Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _ccdc_journal_manuscript_code B717287G _publ_requested_journal 'Dalton Trans.' _publ_contact_author_name 'T. Chivers' _publ_contact_author_address ;Department of Chemistry, University of Calgary, 2500 University Drive NW, Calgary, AB, T2N 1N4 Canada ; _publ_contact_author_email chivers@ucalgary.ca _publ_contact_author_phone '1 403 220 5741' _publ_contact_author_fax '1 403 289 9488' loop_ _publ_author_name _publ_author_address 'Chivers, T.' ;Department of Chemistry, University of Calgary, 2500 University Drive NW, Calgary, AB, T2N 1N4 Canada ; 'Robertson, S.D.' ;Department of Chemistry, University of Calgary, 2500 University Drive NW, Calgary, AB, T2N 1N4 Canada ; _publ_section_title ; Synthesis, NMR characterization and X-ray structures of mixed chalcogenido PNP ligands containing tellurium: X-ray structures of SeiPr2PNP(H)iPr2 and [NaN(EPiPr2)2]? (E = Se, Te) ; data_2b _database_code_depnum_ccdc_archive 'CCDC 666804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H29 N P2 Se' _chemical_formula_sum 'C12 H29 N P2 Se' _chemical_formula_weight 328.26 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' Se Se -0.0929 2.2259 '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 8.6480(3) _cell_length_b 8.8274(4) _cell_length_c 11.5664(4) _cell_angle_alpha 100.606(2) _cell_angle_beta 102.617(2) _cell_angle_gamma 90.515(2) _cell_volume 845.82(6) _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 colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 2.390 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6465 _exptl_absorpt_correction_T_max 0.7961 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 13272 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2979 _reflns_number_gt 2440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0382P)^2^+0.2353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2979 _refine_ls_number_parameters 148 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Se1 Se 0.24447(4) 0.23818(3) 0.11722(3) 0.03453(13) Uani 1 1 d . . . P1 P 0.33090(8) 0.14936(8) 0.27779(6) 0.02034(18) Uani 1 1 d . . . P2 P 0.19805(8) -0.15365(8) 0.15957(6) 0.02191(18) Uani 1 1 d . . . H2 H 0.089(3) -0.094(3) 0.079(2) 0.026 Uiso 1 1 d . . . N1 N 0.2894(3) -0.0317(2) 0.27231(19) 0.0232(5) Uani 1 1 d . . . C10 C 0.5473(3) 0.1788(3) 0.3251(3) 0.0268(7) Uani 1 1 d . . . H10 H 0.5822 0.1351 0.3999 0.032 Uiso 1 1 calc R . . C11 C 0.6262(4) 0.0901(4) 0.2289(3) 0.0399(8) Uani 1 1 d . . . H11A H 0.5890 -0.0187 0.2104 0.060 Uiso 1 1 calc R . . H11B H 0.7417 0.0982 0.2590 0.060 Uiso 1 1 calc R . . H11C H 0.5987 0.1340 0.1556 0.060 Uiso 1 1 calc R . . C12 C 0.6021(4) 0.3500(3) 0.3561(3) 0.0337(7) Uani 1 1 d . . . H12A H 0.5507 0.4041 0.4183 0.051 Uiso 1 1 calc R . . H12B H 0.5733 0.3954 0.2836 0.051 Uiso 1 1 calc R . . H12C H 0.7175 0.3601 0.3863 0.051 Uiso 1 1 calc R . . C20 C 0.2573(3) 0.2554(3) 0.4051(2) 0.0273(7) Uani 1 1 d . . . H20 H 0.2926 0.3665 0.4171 0.033 Uiso 1 1 calc R . . C21 C 0.0762(4) 0.2451(4) 0.3778(3) 0.0404(8) Uani 1 1 d . . . H21A H 0.0343 0.2822 0.3028 0.061 Uiso 1 1 calc R . . H21B H 0.0394 0.3089 0.4442 0.061 Uiso 1 1 calc R . . H21C H 0.0387 0.1376 0.3688 0.061 Uiso 1 1 calc R . . C22 C 0.3254(4) 0.1982(4) 0.5220(3) 0.0438(9) Uani 1 1 d . . . H22A H 0.4416 0.2060 0.5385 0.066 Uiso 1 1 calc R . . H22B H 0.2893 0.0904 0.5134 0.066 Uiso 1 1 calc R . . H22C H 0.2891 0.2616 0.5888 0.066 Uiso 1 1 calc R . . C30 C 0.0902(3) -0.2967(3) 0.2110(3) 0.0304(7) Uani 1 1 d . . . H30 H 0.0696 -0.3918 0.1467 0.037 Uiso 1 1 calc R . . C31 C -0.0688(4) -0.2370(4) 0.2289(3) 0.0445(9) Uani 1 1 d . . . H31A H -0.1289 -0.2113 0.1535 0.067 Uiso 1 1 calc R . . H31B H -0.0513 -0.1444 0.2926 0.067 Uiso 1 1 calc R . . H31C H -0.1286 -0.3167 0.2523 0.067 Uiso 1 1 calc R . . C32 C 0.1864(4) -0.3398(4) 0.3263(3) 0.0463(9) Uani 1 1 d . . . H32A H 0.2885 -0.3774 0.3126 0.069 Uiso 1 1 calc R . . H32B H 0.1277 -0.4209 0.3490 0.069 Uiso 1 1 calc R . . H32C H 0.2050 -0.2487 0.3914 0.069 Uiso 1 1 calc R . . C40 C 0.3220(3) -0.2478(3) 0.0630(2) 0.0256(6) Uani 1 1 d . . . H40 H 0.3718 -0.1645 0.0331 0.031 Uiso 1 1 calc R . . C41 C 0.2224(4) -0.3550(4) -0.0489(3) 0.0372(8) Uani 1 1 d . . . H41A H 0.1374 -0.2976 -0.0894 0.056 Uiso 1 1 calc R . . H41B H 0.1761 -0.4422 -0.0242 0.056 Uiso 1 1 calc R . . H41C H 0.2903 -0.3934 -0.1044 0.056 Uiso 1 1 calc R . . C42 C 0.4578(3) -0.3317(4) 0.1283(3) 0.0331(7) Uani 1 1 d . . . H42A H 0.5200 -0.2602 0.1984 0.050 Uiso 1 1 calc R . . H42B H 0.5262 -0.3702 0.0731 0.050 Uiso 1 1 calc R . . H42C H 0.4144 -0.4187 0.1551 0.050 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 Se1 0.0430(2) 0.0314(2) 0.02614(18) 0.01249(13) -0.00453(14) -0.00258(14) P1 0.0225(4) 0.0183(4) 0.0187(4) 0.0033(3) 0.0015(3) -0.0004(3) P2 0.0227(4) 0.0193(4) 0.0217(4) 0.0025(3) 0.0019(3) -0.0004(3) N1 0.0273(12) 0.0182(12) 0.0232(12) 0.0037(10) 0.0042(10) 0.0005(10) C10 0.0250(15) 0.0257(16) 0.0283(15) 0.0063(12) 0.0019(12) -0.0012(13) C11 0.0289(17) 0.0365(19) 0.054(2) -0.0009(16) 0.0168(15) -0.0026(15) C12 0.0304(17) 0.0287(17) 0.0386(18) 0.0018(14) 0.0049(14) -0.0085(14) C20 0.0261(15) 0.0233(16) 0.0303(16) -0.0005(12) 0.0065(13) -0.0002(13) C21 0.0298(17) 0.043(2) 0.048(2) 0.0022(16) 0.0128(15) 0.0074(15) C22 0.048(2) 0.059(2) 0.0230(16) 0.0038(15) 0.0089(15) 0.0049(18) C30 0.0337(17) 0.0239(16) 0.0315(16) -0.0050(13) 0.0116(14) -0.0099(13) C31 0.0304(17) 0.062(2) 0.0416(19) 0.0052(17) 0.0134(15) -0.0052(17) C32 0.053(2) 0.039(2) 0.058(2) 0.0264(17) 0.0225(18) 0.0047(17) C40 0.0297(16) 0.0241(16) 0.0219(14) 0.0015(12) 0.0063(12) -0.0029(13) C41 0.0405(19) 0.0371(19) 0.0289(16) -0.0056(14) 0.0069(14) -0.0024(15) C42 0.0287(16) 0.0316(17) 0.0368(17) 0.0014(14) 0.0071(14) 0.0038(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 P1 2.1360(9) . ? P1 N1 1.622(2) . ? P1 C10 1.833(3) . ? P1 C20 1.834(3) . ? P2 N1 1.581(2) . ? P2 C40 1.812(3) . ? P2 C30 1.821(3) . ? P2 H2 1.35(3) . ? C10 C11 1.529(4) . ? C10 C12 1.533(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C20 C21 1.527(4) . ? C20 C22 1.529(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C30 C31 1.519(4) . ? C30 C32 1.524(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C40 C42 1.527(4) . ? C40 C41 1.536(4) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C10 106.84(13) . . ? N1 P1 C20 105.95(13) . . ? C10 P1 C20 104.59(13) . . ? N1 P1 Se1 116.92(9) . . ? C10 P1 Se1 110.40(10) . . ? C20 P1 Se1 111.32(10) . . ? N1 P2 C40 114.78(13) . . ? N1 P2 C30 109.34(13) . . ? C40 P2 C30 110.31(13) . . ? N1 P2 H2 114.7(11) . . ? C40 P2 H2 101.0(11) . . ? C30 P2 H2 106.1(11) . . ? P2 N1 P1 127.53(14) . . ? C11 C10 C12 111.0(2) . . ? C11 C10 P1 110.5(2) . . ? C12 C10 P1 112.5(2) . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? P1 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C20 C22 110.4(3) . . ? C21 C20 P1 110.9(2) . . ? C22 C20 P1 111.7(2) . . ? C21 C20 H20 107.9 . . ? C22 C20 H20 107.9 . . ? P1 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 C30 C32 111.0(3) . . ? C31 C30 P2 109.9(2) . . ? C32 C30 P2 111.5(2) . . ? C31 C30 H30 108.1 . . ? C32 C30 H30 108.1 . . ? P2 C30 H30 108.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C40 C41 111.4(2) . . ? C42 C40 P2 113.9(2) . . ? C41 C40 P2 111.3(2) . . ? C42 C40 H40 106.6 . . ? C41 C40 H40 106.6 . . ? P2 C40 H40 106.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C40 P2 N1 P1 86.4(2) . . . . ? C30 P2 N1 P1 -149.09(18) . . . . ? C10 P1 N1 P2 -121.26(19) . . . . ? C20 P1 N1 P2 127.63(18) . . . . ? Se1 P1 N1 P2 2.9(2) . . . . ? N1 P1 C10 C11 65.5(2) . . . . ? C20 P1 C10 C11 177.6(2) . . . . ? Se1 P1 C10 C11 -62.6(2) . . . . ? N1 P1 C10 C12 -169.7(2) . . . . ? C20 P1 C10 C12 -57.7(2) . . . . ? Se1 P1 C10 C12 62.1(2) . . . . ? N1 P1 C20 C21 -68.7(2) . . . . ? C10 P1 C20 C21 178.6(2) . . . . ? Se1 P1 C20 C21 59.4(2) . . . . ? N1 P1 C20 C22 54.9(2) . . . . ? C10 P1 C20 C22 -57.8(2) . . . . ? Se1 P1 C20 C22 -177.03(18) . . . . ? N1 P2 C30 C31 84.1(2) . . . . ? C40 P2 C30 C31 -148.8(2) . . . . ? N1 P2 C30 C32 -39.4(3) . . . . ? C40 P2 C30 C32 87.7(2) . . . . ? N1 P2 C40 C42 57.4(2) . . . . ? C30 P2 C40 C42 -66.7(2) . . . . ? N1 P2 C40 C41 -175.75(19) . . . . ? C30 P2 C40 C41 60.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.290 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.072 #===END data_4Na _database_code_depnum_ccdc_archive 'CCDC 666805' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N Na P2 Se2' _chemical_formula_sum 'C12 H28 N Na P2 Se2' _chemical_formula_weight 429.20 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.9188(4) _cell_length_b 9.6259(4) _cell_length_c 13.0855(6) _cell_angle_alpha 106.746(3) _cell_angle_beta 99.958(3) _cell_angle_gamma 104.559(3) _cell_volume 891.50(8) _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 colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 4.337 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4775 _exptl_absorpt_correction_T_max 0.7229 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 12986 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3139 _reflns_number_gt 2644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0224P)^2^+0.5108P] 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 3139 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Se1 Se 0.00681(4) 0.80065(3) 0.04100(2) 0.02192(10) Uani 1 1 d . . . Se2 Se 0.53202(4) 1.16556(3) 0.16448(2) 0.02343(10) Uani 1 1 d . . . P1 P 0.17407(10) 0.79164(8) 0.18778(6) 0.01603(17) Uani 1 1 d . . . P2 P 0.42679(10) 1.11583(8) 0.29735(6) 0.01685(17) Uani 1 1 d . . . N1 N 0.3114(3) 0.9459(3) 0.28095(19) 0.0184(5) Uani 1 1 d . . . Na1 Na 0.24269(18) 1.00606(14) -0.04082(10) 0.0303(3) Uani 1 1 d . . . C10 C 0.2951(4) 0.6549(3) 0.1405(2) 