Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_address ; Department of Chemistry, University of Calgary, 2500 University Drive NW, Calgary, AB, T2N 1N4, Canada ; _publ_contact_author_email chivers@ucalgary.ca _publ_section_title ; Syntheses, X-ray structures and AACVD studies of group 11 ditelluroimidodiphosphinate complexes ; loop_ _publ_author_name M.Afzaal T.Chivers M.C.Copsey P.O'Brien A.Panneerselvam # Attachment 'Revisedcomplex8.cif' data_complex8 _database_code_depnum_ccdc_archive 'CCDC 612707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H80 Ag4 N4 P8 Te8, 2(C4 H8 O)' _chemical_formula_sum 'C104 H96 Ag4 N4 O2 P8 Te8' _chemical_formula_weight 3133.89 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' 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' Te Te -0.5308 1.6751 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5800(3) _cell_length_b 15.0793(3) _cell_length_c 17.7612(5) _cell_angle_alpha 98.443(2) _cell_angle_beta 100.975(1) _cell_angle_gamma 103.106(2) _cell_volume 2655.29(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11730 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 3.050 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8381 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor, 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18045 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9349 _reflns_number_gt 7760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The phenyl ring situated on P3 is disordered over two positions, C25-C30 and C25A-C30A. The anisotropic displacement parameters were best refined with occupancy factors of 0.5. Pairs of corresponding atoms in the two components of each ring were assigned with the same anisotropic displacement parameters. The complex contains a molecule of tetrahydrofuran in the lattice which is disorderd over two positions, O1/C50-C53 and O2/C54-C57. The anisotropic displacement parameters were best refined with occupancy factors of 0.5. 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^)+(0.0458P)^2^+7.5146P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9349 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Ag1 Ag 0.50287(5) 0.09371(3) 0.67148(3) 0.03573(12) Uani 1 1 d . . . Ag2 Ag 0.60416(5) 0.08920(3) 0.51005(3) 0.03452(12) Uani 1 1 d . . . Te1 Te 0.24273(3) 0.00235(2) 0.57233(2) 0.02496(10) Uani 1 1 d . . . Te2 Te 0.61006(3) -0.06170(2) 0.62929(2) 0.02696(10) Uani 1 1 d . . . Te3 Te 0.55290(5) 0.14856(3) 0.83378(2) 0.04215(12) Uani 1 1 d . A . Te4 Te 0.57228(3) 0.24573(2) 0.59879(2) 0.02562(10) Uani 1 1 d . A . P1 P 0.18694(13) -0.13597(9) 0.62702(8) 0.0226(3) Uani 1 1 d . . . P2 P 0.44573(13) -0.17870(9) 0.66763(8) 0.0230(3) Uani 1 1 d . . . P3 P 0.61922(14) 0.31023(10) 0.83247(8) 0.0244(3) Uani 1 1 d . . . P4 P 0.76445(13) 0.31310(9) 0.70827(8) 0.0222(3) Uani 1 1 d . . . N1 N 0.2897(4) -0.1997(3) 0.6285(3) 0.0243(10) Uani 1 1 d . . . N2 N 0.7404(4) 0.3443(3) 0.7926(3) 0.0281(10) Uani 1 1 d . A . C1 C 0.0294(5) -0.2039(4) 0.5640(3) 0.0231(11) Uani 1 1 d . . . C2 C 0.0200(5) -0.2873(4) 0.5151(3) 0.0266(12) Uani 1 1 d . . . H2 H 0.0953 -0.3121 0.5169 0.032 Uiso 1 1 calc R . . C3 C -0.1025(6) -0.3344(4) 0.4632(3) 0.0320(13) Uani 1 1 d . . . H3 H -0.1097 -0.3906 0.4285 0.038 Uiso 1 1 calc R . . C4 C -0.2097(5) -0.3003(4) 0.4621(3) 0.0280(12) Uani 1 1 d . . . H4 H -0.2918 -0.3334 0.4267 0.034 Uiso 1 1 calc R . . C5 C -0.2036(6) -0.2189(4) 0.5106(4) 0.0374(15) Uani 1 1 d . . . H5 H -0.2809 -0.1966 0.5096 0.045 Uiso 1 1 calc R . . C6 C -0.0824(6) -0.1696(4) 0.5613(4) 0.0349(14) Uani 1 1 d . . . H6 H -0.0761 -0.1122 0.5941 0.042 Uiso 1 1 calc R . . C7 C 0.1504(6) -0.1105(4) 0.7227(3) 0.0288(13) Uani 1 1 d . . . C8 C 0.2319(6) -0.0348(4) 0.7779(3) 0.0334(13) Uani 1 1 d . . . H8 H 0.3021 0.0066 0.7644 0.040 Uiso 1 1 calc R . . C9 C 0.2118(7) -0.0192(5) 0.8530(4) 0.0451(16) Uani 1 1 d . . . H9 H 0.2675 0.0331 0.8908 0.054 Uiso 1 1 calc R . . C10 C 0.1103(8) -0.0800(6) 0.8726(4) 0.057(2) Uani 1 1 d . . . H10 H 0.0973 -0.0696 0.9243 0.068 Uiso 1 1 calc R . . C11 C 0.0272(9) -0.1559(6) 0.8182(5) 0.062(2) Uani 1 1 d . . . H11 H -0.0425 -0.1975 0.8320 0.075 Uiso 1 1 calc R . . C12 C 0.0480(7) -0.1703(5) 0.7427(4) 0.0475(18) Uani 1 1 d . . . H12 H -0.0090 -0.2217 0.7045 0.057 Uiso 1 1 calc R . . C13 C 0.4717(6) -0.1581(4) 0.7735(3) 0.0311(13) Uani 1 1 d . . . C14 C 0.5730(7) -0.0857(5) 0.8241(4) 0.0404(15) Uani 1 1 d . . . H14 H 0.6355 -0.0462 0.8035 0.049 Uiso 1 1 calc R . . C15 C 0.5822(9) -0.0715(5) 0.9038(4) 0.056(2) Uani 1 1 d . . . H15 H 0.6490 -0.0207 0.9375 0.067 Uiso 1 1 calc R . . C16 C 0.4950(9) -0.1307(6) 0.9353(4) 0.056(2) Uani 1 1 d . . . H16 H 0.5032 -0.1215 0.9903 0.068 Uiso 1 1 calc R . . C17 C 0.3953(8) -0.2035(5) 0.8853(4) 0.0483(18) Uani 1 1 d . . . H17 H 0.3345 -0.2439 0.9062 0.058 Uiso 1 1 calc R . . C18 C 0.3844(7) -0.2171(5) 0.8057(4) 0.0401(15) Uani 1 1 d . . . H18 H 0.3165 -0.2674 0.7722 0.048 Uiso 1 1 calc R . . C19 C 0.4872(5) -0.2875(4) 0.6427(3) 0.0258(12) Uani 1 1 d . . . C20 C 0.6166(6) -0.2938(4) 0.6728(4) 0.0392(15) Uani 1 1 d . . . H20 H 0.6818 -0.2417 0.7059 0.047 Uiso 1 1 calc R . . C21 C 0.6479(7) -0.3780(5) 0.6532(5) 0.0491(18) Uani 1 1 d . . . H21 H 0.7358 -0.3828 0.6722 0.059 Uiso 1 1 calc R . . C22 C 0.5519(8) -0.4550(5) 0.6062(4) 0.0457(17) Uani 1 1 d . . . H22 H 0.5734 -0.5126 0.5947 0.055 Uiso 1 1 calc R . . C23 C 0.4281(7) -0.4476(4) 0.5771(4) 0.0389(15) Uani 1 1 d . . . H23 H 0.3630 -0.4997 0.5441 0.047 Uiso 1 1 calc R . . C24 C 0.3956(6) -0.3645(4) 0.5951(3) 0.0337(14) Uani 1 1 d . . . H24 H 0.3080 -0.3604 0.5741 0.040 Uiso 1 1 calc R . . C25 C 0.6812(4) 0.3702(3) 0.93454(19) 0.0268(12) Uani 0.50 1 d PG A 1 C26 C 0.8054(5) 0.3654(4) 0.9740(3) 0.041(2) Uani 0.50 1 d PG A 1 H26 H 0.8548 0.3307 0.9481 0.049 Uiso 0.50 1 calc PR A 1 C27 C 0.8574(5) 0.4112(5) 1.0514(3) 0.051(3) Uani 0.50 1 d PG A 1 H27 H 0.9423 0.4079 1.0784 0.062 Uiso 0.50 1 calc PR A 1 C28 C 0.7852(5) 0.4619(4) 1.0894(2) 0.046(2) Uani 0.50 1 d PG A 1 H28 H 0.8208 0.4932 1.1423 0.055 Uiso 0.50 1 calc PR A 1 C29 C 0.6610(5) 0.4668(4) 1.0499(3) 0.045(3) Uani 0.50 1 d PG A 1 H29 H 0.6116 0.5014 1.0759 0.054 Uiso 0.50 1 calc PR A 1 C30 C 0.6090(4) 0.4209(4) 0.9725(2) 0.039(3) Uani 0.50 1 d PG A 1 H30 H 0.5241 0.4242 0.9455 0.047 Uiso 0.50 1 calc PR A 1 C25A C 0.6802(4) 0.3759(3) 0.93128(19) 0.0268(12) Uani 0.50 1 d PG A 2 C26A C 0.8135(4) 0.4251(4) 0.9574(3) 0.041(2) Uani 0.50 1 d PG A 2 H26A H 0.8731 0.4224 0.9238 0.049 Uiso 0.50 1 calc PR A 2 C27A C 0.8598(4) 0.4784(4) 1.0328(3) 0.051(3) Uani 0.50 1 d PG A 2 H27A H 0.9509 0.5121 1.0506 0.062 Uiso 0.50 1 calc PR A 2 C28A C 0.7727(5) 0.4825(4) 1.0819(2) 0.046(2) Uani 0.50 1 d PG A 2 H28A H 0.8043 0.5189 1.1334 0.055 Uiso 0.50 1 calc PR A 2 C29A C 0.6393(4) 0.4332(5) 1.0558(2) 0.045(3) Uani 0.50 1 d PG A 2 H29A H 0.5798 0.4360 1.0894 0.054 Uiso 0.50 1 calc PR A 2 C30A C 0.5931(3) 0.3799(4) 0.9805(3) 0.039(3) Uani 0.50 1 d PG A 2 H30A H 0.5019 0.3462 0.9626 0.047 Uiso 0.50 1 calc PR A 2 C31 C 0.4812(6) 0.3558(4) 0.7933(3) 0.0333(14) Uani 1 1 d . A . C32 C 0.5118(7) 0.4460(5) 0.7802(4) 0.0425(16) Uani 1 1 d . . . H32 H 0.6025 0.4803 0.7901 0.051 Uiso 1 1 calc R A . C33 C 0.4119(8) 0.4861(6) 0.7528(4) 0.053(2) Uani 1 1 d . A . H33 H 0.4337 0.5483 0.7452 0.064 Uiso 1 1 calc R . . C34 C 0.2808(9) 0.4361(7) 0.7367(4) 0.064(3) Uani 1 1 d . . . H34 H 0.2120 0.4630 0.7163 0.077 Uiso 1 1 calc R A . C35 C 0.2495(7) 0.3488(7) 0.7499(5) 0.065(3) Uani 1 1 d . A . H35 H 0.1584 0.3156 0.7401 0.078 Uiso 1 1 calc R . . C36 C 0.3488(6) 0.3059(6) 0.7779(4) 0.0494(18) Uani 1 1 d . . . H36 H 0.3257 0.2440 0.7862 0.059 Uiso 1 1 calc R A . C37 C 0.8608(5) 0.4193(4) 0.6878(3) 0.0278(12) Uani 1 1 d . A . C38 C 0.8584(6) 0.4340(4) 0.6127(4) 0.0335(14) Uani 1 1 d . . . H38 H 0.8027 0.3885 0.5692 0.040 Uiso 1 1 calc R A . C39 C 0.9372(7) 0.5152(5) 0.6008(4) 0.0422(16) Uani 1 1 d . A . H39 H 0.9360 0.5247 0.5490 0.051 Uiso 1 1 calc R . . C40 C 1.0174(6) 0.5823(4) 0.6634(4) 0.0403(16) Uani 1 1 d . . . H40 H 1.0728 0.6371 0.6547 0.048 Uiso 1 1 calc R A . C41 C 1.0169(7) 0.5697(5) 0.7375(5) 0.0486(18) Uani 1 1 d . A . H41 H 1.0697 0.6168 0.7808 0.058 Uiso 1 1 calc R . . C42 C 0.9394(6) 0.4882(4) 0.7502(4) 0.0372(14) Uani 1 1 d . . . H42 H 0.9402 0.4797 0.8022 0.045 Uiso 1 1 calc R A . C43 C 0.8681(5) 0.2327(4) 0.7115(3) 0.0253(12) Uani 1 1 d . A . C44 C 0.9058(6) 0.1969(4) 0.6452(4) 0.0328(13) Uani 1 1 d . . . H44 H 0.8784 0.2154 0.5972 0.039 Uiso 1 1 calc R A . C45 C 0.9820(6) 0.1353(5) 0.6491(4) 0.0412(16) Uani 1 1 d . A . H45 H 1.0102 0.1135 0.6038 0.049 Uiso 1 1 calc R . . C46 C 1.0184(8) 0.1045(6) 0.7150(5) 0.063(2) Uani 1 1 d . . . H46 H 1.0679 0.0592 0.7155 0.076 Uiso 1 1 calc R A . C47 C 0.9827(9) 0.1396(6) 0.7822(5) 0.068(3) Uani 1 1 d . A . H47 H 1.0102 0.1198 0.8296 0.081 Uiso 1 1 calc R . . C48 C 0.9074(7) 0.2032(5) 0.7804(4) 0.0473(18) Uani 1 1 d . . . H48 H 0.8825 0.2267 0.8264 0.057 Uiso 1 1 calc R A . O1 O 0.797(3) 0.664(3) 0.873(3) 0.115(7) Uani 0.50 1 d P B 1 C50 C 0.704(2) 0.7097(16) 0.9055(15) 0.080(6) Uani 0.50 1 d P B 1 H50A H 0.6271 0.6636 0.9135 0.096 Uiso 0.50 1 calc PR B 