# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 894365' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H28 P2 Si Zr' _chemical_formula_sum 'C17 H28 P2 Si Zr' _chemical_formula_weight 413.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' 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 14.7244(3) _cell_length_b 10.5735(2) _cell_length_c 26.3663(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4104.93(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6886 _cell_measurement_theta_min 2.3715 _cell_measurement_theta_max 27.926 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84609 _exptl_absorpt_correction_T_max 0.939582 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20414 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8435 _reflns_number_gt 7107 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0650P)^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 0.57(4) _refine_ls_number_reflns 8435 _refine_ls_number_parameters 392 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 Zr1 Zr 0.26376(2) -0.05809(3) 0.322885(14) 0.01649(9) Uani 1 1 d . . . P1 P 0.30743(8) 0.12287(11) 0.38752(5) 0.0269(3) Uani 1 1 d . . . C1 C 0.2523(3) 0.1538(4) 0.33426(16) 0.0213(9) Uani 1 1 d . . . Si1 Si 0.21108(8) 0.30482(11) 0.30834(5) 0.0253(3) Uani 1 1 d . . . C2 C 0.1558(4) 0.4034(5) 0.3588(2) 0.0388(12) Uani 1 1 d . . . H2A H 0.0981 0.3645 0.3687 0.058 Uiso 1 1 calc R . . H2B H 0.1445 0.4886 0.3456 0.058 Uiso 1 1 calc R . . H2C H 0.1960 0.4086 0.3883 0.058 Uiso 1 1 calc R . . C3 C 0.3108(4) 0.3969(5) 0.2829(2) 0.0430(13) Uani 1 1 d . . . H3A H 0.3539 0.4135 0.3104 0.064 Uiso 1 1 calc R . . H3B H 0.2894 0.4773 0.2687 0.064 Uiso 1 1 calc R . . H3C H 0.3408 0.3476 0.2562 0.064 Uiso 1 1 calc R . . C4 C 0.1260(3) 0.2791(5) 0.25662(19) 0.0384(11) Uani 1 1 d . . . H4A H 0.1529 0.2261 0.2301 0.058 Uiso 1 1 calc R . . H4B H 0.1084 0.3609 0.2421 0.058 Uiso 1 1 calc R . . H4C H 0.0723 0.2369 0.2706 0.058 Uiso 1 1 calc R . . P2 P 0.35509(6) -0.17853(10) 0.39635(4) 0.0187(2) Uani 1 1 d . . . C5 C 0.4702(3) -0.1212(4) 0.40812(18) 0.0286(10) Uani 1 1 d . . . H5A H 0.4679 -0.0317 0.4177 0.043 Uiso 1 1 calc R . . H5B H 0.5067 -0.1309 0.3773 0.043 Uiso 1 1 calc R . . H5C H 0.4977 -0.1702 0.4357 0.043 Uiso 1 1 calc R . . C6 C 0.3071(3) -0.1694(4) 0.45942(17) 0.0274(9) Uani 1 1 d . . . H6A H 0.2477 -0.2113 0.4598 0.041 Uiso 1 1 calc R . . H6B H 0.2998 -0.0805 0.4691 0.041 Uiso 1 1 calc R . . H6C H 0.3477 -0.2116 0.4835 0.041 Uiso 1 1 calc R . . C7 C 0.3749(3) -0.3490(4) 0.39086(17) 0.0284(10) Uani 1 1 d . . . H7A H 0.4132 -0.3774 0.4190 0.043 Uiso 1 1 calc R . . H7B H 0.4054 -0.3670 0.3586 0.043 Uiso 1 1 calc R . . H7C H 0.3167 -0.3937 0.3920 0.043 Uiso 1 1 calc R . . C8 C 0.1271(3) -0.0987(4) 0.37844(18) 0.0255(9) Uani 1 1 d . . . H8 H 0.1221 -0.0773 0.4153 0.031 Uiso 1 1 calc R . . C9 C 0.1526(3) -0.2172(4) 0.3584(2) 0.0306(11) Uani 1 1 d . . . H9 H 0.1689 -0.2937 0.3787 0.037 Uiso 1 1 calc R . . C10 C 0.1382(3) -0.2145(5) 0.3063(2) 0.0385(12) Uani 1 1 d . . . H10 H 0.1422 -0.2891 0.2831 0.046 Uiso 1 1 calc R . . C11 C 0.1033(3) -0.0951(5) 0.2934(2) 0.0369(12) Uani 1 1 d . . . H11 H 0.0782 -0.0708 0.2595 0.044 Uiso 1 1 calc R . . C12 C 0.0959(3) -0.0234(4) 0.33806(18) 0.0296(10) Uani 1 1 d . . . H12 H 0.0650 0.0605 0.3413 0.036 Uiso 1 1 calc R . . C13 C 0.2939(3) -0.0687(4) 0.22892(17) 0.0318(11) Uani 1 1 d . . . H13 H 0.2474 -0.0611 0.2015 0.038 Uiso 1 1 calc R . . C14 C 0.3491(3) 0.0309(5) 0.24787(18) 0.0346(11) Uani 1 1 d . . . H14 H 0.3472 0.1209 0.2362 0.041 Uiso 1 1 calc R . . C15 C 0.4150(3) -0.0215(5) 0.27879(19) 0.0358(11) Uani 1 1 d . . . H15 H 0.4678 0.0252 0.2936 0.043 Uiso 1 1 calc R . . C16 C 0.4036(3) -0.1547(5) 0.27965(18) 0.0334(11) Uani 1 1 d . . . H16 H 0.4464 -0.2172 0.2951 0.040 Uiso 1 1 calc R . . C17 C 0.3284(3) -0.1832(4) 0.24925(17) 0.0311(10) Uani 1 1 d . . . H17 H 0.3090 -0.2701 0.2390 0.037 Uiso 1 1 calc R . . Zr2 Zr 0.44270(2) 0.56044(3) 0.087081(14) 0.01573(9) Uani 1 1 d . . . P3 P 0.48188(8) 0.38413(10) 0.01944(4) 0.0243(2) Uani 1 1 d . . . C18 C 0.4254(3) 0.3503(4) 0.07213(16) 0.0214(9) Uani 1 1 d . . . Si2 Si 0.38052(8) 0.19990(10) 0.09619(5) 0.0244(3) Uani 1 1 d . . . C19 C 0.2831(3) 0.2301(5) 0.13986(19) 0.0398(12) Uani 1 1 d . . . H19A H 0.2998 0.2963 0.1641 0.060 Uiso 1 1 calc R . . H19B H 0.2682 0.1522 0.1582 0.060 Uiso 1 1 calc R . . H19C H 0.2303 0.2575 0.1201 0.060 Uiso 1 1 calc R . . C20 C 0.4720(3) 0.1117(4) 0.1299(2) 0.0390(12) Uani 1 1 d . . . H20A H 0.5229 0.0970 0.1066 0.058 Uiso 1 1 calc R . . H20B H 0.4482 0.0303 0.1417 0.058 Uiso 1 1 calc R . . H20C H 0.4930 0.1613 0.1590 0.058 Uiso 1 1 calc R . . C21 C 0.3374(4) 0.0972(4) 0.0438(2) 0.0379(12) Uani 1 1 d . . . H21A H 0.2846 0.1375 0.0279 0.057 Uiso 1 1 calc R . . H21B H 0.3197 0.0148 0.0576 0.057 Uiso 1 1 calc R . . H21C H 0.3853 0.0856 0.0184 0.057 Uiso 1 1 calc R . . P4 P 0.53390(7) 0.68392(10) 0.01439(4) 0.0193(2) Uani 1 1 d . . . C22 C 0.6474(3) 0.6246(4) 0.00097(18) 0.0263(10) Uani 1 1 d . . . H22A H 0.6731 0.6708 -0.0279 0.039 Uiso 1 1 calc R . . H22B H 0.6441 0.5343 -0.0073 0.039 Uiso 1 1 calc R . . H22C H 0.6861 0.6366 0.0308 0.039 Uiso 1 1 calc R . . C23 C 0.4826(3) 0.6814(4) -0.04905(16) 0.0295(10) Uani 1 1 d . . . H23A H 0.5224 0.7256 -0.0730 0.044 Uiso 1 1 calc R . . H23B H 0.4234 0.7237 -0.0480 0.044 Uiso 1 1 calc R . . H23C H 0.4745 0.5936 -0.0601 0.044 Uiso 1 1 calc R . . C24 C 0.5571(3) 0.8531(4) 0.02226(19) 0.0297(10) Uani 1 1 d . . . H24A H 0.5920 0.8665 0.0534 0.045 Uiso 1 1 calc R . . H24B H 0.4996 0.8995 0.0244 0.045 Uiso 1 1 calc R . . H24C H 0.5920 0.8839 -0.0069 0.045 Uiso 1 1 calc R . . C25 C 0.3055(3) 0.6110(4) 0.03357(17) 0.0240(9) Uani 1 1 d . . . H25 H 0.2985 0.5923 -0.0034 0.029 Uiso 1 1 calc R . . C26 C 0.2735(3) 0.5350(4) 0.07385(19) 0.0283(10) Uani 1 1 d . . . H26 H 0.2408 0.4526 0.0701 0.034 Uiso 1 1 calc R . . C27 C 0.2842(3) 0.6019(5) 0.1191(2) 0.0330(11) Uani 1 1 d . . . H27 H 0.2600 0.5756 0.1529 0.040 Uiso 1 1 calc R . . C28 C 0.3204(3) 0.7227(4) 0.10727(19) 0.0342(11) Uani 1 1 d . . . H28 H 0.3264 0.7957 0.1312 0.041 Uiso 1 1 calc R . . C29 C 0.3343(3) 0.7265(4) 0.05458(18) 0.0282(10) Uani 1 1 d . . . H29 H 0.3520 0.8032 0.0348 0.034 Uiso 1 1 calc R . . C30 C 0.5276(4) 0.4620(4) 0.1596(2) 0.0398(14) Uani 1 1 d . . . H30 H 0.5246 0.3712 0.1701 0.048 Uiso 1 1 calc R . . C31 C 0.4768(3) 0.5600(4) 0.18006(18) 0.0355(12) Uani 1 1 d . . . H31 H 0.4306 0.5507 0.2076 0.043 Uiso 1 1 calc R . . C32 C 0.5119(3) 0.6756(5) 0.16261(17) 0.0316(10) Uani 1 1 d . . . H32 H 0.4944 0.7616 0.1751 0.038 Uiso 1 1 calc R . . C33 C 0.5847(3) 0.6477(5) 0.13057(17) 0.0331(11) Uani 1 1 d . . . H33 H 0.6277 0.7108 0.1157 0.040 Uiso 1 1 calc R . . C34 C 0.5944(3) 0.5165(5) 0.12841(19) 0.0367(12) Uani 1 1 d . . . H34 H 0.6462 0.4703 0.1124 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 Zr1 0.01720(17) 0.01614(17) 0.01614(18) 0.00011(17) -0.00037(15) -0.00032(14) P1 0.0340(6) 0.0211(5) 0.0255(6) -0.0038(5) -0.0077(5) 0.0003(5) C1 0.0184(19) 0.0165(19) 0.029(3) -0.0041(17) -0.0012(16) 0.0012(16) Si1 0.0310(6) 0.0180(5) 0.0268(6) 0.0018(5) -0.0014(5) 0.0016(5) C2 0.049(3) 0.027(2) 0.040(3) 0.002(2) 0.010(3) 0.006(2) C3 0.058(3) 0.027(2) 0.044(3) 0.005(2) 0.013(3) -0.001(2) C4 0.043(3) 0.037(3) 0.035(3) 0.008(2) -0.008(2) 0.009(2) P2 0.0190(5) 0.0181(5) 0.0190(5) 0.0005(4) 0.0001(4) 0.0012(4) C5 0.026(2) 0.025(2) 0.035(3) 0.003(2) -0.004(2) 0.0033(18) C6 0.028(2) 0.033(2) 0.021(2) 0.0043(18) 0.0013(17) 0.0026(19) C7 0.039(2) 0.019(2) 0.028(2) 0.0014(18) -0.006(2) 0.0075(19) C8 0.0171(19) 0.030(2) 0.029(2) 0.0071(19) 0.0039(18) -0.0009(17) C9 0.021(2) 0.023(2) 0.048(3) 0.007(2) 0.000(2) -0.0040(17) C10 0.033(3) 0.034(3) 0.049(3) -0.013(2) 0.000(2) -0.016(2) C11 0.022(2) 0.054(3) 0.036(3) 0.006(2) -0.012(2) -0.010(2) C12 0.0150(19) 0.035(2) 0.039(3) 0.006(2) -0.0018(18) -0.0026(18) C13 0.040(3) 0.039(3) 0.017(2) 0.0002(19) 0.000(2) 0.006(2) C14 0.042(3) 0.037(3) 0.025(2) 0.007(2) 0.010(2) 0.002(2) C15 0.029(2) 0.048(3) 0.030(3) -0.003(2) 0.011(2) -0.006(2) C16 0.036(3) 0.036(3) 0.028(2) 0.004(2) 0.009(2) 0.016(2) C17 0.046(3) 0.024(2) 0.023(2) -0.0066(19) 0.006(2) 0.005(2) Zr2 0.01580(16) 0.01589(17) 0.01550(18) -0.00035(17) -0.00166(14) 0.00034(13) P3 0.0310(6) 0.0195(5) 0.0223(6) -0.0025(5) 0.0049(5) -0.0013(5) C18 0.0213(19) 0.022(2) 0.021(2) -0.0015(16) 0.0008(16) -0.0040(17) Si2 0.0301(6) 0.0171(5) 0.0259(7) 0.0019(5) -0.0038(5) -0.0029(5) C19 0.050(3) 0.029(3) 0.040(3) 0.007(2) 0.007(2) -0.007(2) C20 0.044(3) 0.027(2) 0.047(3) 0.008(2) -0.012(2) -0.006(2) C21 0.052(3) 0.019(2) 0.042(3) 0.001(2) -0.013(2) -0.006(2) P4 0.0183(5) 0.0196(5) 0.0199(5) 0.0009(4) -0.0021(4) -0.0018(4) C22 0.022(2) 0.024(2) 0.033(3) 0.0017(19) 0.0022(18) -0.0016(17) C23 0.034(2) 0.031(2) 0.023(2) 0.0069(19) -0.0051(19) -0.012(2) C24 0.025(2) 0.021(2) 0.042(3) 0.001(2) 0.004(2) -0.0033(18) C25 0.019(2) 0.028(2) 0.025(2) 0.0039(18) -0.0044(17) 0.0009(18) C26 0.0132(19) 0.032(2) 0.040(3) 0.007(2) -0.0007(18) -0.0027(17) C27 0.023(2) 0.045(3) 0.031(3) 0.005(2) 0.008(2) 0.012(2) C28 0.025(2) 0.033(2) 0.044(3) -0.011(2) 0.001(2) 0.016(2) C29 0.0190(19) 0.023(2) 0.043(3) 0.001(2) -0.007(2) 0.0049(17) C30 0.062(4) 0.023(2) 0.034(3) 0.007(2) -0.031(3) -0.004(2) C31 0.038(3) 0.050(3) 0.018(2) 0.000(2) -0.004(2) -0.009(2) C32 0.034(2) 0.033(3) 0.028(2) -0.011(2) -0.010(2) -0.005(2) C33 0.026(2) 0.047(3) 0.027(2) 0.004(2) -0.010(2) -0.010(2) C34 0.028(2) 0.048(3) 0.034(3) -0.012(2) -0.018(2) 0.014(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 Zr1 C1 2.267(4) . ? Zr1 C11 2.518(4) . ? Zr1 C13 2.519(5) . ? Zr1 C10 2.518(4) . ? Zr1 C8 2.525(4) . ? Zr1 C14 2.525(5) . ? Zr1 C9 2.526(4) . ? Zr1 C12 2.531(4) . ? Zr1 C17 2.535(4) . ? Zr1 C15 2.542(5) . ? Zr1 C16 2.566(4) . ? Zr1 P1 2.6418(12) . ? Zr1 P2 2.6799(11) . ? P1 C1 1.654(4) . ? C1 Si1 1.840(4) . ? Si1 C4 1.871(5) . ? Si1 C2 1.875(5) . ? Si1 C3 1.885(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P2 C6 1.810(4) . ? P2 C5 1.827(4) . ? P2 C7 1.831(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C12 1.407(6) . ? C8 C9 1.411(6) . ? C8 H8 1.0000 . ? C9 C10 1.389(7) . ? C9 H9 1.0000 . ? C10 C11 1.406(7) . ? C10 H10 1.0000 . ? C11 C12 1.405(7) . ? C11 H11 1.0000 . ? C12 H12 1.0000 . ? C13 C17 1.418(6) . ? C13 C14 1.420(7) . ? C13 H13 1.0000 . ? C14 C15 1.384(7) . ? C14 H14 1.0000 . ? C15 C16 1.418(7) . ? C15 H15 1.0000 . ? C16 C17 1.400(7) . ? C16 H16 1.0000 . ? C17 H17 1.0000 . ? Zr2 C18 2.271(4) . ? Zr2 C31 2.502(5) . ? Zr2 C30 2.511(4) . ? Zr2 C27 2.520(4) . ? Zr2 C25 2.521(4) . ? Zr2 C29 2.523(4) . ? Zr2 C34 2.528(4) . ? Zr2 C26 2.530(4) . ? Zr2 C28 2.544(4) . ? Zr2 C32 2.547(4) . ? Zr2 C33 2.557(4) . ? Zr2 P3 2.6436(12) . ? Zr2 P4 2.6797(11) . ? P3 C18 1.658(4) . ? C18 Si2 1.835(4) . ? Si2 C20 1.864(5) . ? Si2 C19 1.866(5) . ? Si2 C21 1.868(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? P4 C22 1.820(4) . ? P4 C24 1.833(4) . ? P4 C23 1.836(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C29 1.406(6) . ? C25 C26 1.413(6) . ? C25 H25 1.0000 . ? C26 C27 1.395(7) . ? C26 H26 1.0000 . ? C27 C28 1.419(7) . ? C27 H27 1.0000 . ? C28 C29 1.405(6) . ? C28 H28 1.0000 . ? C29 H29 1.0000 . ? C30 C31 1.388(7) . ? C30 C34 1.405(8) . ? C30 H30 1.0000 . ? C31 C32 1.404(6) . ? C31 H31 1.0000 . ? C32 C33 1.396(6) . ? C32 H32 1.0000 . ? C33 C34 1.396(7) . ? C33 H33 1.0000 . ? C34 H34 1.0000 . ? 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 C1 Zr1 C11 97.16(16) . . ? C1 Zr1 C13 100.78(15) . . ? C11 Zr1 C13 81.65(17) . . ? C1 Zr1 C10 128.16(15) . . ? C11 Zr1 C10 32.43(16) . . ? C13 Zr1 C10 85.97(17) . . ? C1 Zr1 C8 91.84(15) . . ? C11 Zr1 C8 53.50(16) . . ? C13 Zr1 C8 134.69(16) . . ? C10 Zr1 C8 53.44(16) . . ? C1 Zr1 C14 76.83(16) . . ? C11 Zr1 C14 106.43(17) . . ? C13 Zr1 C14 32.71(15) . . ? C10 Zr1 C14 118.30(17) . . ? C8 Zr1 C14 156.07(15) . . ? C1 Zr1 C9 124.12(14) . . ? C11 Zr1 C9 53.37(16) . . ? C13 Zr1 C9 116.68(16) . . ? C10 Zr1 C9 31.97(17) . . ? C8 Zr1 C9 32.43(14) . . ? C14 Zr1 C9 149.38(16) . . ? C1 Zr1 C12 76.31(14) . . ? C11 Zr1 C12 32.30(16) . . ? C13 Zr1 C12 109.51(16) . . ? C10 Zr1 C12 53.55(16) . . ? C8 Zr1 C12 32.31(14) . . ? C14 Zr1 C12 123.76(15) . . ? C9 Zr1 C12 53.51(15) . . ? C1 Zr1 C17 130.16(15) . . ? C11 Zr1 C17 92.00(17) . . ? C13 Zr1 C17 32.59(14) . . ? C10 Zr1 C17 78.46(16) . . ? C8 Zr1 C17 130.90(16) . . ? C14 Zr1 C17 53.68(16) . . ? C9 Zr1 C17 100.35(16) . . ? C12 Zr1 C17 124.30(16) . . ? C1 Zr1 C15 88.58(15) . . ? C11 Zr1 C15 134.80(17) . . ? C13 Zr1 C15 53.32(17) . . ? C10 Zr1 C15 131.57(17) . . ? C8 Zr1 C15 171.55(16) . . ? C14 Zr1 C15 31.70(16) . . ? C9 Zr1 C15 146.95(16) . . ? C12 Zr1 C15 154.97(16) . . ? C17 Zr1 C15 53.13(16) . . ? C1 Zr1 C16 120.78(15) . . ? C11 Zr1 C16 123.65(17) . . ? C13 Zr1 C16 53.41(15) . . ? C10 Zr1 C16 104.51(16) . . ? C8 Zr1 C16 146.05(15) . . ? C14 Zr1 C16 53.20(15) . . ? C9 Zr1 C16 114.80(15) . . ? C12 Zr1 C16 155.76(16) . . ? C17 Zr1 C16 31.86(15) . . ? C15 Zr1 C16 32.23(15) . . ? C1 Zr1 P1 38.44(11) . . ? C11 Zr1 P1 122.69(13) . . ? C13 Zr1 P1 128.58(11) . . ? C10 Zr1 P1 140.02(12) . . ? C8 Zr1 P1 86.72(11) . . ? C14 Zr1 P1 96.56(12) . . ? C9 Zr1 P1 113.63(12) . . ? C12 Zr1 P1 91.77(11) . . ? C17 Zr1 P1 141.32(12) . . ? C15 Zr1 P1 88.37(12) . . ? C16 Zr1 P1 112.30(12) . . ? P1 Zr1 P2 75.86(4) . . ? C1 Zr1 P2 114.28(11) . . ? C1 P1 Zr1 58.43(14) . . ? P1 C1 Si1 130.5(2) . . ? P1 C1 Zr1 83.13(17) . . ? Si1 C1 Zr1 146.4(2) . . ? C1 Si1 C4 111.5(2) . . ? C1 Si1 C2 111.2(2) . . ? C4 Si1 C2 107.9(2) . . ? C1 Si1 C3 108.9(2) . . ? C4 Si1 C3 109.7(2) . . ? C2 Si1 C3 107.7(2) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 P2 C5 100.9(2) . . ? C6 P2 C7 100.8(2) . . ? C5 P2 C7 101.08(19) . . ? C6 P2 Zr1 116.29(15) . . ? C5 P2 Zr1 115.51(15) . . ? C7 P2 Zr1 119.38(15) . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P2 C7 H7A 109.5 . . ? P2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C8 C9 107.8(4) . . ? C12 C8 Zr1 74.1(2) . . ? C9 C8 Zr1 73.8(2) . . ? C12 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Zr1 C8 H8 125.7 . . ? C10 C9 C8 108.2(4) . . ? C10 C9 Zr1 73.7(3) . . ? C8 C9 Zr1 73.7(2) . . ? C10 C9 H9 125.6 . . ? C8 C9 H9 125.6 . . ? Zr1 C9 H9 125.6 . . ? C9 C10 C11 108.3(4) . . ? C9 C10 Zr1 74.3(3) . . ? C11 C10 Zr1 73.8(3) . . ? C9 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? Zr1 C10 H10 125.5 . . ? C10 C11 C12 108.0(4) . . ? C10 C11 Zr1 73.8(3) . . ? C12 C11 Zr1 74.4(3) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? Zr1 C11 H11 125.6 . . ? C8 C12 C11 107.7(4) . . ? C8 C12 Zr1 73.6(2) . . ? C11 C12 Zr1 73.3(3) . . ? C8 C12 H12 125.8 . . ? C11 C12 H12 125.8 . . ? Zr1 C12 H12 125.8 . . ? C17 C13 C14 107.2(4) . . ? C17 C13 Zr1 74.3(3) . . ? C14 C13 Zr1 73.9(3) . . ? C17 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Zr1 C13 H13 126.0 . . ? C15 C14 C13 108.1(4) . . ? C15 C14 Zr1 74.8(3) . . ? C13 C14 Zr1 73.4(3) . . ? C15 C14 H14 125.5 . . ? C13 C14 H14 125.5 . . ? Zr1 C14 H14 125.5 . . ? C14 C15 C16 108.9(4) . . ? C14 C15 Zr1 73.5(3) . . ? C16 C15 Zr1 74.8(3) . . ? C14 C15 H15 125.2 . . ? C16 C15 H15 125.2 . . ? Zr1 C15 H15 125.2 . . ? C17 C16 C15 107.4(4) . . ? C17 C16 Zr1 72.9(3) . . ? C15 C16 Zr1 73.0(3) . . ? C17 C16 H16 126.1 . . ? C15 C16 H16 126.1 . . ? Zr1 C16 H16 126.1 . . ? C16 C17 C13 108.4(4) . . ? C16 C17 Zr1 75.3(3) . . ? C13 C17 Zr1 73.1(3) . . ? C16 C17 H17 125.4 . . ? C13 C17 H17 125.4 . . ? Zr1 C17 H17 125.4 . . ? C18 Zr2 C31 101.00(15) . . ? C18 Zr2 C30 77.44(15) . . ? C31 Zr2 C30 32.13(16) . . ? C18 Zr2 C27 97.16(16) . . ? C31 Zr2 C27 81.84(17) . . ? C30 Zr2 C27 106.17(18) . . ? C18 Zr2 C25 91.18(14) . . ? C31 Zr2 C25 135.17(16) . . ? C30 Zr2 C25 155.94(16) . . ? C27 Zr2 C25 53.73(15) . . ? C18 Zr2 C29 123.44(14) . . ? C31 Zr2 C29 117.44(16) . . ? C30 Zr2 C29 149.57(17) . . ? C27 Zr2 C29 53.60(16) . . ? C25 Zr2 C29 32.38(14) . . ? C18 Zr2 C34 89.65(16) . . ? C31 Zr2 C34 53.15(17) . . ? C30 Zr2 C34 32.38(17) . . ? C27 Zr2 C34 134.90(17) . . ? C25 Zr2 C34 171.10(16) . . ? C29 Zr2 C34 146.44(16) . . ? C18 Zr2 C26 76.21(15) . . ? C31 Zr2 C26 109.41(16) . . ? C30 Zr2 C26 123.46(17) . . ? C27 Zr2 C26 32.08(16) . . ? C25 Zr2 C26 32.49(14) . . ? C29 Zr2 C26 53.43(15) . . ? C34 Zr2 C26 155.47(17) . . ? C18 Zr2 C28 128.10(15) . . ? C31 Zr2 C28 86.45(16) . . ? C30 Zr2 C28 118.21(17) . . ? C27 Zr2 C28 32.53(16) . . ? C25 Zr2 C28 53.63(15) . . ? C29 Zr2 C28 32.19(14) . . ? C34 Zr2 C28 131.24(16) . . ? C26 Zr2 C28 53.38(15) . . ? C18 Zr2 C32 130.41(15) . . ? C31 Zr2 C32 32.28(15) . . ? C30 Zr2 C32 53.36(16) . . ? C27 Zr2 C32 91.47(16) . . ? C25 Zr2 C32 131.06(15) . . ? C29 Zr2 C32 100.73(15) . . ? C34 Zr2 C32 52.94(15) . . ? C26 Zr2 C32 123.55(16) . . ? C28 Zr2 C32 78.30(15) . . ? C18 Zr2 C33 121.50(16) . . ? C31 Zr2 C33 52.93(16) . . ? C30 Zr2 C33 53.17(16) . . ? C27 Zr2 C33 122.98(16) . . ? C25 Zr2 C33 146.07(15) . . ? C29 Zr2 C33 114.75(15) . . ? C34 Zr2 C33 31.86(16) . . ? C26 Zr2 C33 154.88(16) . . ? C28 Zr2 C33 103.98(16) . . ? C32 Zr2 C33 31.74(15) . . ? C18 Zr2 P3 38.50(11) . . ? C31 Zr2 P3 128.02(12) . . ? C30 Zr2 P3 96.49(12) . . ? C27 Zr2 P3 123.41(13) . . ? C25 Zr2 P3 86.95(11) . . ? C29 Zr2 P3 113.55(11) . . ? C34 Zr2 P3 88.19(12) . . ? C26 Zr2 P3 92.68(12) . . ? C28 Zr2 P3 140.47(11) . . ? C32 Zr2 P3 141.01(11) . . ? C33 Zr2 P3 112.25(11) . . ? P3 Zr2 P4 75.62(3) . . ? C18 Zr2 P4 114.12(11) . . ? C18 P3 Zr2 58.50(14) . . ? P3 C18 Si2 131.1(2) . . ? P3 C18 Zr2 83.00(16) . . ? Si2 C18 Zr2 145.9(2) . . ? C18 Si2 C20 109.8(2) . . ? C18 Si2 C19 110.0(2) . . ? C20 Si2 C19 110.3(2) . . ? C18 Si2 C21 111.7(2) . . ? C20 Si2 C21 107.9(2) . . ? C19 Si2 C21 107.1(2) . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 P4 C24 100.81(19) . . ? C22 P4 C23 101.3(2) . . ? C24 P4 C23 101.2(2) . . ? C22 P4 Zr2 115.54(15) . . ? C24 P4 Zr2 119.20(16) . . ? C23 P4 Zr2 115.99(14) . . ? P4 C22 H22A 109.5 . . ? P4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P4 C23 H23A 109.5 . . ? P4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P4 C24 H24A 109.5 . . ? P4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C29 C25 C26 107.4(4) . . ? C29 C25 Zr2 73.9(2) . . ? C26 C25 Zr2 74.1(2) . . ? C29 C25 H25 125.9 . . ? C26 C25 H25 125.9 . . ? Zr2 C25 H25 125.9 . . ? C27 C26 C25 108.4(4) . . ? C27 C26 Zr2 73.6(2) . . ? C25 C26 Zr2 73.4(2) . . ? C27 C26 H26 125.5 . . ? C25 C26 H26 125.5 . . ? Zr2 C26 H26 125.5 . . ? C26 C27 C28 108.2(4) . . ? C26 C27 Zr2 74.3(3) . . ? C28 C27 Zr2 74.7(2) . . ? C26 C27 H27 125.5 . . ? C28 C27 H27 125.5 . . ? Zr2 C27 H27 125.5 . . ? C29 C28 C27 107.3(4) . . ? C29 C28 Zr2 73.1(3) . . ? C27 C28 Zr2 72.8(2) . . ? C29 C28 H28 126.1 . . ? C27 C28 H28 126.1 . . ? Zr2 C28 H28 126.1 . . ? C25 C29 C28 108.8(4) . . ? C25 C29 Zr2 73.7(2) . . ? C28 C29 Zr2 74.7(3) . . ? C25 C29 H29 125.3 . . ? C28 C29 H29 125.3 . . ? Zr2 C29 H29 125.3 . . ? C31 C30 C34 107.4(4) . . ? C31 C30 Zr2 73.6(3) . . ? C34 C30 Zr2 74.5(3) . . ? C31 C30 H30 125.9 . . ? C34 C30 H30 125.9 . . ? Zr2 C30 H30 125.9 . . ? C30 C31 C32 108.9(4) . . ? C30 C31 Zr2 74.3(3) . . ? C32 C31 Zr2 75.6(3) . . ? C30 C31 H31 125.1 . . ? C32 C31 H31 125.1 . . ? Zr2 C31 H31 125.1 . . ? C33 C32 C31 107.3(4) . . ? C33 C32 Zr2 74.5(3) . . ? C31 C32 Zr2 72.1(3) . . ? C33 C32 H32 126.0 . . ? C31 C32 H32 126.0 . . ? Zr2 C32 H32 126.0 . . ? C32 C33 C34 108.3(4) . . ? C32 C33 Zr2 73.7(2) . . ? C34 C33 Zr2 72.9(2) . . ? C32 C33 H33 125.6 . . ? C34 C33 H33 125.6 . . ? Zr2 C33 H33 125.6 . . ? C33 C34 C30 108.2(4) . . ? C33 C34 Zr2 75.2(2) . . ? C30 C34 Zr2 73.2(3) . . ? C33 C34 H34 125.5 . . ? C30 C34 H34 125.5 . . ? Zr2 C34 H34 125.5 . . ? 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 C11 Zr1 P1 C1 -55.2(2) . . . . ? C13 Zr1 P1 C1 51.7(2) . . . . ? C10 Zr1 P1 C1 -92.5(3) . . . . ? C8 Zr1 P1 C1 -97.11(19) . . . . ? C14 Zr1 P1 C1 59.1(2) . . . . ? C9 Zr1 P1 C1 -115.7(2) . . . . ? C12 Zr1 P1 C1 -65.19(19) . . . . ? C17 Zr1 P1 C1 95.0(2) . . . . ? C15 Zr1 P1 C1 89.8(2) . . . . ? C16 Zr1 P1 C1 111.9(2) . . . . ? Zr1 P1 C1 Si1 180.0(4) . . . . ? C11 Zr1 C1 P1 135.82(17) . . . . ? C13 Zr1 C1 P1 -141.36(17) . . . . ? C10 Zr1 C1 P1 125.28(19) . . . . ? C8 Zr1 C1 P1 82.39(16) . . . . ? C14 Zr1 C1 P1 -118.92(18) . . . . ? C9 Zr1 C1 P1 85.7(2) . . . . ? C12 Zr1 C1 P1 110.97(18) . . . . ? C17 Zr1 C1 P1 -125.44(19) . . . . ? C15 Zr1 C1 P1 -89.17(17) . . . . ? C16 Zr1 C1 P1 -87.7(2) . . . . ? C11 Zr1 C1 Si1 -44.2(4) . . . . ? C13 Zr1 C1 Si1 38.7(4) . . . . ? C10 Zr1 C1 Si1 -54.7(5) . . . . ? C8 Zr1 C1 Si1 -97.6(4) . . . . ? C14 Zr1 C1 Si1 61.1(4) . . . . ? C9 Zr1 C1 Si1 -94.3(4) . . . . ? C12 Zr1 C1 Si1 -69.0(4) . . . . ? C17 Zr1 C1 Si1 54.6(4) . . . . ? C15 Zr1 C1 Si1 90.8(4) . . . . ? C16 Zr1 C1 Si1 92.3(4) . . . . ? P1 Zr1 C1 Si1 -180.0(5) . . . . ? P1 C1 Si1 C4 -164.0(3) . . . . ? Zr1 C1 Si1 C4 16.0(4) . . . . ? P1 C1 Si1 C2 -43.5(4) . . . . ? Zr1 C1 Si1 C2 136.4(4) . . . . ? P1 C1 Si1 C3 75.0(4) . . . . ? Zr1 C1 Si1 C3 -105.1(4) . . . . ? C1 Zr1 P2 C6 61.9(2) . . . . ? C11 Zr1 P2 C6 -60.2(2) . . . . ? C13 Zr1 P2 C6 -171.5(2) . . . . ? C10 Zr1 P2 C6 -78.7(2) . . . . ? C8 Zr1 P2 C6 -27.6(2) . . . . ? C14 Zr1 P2 C6 150.1(2) . . . . ? C9 Zr1 P2 C6 -59.2(2) . . . . ? C12 Zr1 P2 C6 -24.4(2) . . . . ? C17 Zr1 P2 C6 -158.2(2) . . . . ? C15 Zr1 P2 C6 149.4(2) . . . . ? C16 Zr1 P2 C6 179.0(2) . . . . ? P1 Zr1 P2 C6 60.50(17) . . . . ? C1 Zr1 P2 C5 -56.1(2) . . . . ? C11 Zr1 P2 C5 -178.2(2) . . . . ? C13 Zr1 P2 C5 70.5(2) . . . . ? C10 Zr1 P2 C5 163.3(2) . . . . ? C8 Zr1 P2 C5 -145.5(2) . . . . ? C14 Zr1 P2 C5 32.1(2) . . . . ? C9 Zr1 P2 C5 -177.2(2) . . . . ? C12 Zr1 P2 C5 -142.3(2) . . . . ? C17 Zr1 P2 C5 83.9(2) . . . . ? C15 Zr1 P2 C5 31.4(2) . . . . ? C16 Zr1 P2 C5 61.1(2) . . . . ? P1 Zr1 P2 C5 -57.45(17) . . . . ? C1 Zr1 P2 C7 -177.0(2) . . . . ? C11 Zr1 P2 C7 61.0(2) . . . . ? C13 Zr1 P2 C7 -50.4(2) . . . . ? C10 Zr1 P2 C7 42.5(2) . . . . ? C8 Zr1 P2 C7 93.6(2) . . . . ? C14 Zr1 P2 C7 -88.8(2) . . . . ? C9 Zr1 P2 C7 62.0(2) . . . . ? C12 Zr1 P2 C7 96.8(2) . . . . ? C17 Zr1 P2 C7 -37.0(2) . . . . ? C15 Zr1 P2 C7 -89.5(2) . . . . ? C16 Zr1 P2 C7 -59.8(2) . . . . ? P1 Zr1 P2 C7 -178.33(18) . . . . ? C1 Zr1 C8 C12 60.4(3) . . . . ? C11 Zr1 C8 C12 -37.1(3) . . . . ? C13 Zr1 C8 C12 -46.7(4) . . . . ? C10 Zr1 C8 C12 -77.8(3) . . . . ? C14 Zr1 C8 C12 -0.3(6) . . . . ? C9 Zr1 C8 C12 -114.5(4) . . . . ? C17 Zr1 C8 C12 -91.4(3) . . . . ? C15 Zr1 C8 C12 153.1(10) . . . . ? C16 Zr1 C8 C12 -134.9(3) . . . . ? P1 Zr1 C8 C12 98.5(3) . . . . ? C1 Zr1 C8 C9 174.9(3) . . . . ? C11 Zr1 C8 C9 77.3(3) . . . . ? C13 Zr1 C8 C9 67.7(3) . . . . ? C10 Zr1 C8 C9 36.7(3) . . . . ? C14 Zr1 C8 C9 114.2(4) . . . . ? C12 Zr1 C8 C9 114.5(4) . . . . ? C17 Zr1 C8 C9 23.0(3) . . . . ? C15 Zr1 C8 C9 -92.4(11) . . . . ? C16 Zr1 C8 C9 -20.4(4) . . . . ? P1 Zr1 C8 C9 -147.0(3) . . . . ? C12 C8 C9 C10 0.6(5) . . . . ? Zr1 C8 C9 C10 -66.2(3) . . . . ? C12 C8 C9 Zr1 66.8(3) . . . . ? C1 Zr1 C9 C10 108.9(3) . . . . ? C11 Zr1 C9 C10 37.3(3) . . . . ? C13 Zr1 C9 C10 -17.5(3) . . . . ? C8 Zr1 C9 C10 115.1(4) . . . . ? C14 Zr1 C9 C10 -18.3(5) . . . . ? C12 Zr1 C9 C10 77.8(3) . . . . ? C17 Zr1 C9 C10 -47.4(3) . . . . ? C15 Zr1 C9 C10 -80.5(4) . . . . ? C16 Zr1 C9 C10 -77.3(3) . . . . ? P1 Zr1 C9 C10 151.5(3) . . . . ? C1 Zr1 C9 C8 -6.2(3) . . . . ? C11 Zr1 C9 C8 -77.8(3) . . . . ? C13 Zr1 C9 C8 -132.6(3) . . . . ? C10 Zr1 C9 C8 -115.1(4) . . . . ? C14 Zr1 C9 C8 -133.4(3) . . . . ? C12 Zr1 C9 C8 -37.2(3) . . . . ? C17 Zr1 C9 C8 -162.5(3) . . . . ? C15 Zr1 C9 C8 164.4(3) . . . . ? C16 Zr1 C9 C8 167.6(3) . . . . ? P1 Zr1 C9 C8 36.4(3) . . . . ? C8 C9 C10 C11 -0.3(5) . . . . ? Zr1 C9 C10 C11 -66.5(3) . . . . ? C8 C9 C10 Zr1 66.2(3) . . . . ? C1 Zr1 C10 C9 -95.1(3) . . . . ? C11 Zr1 C10 C9 -114.9(4) . . . . ? C13 Zr1 C10 C9 164.4(3) . . . . ? C8 Zr1 C10 C9 -37.2(3) . . . . ? C14 Zr1 C10 C9 169.5(3) . . . . ? C12 Zr1 C10 C9 -77.7(3) . . . . ? C17 Zr1 C10 C9 132.3(3) . . . . ? C15 Zr1 C10 C9 134.0(3) . . . . ? C16 Zr1 C10 C9 113.8(3) . . . . ? P1 Zr1 C10 C9 -42.9(4) . . . . ? C1 Zr1 C10 C11 19.8(4) . . . . ? C13 Zr1 C10 C11 -80.8(3) . . . . ? C8 Zr1 C10 C11 77.7(3) . . . . ? C14 Zr1 C10 C11 -75.6(3) . . . . ? C9 Zr1 C10 C11 114.9(4) . . . . ? C12 Zr1 C10 C11 37.2(3) . . . . ? C17 Zr1 C10 C11 -112.8(3) . . . . ? C15 Zr1 C10 C11 -111.1(3) . . . . ? C16 Zr1 C10 C11 -131.3(3) . . . . ? P1 Zr1 C10 C11 72.0(4) . . . . ? C9 C10 C11 C12 -0.1(5) . . . . ? Zr1 C10 C11 C12 -67.0(3) . . . . ? C9 C10 C11 Zr1 66.9(3) . . . . ? C1 Zr1 C11 C10 -164.4(3) . . . . ? C13 Zr1 C11 C10 95.7(3) . . . . ? C8 Zr1 C11 C10 -77.5(3) . . . . ? C14 Zr1 C11 C10 117.2(3) . . . . ? C9 Zr1 C11 C10 -36.8(3) . . . . ? C12 Zr1 C11 C10 -114.6(4) . . . . ? C17 Zr1 C11 C10 64.7(3) . . . . ? C15 Zr1 C11 C10 100.4(3) . . . . ? C16 Zr1 C11 C10 60.9(4) . . . . ? P1 Zr1 C11 C10 -133.4(3) . . . . ? C1 Zr1 C11 C12 -49.8(3) . . . . ? C13 Zr1 C11 C12 -149.7(3) . . . . ? C10 Zr1 C11 C12 114.6(4) . . . . ? C8 Zr1 C11 C12 37.1(3) . . . . ? C14 Zr1 C11 C12 -128.2(3) . . . . ? C9 Zr1 C11 C12 77.8(3) . . . . ? C17 Zr1 C11 C12 179.3(3) . . . . ? C15 Zr1 C11 C12 -145.0(3) . . . . ? C16 Zr1 C11 C12 175.5(3) . . . . ? P1 Zr1 C11 C12 -18.8(3) . . . . ? C9 C8 C12 C11 -0.7(5) . . . . ? Zr1 C8 C12 C11 66.0(3) . . . . ? C9 C8 C12 Zr1 -66.7(3) . . . . ? C10 C11 C12 C8 0.5(5) . . . . ? Zr1 C11 C12 C8 -66.1(3) . . . . ? C10 C11 C12 Zr1 66.7(3) . . . . ? C1 Zr1 C12 C8 -116.5(3) . . . . ? C11 Zr1 C12 C8 114.7(4) . . . . ? C13 Zr1 C12 C8 146.7(3) . . . . ? C10 Zr1 C12 C8 77.4(3) . . . . ? C14 Zr1 C12 C8 179.9(3) . . . . ? C9 Zr1 C12 C8 37.4(3) . . . . ? C17 Zr1 C12 C8 113.9(3) . . . . ? C15 Zr1 C12 C8 -171.0(3) . . . . ? C16 Zr1 C12 C8 105.6(4) . . . . ? P1 Zr1 C12 C8 -81.0(3) . . . . ? C1 Zr1 C12 C11 128.7(3) . . . . ? C13 Zr1 C12 C11 31.9(3) . . . . ? C10 Zr1 C12 C11 -37.3(3) . . . . ? C8 Zr1 C12 C11 -114.7(4) . . . . ? C14 Zr1 C12 C11 65.1(3) . . . . ? C9 Zr1 C12 C11 -77.4(3) . . . . ? C17 Zr1 C12 C11 -0.9(3) . . . . ? C15 Zr1 C12 C11 74.3(5) . . . . ? C16 Zr1 C12 C11 -9.2(5) . . . . ? P1 Zr1 C12 C11 164.2(3) . . . . ? C1 Zr1 C13 C17 157.1(3) . . . . ? C11 Zr1 C13 C17 -107.1(3) . . . . ? C10 Zr1 C13 C17 -74.8(3) . . . . ? C8 Zr1 C13 C17 -99.4(3) . . . . ? C14 Zr1 C13 C17 113.6(4) . . . . ? C9 Zr1 C13 C17 -65.6(3) . . . . ? C12 Zr1 C13 C17 -123.7(3) . . . . ? C15 Zr1 C13 C17 77.1(3) . . . . ? C16 Zr1 C13 C17 36.6(3) . . . . ? P1 Zr1 C13 C17 127.3(3) . . . . ? C1 Zr1 C13 C14 43.5(3) . . . . ? C11 Zr1 C13 C14 139.2(3) . . . . ? C10 Zr1 C13 C14 171.6(3) . . . . ? C8 Zr1 C13 C14 147.0(3) . . . . ? C9 Zr1 C13 C14 -179.2(3) . . . . ? C12 Zr1 C13 C14 122.6(3) . . . . ? C17 Zr1 C13 C14 -113.6(4) . . . . ? C15 Zr1 C13 C14 -36.5(3) . . . . ? C16 Zr1 C13 C14 -77.0(3) . . . . ? P1 Zr1 C13 C14 13.7(3) . . . . ? C17 C13 C14 C15 0.0(5) . . . . ? Zr1 C13 C14 C15 67.4(3) . . . . ? C17 C13 C14 Zr1 -67.4(3) . . . . ? C1 Zr1 C14 C15 109.3(3) . . . . ? C11 Zr1 C14 C15 -157.0(3) . . . . ? C13 Zr1 C14 C15 -114.7(4) . . . . ? C10 Zr1 C14 C15 -124.2(3) . . . . ? C8 Zr1 C14 C15 172.8(4) . . . . ? C9 Zr1 C14 C15 -113.3(4) . . . . ? C12 Zr1 C14 C15 172.6(3) . . . . ? C17 Zr1 C14 C15 -76.9(3) . . . . ? C16 Zr1 C14 C15 -36.9(3) . . . . ? P1 Zr1 C14 C15 76.1(3) . . . . ? C1 Zr1 C14 C13 -136.0(3) . . . . ? C11 Zr1 C14 C13 -42.3(3) . . . . ? C10 Zr1 C14 C13 -9.6(3) . . . . ? C8 Zr1 C14 C13 -72.5(5) . . . . ? C9 Zr1 C14 C13 1.3(5) . . . . ? C12 Zr1 C14 C13 -72.7(3) . . . . ? C17 Zr1 C14 C13 37.8(3) . . . . ? C15 Zr1 C14 C13 114.7(4) . . . . ? C16 Zr1 C14 C13 77.7(3) . . . . ? P1 Zr1 C14 C13 -169.3(3) . . . . ? C13 C14 C15 C16 0.6(5) . . . . ? Zr1 C14 C15 C16 67.0(3) . . . . ? C13 C14 C15 Zr1 -66.4(3) . . . . ? C1 Zr1 C15 C14 -66.8(3) . . . . ? C11 Zr1 C15 C14 31.9(4) . . . . ? C13 Zr1 C15 C14 37.8(3) . . . . ? C10 Zr1 C15 C14 76.7(4) . . . . ? C8 Zr1 C15 C14 -159.8(10) . . . . ? C9 Zr1 C15 C14 121.0(3) . . . . ? C12 Zr1 C15 C14 -14.6(5) . . . . ? C17 Zr1 C15 C14 78.8(3) . . . . ? C16 Zr1 C15 C14 115.5(4) . . . . ? P1 Zr1 C15 C14 -105.3(3) . . . . ? C1 Zr1 C15 C16 177.7(3) . . . . ? C11 Zr1 C15 C16 -83.6(4) . . . . ? C13 Zr1 C15 C16 -77.8(3) . . . . ? C10 Zr1 C15 C16 -38.8(4) . . . . ? C8 Zr1 C15 C16 84.7(11) . . . . ? C14 Zr1 C15 C16 -115.5(4) . . . . ? C9 Zr1 C15 C16 5.5(5) . . . . ? C12 Zr1 C15 C16 -130.1(4) . . . . ? C17 Zr1 C15 C16 -36.7(3) . . . . ? P1 Zr1 C15 C16 139.2(3) . . . . ? C14 C15 C16 C17 -0.9(5) . . . . ? Zr1 C15 C16 C17 65.2(3) . . . . ? C14 C15 C16 Zr1 -66.1(3) . . . . ? C1 Zr1 C16 C17 -117.6(3) . . . . ? C11 Zr1 C16 C17 7.2(4) . . . . ? C13 Zr1 C16 C17 -37.5(3) . . . . ? C10 Zr1 C16 C17 36.1(3) . . . . ? C8 Zr1 C16 C17 80.3(4) . . . . ? C14 Zr1 C16 C17 -78.6(3) . . . . ? C9 Zr1 C16 C17 68.4(3) . . . . ? C12 Zr1 C16 C17 13.1(5) . . . . ? C15 Zr1 C16 C17 -114.9(4) . . . . ? P1 Zr1 C16 C17 -159.8(2) . . . . ? C1 Zr1 C16 C15 -2.7(3) . . . . ? C11 Zr1 C16 C15 122.1(3) . . . . ? C13 Zr1 C16 C15 77.4(3) . . . . ? C10 Zr1 C16 C15 151.0(3) . . . . ? C8 Zr1 C16 C15 -164.8(3) . . . . ? C14 Zr1 C16 C15 36.3(3) . . . . ? C9 Zr1 C16 C15 -176.7(3) . . . . ? C12 Zr1 C16 C15 128.0(4) . . . . ? C17 Zr1 C16 C15 114.9(4) . . . . ? P1 Zr1 C16 C15 -44.9(3) . . . . ? C15 C16 C17 C13 0.9(5) . . . . ? Zr1 C16 C17 C13 66.2(3) . . . . ? C15 C16 C17 Zr1 -65.3(3) . . . . ? C14 C13 C17 C16 -0.5(5) . . . . ? Zr1 C13 C17 C16 -67.6(3) . . . . ? C14 C13 C17 Zr1 67.1(3) . . . . ? C1 Zr1 C17 C16 84.9(3) . . . . ? C11 Zr1 C17 C16 -174.0(3) . . . . ? C13 Zr1 C17 C16 114.9(4) . . . . ? C10 Zr1 C17 C16 -144.4(3) . . . . ? C8 Zr1 C17 C16 -133.3(3) . . . . ? C14 Zr1 C17 C16 77.0(3) . . . . ? C9 Zr1 C17 C16 -120.9(3) . . . . ? C12 Zr1 C17 C16 -173.6(3) . . . . ? C15 Zr1 C17 C16 37.2(3) . . . . ? P1 Zr1 C17 C16 30.7(4) . . . . ? C1 Zr1 C17 C13 -30.0(4) . . . . ? C11 Zr1 C17 C13 71.1(3) . . . . ? C10 Zr1 C17 C13 100.7(3) . . . . ? C8 Zr1 C17 C13 111.9(3) . . . . ? C14 Zr1 C17 C13 -37.9(3) . . . . ? C9 Zr1 C17 C13 124.2(3) . . . . ? C12 Zr1 C17 C13 71.6(3) . . . . ? C15 Zr1 C17 C13 -77.7(3) . . . . ? C16 Zr1 C17 C13 -114.9(4) . . . . ? P1 Zr1 C17 C13 -84.2(3) . . . . ? C31 Zr2 P3 C18 53.6(2) . . . . ? C30 Zr2 P3 C18 60.4(2) . . . . ? C27 Zr2 P3 C18 -53.9(2) . . . . ? C25 Zr2 P3 C18 -95.74(19) . . . . ? C29 Zr2 P3 C18 -114.7(2) . . . . ? C34 Zr2 P3 C18 91.7(2) . . . . ? C26 Zr2 P3 C18 -63.8(2) . . . . ? C28 Zr2 P3 C18 -91.9(2) . . . . ? C32 Zr2 P3 C18 95.9(2) . . . . ? C33 Zr2 P3 C18 113.1(2) . . . . ? Zr2 P3 C18 Si2 -179.3(4) . . . . ? C31 Zr2 C18 P3 -139.79(17) . . . . ? C30 Zr2 C18 P3 -117.8(2) . . . . ? C27 Zr2 C18 P3 137.18(17) . . . . ? C25 Zr2 C18 P3 83.60(16) . . . . ? C29 Zr2 C18 P3 86.5(2) . . . . ? C34 Zr2 C18 P3 -87.54(18) . . . . ? C26 Zr2 C18 P3 112.70(18) . . . . ? C28 Zr2 C18 P3 126.06(18) . . . . ? C32 Zr2 C18 P3 -124.71(19) . . . . ? C33 Zr2 C18 P3 -86.7(2) . . . . ? C31 Zr2 C18 Si2 39.3(4) . . . . ? C30 Zr2 C18 Si2 61.3(4) . . . . ? C27 Zr2 C18 Si2 -43.7(4) . . . . ? C25 Zr2 C18 Si2 -97.3(4) . . . . ? C29 Zr2 C18 Si2 -94.4(4) . . . . ? C34 Zr2 C18 Si2 91.6(4) . . . . ? C26 Zr2 C18 Si2 -68.2(4) . . . . ? C28 Zr2 C18 Si2 -54.8(5) . . . . ? C32 Zr2 C18 Si2 54.4(5) . . . . ? C33 Zr2 C18 Si2 92.4(4) . . . . ? P3 Zr2 C18 Si2 179.1(5) . . . . ? P3 C18 Si2 C20 83.8(4) . . . . ? Zr2 C18 Si2 C20 -95.0(4) . . . . ? P3 C18 Si2 C19 -154.7(3) . . . . ? Zr2 C18 Si2 C19 26.5(5) . . . . ? P3 C18 Si2 C21 -35.9(4) . . . . ? Zr2 C18 Si2 C21 145.3(4) . . . . ? C18 Zr2 P4 C22 -57.3(2) . . . . ? C31 Zr2 P4 C22 69.4(2) . . . . ? C30 Zr2 P4 C22 31.6(2) . . . . ? C27 Zr2 P4 C22 -179.1(2) . . . . ? C25 Zr2 P4 C22 -145.99(19) . . . . ? C29 Zr2 P4 C22 -177.5(2) . . . . ? C34 Zr2 P4 C22 31.1(2) . . . . ? C26 Zr2 P4 C22 -143.4(2) . . . . ? C28 Zr2 P4 C22 162.61(19) . . . . ? C32 Zr2 P4 C22 83.27(19) . . . . ? C33 Zr2 P4 C22 60.8(2) . . . . ? P3 Zr2 P4 C22 -57.65(16) . . . . ? C18 Zr2 P4 C24 -177.7(2) . . . . ? C31 Zr2 P4 C24 -50.9(2) . . . . ? C30 Zr2 P4 C24 -88.7(2) . . . . ? C27 Zr2 P4 C24 60.6(2) . . . . ? C25 Zr2 P4 C24 93.7(2) . . . . ? C29 Zr2 P4 C24 62.1(2) . . . . ? C34 Zr2 P4 C24 -89.2(2) . . . . ? C26 Zr2 P4 C24 96.2(2) . . . . ? C28 Zr2 P4 C24 42.3(2) . . . . ? C32 Zr2 P4 C24 -37.1(2) . . . . ? C33 Zr2 P4 C24 -59.6(2) . . . . ? P3 Zr2 P4 C24 -178.00(17) . . . . ? C18 Zr2 P4 C23 61.0(2) . . . . ? C31 Zr2 P4 C23 -172.2(2) . . . . ? C30 Zr2 P4 C23 150.0(2) . . . . ? C27 Zr2 P4 C23 -60.8(2) . . . . ? C25 Zr2 P4 C23 -27.6(2) . . . . ? C29 Zr2 P4 C23 -59.2(2) . . . . ? C34 Zr2 P4 C23 149.5(2) . . . . ? C26 Zr2 P4 C23 -25.1(2) . . . . ? C28 Zr2 P4 C23 -79.0(2) . . . . ? C32 Zr2 P4 C23 -158.4(2) . . . . ? C33 Zr2 P4 C23 179.1(2) . . . . ? P3 Zr2 P4 C23 60.69(18) . . . . ? C18 Zr2 C25 C29 175.5(3) . . . . ? C31 Zr2 C25 C29 68.5(3) . . . . ? C30 Zr2 C25 C29 114.7(4) . . . . ? C27 Zr2 C25 C29 77.4(3) . . . . ? C34 Zr2 C25 C29 -89.3(11) . . . . ? C26 Zr2 C25 C29 113.9(4) . . . . ? C28 Zr2 C25 C29 36.8(3) . . . . ? C32 Zr2 C25 C29 24.1(3) . . . . ? C33 Zr2 C25 C29 -19.4(4) . . . . ? P3 Zr2 C25 C29 -146.2(3) . . . . ? C18 Zr2 C25 C26 61.6(3) . . . . ? C31 Zr2 C25 C26 -45.4(4) . . . . ? C30 Zr2 C25 C26 0.7(5) . . . . ? C27 Zr2 C25 C26 -36.5(3) . . . . ? C29 Zr2 C25 C26 -113.9(4) . . . . ? C34 Zr2 C25 C26 156.8(10) . . . . ? C28 Zr2 C25 C26 -77.1(3) . . . . ? C32 Zr2 C25 C26 -89.8(3) . . . . ? C33 Zr2 C25 C26 -133.3(3) . . . . ? P3 Zr2 C25 C26 99.8(3) . . . . ? C29 C25 C26 C27 -1.2(5) . . . . ? Zr2 C25 C26 C27 65.8(3) . . . . ? C29 C25 C26 Zr2 -66.9(3) . . . . ? C18 Zr2 C26 C27 129.3(3) . . . . ? C31 Zr2 C26 C27 32.3(3) . . . . ? C30 Zr2 C26 C27 64.8(3) . . . . ? C25 Zr2 C26 C27 -115.6(4) . . . . ? C29 Zr2 C26 C27 -78.0(3) . . . . ? C34 Zr2 C26 C27 72.9(5) . . . . ? C28 Zr2 C26 C27 -37.6(3) . . . . ? C32 Zr2 C26 C27 -0.4(3) . . . . ? C33 Zr2 C26 C27 -8.8(5) . . . . ? P3 Zr2 C26 C27 164.4(3) . . . . ? C18 Zr2 C26 C25 -115.1(3) . . . . ? C31 Zr2 C26 C25 147.9(3) . . . . ? C30 Zr2 C26 C25 -179.6(3) . . . . ? C27 Zr2 C26 C25 115.6(4) . . . . ? C29 Zr2 C26 C25 37.6(3) . . . . ? C34 Zr2 C26 C25 -171.6(3) . . . . ? C28 Zr2 C26 C25 78.0(3) . . . . ? C32 Zr2 C26 C25 115.2(3) . . . . ? C33 Zr2 C26 C25 106.8(4) . . . . ? P3 Zr2 C26 C25 -80.0(3) . . . . ? C25 C26 C27 C28 1.9(5) . . . . ? Zr2 C26 C27 C28 67.6(3) . . . . ? C25 C26 C27 Zr2 -65.7(3) . . . . ? C18 Zr2 C27 C26 -49.2(3) . . . . ? C31 Zr2 C27 C26 -149.4(3) . . . . ? C30 Zr2 C27 C26 -128.2(3) . . . . ? C25 Zr2 C27 C26 36.9(3) . . . . ? C29 Zr2 C27 C26 77.4(3) . . . . ? C34 Zr2 C27 C26 -145.9(3) . . . . ? C28 Zr2 C27 C26 114.4(4) . . . . ? C32 Zr2 C27 C26 179.7(3) . . . . ? C33 Zr2 C27 C26 175.6(3) . . . . ? P3 Zr2 C27 C26 -18.8(3) . . . . ? C18 Zr2 C27 C28 -163.6(3) . . . . ? C31 Zr2 C27 C28 96.2(3) . . . . ? C30 Zr2 C27 C28 117.4(3) . . . . ? C25 Zr2 C27 C28 -77.4(3) . . . . ? C29 Zr2 C27 C28 -36.9(3) . . . . ? C34 Zr2 C27 C28 99.7(3) . . . . ? C26 Zr2 C27 C28 -114.4(4) . . . . ? C32 Zr2 C27 C28 65.3(3) . . . . ? C33 Zr2 C27 C28 61.2(3) . . . . ? P3 Zr2 C27 C28 -133.2(3) . . . . ? C26 C27 C28 C29 -1.9(5) . . . . ? Zr2 C27 C28 C29 65.4(3) . . . . ? C26 C27 C28 Zr2 -67.4(3) . . . . ? C18 Zr2 C28 C29 -93.9(3) . . . . ? C31 Zr2 C28 C29 164.9(3) . . . . ? C30 Zr2 C28 C29 169.9(3) . . . . ? C27 Zr2 C28 C29 -114.8(4) . . . . ? C25 Zr2 C28 C29 -37.0(3) . . . . ? C34 Zr2 C28 C29 133.4(3) . . . . ? C26 Zr2 C28 C29 -77.7(3) . . . . ? C32 Zr2 C28 C29 133.3(3) . . . . ? C33 