# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _audit_creation_method 'manual editing of .cif file' _journal_coden_Cambridge 182 _publ_contact_author_name 'James A. Ibers' _publ_contact_author_address ; Department of Chemistry Northwestern University 2145 Sheridan Rd. Evanston, IL 60208-3113, USA ; _publ_contact_author_email ibers@chem.northwestern.edu _publ_contact_author_fax '+1 847 491 2976' _publ_contact_author_phone '+1 847 491 5449' _publ_contact_letter ; Please consider this CIF submission as supplemetary information, ; _publ_requested_coeditor_name 'Ian Rothwell' _publ_requested_journal 'Chemical Communications' _publ_requested_category communication _publ_section_title ; [TeSe3]2 and [TeSe2]2 as synthons ; loop_ _publ_author_name _publ_author_address 'Dibrov, Sergey M.' ; Department of Chemistry Northwestern University 2145 Sheridan Rd. Evanston, IL 60208-3113, USA ; 'Ibers, James A.' ; Department of Chemistry Northwestern University 2145 Sheridan Rd. Evanston, IL 60208-3113, USA ; data_au2te4 _database_code_CSD 212389 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Au2 P2 Te4' _chemical_formula_weight 1583.07 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 10.4984(11) _cell_length_b 10.5260(11) _cell_length_c 11.1529(11) _cell_angle_alpha 81.459(2) _cell_angle_beta 77.221(2) _cell_angle_gamma 72.994(2) _cell_volume 1144.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 9.001 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13840 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.75 _reflns_number_total 5450 _reflns_number_gt 4245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.2178P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5450 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Au1 Au 0.026384(18) 0.455207(16) 0.378390(13) 0.04032(7) Uani 1 1 d . . . Te2 Te 0.27743(3) 0.44580(3) 0.35641(3) 0.04788(9) Uani 1 1 d . . . Te1 Te -0.22488(3) 0.46437(3) 0.41006(3) 0.04550(9) Uani 1 1 d . . . P1 P 0.22694(10) -0.04003(10) 0.15877(9) 0.0296(2) Uani 1 1 d . . . C1 C 0.0691(4) -0.0433(4) 0.2604(3) 0.0313(8) Uani 1 1 d . . . C7 C 0.3547(4) -0.0729(4) 0.2503(3) 0.0330(8) Uani 1 1 d . . . C13 C 0.2117(4) 0.1175(4) 0.0698(3) 0.0329(8) Uani 1 1 d . . . C18 C 0.1929(4) 0.2333(4) 0.1262(4) 0.0366(9) Uani 1 1 d . . . H18 H 0.1932 0.2281 0.2101 0.044 Uiso 1 1 calc R . . C2 C -0.0164(4) 0.0727(4) 0.3089(4) 0.0395(9) Uani 1 1 d . . . H2 H 0.0030 0.1541 0.2817 0.047 Uiso 1 1 calc R . . C20 C 0.1766(5) -0.1940(4) 0.0036(4) 0.0435(10) Uani 1 1 d . . . H20 H 0.0856 -0.1493 0.0269 0.052 Uiso 1 1 calc R . . C24 C 0.4083(4) -0.2374(4) 0.0214(4) 0.0407(10) Uani 1 1 d . . . H24 H 0.4737 -0.2224 0.0577 0.049 Uiso 1 1 calc R . . C19 C 0.2730(4) -0.1678(4) 0.0562(3) 0.0328(8) Uani 1 1 d . . . C6 C 0.0387(4) -0.1652(4) 0.3028(4) 0.0380(9) Uani 1 1 d . . . H6 H 0.0946 -0.2437 0.2711 0.046 Uiso 1 1 calc R . . C5 C -0.0746(4) -0.1671(4) 0.3916(4) 0.0405(10) Uani 1 1 d . . . H5 H -0.0949 -0.2479 0.4203 0.049 Uiso 1 1 calc R . . C14 C 0.2140(4) 0.1266(4) -0.0565(4) 0.0397(10) Uani 1 1 d . . . H14 H 0.2276 0.0499 -0.0950 0.048 Uiso 1 1 calc R . . C12 C 0.3698(4) -0.1875(4) 0.3314(4) 0.0400(10) Uani 1 1 d . . . H12 H 0.3140 -0.2430 0.3362 0.048 Uiso 1 1 calc R . . C4 C -0.1586(4) -0.0519(4) 0.4389(4) 0.0409(10) Uani 1 1 d . . . H4 H -0.2348 -0.0553 0.4991 0.049 Uiso 1 1 calc R . . C15 C 0.1959(5) 0.2498(5) -0.1252(4) 0.0481(11) Uani 1 1 d . . . H15 H 0.1984 0.2555 -0.2097 0.058 Uiso 1 1 calc R . . C3 C -0.1310(4) 0.0671(5) 0.3982(4) 0.0467(11) Uani 1 1 d . . . H3 H -0.1887 0.1450 0.4300 0.056 Uiso 1 1 calc R . . C8 C 0.4376(4) 0.0101(4) 0.2442(4) 0.0413(10) Uani 1 1 d . . . H8 H 0.4289 0.0869 0.1898 0.050 Uiso 1 1 calc R . . C11 C 0.4663(4) -0.2199(5) 0.4046(4) 0.0439(10) Uani 1 1 d . . . H11 H 0.4767 -0.2978 0.4576 0.053 