# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ogawa, Satoshi' 'Kawai, Yasushi' 'Mikata, Yuji' 'Nagahora, Noriyoshi' 'Sato, Ryu' 'Yoshimura, Satoko' _publ_contact_author_name 'Prof Satoshi Ogawa' _publ_contact_author_address ; Chemical Engineering Faculty of Engineering, Iwate University 4-3-5 Ueda Morioka, Iwate 020-8551 JAPAN ; _publ_contact_author_email 'OGAWA@IWATE-U.AC.JP' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Novel multi-chalcogen ring systems with different chalcogen-chalcogen bonding: synthesis, structure, and redox property of five-membered trichalcogenaheterocycles ; #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_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. ; data_SeTiS _database_code_CSD 187544 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 7 11:10:53 2002' _audit_creation_method 'from TEXRAY.INF file' #------------------------------------------------------------------------------ _chemical_formula_weight 577.58 _chemical_formula_sum 'C30 H42 O S Se Ti ' _chemical_formula_moiety 'C30 H42 O S Se Ti ' _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.109(4) _cell_length_b 14.855(4) _cell_length_c 18.680(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2805(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 26.1 _cell_measurement_theta_max 38.1 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1208.00 _exptl_absorpt_coefficient_mu 4.904 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.639 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator filter _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_% 4.66 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5630 _reflns_number_total 2852 _reflns_number_observed 1834 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.107 _diffrn_reflns_av_sigmaI/netI 0.082 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 70.20 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01250 _diffrn_orient_matrix_UB_12 0.01542 _diffrn_orient_matrix_UB_13 0.05165 _diffrn_orient_matrix_UB_21 -0.06859 _diffrn_orient_matrix_UB_22 0.04547 _diffrn_orient_matrix_UB_23 -0.01356 _diffrn_orient_matrix_UB_31 -0.07018 _diffrn_orient_matrix_UB_32 -0.04718 _diffrn_orient_matrix_UB_33 0.00381 #------------------------------------------------------------------------------ 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 0 120 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 168 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.333 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 4 -0.794 1.137 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ti 0 4 0.219 1.807 ;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 Se(3) 0.4361(1) -0.04299(9) 0.62614(7) 0.0503(3) Uani d . 1.00 . Ti(2) 0.2985(2) -0.0139(1) 0.51388(10) 0.0370(4) Uani d . 1.00 . S(1) 0.1925(3) 0.0946(2) 0.5923(1) 0.0451(7) Uani d . 1.00 . O(10) 0.645(1) 0.0547(8) 0.7098(5) 0.069(3) Uani d . 1.00 . C(4) 0.541(1) 0.1107(10) 0.6996(6) 0.053(3) Uani d . 1.00 . C(5) 0.535(1) 0.1954(10) 0.7277(6) 0.057(4) Uani d . 1.00 . C(6) 0.425(2) 0.2518(10) 0.7163(6) 0.061(4) Uani d . 1.00 . C(7) 0.322(1) 0.2228(8) 0.6757(5) 0.045(3) Uani d . 1.00 . C(8) 0.325(1) 0.1355(7) 0.6452(5) 0.043(3) Uani d . 1.00 . C(9) 0.433(1) 0.0776(8) 0.6576(6) 0.047(3) Uani d . 1.00 . C(11) 0.766(2) 0.089(1) 0.729(1) 0.088(6) Uani d . 1.00 . C(12) 0.203(2) 0.2850(9) 0.6612(7) 0.060(4) Uani d . 1.00 . C(13) 0.089(2) 0.257(2) 0.7067(10) 0.106(7) Uani d . 1.00 . C(14) 0.231(3) 0.381(1) 0.669(1) 0.133(9) Uani d . 1.00 . C(15) 0.075(1) -0.070(1) 0.5236(7) 0.059(4) Uani d . 1.00 . C(16) 0.122(1) -0.0946(9) 0.4551(7) 0.055(4) Uani d . 1.00 . C(17) 0.225(1) -0.1585(9) 0.4629(6) 0.053(4) Uani d . 1.00 . C(18) 0.245(2) -0.1706(9) 0.5373(6) 0.052(3) Uani d . 1.00 . C(19) 0.150(1) -0.118(1) 0.5744(6) 0.056(4) Uani d . 1.00 . C(20) 0.323(1) 0.0897(9) 0.4132(6) 0.052(3) Uani d . 1.00 . C(21) 0.402(1) 0.1269(9) 0.4678(6) 0.050(3) Uani d . 1.00 . C(22) 0.506(1) 0.0672(9) 0.4818(7) 0.049(3) Uani d . 1.00 . C(23) 0.487(1) -0.0110(9) 0.4373(6) 0.049(3) Uani d . 1.00 . C(24) 0.380(1) 0.0056(9) 0.3910(5) 0.048(3) Uani d . 1.00 . C(25) -0.052(2) -0.018(2) 0.538(1) 0.104(7) Uani d . 1.00 . C(26) 0.046(2) -0.073(1) 0.3873(9) 0.091(6) Uani d . 1.00 . C(27) 0.281(2) -0.221(1) 0.4073(8) 0.083(5) Uani d . 1.00 . C(28) 0.340(2) -0.2391(9) 0.570(1) 0.076(5) Uani d . 1.00 . C(29) 0.123(2) -0.124(1) 0.6540(8) 0.091(6) Uani d . 1.00 . C(30) 0.215(2) 0.140(1) 0.376(1) 0.093(6) Uani d . 1.00 . C(31) 0.398(2) 0.2219(10) 0.4936(9) 0.084(5) Uani d . 1.00 . C(32) 0.627(1) 0.087(2) 0.5253(9) 0.084(5) Uani d . 1.00 . C(33) 0.589(2) -0.085(1) 0.4328(9) 0.076(5) Uani d . 1.00 . C(34) 0.361(2) -0.039(1) 0.3202(6) 0.076(5) Uani d . 1.00 . H(35) 0.6070 0.2168 0.7556 0.0686 Uiso calc . 1.00 . H(36) 0.4226 0.3102 0.7371 0.0732 Uiso calc . 1.00 . H(37) 0.7963 0.1294 0.6927 0.1057 Uiso calc . 1.00 . H(38) 0.8281 0.0415 0.7340 0.1057 Uiso calc . 1.00 . H(39) 0.7586 0.1207 0.7729 0.1057 Uiso calc . 1.00 . H(40) 0.1777 0.2753 0.6129 0.0714 Uiso calc . 1.00 . H(41) 0.0123 0.2899 0.6927 0.1273 Uiso calc . 