Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'T. Chivers' 'Dana Eisler' 'Jamie S. Ritch' _publ_contact_author_name 'Prof Tristram Chivers' _publ_contact_author_address ; Department of Chemistry University of Calgary Calgary T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structures of M[N(TePPri2)2-Te,Te]n(n = 2, M = Zn, Cd, Hg; n = 3, M= Sb, Bi): the First Ditelluroimidodiphosphinato p- and d-Block Metal Complexes ; data_2a _database_code_depnum_ccdc_archive 'CCDC 270998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Te4 Zn' _chemical_formula_sum 'C24 H56 N2 P4 Te4 Zn' _chemical_formula_weight 1072.36 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.438(3) _cell_length_b 15.821(3) _cell_length_c 18.900(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.63(3) _cell_angle_gamma 90.00 _cell_volume 3760.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thick plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 3.881 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5756 _exptl_absorpt_correction_T_max 0.8602 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 59623 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8592 _reflns_number_gt 7040 _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^)+(0.0448P)^2^+3.8670P] 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 8592 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Zn1 Zn 0.36993(3) 0.23526(3) 0.08237(2) 0.01715(10) Uani 1 1 d . . . Te1 Te 0.42042(2) 0.134669(16) 0.200290(14) 0.02015(7) Uani 1 1 d . . . Te2 Te 0.515149(19) 0.351228(16) 0.090450(14) 0.01941(7) Uani 1 1 d . . . Te3 Te 0.326078(19) 0.123391(16) -0.029440(13) 0.01868(7) Uani 1 1 d . . . Te4 Te 0.207113(19) 0.335892(16) 0.071499(13) 0.01909(7) Uani 1 1 d . . . P1 P 0.57096(7) 0.20944(6) 0.28912(5) 0.01502(19) Uani 1 1 d . . . C1 C 0.4591(3) 0.3579(3) 0.2872(2) 0.0254(9) Uani 1 1 d . . . H1A H 0.4323 0.3982 0.3156 0.038 Uiso 1 1 calc R . . H1B H 0.3993 0.3340 0.2457 0.038 Uiso 1 1 calc R . . H1C H 0.5071 0.3871 0.2665 0.038 Uiso 1 1 calc R . . C2 C 0.5192(3) 0.2873(3) 0.3396(2) 0.0207(8) Uani 1 1 d . . . H2A H 0.4675 0.2574 0.3581 0.025 Uiso 1 1 calc R . . C3 C 0.6068(3) 0.3238(3) 0.4085(2) 0.0261(9) Uani 1 1 d . . . H3A H 0.5758 0.3648 0.4338 0.039 Uiso 1 1 calc R . . H3B H 0.6600 0.3521 0.3923 0.039 Uiso 1 1 calc R . . H3C H 0.6406 0.2781 0.4437 0.039 Uiso 1 1 calc R . . C4 C 0.5772(4) 0.0931(3) 0.4035(2) 0.0316(10) Uani 1 1 d . . . H4A H 0.6202 0.0517 0.4401 0.047 Uiso 1 1 calc R . . H4B H 0.5139 0.0653 0.3683 0.047 Uiso 1 1 calc R . . H4C H 0.5556 0.1385 0.4302 0.047 Uiso 1 1 calc R . . C5 C 0.6431(3) 0.1304(2) 0.3592(2) 0.0198(8) Uani 1 1 d . . . H5A H 0.7052 0.1599 0.3967 0.024 Uiso 1 1 calc R . . C6 C 0.6877(3) 0.0612(2) 0.3233(2) 0.0238(9) Uani 1 1 d . . . H6A H 0.7263 0.0201 0.3620 0.036 Uiso 1 1 calc R . . H6B H 0.7363 0.0861 0.3008 0.036 Uiso 1 1 calc R . . H6C H 0.6293 0.0328 0.2840 0.036 Uiso 1 1 calc R . . N1 N 0.6582(2) 0.25100(19) 0.26032(16) 0.0164(6) Uani 1 1 d . . . P2 P 0.66990(7) 0.29046(6) 0.18612(5) 0.01471(19) Uani 1 1 d . . . C7 C 0.8041(3) 0.4119(3) 0.1565(2) 0.0298(10) Uani 1 1 d . . . H7A H 0.8569 0.4566 0.1775 0.045 Uiso 1 1 calc R . . H7B H 0.7421 0.4356 0.1166 0.045 Uiso 1 1 calc R . . H7C H 0.8354 0.3671 0.1353 0.045 Uiso 1 1 calc R . . C8 C 0.7696(3) 0.3753(2) 0.2192(2) 0.0182(8) Uani 1 1 d . . . H8A H 0.8341 0.3499 0.2577 0.022 Uiso 1 1 calc R . . C9 C 0.7304(3) 0.4447(2) 0.2589(2) 0.0240(9) Uani 1 1 d . . . H9A H 0.7846 0.4890 0.2761 0.036 Uiso 1 1 calc R . . H9B H 0.7169 0.4207 0.3024 0.036 Uiso 1 1 calc R . . H9C H 0.6645 0.4689 0.2236 0.036 Uiso 1 1 calc R . . C10 C 0.8406(3) 0.1872(3) 0.1904(2) 0.0283(9) Uani 1 1 d . . . H10A H 0.8696 0.1469 0.1634 0.042 Uiso 1 1 calc R . . H10B H 0.8367 0.1605 0.2362 0.042 Uiso 1 1 calc R . . H10C H 0.8869 0.2370 0.2044 0.042 Uiso 1 1 calc R . . C11 C 0.7294(3) 0.2142(2) 0.1394(2) 0.0193(8) Uani 1 1 d . . . H11A H 0.7364 0.2428 0.0942 0.023 Uiso 1 1 calc R . . C12 C 0.6563(3) 0.1370(2) 0.1109(2) 0.0239(9) Uani 1 1 d . . . H12A H 0.6896 0.0973 0.0861 0.036 Uiso 1 1 calc R . . H12B H 0.5877 0.1556 0.0746 0.036 Uiso 1 1 calc R . . H12C H 0.6452 0.1090 0.1537 0.036 Uiso 1 1 calc R . . P3 P 0.17190(7) 0.18907(6) -0.12297(5) 0.01441(19) Uani 1 1 d . . . C13 C 0.1313(3) 0.3020(3) -0.2446(2) 0.0261(9) Uani 1 1 d . . . H13A H 0.1608 0.3443 -0.2695 0.039 Uiso 1 1 calc R . . H13B H 0.0756 0.3280 -0.2295 0.039 Uiso 1 1 calc R . . H13C H 0.1009 0.2553 -0.2795 0.039 Uiso 1 1 calc R . . C14 C 0.2202(3) 0.2681(2) -0.1739(2) 0.0190(8) Uani 1 1 d . . . H14A H 0.2737 0.2395 -0.1915 0.023 Uiso 1 1 calc R . . C15 C 0.2770(3) 0.3408(3) -0.1224(2) 0.0251(9) Uani 1 1 d . . . H15A H 0.3013 0.3820 -0.1516 0.038 Uiso 1 1 calc R . . H15B H 0.3383 0.3188 -0.0809 0.038 Uiso 1 1 calc R . . H15C H 0.2278 0.3684 -0.1018 0.038 Uiso 1 1 calc R . . C16 C 0.1786(3) 0.0687(3) -0.2306(2) 0.0247(9) Uani 1 1 d . . . H16A H 0.1392 0.0258 -0.2671 0.037 Uiso 1 1 calc R . . H16B H 0.2402 0.0425 -0.1922 0.037 Uiso 1 1 calc R . . H16C H 0.2030 0.1131 -0.2569 0.037 Uiso 1 1 calc R . . C17 C 0.1065(3) 0.1073(2) -0.1928(2) 0.0182(8) Uani 1 1 d . . . H17A H 0.0464 0.1352 -0.2334 0.022 Uiso 1 1 calc R . . C18 C 0.0581(3) 0.0388(2) -0.1577(2) 0.0223(8) Uani 1 1 d . . . H18A H 0.0233 -0.0039 -0.1960 0.033 Uiso 1 1 calc R . . H18B H 0.0056 0.0644 -0.1391 0.033 Uiso 1 1 calc R . . H18C H 0.1144 0.0122 -0.1155 0.033 Uiso 1 1 calc R . . N2 N 0.0796(2) 0.22712(19) -0.09716(17) 0.0168(6) Uani 1 1 d . . . P4 P 0.06196(7) 0.26355(6) -0.02391(5) 0.01466(19) Uani 1 1 d . . . C19 C -0.0977(3) 0.1475(3) -0.0277(3) 0.0281(9) Uani 1 1 d . . . H19A H -0.1226 0.1046 -0.0005 0.042 Uiso 1 1 calc R . . H19B H -0.0899 0.1222 -0.0728 0.042 Uiso 1 1 calc R . . H19C H -0.1493 0.1939 -0.0428 0.042 Uiso 1 1 calc R . . C20 C 0.0103(3) 0.1820(2) 0.0241(2) 0.0202(8) Uani 1 1 d . . . H20A H -0.0014 0.2099 0.0680 0.024 Uiso 1 1 calc R . . C21 C 0.0905(3) 0.1112(3) 0.0557(2) 0.0257(9) Uani 1 1 d . . . H21A H 0.0604 0.0690 0.0804 0.039 Uiso 1 1 calc R . . H21B H 0.1557 0.1345 0.0926 0.039 Uiso 1 1 calc R . . H21C H 0.1071 0.0844 0.0144 0.039 Uiso 1 1 calc R . . C22 C -0.0856(3) 0.3718(3) 0.0035(2) 0.0279(9) Uani 1 1 d . . . H22A H -0.1432 0.4128 -0.0176 0.042 Uiso 1 1 calc R . . H22B H -0.0270 0.3986 0.0439 0.042 Uiso 1 1 calc R . . H22C H -0.1121 0.3234 0.0240 0.042 Uiso 1 1 calc R . . C23 C -0.0457(3) 0.3414(2) -0.0591(2) 0.0205(8) Uani 1 1 d . . . H23A H -0.1065 0.3132 -0.0989 0.025 Uiso 1 1 calc R . . C24 C -0.0094(3) 0.4152(3) -0.0963(2) 0.0280(9) Uani 1 1 d . . . H24A H -0.0673 0.4563 -0.1152 0.042 Uiso 1 1 calc R . . H24B H 0.0099 0.3942 -0.1385 0.042 Uiso 1 1 calc R . . H24C H 0.0525 0.4425 -0.0591 0.042 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 Zn1 0.0156(2) 0.0191(2) 0.0148(2) 0.00017(16) 0.00301(17) -0.00026(17) Te1 0.01818(13) 0.02117(14) 0.01737(13) 0.00384(9) 0.00162(10) -0.00469(10) Te2 0.01674(13) 0.02001(13) 0.01904(13) 0.00494(10) 0.00327(10) -0.00069(10) Te3 0.01715(13) 0.01925(13) 0.01697(13) -0.00191(9) 0.00270(10) 0.00371(10) Te4 0.01609(13) 0.01954(13) 0.01846(13) -0.00551(9) 0.00213(10) 0.00105(10) P1 0.0129(4) 0.0178(5) 0.0139(4) 0.0018(4) 0.0042(3) 0.0010(4) C1 0.025(2) 0.025(2) 0.027(2) 0.0011(17) 0.0101(17) 0.0058(17) C2 0.0171(19) 0.029(2) 0.0175(18) -0.0001(16) 0.0080(15) 0.0037(16) C3 0.028(2) 0.029(2) 0.023(2) -0.0038(17) 0.0116(17) 0.0040(18) C4 0.034(2) 0.036(2) 0.026(2) 0.0126(19) 0.0116(18) 0.001(2) C5 0.022(2) 0.0183(19) 0.0168(18) 0.0029(14) 0.0045(15) 0.0017(16) C6 0.023(2) 0.022(2) 0.021(2) 0.0023(16) 0.0017(16) 0.0029(16) N1 0.0159(16) 0.0191(16) 0.0136(15) -0.0015(12) 0.0044(12) -0.0022(13) P2 0.0134(4) 0.0154(4) 0.0153(4) 0.0003(4) 0.0050(4) -0.0001(4) C7 0.029(2) 0.031(2) 0.033(2) -0.0019(19) 0.0163(19) -0.0102(19) C8 0.0122(18) 0.0195(19) 0.0215(19) -0.0018(15) 0.0044(15) -0.0016(15) C9 0.022(2) 0.022(2) 0.030(2) -0.0046(17) 0.0121(17) -0.0051(16) C10 0.021(2) 0.026(2) 0.037(2) -0.0065(18) 0.0100(18) 0.0042(17) C11 0.0193(19) 0.0216(19) 0.0185(18) 0.0000(15) 0.0086(15) -0.0005(16) C12 0.028(2) 0.021(2) 0.022(2) -0.0049(16) 0.0081(17) 0.0023(17) P3 0.0133(4) 0.0161(5) 0.0133(4) -0.0009(4) 0.0039(3) 0.0006(4) C13 0.027(2) 0.032(2) 0.0172(19) 0.0074(17) 0.0056(16) -0.0007(18) C14 0.0163(19) 0.024(2) 0.0166(18) 0.0025(15) 0.0056(15) 0.0010(16) C15 0.022(2) 0.026(2) 0.026(2) -0.0001(17) 0.0070(17) -0.0069(17) C16 0.027(2) 0.029(2) 0.021(2) -0.0114(16) 0.0118(16) -0.0024(18) C17 0.0181(18) 0.023(2) 0.0139(17) -0.0044(15) 0.0063(14) -0.0009(16) C18 0.024(2) 0.019(2) 0.026(2) -0.0060(16) 0.0100(16) -0.0067(16) N2 0.0177(16) 0.0172(16) 0.0159(15) -0.0001(12) 0.0063(12) -0.0005(13) P4 0.0136(4) 0.0153(5) 0.0147(4) -0.0014(4) 0.0046(4) 0.0004(4) C19 0.021(2) 0.027(2) 0.038(2) -0.0037(18) 0.0129(18) -0.0026(17) C20 0.023(2) 0.022(2) 0.0191(19) -0.0009(15) 0.0119(16) -0.0016(16) C21 0.031(2) 0.023(2) 0.026(2) 0.0019(17) 0.0142(18) -0.0018(18) C22 0.023(2) 0.034(2) 0.027(2) -0.0069(18) 0.0084(17) 0.0067(18) C23 0.0193(19) 0.0202(19) 0.0193(19) -0.0039(15) 0.0035(15) 0.0022(16) C24 0.029(2) 0.025(2) 0.027(2) 0.0050(17) 0.0053(17) 0.0063(18) _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 Zn1 Te1 2.6257(7) . ? Zn1 Te2 2.6434(6) . ? Zn1 Te4 2.6547(6) . ? Zn1 Te3 2.6586(7) . ? Te1 P1 2.4326(12) . ? Te2 P2 2.4226(12) . ? Te3 P3 2.4324(12) . ? Te4 P4 2.4265(12) . ? P1 N1 1.597(3) . ? P1 C5 1.831(4) . ? P1 C2 1.838(4) . ? C1 C2 1.522(5) . ? C2 C3 1.529(5) . ? C4 C5 1.533(6) . ? C5 C6 1.518(5) . ? N1 P2 1.593(3) . ? P2 C11 1.837(4) . ? P2 C8 1.843(4) . ? C7 C8 1.530(5) . ? C8 C9 1.523(5) . ? C10 C11 1.527(5) . ? C11 C12 1.539(5) . ? P3 N2 1.601(3) . ? P3 C14 1.830(4) . ? P3 C17 1.836(4) . ? C13 C14 1.541(5) . ? C14 C15 1.526(5) . ? C16 C17 1.520(5) . ? C17 C18 1.530(5) . ? N2 P4 1.593(3) . ? P4 C23 1.837(4) . ? P4 C20 1.848(4) . ? C19 C20 1.535(5) . ? C20 C21 1.523(6) . ? C22 C23 1.538(5) . ? C23 C24 1.529(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te1 Zn1 Te2 114.01(3) . . ? Te1 Zn1 Te4 112.87(3) . . ? Te2 Zn1 Te4 99.19(2) . . ? Te1 Zn1 Te3 100.95(3) . . ? Te2 Zn1 Te3 117.41(2) . . ? Te4 Zn1 Te3 113.07(3) . . ? P1 Te1 Zn1 101.21(3) . . ? P2 Te2 Zn1 100.94(3) . . ? P3 Te3 Zn1 100.77(3) . . ? P4 