# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'du Mont, Wolf-Walther' 'Armand Blaschette' 'Constantin Daniliuc' 'Christian Druckenbrodt' 'Cristian Hrib' 'Peter G Jones' 'Frank Ruthe' _publ_contact_author_name 'Wolf-Walther du Mont' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Technischen Universitat Carolo-Wilhelmina Braunschweig Postfach 3329 Braunschweig 38023 GERMANY ; _publ_contact_author_email W.DU-MONT@TU-BS.DE _publ_requested_journal 'Chemical Communications' _publ_section_title ; The First Trialkylphosphane Telluride Complexes of Ag(I): Molecular, Ionic and Supramolecular Structural Alternatives ; data_hoover _database_code_depnum_ccdc_archive 'CCDC 611403' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H54 Ag2 N2 O8 P2 S4 Te2' _chemical_formula_weight 1135.80 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' 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' 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' Ag Ag -0.8971 1.1015 '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' 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 11.7663(15) _cell_length_b 7.794(2) _cell_length_c 21.802(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.457(15) _cell_angle_gamma 90.00 _cell_volume 1927.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.841 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details XEMP _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Stoe STADI-4' _diffrn_measurement_method \w-\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 3602 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3396 _reflns_number_gt 2964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _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^)+(0.0191P)^2^+2.8449P] 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 'rigid methyls, others riding' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00107(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3396 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Ag Ag 0.44118(3) 0.42400(5) 0.544189(16) 0.03006(11) Uani 1 1 d . . . P P 0.78925(9) 0.49022(13) 0.61376(5) 0.0188(2) Uani 1 1 d . . . Te Te 0.61753(2) 0.67431(4) 0.584065(13) 0.02564(10) Uani 1 1 d . . . C1 C 0.8148(4) 0.4297(6) 0.69767(19) 0.0255(9) Uani 1 1 d . . . H1 H 0.8374 0.5384 0.7223 0.031 Uiso 1 1 calc R . . C2 C 0.7047(4) 0.3653(6) 0.7152(2) 0.0393(12) Uani 1 1 d . . . H2A H 0.6797 0.2559 0.6937 0.047 Uiso 1 1 calc R . . H2B H 0.6412 0.4498 0.7017 0.047 Uiso 1 1 calc R . . H2C H 0.7227 0.3491 0.7613 0.047 Uiso 1 1 calc R . . C3 C 0.9196(4) 0.3087(6) 0.7212(2) 0.0324(10) Uani 1 1 d . . . H3A H 0.9408 0.3035 0.7678 0.039 Uiso 1 1 calc R . . H3B H 0.9870 0.3514 0.7073 0.039 Uiso 1 1 calc R . . H3C H 0.8983 0.1938 0.7037 0.039 Uiso 1 1 calc R . . C4 C 0.7790(4) 0.3059(5) 0.5599(2) 0.0247(9) Uani 1 1 d . . . H4 H 0.7503 0.3516 0.5156 0.030 Uiso 1 1 calc R . . C5 C 0.6895(4) 0.1721(6) 0.5677(2) 0.0362(11) Uani 1 1 d . . . H5A H 0.6741 0.0919 0.5318 0.043 Uiso 1 1 calc R . . H5B H 0.6159 0.2293 0.5688 0.043 Uiso 1 1 calc R . . H5C H 0.7208 0.1091 0.6075 0.043 Uiso 1 1 calc R . . C6 C 0.8988(4) 0.2194(6) 0.5644(2) 0.0301(10) Uani 1 1 d . . . H6A H 0.9277 0.1646 0.6061 0.036 Uiso 1 1 calc R . . H6B H 0.9557 0.3060 0.5589 0.036 Uiso 1 1 calc R . . H6C H 0.8892 0.1325 0.5309 0.036 Uiso 1 1 calc R . . C7 C 0.9185(3) 0.6140(5) 0.60822(18) 0.0218(9) Uani 1 1 d . . . H7 H 0.9889 0.5371 0.6212 0.026 Uiso 1 1 calc R . . C8 C 0.9069(4) 0.6720(6) 0.5396(2) 0.0338(11) Uani 1 1 d . . . H8A H 0.8414 0.7535 0.5265 0.041 Uiso 1 1 calc R . . H8B H 0.8916 0.5721 0.5113 0.041 Uiso 1 1 calc R . . H8C H 0.9802 0.7276 0.5371 0.041 Uiso 1 1 calc R . . C9 C 0.9407(4) 0.7687(6) 0.6527(2) 0.0305(10) Uani 1 1 d . . . H9A H 1.0090 0.8328 0.6474 0.037 Uiso 1 1 calc R . . H9B H 0.9561 0.7294 0.6969 0.037 Uiso 1 1 calc R . . H9C H 0.8711 0.8433 0.6425 0.037 Uiso 1 1 calc R . . N N 0.3458(3) 0.3239(5) 0.61406(18) 0.0320(9) Uani 1 1 d . . . S1 S 0.25854(9) 0.44701(13) 0.63912(5) 0.0244(2) Uani 1 1 d . . . S2 S 0.37206(10) 0.13103(14) 0.64150(6) 0.0317(3) Uani 1 1 d . . . O1 O 0.2326(3) 0.5890(4) 0.59566(15) 0.0453(9) Uani 1 1 d . . . O2 O 0.1597(3) 0.3549(4) 0.64905(17) 0.0419(8) Uani 1 1 d . . . O3 O 0.4637(4) 0.0672(5) 0.6165(3) 0.0808(16) Uani 1 1 d . . . O4 O 0.3895(3) 0.1239(5) 0.70868(16) 0.0539(10) Uani 1 1 d . . . C11 C 0.3373(5) 0.5285(7) 0.7131(2) 0.0498(14) Uani 1 1 d . . . H11A H 0.2871 0.6080 0.7289 0.060 Uiso 1 1 calc R . . H11B H 0.4073 0.5894 0.7084 0.060 Uiso 1 1 calc R . . H11C H 0.3615 0.4338 0.7433 0.060 Uiso 1 1 calc R . . C12 C 0.2461(5) 0.0110(6) 0.6074(3) 0.0466(13) Uani 1 1 d . . . H12A H 0.2610 -0.1100 0.6190 0.056 Uiso 1 1 calc R . . H12B H 0.2261 0.0226 0.5610 0.056 Uiso 1 1 calc R . . H12C H 0.1804 0.0527 0.6230 0.056 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 Ag 0.02144(18) 0.0361(2) 0.0349(2) 0.01263(15) 0.01140(14) 0.00126(15) P 0.0180(5) 0.0188(5) 0.0208(5) 0.0030(4) 0.0074(4) 0.0006(4) Te 0.01946(15) 0.02315(15) 0.03374(17) 0.00209(12) 0.00611(12) 0.00316(12) C1 0.030(2) 0.027(2) 0.022(2) 0.0049(18) 0.0117(18) 0.0041(19) C2 0.042(3) 0.045(3) 0.041(3) 0.016(2) 0.027(2) 0.009(2) C3 0.034(3) 0.034(3) 0.028(2) 0.008(2) 0.008(2) 0.002(2) C4 0.025(2) 0.019(2) 0.029(2) 0.0003(18) 0.0045(18) -0.0005(17) C5 0.029(2) 0.026(2) 0.056(3) -0.007(2) 0.015(2) -0.004(2) C6 0.029(2) 0.028(2) 0.037(3) -0.009(2) 0.015(2) 0.001(2) C7 0.016(2) 0.026(2) 0.025(2) 0.0033(17) 0.0065(17) -0.0014(17) C8 0.035(3) 0.038(3) 0.029(2) 0.003(2) 0.010(2) -0.012(2) C9 0.028(2) 0.033(2) 0.030(2) -0.002(2) 0.0065(19) -0.008(2) N 0.038(2) 0.0237(19) 0.043(2) 0.0060(17) 0.0247(18) -0.0015(17) S1 0.0245(5) 0.0226(5) 0.0244(5) -0.0009(4) 0.0037(4) -0.0009(4) S2 0.0257(6) 0.0259(6) 0.0471(7) 0.0077(5) 0.0163(5) 0.0028(5) O1 0.075(3) 0.0241(17) 0.0342(18) 0.0044(15) 0.0099(18) 0.0081(17) O2 0.0234(17) 0.0331(18) 0.072(2) -0.0053(17) 0.0171(17) -0.0016(15) O3 0.070(3) 0.041(2) 0.162(5) 0.016(3) 0.085(3) 0.020(2) O4 0.067(3) 0.043(2) 0.038(2) 0.0108(17) -0.0102(18) 0.0072(19) C11 0.057(4) 0.048(3) 0.034(3) -0.014(2) -0.005(3) 0.005(3) C12 0.052(3) 0.022(2) 0.061(3) -0.006(2) 0.006(3) -0.002(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 Ag N 2.258(3) . ? Ag Te 2.8024(6) 3_666 ? Ag Te 2.8117(6) . ? Ag Ag 2.9075(7) 3_666 ? P C7 1.832(4) . ? P C1 1.835(4) . ? P C4 1.839(4) . ? P Te 2.4214(11) . ? Te Ag 2.8024(6) 3_666 ? C1 C3 1.529(6) . ? C1 C2 1.529(6) . ? C4 C5 1.524(6) . ? C4 C6 1.542(6) . ? C7 C9 1.526(6) . ? C7 C8 1.534(6) . ? N S1 1.604(4) . ? N S2 1.617(4) . ? S1 O2 1.432(3) . ? S1 O1 1.436(3) . ? S1 C11 1.751(5) . ? S2 O3 1.422(4) . ? S2 O4 1.425(4) . ? S2 C12 1.743(5) . ? 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 N Ag Te 122.95(10) . 3_666 ? N Ag Te 119.31(10) . . ? Te Ag Te 117.618(16) 3_666 . ? N Ag Ag 176.14(10) . 3_666 ? Te Ag Ag 58.965(17) 3_666 3_666 ? Te Ag Ag 58.654(16) . 3_666 ? C7 P C1 106.42(19) . . ? C7 P C4 106.47(19) . . ? C1 P C4 113.7(2) . . ? C7 P Te 108.58(14) . . ? C1 P Te 108.79(14) . . ? C4 P Te 112.61(14) . . ? P Te Ag 94.07(3) . 3_666 ? P Te Ag 99.55(3) . . ? Ag Te Ag 62.382(16) 3_666 . ? C3 C1 C2 112.0(4) . . ? C3 C1 P 113.4(3) . . ? C2 C1 P 114.1(3) . . ? C5 C4 C6 110.0(3) . . ? C5 C4 P 113.1(3) . . ? C6 C4 P 113.5(3) . . ? C9 C7 C8 110.1(3) . . ? C9 C7 P 112.2(3) . . ? C8 C7 P 111.1(3) . . ? S1 N S2 120.4(2) . . ? S1 N Ag 120.10(19) . . ? S2 N Ag 119.38(19) . . ? O2 S1 O1 116.6(2) . . ? O2 S1 N 111.80(19) . . ? O1 S1 N 106.2(2) . . ? O2 S1 C11 107.1(3) . . ? O1 S1 C11 107.2(2) . . ? N S1 C11 107.5(2) . . ? O3 S2 O4 117.7(3) . . ? O3 S2 N 105.8(2) . . ? O4 S2 N 112.2(2) . . ? O3 S2 C12 107.1(3) . . ? O4 S2 C12 106.9(3) . . ? N S2 C12 106.5(2) . . ? 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 C7 P Te Ag 92.66(14) . . . 3_666 ? C1 P Te Ag -151.91(15) . . . 3_666 ? C4 P Te Ag -24.99(15) . . . 3_666 ? C7 P Te Ag 155.32(14) . . . . ? C1 P Te Ag -89.25(15) . . . . ? C4 P Te Ag 37.67(15) . . . . ? N Ag Te P 94.20(11) . . . . ? Te Ag Te P -89.61(3) 3_666 . . . ? Ag Ag Te P -89.61(3) 3_666 . . . ? N Ag Te Ag -176.20(11) . . . 3_666 ? Te Ag Te Ag 0.0 3_666 . . 3_666 ? C7 P C1 C3 -64.8(4) . . . . ? C4 P C1 C3 52.1(4) . . . . ? Te P C1 C3 178.4(3) . . . . ? C7 P C1 C2 165.3(3) . . . . ? C4 P C1 C2 -77.8(4) . . . . ? Te P C1 C2 48.5(3) . . . . ? C7 P C4 C5 169.6(3) . . . . ? C1 P C4 C5 52.7(4) . . . . ? Te P C4 C5 -71.6(3) . . . . ? C7 P C4 C6 43.4(3) . . . . ? C1 P C4 C6 -73.5(3) . . . . ? Te P C4 C6 162.2(3) . . . . ? C1 P C7 C9 -56.3(3) . . . . ? C4 P C7 C9 -177.8(3) . . . . ? Te P C7 C9 60.7(3) . . . . ? C1 P C7 C8 -180.0(3) . . . . ? C4 P C7 C8 58.5(3) . . . . ? Te P C7 C8 -63.0(3) . . . . ? Te Ag N S1 -107.7(2) 3_666 . . . ? Te Ag N S1 68.3(3) . . . . ? Ag Ag N S1 11.0(17) 3_666 . . . ? Te Ag N S2 75.8(2) 3_666 . . . ? Te Ag N S2 -108.3(2) . . . . ? Ag Ag N S2 -165.5(13) 3_666 . . . ? S2 N S1 O2 -38.4(3) . . . . ? Ag N S1 O2 145.1(2) . . . . ? S2 N S1 O1 -166.6(3) . . . . ? Ag N S1 O1 16.9(3) . . . . ? S2 N S1 C11 78.9(3) . . . . ? Ag N S1 C11 -97.6(3) . . . . ? S1 N S2 O3 -172.1(3) . . . . ? Ag N S2 O3 4.4(3) . . . . ? S1 N S2 O4 -42.5(4) . . . . ? Ag N S2 O4 134.0(2) . . . . ? S1 N S2 C12 74.1(3) . . . . ? Ag N S2 C12 -109.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 O1 1.00 2.53 3.457(5) 153.9 3_666 C3 H3B O2 0.98 2.67 3.599(6) 158.9 1_655 C7 H7 O2 1.00 2.40 3.402(5) 178.0 1_655 C5 H5B O3 0.98 2.62 3.218(6) 119.4 . C9 H9B O4 0.98 2.49 3.343(6) 144.8 2_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.096 # Attachment 'DROGI.CIF.doc' data_drogi _database_code_depnum_ccdc_archive 'CCDC 611440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H99 Ag2 N3 O8 P4 S4 Te4' _chemical_formula_weight 1752.50 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' O O 0.0106 0.0060 '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' Ag Ag -0.8971 1.1015 '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' 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 11.4760(15) _cell_length_b 15.363(3) _cell_length_c 38.378(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.962(10) _cell_angle_gamma 90.00 _cell_volume 6749.