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 'Wolf-Walther du Mont' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Technische Universitat Carolo-Wilhelmina Braunschweig Postfach 3329 Braunschweig 38023 GERMANY ; _publ_contact_author_email W.DU-MONT@TU-BS.DE _publ_section_title ; Telluroselenophosphonium Ions: their Unusual Soft-Soft Interactions with Iodotellurate Anions ; loop_ _publ_author_name 'W.-W.du Mont' 'Cristian Hrib' 'Jorg Jeske' 'Peter G. Jones' data_bujor _database_code_depnum_ccdc_archive 'CCDC 644166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H39 I2 P Se Te2' _chemical_formula_weight 958.49 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.1191(6) _cell_length_b 22.0684(7) _cell_length_c 14.4059(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.726(3) _cell_angle_gamma 90.00 _cell_volume 3125.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7278 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'cut tablet' _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 5.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5797 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33390 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.53 _reflns_number_total 9488 _reflns_number_gt 9073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'methyls rigid and other riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(6) _refine_ls_number_reflns 9488 _refine_ls_number_parameters 290 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0385 _refine_ls_wR_factor_gt 0.0382 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Te2 Te 1.016645(15) 0.125020(7) 0.577654(12) 0.02080(3) Uani 1 1 d . . . Te1 Te 1.112712(15) 0.028293(6) 0.443872(12) 0.01910(3) Uani 1 1 d . . . I2 I 0.848476(16) 0.054120(9) 0.674773(13) 0.02951(4) Uani 1 1 d . . . I1 I 1.188968(19) 0.195448(8) 0.475575(15) 0.03402(5) Uani 1 1 d . . . Se1 Se 1.19842(2) -0.046568(11) 0.325358(18) 0.01971(5) Uani 1 1 d . . . P1 P 1.41943(6) -0.06014(3) 0.38465(4) 0.01576(11) Uani 1 1 d . . . C1 C 1.4444(3) -0.08485(12) 0.51040(18) 0.0245(5) Uani 1 1 d . . . H1 H 1.4064 -0.0514 0.5430 0.029 Uiso 1 1 calc R . . C2 C 1.3620(3) -0.14109(14) 0.5230(2) 0.0359(7) Uani 1 1 d . . . H2A H 1.4087 -0.1774 0.5080 0.043 Uiso 1 1 calc R . . H2B H 1.2714 -0.1386 0.4798 0.043 Uiso 1 1 calc R . . H2C H 1.3533 -0.1433 0.5892 0.043 Uiso 1 1 calc R . . C3 C 1.5939(3) -0.09196(15) 0.5672(2) 0.0340(7) Uani 1 1 d . . . H3A H 1.5966 -0.0980 0.6350 0.041 Uiso 1 1 calc R . . H3B H 1.6450 -0.0553 0.5596 0.041 Uiso 1 1 calc R . . H3C H 1.6347 -0.1270 0.5429 0.041 Uiso 1 1 calc R . . C4 C 1.5143(3) 0.01324(11) 0.38350(19) 0.0208(5) Uani 1 1 d . . . C5 C 1.4477(3) 0.05008(12) 0.2931(2) 0.0323(7) Uani 1 1 d . . . H5A H 1.3534 0.0596 0.2940 0.039 Uiso 1 1 calc R . . H5B H 1.4491 0.0262 0.2360 0.039 Uiso 1 1 calc R . . H5C H 1.4985 0.0878 0.2921 0.039 Uiso 1 1 calc R . . C6 C 1.5040(3) 0.05117(12) 0.4700(2) 0.0281(6) Uani 1 1 d . . . H6A H 1.5479 0.0905 0.4672 0.034 Uiso 1 1 calc R . . H6B H 1.5494 0.0300 0.5286 0.034 Uiso 1 1 calc R . . H6C H 1.4080 0.0574 0.4696 0.034 Uiso 1 1 calc R . . C7 C 1.6642(3) 0.00276(12) 0.3845(2) 0.0272(6) Uani 1 1 d . . . H7A H 1.7111 0.0419 0.3881 0.033 Uiso 1 1 calc R . . H7B H 1.6708 -0.0183 0.3259 0.033 Uiso 1 1 calc R . . H7C H 1.7068 -0.0220 0.4401 0.033 Uiso 1 1 calc R . . C8 C 1.4623(3) -0.11989(11) 0.30363(19) 0.0212(5) Uani 1 1 d . . . C9 C 1.6056(3) -0.14589(12) 0.3432(2) 0.0292(6) Uani 1 1 d . . . H9A H 1.6286 -0.1736 0.2962 0.035 Uiso 1 1 calc R . . H9B H 1.6078 -0.1680 0.4026 0.035 Uiso 1 1 calc R . . H9C H 1.6718 -0.1127 0.3561 0.035 Uiso 1 1 calc R . . C10 C 1.3597(3) -0.17251(12) 0.2951(2) 0.0307(6) Uani 1 1 d . . . H10A H 1.2668 -0.1565 0.2758 0.037 Uiso 1 1 calc R . . H10B H 1.3724 -0.1930 0.3570 0.037 Uiso 1 1 calc R . . H10C H 1.3746 -0.2015 0.2470 0.037 Uiso 1 1 calc R . . C11 C 1.4529(3) -0.09322(13) 0.2036(2) 0.0277(6) Uani 1 1 d . . . H11A H 1.5257 -0.0635 0.2069 0.033 Uiso 1 1 calc R . . H11B H 1.3645 -0.0734 0.1808 