#------------------------------------------------------------------------------
#$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $
#$Revision: 19 $
#$URL: svn://www.crystallography.net/cod/cif/4/4000022.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_4000022
_journal_name_full 'Chemistry of Materials'
_journal_year    2000
_chemical_name_systematic
;
1,2-Bis(ethylenedithiotetrathiafulvalene)ethane cation, tetrachloroferrate,
THF solvate
;
_chemical_name_common             'Bis(EDT-TTF)ethane,FeCl4,0.5 THF'
_chemical_formula_moiety          'C18H14S12,FeCl4,0.5(C4H8O)'
_chemical_formula_sum             'C20 H18 Cl4 Fe O0.50 S12'
_chemical_formula_weight          848.71
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'C2/c'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'
_cell_length_a                    14.5030(14)
_cell_length_b                    13.9152(14)
_cell_length_c                    31.148(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.644(10)
_cell_angle_gamma                 90.00
_cell_volume                      6285.6(10)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     5000
_cell_measurement_theta_min       2.1
_cell_measurement_theta_max       23.8
_exptl_crystal_description        'parallelepipedic plate'
_exptl_crystal_colour             'black'
_exptl_crystal_size_max           0.086
_exptl_crystal_size_mid           0.077
_exptl_crystal_size_min           0.008
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.794
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              3424
_exptl_absorpt_coefficient_mu     1.635
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_process_details    'FACEIT, Stoe-IPDS'
_exptl_absorpt_correction_T_min   0.7733
_exptl_absorpt_correction_T_max   0.9720
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_detector        'area detector'
_diffrn_measurement_device_type   'Stoe IPDS'
_diffrn_measurement_method        'rotation, Df = 0.8¡'
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_decay_%         0
_diffrn_reflns_number             17155
_diffrn_reflns_av_R_equivalents   0.1522
_diffrn_reflns_av_sigmaI/netI     0.2387
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -35
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          2.03
_diffrn_reflns_theta_max          23.96
_reflns_number_total              4811
_reflns_number_observed           1414
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4810
_refine_ls_number_parameters      326
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2077
_refine_ls_R_factor_obs           0.0458
_refine_ls_wR_factor_all          0.0728
_refine_ls_wR_factor_obs          0.0489
_refine_ls_goodness_of_fit_all    0.686
_refine_ls_goodness_of_fit_obs    0.962
_refine_ls_restrained_S_all       0.719
_refine_ls_restrained_S_obs       0.962
_refine_ls_shift/esd_max          0.014
_refine_ls_shift/esd_mean         0.001
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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
S1 S -0.03781(13) 0.1284(2) 0.40790(8) 0.0557(8) Uani 1 d . .
S2 S 0.08289(14) 0.1257(2) 0.48339(7) 0.0507(7) Uani 1 d . .
S3 S 0.13617(14) 0.1162(3) 0.34683(8) 0.0657(9) Uani 1 d . .
S4 S 0.26136(13) 0.1166(2) 0.42044(8) 0.0505(7) Uani 1 d . .
S5 S 0.2794(2) 0.1136(3) 0.28134(9) 0.1086(14) Uani 1 d . .
S6 S 0.43131(14) 0.1151(3) 0.36853(8) 0.0783(10) Uani 1 d . .
S7 S -0.38764(13) 0.1199(2) 0.55347(8) 0.0517(7) Uani 1 d . .
S8 S -0.51707(13) 0.1321(2) 0.48059(7) 0.0518(7) Uani 1 d . .
S9 S -0.55888(14) 0.1278(2) 0.61949(8) 0.0603(8) Uani 1 d . .
S10 S -0.68904(14) 0.1350(2) 0.54630(8) 0.0530(8) Uani 1 d . .
S11 S -0.7001(2) 0.1183(2) 0.68581(9) 0.0739(9) Uani 1 d . .
S12 S -0.85615(14) 0.1267(2) 0.59838(8) 0.0695(9) Uani 1 d . .
C1 C -0.1946(5) 0.1240(7) 0.4567(2) 0.042(2) Uani 1 d . .
H1A H -0.2158(5) 0.0696(7) 0.4398(2) 0.050 Uiso 1 calc R .
H1B H -0.2165(5) 0.1821(7) 0.4427(2) 0.050 Uiso 1 calc R .
C2 C -0.0906(5) 0.1246(7) 0.4576(3) 0.043(2) Uani 1 d . .
