Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; Department of Chemistry University of Calgary Calgary Alberta T2N 1N4 Canada ; _publ_contact_author_name 'Prof Tristram Chivers' _publ_section_title ; Coordination chemistry of a new P,Te-centred ligand: synthesis, NMR spectra and X-ray structures of M(TePPri2NPPri2)2 (M = Zn, Cd, Hg) ; _publ_contact_author_email CHIVERS@UCALGARY.CA loop_ _publ_author_name T.Chivers 'Jamie S. Ritch' data_Compound6 _database_code_depnum_ccdc_archive 'CCDC 663951' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Te2 Zn' _chemical_formula_sum 'C24 H56 N2 P4 Te2 Zn' _chemical_formula_weight 817.16 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.869(2) _cell_length_b 12.626(3) _cell_length_c 14.968(3) _cell_angle_alpha 70.47(3) _cell_angle_beta 89.11(3) _cell_angle_gamma 81.53(3) _cell_volume 1737.5(7) _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 plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 2.552 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8219 _exptl_absorpt_correction_T_max 0.8619 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 31378 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6113 _reflns_number_gt 4653 _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^)+(0.0909P)^2^+0.3764P] 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 6113 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.28008(14) 0.08874(13) 0.22133(11) 0.0256(3) Uani 1 1 d . . . C1 C 0.1143(6) 0.0781(5) 0.1707(4) 0.0320(14) Uani 1 1 d . . . H1A H 0.0451 0.0707 0.2211 0.038 Uiso 1 1 calc R . . C2 C 0.0672(6) 0.1872(6) 0.0894(5) 0.0435(17) Uani 1 1 d . . . H2A H -0.0255 0.1862 0.0675 0.065 Uiso 1 1 calc R . . H2B H 0.1300 0.1936 0.0371 0.065 Uiso 1 1 calc R . . H2C H 0.0667 0.2524 0.1112 0.065 Uiso 1 1 calc R . . C3 C 0.1207(7) -0.0247(6) 0.1375(5) 0.0495(18) Uani 1 1 d . . . H3A H 0.0389 -0.0159 0.0979 0.074 Uiso 1 1 calc R . . H3B H 0.1246 -0.0941 0.1928 0.074 Uiso 1 1 calc R . . H3C H 0.2028 -0.0299 0.1005 0.074 Uiso 1 1 calc R . . C4 C 0.3218(6) -0.0394(5) 0.3259(4) 0.0321(14) Uani 1 1 d . . . H4A H 0.4010 -0.0257 0.3592 0.039 Uiso 1 1 calc R . . C5 C 0.2059(7) -0.0542(6) 0.3971(5) 0.0455(17) Uani 1 1 d . . . H5A H 0.2333 -0.1223 0.4524 0.068 Uiso 1 1 calc R . . H5B H 0.1225 -0.0622 0.3668 0.068 Uiso 1 1 calc R . . H5C H 0.1882 0.0126 0.4174 0.068 Uiso 1 1 calc R . . C6 C 0.3707(7) -0.1482(5) 0.3058(5) 0.0450(17) Uani 1 1 d . . . H6A H 0.4145 -0.2060 0.3634 0.068 Uiso 1 1 calc R . . H6B H 0.4371 -0.1338 0.2553 0.068 Uiso 1 1 calc R . . H6C H 0.2924 -0.1753 0.2857 0.068 Uiso 1 1 calc R . . N1 N 0.3934(5) 0.0835(4) 0.1409(3) 0.0271(11) Uani 1 1 d . . . P2 P 0.50537(15) 0.16539(13) 0.10550(11) 0.0280(4) Uani 1 1 d . . . C7 C 0.5205(6) 0.1974(6) -0.0231(4) 0.0390(15) Uani 1 1 d . . . H7A H 0.5398 0.1234 -0.0351 0.047 Uiso 1 1 calc R . . C8 C 0.3872(7) 0.2620(7) -0.0767(5) 0.053(2) Uani 1 1 d . . . H8A H 0.3960 0.2723 -0.1443 0.080 Uiso 1 1 calc R . . H8B H 0.3676 0.3365 -0.0685 0.080 Uiso 1 1 calc R . . H8C H 0.3121 0.2187 -0.0518 0.080 Uiso 1 1 calc R . . C9 C 0.6391(7) 0.2632(6) -0.0617(5) 0.0501(19) Uani 1 1 d . . . H9A H 0.6412 0.2810 -0.1306 0.075 Uiso 1 1 calc R . . H9B H 0.7257 0.2168 -0.0323 0.075 Uiso 1 1 calc R . . H9C H 0.6263 0.3340 -0.0470 0.075 Uiso 1 1 calc R . . C10 C 0.6753(6) 0.0913(6) 0.1583(5) 0.0408(17) Uani 1 1 d . . . H10A H 0.7438 0.1441 0.1332 0.049 Uiso 1 1 calc R . . C11 C 0.6767(7) 0.0595(6) 0.2655(5) 0.0493(19) Uani 1 1 d . . . H11A H 0.7708 0.0310 0.2912 0.074 Uiso 1 1 calc R . . H11B H 0.6190 0.0003 0.2922 0.074 Uiso 1 1 calc R . . H11C H 0.6411 0.1267 0.2825 0.074 Uiso 1 1 calc R . . C12 C 0.7177(8) -0.0150(7) 0.1308(6) 0.061(2) Uani 1 1 d . . . H12A H 0.8063 -0.0547 0.1620 0.092 Uiso 1 1 calc R . . H12B H 0.7257 0.0072 0.0619 0.092 Uiso 1 1 calc R . . H12C H 0.6483 -0.0655 0.1510 0.092 Uiso 1 1 calc R . . Te1 Te 0.46602(4) 0.34396(4) 0.13738(3) 0.03776(16) Uani 1 1 d . . . Zn1 Zn 0.28687(7) 0.25381(6) 0.26481(5) 0.02843(19) Uani 1 1 d . . . P3 P 0.10445(15) 0.39660(13) 0.27264(11) 0.0271(3) Uani 1 1 d . . . C13 C 0.1236(6) 0.5338(5) 0.1797(4) 0.0315(14) Uani 1 1 d . . . H13A H 0.2237 0.5391 0.1791 0.038 Uiso 1 1 calc R . . C14 C 0.0508(7) 0.6403(6) 0.1991(5) 0.0440(17) Uani 1 1 d . . . H14A H 0.0837 0.7081 0.1559 0.066 Uiso 1 1 calc R . . H14B H 0.0710 0.6337 0.2649 0.066 Uiso 1 1 calc R . . H14C H -0.0483 0.6469 0.1890 0.066 Uiso 1 1 calc R . . C15 C 0.0851(7) 0.5335(6) 0.0810(4) 0.0408(16) Uani 1 1 d . . . H15A H 0.1115 0.6007 0.0326 0.061 Uiso 1 1 calc R . . H15B H -0.0141 0.5349 0.0758 0.061 Uiso 1 1 calc R . . H15C H 0.1333 0.4647 0.0715 0.061 Uiso 1 1 calc R . . C16 C -0.0687(6) 0.3656(6) 0.2552(5) 0.0358(15) Uani 1 1 d . . . H16A H -0.0731 0.3569 0.1914 0.043 Uiso 1 1 calc R . . C17 C -0.1866(7) 0.4580(7) 0.2578(6) 0.055(2) Uani 1 1 d . . . H17A H -0.2740 0.4292 0.2598 0.082 Uiso 1 1 calc R . . H17B H -0.1863 0.5250 0.2008 0.082 Uiso 1 1 calc R . . H17C H -0.1751 0.4789 0.3143 0.082 Uiso 1 1 calc R . . C18 C -0.0888(7) 0.2533(6) 0.3283(6) 0.052(2) Uani 1 1 d . . . H18A H -0.1778 0.2340 0.3162 0.078 Uiso 1 1 calc R . . H18B H -0.0860 0.2593 0.3919 0.078 Uiso 1 1 calc R . . H18C H -0.0156 0.1937 0.3243 0.078 Uiso 1 1 calc R . . N2 N 0.1069(5) 0.4155(4) 0.3754(3) 0.0283(11) Uani 1 1 d . . . P4 P 0.22972(14) 