#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:30:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179793 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008910.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_7008910
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 H36 Fe2 O28 S28'
_chemical_formula_weight         2142.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.56(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.487(2)
_cell_length_b                   21.118(11)
_cell_length_c                   17.514(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3866(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7560
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.212
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0690P)²+0.7363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                3647
_reflns_number_total             6974
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            a906893g.txt
_cod_data_source_block           1
_cod_database_code               7008910
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Fe Fe 0.32046(9) 0.19053(5) 0.32000(5) 0.0459(2) Uani 1 1 d . . .
O1 O 0.1611(4) 0.1929(2) 0.2483(2) 0.0523(11) Uani 1 1 d . . .
O2 O 0.1868(4) 0.2009(2) 0.3954(2) 0.0533(11) Uani 1 1 d . . .
O3 O 0.3254(4) 0.0963(2) 0.3138(3) 0.0560(12) Uani 1 1 d . . .
O4 O 0.4680(4) 0.1730(2) 0.3992(2) 0.0532(11) Uani 1 1 d . . .
O5 O 0.3572(5) 0.2841(2) 0.3254(2) 0.0561(12) Uani 1 1 d . . .
O6 O 0.4292(4) 0.2002(2) 0.2300(2) 0.0526(11) Uani 1 1 d . . .
O7 O -0.0513(5) 0.1954(3) 0.2459(3) 0.0683(14) Uani 1 1 d . . .
O8 O -0.0199(5) 0.2209(3) 0.4026(3) 0.094(2) Uani 1 1 d . . .
O9 O 0.4315(4) 0.0119(2) 0.3595(3) 0.0707(14) Uani 1 1 d . . .
O10 O 0.5911(5) 0.0950(2) 0.4464(3) 0.0672(14) Uani 1 1 d . . .
O11 O 0.4588(4) 0.3608(2) 0.2693(3) 0.0619(13) Uani 1 1 d . . .
O12 O 0.5163(5) 0.2734(3) 0.1590(3) 0.0767(16) Uani 1 1 d . . .
C101 C 0.0552(7) 0.1969(3) 0.2787(3) 0.0471(16) Uani 1 1 d . . .
C102 C 0.0719(7) 0.2063(3) 0.3665(4) 0.0550(18) Uani 1 1 d . . .
C103 C 0.4148(6) 0.0692(3) 0.3567(4) 0.0471(15) Uani 1 1 d . . .
C104 C 0.5002(6) 0.1151(3) 0.4057(3) 0.0431(15) Uani 1 1 d . . .
C105 C 0.4237(6) 0.3064(3) 0.2745(4) 0.0476(15) Uani 1 1 d . . .
C106 C 0.4609(6) 0.2565(4) 0.2149(4) 0.0506(17) Uani 1 1 d . . .
S11 S 0.50255(18) 0.07737(11) -0.08029(10) 0.0649(5) Uani 1 1 d . . .
S12 S 0.53720(18) 0.07396(10) 0.08555(10) 0.0626(5) Uani 1 1 d . . .
C1 C 0.5089(6) 0.0329(3) 0.0015(4) 0.0559(18) Uani 1 1 d . . .
C2 C 0.5300(8) 0.1482(4) -0.0342(5) 0.074(2) Uani 1 1 d . . .
H2 H 0.5355 0.1860 -0.0610 0.050 Uiso 1 1 calc . . .
C3 C 0.5429(7) 0.1463(4) 0.0419(4) 0.065(2) Uani 1 1 d . . .
H3 H 0.5547 0.1832 0.0705 0.050 Uiso 1 1 calc . . .
S21 S 0.19106(17) 0.11279(8) -0.05478(8) 0.0465(4) Uani 1 1 d . . .
S22 S 0.21495(16) 0.08129(9) 0.10876(9) 0.0513(4) Uani 1 1 d . . .
S23 S 0.13932(17) -0.03454(8) -0.09684(9) 0.0491(4) Uani 1 1 d . . .
