# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2003 data_tde242absm _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(3,4-diiodo-3',4'-ethylenedithiotetrathiafulvalene), triiodolead(II), water ; _chemical_name_common '(EDT-TTF-I2)2, PbI3, H20' _chemical_melting_point ? _chemical_formula_moiety '2(C8H4S6I2), PbI3,H2O' _chemical_formula_sum 'C8 H4 I3.50 O0.50 Pb0.50 S6' _chemical_formula_weight 848.22 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' 'Pb' 'Pb' -3.3944 10.1111 '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' _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 8.0312(16) _cell_length_b 12.130(2) _cell_length_c 20.777(4) _cell_angle_alpha 102.29(3) _cell_angle_beta 99.88(3) _cell_angle_gamma 100.13(3) _cell_volume 1900.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'needle' _exptl_crystal_colour black _exptl_crystal_size_max 0.308 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_absorpt_coefficient_mu 10.800 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3817 _exptl_absorpt_correction_T_max 0.6805 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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. 1.1' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19480 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.88 _reflns_number_total 6881 _reflns_number_gt 5135 _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^)+(0.0382P)^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 6881 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 Pb1 Pb 0.0000 0.5000 0.0000 0.02569(12) Uani 1 2 d S . . Pb2 Pb -0.5000 0.5000 0.0000 0.02475(12) Uani 1 2 d S . . I1 I -0.18543(8) 0.71724(4) 0.02536(3) 0.03062(15) Uani 1 1 d . . . I2 I -0.23129(9) 0.40106(5) 0.09513(3) 0.03354(16) Uani 1 1 d . . . I3 I 0.33501(9) 0.62885(5) 0.11854(3) 0.03499(16) Uani 1 1 d . . . I4 I 0.43865(8) 1.08022(5) -0.22755(3) 0.02666(14) Uani 1 1 d . . . I5 I 0.21995(9) 0.77806(5) -0.21131(3) 0.03023(15) Uani 1 1 d . . . S1 S 0.2462(3) 0.96531(17) -0.38555(10) 0.0270(5) Uani 1 1 d . . . S2 S 0.0807(3) 0.73889(18) -0.37009(10) 0.0316(6) Uani 1 1 d . . . C1 C 0.2824(11) 0.9428(7) -0.3037(4) 0.0213(18) Uani 1 1 d . . . C2 C 0.2069(12) 0.8404(7) -0.2973(4) 0.025(2) Uani 1 1 d . . . C3 C 0.1132(12) 0.8284(6) -0.4247(4) 0.025(2) Uani 1 1 d . . . S3 S 0.0622(3) 0.87741(17) -0.54834(10) 0.0292(5) Uani 1 1 d . . . S4 S -0.0882(3) 0.65160(17) -0.52716(10) 0.0304(6) Uani 1 1 d . . . S5 S -0.0616(3) 0.81189(18) -0.69530(10) 0.0300(5) Uani 1 1 d . . . S6 S -0.2236(4) 0.53824(18) -0.67197(11) 0.0350(6) Uani 1 1 d . . . C4 C 0.0391(12) 0.7916(7) -0.4921(4) 0.025(2) Uani 1 1 