1 H50B H 0.6706 0.7497 0.8712 0.096 Uiso 0.50 1 calc PR B 1 C51 C 0.791(4) 0.766(2) 0.9818(19) 0.107(9) Uani 0.50 1 d P B 1 H51A H 0.7395 0.7708 1.0225 0.129 Uiso 0.50 1 calc PR B 1 H51B H 0.8348 0.8294 0.9761 0.129 Uiso 0.50 1 calc PR B 1 C52 C 0.897(3) 0.709(2) 1.0021(19) 0.105(9) Uani 0.50 1 d P B 1 H52A H 0.9888 0.7503 1.0201 0.126 Uiso 0.50 1 calc PR B 1 H52B H 0.8771 0.6729 1.0425 0.126 Uiso 0.50 1 calc PR B 1 C53 C 0.879(3) 0.649(2) 0.9276(19) 0.095(9) Uani 0.50 1 d P B 1 H53A H 0.9662 0.6575 0.9134 0.114 Uiso 0.50 1 calc PR B 1 H53B H 0.8484 0.5841 0.9330 0.114 Uiso 0.50 1 calc PR B 1 C57 C 0.757(5) 0.671(5) 0.888(5) 0.115(7) Uani 0.50 1 d P C 2 H57A H 0.7307 0.7143 0.8546 0.139 Uiso 0.50 1 calc PR C 2 H57B H 0.7478 0.6107 0.8536 0.139 Uiso 0.50 1 calc PR C 2 C54 C 0.680(2) 0.6601(18) 0.9428(18) 0.097(7) Uani 0.50 1 d P C 2 H54A H 0.6649 0.5960 0.9525 0.117 Uiso 0.50 1 calc PR C 2 H54B H 0.5927 0.6720 0.9237 0.117 Uiso 0.50 1 calc PR C 2 C55 C 0.754(3) 0.727(2) 1.015(2) 0.114(11) Uani 0.50 1 d P C 2 H55A H 0.7662 0.6953 1.0597 0.136 Uiso 0.50 1 calc PR C 2 H55B H 0.7061 0.7747 1.0267 0.136 Uiso 0.50 1 calc PR C 2 C56 C 0.895(3) 0.774(3) 0.9987(18) 0.110(11) Uani 0.50 1 d P C 2 H56A H 0.8970 0.8351 0.9847 0.132 Uiso 0.50 1 calc PR C 2 H56B H 0.9687 0.7812 1.0448 0.132 Uiso 0.50 1 calc PR C 2 O2 O 0.904(2) 0.7123(19) 0.9379(19) 0.132(10) Uani 0.50 1 d P C 2 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 0.0420(3) 0.0263(2) 0.0320(3) 0.00098(19) 0.0050(2) 0.00117(19) Ag2 0.0365(3) 0.0357(3) 0.0290(3) 0.00003(19) 0.0092(2) 0.0076(2) Te1 0.02509(19) 0.02165(18) 0.0283(2) 0.00575(14) 0.00652(15) 0.00575(14) Te2 0.02263(19) 0.0265(2) 0.0298(2) 0.00391(15) 0.00552(15) 0.00398(14) Te3 0.0606(3) 0.0277(2) 0.0289(2) 0.00267(17) 0.0095(2) -0.00430(19) Te4 0.02187(18) 0.0270(2) 0.0251(2) 0.00213(15) 0.00105(14) 0.00607(14) P1 0.0210(7) 0.0216(7) 0.0260(8) 0.0043(6) 0.0065(6) 0.0065(5) P2 0.0223(7) 0.0227(7) 0.0245(8) 0.0040(6) 0.0046(6) 0.0077(5) P3 0.0227(7) 0.0246(7) 0.0213(7) -0.0008(6) 0.0058(6) 0.0001(6) P4 0.0196(7) 0.0232(7) 0.0220(7) 0.0010(5) 0.0047(5) 0.0046(5) N1 0.023(2) 0.022(2) 0.028(3) 0.0057(19) 0.0062(19) 0.0048(18) N2 0.024(2) 0.031(3) 0.023(3) -0.005(2) 0.008(2) 0.000(2) C1 0.020(3) 0.021(3) 0.030(3) 0.010(2) 0.007(2) 0.004(2) C2 0.021(3) 0.028(3) 0.032(3) 0.006(2) 0.005(2) 0.010(2) C3 0.039(3) 0.025(3) 0.028(3) 0.001(2) 0.000(3) 0.008(3) C4 0.021(3) 0.025(3) 0.032(3) 0.002(2) 0.003(2) -0.003(2) C5 0.021(3) 0.037(3) 0.053(4) 0.008(3) 0.007(3) 0.007(3) C6 0.029(3) 0.029(3) 0.045(4) -0.001(3) 0.010(3) 0.008(2) C7 0.029(3) 0.029(3) 0.031(3) 0.006(2) 0.009(2) 0.011(2) C8 0.034(3) 0.042(4) 0.026(3) 0.007(3) 0.009(3) 0.012(3) C9 0.050(4) 0.053(4) 0.029(4) 0.002(3) 0.009(3) 0.012(3) C10 0.071(5) 0.071(5) 0.034(4) 0.008(4) 0.032(4) 0.015(4) C11 0.078(6) 0.062(5) 0.051(5) 0.009(4) 0.045(5) 0.003(4) C12 0.048(4) 0.035(4) 0.056(5) -0.001(3) 0.024(4) -0.003(3) C13 0.034(3) 0.037(3) 0.029(3) 0.011(3) 0.009(3) 0.019(3) C14 0.051(4) 0.042(4) 0.025(3) 0.005(3) -0.002(3) 0.013(3) C15 0.091(6) 0.047(4) 0.021(3) 0.000(3) -0.001(4) 0.017(4) C16 0.081(6) 0.073(5) 0.023(4) 0.017(4) 0.014(4) 0.031(5) C17 0.070(5) 0.060(5) 0.030(4) 0.022(3) 0.023(4) 0.028(4) C18 0.043(4) 0.042(4) 0.041(4) 0.015(3) 0.011(3) 0.017(3) C19 0.030(3) 0.029(3) 0.023(3) 0.009(2) 0.008(2) 0.012(2) C20 0.033(3) 0.036(4) 0.049(4) 0.005(3) 0.008(3) 0.013(3) C21 0.039(4) 0.055(4) 0.070(5) 0.023(4) 0.020(4) 0.032(3) C22 0.067(5) 0.032(4) 0.050(4) 0.009(3) 0.026(4) 0.026(3) C23 0.054(4) 0.025(3) 0.038(4) 0.002(3) 0.011(3) 0.012(3) C24 0.044(4) 0.029(3) 0.030(3) 0.006(3) 0.005(3) 0.015(3) C25 0.029(3) 0.029(3) 0.021(3) 0.000(2) 0.008(2) 0.006(2) C26 0.036(5) 0.050(7) 0.031(5) -0.010(5) 0.004(4) 0.014(5) C27 0.047(5) 0.060(7) 0.032(6) -0.013(5) -0.004(4) 0.009(6) C28 0.053(5) 0.054(6) 0.024(4) -0.008(4) 0.002(3) 0.015(4) C29 0.048(5) 0.059(9) 0.030(4) -0.002(5) 0.012(4) 0.023(6) C30 0.038(5) 0.047(9) 0.033(5) -0.001(5) 0.012(4) 0.014(5) C25A 0.029(3) 0.029(3) 0.021(3) 0.000(2) 0.008(2) 0.006(2) C26A 0.036(5) 0.050(7) 0.031(5) -0.010(5) 0.004(4) 0.014(5) C27A 0.047(5) 0.060(7) 0.032(6) -0.013(5) -0.004(4) 0.009(6) C28A 0.053(5) 0.054(6) 0.024(4) -0.008(4) 0.002(3) 0.015(4) C29A 0.048(5) 0.059(9) 0.030(4) -0.002(5) 0.012(4) 0.023(6) C30A 0.038(5) 0.047(9) 0.033(5) -0.001(5) 0.012(4) 0.014(5) C31 0.026(3) 0.048(4) 0.021(3) -0.004(3) 0.006(2) 0.009(3) C32 0.044(4) 0.055(4) 0.041(4) 0.020(3) 0.017(3) 0.024(3) C33 0.069(5) 0.071(5) 0.039(4) 0.023(4) 0.021(4) 0.044(4) C34 0.075(6) 0.104(7) 0.024(4) 0.000(4) 0.002(4) 0.060(6) C35 0.027(4) 0.101(7) 0.050(5) -0.017(5) -0.007(3) 0.019(4) C36 0.026(3) 0.066(5) 0.045(4) -0.008(3) 0.006(3) 0.003(3) C37 0.026(3) 0.028(3) 0.030(3) 0.004(2) 0.006(2) 0.010(2) C38 0.044(4) 0.029(3) 0.032(3) 0.009(3) 0.018(3) 0.010(3) C39 0.051(4) 0.042(4) 0.047(4) 0.017(3) 0.027(3) 0.019(3) C40 0.041(4) 0.028(3) 0.057(5) 0.016(3) 0.021(3) 0.007(3) C41 0.042(4) 0.039(4) 0.055(5) 0.012(3) 0.002(3) -0.003(3) C42 0.031(3) 0.037(3) 0.035(4) 0.011(3) 0.001(3) -0.005(3) C43 0.024(3) 0.028(3) 0.022(3) 0.004(2) 0.004(2) 0.004(2) C44 0.029(3) 0.031(3) 0.033(3) -0.005(3) 0.009(3) 0.005(2) C45 0.034(3) 0.048(4) 0.045(4) 0.007(3) 0.007(3) 0.021(3) C46 0.073(5) 0.071(6) 0.062(5) 0.010(4) 0.012(4) 0.056(5) C47 0.090(6) 0.086(6) 0.050(5) 0.035(4) 0.012(4) 0.061(5) C48 0.056(4) 0.067(5) 0.032(4) 0.012(3) 0.016(3) 0.037(4) O1 0.07(2) 0.109(11) 0.16(2) -0.002(12) 0.027(15) 0.023(14) C50 0.089(15) 0.070(14) 0.096(18) 0.030(13) 0.034(14) 0.032(12) C51 0.12(3) 0.13(3) 0.10(2) 0.019(19) 0.04(2) 0.05(2) C52 0.12(2) 0.11(2) 0.074(19) 0.026(18) 0.003(16) 0.03(2) C53 0.057(16) 0.13(3) 0.09(2) 0.03(2) -0.007(13) 0.030(16) C57 0.07(2) 0.109(11) 0.16(2) -0.002(12) 0.027(15) 0.023(14) C54 0.079(15) 0.091(17) 0.14(2) 0.033(18) 0.031(16) 0.048(13) C55 0.14(3) 0.09(2) 0.13(3) 0.023(19) 0.07(2) 0.034(19) C56 0.11(2) 0.13(3) 0.076(19) -0.026(18) -0.010(16) 0.05(2) O2 0.085(14) 0.16(2) 0.13(2) 0.02(2) 0.051(14) -0.016(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 Te3 2.7918(10) . ? Ag1 Te4 2.8156(10) . ? Ag1 Te1 2.8804(14) . ? Ag1 Te2 2.8901(9) . ? Ag1 Ag2 3.2434(10) . ? Ag2 Te4 2.7642(10) . ? Ag2 Te1 2.8273(10) 2_656 ? Ag2 Te2 2.9275(12) 2_656 ? Ag2 Ag2 2.9919(15) 2_656 ? Te1 P1 2.4283(16) . ? Te1 Ag2 2.8273(10) 2_656 ? Te2 P2 2.4518(17) . ? Te2 Ag2 2.9275(12) 2_656 ? Te3 P3 2.3839(16) . ? Te4 P4 2.4341(18) . ? P1 N1 1.605(4) . ? P1 C1 1.805(5) . ? P1 C7 1.819(6) . ? P2 N1 1.603(5) . ? P2 C19 1.807(5) . ? P2 C13 1.816(6) . ? P3 N2 1.601(5) . ? P3 C25A 1.801(3) . ? P3 C31 1.816(6) . ? P3 C25 1.825(3) . ? P4 N2 1.588(5) . ? P4 C43 1.810(6) . ? P4 C37 1.819(6) . ? C1 C6 1.390(8) . ? C1 C2 1.391(8) . ? C2 C3 1.403(8) . ? C2 H2 0.9500 . ? C3 C4 1.346(8) . ? C3 H3 0.9500 . ? C4 C5 1.373(8) . ? C4 H4 0.9500 . ? C5 C6 1.393(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.382(8) . ? C7 C12 1.383(9) . ? C8 C9 1.384(9) . ? C8 H8 0.9500 . ? C9 C10 1.380(11) . ? C9 H9 0.9500 . ? C10 C11 1.383(11) . ? C10 H10 0.9500 . ? C11 C12 1.393(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.397(9) . ? C13 C14 1.401(9) . ? C14 C15 1.383(9) . ? C14 H14 0.9500 . ? C15 C16 1.389(12) . ? C15 H15 0.9500 . ? C16 C17 1.392(11) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.375(8) . ? C19 C20 1.402(8) . ? C20 C21 1.396(9) . ? C20 H20 0.9500 . ? C21 C22 1.390(11) . ? C21 H21 0.9500 . ? C22 C23 1.350(10) . ? C22 H22 0.9500 . ? C23 C24 1.382(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C25A C26A 1.3900 . ? C25A C30A 1.3901 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C31 C36 1.385(9) . ? C31 C32 1.389(9) . ? C32 C33 1.379(9) . ? C32 H32 0.9500 . ? C33 C34 1.373(12) . ? C33 H33 0.9500 . ? C34 C35 1.349(13) . ? C34 H34 0.9500 . ? C35 C36 1.405(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.380(8) . ? C37 C42 1.386(8) . ? C38 C39 1.385(9) . ? C38 H38 0.9500 . ? C39 C40 1.378(10) . ? C39 H39 0.9500 . ? C40 C41 1.359(10) . ? C40 H40 0.9500 . ? C41 C42 1.388(9) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.385(9) . ? C43 C44 1.388(8) . ? C44 C45 1.362(8) . ? C44 H44 0.9500 . ? C45 C46 1.344(11) . ? C45 H45 0.9500 . ? C46 C47 1.388(11) . ? C46 H46 0.9500 . ? C47 C48 1.378(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? O1 C53 1.25(6) . ? O1 C50 1.48(3) . ? C50 C51 1.50(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.58(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.44(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C57 C54 1.39(6) . ? C57 O2 1.57(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C54 C55 1.47(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.60(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 O2 1.35(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? 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 Te4 111.93(3) . . ? Te3 Ag1 Te1 124.08(3) . . ? Te4 Ag1 Te1 99.55(3) . . ? Te3 Ag1 Te2 111.01(3) . . ? Te4 Ag1 Te2 116.10(3) . . ? Te1 Ag1 Te2 93.11(3) . . ? Te3 Ag1 Ag2 150.35(2) . . ? Te4 Ag1 Ag2 53.72(3) . . ? Te1 Ag1 Ag2 85.43(3) . . ? Te2 Ag1 Ag2 65.49(3) . . ? Te4 Ag2 Te1 151.02(3) . 2_656 ? Te4 Ag2 Te2 100.38(4) . 