Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wieland Tyrra' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat zu Koln Greinstr. 6 Koln D-50939 GERMANY ; _publ_contact_author_email TYRRA@UNI-KOELN.DE _publ_section_title ; Perfluoroalkyl(dithiocarbamato) tellurium(II) compounds ; loop_ _publ_author_name 'Wieland Tyrra' 'Sigrid Buslei' 'Silke Kremer' 'Dieter Naumann' 'Ingo Pantenburg' 'Harald Scherer' data_ipwt095 _database_code_depnum_ccdc_archive 'CCDC 614394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Cs O10, C11 H16 F3 N2 S4 Te' _chemical_formula_sum 'C31 H56 Cs F3 N2 O10 S4 Te' _chemical_formula_weight 1062.53 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Te Te -0.5308 1.6751 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1917(13) _cell_length_b 13.1781(14) _cell_length_c 14.9388(15) _cell_angle_alpha 87.971(8) _cell_angle_beta 78.721(8) _cell_angle_gamma 61.217(7) _cell_volume 2226.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 28505 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.24 _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4023 _exptl_absorpt_correction_T_max 0.7632 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 34762 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.24 _reflns_number_total 9754 _reflns_number_gt 7375 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1185P)^2^+6.1575P] 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 SHELXL _refine_ls_extinction_coef 0.0060(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9754 _refine_ls_number_parameters 471 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2030 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 Te1 Te 0.06901(4) 0.73714(4) 0.30391(3) 0.04165(16) Uani 1 1 d . . . C1 C 0.0299(7) 0.7477(7) 0.4579(5) 0.0528(17) Uani 1 1 d . . . F11 F 0.1014(12) 0.6593(7) 0.4935(4) 0.197(7) Uani 1 1 d . . . F12 F -0.0721(9) 0.7739(15) 0.4961(4) 0.206(7) Uani 1 1 d . . . F13 F 0.0497(10) 0.8247(9) 0.4965(4) 0.132(3) Uani 1 1 d . . . S11 S 0.03646(18) 0.87912(15) 0.13807(11) 0.0500(4) Uani 1 1 d . . . S12 S -0.04941(17) 0.96993(15) 0.33451(11) 0.0474(4) Uani 1 1 d . . . C11 C -0.0362(6) 0.9918(6) 0.2191(5) 0.0438(14) Uani 1 1 d . . . N12 N -0.0852(6) 1.1007(5) 0.1939(4) 0.0520(15) Uani 1 1 d . . . C13 C -0.0827(10) 1.1315(7) 0.0980(5) 0.070(3) Uani 1 1 d . . . H13A H -0.1166 1.0958 0.0666 0.161(9) Uiso 1 1 calc R . . H13B H -0.0026 1.1074 0.0654 0.161(9) Uiso 1 1 calc R . . C14 C -0.1561(18) 1.2607(8) 0.1056(8) 0.136(7) Uani 1 1 d . . . H14A H -0.1149 1.2943 0.0652 0.161(9) Uiso 1 1 calc R . . H14B H -0.2303 1.2829 0.0873 0.161(9) Uiso 1 1 calc R . . C15 C -0.1776(18) 1.3015(8) 0.1945(8) 0.137(7) Uani 1 1 d . . . H15A H -0.2600 1.3599 0.2128 0.161(9) Uiso 1 1 calc R . . H15B H -0.1297 1.3379 0.1985 0.161(9) Uiso 1 1 calc R . . C16 C -0.1498(8) 1.2054(6) 0.2581(5) 0.060(2) Uani 1 1 d . . . H16A H -0.1008 1.2069 0.2982 0.161(9) Uiso 1 1 calc R . . H16B H -0.2213 1.2099 0.2949 0.161(9) Uiso 1 1 calc R . . S21 S 0.18641(18) 0.57066(15) 0.13018(12) 0.0496(4) Uani 1 1 d . . . S22 S 0.17484(18) 0.50654(15) 0.32544(12) 0.0500(4) Uani 1 1 d . . . C21 C 0.2188(6) 0.4690(6) 0.2092(5) 0.0454(15) Uani 1 1 d . . . N22 N 0.2808(6) 0.3562(5) 0.1823(4) 0.0479(13) Uani 1 1 d . . . C23 C 0.3163(8) 0.2619(6) 0.2446(6) 0.060(2) Uani 1 1 d . . . H23A H 0.2485 0.2571 0.2791 0.161(9) Uiso 1 1 calc R . . H23B H 0.3589 0.2716 0.2867 0.161(9) Uiso 1 1 calc R . . C24 C 0.3949(18) 0.1576(9) 0.1792(8) 0.146(8) Uani 1 1 d . . . H24A H 0.4767 0.1319 0.1813 0.161(9) Uiso 1 1 calc R . . H24B H 0.3781 0.0951 0.1978 0.161(9) Uiso 1 1 calc R . . C25 C 0.3791(17) 0.1811(9) 0.0937(8) 0.132(7) Uani 1 1 d . . . H25A H 0.3293 0.1519 0.0783 0.161(9) Uiso 1 1 calc R . . H25B H 0.4547 0.1434 0.0512 0.161(9) Uiso 1 1 calc R . . C26 C 0.3214(10) 0.3112(7) 0.0860(5) 0.068(2) Uani 1 1 d . . . H26A H 0.3777 0.3340 0.0536 0.161(9) Uiso 1 1 calc R . . H26B H 0.2557 0.3380 0.0551 0.161(9) Uiso 1 1 calc R . . Cs1 Cs 0.57323(4) 0.74404(5) 0.26515(4) 0.05934(19) Uani 1 1 d . . . O101 O 0.5284(7) 0.5438(6) 0.1996(5) 0.084(2) Uani 1 1 d D . . C102 C 0.4629(13) 0.5101(10) 0.2608(7) 0.108(5) Uani 1 1 d D . . H10A H 0.4690 0.4400 0.2358 0.161(9) Uiso 1 1 calc R . . H10B H 0.3808 0.5698 0.2698 0.161(9) Uiso 1 1 calc R . . C103 C 0.4981(9) 0.4878(8) 0.3500(6) 0.068(2) Uani 1 1 d D . . H10C H 0.5812 0.4307 0.3410 0.161(9) Uiso 1 1 calc R . . H10D H 0.4534 0.4558 0.3880 0.161(9) Uiso 1 1 calc R . . O104 O 0.4783(7) 0.5936(7) 0.3975(5) 0.089(2) Uani 1 1 d D . . C105 C 0.3669(10) 0.6555(11) 0.4481(7) 0.096(4) Uani 1 1 d D . . H10E H 0.3529 0.6089 0.4955 0.161(9) Uiso 1 1 calc R . . H10F H 0.3101 0.6746 0.4092 0.161(9) Uiso 1 1 calc R . . C106 C 0.3504(10) 0.7634(9) 0.4904(5) 0.074(3) Uani 1 1 d D . . H10G H 0.4132 0.7439 0.5234 0.161(9) Uiso 1 1 calc R . . H10H H 0.2762 0.7983 0.5346 0.161(9) Uiso 1 1 calc R . . O107 O 0.3499(6) 0.8504(7) 0.4240(5) 0.084(2) Uani 1 1 d D . . C108 C 0.2381(9) 0.9161(10) 0.4036(7) 0.085(3) Uani 1 1 d D . . H10I H 0.1797 0.9563 0.4586 0.161(9) Uiso 1 1 calc R . . H10J H 0.2153 0.8668 0.3758 0.161(9) Uiso 1 1 calc R . . C109 C 0.2480(9) 1.0010(8) 0.3381(6) 0.069(2) Uani 1 1 d D . . H10K H 0.1693 1.0575 0.3304 0.161(9) Uiso 1 1 calc R . . H10L H 0.2803 1.0423 0.3648 0.161(9) Uiso 1 1 calc R . . O110 O 0.3200(7) 0.9503(6) 0.2500(5) 0.0789(18) Uani 1 1 d D . . C111 C 0.2597(12) 0.9300(9) 0.1916(7) 0.094(4) Uani 1 1 d D . . H11A H 0.1922 1.0025 0.1828 0.161(9) Uiso 1 1 calc R . . H11B H 0.2311 0.8781 0.2186 0.161(9) Uiso 1 1 calc R . . C112 C 0.3415(8) 0.8767(7) 0.1013(5) 0.062(2) Uani 1 1 d D . . H11C H 0.2962 0.8747 0.0581 0.161(9) Uiso 1 1 calc R . . H11D H 0.3759 0.9255 0.0781 0.161(9) Uiso 1 1 calc R . . O113 O 0.4339(6) 0.7625(7) 0.1062(4) 0.0794(19) Uani 1 1 d D . . C114 C 0.3993(12) 0.6785(9) 0.1014(7) 0.094(4) Uani 1 1 d D . . H11E H 0.3761 0.6798 0.0434 0.161(9) Uiso 1 1 calc R . . H11F H 0.3319 0.6950 0.1502 0.161(9) Uiso 1 1 calc R . . C115 C 0.5005(9) 0.5602(7) 0.1102(5) 0.063(2) Uani 1 1 d D . . H11G H 0.4808 0.5015 0.0956 0.161(9) Uiso 1 1 calc R . . H11H H 0.5700 0.5488 0.0658 0.161(9) Uiso 1 1 calc R . . O201 O 0.6922(15) 0.6831(19) 0.4317(10) 0.256(13) Uani 1 1 d D . . C202 C 0.8131(14) 0.6172(16) 0.4206(14) 0.172(11) Uani 1 1 d D . . H20A H 0.8364 0.5919 0.4786 0.161(9) Uiso 1 1 calc R . . H20B H 0.8526 0.6595 0.3921 0.161(9) Uiso 1 1 calc R . . C203 C 0.8385(19) 0.5168(18) 0.3589(10) 0.164(11) Uani 1 1 d D . . H20C H 0.7886 0.4841 0.3863 0.161(9) Uiso 1 1 calc R . . H20D H 0.9199 0.4574 0.3556 0.161(9) Uiso 1 1 calc R . . O204 O 0.8196(10) 0.5455(10) 0.2630(12) 0.189(8) Uani 1 1 d D . . C205 C 0.9060(17) 0.5410(10) 0.2080(9) 0.186(12) Uani 1 1 d D . . H20E H 0.9726 0.4638 0.2067 0.161(9) Uiso 1 1 calc R . . H20F H 0.9264 0.5952 0.2311 0.161(9) Uiso 1 1 calc R . . C206 C 0.8898(8) 0.5674(7) 0.1115(6) 0.061(2) Uani 1 1 d D . . H20G H 0.9615 0.5161 0.0685 0.161(9) Uiso 1 1 calc R . . H20H H 0.8258 0.5564 0.0999 0.161(9) Uiso 1 1 calc R . . O207 O 0.8620(17) 0.6900(14) 0.1011(8) 0.261(13) Uani 1 1 d D . . C208 C 0.7599(11) 0.7575(15) 0.1110(7) 0.133(8) Uani 1 1 d D . . H20I H 0.7183 0.7522 0.1707 0.161(9) Uiso 1 1 calc R . . H20J H 0.7267 0.7411 0.0646 0.161(9) Uiso 1 1 calc R . . C209 C 0.7468(10) 0.8820(9) 0.1025(7) 0.075(3) Uani 1 1 d D . . H20K H 0.8224 0.8769 0.0757 0.161(9) Uiso 1 1 calc R . . H20L H 0.6911 0.9261 0.0639 0.161(9) Uiso 1 1 calc R . . O210 O 0.7036(14) 0.9386(10) 0.1959(9) 0.254(12) Uani 1 1 d D . . C211 C 0.6264(12) 0.9449(11) 0.2621(8) 0.095(3) Uani 1 1 d D . . H21A H 0.6388 0.8664 0.2683 0.161(9) Uiso 1 1 calc R . . H21B H 0.5516 0.9887 0.2427 0.161(9) Uiso 1 1 calc R . . C212 C 0.6077(12) 0.9903(17) 0.3517(11) 0.170(11) Uani 1 1 d D . . H21C H 0.5247 1.0206 0.3791 0.161(9) Uiso 1 1 calc R . . H21D H 0.6226 1.0558 0.3465 0.161(9) Uiso 1 1 calc R . . O213 O 0.6766(18) 0.9136(17) 0.4162(13) 0.244(10) Uani 1 1 d D . . C214 C 0.6158(14) 0.8564(17) 0.4310(14) 0.33(3) Uani 1 1 d D . . H21E H 0.6178 0.8204 0.3747 0.161(9) Uiso 1 1 calc R . . H21F H 0.5343 0.9066 0.4610 0.161(9) Uiso 1 1 calc R . . C215 C 0.6808(14) 0.7699(17) 0.4912(8) 0.128(7) Uani 1 1 d D . . H21G H 0.7554 0.7656 0.4949 0.161(9) Uiso 1 1 calc R . . H21H H 0.6342 0.7761 0.5518 0.161(9) 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 Te1 0.0487(3) 0.0396(2) 0.0315(2) 0.00238(15) -0.00820(17) -0.01738(19) C1 0.060(4) 0.053(4) 0.032(3) 0.003(3) -0.004(3) -0.019(4) F11 0.287(14) 0.094(5) 0.036(3) 0.014(3) -0.021(5) 0.037(7) F12 0.154(8) 0.51(2) 0.037(3) -0.007(7) 0.002(4) -0.231(13) F13 0.220(10) 0.194(9) 0.044(3) -0.002(4) -0.018(4) -0.152(8) S11 0.0659(11) 0.0388(8) 0.0316(8) -0.0004(6) -0.0072(7) -0.0154(8) S12 0.0599(10) 0.0413(8) 0.0303(7) -0.0001(6) -0.0059(7) -0.0174(8) C11 0.048(4) 0.040(3) 0.036(3) 0.001(2) -0.006(3) -0.017(3) N12 0.067(4) 0.038(3) 0.035(3) 0.002(2) 0.000(3) -0.016(3) C13 0.097(7) 0.044(4) 0.041(4) 0.009(3) -0.005(4) -0.017(4) C14 0.236(19) 0.039(5) 0.061(6) 0.012(4) -0.009(9) -0.019(8) C15 0.242(19) 0.037(5) 0.062(6) 0.008(4) 0.006(9) -0.026(7) C16 0.082(6) 0.034(3) 0.042(4) 0.000(3) 0.002(4) -0.017(4) S21 0.0650(11) 0.0393(8) 0.0369(8) 0.0059(6) -0.0116(7) -0.0191(8) S22 0.0658(11) 0.0425(8) 0.0358(8) 0.0052(6) -0.0105(8) -0.0217(8) C21 0.051(4) 0.043(3) 0.040(3) 0.005(3) -0.012(3) -0.020(3) N22 0.063(4) 0.034(3) 0.040(3) 0.003(2) -0.010(3) -0.019(3) C23 0.076(5) 0.037(4) 0.055(4) 0.009(3) -0.012(4) -0.020(4) C24 0.24(2) 0.036(5) 0.073(7) 0.003(5) 0.002(10) -0.011(8) C25 