# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1793 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C24 H56 N2 P4 S4 Te' _chemical_formula_structural 'C24 H56 N2 P4 S4 Te' _chemical_formula_analytical 'C24 H56 N2 P4 S4 Te' _chemical_formula_sum 'C24 H56 N2 P4 S4 Te' _chemical_formula_weight 752.43 _chemical_melting_point - _chemical_compound_source - 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4727(2) _cell_length_b 14.5022(3) _cell_length_c 11.9760(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.1450(10) _cell_angle_gamma 90.00 _cell_volume 1790.44(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .3 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method - _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.852155 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 7664 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2572 _reflns_number_observed 2332 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+3.2531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0056(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2572 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_obs 0.0196 _refine_ls_wR_factor_all 0.0594 _refine_ls_wR_factor_obs 0.0559 _refine_ls_goodness_of_fit_all 0.528 _refine_ls_goodness_of_fit_obs 0.523 _refine_ls_restrained_S_all 0.528 _refine_ls_restrained_S_obs 0.523 _refine_ls_shift/esd_max -0.029 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.0000 0.0000 0.0000 0.03767(11) Uani 1 d S . S1 S 0.00821(6) 0.15620(4) 0.12341(5) 0.0463(2) Uani 1 d . . P1 P 0.12528(5) 0.11626(4) 0.26946(4) 0.0350(2) Uani 1 d . . N1 N 0.2433(2) 0.04986(13) 0.26146(15) 0.0412(4) Uani 1 d . . C1 C 0.0250(2) 0.0628(2) 0.3625(2) 0.0451(5) Uani 1 d . . H1A H 0.0830(2) 0.0450(2) 0.4326(2) 0.054 Uiso 1 calc R . C2 C -0.0751(3) 0.1291(2) 0.3953(3) 0.0689(8) Uani 1 d . . H2A H -0.0322(3) 0.1834(2) 0.4289(3) 0.103 Uiso 1 calc R . H2B H -0.1202(3) 0.0997(2) 0.4488(3) 0.103 Uiso 1 calc R . H2C H -0.1361(3) 0.1459(2) 0.3288(3) 0.103 Uiso 1 calc R . C3 C -0.0406(3) -0.0249(2) 0.3106(2) 0.0622(7) Uani 1 d . . H3A H 0.0239(3) -0.0663(2) 0.2917(2) 0.093 Uiso 1 calc R . H3B H -0.1011(3) -0.0097(2) 0.2432(2) 0.093 Uiso 1 calc R . H3C H -0.0858(3) -0.0540(2) 0.3642(2) 0.093 Uiso 1 calc R . C4 C 0.1890(2) 0.2223(2) 0.3424(2) 0.0468(6) Uani 1 d . . H4A H 0.1150(2) 0.2585(2) 0.3577(2) 0.056 Uiso 1 calc R . C5 C 0.2739(4) 0.1998(2) 0.4557(2) 0.0800(10) Uani 1 d . . H5A H 0.2252(4) 0.1636(2) 0.5007(2) 0.120 Uiso 1 calc R . H5B H 0.3015(4) 0.2560(2) 0.4950(2) 0.120 Uiso 1 calc R . H5C H 0.3485(4) 0.1656(2) 0.4430(2) 0.120 Uiso 1 calc R . C6 C 0.2618(3) 0.2804(2) 0.2695(2) 0.0626(7) Uani 1 d . . H6A H 0.2059(3) 0.2945(2) 0.1991(2) 0.094 Uiso 1 calc R . H6B H 0.3362(3) 0.2470(2) 0.2547(2) 0.094 Uiso 1 calc R . H6C H 0.2897(3) 0.3367(2) 0.3086(2) 0.094 Uiso 1 calc R . S2 S 0.25491(6) 0.02098(5) 0.00728(5) 0.0455(2) Uani 1 d . . P2 P 0.30871(6) -0.00872(4) 0.17517(5) 0.0340(2) Uani 1 d . . C7 C 0.2750(2) -0.1316(2) 0.1929(2) 0.0442(5) Uani 1 d . . H7A H 0.1820(2) -0.1391(2) 0.1640(2) 0.053 Uiso 1 calc R . C8 C 0.3432(3) -0.1939(2) 0.1188(3) 0.0634(7) Uani 1 d . . H8A H 0.3273(3) -0.1714(2) 0.0423(3) 0.095 Uiso 1 calc R . H8B H 0.3103(3) -0.2556(2) 0.1204(3) 0.095 Uiso 1 calc R . H8C H 0.4348(3) -0.1938(2) 0.1473(3) 0.095 Uiso 1 calc R . C9 C 0.2950(3) -0.1637(2) 0.3165(3) 0.0723(8) Uani 1 d . . H9A H 0.2498(3) -0.1230(2) 0.3593(3) 0.108 Uiso 1 calc R . H9B H 0.3859(3) -0.1630(2) 0.3479(3) 0.108 Uiso 1 calc R . H9C H 0.2620(3) -0.2252(2) 0.3198(3) 0.108 Uiso 1 calc R . C10 C 0.4850(2) 0.0083(2) 0.2061(2) 0.0480(6) Uani 1 d . . H10A H 0.5237(2) -0.0381(2) 0.1627(2) 0.058 Uiso 1 calc R . C11 C 0.5232(3) 0.1021(2) 0.1669(3) 0.0688(8) Uani 1 d . . H11A H 0.4882(3) 0.1096(2) 0.0878(3) 0.103 Uiso 1 calc R . H11B H 0.6160(3) 0.1066(2) 0.1783(3) 0.103 Uiso 1 calc R . H11C H 0.4894(3) 0.1494(2) 0.2097(3) 0.103 Uiso 1 calc R . C12 C 0.5416(4) -0.0066(3) 0.3302(3) 0.1016(15) Uani 1 d . . H12A H 0.5175(4) -0.0666(3) 0.3533(3) 0.152 Uiso 1 calc R . H12B H 0.5088(4) 0.0396(3) 0.3752(3) 0.152 Uiso 1 calc R . H12C H 0.6345(4) -0.0022(3) 0.3409(3) 0.152 Uiso 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 0.0382(2) 0.0464(2) 0.02699(15) 0.00139(8) 0.00197(9) 0.00559(8) S1 0.0531(4) 0.0461(3) 0.0368(3) 0.0009(2) -0.0004(3) 0.0125(3) P1 0.0396(3) 0.0344(3) 0.0305(3) -0.0020(2) 0.0050(2) 0.0025(2) N1 0.0449(10) 0.0434(11) 0.0340(10) -0.0008(8) 0.0029(8) 0.0066(8) C1 0.0479(13) 0.0525(14) 0.0357(12) 0.0001(10) 0.0098(10) 0.0005(11) C2 0.063(2) 0.080(2) 0.072(2) -0.001(2) 0.0329(15) 0.0079(15) C3 0.071(2) 0.067(2) 0.052(2) -0.0019(14) 0.0202(14) -0.0226(15) C4 0.0570(14) 0.0374(12) 0.0467(13) -0.0085(10) 0.0111(11) -0.0003(11) C5 0.115(3) 0.066(2) 0.048(2) -0.0112(14) -0.015(2) -0.022(2) C6 0.073(2) 0.0463(15) 0.070(2) -0.0066(13) 0.0175(14) -0.0098(13) S2 0.0449(4) 0.0569(4) 0.0359(3) 0.0051(3) 0.0101(3) 0.0054(3) P2 0.0328(3) 0.0337(3) 0.0348(3) 0.0006(2) 0.0042(3) 0.0027(2) C7 0.0446(12) 0.0354(12) 0.0522(14) 0.0026(10) 0.0075(10) 0.0018(10) C8 0.070(2) 0.0377(13) 0.086(2) -0.0073(13) 0.023(2) 0.0016(12) C9 0.099(2) 0.051(2) 0.067(2) 0.0178(14) 0.014(2) 0.001(2) C10 0.0338(13) 0.0484(14) 0.061(2) -0.0062(11) 0.0058(12) 0.0025(10) C11 0.052(2) 0.058(2) 0.099(2) -0.009(2) 0.0198(15) -0.0143(13) C12 0.054(2) 0.156(4) 0.082(3) 0.032(2) -0.022(2) -0.019(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 Te1 S2 2.6730(6) 3 ? Te1 S2 2.6730(6) . ? Te1 S1 2.6978(6) 3 ? Te1 S1 2.6978(6) . ? S1 P1 2.0354(8) . ? P1 N1 1.583(2) . ? P1 C1 1.833(2) . ? P1 C4 1.835(2) . ? N1 P2 1.584(2) . ? C1 C2 1.523(4) . ? C1 C3 1.525(4) . ? C4 C6 1.513(3) . ? C4 C5 1.522(4) . ? S2 P2 2.0363(8) . ? P2 C7 1.837(2) . ? P2 C10 1.835(3) . ? C7 C8 1.528(3) . ? C7 C9 1.531(4) . ? C10 C11 1.515(4) . ? C10 C12 1.516(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Te1 S2 180.0 3 . ? S2 Te1 S1 87.21(2) 3 3 ? S2 Te1 S1 92.79(2) . 3 ? S2 Te1 S1 92.79(2) 3 . ? S2 Te1 S1 87.21(2) . . ? S1 Te1 S1 180.0 3 . ? P1 S1 Te1 100.84(3) . . ? N1 P1 C1 108.47(10) . . ? N1 P1 C4 108.44(11) . . ? C1 P1 C4 105.33(11) . . ? N1 P1 S1 118.66(7) . . ? C1 P1 S1 108.66(8) . . ? C4 P1 S1 106.49(8) . . ? P2 N1 P1 142.93(12) . . ? C2 C1 C3 110.5(2) . . ? C2 C1 P1 112.6(2) . . ? C3 C1 P1 111.7(2) . . ? C6 C4 C5 111.0(2) . . ? C6 C4 P1 111.7(2) . . ? C5 C4 P1 110.6(2) . . ? P2 S2 Te1 96.27(3) . . ? N1 P2 C7 109.33(10) . . ? N1 P2 C10 109.35(11) . . ? C7 P2 C10 108.34(11) . . ? N1 P2 S2 117.04(7) . . ? C7 P2 S2 107.09(8) . . ? C10 P2 S2 105.35(10) . . ? C8 C7 C9 112.5(2) . . ? C8 C7 P2 112.8(2) . . ? C9 C7 P2 114.2(2) . . ? C11 C10 C12 110.7(3) . . ? C11 C10 P2 111.7(2) . . ? C12 C10 P2 112.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Te1 S1 P1 116.22(3) 3 . . . ? S2 Te1 S1 P1 -63.78(3) . . . . ? S1 Te1 S1 P1 -94.8(65) 3 . . . ? Te1 S1 P1 N1 37.44(9) . . . . ? Te1 S1 P1 C1 -87.01(8) . . . . ? Te1 S1 P1 C4 159.98(8) . . . . ? C1 P1 N1 P2 119.0(2) . . . . ? C4 P1 N1 P2 -127.1(2) . . . . ? S1 P1 N1 P2 -5.5(3) . . . . ? N1 P1 C1 C2 168.3(2) . . . . ? C4 P1 C1 C2 52.4(2) . . . . ? S1 P1 C1 C2 -61.4(2) . . . . ? N1 P1 C1 C3 -66.7(2) . . . . ? C4 P1 C1 C3 177.4(2) . . . . ? S1 P1 C1 C3 63.6(2) . . . . ? N1 P1 C4 C6 70.7(2) . . . . ? C1 P1 C4 C6 -173.4(2) . . . . ? S1 P1 C4 C6 -58.1(2) . . . . ? N1 P1 C4 C5 -53.6(2) . . . . ? C1 P1 C4 C5 62.4(2) . . . . ? S1 P1 C4 C5 177.7(2) . . . . ? S2 Te1 S2 P2 95.4(3) 3 . . . ? S1 Te1 S2 P2 -109.69(3) 3 . . . ? S1 Te1 S2 P2 70.31(3) . . . . ? P1 N1 P2 C7 -105.4(2) . . . . ? P1 N1 P2 C10 136.1(2) . . . . ? P1 N1 P2 S2 16.5(2) . . . . ? Te1 S2 P2 N1 -54.71(9) . . . . ? Te1 S2 P2 C7 68.37(8) . . . . ? Te1 S2 P2 C10 -176.44(8) . . . . ? N1 P2 C7 C8 -175.7(2) . . . . ? C10 P2 C7 C8 -56.6(2) . . . . ? S2 P2 C7 C8 56.6(2) . . . . ? N1 P2 C7 C9 -45.6(2) . . . . ? C10 P2 C7 C9 73.5(2) . . . . ? S2 P2 C7 C9 -173.3(2) . . . . ? N1 P2 C10 C11 -74.6(2) . . . . ? C7 P2 C10 C11 166.4(2) . . . . ? S2 P2 C10 C11 52.0(2) . . . . ? N1 P2 C10 C12 50.7(2) . . . . ? C7 P2 C10 C12 -68.4(2) . . . . ? S2 P2 C10 C12 177.3(2) . . . . ? _refine_diff_density_max 0.337 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.045 #--- data_2 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C48 H88 N2 P4 S4 Te.