Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name R.Cavell _publ_contact_author_email ron.cavell@ualberta.ca _publ_section_title ; A geminal dithallated bis(phosphoranomethine) carbon bridged dimer with Tl-Tl idnteractions ; loop_ _publ_author_name 'Guibin Ma.' M.Ferguson R.Cavell # Attachment 'Tl4L2-CC-Rev.cif.txt' data_2 _database_code_depnum_ccdc_archive 'CCDC 735560' #TrackingRef 'Tl4L2-CC-Rev.cif.txt' _audit_creation_method 'manual editing of SHELXL template' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 N2 P2 Si2 Tl2' _chemical_formula_weight 965.49 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' Si Si 0.0817 0.0704 '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' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0949(12) _cell_length_b 13.1494(11) _cell_length_c 18.9302(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.7640(10) _cell_angle_gamma 90.00 _cell_volume 3506.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 9.360 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30102 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8033 _reflns_number_gt 7469 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0195P)^2^+2.3396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00156(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8033 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Tl1 Tl 0.568964(7) 0.276657(7) 0.456570(5) 0.02945(4) Uani 1 1 d . . . Tl2 Tl 0.381578(7) 0.500916(7) 0.449441(5) 0.02691(4) Uani 1 1 d . . . P1 P 0.55751(4) 0.42059(5) 0.32716(3) 0.02111(12) Uani 1 1 d . . . P2 P 0.35683(4) 0.31729(5) 0.35267(3) 0.02214(13) Uani 1 1 d . . . Si1 Si 0.75973(6) 0.33051(7) 0.33398(5) 0.03841(19) Uani 1 1 d . . . Si2 Si 0.15423(5) 0.35978(6) 0.39406(4) 0.03112(16) Uani 1 1 d . . . N1 N 0.64800(14) 0.36130(17) 0.35779(12) 0.0266(4) Uani 1 1 d . . . N2 N 0.27534(14) 0.36462(17) 0.39919(12) 0.0271(5) Uani 1 1 d . . . C1 C 0.45826(16) 0.38466(19) 0.37062(13) 0.0223(5) Uani 1 1 d . . . C11 C 0.57107(17) 0.55726(19) 0.34399(13) 0.0232(5) Uani 1 1 d . . . C12 C 0.65264(19) 0.5929(2) 0.37892(14) 0.0288(5) Uani 1 1 d . . . H12 H 0.7026 0.5470 0.3911 0.035 Uiso 1 1 calc R . . C13 C 0.6616(2) 0.6952(2) 0.39605(17) 0.0376(7) Uani 1 1 d . . . H13 H 0.7175 0.7186 0.4202 0.045 Uiso 1 1 calc R . . C14 C 0.5898(2) 0.7634(2) 0.37824(17) 0.0381(7) Uani 1 1 d . . . H14 H 0.5964 0.8333 0.3902 0.046 Uiso 1 1 calc R . . C15 C 0.5086(2) 0.7291(2) 0.34294(17) 0.0365(7) Uani 1 1 d . . . H15 H 0.4594 0.7756 0.3300 0.044 Uiso 1 1 calc R . . C16 