2_656 ? Te1 Ag2 Te2 93.42(3) 2_656 2_656 ? Te4 Ag2 Ag2 117.43(3) . 2_656 ? Te1 Ag2 Ag2 91.29(3) 2_656 2_656 ? Te2 Ag2 Ag2 68.48(4) 2_656 2_656 ? Te4 Ag2 Ag1 55.20(2) . . ? Te1 Ag2 Ag1 139.50(3) 2_656 . ? Te2 Ag2 Ag1 113.78(3) 2_656 . ? Ag2 Ag2 Ag1 73.22(4) 2_656 . ? P1 Te1 Ag2 86.93(4) . 2_656 ? P1 Te1 Ag1 100.46(5) . . ? Ag2 Te1 Ag1 81.44(3) 2_656 . ? P2 Te2 Ag1 96.71(4) . . ? P2 Te2 Ag2 83.67(5) . 2_656 ? Ag1 Te2 Ag2 79.59(3) . 2_656 ? P3 Te3 Ag1 94.18(5) . . ? P4 Te4 Ag2 110.64(5) . . ? P4 Te4 Ag1 88.75(5) . . ? Ag2 Te4 Ag1 71.07(2) . . ? N1 P1 C1 107.7(2) . . ? N1 P1 C7 110.8(3) . . ? C1 P1 C7 104.4(3) . . ? N1 P1 Te1 116.17(18) . . ? C1 P1 Te1 104.47(18) . . ? C7 P1 Te1 112.24(19) . . ? N1 P2 C19 105.0(2) . . ? N1 P2 C13 109.6(3) . . ? C19 P2 C13 104.3(3) . . ? N1 P2 Te2 120.65(18) . . ? C19 P2 Te2 105.80(19) . . ? C13 P2 Te2 110.1(2) . . ? N2 P3 C25A 102.8(2) . . ? N2 P3 C31 109.3(3) . . ? C25A P3 C31 103.4(2) . . ? N2 P3 C25 104.2(2) . . ? C25A P3 C25 3.4 . . ? C31 P3 C25 105.7(2) . . ? N2 P3 Te3 117.01(18) . . ? C25A P3 Te3 109.80(18) . . ? C31 P3 Te3 113.2(2) . . ? C25 P3 Te3 106.46(18) . . ? N2 P4 C43 110.3(3) . . ? N2 P4 C37 104.1(3) . . ? C43 P4 C37 107.3(3) . . ? N2 P4 Te4 118.97(18) . . ? C43 P4 Te4 107.51(18) . . ? C37 P4 Te4 108.14(19) . . ? P2 N1 P1 132.4(3) . . ? P4 N2 P3 132.4(3) . . ? C6 C1 C2 119.7(5) . . ? C6 C1 P1 119.2(4) . . ? C2 C1 P1 121.0(4) . . ? C1 C2 C3 118.9(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.8(5) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 118.9(5) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 120.2(5) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 119.5(6) . . ? C8 C7 P1 119.9(4) . . ? C12 C7 P1 120.4(5) . . ? C7 C8 C9 120.4(6) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.6(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.1(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 118.7(7) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 120.8(7) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C18 C13 C14 118.6(6) . . ? C18 C13 P2 117.9(5) . . ? C14 C13 P2 123.6(5) . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.8(7) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 119.2(6) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.3(7) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 121.0(7) . . ? C17 C18 H18 119.5 . . ? C13 C18 H18 119.5 . . ? C24 C19 C20 118.9(5) . . ? C24 C19 P2 122.0(4) . . ? C20 C19 P2 119.1(4) . . ? C21 C20 C19 118.7(6) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C22 C21 C20 120.8(6) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C23 C22 C21 119.7(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 121.5(6) . . ? C19 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C30 120.0 . . ? C26 C25 P3 118.0(2) . . ? C30 C25 P3 122.0(2) . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C26A C25A C30A 120.0 . . ? C26A C25A P3 119.9(3) . . ? C30A C25A P3 120.1(3) . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C26A C27A C28A 120.0 . . ? C26A C27A H27A 120.0 . . ? C28A C27A H27A 120.0 . . ? C29A C28A C27A 120.0 . . ? C29A C28A H28A 120.0 . . ? C27A C28A H28A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30A 120.0 . . ? C25A C30A H30A 120.0 . . ? C36 C31 C32 119.3(6) . . ? C36 C31 P3 123.2(6) . . ? C32 C31 P3 117.5(5) . . ? C33 C32 C31 120.6(7) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 119.9(8) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.1(7) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 121.5(8) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C31 C36 C35 118.5(8) . . ? C31 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C38 C37 C42 118.8(6) . . ? C38 C37 P4 122.7(5) . . ? C42 C37 P4 118.5(5) . . ? C37 C38 C39 119.9(6) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.7(6) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C41 C40 C39 119.7(6) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 120.2(7) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.6(6) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C48 C43 C44 118.7(5) . . ? C48 C43 P4 120.0(4) . . ? C44 C43 P4 121.3(4) . . ? C45 C44 C43 120.0(6) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 122.0(7) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C46 C47 119.1(6) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C48 C47 C46 120.2(7) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C43 120.0(6) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C53 O1 C50 110(4) . . ? O1 C50 C51 102(3) . . ? O1 C50 H50A 111.4 . . ? C51 C50 H50A 111.4 . . ? O1 C50 H50B 111.4 . . ? C51 C50 H50B 111.4 . . ? H50A C50 H50B 109.3 . . ? C50 C51 C52 103(2) . . ? C50 C51 H51A 111.2 . . ? C52 C51 H51A 111.2 . . ? C50 C51 H51B 111.2 . . ? C52 C51 H51B 111.2 . . ? H51A C51 H51B 109.1 . . ? C53 C52 C51 101(2) . . ? C53 C52 H52A 111.5 . . ? C51 C52 H52A 111.5 . . ? C53 C52 H52B 111.5 . . ? C51 C52 H52B 111.5 . . ? H52A C52 H52B 109.3 . . ? O1 C53 C52 114(3) . . ? O1 C53 H53A 108.7 . . ? C52 C53 H53A 108.7 . . ? O1 C53 H53B 108.7 . . ? C52 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C54 C57 O2 104(5) . . ? C54 C57 H57A 110.9 . . ? O2 C57 H57A 110.9 . . ? C54 C57 H57B 110.9 . . ? O2 C57 H57B 110.9 . . ? H57A C57 H57B 108.9 . . ? C57 C54 C55 107(4) . . ? C57 C54 H54A 110.3 . . ? C55 C54 H54A 110.3 . . ? C57 C54 H54B 110.3 . . ? C55 C54 H54B 110.3 . . ? H54A C54 H54B 108.5 . . ? C54 C55 C56 106(2) . . ? C54 C55 H55A 110.6 . . ? C56 C55 H55A 110.6 . . ? C54 C55 H55B 110.6 . . ? C56 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? O2 C56 C55 103(3) . . ? O2 C56 H56A 111.2 . . ? C55 C56 H56A 111.2 . . ? O2 C56 H56B 111.2 . . ? C55 C56 H56B 111.2 . . ? H56A C56 H56B 109.1 . . ? C56 O2 C57 105(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.551 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.145 # Attachment 'Revisedcomplex6.cif' data_complex6 _database_code_depnum_ccdc_archive 'CCDC 612708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H168 Ag6 N6 P12 Te12' _chemical_formula_sum 'C72 H168 Ag6 N6 P12 Te12' _chemical_formula_weight 3668.18 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5139(5) _cell_length_b 14.7985(6) _cell_length_c 16.3057(9) _cell_angle_alpha 72.726(2) _cell_angle_beta 67.473(3) _cell_angle_gamma 69.256(3) _cell_volume 2972.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37511 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 4.053 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7375 _exptl_absorpt_correction_T_max 0.9233 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor, 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54940 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10470 _reflns_number_gt 6597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10470 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Ag1 Ag 0.71944(5) 0.13967(5) 0.24403(5) 0.03203(19) Uani 1 1 d . . . Ag2 Ag 0.71495(5) -0.12243(5) 0.46766(5) 0.02917(18) Uani 1 1 d . . . Ag3 Ag 0.40705(5) 0.18804(5) 0.34488(5) 0.03230(19) Uani 1 1 d . . . Te1 Te 0.55796(4) 0.24735(4) 0.36147(4) 0.02579(15) Uani 1 1 d . . . Te2 Te 0.84441(5) 0.22811(5) 0.09706(5) 0.04120(19) Uani 1 1 d . . . Te3 Te 0.72282(4) -0.05391(4) 0.29138(4) 0.02414(15) Uani 1 1 d . . . Te4 Te 0.83971(5) -0.29992(4) 0.51383(4) 0.03269(17) Uani 1 1 d . . . Te5 Te 0.28198(5) 0.26547(4) 0.23778(4) 0.02895(16) Uani 1 1 d . . . Te6 Te 0.43097(4) -0.01085(4) 0.42375(4) 0.02451(15) Uani 1 1 d . . . N1 N 0.6661(5) 0.4275(5) 0.1945(5) 0.0252(17) Uani 1 1 d . . . N2 N 0.9439(5) -0.2502(5) 0.2774(5) 0.0278(18) Uani 1 1 d . . . N3 N 0.3429(5) 0.0150(5) 0.2426(5) 0.0252(17) Uani 1 1 d . . . P1 P 0.55953(17) 0.40771(16) 0.25954(17) 0.0244(5) Uani 1 1 d . . . P2 P 0.78655(18) 0.38533(16) 0.14366(17) 0.0286(6) Uani 1 1 d . . . P3 P 0.90483(16) -0.14114(16) 0.22856(16) 0.0222(5) Uani 1 1 d . . . P4 P 0.92535(17) -0.33617(16) 0.36149(17) 0.0268(6) Uani 1 1 d . . . P5 P 0.33937(17) 0.11778(16) 0.17677(17) 0.0257(6) Uani 1 1 d . . . P6 P 0.34169(17) -0.04661(16) 0.34105(17) 0.0262(6) Uani 1 1 d . . . C1 C 0.5048(7) 0.4978(6) 0.3329(6) 0.031(2) Uani 1 1 d . . . H1 H 0.4987 0.5642 0.2929 0.037 Uiso 1 1 calc R . . C2 C 0.3939(6) 0.4954(7) 0.3968(7) 0.037(2) Uani 1 1 d . . . H2A H 0.3969 0.4321 0.4387 0.056 Uiso 1 1 calc R . . H2B H 0.3495 0.5039 0.3609 0.056 Uiso 1 1 calc R . . H2C H 0.3653 0.5487 0.4311 0.056 Uiso 1 1 calc R . . C3 C 0.5775(7) 0.4866(7) 0.3835(7) 0.042(3) Uani 1 1 d . . . H3A H 0.5503 0.5400 0.4176 0.063 Uiso 1 1 calc R . . H3B H 0.6460 0.4893 0.3404 0.063 Uiso 1 1 calc R . . H3C H 0.5835 0.4232 0.4254 0.063 Uiso 1 1 calc R . . C4 C 0.4725(7) 0.4354(6) 0.1936(7) 0.037(3) Uani 1 1 d . . . H4 H 0.4090 0.4141 0.2343 0.044 Uiso 1 1 calc R . . C5 C 0.5250(8) 0.3763(7) 0.1178(7) 0.043(3) Uani 1 1 d . . . H5A H 0.4749 0.3829 0.0883 0.065 Uiso 1 1 calc R . . H5B H 0.5511 0.3068 0.1429 0.065 Uiso 1 1 calc R . . H5C H 0.5830 0.4010 0.0734 0.065 Uiso 1 1 calc R . . C6 C 0.4386(8) 0.5450(7) 0.1547(8) 0.051(3) Uani 1 1 d . . . H6A H 0.4995 0.5706 0.1252 0.077 Uiso 1 1 calc R . . H6B H 0.3903 0.5803 0.2036 