[C H Cl3]1.5' _chemical_formula_structural 'C49.50 H89.50 Cl4.50 N2 P4 S4 Te' _chemical_formula_analytical 'C49.50 H89.50 Cl4.50 N2 P4 S4 Te' _chemical_formula_sum 'C49.50 H89.50 Cl4.50 N2 P4 S4 Te' _chemical_formula_weight 1251.98 _chemical_melting_point - _chemical_compound_source - 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4307(3) _cell_length_b 12.75430(10) _cell_length_c 14.4033(3) _cell_angle_alpha 114.9400(10) _cell_angle_beta 108.6960(10) _cell_angle_gamma 89.7000(10) _cell_volume 1626.86(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 86 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method - _exptl_crystal_F_000 653 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.578974 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 8290 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4623 _reflns_number_observed 3454 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 82 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.8612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4541 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_obs 0.0545 _refine_ls_wR_factor_all 0.1840 _refine_ls_wR_factor_obs 0.1305 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.299 _refine_ls_restrained_S_obs 1.052 _refine_ls_shift/esd_max 5.045 _refine_ls_shift/esd_mean 0.124 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.5000 0.5000 0.5000 0.03623(13) Uani 1 d S . S1 S 0.55140(13) 0.64159(10) 0.71349(10) 0.0424(3) Uani 1 d . . P1 P 0.67993(12) 0.55421(10) 0.78559(9) 0.0326(3) Uani 1 d . . N1 N 0.7902(4) 0.4956(3) 0.7338(3) 0.0377(9) Uani 1 d . . P2 P 0.85905(12) 0.48252(10) 0.64613(9) 0.0346(3) Uani 1 d . . S2 S 0.76598(13) 0.53656(12) 0.52910(10) 0.0516(3) Uani 1 d . . C1 C 0.7699(5) 0.6670(4) 0.9260(4) 0.0391(12) Uani 1 d . . H1A H 0.8235(5) 0.7238(4) 0.9184(4) 0.047 Uiso 1 calc R . C2 C 0.8758(6) 0.6232(5) 0.9988(4) 0.0515(14) Uani 1 d . . H2A H 0.9341(6) 0.5795(5) 0.9602(4) 0.062 Uiso 1 calc R . H2B H 0.8289(6) 0.5714(5) 1.0152(4) 0.062 Uiso 1 calc R . C3 C 0.9642(6) 0.7278(6) 1.1062(4) 0.067(2) Uani 1 d . . H3A H 1.0274(6) 0.6989(6) 1.1527(4) 0.081 Uiso 1 calc R . H3B H 1.0175(6) 0.7752(6) 1.0898(4) 0.081 Uiso 1 calc R . C4 C 0.8792(7) 0.8010(6) 1.1655(5) 0.072(2) Uani 1 d . . H4A H 0.9378(7) 0.8694(6) 1.2287(5) 0.086 Uiso 1 calc R . H4B H 0.8371(7) 0.7569(6) 1.1918(5) 0.086 Uiso 1 calc R . C5 C 0.7674(7) 0.8409(5) 1.0948(5) 0.075(2) Uani 1 d . . H5A H 0.8092(7) 0.8955(5) 1.0783(5) 0.090 Uiso 1 calc R . H5B H 0.7095(7) 0.8816(5) 1.1353(5) 0.090 Uiso 1 calc R . C6 C 0.6792(6) 0.7381(5) 0.9879(4) 0.059(2) Uani 1 d . . H6A H 0.6140(6) 0.7672(5) 0.9426(4) 0.070 Uiso 1 calc R . H6B H 0.6282(6) 0.6882(5) 1.0036(4) 0.070 Uiso 1 calc R . C7 C 0.5769(5) 0.4408(4) 0.7912(4) 0.0369(12) Uani 1 d . . H7A H 0.5405(5) 0.4809(4) 0.8499(4) 0.044 Uiso 1 calc R . C8 C 0.4534(5) 0.3759(4) 0.6844(4) 0.0480(14) Uani 1 d . . H8A H 0.3968(5) 0.4320(4) 0.6705(4) 0.058 Uiso 1 calc R . H8B H 0.4859(5) 0.3380(4) 0.6239(4) 0.058 Uiso 1 calc R . C9 C 0.3668(6) 0.2837(5) 0.6910(5) 0.064(2) Uani 1 d . . H9A H 0.3279(6) 0.3223(5) 0.7475(5) 0.077 Uiso 1 calc R . H9B H 0.2919(6) 0.2427(5) 0.6219(5) 0.077 Uiso 1 calc R . C10 C 0.4519(6) 0.1970(5) 0.7162(5) 0.064(2) Uani 1 d . . H10A H 0.4844(6) 0.1534(5) 0.6567(5) 0.077 Uiso 1 calc R . H10B H 0.3960(6) 0.1419(5) 0.7230(5) 0.077 Uiso 1 calc R . C11 C 0.5748(7) 0.2601(5) 0.8231(5) 0.067(2) Uani 1 d . . H11A H 0.5420(7) 0.2968(5) 0.8836(5) 0.080 Uiso 1 calc R . H11B H 0.6311(7) 0.2034(5) 0.8359(5) 0.080 Uiso 1 calc R . C12 C 0.6617(6) 0.3533(4) 0.8189(4) 0.0532(15) Uani 1 d . . H12A H 0.7344(6) 0.3948(4) 0.8892(4) 0.064 Uiso 1 calc R . H12B H 0.7037(6) 0.3154(4) 0.7644(4) 0.064 Uiso 1 calc R . C13 C 0.8780(5) 0.3285(4) 0.5836(4) 0.0465(13) Uani 1 d . . H13A H 0.9293(5) 0.3106(4) 0.6439(4) 0.056 Uiso 1 calc R . C14 C 0.9603(6) 0.2961(5) 0.5064(5) 0.068(2) Uani 1 d . . H14A H 0.9134(6) 0.3125(5) 0.4451(5) 0.081 Uiso 1 calc R . H14B H 1.0497(6) 0.3443(5) 0.5452(5) 0.081 Uiso 1 calc R . C15 C 0.9783(7) 0.1675(6) 0.4638(6) 0.086(2) Uani 1 d . . H15A H 1.0356(7) 0.1531(6) 0.5238(6) 0.103 Uiso 1 calc R . H15B H 1.0239(7) 0.1490(6) 0.4109(6) 0.103 Uiso 1 calc R . C16 C 0.8387(8) 0.0881(6) 0.4095(6) 0.090(2) Uani 1 d . . H16A H 0.7854(8) 0.0960(6) 0.3445(6) 0.108 Uiso 1 calc R . H16B H 0.8530(8) 0.0071(6) 0.3874(6) 0.108 Uiso 1 calc R . C17 C 0.7615(7) 0.1196(5) 0.4863(6) 0.083(2) Uani 1 d . . H17A H 0.8120(7) 0.1065(5) 0.5489(6) 0.100 Uiso 1 calc R . H17B H 0.6736(7) 0.0695(5) 0.4499(6) 0.100 Uiso 1 calc R . C18 C 0.7392(6) 0.2470(5) 0.5252(5) 0.068(2) Uani 1 d . . H18A H 0.6892(6) 0.2651(5) 0.5752(5) 0.081 Uiso 1 calc R . H18B H 0.6850(6) 0.2596(5) 0.4632(5) 0.081 Uiso 1 calc R . C19 C 1.0331(5) 0.5657(4) 0.7141(4) 0.0395(12) Uani 1 d . . H19A H 1.0743(5) 0.5487(4) 0.6579(4) 0.047 Uiso 1 calc R . C20 C 1.1254(5) 0.5314(5) 0.8000(4) 0.0509(14) Uani 1 d . . H20A H 1.0831(5) 0.5415(5) 0.8536(4) 0.061 Uiso 1 calc R . H20B H 1.1340(5) 0.4493(5) 0.7649(4) 0.061 Uiso 1 calc R . C21 C 1.2663(6) 0.6033(5) 0.8576(5) 0.064(2) Uani 1 d . . H21A H 1.3132(6) 0.5855(5) 0.8057(5) 0.077 Uiso 1 calc R . H21B H 1.3187(6) 0.5820(5) 0.9144(5) 0.077 Uiso 1 calc R . C22 C 1.2603(6) 0.7339(5) 0.9085(5) 0.071(2) Uani 1 d . . H22A H 1.3521(6) 0.7770(5) 0.9407(5) 0.085 Uiso 1 calc R . H22B H 1.2228(6) 0.7534(5) 0.9663(5) 0.085 Uiso 1 calc R . C23 C 1.1717(7) 0.7698(5) 0.8229(5) 0.070(2) Uani 1 d . . H23A H 1.2144(7) 0.7578(5) 0.7692(5) 0.085 Uiso 1 calc R . H23B H 1.1651(7) 0.8523(5) 0.8578(5) 0.085 Uiso 1 calc R . C24 C 1.0281(6) 0.6985(4) 0.7657(5) 0.0534(15) Uani 1 d . . H24A H 0.9756(6) 0.7200(4) 0.7090(5) 0.064 Uiso 1 calc R . H24B H 0.9820(6) 0.7170(4) 0.8182(5) 0.064 Uiso 1 calc R . C30 C 0.2895(10) 0.0944(7) 0.2419(10) 0.108(4) Uani 0.75 d P . H30A H 0.2977(10) 0.1795(7) 0.2692(10) 0.130 Uiso 0.75 calc PR . Cl1 Cl 0.4288(4) 0.0441(2) 0.1968(3) 0.1358(11) Uani 0.75 d P . Cl2 Cl 0.1411(5) 0.0312(3) 0.1362(5) 0.191(2) Uani 0.75 d P . Cl3 Cl 0.3045(6) 0.0585(4) 0.3485(4) 0.210(2) Uani 0.75 d P . 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 0.0282(2) 0.0439(2) 0.0417(2) 0.0254(2) 0.0097(2) 0.0022(2) S1 0.0420(7) 0.0407(6) 0.0491(6) 0.0249(5) 0.0149(5) 0.0091(5) P1 0.0294(6) 0.0349(6) 0.0369(6) 0.0174(5) 0.0138(5) 0.0034(5) N1 0.030(2) 0.051(2) 0.042(2) 0.024(2) 0.018(2) 0.010(2) P2 0.0269(6) 0.0423(6) 0.0356(6) 0.0178(5) 0.0114(5) 0.0024(5) S2 0.0306(7) 0.0855(8) 0.0545(7) 0.0475(6) 0.0119(5) 0.0035(6) C1 0.028(2) 0.043(2) 0.045(2) 0.017(2) 0.016(2) 0.000(2) C2 0.042(3) 0.064(3) 0.039(3) 0.017(2) 0.010(2) 0.005(3) C3 0.057(4) 0.086(4) 0.036(3) 0.013(3) 0.007(3) -0.003(3) C4 0.074(4) 0.075(4) 0.044(3) 0.009(3) 0.017(3) -0.002(4) C5 0.090(5) 0.063(4) 0.056(3) 0.006(3) 0.034(3) 0.014(4) C6 0.057(3) 0.063(3) 0.042(3) 0.009(2) 0.021(2) 0.016(3) C7 0.035(3) 0.040(2) 0.037(2) 0.016(2) 0.014(2) 0.000(2) C8 0.035(3) 0.049(3) 0.058(3) 0.027(2) 0.008(2) -0.006(2) C9 0.046(3) 0.072(3) 0.072(3) 0.039(3) 0.007(3) -0.019(3) C10 0.068(4) 0.045(3) 0.075(3) 0.031(3) 0.011(3) -0.014(3) C11 0.074(4) 0.057(3) 0.078(3) 0.045(3) 0.017(3) 0.005(3) C12 0.050(3) 0.045(3) 0.063(3) 0.028(2) 0.010(3) 0.004(2) C13 0.049(3) 0.046(3) 0.046(3) 0.017(2) 0.023(2) 0.004(2) C14 0.066(4) 0.062(3) 0.070(3) 0.009(3) 0.045(3) -0.001(3) C15 0.087(4) 0.067(4) 0.104(5) 0.016(3) 0.066(4) 0.017(4) C16 0.096(5) 0.060(4) 0.077(4) -0.008(3) 0.039(4) -0.003(4) C17 0.082(5) 0.046(3) 0.100(5) 0.004(3) 0.045(4) -0.012(3) C18 0.052(3) 0.062(4) 0.072(4) 0.007(3) 0.030(3) -0.015(3) C19 0.027(2) 0.054(3) 0.039(2) 0.022(2) 0.011(2) -0.001(2) C20 0.036(3) 0.059(3) 0.054(3) 0.025(2) 0.011(2) 0.008(2) C21 0.032(3) 0.089(4) 0.058(3) 0.026(3) 0.007(2) 0.008(3) C22 0.043(3) 0.069(4) 0.068(4) 0.013(3) 0.004(3) -0.010(3) C23 0.060(4) 0.062(3) 0.069(4) 0.020(3) 0.010(3) -0.015(3) C24 0.042(3) 0.047(3) 0.062(3) 0.022(2) 0.011(2) -0.002(2) C30 0.075(6) 0.050(4) 0.220(10) 0.077(5) 0.053(6) 0.001(4) Cl1 0.143(2) 0.0688(13) 0.254(3) 0.088(2) 0.119(2) 0.0419(15) Cl2 0.117(3) 0.086(2) 0.268(5) 0.043(3) -0.012(3) -0.005(2) Cl3 0.274(5) 0.228(4) 0.262(4) 0.172(3) 0.173(3) 0.128(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 S2 2.6820(13) . ? Te1 S2 2.6821(13) 2_666 ? Te1 S1 2.6971(12) 2_666 ? Te1 S1 2.6971(12) . ? S1 P1 2.046(2) . ? P1 N1 1.584(4) . ? P1 C1 1.839(4) . ? P1 C7 1.850(5) . ? N1 P2 1.594(4) . ? P2 C13 1.825(5) . ? P2 C19 1.840(5) . ? P2 S2 2.045(2) . ? C1 C6 1.538(7) . ? C1 C2 1.541(7) . ? C2 C3 1.542(7) . ? C3 C4 1.480(9) . ? C4 C5 1.525(9) . ? C5 C6 1.529(8) . ? C7 C12 1.525(7) . ? C7 C8 1.541(6) . ? C8 C9 1.539(7) . ? C9 C10 1.505(8) . ? C10 C11 1.537(8) . ? C11 C12 1.531(8) . ? C13 C14 1.537(8) . ? C13 C18 1.544(7) . ? C14 C15 1.525(9) . ? C15 C16 1.541(10) . ? C16 C17 1.492(10) . ? C17 C18 1.523(9) . ? C19 C20 1.529(7) . ? C19 C24 1.545(7) . ? C20 C21 1.509(8) . ? C21 C22 1.522(9) . ? C22 C23 1.524(9) . ? C23 C24 1.530(8) . ? C30 Cl2 1.682(11) . ? C30 Cl3 1.741(13) . ? C30 Cl1 1.785(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 S2 Te1 S2 180.0 . 2_666 ? S2 Te1 S1 89.33(4) . 2_666 ? S2 Te1 S1 90.67(4) 2_666 2_666 ? S2 Te1 S1 90.67(4) . . ? S2 Te1 S1 89.33(4) 2_666 . ? S1 Te1 S1 180.0 2_666 . ? P1 S1 Te1 101.11(6) . . ? N1 P1 C1 108.6(2) . . ? N1 P1 C7 108.6(2) . . ? C1 P1 C7 108.6(2) . . ? N1 P1 S1 117.7(2) . . ? C1 P1 S1 103.8(2) . . ? C7 P1 S1 109.2(2) . . ? P1 N1 P2 145.3(3) . . ? N1 P2 C13 105.5(2) . . ? N1 P2 C19 110.7(2) . . ? C13 P2 C19 106.4(2) . . ? N1 P2 S2 118.7(2) . . ? C13 P2 S2 110.8(2) . . ? C19 P2 S2 104.2(2) . . ? P2 S2 Te1 102.98(6) . . ? C6 C1 C2 109.7(4) . . ? C6 C1 P1 116.2(3) . . ? C2 C1 P1 114.4(3) . . ? C1 C2 C3 110.1(5) . . ? C4 C3 C2 111.8(5) . . ? C3 C4 C5 112.9(5) . . ? C4 C5 C6 112.0(5) . . ? C5 C6 C1 110.2(5) . . ? C12 C7 C8 110.1(4) . . ? C12 C7 P1 112.8(3) . . ? C8 C7 P1 111.9(3) . . ? C9 C8 C7 111.5(4) . . ? C10 C9 C8 111.1(5) . . ? C9 C10 C11 110.5(4) . . ? C12 C11 C10 111.5(5) . . ? C7 C12 C11 112.1(5) . . ? C14 C13 C18 109.7(4) . . ? C14 C13 P2 115.6(4) . . ? C18 C13 P2 112.3(4) . . ? C15 C14 C13 111.9(5) . . ? C14 C15 C16 110.9(6) . . ? C17 C16 C15 110.9(5) . . ? C16 C17 C18 111.4(6) . . ? C17 C18 C13 110.3(5) . . ? C20 C19 C24 110.3(4) . . ? C20 C19 P2 113.0(4) . . ? C24 C19 P2 110.5(3) . . ? C21 C20 C19 112.3(5) . . ? C20 C21 C22 112.0(5) . . ? C21 C22 C23 110.8(5) . . ? C22 C23 C24 111.0(5) . . ? C23 C24 C19 111.6(5) . . ? Cl2 C30 Cl3 112.9(6) . . ? Cl2 C30 Cl1 109.3(7) . . ? Cl3 C30 Cl1 106.3(6) . . ? 