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#$Date: 2016-03-25 11:30:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008911.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7008911
loop_
_publ_author_name
'Coronado, Eugenio'
'Galán-Mascarós, José R.'
'Gómez-García, Carlos J.'
_publ_section_title
;
 Charge transfer salts of tetrathiafulvalene derivatives with magnetic
 iron(III) oxalate complexes: [TTF]7[Fe(ox)3]2·4H2O,
 [TTF]5[Fe2(ox)5]·2PhMe·2H2O and
 [TMTTF]4[Fe2(ox)5]· PhCN·4H2O
 (TMTTF = tetramethyltetrathiafulvalene) †
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              205
_journal_paper_doi               10.1039/a906893g
_journal_year                    2000
_chemical_formula_sum            'C54 H40 Fe2 O22 S20'
_chemical_formula_weight         1793.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 107.400(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   19.777(5)
_cell_length_b                   13.900(5)
_cell_length_c                   13.457(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3530(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3380
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.075
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1861
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0843P)²+13.7918P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1872
_reflns_number_gt                1485
_reflns_number_total             3221
_reflns_threshold_expression     >6sigma(I)
_cod_data_source_file            a906893g.txt
_cod_data_source_block           2
_cod_database_code               7008911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.30335(13) -0.5000 0.0437(5) Uani 1 2 d S . .
O1 O -0.0507(3) 0.4189(4) -0.5901(4) 0.0478(14) Uani 1 1 d . . .
O2 O 0.0504(3) 0.2184(4) -0.3862(4) 0.0507(15) Uani 1 1 d . . .
O3 O -0.0746(3) 0.2934(4) -0.4320(4) 0.0529(15) Uani 1 1 d . . .
O4 O 0.0363(3) 0.1415(5) -0.2472(5) 0.077(2) Uani 1 1 d . . .
O5 O -0.0960(3) 0.2270(6) -0.2933(5) 0.080(2) Uani 1 1 d . . .
C1 C -0.0290(5) 0.5000 -0.5509(8) 0.037(3) Uani 1 2 d S . .
C2 C 0.0157(4) 0.1948(7) -0.3229(7) 0.052(2) Uani 1 1 d . . .
C3 C -0.0587(4) 0.2408(7) -0.3494(7) 0.053(2) Uani 1 1 d . . .
S1 S 0.16641(10) 0.37763(18) -0.20809(16) 0.0520(6) Uani 1 1 d . . .
S2 S 0.32025(10) 0.3808(2) -0.15053(17) 0.0583(7) Uani 1 1 d . . .
S3 S 0.17672(11) 0.37697(18) 0.03805(17) 0.0544(6) Uani 1 1 d . . .
S4 S 0.33058(11) 0.37816(17) 0.09069(16) 0.0524(6) Uani 1 1 d . . .
S5 S -0.02260(13) 0.3831(2) -0.11483(18) 0.0675(8) Uani 1 1 d . . .
C11 C 0.2458(4) 0.3785(6) -0.1105(6) 0.047(2) Uani 1 1 d . . .
C12 C 0.2501(4) 0.3791(6) -0.0050(7) 0.0463(19) Uani 1 1 d . . .
C13 C 0.2042(4) 0.3722(7) -0.3061(6) 0.061(3) Uani 1 1 d . . .
H13 H 0.1767 0.3676 -0.3754 0.050 Uiso 1 1 calc . . .
C14 C 0.2751(5) 0.3747(8) -0.2794(7) 0.067(3) Uani 1 1 d . . .
H14 H 0.2988 0.3731 -0.3296 0.050 Uiso 1 1 calc . . .
C15 C 0.2239(5) 0.3721(7) 0.1660(6) 0.060(2) Uani 1 1 d . . .
H15 H 0.2010 0.3693 0.2171 0.050 Uiso 1 1 calc . . .
C16 C 0.2952(5) 0.3721(7) 0.1922(6) 0.061(2) Uani 1 1 d . . .
H16 H 0.3234 0.3691 0.2611 0.050 Uiso 1 1 calc . . .
C21 C 0.0000 0.4513(9) 0.0000 0.059(4) Uani 1 2 d S . .
C22 C -0.0094(5) 0.2730(7) -0.0507(7) 0.065(3) Uani 1 1 d . . .
H22 H -0.0155 0.2155 -0.0878 0.050 Uiso 1 1 calc . . .
C101 C -0.1655(7) 0.0000 -0.5290(10) 0.066(4) Uani 1 2 d S . .
C201 C -0.0880(7) 0.0000 -0.5008(13) 0.090(5) Uani 1 2 d S . .
C102 C -0.2048(6) 0.0860(8) -0.5439(7) 0.074(3) Uani 1 1 d . . .
H102 H -0.1815 0.1450 -0.5357 0.050 Uiso 1 1 calc . . .
C103 C -0.2773(7) 0.0832(12) -0.5705(9) 0.105(5) Uani 1 1 d . . .