Zr2 C28 C29 114.5(3) . . . . ? P3 Zr2 C28 C29 -41.7(4) . . . . ? C18 Zr2 C28 C27 20.8(4) . . . . ? C31 Zr2 C28 C27 -80.4(3) . . . . ? C30 Zr2 C28 C27 -75.3(3) . . . . ? C25 Zr2 C28 C27 77.8(3) . . . . ? C29 Zr2 C28 C27 114.8(4) . . . . ? C34 Zr2 C28 C27 -111.8(3) . . . . ? C26 Zr2 C28 C27 37.1(3) . . . . ? C32 Zr2 C28 C27 -111.9(3) . . . . ? C33 Zr2 C28 C27 -130.8(3) . . . . ? P3 Zr2 C28 C27 73.1(3) . . . . ? C26 C25 C29 C28 -0.1(5) . . . . ? Zr2 C25 C29 C28 -67.2(3) . . . . ? C26 C25 C29 Zr2 67.1(3) . . . . ? C27 C28 C29 C25 1.2(5) . . . . ? Zr2 C28 C29 C25 66.5(3) . . . . ? C27 C28 C29 Zr2 -65.3(3) . . . . ? C18 Zr2 C29 C25 -5.4(3) . . . . ? C31 Zr2 C29 C25 -132.3(3) . . . . ? C30 Zr2 C29 C25 -133.0(3) . . . . ? C27 Zr2 C29 C25 -77.9(3) . . . . ? C34 Zr2 C29 C25 163.8(3) . . . . ? C26 Zr2 C29 C25 -37.7(3) . . . . ? C28 Zr2 C29 C25 -115.2(4) . . . . ? C32 Zr2 C29 C25 -161.7(3) . . . . ? C33 Zr2 C29 C25 168.2(3) . . . . ? P3 Zr2 C29 C25 37.2(3) . . . . ? C18 Zr2 C29 C28 109.8(3) . . . . ? C31 Zr2 C29 C28 -17.1(3) . . . . ? C30 Zr2 C29 C28 -17.7(5) . . . . ? C27 Zr2 C29 C28 37.4(3) . . . . ? C25 Zr2 C29 C28 115.2(4) . . . . ? C34 Zr2 C29 C28 -81.0(4) . . . . ? C26 Zr2 C29 C28 77.6(3) . . . . ? C32 Zr2 C29 C28 -46.5(3) . . . . ? C33 Zr2 C29 C28 -76.5(3) . . . . ? P3 Zr2 C29 C28 152.5(3) . . . . ? C18 Zr2 C30 C31 -136.3(3) . . . . ? C27 Zr2 C30 C31 -42.3(3) . . . . ? C25 Zr2 C30 C31 -72.8(5) . . . . ? C29 Zr2 C30 C31 1.1(5) . . . . ? C34 Zr2 C30 C31 113.9(4) . . . . ? C26 Zr2 C30 C31 -72.3(3) . . . . ? C28 Zr2 C30 C31 -9.5(3) . . . . ? C32 Zr2 C30 C31 37.2(3) . . . . ? C33 Zr2 C30 C31 77.1(3) . . . . ? P3 Zr2 C30 C31 -169.9(3) . . . . ? C18 Zr2 C30 C34 109.8(3) . . . . ? C31 Zr2 C30 C34 -113.9(4) . . . . ? C27 Zr2 C30 C34 -156.2(3) . . . . ? C25 Zr2 C30 C34 173.3(3) . . . . ? C29 Zr2 C30 C34 -112.8(4) . . . . ? C26 Zr2 C30 C34 173.8(3) . . . . ? C28 Zr2 C30 C34 -123.4(3) . . . . ? C32 Zr2 C30 C34 -76.7(3) . . . . ? C33 Zr2 C30 C34 -36.8(3) . . . . ? P3 Zr2 C30 C34 76.2(3) . . . . ? C34 C30 C31 C32 -1.0(5) . . . . ? Zr2 C30 C31 C32 -68.3(3) . . . . ? C34 C30 C31 Zr2 67.4(3) . . . . ? C18 Zr2 C31 C30 43.4(3) . . . . ? C27 Zr2 C31 C30 139.2(3) . . . . ? C25 Zr2 C31 C30 146.5(3) . . . . ? C29 Zr2 C31 C30 -179.4(3) . . . . ? C34 Zr2 C31 C30 -37.7(3) . . . . ? C26 Zr2 C31 C30 122.5(3) . . . . ? C28 Zr2 C31 C30 171.6(3) . . . . ? C32 Zr2 C31 C30 -114.8(4) . . . . ? C33 Zr2 C31 C30 -77.9(3) . . . . ? P3 Zr2 C31 C30 12.8(3) . . . . ? C18 Zr2 C31 C32 158.2(3) . . . . ? C30 Zr2 C31 C32 114.8(4) . . . . ? C27 Zr2 C31 C32 -106.0(3) . . . . ? C25 Zr2 C31 C32 -98.7(3) . . . . ? C29 Zr2 C31 C32 -64.6(3) . . . . ? C34 Zr2 C31 C32 77.1(3) . . . . ? C26 Zr2 C31 C32 -122.7(3) . . . . ? C28 Zr2 C31 C32 -73.6(3) . . . . ? C33 Zr2 C31 C32 36.9(3) . . . . ? P3 Zr2 C31 C32 127.6(3) . . . . ? C30 C31 C32 C33 0.7(5) . . . . ? Zr2 C31 C32 C33 -66.8(3) . . . . ? C30 C31 C32 Zr2 67.5(3) . . . . ? C18 Zr2 C32 C33 85.9(3) . . . . ? C31 Zr2 C32 C33 114.4(4) . . . . ? C30 Zr2 C32 C33 77.4(3) . . . . ? C27 Zr2 C32 C33 -173.4(3) . . . . ? C25 Zr2 C32 C33 -133.1(3) . . . . ? C29 Zr2 C32 C33 -120.2(3) . . . . ? C34 Zr2 C32 C33 36.6(3) . . . . ? C26 Zr2 C32 C33 -173.2(3) . . . . ? C28 Zr2 C32 C33 -143.5(3) . . . . ? P3 Zr2 C32 C33 31.5(4) . . . . ? C18 Zr2 C32 C31 -28.6(4) . . . . ? C30 Zr2 C32 C31 -37.0(3) . . . . ? C27 Zr2 C32 C31 72.2(3) . . . . ? C25 Zr2 C32 C31 112.5(3) . . . . ? C29 Zr2 C32 C31 125.3(3) . . . . ? C34 Zr2 C32 C31 -77.8(3) . . . . ? C26 Zr2 C32 C31 72.3(3) . . . . ? C28 Zr2 C32 C31 102.1(3) . . . . ? C33 Zr2 C32 C31 -114.4(4) . . . . ? P3 Zr2 C32 C31 -83.0(3) . . . . ? C31 C32 C33 C34 -0.1(5) . . . . ? Zr2 C32 C33 C34 -65.3(3) . . . . ? C31 C32 C33 Zr2 65.2(3) . . . . ? C18 Zr2 C33 C32 -117.0(3) . . . . ? C31 Zr2 C33 C32 -37.6(3) . . . . ? C30 Zr2 C33 C32 -78.1(3) . . . . ? C27 Zr2 C33 C32 7.8(4) . . . . ? C25 Zr2 C33 C32 80.5(4) . . . . ? C29 Zr2 C33 C32 69.2(3) . . . . ? C34 Zr2 C33 C32 -115.5(4) . . . . ? C26 Zr2 C33 C32 13.4(5) . . . . ? C28 Zr2 C33 C32 36.9(3) . . . . ? P3 Zr2 C33 C32 -159.2(3) . . . . ? C18 Zr2 C33 C34 -1.5(4) . . . . ? C31 Zr2 C33 C34 78.0(3) . . . . ? C30 Zr2 C33 C34 37.5(3) . . . . ? C27 Zr2 C33 C34 123.4(3) . . . . ? C25 Zr2 C33 C34 -164.0(3) . . . . ? C29 Zr2 C33 C34 -175.3(3) . . . . ? C26 Zr2 C33 C34 128.9(4) . . . . ? C28 Zr2 C33 C34 152.4(3) . . . . ? C32 Zr2 C33 C34 115.5(4) . . . . ? P3 Zr2 C33 C34 -43.7(3) . . . . ? C32 C33 C34 C30 -0.5(5) . . . . ? Zr2 C33 C34 C30 -66.3(3) . . . . ? C32 C33 C34 Zr2 65.8(3) . . . . ? C31 C30 C34 C33 0.9(5) . . . . ? Zr2 C30 C34 C33 67.6(3) . . . . ? C31 C30 C34 Zr2 -66.8(3) . . . . ? C18 Zr2 C34 C33 178.7(3) . . . . ? C31 Zr2 C34 C33 -77.2(3) . . . . ? C30 Zr2 C34 C33 -114.6(4) . . . . ? C27 Zr2 C34 C33 -81.5(4) . . . . ? C25 Zr2 C34 C33 83.3(10) . . . . ? C29 Zr2 C34 C33 7.7(5) . . . . ? C26 Zr2 C34 C33 -127.3(4) . . . . ? C28 Zr2 C34 C33 -36.7(4) . . . . ? C32 Zr2 C34 C33 -36.5(3) . . . . ? P3 Zr2 C34 C33 140.2(3) . . . . ? C18 Zr2 C34 C30 -66.7(3) . . . . ? C31 Zr2 C34 C30 37.4(3) . . . . ? C27 Zr2 C34 C30 33.1(4) . . . . ? C25 Zr2 C34 C30 -162.0(9) . . . . ? C29 Zr2 C34 C30 122.4(3) . . . . ? C26 Zr2 C34 C30 -12.6(5) . . . . ? C28 Zr2 C34 C30 78.0(4) . . . . ? C32 Zr2 C34 C30 78.1(3) . . . . ? C33 Zr2 C34 C30 114.6(4) . . . . ? P3 Zr2 C34 C30 -105.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.447 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.087 data_4 _database_code_depnum_ccdc_archive 'CCDC 894366' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C46 H38 B F14.39 P2 Si2 Zr2), 3(C6 H6)' _chemical_formula_sum 'C110 H94 B2 F28.77 P4 Si4 Zr4' _chemical_formula_weight 2585.27 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' 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6768(5) _cell_length_b 14.4684(6) _cell_length_c 14.8618(6) _cell_angle_alpha 102.581(2) _cell_angle_beta 102.183(2) _cell_angle_gamma 100.369(2) _cell_volume 2725.79(19) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24130 _cell_measurement_theta_min 2.923 _cell_measurement_theta_max 28.2515 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1299 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836549 _exptl_absorpt_correction_T_max 0.947039 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45201 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 28.29 _reflns_number_total 13297 _reflns_number_gt 10531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+7.0206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13297 _refine_ls_number_parameters 701 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _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 Zr1 Zr 0.77868(2) 0.71461(2) 0.22934(2) 0.02211(8) Uani 1 1 d . . . Zr2 Zr 0.74965(2) 0.75654(2) 0.51392(2) 0.02336(8) Uani 1 1 d . . . P1 P 0.66219(7) 0.75174(7) 0.33340(6) 0.02886(19) Uani 1 1 d . . . P2 P 0.91351(6) 0.72949(6) 0.44307(5) 0.02122(16) Uani 1 1 d . . . Si1 Si 0.46867(8) 0.78977(8) 0.39985(7) 0.0312(2) Uani 1 1 d . . . Si2 Si 1.04867(7) 0.68303(7) 0.30063(7) 0.02591(19) Uani 1 1 d . . . B1 B 1.3269(3) 0.7496(3) 0.7496(3) 0.0256(7) Uani 1 1 d . . . C1 C 0.8450(3) 0.8975(3) 0.2748(3) 0.0386(9) Uani 1 1 d . . . H1A H 0.8620 0.9324 0.3402 0.046 Uiso 1 1 calc R . . C2 C 0.9121(3) 0.8567(3) 0.2268(3) 0.0387(9) Uani 1 1 d . . . H1 H 0.9826 0.8604 0.2537 0.046 Uiso 1 1 calc R . . C3 C 0.8561(3) 0.8097(3) 0.1321(3) 0.0372(9) Uani 1 1 d . . . H3 H 0.8819 0.7752 0.0838 0.045 Uiso 1 1 calc R . . C4 C 0.7549(3) 0.8224(3) 0.1211(3) 0.0344(8) Uani 1 1 d . . . H4 H 0.7006 0.7981 0.0642 0.041 Uiso 1 1 calc R . . C5 C 0.7485(3) 0.8774(3) 0.2090(3) 0.0354(8) Uani 1 1 d . . . H5 H 0.6893 0.8975 0.2218 0.042 Uiso 1 1 calc R . . C6 C 0.7645(3) 0.5736(3) 0.0946(2) 0.0325(8) Uani 1 1 d . . . H6 H 0.8088 0.5821 0.0542 0.039 Uiso 1 1 calc R . . C7 C 0.6652(3) 0.5922(3) 0.0825(2) 0.0327(8) Uani 1 1 d . . . H7 H 0.6312 0.6158 0.0328 0.039 Uiso 1 1 calc R . . C8 C 0.6259(3) 0.5696(3) 0.1571(2) 0.0323(8) Uani 1 1 d . . . H8 H 0.5600 0.5742 0.1660 0.039 Uiso 1 1 calc R . . C9 C 0.7015(3) 0.5386(3) 0.2168(2) 0.0319(8) Uani 1 1 d . . . H9 H 0.6959 0.5202 0.2734 0.038 Uiso 1 1 calc R . . C10 C 0.7859(3) 0.5400(3) 0.1774(3) 0.0319(8) Uani 1 1 d . . . H10 H 0.8472 0.5216 0.2021 0.038 Uiso 1 1 calc R . . C11 C 0.7760(3) 0.9412(3) 0.5497(3) 0.0349(8) Uani 1 1 d . . . H11 H 0.7440 0.9690 0.5025 0.042 Uiso 1 1 calc R . . C12 C 0.8745(3) 0.9237(3) 0.5623(3) 0.0335(8) Uani 1 1 d . . . H12 H 0.9210 0.9374 0.5249 0.040 Uiso 1 1 calc R . . C13 C 0.8936(3) 0.8820(3) 0.6403(3) 0.0354(8) Uani 1 1 d . . . H13 H 0.9541 0.8618 0.6639 0.043 Uiso 1 1 calc R . . C14 C 0.8067(3) 0.8760(3) 0.6762(3) 0.0386(9) Uani 1 1 d . . . H14 H 0.7987 0.8527 0.7299 0.046 Uiso 1 1 calc R . . C15 C 0.7326(3) 0.9106(3) 0.6189(3) 0.0372(8) Uani 1 1 d . . . H15 H 0.6656 0.9128 0.6261 0.045 Uiso 1 1 calc R . . C16 C 0.6960(3) 0.6616(3) 0.6240(3) 0.0405(9) Uani 1 1 d . . . H16 H 0.6952 0.6972 0.6855 0.049 Uiso 1 1 calc R . . C17 C 0.6132(3) 0.6322(3) 0.5416(3) 0.0393(9) Uani 1 1 d . . . H17 H 0.5471 0.6453 0.5376 0.047 Uiso 1 1 calc R . . C18 C 0.6452(3) 0.5797(3) 0.4659(3) 0.0333(8) Uani 1 1 d . . . H18 H 0.6043 0.5511 0.4022 0.040 Uiso 1 1 calc R . . C19 C 0.7482(3) 0.5772(3) 0.5013(3) 0.0314(7) Uani 1 1 d . . . H19 H 0.7889 0.5461 0.4658 0.038 Uiso 1 1 calc R . . C20 C 0.7804(3) 0.6291(3) 0.5990(3) 0.0359(8) Uani 1 1 d . . . H20 H 0.8470 0.6401 0.6405 0.043 Uiso 1 1 calc R . . C21 C 0.6022(3) 0.7730(3) 0.4178(2) 0.0267(7) Uani 1 1 d . . . C22 C 0.4448(3) 0.8571(4) 0.3068(3) 0.0463(10) Uani 1 1 d . . . H22A H 0.3772 0.8724 0.3015 0.069 Uiso 1 1 calc R . . H22B H 0.4465 0.8166 0.2453 0.069 Uiso 1 1 calc R . . H22C H 0.4983 0.9178 0.3248 0.069 Uiso 1 1 calc R . . C23 C 0.3825(3) 0.6658(4) 0.3578(4) 0.0567(13) Uani 1 1 d . . . H23A H 0.3940 0.6318 0.4080 0.085 Uiso 1 1 calc R . . H23B H 0.3972 0.6292 0.3004 0.085 Uiso 1 1 calc R . . H23C H 0.3106 0.6707 0.3426 0.085 Uiso 1 1 calc R . . C24 C 0.4487(4) 0.8589(4) 0.5125(3) 0.0481(11) Uani 1 1 d . . . H24A H 0.4599 0.8228 0.5609 0.072 Uiso 1 1 calc R . . H24B H 0.3782 0.8678 0.5010 0.072 Uiso 1 1 calc R . . H24C H 0.4975 0.9228 0.5352 0.072 Uiso 1 1 calc R . . C25 C 0.9280(2) 0.7068(2) 0.3335(2) 0.0217(6) Uani 1 1 d . . . C26 C 1.1565(3) 0.7955(3) 0.3456(3) 0.0427(10) Uani 1 1 d . . . H26A H 1.1287 0.8528 0.3418 0.064 Uiso 1 1 calc R . . H26B H 1.2056 0.7906 0.3064 0.064 Uiso 1 1 calc R . . H26C H 1.1916 0.8018 0.4121 0.064 Uiso 1 1 calc R . . C27 C 1.0875(3) 0.5812(3) 0.3458(3) 0.0376(9) Uani 1 1 d . . . H27A H 1.1415 0.5613 0.3175 0.056 Uiso 1 1 calc R . . H27B H 1.0277 0.5258 0.3281 0.056 Uiso 1 1 calc R . . H27C H 1.1137 0.6028 0.4154 0.056 Uiso 1 1 calc R . . C28 C 1.0289(3) 0.6455(4) 0.1708(3) 0.0467(10) Uani 1 1 d . . . H28A H 1.0951 0.6428 0.1561 0.070 Uiso 1 1 calc R . . H28B H 0.9996 0.6928 0.1423 0.070 Uiso 1 1 calc R . . H28C H 0.9816 0.5810 0.1447 0.070 Uiso 1 1 calc R . . C29 C 1.0341(2) 0.7395(2) 0.5324(2) 0.0228(6) Uani 1 1 d . . . C30 C 1.1134(3) 0.8232(2) 0.5673(2) 0.0230(6) Uani 1 1 d . . . C31 C 1.2030(2) 0.8291(2) 0.6341(2) 0.0227(6) Uani 1 1 d . . . C32 C 1.2213(2) 0.7539(2) 0.6749(2) 0.0227(6) Uani 1 1 d . . . C33 C 1.1401(3) 0.6714(2) 0.6396(2) 0.0246(6) Uani 1 1 d . . . C34 C 1.0504(2) 0.6642(2) 0.5726(2) 0.0238(6) Uani 1 1 d . . . C35 C 1.3037(3) 0.7189(2) 0.8458(2) 0.0254(7) Uani 1 1 d . . . C36 C 1.3815(3) 0.6937(3) 0.9064(2) 0.0279(7) Uani 1 1 d . . . C37 C 1.3720(3) 0.6700(3) 0.9902(3) 0.0328(8) Uani 1 1 d . . . C38 C 1.2834(3) 0.6709(3) 1.0175(3) 0.0345(8) Uani 1 1 d . . . C39 C 1.2045(3) 0.6958(3) 0.9611(3) 0.0330(8) Uani 1 1 d . . . C40 C 1.2164(3) 0.7198(3) 0.8785(2) 0.0277(7) Uani 1 1 d . . . C41 C 1.4130(2) 0.8539(2) 0.7927(2) 0.0223(6) Uani 1 1 d . . . C42 C 1.5137(3) 0.8693(3) 0.7849(2) 0.0274(7) Uani 1 1 d . . . C43 C 1.5877(3) 0.9538(3) 0.8304(2) 0.0324(8) Uani 1 1 d . . . C44 C 1.5635(3) 1.0306(3) 0.8867(2) 0.0318(8) Uani 1 1 d . . . C45 C 1.4652(3) 1.0212(2) 0.8964(2) 0.0280(7) Uani 1 1 d . . . C46 C 1.3933(3) 0.9347(2) 0.8507(2) 0.0241(6) Uani 1 1 d . . . C47 C 0.6918(4) 0.6112(4) 0.8505(3) 0.0600(15) Uani 1 1 d . . . H47 H 0.6245 0.5724 0.8397 0.072 Uiso 1 1 calc R . . C48 C 0.7740(5) 0.5671(4) 0.8437(3) 0.0558(13) Uani 1 1 d . . . H48 H 0.7627 0.4982 0.8284 0.067 Uiso 1 1 calc R . . C49 C 0.8702(4) 0.6237(4) 0.8591(3) 0.0474(10) Uani 1 1 d . . . H49 H 0.9263 0.5940 0.8550 0.057 Uiso 1 1 calc R . . C50 C 0.8864(3) 0.7231(3) 0.8806(3) 0.0440(10) Uani 1 1 d . . . H50 H 0.9534 0.7621 0.8903 0.053 Uiso 1 1 calc R . . C51 C 0.8066(4) 0.7664(3) 0.8881(3) 0.0435(10) Uani 1 1 d . . . H51 H 0.8188 0.8354 0.9039 0.052 Uiso 1 1 calc R . . C52 C 0.7092(4) 0.7114(4) 0.8731(3) 0.0513(12) Uani 1 1 d . . . H52 H 0.6540 0.7420 0.8782 0.062 Uiso 1 1 calc R . . H53 H 1.0589 -0.0294 0.8641 0.062 Uiso 1 1 d R . . C53 C 1.0350(6) -0.0165(4) 0.9192(3) 0.0707(19) Uani 1 1 d . . . C54 C 0.9154(5) 0.0411(4) 1.0009(4) 0.0680(16) Uani 1 1 d . . . H54 H 0.8574 0.0686 1.0015 0.082 Uiso 1 1 calc R . . C55 C 0.9522(5) 0.0245(4) 0.9198(4) 0.0711(19) Uani 1 1 d . . . H55 H 0.9199 0.0417 0.8647 0.085 Uiso 1 1 calc R . . F1 F 1.10337(15) 0.90219(14) 0.53376(14) 0.0278(4) Uani 1 1 d . . . F2 F 1.27519(15) 0.91446(14) 0.65848(14) 0.0270(4) Uani 1 1 d . . . F3 F 1.14707(16) 0.59153(14) 0.67227(15) 0.0314(4) Uani 1 1 d . . . F4 F 0.97656(15) 0.58056(14) 0.54446(15) 0.0318(5) Uani 1 1 d . . . F5 F 1.47259(16) 0.69244(17) 0.88560(16) 0.0370(5) Uani 1 1 d . . . F6 F 1.45106(19) 0.64806(19) 1.04594(17) 0.0471(6) Uani 1 1 d . . . F7 F 1.2733(2) 0.6495(2) 1.09948(17) 0.0491(6) Uani 1 1 d . . . F8 F 1.11667(19) 0.6988(2) 0.98795(18) 0.0489(6) Uani 1 1 d . . . F9 F 1.13504(16) 0.74609(18) 0.82986(15) 0.0364(5) Uani 1 1 d . . . F10 F 1.54602(18) 0.79893(18) 0.73072(15) 0.0404(5) Uani 1 1 d . . . F11 F 1.68472(18) 0.9632(2) 0.82100(18) 0.0505(7) Uani 1 1 d . . . F12 F 1.6355(2) 1.11366(18) 0.93096(18) 0.0489(6) Uani 1 1 d . . . F13 F 1.44062(19) 1.09588(16) 0.95115(15) 0.0396(5) Uani 1 1 d . . . F14 F 1.29812(16) 0.92900(15) 0.86404(15) 0.0314(4) Uani 1 1 d . . . F15 F 1.3691(5) 0.6664(4) 0.6820(4) 0.038(2) Uani 0.386(9) 1 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 Zr1 0.02750(16) 0.02454(16) 0.01651(14) 0.00679(11) 0.00512(11) 0.01081(12) Zr2 0.02594(16) 0.02838(17) 0.01741(14) 0.00661(12) 0.00703(11) 0.00832(13) P1 0.0305(5) 0.0388(5) 0.0205(4) 0.0089(4) 0.0077(3) 0.0138(4) P2 0.0238(4) 0.0235(4) 0.0175(3) 0.0070(3) 0.0038(3) 0.0084(3) Si1 0.0264(5) 0.0371(6) 0.0312(5) 0.0075(4) 0.0088(4) 0.0108(4) Si2 0.0262(5) 0.0271(5) 0.0286(4) 0.0092(4) 0.0112(4) 0.0096(4) B1 0.0240(18) 0.0245(18) 0.0264(17) 0.0079(14) 0.0008(14) 0.0066(14) C1 0.061(3) 0.0253(18) 0.0272(17) 0.0102(14) 0.0048(17) 0.0089(17) C2 0.040(2) 0.036(2) 0.046(2) 0.0270(18) 0.0083(17) 0.0083(17) C3 0.056(2) 0.037(2) 0.0347(19) 0.0223(16) 0.0236(17) 0.0223(18) C4 0.050(2) 0.0327(19) 0.0261(16) 0.0151(15) 0.0086(15) 0.0175(17) C5 0.054(2) 0.0294(19) 0.0338(18) 0.0163(15) 0.0148(17) 0.0233(17) C6 0.039(2) 0.0322(19) 0.0219(15) 0.0006(14) 0.0064(14) 0.0067(16) C7 0.038(2) 0.037(2) 0.0209(15) 0.0067(14) 0.0018(13) 0.0106(16) C8 0.0345(19) 0.0318(19) 0.0260(16) 0.0034(14) 0.0035(14) 0.0069(15) C9 0.041(2) 0.0253(17) 0.0255(16) 0.0044(13) 0.0043(14) 0.0057(15) C10 0.039(2) 0.0218(17) 0.0286(17) -0.0012(13) 0.0023(14) 0.0100(15) C11 0.046(2) 0.0256(18) 0.0292(17) 0.0026(14) 0.0047(15) 0.0113(16) C12 0.038(2) 0.0287(18) 0.0286(17) -0.0011(14) 0.0113(15) 0.0028(15) C13 0.037(2) 0.033(2) 0.0266(16) -0.0039(14) -0.0009(14) 0.0109(16) C14 0.054(2) 0.038(2) 0.0210(16) 0.0019(15) 0.0100(16) 0.0101(18) C15 0.037(2) 0.038(2) 0.0342(19) -0.0018(16) 0.0139(16) 0.0106(17) C16 0.057(3) 0.044(2) 0.0297(18) 0.0178(17) 0.0221(17) 0.0122(19) C17 0.037(2) 0.044(2) 0.046(2) 0.0222(19) 0.0213(17) 0.0102(17) C18 0.036(2) 0.0291(18) 0.0338(18) 0.0120(15) 0.0088(15) 0.0022(15) C19 0.038(2) 0.0271(18) 0.0319(17) 0.0124(14) 0.0118(15) 0.0077(15) C20 0.044(2) 0.037(2) 0.0288(17) 0.0173(16) 0.0055(15) 0.0082(17) C21 0.0290(17) 0.0281(17) 0.0234(15) 0.0051(13) 0.0089(13) 0.0079(14) C22 0.038(2) 0.064(3) 0.046(2) 0.025(2) 0.0107(18) 0.021(2) C23 0.034(2) 0.046(3) 0.080(4) 0.010(2) 0.005(2) 0.003(2) C24 0.045(2) 0.067(3) 0.039(2) 0.009(2) 0.0185(18) 0.026(2) C25 0.0257(15) 0.0231(15) 0.0192(13) 0.0082(12) 0.0065(11) 0.0092(12) C26 0.032(2) 0.036(2) 0.062(3) 0.0114(19) 0.0196(19) 0.0073(17) C27 0.038(2) 0.038(2) 0.049(2) 0.0179(18) 0.0217(17) 0.0205(17) C28 0.040(2) 0.070(3) 0.037(2) 0.021(2) 0.0105(17) 0.019(2) C29 0.0242(15) 0.0246(16) 0.0191(13) 0.0060(12) 0.0020(11) 0.0084(12) C30 0.0283(16) 0.0209(15) 0.0230(14) 0.0093(12) 0.0064(12) 0.0097(13) C31 0.0230(15) 0.0211(15) 0.0203(14) 0.0028(12) 0.0026(11) 0.0030(12) C32 0.0247(15) 0.0237(16) 0.0208(14) 0.0067(12) 0.0044(12) 0.0091(13) C33 0.0263(16) 0.0224(16) 0.0255(15) 0.0098(12) 0.0028(12) 0.0073(13) C34 0.0246(16) 0.0217(16) 0.0235(14) 0.0060(12) 0.0024(12) 0.0059(12) C35 0.0287(17) 0.0216(16) 0.0230(14) 0.0066(12) -0.0008(12) 0.0063(13) C36 0.0277(17) 0.0256(17) 0.0282(16) 0.0079(13) 0.0005(13) 0.0076(13) C37 0.0367(19) 0.0282(18) 0.0298(17) 0.0119(14) -0.0052(14) 0.0096(15) C38 0.044(2) 0.0286(18) 0.0262(16) 0.0117(14) 0.0018(15) -0.0002(16) C39 0.0307(18) 0.035(2) 0.0315(17) 0.0116(15) 0.0055(14) 0.0024(15) C40 0.0274(17) 0.0287(17) 0.0247(15) 0.0107(13) -0.0007(12) 0.0053(14) C41 0.0248(15) 0.0242(16) 0.0180(13) 0.0071(12) 0.0028(11) 0.0074(12) C42 0.0312(17) 0.0321(18) 0.0190(14) 0.0045(13) 0.0060(12) 0.0117(14) C43 0.0255(17) 0.045(2) 0.0266(16) 0.0117(15) 0.0079(13) 0.0034(15) C44 0.0366(19) 0.0284(18) 0.0228(15) 0.0075(13) -0.0007(13) -0.0019(15) C45 0.0410(19) 0.0233(16) 0.0180(14) 0.0046(12) 0.0021(13) 0.0110(14) C46 0.0279(16) 0.0263(16) 0.0190(14) 0.0067(12) 0.0034(12) 0.0108(13) C47 0.050(3) 0.086(4) 0.0269(19) 0.015(2) 0.0053(18) -0.022(3) C48 0.089(4) 0.039(2) 0.030(2) 0.0082(18) 0.010(2) -0.002(2) C49 0.052(3) 0.050(3) 0.037(2) 0.0054(19) 0.0068(18) 0.018(2) C50 0.040(2) 0.055(3) 0.0300(18) 0.0058(18) 0.0069(16) 0.0023(19) C51 0.057(3) 0.043(2) 0.0301(19) 0.0100(17) 0.0088(18) 0.014(2) C52 0.045(2) 0.084(4) 0.0287(19) 0.018(2) 0.0088(17) 0.023(2) C53 0.098(5) 0.055(3) 0.035(2) 0.009(2) 0.011(3) -0.032(3) C54 0.079(4) 0.052(3) 0.050(3) 0.010(2) 0.007(3) -0.026(3) C55 0.090(4) 0.058(3) 0.038(2) 0.017(2) -0.005(3) -0.030(3) F1 0.0301(10) 0.0227(10) 0.0300(10) 0.0121(8) 0.0005(8) 0.0071(8) F2 0.0271(10) 0.0216(9) 0.0282(9) 0.0073(8) -0.0001(8) 0.0031(8) F3 0.0327(11) 0.0226(10) 0.0349(11) 0.0134(8) -0.0043(8) 0.0052(8) F4 0.0297(10) 0.0232(10) 0.0362(11) 0.0117(8) -0.0047(8) 0.0012(8) F5 0.0309(11) 0.0457(13) 0.0381(11) 0.0158(10) 0.0038(9) 0.0190(10) F6 0.0470(14) 0.0554(15) 0.0403(13) 0.0249(11) -0.0053(10) 0.0206(12) F7 0.0588(16) 0.0571(16) 0.0330(12) 0.0271(11) 0.0057(11) 0.0068(13) F8 0.0392(13) 0.0718(18) 0.0423(13) 0.0280(13) 0.0153(10) 0.0089(12) F9 0.0274(11) 0.0556(14) 0.0323(11) 0.0195(10) 0.0060(8) 0.0177(10) F10 0.0386(12) 0.0523(14) 0.0308(11) 0.0001(10) 0.0113(9) 0.0230(11) F11 0.0273(12) 0.0723(18) 0.0465(14) 0.0113(13) 0.0133(10) -0.0007(12) F12 0.0502(15) 0.0348(13) 0.0430(13) 0.0064(10) -0.0056(11) -0.0107(11) F13 0.0589(15) 0.0269(11) 0.0278(10) -0.0015(9) 0.0008(10) 0.0198(10) F14 0.0311(11) 0.0347(11) 0.0337(10) 0.0099(9) 0.0112(8) 0.0166(9) F15 0.039(4) 0.031(3) 0.043(4) 0.012(3) 0.006(3) 0.011(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 Zr1 C25 2.325(3) . ? Zr1 C3 2.467(4) . ? Zr1 C6 2.475(3) . ? Zr1 C4 2.486(3) . ? Zr1 C7 2.491(4) . ? Zr1 P1 2.4909(9) . ? Zr1 C10 2.502(3) . ? Zr1 C2 2.504(4) . ? Zr1 C1 2.525(4) . ? Zr1 C9 2.525(4) . ? Zr1 C5 2.532(3) . ? Zr1 C8 2.533(4) . ? Zr2 C21 2.295(3) . ? Zr2 C16 2.494(4) . ? Zr2 C20 2.500(4) . ? Zr2 C15 2.507(4) . ? Zr2 C14 2.513(4) . ? Zr2 C17 2.515(4) . ? Zr2 C13 2.523(4) . ? Zr2 C11 2.550(4) . ? Zr2 C12 2.553(4) . ? Zr2 C19 2.557(4) . ? Zr2 C18 2.560(4) . ? Zr2 P1 2.6773(9) . ? P1 C21 1.642(3) . ? P2 C25 1.650(3) . ? P2 C29 1.847(3) . ? Si1 C23 1.855(5) . ? Si1 C24 1.855(4) . ? Si1 C21 1.857(4) . ? Si1 C22 1.866(4) . ? Si2 C28 1.833(4) . ? Si2 C27 1.861(4) . ? Si2 C26 1.875(4) . ? Si2 C25 1.885(3) . ? B1 C41 1.642(5) . ? B1 C32 1.645(5) . ? B1 C35 1.661(5) . ? B1 F15 1.662(7) . ? C1 C5 1.406(6) . ? C1 C2 1.410(6) . ? C1 H1A 0.9500 . ? C2 C3 1.404(6) . ? C2 H1 0.9500 . ? C3 C4 1.408(6) . ? C3 H3 0.9500 . ? C4 C5 1.402(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.412(5) . ? C6 C7 1.413(5) . ? C6 H6 0.9500 . ? C7 C8 1.404(5) . ? C7 H7 0.9500 . ? C8 C9 1.418(5) . ? C8 H8 0.9500 . ? C9 C10 1.400(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.398(6) . ? C11 C15 1.402(6) . ? C11 H11 0.9500 . ? C12 C13 1.417(5) . ? C12 H12 0.9500 . ? C13 C14 1.398(6) . ? C13 H13 0.9500 . ? C14 C15 1.417(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.405(6) . ? C16 C20 1.412(6) . ? C16 H16 0.9500 . ? C17 C18 1.410(6) . ? C17 H17 0.9500 . ? C18 C19 1.405(5) . ? C18 H18 0.9500 . ? C19 C20 1.416(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.382(4) . ? C29 C30 1.388(5) . ? C30 F1 1.359(4) . ? C30 C31 1.380(4) . ? C31 F2 1.359(4) . ? C31 C32 1.391(4) . ? C32 C33 1.392(5) . ? C33 F3 1.358(4) . ? C33 C34 1.379(4) . ? C34 F4 1.349(4) . ? C35 C40 1.381(5) . ? C35 C36 1.397(4) . ? C36 F5 1.349(4) . ? C36 C37 1.387(5) . ? C37 F6 1.347(4) . ? C37 C38 1.359(6) . ? C38 F7 1.349(4) . ? C38 C39 1.374(5) . ? C39 F8 1.347(4) . ? C39 C40 1.381(5) . ? C40 F9 1.356(4) . ? C41 C42 1.389(5) . ? C41 C46 1.398(5) . ? C42 F10 1.355(4) . ? C42 C43 1.372(5) . ? C43 F11 1.348(4) . ? C43 C44 1.375(6) . ? C44 F12 1.342(4) . ? C44 C45 1.369(5) . ? C45 F13 1.344(4) . ? C45 C46 1.378(5) . ? C46 F14 1.348(4) . ? C47 C52 1.378(8) . ? C47 C48 1.399(8) . ? C47 H47 0.9500 . ? C48 C49 1.363(7) . ? C48 H48 0.9500 . ? C49 C50 1.369(7) . ? C49 H49 0.9500 . ? C50 C51 1.364(6) . ? C50 H50 0.9500 . ? C51 C52 1.369(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C55 1.371(10) . ? C53 C54 1.388(8) 2_757 ? C53 H53 0.9381 . ? C54 C53 1.388(8) 2_757 ? C54 C55 1.392(8) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? 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 C25 Zr1 C3 99.41(13) . . ? C25 Zr1 C6 99.57(12) . . ? C3 Zr1 C6 83.76(13) . . ? C25 Zr1 C4 129.49(13) . . ? C3 Zr1 C4 33.03(13) . . ? C6 Zr1 C4 91.87(12) . . ? C25 Zr1 C7 130.21(12) . . ? C3 Zr1 C7 90.87(14) . . ? C6 Zr1 C7 33.07(12) . . ? C4 Zr1 C7 80.45(13) . . ? C25 Zr1 P1 104.37(8) . . ? C3 Zr1 P1 130.80(9) . . ? C6 Zr1 P1 132.17(10) . . ? C4 Zr1 P1 103.32(9) . . ? C7 Zr1 P1 104.82(9) . . ? C25 Zr1 C10 76.53(11) . . ? C3 Zr1 C10 110.46(13) . . ? C6 Zr1 C10 32.97(12) . . ? C4 Zr1 C10 124.77(12) . . ? C7 Zr1 C10 54.43(12) . . ? P1 Zr1 C10 116.64(10) . . ? C25 Zr1 C2 75.65(12) . . ? C3 Zr1 C2 32.79(14) . . ? C6 Zr1 C2 109.63(14) . . ? C4 Zr1 C2 54.29(13) . . ? C7 Zr1 C2 123.51(13) . . ? P1 Zr1 C2 116.11(11) . . ? C10 Zr1 C2 124.70(14) . . ? C25 Zr1 C1 88.20(12) . . ? C3 Zr1 C1 54.14(13) . . ? C6 Zr1 C1 137.90(13) . . ? C4 Zr1 C1 53.93(12) . . ? C7 Zr1 C1 134.17(12) . . ? P1 Zr1 C1 84.04(10) . . ? C10 Zr1 C1 156.61(14) . . ? C2 Zr1 C1 32.55(14) . . ? C25 Zr1 C9 89.65(12) . . ? C3 Zr1 C9 138.00(13) . . ? C6 Zr1 C9 54.25(12) . . ? C4 Zr1 C9 134.27(12) . . ? C7 Zr1 C9 54.21(12) . . ? P1 Zr1 C9 84.91(9) . . ? C10 Zr1 C9 32.33(13) . . ? C2 Zr1 C9 156.56(14) . . ? C1 Zr1 C9 167.84(13) . . ? C25 Zr1 C5 120.47(13) . . ? C3 Zr1 C5 54.07(13) . . ? C6 Zr1 C5 123.75(12) . . ? C4 Zr1 C5 32.43(12) . . ? C7 Zr1 C5 104.98(13) . . ? P1 Zr1 C5 76.77(9) . . ? C10 Zr1 C5 156.62(12) . . ? C2 Zr1 C5 53.78(14) . . ? C1 Zr1 C5 32.27(13) . . ? C9 Zr1 C5 147.65(13) . . ? C25 Zr1 C8 122.21(12) . . ? C3 Zr1 C8 122.58(13) . . ? C6 Zr1 C8 54.08(13) . . ? C4 Zr1 C8 104.31(13) . . ? C7 Zr1 C8 32.44(12) . . ? P1 Zr1 C8 78.15(9) . . ? C10 Zr1 C8 53.75(12) . . ? C2 Zr1 C8 155.32(12) . . ? C1 Zr1 C8 147.65(13) . . ? C9 Zr1 C8 32.56(12) . . ? C5 Zr1 C8 116.26(13) . . ? C21 Zr2 C16 107.16(14) . . ? C21 Zr2 C20 130.92(13) . . ? C16 Zr2 C20 32.85(14) . . ? C21 Zr2 C15 82.04(13) . . ? C16 Zr2 C15 90.98(14) . . ? C20 Zr2 C15 113.97(14) . . ? C21 Zr2 C14 113.92(13) . . ? C16 Zr2 C14 74.93(14) . . ? C20 Zr2 C14 86.44(13) . . ? C15 Zr2 C14 32.78(13) . . ? C21 Zr2 C17 77.98(13) . . ? C16 Zr2 C17 32.58(14) . . ? C20 Zr2 C17 54.03(14) . . ? C15 Zr2 C17 101.12(14) . . ? C14 Zr2 C17 99.73(14) . . ? C21 Zr2 C13 130.83(13) . . ? C16 Zr2 C13 95.57(14) . . ? C20 Zr2 C13 90.58(13) . . ? C15 Zr2 C13 53.97(13) . . ? C14 Zr2 C13 32.23(13) . . ? C17 Zr2 C13 126.52(14) . . ? C21 Zr2 C11 77.74(12) . . ? C16 Zr2 C11 122.91(13) . . ? C20 Zr2 C11 139.55(12) . . ? C15 Zr2 C11 32.19(13) . . ? C14 Zr2 C11 53.43(13) . . ? C17 Zr2 C11 129.74(14) . . ? C13 Zr2 C11 53.52(12) . . ? C21 Zr2 C12 105.38(13) . . ? C16 Zr2 C12 126.41(13) . . ? C20 Zr2 C12 121.59(13) . . ? C15 Zr2 C12 53.21(13) . . ? C14 Zr2 C12 53.17(13) . . ? C17 Zr2 C12 152.13(13) . . ? C13 Zr2 C12 32.42(13) . . ? C11 Zr2 C12 31.79(13) . . ? C21 Zr2 C19 111.32(12) . . ? C16 Zr2 C19 53.77(13) . . ? C20 Zr2 C19 32.49(12) . . ? C15 Zr2 C19 144.28(13) . . ? C14 Zr2 C19 118.93(13) . . ? C17 Zr2 C19 53.34(13) . . ? C13 Zr2 C19 117.26(12) . . ? C11 Zr2 C19 170.75(12) . . ? C12 Zr2 C19 140.84(13) . . ? C21 Zr2 C18 80.90(12) . . ? C16 Zr2 C18 53.67(13) . . ? C20 Zr2 C18 53.62(13) . . ? C15 Zr2 C18 132.89(13) . . ? C14 Zr2 C18 128.41(13) . . ? C17 Zr2 C18 32.25(13) . . ? C13 Zr2 C18 144.09(13) . . ? C11 Zr2 C18 155.70(13) . . ? C12 Zr2 C18 172.50(13) . . ? C19 Zr2 C18 31.88(12) . . ? C21 Zr2 P1 37.57(8) . . ? C16 Zr2 P1 132.36(11) . . ? C20 Zr2 P1 134.15(9) . . ? C15 Zr2 P1 107.31(10) . . ? C14 Zr2 P1 138.57(10) . . ? C17 Zr2 P1 99.88(10) . . ? C13 Zr2 P1 130.96(10) . . ? C11 Zr2 P1 86.27(9) . . ? C12 Zr2 P1 98.64(9) . . ? C19 Zr2 P1 102.04(8) . . ? C18 Zr2 P1 83.81(9) . . ? C21 P1 Zr1 169.18(13) . . ? C21 P1 Zr2 58.50(12) . . ? Zr1 P1 Zr2 110.72(3) . . ? C25 P2 C29 111.83(15) . . ? C25 P2 Zr2 132.43(12) . . ? C29 P2 Zr2 115.73(11) . . ? C23 Si1 C24 110.9(3) . . ? C23 Si1 C21 106.34(19) . . ? C24 Si1 C21 111.03(18) . . ? C23 Si1 C22 110.2(2) . . ? C24 Si1 C22 109.6(2) . . ? C21 Si1 C22 108.73(18) . . ? C28 Si2 C27 106.1(2) . . ? C28 Si2 C26 106.0(2) . . ? C27 Si2 C26 110.8(2) . . ? C28 Si2 C25 111.58(17) . . ? C27 Si2 C25 110.70(16) . . ? C26 Si2 C25 111.55(17) . . ? C41 B1 C32 114.3(3) . . ? C41 B1 C35 104.1(3) . . ? C32 B1 C35 112.2(3) . . ? C41 B1 F15 111.8(3) . . ? C32 B1 F15 101.9(3) . . ? C35 B1 F15 112.8(3) . . ? C5 C1 C2 108.0(3) . . ? C5 C1 Zr1 74.1(2) . . ? C2 C1 Zr1 72.9(2) . . ? C5 C1 H1A 126.0 . . ? C2 C1 H1A 126.0 . . ? Zr1 C1 H1A 118.9 . . ? C3 C2 C1 107.8(4) . . ? C3 C2 Zr1 72.2(2) . . ? C1 C2 Zr1 74.5(2) . . ? C3 C2 H1 126.1 . . ? C1 C2 H1 126.1 . . ? Zr1 C2 H1 119.1 . . ? C2 C3 C4 108.1(3) . . ? C2 C3 Zr1 75.1(2) . . ? C4 C3 Zr1 74.2(2) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? Zr1 C3 H3 116.8 . . ? C5 C4 C3 108.0(4) . . ? C5 C4 Zr1 75.6(2) . . ? C3 C4 Zr1 72.8(2) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Zr1 C4 H4 117.6 . . ? C4 C5 C1 108.1(4) . . ? C4 C5 Zr1 72.0(2) . . ? C1 C5 Zr1 73.6(2) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Zr1 C5 H5 120.3 . . ? C10 C6 C7 107.8(3) . . ? C10 C6 Zr1 74.6(2) . . ? C7 C6 Zr1 74.1(2) . . ? C10 C6 H6 126.1 . . ? C7 C6 H6 126.1 . . ? Zr1 C6 H6 117.3 . . ? C8 C7 C6 107.9(3) . . ? C8 C7 Zr1 75.4(2) . . ? C6 C7 Zr1 72.8(2) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Zr1 C7 H7 117.7 . . ? C7 C8 C9 108.2(3) . . ? C7 C8 Zr1 72.1(2) . . ? C9 C8 Zr1 73.4(2) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Zr1 C8 H8 120.3 . . ? C10 C9 C8 107.8(3) . . ? C10 C9 Zr1 72.9(2) . . ? C8 C9 Zr1 74.0(2) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Zr1 C9 H9 118.9 . . ? C9 C10 C6 108.4(3) . . ? C9 C10 Zr1 74.8(2) . . ? C6 C10 Zr1 72.5(2) . . ? C9 C10 H10 125.8 . . ? C6 C10 H10 125.8 . . ? Zr1 C10 H10 118.8 . . ? C12 C11 C15 108.1(3) . . ? C12 C11 Zr2 74.2(2) . . ? C15 C11 Zr2 72.2(2) . . ? C12 C11 H11 126.0 . . ? C15 C11 H11 126.0 . . ? Zr2 C11 H11 119.5 . . ? C11 C12 C13 108.5(3) . . ? C11 C12 Zr2 74.0(2) . . ? C13 C12 Zr2 72.6(2) . . ? C11 C12 H12 125.8 . . ? C13 C12 H12 125.8 . . ? Zr2 C12 H12 119.4 . . ? C14 C13 C12 107.3(3) . . ? C14 C13 Zr2 73.5(2) . . ? C12 C13 Zr2 75.0(2) . . ? C14 C13 H13 126.4 . . ? C12 C13 H13 126.4 . . ? Zr2 C13 H13 117.3 . . ? C13 C14 C15 108.4(3) . . ? C13 C14 Zr2 74.3(2) . . ? C15 C14 Zr2 73.4(2) . . ? C13 C14 H14 125.8 . . ? C15 C14 H14 125.8 . . ? Zr2 C14 H14 118.5 . . ? C11 C15 C14 107.7(4) . . ? C11 C15 Zr2 75.6(2) . . ? C14 C15 Zr2 73.9(2) . . ? C11 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? Zr2 C15 H15 116.5 . . ? C17 C16 C20 107.9(4) . . ? C17 C16 Zr2 74.5(2) . . ? C20 C16 Zr2 73.8(2) . . ? C17 C16 H16 126.1 . . ? C20 C16 H16 126.1 . . ? Zr2 C16 H16 117.6 . . ? C16 C17 C18 108.3(4) . . ? C16 C17 Zr2 72.9(2) . . ? C18 C17 Zr2 75.6(2) . . ? C16 C17 H17 125.8 . . ? C18 C17 H17 125.8 . . ? Zr2 C17 H17 117.6 . . ? C19 C18 C17 107.9(3) . . ? C19 C18 Zr2 73.9(2) . . ? C17 C18 Zr2 72.1(2) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? Zr2 C18 H18 119.8 . . ? C18 C19 C20 108.0(3) . . ? C18 C19 Zr2 74.2(2) . . ? C20 C19 Zr2 71.5(2) . . ? C18 C19 H19 126.0 . . ? C20 C19 H19 126.0 . . ? Zr2 C19 H19 120.1 . . ? C16 C20 C19 107.8(3) . . ? C16 C20 Zr2 73.4(2) . . ? C19 C20 Zr2 76.0(2) . . ? C16 C20 H20 126.1 . . ? C19 C20 H20 126.1 . . ? Zr2 C20 H20 116.7 . . ? P1 C21 Si1 125.4(2) . . ? P1 C21 Zr2 83.93(14) . . ? Si1 C21 Zr2 150.55(18) . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P2 C25 Si2 124.81(18) . . ? P2 C25 Zr1 108.98(16) . . ? Si2 C25 Zr1 126.17(15) . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 114.7(3) . . ? C34 C29 P2 121.8(3) . . ? C30 C29 P2 123.5(2) . . ? F1 C30 C31 118.5(3) . . ? F1 C30 C29 119.0(3) . . ? C31 C30 C29 122.5(3) . . ? F2 C31 C30 115.7(3) . . ? F2 C31 C32 120.6(3) . . ? C30 C31 C32 123.7(3) . . ? C31 C32 C33 112.5(3) . . ? C31 C32 B1 128.2(3) . . ? C33 C32 B1 119.0(3) . . ? F3 C33 C34 116.2(3) . . ? F3 C33 C32 119.4(3) . . ? C34 C33 C32 124.4(3) . . ? F4 C34 C33 119.0(3) . . ? F4 C34 C29 118.9(3) . . ? C33 C34 C29 122.1(3) . . ? C40 C35 C36 113.3(3) . . ? C40 C35 B1 127.8(3) . . ? C36 C35 B1 118.8(3) . . ? F5 C36 C37 115.9(3) . . ? F5 C36 C35 120.3(3) . . ? C37 C36 C35 123.8(3) . . ? F6 C37 C38 119.6(3) . . ? F6 C37 C36 120.5(4) . . ? C38 C37 C36 119.9(3) . . ? F7 C38 C37 120.7(3) . . ? F7 C38 C39 120.3(4) . . ? C37 C38 C39 118.9(3) . . ? F8 C39 C38 119.7(3) . . ? F8 C39 C40 120.4(3) . . ? C38 C39 C40 119.8(4) . . ? F9 C40 C39 114.9(3) . . ? F9 C40 C35 120.9(3) . . ? C39 C40 C35 124.2(3) . . ? C42 C41 C46 113.1(3) . . ? C42 C41 B1 125.1(3) . . ? C46 C41 B1 121.5(3) . . ? F10 C42 C43 114.8(3) . . ? F10 C42 C41 121.0(3) . . ? C43 C42 C41 124.2(3) . . ? F11 C43 C42 121.1(3) . . ? F11 C43 C44 118.9(3) . . ? C42 C43 C44 120.0(3) . . ? F12 C44 C45 120.8(3) . . ? F12 C44 C43 120.2(4) . . ? C45 C44 C43 119.0(3) . . ? F13 C45 C44 119.5(3) . . ? F13 C45 C46 121.1(3) . . ? C44 C45 C46 119.4(3) . . ? F14 C46 C45 116.8(3) . . ? F14 C46 C41 118.8(3) . . ? C45 C46 C41 124.4(3) . . ? C52 C47 C48 119.6(4) . . ? C52 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C49 C48 C47 119.6(5) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.2(5) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 120.3(4) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 120.7(5) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C51 C52 C47 119.5(5) . . ? C51 C52 H52 120.2 . . ? C47 C52 H52 120.2 . . ? C55 C53 C54 121.1(6) . 2_757 ? C55 C53 H53 120.4 . . ? C54 C53 H53 118.5 2_757 . ? C53 C54 C55 118.7(7) 2_757 . ? C53 C54 H54 120.7 2_757 . ? C55 C54 H54 120.7 . . ? C53 C55 C54 120.2(6) . . ? C53 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? 