0.36276(13) 0.45354(10) 0.0248(3) Uani 1 1 d . . . C19 C 0.1535(6) 0.3261(5) 0.5703(4) 0.0296(13) Uani 1 1 d . . . H19A H 0.0930 0.3956 0.5732 0.036 Uiso 1 1 calc R . . C20 C 0.0646(6) 0.2345(5) 0.5835(4) 0.0361(15) Uani 1 1 d . . . H20A H 0.0176 0.2221 0.6435 0.054 Uiso 1 1 calc R . . H20B H 0.1221 0.1637 0.5847 0.054 Uiso 1 1 calc R . . H20C H -0.0034 0.2583 0.5309 0.054 Uiso 1 1 calc R . . C21 C 0.2624(6) 0.2906(6) 0.6515(4) 0.0366(15) Uani 1 1 d . . . H21A H 0.2176 0.2690 0.7125 0.055 Uiso 1 1 calc R . . H21B H 0.3115 0.3545 0.6460 0.055 Uiso 1 1 calc R . . H21C H 0.3274 0.2258 0.6477 0.055 Uiso 1 1 calc R . . C22 C 0.3411(6) 0.4677(5) 0.4513(4) 0.0329(14) Uani 1 1 d . . . H22A H 0.4131 0.4313 0.5031 0.039 Uiso 1 1 calc R . . C23 C 0.2603(7) 0.5708(6) 0.4692(5) 0.0422(16) Uani 1 1 d . . . H23A H 0.3237 0.6208 0.4759 0.063 Uiso 1 1 calc R . . H23B H 0.2097 0.5456 0.5275 0.063 Uiso 1 1 calc R . . H23C H 0.1957 0.6124 0.4156 0.063 Uiso 1 1 calc R . . C24 C 0.4129(7) 0.5054(6) 0.3564(5) 0.0442(17) Uani 1 1 d . . . H24A H 0.4772 0.5567 0.3588 0.066 Uiso 1 1 calc R . . H24B H 0.3443 0.5450 0.3049 0.066 Uiso 1 1 calc R . . H24C H 0.4631 0.4385 0.3448 0.066 Uiso 1 1 calc R . . Te2 Te 0.38019(4) 0.19554(4) 0.44384(3) 0.03579(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0259(7) 0.0243(8) 0.0265(8) -0.0069(6) 0.0008(6) -0.0076(6) C1 0.029(3) 0.037(4) 0.036(4) -0.018(3) 0.006(3) -0.009(3) C2 0.032(3) 0.044(4) 0.056(5) -0.021(4) -0.015(3) 0.001(3) C3 0.053(4) 0.048(5) 0.057(5) -0.026(4) -0.009(4) -0.015(3) C4 0.029(3) 0.026(3) 0.038(4) -0.004(3) 0.002(3) -0.009(2) C5 0.051(4) 0.042(4) 0.039(4) -0.004(3) 0.009(3) -0.018(3) C6 0.053(4) 0.029(4) 0.045(4) -0.001(3) -0.003(3) -0.008(3) N1 0.027(2) 0.025(3) 0.033(3) -0.011(2) 0.004(2) -0.010(2) P2 0.0284(8) 0.0250(8) 0.0285(8) -0.0049(7) 0.0029(6) -0.0073(6) C7 0.043(4) 0.039(4) 0.034(4) -0.008(3) 0.006(3) -0.011(3) C8 0.061(5) 0.069(5) 0.028(4) -0.013(4) 0.004(3) -0.010(4) C9 0.056(4) 0.048(5) 0.038(4) -0.001(3) 0.012(3) -0.017(4) C10 0.021(3) 0.039(4) 0.053(4) -0.004(3) 0.000(3) -0.007(3) C11 0.042(4) 0.047(5) 0.046(4) 0.002(4) -0.013(3) -0.010(3) C12 0.050(4) 0.047(5) 0.067(5) -0.002(4) 0.019(4) 0.011(4) Te1 0.0461(3) 0.0295(3) 0.0411(3) -0.0120(2) 0.0099(2) -0.01690(19) Zn1 0.0315(4) 0.0267(4) 0.0286(4) -0.0105(3) -0.0001(3) -0.0060(3) P3 0.0291(8) 0.0260(8) 0.0273(8) -0.0100(7) -0.0043(6) -0.0041(6) C13 0.041(3) 0.027(3) 0.029(3) -0.012(3) -0.006(3) -0.005(3) C14 0.059(4) 0.030(4) 0.039(4) -0.008(3) 0.000(3) -0.005(3) C15 0.056(4) 0.039(4) 0.024(3) -0.008(3) -0.009(3) 0.000(3) C16 0.026(3) 0.048(4) 0.038(4) -0.021(3) -0.008(3) -0.005(3) C17 0.033(4) 0.062(5) 0.073(5) -0.028(4) -0.008(3) -0.004(3) C18 0.033(4) 0.052(5) 0.083(6) -0.031(4) 0.003(3) -0.020(3) N2 0.031(3) 0.023(3) 0.028(3) -0.003(2) -0.005(2) -0.005(2) P4 0.0266(7) 0.0243(8) 0.0230(8) -0.0073(6) -0.0026(6) -0.0042(6) C19 0.031(3) 0.032(3) 0.027(3) -0.011(3) 0.005(2) -0.005(3) C20 0.041(4) 0.033(4) 0.034(4) -0.008(3) 0.005(3) -0.012(3) C21 0.043(4) 0.038(4) 0.022(3) -0.004(3) -0.003(3) -0.001(3) C22 0.033(3) 0.038(4) 0.028(3) -0.009(3) -0.007(3) -0.011(3) C23 0.048(4) 0.032(4) 0.046(4) -0.010(3) -0.003(3) -0.013(3) C24 0.047(4) 0.050(4) 0.041(4) -0.015(3) 0.005(3) -0.023(3) Te2 0.0382(3) 0.0360(3) 0.0307(3) -0.0125(2) -0.00784(18) 0.00617(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 P1 N1 1.641(5) . ? P1 C4 1.835(6) . ? P1 C1 1.855(6) . ? P1 Zn1 2.3920(18) . ? C1 C2 1.517(9) . ? C1 C3 1.530(9) . ? C4 C6 1.512(9) . ? C4 C5 1.540(8) . ? N1 P2 1.589(5) . ? P2 C7 1.839(7) . ? P2 C10 1.843(6) . ? P2 Te1 2.4327(18) . ? C7 C8 1.523(9) . ? C7 C9 1.528(9) . ? C10 C11 1.519(10) . ? C10 C12 1.531(10) . ? Te1 Zn1 2.6637(12) . ? Zn1 P3 2.3842(18) . ? Zn1 Te2 2.6702(11) . ? P3 N2 1.635(5) . ? P3 C16 1.850(6) . ? P3 C13 1.857(6) . ? C13 C15 1.532(8) . ? C13 C14 1.543(9) . ? C16 C18 1.512(10) . ? C16 C17 1.531(9) . ? N2 P4 1.602(5) . ? P4 C19 1.832(6) . ? P4 C22 1.834(6) . ? P4 Te2 2.4410(17) . ? C19 C20 1.512(8) . ? C19 C21 1.539(8) . ? C22 C23 1.524(9) . ? C22 C24 1.538(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C4 108.4(3) . . ? N1 P1 C1 105.7(3) . . ? C4 P1 C1 106.5(3) . . ? N1 P1 Zn1 110.09(18) . . ? C4 P1 Zn1 109.6(2) . . ? C1 P1 Zn1 116.2(2) . . ? C2 C1 C3 110.4(5) . . ? C2 C1 P1 109.0(4) . . ? C3 C1 P1 113.3(4) . . ? C6 C4 C5 111.6(5) . . ? C6 C4 P1 115.8(5) . . ? C5 C4 P1 112.2(4) . . ? P2 N1 P1 125.9(3) . . ? N1 P2 C7 108.4(3) . . ? N1 P2 C10 110.2(3) . . ? C7 P2 C10 105.6(3) . . ? N1 P2 Te1 116.68(19) . . ? C7 P2 Te1 108.4(2) . . ? C10 P2 Te1 107.1(2) . . ? C8 C7 C9 110.2(6) . . ? C8 C7 P2 111.4(5) . . ? C9 C7 P2 112.2(5) . . ? C11 C10 C12 110.1(6) . . ? C11 C10 P2 110.9(4) . . ? C12 C10 P2 111.0(5) . . ? P2 Te1 Zn1 87.70(5) . . ? P3 Zn1 P1 129.59(6) . . ? P3 Zn1 Te1 110.61(5) . . ? P1 Zn1 Te1 96.65(5) . . ? P3 Zn1 Te2 96.47(5) . . ? P1 Zn1 Te2 110.79(5) . . ? Te1 Zn1 Te2 113.38(3) . . ? N2 P3 C16 106.5(3) . . ? N2 P3 C13 107.8(3) . . ? C16 P3 C13 107.2(3) . . ? N2 P3 Zn1 111.13(18) . . ? C16 P3 Zn1 114.4(2) . . ? C13 P3 Zn1 109.5(2) . . ? C15 C13 C14 112.0(5) . . ? C15 C13 P3 111.2(4) . . ? C14 C13 P3 114.8(4) . . ? C18 C16 C17 109.8(6) . . ? C18 C16 P3 109.4(4) . . ? C17 C16 P3 114.9(5) . . ? P4 N2 P3 124.6(3) . . ? N2 P4 C19 107.5(3) . . ? N2 P4 C22 111.7(3) . . ? C19 P4 