Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Auban-Senzier, Pascale' 'Canadell, Enric' 'Devic, Thomas' 'Domercq, Benoit' 'Fourmigue, Marc' _publ_contact_author_name 'Dr Marc Fourmigue' _publ_contact_author_address ; Dr Marc Fourmigue Sciences Moleculaires aux Interfaces FRE 2068 CNRS, Institut des Mat Jean Rouxel 2, rue de la Houssiniere Nantes BP32229, F-44322 cedex 3 FRANCE ; _publ_contact_author_email 'Marc.Fourmigue@cnrs-imn.fr' data_mf170eabs _database_code_CSD 155958 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(3,4-dibromo-3',4'-ethylenedithiotetrathiafulvalene) dibromoiodide ; _chemical_name_common '(EDT-TTFBr2)2 IBr2' _chemical_melting_point ? _chemical_formula_moiety '(C8H4S6Br2)2IBr2' _chemical_formula_sum 'C16 H8 Br6 I S12' _chemical_formula_weight 1191.30 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7026(13) _cell_length_b 7.4586(15) _cell_length_c 15.789(3) _cell_angle_alpha 95.60(3) _cell_angle_beta 98.47(3) _cell_angle_gamma 104.20(3) _cell_volume 749.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5822 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'thick plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 559 _exptl_absorpt_coefficient_mu 9.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0985 _exptl_absorpt_correction_T_max 0.1721 _exptl_absorpt_process_details 'SHELX XPREP' _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_measurement_device_type 'area detector' _diffrn_measurement_method 'rotation, phi incr. 1.5 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7378 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.95 _reflns_number_total 2718 _reflns_number_gt 2154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe-IPDS)' _computing_cell_refinement 'SELECT, CELL (Stoe-IPDS)' _computing_data_reduction 'INTEGRATE (Stoe-IPDS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0286P)^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 2718 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0528 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 I1 I 0.0000 0.0000 0.0000 0.04002(12) Uani 1 2 d S . . Br1 Br 0.35410(8) 0.22325(8) -0.03521(4) 0.05730(16) Uani 1 1 d . . . Br2 Br 0.50955(5) 0.00021(6) -0.20342(2) 0.03314(11) Uani 1 1 d . . . Br3 Br 0.98877(5) -0.00998(6) -0.26154(3) 0.03600(12) Uani 1 1 d . . . S1 S 0.32689(13) -0.16820(16) -0.39397(6) 0.0321(2) Uani 1 1 d . . . S2 S 0.73362(14) -0.17799(16) -0.44147(6) 0.0322(2) Uani 1 1 d . . . S3 S 0.49982(14) -0.35840(16) -0.63615(6) 0.0312(2) Uani 1 1 d . . . S4 S 0.09621(14) -0.34701(16) -0.58806(6) 0.0321(2) Uani 1 1 d . . . S5 S 0.31977(15) -0.53237(16) -0.81730(6) 0.0344(2) Uani 1 1 d . . . S6 S -0.15625(14) -0.51105(17) -0.75717(7) 0.0384(3) Uani 