# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Bedford, Robin' 'Yu-Ning Chang.' 'Haddow, Mairi' 'McMullin, Claire' _publ_contact_author_name 'Bedford, Robin' _publ_contact_author_email r.bedford@bristol.ac.uk _publ_section_title ; Chiral palladacycles based on resorcinol monophosphite ligands: the role of the meta-hydroxyl in ligand C-H activation and catalysis. ; # Attachment '- 3b.cif' data_yc3_66_0m _database_code_depnum_ccdc_archive 'CCDC 815807' #TrackingRef '- 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H37 O3 P' _chemical_formula_sum 'C36 H37 O3 P' _chemical_formula_weight 548.63 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.9688(11) _cell_length_b 9.1502(10) _cell_length_c 16.0481(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.461(4) _cell_angle_gamma 90.00 _cell_volume 1443.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15303 _cell_measurement_theta_min 4.50 _cell_measurement_theta_max 60.85 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.082 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4800 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Microstar CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15287 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 60.85 _reflns_number_total 4340 _reflns_number_gt 4228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker PROTEUM' _computing_cell_refinement 'Bruker PROTEUM' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.3000P] 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 0.056(16) _refine_ls_number_reflns 4340 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 P1 P 0.64253(4) 0.62549(5) 0.75744(3) 0.02047(13) Uani 1 1 d . . . O1 O 0.62388(12) 0.80249(14) 0.76060(8) 0.0216(3) Uani 1 1 d . . . O2 O 0.51289(12) 0.58670(14) 0.80469(8) 0.0205(3) Uani 1 1 d . . . O3 O 0.57499(12) 0.58868(14) 0.66069(8) 0.0214(3) Uani 1 1 d . . . C1 C 0.68857(18) 0.8756(2) 0.83344(11) 0.0197(4) Uani 1 1 d . . . C2 C 0.77805(18) 0.9920(2) 0.82656(11) 0.0188(4) Uani 1 1 d . . . C3 C 0.83564(18) 1.0593(2) 0.90211(12) 0.0198(4) Uani 1 1 d . . . H3 H 0.8954 1.1393 0.8990 0.024 Uiso 1 1 calc R . . C4 C 0.81120(18) 1.0168(2) 0.98202(11) 0.0196(4) Uani 1 1 d . . . C5 C 0.71997(18) 0.9024(2) 0.98460(12) 0.0213(4) Uani 1 1 d . . . H5 H 0.6995 0.8711 1.0375 0.026 Uiso 1 1 calc R . . C6 C 0.65880(18) 0.8338(2) 0.91161(12) 0.0213(4) Uani 1 1 d . . . H6 H 0.5956 0.7572 0.9148 0.026 Uiso 1 1 calc R . . C7 C 0.80908(19) 1.0429(2) 0.74014(12) 0.0226(4) Uani 1 1 d . . . C8 C 0.8686(2) 0.9174(2) 0.69376(13) 0.0282(5) Uani 1 1 d . . . H8A H 0.7998 0.8410 0.6795 0.042 Uiso 1 1 calc R . . H8B H 0.9481 0.8764 0.7304 0.042 Uiso 1 1 calc R . . H8C H 0.8960 0.9548 0.6419 0.042 Uiso 1 1 calc R . . C9 C 0.6783(2) 1.1018(2) 0.68701(12) 0.0284(5) Uani 1 1 d . . . H9A H 0.6478 1.1886 0.7144 0.043 Uiso 1 1 calc R . . H9B H 0.6075 1.0265 0.6821 0.043 Uiso 1 1 calc R . . H9C H 0.6961 1.1279 0.6306 0.043 Uiso 1 1 calc R . . C10 C 0.9140(2) 1.1666(2) 0.74953(13) 0.0310(5) Uani 1 1 d . . . H10A H 0.9352 1.1922 0.6938 0.046 Uiso 1 1 calc R . . H10B H 0.9971 1.1344 0.7863 0.046 Uiso 1 1 calc R . . H10C H 0.8768 1.2523 0.7744 0.046 Uiso 1 1 calc R . . C11 C 0.88211(19) 1.0864(2) 1.06486(12) 0.0224(4) Uani 1 1 d . . . C12 C 0.9769(2) 0.9740(3) 1.11426(13) 0.0351(5) Uani 1 1 d . . . H12A H 1.0486 0.9477 1.0819 0.053 Uiso 1 1 calc R . . H12B H 0.9248 0.8864 1.1238 0.053 Uiso 1 1 calc R . . H12C H 1.0180 1.0156 1.1688 0.053 Uiso 1 1 calc R . . C13 C 0.7780(2) 1.1305(3) 1.12091(12) 0.0318(5) Uani 1 1 d . . . H13A H 0.7305 1.0432 1.1362 0.048 Uiso 1 1 calc R . . H13B H 0.7119 1.1986 1.0900 0.048 Uiso 1 1 calc R . . H13C H 0.8250 1.1779 1.1723 0.048 Uiso 1 1 calc R . . C14 C 0.9634(3) 1.2221(3) 1.05062(14) 0.0436(6) Uani 1 1 d . . . H14A H 1.0022 1.2649 1.1053 0.065 Uiso 1 1 calc R . . H14B H 0.9035 1.2936 1.0176 0.065 Uiso 1 1 calc R . . H14C H 1.0369 1.1954 1.0198 0.065 Uiso 1 1 calc R . . C15 C 0.47231(17) 0.4406(2) 0.79627(11) 0.0182(4) Uani 1 1 d . . . C16 C 0.51822(18) 0.3464(2) 0.86498(12) 0.0210(4) Uani 1 1 d . . . C17 C 0.47391(18) 0.2047(2) 0.85824(12) 0.0218(4) Uani 1 1 d . . . H17 H 0.5024 0.1390 0.9035 0.026 Uiso 1 1 calc R . . C18 C 0.38686(17) 0.1534(2) 0.78567(11) 0.0203(4) Uani 1 1 d . . . C19 C 0.34493(19) 0.0053(2) 0.77944(12) 0.0231(4) Uani 1 1 d . . . H19 H 0.3724 -0.0586 0.8257 0.028 Uiso 1 1 calc R . . C20 C 0.26613(19) -0.0470(2) 0.70855(12) 0.0256(4) Uani 1 1 d . . . H20 H 0.2380 -0.1463 0.7058 0.031 Uiso 1 1 calc R . . C21 C 0.22631(19) 0.0463(2) 0.63936(12) 0.0240(4) Uani 1 1 d . . . H21 H 0.1723 0.0090 0.5896 0.029 Uiso 1 1 calc R . . C22 C 0.26451(18) 0.1906(2) 0.64282(12) 0.0199(4) Uani 1 1 d . . . H22 H 0.2372 0.2517 0.5952 0.024 Uiso 1 1 calc R . . C23 C 0.34425(17) 0.2498(2) 0.71649(12) 0.0187(4) Uani 1 1 d . . . C24 C 0.38648(17) 0.4000(2) 0.72393(11) 0.0177(4) Uani 1 1 d . . . C25 C 0.34203(17) 0.51405(19) 0.65847(11) 0.0181(4) Uani 1 1 d . . . C26 C 0.20105(18) 0.5429(2) 0.62840(11) 0.0182(4) Uani 1 1 d . . . C27 C 0.09438(18) 0.4761(2) 0.66412(11) 0.0193(4) Uani 1 1 d . . . H27 H 0.1158 0.4049 0.7074 0.023 Uiso 1 1 calc R . . C28 C -0.03852(18) 0.5133(2) 0.63684(11) 0.0221(4) Uani 1 1 d . . . H28 H -0.1079 0.4686 0.6621 0.027 Uiso 1 1 calc R . . C29 C -0.07408(18) 0.6165(2) 0.57226(11) 0.0245(4) Uani 1 1 d . . . H29 H -0.1669 0.6404 0.5537 0.029 Uiso 1 1 calc R . . C30 C 0.02505(19) 0.6822(2) 0.53634(12) 0.0244(4) Uani 1 1 d . . . H30 H 0.0005 0.7511 0.4922 0.029 Uiso 1 1 calc R . . C31 C 0.16423(18) 0.6494(2) 0.56386(11) 0.0196(4) Uani 1 1 d . . . C32 C 0.26726(19) 0.7246(2) 0.53063(11) 0.0214(4) Uani 1 1 d . . . H32 H 0.2423 0.7905 0.4850 0.026 Uiso 1 1 calc R . . C33 C 0.40173(18) 0.7052(2) 0.56221(11) 0.0209(4) Uani 1 1 d . . . C34 C 0.43574(17) 0.6025(2) 0.62821(11) 0.0187(4) Uani 1 1 d . . . C35 C 0.6099(2) 0.4043(2) 0.94116(13) 0.0293(5) Uani 1 1 d . . . H35A H 0.6360 0.3245 0.9813 0.044 Uiso 1 1 calc R . . H35B H 0.5620 0.4799 0.9680 0.044 Uiso 1 1 calc R . . H35C H 0.6916 0.4463 0.9240 0.044 Uiso 1 1 calc R . . C36 C 0.5113(2) 0.7872(2) 0.52759(13) 0.0301(5) Uani 1 1 d . . . H36A H 0.4695 0.8555 0.4839 0.045 Uiso 1 1 calc R . . H36B H 0.5688 0.7179 0.5031 0.045 Uiso 1 1 calc R . . H36C H 0.5670 0.8417 0.5733 0.045 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 P1 0.0175(2) 0.0217(3) 0.0216(2) -0.0008(2) 0.00149(17) -0.00137(18) O1 0.0231(6) 0.0226(7) 0.0182(7) -0.0009(5) 0.0007(5) -0.0037(5) O2 0.0229(6) 0.0179(7) 0.0203(6) -0.0013(5) 0.0021(5) -0.0039(5) O3 0.0180(6) 0.0233(7) 0.0229(6) -0.0013(5) 0.0039(5) -0.0018(5) C1 0.0185(9) 0.0202(10) 0.0192(10) -0.0009(8) -0.0005(7) -0.0006(7) C2 0.0181(9) 0.0184(10) 0.0197(9) 0.0024(7) 0.0023(7) 0.0004(7) C3 0.0192(9) 0.0176(9) 0.0226(10) 0.0021(8) 0.0028(7) -0.0022(7) C4 0.0186(9) 0.0199(9) 0.0199(9) 0.0015(8) 0.0018(7) 0.0028(7) C5 0.0216(9) 0.0228(10) 0.0201(10) 0.0025(8) 0.0053(7) -0.0018(8) C6 0.0194(9) 0.0204(10) 0.0247(10) 0.0022(8) 0.0055(7) -0.0033(7) C7 0.0280(10) 0.0218(10) 0.0190(9) -0.0008(8) 0.0064(8) -0.0046(8) C8 0.0300(10) 0.0287(11) 0.0285(11) -0.0045(9) 0.0124(8) -0.0053(9) C9 0.0354(10) 0.0314(12) 0.0183(9) 0.0045(9) 0.0039(8) -0.0001(9) C10 0.0412(12) 0.0315(13) 0.0217(10) -0.0020(8) 0.0098(9) -0.0128(9) C11 0.0246(9) 0.0222(11) 0.0191(9) -0.0003(8) 0.0000(7) -0.0026(8) C12 0.0346(11) 0.0424(14) 0.0255(10) -0.0063(10) -0.0039(9) 0.0095(10) C13 0.0339(10) 0.0347(12) 0.0259(10) -0.0018(10) 0.0019(8) 0.0072(10) C14 0.0541(14) 0.0493(15) 0.0255(11) -0.0031(11) 0.0011(10) -0.0287(12) C15 0.0170(8) 0.0172(9) 0.0211(10) -0.0023(8) 0.0048(7) -0.0026(7) C16 0.0187(9) 0.0240(11) 0.0197(9) 0.0013(8) 0.0017(7) 0.0027(7) C17 0.0219(9) 0.0242(10) 0.0189(9) 0.0051(8) 0.0018(7) 0.0037(8) C18 0.0188(8) 0.0198(10) 0.0224(9) 0.0007(8) 0.0039(7) 0.0023(7) C19 0.0268(10) 0.0188(10) 0.0237(10) 0.0042(8) 0.0044(8) 0.0018(8) C20 0.0305(10) 0.0168(9) 0.0301(11) -0.0005(8) 0.0071(9) -0.0016(8) C21 0.0255(10) 0.0221(11) 0.0237(10) -0.0042(8) 0.0026(8) -0.0014(8) C22 0.0205(9) 0.0204(10) 0.0186(9) 0.0006(8) 0.0029(7) 0.0028(7) C23 0.0172(9) 0.0186(10) 0.0211(10) 0.0006(8) 0.0056(7) 0.0023(7) C24 0.0179(8) 0.0181(10) 0.0174(9) 0.0014(7) 0.0036(7) 0.0021(7) C25 0.0213(9) 0.0163(9) 0.0168(9) -0.0032(7) 0.0031(7) -0.0008(7) C26 0.0228(9) 0.0156(9) 0.0156(9) -0.0051(7) 0.0015(7) 0.0006(7) C27 0.0217(9) 0.0183(10) 0.0178(9) -0.0017(8) 0.0032(7) -0.0003(7) C28 0.0217(9) 0.0234(10) 0.0218(10) -0.0051(8) 0.0048(8) 0.0001(8) C29 0.0203(9) 0.0275(10) 0.0240(9) -0.0056(9) -0.0017(7) 