C 0.49908(19) 0.6267(2) 0.32658(15) 0.0302(6) Uani 1 1 d . . . H16 H 0.4426 0.6035 0.3031 0.036 Uiso 1 1 calc R . . C17 C 0.8125(3) 0.4221(3) 0.2711(3) 0.0710(13) Uani 1 1 d . . . H17A H 0.8134 0.4902 0.2920 0.107 Uiso 1 1 calc R . . H17B H 0.7743 0.4230 0.2269 0.107 Uiso 1 1 calc R . . H17C H 0.8775 0.4011 0.2612 0.107 Uiso 1 1 calc R . . C18 C 0.7615(3) 0.2027(3) 0.2927(3) 0.0766(14) Uani 1 1 d . . . H18A H 0.7343 0.1529 0.3248 0.115 Uiso 1 1 calc R . . H18B H 0.8271 0.1837 0.2831 0.115 Uiso 1 1 calc R . . H18C H 0.7240 0.2039 0.2482 0.115 Uiso 1 1 calc R . . C19 C 0.8347(3) 0.3253(5) 0.4166(3) 0.0790(14) Uani 1 1 d . . . H19A H 0.8071 0.2770 0.4496 0.118 Uiso 1 1 calc R . . H19B H 0.8375 0.3929 0.4383 0.118 Uiso 1 1 calc R . . H19C H 0.8989 0.3033 0.4054 0.118 Uiso 1 1 calc R . . C21 C 0.55018(19) 0.4092(2) 0.23074(14) 0.0302(6) Uani 1 1 d . . . C22 C 0.5450(2) 0.3117(3) 0.20258(17) 0.0431(7) Uani 1 1 d . . . H22 H 0.5456 0.2548 0.2335 0.052 Uiso 1 1 calc R . . C23 C 0.5391(3) 0.2961(3) 0.1302(2) 0.0609(10) Uani 1 1 d . . . H23 H 0.5333 0.2291 0.1117 0.073 Uiso 1 1 calc R . . C24 C 0.5416(3) 0.3783(4) 0.08498(19) 0.0674(12) Uani 1 1 d . . . H24 H 0.5394 0.3679 0.0353 0.081 Uiso 1 1 calc R . . C25 C 0.5474(4) 0.4747(4) 0.1116(2) 0.0645(11) Uani 1 1 d . . . H25 H 0.5491 0.5310 0.0802 0.077 Uiso 1 1 calc R . . C26 C 0.5508(3) 0.4912(3) 0.18438(17) 0.0428(8) Uani 1 1 d . . . H26 H 0.5536 0.5587 0.2023 0.051 Uiso 1 1 calc R . . C27 C 0.1106(2) 0.3885(4) 0.4830(2) 0.0630(11) Uani 1 1 d . . . H27A H 0.1359 0.3383 0.5169 0.094 Uiso 1 1 calc R . . H27B H 0.0411 0.3859 0.4819 0.094 Uiso 1 1 calc R . . H27C H 0.1317 0.4567 0.4974 0.094 Uiso 1 1 calc R . . C28 C 0.1080(3) 0.2319(4) 0.3665(3) 0.0797(16) Uani 1 1 d . . . H28A H 0.1328 0.1801 0.3993 0.120 Uiso 1 1 calc R . . H28B H 0.1285 0.2165 0.3186 0.120 Uiso 1 1 calc R . . H28C H 0.0385 0.2322 0.3669 0.120 Uiso 1 1 calc R . . C29 C 0.1038(3) 0.4549(5) 0.3314(3) 0.0881(18) Uani 1 1 d . . . H29A H 0.1267 0.5228 0.3448 0.132 Uiso 1 1 calc R . . H29B H 0.0344 0.4533 0.3327 0.132 Uiso 1 1 calc R . . H29C H 0.1237 0.4390 0.2835 0.132 Uiso 1 1 calc R . . C31 C 0.37613(18) 0.1840(2) 0.37765(15) 0.0283(5) Uani 1 1 d . . . C32 C 0.3383(2) 0.1462(2) 0.43888(15) 0.0358(6) Uani 1 1 d . . . H32 H 0.2950 0.1864 0.4643 0.043 Uiso 1 1 calc R . . C33 C 0.3632(3) 0.0495(3) 0.46361(18) 0.0454(8) Uani 1 1 d . . . H33 H 0.3373 0.0247 0.5060 0.054 Uiso 1 1 calc R . . C34 C 0.4250(3) -0.0101(2) 0.4268(2) 0.0460(9) Uani 1 1 d . . . H34 H 0.4413 -0.0760 0.4437 