# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_address ; Department of Chemistry The University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; The Cyclic [N(PiPr2E)2]+ (E = Se, Te) Cations: A New Class of Inorganic Ring System ; _publ_contact_author 'Professor Tristram Chivers' loop_ _publ_author_name 'T. Chivers' 'Jari Konu' 'Heikki Tuononen' data_4 _database_code_depnum_ccdc_archive 'CCDC 287969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N P2 Se2, I' _chemical_formula_sum 'C12 H28 I N P2 Se2' _chemical_formula_weight 533.11 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 14.494(3) _cell_length_b 9.5920(19) _cell_length_c 14.163(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.45(3) _cell_angle_gamma 90.00 _cell_volume 1897.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6209 _cell_measurement_theta_min 4.23 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 5.679 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1635 _exptl_absorpt_correction_T_max 0.2806 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6209 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3258 _reflns_number_gt 3035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.970(15) _refine_ls_number_reflns 3258 _refine_ls_number_parameters 172 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.24186(4) 0.05014(5) 0.36961(4) 0.04181(15) Uani 1 1 d . . . Se1 Se 0.25161(4) 0.37569(6) 0.34481(4) 0.03015(17) Uani 1 1 d . . . Se2 Se 0.25463(5) 0.63457(6) 0.34829(4) 0.03279(17) Uani 1 1 d . . . P1 P 0.37964(12) 0.36889(15) 0.28082(12) 0.0258(3) Uani 1 1 d . . . P2 P 0.32687(12) 0.65185(16) 0.22818(11) 0.0250(3) Uani 1 1 d . . . N1 N 0.3822(4) 0.5102(5) 0.2226(4) 0.0253(11) Uani 1 1 d . . . C10 C 0.4902(5) 0.3452(8) 0.3778(6) 0.0380(17) Uani 1 1 d . . . H10 H 0.5443 0.3767 0.3515 0.046 Uiso 1 1 calc R . . C11 C 0.4908(6) 0.4369(8) 0.4671(6) 0.050(2) Uani 1 1 d . . . H11A H 0.5542 0.4330 0.5139 0.075 Uiso 1 1 calc R . . H11B H 0.4426 0.4027 0.4985 0.075 Uiso 1 1 calc R . . H11C H 0.4761 0.5334 0.4457 0.075 Uiso 1 1 calc R . . C12 C 0.5099(6) 0.1932(8) 0.4107(6) 0.0453(19) Uani 1 1 d . . . H12A H 0.4561 0.1573 0.4333 0.068 Uiso 1 1 calc R . . H12B H 0.5687 0.1883 0.4642 0.068 Uiso 1 1 calc R . . H12C H 0.5173 0.1369 0.3555 0.068 Uiso 1 1 calc R . . C13 C 0.3676(6) 0.2222(7) 0.1976(5) 0.0384(16) Uani 1 1 d . . . H13 H 0.3718 0.1341 0.2362 0.046 Uiso 1 1 calc R . . C14 C 0.2730(7) 0.2220(8) 0.1172(5) 0.049(2) Uani 1 1 d . . . H14A H 0.2722 0.1434 0.0728 0.074 Uiso 1 1 calc R . . H14B H 0.2667 0.3096 0.0803 0.074 Uiso 1 1 calc R . . H14C H 0.2196 0.2130 0.1470 0.074 Uiso 1 1 calc R . . C15 C 0.4522(7) 0.2266(8) 0.1509(6) 0.053(2) Uani 1 1 d . . . H15A H 0.4529 0.3167 0.1185 0.079 Uiso 1 1 calc R . . H15B H 0.4451 0.1515 0.1025 0.079 Uiso 1 1 calc R . . H15C H 0.5123 0.2143 0.2019 0.079 Uiso 1 1 calc R . . C20 C 0.4084(5) 0.8009(7) 0.2543(5) 0.0345(15) Uani 1 1 d . . . H20 H 0.3694 0.8859 0.2578 0.041 Uiso 1 1 calc R . . C21 C 0.4832(6) 0.7867(8) 0.3518(5) 0.0394(18) Uani 1 1 d . . . H21A H 0.5253 0.8684 0.3625 0.059 Uiso 1 1 calc R . . H21B H 0.5212 0.7024 0.3512 0.059 Uiso 1 1 calc R . . H21C H 0.4514 0.7801 0.4046 0.059 Uiso 1 1 calc R . . C22 C 0.4539(6) 0.8208(9) 0.1701(6) 0.0482(19) Uani 1 1 d . . . H22A H 0.4915 0.7380 0.1642 0.072 Uiso 1 1 calc R . . H22B H 0.4958 0.9027 0.1828 0.072 Uiso 1 1 calc R . . H22C H 0.4036 0.8345 0.1090 0.072 Uiso 1 1 calc R . . C23 C 0.2373(5) 0.6907(9) 0.1136(4) 0.0318(17) Uani 1 1 d . . . H23 H 0.2713 0.6939 0.0608 0.038 Uiso 1 1 calc R . . C24 C 0.1632(6) 0.5742(8) 0.0874(6) 0.051(2) Uani 1 1 d . . . H24A H 0.1120 0.6016 0.0298 0.076 Uiso 1 1 calc R . . H24B H 0.1360 0.5573 0.1427 0.076 Uiso 1 1 calc R . . H24C H 0.1939 0.4888 0.0727 0.076 Uiso 1 1 calc R . . C25 C 0.1915(6) 0.8315(9) 0.1160(6) 0.0439(18) Uani 1 1 d . . . H25A H 0.1644 0.8363 0.1723 0.066 Uiso 1 1 calc R . . H25B H 0.1406 0.8452 0.0554 0.066 Uiso 1 1 calc R . . H25C H 0.2399 0.9047 0.1217 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0516(3) 0.0291(2) 0.0513(3) 0.0011(2) 0.0252(2) -0.0026(2) Se1 0.0321(3) 0.0307(4) 0.0297(3) 0.0007(3) 0.0119(3) -0.0012(3) Se2 0.0433(4) 0.0265(4) 0.0326(3) -0.0007(3) 0.0172(3) 0.0023(3) P1 0.0288(9) 0.0190(8) 0.0310(8) 0.0021(6) 0.0105(7) 0.0007(6) P2 0.0299(9) 0.0192(8) 0.0259(8) -0.0001(6) 0.0074(6) 0.0006(6) N1 0.031(3) 0.015(2) 0.032(3) 0.000(2) 0.011(2) -0.001(2) C10 0.027(3) 0.026(4) 0.057(4) 0.013(3) 0.002(3) 0.002(3) C11 0.047(5) 0.041(5) 0.048(4) 0.007(4) -0.012(4) -0.006(4) C12 0.041(4) 0.028(4) 0.063(5) 0.014(4) 0.007(4) 0.003(3) C13 0.057(5) 0.020(4) 0.047(4) 0.002(3) 0.028(4) 0.001(3) C14 0.071(6) 0.032(5) 0.037(4) -0.008(3) 0.003(4) -0.006(4) C15 0.076(6) 0.033(4) 0.065(5) -0.005(4) 0.047(4) 0.000(4) C20 0.040(4) 0.025(3) 0.038(4) 0.002(3) 0.010(3) 0.002(3) C21 0.041(4) 0.025(4) 0.044(4) 0.000(3) -0.002(3) -0.008(3) C22 0.057(5) 0.036(4) 0.058(5) 0.001(4) 0.026(4) -0.010(4) C23 0.042(4) 0.031(4) 0.021(3) 0.003(2) 0.007(3) 0.004(3) C24 0.046(5) 0.035(4) 0.053(5) -0.009(4) -0.017(4) 0.007(3) C25 0.047(5) 0.036(4) 0.045(4) 0.012(3) 0.005(3) 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 Se1 P1 2.2728(19) . ? Se1 Se2 2.4839(9) . ? Se2 P2 2.2286(19) . ? P1 N1 1.593(5) . ? P1 C13 1.814(7) . ? P1 C10 1.826(7) . ? P2 N1 1.590(5) . ? P2 C23 1.826(6) . ? P2 C20 1.828(7) . ? C10 C12 1.534(11) . ? C10 C11 