#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/89/7008912.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_7008912
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            'C57 H61 Fe2 N O24 S16'
_chemical_formula_weight         1768.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.1100(10)
_cell_angle_beta                 90.6600(10)
_cell_angle_gamma                114.1000(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6100(10)
_cell_length_b                   14.0850(10)
_cell_length_c                   14.2530(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1815.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 '
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7648
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.936
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             910
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.721
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0556P)²+3.4195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                4712
_reflns_number_total             7268
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            a906893g.txt
_cod_data_source_block           a
_cod_original_formula_sum        'C57 H61 Fe2 N1 O24 S16'
_cod_database_code               7008912
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Fe Fe 0.11351(7) 0.18015(7) -0.04487(6) 0.0353(2) Uani 1 1 d . . .
S1 S 0.35948(13) 0.05209(13) 0.14716(12) 0.0425(3) Uani 1 1 d . . .
S2 S 0.62214(13) 0.11859(14) 0.23991(13) 0.0471(4) Uani 1 1 d . . .
S3 S 0.45583(14) 0.16183(14) -0.00190(12) 0.0454(4) Uani 1 1 d . . .
S4 S 0.72474(14) 0.23316(14) 0.08211(13) 0.0466(4) Uani 1 1 d . . .
S5 S 0.72840(13) 0.47342(13) 0.37189(12) 0.0426(3) Uani 1 1 d . . .
S6 S 0.49209(13) 0.43005(13) 0.25150(12) 0.0421(3) Uani 1 1 d . . .
S7 S 0.55122(14) 0.34762(13) 0.49998(12) 0.0427(3) Uani 1 1 d . . .
S8 S 0.32063(14) 0.30249(14) 0.36977(13) 0.0480(4) Uani 1 1 d . . .
O1 O 0.0275(4) 0.2757(4) 0.0426(3) 0.0481(10) Uani 1 1 d . . .
O2 O 0.2710(3) 0.3393(3) 0.0411(3) 0.0410(9) Uani 1 1 d . . .
O3 O 0.2000(4) 0.0918(4) -0.1431(3) 0.0487(10) Uani 1 1 d . . .
O4 O 0.0645(4) 0.1860(4) -0.1756(3) 0.0444(9) Uani 1 1 d . . .
O5 O -0.0580(3) 0.0188(3) -0.0992(3) 0.0436(9) Uani 1 1 d . . .
O6 O 0.1501(3) 0.1303(3) 0.0639(3) 0.0410(9) Uani 1 1 d . . .
O7 O 0.0744(5) 0.4671(4) 0.1691(4) 0.0737(14) Uani 1 1 d . . .
O8 O 0.3349(5) 0.5276(4) 0.1796(4) 0.0712(14) Uani 1 1 d . . .
O9 O 0.2056(5) 0.0006(5) -0.3185(4) 0.0778(15) Uani 1 1 d . . .
O10 O 0.0733(5) 0.1134(4) -0.3511(3) 0.0670(13) Uani 1 1 d . . .
C1 C 0.1053(6) 0.3894(6) 0.1100(5) 0.0434(13) Uani 1 1 d . . .
C2 C 0.2505(6) 0.4267(5) 0.1131(5) 0.0463(14) Uani 1 1 d . . .
C3 C 0.1749(6) 0.0662(6) -0.2424(5) 0.0507(15) Uani 1 1 d . . .
C4 C 0.0982(5) 0.1260(5) -0.2609(5) 0.0436(13) Uani 1 1 d . . .
C5 C 0.0600(5) 0.0326(5) 0.0477(4) 0.0353(12) Uani 1 1 d . . .
C11 C 0.5229(5) 0.1196(5) 0.1520(4) 0.0384(12) Uani 1 1 d . . .
C12 C 0.5655(5) 0.1677(5) 0.0861(4) 0.0403(12) Uani 1 1 d . . .
C13 C 0.3791(5) 0.0179(5) 0.2460(4) 0.0407(13) Uani 1 1 d . . .
C14 C 0.5013(5) 0.0500(5) 0.2904(4) 0.0408(13) Uani 1 1 d . . .
C15 C 0.5708(6) 0.2363(5) -0.0529(4) 0.0429(13) Uani 1 1 d . . .