0.055 Uiso 1 1 calc R . . C35 C 0.4630(3) 0.0257(2) 0.3660(2) 0.0457(8) Uani 1 1 d . . . H35 H 0.5057 -0.0155 0.3407 0.055 Uiso 1 1 calc R . . C36 C 0.4393(2) 0.1223(2) 0.34112(18) 0.0385(7) Uani 1 1 d . . . H36 H 0.4662 0.1467 0.2989 0.046 Uiso 1 1 calc R . . C41 C 0.32165(18) 0.3137(2) 0.25944(14) 0.0277(5) Uani 1 1 d . . . C42 C 0.2946(2) 0.2258(2) 0.22290(18) 0.0397(7) Uani 1 1 d . . . H42 H 0.2950 0.1620 0.2464 0.048 Uiso 1 1 calc R . . C43 C 0.2670(3) 0.2322(3) 0.1516(2) 0.0532(9) Uani 1 1 d . . . H43 H 0.2490 0.1721 0.1268 0.064 Uiso 1 1 calc R . . C44 C 0.2654(3) 0.3236(3) 0.11668(19) 0.0555(9) Uani 1 1 d . . . H44 H 0.2471 0.3264 0.0680 0.067 Uiso 1 1 calc R . . C45 C 0.2905(2) 0.4119(3) 0.15277(18) 0.0493(8) Uani 1 1 d . . . H45 H 0.2887 0.4756 0.1291 0.059 Uiso 1 1 calc R . . C46 C 0.3181(2) 0.4066(2) 0.22319(16) 0.0364(6) Uani 1 1 d . . . H46 H 0.3351 0.4673 0.2477 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl1 0.03141(6) 0.02788(6) 0.02875(7) 0.00709(4) -0.00440(4) 0.00125(4) Tl2 0.03079(6) 0.02460(6) 0.02533(6) -0.00475(4) 0.00084(4) 0.00013(4) P1 0.0211(3) 0.0210(3) 0.0212(3) 0.0005(2) 0.0013(2) 0.0013(2) P2 0.0213(3) 0.0204(3) 0.0245(3) -0.0016(2) -0.0026(2) -0.0013(2) Si1 0.0260(4) 0.0401(4) 0.0497(5) 0.0011(4) 0.0097(3) 0.0108(3) Si2 0.0208(3) 0.0362(4) 0.0362(4) 0.0030(3) -0.0001(3) -0.0035(3) N1 0.0216(10) 0.0289(11) 0.0294(12) 0.0019(9) 0.0030(8) 0.0055(8) N2 0.0194(9) 0.0294(11) 0.0326(12) -0.0054(9) 0.0005(8) -0.0028(8) C1 0.0212(11) 0.0240(12) 0.0216(12) -0.0007(9) -0.0009(9) -0.0005(9) C11 0.0254(11) 0.0232(12) 0.0213(12) 0.0036(9) 0.0048(9) 0.0000(9) C12 0.0300(13) 0.0298(13) 0.0267(13) 0.0006(11) 0.0000(10) 0.0004(10) C13 0.0404(15) 0.0323(14) 0.0398(17) -0.0077(13) -0.0041(13) -0.0055(12) C14 0.0521(18) 0.0234(13) 0.0389(17) -0.0018(12) 0.0046(14) -0.0023(12) C15 0.0406(16) 0.0256(14) 0.0434(17) 0.0049(12) 0.0025(13) 0.0077(11) C16 0.0290(13) 0.0273(13) 0.0342(15) 0.0043(11) 0.0003(11) 0.0016(10) C17 0.054(2) 0.065(3) 0.096(3) 0.015(2) 0.043(2) 0.0074(19) C18 0.074(3) 0.056(2) 0.102(4) -0.020(2) 0.025(3) 0.026(2) C19 0.0322(18) 0.123(4) 0.081(3) 0.003(3) -0.0079(19) 0.023(2) C21 0.0293(13) 0.0389(15) 0.0227(13) -0.0009(11) 0.0046(10) -0.0018(11) C22 0.0567(19) 0.0426(17) 0.0305(16) -0.0052(13) 0.0095(14) 0.0034(15) C23 0.082(3) 0.062(2) 0.039(2) -0.0209(18) 0.0069(19) 0.002(2) C24 0.090(3) 0.088(3) 0.0233(17) -0.0074(19) 0.0032(18) 0.007(3) C25 0.093(3) 0.072(3) 0.0285(18) 0.0093(18) 0.0060(19) 0.007(2) C26 0.056(2) 0.0447(18) 0.0276(16) 