0.077 Uiso 1 1 calc R . . H6C H 0.4041 0.5542 0.1103 0.077 Uiso 1 1 calc R . . C7 C 0.8181(8) 0.4779(7) 0.0426(7) 0.044(3) Uani 1 1 d . . . H7 H 0.8941 0.4553 0.0112 0.053 Uiso 1 1 calc R . . C8 C 0.7968(8) 0.5788(7) 0.0668(8) 0.057(3) Uani 1 1 d . . . H8A H 0.8094 0.6279 0.0112 0.086 Uiso 1 1 calc R . . H8B H 0.8431 0.5728 0.1000 0.086 Uiso 1 1 calc R . . H8C H 0.7246 0.5992 0.1045 0.086 Uiso 1 1 calc R . . C9 C 0.7621(9) 0.4889(7) -0.0237(7) 0.057(3) Uani 1 1 d . . . H9A H 0.6881 0.5205 0.0013 0.086 Uiso 1 1 calc R . . H9B H 0.7710 0.4238 -0.0337 0.086 Uiso 1 1 calc R . . H9C H 0.7913 0.5294 -0.0812 0.086 Uiso 1 1 calc R . . C10 C 0.8629(7) 0.3808(6) 0.2118(7) 0.034(2) Uani 1 1 d . . . H10 H 0.8319 0.4438 0.2352 0.041 Uiso 1 1 calc R . . C11 C 0.8553(8) 0.2986(7) 0.2944(7) 0.041(3) Uani 1 1 d . . . H11A H 0.8817 0.2351 0.2749 0.062 Uiso 1 1 calc R . . H11B H 0.7827 0.3075 0.3323 0.062 Uiso 1 1 calc R . . H11C H 0.8966 0.3003 0.3291 0.062 Uiso 1 1 calc R . . C12 C 0.9770(7) 0.3769(7) 0.1584(8) 0.054(3) Uani 1 1 d . . . H12A H 1.0160 0.3618 0.2006 0.082 Uiso 1 1 calc R . . H12B H 0.9815 0.4407 0.1190 0.082 Uiso 1 1 calc R . . H12C H 1.0064 0.3256 0.1217 0.082 Uiso 1 1 calc R . . C13 C 0.9893(6) -0.0694(6) 0.2221(6) 0.027(2) Uani 1 1 d . . . H13 H 0.9679 -0.0020 0.1868 0.032 Uiso 1 1 calc R . . C14 C 0.9762(7) -0.0603(7) 0.3156(7) 0.044(3) Uani 1 1 d . . . H14A H 0.9876 -0.1258 0.3536 0.066 Uiso 1 1 calc R . . H14B H 0.9059 -0.0204 0.3418 0.066 Uiso 1 1 calc R . . H14C H 1.0268 -0.0285 0.3124 0.066 Uiso 1 1 calc R . . C15 C 1.1038(6) -0.1182(6) 0.1730(6) 0.031(2) Uani 1 1 d . . . H15A H 1.1484 -0.0829 0.1752 0.046 Uiso 1 1 calc R . . H15B H 1.1120 -0.1155 0.1099 0.046 Uiso 1 1 calc R . . H15C H 1.1234 -0.1869 0.2029 0.046 Uiso 1 1 calc R . . C16 C 0.9237(7) -0.1464(6) 0.1127(6) 0.028(2) Uani 1 1 d . . . H16 H 1.0000 -0.1719 0.0838 0.033 Uiso 1 1 calc R . . C17 C 0.8732(7) -0.2179(6) 0.1082(7) 0.038(3) Uani 1 1 d . . . H17A H 0.7981 -0.1963 0.1370 0.058 Uiso 1 1 calc R . . H17B H 0.9013 -0.2836 0.1398 0.058 Uiso 1 1 calc R . . H17C H 0.8876 -0.2200 0.0448 0.058 Uiso 1 1 calc R . . C18 C 0.8890(7) -0.0436(7) 0.0569(6) 0.036(2) Uani 1 1 d . . . H18A H 0.9176 -0.0467 -0.0076 0.055 Uiso 1 1 calc R . . H18B H 0.9143 0.0032 0.0685 0.055 Uiso 1 1 calc R . . H18C H 0.8132 -0.0219 0.0743 0.055 Uiso 1 1 calc R . . C19 C 1.0541(7) -0.4176(6) 0.3606(7) 0.034(2) Uani 1 1 d . . . H19 H 1.0459 -0.4731 0.4133 0.041 Uiso 1 1 calc R . . C20 C 1.1087(8) -0.4605(7) 0.2739(8) 0.064(4) Uani 1 1 d . . . H20A H 1.1143 -0.4069 0.2213 0.095 Uiso 1 1 calc R . . H20B H 1.0686 -0.4998 0.2708 0.095 Uiso 1 1 calc R . . H20C H 1.1783 -0.5024 0.2741 0.095 Uiso 1 1 calc R . . C21 C 1.1194(8) -0.3624(8) 0.3707(8) 0.055(3) Uani 1 1 d . . . H21A H 1.1854 -0.4086 0.3766 0.082 Uiso 1 1 calc R . . H21B H 1.0819 -0.3326 0.4247 0.082 Uiso 1 1 calc R . . H21C H 1.1329 -0.3109 0.3172 0.082 Uiso 1 1 calc R . . C22 C 0.8574(7) -0.4077(7) 0.3431(7) 0.040(3) Uani 1 1 d . . . H22 H 0.8955 -0.4228 0.2809 0.048 Uiso 1 1 calc R . . C23 C 0.8588(8) -0.5064(6) 0.4080(8) 0.051(3) Uani 1 1 d . . . H23A H 0.8257 -0.4952 0.4704 0.076 Uiso 1 1 calc R . . H23B H 0.9307 -0.5464 0.4003 0.076 Uiso 1 1 calc R . . H23C H 0.8209 -0.5409 0.3951 0.076 Uiso 1 1 calc R . . C25 C 0.7477(7) -0.3466(7) 0.3434(7) 0.045(3) Uani 1 1 d . . . H25A H 0.7173 -0.3815 0.3224 0.067 Uiso 1 1 calc R . . H25B H 0.7501 -0.2829 0.3031 0.067 Uiso 1 1 calc R . . H25C H 0.7052 -0.3361 0.4049 0.067 Uiso 1 1 calc R . . C26 C 0.2512(7) 0.1327(7) 0.1154(7) 0.037(3) Uani 1 1 d . . . H26 H 0.2428 0.1996 0.0762 0.045 Uiso 1 1 calc R . . C27 C 0.2949(7) 0.0557(7) 0.0548(7) 0.042(3) Uani 1 1 d . . . H27A H 0.3131 -0.0101 0.0909 0.064 Uiso 1 1 calc R . . H27B H 0.3569 0.0684 0.0061 0.064 Uiso 1 1 calc R . . H27C H 0.2425 0.0596 0.0289 0.064 Uiso 1 1 calc R . . C28 C 0.1440(7) 0.1253(7) 0.1831(7) 0.042(3) Uani 1 1 d . . . H28A H 0.0966 0.1344 0.1499 0.062 Uiso 1 1 calc R . . H28B H 0.1162 0.1764 0.2197 0.062 Uiso 1 1 calc R . . H28C H 0.1511 0.0604 0.2225 0.062 Uiso 1 1 calc R . . C29 C 0.4669(7) 0.1088(7) 0.0904(6) 0.032(2) Uani 1 1 d . . . H29 H 0.4838 0.0499 0.0639 0.039 Uiso 1 1 calc R . . C30 C 0.5532(7) 0.0913(7) 0.1318(7) 0.044(3) Uani 1 1 d . . . H30A H 0.6198 0.0883 0.0837 0.066 Uiso 1 1 calc R . . H30B H 0.5579 0.0291 0.1754 0.066 Uiso 1 1 calc R . . H30C H 0.5366 0.1454 0.1626 0.066 Uiso 1 1 calc R . . C31 C 0.4675(7) 0.1979(7) 0.0127(7) 0.042(3) Uani 1 1 d . . . H31A H 0.4494 0.2576 0.0364 0.063 Uiso 1 1 calc R . . H31B H 0.4168 0.2040 -0.0160 0.063 Uiso 1 1 calc R . . H31C H 0.5368 0.1889 -0.0320 0.063 Uiso 1 1 calc R . . C32 C 0.2078(6) -0.0466(6) 0.4115(7) 0.035(2) Uani 1 1 d . . . H32 H 0.1775 -0.0678 0.3770 0.042 Uiso 1 1 calc R . . C33 C 0.2036(7) -0.1220(7) 0.5020(7) 0.047(3) Uani 1 1 d . . . H33A H 0.2379 -0.1067 0.5355 0.071 Uiso 1 1 calc R . . H33B H 0.2392 -0.1885 0.4890 0.071 Uiso 1 1 calc R . . H33C H 0.1312 -0.1182 0.5382 0.071 Uiso 1 1 calc R . . C34 C 0.1400(7) 0.0550(6) 0.4297(7) 0.039(3) Uani 1 1 d . . . H34A H 0.0669 0.0568 0.4472 0.058 Uiso 1 1 calc R . . H34B H 0.1567 0.1042 0.3749 0.058 Uiso 1 1 calc R . . H34C H 0.1527 0.0695 0.4786 0.058 Uiso 1 1 calc R . . C35 C 0.4092(7) -0.1741(6) 0.3242(7) 0.036(3) Uani 1 1 d . . . H35 H 0.4134 -0.2154 0.3843 0.043 Uiso 1 1 calc R . . C36 C 0.3488(8) -0.2136(7) 0.2915(8) 0.053(3) Uani 1 1 d . . . H36A H 0.3351 -0.1693 0.2368 0.080 Uiso 1 1 calc R . . H36B H 0.2829 -0.2178 0.3386 0.080 Uiso 1 1 calc R . . H36C H 0.3894 -0.2791 0.2778 0.080 Uiso 1 1 calc R . . C37 C 0.5200(7) -0.1823(7) 0.2609(8) 0.048(3) Uani 1 1 d . . . H37A H 0.5572 -0.2517 0.2593 0.072 Uiso 1 1 calc R . . H37B H 0.5553 -0.1533 0.2828 0.072 Uiso 1 1 calc R . . H37C H 0.5185 -0.1470 0.1999 0.072 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 Ag1 0.0351(4) 0.0230(4) 0.0344(5) -0.0051(3) -0.0093(4) -0.0057(3) Ag2 0.0294(4) 0.0262(4) 0.0254(4) -0.0047(3) -0.0062(3) -0.0026(3) Ag3 0.0417(4) 0.0314(4) 0.0298(5) -0.0008(3) -0.0145(4) -0.0172(3) Te1 0.0271(3) 0.0221(3) 0.0274(4) -0.0017(3) -0.0086(3) -0.0081(3) Te2 0.0453(4) 0.0293(4) 0.0351(4) -0.0119(3) 0.0054(3) -0.0089(3) Te3 0.0226(3) 0.0205(3) 0.0251(4) -0.0028(3) -0.0071(3) -0.0025(2) Te4 0.0361(4) 0.0272(3) 0.0239(4) -0.0032(3) -0.0077(3) 0.0009(3) Te5 0.0361(3) 0.0221(3) 0.0297(4) -0.0057(3) -0.0130(3) -0.0053(3) Te6 0.0237(3) 0.0242(3) 0.0263(4) -0.0057(3) -0.0102(3) -0.0040(2) N1 0.027(4) 0.017(4) 0.032(5) -0.010(3) -0.004(4) -0.006(3) N2 0.018(4) 0.026(4) 0.030(5) -0.001(4) -0.004(4) -0.004(3) N3 0.035(4) 0.020(4) 0.021(5) -0.004(3) -0.010(4) -0.006(3) P1 0.0255(12) 0.0186(12) 0.0293(15) -0.0036(11) -0.0090(11) -0.0066(10) P2 0.0299(13) 0.0229(13) 0.0259(15) -0.0019(11) -0.0030(12) -0.0075(10) P3 0.0203(12) 0.0212(12) 0.0234(14) -0.0022(10) -0.0075(11) -0.0045(10) P4 0.0271(13) 0.0204(12) 0.0267(15) -0.0025(11) -0.0078(11) -0.0015(10) P5 0.0288(13) 0.0244(13) 0.0264(15) -0.0078(11) -0.0112(11) -0.0049(10) P6 0.0268(12) 0.0225(12) 0.0321(16) -0.0050(11) -0.0134(12) -0.0054(10) C1 0.036(5) 0.019(5) 0.028(6) -0.008(4) 0.005(5) -0.010(4) C2 0.030(5) 0.039(6) 0.035(7) -0.010(5) -0.007(5) -0.002(4) C3 0.047(6) 0.056(7) 0.036(7) -0.029(6) -0.004(5) -0.020(5) C4 0.033(5) 0.033(6) 0.044(7) 0.001(5) -0.022(5) -0.005(4) C5 0.064(7) 0.047(6) 0.033(7) -0.002(5) -0.027(6) -0.023(6) C6 0.048(6) 0.037(6) 0.067(9) -0.008(6) -0.031(6) 0.003(5) C7 0.042(6) 0.036(6) 0.035(7) 0.005(5) 0.006(5) -0.018(5) C8 0.058(7) 0.029(6) 0.070(9) -0.005(6) 0.001(7) -0.020(5) C9 0.085(9) 0.041(7) 0.037(8) 0.010(5) -0.018(7) -0.023(6) C10 0.033(5) 0.028(5) 0.040(7) -0.010(5) -0.004(5) -0.011(4) C11 0.056(7) 0.035(6) 0.035(7) 0.004(5) -0.020(6) -0.017(5) C12 0.036(6) 0.044(7) 0.076(9) 0.001(6) -0.014(6) -0.017(5) C13 0.030(5) 0.028(5) 0.020(6) -0.001(4) -0.006(4) -0.010(4) C14 0.043(6) 0.060(7) 0.049(8) -0.016(6) -0.015(6) -0.031(5) C15 0.021(5) 0.034(5) 0.037(6) -0.006(5) -0.010(5) -0.005(4) C16 0.030(5) 0.022(5) 0.027(6) -0.004(4) -0.012(5) 0.001(4) C17 0.061(7) 0.033(6) 0.027(6) -0.006(5) -0.014(5) -0.017(5) C18 0.039(6) 0.046(6) 0.027(6) -0.010(5) -0.009(5) -0.014(5) C19 0.035(5) 0.016(5) 0.032(6) 0.009(4) -0.009(5) 0.002(4) C20 0.050(7) 0.029(6) 0.067(9) -0.005(6) 0.006(6) 0.011(5) C21 0.041(6) 0.058(7) 0.049(8) 0.003(6) -0.018(6) -0.001(6) C22 0.047(6) 0.030(5) 0.043(7) -0.006(5) -0.011(5) -0.015(5) C23 0.062(7) 0.029(6) 0.060(9) -0.002(5) -0.023(7) -0.012(5) C25 0.054(7) 0.036(6) 0.053(8) 0.013(5) -0.032(6) -0.023(5) C26 0.042(6) 0.028(5) 0.050(7) -0.015(5) -0.024(6) -0.003(5) C27 0.045(6) 0.047(6) 0.045(7) -0.010(5) -0.026(6) -0.012(5) C28 0.040(6) 0.030(6) 0.059(8) -0.013(5) -0.030(6) 0.005(5) C29 0.037(5) 0.036(6) 0.033(6) -0.009(5) -0.014(5) -0.014(4) C30 0.044(6) 0.044(6) 0.056(8) -0.022(6) -0.029(6) 0.000(5) C31 0.034(6) 0.059(7) 0.035(7) -0.013(5) 0.000(5) -0.021(5) C32 0.028(5) 0.031(5) 0.050(7) -0.005(5) -0.015(5) -0.012(4) C33 0.041(6) 0.043(6) 0.050(8) 0.001(6) -0.009(6) -0.018(5) C34 0.030(5) 0.043(6) 0.045(7) -0.012(5) -0.006(5) -0.015(5) C35 0.045(6) 0.020(5) 0.051(7) -0.003(5) -0.035(6) 0.000(4) C36 0.065(7) 0.032(6) 0.084(10) -0.024(6) -0.040(7) -0.009(5) C37 