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11.5 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 2.536 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details XEMP _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Stoe STADI-4' _diffrn_measurement_method \w-\q-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 12445 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11815 _reflns_number_gt 8595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _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^)+(0.0225P)^2^+35.9073P] 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 'ordered methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11815 _refine_ls_number_parameters 629 _refine_ls_number_restraints 609 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.004 _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 Ag1 Ag 0.51702(6) 0.38929(5) 0.638657(17) 0.03716(17) Uani 1 1 d . . . Ag2 Ag 0.55911(6) 0.19552(4) 0.662676(17) 0.03450(16) Uani 1 1 d . . . Te1 Te 0.66234(5) 0.47582(4) 0.686086(15) 0.03790(15) Uani 1 1 d . . . Te2 Te 0.34249(4) 0.27939(4) 0.658298(13) 0.02782(13) Uani 1 1 d . . . Te3 Te 0.51047(5) 0.42427(4) 0.569120(14) 0.03535(15) Uani 1 1 d . . . Te4 Te 0.75811(5) 0.26140(4) 0.640062(16) 0.03476(14) Uani 1 1 d . A . P1 P 0.69505(17) 0.61558(14) 0.66055(6) 0.0276(5) Uani 1 1 d . . . P2 P 0.30320(18) 0.32249(14) 0.71701(5) 0.0268(5) Uani 1 1 d . . . P3 P 0.31156(18) 0.42729(15) 0.54498(5) 0.0276(5) Uani 1 1 d . . . C1 C 0.7239(7) 0.6957(6) 0.6956(2) 0.039(2) Uani 1 1 d U . . H1 H 0.8007 0.6787 0.7075 0.047 Uiso 1 1 calc R . . C2 C 0.6377(10) 0.6951(7) 0.7238(3) 0.066(3) Uani 1 1 d U . . H2A H 0.6664 0.7329 0.7431 0.079 Uiso 1 1 calc R . . H2B H 0.6292 0.6356 0.7325 0.079 Uiso 1 1 calc R . . H2C H 0.5617 0.7163 0.7141 0.079 Uiso 1 1 calc R . . C3 C 0.7413(8) 0.7868(6) 0.6818(3) 0.047(2) Uani 1 1 d U . . H3A H 0.6670 0.8088 0.6711 0.057 Uiso 1 1 calc R . . H3B H 0.7994 0.7854 0.6643 0.057 Uiso 1 1 calc R . . H3C H 0.7687 0.8250 0.7011 0.057 Uiso 1 1 calc R . . C4 C 0.5705(7) 0.6454(6) 0.6303(2) 0.041(2) Uani 1 1 d U . . H4 H 0.5547 0.5934 0.6151 0.049 Uiso 1 1 calc R . . C5 C 0.5918(10) 0.7204(7) 0.6057(3) 0.067(3) Uani 1 1 d U . . H5A H 0.5310 0.7205 0.5864 0.081 Uiso 1 1 calc R . . H5B H 0.6685 0.7135 0.5963 0.081 Uiso 1 1 calc R . . H5C H 0.5895 0.7756 0.6184 0.081 Uiso 1 1 calc R . . C6 C 0.4592(7) 0.6602(7) 0.6493(3) 0.059(3) Uani 1 1 d U . . H6A H 0.4631 0.7171 0.6608 0.071 Uiso 1 1 calc R . . H6B H 0.4520 0.6144 0.6668 0.071 Uiso 1 1 calc R . . H6C H 0.3912 0.6584 0.6324 0.071 Uiso 1 1 calc R . . C7 C 0.8233(7) 0.6144(6) 0.6354(2) 0.038(2) Uani 1 1 d U . . H7 H 0.8313 0.6737 0.6250 0.045 Uiso 1 1 calc R . . C8 C 0.8078(9) 0.5500(6) 0.6053(2) 0.053(3) Uani 1 1 d U . . H8A H 0.8718 0.5570 0.5899 0.064 Uiso 1 1 calc R . . H8B H 0.7331 0.5609 0.5921 0.064 Uiso 1 1 calc R . . H8C H 0.8086 0.4905 0.6146 0.064 Uiso 1 1 calc R . . C9 C 0.9355(7) 0.5956(7) 0.6583(3) 0.056(3) Uani 1 1 d U . . H9A H 1.0016 0.5912 0.6435 0.067 Uiso 1 1 calc R . . H9B H 0.9269 0.5407 0.6708 0.067 Uiso 1 1 calc R . . H9C H 0.9498 0.6430 0.6751 0.067 Uiso 1 1 calc R . . C10 C 0.2707(8) 0.2271(5) 0.7429(2) 0.038(2) Uani 1 1 d U . . H10 H 0.3431 0.1907 0.7438 0.045 Uiso 1 1 calc R . . C11 C 0.2502(10) 0.2485(7) 0.7808(2) 0.056(3) Uani 1 1 d U . . H11A H 0.1848 0.2893 0.7815 0.067 Uiso 1 1 calc R . . H11B H 0.3208 0.2751 0.7921 0.067 Uiso 1 1 calc R . . H11C H 0.2320 0.1950 0.7932 0.067 Uiso 1 1 calc R . . C12 C 0.1753(9) 0.1705(6) 0.7260(3) 0.053(3) Uani 1 1 d U . . H12A H 0.1819 0.1116 0.7357 0.063 Uiso 1 1 calc R . . H12B H 0.1830 0.1681 0.7007 0.063 Uiso 1 1 calc R . . H12C H 0.0990 0.1949 0.7305 0.063 Uiso 1 1 calc R . . C13 C 0.1808(7) 0.3991(5) 0.7129(2) 0.036(2) Uani 1 1 d U . . H13 H 0.1577 0.4115 0.7370 0.043 Uiso 1 1 calc R . . C14 C 0.0735(7) 0.3630(7) 0.6923(3) 0.062(3) Uani 1 1 d U . . H14A H 0.0172 0.4100 0.6873 0.075 Uiso 1 1 calc R . . H14B H 0.0377 0.3178 0.7061 0.075 Uiso 1 1 calc R . . H14C H 0.0965 0.3379 0.6704 0.075 Uiso 1 1 calc R . . C15 C 0.2186(9) 0.4854(6) 0.6975(2) 0.047(2) Uani 1 1 d U . . H15A H 0.2373 0.4766 0.6732 0.057 Uiso 1 1 calc R . . H15B H 0.2878 0.5073 0.7111 0.057 Uiso 1 1 calc R . . H15C H 0.1550 0.5278 0.6983 0.057 Uiso 1 1 calc R . . C16 C 0.4272(7) 0.3808(5) 0.7384(2) 0.0295(18) Uani 1 1 d U . . H16 H 0.4513 0.4247 0.7211 0.035 Uiso 1 1 calc R . . C17 C 0.5331(7) 0.3223(6) 0.7461(2) 0.042(2) Uani 1 1 d U . . H17A H 0.5992 0.3574 0.7556 0.051 Uiso 1 1 calc R . . H17B H 0.5538 0.2940 0.7245 0.051 Uiso 1 1 calc R . . H17C H 0.5146 0.2778 0.7632 0.051 Uiso 1 1 calc R . . C18 C 0.3995(9) 0.4327(6) 0.7710(2) 0.047(2) Uani 1 1 d U . . H18A H 0.4001 0.3934 0.7912 0.056 Uiso 1 1 calc R . . H18B H 0.3223 0.4595 0.7672 0.056 Uiso 1 1 calc R . . H18C H 0.4586 0.4781 0.7755 0.056 Uiso 1 1 calc R . . C19 C 0.2740(7) 0.3233(6) 0.5228(2) 0.037(2) Uani 1 1 d U . . H19 H 0.1924 0.3279 0.5121 0.044 Uiso 1 1 calc R . . C20 C 0.2782(9) 0.2481(6) 0.5490(3) 0.054(3) Uani 1 1 d U . . H20A H 0.2576 0.1936 0.5368 0.065 Uiso 1 1 calc R . . H20B H 0.2226 0.2591 0.5668 0.065 Uiso 1 1 calc R . . H20C H 0.3572 0.2433 0.5603 0.065 Uiso 1 1 calc R . . C21 C 0.3546(8) 0.3036(7) 0.4940(3) 0.053(3) Uani 1 1 d U . . H21A H 0.4358 0.3031 0.5037 0.063 Uiso 1 1 calc R . . H21B H 0.3450 0.3485 0.4758 0.063 Uiso 1 1 calc R . . H21C H 0.3348 0.2466 0.4837 0.063 Uiso 1 1 calc R . . C22 C 0.2079(7) 0.4416(6) 0.5791(2) 0.037(2) Uani 1 1 d U . . H22 H 0.2293 0.3970 0.5975 0.045 Uiso 1 1 calc R . . C23 C 0.0799(8) 0.4231(8) 0.5664(3) 0.061(3) Uani 1 1 d U . . H23A H 0.0323 0.4185 0.5865 0.073 Uiso 1 1 calc R . . H23B H 0.0757 0.3684 0.5532 0.073 Uiso 1 1 calc R . . H23C H 0.0504 0.4708 0.5512 0.073 Uiso 1 1 calc R . . C24 C 0.2177(9) 0.5279(7) 0.5969(2) 0.052(3) Uani 1 1 d U . . H24A H 0.1800 0.5725 0.5818 0.063 Uiso 1 1 calc R . . H24B H 0.3003 0.5426 0.6018 0.063 Uiso 1 1 calc R . . H24C H 0.1792 0.5252 0.6189 0.063 Uiso 1 1 calc R . . C25 C 0.3005(8) 0.5115(6) 0.5117(2) 0.036(2) Uani 1 1 d U . . H25 H 0.3558 0.4936 0.4940 0.043 Uiso 1 1 calc R . . C26 C 0.1819(8) 0.5202(7) 0.4915(2) 0.053(3) Uani 1 1 d U . . H26A H 0.1266 0.5481 0.5063 0.064 Uiso 1 1 calc R . . H26B H 0.1529 0.4623 0.4845 0.064 Uiso 1 1 calc R . . H26C H 0.1901 0.5558 0.4706 0.064 Uiso 1 1 calc R . . C27 C 0.3423(8) 0.6020(6) 0.5244(2) 0.043(2) Uani 1 1 d U . . H27A H 0.3559 0.6387 0.5042 0.051 Uiso 1 1 calc R . . H27B H 0.4152 0.5960 0.5391 0.051 Uiso 1 1 calc R . . H27C H 0.2826 0.6288 0.5380 0.051 Uiso 1 1 calc R . . P4 P 0.80472(18) 0.13639(15) 0.60572(6) 0.0322(5) Uani 1 1 d D . . C28 C 0.9571(12) 0.1473(11) 0.5934(5) 0.051(5) Uani 0.592(8) 1 d PDU A 1 H28 H 0.9605 0.2082 0.5843 0.076 Uiso 0.592(8) 1 calc PR A 1 C29 C 0.9694(18) 0.0870(13) 0.5586(5) 0.057(6) Uiso 0.592(8) 1 d PDU A 1 H29A H 1.0396 0.1041 0.5472 0.086 Uiso 0.592(8) 1 calc PR A 1 H29B H 0.9005 0.0951 0.5424 0.086 Uiso 0.592(8) 1 calc PR A 1 H29C H 0.9755 0.0256 0.5655 0.086 Uiso 0.592(8) 1 calc PR A 1 C30 C 1.0410(18) 0.1488(16) 0.6258(5) 0.093(7) Uiso 0.592(8) 1 d PDU A 1 H30A H 1.0598 0.0890 0.6330 0.139 Uiso 0.592(8) 1 calc PR A 1 H30B H 1.0045 0.1792 0.6447 0.139 Uiso 0.592(8) 1 calc PR A 1 H30C H 1.1127 0.1793 0.6205 0.139 Uiso 0.592(8) 1 calc PR A 1 C31 C 0.7146(12) 0.1423(10) 0.5631(3) 0.042(4) Uani 0.592(8) 1 d PDU A 1 H31 H 0.7347 0.0896 0.5494 0.063 Uiso 0.592(8) 1 calc PR A 1 C32 C 0.5897(15) 0.1400(17) 0.5659(6) 0.049(6) Uiso 0.592(8) 1 d PDU A 1 H32A H 0.5641 0.1949 0.5759 0.074 Uiso 0.592(8) 1 calc PR A 1 H32B H 0.5699 0.0916 0.5810 0.074 Uiso 0.592(8) 1 calc PR A 1 H32C H 0.5503 0.1320 0.5426 0.074 Uiso 0.592(8) 1 calc PR A 1 C33 C 0.7476(17) 0.2221(13) 0.5413(5) 0.072(6) Uiso 0.592(8) 1 d PDU A 1 H33A H 0.6890 0.2302 0.5218 0.108 Uiso 0.592(8) 1 calc PR A 1 H33B H 0.8243 0.2126 0.5322 0.108 Uiso 0.592(8) 1 calc PR A 1 H33C H 0.7504 0.2742 0.5561 0.108 Uiso 0.592(8) 1 calc PR A 1 C34 C 0.7661(12) 0.0336(9) 0.6244(4) 0.040(4) Uani 0.592(8) 1 d PDU A 1 H34 H 0.6826 0.0385 0.6300 0.060 Uiso 0.592(8) 1 calc PR A 1 C35 C 0.837(2) 0.0163(16) 0.6591(5) 0.064(8) Uiso 0.592(8) 1 d PDU A 1 H35A H 0.7990 -0.0299 0.6718 0.096 Uiso 0.592(8) 1 calc PR A 1 H35B H 0.8405 0.0696 0.6731 0.096 Uiso 0.592(8) 1 calc PR A 1 H35C H 0.9161 -0.0019 0.6544 0.096 Uiso 0.592(8) 1 calc PR A 1 C36 C 0.7738(14) -0.0448(10) 0.6008(4) 0.048(4) Uiso 0.592(8) 1 d PDU A 1 H36A H 0.8554 -0.0631 0.6004 0.072 Uiso 0.592(8) 1 calc PR A 1 H36B H 0.7434 -0.0295 0.5771 0.072 Uiso 0.592(8) 1 calc PR A 1 H36C H 0.7274 -0.0925 0.6097 0.072 Uiso 0.592(8) 1 calc PR A 1 C28' C 0.907(2) 0.1619(15) 0.5726(6) 0.062(8) Uiso 0.408(8) 1 d PDU A 2 H28A H 0.9592 0.2019 0.5873 0.093 Uiso 0.408(8) 1 calc PR A 2 C29' C 0.848(2) 0.2344(15) 0.5469(6) 0.056(7) Uiso 0.408(8) 1 d PDU A 2 H29D H 0.9065 0.2573 0.5318 0.084 Uiso 0.408(8) 1 calc PR A 2 H29E H 0.8181 0.2820 0.5607 0.084 Uiso 0.408(8) 1 calc PR A 2 H29F H 0.7837 0.2082 0.5324 0.084 Uiso 0.408(8) 1 calc PR A 2 C30' C 0.997(2) 0.0895(15) 0.5684(7) 0.038(6) Uiso 0.408(8) 1 d PDU A 2 H30D H 0.9858 0.0648 0.5449 0.057 Uiso 0.408(8) 1 calc PR A 2 H30E H 0.9863 0.0438 0.5857 0.057 Uiso 0.408(8) 1 calc PR A 2 H30F H 1.0760 0.1135 0.5720 0.057 Uiso 0.408(8) 1 calc PR A 2 C31' C 0.6802(14) 0.0691(12) 0.5906(5) 0.040(5) Uiso 0.408(8) 1 d PDU A 2 H31A H 0.6408 0.0560 0.6124 0.059 Uiso 0.408(8) 1 calc PR A 2 C32' C 0.706(2) -0.0171(13) 0.5768(6) 0.049(6) Uiso 0.408(8) 1 d PDU A 2 H32D H 0.7096 -0.0136 0.5514 0.074 Uiso 0.408(8) 1 calc PR A 2 H32E H 0.6449 -0.0581 0.5825 0.074 Uiso 0.408(8) 1 calc PR A 2 H32F H 0.7817 -0.0372 0.5874 0.074 Uiso 0.408(8) 1 calc PR A 2 C33' C 