# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/222 data_DSEDS-TaF6#2 #------------------------------------------------------------------------------ _audit_creation_date 'Tue May 11 10:46:53 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 691.97 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H6 F2 S4 Se4 Ta0.33 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 6.438(1) _cell_length_b 19.151(2) _cell_length_c 3.930(1) _cell_angle_alpha 92.69(2) _cell_angle_beta 95.76(2) _cell_angle_gamma 93.70(1) _cell_volume 480.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.4 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.392 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 320.09 _exptl_absorpt_coefficient_mu 9.947 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.534 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.61 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -1 -1 -2 0 -2 3 0 _diffrn_reflns_number 3035 _reflns_number_total 2803 _reflns_number_observed 1825 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.14388 _diffrn_orient_matrix_UB_12 0.01554 _diffrn_orient_matrix_UB_13 -0.05962 _diffrn_orient_matrix_UB_21 0.04884 _diffrn_orient_matrix_UB_22 0.04873 _diffrn_orient_matrix_UB_23 0.08834 _diffrn_orient_matrix_UB_31 0.03751 _diffrn_orient_matrix_UB_32 0.01141 _diffrn_orient_matrix_UB_33 -0.23288 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 12 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 2 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 6 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 4 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 4 -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ta 0 0 -0.705 6.523 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Ta1 0.2588 0.3853 0.9175 0.0601(6) Uani d . 0.33 S Se1 0.0805(7) -0.4013(3) -1.331(2) 0.0376(7) Uani d . 1.00 . Se2 -0.3769(7) -0.3448(2) -1.400(2) 0.0396(8) Uani d . 1.00 . Se3 0.8915(7) 0.1117(3) 0.213(2) 0.0360(7) Uani d . 1.00 . Se4 0.4394(7) 0.1675(3) 0.157(2) 0.0415(8) Uani d . 1.00 . S1 0.2522(10) -0.2491(4) -0.922(2) 0.030(1) Uani d . 1.00 . S2 -0.1799(8) -0.1992(3) -0.976(2) 0.033(1) Uani d . 1.00 . S3 0.4168(8) -0.1089(3) -0.541(2) 0.032(1) Uani d . 1.00 . S4 -0.0127(8) -0.0607(3) -0.599(2) 0.033(1) Uani d . 1.00 . F1 0.271(7) 0.449(3) 0.61(1) 0.10(1) Uiso d . 0.33 . F2 0.236(10) 0.333(3) 0.55(2) 0.14(2) Uiso d . 0.33 . F3 0.539(9) 0.394(3) 1.01(1) 0.13(2) Uiso d . 0.33 . F4 0.267(8) 0.320(3) 1.29(1) 0.09(1) Uiso d . 0.33 . F5 0.241(5) 0.456(2) 1.253(8) 0.047(7) Uiso d . 0.33 . F6 -0.036(4) 0.373(1) 0.887(7) 0.038(7) Uiso d . 0.33 . C1 -0.134(3) -0.461(1) -1.536(7) 0.044(6) Uani d . 