0.0050(8) C30 0.0278(10) 0.0227(10) 0.0202(10) -0.0015(8) -0.0031(8) 0.0043(8) C31 0.0238(9) 0.0190(10) 0.0153(8) -0.0040(7) 0.0010(7) 0.0019(8) C32 0.0319(10) 0.0173(9) 0.0145(9) -0.0018(7) 0.0018(8) 0.0005(8) C33 0.0275(10) 0.0204(10) 0.0151(9) -0.0023(8) 0.0043(7) -0.0032(8) C34 0.0189(8) 0.0196(10) 0.0168(8) -0.0034(7) 0.0012(7) -0.0004(7) C35 0.0320(11) 0.0298(12) 0.0228(10) 0.0062(9) -0.0049(8) -0.0033(9) C36 0.0327(11) 0.0326(12) 0.0254(11) 0.0029(9) 0.0060(9) -0.0076(9) _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 O3 1.6229(13) . ? P1 O1 1.6320(14) . ? P1 O2 1.6411(13) . ? O1 C1 1.408(2) . ? O2 C15 1.397(2) . ? O3 C34 1.406(2) . ? C1 C6 1.389(3) . ? C1 C2 1.405(3) . ? C2 C3 1.397(3) . ? C2 C7 1.542(3) . ? C3 C4 1.399(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 C11 1.538(3) . ? C5 C6 1.379(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C10 1.532(3) . ? C7 C9 1.533(3) . ? C7 C8 1.540(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.520(3) . ? C11 C12 1.528(3) . ? C11 C13 1.535(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.375(3) . ? C15 C16 1.415(3) . ? C16 C17 1.368(3) . ? C16 C35 1.498(3) . ? C17 C18 1.413(3) . ? C17 H17 0.9500 . ? C18 C19 1.417(3) . ? C18 C23 1.427(3) . ? C19 C20 1.359(3) . ? C19 H19 0.9500 . ? C20 C21 1.405(3) . ? C20 H20 0.9500 . ? C21 C22 1.373(3) . ? C21 H21 0.9500 . ? C22 C23 1.419(3) . ? C22 H22 0.9500 . ? C23 C24 1.436(3) . ? C24 C25 1.495(3) . ? C25 C34 1.383(3) . ? C25 C26 1.433(3) . ? C26 C31 1.426(3) . ? C26 C27 1.426(3) . ? C27 C28 1.368(3) . ? C27 H27 0.9500 . ? C28 C29 1.403(3) . ? C28 H28 0.9500 . ? C29 C30 1.363(3) . ? C29 H29 0.9500 . ? C30 C31 1.417(3) . ? C30 H30 0.9500 . ? C31 C32 1.412(3) . ? C32 C33 1.365(3) . ? C32 H32 0.9500 . ? C33 C34 1.415(3) . ? C33 C36 1.505(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 O3 P1 O1 101.78(6) . . ? O3 P1 O2 99.37(6) . . ? O1 P1 O2 95.62(7) . . ? C1 O1 P1 117.29(11) . . ? C15 O2 P1 113.57(11) . . ? C34 O3 P1 124.41(11) . . ? C6 C1 C2 120.80(16) . . ? C6 C1 O1 118.84(16) . . ? C2 C1 O1 120.32(16) . . ? C3 C2 C1 116.22(16) . . ? C3 C2 C7 122.20(16) . . ? C1 C2 C7 121.58(16) . . ? C2 C3 C4 124.36(17) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C5 C4 C3 116.70(17) . . ? C5 C4 C11 119.73(16) . . ? C3 C4 C11 123.54(16) . . ? C6 C5 C4 121.12(17) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.76(17) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C10 C7 C9 107.41(17) . . ? C10 C7 C8 106.70(15) . . ? C9 C7 C8 110.70(16) . . ? C10 C7 C2 111.69(15) . . ? C9 C7 C2 109.18(15) . . ? C8 C7 C2 111.08(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 109.19(18) . . ? C14 C11 C13 107.59(18) . . ? C12 C11 C13 107.03(16) . . ? C14 C11 C4 112.91(16) . . ? C12 C11 C4 109.07(15) . . ? C13 C11 C4 110.88(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 O2 118.06(16) . . ? C24 C15 C16 124.73(17) . . ? O2 C15 C16 117.15(16) . . ? C17 C16 C15 117.19(17) . . ? C17 C16 C35 123.05(17) . . ? C15 C16 C35 119.76(17) . . ? C16 C17 C18 121.75(17) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 120.64(16) . . ? C17 C18 C23 120.00(17) . . ? C19 C18 C23 119.32(16) . . ? C20 C19 C18 121.28(17) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.81(19) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 120.79(18) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.95(18) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 117.82(17) . . ? C22 C23 C24 123.41(17) . . ? C18 C23 C24 118.75(16) . . ? C15 C24 C23 117.51(16) . . ? C15 C24 C25 118.41(16) . . ? C23 C24 C25 124.08(15) . . ? C34 C25 C26 117.10(16) . . ? C34 C25 C24 121.05(15) . . ? C26 C25 C24 121.74(16) . . ? C31 C26 C27 117.72(16) . . ? C31 C26 C25 119.45(17) . . ? C27 C26 C25 122.71(16) . . ? C28 C27 C26 120.76(17) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 121.17(18) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.76(16) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 121.02(18) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.99(17) . . ? C32 C31 C26 119.42(16) . . ? C30 C31 C26 119.55(17) . . ? C33 C32 C31 121.85(17) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C32 C33 C34 117.66(17) . . ? C32 C33 C36 121.77(17) . . ? C34 C33 C36 120.56(16) . . ? C25 