Te4 Zn1 101.51(3) . . ? N1 P1 C5 105.24(17) . . ? N1 P1 C2 110.99(17) . . ? C5 P1 C2 106.46(18) . . ? N1 P1 Te1 119.77(11) . . ? C5 P1 Te1 105.46(13) . . ? C2 P1 Te1 108.00(13) . . ? C1 C2 C3 110.5(3) . . ? C1 C2 P1 111.4(3) . . ? C3 C2 P1 112.2(3) . . ? C6 C5 C4 111.2(3) . . ? C6 C5 P1 111.2(3) . . ? C4 C5 P1 113.4(3) . . ? P2 N1 P1 140.7(2) . . ? N1 P2 C11 111.13(17) . . ? N1 P2 C8 105.79(17) . . ? C11 P2 C8 104.78(17) . . ? N1 P2 Te2 119.17(12) . . ? C11 P2 Te2 107.84(12) . . ? C8 P2 Te2 107.12(12) . . ? C9 C8 C7 111.1(3) . . ? C9 C8 P2 110.8(3) . . ? C7 C8 P2 113.3(3) . . ? C10 C11 C12 111.2(3) . . ? C10 C11 P2 112.0(3) . . ? C12 C11 P2 111.0(3) . . ? N2 P3 C14 111.08(17) . . ? N2 P3 C17 104.95(16) . . ? C14 P3 C17 105.77(17) . . ? N2 P3 Te3 119.47(12) . . ? C14 P3 Te3 107.74(12) . . ? C17 P3 Te3 106.91(13) . . ? C15 C14 C13 110.5(3) . . ? C15 C14 P3 111.7(3) . . ? C13 C14 P3 112.5(3) . . ? C16 C17 C18 111.0(3) . . ? C16 C17 P3 113.5(3) . . ? C18 C17 P3 110.9(2) . . ? P4 N2 P3 140.3(2) . . ? N2 P4 C23 105.51(17) . . ? N2 P4 C20 111.78(17) . . ? C23 P4 C20 105.18(18) . . ? N2 P4 Te4 119.32(12) . . ? C23 P4 Te4 106.09(13) . . ? C20 P4 Te4 107.90(12) . . ? C21 C20 C19 111.6(3) . . ? C21 C20 P4 111.7(3) . . ? C19 C20 P4 111.7(3) . . ? C24 C23 C22 111.7(3) . . ? C24 C23 P4 109.9(3) . . ? C22 C23 P4 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.331 _refine_diff_density_min -1.443 _refine_diff_density_rms 0.151 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 270999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Cd N2 P4 Te4' _chemical_formula_sum 'C48 H112 Cd2 N4 P8 Te8' _chemical_formula_weight 2238.78 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' Cd Cd -0.8075 1.2024 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5954(19) _cell_length_b 20.202(4) _cell_length_c 21.969(4) _cell_angle_alpha 71.09(3) _cell_angle_beta 80.77(3) _cell_angle_gamma 78.39(3) _cell_volume 3925.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'cut rod' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 3.649 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5596 _exptl_absorpt_correction_T_max 0.7590 _exptl_absorpt_process_details ? _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 54268 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17817 _reflns_number_gt 15714 _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^)+(0.0397P)^2^+7.7606P] 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 17817 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.89941(3) 1.371575(14) 0.262216(13) 0.01803(6) Uani 1 1 d . . . Te1 Te 0.73940(3) 1.486149(14) 0.300647(13) 0.02171(6) Uani 1 1 d . . . Te2 Te 1.14338(3) 1.314167(14) 0.327630(14) 0.02313(6) Uani 1 1 d . . . Te3 Te 0.98185(3) 1.433165(14) 0.130618(12) 0.02211(6) Uani 1 1 d . . . Te4 Te 0.73679(3) 1.264501(14) 0.281899(12) 0.02128(6) Uani 1 1 d . . . P1 P 0.85261(10) 1.47613(5) 0.39501(5) 0.01603(18) Uani 1 1 d . . . C1 C 0.7904(5) 1.3412(2) 0.4606(2) 0.0248(8) Uani 1 1 d . . . H1A H 0.7402 1.3105 0.4982 0.037 Uiso 1 1 calc R . . H1B H 0.8934 1.3239 0.4599 0.037 Uiso 1 1 calc R . . H1C H 0.7566 1.3409 0.4210 0.037 Uiso 1 1 calc R . . C2 C 0.7607(4) 1.4167(2) 0.46503(19) 0.0216(8) Uani 1 1 d . . . H2A H 0.6555 1.4336 0.4640 0.026 Uiso 1 1 calc R . . C3 C 0.8008(6) 1.4183(2) 0.5286(2) 0.0329(10) Uani 1 1 d . . . H3A H 0.7497 1.3862 0.5647 0.049 Uiso 1 1 calc R . . H3B H 0.7745 1.4667 0.5318 0.049 Uiso 1 1 calc R . . H3C H 0.9041 1.4032 0.5304 0.049 Uiso 1 1 calc R . . C4 C 0.8742(5) 1.6198(2) 0.3528(2) 0.0273(9) Uani 1 1 d . . . H4A H 0.8479 1.6657 0.3612 0.041 Uiso 1 1 calc R . . H4B H 0.8396 1.6232 0.3121 0.041 Uiso 1 1 calc R . . H4C H 0.9785 1.6064 0.3497 0.041 Uiso 1 1 calc R . . C5 C 0.8065(4) 1.5636(2) 0.4083(2) 0.0205(8) Uani 1 1 d . . . H5A H 0.8475 1.5598 0.4486 0.025 Uiso 1 1 calc R . . C6 C 0.6445(5) 1.5859(2) 0.4190(2) 0.0307(10) Uani 1 1 d . . . H6A H 0.6242 1.6326 0.4259 0.046 Uiso 1 1 calc R . . H6B H 0.6051 1.5511 0.4571 0.046 Uiso 1 1 calc R . . H6C H 0.6005 1.5882 0.3809 0.046 Uiso 1 1 calc R . . N1 N 1.0217(3) 1.45415(16) 0.39520(15) 0.0173(6) Uani 1 1 d . . . P2 P 1.16094(10) 1.41212(5) 0.36605(5) 0.01617(18) Uani 1 1 d . . . C7 C 1.1732(5) 1.5086(2) 0.2427(2) 0.0283(9) Uani 1 1 d . . . H7A H 1.2281 1.5410 0.2087 0.043 Uiso 1 1 calc R . . H7B H 1.0827 1.5353 0.2560 0.043 Uiso 1 1 calc R . . H7C H 1.1534 1.4722 0.2263 0.043 Uiso 1 1 calc R . . C8 C 1.2594(4) 1.4735(2) 0.30085(19) 0.0209(8) Uani 1 1 d . . . H8A H 1.3493 1.4454 0.2864 0.025 Uiso 1 1 calc R . . C9 C 1.3017(5) 1.5295(2) 0.3243(2) 0.0258(9) Uani 1 1 d . . . H9A H 1.3545 1.5611 0.2884 0.039 Uiso 1 1 calc R . . H9B H 1.3623 1.5062 0.3596 0.039 Uiso 1 1 calc R . . H9C H 1.2154 1.5572 0.3397 0.039 Uiso 1 1 calc R . . C10 C 1.2135(5) 1.3161(2) 0.4870(2) 0.0266(9) Uani 1 1 d . . . H10A H 1.2777 1.2966 0.5212 0.040 Uiso 1 1 calc R . . H10B H 1.2009 1.2781 0.4706 0.040 Uiso 1 1 calc R . . H10C H 1.1204 1.3366 0.5044 0.040 Uiso 1 1 calc R . . C11 C 1.2778(4) 1.3734(2) 0.4319(2) 0.0213(8) Uani 1 1 d . . . H11A H 1.2840 1.4122 0.4498 0.026 Uiso 1 1 calc R . . C12 C 1.4303(4) 1.3457(2) 0.4081(2) 0.0293(9) Uani 1 1 d . . . H12A H 1.4880 1.3257 0.4448 0.044 Uiso 1 1 calc R . . H12B H 1.4724 1.3847 0.3760 0.044 Uiso 1 1 calc R . . H12C H 1.4281 1.3088 0.3884 0.044 Uiso 1 1 calc R . . P3 P 0.79905(10) 1.40312(5) 0.08445(5) 0.01595(18) Uani 1 1 d . . . C13 C 0.6645(5) 1.5449(2) 0.0449(2) 0.0342(10) Uani 1 1 d . . . H13A H 0.5751 1.5783 0.0456 0.051 Uiso 1 1 calc R . . H13B H 0.6999 1.5467 0.0001 0.051 Uiso 1 1 calc R . . H13C H 0.7359 1.5578 0.0645 0.051 Uiso 1 1 calc R . . C14 C 0.6372(4) 1.4697(2) 0.0834(2) 0.0212(8) Uani 1 1 d . . . H14A H 0.5674 1.4578 0.0609 0.025 Uiso 1 1 calc R . . C15 C 0.5677(5) 1.4652(3) 0.1521(2) 0.0322(10) Uani 1 1 d . . . H15A H 0.4814 1.5009 0.1501 0.048 Uiso 1 1 calc R . . H15B H 0.6352 1.4739 0.1766 0.048 Uiso 1 1 calc R . . H15C H 0.5421 1.4179 0.1734 0.048 Uiso 1 1 calc R . . C16 C 0.7516(5) 1.4127(3) -0.0403(2) 0.0307(10) Uani 1 1 d . . . H16A H 0.7916 1.4187 -0.0853 0.046 Uiso 1 1 calc R . . H16B H 0.6723 1.4513 -0.0385 0.046 Uiso 1 1 calc R . . H16C H 0.7166 1.3672 -0.0225 0.046 Uiso 1 1 calc R . . C17 C 0.8674(4) 1.4141(2) -0.00075(18) 0.0194(8) Uani 1 1 d . . . H17A H 0.8993 1.4614 -0.0191 0.023 Uiso 1 1 calc R . . C18 C 0.9967(5) 1.3577(2) -0.0058(2) 0.0259(9) Uani 1 1 d . . . H18A H 1.0322 1.3643 -0.0514 0.039 Uiso 1 1 calc R . . H18B H 0.9691 1.3106 0.0135 0.039 Uiso 1 1 calc R . . H18C H 1.0721 1.3621 0.0173 0.039 Uiso 1 1 calc R . . N2 N 0.7545(4) 1.32653(17) 0.11372(15) 0.0190(6) Uani 1 1 d . . . P4 P 0.76235(10) 1.25596(5) 0.17266(4) 0.01511(18) Uani 1 1 d . . . C19 C 0.4691(5) 1.2612(3) 0.1762(2) 0.0332(10) Uani 1 1 d . . . H19A H 0.3920 1.2370 0.1739 0.050 Uiso 1 1 calc R . . H19B H 0.4663 1.3062 0.1413 0.050 Uiso 1 1 calc R . . H19C H 0.4568 1.2703 0.2181 0.050 Uiso 1 1 calc R . . C20 C 0.6140(4) 1.2140(2) 0.16878(19) 0.0209(8) Uani 1 1 d . . . H20A H 0.6152 1.1693 0.2058 0.025 Uiso 1 1 calc R . . C21 C 0.6313(5) 1.1938(2) 0.1063(2) 0.0269(9) Uani 1 1 d . . . H21A H 0.5503 1.1714 0.1056 0.040 Uiso 1 1 calc R . . H21B H 0.7205 1.1606 0.1043 0.040 Uiso 1 1 calc R . . H21C H 0.6343 1.2365 0.0690 0.040 Uiso 1 1 calc R . . C22 C 1.0597(4) 1.2213(2) 0.1681(2) 0.0253(9) Uani 1 1 d . . . H22A H 1.1457 1.1878 0.1614 0.038 Uiso 1 1 calc R . . H22B H 1.0524 1.2258 0.2116 0.038 Uiso 1 1 calc R . . H22C H 1.0656 1.2677 0.1359 0.038 Uiso 1 1 calc R . . C23 C 0.9269(4) 1.1939(2) 0.16067(19) 0.0207(8) Uani 1 1 d . . . H23A H 0.9353 1.1925 0.1151 0.025 Uiso 1 1 calc R . . C24 C 0.9228(5) 1.1183(2) 0.2051(2) 0.0272(9) Uani 1 1 d . . . H24A H 1.0121 1.0878 0.1965 0.041 Uiso 1 1 calc R . . H24B H 0.8419 1.1006 0.1970 0.041 Uiso 1 1 calc R . . H24C H 0.9119 1.1180 0.2503 0.041 Uiso 1 1 calc R . . Cd2 Cd 0.52436(3) 0.886704(15) 0.246663(13) 0.01813(6) Uani 1 1 d . . . Te5 Te 0.82063(3) 0.840838(14) 0.243856(12) 0.01988(6) Uani 1 1 d . . . Te6 Te 0.40784(3) 0.882167(14) 0.138830(12) 0.01910(6) Uani 1 1 d . . . Te7 Te 0.42939(3) 0.795513(13) 0.366622(12) 0.01987(6) Uani 1 1 d . . . Te8 Te 0.45290(3) 1.031672(13) 0.237111(12) 0.01960(6) Uani 1 1 d . . . P5 P 0.87079(10) 0.85185(5) 0.12984(5) 0.01579(18) Uani 1 1 d . . . C25 C 1.0061(5) 0.9704(2) 0.1052(2) 0.0300(10) Uani 1 1 d . . . H25A H 1.0116 1.0196 0.0793 0.045 Uiso 1 1 calc R . . H25B H 1.0978 0.9405 0.0988 0.045 Uiso 1 1 calc R . . H25C H 0.9846 0.9675 0.1510 0.045 Uiso 1 1 calc R . . C26 C 0.8879(4) 0.9446(2) 0.08400(19) 0.0207(8) Uani 1 1 d . . . H26A H 0.9152 0.9467 0.0376 0.025 Uiso 1 1 calc R . . C27 C 0.7458(4) 0.9931(2) 0.0874(2) 0.0291(9) Uani 1 1 d . . . H27A H 0.7574 1.0419 0.0624 0.044 Uiso 1 1 calc R . . H27B H 0.7134 0.9906 0.1326 0.044 Uiso 1 1 calc R . . H27C H 0.6749 0.9780 0.0694 0.044 Uiso 1 1 calc R . . C28 C 1.1050(4) 0.8127(3) 0.0491(2) 0.0293(9) Uani 1 1 d . . . H28A H 1.1996 0.7842 0.0452 0.044 Uiso 1 1 calc R . . H28B H 1.1124 0.8631 0.0295 0.044 Uiso 1 1 calc R . . H28C H 1.0391 0.7999 0.0266 0.044 Uiso 1 1 calc R . . C29 C 1.0483(4) 0.7987(2) 0.12119(19) 0.0200(8) Uani 1 1 d . . . H29A H 1.1155 0.8132 0.1431 0.024 Uiso 1 1 calc R . . C30 C 1.0401(4) 0.7199(2) 0.1546(2) 0.0275(9) Uani 1 1 d . . . H30A H 1.1349 0.6918 0.1498 0.041 Uiso 1 1 calc R . . H30B H 0.9721 0.7052 0.1346 0.041 Uiso 1 1 calc R . . H30C H 1.0081 0.7124 0.2006 0.041 Uiso 1 1 calc R . . N3 N 0.7677(3) 0.82456(18) 0.09676(16) 0.0191(7) Uani 1 1 d . . . P6 P 0.61096(10) 0.81068(5) 0.09701(5) 0.01586(18) Uani 1 1 d . . . C31 C 0.4644(5) 0.6945(2) 0.1276(3) 0.0331(10) Uani 1 1 d . . . H31A H 0.4637 0.6442 0.1512 0.050 Uiso 1 1 calc R . . H31B H 0.4642 0.7020 0.0813 0.050 Uiso 1 1 calc R . . H31C H 0.3793 0.7229 0.1430 0.050 Uiso 1 1 calc R . . C32 C 0.5992(4) 0.7169(2) 0.1393(2) 0.0233(8) Uani 1 1 d . . . H32A H 0.6836 0.6881 0.1216 0.028 Uiso 1 1 calc R . . C33 C 0.6100(5) 0.6995(2) 0.2112(2) 0.0329(10) Uani 1 1 d . . . H33A H 0.6036 0.6493 0.2327 0.049 Uiso 1 1 calc R . . H33B H 0.5316 0.7288 0.2297 0.049 Uiso 1 1 calc R . . H33C H 0.7017 0.7093 0.2176 0.049 Uiso 1 1 calc R . . C34 C 0.6892(5) 0.7719(3) -0.0154(2) 0.0338(10) Uani 1 1 d . . . H34A H 0.6741 0.7808 -0.0606 0.051 Uiso 1 1 calc