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 C25 Zr1 P1 C21 -7.5(7) . . . . ? C3 Zr1 P1 C21 -123.8(7) . . . . ? C6 Zr1 P1 C21 110.2(7) . . . . ? C4 Zr1 P1 C21 -144.8(7) . . . . ? C7 Zr1 P1 C21 131.7(7) . . . . ? C10 Zr1 P1 C21 74.5(7) . . . . ? C2 Zr1 P1 C21 -88.3(7) . . . . ? C1 Zr1 P1 C21 -94.1(7) . . . . ? C9 Zr1 P1 C21 80.9(7) . . . . ? C5 Zr1 P1 C21 -126.0(7) . . . . ? C8 Zr1 P1 C21 113.1(7) . . . . ? C25 Zr1 P1 Zr2 -3.28(9) . . . . ? C3 Zr1 P1 Zr2 -119.65(14) . . . . ? C6 Zr1 P1 Zr2 114.34(12) . . . . ? C4 Zr1 P1 Zr2 -140.61(10) . . . . ? C7 Zr1 P1 Zr2 135.93(9) . . . . ? C10 Zr1 P1 Zr2 78.64(10) . . . . ? C2 Zr1 P1 Zr2 -84.11(10) . . . . ? C1 Zr1 P1 Zr2 -89.88(9) . . . . ? C9 Zr1 P1 Zr2 85.04(9) . . . . ? C5 Zr1 P1 Zr2 -121.81(10) . . . . ? C8 Zr1 P1 Zr2 117.27(9) . . . . ? C16 Zr2 P1 C21 58.0(2) . . . . ? C20 Zr2 P1 C21 103.6(2) . . . . ? C15 Zr2 P1 C21 -49.99(18) . . . . ? C14 Zr2 P1 C21 -62.1(2) . . . . ? C17 Zr2 P1 C21 55.04(18) . . . . ? C13 Zr2 P1 C21 -106.94(19) . . . . ? C11 Zr2 P1 C21 -74.67(17) . . . . ? C12 Zr2 P1 C21 -104.03(17) . . . . ? C19 Zr2 P1 C21 109.42(17) . . . . ? C18 Zr2 P1 C21 83.11(17) . . . . ? C21 Zr2 P1 Zr1 -179.08(16) . . . . ? C16 Zr2 P1 Zr1 -121.11(14) . . . . ? C20 Zr2 P1 Zr1 -75.48(14) . . . . ? C15 Zr2 P1 Zr1 130.93(10) . . . . ? C14 Zr2 P1 Zr1 118.80(15) . . . . ? C17 Zr2 P1 Zr1 -124.04(10) . . . . ? C13 Zr2 P1 Zr1 73.98(13) . . . . ? C11 Zr2 P1 Zr1 106.25(10) . . . . ? C12 Zr2 P1 Zr1 76.88(9) . . . . ? C19 Zr2 P1 Zr1 -69.67(10) . . . . ? C18 Zr2 P1 Zr1 -95.97(10) . . . . ? C21 Zr2 P2 C25 -9.5(2) . . . . ? C16 Zr2 P2 C25 128.7(2) . . . . ? C20 Zr2 P2 C25 127.93(18) . . . . ? C15 Zr2 P2 C25 -113.6(2) . . . . ? C14 Zr2 P2 C25 -146.83(19) . . . . ? C17 Zr2 P2 C25 90.1(2) . . . . ? C13 Zr2 P2 C25 -141.03(19) . . . . ? C11 Zr2 P2 C25 -91.87(18) . . . . ? C12 Zr2 P2 C25 -108.17(18) . . . . ? C19 Zr2 P2 C25 97.20(18) . . . . ? C18 Zr2 P2 C25 75.44(18) . . . . ? P1 Zr2 P2 C25 -7.08(16) . . . . ? C21 Zr2 P2 C29 169.42(16) . . . . ? C16 Zr2 P2 C29 -52.40(17) . . . . ? C20 Zr2 P2 C29 -53.13(15) . . . . ? C15 Zr2 P2 C29 65.35(17) . . . . ? C14 Zr2 P2 C29 32.12(16) . . . . ? C17 Zr2 P2 C29 -90.98(17) . . . . ? C13 Zr2 P2 C29 37.91(15) . . . . ? C11 Zr2 P2 C29 87.08(15) . . . . ? C12 Zr2 P2 C29 70.77(15) . . . . ? C19 Zr2 P2 C29 -83.86(15) . . . . ? C18 Zr2 P2 C29 -105.62(15) . . . . ? P1 Zr2 P2 C29 171.86(12) . . . . ? C25 Zr1 C1 C5 -179.2(2) . . . . ? C3 Zr1 C1 C5 77.8(2) . . . . ? C6 Zr1 C1 C5 78.4(3) . . . . ? C4 Zr1 C1 C5 36.7(2) . . . . ? C7 Zr1 C1 C5 30.3(3) . . . . ? P1 Zr1 C1 C5 -74.6(2) . . . . ? C10 Zr1 C1 C5 132.0(3) . . . . ? C2 Zr1 C1 C5 115.1(3) . . . . ? C9 Zr1 C1 C5 -99.3(6) . . . . ? C8 Zr1 C1 C5 -18.0(4) . . . . ? C25 Zr1 C1 C2 65.7(2) . . . . ? C3 Zr1 C1 C2 -37.3(2) . . . . ? C6 Zr1 C1 C2 -36.6(3) . . . . ? C4 Zr1 C1 C2 -78.4(2) . . . . ? C7 Zr1 C1 C2 -84.8(3) . . . . ? P1 Zr1 C1 C2 170.3(2) . . . . ? C10 Zr1 C1 C2 16.9(4) . . . . ? C9 Zr1 C1 C2 145.6(6) . . . . ? C5 Zr1 C1 C2 -115.1(3) . . . . ? C8 Zr1 C1 C2 -133.1(3) . . . . ? C5 C1 C2 C3 -1.4(4) . . . . ? Zr1 C1 C2 C3 65.0(3) . . . . ? C5 C1 C2 Zr1 -66.4(3) . . . . ? C25 Zr1 C2 C3 135.1(3) . . . . ? C6 Zr1 C2 C3 39.9(3) . . . . ? C4 Zr1 C2 C3 -37.7(2) . . . . ? C7 Zr1 C2 C3 6.1(3) . . . . ? P1 Zr1 C2 C3 -125.7(2) . . . . ? C10 Zr1 C2 C3 73.1(3) . . . . ? C1 Zr1 C2 C3 -114.9(3) . . . . ? C9 Zr1 C2 C3 82.5(4) . . . . ? C5 Zr1 C2 C3 -78.1(2) . . . . ? C8 Zr1 C2 C3 -4.4(5) . . . . ? C25 Zr1 C2 C1 -109.9(2) . . . . ? C3 Zr1 C2 C1 114.9(3) . . . . ? C6 Zr1 C2 C1 154.9(2) . . . . ? C4 Zr1 C2 C1 77.2(2) . . . . ? C7 Zr1 C2 C1 121.1(2) . . . . ? P1 Zr1 C2 C1 -10.7(2) . . . . ? C10 Zr1 C2 C1 -171.9(2) . . . . ? C9 Zr1 C2 C1 -162.6(3) . . . . ? C5 Zr1 C2 C1 36.8(2) . . . . ? C8 Zr1 C2 C1 110.5(3) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? Zr1 C2 C3 C4 67.4(3) . . . . ? C1 C2 C3 Zr1 -66.6(3) . . . . ? C25 Zr1 C3 C2 -43.8(2) . . . . ? C6 Zr1 C3 C2 -142.6(3) . . . . ? C4 Zr1 C3 C2 114.2(3) . . . . ? C7 Zr1 C3 C2 -174.9(2) . . . . ? P1 Zr1 C3 C2 74.5(3) . . . . ? C10 Zr1 C3 C2 -122.9(2) . . . . ? C1 Zr1 C3 C2 37.0(2) . . . . ? C9 Zr1 C3 C2 -143.9(2) . . . . ? C5 Zr1 C3 C2 77.1(3) . . . . ? C8 Zr1 C3 C2 177.8(2) . . . . ? C25 Zr1 C3 C4 -158.1(2) . . . . ? C6 Zr1 C3 C4 103.2(2) . . . . ? C7 Zr1 C3 C4 70.9(2) . . . . ? P1 Zr1 C3 C4 -39.7(3) . . . . ? C10 Zr1 C3 C4 122.9(2) . . . . ? C2 Zr1 C3 C4 -114.2(3) . . . . ? C1 Zr1 C3 C4 -77.2(3) . . . . ? C9 Zr1 C3 C4 101.9(3) . . . . ? C5 Zr1 C3 C4 -37.1(2) . . . . ? C8 Zr1 C3 C4 63.6(3) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? Zr1 C3 C4 C5 68.0(3) . . . . ? C2 C3 C4 Zr1 -68.0(3) . . . . ? C25 Zr1 C4 C5 -85.9(3) . . . . ? C3 Zr1 C4 C5 -114.4(4) . . . . ? C6 Zr1 C4 C5 170.1(3) . . . . ? C7 Zr1 C4 C5 138.9(3) . . . . ? P1 Zr1 C4 C5 35.8(3) . . . . ? C10 Zr1 C4 C5 172.3(2) . . . . ? C2 Zr1 C4 C5 -77.0(3) . . . . ? C1 Zr1 C4 C5 -36.5(2) . . . . ? C9 Zr1 C4 C5 131.7(3) . . . . ? C8 Zr1 C4 C5 116.7(3) . . . . ? C25 Zr1 C4 C3 28.5(3) . . . . ? C6 Zr1 C4 C3 -75.5(2) . . . . ? C7 Zr1 C4 C3 -106.7(2) . . . . ? P1 Zr1 C4 C3 150.2(2) . . . . ? C10 Zr1 C4 C3 -73.3(3) . . . . ? C2 Zr1 C4 C3 37.5(2) . . . . ? C1 Zr1 C4 C3 77.9(3) . . . . ? C9 Zr1 C4 C3 -113.9(3) . . . . ? C5 Zr1 C4 C3 114.4(4) . . . . ? C8 Zr1 C4 C3 -128.8(2) . . . . ? C3 C4 C5 C1 -0.9(4) . . . . ? Zr1 C4 C5 C1 65.2(3) . . . . ? C3 C4 C5 Zr1 -66.1(3) . . . . ? C2 C1 C5 C4 1.4(4) . . . . ? Zr1 C1 C5 C4 -64.2(3) . . . . ? C2 C1 C5 Zr1 65.6(3) . . . . ? C25 Zr1 C5 C4 116.7(2) . . . . ? C3 Zr1 C5 C4 37.8(2) . . . . ? C6 Zr1 C5 C4 -12.0(3) . . . . ? C7 Zr1 C5 C4 -42.1(3) . . . . ? P1 Zr1 C5 C4 -144.2(3) . . . . ? C10 Zr1 C5 C4 -16.1(5) . . . . ? C2 Zr1 C5 C4 78.7(3) . . . . ? C1 Zr1 C5 C4 115.8(4) . . . . ? C9 Zr1 C5 C4 -87.0(3) . . . . ? C8 Zr1 C5 C4 -74.8(3) . . . . ? C25 Zr1 C5 C1 0.9(3) . . . . ? C3 Zr1 C5 C1 -78.0(3) . . . . ? C6 Zr1 C5 C1 -127.8(2) . . . . ? C4 Zr1 C5 C1 -115.8(4) . . . . ? C7 Zr1 C5 C1 -158.0(2) . . . . ? P1 Zr1 C5 C1 99.9(2) . . . . ? C10 Zr1 C5 C1 -132.0(3) . . . . ? C2 Zr1 C5 C1 -37.2(2) . . . . ? C9 Zr1 C5 C1 157.2(2) . . . . ? C8 Zr1 C5 C1 169.4(2) . . . . ? C25 Zr1 C6 C10 46.0(2) . . . . ? C3 Zr1 C6 C10 144.6(2) . . . . ? C4 Zr1 C6 C10 176.6(2) . . . . ? C7 Zr1 C6 C10 -114.1(3) . . . . ? P1 Zr1 C6 C10 -73.5(2) . . . . ? C2 Zr1 C6 C10 124.1(2) . . . . ? C1 Zr1 C6 C10 144.0(2) . . . . ? C9 Zr1 C6 C10 -36.5(2) . . . . ? C5 Zr1 C6 C10 -177.0(2) . . . . ? C8 Zr1 C6 C10 -77.0(2) . . . . ? C25 Zr1 C6 C7 160.2(2) . . . . ? C3 Zr1 C6 C7 -101.3(2) . . . . ? C4 Zr1 C6 C7 -69.2(2) . . . . ? P1 Zr1 C6 C7 40.7(3) . . . . ? C10 Zr1 C6 C7 114.1(3) . . . . ? C2 Zr1 C6 C7 -121.8(2) . . . . ? C1 Zr1 C6 C7 -101.8(3) . . . . ? C9 Zr1 C6 C7 77.6(2) . . . . ? C5 Zr1 C6 C7 -62.8(3) . . . . ? C8 Zr1 C6 C7 37.1(2) . . . . ? C10 C6 C7 C8 -0.4(4) . . . . ? Zr1 C6 C7 C8 -67.9(3) . . . . ? C10 C6 C7 Zr1 67.5(2) . . . . ? C25 Zr1 C7 C8 88.3(3) . . . . ? C3 Zr1 C7 C8 -168.5(2) . . . . ? C6 Zr1 C7 C8 114.3(3) . . . . ? C4 Zr1 C7 C8 -137.1(2) . . . . ? P1 Zr1 C7 C8 -35.7(2) . . . . ? C10 Zr1 C7 C8 76.7(2) . . . . ? C2 Zr1 C7 C8 -171.8(2) . . . . ? C1 Zr1 C7 C8 -131.9(2) . . . . ? C9 Zr1 C7 C8 36.6(2) . . . . ? C5 Zr1 C7 C8 -115.7(2) . . . . ? C25 Zr1 C7 C6 -26.0(3) . . . . ? C3 Zr1 C7 C6 77.1(2) . . . . ? C4 Zr1 C7 C6 108.6(2) . . . . ? P1 Zr1 C7 C6 -150.0(2) . . . . ? C10 Zr1 C7 C6 -37.6(2) . . . . ? C2 Zr1 C7 C6 73.8(3) . . . . ? C1 Zr1 C7 C6 113.8(3) . . . . ? C9 Zr1 C7 C6 -77.7(2) . . . . ? C5 Zr1 C7 C6 130.0(2) . . . . ? C8 Zr1 C7 C6 -114.3(3) . . . . ? C6 C7 C8 C9 1.1(4) . . . . ? Zr1 C7 C8 C9 -65.1(3) . . . . ? C6 C7 C8 Zr1 66.2(3) . . . . ? C25 Zr1 C8 C7 -115.5(2) . . . . ? C3 Zr1 C8 C7 13.6(3) . . . . ? C6 Zr1 C8 C7 -37.9(2) . . . . ? C4 Zr1 C8 C7 43.9(2) . . . . ? P1 Zr1 C8 C7 144.8(2) . . . . ? C10 Zr1 C8 C7 -79.0(2) . . . . ? C2 Zr1 C8 C7 16.5(4) . . . . ? C1 Zr1 C8 C7 86.8(3) . . . . ? C9 Zr1 C8 C7 -116.0(3) . . . . ? C5 Zr1 C8 C7 76.2(2) . . . . ? C25 Zr1 C8 C9 0.4(3) . . . . ? C3 Zr1 C8 C9 129.6(2) . . . . ? C6 Zr1 C8 C9 78.1(2) . . . . ? C4 Zr1 C8 C9 159.9(2) . . . . ? C7 Zr1 C8 C9 116.0(3) . . . . ? P1 Zr1 C8 C9 -99.2(2) . . . . ? C10 Zr1 C8 C9 37.0(2) . . . . ? C2 Zr1 C8 C9 132.4(3) . . . . ? C1 Zr1 C8 C9 -157.2(2) . . . . ? C5 Zr1 C8 C9 -167.8(2) . . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? Zr1 C8 C9 C10 -65.6(2) . . . . ? C7 C8 C9 Zr1 64.2(3) . . . . ? C25 Zr1 C9 C10 -64.8(2) . . . . ? C3 Zr1 C9 C10 38.9(3) . . . . ? C6 Zr1 C9 C10 37.3(2) . . . . ? C4 Zr1 C9 C10 87.1(3) . . . . ? C7 Zr1 C9 C10 78.3(2) . . . . ? P1 Zr1 C9 C10 -169.3(2) . . . . ? C2 Zr1 C9 C10 -14.4(4) . . . . ? C1 Zr1 C9 C10 -144.6(6) . . . . ? C5 Zr1 C9 C10 135.5(2) . . . . ? C8 Zr1 C9 C10 114.8(3) . . . . ? C25 Zr1 C9 C8 -179.6(2) . . . . ? C3 Zr1 C9 C8 -75.9(3) . . . . ? C6 Zr1 C9 C8 -77.5(2) . . . . ? C4 Zr1 C9 C8 -27.7(3) . . . . ? C7 Zr1 C9 C8 -36.5(2) . . . . ? P1 Zr1 C9 C8 75.9(2) . . . . ? C10 Zr1 C9 C8 -114.8(3) . . . . ? C2 Zr1 C9 C8 -129.2(3) . . . . ? C1 Zr1 C9 C8 100.6(6) . . . . ? C5 Zr1 C9 C8 20.7(3) . . . . ? C8 C9 C10 C6 1.2(4) . . . . ? Zr1 C9 C10 C6 -65.2(2) . . . . ? C8 C9 C10 Zr1 66.4(3) . . . . ? C7 C6 C10 C9 -0.5(4) . . . . ? Zr1 C6 C10 C9 66.7(2) . . . . ? C7 C6 C10 Zr1 -67.2(3) . . . . ? C25 Zr1 C10 C9 111.5(2) . . . . ? C3 Zr1 C10 C9 -153.3(2) . . . . ? C6 Zr1 C10 C9 -115.4(3) . . . . ? C4 Zr1 C10 C9 -119.5(2) . . . . ? C7 Zr1 C10 C9 -77.6(2) . . . . ? P1 Zr1 C10 C9 12.0(2) . . . . ? C2 Zr1 C10 C9 173.1(2) . . . . ? C1 Zr1 C10 C9 162.1(3) . . . . ? C5 Zr1 C10 C9 -109.0(4) . . . . ? C8 Zr1 C10 C9 -37.3(2) . . . . ? C25 Zr1 C10 C6 -133.1(2) . . . . ? C3 Zr1 C10 C6 -38.0(3) . . . . ? C4 Zr1 C10 C6 -4.1(3) . . . . ? C7 Zr1 C10 C6 37.8(2) . . . . ? P1 Zr1 C10 C6 127.4(2) . . . . ? C2 Zr1 C10 C6 -71.5(3) . . . . ? C1 Zr1 C10 C6 -82.5(4) . . . . ? C9 Zr1 C10 C6 115.4(3) . . . . ? C5 Zr1 C10 C6 6.4(5) . . . . ? C8 Zr1 C10 C6 78.1(2) . . . . ? C21 Zr2 C11 C12 -150.0(2) . . . . ? C16 Zr2 C11 C12 107.3(2) . . . . ? C20 Zr2 C11 C12 68.9(3) . . . . ? C15 Zr2 C11 C12 115.4(3) . . . . ? C14 Zr2 C11 C12 77.3(2) . . . . ? C17 Zr2 C11 C12 147.2(2) . . . . ? C13 Zr2 C11 C12 36.9(2) . . . . ? C19 Zr2 C11 C12 41.3(9) . . . . ? C18 Zr2 C11 C12 -179.0(3) . . . . ? P1 Zr2 C11 C12 -113.0(2) . . . . ? C21 Zr2 C11 C15 94.6(2) . . . . ? C16 Zr2 C11 C15 -8.1(3) . . . . ? C20 Zr2 C11 C15 -46.5(3) . . . . ? C14 Zr2 C11 C15 -38.1(2) . . . . ? C17 Zr2 C11 C15 31.8(3) . . . . ? C13 Zr2 C11 C15 -78.5(3) . . . . ? C12 Zr2 C11 C15 -115.4(3) . . . . ? C19 Zr2 C11 C15 -74.1(8) . . . . ? C18 Zr2 C11 C15 65.6(4) . . . . ? P1 Zr2 C11 C15 131.6(2) . . . . ? C15 C11 C12 C13 -0.2(4) . . . . ? Zr2 C11 C12 C13 -64.9(3) . . . . ? C15 C11 C12 Zr2 64.8(3) . . . . ? C21 Zr2 C12 C11 30.4(2) . . . . ? C16 Zr2 C12 C11 -95.2(3) . . . . ? C20 Zr2 C12 C11 -134.7(2) . . . . ? C15 Zr2 C12 C11 -36.9(2) . . . . ? C14 Zr2 C12 C11 -78.2(2) . . . . ? C17 Zr2 C12 C11 -62.9(4) . . . . ? C13 Zr2 C12 C11 -115.8(3) . . . . ? C19 Zr2 C12 C11 -170.3(2) . . . . ? C18 Zr2 C12 C11 176.9(8) . . . . ? P1 Zr2 C12 C11 68.3(2) . . . . ? C21 Zr2 C12 C13 146.3(2) . . . . ? C16 Zr2 C12 C13 20.6(3) . . . . ? C20 Zr2 C12 C13 -18.9(3) . . . . ? C15 Zr2 C12 C13 78.9(2) . . . . ? C14 Zr2 C12 C13 37.6(2) . . . . ? C17 Zr2 C12 C13 52.9(4) . . . . ? C11 Zr2 C12 C13 115.8(3) . . . . ? C19 Zr2 C12 C13 -54.5(3) . . . . ? C18 Zr2 C12 C13 -67.3(10) . . . . ? P1 Zr2 C12 C13 -175.9(2) . . . . ? C11 C12 C13 C14 -1.1(4) . . . . ? Zr2 C12 C13 C14 -66.9(3) . . . . ? C11 C12 C13 Zr2 65.8(3) . . . . ? C21 Zr2 C13 C14 68.6(3) . . . . ? C16 Zr2 C13 C14 -49.9(3) . . . . ? C20 Zr2 C13 C14 -82.4(3) . . . . ? C15 Zr2 C13 C14 37.3(2) . . . . ? C17 Zr2 C13 C14 -38.7(3) . . . . ? C11 Zr2 C13 C14 77.5(3) . . . . ? C12 Zr2 C13 C14 113.6(3) . . . . ? C19 Zr2 C13 C14 -101.7(2) . . . . ? C18 Zr2 C13 C14 -78.2(3) . . . . ? P1 Zr2 C13 C14 119.0(2) . . . . ? C21 Zr2 C13 C12 -45.1(3) . . . . ? C16 Zr2 C13 C12 -163.5(2) . . . . ? C20 Zr2 C13 C12 164.0(2) . . . . ? C15 Zr2 C13 C12 -76.3(2) . . . . ? C14 Zr2 C13 C12 -113.6(3) . . . . ? C17 Zr2 C13 C12 -152.4(2) . . . . ? C11 Zr2 C13 C12 -36.1(2) . . . . ? C19 Zr2 C13 C12 144.7(2) . . . . ? C18 Zr2 C13 C12 168.2(2) . . . . ? P1 Zr2 C13 C12 5.4(3) . . . . ? C12 C13 C14 C15 2.0(4) . . . . ? Zr2 C13 C14 C15 -66.0(3) . . . . ? C12 C13 C14 Zr2 67.9(3) . . . . ? C21 Zr2 C14 C13 -129.6(2) . . . . ? C16 Zr2 C14 C13 128.0(3) . . . . ? C20 Zr2 C14 C13 96.7(3) . . . . ? C15 Zr2 C14 C13 -115.2(4) . . . . ? C17 Zr2 C14 C13 149.3(2) . . . . ? C11 Zr2 C14 C13 -77.8(3) . . . . ? C12 Zr2 C14 C13 -37.9(2) . . . . ? C19 Zr2 C14 C13 96.0(3) . . . . ? C18 Zr2 C14 C13 132.9(2) . . . . ? P1 Zr2 C14 C13 -93.5(3) . . . . ? C21 Zr2 C14 C15 -14.4(3) . . . . ? C16 Zr2 C14 C15 -116.8(3) . . . . ? C20 Zr2 C14 C15 -148.0(3) . . . . ? C17 Zr2 C14 C15 -95.5(3) . . . . ? C13 Zr2 C14 C15 115.2(4) . . . . ? C11 Zr2 C14 C15 37.4(2) . . . . ? C12 Zr2 C14 C15 77.4(3) . . . . ? C19 Zr2 C14 C15 -148.8(2) . . . . ? C18 Zr2 C14 C15 -111.9(3) . . . . ? P1 Zr2 C14 C15 21.8(3) . . . . ? C12 C11 C15 C14 1.4(4) . . . . ? Zr2 C11 C15 C14 67.5(3) . . . . ? C12 C11 C15 Zr2 -66.1(3) . . . . ? C13 C14 C15 C11 -2.1(4) . . . . ? Zr2 C14 C15 C11 -68.7(3) . . . . ? C13 C14 C15 Zr2 66.6(3) . . . . ? C21 Zr2 C15 C11 -79.6(2) . . . . ? C16 Zr2 C15 C11 173.2(2) . . . . ? C20 Zr2 C15 C11 149.0(2) . . . . ? C14 Zr2 C15 C11 113.6(3) . . . . ? C17 Zr2 C15 C11 -155.6(2) . . . . ? C13 Zr2 C15 C11 77.0(3) . . . . ? C12 Zr2 C15 C11 36.4(2) . . . . ? C19 Zr2 C15 C11 164.6(2) . . . . ? C18 Zr2 C15 C11 -149.2(2) . . . . ? P1 Zr2 C15 C11 -51.5(2) . . . . ? C21 Zr2 C15 C14 166.8(3) . . . . ? C16 Zr2 C15 C14 59.6(3) . . . . ? C20 Zr2 C15 C14 35.3(3) . . . . ? C17 Zr2 C15 C14 90.7(3) . . . . ? C13 Zr2 C15 C14 -36.6(2) . . . . ? C11 Zr2 C15 C14 -113.6(3) . . . . ? C12 Zr2 C15 C14 -77.2(3) . . . . ? C19 Zr2 C15 C14 51.0(3) . . . . ? C18 Zr2 C15 C14 97.1(3) . . . . ? P1 Zr2 C15 C14 -165.1(2) . . . . ? C21 Zr2 C16 C17 27.4(3) . . . . ? C20 Zr2 C16 C17 -114.4(4) . . . . ? C15 Zr2 C16 C17 109.4(3) . . . . ? C14 Zr2 C16 C17 138.3(3) . . . . ? C13 Zr2 C16 C17 163.2(3) . . . . ? C11 Zr2 C16 C17 113.7(3) . . . . ? C12 Zr2 C16 C17 152.3(2) . . . . ? C19 Zr2 C16 C17 -76.8(3) . . . . ? C18 Zr2 C16 C17 -37.0(2) . . . . ? P1 Zr2 C16 C17 -5.4(3) . . . . ? C21 Zr2 C16 C20 141.8(2) . . . . ? C15 Zr2 C16 C20 -136.3(2) . . . . ? C14 Zr2 C16 C20 -107.4(3) . . . . ? C17 Zr2 C16 C20 114.4(4) . . . . ? C13 Zr2 C16 C20 -82.4(2) . . . . ? C11 Zr2 C16 C20 -132.0(2) . . . . ? C12 Zr2 C16 C20 -93.3(3) . . . . ? C19 Zr2 C16 C20 37.5(2) . . . . ? C18 Zr2 C16 C20 77.4(3) . . . . ? P1 Zr2 C16 C20 109.0(2) . . . . ? C20 C16 C17 C18 1.1(5) . . . . ? Zr2 C16 C17 C18 67.9(3) . . . . ? C20 C16 C17 Zr2 -66.8(3) . . . . ? C21 Zr2 C17 C16 -153.3(3) . . . . ? C20 Zr2 C17 C16 37.6(2) . . . . ? C15 Zr2 C17 C16 -74.0(3) . . . . ? C14 Zr2 C17 C16 -40.7(3) . . . . ? C13 Zr2 C17 C16 -20.9(3) . . . . ? C11 Zr2 C17 C16 -90.6(3) . . . . ? C12 Zr2 C17 C16 -53.1(4) . . . . ? C19 Zr2 C17 C16 78.3(3) . . . . ? C18 Zr2 C17 C16 114.7(4) . . . . ? P1 Zr2 C17 C16 176.0(2) . . . . ? C21 Zr2 C17 C18 92.0(2) . . . . ? C16 Zr2 C17 C18 -114.7(4) . . . . ? C20 Zr2 C17 C18 -77.1(2) . . . . ? C15 Zr2 C17 C18 171.2(2) . . . . ? C14 Zr2 C17 C18 -155.4(2) . . . . ? C13 Zr2 C17 C18 -135.6(2) . . . . ? C11 Zr2 C17 C18 154.6(2) . . . . ? C12 Zr2 C17 C18 -167.8(3) . . . . ? C19 Zr2 C17 C18 -36.5(2) . . . . ? P1 Zr2 C17 C18 61.2(2) . . . . ? C16 C17 C18 C19 -0.3(4) . . . . ? Zr2 C17 C18 C19 65.8(3) . . . . ? C16 C17 C18 Zr2 -66.1(3) . . . . ? C21 Zr2 C18 C19 162.7(2) . . . . ? C16 Zr2 C18 C19 -78.1(2) . . . . ? C20 Zr2 C18 C19 -37.0(2) . . . . ? C15 Zr2 C18 C19 -127.2(2) . . . . ? C14 Zr2 C18 C19 -83.9(3) . . . . ? C17 Zr2 C18 C19 -115.4(3) . . . . ? C13 Zr2 C18 C19 -42.1(3) . . . . ? C11 Zr2 C18 C19 -168.6(3) . . . . ? C12 Zr2 C18 C19 15.3(10) . . . . ? P1 Zr2 C18 C19 124.9(2) . . . . ? C21 Zr2 C18 C17 -81.9(2) . . . . ? C16 Zr2 C18 C17 37.4(2) . . . . ? C20 Zr2 C18 C17 78.5(3) . . . . ? C15 Zr2 C18 C17 -11.8(3) . . . . ? C14 Zr2 C18 C17 31.5(3) . . . . ? C13 Zr2 C18 C17 73.3(3) . . . . ? C11 Zr2 C18 C17 -53.2(4) . . . . ? C12 Zr2 C18 C17 130.8(9) . . . . ? C19 Zr2 C18 C17 115.4(3) . . . . ? P1 Zr2 C18 C17 -119.7(2) . . . . ? C17 C18 C19 C20 -0.6(4) . . . . ? Zr2 C18 C19 C20 64.0(3) . . . . ? C17 C18 C19 Zr2 -64.6(3) . . . . ? C21 Zr2 C19 C18 -18.4(2) . . . . ? C16 Zr2 C19 C18 77.7(2) . . . . ? C20 Zr2 C19 C18 115.7(3) . . . . ? C15 Zr2 C19 C18 88.4(3) . . . . ? C14 Zr2 C19 C18 117.1(2) . . . . ? C17 Zr2 C19 C18 36.9(2) . . . . ? C13 Zr2 C19 C18 153.7(2) . . . . ? C11 Zr2 C19 C18 149.7(7) . . . . ? C12 Zr2 C19 C18 -176.9(2) . . . . ? P1 Zr2 C19 C18 -56.5(2) . . . . ? C21 Zr2 C19 C20 -134.1(2) . . . . ? C16 Zr2 C19 C20 -38.0(2) . . . . ? C15 Zr2 C19 C20 -27.3(3) . . . . ? C14 Zr2 C19 C20 1.4(3) . . . . ? C17 Zr2 C19 C20 -78.8(3) . . . . ? C13 Zr2 C19 C20 38.0(3) . . . . ? C11 Zr2 C19 C20 34.0(9) . . . . ? C12 Zr2 C19 C20 67.4(3) . . . . ? C18 Zr2 C19 C20 -115.7(3) . . . . ? P1 Zr2 C19 C20 -172.2(2) . . . . ? C17 C16 C20 C19 -1.5(4) . . . . ? Zr2 C16 C20 C19 -68.8(3) . . . . ? C17 C16 C20 Zr2 67.3(3) . . . . ? C18 C19 C20 C16 1.3(4) . . . . ? Zr2 C19 C20 C16 67.0(3) . . . . ? C18 C19 C20 Zr2 -65.7(3) . . . . ? C21 Zr2 C20 C16 -51.5(3) . . . . ? C15 Zr2 C20 C16 49.1(3) . . . . ? C14 Zr2 C20 C16 67.4(3) . . . . ? C17 Zr2 C20 C16 -37.3(2) . . . . ? C13 Zr2 C20 C16 99.4(3) . . . . ? C11 Zr2 C20 C16 74.2(3) . . . . ? C12 Zr2 C20 C16 109.4(3) . . . . ? C19 Zr2 C20 C16 -113.8(3) . . . . ? C18 Zr2 C20 C16 -77.6(3) . . . . ? P1 Zr2 C20 C16 -103.2(2) . . . . ? C21 Zr2 C20 C19 62.3(3) . . . . ? C16 Zr2 C20 C19 113.8(3) . . . . ? C15 Zr2 C20 C19 162.9(2) . . . . ? C14 Zr2 C20 C19 -178.8(2) . . . . ? C17 Zr2 C20 C19 76.5(3) . . . . ? C13 Zr2 C20 C19 -146.8(2) . . . . ? C11 Zr2 C20 C19 -172.0(2) . . . . ? C12 Zr2 C20 C19 -136.8(2) . . . . ? C18 Zr2 C20 C19 36.2(2) . . . . ? P1 Zr2 C20 C19 10.6(3) . . . . ? Zr1 P1 C21 Si1 -172.2(5) . . . . ? Zr2 P1 C21 Si1 -176.8(3) . . . . ? Zr1 P1 C21 Zr2 4.6(8) . . . . ? C23 Si1 C21 P1 82.0(3) . . . . ? C24 Si1 C21 P1 -157.3(3) . . . . ? C22 Si1 C21 P1 -36.6(3) . . . . ? C23 Si1 C21 Zr2 -91.5(4) . . . . ? C24 Si1 C21 Zr2 29.2(5) . . . . ? C22 Si1 C21 Zr2 149.9(4) . . . . ? C16 Zr2 C21 P1 -139.03(15) . . . . ? C20 Zr2 C21 P1 -112.65(17) . . . . ? C15 Zr2 C21 P1 132.41(16) . . . . ? C14 Zr2 C21 P1 140.21(14) . . . . ? C17 Zr2 C21 P1 -124.36(16) . . . . ? C13 Zr2 C21 P1 107.32(17) . . . . ? C11 Zr2 C21 P1 99.99(15) . . . . ? C12 Zr2 C21 P1 84.14(15) . . . . ? C19 Zr2 C21 P1 -81.95(16) . . . . ? C18 Zr2 C21 P1 -91.67(15) . . . . ? C16 Zr2 C21 Si1 35.7(4) . . . . ? C20 Zr2 C21 Si1 62.1(4) . . . . ? C15 Zr2 C21 Si1 -52.9(4) . . . . ? C14 Zr2 C21 Si1 -45.1(4) . . . . ? C17 Zr2 C21 Si1 50.3(4) . . . . ? C13 Zr2 C21 Si1 -78.0(4) . . . . ? C11 Zr2 C21 Si1 -85.3(4) . . . . ? C12 Zr2 C21 Si1 -101.2(4) . . . . ? C19 Zr2 C21 Si1 92.7(4) . . . . ? C18 Zr2 C21 Si1 83.0(4) . . . . ? P1 Zr2 C21 Si1 174.7(5) . . . . ? C29 P2 C25 Si2 5.0(3) . . . . ? Zr2 P2 C25 Si2 -176.05(11) . . . . ? C29 P2 C25 Zr1 -173.09(14) . . . . ? Zr2 P2 C25 Zr1 5.9(2) . . . . ? C28 Si2 C25 P2 172.6(2) . . . . ? C27 Si2 C25 P2 54.8(3) . . . . ? C26 Si2 C25 P2 -69.0(3) . . . . ? C28 Si2 C25 Zr1 -9.6(3) . . . . ? C27 Si2 C25 Zr1 -127.5(2) . . . . ? C26 Si2 C25 Zr1 108.7(2) . . . . ? C3 Zr1 C25 P2 135.66(17) . . . . ? C6 Zr1 C25 P2 -139.15(17) . . . . ? C4 Zr1 C25 P2 120.37(17) . . . . ? C7 Zr1 C25 P2 -125.13(17) . . . . ? P1 Zr1 C25 P2 -0.91(17) . . . . ? C10 Zr1 C25 P2 -115.40(18) . . . . ? C2 Zr1 C25 P2 112.88(19) . . . . ? C1 Zr1 C25 P2 82.47(18) . . . . ? C9 Zr1 C25 P2 -85.56(17) . . . . ? C5 Zr1 C25 P2 82.00(19) . . . . ? C8 Zr1 C25 P2 -85.80(19) . . . . ? C3 Zr1 C25 Si2 -42.4(2) . . . . ? C6 Zr1 C25 Si2 42.8(2) . . . . ? C4 Zr1 C25 Si2 -57.7(2) . . . . ? C7 Zr1 C25 Si2 56.8(3) . . . . ? P1 Zr1 C25 Si2 -178.94(16) . . . . ? C10 Zr1 C25 Si2 66.6(2) . . . . ? C2 Zr1 C25 Si2 -65.2(2) . . . . ? C1 Zr1 C25 Si2 -95.6(2) . . . . ? C9 Zr1 C25 Si2 96.4(2) . . . . ? C5 Zr1 C25 Si2 -96.0(2) . . . . ? C8 Zr1 C25 Si2 96.2(2) . . . . ? C25 P2 C29 C34 -101.7(3) . . . . ? Zr2 P2 C29 C34 79.2(3) . . . . ? C25 P2 C29 C30 80.8(3) . . . . ? Zr2 P2 C29 C30 -98.3(3) . . . . ? C34 C29 C30 F1 -178.5(3) . . . . ? P2 C29 C30 F1 -0.8(4) . . . . ? C34 C29 C30 C31 2.4(5) . . . . ? P2 C29 C30 C31 -179.9(3) . . . . ? F1 C30 C31 F2 -1.6(4) . . . . ? C29 C30 C31 F2 177.5(3) . . . . ? F1 C30 C31 C32 178.7(3) . . . . ? C29 C30 C31 C32 -2.2(5) . . . . ? F2 C31 C32 C33 -178.4(3) . . . . ? C30 C31 C32 C33 1.3(5) . . . . ? F2 C31 C32 B1 -3.8(5) . . . . ? C30 C31 C32 B1 175.8(3) . . . . ? C41 B1 C32 C31 10.4(5) . . . . ? C35 B1 C32 C31 128.8(3) . . . . ? F15 B1 C32 C31 -110.3(4) . . . . ? C41 B1 C32 C33 -175.3(3) . . . . ? C35 B1 C32 C33 -57.0(4) . . . . ? F15 B1 C32 C33 64.0(4) . . . . ? C31 C32 C33 F3 179.5(3) . . . . ? B1 C32 C33 F3 4.4(5) . . . . ? C31 C32 C33 C34 -0.9(5) . . . . ? B1 C32 C33 C34 -176.0(3) . . . . ? F3 C33 C34 F4 0.3(5) . . . . ? C32 C33 C34 F4 -179.3(3) . . . . ? F3 C33 C34 C29 -179.0(3) . . . . ? C32 C33 C34 C29 1.4(5) . . . . ? C30 C29 C34 F4 178.7(3) . . . . ? P2 C29 C34 F4 1.0(4) . . . . ? C30 C29 C34 C33 -2.0(5) . . . . ? P2 C29 C34 C33 -179.8(3) . . . . ? C41 B1 C35 C40 107.9(4) . . . . ? C32 B1 C35 C40 -16.2(5) . . . . ? F15 B1 C35 C40 -130.7(4) . . . . ? C41 B1 C35 C36 -68.1(4) . . . . ? C32 B1 C35 C36 167.7(3) . . . . ? F15 B1 C35 C36 53.3(4) . . . . ? C40 C35 C36 F5 -178.1(3) . . . . ? B1 C35 C36 F5 -1.5(5) . . . . ? C40 C35 C36 C37 1.3(5) . . . . ? B1 C35 C36 C37 177.9(3) . . . . ? F5 C36 C37 F6 0.5(5) . . . . ? C35 C36 C37 F6 -178.9(3) . . . . ? F5 C36 C37 C38 179.0(3) . . . . ? C35 C36 C37 C38 -0.4(6) . . . . ? F6 C37 C38 F7 -0.5(6) . . . . ? C36 C37 C38 F7 -179.0(3) . . . . ? F6 C37 C38 C39 178.4(3) . . . . ? C36 C37 C38 C39 -0.1(6) . . . . ? F7 C38 C39 F8 0.0(6) . . . . ? C37 C38 C39 F8 -178.9(3) . . . . ? F7 C38 C39 C40 178.6(3) . . . . ? C37 C38 C39 C40 -0.3(6) . . . . ? F8 C39 C40 F9 0.5(5) . . . . ? C38 C39 C40 F9 -178.0(3) . . . . ? F8 C39 C40 C35 179.9(3) . . . . ? C38 C39 C40 C35 1.3(6) . . . . ? C36 C35 C40 F9 177.6(3) . . . . ? B1 C35 C40 F9 1.4(5) . . . . ? C36 C35 C40 C39 -1.7(5) . . . . ? B1 C35 C40 C39 -177.9(3) . . . . ? C32 B1 C41 C42 -122.7(3) . . . . ? C35 B1 C41 C42 114.5(3) . . . . ? F15 B1 C41 C42 -7.6(5) . . . . ? C32 B1 C41 C46 64.1(4) . . . . ? C35 B1 C41 C46 -58.7(4) . . . . ? F15 B1 C41 C46 179.2(3) . . . . ? C46 C41 C42 F10 -179.4(3) . . . . ? B1 C41 C42 F10 7.0(5) . . . . ? C46 C41 C42 C43 1.2(5) . . . . ? B1 C41 C42 C43 -172.4(3) . . . . ? F10 C42 C43 F11 -0.7(5) . . . . ? C41 C42 C43 F11 178.8(3) . . . . ? F10 C42 C43 C44 179.5(3) . . . . ? C41 C42 C43 C44 -1.1(5) . . . . ? F11 C43 C44 F12 0.5(5) . . . . ? C42 C43 C44 F12 -179.6(3) . . . . ? F11 C43 C44 C45 -179.9(3) . . . . ? C42 C43 C44 C45 -0.1(5) . . . . ? F12 C44 C45 F13 -0.3(5) . . . . ? C43 C44 C45 F13 -179.8(3) . . . . ? F12 C44 C45 C46 -179.5(3) . . . . ? C43 C44 C45 C46 1.0(5) . . . . ? F13 C45 C46 F14 -0.3(4) . . . . ? C44 C45 C46 F14 178.9(3) . . . . ? F13 C45 C46 C41 -180.0(3) . . . . ? C44 C45 C46 C41 -0.8(5) . . . . ? C42 C41 C46 F14 180.0(3) . . . . ? B1 C41 C46 F14 -6.1(4) . . . . ? C42 C41 C46 C45 -0.3(5) . . . . ? B1 C41 C46 C45 173.6(3) . . . . ? C52 C47 C48 C49 -0.2(6) . . . . ? C47 C48 C49 C50 -0.5(7) . . . . ? C48 C49 C50 C51 1.0(6) . . . . ? C49 C50 C51 C52 -0.9(6) . . . . ? C50 C51 C52 C47 0.2(6) . . . . ? C48 C47 C52 C51 0.3(6) . . . . ? C54 C53 C55 C54 -0.9(9) 2_757 . . . ? C53 C54 C55 C53 0.9(8) 2_757 . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.843 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.108 data_5_toluene _database_code_depnum_ccdc_archive 'CCDC 894367' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H66 Mo P6 Si2 , C7 H8' _chemical_formula_sum 'C67 H74 Mo P6 Si2' _chemical_formula_weight 1217.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mo Mo -1.6832 0.6857 '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 2/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' '-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 27.1407(12) _cell_length_b 12.4561(5) _cell_length_c 18.9658(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.0300(10) _cell_angle_gamma 90.00 _cell_volume 6270.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12140 _cell_measurement_theta_min 3.6135 _cell_measurement_theta_max 28.298 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7466 _exptl_absorpt_correction_T_max 0.9769 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33177 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 28.40 _reflns_number_total 7806 _reflns_number_gt 6365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+7.8915P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7806 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Mo1 Mo 0.5000 0.190529(15) 0.2500 0.01025(5) Uani 1 2 d S . . P1 P 0.585062(16) 0.19651(3) 0.25105(2) 0.01552(9) Uani 1 1 d . . . C1 C 0.64158(7) 0.20048(15) 0.24970(11) 0.0266(4) Uani 1 1 d . . . Si1 Si 0.708345(19) 0.20563(5) 0.24746(3) 0.03118(13) Uani 1 1 d . . . C2 C 0.71572(10) 0.2220(4) 0.15273(14) 0.0862(13) Uani 1 1 d . . . H2A H 0.7038 0.1572 0.1252 0.129 Uiso 1 1 calc R . . H2B H 0.7513 0.2336 0.1521 0.129 Uiso 1 1 calc R . . H2C H 0.6960 0.2840 0.1310 0.129 Uiso 1 1 calc R . . C3 C 0.73940(9) 0.0794(2) 0.28644(18) 0.0606(8) Uani 1 1 d . . . H3A H 0.7339 0.0698 0.3355 0.091 Uiso 1 1 calc R . . H3B H 0.7756 0.0837 0.2878 0.091 Uiso 1 1 calc R . . H3C H 0.7250 0.0183 0.2565 0.091 Uiso 1 1 calc R . . C4 C 0.73883(8) 0.31995(18) 0.30193(13) 0.0374(5) Uani 1 1 d . . . H4A H 0.7218 0.3868 0.2836 0.056 Uiso 1 1 calc R . . H4B H 0.7744 0.3238 0.2987 0.056 Uiso 1 1 calc R . . H4C H 0.7365 0.3098 0.3524 0.056 Uiso 1 1 calc R . . P2 P 0.487733(15) 0.06103(3) 0.14946(2) 0.01273(9) Uani 1 1 d . . . P3 P 0.484975(15) 0.31804(3) 0.14838(2) 0.01271(9) Uani 1 1 d . . . C5 C 0.53578(6) -0.04113(13) 0.14292(8) 0.0155(3) Uani 1 1 d . . . C6 C 0.58244(6) -0.01122(14) 0.12938(9) 0.0176(3) Uani 1 1 d . . . H6 H 0.5889 0.0621 0.1211 0.021 Uiso 1 1 calc R . . C7 C 0.61953(7) -0.08758(15) 0.12791(9) 0.0233(4) Uani 1 1 d . . . H7 H 0.6511 -0.0661 0.1185 0.028 Uiso 1 1 calc R . . C8 C 0.61078(7) -0.19463(15) 0.14005(11) 0.0270(4) Uani 1 1 d . . . H8 H 0.6361 -0.2467 0.1387 0.032 Uiso 1 1 calc R . . C9 C 0.56498(7) -0.22540(15) 0.15418(11) 0.0276(4) Uani 1 1 d . . . H9 H 0.5588 -0.2988 0.1628 0.033 Uiso 1 1 calc R . . C10 C 0.52781(7) -0.14900(15) 0.15585(10) 0.0223(4) Uani 1 1 d . . . H10 H 0.4965 -0.1709 0.1660 0.027 Uiso 1 1 calc R . . C11 C 0.43058(6) -0.02224(13) 0.12269(9) 0.0160(3) Uani 1 1 d . . . C12 C 0.39932(6) -0.04417(14) 0.17058(9) 0.0199(3) Uani 1 1 d . . . H12 H 0.4074 -0.0159 0.2181 0.024 Uiso 1 1 calc R . . C13 C 0.35641(7) -0.10700(15) 0.14952(10) 0.0259(4) Uani 1 1 d . . . H13 H 0.3351 -0.1203 0.1824 0.031 Uiso 1 1 calc R . . C14 C 0.34466(7) -0.15013(16) 0.08106(11) 0.0275(4) Uani 1 1 d . . . H14 H 0.3149 -0.1916 0.0665 0.033 Uiso 1 1 calc R . . C15 C 0.37635(7) -0.13277(15) 0.03367(10) 0.0260(4) Uani 1 1 d . . . H15 H 0.3690 -0.1644 -0.0129 0.031 Uiso 1 1 calc R . . C16 C 0.41869(7) -0.06934(15) 0.05435(9) 0.0219(4) Uani 1 1 d . . . H16 H 0.4402 -0.0575 0.0214 0.026 Uiso 1 1 calc R . . C17 C 0.48606(6) 0.13885(13) 0.06534(8) 0.0164(3) Uani 1 1 d . . . H17A H 0.5207 0.1577 0.0611 0.020 Uiso 1 1 calc R . . H17B H 0.4706 0.0951 0.0229 0.020 Uiso 1 1 calc R . . C18 C 0.45528(6) 0.24090(13) 0.06771(8) 0.0160(3) Uani 1 1 d . . . H18A H 0.4202 0.2223 0.0700 0.019 Uiso 1 1 calc R . . H18B H 0.4546 0.2842 0.0237 0.019 Uiso 1 1 calc R . . C19 C 0.44126(6) 0.43147(13) 0.14564(8) 0.0151(3) Uani 1 1 d . . . C20 C 0.38942(6) 0.41326(14) 0.13177(9) 0.0188(3) Uani 1 1 d . . . H20 H 0.3768 0.3431 0.1192 0.023 Uiso 1 1 calc R . . C21 C 0.35595(7) 0.49597(15) 0.13603(10) 0.0239(4) Uani 1 1 d . . . H21 H 0.3207 0.4826 0.1253 0.029 Uiso 1 1 calc R . . C22 C 0.37386(7) 0.59797(15) 0.15586(11) 0.0270(4) Uani 1 1 d . . . H22 H 0.3510 0.6542 0.1602 0.032 Uiso 1 1 calc R . . C23 C 0.42499(7) 0.61762(15) 0.16937(10) 0.0259(4) Uani 1 1 d . . . H23 H 0.4373 0.6877 0.1826 0.031 Uiso 1 1 calc R . . C24 C 0.45848(7) 0.53535(14) 0.16377(9) 0.0203(3) Uani 1 1 d . . . H24 H 0.4936 0.5500 0.1724 0.024 Uiso 1 1 calc R . . C25 C 0.53841(6) 0.38335(13) 0.11959(9) 0.0160(3) Uani 1 1 d . . . C26 C 0.54477(7) 0.38507(16) 0.04842(9) 0.0245(4) Uani 1 1 d . . . H26 H 0.5203 0.3521 0.0116 0.029 Uiso 1 1 calc R . . C27 C 0.58647(8) 0.43450(18) 0.03084(11) 0.0333(5) Uani 1 1 d . . . H27 H 0.5907 0.4336 -0.0176 0.040 Uiso 1 1 calc R . . C28 C 0.62176(8) 0.48497(17) 0.08343(11) 0.0329(5) Uani 1 1 d . . . H28 H 0.6500 0.5195 0.0711 0.039 Uiso 1 1 calc R . . C29 C 0.61578(7) 0.48499(16) 0.15427(11) 0.0274(4) Uani 1 1 d . . . H29 H 0.6397 0.5203 0.1905 0.033 Uiso 1 1 calc R . . C30 C 0.57468(6) 0.43331(14) 0.17214(9) 0.0203(3) Uani 1 1 d . . . H30 H 0.5713 0.4320 0.2210 0.024 Uiso 1 1 calc R . . C31 C 0.77521(15) 0.2896(3) 0.51162(19) 0.0255(8) Uani 0.50 1 d P . . C32 C 0.7266(5) 0.3225(15) 0.5144(10) 0.023(2) Uani 0.50 1 d P . . H32 H 0.7196 0.3953 0.5234 0.028 Uiso 0.50 1 calc PR . . C33 C 0.68780(16) 0.2437(4) 0.5033(2) 0.0366(10) Uani 0.50 1 d P . . H33 H 0.6546 0.2634 0.5069 0.044 Uiso 0.50 1 calc PR . . C34 C 0.6978(4) 0.1396(13) 0.4875(7) 0.058(3) Uani 0.50 1 d P . . H34 H 0.6713 0.0882 0.4793 0.069 Uiso 0.50 1 calc PR . . C35 C 0.7454(2) 0.1090(4) 0.4834(3) 0.0435(11) Uani 0.50 1 d P . . H35 H 0.7524 0.0367 0.4730 0.052 Uiso 0.50 1 calc PR . . C36 C 0.7850(6) 0.1889(15) 0.4951(10) 0.029(3) Uani 0.50 1 d P . . H36 H 0.8182 0.1694 0.4911 0.035 Uiso 0.50 1 calc PR . . C37 C 0.8158(4) 0.3690(9) 0.5256(6) 0.0330(18) Uani 0.50 1 d P . . H37A H 0.8318 0.3680 0.5770 0.049 Uiso 0.50 1 calc PR . . H37B H 0.8019 0.4405 0.5124 0.049 Uiso 0.50 1 calc PR . . H37C H 0.8408 0.3516 0.4969 0.049 Uiso 0.50 1 calc PR . . 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 Mo1 0.00968(9) 0.01131(9) 0.01001(9) 0.000 0.00259(6) 0.000 P1 0.01305(19) 0.0172(2) 0.0165(2) -0.00154(17) 0.00350(15) -0.00031(16) C1 0.0216(9) 0.0270(10) 0.0317(10) -0.0042(8) 0.0069(8) -0.0007(8) Si1 0.0129(2) 0.0485(4) 0.0328(3) -0.0088(3) 0.0064(2) -0.0021(2) C2 0.0318(14) 0.194(4) 0.0365(14) -0.019(2) 0.0156(11) -0.016(2) C3 0.0258(12) 0.0486(15) 0.104(2) -0.0243(16) 0.0057(13) 0.0112(11) C4 0.0222(10) 0.0391(12) 0.0490(13) 0.0026(10) 0.0027(9) -0.0078(9) P2 0.01360(19) 0.01301(19) 0.01178(18) -0.00085(15) 0.00311(15) -0.00005(15) P3 0.01274(19) 0.01283(19) 0.01247(19) 0.00096(15) 0.00243(15) -0.00031(15) C5 0.0181(8) 0.0158(8) 0.0126(7) -0.0018(6) 0.0034(6) 0.0022(6) C6 0.0192(8) 0.0183(8) 0.0154(7) -0.0013(6) 0.0038(6) -0.0002(6) C7 0.0181(8) 0.0297(10) 0.0230(9) -0.0008(8) 0.0063(7) 0.0034(7) C8 0.0241(9) 0.0253(9) 0.0312(10) -0.0006(8) 0.0052(8) 0.0105(8) C9 0.0281(10) 0.0170(8) 0.0373(11) 0.0041(8) 0.0057(8) 0.0040(7) C10 0.0196(9) 0.0196(8) 0.0282(9) 0.0024(7) 0.0058(7) 0.0014(7) C11 0.0155(8) 0.0134(7) 0.0181(8) -0.0017(6) 0.0015(6) -0.0005(6) C12 0.0213(8) 0.0198(8) 0.0187(8) -0.0023(7) 0.0045(7) -0.0031(7) C13 0.0226(9) 0.0258(10) 0.0304(10) 0.0001(8) 0.0081(8) -0.0062(7) C14 0.0218(9) 0.0241(9) 0.0325(10) 0.0006(8) -0.0037(8) -0.0086(8) C15 0.0296(10) 0.0236(9) 0.0217(9) -0.0048(8) -0.0021(7) -0.0046(8) C16 0.0230(9) 0.0233(9) 0.0194(8) -0.0042(7) 0.0044(7) -0.0026(7) C17 0.0196(8) 0.0170(8) 0.0131(7) -0.0010(6) 0.0046(6) 0.0008(6) C18 0.0176(8) 0.0159(8) 0.0138(7) 0.0005(6) 0.0014(6) -0.0003(6) C19 0.0166(8) 0.0142(7) 0.0141(7) 0.0027(6) 0.0029(6) 0.0028(6) C20 0.0190(8) 0.0161(8) 0.0208(8) 0.0017(7) 0.0028(6) -0.0008(7) C21 0.0181(8) 0.0240(9) 0.0299(9) 0.0036(8) 0.0057(7) 0.0041(7) C22 0.0300(10) 0.0191(9) 0.0341(10) 0.0044(8) 0.0117(8) 0.0083(8) C23 0.0328(10) 0.0146(8) 0.0315(10) -0.0008(7) 0.0096(8) 0.0004(7) C24 0.0222(9) 0.0169(8) 0.0219(8) 0.0005(7) 0.0049(7) -0.0018(7) C25 0.0158(8) 0.0155(8) 0.0173(8) 0.0040(6) 0.0049(6) -0.0004(6) C26 0.0244(9) 0.0314(10) 0.0177(8) 0.0060(8) 0.0045(7) -0.0016(8) C27 0.0325(11) 0.0473(13) 0.0230(9) 0.0115(9) 0.0121(8) -0.0050(9) C28 0.0265(10) 0.0393(12) 0.0354(11) 0.0117(9) 0.0125(8) -0.0086(9) C29 0.0221(9) 0.0303(10) 0.0297(10) 0.0037(8) 0.0053(8) -0.0088(8) C30 0.0190(8) 0.0221(9) 0.0205(8) 0.0031(7) 0.0056(6) -0.0029(7) C31 0.027(2) 0.030(2) 0.0186(17) -0.0008(15) 0.0023(15) -0.0019(17) C32 0.020(6) 0.023(4) 0.025(4) -0.005(3) 0.000(4) -0.002(4) C33 0.023(2) 0.058(3) 0.026(2) -0.003(2) -0.0024(16) -0.003(2) C34 0.059(7) 0.072(6) 0.038(4) -0.002(4) 0.002(4) -0.024(5) C35 0.054(3) 0.034(3) 0.041(3) -0.007(2) 0.006(2) 0.000(2) C36 0.025(6) 0.034(5) 0.028(5) -0.006(3) 0.004(4) -0.004(5) C37 0.032(4) 0.031(3) 0.039(5) -0.002(3) 0.015(4) -0.005(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 Mo1 P1 2.3057(4) 2_655 ? Mo1 P1 2.3058(4) . ? Mo1 P3 2.4649(4) . ? Mo1 P3 2.4650(4) 2_655 ? Mo1 P2 2.4665(4) 2_655 ? Mo1 P2 2.4666(4) . ? P1 C1 1.5404(19) . ? C1 Si1 1.8224(19) . ? Si1 C4 1.850(2) . ? Si1 C2 1.860(3) . ? Si1 C3 1.863(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P2 C5 1.8445(16) . ? P2 C11 1.8470(17) . ? P2 C17 1.8591(16) . ? P3 C19 1.8387(16) . ? P3 C25 1.8420(16) . ? P3 C18 1.8437(16) . ? C5 C10 1.391(2) . ? C5 C6 1.394(2) . ? C6 C7 1.389(2) . ? C6 H6 0.9500 . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.393(2) . ? C11 C16 1.398(2) . ? C12 C13 1.391(2) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.384(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.527(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.394(2) . ? C19 C20 1.395(2) . ? C20 C21 1.387(2) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.393(2) . ? C25 C26 1.396(2) . ? C26 C27 1.388(3) . ? C26 H26 0.9500 . ? C27 C28 1.382(3) . ? C27 H27 0.9500 . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 C30 1.390(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.334(19) . ? C31 C32 1.392(16) . ? C31 C37 1.462(10) . ? C32 C33 1.423(14) . ? C32 H32 0.9500 . ? C33 C34 1.370(16) . ? C33 H33 0.9500 . ? C34 C35 1.365(14) . ? C34 H34 0.9500 . ? C35 C36 1.447(15) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 Mo1 P1 176.30(2) 2_655 . ? P1 Mo1 P3 88.294(14) 2_655 . ? P1 Mo1 P3 89.320(14) . . ? P1 Mo1 P3 89.317(14) 2_655 2_655 ? P1 Mo1 P3 88.296(14) . 2_655 ? P3 Mo1 P3 99.77(2) . 2_655 ? P1 Mo1 P2 90.081(14) 2_655 2_655 ? P1 Mo1 P2 92.341(14) . 2_655 ? P3 Mo1 P2 178.202(14) . 2_655 ? P3 Mo1 P2 80.980(14) 2_655 2_655 ? P1 Mo1 P2 92.343(14) 2_655 . ? P1 Mo1 P2 90.080(14) . . ? P3 Mo1 P2 80.980(13) . . ? P3 Mo1 P2 178.203(14) 2_655 . ? P2 Mo1 P2 98.32(2) 2_655 . ? C1 P1 Mo1 178.58(8) . . ? P1 C1 Si1 179.59(15) . . ? C1 Si1 C4 110.19(9) . . ? C1 Si1 C2 109.52(11) . . ? C4 Si1 C2 109.22(15) . . ? C1 Si1 C3 109.33(11) . . ? C4 Si1 C3 108.38(12) . . ? C2 Si1 C3 110.20(18) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 P2 C11 99.15(7) . . ? C5 P2 C17 101.14(7) . . ? C11 P2 C17 100.84(7) . . ? C5 P2 Mo1 121.31(5) . . ? C11 P2 Mo1 123.37(5) . . ? C17 P2 Mo1 107.32(5) . . ? C19 P3 C25 101.27(7) . . ? C19 P3 C18 102.07(7) . . ? C25 P3 C18 102.66(7) . . ? C19 P3 Mo1 121.19(5) . . ? C25 P3 Mo1 120.28(5) . . ? C18 P3 Mo1 106.59(5) . . ? C10 C5 C6 118.11(15) . . ? C10 C5 P2 121.11(13) . . ? C6 C5 P2 120.66(13) . . ? C7 C6 C5 120.69(16) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.46(17) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 119.57(17) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.08(18) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C5 C10 C9 121.09(17) . . ? C5 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C16 117.91(15) . . ? C12 C11 P2 121.44(13) . . ? C16 C11 P2 120.59(13) . . ? C13 C12 C11 120.69(16) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.32(17) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.81(17) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.82(17) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 121.37(16) . . ? C15 C16 H16 119.3 . . ? C11 C16 H16 119.3 . . ? C18 C17 P2 108.94(10) . . ? C18 C17 H17A 109.9 . . ? P2 C17 H17A 109.9 . . ? C18 C17 H17B 109.9 . . ? P2 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 P3 108.13(11) . . ? C17 C18 H18A 110.1 . . ? P3 C18 H18A 110.1 . . ? C17 C18 H18B 110.1 . . ? P3 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C24 C19 C20 118.06(15) . . ? C24 C19 P3 121.68(12) . . ? C20 C19 P3 119.99(13) . . ? C21 C20 C19 121.03(16) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 120.02(17) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.74(17) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.27(17) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.85(16) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C30 C25 C26 118.26(15) . . ? C30 C25 P3 117.89(12) . . ? C26 C25 P3 123.85(13) . . ? C27 C26 C25 120.68(17) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.37(18) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.73(17) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 119.89(18) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 121.05(16) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C36 C31 C32 121.5(11) . . ? C36 C31 C37 119.9(8) . . ? C32 C31 C37 118.5(8) . . ? C31 C32 C33 118.0(13) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? C34 C33 C32 120.7(9) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 120.6(10) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 118.8(10) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C31 C36 C35 120.3(13) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 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 Mo1 P1 C1 -90(3) 2_655 . . . ? P3 Mo1 P1 C1 -41(3) . . . . ? P3 Mo1 P1 C1 -140(3) 2_655 . . . ? P2 Mo1 P1 C1 139(3) 2_655 . . . ? P2 Mo1 P1 C1 40(3) . . . . ? Mo1 P1 C1 Si1 26(29) . . . . ? P1 C1 Si1 C4 100(27) . . . . ? P1 C1 Si1 C2 -20(27) . . . . ? P1 C1 Si1 C3 -141(100) . . . . ? P1 Mo1 P2 C5 -147.63(6) 2_655 . . . ? P1 Mo1 P2 C5 35.17(6) . . . . ? P3 Mo1 P2 C5 124.47(6) . . . . ? P3 Mo1 P2 C5 9.8(5) 2_655 . . . ? P2 Mo1 P2 C5 -57.21(6) 2_655 . . . ? P1 Mo1 P2 C11 -19.06(7) 2_655 . . . ? P1 Mo1 P2 C11 163.74(6) . . . . ? P3 Mo1 P2 C11 -106.96(7) . . . . ? P3 Mo1 P2 C11 138.4(5) 2_655 . . . ? P2 Mo1 P2 C11 71.36(6) 2_655 . . . ? P1 Mo1 P2 C17 97.11(6) 2_655 . . . ? P1 Mo1 P2 C17 -80.08(6) . . . . ? P3 Mo1 P2 C17 9.22(6) . . . . ? P3 Mo1 P2 C17 -105.4(5) 2_655 . . . ? P2 Mo1 P2 C17 -172.46(6) 2_655 . . . ? P1 Mo1 P3 C19 40.66(6) 2_655 . . . ? P1 Mo1 P3 C19 -136.50(6) . . . . ? P3 Mo1 P3 C19 -48.35(6) 2_655 . . . ? P2 Mo1 P3 C19 66.0(5) 2_655 . . . ? P2 Mo1 P3 C19 133.31(6) . . . . ? P1 Mo1 P3 C25 168.83(6) 2_655 . . . ? P1 Mo1 P3 C25 -8.34(6) . . . . ? P3 Mo1 P3 C25 79.82(6) 2_655 . . . ? P2 Mo1 P3 C25 -165.8(5) 2_655 . . . ? P2 Mo1 P3 C25 -98.52(6) . . . . ? P1 Mo1 P3 C18 -75.15(6) 2_655 . . . ? P1 Mo1 P3 C18 107.68(6) . . . . ? P3 Mo1 P3 C18 -164.16(6) 2_655 . . . ? P2 Mo1 P3 C18 -49.8(5) 2_655 . . . ? P2 Mo1 P3 C18 17.49(6) . . . . ? C11 P2 C5 C10 -30.45(16) . . . . ? C17 P2 C5 C10 -133.50(14) . . . . ? Mo1 P2 C5 C10 108.15(14) . . . . ? C11 P2 C5 C6 153.70(13) . . . . ? C17 P2 C5 C6 50.64(15) . . . . ? Mo1 P2 C5 C6 -67.71(14) . . . . ? C10 C5 C6 C7 0.9(2) . . . . ? P2 C5 C6 C7 176.86(13) . . . . ? C5 C6 C7 C8 -0.2(3) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C7 C8 C9 C10 0.3(3) . . . . ? C6 C5 C10 C9 -1.0(3) . . . . ? P2 C5 C10 C9 -177.00(14) . . . . ? C8 C9 C10 C5 0.5(3) . . . . ? C5 P2 C11 C12 115.35(14) . . . . ? C17 P2 C11 C12 -141.34(14) . . . . ? Mo1 P2 C11 C12 -22.07(17) . . . . ? C5 P2 C11 C16 -61.69(15) . . . . ? C17 P2 C11 C16 41.61(15) . . . . ? Mo1 P2 C11 C16 160.88(12) . . . . ? C16 C11 C12 C13 -2.9(3) . . . . ? P2 C11 C12 C13 179.97(14) . . . . ? C11 C12 C13 C14 1.1(3) . . . . ? C12 C13 C14 C15 1.5(3) . . . . ? C13 C14 C15 C16 -2.2(3) . . . . ? C14 C15 C16 C11 0.3(3) . . . . ? C12 C11 C16 C15 2.2(3) . . . . ? P2 C11 C16 C15 179.34(14) . . . . ? C5 P2 C17 C18 -169.45(11) . . . . ? C11 P2 C17 C18 88.85(12) . . . . ? Mo1 P2 C17 C18 -41.41(12) . . . . ? P2 C17 C18 P3 58.51(13) . . . . ? C19 P3 C18 C17 -176.45(11) . . . . ? C25 P3 C18 C17 78.90(12) . . . . ? Mo1 P3 C18 C17 -48.41(11) . . . . ? C25 P3 C19 C24 -35.02(15) . . . . ? C18 P3 C19 C24 -140.75(14) . . . . ? Mo1 P3 C19 C24 101.16(13) . . . . ? C25 P3 C19 C20 151.10(13) . . . . ? C18 P3 C19 C20 45.37(14) . . . . ? Mo1 P3 C19 C20 -72.71(14) . . . . ? C24 C19 C20 C21 -0.1(2) . . . . ? P3 C19 C20 C21 173.95(13) . . . . ? C19 C20 C21 C22 -1.5(3) . . . . ? C20 C21 C22 C23 1.8(3) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C22 C23 C24 C19 -1.0(3) . . . . ? C20 C19 C24 C23 1.4(2) . . . . ? P3 C19 C24 C23 -172.60(14) . . . . ? C19 P3 C25 C30 86.11(14) . . . . ? C18 P3 C25 C30 -168.62(13) . . . . ? Mo1 P3 C25 C30 -50.59(15) . . . . ? C19 P3 C25 C26 -94.31(16) . . . . ? C18 P3 C25 C26 10.96(17) . . . . ? Mo1 P3 C25 C26 128.99(14) . . . . ? C30 C25 C26 C27 0.6(3) . . . . ? P3 C25 C26 C27 -178.99(15) . . . . ? C25 C26 C27 C28 -1.5(3) . . . . ? C26 C27 C28 C29 0.8(3) . . . . ? C27 C28 C29 C30 0.7(3) . . . . ? C28 C29 C30 C25 -1.6(3) . . . . ? C26 C25 C30 C29 1.0(3) . . . . ? P3 C25 C30 C29 -179.43(14) . . . . ? C36 C31 C32 C33 4(3) . . . . ? C37 C31 C32 C33 -177.7(10) . . . . ? C31 C32 C33 C34 -2.6(19) . . . . ? C32 C33 C34 C35 1.2(17) . . . . ? C33 C34 C35 C36 -0.8(17) . . . . ? C32 C31 C36 C35 -3(3) . . . . ? C37 C31 C36 C35 178.1(11) . . . . ? C34 C35 C36 C31 2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.506 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.062 data_5_DCM _database_code_depnum_ccdc_archive 'CCDC 894368' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H66 Mo P6 Si2, 2(C H2 Cl2)' _chemical_formula_sum 'C62 H70 Cl4 Mo P6 Si2' _chemical_formula_weight 1294.92 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P bcn' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 26.479(4) _cell_length_b 12.5536(18) _cell_length_c 19.030(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6325.