1.00 . C2 -0.323(3) -0.441(1) -1.570(7) 0.046(6) Uani d . 1.00 . C3 -0.078(3) -0.322(1) -1.226(6) 0.027(5) Uani d . 1.00 . C4 -0.012(3) -0.268(1) -1.069(5) 0.023(5) Uani d . 1.00 . C5 0.215(3) -0.1662(9) -0.741(4) 0.026(4) Uani d . 1.00 . C6 0.020(2) -0.1442(7) -0.765(4) 0.024(4) Uani d . 1.00 . C7 0.256(2) -0.0420(8) -0.436(5) 0.028(4) Uani d . 1.00 . C8 0.321(3) 0.014(1) -0.261(7) 0.039(6) Uani d . 1.00 . C9 0.537(3) 0.031(1) -0.136(6) 0.030(6) Uani d . 1.00 . C10 0.617(3) 0.098(1) 0.055(6) 0.034(5) Uani d . 1.00 . C11 0.867(4) 0.196(1) 0.406(7) 0.050(6) Uani d . 1.00 . C12 0.688(4) 0.222(1) 0.375(7) 0.050(7) Uani d . 1.00 . H1 -0.1120 -0.5080 -1.6355 0.0605 Uiso calc . 1.00 . H2 -0.4382 -0.4706 -1.6943 0.0552 Uiso calc . 1.00 . H3 0.2229 0.0497 -0.2048 0.0347 Uiso calc . 1.00 . H4 0.6356 -0.0042 -0.1787 0.0419 Uiso calc . 1.00 . H5 0.9851 0.2243 0.5009 0.0646 Uiso calc . 1.00 . H6 0.6672 0.2684 0.4618 0.0505 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta(1) 0.0325(9) 0.0320(9) 0.114(2) 0.0037(7) -0.0011(10) -0.0004(10) Se(1) 0.030(1) 0.033(1) 0.051(2) 0.0057(9) 0.004(1) -0.002(1) Se(2) 0.024(1) 0.044(2) 0.048(2) 0.002(1) -0.006(1) -0.005(1) Se(3) 0.025(1) 0.041(2) 0.040(2) -0.0046(10) 0.000(1) -0.005(1) Se(4) 0.035(1) 0.038(1) 0.050(2) 0.005(1) 0.002(1) -0.009(1) S(1) 0.018(2) 0.029(2) 0.041(3) 0.004(2) -0.003(2) -0.004(2) S(2) 0.017(2) 0.029(2) 0.051(3) 0.002(1) -0.004(2) -0.005(2) S(3) 0.015(2) 0.035(2) 0.045(3) 0.000(2) -0.003(2) -0.005(2) S(4) 0.022(2) 0.031(2) 0.046(3) 0.004(1) -0.002(2) -0.007(2) C(1) 0.026(9) 0.03(1) 0.07(2) 0.009(7) 0.005(9) -0.01(1) C(2) 0.03(1) 0.04(1) 0.07(2) -0.004(9) 0.00(1) 0.002(10) C(3) 0.022(9) 0.024(9) 0.04(1) 0.011(7) 0.006(8) 0.000(8) C(4) 0.04(1) 0.019(10) 0.013(9) -0.001(8) -0.001(8) 0.000(7) C(5) 0.022(8) 0.034(9) 0.022(7) 0.006(6) 0.005(6) -0.012(7) C(6) 0.013(6) 0.019(7) 0.038(9) -0.005(5) -0.002(6) 0.005(6) C(7) 0.016(7) 0.024(9) 0.046(10) -0.003(6) 0.016(7) -0.006(7) C(8) 0.006(7) 0.05(1) 0.06(1) 0.009(7) 0.005(7) -0.013(10) C(9) 0.019(10) 0.03(1) 0.04(1) 0.000(8) 0.000(9) -0.010(9) C(10) 0.026(9) 0.04(1) 0.03(1) -0.020(8) -0.014(8) 0.000(9) C(11) 0.05(1) 0.03(1) 0.07(2) 0.000(8) -0.02(1) -0.022(10) C(12) 0.06(2) 0.02(1) 0.07(2) -0.012(9) -0.01(1) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1825 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0434 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0474 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.364 _refine_ls_shift/esd_max 0.0920 _refine_ls_shift/esd_mean 0.0040 _refine_diff_density_min -1.01 _refine_diff_density_max 0.85 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta(1) F(1) 