C34 O3 120.00(16) . . ? C25 C34 C33 123.98(15) . . ? O3 C34 C33 115.95(15) . . ? C16 C35 H35A 109.5 . . ? C16 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C16 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 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 O3 P1 O1 C1 -171.63(12) . . . . ? O2 P1 O1 C1 87.55(12) . . . . ? O3 P1 O2 C15 62.03(12) . . . . ? O1 P1 O2 C15 164.98(12) . . . . ? O1 P1 O3 C34 -67.92(14) . . . . ? O2 P1 O3 C34 29.88(15) . . . . ? P1 O1 C1 C6 -57.0(2) . . . . ? P1 O1 C1 C2 125.10(16) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? O1 C1 C2 C3 178.98(15) . . . . ? C6 C1 C2 C7 -178.16(17) . . . . ? O1 C1 C2 C7 -0.3(3) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C7 C2 C3 C4 -179.71(17) . . . . ? C2 C3 C4 C5 -2.0(3) . . . . ? C2 C3 C4 C11 176.24(17) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? C11 C4 C5 C6 -177.41(17) . . . . ? C4 C5 C6 C1 1.1(3) . . . . ? C2 C1 C6 C5 -2.2(3) . . . . ? O1 C1 C6 C5 179.93(16) . . . . ? C3 C2 C7 C10 3.2(3) . . . . ? C1 C2 C7 C10 -177.51(18) . . . . ? C3 C2 C7 C9 -115.43(19) . . . . ? C1 C2 C7 C9 63.8(2) . . . . ? C3 C2 C7 C8 122.22(18) . . . . ? C1 C2 C7 C8 -58.5(2) . . . . ? C5 C4 C11 C14 -172.34(19) . . . . ? C3 C4 C11 C14 9.5(3) . . . . ? C5 C4 C11 C12 66.1(2) . . . . ? C3 C4 C11 C12 -112.1(2) . . . . ? C5 C4 C11 C13 -51.5(2) . . . . ? C3 C4 C11 C13 130.29(19) . . . . ? P1 O2 C15 C24 -83.48(17) . . . . ? P1 O2 C15 C16 99.24(16) . . . . ? C24 C15 C16 C17 0.3(3) . . . . ? O2 C15 C16 C17 177.35(16) . . . . ? C24 C15 C16 C35 -178.94(18) . . . . ? O2 C15 C16 C35 -1.9(2) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C35 C16 C17 C18 179.68(17) . . . . ? C16 C17 C18 C19 178.54(17) . . . . ? C16 C17 C18 C23 0.8(3) . . . . ? C17 C18 C19 C20 -177.08(17) . . . . ? C23 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 C21 0.8(3) . . . . ? C19 C20 C21 C22 -0.9(3) . . . . ? C20 C21 C22 C23 -0.5(3) . . . . ? C21 C22 C23 C18 1.9(2) . . . . ? C21 C22 C23 C24 -179.60(18) . . . . ? C17 C18 C23 C22 175.77(16) . . . . ? C19 C18 C23 C22 -2.0(2) . . . . ? C17 C18 C23 C24 -2.8(2) . . . . ? C19 C18 C23 C24 179.45(17) . . . . ? O2 C15 C24 C23 -179.29(15) . . . . ? C16 C15 C24 C23 -2.2(3) . . . . ? O2 C15 C24 C25 0.2(2) . . . . ? C16 C15 C24 C25 177.27(16) . . . . ? C22 C23 C24 C15 -175.05(16) . . . . ? C18 C23 C24 C15 3.4(2) . . . . ? C22 C23 C24 C25 5.5(3) . . . . ? C18 C23 C24 C25 -176.07(15) . . . . ? C15 C24 C25 C34 51.5(2) . . . . ? C23 C24 C25 C34 -129.08(19) . . . . ? C15 C24 C25 C26 -124.50(18) . . . . ? C23 C24 C25 C26 55.0(3) . . . . ? C34 C25 C26 C31 6.0(2) . . . . ? C24 C25 C26 C31 -177.90(16) . . . . ? C34 C25 C26 C27 -169.81(16) . . . . ? C24 C25 C26 C27 6.3(3) . . . . ? C31 C26 C27 C28 0.2(3) . . . . ? C25 C26 C27 C28 176.06(17) . . . . ? C26 C27 C28 C29 0.9(3) . . . . ? C27 C28 C29 C30 -0.7(3) . . . . ? C28 C29 C30 C31 -0.8(3) . . . . ? C29 C30 C31 C32 -175.72(18) . . . . ? C29 C30 C31 C26 1.9(3) . . . . ? C27 C26 C31 C32 176.08(16) . . . . ? C25 C26 C31 C32 0.1(2) . . . . ? C27 C26 C31 C30 -1.5(2) . . . . ? C25 C26 C31 C30 -177.56(16) . . . . ? C30 C31 C32 C33 173.30(18) . . . . ? C26 C31 C32 C33 -4.3(3) . . . . ? C31 C32 C33 C34 2.1(3) . . . . ? C31 C32 C33 C36 -179.02(18) . . . . ? C26 C25 C34 O3 174.37(14) . . . . ? C24 C25 C34 O3 -1.8(3) . . . . ? C26 C25 C34 C33 -8.5(3) . . . . ? C24 C25 C34 C33 175.32(16) . . . . ? P1 O3 C34 C25 -65.3(2) . . . . ? P1 O3 C34 C33 117.43(15) . . . . ? C32 C33 C34 C25 4.6(3) . . . . ? C36 C33 C34 C25 -174.30(18) . . . . ? C32 C33 C34 O3 -178.24(16) . . . . ? C36 C33 C34 O3 2.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 60.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.281 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.043 # Attachment '- 4c.cif' data_yc4_24_0m _database_code_depnum_ccdc_archive 'CCDC 815808' #TrackingRef '- 4c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C100 H104 Cl2 O6 P2 Pd2 Si4' _chemical_formula_sum 'C100 H104 Cl2 O6 P2 Pd2 Si4' _chemical_formula_weight 1859.83 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 29.464(3) _cell_length_b 9.6174(9) _cell_length_c 22.049(2) _cell_angle_alpha 90.00 _cell_angle_beta 132.779(3) _cell_angle_gamma 90.00 _cell_volume 4585.