1 1 d . . . C2 C 0.7304(5) -0.0951(6) -0.3349(2) 0.0281(9) Uani 1 1 d . . . C1 C 0.5474(5) -0.0907(6) -0.3128(2) 0.0270(8) Uani 1 1 d . . . C3 C 0.4635(5) -0.2261(6) -0.4740(2) 0.0267(8) Uani 1 1 d . . . C4 C 0.3647(5) -0.3024(6) -0.5552(2) 0.0276(9) Uani 1 1 d . . . C5 C 0.2781(5) -0.4488(6) -0.7165(2) 0.0273(8) Uani 1 1 d . . . C6 C 0.0911(5) -0.4430(6) -0.6937(2) 0.0264(8) Uani 1 1 d . . . C7 C 0.0960(6) -0.4894(7) -0.8834(3) 0.0350(10) Uani 1 1 d . . . H7A H 0.1084 -0.3562 -0.8759 0.042 Uiso 1 1 calc R . . H7B H 0.0980 -0.5278 -0.9437 0.042 Uiso 1 1 calc R . . C8 C -0.1101(6) -0.5896(7) -0.8623(3) 0.0376(10) Uani 1 1 d . . . H8A H -0.1179 -0.7218 -0.8661 0.045 Uiso 1 1 calc R . . H8B H -0.2213 -0.5749 -0.9057 0.045 Uiso 1 1 calc R . . 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 I1 0.0552(2) 0.0390(3) 0.0265(2) -0.00335(18) 0.00665(17) 0.01707(19) Br1 0.0615(3) 0.0560(4) 0.0526(3) -0.0014(3) 0.0215(2) 0.0091(2) Br2 0.02960(18) 0.0435(3) 0.02128(19) -0.00559(18) 0.00250(14) 0.00531(16) Br3 0.02590(18) 0.0468(3) 0.0312(2) 0.00039(19) -0.00376(15) 0.00913(17) S1 0.0234(4) 0.0486(7) 0.0211(5) -0.0050(5) 0.0018(3) 0.0085(4) S2 0.0252(4) 0.0461(7) 0.0252(5) -0.0027(5) 0.0035(4) 0.0127(4) S3 0.0261(4) 0.0441(7) 0.0222(5) -0.0042(4) 0.0015(4) 0.0122(4) S4 0.0266(4) 0.0455(7) 0.0222(5) -0.0042(5) 0.0033(4) 0.0096(4) S5 0.0338(5) 0.0479(7) 0.0215(5) -0.0053(5) 0.0030(4) 0.0158(4) S6 0.0258(5) 0.0541(8) 0.0288(5) -0.0095(5) 0.0003(4) 0.0071(4) C2 0.0270(17) 0.032(2) 0.0246(19) 0.0026(18) 0.0010(15) 0.0095(16) C1 0.0258(17) 0.033(2) 0.0211(18) -0.0002(17) 0.0012(14) 0.0097(15) C3 0.0279(18) 0.030(2) 0.0212(18) 0.0005(17) 0.0019(14) 0.0082(15) C4 0.0293(18) 0.027(2) 0.027(2) 0.0020(18) 0.0043(15) 0.0083(15) C5 0.0306(18) 0.029(2) 0.0205(18) -0.0013(17) 0.0027(15) 0.0078(16) C6 0.0287(18) 0.028(2) 0.0201(18) -0.0031(17) 0.0032(14) 0.0066(16) C7 0.038(2) 0.044(3) 0.023(2) 0.0029(19) 0.0021(16) 0.0142(19) C8 0.039(2) 0.043(3) 0.027(2) -0.005(2) -0.0011(17) 0.0101(19) _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 I1 Br1 2.7102(10) 2 ? I1 Br1 2.7102(10) . ? Br2 C1 1.869(4) . ? Br3 C2 1.863(3) . ? S1 C1 1.744(3) . ? S1 C3 1.747(4) . ? S2 C2 1.739(4) . ? S2 C3 1.744(3) . ? S3 C4 1.747(4) . ? S3 C5 1.749(4) . ? S4 C4 1.736(4) . ? S4 C6 1.742(4) . ? S5 C5 1.738(4) . ? S5 C7 1.811(4) . ? S6 C6 1.735(3) . ? S6 C8 1.801(4) . ? C2 C1 1.331(5) . ? C3 C4 1.352(5) . ? C5 C6 1.363(5) . ? C7 C8 1.502(6) . ? 