1.76(5) 1_555 1_555 yes Ta(1) F(2) 1.69(7) 1_555 1_555 yes Ta(1) F(3) 1.80(6) 1_555 1_555 yes Ta(1) F(4) 1.95(5) 1_555 1_555 yes Ta(1) F(5) 1.86(3) 1_555 1_555 yes Ta(1) F(6) 1.89(3) 1_555 1_555 yes Se(1) C(1) 1.84(2) 1_555 1_555 yes Se(1) C(3) 1.94(2) 1_555 1_555 yes Se(2) C(2) 2.00(3) 1_555 1_555 yes Se(2) C(3) 1.99(2) 1_555 1_555 yes Se(3) C(10) 1.81(2) 1_555 1_555 yes Se(3) C(11) 1.77(2) 1_555 1_555 yes Se(4) C(10) 1.86(3) 1_555 1_555 yes Se(4) C(12) 1.95(2) 1_555 1_555 yes S(1) C(4) 1.75(2) 1_555 1_555 yes S(1) C(5) 1.75(2) 1_555 1_555 yes S(2) C(4) 1.80(2) 1_555 1_555 yes S(2) C(6) 1.73(1) 1_555 1_555 yes S(3) C(5) 1.74(2) 1_555 1_555 yes S(3) C(7) 1.76(2) 1_555 1_555 yes S(4) C(6) 1.73(1) 1_555 1_555 yes S(4) C(7) 1.79(2) 1_555 1_555 yes F(1) F(5) 1.41(5) 1_555 1_554 yes F(2) F(4) 1.12(7) 1_555 1_554 yes C(1) C(2) 1.29(3) 1_555 1_555 yes C(3) C(4) 1.21(2) 1_555 1_555 yes C(5) C(6) 1.35(2) 1_555 1_555 yes C(7) C(8) 1.27(3) 1_555 1_555 yes C(8) C(9) 1.44(2) 1_555 1_555 yes C(9) C(10) 1.49(3) 1_555 1_555 yes C(11) C(12) 1.28(3) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) Ta(1) F(2) 79(2) 1_555 1_555 1_555 yes F(1) Ta(1) F(3) 90(2) 1_555 1_555 1_555 yes F(1) Ta(1) F(4) 174(2) 1_555 1_555 1_555 yes F(1) Ta(1) F(5) 89(1) 1_555 1_555 1_555 yes F(1) Ta(1) F(6) 96(1) 1_555 1_555 1_555 yes F(2) Ta(1) F(3) 100(2) 1_555 1_555 1_555 yes F(2) Ta(1) F(4) 104(2) 1_555 1_555 1_555 yes F(2) Ta(1) F(5) 166(2) 1_555 1_555 1_555 yes F(2) Ta(1) F(6) 85(2) 1_555 1_555 1_555 yes F(3) Ta(1) F(4) 85(2) 1_555 1_555 1_555 yes F(3) Ta(1) F(5) 88(2) 1_555 1_555 1_555 yes F(3) Ta(1) F(6) 171(2) 1_555 1_555 1_555 yes F(4) Ta(1) F(5) 86(1) 1_555 1_555 1_555 yes F(4) Ta(1) F(6) 87(1) 1_555 1_555 1_555 yes F(5) Ta(1) F(6) 87(1) 1_555 1_555 1_555 yes C(1) Se(1) C(3) 99.1(9) 1_555 1_555 1_555 yes C(2) Se(2) C(3) 93.1(8) 1_555 1_555 1_555 yes C(10) Se(3) C(11) 94.2(10) 1_555 1_555 1_555 yes C(10) Se(4) C(12) 86.6(9) 1_555 1_555 1_555 yes C(4) S(1) C(5) 94.6(8) 1_555 1_555 1_555 yes C(4) S(2) C(6) 94.2(8) 1_555 1_555 1_555 yes C(5) S(3) C(7) 95.8(8) 1_555 1_555 1_555 yes C(6) S(4) C(7) 95.4(7) 1_555 1_555 1_555 yes Ta(1) F(1) F(5) 141(3) 1_555 1_555 1_554 yes Ta(1) F(2) F(4) 153(6) 1_555 1_555 1_554 yes Ta(1) F(4) F(2) 125(5) 1_555 1_555 1_556 yes Ta(1) F(5) F(1) 125(2) 1_555 1_555 1_556 yes Se(1) C(1) C(2) 119(1) 1_555 1_555 1_555 yes Se(1) C(1) H(1) 122(1) 1_555 1_555 1_555 no C(2) C(1) H(1) 117(2) 1_555 1_555 1_555 no Se(2) C(2) C(1) 119(1) 1_555 1_555 1_555 yes Se(2) C(2) H(2) 118(1) 1_555 1_555 1_555 no C(1) C(2) H(2) 121(2) 1_555 1_555 1_555 no Se(1) C(3) Se(2) 108.6(10) 1_555 1_555 1_555 yes Se(1) C(3) C(4) 126(1) 1_555 1_555 