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27689 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 65.12 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 4.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4653 _exptl_absorpt_correction_T_max 0.7526 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Microstar CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27683 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 65.11 _reflns_number_total 7624 _reflns_number_gt 7197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker PROTEUM' _computing_cell_refinement 'Bruker PROTEUM' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^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 0.007(5) _refine_ls_number_reflns 7624 _refine_ls_number_parameters 534 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _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 Pd1 Pd 0.968510(8) 0.18811(3) 0.898318(12) 0.01816(7) Uani 1 1 d . . . P1 P 0.99572(3) 0.14542(8) 0.83068(5) 0.01878(19) Uani 1 1 d . . . Si1 Si 1.08476(4) -0.23050(10) 0.97997(6) 0.0249(2) Uani 1 1 d . . . Si2 Si 0.96673(4) 0.47130(12) 0.66434(7) 0.0393(3) Uani 1 1 d . . . Cl1 Cl 0.93036(3) 0.21942(9) 0.96575(4) 0.0263(2) Uani 1 1 d . . . O1 O 0.93682(9) 0.0985(2) 0.73907(13) 0.0222(5) Uani 1 1 d . . . O2 O 1.03925(9) 0.0182(2) 0.85238(13) 0.0192(5) Uani 1 1 d . . . O3 O 1.02627(9) 0.2770(2) 0.82627(13) 0.0204(5) Uani 1 1 d . . . C1 C 0.88520(13) 0.1635(3) 0.78375(19) 0.0202(7) Uani 1 1 d . . . C2 C 0.88021(13) 0.1142(3) 0.72080(19) 0.0199(7) Uani 1 1 d . . . C3 C 0.82446(14) 0.0802(3) 0.6420(2) 0.0204(7) Uani 1 1 d . . . C4 C 0.77151(14) 0.1096(4) 0.62834(19) 0.0229(7) Uani 1 1 d . . . H4 H 0.7322 0.0903 0.5753 0.027 Uiso 1 1 calc R . . C5 C 0.77326(12) 0.1658(3) 0.68829(18) 0.0202(7) Uani 1 1 d . . . C6 C 0.83065(12) 0.1892(5) 0.76659(17) 0.0219(6) Uani 1 1 d . . . H6 H 0.8330 0.2231 0.8091 0.026 Uiso 1 1 calc R . . C7 C 0.82035(14) 0.0051(4) 0.5767(2) 0.0261(8) Uani 1 1 d . . . C8 C 0.75318(18) -0.0234(5) 0.4971(2) 0.0393(11) Uani 1 1 d . . . H8A H 0.7327 -0.0780 0.5102 0.059 Uiso 1 1 calc R . . H8B H 0.7526 -0.0754 0.4584 0.059 Uiso 1 1 calc R . . H8C H 0.7314 0.0651 0.4719 0.059 Uiso 1 1 calc R . . C9 C 0.85347(18) -0.1349(4) 0.6119(2) 0.0355(9) Uani 1 1 d . . . H9A H 0.8968 -0.1195 0.6622 0.053 Uiso 1 1 calc R . . H9B H 0.8514 -0.1834 0.5709 0.053 Uiso 1 1 calc R . . H9C H 0.8334 -0.1915 0.6250 0.053 Uiso 1 1 calc R . . C10 C 0.84976(18) 0.0930(5) 0.5534(2) 0.0375(9) Uani 1 1 d . . . H10A H 0.8286 0.1829 0.5318 0.056 Uiso 1 1 calc R . . H10B H 0.8460 0.0445 0.5111 0.056 Uiso 1 1 calc R . . H10C H 0.8936 0.1079 0.6025 0.056 Uiso 1 1 calc R . . C11 C 0.71320(12) 0.1925(5) 0.66938(17) 0.0260(6) Uani 1 1 d . . . C12 C 0.72418(17) 0.2816(5) 0.7359(3) 0.0417(10) Uani 1 1 d . . . H12A H 0.7532 0.2340 0.7893 0.063 Uiso 1 1 calc R . . H12B H 0.6848 0.2964 0.7213 0.063 Uiso 1 1 calc R . . H12C H 0.7415 0.3716 0.7395 0.063 Uiso 1 1 calc R . . C13 C 0.68719(18) 0.0519(5) 0.6668(3) 0.0383(9) Uani 1 1 d . . . H13A H 0.6770 -0.0050 0.6220 0.057 Uiso 1 1 calc R . . H13B H 0.6498 0.0673 0.6571 0.057 Uiso 1 1 calc R . . H13C H 0.7182 0.0037 0.7196 0.057 Uiso 1 1 calc R . . C14 C 0.66595(18) 0.2671(5) 0.5865(3) 0.0488(12) Uani 1 1 d . . . H14A H 0.6831 0.3562 0.5886 0.073 Uiso 1 1 calc R . . H14B H 0.6281 0.2836 0.5754 0.073 Uiso 1 1 calc R . . H14C H 0.6564 0.2093 0.5425 0.073 Uiso 1 1 calc R . . C15 C 1.10340(13) 0.0255(3) 0.92394(19) 0.0182(7) Uani 1 1 d . . . C16 C 1.12680(14) -0.0730(3) 0.9867(2) 0.0216(7) Uani 1 1 d . . . C17 C 1.18944(14) -0.0621(4) 1.0557(2) 0.0221(7) Uani 1 1 d . . . H17 H 1.2080 -0.1294 1.0983 0.027 Uiso 1 1 calc R . . C18 C 1.22696(14) 0.0438(3) 1.0657(2) 0.0203(7) Uani 1 1 d . . . C19 C 1.29013(15) 0.0553(4) 1.1390(2) 0.0272(8) Uani 1 1 d . . . H19 H 1.3078 -0.0096 1.1825 0.033 Uiso 1 1 calc R . . C20 C 1.32582(14) 0.1585(4) 1.1479(2) 0.0289(9) Uani 1 1 d . . . H20 H 1.3682 0.1650 1.1974 0.035 Uiso 1 1 calc R . . C21 C 1.30046(15) 0.2553(4) 1.0843(2) 0.0267(8) Uani 1 1 d . . . H21 H 1.3257 0.3277 1.0916 0.032 Uiso 1 1 calc R . . C22 C 1.23963(14) 0.2466(4) 1.0118(2) 0.0233(7) Uani 1 1 d . . . H22 H 1.2231 0.3131 0.9693 0.028 Uiso 1 1 calc R . . C23 C 1.20138(14) 0.1393(3) 