C16 C 0.6971(6) 0.2724(5) -0.0110(5) 0.0452(14) Uani 1 1 d . . .
C17 C 0.2564(8) -0.0465(8) 0.2723(7) 0.0591(18) Uani 1 1 d . . .
C18 C 0.5422(8) 0.0353(8) 0.3809(6) 0.0526(16) Uani 1 1 d . . .
C19 C 0.5211(9) 0.2553(8) -0.1364(7) 0.0628(19) Uani 1 1 d . . .
C20 C 0.8125(9) 0.3445(9) -0.0389(8) 0.0627(19) Uani 1 1 d . . .
C21 C 0.5621(5) 0.4156(5) 0.3474(4) 0.0358(12) Uani 1 1 d . . .
C22 C 0.4868(5) 0.3618(5) 0.4012(4) 0.0380(12) Uani 1 1 d . . .
C23 C 0.7465(5) 0.5261(5) 0.2817(4) 0.0405(12) Uani 1 1 d . . .
C24 C 0.6365(5) 0.5053(5) 0.2257(4) 0.0385(12) Uani 1 1 d . . .
C25 C 0.4017(5) 0.2683(5) 0.5190(4) 0.0408(13) Uani 1 1 d . . .
C26 C 0.2954(6) 0.2490(5) 0.4590(5) 0.0438(13) Uani 1 1 d . . .
C27 C 0.8822(6) 0.5870(7) 0.2725(6) 0.0499(15) Uani 1 1 d . . .
C28 C 0.6277(9) 0.5407(9) 0.1427(7) 0.0559(18) Uani 1 1 d . . .
C29 C 0.4061(9) 0.2268(8) 0.5987(7) 0.0538(17) Uani 1 1 d . . .
C30 C 0.1567(7) 0.1857(8) 0.4610(8) 0.0600(18) Uani 1 1 d . . .
O51 O 0.1372(6) -0.1248(5) -0.5487(5) 0.0674(14) Uani 1 1 d . . .
O52 O 0.2801(7) 0.7391(7) 0.3469(6) 0.094(2) Uani 1 1 d . . .
N101 N 0.019(4) -0.229(4) -0.256(4) 0.27(2) Uani 0.50 1 d P . .
C101 C 0.010(2) -0.309(3) -0.326(3) 0.114(9) Uani 0.50 1 d P . .
C102 C 0.0045(9) -0.4019(13) -0.4086(9) 0.097(3) Uani 1 1 d . . .
C103 C -0.0648(9) -0.5164(13) -0.4243(10) 0.092(3) Uani 1 1 d . . .
C104 C 0.0710(9) -0.3862(13) -0.4860(11) 0.099(3) Uani 1 1 d . . .
H1 H 0.191(9) -0.085(8) 0.218(7) 0.10(3) Uiso 1 1 d . . .
H2 H 0.251(11) -0.114(10) 0.267(9) 0.16(5) Uiso 1 1 d . . .
H3 H 0.265(8) -0.009(7) 0.349(7) 0.10(3) Uiso 1 1 d . . .
H4 H 0.577(8) 0.108(7) 0.452(7) 0.10(3) Uiso 1 1 d . . .
H5 H 0.599(8) 0.000(7) 0.360(6) 0.09(3) Uiso 1 1 d . . .
H6 H 0.476(6) -0.013(6) 0.388(5) 0.047(19) Uiso 1 1 d . . .
H7 H -0.458(8) -0.183(7) -0.811(7) 0.09(3) Uiso 1 1 d . . .
H8 H -0.584(7) -0.288(7) -0.832(6) 0.08(2) Uiso 1 1 d . . .
H9 H -0.482(7) -0.306(7) -0.893(6) 0.09(3) Uiso 1 1 d . . .
H10 H 0.853(8) 0.415(7) 0.009(7) 0.08(3) Uiso 1 1 d . . .
H11 H 0.866(7) 0.309(6) -0.050(6) 0.07(2) Uiso 1 1 d . . .
H12 H 0.789(8) 0.329(7) -0.105(7) 0.10(3) Uiso 1 1 d . . .
H13 H 0.873(5) 0.606(5) 0.219(4) 0.038(15) Uiso 1 1 d . . .
H14 H 0.916(6) 0.533(6) 0.230(5) 0.056(18) Uiso 1 1 d . . .