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 31397 _cell_measurement_theta_min 3.0175 _cell_measurement_theta_max 26.368 _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.96941 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 193570 _diffrn_reflns_av_R_equivalents 0.1178 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7921 _reflns_number_gt 6134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+57.6259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7921 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.2232 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _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 Mo1 Mo 0.5000 0.19949(5) 0.2500 0.01510(17) Uani 1 2 d S . . P1 P 0.41412(6) 0.20580(12) 0.22781(8) 0.0220(3) Uani 1 1 d . . . C1 C 0.3574(3) 0.2108(6) 0.2090(5) 0.0431(18) Uani 1 1 d . A . Si1 Si 0.29222(8) 0.2200(2) 0.17954(13) 0.0470(6) Uani 1 1 d . . . C2 C 0.2671(6) 0.3574(15) 0.1907(19) 0.254(19) Uani 1 1 d . A 1 H2A H 0.2369 0.3553 0.2204 0.381 Uiso 1 1 calc R A 1 H2B H 0.2585 0.3870 0.1446 0.381 Uiso 1 1 calc R A 1 H2C H 0.2929 0.4021 0.2130 0.381 Uiso 1 1 calc R A 1 C3 C 0.2524(5) 0.145(2) 0.2334(10) 0.217(15) Uani 1 1 d . A 1 H3A H 0.2184 0.1760 0.2323 0.325 Uiso 1 1 calc R A 1 H3B H 0.2652 0.1465 0.2817 0.325 Uiso 1 1 calc R A 1 H3C H 0.2512 0.0717 0.2164 0.325 Uiso 1 1 calc R A 1 C4 C 0.2858(6) 0.176(2) 0.0913(7) 0.208(15) Uani 1 1 d . A 2 H4A H 0.2584 0.1241 0.0882 0.312 Uiso 1 1 calc R A 2 H4B H 0.3175 0.1434 0.0758 0.312 Uiso 1 1 calc R A 2 H4C H 0.2781 0.2374 0.0611 0.312 Uiso 1 1 calc R A 2 P2 P 0.51298(5) 0.32670(11) 0.15249(8) 0.0181(3) Uani 1 1 d . . . P3 P 0.51073(5) 0.07130(11) 0.15250(7) 0.0188(3) Uani 1 1 d . . . C5 C 0.5563(2) 0.4395(4) 0.1623(3) 0.0222(11) Uani 1 1 d . . . C6 C 0.6081(2) 0.4209(5) 0.1644(3) 0.0262(13) Uani 1 1 d . . . H6 H 0.6205 0.3509 0.1569 0.031 Uiso 1 1 calc R . . C7 C 0.6418(3) 0.5034(6) 0.1774(4) 0.0371(16) Uani 1 1 d . . . H7 H 0.6771 0.4896 0.1784 0.044 Uiso 1 1 calc R . . C8 C 0.6240(3) 0.6057(6) 0.1889(4) 0.0418(18) Uani 1 1 d . . . H8 H 0.6469 0.6618 0.1991 0.050 Uiso 1 1 calc R . . C9 C 0.5722(3) 0.6261(6) 0.1855(4) 0.0422(18) Uani 1 1 d . . . H9 H 0.5598 0.6964 0.1924 0.051 Uiso 1 1 calc R . . C10 C 0.5393(3) 0.5442(5) 0.1720(4) 0.0303(14) Uani 1 1 d . . . H10 H 0.5042 0.5588 0.1692 0.036 Uiso 1 1 calc R . . C11 C 0.4584(2) 0.3916(5) 0.1094(3) 0.0240(12) Uani 1 1 d . . . C12 C 0.4515(3) 0.3925(6) 0.0370(3) 0.0342(15) Uani 1 1 d . . . H12 H 0.4757 0.3587 0.0075 0.041 Uiso 1 1 calc R . . C13 C 0.4102(3) 0.4418(7) 0.0073(4) 0.0431(19) Uani 1 1 d . . . H13 H 0.4045 0.4370 -0.0419 0.052 Uiso 1 1 calc R . . C14 C 0.3768(3) 0.4987(7) 0.0494(4) 0.0442(19) Uani 1 1 d . . . H14 H 0.3494 0.5362 0.0288 0.053 Uiso 1 1 calc R . . C15 C 0.3835(3) 0.5003(6) 0.1214(4) 0.0385(16) Uani 1 1 d . . . H15 H 0.3607 0.5388 0.1504 0.046 Uiso 1 1 calc R . . C16 C 0.4234(2) 0.4459(5) 0.1512(4) 0.0298(13) Uani 1 1 d . . . H16 H 0.4272 0.4454 0.2009 0.036 Uiso 1 1 calc R . . C17 C 0.5676(2) -0.0113(5) 0.1431(3) 0.0242(12) Uani 1 1 d . . . C18 C 0.5803(3) -0.0571(6) 0.0779(4) 0.0336(15) Uani 1 1 d . . . H18 H 0.5591 -0.0432 0.0387 0.040 Uiso 1 1 calc R . . C19 C 0.6222(3) -0.1215(7) 0.0683(4) 0.0432(18) Uani 1 1 d . . . H19 H 0.6292 -0.1526 0.0239 0.052 Uiso 1 1 calc R . . C20 C 0.6541(3) -0.1393(6) 0.1265(4) 0.0387(17) Uani 1 1 d . . . H20 H 0.6838 -0.1811 0.1213 0.046 Uiso 1 1 calc R . . C21 C 0.6420(3) -0.0952(6) 0.1923(4) 0.0369(16) Uani 1 1 d . . . H21 H 0.6634 -0.1078 0.2315 0.044 Uiso 1 1 calc R . . C22 C 0.5989(3) -0.0335(5) 0.2000(3) 0.0286(13) Uani 1 1 d . . . H22 H 0.5906 -0.0057 0.2450 0.034 Uiso 1 1 calc R . . C23 C 0.4627(2) -0.0314(5) 0.1320(3) 0.0224(11) Uani 1 1 d . . . C24 C 0.4154(2) -0.0012(5) 0.1057(3) 0.0275(13) Uani 1 1 d . . . H24 H 0.4083 0.0717 0.0966 0.033 Uiso 1 1 calc R . . C25 C 0.3787(3) -0.0791(7) 0.0930(4) 0.0409(18) Uani 1 1 d . . . H25 H 0.3469 -0.0587 0.0744 0.049 Uiso 1 1 calc R . . C26 C 0.3881(3) -0.1846(7) 0.1072(5) 0.050(2) Uani 1 1 d . . . H26 H 0.3629 -0.2367 0.0983 0.059 Uiso 1 1 calc R . . C27 C 0.4349(4) -0.2149(6) 0.1347(5) 0.050(2) Uani 1 1 d . . . H27 H 0.4416 -0.2874 0.1454 0.060 Uiso 1 1 calc R . . C28 C 0.4706(3) -0.1388(5) 0.1458(4) 0.0327(14) Uani 1 1 d . . . H28 H 0.5024 -0.1602 0.1640 0.039 Uiso 1 1 calc R . . C29 C 0.5420(2) 0.2516(5) 0.0796(3) 0.0236(12) Uani 1 1 d . . . H29A H 0.5413 0.2947 0.0361 0.028 Uiso 1 1 calc R . . H29B H 0.5776 0.2346 0.0909 0.028 Uiso 1 1 calc R . . C30 C 0.5115(2) 0.1477(4) 0.0691(3) 0.0243(12) Uani 1 1 d . . . H30A H 0.5271 0.1044 0.0315 0.029 Uiso 1 1 calc R . . H30B H 0.4765 0.1651 0.0548 0.029 Uiso 1 1 calc R . . C31 C 0.6909(4) 0.1287(8) 0.0847(6) 0.060(2) Uani 1 1 d . . . H31A H 0.6852 0.1188 0.1357 0.072 Uiso 1 1 calc R . . H31B H 0.6609 0.1012 0.0593 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.69905(12) 0.2653(2) 0.06588(18) 0.0807(9) Uani 1 1 d . . . Cl2 Cl 0.74450(13) 0.0584(3) 0.0587(3) 0.1095(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0163(3) 0.0156(3) 0.0134(3) 0.000 -0.0003(2) 0.000 P1 0.0187(7) 0.0220(7) 0.0253(7) -0.0013(6) -0.0018(5) -0.0007(6) C1 0.027(3) 0.040(4) 0.062(5) -0.004(4) -0.002(3) -0.002(3) Si1 0.0223(9) 0.0692(16) 0.0496(13) -0.0005(12) -0.0041(9) -0.0012(10) C2 0.061(9) 0.102(13) 0.60(6) -0.03(2) -0.131(19) 0.023(9) C3 0.047(7) 0.45(4) 0.148(16) 0.13(2) -0.033(9) -0.087(15) C4 0.119(13) 0.45(4) 0.056(8) -0.090(15) -0.038(8) 0.16(2) P2 0.0191(7) 0.0181(7) 0.0170(7) 0.0018(5) 0.0006(5) -0.0010(5) P3 0.0222(7) 0.0181(7) 0.0160(7) -0.0010(5) 0.0005(5) 0.0005(5) C5 0.029(3) 0.017(3) 0.021(3) 0.004(2) -0.003(2) -0.005(2) C6 0.030(3) 0.020(3) 0.028(3) 0.005(2) 0.002(2) -0.003(2) C7 0.033(3) 0.038(4) 0.040(4) 0.005(3) -0.004(3) -0.012(3) C8 0.038(4) 0.038(4) 0.049(5) 0.004(3) -0.007(3) -0.020(3) C9 0.046(4) 0.025(3) 0.055(5) -0.003(3) -0.011(4) -0.009(3) C10 0.031(3) 0.024(3) 0.036(4) -0.001(3) -0.004(3) -0.005(3) C11 0.024(3) 0.024(3) 0.024(3) 0.007(2) -0.004(2) -0.003(2) C12 0.042(4) 0.041(4) 0.020(3) 0.009(3) -0.003(3) 0.004(3) C13 0.044(4) 0.058(5) 0.027(4) 0.018(3) -0.012(3) 0.007(4) C14 0.039(4) 0.048(4) 0.045(4) 0.021(4) -0.016(3) 0.002(3) C15 0.034(4) 0.039(4) 0.042(4) 0.003(3) -0.002(3) 0.008(3) C16 0.030(3) 0.033(3) 0.026(3) 0.004(3) -0.002(3) 0.002(3) C17 0.030(3) 0.022(3) 0.022(3) -0.004(2) 0.002(2) 0.000(2) C18 0.043(4) 0.034(4) 0.023(3) -0.009(3) 0.005(3) 0.009(3) C19 0.051(4) 0.050(5) 0.029(4) 0.007(3) 0.015(3) 0.012(4) C20 0.031(3) 0.041(4) 0.043(4) 0.008(3) 0.017(3) 0.014(3) C21 0.041(4) 0.030(3) 0.040(4) 0.004(3) -0.002(3) 0.012(3) C22 0.036(3) 0.027(3) 0.023(3) 0.002(2) 0.002(3) 0.005(3) C23 0.024(3) 0.024(3) 0.019(3) -0.004(2) 0.000(2) -0.003(2) C24 0.034(3) 0.027(3) 0.021(3) -0.001(2) -0.005(2) -0.004(3) C25 0.042(4) 0.051(5) 0.029(4) -0.003(3) -0.010(3) -0.013(4) C26 0.056(5) 0.043(5) 0.049(5) -0.006(4) -0.003(4) -0.023(4) C27 0.064(5) 0.020(3) 0.067(6) 0.006(3) 0.003(4) -0.013(3) C28 0.039(4) 0.022(3) 0.037(4) 0.004(3) 0.003(3) -0.002(3) C29 0.030(3) 0.021(3) 0.020(3) 0.001(2) 0.006(2) -0.004(2) C30 0.038(3) 0.017(3) 0.017(3) -0.001(2) 0.000(2) -0.001(2) C31 0.050(5) 0.065(6) 0.066(6) 0.001(5) 0.002(5) -0.004(5) Cl1 0.0812(19) 0.0612(15) 0.100(2) 0.0186(15) 0.0374(17) 0.0167(14) Cl2 0.075(2) 0.080(2) 0.173(4) 0.005(2) 0.022(2) 0.0274(17) _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 Mo1 P1 2.3142(15) 3_655 ? Mo1 P1 2.3143(15) . ? Mo1 P2 2.4721(15) 3_655 ? Mo1 P2 2.4722(15) . ? Mo1 P3 2.4725(15) . ? Mo1 P3 2.4725(15) 3_655 ? P1 C1 1.545(7) . ? C1 Si1 1.818(8) . ? Si1 C3 1.743(16) . ? Si1 C4 1.775(13) . ? Si1 C2 1.860(18) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P2 C5 1.832(6) . ? P2 C29 1.844(6) . ? P2 C11 1.851(6) . ? P3 C17 1.836(6) . ? P3 C23 1.853(6) . ? P3 C30 1.855(6) . ? C5 C6 1.390(9) . ? C5 C10 1.402(9) . ? C6 C7 1.390(9) . ? C6 H6 0.9500 . ? C7 C8 1.387(11) . ? C7 H7 0.9500 . ? C8 C9 1.396(11) . ? C8 H8 0.9500 . ? C9 C10 1.372(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.390(9) . ? C11 C16 1.398(9) . ? C12 C13 1.380(9) . ? C12 H12 0.9500 . ? C13 C14 1.391(12) . ? C13 H13 0.9500 . ? C14 C15 1.382(11) . ? C14 H14 0.9500 . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(9) . ? C17 C18 1.407(8) . ? C18 C19 1.385(10) . ? C18 H18 0.9500 . ? C19 C20 1.412(11) . ? C19 H19 0.9500 . ? C20 C21 1.405(10) . ? C20 H20 0.9500 . ? C21 C22 1.388(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.390(9) . ? C23 C24 1.400(9) . ? C24 C25 1.400(9) . ? C24 H24 0.9500 . ? C25 C26 1.374(12) . ? C25 H25 0.9500 . ? C26 C27 1.397(13) . ? C26 H26 0.9500 . ? C27 C28 1.360(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.547(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 Cl2 1.743(10) . ? C31 Cl1 1.765(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? 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 Mo1 P1 176.08(8) 3_655 . ? P1 Mo1 P2 88.71(5) 3_655 3_655 ? P1 Mo1 P2 88.75(5) . 3_655 ? P1 Mo1 P2 88.75(5) 3_655 . ? P1 Mo1 P2 88.71(5) . . ? P2 Mo1 P2 99.52(7) 3_655 . ? P1 Mo1 P3 92.66(5) 3_655 . ? P1 Mo1 P3 89.90(5) . . ? P2 Mo1 P3 178.59(5) 3_655 . ? P2 Mo1 P3 80.86(5) . . ? P1 Mo1 P3 89.90(5) 3_655 3_655 ? P1 Mo1 P3 92.66(5) . 3_655 ? P2 Mo1 P3 80.86(5) 3_655 3_655 ? P2 Mo1 P3 178.59(5) . 3_655 ? P3 Mo1 P3 98.79(7) . 3_655 ? C1 P1 Mo1 177.1(3) . . ? P1 C1 Si1 175.2(6) . . ? C3 Si1 C4 109.4(12) . . ? C3 Si1 C1 111.0(6) . . ? C4 Si1 C1 111.3(6) . . ? C3 Si1 C2 102.4(14) . . ? C4 Si1 C2 111.1(13) . . ? C1 Si1 C2 111.2(6) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 P2 C29 102.1(3) . . ? C5 P2 C11 101.2(3) . . ? C29 P2 C11 102.5(3) . . ? C5 P2 Mo1 120.66(19) . . ? C29 P2 Mo1 107.0(2) . . ? C11 P2 Mo1 120.5(2) . . ? C17 P3 C23 98.6(3) . . ? C17 P3 C30 101.5(3) . . ? C23 P3 C30 100.8(3) . . ? C17 P3 Mo1 122.3(2) . . ? C23 P3 Mo1 122.14(19) . . ? C30 P3 Mo1 107.86(19) . . ? C6 C5 C10 118.0(6) . . ? C6 C5 P2 119.4(5) . . ? C10 C5 P2 122.5(5) . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 119.9(7) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.8(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 119.6(7) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C5 121.6(7) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? C12 C11 C16 118.3(6) . . ? C12 C11 P2 123.0(5) . . ? C16 C11 P2 118.6(5) . . ? C13 C12 C11 120.9(7) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.9(7) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.0(7) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.9(6) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C22 C17 C18 117.5(6) . . ? C22 C17 P3 121.7(5) . . ? C18 C17 P3 120.8(5) . . ? C19 C18 C17 123.1(7) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C20 117.9(7) . . ? C18 C19 H19 121.0 . . ? C20 C19 H19 121.0 . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.1(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 121.3(6) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? C28 C23 C24 117.7(6) . . ? C28 C23 P3 122.2(5) . . ? C24 C23 P3 120.0(5) . . ? C25 C24 C23 119.5(6) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 120.9(7) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.8(7) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 118.9(7) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C23 123.2(7) . . ? C27 C28 H28 118.4 . . ? C23 C28 H28 118.4 . . ? C30 C29 P2 108.1(4) . . ? C30 C29 H29A 110.1 . . ? P2 C29 H29A 110.1 . . ? C30 C29 H29B 110.1 . . ? P2 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? C29 C30 P3 109.3(4) . . ? C29 C30 H30A 109.8 . . ? P3 C30 H30A 109.8 . . ? C29 C30 H30B 109.8 . . ? P3 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? Cl2 C31 Cl1 109.5(5) . . ? Cl2 C31 H31A 109.8 . . ? Cl1 C31 H31A 109.8 . . ? Cl2 C31 H31B 109.8 . . ? Cl1 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? 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 P1 Mo1 P1 C1 83(6) 3_655 . . . ? P2 Mo1 P1 C1 133(6) 3_655 . . . ? P2 Mo1 P1 C1 33(6) . . . . ? P3 Mo1 P1 C1 -48(6) . . . . ? P3 Mo1 P1 C1 -147(6) 3_655 . . . ? Mo1 P1 C1 Si1 -9(13) . . . . ? P1 C1 Si1 C3 159(7) . . . . ? P1 C1 Si1 C4 36(7) . . . . ? P1 C1 Si1 C2 -88(7) . . . . ? P1 Mo1 P2 C5 -41.0(2) 3_655 . . . ? P1 Mo1 P2 C5 136.1(2) . . . . ? P2 Mo1 P2 C5 47.5(2) 3_655 . . . ? P3 Mo1 P2 C5 -133.8(2) . . . . ? P3 Mo1 P2 C5 -58(2) 3_655 . . . ? P1 Mo1 P2 C29 75.0(2) 3_655 . . . ? P1 Mo1 P2 C29 -108.0(2) . . . . ? P2 Mo1 P2 C29 163.4(2) 3_655 . . . ? P3 Mo1 P2 C29 -17.9(2) . . . . ? P3 Mo1 P2 C29 58(2) 3_655 . . . ? P1 Mo1 P2 C11 -168.7(2) 3_655 . . . ? P1 Mo1 P2 C11 8.3(2) . . . . ? P2 Mo1 P2 C11 -80.2(2) 3_655 . . . ? P3 Mo1 P2 C11 98.4(2) . . . . ? P3 Mo1 P2 C11 174(2) 3_655 . . . ? P1 Mo1 P3 C17 20.0(2) 3_655 . . . ? P1 Mo1 P3 C17 -163.0(2) . . . . ? P2 Mo1 P3 C17 -146(2) 3_655 . . . ? P2 Mo1 P3 C17 108.3(2) . . . . ? P3 Mo1 P3 C17 -70.3(2) 3_655 . . . ? P1 Mo1 P3 C23 147.4(2) 3_655 . . . ? P1 Mo1 P3 C23 -35.6(2) . . . . ? P2 Mo1 P3 C23 -18(2) 3_655 . . . ? P2 Mo1 P3 C23 -124.3(2) . . . . ? P3 Mo1 P3 C23 57.0(2) 3_655 . . . ? P1 Mo1 P3 C30 -96.9(2) 3_655 . . . ? P1 Mo1 P3 C30 80.1(2) . . . . ? P2 Mo1 P3 C30 97(2) 3_655 . . . ? P2 Mo1 P3 C30 -8.6(2) . . . . ? P3 Mo1 P3 C30 172.8(2) 3_655 . . . ? C29 P2 C5 C6 -47.3(6) . . . . ? C11 P2 C5 C6 -152.9(5) . . . . ? Mo1 P2 C5 C6 71.1(5) . . . . ? C29 P2 C5 C10 136.6(6) . . . . ? C11 P2 C5 C10 31.0(6) . . . . ? Mo1 P2 C5 C10 -105.0(5) . . . . ? C10 C5 C6 C7 1.5(10) . . . . ? P2 C5 C6 C7 -174.8(5) . . . . ? C5 C6 C7 C8 0.4(11) . . . . ? C6 C7 C8 C9 -1.8(12) . . . . ? C7 C8 C9 C10 1.2(12) . . . . ? C8 C9 C10 C5 0.7(12) . . . . ? C6 C5 C10 C9 -2.1(10) . . . . ? P2 C5 C10 C9 174.1(6) . . . . ? C5 P2 C11 C12 94.9(6) . . . . ? C29 P2 C11 C12 -10.4(6) . . . . ? Mo1 P2 C11 C12 -129.0(5) . . . . ? C5 P2 C11 C16 -82.4(5) . . . . ? C29 P2 C11 C16 172.3(5) . . . . ? Mo1 P2 C11 C16 53.7(6) . . . . ? C16 C11 C12 C13 -2.8(11) . . . . ? P2 C11 C12 C13 179.9(6) . . . . ? C11 C12 C13 C14 5.1(12) . . . . ? C12 C13 C14 C15 -3.8(12) . . . . ? C13 C14 C15 C16 0.2(12) . . . . ? C14 C15 C16 C11 2.1(11) . . . . ? C12 C11 C16 C15 -0.8(10) . . . . ? P2 C11 C16 C15 176.6(5) . . . . ? C23 P3 C17 C22 -115.0(6) . . . . ? C30 P3 C17 C22 142.1(5) . . . . ? Mo1 P3 C17 C22 22.1(6) . . . . ? C23 P3 C17 C18 63.3(6) . . . . ? C30 P3 C17 C18 -39.7(6) . . . . ? Mo1 P3 C17 C18 -159.7(5) . . . . ? C22 C17 C18 C19 -0.5(11) . . . . ? P3 C17 C18 C19 -178.8(6) . . . . ? C17 C18 C19 C20 -1.6(12) . . . . ? C18 C19 C20 C21 2.1(12) . . . . ? C19 C20 C21 C22 -0.5(12) . . . . ? C20 C21 C22 C17 -1.8(11) . . . . ? C18 C17 C22 C21 2.2(10) . . . . ? P3 C17 C22 C21 -179.5(5) . . . . ? C17 P3 C23 C28 29.0(6) . . . . ? C30 P3 C23 C28 132.6(6) . . . . ? Mo1 P3 C23 C28 -108.2(5) . . . . ? C17 P3 C23 C24 -155.0(5) . . . . ? C30 P3 C23 C24 -51.5(5) . . . . ? Mo1 P3 C23 C24 67.8(5) . . . . ? C28 C23 C24 C25 -1.4(9) . . . . ? P3 C23 C24 C25 -177.5(5) . . . . ? C23 C24 C25 C26 1.2(11) . . . . ? C24 C25 C26 C27 0.1(13) . . . . ? C25 C26 C27 C28 -1.1(13) . . . . ? C26 C27 C28 C23 0.8(13) . . . . ? C24 C23 C28 C27 0.4(11) . . . . ? P3 C23 C28 C27 176.4(6) . . . . ? C5 P2 C29 C30 175.5(4) . . . . ? C11 P2 C29 C30 -79.9(4) . . . . ? Mo1 P2 C29 C30 47.8(4) . . . . ? P2 C29 C30 P3 -57.2(5) . . . . ? C17 P3 C30 C29 -89.7(4) . . . . ? C23 P3 C30 C29 169.2(4) . . . . ? Mo1 P3 C30 C29 40.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.693 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.156 data_6 _database_code_depnum_ccdc_archive 'CCDC 894369' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H19 Mo2 O4 P Si' _chemical_formula_sum 'C18 H19 Mo2 O4 P Si' _chemical_formula_weight 550.27 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' O O 0.0106 0.0060 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3831(3) _cell_length_b 8.4729(2) _cell_length_c 15.5429(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.1520(10) _cell_angle_gamma 90.00 _cell_volume 2025.44(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4933 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81278284 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; 'Data collected at the EPSRC National Crystallography Service, Southhampton' ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22459 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4624 _reflns_number_gt 4412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.0732P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4624 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 1.04296(3) -0.00956(6) 0.72574(3) 0.01667(11) Uani 1 1 d . . . C1 C 1.03795(12) 0.1931(2) 0.71576(12) 0.0152(4) Uani 1 1 d . . . Si1 Si 1.13149(4) 0.32042(7) 0.68817(4) 0.02064(13) Uani 1 1 d . . . C2 C 1.19099(17) 0.2314(4) 0.59608(17) 0.0386(6) Uani 1 1 d . . . H2A H 1.2083 0.1257 0.6106 0.058 Uiso 1 1 calc R . . H2B H 1.2416 0.2935 0.5845 0.058 Uiso 1 1 calc R . . H2C H 1.1536 0.2294 0.5459 0.058 Uiso 1 1 calc R . . C3 C 1.10175(17) 0.5280(3) 0.65977(18) 0.0344(6) Uani 1 1 d . . . H3A H 1.0550 0.5276 0.6179 0.052 Uiso 1 1 calc R . . H3B H 1.1512 0.5805 0.6363 0.052 Uiso 1 1 calc R . . H3C H 1.0837 0.5826 0.7105 0.052 Uiso 1 1 calc R . . C4 C 1.20954(16) 0.3290(3) 0.78171(18) 0.0349(6) Uani 1 1 d . . . H4A H 1.1827 0.3818 0.8289 0.052 Uiso 1 1 calc R . . H4B H 1.2607 0.3859 0.7656 0.052 Uiso 1 1 calc R . . H4C H 1.2254 0.2238 0.7987 0.052 Uiso 1 1 calc R . . Mo1 Mo 0.973869(11) 0.16097(2) 0.839375(10) 0.01464(6) Uani 1 1 d . . . C5 C 0.96692(19) 0.4392(3) 0.85295(17) 0.0376(6) Uani 1 1 d . . . H5 H 0.9932 0.5071 0.8143 0.045 Uiso 1 1 calc R . . C6 C 0.88076(18) 0.3829(3) 0.84705(16) 0.0329(6) Uani 1 1 d . . . H6 H 0.8403 0.4073 0.8039 0.039 Uiso 1 1 calc R . . C7 C 0.86669(15) 0.2829(3) 0.91818(15) 0.0281(5) Uani 1 1 d . . . H7 H 0.8155 0.2291 0.9298 0.034 Uiso 1 1 calc R . . C8 C 0.94404(16) 0.2792(3) 0.96827(14) 0.0292(5) Uani 1 1 d . . . H8 H 0.9527 0.2236 1.0193 0.035 Uiso 1 1 calc R . . C9 C 1.00602(18) 0.3747(3) 0.92732(18) 0.0345(6) Uani 1 1 d . . . H9 H 1.0629 0.3919 0.9464 0.041 Uiso 1 1 calc R . . C10 C 0.92758(13) -0.0520(3) 0.86594(13) 0.0213(4) Uani 1 1 d . . . C11 C 1.08404(15) 0.0811(3) 0.89326(14) 0.0235(4) Uani 1 1 d . . . O1 O 0.90083(11) -0.1742(2) 0.88327(11) 0.0309(4) Uani 1 1 d . . . O2 O 0.75809(10) 0.0864(2) 0.77839(10) 0.0313(4) Uani 1 1 d . . . Mo2 Mo 0.914170(10) 0.121221(19) 0.656183(10) 0.01313(6) Uani 1 1 d . . . C12 C 0.95157(15) 0.2845(3) 0.53902(14) 0.0272(5) Uani 1 1 d . . . H12 H 1.0093 0.3095 0.5285 0.033 Uiso 1 1 calc R . . C13 C 0.89402(18) 0.3731(3) 0.59073(15) 0.0302(5) Uani 1 1 d . . . H13 H 0.9073 0.4661 0.6199 0.036 Uiso 1 1 calc R . . C14 C 0.81364(16) 0.2948(3) 0.58972(15) 0.0298(5) Uani 1 1 d . . . H14 H 0.7640 0.3272 0.6180 0.036 Uiso 1 1 calc R . . C15 C 0.82102(16) 0.1585(3) 0.53848(15) 0.0264(5) Uani 1 1 d . . . H15 H 0.7773 0.0850 0.5275 0.032 Uiso 1 1 calc R . . C16 C 0.90619(16) 0.1529(3) 0.50662(14) 0.0250(5) Uani 1 1 d . . . H16 H 0.9283 0.0758 0.4706 0.030 Uiso 1 1 calc R . . C17 C 0.82211(14) 0.0987(3) 0.74074(14) 0.0215(4) Uani 1 1 d . . . C18 C 0.90701(14) -0.1076(3) 0.64127(14) 0.0217(4) Uani 1 1 d . . . O3 O 0.89914(12) -0.24057(19) 0.62706(11) 0.0328(4) Uani 1 1 d . . . O4 O 1.14601(11) 0.0373(2) 0.92734(11) 0.0358(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0160(2) 0.0156(2) 0.0185(3) -0.00102(19) 0.00262(19) 0.00359(18) C1 0.0131(9) 0.0167(9) 0.0159(9) -0.0003(7) 0.0021(7) -0.0003(7) Si1 0.0176(3) 0.0213(3) 0.0231(3) 0.0017(2) 0.0008(2) -0.0060(2) C2 0.0313(13) 0.0457(16) 0.0395(14) -0.0062(12) 0.0159(11) -0.0130(12) C3 0.0340(13) 0.0248(12) 0.0440(15) 0.0110(11) -0.0063(11) -0.0098(10) C4 0.0215(12) 0.0392(15) 0.0436(15) 0.0091(12) -0.0091(11) -0.0109(10) Mo1 0.01550(10) 0.01498(10) 0.01346(10) -0.00127(6) 0.00094(7) 0.00235(6) C5 0.0597(18) 0.0167(12) 0.0372(14) -0.0074(10) 0.0203(13) 0.0029(11) C6 0.0463(15) 0.0294(13) 0.0228(12) -0.0068(9) -0.0026(10) 0.0239(11) C7 0.0279(12) 0.0308(12) 0.0259(11) -0.0088(10) 0.0064(9) 0.0077(10) C8 0.0364(13) 0.0343(13) 0.0168(10) -0.0089(9) -0.0005(9) 0.0120(10) C9 0.0330(13) 0.0327(13) 0.0378(14) -0.0226(11) 0.0018(11) 0.0002(10) C10 0.0192(10) 0.0254(11) 0.0196(10) 0.0023(9) 0.0021(8) 0.0044(8) C11 0.0261(11) 0.0264(11) 0.0181(10) -0.0005(9) 0.0020(8) 0.0033(9) O1 0.0316(9) 0.0254(9) 0.0358(10) 0.0072(7) 0.0037(7) -0.0050(7) O2 0.0171(8) 0.0505(11) 0.0264(8) -0.0040(8) 0.0059(6) -0.0057(7) Mo2 0.01280(10) 0.01294(10) 0.01369(10) -0.00167(6) 0.00133(7) 0.00018(6) C12 0.0279(12) 0.0313(12) 0.0223(11) 0.0116(9) -0.0015(9) -0.0034(10) C13 0.0509(16) 0.0160(11) 0.0232(12) 0.0034(9) -0.0099(11) 0.0045(10) C14 0.0299(12) 0.0354(13) 0.0241(11) 0.0033(10) -0.0015(9) 0.0193(10) C15 0.0248(11) 0.0306(12) 0.0233(11) 0.0031(9) -0.0091(9) -0.0014(9) C16 0.0348(13) 0.0277(12) 0.0125(10) -0.0004(8) 0.0001(9) 0.0076(9) C17 0.0187(10) 0.0262(11) 0.0196(10) -0.0023(8) -0.0015(8) -0.0017(8) C18 0.0211(11) 0.0217(11) 0.0225(11) -0.0010(8) 0.0025(8) -0.0027(8) O3 0.0421(10) 0.0160(8) 0.0405(10) -0.0064(7) 0.0022(8) -0.0056(7) O4 0.0258(9) 0.0511(12) 0.0302(9) 0.0046(8) -0.0049(7) 0.0123(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 P1 C1 1.725(2) . ? P1 Mo2 2.4971(5) . ? P1 Mo1 2.5323(5) . ? C1 Si1 1.856(2) . ? C1 Mo2 2.1869(19) . ? C1 Mo1 2.1939(19) . ? Si1 C3 1.868(3) . ? Si1 C4 1.868(3) . ? Si1 C2 1.873(3) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? Mo1 C10 1.986(2) . ? Mo1 C11 1.994(2) . ? Mo1 C8 2.294(2) . ? Mo1 C9 2.316(2) . ? Mo1 C7 2.317(2) . ? Mo1 C6 2.368(2) . ? Mo1 C5 2.369(2) . ? Mo1 Mo2 2.9932(2) . ? C5 C9 1.403(4) . ? C5 C6 1.410(4) . ? C5 H5 0.9300 . ? C6 C7 1.413(4) . ? C6 H6 0.9300 . ? C7 C8 1.409(3) . ? C7 H7 0.9300 . ? C8 C9 1.412(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 O1 1.148(3) . ? C11 O4 1.143(3) . ? O2 C17 1.160(3) . ? Mo2 C18 1.955(2) . ? Mo2 C17 1.961(2) . ? Mo2 C15 2.323(2) . ? Mo2 C16 2.341(2) . ? Mo2 C14 2.357(2) . ? Mo2 C12 2.367(2) . ? Mo2 C13 2.382(2) . ? C12 C16 1.404(3) . ? C12 C13 1.421(4) . ? C12 H12 0.9300 . ? C13 C14 1.403(4) . ? C13 H13 0.9300 . ? C14 C15 1.408(3) . ? C14 H14 0.9300 . ? C15 C16 1.411(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 O3 1.154(3) . ? 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 C1 P1 Mo2 59.06(7) . . ? C1 P1 Mo1 58.42(6) . . ? Mo2 P1 Mo1 73.040(15) . . ? P1 C1 Si1 124.46(11) . . ? P1 C1 Mo2 78.35(8) . . ? Si1 C1 Mo2 137.44(11) . . ? P1 C1 Mo1 79.51(8) . . ? Si1 C1 Mo1 129.68(10) . . ? Mo2 C1 Mo1 86.19(7) . . ? C1 Si1 C3 114.50(10) . . ? C1 Si1 C4 109.39(10) . . ? C3 Si1 C4 107.32(12) . . ? C1 Si1 C2 109.61(11) . . ? C3 Si1 C2 108.64(13) . . ? C4 Si1 C2 107.10(13) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 Mo1 C11 84.81(9) . . ? C10 Mo1 C1 117.64(8) . . ? C11 Mo1 C1 90.97(8) . . ? C10 Mo1 C8 97.83(9) . . ? C11 Mo1 C8 87.97(9) . . ? C1 Mo1 C8 144.28(9) . . ? C10 Mo1 C9 131.36(10) . . ? C11 Mo1 C9 81.25(10) . . ? C1 Mo1 C9 109.00(9) . . ? C8 Mo1 C9 35.66(10) . . ? C10 Mo1 C7 91.90(9) . . ? C11 Mo1 C7 122.50(8) . . ? C1 Mo1 C7 138.14(8) . . ? C8 Mo1 C7 35.59(8) . . ? C9 Mo1 C7 59.02(9) . . ? C10 Mo1 C6 119.41(9) . . ? C11 Mo1 C6 139.31(9) . . ? C1 Mo1 C6 103.21(8) . . ? C8 Mo1 C6 58.51(8) . . ? C9 Mo1 C6 58.11(9) . . ? C7 Mo1 C6 35.09(9) . . ? C10 Mo1 C5 150.26(9) . . ? C11 Mo1 C5 109.86(10) . . ? C1 Mo1 C5 88.66(8) . . ? C8 Mo1 C5 58.52(9) . . ? C9 Mo1 C5 34.82(10) . . ? C7 Mo1 C5 58.36(9) . . ? C6 Mo1 C5 34.63(10) . . ? C10 Mo1 P1 77.52(6) . . ? C11 Mo1 P1 74.58(6) . . ? C1 Mo1 P1 42.07(5) . . ? C8 Mo1 P1 162.22(6) . . ? C9 Mo1 P1 140.36(7) . . ? C7 Mo1 P1 159.45(6) . . ? C6 Mo1 P1 138.67(6) . . ? C5 Mo1 P1 130.55(6) . . ? C10 Mo1 Mo2 89.49(6) . . ? C11 Mo1 Mo2 127.11(6) . . ? C1 Mo1 Mo2 46.80(5) . . ? C8 Mo1 Mo2 144.77(6) . . ? C9 Mo1 Mo2 135.00(7) . . ? C7 Mo1 Mo2 110.19(6) . . ? C6 Mo1 Mo2 87.88(6) . . ? C5 Mo1 Mo2 100.55(7) . . ? P1 Mo1 Mo2 52.939(13) . . ? C9 C5 C6 108.0(2) . . ? C9 C5 Mo1 70.53(14) . . ? C6 C5 Mo1 72.64(14) . . ? C9 C5 H5 126.0 . . ? C6 C5 H5 126.0 . . ? Mo1 C5 H5 122.5 . . ? C5 C6 C7 108.1(2) . . ? C5 C6 Mo1 72.74(14) . . ? C7 C6 Mo1 70.47(12) . . ? C5 C6 H6 126.0 . . ? C7 C6 H6 126.0 . . ? Mo1 C6 H6 122.5 . . ? C8 C7 C6 107.7(2) . . ? C8 C7 Mo1 71.35(13) . . ? C6 C7 Mo1 74.44(13) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Mo1 C7 H7 119.9 . . ? C7 C8 C9 108.0(2) . . ? C7 C8 Mo1 73.07(12) . . ? C9 C8 Mo1 73.02(13) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Mo1 C8 H8 119.7 . . ? C5 C9 C8 108.2(2) . . ? C5 C9 Mo1 74.65(14) . . ? C8 C9 Mo1 71.32(13) . . ? C5 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Mo1 C9 H9 119.9 . . ? O1 C10 Mo1 178.42(19) . . ? O4 C11 Mo1 177.19(19) . . ? C18 Mo2 C17 86.74(9) . . ? C18 Mo2 C1 111.88(8) . . ? C17 Mo2 C1 112.20(8) . . ? C18 Mo2 C15 90.53(9) . . ? C17 Mo2 C15 95.67(9) . . ? C1 Mo2 C15 144.46(8) . . ? C18 Mo2 C16 89.68(9) . . ? C17 Mo2 C16 130.75(9) . . ? C1 Mo2 C16 114.60(8) . . ? C15 Mo2 C16 35.22(8) . . ? C18 Mo2 C14 122.12(9) . . ? C17 Mo2 C14 83.00(9) . . ? C1 Mo2 C14 124.74(9) . . ? C15 Mo2 C14 35.02(8) . . ? C16 Mo2 C14 58.16(8) . . ? C18 Mo2 C12 120.15(9) . . ? C17 Mo2 C12 139.69(9) . . ? C1 Mo2 C12 86.56(8) . . ? C15 Mo2 C12 58.01(8) . . ? C16 Mo2 C12 34.68(8) . . ? C14 Mo2 C12 57.70(8) . . ? C18 Mo2 C13 146.22(9) . . ? C17 Mo2 C13 106.51(10) . . ? C1 Mo2 C13 92.07(8) . . ? C15 Mo2 C13 57.90(9) . . ? C16 Mo2 C13 57.94(8) . . ? C14 Mo2 C13 34.44(9) . . ? C12 Mo2 C13 34.83(9) . . ? C18 Mo2 P1 69.74(7) . . ? C17 Mo2 P1 104.12(7) . . ? C1 Mo2 P1 42.59(5) . . ? C15 Mo2 P1 150.80(6) . . ? C16 Mo2 P1 120.41(6) . . ? C14 Mo2 P1 166.99(7) . . ? C12 Mo2 P1 112.92(6) . . ? C13 Mo2 P1 132.68(7) . . ? C18 Mo2 Mo1 103.88(7) . . ? C17 Mo2 Mo1 65.50(6) . . ? C1 Mo2 Mo1 47.00(5) . . ? C15 Mo2 Mo1 155.04(6) . . ? C16 Mo2 Mo1 160.17(6) . . ? C14 Mo2 Mo1 122.19(6) . . ? C12 Mo2 Mo1 126.25(6) . . ? C13 Mo2 Mo1 109.90(6) . . ? P1 Mo2 Mo1 54.021(13) . . ? C16 C12 C13 108.1(2) . . ? C16 C12 Mo2 71.63(13) . . ? C13 C12 Mo2 73.13(13) . . ? C16 C12 H12 125.9 . . ? C13 C12 H12 125.9 . . ? Mo2 C12 H12 121.0 . . ? C14 C13 C12 107.6(2) . . ? C14 C13 Mo2 71.83(13) . . ? C12 C13 Mo2 72.04(13) . . ? C14 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? Mo2 C13 H13 121.7 . . ? C13 C14 C15 108.2(2) . . ? C13 C14 Mo2 73.73(13) . . ? C15 C14 Mo2 71.15(13) . . ? C13 C14 H14 125.9 . . ? C15 C14 H14 125.9 . . ? Mo2 C14 H14 121.0 . . ? C14 C15 C16 108.2(2) . . ? C14 C15 Mo2 73.84(13) . . ? C16 C15 Mo2 73.10(13) . . ? C14 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Mo2 C15 H15 119.0 . . ? C12 C16 C15 107.8(2) . . ? C12 C16 Mo2 73.69(12) . . ? C15 C16 Mo2 71.68(13) . . ? C12 C16 H16 126.1 . . ? C15 C16 H16 126.1 . . ? Mo2 C16 H16 120.3 . . ? O2 C17 Mo2 168.14(19) . . ? O3 C18 Mo2 175.0(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 Mo2 P1 C1 Si1 -140.41(15) . . . . ? Mo1 P1 C1 Si1 131.35(15) . . . . ? Mo1 P1 C1 Mo2 -88.24(5) . . . . ? Mo2 P1 C1 Mo1 88.24(5) . . . . ? P1 C1 Si1 C3 167.95(14) . . . . ? Mo2 C1 Si1 C3 55.29(19) . . . . ? Mo1 C1 Si1 C3 -85.63(16) . . . . ? P1 C1 Si1 C4 -71.56(17) . . . . ? Mo2 C1 Si1 C4 175.77(15) . . . . ? Mo1 C1 Si1 C4 34.86(17) . . . . ? P1 C1 Si1 C2 45.59(18) . . . . ? Mo2 C1 Si1 C2 -67.08(19) . . . . ? Mo1 C1 Si1 C2 152.01(14) . . . . ? P1 C1 Mo1 C10 -19.20(11) . . . . ? Si1 C1 Mo1 C10 -145.66(12) . . . . ? Mo2 C1 Mo1 C10 59.64(10) . . . . ? P1 C1 Mo1 C11 65.45(9) . . . . ? Si1 C1 Mo1 C11 -61.01(14) . . . . ? Mo2 C1 Mo1 C11 144.29(9) . . . . ? P1 C1 Mo1 C8 153.32(11) . . . . ? Si1 C1 Mo1 C8 26.9(2) . . . . ? Mo2 C1 Mo1 C8 -127.84(12) . . . . ? P1 C1 Mo1 C9 146.52(9) . . . . ? Si1 C1 Mo1 C9 20.06(16) . . . . ? Mo2 C1 Mo1 C9 -134.64(8) . . . . ? P1 C1 Mo1 C7 -149.05(10) . . . . ? Si1 C1 Mo1 C7 84.49(17) . . . . ? Mo2 C1 Mo1 C7 -70.21(13) . . . . ? P1 C1 Mo1 C6 -153.02(9) . . . . ? Si1 C1 Mo1 C6 80.52(15) . . . . ? Mo2 C1 Mo1 C6 -74.18(9) . . . . ? P1 C1 Mo1 C5 175.30(10) . . . . ? Si1 C1 Mo1 C5 48.84(14) . . . . ? Mo2 C1 Mo1 C5 -105.86(9) . . . . ? Si1 C1 Mo1 P1 -126.46(16) . . . . ? Mo2 C1 Mo1 P1 78.84(7) . . . . ? P1 C1 Mo1 Mo2 -78.84(7) . . . . ? Si1 C1 Mo1 Mo2 154.70(17) . . . . ? C1 P1 Mo1 C10 162.64(10) . . . . ? Mo2 P1 Mo1 C10 98.96(6) . . . . ? C1 P1 Mo1 C11 -109.37(10) . . . . ? Mo2 P1 Mo1 C11 -173.05(7) . . . . ? Mo2 P1 Mo1 C1 -63.68(8) . . . . ? C1 P1 Mo1 C8 -120.9(2) . . . . ? Mo2 P1 Mo1 C8 175.5(2) . . . . ? C1 P1 Mo1 C9 -54.84(14) . . . . ? Mo2 P1 Mo1 C9 -118.52(12) . . . . ? C1 P1 Mo1 C7 102.2(2) . . . . ? Mo2 P1 Mo1 C7 38.53(18) . . . . ? C1 P1 Mo1 C6 41.98(14) . . . . ? Mo2 P1 Mo1 C6 -21.70(11) . . . . ? C1 P1 Mo1 C5 -6.19(13) . . . . ? Mo2 P1 Mo1 C5 -69.87(10) . . . . ? C1 P1 Mo1 Mo2 63.68(8) . . . . ? C10 Mo1 C5 C9 79.4(3) . . . . ? C11 Mo1 C5 C9 -36.61(18) . . . . ? C1 Mo1 C5 C9 -127.15(16) . . . . ? C8 Mo1 C5 C9 38.00(15) . . . . ? C7 Mo1 C5 C9 80.03(17) . . . . ? C6 Mo1 C5 C9 117.0(2) . . . . ? P1 Mo1 C5 C9 -123.01(14) . . . . ? Mo2 Mo1 C5 C9 -172.66(15) . . . . ? C10 Mo1 C5 C6 -37.6(3) . . . . ? C11 Mo1 C5 C6 -153.59(15) . . . . ? C1 Mo1 C5 C6 115.87(15) . . . . ? C8 Mo1 C5 C6 -78.98(16) . . . . ? C9 Mo1 C5 C6 -117.0(2) . . . . ? C7 Mo1 C5 C6 -36.95(14) . . . . ? P1 Mo1 C5 C6 120.01(13) . . . . ? Mo2 Mo1 C5 C6 70.36(14) . . . . ? C9 C5 C6 C7 -0.1(3) . . . . ? Mo1 C5 C6 C7 61.97(15) . . . . ? C9 C5 C6 Mo1 -62.05(16) . . . . ? C10 Mo1 C6 C5 159.68(15) . . . . ? C11 Mo1 C6 C5 39.9(2) . . . . ? C1 Mo1 C6 C5 -67.52(16) . . . . ? C8 Mo1 C6 C5 79.00(16) . . . . ? C9 Mo1 C6 C5 36.82(15) . . . . ? C7 Mo1 C6 C5 117.1(2) . . . . ? P1 Mo1 C6 C5 -94.93(16) . . . . ? Mo2 Mo1 C6 C5 -112.10(14) . . . . ? C10 Mo1 C6 C7 42.59(18) . . . . ? C11 Mo1 C6 C7 -77.2(2) . . . . ? C1 Mo1 C6 C7 175.39(14) . . . . ? C8 Mo1 C6 C7 -38.08(15) . . . . ? C9 Mo1 C6 C7 -80.26(16) . . . . ? C5 Mo1 C6 C7 -117.1(2) . . . . ? P1 Mo1 C6 C7 147.98(12) . . . . ? Mo2 Mo1 C6 C7 130.81(15) . . . . ? C5 C6 C7 C8 0.6(3) . . . . ? Mo1 C6 C7 C8 64.05(15) . . . . ? C5 C6 C7 Mo1 -63.44(16) . . . . ? C10 Mo1 C7 C8 100.82(16) . . . . ? C11 Mo1 C7 C8 15.76(19) . . . . ? C1 Mo1 C7 C8 -122.06(16) . . . . ? C9 Mo1 C7 C8 -37.87(16) . . . . ? C6 Mo1 C7 C8 -115.3(2) . . . . ? C5 Mo1 C7 C8 -78.87(17) . . . . ? P1 Mo1 C7 C8 159.00(15) . . . . ? Mo2 Mo1 C7 C8 -169.02(14) . . . . ? C10 Mo1 C7 C6 -143.85(16) . . . . ? C11 Mo1 C7 C6 131.09(16) . . . . ? C1 Mo1 C7 C6 -6.7(2) . . . . ? C8 Mo1 C7 C6 115.3(2) . . . . ? C9 Mo1 C7 C6 77.46(17) . . . . ? C5 Mo1 C7 C6 36.46(16) . . . . ? P1 Mo1 C7 C6 -85.7(2) . . . . ? Mo2 Mo1 C7 C6 -53.69(16) . . . . ? C6 C7 C8 C9 -0.9(3) . . . . ? Mo1 C7 C8 C9 65.19(16) . . . . ? C6 C7 C8 Mo1 -66.10(15) . . . . ? C10 Mo1 C8 C7 -82.27(16) . . . . ? C11 Mo1 C8 C7 -166.75(16) . . . . ? C1 Mo1 C8 C7 104.42(18) . . . . ? C9 Mo1 C8 C7 115.5(2) . . . . ? C6 Mo1 C8 C7 37.54(15) . . . . ? C5 Mo1 C8 C7 78.39(17) . . . . ? P1 Mo1 C8 C7 -155.67(18) . . . . ? Mo2 Mo1 C8 C7 18.1(2) . . . . ? C10 Mo1 C8 C9 162.25(16) . . . . ? C11 Mo1 C8 C9 77.77(16) . . . . ? C1 Mo1 C8 C9 -11.1(2) . . . . ? C7 Mo1 C8 C9 -115.5(2) . . . . ? C6 Mo1 C8 C9 -77.94(17) . . . . ? C5 Mo1 C8 C9 -37.09(16) . . . . ? P1 Mo1 C8 C9 88.8(3) . . . . ? Mo2 Mo1 C8 C9 -97.43(17) . . . . ? C6 C5 C9 C8 -0.5(3) . . . . ? Mo1 C5 C9 C8 -63.90(16) . . . . ? C6 C5 C9 Mo1 63.41(16) . . . . ? C7 C8 C9 C5 0.9(3) . . . . ? Mo1 C8 C9 C5 66.09(17) . . . . ? C7 C8 C9 Mo1 -65.22(16) . . . . ? C10 Mo1 C9 C5 -139.49(16) . . . . ? C11 Mo1 C9 C5 145.43(17) . . . . ? C1 Mo1 C9 C5 57.43(17) . . . . ? C8 Mo1 C9 C5 -115.8(2) . . . . ? C7 Mo1 C9 C5 -77.98(17) . . . . ? C6 Mo1 C9 C5 -36.61(16) . . . . ? P1 Mo1 C9 C5 92.83(17) . . . . ? Mo2 Mo1 C9 C5 10.2(2) . . . . ? C10 Mo1 C9 C8 -23.7(2) . . . . ? C11 Mo1 C9 C8 -98.81(16) . . . . ? C1 Mo1 C9 C8 173.20(14) . . . . ? C7 Mo1 C9 C8 37.79(14) . . . . ? C6 Mo1 C9 C8 79.15(16) . . . . ? C5 Mo1 C9 C8 115.8(2) . . . . ? P1 Mo1 C9 C8 -151.40(11) . . . . ? Mo2 Mo1 C9 C8 126.00(13) . . . . ? C11 Mo1 C10 O1 72(7) . . . . ? C1 Mo1 C10 O1 160(7) . . . . ? C8 Mo1 C10 O1 -16(7) . . . . ? C9 Mo1 C10 O1 -2(7) . . . . ? C7 Mo1 C10 O1 -51(7) . . . . ? C6 Mo1 C10 O1 -74(7) . . . . ? C5 Mo1 C10 