0.0188(6) Uani 1 1 d . . . H10 H 0.2043 0.5598 0.0836 0.023 Uiso 1 1 calc R . . C11 C 0.3828(5) 0.6102(4) 0.2342(3) 0.0292(8) Uani 1 1 d . . . H11A H 0.4521 0.5432 0.2066 0.044 Uiso 1 1 calc R . . H11B H 0.2886 0.5562 0.2616 0.044 Uiso 1 1 calc R . . H11C H 0.4640 0.7026 0.2945 0.044 Uiso 1 1 calc R . . C12 C 0.4347(4) 0.7188(4) 0.0853(3) 0.0269(7) Uani 1 1 d . . . H12A H 0.5246 0.8133 0.1388 0.040 Uiso 1 1 calc R . . H12B H 0.3745 0.7407 0.0226 0.040 Uiso 1 1 calc R . . H12C H 0.4950 0.6435 0.0588 0.040 Uiso 1 1 calc R . . C20 C 0.0246(4) 0.7024(3) 0.2593(2) 0.0213(7) Uani 1 1 d . . . H20 H 0.1033 0.6934 0.3240 0.026 Uiso 1 1 calc R . . C21 C -0.0852(4) 0.8029(3) 0.3046(3) 0.0260(7) Uani 1 1 d . . . H21A H -0.1683 0.8102 0.2430 0.039 Uiso 1 1 calc R . . H21B H -0.0033 0.9054 0.3511 0.039 Uiso 1 1 calc R . . H21C H -0.1547 0.7579 0.3488 0.039 Uiso 1 1 calc R . . C22 C -0.1007(5) 0.5411(3) 0.1877(3) 0.0319(8) Uani 1 1 d . . . H22A H -0.1706 0.4968 0.2320 0.048 Uiso 1 1 calc R . . H22B H -0.0282 0.4770 0.1603 0.048 Uiso 1 1 calc R . . H22C H -0.1834 0.5461 0.1249 0.048 Uiso 1 1 calc R . . C30 C 0.3028(4) 1.2504(3) 0.3416(2) 0.0210(7) Uani 1 1 d . . . H30 H 0.3821 1.3556 0.3534 0.025 Uiso 1 1 calc R . . C31 C 0.2578(4) 1.2508(3) 0.4511(2) 0.0258(7) Uani 1 1 d . . . H31A H 0.1758 1.3107 0.4661 0.039 Uiso 1 1 calc R . . H31B H 0.3695 1.2965 0.5113 0.039 Uiso 1 1 calc R . . H31C H 0.1995 1.1454 0.4458 0.039 Uiso 1 1 calc R . . C32 C 0.1294(4) 1.2142(4) 0.2521(3) 0.0289(8) Uani 1 1 d . . . H32A H 0.0518 1.1095 0.2365 0.043 Uiso 1 1 calc R . . H32B H 0.1604 1.2234 0.1845 0.043 Uiso 1 1 calc R . . H32C H 0.0650 1.2864 0.2782 0.043 Uiso 1 1 calc R . . C40 C 0.6178(4) 1.1730(3) 0.4194(2) 0.0221(7) Uani 1 1 d . . . H40 H 0.5667 1.1588 0.4818 0.026 Uiso 1 1 calc R . . C41 C 0.7315(4) 1.3424(3) 0.4554(3) 0.0338(8) Uani 1 1 d . . . H41A H 0.8356 1.3662 0.5176 0.051 Uiso 1 1 calc R . . H41B H 0.6572 1.4070 0.4782 0.051 Uiso 1 1 calc R . . H41C H 0.7743 1.3619 0.3933 0.051 Uiso 1 1 calc R . . C42 C 0.7342(4) 1.0693(4) 0.3979(3) 0.0292(8) Uani 1 1 d . . . H42A H 0.7890 1.0830 0.3383 0.044 Uiso 1 1 calc R . . H42B H 0.6588 0.9624 0.3762 0.044 Uiso 1 1 calc R . . H42C H 0.8298 1.0957 0.4654 0.044 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 Se1 0.02612(18) 0.02238(16) 0.01698(17) 0.00785(13) 0.00179(13) 0.00875(13) Se2 0.02828(19) 0.02264(17) 0.01993(17) 0.00888(13) 0.01005(14) 0.00486(14) P1 0.0192(4) 0.0141(4) 0.0148(4) 0.0059(3) 0.0037(3) 0.0048(3) P2 0.0201(4) 0.0147(4) 0.0148(4) 0.0050(3) 0.0040(3) 0.0045(3) N1 0.0207(13) 0.0166(12) 0.0166(12) 0.0067(10) 0.0039(11) 0.0035(10) Na1 0.0328(7) 0.0358(7) 0.0263(7) 0.0138(6) 0.0092(6) 0.0134(6) C10 0.0207(16) 0.0157(14) 0.0184(15) 0.0035(12) 0.0046(13) 0.0063(12) C11 0.0316(19) 0.0302(17) 0.0368(19) 0.0198(15) 0.0120(16) 0.0171(15) C12 0.0278(19) 0.0297(17) 0.0275(18) 0.0105(14) 0.0106(15) 0.0133(15) C20 0.0238(17) 0.0203(15) 0.0198(16) 0.0102(13) 0.0041(13) 0.0043(13) C21 0.0249(17) 0.0278(17) 0.0246(17) 0.0079(14) 0.0107(14) 0.0061(14) C22 0.034(2) 0.0238(16) 0.037(2) 0.0113(15) 0.0168(16) 0.0027(15) C30 0.0284(18) 0.0155(14) 0.0201(16) 0.0061(12) 0.0078(14) 0.0079(13) C31 0.0342(19) 0.0233(16) 0.0234(17) 0.0070(13) 0.0125(15) 0.0126(14) C32 0.0341(19) 0.0287(17) 0.0311(18) 0.0131(15) 0.0093(15) 0.0186(15) C40 0.0240(17) 0.0212(15) 0.0163(16) 0.0048(13) -0.0001(13) 0.0050(13) C41 0.030(2) 0.0268(17) 0.0292(19) 0.0058(15) -0.0046(16) -0.0031(15) C42 0.0268(18) 0.0291(17) 0.0299(19) 0.0091(15) 0.0023(15) 0.0107(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 Se1 P1 2.1737(10) . ? Se1 Na1 2.9325(16) . ? Se1 Na1 3.0356(15) 2_575 ? Se2 P2 2.1741(10) . ? Se2 Na1 2.924(2) . ? Se2 Na1 3.0772(16) 2_675 ? P1 N1 1.600(2) . ? P1 C20 1.831(3) . ? P1 C10 1.845(3) . ? P2 N1 1.592(2) . ? P2 C40 1.838(3) . ? P2 C30 1.839(3) . ? C10 C12 1.521(4) . ? C10 C11 1.526(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C20 C21 1.521(4) . ? C20 C22 1.529(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C30 C32 1.532(4) . ? C30 C31 1.534(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C40 C42 1.522(4) . ? C40 C41 1.537(4) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Se1 Na1 107.04(4) . . ? P1 Se1 Na1 125.36(4) . 2_575 ? Na1 Se1 Na1 88.01(4) . 2_575 ? P2 Se2 Na1 107.61(4) . . ? P2 Se2 Na1 124.67(4) . 2_675 ? Na1 Se2 Na1 85.37(4) . 2_675 ? N1 P1 C20 105.25(13) . . ? N1 P1 C10 110.26(13) . . ? C20 P1 C10 104.52(13) . . ? N1 P1 Se1 120.23(9) . . ? C20 P1 Se1 108.20(10) . . ? C10 P1 Se1 107.27(10) . . ? N1 P2 C40 105.48(13) . . ? N1 P2 C30 110.91(14) . . ? C40 P2 C30 103.20(13) . . ? N1 P2 Se2 120.41(10) . . ? C40 P2 Se2 108.52(11) . . ? C30 P2 Se2 106.98(10) . . ? P2 N1 P1 141.59(16) . . ? Se2 Na1 Se1 97.23(5) . . ? Se2 Na1 Se1 106.40(5) . 2_575 ? Se1 Na1 Se1 91.99(4) . 2_575 ? Se2 Na1 Se2 94.63(4) . 2_675 ? Se1 Na1 Se2 109.10(4) . 2_675 ? Se1 Na1 Se2 148.16(5) 2_575 2_675 ? C12 C10 C11 110.8(3) . . ? C12 C10 P1 110.6(2) . . ? C11 C10 P1 112.3(2) . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? P1 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C20 C22 110.3(3) . . ? C21 C20 P1 111.0(2) . . ? C22 C20 P1 113.4(2) . . ? C21 C20 H20 107.3 . . ? C22 C20 H20 107.3 . . ? P1 C20 H20 107.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C32 C30 C31 110.1(3) . . ? C32 C30 P2 111.1(2) . . ? C31 C30 P2 111.7(2) . . ? C32 C30 H30 107.9 . . ? C31 C30 H30 107.9 . . ? P2 C30 H30 107.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C40 C41 111.2(3) . . ? C42 C40 P2 110.3(2) . . ? C41 C40 P2 112.3(2) . . ? C42 C40 H40 107.6 . . ? C41 C40 H40 107.6 . . ? P2 C40 H40 107.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Na1 Se1 P1 N1 46.10(12) . . . . ? Na1 Se1 P1 N1 -53.85(12) 2_575 . . . ? Na1 Se1 P1 C20 166.91(10) . . . . ? Na1 Se1 P1 C20 66.96(11) 2_575 . . . ? Na1 Se1 P1 C10 -80.84(11) . . . . ? Na1 Se1 P1 C10 179.21(10) 2_575 . . . ? Na1 Se2 P2 N1 44.52(12) . . . . ? Na1 Se2 P2 N1 -52.18(12) 2_675 . . . ? Na1 Se2 P2 C40 166.06(10) . . . . ? Na1 Se2 P2 C40 69.36(11) 2_675 . . . ? Na1 Se2 P2 C30 -83.21(11) . . . . ? Na1 Se2 P2 C30 -179.90(10) 2_675 . . . ? C40 P2 N1 P1 -154.0(3) . . . . ? C30 P2 N1 P1 94.9(3) . . . . ? Se2 P2 N1 P1 -31.0(3) . . . . ? C20 P1 N1 P2 -148.7(3) . . . . ? C10 P1 N1 P2 99.1(3) . . . . ? Se1 P1 N1 P2 -26.5(3) . . . . ? P2 Se2 Na1 Se1 -15.02(4) . . . . ? Na1 Se2 Na1 Se1 109.95(5) 2_675 . . . ? P2 Se2 Na1 Se1 79.22(5) . . . 2_575 ? Na1 Se2 Na1 Se1 -155.82(6) 2_675 . . 2_575 ? P2 Se2 Na1 Se2 -124.97(4) . . . 2_675 ? Na1 Se2 Na1 Se2 0.0 2_675 . . 2_675 ? P1 Se1 Na1 Se2 -19.70(4) . . . . ? Na1 Se1 Na1 Se2 106.81(5) 2_575 . . . ? P1 Se1 Na1 Se1 -126.51(4) . . . 2_575 ? Na1 Se1 Na1 Se1 0.0 2_575 . . 2_575 ? P1 Se1 Na1 Se2 77.77(5) . . . 2_675 ? Na1 Se1 Na1 Se2 -155.72(6) 2_575 . . 2_675 ? N1 P1 C10 C12 -63.7(2) . . . . ? C20 P1 C10 C12 -176.4(2) . . . . ? Se1 P1 C10 C12 68.9(2) . . . . ? N1 P1 C10 C11 60.6(2) . . . . ? C20 P1 C10 C11 -52.0(2) . . . . ? Se1 P1 C10 C11 -166.75(19) . . . . ? N1 P1 C20 C21 63.4(2) . . . . ? C10 P1 C20 C21 179.6(2) . . . . ? Se1 P1 C20 C21 -66.3(2) . . . . ? N1 P1 C20 C22 -171.8(2) . . . . ? C10 P1 C20 C22 -55.6(2) . . . . ? Se1 P1 C20 C22 58.5(2) . . . . ? N1 P2 C30 C32 -63.9(2) . . . . ? C40 P2 C30 C32 -176.4(2) . . . . ? Se2 P2 C30 C32 69.2(2) . . . . ? N1 P2 C30 C31 59.4(2) . . . . ? C40 P2 C30 C31 -53.1(2) . . . . ? Se2 P2 C30 C31 -167.46(18) . . . . ? N1 P2 C40 C42 62.2(2) . . . . ? C30 P2 C40 C42 178.6(2) . . . . ? Se2 P2 C40 C42 -68.1(2) . . . . ? N1 P2 C40 C41 -173.2(2) . . . . ? C30 P2 C40 C41 -56.8(3) . . . . ? Se2 P2 C40 C41 56.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.432 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.077 #===END data_5Na _database_code_depnum_ccdc_archive 'CCDC 666806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N Na P2 Te2' _chemical_formula_sum 'C12 H28 N Na P2 Te2' _chemical_formula_weight 526.48 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' Na Na 0.0362 0.0249 '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 8.0496(16) _cell_length_b 10.349(2) _cell_length_c 12.897(3) _cell_angle_alpha 103.58(3) _cell_angle_beta 102.01(3) _cell_angle_gamma 106.27(3) _cell_volume 958.4(5) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 3.220 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8820 _exptl_absorpt_correction_T_max 0.9384 _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 18304 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3334 _reflns_number_gt 2990 _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^)+(0.0265P)^2^+1.2459P] 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 3334 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Te1 Te -0.87588(3) 0.98525(2) 0.180470(19) 0.03263(9) Uani 1 1 d . . . Te2 Te -0.45085(3) 1.23635(2) 0.026829(18) 0.03015(9) Uani 1 1 d . . . Na1 Na -0.2145(2) 1.04247(16) 0.04749(13) 0.0423(4) Uani 1 1 d . . . P1 P -0.62663(11) 1.18259(8) 0.31713(7) 0.02144(17) Uani 1 1 d . . . C1 C -0.4592(4) 1.1059(3) 0.3711(3) 0.0259(7) Uani 1 1 d . . . H1A H -0.5251 1.0212 0.3898 0.031 Uiso 1 1 calc R . . C2 C -0.3727(5) 1.0553(4) 0.2817(3) 0.0348(8) Uani 1 1 d . . . H2A H -0.2878 1.0115 0.3110 0.052 Uiso 1 1 calc R . . H2B H -0.3075 1.1363 0.2614 0.052 Uiso 1 1 calc R . . H2C H -0.4673 0.9856 0.2156 0.052 Uiso 1 1 calc R . . C3 C -0.3145(5) 1.2095(4) 0.4777(3) 0.0330(8) Uani 1 1 d . . . H3A H -0.2167 1.1722 0.4959 0.050 Uiso 1 1 calc R . . H3B H -0.3685 1.2213 0.5392 0.050 Uiso 1 1 calc R . . H3C H -0.2657 1.3013 0.4662 0.050 Uiso 1 1 calc R . . C4 C -0.8421(5) 1.3164(4) 0.4057(3) 0.0357(8) Uani 1 1 d . . . H4A H -0.8768 1.3548 0.4716 0.053 Uiso 1 1 calc R . . H4B H -0.9496 1.2460 0.3477 0.053 Uiso 1 1 calc R . . H4C H -0.7888 1.3934 0.3776 0.053 Uiso 1 1 calc