1.538(12) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.531(11) . ? C13 C15 1.541(10) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C21 1.517(9) . ? C20 C22 1.521(10) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.510(11) . ? C23 C24 1.526(11) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Se1 Se2 91.41(4) . . ? P2 Se2 Se1 93.94(4) . . ? N1 P1 C13 109.6(3) . . ? N1 P1 C10 111.0(3) . . ? C13 P1 C10 107.8(4) . . ? N1 P1 Se1 108.4(2) . . ? C13 P1 Se1 109.5(2) . . ? C10 P1 Se1 110.5(3) . . ? N1 P2 C23 112.2(3) . . ? N1 P2 C20 111.8(3) . . ? C23 P2 C20 106.8(3) . . ? N1 P2 Se2 108.7(2) . . ? C23 P2 Se2 109.0(2) . . ? C20 P2 Se2 108.2(2) . . ? P2 N1 P1 128.3(4) . . ? C12 C10 C11 109.5(6) . . ? C12 C10 P1 113.7(5) . . ? C11 C10 P1 111.0(5) . . ? C12 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? P1 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 109.7(6) . . ? C14 C13 P1 113.3(5) . . ? C15 C13 P1 107.9(5) . . ? C14 C13 H13 108.6 . . ? C15 C13 H13 108.6 . . ? P1 C13 H13 108.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C20 C22 111.7(6) . . ? C21 C20 P2 112.4(5) . . ? C22 C20 P2 109.3(5) . . ? C21 C20 H20 107.7 . . ? C22 C20 H20 107.7 . . ? P2 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 112.1(6) . . ? C25 C23 P2 112.0(5) . . ? C24 C23 P2 110.8(5) . . ? C25 C23 H23 107.2 . . ? C24 C23 H23 107.2 . . ? P2 C23 H23 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Se1 Se2 P2 25.05(7) . . . . ? Se2 Se1 P1 N1 -26.2(2) . . . . ? Se2 Se1 P1 C13 -145.7(2) . . . . ? Se2 Se1 P1 C10 95.7(3) . . . . ? Se1 Se2 P2 N1 -22.9(2) . . . . ? Se1 Se2 P2 C23 99.7(3) . . . . ? Se1 Se2 P2 C20 -144.5(2) . . . . ? C23 P2 N1 P1 -113.6(5) . . . . ? C20 P2 N1 P1 126.5(4) . . . . ? Se2 P2 N1 P1 7.1(5) . . . . ? C13 P1 N1 P2 135.2(4) . . . . ? C10 P1 N1 P2 -105.8(5) . . . . ? Se1 P1 N1 P2 15.8(5) . . . . ? N1 P1 C10 C12 -158.3(6) . . . . ? C13 P1 C10 C12 -38.2(7) . . . . ? Se1 P1 C10 C12 81.4(7) . . . . ? N1 P1 C10 C11 77.7(6) . . . . ? C13 P1 C10 C11 -162.3(5) . . . . ? Se1 P1 C10 C11 -42.7(6) . . . . ? N1 P1 C13 C14 -64.1(6) . . . . ? C10 P1 C13 C14 174.9(5) . . . . ? Se1 P1 C13 C14 54.7(5) . . . . ? N1 P1 C13 C15 57.6(6) . . . . ? C10 P1 C13 C15 -63.3(6) . . . . ? Se1 P1 C13 C15 176.5(5) . . . . ? N1 P2 C20 C21 -60.7(6) . . . . ? C23 P2 C20 C21 176.2(5) . . . . ? Se2 P2 C20 C21 59.0(6) . . . . ? N1 P2 C20 C22 64.0(6) . . . . ? C23 P2 C20 C22 -59.1(6) . . . . ? Se2 P2 C20 C22 -176.4(5) . . . . ? N1 P2 C23 C25 -174.6(5) . . . . ? C20 P2 C23 C25 -51.8(6) . . . . ? Se2 P2 C23 C25 64.9(6) . . . . ? N1 P2 C23 C24 59.4(6) . . . . ? C20 P2 C23 C24 -177.8(5) . . . . ? Se2 P2 C23 C24 -61.