0.041(6) 0.040(6) 0.069(9) -0.029(6) -0.020(6) 0.001(5) _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 Te2 2.6897(15) . ? Ag1 Te3 2.7241(11) . ? Ag1 Te1 2.7253(15) . ? Ag2 Te4 2.6917(13) . ? Ag2 Te3 2.7208(12) . ? Ag2 Te6 2.7844(15) 2_656 ? Ag2 Ag3 2.9546(15) 2_656 ? Ag3 Te5 2.7249(12) . ? Ag3 Te1 2.7563(10) . ? Ag3 Te6 2.7943(12) . ? Ag3 Ag2 2.9546(15) 2_656 ? Te1 P1 2.462(2) . ? Te2 P2 2.423(3) . ? Te3 P3 2.448(2) . ? Te4 P4 2.440(3) . ? Te5 P5 2.414(2) . ? Te6 P6 2.455(2) . ? Te6 Ag2 2.7844(15) 2_656 ? N1 P1 1.575(7) . ? N1 P2 1.599(7) . ? N2 P3 1.579(7) . ? N2 P4 1.580(7) . ? N3 P5 1.576(7) . ? N3 P6 1.590(7) . ? P1 C1 1.818(9) . ? P1 C4 1.826(9) . ? P2 C10 1.820(9) . ? P2 C7 1.824(10) . ? P3 C16 1.824(9) . ? P3 C13 1.843(9) . ? P4 C22 1.827(9) . ? P4 C19 1.827(8) . ? P5 C26 1.827(9) . ? P5 C29 1.835(10) . ? P6 C35 1.840(9) . ? P6 C32 1.840(9) . ? C1 C3 1.512(12) . ? C1 C2 1.552(12) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.524(13) . ? C4 C6 1.529(12) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.526(14) . ? C7 C8 1.552(13) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.521(12) . ? C10 C12 1.537(12) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.504(12) . ? C13 C15 1.549(11) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.516(12) . ? C16 C18 1.544(11) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.529(13) . ? C19 C20 1.534(14) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C25 1.527(12) . ? C22 C23 1.527(12) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.533(12) . ? C26 C28 1.544(13) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.533(12) . ? C29 C30 1.552(11) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.519(12) . ? C32 C33 1.558(13) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.518(12) . ? C35 C37 1.527(13) . ? C35 H35 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? 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 Te2 Ag1 Te3 127.87(4) . . ? Te2 Ag1 Te1 120.54(4) . . ? Te3 Ag1 Te1 111.47(4) . . ? Te4 Ag2 Te3 119.16(5) . . ? Te4 Ag2 Te6 129.53(4) . 2_656 ? Te3 Ag2 Te6 111.31(4) . 2_656 ? Te4 Ag2 Ag3 77.82(5) . 2_656 ? Te3 Ag2 Ag3 147.97(3) . 2_656 ? Te6 Ag2 Ag3 58.18(4) 2_656 2_656 ? Te5 Ag3 Te1 133.13(4) . . ? Te5 Ag3 Te6 116.34(4) . . ? Te1 Ag3 Te6 108.44(4) . . ? Te5 Ag3 Ag2 109.81(4) . 2_656 ? Te1 Ag3 Ag2 104.99(4) . 2_656 ? Te6 Ag3 Ag2 57.86(4) . 2_656 ? P1 Te1 Ag1 95.65(7) . . ? P1 Te1 Ag3 106.23(6) . . ? Ag1 Te1 Ag3 95.48(4) . . ? P2 Te2 Ag1 96.57(7) . . ? P3 Te3 Ag2 95.80(7) . . ? P3 Te3 Ag1 104.52(7) . . ? Ag2 Te3 Ag1 110.20(4) . . ? P4 Te4 Ag2 96.49(7) . . ? P5 Te5 Ag3 93.43(6) . . ? P6 Te6 Ag2 107.44(6) . 2_656 ? P6 Te6 Ag3 96.85(6) . . ? Ag2 Te6 Ag3 63.96(4) 2_656 . ? P1 N1 P2 149.2(5) . . ? P3 N2 P4 149.5(5) . . ? P5 N3 P6 147.4(5) . . ? N1 P1 C1 105.1(4) . . ? N1 P1 C4 109.2(4) . . ? C1 P1 C4 107.1(4) . . ? N1 P1 Te1 119.5(3) . . ? C1 P1 Te1 105.6(3) . . ? C4 P1 Te1 109.6(3) . . ? N1 P2 C10 109.6(4) . . ? N1 P2 C7 105.5(4) . . ? C10 P2 C7 105.9(5) . . ? N1 P2 Te2 118.7(3) . . ? C10 P2 Te2 108.6(3) . . ? C7 P2 Te2 107.9(4) . . ? N2 P3 C16 106.9(4) . . ? N2 P3 C13 108.8(4) . . ? C16 P3 C13 106.8(4) . . ? N2 P3 Te3 117.2(3) . . ? C16 P3 Te3 106.8(3) . . ? C13 P3 Te3 109.9(3) . . ? N2 P4 C22 109.0(4) . . ? N2 P4 C19 105.7(4) . . ? C22 P4 C19 106.4(4) . . ? N2 P4 Te4 120.2(3) . . ? C22 P4 Te4 108.7(4) . . ? C19 P4 Te4 105.9(3) . . ? N3 P5 C26 106.3(4) . . ? N3 P5 C29 107.9(4) . . ? C26 P5 C29 104.8(4) . . ? N3 P5 Te5 119.7(3) . . ? C26 P5 Te5 106.5(3) . . ? C29 P5 Te5 110.6(3) . . ? N3 P6 C35 104.6(4) . . ? N3 P6 C32 109.8(4) . . ? C35 P6 C32 105.9(4) . . ? N3 P6 Te6 119.3(3) . . ? C35 P6 Te6 105.5(3) . . ? C32 P6 Te6 110.5(3) . . ? C3 C1 C2 112.5(8) . . ? C3 C1 P1 110.7(6) . . ? C2 C1 P1 112.4(6) . . ? C3 C1 H1 107.0 . . ? C2 C1 H1 107.0 . . ? P1 C1 H1 107.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 110.2(8) . . ? C5 C4 P1 109.3(6) . . ? C6 C4 P1 112.9(7) . . ? C5 C4 H4 108.1 . . ? C6 C4 H4 108.1 . . ? P1 C4 H4 108.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 110.7(8) . . ? C9 C7 P2 112.5(7) . . ? C8 C7 P2 111.6(8) . . ? C9 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? P2 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 110.3(8) . . ? C11 C10 P2 112.9(6) . . ? C12 C10 P2 114.1(7) . . ? C11 C10 H10 106.3 . . ? C12 C10 H10 106.3 . . ? P2 C10 H10 106.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.0(7) . . ? C14 C13 P3 109.8(6) . . ? C15 C13 P3 110.4(6) . . ? C14 C13 H13 108.5 . . ? C15 C13 H13 108.5 . . ? P3 C13 H13 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 111.5(7) . . ? C17 C16 P3 112.4(6) . . ? C18 C16 P3 112.1(6) . . ? C17 C16 H16 106.8 . . ? C18 C16 H16 106.8 . . ? P3 C16 H16 106.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 110.5(8) . . ? C21 C19 P4 110.4(6) . . ? C20 C19 P4 110.9(7) . . ? C21 C19 H19 108.3 . . ? C20 C19 H19 108.3 . . ? P4 C19 H19 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 112.2(8) . . ? C25 C22 P4 110.9(7) . . ? C23 C22 P4 113.4(7) . . ? C25 C22 H22 106.6 . . ? C23 C22 H22 106.6 . . ? P4 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C28 110.6(8) . . ? C27 C26 P5 111.1(6) . . ? C28 C26 P5 109.7(7) . . ? C27 C26 H26 108.5 . . ? C28 C26 H26 108.5 . . ? P5 C26 H26 108.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 110.8(8) . . ? C31 C29 P5 112.7(6) . . ? C30 C29 P5 111.8(7) . . ? C31 C29 H29 107.0 . . ? C30 C29 H29 107.0 . . ? P5 C29 H29 107.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 110.5(8) . . ? C34 C32 P6 112.7(6) . . ? C33 C32 P6 112.0(6) . . ? C34 C32 H32 107.1 . . ? C33 C32 H32 107.1 . . ? P6 C32 H32 107.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 111.9(9) . . ? C36 C35 P6 111.2(6) . . ? C37 C35 P6 110.9(7) . . ? C36 C35 H35 107.5 . . ? C37 C35 H35 107.5 . . ? P6 C35 H35 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.897 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.203 # Attachment 'Revisedcomplex7.cif' data_complex7 _database_code_depnum_ccdc_archive 'CCDC 612709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H43 Au N P3 Te2' _chemical_formula_sum 'C30 H43 Au N P3 Te2' _chemical_formula_weight 962.73 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6560(2) _cell_length_b 43.2277(8) _cell_length_c 9.9070(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.363(2) _cell_angle_gamma 90.00 _cell_volume 3403.06(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21882 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 6.164 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4791 _exptl_absorpt_correction_T_max 0.7906 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor, 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33665 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5774 _reflns_number_gt 4990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0796P)^2^+4.4751P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5774 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.02578(3) 0.141919(6) 0.22960(3) 0.03052(12) Uani 1 1 d . . . Te2 Te 0.14114(6) 0.137717(10) 0.51700(5) 0.03419(15) Uani 1 1 d . . . Te3 Te -0.18990(5) 0.092357(10) 0.08286(4) 0.03371(15) Uani 1 1 d . . . N1 N -0.0117(6) 0.06161(12) 0.4419(5) 0.0262(11) Uani 1 1 d . . . P1 P -0.04989(19) 0.05443(4) 0.27416(17) 0.0244(4) Uani 1 1 d . . . P2 P 0.0200(2) 0.08943(4) 0.55648(17) 0.0261(4) Uani 1 1 d . . . P3 P 0.00113(19) 0.18501(4) 0.10298(16) 0.0239(3) Uani 1 1 d . . . C1 C -0.1806(8) 0.01925(14) 0.2280(7) 0.0289(14) Uani 1 1 d . . . H1 H -0.1214 0.0033 0.3040 0.035 Uiso 1 1 calc R . . C2 C -0.3506(8) 0.02567(17) 0.2363(8) 0.0423(18) Uani 1 1 d . . . H2A H -0.4138 0.0406 0.1601 0.063 Uiso 1 1 calc R . . H2B H -0.3321 0.0341 0.3333 0.063 Uiso 1 1 calc R . . H2C H -0.4147 0.0064 0.2208 0.063 Uiso 1 1 calc R . . C3 C -0.2052(10) 0.00567(18) 0.0766(8) 0.048(2) Uani 1 1 d . . . H3A H -0.2735 -0.0132 0.0585 0.072 Uiso 1 1 calc R . . H3B H -0.0952 0.0007 0.0756 0.072 Uiso 1 1 calc R . . H3C H -0.2624 0.0209 -0.0004 0.072 Uiso 1 1 calc R . . C4 C 0.1447(8) 0.04302(15) 0.2522(8) 0.0343(15) Uani 1 1 d . . . H4 H 0.1137 0.0377 0.1464 0.041 Uiso 1 1 calc R . . C5 C 0.2709(8) 0.07000(18) 0.2914(8) 0.0427(18) Uani 1 1 d . . . H5A H 0.2984 0.0764 0.3932 0.064 Uiso 1 1 calc R . . H5B H 0.2210 0.0874 0.2251 0.064 Uiso 1 1 calc R . . H5C H 0.3737 0.0633 0.2808 0.064 Uiso 1 1 calc R . . C6 C 0.2243(10) 0.01410(18) 0.3444(10) 0.053(2) Uani 1 1 d . . . H6A H 0.3315 0.0095 0.3369 0.079 Uiso 1 1 calc R . . H6B H 0.1480 -0.0035 0.3075 0.079 Uiso 1 1 calc R . . H6C H 0.2441 0.0179 0.4475 0.079 Uiso 1 1 calc R . . C7 C -0.1743(8) 0.09945(16) 0.5801(7) 0.0343(16) Uani 1 1 d . . . H7 H -0.1471 0.1167 0.6529 0.041 Uiso 1 1 calc R . . C8 C -0.2399(10) 0.07205(18) 0.6424(9) 0.0473(19) Uani 1 1 d . . . H8A H -0.3472 0.0777 0.6472 0.071 Uiso 1 1 calc R . . H8B H -0.1577 0.0670 0.7413 0.071 Uiso 1 1 calc R . . H8C H -0.2565 0.0540 0.5782 0.071 Uiso 1 1 calc R . . C9 C -0.3100(8) 0.11116(18) 0.4348(8) 0.0396(17) Uani 1 1 d . . . H9A H -0.3383 0.0947 0.3607 0.059 Uiso 1 1 calc R . . H9B H -0.2673 0.1292 0.4004 