Uiso 1 1 calc R . . C17 C 0.1737(5) 0.3557(4) 0.0571(4) 0.0421(10) Uani 1 1 d . . . H17 H 0.1604 0.4328 0.0949 0.051 Uiso 1 1 calc R . . C21 C 0.2139(5) -0.2857(5) -0.0830(5) 0.0536(12) Uani 1 1 d . . . H21 H 0.1484 -0.3031 -0.1173 0.064 Uiso 1 1 calc R . . C16 C 0.1744(5) 0.3637(4) -0.0677(4) 0.0467(11) Uani 1 1 d . . . H16 H 0.1603 0.4464 -0.1133 0.056 Uiso 1 1 calc R . . C9 C 0.5334(5) -0.0221(5) 0.3194(4) 0.0494(12) Uani 1 1 d . . . H9 H 0.5886 0.0336 0.3163 0.059 Uiso 1 1 calc R . . C10 C 0.5470(4) -0.1370(5) 0.3992(4) 0.0474(11) Uani 1 1 d . . . H10 H 0.6113 -0.1581 0.4496 0.057 Uiso 1 1 calc R . . C23 C 0.4469(5) -0.3277(5) -0.0653(4) 0.0509(12) Uani 1 1 d . . . H23 H 0.5378 -0.3726 -0.0886 0.061 Uiso 1 1 calc R . . C22 C 0.3488(6) -0.3514(5) -0.1182(4) 0.0559(13) Uani 1 1 d . . . H22 H 0.3744 -0.4120 -0.1776 0.067 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 Au1 0.05562(12) 0.03444(10) 0.02730(9) -0.00787(6) -0.00244(7) -0.00808(8) Te2 0.05326(19) 0.04866(19) 0.03648(16) -0.01108(13) 0.00201(13) -0.00989(15) Te1 0.0572(2) 0.04269(18) 0.03737(16) -0.00741(13) -0.00978(14) -0.01205(15) P1 0.0323(5) 0.0278(5) 0.0286(5) -0.0037(4) -0.0040(4) -0.0087(4) C1 0.032(2) 0.032(2) 0.0293(19) -0.0016(16) -0.0050(16) -0.0095(17) C7 0.034(2) 0.036(2) 0.0297(19) -0.0091(16) -0.0010(16) -0.0112(17) C13 0.037(2) 0.031(2) 0.0286(19) -0.0035(16) -0.0015(16) -0.0094(17) C18 0.045(2) 0.036(2) 0.030(2) -0.0047(17) -0.0035(17) -0.0146(19) C2 0.039(2) 0.030(2) 0.046(2) -0.0029(18) -0.0011(19) -0.0104(18) C20 0.041(2) 0.040(3) 0.051(3) -0.010(2) -0.014(2) -0.007(2) C24 0.039(2) 0.040(2) 0.043(2) -0.0095(19) -0.0018(19) -0.0119(19) C19 0.038(2) 0.028(2) 0.0308(19) -0.0043(16) -0.0030(16) -0.0086(17) C6 0.039(2) 0.028(2) 0.045(2) -0.0006(17) -0.0073(19) -0.0084(18) C5 0.043(2) 0.038(2) 0.044(2) 0.0050(19) -0.0104(19) -0.019(2) C14 0.053(3) 0.035(2) 0.030(2) -0.0047(17) -0.0059(18) -0.011(2) C12 0.038(2) 0.042(2) 0.043(2) 0.0008(19) -0.0130(19) -0.0139(19) C4 0.035(2) 0.050(3) 0.039(2) -0.005(2) -0.0014(18) -0.018(2) C15 0.064(3) 0.046(3) 0.032(2) -0.0041(19) -0.007(2) -0.013(2) C3 0.040(2) 0.044(3) 0.050(3) -0.011(2) 0.002(2) -0.007(2) C8 0.041(2) 0.047(3) 0.037(2) -0.0020(19) -0.0049(19) -0.017(2) C11 0.039(2) 0.042(3) 0.045(2) 0.004(2) -0.011(2) -0.005(2) C17 0.057(3) 0.034(2) 0.035(2) -0.0075(18) 0.000(2) -0.016(2) C21 0.063(3) 0.049(3) 0.061(3) -0.019(2) -0.021(3) -0.020(3) C16 0.067(3) 0.034(2) 0.035(2) 0.0057(18) -0.009(2) -0.015(2) C9 0.041(3) 0.060(3) 0.054(3) -0.004(2) -0.010(2) -0.025(2) C10 0.036(2) 0.060(3) 0.046(3) -0.002(2) -0.012(2) -0.011(2) C23 0.048(3) 0.048(3) 0.054(3) -0.022(2) 0.000(2) -0.008(2) C22 0.080(4) 0.047(3) 0.044(3) -0.019(2) -0.008(2) -0.016(3) _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 Au1 Te1 2.5576(5) . ? Au1 Te2 2.5660(5) . ? Au1 Au1 2.8886(4) 2_566 ? Te2 Te1 2.7880(5) 2_566 ? Te1 Te2 2.7880(5) 2_566 ? P1 C19 1.784(4) . ? P1 C13 1.785(4) . ? P1 C7 1.787(4) . ? P1 C1 1.795(4) . ? C1 C2 1.389(5) . ? C1 C6 1.401(5) . ? C7 C12 1.387(6) . ? C7 C8 1.388(5) . ? C13 C14 1.393(5) . ? C13 C18 1.397(5) . ? C18 C17 1.385(6) . ? C2 C3 1.392(6) . ? C20 C21 1.381(6) . ? C20 C19 1.385(6) . ? C24 C23 1.370(6) . ? C24 C19 1.392(6) . ? C6 C5 1.373(6) . ? C5 C4 1.374(6) . ? C14 C15 1.389(6) . ? C12 C11 1.375(6) . ? C4 C3 1.358(6) . ? C15 C16 1.381(6) . ? C8 C9 1.386(6) . ? C11 C10 1.371(6) . ? C17 C16 1.381(6) . ? C21 C22 1.378(7) . ? C9 C10 1.381(7) . ? C23 C22 1.390(7) . ? 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 Te1 Au1 Te2 177.609(10) . . ? Te1 Au1 Au1 88.219(10) . 2_566 ? Te2 Au1 Au1 89.524(10) . 2_566 ? Au1 Te2 Te1 90.274(11) . 2_566 ? Au1 Te1 Te2 91.973(12) . 