Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_etfetdas _database_code_CSD 156842 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'John A. Schlueter' 'Eugenio Coronado' 'P. Deplano' 'Urs Geiser' 'Carlos J. Gomez-Garcia' 'A. Kini' 'Hyun-Joo Koo' 'Laura Leoni' 'Jamie L. Manson' 'Maria Laura Mercuri' 'Hau H. Wang' 'M. Whangbo' _publ_contact_author_name 'Dr John A Schlueter' _publ_contact_author_address ; Dr John A Schlueter Materials Science Division Argonne National Laboratory 9700 South Cass Avenue Building 200 Room A 185 Argonne Illinois 60439 UNITED STATES OF AMERICA ; _publ_contact_author_email 'JASCHLUETER@ANL.GOV' _publ_section_title ; A two dimensional radical salt based upon BEDT-TTF and the dimeric anion [Fe(tdas)2]22-: (BEDT-TTF)2[Fe(tdas)2] (tdas = 1,2,5-thiadiazole-3,4-dithiolate) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethylenedithio)tetrathiafulvalenium bis(1,2,5-thiadizole-3,4-dithiol) iron(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C10 H8 S8)2 Fe (C2 S3 N2)2' _chemical_formula_sum 'C24 H16 Fe N4 S22' _chemical_formula_weight 1121.58 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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' _cell_length_a 11.6342(12) _cell_length_b 4.1608(5) _cell_length_c 40.513(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.070(6) _cell_angle_gamma 90.00 _cell_volume 1941.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2939 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 28.36 _exptl_crystal_description 'triangular plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type none _exptl_special_details ; The first 50 frames of the data collection were repeated in the end (after 13 hours). From the comparison of the repeatedly measured reflections, no decay was noted, and no decay correction was therefore applied. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12582 _diffrn_reflns_av_R_equivalents 0.1211 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.36 _reflns_number_total 4620 _reflns_number_gt 2582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4620 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2474 _refine_ls_R_factor_gt 0.1918 _refine_ls_wR_factor_ref 0.4876 _refine_ls_wR_factor_gt 0.4787 _refine_ls_goodness_of_fit_ref 2.569 _refine_ls_restrained_S_all 2.569 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.010 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 S1 S 0.8393(4) 0.5542(14) 0.18962(10) 0.0513(13) Uani 1 1 d . . . S2 S 0.6059(4) 0.2936(14) 0.18970(10) 0.0543(14) Uani 1 1 d . . . S3 S 0.8791(4) 0.5435(14) 0.27016(10) 0.0525(14) Uani 1 1 d . . . S4 S 0.6426(4) 0.2923(15) 0.26994(10) 0.0560(14) Uani 1 1 d . . . S5 S 0.8306(4) 0.5648(13) 0.11679(10) 0.0478(12) Uani 1 1 d . . . S6 S 0.5446(4) 0.2824(13) 0.11657(11) 0.0518(13) Uani 1 1 d . . . S7 S 0.9370(4) 0.5709(13) 0.34282(10) 0.0479(12) Uani 1 1 d . . . S8 S 0.6544(4) 0.2657(14) 0.34253(10) 