1_555 yes Se(2) C(3) C(4) 124(1) 1_555 1_555 1_555 yes S(1) C(4) S(2) 114(1) 1_555 1_555 1_555 yes S(1) C(4) C(3) 123(1) 1_555 1_555 1_555 yes S(2) C(4) C(3) 121(1) 1_555 1_555 1_555 yes S(1) C(5) S(3) 124.1(9) 1_555 1_555 1_555 yes S(1) C(5) C(6) 118(1) 1_555 1_555 1_555 yes S(3) C(5) C(6) 117(1) 1_555 1_555 1_555 yes S(2) C(6) S(4) 124.0(8) 1_555 1_555 1_555 yes S(2) C(6) C(5) 118(1) 1_555 1_555 1_555 yes S(4) C(6) C(5) 117(1) 1_555 1_555 1_555 yes S(3) C(7) S(4) 113.2(9) 1_555 1_555 1_555 yes S(3) C(7) C(8) 123(1) 1_555 1_555 1_555 yes S(4) C(7) C(8) 122(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 124(1) 1_555 1_555 1_555 yes C(7) C(8) H(3) 120(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 115(2) 1_555 1_555 1_555 no C(8) C(9) C(10) 124(1) 1_555 1_555 1_555 yes C(8) C(9) H(4) 116(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 118(1) 1_555 1_555 1_555 no Se(3) C(10) Se(4) 118(1) 1_555 1_555 1_555 yes Se(3) C(10) C(9) 119(1) 1_555 1_555 1_555 yes Se(4) C(10) C(9) 121(1) 1_555 1_555 1_555 yes Se(3) C(11) C(12) 119(1) 1_555 1_555 1_555 yes Se(3) C(11) H(5) 121(2) 1_555 1_555 1_555 no C(12) C(11) H(5) 118(2) 1_555 1_555 1_555 no Se(4) C(12) C(11) 121(1) 1_555 1_555 1_555 yes Se(4) C(12) H(6) 115(1) 1_555 1_555 1_555 no C(11) C(12) H(6) 122(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ta(1) F(2) 2.75(7) 1_555 1_556 ? Ta(1) F(1) 2.92(5) 1_555 1_556 ? Se(1) F(1) 3.20(5) 1_555 1_543 ? Se(1) F(5) 3.39(3) 1_555 1_542 ? Se(3) S(4) 3.497(4) 1_555 1_656 ? Se(4) F(4) 3.23(5) 1_555 1_554 ? F(1) C(1) 3.23(5) 1_555 1_567 ? F(1) C(2) 3.40(5) 1_555 1_667 ? F(2) C(11) 3.42(6) 1_555 1_455 ? F(3) F(6) 2.88(5) 1_555 1_655 ? F(3) C(2) 3.50(6) 1_555 1_668 ? F(4) F(6) 3.37(6) 1_555 1_556 ? F(4) C(12) 3.40(6) 1_555 1_556 ? F(4) C(11) 3.48(5) 1_555 1_456 ? F(5) C(1) 3.13(4) 1_555 1_568 ? F(5) C(2) 3.31(4) 1_555 1_668 ? F(5) F(6) 3.58(4) 1_555 1_556 ? C(3) C(4) 3.58(3) 1_555 1_554 ? C(7) C(8) 3.52(3) 1_555 1_554 ? C(9) C(10) 3.56(3) 1_555 1_554 ? #------------------------------------------------------------------------------ _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author ; Misaki Yohji Department of Molecular Engineering, Graduate School of Engineering, Kyoto University, Yoshida, Kyoto 606-8501, Japan ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-75-753-5933' _publ_contact_author_fax '+81-75-771-0172' _publ_contact_author_email 'misaki@mee3.moleng.kyoto-u.ac.jp' loop_ _publ_author_name _publ_author_address 'Hideki Fujiwara' ; Department of Molecular Engineering, Graduate School of Engineering, Kyoto University, Yoshida, Kyoto 606-8501, Japan ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;