0.033 Uiso 1 1 calc R . . H11C H 1.4625 -0.1258 0.1595 0.033 Uiso 1 1 calc R . . C12 C 1.0570(3) -0.04670(11) 0.51804(19) 0.0196(5) Uani 1 1 d . . . C13 C 0.9683(2) -0.09088(11) 0.47067(18) 0.0194(5) Uani 1 1 d . . . H13 H 0.9266 -0.0865 0.4046 0.023 Uiso 1 1 calc R . . C14 C 0.9408(3) -0.14157(12) 0.5203(2) 0.0238(5) Uani 1 1 d . . . H14 H 0.8807 -0.1718 0.4875 0.029 Uiso 1 1 calc R . . C15 C 0.9997(3) -0.14869(12) 0.6170(2) 0.0249(5) Uani 1 1 d . . . C16 C 1.0852(3) -0.10360(13) 0.6636(2) 0.0288(6) Uani 1 1 d . . . H16 H 1.1240 -0.1072 0.7302 0.035 Uiso 1 1 calc R . . C17 C 1.1155(3) -0.05318(12) 0.6148(2) 0.0264(5) Uani 1 1 d . . . H17 H 1.1762 -0.0232 0.6477 0.032 Uiso 1 1 calc R . . C18 C 0.9705(4) -0.20387(13) 0.6697(2) 0.0381(7) Uani 1 1 d . . . H18A H 1.0223 -0.2383 0.6540 0.046 Uiso 1 1 calc R . . H18B H 0.8731 -0.2130 0.6509 0.046 Uiso 1 1 calc R . . H18C H 0.9972 -0.1963 0.7386 0.046 Uiso 1 1 calc R . . C19 C 0.8401(3) 0.16413(11) 0.4858(2) 0.0233(5) Uani 1 1 d . . . C20 C 0.7494(3) 0.19504(13) 0.5261(2) 0.0295(6) Uani 1 1 d . . . H20 H 0.7645 0.1982 0.5935 0.035 Uiso 1 1 calc R . . C21 C 0.6343(3) 0.22183(13) 0.4663(2) 0.0365(7) Uani 1 1 d . . . H21 H 0.5714 0.2429 0.4940 0.044 Uiso 1 1 calc R . . C22 C 0.6108(3) 0.21808(12) 0.3681(2) 0.0310(6) Uani 1 1 d . . . C23 C 0.7039(3) 0.18712(12) 0.3291(2) 0.0294(6) Uani 1 1 d . . . H23 H 0.6896 0.1845 0.2616 0.035 Uiso 1 1 calc R . . C24 C 0.8186(3) 0.15977(12) 0.3874(2) 0.0258(5) Uani 1 1 d . . . H24 H 0.8812 0.1384 0.3599 0.031 Uiso 1 1 calc R . . C25 C 0.4866(3) 0.24845(17) 0.3044(3) 0.0476(9) Uani 1 1 d . . . H25A H 0.4046 0.2355 0.3239 0.057 Uiso 1 1 calc R . . H25B H 0.4795 0.2368 0.2378 0.057 Uiso 1 1 calc R . . H25C H 0.4960 0.2926 0.3107 0.057 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 Te2 0.01877(7) 0.02126(7) 0.02184(8) -0.00266(6) 0.00375(5) 0.00018(6) Te1 0.01807(7) 0.01726(7) 0.02286(8) 0.00256(7) 0.00658(6) 0.00077(6) I2 0.01899(7) 0.04888(11) 0.02068(8) 0.00439(8) 0.00473(6) -0.00306(7) I1 0.02886(9) 0.02636(8) 0.04504(12) 0.01029(8) 0.00520(8) -0.00750(7) Se1 0.01653(11) 0.02397(12) 0.01849(12) -0.00119(9) 0.00385(9) 0.00168(9) P1 0.0163(3) 0.0158(3) 0.0153(3) -0.0003(2) 0.0041(2) -0.0001(2) C1 0.0268(13) 0.0305(13) 0.0169(12) 0.0054(10) 0.0067(10) 0.0030(10) C2 0.0379(16) 0.0362(15) 0.0365(17) 0.0167(13) 0.0146(13) 0.0029(12) C3 0.0296(15) 0.0489(18) 0.0212(14) 0.0076(12) 0.0015(11) 0.0057(13) C4 0.0200(11) 0.0183(11) 0.0232(13) -0.0015(9) 0.0037(9) -0.0036(9) C5 0.0388(16) 0.0204(12) 0.0328(16) 0.0092(11) -0.0010(12) -0.0058(11) C6 0.0211(12) 0.0254(13) 0.0369(16) -0.0124(11) 0.0055(11) -0.0021(10) C7 0.0218(12) 0.0277(14) 0.0341(15) -0.0047(11) 0.0109(10) -0.0069(10) C8 0.0214(11) 0.0193(11) 0.0234(13) -0.0058(9) 0.0062(9) 0.0012(9) C9 0.0258(13) 0.0233(12) 0.0382(16) -0.0041(11) 0.0069(11) 0.0058(10) C10 0.0314(14) 0.0195(12) 0.0417(17) -0.0093(12) 0.0096(12) -0.0039(10) C11 0.0294(14) 0.0321(14) 0.0230(14) -0.0055(11) 0.0086(11) 0.0021(11) C12 0.0199(11) 0.0181(11) 0.0220(13) 0.0003(9) 0.0075(9) 0.0031(9) C13 0.0167(11) 0.0222(11) 0.0181(12) 0.0027(9) 0.0018(9) 0.0022(9) C14 0.0213(12) 0.0231(12) 0.0271(14) -0.0009(10) 0.0056(10) -0.0049(9) C15 0.0286(13) 0.0233(12) 0.0241(13) 0.0033(10) 0.0091(10) -0.0003(10) C16 0.0395(15) 0.0293(14) 0.0162(13) 0.0023(10) 0.0039(11) -0.0039(12) C17 0.0315(14) 0.0253(13) 0.0211(13) -0.0029(10) 0.0039(10) -0.0065(10) C18 0.056(2) 0.0286(15) 0.0311(17) 0.0044(12) 0.0125(14) -0.0121(14) C19 0.0225(12) 0.0200(12) 0.0256(14) -0.0013(10) 0.0022(10) -0.0002(9) C20 0.0298(14) 0.0277(13) 0.0302(15) -0.0033(11) 0.0057(11) 0.0080(11) C21 0.0318(16) 0.0331(15) 0.044(2) -0.0005(13) 0.0085(13) 0.0108(12) C22 0.0250(14) 0.0239(13) 0.0411(18) 0.0060(12) 0.0021(12) -0.0009(10) C23 0.0304(14) 0.0282(13) 0.0267(14) 0.0048(11) 0.0009(11) -0.0060(11) C24 0.0229(13) 0.0240(12) 0.0301(14) 0.0009(11) 0.0055(10) -0.0033(10) C25 0.0368(18) 0.050(2) 0.050(2) 0.0133(17) -0.0018(16) 0.0133(15) _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 