R . . C5 C -0.7041(4) 1.2466(3) 0.4373(3) 0.0262(7) Uani 1 1 d . . . H5A H -0.5966 1.3216 0.4960 0.031 Uiso 1 1 calc R . . C6 C -0.7773(5) 1.1310(4) 0.4889(3) 0.0370(8) Uani 1 1 d . . . H6A H -0.8092 1.1726 0.5550 0.055 Uiso 1 1 calc R . . H6B H -0.6843 1.0903 0.5103 0.055 Uiso 1 1 calc R . . H6C H -0.8851 1.0565 0.4341 0.055 Uiso 1 1 calc R . . N1 N -0.5310(3) 1.3208(3) 0.2886(2) 0.0245(6) Uani 1 1 d . . . P2 P -0.48310(10) 1.38332(8) 0.19207(7) 0.02073(17) Uani 1 1 d . . . C7 C -0.2103(5) 1.6208(4) 0.1883(3) 0.0410(9) Uani 1 1 d . . . H7A H -0.0959 1.6981 0.2308 0.062 Uiso 1 1 calc R . . H7B H -0.3039 1.6603 0.1651 0.062 Uiso 1 1 calc R . . H7C H -0.1944 1.5620 0.1222 0.062 Uiso 1 1 calc R . . C8 C -0.2676(4) 1.5306(3) 0.2612(3) 0.0266(7) Uani 1 1 d . . . H8A H -0.2845 1.5938 0.3268 0.032 Uiso 1 1 calc R . . C9 C -0.1177(5) 1.4779(4) 0.3067(3) 0.0347(8) Uani 1 1 d . . . H9A H -0.0068 1.5590 0.3486 0.052 Uiso 1 1 calc R . . H9B H -0.0953 1.4168 0.2446 0.052 Uiso 1 1 calc R . . H9C H -0.1547 1.4240 0.3562 0.052 Uiso 1 1 calc R . . C10 C -0.8360(5) 1.3559(4) 0.0907(3) 0.0333(8) Uani 1 1 d . . . H10A H -0.9200 1.4009 0.0624 0.050 Uiso 1 1 calc R . . H10B H -0.8747 1.3161 0.1472 0.050 Uiso 1 1 calc R . . H10C H -0.8355 1.2799 0.0290 0.050 Uiso 1 1 calc R . . C11 C -0.6461(4) 1.4658(3) 0.1427(3) 0.0250(7) Uani 1 1 d . . . H11A H -0.6101 1.5027 0.0827 0.030 Uiso 1 1 calc R . . C12 C -0.6434(5) 1.5916(4) 0.2344(3) 0.0337(8) Uani 1 1 d . . . H12A H -0.7330 1.6310 0.2042 0.051 Uiso 1 1 calc R . . H12B H -0.5227 1.6646 0.2614 0.051 Uiso 1 1 calc R . . H12C H -0.6728 1.5598 0.2963 0.051 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 Te1 0.02955(14) 0.02550(13) 0.02957(14) 0.00593(10) -0.00145(10) -0.00070(10) Te2 0.04038(15) 0.02822(13) 0.02365(13) 0.00626(10) 0.01078(10) 0.01511(10) Na1 0.0369(8) 0.0434(8) 0.0404(9) 0.0040(7) 0.0050(7) 0.0170(7) P1 0.0212(4) 0.0204(4) 0.0202(4) 0.0068(3) 0.0034(3) 0.0050(3) C1 0.0259(16) 0.0237(16) 0.0270(17) 0.0093(14) 0.0058(14) 0.0072(13) C2 0.039(2) 0.038(2) 0.032(2) 0.0101(16) 0.0118(16) 0.0210(16) C3 0.0295(18) 0.0365(19) 0.0296(19) 0.0098(15) 0.0014(15) 0.0119(15) C4 0.036(2) 0.044(2) 0.034(2) 0.0139(17) 0.0138(16) 0.0205(17) C5 0.0276(17) 0.0286(17) 0.0231(17) 0.0092(14) 0.0089(14) 0.0088(14) C6 0.048(2) 0.0366(19) 0.036(2) 0.0208(17) 0.0200(18) 0.0149(17) N1 0.0240(14) 0.0232(13) 0.0250(14) 0.0102(11) 0.0070(11) 0.0042(11) P2 0.0219(4) 0.0186(4) 0.0201(4) 0.0056(3) 0.0055(3) 0.0054(3) C7 0.037(2) 0.036(2) 0.045(2) 0.0210(18) 0.0070(18) 0.0010(16) C8 0.0255(17) 0.0224(16) 0.0252(17) 0.0037(13) 0.0066(14) 0.0018(13) C9 0.0245(17) 0.0370(19) 0.036(2) 0.0085(16) 0.0046(15) 0.0053(15) C10 0.0248(17) 0.0363(19) 0.034(2) 0.0104(16) 0.0038(15) 0.0077(15) C11 0.0265(16) 0.0243(16) 0.0253(17) 0.0096(13) 0.0062(13) 0.0099(13) C12 0.041(2) 0.0285(18) 0.0345(19) 0.0075(15) 0.0107(16) 0.0185(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 Te1 P1 2.4176(16) . ? Te1 Na1 3.1411(17) 2_475 ? Te1 Na1 3.1870(17) 1_455 ? Te2 P2 2.4191(11) . ? Te2 Na1 3.126(2) 2_475 ? Te2 Na1 3.1458(17) . ? Na1 Na1 4.142(3) 2_575 ? P1 N1 1.589(3) . ? P1 C5 1.839(3) . ? P1 C1 1.844(3) . ? C1 C3 1.529(5) . ? C1 C2 1.531(5) . ? C4 C5 1.524(5) . ? C5 C6 1.537(5) . ? N1 P2 1.598(3) . ? P2 C8 1.834(3) . ? P2 C11 1.841(3) . ? C7 C8 1.522(5) . ? C8 C9 1.524(5) . ? C10 C11 1.524(5) . ? C11 C12 1.531(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Na1 105.85(5) . 2_475 ? P1 Te1 Na1 119.22(4) . 1_455 ? Na1 Te1 Na1 81.76(5) 2_475 1_455 ? P2 Te2 Na1 104.28(5) . 2_475 ? P2 Te2 Na1 120.44(4) . . ? Na1 Te2 Na1 85.97(4) 2_475 . ? Te2 Na1 Te1 98.80(5) 2_475 2_475 ? Te2 Na1 Te2 94.03(4) 2_475 . ? Te1 Na1 Te2 98.70(5) 2_475 . ? Te2 Na1 Te1 107.44(5) 2_475 1_655 ? Te1 Na1 Te1 98.24(5) 2_475 1_655 ? Te2 Na1 Te1 150.13(5) . 1_655 ? N1 P1 C5 104.99(15) . . ? N1 P1 C1 110.66(15) . . ? C5 P1 C1 104.36(15) . . ? N1 P1 Te1 121.90(11) . . ? C5 P1 Te1 108.11(11) . . ? C1 P1 Te1 105.53(11) . . ? C3 C1 C2 110.9(3) . . ? C3 C1 P1 112.0(2) . . ? C2 C1 P1 110.7(2) . . ? C4 C5 C6 111.5(3) . . ? C4 C5 P1 110.4(2) . . ? C6 C5 P1 113.2(2) . . ? P1 N1 P2 145.37(19) . . ? N1 P2 C8 104.89(15) . . ? N1 P2 C11 110.73(15) . . ? C8 P2 C11 105.01(15) . . ? N1 P2 Te2 121.22(10) . . ? C8 P2 Te2 107.54(11) . . ? C11 P2 Te2 106.32(11) . . ? C7 C8 C9 110.7(3) . . ? C7 C8 P2 113.8(2) . . ? C9 C8 P2 111.0(2) . . ? C10 C11 C12 111.2(3) . . ? C10 C11 P2 110.6(2) . . ? C12 C11 P2 112.7(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.464 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.095 #===END data_4Li _database_code_depnum_ccdc_archive 'CCDC 666807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H44 Li N3 P2 Se2' _chemical_formula_sum 'C18 H44 Li N3 P2 Se2' _chemical_formula_weight 529.36 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' Li Li -0.0003 0.0001 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9918(4) _cell_length_b 14.3484(8) _cell_length_c 19.232(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.06(3) _cell_angle_gamma 90.00 _cell_volume 2662.5(5) _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 plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 2.905 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5943 _exptl_absorpt_correction_T_max 0.8009 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski and Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_reflns_number 17981 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4559 _reflns_number_gt 3183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0475P)^2^+0.2064P] 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 4559 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Se1 Se 0.88950(5) 0.88239(4) 0.00818(3) 0.02906(17) Uani 1 1 d . . . Se2 Se 0.61499(5) 0.74287(4) -0.16786(3) 0.02601(16) Uani 1 1 d . . . P1 P 0.81677(12) 0.75492(9) 0.04560(7) 0.0207(3) Uani 1 1 d . . . P2 P 0.55771(12) 0.70989(9) -0.06979(7) 0.0185(3) Uani 1 1 d . . . N1 N 0.6687(4) 0.7143(3) 0.0060(2) 0.0210(9) Uani 1 1 d . . . N2 N 0.7107(4) 1.0057(3) -0.1739(2) 0.0287(10) Uani 1 1 d . . . N3 N 0.9325(4) 0.8774(3) -0.1873(2) 0.0305(11) Uani 1 1 d . . . Li1 Li 0.7821(8) 0.8760(6) -0.1277(5) 0.027(2) Uani 1 1 d . . . C10 C 0.9449(5) 0.6627(4) 0.0482(3) 0.0298(13) Uani 1 1 d . . . H10 H 0.9069 0.6042 0.0640 0.036 Uiso 1 1 calc R . . C11 C 1.0840(5) 0.6822(4) 0.1024(3) 0.0419(16) Uani 1 1 d . . . H11A H 1.1508 0.6338 0.0984 0.063 Uiso 1 1 calc R . . H11B H 1.0716 0.6822 0.1513 0.063 Uiso 1 1 calc R . . H11C H 1.1188 0.7432 0.0921 0.063 Uiso 1 1 calc R . . C12 C 0.9646(5) 0.6446(4) -0.0265(3) 0.0383(15) Uani 1 1 d . . . H12A H 1.0102 0.6984 -0.0418 0.057 Uiso 1 1 calc R . . H12B H 0.8741 0.6347 -0.0606 0.057 Uiso 1 1 calc R . . H12C H 1.0222 0.5890 -0.0252 0.057 Uiso 1 1 calc R . . C20 C 0.8137(5) 0.7732(4) 0.1398(3) 0.0283(13) Uani 1 1 d . . . H20 H 0.9087 0.7927 0.1673 0.034 Uiso 1 1 calc R . . C21 C 0.7777(5) 0.6837(4) 0.1742(3) 0.0380(15) Uani 1 1 d . . . H21A H 0.7804 0.6955 0.2247 0.057 Uiso 1 1 calc R . . H21B H 0.8450 0.6350 0.1715 0.057 Uiso 1 1 calc R . . H21C H 0.6845 0.6631 0.1484 0.057 Uiso 1 1 calc R . . C22 C 0.7130(6) 0.8517(4) 0.1458(3) 0.0395(15) Uani 1 1 d . . . H22A H 0.6181 0.8328 0.1216 0.059 Uiso 1 1 calc R . . H22B H 0.7368 0.9082 0.1230 0.059 Uiso 1 1 calc R . . H22C H 0.7198 0.8642 0.1967 0.059 Uiso 1 1 calc R . . C30 C 0.4094(5) 0.7823(3) -0.0652(3) 0.0238(12) Uani 1 1 d . . . H30 H 0.3372 0.7759 -0.1119 0.029 Uiso 1 1 calc R . . C31 C 0.3459(5) 0.7492(4) -0.0047(3) 0.0312(13) Uani 1 1 d . . . H31A H 0.4180 0.7474 0.0409 0.047 Uiso 1 1 calc R . . H31B H 0.3068 0.6866 -0.0160 0.047 Uiso 1 1 calc R . . H31C H 0.2724 0.7923 -0.0004 0.047 Uiso 1 1 calc R . . C32 C 0.4517(5) 0.8849(3) -0.0556(3) 0.0327(13) Uani 1 1 d . . . H32A H 0.3712 0.9228 -0.0536 0.049 Uiso 1 1 calc R . . H32B H 0.4867 0.9051 -0.0963 0.049 Uiso 1 1 calc R . . H32C H 0.5245 0.8926 -0.0107 0.049 Uiso 1 1 calc R . . C40 C 0.4916(5) 0.5902(3) -0.0786(3) 0.0273(12) Uani 1 1 d . . . H40 H 0.4601 0.5762 -0.0344 0.033 Uiso 1 1 calc R . . C41 C 0.6085(5) 0.5217(4) -0.0799(3) 0.0323(13) Uani 1 1 d . . . H41A H 0.5716 0.4580 -0.0855 0.048 Uiso 1 1 calc R . . H41B H 0.6812 0.5264 -0.0347 0.048 Uiso 1 1 calc R . . H41C H 0.6474 0.5367 -0.1203 0.048 Uiso 1 1 calc R . . C42 C 0.3668(5) 0.5777(4) -0.1430(3) 0.0414(15) Uani 1 1 d . . . H42A H 0.3907 0.5983 -0.1869 0.062 Uiso 1 1 calc R . . H42B H 0.2892 0.6149 -0.1359 0.062 Uiso 1 1 calc R . . H42C H 0.3403 0.5118 -0.1477 0.062 Uiso 1 1 calc R . . C51 C 0.8877(6) 0.9541(5) -0.2356(4) 0.0526(18) Uani 1 1 d . . . H51A H 0.8152 0.9320 -0.2779 0.063 Uiso 1 1 calc R . . H51B H 0.9669 0.9765 -0.2530 0.063 Uiso 1 1 calc R . . C52 C 0.8320(7) 1.0327(4) -0.2018(4) 0.0531(18) Uani 1 1 d . . . H52A H 0.8034 1.0832 -0.2377 0.064 Uiso 1 1 calc R . . H52B H 0.9064 1.0574 -0.1615 0.064 Uiso 1 1 calc R . . C53 C 0.9325(7) 0.7928(5) -0.2305(4) 0.065(2) Uani 1 1 d . . . H53A H 0.8388 0.7814 -0.2609 0.097 Uiso 1 1 calc R . . H53B H 0.9623 0.7394 -0.1984 0.097 Uiso 1 1 calc R . . H53C H 0.9964 0.8010 -0.2610 0.097 Uiso 1 1 calc R . . C54 C 1.0725(5) 0.8899(4) -0.1414(3) 0.0397(15) Uani 1 1 d . . . H54A H 1.1380 0.8943 -0.1713 0.060 Uiso 1 1 calc R . . H54B H 1.0970 0.8367 -0.1086 0.060 Uiso 1 1 calc R . . H54C H 1.0765 0.9473 -0.1133 0.060 Uiso 1 1 calc R . . C55 C 0.5834(6) 1.0004(4) -0.2306(3) 0.0502(16) Uani 1 1 d . . . H55A H 0.5068 0.9842 -0.2098 0.075 Uiso 1 1 calc R . . H55B H 0.5925 0.9526 -0.2654 0.075 Uiso 1 1 calc R . . H55C H 0.5648 1.0609 -0.2549 0.075 Uiso 1 1 calc R . . C56 C 0.6952(6) 1.0745(4) -0.1211(3) 0.0365(14) Uani 1 1 d . . . H56A H 0.6783 1.1359 -0.1440 0.055 Uiso 1 1 calc R . . H56B H 0.7801 1.0766 -0.0817 0.055 Uiso 1 1 calc R . . H56C H 0.6168 1.0574 -0.1019 