1.00 . H(42) 0.0733 0.1947 0.7010 0.1273 Uiso calc . 1.00 . H(43) 0.1081 0.2698 0.7555 0.1273 Uiso calc . 1.00 . H(44) 0.1555 0.4150 0.6547 0.1606 Uiso calc . 1.00 . H(45) 0.3038 0.3971 0.6389 0.1606 Uiso calc . 1.00 . H(46) 0.2522 0.3945 0.7171 0.1606 Uiso calc . 1.00 . H(47) -0.1251 -0.0510 0.5198 0.1249 Uiso calc . 1.00 . H(48) -0.0473 0.0389 0.5155 0.1249 Uiso calc . 1.00 . H(49) -0.0624 -0.0103 0.5883 0.1249 Uiso calc . 1.00 . H(50) -0.0387 -0.1012 0.3890 0.1093 Uiso calc . 1.00 . H(51) 0.0933 -0.0945 0.3470 0.1093 Uiso calc . 1.00 . H(52) 0.0344 -0.0097 0.3834 0.1093 Uiso calc . 1.00 . H(53) 0.2555 -0.2006 0.3611 0.1001 Uiso calc . 1.00 . H(54) 0.3745 -0.2217 0.4108 0.1001 Uiso calc . 1.00 . H(55) 0.2472 -0.2799 0.4150 0.1001 Uiso calc . 1.00 . H(56) 0.3156 -0.2980 0.5560 0.0918 Uiso calc . 1.00 . H(57) 0.4279 -0.2269 0.5546 0.0918 Uiso calc . 1.00 . H(58) 0.3365 -0.2348 0.6211 0.0918 Uiso calc . 1.00 . H(59) 0.0965 -0.1833 0.6659 0.1092 Uiso calc . 1.00 . H(60) 0.2014 -0.1091 0.6796 0.1092 Uiso calc . 1.00 . H(61) 0.0549 -0.0827 0.6664 0.1092 Uiso calc . 1.00 . H(62) 0.1755 0.1020 0.3411 0.1120 Uiso calc . 1.00 . H(63) 0.2501 0.1919 0.3539 0.1120 Uiso calc . 1.00 . H(64) 0.1499 0.1570 0.4104 0.1120 Uiso calc . 1.00 . H(65) 0.3180 0.2496 0.4778 0.1004 Uiso calc . 1.00 . H(66) 0.4713 0.2540 0.4750 0.1004 Uiso calc . 1.00 . H(67) 0.4006 0.2227 0.5444 0.1004 Uiso calc . 1.00 . H(68) 0.6814 0.0351 0.5269 0.1002 Uiso calc . 1.00 . H(69) 0.6738 0.1354 0.5041 0.1002 Uiso calc . 1.00 . H(70) 0.6011 0.1030 0.5726 0.1002 Uiso calc . 1.00 . H(71) 0.5592 -0.1310 0.4012 0.0912 Uiso calc . 1.00 . H(72) 0.6705 -0.0614 0.4156 0.0912 Uiso calc . 1.00 . H(73) 0.6029 -0.1105 0.4791 0.0912 Uiso calc . 1.00 . H(74) 0.2821 -0.0169 0.2987 0.0912 Uiso calc . 1.00 . H(75) 0.4341 -0.0261 0.2900 0.0912 Uiso calc . 1.00 . H(76) 0.3539 -0.1022 0.3268 0.0912 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 Se(3) 0.0528(7) 0.0573(7) 0.0408(6) -0.0019(7) -0.0097(6) 0.0069(6) Ti(2) 0.0348(9) 0.051(1) 0.0255(7) 0.0005(9) 0.0001(7) 0.0008(7) S(1) 0.035(1) 0.064(2) 0.036(1) -0.001(1) -0.002(1) -0.012(1) O(10) 0.066(6) 0.079(6) 0.062(5) -0.001(6) -0.021(5) -0.002(5) C(4) 0.053(7) 0.072(8) 0.035(5) 0.009(7) -0.007(5) -0.006(5) C(5) 0.066(8) 0.073(8) 0.032(5) -0.018(7) -0.002(6) 0.002(5) C(6) 0.077(9) 0.072(9) 0.034(6) -0.004(9) -0.007(6) -0.007(5) C(7) 0.057(7) 0.049(6) 0.030(5) 0.005(6) -0.007(5) 0.000(4) C(8) 0.041(6) 0.048(6) 0.038(5) -0.007(6) 0.003(5) 0.004(4) C(9) 0.054(7) 0.054(6) 0.032(4) -0.007(7) 0.000(5) -0.002(5) C(11) 0.067(10) 0.10(1) 0.10(1) -0.01(1) -0.033(10) 0.00(1) C(12) 0.073(9) 0.059(7) 0.046(6) 0.020(8) 0.000(7) -0.009(5) C(13) 0.10(1) 0.15(2) 0.070(10) 0.08(2) 0.02(1) 0.01(1) C(14) 0.17(3) 0.08(1) 0.15(2) 0.03(1) -0.09(2) -0.03(1) C(15) 0.044(7) 0.081(9) 0.053(7) -0.013(7) -0.004(6) -0.021(6) C(16) 0.054(7) 0.061(8) 0.049(6) -0.007(7) -0.032(6) -0.010(6) C(17) 0.069(9) 0.050(7) 0.039(5) -0.010(7) 0.005(6) -0.001(5) C(18) 0.063(8) 0.060(7) 0.033(5) -0.021(7) -0.008(6) 0.009(5) C(19) 0.055(7) 0.083(9) 0.031(5) -0.019(7) -0.001(5) -0.004(6) C(20) 0.064(8) 0.059(7) 0.034(5) 0.001(7) 0.008(6) 0.000(5) C(21) 0.044(7) 0.062(7) 0.044(6) -0.001(6) 0.013(5) 0.005(5) C(22) 0.044(6) 0.063(7) 0.041(5) -0.001(6) 0.001(5) 0.005(6) C(23) 0.049(7) 0.049(6) 0.048(6) -0.002(6) 0.015(6) 0.000(5) C(24) 0.055(7) 0.062(7) 0.028(4) -0.014(6) 0.012(4) 0.002(5) C(25) 0.045(8) 0.12(2) 0.15(2) 0.00(1) 0.00(1) -0.04(1) C(26) 0.09(1) 0.11(1) 0.068(9) -0.04(1) -0.041(10) -0.011(9) C(27) 0.13(2) 0.065(9) 0.057(7) 0.01(1) 0.015(10) -0.026(7) C(28) 0.065(8) 0.035(7) 0.13(1) -0.008(7) -0.03(1) 0.013(8) C(29) 0.11(1) 0.12(1) 0.044(7) -0.06(1) 0.030(9) -0.024(9) C(30) 0.08(1) 0.11(1) 0.09(1) 0.00(1) -0.03(1) 0.06(1) C(31) 0.11(1) 0.060(8) 0.081(10) 0.016(9) 0.04(1) 0.003(8) C(32) 0.028(6) 0.16(2) 0.067(9) 0.002(9) 0.009(6) 0.04(1) C(33) 0.08(1) 0.069(9) 0.076(9) 0.020(9) 0.051(9) -0.005(8) C(34) 0.12(1) 0.080(10) 0.029(5) -0.02(1) 0.004(7) -0.008(6) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00578|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 1834 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0553 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0847 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.762 _refine_ls_shift/esd_max 0.0051 _refine_ls_shift/esd_mean 0.0002 _refine_diff_density_min -0.62 _refine_diff_density_max 0.69 #------------------------------------------------------------------------------ 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 Se(3) Ti(2) 2.553(2) 1_555 1_555 yes Se(3) C(9) 1.89(1) 1_555 1_555 yes Ti(2) S(1) 2.428(3) 1_555 1_555 yes Ti(2) C(15) 2.41(1) 1_555 1_555 yes Ti(2) C(16) 2.42(1) 1_555 1_555 yes Ti(2) C(17) 2.46(1) 1_555 1_555 yes Ti(2) C(18) 2.43(1) 1_555 1_555 yes Ti(2) C(19) 2.43(1) 1_555 1_555 yes Ti(2) C(20) 2.44(1) 1_555 1_555 yes Ti(2) C(21) 2.49(1) 1_555 1_555 yes Ti(2) C(22) 2.49(1) 1_555 1_555 yes Ti(2) C(23) 2.38(1) 1_555 1_555 yes Ti(2) C(24) 2.458(10) 1_555 1_555 yes S(1) C(8) 1.77(1) 1_555 1_555 yes O(10) C(4) 1.36(2) 1_555 1_555 yes O(10) C(11) 1.38(2) 1_555 1_555 yes