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 Br1 I1 Br1 180.0 2 . ? C1 S1 C3 94.92(17) . . ? C2 S2 C3 94.52(17) . . ? C4 S3 C5 95.79(17) . . ? C4 S4 C6 95.91(18) . . ? C5 S5 C7 98.55(18) . . ? C6 S6 C8 103.90(18) . . ? C1 C2 S2 118.3(3) . . ? C1 C2 Br3 125.1(3) . . ? S2 C2 Br3 116.5(2) . . ? C2 C1 S1 117.0(3) . . ? C2 C1 Br2 125.4(3) . . ? S1 C1 Br2 117.60(19) . . ? C4 C3 S2 123.1(3) . . ? C4 C3 S1 121.7(3) . . ? S2 C3 S1 115.2(2) . . ? C3 C4 S4 123.1(3) . . ? C3 C4 S3 122.2(3) . . ? S4 C4 S3 114.8(2) . . ? C6 C5 S5 127.0(3) . . ? C6 C5 S3 116.3(3) . . ? S5 C5 S3 116.7(2) . . ? C5 C6 S6 128.8(3) . . ? C5 C6 S4 117.1(3) . . ? S6 C6 S4 114.1(2) . . ? C8 C7 S5 113.7(3) . . ? C7 C8 S6 114.9(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.491 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.103 #======END data_tde89absm _database_code_CSD 155959 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(3,4-dibromo-3',4'-ethylenedithiotetrathiafulvalene) triiodide ; _chemical_name_common '2(EDT-TTF-BR2), I3' _chemical_melting_point ? _chemical_formula_moiety '2(C8H4S6BR2), I3' _chemical_formula_sum 'C8 H4 Br2 I1.50 S6' _chemical_formula_weight 642.64 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7796(14) _cell_length_b 7.5112(15) _cell_length_c 16.117(3) _cell_angle_alpha 95.61(3) _cell_angle_beta 99.74(3) _cell_angle_gamma 103.10(3) _cell_volume 779.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6017 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.95 _exptl_crystal_description 'prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.3273 _exptl_crystal_size_mid 0.1155 _exptl_crystal_size_min 0.0674 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 595 _exptl_absorpt_coefficient_mu 8.946 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2375 _exptl_absorpt_correction_T_max 0.5689 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7779 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.95 _reflns_number_total 2854 _reflns_number_gt 2182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0190P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2854 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.845 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 I1 I 0.5000 0.5000 0.0000 0.03460(12) Uani 1 2 d S . . I2 I 0.13110(6) 0.27030(5) 0.03999(2) 0.04567(11) Uani 1 1 d . . . Br1 Br 0.50528(7) 1.50417(7) 0.26618(3) 0.03769(13) Uani 1 1 d . . . Br2 Br 0.97927(7) 1.49884(6) 0.21009(3) 0.03363(13) Uani 1 1 d . . . S1 S 0.76282(18) 1.67647(17) 0.44328(7) 0.0329(3) Uani 1 1 d . . . S2 S 1.16328(18) 1.66956(17) 0.39717(7) 0.0324(3) Uani 1 1 d . . . S3 S 0.99868(18) 1.14001(16) 0.36504(7) 0.0314(3) Uani 1 1 d . . . S4 S 0.60247(18) 1.14852(16) 0.41306(7) 0.0326(3) Uani 1 1 d . . . S5 S 0.81517(19) 0.96659(17) 0.18689(7) 0.0350(3) Uani 1 1 d . . . S6 S 0.34544(19) 0.98203(18) 0.24708(8) 0.0392(3) Uani 1 1 d . . . C1 C 0.7630(7) 1.5931(6) 0.3385(3) 0.0268(10) Uani 1 1 d . . . C2 C 0.9428(7) 1.5904(6) 0.3172(3) 0.0283(10) Uani 1 1 d . . . C3 C 1.0314(7) 1.7260(6) 0.4755(3) 0.0292(10) Uani 1 1 d . . . C4 C 0.8688(7) 1.1958(6) 0.4438(3) 0.0277(10) Uani 1 1 d . . . C5 C 0.7754(7) 1.0481(6) 0.2861(3) 0.0268(10) Uani 1 1 d . . . C6 C 0.5935(7) 1.0536(5) 0.3086(3) 0.0267(10) Uani 1 1 d . . . C7 C 0.5856(9) 1.0015(7) 0.1225(3) 0.0372(12) Uani 1 1 d . . . H7A H 0.589(8) 1.118(7) 0.123(3) 0.035(14) Uiso 1 1 d . . . H7B H 0.587(10) 0.950(8) 0.064(4) 0.07(2) Uiso 1 1 d . . . C8 C 0.3875(9) 0.8980(7) 0.1444(3) 0.0370(12) Uani 1 1 d . . . H8A H 0.256(9) 0.899(8) 0.107(4) 0.060(17) Uiso 1 1 d . . . H8B H 0.396(10) 0.756(9) 0.146(4) 0.08(2) Uiso 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 I1 0.0426(3) 0.0315(2) 0.0273(2) -0.00389(17) 0.0062(2) 0.0081(2) I2 0.0451(2) 0.04314(19) 0.0450(2) -0.00057(15) 0.01359(16) 0.00273(16) Br1 0.0262(3) 0.0477(3) 0.0342(3) 0.0014(2) -0.0056(2) 0.0094(2) Br2 0.0317(3) 0.0434(3) 0.0210(2) -0.00541(19) 0.00195(19) 0.0063(2) S1 0.0277(6) 0.0456(6) 0.0256(6) -0.0022(5) 0.0035(5) 0.0138(5) S2 0.0246(6) 0.0496(7) 0.0192(6) -0.0057(5) 0.0009(5) 0.0087(5) S3 0.0260(6) 0.0460(6) 0.0218(6) -0.0032(5) 0.0017(5) 0.0135(5) S4 0.0261(6) 0.0459(7) 0.0229(6) -0.0050(5) 0.0030(5) 0.0088(5) S5 0.0344(7) 0.0483(7) 0.0224(6) -0.0049(5) 0.0040(5) 0.0158(6) S6 0.0265(6) 0.0537(7) 0.0302(7) -0.0089(6) 0.0003(5) 0.0058(6) C1 0.027(2) 0.030(2) 0.021(2) 0.0004(18) -0.0041(19) 0.009(2) C2 0.030(3) 0.031(2) 0.022(2) 0.0021(18) -0.0009(19) 0.011(2) C3 0.029(3) 0.036(2) 0.023(2) 0.0008(19) 0.0020(19) 0.012(2) C4 0.027(2) 0.032(2) 0.021(2) 0.0005(18) 0.0006(18) 0.006(2) C5 0.029(2) 0.028(2) 0.021(2) -0.0023(17) 0.0008(19) 0.0072(19) C6 0.033(3) 0.025(2) 0.019(2) -0.0013(17) -0.0009(19) 0.009(2) C7 0.051(3) 0.038(3) 0.020(3) -0.002(2) 0.000(2) 0.014(3) C8 0.039(3) 0.041(3) 0.026(3) -0.005(2) -0.003(2) 0.010(3) _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 I1 I2 2.9075(10) 2_665 ? I1 I2 2.9075(10) . ? Br1 C1 1.867(4) . ? Br2 C2 1.872(4) . ? S1 C1 1.743(4) . ? S1 C3 1.749(5) . ? S2 C3 1.739(5) . ? S2 C2 1.744(5) . ? S3 C4 1.733(5) . ? S3 C5 1.757(4) . ? S4 C4 1.733(5) . ? S4 C6 1.748(4) . ? S5 C5 1.742(4) . ? S5 C7 1.806(6) . ? S6 C6 1.739(5) . ? S6 C8 1.804(5) . ? C1 C2 1.325(7) . ? C3 C4 1.366(6) 2_786 ? C4 C3 1.366(6) 2_786 ? C5 C6 1.351(6) . ? C7 C8 1.508(8) . ? 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 I2 I1 I2 180.0 2_665 . ? C1 S1 C3 94.5(2) . . ? C3 S2 C2 95.1(2) . . ? C4 S3 C5 95.5(2) . . ? C4 S4 C6 95.5(2) . . ? C5 S5 C7 98.3(2) . . ? C6 S6 C8 103.4(2) . . ? C2 C1 S1 118.2(3) . . ? C2 C1 Br1 125.2(3) . . ? S1 C1 Br1 116.6(3) . . ? C1 C2 S2 117.2(3) . . ? C1 C2 Br2 125.6(3) . . ? S2 C2 Br2 117.2(3) . . ? C4 C3 S2 122.2(4) 2_786 . ? C4 C3 S1 122.7(4) 2_786 . ? S2 C3 S1 115.1(2) . . ? C3 