S24 S 0.16174(17) -0.06703(9) 0.06601(9) 0.0538(4) Uani 1 1 d . . .
C21 C 0.1866(6) 0.0546(3) 0.0153(3) 0.0430(15) Uani 1 1 d . . .
C22 C 0.1650(5) -0.0082(3) -0.0032(3) 0.0390(14) Uani 1 1 d . . .
C23 C 0.2164(7) 0.1744(3) 0.0095(4) 0.0513(17) Uani 1 1 d . . .
H23 H 0.2233 0.2161 -0.0070 0.050 Uiso 1 1 calc . . .
C24 C 0.2256(6) 0.1600(3) 0.0827(3) 0.0514(17) Uani 1 1 d . . .
H24 H 0.2376 0.1914 0.1198 0.050 Uiso 1 1 calc . . .
C25 C 0.1133(7) -0.1125(3) -0.0719(4) 0.0541(17) Uani 1 1 d . . .
H25 H 0.0936 -0.1432 -0.1090 0.050 Uiso 1 1 calc . . .
C26 C 0.1225(7) -0.1266(3) 0.0011(4) 0.062(2) Uani 1 1 d . . .
H26 H 0.1082 -0.1677 0.0175 0.050 Uiso 1 1 calc . . .
S31 S -0.05379(17) 0.14445(8) 0.77350(9) 0.0497(4) Uani 1 1 d . . .
S32 S -0.18402(16) 0.03724(9) 0.69901(10) 0.0545(4) Uani 1 1 d . . .
S33 S 0.21819(15) 0.07814(8) 0.75248(8) 0.0481(4) Uani 1 1 d . . .
S34 S 0.08657(19) -0.03104(9) 0.68251(11) 0.0633(5) Uani 1 1 d . . .
C31 C -0.0407(6) 0.0725(3) 0.7316(3) 0.0427(14) Uani 1 1 d . . .
C32 C 0.0756(6) 0.0423(3) 0.7235(3) 0.0445(15) Uani 1 1 d . . .
C33 C -0.2185(7) 0.1474(3) 0.7624(4) 0.0553(18) Uani 1 1 d . . .
H33 H -0.2644 0.1816 0.7794 0.050 Uiso 1 1 calc . . .
C34 C -0.2756(6) 0.0979(4) 0.7283(4) 0.0571(18) Uani 1 1 d . . .
H34 H -0.3643 0.0963 0.7205 0.050 Uiso 1 1 calc . . .
C35 C 0.3101(7) 0.0166(4) 0.7246(4) 0.066(2) Uani 1 1 d . . .
H35 H 0.3989 0.0180 0.7313 0.050 Uiso 1 1 calc . . .
C36 C 0.2502(8) -0.0327(4) 0.6934(5) 0.073(2) Uani 1 1 d . . .
H36 H 0.2954 -0.0676 0.6777 0.050 Uiso 1 1 calc . . .
S41 S -0.01825(16) 0.21863(7) 0.61301(9) 0.0454(4) Uani 1 1 d . . .
S42 S -0.14405(16) 0.11792(8) 0.52263(9) 0.0497(4) Uani 1 1 d . . .
S43 S 0.25428(16) 0.15936(8) 0.59381(9) 0.0480(4) Uani 1 1 d . . .
S44 S 0.14102(17) 0.05307(8) 0.50888(10) 0.0542(4) Uani 1 1 d . . .
C41 C -0.0033(6) 0.1507(3) 0.5610(3) 0.0391(14) Uani 1 1 d . . .
C42 C 0.1165(6) 0.1236(3) 0.5541(3) 0.0403(14) Uani 1 1 d . . .
C43 C -0.1829(7) 0.2214(3) 0.5985(4) 0.0525(17) Uani 1 1 d . . .
H43 H -0.2297 0.2538 0.6190 0.050 Uiso 1 1 calc . . .