C(4) C(5) 1.36(2) 1_555 1_555 yes C(4) C(9) 1.43(2) 1_555 1_555 yes C(5) C(6) 1.41(2) 1_555 1_555 yes C(5) H(35) 0.950 1_555 1_555 no C(6) C(7) 1.36(2) 1_555 1_555 yes C(6) H(36) 0.950 1_555 1_555 no C(7) C(8) 1.42(2) 1_555 1_555 yes C(7) C(12) 1.54(2) 1_555 1_555 yes C(8) C(9) 1.41(2) 1_555 1_555 yes C(11) H(37) 0.951 1_555 1_555 no C(11) H(38) 0.950 1_555 1_555 no C(11) H(39) 0.950 1_555 1_555 no C(12) C(13) 1.49(3) 1_555 1_555 yes C(12) C(14) 1.47(3) 1_555 1_555 yes C(12) H(40) 0.950 1_555 1_555 no C(13) H(41) 0.950 1_555 1_555 no C(13) H(42) 0.950 1_555 1_555 no C(13) H(43) 0.950 1_555 1_555 no C(14) H(44) 0.948 1_555 1_555 no C(14) H(45) 0.953 1_555 1_555 no C(14) H(46) 0.950 1_555 1_555 no C(15) C(16) 1.41(2) 1_555 1_555 yes C(15) C(19) 1.40(2) 1_555 1_555 yes C(15) C(25) 1.52(2) 1_555 1_555 yes C(16) C(17) 1.42(2) 1_555 1_555 yes C(16) C(26) 1.52(2) 1_555 1_555 yes C(17) C(18) 1.42(2) 1_555 1_555 yes C(17) C(27) 1.50(2) 1_555 1_555 yes C(18) C(19) 1.42(2) 1_555 1_555 yes C(18) C(28) 1.53(2) 1_555 1_555 yes C(19) C(29) 1.51(2) 1_555 1_555 yes C(20) C(21) 1.41(2) 1_555 1_555 yes C(20) C(24) 1.44(2) 1_555 1_555 yes C(20) C(30) 1.49(2) 1_555 1_555 yes C(21) C(22) 1.40(2) 1_555 1_555 yes C(21) C(31) 1.49(2) 1_555 1_555 yes C(22) C(23) 1.44(2) 1_555 1_555 yes C(22) C(32) 1.50(2) 1_555 1_555 yes C(23) C(24) 1.40(2) 1_555 1_555 yes C(23) C(33) 1.52(2) 1_555 1_555 yes C(24) C(34) 1.49(2) 1_555 1_555 yes C(25) H(47) 0.950 1_555 1_555 no C(25) H(48) 0.951 1_555 1_555 no C(25) H(49) 0.950 1_555 1_555 no C(26) H(50) 0.950 1_555 1_555 no C(26) H(51) 0.950 1_555 1_555 no C(26) H(52) 0.950 1_555 1_555 no C(27) H(53) 0.950 1_555 1_555 no C(27) H(54) 0.949 1_555 1_555 no C(27) H(55) 0.950 1_555 1_555 no C(28) H(56) 0.950 1_555 1_555 no C(28) H(57) 0.949 1_555 1_555 no C(28) H(58) 0.950 1_555 1_555 no C(29) H(59) 0.950 1_555 1_555 no C(29) H(60) 0.950 1_555 1_555 no C(29) H(61) 0.950 1_555 1_555 no C(30) H(62) 0.950 1_555 1_555 no C(30) H(63) 0.950 1_555 1_555 no C(30) H(64) 0.950 1_555 1_555 no C(31) H(65) 0.950 1_555 1_555 no C(31) H(66) 0.950 1_555 1_555 no C(31) H(67) 0.950 1_555 1_555 no C(32) H(68) 0.951 1_555 1_555 no C(32) H(69) 0.950 1_555 1_555 no C(32) H(70) 0.950 1_555 1_555 no C(33) H(71) 0.949 1_555 1_555 no C(33) H(72) 0.951 1_555 1_555 no C(33) H(73) 0.951 1_555 1_555 no C(34) H(74) 0.950 1_555 1_555 no C(34) H(75) 0.950 1_555 1_555 no C(34) H(76) 0.950 1_555 1_555 no #------------------------------------------------------------------------------ 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 Ti(2) Se(3) C(9) 94.9(4) 1_555 1_555 1_555 yes Se(3) Ti(2) S(1) 81.80(9) 1_555 1_555 1_555 yes Se(3) Ti(2) C(15) 112.8(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(16) 133.8(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(17) 109.5(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(18) 79.1(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(19) 81.2(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(20) 133.0(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(21) 101.4(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(22) 79.7(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(23) 93.5(3) 1_555 1_555 1_555 yes Se(3) Ti(2) C(24) 127.1(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(15) 76.9(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(16) 106.1(4) 1_555 1_555 1_555 yes S(1) Ti(2) C(17) 132.9(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(18) 115.5(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(19) 82.5(4) 1_555 1_555 1_555 yes S(1) Ti(2) C(20) 95.3(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(21) 80.6(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(22) 101.3(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(23) 134.7(3) 1_555 1_555 1_555 yes S(1) Ti(2) C(24) 129.4(3) 1_555 1_555 1_555 yes C(15) Ti(2) C(16) 33.9(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(17) 56.3(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(18) 56.4(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(19) 33.6(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(20) 112.0(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(21) 135.3(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(22) 166.6(5) 1_555 1_555 1_555 yes C(15) Ti(2) C(23) 143.0(4) 1_555 1_555 1_555 yes C(15) Ti(2) C(24) 115.3(4) 1_555 1_555 1_555 yes C(16) Ti(2) C(17) 33.8(5) 1_555 1_555 1_555 yes C(16) Ti(2) C(18) 56.1(4) 1_555 1_555 1_555 yes C(16) Ti(2) C(19) 55.9(4) 1_555 1_555 1_555 yes C(16) Ti(2) C(20) 92.3(5) 1_555 1_555 1_555 yes C(16) Ti(2) C(21) 124.8(5) 1_555 1_555 1_555 yes C(16) Ti(2) C(22) 138.9(5) 1_555 1_555 1_555 yes C(16) Ti(2) C(23) 109.1(5) 1_555 1_555 1_555 yes C(16) Ti(2) C(24) 83.3(5) 1_555 1_555 1_555 yes C(17) Ti(2) C(18) 33.6(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(19) 56.0(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(20) 106.4(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(21) 136.4(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(22) 125.5(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(23) 91.3(4) 1_555 