O1 -50(7) . . . . ? P1 Mo1 C10 O1 147(7) . . . . ? Mo2 Mo1 C10 O1 -161(7) . . . . ? C10 Mo1 C11 O4 -88(4) . . . . ? C1 Mo1 C11 O4 154(4) . . . . ? C8 Mo1 C11 O4 10(4) . . . . ? C9 Mo1 C11 O4 45(4) . . . . ? C7 Mo1 C11 O4 1(4) . . . . ? C6 Mo1 C11 O4 43(5) . . . . ? C5 Mo1 C11 O4 65(4) . . . . ? P1 Mo1 C11 O4 -167(4) . . . . ? Mo2 Mo1 C11 O4 -174(4) . . . . ? P1 C1 Mo2 C18 -8.72(10) . . . . ? Si1 C1 Mo2 C18 120.31(16) . . . . ? Mo1 C1 Mo2 C18 -88.79(9) . . . . ? P1 C1 Mo2 C17 86.88(9) . . . . ? Si1 C1 Mo2 C17 -144.09(15) . . . . ? Mo1 C1 Mo2 C17 6.81(10) . . . . ? P1 C1 Mo2 C15 -134.13(12) . . . . ? Si1 C1 Mo2 C15 -5.1(2) . . . . ? Mo1 C1 Mo2 C15 145.81(11) . . . . ? P1 C1 Mo2 C16 -108.93(8) . . . . ? Si1 C1 Mo2 C16 20.10(18) . . . . ? Mo1 C1 Mo2 C16 171.00(7) . . . . ? P1 C1 Mo2 C14 -176.06(8) . . . . ? Si1 C1 Mo2 C14 -47.03(19) . . . . ? Mo1 C1 Mo2 C14 103.87(9) . . . . ? P1 C1 Mo2 C12 -129.93(9) . . . . ? Si1 C1 Mo2 C12 -0.90(16) . . . . ? Mo1 C1 Mo2 C12 150.00(8) . . . . ? P1 C1 Mo2 C13 -164.35(8) . . . . ? Si1 C1 Mo2 C13 -35.31(16) . . . . ? Mo1 C1 Mo2 C13 115.59(8) . . . . ? Si1 C1 Mo2 P1 129.03(19) . . . . ? Mo1 C1 Mo2 P1 -80.07(7) . . . . ? P1 C1 Mo2 Mo1 80.07(7) . . . . ? Si1 C1 Mo2 Mo1 -150.90(19) . . . . ? C1 P1 Mo2 C18 171.37(10) . . . . ? Mo1 P1 Mo2 C18 -125.73(7) . . . . ? C1 P1 Mo2 C17 -107.57(10) . . . . ? Mo1 P1 Mo2 C17 -44.67(7) . . . . ? Mo1 P1 Mo2 C1 62.90(7) . . . . ? C1 P1 Mo2 C15 121.21(15) . . . . ? Mo1 P1 Mo2 C15 -175.89(13) . . . . ? C1 P1 Mo2 C16 94.29(10) . . . . ? Mo1 P1 Mo2 C16 157.19(7) . . . . ? C1 P1 Mo2 C14 14.5(3) . . . . ? Mo1 P1 Mo2 C14 77.4(3) . . . . ? C1 P1 Mo2 C12 56.20(10) . . . . ? Mo1 P1 Mo2 C12 119.10(7) . . . . ? C1 P1 Mo2 C13 21.52(11) . . . . ? Mo1 P1 Mo2 C13 84.42(8) . . . . ? C1 P1 Mo2 Mo1 -62.90(7) . . . . ? C10 Mo1 Mo2 C18 -23.02(9) . . . . ? C11 Mo1 Mo2 C18 60.09(11) . . . . ? C1 Mo1 Mo2 C18 107.13(10) . . . . ? C8 Mo1 Mo2 C18 -125.93(14) . . . . ? C9 Mo1 Mo2 C18 179.22(12) . . . . ? C7 Mo1 Mo2 C18 -114.86(9) . . . . ? C6 Mo1 Mo2 C18 -142.47(10) . . . . ? C5 Mo1 Mo2 C18 -174.85(9) . . . . ? P1 Mo1 Mo2 C18 51.67(7) . . . . ? C10 Mo1 Mo2 C17 56.79(9) . . . . ? C11 Mo1 Mo2 C17 139.89(11) . . . . ? C1 Mo1 Mo2 C17 -173.07(10) . . . . ? C8 Mo1 Mo2 C17 -46.13(14) . . . . ? C9 Mo1 Mo2 C17 -100.97(12) . . . . ? C7 Mo1 Mo2 C17 -35.05(10) . . . . ? C6 Mo1 Mo2 C17 -62.67(10) . . . . ? C5 Mo1 Mo2 C17 -95.05(10) . . . . ? P1 Mo1 Mo2 C17 131.47(7) . . . . ? C10 Mo1 Mo2 C1 -130.15(9) . . . . ? C11 Mo1 Mo2 C1 -47.04(11) . . . . ? C8 Mo1 Mo2 C1 126.94(14) . . . . ? C9 Mo1 Mo2 C1 72.09(12) . . . . ? C7 Mo1 Mo2 C1 138.01(10) . . . . ? C6 Mo1 Mo2 C1 110.40(10) . . . . ? C5 Mo1 Mo2 C1 78.02(10) . . . . ? P1 Mo1 Mo2 C1 -55.46(7) . . . . ? C10 Mo1 Mo2 C15 100.56(16) . . . . ? C11 Mo1 Mo2 C15 -176.33(17) . . . . ? C1 Mo1 Mo2 C15 -129.29(16) . . . . ? C8 Mo1 Mo2 C15 -2.35(19) . . . . ? C9 Mo1 Mo2 C15 -57.20(17) . . . . ? C7 Mo1 Mo2 C15 8.72(16) . . . . ? C6 Mo1 Mo2 C15 -18.89(16) . . . . ? C5 Mo1 Mo2 C15 -51.27(16) . . . . ? P1 Mo1 Mo2 C15 175.25(15) . . . . ? C10 Mo1 Mo2 C16 -154.94(18) . . . . ? C11 Mo1 Mo2 C16 -71.83(19) . . . . ? C1 Mo1 Mo2 C16 -24.79(18) . . . . ? C8 Mo1 Mo2 C16 102.1(2) . . . . ? C9 Mo1 Mo2 C16 47.30(19) . . . . ? C7 Mo1 Mo2 C16 113.23(18) . . . . ? C6 Mo1 Mo2 C16 85.61(18) . . . . ? C5 Mo1 Mo2 C16 53.23(18) . . . . ? P1 Mo1 Mo2 C16 -80.25(17) . . . . ? C10 Mo1 Mo2 C14 120.36(10) . . . . ? C11 Mo1 Mo2 C14 -156.54(12) . . . . ? C1 Mo1 Mo2 C14 -109.49(11) . . . . ? C8 Mo1 Mo2 C14 17.44(14) . . . . ? C9 Mo1 Mo2 C14 -37.40(12) . . . . ? C7 Mo1 Mo2 C14 28.52(10) . . . . ? C6 Mo1 Mo2 C14 0.90(11) . . . . ? C5 Mo1 Mo2 C14 -31.48(11) . . . . ? P1 Mo1 Mo2 C14 -164.95(8) . . . . ? C10 Mo1 Mo2 C12 -168.38(10) . . . . ? C11 Mo1 Mo2 C12 -85.28(11) . . . . ? C1 Mo1 Mo2 C12 -38.24(10) . . . . ? C8 Mo1 Mo2 C12 88.70(14) . . . . ? C9 Mo1 Mo2 C12 33.86(12) . . . . ? C7 Mo1 Mo2 C12 99.78(10) . . . . ? C6 Mo1 Mo2 C12 72.16(11) . . . . ? C5 Mo1 Mo2 C12 39.78(10) . . . . ? P1 Mo1 Mo2 C12 -93.70(8) . . . . ? C10 Mo1 Mo2 C13 156.41(10) . . . . ? C11 Mo1 Mo2 C13 -120.49(11) . . . . ? C1 Mo1 Mo2 C13 -73.45(10) . . . . ? C8 Mo1 Mo2 C13 53.49(14) . . . . ? C9 Mo1 Mo2 C13 -1.35(13) . . . . ? C7 Mo1 Mo2 C13 64.57(10) . . . . ? C6 Mo1 Mo2 C13 36.95(10) . . . . ? C5 Mo1 Mo2 C13 4.57(10) . . . . ? P1 Mo1 Mo2 C13 -128.91(8) . . . . ? C10 Mo1 Mo2 P1 -74.69(6) . . . . ? C11 Mo1 Mo2 P1 8.42(9) . . . . ? C1 Mo1 Mo2 P1 55.46(7) . . . . ? C8 Mo1 Mo2 P1 -177.60(12) . . . . ? C9 Mo1 Mo2 P1 127.55(10) . . . . ? C7 Mo1 Mo2 P1 -166.53(7) . . . . ? C6 Mo1 Mo2 P1 165.86(7) . . . . ? C5 Mo1 Mo2 P1 133.48(7) . . . . ? C18 Mo2 C12 C16 31.68(17) . . . . ? C17 Mo2 C12 C16 -93.99(18) . . . . ? C1 Mo2 C12 C16 145.07(15) . . . . ? C15 Mo2 C12 C16 -37.80(14) . . . . ? C14 Mo2 C12 C16 -79.43(15) . . . . ? C13 Mo2 C12 C16 -116.3(2) . . . . ? P1 Mo2 C12 C16 110.78(13) . . . . ? Mo1 Mo2 C12 C16 172.03(11) . . . . ? C18 Mo2 C12 C13 148.00(14) . . . . ? C17 Mo2 C12 C13 22.3(2) . . . . ? C1 Mo2 C12 C13 -98.62(15) . . . . ? C15 Mo2 C12 C13 78.51(15) . . . . ? C16 Mo2 C12 C13 116.3(2) . . . . ? C14 Mo2 C12 C13 36.89(14) . . . . ? P1 Mo2 C12 C13 -132.91(13) . . . . ? Mo1 Mo2 C12 C13 -71.65(15) . . . . ? C16 C12 C13 C14 0.1(3) . . . . ? Mo2 C12 C13 C14 -63.45(16) . . . . ? C16 C12 C13 Mo2 63.52(15) . . . . ? C18 Mo2 C13 C14 60.7(2) . . . . ? C17 Mo2 C13 C14 -48.94(16) . . . . ? C1 Mo2 C13 C14 -162.83(14) . . . . ? C15 Mo2 C13 C14 37.37(14) . . . . ? C16 Mo2 C13 C14 79.20(15) . . . . ? C12 Mo2 C13 C14 116.2(2) . . . . ? P1 Mo2 C13 C14 -177.22(11) . . . . ? Mo1 Mo2 C13 C14 -118.29(13) . . . . ? C18 Mo2 C13 C12 -55.5(2) . . . . ? C17 Mo2 C13 C12 -165.15(14) . . . . ? C1 Mo2 C13 C12 80.96(14) . . . . ? C15 Mo2 C13 C12 -78.84(15) . . . . ? C16 Mo2 C13 C12 -37.00(14) . . . . ? C14 Mo2 C13 C12 -116.2(2) . . . . ? P1 Mo2 C13 C12 66.58(16) . . . . ? Mo1 Mo2 C13 C12 125.51(13) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? Mo2 C13 C14 C15 -63.22(16) . . . . ? C12 C13 C14 Mo2 63.58(15) . . . . ? C18 Mo2 C14 C13 -145.07(15) . . . . ? C17 Mo2 C14 C13 133.25(15) . . . . ? C1 Mo2 C14 C13 21.03(17) . . . . ? C15 Mo2 C14 C13 -116.4(2) . . . . ? C16 Mo2 C14 C13 -78.50(15) . . . . ? C12 Mo2 C14 C13 -37.32(14) . . . . ? P1 Mo2 C14 C13 9.1(4) . . . . ? Mo1 Mo2 C14 C13 78.07(15) . . . . ? C18 Mo2 C14 C15 -28.72(18) . . . . ? C17 Mo2 C14 C15 -110.39(16) . . . . ? C1 Mo2 C14 C15 137.39(14) . . . . ? C16 Mo2 C14 C15 37.85(14) . . . . ? C12 Mo2 C14 C15 79.04(15) . . . . ? C13 Mo2 C14 C15 116.4(2) . . . . ? P1 Mo2 C14 C15 125.5(2) . . . . ? Mo1 Mo2 C14 C15 -165.58(12) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? Mo2 C14 C15 C16 -65.56(16) . . . . ? C13 C14 C15 Mo2 64.90(16) . . . . ? C18 Mo2 C15 C14 155.99(16) . . . . ? C17 Mo2 C15 C14 69.21(16) . . . . ? C1 Mo2 C15 C14 -73.2(2) . . . . ? C16 Mo2 C15 C14 -115.3(2) . . . . ? C12 Mo2 C15 C14 -78.10(16) . . . . ? C13 Mo2 C15 C14 -36.74(15) . . . . ? P1 Mo2 C15 C14 -157.93(12) . . . . ? Mo1 Mo2 C15 C14 30.0(2) . . . . ? C18 Mo2 C15 C16 -88.70(15) . . . . ? C17 Mo2 C15 C16 -175.47(14) . . . . ? C1 Mo2 C15 C16 42.2(2) . . . . ? C14 Mo2 C15 C16 115.3(2) . . . . ? C12 Mo2 C15 C16 37.22(14) . . . . ? C13 Mo2 C15 C16 78.58(15) . . . . ? P1 Mo2 C15 C16 -42.6(2) . . . . ? Mo1 Mo2 C15 C16 145.29(13) . . . . ? C13 C12 C16 C15 -0.5(2) . . . . ? Mo2 C12 C16 C15 64.02(15) . . . . ? C13 C12 C16 Mo2 -64.50(15) . . . . ? C14 C15 C16 C12 0.7(3) . . . . ? Mo2 C15 C16 C12 -65.34(15) . . . . ? C14 C15 C16 Mo2 66.04(16) . . . . ? C18 Mo2 C16 C12 -152.99(15) . . . . ? C17 Mo2 C16 C12 121.60(16) . . . . ? C1 Mo2 C16 C12 -38.95(16) . . . . ? C15 Mo2 C16 C12 115.6(2) . . . . ? C14 Mo2 C16 C12 78.01(15) . . . . ? C13 Mo2 C16 C12 37.17(14) . . . . ? P1 Mo2 C16 C12 -86.87(14) . . . . ? Mo1 Mo2 C16 C12 -19.2(3) . . . . ? C18 Mo2 C16 C15 91.37(15) . . . . ? C17 Mo2 C16 C15 5.95(19) . . . . ? C1 Mo2 C16 C15 -154.59(13) . . . . ? C14 Mo2 C16 C15 -37.63(14) . . . . ? C12 Mo2 C16 C15 -115.6(2) . . . . ? C13 Mo2 C16 C15 -78.47(15) . . . . ? P1 Mo2 C16 C15 157.48(12) . . . . ? Mo1 Mo2 C16 C15 -134.88(16) . . . . ? C18 Mo2 C17 O2 -84.5(10) . . . . ? C1 Mo2 C17 O2 163.1(10) . . . . ? C15 Mo2 C17 O2 5.7(10) . . . . ? C16 Mo2 C17 O2 2.2(10) . . . . ? C14 Mo2 C17 O2 38.4(10) . . . . ? C12 Mo2 C17 O2 50.8(10) . . . . ? C13 Mo2 C17 O2 63.8(10) . . . . ? P1 Mo2 C17 O2 -152.7(10) . . . . ? Mo1 Mo2 C17 O2 168.6(10) . . . . ? C17 Mo2 C18 O3 100(2) . . . . ? C1 Mo2 C18 O3 -147(2) . . . . ? C15 Mo2 C18 O3 4(2) . . . . ? C16 Mo2 C18 O3 -31(2) . . . . ? C14 Mo2 C18 O3 20(2) . . . . ? C12 Mo2 C18 O3 -48(2) . . . . ? C13 Mo2 C18 O3 -15(2) . . . . ? P1 Mo2 C18 O3 -154(2) . . . . ? Mo1 Mo2 C18 O3 164(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.710 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.238 data_7 _database_code_depnum_ccdc_archive 'CCDC 894370' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H39 P3 Pt Si' _chemical_formula_sum 'C40 H39 P3 Pt Si' _chemical_formula_weight 835.80 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1854(2) _cell_length_b 15.5576(4) _cell_length_c 19.0907(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.217(2) _cell_angle_gamma 90.00 _cell_volume 3572.40(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 30591 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 4.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.676141 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; 'Data collected at the EPSRC National Crystallography Service, Southhampton' ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; 'Bruker-Nonius APEX II CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34735 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8165 _reflns_number_gt 6318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.0511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8165 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 Pt1 Pt 0.878159(18) 0.124265(15) 0.743610(12) 0.01606(7) Uani 1 1 d . . . P1 P 0.83952(14) 0.11329(12) 0.85854(8) 0.0236(4) Uani 1 1 d . . . C1 C 0.7371(5) 0.1268(4) 0.7922(3) 0.0191(12) Uani 1 1 d . . . Si1 Si 0.58329(14) 0.13281(12) 0.78009(9) 0.0213(4) Uani 1 1 d . . . C2 C 0.5365(6) 0.0509(5) 0.8408(4) 0.0336(17) Uani 1 1 d . . . H2A H 0.5493 -0.0069 0.8234 0.050 Uiso 1 1 calc R . . H2B H 0.4570 0.0586 0.8422 0.050 Uiso 1 1 calc R . . H2C H 0.5786 0.0581 0.8887 0.050 Uiso 1 1 calc R . . C3 C 0.5363(6) 0.2407(4) 0.8046(4) 0.0299(16) Uani 1 1 d . . . H3A H 0.5723 0.2550 0.8528 0.045 Uiso 1 1 calc R . . H3B H 0.4555 0.2403 0.8026 0.045 Uiso 1 1 calc R . . H3C H 0.5565 0.2836 0.7713 0.045 Uiso 1 1 calc R . . C4 C 0.5155(6) 0.1104(5) 0.6872(4) 0.0334(17) Uani 1 1 d . . . H4A H 0.5455 0.1494 0.6546 0.050 Uiso 1 1 calc R . . H4B H 0.4351 0.1193 0.6831 0.050 Uiso 1 1 calc R . . H4C H 0.5302 0.0508 0.6749 0.050 Uiso 1 1 calc R . . P2 P 1.06587(13) 0.11444(10) 0.74969(8) 0.0186(3) Uani 1 1 d . . . P3 P 0.81846(13) 0.14234(10) 0.62474(8) 0.0169(3) Uani 1 1 d . . . C5 C 1.1433(5) 0.1033(4) 0.8400(3) 0.0241(14) Uani 1 1 d . . . C6 C 1.1168(6) 0.0338(5) 0.8802(4) 0.0341(17) Uani 1 1 d . . . H6 H 1.0584 -0.0039 0.8609 0.041 Uiso 1 1 calc R . . C7 C 1.1742(7) 0.0185(5) 0.9480(4) 0.0400(19) Uani 1 1 d . . . H7 H 1.1542 -0.0286 0.9750 0.048 Uiso 1 1 calc R . . C8 C 1.2601(7) 0.0718(6) 0.9757(4) 0.043(2) Uani 1 1 d . . . H8 H 1.3004 0.0611 1.0217 0.052 Uiso 1 1 calc R . . C9 C 1.2882(6) 0.1411(6) 0.9370(4) 0.044(2) Uani 1 1 d . . . H9 H 1.3469 0.1782 0.9570 0.053 Uiso 1 1 calc R . . C10 C 1.2315(5) 0.1573(5) 0.8686(4) 0.0295(16) Uani 1 1 d . . . H10 H 1.2524 0.2043 0.8419 0.035 Uiso 1 1 calc R . . C11 C 1.1228(5) 0.0204(4) 0.7101(3) 0.0186(13) Uani 1 1 d . . . C12 C 1.0517(5) -0.0425(4) 0.6771(3) 0.0240(14) Uani 1 1 d . . . H12 H 0.9735 -0.0349 0.6720 0.029 Uiso 1 1 calc R . . C13 C 1.0954(6) -0.1170(4) 0.6513(3) 0.0264(14) Uani 1 1 d . . . H13 H 1.0466 -0.1602 0.6291 0.032 Uiso 1 1 calc R . . C14 C 1.2094(6) -0.1284(5) 0.6578(3) 0.0299(15) Uani 1 1 d . . . H14 H 1.2388 -0.1788 0.6396 0.036 Uiso 1 1 calc R . . C15 C 1.2804(6) -0.0659(4) 0.6910(4) 0.0254(14) Uani 1 1 d . . . H15 H 1.3586 -0.0729 0.6951 0.030 Uiso 1 1 calc R . . C16 C 1.2367(5) 0.0070(4) 0.7183(3) 0.0232(14) Uani 1 1 d . . . H16 H 1.2856 0.0483 0.7430 0.028 Uiso 1 1 calc R . . C17 C 1.1295(5) 0.2089(4) 0.7155(3) 0.0203(13) Uani 1 1 d . . . C18 C 1.0928(6) 0.2884(4) 0.7353(4) 0.0276(15) Uani 1 1 d . . . H18 H 1.0353 0.2910 0.7635 0.033 Uiso 1 1 calc R . . C19 C 1.1386(6) 0.3640(4) 0.7145(4) 0.0302(15) Uani 1 1 d . . . H19 H 1.1131 0.4179 0.7289 0.036 Uiso 1 1 calc R . . C20 C 1.2215(6) 0.3608(5) 0.6727(4) 0.0324(17) Uani 1 1 d . . . H20 H 1.2541 0.4124 0.6589 0.039 Uiso 1 1 calc R . . C21 C 1.2560(6) 0.2827(5) 0.6514(4) 0.0311(16) Uani 1 1 d . . . H21 H 1.3121 0.2806 0.6222 0.037 Uiso 1 1 calc R . . C22 C 1.2107(6) 0.2060(4) 0.6717(4) 0.0271(15) Uani 1 1 d . . . H22 H 1.2349 0.1524 0.6558 0.033 Uiso 1 1 calc R . . C23 C 0.9214(5) 0.1708(4) 0.5690(3) 0.0213(13) Uani 1 1 d . . . C24 C 0.9424(5) 0.2572(4) 0.5538(4) 0.0268(15) Uani 1 1 d . . . H24 H 0.8985 0.3016 0.5692 0.032 Uiso 1 1 calc R . . C25 C 1.0273(6) 0.2771(4) 0.5163(4) 0.0308(16) Uani 1 1 d . . . H25 H 1.0410 0.3355 0.5059 0.037 Uiso 1 1 calc R . . C26 C 1.0915(6) 0.2141(5) 0.4940(4) 0.0349(17) Uani 1 1 d . . . H26 H 1.1499 0.2290 0.4687 0.042 Uiso 1 1 calc R . . C27 C 1.0719(5) 0.1281(5) 0.5081(3) 0.0290(15) Uani 1 1 d . . . H27 H 1.1165 0.0844 0.4921 0.035 Uiso 1 1 calc R . . C28 C 0.9875(5) 0.1062(4) 0.5453(3) 0.0208(13) Uani 1 1 d . . . H28 H 0.9741 0.0476 0.5548 0.025 Uiso 1 1 calc R . . C29 C 0.7183(5) 0.2292(4) 0.6016(3) 0.0186(13) Uani 1 1 d . . . C30 C 0.6552(6) 0.2380(5) 0.5346(4) 0.0328(17) Uani 1 1 d . . . H30 H 0.6587 0.1945 0.5001 0.039 Uiso 1 1 calc R . . C31 C 0.5873(6) 0.3086(5) 0.5171(4) 0.0355(18) Uani 1 1 d . . . H31 H 0.5464 0.3140 0.4706 0.043 Uiso 1 1 calc R . . C32 C 0.5792(6) 0.3708(5) 0.5668(3) 0.0289(15) Uani 1 1 d . . . H32 H 0.5309 0.4185 0.5555 0.035 Uiso 1 1 calc R . . C33 C 0.6410(7) 0.3637(5) 0.6327(4) 0.0395(19) Uani 1 1 d . . . H33 H 0.6370 0.4075 0.6670 0.047 Uiso 1 1 calc R . . C34 C 0.7092(6) 0.2936(4) 0.6502(4) 0.0306(16) Uani 1 1 d . . . H34 H 0.7509 0.2895 0.6967 0.037 Uiso 1 1 calc R . . C35 C 0.7483(5) 0.0467(4) 0.5813(3) 0.0213(13) Uani 1 1 d . . . C36 C 0.7139(5) -0.0172(4) 0.6237(4) 0.0242(14) Uani 1 1 d . . . H36 H 0.7318 -0.0131 0.6739 0.029 Uiso 1 1 calc R . . C37 C 0.6538(6) -0.0867(5) 0.5931(4) 0.0338(17) Uani 1 1 d . . . H37 H 0.6313 -0.1305 0.6225 0.041 Uiso 1 1 calc R . . C38 C 0.6262(6) -0.0931(4) 0.5206(4) 0.0332(17) Uani 1 1 d . . . H38 H 0.5822 -0.1398 0.5001 0.040 Uiso 1 1 calc R . . C39 C 0.6623(6) -0.0319(5) 0.4776(4) 0.0294(16) Uani 1 1 d . . . H39 H 0.6452 -0.0372 0.4275 0.035 Uiso 1 1 calc R . . C40 C 0.7240(5) 0.0380(4) 0.5079(4) 0.0263(15) Uani 1 1 d . . . H40 H 0.7497 0.0800 0.4782 0.032 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 Pt1 0.01424(11) 0.01699(11) 0.01656(11) 0.00030(10) 0.00131(8) 0.00058(10) P1 0.0212(8) 0.0319(10) 0.0179(8) 0.0009(7) 0.0033(6) -0.0018(7) C1 0.020(3) 0.018(3) 0.021(3) -0.001(3) 0.006(2) -0.001(3) Si1 0.0164(8) 0.0228(9) 0.0254(9) -0.0024(7) 0.0054(7) -0.0028(7) C2 0.023(4) 0.027(4) 0.052(5) 0.004(3) 0.011(3) 0.000(3) C3 0.022(4) 0.029(4) 0.040(4) -0.009(3) 0.010(3) -0.004(3) C4 0.023(4) 0.042(5) 0.034(4) -0.010(3) 0.003(3) -0.007(3) P2 0.0172(8) 0.0184(8) 0.0197(8) -0.0011(6) 0.0017(6) 0.0033(7) P3 0.0141(7) 0.0199(8) 0.0163(7) -0.0004(6) 0.0013(6) 0.0008(6) C5 0.023(3) 0.022(3) 0.026(3) -0.005(3) 0.001(3) 0.015(3) C6 0.039(4) 0.040(4) 0.019(4) 0.000(3) -0.006(3) 0.006(3) C7 0.041(5) 0.048(5) 0.031(4) -0.001(4) 0.004(3) 0.023(4) C8 0.040(5) 0.065(6) 0.022(4) -0.010(4) -0.006(3) 0.030(4) C9 0.024(4) 0.058(6) 0.044(5) -0.025(4) -0.010(3) 0.009(4) C10 0.017(3) 0.039(4) 0.031(4) -0.007(3) -0.001(3) 0.006(3) C11 0.015(3) 0.023(3) 0.017(3) 0.004(2) 0.000(2) 0.007(2) C12 0.019(3) 0.029(4) 0.024(3) 0.001(3) 0.004(3) 0.001(3) C13 0.035(4) 0.021(3) 0.023(3) -0.007(3) 0.007(3) -0.001(3) C14 0.043(4) 0.021(3) 0.029(3) 0.006(3) 0.015(3) 0.004(3) C15 0.026(4) 0.021(3) 0.031(4) 0.004(3) 0.010(3) 0.008(3) C16 0.019(3) 0.022(3) 0.028(4) 0.000(3) 0.003(3) -0.002(3) C17 0.020(3) 0.012(3) 0.027(3) 0.002(2) -0.001(3) 0.001(2) C18 0.030(4) 0.024(3) 0.030(4) -0.008(3) 0.009(3) 0.002(3) C19 0.035(4) 0.021(4) 0.034(4) -0.004(3) 0.001(3) -0.003(3) C20 0.026(4) 0.028(4) 0.043(4) 0.007(3) 0.004(3) -0.007(3) C21 0.033(4) 0.031(4) 0.033(4) -0.003(3) 0.015(3) 0.003(3) C22 0.029(4) 0.019(3) 0.032(4) 0.000(3) 0.001(3) 0.004(3) C23 0.019(3) 0.025(3) 0.018(3) 0.003(3) -0.002(2) -0.003(3) C24 0.021(3) 0.025(4) 0.034(4) 0.003(3) 0.006(3) 0.003(3) C25 0.033(4) 0.023(4) 0.037(4) 0.009(3) 0.005(3) -0.009(3) C26 0.031(4) 0.044(5) 0.032(4) 0.003(3) 0.012(3) -0.017(3) C27 0.029(4) 0.030(4) 0.030(3) -0.015(3) 0.009(3) 0.000(3) C28 0.022(3) 0.023(3) 0.017(3) -0.005(2) 0.002(2) 0.001(3) C29 0.018(3) 0.021(3) 0.016(3) -0.003(2) 0.001(2) 0.000(2) C30 0.033(4) 0.045(5) 0.018(3) -0.002(3) 0.000(3) 0.015(3) C31 0.035(4) 0.046(5) 0.022(4) -0.002(3) -0.005(3) 0.010(4) C32 0.031(4) 0.024(3) 0.030(4) 0.000(3) -0.002(3) 0.009(3) C33 0.050(5) 0.028(4) 0.036(4) -0.006(3) -0.007(3) 0.014(4) C34 0.038(4) 0.023(4) 0.028(4) -0.005(3) -0.006(3) 0.010(3) C35 0.016(3) 0.023(3) 0.025(3) 0.001(3) 0.004(3) 0.001(3) C36 0.026(4) 0.022(3) 0.024(3) -0.001(3) 0.003(3) 0.000(3) C37 0.037(4) 0.021(4) 0.044(5) -0.003(3) 0.010(3) -0.008(3) C38 0.028(4) 0.018(3) 0.051(5) -0.012(3) 0.001(3) -0.010(3) C39 0.025(4) 0.033(4) 0.028(4) -0.009(3) -0.002(3) -0.004(3) C40 0.023(4) 0.029(4) 0.027(4) -0.003(3) 0.004(3) 0.000(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 Pt1 C1 2.081(6) . ? Pt1 P2 2.2768(16) . ? Pt1 P3 2.2867(15) . ? Pt1 P1 2.3229(16) . ? P1 C1 1.643(6) . ? C1 Si1 1.853(6) . ? Si1 C3 1.857(7) . ? Si1 C4 1.866(7) . ? Si1 C2 1.872(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P2 C17 1.831(6) . ? P2 C11 1.834(6) . ? P2 C5 1.836(7) . ? P3 C23 1.825(6) . ? P3 C29 1.827(6) . ? P3 C35 1.846(7) . ? C5 C6 1.394(10) . ? C5 C10 1.404(9) . ? C6 C7 1.389(10) . ? C6 H6 0.9500 . ? C7 C8 1.373(12) . ? C7 H7 0.9500 . ? C8 C9 1.380(12) . ? C8 H8 0.9500 . ? C9 C10 1.398(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.389(9) . ? C11 C16 1.387(8) . ? C12 C13 1.398(9) . ? C12 H12 0.9500 . ? C13 C14 1.387(9) . ? C13 H13 0.9500 . ? C14 C15 1.385(10) . ? C14 H14 0.9500 . ? C15 C16 1.390(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.388(8) . ? C17 C22 1.395(9) . ? C18 C19 1.387(9) . ? C18 H18 0.9500 . ? C19 C20 1.386(10) . ? C19 H19 0.9500 . ? C20 C21 1.369(9) . ? C20 H20 0.9500 . ? C21 C22 1.395(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.407(9) . ? C23 C28 1.406(9) . ? C24 C25 1.384(9) . ? C24 H24 0.9500 . ? C25 C26 1.363(10) . ? C25 H25 0.9500 . ? C26 C27 1.394(10) . ? C26 H26 0.9500 . ? C27 C28 1.383(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.383(9) . ? C29 C30 1.389(9) . ? C30 C31 1.384(10) . ? C30 H30 0.9500 . ? C31 C32 1.370(10) . ? C31 H31 0.9500 . ? C32 C33 1.363(10) . ? C32 H32 0.9500 . ? C33 C34 1.380(9) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.389(9) . ? C35 C40 1.391(9) . ? C36 C37 1.382(9) . ? C36 H36 0.9500 . ? C37 C38 1.376(11) . ? C37 H37 0.9500 . ? C38 C39 1.374(10) . ? C38 H38 0.9500 . ? C39 C40 1.393(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 C1 Pt1 P2 150.87(17) . . ? C1 Pt1 P3 106.63(17) . . ? P2 Pt1 P3 102.48(5) . . ? C1 Pt1 P1 43.37(17) . . ? P2 Pt1 P1 107.51(6) . . ? P3 Pt1 P1 150.00(6) . . ? C1 P1 Pt1 60.5(2) . . ? P1 C1 Si1 137.0(4) . . ? P1 C1 Pt1 76.2(2) . . ? Si1 C1 Pt1 146.7(3) . . ? C1 Si1 C3 111.1(3) . . ? C1 Si1 C4 113.2(3) . . ? C3 Si1 C4 107.5(3) . . ? C1 Si1 C2 106.9(3) . . ? C3 Si1 C2 108.8(3) . . ? C4 Si1 C2 109.2(3) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C17 P2 C11 106.5(3) . . ? C17 P2 C5 103.2(3) . . ? C11 P2 C5 98.1(3) . . ? C17 P2 Pt1 114.0(2) . . ? C11 P2 Pt1 118.4(2) . . ? C5 P2 Pt1 114.5(2) . . ? C23 P3 C29 100.1(3) . . ? C23 P3 C35 104.2(3) . . ? C29 P3 C35 104.1(3) . . ? C23 P3 Pt1 118.0(2) . . ? C29 P3 Pt1 115.2(2) . . ? C35 P3 Pt1 113.4(2) . . ? C6 C5 C10 118.7(6) . . ? C6 C5 P2 117.5(5) . . ? C10 C5 P2 123.7(5) . . ? C7 C6 C5 121.3(8) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 119.6(8) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 120.3(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 120.9(7) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C5 119.2(7) . . ? C9 C10 H10 120.4 . . ? C5 C10 H10 120.4 . . ? C12 C11 C16 119.1(6) . . ? C12 C11 P2 120.0(5) . . ? C16 C11 P2 120.7(5) . . ? C11 C12 C13 119.9(6) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.5(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.7(6) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 121.1(6) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C22 118.9(6) . . ? C18 C17 P2 116.4(5) . . ? C22 C17 P2 124.7(5) . . ? C17 C18 C19 121.1(6) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 119.9(6) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 119.3(7) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 121.6(7) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C17 C22 C21 119.3(6) . . ? C17 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C28 118.9(6) . . ? C24 C23 P3 121.1(5) . . ? C28 C23 P3 119.8(5) . . ? C25 C24 C23 119.8(6) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.9(6) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 120.1(6) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C34 C29 C30 117.0(6) . . ? C34 C29 P3 119.7(5) . . ? C30 C29 P3 123.0(5) . . ? C31 C30 C29 121.5(7) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 120.0(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 120.6(7) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 121.4(6) . . ? C33 C34 H34 119.3 . . ? C29 C34 H34 119.3 . . ? C36 C35 C40 118.8(6) . . ? C36 C35 P3 118.4(5) . . ? C40 C35 P3 122.7(5) . . ? C37 C36 C35 120.2(6) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.6(7) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 120.1(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 119.8(7) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C35 C40 C39 120.4(7) . . ? C35 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? 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 P2 Pt1 P1 C1 179.3(3) . . . . ? P3 Pt1 P1 C1 0.8(3) . . . . ? Pt1 P1 C1 Si1 177.1(7) . . . . ? P2 Pt1 C1 P1 -1.3(5) . . . . ? P3 Pt1 C1 P1 -179.59(15) . . . . ? P2 Pt1 C1 Si1 -177.7(3) . . . . ? P3 Pt1 C1 Si1 4.0(7) . . . . ? P1 Pt1 C1 Si1 -176.4(8) . . . . ? P1 C1 Si1 C3 79.5(6) . . . . ? Pt1 C1 Si1 C3 -105.6(7) . . . . ? P1 C1 Si1 C4 -159.4(5) . . . . ? Pt1 C1 Si1 C4 15.5(8) . . . . ? P1 C1 Si1 C2 -39.1(6) . . . . ? Pt1 C1 Si1 C2 135.8(6) . . . . ? C1 Pt1 P2 C17 -119.0(4) . . . . ? P3 Pt1 P2 C17 59.3(2) . . . . ? P1 Pt1 P2 C17 -120.0(2) . . . . ? C1 Pt1 P2 C11 114.5(4) . . . . ? P3 Pt1 P2 C11 -67.2(2) . . . . ? P1 Pt1 P2 C11 113.5(2) . . . . ? C1 Pt1 P2 C5 -0.5(4) . . . . ? P3 Pt1 P2 C5 177.8(2) . . . . ? P1 Pt1 P2 C5 -1.4(2) . . . . ? C1 Pt1 P3 C23 164.6(3) . . . . ? P2 Pt1 P3 C23 -14.6(3) . . . . ? P1 Pt1 P3 C23 164.0(3) . . . . ? C1 Pt1 P3 C29 46.7(3) . . . . ? P2 Pt1 P3 C29 -132.5(2) . . . . ? P1 Pt1 P3 C29 46.1(3) . . . . ? C1 Pt1 P3 C35 -73.2(3) . . . . ? P2 Pt1 P3 C35 107.7(2) . . . . ? P1 Pt1 P3 C35 -73.8(3) . . . . ? C17 P2 C5 C6 -177.7(5) . . . . ? C11 P2 C5 C6 -68.6(6) . . . . ? Pt1 P2 C5 C6 57.8(5) . . . . ? C17 P2 C5 C10 -1.9(6) . . . . ? C11 P2 C5 C10 107.2(6) . . . . ? Pt1 P2 C5 C10 -126.4(5) . . . . ? C10 C5 C6 C7 1.4(10) . . . . ? P2 C5 C6 C7 177.4(6) . . . . ? C5 C6 C7 C8 -1.1(11) . . . . ? C6 C7 C8 C9 1.0(11) . . . . ? C7 C8 C9 C10 -1.2(11) . . . . ? C8 C9 C10 C5 1.4(11) . . . . ? C6 C5 C10 C9 -1.5(10) . . . . ? P2 C5 C10 C9 -177.3(5) . . . . ? C17 P2 C11 C12 -129.7(5) . . . . ? C5 P2 C11 C12 123.9(5) . . . . ? Pt1 P2 C11 C12 0.3(6) . . . . ? C17 P2 C11 C16 56.3(6) . . . . ? C5 P2 C11 C16 -50.1(6) . . . . ? Pt1 P2 C11 C16 -173.7(4) . . . . ? C16 C11 C12 C13 -1.5(9) . . . . ? P2 C11 C12 C13 -175.5(5) . . . . ? C11 C12 C13 C14 -0.6(10) . . . . ? C12 C13 C14 C15 0.9(10) . . . . ? C13 C14 C15 C16 0.9(10) . . . . ? C12 C11 C16 C15 3.3(9) . . . . ? P2 C11 C16 C15 177.3(5) . . . . ? C14 C15 C16 C11 -3.0(10) . . . . ? C11 P2 C17 C18 176.1(5) . . . . ? C5 P2 C17 C18 -81.2(5) . . . . ? Pt1 P2 C17 C18 43.6(6) . . . . ? C11 P2 C17 C22 -3.9(6) . . . . ? C5 P2 C17 C22 98.8(6) . . . . ? Pt1 P2 C17 C22 -136.3(5) . . . . ? C22 C17 C18 C19 -2.6(10) . . . . ? P2 C17 C18 C19 177.5(5) . . . . ? C17 C18 C19 C20 0.7(10) . . . . ? C18 C19 C20 C21 1.0(11) . . . . ? C19 C20 C21 C22 -0.9(11) . . . . ? C18 C17 C22 C21 2.6(10) . . . . ? P2 C17 C22 C21 -177.4(5) . . . . ? C20 C21 C22 C17 -0.9(11) . . . . ? C29 P3 C23 C24 32.6(6) . . . . ? C35 P3 C23 C24 140.1(5) . . . . ? Pt1 P3 C23 C24 -93.1(5) . . . . ? C29 P3 C23 C28 -152.5(5) . . . . ? C35 P3 C23 C28 -45.0(5) . . . . ? Pt1 P3 C23 C28 81.8(5) . . . . ? C28 C23 C24 C25 -0.3(10) . . . . ? P3 C23 C24 C25 174.7(5) . . . . ? C23 C24 C25 C26 -0.3(11) . . . . ? C24 C25 C26 C27 0.6(11) . . . . ? C25 C26 C27 C28 -0.5(11) . . . . ? C26 C27 C28 C23 -0.1(10) . . . . ? C24 C23 C28 C27 0.4(9) . . . . ? P3 C23 C28 C27 -174.6(5) . . . . ? C23 P3 C29 C34 -108.1(6) . . . . ? C35 P3 C29 C34 144.4(6) . . . . ? Pt1 P3 C29 C34 19.5(6) . . . . ? C23 P3 C29 C30 66.8(6) . . . . ? C35 P3 C29 C30 -40.7(7) . . . . ? Pt1 P3 C29 C30 -165.6(5) . . . . ? C34 C29 C30 C31 0.8(11) . . . . ? P3 C29 C30 C31 -174.3(6) . . . . ? C29 C30 C31 C32 -1.6(12) . . . . ? C30 C31 C32 C33 2.0(12) . . . . ? C31 C32 C33 C34 -1.6(12) . . . . ? C32 C33 C34 C29 0.8(13) . . . . ? C30 C29 C34 C33 -0.4(11) . . . . ? P3 C29 C34 C33 174.8(6) . . . . ? C23 P3 C35 C36 144.8(5) . . . . ? C29 P3 C35 C36 -110.7(5) . . . . ? Pt1 P3 C35 C36 15.2(6) . . . . ? C23 P3 C35 C40 -38.3(6) . . . . ? C29 P3 C35 C40 66.2(6) . . . . ? Pt1 P3 C35 C40 -167.9(5) . . . . ? C40 C35 C36 C37 -1.9(10) . . . . ? P3 C35 C36 C37 175.1(5) . . . . ? C35 C36 C37 C38 -0.7(11) . . . . ? C36 C37 C38 C39 2.7(11) . . . . ? C37 C38 C39 C40 -1.9(11) . . . . ? C36 C35 C40 C39 2.6(10) . . . . ? P3 C35 C40 C39 -174.3(5) . . . . ? C38 C39 C40 C35 -0.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.995 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.181 data_8 _database_code_depnum_ccdc_archive 'CCDC 894371' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H57 P5 Pd2 Si1, 1.5 C7 H8' _chemical_formula_sum 'C66.50 H69 P5 Pd2 Si' _chemical_formula_weight 1263.96 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1118(2) _cell_length_b 14.1587(3) _cell_length_c 20.7997(5) _cell_angle_alpha 79.4380(10) _cell_angle_beta 83.5530(10) _cell_angle_gamma 67.8970(10) _cell_volume 2977.16(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13699 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1298 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7744 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; 'Bruker-Nonius FR591 rotating anode' ; _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; 'Bruker-Nonius APEX II CCD camera on \k-goniostat' ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46928 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.68 _reflns_number_total 13622 _reflns_number_gt 9446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_data_reduction ; 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+26.9145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13622 _refine_ls_number_parameters 658 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.46895(14) 0.33108(12) 0.20334(8) 0.0195(3) Uani 1 1 d . . . P2 P 0.24569(14) 0.30525(12) 0.09110(8) 0.0196(3) Uani 1 1 d . . . P3 P 0.02858(14) 0.44133(12) 0.18129(8) 0.0206(3) Uani 1 1 d . . . P4 P 0.48621(15) 0.08035(12) 0.32678(8) 0.0196(3) Uani 1 1 d . . . P5 P 0.30649(14) 0.25333(12) 0.40926(8) 0.0183(3) Uani 1 1 d . . . Pd1 Pd 0.25269(4) 0.37401(3) 0.18091(2) 0.01775(11) Uani 1 1 d . . . Pd2 Pd 0.39589(4) 0.25674(3) 0.30352(2) 0.01712(11) Uani 1 1 d . . . C1 C 0.3516(5) 0.4085(4) 0.2513(3) 0.0184(12) Uani 1 1 d . . . Si1 Si 0.33592(17) 0.53445(13) 0.26992(9) 0.0242(4) Uani 1 1 d . . . C2 C 0.4955(7) 0.5281(6) 0.2962(4) 0.0391(18) Uani 1 1 d . . . H2A H 0.5164 0.4821 0.3381 0.059 Uiso 1 1 calc R . . H2B H 0.4892 0.5973 0.3012 0.059 Uiso 1 1 calc R . . H2C H 0.5641 0.5016 0.2630 0.059 Uiso 1 1 calc R . . C3 C 0.2117(9) 0.5891(6) 0.3344(5) 0.053(3) Uani 1 1 d . . . H3A H 0.1248 0.6031 0.3201 0.080 Uiso 1 1 calc R . . H3B H 0.2175 0.6534 0.3422 0.080 Uiso 1 1 calc R . . H3C H 0.2274 0.5395 0.3751 0.080 Uiso 1 1 calc R . . C4 C 0.2897(7) 0.6324(5) 0.1945(4) 0.0381(18) Uani 1 1 d . . . H4A H 0.3465 0.6054 0.1573 0.057 Uiso 1 1 calc R . . H4B H 0.2994 0.6959 0.2010 0.057 Uiso 1 1 calc R . . H4C H 0.1991 0.6472 0.1856 0.057 Uiso 1 1 calc R . . C5 C 0.3242(6) 0.1683(5) 0.0865(3) 0.0243(14) Uani 1 1 d . . . C6 C 0.4429(7) 0.1147(5) 0.1163(4) 0.0325(16) Uani 1 1 d . . . H6 H 0.4792 0.1500 0.1384 0.039 Uiso 1 1 calc R . . C7 C 0.5072(8) 0.0117(6) 0.1138(4) 0.045(2) Uani 1 1 d . . . H7 H 0.5889 -0.0237 0.1330 0.053 Uiso 1 1 calc R . . C8 C 0.4535(8) -0.0410(6) 0.0834(5) 0.049(2) Uani 1 1 d . . . H8 H 0.4972 -0.1129 0.0832 0.058 Uiso 1 1 calc R . . C9 C 0.3369(8) 0.0098(6) 0.0533(4) 0.044(2) Uani 1 1 d . . . H9 H 0.3016 -0.0263 0.0313 0.053 Uiso 1 1 calc R . . C10 C 0.2717(7) 0.1147(5) 0.0555(4) 0.0313(16) Uani 1 1 d . . . H10 H 0.1905 0.1499 0.0357 0.038 Uiso 1 1 calc R . . C11 C 0.3025(5) 0.3661(4) 0.0145(3) 0.0201(13) Uani 1 1 d . . . C12 C 0.3240(6) 0.3250(5) -0.0433(3) 0.0238(13) Uani 1 1 d . . . H12 H 0.3069 0.2642 -0.0437 0.029 Uiso 1 1 calc R . . C13 C 0.3697(6) 0.3708(5) -0.1003(4) 0.0302(15) Uani 1 1 d . . . H13 H 0.3852 0.3414 -0.1394 0.036 Uiso 1 1 calc R . . C14 C 0.3922(6) 0.4602(5) -0.0991(4) 0.0316(16) Uani 1 1 d . . . H14 H 0.4228 0.4928 -0.1381 0.038 Uiso 1 1 calc R . . C15 C 0.3711(7) 0.5025(6) -0.0427(4) 0.0364(17) Uani 1 1 d . . . H15 H 0.3874 0.5637 -0.0427 0.044 Uiso 1 1 calc R . . C16 C 0.3256(6) 0.4558(5) 0.0145(4) 0.0296(15) Uani 1 1 d . . . H16 H 0.3103 0.4854 0.0535 0.035 Uiso 1 1 calc R . . C17 C 0.0726(6) 0.3351(5) 0.0762(3) 0.0229(13) Uani 1 1 d . . . H17A H 0.0628 0.3378 0.0291 0.027 Uiso 1 1 calc R . . H17B H 0.0437 0.2803 0.1013 0.027 Uiso 1 1 calc R . . C18 C -0.0105(6) 0.4386(5) 0.0973(3) 0.0262(14) Uani 1 1 d . . . H18A H -0.1037 0.4495 0.0964 0.031 Uiso 1 1 calc R . . H18B H 0.0064 0.4949 0.0664 0.031 Uiso 1 1 calc R . . C19 C -0.0840(6) 0.5699(5) 0.1939(3) 0.0233(13) Uani 1 1 d . . . C20 C -0.1780(6) 0.5855(5) 0.2463(3) 0.0283(15) Uani 1 1 d . . . H20 H -0.1849 0.5282 0.2762 0.034 Uiso 1 1 calc R . . C21 C -0.2601(7) 0.6844(5) 0.2540(4) 0.0339(16) Uani 1 1 d . . . H21 H -0.3237 0.6940 0.2892 0.041 Uiso 1 1 calc R . . C22 C -0.2523(7) 0.7687(5) 0.2124(4) 0.0347(17) Uani 1 1 d . . . H22 H -0.3093 0.8362 0.2187 0.042 Uiso 1 1 calc R . . C23 C -0.1602(7) 0.7545(5) 0.1607(4) 0.0334(16) Uani 1 1 d . . . H23 H -0.1548 0.8124 0.1309 0.040 Uiso 1 1 calc R . . C24 C -0.0768(6) 0.6570(5) 0.1526(3) 0.0267(14) Uani 1 1 d . . . H24 H -0.0123 0.6488 0.1178 0.032 Uiso 1 1 calc R . . C58 C -0.0415(5) 0.3549(5) 0.2327(3) 0.0219(13) Uani 1 1 d . . . C59 C 0.0226(6) 0.2945(5) 0.2884(3) 0.0289(15) Uani 1 1 d . . . H59 H 0.1022 0.2987 0.2975 0.035 Uiso 1 1 calc R . . C60 C -0.0257(7) 0.2292(6) 0.3302(4) 0.0358(17) Uani 1 1 d . . . H60 H 0.0197 0.1894 0.3680 0.043 Uiso 1 1 calc R . . C61 C -0.1405(7) 0.2212(6) 0.3175(4) 0.0348(17) Uani 1 1 d . . . H61 H -0.1743 0.1759 0.3464 0.042 Uiso 1 1 calc R . . C62 C -0.2057(6) 0.2792(6) 0.2628(4) 0.0367(18) Uani 1 1 d . . . H62 H -0.2848 0.2738 0.2541 0.044 Uiso 1 1 calc R . . C63 C -0.1578(6) 0.3455(6) 0.2204(4) 0.0335(16) Uani 1 1 d . . . H63 H -0.2038 0.3848 0.1827 0.040 Uiso 1 1 calc R . . C64 C 0.6576(6) 0.0032(5) 0.3100(3) 0.0229(13) Uani 1 1 d . . . C65 C 0.7268(6) -0.0889(5) 0.3488(3) 0.0289(15) Uani 1 1 d . . . H65 H 0.6857 -0.1138 0.3870 0.035 Uiso 1 1 calc R . . C66 C 0.8555(6) -0.1445(6) 0.3320(4) 0.0335(17) Uani 1 1 d . . . H66 H 0.9016 -0.2076 0.3585 0.040 Uiso 1 1 calc R . . C67 C 0.9168(7) -0.1084(6) 0.2769(4) 0.0408(19) Uani 1 1 d . . . H67 H 1.0048 -0.1467 0.2654 0.049 Uiso 1 1 calc R . . C68 C 0.8497(7) -0.0165(6) 0.2385(4) 0.0394(19) Uani 1 1 d . . . H68 H 0.8917 0.0088 0.2008 0.047 Uiso 1 1 calc R . . C69 C 0.7208(6) 0.0388(5) 0.2551(4) 0.0300(15) Uani 1 1 d . . . H69 H 0.6752 0.1020 0.2286 0.036 Uiso 1 1 calc R . . C70 C 0.4002(6) 0.0103(5) 0.2970(3) 0.0218(13) Uani 1 1 d . . . C71 C 0.4365(7) -0.0953(5) 0.3093(4) 0.0359(18) Uani 1 1 d . . . H71 H 0.5098 -0.1355 0.3347 0.043 Uiso 1 1 calc R . . C72 C 0.3670(7) -0.1439(6) 0.2850(5) 0.044(2) Uani 1 1 d . . . H72 H 0.3937 -0.2169 0.2934 0.053 Uiso 1 1 calc R . . C73 C 0.2604(7) -0.0868(6) 0.2491(4) 0.0407(19) Uani 1 1 d . . . H73 H 0.2134 -0.1205 0.2328 0.049 Uiso 1 1 calc R . . C74 C 0.2209(7) 0.0185(6) 0.2366(4) 0.0362(17) Uani 1 1 d . . . H74 H 0.1458 0.0580 0.2123 0.043 Uiso 1 1 calc R . . C75 C 0.2920(7) 0.0675(5) 0.2596(4) 0.0306(15) Uani 1 1 d . . . H75 H 0.2665 0.1404 0.2498 0.037 Uiso 1 1 calc R . . C76 C 0.4684(6) 0.0457(5) 0.4165(3) 0.0229(13) Uani 1 1 d . . . H76A H 0.4758 -0.0272 0.4275 0.028 Uiso 1 1 calc R . . H76B H 0.5385 0.0538 0.4378 0.028 Uiso 1 1 calc R . . C77 C 0.3362(6) 0.1156(5) 0.4413(3) 0.0211(13) Uani 1 1 d . . . H77A H 0.3326 0.1053 0.4897 0.025 Uiso 1 1 calc R . . H77B H 0.2671 0.0966 0.4274 0.025 Uiso 1 1 calc R . . C78 C 0.4001(6) 0.2879(5) 0.4624(3) 0.0233(13) Uani 1 1 d . . . C79 C 0.5207(7) 0.2914(7) 0.4377(4) 0.042(2) Uani 1 1 d . . . H79 H 0.5519 0.2744 0.3952 0.050 Uiso 1 1 calc R . . C80 C 0.5961(8) 0.3194(7) 0.4743(4) 0.048(2) Uani 1 1 d . . . H80 H 0.6787 0.3204 0.4573 0.057 Uiso 1 1 calc R . . C81 C 0.5499(8) 0.3454(6) 0.5349(4) 0.045(2) Uani 1 1 d . . . H81 H 0.6001 0.3657 0.5598 0.054 Uiso 1 1 calc R . . C82 C 0.4300(7) 0.3424(6) 0.5602(4) 0.0330(16) Uani 1 1 d . . . H82 H 0.3981 0.3607 0.6023 0.040 Uiso 1 1 calc R . . C83 C 0.3574(6) 0.3127(5) 0.5236(3) 0.0291(15) Uani 1 1 d . . . H83 H 0.2763 0.3094 0.5414 0.035 Uiso 1 1 calc R . . C84 C 0.1376(5) 0.3158(4) 0.4375(3) 0.0188(12) Uani 1 1 d . . . C85 C 0.0755(6) 0.2721(5) 0.4888(3) 0.0279(14) Uani 1 1 d . . . H85 H 0.1215 0.2058 0.5119 0.034 Uiso 1 1 calc R . . C86 C -0.0537(6) 0.3245(5) 0.5068(4) 0.0325(16) Uani 1 1 d . . . H86 H -0.0958 0.2935 0.5418 0.039 Uiso 1 1 calc R . . C87 C -0.1211(6) 0.4212(6) 0.4742(4) 0.0334(16) Uani 1 1 d . . . H87 H -0.2088 0.4574 0.4874 0.040 Uiso 1 1 calc R . . C88 C -0.0609(6) 0.4653(5) 0.4223(4) 0.0327(16) Uani 1 1 d . . . H88 H -0.1074 0.5318 0.3996 0.039 Uiso 1 1 calc R . . C89 C 0.0672(6) 0.4129(5) 0.4035(3) 0.0262(14) Uani 1 1 d . . . H89 H 0.1075 0.4429 0.3672 0.031 Uiso 1 1 calc R . . C90 C 0.8574(7) 0.1549(6) -0.0371(4) 0.0376(18) Uani 1 1 d . . . C91 C 0.9405(7) 0.1315(6) 0.0136(4) 0.0363(18) Uani 1 1 d . . . H91 H 1.0310 0.0957 0.0061 0.044 Uiso 1 1 calc R . . C92 C 0.8938(8) 0.1594(6) 0.0749(4) 0.0425(19) Uani 1 1 d . . . H92 H 0.9523 0.1431 0.1087 0.051 Uiso 1 1 calc R . . C93 C 0.7624(8) 0.2107(6) 0.0865(5) 0.047(2) Uani 1 1 d . . . H93 H 0.7302 0.2299 0.1283 0.056 Uiso 1 1 calc R . . C94 C 0.6783(7) 0.2338(6) 