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.354 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.135 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 287970' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H28 N P2 Te2, I' _chemical_formula_sum 'C12 H28 I N P2 Te2' _chemical_formula_weight 630.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 14.187(3) _cell_length_b 9.756(2) _cell_length_c 14.682(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.60(3) _cell_angle_gamma 90.00 _cell_volume 1926.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5647 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 4.786 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5148 _exptl_absorpt_correction_T_max 0.7958 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5647 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3201 _reflns_number_gt 2994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+13.4527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 3201 _refine_ls_number_parameters 179 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1A I 0.27702(7) 0.00818(5) 0.31515(7) 0.0360(2) Uani 0.9238(9) 1 d P A 1 Te1A Te 0.27674(3) 0.35931(5) 0.32669(3) 0.02164(15) Uani 0.9238(9) 1 d P A 1 Te2A Te 0.27194(3) 0.65020(5) 0.31917(3) 0.02255(16) Uani 0.9238(9) 1 d P A 1 P1A P 0.14051(17) 0.3663(2) 0.38984(17) 0.0199(4) Uani 0.9238(9) 1 d P A 1 P2A P 0.19838(17) 0.6478(2) 0.44822(17) 0.0184(4) Uani 0.9238(9) 1 d P A 1 I1B I 0.2755(11) 0.5012(6) 0.3162(12) 0.0360(2) Uani 0.0762(9) 1 d P A 2 Te1B Te 0.2632(6) 0.8552(6) 0.3135(8) 0.02164(15) Uani 0.0762(9) 1 d P . 2 Te2B Te 0.2713(7) 1.1435(6) 0.3198(8) 0.02255(16) Uani 0.0762(9) 1 d P . 2 P1B P 0.2011(18) 0.860(2) 0.4485(17) 0.0199(4) Uani 0.0762(9) 1 d P . 2 P2B P 0.1414(18) 1.154(2) 0.3900(17) 0.0184(4) Uani 0.0762(9) 1 d P . 2 N1A N 0.1421(5) 0.5105(6) 0.4451(5) 0.0251(14) Uani 1 1 d . . . C10 C 0.1508(6) 0.2258(8) 0.4723(5) 0.0309(17) Uani 1 1 d . . . H10 H 0.1440 0.1384 0.4352 0.037 Uiso 1 1 calc R A 1 C11 C 0.0690(7) 0.2310(10) 0.5152(7) 0.048(2) Uani 1 1 d . A . H11A H 0.0876 0.1771 0.5745 0.072 Uiso 1 1 calc R . . H11B H 0.0082 0.1932 0.4696 0.072 Uiso 1 1 calc R . . H11C H 0.0574 0.3264 0.5296 0.072 Uiso 1 1 calc R . . C12 C 0.2468(6) 0.2206(10) 0.5531(6) 0.039(2) Uani 1 1 d . A . H12A H 0.2530 0.3026 0.5932 0.058 Uiso 1 1 calc R . . H12B H 0.3023 0.2170 0.5271 0.058 Uiso 1 1 calc R . . H12C H 0.2480 0.1387 0.5922 0.058 Uiso 1 1 calc R . . C13 C 0.0281(6) 0.3455(9) 0.2916(6) 0.035(2) Uani 1 1 d . . . H13 H -0.0283 0.3671 0.3163 0.043 Uiso 1 1 calc R A 1 C14 C 0.0211(7) 0.4452(9) 0.2094(7) 0.050(2) Uani 1 1 d . A . H14A H 0.0664 0.4157 0.1749 0.074 Uiso 1 1 calc R . . H14B H 0.0396 0.5374 0.2355 0.074 Uiso 1 1 calc R . . H14C H -0.0473 0.4464 0.1651 0.074 