0.586(3) 0.118(2) 0.5678(10) 0.072(13) Uiso 0.408(8) 1 d PDU A 2 H33D H 0.6195 0.1370 0.5462 0.109 Uiso 0.408(8) 1 calc PR A 2 H33E H 0.5596 0.1682 0.5805 0.109 Uiso 0.408(8) 1 calc PR A 2 H33F H 0.5204 0.0786 0.5620 0.109 Uiso 0.408(8) 1 calc PR A 2 C34' C 0.8890(14) 0.0582(12) 0.6361(4) 0.030(5) Uiso 0.408(8) 1 d PDU A 2 H34A H 0.9104 0.0066 0.6220 0.045 Uiso 0.408(8) 1 calc PR A 2 C35' C 1.0026(16) 0.0993(15) 0.6516(6) 0.045(6) Uiso 0.408(8) 1 d PDU A 2 H35D H 0.9851 0.1395 0.6704 0.068 Uiso 0.408(8) 1 calc PR A 2 H35E H 1.0403 0.1312 0.6334 0.068 Uiso 0.408(8) 1 calc PR A 2 H35F H 1.0552 0.0534 0.6611 0.068 Uiso 0.408(8) 1 calc PR A 2 C36' C 0.819(2) 0.0255(18) 0.6654(6) 0.030(7) Uiso 0.408(8) 1 d PDU A 2 H36D H 0.8620 -0.0210 0.6781 0.045 Uiso 0.408(8) 1 calc PR A 2 H36E H 0.7436 0.0029 0.6556 0.045 Uiso 0.408(8) 1 calc PR A 2 H36F H 0.8052 0.0735 0.6814 0.045 Uiso 0.408(8) 1 calc PR A 2 S1 S 0.44004(18) -0.02589(15) 0.65482(6) 0.0368(5) Uani 1 1 d U . . S2 S 0.51983(19) 0.04589(14) 0.71847(6) 0.0335(5) Uani 1 1 d U . . N1 N 0.5183(5) 0.0452(4) 0.67655(17) 0.0310(16) Uani 1 1 d U . . O1 O 0.4795(6) -0.0265(5) 0.62039(16) 0.068(2) Uani 1 1 d U . . O2 O 0.4389(6) -0.1080(4) 0.67226(19) 0.0565(19) Uani 1 1 d U . . O3 O 0.5819(6) 0.1241(4) 0.72914(16) 0.0495(17) Uani 1 1 d U . . O4 O 0.4058(5) 0.0360(4) 0.73138(16) 0.0476(16) Uani 1 1 d U . . C37 C 0.2970(7) 0.0138(6) 0.6521(3) 0.048(3) Uani 1 1 d U . . H37A H 0.2951 0.0713 0.6411 0.072 Uiso 1 1 calc R . . H37B H 0.2693 0.0184 0.6756 0.072 Uiso 1 1 calc R . . H37C H 0.2464 -0.0262 0.6381 0.072 Uiso 1 1 calc R . . C38 C 0.6037(8) -0.0428(6) 0.7342(2) 0.048(3) Uani 1 1 d U . . H38A H 0.6085 -0.0424 0.7598 0.071 Uiso 1 1 calc R . . H38B H 0.6825 -0.0384 0.7260 0.071 Uiso 1 1 calc R . . H38C H 0.5671 -0.0970 0.7257 0.071 Uiso 1 1 calc R . . S3 S -0.0075(2) 0.25603(16) 0.44617(6) 0.0468(6) Uani 1 1 d U . . S4 S -0.06296(18) 0.18267(16) 0.38146(6) 0.0373(5) Uani 1 1 d U . . N2 N 0.0153(6) 0.2460(5) 0.40610(19) 0.0424(19) Uani 1 1 d U . . O5 O 0.0594(8) 0.3289(5) 0.4590(2) 0.087(3) Uani 1 1 d U . . O6 O -0.1297(6) 0.2566(5) 0.45267(17) 0.063(2) Uani 1 1 d U . . O7 O -0.0122(6) 0.1793(5) 0.34848(17) 0.065(2) Uani 1 1 d U . . O8 O -0.0850(5) 0.1004(4) 0.39749(17) 0.0505(17) Uani 1 1 d U . . C39 C 0.0528(10) 0.1644(7) 0.4674(3) 0.061(3) Uani 1 1 d U . . H39A H 0.1372 0.1631 0.4650 0.091 Uiso 1 1 calc R . . H39B H 0.0170 0.1117 0.4570 0.091 Uiso 1 1 calc R . . H39C H 0.0380 0.1669 0.4923 0.091 Uiso 1 1 calc R . . C40 C -0.1993(7) 0.2335(6) 0.3736(2) 0.041(2) Uani 1 1 d U . . H40A H -0.1880 0.2926 0.3649 0.061 Uiso 1 1 calc R . . H40B H -0.2389 0.2362 0.3954 0.061 Uiso 1 1 calc R . . H40C H -0.2471 0.2000 0.3563 0.061 Uiso 1 1 calc R . . N99 N 0.720(2) -0.0241(16) 0.4909(6) 0.210(10) Uiso 1 1 d U . . C98 C 0.6591(15) 0.1009(12) 0.4519(4) 0.129(7) Uani 1 1 d U . . H98A H 0.5794 0.1132 0.4582 0.194 Uiso 1 1 calc R . . H98B H 0.6579 0.0865 0.4270 0.194 Uiso 1 1 calc R . . H98C H 0.7083 0.1522 0.4567 0.194 Uiso 1 1 calc R . . C99 C 0.7046(19) 0.0300(15) 0.4718(5) 0.134(7) Uani 1 1 d U . . 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 Ag1 0.0391(4) 0.0416(4) 0.0301(3) 0.0020(3) -0.0024(3) -0.0097(3) Ag2 0.0324(3) 0.0343(4) 0.0373(4) 0.0010(3) 0.0059(3) -0.0002(3) Te1 0.0430(3) 0.0350(3) 0.0342(3) 0.0035(3) -0.0077(3) -0.0116(3) Te2 0.0271(3) 0.0305(3) 0.0255(3) -0.0028(2) 0.0002(2) -0.0020(2) Te3 0.0225(3) 0.0572(4) 0.0260(3) 0.0007(3) -0.0008(2) -0.0018(3) Te4 0.0282(3) 0.0277(3) 0.0488(4) -0.0025(3) 0.0058(2) -0.0004(2) P1 0.0222(10) 0.0260(12) 0.0341(12) -0.0024(9) -0.0018(9) 0.0013(9) P2 0.0320(11) 0.0225(11) 0.0260(11) -0.0008(9) 0.0035(9) 0.0033(9) P3 0.0242(11) 0.0355(13) 0.0228(11) -0.0006(9) -0.0011(8) 0.0020(10) C1 0.031(5) 0.038(5) 0.049(5) -0.007(4) -0.002(4) 0.004(4) C2 0.082(8) 0.063(7) 0.055(7) -0.026(5) 0.012(5) -0.010(6) C3 0.042(5) 0.033(5) 0.065(6) -0.012(4) -0.008(5) 0.001(4) C4 0.034(5) 0.032(5) 0.053(6) -0.012(4) -0.012(4) -0.001(4) C5 0.086(8) 0.038(6) 0.074(7) -0.001(5) -0.025(6) -0.004(6) C6 0.028(5) 0.058(7) 0.089(8) -0.015(6) -0.014(4) 0.012(5) C7 0.033(5) 0.029(5) 0.053(5) 0.011(4) 0.010(4) 0.004(4) C8 0.058(6) 0.053(6) 0.052(6) 0.000(5) 0.029(5) 0.005(5) C9 0.025(5) 0.063(7) 0.081(7) 0.015(6) 0.008(4) 0.004(5) C10 0.054(6) 0.023(5) 0.036(5) 0.005(4) 0.009(4) -0.002(4) C11 0.084(8) 0.048(6) 0.039(5) 0.006(5) 0.021(5) -0.006(6) C12 0.058(6) 0.035(6) 0.066(6) 0.005(5) 0.011(5) -0.008(5) C13 0.040(5) 0.028(5) 0.040(5) -0.007(4) 0.005(4) 0.011(4) C14 0.024(5) 0.062(7) 0.100(9) -0.017(6) 0.002(5) 0.018(4) C15 0.062(6) 0.041(5) 0.039(5) 0.009(4) 0.003(5) 0.011(4) C16 0.036(4) 0.023(4) 0.030(4) 0.001(3) 0.001(4) -0.003(4) C17 0.040(5) 0.042(6) 0.043(5) -0.001(4) -0.015(4) 0.003(4) C18 0.072(7) 0.031(5) 0.035(5) -0.009(4) -0.011(5) 0.003(5) C19 0.029(5) 0.037(5) 0.042(5) -0.002(4) -0.009(4) -0.001(4) C20 0.056(6) 0.039(6) 0.065(6) 0.002(5) -0.006(5) -0.007(5) C21 0.050(6) 0.050(6) 0.058(6) -0.018(5) 0.004(5) -0.009(5) C22 0.024(4) 0.058(6) 0.030(5) -0.001(4) 0.003(3) 0.007(4) C23 0.030(5) 0.088(8) 0.067(7) -0.007(6) 0.009(5) 0.005(5) C24 0.060(6) 0.067(7) 0.033(5) -0.008(5) 0.015(5) 0.013(5) C25 0.049(5) 0.036(5) 0.021(4) 0.006(4) -0.002(4) 0.000(4) C26 0.056(6) 0.054(7) 0.048(6) 0.013(5) -0.014(5) -0.004(5) C27 0.047(5) 0.045(5) 0.037(5) 0.004(4) 0.007(4) -0.005(4) P4 0.0260(11) 0.0317(13) 0.0396(13) -0.0019(10) 0.0068(10) 0.0014(10) C28 0.041(9) 0.046(10) 0.069(11) -0.012(9) 0.031(9) -0.001(8) C31 0.052(9) 0.039(9) 0.035(8) -0.010(7) -0.001(7) 0.027(8) C34 0.027(7) 0.043(9) 0.050(9) 0.003(7) 0.001(7) 0.003(7) S1 0.0291(11) 0.0381(13) 0.0430(13) -0.0081(11) -0.0002(10) -0.0037(10) S2 0.0372(12) 0.0286(12) 0.0347(12) 0.0000(9) 0.0018(9) 0.0023(10) N1 0.026(4) 0.031(4) 0.035(4) 0.001(3) 0.000(3) -0.003(3) O1 0.050(4) 0.113(7) 0.040(4) -0.031(4) 0.010(3) -0.026(4) O2 0.054(4) 0.028(4) 0.084(5) -0.001(3) -0.024(4) -0.002(3) O3 0.068(4) 0.036(4) 0.043(4) -0.009(3) -0.012(3) -0.003(3) O4 0.047(4) 0.049(4) 0.049(4) 0.003(3) 0.017(3) 0.006(3) C37 0.030(5) 0.035(5) 0.076(7) -0.004(5) -0.009(5) 0.000(4) C38 0.042(6) 0.055(6) 0.044(6) -0.002(5) -0.012(4) 0.016(5) S3 0.0599(16) 0.0389(14) 0.0393(13) -0.0031(11) -0.0139(12) -0.0017(12) S4 0.0290(11) 0.0450(14) 0.0372(12) -0.0091(11) -0.0028(9) 0.0000(10) N2 0.032(4) 0.047(5) 0.047(4) 0.008(4) -0.008(3) -0.012(4) O5 0.125(7) 0.052(5) 0.074(5) -0.004(4) -0.055(5) -0.024(5) O6 0.059(5) 0.077(5) 0.053(4) -0.018(4) 0.008(3) 0.024(4) O7 0.050(4) 0.104(6) 0.044(4) -0.023(4) 0.008(3) 0.009(4) O8 0.047(4) 0.037(4) 0.065(4) -0.003(3) -0.014(3) -0.002(3) C39 0.076(8) 0.062(7) 0.043(6) 0.000(5) -0.012(5) 0.005(6) C40 0.030(5) 0.053(6) 0.038(5) -0.005(5) -0.010(4) 0.009(4) C98 0.135(15) 0.170(18) 0.080(11) -0.002(11) -0.015(10) -0.064(13) C99 0.186(19) 0.136(16) 0.078(12) -0.047(10) -0.002(12) -0.019(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 Ag1 Te3 2.7182(8) . ? Ag1 Te1 2.7280(9) . ? Ag1 Te2 2.7638(9) . ? Ag2 N1 2.422(7) . ? Ag2 Te4 2.6957(9) . ? Ag2 O3 2.772(6) . ? Ag2 Te2 2.7947(9) . ? Te1 P1 2.400(2) . ? Te2 P2 2.421(2) . ? Te3 P3 2.404(2) . ? Te4 P4 2.410(2) . ? P1 C7 1.816(8) . ? P1 C4 1.836(8) . ? P1 C1 1.836(9) . ? P2 C10 1.823(8) . ? P2 C16 1.828(8) . ? P2 C13 1.831(8) . ? P3 C25 1.816(8) . ? P3 C22 1.843(8) . ? P3 C19 1.846(9) . ? C1 C3 1.514(12) . ? C1 C2 1.517(13) . ? C4 C5 1.520(13) . ? C4 C6 1.531(12) . ? C7 C8 1.522(12) . ? C7 C9 1.535(12) . ? C10 C12 1.509(12) . ? C10 C11 1.526(11) . ? C13 C14 1.520(12) . ? C13 C15 1.526(12) . ? C16 C17 1.524(11) . ? C16 C18 1.535(11) . ? C19 C21 1.522(12) . ? C19 C20 1.530(12) . ? C22 C24 1.491(13) . ? C22 C23 1.542(11) . ? C25 C26 1.525(11) . ? C25 C27 1.539(12) . ? P4 C34 1.802(13) . ? P4 C31' 1.826(15) . ? P4 C28' 1.833(17) . ? P4 C28 1.851(13) . ? P4 C31 1.876(13) . ? P4 C34' 1.893(15) . ? C28 C30 1.52(2) . ? C28 C29 1.64(2) . ? C31 C32 1.45(2) . ? C31 C33 1.55(2) . ? C34 C36 1.512(18) . ? C34 C35 1.53(2) . ? C28' C30' 1.53(3) . ? C28' C29' 1.61(2) . ? C31' C32' 1.46(2) . ? C31' C33' 1.53(2) . ? C34' C36' 1.51(2) . ? C34' C35' 1.53(2) . ? S1 O1 1.426(6) . ? S1 O2 1.428(7) . ? S1 N1 1.610(7) . ? S1 C37 1.748(8) . ? S2 O4 1.439(6) . ? S2 O3 1.442(6) . ? S2 N1 1.608(7) . ? S2 C38 1.751(9) . ? S3 O5 1.426(7) . ? S3 O6 1.442(7) . ? S3 N2 1.585(8) . ? S3 C39 1.746(10) . ? S4 O7 1.430(7) . ? S4 O8 1.436(7) . ? S4 N2 1.590(7) . ? S4 C40 1.755(8) . ? N99 C99 1.11(3) . ? C98 C99 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 Te3 Ag1 Te1 122.20(3) . . ? Te3 Ag1 Te2 114.65(3) . . ? Te1 Ag1 Te2 122.47(3) . . ? N1 Ag2 Te4 127.57(16) . . ? N1 Ag2 O3 55.1(2) . . ? Te4 Ag2 O3 114.61(14) . . ? N1 Ag2 Te2 105.53(15) . . ? Te4 Ag2 Te2 125.27(3) . . ? O3 Ag2 Te2 105.36(14) . . ? P1 Te1 Ag1 105.61(5) . . ? P2 Te2 Ag1 105.77(6) . . ? P2 Te2 Ag2 106.99(5) . . ? Ag1 Te2 Ag2 68.88(3) . . ? P3 Te3 Ag1 110.08(6) . . ? P4 Te4 Ag2 95.84(6) . . ? C7 P1 C4 106.8(4) . . ? C7 P1 C1 106.6(4) . . ? C4 P1 C1 112.9(4) . . ? C7 P1 Te1 111.3(3) . . ? C4 P1 Te1 110.2(3) . . ? C1 P1 Te1 109.0(3) . . ? C10 P2 C16 109.3(4) . . ? C10 P2 C13 112.3(4) . . ? C16 P2 C13 107.0(4) . . ? C10 P2 Te2 110.2(3) . . ? C16 P2 Te2 111.3(3) . . ? C13 P2 Te2 106.6(3) . . ? C25 P3 C22 113.4(4) . . ? C25 P3 C19 106.9(4) . . ? C22 P3 C19 106.8(4) . . ? C25 P3 Te3 107.7(3) . . ? C22 P3 Te3 111.8(3) . . ? C19 P3 Te3 110.2(3) . . ? C3 C1 C2 111.3(8) . . ? C3 C1 P1 112.6(6) . . ? C2 C1 P1 115.2(7) . . ? C5 C4 C6 111.0(8) . . ? C5 C4 P1 115.6(7) . . ? C6 C4 P1 112.0(7) . . ? C8 C7 C9 111.2(8) . . ? C8 C7 P1 110.7(6) . . ? C9 C7 P1 112.1(6) . . ? C12 C10 C11 112.2(8) . . ? C12 C10 P2 113.5(6) . . ? C11 C10 P2 113.4(6) . . ? C14 C13 C15 111.0(8) . . ? C14 C13 P2 113.5(6) . . ? C15 C13 P2 110.8(6) . . ? C17 C16 C18 110.8(7) . . ? C17 C16 P2 112.6(6) . . ? C18 C16 P2 115.0(6) . . ? C21 C19 C20 109.6(8) . . ? C21 C19 P3 111.9(6) . . ? C20 C19 P3 110.8(6) . . ? C24 C22 C23 110.4(8) . . ? C24 