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 S2 Te1 S1 P1 -62.05(6) . . . . ? S2 Te1 S1 P1 117.96(6) 2_666 . . . ? S1 Te1 S1 P1 127.0(248) 2_666 . . . ? Te1 S1 P1 N1 39.4(2) . . . . ? Te1 S1 P1 C1 159.4(2) . . . . ? Te1 S1 P1 C7 -84.9(2) . . . . ? C1 P1 N1 P2 -109.3(4) . . . . ? C7 P1 N1 P2 132.8(4) . . . . ? S1 P1 N1 P2 8.2(5) . . . . ? P1 N1 P2 C13 -139.1(4) . . . . ? P1 N1 P2 C19 106.2(4) . . . . ? P1 N1 P2 S2 -14.2(5) . . . . ? N1 P2 S2 Te1 -30.5(2) . . . . ? C13 P2 S2 Te1 91.7(2) . . . . ? C19 P2 S2 Te1 -154.2(2) . . . . ? S2 Te1 S2 P2 143.0(30) 2_666 . . . ? S1 Te1 S2 P2 -121.95(6) 2_666 . . . ? S1 Te1 S2 P2 58.05(6) . . . . ? N1 P1 C1 C6 177.1(4) . . . . ? C7 P1 C1 C6 -65.0(5) . . . . ? S1 P1 C1 C6 51.1(4) . . . . ? N1 P1 C1 C2 -53.6(4) . . . . ? C7 P1 C1 C2 64.3(4) . . . . ? S1 P1 C1 C2 -179.5(3) . . . . ? C6 C1 C2 C3 -58.3(6) . . . . ? P1 C1 C2 C3 169.2(4) . . . . ? C1 C2 C3 C4 56.3(7) . . . . ? C2 C3 C4 C5 -53.5(8) . . . . ? C3 C4 C5 C6 53.2(8) . . . . ? C4 C5 C6 C1 -54.9(7) . . . . ? C2 C1 C6 C5 57.9(6) . . . . ? P1 C1 C6 C5 -170.5(4) . . . . ? N1 P1 C7 C12 37.2(4) . . . . ? C1 P1 C7 C12 -80.7(4) . . . . ? S1 P1 C7 C12 166.7(3) . . . . ? N1 P1 C7 C8 -87.6(4) . . . . ? C1 P1 C7 C8 154.5(3) . . . . ? S1 P1 C7 C8 41.9(4) . . . . ? C12 C7 C8 C9 54.9(6) . . . . ? P1 C7 C8 C9 -178.8(4) . . . . ? C7 C8 C9 C10 -57.2(6) . . . . ? C8 C9 C10 C11 56.8(7) . . . . ? C9 C10 C11 C12 -55.9(7) . . . . ? C8 C7 C12 C11 -54.1(6) . . . . ? P1 C7 C12 C11 -180.0(4) . . . . ? C10 C11 C12 C7 55.1(7) . . . . ? N1 P2 C13 C14 -172.0(4) . . . . ? C19 P2 C13 C14 -54.4(5) . . . . ? S2 P2 C13 C14 58.3(4) . . . . ? N1 P2 C13 C18 61.0(4) . . . . ? C19 P2 C13 C18 178.6(4) . . . . ? S2 P2 C13 C18 -68.7(4) . . . . ? C18 C13 C14 C15 -55.3(7) . . . . ? P2 C13 C14 C15 176.4(4) . . . . ? C13 C14 C15 C16 54.4(8) . . . . ? C14 C15 C16 C17 -55.3(9) . . . . ? C15 C16 C17 C18 57.9(8) . . . . ? C16 C17 C18 C13 -59.0(8) . . . . ? C14 C13 C18 C17 56.6(7) . . . . ? P2 C13 C18 C17 -173.3(5) . . . . ? N1 P2 C19 C20 55.8(4) . . . . ? C13 P2 C19 C20 -58.3(4) . . . . ? S2 P2 C19 C20 -175.5(3) . . . . ? N1 P2 C19 C24 -68.4(4) . . . . ? C13 P2 C19 C24 177.5(4) . . . . ? S2 P2 C19 C24 60.3(4) . . . . ? C24 C19 C20 C21 -53.7(6) . . . . ? P2 C19 C20 C21 -178.0(4) . . . . ? C19 C20 C21 C22 55.1(7) . . . . ? C20 C21 C22 C23 -55.6(7) . . . . ? C21 C22 C23 C24 55.9(7) . . . . ? C22 C23 C24 C19 -55.9(7) . . . . ? C20 C19 C24 C23 54.2(6) . . . . ? P2 C19 C24 C23 179.9(4) . . . . ? _refine_diff_density_max 1.042 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.099 #--- data_3 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C32 H40 N2 O4 P4 S4 Te' _chemical_formula_structural 'C32 H40 N2 O4 P4 S4 Te' _chemical_formula_analytical 'C32 H40 N2 O4 P4 S4 Te' _chemical_formula_sum 'C32 H40 N2 O4 P4 S4 Te' _chemical_formula_weight 896.38 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.7944(11) _cell_length_b 11.8286(5) _cell_length_c 30.2546(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.0180(10) _cell_angle_gamma 90.00 _cell_volume 7947.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method - _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.794274 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 17090 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5721 _reflns_number_observed 3895 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+8.0200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00145(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5671 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_obs 0.0323 _refine_ls_wR_factor_all 0.0809 _refine_ls_wR_factor_obs 0.0599 _refine_ls_goodness_of_fit_all 0.894 _refine_ls_goodness_of_fit_obs 0.930 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 0.930 _refine_ls_shift/esd_max -0.026 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.132294(13) 0.09180(2) 0.119680(9) 0.05541(12) Uani 1 d . . S1 S 0.13008(6) 0.04190(10) 0.03812(4) 0.0679(3) Uani 1 d . . P1 P 0.09892(5) 0.18601(10) 0.00324(4) 0.0555(3) Uani 1 d . . N1 N 0.12339(14) 0.3029(3) 0.02525(10) 0.0529(9) Uani 1 d . . P2 P 0.17412(5) 0.35532(9) 0.06295(4) 0.0506(3) Uani 1 d . . S2 S 0.22173(5) 0.26111(10) 0.11139(4) 0.0644(3) Uani 1 d . . C1 C 0.1206(2) 0.1624(4) -0.04993(14) 0.0815(15) Uani 1 d . . H1A H 0.1642(2) 0.1618(4) -0.04401(14) 0.098 Uiso 1 calc R . H1B H 0.1067(2) 0.0879(4) -0.06090(14) 0.098 Uiso 1 calc R . C2 C 0.0977(2) 0.2466(5) -0.0874(2) 0.097(2) Uani 1 d . . H2A H 0.1117(2) 0.2258(5) -0.1139(2) 0.146 Uiso 1 calc R . H2B H 0.1122(2) 0.3207(5) -0.0777(2) 0.146 Uiso 1 calc R . H2C H 0.0544(2) 0.2468(5) -0.0945(2) 0.146 Uiso 1 calc R . C3 C 0.0180(2) 0.1889(5) -0.0103(2) 0.092(2) Uani 1 d . . H3A H 0.0051(2) 0.2560(5) -0.0283(2) 0.110 Uiso 1 calc R . H3B H 0.0038(2) 0.1241(5) -0.0294(2) 0.110 Uiso 1 calc R . C4 C -0.0114(2) 0.1882(5) 0.0264(2) 0.113(2) Uani 1 d . . H4A H -0.0542(2) 0.1902(5) 0.0147(2) 0.170 Uiso 1 calc R . H4B H 0.0008(2) 0.2532(5) 0.0452(2) 0.170 Uiso 1 calc R . H4C H -0.0008(2) 0.1207(5) 0.0440(2) 0.170 Uiso 1 calc R . O5 O 0.22288(11) 0.4208(2) 0.04222(9) 0.0617(8) Uani 1 d . . C5 C 0.2078(2) 0.4910(4) 0.0033(2) 0.0594(11) Uani 1 d . . C6 C 0.2139(2) 0.4486(4) -0.0370(2) 0.0724(13) Uani 1 d . . H6A H 0.2246(2) 0.3733(4) -0.0393(2) 0.087 Uiso 1 calc R . C7 C 0.2042(2) 0.5182(5) -0.0748(2) 0.086(2) Uani 1 d . . H7A H 0.2090(2) 0.4901(5) -0.1025(2) 0.103 Uiso 1 calc R . C8 C 0.1876(2) 0.6267(6) -0.0714(2) 0.090(2) Uani 1 d . . H8A H 0.1799(2) 0.6728(6) -0.0970(2) 0.108 Uiso 1 calc R . C9 C 0.1820(2) 0.6695(5) -0.0306(2) 0.092(2) Uani 1 d . . H9A H 0.1714(2) 0.7448(5) -0.0284(2) 0.110 Uiso 1 calc R . C10 C 0.1921(2) 0.6010(4) 0.0078(2) 0.0759(14) Uani 1 d . . H10A H 0.1883(2) 0.6294(4) 0.0357(2) 0.091 Uiso 1 calc R . O11 O 0.14489(12) 0.4626(2) 0.08258(9) 0.0563(7) Uani 1 d . . C11 C 0.0906(2) 0.4522(4) 0.0960(2) 0.0612(12) Uani 1 d . . C12 C 0.0902(3) 0.4121(4) 0.1379(2) 0.088(2) Uani 1 d . . H12A H 0.1257(3) 0.3897(4) 0.1577(2) 0.106 Uiso 1 calc R . C13 C 0.0351(4) 0.4056(6) 0.1505(3) 0.123(3) Uani 1 d . . H13A H 0.0337(4) 0.3787(6) 0.1791(3) 0.148 Uiso 1 calc R . C14 C -0.0167(4) 0.4383(7) 0.1214(4) 0.146(4) Uani 1 d . . H14A H -0.0532(4) 0.4327(7) 0.1300(4) 0.175 Uiso 1 calc R . C15 C -0.0152(3) 0.4792(7) 0.0796(3) 0.138(3) Uani 1 d . . H15A H -0.0507(3) 0.5022(7) 0.0599(3) 0.166 Uiso 1 calc R . C16 C 0.0390(3) 0.4868(4) 0.0664(2) 0.086(2) Uani 1 d . . H16A H 0.0403(3) 0.5148(4) 0.0379(2) 0.104 Uiso 1 calc R . S3 S 0.05812(5) -0.06358(9) 0.12274(4) 0.0632(3) Uani 1 d . . P3 P 0.11896(5) -0.17482(9) 0.15990(3) 0.0514(3) Uani 1 d . . N3 N 0.16103(14) -0.1275(3) 0.20428(10) 0.0543(9) Uani 1 d . . P4 P 0.16281(5) -0.02447(9) 0.23756(3) 0.0543(3) Uani 1 d . . S4 S 0.12825(6) 0.12204(9) 0.21417(4) 0.0686(3) Uani 1 d . . C17 C 0.1654(2) -0.2285(4) 0.12377(15) 0.0761(14) Uani 1 d . . H17A H 0.1398(2) -0.2674(4) 0.09834(15) 0.091 Uiso 1 calc R . H17B H 0.1838(2) -0.1651(4) 0.11171(15) 0.091 Uiso 1 calc R . C18 C 0.2137(2) -0.3073(5) 0.1465(2) 0.102(2) Uani 1 d . . H18A H 0.2363(2) -0.3320(5) 0.1251(2) 0.153 Uiso 1 calc R . H18B H 0.1960(2) -0.3715(5) 0.1578(2) 0.153 Uiso 1 calc R . H18C H 0.2400(2) -0.2691(5) 0.1712(2) 0.153 Uiso 1 calc R . C19 C 0.0743(2) -0.2900(4) 0.17232(14) 0.0674(13) Uani 1 d . . H19A H 0.0516(2) -0.3212(4) 0.14395(14) 0.081 Uiso 1 calc R . H19B H 0.1010(2) -0.3487(4) 0.18762(14) 0.081 Uiso 1 calc R . C20 C 0.0307(2) -0.2586(4) 0.2016(2) 0.091(2) Uani 1 d . . H20A H 0.0086(2) -0.3244(4) 0.2067(2) 0.137 Uiso 1 calc R . H20B H 0.0032(2) -0.2020(4) 0.1864(2) 0.137 Uiso 1 calc R . H20C H 0.0528(2) -0.2294(4) 0.2301(2) 0.137 Uiso 1 calc R . O21 O 0.23111(13) -0.0111(2) 0.26502(8) 0.0612(8) Uani 1 d . . C21 C 0.2777(2) 0.0041(4) 0.24259(14) 0.0576(11) Uani 1 d . . C22 C 0.3118(2) -0.0874(4) 0.2367(2) 0.087(2) Uani 1 d . . H22A H 0.3026(2) -0.1585(4) 0.2463(2) 0.104 Uiso 1 calc R . C23 C 0.3597(3) -0.0739(5) 0.2165(2) 0.112(2) Uani 1 d . . H23A H 0.3830(3) -0.1359(5) 0.2124(2) 0.134 Uiso 1 calc R . C24 C 0.3729(3) 0.0312(7) 0.2024(2) 0.103(2) Uani 1 d . . H24A H 0.4054(3) 0.0406(7) 0.1888(2) 0.123 Uiso 1 calc R . C25 C 0.3386(3) 0.1221(5) 0.2082(2) 0.086(2) Uani 1 d . . H25A H 0.3476(3) 0.1934(5) 0.1985(2) 0.103 Uiso 1 calc R . C26 C 0.2909(2) 0.1084(4) 0.22838(15) 0.0701(13) Uani 1 d . . H26A H 0.2676(2) 0.1704(4) 0.23237(15) 0.084 Uiso 1 calc R . O27 O 0.13389(13) -0.0678(2) 0.27779(9) 0.0660(8) Uani 1 d . . C27 C 0.1218(2) -0.0005(4) 0.31242(14) 0.0540(11) Uani 1 d . . C28 C 0.1636(2) 0.0088(4) 0.35217(15) 0.0600(11) Uani 1 d . . H28A H 0.2007(2) -0.0271(4) 0.35602(15) 0.072 Uiso 1 calc R . C29 C 0.1499(2) 0.0725(4) 0.3868(2) 0.0712(13) Uani 1 d . . H29A H 0.1781(2) 0.0796(4) 0.4141(2) 0.085 Uiso 1 calc R . C30 C 0.0961(3) 0.1247(4) 0.3814(2) 0.083(2) Uani 1 d . . H30A H 0.0877(3) 0.1680(4) 0.4048(2) 0.099 Uiso 1 calc R . C31 C 0.0541(2) 0.1143(5) 0.3420(2) 0.094(2) Uani 1 d . . H31A H 0.0169(2) 0.1496(5) 0.3386(2) 0.112 Uiso 1 calc R . C32 C 0.0668(2) 0.0512(5) 0.3070(2) 0.0818(15) Uani 1 d . . H32A H 0.0383(2) 0.0438(5) 0.2798(2) 0.098 Uiso 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 0.0607(2) 0.0438(2) 0.0562(2) -0.00059(14) 0.00152(13) -0.0012(2) S1 0.0881(9) 0.0500(7) 0.0627(7) -0.0065(6) 0.0107(6) 0.0039(6) P1 0.0530(7) 0.0573(8) 0.0519(7) -0.0071(6) 0.0026(5) 0.0011(6) N1 0.054(2) 0.052(2) 0.049(2) -0.005(2) 0.003(2) 0.005(2) P2 0.0476(7) 0.0480(7) 0.0536(6) -0.0018(5) 0.0061(5) -0.0016(5) S2 0.0601(7) 0.0581(7) 0.0655(7) 0.0070(6) -0.0056(6) -0.0038(6) C1 0.110(4) 0.074(3) 0.059(3) -0.014(3) 0.016(3) 0.006(3) C2 0.108(4) 0.111(5) 0.066(3) 0.006(3) 0.008(3) 0.001(4) C3 0.073(4) 0.095(4) 0.103(4) -0.024(3) 0.009(3) -0.014(3) C4 0.086(4) 0.139(6) 0.121(5) -0.027(4) 0.034(4) -0.014(4) O5 0.046(2) 0.070(2) 0.067(2) 0.013(2) 0.0083(14) -0.0008(15) C5 0.045(3) 0.064(3) 0.070(3) 0.007(3) 