R . . H34B H 0.6718 0.7240 0.0098 0.051 Uiso 1 1 calc R . . H34C H 0.7879 0.7763 -0.0129 0.051 Uiso 1 1 calc R . . C35 C 0.5856(4) 0.8261(2) 0.01219(19) 0.0228(8) Uani 1 1 d . . . H35A H 0.4855 0.8204 0.0101 0.027 Uiso 1 1 calc R . . C36 C 0.6066(5) 0.9013(2) -0.0278(2) 0.0313(10) Uani 1 1 d . . . H36A H 0.5922 0.9089 -0.0729 0.047 Uiso 1 1 calc R . . H36B H 0.7039 0.9080 -0.0256 0.047 Uiso 1 1 calc R . . H36C H 0.5373 0.9353 -0.0106 0.047 Uiso 1 1 calc R . . P7 P 0.26676(10) 0.88387(5) 0.40774(4) 0.01445(18) Uani 1 1 d . . . C37 C 0.1244(5) 0.8905(2) 0.5270(2) 0.0292(9) Uani 1 1 d . . . H37A H 0.1154 0.8689 0.5740 0.044 Uiso 1 1 calc R . . H37B H 0.0344 0.8926 0.5102 0.044 Uiso 1 1 calc R . . H37C H 0.1461 0.9386 0.5165 0.044 Uiso 1 1 calc R . . C38 C 0.2461(4) 0.8456(2) 0.49584(18) 0.0202(8) Uani 1 1 d . . . H38A H 0.2223 0.7969 0.5067 0.024 Uiso 1 1 calc R . . C39 C 0.3855(5) 0.8403(2) 0.5231(2) 0.0270(9) Uani 1 1 d . . . H39A H 0.3737 0.8196 0.5703 0.040 Uiso 1 1 calc R . . H39B H 0.4107 0.8878 0.5123 0.040 Uiso 1 1 calc R . . H39C H 0.4618 0.8103 0.5044 0.040 Uiso 1 1 calc R . . C40 C 0.0973(5) 0.9274(2) 0.3065(2) 0.0297(9) Uani 1 1 d . . . H40A H 0.0024 0.9326 0.2927 0.044 Uiso 1 1 calc R . . H40B H 0.1661 0.8964 0.2855 0.044 Uiso 1 1 calc R . . H40C H 0.1271 0.9740 0.2940 0.044 Uiso 1 1 calc R . . C41 C 0.0915(4) 0.8946(2) 0.3800(2) 0.0222(8) Uani 1 1 d . . . H41A H 0.0253 0.9291 0.3995 0.027 Uiso 1 1 calc R . . C42 C 0.0288(5) 0.8257(2) 0.4033(2) 0.0289(9) Uani 1 1 d . . . H42A H -0.0647 0.8342 0.3871 0.043 Uiso 1 1 calc R . . H42B H 0.0176 0.8091 0.4507 0.043 Uiso 1 1 calc R . . H42C H 0.0933 0.7896 0.3869 0.043 Uiso 1 1 calc R . . N4 N 0.3103(3) 0.95910(16) 0.39479(15) 0.0162(6) Uani 1 1 d . . . P8 P 0.40212(10) 1.01789(5) 0.35189(4) 0.01423(18) Uani 1 1 d . . . C43 C 0.6527(5) 1.0678(2) 0.3543(2) 0.0284(9) Uani 1 1 d . . . H43A H 0.7408 1.0593 0.3748 0.043 Uiso 1 1 calc R . . H43B H 0.5940 1.1121 0.3583 0.043 Uiso 1 1 calc R . . H43C H 0.6768 1.0713 0.3084 0.043 Uiso 1 1 calc R . . C44 C 0.5692(4) 1.0064(2) 0.38749(18) 0.0187(7) Uani 1 1 d . . . H44A H 0.5426 1.0059 0.4335 0.022 Uiso 1 1 calc R . . C45 C 0.6637(4) 0.9354(2) 0.3882(2) 0.0256(9) Uani 1 1 d . . . H45A H 0.7515 0.9312 0.4076 0.038 Uiso 1 1 calc R . . H45B H 0.6882 0.9331 0.3438 0.038 Uiso 1 1 calc R . . H45C H 0.6119 0.8965 0.4137 0.038 Uiso 1 1 calc R . . C46 C 0.1507(4) 1.1120(2) 0.3358(2) 0.0244(9) Uani 1 1 d . . . H46A H 0.0952 1.1573 0.3391 0.037 Uiso 1 1 calc R . . H46B H 0.1005 1.0732 0.3630 0.037 Uiso 1 1 calc R . . H46C H 0.1619 1.1119 0.2907 0.037 Uiso 1 1 calc R . . C47 C 0.2984(4) 1.1022(2) 0.35855(18) 0.0195(8) Uani 1 1 d . . . H47A H 0.3492 1.1414 0.3295 0.023 Uiso 1 1 calc R . . C48 C 0.2846(4) 1.1057(2) 0.4283(2) 0.0243(8) Uani 1 1 d . . . H48A H 0.2291 1.1514 0.4304 0.036 Uiso 1 1 calc R . . H48B H 0.3800 1.1007 0.4414 0.036 Uiso 1 1 calc R . . H48C H 0.2358 1.0673 0.4574 0.036 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 Cd1 0.02375(14) 0.01689(13) 0.01536(13) -0.00571(11) -0.00286(10) -0.00547(10) Te1 0.02471(13) 0.01958(13) 0.02331(13) -0.00984(10) -0.00934(10) 0.00195(10) Te2 0.02726(14) 0.01784(13) 0.02844(14) -0.01265(11) -0.01050(11) 0.00254(10) Te3 0.02801(14) 0.02489(13) 0.01539(12) -0.00260(10) -0.00208(10) -0.01458(11) Te4 0.03216(14) 0.02203(13) 0.01281(12) -0.00558(10) 0.00164(10) -0.01405(10) P1 0.0184(4) 0.0134(4) 0.0170(5) -0.0059(4) -0.0019(4) -0.0016(3) C1 0.032(2) 0.0178(19) 0.025(2) -0.0063(16) 0.0007(17) -0.0060(16) C2 0.0220(19) 0.0203(19) 0.022(2) -0.0079(16) 0.0032(15) -0.0040(15) C3 0.053(3) 0.028(2) 0.018(2) -0.0076(18) 0.0006(19) -0.009(2) C4 0.036(2) 0.0120(18) 0.034(2) -0.0045(17) -0.0060(19) -0.0065(16) C5 0.0222(19) 0.0156(18) 0.025(2) -0.0099(16) -0.0029(15) -0.0001(14) C6 0.026(2) 0.027(2) 0.044(3) -0.022(2) -0.0059(19) 0.0050(17) N1 0.0205(16) 0.0148(15) 0.0175(15) -0.0058(13) -0.0021(12) -0.0034(12) P2 0.0170(4) 0.0163(4) 0.0168(5) -0.0066(4) -0.0028(4) -0.0025(3) C7 0.034(2) 0.031(2) 0.019(2) -0.0025(17) 0.0014(17) -0.0136(18) C8 0.0200(18) 0.0215(19) 0.022(2) -0.0087(16) 0.0013(15) -0.0038(15) C9 0.028(2) 0.022(2) 0.027(2) -0.0055(17) -0.0009(17) -0.0086(17) C10 0.031(2) 0.027(2) 0.021(2) -0.0024(17) -0.0097(17) -0.0065(17) C11 0.0191(18) 0.0203(19) 0.025(2) -0.0065(16) -0.0070(15) -0.0011(15) C12 0.0187(19) 0.032(2) 0.035(2) -0.009(2) -0.0075(17) 0.0007(17) P3 0.0205(5) 0.0149(4) 0.0119(4) -0.0023(4) -0.0010(3) -0.0051(4) C13 0.039(3) 0.018(2) 0.041(3) -0.0039(19) -0.006(2) -0.0018(18) C14 0.0214(19) 0.0191(19) 0.023(2) -0.0061(16) -0.0049(15) -0.0013(15) C15 0.032(2) 0.033(2) 0.031(2) -0.015(2) 0.0000(19) 0.0010(19) C16 0.039(2) 0.036(2) 0.0149(19) -0.0065(18) -0.0075(17) 0.001(2) C17 0.0252(19) 0.0168(18) 0.0134(17) -0.0001(14) -0.0002(14) -0.0059(15) C18 0.030(2) 0.026(2) 0.021(2) -0.0092(17) 0.0022(16) -0.0023(17) N2 0.0269(17) 0.0184(16) 0.0130(15) -0.0030(13) -0.0024(13) -0.0091(13) P4 0.0182(4) 0.0160(4) 0.0120(4) -0.0036(4) -0.0013(3) -0.0058(3) C19 0.021(2) 0.044(3) 0.041(3) -0.019(2) -0.0037(19) -0.0085(19) C20 0.027(2) 0.023(2) 0.0159(18) -0.0052(15) -0.0039(15) -0.0104(16) C21 0.036(2) 0.027(2) 0.023(2) -0.0096(18) -0.0033(18) -0.0126(18) C22 0.023(2) 0.027(2) 0.023(2) -0.0044(17) 0.0009(16) -0.0064(16) C23 0.0236(19) 0.0199(19) 0.0173(18) -0.0054(15) -0.0022(15) -0.0011(15) C24 0.030(2) 0.0170(19) 0.031(2) -0.0026(17) -0.0056(18) -0.0015(16) Cd2 0.02081(13) 0.01889(14) 0.01626(13) -0.00794(11) 0.00069(10) -0.00435(10) Te5 0.01959(12) 0.02648(14) 0.01525(12) -0.00806(10) -0.00362(9) -0.00309(10) Te6 0.01507(11) 0.02282(13) 0.02208(13) -0.01172(10) -0.00362(9) 0.00053(9) Te7 0.02568(13) 0.01371(12) 0.01822(12) -0.00524(9) 0.00269(10) -0.00184(9) Te8 0.03043(14) 0.01585(12) 0.01249(11) -0.00420(9) 0.00072(10) -0.00609(10) P5 0.0136(4) 0.0181(5) 0.0163(4) -0.0060(4) -0.0030(3) -0.0016(3) C25 0.029(2) 0.022(2) 0.040(3) -0.0077(19) -0.0014(19) -0.0114(17) C26 0.0229(19) 0.0200(19) 0.0192(19) -0.0059(15) -0.0005(15) -0.0046(15) C27 0.022(2) 0.021(2) 0.039(3) -0.0039(18) -0.0035(18) -0.0007(16) C28 0.019(2) 0.037(2) 0.031(2) -0.015(2) 0.0038(17) -0.0002(17) C29 0.0149(17) 0.0224(19) 0.024(2) -0.0076(16) -0.0057(15) -0.0015(14) C30 0.0195(19) 0.023(2) 0.039(2) -0.0108(19) -0.0036(17) 0.0017(16) N3 0.0149(15) 0.0256(17) 0.0201(16) -0.0121(14) -0.0018(12) -0.0023(13) P6 0.0157(4) 0.0180(5) 0.0165(4) -0.0085(4) -0.0047(3) -0.0009(3) C31 0.030(2) 0.025(2) 0.048(3) -0.012(2) -0.009(2) -0.0097(18) C32 0.0205(19) 0.0164(18) 0.035(2) -0.0097(17) -0.0080(17) -0.0005(15) C33 0.041(3) 0.018(2) 0.037(3) 0.0002(18) -0.015(2) -0.0057(18) C34 0.031(2) 0.047(3) 0.027(2) -0.022(2) -0.0058(18) 0.003(2) C35 0.0182(18) 0.032(2) 0.0207(19) -0.0131(17) -0.0066(15) 0.0023(16) C36 0.037(2) 0.036(3) 0.018(2) -0.0037(18) -0.0067(18) -0.003(2) P7 0.0166(4) 0.0120(4) 0.0143(4) -0.0030(3) -0.0003(3) -0.0041(3) C37 0.028(2) 0.035(2) 0.025(2) -0.0136(19) 0.0057(17) -0.0041(18) C38 0.028(2) 0.0170(18) 0.0151(18) -0.0043(15) 0.0016(15) -0.0076(15) C39 0.034(2) 0.027(2) 0.0176(19) -0.0049(17) -0.0050(17) -0.0003(18) C40 0.031(2) 0.030(2) 0.029(2) -0.0035(19) -0.0135(18) -0.0090(18) C41 0.0217(19) 0.0159(18) 0.030(2) -0.0052(16) -0.0070(16) -0.0041(15) C42 0.023(2) 0.026(2) 0.041(3) -0.0090(19) -0.0069(18) -0.0101(17) N4 0.0182(15) 0.0148(15) 0.0163(15) -0.0058(12) 0.0001(12) -0.0041(12) P8 0.0178(4) 0.0122(4) 0.0132(4) -0.0037(3) -0.0012(3) -0.0040(3) C43 0.027(2) 0.034(2) 0.029(2) -0.0099(19) -0.0003(18) -0.0186(18) C44 0.0199(18) 0.0232(19) 0.0154(17) -0.0062(15) -0.0013(14) -0.0084(15) C45 0.0190(19) 0.029(2) 0.030(2) -0.0115(18) -0.0048(16) -0.0009(16) C46 0.026(2) 0.020(2) 0.026(2) -0.0085(17) -0.0096(17) 0.0070(16) C47 0.0250(19) 0.0137(17) 0.0174(18) -0.0009(14) -0.0021(15) -0.0043(14) C48 0.025(2) 0.022(2) 0.029(2) -0.0136(17) -0.0030(16) 0.0003(16) _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 Cd1 Te2 2.7922(10) . ? Cd1 Te4 2.7995(9) . ? Cd1 Te1 2.8014(10) . ? Cd1 Te3 2.8043(10) . ? Te1 P1 2.4249(12) . ? Te2 P2 2.4329(11) . ? Te3 P3 2.4232(11) . ? Te4 P4 2.4315(11) . ? P1 N1 1.594(3) . ? P1 C5 1.838(4) . ? P1 C2 1.839(4) . ? C1 C2 1.525(5) . ? C2 C3 1.520(6) . ? C4 C5 1.530(6) . ? C5 C6 1.532(6) . ? N1 P2 1.593(3) . ? P2 C8 1.836(4) . ? P2 C11 1.842(4) . ? C7 C8 1.527(6) . ? C8 C9 1.529(5) . ? C10 C11 1.526(6) . ? C11 C12 1.530(6) . ? P3 N2 1.589(3) . ? P3 C14 1.836(4) . ? P3 C17 1.838(4) . ? C13 C14 1.533(6) . ? C14 C15 1.530(6) . ? C16 C17 1.525(6) . ? C17 C18 1.522(5) . ? N2 P4 1.583(3) . ? P4 C20 1.823(4) . ? P4 C23 1.849(4) . ? C19 C20 1.536(6) . ? C20 C21 1.530(5) . ? C22 C23 1.536(6) . ? C23 C24 1.528(5) . ? Cd2 Te5 2.8045(8) . ? Cd2 Te6 2.8111(8) . ? Cd2 Te7 2.8158(11) . ? Cd2 Te8 2.8162(8) . ? Te5 P5 2.4188(11) . ? Te6 P6 2.4252(12) . ? Te7 P7 2.4309(12) . ? Te8 P8 2.4247(11) . ? P5 N3 1.587(3) . ? P5 C29 1.839(4) . ? P5 C26 1.845(4) . ? C25 C26 1.528(6) . ? C26 C27 1.516(5) . ? C28 C29 1.544(6) . ? C29 C30 1.535(6) . ? N3 P6 1.584(3) . ? P6 C35 1.835(4) . ? P6 C32 1.838(4) . ? C31 C32 1.536(6) . ? C32 C33 1.521(6) . ? C34 C35 1.534(6) . ? C35 C36 1.523(6) . ? P7 N4 1.582(3) . ? P7 C41 1.828(4) . ? P7 C38 1.831(4) . ? C37 C38 1.540(5) . ? C38 C39 1.523(6) . ? C40 C41 1.532(6) . ? C41 C42 1.529(5) . ? N4 P8 1.583(3) . ? P8 C47 1.829(4) . ? P8 C44 1.836(4) . ? C43 C44 1.529(5) . ? C44 C45 1.532(5) . ? C46 C47 1.532(5) . ? C47 C48 1.540(6) . ? 