C22 P3 113.6(6) . . ? C23 C22 P3 113.5(6) . . ? C26 C25 C27 109.3(8) . . ? C26 C25 P3 115.9(6) . . ? C27 C25 P3 114.6(6) . . ? C34 P4 C31' 54.7(7) . . ? C34 P4 C28' 130.6(9) . . ? C31' P4 C28' 115.3(11) . . ? C34 P4 C28 116.3(7) . . ? C31' P4 C28 134.7(8) . . ? C28' P4 C28 30.7(7) . . ? C34 P4 C31 104.7(7) . . ? C31' P4 C31 51.5(7) . . ? C28' P4 C31 74.2(10) . . ? C28 P4 C31 104.3(7) . . ? C34 P4 C34' 47.8(6) . . ? C31' P4 C34' 101.1(8) . . ? C28' P4 C34' 103.7(9) . . ? C28 P4 C34' 76.3(8) . . ? C31 P4 C34' 142.7(7) . . ? C34 P4 Te4 114.2(5) . . ? C31' P4 Te4 115.3(6) . . ? C28' P4 Te4 112.7(8) . . ? C28 P4 Te4 108.4(5) . . ? C31 P4 Te4 108.0(4) . . ? C34' P4 Te4 107.0(6) . . ? C30 C28 C29 126.1(15) . . ? C30 C28 P4 110.5(13) . . ? C29 C28 P4 107.0(11) . . ? C32 C31 C33 109.9(14) . . ? C32 C31 P4 115.1(12) . . ? C33 C31 P4 111.7(11) . . ? C36 C34 C35 109.4(14) . . ? C36 C34 P4 115.7(10) . . ? C35 C34 P4 111.6(12) . . ? C30' C28' C29' 134.2(18) . . ? C30' C28' P4 112.7(14) . . ? C29' C28' P4 108.0(15) . . ? C32' C31' C33' 112.8(19) . . ? C32' C31' P4 116.9(14) . . ? C33' C31' P4 114.1(17) . . ? C36' C34' C35' 109.3(15) . . ? C36' C34' P4 113.1(13) . . ? C35' C34' P4 111.3(13) . . ? O1 S1 O2 116.3(5) . . ? O1 S1 N1 106.4(4) . . ? O2 S1 N1 112.3(4) . . ? O1 S1 C37 107.7(5) . . ? O2 S1 C37 107.3(4) . . ? N1 S1 C37 106.4(4) . . ? O4 S2 O3 115.7(4) . . ? O4 S2 N1 113.3(4) . . ? O3 S2 N1 105.1(4) . . ? O4 S2 C38 106.9(4) . . ? O3 S2 C38 107.5(4) . . ? N1 S2 C38 108.0(4) . . ? S2 N1 S1 119.3(4) . . ? S2 N1 Ag2 103.0(3) . . ? S1 N1 Ag2 130.0(4) . . ? S2 O3 Ag2 93.2(3) . . ? O5 S3 O6 116.3(5) . . ? O5 S3 N2 106.9(5) . . ? O6 S3 N2 113.3(4) . . ? O5 S3 C39 106.6(5) . . ? O6 S3 C39 106.4(5) . . ? N2 S3 C39 106.8(5) . . ? O7 S4 O8 116.2(5) . . ? O7 S4 N2 107.5(4) . . ? O8 S4 N2 113.1(4) . . ? O7 S4 C40 106.1(4) . . ? O8 S4 C40 106.4(4) . . ? N2 S4 C40 106.8(4) . . ? S3 N2 S4 120.8(5) . . ? N99 C99 C98 165(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 Te3 Ag1 Te1 P1 26.94(7) . . . . ? Te2 Ag1 Te1 P1 -143.12(6) . . . . ? Te3 Ag1 Te2 P2 -149.31(6) . . . . ? Te1 Ag1 Te2 P2 21.44(7) . . . . ? Te3 Ag1 Te2 Ag2 108.18(3) . . . . ? Te1 Ag1 Te2 Ag2 -81.06(4) . . . . ? N1 Ag2 Te2 P2 85.42(17) . . . . ? Te4 Ag2 Te2 P2 -108.26(6) . . . . ? O3 Ag2 Te2 P2 28.06(14) . . . . ? N1 Ag2 Te2 Ag1 -173.82(16) . . . . ? Te4 Ag2 Te2 Ag1 -7.50(3) . . . . ? O3 Ag2 Te2 Ag1 128.82(13) . . . . ? Te1 Ag1 Te3 P3 -137.43(7) . . . . ? Te2 Ag1 Te3 P3 33.36(7) . . . . ? N1 Ag2 Te4 P4 34.8(2) . . . . ? O3 Ag2 Te4 P4 98.58(15) . . . . ? Te2 Ag2 Te4 P4 -128.52(6) . . . . ? Ag1 Te1 P1 C7 -91.4(3) . . . . ? Ag1 Te1 P1 C4 26.9(3) . . . . ? Ag1 Te1 P1 C1 151.3(3) . . . . ? Ag1 Te2 P2 C10 -143.4(3) . . . . ? Ag2 Te2 P2 C10 -71.2(3) . . . . ? Ag1 Te2 P2 C16 -21.9(3) . . . . ? Ag2 Te2 P2 C16 50.3(3) . . . . ? Ag1 Te2 P2 C13 94.5(3) . . . . ? Ag2 Te2 P2 C13 166.7(3) . . . . ? Ag1 Te3 P3 C25 143.9(3) . . . . ? Ag1 Te3 P3 C22 18.7(3) . . . . ? Ag1 Te3 P3 C19 -99.9(3) . . . . ? C7 P1 C1 C3 61.8(7) . . . . ? C4 P1 C1 C3 -55.2(8) . . . . ? Te1 P1 C1 C3 -177.9(5) . . . . ? C7 P1 C1 C2 -169.0(7) . . . . ? C4 P1 C1 C2 74.0(8) . . . . ? Te1 P1 C1 C2 -48.8(8) . . . . ? C7 P1 C4 C5 -44.2(8) . . . . ? C1 P1 C4 C5 72.6(8) . . . . ? Te1 P1 C4 C5 -165.3(6) . . . . ? C7 P1 C4 C6 -172.7(7) . . . . ? C1 P1 C4 C6 -55.9(8) . . . . ? Te1 P1 C4 C6 66.2(7) . . . . ? C4 P1 C7 C8 -58.7(7) . . . . ? C1 P1 C7 C8 -179.6(6) . . . . ? Te1 P1 C7 C8 61.6(7) . . . . ? C4 P1 C7 C9 176.5(7) . . . . ? C1 P1 C7 C9 55.6(8) . . . . ? Te1 P1 C7 C9 -63.2(7) . . . . ? C16 P2 C10 C12 -175.5(6) . . . . ? C13 P2 C10 C12 65.8(7) . . . . ? Te2 P2 C10 C12 -52.9(7) . . . . ? C16 P2 C10 C11 54.8(8) . . . . ? C13 P2 C10 C11 -63.9(8) . . . . ? Te2 P2 C10 C11 177.4(6) . . . . ? C10 P2 C13 C14 -65.5(8) . . . . ? C16 P2 C13 C14 174.5(7) . . . . ? Te2 P2 C13 C14 55.3(7) . . . . ? C10 P2 C13 C15 168.8(6) . . . . ? C16 P2 C13 C15 48.8(7) . . . . ? Te2 P2 C13 C15 -70.4(6) . . . . ? C10 P2 C16 C17 53.7(7) . . . . ? C13 P2 C16 C17 175.6(6) . . . . ? Te2 P2 C16 C17 -68.3(6) . . . . ? C10 P2 C16 C18 -74.6(7) . . . . ? C13 P2 C16 C18 47.3(7) . . . . ? Te2 P2 C16 C18 163.5(5) . . . . ? C25 P3 C19 C21 58.7(7) . . . . ? C22 P3 C19 C21 -179.6(6) . . . . ? Te3 P3 C19 C21 -58.1(7) . . . . ? C25 P3 C19 C20 -178.7(6) . . . . ? C22 P3 C19 C20 -57.0(7) . . . . ? Te3 P3 C19 C20 64.6(7) . . . . ? C25 P3 C22 C24 -56.0(7) . . . . ? C19 P3 C22 C24 -173.4(6) . . . . ? Te3 P3 C22 C24 66.0(7) . . . . ? C25 P3 C22 C23 71.3(8) . . . . ? C19 P3 C22 C23 -46.2(8) . . . . ? Te3 P3 C22 C23 -166.8(6) . . . . ? C22 P3 C25 C26 -59.5(8) . . . . ? C19 P3 C25 C26 58.0(8) . . . . ? Te3 P3 C25 C26 176.4(6) . . . . ? C22 P3 C25 C27 69.3(8) . . . . ? C19 P3 C25 C27 -173.3(6) . . . . ? Te3 P3 C25 C27 -54.9(7) . . . . ? Ag2 Te4 P4 C34 -35.8(5) . . . . ? Ag2 Te4 P4 C31' 25.0(7) . . . . ? Ag2 Te4 P4 C28' 160.2(9) . . . . ? Ag2 Te4 P4 C28 -167.3(6) . . . . ? Ag2 Te4 P4 C31 80.2(5) . . . . ? Ag2 Te4 P4 C34' -86.5(5) . . . . ? C34 P4 C28 C30 -68.4(15) . . . . ? C31' P4 C28 C30 -133.8(15) . . . . ? C28' P4 C28 C30 166(3) . . . . ? C31 P4 C28 C30 176.8(13) . . . . ? C34' P4 C28 C30 -41.7(14) . . . . ? Te4 P4 C28 C30 61.9(14) . . . . ? C34 P4 C28 C29 72.1(14) . . . . ? C31' P4 C28 C29 6.8(19) . . . . ? C28' P4 C28 C29 -54(2) . . . . ? C31 P4 C28 C29 -42.6(13) . . . . ? C34' P4 C28 C29 98.9(13) . . . . ? Te4 P4 C28 C29 -157.5(11) . . . . ? C34 P4 C31 C32 60.6(16) . . . . ? C31' P4 C31 C32 46.9(16) . . . . ? C28' P4 C31 C32 -170.8(17) . . . . ? C28 P4 C31 C32 -176.7(15) . . . . ? C34' P4 C31 C32 97.2(17) . . . . ? Te4 P4 C31 C32 -61.5(15) . . . . ? C34 P4 C31 C33 -173.3(11) . . . . ? C31' P4 C31 C33 173.1(16) . . . . ? C28' P4 C31 C33 -44.6(13) . . . . ? C28 P4 C31 C33 -50.6(12) . . . . ? C34' P4 C31 C33 -136.6(13) . . . . ? Te4 P4 C31 C33 64.7(11) . . . . ? C31' P4 C34 C36 64.7(12) . . . . ? C28' P4 C34 C36 -30.1(18) . . . . ? C28 P4 C34 C36 -63.0(13) . . . . ? C31 P4 C34 C36 51.6(12) . . . . ? C34' P4 C34 C36 -99.2(14) . . . . ? Te4 P4 C34 C36 169.4(9) . . . . ? C31' P4 C34 C35 -169.4(17) . . . . ? C28' P4 C34 C35 95.8(17) . . . . ? C28 P4 C34 C35 62.9(15) . . . . ? C31 P4 C34 C35 177.5(13) . . . . ? C34' P4 C34 C35 26.7(13) . . . . ? Te4 P4 C34 C35 -64.7(13) . . . . ? C34 P4 C28' C30' -19(3) . . . . ? C31' P4 C28' C30' -84(2) . . . . ? C28 P4 C28' C30' 53.2(19) . . . . ? C31 P4 C28' C30' -115(2) . . . . ? C34' P4 C28' C30' 26(2) . . . . ? Te4 P4 C28' C30' 141.3(17) . . . . ? C34 P4 C28' C29' 139.0(14) . . . . ? C31' P4 C28' C29' 74.9(18) . . . . ? C28 P4 C28' C29' -148(3) . . . . ? C31 P4 C28' C29' 43.0(16) . . . . ? C34' P4 C28' C29' -175.6(16) . . . . ? Te4 P4 C28' C29' -60.3(18) . . . . ? C34 P4 C31' C32' -63.4(16) . . . . ? C28' P4 C31' C32' 59.7(19) . . . . ? C28 P4 C31' C32' 30(2) . . . . ? C31 P4 C31' C32' 100.3(18) . . . . ? C34' P4 C31' C32' -51.3(17) . . . . ? Te4 P4 C31' C32' -166.2(14) . . . . ? C34 P4 C31' C33' 162(2) . . . . ? C28' P4 C31' C33' -75(2) . . . . ? C28 P4 C31' C33' -104(2) . . . . ? C31 P4 C31' C33' -34.3(19) . . . . ? C34' P4 C31' C33' 174(2) . . . . ? Te4 P4 C31' C33' 59(2) . . . . ? C34 P4 C34' C36' -45.1(15) . . . . ? C31' P4 C34' C36' -58.5(16) . . . . ? C28' P4 C34' C36' -178.2(17) . . . . ? C28 P4 C34' C36' 167.9(16) . . . . ? C31 P4 C34' C36' -96.3(18) . . . . ? Te4 P4 C34' C36' 62.5(15) . . . . ? C34 P4 C34' C35' -168.6(18) . . . . ? C31' P4 C34' C35' 178.0(14) . . . . ? C28' P4 C34' C35' 58.3(16) . . . . ? C28 P4 C34' C35' 44.4(13) . . . . ? C31 P4 C34' C35' 140.1(13) . . . . ? Te4 P4 C34' C35' -61.0(14) . . . . ? O4 S2 N1 S1 -44.0(6) . . . . ? O3 S2 N1 S1 -171.3(4) . . . . ? C38 S2 N1 S1 74.1(6) . . . . ? O4 S2 N1 Ag2 108.3(4) . . . . ? O3 S2 N1 Ag2 -18.9(4) . . . . ? C38 S2 N1 Ag2 -133.5(4) . . . . ? O1 S1 N1 S2 -164.6(5) . . . . ? O2 S1 N1 S2 -36.4(6) . . . . ? C37 S1 N1 S2 80.7(6) . . . . ? O1 S1 N1 Ag2 51.5(6) . . . . ? O2 S1 N1 Ag2 179.7(4) . . . . ? C37 S1 N1 Ag2 -63.2(6) . . . . ? Te4 Ag2 N1 S2 107.4(3) . . . . ? O3 Ag2 N1 S2 11.5(2) . . . . ? Te2 Ag2 N1 S2 -86.7(3) . . . . ? Te4 Ag2 N1 S1 -104.4(4) . . . . ? O3 Ag2 N1 S1 159.7(6) . . . . ? Te2 Ag2 N1 S1 61.5(5) . . . . ? O4 S2 O3 Ag2 -109.8(3) . . . . ? N1 S2 O3 Ag2 16.1(3) . . . . ? C38 S2 O3 Ag2 130.9(4) . . . . ? N1 Ag2 O3 S2 -12.5(3) . . . . ? Te4 Ag2 O3 S2 -132.4(3) . . . . ? Te2 Ag2 O3 S2 86.0(3) . . . . ? O5 S3 N2 S4 -168.4(5) . . . . ? O6 S3 N2 S4 -39.1(7) . . . . ? C39 S3 N2 S4 77.8(6) . . . . ? O7 S4 N2 S3 -172.7(5) . . . . ? O8 S4 N2 S3 -43.1(7) . . . . ? C40 S4 N2 S3 73.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17B O3 0.98 2.63 3.171(11) 114.7 . C10 H10 O4 1.00 2.54 3.363(11) 139.7 . C13 H13 O4 1.00 2.40 3.207(10) 136.8 2_556 C19 H19 O5 1.00 2.46 3.353(11) 148.6 . C3 H3B O7 0.98 2.58 3.434(12) 145.4 3_666 C18 H18A O7 0.98 2.61 3.522(11) 155.6 4_666 C37 H37C O8 0.98 2.50 3.460(11) 167.0 3_556 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.749 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.153 #============================================================================= # cif data for "defender" #============================================================================= data_illimun _database_code_depnum_ccdc_archive 'CCDC 611443' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cl4 Te' _chemical_formula_weight 447.62 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.078(2) _cell_length_b 8.1839(6) _cell_length_c 9.0746(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1565.