0.223(18) 0.041(5) 0.061(6) -0.005(4) -0.010(8) -0.015(7) C26 0.099(7) 0.042(4) 0.042(4) -0.003(3) -0.002(4) -0.022(4) Cs1 0.0521(3) 0.0760(4) 0.0530(3) -0.0104(2) -0.0061(2) -0.0341(3) O101 0.087(5) 0.070(4) 0.080(5) -0.004(3) -0.008(4) -0.028(4) C102 0.159(13) 0.067(6) 0.066(6) 0.002(5) 0.010(7) -0.041(8) C103 0.084(6) 0.060(5) 0.064(5) 0.012(4) -0.032(5) -0.031(5) O104 0.086(5) 0.105(6) 0.081(5) 0.026(4) -0.036(4) -0.045(5) C105 0.093(8) 0.123(10) 0.058(6) 0.030(6) -0.020(6) -0.041(8) C106 0.101(7) 0.087(6) 0.034(4) -0.001(4) -0.007(4) -0.048(6) O107 0.076(4) 0.103(5) 0.070(4) -0.029(4) 0.002(3) -0.045(4) C108 0.069(6) 0.094(8) 0.071(6) -0.017(5) -0.003(5) -0.026(6) C109 0.072(6) 0.059(5) 0.065(5) -0.018(4) 0.005(4) -0.029(4) O110 0.085(5) 0.072(4) 0.084(5) 0.003(3) -0.019(4) -0.039(4) C111 0.139(11) 0.064(6) 0.073(7) 0.004(5) -0.031(7) -0.040(7) C112 0.078(6) 0.053(4) 0.046(4) 0.008(3) -0.013(4) -0.026(4) O113 0.089(5) 0.100(5) 0.053(4) -0.007(3) -0.002(3) -0.053(4) C114 0.150(12) 0.089(7) 0.055(5) 0.002(5) -0.016(6) -0.069(8) C115 0.081(6) 0.056(4) 0.046(4) -0.008(3) -0.016(4) -0.026(4) O201 0.28(2) 0.55(4) 0.120(11) 0.095(17) -0.098(13) -0.33(3) C202 0.135(14) 0.24(2) 0.22(2) 0.17(2) -0.105(16) -0.136(17) C203 0.27(2) 0.26(2) 0.135(13) 0.156(16) -0.165(17) -0.23(2) O204 0.089(7) 0.089(7) 0.38(3) 0.005(11) -0.043(11) -0.037(6) C205 0.26(2) 0.048(6) 0.124(12) -0.028(7) 0.109(15) -0.029(10) C206 0.062(5) 0.051(4) 0.052(4) -0.007(3) -0.001(4) -0.018(4) O207 0.29(2) 0.28(2) 0.053(6) -0.012(9) -0.046(11) -0.009(19) C208 0.099(9) 0.33(3) 0.037(5) 0.004(9) -0.007(6) -0.153(14) C209 0.094(7) 0.074(6) 0.075(6) 0.025(5) -0.035(6) -0.050(6) O210 0.219(15) 0.100(8) 0.216(15) 0.085(9) 0.121(13) 0.034(9) C211 0.102(9) 0.086(8) 0.104(9) 0.006(7) -0.026(7) -0.049(7) C212 0.067(7) 0.219(19) 0.143(14) -0.138(15) -0.047(9) 0.013(10) O213 0.27(2) 0.28(2) 0.21(2) -0.098(18) 0.004(17) -0.16(2) C214 0.085(11) 0.45(5) 0.45(5) -0.40(5) 0.08(2) -0.14(2) C215 0.104(10) 0.27(2) 0.052(6) -0.011(9) -0.015(6) -0.125(14) _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 Te1 C1 2.252(7) . ? Te1 S12 2.6955(18) . ? Te1 S22 2.7034(18) . ? C1 F12 1.234(11) . ? C1 F11 1.274(10) . ? C1 F13 1.336(11) . ? S11 C11 1.700(7) . ? S12 C11 1.727(7) . ? C11 N12 1.336(9) . ? N12 C13 1.474(10) . ? N12 C16 1.481(9) . ? C13 C14 1.494(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.375(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.499(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? S21 C21 1.705(7) . ? S22 C21 1.729(7) . ? C21 N22 1.335(9) . ? N22 C23 1.469(9) . ? N22 C26 1.469(9) . ? C23 C24 1.498(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.336(18) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.515(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? Cs1 O204 3.031(11) . ? Cs1 C211 3.044(12) . ? Cs1 O201 3.077(14) . ? Cs1 C208 3.094(10) . ? Cs1 O107 3.131(7) . ? Cs1 O110 3.180(7) . ? Cs1 O101 3.191(8) . ? Cs1 O113 3.211(7) . ? Cs1 C214 3.202(14) . ? Cs1 O104 3.248(8) . ? Cs1 O210 3.737(16) . ? Cs1 C205 3.813(18) . ? O101 C102 1.346(12) . ? O101 C115 1.436(10) . ? C102 C103 1.470(13) . ? C102 H10A 0.9700 . ? C102 H10B 0.9700 . ? C103 O104 1.470(10) . ? C103 H10C 0.9700 . ? C103 H10D 0.9700 . ? O104 C105 1.360(12) . ? C105 C106 1.477(13) . ? C105 H10E 0.9700 . ? C105 H10F 0.9700 . ? C106 O107 1.488(11) . ? C106 H10G 0.9700 . ? C106 H10H 0.9700 . ? O107 C108 1.394(11) . ? C108 C109 1.497(13) . ? C108 H10I 0.9700 . ? C108 H10J 0.9700 . ? C109 O110 1.429(10) . ? C109 H10K 0.9700 . ? C109 H10L 0.9700 . ? O110 C111 1.399(12) . ? C111 C112 1.499(12) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 O113 1.420(10) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? O113 C114 1.395(11) . ? C114 C115 1.510(13) . ? C114 H11E 0.9700 . ? C114 H11F 0.9700 . ? C115 H11G 0.9700 . ? C115 H11H 0.9700 . ? O201 C202 1.377(16) . ? O201 C215 1.407(16) . ? C202 C203 1.501(17) . ? C202 C215 2.06(3) . ? C202 H20A 0.9700 . ? C202 H20B 0.9700 . ? C203 O204 1.506(15) . ? C203 H20C 0.9700 . ? C203 H20D 0.9700 . ? O204 C205 1.244(14) . ? C205 C206 1.502(15) . ? C205 H20E 0.9700 . ? C205 H20F 0.9700 . ? C206 O207 1.485(16) . ? C206 H20G 0.9700 . ? C206 H20H 0.9700 . ? O207 C208 1.185(15) . ? C208 C209 1.568(15) . ? C208 H20I 0.9700 . ? C208 H20J 0.9700 . ? C209 O210 1.476(14) . ? C209 H20K 0.9700 . ? C209 H20L 0.9700 . ? O210 C211 1.246(13) . ? C211 C212 1.413(13) . ? C211 H21A 0.9700 . ? C211 H21B 0.9700 . ? C212 O213 1.472(17) . ? C212 H21C 0.9700 . ? C212 H21D 0.9700 . ? O213 C214 1.328(16) . ? C214 C215 1.460(18) . ? C214 H21E 0.9700 . ? C214 H21F 0.9700 . ? C215 H21G 0.9700 . ? C215 H21H 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te1 S12 81.3(2) . . ? C1 Te1 S22 82.5(2) . . ? S12 Te1 S22 163.76(5) . . ? F12 C1 F11 108.9(10) . . ? F12 C1 F13 103.4(9) . . ? F11 C1 F13 96.3(10) . . ? F12 C1 Te1 116.7(6) . . ? F11 C1 Te1 114.8(5) . . ? F13 C1 Te1 114.4(5) . . ? C11 S12 Te1 92.7(2) . . ? N12 C11 S11 119.8(5) . . ? N12 C11 S12 118.3(5) . . ? S11 C11 S12 121.8(4) . . ? C11 N12 C13 123.9(6) . . ? C11 N12 C16 124.7(6) . . ? C13 N12 C16 111.5(6) . . ? N12 C13 C14 103.7(7) . . ? N12 C13 H13A 111.0 . . ? C14 C13 H13A 111.0 . . ? N12 C13 H13B 111.0 . . ? C14 C13 H13B 111.0 . . ? H13A C13 H13B 109.0 . . ? C15 C14 C13 109.4(9) . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C14 C15 C16 111.2(8) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N12 C16 C15 102.3(7) . . ? N12 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? N12 C16 H16B 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? C21 S22 Te1 93.9(2) . . ? N22 C21 S21 120.2(5) . . ? N22 C21 S22 117.7(5) . . ? S21 C21 S22 122.0(4) . . ? C21 N22 C23 124.5(6) . . ? C21 N22 C26 123.9(6) . . ? C23 N22 C26 111.6(6) . . ? N22 C23 C24 101.8(7) . . ? N22 C23 H23A 111.4 . . ? C24 C23 H23A 111.4 . . ? N22 C23 H23B 111.4 . . ? C24 C23 H23B 111.4 . . ? H23A C23 H23B 109.3 . . ? C25 C24 C23 111.4(10) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 109.2(9) . . ? C24 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? C24 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? N22 C26 C25 102.5(7) . . ? N22 C26 H26A 111.3 . . ? C25 C26 H26A 111.3 . . ? N22 C26 H26B 111.3 . . ? C25 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? O204 Cs1 C211 98.8(3) . . ? O204 Cs1 O201 55.9(5) . . ? C211 Cs1 O201 83.0(4) . . ? O204 Cs1 C208 67.9(4) . . ? C211 Cs1 C208 58.3(4) . . ? O201 Cs1 C208 103.7(3) . . ? O204 Cs1 O107 130.1(4) . . ? C211 Cs1 O107 97.1(3) . . ? O201 Cs1 O107 79.8(3) . . ? C208 Cs1 O107 153.8(3) . . ? O204 Cs1 O110 175.4(4) . . ? C211 Cs1 O110 81.1(3) . . ? O201 Cs1 O110 128.5(4) . . ? C208 Cs1 O110 108.5(3) . . ? O107 Cs1 O110 54.3(2) . . ? O204 Cs1 O101 83.5(3) . . ? C211 Cs1 O101 161.6(3) . . ? O201 Cs1 O101 112.8(4) . . ? C208 Cs1 O101 106.7(3) . . ? O107 Cs1 O101 95.25(19) . . ? O110 Cs1 O101 95.15(19) . . ? O204 Cs1 O113 121.7(3) . . ? C211 Cs1 O113 109.9(3) . . ? O201 Cs1 O113 167.0(3) . . ? C208 Cs1 O113 85.6(2) . . ? O107 Cs1 O113 95.97(18) . . ? O110 Cs1 O113 54.38(18) . . ? O101 Cs1 O113 55.01(19) . . ? O204 Cs1 C214 85.1(4) . . ? C211 Cs1 C214 52.2(5) . . ? O201 Cs1 C214 37.2(5) . . ? C208 Cs1 C214 98.3(4) . . ? O107 Cs1 C214 68.6(3) . . ? O110 Cs1 C214 98.3(4) . . ? O101 Cs1 C214 146.1(4) . . ? O113 Cs1 C214 151.7(4) . . ? O204 Cs1 O104 86.4(3) . . ? C211 Cs1 O104 144.1(3) . . ? O201 Cs1 O104 70.7(3) . . ? C208 Cs1 O104 150.6(4) . . ? O107 Cs1 O104 55.4(2) . . ? O110 Cs1 O104 96.30(19) . . ? O101 Cs1 O104 54.04(19) . . ? O113 Cs1 O104 96.68(18) . . ? C214 Cs1 O104 93.5(4) . . ? O204 Cs1 O210 89.1(3) . . ? C211 Cs1 O210 17.7(3) . . ? O201 Cs1 O210 89.5(4) . . ? C208 Cs1 O210 40.7(3) . . ? O107 Cs1 O210 114.5(2) . . ? O110 Cs1 O210 89.7(3) . . ? O101 Cs1 O210 146.0(3) . . ? O113 Cs1 O210 103.5(3) . . ? C214 Cs1 O210 65.3(5) . . ? O104 Cs1 O210 158.6(3) . . ? O204 Cs1 C205 16.4(3) . . ? C211 Cs1 C205 87.6(4) . . ? O201 Cs1 C205 65.5(4) . . ? C208 Cs1 C205 51.6(3) . . ? O107 Cs1 C205 144.3(3) . . ? O110 Cs1 C205 160.0(2) . . ? O101 Cs1 C205 90.4(3) . . ? O113 Cs1 C205 115.8(3) . . ? C214 Cs1 C205 87.4(4) . . ? O104 Cs1 C205 102.5(2) . . ? O210 Cs1 C205 75.3(3) . . ? C102 O101 C115 115.2(9) . . ? C102 O101 Cs1 117.8(7) . . ? C115 O101 Cs1 111.8(5) . . ? O101 C102 C103 113.7(12) . . ? O101 C102 H10A 108.8 . . ? C103 C102 H10A 108.8 . . ? O101 C102 H10B 108.8 . . ? C103 C102 H10B 108.8 . . ? H10A C102 H10B 107.7 . . ? C102 C103 O104 112.2(8) . . ? C102 C103 H10C 109.2 . . ? O104 C103 H10C 109.2 . . ? C102 C103 H10D 109.2 . . ? O104 C103 H10D 109.2 . . ? H10C C103 H10D 107.9 . . ? C105 O104 C103 113.1(9) . . ? C105 O104 Cs1 115.2(7) . . ? C103 O104 Cs1 112.8(6) . . ? O104 C105 C106 110.7(10) . . ? O104 C105 H10E 109.5 . . ? C106 C105 H10E 109.5 . . ? O104 C105 H10F 109.5 . . ? C106 C105 H10F 109.5 . . ? H10E C105 H10F 108.1 . . ? C105 C106 O107 114.1(7) . . ? C105 C106 H10G 108.7 . . ? O107 C106 H10G 108.7 . . ? C105 C106 H10H 108.7 . . ? O107 C106 H10H 108.7 . . ? H10G C106 H10H 107.6 . . ? C108 O107 C106 110.7(8) . . ? C108 O107 Cs1 119.7(6) . . ? C106 O107 Cs1 112.0(5) . . ? O107 C108 C109 105.8(9) . . ? O107 C108 H10I 110.6 . . ? C109 C108 H10I 110.6 . . ? O107 C108 H10J 110.6 . . ? C109 C108 H10J 110.6 . . ? H10I C108 H10J 108.7 . . ? O110 C109 C108 114.6(7) . . ? O110 C109 H10K 108.6 . . ? C108 C109 H10K 108.6 . . ? O110 C109 H10L 108.6 . . ? C108 C109 H10L 108.6 . . ? H10K C109 H10L 107.6 . . ? C111 O110 C109 113.0(8) . . ? C111 O110 Cs1 117.3(6) . . ? C109 