1_555 1_555 yes C(17) Ti(2) C(24) 80.9(4) 1_555 1_555 1_555 yes C(18) Ti(2) C(19) 34.0(5) 1_555 1_555 1_555 yes C(18) Ti(2) C(20) 139.9(4) 1_555 1_555 1_555 yes C(18) Ti(2) C(21) 163.6(4) 1_555 1_555 1_555 yes C(18) Ti(2) C(22) 133.9(5) 1_555 1_555 1_555 yes C(18) Ti(2) C(23) 107.6(5) 1_555 1_555 1_555 yes C(18) Ti(2) C(24) 110.8(4) 1_555 1_555 1_555 yes C(19) Ti(2) C(20) 145.2(5) 1_555 1_555 1_555 yes C(19) Ti(2) C(21) 162.3(5) 1_555 1_555 1_555 yes C(19) Ti(2) C(22) 159.8(5) 1_555 1_555 1_555 yes C(19) Ti(2) C(23) 141.6(5) 1_555 1_555 1_555 yes C(19) Ti(2) C(24) 135.8(4) 1_555 1_555 1_555 yes C(20) Ti(2) C(21) 33.1(4) 1_555 1_555 1_555 yes C(20) Ti(2) C(22) 54.7(4) 1_555 1_555 1_555 yes C(20) Ti(2) C(23) 56.2(5) 1_555 1_555 1_555 yes C(20) Ti(2) C(24) 34.1(4) 1_555 1_555 1_555 yes C(21) Ti(2) C(22) 32.6(4) 1_555 1_555 1_555 yes C(21) Ti(2) C(23) 56.1(4) 1_555 1_555 1_555 yes C(21) Ti(2) C(24) 55.7(4) 1_555 1_555 1_555 yes C(22) Ti(2) C(23) 34.3(4) 1_555 1_555 1_555 yes C(22) Ti(2) C(24) 55.5(4) 1_555 1_555 1_555 yes C(23) Ti(2) C(24) 33.7(4) 1_555 1_555 1_555 yes Ti(2) S(1) C(8) 103.4(4) 1_555 1_555 1_555 yes C(4) O(10) C(11) 120(1) 1_555 1_555 1_555 yes O(10) C(4) C(5) 122(1) 1_555 1_555 1_555 yes O(10) C(4) C(9) 117(1) 1_555 1_555 1_555 yes C(5) C(4) C(9) 119(1) 1_555 1_555 1_555 yes C(4) C(5) C(6) 121(1) 1_555 1_555 1_555 yes C(4) C(5) H(35) 119(1) 1_555 1_555 1_555 no C(6) C(5) H(35) 119(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 120(1) 1_555 1_555 1_555 yes C(5) C(6) H(36) 120(1) 1_555 1_555 1_555 no C(7) C(6) H(36) 119(1) 1_555 1_555 1_555 no C(6) C(7) C(8) 120(1) 1_555 1_555 1_555 yes C(6) C(7) C(12) 120(1) 1_555 1_555 1_555 yes C(8) C(7) C(12) 119(1) 1_555 1_555 1_555 yes S(1) C(8) C(7) 121.6(9) 1_555 1_555 1_555 yes S(1) C(8) C(9) 117.9(8) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120(1) 1_555 1_555 1_555 yes Se(3) C(9) C(4) 118(1) 1_555 1_555 1_555 yes Se(3) C(9) C(8) 122.9(9) 1_555 1_555 1_555 yes C(4) C(9) C(8) 118(1) 1_555 1_555 1_555 yes O(10) C(11) H(37) 109(1) 1_555 1_555 1_555 no O(10) C(11) H(38) 109(1) 1_555 1_555 1_555 no O(10) C(11) H(39) 109(1) 1_555 1_555 1_555 no H(37) C(11) H(38) 109(2) 1_555 1_555 1_555 no H(37) C(11) H(39) 109(1) 1_555 1_555 1_555 no H(38) C(11) H(39) 109(1) 1_555 1_555 1_555 no C(7) C(12) C(13) 109(1) 1_555 1_555 1_555 yes C(7) C(12) C(14) 114(1) 1_555 1_555 1_555 yes C(7) C(12) H(40) 106(1) 1_555 1_555 1_555 no C(13) C(12) C(14) 111(1) 1_555 1_555 1_555 yes C(13) C(12) H(40) 106(1) 1_555 1_555 1_555 no C(14) C(12) H(40) 106(1) 1_555 1_555 1_555 no C(12) C(13) H(41) 109(1) 1_555 1_555 1_555 no C(12) C(13) H(42) 109(1) 1_555 1_555 1_555 no C(12) C(13) H(43) 109(2) 1_555 1_555 1_555 no H(41) C(13) H(42) 109(2) 1_555 1_555 1_555 no H(41) C(13) H(43) 109(1) 1_555 1_555 1_555 no H(42) C(13) H(43) 109(1) 1_555 1_555 1_555 no C(12) C(14) H(44) 109(2) 1_555 1_555 1_555 no C(12) C(14) H(45) 109(2) 1_555 1_555 1_555 no C(12) C(14) H(46) 109(2) 1_555 1_555 1_555 no H(44) C(14) H(45) 109(2) 1_555 1_555 1_555 no H(44) C(14) H(46) 109(2) 1_555 1_555 1_555 no H(45) C(14) H(46) 109(2) 1_555 1_555 1_555 no Ti(2) C(15) C(16) 73.1(8) 1_555 1_555 1_555 yes Ti(2) C(15) C(19) 74.0(8) 1_555 1_555 1_555 yes Ti(2) C(15) C(25) 128(1) 1_555 1_555 1_555 yes C(16) C(15) C(19) 107(1) 1_555 1_555 1_555 yes C(16) C(15) C(25) 124(1) 1_555 1_555 1_555 yes C(19) C(15) C(25) 126(1) 1_555 1_555 1_555 yes Ti(2) C(16) C(15) 73.0(7) 1_555 1_555 1_555 yes Ti(2) C(16) C(17) 74.9(7) 1_555 1_555 1_555 yes Ti(2) C(16) C(26) 130(1) 1_555 1_555 1_555 yes C(15) C(16) C(17) 108(1) 1_555 1_555 1_555 yes C(15) C(16) C(26) 122(1) 1_555 1_555 1_555 yes C(17) C(16) C(26) 126(1) 1_555 1_555 1_555 yes Ti(2) C(17) C(16) 71.3(7) 1_555 1_555 1_555 yes Ti(2) C(17) C(18) 71.9(7) 1_555 1_555 1_555 yes Ti(2) C(17) C(27) 133(1) 1_555 1_555 1_555 yes C(16) C(17) C(18) 106(1) 1_555 1_555 1_555 yes C(16) C(17) C(27) 128(1) 1_555 1_555 1_555 yes C(18) C(17) C(27) 123(1) 1_555 1_555 1_555 yes Ti(2) C(18) C(17) 74.5(7) 1_555 1_555 1_555 yes Ti(2) C(18) C(19) 73.2(8) 1_555 1_555 1_555 yes Ti(2) C(18) C(28) 124.8(9) 1_555 1_555 1_555 yes C(17) C(18) C(19) 108(1) 1_555 1_555 1_555 yes C(17) C(18) C(28) 124(1) 1_555 1_555 1_555 yes C(19) C(18) C(28) 126(1) 1_555 1_555 1_555 yes Ti(2) C(19) C(15) 72.4(8) 1_555 1_555 1_555 yes Ti(2) C(19) C(18) 72.8(7) 1_555 1_555 1_555 yes Ti(2) C(19) C(29) 127(1) 1_555 1_555 1_555 yes C(15) C(19) C(18) 108.2(10) 1_555 1_555 1_555 yes C(15) C(19) C(29) 126(1) 1_555 1_555 1_555 yes C(18) C(19) C(29) 124(1) 1_555 1_555 1_555 yes Ti(2) C(20) C(21) 75.3(7) 1_555 1_555 1_555 yes Ti(2) C(20) C(24) 73.5(6) 1_555 1_555 1_555 yes Ti(2) C(20) C(30) 126(1) 1_555 1_555 1_555 yes C(21) C(20) C(24) 108(1) 1_555 1_555 1_555 yes C(21) C(20) C(30) 123(1) 1_555 1_555 1_555 yes C(24) C(20) C(30) 126(1) 1_555 1_555 1_555 yes Ti(2) C(21) C(20) 71.6(7) 1_555 1_555 1_555 yes Ti(2) C(21) C(22) 73.6(7) 1_555 1_555 1_555 yes Ti(2) C(21) C(31) 132.1(9) 1_555 1_555 1_555 yes C(20) C(21) C(22) 108(1) 1_555 1_555 1_555 yes C(20) C(21) C(31) 126(1) 1_555 1_555 1_555 yes C(22) C(21) C(31) 124(1) 1_555 1_555 