Te2 C19 2.137(3) . ? Te2 I2 2.9037(3) . ? Te2 I1 2.9725(3) . ? Te2 Te1 3.1788(2) . ? Te1 C12 2.118(2) . ? Te1 Se1 2.6644(3) . ? Se1 P1 2.2169(6) . ? Se1 I2 3.6916(4) 2_554 ? Se1 Te2 3.9999(4) 2_554 ? P1 C1 1.851(3) . ? P1 C8 1.879(2) . ? P1 C4 1.885(2) . ? C1 C2 1.530(4) . ? C1 C3 1.547(4) . ? C4 C6 1.525(4) . ? C4 C7 1.531(4) . ? C4 C5 1.547(4) . ? C8 C11 1.538(4) . ? C8 C9 1.538(4) . ? C8 C10 1.543(4) . ? C12 C17 1.386(4) . ? C12 C13 1.390(4) . ? C13 C14 1.391(4) . ? C14 C15 1.388(4) . ? C15 C16 1.383(4) . ? C15 C18 1.501(4) . ? C16 C17 1.389(4) . ? C19 C20 1.377(4) . ? C19 C24 1.386(4) . ? C20 C21 1.403(4) . ? C21 C22 1.381(5) . ? C22 C23 1.386(4) . ? C22 C25 1.524(4) . ? C23 C24 1.398(4) . ? 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 C19 Te2 I2 90.93(7) . . ? C19 Te2 I1 89.15(7) . . ? I2 Te2 I1 178.818(8) . . ? C19 Te2 Te1 103.12(7) . . ? I2 Te2 Te1 103.225(7) . . ? I1 Te2 Te1 75.611(7) . . ? C12 Te1 Se1 90.28(7) . . ? C12 Te1 Te2 93.59(7) . . ? Se1 Te1 Te2 176.135(9) . . ? P1 Se1 Te1 106.791(19) . . ? P1 Se1 I2 163.673(19) . 2_554 ? Te1 Se1 I2 89.533(8) . 2_554 ? P1 Se1 Te2 119.576(19) . 2_554 ? Te1 Se1 Te2 133.577(9) . 2_554 ? I2 Se1 Te2 44.133(5) 2_554 2_554 ? C1 P1 C8 113.78(12) . . ? C1 P1 C4 108.07(12) . . ? C8 P1 C4 113.86(12) . . ? C1 P1 Se1 107.93(9) . . ? C8 P1 Se1 102.47(8) . . ? C4 P1 Se1 110.49(8) . . ? C2 C1 C3 110.3(2) . . ? C2 C1 P1 113.8(2) . . ? C3 C1 P1 115.87(19) . . ? C6 C4 C7 109.6(2) . . ? C6 C4 C5 107.4(2) . . ? C7 C4 C5 108.7(2) . . ? C6 C4 P1 109.31(19) . . ? C7 C4 P1 112.07(17) . . ? C5 C4 P1 109.74(17) . . ? C11 C8 C9 109.5(2) . . ? C11 C8 C10 108.8(2) . . ? C9 C8 C10 107.8(2) . . ? C11 C8 P1 109.95(17) . . ? C9 C8 P1 111.58(18) . . ? C10 C8 P1 109.13(18) . . ? C17 C12 C13 119.6(2) . . ? C17 C12 Te1 119.12(19) . . ? C13 C12 Te1 121.25(19) . . ? C12 C13 C14 119.8(2) . . ? C15 C14 C13 121.1(2) . . ? C16 C15 C14 118.4(2) . . ? C16 C15 C18 120.9(3) . . ? C14 C15 C18 120.7(3) . . ? C15 C16 C17 121.2(3) . . ? C12 C17 C16 119.9(2) . . ? C20 C19 C24 120.4(3) . . ? C20 C19 Te2 118.9(2) . . ? C24 C19 Te2 120.7(2) . . ? C19 C20 C21 119.3(3) . . ? C22 C21 C20 121.3(3) . . ? C21 C22 C23 118.5(3) . . ? C21 C22 C25 120.5(3) . . ? C23 C22 C25 121.0(3) . . ? C22 C23 C24 121.0(3) . . ? C19 C24 C23 119.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 Te2 Te1 C12 -109.85(10) . . . . ? I2 Te2 Te1 C12 -15.73(7) . . . . ? I1 Te2 Te1 C12 164.48(7) . . . . ? C19 Te2 Te1 Se1 71.16(15) . . . . ? I2 Te2 Te1 Se1 165.29(12) . . . . ? I1 Te2 Te1 Se1 -14.51(13) . . . . ? C12 Te1 Se1 P1 -93.81(7) . . . . ? Te2 Te1 Se1 P1 85.17(13) . . . . ? C12 Te1 Se1 I2 85.88(7) . . . 2_554 ? Te2 Te1 Se1 I2 -95.13(13) . . . 2_554 ? C12 Te1 Se1 Te2 89.00(7) . . . 2_554 ? Te2 Te1 Se1 Te2 -92.01(13) . . . 2_554 ? Te1 Se1 P1 C1 53.34(9) . . . . ? I2 Se1 P1 C1 -125.56(11) 2_554 . . . ? Te2 Se1 P1 C1 -129.00(9) 2_554 . . . ? Te1 Se1 P1 C8 173.71(8) . . . . ? I2 Se1 P1 C8 -5.19(12) 2_554 . . . ? Te2 Se1 P1 C8 -8.63(9) 2_554 . . . ? Te1 Se1 P1 C4 -64.63(9) . . . . ? I2 Se1 P1 C4 116.47(10) 2_554 . . . ? Te2 Se1 P1 C4 113.03(9) 2_554 . . . ? C8 P1 C1 C2 -57.8(2) . . . . ? C4 P1 C1 C2 174.7(2) . . . . ? Se1 P1 C1 C2 55.2(2) . . . . ? C8 P1 C1 C3 71.6(2) . . . . ? C4 P1 C1 C3 -55.9(2) . . . . ? Se1 P1 C1 C3 -175.4(2) . . . . ? C1 P1 C4 C6 -36.6(2) . . . . ? C8 P1 C4 C6 -164.04(17) . . . . ? Se1 P1 C4 C6 81.30(18) . . . . ? C1 P1 C4 C7 85.1(2) . . . . ? C8 P1 C4 C7 -42.3(2) . . . . ? Se1 P1 C4 C7 -156.99(17) . . . . ? C1 P1 C4 C5 -154.1(2) . . . . ? C8 P1 C4 C5 78.5(2) . . . . ? Se1 P1 C4 C5 -36.2(2) . . . . ? C1 P1 C8 C11 -174.08(17) . . . . ? C4 P1 C8 C11 -49.6(2) . . . . ? Se1 P1 C8 C11 69.69(18) . . . . ? C1 P1 C8 C9 -52.4(2) . . . . ? C4 P1 C8 C9 72.0(2) . . . . ? Se1 P1 C8 C9 -168.66(17) . . . . ? C1 P1 C8 C10 66.6(2) . . . . ? C4 P1 C8 C10 -168.91(18) . . . . ? Se1 P1 C8 C10 -49.58(19) . . . . ? Se1 Te1 C12 C17 121.1(2) . . . . ? Te2 Te1 C12 C17 -58.8(2) . . . . ? Se1 Te1 C12 C13 -55.72(19) . . . . ? Te2 Te1 C12 C13 124.35(19) . . . . ? C17 