O110 Cs1 111.6(6) . . ? O110 C111 C112 109.4(10) . . ? O110 C111 H11A 109.8 . . ? C112 C111 H11A 109.8 . . ? O110 C111 H11B 109.8 . . ? C112 C111 H11B 109.8 . . ? H11A C111 H11B 108.2 . . ? O113 C112 C111 113.3(7) . . ? O113 C112 H11C 108.9 . . ? C111 C112 H11C 108.9 . . ? O113 C112 H11D 108.9 . . ? C111 C112 H11D 108.9 . . ? H11C C112 H11D 107.7 . . ? C114 O113 C112 112.6(8) . . ? C114 O113 Cs1 116.5(6) . . ? C112 O113 Cs1 112.9(5) . . ? O113 C114 C115 109.6(10) . . ? O113 C114 H11E 109.8 . . ? C115 C114 H11E 109.8 . . ? O113 C114 H11F 109.8 . . ? C115 C114 H11F 109.8 . . ? H11E C114 H11F 108.2 . . ? O101 C115 C114 113.7(7) . . ? O101 C115 H11G 108.8 . . ? C114 C115 H11G 108.8 . . ? O101 C115 H11H 108.8 . . ? C114 C115 H11H 108.8 . . ? H11G C115 H11H 107.7 . . ? C202 O201 C215 95.6(14) . . ? C202 O201 Cs1 120.8(11) . . ? C215 O201 Cs1 121.4(12) . . ? O201 C202 C203 101.6(16) . . ? O201 C202 C215 42.7(8) . . ? C203 C202 C215 144.3(14) . . ? O201 C202 H20A 111.4 . . ? C203 C202 H20A 111.4 . . ? C215 C202 H20A 87.1 . . ? O201 C202 H20B 111.4 . . ? C203 C202 H20B 111.4 . . ? C215 C202 H20B 88.8 . . ? H20A C202 H20B 109.3 . . ? C202 C203 O204 115.2(13) . . ? C202 C203 Cs1 83.8(10) . . ? O204 C203 Cs1 47.6(8) . . ? C202 C203 H20C 108.5 . . ? O204 C203 H20C 108.5 . . ? Cs1 C203 H20C 87.2 . . ? C202 C203 H20D 108.5 . . ? O204 C203 H20D 108.5 . . ? Cs1 C203 H20D 155.8 . . ? H20C C203 H20D 107.5 . . ? C205 O204 C203 115.2(15) . . ? C205 O204 Cs1 120.3(11) . . ? C203 O204 Cs1 110.8(11) . . ? O204 C205 C206 116(2) . . ? O204 C205 Cs1 43.3(9) . . ? C206 C205 Cs1 83.0(8) . . ? O204 C205 H20E 108.3 . . ? C206 C205 H20E 108.3 . . ? Cs1 C205 H20E 149.3 . . ? O204 C205 H20F 108.3 . . ? C206 C205 H20F 108.3 . . ? Cs1 C205 H20F 95.2 . . ? H20E C205 H20F 107.4 . . ? O207 C206 C205 107.3(9) . . ? O207 C206 H20G 110.3 . . ? C205 C206 H20G 110.3 . . ? O207 C206 H20H 110.3 . . ? C205 C206 H20H 110.3 . . ? H20G C206 H20H 108.5 . . ? C208 O207 C206 115(2) . . ? O207 C208 C209 107.8(13) . . ? O207 C208 Cs1 122.2(13) . . ? C209 C208 Cs1 114.0(8) . . ? O207 C208 H20I 110.2 . . ? C209 C208 H20I 110.2 . . ? Cs1 C208 H20I 17.8 . . ? O207 C208 H20J 110.2 . . ? C209 C208 H20J 110.2 . . ? Cs1 C208 H20J 91.2 . . ? H20I C208 H20J 108.5 . . ? O210 C209 C208 107.0(9) . . ? O210 C209 H20K 110.3 . . ? C208 C209 H20K 110.3 . . ? O210 C209 H20L 110.3 . . ? C208 C209 H20L 110.3 . . ? H20K C209 H20L 108.6 . . ? C211 O210 C209 133.9(18) . . ? C211 O210 Cs1 47.8(9) . . ? C209 O210 Cs1 89.1(9) . . ? O210 C211 C212 125.9(17) . . ? O210 C211 Cs1 114.5(11) . . ? C212 C211 Cs1 111.1(12) . . ? O210 C211 H21A 105.9 . . ? C212 C211 H21A 105.9 . . ? Cs1 C211 H21A 21.6 . . ? O210 C211 H21B 105.9 . . ? C212 C211 H21B 105.9 . . ? Cs1 C211 H21B 84.7 . . ? H21A C211 H21B 106.2 . . ? C211 C212 O213 119.0(14) . . ? C211 C212 Cs1 48.5(9) . . ? O213 C212 Cs1 89.6(11) . . ? C211 C212 H21C 107.6 . . ? O213 C212 H21C 107.6 . . ? Cs1 C212 H21C 82.6 . . ? C211 C212 H21D 107.6 . . ? O213 C212 H21D 107.6 . . ? Cs1 C212 H21D 156.0 . . ? H21C C212 H21D 107.0 . . ? C214 O213 C212 94.7(19) . . ? O213 C214 C215 100.8(15) . . ? O213 C214 Cs1 121.4(14) . . ? C215 C214 Cs1 112.5(9) . . ? O213 C214 H21E 111.6 . . ? C215 C214 H21E 111.6 . . ? Cs1 C214 H21E 11.2 . . ? O213 C214 H21F 111.6 . . ? C215 C214 H21F 111.6 . . ? Cs1 C214 H21F 99.4 . . ? H21E C214 H21F 109.4 . . ? O201 C215 C214 88.7(11) . . ? O201 C215 C202 41.7(8) . . ? C214 C215 C202 112.7(10) . . ? O201 C215 H21G 113.9 . . ? C214 C215 H21G 113.9 . . ? C202 C215 H21G 73.0 . . ? O201 C215 H21H 113.9 . . ? C214 C215 H21H 113.9 . . ? C202 C215 H21H 125.4 . . ? H21G C215 H21H 111.1 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.113 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.157 # Attachment '3j.cif' data_ipwt100 _database_code_depnum_ccdc_archive 'CCDC 614395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H30 N P2, C11 H16 F3 N2 S4 Te ; _chemical_formula_sum 'C47 H46 F3 N3 P2 S4 Te' _chemical_formula_weight 1027.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall 'P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8596(14) _cell_length_b 14.8867(9) _cell_length_c 19.4238(17) _cell_angle_alpha 90 _cell_angle_beta 91.203(7) _cell_angle_gamma 90 _cell_volume 4584.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27953 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.33 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6679 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 64295 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9021 _reflns_number_gt 5859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0801P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0044(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9021 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 Te1 Te 0.29924(2) -0.14223(2) 0.156827(17) 0.03717(12) Uani 1 1 d . . . C1 C 0.1644(3) -0.1009(4) 0.1427(3) 0.0486(13) Uani 1 1 d . . . F11 F 0.1091(2) -0.1580(3) 0.1688(3) 0.0872(13) Uani 1 1 d . . . F12 F 0.1468(3) -0.0222(3) 0.1731(2) 0.0864(14) Uani 1 1 d . . . F13 F 0.1403(2) -0.0867(3) 0.07612(18) 0.0694(10) Uani 1 1 d . . . C11 C 0.3433(3) -0.1564(3) 0.3246(3) 0.0395(11) Uani 1 1 d . . . S111 S 0.24312(8) -0.15283(8) 0.28742(7) 0.0397(3) Uani 1 1 d . . . S112 S 0.43026(8) -0.17749(10) 0.27821(7) 0.0455(3) Uani 1 1 d . . . N12 N 0.3494(3) -0.1416(3) 0.3929(2) 0.0409(9) Uani 1 1 d . . . C13 C 0.2772(4) -0.1218(4) 0.4367(3) 0.0500(13) Uani 1 1 d . . . H13A H 0.2346 -0.1683 0.4323 0.076(5) Uiso 1 1 calc R . . H13B H 0.2521 -0.0644 0.4245 0.076(5) Uiso 1 1 calc R . . C14 C 0.3145(4) -0.1194(5) 0.5092(3) 0.0602(16) Uani 1 1 d . . . H14A H 0.3110 -0.1779 0.5309 0.076(5) Uiso 1 1 calc R . . H14B H 0.2856 -0.0757 0.5373 0.076(5) Uiso 1 1 calc R . . C15 C 0.4061(4) -0.0923(4) 0.4992(3) 0.0559(15) Uani 1 1 d . . . H15A H 0.4416 -0.1126 0.5374 0.076(5) Uiso 1 1 calc R . . H15B H 0.4115 -0.0277 0.4947 0.076(5) Uiso 1 1 calc R . . C16 C 0.4290(3) -0.1398(4) 0.4325(3) 0.0459(12) Uani 1 1 d . . . H16A H 0.4719 -0.1067 0.4083 0.076(5) Uiso 1 1 calc R . . H16B H 0.4493 -0.2002 0.4417 0.076(5) Uiso 1 1 calc R . . C21 C 0.4125(3) -0.1299(3) 0.0176(3) 0.0396(11) Uani 1 1 d . . . S211 S 0.30518(8) -0.11459(10) 0.02032(7) 0.0462(3) Uani 1 1 d . . . S212 S 0.46921(9) -0.16775(11) 0.08673(7) 0.0520(4) Uani 1 1 d . . . N22 N 0.4510(3) -0.1095(3) -0.0414(2) 0.0400(9) Uani 1 1 d . . . C23 C 0.4070(4) -0.0848(4) -0.1060(3) 0.0519(14) Uani 1 1 d . . . H23A H 0.3726 -0.0317 -0.0998 0.076(5) Uiso 1 1 calc R . . H23B H 0.3714 -0.1336 -0.1224 0.076(5) Uiso 1 1 calc R . . C24 C 0.4780(4) -0.0665(5) -0.1558(3) 0.0609(16) Uani 1 1 d . . . H24A H 0.4632 -0.0883 -0.2015 0.076(5) Uiso 1 1 calc R . . H24B H 0.4896 -0.0026 -0.1585 0.076(5) Uiso 1 1 calc R . . C25 C 0.5530(4) -0.1161(5) -0.1268(3) 0.0621(16) Uani 1 1 d . . . H25A H 0.6051 -0.0874 -0.1401 0.076(5) Uiso 1 1 calc R . . H25B H 0.5532 -0.1779 -0.1427 0.076(5) Uiso 1 1 calc R . . C26 C 0.5430(3) -0.1121(4) -0.0496(3) 0.0466(12) Uani 1 1 d . . . H26A H 0.5673 -0.1647 -0.0275 0.076(5) Uiso 1 1 calc R . . H26B H 0.5695 -0.0586 -0.0305 0.076(5) Uiso 1 1 calc R . . P11 P 0.22293(7) 0.33881(7) 0.26936(6) 0.0308(3) Uani 1 1 d . . . C111 C 0.1837(3) 0.3595(3) 0.3547(2) 0.0328(9) Uani 1 1 d . . . C112 C 0.0980(3) 0.3586(3) 0.3665(3) 0.0386(10) Uani 1 1 d . . . H112 H 0.0598 0.3480 0.3304 0.055(3) Uiso 1 1 calc R . . C113 C 0.0692(3) 0.3738(4) 0.4327(3) 0.0459(12) Uani 1 1 d . . . H113 H 0.0116 0.3729 0.4409 0.055(3) Uiso 1 1 calc R . . C114 C 0.1255(3) 0.3899(4) 0.4861(3) 0.0438(12) Uani 1 1 d . . . H114 H 0.1060 0.4003 0.5302 0.055(3) Uiso 1 1 calc R . . C115 C 0.2113(3) 0.3907(4) 0.4739(3) 0.0435(12) Uani 1 1 d . . . H115 H 0.2494 0.4019 0.5100 0.055(3) Uiso 1 1 calc R . . C116 C 0.2405(3) 0.3751(3) 0.4087(3) 0.0390(11) Uani 1 1 d . . . H116 H 0.2981 0.3751 0.4008 0.055(3) Uiso 1 1 calc R . . C121 C 0.2782(3) 0.4384(3) 0.2446(2) 0.0341(10) Uani 1 1 d . . . C122 C 0.3472(3) 0.4364(3) 0.2010(2) 0.0357(10) Uani 1 1 d . . . H122 H 0.3716 0.3817 0.1898 0.055(3) Uiso 1 1 calc R . . C123 C 0.3795(3) 0.5155(3) 0.1745(3) 0.0416(11) Uani 1 1 d . . . H123 H 0.4258 0.5137 0.1458 0.055(3) Uiso 1 1 calc R . . C124 C 0.3430(3) 0.5972(3) 0.1907(3) 0.0420(12) Uani 1 1 d . . . H124 H 0.3641 0.6500 0.1721 0.055(3) Uiso 1 1 calc R . . C125 C 0.2752(3) 0.6007(3) 0.2343(3) 0.0440(12) Uani 1 1 d . . . H125 H 0.2513 0.6557 0.2455 0.055(3) Uiso 1 1 calc R . . C126 C 0.2428(3) 0.5212(3) 0.2616(3) 0.0389(11) Uani 1 1 d . . . H126 H 0.1975 0.5235 0.2912 0.055(3) Uiso 1 1 calc R . . C131 C 0.2941(3) 0.2448(3) 0.2765(2) 0.0318(10) Uani 1 1 d . . . C132 C 0.3773(3) 0.2537(3) 0.3005(2) 0.0354(10) Uani 1 1 d . . . H132 H 0.3999 0.3104 0.3093 0.055(3) Uiso 1 1 calc R . . C133 C 0.4263(3) 0.1772(3) 0.3112(3) 0.0386(11) Uani 1 1 d . . . H133 H 0.4817 0.1829 0.3271 0.055(3) Uiso 1 1 calc R . . C134 C 0.3933(3) 0.0928(3) 0.2984(3) 0.0374(11) Uani 1 1 d . . . H134 H 0.4264 0.0420 0.3060 0.055(3) Uiso 1 1 calc R . . C135 C 0.3108(3) 0.0838(3) 0.2741(3) 0.0395(11) Uani 1 1 d . . . H135 H 0.2886 0.0270 0.2654 0.055(3) Uiso 1 1 calc R . . C136 C 0.2617(3) 0.1592(3) 0.2627(3) 0.0365(10) Uani 1 1 d . . . H136 H 0.2067 0.1530 0.2459 0.055(3) Uiso 1 1 calc R . . N31 N 0.1470(2) 0.3113(3) 0.2193(2) 0.0337(8) Uani 1 1 d . . . P21 P 0.10496(7) 0.33798(8) 0.14760(6) 0.0325(3) Uani 1 1 d . . . C211 C 0.0558(3) 0.4470(3) 0.1468(2) 0.0375(10) Uani 1 1 d . . . C212 C 0.1005(4) 0.5231(3) 0.1272(3) 0.0477(13) Uani 1 1 d . . . H212 H 