0.014(2) 0.000(2) C6 0.075(3) 0.068(3) 0.077(3) 0.005(3) 0.024(3) 0.003(3) C7 0.084(4) 0.104(5) 0.076(4) 0.017(4) 0.030(3) 0.011(3) C8 0.082(4) 0.102(5) 0.086(4) 0.039(4) 0.016(3) 0.006(3) C9 0.104(4) 0.065(4) 0.108(4) 0.026(4) 0.028(4) 0.010(3) C10 0.085(4) 0.067(4) 0.078(3) 0.008(3) 0.024(3) 0.003(3) O11 0.057(2) 0.046(2) 0.066(2) -0.0082(14) 0.0151(15) -0.0056(14) C11 0.070(4) 0.040(3) 0.074(3) -0.017(2) 0.020(3) -0.002(2) C12 0.122(5) 0.061(3) 0.096(4) -0.010(3) 0.055(4) 0.000(3) C13 0.174(8) 0.080(5) 0.149(7) -0.015(4) 0.105(7) -0.020(5) C14 0.136(8) 0.108(7) 0.229(12) -0.090(8) 0.116(9) -0.041(6) C15 0.068(5) 0.138(7) 0.211(9) -0.101(7) 0.036(6) 0.006(4) C16 0.075(4) 0.086(4) 0.095(4) -0.037(3) 0.014(3) 0.010(3) S3 0.0596(7) 0.0567(8) 0.0655(7) -0.0006(6) -0.0026(6) -0.0079(6) P3 0.0577(7) 0.0432(7) 0.0520(7) -0.0101(5) 0.0097(6) -0.0031(5) N3 0.060(2) 0.042(2) 0.056(2) -0.008(2) 0.003(2) 0.005(2) P4 0.0657(8) 0.0436(7) 0.0499(7) -0.0068(5) 0.0054(6) -0.0049(6) S4 0.0909(9) 0.0445(7) 0.0665(7) -0.0072(6) 0.0096(7) 0.0045(6) C17 0.094(4) 0.067(3) 0.067(3) -0.009(3) 0.018(3) 0.007(3) C18 0.108(4) 0.107(5) 0.093(4) -0.011(4) 0.027(3) 0.027(4) C19 0.079(3) 0.051(3) 0.067(3) -0.005(2) 0.008(3) -0.017(2) C20 0.097(4) 0.096(4) 0.087(4) -0.007(3) 0.033(3) -0.030(3) O21 0.066(2) 0.063(2) 0.049(2) -0.0034(14) -0.001(2) -0.013(2) C21 0.061(3) 0.051(3) 0.053(3) -0.006(2) -0.004(2) -0.006(3) C22 0.071(4) 0.061(4) 0.120(4) 0.004(3) 0.003(3) 0.000(3) C23 0.077(4) 0.078(5) 0.181(7) -0.029(4) 0.030(4) 0.004(4) C24 0.079(4) 0.126(6) 0.109(5) -0.025(4) 0.035(3) -0.020(4) C25 0.088(4) 0.081(4) 0.087(4) 0.006(3) 0.017(3) -0.015(3) C26 0.078(4) 0.059(3) 0.072(3) -0.007(3) 0.015(3) -0.008(3) O27 0.090(2) 0.048(2) 0.061(2) -0.0113(15) 0.021(2) -0.014(2) C27 0.054(3) 0.052(3) 0.056(3) 0.001(2) 0.013(2) -0.010(2) C28 0.057(3) 0.059(3) 0.063(3) 0.001(2) 0.012(2) 0.000(2) C29 0.078(4) 0.077(4) 0.059(3) -0.009(3) 0.015(3) -0.016(3) C30 0.094(4) 0.078(4) 0.086(4) -0.025(3) 0.043(4) -0.019(3) C31 0.062(4) 0.100(5) 0.127(5) -0.022(4) 0.038(4) 0.007(3) C32 0.055(3) 0.101(4) 0.080(3) -0.014(3) -0.002(3) -0.003(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 S3 2.5131(12) . ? Te1 S1 2.5267(11) . ? S1 P1 2.046(2) . ? P1 N1 1.580(3) . ? P1 C3 1.798(5) . ? P1 C1 1.808(4) . ? N1 P2 1.558(3) . ? P2 O5 1.595(3) . ? P2 O11 1.607(3) . ? P2 S2 1.9624(15) . ? C1 C2 1.511(6) . ? C3 C4 1.419(6) . ? O5 C5 1.418(5) . ? C5 C6 1.355(6) . ? C5 C10 1.364(6) . ? C6 C7 1.387(6) . ? C7 C8 1.349(7) . ? C8 C9 1.367(7) . ? C9 C10 1.390(6) . ? O11 C11 1.393(5) . ? C11 C12 1.355(6) . ? C11 C16 1.373(6) . ? C12 C13 1.395(8) . ? C13 C14 1.360(10) . ? C14 C15 1.360(11) . ? C15 C16 1.384(8) . ? S3 P3 2.053(2) . ? P3 N3 1.567(3) . ? P3 C19 1.790(4) . ? P3 C17 1.800(4) . ? N3 P4 1.576(3) . ? P4 O27 1.594(3) . ? P4 O21 1.599(3) . ? P4 S4 1.968(2) . ? C17 C18 1.488(6) . ? C19 C20 1.519(6) . ? O21 C21 1.394(5) . ? C21 C26 1.362(6) . ? C21 C22 1.368(6) . ? C22 C23 1.376(7) . ? C23 C24 1.369(8) . ? C24 C25 1.364(7) . ? C25 C26 1.372(6) . ? O27 C27 1.391(5) . ? C27 C28 1.360(5) . ? C27 C32 1.372(6) . ? C28 C29 1.381(6) . ? C29 C30 1.349(6) . ? C30 C31 1.355(7) . ? C31 C32 1.379(7) . ? 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 S3 Te1 S1 89.97(4) . . ? P1 S1 Te1 103.72(5) . . ? N1 P1 C3 109.0(2) . . ? N1 P1 C1 111.6(2) . . ? C3 P1 C1 105.8(2) . . ? N1 P1 S1 117.57(12) . . ? C3 P1 S1 110.6(2) . . ? C1 P1 S1 101.4(2) . . ? P2 N1 P1 142.2(2) . . ? N1 P2 O5 111.9(2) . . ? N1 P2 O11 106.5(2) . . ? O5 P2 O11 98.4(2) . . ? N1 P2 S2 120.98(13) . . ? O5 P2 S2 104.61(11) . . ? O11 P2 S2 112.19(11) . . ? C2 C1 P1 116.6(4) . . ? C4 C3 P1 117.6(4) . . ? C5 O5 P2 123.4(2) . . ? C6 C5 C10 121.6(4) . . ? C6 C5 O5 118.4(4) . . ? C10 C5 O5 119.8(4) . . ? C5 C6 C7 119.6(5) . . ? C8 C7 C6 119.8(5) . . ? C7 C8 C9 120.4(5) . . ? C8 C9 C10 120.4(5) . . ? C5 C10 C9 118.1(5) . . ? C11 O11 P2 120.5(2) . . ? C12 C11 C16 122.1(5) . . ? C12 C11 O11 119.9(5) . . ? C16 C11 O11 118.0(5) . . ? C11 C12 C13 118.1(6) . . ? C14 C13 C12 120.7(8) . . ? C15 C14 C13 120.2(9) . . ? C14 C15 C16 120.2(8) . . ? C11 C16 C15 118.7(6) . . ? P3 S3 Te1 96.42(5) . . ? N3 P3 C19 111.0(2) . . ? N3 P3 C17 108.4(2) . . ? C19 P3 C17 107.4(2) . . ? N3 P3 S3 116.61(13) . . ? C19 P3 S3 104.9(2) . . ? C17 P3 S3 108.1(2) . . ? P3 N3 P4 138.3(2) . . ? N3 P4 O27 106.5(2) . . ? N3 P4 O21 106.9(2) . . ? O27 P4 O21 99.0(2) . . ? N3 P4 S4 120.05(13) . . ? O27 P4 S4 110.91(13) . . ? O21 P4 S4 111.31(12) . . ? C18 C17 P3 114.6(3) . . ? C20 C19 P3 114.5(3) . . ? C21 O21 P4 121.3(2) . . ? C26 C21 C22 120.1(5) . . ? C26 C21 O21 121.2(4) . . ? C22 C21 O21 118.6(4) . . ? C21 C22 C23 119.9(5) . . ? C22 C23 C24 119.7(6) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 119.9(5) . . ? C21 C26 C25 120.1(5) . . ? C27 O27 P4 125.2(2) . . ? C28 C27 C32 120.6(4) . . ? C28 C27 O27 119.7(4) . . ? C32 C27 O27 119.7(4) . . ? C27 C28 C29 118.8(4) . . ? C30 C29 C28 120.8(4) . . ? C29 C30 C31 120.5(5) . . ? C30 C31 C32 119.6(5) . . ? C27 C32 C31 119.6(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 S3 Te1 S1 P1 118.94(6) . . . . ? Te1 S1 P1 N1 40.7(2) . . . . ? Te1 S1 P1 C3 -85.5(2) . . . . ? Te1 S1 P1 C1 162.6(2) . . . . ? C3 P1 N1 P2 141.8(4) . . . . ? C1 P1 N1 P2 -101.6(4) . . . . ? S1 P1 N1 P2 14.9(4) . . . . ? P1 N1 P2 O5 107.9(3) . . . . ? P1 N1 P2 O11 -145.6(3) . . . . ? P1 N1 P2 S2 -16.1(4) . . . . ? N1 P1 C1 C2 -61.6(4) . . . . ? C3 P1 C1 C2 56.9(4) . . . . ? S1 P1 C1 C2 172.4(4) . . . . ? N1 P1 C3 C4 -69.7(5) . . . . ? C1 P1 C3 C4 170.1(5) . . . . ? S1 P1 C3 C4 61.1(5) . . . . ? N1 P2 O5 C5 41.3(4) . . . . ? O11 P2 O5 C5 -70.3(3) . . . . ? S2 P2 O5 C5 174.1(3) . . . . ? P2 O5 C5 C6 -100.6(4) . . . . ? P2 O5 C5 C10 84.4(5) . . . . ? C10 C5 C6 C7 0.0(7) . . . . ? O5 C5 C6 C7 -174.8(4) . . . . ? C5 C6 C7 C8 -1.2(7) . . . . ? C6 C7 C8 C9 1.9(8) . . . . ? C7 C8 C9 C10 -1.4(8) . . . . ? C6 C5 C10 C9 0.5(7) . . . . ? O5 C5 C10 C9 175.3(4) . . . . ? C8 C9 C10 C5 0.2(8) . . . . ? N1 P2 O11 C11 50.4(3) . . . . ? O5 P2 O11 C11 166.3(3) . . . . ? S2 P2 O11 C11 -84.1(3) . . . . ? P2 O11 C11 C12 82.9(4) . . . . ? P2 O11 C11 C16 -99.2(4) . . . . ? C16 C11 C12 C13 0.6(7) . . . . ? O11 C11 C12 C13 178.5(4) . . . . ? C11 C12 C13 C14 0.2(9) . . . . ? C12 C13 C14 C15 -0.8(12) . . . . ? C13 C14 C15 C16 0.7(12) . . . . ? C12 C11 C16 C15 -0.7(7) . . . . ? O11 C11 C16 C15 -178.7(4) . . . . ? C14 C15 C16 C11 0.1(9) . . . . ? S1 Te1 S3 P3 104.43(5) . . . . ? Te1 S3 P3 N3 50.4(2) . . . . ? Te1 S3 P3 C19 173.64(15) . . . . ? Te1 S3 P3 C17 -72.0(2) . . . . ? C19 P3 N3 P4 -101.2(3) . . . . ? C17 P3 N3 P4 141.0(3) . . . . ? S3 P3 N3 P4 18.8(4) . . . . ? P3 N3 P4 O27 94.4(3) . . . . ? P3 N3 P4 O21 -160.4(3) . . . . ? P3 N3 P4 S4 -32.5(4) . . . . ? N3 P3 C17 C18 50.3(4) . . . . ? C19 P3 C17 C18 -69.7(4) . . . . ? S3 P3 C17 C18 177.6(3) . . . . ? N3 P3 C19 C20 63.3(4) . . . . ? C17 P3 C19 C20 -178.3(3) . . . . ? S3 P3 C19 C20 -63.4(3) . . . . ? N3 P4 O21 C21 56.7(3) . . . . ? O27 P4 O21 C21 167.1(3) . . . . ? S4 P4 O21 C21 -76.2(3) . . . . ? P4 O21 C21 C26 83.5(4) . . . . ? P4 O21 C21 C22 -99.3(4) . . . . ? C26 C21 C22 C23 0.2(7) . . . . ? O21 C21 C22 C23 -177.1(5) . . . . ? C21 C22 C23 C24 0.0(9) . . . . ? C22 C23 C24 C25 -0.3(9) . . . . ? C23 C24 C25 C26 0.3(9) . . . . ? C22 C21 C26 C25 -0.2(7) . . . . ? O21 C21 C26 C25 177.1(4) . . . . ? C24 C25 C26 C21 -0.1(7) . . . . ? N3 P4 O27 C27 -173.9(3) . . . . ? O21 P4 O27 C27 75.3(3) . . . . ? S4 P4 O27 C27 -41.7(3) . . . . ? P4 O27 C27 C28 -93.0(4) . . . . ? P4 O27 C27 C32 90.3(5) . . . . ? C32 C27 C28 C29 -0.9(6) . . . . ? O27 C27 C28 C29 -177.6(4) . . . . ? C27 C28 C29 C30 0.1(7) . . . . ? C28 C29 C30 C31 0.8(8) . . . . ? C29 C30 C31 C32 -0.9(8) . . . . ? C28 C27 C32 C31 0.8(7) . . . . ? O27 C27 C32 C31 177.5(4) . . . . ? C30 C31 C32 C27 0.1(8) . . . . ? _refine_diff_density_max 0.337 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.054 #--- data_4 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C36 H48 N2 P4 S4 Te' _chemical_formula_structural 'C36 H48 N2 P4 S4 Te' _chemical_formula_analytical 'C36 H48 N2 P4 S4 Te' _chemical_formula_sum 'C36 H48 N2 P4 S4 Te' _chemical_formula_weight 888.48 _chemical_melting_point - _chemical_compound_source - 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7171(7) _cell_length_b 11.9430(8) _cell_length_c 18.4530(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.162(2) _cell_angle_gamma 90.00 _cell_volume 2076.