C44 C -0.2400(6) 0.1755(3) 0.5570(4) 0.0522(17) Uani 1 1 d . . .
H44 H -0.3284 0.1745 0.5469 0.050 Uiso 1 1 calc . . .
C45 C 0.3557(6) 0.1012(4) 0.5677(4) 0.0550(18) Uani 1 1 d . . .
H45 H 0.4435 0.1038 0.5798 0.050 Uiso 1 1 calc . . .
C46 C 0.3038(7) 0.0525(3) 0.5296(4) 0.0530(17) Uani 1 1 d . . .
H46 H 0.3537 0.0190 0.5146 0.050 Uiso 1 1 calc . . .
O101 O -0.3043(7) 0.1558(4) 0.2101(4) 0.124(2) Uani 1 1 d . . .
O102 O -0.2878(6) 0.2375(3) 0.3659(4) 0.108(2) Uani 1 1 d . . .
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
O3 Fe O1 90.84(19) . . ?
O3 Fe O2 99.61(19) . . ?
O1 Fe O2 79.59(18) . . ?
O3 Fe O5 167.46(19) . . ?
O1 Fe O5 98.7(2) . . ?
O2 Fe O5 90.17(18) . . ?
O3 Fe O6 92.27(19) . . ?
O1 Fe O6 90.15(17) . . ?
O2 Fe O6 164.35(19) . . ?
O5 Fe O6 79.65(18) . . ?
O3 Fe O4 80.45(19) . . ?
O1 Fe O4 169.50(19) . . ?
O2 Fe O4 96.00(18) . . ?
O5 Fe O4 90.80(19) . . ?
O6 Fe O4 95.99(18) . . ?
C101 O1 Fe 116.8(4) . . ?
C102 O2 Fe 115.8(4) . . ?
C103 O3 Fe 115.6(4) . . ?
C104 O4 Fe 114.8(4) . . ?
C105 O5 Fe 116.5(4) . . ?
C106 O6 Fe 115.4(4) . . ?
O7 C101 O1 126.9(6) . . ?
O7 C101 C102 120.0(6) . . ?
O1 C101 C102 113.0(6) . . ?
O8 C102 O2 124.9(6) . . ?
O8 C102 C101 120.7(6) . . ?
O2 C102 C101 114.3(6) . . ?
O9 C103 O3 124.0(6) . . ?
O9 C103 C104 121.8(6) . . ?
O3 C103 C104 114.2(6) . . ?
O10 C104 O4 125.2(6) . . ?
O10 C104 C103 120.0(6) . . ?
O4 C104 C103 114.7(6) . . ?
O11 C105 O5 126.4(6) . . ?
O11 C105 C106 119.9(6) . . ?
O5 C105 C106 113.7(6) . . ?
O12 C106 O6 125.9(7) . . ?
O12 C106 C105 119.8(7) . . ?
O6 C106 C105 114.3(6) . . ?
C1 S11 C2 95.2(4) . . ?
C3 S12 C1 94.4(4) . . ?
C1 C1 S11 121.1(7) 3_655 . ?
C1 C1 S12 123.1(7) 3_655 . ?
S11 C1 S12 115.8(4) . . ?
C3 C2 S11 116.5(6) . . ?
C2 C3 S12 118.1(6) . . ?
C23 S21 C21 94.8(3) . . ?
C24 S22 C21 94.2(3) . . ?
C25 S23 C22 94.7(3) . . ?
C26 S24 C22 94.5(3) . . ?
C22 C21 S22 123.1(4) . . ?
C22 C21 S21 121.8(4) . . ?
S22 C21 S21 115.1(4) . . ?
C21 C22 S23 122.7(4) . . ?
C21 C22 S24 122.4(4) . . ?
S23 C22 S24 114.9(4) . . ?
C24 C23 S21 117.2(5) . . ?
C23 C24 S22 118.6(5) . . ?
C26 C25 S23 117.6(6) . . ?