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 Cd1 Te4 109.00(3) . . ? Te2 Cd1 Te1 111.70(3) . . ? Te4 Cd1 Te1 111.62(2) . . ? Te2 Cd1 Te3 109.25(3) . . ? Te4 Cd1 Te3 111.93(3) . . ? Te1 Cd1 Te3 103.25(3) . . ? P1 Te1 Cd1 101.19(4) . . ? P2 Te2 Cd1 99.88(3) . . ? P3 Te3 Cd1 99.30(4) . . ? P4 Te4 Cd1 99.95(4) . . ? N1 P1 C5 106.82(18) . . ? N1 P1 C2 110.54(18) . . ? C5 P1 C2 104.99(18) . . ? N1 P1 Te1 120.11(12) . . ? C5 P1 Te1 106.17(14) . . ? C2 P1 Te1 107.14(14) . . ? C3 C2 C1 110.9(4) . . ? C3 C2 P1 111.8(3) . . ? C1 C2 P1 110.8(3) . . ? C4 C5 C6 111.1(4) . . ? C4 C5 P1 111.3(3) . . ? C6 C5 P1 111.9(3) . . ? P2 N1 P1 144.6(2) . . ? N1 P2 C8 110.65(18) . . ? N1 P2 C11 105.69(18) . . ? C8 P2 C11 106.23(19) . . ? N1 P2 Te2 120.59(12) . . ? C8 P2 Te2 107.37(13) . . ? C11 P2 Te2 105.34(13) . . ? C7 C8 C9 110.6(3) . . ? C7 C8 P2 111.1(3) . . ? C9 C8 P2 111.6(3) . . ? C10 C11 C12 111.2(3) . . ? C10 C11 P2 111.4(3) . . ? C12 C11 P2 112.6(3) . . ? N2 P3 C14 108.58(19) . . ? N2 P3 C17 107.31(18) . . ? C14 P3 C17 105.88(18) . . ? N2 P3 Te3 119.68(13) . . ? C14 P3 Te3 109.27(13) . . ? C17 P3 Te3 105.25(13) . . ? C15 C14 C13 111.9(4) . . ? C15 C14 P3 111.1(3) . . ? C13 C14 P3 112.6(3) . . ? C18 C17 C16 111.1(3) . . ? C18 C17 P3 110.3(3) . . ? C16 C17 P3 111.7(3) . . ? P4 N2 P3 145.7(2) . . ? N2 P4 C20 105.54(18) . . ? N2 P4 C23 110.26(18) . . ? C20 P4 C23 106.00(19) . . ? N2 P4 Te4 118.85(13) . . ? C20 P4 Te4 105.94(13) . . ? C23 P4 Te4 109.36(13) . . ? C21 C20 C19 110.7(3) . . ? C21 C20 P4 111.3(3) . . ? C19 C20 P4 111.6(3) . . ? C24 C23 C22 110.9(3) . . ? C24 C23 P4 113.0(3) . . ? C22 C23 P4 110.7(3) . . ? Te5 Cd2 Te6 113.53(3) . . ? Te5 Cd2 Te7 100.76(4) . . ? Te6 Cd2 Te7 115.56(2) . . ? Te5 Cd2 Te8 111.78(3) . . ? Te6 Cd2 Te8 101.62(3) . . ? Te7 Cd2 Te8 114.11(3) . . ? P5 Te5 Cd2 98.09(4) . . ? P6 Te6 Cd2 98.26(3) . . ? P7 Te7 Cd2 98.05(4) . . ? P8 Te8 Cd2 97.50(4) . . ? N3 P5 C29 106.13(17) . . ? N3 P5 C26 109.48(18) . . ? C29 P5 C26 106.77(18) . . ? N3 P5 Te5 118.99(13) . . ? C29 P5 Te5 105.49(14) . . ? C26 P5 Te5 109.24(13) . . ? C27 C26 C25 111.5(3) . . ? C27 C26 P5 111.0(3) . . ? C25 C26 P5 112.5(3) . . ? C30 C29 C28 111.4(3) . . ? C30 C29 P5 109.7(3) . . ? C28 C29 P5 110.4(3) . . ? P6 N3 P5 146.7(2) . . ? N3 P6 C35 106.13(19) . . ? N3 P6 C32 109.55(18) . . ? C35 P6 C32 106.8(2) . . ? N3 P6 Te6 119.66(12) . . ? C35 P6 Te6 105.81(13) . . ? C32 P6 Te6 108.18(14) . . ? C33 C32 C31 110.9(4) . . ? C33 C32 P6 110.9(3) . . ? C31 C32 P6 113.0(3) . . ? C36 C35 C34 110.5(4) . . ? C36 C35 P6 110.3(3) . . ? C34 C35 P6 110.5(3) . . ? N4 P7 C41 109.80(18) . . ? N4 P7 C38 105.42(17) . . ? C41 P7 C38 106.89(19) . . ? N4 P7 Te7 119.43(12) . . ? C41 P7 Te7 108.50(14) . . ? C38 P7 Te7 106.06(13) . . ? C39 C38 C37 109.7(3) . . ? C39 C38 P7 110.0(3) . . ? C37 C38 P7 111.1(3) . . ? C42 C41 C40 112.0(4) . . ? C42 C41 P7 112.6(3) . . ? C40 C41 P7 110.9(3) . . ? P7 N4 P8 148.4(2) . . ? N4 P8 C47 105.61(17) . . ? N4 P8 C44 109.77(17) . . ? C47 P8 C44 106.38(18) . . ? N4 P8 Te8 118.27(12) . . ? C47 P8 Te8 106.14(13) . . ? C44 P8 Te8 109.90(13) . . ? C43 C44 C45 110.7(3) . . ? C43 C44 P8 112.4(3) . . ? C45 C44 P8 111.8(3) . . ? C46 C47 C48 110.9(3) . . ? C46 C47 P8 109.4(3) . . ? C48 C47 P8 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.824 _refine_diff_density_min -1.332 _refine_diff_density_rms 0.154 #===END data_2c _database_code_depnum_ccdc_archive 'CCDC 271000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Hg N2 P4 Te4' _chemical_formula_sum 'C72 H168 Hg3 N6 P12 Te12' _chemical_formula_weight 3622.73 loop_ _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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.941(3) _cell_length_b 18.177(4) _cell_length_c 20.526(4) _cell_angle_alpha 95.78(3) _cell_angle_beta 91.69(3) _cell_angle_gamma 93.24(3) _cell_volume 5904(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3372 _exptl_absorpt_coefficient_mu 6.995 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3352 _exptl_absorpt_correction_T_max 0.3658 _exptl_absorpt_process_details ? _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 83856 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.49 _reflns_number_total 26842 _reflns_number_gt 21683 _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^)+(0.0291P)^2^+22.9547P] 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 26842 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.006 _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 Hg1 Hg 0.290555(15) -1.203957(13) 0.417892(11) 0.02978(5) Uani 1 1 d . . . Te1 Te 0.15873(2) -1.21931(2) 0.324962(18) 0.03065(9) Uani 1 1 d . . . P1 P 0.23679(9) -1.24352(8) 0.22512(7) 0.0253(3) Uani 1 1 d . . . C1 C 0.1627(4) -1.2989(4) 0.1651(3) 0.0382(15) Uani 1 1 d . . . H1A H 0.1913 -1.3041 0.1223 0.046 Uiso 1 1 calc R . . C2 C 0.1453(4) -1.3762(4) 0.1845(3) 0.0430(16) Uani 1 1 d . . . H2A H 0.1065 -1.4043 0.1520 0.064 Uiso 1 1 calc R . . H2B H 0.1201 -1.3733 0.2276 0.064 Uiso 1 1 calc R . . H2C H 0.1982 -1.4011 0.1866 0.064 Uiso 1 1 calc R . . C3 C 0.0821(4) -1.2602(5) 0.1540(3) 0.0491(18) Uani 1 1 d . . . H3A H 0.0449 -1.2915 0.1224 0.074 Uiso 1 1 calc R . . H3B H 0.0957 -1.2128 0.1367 0.074 Uiso 1 1 calc R . . H3C H 0.0539 -1.2514 0.1955 0.074 Uiso 1 1 calc R . . C4 C 0.2578(4) -1.1550(4) 0.1926(3) 0.0408(16) Uani 1 1 d . . . H4A H 0.2054 -1.1273 0.1954 0.049 Uiso 1 1 calc R . . C5 C 0.2815(5) -1.1652(5) 0.1206(4) 0.057(2) Uani 1 1 d . . . H5A H 0.2926 -1.1166 0.1048 0.086 Uiso 1 1 calc R . . H5B H 0.2350 -1.1921 0.0943 0.086 Uiso 1 1 calc R . . H5C H 0.3320 -1.1934 0.1164 0.086 Uiso 1 1 calc R . . C6 C 0.3264(5) -1.1102(4) 0.2353(4) 0.059(2) Uani 1 1 d . . . H6A H 0.3379 -1.0623 0.2183 0.089 Uiso 1 1 calc R . . H6B H 0.3778 -1.1374 0.2348 0.089 Uiso 1 1 calc R . . H6C H 0.3076 -1.1020 0.2804 0.089 Uiso 1 1 calc R . . N1 N 0.3206(3) -1.2862(2) 0.2258(2) 0.0245(10) Uani 1 1 d . . . P2 P 0.38965(9) -1.32032(7) 0.26912(7) 0.0211(3) Uani 1 1 d . . . Te2 Te 0.44314(3) -1.24879(3) 0.36863(2) 0.03602(10) Uani 1 1 d . . . C7 C 0.4816(4) -1.3327(3) 0.2184(3) 0.0268(12) Uani 1 1 d . . . H7A H 0.5248 -1.3564 0.2442 0.032 Uiso 1 1 calc R . . C8 C 0.4599(5) -1.3836(5) 0.1557(3) 0.0498(19) Uani 1 1 d . . . H8A H 0.5104 -1.3894 0.1301 0.075 Uiso 1 1 calc R . . H8B H 0.4168 -1.3619 0.1298 0.075 Uiso 1 1 calc R . . H8C H 0.4384 -1.4321 0.1670 0.075 Uiso 1 1 calc R . . C9 C 0.5199(4) -1.2582(4) 0.2021(3) 0.0394(15) Uani 1 1 d . . . H9A H 0.5691 -1.2662 0.1753 0.059 Uiso 1 1 calc R . . H9B H 0.5371 -1.2274 0.2427 0.059 Uiso 1 1 calc R . . H9C H 0.4782 -1.2331 0.1777 0.059 Uiso 1 1 calc R . . C10 C 0.3519(4) -1.4133(3) 0.2863(3) 0.0300(13) Uani 1 1 d . . . H10A H 0.3307 -1.4405 0.2438 0.036 Uiso 1 1 calc R . . C11 C 0.2786(4) -1.4112(4) 0.3323(3) 0.0391(15) Uani 1 1 d . . . H11A H 0.2606 -1.4619 0.3404 0.059 Uiso 1 1 calc R . . H11B H 0.2317 -1.3880 0.3122 0.059 Uiso 1 1 calc R . . H11C H 0.2962 -1.3825 0.3739 0.059 Uiso 1 1 calc R . . C12 C 0.4224(5) -1.4576(4) 0.3131(5) 0.063(2) Uani 1 1 d . . . H12A H 0.3991 -1.5067 0.3217 0.094 Uiso 1 1 calc R . . H12B H 0.4467 -1.4313 0.3539 0.094 Uiso 1 1 calc R . . H12C H 0.4662 -1.4633 0.2808 0.094 Uiso 1 1 calc R . . Te3 Te 0.34150(3) -1.05670(2) 0.462892(19) 0.03488(10) Uani 1 1 d . . . P3 P 0.28638(10) -1.05387(8) 0.57155(7) 0.0257(3) Uani 1 1 d . . . C13 C 0.1764(4) -1.0302(3) 0.5676(3) 0.0327(13) Uani 1 1 d . . . H13A H 0.1552 -1.0292 0.6130 0.039 Uiso 1 1 calc R . . C14 C 0.1640(5) -0.9542(4) 0.5444(4) 0.0482(18) Uani 1 1 d . . . H14A H 0.1040 -0.9451 0.5436 0.072 Uiso 1 1 calc R . . H14B H 0.1854 -0.9528 0.5002 0.072 Uiso 1 1 calc R . . H14C H 0.1947 -0.9159 0.5744 0.072 Uiso 1 1 calc R . . C15 C 0.1225(4) -1.0900(4) 0.5245(3) 0.0389(15) Uani 1 1 d . . . H15A H 0.0639 -1.0763 0.5234 0.058 Uiso 1 1 calc R . . H15B H 0.1257 -1.1376 0.5427 0.058 Uiso 1 1 calc R . . H15C H 0.1433 -1.0942 0.4799 0.058 Uiso 1 1 calc R . . C16 C 0.3437(4) -0.9750(3) 0.6203(3) 0.0361(14) Uani 1 1 d . . . H16A H 0.3439 -0.9311 0.5946 0.043 Uiso 1 1 calc R . . C17 C 0.4343(5) -0.9937(4) 0.6327(4) 0.053(2) Uani 1 1 d . . . H17A H 0.4648 -0.9518 0.6585 0.079 Uiso 1 1 calc R . . H17B H 0.4613 -1.0039 0.5907 0.079 Uiso 1 1 calc R . . H17C H 0.4351 -1.0376 0.6568 0.079 Uiso 1 1 calc R . . C18 C 0.3016(5) -0.9553(4) 0.6852(3) 0.0482(18) Uani 1 1 d . . . H18A H 0.3332 -0.9132 0.7099 0.072 Uiso 1 1 calc R . . H18B H 0.3008 -0.9980 0.7108 0.072 Uiso 1 1 calc R . . H18C H 0.2439 -0.9422 0.6765 0.072 Uiso 1 1 calc R . . N2 N 0.2938(3) -1.1231(2) 0.6111(2) 0.0277(10) Uani 1 1 d . . . P4 P 0.30183(9) -1.21006(8) 0.60984(7) 0.0228(3) Uani 1 1 d . . . Te4 Te 0.23860(2) -1.28953(2) 0.517338(18) 0.02862(8) Uani 1 1 d . . . C19 C 0.2498(4) -1.2387(3) 0.6828(3) 0.0300(13) Uani 1 1 d . . . H19A H 0.2543 -1.2933 0.6831 0.036 Uiso 1 1 calc R . . C20 C 0.1579(4) -1.2234(4) 0.6806(3) 0.0457(17) Uani 1 1 d . . . H20A H 0.1315 -1.2397 0.7196 0.069 Uiso 1 1 calc R . . H20B H 0.1304 -1.2504 0.6413 0.069 Uiso 1 1 calc R . . H20C H 0.1521 -1.1701 0.6796 0.069 Uiso 1 1 calc R . . C21 C 0.2945(5) -1.1998(4) 0.7457(3) 0.0467(18) Uani 1 1 d . . . H21A H 0.2664 -1.2158 0.7841 0.070 Uiso 1 1 calc R . . H21B H 0.2923 -1.1460 0.7458 0.070 Uiso 1 1 calc R . . H21C H 0.3533 -1.2128 0.7472 0.070 Uiso 1 1 calc R . . C22 C 0.4133(4) -1.2302(3) 0.6203(3) 0.0333(13) Uani 1 1 d . . . H22A H 0.4371 -1.1968 0.6590 0.040 Uiso 1 1 calc R . . C23 C 0.4232(5) -1.3100(4) 0.6360(4) 0.053(2) Uani 1 1 d . . . H23A H 0.4831 -1.3184 0.6413 0.080 Uiso 1 1 calc R . . H23B H 0.3980 -1.3444 0.6000 0.080 Uiso 1 1 calc R . . H23C H 0.3950 -1.3180 0.6767 0.080 Uiso 1 1 calc R . . C24 C 0.4634(4) -1.2125(4) 0.5618(3) 0.0434(16) Uani 1 1 d . . . H24A H 0.5222 -1.2235 0.5693 0.065 Uiso 1 1 calc R . . H24B H 0.4604 -1.1599 0.5559 0.065 Uiso 1 1 calc R . . H24C H 0.4402 -1.2427 0.5225 0.065 Uiso 1 1 calc R . . Hg2 Hg 0.210708(14) -0.543731(12) 0.764729(10) 0.02668(5) Uani 1 1 d . . . P5 P 0.09001(9) -0.62500(8) 0.60139(7) 0.0223(3) Uani 1 1 d . . . Te5 Te 0.07238(3) -0.63430(2) 0.717069(18) 0.03228(9) Uani 1 1 d . . . C25 C 0.0428(4) -0.5408(3) 0.5797(3) 0.0343(14) Uani 1 1 d . . . H25A H 0.0511 -0.5382 0.5319 0.041 Uiso 1 1 calc R . . C26 C -0.0523(4) -0.5431(4) 0.5895(4) 0.0491(18) Uani 1 1 d . . . H26A H -0.0748 -0.4972 0.5770 0.074 Uiso 1 1 calc R . . H26B H -0.0633 -0.5480 0.6356 0.074 Uiso 1 1 calc R . . H26C H -0.0795 -0.5855 0.5621 0.074 Uiso 1 1 calc R . . C27 C 0.0881(5) -0.4718(4) 0.6157(4) 0.0487(18) Uani 1 1 d . . . H27A H 0.0620 -0.4276 0.6029 0.073 Uiso 1 1 calc R . . H27B H 0.1474 -0.4698 0.6043 0.073 Uiso 1 1 calc R . . H27C H 0.0840 -0.4735 0.6631 0.073 Uiso 1 1 calc R . . C28 C 0.0258(4) -0.7026(3) 0.5583(3) 0.0306(13) Uani 1 1 d . . . H28A H -0.0333 -0.6981 0.5725 0.037 Uiso 1 1 calc R . . C29 C 0.0254(5) -0.6989(4) 0.4842(3) 0.0474(18) Uani 1 1 d . . . H29A H -0.0095 -0.7408 0.4623 0.071 Uiso 1 1 calc R . . H29B H 0.0830 -0.7011 0.4690 0.071 Uiso 1 1 calc R . . H29C H 0.0024 -0.6524 0.4739 0.071 Uiso 1 1 calc R . . C30 C 0.0541(4) -0.7771(3) 0.5759(3) 0.0393(15) Uani 