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method - _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.673396 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 8677 _diffrn_reflns_av_R_equivalents 0.1445 _diffrn_reflns_av_sigmaI/netI 0.1787 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2974 _reflns_number_observed 1530 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2924 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_obs 0.0474 _refine_ls_wR_factor_all 0.1051 _refine_ls_wR_factor_obs 0.0765 _refine_ls_goodness_of_fit_all 0.777 _refine_ls_goodness_of_fit_obs 0.892 _refine_ls_restrained_S_all 0.859 _refine_ls_restrained_S_obs 0.892 _refine_ls_shift/esd_max -1.572 _refine_ls_shift/esd_mean 0.007 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.5000 0.0000 0.0000 0.0425(3) Uani 1 d S . S1 S 0.7434(2) 0.04072(14) 0.10148(12) 0.0489(6) Uani 1 d . . P1 P 0.7521(2) 0.20393(14) 0.07375(11) 0.0367(5) Uani 1 d . . N1 N 0.6184(5) 0.2825(4) 0.0697(3) 0.042(2) Uani 1 d . . P2 P 0.4631(2) 0.27445(14) 0.08340(12) 0.0400(5) Uani 1 d . . S2 S 0.3763(2) 0.12085(14) 0.08920(13) 0.0551(6) Uani 1 d . . C1 C 0.8020(6) 0.2175(5) -0.0151(4) 0.032(2) Uani 1 d . . C2 C 0.7790(7) 0.3169(6) -0.0521(4) 0.046(2) Uani 1 d . . H2A H 0.7307(7) 0.3737(6) -0.0343(4) 0.055 Uiso 1 calc R . C3 C 0.8265(8) 0.3342(6) -0.1155(5) 0.060(2) Uani 1 d . . H3A H 0.8095(8) 0.4021(6) -0.1407(5) 0.072 Uiso 1 calc R . C4 C 0.8995(7) 0.2503(8) -0.1415(5) 0.061(2) Uani 1 d . . H4A H 0.9320(7) 0.2612(8) -0.1844(5) 0.073 Uiso 1 calc R . C5 C 0.9233(8) 0.1523(7) -0.1041(5) 0.066(3) Uani 1 d . . H5A H 0.9729(8) 0.0961(7) -0.1217(5) 0.080 Uiso 1 calc R . C6 C 0.8760(7) 0.1332(6) -0.0405(5) 0.053(2) Uani 1 d . . H6A H 0.8935(7) 0.0653(6) -0.0153(5) 0.063 Uiso 1 calc R . C7 C 0.9031(6) 0.2611(6) 0.1405(4) 0.039(2) Uani 1 d . . C8 C 0.9059(8) 0.3719(6) 0.1635(5) 0.055(2) Uani 1 d . . H8A H 0.8274(8) 0.4169(6) 0.1444(5) 0.065 Uiso 1 calc R . C9 C 1.0215(9) 0.4174(7) 0.2136(5) 0.069(3) Uani 1 d . . H9A H 1.0201(9) 0.4917(7) 0.2284(5) 0.083 Uiso 1 calc R . C10 C 1.1382(9) 0.3520(9) 0.2414(5) 0.080(3) Uani 1 d . . H10A H 1.2165(9) 0.3822(9) 0.2751(5) 0.095 Uiso 1 calc R . C11 C 1.1403(7) 0.2406(8) 0.2194(5) 0.066(2) Uani 1 d . . H11A H 1.2192(7) 0.1959(8) 0.2386(5) 0.079 Uiso 1 calc R . C12 C 1.0242(7) 0.1976(6) 0.1691(4) 0.051(2) Uani 1 d . . H12A H 1.0266(7) 0.1237(6) 0.1536(4) 0.061 Uiso 1 calc R . C13 C 0.3470(6) 0.3536(5) 0.0105(5) 0.047(2) Uani 1 d . . H13A H 0.3884(6) 0.4284(5) 0.0106(5) 0.056 Uiso 1 calc R . C14 C 0.3399(8) 0.3017(6) -0.0665(5) 0.070(3) Uani 1 d . . H14A H 0.4343(8) 0.2923(6) -0.0730(5) 0.105 Uiso 1 calc R . H14B H 0.2872(8) 0.3503(6) -0.1049(5) 0.105 Uiso 1 calc R . H14C H 0.2937(8) 0.2302(6) -0.0699(5) 0.105 Uiso 1 calc R . C15 C 0.1973(7) 0.3687(6) 0.0210(5) 0.067(3) Uani 1 d . . H15A H 0.2021(7) 0.4011(6) 0.0691(5) 0.101 Uiso 1 calc R . H15B H 0.1510(7) 0.2972(6) 0.0177(5) 0.101 Uiso 1 calc R . H15C H 0.1445(7) 0.4174(6) -0.0173(5) 0.101 Uiso 1 calc R . C16 C 0.4632(7) 0.3456(6) 0.1702(5) 0.050(2) Uani 1 d . . H16A H 0.3651(7) 0.3447(6) 0.1752(5) 0.060 Uiso 1 calc R . C17 C 0.5514(8) 0.2813(7) 0.2366(5) 0.077(3) Uani 1 d . . H17A H 0.5206(8) 0.2047(7) 0.2340(5) 0.115 Uiso 1 calc R . H17B H 0.5395(8) 0.3143(7) 0.2821(5) 0.115 Uiso 1 calc R . H17C H 0.6496(8) 0.2843(7) 0.2357(5) 0.115 Uiso 1 calc R . C18 C 0.5072(8) 0.4667(6) 0.1716(5) 0.073(3) Uani 1 d . . H18A H 0.4496(8) 0.5047(6) 0.1290(5) 0.109 Uiso 1 calc R . H18B H 0.6052(8) 0.4713(6) 0.1701(5) 0.109 Uiso 1 calc R . H18C H 0.4950(8) 0.5013(6) 0.2165(5) 0.109 Uiso 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 0.0388(4) 0.0326(4) 0.0592(6) 0.0019(4) 0.0182(3) -0.0021(4) S1 0.0385(10) 0.0408(11) 0.064(2) 0.0101(10) 0.0071(10) -0.0016(8) P1 0.0337(10) 0.0357(11) 0.044(2) -0.0004(10) 0.0161(9) -0.0010(8) N1 0.034(3) 0.039(3) 0.060(5) 0.001(3) 0.023(3) 0.002(3) P2 0.0358(10) 0.0387(11) 0.051(2) -0.0016(10) 0.0211(10) -0.0010(8) S2 0.0510(12) 0.0451(12) 0.082(2) -0.0007(11) 0.0408(12) -0.0048(9) C1 0.027(4) 0.033(4) 0.036(5) -0.009(4) 0.010(3) 0.003(3) C2 0.059(5) 0.042(5) 0.041(6) 0.002(4) 0.021(4) 0.015(4) C3 0.077(6) 0.065(6) 0.045(7) 0.009(5) 0.029(5) 0.012(5) C4 0.052(5) 0.087(6) 0.051(7) -0.009(6) 0.027(4) -0.002(5) C5 0.081(6) 0.066(6) 0.064(8) -0.012(5) 0.041(5) 0.022(5) C6 0.065(5) 0.049(5) 0.052(7) 0.002(4) 0.027(5) 0.011(4) C7 0.037(4) 0.044(5) 0.040(6) -0.006(4) 0.019(4) -0.009(3) C8 0.050(5) 0.062(5) 0.059(7) -0.032(5) 0.027(4) -0.017(4) C9 0.071(6) 0.073(6) 0.078(8) -0.035(6) 0.046(6) -0.027(5) C10 0.069(7) 0.139(10) 0.047(7) -0.042(7) 0.045(6) -0.054(6) C11 0.043(5) 0.104(7) 0.052(7) -0.012(6) 0.013(4) -0.014(5) C12 0.046(5) 0.062(5) 0.044(6) -0.004(4) 0.012(4) -0.008(4) C13 0.034(4) 0.046(4) 0.060(7) 0.000(4) 0.011(4) -0.003(3) C14 0.077(6) 0.080(6) 0.053(7) 0.021(5) 0.013(5) 0.006(5) C15 0.036(4) 0.084(6) 0.080(8) 0.004(5) 0.012(4) 0.008(4) C16 0.036(4) 0.070(6) 0.053(7) -0.020(5) 0.027(4) -0.004(4) C17 0.083(6) 0.094(7) 0.053(7) 0.003(6) 0.015(5) 0.001(5) C18 0.078(6) 0.064(7) 0.080(8) -0.035(5) 0.026(5) -0.001(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 S1 2.678(2) 3_655 ? Te1 S1 2.678(2) . ? Te1 S2 2.684(2) . ? Te1 S2 2.684(2) 3_655 ? S1 P1 2.022(2) . ? P1 N1 1.589(5) . ? P1 C7 1.804(7) . ? P1 C1 1.827(7) . ? N1 P2 1.593(5) . ? P2 C13 1.798(7) . ? P2 C16 1.813(7) . ? P2 S2 2.032(2) . ? C1 C2 1.361(8) . ? C1 C6 1.383(8) . ? C2 C3 1.374(10) . ? C3 C4 1.381(9) . ? C4 C5 1.349(10) . ? C5 C6 1.380(11) . ? C7 C8 1.387(8) . ? C7 C12 1.391(8) . ? C8 C9 1.380(9) . ? C9 C10 1.368(11) . ? C10 C11 1.393(10) . ? C11 C12 1.373(9) . ? C13 C15 1.525(8) . ? C13 C14 1.536(10) . ? C16 C18 1.507(8) . ? C16 C17 1.521(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Te1 S1 179.998(1) 3_655 . ? S1 Te1 S2 94.31(6) 3_655 . ? S1 Te1 S2 85.69(6) . . ? S1 Te1 S2 85.69(6) 3_655 3_655 ? S1 Te1 S2 94.31(6) . 3_655 ? S2 Te1 S2 180.0 . 3_655 ? P1 S1 Te1 94.72(9) . . ? N1 P1 C7 109.1(3) . . ? N1 P1 C1 107.4(3) . . ? C7 P1 C1 103.2(3) . . ? N1 P1 S1 119.8(2) . . ? C7 P1 S1 105.6(2) . . ? C1 P1 S1 110.4(2) . . ? P1 N1 P2 138.8(3) . . ? N1 P2 C13 107.2(3) . . ? N1 P2 C16 108.4(3) . . ? C13 P2 C16 106.2(4) . . ? N1 P2 S2 118.9(2) . . ? C13 P2 S2 108.8(2) . . ? C16 P2 S2 106.7(3) . . ? P2 S2 Te1 101.51(9) . . ? C2 C1 C6 120.0(7) . . ? C2 C1 P1 118.7(5) . . ? C6 C1 P1 120.9(6) . . ? C1 C2 C3 120.7(7) . . ? C2 C3 C4 119.7(8) . . ? C5 C4 C3 119.3(8) . . ? C4 C5 C6 121.8(7) . . ? C5 C6 C1 118.5(7) . . ? C8 C7 C12 116.9(7) . . ? C8 C7 P1 121.5(6) . . ? C12 C7 P1 121.6(5) . . ? C9 C8 C7 122.2(8) . . ? C10 C9 C8 119.4(8) . . ? C9 C10 C11 120.4(8) . . ? C12 C11 C10 119.1(8) . . ? C11 C12 C7 122.1(7) . . ? C15 C13 C14 109.7(6) . . ? C15 C13 P2 114.2(6) . . ? C14 C13 P2 111.0(5) . . ? C18 C16 C17 111.7(6) . . ? C18 C16 P2 113.8(5) . . ? C17 C16 P2 110.7(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 S1 Te1 S1 P1 -90.4(12) 3_655 . . . ? S2 Te1 S1 P1 -72.16(9) . . . . ? S2 Te1 S1 P1 107.84(9) 3_655 . . . ? Te1 S1 P1 N1 51.5(3) . . . . ? Te1 S1 P1 C7 175.0(2) . . . . ? Te1 S1 P1 C1 -74.0(2) . . . . ? C7 P1 N1 P2 -120.2(6) . . . . ? C1 P1 N1 P2 128.6(6) . . . . ? S1 P1 N1 P2 1.7(7) . . . . ? P1 N1 P2 C13 -139.6(6) . . . . ? P1 N1 P2 C16 106.2(6) . . . . ? P1 N1 P2 S2 -15.8(7) . . . . ? N1 P2 S2 Te1 -29.7(3) . . . . ? C13 P2 S2 Te1 93.2(3) . . . . ? C16 P2 S2 Te1 -152.5(2) . . . . ? S1 Te1 S2 P2 -115.38(10) 3_655 . . . ? S1 Te1 S2 P2 64.62(10) . . . . ? S2 Te1 S2 P2 -6.9(242) 3_655 . . . ? N1 P1 C1 C2 31.4(6) . . . . ? C7 P1 C1 C2 -83.8(6) . . . . ? S1 P1 C1 C2 163.7(5) . . . . ? N1 P1 C1 C6 -155.8(5) . . . . ? C7 P1 C1 C6 89.0(6) . . . . ? S1 P1 C1 C6 -23.5(6) . . . . ? C6 C1 C2 C3 1.2(11) . . . . ? P1 C1 C2 C3 174.0(6) . . . . ? C1 C2 C3 C4 -0.7(12) . . . . ? C2 C3 C4 C5 -0.1(12) . . . . ? C3 C4 C5 C6 0.3(13) . . . . ? C4 C5 C6 C1 0.2(13) . . . . ? C2 C1 C6 C5 -0.9(11) . . . . ? P1 C1 C6 C5 -173.6(6) . . . . ? N1 P1 C7 C8 -18.4(7) . . . . ? C1 P1 C7 C8 95.6(6) . . . . ? S1 P1 C7 C8 -148.4(5) . . . . ? N1 P1 C7 C12 164.1(5) . . . . ? C1 P1 C7 C12 -81.9(6) . . . . ? S1 P1 C7 C12 34.1(6) . . . . ? C12 C7 C8 C9 -1.4(11) . . . . ? P1 C7 C8 C9 -179.0(6) . . . . ? C7 C8 C9 C10 0.6(12) . . . . ? C8 C9 C10 C11 -0.2(13) . . . . ? C9 C10 C11 C12 0.5(12) . . . . ? C10 C11 C12 C7 -1.4(12) . . . . ? C8 C7 C12 C11 1.8(11) . . . . ? P1 C7 C12 C11 179.4(6) . . . . ? N1 P2 C13 C15 -171.8(5) . . . . ? C16 P2 C13 C15 -56.1(6) . . . . ? S2 P2 C13 C15 58.4(6) . . . . ? N1 P2 C13 C14 63.5(6) . . . . ? C16 P2 C13 C14 179.2(5) . . . . ? S2 P2 C13 C14 -66.3(5) . . . . ? N1 P2 C16 C18 58.1(6) . . . . ? C13 P2 C16 C18 -56.8(6) . . . . ? S2 P2 C16 C18 -172.7(4) . . . . ? N1 P2 C16 C17 -68.7(6) . . . . ? C13 P2 C16 C17 176.4(5) . . . . ? S2 P2 C16 C17 60.5(5) . . . . ? _refine_diff_density_max 0.515 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.131 #--- data_7 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C24 H56 N2 P4 Se4 Te' _chemical_formula_structural 'C24 H56 N2 P4 Se4 Te' _chemical_formula_analytical 'C24 H56 N2 P4 Se4 Te' _chemical_formula_sum 'C24 H56 N2 P4 Se4 Te' _chemical_formula_weight 940.03 _chemical_melting_point - _chemical_compound_source - 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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4104(7) _cell_length_b 14.7541(11) _cell_length_c 12.1815(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.739(2) _cell_angle_gamma 90.00 _cell_volume 1849.