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 Se1 0.0339(3) 0.0282(3) 0.0206(3) 0.0039(2) -0.0011(2) -0.0109(2) Se2 0.0320(3) 0.0288(3) 0.0173(3) -0.0007(2) 0.0065(2) -0.0068(2) P1 0.0191(6) 0.0236(7) 0.0170(7) 0.0017(6) 0.0003(5) -0.0021(6) P2 0.0186(6) 0.0190(7) 0.0165(8) -0.0007(6) 0.0023(5) -0.0026(5) N1 0.019(2) 0.028(2) 0.014(2) 0.0009(18) 0.0019(18) -0.0031(17) N2 0.032(2) 0.023(3) 0.031(3) 0.003(2) 0.008(2) -0.0008(19) N3 0.027(2) 0.038(3) 0.025(3) 0.000(2) 0.005(2) 0.000(2) Li1 0.028(4) 0.028(5) 0.023(5) 0.002(4) 0.002(4) -0.003(4) C10 0.024(3) 0.028(3) 0.038(4) 0.010(3) 0.010(3) 0.001(2) C11 0.021(3) 0.054(4) 0.046(4) 0.016(3) 0.001(3) 0.004(3) C12 0.029(3) 0.041(4) 0.046(4) 0.001(3) 0.012(3) 0.006(3) C20 0.028(3) 0.039(3) 0.014(3) 0.001(2) -0.001(2) -0.007(2) C21 0.037(3) 0.051(4) 0.027(4) 0.004(3) 0.010(3) -0.015(3) C22 0.046(3) 0.045(4) 0.027(4) -0.012(3) 0.009(3) -0.001(3) C30 0.024(3) 0.021(3) 0.026(3) -0.004(2) 0.006(2) 0.001(2) C31 0.025(3) 0.034(3) 0.038(4) -0.001(3) 0.014(3) 0.005(2) C32 0.031(3) 0.028(3) 0.038(4) 0.000(3) 0.008(3) 0.002(2) C40 0.027(3) 0.026(3) 0.028(3) -0.001(2) 0.006(2) -0.008(2) C41 0.045(3) 0.022(3) 0.032(4) -0.004(3) 0.014(3) -0.002(2) C42 0.041(3) 0.030(3) 0.047(4) -0.011(3) -0.001(3) -0.008(3) C51 0.048(4) 0.073(5) 0.038(4) 0.022(4) 0.014(3) 0.001(3) C52 0.082(5) 0.033(4) 0.054(5) 0.016(3) 0.035(4) 0.002(3) C53 0.059(4) 0.079(5) 0.067(5) -0.036(4) 0.035(4) -0.020(4) C54 0.027(3) 0.054(4) 0.038(4) 0.002(3) 0.006(3) -0.004(3) C55 0.065(4) 0.042(4) 0.030(4) 0.005(3) -0.013(3) -0.001(3) C56 0.041(3) 0.021(3) 0.043(4) -0.004(3) 0.002(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 P1 2.1595(14) . ? Se1 Li1 2.556(9) . ? Se2 P2 2.1610(14) . ? Se2 Li1 2.522(8) . ? P1 N1 1.589(4) . ? P1 C10 1.833(5) . ? P1 C20 1.839(5) . ? P2 N1 1.586(4) . ? P2 C30 1.831(5) . ? P2 C40 1.832(5) . ? N2 C55 1.446(7) . ? N2 C56 1.454(6) . ? N2 C52 1.498(7) . ? N2 Li1 2.106(9) . ? N3 C51 1.434(7) . ? N3 C54 1.460(6) . ? N3 C53 1.471(7) . ? N3 Li1 2.114(9) . ? Li1 C52 2.775(10) . ? C10 C12 1.523(7) . ? C10 C11 1.531(7) . ? C20 C21 1.530(7) . ? C20 C22 1.535(7) . ? C30 C32 1.530(7) . ? C30 C31 1.539(7) . ? C40 C42 1.524(7) . ? C40 C41 1.532(7) . ? C51 C52 1.480(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 P1 Se1 Li1 102.83(19) . . ? P2 Se2 Li1 101.72(19) . . ? N1 P1 C10 107.8(2) . . ? N1 P1 C20 105.9(2) . . ? C10 P1 C20 105.4(2) . . ? N1 P1 Se1 120.19(16) . . ? C10 P1 Se1 109.12(16) . . ? C20 P1 Se1 107.52(17) . . ? N1 P2 C30 108.3(2) . . ? N1 P2 C40 105.7(2) . . ? C30 P2 C40 105.0(2) . . ? N1 P2 Se2 120.81(14) . . ? C30 P2 Se2 108.61(17) . . ? C40 P2 Se2 107.20(18) . . ? P2 N1 P1 142.8(3) . . ? C55 N2 C56 109.3(4) . . ? C55 N2 C52 112.3(5) . . ? C56 N2 C52 108.6(4) . . ? C55 N2 Li1 114.0(4) . . ? C56 N2 Li1 113.0(4) . . ? C52 N2 Li1 99.4(4) . . ? C51 N3 C54 112.7(5) . . ? C51 N3 C53 108.3(5) . . ? C54 N3 C53 107.6(5) . . ? C51 N3 Li1 102.3(4) . . ? C54 N3 Li1 112.2(4) . . ? C53 N3 Li1 113.7(4) . . ? N2 Li1 N3 88.5(3) . . ? N2 Li1 Se2 114.6(4) . . ? N3 Li1 Se2 110.4(4) . . ? N2 Li1 Se1 113.9(4) . . ? N3 Li1 Se1 112.7(3) . . ? Se2 Li1 Se1 114.1(3) . . ? N2 Li1 C52 32.2(2) . . ? N3 Li1 C52 57.7(3) . . ? Se2 Li1 C52 130.5(4) . . ? Se1 Li1 C52 114.3(3) . . ? C12 C10 C11 110.8(4) . . ? C12 C10 P1 110.9(4) . . ? C11 C10 P1 113.0(4) . . ? C21 C20 C22 110.5(4) . . ? C21 C20 P1 111.9(4) . . ? C22 C20 P1 111.0(4) . . ? C32 C30 C31 111.2(4) . . ? C32 C30 P2 110.5(3) . . ? C31 C30 P2 111.1(3) . . ? C42 C40 C41 112.1(4) . . ? C42 C40 P2 112.6(4) . . ? C41 C40 P2 110.2(3) . . ? N3 C51 C52 112.9(5) . . ? C51 C52 N2 113.1(5) . . ? C51 C52 Li1 75.3(4) . . ? N2 C52 Li1 48.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 Se1 P1 N1 -33.0(3) . . . . ? Li1 Se1 P1 C10 92.1(3) . . . . ? Li1 Se1 P1 C20 -154.0(2) . . . . ? Li1 Se2 P2 N1 -37.8(3) . . . . ? Li1 Se2 P2 C30 88.2(3) . . . . ? Li1 Se2 P2 C40 -158.8(3) . . . . ? C30 P2 N1 P1 -108.5(4) . . . . ? C40 P2 N1 P1 139.3(4) . . . . ? Se2 P2 N1 P1 17.6(5) . . . . ? C10 P1 N1 P2 -97.0(5) . . . . ? C20 P1 N1 P2 150.6(4) . . . . ? Se1 P1 N1 P2 28.7(5) . . . . ? C55 N2 Li1 N3 103.5(4) . . . . ? C56 N2 Li1 N3 -131.0(4) . . . . ? C52 N2 Li1 N3 -16.1(4) . . . . ? C55 N2 Li1 Se2 -8.3(5) . . . . ? C56 N2 Li1 Se2 117.2(4) . . . . ? C52 N2 Li1 Se2 -127.9(4) . . . . ? C55 N2 Li1 Se1 -142.3(4) . . . . ? C56 N2 Li1 Se1 -16.8(5) . . . . ? C52 N2 Li1 Se1 98.1(4) . . . . ? C55 N2 Li1 C52 119.6(5) . . . . ? C56 N2 Li1 C52 -114.9(5) . . . . ? C51 N3 Li1 N2 -10.6(5) . . . . ? C54 N3 Li1 N2 110.4(4) . . . . ? C53 N3 Li1 N2 -127.1(5) . . . . ? C51 N3 Li1 Se2 105.1(5) . . . . ? C54 N3 Li1 Se2 -133.9(4) . . . . ? C53 N3 Li1 Se2 -11.4(6) . . . . ? C51 N3 Li1 Se1 -126.0(4) . . . . ? C54 N3 Li1 Se1 -5.0(6) . . . . ? C53 N3 Li1 Se1 117.5(5) . . . . ? C51 N3 Li1 C52 -20.7(4) . . . . ? C54 N3 Li1 C52 100.4(4) . . . . ? C53 N3 Li1 C52 -137.2(5) . . . . ? P2 Se2 Li1 N2 -112.4(3) . . . . ? P2 Se2 Li1 N3 149.6(3) . . . . ? P2 Se2 Li1 Se1 21.5(3) . . . . ? P2 Se2 Li1 C52 -146.0(4) . . . . ? P1 Se1 Li1 N2 141.0(3) . . . . ? P1 Se1 Li1 N3 -120.1(3) . . . . ? P1 Se1 Li1 Se2 6.8(3) . . . . ? P1 Se1 Li1 C52 176.4(3) . . . . ? N1 P1 C10 C12 70.8(4) . . . . ? C20 P1 C10 C12 -176.5(4) . . . . ? Se1 P1 C10 C12 -61.2(4) . . . . ? N1 P1 C10 C11 -163.9(4) . . . . ? C20 P1 C10 C11 -51.2(4) . . . . ? Se1 P1 C10 C11 64.0(4) . . . . ? N1 P1 C20 C21 56.2(4) . . . . ? C10 P1 C20 C21 -57.9(4) . . . . ? Se1 P1 C20 C21 -174.2(3) . . . . ? N1 P1 C20 C22 -67.8(4) . . . . ? C10 P1 C20 C22 178.2(4) . . . . ? Se1 P1 C20 C22 61.8(4) . . . . ? N1 P2 C30 C32 65.8(4) . . . . ? C40 P2 C30 C32 178.4(4) . . . . ? Se2 P2 C30 C32 -67.2(4) . . . . ? N1 P2 C30 C31 -58.1(4) . . . . ? C40 P2 C30 C31 54.5(4) . . . . ? Se2 P2 C30 C31 169.0(3) . . . . ? N1 P2 C40 C42 170.7(4) . . . . ? C30 P2 C40 C42 56.2(4) . . . . ? Se2 P2 C40 C42 -59.2(4) . . . . ? N1 P2 C40 C41 -63.2(4) . . . . ? C30 P2 C40 C41 -177.7(4) . . . . ? Se2 P2 C40 C41 66.9(4) . . . . ? C54 N3 C51 C52 -83.2(6) . . . . ? C53 N3 C51 C52 157.8(5) . . . . ? Li1 N3 C51 C52 37.4(6) . . . . ? N3 C51 C52 N2 -58.9(7) . . . . ? N3 C51 C52 Li1 -27.9(5) . . . . ? C55 N2 C52 C51 -79.0(6) . . . . ? C56 N2 C52 C51 160.1(5) . . . . ? Li1 N2 C52 C51 41.8(6) . . . . ? C55 N2 C52 Li1 -120.8(5) . . . . ? C56 N2 C52 Li1 118.3(5) . . . . ? N2 Li1 C52 C51 -140.7(6) . . . . ? N3 Li1 C52 C51 20.2(4) . . . . ? Se2 Li1 C52 C51 -69.9(5) . . . . ? Se1 Li1 C52 C51 122.6(5) . . . . ? N3 Li1 C52 N2 160.9(5) . . . . ? Se2 Li1 C52 N2 70.7(5) . . . . ? Se1 Li1 C52 N2 -96.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.815 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.205 #===END data_5Li _database_code_depnum_ccdc_archive 'CCDC 666808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H44 Li N3 P2 Te2' _chemical_formula_sum 'C18 H44 Li N3 P2 Te2' _chemical_formula_weight 626.64 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.895(5) _cell_length_b 14.5762(4) _cell_length_c 19.910(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.171(2) _cell_angle_gamma 90.00 _cell_volume 2796.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14792 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The structure was well-ordered with the exception of the coordinated TMEDA molecule, which was disordered over two sites. The disorder was modeled as an isotropic 50:50 mixture with mild geometric restraints. ; _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_reflns_number 16994 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4921 _reflns_number_gt 3765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius DENZO' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0503P)^2^+1.9871P] 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 4921 _refine_ls_number_parameters 240 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.048 _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 Te1 Te 0.10916(4) 0.38904(2) 0.001714(19) 0.03737(14) Uani 1 1 d . A . Te2 Te 0.23400(4) 0.24666(2) -0.178872(18) 0.03761(13) Uani 1 1 d . A . P1 P 0.23568(14) 0.24920(8) 0.03712(7) 0.0281(3) Uani 1 1 d . . . P2 P 0.39729(14) 0.21514(8) -0.07238(7) 0.0290(3) Uani 1 1 d . . . N1 N 0.3517(4) 0.2148(3) -0.0004(2) 0.0295(9) Uani 1 1 d . . . C10 C 0.1111(6) 0.1556(3) 0.0361(3) 0.0394(14) Uani 1 1 d . . . H10 H 0.1669 0.0985 0.0490 0.047 Uiso 1 1 calc R . . C11 C 0.0223(6) 0.1400(4) -0.0354(3) 0.0525(16) Uani 1 1 d . . . H11A H -0.0328 0.0841 -0.0356 0.079 Uiso 1 1 calc R . . H11B H 0.0820 0.1332 -0.0682 0.079 Uiso 1 1 calc R . . H11C H -0.0400 0.1924 -0.0488 0.079 Uiso 1 1 calc R . . C12 C 0.0217(6) 0.1669(4) 0.0891(3) 0.0560(17) Uani 1 1 d . . . H12A H -0.0274 0.2257 0.0817 0.084 Uiso 1 1 calc R . . H12B H 0.0813 0.1654 0.1358 0.084 Uiso 1 1 calc R . . H12C H -0.0459 0.1168 0.0839 0.084 Uiso 1 1 calc R . . C20 C 0.3229(6) 0.2637(3) 0.1283(3) 0.0385(13) Uani 1 1 d . . . H20 H 0.2504 0.2785 0.1544 0.046 Uiso 1 1 calc R . . C21 C 0.4269(6) 0.3431(4) 0.1386(3) 0.0513(16) Uani 1 1 d . . . H21A H 0.4697 0.3498 0.1878 0.077 Uiso 1 1 calc R . . H21B H 0.3787 0.4000 0.1212 0.077 Uiso 1 1 calc R . . H21C H 0.4991 0.3302 0.1133 0.077 Uiso 1 1 calc R . . C22 C 0.3963(6) 0.1744(4) 0.1586(3) 0.0514(16) Uani 1 1 d . . . H22A H 0.4681 0.1585 0.1340 0.077 Uiso 1 1 calc R . . H22B H 0.3282 0.1246 0.1536 0.077 Uiso 1 1 calc R . . H22C H 0.4390 0.1835 0.2076 0.077 Uiso 1 1 calc R . . C30 C 0.5462(5) 0.2922(4) -0.0656(3) 0.0378(13) Uani 1 1 d . . . H30 H 0.5760 0.2896 -0.1103 0.045 Uiso 1 1 calc R . . C31 C 0.5043(7) 0.3914(4) -0.0548(4) 0.0529(16) Uani 1 1 d . . . H31A H 0.4690 0.3952 -0.0127 0.079 Uiso 1 1 calc R . . H31B H 0.4318 0.4110 -0.0944 0.079 Uiso 1 1 calc R . . H31C H 0.5853 0.4316 -0.0503 0.079 Uiso 1 1 calc R . . C32 C 0.6690(6) 0.2626(4) -0.0086(4) 0.0556(17) Uani 1 1 d . . . H32A H 0.7433 0.3082 -0.0038 0.083 Uiso 1 1 calc R . . H32B H 0.7031 0.2030 -0.0204 0.083 Uiso 1 1 calc R . . H32C H 0.6394 0.2575 0.0350 0.083 Uiso 1 1 calc R . . C40 C 0.4660(6) 0.0986(4) -0.0799(3) 0.0442(15) Uani 1 1 d . . . H40 H 0.5395 0.0871 -0.0371 0.053 Uiso 1 1 calc R . . C41 C 0.3540(7) 0.0266(4) -0.0822(3) 0.0528(16) Uani 1 1 d . . . H41A H 0.2780 0.0373 -0.1226 0.079 Uiso 1 1 calc R . . H41B H 0.3184 0.0307 -0.0402 0.079 Uiso 1 1 calc R . . H41C H 0.3932 -0.0345 -0.0854 0.079 Uiso 1 1 calc R . . C42 C 0.5350(8) 0.0896(4) -0.1415(4) 0.064(2) Uani 1 1 d . . . H42A H 0.5750 0.0281 -0.1417 0.096 Uiso 1 1 calc R . . H42B H 0.6086 0.1356 -0.1375 0.096 Uiso 1 1 calc R . . H42C H 0.4654 0.0993 -0.1846 0.096 Uiso 1 1 calc R . . Li1 Li 0.0928(9) 0.3899(5) -0.1393(5) 0.036(2) Uani 1 1 d . . . N2 N -0.1129(14) 0.3904(7) -0.1994(6) 0.0376(14) Uiso 0.50 1 d PD A 1 N3 N 0.1265(10) 0.5182(9) -0.1773(6) 0.0367(14) Uiso 0.50 1 d PD A 1 C51 C -0.1109(12) 0.4731(7) -0.2433(6) 0.046(3) Uiso 0.50 1 d PD A 1 H51A H -0.2067 0.4964 -0.2598 0.056 Uiso 0.50 1 calc PR A 1 H51B H -0.0751 0.4560 -0.2841 0.056 Uiso 0.50 1 calc PR A 1 C52 C -0.0187(9) 0.5499(7) -0.2028(6) 0.040(3) Uiso 0.50 1 d PD A 1 H52A H -0.0198 0.6038 -0.2331 0.048 Uiso 0.50 1 calc PR A 1 H52B H -0.0570 0.5691 -0.1632 0.048 Uiso 0.50 1 calc PR A 1 C53 C -0.2133(15) 0.4131(10) -0.1553(7) 0.048(4) Uiso 0.50 1 d PD A 1 H53A H -0.3071 0.4185 -0.1845 0.072 Uiso 0.50 1 calc PR A 1 H53B H -0.1866 0.4713 -0.1314 0.072 Uiso 0.50 1 calc PR A 1 H53C H -0.2117 0.3642 -0.1213 0.072 Uiso 0.50 1 calc PR A 1 C54 C -0.1574(14) 0.3097(8) -0.2427(7) 0.051(3) Uiso 0.50 1 d PD A 1 H54A H -0.2488 0.3215 -0.2730 0.076 Uiso 0.50 1 calc PR A 1 H54B H -0.1631 0.2566 -0.2134 0.076 Uiso 0.50 1 calc PR A 1 H54C H -0.0901 0.2973 -0.2709 0.076 Uiso 0.50 1 calc PR A 1 C55 C 0.1963(14) 0.5117(9) -0.2358(7) 0.046(4) Uiso 0.50 1 d PD A 1 H55A H 0.2083 0.5734 -0.2531 0.069 Uiso 0.50 1 calc PR A 1 H55B H 0.1393 0.4748 -0.2728 0.069 Uiso 0.50 1 calc PR A 1 H55C H 0.2873 0.4826 -0.2200 0.069 Uiso 0.50 1 calc PR A 1 C56 C 0.2019(15) 0.5817(10) -0.1235(8) 0.044(2) Uiso 0.50 1 d PD A 1 H56A H 0.2098 0.6420 -0.1441 0.066 Uiso 0.50 1 calc PR A 1 H56B H 0.2949 0.5573 -0.1040 0.066 Uiso 0.50 1 calc PR A 1 H56C H 0.1510 0.5877 -0.0869 0.066 Uiso 0.50 1 calc PR A 1 N2A N -0.1174(14) 0.4069(7) -0.1958(6) 0.0376(14) Uiso 0.50 1 d PD A 2 N3A N 0.1337(11) 0.5129(9) -0.1890(6) 0.0367(14) Uiso 0.50 1 d PD A 2 C51A C -0.1171(13) 0.5064(7) -0.2107(7) 0.054(3) Uiso 0.50 1 d PD A 2 H51C H -0.2039 0.5225 -0.2445 0.065 Uiso 0.50 1 calc PR A 2 H51D H -0.1155 0.5411 -0.1678 0.065 Uiso 0.50 1 calc PR A 2 C52A C 0.0021(10) 0.5342(9) -0.2385(7) 0.057(3) Uiso 0.50 1 d PD A 2 H52C H -0.0029 0.6009 -0.2481 0.069 Uiso 0.50 1 calc PR A 2 H52D H -0.0010 0.5016 -0.2824 0.069 Uiso 0.50 1 calc PR A 2 C53A C -0.2178(13) 0.3832(10) -0.1533(6) 0.039(4) Uiso 0.50 1 d PD A 2 H53D H -0.3126 0.3900 -0.1811 0.058 Uiso 0.50 1 calc PR A 2 H53E H -0.2041 0.4243 -0.1134 0.058 Uiso 0.50 1 calc PR A 2 H53F H -0.2028 0.3196 -0.1374 0.058 Uiso 0.50 1 calc PR A 2 C54A C -0.1459(15) 0.3484(9) -0.2580(6) 0.054(4) Uiso 0.50 1 d PD A 2 H54D H -0.2362 0.3649 -0.2875 0.081 Uiso 0.50 1 calc PR A 2 H54E H -0.1473 0.2839 -0.2443 0.081 Uiso 0.50 1 calc PR A 2 H54F H -0.0732 0.3575 -0.2835 0.081 Uiso 0.50 1 calc PR A 2 C55A C 0.2494(14) 0.5132(9) -0.2260(7) 0.047(4) Uiso 0.50 1 d PD A 2 H55D H 0.2591 0.5748 -0.2440 0.070 Uiso 0.50 1 calc PR A 2 H55E H 0.2287 0.4693 -0.2643 0.070 Uiso 0.50 1 calc PR A 2 H55F H 0.3362 0.4957 -0.1939 0.070 Uiso 0.50 1 calc PR A 2 C56A C 0.1682(15) 0.5860(10) -0.1362(7) 0.044(2) Uiso 0.50 1 d PD A 2 H56D H 0.1742 0.6450 -0.1588 0.066 Uiso 0.50 1 calc PR A 2 H56E H 0.2575 0.5721 -0.1048 0.066 Uiso 0.50 1 calc PR A 2 H56F H 0.0957 0.5891 -0.1099 0.066 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0445(2) 0.0363(2) 0.0341(2) 0.00348(16) 0.01484(17) 0.01602(15) Te2 0.0460(2) 0.0371(2) 0.0290(2) -0.00147(15) 0.00716(17) 0.00663(15) P1 0.0309(7) 0.0289(7) 0.0267(8) 0.0011(5) 0.0112(6) 0.0053(5) P2 0.0323(8) 0.0296(7) 0.0266(8) -0.0013(6) 0.0102(6) 0.0046(5) N1 0.028(2) 0.031(2) 0.031(3) 0.0002(19) 0.010(2) 0.0069(17) C10 0.040(3) 0.033(3) 0.052(4) 0.005(3) 0.021(3) 0.001(2) C11 0.043(4) 0.049(3) 0.069(5) -0.004(3) 0.021(3) -0.013(3) C12 0.051(4) 0.062(4) 0.063(5) 0.011(3) 0.029(4) -0.009(3) C20 0.044(3) 0.044(3) 0.030(3) 0.004(2) 0.013(3) 0.010(2) C21 0.056(4) 0.064(4) 0.032(3) -0.007(3) 0.008(3) -0.001(3) C22 0.055(4) 0.060(4) 0.040(4) 0.014(3) 0.012(3) 0.025(3) C30 0.035(3) 0.046(3) 0.037(3) -0.003(3) 0.017(3) -0.003(2) C31 0.052(4) 0.042(3) 0.067(5) -0.005(3) 0.020(3) -0.008(3) C32 0.028(3) 0.073(4) 0.063(5) -0.011(3) 0.005(3) 0.007(3) C40 0.055(4) 0.049(3) 0.030(3) -0.001(3) 0.012(3) 0.022(3) C41 0.078(5) 0.030(3) 0.050(4) 0.000(3) 0.016(3) 0.007(3) C42 0.082(5) 0.054(4) 0.065(5) -0.005(3) 0.037(4) 0.030(3) Li1 0.038(5) 0.032(4) 0.038(5) 0.004(4) 0.010(4) 0.004(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 Te1 P1 2.4118(13) . ? Te1 Li1 2.775(9) . ? Te2 P2 2.3992(16) . ? Te2 Li1 2.727(8) . ? P1 N1 1.587(4) . ? P1 C20 1.836(6) . ? P1 C10 1.836(5) . ? P2 N1 1.598(4) . ? P2 C30 1.834(5) . ? P2 C40 1.848(5) . ? C10 C11 1.510(9) . ? C10 C12 1.533(7) . ? C20 C21 1.531(8) . ? C20 C22 1.545(7) . ? C30 C32 1.523(8) . ? C30 C31 1.533(7) . ? C40 C41 1.519(8) . ? C40 C42 1.540(8) . ? Li1 N3 2.072(16) . ? Li1 N2 2.113(17) . ? Li1 N3A 2.130(16) . ? Li1 N2A 2.142(17) . ? N2 C54 1.466(13) . ? N2 C51 1.493(9) . ? N2 C53 1.505(13) . ? N3 C56 1.482(13) . ? N3 C52 1.484(9) . ? N3 C55 1.486(13) . ? C51 C52 1.549(12) . ? N2A C54A 1.478(14) . ? N2A C51A 1.481(9) . ? N2A C53A 1.485(13) . ? N3A C52A 1.476(9) . ? N3A C56A 1.481(13) . ? N3A C55A 1.496(13) . ? C51A C52A 1.469(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Li1 101.91(17) . . ? P2 Te2 Li1 100.2(2) . . ? N1 P1 C20 105.9(2) . . ? N1 P1 C10 108.4(2) . . ? C20 P1 C10 105.1(3) . . ? N1 P1 Te1 120.82(16) . . ? C20 P1 Te1 106.70(16) . . ? C10 P1 Te1 108.78(18) . . ? N1 P2 C30 108.8(2) . . ? N1 P2 C40 104.7(2) . . ? C30 P2 C40 105.4(3) . . ? N1 P2 Te2 121.48(16) . . ? C30 P2 Te2 108.41(19) . . ? C40 P2 Te2 106.9(2) . . ? P1 N1 P2 143.5(3) . . ? C11 C10 C12 111.2(5) . . ? C11 C10 P1 111.6(4) . . ? C12 C10 P1 113.9(4) . . ? C21 C20 C22 110.0(5) . . ? C21 C20 P1 111.7(4) . . ? C22 C20 P1 111.3(4) . . ? C32 C30 C31 111.0(5) . . ? C32 C30 P2 111.8(4) . . ? C31 C30 P2 110.4(4) . . ? C41 C40 C42 111.7(5) . . ? C41 C40 P2 111.0(4) . . ? C42 C40 P2 112.4(4) . . ? N3 Li1 N2 90.3(5) . . ? N3 Li1 N3A 7.2(5) . . ? N2 Li1 N3A 89.7(5) . . ? N3 Li1 N2A 85.5(5) . . ? N2 Li1 N2A 6.9(5) . . ? N3A Li1 N2A 85.6(5) . . ? N3 Li1 Te2 116.7(5) . . ? N2 Li1 Te2 109.2(5) . . ? N3A Li1 Te2 110.2(4) . . ? N2A Li1 Te2 115.9(5) . . ? N3 Li1 Te1 113.4(5) . . ? N2 Li1 Te1 113.5(5) . . ? N3A Li1 Te1 120.0(5) . . ? N2A Li1 Te1 110.9(5) . . ? Te2 Li1 Te1 111.9(3) . . ? C54 N2 C51 110.2(10) . . ? C54 N2 C53 111.7(11) . . ? C51 N2 C53 105.2(10) . . ? C54 N2 Li1 116.9(9) . . ? C51 N2 Li1 101.2(8) . . ? C53 N2 Li1 110.5(9) . . ? C56 N3 C52 110.0(10) . . ? C56 N3 C55 111.0(11) . . ? C52 N3 C55 109.8(10) . . ? C56 N3 Li1 113.3(10) . . ? C52 N3 Li1 100.5(8) . . ? C55 N3 Li1 111.8(9) . . ? N2 C51 C52 111.3(10) . . ? N3 C52 C51 111.2(9) . . ? C54A N2A C51A 114.0(11) . . ? C54A N2A C53A 108.6(10) . . ? C51A N2A C53A 112.0(10) . . ? C54A N2A Li1 110.5(9) . . ? C51A N2A Li1 100.0(9) . . ? C53A N2A Li1 111.7(9) . . ? C52A N3A C56A 110.4(11) . . ? C52A N3A C55A 109.2(10) . . ? C56A N3A C55A 105.6(10) . . ? C52A N3A Li1 104.8(9) . . ? C56A N3A Li1 108.2(10) . . ? C55A N3A Li1 118.6(9) . . ? C52A C51A N2A 112.6(10) . . ? C51A C52A N3A 110.7(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 Te1 P1 N1 33.7(3) . . . . ? Li1 Te1 P1 C20 154.5(3) . . . . ? Li1 Te1 P1 C10 -92.6(3) . . . . ? Li1 Te2 P2 N1 42.6(2) . . . . ? Li1 Te2 P2 C30 -84.4(3) . . . . ? Li1 Te2 P2 C40 162.4(3) . . . . ? C20 P1 N1 P2 -151.1(4) . . . . ? C10 P1 N1 P2 96.5(5) . . . . ? Te1 P1 N1 P2 -29.9(5) . . . . ? C30 P2 N1 P1 107.4(5) . . . . ? C40 P2 N1 P1 -140.4(5) . . . . ? Te2 P2 N1 P1 -19.5(5) . . . . ? N1 P1 C10 C11 -71.5(4) . . . . ? C20 P1 C10 C11 175.6(4) . . . . ? Te1 P1 C10 C11 61.6(4) . . . . ? N1 P1 C10 C12 161.6(4) . . . . ? C20 P1 C10 C12 48.6(5) . . . . ? Te1 P1 C10 C12 -65.3(5) . . . . ? N1 P1 C20 C21 67.9(4) . . . . ? C10 P1 C20 C21 -177.5(4) . . . . ? Te1 P1 C20 C21 -62.1(4) . . . . ? N1 P1 C20 C22 -55.5(4) . . . . ? C10 P1 C20 C22 59.2(4) . . . . ? Te1 P1 C20 C22 174.5(3) . . . . ? N1 P2 C30 C32 59.3(4) . . . . ? C40 P2 C30 C32 -52.6(4) . . . . ? Te2 P2 C30 C32 -166.7(3) . . . . ? N1 P2 C30 C31 -64.8(5) . . . . ? C40 P2 C30 C31 -176.7(4) . . . . ? Te2 P2 C30 C31 69.2(4) . . . . ? N1 P2 C40 C41 62.4(5) . . . . ? C30 P2 C40 C41 177.1(4) . . . . ? Te2 P2 C40 C41 -67.7(4) . . . . ? N1 P2 C40 C42 -171.8(5) . . . . ? C30 P2 C40 C42 -57.0(5) . . . . ? Te2 P2 C40 C42 58.2(5) . . . . ? P2 Te2 Li1 N3 108.8(5) . . . . ? P2 Te2 Li1 N2 -150.7(4) . . . . ? P2 Te2 Li1 N3A 112.2(5) . . . . ? P2 Te2 Li1 N2A -152.7(4) . . . . ? P2 Te2 Li1 Te1 -24.1(3) . . . . ? P1 Te1 Li1 N3 -138.4(4) . . . . ? P1 Te1 Li1 N2 120.5(4) . . . . ? P1 Te1 Li1 N3A -135.4(5) . . . . ? P1 Te1 Li1 N2A 127.4(4) . . . . ? P1 Te1 Li1 Te2 -3.8(3) . . . . ? N3 Li1 N2 C54 128.7(9) . . . . ? N3A Li1 N2 C54 121.6(9) . . . . ? N2A Li1 N2 C54 175(5) . . . . ? Te2 Li1 N2 C54 10.2(10) . . . . ? Te1 Li1 N2 C54 -115.5(9) . . . . ? N3 Li1 N2 C51 9.0(8) . . . . ? N3A Li1 N2 C51 1.9(8) . . . . ? N2A Li1 N2 C51 55(4) . . . . ? Te2 Li1 N2 C51 -109.5(7) . . . . ? Te1 Li1 N2 C51 124.8(7) . . . . ? N3 Li1 N2 C53 -102.0(9) . . . . ? N3A Li1 N2 C53 -109.2(9) . . . . ? N2A Li1 N2 C53 -56(4) . . . . ? Te2 Li1 N2 C53 139.4(8) . . . . ? Te1 Li1 N2 C53 