C25 C26 S24 118.2(6) . . ?
C31 S31 C33 95.7(3) . . ?
C34 S32 C31 94.2(3) . . ?
C35 S33 C32 94.4(4) . . ?
C36 S34 C32 94.1(4) . . ?
C32 C31 S31 123.7(5) . . ?
C32 C31 S32 120.9(5) . . ?
S31 C31 S32 115.4(4) . . ?
C31 C32 S34 122.9(5) . . ?
C31 C32 S33 121.2(5) . . ?
S34 C32 S33 115.9(4) . . ?
C34 C33 S31 115.8(5) . . ?
C33 C34 S32 119.0(5) . . ?
C36 C35 S33 117.3(6) . . ?
C35 C36 S34 118.2(6) . . ?
C41 S41 C43 94.7(3) . . ?
C41 S42 C44 95.0(3) . . ?
C45 S43 C42 95.5(3) . . ?
C42 S44 C46 95.2(3) . . ?
C42 C41 S41 120.6(4) . . ?
C42 C41 S42 123.6(5) . . ?
S41 C41 S42 115.7(4) . . ?
C41 C42 S44 124.4(4) . . ?
C41 C42 S43 121.2(4) . . ?
S44 C42 S43 114.5(4) . . ?
C44 C43 S41 117.3(5) . . ?
C43 C44 S42 117.3(5) . . ?
C46 C45 S43 117.0(5) . . ?
C45 C46 S44 117.7(5) . . ?
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
Fe O3 1.994(5) . ?
Fe O1 2.009(4) . ?
Fe O2 2.012(4) . ?
Fe O5 2.013(5) . ?
Fe O6 2.027(4) . ?
Fe O4 2.028(4) . ?
O1 C101 1.273(7) . ?
O2 C102 1.275(8) . ?
O3 C103 1.289(7) . ?
O4 C104 1.272(7) . ?
O5 C105 1.266(7) . ?
O6 C106 1.268(8) . ?
O7 C101 1.215(8) . ?
O8 C102 1.232(8) . ?
O9 C103 1.223(8) . ?
O10 C104 1.221(8) . ?
O11 C105 1.213(7) . ?
O12 C106 1.231(7) . ?
C101 C102 1.547(8) . ?
C103 C104 1.536(9) . ?
C105 C106 1.553(9) . ?
S11 C1 1.709(7) . ?
S11 C2 1.714(9) . ?
S12 C3 1.712(8) . ?
S12 C1 1.714(7) . ?
C1 C1 1.404(14) 3_655 ?
C2 C3 1.329(10) . ?
S21 C23 1.728(7) . ?
S21 C21 1.740(6) . ?
S22 C24 1.730(7) . ?
S22 C21 1.734(6) . ?
S23 C25 1.730(7) . ?
S23 C22 1.733(6) . ?
S24 C26 1.723(8) . ?
S24 C22 1.737(6) . ?
C21 C22 1.380(9) . ?
C23 C24 1.315(8) . ?
C25 C26 1.310(9) . ?
S31 C31 1.698(6) . ?
S31 C33 1.724(7) . ?
S32 C34 1.705(7) . ?
S32 C31 1.733(6) . ?
S33 C35 1.712(8) . ?
S33 C32 1.716(6) . ?
S34 C36 1.712(8) . ?
S34 C32 1.715(6) . ?
C31 C32 1.393(8) . ?
C33 C34 1.323(10) . ?
C35 C36 1.311(11) . ?
S41 C41 1.714(6) . ?
S41 C43 1.726(7) . ?
S42 C41 1.717(6) . ?
S42 C44 1.717(7) . ?
S43 C45 1.711(7) . ?
S43 C42 1.726(6) . ?
S44 C42 1.717(6) . ?
S44 C46 1.717(7) . ?
C41 C42 1.394(8) . ?
C43 C44 1.326(9) . ?
C45 C46 1.319(10) . ?