C12 C13 C14 -1.1(4) . . . . ? Te1 C12 C13 C14 175.78(19) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C13 C14 C15 C18 -179.3(3) . . . . ? C14 C15 C16 C17 -2.0(4) . . . . ? C18 C15 C16 C17 178.3(3) . . . . ? C13 C12 C17 C16 0.0(4) . . . . ? Te1 C12 C17 C16 -176.9(2) . . . . ? C15 C16 C17 C12 1.5(4) . . . . ? I2 Te2 C19 C20 57.6(2) . . . . ? I1 Te2 C19 C20 -123.6(2) . . . . ? Te1 Te2 C19 C20 161.4(2) . . . . ? I2 Te2 C19 C24 -123.9(2) . . . . ? I1 Te2 C19 C24 54.9(2) . . . . ? Te1 Te2 C19 C24 -20.1(2) . . . . ? C24 C19 C20 C21 0.4(4) . . . . ? Te2 C19 C20 C21 178.9(2) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? C20 C21 C22 C23 -0.1(5) . . . . ? C20 C21 C22 C25 -178.9(3) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C25 C22 C23 C24 179.4(3) . . . . ? C20 C19 C24 C23 0.1(4) . . . . ? Te2 C19 C24 C23 -178.36(19) . . . . ? C22 C23 C24 C19 -0.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.674 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.078 # Attachment '5.cif.CIF' data_alun _database_code_depnum_ccdc_archive 'CCDC 644167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H41 Cl2 I8 P2 Se2 Te3' _chemical_formula_weight 1958.28 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' I I -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9947(8) _cell_length_b 12.4377(10) _cell_length_c 16.7112(14) _cell_angle_alpha 90.470(3) _cell_angle_beta 92.610(3) _cell_angle_gamma 92.474(3) _cell_volume 2280.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7943 _cell_measurement_theta_min 60 _cell_measurement_theta_max 2 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734 _exptl_absorpt_coefficient_mu 9.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3129 _exptl_absorpt_correction_T_max 0.4625 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49396 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 30.52 _reflns_number_total 13835 _reflns_number_gt 10090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0451P)^2^+5.9270P] 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 'methyls rigid and other riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13835 _refine_ls_number_parameters 331 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.009 _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 0.62119(4) 0.85613(3) 0.318990(19) 0.02428(8) Uani 1 1 d . . . Te2 Te 0.32615(3) 0.97251(3) 0.04094(2) 0.01868(7) Uani 1 1 d . . . Te3 Te 0.22224(3) 0.76267(3) 0.255487(19) 0.02345(8) Uani 1 1 d . . . I1 I 0.73936(4) 1.05880(3) 0.34603(2) 0.03044(9) Uani 1 1 d . . . I2 I 0.27996(4) 0.95006(3) -0.12216(2) 0.03011(9) Uani 1 1 d . . . I3 I 0.45974(4) 0.63777(3) 0.28825(3) 0.03456(10) Uani 1 1 d . . . I4 I 0.01149(4) 0.88008(3) 0.22334(2) 0.03422(9) Uani 1 1 d . . . I5 I 0.21961(6) 0.79838(4) 0.42538(2) 0.05059(13) Uani 1 1 d . . . I6 I 0.08340(4) 0.56512(3) 0.26726(3) 0.03914(11) Uani 1 1 d . . . I7 I 0.24549(4) 0.71703(3) 0.07815(2) 0.02469(8) Uani 1 1 d . . . I8 I 0.37517(4) 0.97277(3) 0.23853(2) 0.02629(8) Uani 1 1 d . . . Se1 Se 0.79393(6) 0.75005(6) 0.38355(3) 0.03444(15) Uani 1 1 d . . . Se2 Se 0.40637(5) 1.16905(5) 0.03201(5) 0.03625(16) Uani 1 1 d . . . P1 P 0.74656(15) 0.73322(14) 0.51108(9) 0.0309(3) Uani 1 1 d . . . P2 P 0.24564(12) 1.26962(10) 0.04328(8) 0.0189(3) Uani 1 1 d . . . C11 C 0.8703(10) 0.8018(9) 0.5688(5) 0.075(3) Uani 1 1 d U . . H11 H 0.9432 0.7614 0.5549 0.090 Uiso 1 1 calc R . . C12 C 0.9033(13) 0.9089(9) 0.5504(7) 0.108(5) Uani 1 1 d U . . H12A H 0.8344 0.9545 0.5587 0.129 Uiso 1 1 calc R . . H12B H 0.9256 0.9130 0.4944 0.129 Uiso 1 1 calc R . . H12C H 0.9730 0.9338 0.5854 0.129 Uiso 1 1 calc R . . C13 C 0.8613(9) 0.7830(9) 0.6604(4) 0.075(3) Uani 1 1 d U . . H13A H 0.9415 0.7974 0.6873 0.091 Uiso 1 1 calc R . . H13B H 0.8342 0.7082 0.6696 0.091 Uiso 1 1 calc R . . H13C H 0.8027 0.8315 0.6820 0.091 Uiso 1 1 calc R . . C14 C 0.7518(7) 0.5879(7) 0.5309(5) 0.0514(19) Uani 1 1 d U . . H14 H 0.7326 0.5761 0.5882 0.062 Uiso 1 1 calc R . . C15 C 0.6578(9) 0.5236(6) 