13.7(9) . . . . ? N2 Li1 N3 C56 136.6(9) . . . . ? N3A Li1 N3 C56 -138(4) . . . . ? N2A Li1 N3 C56 131.6(9) . . . . ? Te2 Li1 N3 C56 -111.6(9) . . . . ? Te1 Li1 N3 C56 20.7(10) . . . . ? N2 Li1 N3 C52 19.3(8) . . . . ? N3A Li1 N3 C52 105(4) . . . . ? N2A Li1 N3 C52 14.3(8) . . . . ? Te2 Li1 N3 C52 131.1(7) . . . . ? Te1 Li1 N3 C52 -96.6(8) . . . . ? N2 Li1 N3 C55 -97.1(9) . . . . ? N3A Li1 N3 C55 -12(4) . . . . ? N2A Li1 N3 C55 -102.1(9) . . . . ? Te2 Li1 N3 C55 14.7(10) . . . . ? Te1 Li1 N3 C55 147.0(8) . . . . ? C54 N2 C51 C52 -160.3(10) . . . . ? C53 N2 C51 C52 79.2(13) . . . . ? Li1 N2 C51 C52 -35.9(11) . . . . ? C56 N3 C52 C51 -164.4(11) . . . . ? C55 N3 C52 C51 73.3(13) . . . . ? Li1 N3 C52 C51 -44.6(11) . . . . ? N2 C51 C52 N3 59.3(14) . . . . ? N3 Li1 N2A C54A 106.1(9) . . . . ? N2 Li1 N2A C54A -27(4) . . . . ? N3A Li1 N2A C54A 98.9(9) . . . . ? Te2 Li1 N2A C54A -11.5(9) . . . . ? Te1 Li1 N2A C54A -140.6(8) . . . . ? N3 Li1 N2A C51A -14.3(8) . . . . ? N2 Li1 N2A C51A -148(5) . . . . ? N3A Li1 N2A C51A -21.5(8) . . . . ? Te2 Li1 N2A C51A -131.9(7) . . . . ? Te1 Li1 N2A C51A 99.0(8) . . . . ? N3 Li1 N2A C53A -132.9(8) . . . . ? N2 Li1 N2A C53A 93(4) . . . . ? N3A Li1 N2A C53A -140.2(8) . . . . ? Te2 Li1 N2A C53A 109.4(8) . . . . ? Te1 Li1 N2A C53A -19.6(9) . . . . ? N3 Li1 N3A C52A -95(4) . . . . ? N2 Li1 N3A C52A -0.3(9) . . . . ? N2A Li1 N3A C52A -5.9(9) . . . . ? Te2 Li1 N3A C52A 110.1(8) . . . . ? Te1 Li1 N3A C52A -117.6(8) . . . . ? N3 Li1 N3A C56A 23(4) . . . . ? N2 Li1 N3A C56A 117.4(8) . . . . ? N2A Li1 N3A C56A 111.9(8) . . . . ? Te2 Li1 N3A C56A -132.1(8) . . . . ? Te1 Li1 N3A C56A 0.2(10) . . . . ? N3 Li1 N3A C55A 143(4) . . . . ? N2 Li1 N3A C55A -122.4(9) . . . . ? N2A Li1 N3A C55A -128.0(9) . . . . ? Te2 Li1 N3A C55A -12.0(10) . . . . ? Te1 Li1 N3A C55A 120.3(9) . . . . ? C54A N2A C51A C52A -69.5(16) . . . . ? C53A N2A C51A C52A 166.7(12) . . . . ? Li1 N2A C51A C52A 48.4(13) . . . . ? N2A C51A C52A N3A -59.8(16) . . . . ? C56A N3A C52A C51A -82.4(15) . . . . ? C55A N3A C52A C51A 162.0(11) . . . . ? Li1 N3A C52A C51A 33.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.770 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.147 #===END data_8Li _database_code_depnum_ccdc_archive 'CCDC 666809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H44 Li N3 P2 Se1.10 Te0.90' _chemical_formula_sum 'C18 H44 Li N3 P2 Se1.10 Te0.90' _chemical_formula_weight 573.14 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' Li Li -0.0003 0.0001 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9363(3) _cell_length_b 14.4509(3) _cell_length_c 19.5906(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.451(1) _cell_angle_gamma 90.00 _cell_volume 2723.99(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25589 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1161 _exptl_absorpt_coefficient_mu 2.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The coordinated TMEDA molecule was disordered over two sites and was modeled as an isotropic 50:50 mixture with mild geometric restraints. The overall crystal structure is comprised of the two complexes C18H44LiN3P2SeTe (90%) and C18H44LiN3P2Se2 (10%) which are co-crystallized. Furthermore, there is some positional disorder of the tellurium and selenium sites, which was modeled as an 80:20 anisotropic mixture; the P-Se and P-Te bond distances of the minor disorder component were restrained to correlate with the major component distances. ; _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 40390 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4803 _reflns_number_gt 3617 _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^)+(0.0208P)^2^+4.5261P] 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 4803 _refine_ls_number_parameters 248 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.069 _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 Te1 Te 0.6069(3) 0.89415(13) -0.00612(15) 0.0305(2) Uani 0.70 1 d P A 1 Se1 Se 0.8969(6) 0.7466(4) 0.16829(15) 0.0310(3) Uani 0.80 1 d P A 1 Se1A Se 0.6164(12) 0.8787(5) -0.0034(6) 0.0305(2) Uani 0.30 1 d PD A 2 Te1A Te 0.9015(17) 0.7472(12) 0.1799(5) 0.0310(3) Uani 0.20 1 d PD A 2 P1 P 0.69490(11) 0.75178(7) -0.04113(5) 0.0245(2) Uani 1 1 d D . . P2 P 0.95728(11) 0.71464(7) 0.07159(6) 0.0246(3) Uani 1 1 d D . . N1 N 0.8459(3) 0.7153(2) -0.00227(17) 0.0259(8) Uani 1 1 d . A . C10 C 0.6962(5) 0.7671(3) -0.1341(2) 0.0336(11) Uani 1 1 d . A . H10A H 0.5999 0.7844 -0.1608 0.040 Uiso 1 1 calc R . . C11 C 0.7932(5) 0.8446(4) -0.1436(2) 0.0499(13) Uani 1 1 d . . . H11A H 0.7849 0.8544 -0.1940 0.075 Uiso 1 1 calc R A . H11B H 0.8892 0.8277 -0.1202 0.075 Uiso 1 1 calc R . . H11C H 0.7682 0.9017 -0.1227 0.075 Uiso 1 1 calc R . . C12 C 0.7350(5) 0.6757(3) -0.1657(2) 0.0439(13) Uani 1 1 d . . . H12A H 0.7258 0.6837 -0.2163 0.066 Uiso 1 1 calc R A . H12B H 0.6727 0.6263 -0.1582 0.066 Uiso 1 1 calc R . . H12C H 0.8312 0.6593 -0.1424 0.066 Uiso 1 1 calc R . . C20 C 0.5696(4) 0.6583(3) -0.0406(2) 0.0350(11) Uani 1 1 d . A . H20A H 0.6108 0.6003 -0.0546 0.042 Uiso 1 1 calc R . . C21 C 0.4290(5) 0.6723(4) -0.0937(3) 0.0486(13) Uani 1 1 d . . . H21A H 0.3664 0.6214 -0.0894 0.073 Uiso 1 1 calc R A . H21B H 0.4423 0.6733 -0.1416 0.073 Uiso 1 1 calc R . . H21C H 0.3883 0.7312 -0.0841 0.073 Uiso 1 1 calc R . . C22 C 0.5503(5) 0.6424(3) 0.0336(2) 0.0439(12) Uani 1 1 d . . . H22A H 0.4970 0.5855 0.0342 0.066 Uiso 1 1 calc R A . H22B H 0.5000 0.6949 0.0471 0.066 Uiso 1 1 calc R . . H22C H 0.6414 0.6367 0.0671 0.066 Uiso 1 1 calc R . . C30 C 1.0295(5) 0.5973(3) 0.0814(2) 0.0355(11) Uani 1 1 d . A . H30A H 1.0639 0.5846 0.0385 0.043 Uiso 1 1 calc R . . C31 C 0.9154(5) 0.5261(3) 0.0819(2) 0.0446(13) Uani 1 1 d . . . H31A H 0.9555 0.4637 0.0864 0.067 Uiso 1 1 calc R A . H31B H 0.8428 0.5305 0.0378 0.067 Uiso 1 1 calc R . . H31C H 0.8751 0.5384 0.1218 0.067 Uiso 1 1 calc R . . C32 C 1.1547(5) 0.5871(4) 0.1452(3) 0.0565(15) Uani 1 1 d . . . H32A H 1.1886 0.5232 0.1480 0.085 Uiso 1 1 calc R A . H32B H 1.1265 0.6025 0.1884 0.085 Uiso 1 1 calc R . . H32C H 1.2288 0.6292 0.1400 0.085 Uiso 1 1 calc R . . C40 C 1.1015(4) 0.7902(3) 0.0656(2) 0.0325(10) Uani 1 1 d . A . H40A H 1.1728 0.7869 0.1117 0.039 Uiso 1 1 calc R . . C41 C 1.0537(5) 0.8905(3) 0.0539(3) 0.0426(12) Uani 1 1 d . . . H41A H 1.1333 0.9299 0.0527 0.064 Uiso 1 1 calc R A . H41B H 1.0137 0.9104 0.0924 0.064 Uiso 1 1 calc R . . H41C H 0.9834 0.8957 0.0090 0.064 Uiso 1 1 calc R . . C42 C 1.1704(5) 0.7578(4) 0.0080(3) 0.0472(13) Uani 1 1 d . . . H42A H 1.2419 0.8024 0.0035 0.071 Uiso 1 1 calc R A . H42B H 1.1001 0.7532 -0.0369 0.071 Uiso 1 1 calc R . . H42C H 1.2132 0.6971 0.0206 0.071 Uiso 1 1 calc R . . Li1 Li 0.7271(7) 0.8845(5) 0.1348(4) 0.0333(17) Uani 1 1 d D . . C51 C 0.6232(10) 0.9595(6) 0.2426(5) 0.037(2) Uiso 0.50 1 d PD A 1 H51A H 0.7000 0.9401 0.2828 0.045 Uiso 0.50 1 calc PR A 1 H51B H 0.5450 0.9804 0.2617 0.045 Uiso 0.50 1 calc PR A 1 C52 C 0.6721(9) 1.0397(6) 0.2042(5) 0.037(2) Uiso 0.50 1 d PD A 1 H52A H 0.5953 1.0591 0.1640 0.044 Uiso 0.50 1 calc PR A 1 H52B H 0.6964 1.0929 0.2368 0.044 Uiso 0.50 1 calc PR A 1 N2 N 0.5776(9) 0.8789(6) 0.1951(5) 0.0318(11) Uiso 0.50 1 d PD A 1 N3 N 0.7944(10) 1.0139(6) 0.1779(5) 0.031(4) Uiso 0.50 1 d PD A 1 C53 C 0.4348(11) 0.8989(9) 0.1505(6) 0.037(4) Uiso 0.50 1 d PD A 1 H53A H 0.3702 0.9053 0.1807 0.056 Uiso 0.50 1 calc PR A 1 H53B H 0.4044 0.8480 0.1172 0.056 Uiso 0.50 1 calc PR A 1 H53C H 0.4364 0.9566 0.1244 0.056 Uiso 0.50 1 calc PR A 1 C54 C 0.5788(12) 0.7934(7) 0.2366(6) 0.048(3) Uiso 0.50 1 d PD A 1 H54A H 0.5180 0.8013 0.2686 0.072 Uiso 0.50 1 calc PR A 1 H54B H 0.6737 0.7806 0.2640 0.072 Uiso 0.50 1 calc PR A 1 H54C H 0.5453 0.7416 0.2046 0.072 Uiso 0.50 1 calc PR A 1 C55 C 0.8173(16) 1.0800(10) 0.1237(7) 0.046(4) Uiso 0.50 1 d PD A 1 H55A H 0.8405 1.1411 0.1452 0.069 Uiso 0.50 1 calc PR A 1 H55B H 0.7326 1.0845 0.0854 0.069 Uiso 0.50 1 calc PR A 1 H55C H 0.8940 1.0580 0.1048 0.069 Uiso 0.50 1 calc PR A 1 C56 C 0.9208(12) 1.0057(8) 0.2347(6) 0.046(3) Uiso 0.50 1 d PD A 1 H56A H 0.9415 1.0654 0.2587 0.069 Uiso 0.50 1 calc PR A 1 H56B H 0.9984 0.9875 0.2150 0.069 Uiso 0.50 1 calc PR A 1 H56C H 0.9072 0.9587 0.2684 0.069 Uiso 0.50 1 calc PR A 1 C51A C 0.5867(9) 0.9974(6) 0.2108(5) 0.041(2) Uiso 0.50 1 d PD A 2 H51C H 0.5336 1.0104 0.2463 0.049 Uiso 0.50 1 calc PR A 2 H51D H 0.5454 1.0344 0.1681 0.049 Uiso 0.50 1 calc PR A 2 C52A C 0.7334(9) 1.0252(7) 0.2391(5) 0.041(2) Uiso 0.50 1 d PD A 2 H52C H 0.7374 1.0920 0.2505 0.049 Uiso 0.50 1 calc PR A 2 H52D H 0.7727 0.9908 0.2833 0.049 Uiso 0.50 1 calc PR A 2 N2A N 0.5756(9) 0.8982(5) 0.1927(5) 0.0318(11) Uiso 0.50 1 d PD A 2 N3A N 0.8185(10) 1.0068(6) 0.1887(5) 0.035(4) Uiso 0.50 1 d PD A 2 C53A C 0.4350(12) 0.8723(9) 0.1531(6) 0.042(4) Uiso 0.50 1 d PD A 2 H53D H 0.3694 0.8837 0.1822 0.063 Uiso 0.50 1 calc PR A 2 H53E H 0.4333 0.8065 0.1408 0.063 Uiso 0.50 1 calc PR A 2 H53F H 0.4084 0.9094 0.1100 0.063 Uiso 0.50 1 calc PR A 2 C54A C 0.6094(11) 0.8363(7) 0.2553(5) 0.047(3) Uiso 0.50 1 d PD A 2 H54D H 0.5439 0.8476 0.2844 0.070 Uiso 0.50 1 calc PR A 2 H54E H 0.7043 0.8489 0.2830 0.070 Uiso 0.50 1 calc PR A 2 H54F H 0.6024 0.7716 0.2397 0.070 Uiso 0.50 1 calc PR A 2 C55A C 0.7989(14) 1.0821(8) 0.1364(6) 0.031(4) Uiso 0.50 1 d PD A 2 H55D H 0.8325 1.1403 0.1603 0.047 Uiso 0.50 1 calc PR A 2 H55E H 0.6999 1.0879 0.1129 0.047 Uiso 0.50 1 calc PR A 2 H55F H 0.8511 1.0681 0.1014 0.047 Uiso 0.50 1 calc PR A 2 C56A C 0.9672(11) 1.0061(8) 0.2276(6) 0.046(3) Uiso 0.50 1 d PD A 2 H56D H 0.9897 1.0640 0.2541 0.069 Uiso 0.50 1 calc PR A 2 H56E H 1.0252 1.0003 0.1941 0.069 Uiso 0.50 1 calc PR A 2 H56F H 0.9848 0.9537 0.2604 0.069 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0348(5) 0.0283(8) 0.0255(3) -0.0034(6) 0.0021(3) 