0.9998(2) 0.0196(7) Uani 1 1 d . . . C24 C 1.13801(13) 0.1217(3) 0.92426(19) 0.0185(6) Uani 1 1 d . . . C25 C 1.11280(11) 0.1940(4) 0.84697(16) 0.0194(6) Uani 1 1 d . . . C26 C 1.14343(12) 0.1806(5) 0.81705(17) 0.0228(6) Uani 1 1 d . . . C27 C 1.19642(15) 0.0959(4) 0.8560(2) 0.0258(8) Uani 1 1 d . . . H27 H 1.2133 0.0461 0.9046 0.031 Uiso 1 1 calc R . . C28 C 1.22361(17) 0.0847(4) 0.8248(2) 0.0343(9) Uani 1 1 d . . . H28 H 1.2592 0.0278 0.8522 0.041 Uiso 1 1 calc R . . C29 C 1.19939(17) 0.1565(4) 0.7526(2) 0.0377(10) Uani 1 1 d . . . H29 H 1.2190 0.1496 0.7319 0.045 Uiso 1 1 calc R . . C30 C 1.14845(18) 0.2348(4) 0.7130(2) 0.0361(9) Uani 1 1 d . . . H30 H 1.1319 0.2816 0.6637 0.043 Uiso 1 1 calc R . . C31 C 1.11856(15) 0.2497(4) 0.7433(2) 0.0273(8) Uani 1 1 d . . . C32 C 1.06574(16) 0.3326(4) 0.7027(2) 0.0313(8) Uani 1 1 d . . . H32 H 1.0508 0.3821 0.6549 0.038 Uiso 1 1 calc R . . C33 C 1.03419(15) 0.3464(4) 0.7281(2) 0.0284(8) Uani 1 1 d . . . C34 C 1.05846(13) 0.2699(3) 0.7997(2) 0.0206(7) Uani 1 1 d . . . C35 C 1.11990(15) -0.2699(4) 1.0881(2) 0.0250(8) Uani 1 1 d . . . C36 C 1.12023(18) -0.4057(4) 1.1101(3) 0.0336(9) Uani 1 1 d . . . H36 H 1.1046 -0.4781 1.0710 0.040 Uiso 1 1 calc R . . C37 C 1.1427(2) -0.4383(4) 1.1876(3) 0.0370(10) Uani 1 1 d . . . H37 H 1.1422 -0.5318 1.2011 0.044 Uiso 1 1 calc R . . C38 C 1.16586(17) -0.3333(5) 1.2455(2) 0.0384(10) Uani 1 1 d . . . H38 H 1.1818 -0.3549 1.2990 0.046 Uiso 1 1 calc R . . C39 C 1.16560(17) -0.1979(4) 1.2250(2) 0.0330(9) Uani 1 1 d . . . H39 H 1.1812 -0.1259 1.2644 0.040 Uiso 1 1 calc R . . C40 C 1.14273(15) -0.1663(4) 1.1472(2) 0.0272(8) Uani 1 1 d . . . H40 H 1.1426 -0.0723 1.1338 0.033 Uiso 1 1 calc R . . C41 C 1.09980(18) -0.3814(4) 0.9420(3) 0.0377(9) Uani 1 1 d . . . H41A H 1.0787 -0.4641 0.9386 0.057 Uiso 1 1 calc R . . H41B H 1.1444 -0.3991 0.9804 0.057 Uiso 1 1 calc R . . H41C H 1.0842 -0.3601 0.8872 0.057 Uiso 1 1 calc R . . C42 C 1.00025(16) -0.2024(4) 0.9116(3) 0.0392(9) Uani 1 1 d . . . H42A H 0.9816 -0.1898 0.8546 0.059 Uiso 1 1 calc R . . H42B H 0.9929 -0.1192 0.9296 0.059 Uiso 1 1 calc R . . H42C H 0.9816 -0.2833 0.9146 0.059 Uiso 1 1 calc R . . C43 C 0.99714(15) 0.6422(4) 0.6628(2) 0.0338(9) Uani 1 1 d . . . C44 C 1.00933(17) 0.7549(4) 0.7114(3) 0.0383(9) Uani 1 1 d . . . H44 H 1.0014 0.7470 0.7464 0.046 Uiso 1 1 calc R . . C45 C 1.03287(19) 0.8791(5) 0.7100(3) 0.0440(10) Uani 1 1 d . . . H45 H 1.0397 0.9552 0.7428 0.053 Uiso 1 1 calc R . . C46 C 1.0462(2) 0.8924(4) 0.6619(3) 0.0441(10) Uani 1 1 d . . . H46 H 1.0632 0.9769 0.6624 0.053 Uiso 1 1 calc R . . C47 C 1.03525(18) 0.7845(5) 0.6128(2) 0.0422(10) Uani 1 1 d . . . H47 H 1.0444 0.7939 0.5791 0.051 Uiso 1 1 calc R . . C48 C 1.01048(17) 0.6607(4) 0.6126(2) 0.0382(10) Uani 1 1 d . . . H48 H 1.0023 0.5868 0.5778 0.046 Uiso 1 1 calc R . . C49 C 0.9127(2) 0.4061(6) 0.5553(3) 0.0706(17) Uani 1 1 d . . . H49A H 0.9055 0.3064 0.5547 0.106 Uiso 1 1 calc R . . H49B H 0.9311 0.4217 0.5319 0.106 Uiso 1 1 calc R . . H49C H 0.8733 0.4561 0.5224 0.106 Uiso 1 1 calc R . . C50 C 0.9274(2) 0.4940(5) 0.7028(4) 0.0628(15) Uani 1 1 d . . . H50A H 0.8964 0.5679 0.6713 0.094 Uiso 1 1 calc R . . H50B H 0.9579 0.5192 0.7614 0.094 Uiso 1 1 calc R . . H50C H 0.9071 0.4068 0.6959 0.094 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 Pd1 0.01369(10) 0.02361(12) 0.01600(10) -0.00072(11) 0.00961(8) -0.00037(10) P1 0.0132(3) 0.0234(5) 0.0186(4) -0.0004(3) 0.0103(3) -0.0004(3) Si1 0.0241(4) 0.0235(5) 0.0309(5) 0.0006(4) 0.0202(4) -0.0023(4) Si2 0.0213(5) 0.0410(7) 0.0438(6) 0.0207(5) 0.0174(5) 0.0065(4) Cl1 0.0158(3) 0.0441(7) 0.0174(3) 0.0022(3) 0.0107(3) 0.0047(3) O1 0.0130(10) 0.0324(14) 0.0221(11) -0.0034(10) 0.0123(9) -0.0001(9) O2 0.0112(10) 0.0229(13) 0.0213(11) -0.0002(9) 0.0102(9) -0.0007(9) O3 0.0163(10) 0.0212(13) 0.0252(12) 0.0024(9) 0.0147(10) 0.0015(9) C1 0.0232(14) 0.015(2) 0.0281(16) 0.0012(13) 0.0197(13) 0.0003(12) C2 0.0101(14) 0.0219(17) 0.0245(17) -0.0002(14) 0.0105(13) 0.0002(12) C3 0.0185(15) 0.0216(17) 0.0219(17) -0.0001(13) 0.0140(14) -0.0002(12) C4 0.0162(15) 0.0268(19) 0.0202(16) -0.0035(14) 0.0102(14) -0.0028(13) C5 0.0163(13) 0.019(2) 0.0232(15) 0.0029(13) 0.0124(12) 0.0021(12) C6 0.0215(13) 0.0214(15) 0.0252(14) -0.0012(18) 