H15 H 0.943(6) 0.641(6) 0.344(5) 0.057(18) Uiso 1 1 d . . .
H16 H 0.539(12) 0.519(10) 0.114(9) 0.16(5) Uiso 1 1 d . . .
H17 H 0.640(8) 0.502(8) 0.089(7) 0.09(3) Uiso 1 1 d . . .
H18 H 0.654(10) 0.608(9) 0.169(8) 0.11(5) Uiso 1 1 d . . .
H19 H 0.440(10) 0.165(10) 0.569(8) 0.15(4) Uiso 1 1 d . . .
H20 H 0.459(8) 0.286(8) 0.652(7) 0.09(3) Uiso 1 1 d . . .
H21 H 0.333(7) 0.208(6) 0.618(6) 0.07(2) Uiso 1 1 d . . .
H22 H 0.106(8) 0.130(7) 0.389(7) 0.09(3) Uiso 1 1 d . . .
H23 H 0.121(9) 0.230(8) 0.472(7) 0.11(4) Uiso 1 1 d . . .
H24 H 0.152(7) 0.138(7) 0.490(6) 0.09(3) Uiso 1 1 d . . .
H103 H -0.130(8) 0.468(7) -0.381(7) 0.10(3) Uiso 1 1 d . . .
H104 H 0.114(8) -0.295(7) -0.458(6) 0.09(3) Uiso 1 1 d . . .
H51 H -0.081(8) 0.117(7) -0.425(7) 0.09(3) Uiso 1 1 d . . .
H52 H -0.150(9) 0.085(8) -0.516(8) 0.11(4) Uiso 1 1 d . . .
H53 H -0.242(7) 0.317(7) -0.298(6) 0.06(3) Uiso 1 1 d . . .
H54 H -0.221(8) 0.244(8) -0.368(7) 0.09(3) Uiso 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'
N N 0.0061 0.0033 '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 Fe O1 82.31(16) . . ?
O2 Fe O3 96.55(16) . . ?
O1 Fe O3 173.67(17) . . ?
O2 Fe O4 100.47(15) . . ?
O1 Fe O4 92.59(16) . . ?
O3 Fe O4 81.47(16) . . ?
O2 Fe O6 90.46(14) . . ?
O1 Fe O6 97.20(16) . . ?
O3 Fe O6 89.02(15) . . ?
O4 Fe O6 166.22(16) . . ?
O2 Fe O5 166.43(15) . . ?
O1 Fe O5 90.30(16) . . ?
O3 Fe O5 92.01(16) . . ?
O4 Fe O5 91.18(14) . . ?
O6 Fe O5 79.14(13) . . ?
C11 S1 C13 95.6(3) . . ?
C11 S2 C14 96.5(3) . . ?
C12 S3 C15 96.1(3) . . ?
C12 S4 C16 96.1(3) . . ?
C21 S5 C23 95.9(3) . . ?
C21 S6 C24 95.9(3) . . ?
C22 S7 C25 95.7(3) . . ?
C22 S8 C26 95.8(3) . . ?
C1 O1 Fe 114.6(3) . . ?
C2 O2 Fe 114.7(3) . . ?
C3 O3 Fe 115.2(4) . . ?
C4 O4 Fe 114.7(3) . . ?
C5 O5 Fe 113.9(3) 2 . ?
C5 O6 Fe 113.9(3) . . ?
O7 C1 O1 126.5(6) . . ?
O7 C1 C2 119.1(6) . . ?
O1 C1 C2 114.4(5) . . ?
O8 C2 O2 124.7(6) . . ?
O8 C2 C1 121.4(6) . . ?
O2 C2 C1 113.8(5) . . ?
O9 C3 O3 125.6(6) . . ?
O9 C3 C4 120.6(5) . . ?
O3 C3 C4 113.8(5) . . ?
O10 C4 O4 125.5(6) . . ?
O10 C4 C3 120.3(6) . . ?
O4 C4 C3 114.2(5) . . ?
O5 C5 O6 127.0(4) 2 . ?
O5 C5 C5 116.6(6) 2 2 ?
O6 C5 C5 116.4(5) . 2 ?
C12 C11 S2 124.4(4) . . ?
C12 C11 S1 120.8(4) . . ?
S2 C11 S1 114.8(3) . . ?