0.4789(6) 0.064(2) Uani 1 1 d U . . H15A H 0.6811 0.5258 0.4230 0.077 Uiso 1 1 calc R . . H15B H 0.5779 0.5546 0.4832 0.077 Uiso 1 1 calc R . . H15C H 0.6537 0.4488 0.4969 0.077 Uiso 1 1 calc R . . C16 C 0.8782(8) 0.5469(8) 0.5186(6) 0.069(3) Uani 1 1 d U . . H16A H 0.8809 0.4718 0.5358 0.083 Uiso 1 1 calc R . . H16B H 0.9390 0.5909 0.5503 0.083 Uiso 1 1 calc R . . H16C H 0.8960 0.5514 0.4617 0.083 Uiso 1 1 calc R . . C17 C 0.5912(6) 0.7712(5) 0.5301(3) 0.0332(13) Uani 1 1 d U . . H17 H 0.5385 0.7460 0.4827 0.040 Uiso 1 1 calc R . . C18 C 0.5811(8) 0.8930(6) 0.5356(4) 0.050(2) Uani 1 1 d U . . H18A H 0.4952 0.9108 0.5298 0.060 Uiso 1 1 calc R . . H18B H 0.6265 0.9273 0.4929 0.060 Uiso 1 1 calc R . . H18C H 0.6152 0.9190 0.5878 0.060 Uiso 1 1 calc R . . C19 C 0.5398(7) 0.7145(7) 0.6040(4) 0.0461(17) Uani 1 1 d U . . C21 C 0.1879(6) 1.3135(5) -0.0559(3) 0.0328(13) Uani 1 1 d U . . H21 H 0.1301 1.2548 -0.0771 0.039 Uiso 1 1 calc R . . C22 C 0.2872(8) 1.3271(6) -0.1173(4) 0.0518(19) Uani 1 1 d U . . H22A H 0.2495 1.3437 -0.1698 0.062 Uiso 1 1 calc R . . H22B H 0.3307 1.2602 -0.1212 0.062 Uiso 1 1 calc R . . H22C H 0.3448 1.3860 -0.1002 0.062 Uiso 1 1 calc R . . C23 C 0.1132(7) 1.4135(6) -0.0478(4) 0.0456(17) Uani 1 1 d U . . H23A H 0.1668 1.4743 -0.0290 0.055 Uiso 1 1 calc R . . H23B H 0.0499 1.3997 -0.0093 0.055 Uiso 1 1 calc R . . H23C H 0.0750 1.4305 -0.1001 0.055 Uiso 1 1 calc R . . C24 C 0.3034(5) 1.3841(4) 0.1060(3) 0.0217(10) Uani 1 1 d U . . H24 H 0.2348 1.4330 0.1132 0.026 Uiso 1 1 calc R . . C25 C 0.3458(6) 1.3441(5) 0.1888(3) 0.0344(14) Uani 1 1 d U . . H25A H 0.4217 1.3064 0.1843 0.041 Uiso 1 1 calc R . . H25B H 0.2830 1.2947 0.2093 0.041 Uiso 1 1 calc R . . H25C H 0.3599 1.4056 0.2256 0.041 Uiso 1 1 calc R . . C26 C 0.4056(5) 1.4479(4) 0.0665(3) 0.0263(11) Uani 1 1 d U . . H26A H 0.4360 1.5070 0.1021 0.032 Uiso 1 1 calc R . . H26B H 0.3744 1.4773 0.0157 0.032 Uiso 1 1 calc R . . H26C H 0.4721 1.4004 0.0562 0.032 Uiso 1 1 calc R . . C27 C 0.1212(5) 1.1982(4) 0.0933(3) 0.0234(11) Uani 1 1 d U . . H27 H 0.1593 1.1511 0.1348 0.028 Uiso 1 1 calc R . . C28 C 0.0455(5) 1.1245(5) 0.0342(4) 0.0287(12) Uani 1 1 d U . . H28A H -0.0021 1.0712 0.0640 0.034 Uiso 1 1 calc R . . H28B H 0.1000 1.0875 -0.0006 0.034 Uiso 1 1 calc R . . H28C H -0.0098 1.1678 0.0015 0.034 Uiso 1 1 calc R . . C29 C 0.0373(5) 1.2733(5) 0.1369(4) 0.0325(13) Uani 1 1 d U . . H29A H -0.0060 1.3174 0.0975 0.039 Uiso 1 1 calc R . . H29B H 0.0865 1.3202 0.1744 0.039 Uiso 1 1 calc R . . H29C H -0.0219 1.2301 0.1665 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.8230(3) 1.3577(2) 0.3265(2) 0.0835(8) Uani 1 1 d D . . Cl2 Cl 0.7179(3) 1.3673(2) 0.1591(2) 0.0960(10) Uani 1 1 d D . . C99 C 0.703(2) 1.4041(18) 0.2585(8) 0.199(9) Uiso 1 1 d D . . H99A H 0.6231 1.3746 0.2760 0.239 Uiso 1 1 calc R . . H99B H 0.7016 1.4835 0.2622 0.239 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 0.0326(2) 0.02493(17) 0.01533(15) 0.00081(12) 0.00021(14) 0.00238(15) Te2 0.01609(16) 0.01705(15) 0.02334(16) 0.00251(12) 0.00342(12) 0.00262(12) Te3 0.0299(2) 0.02294(17) 0.01718(15) 0.00111(12) 0.00008(14) -0.00150(14) I1 0.0353(2) 0.03060(19) 0.02482(18) -0.00079(14) 0.00045(15) -0.00454(16) I2 0.02530(19) 0.0440(2) 0.02164(17) 0.00440(15) 0.00457(14) 0.00370(16) I3 0.0367(2) 0.02568(19) 0.0401(2) -0.00374(16) -0.01187(18) 0.00264(16) I4 0.0273(2) 0.0402(2) 0.0358(2) -0.00007(17) 0.00557(16) 0.00517(17) I5 0.0814(4) 0.0521(3) 0.01843(18) -0.00173(18) 0.0022(2) 0.0049(3) I6 0.0473(3) 0.0339(2) 0.0350(2) 0.00788(17) 0.00163(19) -0.01422(19) I7 0.0342(2) 0.01944(16) 0.02035(15) -0.00092(12) 0.00037(14) 0.00110(14) I8 0.0324(2) 0.02326(17) 0.02237(16) -0.00027(13) -0.00455(14) -0.00234(14) Se1 0.0378(4) 0.0430(4) 0.0241(3) 0.0070(2) 0.0054(2) 0.0154(3) Se2 0.0176(3) 0.0172(3) 0.0750(5) 0.0035(3) 0.0126(3) 0.0014(2) P1 0.0306(8) 0.0390(9) 0.0230(7) 0.0110(6) 0.0008(6) 0.0007(7) P2 0.0180(6) 0.0159(6) 0.0228(6) -0.0009(5) 0.0013(5) 0.0020(5) C11 0.086(7) 0.104(7) 0.030(4) 0.007(4) -0.003(4) -0.051(6) C12 