0.059 Uiso 1 1 calc R . . H9C H -0.4109 0.1170 0.4507 0.059 Uiso 1 1 calc R . . C10 C 0.1661(9) 0.07393(16) 0.7352(7) 0.0366(17) Uani 1 1 d . . . H10 H 0.1168 0.0542 0.7534 0.044 Uiso 1 1 calc R . . C11 C 0.3355(9) 0.06608(19) 0.7293(8) 0.0462(19) Uani 1 1 d . . . H11A H 0.3850 0.0849 0.7077 0.069 Uiso 1 1 calc R . . H11B H 0.3187 0.0507 0.6520 0.069 Uiso 1 1 calc R . . H11C H 0.4113 0.0576 0.8243 0.069 Uiso 1 1 calc R . . C12 C 0.1888(10) 0.09608(18) 0.8636(8) 0.049(2) Uani 1 1 d . . . H12A H 0.2653 0.0867 0.9561 0.073 Uiso 1 1 calc R . . H12B H 0.0794 0.0999 0.8682 0.073 Uiso 1 1 calc R . . H12C H 0.2362 0.1157 0.8482 0.073 Uiso 1 1 calc R . . C13 C 0.2216(7) 0.18822(14) 0.1321(6) 0.0264(14) Uani 1 1 d . . . C14 C 0.2974(8) 0.16150(16) 0.1085(7) 0.0344(15) Uani 1 1 d . . . H14 H 0.2329 0.1432 0.0756 0.041 Uiso 1 1 calc R . . C15 C 0.4659(8) 0.16155(18) 0.1325(8) 0.0396(17) Uani 1 1 d . . . H15 H 0.5167 0.1432 0.1160 0.047 Uiso 1 1 calc R . . C16 C 0.5606(8) 0.18793(17) 0.1802(7) 0.0400(17) Uani 1 1 d . . . H16 H 0.6760 0.1879 0.1951 0.048 Uiso 1 1 calc R . . C17 C 0.4880(8) 0.21428(18) 0.2062(7) 0.0362(16) Uani 1 1 d . . . H17 H 0.5543 0.2324 0.2412 0.043 Uiso 1 1 calc R . . C18 C 0.3195(8) 0.21468(15) 0.1819(7) 0.0324(15) Uani 1 1 d . . . H18 H 0.2702 0.2331 0.1993 0.039 Uiso 1 1 calc R . . C19 C -0.0550(7) 0.22253(15) 0.1552(7) 0.0266(14) Uani 1 1 d . . . C20 C -0.0408(9) 0.22683(16) 0.2973(7) 0.0348(16) Uani 1 1 d . . . H20 H -0.0046 0.2101 0.3648 0.042 Uiso 1 1 calc R . . C21 C -0.0779(11) 0.25486(19) 0.3443(9) 0.052(2) Uani 1 1 d . . . H21 H -0.0645 0.2575 0.4435 0.063 Uiso 1 1 calc R . . C22 C -0.1342(9) 0.27893(17) 0.2463(10) 0.047(2) Uani 1 1 d . . . H22 H -0.1614 0.2982 0.2772 0.056 Uiso 1 1 calc R . . C23 C -0.1512(10) 0.27491(18) 0.1029(9) 0.050(2) Uani 1 1 d . . . H23 H -0.1900 0.2916 0.0351 0.060 Uiso 1 1 calc R . . C24 C -0.1125(10) 0.24702(15) 0.0573(8) 0.0435(19) Uani 1 1 d . . . H24 H -0.1252 0.2445 -0.0418 0.052 Uiso 1 1 calc R . . C25 C -0.1070(8) 0.18389(14) -0.0967(6) 0.0265(14) Uani 1 1 d . . . C26 C -0.2628(8) 0.16934(16) -0.1579(8) 0.0391(17) Uani 1 1 d . . . H26 H -0.3084 0.1599 -0.0953 0.047 Uiso 1 1 calc R . . C27 C -0.3520(10) 0.16840(18) -0.3080(8) 0.051(2) Uani 1 1 d . . . H27 H -0.4570 0.1579 -0.3479 0.061 Uiso 1 1 calc R . . C28 C -0.2907(11) 0.18235(19) -0.3993(8) 0.054(2) Uani 1 1 d . . . H28 H -0.3542 0.1820 -0.5025 0.065 Uiso 1 1 calc R . . C29 C -0.1351(12) 0.19711(19) -0.3419(8) 0.053(2) Uani 1 1 d . . . H29 H -0.0910 0.2066 -0.4056 0.064 Uiso 1 1 calc R . . C30 C -0.0439(10) 0.19782(17) -0.1890(7) 0.0405(17) Uani 1 1 d . . . H30 H 0.0621 0.2080 -0.1490 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03137(17) 0.02702(17) 0.03703(18) 0.00532(10) 0.01768(13) 0.00239(10) Te2 0.0377(3) 0.0269(3) 0.0337(3) -0.00160(16) 0.0096(2) -0.00928(17) Te3 0.0379(3) 0.0311(3) 0.0272(2) 0.00075(16) 0.00756(19) -0.00022(18) N1 0.029(3) 0.026(3) 0.024(2) 0.000(2) 0.012(2) -0.002(2) P1 0.0244(8) 0.0227(9) 0.0259(8) -0.0038(6) 0.0097(6) -0.0016(6) P2 0.0284(8) 0.0230(8) 0.0256(8) -0.0017(6) 0.0093(7) -0.0016(6) P3 0.0245(8) 0.0235(8) 0.0244(8) 0.0003(6) 0.0104(6) -0.0001(6) C1 0.035(3) 0.020(3) 0.032(3) -0.005(2) 0.014(3) -0.007(3) C2 0.034(4) 0.041(4) 0.050(4) -0.009(3) 0.014(3) -0.012(3) C3 0.061(5) 0.033(4) 0.047(4) -0.011(3) 0.017(4) -0.010(4) C4 0.031(3) 0.032(4) 0.044(4) -0.005(3) 0.018(3) -0.001(3) C5 0.029(3) 0.052(5) 0.054(4) -0.003(4) 0.024(3) -0.003(3) C6 0.042(4) 0.043(5) 0.070(5) 0.000(4) 0.019(4) 0.013(3) C7 0.037(4) 0.036(4) 0.036(4) -0.006(3) 0.021(3) 0.001(3) C8 0.052(5) 0.044(5) 0.057(5) -0.005(4) 0.034(4) -0.005(4) C9 0.033(4) 0.041(4) 0.047(4) -0.009(3) 0.019(3) 0.002(3) C10 0.045(4) 0.034(4) 0.024(3) 0.004(3) 0.006(3) -0.003(3) C11 0.038(4) 0.057(5) 0.033(4) 0.002(3) 0.003(3) 0.007(3) C12 0.061(5) 0.050(5) 0.029(4) -0.003(3) 0.012(3) 0.001(4) C13 0.027(3) 0.032(4) 0.019(3) 0.002(2) 0.008(2) 0.004(3) C14 0.036(4) 0.032(4) 0.037(4) -0.007(3) 0.017(3) -0.001(3) C15 0.037(4) 0.042(4) 0.048(4) 0.002(3) 0.025(3) 0.012(3) C16 0.028(3) 0.051(5) 0.042(4) 0.013(3) 0.014(3) 0.003(3) C17 0.030(3) 0.043(4) 0.035(4) 0.000(3) 0.012(3) -0.005(3) C18 0.034(3) 0.025(4) 0.041(4) 0.001(3) 0.017(3) -0.001(3) C19 0.024(3) 0.029(3) 0.031(3) -0.002(3) 0.015(3) -0.002(2) C20 0.049(4) 0.029(4) 0.031(3) 0.000(3) 0.021(3) 0.000(3) C21 0.068(5) 0.051(5) 0.047(4) -0.017(4) 0.033(4) -0.005(4) C22 0.047(4) 0.027(4) 0.080(6) -0.019(4) 0.039(4) -0.005(3) C23 0.052(5) 0.036(4) 0.056(5) 0.003(4) 0.016(4) 0.009(4) C24 0.061(5) 0.022(4) 0.039(4) 0.002(3) 0.011(3) 0.011(3) C25 0.031(3) 0.026(3) 0.024(3) 0.000(2) 0.013(3) 0.004(3) C26 0.033(4) 0.039(4) 0.041(4) 0.001(3) 0.009(3) 0.004(3) C27 0.045(4) 0.046(5) 0.041(4) -0.010(4) -0.006(3) 0.011(4) C28 0.068(5) 0.052(5) 0.026(4) -0.008(3) 0.000(4) 0.026(4) C29 0.084(6) 0.047(5) 0.030(4) 0.006(3) 0.024(4) 0.023(4) C30 0.051(4) 0.041(4) 0.038(4) 0.000(3) 0.026(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P3 2.3086(16) . ? Au1 Te2 2.6391(10) . ? Au1 Te3 2.6616(7) . ? Te2 P2 2.4360(17) . ? Te3 P1 2.4347(17) . ? N1 P1 1.591(5) . ? N1 P2 1.601(5) . ? P1 C1 1.842(6) . ? P1 C4 1.848(7) . ? P2 C7 1.839(7) . ? P2 C10 1.846(6) . ? P3 C13 1.819(6) . ? P3 C25 1.823(6) . ? P3 C19 1.825(6) . ? C1 C2 1.531(9) . ? C1 C3 1.545(9) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.539(9) . ? C4 C6 1.541(10) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.539(9) . ? C7 C8 1.544(10) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.528(10) . ? C10 C12 1.542(10) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.392(9) . ? C13 C14 1.394(9) . ? C14 C15 1.381(9) . ? C14 H14 0.9500 . ? C15 C16 1.374(10) . ? C15 H15 0.9500 . ? C16 C17 1.374(10) . ? C16 H16 0.9500 . ? C17 C18 1.382(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.377(9) . ? C19 C24 1.388(9) . ? C20 C21 1.381(10) . ? C20 H20 0.9500 . ? C21 C22 1.373(12) . ? C21 H21 0.9500 . ? C22 C23 1.381(11) . ? C22 H22 0.9500 . ? C23 C24 1.375(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.377(10) . ? C25 C26 1.390(9) . ? C26 C27 1.378(10) . ? C26 H26 0.9500 . ? C27 C28 1.357(12) . ? C27 H27 0.9500 . ? C28 C29 1.393(13) . ? C28 H28 0.9500 . ? C29 C30 1.403(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 P3 Au1 Te2 120.78(4) . . ? P3 Au1 Te3 119.98(4) . . ? Te2 Au1 Te3 118.63(2) . . ? P2 Te2 Au1 98.39(4) . . ? P1 Te3 Au1 97.11(5) . . ? P1 N1 P2 142.5(3) . . ? N1 P1 C1 105.9(3) . . ? N1 P1 C4 110.7(3) . . ? C1 P1 C4 104.4(3) . . ? N1 P1 Te3 121.0(2) . . ? C1 P1 Te3 107.2(2) . . ? C4 P1 Te3 106.5(2) . . ? N1 P2 C7 111.0(3) . . ? N1 P2 C10 105.5(3) . . ? C7 P2 C10 106.1(3) . . ? N1 P2 Te2 119.6(2) . . ? C7 P2 Te2 107.0(2) . . ? C10 P2 Te2 106.9(2) . . ? C13 P3 C25 103.3(3) . . ? C13 P3 C19 105.5(3) . . ? C25 P3 C19 104.6(3) . . ? C13 P3 Au1 107.5(2) . . ? C25 P3 Au1 116.7(2) . . ? C19 P3 Au1 117.9(2) . . ? C2 C1 C3 110.8(6) . . ? C2 C1 P1 110.2(4) . . ? C3 C1 P1 112.9(5) . . ? C2 C1 H1 107.5 . . ? C3 C1 H1 107.5 . . ? P1 C1 H1 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 111.1(6) . . ? C5 C4 P1 110.9(5) . . ? C6 C4 P1 111.2(5) . . ? C5 C4 H4 107.8 . . ? C6 C4 H4 107.8 . . ? P1 C4 H4 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 111.1(6) . . ? C9 C7 P2 110.9(5) . . ? C8 C7 P2 111.7(5) . . ? C9 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? P2 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.0(6) . . ? C11 C10 P2 110.3(5) . . ? C12 C10 P2 112.4(5) . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? P2 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.7(6) . . ? C18 C13 P3 124.9(5) . . ? C14 C13 P3 116.4(5) . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.4(7) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.9(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(7) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.2(6) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C20 C19 C24 118.3(6) . . ? C20 C19 P3 118.9(5) . . ? C24 C19 P3 122.8(5) . . ? C19 C20 C21 121.6(7) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 119.5(7) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 119.7(7) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 120.5(7) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 120.4(7) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 118.7(6) . . ? C30 C25 P3 122.8(5) . . ? C26 C25 P3 118.5(5) . . ? C27 C26 C25 121.1(7) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.4(7) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.1(7) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 119.3(8) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C25 C30 C29 120.4(7) . . ? C25 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.731 _refine_diff_density_min -1.858 _refine_diff_density_rms 0.184 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 612711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 Cu3 N3 P6 Te6' _chemical_formula_sum 'C36 H84 Cu3 N3 P6 Te6' _chemical_formula_weight 1701.10 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0073(3) _cell_length_b 14.4237(4) _cell_length_c 16.5375(4) _cell_angle_alpha 83.975(1) _cell_angle_beta 