C22 105.7(3) . . ? N2 P4 Te2 116.52(19) . . ? C19 P4 Te2 108.6(2) . . ? C22 P4 Te2 106.3(2) . . ? C20 C19 C21 110.7(5) . . ? C20 C19 P4 111.1(4) . . ? C21 C19 P4 112.2(4) . . ? C23 C22 C24 110.0(5) . . ? C23 C22 P4 111.1(4) . . ? C24 C22 P4 111.1(4) . . ? P4 Te2 Zn1 87.46(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.789 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.192 #===END data_Compound7 _database_code_depnum_ccdc_archive 'CCDC 663952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Cd N2 P4 Te2' _chemical_formula_sum 'C24 H56 Cd N2 P4 Te2' _chemical_formula_weight 864.20 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.429(3) _cell_length_b 17.716(4) _cell_length_c 18.206(4) _cell_angle_alpha 68.62(3) _cell_angle_beta 71.88(3) _cell_angle_gamma 83.82(3) _cell_volume 3547.7(17) _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 block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 2.423 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4595 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 73691 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14470 _reflns_number_gt 10793 _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^)+(0.0619P)^2^+25.0485P] 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 14470 _refine_ls_number_parameters 626 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _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 Cd1 Cd 0.74803(4) 0.28529(3) 0.00761(3) 0.02770(12) Uani 1 1 d . . . Te1 Te 0.76275(4) 0.42085(3) 0.05154(3) 0.03291(12) Uani 1 1 d . . . P1 P 0.89510(13) 0.34208(9) 0.12518(10) 0.0249(3) Uani 1 1 d . . . C1 C 0.7640(7) 0.3531(5) 0.2757(5) 0.0475(19) Uani 1 1 d . . . H1B H 0.7622 0.3651 0.3245 0.071 Uiso 1 1 calc R . . H1C H 0.7472 0.2955 0.2919 0.071 Uiso 1 1 calc R . . H1D H 0.7073 0.3860 0.2507 0.071 Uiso 1 1 calc R . . C2 C 0.8814(6) 0.3730(4) 0.2132(4) 0.0339(15) Uani 1 1 d . . . H2B H 0.9373 0.3408 0.2417 0.041 Uiso 1 1 calc R . . C3 C 0.9116(8) 0.4635(5) 0.1857(5) 0.051(2) Uani 1 1 d . . . H3B H 0.9098 0.4765 0.2340 0.076 Uiso 1 1 calc R . . H3C H 0.8566 0.4971 0.1594 0.076 Uiso 1 1 calc R . . H3D H 0.9877 0.4742 0.1464 0.076 Uiso 1 1 calc R . . C4 C 1.0649(6) 0.3445(5) -0.0171(5) 0.0440(18) Uani 1 1 d . . . H4B H 1.1388 0.3660 -0.0555 0.066 Uiso 1 1 calc R . . H4C H 1.0063 0.3647 -0.0452 0.066 Uiso 1 1 calc R . . H4D H 1.0661 0.2851 0.0018 0.066 Uiso 1 1 calc R . . C5 C 1.0390(5) 0.3717(4) 0.0565(4) 0.0327(15) Uani 1 1 d . . . H5A H 1.0436 0.4323 0.0351 0.039 Uiso 1 1 calc R . . C6 C 1.1275(6) 0.3395(5) 0.1018(6) 0.051(2) Uani 1 1 d . . . H6A H 1.2029 0.3572 0.0634 0.076 Uiso 1 1 calc R . . H6B H 1.1240 0.2801 0.1243 0.076 Uiso 1 1 calc R . . H6C H 1.1128 0.3604 0.1469 0.076 Uiso 1 1 calc R . . N1 N 0.8796(4) 0.2463(3) 0.1609(3) 0.0292(12) Uani 1 1 d . . . P2 P 0.82714(14) 0.19163(10) 0.12452(10) 0.0265(3) Uani 1 1 d . . . C7 C 0.7627(8) 0.0827(5) 0.2888(5) 0.049(2) Uani 1 1 d . . . H7A H 0.6995 0.0564 0.3372 0.074 Uiso 1 1 calc R . . H7B H 0.7982 0.1228 0.2995 0.074 Uiso 1 1 calc R . . H7C H 0.8186 0.0418 0.2775 0.074 Uiso 1 1 calc R . . C8 C 0.7190(6) 0.1247(4) 0.2146(4) 0.0345(15) Uani 1 1 d . . . H8A H 0.6970 0.0820 0.1980 0.041 Uiso 1 1 calc R . . C9 C 0.6142(6) 0.1754(5) 0.2356(5) 0.0450(18) Uani 1 1 d . . . H9A H 0.5557 0.1408 0.2824 0.068 Uiso 1 1 calc R . . H9B H 0.5853 0.1989 0.1877 0.068 Uiso 1 1 calc R . . H9C H 0.6345 0.2190 0.2501 0.068 Uiso 1 1 calc R . . C10 C 1.0296(7) 0.1022(5) 0.1371(6) 0.056(2) Uani 1 1 d . . . H10A H 1.0956 0.0785 0.1072 0.084 Uiso 1 1 calc R . . H10B H 0.9963 0.0624 0.1921 0.084 Uiso 1 1 calc R . . H10C H 1.0530 0.1505 0.1426 0.084 Uiso 1 1 calc R . . C11 C 0.9425(6) 0.1256(4) 0.0899(5) 0.0368(16) Uani 1 1 d . . . H11A H 0.9844 0.1580 0.0317 0.044 Uiso 1 1 calc R . . C12 C 0.8969(8) 0.0511(5) 0.0862(6) 0.055(2) Uani 1 1 d . . . H12A H 0.9594 0.0230 0.0585 0.082 Uiso 1 1 calc R . . H12B H 0.8410 0.0677 0.0555 0.082 Uiso 1 1 calc R . . H12C H 0.8610 0.0144 0.1424 0.082 Uiso 1 1 calc R . . Te2 Te 0.87467(4) 0.32028(3) -0.15992(3) 0.04274(14) Uani 1 1 d . . . P3 P 0.72676(14) 0.25556(10) -0.17868(10) 0.0289(4) Uani 1 1 d . . . C13 C 0.8242(7) 0.3206(6) -0.3512(5) 0.053(2) Uani 1 1 d . . . H13A H 0.8120 0.3515 -0.4049 0.079 Uiso 1 1 calc R . . H13B H 0.8533 0.2668 -0.3506 0.079 Uiso 1 1 calc R . . H13C H 0.8792 0.3492 -0.3420 0.079 Uiso 1 1 calc R . . C14 C 0.7114(6) 0.3117(5) -0.2825(4) 0.0405(17) Uani 1 1 d . . . H14A H 0.6592 0.2792 -0.2919 0.049 Uiso 1 1 calc R . . C15 C 0.6563(6) 0.3934(5) -0.2876(5) 0.0454(18) Uani 1 1 d . . . H15A H 0.6480 0.4213 -0.3430 0.068 Uiso 1 1 calc R . . H15B H 0.7038 0.4263 -0.2766 0.068 Uiso 1 1 calc R . . H15C H 0.5815 0.3855 -0.2467 0.068 Uiso 1 1 calc R . . C16 C 0.8168(9) 0.1046(6) -0.1078(7) 0.074(3) Uani 1 1 d . . . H16A H 0.8455 0.0525 -0.1129 0.111 Uiso 1 1 calc R . . H16B H 0.7511 0.0953 -0.0587 0.111 Uiso 1 1 calc R . . H16C H 0.8762 0.1328 -0.1026 0.111 Uiso 1 1 calc R . . C17 C 0.7818(7) 0.1565(5) -0.1844(5) 0.051(2) Uani 1 1 d . . . H17A H 0.8511 0.1668 -0.2330 0.062 Uiso 1 1 calc R . . C18 C 0.6957(10) 0.1122(6) -0.1992(8) 0.085(4) Uani 1 1 d . . . H18A H 0.7254 0.0589 -0.2000 0.128 Uiso 1 1 calc R . . H18B H 0.6824 0.1440 -0.2522 0.128 Uiso 1 1 calc R . . H18C H 0.6244 0.1054 -0.1548 0.128 Uiso 1 1 calc R . . N2 N 