0.149(12) 0.095(8) 0.069(7) 0.029(6) -0.047(7) -0.059(8) C13 0.074(6) 0.122(9) 0.027(3) 0.005(4) -0.002(4) -0.036(6) C14 0.044(4) 0.062(5) 0.050(4) 0.030(4) 0.009(3) 0.014(4) C15 0.067(5) 0.038(4) 0.088(6) 0.008(4) 0.000(5) 0.007(4) C16 0.059(5) 0.078(6) 0.075(6) 0.040(5) 0.015(4) 0.028(5) C17 0.040(4) 0.038(3) 0.022(3) 0.002(2) 0.001(2) 0.009(3) C18 0.085(6) 0.040(4) 0.029(3) 0.000(3) 0.015(4) 0.017(4) C19 0.043(4) 0.061(5) 0.035(3) 0.017(3) 0.010(3) 0.007(4) C21 0.042(4) 0.032(3) 0.024(3) 0.003(2) -0.002(2) -0.009(3) C22 0.080(6) 0.047(4) 0.030(3) 0.002(3) 0.014(3) 0.001(4) C23 0.034(4) 0.056(4) 0.046(4) 0.018(3) -0.012(3) 0.008(3) C24 0.025(3) 0.017(2) 0.022(2) -0.0027(19) 0.003(2) -0.002(2) C25 0.036(4) 0.043(4) 0.023(3) -0.001(2) -0.002(2) -0.014(3) C26 0.026(3) 0.020(3) 0.033(3) 0.000(2) 0.004(2) -0.005(2) C27 0.017(3) 0.024(3) 0.029(3) 0.002(2) 0.002(2) -0.004(2) C28 0.018(3) 0.024(3) 0.043(3) -0.004(2) -0.005(2) -0.005(2) C29 0.020(3) 0.039(3) 0.040(3) -0.007(3) 0.009(2) 0.000(2) Cl1 0.0662(16) 0.0562(14) 0.127(2) -0.0053(14) 0.0070(16) -0.0104(12) Cl2 0.0649(17) 0.085(2) 0.140(3) -0.0024(18) 0.0029(17) 0.0205(15) _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 Se1 2.5622(7) . ? Te1 I1 2.8092(6) . ? Te1 I3 3.2045(6) . ? Te1 I8 3.3570(6) . ? Te2 Se2 2.5705(7) . ? Te2 I2 2.7593(5) . ? Te2 I8 3.3212(5) . ? Te2 I7 3.3331(5) . ? Te2 Se2 3.7381(7) 2_675 ? Te3 I4 2.8252(6) . ? Te3 I6 2.8491(6) . ? Te3 I5 2.8716(6) . ? Te3 I7 3.0370(5) . ? Te3 I8 3.0679(5) . ? Te3 I3 3.1250(6) . ? I1 I2 3.7379(6) 2_675 ? I1 I5 4.1970(6) 2_676 ? Se1 P1 2.2262(16) . ? Se2 P2 2.2226(14) . ? P1 C11 1.810(8) . ? P1 C17 1.833(7) . ? P1 C14 1.843(8) . ? P2 C24 1.834(5) . ? P2 C27 1.837(6) . ? P2 C21 1.843(6) . ? C11 C12 1.406(13) . ? C11 C13 1.557(11) . ? C14 C15 1.517(12) . ? C14 C16 1.523(11) . ? C17 C18 1.525(9) . ? C17 C19 1.544(9) . ? C21 C23 1.527(9) . ? C21 C22 1.537(10) . ? C24 C26 1.525(8) . ? C24 C25 1.534(8) . ? C27 C28 1.533(7) . ? C27 C29 1.542(8) . ? Cl1 C99 1.822(15) . ? Cl2 C99 1.736(15) . ? 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 Se1 Te1 I1 94.97(2) . . ? Se1 Te1 I3 90.49(2) . . ? I1 Te1 I3 173.921(18) . . ? Se1 Te1 I8 173.95(2) . . ? I1 Te1 I8 90.572(15) . . ? I3 Te1 I8 83.859(14) . . ? Se2 Te2 I2 94.04(2) . . ? Se2 Te2 I8 91.76(2) . . ? I2 Te2 I8 174.156(16) . . ? Se2 Te2 I7 171.58(2) . . ? I2 Te2 I7 93.759(14) . . ? I8 Te2 I7 80.414(12) . . ? Se2 Te2 Se2 100.074(18) . 2_675 ? I2 Te2 Se2 75.330(17) . 2_675 ? I8 Te2 Se2 102.893(16) . 2_675 ? I7 Te2 Se2 78.851(14) . 2_675 ? I4 Te3 I6 92.393(18) . . ? I4 Te3 I5 93.510(18) . . ? I6 Te3 I5 91.457(18) . . ? I4 Te3 I7 91.171(14) . . ? I6 Te3 I7 89.048(15) . . ? I5 Te3 I7 175.27(2) . . ? I4 Te3 I8 88.322(16) . . ? I6 Te3 I8 178.339(18) . . ? I5 Te3 I8 89.996(16) . . ? I7 Te3 I8 89.438(14) . . ? I4 Te3 I3 178.326(19) . . ? I6 Te3 I3 89.089(17) . . ? I5 Te3 I3 87.227(17) . . ? I7 Te3 I3 88.075(15) . . ? I8 Te3 I3 90.176(15) . . ? Te1 I1 I2 79.513(13) . 2_675 ? Te1 I1 I5 122.416(16) . 2_676 ? I2 I1 I5 156.555(15) 2_675 2_676 ? Te3 I3 Te1 92.286(15) . . ? Te3 I7 Te2 92.571(13) . . ? Te3 I8 Te2 92.245(12) . . ? Te3 I8 Te1 90.422(14) . . ? Te2 I8 Te1 119.711(14) . . ? P1 Se1 Te1 104.62(5) . . ? P2 Se2 Te2 106.14(4) . . ? C11 P1 C17 117.4(5) . . ? C11 P1 C14 108.3(5) . . ? C17 P1 C14 106.4(3) . . ? C11 P1 Se1 105.5(3) . . ? C17 P1 Se1 113.52(19) . . ? C14 P1 Se1 104.8(3) . . ? C24 P2 C27 109.2(2) . . ? C24 P2 C21 111.6(3) . . ? C27 P2 C21 108.8(3) . . ? C24 P2 Se2 104.15(18) . . ? C27 P2 Se2 112.20(18) . . ? C21 P2 Se2 110.8(2) . . ? C12 C11 C13 112.9(9) . . ? C12 C11 P1 119.1(8) . . ? C13 C11 P1 112.2(6) . . ? C15 C14 C16 109.8(8) . . ? C15 C14 P1 111.5(5) . . ? C16 C14 P1 111.4(6) . . ? C18 C17 C19 111.5(5) . . ? C18 C17 P1 112.1(5) . . ? C19 C17 P1 112.5(4) . . ? C23 C21 C22 112.9(6) . . ? C23 C21 P2 110.6(4) . . ? C22 C21 P2 113.7(5) . . ? C26 C24 C25 111.1(5) . . ? C26 C24 P2 111.5(4) . . ? C25 C24 P2 109.7(4) . . ? C28 C27 C29 110.1(5) . . ? C28 C27 P2 111.0(4) . . ? C29 C27 P2 113.7(4) . . ? Cl2 C99 Cl1 113.9(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se1 Te1 I1 I2 116.281(18) . . . 