0.0167(12) -0.0011(17) C7 0.0219(16) 0.032(2) 0.0230(17) -0.0031(14) 0.0149(15) 0.0006(14) C8 0.0305(19) 0.055(3) 0.0296(19) -0.016(2) 0.0194(16) -0.0063(19) C9 0.040(2) 0.031(2) 0.038(2) -0.0067(17) 0.0272(19) 0.0009(17) C10 0.039(2) 0.050(3) 0.032(2) -0.0046(18) 0.0273(18) -0.0038(18) C11 0.0187(13) 0.0340(18) 0.0277(15) 0.001(2) 0.0167(12) 0.0018(18) C12 0.032(2) 0.052(3) 0.056(3) -0.013(2) 0.035(2) -0.0027(18) C13 0.033(2) 0.046(3) 0.044(2) -0.0058(19) 0.0295(19) -0.0089(17) C14 0.036(2) 0.069(3) 0.052(3) 0.027(2) 0.034(2) 0.024(2) C15 0.0119(14) 0.0218(18) 0.0193(16) -0.0017(13) 0.0100(13) -0.0006(12) C16 0.0200(16) 0.0232(18) 0.0252(17) 0.0022(14) 0.0167(15) 0.0028(13) C17 0.0210(16) 0.0243(18) 0.0244(17) 0.0069(14) 0.0168(15) 0.0061(13) C18 0.0175(15) 0.0221(18) 0.0232(17) -0.0001(13) 0.0146(14) 0.0019(13) C19 0.0195(16) 0.038(2) 0.0240(18) 0.0030(15) 0.0147(15) 0.0037(14) C20 0.0164(14) 0.036(3) 0.0273(17) -0.0027(15) 0.0120(13) -0.0007(14) C21 0.0216(16) 0.0282(19) 0.032(2) -0.0056(15) 0.0189(16) -0.0065(14) C22 0.0202(16) 0.0255(18) 0.0244(18) 0.0015(13) 0.0151(15) -0.0002(13) C23 0.0163(14) 0.0218(18) 0.0238(17) -0.0001(12) 0.0149(14) 0.0009(12) C24 0.0146(14) 0.0212(16) 0.0203(16) 0.0015(13) 0.0121(13) 0.0029(12) C25 0.0151(12) 0.0209(15) 0.0211(14) 0.0024(17) 0.0119(11) -0.0001(16) C26 0.0208(13) 0.0226(16) 0.0255(15) -0.0041(18) 0.0159(12) -0.0057(17) C27 0.0271(17) 0.0227(19) 0.0339(19) -0.0029(15) 0.0232(16) -0.0014(14) C28 0.038(2) 0.029(2) 0.052(2) -0.0057(18) 0.037(2) -0.0027(16) C29 0.047(2) 0.038(3) 0.053(2) -0.0085(18) 0.044(2) -0.0071(17) C30 0.050(2) 0.035(2) 0.039(2) -0.0028(16) 0.036(2) -0.0115(17) C31 0.0269(17) 0.0294(19) 0.0295(19) -0.0012(14) 0.0207(16) -0.0062(14) C32 0.0315(19) 0.036(2) 0.0267(19) 0.0072(15) 0.0199(17) -0.0026(15) C33 0.0218(16) 0.031(2) 0.0249(18) 0.0061(15) 0.0130(15) -0.0020(14) C34 0.0176(15) 0.0204(18) 0.0255(17) 0.0003(14) 0.0153(14) -0.0008(13) C35 0.0228(16) 0.023(2) 0.0379(19) 0.0024(14) 0.0241(16) 0.0028(13) C36 0.039(2) 0.025(2) 0.045(2) 0.0018(17) 0.032(2) 0.0029(16) C37 0.052(3) 0.022(2) 0.055(3) 0.0082(19) 0.043(2) 0.0059(18) C38 0.0438(19) 0.042(3) 0.040(2) 0.013(2) 0.0324(17) 0.0119(19) C39 0.036(2) 0.037(2) 0.035(2) -0.0013(18) 0.0277(19) -0.0001(17) C40 0.0298(19) 0.025(2) 0.037(2) 0.0056(16) 0.0269(18) 0.0009(14) C41 0.045(2) 0.033(2) 0.045(2) -0.0049(18) 0.034(2) -0.0082(18) C42 0.0299(19) 0.036(2) 0.049(2) 0.0059(19) 0.0258(18) -0.0038(17) C43 0.0197(16) 0.040(2) 0.0313(19) 0.0110(16) 0.0134(16) 0.0069(14) C44 0.035(2) 0.046(3) 0.039(2) 0.0088(19) 0.0278(19) 0.0128(17) C45 0.050(2) 0.036(2) 0.047(2) -0.0047(19) 0.034(2) 0.0020(19) C46 0.054(3) 0.032(2) 0.055(3) -0.0055(19) 0.041(2) -0.0087(19) C47 0.052(2) 0.044(3) 0.047(2) 0.001(2) 0.040(2) -0.0064(19) C48 0.044(2) 0.035(3) 0.0349(19) -0.0020(17) 0.0265(17) -0.0030(17) C49 0.040(3) 0.067(4) 0.055(3) 0.030(3) 0.012(2) -0.013(2) C50 0.049(3) 0.058(3) 0.104(4) 0.045(3) 0.061(3) 0.030(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 Pd1 C1 2.010(3) . ? Pd1 P1 2.1587(8) . ? Pd1 Cl1 2.4127(8) 2_757 ? Pd1 Cl1 2.4155(7) . ? P1 O1 1.592(2) . ? P1 O2 1.593(2) . ? P1 O3 1.594(2) . ? Si1 C42 1.857(4) . ? Si1 C41 1.873(4) . ? Si1 C35 1.883(4) . ? Si1 C16 1.898(3) . ? Si2 C50 1.856(5) . ? Si2 C49 1.873(6) . ? Si2 C43 1.883(4) . ? Si2 C33 1.891(4) . ? Cl1 Pd1 2.4126(7) 2_757 ? O1 C2 1.433(3) . ? O2 C15 1.420(4) . ? O3 C34 1.414(4) . ? C1 C2 1.377(5) . ? C1 C6 1.401(4) . ? C2 C3 1.396(4) . ? C3 C4 1.403(4) . ? C3 C7 1.539(5) . ? C4 C5 1.396(5) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 C11 1.539(4) . ? C6 H6 0.9500 . ? C7 C10 1.528(5) . ? C7 C9 1.529(5) . ? C7 C8 1.534(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.528(5) . ? C11 C12 1.531(5) . ? C11 C13 1.536(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.373(5) . ? C15 C16 1.411(5) . ? C16 C17 1.385(5) . ? C17 C18 1.406(5) . ? C17 H17 0.9500 . ? C18 C19 1.415(5) . ? C18 C23 1.426(5) . ? C19 C20 1.360(5) . ? C19 H19 0.9500 . ? C20 C21 1.402(5) . ? C20 H20 0.9500 . ? C21 C22 1.373(5) . ? C21 H21 0.9500 . ? C22 C23 1.414(4) . ? C22 H22 0.9500 . ? C23 C24 1.437(4) . ? C24 C25 1.490(4) . ? C25 C34 1.384(4) . ? C25 C26 1.441(4) . ? C26 C31 1.415(5) . ? C26 C27 1.420(5) . ? C27 C28 1.368(5) . ? C27 