0.6052(4) 0.2477(3) -0.1130(3) 0.0307(12) Uani 1 1 d . . . P4 P 0.57072(13) 0.26054(10) -0.02402(10) 0.0254(3) Uani 1 1 d . . . C19 C 0.5426(7) 0.0956(5) 0.0673(5) 0.052(2) Uani 1 1 d . . . H19A H 0.4963 0.0531 0.1151 0.077 Uiso 1 1 calc R . . H19B H 0.6123 0.1033 0.0782 0.077 Uiso 1 1 calc R . . H19C H 0.5618 0.0796 0.0186 0.077 Uiso 1 1 calc R . . C20 C 0.4767(6) 0.1743(4) 0.0519(4) 0.0348(15) Uani 1 1 d . . . H20A H 0.4483 0.1845 0.1052 0.042 Uiso 1 1 calc R . . C21 C 0.3738(6) 0.1672(5) 0.0260(5) 0.0484(19) Uani 1 1 d . . . H21A H 0.3324 0.1170 0.0638 0.073 Uiso 1 1 calc R . . H21B H 0.3987 0.1662 -0.0303 0.073 Uiso 1 1 calc R . . H21C H 0.3241 0.2137 0.0279 0.073 Uiso 1 1 calc R . . C22 C 0.5378(6) 0.4268(4) -0.0875(5) 0.0404(17) Uani 1 1 d . . . H22A H 0.4847 0.4721 -0.0904 0.061 Uiso 1 1 calc R . . H22B H 0.5692 0.4223 -0.1422 0.061 Uiso 1 1 calc R . . H22C H 0.5994 0.4363 -0.0689 0.061 Uiso 1 1 calc R . . C23 C 0.4760(5) 0.3483(4) -0.0266(4) 0.0296(14) Uani 1 1 d . . . H23A H 0.4108 0.3407 -0.0446 0.036 Uiso 1 1 calc R . . C24 C 0.4302(6) 0.3547(4) 0.0591(4) 0.0357(16) Uani 1 1 d . . . H24A H 0.3828 0.4030 0.0562 0.054 Uiso 1 1 calc R . . H24B H 0.4936 0.3588 0.0787 0.054 Uiso 1 1 calc R . . H24C H 0.3849 0.3063 0.0973 0.054 Uiso 1 1 calc R . . Cd2 Cd 1.26558(4) 0.21402(3) 0.52250(3) 0.02822(12) Uani 1 1 d . A . Te3 Te 1.23612(4) 0.07903(3) 0.48239(3) 0.03581(12) Uani 1 1 d . . . P5 P 1.11406(13) 0.16274(10) 0.40213(10) 0.0247(3) Uani 1 1 d . . . C25 C 1.2538(7) 0.1551(5) 0.2535(5) 0.051(2) Uani 1 1 d . . . H25A H 1.2634 0.1383 0.2062 0.077 Uiso 1 1 calc R . . H25B H 1.3090 0.1270 0.2826 0.077 Uiso 1 1 calc R . . H25C H 1.2657 0.2138 0.2341 0.077 Uiso 1 1 calc R . . C26 C 1.1347(6) 0.1337(4) 0.3118(4) 0.0354(15) Uani 1 1 d . . . H26A H 1.0806 0.1660 0.2816 0.043 Uiso 1 1 calc R . . C27 C 1.1088(7) 0.0439(4) 0.3352(5) 0.0452(18) Uani 1 1 d . . . H27A H 1.1229 0.0312 0.2850 0.068 Uiso 1 1 calc R . . H27B H 1.0294 0.0325 0.3680 0.068 Uiso 1 1 calc R . . H27C H 1.1578 0.0105 0.3677 0.068 Uiso 1 1 calc R . . C28 C 0.9396(6) 0.1582(4) 0.5420(5) 0.0429(18) Uani 1 1 d . . . H28A H 0.8637 0.1384 0.5779 0.064 Uiso 1 1 calc R . . H28B H 0.9423 0.2173 0.5257 0.064 Uiso 1 1 calc R . . H28C H 0.9954 0.1337 0.5717 0.064 Uiso 1 1 calc R . . C29 C 0.9668(6) 0.1351(4) 0.4642(4) 0.0364(16) Uani 1 1 d . . . H29A H 0.9576 0.0751 0.4817 0.044 Uiso 1 1 calc R . . C30 C 0.8855(7) 0.1772(6) 0.4142(6) 0.062(2) Uani 1 1 d . . . H30A H 0.8075 0.1623 0.4487 0.093 Uiso 1 1 calc R . . H30B H 0.9017 0.1605 0.3662 0.093 Uiso 1 1 calc R . . H30C H 0.8951 0.2361 0.3956 0.093 Uiso 1 1 calc R . . N3 N 1.1310(4) 0.2578(3) 0.3694(3) 0.0274(11) Uani 1 1 d . . . P6 P 1.18913(13) 0.30969(10) 0.40560(10) 0.0257(3) Uani 1 1 d . . . C31 C 0.9977(7) 0.4142(5) 0.3950(6) 0.056(2) Uani 1 1 d . . . H31A H 0.9284 0.4309 0.4291 0.085 Uiso 1 1 calc R . . H31B H 0.9785 0.3751 0.3743 0.085 Uiso 1 1 calc R . . H31C H 1.0345 0.4618 0.3484 0.085 Uiso 1 1 calc R . . C32 C 1.0782(6) 0.3747(4) 0.4471(4) 0.0336(15) Uani 1 1 d . . . H32A H 1.0302 0.3379 0.5011 0.040 Uiso 1 1 calc R . . C33 C 1.1313(7) 0.4349(5) 0.4670(6) 0.052(2) Uani 1 1 d . . . H33A H 1.0731 0.4559 0.5050 0.078 Uiso 1 1 calc R . . H33B H 1.1650 0.4797 0.4161 0.078 Uiso 1 1 calc R . . H33C H 1.1902 0.4079 0.4929 0.078 Uiso 1 1 calc R . . C34 C 1.2515(7) 0.4147(5) 0.2407(5) 0.049(2) Uani 1 1 d . . . H34A H 1.3113 0.4476 0.1936 0.073 Uiso 1 1 calc R . . H34B H 1.1864 0.4491 0.2536 0.073 Uiso 1 1 calc R . . H34C H 1.2282 0.3717 0.2270 0.073 Uiso 1 1 calc R . . C35 C 1.2962(6) 0.3768(4) 0.3156(4) 0.0347(15) Uani 1 1 d . . . H35A H 1.3146 0.4216 0.3310 0.042 Uiso 1 1 calc R . . C36 C 1.4040(6) 0.3292(6) 0.2953(5) 0.053(2) Uani 1 1 d . . . H36A H 1.4615 0.3652 0.2489 0.080 Uiso 1 1 calc R . . H36B H 1.3876 0.2848 0.2803 0.080 Uiso 1 1 calc R . . H36C H 1.4323 0.3070 0.3436 0.080 Uiso 1 1 calc R . . Te4 Te 1.12955(4) 0.19307(4) 0.68467(3) 0.04893(15) Uani 1 1 d . A . P7 P 1.28569(14) 0.23900(11) 0.71272(11) 0.0323(4) Uani 1 1 d . . . C37 C 1.3386(10) 0.3653(7) 0.7511(8) 0.089(4) Uani 1 1 d . . . H37A H 1.3182 0.4190 0.7552 0.133 Uiso 1 1 calc R A . H37B H 1.4092 0.3694 0.7066 0.133 Uiso 1 1 calc R . . H37C H 1.3490 0.3279 0.8034 0.133 Uiso 1 1 calc R . . C38 C 1.2446(7) 0.3337(5) 0.7327(5) 0.0459(19) Uani 1 1 d . . . H38A H 1.1776 0.3215 0.7831 0.055 Uiso 1 1 calc R . . C39 C 1.2089(9) 0.3975(6) 0.6622(6) 0.067(3) Uani 1 1 d . . . H39A H 1.1932 0.4485 0.6731 0.101 Uiso 1 1 calc R A . H39B H 1.1405 0.3791 0.6576 0.101 Uiso 1 1 calc R . . H39C H 1.2699 0.4062 0.6106 0.101 Uiso 1 1 calc R . . C40 C 1.3568(16) 0.0940(10) 0.8200(12) 0.064(5) Uiso 0.50 1 d PD A 1 H40A H 1.3477 0.0636 0.8786 0.096 Uiso 0.50 1 calc PR A 1 H40B H 1.4371 0.1069 0.7909 0.096 Uiso 0.50 1 calc PR A 1 H40C H 1.3289 0.0612 0.7964 0.096 Uiso 0.50 1 calc PR A 1 C41 C 1.2939(7) 0.1674(7) 0.8114(5) 0.077(3) Uani 0.50 1 d PD A 1 H41A H 1.3447 0.1989 0.8231 0.092 Uiso 0.50 1 calc PR A 1 C42 C 1.1902(8) 0.1611(6) 0.8844(5) 0.061(2) Uani 0.50 1 d P A 1 H42A H 1.1988 0.1154 0.9327 0.091 Uiso 0.50 1 calc PR A 1 H42B H 1.1228 0.1526 0.8713 0.091 Uiso 0.50 1 calc PR A 1 H42C H 1.1821 0.2114 0.8965 0.091 Uiso 0.50 1 calc PR A 1 C40A C 1.4104(11) 0.1472(10) 0.8196(10) 0.046(4) Uiso 0.50 1 d PD A 2 H40D H 1.4094 0.0939 0.8626 0.069 Uiso 0.50 1 