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 82 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max .12 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .13 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method - _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 4.931 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.738585 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 7968 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2660 _reflns_number_observed 1955 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00044(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2610 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_obs 0.0249 _refine_ls_wR_factor_all 0.0525 _refine_ls_wR_factor_obs 0.0425 _refine_ls_goodness_of_fit_all 0.911 _refine_ls_goodness_of_fit_obs 0.980 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 0.980 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.0000 0.5000 -0.5000 0.03787(13) Uani 1 d S . Se1 Se -0.00151(4) 0.33858(3) -0.37697(3) 0.04512(14) Uani 1 d . . P1 P 0.12422(9) 0.38335(7) -0.22563(8) 0.0326(3) Uani 1 d . . N1 N 0.2418(3) 0.4487(2) -0.2365(2) 0.0383(8) Uani 1 d . . P2 P 0.31346(9) 0.50523(7) -0.32009(8) 0.0328(2) Uani 1 d . . Se2 Se 0.26593(4) 0.47151(3) -0.49657(3) 0.04568(14) Uani 1 d . . C1 C 0.0227(3) 0.4372(3) -0.1342(3) 0.0378(10) Uani 1 d . . H1A H 0.0801(3) 0.4559(3) -0.0667(3) 0.045 Uiso 1 calc R . C2 C -0.0431(4) 0.5226(3) -0.1870(3) 0.0557(12) Uani 1 d . . H2A H 0.0215(4) 0.5625(3) -0.2086(3) 0.084 Uiso 1 calc R . H2B H -0.0881(4) 0.5527(3) -0.1342(3) 0.084 Uiso 1 calc R . H2C H -0.1039(4) 0.5062(3) -0.2512(3) 0.084 Uiso 1 calc R . C3 C -0.0790(4) 0.3723(3) -0.0987(4) 0.0636(13) Uani 1 d . . H3A H -0.0364(4) 0.3191(3) -0.0657(4) 0.095 Uiso 1 calc R . H3B H -0.1400(4) 0.3553(3) -0.1626(4) 0.095 Uiso 1 calc R . H3C H -0.1242(4) 0.4020(3) -0.0457(4) 0.095 Uiso 1 calc R . C4 C 0.1885(4) 0.2796(3) -0.1542(3) 0.0416(10) Uani 1 d . . H4A H 0.1144(4) 0.2442(3) -0.1372(3) 0.050 Uiso 1 calc R . C5 C 0.2735(5) 0.3038(3) -0.0432(4) 0.0701(15) Uani 1 d . . H5A H 0.2242(5) 0.3405(3) 0.0005(4) 0.105 Uiso 1 calc R . H5B H 0.3486(5) 0.3368(3) -0.0575(4) 0.105 Uiso 1 calc R . H5C H 0.3005(5) 0.2492(3) -0.0035(4) 0.105 Uiso 1 calc R . C6 C 0.2615(4) 0.2217(3) -0.2265(4) 0.0585(13) Uani 1 d . . H6A H 0.2059(4) 0.2080(3) -0.2947(4) 0.088 Uiso 1 calc R . H6B H 0.2885(4) 0.1664(3) -0.1883(4) 0.088 Uiso 1 calc R . H6C H 0.3366(4) 0.2541(3) -0.2423(4) 0.088 Uiso 1 calc R . C7 C 0.2759(4) 0.6264(3) -0.3062(3) 0.0435(10) Uani 1 d . . H7A H 0.1834(4) 0.6328(3) -0.3357(3) 0.052 Uiso 1 calc R . C8 C 0.2904(5) 0.6593(3) -0.1858(4) 0.0734(15) Uani 1 d . . H8A H 0.2438(5) 0.6193(3) -0.1437(4) 0.110 Uiso 1 calc R . H8B H 0.2558(5) 0.7195(3) -0.1840(4) 0.110 Uiso 1 calc R . H8C H 0.3807(5) 0.6597(3) -0.1543(4) 0.110 Uiso 1 calc R . C9 C 0.3476(4) 0.6865(3) -0.3794(4) 0.0652(14) Uani 1 d . . H9A H 0.3353(4) 0.6629(3) -0.4537(4) 0.098 Uiso 1 calc R . H9B H 0.4386(4) 0.6873(3) -0.3504(4) 0.098 Uiso 1 calc R . H9C H 0.3137(4) 0.7471(3) -0.3801(4) 0.098 Uiso 1 calc R . C10 C 0.4897(4) 0.4884(3) -0.2850(4) 0.0452(11) Uani 1 d . . H10A H 0.5305(4) 0.5310(3) -0.3310(4) 0.054 Uiso 1 calc R . C11 C 0.5427(5) 0.5110(4) -0.1652(4) 0.094(2) Uani 1 d . . H11A H 0.5155(5) 0.5709(4) -0.1482(4) 0.141 Uiso 1 calc R . H11B H 0.6359(5) 0.5083(4) -0.1545(4) 0.141 Uiso 1 calc R . H11C H 0.5101(5) 0.4680(4) -0.1170(4) 0.141 Uiso 1 calc R . C12 C 0.5298(4) 0.3952(3) -0.3155(4) 0.0701(15) Uani 1 d . . H12A H 0.4950(4) 0.3830(3) -0.3916(4) 0.105 Uiso 1 calc R . H12B H 0.4971(4) 0.3514(3) -0.2686(4) 0.105 Uiso 1 calc R . H12C H 0.6229(4) 0.3917(3) -0.3058(4) 0.105 Uiso 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 0.0417(2) 0.0487(3) 0.0223(2) 0.0000(2) 0.0018(2) -0.0074(2) Se1 0.0542(3) 0.0471(3) 0.0317(3) 0.0009(2) -0.0013(2) -0.0145(2) P1 0.0378(6) 0.0361(6) 0.0240(6) 0.0013(5) 0.0050(5) -0.0032(5) N1 0.043(2) 0.044(2) 0.028(2) 0.003(2) 0.0043(15) -0.011(2) P2 0.0339(6) 0.0340(6) 0.0306(6) -0.0002(5) 0.0057(5) -0.0024(5) Se2 0.0492(3) 0.0588(3) 0.0309(2) -0.0043(2) 0.0117(2) -0.0052(2) C1 0.044(2) 0.045(3) 0.024(2) -0.003(2) 0.006(2) -0.004(2) C2 0.064(3) 0.062(3) 0.046(3) -0.001(2) 0.021(2) 0.017(2) C3 0.060(3) 0.079(3) 0.058(3) 0.005(3) 0.030(2) -0.010(3) C4 0.048(3) 0.037(2) 0.040(3) 0.008(2) 0.010(2) -0.002(2) C5 0.096(4) 0.062(3) 0.044(3) 0.008(2) -0.018(3) 0.018(3) C6 0.071(3) 0.045(3) 0.060(3) 0.004(2) 0.013(3) 0.014(2) C7 0.040(2) 0.038(2) 0.052(3) -0.003(2) 0.006(2) 0.000(2) C8 0.101(4) 0.052(3) 0.067(4) -0.029(3) 0.013(3) 0.000(3) C9 0.073(3) 0.041(3) 0.083(4) 0.009(3) 0.019(3) -0.007(2) C10 0.034(2) 0.048(3) 0.055(3) 0.005(2) 0.011(2) 0.000(2) C11 0.051(3) 0.146(6) 0.074(4) -0.021(4) -0.027(3) 0.019(3) C12 0.050(3) 0.064(3) 0.097(4) 0.019(3) 0.013(3) 0.013(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 Te1 Se2 2.7941(4) 3_564 ? Te1 Se2 2.7942(4) . ? Te1 Se1 2.8152(4) 3_564 ? Te1 Se1 2.8152(4) . ? Se1 P1 2.1944(10) . ? P1 N1 1.579(3) . ? P1 C1 1.829(4) . ? P1 C4 1.836(4) . ? N1 P2 1.588(3) . ? P2 C10 1.837(4) . ? P2 C7 1.843(4) . ? P2 Se2 2.1888(11) . ? C1 C2 1.528(5) . ? C1 C3 1.537(5) . ? C4 C6 1.512(5) . ? C4 C5 1.541(5) . ? C7 C9 1.530(5) . ? C7 C8 1.530(6) . ? C10 C12 1.500(5) . ? C10 C11 1.517(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se2 Te1 Se2 180.0 3_564 . ? Se2 Te1 Se1 87.160(13) 3_564 3_564 ? Se2 Te1 Se1 92.840(12) . 3_564 ? Se2 Te1 Se1 92.840(12) 3_564 . ? Se2 Te1 Se1 87.159(12) . . ? Se1 Te1 Se1 180.0 3_564 . ? P1 Se1 Te1 98.15(3) . . ? N1 P1 C1 108.2(2) . . ? N1 P1 C4 108.5(2) . . ? C1 P1 C4 106.0(2) . . ? N1 P1 Se1 118.98(12) . . ? C1 P1 Se1 108.44(13) . . ? C4 P1 Se1 105.96(13) . . ? P1 N1 P2 145.1(2) . . ? N1 P2 C10 109.3(2) . . ? N1 P2 C7 108.9(2) . . ? C10 P2 C7 109.1(2) . . ? N1 P2 Se2 116.90(12) . . ? C10 P2 Se2 105.47(14) . . ? C7 P2 Se2 106.95(14) . . ? P2 Se2 Te1 93.22(3) . . ? C2 C1 C3 110.3(3) . . ? C2 C1 P1 111.4(3) . . ? C3 C1 P1 112.8(3) . . ? C6 C4 C5 111.7(3) . . ? C6 C4 P1 112.0(3) . . ? C5 C4 P1 110.0(3) . . ? C9 C7 C8 112.9(3) . . ? C9 C7 P2 112.3(3) . . ? C8 C7 P2 113.9(3) . . ? C12 C10 C11 111.4(4) . . ? C12 C10 P2 111.8(3) . . ? C11 C10 P2 113.5(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 Se2 Te1 Se1 P1 -115.36(3) 3_564 . . . ? Se2 Te1 Se1 P1 64.64(3) . . . . ? Se1 Te1 Se1 P1 -2.1(24) 3_564 . . . ? Te1 Se1 P1 N1 -36.45(14) . . . . ? Te1 Se1 P1 C1 87.71(13) . . . . ? Te1 Se1 P1 C4 -158.83(13) . . . . ? C1 P1 N1 P2 -120.7(4) . . . . ? C4 P1 N1 P2 124.7(4) . . . . ? Se1 P1 N1 P2 3.6(4) . . . . ? P1 N1 P2 C10 -135.8(4) . . . . ? P1 N1 P2 C7 105.1(4) . . . . ? P1 N1 P2 Se2 -16.2(4) . . . . ? N1 P2 Se2 Te1 56.01(13) . . . . ? C10 P2 Se2 Te1 177.63(14) . . . . ? C7 P2 Se2 Te1 -66.28(13) . . . . ? Se2 Te1 Se2 P2 -140.6(47) 3_564 . . . ? Se1 Te1 Se2 P2 108.06(3) 3_564 . . . ? Se1 Te1 Se2 P2 -71.94(3) . . . . ? N1 P1 C1 C2 66.8(3) . . . . ? C4 P1 C1 C2 -177.0(3) . . . . ? Se1 P1 C1 C2 -63.6(3) . . . . ? N1 P1 C1 C3 -168.5(3) . . . . ? C4 P1 C1 C3 -52.3(3) . . . . ? Se1 P1 C1 C3 61.1(3) . . . . ? N1 P1 C4 C6 -70.9(3) . . . . ? C1 P1 C4 C6 173.0(3) . . . . ? Se1 P1 C4 C6 57.9(3) . . . . ? N1 P1 C4 C5 53.9(3) . . . . ? C1 P1 C4 C5 -62.2(3) . . . . ? Se1 P1 C4 C5 -177.3(3) . . . . ? N1 P2 C7 C9 176.8(3) . . . . ? C10 P2 C7 C9 57.6(3) . . . . ? Se2 P2 C7 C9 -56.0(3) . . . . ? N1 P2 C7 C8 46.9(3) . . . . ? C10 P2 C7 C8 -72.3(3) . . . . ? Se2 P2 C7 C8 174.0(3) . . . . ? N1 P2 C10 C12 72.1(4) . . . . ? C7 P2 C10 C12 -169.0(3) . . . . ? Se2 P2 C10 C12 -54.4(3) . . . . ? N1 P2 C10 C11 -55.0(4) . . . . ? C7 P2 C10 C11 63.9(4) . . . . ? Se2 P2 C10 C11 178.5(3) . . . . ? _refine_diff_density_max 0.278 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.065 #--- data_8 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C19 H35 Cl2 N O P2 S2 Te' _chemical_formula_structural 'C19 H35 Cl2 N O P2 S2 Te' _chemical_formula_analytical 'C19 H35 Cl2 N O P2 S2 Te' _chemical_formula_sum 'C19 H35 Cl2 N O P2 S2 Te' _chemical_formula_weight 618.04 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1666(3) _cell_length_b 11.1730(4) _cell_length_c 13.5041(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.1440(10) _cell_angle_gamma 90.00 _cell_volume 1361.45(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .15 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .4 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method - _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.571 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.663199 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 5986 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.30 _reflns_number_total 3692 _reflns_number_observed 3599 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SMART/SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.2999P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 3642 _refine_ls_number_parameters 254 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_obs 0.0232 _refine_ls_wR_factor_all 0.0758 _refine_ls_wR_factor_obs 0.0599 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.052 _refine_ls_restrained_S_all 1.323 _refine_ls_restrained_S_obs 1.052 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te 0.14770(2) 0.85937(2) 0.809046(15) 0.03688(10) Uani 1 d . . S1 S 0.36546(10) 0.71599(9) 0.87737(8) 0.0442(2) Uani 1 d . . P1 P 0.24239(10) 0.57071(9) 0.90843(8) 0.0402(2) Uani 1 d . . Cl1 Cl -0.05668(13) 1.00348(12) 0.73178(9) 0.0646(3) Uani 1 d . . N1 N 0.0874(3) 0.5541(3) 0.8372(3) 0.0482(8) Uani 1 d . . C1 C 0.2064(5) 0.5843(5) 1.0364(3) 0.0553(11) Uani 1 d . . H1A H 0.1454(5) 0.5156(5) 1.0486(3) 0.066 Uiso 1 calc R . P2 P -0.00172(11) 0.57674(9) 0.72755(8) 0.0419(2) Uani 1 d . . S2 S 0.06948(13) 0.71846(9) 0.65343(7) 0.0501(3) Uani 1 d . . Cl2 Cl 0.23951(14) 1.00488(11) 0.94972(9) 0.0615(3) Uani 1 d . . C2 C 0.3481(6) 0.5795(8) 1.1147(4) 0.094(2) Uani 1 d . . H2A H 0.4020(6) 0.5079(8) 1.1053(4) 0.140 Uiso 1 calc R . H2B H 0.3234(6) 0.5794(8) 1.1809(4) 0.140 Uiso 1 calc R . H2C H 0.4082(6) 0.6481(8) 1.1071(4) 0.140 Uiso 1 calc R . C3 C 0.1190(7) 0.6958(6) 1.0491(4) 0.081(2) Uani 1 d . . H3A H 0.0303(7) 0.6970(6) 0.9991(4) 0.121 Uiso 1 calc R . H3B H 0.1778(7) 0.7650(6) 1.0412(4) 0.121 Uiso 1 calc R . H3C H 0.0930(7) 0.6963(6) 1.1149(4) 0.121 Uiso 1 calc R . C4 C 0.3672(5) 0.4439(4) 0.9067(4) 0.0592(12) Uani 1 d . . H4A H 0.4538(5) 0.4576(4) 0.9592(4) 0.071 Uiso 1 calc R . C5 C 0.2929(7) 0.3280(5) 0.9334(7) 0.094(2) Uani 1 d . . H5A H 0.2598(7) 0.3381(5) 0.9965(7) 0.142 Uiso 1 calc R . H5B H 0.3629(7) 0.2635(5) 0.9387(7) 0.142 Uiso 1 calc R . H5C H 0.2097(7) 0.3102(5) 0.8817(7) 0.142 Uiso 1 calc R . C6 C 