0.1551 0.5179 0.1113 0.055(3) Uiso 1 1 calc R . . C213 C 0.0620(5) 0.6074(4) 0.1317(3) 0.0615(16) Uani 1 1 d . . . H213 H 0.0914 0.6587 0.1191 0.055(3) Uiso 1 1 calc R . . C214 C -0.0187(5) 0.6149(4) 0.1544(3) 0.0625(17) Uani 1 1 d . . . H214 H -0.0443 0.6710 0.1560 0.055(3) Uiso 1 1 calc R . . C215 C -0.0630(4) 0.5393(4) 0.1751(3) 0.0574(15) Uani 1 1 d . . . H215 H -0.1174 0.5452 0.1913 0.055(3) Uiso 1 1 calc R . . C216 C -0.0262(3) 0.4558(4) 0.1714(3) 0.0452(12) Uani 1 1 d . . . H216 H -0.0557 0.4052 0.1853 0.055(3) Uiso 1 1 calc R . . C221 C 0.1773(3) 0.3382(3) 0.0775(3) 0.0363(10) Uani 1 1 d . . . C222 C 0.2592(3) 0.3052(3) 0.0882(3) 0.0411(11) Uani 1 1 d . . . H222 H 0.2747 0.2800 0.1304 0.055(3) Uiso 1 1 calc R . . C223 C 0.3177(4) 0.3102(4) 0.0353(3) 0.0485(13) Uani 1 1 d . . . H223 H 0.3727 0.2904 0.0431 0.055(3) Uiso 1 1 calc R . . C224 C 0.2943(4) 0.3441(4) -0.0281(3) 0.0539(14) Uani 1 1 d . . . H224 H 0.3332 0.3472 -0.0631 0.055(3) Uiso 1 1 calc R . . C225 C 0.2125(4) 0.3736(4) -0.0394(3) 0.0571(15) Uani 1 1 d . . . H225 H 0.1962 0.3950 -0.0827 0.055(3) Uiso 1 1 calc R . . C226 C 0.1549(4) 0.3716(4) 0.0129(3) 0.0496(13) Uani 1 1 d . . . H226 H 0.1004 0.3929 0.0047 0.055(3) Uiso 1 1 calc R . . C231 C 0.0240(3) 0.2573(3) 0.1276(2) 0.0354(10) Uani 1 1 d . . . C232 C 0.0221(3) 0.1761(4) 0.1637(3) 0.0452(12) Uani 1 1 d . . . H232 H 0.0612 0.1656 0.1991 0.055(3) Uiso 1 1 calc R . . C233 C -0.0374(4) 0.1114(4) 0.1469(3) 0.0542(14) Uani 1 1 d . . . H233 H -0.0386 0.0577 0.1713 0.055(3) Uiso 1 1 calc R . . C234 C -0.0953(3) 0.1267(4) 0.0939(3) 0.0495(13) Uani 1 1 d . . . H234 H -0.1352 0.0830 0.0824 0.055(3) Uiso 1 1 calc R . . C235 C -0.0939(3) 0.2068(4) 0.0581(3) 0.0486(13) Uani 1 1 d . . . H235 H -0.1332 0.2169 0.0227 0.055(3) Uiso 1 1 calc R . . C236 C -0.0349(3) 0.2718(4) 0.0742(3) 0.0443(12) Uani 1 1 d . . . H236 H -0.0343 0.3253 0.0495 0.055(3) 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 Te1 0.03855(18) 0.03363(17) 0.03921(19) -0.00313(14) -0.00195(12) 0.00209(14) C1 0.032(3) 0.065(3) 0.049(3) -0.009(3) -0.008(2) 0.007(2) F11 0.0372(19) 0.114(3) 0.110(3) 0.029(3) -0.003(2) -0.015(2) F12 0.067(2) 0.096(3) 0.096(3) -0.035(2) -0.021(2) 0.043(2) F13 0.0447(18) 0.113(3) 0.050(2) 0.000(2) -0.0131(15) 0.0112(19) C11 0.051(3) 0.030(2) 0.037(3) -0.0017(19) 0.004(2) -0.004(2) S111 0.0383(6) 0.0375(6) 0.0434(7) -0.0026(5) 0.0019(5) -0.0005(5) S112 0.0405(7) 0.0564(8) 0.0396(7) -0.0004(6) 0.0026(5) 0.0089(6) N12 0.041(2) 0.045(2) 0.037(2) -0.0044(19) 0.0022(17) 0.0010(19) C13 0.047(3) 0.057(3) 0.046(3) -0.009(3) 0.014(2) -0.002(3) C14 0.067(4) 0.071(4) 0.043(3) -0.012(3) 0.008(3) 0.005(3) C15 0.062(4) 0.061(4) 0.044(3) -0.012(3) -0.004(3) 0.003(3) C16 0.052(3) 0.050(3) 0.035(3) -0.001(2) -0.006(2) 0.003(3) C21 0.046(3) 0.036(3) 0.037(3) -0.002(2) -0.001(2) 0.006(2) S211 0.0422(7) 0.0565(8) 0.0397(7) 0.0000(6) -0.0054(5) 0.0077(6) S212 0.0455(7) 0.0714(9) 0.0389(7) 0.0114(6) -0.0027(6) 0.0105(7) N22 0.045(2) 0.045(2) 0.030(2) 0.0024(17) -0.0026(17) 0.0064(18) C23 0.057(3) 0.068(4) 0.031(3) 0.007(3) -0.002(2) 0.010(3) C24 0.073(4) 0.070(4) 0.040(3) 0.009(3) -0.004(3) -0.007(3) C25 0.051(3) 0.092(5) 0.044(3) 0.000(3) 0.003(3) -0.008(3) C26 0.046(3) 0.050(3) 0.044(3) 0.001(2) 0.002(2) 0.000(2) P11 0.0301(6) 0.0307(6) 0.0315(6) 0.0004(4) -0.0009(5) -0.0014(5) C111 0.032(2) 0.026(2) 0.040(3) 0.0018(19) -0.0020(19) -0.0026(18) C112 0.038(2) 0.040(2) 0.038(3) 0.001(2) 0.0002(19) 0.004(2) C113 0.041(3) 0.056(3) 0.041(3) 0.000(2) 0.009(2) 0.002(2) C114 0.050(3) 0.044(3) 0.037(3) 0.001(2) 0.010(2) 0.003(2) C115 0.052(3) 0.045(3) 0.033(3) -0.002(2) -0.002(2) -0.001(2) C116 0.034(2) 0.043(3) 0.040(3) -0.006(2) 0.000(2) -0.001(2) C121 0.037(3) 0.031(2) 0.034(2) 0.0006(19) -0.0003(19) -0.0005(19) C122 0.038(3) 0.033(2) 0.035(3) 0.0005(19) -0.001(2) 0.001(2) C123 0.037(3) 0.042(3) 0.046(3) 0.005(2) 0.002(2) -0.007(2) C124 0.045(3) 0.031(2) 0.050(3) 0.007(2) -0.007(2) -0.009(2) C125 0.049(3) 0.028(2) 0.055(3) 0.002(2) -0.006(2) 0.000(2) C126 0.042(3) 0.033(2) 0.042(3) -0.001(2) 0.003(2) 0.002(2) C131 0.031(2) 0.031(2) 0.033(2) -0.0024(18) 0.0016(18) 0.0000(18) C132 0.037(3) 0.030(2) 0.038(3) 0.0000(19) -0.001(2) -0.0012(19) C133 0.034(2) 0.043(3) 0.039(3) 0.000(2) -0.001(2) 0.005(2) C134 0.042(3) 0.030(2) 0.040(3) 0.000(2) 0.002(2) 0.005(2) C135 0.049(3) 0.026(2) 0.043(3) -0.003(2) 0.003(2) -0.002(2) C136 0.037(2) 0.028(2) 0.045(3) -0.0004(19) 0.001(2) -0.0052(19) N31 0.031(2) 0.037(2) 0.033(2) 0.0008(16) -0.0067(16) -0.0029(16) P21 0.0320(6) 0.0333(6) 0.0321(6) -0.0004(5) -0.0021(5) -0.0001(5) C211 0.040(3) 0.040(3) 0.032(2) 0.000(2) -0.006(2) 0.003(2) C212 0.051(3) 0.037(3) 0.055(3) 0.005(2) 0.003(3) 0.000(2) C213 0.081(5) 0.043(3) 0.061(4) 0.007(3) -0.004(3) -0.004(3) C214 0.079(5) 0.047(3) 0.061(4) -0.010(3) -0.006(3) 0.023(3) C215 0.057(4) 0.057(4) 0.058(4) -0.010(3) 0.001(3) 0.022(3) C216 0.044(3) 0.048(3) 0.044(3) -0.004(2) 0.005(2) 0.006(2) C221 0.038(3) 0.032(2) 0.039(3) -0.0027(19) -0.003(2) -0.0049(19) C222 0.045(3) 0.038(3) 0.040(3) -0.002(2) 0.003(2) 0.001(2) C223 0.048(3) 0.048(3) 0.050(3) -0.011(3) 0.012(2) 0.001(2) C224 0.060(4) 0.053(3) 0.049(3) -0.004(3) 0.018(3) -0.006(3) C225 0.070(4) 0.066(4) 0.036(3) 0.005(3) 0.010(3) -0.003(3) C226 0.046(3) 0.058(3) 0.044(3) 0.009(3) 0.000(2) 0.004(3) C231 0.033(2) 0.037(2) 0.036(3) -0.004(2) 0.000(2) 0.005(2) C232 0.039(3) 0.050(3) 0.046(3) 0.007(2) -0.005(2) -0.011(2) C233 0.049(3) 0.049(3) 0.064(4) 0.008(3) -0.010(3) -0.017(3) C234 0.037(3) 0.056(3) 0.055(3) -0.009(3) -0.004(2) -0.017(2) C235 0.037(3) 0.056(3) 0.052(3) -0.011(3) -0.011(2) 0.001(2) C236 0.042(3) 0.043(3) 0.048(3) -0.004(2) -0.010(2) 0.000(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 Te1 C1 2.237(5) . ? Te1 S211 2.6868(14) . ? Te1 S111 2.7105(14) . ? C1 F11 1.329(7) . ? C1 F12 1.343(7) . ? C1 F13 1.358(6) . ? C11 N12 1.347(6) . ? C11 S112 1.692(5) . ? C11 S111 1.732(5) . ? N12 C16 1.466(6) . ? N12 C13 1.470(6) . ? C13 C14 1.516(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.523(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.526(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C21 N22 1.346(7) . ? C21 S212 1.696(5) . ? C21 S211 1.719(5) . ? N22 C23 1.469(6) . ? N22 C26 1.471(7) . ? C23 C24 1.525(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.500(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.511(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? P11 N31 1.586(4) . ? P11 C121 1.793(5) . ? P11 C131 1.801(5) . ? P11 C111 1.809(5) . ? C111 C112 1.384(6) . ? C111 C116 1.387(6) . ? C112 C113 1.392(7) . ? C112 H112 0.9300 . ? C113 C114 1.375(8) . ? C113 H113 0.9300 . ? C114 C115 1.386(7) . ? C114 H114 0.9300 . ? C115 C116 1.378(7) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C126 1.396(7) . ? C121 C122 1.398(7) . ? C122 C123 1.389(7) . ? C122 H122 0.9300 . ? C123 C124 1.386(7) . ? C123 H123 0.9300 . ? C124 C125 1.385(8) . ? C124 H124 0.9300 . ? C125 C126 1.399(7) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C136 1.397(6) . ? C131 C132 1.398(6) . ? C132 C133 1.392(7) . ? C132 H132 0.9300 . ? C133 C134 1.381(7) . ? C133 H133 0.9300 . ? C134 C135 1.389(7) . ? C134 H134 0.9300 . ? C135 C136 1.382(7) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? N31 P21 1.581(4) . ? P21 C231 1.796(5) . ? P21 C221 1.799(5) . ? P21 C211 1.800(5) . ? C211 C212 1.393(7) . ? C211 C216 1.400(7) . ? C212 C213 1.400(8) . ? C212 H212 0.9300 . ? C213 C214 1.367(9) . ? C213 H213 0.9300 . ? C214 C215 1.390(9) . ? C214 H214 0.9300 . ? C215 C216 1.376(8) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C226 1.389(7) . ? C221 C222 1.400(7) . ? C222 C223 1.401(7) . ? C222 H222 0.9300 . ? C223 C224 1.375(8) . ? C223 H223 0.9300 . ? C224 C225 1.382(9) . ? C224 H224 0.9300 . ? C225 C226 1.382(8) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C232 1.397(7) . ? C231 C236 1.398(7) . ? C232 C233 1.383(7) . ? C232 H232 0.9300 . ? C233 C234 1.384(8) . ? C233 H233 0.9300 . ? C234 C235 1.381(8) . ? C234 H234 0.9300 . ? C235 C236 1.377(7) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te1 S211 83.70(15) . . ? C1 Te1 S111 78.39(15) . . ? S211 Te1 S111 162.08(4) . . ? F11 C1 F12 104.3(5) . . ? F11 C1 F13 106.8(4) . . ? F12 C1 F13 103.0(5) . . ? F11 C1 Te1 114.4(4) . . ? F12 C1 Te1 113.1(3) . . ? F13 C1 Te1 114.1(4) . . ? N12 C11 S112 120.8(4) . . ? N12 C11 S111 116.8(4) . . ? S112 C11 S111 122.3(3) . . ? C11 S111 Te1 94.30(18) . . ? C11 N12 C16 124.3(4) . . ? C11 N12 C13 124.3(4) . . ? C16 N12 C13 111.4(4) . . ? N12 C13 C14 104.4(5) . . ? N12 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? N12 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C13 C14 C15 104.0(5) . . ? C13 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? C13 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? C14 C15 C16 103.3(5) . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? N12 C16 C15 103.7(4) . . ? N12 C16 H16A 111.0 . . ? C15 C16 H16A 111.0 . . ? N12 C16 H16B 111.0 . . ? C15 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? N22 C21 S212 120.4(4) . . ? N22 C21 S211 117.6(4) . . ? S212 C21 S211 122.0(3) . . ? C21 S211 Te1 93.72(17) . . ? C21 N22 C23 124.6(4) . . ? C21 N22 C26 123.8(4) . . ? C23 N22 C26 111.6(4) . . ? N22 C23 C24 104.0(5) . . ? N22 C23 H23A 110.9 . . ? C24 C23 H23A 110.9 . . ? N22 C23 H23B 110.9 . . ? C24 C23 H23B 110.9 . . ? H23A C23 H23B 109.0 . . ? C25 C24 C23 105.3(5) . . ? C25 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? C25 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C24 C25 C26 104.7(5) . . ? C24 C25 H25A 110.8 . . ? C26 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C26 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? N22 C26 C25 103.5(4) . . ? N22 C26 H26A 111.1 . . ? C25 C26 H26A 111.1 . . ? N22 C26 H26B 111.1 . . ? C25 C26 H26B 111.1 . . ? H26A C26 H26B 109.0 . . ? N31 P11 C121 114.7(2) . . ? N31 P11 C131 108.2(2) . . ? C121 P11 C131 110.8(2) . . ? N31 P11 C111 109.6(2) . . ? C121 P11 C111 106.5(2) . . ? C131 P11 C111 106.8(2) . . ? C112 C111 C116 120.0(4) . . ? C112 C111 P11 120.6(4) . . ? C116 C111 P11 119.4(3) . . ? C111 C112 C113 119.6(5) . . ? C111 C112 H112 120.2 . . ? C113 C112 H112 120.2 . . ? C114 C113 C112 120.3(5) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C113 C114 C115 119.8(5) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C116 C115 C114 120.3(5) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C111 119.9(5) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C126 C121 C122 119.1(4) . . ? C126 C121 P11 117.7(4) . . ? C122 C121 P11 122.5(4) . . ? C123 C122 C121 120.4(4) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 120.0(5) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C125 C124 C123 120.4(5) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C124 C125 C126 119.7(5) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C121 C126 C125 120.3(5) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? C136 C131 C132 119.4(4) . . ? C136 C131 P11 117.8(3) . . ? C132 C131 P11 122.6(3) . . ? C133 C132 C131 119.5(4) . . ? C133 C132 H132 120.3 . . ? C131 C132 H132 120.3 . . ? C134 C133 C132 120.7(4) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.9(4) . . ? C133 C134 H134 120.0 . . ? C135 C134 H134 120.0 . . ? C136 C135 C134 120.0(4) . . ? C136 C135 H135 120.0 . . ? C134 C135 H135 120.0 . . ? C135 C136 C131 120.4(4) . . ? C135 C136 H136 119.8 . . ? C131 C136 H136 119.8 . . ? P21 N31 P11 140.9(3) . . ? N31 P21 C231 108.0(2) . . ? N31 P21 C221 113.8(2) . . ? C231 P21 C221 107.6(2) . . ? N31 P21 C211 114.1(2) . . ? C231 P21 C211 107.1(2) . . ? C221 P21 C211 105.9(2) . . ? C212 C211 C216 119.9(5) . . ? C212 C211 P21 120.8(4) . . ? C216 C211 P21 119.1(4) . . ? C211 C212 C213 119.2(5) . . ? C211 C212 H212 120.4 . . ? C213 C212 H212 120.4 . . ? C214 C213 C212 120.4(6) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C213 C214 C215 120.6(6) . . ? C213 C214 H214 119.7 . . ? C215 C214 H214 119.7 . . ? C216 C215 C214 120.0(6) . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 C211 120.0(5) . . ? C215 C216 H216 120.0 . . ? C211 C216 H216 120.0 . . ? C226 C221 C222 118.6(5) . . ? C226 C221 P21 122.0(4) . . ? C222 C221 P21 119.4(4) . . ? C221 C222 C223 120.0(5) . . ? C221 C222 H222 120.0 . . ? C223 C222 H222 120.0 . . ? C224 C223 C222 120.3(5) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 119.7(5) . . ? C223 C224 H224 120.2 . . ? C225 C224 H224 120.2 . . ? C226 C225 C224 120.6(6) . . ? C226 C225 H225 119.7 . . ? C224 C225 H225 119.7 . . ? C225 C226 C221 120.8(5) . . ? C225 C226 H226 119.6 . . ? C221 C226 H226 119.6 . . ? C232 C231 C236 119.0(5) . . ? C232 C231 P21 119.5(4) . . ? C236 C231 P21 121.4(4) . . ? C233 C232 C231 120.4(5) . . ? C233 C232 H232 119.8 . . ? C231 C232 H232 119.8 . . ? C232 C233 C234 120.0(5) . . ? C232 C233 H233 120.0 . . ? C234 C233 H233 120.0 . . ? C235 C234 C233 119.9(5) . . ? C235 C234 H234 120.0 . . ? C233 C234 H234 120.0 . . ? C236 C235 C234 120.7(5) . . ? C236 C235 H235 119.7 . . ? C234 C235 H235 119.6 . . ? C235 C236 C231 120.0(5) . . ? C235 C236 H236 120.0 . . ? C231 C236 H236 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.942 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.132 # Attachment '3k.cif' data_ipwt085 _database_code_depnum_ccdc_archive 'CCDC 614396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N P2, C16 H14 Cl F3 N' _chemical_formula_sum 'C52 H44 Cl F3 N2 P2 S2 Te' _chemical_formula_weight 1043.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3944(8) _cell_length_b 14.7103(9) _cell_length_c 20.9587(11) _cell_angle_alpha 90 _cell_angle_beta 94.076(4) _cell_angle_gamma 90 _cell_volume 4734.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50878 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.33 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6956 _exptl_absorpt_correction_T_max 0.8778 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'IPDS II (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 73923 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.33 _reflns_number_total 10567 _reflns_number_gt 8412 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0728P)^2^+0.8236P] 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 SHELXL _refine_ls_extinction_coef 0.0024(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10567 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _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 Te1 Te 0.580757(11) 0.237612(12) 0.326497(9) 0.02912(8) Uani 1 1 d . . . Cl1 Cl 0.55867(4) 0.24482(4) 0.19638(3) 0.02973(14) Uani 1 1 d . . . C1 C 0.7179(2) 0.2132(2) 0.30785(17) 0.0431(7) Uani 1 1 d . . . F11 F 0.77152(13) 0.2133(2) 0.36191(11) 0.0681(7) Uani 1 1 d . . . F12 F 0.73113(15) 0.13338(19) 0.28025(14) 0.0803(8) Uani 1 1 d . . . F13 F 0.75049(16) 0.2748(2) 0.27014(15) 0.0827(9) Uani 1 1 d . . . S1 S 0.62993(5) 0.22073(5) 0.44565(4) 0.03262(15) Uani 1 1 d . . . S2 S 0.44254(5) 0.27122(5) 0.42330(3) 0.03256(16) Uani 1 1 d . . . C2 C 0.52974(19) 0.24887(17) 0.47441(14) 0.0280(5) Uani 1 1 d . . . N1 N 0.52554(16) 0.25001(15) 0.53864(12) 0.0303(5) Uani 1 1 d . . . C3 C 0.59941(19) 0.22679(19) 0.58267(14) 0.0324(6) Uani 1 1 d . . . H3A H 0.5996 0.2668 0.6195 0.043(5) Uiso 1 1 calc R . . H3B H 0.6526 0.2380 0.5617 0.043(5) Uiso 1 1 calc R . . C31 C 0.60013(17) 0.12872(18) 0.60607(13) 0.0287(5) Uani 1 1 d . . . C32 C 0.66017(19) 0.10465(19) 0.65599(14) 0.0332(6) Uani 1 1 d . . . H32 H 0.6992 0.1479 0.6732 0.0476(16) Uiso 1 1 calc R . . C33 C 0.6625(2) 0.0172(2) 0.68030(15) 0.0394(7) Uani 1 1 d . . . H33 H 0.7026 0.0021 0.7139 0.0476(16) Uiso 1 1 calc R . . C34 C 0.6047(2) -0.0482(2) 0.65430(16) 0.0402(7) Uani 1 1 d . . . H34 H 0.6061 -0.1072 0.6703 0.0476(16) Uiso 1 1 calc R . . C35 C 0.5455(2) -0.02441(19) 0.60476(15) 0.0362(6) Uani 1 1 d . . . H35 H 0.5069 -0.0678 0.5873 0.0476(16) Uiso 1 1 calc R . . C36 C 0.54268(18) 0.0632(2) 0.58065(13) 0.0325(6) Uani 1 1 d . . . H36 H 0.5021 0.0783 0.5473 0.0476(16) Uiso 1 1 calc R . . C4 C 0.4444(2) 0.2694(2) 0.56882(14) 0.0342(6) Uani 1 1 d . . . H4A H 0.4282 0.2165 0.5929 0.043(5) Uiso 1 1 calc R . . H4B H 0.3983 0.2806 0.5357 0.043(5) Uiso 1 1 calc R . . C41 C 0.45224(19) 0.35054(19) 0.61298(14) 0.0325(6) Uani 1 1 d . . . C42 C 0.5053(2) 0.4245(2) 0.60085(17) 0.0456(8) Uani 1 1 d . . . H42 H 0.5367 0.4248 0.5645 0.0476(16) Uiso 1 1 calc R . . C43 C 0.5117(3) 0.4979(2) 0.64281(19) 0.0517(9) Uani 1 1 d . . . H43 H 0.5476 0.5468 0.6346 0.0476(16) Uiso 1 1 calc R . . C44 C 0.4651(2) 0.4986(2) 0.69623(17) 0.0480(8) Uani 1 1 d . . . H44 H 0.4702 0.5473 0.7245 0.0476(16) Uiso 1 1 calc R . . C45 C 0.4106(2) 0.4268(2) 0.70791(15) 0.0417(7) Uani 1 1 d . . . H45 H 0.3778 0.4280 0.7435 0.0476(16) Uiso 1 1 calc R . . C46 C 0.4048(2) 0.3529(2) 0.66673(14) 0.0354(6) Uani 1 1 d . . . H46 H 0.3686 0.3044 0.6753 0.0476(16) Uiso 1 1 calc R . . P1 P 0.63101(4) 0.24690(4) 0.85240(3) 0.02557(14) Uani 1 1 d . . . C111 C 0.70859(18) 0.26553(18) 0.79311(13) 0.0288(5) Uani 1 1 d . . . C112 C 0.78546(18) 0.2147(2) 0.79774(14) 0.0333(6) Uani 1 1 d . . . H112 H 0.7965 0.1742 0.8314 0.0476(16) Uiso 1 1 calc R . . C113 C 0.8454(2) 0.2250(2) 0.75159(15) 0.0390(7) Uani 1 1 d . . . H113 H 0.8963 0.1907 0.7543 0.0476(16) Uiso 1 1 calc R . . C114 C 0.8301(2) 0.2859(2) 0.70173(15) 0.0417(7) Uani 1 1 d . . . H114 H 0.8709 0.2932 0.6715 0.0476(16) Uiso 1 1 calc R . . C115 C 0.7532(2) 0.3362(2) 0.69703(15) 0.0403(7) Uani 1 1 d . . . H115 H 0.7427 0.3770 0.6635 0.0476(16) Uiso 1 1 calc R . . C116 C 0.6922(2) 0.32571(19) 0.74215(13) 0.0338(6) Uani 1 1 d . . . H116 H 0.6405 0.3587 0.7385 0.0476(16) Uiso 1 1 calc R . . C121 C 0.55975(17) 0.15783(19) 0.82152(13) 0.0292(5) Uani 1 1 d . . . C122 C 0.50228(19) 0.1732(2) 0.76803(14) 0.0359(6) Uani 1 1 d . . . H122 H 0.4977 0.2308 0.7498 0.0476(16) Uiso 1 1 calc R . . C123 C 0.4519(2) 0.1018(2) 0.74214(16) 0.0442(7) Uani 1 1 d . . . H123 H 0.4135 0.1115 0.7065 0.0476(16) Uiso 1 1 calc R . . C124 C 0.4593(2) 0.0160(2) 0.76966(18) 0.0473(8) Uani 1 1 d . . . H124 H 0.4252 -0.0314 0.7525 0.0476(16) Uiso 1 1 calc R . . C125 C 0.5163(2) 0.0006(2) 0.82192(17) 0.0446(8) Uani 1 1 d . . . H125 H 0.5210 -0.0573 0.8397 0.0476(16) Uiso 1 1 calc R . . C126 C 0.5668(2) 0.0710(2) 0.84828(15) 0.0368(6) Uani 1 1 d . . . H126 H 0.6054 0.0604 0.8837 0.0476(16) Uiso 1 1 calc R . . C131 C 0.56970(18) 0.35057(18) 0.85765(13) 0.0294(5) Uani 1 1 d . . . C132 C 0.6142(2) 0.4334(2) 0.85727(14) 0.0365(6) Uani 1 1 d . . . H132 H 0.6739 0.4341 0.8531 0.0476(16) Uiso 1 1 calc R . . C133 C 0.5695(2) 0.5147(2) 0.86303(16) 0.0435(7) Uani 1 1 d . . . H133 H 0.5990 0.5698 0.8616 0.0476(16) Uiso 1 1 calc R . . C134 C 0.4811(2) 0.5136(2) 0.87090(16) 0.0454(8) Uani 1 1 d . . . H134 H 0.4512 0.5681 0.8745 0.0476(16) Uiso 1 1 calc R . . C135 C 0.4369(2) 0.4319(2) 0.87353(15) 0.0417(7) Uani 1 1 d . . . H135 H 0.3778 0.4318 0.8802 0.0476(16) Uiso 1 1 calc R . . C136 C 0.48047(19) 0.3497(2) 0.86619(14) 0.0350(6) Uani 1 1 d . . . H136 H 0.4504 0.2950 0.8670 