0.0142(5) Se1 0.0416(5) 0.0323(2) 0.0223(11) 0.0009(11) 0.0142(11) 0.0071(3) Se1A 0.0348(5) 0.0283(8) 0.0255(3) -0.0034(6) 0.0021(3) 0.0142(5) Te1A 0.0416(5) 0.0323(2) 0.0223(11) 0.0009(11) 0.0142(11) 0.0071(3) P1 0.0221(6) 0.0288(6) 0.0213(6) -0.0013(5) 0.0030(5) 0.0028(5) P2 0.0244(6) 0.0262(6) 0.0225(6) 0.0017(5) 0.0047(5) 0.0055(5) N1 0.024(2) 0.032(2) 0.0219(19) 0.0007(15) 0.0059(15) 0.0050(15) C10 0.029(3) 0.044(3) 0.023(2) 0.000(2) -0.0014(19) 0.008(2) C11 0.059(4) 0.060(3) 0.030(3) 0.014(3) 0.011(2) -0.002(3) C12 0.043(3) 0.061(3) 0.029(3) -0.007(2) 0.010(2) 0.009(2) C20 0.030(3) 0.036(3) 0.039(3) -0.009(2) 0.007(2) -0.006(2) C21 0.028(3) 0.061(3) 0.053(3) -0.012(3) 0.004(2) -0.012(2) C22 0.038(3) 0.046(3) 0.052(3) 0.003(2) 0.020(2) -0.008(2) C30 0.038(3) 0.033(3) 0.034(3) 0.003(2) 0.006(2) 0.016(2) C31 0.066(4) 0.028(3) 0.037(3) 0.003(2) 0.008(2) 0.009(2) C32 0.054(4) 0.048(3) 0.056(3) 0.011(3) -0.008(3) 0.024(3) C40 0.024(2) 0.039(3) 0.033(3) 0.004(2) 0.004(2) 0.003(2) C41 0.043(3) 0.034(3) 0.052(3) -0.001(2) 0.015(2) -0.010(2) C42 0.034(3) 0.064(3) 0.048(3) 0.006(3) 0.019(2) 0.005(3) Li1 0.035(4) 0.041(4) 0.025(4) 0.005(3) 0.011(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 P1 2.4016(19) . ? Te1 Li1 2.724(7) . ? Se1 P2 2.174(3) . ? Se1 Li1 2.589(9) . ? Se1A P1 2.193(6) . ? Se1A Li1 2.656(13) . ? Te1A P2 2.370(7) . ? Te1A Li1 2.638(18) . ? P1 N1 1.593(3) . ? P1 C10 1.838(4) . ? P1 C20 1.839(4) . ? P2 N1 1.588(3) . ? P2 C40 1.828(4) . ? P2 C30 1.832(4) . ? C10 C11 1.519(6) . ? C10 C12 1.548(6) . ? C20 C22 1.531(6) . ? C20 C21 1.533(6) . ? C30 C31 1.533(6) . ? C30 C32 1.535(6) . ? C40 C41 1.526(6) . ? C40 C42 1.532(6) . ? Li1 N3 2.091(10) . ? Li1 N2A 2.109(10) . ? Li1 N2 2.118(10) . ? Li1 N3A 2.140(11) . ? C51 N2 1.488(8) . ? C51 C52 1.525(11) . ? C52 N3 1.482(8) . ? N2 C54 1.477(11) . ? N2 C53 1.497(12) . ? N3 C56 1.460(12) . ? N3 C55 1.487(12) . ? C51A N2A 1.475(8) . ? C51A C52A 1.480(11) . ? C52A N3A 1.475(8) . ? N2A C53A 1.467(12) . ? N2A C54A 1.486(12) . ? N3A C55A 1.474(12) . ? N3A C56A 1.484(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Li1 98.44(17) . . ? P2 Se1 Li1 104.3(2) . . ? P1 Se1A Li1 106.2(4) . . ? P2 Te1A Li1 97.5(5) . . ? N1 P1 C10 105.97(19) . . ? N1 P1 C20 108.21(19) . . ? C10 P1 C20 105.4(2) . . ? N1 P1 Se1A 119.2(3) . . ? C10 P1 Se1A 108.9(3) . . ? C20 P1 Se1A 108.3(4) . . ? N1 P1 Te1 120.89(15) . . ? C10 P1 Te1 105.81(16) . . ? C20 P1 Te1 109.43(17) . . ? N1 P2 C40 108.51(19) . . ? N1 P2 C30 105.49(19) . . ? C40 P2 C30 105.4(2) . . ? N1 P2 Se1 120.8(2) . . ? C40 P2 Se1 108.7(2) . . ? C30 P2 Se1 106.9(2) . . ? N1 P2 Te1A 123.3(4) . . ? C40 P2 Te1A 107.5(5) . . ? C30 P2 Te1A 105.2(4) . . ? P2 N1 P1 142.9(2) . . ? C11 C10 C12 110.5(4) . . ? C11 C10 P1 111.8(3) . . ? C12 C10 P1 110.9(3) . . ? C22 C20 C21 110.8(4) . . ? C22 C20 P1 111.2(3) . . ? C21 C20 P1 113.8(3) . . ? C31 C30 C32 112.4(4) . . ? C31 C30 P2 110.6(3) . . ? C32 C30 P2 113.0(3) . . ? C41 C40 C42 111.0(4) . . ? C41 C40 P2 110.9(3) . . ? C42 C40 P2 111.5(3) . . ? N3 Li1 N2 90.4(4) . . ? N2A Li1 N3A 85.9(4) . . ? N3 Li1 Se1 117.6(4) . . ? N2A Li1 Se1 116.3(4) . . ? N2 Li1 Se1 109.4(4) . . ? N3A Li1 Se1 109.9(4) . . ? N3 Li1 Te1A 114.8(5) . . ? N2A Li1 Te1A 112.8(4) . . ? N2 Li1 Te1A 106.1(4) . . ? N3A Li1 Te1A 107.1(5) . . ? N3 Li1 Se1A 116.7(4) . . ? N2A Li1 Se1A 112.4(5) . . ? N2 Li1 Se1A 113.4(5) . . ? N3A Li1 Se1A 123.1(5) . . ? Te1A Li1 Se1A 112.8(3) . . ? N3 Li1 Te1 112.3(4) . . ? N2A Li1 Te1 110.5(4) . . ? N2 Li1 Te1 112.1(4) . . ? N3A Li1 Te1 118.9(4) . . ? Se1 Li1 Te1 112.9(3) . . ? N2 C51 C52 111.8(7) . . ? N3 C52 C51 111.7(7) . . ? C54 N2 C51 110.6(8) . . ? C54 N2 C53 111.0(8) . . ? C51 N2 C53 108.1(8) . . ? C54 N2 Li1 115.4(7) . . ? C51 N2 Li1 99.9(6) . . ? C53 N2 Li1 111.1(7) . . ? C56 N3 C52 112.3(8) . . ? C56 N3 C55 109.9(9) . . ? C52 N3 C55 111.8(9) . . ? C56 N3 Li1 111.3(7) . . ? C52 N3 Li1 99.1(6) . . ? C55 N3 Li1 112.1(8) . . ? N2A C51A C52A 111.2(8) . . ? N3A C52A C51A 112.0(8) . . ? C53A N2A C51A 112.2(8) . . ? C53A N2A C54A 105.8(8) . . ? C51A N2A C54A 113.6(8) . . ? C53A N2A Li1 113.9(7) . . ? C51A N2A Li1 101.5(6) . . ? C54A N2A Li1 110.1(7) . . ? C55A N3A C52A 109.5(9) . . ? C55A N3A C56A 107.7(9) . . ? C52A N3A C56A 108.7(9) . . ? C55A N3A Li1 107.5(8) . . ? C52A N3A Li1 103.7(6) . . ? C56A N3A Li1 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.488 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.162 #===END #===END data_7Li _database_code_depnum_ccdc_archive 'CCDC 666810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H44 Li N3 P2 Te2' _chemical_formula_sum 'C18 H44 Li N3 P2 Te2' _chemical_formula_weight 626.64 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.895(5) _cell_length_b 14.5762(4) _cell_length_c 19.910(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.171(2) _cell_angle_gamma 90.00 _cell_volume 2796.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14792 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The structure was well-ordered with the exception of the coordinated TMEDA molecule, which was disordered over two sites. The disorder was modeled as an isotropic 50:50 mixture with mild geometric restraints. ; _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_reflns_number 16994 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4921 _reflns_number_gt 3765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius DENZO' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0503P)^2^+1.9871P] 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 4921 _refine_ls_number_parameters 240 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.048 _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 Te1 Te 0.10916(4) 0.38904(2) 0.001714(19) 0.03737(14) Uani 1 1 d . A . Te2 Te 0.23400(4) 0.24666(2) -0.178872(18) 0.03761(13) Uani 1 1 d . A . P1 P 0.23568(14) 0.24920(8) 0.03712(7) 0.0281(3) Uani 1 1 d . . . P2 P 0.39729(14) 0.21514(8) -0.07238(7) 0.0290(3) Uani 1 1 d . . . N1 N 0.3517(4) 0.2148(3) -0.0004(2) 0.0295(9) Uani 1 1 d . . . C10 C 0.1111(6) 0.1556(3) 0.0361(3) 0.0394(14) Uani 1 1 d . . . H10 H 0.1669 0.0985 0.0490 0.047 Uiso 1 1 calc R . . C11 C 0.0223(6) 0.1400(4) -0.0354(3) 0.0525(16) Uani 1 1 d . . . H11A H -0.0328 0.0841 -0.0356 0.079 Uiso 1 1 calc R . . H11B H 0.0820 0.1332 -0.0682 0.079 Uiso 1 1 calc R . . H11C H -0.0400 0.1924 -0.0488 0.079 Uiso 1 1 calc R . . C12 C 0.0217(6) 0.1669(4) 0.0891(3) 0.0560(17) Uani 1 1 d . . . H12A H -0.0274 0.2257 0.0817 0.084 Uiso 1 1 calc R . . H12B H 0.0813 0.1654 0.1358 0.084 Uiso 1 1 calc R . . H12C H -0.0459 0.1168 0.0839 0.084 Uiso 1 1 calc R . . C20 C 0.3229(6) 0.2637(3) 0.1283(3) 0.0385(13) Uani 1 1 d . . . H20 H 0.2504 0.2785 0.1544 0.046 Uiso 1 1 calc R . . C21 C 0.4269(6) 0.3431(4) 0.1386(3) 0.0513(16) Uani 1 1 d . . . H21A H 0.4697 0.3498 0.1878 0.077 Uiso 1 1 calc R . . H21B H 0.3787 0.4000 0.1212 0.077 Uiso 1 1 calc R . . H21C H 0.4991 0.3302 0.1133 0.077 Uiso 1 1 calc R . . C22 C 0.3963(6) 0.1744(4) 0.1586(3) 0.0514(16) Uani 1 1 d . . . H22A H 0.4681 0.1585 0.1340 0.077 Uiso 1 1 calc R . . H22B H 0.3282 0.1246 0.1536 0.077 Uiso 1 1 calc R . . H22C H 0.4390 0.1835 0.2076 0.077 Uiso 1 1 calc R . . C30 C 0.5462(5) 0.2922(4) -0.0656(3) 0.0378(13) Uani 1 1 d . . . H30 H 0.5760 0.2896 -0.1103 0.045 Uiso 1 1 calc R . . C31 C 0.5043(7) 0.3914(4) -0.0548(4) 0.0529(16) Uani 1 1 d . . . H31A H 0.4690 0.3952 -0.0127 0.079 Uiso 1 1 calc R . . H31B H 0.4318 0.4110 -0.0944 0.079 Uiso 1 1 calc R . . H31C H 0.5853 0.4316 -0.0503 0.079 Uiso 1 1 calc R . . C32 C 0.6690(6) 0.2626(4) -0.0086(4) 0.0556(17) Uani 1 1 d . . . H32A H 0.7433 0.3082 -0.0038 0.083 Uiso 1 1 calc R . . H32B H 0.7031 0.2030 -0.0204 0.083 Uiso 1 1 calc R . . H32C H 0.6394 0.2575 0.0350 0.083 Uiso 1 1 calc R . . C40 C 0.4660(6) 0.0986(4) -0.0799(3) 0.0442(15) Uani 1 1 d . . . H40 H 0.5395 0.0871 -0.0371 0.053 Uiso 1 1 calc R . . C41 C 0.3540(7) 0.0266(4) -0.0822(3) 0.0528(16) Uani 1 1 d . . . H41A H 0.2780 0.0373 -0.1226 0.079 Uiso 1 1 calc R . . H41B H 0.3184 0.0307 -0.0402 0.079 Uiso 1 1 calc R . . H41C H 0.3932 -0.0345 -0.0854 0.079 Uiso 1 1 calc R . . C42 C 0.5350(8) 0.0896(4) -0.1415(4) 0.064(2) Uani 1 1 d . . . H42A H 0.5750 0.0281 -0.1417 0.096 Uiso 1 1 calc R . . H42B H 0.6086 0.1356 -0.1375 0.096 Uiso 1 1 calc R . . H42C H 0.4654 0.0993 -0.1846 0.096 Uiso 1 1 calc R . . Li1 Li 0.0928(9) 0.3899(5) -0.1393(5) 0.036(2) Uani 1 1 d . . . N2 N -0.1129(14) 0.3904(7) -0.1994(6) 0.0376(14) Uiso 0.50 1 d PD A 1 N3 N 0.1265(10) 0.5182(9) -0.1773(6) 0.0367(14) Uiso 0.50 1 d PD A 1 C51 C -0.1109(12) 0.4731(7) -0.2433(6) 0.046(3) Uiso 0.50 1 d PD A 1 H51A H -0.2067 0.4964 -0.2598 0.056 Uiso 0.50 1 calc PR A 1 H51B H -0.0751 0.4560 -0.2841 0.056 Uiso 0.50 1 calc PR A 1 C52 C -0.0187(9) 0.5499(7) -0.2028(6) 0.040(3) Uiso 0.50 1 d PD A 1 H52A H -0.0198 0.6038 -0.2331 0.048 Uiso 0.50 1 calc PR A 1 H52B H -0.0570 0.5691 -0.1632 0.048 Uiso 0.50 1 calc PR A 1 C53 C -0.2133(15) 0.4131(10) -0.1553(7) 0.048(4) Uiso 0.50 1 d PD A 1 H53A H -0.3071 0.4185 -0.1845 0.072 Uiso 0.50 1 calc PR A 1 H53B H -0.1866 0.4713 -0.1314 0.072 Uiso 0.50 1 calc PR A 1 H53C H -0.2117 0.3642 -0.1213 0.072 Uiso 0.50 1 calc PR A 1 C54 C -0.1574(14) 0.3097(8) -0.2427(7) 0.051(3) Uiso 0.50 1 d PD A 1 H54A H -0.2488 0.3215 -0.2730 0.076 Uiso 0.50 1 calc PR A 1 H54B H -0.1631 0.2566 -0.2134 0.076 Uiso 0.50 1 calc PR A 1 H54C H -0.0901 0.2973 -0.2709 0.076 Uiso 0.50 1 calc PR A 1 C55 C 0.1963(14) 0.5117(9) -0.2358(7) 0.046(4) Uiso 0.50 1 d PD A 1 H55A H 0.2083 0.5734 -0.2531 0.069 Uiso 0.50 1 calc PR A 1 H55B H 0.1393 0.4748 -0.2728 0.069 Uiso 0.50 1 calc PR A 1 H55C H 0.2873 0.4826 -0.2200 0.069 Uiso 0.50 1 calc PR A 1 C56 C 0.2019(15) 0.5817(10) -0.1235(8) 0.044(2) Uiso 0.50 1 d PD A 1 H56A H 0.2098 0.6420 -0.1441 0.066 Uiso 0.50 