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.565 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.5958 _exptl_absorpt_correction_T_max 0.9776 _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 \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 247 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.82 _diffrn_reflns_number 13864 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3585 _reflns_number_gt 3466 _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^)+(0.0264P)^2^+0.5110P] 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 SHELXL _refine_ls_extinction_coef 0.0071(2) _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 -0.006(14) _refine_ls_number_reflns 3585 _refine_ls_number_parameters 173 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0438 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.032 _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 Te Te 0.386941(5) 0.927270(15) 0.69115(2) 0.02479(5) Uani 1 1 d . . . Cl1 Cl 0.38849(4) 0.87643(11) 0.95947(8) 0.03892(16) Uani 1 1 d . . . Cl2 Cl 0.49290(2) 0.85932(7) 0.68549(12) 0.03639(12) Uani 1 1 d . . . Cl3 Cl 0.38721(4) 0.94505(11) 0.41873(11) 0.0472(2) Uani 1 1 d . . . Cl4 Cl 0.24678(2) 0.86838(6) 0.68925(14) 0.03960(13) Uani 1 1 d . . . C1 C 0.34953(10) 0.6859(2) 0.6703(3) 0.0221(5) Uani 1 1 d U . . C2 C 0.28628(10) 0.6813(2) 0.6683(3) 0.0236(5) Uani 1 1 d U . . C3 C 0.39473(9) 0.5479(2) 0.6759(4) 0.0233(5) Uani 1 1 d U . . C4 C 0.43527(12) 0.5157(3) 0.5588(3) 0.0291(5) Uani 1 1 d U . . H4 H 0.4328 0.5797 0.4716 0.035 Uiso 1 1 calc R . . C5 C 0.47920(14) 0.3907(3) 0.5688(3) 0.0367(6) Uani 1 1 d U . . H5 H 0.5065 0.3680 0.4882 0.044 Uiso 1 1 calc R . . C6 C 0.48335(10) 0.2986(3) 0.6966(5) 0.0378(5) Uani 1 1 d U . . H6 H 0.5142 0.2144 0.7044 0.045 Uiso 1 1 calc R . . C7 C 0.44268(14) 0.3291(3) 0.8125(3) 0.0346(6) Uani 1 1 d U . . H7 H 0.4452 0.2644 0.8992 0.041 Uiso 1 1 calc R . . C8 C 0.39802(13) 0.4538(3) 0.8033(3) 0.0282(5) Uani 1 1 d U . . H8 H 0.3701 0.4745 0.8833 0.034 Uiso 1 1 calc R . . C9 C 0.24435(11) 0.5365(3) 0.6538(2) 0.0249(5) Uani 1 1 d U . . C10 C 0.26481(12) 0.4007(3) 0.5727(3) 0.0296(5) Uani 1 1 d U . . H10 H 0.3050 0.4026 0.5253 0.035 Uiso 1 1 calc R . . C11 C 0.22665(13) 0.2641(3) 0.5617(3) 0.0338(5) Uani 1 1 d U . . H11 H 0.2406 0.1725 0.5062 0.041 Uiso 1 1 calc R . . C12 C 0.16782(14) 0.2596(3) 0.6313(3) 0.0369(6) Uani 1 1 d U . . H12 H 0.1422 0.1643 0.6263 0.044 Uiso 1 1 calc R . . C13 C 0.14719(12) 0.3952(4) 0.7074(4) 0.0400(6) Uani 1 1 d U . . H13 H 0.1066 0.3936 0.7530 0.048 Uiso 1 1 calc R . . C14 C 0.18450(12) 0.5336(3) 0.7187(3) 0.0318(6) Uani 1 1 d U . . H14 H 0.1693 0.6266 0.7705 0.038 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 Te 0.02215(7) 0.01639(7) 0.03582(8) -0.00022(7) -0.00206(12) -0.00155(4) Cl1 0.0449(4) 0.0385(4) 0.0334(4) -0.0078(4) -0.0006(3) 0.0069(3) Cl2 0.0222(2) 0.0313(2) 0.0556(3) -0.0069(4) 0.0012(4) -0.00316(18) Cl3 0.0548(5) 0.0470(4) 0.0399(4) 0.0140(4) -0.0040(3) -0.0129(4) Cl4 0.0239(2) 0.0217(2) 0.0732(4) -0.0023(5) -0.0025(4) 0.00345(18) C1 0.0225(8) 0.0179(8) 0.0258(13) 0.0005(8) 0.0016(9) -0.0019(7) C2 0.0252(9) 0.0162(8) 0.0294(14) 0.0009(9) 0.0000(9) 0.0016(7) C3 0.0225(8) 0.0164(8) 0.0310(14) 0.0012(12) -0.0054(11) -0.0023(7) C4 0.0310(13) 0.0232(10) 0.0331(12) -0.0010(10) 0.0024(10) -0.0003(9) C5 0.0310(14) 0.0263(11) 0.0529(16) -0.0082(12) 0.0113(12) 0.0018(11) C6 0.0306(10) 0.0194(9) 0.0634(15) -0.0028(17) -0.010(2) 0.0050(8) C7 0.0392(14) 0.0212(11) 0.0433(14) 0.0050(10) -0.0147(11) -0.0015(11) C8 0.0308(12) 0.0226(11) 0.0311(11) 0.0005(9) -0.0024(10) -0.0029(10) C9 0.0274(10) 0.0215(9) 0.0259(12) 0.0030(7) -0.0020(8) -0.0032(8) C10 0.0279(12) 0.0253(10) 0.0355(13) 0.0020(10) -0.0011(9) -0.0029(9) C11 0.0407(14) 0.0228(10) 0.0380(13) -0.0007(10) -0.0066(11) -0.0052(10) C12 0.0428(15) 0.0296(12) 0.0383(12) 0.0051(10) -0.0078(11) -0.0151(11) C13 0.0331(11) 0.0481(13) 0.0387(17) -0.0004(15) 0.0029(14) -0.0200(10) C14 0.0299(11) 0.0325(11) 0.0328(16) -0.0046(10) 0.0028(9) -0.0069(9) _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 Te C1 2.1356(19) . ? Te Cl2 2.3021(5) . ? Te Cl1 2.4704(8) . ? Te Cl3 2.4764(10) . ? Cl4 C2 1.753(2) . ? C1 C2 1.334(3) . ? C1 C3 1.478(3) . ? C2 C9 1.484(3) . ? C3 C4 1.389(4) . ? C3 C8 1.391(4) . ? C4 C5 1.383(4) . ? C5 C6 1.386(5) . ? C6 C7 1.379(5) . ? C7 C8 1.391(4) . ? C9 C14 1.392(3) . ? C9 C10 1.401(3) . ? C10 C11 1.381(3) . ? C11 C12 1.392(4) . ? C12 C13 1.377(4) . ? C13 C14 1.383(3) . ? 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 Te Cl2 97.63(6) . . ? C1 Te Cl1 86.35(7) . . ? Cl2 Te Cl1 88.20(3) . . ? C1 Te Cl3 88.10(7) . . ? Cl2 Te Cl3 89.41(4) . . ? Cl1 Te Cl3 173.61(4) . . ? C2 C1 C3 128.56(19) . . ? C2 C1 Te 113.33(15) . . ? C3 C1 Te 117.75(13) . . ? C1 C2 C9 128.21(19) . . ? C1 C2 Cl4 116.68(16) . . ? C9 C2 Cl4 115.10(16) . . ? C4 C3 C8 120.0(2) . . ? C4 C3 C1 121.0(3) . . ? C8 C3 C1 118.9(3) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 120.0(3) . . ? C7 C6 C5 120.0(2) . . ? C6 C7 C8 120.5(3) . . ? C7 C8 C3 119.3(3) . . ? C14 C9 C10 119.2(2) . . ? C14 C9 C2 121.0(2) . . ? C10 C9 C2 119.8(2) . . ? C11 C10 C9 120.1(2) . . ? C10 C11 C12 120.5(2) . . ? C13 C12 C11 119.2(2) . . ? C12 C13 C14 121.2(3) . . ? C13 C14 C9 119.9(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.564 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.059 # end of cif file #============================================================================= data_gaina _database_code_depnum_ccdc_archive 'CCDC 636033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Bis-(triisopropylphosphine telluride)-silver(I) hexafluoroantimonate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H42 Ag F6 P2 Sb Te2' _chemical_formula_weight 919.28 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' 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 28.5566(15) _cell_length_b 8.4221(5) _cell_length_c 28.2425(15) _cell_angle_alpha 90.00 _cell_angle_beta 118.8840(10) _cell_angle_gamma 90.00 _cell_volume 5947.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9528 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 3.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6108 _exptl_absorpt_correction_T_max 0.6902 _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 'phi and omega 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 107897 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.81 _diffrn_reflns_theta_max 28.58 _reflns_number_total 15108 _reflns_number_gt 9708 _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^)+(0.0252P)^2^+41.2376P] 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 15108 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 -0.061510(16) 0.01208(5) 0.011790(17) 0.02318(9) Uani 1 1 d . . . Te2 Te 0.040433(15) 0.49969(5) 0.075038(15) 0.02124(9) Uani 1 1 d . . . Te3 Te 0.456658(15) 0.99957(5) 0.029886(17) 0.02160(9) Uani 1 1 d . . . Te4 Te 0.566149(16) 1.51336(5) 0.069340(15) 0.02172(9) Uani 1 1 d . . . Sb1 Sb 0.335931(18) 0.56221(6) 0.154950(19) 0.02821(11) Uani 1 1 d . . . Sb2 Sb -0.17798(2) 0.55378(6) 0.180001(18) 0.03018(11) Uani 1 1 d . . . Ag1 Ag 0.00638(2) 0.24818(6) -0.00234(2) 0.03463(13) Uani 1 1 d . . . Ag2 Ag 0.50538(2) 1.25818(6) 0.00918(2) 0.03293(13) Uani 1 1 d . . . P1 P -0.07810(6) -0.0068(2) 0.08844(6) 0.0211(3) Uani 1 1 d . . . P2 P 0.13212(6) 0.55664(19) 0.14130(6) 0.0167(3) Uani 1 1 d . . . P3 P 0.36764(6) 1.05969(19) 0.01504(6) 0.0152(3) Uani 1 1 d . . . P4 P 0.58306(6) 1.4991(2) 0.16207(6) 0.0172(3) Uani 1 1 d . . . C11 C -0.1124(3) -0.1939(8) 0.0852(3) 0.0285(16) Uani 1 1 d . . . H11 H -0.1227 -0.1909 0.1143 0.034 Uiso 1 1 calc R . . C12 C -0.0765(4) -0.3380(9) 0.0956(4) 0.060(3) Uani 1 1 d . . . H12A H -0.0954 -0.4338 0.0968 0.072 Uiso 1 1 calc R . . H12B H -0.0437 -0.3251 0.1302 0.072 Uiso 1 1 calc R . . H12C H -0.0673 -0.3479 0.0664 0.072 Uiso 1 1 calc R . . C13 C -0.1633(3) -0.2121(9) 0.0316(3) 0.041(2) Uani 1 1 d . . . H13A H -0.1544 -0.2166 0.0022 0.049 Uiso 1 1 calc R . . H13B H -0.1868 -0.1211 0.0260 0.049 Uiso 1 1 calc R . . H13C H -0.1816 -0.3102 0.0320 0.049 Uiso 1 1 calc R . . C14 C -0.0159(3) -0.0019(11) 0.1530(3) 0.0389(18) Uani 1 1 d . . . H14 H 0.0063 -0.0929 0.1524 0.047 Uiso 1 1 calc R . . C15 C -0.0245(3) -0.0285(15) 0.2019(3) 0.071(3) Uani 1 1 d . . . H15A H 0.0102 -0.0401 0.2346 0.085 Uiso 1 1 calc R . . H15B H -0.0458 -0.1250 0.1964 0.085 Uiso 1 1 calc R . . H15C H -0.0436 0.0627 0.2060 0.085 Uiso 1 1 calc R . . C16 C 0.0165(3) 0.1484(11) 0.1591(3) 0.045(2) Uani 1 1 d . . . H16A H -0.0030 0.2408 0.1617 0.054 Uiso 1 1 calc R . . H16B H 0.0219 0.1602 0.1275 0.054 Uiso 1 1 calc R . . H16C H 0.0513 0.1407 0.1919 0.054 Uiso 1 1 calc R . . C17 C -0.1206(3) 0.1583(8) 0.0896(3) 0.0267(15) Uani 1 1 d . . . H17 H -0.0954 0.2406 0.1142 0.032 Uiso 1 1 calc R . . C18 C -0.1535(4) 0.2394(10) 0.0361(3) 0.047(2) Uani 1 1 d . . . H18A H -0.1782 0.1627 0.0098 0.057 Uiso 1 1 calc R . . H18B H -0.1298 0.2821 0.0231 0.057 Uiso 1 1 calc R . . H18C H -0.1739 0.3263 0.0405 0.057 Uiso 1 1 calc R . . C19 C -0.1557(3) 0.1092(9) 0.1148(3) 0.0376(18) Uani 1 1 d . . . H19A H -0.1752 0.2020 0.1170 0.045 Uiso 1 1 calc R . . H19B H -0.1329 0.0668 0.1511 0.045 Uiso 1 1 calc R . . H19C H -0.1812 0.0276 0.0922 0.045 Uiso 1 1 calc R . . C41 C 0.6251(3) 1.6656(8) 0.2039(3) 0.0258(15) Uani 1 1 d . . . H41 H 0.6000 1.7467 0.2047 0.031 Uiso 1 1 calc R . . C42 C 0.6622(3) 1.6165(10) 0.2631(3) 0.043(2) Uani 1 1 d . . . H42A H 0.6893 1.5424 0.2648 0.051 Uiso 1 1 calc R . . H42B H 0.6409 1.5650 0.2776 0.051 Uiso 1 1 calc R . . H42C H 0.6797 1.7110 0.2847 0.051 Uiso 1 1 calc R . . C43 C 0.6566(3) 1.7483(10) 0.1805(3) 0.043(2) Uani 1 1 d . . . H43A H 0.6747 1.8414 0.2025 0.052 Uiso 1 1 calc R . . H43B H 0.6321 1.7819 0.1433 0.052 Uiso 1 1 calc R . . H43C H 0.6832 1.6749 0.1804 0.052 Uiso 1 1 calc R . . C44 C 0.6167(3) 1.3116(8) 0.1916(2) 0.0239(14) Uani 1 1 d . . . H44 H 0.6281 1.3163 0.2310 0.029 Uiso 1 1 calc R . . C45 C 0.5797(3) 1.1687(9) 0.1686(3) 0.047(2) Uani 1 1 d . . . H45A H 0.5677 1.1595 0.1299 0.057 Uiso 1 1 calc R . . H45B H 0.5486 1.1828 0.1742 0.057 Uiso 1 1 calc R . . H45C H 0.5989 1.0721 0.1871 0.057 Uiso 1 1 calc R . . C46 C 0.6672(3) 1.2905(9) 0.1870(3) 0.0361(18) Uani 1 1 d . . . H46A H 0.6857 1.1935 0.2060 0.043 Uiso 1 1 