1_555 yes Ti(2) C(22) C(21) 73.8(7) 1_555 1_555 1_555 yes Ti(2) C(22) C(23) 68.9(7) 1_555 1_555 1_555 yes Ti(2) C(22) C(32) 130.6(9) 1_555 1_555 1_555 yes C(21) C(22) C(23) 107(1) 1_555 1_555 1_555 yes C(21) C(22) C(32) 126(1) 1_555 1_555 1_555 yes C(23) C(22) C(32) 125(1) 1_555 1_555 1_555 yes Ti(2) C(23) C(22) 76.8(7) 1_555 1_555 1_555 yes Ti(2) C(23) C(24) 76.0(7) 1_555 1_555 1_555 yes Ti(2) C(23) C(33) 124.4(9) 1_555 1_555 1_555 yes C(22) C(23) C(24) 108(1) 1_555 1_555 1_555 yes C(22) C(23) C(33) 122(1) 1_555 1_555 1_555 yes C(24) C(23) C(33) 128(1) 1_555 1_555 1_555 yes Ti(2) C(24) C(20) 72.4(6) 1_555 1_555 1_555 yes Ti(2) C(24) C(23) 70.3(6) 1_555 1_555 1_555 yes Ti(2) C(24) C(34) 137.0(9) 1_555 1_555 1_555 yes C(20) C(24) C(23) 106(1) 1_555 1_555 1_555 yes C(20) C(24) C(34) 126(1) 1_555 1_555 1_555 yes C(23) C(24) C(34) 124(1) 1_555 1_555 1_555 yes C(15) C(25) H(47) 109(1) 1_555 1_555 1_555 no C(15) C(25) H(48) 109(1) 1_555 1_555 1_555 no C(15) C(25) H(49) 109(1) 1_555 1_555 1_555 no H(47) C(25) H(48) 109(2) 1_555 1_555 1_555 no H(47) C(25) H(49) 109(2) 1_555 1_555 1_555 no H(48) C(25) H(49) 109(2) 1_555 1_555 1_555 no C(16) C(26) H(50) 109(1) 1_555 1_555 1_555 no C(16) C(26) H(51) 109(1) 1_555 1_555 1_555 no C(16) C(26) H(52) 109(1) 1_555 1_555 1_555 no H(50) C(26) H(51) 109(1) 1_555 1_555 1_555 no H(50) C(26) H(52) 109(2) 1_555 1_555 1_555 no H(51) C(26) H(52) 109(1) 1_555 1_555 1_555 no C(17) C(27) H(53) 109(1) 1_555 1_555 1_555 no C(17) C(27) H(54) 109(1) 1_555 1_555 1_555 no C(17) C(27) H(55) 109(1) 1_555 1_555 1_555 no H(53) C(27) H(54) 109(1) 1_555 1_555 1_555 no H(53) C(27) H(55) 109(1) 1_555 1_555 1_555 no H(54) C(27) H(55) 109(1) 1_555 1_555 1_555 no C(18) C(28) H(56) 109(1) 1_555 1_555 1_555 no C(18) C(28) H(57) 109(1) 1_555 1_555 1_555 no C(18) C(28) H(58) 109(1) 1_555 1_555 1_555 no H(56) C(28) H(57) 109(1) 1_555 1_555 1_555 no H(56) C(28) H(58) 109(1) 1_555 1_555 1_555 no H(57) C(28) H(58) 109(1) 1_555 1_555 1_555 no C(19) C(29) H(59) 109(1) 1_555 1_555 1_555 no C(19) C(29) H(60) 109(1) 1_555 1_555 1_555 no C(19) C(29) H(61) 109(1) 1_555 1_555 1_555 no H(59) C(29) H(60) 109(2) 1_555 1_555 1_555 no H(59) C(29) H(61) 109(1) 1_555 1_555 1_555 no H(60) C(29) H(61) 109(1) 1_555 1_555 1_555 no C(20) C(30) H(62) 109(1) 1_555 1_555 1_555 no C(20) C(30) H(63) 109(1) 1_555 1_555 1_555 no C(20) C(30) H(64) 109(1) 1_555 1_555 1_555 no H(62) C(30) H(63) 109(1) 1_555 1_555 1_555 no H(62) C(30) H(64) 109(1) 1_555 1_555 1_555 no H(63) C(30) H(64) 109(2) 1_555 1_555 1_555 no C(21) C(31) H(65) 109(1) 1_555 1_555 1_555 no C(21) C(31) H(66) 109(1) 1_555 1_555 1_555 no C(21) C(31) H(67) 109(1) 1_555 1_555 1_555 no H(65) C(31) H(66) 109(1) 1_555 1_555 1_555 no H(65) C(31) H(67) 109(1) 1_555 1_555 1_555 no H(66) C(31) H(67) 109(2) 1_555 1_555 1_555 no C(22) C(32) H(68) 109(1) 1_555 1_555 1_555 no C(22) C(32) H(69) 109(1) 1_555 1_555 1_555 no C(22) C(32) H(70) 109(1) 1_555 1_555 1_555 no H(68) C(32) H(69) 109(1) 1_555 1_555 1_555 no H(68) C(32) H(70) 109(1) 1_555 1_555 1_555 no H(69) C(32) H(70) 109(2) 1_555 1_555 1_555 no C(23) C(33) H(71) 109(1) 1_555 1_555 1_555 no C(23) C(33) H(72) 109(1) 1_555 1_555 1_555 no C(23) C(33) H(73) 109(1) 1_555 1_555 1_555 no H(71) C(33) H(72) 109(1) 1_555 1_555 1_555 no H(71) C(33) H(73) 109(1) 1_555 1_555 1_555 no H(72) C(33) H(73) 109(1) 1_555 1_555 1_555 no C(24) C(34) H(74) 109(1) 1_555 1_555 1_555 no C(24) C(34) H(75) 109(1) 1_555 1_555 1_555 no C(24) C(34) H(76) 109(1) 1_555 1_555 1_555 no H(74) C(34) H(75) 109(1) 1_555 1_555 1_555 no H(74) C(34) H(76) 109(1) 1_555 1_555 1_555 no H(75) C(34) H(76) 109(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ data_SSeTe/Mo _database_code_CSD 187545 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 6 11:02:07 2002' _audit_creation_method 'from TEXRAY.INF file' #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' #------------------------------------------------------------------------------ _publ_section_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. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; #------------------------------------------------------------------------------ _chemical_formula_weight 386.82 _chemical_formula_sum 'C10 H12 O S Se Te ' _chemical_formula_moiety 'C10 H12 O S Se Te ' _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.373(2) _cell_length_b 16.563(3) _cell_length_c 10.046(2) _cell_angle_alpha 90 _cell_angle_beta 94.66(2) _cell_angle_gamma 90 _cell_volume 1222.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 728.00 _exptl_absorpt_coefficient_mu 5.548 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.761 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 294.2 _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_% 1.57 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 -1 1 -2 0 1 -3 -1 _diffrn_reflns_number 2420 _reflns_number_total 2240 _reflns_number_observed 1926 _reflns_observed_criterion >1.5sigma(I) _diffrn_reflns_av_R_equivalents 0.008 _diffrn_reflns_av_sigmaI/netI 0.017 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02042 _diffrn_orient_matrix_UB_12 -0.04468 _diffrn_orient_matrix_UB_13 -0.06648 _diffrn_orient_matrix_UB_21 -0.02657 _diffrn_orient_matrix_UB_22 0.04059 _diffrn_orient_matrix_UB_23 -0.07267 _diffrn_orient_matrix_UB_31 0.13189 _diffrn_orient_matrix_UB_32 0.00126 _diffrn_orient_matrix_UB_33 -0.01656 #------------------------------------------------------------------------------ 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 40 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; Te 0 4 -0.531 1.675 ;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 Te(3) 0.73172(3) 0.18509(1) 0.92059(2) 0.04611(10) Uani d . 