1 calc PR A 1 H56B H 0.2949 0.5573 -0.1040 0.066 Uiso 0.50 1 calc PR A 1 H56C H 0.1510 0.5877 -0.0869 0.066 Uiso 0.50 1 calc PR A 1 N2A N -0.1174(14) 0.4069(7) -0.1958(6) 0.0376(14) Uiso 0.50 1 d PD A 2 N3A N 0.1337(11) 0.5129(9) -0.1890(6) 0.0367(14) Uiso 0.50 1 d PD A 2 C51A C -0.1171(13) 0.5064(7) -0.2107(7) 0.054(3) Uiso 0.50 1 d PD A 2 H51C H -0.2039 0.5225 -0.2445 0.065 Uiso 0.50 1 calc PR A 2 H51D H -0.1155 0.5411 -0.1678 0.065 Uiso 0.50 1 calc PR A 2 C52A C 0.0021(10) 0.5342(9) -0.2385(7) 0.057(3) Uiso 0.50 1 d PD A 2 H52C H -0.0029 0.6009 -0.2481 0.069 Uiso 0.50 1 calc PR A 2 H52D H -0.0010 0.5016 -0.2824 0.069 Uiso 0.50 1 calc PR A 2 C53A C -0.2178(13) 0.3832(10) -0.1533(6) 0.039(4) Uiso 0.50 1 d PD A 2 H53D H -0.3126 0.3900 -0.1811 0.058 Uiso 0.50 1 calc PR A 2 H53E H -0.2041 0.4243 -0.1134 0.058 Uiso 0.50 1 calc PR A 2 H53F H -0.2028 0.3196 -0.1374 0.058 Uiso 0.50 1 calc PR A 2 C54A C -0.1459(15) 0.3484(9) -0.2580(6) 0.054(4) Uiso 0.50 1 d PD A 2 H54D H -0.2362 0.3649 -0.2875 0.081 Uiso 0.50 1 calc PR A 2 H54E H -0.1473 0.2839 -0.2443 0.081 Uiso 0.50 1 calc PR A 2 H54F H -0.0732 0.3575 -0.2835 0.081 Uiso 0.50 1 calc PR A 2 C55A C 0.2494(14) 0.5132(9) -0.2260(7) 0.047(4) Uiso 0.50 1 d PD A 2 H55D H 0.2591 0.5748 -0.2440 0.070 Uiso 0.50 1 calc PR A 2 H55E H 0.2287 0.4693 -0.2643 0.070 Uiso 0.50 1 calc PR A 2 H55F H 0.3362 0.4957 -0.1939 0.070 Uiso 0.50 1 calc PR A 2 C56A C 0.1682(15) 0.5860(10) -0.1362(7) 0.044(2) Uiso 0.50 1 d PD A 2 H56D H 0.1742 0.6450 -0.1588 0.066 Uiso 0.50 1 calc PR A 2 H56E H 0.2575 0.5721 -0.1048 0.066 Uiso 0.50 1 calc PR A 2 H56F H 0.0957 0.5891 -0.1099 0.066 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0445(2) 0.0363(2) 0.0341(2) 0.00348(16) 0.01484(17) 0.01602(15) Te2 0.0460(2) 0.0371(2) 0.0290(2) -0.00147(15) 0.00716(17) 0.00663(15) P1 0.0309(7) 0.0289(7) 0.0267(8) 0.0011(5) 0.0112(6) 0.0053(5) P2 0.0323(8) 0.0296(7) 0.0266(8) -0.0013(6) 0.0102(6) 0.0046(5) N1 0.028(2) 0.031(2) 0.031(3) 0.0002(19) 0.010(2) 0.0069(17) C10 0.040(3) 0.033(3) 0.052(4) 0.005(3) 0.021(3) 0.001(2) C11 0.043(4) 0.049(3) 0.069(5) -0.004(3) 0.021(3) -0.013(3) C12 0.051(4) 0.062(4) 0.063(5) 0.011(3) 0.029(4) -0.009(3) C20 0.044(3) 0.044(3) 0.030(3) 0.004(2) 0.013(3) 0.010(2) C21 0.056(4) 0.064(4) 0.032(3) -0.007(3) 0.008(3) -0.001(3) C22 0.055(4) 0.060(4) 0.040(4) 0.014(3) 0.012(3) 0.025(3) C30 0.035(3) 0.046(3) 0.037(3) -0.003(3) 0.017(3) -0.003(2) C31 0.052(4) 0.042(3) 0.067(5) -0.005(3) 0.020(3) -0.008(3) C32 0.028(3) 0.073(4) 0.063(5) -0.011(3) 0.005(3) 0.007(3) C40 0.055(4) 0.049(3) 0.030(3) -0.001(3) 0.012(3) 0.022(3) C41 0.078(5) 0.030(3) 0.050(4) 0.000(3) 0.016(3) 0.007(3) C42 0.082(5) 0.054(4) 0.065(5) -0.005(3) 0.037(4) 0.030(3) Li1 0.038(5) 0.032(4) 0.038(5) 0.004(4) 0.010(4) 0.004(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 Te1 P1 2.4118(13) . ? Te1 Li1 2.775(9) . ? Te2 P2 2.3992(16) . ? Te2 Li1 2.727(8) . ? P1 N1 1.587(4) . ? P1 C20 1.836(6) . ? P1 C10 1.836(5) . ? P2 N1 1.598(4) . ? P2 C30 1.834(5) . ? P2 C40 1.848(5) . ? C10 C11 1.510(9) . ? C10 C12 1.533(7) . ? C20 C21 1.531(8) . ? C20 C22 1.545(7) . ? C30 C32 1.523(8) . ? C30 C31 1.533(7) . ? C40 C41 1.519(8) . ? C40 C42 1.540(8) . ? Li1 N3 2.072(16) . ? Li1 N2 2.113(17) . ? Li1 N3A 2.130(16) . ? Li1 N2A 2.142(17) . ? N2 C54 1.466(13) . ? N2 C51 1.493(9) . ? N2 C53 1.505(13) . ? N3 C56 1.482(13) . ? N3 C52 1.484(9) . ? N3 C55 1.486(13) . ? C51 C52 1.549(12) . ? N2A C54A 1.478(14) . ? N2A C51A 1.481(9) . ? N2A C53A 1.485(13) . ? N3A C52A 1.476(9) . ? N3A C56A 1.481(13) . ? N3A C55A 1.496(13) . ? C51A C52A 1.469(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Li1 101.91(17) . . ? P2 Te2 Li1 100.2(2) . . ? N1 P1 C20 105.9(2) . . ? N1 P1 C10 108.4(2) . . ? C20 P1 C10 105.1(3) . . ? N1 P1 Te1 120.82(16) . . ? C20 P1 Te1 106.70(16) . . ? C10 P1 Te1 108.78(18) . . ? N1 P2 C30 108.8(2) . . ? N1 P2 C40 104.7(2) . . ? C30 P2 C40 105.4(3) . . ? N1 P2 Te2 121.48(16) . . ? C30 P2 Te2 108.41(19) . . ? C40 P2 Te2 106.9(2) . . ? P1 N1 P2 143.5(3) . . ? C11 C10 C12 111.2(5) . . ? C11 C10 P1 111.6(4) . . ? C12 C10 P1 113.9(4) . . ? C21 C20 C22 110.0(5) . . ? C21 C20 P1 111.7(4) . . ? C22 C20 P1 111.3(4) . . ? C32 C30 C31 111.0(5) . . ? C32 C30 P2 111.8(4) . . ? C31 C30 P2 110.4(4) . . ? C41 C40 C42 111.7(5) . . ? C41 C40 P2 111.0(4) . . ? C42 C40 P2 112.4(4) . . ? N3 Li1 N2 90.3(5) . . ? N3 Li1 N3A 7.2(5) . . ? N2 Li1 N3A 89.7(5) . . ? N3 Li1 N2A 85.5(5) . . ? N2 Li1 N2A 6.9(5) . . ? N3A Li1 N2A 85.6(5) . . ? N3 Li1 Te2 116.7(5) . . ? N2 Li1 Te2 109.2(5) . . ? N3A Li1 Te2 110.2(4) . . ? N2A Li1 Te2 115.9(5) . . ? N3 Li1 Te1 113.4(5) . . ? N2 Li1 Te1 113.5(5) . . ? N3A Li1 Te1 120.0(5) . . ? N2A Li1 Te1 110.9(5) . . ? Te2 Li1 Te1 111.9(3) . . ? C54 N2 C51 110.2(10) . . ? C54 N2 C53 111.7(11) . . ? C51 N2 C53 105.2(10) . . ? C54 N2 Li1 116.9(9) . . ? C51 N2 Li1 101.2(8) . . ? C53 N2 Li1 110.5(9) . . ? C56 N3 C52 110.0(10) . . ? C56 N3 C55 111.0(11) . . ? C52 N3 C55 109.8(10) . . ? C56 N3 Li1 113.3(10) . . ? C52 N3 Li1 100.5(8) . . ? C55 N3 Li1 111.8(9) . . ? N2 C51 C52 111.3(10) . . ? N3 C52 C51 111.2(9) . . ? C54A N2A C51A 114.0(11) . . ? C54A N2A C53A 108.6(10) . . ? C51A N2A C53A 112.0(10) . . ? C54A N2A Li1 110.5(9) . . ? C51A N2A Li1 100.0(9) . . ? C53A N2A Li1 111.7(9) . . ? C52A N3A C56A 110.4(11) . . ? C52A N3A C55A 109.2(10) . . ? C56A N3A C55A 105.6(10) . . ? C52A N3A Li1 104.8(9) . . ? C56A N3A Li1 108.2(10) . . ? C55A N3A Li1 118.6(9) . . ? C52A C51A N2A 112.6(10) . . ? C51A C52A N3A 110.7(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 Te1 P1 N1 33.7(3) . . . . ? Li1 Te1 P1 C20 154.5(3) . . . . ? Li1 Te1 P1 C10 -92.6(3) . . . . ? Li1 Te2 P2 N1 42.6(2) . . . . ? Li1 Te2 P2 C30 -84.4(3) . . . . ? Li1 Te2 P2 C40 162.4(3) . . . . ? C20 P1 N1 P2 -151.1(4) . . . . ? C10 P1 N1 P2 96.5(5) . . . . ? Te1 P1 N1 P2 -29.9(5) . . . . ? C30 P2 N1 P1 107.4(5) . . . . ? C40 P2 N1 P1 -140.4(5) . . . . ? Te2 P2 N1 P1 -19.5(5) . . . . ? N1 P1 C10 C11 -71.5(4) . . . . ? C20 P1 C10 C11 175.6(4) . . . . ? Te1 P1 C10 C11 61.6(4) . . . . ? N1 P1 C10 C12 161.6(4) . . . . ? C20 P1 C10 C12 48.6(5) . . . . ? Te1 P1 C10 C12 -65.3(5) . . . . ? N1 P1 C20 C21 67.9(4) . . . . ? C10 P1 C20 C21 -177.5(4) . . . . ? Te1 P1 C20 C21 -62.1(4) . . . . ? N1 P1 C20 C22 -55.5(4) . . . . ? C10 P1 C20 C22 59.2(4) . . . . ? Te1 P1 C20 C22 174.5(3) . . . . ? N1 P2 C30 C32 59.3(4) . . . . ? C40 P2 C30 C32 -52.6(4) . . . . ? Te2 P2 C30 C32 -166.7(3) . . . . ? N1 P2 C30 C31 -64.8(5) . . . . ? C40 P2 C30 C31 -176.7(4) . . . . ? Te2 P2 C30 C31 69.2(4) . . . . ? N1 P2 C40 C41 62.4(5) . . . . ? C30 P2 C40 C41 177.1(4) . . . . ? Te2 P2 C40 C41 -67.7(4) . . . . ? N1 P2 C40 C42 -171.8(5) . . . . ? C30 P2 C40 C42 -57.0(5) . . . . ? Te2 P2 C40 C42 58.2(5) . . . . ? P2 Te2 Li1 N3 108.8(5) . . . . ? P2 Te2 Li1 N2 -150.7(4) . . . . ? P2 Te2 Li1 N3A 112.2(5) . . . . ? P2 Te2 Li1 N2A -152.7(4) . . . . ? P2 Te2 Li1 Te1 -24.1(3) . . . . ? P1 Te1 Li1 N3 -138.4(4) . . . . ? P1 Te1 Li1 N2 120.5(4) . . . . ? P1 Te1 Li1 N3A -135.4(5) . . . . ? P1 Te1 Li1 N2A 127.4(4) . . . . ? P1 Te1 Li1 Te2 -3.8(3) . . . . ? N3 Li1 N2 C54 128.7(9) . . . . ? N3A Li1 N2 C54 121.6(9) . . . . ? N2A Li1 N2 C54 175(5) . . . . ? Te2 Li1 N2 C54 10.2(10) . . . . ? Te1 Li1 N2 C54 -115.5(9) . . . . ? N3 Li1 N2 C51 9.0(8) . . . . ? N3A Li1 N2 C51 1.9(8) . . . . ? N2A Li1 N2 C51 55(4) . . . . ? Te2 Li1 N2 C51 -109.5(7) . . . . ? Te1 Li1 N2 C51 124.8(7) . . . . ? N3 Li1 N2 C53 -102.0(9) . . . . ? N3A Li1 N2 C53 -109.2(9) . . . . ? N2A Li1 N2 C53 -56(4) . . . . ? Te2 Li1 N2 C53 139.4(8) . . . . ? Te1 Li1 N2 C53 13.7(9) . . . . ? N2 Li1 N3 C56 136.6(9) . . . . ? N3A Li1 N3 C56 -138(4) . . . . ? N2A Li1 N3 C56 131.6(9) . . . . ? Te2 Li1 N3 C56 -111.6(9) . . . . ? Te1 Li1 N3 C56 20.7(10) . . . . ? N2 Li1 N3 C52 19.3(8) . . . . ? N3A Li1 N3 C52 105(4) . . . . ? N2A Li1 N3 C52 14.3(8) . . . . ? Te2 Li1 N3 C52 131.1(7) . . . . ? Te1 Li1 N3 C52 -96.6(8) . . . . ? N2 Li1 N3 C55 -97.1(9) . . . . ? N3A Li1 N3 C55 -12(4) . . . . ? N2A Li1 N3 C55 -102.1(9) . . . . ? Te2 Li1 N3 C55 14.7(10) . . . . ? Te1 Li1 N3 C55 147.0(8) . . . . ? C54 N2 C51 C52 -160.3(10) . . . . ? C53 N2 C51 C52 79.2(13) . . . . ? Li1 N2 C51 C52 -35.9(11) . . . . ? C56 N3 C52 C51 -164.4(11) . . . . ? C55 N3 C52 C51 73.3(13) . . . . ? Li1 N3 C52 C51 -44.6(11) . . . . ? N2 C51 C52 N3 59.3(14) . . . . ? N3 Li1 N2A C54A 106.1(9) . . . . ? N2 Li1 N2A C54A -27(4) . . . . ? N3A Li1 N2A C54A 98.9(9) . . . . ? Te2 Li1 N2A C54A -11.5(9) . . . . ? Te1 Li1 N2A C54A -140.6(8) . . . . ? N3 Li1 N2A C51A -14.3(8) . . . . ? N2 Li1 N2A C51A -148(5) . . . . ? N3A Li1 N2A C51A -21.5(8) . . . . ? Te2 Li1 N2A C51A -131.9(7) . . . . ? Te1 Li1 N2A C51A 99.0(8) . . . . ? N3 Li1 N2A C53A -132.9(8) . . . . ? N2 Li1 N2A C53A 93(4) . . . . ? N3A Li1 N2A C53A -140.2(8) . . . . ? Te2 Li1 N2A C53A 109.4(8) . . . . ? Te1 Li1 N2A C53A -19.6(9) . . . . ? N3 Li1 N3A C52A -95(4) . . . . ? N2 Li1 N3A C52A -0.3(9) . . . . ? N2A Li1 N3A C52A -5.9(9) . . . . ? Te2 Li1 N3A C52A 110.1(8) . . . . ? Te1 Li1 N3A C52A -117.6(8) . . . . ? N3 Li1 N3A C56A 23(4) . . . . ? N2 Li1 N3A C56A 117.4(8) . . . . ? N2A Li1 N3A C56A 111.9(8) . . . . ? Te2 Li1 N3A C56A -132.1(8) . . . . ? Te1 Li1 N3A C56A 0.2(10) . . . . ? N3 Li1 N3A C55A 143(4) . . . . ? N2 Li1 N3A C55A -122.4(9) . . . . ? N2A Li1 N3A C55A -128.0(9) . . . . ? Te2 Li1 N3A C55A -12.0(10) . . . . ? Te1 Li1 N3A C55A 120.3(9) . . . . ? C54A N2A C51A C52A -69.5(16) . . . . ? C53A N2A C51A C52A 166.7(12) . . . . ? Li1 N2A C51A C52A 48.4(13) . . . . ? N2A C51A C52A N3A -59.8(16) . . . . ? C56A N3A C52A C51A -82.4(15) . . . . ? C55A N3A C52A C51A 162.0(11) . . . . ? Li1 N3A C52A C51A 33.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.770 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.147