0.0476(16) Uiso 1 1 calc R . . N2 N 0.68359(15) 0.21615(17) 0.91653(11) 0.0306(5) Uani 1 1 d . . . P2 P 0.66551(4) 0.21800(5) 0.99025(3) 0.02559(14) Uani 1 1 d . . . C211 C 0.70971(17) 0.11588(18) 1.02725(13) 0.0283(5) Uani 1 1 d . . . C212 C 0.68512(19) 0.0889(2) 1.08728(14) 0.0347(6) Uani 1 1 d . . . H212 H 0.6450 0.1231 1.1082 0.0476(16) Uiso 1 1 calc R . . C213 C 0.7208(2) 0.0110(2) 1.11547(15) 0.0396(7) Uani 1 1 d . . . H213 H 0.7047 -0.0071 1.1555 0.0476(16) Uiso 1 1 calc R . . C214 C 0.7803(2) -0.0400(2) 1.08444(17) 0.0415(7) Uani 1 1 d . . . H214 H 0.8041 -0.0923 1.1036 0.0476(16) Uiso 1 1 calc R . . C215 C 0.8045(2) -0.0135(2) 1.02538(18) 0.0443(8) Uani 1 1 d . . . H215 H 0.8444 -0.0483 1.0047 0.0476(16) Uiso 1 1 calc R . . C216 C 0.76996(19) 0.0646(2) 0.99620(15) 0.0362(6) Uani 1 1 d . . . H216 H 0.7869 0.0825 0.9564 0.0476(16) Uiso 1 1 calc R . . C221 C 0.71675(16) 0.31535(18) 1.02882(12) 0.0266(5) Uani 1 1 d . . . C222 C 0.76339(18) 0.37674(19) 0.99353(14) 0.0318(6) Uani 1 1 d . . . H222 H 0.7689 0.3669 0.9502 0.0476(16) Uiso 1 1 calc R . . C223 C 0.8016(2) 0.4527(2) 1.02356(16) 0.0388(7) Uani 1 1 d . . . H223 H 0.8315 0.4942 0.9999 0.0476(16) Uiso 1 1 calc R . . C224 C 0.79537(19) 0.4670(2) 1.08830(15) 0.0374(7) Uani 1 1 d . . . H224 H 0.8214 0.5178 1.1080 0.0476(16) Uiso 1 1 calc R . . C225 C 0.75035(19) 0.4055(2) 1.12378(14) 0.0354(6) Uani 1 1 d . . . H225 H 0.7465 0.4151 1.1673 0.0476(16) Uiso 1 1 calc R . . C226 C 0.71113(18) 0.32990(19) 1.09465(13) 0.0309(6) Uani 1 1 d . . . H226 H 0.6811 0.2888 1.1187 0.0476(16) Uiso 1 1 calc R . . C231 C 0.55128(17) 0.22012(19) 1.00566(13) 0.0288(5) Uani 1 1 d . . . C232 C 0.50387(19) 0.1391(2) 1.00041(16) 0.0390(7) Uani 1 1 d . . . H232 H 0.5325 0.0845 0.9942 0.0476(16) Uiso 1 1 calc R . . C233 C 0.4144(2) 0.1399(3) 1.00447(18) 0.0482(8) Uani 1 1 d . . . H233 H 0.3830 0.0860 1.0010 0.0476(16) Uiso 1 1 calc R . . C234 C 0.3720(2) 0.2218(3) 1.01367(17) 0.0476(8) Uani 1 1 d . . . H234 H 0.3119 0.2226 1.0161 0.0476(16) Uiso 1 1 calc R . . C235 C 0.4187(2) 0.3020(3) 1.01922(16) 0.0447(8) Uani 1 1 d . . . H235 H 0.3900 0.3566 1.0255 0.0476(16) Uiso 1 1 calc R . . C236 C 0.50856(19) 0.3013(2) 1.01542(14) 0.0356(6) Uani 1 1 d . . . H236 H 0.5399 0.3552 1.0194 0.0476(16) 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 Te1 0.02754(11) 0.02633(11) 0.03389(12) -0.00045(6) 0.00497(7) -0.00056(6) Cl1 0.0287(3) 0.0370(3) 0.0247(3) 0.0012(2) 0.0101(2) -0.0019(2) C1 0.0286(15) 0.0522(19) 0.0494(18) -0.0031(15) 0.0086(13) 0.0032(13) F11 0.0305(10) 0.117(2) 0.0568(13) -0.0069(13) 0.0006(9) 0.0126(12) F12 0.0491(13) 0.0861(18) 0.107(2) -0.0424(16) 0.0176(13) 0.0178(12) F13 0.0382(12) 0.115(2) 0.098(2) 0.0438(17) 0.0237(13) -0.0091(13) S1 0.0261(3) 0.0351(3) 0.0364(4) -0.0016(3) 0.0002(3) 0.0031(3) S2 0.0283(3) 0.0378(4) 0.0312(3) 0.0033(3) -0.0007(3) 0.0058(3) C2 0.0295(13) 0.0236(12) 0.0306(13) 0.0005(10) 0.0009(11) -0.0016(10) N1 0.0279(12) 0.0316(11) 0.0310(12) 0.0007(9) -0.0008(10) 0.0008(9) C3 0.0331(14) 0.0311(14) 0.0320(14) -0.0016(11) -0.0039(12) -0.0027(11) C31 0.0282(13) 0.0285(13) 0.0294(13) -0.0022(10) 0.0029(11) 0.0002(10) C32 0.0306(14) 0.0336(14) 0.0344(15) -0.0023(11) -0.0038(11) 0.0009(11) C33 0.0372(16) 0.0405(16) 0.0398(16) 0.0025(12) -0.0026(13) 0.0068(13) C34 0.0451(17) 0.0299(14) 0.0459(17) 0.0030(12) 0.0052(14) 0.0038(12) C35 0.0411(16) 0.0301(14) 0.0373(15) -0.0030(11) 0.0024(13) -0.0058(12) C36 0.0311(14) 0.0367(14) 0.0293(13) -0.0023(11) -0.0011(11) -0.0009(11) C4 0.0323(15) 0.0375(15) 0.0333(15) -0.0003(11) 0.0051(12) -0.0024(11) C41 0.0349(15) 0.0297(13) 0.0324(14) 0.0026(11) 0.0005(12) 0.0029(11) C42 0.0531(19) 0.0353(16) 0.0505(19) 0.0022(14) 0.0174(16) -0.0041(14) C43 0.060(2) 0.0300(15) 0.065(2) 0.0027(15) 0.0063(19) -0.0084(15) C44 0.057(2) 0.0369(16) 0.0487(19) -0.0072(14) -0.0045(16) 0.0064(15) C45 0.0469(18) 0.0447(17) 0.0335(15) -0.0014(13) 0.0022(13) 0.0058(14) C46 0.0370(15) 0.0364(15) 0.0327(15) 0.0037(11) 0.0016(12) 0.0028(12) P1 0.0238(3) 0.0277(3) 0.0250(3) -0.0025(2) 0.0003(3) -0.0007(2) C111 0.0287(13) 0.0307(13) 0.0269(13) -0.0053(10) 0.0006(11) -0.0053(10) C112 0.0264(13) 0.0408(15) 0.0324(14) -0.0055(12) -0.0001(11) -0.0051(11) C113 0.0258(14) 0.0541(18) 0.0372(16) -0.0102(13) 0.0027(12) -0.0052(13) C114 0.0355(16) 0.0557(19) 0.0349(16) -0.0107(14) 0.0086(13) -0.0181(14) C115 0.0504(18) 0.0387(16) 0.0321(15) 0.0000(12) 0.0040(13) -0.0133(14) C116 0.0374(15) 0.0333(14) 0.0304(14) -0.0026(11) 0.0003(12) -0.0036(12) C121 0.0260(12) 0.0312(13) 0.0305(13) -0.0053(10) 0.0022(10) -0.0032(10) C122 0.0320(14) 0.0396(15) 0.0356(15) -0.0037(12) -0.0018(12) -0.0011(12) C123 0.0366(16) 0.056(2) 0.0386(16) -0.0129(14) -0.0041(13) -0.0080(14) C124 0.0383(17) 0.0449(18) 0.060(2) -0.0199(15) 0.0098(15) -0.0137(14) C125 0.0477(18) 0.0304(15) 0.057(2) -0.0052(14) 0.0109(16) -0.0067(13) C126 0.0372(15) 0.0317(14) 0.0414(16) -0.0006(12) 0.0025(13) -0.0015(12) C131 0.0313(14) 0.0300(13) 0.0268(13) -0.0033(10) 0.0003(11) 0.0029(10) C132 0.0385(16) 0.0352(15) 0.0357(15) -0.0045(12) 0.0023(12) -0.0022(12) C133 0.059(2) 0.0289(14) 0.0432(17) -0.0062(12) 0.0042(15) 0.0011(14) C134 0.055(2) 0.0389(16) 0.0411(17) -0.0105(13) -0.0031(15) 0.0162(15) C135 0.0377(16) 0.0471(17) 0.0399(16) -0.0102(13) 0.0004(13) 0.0113(14) C136 0.0317(14) 0.0374(15) 0.0353(15) -0.0040(12) -0.0011(12) 0.0033(11) N2 0.0264(11) 0.0356(12) 0.0295(12) -0.0040(9) 0.0005(9) 0.0019(9) P2 0.0223(3) 0.0280(3) 0.0263(3) -0.0012(2) 0.0003(2) -0.0001(2) C211 0.0248(12) 0.0276(12) 0.0323(13) -0.0024(10) -0.0009(10) -0.0025(10) C212 0.0355(15) 0.0344(14) 0.0340(14) 0.0006(11) 0.0012(12) 0.0021(12) C213 0.0451(17) 0.0352(15) 0.0379(16) 0.0049(12) -0.0011(13) 0.0007(13) C214 0.0365(16) 0.0317(14) 0.0555(19) 0.0055(13) -0.0033(14) 0.0014(12) C215 0.0349(16) 0.0340(15) 0.065(2) -0.0001(14) 0.0119(15) 0.0079(13) C216 0.0328(15) 0.0343(15) 0.0426(16) 0.0013(12) 0.0106(12) 0.0009(12) C221 0.0225(12) 0.0287(12) 0.0288(13) -0.0013(10) 0.0027(10) 0.0022(10) C222 0.0310(14) 0.0326(14) 0.0316(14) 0.0009(11) 0.0020(11) -0.0028(11) C223 0.0358(15) 0.0346(15) 0.0464(17) 0.0035(13) 0.0057(13) -0.0075(12) C224 0.0336(15) 0.0318(14) 0.0459(17) -0.0085(12) -0.0032(13) -0.0039(12) C225 0.0309(14) 0.0400(16) 0.0349(15) -0.0078(12) -0.0004(12) 0.0009(12) C226 0.0302(13) 0.0319(13) 0.0306(14) -0.0015(11) 0.0030(11) -0.0024(11) C231 0.0245(12) 0.0355(14) 0.0258(12) -0.0012(10) -0.0022(10) -0.0008(10) C232 0.0288(14) 0.0399(16) 0.0483(18) -0.0019(13) 0.0025(13) -0.0026(12) C233 0.0317(16) 0.055(2) 0.058(2) -0.0016(16) 0.0040(15) -0.0118(14) C234 0.0220(14) 0.075(2) 0.0458(18) -0.0053(17) 0.0037(13) 0.0009(14) C235 0.0345(16) 0.059(2) 0.0400(17) -0.0086(15) 0.0013(13) 0.0129(15) C236 0.0327(14) 0.0408(16) 0.0332(14) -0.0068(12) 0.0011(12) 0.0034(12) _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 Te1 C1 2.204(3) . ? Te1 S1 2.5695(8) . ? Te1 Cl1 2.7262(7) . ? C1 F13 1.324(4) . ? C1 F12 1.331(4) . ? C1 F11 1.353(4) . ? S1 C2 1.745(3) . ? S2 C2 1.689(3) . ? C2 N1 1.352(4) . ? N1 C3 1.454(3) . ? N1 C4 1.468(4) . ? C3 C31 1.523(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C31 C36 1.388(4) . ? C31 C32 1.392(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9300 . ? C33 C34 1.395(5) . ? C33 H33 0.9300 . ? C34 C35 1.377(4) . ? C34 H34 0.9300 . ? C35 C36 1.384(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C4 C41 1.510(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C41 C46 1.386(4) . ? C41 C42 1.396(4) . ? C42 C43 1.391(5) . ? C42 H42 0.9300 . ? C43 C44 1.372(5) . ? C43 H43 0.9300 . ? C44 C45 1.381(5) . ? C44 H44 0.9300 . ? C45 C46 1.386(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? P1 N2 1.585(2) . ? P1 C121 1.799(3) . ? P1 C131 1.801(3) . ? P1 C111 1.804(3) . ? C111 C116 1.396(4) . ? C111 C112 1.397(4) . ? C112 C113 1.392(4) . ? C112 H112 0.9300 . ? C113 C114 1.384(5) . ? C113 H113 0.9300 . ? C114 C115 1.394(5) . ? C114 H114 0.9300 . ? C115 C116 1.387(4) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C122 1.396(4) . ? C121 C126 1.396(4) . ? C122 C123 1.393(4) . ? C122 H122 0.9300 . ? C123 C124 1.388(5) . ? C123 H123 0.9300 . ? C124 C125 1.373(5) . ? C124 H124 0.9300 . ? C125 C126 1.386(4) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C136 1.398(4) . ? C131 C132 1.398(4) . ? C132 C133 1.389(4) . ? C132 H132 0.9300 . ? C133 C134 1.382(5) . ? C133 H133 0.9300 . ? C134 C135 1.383(5) . ? C134 H134 0.9300 . ? C135 C136 1.397(4) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? N2 P2 1.590(2) . ? P2 C221 1.799(3) . ? P2 C211 1.802(3) . ? P2 C231 1.811(3) . ? C211 C216 1.392(4) . ? C211 C212 1.397(4) . ? C212 C213 1.386(4) . ? C212 H212 0.9300 . ? C213 C214 1.381(5) . ? C213 H213 0.9300 . ? C214 C215 1.374(5) . ? C214 H214 0.9300 . ? C215 C216 1.390(4) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C222 1.398(4) . ? C221 C226 1.405(4) . ? C222 C223 1.391(4) . ? C222 H222 0.9300 . ? C223 C224 1.383(4) . ? C223 H223 0.9300 . ? C224 C225 1.387(4) . ? C224 H224 0.9300 . ? C225 C226 1.386(4) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C236 1.385(4) . ? C231 C232 1.397(4) . ? C232 C233 1.386(4) . ? C232 H232 0.9300 . ? C233 C234 1.390(5) . ? C233 H233 0.9300 . ? C234 C235 1.383(5) . ? C234 H234 0.9300 . ? C235 C236 1.391(4) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te1 S1 86.38(9) . . ? C1 Te1 Cl1 83.22(9) . . ? S1 Te1 Cl1 169.47(2) . . ? F13 C1 F12 105.6(3) . . ? F13 C1 F11 105.4(3) . . ? F12 C1 F11 105.2(3) . . ? F13 C1 Te1 113.7(2) . . ? F12 C1 Te1 113.5(2) . . ? F11 C1 Te1 112.7(2) . . ? C2 S1 Te1 96.10(10) . . ? N1 C2 S2 122.5(2) . . ? N1 C2 S1 116.9(2) . . ? S2 C2 S1 120.61(17) . . ? C2 N1 C3 122.6(2) . . ? C2 N1 C4 122.3(2) . . ? C3 N1 C4 115.1(2) . . ? N1 C3 C31 114.5(2) . . ? N1 C3 H3A 108.6 . . ? C31 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C31 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C36 C31 C32 118.9(3) . . ? C36 C31 C3 122.9(2) . . ? C32 C31 C3 118.2(2) . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 120.2(3) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? N1 C4 C41 112.6(2) . . ? N1 C4 H4A 109.1 . . ? C41 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C41 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C46 C41 C42 118.5(3) . . ? C46 C41 C4 119.6(3) . . ? C42 C41 C4 121.8(3) . . ? C43 C42 C41 120.4(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.3(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 120.7(3) . . ? C41 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? N2 P1 C121 111.02(13) . . ? N2 P1 C131 115.34(13) . . ? C121 P1 C131 109.25(13) . . ? N2 P1 C111 107.71(13) . . ? C121 P1 C111 106.22(12) . . ? C131 P1 C111 106.80(13) . . ? C116 C111 C112 119.9(3) . . ? C116 C111 P1 122.0(2) . . ? C112 C111 P1 118.0(2) . . ? C113 C112 C111 119.6(3) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C114 C113 C112 120.6(3) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.7(3) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C116 C115 C114 120.3(3) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C111 119.8(3) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C122 C121 C126 119.8(3) . . ? C122 C121 P1 120.4(2) . . ? C126 C121 P1 119.6(2) . . ? C123 C122 C121 119.6(3) . . ? C123 C122 H122 120.2 . . ? C121 C122 H122 120.2 . . ? C124 C123 C122 119.8(3) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C125 C124 C123 120.7(3) . . ? C125 C124 H124 119.7 . . ? C123 C124 H124 119.7 . . ? C124 C125 C126 120.2(3) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C126 C121 119.9(3) . . ? C125 C126 H126 120.1 . . ? C121 C126 H126 120.1 . . ? C136 C131 C132 119.6(3) . . ? C136 C131 P1 121.6(2) . . ? C132 C131 P1 118.6(2) . . ? C133 C132 C131 120.3(3) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 119.8(3) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 120.4(3) . . ? C133 C134 H134 119.8 . . ? C135 C134 H134 119.8 . . ? C134 C135 C136 120.4(3) . . ? C134 C135 H135 119.8 . . ? C136 C135 H135 119.8 . . ? C135 C136 C131 119.4(3) . . ? C135 C136 H136 120.3 . . ? C131 C136 H136 120.3 . . ? P1 N2 P2 134.86(16) . . ? N2 P2 C221 110.42(13) . . ? N2 P2 C211 108.49(13) . . ? C221 P2 C211 109.28(12) . . ? N2 P2 C231 114.39(12) . . ? C221 P2 C231 107.85(12) . . ? C211 P2 C231 106.23(13) . . ? C216 C211 C212 120.0(3) . . ? C216 C211 P2 119.6(2) . . ? C212 C211 P2 120.4(2) . . ? C213 C212 C211 119.6(3) . . ? C213 C212 H212 120.2 . . ? C211 C212 H212 120.2 . . ? C214 C213 C212 120.3(3) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C215 C214 C213 120.1(3) . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 120.8(3) . . ? C214 C215 H215 119.6 . . ? C216 C215 H215 119.6 . . ? C215 C216 C211 119.3(3) . . ? C215 C216 H216 120.4 . . ? C211 C216 H216 120.4 . . ? C222 C221 C226 119.4(2) . . ? C222 C221 P2 120.1(2) . . ? C226 C221 P2 120.5(2) . . ? C223 C222 C221 119.7(3) . . ? C223 C222 H222 120.1 . . ? C221 C222 H222 120.1 . . ? C224 C223 C222 120.6(3) . . ? C224 C223 H223 119.7 . . ? C222 C223 H223 119.7 . . ? C223 C224 C225 119.9(3) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C226 C225 C224 120.4(3) . . ? C226 C225 H225 119.8 . . ? C224 C225 H225 119.8 . . ? C225 C226 C221 120.0(3) . . ? C225 C226 H226 120.0 . . ? C221 C226 H226 120.0 . . ? C236 C231 C232 119.7(3) . . ? C236 C231 P2 121.2(2) . . ? C232 C231 P2 118.7(2) . . ? C233 C232 C231 120.2(3) . . ? C233 C232 H232 119.9 . . ? C231 C232 H232 119.9 . . ? C232 C233 C234 119.7(3) . . ? C232 C233 H233 120.2 . . ? C234 C233 H233 120.2 . . ? C235 C234 C233 120.3(3) . . ? C235 C234 H234 119.9 . . ? C233 C234 H234 119.9 . . ? C234 C235 C236 120.1(3) . . ? C234 C235 H235 119.9 . . ? C236 C235 H235 119.9 . . ? C231 C236 C235 120.0(3) . . ? C231 C236 H236 120.0 . . ? C235 C236 H236 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.33 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.474 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.098 # Attachment '4b.cif' data_ipwt102 _database_code_depnum_ccdc_archive 'CCDC 614397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 N2 S4 Te' _chemical_formula_sum 'C10 H16 N2 S4 Te' _chemical_formula_weight 420.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.0940(11) _cell_length_b 11.7267(13) _cell_length_c 16.101(2) _cell_angle_alpha 90 _cell_angle_beta 92.147(10) _cell_angle_gamma 90 _cell_volume 1527.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9639 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.02 _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.476 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6382 _exptl_absorpt_correction_T_max 0.7576 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _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 'IPDS I (Stoe & Cie)' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 17701 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.02 _reflns_number_total 3635 _reflns_number_gt 2472 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0284P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3635 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Te1 Te 0.62435(3) 0.136769(18) 0.882006(19) 0.05231(10) Uani 1 1 d . . . C11 C 0.6365(5) 0.2488(3) 1.0582(3) 0.0486(9) Uani 1 1 d . . . S111 S 0.62396(17) 0.10510(8) 1.06050(8) 0.0701(3) Uani 1 1 d . . . S112 S 0.65251(14) 0.31892(8) 0.96412(7) 0.0596(3) Uani 1 1 d . . . N12 N 0.6355(4) 0.3118(2) 1.1265(2) 0.0546(8) Uani 1 1 d . . . C13 C 0.6435(6) 0.4376(3) 1.1279(3) 0.0719(13) Uani 1 1 d . . . H13A H 0.5552 0.4704 1.0932 0.129(6) Uiso 1 1 calc R . . H13B H 0.7488 0.4644 1.1087 0.129(6) Uiso 1 1 calc R . . C14 C 0.6240(10) 0.4673(5) 1.2162(4) 0.112(2) Uani 1 1 d . . . H14A H 0.7151 0.5155 1.2353 0.129(6) Uiso 1 1 calc R . . H14B H 0.5220 0.5094 1.2221 0.129(6) Uiso 1 1 calc R . . C15 C 0.6209(9) 0.3662(5) 1.2656(4) 0.1018(18) Uani 1 1 d . . . H15A H 0.5210 0.3647 1.2970 0.129(6) Uiso 1 1 calc R . . H15B H 0.7152 0.3655 1.3046 0.129(6) Uiso 1 1 calc R . . C16 C 0.6261(7) 0.2653(4) 1.2112(3) 0.0790(14) Uani 1 1 d . . . H16A H 0.7222 0.2187 1.2251 0.129(6) Uiso 1 1 calc R . . H16B H 0.5274 0.2193 1.2162 0.129(6) Uiso 1 1 calc R . . C21 C 0.6283(5) 0.1742(3) 0.6905(3) 0.0503(9) Uani 1 1 d . . . S211 S 0.64922(15) 0.27790(8) 0.76720(7) 0.0641(3) Uani 1 1 d . . . S212 S 0.61072(16) 0.03605(7) 0.71764(8) 0.0679(3) Uani 1 1 d . . . N22 N 0.6298(4) 0.2095(2) 0.6130(2) 0.0550(8) Uani 1 1 d . . . C23 C 0.6415(6) 0.3306(3) 0.5876(3) 0.0676(12) Uani 1 1 d . . . H23A H 0.7503 0.3613 0.6016 0.129(6) Uiso 1 1 calc R . . H23B H 0.5591 0.3765 0.6143 0.129(6) Uiso 1 1 calc R . . C24 C 0.6100(7) 0.3275(4) 0.4958(3) 0.0773(14) Uani 1 1 d . . . H24A H 0.6782 0.3834 0.4689 0.129(6) Uiso 1 1 calc R . . H24B H 0.4948 0.3443 0.4821 0.129(6) Uiso 1 1 calc R . . C25 C 0.6525(7) 0.2094(4) 0.4676(3) 0.0846(15) Uani 1 1 d . . . H25A H 0.7677 0.2050 0.4533 0.129(6) Uiso 1 1 calc R . . H25B H 0.5839 0.1876 0.4195 0.129(6) Uiso 1 1 calc R . . C26 C 0.6194(6) 0.1338(4) 0.5404(3) 0.0669(11) Uani 1 1 d . . . H26A H 0.5105 0.0996 0.5344 0.129(6) Uiso 1 1 calc R . . H26B H 0.7013 0.0736 0.5455 0.129(6) 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 Te1 0.05273(14) 0.03800(12) 0.06588(18) -0.00095(12) -0.00228(10) 0.00087(11) C11 0.045(2) 0.0400(17) 0.060(3) 0.0048(17) 0.0017(17) 0.0013(13) S111 0.0979(9) 0.0370(4) 0.0764(8) 0.0082(4) 0.0154(7) -0.0030(5) S112 0.0829(7) 0.0376(4) 0.0579(7) 0.0047(4) -0.0025(5) -0.0035(4) N12 0.062(2) 0.0442(15) 0.057(2) 0.0061(15) 0.0026(17) 0.0057(14) C13 0.095(3) 0.045(2) 0.076(3) -0.004(2) -0.002(3) 0.004(2) C14 0.173(7) 0.076(3) 0.088(4) -0.020(3) 0.018(4) 0.030(4) C15 0.126(5) 0.112(4) 0.068(4) -0.011(4) 0.006(3) -0.025(4) C16 0.102(4) 0.075(3) 0.061(3) 0.015(3) 0.016(3) 0.013(3) C21 0.052(2) 0.0368(15) 0.061(3) -0.0066(16) -0.0024(18) 0.0025(15) S211 0.0915(8) 0.0370(4) 0.0635(7) -0.0071(4) -0.0019(6) -0.0041(5) S212 0.0929(8) 0.0343(4) 0.0755(8) -0.0043(5) -0.0094(6) 0.0011(5) N22 0.062(2) 0.0372(14) 0.066(2) -0.0078(15) -0.0018(17) -0.0015(13) C23 0.087(3) 0.0474(19) 0.068(3) 0.0019(19) 0.000(2) -0.008(2) C24 0.104(4) 0.064(2) 0.063(3) 0.003(2) 0.000(3) -0.013(2) C25 0.099(4) 0.086(3) 0.070(3) -0.011(3) 0.014(3) -0.006(3) C26 0.078(3) 0.059(2) 0.064(3) -0.016(2) -0.001(2) 0.006(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 Te1 S211 2.4948(12) . ? Te1 S112 2.5179(10) . ? Te1 S212 2.8963(13) . ? Te1 S111 2.8979(14) . ? C11 N12 1.325(5) . ? C11 S111 1.688(3) . ? C11 S112 1.733(4) . ? N12 C16 1.472(6) . ? N12 C13 1.476(5) . ? C13 C14 1.478(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.428(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.474(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C21 N22 1.316(5) . ? C21 S212 1.686(4) . ? C21 S211 1.737(4) . ? N22 C26 1.467(5) . ? N22 C23 1.481(5) . ? C23 C24 1.491(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.501(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.502(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? 