calc R . . H46B H 0.6908 1.3821 0.2033 0.043 Uiso 1 1 calc R . . H46C H 0.6577 1.2824 0.1488 0.043 Uiso 1 1 calc R . . C47 C 0.5202(2) 1.5074(9) 0.1650(2) 0.0276(14) Uani 1 1 d . . . H47 H 0.4979 1.4150 0.1439 0.033 Uiso 1 1 calc R . . C48 C 0.5296(3) 1.4912(12) 0.2236(3) 0.051(2) Uani 1 1 d . . . H48A H 0.5510 1.5812 0.2452 0.061 Uiso 1 1 calc R . . H48B H 0.5488 1.3920 0.2394 0.061 Uiso 1 1 calc R . . H48C H 0.4951 1.4902 0.2232 0.061 Uiso 1 1 calc R . . C49 C 0.4889(3) 1.6564(9) 0.1389(3) 0.0322(17) Uani 1 1 d . . . H49A H 0.4542 1.6520 0.1380 0.039 Uiso 1 1 calc R . . H49B H 0.4834 1.6646 0.1019 0.039 Uiso 1 1 calc R . . H49C H 0.5090 1.7492 0.1598 0.039 Uiso 1 1 calc R . . C31 C 0.3641(2) 0.9932(8) 0.0753(2) 0.0226(13) Uani 1 1 d . . . H31 H 0.3735 0.8778 0.0794 0.027 Uiso 1 1 calc R . . C32 C 0.4045(3) 1.0713(11) 0.1272(3) 0.047(2) Uani 1 1 d . . . H32A H 0.3926 1.1792 0.1290 0.057 Uiso 1 1 calc R . . H32B H 0.4393 1.0758 0.1282 0.057 Uiso 1 1 calc R . . H32C H 0.4078 1.0096 0.1581 0.057 Uiso 1 1 calc R . . C33 C 0.3079(3) 1.0035(10) 0.0698(3) 0.0371(17) Uani 1 1 d . . . H33A H 0.3088 0.9601 0.1024 0.045 Uiso 1 1 calc R . . H33B H 0.2827 0.9422 0.0382 0.045 Uiso 1 1 calc R . . H33C H 0.2965 1.1147 0.0653 0.045 Uiso 1 1 calc R . . C34 C 0.3544(2) 1.2716(7) -0.0002(2) 0.0187(13) Uani 1 1 d . . . H34 H 0.3564 1.2896 -0.0341 0.022 Uiso 1 1 calc R . . C35 C 0.3963(2) 1.3799(8) 0.0420(3) 0.0271(15) Uani 1 1 d . . . H35A H 0.3888 1.4901 0.0294 0.033 Uiso 1 1 calc R . . H35B H 0.4318 1.3495 0.0477 0.033 Uiso 1 1 calc R . . H35C H 0.3953 1.3700 0.0761 0.033 Uiso 1 1 calc R . . C36 C 0.2979(2) 1.3224(8) -0.0131(3) 0.0269(15) Uani 1 1 d . . . H36A H 0.2948 1.3185 0.0199 0.032 Uiso 1 1 calc R . . H36B H 0.2717 1.2502 -0.0401 0.032 Uiso 1 1 calc R . . H36C H 0.2911 1.4309 -0.0274 0.032 Uiso 1 1 calc R . . C37 C 0.3159(2) 0.9510(8) -0.0426(2) 0.0230(14) Uani 1 1 d . . . H37 H 0.2807 0.9794 -0.0451 0.028 Uiso 1 1 calc R . . C38 C 0.3226(3) 0.7714(8) -0.0345(3) 0.0315(16) Uani 1 1 d . . . H38A H 0.2939 0.7175 -0.0659 0.038 Uiso 1 1 calc R . . H38B H 0.3207 0.7417 -0.0019 0.038 Uiso 1 1 calc R . . H38C H 0.3573 0.7397 -0.0305 0.038 Uiso 1 1 calc R . . C39 C 0.3134(3) 1.0000(9) -0.0956(2) 0.0322(15) Uani 1 1 d . . . H39A H 0.3481 0.9803 -0.0936 0.039 Uiso 1 1 calc R . . H39B H 0.3047 1.1132 -0.1020 0.039 Uiso 1 1 calc R . . H39C H 0.2858 0.9379 -0.1253 0.039 Uiso 1 1 calc R . . C21 C 0.1786(2) 0.4539(7) 0.1242(2) 0.0222(14) Uani 1 1 d . . . H21 H 0.2155 0.4888 0.1510 0.027 Uiso 1 1 calc R . . C22 C 0.1766(3) 0.2749(8) 0.1289(3) 0.0364(18) Uani 1 1 d . . . H22A H 0.1405 0.2367 0.1040 0.044 Uiso 1 1 calc R . . H22B H 0.1857 0.2467 0.1661 0.044 Uiso 1 1 calc R . . H22C H 0.2023 0.2256 0.1198 0.044 Uiso 1 1 calc R . . C23 C 0.1690(3) 0.5052(10) 0.0684(2) 0.0323(16) Uani 1 1 d . . . H23A H 0.1958 0.4554 0.0609 0.039 Uiso 1 1 calc R . . H23B H 0.1720 0.6209 0.0675 0.039 Uiso 1 1 calc R . . H23C H 0.1332 0.4720 0.0409 0.039 Uiso 1 1 calc R . . C24 C 0.1443(3) 0.7714(8) 0.1400(3) 0.0266(15) Uani 1 1 d . . . H24 H 0.1393 0.7940 0.1031 0.032 Uiso 1 1 calc R . . C25 C 0.1043(3) 0.8763(9) 0.1462(3) 0.0341(17) Uani 1 1 d . . . H25A H 0.1088 0.8637 0.1827 0.041 Uiso 1 1 calc R . . H25B H 0.0679 0.8453 0.1195 0.041 Uiso 1 1 calc R . . H25C H 0.1103 0.9875 0.1405 0.041 Uiso 1 1 calc R . . C26 C 0.2020(3) 0.8200(8) 0.1797(3) 0.0314(16) Uani 1 1 d . . . H26A H 0.2090 0.9262 0.1704 0.038 Uiso 1 1 calc R . . H26B H 0.2268 0.7438 0.1775 0.038 Uiso 1 1 calc R . . H26C H 0.2070 0.8209 0.2166 0.038 Uiso 1 1 calc R . . C27 C 0.1436(2) 0.4821(8) 0.2069(2) 0.0248(14) Uani 1 1 d . . . H27 H 0.1358 0.3658 0.2015 0.030 Uiso 1 1 calc R . . C28 C 0.1059(3) 0.5473(11) 0.2256(3) 0.044(2) Uani 1 1 d . . . H28A H 0.1059 0.4770 0.2533 0.053 Uiso 1 1 calc R . . H28B H 0.0697 0.5537 0.1948 0.053 Uiso 1 1 calc R . . H28C H 0.1178 0.6536 0.2409 0.053 Uiso 1 1 calc R . . C29 C 0.2025(3) 0.4942(11) 0.2514(3) 0.046(2) Uani 1 1 d . . . H29A H 0.2113 0.6053 0.2624 0.055 Uiso 1 1 calc R . . H29B H 0.2257 0.4544 0.2375 0.055 Uiso 1 1 calc R . . H29C H 0.2079 0.4305 0.2827 0.055 Uiso 1 1 calc R . . F11 F 0.3773(2) 0.7395(6) 0.19010(19) 0.0590(14) Uani 1 1 d . . . F12 F 0.39624(19) 0.4346(7) 0.1876(3) 0.0799(19) Uani 1 1 d . . . F13 F 0.3476(2) 0.6049(6) 0.09644(19) 0.0542(13) Uani 1 1 d . . . F14 F 0.27526(18) 0.6906(5) 0.1226(2) 0.0525(13) Uani 1 1 d . . . F15 F 0.29490(17) 0.3844(5) 0.11941(18) 0.0409(11) Uani 1 1 d . . . F16 F 0.3208(2) 0.5268(6) 0.21193(18) 0.0573(14) Uani 1 1 d . . . F21 F -0.2416(3) 0.6563(11) 0.1462(2) 0.145(4) Uani 1 1 d . . . F22 F -0.1409(5) 0.7350(8) 0.1844(3) 0.167(5) Uani 1 1 d . . . F23 F -0.1143(2) 0.4403(9) 0.2150(2) 0.097(2) Uani 1 1 d . . . F24 F -0.2124(3) 0.3662(8) 0.1779(2) 0.088(2) Uani 1 1 d . . . F25 F -0.1733(2) 0.6040(6) 0.24677(17) 0.0558(14) Uani 1 1 d . . . F26 F -0.1818(2) 0.5058(6) 0.11378(17) 0.0499(12) Uani 1 1 d . . . 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 0.0272(2) 0.0222(2) 0.0281(2) 0.00118(19) 0.01969(18) -0.00127(18) Te2 0.01481(18) 0.0231(2) 0.01856(18) -0.00242(19) 0.00236(15) -0.00207(17) Te3 0.01738(19) 0.0186(2) 0.0314(2) 0.00313(19) 0.01385(17) 0.00328(17) Te4 0.0278(2) 0.0215(2) 0.01391(17) 0.00095(18) 0.00847(16) -0.00166(18) Sb1 0.0301(2) 0.0300(3) 0.0305(2) -0.0125(2) 0.0194(2) -0.0092(2) Sb2 0.0421(3) 0.0257(3) 0.0263(2) 0.0034(2) 0.0193(2) 0.0040(2) Ag1 0.0386(3) 0.0220(3) 0.0352(3) -0.0015(2) 0.0114(2) 0.0000(2) Ag2 0.0432(3) 0.0204(3) 0.0374(3) -0.0012(2) 0.0212(3) -0.0028(2) P1 0.0202(8) 0.0239(9) 0.0236(8) 0.0055(8) 0.0141(6) 0.0005(7) P2 0.0151(7) 0.0170(8) 0.0143(7) -0.0014(6) 0.0042(6) -0.0006(6) P3 0.0147(7) 0.0162(7) 0.0153(7) 0.0005(6) 0.0079(6) 0.0006(6) P4 0.0151(7) 0.0201(8) 0.0133(7) 0.0013(7) 0.0044(6) -0.0004(7) C11 0.038(4) 0.016(3) 0.046(4) 0.006(3) 0.032(4) 0.002(3) C12 0.064(6) 0.029(5) 0.125(9) 0.029(5) 0.075(6) 0.014(4) C13 0.049(5) 0.035(5) 0.050(5) -0.016(4) 0.033(4) -0.020(4) C14 0.021(3) 0.062(5) 0.031(4) 0.019(4) 0.010(3) 0.001(4) C15 0.038(5) 0.141(11) 0.026(4) 0.024(6) 0.010(4) -0.020(6) C16 0.028(4) 0.068(6) 0.025(4) 0.005(4) 0.002(3) -0.009(4) C17 0.030(4) 0.020(4) 0.032(4) 0.003(3) 0.016(3) 0.001(3) C18 0.072(6) 0.034(5) 0.050(5) 0.007(4) 0.041(5) 0.013(4) C19 0.050(5) 0.027(4) 0.050(5) 0.003(4) 0.035(4) 0.007(3) C41 0.027(4) 0.026(4) 0.025(3) -0.007(3) 0.013(3) -0.006(3) C42 0.049(5) 0.042(5) 0.020(4) -0.013(3) 0.003(3) 0.000(4) C43 0.048(5) 0.037(5) 0.049(5) -0.016(4) 0.026(4) -0.021(4) C44 0.029(4) 0.021(3) 0.015(3) 0.002(3) 0.005(3) 0.003(3) C45 0.057(5) 0.025(4) 0.031(4) 0.005(4) -0.001(4) -0.004(4) C46 0.035(4) 0.039(5) 0.033(4) 0.001(3) 0.015(3) 0.020(3) C47 0.018(3) 0.038(4) 0.024(3) 0.010(3) 0.008(3) 0.007(3) C48 0.025(4) 0.095(7) 0.038(4) 0.026(5) 0.021(3) 0.015(4) C49 0.027(4) 0.040(5) 0.037(4) 0.014(3) 0.020(3) 0.019(3) C31 0.032(3) 0.018(3) 0.023(3) 0.009(3) 0.017(3) 0.008(3) C32 0.066(6) 0.059(6) 0.019(4) -0.003(4) 0.022(4) -0.009(5) C33 0.038(4) 0.045(5) 0.045(4) 0.013(4) 0.032(4) 0.012(4) C34 0.020(3) 0.017(3) 0.020(3) 0.000(3) 0.010(3) -0.002(2) C35 0.023(3) 0.022(4) 0.039(4) -0.005(3) 0.017(3) 0.000(3) C36 0.023(3) 0.018(3) 0.035(4) 0.006(3) 0.010(3) 0.009(3) C37 0.017(3) 0.023(3) 0.026(3) -0.005(3) 0.008(3) -0.002(2) C38 0.033(4) 0.021(4) 0.034(4) 0.000(3) 0.011(3) -0.004(3) C39 0.037(4) 0.031(4) 0.016(3) 0.000(3) 0.003(3) 0.003(3) C21 0.021(3) 0.021(3) 0.024(3) -0.007(3) 0.010(3) -0.006(2) C22 0.031(4) 0.024(4) 0.047(5) -0.002(3) 0.013(4) 0.006(3) C23 0.026(3) 0.044(4) 0.025(3) -0.003(4) 0.011(3) 0.001(3) C24 0.032(4) 0.024(4) 0.024(3) 0.000(3) 0.014(3) -0.002(3) C25 0.025(4) 0.028(4) 0.038(4) -0.008(3) 0.006(3) 0.002(3) C26 0.031(4) 0.020(4) 0.047(4) -0.012(3) 0.021(3) -0.009(3) C27 0.029(3) 0.023(4) 0.015(3) 0.004(3) 0.005(3) -0.003(3) C28 0.052(5) 0.064(6) 0.025(4) -0.004(4) 0.025(4) 0.005(4) C29 0.041(4) 0.063(6) 0.020(3) 0.014(4) 0.003(3) -0.013(4) F11 0.077(4) 0.059(3) 0.049(3) -0.029(3) 0.036(3) -0.044(3) F12 0.034(3) 0.065(4) 0.111(5) 0.007(4) 0.012(3) 0.004(3) F13 0.082(4) 0.052(3) 0.058(3) -0.019(2) 0.058(3) -0.018(3) F14 0.052(3) 0.032(3) 0.091(4) 0.010(3) 0.048(3) 0.005(2) F15 0.045(3) 0.027(2) 0.052(3) -0.017(2) 0.025(2) -0.0104(19) F16 0.092(4) 0.055(3) 0.038(2) -0.012(2) 0.042(3) -0.030(3) F21 0.149(7) 0.223(9) 0.047(3) 0.029(5) 0.034(4) 0.152(7) F22 0.377(14) 0.074(5) 0.177(8) -0.070(5) 0.236(10) -0.127(7) F23 0.053(4) 0.139(6) 0.073(4) 0.001(4) 0.010(3) 0.035(4) F24 0.129(5) 0.082(5) 0.090(4) -0.035(4) 0.081(4) -0.051(4) F25 0.093(4) 0.052(3) 0.027(2) -0.006(2) 0.033(3) -0.004(3) F26 0.081(3) 0.043(3) 0.042(2) 0.004(2) 0.042(3) 0.018(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 Te1 P1 2.4346(15) . ? Te1 Ag1 2.7857(7) 3 ? Te1 Ag1 2.9359(7) . ? Te2 P2 2.4194(15) . ? Te2 Ag1 2.8036(7) 3_565 ? Te2 Ag1 2.8557(7) . ? Te3 P3 2.4218(15) . ? Te3 Ag2 2.7943(7) . ? Te3 Ag2 2.8740(7) 3_675 ? Te4 P4 2.4257(15) . ? Te4 Ag2 2.7692(7) . ? Te4 Ag2 2.9011(7) 3_685 ? Sb1 F12 1.854(5) . ? Sb1 F11 1.865(4) . ? Sb1 F14 1.865(4) . ? Sb1 F15 1.867(4) . ? Sb1 F13 1.871(4) . ? Sb1 F16 1.880(4) . ? Sb2 F21 1.813(6) . ? Sb2 F22 1.826(6) . ? Sb2 F24 1.847(6) . ? Sb2 F23 1.861(6) . ? Sb2 F26 1.864(4) . ? Sb2 F25 1.874(4) . ? Ag1 Te1 2.7857(7) 3 ? Ag1 Te2 2.8035(7) 3_565 ? Ag2 Te3 2.8740(7) 3_675 ? Ag2 Te4 2.9011(7) 3_685 ? P1 C14 1.831(7) . ? P1 C11 1.833(7) . ? P1 C17 1.856(7) . ? P2 C27 1.830(6) . ? P2 C21 1.833(6) . ? P2 C24 1.846(7) . ? P3 C37 1.829(6) . ? P3 C34 1.832(6) . ? P3 C31 1.839(6) . ? P4 C44 1.828(6) . ? P4 C47 1.838(6) . ? P4 C41 1.853(7) . ? C11 C13 1.518(10) . ? C11 C12 1.522(10) . ? C14 C16 1.527(11) . ? C14 C15 1.534(10) . ? C17 C18 1.503(10) . ? C17 C19 1.538(9) . ? C41 C43 1.516(9) . ? C41 C42 1.543(9) . ? C44 C46 1.518(9) . ? C44 C45 1.524(10) . ? C47 C49 1.509(9) . ? C47 C48 1.548(9) . ? C31 C32 1.509(9) . ? C31 C33 1.538(8) . ? C34 C35 1.519(8) . ? C34 C36 1.532(8) . ? C37 C39 1.521(9) . ? C37 C38 1.528(9) . ? C21 C22 1.517(9) . ? C21 C23 1.527(9) . ? C24 C25 1.520(9) . ? C24 C26 1.534(9) . ? C27 C28 1.513(9) . ? C27 C29 1.541(9) . ? 