R 1
H H21C 0.1481 0.4124 0.6341 0.079 Uiso calc R 1
O O12 0.04943(13) 0.6332(4) 1.0263(6) 0.0353(13) Uani d . 1
O O22 0.09833(14) 0.5462(4) 1.1763(6) 0.0422(14) Uani d . 1
C C12 0.06033(17) 0.5677(5) 1.1361(8) 0.0268(16) Uani d . 1
C C22 0.02711(18) 0.5105(6) 1.2318(8) 0.0381(19) Uani d . 1
H H22A 0.0116 0.5642 1.2945 0.057 Uiso calc R 1
H H22B 0.0395 0.4576 1.3060 0.057 Uiso calc R 1
H H22C 0.0088 0.4727 1.1567 0.057 Uiso calc R 1
O O13 0.20923(13) 0.6585(4) 1.0038(6) 0.0427(14) Uani d . 1
C C13 0.2271(2) 0.7500 0.9800(13) 0.036(3) Uani d S 1
C C23 0.2717(2) 0.7500 0.9331(14) 0.043(3) Uani d S 1
H H23A 0.2872 0.7936 1.0114 0.064 Uiso calc PR 0.50
H H23B 0.2748 0.7812 0.8243 0.064 Uiso calc PR 0.50
H H23C 0.2820 0.6752 0.9334 0.064 Uiso calc PR 0.50
O O14 0.16757(15) 0.6574(4) 1.3165(6) 0.0393(13) Uani d . 1
C C14 0.1737(3) 0.7500 1.3862(10) 0.036(3) Uani d S 1
C C24 0.1906(3) 0.7500 1.5580(9) 0.053(4) Uani d S 1
H H24A 0.2173 0.7856 1.5588 0.080 Uiso calc PR 0.50
H H24B 0.1934 0.6749 1.5962 0.080 Uiso calc PR 0.50
H H24C 0.1719 0.7895 1.6298 0.080 Uiso calc PR 0.50
O O15 0.02623(17) 0.7500 0.7451(8) 0.0250(16) Uani d S 1
O O25 -0.0213(2) 0.7500 0.5473(10) 0.054(2) Uani d S 1
C C15 0.0166(3) 0.7500 0.5887(11) 0.040(3) Uani d S 1
C C25 0.0501(3) 0.7500 0.4605(11) 0.040(3) Uani d S 1
H H25A 0.0744 0.7861 0.5039 0.061 Uiso calc PR 0.50
H H25B 0.0406 0.7890 0.3639 0.061 Uiso calc PR 0.50
H H25C 0.0568 0.6749 0.4312 0.061 Uiso calc PR 0.50
C C1 0.0911(2) 0.2500 1.1040(11) 0.043(3) Uani d S 1
C C2 0.0771(3) 0.2500 0.8327(14) 0.064(4) Uani d S 1
H H2 0.0808 0.2500 0.7183 0.076 Uiso calc SR 1
C C3 0.0407(3) 0.2500 0.9196(15) 0.091(6) Uani d S 1
H H3 0.0140 0.2500 0.8745 0.109 Uiso calc SR 1
C C4 0.1144(4) 0.2500 1.2666(14) 0.068(4) Uani d S 1
H H4A 0.1382 0.2022 1.2581 0.101 Uiso calc PR 0.50
H H4B 0.0964 0.2237 1.3532 0.101 Uiso calc PR 0.50
H H4C 0.1234 0.3241 1.2918 0.101 Uiso calc PR 0.50
N N1 0.0502(3) 0.2500 1.0820(14) 0.081(4) Uani d S 1
H H1N 0.0322 0.2500 1.1610 0.097 Uiso calc SR 1
N N2 0.1077(2) 0.2500 0.9558(10) 0.047(3) Uani d S 1
H H2N 0.1340 0.2500 0.9368 0.057 Uiso calc SR 1
Cl Cl1 0.20342(8) 0.2500 0.9160(4) 0.0503(8) Uani d S 1
O O2W 0.24374(17) 0.4883(5) 0.7884(9) 0.076(2) Uani d . 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Fe1 O14 . . 98.2(2)
O1 Fe1 O21 . . 98.7(2)
O14 Fe1 O21 . . 162.9(2)
O1 Fe1 O22 . . 96.7(2)
O14 Fe1 O22 . . 90.0(2)
O21 Fe1 O22 . . 90.9(2)
O1 Fe1 O13 . . 92.1(2)
O14 Fe1 O13 . . 89.4(2)
O21 Fe1 O13 . . 87.1(2)
O22 Fe1 O13 . . 171.2(2)
O1 Fe1 O1W . . 175.0(2)
O14 Fe1 O1W . . 81.2(2)
O21 Fe1 O1W . . 81.75(19)
O22 Fe1 O1W . . 88.29(19)
O13 Fe1 O1W . . 82.94(19)
O1 Fe2 O15 . . 178.9(3)
O1 Fe2 O11 . . 92.80(18)
O15 Fe2 O11 . . 87.96(18)
O1 Fe2 O11 . 7_575 92.80(18)
O15 Fe2 O11 . 7_575 87.96(18)
O11 Fe2 O11 . 7_575 92.3(3)
O1 Fe2 O12 . 7_575 92.32(18)
O15 Fe2 O12 . 7_575 86.89(18)
O11 Fe2 O12 . 7_575 174.24(19)
O11 Fe2 O12 7_575 7_575 90.08(19)
O1 Fe2 O12 . . 92.32(18)
O15 Fe2 O12 . . 86.89(18)
O11 Fe2 O12 . . 90.08(19)
O11 Fe2 O12 7_575 . 174.24(19)
O12 Fe2 O12 7_575 . 87.1(3)
Fe1 O1 Fe1 . 7_575 121.0(3)
Fe1 O1 Fe2 . . 119.50(15)
Fe1 O1 Fe2 7_575 . 119.50(15)