0.0048(13) 0.0011(14) -0.0012(14) C27 0.0318(16) 0.104(3) 0.053(2) -0.010(2) 0.0097(15) 0.0046(19) C28 0.0336(19) 0.075(3) 0.131(5) -0.039(3) 0.003(2) -0.0178(18) C29 0.0331(18) 0.126(4) 0.104(4) 0.070(4) -0.009(2) 0.003(2) C31 0.0295(13) 0.0222(12) 0.0327(14) -0.0012(10) -0.0072(11) -0.0034(10) C32 0.0450(16) 0.0298(14) 0.0323(15) 0.0011(12) -0.0065(12) -0.0069(12) C33 0.063(2) 0.0365(17) 0.0360(17) 0.0109(13) -0.0129(15) -0.0139(15) C34 0.058(2) 0.0264(14) 0.052(2) 0.0031(13) -0.0223(17) -0.0009(13) C35 0.0519(19) 0.0270(14) 0.057(2) -0.0036(14) -0.0084(16) 0.0055(13) C36 0.0423(16) 0.0255(13) 0.0475(18) 0.0001(12) -0.0022(13) 0.0028(12) C41 0.0244(12) 0.0314(13) 0.0272(13) -0.0036(11) -0.0035(10) 0.0006(10) C42 0.0394(16) 0.0394(17) 0.0399(17) -0.0113(13) -0.0078(13) -0.0015(13) C43 0.052(2) 0.059(2) 0.047(2) -0.0242(17) -0.0177(16) -0.0006(16) C44 0.055(2) 0.075(3) 0.0343(18) -0.0062(18) -0.0189(15) 0.0020(19) C45 0.0507(19) 0.057(2) 0.0395(18) 0.0085(15) -0.0158(15) 0.0034(16) C46 0.0382(15) 0.0366(15) 0.0336(15) 0.0002(12) -0.0128(12) 0.0013(12) _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 Tl1 N1 2.471(2) . ? Tl1 C1 2.635(2) . ? Tl1 P1 3.0960(7) . ? Tl1 Tl2 3.4828(3) 3_666 ? Tl2 C1 2.415(2) . ? Tl2 N2 2.504(2) . ? Tl2 P2 3.0444(7) . ? Tl2 Tl1 3.4828(3) 3_666 ? P1 N1 1.589(2) . ? P1 C1 1.711(2) . ? P1 C21 1.831(3) . ? P1 C11 1.834(3) . ? P2 N2 1.595(2) . ? P2 C1 1.707(2) . ? P2 C41 1.819(3) . ? P2 C31 1.833(3) . ? Si1 N1 1.700(2) . ? Si1 C18 1.854(4) . ? Si1 C19 1.861(4) . ? Si1 C17 1.864(4) . ? Si2 N2 1.708(2) . ? Si2 C27 1.849(4) . ? Si2 C29 1.851(4) . ? Si2 C28 1.872(4) . ? C11 C12 1.390(4) . ? C11 C16 1.397(4) . ? C12 C13 1.389(4) . ? C13 C14 1.386(4) . ? C14 C15 1.384(4) . ? C15 C16 1.387(4) . ? C21 C22 1.390(4) . ? C21 C26 1.390(4) . ? C22 C23 1.386(5) . ? C23 C24 1.380(6) . ? C24 C25 1.365(6) . ? C25 C26 1.395(5) . ? C31 C32 1.383(4) . ? C31 C36 1.403(4) . ? C32 C33 1.395(4) . ? C33 C34 1.377(6) . ? C34 C35 1.367(5) . ? C35 C36 1.392(4) . ? C41 C42 1.394(4) . ? C41 C46 1.401(4) . ? C42 C43 1.396(5) . ? C43 C44 1.371(6) . ? C44 C45 1.388(5) . ? C45 C46 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tl1 C1 64.03(7) . . ? N1 Tl1 P1 30.63(5) . . ? C1 Tl1 P1 33.53(5) . . ? N1 Tl1 Tl2 85.44(5) . 3_666 ? C1 Tl1 Tl2 88.18(5) . 3_666 ? P1 Tl1 Tl2 84.008(13) . 3_666 ? C1 Tl2 N2 65.55(7) . . ? C1 Tl2 P2 34.03(6) . . ? N2 Tl2 P2 31.54(5) . . ? C1 Tl2 Tl1 139.55(6) . 3_666 ? N2 Tl2 Tl1 154.55(5) . 3_666 ? P2 Tl2 Tl1 172.257(13) . 