76.891(2) _cell_angle_gamma 62.512(1) _cell_volume 2886.75(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35862 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 4.260 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8481 _exptl_absorpt_correction_T_max 0.9196 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski and Minor, 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scnas' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55172 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10186 _reflns_number_gt 7864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0914P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10186 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 P1 P 0.61069(16) 0.40049(16) 0.21993(13) 0.0257(5) Uani 1 1 d . . . P2 P 0.56894(15) 0.21198(16) 0.24426(12) 0.0222(4) Uani 1 1 d . . . P3 P 0.79855(16) -0.30649(16) 0.33948(12) 0.0231(4) Uani 1 1 d . . . P4 P 1.01264(15) -0.37017(16) 0.21563(12) 0.0229(4) Uani 1 1 d . . . P5 P 1.20373(15) 0.02693(16) 0.13084(12) 0.0209(4) Uani 1 1 d . . . P6 P 1.11308(16) 0.04701(16) 0.31561(12) 0.0231(4) Uani 1 1 d . . . N1 N 0.5474(5) 0.3300(5) 0.2409(4) 0.0264(15) Uani 1 1 d . . . N2 N 0.9191(5) -0.3764(5) 0.2878(4) 0.0237(14) Uani 1 1 d . . . N3 N 1.1942(5) 0.0313(5) 0.2278(4) 0.0276(15) Uani 1 1 d . . . Te1 Te 0.80294(4) 0.32938(5) 0.22524(5) 0.04213(19) Uani 1 1 d . . . Te2 Te 0.73713(4) 0.09017(4) 0.15259(3) 0.02273(14) Uani 1 1 d . . . Te3 Te 0.74572(5) -0.12796(4) 0.37287(3) 0.03233(16) Uani 1 1 d . . . Te4 Te 0.97676(4) -0.21446(4) 0.12668(3) 0.02369(14) Uani 1 1 d . . . Te5 Te 1.05103(4) 0.04455(4) 0.07231(3) 0.02362(14) Uani 1 1 d . . . Te6 Te 0.96603(4) -0.00415(5) 0.33005(3) 0.02977(15) Uani 1 1 d . . . Cu1 Cu 0.87709(8) 0.13415(9) 0.19767(8) 0.0417(3) Uani 1 1 d . . . Cu2 Cu 0.81402(8) -0.08259(8) 0.22825(6) 0.0281(2) Uani 1 1 d . . . Cu3 Cu 0.99991(8) -0.06986(8) 0.18523(6) 0.0286(2) Uani 1 1 d . . . C1 C 0.5903(7) 0.4601(7) 0.1173(5) 0.035(2) Uani 1 1 d . . . H1 H 0.5103 0.4890 0.1168 0.041 Uiso 1 1 calc R . . C2 C 0.6536(8) 0.3777(8) 0.0488(6) 0.046(2) Uani 1 1 d . . . H2A H 0.6312 0.4080 -0.0037 0.069 Uiso 1 1 calc R . . H2B H 0.6376 0.3180 0.0634 0.069 Uiso 1 1 calc R . . H2C H 0.7326 0.3543 0.0427 0.069 Uiso 1 1 calc R . . C3 C 0.6200(8) 0.5509(8) 0.1005(6) 0.049(3) Uani 1 1 d . . . H3A H 0.6954 0.5270 0.1076 0.073 Uiso 1 1 calc R . . H3B H 0.5694 0.6077 0.1396 0.073 Uiso 1 1 calc R . . H3C H 0.6142 0.5760 0.0436 0.073 Uiso 1 1 calc R . . C4 C 0.5370(7) 0.5097(7) 0.2932(6) 0.033(2) Uani 1 1 d . . . H4 H 0.5737 0.5562 0.2802 0.040 Uiso 1 1 calc R . . C5 C 0.4153(7) 0.5756(8) 0.2844(7) 0.054(3) Uani 1 1 d . . . H5A H 0.3789 0.5304 0.2925 0.081 Uiso 1 1 calc R . . H5B H 0.4130 0.6067 0.2288 0.081 Uiso 1 1 calc R . . H5C H 0.3775 0.6312 0.3262 0.081 Uiso 1 1 calc R . . C6 C 0.5407(9) 0.4733(8) 0.3833(6) 0.052(3) Uani 1 1 d . . . H6A H 0.5164 0.5336 0.4188 0.079 Uiso 1 1 calc R . . H6B H 0.6160 0.4228 0.3872 0.079 Uiso 1 1 calc R . . H6C H 0.4919 0.4403 0.4016 0.079 Uiso 1 1 calc R . . C7 C 0.4533(6) 0.2093(7) 0.2100(5) 0.0308(19) Uani 1 1 d . . . H7 H 0.3843 0.2549 0.2489 0.037 Uiso 1 1 calc R . . C8 C 0.4623(7) 0.1002(7) 0.2166(7) 0.041(2) Uani 1 1 d . . . H8A H 0.3935 0.1032 0.2091 0.062 Uiso 1 1 calc R . . H8B H 0.4761 0.0711 0.2714 0.062 Uiso 1 1 calc R . . H8C H 0.5230 0.0558 0.1735 0.062 Uiso 1 1 calc R . . C9 C 0.4442(7) 0.2562(8) 0.1231(6) 0.042(2) Uani 1 1 d . . . H9A H 0.5052 0.2080 0.0821 0.062 Uiso 1 1 calc R . . H9B H 0.4471 0.3230 0.1206 0.062 Uiso 1 1 calc R . . H9C H 0.3743 0.2676 0.1108 0.062 Uiso 1 1 calc R . . C10 C 0.5610(7) 0.1618(7) 0.3518(5) 0.033(2) Uani 1 1 d . . . H10 H 0.5795 0.0862 0.3500 0.040 Uiso 1 1 calc R . . C11 C 0.6455(7) 0.1708(8) 0.3899(6) 0.041(2) Uani 1 1 d . . . H11A H 0.6222 0.2445 0.4005 0.061 Uiso 1 1 calc R . . H11B H 0.7169 0.1418 0.3514 0.061 Uiso 1 1 calc R . . H11C H 0.6519 0.1319 0.4422 0.061 Uiso 1 1 calc R . . C12 C 0.4454(7) 0.2195(8) 0.4040(6) 0.043(2) Uani 1 1 d . . . H12A H 0.4436 0.1909 0.4605 0.065 Uiso 1 1 calc R . . H12B H 0.3931 0.2106 0.3790 0.065 Uiso 1 1 calc R . . H12C H 0.4255 0.2940 0.4060 0.065 Uiso 1 1 calc R . . C13 C 0.6952(6) -0.3078(7) 0.2890(6) 0.034(2) Uani 1 1 d . . . H13 H 0.7191 -0.3823 0.2756 0.041 Uiso 1 1 calc R . . C14 C 0.5792(7) -0.2670(8) 0.3466(7) 0.048(3) Uani 1 1 d . . . H14A H 0.5544 -0.1949 0.3632 0.071 Uiso 1 1 calc R . . H14B H 0.5829 -0.3113 0.3961 0.071 Uiso 1 1 calc R . . H14C H 0.5274 -0.2691 0.3166 0.071 Uiso 1 1 calc R . . C15 C 0.6873(8) -0.2472(8) 0.2070(6) 0.043(2) Uani 1 1 d . . . H15A H 0.6460 -0.2648 0.1759 0.064 Uiso 1 1 calc R . . H15B H 0.7613 -0.2661 0.1741 0.064 Uiso 1 1 calc R . . H15C H 0.6494 -0.1720 0.2185 0.064 Uiso 1 1 calc R . . C16 C 0.7900(7) -0.3763(7) 0.4373(5) 0.035(2) Uani 1 1 d . . . H16 H 0.7142 -0.3375 0.4711 0.042 Uiso 1 1 calc R . . C17 C 0.8091(9) -0.4864(8) 0.4241(7) 0.054(3) Uani 1 1 d . . . H17A H 0.8767 -0.5218 0.3827 0.081 Uiso 1 1 calc R . . H17B H 0.7469 -0.4836 0.4045 0.081 Uiso 1 1 calc R . . H17C H 0.8160 -0.5249 0.4767 0.081 Uiso 1 1 calc R . . C18 C 0.8714(10) -0.3773(10) 0.4860(6) 0.064(3) Uani 1 1 d . . . H18A H 0.8563 -0.4023 0.5426 0.097 Uiso 1 1 calc R . . H18B H 0.8635 -0.3064 0.4881 0.097 Uiso 1 1 calc R . . H18C H 0.9466 -0.4238 0.4585 0.097 Uiso 1 1 calc R . . C19 C 1.1349(6) -0.4024(7) 0.2591(6) 0.032(2) Uani 1 1 d . . . H19 H 1.1919 -0.3951 0.2138 0.038 Uiso 1 1 calc R . . C20 C 1.1047(8) -0.3248(8) 0.3270(6) 0.044(2) Uani 1 1 d . . . H20A H 1.0462 -0.3282 0.3710 0.066 Uiso 1 1 calc R . . H20B H 1.0790 -0.2541 0.3037 0.066 Uiso 1 1 calc R . . H20C H 1.1694 -0.3421 0.3503 0.066 Uiso 1 1 calc R . . C21 C 1.1828(7) -0.5156(7) 0.2901(6) 0.040(2) Uani 1 1 d . . . H21A H 1.2389 -0.5275 0.3216 0.060 Uiso 1 1 calc R . . H21B H 1.2161 -0.5633 0.2425 0.060 Uiso 1 1 calc R . . H21C H 1.1241 -0.5285 0.3260 0.060 Uiso 1 1 calc R . . C22 C 1.0528(7) -0.4776(7) 0.1442(5) 0.0307(19) Uani 1 1 d . . . H22 H 1.0778 -0.5438 0.1772 0.037 Uiso 1 1 calc R . . C23 C 1.1501(7) -0.4892(7) 0.0728(5) 0.037(2) Uani 1 1 d . . . H23A H 1.1726 -0.5512 0.0398 0.056 Uiso 1 1 calc R . . H23B H 1.2118 -0.4967 0.0959 0.056 Uiso 1 1 calc R . . H23C H 1.1275 -0.4270 0.0373 0.056 Uiso 1 1 calc R . . C24 C 0.9553(7) -0.4666(7) 0.1117(6) 0.037(2) Uani 1 1 d . . . H24A H 0.9323 -0.4057 0.0750 0.055 Uiso 1 1 calc R . . H24B H 0.8944 -0.4575 0.1584 0.055 Uiso 1 1 calc R . . H24C H 0.9761 -0.5296 0.0806 0.055 Uiso 1 1 calc R . . C25 C 1.3201(6) -0.0983(7) 0.0909(5) 0.0303(19) Uani 1 1 d . . . H25 H 1.3323 -0.0970 0.0289 0.036 Uiso 1 1 calc R . . C26 C 1.2963(7) -0.1904(7) 0.1225(6) 0.043(2) Uani 1 1 d . . . H26A H 1.3570 -0.2552 0.0969 0.065 Uiso 1 1 calc R . . H26B H 1.2279 -0.1798 0.1078 0.065 Uiso 1 1 calc R . . H26C H 1.2887 -0.1955 0.1829 0.065 Uiso 1 1 calc R . . C27 C 1.4245(7) -0.1120(8) 0.1159(6) 0.045(2) Uani 1 1 d . . . H27A H 1.4126 -0.1097 0.1765 0.067 Uiso 1 1 calc R . . H27B H 1.4424 -0.0556 0.0916 0.067 Uiso 1 1 calc R . . H27C H 1.4854 -0.1796 0.0956 0.067 Uiso 1 1 calc R . . C28 C 1.2402(6) 0.1295(7) 0.0830(5) 0.0306(19) Uani 1 1 d . . . H28 H 1.2951 0.1299 0.1124 0.037 Uiso 1 1 calc R . . C29 C 1.2922(8) 0.1145(9) -0.0083(6) 0.046(3) Uani 1 1 d . . . H29A H 1.2440 0.1060 -0.0384 0.069 Uiso 1 1 calc R . . H29B H 1.3634 0.0520 -0.0159 0.069 Uiso 1 1 calc R . . H29C H 1.3028 0.1757 -0.0297 0.069 Uiso 1 1 calc R . . C30 C 1.1392(8) 0.2374(7) 0.0971(6) 0.042(2) Uani 1 1 d . . . H30A H 1.1632 0.2923 0.0841 0.063 Uiso 1 1 calc R . . H30B H 1.1007 0.2438 0.1552 0.063 Uiso 1 1 calc R . . H30C H 1.0896 0.2449 0.0608 0.063 Uiso 1 1 calc R . . C31 C 1.1981(6) -0.0309(7) 0.3925(5) 0.0282(18) Uani 1 1 d . . . H31 H 1.1494 -0.0159 0.4488 0.034 Uiso 1 1 calc R . . C32 C 1.2452(7) -0.1473(7) 0.3750(6) 0.040(2) Uani 1 1 d . . . H32A H 1.3027 -0.1661 0.3246 0.060 Uiso 1 1 calc R . . H32B H 1.1865 -0.1626 0.3673 0.060 Uiso 1 1 calc R . . H32C H 1.2765 -0.1879 0.4220 0.060 Uiso 1 1 calc R . . C33 C 1.2911(8) -0.0019(8) 0.3929(6) 0.046(2) Uani 1 1 d . . . H33A H 1.3415 -0.0525 0.4267 0.070 Uiso 1 1 calc R . . H33B H 1.2596 0.0682 0.4164 0.070 Uiso 1 1 calc R . . H33C H 1.3314 -0.0029 0.3359 0.070 Uiso 1 1 calc R . . C34 C 1.0457(7) 0.1856(7) 0.3477(5) 0.0307(19) Uani 1 1 d . . . H34 H 0.9879 0.2234 0.3139 0.037 Uiso 1 1 calc R . . C35 C 1.1212(8) 0.2390(8) 0.3285(6) 0.045(2) Uani 1 1 d . . . H35A H 1.0765 0.3150 0.3280 0.067 Uiso 1 1 calc R . . H35B H 1.1698 0.2160 0.2740 0.067 Uiso 1 1 calc R . . H35C H 1.1656 0.2201 0.3712 0.067 Uiso 1 1 calc R . . C36 C 0.9842(9) 0.2005(8) 0.4392(6) 0.054(3) Uani 1 1 d . . . H36A H 1.0375 0.1735 0.4757 0.081 Uiso 1 1 calc R . . H36B H 0.9400 0.1624 0.4496 0.081 Uiso 1 1 calc R . . H36C H 0.9360 0.2750 0.4504 0.081 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 P1 0.0206(10) 0.0217(11) 0.0330(12) -0.0018(9) -0.0066(9) -0.0072(8) P2 0.0176(9) 0.0219(11) 0.0251(11) -0.0009(8) -0.0040(8) -0.0073(8) P3 0.0216(10) 0.0210(11) 0.0233(10) 0.0005(8) -0.0024(8) -0.0077(8) P4 0.0204(10) 0.0212(11) 0.0247(10) 0.0007(9) -0.0041(8) -0.0077(8) P5 0.0186(9) 0.0237(11) 0.0225(10) 