2_566 ? C19 P1 C13 108.75(18) . . ? C19 P1 C7 108.39(19) . . ? C13 P1 C7 111.40(19) . . ? C19 P1 C1 109.78(18) . . ? C13 P1 C1 110.28(18) . . ? C7 P1 C1 108.20(18) . . ? C2 C1 C6 119.3(4) . . ? C2 C1 P1 120.2(3) . . ? C6 C1 P1 120.1(3) . . ? C12 C7 C8 119.3(4) . . ? C12 C7 P1 117.3(3) . . ? C8 C7 P1 123.3(3) . . ? C14 C13 C18 119.3(4) . . ? C14 C13 P1 120.0(3) . . ? C18 C13 P1 120.7(3) . . ? C17 C18 C13 120.0(4) . . ? C1 C2 C3 120.0(4) . . ? C21 C20 C19 120.8(4) . . ? C23 C24 C19 121.2(4) . . ? C20 C19 C24 118.6(4) . . ? C20 C19 P1 120.9(3) . . ? C24 C19 P1 120.4(3) . . ? C5 C6 C1 119.2(4) . . ? C6 C5 C4 121.1(4) . . ? C15 C14 C13 120.3(4) . . ? C11 C12 C7 120.8(4) . . ? C3 C4 C5 120.4(4) . . ? C16 C15 C14 119.8(4) . . ? C4 C3 C2 120.0(4) . . ? C9 C8 C7 119.6(4) . . ? C10 C11 C12 119.6(4) . . ? C16 C17 C18 120.2(4) . . ? C22 C21 C20 119.6(4) . . ? C17 C16 C15 120.5(4) . . ? C10 C9 C8 120.1(4) . . ? C11 C10 C9 120.5(4) . . ? C24 C23 C22 119.3(4) . . ? C21 C22 C23 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.144 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.110 data_Au2(TeSe2)2 _database_code_CSD 212390 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Au2 P2 Se4 Te2' _chemical_formula_weight 1643.71 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 9.8089(5) _cell_length_b 13.6406(7) _cell_length_c 17.5009(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.7510(10) _cell_angle_gamma 90.00 _cell_volume 2320.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 10.788 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19346 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0168 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3331 _reflns_number_gt 3137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+12.9493P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3331 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Au1 Au 0.83057(3) 0.05884(2) 0.947625(15) 0.03162(13) Uani 1 1 d . . . Te1 Te 1.09762(5) -0.03038(4) 0.83817(3) 0.03756(16) Uani 1 1 d . . . Se2 Se 0.93933(8) 0.11185(5) 0.83940(4) 0.03519(19) Uani 1 1 d . . . Se1 Se 0.71736(8) -0.00004(6) 1.05209(5) 0.0391(2) Uani 1 1 d . . . P1 P 1.28624(16) -0.09130(11) 0.60183(9) 0.0181(3) Uani 1 1 d . . . C2 C 1.4380(7) -0.0600(4) 0.7423(4) 0.0254(15) Uani 1 1 d . . . H2 H 1.3546 -0.0345 0.7561 0.030 Uiso 1 1 calc R . . C14 C 1.0992(7) 0.0561(5) 0.6276(4) 0.0235(14) Uani 1 1 d . . . H14 H 1.0441 0.0058 0.6453 0.028 Uiso 1 1 calc R . . C7 C 1.1642(6) -0.1753(4) 0.6327(3) 0.0201(13) Uani 1 1 d . . . C19 C 1.3145(6) -0.1314(5) 0.5077(3) 0.0211(13) Uani 1 1 d . . . C20 C 1.2945(7) -0.0724(5) 0.4415(4) 0.0230(14) Uani 1 1 d . . . H20 H 1.2670 -0.0060 0.4450 0.028 Uiso 1 1 calc R . . C9 C 0.9457(7) -0.2568(5) 0.6060(4) 0.0285(15) Uani 1 1 d . . . H9 H 0.8595 -0.2650 0.5747 0.034 Uiso 1 1 calc R . . C18 C 1.3038(6) 0.1070(5) 0.5752(3) 0.0214(13) Uani 1 1 d . . . H18 H 1.3890 0.0913 0.5580 0.026 Uiso 1 1 calc R . . C13 C 1.2222(6) 0.0330(4) 0.5996(3) 0.0196(13) Uani 1 1 d . . . C8 C 1.0389(7) -0.1878(5) 0.5861(4) 0.0271(14) Uani 1 1 d . . . H8 H 1.0172 -0.1493 0.5409 0.033 Uiso 1 1 calc R . . C1 C 1.4434(6) -0.0949(4) 0.6674(3) 0.0197(13) Uani 1 1 d . . . C3 C 1.5564(7) -0.0631(5) 0.7963(4) 0.0289(16) Uani 1 1 d . . . H3 H 1.5531 -0.0414 0.8476 0.035 Uiso 1 1 calc R . . C10 C 0.9781(7) -0.3131(5) 0.6708(4) 0.0277(15) Uani 1 1 d . . . H10 H 0.9142 -0.3604 0.6840 0.033 Uiso 1 1 calc R . . C17 C 1.2607(7) 0.2035(5) 0.5760(4) 0.0249(14) Uani 1 1 d . . . H17 H 1.3153 0.2539 0.5582 0.030 Uiso 1 1 calc R . . C12 C 1.1967(7) -0.2337(5) 0.6978(4) 0.0251(14) Uani 1 1 d . . . H12 H 1.2832 -0.2268 0.7290 0.030 Uiso 1 1 calc R . . C6 C 1.5650(7) -0.1317(5) 0.6474(4) 0.0255(14) Uani 1 1 d . . . H6 H 1.5680 -0.1566 0.5970 0.031 Uiso 1 1 calc R . . C21 C 1.3145(7) -0.1109(5) 0.3719(4) 0.0286(15) Uani 1 1 d . . . H21 H 1.2994 -0.0712 0.3269 0.034 Uiso 1 1 calc R . . C15 C 1.0590(7) 0.1530(5) 0.6292(4) 0.0270(15) Uani 