3_666 ? N1 P1 C1 110.36(12) . . ? N1 P1 C21 110.11(12) . . ? C1 P1 C21 115.78(12) . . ? N1 P1 C11 109.82(12) . . ? C1 P1 C11 105.63(11) . . ? C21 P1 C11 104.80(12) . . ? N1 P1 Tl1 52.38(8) . . ? C1 P1 Tl1 58.28(8) . . ? C21 P1 Tl1 137.64(10) . . ? C11 P1 Tl1 117.32(8) . . ? N2 P2 C1 107.49(12) . . ? N2 P2 C41 111.49(12) . . ? C1 P2 C41 114.08(12) . . ? N2 P2 C31 109.52(13) . . ? C1 P2 C31 109.15(12) . . ? C41 P2 C31 105.04(12) . . ? N2 P2 Tl2 55.21(8) . . ? C1 P2 Tl2 52.33(8) . . ? C41 P2 Tl2 128.83(9) . . ? C31 P2 Tl2 126.13(9) . . ? N1 Si1 C18 110.62(18) . . ? N1 Si1 C19 106.99(16) . . ? C18 Si1 C19 107.8(3) . . ? N1 Si1 C17 113.99(15) . . ? C18 Si1 C17 107.8(2) . . ? C19 Si1 C17 109.5(2) . . ? N2 Si2 C27 107.48(14) . . ? N2 Si2 C29 111.99(16) . . ? C27 Si2 C29 108.3(2) . . ? N2 Si2 C28 112.83(16) . . ? C27 Si2 C28 108.4(2) . . ? C29 Si2 C28 107.7(3) . . ? P1 N1 Si1 139.43(15) . . ? P1 N1 Tl1 96.99(10) . . ? Si1 N1 Tl1 122.43(11) . . ? P2 N2 Si2 133.59(14) . . ? P2 N2 Tl2 93.24(9) . . ? Si2 N2 Tl2 129.28(12) . . ? P2 C1 P1 137.70(16) . . ? P2 C1 Tl2 93.64(10) . . ? P1 C1 Tl2 120.69(12) . . ? P2 C1 Tl1 108.64(11) . . ? P1 C1 Tl1 88.19(9) . . ? Tl2 C1 Tl1 103.15(9) . . ? C12 C11 C16 118.4(2) . . ? C12 C11 P1 119.55(19) . . ? C16 C11 P1 121.92(19) . . ? C13 C12 C11 120.4(3) . . ? C14 C13 C12 120.7(3) . . ? C15 C14 C13 119.6(3) . . ? C14 C15 C16 119.8(3) . . ? C15 C16 C11 121.2(3) . . ? C22 C21 C26 118.3(3) . . ? C22 C21 P1 117.3(2) . . ? C26 C21 P1 124.4(2) . . ? C23 C22 C21 121.1(3) . . ? C24 C23 C22 119.7(4) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.6(4) . . ? C21 C26 C25 120.1(3) . . ? C32 C31 C36 118.1(3) . . ? C32 C31 P2 120.1(2) . . ? C36 C31 P2 121.2(2) . . ? C31 C32 C33 120.6(3) . . ? C34 C33 C32 120.3(3) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 120.2(3) . . ? C35 C36 C31 120.7(3) . . ? C42 C41 C46 118.3(3) . . ? C42 C41 P2 124.4(2) . . ? C46 C41 P2 117.2(2) . . ? C41 C42 C43 119.6(3) . . ? C44 C43 C42 121.2(3) . . ? C43 C44 C45 119.7(3) . . ? C46 C45 C44 119.6(3) . . ? C45 C46 C41 121.5(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 C1 Tl1 P1 N1 -173.06(14) . . . . ? Tl2 Tl1 P1 N1 91.17(10) 3_666 . . . ? N1 Tl1 P1 C1 173.06(14) . . . . ? Tl2 Tl1 P1 C1 -95.77(10) 3_666 . . . ? N1 Tl1 P1 C21 78.42(17) . . . . ? C1 Tl1 P1 C21 -94.64(16) . . . . ? Tl2 Tl1 P1 C21 169.58(13) 3_666 . . . ? N1 Tl1 P1 C11 -94.81(14) . . . . ? C1 Tl1 P1 C11 92.13(13) . . . . ? Tl2 Tl1 P1 C11 -3.64(9) 3_666 . . . ? C1 Tl2 P2 N2 176.92(15) . . . . ? Tl1 Tl2 P2 N2 -146.11(12) 3_666 . . . ? N2 Tl2 P2 C1 -176.92(15) . . . . ? Tl1 Tl2 P2 C1 36.97(14) 3_666 . . . ? C1 Tl2 P2 C41 -92.31(15) . . . . ? N2 Tl2 P2 C41 90.77(15) . . . . ? Tl1 Tl2 P2 C41 -55.34(15) 3_666 . . . ? C1 Tl2 P2 C31 87.11(15) . . . . ? N2 Tl2 P2 C31 -89.81(15) . . . . ? Tl1 Tl2 P2 C31 124.08(13) 3_666 . . . ? C1 P1 N1 Si1 160.6(2) . . . . ? C21 P1 N1 Si1 31.5(3) . . . . ? C11 P1 N1 Si1 -83.4(2) . . . . ? Tl1 P1 N1 Si1 166.9(3) . . . . ? C1 P1 N1 Tl1 -6.30(13) . . . . ? C21 P1 N1 Tl1 -135.34(11) . . . . ? C11 P1 N1 Tl1 109.76(10) . . . . ? C18 Si1 N1 P1 -94.2(3) . . . . ? C19 Si1 N1 P1 148.6(3) . . . . ? C17 Si1 N1 P1 27.4(3) . . . . ? C18 Si1 N1 Tl1 70.3(2) . . . . ? C19 Si1 N1 Tl1 -46.9(2) . . . . ? C17 Si1 N1 Tl1 -168.1(2) . . . . ? C1 Tl1 N1 P1 4.26(9) . . . . ? Tl2 Tl1 N1 P1 -85.94(9) 3_666 . . . ? C1 Tl1 N1 Si1 -165.66(16) . . . . ? P1 Tl1 N1 Si1 -169.9(2) . . . . ? Tl2 Tl1 N1 Si1 104.14(13) 3_666 . . . ? C1 P2 N2 Si2 160.91(19) . . . . ? C41 P2 N2 Si2 35.2(2) . . . . ? C31 P2 N2 Si2 -80.6(2) . . . . ? Tl2 P2 N2 Si2 158.4(2) . . . . ? C1 P2 N2 Tl2 2.56(12) . . . . ? C41 P2 N2 Tl2 -123.16(11) . . . . ? C31 P2 N2 Tl2 121.02(10) . . . . ? C27 Si2 N2 P2 158.0(2) . . . . ? C29 Si2 N2 P2 -83.2(3) . . . . ? C28 Si2 N2 P2 38.6(3) . . . . ? C27 Si2 N2 Tl2 -50.4(2) . . . . ? C29 Si2 N2 Tl2 68.4(3) . . . . ? C28 Si2 N2 Tl2 -169.8(2) . . . . ? C1 Tl2 N2 P2 -1.89(9) . . . . ? Tl1 Tl2 N2 P2 169.93(4) 3_666 . . . ? C1 Tl2 N2 Si2 -161.70(18) . . . . ? P2 Tl2 N2 Si2 -159.8(2) . . . . ? Tl1 Tl2 N2 Si2 10.1(3) 3_666 . . . ? N2 P2 C1 P1 -148.7(2) . . . . ? C41 P2 C1 P1 -24.6(3) . . . . ? C31 P2 C1 P1 92.6(2) . . . . ? Tl2 P2 C1 P1 -146.1(3) . . . . ? N2 P2 C1 Tl2 -2.65(13) . . . . ? C41 P2 C1 Tl2 121.51(11) . . . . ? C31 P2 C1 Tl2 -121.36(11) . . . . ? N2 P2 C1 Tl1 102.53(13) . . . . ? C41 P2 C1 Tl1 -133.31(12) . . . . ? C31 P2 C1 Tl1 -16.17(15) . . . . ? Tl2 P2 C1 Tl1 105.18(12) . . . . ? N1 P1 C1 P2 -110.3(2) . . . . ? C21 P1 C1 P2 15.6(3) . . . . ? C11 P1 C1 P2 131.1(2) . . . . ? Tl1 P1 C1 P2 -116.1(2) . . . . ? N1 P1 C1 Tl2 110.09(14) . . . . ? C21 P1 C1 Tl2 -124.00(14) . . . . ? C11 P1 C1 Tl2 -8.56(16) . . . . ? Tl1 P1 C1 Tl2 104.23(13) . . . . ? N1 P1 C1 Tl1 5.86(12) . . . . ? C21 P1 C1 Tl1 131.77(11) . . . . ? C11 P1 C1 Tl1 -112.79(10) . . . . ? N2 Tl2 C1 P2 1.77(9) . . . . ? Tl1 Tl2 C1 P2 -172.83(3) 3_666 . . . ? N2 Tl2 C1 P1 155.88(16) . . . . ? P2 Tl2 C1 P1 154.1(2) . . . . ? Tl1 Tl2 C1 P1 -18.72(19) 3_666 . . . ? N2 Tl2 C1 Tl1 -108.33(10) . . . . ? P2 Tl2 C1 Tl1 -110.10(13) . . . . ? Tl1 Tl2 C1 Tl1 77.08(11) 3_666 . . . ? N1 