C4 S4 122.0(4) 2_786 . ? C3 C4 S3 122.6(4) 2_786 . ? S4 C4 S3 115.5(2) . . ? C6 C5 S5 127.5(3) . . ? C6 C5 S3 116.4(3) . . ? S5 C5 S3 116.0(3) . . ? C5 C6 S6 128.9(3) . . ? C5 C6 S4 117.2(3) . . ? S6 C6 S4 113.9(3) . . ? C8 C7 S5 113.7(4) . . ? C7 C8 S6 114.2(3) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.637 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.115 #======END data_tde40absm _database_code_CSD 155960 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(3,4-diiodo-3',4'-ethylenedithiotetrathiafulvalene), triiodide ; _chemical_name_common '2(EDT-TTF-I2), I3' _chemical_melting_point ? _chemical_formula_moiety '2(C8H4S6I2), I3' _chemical_formula_sum 'C16 H8 I7 S12' _chemical_formula_weight 1473.24 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0316(14) _cell_length_b 7.6515(15) _cell_length_c 16.138(3) _cell_angle_alpha 95.20(3) _cell_angle_beta 98.54(3) _cell_angle_gamma 103.49(3) _cell_volume 827.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description 'prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.461 _exptl_crystal_size_mid 0.1156 _exptl_crystal_size_min 0.1156 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 667 _exptl_absorpt_coefficient_mu 7.330 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1391 _exptl_absorpt_correction_T_max 0.4882 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8088 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.87 _reflns_number_total 2975 _reflns_number_gt 2557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0749P)^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 2975 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 I3 I 0.0000 0.0000 1.0000 0.0388(2) Uani 1 2 d S . . I4 I 0.36784(10) 0.23139(9) 0.96792(4) 0.0500(2) Uani 1 1 d . . . I1 I 0.48977(7) -0.00081(7) 0.20453(3) 0.03449(18) Uani 1 1 d . . . I2 I 0.00372(7) 0.01068(8) 0.27368(4) 0.03978(19) Uani 1 1 d . . . S1 S 0.6678(3) 0.1812(3) 0.40158(11) 0.0351(5) Uani 1 1 d . . . S2 S 0.2858(3) 0.1867(3) 0.45329(12) 0.0358(5) Uani 1 1 d . . . S3 S 0.8979(3) 0.3604(3) 0.58916(12) 0.0351(5) Uani 1 1 d . . . S4 S 0.5171(3) 0.3700(3) 0.64110(11) 0.0336(5) Uani 1 1 d . . . S5 S 1.1457(3) 0.5157(3) 0.75424(14) 0.0417(5) Uani 1 1 d . . . S6 S 0.6928(3) 0.5348(3) 0.81816(13) 0.0378(5) Uani 1 1 d . . . C1 C 0.4559(11) 0.1011(10) 0.3244(4) 0.0268(15) Uani 1 1 d . . . C2 C 0.2813(11) 0.1027(11) 0.3482(5) 0.0299(17) Uani 1 1 d . . . C3 C 0.5417(11) 0.2381(12) 0.4822(5) 0.0314(17) Uani 1 1 d . . . C4 C 0.6407(11) 0.3146(11) 0.5612(5) 0.0288(16) Uani 1 1 d . . . C5 C 0.9076(11) 0.4509(10) 0.6940(5) 0.0281(16) Uani 1 1 d . . . C6 C 0.7316(11) 0.4550(10) 0.7176(5) 0.0290(16) Uani 1 1 d . . . C7 C 1.1029(13) 0.5914(12) 0.8563(5) 0.039(2) Uani 1 1 d . . . H7A H 1.2115 0.5795 0.8983 0.047 Uiso 1 1 calc R . . H7B H 1.1062 0.7192 0.8591 0.047 Uiso 1 1 calc R . . C8 C 0.9106(14) 0.4933(14) 0.8799(5) 0.043(2) Uani 1 1 d . . . H8A H 0.9125 0.5302 0.9391 0.052 Uiso 1 1 calc R . . H8B H 0.9010 0.3641 0.8726 0.052 Uiso 1 1 calc R . . 