0.0010(8) -0.0075(8) -0.0099(8) P6 0.0227(10) 0.0258(11) 0.0229(10) -0.0010(8) -0.0086(8) -0.0108(8) N1 0.019(3) 0.025(4) 0.032(4) -0.001(3) -0.004(3) -0.007(3) N2 0.021(3) 0.019(3) 0.025(3) -0.001(3) -0.001(3) -0.005(3) N3 0.023(3) 0.034(4) 0.031(4) 0.003(3) -0.012(3) -0.015(3) Te1 0.0255(3) 0.0280(3) 0.0757(5) -0.0057(3) -0.0182(3) -0.0097(2) Te2 0.0187(3) 0.0214(3) 0.0256(3) -0.0012(2) -0.0050(2) -0.0066(2) Te3 0.0367(3) 0.0242(3) 0.0313(3) -0.0039(2) 0.0008(2) -0.0125(2) Te4 0.0252(3) 0.0210(3) 0.0244(3) 0.0015(2) -0.0059(2) -0.0099(2) Te5 0.0211(3) 0.0297(3) 0.0233(3) 0.0032(2) -0.0090(2) -0.0128(2) Te6 0.0268(3) 0.0386(3) 0.0281(3) -0.0006(2) -0.0058(2) -0.0180(2) Cu1 0.0243(5) 0.0344(7) 0.0661(8) -0.0124(6) -0.0079(5) -0.0112(5) Cu2 0.0239(5) 0.0239(6) 0.0337(6) 0.0011(4) -0.0043(4) -0.0093(4) Cu3 0.0298(5) 0.0307(6) 0.0306(6) 0.0026(4) -0.0088(4) -0.0175(4) C1 0.032(4) 0.032(5) 0.035(5) 0.009(4) -0.007(4) -0.011(4) C2 0.061(6) 0.041(6) 0.030(5) 0.004(4) -0.008(5) -0.020(5) C3 0.051(6) 0.045(6) 0.045(6) 0.010(5) -0.004(5) -0.022(5) C4 0.030(4) 0.023(5) 0.046(5) -0.001(4) -0.009(4) -0.010(4) C5 0.034(5) 0.036(6) 0.071(7) -0.014(5) 0.009(5) -0.004(4) C6 0.070(7) 0.043(6) 0.041(6) -0.011(5) -0.010(5) -0.021(5) C7 0.018(4) 0.032(5) 0.042(5) 0.001(4) -0.012(4) -0.009(3) C8 0.026(4) 0.039(6) 0.070(7) 0.002(5) -0.022(4) -0.019(4) C9 0.038(5) 0.045(6) 0.050(6) 0.004(5) -0.028(4) -0.018(4) C10 0.032(5) 0.023(5) 0.030(5) 0.005(4) -0.001(4) -0.005(4) C11 0.038(5) 0.047(6) 0.031(5) 0.000(4) -0.010(4) -0.012(4) C12 0.032(5) 0.051(6) 0.034(5) -0.001(5) 0.005(4) -0.013(4) C13 0.023(4) 0.032(5) 0.046(5) -0.009(4) -0.002(4) -0.012(4) C14 0.024(5) 0.049(6) 0.068(7) -0.006(5) -0.003(4) -0.016(4) C15 0.039(5) 0.042(6) 0.050(6) 0.000(5) -0.024(4) -0.013(4) C16 0.031(5) 0.040(5) 0.023(4) 0.003(4) 0.001(4) -0.011(4) C17 0.065(7) 0.030(6) 0.054(6) 0.015(5) -0.002(5) -0.019(5) C18 0.085(8) 0.072(9) 0.032(6) 0.018(6) -0.022(6) -0.031(7) C19 0.017(4) 0.032(5) 0.045(5) 0.008(4) -0.009(4) -0.011(3) C20 0.045(5) 0.044(6) 0.056(6) 0.006(5) -0.034(5) -0.022(5) C21 0.037(5) 0.033(5) 0.051(6) 0.010(4) -0.015(4) -0.016(4) C22 0.031(4) 0.023(5) 0.030(5) -0.002(4) 0.004(4) -0.010(4) C23 0.041(5) 0.039(5) 0.028(5) -0.004(4) 0.006(4) -0.019(4) C24 0.042(5) 0.032(5) 0.035(5) -0.004(4) -0.007(4) -0.016(4) C25 0.021(4) 0.034(5) 0.030(4) -0.006(4) -0.005(3) -0.006(4) C26 0.036(5) 0.024(5) 0.066(7) -0.009(5) -0.020(5) -0.006(4) C27 0.024(4) 0.049(6) 0.053(6) -0.011(5) -0.015(4) -0.005(4) C28 0.030(4) 0.036(5) 0.039(5) 0.009(4) -0.016(4) -0.023(4) C29 0.055(6) 0.061(7) 0.041(6) 0.018(5) -0.011(5) -0.045(5) C30 0.056(6) 0.029(5) 0.045(6) 0.011(4) -0.016(5) -0.022(5) C31 0.027(4) 0.039(5) 0.020(4) 0.000(4) -0.011(3) -0.013(4) C32 0.036(5) 0.035(5) 0.044(6) 0.009(4) -0.024(4) -0.007(4) C33 0.049(6) 0.058(7) 0.043(6) 0.012(5) -0.033(5) -0.025(5) C34 0.029(4) 0.032(5) 0.032(5) -0.004(4) -0.012(4) -0.012(4) C35 0.060(6) 0.040(6) 0.044(6) -0.007(5) -0.012(5) -0.028(5) C36 0.066(7) 0.035(6) 0.042(6) -0.006(5) 0.007(5) -0.015(5) _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 P1 N1 1.599(7) . ? P1 C4 1.830(9) . ? P1 C1 1.840(9) . ? P1 Te1 2.419(2) . ? P2 N1 1.583(7) . ? P2 C10 1.848(8) . ? P2 C7 1.850(8) . ? P2 Te2 2.460(2) . ? P3 N2 1.598(6) . ? P3 C16 1.824(8) . ? P3 C13 1.836(9) . ? P3 Te3 2.416(2) . ? P4 N2 1.589(6) . ? P4 C22 1.842(9) . ? P4 C19 1.850(8) . ? P4 Te4 2.462(2) . ? P5 N3 1.585(7) . ? P5 C28 1.828(8) . ? P5 C25 1.844(8) . ? P5 Te5 2.442(2) . ? P6 N3 1.591(7) . ? P6 C34 1.850(9) . ? P6 C31 1.857(8) . ? P6 Te6 2.447(2) . ? Te1 Cu1 2.5633(15) . ? Te2 Cu2 2.5326(15) . ? Te2 Cu1 2.5908(13) . ? Te3 Cu2 2.5049(13) . ? Te4 Cu2 2.5626(17) . ? Te4 Cu3 2.5658(13) . ? Te5 Cu3 2.5614(13) . ? Te5 Cu1 2.6961(17) . ? Te6 Cu3 2.5308(13) . ? Te6 Cu1 2.8897(18) . ? Cu1 Cu3 2.6372(18) . ? Cu2 Cu3 2.6255(14) . ? C1 C2 1.529(13) . ? C1 C3 1.529(13) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.530(13) . ? C4 C5 1.554(12) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.514(12) . ? C7 C9 1.530(12) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.520(13) . ? C10 C12 1.527(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.531(13) . ? C13 C14 1.557(11) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.515(14) . ? C16 C18 1.533(15) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(13) . ? C19 C21 1.533(12) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.515(12) . ? C22 C23 1.543(11) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.528(13) . ? C25 C27 1.530(11) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.511(13) . ? C28 C30 1.540(12) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.527(12) . ? C31 C33 1.543(12) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.537(12) . ? C34 C36 1.543(12) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N1 P1 C4 106.3(4) . . ? N1 P1 C1 107.7(4) . . ? C4 P1 C1 105.1(4) . . ? N1 P1 Te1 121.3(3) . . ? C4 P1 Te1 106.3(3) . . ? C1 P1 Te1 109.0(3) . . ? N1 P2 C10 111.7(4) . . ? N1 P2 C7 107.0(4) . . ? C10 P2 C7 104.5(4) . . ? N1 P2 Te2 116.0(2) . . ? C10 P2 Te2 110.7(3) . . ? C7 P2 Te2 106.0(3) . . ? N2 P3 C16 104.7(4) . . ? N2 P3 C13 110.0(4) . . ? C16 P3 C13 105.7(4) . . ? N2 P3 Te3 119.5(3) . . ? C16 P3 Te3 107.4(3) . . ? C13 P3 Te3 108.7(3) . . ? N2 P4 C22 105.3(4) . . ? N2 P4 C19 108.8(4) . . ? C22 P4 C19 106.0(4) . . ? N2 P4 Te4 121.4(2) . . ? C22 P4 Te4 105.0(3) . . ? C19 P4 Te4 109.1(3) . . ? N3 P5 C28 107.4(4) . . ? N3 P5 C25 108.5(4) . . ? C28 P5 C25 106.4(4) . . ? N3 P5 Te5 121.8(2) . . ? C28 P5 Te5 106.3(3) . . ? C25 P5 Te5 105.5(3) . . ? N3 P6 C34 110.2(4) . . ? N3 P6 C31 107.2(3) . . ? C34 P6 C31 107.5(4) . . ? N3 P6 Te6 118.3(3) . . ? C34 P6 Te6 106.3(3) . . ? C31 P6 Te6 106.8(3) . . ? P2 N1 P1 141.5(4) . . ? P4 N2 P3 142.3(4) . . ? P5 N3 P6 143.9(4) . . ? P1 Te1 Cu1 103.23(7) . . ? P2 Te2 Cu2 107.75(6) . . ? P2 Te2 Cu1 98.66(6) . . ? Cu2 Te2 Cu1 88.68(5) . . ? P3 Te3 Cu2 94.58(6) . . ? P4 Te4 Cu2 97.41(6) . . ? P4 Te4 Cu3 114.68(6) . . ? Cu2 Te4 Cu3 61.59(4) . . ? P5 Te5 Cu3 92.92(6) . . ? P5 Te5 Cu1 102.49(6) . . ? Cu3 Te5 Cu1 60.15(4) . . ? P6 Te6 Cu3 101.13(6) . . ? P6 Te6 Cu1 92.22(6) . . ? Cu3 Te6 Cu1 57.77(4) . . ? Te1 Cu1 Te2 113.16(5) . . ? Te1 Cu1 Cu3 163.92(5) . . ? Te2 Cu1 Cu3 82.85(5) . . ? Te1 Cu1 Te5 118.18(6) . . ? Te2 Cu1 Te5 99.94(5) . . ? Cu3 Cu1 Te5 57.39(5) . . ? Te1 Cu1 Te6 115.36(5) . . ? Te2 Cu1 Te6 109.85(5) . . ? Cu3 Cu1 Te6 54.27(4) . . ? Te5 Cu1 Te6 98.49(5) . . ? Te3 Cu2 Te2 128.73(5) . . ? Te3 Cu2 Te4 123.71(5) . . ? Te2 Cu2 Te4 107.50(5) . . ? Te3 Cu2 Cu3 122.35(5) . . ? Te2 Cu2 Cu3 84.21(5) . . ? Te4 Cu2 Cu3 59.27(4) . . ? Te6 Cu3 Te5 112.47(5) . . ? Te6 Cu3 Te4 134.10(5) . . ? Te5 Cu3 Te4 113.12(4) . . ? Te6 Cu3 Cu2 88.27(5) . . ? Te5 Cu3 Cu2 128.24(5) . . ? Te4 Cu3 Cu2 59.15(4) . . ? Te6 Cu3 Cu1 67.96(5) . . ? Te5 Cu3 Cu1 62.46(5) . . ? Te4 Cu3 Cu1 132.19(5) . . ? Cu2 Cu3 Cu1 85.76(5) . . ? C2 C1 C3 111.3(8) . . ? C2 C1 P1 110.8(6) . . ? C3 C1 P1 112.3(7) . . ? C2 C1 H1 107.4 . . ? C3 C1 H1 107.4 . . ? P1 C1 H1 107.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 109.4(8) . . ? C6 C4 P1 112.2(6) . . ? C5 C4 P1 111.7(7) . . ? C6 C4 H4 107.8 . . ? C5 C4 H4 107.8 . . ? P1 C4 H4 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 112.9(8) . . ? C8 C7 P2 111.1(6) . . ? C9 C7 P2 110.8(6) . . ? C8 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? P2 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.2(8) . . ? C11 C10 P2 109.3(6) . . ? C12 C10 P2 111.3(6) . . ? C11 C10 H10 108.3 . . ? C12 C10 H10 108.3 . . ? P2 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 109.7(8) . . ? C15 C13 P3 112.7(6) . . ? C14 C13 P3 112.8(6) . . ? C15 C13 H13 107.1 . . ? C14 C13 H13 107.1 . . ? P3 C13 H13 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 110.9(8) . . ? C17 C16 P3 112.0(6) . . ? C18 C16 P3 110.1(7) . . ? C17 C16 H16 107.9 . . ? C18 C16 H16 107.9 . . ? P3 C16 H16 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 112.3(8) . . ? C20 C19 P4 109.5(6) . . ? C21 C19 P4 110.7(6) . . ? C20 C19 H19 108.1 . . ? C21 C19 H19 108.1 . . ? P4 C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 111.5(7) . . ? C24 C22 P4 111.1(6) . . ? C23 C22 P4 112.7(6) . . ? C24 C22 H22 107.0 . . ? C23 C22 H22 107.0 . . ? P4 C22 H22 107.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 110.0(8) . . ? C26 C25 P5 111.4(6) . . ? C27 C25 P5 110.1(6) . . ? C26 C25 H25 108.4 . . ? C27 C25 H25 108.4 . . ? P5 C25 H25 108.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 109.6(8) . . ? C29 C28 P5 115.1(6) . . ? C30 C28 P5 110.5(6) . . ? C29 C28 H28 107.1 . . ? C30 C28 H28 107.1 . . ? P5 C28 H28 107.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C33 110.5(7) . . ? C32 C31 P6 109.8(6) . . ? C33 C31 P6 112.1(6) . . ? C32 C31 H31 108.1 . . ? C33 C31 H31 108.1 . . ? P6 C31 H31 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C36 112.0(8) . . ? C35 C34 P6 114.6(6) . . ? C36 C34 P6 111.7(6) . . ? C35 C34 H34 105.9 . . ? C36 C34 H34 105.9 . . ? P6 C34 H34 105.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.211 _refine_diff_density_min -2.136 _refine_diff_density_rms 0.284