H103 H -0.3017 0.1413 -0.5790 0.050 Uiso 1 1 calc . . .
C104 C -0.3158(10) 0.0000 -0.5854(14) 0.115(9) Uani 1 2 d S . .
H104 H -0.3650 0.0000 -0.6044 0.050 Uiso 1 2 calc S . .
O100 O -0.0564(5) 0.0000 -0.2066(8) 0.086(3) Uani 1 2 d S . .
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'
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O2 105.7(3) 2_554 . ?
O2 Fe1 O3 82.5(2) 2_554 2_554 ?
O2 Fe1 O3 92.6(2) . 2_554 ?
O2 Fe1 O3 92.6(2) 2_554 . ?
O2 Fe1 O3 82.5(2) . . ?
O3 Fe1 O3 171.9(4) 2_554 . ?
O2 Fe1 O1 165.2(2) 2_554 2_554 ?
O2 Fe1 O1 88.0(2) . 2_554 ?
O3 Fe1 O1 91.6(2) 2_554 2_554 ?
O3 Fe1 O1 94.7(2) . 2_554 ?
O2 Fe1 O1 88.0(2) 2_554 . ?
O2 Fe1 O1 165.2(2) . . ?
O3 Fe1 O1 94.7(2) 2_554 . ?
O3 Fe1 O1 91.6(2) . . ?
O1 Fe1 O1 78.9(3) 2_554 . ?
C1 O1 Fe1 113.6(5) . . ?
C2 O2 Fe1 115.2(5) . . ?
C3 O3 Fe1 114.8(5) . . ?
O1 C1 O1 126.2(9) . 6_565 ?
O1 C1 C1 116.9(5) . 5_564 ?
O1 C1 C1 116.9(5) 6_565 5_564 ?
O4 C2 O2 126.4(8) . . ?
O4 C2 C3 120.0(9) . . ?
O2 C2 C3 113.6(8) . . ?
O5 C3 O3 126.0(8) . . ?
O5 C3 C2 120.2(9) . . ?
O3 C3 C2 113.8(8) . . ?
C13 S1 C11 94.6(4) . . ?
C14 S2 C11 94.7(4) . . ?
C15 S3 C12 94.6(4) . . ?
C16 S4 C12 95.1(4) . . ?
C22 S5 C21 94.5(5) . . ?
C12 C11 S2 121.5(6) . . ?
C12 C11 S1 122.8(6) . . ?
S2 C11 S1 115.7(5) . . ?
C11 C12 S4 121.4(6) . . ?
C11 C12 S3 122.9(6) . . ?
S4 C12 S3 115.7(5) . . ?
C14 C13 S1 117.3(7) . . ?
C13 C14 S2 117.6(7) . . ?
C16 C15 S3 118.7(7) . . ?
C15 C16 S4 115.9(6) . . ?
C21 C21 S5 122.8(4) 5_565 . ?
C21 C21 S5 122.8(4) 5_565 2 ?
S5 C21 S5 114.5(7) . 2 ?
C22 C22 S5 118.3(3) 2 . ?
C102 C101 C102 116.3(13) 6 . ?
C102 C101 C201 121.8(7) 6 . ?
C102 C101 C201 121.8(7) . . ?
C103 C102 C101 120.2(12) . . ?
C104 C103 C102 123.8(15) . . ?
C103 C104 C103 115.7(18) . 6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.954(6) 2_554 ?
Fe1 O2 1.954(6) . ?
Fe1 O3 1.960(5) 2_554 ?
Fe1 O3 1.960(5) . ?
Fe1 O1 2.081(6) 2_554 ?
Fe1 O1 2.081(6) . ?
O1 C1 1.264(6) . ?
O2 C2 1.286(9) . ?
O3 C3 1.288(10) . ?
O4 C2 1.227(10) . ?
O5 C3 1.219(9) . ?
C1 O1 1.264(6) 6_565 ?
C1 C1 1.501(19) 5_564 ?
C2 C3 1.545(12) . ?
S1 C13 1.701(8) . ?
S1 C11 1.719(8) . ?
S2 C14 1.699(9) . ?
S2 C11 1.714(8) . ?
S3 C15 1.697(9) . ?
S3 C12 1.715(8) . ?
S4 C16 1.713(9) . ?
S4 C12 1.723(8) . ?
S5 C22 1.738(9) . ?
S5 C21 1.754(7) . ?
C11 C12 1.396(11) . ?
C13 C14 1.341(12) . ?
C15 C16 1.347(12) . ?
C21 C21 1.35(3) 5_565 ?
C21 S5 1.754(7) 2 ?
C22 C22 1.302(17) 2 ?
C101 C102 1.407(11) 6 ?
C101 C102 1.407(11) . ?
C101 C201 1.465(18) . ?
C102 C103 1.370(15) . ?
C103 C104 1.366(16) . ?
C104 C103 1.366(16) 6 ?