1 1 d . . . H15 H 0.9762 0.1696 0.6488 0.032 Uiso 1 1 calc R . . C4 C 1.6786(7) -0.0978(5) 0.7753(4) 0.0320(16) Uani 1 1 d . . . H4 H 1.7597 -0.0980 0.8117 0.038 Uiso 1 1 calc R . . C5 C 1.6830(7) -0.1322(5) 0.7013(4) 0.0323(16) Uani 1 1 d . . . H5 H 1.7670 -0.1563 0.6872 0.039 Uiso 1 1 calc R . . C16 C 1.1384(7) 0.2265(5) 0.6025(4) 0.0294(15) Uani 1 1 d . . . H16 H 1.1085 0.2928 0.6025 0.035 Uiso 1 1 calc R . . C22 C 1.3567(7) -0.2071(5) 0.3660(4) 0.0304(16) Uani 1 1 d . . . H22 H 1.3720 -0.2327 0.3174 0.036 Uiso 1 1 calc R . . C11 C 1.1023(7) -0.3019(5) 0.7168(4) 0.0302(15) Uani 1 1 d . . . H11 H 1.1233 -0.3410 0.7618 0.036 Uiso 1 1 calc R . . C24 C 1.3546(7) -0.2299(5) 0.5015(4) 0.0279(15) Uani 1 1 d . . . H24 H 1.3664 -0.2709 0.5457 0.033 Uiso 1 1 calc R . . C23 C 1.3767(7) -0.2664(5) 0.4312(4) 0.0310(15) Uani 1 1 d . . . H23 H 1.4057 -0.3324 0.4270 0.037 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 Au1 0.03190(19) 0.02892(19) 0.03258(19) -0.00590(11) -0.00091(13) 0.00675(11) Te1 0.0459(3) 0.0327(3) 0.0363(3) -0.0021(2) 0.0137(2) -0.0007(2) Se2 0.0426(4) 0.0286(4) 0.0317(4) 0.0005(3) -0.0045(3) 0.0002(3) Se1 0.0338(4) 0.0380(4) 0.0465(5) -0.0023(3) 0.0098(3) 0.0062(3) P1 0.0183(8) 0.0178(8) 0.0178(8) 0.0002(6) 0.0008(6) -0.0020(6) C2 0.026(4) 0.024(3) 0.026(4) -0.002(3) 0.002(3) -0.001(3) C14 0.021(3) 0.032(4) 0.017(3) 0.001(3) -0.001(3) -0.001(3) C7 0.023(3) 0.017(3) 0.020(3) 0.001(2) 0.004(3) -0.002(2) C19 0.023(3) 0.022(3) 0.018(3) 0.000(3) 0.002(3) -0.002(3) C20 0.022(3) 0.025(3) 0.022(3) -0.003(3) -0.001(3) -0.006(3) C9 0.019(3) 0.034(4) 0.031(4) 0.002(3) -0.003(3) -0.006(3) C18 0.020(3) 0.024(3) 0.019(3) -0.001(3) -0.001(3) 0.002(3) C13 0.024(3) 0.019(3) 0.014(3) -0.001(2) -0.003(2) 0.000(3) C8 0.025(3) 0.027(4) 0.026(3) 0.007(3) -0.005(3) -0.003(3) C1 0.021(3) 0.014(3) 0.022(3) 0.002(2) -0.003(3) -0.003(3) C3 0.036(4) 0.023(3) 0.025(4) 0.001(3) -0.006(3) -0.004(3) C10 0.034(4) 0.019(3) 0.031(4) -0.002(3) 0.011(3) -0.008(3) C17 0.027(4) 0.024(3) 0.022(3) 0.000(3) -0.003(3) -0.004(3) C12 0.024(3) 0.026(3) 0.023(3) 0.001(3) -0.005(3) -0.003(3) C6 0.027(4) 0.019(3) 0.030(3) -0.001(3) 0.003(3) -0.003(3) C21 0.029(4) 0.034(4) 0.023(3) 0.001(3) 0.002(3) -0.014(3) C15 0.022(3) 0.031(4) 0.028(4) -0.005(3) 0.002(3) 0.006(3) C4 0.030(4) 0.019(3) 0.040(4) 0.006(3) -0.016(3) -0.003(3) C5 0.022(3) 0.023(4) 0.052(5) 0.001(3) 0.004(3) 0.005(3) C16 0.033(4) 0.023(3) 0.030(4) -0.005(3) -0.007(3) 0.005(3) C22 0.035(4) 0.029(4) 0.028(4) -0.010(3) 0.010(3) -0.015(3) C11 0.034(4) 0.032(4) 0.023(3) 0.007(3) -0.002(3) -0.007(3) C24 0.036(4) 0.019(3) 0.028(3) 0.001(3) 0.001(3) -0.002(3) C23 0.037(4) 0.024(4) 0.032(4) -0.005(3) 0.007(3) -0.002(3) _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 Au1 Se1 2.4017(8) . ? Au1 Se2 2.4069(8) . ? Te1 Se2 2.4868(9) . ? Te1 Se1 2.4929(10) 3_757 ? Se1 Te1 2.4929(10) 3_757 ? P1 C19 1.792(6) . ? P1 C7 1.792(6) . ? P1 C1 1.794(6) . ? P1 C13 1.806(6) . ? C2 C3 1.396(10) . ? C2 C1 1.403(9) . ? C14 C15 1.382(9) . ? C14 C13 1.399(9) . ? C7 C8 1.391(9) . ? C7 C12 1.391(9) . ? C19 C20 1.403(9) . ? C19 C24 1.409(9) . ? C20 C21 1.365(9) . ? C9 C10 1.370(10) . ? C9 C8 1.388(9) . ? C18 C17 1.383(9) . ? C18 C13 1.391(9) . ? C1 C6 1.381(9) . ? C3 C4 1.384(11) . ? C10 C11 1.376(10) . ? C17 C16 1.380(10) . ? C12 C11 1.384(9) . ? C6 C5 1.391(10) . ? C21 C22 1.384(10) . ? C15 C16 1.389(10) . ? C4 C5 1.384(10) . ? C22 C23 1.390(10) . ? C24 C23 1.371(10) . ? 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 Au1 Se2 177.41(3) . . ? Se2 Te1 Se1 104.71(3) . 3_757 ? Au1 Se2 Te1 96.66(3) . . ? Au1 Se1 Te1 99.64(3) . 