calc PR A 2 H40E H 1.4363 0.1883 0.8346 0.069 Uiso 0.50 1 calc PR A 2 H40F H 1.4621 0.1459 0.7670 0.069 Uiso 0.50 1 calc PR A 2 C41A C 1.2939(7) 0.1674(7) 0.8114(5) 0.077(3) Uani 0.50 1 d PD A 2 H41B H 1.2800 0.1171 0.8029 0.092 Uiso 0.50 1 calc PR A 2 C42A C 1.1902(8) 0.1611(6) 0.8844(5) 0.061(2) Uani 0.50 1 d P A 2 H42D H 1.1538 0.1082 0.9038 0.091 Uiso 0.50 1 calc PR A 2 H42E H 1.1369 0.2042 0.8676 0.091 Uiso 0.50 1 calc PR A 2 H42F H 1.2129 0.1671 0.9290 0.091 Uiso 0.50 1 calc PR A 2 N4 N 1.4060(5) 0.2486(3) 0.6463(3) 0.0329(12) Uani 1 1 d . A . P8 P 1.44177(13) 0.23589(10) 0.55705(10) 0.0264(3) Uani 1 1 d . . . C43 C 1.4757(8) 0.0709(5) 0.6255(6) 0.057(2) Uani 1 1 d . . . H43A H 1.5275 0.0250 0.6272 0.086 Uiso 1 1 calc R A . H43B H 1.4096 0.0611 0.6116 0.086 Uiso 1 1 calc R . . H43C H 1.4510 0.0773 0.6795 0.086 Uiso 1 1 calc R . . C44 C 1.5361(6) 0.1477(4) 0.5604(5) 0.0375(16) Uani 1 1 d . A . H44A H 1.6046 0.1568 0.5740 0.045 Uiso 1 1 calc R . . C45 C 1.5730(6) 0.1379(5) 0.4753(5) 0.049(2) Uani 1 1 d . . . H45A H 1.6243 0.0917 0.4766 0.073 Uiso 1 1 calc R A . H45B H 1.6121 0.1874 0.4332 0.073 Uiso 1 1 calc R . . H45C H 1.5061 0.1286 0.4620 0.073 Uiso 1 1 calc R . . C46 C 1.4707(7) 0.4011(5) 0.4640(6) 0.055(2) Uani 1 1 d . . . H46A H 1.5210 0.4445 0.4205 0.082 Uiso 1 1 calc R A . H46B H 1.4408 0.4153 0.5138 0.082 Uiso 1 1 calc R . . H46C H 1.4078 0.3942 0.4451 0.082 Uiso 1 1 calc R . . C47 C 1.5369(6) 0.3220(4) 0.4834(4) 0.0363(15) Uani 1 1 d . A . H47A H 1.5705 0.3110 0.4307 0.044 Uiso 1 1 calc R . . C48 C 1.6346(7) 0.3311(6) 0.5141(5) 0.052(2) Uani 1 1 d . . . H48A H 1.6759 0.3816 0.4774 0.078 Uiso 1 1 calc R A . H48B H 1.6860 0.2851 0.5145 0.078 Uiso 1 1 calc R . . H48C H 1.6043 0.3325 0.5702 0.078 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 0.0218(2) 0.0299(2) 0.0304(3) -0.01064(19) -0.00656(18) 0.00145(18) Te1 0.0272(2) 0.0272(2) 0.0476(3) -0.01414(19) -0.01637(19) 0.00628(17) P1 0.0205(7) 0.0246(8) 0.0295(8) -0.0095(7) -0.0074(6) 0.0009(6) C1 0.051(5) 0.053(5) 0.036(4) -0.021(4) -0.003(3) 0.000(4) C2 0.038(4) 0.031(3) 0.036(4) -0.014(3) -0.011(3) -0.001(3) C3 0.073(6) 0.036(4) 0.052(5) -0.022(4) -0.021(4) -0.004(4) C4 0.031(4) 0.048(4) 0.048(5) -0.018(4) 0.000(3) -0.006(3) C5 0.022(3) 0.030(3) 0.045(4) -0.010(3) -0.013(3) 0.001(3) C6 0.028(4) 0.060(5) 0.066(6) -0.016(4) -0.024(4) 0.004(4) N1 0.027(3) 0.025(3) 0.034(3) -0.009(2) -0.008(2) 0.001(2) P2 0.0260(8) 0.0236(8) 0.0285(8) -0.0095(7) -0.0065(7) 0.0023(6) C7 0.063(5) 0.045(4) 0.037(4) -0.006(3) -0.017(4) -0.010(4) C8 0.036(4) 0.034(4) 0.033(4) -0.011(3) -0.009(3) -0.007(3) C9 0.031(4) 0.053(5) 0.042(4) -0.016(4) 0.002(3) -0.005(3) C10 0.049(5) 0.046(5) 0.080(6) -0.028(4) -0.029(5) 0.023(4) C11 0.030(3) 0.034(4) 0.046(4) -0.019(3) -0.008(3) 0.008(3) C12 0.061(5) 0.043(5) 0.073(6) -0.036(4) -0.022(5) 0.013(4) Te2 0.0232(2) 0.0684(3) 0.0348(3) -0.0216(2) 0.00154(18) -0.0096(2) P3 0.0223(8) 0.0315(9) 0.0298(9) -0.0146(7) 0.0007(7) 0.0012(7) C13 0.045(5) 0.070(6) 0.032(4) -0.019(4) 0.002(3) 0.003(4) C14 0.033(4) 0.052(5) 0.035(4) -0.019(3) -0.006(3) 0.005(3) C15 0.038(4) 0.055(5) 0.039(4) -0.014(4) -0.010(3) 0.007(4) C16 0.065(6) 0.043(5) 0.087(7) -0.012(5) -0.007(5) 0.021(5) C17 0.048(5) 0.041(4) 0.050(5) -0.019(4) 0.009(4) 0.006(4) C18 0.097(8) 0.064(6) 0.098(9) -0.055(6) 0.005(7) -0.018(6) N2 0.022(3) 0.038(3) 0.033(3) -0.019(2) 0.000(2) -0.002(2) P4 0.0177(7) 0.0294(8) 0.0272(8) -0.0123(7) -0.0007(6) -0.0007(6) C19 0.050(5) 0.036(4) 0.056(5) -0.002(4) -0.011(4) -0.010(4) C20 0.034(4) 0.031(3) 0.034(4) -0.011(3) -0.001(3) -0.005(3) C21 0.032(4) 0.055(5) 0.053(5) -0.019(4) 0.000(3) -0.017(3) C22 0.036(4) 0.036(4) 0.044(4) -0.017(3) -0.004(3) 0.007(3) C23 0.022(3) 0.037(4) 0.031(3) -0.015(3) -0.008(3) 0.005(3) C24 0.023(3) 0.046(4) 0.039(4) -0.024(3) -0.002(3) 0.004(3) Cd2 0.0231(2) 0.0317(3) 0.0304(3) -0.0118(2) -0.00828(19) 0.00264(18) Te3 0.0393(3) 0.0286(2) 0.0443(3) -0.0135(2) -0.0203(2) 0.00751(19) P5 0.0251(8) 0.0258(8) 0.0222(8) -0.0087(6) -0.0052(6) 0.0000(6) C25 0.055(5) 0.058(5) 0.034(4) -0.025(4) 0.011(4) -0.016(4) C26 0.048(4) 0.032(4) 0.026(3) -0.011(3) -0.006(3) -0.007(3) C27 0.063(5) 0.040(4) 0.035(4) -0.017(3) -0.010(4) -0.006(4) C28 0.035(4) 0.037(4) 0.046(4) -0.021(3) 0.011(3) -0.008(3) C29 0.032(4) 0.034(4) 0.040(4) -0.012(3) -0.006(3) -0.007(3) C30 0.034(4) 0.075(6) 0.086(7) -0.034(5) -0.021(4) 0.002(4) N3 0.031(3) 0.027(3) 0.026(3) -0.009(2) -0.011(2) 0.000(2) P6 0.0252(8) 0.0248(8) 0.0260(8) -0.0098(6) -0.0060(6) 0.0028(6) C31 0.051(5) 0.058(5) 0.077(6) -0.037(5) -0.034(5) 0.031(4) C32 0.030(3) 0.034(4) 0.036(4) -0.014(3) -0.009(3) 0.008(3) C33 0.046(5) 0.054(5) 0.073(6) -0.045(5) -0.017(4) 0.013(4) C34 0.062(5) 0.043(4) 0.032(4) -0.005(3) -0.007(4) -0.012(4) C35 0.038(4) 0.027(3) 0.037(4) -0.011(3) -0.004(3) -0.010(3) C36 0.029(4) 0.071(6) 0.053(5) -0.026(4) 0.008(3) -0.012(4) Te4 0.0258(2) 0.0803(4) 0.0432(3) -0.0347(3) 0.0052(2) -0.0093(2) P7 0.0252(8) 0.0431(10) 0.0281(9) -0.0173(8) -0.0029(7) 0.0048(7) C37 0.085(8) 0.101(9) 0.131(11) -0.095(9) -0.041(7) 0.015(7) C38 0.041(4) 0.058(5) 0.049(5) -0.038(4) -0.009(3) 0.015(4) C39 0.073(6) 0.058(6) 0.077(7) -0.038(5) -0.022(5) 0.030(5) C41 0.033(4) 0.108(8) 0.041(5) 0.015(5) 0.004(4) 0.007(5) C42 0.060(6) 0.077(6) 0.032(4) -0.015(4) 0.004(4) -0.011(5) C41A 