0.0525(13) Uani 1 1 d . . . C1 C 0.7344(17) 0.422(5) 0.2119(3) 0.047(5) Uani 1 1 d . . . C2 C 0.7484(13) 0.414(4) 0.2473(3) 0.037(4) Uani 1 1 d . . . C3 C 0.7567(14) 0.477(4) 0.1501(4) 0.038(4) Uani 1 1 d . . . C4 C 0.6524(15) 0.371(4) 0.1504(4) 0.040(4) Uani 1 1 d . . . C5 C 0.8347(15) 0.473(4) 0.3094(4) 0.044(4) Uani 1 1 d . . . C6 C 0.7217(15) 0.360(4) 0.3088(3) 0.037(4) Uani 1 1 d . . . C7 C 0.7354(17) 0.382(5) 0.0847(4) 0.051(5) Uani 1 1 d . . . H7A H 0.7583 0.4475 0.0636 0.061 Uiso 1 1 calc R . . H7B H 0.7467 0.1510 0.0865 0.061 Uiso 1 1 calc R . . C8 C 0.6112(16) 0.447(5) 0.0834(4) 0.050(5) Uani 1 1 d . . . H8A H 0.5713 0.3629 0.0625 0.060 Uiso 1 1 calc R . . H8B H 0.5999 0.6776 0.0831 0.060 Uiso 1 1 calc R . . C9 C 0.8766(14) 0.386(4) 0.3764(3) 0.041(4) Uani 1 1 d . . . H9A H 0.8879 0.1551 0.3753 0.049 Uiso 1 1 calc R . . H9B H 0.9185 0.4611 0.3973 0.049 Uiso 1 1 calc R . . C10 C 0.7464(18) 0.455(5) 0.3759(4) 0.059(6) Uani 1 1 d . . . H10A H 0.7342 0.6852 0.3743 0.071 Uiso 1 1 calc R . . H10B H 0.7237 0.3837 0.3968 0.071 Uiso 1 1 calc R . . Fe1 Fe 0.0019(5) 0.6117(11) -0.00489(13) 0.0481(14) Uiso 0.50 1 d P . . S11 S 0.0983(5) 0.146(2) -0.02838(13) 0.089(2) Uani 1 1 d . . . S12 S 0.1314(6) 0.4530(17) 0.04596(12) 0.088(2) Uani 1 1 d . . . S13 S 0.4039(7) -0.0797(19) 0.02595(15) 0.091(2) Uani 1 1 d . . . N1 N 0.304(2) -0.055(6) -0.0078(5) 0.105(9) Uani 1 1 d . . . N2 N 0.332(2) 0.131(6) 0.0501(5) 0.102(8) Uani 1 1 d . . . C11 C 0.2264(19) 0.130(6) -0.0015(4) 0.068(7) Uani 1 1 d . . . C12 C 0.237(2) 0.213(7) 0.0330(5) 0.078(8) Uani 1 1 d . . . 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 0.043(3) 0.088(4) 0.0201(19) -0.004(2) -0.0033(18) -0.011(2) S2 0.048(3) 0.091(4) 0.023(2) 0.002(2) 0.0004(19) -0.009(3) S3 0.042(3) 0.093(4) 0.0211(19) 0.002(2) 0.0014(18) -0.014(2) S4 0.047(3) 0.101(4) 0.0195(19) 0.001(2) 0.0030(18) -0.014(3) S5 0.044(2) 0.074(3) 0.0235(19) 0.008(2) -0.0010(17) -0.010(2) S6 0.046(3) 0.076(3) 0.031(2) -0.008(2) -0.0027(19) -0.005(2) S7 0.045(3) 0.072(3) 0.024(2) 0.003(2) -0.0028(18) -0.015(2) S8 0.050(3) 0.082(3) 0.026(2) 0.009(2) 0.009(2) -0.001(3) C1 0.069(12) 0.060(11) 0.011(7) 0.003(8) -0.006(7) 0.003(9) C2 0.043(9) 0.055(10) 0.012(6) -0.009(7) 0.005(6) -0.011(8) C3 0.040(9) 0.048(10) 0.026(8) -0.007(7) 0.002(7) -0.003(7) C4 0.052(11) 0.048(10) 0.022(7) -0.010(7) 0.011(7) 0.010(8) C5 0.043(10) 0.052(11) 0.034(9) -0.006(8) -0.002(8) 0.006(8) C6 0.056(11) 0.040(9) 0.011(6) -0.004(6) -0.013(6) 0.008(8) C7 0.076(14) 0.047(10) 0.030(9) -0.006(8) 0.008(9) -0.017(10) C8 0.059(12) 0.066(12) 0.021(8) -0.001(8) -0.009(8) -0.020(10) C9 0.058(11) 0.062(11) 0.002(6) -0.003(7) 0.007(6) 0.001(9) C10 0.082(14) 0.068(13) 0.026(9) 0.014(9) 0.001(9) 0.044(11) S11 0.074(4) 0.159(6) 0.038(3) -0.052(4) 0.021(3) -0.060(4) S12 0.122(5) 0.115(5) 0.031(3) -0.022(3) 0.021(3) -0.079(4) S13 0.121(6) 0.103(5) 0.042(3) 0.001(3) -0.014(3) -0.015(4) N1 0.14(2) 0.113(18) 