0.4220(8) 0.4339(6) 0.8077(6) 0.094(2) Uani 1 d . . H6A H 0.4677(8) 0.5079(6) 0.7938(6) 0.141 Uiso 1 calc R . H6B H 0.3400(8) 0.4172(6) 0.7548(6) 0.141 Uiso 1 calc R . H6C H 0.4932(8) 0.3702(6) 0.8117(6) 0.141 Uiso 1 calc R . C7 C 0.0103(7) 0.4490(5) 0.6445(4) 0.0708(14) Uani 1 d . . H7A H 0.1166(7) 0.4328(5) 0.6504(4) 0.085 Uiso 1 calc R . C8 C -0.0552(12) 0.3352(6) 0.6846(7) 0.128(3) Uani 1 d . . H8A H -0.0172(12) 0.3269(6) 0.7552(7) 0.192 Uiso 1 calc R . H8B H -0.0278(12) 0.2665(6) 0.6494(7) 0.192 Uiso 1 calc R . H8C H -0.1612(12) 0.3416(6) 0.6741(7) 0.192 Uiso 1 calc R . C9 C -0.0444(9) 0.4673(6) 0.5347(5) 0.094(2) Uani 1 d . . H9A H -0.0011(9) 0.5388(6) 0.5129(5) 0.142 Uiso 1 calc R . H9B H -0.1503(9) 0.4751(6) 0.5227(5) 0.142 Uiso 1 calc R . H9C H -0.0169(9) 0.3999(6) 0.4979(5) 0.142 Uiso 1 calc R . C10 C -0.1952(5) 0.5981(5) 0.7411(4) 0.0637(12) Uani 1 d . . H10A H -0.2265(5) 0.5237(5) 0.7697(4) 0.076 Uiso 1 calc R . C11 C -0.2154(6) 0.6968(7) 0.8138(5) 0.087(2) Uani 1 d . . H11A H -0.1495(6) 0.6840(7) 0.8765(5) 0.131 Uiso 1 calc R . H11B H -0.3159(6) 0.6968(7) 0.8250(5) 0.131 Uiso 1 calc R . H11C H -0.1936(6) 0.7726(7) 0.7861(5) 0.131 Uiso 1 calc R . C12 C -0.2984(7) 0.6168(11) 0.6416(5) 0.133(4) Uani 1 d . . H12A H -0.2845(7) 0.5536(11) 0.5961(5) 0.200 Uiso 1 calc R . H12B H -0.2770(7) 0.6923(11) 0.6134(5) 0.200 Uiso 1 calc R . H12C H -0.3992(7) 0.6164(11) 0.6523(5) 0.200 Uiso 1 calc R . C13 C 0.2909(4) 0.9444(4) 0.7219(3) 0.0449(9) Uani 1 d . . C14 C 0.2876(6) 1.0676(4) 0.7141(4) 0.0604(12) Uani 1 d . . H14A H 0.2257(6) 1.1125(4) 0.7472(4) 0.073 Uiso 1 calc R . C15 C 0.3782(7) 1.1232(6) 0.6558(4) 0.077(2) Uani 1 d . . H15A H 0.3746(7) 1.2059(6) 0.6479(4) 0.093 Uiso 1 calc R . O16 O 0.5573(5) 1.1248(6) 0.5562(3) 0.117(2) Uani 1 d . . C16 C 0.4731(6) 1.0570(7) 0.6099(4) 0.075(2) Uani 1 d . . C17 C 0.4759(6) 0.9372(7) 0.6181(4) 0.076(2) Uani 1 d . . H17A H 0.5391(6) 0.8928(7) 0.5855(4) 0.091 Uiso 1 calc R . C18 C 0.3843(5) 0.8791(6) 0.6754(3) 0.0618(14) Uani 1 d . . H18A H 0.3872(5) 0.7962(6) 0.6816(3) 0.074 Uiso 1 calc R . C19 C 0.6618(8) 1.0663(13) 0.5099(7) 0.160(5) Uani 1 d . . H19A H 0.7122(8) 1.1238(13) 0.4751(7) 0.240 Uiso 1 calc R . H19B H 0.6128(8) 1.0088(13) 0.4626(7) 0.240 Uiso 1 calc R . H19C H 0.7324(8) 1.0262(13) 0.5599(7) 0.240 Uiso 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 0.03842(13) 0.03450(14) 0.03764(14) -0.00085(11) 0.00642(8) 0.00111(11) S1 0.0347(5) 0.0436(6) 0.0532(6) 0.0088(5) 0.0045(4) -0.0018(4) P1 0.0369(5) 0.0409(5) 0.0400(5) 0.0096(4) -0.0009(4) -0.0027(4) Cl1 0.0604(6) 0.0604(7) 0.0703(8) 0.0019(6) 0.0037(5) 0.0246(6) N1 0.040(2) 0.050(2) 0.051(2) 0.013(2) -0.0039(15) -0.0083(15) C1 0.051(2) 0.073(3) 0.041(2) 0.011(2) 0.006(2) -0.010(2) P2 0.0438(5) 0.0375(6) 0.0401(5) 0.0017(4) -0.0041(4) -0.0035(4) S2 0.0718(7) 0.0396(6) 0.0368(5) 0.0018(4) 0.0038(5) -0.0041(5) Cl2 0.0777(7) 0.0506(6) 0.0536(6) -0.0154(5) 0.0042(5) -0.0018(6) C2 0.063(3) 0.166(7) 0.045(3) 0.011(3) -0.006(2) -0.020(4) C3 0.091(4) 0.102(5) 0.056(3) -0.002(3) 0.028(3) -0.003(3) C4 0.049(2) 0.045(3) 0.077(3) 0.007(2) -0.008(2) 0.001(2) C5 0.080(4) 0.050(4) 0.144(6) 0.037(3) -0.007(4) -0.001(3) C6 0.103(5) 0.073(4) 0.109(5) -0.010(4) 0.030(4) 0.032(4) C7 0.091(4) 0.044(3) 0.073(3) -0.012(2) 0.000(3) 0.000(3) C8 0.200(9) 0.047(5) 0.120(6) 0.007(4) -0.020(5) -0.033(5) C9 0.122(5) 0.086(5) 0.071(4) -0.032(3) 0.005(3) -0.006(4) C10 0.046(2) 0.077(3) 0.064(3) 0.004(2) -0.003(2) -0.006(2) C11 0.047(3) 0.119(5) 0.098(4) -0.010(4) 0.020(3) -0.002(3) C12 0.070(4) 0.245(12) 0.073(4) -0.015(6) -0.019(3) 0.050(6) C13 0.047(2) 0.044(2) 0.043(2) 0.006(2) 0.006(2) -0.006(2) C14 0.081(3) 0.046(3) 0.055(3) 0.001(2) 0.012(2) -0.012(2) C15 0.097(4) 0.065(4) 0.065(3) 0.016(3) 0.002(3) -0.037(3) O16 0.079(3) 0.184(6) 0.086(3) 0.056(3) 0.011(2) -0.054(3) C16 0.055(3) 0.108(5) 0.056(3) 0.032(3) -0.004(2) -0.032(3) C17 0.056(3) 0.107(5) 0.068(3) 0.024(3) 0.020(2) 0.013(3) C18 0.061(2) 0.073(4) 0.055(2) 0.018(3) 0.020(2) 0.006(3) C19 0.067(4) 0.309(15) 0.104(5) 0.096(8) 0.014(4) -0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 C13 2.134(4) . ? Te1 Cl2 2.5293(11) . ? Te1 Cl1 2.5501(11) . ? Te1 S1 2.5987(10) . ? Te1 S2 2.6227(10) . ? S1 P1 2.0615(14) . ? P1 N1 1.580(3) . ? P1 C1 1.822(4) . ? P1 C4 1.824(5) . ? N1 P2 1.580(3) . ? C1 C3 1.507(8) . ? C1 C2 1.525(6) . ? P2 C7 1.831(5) . ? P2 C10 1.830(5) . ? P2 S2 2.041(2) . ? C4 C6 1.513(9) . ? C4 C5 1.534(7) . ? C7 C9 1.493(9) . ? C7 C8 1.544(9) . ? C10 C11 1.510(9) . ? C10 C12 1.516(7) . ? C13 C18 1.361(7) . ? C13 C14 1.380(7) . ? C14 C15 1.387(8) . ? C15 C16 1.370(10) . ? O16 C16 1.376(6) . ? O16 C19 1.396(12) . ? C16 C17 1.342(10) . ? C17 C18 1.398(7) . ? 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 C13 Te1 Cl2 88.41(12) . . ? C13 Te1 Cl1 88.40(12) . . ? Cl2 Te1 Cl1 91.42(4) . . ? C13 Te1 S1 87.81(12) . . ? Cl2 Te1 S1 89.80(4) . . ? Cl1 Te1 S1 175.99(4) . . ? C13 Te1 S2 86.18(12) . . ? Cl2 Te1 S2 174.60(4) . . ? Cl1 Te1 S2 88.49(4) . . ? S1 Te1 S2 89.94(4) . . ? P1 S1 Te1 98.28(4) . . ? N1 P1 C1 107.1(2) . . ? N1 P1 C4 113.5(2) . . ? C1 P1 C4 107.2(2) . . ? N1 P1 S1 115.74(14) . . ? C1 P1 S1 108.9(2) . . ? C4 P1 S1 104.0(2) . . ? P1 N1 P2 144.3(2) . . ? C3 C1 C2 110.8(5) . . ? C3 C1 P1 111.4(3) . . ? C2 C1 P1 112.3(3) . . ? N1 P2 C7 111.9(2) . . ? N1 P2 C10 106.1(2) . . ? C7 P2 C10 109.1(3) . . ? N1 P2 S2 115.25(14) . . ? C7 P2 S2 104.2(2) . . ? C10 P2 S2 110.3(2) . . ? P2 S2 Te1 97.97(5) . . ? C6 C4 C5 112.1(6) . . ? C6 C4 P1 112.1(4) . . ? C5 C4 P1 110.3(4) . . ? C9 C7 C8 112.2(6) . . ? C9 C7 P2 117.1(4) . . ? C8 C7 P2 111.0(5) . . ? C11 C10 C12 110.3(6) . . ? C11 C10 P2 113.1(3) . . ? C12 C10 P2 113.2(4) . . ? C18 C13 C14 120.4(4) . . ? C18 C13 Te1 120.9(4) . . ? C14 C13 Te1 118.6(4) . . ? C13 C14 C15 118.9(6) . . ? C16 C15 C14 120.4(6) . . ? C16 O16 C19 118.2(7) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 O16 126.0(7) . . ? C15 C16 O16 113.6(6) . . ? C16 C17 C18 120.2(6) . . ? C13 C18 C17 119.6(6) . . ? _refine_diff_density_max 0.520 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.055 #--- data_9 _audit_creation_method SHELXL _chemical_name_systematic ; 9 ; _chemical_name_common - _chemical_formula_moiety 'C25 H31 Cl2 N O P2 S2 Te' _chemical_formula_structural 'C25 H31 Cl2 N O P2 S2 Te' _chemical_formula_analytical 'C25 H31 Cl2 N O P2 S2 Te' _chemical_formula_sum 'C25 H31 Cl2 N O P2 S2 Te' _chemical_formula_weight 686.07 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.4268(2) _cell_length_b 14.0714(4) _cell_length_c 15.5035(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2929.14(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 59 _cell_measurement_theta_min 23 _cell_measurement_theta_max 337 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max .05 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .15 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method - _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.469 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.403826 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 12947 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.1221 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4216 _reflns_number_observed 2666 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(4) _refine_ls_number_reflns 4166 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_obs 0.0573 _refine_ls_wR_factor_all 0.1385 _refine_ls_wR_factor_obs 0.1119 _refine_ls_goodness_of_fit_all 0.893 _refine_ls_goodness_of_fit_obs 0.975 _refine_ls_restrained_S_all 0.960 _refine_ls_restrained_S_obs 0.975 _refine_ls_shift/esd_max -2.481 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Te1 Te -1.27014(5) -0.79036(5) -0.23793(4) 0.0500(3) Uani 1 d . . Cl2 Cl -1.2973(3) -0.7281(3) -0.3878(2) 0.0997(14) Uani 1 d . . Cl1 Cl -1.4532(2) -0.8173(3) -0.2185(3) 0.0905(13) Uani 1 d . . S1 S -1.0776(2) -0.7442(2) -0.2465(3) 0.0674(9) Uani 1 d . . P1 P -1.0316(2) -0.8812(2) -0.2388(2) 0.0440(7) Uani 1 d . . N1 N -1.0926(6) -0.9505(6) -0.1810(6) 0.050(3) Uani 1 d . . P2 P -1.1550(2) -0.9485(2) -0.0931(2) 0.0494(8) Uani 1 d . . S2 S -1.2521(3) -0.8408(2) -0.0772(2) 0.0684(10) Uani 1 d . . C1 C -1.0282(8) -0.9332(8) -0.3455(6) 0.042(3) Uani 1 d . . C2 C -1.0056(9) -0.8770(10) -0.4164(7) 0.063(4) Uani 1 d . . H2A H -0.9934(9) -0.8124(10) -0.4098(7) 0.075 Uiso 1 calc R . C3 C -1.0015(10) -0.9191(12) -0.4978(9) 0.077(4) Uani 1 d . . H3A H -0.9856(10) -0.8816(12) -0.5452(9) 0.092 Uiso 1 calc R . C4 C -1.0203(10) -1.0146(11) -0.5104(9) 0.072(4) Uani 1 d . . H4A H -1.0164(10) -1.0418(11) -0.5650(9) 0.086 Uiso 1 calc R . C5 C -1.0459(9) -1.0697(10) -0.4367(9) 0.069(4) Uani 1 d . . H5A H -1.0591(9) -1.1342(10) -0.4430(9) 0.083 Uiso 1 calc R . C6 C -1.0515(9) -1.0291(9) -0.3562(8) 0.060(3) Uani 1 d . . H6A H -1.0707(9) -1.0655(9) -0.3090(8) 0.073 Uiso 1 calc R . C7 C -0.9052(9) -0.8759(8) -0.2027(7) 0.051(3) Uani 1 d . . C8 C -0.8634(10) -0.9575(10) -0.1710(8) 0.065(4) Uani 1 d . . H8A H -0.9010(10) -1.0131(10) -0.1720(8) 0.078 Uiso 1 calc R . C9 C -0.7697(14) -0.9612(11) -0.1383(9) 0.080(4) Uani 1 d . . H9A H -0.7448(14) -1.0179(11) -0.1163(9) 0.096 Uiso 1 calc R . C10 C -0.7119(12) -0.8807(16) -0.1379(10) 0.098(6) Uani 1 d . . H10A H -0.6470(12) -0.8821(16) -0.1172(10) 0.118 Uiso 1 calc R . C11 C -0.7518(11) -0.8000(13) -0.1682(9) 0.091(4) Uani 1 d . . H11A H -0.7137(11) -0.7449(13) -0.1661(9) 0.109 Uiso 1 calc R . C12 C -0.8474(10) -0.7946(10) -0.2028(8) 0.072(4) Uani 1 d . . H12A H -0.8717(10) -0.7378(10) -0.2252(8) 