1 1 d . . . H30A H 0.0179 -0.8172 0.5525 0.059 Uiso 1 1 calc R . . H30B H 0.0502 -0.7794 0.6232 0.059 Uiso 1 1 calc R . . H30C H 0.1125 -0.7826 0.5634 0.059 Uiso 1 1 calc R . . N3 N 0.1814(3) -0.6278(2) 0.5728(2) 0.0238(9) Uani 1 1 d . . . P6 P 0.27956(8) -0.61510(7) 0.58652(6) 0.0194(3) Uani 1 1 d . . . Te6 Te 0.33380(3) -0.52384(2) 0.674014(19) 0.03408(9) Uani 1 1 d . . . C31 C 0.3243(4) -0.5843(3) 0.5118(3) 0.0262(12) Uani 1 1 d . . . H31A H 0.3034 -0.6213 0.4747 0.031 Uiso 1 1 calc R . . C32 C 0.4204(4) -0.5825(4) 0.5122(3) 0.0424(16) Uani 1 1 d . . . H32A H 0.4402 -0.5656 0.4711 0.064 Uiso 1 1 calc R . . H32B H 0.4390 -0.6324 0.5164 0.064 Uiso 1 1 calc R . . H32C H 0.4436 -0.5485 0.5492 0.064 Uiso 1 1 calc R . . C33 C 0.2915(5) -0.5104(4) 0.4982(3) 0.0412(16) Uani 1 1 d . . . H33A H 0.3159 -0.4948 0.4582 0.062 Uiso 1 1 calc R . . H33B H 0.3071 -0.4733 0.5351 0.062 Uiso 1 1 calc R . . H33C H 0.2301 -0.5155 0.4924 0.062 Uiso 1 1 calc R . . C34 C 0.3258(4) -0.7026(3) 0.5982(3) 0.0289(12) Uani 1 1 d . . . H34A H 0.3878 -0.6919 0.6054 0.035 Uiso 1 1 calc R . . C35 C 0.2930(4) -0.7347(4) 0.6593(3) 0.0434(17) Uani 1 1 d . . . H35A H 0.3191 -0.7814 0.6644 0.065 Uiso 1 1 calc R . . H35B H 0.2319 -0.7438 0.6547 0.065 Uiso 1 1 calc R . . H35C H 0.3071 -0.6995 0.6979 0.065 Uiso 1 1 calc R . . C36 C 0.3128(5) -0.7580(3) 0.5386(3) 0.0410(16) Uani 1 1 d . . . H36A H 0.3389 -0.8039 0.5469 0.062 Uiso 1 1 calc R . . H36B H 0.3386 -0.7377 0.5011 0.062 Uiso 1 1 calc R . . H36C H 0.2525 -0.7685 0.5292 0.062 Uiso 1 1 calc R . . P7 P 0.23941(9) -0.53329(7) 0.95691(6) 0.0205(3) Uani 1 1 d . . . Te7 Te 0.27424(3) -0.61900(2) 0.865481(18) 0.02872(8) Uani 1 1 d . . . C37 C 0.3021(4) -0.5573(3) 1.0277(3) 0.0269(12) Uani 1 1 d . . . H37A H 0.2906 -0.6113 1.0316 0.032 Uiso 1 1 calc R . . C38 C 0.3946(4) -0.5444(4) 1.0181(3) 0.0406(16) Uani 1 1 d . . . H38A H 0.4262 -0.5581 1.0562 0.061 Uiso 1 1 calc R . . H38B H 0.4074 -0.4919 1.0131 0.061 Uiso 1 1 calc R . . H38C H 0.4104 -0.5746 0.9787 0.061 Uiso 1 1 calc R . . C39 C 0.2748(4) -0.5140(3) 1.0911(3) 0.0341(14) Uani 1 1 d . . . H39A H 0.3085 -0.5273 1.1284 0.051 Uiso 1 1 calc R . . H39B H 0.2152 -0.5264 1.0976 0.051 Uiso 1 1 calc R . . H39C H 0.2833 -0.4607 1.0878 0.051 Uiso 1 1 calc R . . C40 C 0.1289(4) -0.5510(3) 0.9763(3) 0.0272(12) Uani 1 1 d . . . H40A H 0.1174 -0.5160 1.0153 0.033 Uiso 1 1 calc R . . C41 C 0.1115(4) -0.6303(4) 0.9956(4) 0.0427(16) Uani 1 1 d . . . H41A H 0.0521 -0.6376 1.0058 0.064 Uiso 1 1 calc R . . H41B H 0.1467 -0.6373 1.0342 0.064 Uiso 1 1 calc R . . H41C H 0.1247 -0.6663 0.9592 0.064 Uiso 1 1 calc R . . C42 C 0.0691(4) -0.5361(4) 0.9218(3) 0.0368(14) Uani 1 1 d . . . H42A H 0.0111 -0.5460 0.9346 0.055 Uiso 1 1 calc R . . H42B H 0.0800 -0.5683 0.8821 0.055 Uiso 1 1 calc R . . H42C H 0.0772 -0.4841 0.9132 0.055 Uiso 1 1 calc R . . N4 N 0.2591(3) -0.4470(2) 0.9525(2) 0.0259(10) Uani 1 1 d . . . P8 P 0.25754(10) -0.38189(7) 0.90807(7) 0.0234(3) Uani 1 1 d . . . Te8 Te 0.17695(3) -0.39586(2) 0.804894(18) 0.02967(9) Uani 1 1 d . . . C43 C 0.3658(4) -0.3509(4) 0.8909(3) 0.0358(14) Uani 1 1 d . . . H43A H 0.3628 -0.3078 0.8644 0.043 Uiso 1 1 calc R . . C44 C 0.4163(5) -0.3245(5) 0.9544(4) 0.058(2) Uani 1 1 d . . . H44A H 0.4736 -0.3083 0.9439 0.087 Uiso 1 1 calc R . . H44B H 0.4184 -0.3652 0.9821 0.087 Uiso 1 1 calc R . . H44C H 0.3893 -0.2830 0.9778 0.087 Uiso 1 1 calc R . . C45 C 0.4084(4) -0.4120(5) 0.8504(4) 0.0500(18) Uani 1 1 d . . . H45A H 0.4658 -0.3945 0.8416 0.075 Uiso 1 1 calc R . . H45B H 0.3766 -0.4251 0.8088 0.075 Uiso 1 1 calc R . . H45C H 0.4101 -0.4557 0.8746 0.075 Uiso 1 1 calc R . . C46 C 0.2141(4) -0.3047(3) 0.9591(3) 0.0343(14) Uani 1 1 d . . . H46A H 0.2493 -0.2961 1.0007 0.041 Uiso 1 1 calc R . . C47 C 0.1250(5) -0.3258(4) 0.9774(4) 0.0473(18) Uani 1 1 d . . . H47A H 0.1027 -0.2843 1.0043 0.071 Uiso 1 1 calc R . . H47B H 0.1252 -0.3691 1.0022 0.071 Uiso 1 1 calc R . . H47C H 0.0896 -0.3376 0.9375 0.071 Uiso 1 1 calc R . . C48 C 0.2166(6) -0.2330(4) 0.9282(4) 0.054(2) Uani 1 1 d . . . H48A H 0.1924 -0.1947 0.9577 0.082 Uiso 1 1 calc R . . H48B H 0.1841 -0.2399 0.8865 0.082 Uiso 1 1 calc R . . H48C H 0.2750 -0.2177 0.9201 0.082 Uiso 1 1 calc R . . Hg3 Hg 0.216337(15) 0.134795(12) 1.087727(11) 0.02830(5) Uani 1 1 d . . . P9 P 0.16762(9) 0.06883(7) 0.89937(7) 0.0218(3) Uani 1 1 d . . . Te9 Te 0.11345(3) 0.15869(2) 0.981063(19) 0.03146(9) Uani 1 1 d . . . C49 C 0.1050(4) -0.0178(3) 0.9029(3) 0.0305(13) Uani 1 1 d . . . H49A H 0.0445 -0.0069 0.8982 0.037 Uiso 1 1 calc R . . C50 C 0.1177(5) -0.0475(4) 0.9688(4) 0.0468(18) Uani 1 1 d . . . H50A H 0.0835 -0.0939 0.9696 0.070 Uiso 1 1 calc R . . H50B H 0.1006 -0.0111 1.0037 0.070 Uiso 1 1 calc R . . H50C H 0.1771 -0.0566 0.9758 0.070 Uiso 1 1 calc R . . C51 C 0.1238(4) -0.0756(3) 0.8463(4) 0.0462(18) Uani 1 1 d . . . H51A H 0.0892 -0.1213 0.8495 0.069 Uiso 1 1 calc R . . H51B H 0.1834 -0.0860 0.8486 0.069 Uiso 1 1 calc R . . H51C H 0.1107 -0.0564 0.8044 0.069 Uiso 1 1 calc R . . C52 C 0.1457(4) 0.1006(3) 0.8190(3) 0.0274(12) Uani 1 1 d . . . H52A H 0.1649 0.0621 0.7853 0.033 Uiso 1 1 calc R . . C53 C 0.0531(4) 0.1079(4) 0.8047(3) 0.0463(17) Uani 1 1 d . . . H53A H 0.0453 0.1251 0.7613 0.070 Uiso 1 1 calc R . . H53B H 0.0313 0.1438 0.8380 0.070 Uiso 1 1 calc R . . H53C H 0.0227 0.0597 0.8057 0.070 Uiso 1 1 calc R . . C54 C 0.1960(5) 0.1725(4) 0.8108(3) 0.0474(18) Uani 1 1 d . . . H54A H 0.1833 0.1880 0.7674 0.071 Uiso 1 1 calc R . . H54B H 0.2562 0.1649 0.8152 0.071 Uiso 1 1 calc R . . H54C H 0.1810 0.2111 0.8446 0.071 Uiso 1 1 calc R . . N5 N 0.2647(3) 0.0535(3) 0.9006(2) 0.0275(10) Uani 1 1 d . . . P10 P 0.35155(8) 0.06284(7) 0.94060(7) 0.0204(3) Uani 1 1 d . . . Te10 Te 0.35236(2) 0.04949(2) 1.056643(18) 0.02939(9) Uani 1 1 d . . . C55 C 0.4068(3) 0.1510(3) 0.9287(3) 0.0246(11) Uani 1 1 d . . . H55A H 0.4048 0.1556 0.8806 0.030 Uiso 1 1 calc R . . C56 C 0.4996(4) 0.1529(4) 0.9505(3) 0.0383(15) Uani 1 1 d . . . H56A H 0.5270 0.2009 0.9435 0.057 Uiso 1 1 calc R . . H56B H 0.5271 0.1133 0.9249 0.057 Uiso 1 1 calc R . . H56C H 0.5041 0.1457 0.9972 0.057 Uiso 1 1 calc R . . C57 C 0.3648(4) 0.2171(3) 0.9617(3) 0.0327(13) Uani 1 1 d . . . H57A H 0.3967 0.2629 0.9539 0.049 Uiso 1 1 calc R . . H57B H 0.3632 0.2133 1.0089 0.049 Uiso 1 1 calc R . . H57C H 0.3073 0.2179 0.9436 0.049 Uiso 1 1 calc R . . C58 C 0.4167(4) -0.0099(3) 0.9048(3) 0.0293(12) Uani 1 1 d . . . H58A H 0.4709 -0.0066 0.9310 0.035 Uiso 1 1 calc R . . C59 C 0.4373(5) 0.0009(4) 0.8338(3) 0.0465(17) Uani 1 1 d . . . H59A H 0.4724 -0.0385 0.8164 0.070 Uiso 1 1 calc R . . H59B H 0.4677 0.0491 0.8324 0.070 Uiso 1 1 calc R . . H59C H 0.3850 -0.0009 0.8072 0.070 Uiso 1 1 calc R . . C60 C 0.3739(4) -0.0860(3) 0.9095(3) 0.0366(15) Uani 1 1 d . . . H60A H 0.4096 -0.1243 0.8906 0.055 Uiso 1 1 calc R . . H60B H 0.3196 -0.0901 0.8853 0.055 Uiso 1 1 calc R . . H60C H 0.3648 -0.0928 0.9556 0.055 Uiso 1 1 calc R . . P11 P 0.18431(9) 0.12288(7) 1.27914(7) 0.0214(3) Uani 1 1 d . . . Te11 Te 0.14055(2) 0.04797(2) 1.177941(18) 0.02758(8) Uani 1 1 d . . . C61 C 0.2869(4) 0.0942(3) 1.3071(3) 0.0296(13) Uani 1 1 d . . . H61A H 0.2817 0.0392 1.3075 0.036 Uiso 1 1 calc R . . C62 C 0.3553(4) 0.1113(4) 1.2597(4) 0.0430(16) Uani 1 1 d . . . H62A H 0.4090 0.0952 1.2759 0.064 Uiso 1 1 calc R . . H62B H 0.3601 0.1647 1.2562 0.064 Uiso 1 1 calc R . . H62C H 0.3407 0.0849 1.2164 0.064 Uiso 1 1 calc R . . C63 C 0.3093(4) 0.1275(3) 1.3772(3) 0.0403(16) Uani 1 1 d . . . H63A H 0.3639 0.1111 1.3910 0.060 Uiso 1 1 calc R . . H63B H 0.2661 0.1112 1.4065 0.060 Uiso 1 1 calc R . . H63C H 0.3121 0.1817 1.3791 0.060 Uiso 1 1 calc R . . C64 C 0.1102(4) 0.0974(3) 1.3410(3) 0.0301(13) Uani 1 1 d . . . H64A H 0.1307 0.1245 1.3838 0.036 Uiso 1 1 calc R . . C65 C 0.0235(4) 0.1240(4) 1.3256(3) 0.0469(18) Uani 1 1 d . . . H65A H -0.0154 0.1101 1.3590 0.070 Uiso 1 1 calc R . . H65B H 0.0030 0.1011 1.2824 0.070 Uiso 1 1 calc R . . H65C H 0.0273 0.1780 1.3256 0.070 Uiso 1 1 calc R . . C66 C 0.1056(5) 0.0151(4) 1.3497(3) 0.0425(16) Uani 1 1 d . . . H66A H 0.0652 0.0052 1.3833 0.064 Uiso 1 1 calc R . . H66B H 0.1612 0.0006 1.3634 0.064 Uiso 1 1 calc R . . H66C H 0.0874 -0.0134 1.3082 0.064 Uiso 1 1 calc R . . N6 N 0.1852(3) 0.2102(2) 1.2810(2) 0.0252(10) Uani 1 1 d . . . P12 P 0.19305(9) 0.28034(8) 1.24103(7) 0.0233(3) Uani 1 1 d . . . Te12 Te 0.27839(3) 0.27535(2) 1.145070(19) 0.02971(8) Uani 1 1 d . . . C67 C 0.2409(4) 0.3562(3) 1.2984(3) 0.0338(14) Uani 1 1 d . . . H67A H 0.2459 0.4017 1.2749 0.041 Uiso 1 1 calc R . . C68 C 0.1843(5) 0.3718(4) 1.3563(3) 0.0488(18) Uani 1 1 d . . . H68A H 0.2104 0.4124 1.3865 0.073 Uiso 1 1 calc R . . H68B H 0.1768 0.3272 1.3792 0.073 Uiso 1 1 calc R . . H68C H 0.1295 0.3857 1.3403 0.073 Uiso 1 1 calc R . . C69 C 0.3283(4) 0.3395(4) 1.3216(3) 0.0403(16) Uani 1 1 d . . . H69A H 0.3521 0.3811 1.3519 0.060 Uiso 1 1 calc R . . H69B H 0.3642 0.3323 1.2838 0.060 Uiso 1 1 calc R . . H69C H 0.3251 0.2944 1.3441 0.060 Uiso 1 1 calc R . . C70 C 0.0881(4) 0.3088(3) 1.2196(3) 0.0317(13) Uani 1 1 d . . . H70A H 0.0551 0.3097 1.2604 0.038 Uiso 1 1 calc R . . C71 C 0.0896(5) 0.3876(4) 1.1980(4) 0.0432(17) Uani 1 1 d . . . H71A H 0.0321 0.4000 1.1874 0.065 Uiso 1 1 calc R . . H71B H 0.1238 0.3898 1.1593 0.065 Uiso 1 1 calc R . . H71C H 0.1139 0.4230 1.2337 0.065 Uiso 1 1 calc R . . C72 C 0.0416(4) 0.2535(4) 1.1687(3) 0.0403(15) Uani 1 1 d . . . H72A H -0.0141 0.2707 1.1589 0.061 Uiso 1 1 calc R . . H72B H 0.0353 0.2051 1.1858 0.061 Uiso 1 1 calc R . . H72C H 0.0736 0.2489 1.1286 0.061 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 Hg1 0.03000(12) 0.03331(12) 0.02560(11) -0.00119(9) 0.00428(9) 0.00395(9) Te1 0.02331(19) 0.0443(2) 0.02467(19) -0.00022(16) 0.00604(15) 0.00863(16) P1 0.0234(7) 0.0321(8) 0.0228(7) 0.0086(6) 0.0059(6) 0.0089(6) C1 0.026(3) 0.065(4) 0.023(3) -0.005(3) 0.001(2) 0.016(3) C2 0.027(3) 0.058(4) 0.041(4) -0.011(3) -0.001(3) 0.003(3) C3 0.036(4) 0.076(5) 0.036(4) 0.004(4) -0.003(3) 0.019(4) C4 0.040(4) 0.037(4) 0.050(4) 0.019(3) 0.015(3) 0.012(3) C5 0.062(5) 0.065(5) 0.052(5) 0.029(4) 0.026(4) 0.018(4) C6 0.069(6) 0.024(3) 0.086(6) 0.009(4) 0.015(5) 0.004(3) N1 0.025(2) 0.027(2) 0.023(2) 0.0048(18) 0.0048(19) 0.0080(19) P2 0.0184(7) 