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 I3 0.0522(5) 0.0335(4) 0.0270(4) -0.0046(3) 0.0059(3) 0.0072(3) I4 0.0550(4) 0.0469(4) 0.0430(4) -0.0034(3) 0.0155(3) 0.0017(3) I1 0.0337(3) 0.0426(3) 0.0199(3) -0.0054(2) -0.00096(19) 0.0024(2) I2 0.0302(3) 0.0465(4) 0.0379(3) 0.0028(2) -0.0060(2) 0.0087(2) S1 0.0271(9) 0.0549(14) 0.0192(9) -0.0070(8) -0.0004(7) 0.0093(8) S2 0.0311(10) 0.0525(14) 0.0239(9) -0.0032(9) 0.0019(7) 0.0157(9) S3 0.0312(9) 0.0517(13) 0.0201(9) -0.0042(8) 0.0016(7) 0.0108(8) S4 0.0315(9) 0.0500(13) 0.0184(8) -0.0039(8) -0.0004(7) 0.0145(8) S5 0.0329(10) 0.0455(13) 0.0394(11) -0.0104(9) 0.0046(8) 0.0028(9) S6 0.0373(10) 0.0450(13) 0.0294(10) -0.0035(9) 0.0032(8) 0.0114(9) C1 0.029(4) 0.027(4) 0.022(3) 0.002(3) -0.001(3) 0.007(3) C2 0.030(4) 0.030(4) 0.026(4) 0.002(3) -0.005(3) 0.007(3) C3 0.033(4) 0.045(5) 0.017(3) -0.002(3) 0.001(3) 0.015(3) C4 0.036(4) 0.031(4) 0.020(3) -0.002(3) 0.002(3) 0.013(3) C5 0.035(4) 0.026(4) 0.021(3) 0.001(3) 0.001(3) 0.006(3) C6 0.035(4) 0.025(4) 0.024(4) -0.001(3) -0.002(3) 0.007(3) C7 0.046(5) 0.040(5) 0.022(4) -0.003(3) -0.009(3) 0.007(4) C8 0.054(5) 0.052(6) 0.022(4) 0.003(4) 0.006(4) 0.012(4) _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 I3 I4 2.9188(11) 2_557 ? I3 I4 2.9188(11) . ? I1 C1 2.087(7) . ? I2 C2 2.063(7) . ? S1 C1 1.742(7) . ? S1 C3 1.757(8) . ? S2 C3 1.731(8) . ? S2 C2 1.752(8) . ? S3 C4 1.741(8) . ? S3 C5 1.755(7) . ? S4 C4 1.734(7) . ? S4 C6 1.750(7) . ? S5 C5 1.742(8) . ? S5 C7 1.787(8) . ? S6 C6 1.764(8) . ? S6 C8 1.808(10) . ? C1 C2 1.342(11) . ? C3 C4 1.365(10) . ? C5 C6 1.353(11) . ? C7 C8 1.506(12) . ? 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 I4 I3 I4 180.00(2) 2_557 . ? C1 S1 C3 95.6(4) . . ? C3 S2 C2 95.4(3) . . ? C4 S3 C5 95.5(4) . . ? C4 S4 C6 95.4(4) . . ? C5 S5 C7 103.0(4) . . ? C6 S6 C8 97.7(4) . . ? C2 C1 S1 116.8(6) . . ? C2 C1 I1 125.0(5) . . ? S1 C1 I1 118.2(4) . . ? C1 C2 S2 117.6(5) . . ? C1 C2 I2 126.5(6) . . ? S2 C2 I2 115.9(4) . . ? C4 C3 S2 123.6(6) . . ? C4 C3 S1 121.7(6) . . ? S2 C3 S1 114.7(4) . . ? C3 C4 S4 121.9(6) . . ? C3 C4 S3 122.7(6) . . ? S4 C4 S3 115.4(4) . . ? C6 C5 S5 129.3(6) . . ? C6 C5 S3 116.4(6) . . ? S5 C5 S3 114.2(4) . . ? C5 C6 S4 117.3(6) . . ? C5 C6 S6 127.1(6) . . ? S4 C6 S6 115.7(4) . . ? C8 C7 S5 115.7(6) . . ? C7 C8 S6 113.7(6) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 2.205 _refine_diff_density_min -1.667 _refine_diff_density_rms 0.280