3_757 ? C19 P1 C7 106.0(3) . . ? C19 P1 C1 110.7(3) . . ? C7 P1 C1 109.9(3) . . ? C19 P1 C13 111.3(3) . . ? C7 P1 C13 111.2(3) . . ? C1 P1 C13 107.8(3) . . ? C3 C2 C1 119.3(6) . . ? C15 C14 C13 119.0(6) . . ? C8 C7 C12 119.8(6) . . ? C8 C7 P1 118.3(5) . . ? C12 C7 P1 121.6(5) . . ? C20 C19 C24 119.5(6) . . ? C20 C19 P1 124.3(5) . . ? C24 C19 P1 116.2(5) . . ? C21 C20 C19 119.8(6) . . ? C10 C9 C8 120.0(6) . . ? C17 C18 C13 119.9(6) . . ? C18 C13 C14 120.2(6) . . ? C18 C13 P1 118.4(5) . . ? C14 C13 P1 121.2(5) . . ? C9 C8 C7 119.7(6) . . ? C6 C1 C2 120.2(6) . . ? C6 C1 P1 123.0(5) . . ? C2 C1 P1 116.8(5) . . ? C4 C3 C2 120.1(7) . . ? C9 C10 C11 120.7(6) . . ? C16 C17 C18 120.1(6) . . ? C11 C12 C7 119.6(6) . . ? C1 C6 C5 119.9(6) . . ? C20 C21 C22 120.7(6) . . ? C14 C15 C16 120.6(6) . . ? C3 C4 C5 120.2(6) . . ? C4 C5 C6 120.3(6) . . ? C17 C16 C15 120.1(6) . . ? C21 C22 C23 120.1(6) . . ? C10 C11 C12 120.1(6) . . ? C23 C24 C19 119.7(6) . . ? C24 C23 C22 120.2(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.737 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.169 data_Te2Au2Te2Se _database_code_CSD 212391 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 Au2 P2 Se0.61 Te4.39' _chemical_formula_weight 1681.00 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' 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' Au Au -2.0133 8.8022 '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 10.591(3) _cell_length_b 11.161(3) _cell_length_c 21.245(5) _cell_angle_alpha 104.928(4) _cell_angle_beta 95.396(4) _cell_angle_gamma 98.466(4) _cell_volume 2377.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1530.2 _exptl_absorpt_coefficient_mu 9.377 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19937 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6844 _reflns_number_gt 5836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6844 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 1.929 _refine_ls_restrained_S_all 1.929 _refine_ls_shift/su_max 0.157 _refine_ls_shift/su_mean 0.010 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 Au1 Au 0.82790(5) 0.30404(5) 0.24101(3) 0.0333(2) Uani 1 1 d . . . Au2 Au 0.75611(5) 0.57358(5) 0.26016(3) 0.0360(2) Uani 1 1 d . . . Te1 Te 0.92154(9) 0.38489(8) 0.36234(5) 0.0342(3) Uani 1 1 d . . . Te2 Te 0.84921(9) 0.61834(9) 0.38133(5) 0.0379(3) Uani 1 1 d . . . Te3 Te 0.73988(12) 0.20529(15) 0.11983(6) 0.0703(4) Uani 1 1 d . . . Te4 Te 0.64661(13) 0.53567(14) 0.14348(7) 0.0776(5) Uani 1 1 d . . . Te5 Te 0.79257(13) 0.40352(13) 0.07791(7) 0.0534(6) Uani 0.395(12) 1 d P . . Se5 Se 0.79257(13) 0.40352(13) 0.07791(7) 0.0534(6) Uani 0.605(12) 1 d P . . P1 P 0.2627(3) 0.1003(3) 0.15382(15) 0.0246(7) Uani 1 1 d . . . P2 P 0.3436(3) 0.8167(3) 0.36852(16) 0.0229(7) Uani 1 1 d . . . C9 C -0.0981(14) -0.0273(14) 0.1862(7) 0.046(4) Uani 1 1 d . . . H9 H -0.1733 0.0068 0.1959 0.055 Uiso 1 1 calc R . . C25 C 0.3616(11) 0.7355(11) 0.4307(6) 0.022(3) Uani 1 1 d . . . C7 C 0.1210(12) -0.0004(11) 0.1627(6) 0.027(3) Uani 1 1 d . . . C32 C 0.6012(11) 0.8422(12) 0.3479(6) 0.025(3) Uani 1 1 d . . . H32 H 0.5929 0.7545 0.3438 0.030 Uiso 1 1 calc R . . C37 C 0.2382(11) 0.9258(11) 0.3928(6) 0.023(3) Uani 1 1 d . . . C33 C 0.7150(11) 0.9098(12) 0.3407(6) 0.030(3) Uani 1 1 d . . . H33 H 0.7860 0.8682 0.3315 0.036 Uiso 1 1 calc R . . C29 C 0.4885(14) 0.6769(13) 0.5147(7) 0.035(3) Uani 1 1 d . . . H29 H 0.5685 0.6827 0.5406 0.042 Uiso 1 1 calc R . . C2 C 0.3936(13) -0.0503(13) 0.0662(7) 0.034(3) Uani 1 1 d . . . H2 H 0.3413 -0.0317 0.0324 0.041 Uiso 1 1 calc R . . C8 C 0.0078(12) 0.0478(13) 0.1755(7) 0.035(3) Uani 1 1 d . . . H8 H 0.0046 0.1330 0.1768 0.041 Uiso 1 1 calc R . . C36 C 0.5105(12) 1.0331(12) 0.3684(6) 0.030(3) Uani 1 1 d . . . H36 H 0.4407 1.0759 0.3784 0.036 Uiso 1 1 calc R . . C13 C 0.2286(12) 0.1756(11) 0.0898(6) 0.026(3) Uani 1 1 d . . . C31 C 0.4973(12) 0.9044(12) 0.3614(6) 0.027(3) Uani 1 1 d . . . C35 C 0.6278(12) 1.0981(12) 0.3604(6) 0.032(3) Uani 1 1 d . . . H35 H 0.6378 1.1859 0.3647 0.039 