Uiso 1 1 calc R . . C15 C 0.0135(6) 0.1969(9) 0.2545(7) 0.042(2) Uani 1 1 d . . . H15A H -0.0471 0.1910 0.1990 0.064 Uiso 1 1 calc R . . H15B H 0.0074 0.1362 0.3056 0.064 Uiso 1 1 calc R . . H15C H 0.0709 0.1689 0.2355 0.064 Uiso 1 1 calc R . . C20 C 0.2904(6) 0.6723(7) 0.5645(6) 0.0286(18) Uani 1 1 d . . . H20 H 0.2552 0.6590 0.6130 0.034 Uiso 1 1 calc R A 1 C21 C 0.3662(7) 0.5613(9) 0.5818(6) 0.048(2) Uani 1 1 d . A . H21A H 0.4110 0.5796 0.5443 0.071 Uiso 1 1 calc R . . H21B H 0.3329 0.4731 0.5621 0.071 Uiso 1 1 calc R . . H21C H 0.4047 0.5582 0.6503 0.071 Uiso 1 1 calc R . . C22 C 0.3307(7) 0.8155(9) 0.5783(6) 0.040(2) Uani 1 1 d . . . H22A H 0.3772 0.8254 0.6436 0.060 Uiso 1 1 calc R B 2 H22B H 0.2759 0.8806 0.5686 0.060 Uiso 1 1 calc R B 2 H22C H 0.3655 0.8340 0.5316 0.060 Uiso 1 1 calc R B 2 C23 C 0.1171(6) 0.7927(9) 0.4304(6) 0.0345(18) Uani 1 1 d . . . H23 H 0.1573 0.8773 0.4321 0.041 Uiso 1 1 calc R A 1 C24 C 0.0389(6) 0.7847(10) 0.3341(6) 0.037(2) Uani 1 1 d . A . H24A H 0.0024 0.6982 0.3289 0.056 Uiso 1 1 calc R . . H24B H 0.0704 0.7888 0.2837 0.056 Uiso 1 1 calc R . . H24C H -0.0073 0.8617 0.3267 0.056 Uiso 1 1 calc R . . C25 C 0.0731(7) 0.8002(10) 0.5144(7) 0.044(2) Uani 1 1 d . A . H25A H 0.0241 0.8745 0.5024 0.066 Uiso 1 1 calc R . . H25B H 0.1267 0.8180 0.5747 0.066 Uiso 1 1 calc R . . H25C H 0.0408 0.7130 0.5194 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1A 0.0427(3) 0.0265(3) 0.0476(5) 0.0012(3) 0.0266(3) 0.0026(3) Te1A 0.0193(3) 0.0252(2) 0.0230(4) 0.0003(4) 0.0104(2) 0.0027(5) Te2A 0.0239(3) 0.0254(2) 0.0214(3) 0.0022(4) 0.0116(3) 0.0008(4) P1A 0.0128(8) 0.0254(10) 0.0211(10) -0.0035(8) 0.0050(7) -0.0008(8) P2A 0.0141(8) 0.0234(9) 0.0177(10) 0.0008(7) 0.0051(7) 0.0001(8) I1B 0.0427(3) 0.0265(3) 0.0476(5) 0.0012(3) 0.0266(3) 0.0026(3) Te1B 0.0193(3) 0.0252(2) 0.0230(4) 0.0003(4) 0.0104(2) 0.0027(5) Te2B 0.0239(3) 0.0254(2) 0.0214(3) 0.0022(4) 0.0116(3) 0.0008(4) P1B 0.0128(8) 0.0254(10) 0.0211(10) -0.0035(8) 0.0050(7) -0.0008(8) P2B 0.0141(8) 0.0234(9) 0.0177(10) 0.0008(7) 0.0051(7) 0.0001(8) N1A 0.023(3) 0.025(3) 0.032(3) -0.009(2) 0.014(3) 0.003(2) C10 0.034(4) 0.032(4) 0.029(4) -0.006(3) 0.014(3) -0.005(3) C11 0.045(5) 0.052(6) 0.061(6) 0.016(5) 0.036(5) -0.001(4) C12 0.039(5) 0.051(6) 0.029(5) 0.008(4) 0.016(4) 0.010(4) C13 0.022(4) 0.038(5) 0.044(5) 0.000(4) 0.006(4) 0.007(3) C14 0.042(5) 0.036(5) 0.050(5) -0.010(4) -0.015(4) 0.008(4) C15 0.025(4) 0.051(5) 0.048(5) -0.020(4) 0.007(4) -0.001(4) C20 0.032(4) 0.033(4) 0.020(4) 0.002(3) 0.005(3) 0.002(3) C21 0.042(5) 0.043(5) 0.038(5) -0.002(4) -0.016(4) -0.006(4) C22 0.043(5) 0.042(5) 0.028(5) -0.011(3) 0.002(4) -0.015(4) C23 0.029(4) 0.044(5) 0.036(5) -0.001(4) 0.019(4) 