d . . . C5 C -0.0498(12) 0.7678(7) -0.6201(4) 0.024(2) Uani 1 1 d . . . C6 C -0.1156(12) 0.6644(7) -0.6101(4) 0.0232(19) Uani 1 1 d . . . C7 C -0.1606(13) 0.6782(7) -0.7592(4) 0.032(2) Uani 1 1 d . . . H7A H -0.2089 0.6967 -0.8007 0.038 Uiso 1 1 calc R . . H7B H -0.0715 0.6361 -0.7682 0.038 Uiso 1 1 calc R . . C8 C -0.3015(12) 0.6012(8) -0.7396(4) 0.031(2) Uani 1 1 d . . . H8A H -0.3624 0.5394 -0.7788 0.037 Uiso 1 1 calc R . . H8B H -0.3841 0.6459 -0.7259 0.037 Uiso 1 1 calc R . . I40 I -0.04823(8) 1.05405(5) -0.16903(3) 0.02799(14) Uani 1 1 d . . . I50 I -0.25688(9) 0.76211(5) -0.14541(3) 0.03113(15) Uani 1 1 d . . . S10 S -0.2472(3) 0.93422(17) -0.32647(10) 0.0289(5) Uani 1 1 d . . . S20 S -0.4172(3) 0.71277(17) -0.30548(10) 0.0294(5) Uani 1 1 d . . . S30 S -0.4277(4) 0.84405(18) -0.48626(10) 0.0341(6) Uani 1 1 d . . . S40 S -0.5954(3) 0.62300(18) -0.46413(10) 0.0326(6) Uani 1 1 d . . . S50 S -0.5471(4) 0.7764(2) -0.63370(11) 0.0381(6) Uani 1 1 d . . . S60 S -0.7564(3) 0.51281(18) -0.60675(10) 0.0290(5) Uani 1 1 d . . . C10 C -0.2045(12) 0.9148(7) -0.2444(4) 0.025(2) Uani 1 1 d . . . C20 C -0.2814(12) 0.8136(7) -0.2359(4) 0.0226(19) Uani 1 1 d . . . C30 C -0.3829(12) 0.7967(7) -0.3627(4) 0.0251(19) Uani 1 1 d . . . C40 C -0.4569(13) 0.7594(7) -0.4291(4) 0.027(2) Uani 1 1 d . . . C50 C -0.5467(12) 0.7355(7) -0.5575(4) 0.025(2) Uani 1 1 d . . . C60 C -0.6240(12) 0.6351(7) -0.5478(4) 0.0231(19) Uani 1 1 d . . . C70 C -0.7240(14) 0.6646(8) -0.6887(4) 0.035(2) Uani 1 1 d . . . H70A H -0.8320 0.6796 -0.6779 0.042 Uiso 1 1 calc R . . H70B H -0.7267 0.6690 -0.7349 0.042 Uiso 1 1 calc R . . C80 C -0.7136(14) 0.5438(8) -0.6840(4) 0.035(2) Uani 1 1 d . . . H80A H -0.5988 0.5325 -0.6880 0.042 Uiso 1 1 calc R . . H80B H -0.7963 0.4890 -0.7217 0.042 Uiso 1 1 calc R . . O1 O 0.744(4) 0.0677(16) -0.0048(10) 0.300(17) 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 Pb1 0.0219(3) 0.0367(3) 0.0177(2) 0.00555(18) 0.00170(18) 0.0083(2) Pb2 0.0220(3) 0.0292(2) 0.0221(2) 0.00595(18) 0.00359(19) 0.00491(19) I1 0.0330(4) 0.0269(3) 0.0271(3) 0.0055(2) 0.0006(2) 0.0010(2) I2 0.0421(4) 0.0423(3) 0.0238(3) 0.0176(2) 0.0114(3) 0.0137(3) I3 0.0288(4) 0.0501(4) 0.0163(3) -0.0043(2) -0.0023(2) 0.0058(3) I4 0.0254(4) 0.0338(3) 0.0156(2) 0.0017(2) -0.0033(2) 0.0060(2) I5 0.0365(4) 0.0409(3) 0.0184(3) 0.0143(2) 0.0063(2) 0.0134(3) S1 0.0402(16) 0.0228(10) 0.0132(9) 0.0037(7) -0.0014(9) 0.0025(9) S2 0.0453(17) 0.0245(10) 0.0193(10) 0.0066(8) -0.0020(10) -0.0001(10) C1 0.017(5) 0.037(5) 0.011(4) 0.005(3) 0.000(3) 0.011(4) C2 0.030(6) 0.037(5) 0.008(3) 0.009(3) -0.001(3) 0.012(4) C3 0.039(6) 0.018(4) 0.013(4) 