0.086 Uiso 1 calc R . C13 C -1.2880(9) -0.6495(8) -0.1871(7) 0.047(3) Uani 1 d . . C14 C -1.3668(10) -0.5941(9) -0.2141(8) 0.070(4) Uani 1 d . . H14A H -1.4109(10) -0.6162(9) -0.2558(8) 0.084 Uiso 1 calc R . C15 C -1.3792(11) -0.5024(10) -0.1767(11) 0.077(4) Uani 1 d . . H15A H -1.4317(11) -0.4631(10) -0.1926(11) 0.093 Uiso 1 calc R . C16 C -1.3119(15) -0.4752(11) -0.1179(11) 0.086(5) Uani 1 d . . C17 C -1.2352(14) -0.5270(11) -0.0945(9) 0.092(5) Uani 1 d . . H17A H -1.1900(14) -0.5044(11) -0.0539(9) 0.110 Uiso 1 calc R . C18 C -1.2229(10) -0.6136(9) -0.1303(7) 0.061(3) Uani 1 d . . H18A H -1.1675(10) -0.6495(9) -0.1151(7) 0.074 Uiso 1 calc R . O16 O -1.3121(10) -0.3813(9) -0.0756(9) 0.122(4) Uani 1 d . . C19 C -1.3933(14) -0.3310(13) -0.0863(14) 0.129(7) Uani 1 d . . H19A H -1.3866(14) -0.2714(13) -0.0567(14) 0.193 Uiso 1 calc R . H19B H -1.4493(14) -0.3651(13) -0.0634(14) 0.193 Uiso 1 calc R . H19C H -1.4035(14) -0.3195(13) -0.1467(14) 0.193 Uiso 1 calc R . C20 C -1.0750(10) -0.9436(11) 0.0017(8) 0.073(4) Uani 1 d . . H20A H -1.0237(10) -0.9927(11) -0.0048(8) 0.088 Uiso 1 calc R . C21 C -1.1367(12) -0.9677(11) 0.0838(8) 0.094(5) Uani 1 d . . H21A H -1.1674(12) -1.0288(11) 0.0769(8) 0.141 Uiso 1 calc R . H21B H -1.1872(12) -0.9203(11) 0.0920(8) 0.141 Uiso 1 calc R . H21C H -1.0935(12) -0.9689(11) 0.1331(8) 0.141 Uiso 1 calc R . C22 C -1.0222(10) -0.8473(11) 0.0065(9) 0.092(5) Uani 1 d . . H22A H -0.9852(10) -0.8369(11) -0.0456(9) 0.138 Uiso 1 calc R . H22B H -0.9775(10) -0.8469(11) 0.0549(9) 0.138 Uiso 1 calc R . H22C H -1.0707(10) -0.7978(11) 0.0133(9) 0.138 Uiso 1 calc R . C23 C -1.2251(10) -1.0596(8) -0.0918(7) 0.060(3) Uani 1 d . . H23A H -1.2665(10) -1.0612(8) -0.0398(7) 0.072 Uiso 1 calc R . C24 C -1.1486(10) -1.1427(9) -0.0877(9) 0.084(4) Uani 1 d . . H24A H -1.1078(10) -1.1357(9) -0.0373(9) 0.125 Uiso 1 calc R . H24B H -1.1074(10) -1.1415(9) -0.1383(9) 0.125 Uiso 1 calc R . H24C H -1.1836(10) -1.2021(9) -0.0850(9) 0.125 Uiso 1 calc R . C25 C -1.2917(10) -1.0666(9) -0.1699(9) 0.084(4) Uani 1 d . . H25A H -1.3372(10) -1.0140(9) -0.1705(9) 0.126 Uiso 1 calc R . H25B H -1.3286(10) -1.1251(9) -0.1677(9) 0.126 Uiso 1 calc R . H25C H -1.2518(10) -1.0654(9) -0.2213(9) 0.126 Uiso 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 0.0651(5) 0.0436(4) 0.0414(4) 0.0011(4) -0.0050(4) -0.0046(4) Cl2 0.176(4) 0.083(3) 0.041(2) 0.005(2) -0.028(2) -0.004(3) Cl1 0.063(2) 0.096(3) 0.113(3) -0.003(2) -0.009(2) -0.020(2) S1 0.074(2) 0.046(2) 0.082(2) -0.004(2) 0.006(2) 0.0018(13) P1 0.064(2) 0.0317(14) 0.036(2) -0.002(2) 0.005(2) -0.0002(12) N1 0.067(6) 0.031(6) 0.051(6) -0.010(5) 0.024(5) -0.005(5) P2 0.067(2) 0.041(2) 0.041(2) -0.001(2) 0.004(2) 0.006(2) S2 0.097(3) 0.056(2) 0.052(2) 0.013(2) 0.010(2) 0.018(2) C1 0.059(8) 0.038(7) 0.028(6) -0.007(6) -0.002(6) -0.012(6) C2 0.086(10) 0.062(9) 0.040(8) -0.004(7) 0.000(7) -0.006(7) C3 0.084(11) 0.098(12) 0.049(9) 0.003(9) 0.000(8) -0.010(9) C4 0.084(11) 0.081(12) 0.050(9) -0.031(9) -0.017(8) 0.024(9) C5 0.078(10) 0.057(9) 0.071(10) -0.032(9) -0.010(9) 0.005(7) C6 0.095(10) 0.043(8) 0.043(7) 0.001(7) -0.004(7) -0.006(7) C7 0.093(9) 0.026(6) 0.034(6) 0.006(5) 0.006(6) 0.009(7) C8 0.070(10) 0.062(10) 0.062(9) -0.017(8) 0.006(8) -0.014(8) C9 0.099(13) 0.073(11) 0.069(9) -0.005(8) 0.007(11) 0.012(11) C10 0.067(12) 0.150(18) 0.078(11) 0.015(12) -0.019(10) 0.006(13) C11 0.071(11) 0.104(13) 0.097(10) -0.006(10) -0.019(8) -0.032(10) C12 0.085(10) 0.054(8) 0.075(9) 0.012(8) -0.006(7) -0.020(8) C13 0.052(7) 0.042(7) 0.047(7) 0.011(6) -0.001(6) 0.001(6) C14 0.087(10) 0.069(10) 0.053(9) 0.000(7) -0.001(8) 0.012(8) C15 0.066(10) 0.060(11) 0.105(13) 0.013(9) 0.023(9) 0.023(8) C16 0.131(16) 0.057(11) 0.070(11) -0.014(9) 0.022(11) 0.023(11) C17 0.148(16) 0.061(11) 0.066(9) -0.007(9) 0.011(12) -0.002(12) C18 0.069(8) 0.063(9) 0.053(7) -0.009(7) 0.001(8) 0.001(8) O16 0.154(12) 0.078(9) 0.135(10) -0.015(8) 0.000(9) -0.007(8) C19 0.124(15) 0.113(16) 0.150(19) 0.003(14) 0.010(15) 0.015(13) C20 0.098(11) 0.086(12) 0.035(7) 0.001(8) -0.007(8) 0.002(9) C21 0.135(13) 0.107(13) 0.040(8) 0.004(9) 0.001(9) 0.005(11) C22 0.117(13) 0.094(12) 0.065(10) -0.019(9) -0.012(10) -0.029(10) C23 0.078(8) 0.054(8) 0.047(7) 0.006(6) 0.018(8) -0.012(8) C24 0.127(12) 0.048(9) 0.076(10) 0.008(8) 0.035(10) 0.014(8) C25 0.096(11) 0.061(9) 0.096(11) -0.012(8) 0.002(10) -0.016(8) _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 C13 2.147(11) . ? Te1 Cl1 2.505(3) . ? Te1 Cl2 2.510(3) . ? Te1 S2 2.603(3) . ? Te1 S1 2.669(3) . ? S1 P1 2.029(4) . ? P1 N1 1.558(9) . ? P1 C7 1.788(13) . ? P1 C1 1.810(10) . ? N1 P2 1.599(9) . ? P2 C23 1.824(12) . ? P2 C20 1.823(12) . ? P2 S2 2.015(4) . ? C1 C2 1.387(15) . ? C1 C6 1.396(15) . ? C2 C3 1.39(2) . ? C3 C4 1.38(2) . ? C4 C5 1.42(2) . ? C5 C6 1.37(2) . ? C7 C8 1.37(2) . ? C7 C12 1.38(2) . ? C8 C9 1.36(2) . ? C9 C10 1.37(2) . ? C10 C11 1.34(2) . ? C11 C12 1.39(2) . ? C13 C18 1.340(15) . ? C13 C14 1.38(2) . ? C14 C15 1.42(2) . ? C15 C16 1.34(2) . ? C16 C17 1.31(2) . ? C16 O16 1.47(2) . ? C17 C18 1.35(2) . ? O16 C19 1.31(2) . ? C20 C22 1.53(2) . ? C20 C21 1.56(2) . ? C23 C25 1.51(2) . ? C23 C24 1.56(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Te1 Cl1 89.2(3) . . ? C13 Te1 Cl2 90.1(3) . . ? Cl1 Te1 Cl2 91.23(14) . . ? C13 Te1 S2 84.9(3) . . ? Cl1 Te1 S2 86.25(12) . . ? Cl2 Te1 S2 174.39(12) . . ? C13 Te1 S1 84.4(3) . . ? Cl1 Te1 S1 173.33(12) . . ? Cl2 Te1 S1 90.56(13) . . ? S2 Te1 S1 91.39(12) . . ? P1 S1 Te1 93.50(13) . . ? N1 P1 C7 110.2(5) . . ? N1 P1 C1 106.7(5) . . ? C7 P1 C1 106.2(5) . . ? N1 P1 S1 117.9(4) . . ? C7 P1 S1 105.5(4) . . ? C1 P1 S1 109.7(4) . . ? P1 N1 P2 139.0(6) . . ? N1 P2 C23 105.3(5) . . ? N1 P2 C20 112.3(6) . . ? C23 P2 C20 109.2(6) . . ? N1 P2 S2 117.2(4) . . ? C23 P2 S2 108.0(4) . . ? C20 P2 S2 104.7(5) . . ? P2 S2 Te1 98.51(15) . . ? C2 C1 C6 120.4(10) . . ? C2 C1 P1 120.0(8) . . ? C6 C1 P1 119.6(9) . . ? C3 C2 C1 118.9(13) . . ? C4 C3 C2 122.3(14) . . ? C3 C4 C5 117.4(13) . . ? C6 C5 C4 121.0(12) . . ? C5 C6 C1 119.9(12) . . ? C8 C7 C12 117.7(12) . . ? C8 C7 P1 117.7(10) . . ? C12 C7 P1 124.5(10) . . ? C9 C8 C7 123.1(12) . . ? C8 C9 C10 119.6(15) . . ? C11 C10 C9 118.2(15) . . ? C10 C11 C12 123.3(15) . . ? C7 C12 C11 118.1(13) . . ? C18 C13 C14 119.1(12) . . ? C18 C13 Te1 121.1(9) . . ? C14 C13 Te1 119.8(9) . . ? C13 C14 C15 118.6(13) . . ? C16 C15 C14 117.2(13) . . ? C17 C16 C15 123.9(15) . . ? C17 C16 O16 112.1(17) . . ? C15 C16 O16 123.9(17) . . ? C16 C17 C18 119.0(16) . . ? C13 C18 C17 122.1(14) . . ? C19 O16 C16 115.4(16) . . ? C22 C20 C21 113.6(12) . . ? C22 C20 P2 110.2(10) . . ? C21 C20 P2 109.7(10) . . ? C25 C23 C24 112.0(11) . . ? C25 C23 P2 110.7(8) . . ? C24 C23 P2 107.7(9) . . ? 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 C13 Te1 S1 P1 154.4(3) . . . . ? Cl1 Te1 S1 P1 138.9(11) . . . . ? Cl2 Te1 S1 P1 -115.5(2) . . . . ? S2 Te1 S1 P1 69.7(2) . . . . ? Te1 S1 P1 N1 -35.3(4) . . . . ? Te1 S1 P1 C7 -158.9(4) . . . . ? Te1 S1 P1 C1 87.0(4) . . . . ? C7 P1 N1 P2 87.1(10) . . . . ? C1 P1 N1 P2 -158.0(9) . . . . ? S1 P1 N1 P2 -34.2(11) . . . . ? P1 N1 P2 C23 166.2(9) . . . . ? P1 N1 P2 C20 -75.1(11) . . . . ? P1 N1 P2 S2 46.2(11) . . . . ? N1 P2 S2 Te1 19.4(4) . . . . ? C23 P2 S2 Te1 -99.2(4) . . . . ? C20 P2 S2 Te1 144.6(5) . . . . ? C13 Te1 S2 P2 -146.9(3) . . . . ? Cl1 Te1 S2 P2 123.6(2) . . . . ? Cl2 Te1 S2 P2 -173.0(13) . . . . ? S1 Te1 S2 P2 -62.7(2) . . . . ? N1 P1 C1 C2 160.9(9) . . . . ? C7 P1 C1 C2 -81.5(11) . . . . ? S1 P1 C1 C2 32.1(11) . . . . ? N1 P1 C1 C6 -17.0(11) . . . . ? C7 P1 C1 C6 100.6(10) . . . . ? S1 P1 C1 C6 -145.8(9) . . . . ? C6 C1 C2 C3 -3.3(18) . . . . ? P1 C1 C2 C3 178.7(10) . . . . ? C1 C2 C3 C4 0.8(21) . . . . ? C2 C3 C4 C5 0.9(22) . . . . ? C3 C4 C5 C6 -0.1(21) . . . . ? C4 C5 C6 C1 -2.4(20) . . . . ? C2 C1 C6 C5 4.2(18) . . . . ? P1 C1 C6 C5 -177.9(10) . . . . ? N1 P1 C7 C8 35.4(11) . . . . ? C1 P1 C7 C8 -79.8(10) . . . . ? S1 P1 C7 C8 163.8(8) . . . . ? N1 P1 C7 C12 -143.1(10) . . . . ? C1 P1 C7 C12 101.7(11) . . . . ? S1 P1 C7 C12 -14.7(11) . . . . ? C12 C7 C8 C9 1.6(18) . . . . ? P1 C7 C8 C9 -177.0(10) . . . . ? C7 C8 C9 C10 -1.4(20) . . . . ? C8 C9 C10 C11 1.7(22) . . . . ? C9 C10 C11 C12 -2.3(24) . . . . ? C8 C7 C12 C11 -2.0(18) . . . . ? P1 C7 C12 C11 176.5(9) . . . . ? C10 C11 C12 C7 2.5(22) . . . . ? Cl1 Te1 C13 C18 136.9(9) . . . . ? Cl2 Te1 C13 C18 -131.8(9) . . . . ? S2 Te1 C13 C18 50.6(9) . . . . ? S1 Te1 C13 C18 -41.3(9) . . . . ? Cl1 Te1 C13 C14 -44.1(9) . . . . ? Cl2 Te1 C13 C14 47.1(9) . . . . ? S2 Te1 C13 C14 -130.4(9) . . . . ? S1 Te1 C13 C14 137.7(9) . . . . ? C18 C13 C14 C15 -3.5(17) . . . . ? Te1 C13 C14 C15 177.5(9) . . . . ? C13 C14 C15 C16 0.8(19) . . . . ? C14 C15 C16 C17 1.5(24) . . . . ? C14 C15 C16 O16 177.7(13) . . . . ? C15 C16 C17 C18 -1.0(25) . . . . ? O16 C16 C17 C18 -177.6(12) . . . . ? C14 C13 C18 C17 4.1(18) . . . . ? Te1 C13 C18 C17 -176.9(10) . . . . ? C16 C17 C18 C13 -1.9(22) . . . . ? C17 C16 O16 C19 -170.9(16) . . . . ? C15 C16 O16 C19 12.5(24) . . . . ? N1 P2 C20 C22 68.6(11) . . . . ? C23 P2 C20 C22 -175.0(9) . . . . ? S2 P2 C20 C22 -59.5(10) . . . . ? N1 P2 C20 C21 -165.6(9) . . . . ? C23 P2 C20 C21 -49.2(12) . . . . ? S2 P2 C20 C21 66.3(11) . . . . ? N1 P2 C23 C25 -58.8(10) . . . . ? C20 P2 C23 C25 -179.5(9) . . . . ? S2 P2 C23 C25 67.2(9) . . . . ? N1 P2 C23 C24 64.0(9) . . . . ? C20 P2 C23 C24 -56.8(10) . . . . ? S2 P2 C23 C24 -170.1(7) . . . . ? _refine_diff_density_max 1.513 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.111 #---end