0.0214(6) 0.0242(7) 0.0035(5) 0.0039(5) 0.0043(5) Te2 0.0221(2) 0.0530(3) 0.0302(2) -0.01037(18) 0.00014(16) 0.00508(17) C7 0.021(3) 0.029(3) 0.031(3) 0.002(2) 0.004(2) 0.006(2) C8 0.033(4) 0.071(5) 0.042(4) -0.015(4) 0.008(3) 0.002(3) C9 0.036(4) 0.042(4) 0.044(4) 0.015(3) 0.018(3) 0.005(3) C10 0.027(3) 0.021(3) 0.044(3) 0.007(2) 0.007(3) 0.002(2) C11 0.039(4) 0.037(3) 0.044(4) 0.018(3) 0.008(3) -0.004(3) C12 0.048(5) 0.038(4) 0.111(7) 0.042(4) 0.009(5) 0.010(3) Te3 0.0492(3) 0.02775(19) 0.0279(2) 0.00441(15) 0.01385(18) -0.00466(17) P3 0.0348(8) 0.0185(6) 0.0240(7) 0.0031(5) 0.0041(6) 0.0005(6) C13 0.040(4) 0.027(3) 0.033(3) 0.009(2) 0.010(3) 0.007(3) C14 0.061(5) 0.034(4) 0.052(4) 0.008(3) 0.005(4) 0.018(3) C15 0.034(4) 0.043(4) 0.041(4) 0.008(3) 0.005(3) 0.009(3) C16 0.050(4) 0.027(3) 0.030(3) 0.001(2) 0.001(3) -0.002(3) C17 0.051(5) 0.050(4) 0.053(4) -0.007(4) -0.006(4) -0.017(4) C18 0.077(6) 0.034(4) 0.031(3) -0.007(3) -0.004(3) 0.003(3) N2 0.040(3) 0.022(2) 0.020(2) 0.0000(18) 0.003(2) 0.004(2) P4 0.0259(7) 0.0213(7) 0.0217(7) 0.0041(5) 0.0025(6) 0.0024(5) Te4 0.0318(2) 0.02468(18) 0.02826(19) 0.00059(14) 0.00031(15) -0.00416(15) C19 0.039(3) 0.029(3) 0.024(3) 0.010(2) 0.007(2) 0.006(3) C20 0.041(4) 0.058(5) 0.042(4) 0.021(3) 0.014(3) 0.007(3) C21 0.071(5) 0.047(4) 0.022(3) 0.003(3) 0.005(3) -0.001(4) C22 0.024(3) 0.034(3) 0.041(3) 0.001(3) -0.002(3) 0.002(2) C23 0.039(4) 0.052(4) 0.071(5) 0.008(4) -0.011(4) 0.025(3) C24 0.031(4) 0.059(4) 0.039(4) 0.000(3) 0.003(3) 0.003(3) Hg2 0.03042(12) 0.02873(11) 0.02034(10) 0.00031(8) -0.00085(8) 0.00193(9) P5 0.0188(7) 0.0272(7) 0.0207(7) 0.0010(5) -0.0016(5) 0.0037(5) Te5 0.0293(2) 0.0446(2) 0.02151(18) 0.00186(16) 0.00269(15) -0.00874(17) C25 0.038(4) 0.033(3) 0.034(3) 0.005(3) 0.001(3) 0.020(3) C26 0.032(4) 0.058(5) 0.059(5) 0.005(4) -0.001(3) 0.021(3) C27 0.059(5) 0.035(4) 0.054(4) 0.008(3) -0.005(4) 0.018(3) C28 0.022(3) 0.039(3) 0.029(3) -0.006(2) 0.001(2) -0.004(2) C29 0.045(4) 0.067(5) 0.026(3) -0.005(3) -0.006(3) -0.017(4) C30 0.039(4) 0.026(3) 0.050(4) -0.006(3) -0.005(3) -0.004(3) N3 0.021(2) 0.025(2) 0.025(2) 0.0009(18) -0.0019(18) -0.0020(18) P6 0.0172(6) 0.0229(6) 0.0183(6) 0.0027(5) 0.0019(5) 0.0011(5) Te6 0.0291(2) 0.0452(2) 0.02431(19) -0.00679(16) 0.00287(15) -0.01204(17) C31 0.031(3) 0.028(3) 0.020(3) 0.002(2) 0.006(2) -0.001(2) C32 0.039(4) 0.053(4) 0.034(3) 0.005(3) 0.013(3) -0.011(3) C33 0.062(5) 0.037(4) 0.026(3) 0.010(3) -0.003(3) 0.003(3) C34 0.022(3) 0.027(3) 0.038(3) 0.007(2) 0.002(2) 0.006(2) C35 0.041(4) 0.043(4) 0.052(4) 0.022(3) 0.006(3) 0.013(3) C36 0.048(4) 0.023(3) 0.052(4) 0.000(3) 0.011(3) 0.006(3) P7 0.0234(7) 0.0199(6) 0.0185(6) 0.0031(5) -0.0004(5) 0.0034(5) Te7 0.0416(2) 0.02208(17) 0.02295(18) -0.00001(14) -0.00163(16) 0.01130(15) C37 0.031(3) 0.029(3) 0.021(3) 0.005(2) -0.006(2) -0.001(2) C38 0.035(4) 0.055(4) 0.033(3) 0.005(3) -0.007(3) 0.013(3) C39 0.042(4) 0.035(3) 0.024(3) -0.002(2) -0.003(3) 0.002(3) C40 0.026(3) 0.028(3) 0.026(3) -0.001(2) 0.004(2) -0.001(2) C41 0.036(4) 0.040(4) 0.053(4) 0.014(3) 0.007(3) -0.012(3) C42 0.027(3) 0.045(4) 0.038(3) 0.006(3) -0.001(3) 0.001(3) N4 0.031(3) 0.020(2) 0.026(2) 0.0020(18) -0.005(2) -0.0023(19) P8 0.0317(8) 0.0165(6) 0.0215(7) 0.0010(5) -0.0029(6) 0.0016(5) Te8 0.0407(2) 0.02455(18) 0.02404(18) 0.00285(14) -0.00700(16) 0.00860(16) C43 0.032(3) 0.036(3) 0.038(3) 0.004(3) -0.005(3) -0.010(3) C44 0.040(4) 0.067(5) 0.061(5) -0.014(4) -0.005(4) -0.013(4) C45 0.029(4) 0.072(5) 0.047(4) -0.003(4) 0.005(3) 0.000(3) C46 0.050(4) 0.020(3) 0.032(3) 0.000(2) -0.004(3) 0.003(3) C47 0.058(5) 0.040(4) 0.043(4) -0.006(3) 0.004(3) 0.017(3) C48 0.088(6) 0.021(3) 0.055(5) 0.004(3) 0.011(4) 0.010(3) Hg3 0.03041(12) 0.03059(11) 0.02456(11) 0.00261(9) 0.00504(9) 0.00582(9) P9 0.0186(7) 0.0197(6) 0.0268(7) 0.0012(5) -0.0024(5) 0.0013(5) Te9 0.0316(2) 0.0332(2) 0.0301(2) -0.00039(16) -0.00018(16) 0.01394(16) C49 0.020(3) 0.020(3) 0.050(4) -0.002(2) -0.002(3) -0.001(2) C50 0.044(4) 0.032(3) 0.066(5) 0.012(3) 0.013(4) -0.008(3) C51 0.035(4) 0.027(3) 0.074(5) -0.005(3) -0.014(3) -0.003(3) C52 0.030(3) 0.028(3) 0.024(3) 0.000(2) -0.004(2) 0.005(2) C53 0.037(4) 0.059(5) 0.043(4) 0.011(3) -0.015(3) 0.007(3) C54 0.065(5) 0.043(4) 0.034(4) 0.012(3) -0.005(3) -0.014(3) N5 0.024(3) 0.029(2) 0.030(3) 0.000(2) 0.000(2) 0.0051(19) P10 0.0175(7) 0.0230(7) 0.0212(7) 0.0045(5) 0.0010(5) 0.0006(5) Te10 0.0283(2) 0.0388(2) 0.02440(18) 0.01171(16) 0.00647(15) 0.01279(16) C55 0.026(3) 0.026(3) 0.022(3) 0.007(2) -0.002(2) -0.007(2) C56 0.021(3) 0.049(4) 0.043(4) 0.006(3) -0.001(3) -0.012(3) C57 0.033(3) 0.024(3) 0.042(4) 0.011(3) 0.004(3) -0.003(2) C58 0.021(3) 0.033(3) 0.033(3) -0.001(2) -0.003(2) 0.007(2) C59 0.045(4) 0.061(5) 0.034(4) -0.002(3) 0.009(3) 0.008(3) C60 0.036(4) 0.028(3) 0.045(4) -0.002(3) -0.007(3) 0.014(3) P11 0.0222(7) 0.0215(6) 0.0210(7) 0.0036(5) 0.0011(5) 0.0016(5) Te11 0.0319(2) 0.02664(18) 0.02320(18) 0.00086(14) 0.00175(15) -0.00476(15) C61 0.035(3) 0.024(3) 0.031(3) 0.007(2) -0.004(3) 0.006(2) C62 0.034(4) 0.041(4) 0.054(4) 0.006(3) -0.004(3) 0.001(3) C63 0.042(4) 0.031(3) 0.047(4) 0.009(3) -0.018(3) -0.006(3) C64 0.031(3) 0.038(3) 0.022(3) 0.006(2) 0.006(2) 0.001(3) C65 0.041(4) 0.064(5) 0.039(4) 0.019(3) 0.016(3) 0.009(3) C66 0.054(4) 0.040(4) 0.035(4) 0.015(3) 0.010(3) -0.007(3) N6 0.034(3) 0.022(2) 0.021(2) 0.0046(18) 0.0039(19) 0.0041(19) P12 0.0284(8) 0.0200(6) 0.0219(7) 0.0024(5) 0.0013(6) 0.0035(5) Te12 0.0357(2) 0.02676(19) 0.02713(19) 0.00422(15) 0.00830(16) -0.00006(15) C67 0.043(4) 0.022(3) 0.037(3) 0.003(2) 0.001(3) 0.004(3) C68 0.063(5) 0.051(4) 0.029(3) -0.016(3) 0.002(3) 0.012(4) C69 0.042(4) 0.034(3) 0.042(4) -0.003(3) -0.014(3) -0.003(3) C70 0.032(3) 0.032(3) 0.032(3) 0.006(2) 0.000(3) 0.008(2) C71 0.045(4) 0.035(4) 0.052(4) 0.012(3) -0.009(3) 0.012(3) C72 0.030(3) 0.037(3) 0.054(4) 0.000(3) -0.006(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 Hg1 Te1 2.7788(10) . ? Hg1 Te2 2.7940(9) . ? Hg1 Te4 2.8047(9) . ? Hg1 Te3 2.8088(9) . ? Te1 P1 2.4441(16) . ? P1 N1 1.583(5) . ? P1 C4 1.821(6) . ? P1 C1 1.858(7) . ? C1 C2 1.511(10) . ? C1 C3 1.522(9) . ? C4 C6 1.526(11) . ? C4 C5 1.532(10) . ? N1 P2 1.586(5) . ? P2 C10 1.832(6) . ? P2 C7 1.834(6) . ? P2 Te2 2.4138(17) . ? C7 C8 1.526(9) . ? C7 C9 1.526(8) . ? C10 C11 1.524(8) . ? C10 C12 1.539(9) . ? Te3 P3 2.4181(16) . ? P3 N2 1.573(5) . ? P3 C13 1.829(6) . ? P3 C16 1.844(6) . ? C13 C14 1.528(8) . ? C13 C15 1.536(9) . ? C16 C17 1.522(10) . ? C16 C18 1.529(9) . ? N2 P4 1.590(5) . ? P4 C19 1.839(6) . ? P4 C22 1.845(6) . ? P4 Te4 2.4244(17) . ? C19 C20 1.506(9) . ? C19 C21 1.543(9) . ? C22 C24 1.514(9) . ? C22 C23 1.532(9) . ? Hg2 Te5 2.7689(10) . ? Hg2 Te6 2.7784(9) . ? Hg2 Te7 2.7888(9) . ? Hg2 Te8 2.8174(8) . ? P5 N3 1.588(5) . ? P5 C28 1.831(6) . ? P5 C25 1.832(6) . ? P5 Te5 2.4210(15) . ? C25 C27 1.524(9) . ? C25 C26 1.533(9) . ? C28 C30 1.526(9) . ? C28 C29 1.527(8) . ? N3 P6 1.582(5) . ? P6 C34 1.825(6) . ? P6 C31 1.835(5) . ? P6 Te6 2.4230(16) . ? C31 C33 1.518(8) . ? C31 C32 1.531(9) . ? C34 C36 1.504(9) . ? C34 C35 1.529(8) . ? P7 N4 1.593(5) . ? P7 C40 1.836(6) . ? P7 C37 1.842(5) . ? P7 Te7 2.4141(16) . ? C37 C38 1.501(9) . ? C37 C39 1.540(8) . ? C40 C42 1.505(8) . ? C40 C41 1.544(8) . ? N4 P8 1.567(5) . ? P8 C43 1.840(6) . ? P8 C46 1.844(6) . ? P8 Te8 2.4277(16) . ? C43 C45 1.523(10) . ? C43 C44 1.532(9) . ? C46 C48 1.506(8) . ? C46 C47 1.518(10) . ? Hg3 Te9 2.7806(9) . ? Hg3 Te10 2.7885(9) . ? Hg3 Te11 2.8080(9) . ? Hg3 Te12 2.8162(10) . ? P9 N5 1.588(5) . ? P9 C49 1.825(6) . ? P9 C52 1.833(6) . ? P9 Te9 2.4330(17) . ? C49 C50 1.519(9) . ? C49 C51 1.535(9) . ? C52 C53 1.512(9) . ? C52 C54 1.522(8) . ? N5 P10 1.580(5) . ? P10 C55 1.825(5) . ? P10 C58 1.836(6) . ? P10 Te10 2.4181(15) . ? C55 C57 1.520(8) . ? C55 C56 1.530(8) . ? C58 C60 1.522(8) . ? C58 C59 1.532(9) . ? P11 N6 1.584(5) . ? P11 C64 1.835(6) . ? P11 C61 1.838(6) . ? P11 Te11 2.4275(16) . ? C61 C62 1.521(9) . ? C61 C63 1.529(8) . ? C64 C66 1.523(8) . ? C64 C65 1.523(9) . ? N6 P12 1.585(4) . ? P12 C70 1.832(6) . ? P12 C67 1.836(6) . ? P12 Te12 2.4238(16) . ? C67 C69 1.516(9) . ? C67 C68 1.526(9) . ? C70 C72 1.521(9) . ? C70 C71 1.540(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te1 Hg1 Te2 113.73(2) . . ? Te1 Hg1 Te4 105.47(3) . . ? Te2 Hg1 Te4 110.92(3) . . ? Te1 Hg1 Te3 114.54(3) . . ? Te2 Hg1 Te3 98.53(3) . . ? Te4 Hg1 Te3 113.86(2) . . ? P1 Te1 Hg1 100.05(4) . . ? N1 P1 C4 109.1(3) . . ? N1 P1 C1 106.5(3) . . ? C4 P1 C1 106.2(3) . . ? N1 P1 Te1 120.83(18) . . ? C4 P1 Te1 107.3(2) . . ? C1 P1 Te1 106.0(2) . . ? C2 C1 C3 112.0(6) . . ? C2 C1 P1 111.1(4) . . ? C3 C1 P1 112.3(5) . . ? C6 C4 C5 111.8(6) . . ? C6 C4 P1 109.0(5) . . ? C5 C4 P1 111.8(5) . . ? P1 N1 P2 146.6(3) . . ? N1 P2 C10 109.4(3) . . ? N1 P2 C7 106.8(3) . . ? C10 P2 C7 106.2(3) . . ? N1 P2 Te2 118.33(18) . . ? C10 P2 Te2 110.3(2) . . ? C7 P2 Te2 105.01(19) . . ? P2 Te2 Hg1 98.63(4) . . ? C8 C7 C9 110.4(5) . . ? C8 C7 P2 111.6(4) . . ? C9 C7 P2 111.0(4) . . ? C11 C10 C12 110.4(6) . . ? C11 C10 P2 112.1(4) . . ? C12 C10 P2 112.6(4) . . ? P3 Te3 Hg1 98.29(5) . . ? N2 P3 C13 109.2(3) . . ? N2 P3 C16 106.9(3) . . ? C13 P3 C16 105.9(3) . . ? N2 P3 Te3 119.46(19) . . ? C13 P3 Te3 108.8(2) . . ? C16 P3 Te3 105.7(2) . . ? C14 C13 C15 109.9(5) . . ? C14 C13 P3 113.8(5) . . ? C15 C13 P3 111.0(4) . . ? C17 C16 C18 110.4(6) . . ? C17 C16 P3 109.4(5) . . ? C18 C16 P3 111.3(5) . . ? P3 N2 P4 148.2(3) . . ? N2 P4 C19 106.6(3) . . ? N2 P4 C22 109.8(3) . . ? C19 P4 C22 105.9(3) . . ? N2 P4 Te4 118.25(18) . . ? C19 P4 Te4 106.1(2) . . ? C22 P4 Te4 109.3(2) . . ? P4 Te4 Hg1 97.91(4) . . ? C20 C19 C21 111.0(6) . . ? C20 C19 P4 111.0(4) . . ? C21 C19 P4 110.4(4) . . ? C24 C22 C23 111.5(6) . . ? C24 C22 P4 111.8(4) . . ? C23 C22 P4 111.9(5) . . ? Te5 Hg2 Te6 114.66(2) . . ? Te5 Hg2 Te7 102.78(3) . . ? Te6 Hg2 Te7 109.79(2) . . ? Te5 Hg2 Te8 115.19(3) . . ? Te6 Hg2 Te8 101.12(3) . . ? Te7 Hg2 Te8 113.65(3) . . ? N3 P5 C28 107.1(3) . . ? N3 P5 C25 109.0(3) . . ? C28 P5 C25 106.0(3) . . ? N3 P5 Te5 119.42(17) . . ? C28 P5 Te5 106.0(2) . . ? C25 P5 Te5 108.6(2) . . ? P5 Te5 Hg2 98.13(5) . . ? C27 C25 C26 112.2(6) . . ? C27 C25 P5 111.2(4) . . ? C26 C25 P5 112.4(5) . . ? C30 C28 C29 