0.005(4) C24 0.022(4) 0.047(6) 0.037(5) 0.000(4) 0.002(4) 0.004(4) C25 0.038(5) 0.051(5) 0.048(5) 0.003(4) 0.021(4) 0.009(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 Te1A P1A 2.396(2) . ? Te1A Te2A 2.8401(9) . ? Te2A P2A 2.437(3) . ? P1A N1A 1.621(6) . ? P1A C13 1.788(8) . ? P1A C10 1.804(8) . ? P2A N1A 1.552(6) . ? P2A C23 1.790(8) . ? P2A C20 1.804(9) . ? Te1B P1B 2.41(2) . ? Te1B Te2B 2.815(8) . ? Te2B P2B 2.38(3) . ? P1B C23 1.31(3) . ? P1B C22 2.23(3) . ? P2B C10 1.36(3) 1_565 ? P2B C15 2.26(3) 1_565 ? C10 P2B 1.36(3) 1_545 ? C10 C11 1.486(11) . ? C10 C12 1.495(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.529(13) . ? C13 C15 1.539(11) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 P2B 2.26(3) 1_545 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C21 1.490(12) . ? C20 C22 1.498(11) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.495(11) . ? C23 C25 1.551(12) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1A Te1A Te2A 88.53(5) . . ? P2A Te2A Te1A 88.34(5) . . ? N1A P1A C13 111.6(4) . . ? N1A P1A C10 109.8(3) . . ? C13 P1A C10 108.4(4) . . ? N1A P1A Te1A 109.5(2) . . ? C13 P1A Te1A 107.9(3) . . ? C10 P1A Te1A 109.6(3) . . ? N1A P2A C23 112.0(4) . . ? N1A P2A C20 110.7(4) . . ? C23 P2A C20 105.8(4) . . ? N1A P2A Te2A 109.2(2) . . ? C23 P2A Te2A 107.1(3) . . ? C20 P2A Te2A 112.0(3) . . ? P1B Te1B Te2B 88.5(6) . . ? P2B Te2B Te1B 91.7(6) . . ? C23 P1B C22 121.5(16) . . ? C23 P1B Te1B 111.7(14) . . ? C22 P1B Te1B 106.2(10) . . ? C10 P2B C15 120.5(15) 1_565 1_565 ? C10 P2B Te2B 122.3(15) 1_565 . ? C15 P2B Te2B 98.2(9) 1_565 . ? P2A N1A P1A 133.5(4) . . ? P2B C10 C11 121.6(12) 1_545 . ? P2B C10 C12 119.5(12) 1_545 . ? C11 C10 C12 107.5(7) . . ? P2B C10 P1A 80.3(10) 1_545 . ? C11 C10 P1A 110.5(6) . . ? C12 C10 P1A 114.6(6) . . ? P2B C10 H10 27.8 1_545 . ? C11 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? P1A C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 110.6(7) . . ? C14 C13 P1A 112.4(6) . . ? C15 C13 P1A 112.2(6) . . ? C14 C13 H13 107.1 . . ? C15 C13 H13 107.1 . . ? P1A C13 H13 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 P2B 83.3(8) . 1_545 ? C13 C15 H15A 109.5 . . ? P2B C15 H15A 164.9 1_545 . ? C13 C15 H15B 109.5 . . ? P2B C15 H15B 57.2 1_545 . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? P2B C15 H15C 72.1 1_545 . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C20 C22 115.5(8) . . ? C21 C20 P2A 109.3(6) . . ? C22 C20 P2A 112.4(6) . . ? C21 C20 H20 106.3 . . ? C22 C20 H20 106.3 . . ? P2A C20 H20 106.