0.0372(5) 0.043(2) Uani 1 1 d . . . H94 H 0.5877 0.2682 0.0453 0.051 Uiso 1 1 calc R . . C95 C 0.7250(7) 0.2074(6) -0.0237(4) 0.0406(19) Uani 1 1 d . . . H95 H 0.6658 0.2251 -0.0575 0.049 Uiso 1 1 calc R . . C96 C 0.9093(8) 0.1221(7) -0.1026(4) 0.047(2) Uani 1 1 d . . . H96A H 0.9122 0.1820 -0.1340 0.071 Uiso 1 1 calc R . . H96B H 0.8524 0.0931 -0.1180 0.071 Uiso 1 1 calc R . . H96C H 0.9971 0.0698 -0.0984 0.071 Uiso 1 1 calc R . . C97 C 0.0071(12) 0.9728(10) 0.4279(5) 0.070(6) Uiso 0.50 1 d PG . . H97 H -0.0143 0.9660 0.3865 0.084 Uiso 0.50 1 calc PR . . C98 C -0.0909(8) 1.0189(10) 0.4725(6) 0.048(4) Uiso 0.50 1 d PG . . H98 H -0.1793 1.0436 0.4615 0.057 Uiso 0.50 1 calc PR . . C99 C -0.0595(9) 1.0289(9) 0.5331(6) 0.063(5) Uiso 0.50 1 d PGD . . C100 C 0.0699(11) 0.9928(10) 0.5491(5) 0.051(5) Uiso 0.50 1 d PG . . H100 H 0.0913 0.9996 0.5906 0.061 Uiso 0.50 1 calc PR . . C101 C 0.1679(8) 0.9467(10) 0.5045(7) 0.068(5) Uiso 0.50 1 d PG . . H101 H 0.2564 0.9221 0.5155 0.081 Uiso 0.50 1 calc PR . . C102 C 0.1365(10) 0.9368(9) 0.4439(6) 0.067(6) Uiso 0.50 1 d PG . . H102 H 0.2035 0.9053 0.4135 0.081 Uiso 0.50 1 calc PR . . C103 C -0.1700(14) 1.0881(13) 0.5791(8) 0.142(13) Uiso 0.50 1 d PGD . . H10A H -0.2536 1.0914 0.5658 0.213 Uiso 0.50 1 calc PR . . H10B H -0.1710 1.1582 0.5766 0.213 Uiso 0.50 1 calc PR . . H10C H -0.1557 1.0522 0.6242 0.213 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0182(7) 0.0220(8) 0.0183(9) -0.0025(6) -0.0017(6) -0.0074(6) P2 0.0191(7) 0.0187(8) 0.0203(9) -0.0036(6) -0.0027(6) -0.0053(6) P3 0.0180(7) 0.0202(8) 0.0220(9) -0.0042(7) -0.0035(6) -0.0037(6) P4 0.0207(7) 0.0184(8) 0.0183(9) -0.0029(6) -0.0015(6) -0.0051(6) P5 0.0182(7) 0.0187(8) 0.0158(9) -0.0031(6) -0.0010(6) -0.0040(6) Pd1 0.0171(2) 0.0182(2) 0.0174(3) -0.00251(18) -0.00358(17) -0.00509(18) Pd2 0.0181(2) 0.0169(2) 0.0155(3) -0.00260(18) -0.00164(17) -0.00512(18) C1 0.021(3) 0.018(3) 0.015(3) -0.001(2) -0.007(2) -0.005(2) Si1 0.0281(9) 0.0178(9) 0.0277(11) -0.0055(7) -0.0008(7) -0.0085(7) C2 0.047(4) 0.034(4) 0.047(5) -0.012(4) -0.010(4) -0.022(4) C3 0.069(6) 0.042(5) 0.062(6) -0.033(4) 0.034(5) -0.034(4) C4 0.043(4) 0.022(4) 0.050(5) -0.003(3) -0.007(4) -0.013(3) C5 0.032(3) 0.019(3) 0.020(4) -0.001(3) 0.006(3) -0.010(3) C6 0.033(4) 0.026(4) 0.028(4) -0.002(3) 0.002(3) -0.001(3) C7 0.040(4) 0.031(4) 0.044(5) -0.005(4) 0.003(4) 0.007(3) C8 0.055(5) 0.016(4) 0.060(6) -0.006(4) 0.017(4) -0.001(4) C9 0.058(5) 0.032(4) 0.053(6) -0.018(4) 0.018(4) -0.029(4) C10 0.031(4) 0.024(3) 0.039(5) -0.006(3) 0.000(3) -0.010(3) C11 0.019(3) 0.015(3) 0.024(4) 0.001(2) -0.007(2) -0.004(2) C12 0.028(3) 0.021(3) 0.023(4) -0.003(3) -0.004(3) -0.008(3) C13 0.025(3) 0.034(4) 0.026(4) -0.001(3) -0.002(3) -0.006(3) C14 0.021(3) 0.035(4) 0.030(4) 0.013(3) -0.007(3) -0.007(3) C15 0.037(4) 0.032(4) 0.046(5) 0.001(3) -0.007(3) -0.021(3) C16 0.038(4) 0.029(4) 0.025(4) -0.006(3) -0.010(3) -0.012(3) C17 0.023(3) 0.029(3) 0.018(4) -0.007(3) -0.006(2) -0.008(3) C18 0.026(3) 0.023(3) 0.025(4) -0.003(3) -0.002(3) -0.004(3) C19 0.023(3) 0.023(3) 0.024(4) -0.008(3) -0.005(2) -0.005(3) C20 0.032(3) 0.025(3) 0.024(4) -0.005(3) 0.002(3) -0.007(3) C21 0.038(4) 0.030(4) 0.026(4) -0.006(3) 0.004(3) -0.005(3) C22 0.039(4) 0.022(4) 0.041(5) -0.012(3) -0.007(3) -0.004(3) C23 0.044(4) 0.027(4) 0.034(5) -0.002(3) -0.010(3) -0.017(3) C24 0.026(3) 0.025(3) 0.029(4) -0.007(3) -0.001(3) -0.008(3) C58 0.017(3) 0.019(3) 0.030(4) -0.007(3) 0.001(2) -0.006(2) C59 0.033(3) 0.034(4) 0.026(4) -0.004(3) -0.003(3) -0.018(3) C60 0.034(4) 0.035(4) 0.037(5) 0.003(3) -0.010(3) -0.013(3) C61 0.032(4) 0.035(4) 0.037(5) -0.001(3) 0.001(3) -0.014(3) C62 0.024(3) 0.041(4) 0.047(5) 0.002(4) -0.010(3) -0.016(3) C63 0.027(3) 0.035(4) 0.034(5) 0.005(3) -0.010(3) -0.008(3) C64 0.024(3) 0.023(3) 0.022(4) -0.007(3) 0.000(2) -0.007(3) C65 0.026(3) 0.028(4) 0.025(4) -0.002(3) -0.003(3) -0.003(3) C66 0.023(3) 0.034(4) 0.039(5) -0.012(3) -0.010(3) 0.000(3) C67 0.022(3) 0.043(5) 0.053(6) -0.011(4) 0.005(3) -0.007(3) C68 0.030(4) 0.035(4) 0.050(5) -0.009(4) 0.011(3) -0.011(3) C69 0.030(3) 0.024(3) 0.031(4) -0.002(3) 0.000(3) -0.006(3) C70 0.024(3) 0.024(3) 0.018(4) -0.008(3) 0.002(2) -0.010(3) C71 0.030(4) 0.020(3) 0.059(5) -0.008(3) -0.008(3) -0.008(3) C72 0.040(4) 0.024(4) 0.070(6) -0.010(4) -0.003(4) -0.012(3) C73 0.043(4) 0.038(4) 0.051(5) -0.013(4) -0.001(4) -0.023(4) C74 0.035(4) 0.045(5) 0.031(4) 0.001(3) -0.013(3) -0.017(3) C75 0.038(4) 0.024(3) 0.031(4) -0.001(3) -0.004(3) -0.013(3) C76 0.027(3) 0.014(3) 0.019(4) -0.003(2) 0.002(2) 0.003(2) C77 0.022(3) 0.022(3) 0.016(3) -0.001(3) -0.003(2) -0.004(3) C78 0.023(3) 0.020(3) 0.025(4) -0.005(3) -0.004(3) -0.004(3) C79 0.032(4) 0.071(6) 0.033(5) -0.022(4) 0.008(3) -0.027(4) C80 0.039(4) 0.076(6) 0.038(5) -0.015(4) -0.002(4) -0.029(4) C81 0.046(4) 0.050(5) 0.046(5) -0.005(4) -0.015(4) -0.024(4) C82 0.036(4) 0.042(4) 0.023(4) -0.010(3) -0.001(3) -0.013(3) C83 0.024(3) 0.034(4) 0.030(4) -0.002(3) -0.003(3) -0.012(3) C84 0.016(3) 0.018(3) 0.020(3) -0.006(2) -0.002(2) -0.002(2) C85 0.032(3) 0.026(3) 0.021(4) 0.001(3) -0.003(3) -0.007(3) C86 0.026(3) 0.036(4) 0.031(4) -0.003(3) 0.008(3) -0.009(3) C87 0.019(3) 0.037(4) 0.038(5) -0.008(3) -0.002(3) -0.001(3) C88 0.032(4) 0.025(4) 0.033(4) -0.002(3) -0.002(3) -0.002(3) C89 0.023(3) 0.026(3) 0.027(4) -0.003(3) 0.000(3) -0.007(3) C90 0.034(4) 0.034(4) 0.044(5) 0.001(3) 0.000(3) -0.015(3) C91 0.025(3) 0.035(4) 0.051(5) -0.008(4) 0.004(3) -0.014(3) C92 0.053(5) 0.037(4) 0.041(5) -0.003(4) -0.006(4) -0.022(4) C93 0.056(5) 0.033(4) 0.050(6) -0.013(4) 0.020(4) -0.018(4) C94 0.030(4) 0.033(4) 0.064(6) -0.013(4) 0.009(4) -0.010(3) C95 0.038(4) 0.033(4) 0.054(6) 0.001(4) -0.012(4) -0.018(3) C96 0.062(5) 0.047(5) 0.029(5) 0.005(4) -0.007(4) -0.020(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 P1 C1 1.712(6) . ? P1 Pd1 2.3260(15) . ? P1 Pd2 2.3597(16) . ? P2 C5 1.818(6) . ? P2 C11 1.832(6) . ? P2 C17 1.857(6) . ? P2 Pd1 2.2804(17) . ? P3 C58 1.817(6) . ? P3 C19 1.826(6) . ? P3 C18 1.858(7) . ? P3 Pd1 2.3069(15) . ? P4 C70 1.831(6) . ? P4 C64 1.835(6) . ? P4 C76 1.848(6) . ? P4 Pd2 2.2931(16) . ? P5 C84 1.828(6) . ? P5 C78 1.839(6) . ? P5 C77 1.856(6) . ? P5 Pd2 2.3093(16) . ? Pd1 C1 2.149(6) . ? Pd1 Pd2 3.0270(7) . ? Pd2 C1 2.123(6) . ? C1 Si1 1.835(6) . ? Si1 C3 1.862(8) . ? Si1 C4 1.870(8) . ? Si1 C2 1.879(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C10 1.389(9) . ? C5 C6 1.399(9) . ? C6 C7 1.370(10) . ? C6 H6 0.9500 . ? C7 C8 1.379(12) . ? C7 H7 0.9500 . ? C8 C9 1.380(12) . ? C8 H8 0.9500 . ? C9 C10 1.393(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C16 1.387(8) . ? C11 C12 1.388(9) . ? C12 C13 1.384(9) . ? C12 H12 0.9500 . ? C13 C14 1.386(9) . ? C13 H13 0.9500 . ? C14 C15 1.372(11) . ? C14 H14 0.9500 . ? C15 C16 1.392(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.522(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.392(9) . ? C19 C20 1.409(9) . ? C20 C21 1.381(9) . ? C20 H20 0.9500 . ? C21 C22 1.366(10) . ? C21 H21 0.9500 . ? C22 C23 1.385(10) . ? C22 H22 0.9500 . ? C23 C24 1.371(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C58 C59 1.394(9) . ? C58 C63 1.403(8) . ? C59 C60 1.369(9) . ? C59 H59 0.9500 . ? C60 C61 1.380(9) . ? C60 H60 0.9500 . ? C61 C62 1.374(10) . ? C61 H61 0.9500 . ? C62 C63 1.382(9) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C69 1.387(9) . ? C64 C65 1.393(9) . ? C65 C66 1.389(9) . ? C65 H65 0.9500 . ? C66 C67 1.382(11) . ? C66 H66 0.9500 . ? C67 C68 1.382(11) . ? C67 H67 0.9500 . ? C68 C69 1.389(9) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.375(9) . ? C70 C75 1.397(9) . ? C71 C72 1.393(10) . ? C71 H71 0.9500 . ? C72 C73 1.368(11) . ? C72 H72 0.9500 . ? C73 C74 1.370(10) . ? C73 H73 0.9500 . ? C74 C75 1.398(9) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.525(8) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C83 1.368(9) . ? C78 C79 1.397(9) . ? C79 C80 1.394(10) . ? C79 H79 0.9500 . ? C80 C81 1.367(11) . ? C80 H80 0.9500 . ? C81 C82 1.389(10) . ? C81 H81 0.9500 . ? C82 C83 1.385(9) . ? C82 H82 0.9500 . ? C83 H83 0.9500 . ? C84 C85 1.383(9) . ? C84 C89 1.400(9) . ? C85 C86 1.390(9) . ? C85 H85 0.9500 . ? C86 C87 1.377(10) . ? C86 H86 0.9500 . ? C87 C88 1.381(10) . ? C87 H87 0.9500 . ? C88 C89 1.384(9) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C91 1.390(11) . ? C90 C95 1.398(10) . ? C90 C96 1.502(11) . ? C91 C92 1.391(11) . ? C91 H91 0.9500 . ? C92 C93 1.380(11) . ? C92 H92 0.9500 . ? C93 C94 1.376(12) . ? C93 H93 0.9500 . ? C94 C95 1.377(11) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C98 1.3900 . ? C97 C102 1.3900 . ? C97 H97 0.9500 . ? C98 C99 1.3900 . ? C98 H98 0.9500 . ? C99 C100 1.3900 . ? C99 C103 1.5436 . ? C100 C101 1.3900 . ? C100 H100 0.9500 . ? C101 C102 1.3900 . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? C103 H10A 0.9800 . ? C103 H10B 0.9800 . ? C103 H10C 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 C1 P1 Pd1 62.12(19) . . ? C1 P1 Pd2 60.4(2) . . ? Pd1 P1 Pd2 80.48(5) . . ? C5 P2 C11 103.1(3) . . ? C5 P2 C17 104.3(3) . . ? C11 P2 C17 102.4(3) . . ? C5 P2 Pd1 122.6(2) . . ? C11 P2 Pd1 114.0(2) . . ? C17 P2 Pd1 108.3(2) . . ? C58 P3 C19 104.0(3) . . ? C58 P3 C18 103.5(3) . . ? C19 P3 C18 100.5(3) . . ? C58 P3 Pd1 111.5(2) . . ? C19 P3 Pd1 129.4(2) . . ? C18 P3 Pd1 104.8(2) . . ? C70 P4 C64 102.8(3) . . ? C70 P4 C76 101.9(3) . . ? C64 P4 C76 101.9(3) . . ? C70 P4 Pd2 115.6(2) . . ? C64 P4 Pd2 124.7(2) . . ? C76 P4 Pd2 106.90(19) . . ? C84 P5 C78 103.8(3) . . ? C84 P5 C77 101.7(3) . . ? C78 P5 C77 103.4(3) . . ? C84 P5 Pd2 128.7(2) . . ? C78 P5 Pd2 110.6(2) . . ? C77 P5 Pd2 105.8(2) . . ? C1 Pd1 P2 153.49(16) . . ? C1 Pd1 P3 119.95(16) . . ? P2 Pd1 P3 86.40(6) . . ? C1 Pd1 P1 44.77(16) . . ? P2 Pd1 P1 108.83(6) . . ? P3 Pd1 P1 164.72(6) . . ? C1 Pd1 Pd2 44.53(16) . . ? P2 Pd1 Pd2 125.91(4) . . ? P3 Pd1 Pd2 121.68(5) . . ? P1 Pd1 Pd2 50.25(4) . . ? C1 Pd2 P4 159.95(17) . . ? C1 Pd2 P5 113.08(17) . . ? P4 Pd2 P5 86.91(6) . . ? C1 Pd2 P1 44.52(17) . . ? P4 Pd2 P1 115.52(6) . . ? P5 Pd2 P1 155.86(6) . . ? C1 Pd2 Pd1 45.22(15) . . ? P4 Pd2 Pd1 124.33(5) . . ? P5 Pd2 Pd1 126.08(4) . . ? P1 Pd2 Pd1 49.27(4) . . ? P1 C1 Si1 128.4(3) . . ? P1 C1 Pd2 75.1(2) . . ? Si1 C1 Pd2 136.5(3) . . ? P1 C1 Pd1 73.1(2) . . ? Si1 C1 Pd1 129.1(3) . . ? Pd2 C1 Pd1 90.2(2) . . ? C1 Si1 C3 117.4(3) . . ? C1 Si1 C4 108.9(3) . . ? C3 Si1 C4 105.2(4) . . ? C1 Si1 C2 110.0(3) . . ? C3 Si1 C2 106.3(4) . . ? C4 Si1 C2 108.7(3) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.8(6) . . ? C10 C5 P2 123.3(5) . . ? C6 C5 P2 117.9(5) . . ? C7 C6 C5 120.5(7) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.2(8) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.6(7) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 119.2(7) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C5 C10 C9 120.6(7) . . ? C5 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C16 C11 C12 119.0(6) . . ? C16 C11 P2 118.8(5) . . ? C12 C11 P2 122.2(4) . . ? C13 C12 C11 121.4(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 118.6(7) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 121.0(6) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.0(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.0(7) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 P2 109.4(4) . . ? C18 C17 H17A 109.8 . . ? P2 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? P2 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C17 C18 P3 109.9(4) . . ? C17 C18 H18A 109.7 . . ? P3 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? P3 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C24 C19 C20 117.4(6) . . ? C24 C19 P3 120.5(5) . . ? C20 C19 P3 122.1(5) . . ? C21 C20 C19 119.8(6) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 121.7(7) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 119.0(6) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 120.1(7) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 121.8(6) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? C59 C58 C63 117.4(6) . . ? C59 C58 P3 118.5(4) . . ? C63 C58 P3 124.1(5) . . ? C60 C59 C58 121.8(6) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? C59 C60 C61 120.0(7) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 119.6(7) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C63 120.9(6) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C62 C63 C58 120.3(6) . . ? C62 C63 H63 119.8 . . ? C58 C63 H63 119.8 . . ? C69 C64 C65 118.6(6) . . ? C69 C64 P4 117.7(5) . . ? C65 C64 P4 123.7(5) . . ? C66 C65 C64 120.5(7) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C67 C66 C65 120.2(7) . . ? C67 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? C68 C67 C66 119.8(7) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C67 C68 C69 120.0(7) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C64 C69 C68 120.9(7) . . ? C64 C69 H69 119.5 . . ? C68 C69 H69 119.5 . . ? C71 C70 C75 118.4(6) . . ? C71 C70 P4 123.6(5) . . ? C75 C70 P4 118.0(5) . . ? C70 C71 C72 120.7(7) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C73 C72 C71 120.3(7) . . ? C73 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? C72 C73 C74 120.5(7) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C73 C74 C75 119.4(7) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C70 C75 C74 120.6(6) . . ? C70 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C77 C76 P4 109.4(4) . . ? C77 C76 H76A 109.8 . . ? P4 C76 H76A 109.8 . . ? C77 C76 H76B 109.8 . . ? P4 C76 H76B 109.8 . . ? H76A C76 H76B 108.2 . . ? C76 C77 P5 111.2(4) . . ? C76 C77 H77A 109.4 . . ? P5 C77 H77A 109.4 . . ? C76 C77 H77B 109.4 . . ? P5 C77 H77B 109.4 . . ? H77A C77 H77B 108.0 . . ? C83 C78 C79 118.4(6) . . ? C83 C78 P5 124.1(5) . . ? C79 C78 P5 117.5(5) . . ? C80 C79 C78 120.9(7) . . ? C80 C79 H79 119.5 . . ? C78 C79 H79 119.5 . . ? C81 C80 C79 119.3(7) . . ? C81 C80 H80 120.3 . . ? C79 C80 H80 120.3 . . ? C80 C81 C82 120.5(7) . . ? C80 C81 H81 119.8 . . ? C82 C81 H81 119.8 . . ? C83 C82 C81 119.5(7) . . ? C83 C82 H82 120.3 . . ? C81 C82 H82 120.3 . . ? C78 C83 C82 121.4(6) . . ? C78 C83 H83 119.3 . . ? C82 C83 H83 119.3 . . ? C85 C84 C89 118.7(5) . . ? C85 C84 P5 124.1(5) . . ? C89 C84 P5 117.2(5) . . ? C84 C85 C86 120.5(6) . . ? C84 C85 H85 119.8 . . ? C86 C85 H85 119.8 . . ? C87 C86 C85 120.4(6) . . ? C87 C86 H86 119.8 . . ? C85 C86 H86 119.8 . . ? C86 C87 C88 119.8(6) . . ? C86 C87 H87 120.1 . . ? C88 C87 H87 120.1 . . ? C87 C88 C89 120.1(7) . . ? C87 C88 H88 119.9 . . ? C89 C88 H88 119.9 . . ? C88 C89 C84 120.5(6) . . ? C88 C89 H89 119.8 . . ? C84 C89 H89 119.8 . . ? C91 C90 C95 117.2(8) . . ? C91 C90 C96 120.5(7) . . ? C95 C90 C96 122.2(7) . . ? C90 C91 C92 121.3(7) . . ? C90 C91 H91 119.3 . . ? C92 C91 H91 119.3 . . ? C93 C92 C91 120.0(8) . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C94 C93 C92 119.7(8) . . ? C94 C93 H93 120.2 . . ? C92 C93 H93 120.2 . . ? C93 C94 C95 120.3(7) . . ? C93 C94 H94 119.9 . . ? C95 C94 H94 119.9 . . ? C94 C95 C90 121.6(8) . . ? C94 C95 H95 119.2 . . ? C90 C95 H95 119.2 . . ? C90 C96 H96A 109.5 . . ? C90 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C90 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C98 C97 C102 120.0 . . ? C98 C97 H97 120.0 . . ? C102 C97 H97 120.0 . . ? C99 C98 C97 120.0 . . ? C99 C98 H98 120.0 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 120.0 . . ? C98 C99 C103 118.5 . . ? C100 C99 C103 121.3 . . ? C101 C100 C99 120.0 . . ? C101 C100 H100 120.0 . . ? C99 C100 H100 120.0 . . ? C100 C101 C102 120.0 . . ? C100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C101 C102 C97 120.0 . . ? C101 C102 H102 120.0 . . ? C97 C102 H102 120.0 . . ? C99 C103 H10A 109.5 . . ? C99 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C99 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 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 C5 P2 Pd1 C1 60.8(4) . . . . ? C11 P2 Pd1 C1 -64.7(4) . . . . ? C17 P2 Pd1 C1 -177.9(4) . . . . ? C5 P2 Pd1 P3 -125.1(2) . . . . ? C11 P2 Pd1 P3 109.5(2) . . . . ? C17 P2 Pd1 P3 -3.8(2) . . . . ? C5 P2 Pd1 P1 56.2(2) . . . . ? C11 P2 Pd1 P1 -69.3(2) . . . . ? C17 P2 Pd1 P1 177.4(2) . . . . ? C5 P2 Pd1 Pd2 2.1(2) . . . . ? C11 P2 Pd1 Pd2 -123.4(2) . . . . ? C17 P2 Pd1 Pd2 123.4(2) . . . . ? C58 P3 Pd1 C1 -90.9(3) . . . . ? C19 P3 Pd1 C1 40.4(3) . . . . ? C18 P3 Pd1 C1 157.8(3) . . . . ? C58 P3 Pd1 P2 92.1(2) . . . . ? C19 P3 Pd1 P2 -136.6(3) . . . . ? C18 P3 Pd1 P2 -19.2(2) . . . . ? C58 P3 Pd1 P1 -92.3(3) . . . . ? C19 P3 Pd1 P1 39.0(4) . . . . ? C18 P3 Pd1 P1 156.4(3) . . . . ? C58 P3 Pd1 Pd2 -38.6(2) . . . . ? C19 P3 Pd1 Pd2 92.7(3) . . . . ? C18 P3 Pd1 Pd2 -149.9(2) . . . . ? Pd2 P1 Pd1 C1 61.4(2) . . . . ? C1 P1 Pd1 P2 177.1(2) . . . . ? Pd2 P1 Pd1 P2 -121.49(5) . . . . ? C1 P1 Pd1 P3 1.6(3) . . . . ? Pd2 P1 Pd1 P3 63.1(2) . . . . ? C1 P1 Pd1 Pd2 -61.4(2) . . . . ? C70 P4 Pd2 C1 -84.9(5) . . . . ? C64 P4 Pd2 C1 44.2(5) . . . . ? C76 P4 Pd2 C1 162.4(5) . . . . ? C70 P4 Pd2 P5 99.6(2) . . . . ? C64 P4 Pd2 P5 -131.2(3) . . . . ? C76 P4 Pd2 P5 -13.0(2) . . . . ? C70 P4 Pd2 P1 -89.7(2) . . . . ? C64 P4 Pd2 P1 39.5(3) . . . . ? C76 P4 Pd2 P1 157.7(2) . . . . ? C70 P4 Pd2 Pd1 -33.0(2) . . . . ? C64 P4 Pd2 Pd1 96.1(3) . . . . ? C76 P4 Pd2 Pd1 -145.7(2) . . . . ? C84 P5 Pd2 C1 52.2(3) . . . . ? C78 P5 Pd2 C1 -76.6(3) . . . . ? C77 P5 Pd2 C1 172.0(2) . . . . ? C84 P5 Pd2 P4 -129.5(2) . . . . ? C78 P5 Pd2 P4 101.7(2) . . . . ? C77 P5 Pd2 P4 -9.7(2) . . . . ? C84 P5 Pd2 P1 71.4(3) . . . . ? C78 P5 Pd2 P1 -57.4(3) . . . . ? C77 P5 Pd2 P1 -168.8(2) . . . . ? C84 P5 Pd2 Pd1 1.7(3) . . . . ? C78 P5 Pd2 Pd1 -127.1(2) . . . . ? C77 P5 Pd2 Pd1 121.55(19) . . . . ? Pd1 P1 Pd2 C1 -63.2(2) . . . . ? C1 P1 Pd2 P4 177.7(2) . . . . ? Pd1 P1 Pd2 P4 114.43(6) . . . . ? C1 P1 Pd2 P5 -25.5(3) . . . . ? Pd1 P1 Pd2 P5 -88.79(13) . . . . ? C1 P1 Pd2 Pd1 63.2(2) . . . . ? P2 Pd1 Pd2 C1 147.1(2) . . . . ? P3 Pd1 Pd2 C1 -102.1(2) . . . . ? P1 Pd1 Pd2 C1 61.9(2) . . . . ? C1 Pd1 Pd2 P4 -157.6(2) . . . . ? P2 Pd1 Pd2 P4 -10.57(7) . . . . ? P3 Pd1 Pd2 P4 100.27(7) . . . . ? P1 Pd1 Pd2 P4 -95.76(7) . . . . ? C1 Pd1 Pd2 P5 87.7(2) . . . . ? P2 Pd1 Pd2 P5 -125.20(7) . . . . ? P3 Pd1 Pd2 P5 -14.36(7) . . . . ? P1 Pd1 Pd2 P5 149.61(7) . . . . ? C1 Pd1 Pd2 P1 -61.9(2) . . . . ? P2 Pd1 Pd2 P1 85.18(7) . . . . ? P3 Pd1 Pd2 P1 -163.97(7) . . . . ? Pd1 P1 C1 Si1 -126.8(5) . . . . ? Pd2 P1 C1 Si1 138.2(5) . . . . ? Pd1 P1 C1 Pd2 94.91(15) . . . . ? Pd2 P1 C1 Pd1 -94.91(15) . . . . ? P4 Pd2 C1 P1 -6.1(6) . . . . ? P5 Pd2 C1 P1 168.95(11) . . . . ? Pd1 Pd2 C1 P1 -72.4(2) . . . . ? P4 Pd2 C1 Si1 -136.8(4) . . . . ? P5 Pd2 C1 Si1 38.3(5) . . . . ? P1 Pd2 C1 Si1 -130.7(5) . . . . ? Pd1 Pd2 C1 Si1 156.9(6) . . . . ? P4 Pd2 C1 Pd1 66.3(5) . . . . ? P5 Pd2 C1 Pd1 -118.62(15) . . . . ? P1 Pd2 C1 Pd1 72.4(2) . . . . ? P2 Pd1 C1 P1 -6.2(5) . . . . ? P3 Pd1 C1 P1 -179.50(10) . . . . ? Pd2 Pd1 C1 P1 74.3(2) . . . . ? P2 Pd1 C1 Si1 119.9(4) . . . . ? P3 Pd1 C1 Si1 -53.4(4) . . . . ? P1 Pd1 C1 Si1 126.1(5) . . . . ? Pd2 Pd1 C1 Si1 -159.6(5) . . . . ? P2 Pd1 C1 Pd2 -80.5(4) . . . . ? P3 Pd1 C1 Pd2 106.17(17) . . . . ? P1 Pd1 C1 Pd2 -74.3(2) . . . . ? P1 C1 Si1 C3 -170.5(5) . . . . ? Pd2 C1 Si1 C3 -59.6(6) . . . . ? Pd1 C1 Si1 C3 90.0(5) . . . . ? P1 C1 Si1 C4 70.2(5) . . . . ? Pd2 C1 Si1 C4 -178.9(4) . . . . ? Pd1 C1 Si1 C4 -29.3(5) . . . . ? P1 C1 Si1 C2 -48.9(5) . . . . ? Pd2 C1 Si1 C2 62.0(5) . . . . ? Pd1 C1 Si1 C2 -148.4(4) . . . . ? C11 P2 C5 C10 -86.4(6) . . . . ? C17 P2 C5 C10 20.3(6) . . . . ? Pd1 P2 C5 C10 143.4(5) . . . . ? C11 P2 C5 C6 94.1(5) . . . . ? C17 P2 C5 C6 -159.2(5) . . . . ? Pd1 P2 C5 C6 -36.1(6) . . . . ? C10 C5 C6 C7 1.2(10) . . . . ? P2 C5 C6 C7 -179.3(6) . . . . ? C5 C6 C7 C8 -1.8(12) . . . . ? C6 C7 C8 C9 2.2(13) . . . . ? C7 C8 C9 C10 -1.9(12) . . . . ? C6 C5 C10 C9 -0.9(10) . . . . ? P2 C5 C10 C9 179.6(5) . . . . ? C8 C9 C10 C5 1.3(11) . . . . ? C5 P2 C11 C16 -144.8(5) . . . . ? C17 P2 C11 C16 107.1(5) . . . . ? Pd1 P2 C11 C16 -9.6(5) . . . . ? C5 P2 C11 C12 34.8(6) . . . . ? C17 P2 C11 C12 -73.3(5) . . . . ? Pd1 P2 C11 C12 170.0(4) . . . . ? C16 C11 C12 C13 1.1(9) . . . . ? P2 C11 C12 C13 -178.5(5) . . . . ? C11 C12 C13 C14 -0.9(9) . . . . ? C12 C13 C14 C15 0.6(10) . . . . ? C13 C14 C15 C16 -0.3(10) . . . . ? C12 C11 C16 C15 -0.8(9) . . . . ? P2 C11 C16 C15 178.8(5) . . . . ? C14 C15 C16 C11 0.4(10) . . . . ? C5 P2 C17 C18 164.3(5) . . . . ? C11 P2 C17 C18 -88.5(5) . . . . ? Pd1 P2 C17 C18 32.2(5) . . . . ? P2 C17 C18 P3 -50.0(5) . . . . ? C58 P3 C18 C17 -71.8(5) . . . . ? C19 P3 C18 C17 -179.2(4) . . . . ? Pd1 P3 C18 C17 45.1(4) . . . . ? C58 P3 C19 C24 -167.0(5) . . . . ? C18 P3 C19 C24 -60.1(6) . . . . ? Pd1 P3 C19 C24 59.1(6) . . . . ? C58 P3 C19 C20 15.0(6) . . . . ? C18 P3 C19 C20 121.9(5) . . . . ? Pd1 P3 C19 C20 -118.9(5) . . . . ? C24 C19 C20 C21 1.4(9) . . . . ? P3 C19 C20 C21 179.4(5) . . . . ? C19 C20 C21 C22 -0.6(11) . . . . ? C20 C21 C22 C23 0.5(11) . . . . ? C21 C22 C23 C24 -1.2(10) . . . . ? C22 C23 C24 C19 2.1(10) . . . . ? C20 C19 C24 C23 -2.1(9) . . . . ? P3 C19 C24 C23 179.8(5) . . . . ? C19 P3 C58 C59 -110.4(5) . . . . ? C18 P3 C58 C59 145.0(5) . . . . ? Pd1 P3 C58 C59 32.9(6) . . . . ? C19 P3 C58 C63 69.0(6) . . . . ? C18 P3 C58 C63 -35.7(6) . . . . ? Pd1 P3 C58 C63 -147.8(5) . . . . ? C63 C58 C59 C60 -0.8(10) . . . . ? P3 C58 C59 C60 178.6(6) . . . . ? C58 C59 C60 C61 0.6(11) . . . . ? C59 C60 C61 C62 -0.2(12) . . . . ? C60 C61 C62 C63 0.0(12) . . . . ? C61 C62 C63 C58 -0.3(11) . . . . ? C59 C58 C63 C62 0.7(10) . . . . ? P3 C58 C63 C62 -178.7(6) . . . . ? C70 P4 C64 C69 101.2(5) . . . . ? C76 P4 C64 C69 -153.5(5) . . . . ? Pd2 P4 C64 C69 -33.0(6) . . . . ? C70 P4 C64 C65 -78.4(6) . . . . ? C76 P4 C64 C65 26.9(6) . . . . ? Pd2 P4 C64 C65 147.4(5) . . . . ? C69 C64 C65 C66 -1.3(10) . . . . ? P4 C64 C65 C66 178.3(5) . . . . ? C64 C65 C66 C67 0.7(10) . . . . ? C65 C66 C67 C68 0.2(11) . . . . ? C66 C67 C68 C69 -0.5(12) . . . . ? C65 C64 C69 C68 1.0(10) . . . . ? P4 C64 C69 C68 -178.7(6) . . . . ? C67 C68 C69 C64 -0.1(11) . . . . ? C64 P4 C70 C71 44.2(7) . . . . ? C76 P4 C70 C71 -61.1(6) . . . . ? Pd2 P4 C70 C71 -176.6(5) . . . . ? C64 P4 C70 C75 -135.5(5) . . . . ? C76 P4 C70 C75 119.1(5) . . . . ? Pd2 P4 C70 C75 3.6(6) . . . . ? C75 C70 C71 C72 0.0(11) . . . . ? P4 C70 C71 C72 -179.8(6) . . . . ? C70 C71 C72 C73 -0.8(13) . . . . ? C71 C72 C73 C74 0.1(13) . . . . ? C72 C73 C74 C75 1.3(12) . . . . ? C71 C70 C75 C74 1.4(10) . . . . ? P4 C70 C75 C74 -178.8(5) . . . . ? C73 C74 C75 C70 -2.0(11) . . . . ? C70 P4 C76 C77 -82.7(5) . . . . ? C64 P4 C76 C77 171.3(4) . . . . ? Pd2 P4 C76 C77 39.1(5) . . . . ? P4 C76 C77 P5 -49.5(5) . . . . ? C84 P5 C77 C76 173.2(4) . . . . ? C78 P5 C77 C76 -79.4(5) . . . . ? Pd2 P5 C77 C76 36.9(5) . . . . ? C84 P5 C78 C83 25.1(6) . . . . ? C77 P5 C78 C83 -80.7(6) . . . . ? Pd2 P5 C78 C83 166.3(5) . . . . ? C84 P5 C78 C79 -153.2(6) . . . . ? C77 P5 C78 C79 100.9(6) . . . . ? Pd2 P5 C78 C79 -12.0(6) . . . . ? C83 C78 C79 C80 0.0(12) . . . . ? P5 C78 C79 C80 178.4(7) . . . . ? C78 C79 C80 C81 -1.1(13) . . . . ? C79 C80 C81 C82 1.0(13) . . . . ? C80 C81 C82 C83 0.1(12) . . . . ? C79 C78 C83 C82 1.2(11) . . . . ? P5 C78 C83 C82 -177.1(5) . . . . ? C81 C82 C83 C78 -1.2(11) . . . . ? C78 P5 C84 C85 -86.1(6) . . . . ? C77 P5 C84 C85 21.1(6) . . . . ? Pd2 P5 C84 C85 142.6(5) . . . . ? C78 P5 C84 C89 95.6(5) . . . . ? C77 P5 C84 C89 -157.3(5) . . . . ? Pd2 P5 C84 C89 -35.8(6) . . . . ? C89 C84 C85 C86 -1.1(10) . . . . ? P5 C84 C85 C86 -179.4(5) . . . . ? C84 C85 C86 C87 -0.8(11) . . . . ? C85 C86 C87 C88 1.5(11) . . . . ? C86 C87 C88 C89 -0.5(11) . . . . ? C87 C88 C89 C84 -1.3(10) . . . . ? C85 C84 C89 C88 2.1(9) . . . . ? P5 C84 C89 C88 -179.5(5) . . . . ? C95 C90 C91 C92 -0.2(10) . . . . ? C96 C90 C91 C92 -178.6(7) . . . . ? C90 C91 C92 C93 0.5(11) . . . . ? C91 C92 C93 C94 0.1(11) . . . . ? C92 C93 C94 C95 -1.0(11) . . . . ? C93 C94 C95 C90 1.2(11) . . . . ? C91 C90 C95 C94 -0.6(11) . . . . ? C96 C90 C95 C94 177.7(7) . . . . ? C102 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C100 0.0 . . . . ? C97 C98 C99 C103 175.2 . . . . ? C98 C99 C100 C101 0.0 . . . . ? C103 C99 C100 C101 -175.1 . . . . ? C99 C100 C101 C102 0.0 . . . . ? C100 C101 C102 C97 0.0 . . . . ? C98 C97 C102 C101 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.187 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.160 data_9 _database_code_depnum_ccdc_archive 'CCDC 894372' #TrackingRef 'Phosphaalkynes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H102 P8 Pd5 Si3, 2(C7 H8)' _chemical_formula_sum 'C116 H118 P8 Pd5 Si3' _chemical_formula_weight 2376.13 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.936(2) _cell_length_b 15.000(2) _cell_length_c 27.470(4) _cell_angle_alpha 87.751(8) _cell_angle_beta 80.249(7) _cell_angle_gamma 71.765(7) _cell_volume 5760.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36905 _cell_measurement_theta_min 2.794 _cell_measurement_theta_max 28.289 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631123 _exptl_absorpt_correction_T_max 0.858575 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Kappa-APEX-II area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94768 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.41 _reflns_number_total 28377 _reflns_number_gt 21905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (Bruker, 2004)' _computing_cell_refinement 'APEX-II and SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT v7.51A (BRUKER)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+2.5597P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28377 _refine_ls_number_parameters 1314 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _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 Pd1 Pd 0.64292(2) 0.40253(2) 0.283019(10) 0.02337(8) Uani 1 1 d . A . Pd2 Pd 0.56187(2) 0.30009(2) 0.242596(10) 0.02502(8) Uani 1 1 d . A . Pd3 Pd 0.43616(2) 0.45578(2) 0.306095(10) 0.02464(8) Uani 1 1 d . A . Pd4 Pd 0.67359(2) 0.39549(2) 0.176392(11) 0.02882(8) Uani 1 1 d . A . Pd5 Pd 0.69654(2) 0.20465(2) 0.307069(10) 0.02494(8) Uani 1 1 d . A . P1 P 0.71496(7) 0.49411(7) 0.31698(4) 0.0254(2) Uani 1 1 d . . . P2 P 0.49294(8) 0.20881(8) 0.20628(4) 0.0325(2) Uani 1 1 d . . . P3 P 0.29550(7) 0.57833(7) 0.30776(4) 0.0249(2) Uani 1 1 d . . . P4 P 0.78554(8) 0.36601(10) 0.10545(4) 0.0419(3) Uani 1 1 d . . . P5 P 0.70756(7) 0.09398(7) 0.36891(4) 0.0244(2) Uani 1 1 d . . . P6 P 0.52120(8) 0.47141(8) 0.23019(4) 0.0297(2) Uani 1 1 d . . . P7 P 0.73718(8) 0.27341(8) 0.22653(4) 0.0307(2) Uani 1 1 d . . . P8 P 0.55072(7) 0.31340(7) 0.33366(4) 0.0259(2) Uani 1 1 d . . . Si1 Si 0.50328(9) 0.61492(10) 0.13603(5) 0.0386(3) Uani 1 1 d . . . Si2 Si 0.38296(8) 0.36121(8) 0.43159(4) 0.0290(2) Uani 1 1 d . . . Si3 Si 0.93308(9) 0.09508(9) 0.22907(5) 0.0373(3) Uani 1 1 d . . . C1 C 0.7867(3) 0.5507(3) 0.27298(15) 0.0292(8) Uani 1 1 d . . . C2 C 0.8734(3) 0.5580(3) 0.28071(16) 0.0358(10) Uani 1 1 d . . . H2 H 0.8990 0.5312 0.3092 0.043 Uiso 1 1 calc R . . C3 C 0.9230(3) 0.6040(4) 0.24736(18) 0.0429(11) Uani 1 1 d . . . H3 H 0.9827 0.6080 0.2529 0.052 Uiso 1 1 calc R . . C4 C 0.8863(4) 0.6443(3) 0.20574(18) 0.0434(11) Uani 1 1 d . . . H4 H 0.9198 0.6772 0.1832 0.052 Uiso 1 1 calc R . . C5 C 0.8005(4) 0.6361(3) 0.19740(18) 0.0428(11) Uani 1 1 d . . . H5 H 0.7754 0.6626 0.1687 0.051 Uiso 1 1 calc R . . C6 C 0.7510(3) 0.5893(3) 0.23078(16) 0.0364(10) Uani 1 1 d . . . H6 H 0.6923 0.5836 0.2247 0.044 Uiso 1 1 calc R . . C7 C 0.7982(3) 0.4355(3) 0.35853(14) 0.0293(8) Uani 1 1 d . . . C8 C 0.8626(3) 0.3472(3) 0.34468(18) 0.0406(11) Uani 1 1 d . . . H8 H 0.8596 0.3179 0.3152 0.049 Uiso 1 1 calc R . . C9 C 0.9310(4) 0.3016(4) 0.37324(19) 0.0489(13) Uani 1 1 d . . . H9 H 0.9749 0.2418 0.3630 0.059 Uiso 1 1 calc R . . C10 C 0.9356(4) 0.3427(4) 0.41672(18) 0.0457(12) Uani 1 1 d . . . H10 H 0.9827 0.3116 0.4363 0.055 Uiso 1 1 calc R . . C11 C 0.8706(4) 0.4300(4) 0.43135(17) 0.0439(11) Uani 1 1 d . . . H11 H 0.8726 0.4581 0.4614 0.053 Uiso 1 1 calc R . . C12 C 0.8028(3) 0.4765(3) 0.40251(15) 0.0355(9) Uani 1 1 d . . . H12 H 0.7593 0.5364 0.4127 0.043 Uiso 1 1 calc R . . C13 C 0.6338(3) 0.5939(3) 0.35465(14) 0.0280(8) Uani 1 1 d . . . C14 C 0.5562(3) 0.5796(3) 0.38557(15) 0.0330(9) Uani 1 1 d . . . H14 H 0.5451 0.5206 0.3859 0.040 Uiso 1 1 calc R . . C15 C 0.4942(3) 0.6537(3) 0.41636(16) 0.0389(10) Uani 1 1 d . . . H15 H 0.4413 0.6439 0.4379 0.047 Uiso 1 1 calc R . . C16 C 0.5083(4) 0.7401(3) 0.41609(17) 0.0425(11) Uani 1 1 d . . . H16 H 0.4658 0.7893 0.4373 0.051 Uiso 1 1 calc R . . C17 C 0.5848(4) 0.7546(3) 0.38463(19) 0.0448(12) Uani 1 1 d . . . H17 H 0.5943 0.8144 0.3837 0.054 Uiso 1 1 calc R . . C18 C 0.6487(3) 0.6809(3) 0.35397(18) 0.0401(10) Uani 1 1 d . . . H18 H 0.7020 0.6906 0.3328 0.048 Uiso 1 1 calc R . . C19 C 0.5217(8) 0.1391(5) 0.1090(2) 0.110(4) Uani 1 1 d . . . H19 H 0.5261 0.0794 0.1231 0.132 Uiso 1 1 calc R . . C20 C 0.5330(11) 0.1490(6) 0.0574(3) 0.167(6) Uani 1 1 d . . . H20 H 0.5492 0.0954 0.0365 0.201 Uiso 1 1 calc R . . C21 C 0.5206(9) 0.2355(5) 0.0374(2) 0.127(4) Uani 1 1 d . . . H21 H 0.5217 0.2427 0.0028 0.152 Uiso 1 1 calc R . . C22 C 0.5069(5) 0.3107(5) 0.0658(2) 0.0665(18) Uani 1 1 d . . . H22 H 0.5035 0.3698 0.0511 0.080 Uiso 1 1 calc R . . C23 C 0.4977(4) 0.3021(4) 0.11660(18) 0.0463(12) Uani 1 1 d . . . H23 H 0.4867 0.3561 0.1365 0.056 Uiso 1 1 calc R . . C24 C 0.5043(4) 0.2162(4) 0.13915(17) 0.0459(12) Uani 1 1 d . . . C25 C 0.3646(3) 0.2338(3) 0.22675(19) 0.0416(11) Uani 1 1 d . . . C26 C 0.3275(4) 0.2618(4) 0.2756(2) 0.0470(12) Uani 1 1 d . . . H26 H 0.3685 0.2694 0.2970 0.056 Uiso 1 1 calc R . . C27 C 0.2302(4) 0.2788(4) 0.2935(3) 0.0669(17) Uani 1 1 d . . . H27 H 0.2051 0.2964 0.3271 0.080 Uiso 1 1 calc R . . C28 C 0.1713(5) 0.2698(5) 0.2621(3) 0.082(2) Uani 1 1 d . . . H28 H 0.1050 0.2824 0.2742 0.099 Uiso 1 1 calc R . . C29 C 0.2050(5) 0.2437(5) 0.2145(3) 0.076(2) Uani 1 1 d . . . H29 H 0.1630 0.2377 0.1934 0.092 Uiso 1 1 calc R . . C30 C 0.3015(4) 0.2256(4) 0.1965(3) 0.0612(16) Uani 1 1 d . . . H30 H 0.3251 0.2073 0.1629 0.073 Uiso 1 1 calc R . . C31 C 0.5400(3) 0.0817(3) 0.21553(15) 0.0352(10) Uani 1 1 d . . . C32 C 0.4837(4) 0.0224(3) 0.21777(19) 0.0449(11) Uani 1 1 d . . . H32 H 0.4178 0.0481 0.2156 0.054 Uiso 1 1 calc R . . C33 C 0.5228(4) -0.0737(4) 0.2231(2) 0.0546(14) Uani 1 1 d . . . H33 H 0.4840 -0.1135 0.2243 0.066 Uiso 1 1 calc R . . C34 C 0.6192(5) -0.1114(4) 0.2266(2) 0.0551(14) Uani 1 1 d . . . H34 H 0.6465 -0.1772 0.2299 0.066 Uiso 1 1 calc R . . C35 C 0.6743(4) -0.0542(4) 0.22516(19) 0.0529(14) Uani 1 1 d . . . H35 H 0.7399 -0.0803 0.2280 0.063 Uiso 1 1 calc R . . C36 C 0.6354(4) 0.0435(3) 0.21954(17) 0.0409(11) Uani 1 1 d . . . H36 H 0.6746 0.0828 0.2185 0.049 Uiso 1 1 calc R . . C37 C 0.1903(3) 0.5862(3) 0.35482(15) 0.0304(9) Uani 1 1 d . . . C38 C 0.1824(4) 0.6265(3) 0.40113(16) 0.0424(11) Uani 1 1 d . . . H38 H 0.2302 0.6521 0.4072 0.051 Uiso 1 1 calc R . . C39 C 0.1066(5) 0.6295(4) 0.4378(2) 0.0597(16) Uani 1 1 d . . . H39 H 0.1015 0.6580 0.4688 0.072 Uiso 1 1 calc R . . C40 C 0.0383(4) 0.5913(4) 0.4295(2) 0.0657(19) Uani 1 1 d . . . H40 H -0.0142 0.5934 0.4548 0.079 Uiso 1 1 calc R . . C41 C 0.0459(4) 0.5500(4) 0.3844(2) 0.0600(16) Uani 1 1 d . . . H41 H -0.0010 0.5224 0.3791 0.072 Uiso 1 1 calc R . . C42 C 0.1213(3) 0.5479(4) 0.34651(18) 0.0405(11) Uani 1 1 d . . . H42 H 0.1252 0.5206 0.3153 0.049 Uiso 1 1 calc R . . C43 C 0.2433(3) 0.5837(3) 0.25148(15) 0.0305(9) Uani 1 1 d . . . C44 C 0.2724(4) 0.5042(3) 0.22217(17) 0.0418(11) Uani 1 1 d . . . H44 H 0.3192 0.4496 0.2309 0.050 Uiso 1 1 calc R . . C45 C 0.2332(5) 0.5036(4) 0.1795(2) 0.0635(17) Uani 1 1 d . . . H45 H 0.2539 0.4485 0.1594 0.076 Uiso 1 1 calc R . . C46 C 0.1659(4) 0.5812(4) 0.1665(2) 0.0570(15) Uani 1 1 d . . . H46 H 0.1390 0.5798 0.1377 0.068 Uiso 1 1 calc R . . C47 C 0.1366(3) 0.6619(4) 0.19534(18) 0.0462(12) Uani 1 1 d . . . H47 H 0.0909 0.7166 0.1857 0.055 Uiso 1 1 calc R . . C48 C 0.1733(3) 0.6638(3) 0.23813(16) 0.0360(10) Uani 1 1 d . . . H48 H 0.1514 0.7188 0.2584 0.043 Uiso 1 1 calc R . . C49 C 0.3098(3) 0.6947(3) 0.31194(15) 0.0308(9) Uani 1 1 d . . . C50 C 0.4009(3) 0.7014(3) 0.30255(17) 0.0380(10) Uani 1 1 d . . . H50 H 0.4540 0.6465 0.2946 0.046 Uiso 1 1 calc R . . C51 C 0.4159(4) 0.7892(4) 0.3047(2) 0.0497(13) Uani 1 1 d . . . H51 H 0.4791 0.7929 0.2984 0.060 Uiso 1 1 calc R . . C52 C 0.3412(4) 0.8681(4) 0.3156(2) 0.0562(15) Uani 1 1 d . . . H52 H 0.3517 0.9274 0.3158 0.067 Uiso 1 1 calc R . . C53 C 0.2481(4) 0.8621(4) 0.3267(2) 0.0569(14) Uani 1 1 d . . . H53 H 0.1957 0.9172 0.3356 0.068 Uiso 1 1 calc R . . C54 C 0.2320(4) 0.7763(3) 0.3246(2) 0.0448(11) Uani 1 1 d . . . H54 H 0.1687 0.7726 0.3317 0.054 Uiso 1 1 calc R . . C55 C 0.8980(3) 0.3860(4) 0.1114(2) 0.0526(14) Uani 1 1 d . A . C56 C 0.9621(4) 0.3961(7) 0.0706(3) 0.092(3) Uani 1 1 d . . . H56 H 0.9467 0.3959 0.0385 0.110 Uiso 1 1 calc R A . C57 C 1.0482(5) 0.4065(8) 0.0763(4) 0.111(3) Uani 1 1 d . A . H57 H 1.0923 0.4124 0.0481 0.133 Uiso 1 1 calc R . . C58 C 1.0696(5) 0.4082(6) 0.1214(4) 0.097(3) Uani 1 1 d . . . H58 H 1.1296 0.4143 0.1249 0.117 Uiso 1 1 calc R A . C59 C 1.0057(5) 0.4014(5) 0.1630(3) 0.078(2) Uani 1 1 d . A . H59 H 1.0209 0.4044 0.1950 0.093 Uiso 1 1 calc R . . C60 C 0.9181(4) 0.3899(4) 0.1576(2) 0.0519(13) Uani 1 1 d . . . H60 H 0.8736 0.3849 0.1858 0.062 Uiso 1 1 calc R A . C61A C 0.7611(10) 0.4153(16) 0.0459(3) 0.038(4) Uani 0.59(5) 1 d PG A 1 C62A C 0.7413(9) 0.3682(18) 0.0085(3) 0.052(4) Uani 0.59(5) 1 d PG A 1 H62A H 0.7440 0.3043 0.0123 0.063 Uiso 0.59(5) 1 calc PR A 1 C63A C 0.7177(7) 0.415(2) -0.0345(3) 0.064(6) Uani 0.59(5) 1 d PG A 1 H63A H 0.7041 0.3826 -0.0601 0.077 Uiso 0.59(5) 1 calc PR A 1 C64A C 0.7138(9) 0.508(2) -0.0401(4) 0.070(8) Uani 0.59(5) 1 d PG A 1 H64A H 0.6976 0.5401 -0.0695 0.084 Uiso 0.59(5) 1 calc PR A 1 C65A C 0.7335(10) 0.5554(19) -0.0027(6) 0.076(7) Uani 0.59(5) 1 d PG A 1 H65A H 0.7309 0.6193 -0.0065 0.091 Uiso 0.59(5) 1 calc PR A 1 C66A C 0.7572(10) 0.5088(16) 0.0403(5) 0.054(5) Uani 0.59(5) 1 d PG A 1 H66A H 0.7707 0.5410 0.0659 0.065 Uiso 0.59(5) 1 calc PR A 1 C67 C 0.8222(4) 0.2442(5) 0.08574(19) 0.0601(16) Uani 1 1 d . A 1 C61B C 0.7595(16) 0.4462(17) 0.0504(6) 0.039(5) Uani 0.41(5) 1 d PG A 2 C62B C 0.7374(15) 0.410(2) 0.0098(6) 0.056(5) Uani 0.41(5) 1 d PG A 2 H62B H 0.7375 0.3465 0.0098 0.067 Uiso 0.41(5) 1 calc PR A 2 C63B C 0.7152(12) 0.466(3) -0.0306(6) 0.055(7) Uani 0.41(5) 1 d PG A 2 H63B H 0.7001 0.4413 -0.0583 0.066 Uiso 0.41(5) 1 calc PR A 2 C64B C 0.7151(14) 0.559(3) -0.0304(9) 0.079(9) Uani 0.41(5) 1 d PG A 2 H64B H 0.6999 0.5973 -0.0581 0.095 Uiso 0.41(5) 1 calc PR A 2 C65B C 0.7371(18) 0.5953(19) 0.0101(11) 0.091(9) Uani 0.41(5) 1 d PG A 2 H65B H 0.7370 0.6586 0.0102 0.109 Uiso 0.41(5) 1 calc PR A 2 C66B C 0.7593(18) 0.5389(16) 0.0505(9) 0.053(5) Uani 0.41(5) 1 d PG A 2 H66B H 0.7744 0.5638 0.0782 0.063 Uiso 0.41(5) 1 calc PR A 2 C68 C 0.9071(6) 0.2016(6) 0.0534(2) 0.097(3) Uani 1 1 d . . . H68 H 0.9494 0.2365 0.0415 0.116 Uiso 1 1 calc R A 1 C69 C 0.9299(10) 0.1083(10) 0.0384(4) 0.165(7) Uani 1 1 d . A . H69 H 0.9859 0.0807 0.0152 0.198 Uiso 1 1 calc R . . C70 C 0.8707(10) 0.0559(8) 0.0574(4) 0.151(6) Uani 1 1 d . . . H70 H 0.8893 -0.0089 0.0491 0.182 Uiso 