C11 O11 Fe2 . . 136.3(4)
C11 O21 Fe1 . . 132.2(4)
O21 C11 O11 . . 123.4(6)
O21 C11 C21 . . 118.0(6)
O11 C11 C21 . . 118.6(6)
C11 C21 H21A . . 109.5
C11 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C11 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
C12 O12 Fe2 . . 136.3(4)
C12 O22 Fe1 . . 128.9(4)
O12 C12 O22 . . 125.2(5)
O12 C12 C22 . . 117.6(5)
O22 C12 C22 . . 117.2(5)
C12 C22 H22A . . 109.5
C12 C22 H22B . . 109.5
H22A C22 H22B . . 109.5
C12 C22 H22C . . 109.5
H22A C22 H22C . . 109.5
H22B C22 H22C . . 109.5
C13 O13 Fe1 . . 134.2(4)
O13 C13 O13 7_575 . 122.4(7)
O13 C13 C23 7_575 . 118.7(3)
O13 C13 C23 . . 118.7(3)
C13 C23 H23A . . 109.5
C13 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C13 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C14 O14 Fe1 . . 133.5(5)
O14 C14 O14 . 7_575 123.8(7)
O14 C14 C24 . . 118.1(4)
O14 C14 C24 7_575 . 118.1(4)
C14 C24 H24A . . 109.5
C14 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C14 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
C15 O15 Fe2 . . 137.3(5)
O25 C15 O15 . . 119.1(7)
O25 C15 C25 . . 120.8(8)
O15 C15 C25 . . 120.2(8)
C15 C25 H25A . . 109.5
C15 C25 H25B . . 109.5
H25A C25 H25B . . 109.5
C15 C25 H25C . . 109.5
H25A C25 H25C . . 109.5
H25B C25 H25C . . 109.5
N2 C1 N1 . . 106.4(8)
N2 C1 C4 . . 126.2(8)
N1 C1 C4 . . 127.4(9)
C3 C2 N2 . . 103.8(9)
C3 C2 H2 . . 128.1
N2 C2 H2 . . 128.1
N1 C3 C2 . . 107.6(10)
N1 C3 H3 . . 126.2
C2 C3 H3 . . 126.2
C1 C4 H4A . . 109.5
C1 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C1 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C1 N1 C3 . . 110.9(9)
C1 N1 H1N . . 124.6
C3 N1 H1N . . 124.6
C1 N2 C2 . . 111.3(8)
C1 N2 H2N . . 124.4
C2 N2 H2N . . 124.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O1 . 1.894(3) y
Fe1 O14 . 1.996(5) y
Fe1 O21 . 2.009(5) y
Fe1 O22 . 2.009(5) y
Fe1 O13 . 2.062(5) y
Fe1 O1W . 2.118(5) y
Fe2 O1 . 1.950(6) y
Fe2 O15 . 1.988(6) y
Fe2 O11 . 2.029(5) y
Fe2 O12 . 2.042(5) y
O11 C11 . 1.253(8) ?
O21 C11 . 1.241(7) ?
C11 C21 . 1.482(7) ?
C21 H21A . 0.9600 ?
C21 H21B . 0.9600 ?
C21 H21C . 0.9600 ?
O12 C12 . 1.237(7) ?
O22 C12 . 1.290(7) ?
C12 C22 . 1.487(7) ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
O13 C13 . 1.258(6) ?
C13 O13 7_575 1.258(6) ?
C13 C23 . 1.484(9) ?
C23 H23A . 0.9600 ?
C23 H23B . 0.9600 ?
C23 H23C . 0.9600 ?
O14 C14 . 1.264(6) ?
C14 O14 7_575 1.264(6) ?
C14 C24 . 1.489(9) ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
O15 C15 . 1.298(10) ?
O25 C15 . 1.264(11) ?
C15 C25 . 1.492(9) ?
C25 H25A . 0.9600 ?
C25 H25B . 0.9600 ?
C25 H25C . 0.9600 ?
C1 N2 . 1.308(11) ?
C1 N1 . 1.325(11) ?
C1 C4 . 1.510(12) ?
C2 C3 . 1.366(12) ?
C2 N2 . 1.397(11) ?
C2 H2 . 0.9300 ?
C3 N1 . 1.346(13) ?
C3 H3 . 0.9300 ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
N1 H1N . 0.8600 ?
N2 H2N . 0.8600 ?
Fe1 Fe1 7_575 3.298(2) y
Fe1 Fe2 . 3.321(2) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2N Cl1 . 0.86 2.24 3.094(13) 174
O2W ? Cl1 . ? ? 3.315(9) ?
O1W ? Cl1 . ? ? 3.323(8) ?
O1W ? O2W 2_565 ? ? 2.651(11) ?
O2W ? O13 . ? ? 2.910(13) ?
N1 H1N O15 5_567 0.86 2.03 2.826(12) 154
N1 H1N O25 5_567 0.86 2.38 3.132(12) 146