C3 C -0.0356(5) 0.1233(7) 0.4912(3) 0.045(3) Uani 1 d . .
H3 H -0.0595(5) 0.1212(7) 0.5187(3) 0.054 Uiso 1 calc R .
C4 C 0.0738(5) 0.1247(7) 0.4281(3) 0.045(3) Uani 1 d . .
C5 C 0.1469(5) 0.1229(7) 0.4026(3) 0.048(3) Uani 1 d . .
C6 C 0.2537(5) 0.1137(8) 0.3361(3) 0.055(3) Uani 1 d . .
C7 C 0.3115(5) 0.1172(7) 0.3695(3) 0.043(3) Uani 1 d . .
C8 C 0.3993(7) 0.0917(11) 0.2828(3) 0.126(6) Uani 1 d . .
H8A H 0.4105(7) 0.0429(11) 0.2613(3) 0.151 Uiso 1 calc R .
H8B H 0.4281(7) 0.1501(11) 0.2724(3) 0.151 Uiso 1 calc R .
C9 C 0.4483(7) 0.0650(10) 0.3179(3) 0.102(5) Uani 1 d . .
H9A H 0.5127(7) 0.0747(10) 0.3112(3) 0.123 Uiso 1 calc R .
H9B H 0.4397(7) -0.0038(10) 0.3210(3) 0.123 Uiso 1 calc R .
C10 C -0.2362(5) 0.1179(8) 0.5012(3) 0.048(3) Uani 1 d . .
H10A H -0.2157(5) 0.0586(8) 0.5147(3) 0.058 Uiso 1 calc R .
H10B H -0.2123(5) 0.1707(8) 0.5184(3) 0.058 Uiso 1 calc R .
C11 C -0.3406(5) 0.1210(7) 0.5021(3) 0.044(2) Uani 1 d . .
C12 C -0.4008(5) 0.1264(7) 0.4694(3) 0.049(3) Uani 1 d . .
H12 H -0.3805(5) 0.1271(7) 0.4412(3) 0.059 Uiso 1 calc R .
C13 C -0.5028(5) 0.1299(7) 0.5366(3) 0.041(2) Uani 1 d . .
C14 C -0.5741(5) 0.1301(7) 0.5634(3) 0.046(2) Uani 1 d . .
C15 C -0.6773(5) 0.1267(7) 0.6308(3) 0.050(3) Uani 1 d . .
C16 C -0.7360(5) 0.1290(7) 0.5974(3) 0.047(3) Uani 1 d . .
C17 C -0.8149(7) 0.0774(12) 0.6837(4) 0.141(7) Uani 1 d . .
H17A H -0.8130(7) 0.0085(12) 0.6790(4) 0.169 Uiso 1 calc R .
H17B H -0.8409(7) 0.0874(12) 0.7119(4) 0.169 Uiso 1 calc R .
C18 C -0.8754(7) 0.1143(12) 0.6546(3) 0.123(6) Uani 1 d . .
H18A H -0.8905(7) 0.1782(12) 0.6649(3) 0.147 Uiso 1 calc R .
H18B H -0.9313(7) 0.0765(12) 0.6572(3) 0.147 Uiso 1 calc R .
Fe Fe -0.32675(8) 0.29232(12) 0.34255(4) 0.0634(4) Uani 1 d . .
Cl1 Cl -0.4084(2) 0.3243(3) 0.28624(8) 0.1121(13) Uani 1 d . .
Cl2 Cl -0.3917(2) 0.3600(3) 0.39805(8) 0.0964(10) Uani 1 d . .
Cl3 Cl -0.3213(2) 0.1370(2) 0.35238(9) 0.0949(10) Uani 1 d . .
Cl4 Cl -0.1877(2) 0.3438(3) 0.33708(13) 0.142(2) Uani 1 d . .
C19 C 0.0607(10) 0.1819(11) 0.2263(5) 0.163(6) Uiso 1 d . .
H19A H 0.0491(10) 0.1875(11) 0.1957(5) 0.196 Uiso 1 calc R .
H19B H 0.1249(10) 0.1975(11) 0.2319(5) 0.196 Uiso 1 calc R .
C20 C 0.0426(9) 0.0886(11) 0.2397(5) 0.179(7) Uiso 1 d . .