1.00 . Se(2) 0.92679(5) 0.19568(2) 0.72537(4) 0.0463(1) Uani d . 1.00 . S(1) 0.7998(1) 0.08459(5) 0.63569(7) 0.0415(2) Uani d . 1.00 . O(13) 0.7076(3) 0.0544(2) 1.1275(2) 0.0490(7) Uani d . 1.00 . C(4) 0.7427(4) 0.0125(2) 1.0153(3) 0.0348(7) Uani d . 1.00 . C(5) 0.7571(4) -0.0707(2) 1.0063(3) 0.0436(9) Uani d . 1.00 . C(6) 0.7931(4) -0.1049(2) 0.8862(3) 0.0426(9) Uani d . 1.00 . C(7) 0.8144(4) -0.0604(2) 0.7711(3) 0.0348(7) Uani d . 1.00 . C(8) 0.7627(4) 0.0595(2) 0.9035(3) 0.0317(7) Uani d . 1.00 . C(9) 0.7974(4) 0.0237(2) 0.7814(3) 0.0299(7) Uani d . 1.00 . C(10) 0.8527(5) -0.1007(2) 0.6413(3) 0.0446(9) Uani d . 1.00 . C(11) 0.6786(7) -0.1117(3) 0.5508(5) 0.061(1) Uani d . 1.00 . C(12) 0.9561(9) -0.1808(3) 0.6607(5) 0.068(2) Uani d . 1.00 . C(14) 0.6943(6) 0.0097(3) 1.2479(4) 0.056(1) Uani d . 1.00 . H(15) 0.733(4) -0.101(2) 1.085(4) 0.046(10) Uiso calc . 1.00 . H(16) 0.811(5) -0.163(2) 0.884(3) 0.034(8) Uiso calc . 1.00 . H(17) 0.924(5) -0.069(2) 0.585(4) 0.045(9) Uiso calc . 1.00 . H(18) 0.699(7) -0.132(3) 0.477(6) 0.08(2) Uiso calc . 1.00 . H(19) 0.591(6) -0.058(3) 0.522(5) 0.07(1) Uiso calc . 1.00 . H(20) 0.601(8) -0.143(4) 0.602(6) 0.10(2) Uiso calc . 1.00 . H(21) 0.993(7) -0.210(3) 0.594(5) 0.08(1) Uiso calc . 1.00 . H(22) 1.056(7) -0.171(3) 0.720(5) 0.07(2) Uiso calc . 1.00 . H(23) 0.884(6) -0.215(3) 0.694(4) 0.06(1) Uiso calc . 1.00 . H(24) 0.805(6) -0.020(2) 1.266(4) 0.06(1) Uiso calc . 1.00 . H(25) 0.591(9) -0.024(4) 1.243(6) 0.11(2) Uiso calc . 1.00 . H(26) 0.672(7) 0.060(3) 1.319(5) 0.09(2) 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 Te(3) 0.0613(2) 0.0323(2) 0.0454(2) 0.00974(9) 0.0080(1) -0.00412(8) Se(2) 0.0602(3) 0.0314(2) 0.0478(2) -0.0036(1) 0.0072(2) 0.0051(1) S(1) 0.0569(5) 0.0368(4) 0.0302(4) -0.0030(3) 0.0003(3) 0.0038(3) O(13) 0.059(1) 0.059(2) 0.030(1) 0.006(1) 0.0106(10) -0.003(1) C(4) 0.033(1) 0.043(2) 0.029(1) 0.005(1) 0.006(1) 0.002(1) C(5) 0.051(2) 0.038(2) 0.043(2) 0.001(2) 0.009(1) 0.011(1) C(6) 0.049(2) 0.031(2) 0.049(2) 0.000(1) 0.006(1) 0.006(1) C(7) 0.036(1) 0.032(2) 0.037(2) 0.001(1) 0.004(1) -0.002(1) C(8) 0.030(1) 0.030(1) 0.034(1) -0.001(1) 0.002(1) 0.001(1) C(9) 0.030(1) 0.031(1) 0.028(1) -0.001(1) 0.002(1) 0.001(1) C(10) 0.056(2) 0.035(2) 0.043(2) -0.002(2) 0.011(1) -0.007(1) C(11) 0.078(3) 0.058(3) 0.048(2) -0.004(2) -0.001(2) -0.015(2) C(12) 0.097(4) 0.050(3) 0.061(3) 0.019(2) 0.020(3) -0.011(2) C(14) 0.047(2) 0.086(3) 0.035(2) -0.004(2) 0.008(1) 0.007(2) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00123|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method ; Zachariasen(1967) type 2 Gaussian isotropic ; _refine_ls_extinction_coef 0.0075(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1926 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0206 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0370 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.936 _refine_ls_shift/esd_max 0.0220 _refine_ls_shift/esd_mean 0.0010 _refine_diff_density_min -0.43 _refine_diff_density_max 0.52 #------------------------------------------------------------------------------ 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 Te(3) Se(2) 2.5306(5) 1_555 1_555 yes Te(3) C(8) 2.101(3) 1_555 1_555 yes Se(2) S(1) 2.2218(9) 1_555 1_555 yes S(1) C(9) 1.779(3) 1_555 1_555 yes O(13) C(4) 1.367(4) 1_555 1_555 yes O(13) C(14) 1.429(4) 1_555 1_555 yes C(4) C(5) 1.385(4) 1_555 1_555 yes C(4) C(8) 1.385(4) 1_555 1_555 yes C(5) C(6) 1.378(5) 1_555 1_555 yes C(5) H(15) 0.96(4) 1_555 1_555 no C(6) C(7) 1.392(4) 1_555 1_555 yes C(6) H(16) 0.97(4) 1_555 1_555 no C(7) C(9) 1.402(4) 1_555 1_555 yes C(7) C(10) 1.512(4) 1_555 1_555 yes C(8) C(9) 1.405(4) 1_555 1_555 yes C(10) C(11) 1.523(6) 1_555 1_555 yes C(10) C(12) 1.534(6) 1_555 1_555 yes C(10) H(17) 0.96(4) 1_555 1_555 no C(11) H(18) 0.84(6) 1_555 1_555 no C(11) H(19) 1.12(5) 1_555 1_555 no C(11) H(20) 0.96(6) 1_555 1_555 no C(12) H(21) 0.89(5) 1_555 1_555 no C(12) H(22) 0.93(6) 1_555 1_555 no C(12) H(23) 0.87(5) 1_555 1_555 no C(14) H(24) 0.96(4) 1_555 1_555 no C(14) H(25) 0.94(7) 1_555 1_555 no C(14) H(26) 1.12(5) 1_555 1_555 no #------------------------------------------------------------------------------ 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 Se(2) Te(3) C(8) 86.16(8) 1_555 1_555 1_555 yes Te(3) Se(2) S(1) 90.54(3) 1_555 1_555 1_555 yes Se(2) S(1) C(9) 99.68(10) 1_555 1_555 1_555 yes C(4) O(13) C(14) 117.7(3) 1_555 1_555 1_555 yes O(13) C(4) C(5) 125.4(3) 1_555 1_555 1_555 yes O(13) C(4) C(8) 115.0(3) 1_555 