2_675 ? I3 Te1 I1 I2 -89.73(16) . . . 2_675 ? I8 Te1 I1 I2 -66.132(12) . . . 2_675 ? Se1 Te1 I1 I5 -72.71(2) . . . 2_676 ? I3 Te1 I1 I5 81.28(16) . . . 2_676 ? I8 Te1 I1 I5 104.875(18) . . . 2_676 ? I4 Te3 I3 Te1 40.5(6) . . . . ? I6 Te3 I3 Te1 -167.186(15) . . . . ? I5 Te3 I3 Te1 -75.683(17) . . . . ? I7 Te3 I3 Te1 103.736(14) . . . . ? I8 Te3 I3 Te1 14.304(14) . . . . ? Se1 Te1 I3 Te3 164.708(19) . . . . ? I1 Te1 I3 Te3 10.61(16) . . . . ? I8 Te1 I3 Te3 -13.126(13) . . . . ? I4 Te3 I7 Te2 70.319(15) . . . . ? I6 Te3 I7 Te2 162.693(15) . . . . ? I5 Te3 I7 Te2 -101.1(2) . . . . ? I8 Te3 I7 Te2 -17.991(13) . . . . ? I3 Te3 I7 Te2 -108.186(14) . . . . ? Se2 Te2 I7 Te3 38.65(14) . . . . ? I2 Te2 I7 Te3 -163.639(15) . . . . ? I8 Te2 I7 Te3 16.818(13) . . . . ? Se2 Te2 I7 Te3 122.122(17) 2_675 . . . ? I4 Te3 I8 Te2 -73.136(14) . . . . ? I6 Te3 I8 Te2 42.4(6) . . . . ? I5 Te3 I8 Te2 -166.647(16) . . . . ? I7 Te3 I8 Te2 18.053(13) . . . . ? I3 Te3 I8 Te2 106.125(14) . . . . ? I4 Te3 I8 Te1 167.108(14) . . . . ? I6 Te3 I8 Te1 -77.4(6) . . . . ? I5 Te3 I8 Te1 73.596(16) . . . . ? I7 Te3 I8 Te1 -101.704(14) . . . . ? I3 Te3 I8 Te1 -13.631(13) . . . . ? Se2 Te2 I8 Te3 166.486(18) . . . . ? I2 Te2 I8 Te3 -21.13(16) . . . . ? I7 Te2 I8 Te3 -16.640(13) . . . . ? Se2 Te2 I8 Te3 -92.763(16) 2_675 . . . ? Se2 Te2 I8 Te1 -101.75(2) . . . . ? I2 Te2 I8 Te1 70.64(16) . . . . ? I7 Te2 I8 Te1 75.129(17) . . . . ? Se2 Te2 I8 Te1 -1.00(2) 2_675 . . . ? Se1 Te1 I8 Te3 -7.66(19) . . . . ? I1 Te1 I8 Te3 -164.192(14) . . . . ? I3 Te1 I8 Te3 13.364(13) . . . . ? Se1 Te1 I8 Te2 -100.49(19) . . . . ? I1 Te1 I8 Te2 102.982(17) . . . . ? I3 Te1 I8 Te2 -79.462(17) . . . . ? I1 Te1 Se1 P1 91.85(5) . . . . ? I3 Te1 Se1 P1 -85.49(5) . . . . ? I8 Te1 Se1 P1 -64.6(2) . . . . ? I2 Te2 Se2 P2 90.25(5) . . . . ? I8 Te2 Se2 P2 -90.53(5) . . . . ? I7 Te2 Se2 P2 -112.05(14) . . . . ? Se2 Te2 Se2 P2 166.05(5) 2_675 . . . ? Te1 Se1 P1 C11 -118.2(4) . . . . ? Te1 Se1 P1 C17 11.8(2) . . . . ? Te1 Se1 P1 C14 127.5(3) . . . . ? Te2 Se2 P2 C24 140.43(18) . . . . ? Te2 Se2 P2 C27 22.40(19) . . . . ? Te2 Se2 P2 C21 -99.4(2) . . . . ? C17 P1 C11 C12 -74.1(11) . . . . ? C14 P1 C11 C12 165.4(10) . . . . ? Se1 P1 C11 C12 53.6(11) . . . . ? C17 P1 C11 C13 61.0(10) . . . . ? C14 P1 C11 C13 -59.6(10) . . . . ? Se1 P1 C11 C13 -171.4(8) . . . . ? C11 P1 C14 C15 -174.9(6) . . . . ? C17 P1 C14 C15 58.0(7) . . . . ? Se1 P1 C14 C15 -62.6(6) . . . . ? C11 P1 C14 C16 -51.8(7) . . . . ? C17 P1 C14 C16 -178.9(6) . . . . ? Se1 P1 C14 C16 60.5(6) . . . . ? C11 P1 C17 C18 44.8(6) . . . . ? C14 P1 C17 C18 166.3(5) . . . . ? Se1 P1 C17 C18 -79.0(4) . . . . ? C11 P1 C17 C19 -81.9(6) . . . . ? C14 P1 C17 C19 39.6(6) . . . . ? Se1 P1 C17 C19 154.4(4) . . . . ? C24 P2 C21 C23 -42.8(6) . . . . ? C27 P2 C21 C23 77.8(5) . . . . ? Se2 P2 C21 C23 -158.3(4) . . . . ? C24 P2 C21 C22 85.4(5) . . . . ? C27 P2 C21 C22 -154.0(5) . . . . ? Se2 P2 C21 C22 -30.2(5) . . . . ? C27 P2 C24 C26 -178.9(4) . . . . ? C21 P2 C24 C26 -58.5(5) . . . . ? Se2 P2 C24 C26 61.1(4) . . . . ? C27 P2 C24 C25 57.5(5) . . . . ? C21 P2 C24 C25 177.9(4) . . . . ? Se2 P2 C24 C25 -62.5(4) . . . . ? C24 P2 C27 C28 163.0(4) . . . . ? C21 P2 C27 C28 41.0(5) . . . . ? Se2 P2 C27 C28 -82.0(4) . . . . ? C24 P2 C27 C29 38.2(5) . . . . ? C21 P2 C27 C29 -83.8(5) . . . . ? Se2 P2 C27 C29 153.