C11 C12 S4 124.4(4) . . ?
C11 C12 S3 120.6(4) . . ?
S4 C12 S3 115.0(3) . . ?
C14 C13 C17 126.7(6) . . ?
C14 C13 S1 117.0(4) . . ?
C17 C13 S1 116.3(5) . . ?
C13 C14 C18 126.3(6) . . ?
C13 C14 S2 116.0(4) . . ?
C18 C14 S2 117.7(5) . . ?
C16 C15 C19 127.2(6) . . ?
C16 C15 S3 116.0(4) . . ?
C19 C15 S3 116.8(5) . . ?
C15 C16 C20 124.7(6) . . ?
C15 C16 S4 116.7(4) . . ?
C20 C16 S4 118.6(5) . . ?
C22 C21 S5 123.8(4) . . ?
C22 C21 S6 121.1(4) . . ?
S5 C21 S6 115.0(3) . . ?
C21 C22 S8 121.2(4) . . ?
C21 C22 S7 123.4(4) . . ?
S8 C22 S7 115.4(3) . . ?
C24 C23 C27 126.9(5) . . ?
C24 C23 S5 116.4(4) . . ?
C27 C23 S5 116.8(4) . . ?
C23 C24 C28 125.9(6) . . ?
C23 C24 S6 116.8(4) . . ?
C28 C24 S6 117.4(5) . . ?
C26 C25 C29 127.5(6) . . ?
C26 C25 S7 116.0(4) . . ?
C29 C25 S7 116.5(5) . . ?
C25 C26 C30 126.8(6) . . ?
C25 C26 S8 117.0(4) . . ?
C30 C26 S8 116.2(5) . . ?
N101 C101 C102 178(4) . . ?
C101 C102 C104 118(2) . . ?
C101 C102 C103 121.7(19) . . ?
C104 C102 C103 120.3(12) . . ?
C104 C103 C102 120.3(11) 2_544 . ?
C103 C104 C102 119.4(12) 2_544 . ?
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 O2 1.970(4) . ?
Fe O1 1.976(4) . ?
Fe O3 1.982(4) . ?
Fe O4 1.990(4) . ?
Fe O6 2.081(3) . ?
Fe O5 2.083(4) . ?
S1 C11 1.723(5) . ?
S1 C13 1.729(6) . ?
S2 C11 1.702(5) . ?
S2 C14 1.730(6) . ?
S3 C12 1.726(5) . ?
S3 C15 1.734(6) . ?
S4 C12 1.712(6) . ?
S4 C16 1.731(5) . ?
S5 C21 1.716(5) . ?
S5 C23 1.739(5) . ?
S6 C21 1.716(5) . ?
S6 C24 1.732(5) . ?
S7 C22 1.716(5) . ?
S7 C25 1.745(6) . ?
S8 C22 1.712(5) . ?
S8 C26 1.733(6) . ?
O1 C1 1.285(7) . ?
O2 C2 1.296(7) . ?
O3 C3 1.281(7) . ?
O4 C4 1.288(7) . ?
O5 C5 1.244(6) 2 ?
O6 C5 1.249(6) . ?
O7 C1 1.222(7) . ?
O8 C2 1.204(7) . ?
O9 C3 1.220(7) . ?
O10 C4 1.226(6) . ?
C1 C2 1.541(8) . ?
C3 C4 1.546(8) . ?
C5 O5 1.244(6) 2 ?
C5 C5 1.540(9) 2 ?
C11 C12 1.386(8) . ?
C13 C14 1.343(7) . ?
C13 C17 1.507(9) . ?
C14 C18 1.499(8) . ?
C15 C16 1.360(8) . ?
C15 C19 1.494(8) . ?
C16 C20 1.505(10) . ?
C21 C22 1.396(7) . ?
C23 C24 1.343(7) . ?
C23 C27 1.497(8) . ?
C24 C28 1.501(9) . ?
C25 C26 1.345(8) . ?
C25 C29 1.512(8) . ?
C26 C30 1.497(9) . ?
N101 C101 1.06(5) . ?
C101 C102 1.25(3) . ?
C102 C104 1.404(14) . ?
C102 C103 1.377(15) . ?
C103 C104 1.337(15) 2_544 ?
C104 C103 1.337(15) 2_544 ?