0.001(3) -0.003(4) 0.003(4) S3 0.0461(16) 0.0210(10) 0.0130(9) 0.0013(7) -0.0036(9) 0.0013(9) S4 0.0425(16) 0.0262(11) 0.0157(10) 0.0035(8) -0.0002(9) -0.0018(9) S5 0.0428(17) 0.0288(11) 0.0143(9) 0.0033(8) -0.0032(9) 0.0089(10) S6 0.0435(17) 0.0244(11) 0.0247(11) -0.0024(8) -0.0108(10) 0.0031(10) C4 0.029(6) 0.024(4) 0.020(4) 0.006(3) -0.001(4) 0.003(3) C5 0.024(6) 0.025(4) 0.020(4) 0.000(3) 0.000(4) 0.005(4) C6 0.022(6) 0.027(4) 0.015(4) -0.003(3) -0.003(3) 0.007(3) C7 0.031(6) 0.036(5) 0.015(4) -0.006(3) -0.010(4) 0.003(4) C8 0.021(6) 0.040(5) 0.022(4) -0.004(4) -0.008(4) 0.007(4) I40 0.0291(4) 0.0317(3) 0.0166(3) 0.0022(2) -0.0012(2) 0.0003(2) I50 0.0331(4) 0.0402(3) 0.0212(3) 0.0133(2) 0.0026(2) 0.0074(3) S10 0.0398(16) 0.0253(10) 0.0153(10) 0.0018(8) 0.0012(9) -0.0003(9) S20 0.0390(16) 0.0245(10) 0.0194(10) 0.0032(8) 0.0024(9) 0.0001(9) S30 0.0518(18) 0.0266(11) 0.0169(10) 0.0040(8) 0.0013(10) -0.0019(10) S40 0.0430(17) 0.0291(11) 0.0169(10) 0.0040(8) -0.0013(10) -0.0053(10) S50 0.0539(19) 0.0366(12) 0.0183(10) 0.0081(9) 0.0051(10) -0.0031(11) S60 0.0297(15) 0.0292(11) 0.0202(10) 0.0006(8) 0.0002(9) -0.0024(9) C10 0.025(6) 0.034(5) 0.014(4) -0.002(3) 0.002(3) 0.012(4) C20 0.026(6) 0.026(4) 0.012(4) 0.003(3) 0.000(3) 0.002(3) C30 0.021(6) 0.032(4) 0.019(4) 0.005(3) 0.000(4) 0.003(4) C40 0.030(6) 0.031(4) 0.022(4) 0.007(3) 0.008(4) 0.012(4) C50 0.026(6) 0.035(5) 0.012(4) 0.001(3) 0.001(3) 0.013(4) C60 0.022(6) 0.026(4) 0.020(4) 0.003(3) 0.002(3) 0.007(3) C70 0.046(7) 0.043(5) 0.015(4) 0.004(4) 0.006(4) 0.015(4) C80 0.033(7) 0.048(6) 0.022(4) 0.004(4) 0.001(4) 0.011(4) O1 0.53(5) 0.147(15) 0.133(15) -0.079(12) 0.12(2) -0.06(2) _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 Pb1 I2 3.2069(11) . ? Pb1 I2 3.2069(11) 2_565 ? Pb1 I3 3.2180(16) . ? Pb1 I3 3.2180(16) 2_565 ? Pb1 I1 3.2401(10) 2_565 ? Pb1 I1 3.2401(10) . ? Pb2 I1 3.1960(13) 2_465 ? Pb2 I1 3.1960(13) . ? Pb2 I2 3.2344(11) . ? Pb2 I2 3.2344(11) 2_465 ? Pb2 I3 3.2366(11) 1_455 ? Pb2 I3 3.2366(11) 2_565 ? I3 Pb2 3.2366(11) 1_655 ? I4 C1 2.078(8) . ? I5 C2 2.078(7) . ? S1 C3 1.750(8) . ? S1 C1 1.762(8) . ? S2 C3 1.750(8) . ? S2 C2 1.753(8) . ? C1 C2 1.327(12) . ? C3 C4 1.366(11) . ? S3 C4 1.735(8) . ? S3 C5 1.753(8) . ? S4 C6 1.744(8) . ? S4 C4 1.752(8) . ? S5 C5 1.749(8) . ? S5 C7 1.815(8) . ? S6 C6 1.749(8) . ? S6 C8 1.809(9) . ? C5 C6 1.345(12) . ? C7 C8 1.506(14) . ? I40 C10 2.082(8) . ? I50 C20 2.093(8) . ? S10 C10 1.755(8) . ? S10 C30 1.756(8) . ? S20 C20 1.736(8) . ? S20 C30 1.747(9) . ? S30 C40 1.746(9) . ? S30 C50 1.755(8) . ? S40 C40 1.751(9) . ? S40 C60 1.754(8) . ? S50 C50 1.756(8) . ? S50 C70 1.808(10) . ? S60 C60 1.748(8) . ? S60 C80 1.799(9) . ? C10 C20 1.336(12) . ? C30 C40 1.350(11) . ? C50 C60 1.339(12) . ? C70 C80 1.505(13) . ? 