Uiso 1 1 calc R . . C39 C 0.1561(13) 1.0666(13) 0.4782(7) 0.038(4) Uani 1 1 d . . . H39 H 0.1497 1.0992 0.5235 0.046 Uiso 1 1 calc R . . C43 C 0.2782(11) 0.7042(11) 0.2908(6) 0.024(3) Uani 1 1 d . . . C34 C 0.7287(12) 1.0370(12) 0.3466(6) 0.030(3) Uani 1 1 d . . . H34 H 0.8083 1.0821 0.3410 0.036 Uiso 1 1 calc R . . C1 C 0.3835(11) 0.0057(12) 0.1333(6) 0.025(3) Uani 1 1 d . . . C30 C 0.4811(12) 0.7440(12) 0.4680(6) 0.032(3) Uani 1 1 d . . . H30 H 0.5560 0.7951 0.4615 0.038 Uiso 1 1 calc R . . C6 C 0.4589(13) -0.0276(13) 0.1804(7) 0.037(3) Uani 1 1 d . . . H6 H 0.4533 0.0083 0.2255 0.045 Uiso 1 1 calc R . . C26 C 0.2524(12) 0.6608(13) 0.4409(6) 0.032(3) Uani 1 1 d . . . H26 H 0.1713 0.6568 0.4164 0.039 Uiso 1 1 calc R . . C14 C 0.3236(12) 0.2675(12) 0.0819(6) 0.028(3) Uani 1 1 d . . . H14 H 0.4043 0.2885 0.1094 0.034 Uiso 1 1 calc R . . C42 C 0.1690(13) 0.9697(13) 0.3465(7) 0.036(3) Uani 1 1 d . . . H42 H 0.1727 0.9348 0.3010 0.044 Uiso 1 1 calc R . . C38 C 0.2284(12) 0.9769(12) 0.4593(6) 0.030(3) Uani 1 1 d . . . H38 H 0.2733 0.9480 0.4917 0.036 Uiso 1 1 calc R . . C28 C 0.3770(13) 0.6002(12) 0.5235(6) 0.033(3) Uani 1 1 d . . . H28 H 0.3823 0.5540 0.5552 0.039 Uiso 1 1 calc R . . C12 C 0.1221(13) -0.1268(13) 0.1588(7) 0.037(3) Uani 1 1 d . . . H12 H 0.1966 -0.1626 0.1497 0.045 Uiso 1 1 calc R . . C18 C 0.1078(13) 0.1460(14) 0.0519(7) 0.040(4) Uani 1 1 d . . . H18 H 0.0434 0.0826 0.0579 0.048 Uiso 1 1 calc R . . C15 C 0.3020(14) 0.3289(12) 0.0342(7) 0.038(4) Uani 1 1 d . . . H15 H 0.3689 0.3891 0.0274 0.045 Uiso 1 1 calc R . . C27 C 0.2613(13) 0.5918(12) 0.4868(6) 0.034(3) Uani 1 1 d . . . H27 H 0.1869 0.5389 0.4925 0.041 Uiso 1 1 calc R . . C19 C 0.3229(12) 0.2218(11) 0.2292(6) 0.023(3) Uani 1 1 d . . . C44 C 0.1503(12) 0.6428(13) 0.2822(7) 0.034(3) Uani 1 1 d . . . H44 H 0.0976 0.6650 0.3156 0.040 Uiso 1 1 calc R . . C21 C 0.5000(13) 0.3710(12) 0.2983(7) 0.034(3) Uani 1 1 d . . . H21 H 0.5895 0.4049 0.3080 0.041 Uiso 1 1 calc R . . C46 C 0.1739(12) 0.5183(13) 0.1767(7) 0.041(4) Uani 1 1 d . . . H46 H 0.1384 0.4541 0.1375 0.049 Uiso 1 1 calc R . . C24 C 0.2400(12) 0.2728(13) 0.2702(6) 0.034(3) Uani 1 1 d . . . H24 H 0.1504 0.2388 0.2608 0.041 Uiso 1 1 calc R . . C20 C 0.4540(12) 0.2711(13) 0.2444(6) 0.032(3) Uani 1 1 d . . . H20 H 0.5123 0.2349 0.2171 0.038 Uiso 1 1 calc R . . C5 C 0.5426(12) -0.1117(13) 0.1641(7) 0.033(3) Uani 1 1 d . . . H5 H 0.5914 -0.1363 0.1970 0.040 Uiso 1 1 calc R . . C4 C 0.5522(14) -0.1579(13) 0.0992(7) 0.043(4) Uani 1 1 d . . . H4 H 0.6131 -0.2115 0.0873 0.052 Uiso 1 1 calc R . . C45 C 0.1011(12) 0.5502(12) 0.2250(7) 0.031(3) Uani 1 1 d . . . H45 H 0.0144 0.5079 0.2195 0.037 Uiso 1 1 calc R . . C41 C 0.0953(14) 1.0626(14) 0.3649(7) 0.043(4) Uani 1 1 d . . . H41 H 0.0495 1.0912 0.3326 0.051 Uiso 1 1 calc R . . C3 C 0.4779(15) -0.1304(13) 0.0504(7) 0.043(4) Uani 1 1 d . . . H3 H 0.4851 -0.1672 0.0056 0.051 Uiso 1 1 calc R . . C22 C 0.4161(12) 0.4217(12) 0.3381(6) 0.031(3) Uani 1 1 d . . . H22 H 0.4480 0.4914 0.3755 0.037 Uiso 1 1 calc R . . C11 C 0.0104(15) -0.1991(14) 0.1686(7) 0.046(4) Uani 1 1 d . . . H11 H 0.0083 -0.2860 0.1652 0.055 Uiso 1 1 calc R . . C23 C 0.2865(13) 0.3735(14) 0.3250(7) 0.041(4) Uani 1 1 d . . . H23 H 0.2292 0.4090 0.3533 0.049 Uiso 1 1 calc R . . C40 C 0.0895(13) 1.1126(13) 0.4305(7) 0.041(4) Uani 1 1 d . . . H40 H 0.0412 1.1777 0.4440 0.049 Uiso 1 1 calc R . . C48 C 0.3496(13) 0.6763(14) 0.2415(8) 0.046(4) Uani 1 1 d . . . H48 H 0.4341 0.7227 0.2456 0.056 Uiso 1 1 calc R . . C17 C 0.0817(16) 0.2104(16) 0.0051(7) 0.055(5) Uani 1 1 d . . . H17 H -0.0012 0.1931 -0.0200 0.066 Uiso 1 1 calc R . . C16 C 0.1804(16) 0.3016(15) -0.0043(7) 0.048(4) Uani 1 1 d . . . H16 H 0.1645 0.3446 -0.0367 0.058 Uiso 1 1 calc R . . C10 C -0.0962(15) -0.1468(15) 0.1830(7) 0.049(4) Uani 1 1 d . . . H10 H -0.1701 -0.1974 0.1909 0.058 Uiso 1 1 calc R . . C47 C 0.2997(16) 0.5789(19) 0.1841(8) 0.070(6) Uani 1 1 d . . . H47 H 0.3521 0.5551 0.1507 0.084 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 Au1 0.0303(3) 0.0343(4) 0.0367(4) 0.0109(3) 0.0080(3) 0.0059(2) Au2 0.0321(4) 0.0269(3) 0.0490(4) 0.0102(3) 0.0088(3) 0.0038(2) Te1 0.0352(5) 0.0311(5) 0.0380(6) 0.0096(4) 0.0091(4) 0.0083(4) Te2 0.0355(5) 0.0290(5) 0.0458(6) 0.0028(4) 0.0116(4) 0.0049(4) Te3 0.0488(7) 0.1115(12) 0.0456(7) 0.0215(7) -0.0004(6) 0.0030(7) Te4 0.0675(9) 0.0777(10) 0.0795(10) 0.0379(8) -0.0143(7) -0.0255(7) Te5 0.0538(10) 0.0543(10) 0.0482(9) 0.0208(7) -0.0027(7) -0.0089(7) Se5 0.0538(10) 0.0543(10) 0.0482(9) 0.0208(7) -0.0027(7) -0.0089(7) P1 0.0238(17) 0.0262(18) 0.0208(18) 0.0025(14) 0.0016(14) 0.0032(14) P2 0.0240(17) 0.0209(17) 0.0253(18) 0.0072(14) 0.0068(14) 0.0053(14) C9 0.030(8) 0.041(10) 0.055(10) 0.000(8) 0.005(7) -0.009(7) C25 0.024(7) 0.020(7) 0.020(7) 0.002(5) 0.002(5) 0.008(5) C7 0.030(7) 0.023(7) 0.027(7) 0.007(6) 0.001(6) 0.010(6) C32 0.030(7) 0.025(7) 0.028(7) 0.013(6) 0.011(6) 0.013(6) C37 0.024(7) 0.019(6) 0.025(7) 0.003(5) 0.007(5) 0.002(5) C33 0.019(7) 0.025(7) 0.039(8) -0.002(6) 0.006(6) 0.004(6) C29 0.044(8) 0.028(8) 0.033(8) 0.004(6) 0.001(6) 0.015(7) C2 0.031(7) 0.045(9) 0.034(8) 0.018(7) 0.009(6) 0.015(7) C8 0.029(8) 0.029(8) 0.038(8) -0.005(6) 0.008(6) 0.005(6) C36 0.029(7) 0.028(8) 0.031(8) 0.004(6) 0.011(6) 0.003(6) C13 0.029(7) 0.022(7) 0.026(7) 0.004(6) 0.002(6) 0.007(6) C31 0.025(7) 0.028(7) 0.025(7) 0.004(6) -0.001(5) -0.001(6) C35 0.038(8) 0.023(7) 0.030(8) -0.002(6) 0.010(6) -0.001(6) C39 0.038(8) 0.041(9) 0.033(8) -0.002(7) 0.008(6) 0.017(7) C43 0.023(7) 0.025(7) 0.027(7) 0.012(6) 0.005(5) 0.008(6) C34 0.024(7) 0.025(7) 0.036(8) 0.000(6) 0.005(6) 0.005(6) C1 0.019(6) 0.029(7) 0.031(8) 0.010(6) 0.010(6) 0.010(5) C30 0.027(7) 0.026(7) 0.040(8) 0.011(6) 0.003(6) -0.002(6) C6 0.033(8) 0.044(9) 0.030(8) 0.009(7) -0.002(6) -0.005(7) C26 0.027(7) 0.042(8) 0.029(8) 0.014(6) 0.002(6) 0.002(6) C14 0.027(7) 0.033(8) 0.025(7) 0.010(6) 0.003(6) 0.005(6) C42 0.046(9) 0.035(8) 0.027(8) 0.010(6) 0.001(6) 0.004(7) C38 0.034(7) 0.028(7) 0.028(8) 0.010(6) -0.001(6) 0.008(6) C28 0.048(9) 0.034(8) 0.015(7) 0.008(6) 0.001(6) 0.007(7) C12 0.036(8) 0.033(8) 0.039(8) 0.010(6) -0.013(7) 0.006(7) C18 0.041(9) 0.045(9) 0.031(8) 0.013(7) -0.002(7) -0.001(7) C15 0.057(10) 0.018(7) 0.038(9) 0.000(6) 0.025(7) 0.007(6) C27 0.042(8) 0.030(8) 0.030(8) 0.006(6) 0.013(7) 0.002(6) C19 0.032(7) 0.016(6) 0.028(7) 0.014(5) 0.008(6) 0.007(5) C44 0.017(7) 0.050(9) 0.028(8) 0.008(7) -0.001(6) -0.004(6) C21 0.024(7) 0.034(8) 0.040(8) 0.009(7) -0.001(6) -0.006(6) C46 0.026(8) 0.039(9) 0.043(9) -0.005(7) -0.007(7) -0.003(6) C24 0.021(7) 0.040(8) 0.032(8) -0.001(6) -0.003(6) -0.003(6) C20 0.021(7) 0.038(8) 0.035(8) 0.002(6) 0.012(6) 0.005(6) C5 0.025(7) 0.048(9) 0.031(8) 0.014(7) 0.006(6) 0.013(6) C4 0.050(9) 0.028(8) 0.055(11) 0.009(7) 0.023(8) 0.009(7) C45 0.024(7) 0.027(7) 0.042(9) 0.015(6) -0.001(6) -0.003(6) C41 0.052(9) 0.051(10) 0.036(9) 0.018(7) 0.011(7) 0.026(8) C3 0.068(10) 0.030(8) 0.031(8) 0.000(6) 0.000(7) 0.030(8) C22 0.036(8) 0.027(7) 0.025(7) -0.002(6) -0.006(6) 0.014(6) C11 0.058(11) 0.031(8) 0.041(9) 0.020(7) -0.015(8) -0.019(8) C23 0.026(8) 0.054(10) 0.037(9) -0.003(7) 0.003(6) 0.016(7) C40 0.040(8) 0.035(8) 0.051(10) 0.008(7) 0.012(7) 0.021(7) C48 0.029(8) 0.041(9) 0.057(10) -0.007(8) 0.020(7) -0.003(7) C17 0.061(11) 0.059(11) 0.037(9) 0.017(8) -0.029(8) 0.002(9) C16 0.070(11) 0.047(10) 0.035(9) 0.028(7) 0.005(8) 0.008(8) C10 0.039(9) 0.054(11) 0.046(10) 0.012(8) 0.004(7) -0.012(8) C47 0.047(10) 0.104(16) 0.038(10) -0.020(10) 0.011(8) 0.015(10) _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 Au1 Te1 2.5495(12) . ? Au1 Te3 2.5486(14) . ? Au1 Au2 3.1456(10) . ? Au2 