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 P1B 83.8(8) . . ? C20 C22 H22A 109.5 . . ? P1B C22 H22A 158.6 . . ? C20 C22 H22B 109.5 . . ? P1B C22 H22B 49.3 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? P1B C22 H22C 80.2 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1B C23 C24 124.7(13) . . ? P1B C23 C25 112.6(13) . . ? C24 C23 C25 112.9(7) . . ? P1B C23 P2A 82.3(11) . . ? C24 C23 P2A 110.2(6) . . ? C25 C23 P2A 109.0(6) . . ? P1B C23 H23 26.6 . . ? C24 C23 H23 108.2 . . ? C25 C23 H23 108.2 . . ? P2A C23 H23 108.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1A Te1A Te2A P2A 25.84(7) . . . . ? Te2A Te1A P1A N1A -26.5(3) . . . . ? Te2A Te1A P1A C13 95.2(3) . . . . ? Te2A Te1A P1A C10 -147.0(3) . . . . ? Te1A Te2A P2A N1A -26.4(3) . . . . ? Te1A Te2A P2A C23 -147.9(3) . . . . ? Te1A Te2A P2A C20 96.5(3) . . . . ? P1B Te1B Te2B P2B -26.9(8) . . . . ? Te2B Te1B P1B C23 125.8(14) . . . . ? Te2B Te1B P1B C22 -99.7(8) . . . . ? Te1B Te2B P2B C10 127.7(15) . . . 1_565 ? Te1B Te2B P2B C15 -98.0(7) . . . 1_565 ? C23 P2A N1A P1A 131.9(5) . . . . ? C20 P2A N1A P1A -110.4(6) . . . . ? Te2A P2A N1A P1A 13.4(6) . . . . ? C13 P1A N1A P2A -106.1(6) . . . . ? C10 P1A N1A P2A 133.7(6) . . . . ? Te1A P1A N1A P2A 13.3(6) . . . . ? N1A P1A C10 P2B 177.8(11) . . . 1_545 ? C13 P1A C10 P2B 55.6(11) . . . 1_545 ? Te1A P1A C10 P2B -61.9(11) . . . 1_545 ? N1A P1A C10 C11 57.5(7) . . . . ? C13 P1A C10 C11 -64.6(7) . . . . ? Te1A P1A C10 C11 177.9(6) . . . . ? N1A P1A C10 C12 -64.2(7) . . . . ? C13 P1A C10 C12 173.7(6) . . . . ? Te1A P1A C10 C12 56.2(6) . . . . ? N1A P1A C13 C14 68.8(7) . . . . ? C10 P1A C13 C14 -170.1(6) . . . . ? Te1A P1A C13 C14 -51.6(7) . . . . ? N1A P1A C13 C15 -165.8(6) . . . . ? C10 P1A C13 C15 -44.8(7) . . . . ? Te1A P1A C13 C15 73.8(6) . . . . ? C14 C13 C15 P2B 137.4(9) . . . 1_545 ? P1A C13 C15 P2B 11.1(8) . . . 1_545 ? N1A P2A C20 C21 62.9(7) . . . . ? C23 P2A C20 C21 -175.5(6) . . . . ? Te2A P2A C20 C21 -59.2(6) . . . . ? N1A P2A C20 C22 -167.4(6) . . . . ? C23 P2A C20 C22 -45.9(7) . . . . ? Te2A P2A C20 C22 70.5(6) . . . . ? C21 C20 C22 P1B 140.2(9) . . . . ? P2A C20 C22 P1B 13.8(8) . . . . ? C23 P1B C22 C20 31.6(17) . . . . ? Te1B P1B C22 C20 -97.5(9) . . . . ? C22 P1B C23 C24 -160.7(10) . . . . ? Te1B P1B C23 C24 -34.1(19) . . . . ? C22 P1B C23 C25 56.0(18) . . . . ? Te1B P1B C23 C25 -177.3(8) . . . . ? C22 P1B C23 P2A -51.4(14) . . . . ? Te1B P1B C23 P2A 75.3(11) . . . . ? N1A P2A C23 P1B 174.9(11) . . . . ? C20 P2A C23 P1B 54.2(12) . . . . ? Te2A P2A C23 P1B -65.4(11) . . . . ? N1A P2A C23 C24 -60.9(7) . . . . ? C20 P2A C23 C24 178.4(6) . . . . ? Te2A P2A C23 C24 58.8(6) . . . . ? N1A P2A C23 C25 63.5(7) . . . . ? C20 P2A C23 C25 -57.1(7) . . . . ? Te2A P2A C23 C25 -176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.158 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.131 #===END