0.033(4) 0.108(8) 0.041(5) 0.015(5) 0.004(4) 0.007(5) C42A 0.060(6) 0.077(6) 0.032(4) -0.015(4) 0.004(4) -0.011(5) N4 0.029(3) 0.043(3) 0.030(3) -0.019(3) -0.002(2) -0.004(2) P8 0.0185(7) 0.0325(9) 0.0276(8) -0.0133(7) -0.0029(6) 0.0014(6) C43 0.059(5) 0.035(4) 0.063(6) -0.011(4) -0.008(4) 0.009(4) C44 0.031(4) 0.039(4) 0.049(4) -0.022(3) -0.015(3) 0.012(3) C45 0.034(4) 0.064(5) 0.057(5) -0.036(4) -0.011(4) 0.013(4) C46 0.048(5) 0.042(5) 0.066(6) -0.009(4) -0.015(4) -0.009(4) C47 0.032(4) 0.040(4) 0.034(4) -0.014(3) -0.003(3) -0.006(3) C48 0.034(4) 0.069(6) 0.056(5) -0.025(4) -0.010(4) -0.015(4) _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 P4 2.5615(18) . ? Cd1 P2 2.5740(19) . ? Cd1 Te2 2.8301(12) . ? Cd1 Te1 2.8333(9) . ? Te1 P1 2.4421(18) . ? P1 N1 1.590(5) . ? P1 C2 1.830(7) . ? P1 C5 1.836(7) . ? C1 C2 1.528(10) . ? C2 C3 1.546(10) . ? C4 C5 1.517(10) . ? C5 C6 1.517(9) . ? N1 P2 1.635(6) . ? P2 C11 1.853(7) . ? P2 C8 1.859(7) . ? C7 C8 1.521(10) . ? C8 C9 1.529(10) . ? C10 C11 1.517(11) . ? C11 C12 1.523(10) . ? Te2 P3 2.4372(19) . ? P3 N2 1.591(5) . ? P3 C17 1.840(8) . ? P3 C14 1.847(8) . ? C13 C14 1.540(10) . ? C14 C15 1.518(10) . ? C16 C17 1.528(13) . ? C17 C18 1.533(14) . ? N2 P4 1.635(5) . ? P4 C23 1.842(6) . ? P4 C20 1.857(7) . ? C19 C20 1.519(10) . ? C20 C21 1.526(10) . ? C22 C23 1.526(10) . ? C23 C24 1.528(9) . ? Cd2 P8 2.5608(18) . ? Cd2 P6 2.5663(19) . ? Cd2 Te4 2.8186(12) . ? Cd2 Te3 2.8309(9) . ? Te3 P5 2.4393(18) . ? P5 N3 1.582(5) . ? P5 C26 1.833(7) . ? P5 C29 1.836(7) . ? C25 C26 1.521(10) . ? C26 C27 1.532(10) . ? C28 C29 1.544(10) . ? C29 C30 1.523(11) . ? N3 P6 1.638(5) . ? P6 C35 1.853(7) . ? P6 C32 1.855(6) . ? C31 C32 1.531(10) . ? C32 C33 1.511(10) . ? C34 C35 1.530(10) . ? C35 C36 1.523(10) . ? Te4 P7 2.439(2) . ? P7 N4 1.583(5) . ? P7 C41 1.809(9) . ? P7 C38 1.831(7) . ? C37 C38 1.521(13) . ? C38 C39 1.520(12) . ? C40 C41 1.426(15) . ? C41 C42 1.515(11) . ? N4 P8 1.639(5) . ? P8 C44 1.844(7) . ? P8 C47 1.853(7) . ? C43 C44 1.519(11) . ? C44 C45 1.542(10) . ? C46 C47 1.530(11) . ? C47 C48 1.531(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Cd1 P2 126.74(6) . . ? P4 Cd1 Te2 90.32(5) . . ? P2 Cd1 Te2 121.01(5) . . ? P4 Cd1 Te1 120.72(5) . . ? P2 Cd1 Te1 91.07(5) . . ? Te2 Cd1 Te1 108.28(4) . . ? P1 Te1 Cd1 87.28(5) . . ? N1 P1 C2 106.5(3) . . ? N1 P1 C5 111.1(3) . . ? C2 P1 C5 105.7(3) . . ? N1 P1 Te1 116.7(2) . . ? C2 P1 Te1 108.6(2) . . ? C5 P1 Te1 107.6(2) . . ? C1 C2 C3 111.3(6) . . ? C1 C2 P1 111.7(5) . . ? C3 C2 P1 111.9(5) . . ? C6 C5 C4 110.2(6) . . ? C6 C5 P1 111.9(5) . . ? C4 C5 P1 111.4(5) . . ? P1 N1 P2 127.0(4) . . ? N1 P2 C11 106.9(3) . . ? N1 P2 C8 105.6(3) . . ? C11 P2 C8 107.2(3) . . ? N1 P2 Cd1 109.6(2) . . ? C11 P2 Cd1 112.9(2) . . ? C8 P2 Cd1 114.0(2) . . ? C7 C8 C9 111.3(6) . . ? C7 C8 P2 112.6(5) . . ? C9 C8 P2 108.4(5) . . ? C10 C11 C12 111.0(6) . . ? C10 C11 P2 115.2(5) . . ? C12 C11 P2 111.9(5) . . ? P3 Te2 Cd1 89.12(5) . . ? N2 P3 C17 112.0(3) . . ? N2 P3 C14 108.3(3) . . ? C17 P3 C14 103.5(4) . . ? N2 P3 Te2 116.6(2) . . ? C17 P3 Te2 106.8(3) . . ? C14 P3 Te2 108.8(3) . . ? C15 C14 C13 111.3(7) . . ? C15 C14 P3 111.3(5) . . ? C13 C14 P3 112.5(5) . . ? C16 C17 C18 111.5(8) . . ? C16 C17 P3 111.8(6) . . ? C18 C17 P3 110.7(7) . . ? P3 N2 P4 128.5(4) . . ? N2 P4 C23 109.5(3) . . ? N2 P4 C20 106.7(3) . . ? C23 P4 C20 102.6(3) . . ? N2 P4 Cd1 110.4(2) . . ? C23 P4 Cd1 109.2(2) . . ? C20 P4 Cd1 117.9(2) . . ? C19 C20 C21 111.0(6) . . ? C19 C20 P4 110.6(5) . . ? C21 C20 P4 112.5(5) . . ? C22 C23 C24 109.3(6) . . ? C22 C23 P4 110.9(4) . . ? C24 C23 P4 110.4(5) . . ? P8 Cd2 P6 126.94(6) . . ? P8 Cd2 Te4 91.07(5) . . ? P6 Cd2 Te4 116.41(5) . . ? P8 Cd2 Te3 123.36(5) . . ? P6 Cd2 Te3 90.88(5) . . ? Te4 Cd2 Te3 109.22(4) . . ? P5 Te3 Cd2 88.32(5) . . ? N3 P5 C26 107.1(3) . . ? N3 P5 C29 110.4(3) . . ? C26 P5 C29 105.1(3) . . ? N3 P5 Te3 117.4(2) . . ? C26 P5 Te3 108.5(2) . . ? C29 P5 Te3 107.6(2) . . ? C25 C26 C27 110.6(6) . . ? C25 C26 P5 110.8(5) . . ? C27 C26 P5 112.7(5) . . ? C30 C29 C28 110.2(7) . . ? C30 C29 P5 110.8(5) . . ? C28 C29 P5 109.5(5) . . ? P5 N3 P6 127.4(3) . . ? N3 P6 C35 106.1(3) . . ? N3 P6 C32 107.8(3) . . ? C35 P6 C32 107.9(3) . . ? N3 P6 Cd2 110.49(19) . . ? C35 P6 Cd2 115.2(2) . . ? C32 P6 Cd2 109.0(2) . . ? C33 C32 C31 113.1(6) . . ? C33 C32 P6 110.0(5) . . ? C31 C32 P6 115.2(5) . . ? C36 C35 C34 111.0(6) . . ? C36 C35 P6 109.5(5) . . ? C34 C35 P6 111.6(5) . . ? P7 Te4 Cd2 90.16(5) . . ? N4 P7 C41 109.8(3) . . ? N4 P7 C38 110.4(4) . . ? C41 P7 C38 103.6(5) . . ? N4 P7 Te4 117.3(2) . . ? C41 P7 Te4 106.1(4) . . ? C38 P7 Te4 108.6(3) . . ? C39 C38 C37 111.2(9) . . ? C39 C38 P7 111.8(5) . . ? C37 C38 P7 111.1(6) . . ? C40 C41 C42 113.5(11) . . ? C40 C41 P7 123.0(11) . . ? C42 C41 P7 116.1(6) . . ? P7 N4 P8 129.2(4) . . ? N4 P8 C44 109.5(3) . . ? N4 P8 C47 105.9(3) . . ? C44 P8 C47 102.7(3) . . ? N4 P8 Cd2 110.5(2) . . ? C44 P8 Cd2 109.8(2) . . ? C47 P8 Cd2 117.9(2) . . ? C43 C44 C45 109.2(7) . . ? C43 C44 P8 110.6(5) . . ? C45 C44 P8 109.2(5) . . ? C46 C47 C48 110.3(7) . . ? C46 C47 P8 111.0(5) . . ? C48 C47 P8 112.4(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.473 _refine_diff_density_min -1.872 _refine_diff_density_rms 0.153 #===END data_Compound8 _database_code_depnum_ccdc_archive 'CCDC 