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 P1 Te1 Ag1 113.30(5) . 3 ? P1 Te1 Ag1 126.16(5) . . ? Ag1 Te1 Ag1 94.535(19) 3 . ? P2 Te2 Ag1 111.80(4) . 3_565 ? P2 Te2 Ag1 125.47(4) . . ? Ag1 Te2 Ag1 97.800(19) 3_565 . ? P3 Te3 Ag2 112.83(4) . . ? P3 Te3 Ag2 130.58(4) . 3_675 ? Ag2 Te3 Ag2 100.961(19) . 3_675 ? P4 Te4 Ag2 111.28(4) . . ? P4 Te4 Ag2 123.89(4) . 3_685 ? Ag2 Te4 Ag2 92.553(19) . 3_685 ? F12 Sb1 F11 90.1(2) . . ? F12 Sb1 F14 179.5(3) . . ? F11 Sb1 F14 89.8(2) . . ? F12 Sb1 F15 89.6(2) . . ? F11 Sb1 F15 179.5(2) . . ? F14 Sb1 F15 90.5(2) . . ? F12 Sb1 F13 91.9(3) . . ? F11 Sb1 F13 88.8(2) . . ? F14 Sb1 F13 88.6(2) . . ? F15 Sb1 F13 90.7(2) . . ? F12 Sb1 F16 91.4(3) . . ? F11 Sb1 F16 91.1(2) . . ? F14 Sb1 F16 88.2(2) . . ? F15 Sb1 F16 89.36(19) . . ? F13 Sb1 F16 176.8(2) . . ? F21 Sb2 F22 92.2(5) . . ? F21 Sb2 F24 90.4(4) . . ? F22 Sb2 F24 177.3(5) . . ? F21 Sb2 F23 177.4(4) . . ? F22 Sb2 F23 90.4(4) . . ? F24 Sb2 F23 86.9(3) . . ? F21 Sb2 F26 90.9(2) . . ? F22 Sb2 F26 90.1(2) . . ? F24 Sb2 F26 90.6(2) . . ? F23 Sb2 F26 89.5(2) . . ? F21 Sb2 F25 89.3(2) . . ? F22 Sb2 F25 89.2(2) . . ? F24 Sb2 F25 90.2(2) . . ? F23 Sb2 F25 90.3(3) . . ? F26 Sb2 F25 179.2(2) . . ? Te1 Ag1 Te2 128.13(2) 3 3_565 ? Te1 Ag1 Te2 131.12(2) 3 . ? Te2 Ag1 Te2 82.197(19) 3_565 . ? Te1 Ag1 Te1 85.464(19) 3 . ? Te2 Ag1 Te1 120.00(2) 3_565 . ? Te2 Ag1 Te1 113.67(2) . . ? Te4 Ag2 Te3 134.78(2) . . ? Te4 Ag2 Te3 125.52(2) . 3_675 ? Te3 Ag2 Te3 79.039(18) . 3_675 ? Te4 Ag2 Te4 87.446(19) . 3_685 ? Te3 Ag2 Te4 116.04(2) . 3_685 ? Te3 Ag2 Te4 117.67(2) 3_675 3_685 ? C14 P1 C11 107.9(3) . . ? C14 P1 C17 107.1(4) . . ? C11 P1 C17 107.9(3) . . ? C14 P1 Te1 111.8(2) . . ? C11 P1 Te1 109.9(2) . . ? C17 P1 Te1 112.1(2) . . ? C27 P2 C21 107.8(3) . . ? C27 P2 C24 114.4(3) . . ? C21 P2 C24 106.9(3) . . ? C27 P2 Te2 108.2(2) . . ? C21 P2 Te2 110.7(2) . . ? C24 P2 Te2 108.9(2) . . ? C37 P3 C34 107.0(3) . . ? C37 P3 C31 106.8(3) . . ? C34 P3 C31 114.6(3) . . ? C37 P3 Te3 112.3(2) . . ? C34 P3 Te3 108.97(19) . . ? C31 P3 Te3 107.3(2) . . ? C44 P4 C47 108.8(3) . . ? C44 P4 C41 109.1(3) . . ? C47 P4 C41 106.8(3) . . ? C44 P4 Te4 108.8(2) . . ? C47 P4 Te4 110.9(2) . . ? C41 P4 Te4 112.3(2) . . ? C13 C11 C12 110.1(7) . . ? C13 C11 P1 111.6(5) . . ? C12 C11 P1 112.5(5) . . ? C16 C14 C15 111.8(7) . . ? C16 C14 P1 112.0(5) . . ? C15 C14 P1 113.1(5) . . ? C18 C17 C19 110.8(6) . . ? C18 C17 P1 114.8(5) . . ? C19 C17 P1 112.6(5) . . ? C43 C41 C42 110.9(6) . . ? C43 C41 P4 114.1(5) . . ? C42 C41 P4 112.5(5) . . ? C46 C44 C45 111.4(6) . . ? C46 C44 P4 112.0(5) . . ? C45 C44 P4 112.6(5) . . ? C49 C47 C48 110.6(6) . . ? C49 C47 P4 111.7(5) . . ? C48 C47 P4 112.0(4) . . ? C32 C31 C33 110.1(6) . . ? C32 C31 P3 114.1(5) . . ? C33 C31 P3 114.2(4) . . ? C35 C34 C36 111.1(5) . . ? C35 C34 P3 113.9(4) . . ? C36 C34 P3 113.7(4) . . ? C39 C37 C38 111.0(6) . . ? C39 C37 P3 111.9(5) . . ? C38 C37 P3 111.9(5) . . ? C22 C21 C23 112.1(6) . . ? C22 C21 P2 112.6(5) . . ? C23 C21 P2 110.4(5) . . ? C25 C24 C26 111.3(6) . . ? C25 C24 P2 114.1(5) . . ? C26 C24 P2 113.2(5) . . ? C28 C27 C29 111.8(6) . . ? C28 C27 P2 114.8(5) . . ? C29 C27 P2 113.3(5) . . ? 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 P2 Te2 Ag1 Te1 11.14(6) . . . 3 ? Ag1 Te2 Ag1 Te1 135.05(4) 3_565 . . 3 ? P2 Te2 Ag1 Te2 -123.90(5) . . . 3_565 ? Ag1 Te2 Ag1 Te2 0.0 3_565 . . 3_565 ? P2 Te2 Ag1 Te1 116.70(5) . . . . ? Ag1 Te2 Ag1 Te1 -119.40(3) 3_565 . . . ? P1 Te1 Ag1 Te1 123.32(5) . . . 3 ? Ag1 Te1 Ag1 Te1 -0.002(2) 3 . . 3 ? P1 Te1 Ag1 Te2 -104.66(6) . . . 3_565 ? Ag1 Te1 Ag1 Te2 132.02(3) 3 . . 3_565 ? P1 Te1 Ag1 Te2 -9.96(6) . . . . ? Ag1 Te1 Ag1 Te2 -133.28(3) 3 . . . ? P4 Te4 Ag2 Te3 2.96(6) . . . . ? Ag2 Te4 Ag2 Te3 -125.09(4) 3_685 . . . ? P4 Te4 Ag2 Te3 -109.32(5) . . . 3_675 ? Ag2 Te4 Ag2 Te3 122.64(3) 3_685 . . 3_675 ? P4 Te4 Ag2 Te4 128.05(4) . . . 3_685 ? Ag2 Te4 Ag2 Te4 0.0 3_685 . . 3_685 ? P3 Te3 Ag2 Te4 86.93(5) . . . . ? Ag2 Te3 Ag2 Te4 -129.90(4) 3_675 . . . ? P3 Te3 Ag2 Te3 -143.17(4) . . . 3_675 ? Ag2 Te3 Ag2 Te3 0.0 3_675 . . 3_675 ? P3 Te3 Ag2 Te4 -27.59(5) . . . 3_685 ? Ag2 Te3 Ag2 Te4 115.58(3) 3_675 . . 3_685 ? Ag1 Te1 P1 C14 65.4(3) 3 . . . ? Ag1 Te1 P1 C14 -49.6(3) . . . . ? Ag1 Te1 P1 C11 -54.4(2) 3 . . . ? Ag1 Te1 P1 C11 -169.3(2) . . . . ? Ag1 Te1 P1 C17 -174.3(2) 3 . . . ? Ag1 Te1 P1 C17 70.7(2) . . . . ? Ag1 Te2 P2 C27 139.8(2) 3_565 . . . ? Ag1 Te2 P2 C27 -102.5(2) . . . . ? Ag1 Te2 P2 C21 -102.2(2) 3_565 . . . ? Ag1 Te2 P2 C21 15.5(2) . . . . ? Ag1 Te2 P2 C24 15.0(2) 3_565 . . . ? Ag1 Te2 P2 C24 132.7(2) . . . . ? Ag2 Te3 P3 C37 112.6(2) . . . . ? Ag2 Te3 P3 C37 -16.7(2) 3_675 . . . ? Ag2 Te3 P3 C34 -5.8(2) . . . . ? Ag2 Te3 P3 C34 -135.0(2) 3_675 . . . ? Ag2 Te3 P3 C31 -130.4(2) . . . . ? Ag2 Te3 P3 C31 100.4(2) 3_675 . . . ? Ag2 Te4 P4 C44 57.7(2) . . . . ? Ag2 Te4 P4 C44 166.3(2) 3_685 . . . ? Ag2 Te4 P4 C47 -62.0(3) . . . . ? Ag2 Te4 P4 C47 46.6(3) 3_685 . . . ? Ag2 Te4 P4 C41 178.5(2) . . . . ? Ag2 Te4 P4 C41 -72.9(2) 3_685 . . . ? C14 P1 C11 C13 -177.2(5) . . . . ? C17 P1 C11 C13 67.4(5) . . . . ? Te1 P1 C11 C13 -55.1(5) . . . . ? C14 P1 C11 C12 -52.9(7) . . . . ? C17 P1 C11 C12 -168.3(6) . . . . ? Te1 P1 C11 C12 69.2(6) . . . . ? C11 P1 C14 C16 178.6(6) . . . . ? C17 P1 C14 C16 -65.4(6) . . . . ? Te1 P1 C14 C16 57.7(6) . . . . ? C11 P1 C14 C15 -54.0(8) . . . . ? C17 P1 C14 C15 62.0(8) . . . . ? Te1 P1 C14 C15 -174.9(6) . . . . ? C14 P1 C17 C18 144.0(6) . . . . ? C11 P1 C17 C18 -100.1(6) . . . . ? Te1 P1 C17 C18 21.0(6) . . . . ? C14 P1 C17 C19 -88.0(6) . . . . ? C11 P1 C17 C19 28.0(6) . . . . ? Te1 P1 C17 C19 149.0(4) . . . . ? C44 P4 C41 C43 101.4(6) . . . . ? C47 P4 C41 C43 -141.1(5) . . . . ? Te4 P4 C41 C43 -19.3(6) . . . . ? C44 P4 C41 C42 -26.0(6) . . . . ? C47 P4 C41 C42 91.5(5) . . . . ? Te4 P4 C41 C42 -146.7(4) . . . . ? C47 P4 C44 C46 175.9(5) . . . . ? C41 P4 C44 C46 -67.9(5) . . . . ? Te4 P4 C44 C46 55.0(5) . . . . ? C47 P4 C44 C45 49.5(6) . . . . ? C41 P4 C44 C45 165.7(5) . . . . ? Te4 P4 C44 C45 -71.4(5) . . . . ? C44 P4 C47 C49 -177.3(5) . . . . ? C41 P4 C47 C49 65.0(6) . . . . ? Te4 P4 C47 C49 -57.7(5) . . . . ? C44 P4 C47 C48 57.9(7) . . . . ? C41 P4 C47 C48 -59.7(7) . . . . ? Te4 P4 C47 C48 177.5(5) . . . . ? C37 P3 C31 C32 180.0(5) . . . . ? C34 P3 C31 C32 -61.8(6) . . . . ? Te3 P3 C31 C32 59.4(6) . . . . ? C37 P3 C31 C33 -52.2(6) . . . . ? C34 P3 C31 C33 66.0(6) . . . . ? Te3 P3 C31 C33 -172.8(5) . . . . ? C37 P3 C34 C35 -175.7(4) . . . . ? C31 P3 C34 C35 66.1(5) . . . . ? Te3 P3 C34 C35 -54.1(5) . . . . ? C37 P3 C34 C36 55.6(5) . . . . ? C31 P3 C34 C36 -62.6(5) . . . . ? Te3 P3 C34 C36 177.2(4) . . . . ? C34 P3 C37 C39 54.9(5) . . . . ? C31 P3 C37 C39 178.0(5) . . . . ? Te3 P3 C37 C39 -64.6(5) . . . . ? C34 P3 C37 C38 -179.8(5) . . . . ? C31 P3 C37 C38 -56.6(5) . . . . ? Te3 P3 C37 C38 60.7(5) . . . . ? C27 P2 C21 C22 51.2(5) . . . . ? C24 P2 C21 C22 174.6(5) . . . . ? Te2 P2 C21 C22 -67.1(5) . . . . ? C27 P2 C21 C23 177.2(4) . . . . ? C24 P2 C21 C23 -59.4(5) . . . . ? Te2 P2 C21 C23 59.0(5) . . . . ? C27 P2 C24 C25 -68.2(6) . . . . ? C21 P2 C24 C25 172.5(5) . . . . ? Te2 P2 C24 C25 52.9(5) . . . . ? C27 P2 C24 C26 60.3(6) . . . . ? C21 P2 C24 C26 -58.9(5) . . . . ? Te2 P2 C24 C26 -178.5(4) . . . . ? C21 P2 C27 C28 -176.3(5) . . . . ? C24 P2 C27 C28 65.0(6) . . . . ? Te2 P2 C27 C28 -56.5(6) . . . . ? C21 P2 C27 C29 53.7(6) . . . . ? C24 P2 C27 C29 -65.0(6) . . . . ? Te2 P2 C27 C29 173.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 F22 1.00 2.36 3.331(9) 162.9 1_545 C15 H15A F23 0.98 2.61 3.508(10) 152.6 2_545 C44 H44 F11 1.00 2.39 3.318(8) 153.4 2_655 C48 H48B F11 0.98 2.45 3.353(9) 152.7 2_655 C48 H48C F12 0.98 2.54 3.469(9) 157.7 1_565 C39 H39B F21 0.98 2.53 3.434(10) 153.4 3_575 C27 H27 F25 1.00 2.57 3.391(8) 138.7 2_545 C28 H28A F22 0.98 2.56 3.453(10) 151.4 2_545 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.826 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.200 # Attachment 'lacra.cif' #============================================================================= # cif data for "lacra" #============================================================================= data_lacra _database_code_depnum_ccdc_archive 'CCDC 636034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Bis-(triisopropylphosphine selenide)-silver(i) hexafluoroantimonate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H42 Ag F6 P2 Sb Se2' _chemical_formula_weight 822.00 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' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' 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 8.6889(6) _cell_length_b 23.6812(16) _cell_length_c 13.6253(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.965(3) _cell_angle_gamma 90.00 _cell_volume 2799.