Tl1 C1 P2 136.46(14) . . . . ? P1 Tl1 C1 P2 140.38(18) . . . . ? Tl2 Tl1 C1 P2 -137.73(11) 3_666 . . . ? N1 Tl1 C1 P1 -3.93(8) . . . . ? Tl2 Tl1 C1 P1 81.89(8) 3_666 . . . ? N1 Tl1 C1 Tl2 -125.06(10) . . . . ? P1 Tl1 C1 Tl2 -121.14(13) . . . . ? Tl2 Tl1 C1 Tl2 -39.25(7) 3_666 . . . ? N1 P1 C11 C12 0.1(2) . . . . ? C1 P1 C11 C12 119.1(2) . . . . ? C21 P1 C11 C12 -118.1(2) . . . . ? Tl1 P1 C11 C12 57.2(2) . . . . ? N1 P1 C11 C16 -175.9(2) . . . . ? C1 P1 C11 C16 -56.9(2) . . . . ? C21 P1 C11 C16 65.9(2) . . . . ? Tl1 P1 C11 C16 -118.8(2) . . . . ? C16 C11 C12 C13 0.2(4) . . . . ? P1 C11 C12 C13 -176.0(2) . . . . ? C11 C12 C13 C14 -0.4(5) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C14 C15 C16 C11 -1.2(5) . . . . ? C12 C11 C16 C15 0.6(4) . . . . ? P1 C11 C16 C15 176.7(2) . . . . ? N1 P1 C21 C22 58.3(3) . . . . ? C1 P1 C21 C22 -67.7(3) . . . . ? C11 P1 C21 C22 176.4(2) . . . . ? Tl1 P1 C21 C22 2.6(3) . . . . ? N1 P1 C21 C26 -120.7(3) . . . . ? C1 P1 C21 C26 113.3(3) . . . . ? C11 P1 C21 C26 -2.6(3) . . . . ? Tl1 P1 C21 C26 -176.4(2) . . . . ? C26 C21 C22 C23 -1.1(5) . . . . ? P1 C21 C22 C23 179.8(3) . . . . ? C21 C22 C23 C24 2.3(6) . . . . ? C22 C23 C24 C25 -1.8(7) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C22 C21 C26 C25 -0.7(5) . . . . ? P1 C21 C26 C25 178.3(3) . . . . ? C24 C25 C26 C21 1.2(7) . . . . ? N2 P2 C31 C32 -13.5(2) . . . . ? C1 P2 C31 C32 104.0(2) . . . . ? C41 P2 C31 C32 -133.3(2) . . . . ? Tl2 P2 C31 C32 47.2(2) . . . . ? N2 P2 C31 C36 175.3(2) . . . . ? C1 P2 C31 C36 -67.3(3) . . . . ? C41 P2 C31 C36 55.4(2) . . . . ? Tl2 P2 C31 C36 -124.1(2) . . . . ? C36 C31 C32 C33 0.5(4) . . . . ? P2 C31 C32 C33 -171.1(2) . . . . ? C31 C32 C33 C34 -0.7(4) . . . . ? C32 C33 C34 C35 0.5(5) . . . . ? C33 C34 C35 C36 0.0(5) . . . . ? C34 C35 C36 C31 -0.3(5) . . . . ? C32 C31 C36 C35 0.0(4) . . . . ? P2 C31 C36 C35 171.5(2) . . . . ? N2 P2 C41 C42 -105.1(3) . . . . ? C1 P2 C41 C42 132.9(2) . . . . ? C31 P2 C41 C42 13.4(3) . . . . ? Tl2 P2 C41 C42 -167.1(2) . . . . ? N2 P2 C41 C46 72.2(2) . . . . ? C1 P2 C41 C46 -49.8(3) . . . . ? C31 P2 C41 C46 -169.2(2) . . . . ? Tl2 P2 C41 C46 10.3(3) . . . . ? C46 C41 C42 C43 1.3(5) . . . . ? P2 C41 C42 C43 178.6(3) . . . . ? C41 C42 C43 C44 -0.4(5) . . . . ? C42 C43 C44 C45 -0.8(6) . . . . ? C43 C44 C45 C46 0.8(6) . . . . ? C44 C45 C46 C41 0.2(5) . . . . ? C42 C41 C46 C45 -1.3(5) . . . . ? P2 C41 C46 C45 -178.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.288 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.097 #===END