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.225 _refine_diff_density_min -2.254 _refine_diff_density_rms 0.239 # Attachment '6.cif.CIF' data_freya _database_code_depnum_ccdc_archive 'CCDC 644168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 I6 Te3' _chemical_formula_weight 1606.80 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.8246(15) _cell_length_b 14.8246(15) _cell_length_c 16.8024(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3197.9(5) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11.5 _exptl_crystal_description needle _exptl_crystal_colour 'black-green metallic' _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 6.407 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details XEMP _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'SIEMENS P4' _diffrn_measurement_method Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 147 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9563 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1638 _reflns_number_gt 1402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SIEMENS XSCANS' _computing_cell_refinement 'SIEMENS XSCANS' _computing_data_reduction 'SIEMENS XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS XP' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0142P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1638 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0361 _refine_ls_wR_factor_gt 0.0351 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _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 0.0000 0.0000 0.284671(17) 0.02069(7) Uani 1 3 d S . . Te2 Te 0.0000 0.0000 0.0000 0.01859(9) Uani 1 6 d S . . I I 0.092939(15) 0.186759(14) -0.101827(10) 0.02977(6) Uani 1 1 d . . . C1 C 0.0329(2) -0.1039(2) 0.34756(16) 0.0238(6) Uani 1 1 d . . . C2 C -0.0219(2) -0.2077(2) 0.32510(17) 0.0315(6) Uani 1 1 d . . . H2 H -0.0729 -0.2302 0.2842 0.038 Uiso 1 1 calc R . . C3 C -0.0010(3) -0.2783(2) 0.36340(19) 0.0393(8) Uani 1 1 d . . . H3 H -0.0381 -0.3497 0.3488 0.047 Uiso 1 1 calc R . . C4 C 0.0731(3) -0.2452(3) 0.42242(19) 0.0398(8) Uani 1 1 d . . . H4 H 0.0863 -0.2941 0.4488 0.048 Uiso 1 1 calc R . . C5 C 0.1284(2) -0.1413(3) 0.44359(18) 0.0377(7) Uani 1 1 d . . . H5 H 0.1806 -0.1188 0.4835 0.045 Uiso 1 1 calc R . . C6 C 0.1079(2) -0.0694(2) 0.40657(16) 0.0322(7) Uani 1 1 d . . . H6 H 0.1447 0.0020 0.4216 0.039 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 0.02036(10) 0.02036(10) 0.02136(14) 0.000 0.000 0.01018(5) Te2 0.01993(13) 0.01993(13) 0.01590(18) 0.000 0.000 0.00996(6) I 0.03813(11) 0.02306(10) 0.02370(10) 0.00337(7) 0.00548(7) 0.01197(8) C1 0.0243(14) 0.0268(14) 0.0249(13) 0.0029(10) 0.0009(11) 0.0162(12) C2 0.0363(17) 0.0277(15) 0.0292(14) -0.0026(12) -0.0057(12) 0.0150(13) C3 0.053(2) 0.0265(16) 0.0418(18) 0.0032(13) -0.0006(15) 0.0220(15) C4 0.054(2) 0.0432(19) 0.0370(17) 0.0098(14) 0.0058(15) 0.0353(18) C5 0.0392(18) 0.051(2) 0.0304(16) 0.0011(14) -0.0059(13) 0.0286(16) C6 0.0370(17) 0.0331(16) 0.0293(15) -0.0049(12) -0.0047(12) 0.0195(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 2.116(3) 2 ? Te1 C1 2.116(3) 3 ? Te1 C1 2.116(3) . ? Te1 I 3.8971(4) 10 ? Te1 I 3.8971(4) 12 ? Te1 I 3.8971(4) 11 ? Te2 I 2.9456(3) 2 ? Te2 I 2.9456(3) 11 ? Te2 I 2.9456(3) 3 ? Te2 I 2.9456(3) 10 ? Te2 I 2.9456(3) 12 ? Te2 I 2.9456(3) . ? C1 C6 1.383(4) . ? C1 C2 1.386(4) . ? C2 C3 1.389(4) . ? C3 C4 1.376(5) . ? C4 C5 1.382(5) . ? C5 C6 1.393(4) . ? 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 C1 97.24(10) 2 3 ? C1 Te1 C1 97.24(10) 2 . ? C1 Te1 C1 97.24(10) 3 . ? C1 Te1 I 154.66(7) 2 10 ? C1 Te1 I 105.80(7) 3 10 ? C1 Te1 I 90.27(7) . 10 ? C1 Te1 I 105.80(7) 2 12 ? C1 Te1 I 90.27(7) 3 12 ? C1 Te1 I 154.66(7) . 12 ? I Te1 I 64.393(8) 10 12 ? C1 Te1 I 90.27(7) 2 11 ? C1 Te1 I 154.66(7) 3 11 ? C1 Te1 I 105.80(7) . 11 ? I Te1 I 64.393(8) 10 11 ? I Te1 I 64.393(8) 12 11 ? I Te2 I 180.000(10) 2 11 ? I Te2 I 89.651(7) 2 3 ? I Te2 I 90.349(7) 11 3 ? I Te2 I 90.349(7) 2 10 ? I Te2 I 89.651(7) 11 10 ? I Te2 I 90.349(7) 3 10 ? I Te2 I 90.349(7) 2 12 ? I Te2 I 89.651(7) 11 12 ? I Te2 I 180.000(8) 3 12 ? I Te2 I 89.651(7) 10 12 ? I Te2 I 89.651(7) 2 . ? I Te2 I 90.349(7) 11 . ? I Te2 I 89.651(7) 3 . ? I Te2 I 180.000(10) 10 . ? I Te2 I 90.349(7) 12 . ? C6 C1 C2 121.5(3) . . ? C6 C1 Te1 121.6(2) . . ? C2 C1 Te1 116.9(2) . . ? C1 C2 C3 118.8(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 120.4(3) . . ? C4 C5 C6 120.2(3) . . ? C1 C6 C5 118.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.467 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.099