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7159 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.423 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5234 _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 'phi and omega 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 59721 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.53 _reflns_number_total 8562 _reflns_number_gt 7322 _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^)+(0.0424P)^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 others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8562 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Sb Sb 0.545973(16) 0.165675(6) 0.512250(11) 0.02114(4) Uani 1 1 d . . . Ag Ag 0.75781(2) 0.027862(7) 1.033136(14) 0.02694(5) Uani 1 1 d . . . Se1 Se 0.98676(2) -0.018482(9) 1.118778(14) 0.01825(5) Uani 1 1 d . . . Se2 Se 0.51779(2) 0.068505(8) 0.952810(18) 0.02207(6) Uani 1 1 d . . . P1 P 1.02390(6) 0.01283(2) 1.26772(4) 0.01390(9) Uani 1 1 d . . . P2 P 0.54065(6) 0.16007(2) 0.95572(4) 0.01510(10) Uani 1 1 d . . . F1 F 0.5444(2) 0.11991(7) 0.62436(13) 0.0515(5) Uani 1 1 d . . . F2 F 0.5518(2) 0.21178(7) 0.40132(13) 0.0509(5) Uani 1 1 d . . . F3 F 0.74987(17) 0.18519(7) 0.54724(14) 0.0443(4) Uani 1 1 d . . . F4 F 0.47695(18) 0.22722(7) 0.58417(14) 0.0429(4) Uani 1 1 d . . . F5 F 0.34131(18) 0.14596(8) 0.47852(16) 0.0512(5) Uani 1 1 d . . . F6 F 0.61266(18) 0.10422(6) 0.43918(13) 0.0392(4) Uani 1 1 d . . . C1 C 0.9521(2) 0.08528(9) 1.27829(15) 0.0176(4) Uani 1 1 d . . . H1 H 0.8379 0.0830 1.2656 0.021 Uiso 1 1 calc R . . C2 C 0.9777(3) 0.10940(10) 1.38270(16) 0.0236(4) Uani 1 1 d . . . H2A H 1.0880 0.1160 1.3968 0.028 Uiso 1 1 calc R . . H2B H 0.9398 0.0824 1.4304 0.028 Uiso 1 1 calc R . . H2C H 0.9217 0.1451 1.3875 0.028 Uiso 1 1 calc R . . C3 C 1.0103(3) 0.12599(10) 1.20112(17) 0.0255(5) Uani 1 1 d . . . H3A H 0.9502 0.1610 1.2015 0.031 Uiso 1 1 calc R . . H3B H 0.9988 0.1085 1.1360 0.031 Uiso 1 1 calc R . . H3C H 1.1193 0.1345 1.2165 0.031 Uiso 1 1 calc R . . C4 C 0.9168(2) -0.03028(8) 1.35258(14) 0.0160(4) Uani 1 1 d . . . H4 H 0.9417 -0.0161 1.4207 0.019 Uiso 1 1 calc R . . C5 C 0.7417(2) -0.02408(10) 1.33150(17) 0.0232(4) Uani 1 1 d . . . H5A H 0.7161 -0.0325 1.2621 0.028 Uiso 1 1 calc R . . H5B H 0.7104 0.0147 1.3461 0.028 Uiso 1 1 calc R . . H5C H 0.6873 -0.0505 1.3729 0.028 Uiso 1 1 calc R . . C6 C 0.9682(3) -0.09246(9) 1.34867(17) 0.0228(4) Uani 1 1 d . . . H6A H 0.9091 -0.1149 1.3940 0.027 Uiso 1 1 calc R . . H6B H 1.0782 -0.0951 1.3678 0.027 Uiso 1 1 calc R . . H6C H 0.9500 -0.1069 1.2817 0.027 Uiso 1 1 calc R . . C7 C 1.2310(2) 0.00371(9) 1.29887(15) 0.0178(4) Uani 1 1 d . . . H7 H 1.2580 -0.0351 1.2765 0.021 Uiso 1 1 calc R . . C8 C 1.2745(2) 0.00585(10) 1.41002(16) 0.0226(4) Uani 1 1 d . . . H8A H 1.3841 -0.0030 1.4213 0.027 Uiso 1 1 calc R . . H8B H 1.2128 -0.0218 1.4443 0.027 Uiso 1 1 calc R . . H8C H 1.2541 0.0438 1.4351 0.027 Uiso 1 1 calc R . . C9 C 1.3315(3) 0.04438(11) 1.24327(18) 0.0275(5) Uani 1 1 d . . . H9A H 1.3278 0.0819 1.2733 0.033 Uiso 1 1 calc R . . H9B H 1.2931 0.0466 1.1745 0.033 Uiso 1 1 calc R . . H9C H 1.4381 0.0307 1.2464 0.033 Uiso 1 1 calc R . . C10 C 0.3467(2) 0.18958(9) 0.93569(16) 0.0187(4) Uani 1 1 d . . . H10 H 0.3559 0.2317 0.9364 0.022 Uiso 1 1 calc R . . C11 C 0.2406(3) 0.17263(11) 1.01645(18) 0.0264(5) Uani 1 1 d . . . H11A H 0.1374 0.1881 1.0016 0.032 Uiso 1 1 calc R . . H11B H 0.2816 0.1875 1.0796 0.032 Uiso 1 1 calc R . . H11C H 0.2346 0.1314 1.0200 0.032 Uiso 1 1 calc R . . C12 C 0.2763(3) 0.17192(11) 0.83432(18) 0.0279(5) Uani 1 1 d . . . H12A H 0.2645 0.1308 0.8321 0.034 Uiso 1 1 calc R . . H12B H 0.3444 0.1840 0.7831 0.034 Uiso 1 1 calc R . . H12C H 0.1752 0.1898 0.8232 0.034 Uiso 1 1 calc R . . C13 C 0.6528(2) 0.18178(9) 0.85150(16) 0.0200(4) Uani 1 1 d . . . H13 H 0.6132 0.1590 0.7938 0.024 Uiso 1 1 calc R . . C14 C 0.6349(3) 0.24414(10) 0.8214(2) 0.0301(5) Uani 1 1 d . . . H14A H 0.6867 0.2681 0.8717 0.036 Uiso 1 1 calc R . . H14B H 0.5252 0.2539 0.8152 0.036 Uiso 1 1 calc R . . H14C H 0.6815 0.2502 0.7583 0.036 Uiso 1 1 calc R . . C15 C 0.8228(3) 0.16716(11) 0.8675(2) 0.0343(6) Uani 1 1 d . . . H15A H 0.8742 0.1720 0.8057 0.041 Uiso 1 1 calc R . . H15B H 0.8332 0.1279 0.8894 0.041 Uiso 1 1 calc R . . H15C H 0.8703 0.1922 0.9176 0.041 Uiso 1 1 calc R . . C16 C 0.6312(2) 0.18817(10) 1.07097(16) 0.0210(4) Uani 1 1 d . . . H16 H 0.7450 0.1840 1.0657 0.025 Uiso 1 1 calc R . . C17 C 0.5897(3) 0.15533(11) 1.16305(18) 0.0313(5) Uani 1 1 d . . . H17A H 0.6559 0.1678 1.2193 0.038 Uiso 1 1 calc R . . H17B H 0.6051 0.1149 1.1523 0.038 Uiso 1 1 calc R . . H17C H 0.4816 0.1624 1.1764 0.038 Uiso 1 1 calc R . . C18 C 0.6005(3) 0.25148(10) 1.08256(19) 0.0292(5) Uani 1 1 d . . . H18A H 0.4916 0.2574 1.0950 0.035 Uiso 1 1 calc R . . H18B H 0.6253 0.2712 1.0222 0.035 Uiso 1 1 calc R . . H18C H 0.6649 0.2663 1.1379 0.035 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 Sb 0.01854(7) 0.01704(7) 0.02781(8) -0.00082(5) 0.00077(5) -0.00118(5) Ag 0.02514(9) 0.02304(9) 0.03159(10) 0.00086(7) -0.00882(7) 0.00667(6) Se1 0.02082(10) 0.02256(11) 0.01120(9) -0.00169(7) -0.00091(7) 0.00605(7) Se2 0.01916(10) 0.01189(10) 0.03445(13) 0.00327(8) -0.00549(8) -0.00001(7) P1 0.0150(2) 0.0152(2) 0.0114(2) 0.00054(18) 0.00003(16) 0.00007(17) P2 0.0149(2) 0.0118(2) 0.0185(2) 0.00095(18) -0.00110(18) 0.00044(17) F1 0.0767(13) 0.0400(10) 0.0384(10) 0.0105(8) 0.0073(9) -0.0168(9) F2 0.0845(14) 0.0312(9) 0.0365(9) 0.0100(7) -0.0032(9) 0.0019(9) F3 0.0223(7) 0.0369(9) 0.0729(13) -0.0018(8) -0.0057(7) -0.0051(6) F4 0.0371(8) 0.0327(8) 0.0598(11) -0.0232(8) 0.0117(7) -0.0045(7) F5 0.0247(8) 0.0395(9) 0.0880(14) -0.0217(10) -0.0092(8) -0.0024(7) F6 0.0420(9) 0.0255(7) 0.0507(10) -0.0097(7) 0.0076(7) 0.0067(6) C1 0.0191(9) 0.0151(9) 0.0185(9) 0.0008(7) 0.0000(7) 0.0007(7) C2 0.0292(11) 0.0208(10) 0.0211(10) -0.0035(8) 0.0031(8) -0.0001(8) C3 0.0348(12) 0.0180(10) 0.0240(11) 0.0038(9) 0.0033(9) -0.0014(9) C4 0.0203(9) 0.0170(9) 0.0106(8) 0.0003(7) 0.0012(7) -0.0031(7) C5 0.0202(10) 0.0256(11) 0.0240(11) 0.0004(9) 0.0026(8) -0.0031(8) C6 0.0295(11) 0.0182(10) 0.0206(10) 0.0033(8) -0.0008(8) -0.0016(8) C7 0.0155(8) 0.0210(10) 0.0168(9) 0.0010(8) -0.0011(7) 0.0012(7) C8 0.0204(9) 0.0280(11) 0.0188(10) 0.0008(9) -0.0044(7) 0.0006(8) C9 0.0188(10) 0.0378(13) 0.0260(11) 0.0069(10) 0.0026(8) -0.0030(9) C10 0.0153(9) 0.0166(9) 0.0238(10) 0.0019(8) -0.0017(7) 0.0030(7) C11 0.0184(10) 0.0285(12) 0.0327(12) 0.0025(10) 0.0052(9) 0.0015(8) C12 0.0247(11) 0.0292(12) 0.0287(12) -0.0003(10) -0.0098(9) 0.0033(9) C13 0.0229(10) 0.0162(9) 0.0213(10) 0.0000(8) 0.0055(8) -0.0003(8) C14 0.0364(13) 0.0218(11) 0.0330(13) 0.0078(10) 0.0099(10) 0.0016(9) C15 0.0258(12) 0.0290(13) 0.0492(16) 0.0051(12) 0.0146(11) 0.0065(9) C16 0.0182(9) 0.0246(11) 0.0201(10) -0.0005(8) -0.0017(7) -0.0009(8) C17 0.0371(13) 0.0341(13) 0.0222(11) 0.0039(10) -0.0031(10) 0.0032(10) C18 0.0342(12) 0.0250(11) 0.0279(12) -0.0078(10) -0.0036(9) -0.0034(9) _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 Sb F2 1.8674(17) . ? Sb F3 1.8687(15) . ? Sb F4 1.8721(15) . ? Sb F6 1.8721(15) . ? Sb F5 1.8727(16) . ? Sb F1 1.8736(17) . ? Ag Se2 2.4975(3) . ? Ag Se1 2.5067(3) . ? Se1 P1 2.1691(5) . ? Se2 P2 2.1776(6) . ? P1 C4 1.832(2) . ? P1 C1 1.834(2) . ? P1 C7 1.8401(19) . ? P2 C10 1.832(2) . ? P2 C13 1.837(2) . ? P2 C16 1.844(2) . ? C1 C3 1.532(3) . ? C1 C2 1.538(3) . ? C4 C6 1.540(3) . ? C4 C5 1.541(3) . ? C7 C9 1.527(3) . ? C7 C8 1.543(3) . ? C10 C11 1.525(3) . ? C10 C12 1.539(3) . ? C13 C15 1.521(3) . ? C13 C14 1.538(3) . ? C16 C18 1.533(3) . ? C16 C17 1.535(3) . ? 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 F2 Sb F3 89.82(9) . . ? F2 Sb F4 89.50(8) . . ? F3 Sb F4 89.95(7) . . ? F2 Sb F6 90.12(8) . . ? F3 Sb F6 90.71(8) . . ? F4 Sb F6 179.23(8) . . ? F2 Sb F5 90.70(9) . . ? F3 Sb F5 179.42(9) . . ? F4 Sb F5 89.81(7) . . ? F6 Sb F5 89.53(7) . . ? F2 Sb F1 178.78(9) . . ? F3 Sb F1 88.96(9) . . ? F4 Sb F1 90.42(9) . . ? F6 Sb F1 89.97(8) . . ? F5 Sb F1 90.51(9) . . ? Se2 Ag Se1 175.816(11) . . ? P1 Se1 Ag 111.220(16) . . ? P2 Se2 Ag 107.605(16) . . ? C4 P1 C1 106.61(10) . . ? C4 P1 C7 108.15(9) . . ? C1 P1 C7 115.11(10) . . ? C4 P1 Se1 110.13(7) . . ? C1 P1 Se1 111.02(7) . . ? C7 P1 Se1 105.79(7) . . ? C10 P2 C13 107.40(10) . . ? C10 P2 C16 109.75(10) . . ? C13 P2 C16 109.71(10) . . ? C10 P2 Se2 107.15(7) . . ? C13 P2 Se2 108.43(7) . . ? C16 P2 Se2 114.16(8) . . ? C3 C1 C2 111.36(18) . . ? C3 C1 P1 114.15(15) . . ? C2 C1 P1 112.73(14) . . ? C6 C4 C5 111.71(17) . . ? C6 C4 P1 110.69(14) . . ? C5 C4 P1 110.98(14) . . ? C9 C7 C8 110.43(18) . . ? C9 C7 P1 112.89(14) . . ? C8 C7 P1 114.17(15) . . ? C11 C10 C12 110.41(19) . . ? C11 C10 P2 112.21(15) . . ? C12 C10 P2 110.48(15) . . ? C15 C13 C14 109.92(19) . . ? C15 C13 P2 112.07(16) . . ? C14 C13 P2 115.09(16) . . ? C18 C16 C17 111.2(2) . . ? C18 C16 P2 111.84(15) . . ? C17 C16 P2 113.92(16) . . ? 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 Se2 Ag Se1 P1 -88.09(15) . . . . ? Se1 Ag Se2 P2 144.21(15) . . . . ? Ag Se1 P1 C4 89.77(7) . . . . ? Ag Se1 P1 C1 -28.07(7) . . . . ? Ag Se1 P1 C7 -153.58(7) . . . . ? Ag Se2 P2 C10 -161.57(7) . . . . ? Ag Se2 P2 C13 82.79(7) . . . . ? Ag Se2 P2 C16 -39.84(8) . . . . ? C4 P1 C1 C3 -171.01(15) . . . . ? C7 P1 C1 C3 69.07(18) . . . . ? Se1 P1 C1 C3 -51.05(16) . . . . ? C4 P1 C1 C2 60.63(17) . . . . ? C7 P1 C1 C2 -59.29(18) . . . . ? Se1 P1 C1 C2 -179.41(13) . . . . ? C1 P1 C4 C6 179.60(14) . . . . ? C7 P1 C4 C6 -56.08(16) . . . . ? Se1 P1 C4 C6 59.07(15) . . . . ? C1 P1 C4 C5 54.97(16) . . . . ? C7 P1 C4 C5 179.29(14) . . . . ? Se1 P1 C4 C5 -65.56(15) . . . . ? C4 P1 C7 C9 -171.33(16) . . . . ? C1 P1 C7 C9 -52.26(19) . . . . ? Se1 P1 C7 C9 70.70(17) . . . . ? C4 P1 C7 C8 -44.12(18) . . . . ? C1 P1 C7 C8 74.95(18) . . . . ? Se1 P1 C7 C8 -162.09(14) . . . . ? C13 P2 C10 C11 178.11(16) . . . . ? C16 P2 C10 C11 -62.68(18) . . . . ? Se2 P2 C10 C11 61.78(16) . . . . ? C13 P2 C10 C12 54.42(18) . . . . ? C16 P2 C10 C12 173.63(16) . . . . ? Se2 P2 C10 C12 -61.90(16) . . . . ? C10 P2 C13 C15 171.45(17) . . . . ? C16 P2 C13 C15 52.21(19) . . . . ? Se2 P2 C13 C15 -73.08(17) . . . . ? C10 P2 C13 C14 44.88(19) . . . . ? C16 P2 C13 C14 -74.36(19) . . . . ? Se2 P2 C13 C14 160.35(15) . . . . ? C10 P2 C16 C18 -42.18(19) . . . . ? C13 P2 C16 C18 75.60(18) . . . . ? Se2 P2 C16 C18 -162.48(14) . . . . ? C10 P2 C16 C17 84.99(18) . . . . ? C13 P2 C16 C17 -157.23(16) . . . . ? Se2 P2 C16 C17 -35.31(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C5 H5C F1 0.98 2.60 3.442(3) 144.0 3_657 C18 H18A F3 0.98 2.56 3.407(3) 145.1 4_566 C2 H2A F5 0.98 2.52 3.465(3) 162.8 1_656 C8 H8C F5 0.98 2.60 3.487(3) 151.4 1_656 C5 H5B F6 0.98 2.63 3.579(3) 162.0 1_556 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.046 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.124