H20A H 0.0907(9) 0.0669(11) 0.2593(5) 0.214 Uiso 1 calc R .
H20B H 0.0408(9) 0.0456(11) 0.2152(5) 0.214 Uiso 1 calc R .
O1 O 0.0000 0.2495(17) 0.2500 0.267(10) Uiso 1 d S .
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
S1 0.0278(13) 0.084(2) 0.055(2) -0.001(2) 0.0085(11) -0.006(2)
S2 0.0310(13) 0.065(2) 0.056(2) 0.009(2) 0.0072(11) 0.0041(15)
S3 0.0301(14) 0.108(3) 0.059(2) 0.001(2) 0.0070(13) -0.001(2)
S4 0.0297(12) 0.066(2) 0.056(2) 0.007(2) 0.0060(12) 0.0077(14)
S5 0.054(2) 0.219(4) 0.053(2) 0.010(3) 0.0121(14) 0.025(3)
S6 0.0347(14) 0.133(3) 0.068(2) -0.001(2) 0.0093(13) 0.011(2)
S7 0.0297(13) 0.067(2) 0.059(2) 0.004(2) 0.0059(11) 0.0030(15)
S8 0.0290(12) 0.066(2) 0.060(2) -0.006(2) 0.0067(11) -0.0004(15)
S9 0.0344(14) 0.087(2) 0.060(2) 0.006(2) 0.0051(12) 0.006(2)
S10 0.0287(12) 0.070(2) 0.060(2) -0.005(2) 0.0078(11) -0.0042(15)
S11 0.063(2) 0.098(2) 0.061(2) 0.000(2) 0.0177(14) -0.006(2)
S12 0.0306(13) 0.101(2) 0.078(2) -0.007(2) 0.0160(13) -0.007(2)
C1 0.025(5) 0.057(7) 0.044(6) -0.007(6) 0.016(4) 0.004(5)
C2 0.032(5) 0.036(7) 0.060(7) 0.006(6) -0.003(5) 0.000(5)
C3 0.037(5) 0.059(7) 0.038(6) 0.018(7) 0.023(5) 0.007(6)
C4 0.036(5) 0.034(7) 0.065(7) 0.005(6) 0.015(5) -0.007(6)
C5 0.041(5) 0.045(7) 0.060(7) 0.003(6) 0.009(5) 0.000(6)
C6 0.034(5) 0.085(9) 0.046(6) 0.003(7) 0.009(5) 0.012(6)
C7 0.032(5) 0.066(8) 0.032(5) -0.005(6) 0.010(4) -0.002(5)
C8 0.062(8) 0.263(19) 0.054(7) -0.012(10) 0.022(6) 0.037(10)
C9 0.068(7) 0.186(14) 0.053(7) -0.029(8) 0.010(6) 0.026(8)
C10 0.025(5) 0.054(8) 0.065(6) 0.008(6) 0.005(4) -0.004(5)
C11 0.028(5) 0.053(7) 0.052(6) 0.003(6) 0.024(4) -0.003(5)
C12 0.035(5) 0.051(7) 0.063(6) 0.004(7) 0.009(5) -0.005(6)
C13 0.025(5) 0.044(7) 0.055(6) 0.008(6) 0.006(4) -0.002(5)
C14 0.028(5) 0.050(7) 0.061(7) 0.006(6) 0.011(4) 0.003(5)
C15 0.038(5) 0.051(7) 0.061(7) -0.006(7) 0.017(5) 0.012(6)
C16 0.043(5) 0.054(7) 0.044(6) -0.001(6) 0.012(5) 0.002(6)
C17 0.058(8) 0.274(21) 0.091(11) 0.079(12) 0.032(7) 0.002(10)
C18 0.063(7) 0.241(17) 0.064(8) 0.032(11) 0.039(6) -0.008(10)
Fe 0.0496(7) 0.0734(11) 0.0671(9) -0.0048(10) 0.0011(6) -0.0012(9)
Cl1 0.105(2) 0.169(4) 0.062(2) 0.003(2) -0.005(2) 0.030(2)
Cl2 0.112(2) 0.111(3) 0.067(2) -0.018(2) 0.007(2) 0.021(2)
Cl3 0.093(2) 0.077(2) 0.114(2) 0.001(2) -0.003(2) 0.006(2)
Cl4 0.077(2) 0.149(4) 0.200(4) -0.016(3) 0.017(2) -0.040(2)