0.052(11) 0.042(13) -0.038(13) -0.068(16) N2 0.15(2) 0.109(16) 0.042(10) 0.036(12) -0.013(13) -0.059(16) C11 0.077(15) 0.110(19) 0.015(8) -0.032(10) -0.007(9) 0.037(14) C12 0.096(18) 0.102(18) 0.038(11) -0.018(13) 0.010(12) -0.055(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 S1 C1 1.709(19) . ? S1 C3 1.778(16) . ? S2 C1 1.719(19) . ? S2 C4 1.783(16) . ? S3 C2 1.750(16) . ? S3 C5 1.762(17) . ? S4 C2 1.712(15) . ? S4 C6 1.733(14) . ? S5 C3 1.736(16) . ? S5 C7 1.760(17) . ? S6 C4 1.761(17) . ? S6 C8 1.780(17) . ? S7 C5 1.722(17) . ? S7 C9 1.789(15) . ? S8 C6 1.712(16) . ? S8 C10 1.78(2) . ? C1 C2 1.420(19) . ? C3 C4 1.29(2) . ? C5 C6 1.39(2) . ? C7 C8 1.46(3) . ? C9 C10 1.54(2) . ? Fe1 Fe1 1.014(9) 3_565 ? Fe1 S12 2.126(8) 3_565 ? Fe1 S11 2.154(8) 3_565 ? Fe1 S12 2.465(9) . ? Fe1 S11 2.495(9) . ? Fe1 S11 2.720(8) 1_565 ? S11 C11 1.72(2) . ? S11 Fe1 2.154(8) 3_565 ? S11 Fe1 2.720(8) 1_545 ? S12 C12 1.72(3) . ? S12 Fe1 2.126(8) 3_565 ? S13 N2 1.63(3) . ? S13 N1 1.67(2) . ? N1 C11 1.24(3) . ? N2 C12 1.27(3) . ? C11 C12 1.43(3) . ? 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 C1 S1 C3 94.8(8) . . ? C1 S2 C4 93.5(8) . . ? C2 S3 C5 94.7(7) . . ? C2 S4 C6 96.2(8) . . ? C3 S5 C7 98.9(8) . . ? C4 S6 C8 99.7(8) . . ? C5 S7 C9 101.2(8) . . ? C6 S8 C10 102.1(9) . . ? C2 C1 S1 123.5(14) . . ? C2 C1 S2 119.4(14) . . ? S1 C1 S2 117.1(8) . . ? C1 C2 S4 123.9(13) . . ? C1 C2 S3 119.7(12) . . ? S4 C2 S3 116.4(8) . . ? C4 C3 S5 130.2(13) . . ? C4 C3 S1 116.3(12) . . ? S5 C3 S1 113.5(9) . . ? C3 C4 S6 129.2(13) . . ? C3 C4 S2 118.2(13) . . ? S6 C4 S2 112.6(10) . . ? C6 C5 S7 129.6(13) . . ? C6 C5 S3 116.0(12) . . ? S7 C5 S3 114.4(10) . . ? C5 C6 S8 127.0(12) . . ? C5 C6 S4 116.6(12) . . ? S8 C6 S4 116.3(10) . . ? C8 C7 S5 117.5(13) . . ? C7 C8 S6 115.7(13) . . ? C10 C9 S7 113.6(12) . . ? C9 C10 S8 114.3(12) . . ? Fe1 Fe1 S12 97.0(7) 3_565 3_565 ? Fe1 Fe1 S11 97.4(6) 3_565 3_565 ? S12 Fe1 S11 98.6(3) 3_565 3_565 ? Fe1 Fe1 S12 58.9(6) 3_565 . ? S12 Fe1 S12 155.9(2) 3_565 . ? S11 Fe1 S12 85.6(3) 3_565 . ? Fe1 Fe1 S11 58.9(6) 3_565 . ? S12 Fe1 S11 85.4(3) 3_565 . ? S11 Fe1 S11 156.2(2) 3_565 . ? S12 Fe1 S11 81.7(3) . . ? Fe1 Fe1 S11 158.2(7) 3_565 1_565 ? S12 Fe1 S11 96.9(3) 3_565 1_565 ? S11 Fe1 S11 97.0(2) 3_565 1_565 ? S12 Fe1 S11 106.1(3) . 1_565 ? S11 Fe1 S11 105.8(3) . 1_565 ? C11 S11 Fe1 96.8(6) . 3_565 ? C11 S11 Fe1 100.5(7) . . ? Fe1 S11 Fe1 23.8(2) 3_565 . ? C11 S11 Fe1 96.4(10) . 1_545 ? Fe1 S11 Fe1 83.0(2) 3_565 1_545 ? Fe1 S11 Fe1 105.8(3) . 1_545 ? C12 S12 Fe1 99.3(8) . 3_565 ? C12 S12 Fe1 106.2(8) . . ? Fe1 S12 Fe1 24.1(2) 3_565 . ? N2 S13 N1 95.8(14) . . ? C11 N1 S13 108.2(19) . . ? C12 N2 S13 107.4(17) . . ? N1 C11 C12 113(2) . . ? N1 C11 S11 118.9(16) . . ? C12 C11 S11 124.0(18) . . ? N2 C12 C11 115(2) . . ? N2 C12 S12 127(2) . . ? C11 C12 S12 118(2) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 2.104 _refine_diff_density_min -1.919 _refine_diff_density_rms 0.310