111.1(6) . . ? C30 C28 P5 111.8(4) . . ? C29 C28 P5 111.0(4) . . ? P6 N3 P5 147.4(3) . . ? N3 P6 C34 110.4(3) . . ? N3 P6 C31 106.8(3) . . ? C34 P6 C31 106.0(3) . . ? N3 P6 Te6 119.81(18) . . ? C34 P6 Te6 107.9(2) . . ? C31 P6 Te6 104.96(19) . . ? P6 Te6 Hg2 99.06(4) . . ? C33 C31 C32 111.8(5) . . ? C33 C31 P6 110.5(4) . . ? C32 C31 P6 113.6(4) . . ? C36 C34 C35 111.2(5) . . ? C36 C34 P6 112.2(4) . . ? C35 C34 P6 111.3(4) . . ? N4 P7 C40 110.2(3) . . ? N4 P7 C37 106.3(3) . . ? C40 P7 C37 106.1(3) . . ? N4 P7 Te7 118.24(19) . . ? C40 P7 Te7 109.39(19) . . ? C37 P7 Te7 105.83(19) . . ? P7 Te7 Hg2 98.26(4) . . ? C38 C37 C39 111.5(5) . . ? C38 C37 P7 111.4(4) . . ? C39 C37 P7 110.2(4) . . ? C42 C40 C41 110.6(5) . . ? C42 C40 P7 112.6(4) . . ? C41 C40 P7 111.9(4) . . ? P8 N4 P7 146.2(3) . . ? N4 P8 C43 109.7(3) . . ? N4 P8 C46 105.2(3) . . ? C43 P8 C46 106.4(3) . . ? N4 P8 Te8 120.72(18) . . ? C43 P8 Te8 107.5(2) . . ? C46 P8 Te8 106.5(2) . . ? P8 Te8 Hg2 98.05(4) . . ? C45 C43 C44 111.6(6) . . ? C45 C43 P8 110.5(4) . . ? C44 C43 P8 111.1(5) . . ? C48 C46 C47 110.2(6) . . ? C48 C46 P8 113.8(5) . . ? C47 C46 P8 110.4(4) . . ? Te9 Hg3 Te10 114.65(3) . . ? Te9 Hg3 Te11 114.94(2) . . ? Te10 Hg3 Te11 98.96(3) . . ? Te9 Hg3 Te12 106.65(3) . . ? Te10 Hg3 Te12 108.59(3) . . ? Te11 Hg3 Te12 112.97(2) . . ? N5 P9 C49 109.7(3) . . ? N5 P9 C52 105.4(3) . . ? C49 P9 C52 107.3(3) . . ? N5 P9 Te9 120.14(19) . . ? C49 P9 Te9 106.6(2) . . ? C52 P9 Te9 107.13(19) . . ? P9 Te9 Hg3 99.02(4) . . ? C50 C49 C51 111.4(5) . . ? C50 C49 P9 111.0(4) . . ? C51 C49 P9 111.5(4) . . ? C53 C52 C54 110.8(5) . . ? C53 C52 P9 113.2(4) . . ? C54 C52 P9 111.3(4) . . ? P10 N5 P9 147.1(3) . . ? N5 P10 C55 110.7(3) . . ? N5 P10 C58 106.6(3) . . ? C55 P10 C58 106.3(3) . . ? N5 P10 Te10 118.68(19) . . ? C55 P10 Te10 108.48(18) . . ? C58 P10 Te10 105.37(19) . . ? P10 Te10 Hg3 97.50(4) . . ? C57 C55 C56 110.7(5) . . ? C57 C55 P10 112.7(4) . . ? C56 C55 P10 111.9(4) . . ? C60 C58 C59 111.1(5) . . ? C60 C58 P10 110.4(4) . . ? C59 C58 P10 111.7(4) . . ? N6 P11 C64 105.9(3) . . ? N6 P11 C61 110.5(3) . . ? C64 P11 C61 105.6(3) . . ? N6 P11 Te11 118.76(18) . . ? C64 P11 Te11 106.4(2) . . ? C61 P11 Te11 108.7(2) . . ? P11 Te11 Hg3 99.48(4) . . ? C62 C61 C63 112.5(5) . . ? C62 C61 P11 111.5(4) . . ? C63 C61 P11 111.1(4) . . ? C66 C64 C65 111.3(6) . . ? C66 C64 P11 113.5(4) . . ? C65 C64 P11 110.3(4) . . ? P11 N6 P12 147.1(3) . . ? N6 P12 C70 109.9(3) . . ? N6 P12 C67 105.9(3) . . ? C70 P12 C67 105.6(3) . . ? N6 P12 Te12 118.97(18) . . ? C70 P12 Te12 109.6(2) . . ? C67 P12 Te12 106.0(2) . . ? P12 Te12 Hg3 97.31(5) . . ? C69 C67 C68 111.0(6) . . ? C69 C67 P12 111.5(4) . . ? C68 C67 P12 110.2(5) . . ? C72 C70 C71 110.9(5) . . ? C72 C70 P12 112.2(4) . . ? C71 C70 P12 112.8(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.137 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.158 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 271001' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 N3 P6 Sb Te6' _chemical_formula_sum 'C36 H84 N3 P6 Sb Te6' _chemical_formula_weight 1632.23 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.817(5) _cell_length_b 13.084(3) _cell_length_c 20.050(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.10(3) _cell_angle_gamma 90.00 _cell_volume 5737(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 3.665 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8980 _exptl_absorpt_process_details ? _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 47603 _diffrn_reflns_av_R_equivalents 0.10 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5051 _reflns_number_gt 4001 _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^)+(0.0301P)^2^+45.1915P] 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 5051 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.0000 0.97500(4) 0.2500 0.01992(14) Uani 1 2 d S . . Te1 Te 0.085251(19) 0.81320(3) 0.36652(2) 0.02680(12) Uani 1 1 d . . . P1 P 0.06706(7) 0.64123(13) 0.31266(9) 0.0218(4) Uani 1 1 d . . . N1 N 0.0000 0.6032(6) 0.2500 0.0256(17) Uani 1 2 d S . . C1 C 0.1834(3) 0.6246(6) 0.3323(5) 0.048(2) Uani 1 1 d . . . H1A H 0.2058 0.6129 0.3060 0.072 Uiso 1 1 calc R . . H1B H 0.1945 0.5718 0.3724 0.072 Uiso 1 1 calc R . . H1C H 0.1941 0.6920 0.3574 0.072 Uiso 1 1 calc R . . C2 C 0.1150(3) 0.6201(5) 0.2720(4) 0.0307(16) Uani 1 1 d . . . H2A H 0.1059 0.5495 0.2494 0.037 Uiso 1 1 calc R . . C3 C 0.0970(3) 0.6933(6) 0.2041(4) 0.0416(19) Uani 1 1 d . . . H3A H 0.1143 0.6694 0.1736 0.062 Uiso 1 1 calc R . . H3B H 0.1127 0.7617 0.2249 0.062 Uiso 1 1 calc R . . H3C H 0.0523 0.6959 0.1700 0.062 Uiso 1 1 calc R . . C4 C 0.0983(4) 0.4457(5) 0.3753(4) 0.046(2) Uani 1 1 d . . . H4A H 0.1160 0.4026 0.4223 0.068 Uiso 1 1 calc R . . H4B H 0.1233 0.4408 0.3519 0.068 Uiso 1 1 calc R . . H4C H 0.0566 0.4227 0.3370 0.068 Uiso 1 1 calc R . . C5 C 0.0967(3) 0.5564(5) 0.3979(4) 0.0286(16) Uani 1 1 d . . . H5A H 0.1396 0.5778 0.4375 0.034 Uiso 1 1 calc R . . C6 C 0.0592(4) 0.5652(6) 0.4366(4) 0.0436(19) Uani 1 1 d . . . H6A H 0.0753 0.5174 0.4809 0.065 Uiso 1 1 calc R . . H6B H 0.0164 0.5487 0.3979 0.065 Uiso 1 1 calc R . . H6C H 0.0620 0.6351 0.4558 0.065 Uiso 1 1 calc R . . Te2 Te 0.103899(19) 1.12278(4) 0.36302(2) 0.02784(12) Uani 1 1 d . . . P2 P 0.17769(7) 1.10561(13) 0.32238(9) 0.0216(4) Uani 1 1 d . . . C7 C 0.2271(4) 0.9335(6) 0.2885(4) 0.0438(19) Uani 1 1 d . . . H7A H 0.2319 0.8590 0.2928 0.066 Uiso 1 1 calc R . . H7B H 0.2670 0.9657 0.3085 0.066 Uiso 1 1 calc R . . H7C H 0.1993 0.9524 0.2332 0.066 Uiso 1 1 calc R . . C8 C 0.2005(3) 0.9700(5) 0.3371(4) 0.0292(15) Uani 1 1 d . . . H8A H 0.1618 0.9303 0.3171 0.035 Uiso 1 1 calc R . . C9 C 0.2408(3) 0.9433(6) 0.4244(4) 0.0426(19) Uani 1 1 d . . . H9A H 0.2441 0.8689 0.4306 0.064 Uiso 1 1 calc R . . H9B H 0.2227 0.9714 0.4527 0.064 Uiso 1 1 calc R . . H9C H 0.2817 0.9726 0.4458 0.064 Uiso 1 1 calc R . . C10 C 0.2968(3) 1.1712(7) 0.3773(4) 0.046(2) Uani 1 1 d . . . H10A H 0.3307 1.2156 0.4140 0.069 Uiso 1 1 calc R . . H10B H 0.2826 1.1912 0.3231 0.069 Uiso 1 1 calc R . . H10C H 0.3107 1.1000 0.3859 0.069 Uiso 1 1 calc R . . C11 C 0.2447(3) 1.1819(6) 0.3912(4) 0.0312(16) Uani 1 1 d . . . H11A H 0.2596 1.1565 0.4456 0.037 Uiso 1 1 calc R . . C12 C 0.2287(3) 1.2941(6) 0.3883(4) 0.0440(19) Uani 1 1 d . . . H12A H 0.2642 1.3310 0.4302 0.066 Uiso 1 1 calc R . . H12B H 0.1943 1.3009 0.3959 0.066 Uiso 1 1 calc R . . H12C H 0.2173 1.3227 0.3371 0.066 Uiso 1 1 calc R . . N2 N 0.1575(2) 1.1434(4) 0.2361(3) 0.0216(11) Uani 1 1 d . . . P3 P 0.09449(7) 1.13187(12) 0.15246(9) 0.0193(3) Uani 1 1 d . . . Te3 Te 0.036033(19) 0.97496(3) 0.12740(2) 0.02415(12) Uani 1 1 d . . . C13 C 0.1562(3) 1.2323(6) 0.0933(4) 0.0357(17) Uani 1 1 d . . . H13A H 0.1666 1.2352 0.0529 0.054 Uiso 1 1 calc R . . H13B H 0.1937 1.2261 0.1454 0.054 Uiso 1 1 calc R . . H13C H 0.1345 1.2948 0.0912 0.054 Uiso 1 1 calc R . . C14 C 0.1152(3) 1.1397(5) 0.0782(3) 0.0228(14) Uani 1 1 d . . . H14A H 0.0767 1.1491 0.0257 0.027 Uiso 1 1 calc R . . C15 C 0.1463(3) 1.0425(5) 0.0746(4) 0.0331(17) Uani 1 1 d . . . H15A H 0.1533 1.0478 0.0313 0.050 Uiso 1 1 calc R . . H15B H 0.1199 0.9836 0.0658 0.050 Uiso 1 1 calc R . . H15C H 0.1855 1.0338 0.1244 0.050 Uiso 1 1 calc R . . C16 C 0.0742(4) 1.3395(5) 0.1723(5) 0.050(2) Uani 1 1 d . . . H16A H 0.0468 1.3849 0.1783 0.074 Uiso 1 1 calc R . . H16B H 0.0851 1.3715 0.1371 0.074 Uiso 1 1 calc R . . H16C H 0.1114 1.3275 0.2238 0.074 Uiso 1 1 calc R . . C17 C 0.0419(3) 1.2374(5) 0.1370(4) 0.0292(15) Uani 1 1 d . . . H17A H 0.0220 1.2180 0.1665 0.035 Uiso 1 1 calc R . . C18 C -0.0101(3) 1.2481(5) 0.0505(4) 0.0367(17) Uani 1 1 d . . . H18A H -0.0425 1.2912 0.0471 0.055 Uiso 1 1 calc R . . H18B H -0.0268 1.1804 0.0288 0.055 Uiso 1 1 calc R . . H18C H 0.0056 1.2796 0.0204 0.055 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 Sb1 0.0190(3) 0.0232(3) 0.0187(3) 0.000 0.0108(3) 0.000 Te1 0.0260(2) 0.0254(2) 0.0213(2) -0.00195(18) 0.00734(19) 0.00137(19) P1 0.0179(8) 0.0243(9) 0.0212(8) 0.0007(7) 0.0089(7) 0.0019(7) N1 0.020(4) 0.025(4) 0.025(4) 0.000 0.007(3) 0.000 C1 0.033(4) 0.050(5) 0.066(5) 0.003(4) 0.030(4) 0.007(4) C2 0.025(4) 0.032(4) 0.038(4) 0.002(3) 0.018(3) 0.006(3) C3 0.039(4) 0.056(5) 0.045(4) -0.006(4) 0.032(4) 0.000(4) C4 0.057(5) 0.027(4) 0.051(5) 0.017(4) 0.028(4) 0.016(4) C5 0.024(4) 0.029(4) 0.022(3) 0.008(3) 0.005(3) 0.005(3) C6 0.057(5) 0.046(5) 0.026(4) 0.004(3) 0.021(4) -0.003(4) Te2 0.0242(2) 0.0387(3) 0.0245(2) -0.0076(2) 0.01556(19) -0.0053(2) P2 0.0171(8) 0.0312(10) 0.0157(8) 0.0014(7) 0.0082(7) 0.0004(7) C7 0.049(5) 0.039(5) 0.048(5) 0.004(4) 0.029(4) 0.014(4) C8 0.025(4) 0.031(4) 0.025(3) 0.009(3) 0.008(3) 0.004(3) C9 0.039(4) 0.043(5) 0.026(4) 0.008(3) 0.004(3) 0.005(4) C10 0.022(4) 0.072(6) 0.043(4) -0.010(4) 0.016(4) -0.007(4) C11 0.019(3) 0.050(5) 0.020(3) -0.005(3) 0.007(3) -0.009(3) C12 0.034(4) 0.046(5) 0.045(5) -0.017(4) 0.015(4) -0.010(4) N2 0.018(3) 0.024(3) 0.019(3) -0.005(2) 0.008(2) -0.001(2) P3 0.0188(8) 0.0223(9) 0.0160(8) -0.0004(7) 0.0086(7) -0.0016(7) Te3 0.0287(2) 0.0267(2) 0.0207(2) -0.00419(18) 0.01561(19) -0.0076(2) C13 0.029(4) 0.049(5) 0.030(4) 0.003(3) 0.016(3) -0.013(3) C14 0.023(3) 0.031(4) 0.012(3) 0.005(3) 0.007(3) -0.006(3) C15 0.037(4) 0.041(4) 0.032(4) -0.005(3) 0.026(3) -0.005(3) C16 0.043(5) 0.030(4) 0.059(5) -0.005(4) 0.017(4) 0.004(4) C17 0.024(4) 0.031(4) 0.029(4) -0.003(3) 0.011(3) 0.000(3) C18 0.036(4) 0.034(4) 0.030(4) 0.004(3) 0.010(3) 0.009(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 Sb1 Te1 3.0526(10) . ? Sb1 Te3 3.0558(7) . ? Sb1 Te2 3.0996(11) . ? Te1 P1 2.4310(17) . ? P1 N1 1.585(3) . ? P1 C2 1.829(6) . ? P1 C5 1.830(6) . ? C1 C2 1.522(9) . ? C2 C3 1.521(9) . ? C4 C5 1.525(9) . ? C5 C6 1.533(9) . ? Te2 P2 2.4482(17) . ? P2 N2 1.596(5) . ? P2 C11 1.832(6) . ? P2 C8 1.844(7) . ? C7 C8 1.537(9) . ? C8 C9 1.527(8) . ? C10 C11 1.518(9) . ? C11 C12 1.516(10) . ? N2 P3 1.607(5) . ? P3 C14 1.832(6) . ? P3 C17 1.843(7) . ? P3 Te3 2.4369(17) . ? C13 C14 1.529(8) . ? C14 C15 1.525(9) . ? C16 C17 1.534(9) . ? C17 C18 1.536(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te1 Sb1 Te1 92.18(4) 2 . ? Te1 Sb1 Te3 77.772(19) 2 . ? Te1 Sb1 Te3 102.22(2) . . ? Te3 Sb1 Te3 179.98(3) . 