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 Pb1 I2 180.00(2) . 2_565 ? I2 Pb1 I3 96.02(3) . . ? I2 Pb1 I3 83.98(3) 2_565 . ? I2 Pb1 I3 83.98(3) . 2_565 ? I2 Pb1 I3 96.02(3) 2_565 2_565 ? I3 Pb1 I3 180.0 . 2_565 ? I2 Pb1 I1 94.92(3) . 2_565 ? I2 Pb1 I1 85.08(3) 2_565 2_565 ? I3 Pb1 I1 86.71(3) . 2_565 ? I3 Pb1 I1 93.29(3) 2_565 2_565 ? I2 Pb1 I1 85.08(3) . . ? I2 Pb1 I1 94.92(3) 2_565 . ? I3 Pb1 I1 93.29(3) . . ? I3 Pb1 I1 86.71(3) 2_565 . ? I1 Pb1 I1 180.0 2_565 . ? I1 Pb2 I1 180.000(15) 2_465 . ? I1 Pb2 I2 94.65(3) 2_465 . ? I1 Pb2 I2 85.35(3) . . ? I1 Pb2 I2 85.35(3) 2_465 2_465 ? I1 Pb2 I2 94.65(3) . 2_465 ? I2 Pb2 I2 180.0 . 2_465 ? I1 Pb2 I3 87.14(3) 2_465 1_455 ? I1 Pb2 I3 92.86(3) . 1_455 ? I2 Pb2 I3 96.75(3) . 1_455 ? I2 Pb2 I3 83.25(3) 2_465 1_455 ? I1 Pb2 I3 92.86(3) 2_465 2_565 ? I1 Pb2 I3 87.14(3) . 2_565 ? I2 Pb2 I3 83.25(3) . 2_565 ? I2 Pb2 I3 96.75(3) 2_465 2_565 ? I3 Pb2 I3 180.000(14) 1_455 2_565 ? Pb2 I1 Pb1 77.20(2) . . ? Pb1 I2 Pb2 77.13(2) . . ? Pb1 I3 Pb2 76.94(3) . 1_655 ? C3 S1 C1 95.6(4) . . ? C3 S2 C2 95.4(4) . . ? C2 C1 S1 116.7(6) . . ? C2 C1 I4 127.0(6) . . ? S1 C1 I4 116.2(4) . . ? C1 C2 S2 118.0(6) . . ? C1 C2 I5 129.0(6) . . ? S2 C2 I5 113.0(4) . . ? C4 C3 S2 121.4(6) . . ? C4 C3 S1 124.3(6) . . ? S2 C3 S1 114.3(4) . . ? C4 S3 C5 95.0(4) . . ? C6 S4 C4 94.7(4) . . ? C5 S5 C7 102.9(4) . . ? C6 S6 C8 99.6(4) . . ? C3 C4 S3 123.5(6) . . ? C3 C4 S4 121.0(6) . . ? S3 C4 S4 115.4(4) . . ? C6 C5 S5 129.4(6) . . ? C6 C5 S3 117.0(6) . . ? S5 C5 S3 113.6(5) . . ? C5 C6 S4 117.5(6) . . ? C5 C6 S6 127.1(6) . . ? S4 C6 S6 115.4(5) . . ? C8 C7 S5 113.6(6) . . ? C7 C8 S6 113.9(6) . . ? C10 S10 C30 95.2(4) . . ? C20 S20 C30 95.2(4) . . ? C40 S30 C50 95.0(4) . . ? C40 S40 C60 95.4(4) . . ? C50 S50 C70 99.8(4) . . ? C60 S60 C80 100.5(4) . . ? C20 C10 S10 116.7(6) . . ? C20 C10 I40 126.2(6) . . ? S10 C10 I40 117.0(5) . . ? C10 C20 S20 118.3(6) . . ? C10 C20 I50 126.5(6) . . ? S20 C20 I50 115.2(4) . . ? C40 C30 S20 122.7(7) . . ? C40 C30 S10 122.7(7) . . ? S20 C30 S10 114.6(4) . . ? C30 C40 S30 123.0(7) . . ? C30 C40 S40 122.1(7) . . ? S30 C40 S40 114.8(5) . . ? C60 C50 S30 117.8(6) . . ? C60 C50 S50 128.7(6) . . ? S30 C50 S50 113.5(5) . . ? C50 C60 S60 129.3(6) . . ? C50 C60 S40 116.7(6) . . ? S60 C60 S40 114.0(5) . . ? C80 C70 S50 114.4(7) . . ? C70 C80 S60 113.6(6) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.88 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 2.591 _refine_diff_density_min -2.101 _refine_diff_density_rms 0.259