1 1 calc R A . C71 C 0.7840(7) 0.0968(6) 0.0886(3) 0.110(3) Uani 1 1 d . A . H71 H 0.7412 0.0621 0.0998 0.132 Uiso 1 1 calc R . . C72 C 0.7627(5) 0.1907(5) 0.1029(2) 0.0708(19) Uani 1 1 d . . . H72 H 0.7053 0.2189 0.1251 0.085 Uiso 1 1 calc R A 1 C73 C 0.7235(3) 0.1361(3) 0.42794(14) 0.0271(8) Uani 1 1 d . . . C74 C 0.7499(3) 0.0755(3) 0.46711(15) 0.0315(9) Uani 1 1 d . . . H74 H 0.7615 0.0100 0.4633 0.038 Uiso 1 1 calc R . . C75 C 0.7591(3) 0.1108(3) 0.51126(16) 0.0365(10) Uani 1 1 d . . . H75 H 0.7760 0.0697 0.5377 0.044 Uiso 1 1 calc R . . C76 C 0.7436(3) 0.2063(3) 0.51666(17) 0.0405(11) Uani 1 1 d . . . H76 H 0.7493 0.2309 0.5469 0.049 Uiso 1 1 calc R . . C77 C 0.7198(3) 0.2656(3) 0.47791(17) 0.0394(10) Uani 1 1 d . . . H77 H 0.7102 0.3308 0.4816 0.047 Uiso 1 1 calc R . . C78 C 0.7098(3) 0.2312(3) 0.43370(16) 0.0324(9) Uani 1 1 d . . . H78 H 0.6935 0.2728 0.4073 0.039 Uiso 1 1 calc R . . C79 C 0.8003(3) -0.0215(3) 0.36080(14) 0.0282(8) Uani 1 1 d . . . C80 C 0.8910(3) -0.0322(3) 0.37104(17) 0.0378(10) Uani 1 1 d . . . H80 H 0.9037 0.0194 0.3842 0.045 Uiso 1 1 calc R . . C81 C 0.9635(4) -0.1175(4) 0.36222(19) 0.0485(13) Uani 1 1 d . . . H81 H 1.0251 -0.1242 0.3697 0.058 Uiso 1 1 calc R . . C82 C 0.9459(4) -0.1926(4) 0.3425(2) 0.0516(14) Uani 1 1 d . . . H82 H 0.9955 -0.2507 0.3365 0.062 Uiso 1 1 calc R . . C83 C 0.8571(4) -0.1836(3) 0.3316(2) 0.0502(13) Uani 1 1 d . . . H83 H 0.8456 -0.2350 0.3176 0.060 Uiso 1 1 calc R . . C84 C 0.7833(3) -0.0976(3) 0.34112(17) 0.0370(10) Uani 1 1 d . . . H84 H 0.7215 -0.0916 0.3341 0.044 Uiso 1 1 calc R . . C85 C 0.5993(3) 0.0590(3) 0.38386(14) 0.0255(8) Uani 1 1 d . . . C86 C 0.5807(3) 0.0079(3) 0.42613(14) 0.0300(9) Uani 1 1 d . . . H86 H 0.6244 -0.0082 0.4488 0.036 Uiso 1 1 calc R . . C87 C 0.4993(3) -0.0192(3) 0.43494(16) 0.0337(9) Uani 1 1 d . . . H87 H 0.4868 -0.0530 0.4639 0.040 Uiso 1 1 calc R . . C88 C 0.4360(3) 0.0026(3) 0.40182(17) 0.0366(10) Uani 1 1 d . . . H88 H 0.3801 -0.0161 0.4081 0.044 Uiso 1 1 calc R . . C89 C 0.4535(3) 0.0515(3) 0.35952(18) 0.0386(10) Uani 1 1 d . . . H89 H 0.4104 0.0655 0.3365 0.046 Uiso 1 1 calc R . . C90 C 0.5344(3) 0.0800(3) 0.35088(16) 0.0321(9) Uani 1 1 d . . . H90 H 0.5459 0.1145 0.3220 0.039 Uiso 1 1 calc R . . C91 C 0.5458(3) 0.5170(3) 0.17745(15) 0.0335(9) Uani 1 1 d . A . C92 C 0.5038(4) 0.5675(4) 0.07463(19) 0.0531(14) Uani 1 1 d . A . H92A H 0.5670 0.5233 0.0626 0.080 Uiso 1 1 calc R . . H92B H 0.4891 0.6191 0.0513 0.080 Uiso 1 1 calc R . . H92C H 0.4556 0.5350 0.0774 0.080 Uiso 1 1 calc R . . C93 C 0.5794(5) 0.6920(4) 0.1310(2) 0.0609(15) Uani 1 1 d . A . H93A H 0.5732 0.7209 0.1633 0.091 Uiso 1 1 calc R . . H93B H 0.5593 0.7412 0.1070 0.091 Uiso 1 1 calc R . . H93C H 0.6462 0.6549 0.1201 0.091 Uiso 1 1 calc R . . C94 C 0.3795(4) 0.6868(4) 0.1599(2) 0.0684(19) Uani 1 1 d . A . H94A H 0.3382 0.6466 0.1652 0.103 Uiso 1 1 calc R . . H94B H 0.3568 0.7352 0.1359 0.103 Uiso 1 1 calc R . . H94C H 0.3778 0.7168 0.1912 0.103 Uiso 1 1 calc R . . C95 C 0.4510(3) 0.3630(3) 0.36935(14) 0.0293(8) Uani 1 1 d . A . C96 C 0.2571(3) 0.3707(4) 0.4270(2) 0.0473(12) Uani 1 1 d . A . H96A H 0.2280 0.4292 0.4105 0.071 Uiso 1 1 calc R . . H96B H 0.2207 0.3708 0.4602 0.071 Uiso 1 1 calc R . . H96C H 0.2565 0.3172 0.4079 0.071 Uiso 1 1 calc R . . C97 C 0.3849(4) 0.4622(4) 0.46815(17) 0.0473(12) Uani 1 1 d . A . H97A H 0.4507 0.4546 0.4724 0.071 Uiso 1 1 calc R . . H97B H 0.3450 0.4646 0.5006 0.071 Uiso 1 1 calc R . . H97C H 0.3599 0.5207 0.4507 0.071 Uiso 1 1 calc R . . C98 C 0.4356(3) 0.2487(3) 0.46325(16) 0.0388(10) Uani 1 1 d . A . H98A H 0.4360 0.1957 0.4434 0.058 Uiso 1 1 calc R . . H98B H 0.3971 0.2485 0.4959 0.058 Uiso 1 1 calc R . . H98C H 0.5012 0.2432 0.4670 0.058 Uiso 1 1 calc R . . C99 C 0.8123(3) 0.1796(3) 0.24435(16) 0.0344(10) Uani 1 1 d . A . C100 C 0.9255(4) -0.0262(4) 0.2238(2) 0.0562(14) Uani 1 1 d . A . H10A H 0.8893 -0.0414 0.2544 0.084 Uiso 1 1 calc R . . H10B H 0.9900 -0.0712 0.2182 0.084 Uiso 1 1 calc R . . H10C H 0.8931 -0.0294 0.1960 0.084 Uiso 1 1 calc R . . C101 C 1.0014(4) 0.0998(4) 0.2797(2) 0.0555(14) Uani 1 1 d . A . H10D H 1.0261 0.1533 0.2747 0.083 Uiso 1 1 calc R . . H10E H 1.0547 0.0416 0.2793 0.083 Uiso 1 1 calc R . . H10F H 0.9589 0.1070 0.3117 0.083 Uiso 1 1 calc R . . C102 C 0.9974(4) 0.1255(5) 0.1697(2) 0.0701(19) Uani 1 1 d . A 3 H10G H 0.9693 0.1120 0.1422 0.105 Uiso 1 1 calc R A 3 H10H H 1.0651 0.0881 0.1656 0.105 Uiso 1 1 calc R A 3 H10I H 0.9917 0.1924 0.1700 0.105 Uiso 1 1 calc R A 3 C103 C 0.8562(2) 0.8435(2) 0.51671(11) 0.0467(12) Uani 1 1 d G B 3 C104 C 0.9400(2) 0.8671(2) 0.50454(10) 0.0515(13) Uani 1 1 d G B 3 H104 H 0.9743 0.8575 0.4717 0.062 Uiso 1 1 calc R B 3 C105 C 0.9737(2) 0.9049(3) 0.54036(14) 0.0578(15) Uani 1 1 d G B 3 H105 H 1.0310 0.9210 0.5320 0.069 Uiso 1 1 calc R B 3 C106 C 0.9236(3) 0.9189(2) 0.58836(12) 0.0559(14) Uani 1 1 d G B 3 H106 H 0.9466 0.9447 0.6128 0.067 Uiso 1 1 calc R B 3 C107 C 0.8398(2) 0.8953(2) 0.60053(10) 0.0543(14) Uani 1 1 d G B 3 H107 H 0.8055 0.9049 0.6333 0.065 Uiso 1 1 calc R B 3 C108 C 0.80607(19) 0.8575(2) 0.56471(13) 0.0468(12) Uani 1 1 d G B 3 H108 H 0.7488 0.8414 0.5730 0.056 Uiso 1 1 calc R B 3 C109 C 0.8194(4) 0.8040(4) 0.4776(2) 0.0574(14) Uani 1 1 d . B 3 H10J H 0.8350 0.8320 0.4457 0.086 Uiso 1 1 calc R B 3 H10K H 0.7499 0.8186 0.4863 0.086 Uiso 1 1 calc R B 3 H10L H 0.8493 0.7358 0.4753 0.086 Uiso 1 1 calc R B 3 C110 C 0.7406(9) 0.0700(7) 0.8515(3) 0.053(6) Uani 0.277(3) 1 d PG C 3 C111 C 0.8065(7) 0.0907(8) 0.8757(5) 0.053(5) Uani 0.277(3) 1 d PG C 3 H111 H 0.8646 0.0957 0.8573 0.064 Uiso 0.277(3) 1 calc PR C 3 C112 C 0.7874(8) 0.1040(9) 0.9266(5) 0.056(6) Uani 0.277(3) 1 d PG C 3 H112 H 0.8324 0.1181 0.9431 0.067 Uiso 0.277(3) 1 calc PR C 3 C113 C 0.7024(10) 0.0966(10) 0.9534(3) 0.098(11) Uani 0.277(3) 1 d PG C 3 H113 H 0.6893 0.1057 0.9883 0.117 Uiso 0.277(3) 1 calc PR C 3 C114 C 0.6365(8) 0.0760(9) 0.9293(4) 0.052(5) Uani 0.277(3) 1 d PG C 3 H114 H 0.5784 0.0710 0.9477 0.063 Uiso 0.277(3) 1 calc PR C 3 C115 C 0.6556(8) 0.0627(8) 0.8784(4) 0.057(6) Uani 0.277(3) 1 d PG C 3 H115 H 0.6106 0.0486 0.8619 0.069 Uiso 0.277(3) 1 calc PR C 3 C116 C 0.7551(15) 0.0579(13) 0.7987(8) 0.057(5) Uani 0.277(3) 1 d P C 3 H11A H 0.8106 0.0767 0.7836 0.086 Uiso 0.277(3) 1 calc PR C 3 H11B H 0.6982 0.0970 0.7859 0.086 Uiso 0.277(3) 1 calc PR C 3 H11C H 0.7663 -0.0081 0.7906 0.086 Uiso 0.277(3) 1 calc PR C 3 C117 C 0.2293(11) 0.1682(9) 1.0048(4) 0.070(5) Uani 0.340(5) 1 d PGU D 4 C118 C 0.1498(9) 0.2186(10) 0.9842(5) 0.092(7) Uani 0.340(5) 1 d PGU D 4 H118 H 0.0922 0.2517 1.0050 0.110 Uiso 0.340(5) 1 calc PR D 4 C119 C 0.1547(10) 0.2205(10) 0.9332(6) 0.081(7) Uani 0.340(5) 1 d PGU D 4 H119 H 0.1004 0.2550 0.9192 0.097 Uiso 0.340(5) 1 calc PR D 4 C120 C 0.2390(13) 0.1720(11) 0.9028(4) 0.073(7) Uani 0.340(5) 1 d PGU D 4 H120 H 0.2423 0.1734 0.8680 0.088 Uiso 0.340(5) 1 calc PR D 4 C121 C 0.3185(10) 0.1216(11) 0.9234(6) 0.077(8) Uani 0.340(5) 1 d PGU D 4 H121 H 0.3761 0.0885 0.9026 0.092 Uiso 0.340(5) 1 calc PR D 4 C122 C 0.3136(9) 0.1197(9) 0.9744(6) 0.084(7) Uani 0.340(5) 1 d PGU D 4 H122 H 0.3679 0.0852 0.9884 0.101 Uiso 0.340(5) 1 calc PR D 4 C123 C 0.2274(17) 0.155(2) 1.0541(8) 0.104(9) Uani 0.340(5) 1 d PU D 4 H12A H 0.1730 0.2038 1.0722 0.155 Uiso 0.340(5) 1 calc PR D 4 H12B H 0.2869 0.1592 1.0630 0.155 Uiso 0.340(5) 1 calc PR D 4 H12C H 0.2211 0.0932 1.0627 0.155 Uiso 0.340(5) 1 calc PR D 4 C124 C 0.1724(10) 0.1893(9) 0.9107(5) 0.086(7) Uani 0.383(5) 1 d PGU E 5 C125 C 0.1587(8) 0.2779(10) 0.9298(4) 0.076(6) Uani 0.383(5) 1 d PGU E 5 H125 H 0.2118 0.2948 0.9361 0.091 Uiso 0.383(5) 1 calc PR E 5 C126 C 0.0672(10) 0.3417(9) 0.9396(3) 0.105(8) Uani 0.383(5) 1 d PGU E 5 H126 H 0.0578 0.4022 0.9526 0.126 Uiso 0.383(5) 1 calc PR E 5 C127 C -0.0106(7) 0.3168(13) 0.9303(4) 0.099(8) Uani 0.383(5) 1 d PGU E 5 H127 H -0.0731 0.3604 0.9370 0.119 Uiso 0.383(5) 1 calc PR E 5 C128 C 0.0031(11) 0.2282(14) 0.9111(4) 0.123(9) Uani 0.383(5) 1 d PGU E 5 H128 H -0.0500 0.2113 0.9048 0.148 Uiso 0.383(5) 1 calc PR E 5 C129 C 0.0946(14) 0.1645(9) 0.9013(4) 0.094(7) Uani 0.383(5) 1 d PGU E 5 H129 H 0.1040 0.1039 0.8883 0.112 Uiso 0.383(5) 1 calc PR E 5 C130 C 0.269(2) 0.1300(14) 0.9122(8) 0.080(8) Uani 0.383(5) 1 d PU E 5 H13A H 0.3135 0.1527 0.8888 0.120 Uiso 0.383(5) 1 calc PR E 5 H13B H 0.2748 0.0655 0.9033 0.120 Uiso 0.383(5) 1 calc PR E 5 H13C H 0.2829 0.1314 0.9457 0.120 Uiso 0.383(5) 1 calc PR E 5 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 Pd1 0.02225(15) 0.02250(16) 0.02353(14) 0.00037(11) -0.00131(11) -0.00568(11) Pd2 0.02508(16) 0.02406(16) 0.02431(15) -0.00056(11) -0.00285(11) -0.00590(12) Pd3 0.02152(15) 0.02346(16) 0.02466(15) 0.00154(11) -0.00045(11) -0.00282(11) Pd4 0.02711(17) 0.03216(18) 0.02319(15) 0.00302(12) 0.00015(11) -0.00606(13) Pd5 0.02293(15) 0.02182(16) 0.02549(15) 0.00108(11) -0.00102(11) -0.00211(11) P1 0.0242(5) 0.0236(5) 0.0266(5) -0.0007(4) -0.0023(4) -0.0058(4) P2 0.0391(6) 0.0291(6) 0.0318(5) 0.0010(4) -0.0103(4) -0.0117(5) P3 0.0220(5) 0.0230(5) 0.0273(5) -0.0006(4) -0.0024(4) -0.0044(4) P4 0.0281(6) 0.0651(9) 0.0254(5) 0.0045(5) -0.0001(4) -0.0073(5) P5 0.0232(5) 0.0209(5) 0.0266(5) -0.0003(4) -0.0027(4) -0.0040(4) P6 0.0262(5) 0.0296(6) 0.0270(5) 0.0048(4) 0.0004(4) -0.0026(4) P7 0.0295(6) 0.0288(6) 0.0263(5) 0.0001(4) 0.0024(4) -0.0022(4) P8 0.0247(5) 0.0218(5) 0.0255(5) 0.0022(4) 0.0003(4) -0.0017(4) Si1 0.0334(7) 0.0409(7) 0.0401(7) 0.0177(5) -0.0066(5) -0.0114(5) Si2 0.0287(6) 0.0261(6) 0.0268(5) 0.0014(4) 0.0037(4) -0.0052(4) Si3 0.0294(6) 0.0350(7) 0.0368(6) -0.0009(5) 0.0033(5) 0.0009(5) C1 0.026(2) 0.027(2) 0.033(2) -0.0011(16) 0.0008(16) -0.0085(16) C2 0.034(2) 0.042(3) 0.035(2) 0.0009(18) -0.0058(18) -0.0174(19) C3 0.037(3) 0.053(3) 0.044(3) -0.002(2) -0.004(2) -0.023(2) C4 0.041(3) 0.040(3) 0.048(3) 0.007(2) 0.004(2) -0.018(2) C5 0.047(3) 0.039(3) 0.041(2) 0.014(2) -0.007(2) -0.013(2) C6 0.033(2) 0.037(3) 0.040(2) 0.0079(19) -0.0070(18) -0.0120(18) C7 0.026(2) 0.033(2) 0.0293(19) 0.0043(16) -0.0040(15) -0.0107(16) C8 0.041(3) 0.037(3) 0.042(2) 0.0000(19) -0.012(2) -0.006(2) C9 0.047(3) 0.043(3) 0.050(3) 0.001(2) -0.017(2) 0.001(2) C10 0.043(3) 0.044(3) 0.049(3) 0.016(2) -0.019(2) -0.008(2) C11 0.053(3) 0.048(3) 0.035(2) 0.006(2) -0.015(2) -0.019(2) C12 0.038(2) 0.036(2) 0.032(2) 0.0014(17) -0.0043(17) -0.0115(19) C13 0.029(2) 0.026(2) 0.0276(19) -0.0031(15) -0.0031(15) -0.0072(16) C14 0.033(2) 0.031(2) 0.032(2) -0.0020(17) 0.0024(17) -0.0092(17) C15 0.037(2) 0.038(3) 0.035(2) -0.0056(18) 0.0074(18) -0.0070(19) C16 0.047(3) 0.032(3) 0.038(2) -0.0116(19) 0.002(2) -0.001(2) C17 0.049(3) 0.029(2) 0.055(3) -0.010(2) 0.000(2) -0.013(2) C18 0.035(2) 0.035(3) 0.048(3) -0.007(2) 0.005(2) -0.0126(19) C19 0.248(12) 0.050(4) 0.045(3) 0.012(3) -0.054(5) -0.050(5) C20 0.40(2) 0.080(6) 0.042(4) 0.000(4) -0.059(7) -0.096(9) C21 0.280(14) 0.059(5) 0.038(3) 0.010(3) -0.038(5) -0.043(6) C22 0.100(5) 0.057(4) 0.043(3) 0.014(3) -0.027(3) -0.019(3) C23 0.061(3) 0.037(3) 0.043(3) 0.003(2) -0.013(2) -0.015(2) C24 0.066(3) 0.043(3) 0.034(2) 0.004(2) -0.020(2) -0.018(2) C25 0.042(3) 0.036(3) 0.055(3) 0.008(2) -0.017(2) -0.020(2) C26 0.041(3) 0.042(3) 0.060(3) 0.002(2) -0.005(2) -0.016(2) C27 0.040(3) 0.059(4) 0.099(5) 0.005(3) 0.000(3) -0.020(3) C28 0.041(4) 0.075(5) 0.135(7) 0.019(5) -0.016(4) -0.026(3) C29 0.047(4) 0.077(5) 0.117(6) 0.011(4) -0.039(4) -0.025(3) C30 0.058(4) 0.055(4) 0.083(4) 0.012(3) -0.035(3) -0.024(3) C31 0.046(3) 0.030(2) 0.030(2) -0.0009(17) -0.0077(18) -0.0110(19) C32 0.049(3) 0.034(3) 0.053(3) 0.002(2) -0.011(2) -0.015(2) C33 0.076(4) 0.036(3) 0.058(3) 0.004(2) -0.016(3) -0.024(3) C34 0.073(4) 0.026(3) 0.061(3) 0.003(2) -0.010(3) -0.008(2) C35 0.059(3) 0.040(3) 0.051(3) -0.005(2) -0.015(3) 0.002(2) C36 0.047(3) 0.034(3) 0.041(2) -0.0032(19) -0.007(2) -0.010(2) C37 0.026(2) 0.026(2) 0.033(2) 0.0028(16) 0.0004(16) -0.0021(16) C38 0.051(3) 0.035(3) 0.035(2) -0.0024(19) 0.001(2) -0.008(2) C39 0.069(4) 0.045(3) 0.042(3) 0.000(2) 0.016(3) 0.002(3) C40 0.043(3) 0.068(4) 0.057(3) 0.027(3) 0.018(3) 0.007(3) C41 0.033(3) 0.076(4) 0.068(4) 0.037(3) -0.009(2) -0.016(3) C42 0.028(2) 0.051(3) 0.045(3) 0.017(2) -0.0093(19) -0.016(2) C43 0.029(2) 0.034(2) 0.029(2) 0.0037(16) -0.0032(16) -0.0107(17) C44 0.050(3) 0.036(3) 0.040(2) -0.0003(19) -0.016(2) -0.010(2) C45 0.080(4) 0.057(4) 0.052(3) -0.013(3) -0.031(3) -0.008(3) C46 0.056(3) 0.077(4) 0.042(3) 0.010(3) -0.025(2) -0.020(3) C47 0.033(3) 0.059(3) 0.043(3) 0.017(2) -0.011(2) -0.009(2) C48 0.028(2) 0.038(3) 0.039(2) 0.0085(18) -0.0061(17) -0.0063(18) C49 0.036(2) 0.023(2) 0.032(2) 0.0028(16) -0.0057(17) -0.0079(16) C50 0.038(2) 0.032(2) 0.046(3) 0.0075(19) -0.014(2) -0.0119(19) C51 0.051(3) 0.046(3) 0.065(3) 0.010(2) -0.022(3) -0.029(2) C52 0.077(4) 0.027(3) 0.078(4) 0.007(2) -0.027(3) -0.029(3) C53 0.060(4) 0.028(3) 0.076(4) -0.008(2) -0.005(3) -0.008(2) C54 0.039(3) 0.027(2) 0.062(3) -0.001(2) -0.003(2) -0.0044(19) C55 0.026(2) 0.074(4) 0.053(3) 0.006(3) -0.006(2) -0.009(2) C56 0.032(3) 0.166(8) 0.076(4) 0.027(5) 0.002(3) -0.038(4) C57 0.040(4) 0.182(10) 0.109(7) 0.023(7) -0.003(4) -0.041(5) C58 0.034(4) 0.106(7) 0.149(8) -0.022(6) -0.012(4) -0.016(4) C59 0.057(4) 0.064(4) 0.105(6) -0.032(4) -0.030(4) 0.003(3) C60 0.038(3) 0.043(3) 0.068(3) -0.008(2) -0.012(2) 0.001(2) C61A 0.028(5) 0.056(10) 0.026(5) 0.012(5) -0.006(4) -0.007(6) C62A 0.041(5) 0.085(12) 0.023(4) 0.014(5) -0.007(4) -0.009(6) C63A 0.044(6) 0.098(15) 0.039(5) 0.011(7) -0.015(4) -0.002(8) C64A 0.038(6) 0.119(19) 0.043(7) 0.058(10) -0.013(5) -0.012(8) C65A 0.043(7) 0.118(15) 0.058(9) 0.062(10) -0.011(6) -0.017(8) C66A 0.032(5) 0.088(14) 0.042(7) 0.018(8) -0.002(5) -0.022(8) C67 0.051(3) 0.079(4) 0.035(3) -0.013(3) 0.000(2) 0.000(3) C61B 0.036(8) 0.052(13) 0.030(8) -0.005(7) 0.007(6) -0.021(9) C62B 0.052(9) 0.054(13) 0.063(11) 0.013(8) -0.013(8) -0.018(9) C63B 0.060(10) 0.071(19) 0.031(9) 0.032(9) -0.021(7) -0.013(10) C64B 0.051(10) 0.11(2) 0.071(16) 0.059(15) 0.000(10) -0.023(13) C65B 0.047(11) 0.13(2) 0.096(19) 0.047(17) 0.000(12) -0.031(14) C66B 0.059(11) 0.057(11) 0.040(9) 0.009(8) 0.008(8) -0.023(9) C68 0.081(5) 0.114(7) 0.057(4) -0.025(4) 0.017(4) 0.012(5) C69 0.154(12) 0.166(13) 0.091(8) -0.052(8) 0.033(7) 0.049(9) C70 0.203(15) 0.105(9) 0.092(8) -0.061(7) 0.007(8) 0.021(9) C71 0.139(8) 0.073(6) 0.105(6) -0.049(5) -0.005(6) -0.016(5) C72 0.079(5) 0.063(4) 0.054(3) -0.021(3) -0.002(3) 0.001(3) C73 0.0221(19) 0.029(2) 0.0288(19) -0.0005(15) -0.0013(14) -0.0070(15) C74 0.032(2) 0.027(2) 0.036(2) 0.0017(16) -0.0095(17) -0.0083(17) C75 0.033(2) 0.041(3) 0.034(2) 0.0016(18) -0.0089(18) -0.0090(19) C76 0.044(3) 0.042(3) 0.037(2) -0.010(2) -0.007(2) -0.015(2) C77 0.047(3) 0.027(2) 0.044(2) -0.0069(19) -0.005(2) -0.0123(19) C78 0.034(2) 0.025(2) 0.037(2) 0.0006(16) -0.0062(17) -0.0090(17) C79 0.024(2) 0.026(2) 0.0298(19) -0.0018(15) -0.0014(15) -0.0023(15) C80 0.027(2) 0.037(3) 0.042(2) -0.0039(19) -0.0022(18) -0.0019(18) C81 0.032(3) 0.044(3) 0.058(3) 0.001(2) 0.000(2) 0.001(2) C82 0.035(3) 0.032(3) 0.067(3) -0.001(2) 0.012(2) 0.009(2) C83 0.049(3) 0.024(2) 0.065(3) -0.011(2) 0.012(2) -0.004(2) C84 0.033(2) 0.024(2) 0.048(3) -0.0064(18) 0.0031(19) -0.0055(17) C85 0.0246(19) 0.0215(19) 0.0275(18) -0.0014(14) -0.0038(14) -0.0032(14) C86 0.030(2) 0.031(2) 0.0273(19) -0.0015(16) -0.0023(16) -0.0078(16) C87 0.038(2) 0.027(2) 0.034(2) -0.0015(16) 0.0015(17) -0.0122(18) C88 0.028(2) 0.036(2) 0.046(2) -0.0045(19) -0.0015(18) -0.0118(18) C89 0.030(2) 0.043(3) 0.047(3) 0.004(2) -0.0121(19) -0.0134(19) C90 0.031(2) 0.031(2) 0.035(2) 0.0044(17) -0.0070(17) -0.0098(17) C91 0.030(2) 0.036(2) 0.033(2) 0.0073(17) -0.0042(17) -0.0104(18) C92 0.047(3) 0.072(4) 0.047(3) 0.018(3) -0.018(2) -0.024(3) C93 0.067(4) 0.056(4) 0.068(4) 0.023(3) -0.019(3) -0.030(3) C94 0.054(4) 0.062(4) 0.068(4) 0.030(3) -0.001(3) 0.005(3) C95 0.030(2) 0.029(2) 0.0250(18) 0.0027(15) -0.0021(15) -0.0050(16) C96 0.036(3) 0.041(3) 0.059(3) 0.016(2) -0.002(2) -0.009(2) C97 0.060(3) 0.043(3) 0.035(2) -0.006(2) 0.005(2) -0.016(2) C98 0.041(3) 0.033(2) 0.036(2) 0.0090(18) 0.0010(19) -0.0074(19) C99 0.027(2) 0.033(2) 0.034(2) -0.0053(17) 0.0016(16) 0.0008(17) C100 0.053(3) 0.039(3) 0.064(3) -0.011(2) 0.003(3) -0.003(2) C101 0.035(3) 0.060(4) 0.065(3) 0.000(3) -0.008(2) -0.006(2) C102 0.054(4) 0.062(4) 0.064(4) 0.012(3) 0.024(3) 0.007(3) C103 0.044(3) 0.029(2) 0.061(3) 0.016(2) -0.012(2) -0.003(2) C104 0.038(3) 0.052(3) 0.058(3) 0.018(2) -0.002(2) -0.008(2) C105 0.036(3) 0.058(4) 0.078(4) 0.024(3) -0.018(3) -0.012(2) C106 0.051(3) 0.042(3) 0.072(4) 0.017(3) -0.022(3) -0.006(2) C107 0.053(3) 0.040(3) 0.062(3) 0.012(2) -0.003(3) -0.007(2) C108 0.038(3) 0.027(2) 0.068(3) 0.006(2) 0.003(2) -0.0060(19) C109 0.066(4) 0.041(3) 0.067(4) 0.007(3) -0.013(3) -0.019(3) C110 0.069(13) 0.005(7) 0.057(11) -0.014(7) -0.007(9) 0.028(7) C111 0.031(9) 0.016(8) 0.103(16) 0.015(9) -0.025(10) 0.012(6) C112 0.056(12) 0.048(12) 0.049(11) -0.002(9) -0.017(9) 0.011(9) C113 0.11(2) 0.080(19) 0.14(3) 0.066(18) -0.07(2) -0.063(17) C114 0.076(14) 0.061(13) 0.032(9) 0.016(8) -0.015(9) -0.038(11) C115 0.062(13) 0.007(7) 0.097(16) 0.002(8) -0.014(11) -0.002(7) C116 0.050(12) 0.033(10) 0.081(14) 0.002(9) -0.022(10) 0.004(8) C117 0.094(14) 0.034(9) 0.079(12) -0.012(8) 0.006(11) -0.024(9) C118 0.085(15) 0.108(17) 0.078(13) -0.033(12) 0.012(12) -0.034(13) C119 0.076(13) 0.086(16) 0.088(16) 0.034(13) -0.011(12) -0.040(12) C120 0.15(2) 0.036(11) 0.046(10) 0.019(9) 0.007(12) -0.058(13) C121 0.070(14) 0.039(11) 0.110(18) -0.014(11) 0.022(13) -0.016(10) C122 0.096(15) 0.040(10) 0.107(15) -0.001(10) -0.043(13) 0.004(10) C123 0.083(17) 0.15(2) 0.066(13) 0.027(14) -0.023(12) -0.023(16) C124 0.102(15) 0.087(14) 0.057(11) 0.033(10) 0.020(11) -0.035(13) C125 0.073(11) 0.096(14) 0.054(9) 0.047(9) 0.002(8) -0.030(10) C126 0.054(10) 0.18(2) 0.029(7) 0.037(10) 0.016(7) 0.018(12) C127 0.057(10) 0.19(2) 0.027(7) 0.056(10) -0.003(7) -0.008(12) C128 0.15(2) 0.18(2) 0.057(12) 0.089(14) -0.044(12) -0.066(18) C129 0.146(19) 0.081(13) 0.062(10) 0.047(10) -0.029(12) -0.045(13) C130 0.15(2) 0.034(11) 0.065(11) 0.019(9) -0.003(13) -0.056(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2982(11) . ? Pd1 P7 2.4353(11) . ? Pd1 P8 2.4445(11) . ? Pd1 P6 2.4656(11) . ? Pd1 Pd2 2.6102(5) . ? Pd1 Pd4 2.8878(6) . ? Pd1 Pd3 2.8999(6) . ? Pd1 Pd5 2.9027(6) . ? Pd2 P2 2.2951(12) . ? Pd2 P6 2.4727(12) . ? Pd2 P7 2.4857(12) . ? Pd2 P8 2.4904(11) . ? Pd2 Pd4 2.8986(5) . ? Pd2 Pd5 2.9048(5) . ? Pd2 Pd3 2.9135(6) . ? Pd3 C95 2.180(4) . ? Pd3 P6 2.2949(11) . ? Pd3 P3 2.3135(10) . ? Pd3 P8 2.4673(11) . ? Pd4 C91 2.185(4) . ? Pd4 P4 2.3001(12) . ? Pd4 P7 2.3043(12) . ? Pd4 P6 2.4561(11) . ? Pd5 C99 2.176(4) . ? Pd5 P8 2.2955(10) . ? Pd5 P5 2.3176(11) . ? Pd5 P7 2.4667(12) . ? P1 C7 1.828(4) . ? P1 C13 1.828(4) . ? P1 C1 1.839(4) . ? P2 C24 1.825(5) . ? P2 C25 1.825(5) . ? P2 C31 1.838(5) . ? P3 C43 1.834(4) . ? P3 C37 1.834(4) . ? P3 C49 1.834(4) . ? P4 C67 1.811(7) . ? P4 C61A 1.814(7) . ? P4 C55 1.830(5) . ? P4 C61B 1.911(13) . ? P5 C85 1.830(4) . ? P5 C73 1.841(4) . ? P5 C79 1.843(4) . ? P6 C91 1.613(4) . ? P7 C99 1.620(4) . ? P8 C95 1.613(4) . ? Si1 C91 1.840(4) . ? Si1 C94 1.846(6) . ? Si1 C93 1.846(6) . ? Si1 C92 1.854(5) . ? Si2 C95 1.839(4) . ? Si2 C97 1.861(5) . ? Si2 C96 1.866(5) . ? Si2 C98 1.873(4) . ? Si3 C99 1.841(4) . ? Si3 C102 1.865(6) . ? Si3 C100 1.870(6) . ? Si3 C101 1.876(6) . ? C1 C2 1.385(6) . ? C1 C6 1.388(6) . ? C2 C3 1.379(7) . ? C2 H2 0.9500 . ? C3 C4 1.387(7) . ? C3 H3 0.9500 . ? C4 C5 1.382(7) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.394(6) . ? C7 C12 1.398(6) . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 C10 1.388(7) . ? C9 H9 0.9500 . ? C10 C11 1.390(7) . ? C10 H10 0.9500 . ? C11 C12 1.388(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.386(6) . ? C13 C18 1.389(6) . ? C14 C15 1.404(6) . ? C14 H14 0.9500 . ? C15 C16 1.377(7) . ? C15 H15 0.9500 . ? C16 C17 1.381(7) . ? C16 H16 0.9500 . ? C17 C18 1.409(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.380(8) . ? C19 C20 1.406(9) . ? C19 H19 0.9500 . ? C20 C21 1.358(11) . ? C20 H20 0.9500 . ? C21 C22 1.340(9) . ? C21 H21 0.9500 . ? C22 C23 1.384(7) . ? C22 H22 0.9500 . ? C23 C24 1.390(7) . ? C23 H23 0.9500 . ? C25 C26 1.390(7) . ? C25 C30 1.392(7) . ? C26 C27 1.398(7) . ? C26 H26 0.9500 . ? C27 C28 1.370(10) . ? C27 H27 0.9500 . ? C28 C29 1.346(11) . ? C28 H28 0.9500 . ? C29 C30 1.385(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.381(7) . ? C31 C32 1.396(7) . ? C32 C33 1.387(7) . ? C32 H32 0.9500 . ? C33 C34 1.390(8) . ? C33 H33 0.9500 . ? C34 C35 1.358(8) . ? C34 H34 0.9500 . ? C35 C36 1.409(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.379(6) . ? C37 C38 1.401(6) . ? C38 C39 1.372(7) . ? C38 H38 0.9500 . ? C39 C40 1.369(9) . ? C39 H39 0.9500 . ? C40 C41 1.379(9) . ? C40 H40 0.9500 . ? C41 C42 1.391(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.375(6) . ? C43 C48 1.408(6) . ? C44 C45 1.397(7) . ? C44 H44 0.9500 . ? C45 C46 1.360(8) . ? C45 H45 0.9500 . ? C46 C47 1.383(8) . ? C46 H46 0.9500 . ? C47 C48 1.383(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.376(6) . ? C49 C54 1.405(6) . ? C50 C51 1.407(7) . ? C50 H50 0.9500 . ? C51 C52 1.350(8) . ? C51 H51 0.9500 . ? C52 C53 1.403(8) . ? C52 H52 0.9500 . ? C53 C54 1.387(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.360(7) . ? C55 C56 1.382(8) . ? C56 C57 1.377(10) . ? C56 H56 0.9500 . ? C57 C58 1.333(12) . ? C57 H57 0.9500 . ? C58 C59 1.383(11) . ? C58 H58 0.9500 . ? C59 C60 1.403(9) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61A C62A 1.3900 . ? C61A C66A 1.3900 . ? C62A C63A 1.3900 . ? C62A H62A 0.9500 . ? C63A C64A 1.3900 . ? C63A H63A 0.9500 . ? C64A C65A 1.3900 . ? C64A H64A 0.9500 . ? C65A C66A 1.3900 . ? C65A H65A 0.9500 . ? C66A H66A 0.9500 . ? C67 C72 1.390(10) . ? C67 C68 1.401(8) . ? C61B C62B 1.3900 . ? C61B C66B 1.3900 . ? C62B C63B 1.3900 . ? C62B H62B 0.9500 . ? C63B C64B 1.3900 . ? C63B H63B 0.9500 . ? C64B C65B 1.3900 . ? C64B H64B 0.9500 . ? C65B C66B 1.3900 . ? C65B H65B 0.9500 . ? C66B H66B 0.9500 . ? C68 C69 1.394(15) . ? C68 H68 0.9500 . ? C69 C70 1.385(18) . ? C69 H69 0.9500 . ? C70 C71 1.398(14) . ? C70 H70 0.9500 . ? C71 C72 1.399(9) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C78 1.388(6) . ? C73 C74 1.408(6) . ? C74 C75 1.387(6) . ? C74 H74 0.9500 . ? C75 C76 1.387(6) . ? C75 H75 0.9500 . ? C76 C77 1.380(7) . ? C76 H76 0.9500 . ? C77 C78 1.386(6) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.389(6) . ? C79 C84 1.391(6) . ? C80 C81 1.392(6) . ? C80 H80 0.9500 . ? C81 C82 1.382(8) . ? C81 H81 0.9500 . ? C82 C83 1.374(8) . ? C82 H82 0.9500 . ? C83 C84 1.410(6) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C90 1.393(5) . ? C85 C86 1.403(6) . ? C86 C87 1.380(6) . ? C86 H86 0.9500 . ? C87 C88 1.379(6) . ? C87 H87 0.9500 . ? C88 C89 1.381(7) . ? C88 H88 0.9500 . ? C89 C90 1.385(6) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? C102 H10G 0.9800 . ? C102 H10H 0.9800 . ? C102 H10I 0.9800 . ? C103 C104 1.3900 . ? C103 C108 1.3900 . ? C103 C109 1.503(6) . ? C104 C105 1.3900 . ? C104 H104 0.9500 . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 C107 1.3900 . ? C106 H106 0.9500 . ? C107 C108 1.3900 . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 H10J 0.9800 . ? C109 H10K 0.9800 . ? C109 H10L 0.9800 . ? C110 C111 1.3900 . ? C110 C115 1.3900 . ? C110 C116 1.44(2) . ? C111 C112 1.3900 . ? C111 H111 0.9500 . ? C112 C113 1.3900 . ? C112 H112 0.9500 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 H11A 0.9800 . ? C116 H11B 0.9800 . ? C116 H11C 0.9800 . ? C117 C123 1.36(2) . ? C117 C118 1.3900 . ? C117 C122 1.3900 . ? C118 C119 1.3900 . ? C118 H118 0.9500 . ? C119 C120 1.3900 . ? C119 H119 0.9500 . ? C120 C121 1.3900 . ? C120 H120 0.9500 . ? C121 C122 1.3900 . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 C125 1.3900 . ? C124 C129 1.3900 . ? C124 C130 1.44(3) . ? C125 C126 1.3900 . ? C125 H125 0.9500 . ? C126 C127 1.3900 . ? C126 H126 0.9500 . ? C127 C128 1.3900 . ? C127 H127 0.9500 . ? C128 C129 1.3900 . ? C128 H128 0.9500 . ? C129 H129 0.9500 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 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 Pd1 P7 120.67(4) . . ? P1 Pd1 P8 122.28(4) . . ? P7 Pd1 P8 95.72(4) . . ? P1 Pd1 P6 120.98(4) . . ? P7 Pd1 P6 95.48(4) . . ? P8 Pd1 P6 95.13(4) . . ? P1 Pd1 Pd2 178.77(3) . . ? P7 Pd1 Pd2 58.91(3) . . ? P8 Pd1 Pd2 58.93(3) . . ? P6 Pd1 Pd2 58.22(3) . . ? P1 Pd1 Pd4 115.40(3) . . ? P7 Pd1 Pd4 50.43(3) . . ? P8 Pd1 Pd4 122.29(3) . . ? P6 Pd1 Pd4 53.92(3) . . ? Pd2 Pd1 Pd4 63.398(13) . . ? P1 Pd1 Pd3 116.77(3) . . ? P7 Pd1 Pd3 122.45(3) . . ? P8 Pd1 Pd3 54.18(3) . . ? P6 Pd1 Pd3 49.84(3) . . ? Pd2 Pd1 Pd3 63.588(14) . . ? Pd4 Pd1 Pd3 101.381(14) . . ? P1 Pd1 Pd5 117.50(3) . . ? P7 Pd1 Pd5 54.19(3) . . ? P8 Pd1 Pd5 49.95(2) . . ? P6 Pd1 Pd5 121.49(3) . . ? Pd2 Pd1 Pd5 63.332(14) . . ? Pd4 Pd1 Pd5 101.801(15) . . ? Pd3 Pd1 Pd5 101.442(14) . . ? P2 Pd2 P6 122.40(4) . . ? P2 Pd2 P7 122.05(4) . . ? P6 Pd2 P7 94.03(4) . . ? P2 Pd2 P8 123.34(4) . . ? P6 Pd2 P8 93.80(4) . . ? P7 Pd2 P8 93.30(4) . . ? P2 Pd2 Pd1 179.07(3) . . ? P6 Pd2 Pd1 57.96(3) . . ? P7 Pd2 Pd1 57.03(3) . . ? P8 Pd2 Pd1 57.22(3) . . ? P2 Pd2 Pd4 116.44(3) . . ? P6 Pd2 Pd4 53.71(3) . . ? P7 Pd2 Pd4 49.96(3) . . ? P8 Pd2 Pd4 120.16(3) . . ? Pd1 Pd2 Pd4 62.975(15) . . ? P2 Pd2 Pd5 116.42(3) . . ? P6 Pd2 Pd5 121.15(3) . . ? P7 Pd2 Pd5 53.78(3) . . ? P8 Pd2 Pd5 49.63(2) . . ? Pd1 Pd2 Pd5 63.251(14) . . ? Pd4 Pd2 Pd5 101.489(16) . . ? P2 Pd2 Pd3 117.86(3) . . ? P6 Pd2 Pd3 49.61(3) . . ? P7 Pd2 Pd3 120.05(3) . . ? P8 Pd2 Pd3 53.64(2) . . ? Pd1 Pd2 Pd3 63.055(15) . . ? Pd4 Pd2 Pd3 100.795(17) . . ? Pd5 Pd2 Pd3 101.066(16) . . ? C95 Pd3 P6 139.05(11) . . ? C95 Pd3 P3 118.37(11) . . ? P6 Pd3 P3 102.56(4) . . ? C95 Pd3 P8 40.02(11) . . ? P6 Pd3 P8 99.03(4) . . ? P3 Pd3 P8 158.30(4) . . ? C95 Pd3 Pd1 88.54(11) . . ? P6 Pd3 Pd1 55.20(3) . . ? P3 Pd3 Pd1 144.79(3) . . ? P8 Pd3 Pd1 53.45(3) . . ? C95 Pd3 Pd2 89.29(10) . . ? P6 Pd3 Pd2 55.15(3) . . ? P3 Pd3 Pd2 140.44(3) . . ? P8 Pd3 Pd2 54.38(3) . . ? Pd1 Pd3 Pd2 53.358(11) . . ? C91 Pd4 P4 117.72(12) . . ? C91 Pd4 P7 139.35(11) . . ? P4 Pd4 P7 102.90(4) . . ? C91 Pd4 P6 40.14(11) . . ? P4 Pd4 P6 157.57(4) . . ? P7 Pd4 P6 99.22(4) . . ? C91 Pd4 Pd1 89.20(11) . . ? P4 Pd4 Pd1 145.60(3) . . ? P7 Pd4 Pd1 54.55(3) . . ? P6 Pd4 Pd1 54.23(3) . . ? C91 Pd4 Pd2 89.42(12) . . ? P4 Pd4 Pd2 139.58(4) . . ? P7 Pd4 Pd2 55.67(3) . . ? P6 Pd4 Pd2 54.24(3) . . ? Pd1 Pd4 Pd2 53.627(12) . . ? C99 Pd5 P8 139.01(12) . . ? C99 Pd5 P5 118.41(12) . . ? P8 Pd5 P5 102.55(4) . . ? C99 Pd5 P7 40.22(12) . . ? P8 Pd5 P7 98.83(4) . . ? P5 Pd5 P7 158.17(4) . . ? C99 Pd5 Pd1 88.29(12) . . ? P8 Pd5 Pd1 54.60(3) . . ? P5 Pd5 Pd1 146.67(3) . . ? P7 Pd5 Pd1 53.19(3) . . ? C99 Pd5 Pd2 89.61(11) . . ? P8 Pd5 Pd2 55.75(3) . . ? P5 Pd5 Pd2 138.16(3) . . ? P7 Pd5 Pd2 54.39(3) . . ? Pd1 Pd5 Pd2 53.418(11) . . ? C7 P1 C13 102.29(18) . . ? C7 P1 C1 102.46(19) . . ? C13 P1 C1 101.97(19) . . ? C7 P1 Pd1 116.41(14) . . ? C13 P1 Pd1 115.51(14) . . ? C1 P1 Pd1 116.03(14) . . ? C24 P2 C25 103.5(2) . . ? C24 P2 C31 102.2(2) . . ? C25 P2 C31 102.9(2) . . ? C24 P2 Pd2 115.35(18) . . ? C25 P2 Pd2 115.15(16) . . ? C31 P2 Pd2 115.93(15) . . ? C43 P3 C37 100.17(19) . . ? C43 P3 C49 103.79(19) . . ? C37 P3 C49 102.50(19) . . ? C43 P3 Pd3 112.83(14) . . ? C37 P3 Pd3 121.50(14) . . ? C49 P3 Pd3 113.80(14) . . ? C67 P4 C61A 96.0(7) . . ? C67 P4 C55 103.6(3) . . ? C61A P4 C55 103.9(6) . . ? C67 P4 C61B 110.0(8) . . ? C61A P4 C61B 14.4(7) . . ? C55 P4 C61B 96.5(7) . . ? C67 P4 Pd4 112.0(2) . . ? C61A P4 Pd4 123.7(5) . . ? C55 P4 Pd4 114.51(18) . . ? C61B P4 Pd4 118.3(7) . . ? C85 P5 C73 104.79(18) . . ? C85 P5 C79 100.93(18) . . ? C73 P5 C79 102.35(18) . . ? C85 P5 Pd5 112.16(13) . . ? C73 P5 Pd5 113.55(14) . . ? C79 P5 Pd5 121.15(13) . . ? C91 P6 Pd3 158.18(16) . . ? C91 P6 Pd4 60.85(16) . . ? Pd3 P6 Pd4 140.96(5) . . ? C91 P6 Pd1 122.37(16) . . ? Pd3 P6 Pd1 74.96(3) . . ? Pd4 P6 Pd1 71.85(3) . . ? C91 P6 Pd2 122.91(17) . . ? Pd3 P6 Pd2 75.24(3) . . ? Pd4 P6 Pd2 72.04(3) . . ? Pd1 P6 Pd2 63.82(3) . . ? C99 P7 Pd4 159.04(16) . . ? C99 P7 Pd1 122.45(16) . . ? Pd4 P7 Pd1 75.02(3) . . ? C99 P7 Pd5 60.19(15) . . ? Pd4 P7 Pd5 140.73(5) . . ? Pd1 P7 Pd5 72.62(3) . . ? C99 P7 Pd2 122.17(18) . . ? Pd4 P7 Pd2 74.37(3) . . ? Pd1 P7 Pd2 64.06(3) . . ? Pd5 P7 Pd2 71.82(3) . . ? C95 P8 Pd5 158.46(15) . . ? C95 P8 Pd1 122.72(16) . . ? Pd5 P8 Pd1 75.45(3) . . ? C95 P8 Pd3 60.36(14) . . ? Pd5 P8 Pd3 141.12(5) . . ? Pd1 P8 Pd3 72.37(3) . . ? C95 P8 Pd2 122.19(15) . . ? Pd5 P8 Pd2 74.61(3) . . ? Pd1 P8 Pd2 63.86(3) . . ? Pd3 P8 Pd2 71.98(3) . . ? C91 Si1 C94 111.1(2) . . ? C91 Si1 C93 110.0(2) . . ? C94 Si1 C93 107.7(3) . . ? C91 Si1 C92 109.3(2) . . ? C94 Si1 C92 107.6(3) . . ? C93 Si1 C92 111.1(3) . . ? C95 Si2 C97 108.8(2) . . ? C95 Si2 C96 109.6(2) . . ? C97 Si2 C96 109.8(2) . . ? C95 Si2 C98 110.88(19) . . ? C97 Si2 C98 109.8(2) . . ? C96 Si2 C98 108.0(2) . . ? C99 Si3 C102 110.9(2) . . ? C99 Si3 C100 110.1(2) . . ? C102 Si3 C100 109.2(3) . . ? C99 Si3 C101 108.3(2) . . ? C102 Si3 C101 108.8(3) . . ? C100 Si3 C101 109.7(3) . . ? C2 C1 C6 119.0(4) . . ? C2 C1 P1 122.8(3) . . ? C6 C1 P1 118.2(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 118.5(4) . . ? C8 C7 P1 118.2(3) . . ? C12 C7 P1 123.2(3) . . ? C9 C8 C7 120.9(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 119.2(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.6(4) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.4(4) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C14 C13 C18 120.0(4) . . ? C14 C13 P1 117.4(3) . . ? C18 C13 P1 122.6(3) . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 121.5(4) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.3(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 120.0(4) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C24 C19 C20 120.0(6) . . ? C24 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.9(7) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.9(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.8(6) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 121.5(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C19 C24 C23 117.6(5) . . ? C19 C24 P2 122.9(4) . . ? C23 C24 P2 119.5(4) . . ? C26 C25 C30 117.8(5) . . ? C26 C25 P2 118.2(4) . . ? C30 C25 P2 124.0(4) . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.4(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 121.6(7) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 119.5(6) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C29 C30 C25 121.4(6) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? C36 C31 C32 118.9(4) . . ? C36 C31 P2 118.4(4) . . ? C32 C31 P2 122.7(4) . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.6(5) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.8(5) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C31 C36 C35 119.7(5) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C42 C37 C38 119.2(4) . . ? C42 C37 P3 121.1(3) . . ? C38 C37 P3 119.6(4) . . ? C39 C38 C37 120.9(5) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C38 119.8(5) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 120.0(5) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C42 120.9(6) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C37 C42 C41 119.2(5) . . ? C37 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C48 119.2(4) . . ? C44 C43 P3 117.8(3) . . ? C48 C43 P3 123.0(3) . . ? C43 C44 C45 120.2(5) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.6(5) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 119.9(5) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C48 120.6(5) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C43 119.5(4) . . ? C47 C48 H48 120.2 . . ? C43 C48 H48 120.2 . . ? C50 C49 C54 119.2(4) . . ? C50 C49 P3 118.0(3) . . ? C54 C49 P3 122.7(4) . . ? C49 C50 C51 120.4(4) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 120.7(5) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 119.6(5) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C54 C53 C52 120.5(5) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C49 119.6(5) . . ? C53 C54 H54 120.2 . . ? C49 C54 H54 120.2 . . ? C60 C55 C56 120.0(6) . . ? C60 C55 P4 118.2(4) . . ? C56 C55 P4 121.8(5) . . ? C57 C56 C55 120.4(8) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C58 C57 C56 120.1(8) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.9(7) . . ? C57 C58 H58 119.5 . . ? C59 C58 H58 119.5 . . ? C58 C59 C60 119.4(7) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C55 C60 C59 119.1(6) . . ? C55 C60 H60 120.4 . . ? C59 C60 H60 120.4 . . ? C62A C61A C66A 120.0 . . ? C62A C61A P4 124.8(7) . . ? C66A C61A P4 115.0(7) . . ? C61A C62A C63A 120.0 . . ? C61A C62A H62A 120.0 . . ? C63A C62A H62A 120.0 . . ? C64A C63A C62A 120.0 . . ? C64A C63A H63A 120.0 . . ? C62A C63A H63A 120.0 . . ? C63A C64A C65A 120.0 . . ? C63A C64A H64A 120.0 . . ? C65A C64A H64A 120.0 . . ? C66A C65A C64A 120.0 . . ? C66A C65A H65A 120.0 . . ? C64A C65A H65A 120.0 . . ? C65A C66A C61A 120.0 . . ? C65A C66A H66A 120.0 . . ? C61A C66A H66A 120.0 . . ? C72 C67 C68 118.2(7) . . ? C72 C67 P4 118.6(4) . . ? C68 C67 P4 123.2(7) . . ? C62B C61B C66B 120.0 . . ? C62B C61B P4 117.7(9) . . ? C66B C61B P4 122.2(9) . . ? C61B C62B C63B 120.0 . . ? C61B C62B H62B 120.0 . . ? C63B C62B H62B 120.0 . . ? C62B C63B C64B 120.0 . . ? C62B C63B H63B 120.0 . . ? C64B C63B H63B 120.0 . . ? C65B C64B C63B 120.0 . . ? C65B C64B H64B 120.0 . . ? C63B C64B H64B 120.0 . . ? C64B C65B C66B 120.0 . . ? C64B C65B H65B 120.0 . . ? C66B C65B H65B 120.0 . . ? C65B C66B C61B 120.0 . . ? C65B C66B H66B 120.0 . . ? C61B C66B H66B 120.0 . . ? C69 C68 C67 120.4(10) . . ? C69 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C70 C69 C68 120.0(9) . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C70 C71 121.2(11) . . ? C69 C70 H70 119.4 . . ? C71 C70 H70 119.4 . . ? C70 C71 C72 117.5(10) . . ? C70 C71 H71 121.2 . . ? C72 C71 H71 121.2 . . ? C67 C72 C71 122.5(7) . . ? C67 C72 H72 118.7 . . ? C71 C72 H72 118.7 . . ? C78 C73 C74 118.9(4) . . ? C78 C73 P5 118.5(3) . . ? C74 C73 P5 122.6(3) . . ? C75 C74 C73 120.5(4) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 119.8(4) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? C77 C76 C75 119.8(4) . . ? C77 C76 H76 120.1 . . ? C75 C76 H76 120.1 . . ? C76 C77 C78 120.9(4) . . ? C76 C77 H77 119.6 . . ? C78 C77 H77 119.6 . . ? C77 C78 C73 120.1(4) . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? C80 C79 C84 118.8(4) . . ? C80 C79 P5 120.1(3) . . ? C84 C79 P5 120.9(3) . . ? C79 C80 C81 120.8(5) . . ? C79 C80 H80 119.6 . . ? C81 C80 H80 119.6 . . ? C82 C81 C80 119.9(5) . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C83 C82 C81 120.4(4) . . ? C83 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C82 C83 C84 119.7(5) . . ? C82 C83 H83 120.1 . . ? C84 C83 H83 120.1 . . ? C79 C84 C83 120.3(4) . . ? C79 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? C90 C85 C86 118.3(4) . . ? C90 C85 P5 118.9(3) . . ? C86 C85 P5 122.7(3) . . ? C87 C86 C85 120.5(4) . . ? C87 C86 H86 119.8 . . ? C85 C86 H86 119.8 . . ? C88 C87 C86 120.2(4) . . ? C88 C87 H87 119.9 . . ? C86 C87 H87 119.9 . . ? C87 C88 C89 120.5(4) . . ? C87 C88 H88 119.8 . . ? C89 C88 H88 119.8 . . ? C88 C89 C90 119.6(4) . . ? C88 C89 H89 120.2 . . ? C90 C89 H89 120.2 . . ? C89 C90 C85 121.0(4) . . ? C89 C90 H90 119.5 . . ? C85 C90 H90 119.5 . . ? P6 C91 Si1 144.8(3) . . ? P6 C91 Pd4 79.01(17) . . ? Si1 C91 Pd4 136.2(2) . . ? Si1 C92 H92A 109.5 . . ? Si1 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? Si1 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? Si1 C93 H93A 109.5 . . ? Si1 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? Si1 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? Si1 C94 H94A 109.5 . . ? Si1 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? Si1 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? P8 C95 Si2 143.8(3) . . ? P8 C95 Pd3 79.62(16) . . ? Si2 C95 Pd3 136.2(2) . . ? Si2 C96 H96A 109.5 . . ? Si2 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? Si2 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? Si2 C97 H97A 109.5 . . ? Si2 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? Si2 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? Si2 C98 H98A 109.5 . . ? Si2 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? Si2 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? P7 C99 Si3 144.6(3) . . ? P7 C99 Pd5 79.59(16) . . ? Si3 C99 Pd5 135.6(2) . . ? Si3 C100 H10A 109.5 . . ? Si3 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? Si3 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? Si3 C101 H10D 109.5 . . ? Si3 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? Si3 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? Si3 C102 H10G 109.5 . . ? Si3 C102 H10H 109.5 . . ? Si3 C102 H10I 109.5 . . ? C104 C103 C108 120.0 . . ? C104 C103 C109 119.7(3) . . ? C108 C103 C109 120.3(3) . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C106 C105 C104 120.0 . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C105 C106 C107 120.0 . . ? C105 C106 H106 120.0 . . ? C107 C106 H106 120.0 . . ? C106 C107 C108 120.0 . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? C107 C108 C103 120.0 . . ? C107 C108 H108 120.0 . . ? C103 C108 H108 120.0 . . ? C111 C110 C115 120.0 . . ? C111 C110 C116 122.7(13) . . ? C115 C110 C116 117.3(12) . . ? C112 C111 C110 120.0 . . ? C112 C111 H111 120.0 . . ? C110 C111 H111 120.0 . . ? C111 C112 C113 120.0 . . ? C111 C112 H112 120.0 . . ? C113 C112 H112 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C110 120.0 . . ? C114 C115 H115 120.0 . . ? C110 C115 H115 120.0 . . ? C123 C117 C118 123.4(15) . . ? C123 C117 C122 116.3(15) . . ? C118 C117 C122 120.0 . . ? C117 C118 C119 120.0 . . ? C117 C118 H118 120.0 . . ? C119 C118 H118 120.0 . . ? C118 C119 C120 120.0 . . ? C118 C119 H119 120.0 . . ? C120 C119 H119 120.0 . . ? C119 C120 C121 120.0 . . ? C119 C120 H120 120.0 . . ? C121 C120 H120 120.0 . . ? C122 C121 C120 120.0 . . ? C122 C121 H121 120.0 . . ? C120 C121 H121 120.0 . . ? C121 C122 C117 120.0 . . ? C121 C122 H122 120.0 . . ? C117 C122 H122 120.0 . . ? C125 C124 C129 120.0 . . ? C125 C124 C130 110.1(14) . . ? C129 C124 C130 128.8(14) . . ? C126 C125 C124 120.0 . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C127 120.0 . . ? C125 C126 H126 120.0 . . ? C127 C126 H126 120.0 . . ? C128 C127 C126 120.0 . . ? C128 C127 H127 120.0 . . ? C126 C127 H127 120.0 . . ? C127 C128 C129 120.0 . . ? C127 C128 H128 120.0 . . ? C129 C128 H128 120.0 . . ? C128 C129 C124 120.0 . . ? C128 C129 H129 120.0 . . ? C124 C129 H129 120.0 . . ? 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 Pd1 Pd2 P2 63(3) . . . . ? P7 Pd1 Pd2 P2 -7(2) . . . . ? P8 Pd1 Pd2 P2 -127(2) . . . . ? P6 Pd1 Pd2 P2 113(2) . . . . ? Pd4 Pd1 Pd2 P2 51(2) . . . . ? Pd3 Pd1 Pd2 P2 171(15) . . . . ? Pd5 Pd1 Pd2 P2 -69(2) . . . . ? P1 Pd1 Pd2 P6 -49.9(13) . . . . ? P7 Pd1 Pd2 P6 -120.31(4) . . . . ? P8 Pd1 Pd2 P6 119.74(4) . . . . ? Pd4 Pd1 Pd2 P6 -62.32(3) . . . . ? Pd3 Pd1 Pd2 P6 57.36(3) . . . . ? Pd5 Pd1 Pd2 P6 177.18(3) . . . . ? P1 Pd1 Pd2 P7 70.4(13) . . . . ? P8 Pd1 Pd2 P7 -119.95(4) . . . . ? P6 Pd1 Pd2 P7 120.31(4) . . . . ? Pd4 Pd1 Pd2 P7 57.99(3) . . . . ? Pd3 Pd1 Pd2 P7 177.67(3) . . . . ? Pd5 Pd1 Pd2 P7 -62.50(3) . . . . ? P1 Pd1 Pd2 P8 -169.7(13) . . . . ? P7 Pd1 Pd2 P8 119.95(4) . . . . ? P6 Pd1 Pd2 P8 -119.74(4) . . . . ? Pd4 Pd1 Pd2 P8 177.94(3) . . . . ? Pd3 Pd1 Pd2 P8 -62.38(3) . . . . ? Pd5 Pd1 Pd2 P8 57.45(3) . . . . ? P1 Pd1 Pd2 Pd4 12.4(13) . . . . ? P7 Pd1 Pd2 Pd4 -57.99(3) . . . . ? P8 Pd1 Pd2 Pd4 -177.94(3) . . . . ? P6 Pd1 Pd2 Pd4 62.32(3) . . . . ? Pd3 Pd1 Pd2 Pd4 119.680(15) . . . . ? Pd5 Pd1 Pd2 Pd4 -120.497(15) . . . . ? P1 Pd1 Pd2 Pd5 132.9(13) . . . . ? P7 Pd1 Pd2 Pd5 62.50(3) . . . . ? P8 Pd1 Pd2 Pd5 -57.45(3) . . . . ? P6 Pd1 Pd2 Pd5 -177.18(3) . . . . ? Pd4 Pd1 Pd2 Pd5 120.497(15) . . . . ? Pd3 Pd1 Pd2 Pd5 -119.824(15) . . . . ? P1 Pd1 Pd2 Pd3 -107.3(13) . . . . ? P7 Pd1 Pd2 Pd3 -177.67(3) . . . . ? P8 Pd1 Pd2 Pd3 62.38(3) . . . . ? P6 Pd1 Pd2 Pd3 -57.36(3) . . . . ? Pd4 Pd1 Pd2 Pd3 -119.680(15) . . . . ? Pd5 Pd1 Pd2 Pd3 119.824(15) . . . . ? P1 Pd1 Pd3 C95 -91.12(11) . . . . ? P7 Pd1 Pd3 C95 92.56(11) . . . . ? P8 Pd1 Pd3 C95 20.82(11) . . . . ? P6 Pd1 Pd3 C95 159.69(12) . . . . ? Pd2 Pd1 Pd3 C95 90.20(11) . . . . ? Pd4 Pd1 Pd3 C95 142.61(11) . . . . ? Pd5 Pd1 Pd3 C95 37.92(11) . . . . ? P1 Pd1 Pd3 P6 109.19(5) . . . . ? P7 Pd1 Pd3 P6 -67.14(5) . . . . ? P8 Pd1 Pd3 P6 -138.87(5) . . . . ? Pd2 Pd1 Pd3 P6 -69.50(4) . . . . ? Pd4 Pd1 Pd3 P6 -17.09(4) . . . . ? Pd5 Pd1 Pd3 P6 -121.78(4) . . . . ? P1 Pd1 Pd3 P3 50.91(6) . . . . ? P7 Pd1 Pd3 P3 -125.41(6) . . . . ? P8 Pd1 Pd3 P3 162.85(6) . . . . ? P6 Pd1 Pd3 P3 -58.28(6) . . . . ? Pd2 Pd1 Pd3 P3 -127.78(5) . . . . ? Pd4 Pd1 Pd3 P3 -75.36(5) . . . . ? Pd5 Pd1 Pd3 P3 179.95(5) . . . . ? P1 Pd1 Pd3 P8 -111.94(4) . . . . ? P7 Pd1 Pd3 P8 71.74(5) . . . . ? P6 Pd1 Pd3 P8 138.87(5) . . . . ? Pd2 Pd1 Pd3 P8 69.38(3) . . . . ? Pd4 Pd1 Pd3 P8 121.79(3) . . . . ? Pd5 Pd1 Pd3 P8 17.10(3) . . . . ? P1 Pd1 Pd3 Pd2 178.68(3) . . . . ? P7 Pd1 Pd3 Pd2 2.36(3) . . . . ? P8 Pd1 Pd3 Pd2 -69.38(3) . . . . ? P6 Pd1 Pd3 Pd2 69.50(4) . . . . ? Pd4 Pd1 Pd3 Pd2 52.412(14) . . . . ? Pd5 Pd1 Pd3 Pd2 -52.278(15) . . . . ? P2 Pd2 Pd3 C95 91.46(12) . . . . ? P6 Pd2 Pd3 C95 -158.29(12) . . . . ? P7 Pd2 Pd3 C95 -90.97(12) . . . . ? P8 Pd2 Pd3 C95 -21.05(12) . . . . ? Pd1 Pd2 Pd3 C95 -88.71(12) . . . . ? Pd4 Pd2 Pd3 C95 -140.70(12) . . . . ? Pd5 Pd2 Pd3 C95 -36.58(12) . . . . ? P2 Pd2 Pd3 P6 -110.25(5) . . . . ? P7 Pd2 Pd3 P6 67.32(5) . . . . ? P8 Pd2 Pd3 P6 137.24(5) . . . . ? Pd1 Pd2 Pd3 P6 69.58(4) . . . . ? Pd4 Pd2 Pd3 P6 17.59(4) . . . . ? Pd5 Pd2 Pd3 P6 121.71(4) . . . . ? P2 Pd2 Pd3 P3 -45.52(6) . . . . ? P6 Pd2 Pd3 P3 64.73(6) . . . . ? P7 Pd2 Pd3 P3 132.05(5) . . . . ? P8 Pd2 Pd3 P3 -158.03(6) . . . . ? Pd1 Pd2 Pd3 P3 134.31(5) . . . . ? Pd4 Pd2 Pd3 P3 82.32(5) . . . . ? Pd5 Pd2 Pd3 P3 -173.56(5) . . . . ? P2 Pd2 Pd3 P8 112.51(5) . . . . ? P6 Pd2 Pd3 P8 -137.24(5) . . . . ? P7 Pd2 Pd3 P8 -69.92(4) . . . . ? Pd1 Pd2 Pd3 P8 -67.66(3) . . . . ? Pd4 Pd2 Pd3 P8 -119.65(3) . . . . ? Pd5 Pd2 Pd3 P8 -15.53(3) . . . . ? P2 Pd2 Pd3 Pd1 -179.83(4) . . . . ? P6 Pd2 Pd3 Pd1 -69.58(4) . . . . ? P7 Pd2 Pd3 Pd1 -2.26(3) . . . . ? P8 Pd2 Pd3 Pd1 67.66(3) . . . . ? Pd4 Pd2 Pd3 Pd1 -51.988(13) . . . . ? Pd5 Pd2 Pd3 Pd1 52.129(13) . . . . ? P1 Pd1 Pd4 C91 -89.84(12) . . . . ? P7 Pd1 Pd4 C91 160.28(13) . . . . ? P8 Pd1 Pd4 C91 91.95(12) . . . . ? P6 Pd1 Pd4 C91 21.20(12) . . . . ? Pd2 Pd1 Pd4 C91 89.87(12) . . . . ? Pd3 Pd1 Pd4 C91 37.33(12) . . . . ? Pd5 Pd1 Pd4 C91 141.74(12) . . . . ? P1 Pd1 Pd4 P4 53.58(8) . . . . ? P7 Pd1 Pd4 P4 -56.31(8) . . . . ? P8 Pd1 Pd4 P4 -124.63(8) . . . . ? P6 Pd1 Pd4 P4 164.62(8) . . . . ? Pd2 Pd1 Pd4 P4 -126.72(7) . . . . ? Pd3 Pd1 Pd4 P4 -179.25(7) . . . . ? Pd5 Pd1 Pd4 P4 -74.85(7) . . . . ? P1 Pd1 Pd4 P7 109.89(5) . . . . ? P8 Pd1 Pd4 P7 -68.32(5) . . . . ? P6 Pd1 Pd4 P7 -139.07(5) . . . . ? Pd2 Pd1 Pd4 P7 -70.41(4) . . . . ? Pd3 Pd1 Pd4 P7 -122.94(4) . . . . ? Pd5 Pd1 Pd4 P7 -18.54(4) . . . . ? P1 Pd1 Pd4 P6 -111.04(5) . . . . ? P7 Pd1 Pd4 P6 139.07(5) . . . . ? P8 Pd1 Pd4 P6 70.75(5) . . . . ? Pd2 Pd1 Pd4 P6 68.67(4) . . . . ? Pd3 Pd1 Pd4 P6 16.13(4) . . . . ? Pd5 Pd1 Pd4 P6 120.54(4) . . . . ? P1 Pd1 Pd4 Pd2 -179.71(3) . . . . ? P7 Pd1 Pd4 Pd2 70.41(4) . . . . ? P8 Pd1 Pd4 Pd2 2.08(3) . . . . ? P6 Pd1 Pd4 Pd2 -68.67(4) . . . . ? Pd3 Pd1 Pd4 Pd2 -52.535(15) . . . . ? Pd5 Pd1 Pd4 Pd2 51.871(14) . . . . ? P2 Pd2 Pd4 C91 91.37(12) . . . . ? P6 Pd2 Pd4 C91 -20.80(12) . . . . ? P7 Pd2 Pd4 C91 -157.76(12) . . . . ? P8 Pd2 Pd4 C91 -91.43(12) . . . . ? Pd1 Pd2 Pd4 C91 -89.43(12) . . . . ? Pd5 Pd2 Pd4 C91 -141.17(12) . . . . ? Pd3 Pd2 Pd4 C91 -37.39(12) . . . . ? P2 Pd2 Pd4 P4 -43.50(6) . . . . ? P6 Pd2 Pd4 P4 -155.67(6) . . . . ? P7 Pd2 Pd4 P4 67.36(6) . . . . ? P8 Pd2 Pd4 P4 133.69(6) . . . . ? Pd1 Pd2 Pd4 P4 135.69(5) . . . . ? Pd5 Pd2 Pd4 P4 83.95(5) . . . . ? Pd3 Pd2 Pd4 P4 -172.27(5) . . . . ? P2 Pd2 Pd4 P7 -110.87(5) . . . . ? P6 Pd2 Pd4 P7 136.96(5) . . . . ? P8 Pd2 Pd4 P7 66.33(4) . . . . ? Pd1 Pd2 Pd4 P7 68.33(3) . . . . ? Pd5 Pd2 Pd4 P7 16.59(3) . . . . ? Pd3 Pd2 Pd4 P7 120.37(4) . . . . ? P2 Pd2 Pd4 P6 112.17(5) . . . . ? P7 Pd2 Pd4 P6 -136.96(5) . . . . ? P8 Pd2 Pd4 P6 -70.63(4) . . . . ? Pd1 Pd2 Pd4 P6 -68.63(3) . . . . ? Pd5 Pd2 Pd4 P6 -120.37(3) . . . . ? Pd3 Pd2 Pd4 P6 -16.59(3) . . . . ? P2 Pd2 Pd4 Pd1 -179.19(3) . . . . ? P6 Pd2 Pd4 Pd1 68.63(3) . . . . ? P7 Pd2 Pd4 Pd1 -68.33(3) . . . . ? P8 Pd2 Pd4 Pd1 -2.00(3) . . . . ? Pd5 Pd2 Pd4 Pd1 -51.737(13) . . . . ? Pd3 Pd2 Pd4 Pd1 52.040(14) . . . . ? P1 Pd1 Pd5 C99 -88.20(12) . . . . ? P7 Pd1 Pd5 C99 21.28(12) . . . . ? P8 Pd1 Pd5 C99 161.37(12) . . . . ? P6 Pd1 Pd5 C99 93.59(12) . . . . ? Pd2 Pd1 Pd5 C99 90.78(12) . . . . ? Pd4 Pd1 Pd5 C99 38.87(12) . . . . ? Pd3 Pd1 Pd5 C99 143.23(12) . . . . ? P1 Pd1 Pd5 P8 110.43(4) . . . . ? P7 Pd1 Pd5 P8 -140.09(5) . . . . ? P6 Pd1 Pd5 P8 -67.78(5) . . . . ? Pd2 Pd1 Pd5 P8 -70.59(3) . . . . ? Pd4 Pd1 Pd5 P8 -122.50(3) . . . . ? Pd3 Pd1 Pd5 P8 -18.15(3) . . . . ? P1 Pd1 Pd5 P5 56.97(6) . . . . ? P7 Pd1 Pd5 P5 166.46(6) . . . . ? P8 Pd1 Pd5 P5 -53.45(6) . . . . ? P6 Pd1 Pd5 P5 -121.24(6) . . . . ? Pd2 Pd1 Pd5 P5 -124.04(5) . . . . ? Pd4 Pd1 Pd5 P5 -175.96(5) . . . . ? Pd3 Pd1 Pd5 P5 -71.60(5) . . . . ? P1 Pd1 Pd5 P7 -109.48(5) . . . . ? P8 Pd1 Pd5 P7 140.09(5) . . . . ? P6 Pd1 Pd5 P7 72.31(5) . . . . ? Pd2 Pd1 Pd5 P7 69.50(4) . . . . ? Pd4 Pd1 Pd5 P7 17.59(4) . . . . ? Pd3 Pd1 Pd5 P7 121.94(4) . . . . ? P1 Pd1 Pd5 Pd2 -178.98(3) . . . . ? P7 Pd1 Pd5 Pd2 -69.50(4) . . . . ? P8 Pd1 Pd5 Pd2 70.59(3) . . . . ? P6 Pd1 Pd5 Pd2 2.81(3) . . . . ? Pd4 Pd1 Pd5 Pd2 -51.914(14) . . . . ? Pd3 Pd1 Pd5 Pd2 52.444(14) . . . . ? P2 Pd2 Pd5 C99 90.87(13) . . . . ? P6 Pd2 Pd5 C99 -90.95(13) . . . . ? P7 Pd2 Pd5 C99 -20.88(13) . . . . ? P8 Pd2 Pd5 C99 -156.61(13) . . . . ? Pd1 Pd2 Pd5 C99 -88.16(12) . . . . ? Pd4 Pd2 Pd5 C99 -36.60(12) . . . . ? Pd3 Pd2 Pd5 C99 -140.17(12) . . . . ? P2 Pd2 Pd5 P8 -112.52(5) . . . . ? P6 Pd2 Pd5 P8 65.66(5) . . . . ? P7 Pd2 Pd5 P8 135.73(5) . . . . ? Pd1 Pd2 Pd5 P8 68.45(4) . . . . ? Pd4 Pd2 Pd5 P8 120.01(4) . . . . ? Pd3 Pd2 Pd5 P8 16.44(4) . . . . ? P2 Pd2 Pd5 P5 -44.01(5) . . . . ? P6 Pd2 Pd5 P5 134.17(5) . . . . ? P7 Pd2 Pd5 P5 -155.76(5) . . . . ? P8 Pd2 Pd5 P5 68.51(5) . . . . ? Pd1 Pd2 Pd5 P5 136.96(4) . . . . ? Pd4 Pd2 Pd5 P5 -171.48(4) . . . . ? Pd3 Pd2 Pd5 P5 84.96(4) . . . . ? P2 Pd2 Pd5 P7 111.75(5) . . . . ? P6 Pd2 Pd5 P7 -70.07(4) . . . . ? P8 Pd2 Pd5 P7 -135.73(5) . . . . ? Pd1 Pd2 Pd5 P7 -67.28(3) . . . . ? Pd4 Pd2 Pd5 P7 -15.72(3) . . . . ? Pd3 Pd2 Pd5 P7 -119.28(3) . . . . ? P2 Pd2 Pd5 Pd1 179.03(4) . . . . ? P6 Pd2 Pd5 Pd1 -2.79(3) . . . . ? P7 Pd2 Pd5 Pd1 67.28(3) . . . . ? P8 Pd2 Pd5 Pd1 -68.45(4) . . . . ? Pd4 Pd2 Pd5 Pd1 51.561(14) . . . . ? Pd3 Pd2 Pd5 Pd1 -52.002(14) . . . . ? P7 Pd1 P1 C7 -64.72(15) . . . . ? P8 Pd1 P1 C7 56.05(15) . . . . ? P6 Pd1 P1 C7 176.23(15) . . . . ? Pd2 Pd1 P1 C7 -134.4(13) . . . . ? Pd4 Pd1 P1 C7 -122.15(15) . . . . ? Pd3 Pd1 P1 C7 118.88(15) . . . . ? Pd5 Pd1 P1 C7 -1.99(15) . . . . ? P7 Pd1 P1 C13 175.25(15) . . . . ? P8 Pd1 P1 C13 -63.97(15) . . . . ? P6 Pd1 P1 C13 56.20(15) . . . . ? Pd2 Pd1 P1 C13 105.6(13) . . . . ? Pd4 Pd1 P1 C13 117.82(15) . . . . ? Pd3 Pd1 P1 C13 -1.14(15) . . . . ? Pd5 Pd1 P1 C13 -122.02(15) . . . . ? P7 Pd1 P1 C1 55.98(15) . . . . ? P8 Pd1 P1 C1 176.76(14) . . . . ? P6 Pd1 P1 C1 -63.07(15) . . . . ? Pd2 Pd1 P1 C1 -13.7(14) . . . . ? Pd4 Pd1 P1 C1 -1.45(15) . . . . ? Pd3 Pd1 P1 C1 -120.41(14) . . . . ? Pd5 Pd1 P1 C1 118.71(14) . . . . ? P6 Pd2 P2 C24 55.4(2) . . . . ? P7 Pd2 P2 C24 -64.3(2) . . . . ? P8 Pd2 P2 C24 176.20(19) . . . . ? Pd1 Pd2 P2 C24 -57(2) . . . . ? Pd4 Pd2 P2 C24 -6.7(2) . . . . ? Pd5 Pd2 P2 C24 -126.41(19) . . . . ? Pd3 Pd2 P2 C24 113.26(19) . . . . ? P6 Pd2 P2 C25 -65.04(18) . . . . ? P7 Pd2 P2 C25 175.25(17) . . . . ? P8 Pd2 P2 C25 55.72(18) . . . . ? Pd1 Pd2 P2 C25 -178(100) . . . . ? Pd4 Pd2 P2 C25 -127.19(17) . . . . ? Pd5 Pd2 P2 C25 113.11(17) . . . . ? Pd3 Pd2 P2 C25 -7.22(18) . . . . ? P6 Pd2 P2 C31 174.85(16) . . . . ? P7 Pd2 P2 C31 55.14(17) . . . . ? P8 Pd2 P2 C31 -64.39(17) . . . . ? Pd1 Pd2 P2 C31 62(2) . . . . ? Pd4 Pd2 P2 C31 112.70(17) . . . . ? Pd5 Pd2 P2 C31 -7.00(17) . . . . ? Pd3 Pd2 P2 C31 -127.33(16) . . . . ? C95 Pd3 P3 C43 -130.0(2) . . . . ? P6 Pd3 P3 C43 48.61(16) . . . . ? P8 Pd3 P3 C43 -125.54(17) . . . . ? Pd1 Pd3 P3 C43 94.30(16) . . . . ? Pd2 Pd3 P3 C43 -0.88(17) . . . . ? C95 Pd3 P3 C37 -11.2(2) . . . . ? P6 Pd3 P3 C37 167.47(17) . . . . ? P8 Pd3 P3 C37 -6.7(2) . . . . ? Pd1 Pd3 P3 C37 -146.84(17) . . . . ? Pd2 Pd3 P3 C37 117.97(17) . . . . ? C95 Pd3 P3 C49 112.02(19) . . . . ? P6 Pd3 P3 C49 -69.32(15) . . . . ? P8 Pd3 P3 C49 116.53(17) . . . . ? Pd1 Pd3 P3 C49 -23.63(16) . . . . ? Pd2 Pd3 P3 C49 -118.81(15) . . . . ? C91 Pd4 P4 C67 -131.7(2) . . . . ? P7 Pd4 P4 C67 46.6(2) . . . . ? P6 Pd4 P4 C67 -123.7(2) . . . . ? Pd1 Pd4 P4 C67 90.6(2) . . . . ? Pd2 Pd4 P4 C67 -4.9(2) . . . . ? C91 Pd4 P4 C61A -17.7(9) . . . . ? P7 Pd4 P4 C61A 160.5(9) . . . . ? P6 Pd4 P4 C61A -9.7(9) . . . . ? Pd1 Pd4 P4 C61A -155.4(9) . . . . ? Pd2 Pd4 P4 C61A 109.1(9) . . . . ? C91 Pd4 P4 C55 110.7(3) . . . . ? P7 Pd4 P4 C55 -71.1(2) . . . . ? P6 Pd4 P4 C55 118.7(2) . . . . ? Pd1 Pd4 P4 C55 -27.0(2) . . . . ? Pd2 Pd4 P4 C55 -122.5(2) . . . . ? C91 Pd4 P4 C61B -2.1(9) . . . . ? P7 Pd4 P4 C61B 176.2(9) . . . . ? P6 Pd4 P4 C61B 5.9(9) . . . . ? Pd1 Pd4 P4 C61B -139.8(9) . . . . ? Pd2 Pd4 P4 C61B 124.7(9) . . . . ? C99 Pd5 P5 C85 -129.55(19) . . . . ? P8 Pd5 P5 C85 48.78(13) . . . . ? P7 Pd5 P5 C85 -119.37(16) . . . . ? Pd1 Pd5 P5 C85 90.92(14) . . . . ? Pd2 Pd5 P5 C85 -3.22(14) . . . . ? C99 Pd5 P5 C73 111.89(19) . . . . ? P8 Pd5 P5 C73 -69.78(14) . . . . ? P7 Pd5 P5 C73 122.08(16) . . . . ? Pd1 Pd5 P5 C73 -27.64(15) . . . . ? Pd2 Pd5 P5 C73 -121.78(14) . . . . ? C99 Pd5 P5 C79 -10.5(2) . . . . ? P8 Pd5 P5 C79 167.82(16) . . . . ? P7 Pd5 P5 C79 -0.3(2) . . . . ? Pd1 Pd5 P5 C79 -150.05(16) . . . . ? Pd2 Pd5 P5 C79 115.82(16) . . . . ? C95 Pd3 P6 C91 -177.1(5) . . . . ? P3 Pd3 P6 C91 4.7(5) . . . . ? P8 Pd3 P6 C91 -177.5(5) . . . . ? Pd1 Pd3 P6 C91 -145.1(5) . . . . ? Pd2 Pd3 P6 C91 148.6(5) . . . . ? C95 Pd3 P6 Pd4 0.6(2) . . . . ? P3 Pd3 P6 Pd4 -177.64(8) . . . . ? P8 Pd3 P6 Pd4 0.18(9) . . . . ? Pd1 Pd3 P6 Pd4 32.52(7) . . . . ? Pd2 Pd3 P6 Pd4 -33.79(7) . . . . ? C95 Pd3 P6 Pd1 -31.96(18) . . . . ? P3 Pd3 P6 Pd1 149.84(3) . . . . ? P8 Pd3 P6 Pd1 -32.35(4) . . . . ? Pd2 Pd3 P6 Pd1 -66.32(2) . . . . ? C95 Pd3 P6 Pd2 34.36(18) . . . . ? P3 Pd3 P6 Pd2 -143.84(3) . . . . ? P8 Pd3 P6 Pd2 33.97(4) . . . . ? Pd1 Pd3 P6 Pd2 66.32(2) . . . . ? P4 Pd4 P6 C91 -11.0(2) . . . . ? P7 Pd4 P6 C91 178.60(19) . . . . ? Pd1 Pd4 P6 C91 145.87(19) . . . . ? Pd2 Pd4 P6 C91 -146.58(19) . . . . ? C91 Pd4 P6 Pd3 -179.0(2) . . . . ? P4 Pd4 P6 Pd3 170.01(10) . . . . ? P7 Pd4 P6 Pd3 -0.39(9) . . . . ? Pd1 Pd4 P6 Pd3 -33.12(7) . . . . ? Pd2 Pd4 P6 Pd3 34.43(7) . . . . ? C91 Pd4 P6 Pd1 -145.87(19) . . . . ? P4 Pd4 P6 Pd1 -156.87(12) . . . . ? P7 Pd4 P6 Pd1 32.73(4) . . . . ? Pd2 Pd4 P6 Pd1 67.55(2) . . . . ? C91 Pd4 P6 Pd2 146.58(19) . . . . ? P4 Pd4 P6 Pd2 135.58(12) . . . . ? P7 Pd4 P6 Pd2 -34.82(4) . . . . ? Pd1 Pd4 P6 Pd2 -67.55(2) . . . . ? P1 Pd1 P6 C91 65.0(2) . . . . ? P7 Pd1 P6 C91 -65.9(2) . . . . ? P8 Pd1 P6 C91 -162.2(2) . . . . ? Pd2 Pd1 P6 C91 -113.9(2) . . . . ? Pd4 Pd1 P6 C91 -35.5(2) . . . . ? Pd3 Pd1 P6 C91 165.4(2) . . . . ? Pd5 Pd1 P6 C91 -116.9(2) . . . . ? P1 Pd1 P6 Pd3 -100.42(4) . . . . ? P7 Pd1 P6 Pd3 128.64(4) . . . . ? P8 Pd1 P6 Pd3 32.37(4) . . . . ? Pd2 Pd1 P6 Pd3 80.68(3) . . . . ? Pd4 Pd1 P6 Pd3 159.12(4) . . . . ? Pd5 Pd1 P6 Pd3 77.73(3) . . . . ? P1 Pd1 P6 Pd4 100.46(4) . . . . ? P7 Pd1 P6 Pd4 -30.48(4) . . . . ? P8 Pd1 P6 Pd4 -126.75(3) . . . . ? Pd2 Pd1 P6 Pd4 -78.44(3) . . . . ? Pd3 Pd1 P6 Pd4 -159.12(4) . . . . ? Pd5 Pd1 P6 Pd4 -81.39(3) . . . . ? P1 Pd1 P6 Pd2 178.90(3) . . . . ? P7 Pd1 P6 Pd2 47.96(3) . . . . ? P8 Pd1 P6 Pd2 -48.30(3) . . . . ? Pd4 Pd1 P6 Pd2 78.44(3) . . . . ? Pd3 Pd1 P6 Pd2 -80.68(3) . . . . ? Pd5 Pd1 P6 Pd2 -2.95(3) . . . . ? P2 Pd2 P6 C91 -65.9(2) . . . . ? P7 Pd2 P6 C91 66.5(2) . . . . ? P8 Pd2 P6 C91 160.1(2) . . . . ? Pd1 Pd2 P6 C91 113.1(2) . . . . ? Pd4 Pd2 P6 C91 34.96(19) . . . . ? Pd5 Pd2 P6 C91 116.04(19) . . . . ? Pd3 Pd2 P6 C91 -166.7(2) . . . . ? P2 Pd2 P6 Pd3 100.76(5) . . . . ? P7 Pd2 P6 Pd3 -126.80(3) . . . . ? P8 Pd2 P6 Pd3 -33.22(4) . . . . ? Pd1 Pd2 P6 Pd3 -80.25(3) . . . . ? Pd4 Pd2 P6 Pd3 -158.39(4) . . . . ? Pd5 Pd2 P6 Pd3 -77.31(3) . . . . ? P2 Pd2 P6 Pd4 -100.85(5) . . . . ? P7 Pd2 P6 Pd4 31.59(3) . . . . ? P8 Pd2 P6 Pd4 125.16(3) . . . . ? Pd1 Pd2 P6 Pd4 78.14(3) . . . . ? Pd5 Pd2 P6 Pd4 81.08(3) . . . . ? Pd3 Pd2 P6 Pd4 158.39(4) . . . . ? P2 Pd2 P6 Pd1 -178.99(4) . . . . ? P7 Pd2 P6 Pd1 -46.56(3) . . . . ? P8 Pd2 P6 Pd1 47.02(3) . . . . ? Pd4 Pd2 P6 Pd1 -78.14(3) . . . . ? Pd5 Pd2 P6 Pd1 2.94(3) . . . . ? Pd3 Pd2 P6 Pd1 80.25(3) . . . . ? C91 Pd4 P7 C99 -179.9(5) . . . . ? P4 Pd4 P7 C99 2.5(5) . . . . ? P6 Pd4 P7 C99 178.7(5) . . . . ? Pd1 Pd4 P7 C99 -148.7(5) . . . . ? Pd2 Pd4 P7 C99 144.6(5) . . . . ? C91 Pd4 P7 Pd1 -31.20(19) . . . . ? P4 Pd4 P7 Pd1 151.16(4) . . . . ? P6 Pd4 P7 Pd1 -32.58(4) . . . . ? Pd2 Pd4 P7 Pd1 -66.71(2) . . . . ? C91 Pd4 P7 Pd5 4.1(2) . . . . ? P4 Pd4 P7 Pd5 -173.49(8) . . . . ? P6 Pd4 P7 Pd5 2.76(9) . . . . ? Pd1 Pd4 P7 Pd5 35.34(6) . . . . ? Pd2 Pd4 P7 Pd5 -31.37(7) . . . . ? C91 Pd4 P7 Pd2 35.51(19) . . . . ? P4 Pd4 P7 Pd2 -142.12(4) . . . . ? P6 Pd4 P7 Pd2 34.13(4) . . . . ? Pd1 Pd4 P7 Pd2 66.71(2) . . . . ? P1 Pd1 P7 C99 68.3(2) . . . . ? P8 Pd1 P7 C99 -64.9(2) . . . . ? P6 Pd1 P7 C99 -160.6(2) . . . . ? Pd2 Pd1 P7 C99 -113.1(2) . . . . ? Pd4 Pd1 P7 C99 167.3(2) . . . . ? Pd3 Pd1 P7 C99 -115.6(2) . . . . ? Pd5 Pd1 P7 C99 -35.3(2) . . . . ? P1 Pd1 P7 Pd4 -99.02(4) . . . . ? P8 Pd1 P7 Pd4 127.86(4) . . . . ? P6 Pd1 P7 Pd4 32.13(4) . . . . ? Pd2 Pd1 P7 Pd4 79.63(3) . . . . ? Pd3 Pd1 P7 Pd4 77.16(4) . . . . ? Pd5 Pd1 P7 Pd4 157.44(4) . . . . ? P1 Pd1 P7 Pd5 103.54(4) . . . . ? P8 Pd1 P7 Pd5 -29.57(3) . . . . ? P6 Pd1 P7 Pd5 -125.30(4) . . . . ? Pd2 Pd1 P7 Pd5 -77.81(3) . . . . ? Pd4 Pd1 P7 Pd5 -157.44(4) . . . . ? Pd3 Pd1 P7 Pd5 -80.28(3) . . . . ? P1 Pd1 P7 Pd2 -178.65(3) . . . . ? P8 Pd1 P7 Pd2 48.23(3) . . . . ? P6 Pd1 P7 Pd2 -47.50(3) . . . . ? Pd4 Pd1 P7 Pd2 -79.63(3) . . . . ? Pd3 Pd1 P7 Pd2 -2.47(3) . . . . ? Pd5 Pd1 P7 Pd2 77.81(3) . . . . ? P8 Pd5 P7 C99 177.77(19) . . . . ? P5 Pd5 P7 C99 -13.9(2) . . . . ? Pd1 Pd5 P7 C99 145.8(2) . . . . ? Pd2 Pd5 P7 C99 -146.5(2) . . . . ? C99 Pd5 P7 Pd4 178.3(2) . . . . ? P8 Pd5 P7 Pd4 -3.89(9) . . . . ? P5 Pd5 P7 Pd4 164.40(8) . . . . ? Pd1 Pd5 P7 Pd4 -35.84(7) . . . . ? Pd2 Pd5 P7 Pd4 31.85(7) . . . . ? C99 Pd5 P7 Pd1 -145.8(2) . . . . ? P8 Pd5 P7 Pd1 31.96(4) . . . . ? P5 Pd5 P7 Pd1 -159.75(9) . . . . ? Pd2 Pd5 P7 Pd1 67.69(2) . . . . ? C99 Pd5 P7 Pd2 146.5(2) . . . . ? P8 Pd5 P7 Pd2 -35.73(4) . . . . ? P5 Pd5 P7 Pd2 132.56(10) . . . . ? Pd1 Pd5 P7 Pd2 -67.69(2) . . . . ? P2 Pd2 P7 C99 -66.62(19) . . . . ? P6 Pd2 P7 C99 160.70(19) . . . . ? P8 Pd2 P7 C99 66.65(19) . . . . ? Pd1 Pd2 P7 C99 113.51(19) . . . . ? Pd4 Pd2 P7 C99 -165.83(19) . . . . ? Pd5 Pd2 P7 C99 34.46(18) . . . . ? Pd3 Pd2 P7 C99 115.91(18) . . . . ? P2 Pd2 P7 Pd4 99.21(5) . . . . ? P6 Pd2 P7 Pd4 -33.47(3) . . . . ? P8 Pd2 P7 Pd4 -127.52(3) . . . . ? Pd1 Pd2 P7 Pd4 -80.66(3) . . . . ? Pd5 Pd2 P7 Pd4 -159.71(4) . . . . ? Pd3 Pd2 P7 Pd4 -78.26(3) . . . . ? P2 Pd2 P7 Pd1 179.87(4) . . . . ? P6 Pd2 P7 Pd1 47.19(3) . . . . ? P8 Pd2 P7 Pd1 -46.86(3) . . . . ? Pd4 Pd2 P7 Pd1 80.66(3) . . . . ? Pd5 Pd2 P7 Pd1 -79.05(3) . . . . ? Pd3 Pd2 P7 Pd1 2.40(3) . . . . ? P2 Pd2 P7 Pd5 -101.08(4) . . . . ? P6 Pd2 P7 Pd5 126.24(3) . . . . ? P8 Pd2 P7 Pd5 32.19(3) . . . . ? Pd1 Pd2 P7 Pd5 79.05(3) . . . . ? Pd4 Pd2 P7 Pd5 159.71(4) . . . . ? Pd3 Pd2 P7 Pd5 81.45(3) . . . . ? C99 Pd5 P8 C95 -178.9(5) . . . . ? P5 Pd5 P8 C95 3.4(5) . . . . ? P7 Pd5 P8 C95 178.9(5) . . . . ? Pd1 Pd5 P8 C95 -149.8(5) . . . . ? Pd2 Pd5 P8 C95 143.9(5) . . . . ? C99 Pd5 P8 Pd1 -29.13(19) . . . . ? P5 Pd5 P8 Pd1 153.11(3) . . . . ? P7 Pd5 P8 Pd1 -31.32(4) . . . . ? Pd2 Pd5 P8 Pd1 -66.38(2) . . . . ? C99 Pd5 P8 Pd3 5.7(2) . . . . ? P5 Pd5 P8 Pd3 -172.02(7) . . . . ? P7 Pd5 P8 Pd3 3.54(9) . . . . ? Pd1 Pd5 P8 Pd3 34.86(6) . . . . ? Pd2 Pd5 P8 Pd3 -31.51(6) . . . . ? C99 Pd5 P8 Pd2 37.25(19) . . . . ? P5 Pd5 P8 Pd2 -140.51(3) . . . . ? P7 Pd5 P8 Pd2 35.06(4) . . . . ? Pd1 Pd5 P8 Pd2 66.38(2) . . . . ? P1 Pd1 P8 C95 66.79(19) . . . . ? P7 Pd1 P8 C95 -161.17(18) . . . . ? P6 Pd1 P8 C95 -65.12(18) . . . . ? Pd2 Pd1 P8 C95 -112.95(18) . . . . ? Pd4 Pd1 P8 C95 -115.13(18) . . . . ? Pd3 Pd1 P8 C95 -34.81(18) . . . . ? Pd5 Pd1 P8 C95 167.30(19) . . . . ? P1 Pd1 P8 Pd5 -100.51(4) . . . . ? P7 Pd1 P8 Pd5 31.53(4) . . . . ? P6 Pd1 P8 Pd5 127.57(3) . . . . ? Pd2 Pd1 P8 Pd5 79.75(3) . . . . ? Pd4 Pd1 P8 Pd5 77.57(3) . . . . ? Pd3 Pd1 P8 Pd5 157.89(4) . . . . ? P1 Pd1 P8 Pd3 101.60(4) . . . . ? P7 Pd1 P8 Pd3 -126.36(3) . . . . ? P6 Pd1 P8 Pd3 -30.31(3) . . . . ? Pd2 Pd1 P8 Pd3 -78.14(2) . . . . ? Pd4 Pd1 P8 Pd3 -80.31(3) . . . . ? Pd5 Pd1 P8 Pd3 -157.89(4) . . . . ? P1 Pd1 P8 Pd2 179.74(3) . . . . ? P7 Pd1 P8 Pd2 -48.22(3) . . . . ? P6 Pd1 P8 Pd2 47.83(3) . . . . ? Pd4 Pd1 P8 Pd2 -2.18(3) . . . . ? Pd3 Pd1 P8 Pd2 78.14(2) . . . . ? Pd5 Pd1 P8 Pd2 -79.75(3) . . . . ? P6 Pd3 P8 C95 179.61(18) . . . . ? P3 Pd3 P8 C95 -6.2(2) . . . . ? Pd1 Pd3 P8 C95 146.46(18) . . . . ? Pd2 Pd3 P8 C95 -146.05(18) . . . . ? C95 Pd3 P8 Pd5 178.1(2) . . . . ? P6 Pd3 P8 Pd5 -2.34(9) . . . . ? P3 Pd3 P8 Pd5 171.88(8) . . . . ? Pd1 Pd3 P8 Pd5 -35.49(6) . . . . ? Pd2 Pd3 P8 Pd5 32.00(6) . . . . ? C95 Pd3 P8 Pd1 -146.46(18) . . . . ? P6 Pd3 P8 Pd1 33.15(4) . . . . ? P3 Pd3 P8 Pd1 -152.63(9) . . . . ? Pd2 Pd3 P8 Pd1 67.49(2) . . . . ? C95 Pd3 P8 Pd2 146.05(18) . . . . ? P6 Pd3 P8 Pd2 -34.34(4) . . . . ? P3 Pd3 P8 Pd2 139.88(9) . . . . ? Pd1 Pd3 P8 Pd2 -67.49(2) . . . . ? P2 Pd2 P8 C95 -67.1(2) . . . . ? P6 Pd2 P8 C95 66.2(2) . . . . ? P7 Pd2 P8 C95 160.5(2) . . . . ? Pd1 Pd2 P8 C95 113.7(2) . . . . ? Pd4 Pd2 P8 C95 115.86(19) . . . . ? Pd5 Pd2 P8 C95 -165.2(2) . . . . ? Pd3 Pd2 P8 C95 35.00(19) . . . . ? P2 Pd2 P8 Pd5 98.04(5) . . . . ? P6 Pd2 P8 Pd5 -128.61(4) . . . . ? P7 Pd2 P8 Pd5 -34.34(4) . . . . ? Pd1 Pd2 P8 Pd5 -81.07(3) . . . . ? Pd4 Pd2 P8 Pd5 -78.95(3) . . . . ? Pd3 Pd2 P8 Pd5 -159.82(4) . . . . ? P2 Pd2 P8 Pd1 179.11(4) . . . . ? P6 Pd2 P8 Pd1 -47.53(3) . . . . ? P7 Pd2 P8 Pd1 46.73(3) . . . . ? Pd4 Pd2 P8 Pd1 2.12(3) . . . . ? Pd5 Pd2 P8 Pd1 81.07(3) . . . . ? Pd3 Pd2 P8 Pd1 -78.75(3) . . . . ? P2 Pd2 P8 Pd3 -102.14(4) . . . . ? P6 Pd2 P8 Pd3 31.21(3) . . . . ? P7 Pd2 P8 Pd3 125.48(3) . . . . ? Pd1 Pd2 P8 Pd3 78.75(3) . . . . ? Pd4 Pd2 P8 Pd3 80.86(3) . . . . ? Pd5 Pd2 P8 Pd3 159.82(4) . . . . ? C7 P1 C1 C2 -11.9(4) . . . . ? C13 P1 C1 C2 93.7(4) . . . . ? Pd1 P1 C1 C2 -139.9(3) . . . . ? C7 P1 C1 C6 169.4(3) . . . . ? C13 P1 C1 C6 -85.0(4) . . . . ? Pd1 P1 C1 C6 41.4(4) . . . . ? C6 C1 C2 C3 0.8(7) . . . . ? P1 C1 C2 C3 -177.8(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C2 C3 C4 C5 -1.5(7) . . . . ? C3 C4 C5 C6 1.0(8) . . . . ? C4 C5 C6 C1 0.4(7) . . . . ? C2 C1 C6 C5 -1.3(7) . . . . ? P1 C1 C6 C5 177.4(4) . . . . ? C13 P1 C7 C8 170.4(4) . . . . ? C1 P1 C7 C8 -84.2(4) . . . . ? Pd1 P1 C7 C8 43.5(4) . . . . ? C13 P1 C7 C12 -12.1(4) . . . . ? C1 P1 C7 C12 93.3(4) . . . . ? Pd1 P1 C7 C12 -139.0(3) . . . . ? C12 C7 C8 C9 -1.2(7) . . . . ? P1 C7 C8 C9 176.4(4) . . . . ? C7 C8 C9 C10 0.9(8) . . . . ? C8 C9 C10 C11 0.3(8) . . . . ? C9 C10 C11 C12 -1.2(8) . . . . ? C10 C11 C12 C7 0.8(7) . . . . ? C8 C7 C12 C11 0.4(7) . . . . ? P1 C7 C12 C11 -177.1(4) . . . . ? C7 P1 C13 C14 -87.0(3) . . . . ? C1 P1 C13 C14 167.2(3) . . . . ? Pd1 P1 C13 C14 40.5(4) . . . . ? C7 P1 C13 C18 91.5(4) . . . . ? C1 P1 C13 C18 -14.3(4) . . . . ? Pd1 P1 C13 C18 -141.0(3) . . . . ? C18 C13 C14 C15 -0.8(6) . . . . ? P1 C13 C14 C15 177.7(3) . . . . ? C13 C14 C15 C16 0.7(7) . . . . ? C14 C15 C16 C17 0.4(7) . . . . ? C15 C16 C17 C18 -1.4(8) . . . . ? C14 C13 C18 C17 -0.1(7) . . . . ? P1 C13 C18 C17 -178.6(4) . . . . ? C16 C17 C18 C13 1.3(8) . . . . ? C24 C19 C20 C21 -4(2) . . . . ? C19 C20 C21 C22 7(2) . . . . ? C20 C21 C22 C23 -5.1(17) . . . . ? C21 C22 C23 C24 1.3(11) . . . . ? C20 C19 C24 C23 0.5(14) . . . . ? C20 C19 C24 P2 -177.8(9) . . . . ? C22 C23 C24 C19 1.0(10) . . . . ? C22 C23 C24 P2 179.3(5) . . . . ? C25 P2 C24 C19 -92.8(7) . . . . ? C31 P2 C24 C19 13.8(7) . . . . ? Pd2 P2 C24 C19 140.5(6) . . . . ? C25 P2 C24 C23 89.0(5) . . . . ? C31 P2 C24 C23 -164.4(4) . . . . ? Pd2 P2 C24 C23 -37.7(5) . . . . ? C24 P2 C25 C26 -160.8(4) . . . . ? C31 P2 C25 C26 93.1(4) . . . . ? Pd2 P2 C25 C26 -34.0(4) . . . . ? C24 P2 C25 C30 19.9(5) . . . . ? C31 P2 C25 C30 -86.2(5) . . . . ? Pd2 P2 C25 C30 146.7(4) . . . . ? C30 C25 C26 C27 1.4(8) . . . . ? P2 C25 C26 C27 -177.9(4) . . . . ? C25 C26 C27 C28 -1.6(9) . . . . ? C26 C27 C28 C29 1.0(11) . . . . ? C27 C28 C29 C30 -0.2(11) . . . . ? C28 C29 C30 C25 0.1(10) . . . . ? C26 C25 C30 C29 -0.7(8) . . . . ? P2 C25 C30 C29 178.6(5) . . . . ? C24 P2 C31 C36 94.0(4) . . . . ? C25 P2 C31 C36 -158.9(4) . . . . ? Pd2 P2 C31 C36 -32.3(4) . . . . ? C24 P2 C31 C32 -84.8(4) . . . . ? C25 P2 C31 C32 22.3(4) . . . . ? Pd2 P2 C31 C32 148.9(3) . . . . ? C36 C31 C32 C33 -1.1(7) . . . . ? P2 C31 C32 C33 177.7(4) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C32 C33 C34 C35 0.6(9) . . . . ? C33 C34 C35 C36 -0.9(9) . . . . ? C32 C31 C36 C35 0.8(7) . . . . ? P2 C31 C36 C35 -178.1(4) . . . . ? C34 C35 C36 C31 0.2(8) . . . . ? C43 P3 C37 C42 32.9(4) . . . . ? C49 P3 C37 C42 139.7(4) . . . . ? Pd3 P3 C37 C42 -92.0(4) . . . . ? C43 P3 C37 C38 -151.0(4) . . . . ? C49 P3 C37 C38 -44.2(4) . . . . ? Pd3 P3 C37 C38 84.1(4) . . . . ? C42 C37 C38 C39 -0.9(7) . . . . ? P3 C37 C38 C39 -177.1(4) . . . . ? C37 C38 C39 C40 1.1(8) . . . . ? C38 C39 C40 C41 0.0(9) . . . . ? C39 C40 C41 C42 -1.3(8) . . . . ? C38 C37 C42 C41 -0.3(7) . . . . ? P3 C37 C42 C41 175.8(4) . . . . ? C40 C41 C42 C37 1.4(8) . . . . ? C37 P3 C43 C44 -111.6(4) . . . . ? C49 P3 C43 C44 142.7(4) . . . . ? Pd3 P3 C43 C44 19.0(4) . . . . ? C37 P3 C43 C48 66.3(4) . . . . ? C49 P3 C43 C48 -39.4(4) . . . . ? Pd3 P3 C43 C48 -163.1(3) . . . . ? C48 C43 C44 C45 0.5(8) . . . . ? P3 C43 C44 C45 178.4(5) . . . . ? C43 C44 C45 C46 -0.2(10) . . . . ? C44 C45 C46 C47 0.8(10) . . . . ? C45 C46 C47 C48 -1.8(9) . . . . ? C46 C47 C48 C43 2.0(8) . . . . ? C44 C43 C48 C47 -1.4(7) . . . . ? P3 C43 C48 C47 -179.2(4) . . . . ? C43 P3 C49 C50 -108.6(4) . . . . ? C37 P3 C49 C50 147.4(3) . . . . ? Pd3 P3 C49 C50 14.4(4) . . . . ? C43 P3 C49 C54 71.8(4) . . . . ? C37 P3 C49 C54 -32.1(4) . . . . ? Pd3 P3 C49 C54 -165.1(3) . . . . ? C54 C49 C50 C51 -1.2(7) . . . . ? P3 C49 C50 C51 179.3(4) . . . . ? C49 C50 C51 C52 -0.5(8) . . . . ? C50 C51 C52 C53 2.3(9) . . . . ? C51 C52 C53 C54 -2.5(9) . . . . ? C52 C53 C54 C49 0.8(8) . . . . ? C50 C49 C54 C53 1.0(7) . . . . ? P3 C49 C54 C53 -179.5(4) . . . . ? C67 P4 C55 C60 -104.2(5) . . . . ? C61A P4 C55 C60 155.9(8) . . . . ? C61B P4 C55 C60 143.3(8) . . . . ? Pd4 P4 C55 C60 18.1(5) . . . . ? C67 P4 C55 C56 75.2(6) . . . . ? C61A P4 C55 C56 -24.7(9) . . . . ? C61B P4 C55 C56 -37.3(10) . . . . ? Pd4 P4 C55 C56 -162.5(6) . . . . ? C60 C55 C56 C57 2.6(13) . . . . ? P4 C55 C56 C57 -176.8(8) . . . . ? C55 C56 C57 C58 -1.0(16) . . . . ? C56 C57 C58 C59 -1.1(16) . . . . ? C57 C58 C59 C60 1.7(13) . . . . ? C56 C55 C60 C59 -1.9(9) . . . . ? P4 C55 C60 C59 177.5(5) . . . . ? C58 C59 C60 C55 -0.1(10) . . . . ? C67 P4 C61A C62A 22.1(8) . . . . ? C55 P4 C61A C62A 127.8(7) . . . . ? C61B P4 C61A C62A -172(5) . . . . ? Pd4 P4 C61A C62A -99.4(9) . . . . ? C67 P4 C61A C66A -161.7(6) . . . . ? C55 P4 C61A C66A -56.0(7) . . . . ? C61B P4 C61A C66A 5(4) . . . . ? Pd4 P4 C61A C66A 76.7(8) . . . . ? C66A C61A C62A C63A 0.0 . . . . ? P4 C61A C62A C63A 175.9(10) . . . . ? C61A C62A C63A C64A 0.0 . . . . ? C62A C63A C64A C65A 0.0 . . . . ? C63A C64A C65A C66A 0.0 . . . . ? C64A C65A C66A C61A 0.0 . . . . ? C62A C61A C66A C65A 0.0 . . . . ? P4 C61A C66A C65A -176.3(9) . . . . ? C61A P4 C67 C72 -109.7(7) . . . . ? C55 P4 C67 C72 144.4(5) . . . . ? C61B P4 C67 C72 -113.3(9) . . . . ? Pd4 P4 C67 C72 20.5(5) . . . . ? C61A P4 C67 C68 69.2(7) . . . . ? C55 P4 C67 C68 -36.7(6) . . . . ? C61B P4 C67 C68 65.6(9) . . . . ? Pd4 P4 C67 C68 -160.6(5) . . . . ? C67 P4 C61B C62B 22.5(13) . . . . ? C61A P4 C61B C62B 8(4) . . . . ? C55 P4 C61B C62B 129.6(11) . . . . ? Pd4 P4 C61B C62B -108.0(10) . . . . ? C67 P4 C61B C66B -159.4(10) . . . . ? C61A P4 C61B C66B -174(5) . . . . ? C55 P4 C61B C66B -52.3(12) . . . . ? Pd4 P4 C61B C66B 70.1(12) . . . . ? C66B C61B C62B C63B 0.0 . . . . ? P4 C61B C62B C63B 178.2(15) . . . . ? C61B C62B C63B C64B 0.0 . . . . ? C62B C63B C64B C65B 0.0 . . . . ? C63B C64B C65B C66B 0.0 . . . . ? C64B C65B C66B C61B 0.0 . . . . ? C62B C61B C66B C65B 0.0 . . . . ? P4 C61B C66B C65B -178.1(15) . . . . ? C72 C67 C68 C69 0.9(12) . . . . ? P4 C67 C68 C69 -178.0(8) . . . . ? C67 C68 C69 C70 -3.1(19) . . . . ? C68 C69 C70 C71 5(2) . . . . ? C69 C70 C71 C72 -4.6(18) . . . . ? C68 C67 C72 C71 -0.6(10) . . . . ? P4 C67 C72 C71 178.4(6) . . . . ? C70 C71 C72 C67 2.4(13) . . . . ? C85 P5 C73 C78 -110.9(3) . . . . ? C79 P5 C73 C78 144.1(3) . . . . ? Pd5 P5 C73 C78 11.9(4) . . . . ? C85 P5 C73 C74 69.8(4) . . . . ? C79 P5 C73 C74 -35.2(4) . . . . ? Pd5 P5 C73 C74 -167.5(3) . . . . ? C78 C73 C74 C75 2.0(6) . . . . ? P5 C73 C74 C75 -178.7(3) . . . . ? C73 C74 C75 C76 -0.9(7) . . . . ? C74 C75 C76 C77 -0.5(7) . . . . ? C75 C76 C77 C78 1.0(7) . . . . ? C76 C77 C78 C73 0.1(7) . . . . ? C74 C73 C78 C77 -1.6(6) . . . . ? P5 C73 C78 C77 179.1(3) . . . . ? C85 P5 C79 C80 -150.7(4) . . . . ? C73 P5 C79 C80 -42.7(4) . . . . ? Pd5 P5 C79 C80 84.9(4) . . . . ? C85 P5 C79 C84 33.9(4) . . . . ? C73 P5 C79 C84 141.9(4) . . . . ? Pd5 P5 C79 C84 -90.5(4) . . . . ? C84 C79 C80 C81 -0.5(7) . . . . ? P5 C79 C80 C81 -176.0(4) . . . . ? C79 C80 C81 C82 0.7(8) . . . . ? C80 C81 C82 C83 0.0(8) . . . . ? C81 C82 C83 C84 -0.8(8) . . . . ? C80 C79 C84 C83 -0.4(7) . . . . ? P5 C79 C84 C83 175.1(4) . . . . ? C82 C83 C84 C79 1.0(8) . . . . ? C73 P5 C85 C90 139.7(3) . . . . ? C79 P5 C85 C90 -114.3(3) . . . . ? Pd5 P5 C85 C90 16.1(3) . . . . ? C73 P5 C85 C86 -43.4(4) . . . . ? C79 P5 C85 C86 62.7(4) . . . . ? Pd5 P5 C85 C86 -167.0(3) . . . . ? C90 C85 C86 C87 -1.1(6) . . . . ? P5 C85 C86 C87 -178.0(3) . . . . ? C85 C86 C87 C88 0.9(6) . . . . ? C86 C87 C88 C89 0.1(7) . . . . ? C87 C88 C89 C90 -1.1(7) . . . . ? C88 C89 C90 C85 0.9(7) . . . . ? C86 C85 C90 C89 0.1(6) . . . . ? P5 C85 C90 C89 177.2(3) . . . . ? Pd3 P6 C91 Si1 -0.1(9) . . . . ? Pd4 P6 C91 Si1 -178.4(6) . . . . ? Pd1 P6 C91 Si1 -139.3(4) . . . . ? Pd2 P6 C91 Si1 142.9(4) . . . . ? Pd3 P6 C91 Pd4 178.3(4) . . . . ? Pd1 P6 C91 Pd4 39.14(19) . . . . ? Pd2 P6 C91 Pd4 -38.62(19) . . . . ? C94 Si1 C91 P6 -7.5(6) . . . . ? C93 Si1 C91 P6 111.7(5) . . . . ? C92 Si1 C91 P6 -126.1(5) . . . . ? C94 Si1 C91 Pd4 174.7(4) . . . . ? C93 Si1 C91 Pd4 -66.1(4) . . . . ? C92 Si1 C91 Pd4 56.1(4) . . . . ? P4 Pd4 C91 P6 175.28(10) . . . . ? P7 Pd4 C91 P6 -2.1(3) . . . . ? Pd1 Pd4 C91 P6 -27.08(15) . . . . ? Pd2 Pd4 C91 P6 26.55(15) . . . . ? P4 Pd4 C91 Si1 -6.0(4) . . . . ? P7 Pd4 C91 Si1 176.6(2) . . . . ? P6 Pd4 C91 Si1 178.7(5) . . . . ? Pd1 Pd4 C91 Si1 151.6(3) . . . . ? Pd2 Pd4 C91 Si1 -154.7(3) . . . . ? Pd5 P8 C95 Si2 10.2(9) . . . . ? Pd1 P8 C95 Si2 -134.3(4) . . . . ? Pd3 P8 C95 Si2 -173.1(5) . . . . ? Pd2 P8 C95 Si2 148.0(4) . . . . ? Pd5 P8 C95 Pd3 -176.7(4) . . . . ? Pd1 P8 C95 Pd3 38.75(18) . . . . ? Pd2 P8 C95 Pd3 -38.87(18) . . . . ? C97 Si2 C95 P8 104.9(5) . . . . ? C96 Si2 C95 P8 -135.1(5) . . . . ? C98 Si2 C95 P8 -15.9(5) . . . . ? C97 Si2 C95 Pd3 -65.3(4) . . . . ? C96 Si2 C95 Pd3 54.7(4) . . . . ? C98 Si2 C95 Pd3 173.9(3) . . . . ? P6 Pd3 C95 P8 -0.6(3) . . . . ? P3 Pd3 C95 P8 177.41(9) . . . . ? Pd1 Pd3 C95 P8 -26.36(14) . . . . ? Pd2 Pd3 C95 P8 27.00(14) . . . . ? P6 Pd3 C95 Si2 173.5(2) . . . . ? P3 Pd3 C95 Si2 -8.5(4) . . . . ? P8 Pd3 C95 Si2 174.1(5) . . . . ? Pd1 Pd3 C95 Si2 147.8(3) . . . . ? Pd2 Pd3 C95 Si2 -158.9(3) . . . . ? Pd4 P7 C99 Si3 7.8(9) . . . . ? Pd1 P7 C99 Si3 -135.7(4) . . . . ? Pd5 P7 C99 Si3 -175.2(6) . . . . ? Pd2 P7 C99 Si3 146.5(4) . . . . ? Pd4 P7 C99 Pd5 -177.1(4) . . . . ? Pd1 P7 C99 Pd5 39.4(2) . . . . ? Pd2 P7 C99 Pd5 -38.28(18) . . . . ? C102 Si3 C99 P7 -0.6(6) . . . . ? C100 Si3 C99 P7 -121.5(5) . . . . ? C101 Si3 C99 P7 118.6(5) . . . . ? C102 Si3 C99 Pd5 -173.8(4) . . . . ? C100 Si3 C99 Pd5 65.3(4) . . . . ? C101 Si3 C99 Pd5 -54.6(4) . . . . ? P8 Pd5 C99 P7 -3.4(3) . . . . ? P5 Pd5 C99 P7 174.16(10) . . . . ? Pd1 Pd5 C99 P7 -26.75(15) . . . . ? Pd2 Pd5 C99 P7 26.67(15) . . . . ? P8 Pd5 C99 Si3 172.7(2) . . . . ? P5 Pd5 C99 Si3 -9.8(4) . . . . ? P7 Pd5 C99 Si3 176.0(5) . . . . ? Pd1 Pd5 C99 Si3 149.3(3) . . . . ? Pd2 Pd5 C99 Si3 -157.3(3) . . . . ? C108 C103 C104 C105 0.0 . . . . ? C109 C103 C104 C105 179.1(4) . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C107 0.0 . . . . ? C105 C106 C107 C108 0.0 . . . . ? C106 C107 C108 C103 0.0 . . . . ? C104 C103 C108 C107 0.0 . . . . ? C109 C103 C108 C107 -179.1(4) . . . . ? C115 C110 C111 C112 0.0 . . . . ? C116 C110 C111 C112 178.3(13) . . . . ? C110 C111 C112 C113 0.0 . . . . ? C111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C110 0.0 . . . . ? C111 C110 C115 C114 0.0 . . . . ? C116 C110 C115 C114 -178.4(12) . . . . ? C123 C117 C118 C119 -173(2) . . . . ? C122 C117 C118 C119 0.0 . . . . ? C117 C118 C119 C120 0.0 . . . . ? C118 C119 C120 C121 0.0 . . . . ? C119 C120 C121 C122 0.0 . . . . ? C120 C121 C122 C117 0.0 . . . . ? C123 C117 C122 C121 173.7(18) . . . . ? C118 C117 C122 C121 0.0 . . . . ? C129 C124 C125 C126 0.0 . . . . ? C130 C124 C125 C126 -169.2(12) . . . . ? C124 C125 C126 C127 0.0 . . . . ? C125 C126 C127 C128 0.0 . . . . ? C126 C127 C128 C129 0.0 . . . . ? C127 C128 C129 C124 0.0 . . . . ? C125 C124 C129 C128 0.0 . . . . ? C130 C124 C129 C128 167.0(15) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.228 _refine_diff_density_min -1.862 _refine_diff_density_rms 0.227