1_555 1_555 yes C(5) C(4) C(8) 119.5(3) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119.1(3) 1_555 1_555 1_555 yes C(4) C(5) H(15) 116(2) 1_555 1_555 1_555 no C(6) C(5) H(15) 124(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 123.6(3) 1_555 1_555 1_555 yes C(5) C(6) H(16) 117(2) 1_555 1_555 1_555 no C(7) C(6) H(16) 118(2) 1_555 1_555 1_555 no C(6) C(7) C(9) 116.6(3) 1_555 1_555 1_555 yes C(6) C(7) C(10) 121.6(3) 1_555 1_555 1_555 yes C(9) C(7) C(10) 121.8(3) 1_555 1_555 1_555 yes Te(3) C(8) C(4) 118.1(2) 1_555 1_555 1_555 yes Te(3) C(8) C(9) 121.2(2) 1_555 1_555 1_555 yes C(4) C(8) C(9) 120.6(3) 1_555 1_555 1_555 yes S(1) C(9) C(7) 119.7(2) 1_555 1_555 1_555 yes S(1) C(9) C(8) 119.6(2) 1_555 1_555 1_555 yes C(7) C(9) C(8) 120.5(3) 1_555 1_555 1_555 yes C(7) C(10) C(11) 111.1(3) 1_555 1_555 1_555 yes C(7) C(10) C(12) 113.5(3) 1_555 1_555 1_555 yes C(7) C(10) H(17) 114(2) 1_555 1_555 1_555 no C(11) C(10) C(12) 111.0(4) 1_555 1_555 1_555 yes C(11) C(10) H(17) 100(2) 1_555 1_555 1_555 no C(12) C(10) H(17) 105(2) 1_555 1_555 1_555 no C(10) C(11) H(18) 112(3) 1_555 1_555 1_555 no C(10) C(11) H(19) 119(2) 1_555 1_555 1_555 no C(10) C(11) H(20) 105(3) 1_555 1_555 1_555 no H(18) C(11) H(19) 102(4) 1_555 1_555 1_555 no H(18) C(11) H(20) 114(4) 1_555 1_555 1_555 no H(19) C(11) H(20) 102(4) 1_555 1_555 1_555 no C(10) C(12) H(21) 123(3) 1_555 1_555 1_555 no C(10) C(12) H(22) 107(3) 1_555 1_555 1_555 no C(10) C(12) H(23) 107(3) 1_555 1_555 1_555 no H(21) C(12) H(22) 107(4) 1_555 1_555 1_555 no H(21) C(12) H(23) 99(4) 1_555 1_555 1_555 no H(22) C(12) H(23) 110(4) 1_555 1_555 1_555 no O(13) C(14) H(24) 107(2) 1_555 1_555 1_555 no O(13) C(14) H(25) 111(3) 1_555 1_555 1_555 no O(13) C(14) H(26) 100(2) 1_555 1_555 1_555 no H(24) C(14) H(25) 112(4) 1_555 1_555 1_555 no H(24) C(14) H(26) 115(3) 1_555 1_555 1_555 no H(25) C(14) H(26) 108(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ data_Benzo-Se-Se-Te _database_code_CSD 187546 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 7 12:39:38 2002' _audit_creation_method 'from TEXRAY.INF file' #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' #------------------------------------------------------------------------------ _chemical_formula_weight 433.72 _chemical_formula_sum 'C10 H12 O Se2 Te ' _chemical_formula_moiety 'C10 H12 O Se2 Te ' _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 7.389(3) _cell_length_b 16.581(3) _cell_length_c 10.165(3) _cell_angle_alpha 90 _cell_angle_beta 93.14(3) _cell_angle_gamma 90 _cell_volume 1243.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 2.316 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 800.00 _exptl_absorpt_coefficient_mu 8.215 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.382 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _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_% -0.51 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 0 -1 -4 -1 1 -4 1 _diffrn_reflns_number 2467 _reflns_number_total 2282 _reflns_number_observed 2192 _reflns_observed_criterion >0.0sigma(I) _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01027 _diffrn_orient_matrix_UB_12 -0.05897 _diffrn_orient_matrix_UB_13 -0.01961 _diffrn_orient_matrix_UB_21 0.00592 _diffrn_orient_matrix_UB_22 0.01160 _diffrn_orient_matrix_UB_23 -0.09620 _diffrn_orient_matrix_UB_31 0.13502 _diffrn_orient_matrix_UB_32 -0.00499 _diffrn_orient_matrix_UB_33 0.00815 #------------------------------------------------------------------------------ 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 40 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 4 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 8 -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 4 -0.531 1.675 ;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 Te(3) 0.77049(4) 0.18273(1) 0.57126(3) 0.04460(9) Uani d . 1.00 . Se(1) 0.70579(6) 0.08850(2) 0.86912(4) 0.0399(1) Uani d . 1.00 . Se(2) 0.57421(6) 0.20220(2) 0.76422(4) 0.0445(1) Uani d . 1.00 . O(13) 0.7920(4) 0.0511(2) 0.3698(3) 0.0471(9) Uani d . 1.00 . C(4) 0.7571(5) 0.0100(2) 0.4817(4) 0.035(1) Uani d . 1.00 . C(5) 0.7405(6) -0.0728(2) 0.4918(5) 0.043(1) Uani d . 1.00 . C(6) 0.7072(5) -0.1068(2) 0.6119(4) 0.041(1) Uani d . 1.00 . C(7) 0.6867(5) -0.0626(2) 0.7245(4) 0.032(1) Uani d . 1.00 . C(8) 0.7390(5) 0.0569(2) 0.5933(3) 0.028(1) Uani d . 1.00 . C(9) 0.7060(4) 0.0218(2) 0.7136(4) 0.029(1) Uani d . 1.00 . C(10) 0.6505(6) -0.1021(2) 0.8548(4) 0.042(1) Uani d . 1.00 . C(11) 0.8224(8) -0.1133(3) 0.9414(6) 0.059(2) Uani d . 1.00 . C(12) 0.5466(9) -0.1815(3) 0.8375(7) 0.069(2) Uani d . 1.00 . C(14) 0.8004(7) 0.0063(4) 0.2512(5) 0.054(2) Uani d . 1.00 . H(1) 0.748(5) -0.103(2) 0.421(4) 0.04(1) Uiso calc . 1.00 . H(2) 0.693(5) -0.164(2) 0.621(4) 0.05(1) Uiso calc . 1.00 . H(3) 0.576(5) -0.069(2) 0.897(3) 0.04(1) Uiso calc . 1.00 . H(4) 0.788(5) -0.138(2) 1.020(4) 0.06(1) Uiso calc . 1.00 . H(5) 0.880(6) -0.064(2) 0.955(4) 0.06(1) Uiso calc . 1.00 . H(6) 0.894(6) -0.149(3) 0.887(5) 0.09(2) Uiso calc . 1.00 . H(7) 0.510(6) -0.198(3) 0.919(5) 0.08(2) Uiso calc . 1.00 . H(8) 0.428(7) -0.178(3) 0.782(6) 0.11(2) Uiso calc . 