2 ? Te1 Sb1 Te2 169.715(15) 2 . ? Te1 Sb1 Te2 83.18(3) . . ? Te3 Sb1 Te2 94.19(2) . . ? Te3 Sb1 Te2 85.82(2) 2 . ? Te2 Sb1 Te2 102.81(4) . 2 ? P1 Te1 Sb1 114.29(5) . . ? N1 P1 C2 108.2(2) . . ? N1 P1 C5 106.8(3) . . ? C2 P1 C5 106.2(3) . . ? N1 P1 Te1 120.9(2) . . ? C2 P1 Te1 108.7(2) . . ? C5 P1 Te1 105.1(2) . . ? P1 N1 P1 143.4(5) . 2 ? C3 C2 C1 111.1(6) . . ? C3 C2 P1 110.3(4) . . ? C1 C2 P1 114.5(5) . . ? C4 C5 C6 110.3(6) . . ? C4 C5 P1 111.2(5) . . ? C6 C5 P1 111.4(5) . . ? P2 Te2 Sb1 102.92(4) . . ? N2 P2 C11 106.4(3) . . ? N2 P2 C8 111.4(3) . . ? C11 P2 C8 108.1(3) . . ? N2 P2 Te2 117.90(19) . . ? C11 P2 Te2 106.8(2) . . ? C8 P2 Te2 105.8(2) . . ? C9 C8 C7 113.1(6) . . ? C9 C8 P2 111.6(5) . . ? C7 C8 P2 114.2(5) . . ? C12 C11 C10 109.4(6) . . ? C12 C11 P2 111.7(5) . . ? C10 C11 P2 112.7(5) . . ? P2 N2 P3 132.0(3) . . ? N2 P3 C14 105.8(3) . . ? N2 P3 C17 110.6(3) . . ? C14 P3 C17 109.2(3) . . ? N2 P3 Te3 117.8(2) . . ? C14 P3 Te3 107.2(2) . . ? C17 P3 Te3 106.0(2) . . ? P3 Te3 Sb1 104.71(4) . . ? C15 C14 C13 110.1(5) . . ? C15 C14 P3 112.3(4) . . ? C13 C14 P3 110.7(4) . . ? C16 C17 C18 112.1(6) . . ? C16 C17 P3 113.8(5) . . ? C18 C17 P3 112.5(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.242 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.153 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 271002' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 Bi N3 P6 Te6' _chemical_formula_sum 'C36 H84 Bi N3 P6 Te6' _chemical_formula_weight 1719.46 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' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.156(4) _cell_length_b 13.360(3) _cell_length_c 20.560(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.24(3) _cell_angle_gamma 90.00 _cell_volume 5872(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 6.114 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7105 _exptl_absorpt_correction_T_max 0.8875 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 17827 _diffrn_reflns_av_R_equivalents 0.153 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 21.96 _reflns_number_total 3573 _reflns_number_gt 2239 _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^)+(0.0236P)^2^+22.2182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 3573 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Bi1 Bi 0.0000 0.15002(6) 0.2500 0.0457(3) Uani 1 2 d S . . Te1 Te -0.01657(5) 0.31860(7) 0.35576(5) 0.0604(3) Uani 1 1 d . . . Te2 Te -0.00464(5) -0.00629(8) 0.13730(5) 0.0625(3) Uani 1 1 d . . . Te3 Te -0.14515(5) 0.14077(9) 0.23198(5) 0.0685(4) Uani 1 1 d . . . P1 P 0.03309(19) 0.4648(3) 0.32130(19) 0.0505(10) Uani 1 1 d . . . C1 C -0.0305(10) 0.6080(16) 0.3721(11) 0.148(10) Uani 1 1 d . . . H1A H -0.0299 0.6624 0.4028 0.223 Uiso 1 1 calc R . . H1B H -0.0576 0.5562 0.3802 0.223 Uiso 1 1 calc R . . H1C H -0.0456 0.6317 0.3266 0.223 Uiso 1 1 calc R . . C2 C 0.0359(8) 0.5663(11) 0.3826(8) 0.068(5) Uani 1 1 d . . . H2A H 0.0608 0.6201 0.3702 0.081 Uiso 1 1 calc R . . C3 C 0.0682(12) 0.5392(15) 0.4556(9) 0.129(8) Uani 1 1 d . . . H3A H 0.0686 0.5966 0.4838 0.194 Uiso 1 1 calc R . . H3B H 0.1103 0.5184 0.4589 0.194 Uiso 1 1 calc R . . H3C H 0.0458 0.4856 0.4699 0.194 Uiso 1 1 calc R . . C4 C 0.1549(10) 0.3851(14) 0.3876(12) 0.125(8) Uani 1 1 d . . . H4A H 0.1949 0.3694 0.3804 0.187 Uiso 1 1 calc R . . H4B H 0.1359 0.3251 0.3986 0.187 Uiso 1 1 calc R . . H4C H 0.1603 0.4320 0.4241 0.187 Uiso 1 1 calc R . . C5 C 0.1133(7) 0.4307(12) 0.3242(8) 0.067(5) Uani 1 1 d . . . H5A H 0.1098 0.3794 0.2893 0.081 Uiso 1 1 calc R . . C6 C 0.1479(8) 0.5169(16) 0.3022(10) 0.115(8) Uani 1 1 d . . . H6A H 0.1896 0.4962 0.3033 0.172 Uiso 1 1 calc R . . H6B H 0.1496 0.5725 0.3322 0.172 Uiso 1 1 calc R . . H6C H 0.1263 0.5366 0.2572 0.172 Uiso 1 1 calc R . . N1 N 0.0000 0.5123(11) 0.2500 0.051(4) Uani 1 2 d S . . P2 P -0.11150(18) 0.0052(3) 0.06472(18) 0.0455(9) Uani 1 1 d . . . C7 C -0.1804(9) -0.0745(14) -0.0592(8) 0.095(6) Uani 1 1 d . . . H7A H -0.1806 -0.1194 -0.0957 0.142 Uiso 1 1 calc R . . H7B H -0.1882 -0.0075 -0.0764 0.142 Uiso 1 1 calc R . . H7C H -0.2124 -0.0938 -0.0381 0.142 Uiso 1 1 calc R . . C8 C -0.1163(8) -0.0787(10) -0.0073(8) 0.064(5) Uani 1 1 d . . . H8A H -0.0848 -0.0569 -0.0299 0.077 Uiso 1 1 calc R . . C9 C -0.1010(9) -0.1847(12) 0.0162(9) 0.099(7) Uani 1 1 d . . . H9A H -0.1032 -0.2271 -0.0221 0.148 Uiso 1 1 calc R . . H9B H -0.1304 -0.2074 0.0399 0.148 Uiso 1 1 calc R . . H9C H -0.0595 -0.1871 0.0457 0.148 Uiso 1 1 calc R . . C10 C -0.1885(8) 0.1620(14) 0.0019(9) 0.097(6) Uani 1 1 d . . . H10A H -0.1903 0.2297 -0.0140 0.145 Uiso 1 1 calc R . . H10B H -0.2115 0.1566 0.0353 0.145 Uiso 1 1 calc R . . H10C H -0.2064 0.1181 -0.0351 0.145 Uiso 1 1 calc R . . C11 C -0.1214(7) 0.1331(9) 0.0326(7) 0.047(4) Uani 1 1 d . . . H11A H -0.1078 0.1756 0.0727 0.056 Uiso 1 1 calc R . . C12 C -0.0770(8) 0.1592(12) -0.0111(7) 0.075(5) Uani 1 1 d . . . H12A H -0.0839 0.2272 -0.0264 0.112 Uiso 1 1 calc R . . H12B H -0.0848 0.1152 -0.0493 0.112 Uiso 1 1 calc R . . H12C H -0.0344 0.1516 0.0150 0.112 Uiso 1 1 calc R . . N2 N -0.1673(6) -0.0239(8) 0.0962(6) 0.057(3) Uani 1 1 d . . . P3 P -0.17974(19) -0.0136(3) 0.16880(19) 0.0572(11) Uani 1 1 d . . . C13 C -0.1693(10) -0.1266(16) 0.2874(9) 0.125(8) Uani 1 1 d . . . H13A H -0.1479 -0.1801 0.3154 0.187 Uiso 1 1 calc R . . H13B H -0.2133 -0.1406 0.2737 0.187 Uiso 1 1 calc R . . H13C H -0.1622 -0.0650 0.3123 0.187 Uiso 1 1 calc R . . C14 C -0.1447(10) -0.1174(14) 0.2260(9) 0.096(6) Uani 1 1 d . . . H14A H -0.1013 -0.0957 0.2446 0.115 Uiso 1 1 calc R . . C15 C -0.1383(13) -0.2105(14) 0.1947(10) 0.158(12) Uani 1 1 d . . . H15A H -0.1184 -0.2581 0.2285 0.237 Uiso 1 1 calc R . . H15B H -0.1134 -0.2013 0.1635 0.237 Uiso 1 1 calc R . . H15C H -0.1789 -0.2348 0.1711 0.237 Uiso 1 1 calc R . . C16 C -0.2951(8) 0.0695(19) 0.1162(11) 0.127(9) Uani 1 1 d . . . H16A H -0.3394 0.0650 0.1107 0.191 Uiso 1 1 calc R . . H16B H -0.2867 0.0700 0.0728 0.191 Uiso 1 1 calc R . . H16C H -0.2796 0.1301 0.1399 0.191 Uiso 1 1 calc R . . C17 C -0.2640(7) -0.0171(16) 0.1551(8) 0.080(6) Uani 1 1 d . . . H17A H -0.2729 -0.0152 0.1994 0.095 Uiso 1 1 calc R . . C18 C -0.2917(9) -0.1163(16) 0.1198(12) 0.136(9) Uani 1 1 d . . . H18A H -0.3363 -0.1164 0.1130 0.204 Uiso 1 1 calc R . . H18B H -0.2739 -0.1721 0.1477 0.204 Uiso 1 1 calc R . . H18C H -0.2821 -0.1215 0.0771 0.204 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 Bi1 0.0468(6) 0.0491(5) 0.0396(5) 0.000 0.0087(4) 0.000 Te1 0.0801(9) 0.0565(7) 0.0469(6) -0.0012(5) 0.0210(6) -0.0079(6) Te2 0.0504(7) 0.0834(8) 0.0495(7) -0.0144(6) 0.0058(5) 0.0177(6) Te3 0.0523(8) 0.0886(9) 0.0669(7) -0.0254(7) 0.0197(6) -0.0038(6) P1 0.056(3) 0.053(2) 0.041(2) -0.0073(19) 0.009(2) -0.001(2) C1 0.101(18) 0.19(2) 0.15(2) -0.123(18) 0.018(16) 0.043(17) C2 0.085(14) 0.052(10) 0.060(11) -0.004(8) 0.007(10) -0.003(9) C3 0.18(3) 0.129(18) 0.062(13) -0.021(13) 0.011(15) 0.009(17) C4 0.102(19) 0.098(16) 0.16(2) 0.030(16) 0.004(17) -0.014(13) C5 0.049(11) 0.084(12) 0.058(11) -0.004(9) -0.003(9) 0.016(10) C6 0.044(12) 0.19(2) 0.117(17) 0.033(17) 0.034(12) -0.004(14) N1 0.061(12) 0.060(11) 0.032(9) 0.000 0.009(9) 0.000 P2 0.046(2) 0.053(2) 0.035(2) -0.0075(19) 0.0072(18) 0.004(2) C7 0.098(16) 0.119(16) 0.041(10) -0.034(10) -0.029(11) -0.012(13) C8 0.105(15) 0.042(9) 0.053(10) -0.009(8) 0.037(11) -0.007(9) C9 0.142(19) 0.078(13) 0.087(14) -0.040(11) 0.048(14) -0.006(12) C10 0.066(14) 0.113(15) 0.098(14) 0.003(13) -0.005(11) 0.029(12) C11 0.056(11) 0.036(8) 0.048(9) -0.003(7) 0.013(8) -0.002(7) C12 0.098(15) 0.082(11) 0.052(10) 0.012(9) 0.033(10) 0.007(10) N2 0.064(9) 0.059(8) 0.048(8) 0.000(6) 0.011(7) -0.014(7) P3 0.048(3) 0.080(3) 0.045(2) -0.002(2) 0.015(2) -0.008(2) C13 0.16(2) 0.17(2) 0.056(12) 0.045(14) 0.050(13) 0.014(17) C14 0.128(19) 0.097(15) 0.054(12) 0.017(11) 0.010(12) 0.003(13) C15 0.33(4) 0.064(14) 0.094(16) 0.007(13) 0.09(2) -0.004(18) C16 0.021(11) 0.24(3) 0.113(18) -0.013(19) 0.003(12) 0.014(14) C17 0.039(11) 0.156(18) 0.045(10) 0.005(12) 0.014(9) -0.012(12) C18 0.070(15) 0.17(2) 0.16(2) -0.041(18) 0.006(15) -0.073(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 Bi1 Te2 3.1008(12) . ? Bi1 Te3 3.1415(12) . ? Bi1 Te1 3.2179(12) . ? Te1 P1 2.437(4) . ? Te2 P2 2.449(4) . ? Te3 P3 2.451(4) . ? P1 N1 1.588(7) . ? P1 C5 1.821(16) . ? P1 C2 1.841(15) . ? C1 C2 1.54(2) . ? C2 C3 1.53(2) . ? C4 C5 1.51(2) . ? C5 C6 1.52(2) . ? N1 P1 1.588(7) 2 ? P2 N2 1.587(11) . ? P2 C11 1.825(12) . ? P2 C8 1.838(14) . ? C7 C8 1.54(2) . ? C8 C9 1.51(2) . ? C10 C11 1.504(19) . ? C11 C12 1.539(17) . ? N2 P3 1.593(11) . ? P3 C17 1.815(16) . ? P3 C14 1.851(17) . ? C13 C14 1.51(2) . ? C14 C15 1.42(2) . ? C16 C17 1.47(2) . ? C17 C18 1.56(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te2 Bi1 Te2 95.33(5) . 2 ? Te2 Bi1 Te3 93.07(4) . . ? Te2 Bi1 Te3 83.89(4) 2 . ? Te3 Bi1 Te3 175.50(5) . 2 ? Te2 Bi1 Te1 171.50(3) . . ? Te2 Bi1 Te1 87.35(3) 2 . ? Te3 Bi1 Te1 79.17(4) . . ? Te3 Bi1 Te1 104.05(4) 2 . ? Te1 Bi1 Te1 91.16(4) . 2 ? P1 Te1 Bi1 102.96(9) . . ? P2 Te2 Bi1 104.49(9) . . ? P3 Te3 Bi1 105.27(10) . . ? N1 P1 C5 109.9(6) . . ? N1 P1 C2 105.3(7) . . ? C5 P1 C2 107.7(8) . . ? N1 P1 Te1 117.0(4) . . ? C5 P1 Te1 107.5(6) . . ? C2 P1 Te1 109.1(5) . . ? C3 C2 C1 114.1(17) . . ? C3 C2 P1 115.0(12) . . ? C1 C2 P1 108.1(12) . . ? C4 C5 C6 108.8(15) . . ? C4 C5 P1 119.8(13) . . ? C6 C5 P1 111.4(12) . . ? P1 N1 P1 133.0(11) . 2 ? N2 P2 C11 110.1(6) . . ? N2 P2 C8 107.1(7) . . ? C11 P2 C8 107.7(6) . . ? N2 P2 Te2 117.9(5) . . ? C11 P2 Te2 106.5(5) . . ? C8 P2 Te2 107.2(6) . . ? C9 C8 C7 110.3(15) . . ? C9 C8 P2 110.8(10) . . ? C7 C8 P2 112.7(11) . . ? C10 C11 C12 114.2(12) . . ? C10 C11 P2 113.8(11) . . ? C12 C11 P2 112.9(9) . . ? P2 N2 P3 135.0(8) . . ? N2 P3 C17 106.1(7) . . ? N2 P3 C14 112.5(7) . . ? C17 P3 C14 108.8(9) . . ? N2 P3 Te3 117.5(4) . . ? C17 P3 Te3 105.6(7) . . ? C14 P3 Te3 105.8(6) . . ? C15 C14 C13 114.0(16) . . ? C15 C14 P3 116.3(13) . . ? C13 C14 P3 114.2(14) . . ? C16 C17 C18 110.2(16) . . ? C16 C17 P3 112.3(12) . . ? C18 C17 P3 111.0(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.96 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.406 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.145 #===END