663953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Hg N2 P4 Te2' _chemical_formula_sum 'C24 H56 Hg N2 P4 Te2' _chemical_formula_weight 952.38 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' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.268(2) _cell_length_b 12.423(3) _cell_length_c 14.447(3) _cell_angle_alpha 76.26(3) _cell_angle_beta 88.47(3) _cell_angle_gamma 80.04(3) _cell_volume 1762.9(7) _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 plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 6.184 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6375 _exptl_absorpt_correction_T_max 0.8863 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _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 31073 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.44 _reflns_number_total 8025 _reflns_number_gt 5723 _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^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8025 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Hg1 Hg 0.27593(2) 0.273037(19) 0.223910(15) 0.02909(8) Uani 1 1 d . . . Te1 Te 0.38483(4) 0.23841(3) 0.04448(3) 0.03397(11) Uani 1 1 d . . . Te2 Te 0.46678(5) 0.13333(3) 0.36312(3) 0.04225(13) Uani 1 1 d . . . P2 P 0.08554(14) 0.18363(13) 0.20087(10) 0.0244(3) Uani 1 1 d . . . P4 P 0.45232(15) 0.28848(13) 0.44061(10) 0.0302(4) Uani 1 1 d . . . P3 P 0.30700(15) 0.44174(13) 0.27781(10) 0.0268(3) Uani 1 1 d . . . P1 P 0.22924(15) 0.11121(13) 0.04608(10) 0.0263(3) Uani 1 1 d . . . N1 N 0.1020(4) 0.1270(4) 0.1096(3) 0.0293(11) Uani 1 1 d . . . N2 N 0.3882(5) 0.4095(4) 0.3789(3) 0.0306(11) Uani 1 1 d . . . C8 C -0.0715(6) 0.2848(5) 0.1825(4) 0.0343(14) Uani 1 1 d . . . H8A H -0.0941 0.3059 0.2443 0.041 Uiso 1 1 calc R . . C16 C 0.3108(7) 0.5742(5) 0.0935(4) 0.0434(17) Uani 1 1 d . . . H16A H 0.3573 0.6239 0.0462 0.065 Uiso 1 1 calc R . . H16B H 0.2248 0.6158 0.1064 0.065 Uiso 1 1 calc R . . H16C H 0.2975 0.5098 0.0689 0.065 Uiso 1 1 calc R . . C19 C 0.7023(6) 0.3401(6) 0.3967(4) 0.0448(17) Uani 1 1 d . . . H19A H 0.7892 0.3454 0.4199 0.067 Uiso 1 1 calc R . . H19B H 0.6583 0.4149 0.3624 0.067 Uiso 1 1 calc R . . H19C H 0.7132 0.2891 0.3537 0.067 Uiso 1 1 calc R . . C2 C 0.3198(6) -0.0337(5) 0.0828(4) 0.0363(15) Uani 1 1 d . . . H2B H 0.3980 -0.0411 0.0406 0.044 Uiso 1 1 calc R . . C9 C -0.1865(6) 0.2361(6) 0.1541(5) 0.0493(18) Uani 1 1 d . . . H9A H -0.2635 0.2960 0.1367 0.074 Uiso 1 1 calc R . . H9B H -0.2086 0.1777 0.2079 0.074 Uiso 1 1 calc R . . H9C H -0.1615 0.2033 0.0995 0.074 Uiso 1 1 calc R . . C17 C 0.3937(6) 0.5321(5) 0.1863(4) 0.0329(14) Uani 1 1 d . . . H17A H 0.4066 0.5988 0.2102 0.039 Uiso 1 1 calc R . . C20 C 0.6200(6) 0.2960(5) 0.4793(4) 0.0364(15) Uani 1 1 d . . . H20A H 0.6094 0.3511 0.5205 0.044 Uiso 1 1 calc R . . C5 C 0.1683(6) 0.1271(6) -0.0757(4) 0.0394(16) Uani 1 1 d . . . H5A H 0.1070 0.0719 -0.0725 0.047 Uiso 1 1 calc R . . C1 C 0.3705(7) -0.0591(6) 0.1852(5) 0.0508(18) Uani 1 1 d . . . H1B H 0.4290 -0.1324 0.2003 0.076 Uiso 1 1 calc R . . H1C H 0.2954 -0.0607 0.2286 0.076 Uiso 1 1 calc R . . H1D H 0.4195 -0.0006 0.1926 0.076 Uiso 1 1 calc R . . C7 C -0.0512(6) 0.3925(5) 0.1088(5) 0.0457(17) Uani 1 1 d . . . H7A H -0.1351 0.4454 0.0975 0.069 Uiso 1 1 calc R . . H7B H -0.0207 0.3734 0.0489 0.069 Uiso 1 1 calc R . . H7C H 0.0150 0.4273 0.1332 0.069 Uiso 1 1 calc R . . C4 C 0.0891(7) 0.2433(6) -0.1138(4) 0.0503(18) Uani 1 1 d . . . H4A H 0.0538 0.2483 -0.1774 0.075 Uiso 1 1 calc R . . H4B H 0.1463 0.2997 -0.1179 0.075 Uiso 1 1 calc R . . H4C H 0.0158 0.2571 -0.0710 0.075 Uiso 1 1 calc R . . C14 C 0.1494(6) 0.5340(5) 0.2929(4) 0.0360(15) Uani 1 1 d . . . H14A H 0.1051 0.5623 0.2289 0.043 Uiso 1 1 calc R . . C15 C 0.1718(7) 0.6366(6) 0.3275(5) 0.0498(18) Uani 1 1 d . . . H15A H 0.0863 0.6831 0.3341 0.075 Uiso 1 1 calc R . . H15B H 0.2253 0.6807 0.2812 0.075 Uiso 1 1 calc R . . H15C H 0.2181 0.6117 0.3893 0.075 Uiso 1 1 calc R . . C13 C 0.0559(7) 0.4701(6) 0.3589(5) 0.0507(18) Uani 1 1 d . . . H13A H -0.0298 0.5190 0.3589 0.076 Uiso 1 1 calc R . . H13B H 0.0934 0.4462 0.4237 0.076 Uiso 1 1 calc R . . H13C H 0.0440 0.4038 0.3365 0.076 Uiso 1 1 calc R . . C11 C 0.0692(6) 0.0730(5) 0.3090(4) 0.0334(14) Uani 1 1 d . . . H11A H 0.1607 0.0306 0.3260 0.040 Uiso 1 1 calc R . . C6 C 0.2817(7) 0.0982(7) -0.1428(4) 0.0514(19) Uani 1 1 d . . . H6A H 0.2450 0.1028 -0.2058 0.077 Uiso 1 1 calc R . . H6B H 0.3290 0.0218 -0.1166 0.077 Uiso 1 1 calc R . . H6C H 0.3430 0.1517 -0.1485 0.077 Uiso 1 1 calc R . . C21 C 0.6887(7) 0.1843(6) 0.5397(5) 0.0533(19) Uani 1 1 d . . . H21A H 0.7750 0.1930 0.5616 0.080 Uiso 1 1 calc R . . H21B H 0.7012 0.1278 0.5016 0.080 Uiso 1 1 calc R . . H21C H 0.6343 0.1600 0.5949 0.080 Uiso 1 1 calc R . . C12 C 0.0242(8) 0.1260(6) 0.3928(4) 0.054(2) Uani 1 1 d . . . H12A H 0.0441 0.0693 0.4528 0.081 Uiso 1 1 calc R . . H12B H -0.0712 0.1539 0.3872 0.081 Uiso 1 1 calc R . . H12C H 0.0711 0.1886 0.3917 0.081 Uiso 1 1 calc R . . C10 C -0.0136(7) -0.0144(6) 0.2992(5) 0.054(2) Uani 1 1 d . . . H10A H 0.0026 -0.0785 0.3545 0.081 Uiso 1 1 calc R . . H10B H 0.0108 -0.0401 0.2410 0.081 Uiso 1 1 calc R . . H10C H -0.1075 0.0192 0.2957 0.081 Uiso 1 1 calc R . . C18 C 0.5286(6) 0.4709(6) 0.1654(4) 0.0487(18) Uani 1 1 d . . . H18A H 0.5753 0.5235 0.1210 0.073 Uiso 1 1 calc R . . H18B H 0.5174 0.4089 0.1369 0.073 Uiso 