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 S211 Te1 S112 79.52(4) . . ? S211 Te1 S212 66.10(3) . . ? S112 Te1 S212 145.62(3) . . ? S211 Te1 S111 145.38(3) . . ? S112 Te1 S111 65.88(3) . . ? S212 Te1 S111 148.48(3) . . ? N12 C11 S111 122.4(3) . . ? N12 C11 S112 117.6(3) . . ? S111 C11 S112 119.9(2) . . ? C11 S111 Te1 81.27(15) . . ? C11 S112 Te1 92.76(13) . . ? C11 N12 C16 124.3(3) . . ? C11 N12 C13 124.6(4) . . ? C16 N12 C13 111.1(4) . . ? N12 C13 C14 104.1(4) . . ? N12 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? N12 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 109.0 . . ? C15 C14 C13 110.2(4) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 109.5(5) . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? N12 C16 C15 104.9(4) . . ? N12 C16 H16A 110.8 . . ? C15 C16 H16A 110.8 . . ? N12 C16 H16B 110.8 . . ? C15 C16 H16B 110.8 . . ? H16A C16 H16B 108.8 . . ? N22 C21 S212 123.5(3) . . ? N22 C21 S211 116.8(3) . . ? S212 C21 S211 119.7(3) . . ? C21 S211 Te1 93.10(14) . . ? C21 S212 Te1 81.03(15) . . ? C21 N22 C26 124.3(3) . . ? C21 N22 C23 124.4(3) . . ? C26 N22 C23 111.3(4) . . ? N22 C23 C24 103.8(3) . . ? N22 C23 H23A 111.0 . . ? C24 C23 H23A 111.0 . . ? N22 C23 H23B 111.0 . . ? C24 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C23 C24 C25 106.9(4) . . ? C23 C24 H24A 110.3 . . ? C25 C24 H24A 110.3 . . ? C23 C24 H24B 110.3 . . ? C25 C24 H24B 110.3 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C26 105.0(4) . . ? C24 C25 H25A 110.8 . . ? C26 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C26 C25 H25B 110.8 . . ? H25A C25 H25B 108.8 . . ? N22 C26 C25 104.9(4) . . ? N22 C26 H26A 110.8 . . ? C25 C26 H26A 110.8 . . ? N22 C26 H26B 110.8 . . ? C25 C26 H26B 110.8 . . ? H26A C26 H26B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.400 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.075 # Attachment '6c.cif' data_ipwt103 _database_code_depnum_ccdc_archive 'CCDC 614398' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H56 N4 S8 Te' _chemical_formula_sum 'C60 H56 N4 S8 Te' _chemical_formula_weight 1217.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 15.4060(15) _cell_length_b 15.4060(15) _cell_length_c 12.1612(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2886.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.12 _exptl_crystal_description polyhedron _exptl_crystal_colour yollow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7781 _exptl_absorpt_correction_T_max 0.9051 _exptl_absorpt_process_details ; The absorption correction (X-RED; Stoe & Cie, 2001) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999). ; _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 'IPDS I (Stoe & Cie)' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_reflns_number 32889 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.12 _reflns_number_total 3484 _reflns_number_gt 2203 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0366P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0011(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 3484 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 Te1 Te 1.0000 0.0000 1.0000 0.04460(15) Uani 1 4 d S . . S11 S 0.96141(8) 0.09594(8) 1.18483(11) 0.0564(3) Uani 1 1 d . . . S12 S 0.92945(9) 0.15886(8) 0.95927(11) 0.0576(3) Uani 1 1 d . . . C1 C 0.9348(3) 0.1787(3) 1.0978(4) 0.0486(11) Uani 1 1 d . . . N1 N 0.9210(3) 0.2596(2) 1.1384(3) 0.0523(10) Uani 1 1 d . . . C11 C 0.9329(4) 0.2790(3) 1.2550(5) 0.0601(14) Uani 1 1 d . . . H11A H 0.9259 0.2261 1.2972 0.073(8) Uiso 1 1 calc R . . H11B H 0.8882 0.3195 1.2783 0.073(8) Uiso 1 1 calc R . . C12 C 1.0213(3) 0.3178(3) 1.2794(5) 0.0628(15) Uani 1 1 d . . . C13 C 1.0312(5) 0.3725(5) 1.3681(7) 0.130(4) Uani 1 1 d . . . H13 H 0.9830 0.3885 1.4094 0.139(9) Uiso 1 1 calc R . . C14 C 1.1131(6) 0.4040(6) 1.3964(10) 0.157(4) Uani 1 1 d . . . H14 H 1.1184 0.4394 1.4580 0.139(9) Uiso 1 1 calc R . . C15 C 1.1837(5) 0.3853(5) 1.3383(8) 0.102(3) Uani 1 1 d . . . H15 H 1.2374 0.4094 1.3557 0.139(9) Uiso 1 1 calc R . . C16 C 1.1745(5) 0.3302(5) 1.2535(7) 0.0917(18) Uani 1 1 d . . . H16 H 1.2233 0.3144 1.2133 0.139(9) Uiso 1 1 calc R . . C17 C 1.0953(4) 0.2964(4) 1.2242(6) 0.082(2) Uani 1 1 d . . . H17 H 1.0921 0.2580 1.1654 0.139(9) Uiso 1 1 calc R . . C21 C 0.8987(3) 0.3333(3) 1.0680(5) 0.0610(14) Uani 1 1 d . . . H21A H 0.9135 0.3192 0.9925 0.073(8) Uiso 1 1 calc R . . H21B H 0.9332 0.3831 1.0897 0.073(8) Uiso 1 1 calc R . . C22 C 0.8040(4) 0.3572(3) 1.0737(5) 0.0644(15) Uani 1 1 d . . . C23 C 0.7436(4) 0.3108(4) 1.0150(7) 0.0807(18) Uani 1 1 d . . . H23 H 0.7615 0.2642 0.9719 0.139(9) Uiso 1 1 calc R . . C24 C 0.6567(4) 0.3323(5) 1.0192(8) 0.102(2) Uani 1 1 d . . . H24 H 0.6168 0.3010 0.9777 0.139(9) Uiso 1 1 calc R . . C25 C 0.6290(6) 0.3993(6) 1.0839(7) 0.116(3) Uani 1 1 d . . . H25 H 0.5703 0.4133 1.0877 0.139(9) Uiso 1 1 calc R . . C26 C 0.6888(6) 0.4457(6) 1.1432(7) 0.114(3) Uani 1 1 d . . . H26 H 0.6703 0.4912 1.1876 0.139(9) Uiso 1 1 calc R . . C27 C 0.7753(5) 0.4260(4) 1.1380(6) 0.093(2) Uani 1 1 d . . . H27 H 0.8151 0.4588 1.1777 0.139(9) 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 Te1 0.04052(16) 0.04052(16) 0.0528(3) 0.000 0.000 0.000 S11 0.0641(7) 0.0505(7) 0.0545(8) -0.0033(6) 0.0024(6) -0.0012(5) S12 0.0694(8) 0.0474(6) 0.0561(8) -0.0027(6) -0.0006(6) 0.0107(6) C1 0.041(2) 0.057(3) 0.048(3) 0.003(2) 0.006(2) -0.008(2) N1 0.058(2) 0.040(2) 0.059(3) -0.0079(19) 0.007(2) 0.0020(18) C11 0.064(3) 0.056(3) 0.061(4) -0.014(3) 0.016(3) -0.004(3) C12 0.072(4) 0.050(3) 0.066(3) -0.007(2) 0.010(3) -0.012(2) C13 0.096(6) 0.148(7) 0.147(8) -0.096(6) 0.035(5) -0.035(5) C14 0.125(8) 0.159(9) 0.186(10) -0.104(8) 0.006(7) -0.054(7) C15 0.089(5) 0.092(5) 0.127(8) -0.003(5) -0.005(5) -0.033(4) C16 0.073(5) 0.095(6) 0.107(5) -0.016(5) 0.003(4) -0.019(3) C17 0.066(4) 0.090(5) 0.090(6) -0.016(4) 0.011(4) -0.017(4) C21 0.068(3) 0.043(3) 0.072(4) -0.002(3) 0.009(3) -0.001(2) C22 0.068(3) 0.049(3) 0.076(4) 0.003(3) 0.014(3) 0.009(3) C23 0.072(3) 0.082(3) 0.088(5) 0.004(4) 0.006(4) 0.012(3) C24 0.072(4) 0.118(6) 0.116(7) 0.026(6) 0.000(5) 0.011(3) C25 0.085(5) 0.156(9) 0.105(6) 0.043(6) 0.030(5) 0.050(6) C26 0.122(7) 0.112(6) 0.108(7) 0.006(5) 0.031(5) 0.063(6) C27 0.104(5) 0.073(4) 0.102(5) -0.016(4) 0.019(4) 0.033(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 Te1 S12 2.7232(12) 2_755 ? Te1 S12 2.7232(12) 8_667 ? Te1 S12 2.7232(12) 7_647 ? Te1 S12 2.7232(12) . ? Te1 S11 2.7551(13) 7_647 ? Te1 S11 2.7551(13) . ? Te1 S11 2.7551(13) 8_667 ? Te1 S11 2.7551(13) 2_755 ? S11 C1 1.708(5) . ? S12 C1 1.714(5) . ? C1 N1 1.356(6) . ? N1 C11 1.460(7) . ? N1 C21 1.463(6) . ? C11 C12 1.517(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.363(8) . ? C12 C13 1.378(8) . ? C13 C14 1.395(10) . ? C13 H13 0.9300 . ? C14 C15 1.329(11) . ? C14 H14 0.9300 . ? C15 C16 1.343(10) . ? C15 H15 0.9300 . ? C16 C17 1.373(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C21 C22 1.506(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.373(8) . ? C22 C27 1.390(8) . ? C23 C24 1.380(8) . ? C23 H23 0.9300 . ? C24 C25 1.368(12) . ? C24 H24 0.9300 . ? C25 C26 1.370(11) . ? C25 H25 0.9300 . ? C26 C27 1.368(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 S12 Te1 S12 91.896(10) 2_755 8_667 ? S12 Te1 S12 91.896(10) 2_755 7_647 ? S12 Te1 S12 159.04(6) 8_667 7_647 ? S12 Te1 S12 159.04(6) 2_755 . ? S12 Te1 S12 91.896(10) 8_667 . ? S12 Te1 S12 91.896(10) 7_647 . ? S12 Te1 S11 82.63(4) 2_755 7_647 ? S12 Te1 S11 135.78(4) 8_667 7_647 ? S12 Te1 S11 65.17(4) 7_647 7_647 ? S12 Te1 S11 80.29(4) . 7_647 ? S12 Te1 S11 135.78(4) 2_755 . ? S12 Te1 S11 80.29(4) 8_667 . ? S12 Te1 S11 82.63(4) 7_647 . ? S12 Te1 S11 65.17(4) . . ? S11 Te1 S11 131.73(3) 7_647 . ? S12 Te1 S11 80.29(4) 2_755 8_667 ? S12 Te1 S11 65.17(4) 8_667 8_667 ? S12 Te1 S11 135.78(4) 7_647 8_667 ? S12 Te1 S11 82.63(4) . 8_667 ? S11 Te1 S11 70.66(6) 7_647 8_667 ? S11 Te1 S11 131.73(4) . 8_667 ? S12 Te1 S11 65.17(4) 2_755 2_755 ? S12 Te1 S11 82.63(4) 8_667 2_755 ? S12 Te1 S11 80.29(4) 7_647 2_755 ? S12 Te1 S11 135.78(4) . 2_755 ? S11 Te1 S11 131.73(4) 7_647 2_755 ? S11 Te1 S11 70.66(6) . 2_755 ? S11 Te1 S11 131.73(3) 8_667 2_755 ? C1 S11 Te1 86.96(17) . . ? C1 S12 Te1 87.87(17) . . ? N1 C1 S11 119.9(4) . . ? N1 C1 S12 121.0(4) . . ? S11 C1 S12 119.1(3) . . ? C1 N1 C11 121.5(4) . . ? C1 N1 C21 122.4(4) . . ? C11 N1 C21 116.0(4) . . ? N1 C11 C12 112.5(4) . . ? N1 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N1 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C17 C12 C13 116.2(6) . . ? C17 C12 C11 124.1(5) . . ? C13 C12 C11 119.5(5) . . ? C12 C13 C14 120.4(7) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 122.3(8) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 117.3(7) . . ? C14 C15 H15 121.4 . . ? C16 C15 H15 121.4 . . ? C15 C16 C17 122.2(7) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C12 C17 C16 121.5(7) . . ? C12 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? N1 C21 C22 113.0(4) . . ? N1 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N1 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C27 118.3(6) . . ? C23 C22 C21 120.3(5) . . ? C27 C22 C21 121.3(6) . . ? C22 C23 C24 120.9(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 120.4(9) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.1(8) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 121.0(8) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 120.3(7) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.356 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.063