Te4 2.5385(15) . ? Au2 Te2 2.5619(12) . ? Te1 Te2 2.7645(14) . ? Te3 Te5 2.597(2) . ? Te4 Te5 2.554(2) . ? P1 C1 1.791(12) . ? P1 C7 1.793(13) . ? P1 C19 1.801(13) . ? P1 C13 1.810(13) . ? P2 C37 1.783(12) . ? P2 C43 1.801(13) . ? P2 C25 1.795(12) . ? P2 C31 1.813(13) . ? C9 C10 1.32(2) . ? C9 C8 1.371(19) . ? C25 C26 1.391(17) . ? C25 C30 1.406(17) . ? C7 C8 1.406(17) . ? C7 C12 1.393(18) . ? C32 C33 1.368(17) . ? C32 C31 1.398(17) . ? C37 C38 1.401(17) . ? C37 C42 1.402(18) . ? C33 C34 1.377(17) . ? C29 C30 1.392(18) . ? C29 C28 1.411(19) . ? C2 C3 1.358(18) . ? C2 C1 1.421(18) . ? C36 C31 1.390(18) . ? C36 C35 1.391(18) . ? C13 C14 1.381(18) . ? C13 C18 1.392(18) . ? C35 C34 1.365(17) . ? C39 C38 1.351(18) . ? C39 C40 1.42(2) . ? C43 C48 1.348(18) . ? C43 C44 1.397(17) . ? C1 C6 1.381(18) . ? C6 C5 1.386(19) . ? C26 C27 1.395(18) . ? C14 C15 1.382(19) . ? C42 C41 1.388(19) . ? C28 C27 1.366(19) . ? C12 C11 1.39(2) . ? C18 C17 1.40(2) . ? C15 C16 1.41(2) . ? C19 C24 1.374(17) . ? C19 C20 1.391(17) . ? C44 C45 1.375(18) . ? C21 C20 1.367(18) . ? C21 C22 1.367(18) . ? C46 C45 1.347(19) . ? C46 C47 1.38(2) . ? C24 C23 1.386(18) . ? C5 C4 1.363(19) . ? C4 C3 1.37(2) . ? C41 C40 1.37(2) . ? C22 C23 1.373(18) . ? C11 C10 1.37(2) . ? C48 C47 1.41(2) . ? C17 C16 1.41(2) . ? 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 Te1 Au1 Te3 175.11(4) . . ? Te1 Au1 Au2 84.81(3) . . ? Te3 Au1 Au2 100.08(4) . . ? Te4 Au2 Te2 175.09(4) . . ? Te4 Au2 Au1 96.46(4) . . ? Te2 Au2 Au1 86.58(3) . . ? Au1 Te1 Te2 95.51(4) . . ? Au2 Te2 Te1 92.99(4) . . ? Au1 Te3 Te5 98.69(6) . . ? Au2 Te4 Te5 101.06(6) . . ? Te4 Te5 Te3 97.66(6) . . ? C1 P1 C7 108.1(6) . . ? C1 P1 C19 109.0(6) . . ? C7 P1 C19 111.1(6) . . ? C1 P1 C13 109.8(6) . . ? C7 P1 C13 110.8(6) . . ? C19 P1 C13 108.1(6) . . ? C37 P2 C43 110.9(6) . . ? C37 P2 C25 107.9(6) . . ? C43 P2 C25 109.4(6) . . ? C37 P2 C31 108.3(6) . . ? C43 P2 C31 109.6(6) . . ? C25 P2 C31 110.8(6) . . ? C10 C9 C8 120.5(15) . . ? C26 C25 C30 119.8(11) . . ? C26 C25 P2 117.8(9) . . ? C30 C25 P2 122.4(9) . . ? C8 C7 C12 118.8(12) . . ? C8 C7 P1 120.5(10) . . ? C12 C7 P1 120.7(10) . . ? C33 C32 C31 118.9(12) . . ? C38 C37 C42 117.7(12) . . ? C38 C37 P2 121.0(10) . . ? C42 C37 P2 121.2(10) . . ? C32 C33 C34 121.3(12) . . ? C30 C29 C28 119.8(12) . . ? C3 C2 C1 120.2(12) . . ? C9 C8 C7 120.5(14) . . ? C31 C36 C35 118.8(12) . . ? C14 C13 C18 121.2(12) . . ? C14 C13 P1 118.0(9) . . ? C18 C13 P1 120.7(10) . . ? C32 C31 C36 120.4(11) . . ? C32 C31 P2 120.0(10) . . ? C36 C31 P2 119.6(10) . . ? C34 C35 C36 120.7(13) . . ? C38 C39 C40 120.2(13) . . ? C48 C43 C44 119.4(12) . . ? C48 C43 P2 121.9(10) . . ? C44 C43 P2 118.7(10) . . ? C35 C34 C33 119.9(12) . . ? C6 C1 C2 117.5(12) . . ? C6 C1 P1 122.1(10) . . ? C2 C1 P1 120.0(9) . . ? C29 C30 C25 119.4(12) . . ? C5 C6 C1 122.3(13) . . ? C27 C26 C25 120.4(12) . . ? C15 C14 C13 120.3(12) . . ? C41 C42 C37 122.0(13) . . ? C39 C38 C37 121.2(12) . . ? C27 C28 C29 120.5(12) . . ? C7 C12 C11 118.0(13) . . ? C13 C18 C17 119.5(14) . . ? C14 C15 C16 119.6(13) . . ? C28 C27 C26 120.0(13) . . ? C24 C19 C20 119.0(12) . . ? C24 C19 P1 120.9(9) . . ? C20 C19 P1 120.0(9) . . ? C45 C44 C43 119.7(13) . . ? C20 C21 C22 119.5(12) . . ? C45 C46 C47 120.1(13) . . ? C19 C24 C23 120.3(12) . . ? C21 C20 C19 120.8(12) . . ? C4 C5 C6 117.4(13) . . ? C5 C4 C3 122.7(14) . . ? C46 C45 C44 121.0(12) . . ? C42 C41 C40 119.0(13) . . ? C2 C3 C4 119.8(14) . . ? C21 C22 C23 121.1(12) . . ? C10 C11 C12 121.0(14) . . ? C22 C23 C24 119.4(12) . . ? C41 C40 C39 119.9(13) . . ? C43 C48 C47 120.3(13) . . ? C18 C17 C16 119.2(13) . . ? C15 C16 C17 120.1(13) . . ? C9 C10 C11 121.2(14) . . ? C46 C47 C48 119.3(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 7.069 _refine_diff_density_min -5.714 _refine_diff_density_rms 0.267