1 1 calc R . . H18C H 0.5801 0.4410 0.2249 0.073 Uiso 1 1 calc R . . C3 C 0.2340(8) -0.1187(6) 0.0711(6) 0.061(2) Uani 1 1 d . . . H3A H 0.2842 -0.1951 0.0922 0.091 Uiso 1 1 calc R . . H3B H 0.2082 -0.1049 0.0040 0.091 Uiso 1 1 calc R . . H3C H 0.1546 -0.1107 0.1098 0.091 Uiso 1 1 calc R . . C23 C 0.3680(7) 0.2530(7) 0.5553(5) 0.056(2) Uani 1 1 d . . . H23A H 0.4296 0.1907 0.5976 0.067 Uiso 1 1 calc R . . C24 C 0.3503(9) 0.3542(8) 0.6032(5) 0.073(3) Uani 1 1 d . . . H24A H 0.3127 0.3326 0.6665 0.109 Uiso 1 1 calc R . . H24B H 0.2907 0.4179 0.5639 0.109 Uiso 1 1 calc R . . H24C H 0.4365 0.3759 0.6092 0.109 Uiso 1 1 calc R . . C22 C 0.2438(9) 0.2113(8) 0.5518(6) 0.084(3) Uani 1 1 d . . . H22A H 0.2085 0.1924 0.6162 0.126 Uiso 1 1 calc R . . H22B H 0.2600 0.1440 0.5261 0.126 Uiso 1 1 calc R . . H22C H 0.1798 0.2696 0.5107 0.126 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 0.03107(13) 0.02682(14) 0.03094(13) -0.00909(10) -0.00278(10) -0.00556(10) Te1 0.0367(2) 0.0333(3) 0.0367(2) -0.01304(18) 0.01047(18) -0.01374(19) Te2 0.0537(3) 0.0251(2) 0.0454(2) -0.00787(19) -0.0206(2) 0.0030(2) P2 0.0234(7) 0.0249(8) 0.0250(7) -0.0072(6) 0.0011(6) -0.0032(6) P4 0.0324(9) 0.0288(9) 0.0285(8) -0.0051(7) -0.0039(7) -0.0049(7) P3 0.0269(8) 0.0238(8) 0.0297(8) -0.0077(6) -0.0053(6) -0.0012(7) P1 0.0272(8) 0.0241(8) 0.0281(7) -0.0078(6) -0.0009(6) -0.0032(7) N1 0.026(3) 0.030(3) 0.033(3) -0.012(2) 0.000(2) -0.002(2) N2 0.033(3) 0.027(3) 0.030(2) -0.008(2) -0.009(2) 0.004(2) C8 0.034(3) 0.039(4) 0.032(3) -0.016(3) -0.001(3) -0.001(3) C16 0.062(5) 0.033(4) 0.033(3) 0.000(3) -0.010(3) -0.012(4) C19 0.035(4) 0.043(4) 0.051(4) -0.005(3) -0.005(3) 0.000(3) C2 0.036(4) 0.035(4) 0.039(3) -0.016(3) 0.006(3) -0.003(3) C9 0.028(4) 0.060(5) 0.061(4) -0.024(4) -0.006(3) 0.004(3) C17 0.036(4) 0.032(4) 0.034(3) -0.010(3) -0.003(3) -0.009(3) C20 0.036(4) 0.040(4) 0.035(3) -0.013(3) -0.007(3) -0.006(3) C5 0.038(4) 0.051(4) 0.031(3) -0.015(3) -0.008(3) -0.004(3) C1 0.056(5) 0.038(4) 0.049(4) -0.004(3) 0.005(4) 0.009(4) C7 0.040(4) 0.033(4) 0.053(4) 0.000(3) -0.011(3) 0.012(3) C4 0.049(4) 0.059(5) 0.035(4) -0.007(3) -0.010(3) 0.007(4) C14 0.037(4) 0.033(4) 0.037(3) -0.015(3) -0.010(3) 0.007(3) C15 0.050(4) 0.035(4) 0.064(5) -0.026(4) -0.006(4) 0.014(3) C13 0.040(4) 0.050(5) 0.065(5) -0.024(4) 0.009(4) -0.005(4) C11 0.035(3) 0.031(4) 0.030(3) -0.001(3) 0.004(3) -0.003(3) C6 0.050(4) 0.079(6) 0.028(3) -0.019(4) 0.008(3) -0.011(4) C21 0.051(4) 0.044(5) 0.057(4) -0.001(4) -0.025(4) 0.002(4) C12 0.078(6) 0.048(5) 0.032(3) -0.005(3) 0.010(4) -0.010(4) C10 0.062(5) 0.051(5) 0.049(4) 0.000(4) -0.001(4) -0.031(4) C18 0.042(4) 0.058(5) 0.039(4) 0.003(3) 0.005(3) -0.007(4) C3 0.068(5) 0.035(4) 0.086(6) -0.023(4) 0.004(4) -0.016(4) C23 0.054(5) 0.066(6) 0.045(4) -0.004(4) 0.006(4) -0.018(4) C24 0.082(6) 0.098(7) 0.049(5) -0.035(5) 0.029(4) -0.021(5) C22 0.081(7) 0.102(8) 0.078(6) -0.016(6) 0.020(5) -0.053(6) _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 P3 2.4739(15) . ? Hg1 P2 2.4753(15) . ? Hg1 Te2 2.8762(13) . ? Hg1 Te1 2.8922(9) . ? Te1 P1 2.4298(16) . ? Te2 P4 2.4304(17) . ? P2 N1 1.628(4) . ? P2 C11 1.845(6) . ? P2 C8 1.847(6) . ? P4 N2 1.594(5) . ? P4 C23 1.844(7) . ? P4 C20 1.849(6) . ? P3 N2 1.631(4) . ? P3 C17 1.839(6) . ? P3 C14 1.854(6) . ? P1 N1 1.588(5) . ? P1 C5 1.838(6) . ? P1 C2 1.839(6) . ? C8 C9 1.523(8) . ? C8 C7 1.541(9) . ? C16 C17 1.539(8) . ? C19 C20 1.495(8) . ? C2 C1 1.523(8) . ? C2 C3 1.528(8) . ? C17 C18 1.520(9) . ? C20 C21 1.517(9) . ? C5 C4 1.512(9) . ? C5 C6 1.544(9) . ? C14 C13 1.522(9) . ? C14 C15 1.528(8) . ? C11 C10 1.523(8) . ? C11 C12 1.535(8) . ? C23 C22 1.462(9) . ? C23 C24 1.556(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P3 Hg1 P2 135.87(5) . . ? P3 Hg1 Te2 90.75(4) . . ? P2 Hg1 Te2 113.84(4) . . ? P3 Hg1 Te1 119.75(4) . . ? P2 Hg1 Te1 90.57(4) . . ? Te2 Hg1 Te1 103.70(3) . . ? P1 Te1 Hg1 87.78(4) . . ? P4 Te2 Hg1 88.55(5) . . ? N1 P2 C11 108.6(3) . . ? N1 P2 C8 106.8(2) . . ? C11 P2 C8 107.7(3) . . ? N1 P2 Hg1 112.87(18) . . ? C11 P2 Hg1 108.5(2) . . ? C8 P2 Hg1 112.21(19) . . ? N2 P4 C23 111.3(3) . . ? N2 P4 C20 108.3(3) . . ? C23 P4 C20 102.0(3) . . ? N2 P4 Te2 116.28(17) . . ? C23 P4 Te2 109.1(2) . . ? C20 P4 Te2 108.8(2) . . ? N2 P3 C17 109.8(3) . . ? N2 P3 C14 107.2(3) . . ? C17 P3 C14 103.9(3) . . ? N2 P3 Hg1 112.26(18) . . ? C17 P3 Hg1 109.91(19) . . ? C14 P3 Hg1 113.40(19) . . ? N1 P1 C5 106.3(3) . . ? N1 P1 C2 110.1(3) . . ? C5 P1 C2 105.8(3) . . ? N1 P1 Te1 116.45(17) . . ? C5 P1 Te1 109.6(2) . . ? C2 P1 Te1 108.0(2) . . ? P1 N1 P2 127.4(3) . . ? P4 N2 P3 128.8(3) . . ? C9 C8 C7 111.5(5) . . ? C9 C8 P2 113.2(4) . . ? C7 C8 P2 109.4(4) . . ? C1 C2 C3 110.6(6) . . ? C1 C2 P1 110.8(4) . . ? C3 C2 P1 111.3(5) . . ? C18 C17 C16 109.3(5) . . ? C18 C17 P3 111.7(4) . . ? C16 C17 P3 110.5(4) . . ? C19 C20 C21 111.7(6) . . ? C19 C20 P4 111.6(4) . . ? C21 C20 P4 112.1(4) . . ? C4 C5 C6 111.9(6) . . ? C4 C5 P1 111.1(4) . . ? C6 C5 P1 111.7(4) . . ? C13 C14 C15 110.5(5) . . ? C13 C14 P3 111.9(5) . . ? C15 C14 P3 112.2(4) . . ? C10 C11 C12 111.7(5) . . ? C10 C11 P2 116.5(4) . . ? C12 C11 P2 110.2(4) . . ? C22 C23 C24 111.6(7) . . ? C22 C23 P4 115.7(5) . . ? C24 C23 P4 109.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.898 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.168