1.00 . H(9) 0.618(6) -0.220(2) 0.803(4) 0.06(1) Uiso calc . 1.00 . H(10) 0.682(6) -0.026(2) 0.229(4) 0.06(1) Uiso calc . 1.00 . H(11) 0.884(5) -0.029(2) 0.262(4) 0.04(1) Uiso calc . 1.00 . H(12) 0.809(6) 0.047(3) 0.189(5) 0.08(2) 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 Te(3) 0.0589(2) 0.0320(1) 0.0433(2) -0.0094(1) 0.0062(1) 0.0040(1) Se(1) 0.0541(3) 0.0370(2) 0.0284(2) 0.0048(2) -0.0005(2) -0.0043(2) Se(2) 0.0537(3) 0.0313(2) 0.0486(3) 0.0043(2) 0.0045(2) -0.0049(2) O(13) 0.060(2) 0.057(2) 0.025(2) -0.008(1) 0.007(1) 0.001(1) C(4) 0.030(2) 0.045(2) 0.030(2) -0.001(2) 0.005(2) -0.003(2) C(5) 0.048(3) 0.040(2) 0.041(3) 0.000(2) 0.006(2) -0.016(2) C(6) 0.049(3) 0.030(2) 0.043(3) -0.001(2) 0.005(2) -0.005(2) C(7) 0.032(2) 0.030(2) 0.035(2) 0.000(2) 0.005(2) 0.001(2) C(8) 0.028(2) 0.031(2) 0.027(2) -0.003(1) -0.001(2) 0.000(2) C(9) 0.024(2) 0.035(2) 0.029(2) 0.003(1) 0.000(2) -0.005(2) C(10) 0.050(3) 0.037(2) 0.039(3) 0.002(2) 0.012(2) 0.000(2) C(11) 0.074(4) 0.051(3) 0.052(4) 0.005(3) 0.000(3) 0.016(3) C(12) 0.088(5) 0.050(3) 0.070(4) -0.019(3) 0.024(4) 0.012(3) C(14) 0.050(3) 0.082(4) 0.030(3) 0.006(3) 0.006(2) -0.005(3) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method ; Zachariasen(1967) type 2 Gaussian isotropic ; _refine_ls_extinction_coef 0.0084(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2192 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.03304 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.03929 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.874 _refine_ls_shift/esd_max 0.0200 _refine_ls_shift/esd_mean 0.0008 _refine_diff_density_min -0.65 _refine_diff_density_max 0.53 #------------------------------------------------------------------------------ _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 Te(3) Se(2) 2.5233(6) 1_555 1_555 yes Te(3) C(8) 2.113(3) 1_555 1_555 yes Se(1) Se(2) 2.3500(6) 1_555 1_555 yes Se(1) C(9) 1.929(3) 1_555 1_555 yes O(13) C(4) 1.363(4) 1_555 1_555 yes O(13) C(14) 1.420(5) 1_555 1_555 yes C(4) C(5) 1.383(5) 1_555 1_555 yes C(4) C(8) 1.387(5) 1_555 1_555 yes C(5) C(6) 1.379(6) 1_555 1_555 yes C(5) H(1) 0.88(4) 1_555 1_555 no C(6) C(7) 1.374(5) 1_555 1_555 yes C(6) H(2) 0.96(4) 1_555 1_555 no C(7) C(9) 1.413(4) 1_555 1_555 yes C(7) C(10) 1.515(5) 1_555 1_555 yes C(8) C(9) 1.388(5) 1_555 1_555 yes C(10) C(11) 1.517(6) 1_555 1_555 yes C(10) C(12) 1.530(6) 1_555 1_555 yes C(10) H(3) 0.90(3) 1_555 1_555 no C(11) H(4) 0.95(4) 1_555 1_555 no C(11) H(5) 0.93(4) 1_555 1_555 no C(11) H(6) 0.98(5) 1_555 1_555 no C(12) H(7) 0.92(5) 1_555 1_555 no C(12) H(8) 1.02(5) 1_555 1_555 no C(12) H(9) 0.91(4) 1_555 1_555 no C(14) H(10) 1.04(4) 1_555 1_555 no C(14) H(11) 0.85(4) 1_555 1_555 no C(14) H(12) 0.93(5) 1_555 1_555 no #------------------------------------------------------------------------------ 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 Se(2) Te(3) C(8) 88.43(9) 1_555 1_555 1_555 yes Se(2) Se(1) C(9) 96.1(1) 1_555 1_555 1_555 yes Te(3) Se(2) Se(1) 90.52(2) 1_555 1_555 1_555 yes C(4) O(13) C(14) 117.8(4) 1_555 1_555 1_555 yes O(13) C(4) C(5) 125.4(4) 1_555 1_555 1_555 yes O(13) C(4) C(8) 115.7(3) 1_555 1_555 1_555 yes C(5) C(4) C(8) 118.8(4) 1_555 1_555 1_555 yes C(4) C(5) C(6) 119.5(4) 1_555 1_555 1_555 yes C(4) C(5) H(1) 120(2) 1_555 1_555 1_555 no C(6) C(5) H(1) 120(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 123.6(4) 1_555 1_555 1_555 yes C(5) C(6) H(2) 120(2) 1_555 1_555 1_555 no C(7) C(6) H(2) 115(2) 1_555 1_555 1_555 no C(6) C(7) C(9) 116.5(3) 1_555 1_555 1_555 yes C(6) C(7) C(10) 122.1(3) 1_555 1_555 1_555 yes C(9) C(7) C(10) 121.3(3) 1_555 1_555 1_555 yes Te(3) C(8) C(4) 116.8(3) 1_555 1_555 1_555 yes Te(3) C(8) C(9) 122.2(3) 1_555 1_555 1_555 yes C(4) C(8) C(9) 121.1(3) 1_555 1_555 1_555 yes Se(1) C(9) C(7) 120.0(3) 1_555 1_555 1_555 yes Se(1) C(9) C(8) 119.4(3) 1_555 1_555 1_555 yes C(7) C(9) C(8) 120.5(3) 1_555 1_555 1_555 yes C(7) C(10) C(11) 112.2(4) 1_555 1_555 1_555 yes C(7) C(10) C(12) 112.5(4) 1_555 1_555 1_555 yes C(7) C(10) H(3) 107(2) 1_555 1_555 1_555 no C(11) C(10) C(12) 111.1(4) 1_555 1_555 1_555 yes C(11) C(10) H(3) 108(2) 1_555 1_555 1_555 no C(12) C(10) H(3) 104(2) 1_555 1_555 1_555 no C(10) C(11) H(4) 106(2) 1_555 1_555 1_555 no C(10) C(11) H(5) 109(2) 1_555 1_555 1_555 no C(10) C(11) H(6) 101(2) 1_555 1_555 1_555 no H(4) C(11) H(5) 113(3) 1_555 1_555 1_555 no H(4) C(11) H(6) 113(3) 1_555 1_555 1_555 no H(5) C(11) H(6) 110(3) 1_555 1_555 1_555 no C(10) C(12) H(7) 108(2) 1_555 1_555 1_555 no C(10) C(12) H(8) 115(2) 1_555 1_555 1_555 no C(10) C(12) H(9) 110(2) 1_555 1_555 1_555 no H(7) C(12) H(8) 102(4) 1_555 1_555 1_555 no H(7) C(12) H(9) 110(3) 1_555 1_555 1_555 no H(8) C(12) H(9) 109(4) 1_555 1_555 1_555 no O(13) C(14) H(10) 112(2) 1_555 1_555 1_555 no O(13) C(14) H(11) 108(2) 1_555 1_555 1_555 no O(13) C(14) H(12) 101(3) 1_555 1_555 1_555 no H(10) C(14) H(11) 105(3) 1_555 1_555 1_555 no H(10) C(14) H(12) 108(3) 1_555 1_555 1_555 no H(11) C(14) H(12) 120(4) 1_555 1_555 1_555 no #------------------------------------------------------------------------------