H27 0.9500 . ? C28 C29 1.407(6) . ? C28 H28 0.9500 . ? C29 C30 1.343(6) . ? C29 H29 0.9500 . ? C30 C31 1.429(5) . ? C30 H30 0.9500 . ? C31 C32 1.402(5) . ? C32 C33 1.378(5) . ? C32 H32 0.9500 . ? C33 C34 1.419(5) . ? C35 C36 1.391(6) . ? C35 C40 1.398(5) . ? C36 C37 1.386(6) . ? C36 H36 0.9500 . ? C37 C38 1.389(6) . ? C37 H37 0.9500 . ? C38 C39 1.377(6) . ? C38 H38 0.9500 . ? C39 C40 1.386(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.388(6) . ? C43 C48 1.415(5) . ? C44 C45 1.392(6) . ? C44 H44 0.9500 . ? C45 C46 1.365(6) . ? C45 H45 0.9500 . ? C46 C47 1.370(6) . ? C46 H46 0.9500 . ? C47 C48 1.395(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 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 Pd1 P1 79.57(9) . . ? C1 Pd1 Cl1 178.46(9) . 2_757 ? P1 Pd1 Cl1 99.04(3) . 2_757 ? C1 Pd1 Cl1 96.12(9) . . ? P1 Pd1 Cl1 174.51(3) . . ? Cl1 Pd1 Cl1 85.31(3) 2_757 . ? O1 P1 O2 97.18(12) . . ? O1 P1 O3 108.79(12) . . ? O2 P1 O3 104.80(11) . . ? O1 P1 Pd1 109.51(8) . . ? O2 P1 Pd1 122.65(9) . . ? O3 P1 Pd1 112.41(9) . . ? C42 Si1 C41 110.1(2) . . ? C42 Si1 C35 109.76(17) . . ? C41 Si1 C35 108.45(17) . . ? C42 Si1 C16 113.04(17) . . ? C41 Si1 C16 108.30(16) . . ? C35 Si1 C16 107.03(15) . . ? C50 Si2 C49 112.1(3) . . ? C50 Si2 C43 111.0(2) . . ? C49 Si2 C43 105.6(2) . . ? C50 Si2 C33 113.74(18) . . ? C49 Si2 C33 106.8(2) . . ? C43 Si2 C33 107.17(15) . . ? Pd1 Cl1 Pd1 92.91(3) 2_757 . ? C2 O1 P1 112.62(19) . . ? C15 O2 P1 119.2(2) . . ? C34 O3 P1 123.5(2) . . ? C2 C1 C6 118.1(3) . . ? C2 C1 Pd1 120.7(2) . . ? C6 C1 Pd1 121.1(2) . . ? C1 C2 C3 124.5(3) . . ? C1 C2 O1 116.5(2) . . ? C3 C2 O1 119.1(3) . . ? C2 C3 C4 114.6(3) . . ? C2 C3 C7 123.6(3) . . ? C4 C3 C7 121.6(3) . . ? C5 C4 C3 123.7(3) . . ? C5 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C11 121.0(3) . . ? C4 C5 C11 120.8(3) . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C10 C7 C9 110.2(3) . . ? C10 C7 C3 110.6(3) . . ? C9 C7 C3 108.8(3) . . ? C10 C7 C8 107.4(3) . . ? C9 C7 C8 107.8(3) . . ? C3 C7 C8 112.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 108.0(4) . . ? C14 C11 C13 110.0(3) . . ? C12 C11 C13 107.7(3) . . ? C14 C11 C5 110.4(3) . . ? C12 C11 C5 112.2(3) . . ? C13 C11 C5 108.4(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 C16 125.5(3) . . ? C24 C15 O2 117.6(3) . . ? C16 C15 O2 116.8(3) . . ? C17 C16 C15 115.2(3) . . ? C17 C16 Si1 117.3(2) . . ? C15 C16 Si1 126.9(2) . . ? C16 C17 C18 123.1(3) . . ? C16 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C19 121.3(3) . . ? C17 C18 C23 119.4(3) . . ? C19 C18 C23 119.2(3) . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 118.5(3) . . ? C22 C23 C24 123.1(3) . . ? C18 C23 C24 118.5(3) . . ? C15 C24 C23 117.4(3) . . ? C15 C24 C25 121.1(3) . . ? C23 C24 C25 121.1(3) . . ? C34 C25 C26 117.8(3) . . ? C34 C25 C24 122.0(3) . . ? C26 C25 C24 120.1(3) . . ? C31 C26 C27 117.6(3) . . ? C31 C26 C25 119.2(3) . . ? C27 C26 C25 123.2(3) . . ? C28 C27 C26 121.3(3) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 120.6(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 121.6(4) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C26 119.0(3) . . ? C32 C31 C30 121.8(3) . . ? C26 C31 C30 119.1(3) . . ? C33 C32 C31 123.9(3) . . ? C33 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? C32 C33 C34 115.7(3) . . ? C32 C33 Si2 114.7(3) . . ? C34 C33 Si2 129.6(3) . . ? C25 C34 O3 118.2(3) . . ? C25 C34 C33 124.2(3) . . ? O3 C34 C33 117.6(3) . . ? C36 C35 C40 117.3(3) . . ? C36 C35 Si1 119.9(3) . . ? C40 C35 Si1 122.7(3) . . ? C37 C36 C35 121.8(4) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C38 C37 C36 119.6(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 119.8(4) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.2(4) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C35 121.3(4) . . ? C39 C40 H40 119.3 . . ? C35 C40 H40 119.3 . . ? Si1 C41 H41A 109.5 . . ? Si1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C42 H42A 109.5 . . ? Si1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 116.2(3) . . ? C44 C43 Si2 123.0(3) . . ? C48 C43 Si2 120.8(3) . . ? C43 C44 C45 121.7(4) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C46 C45 C44 120.5(4) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.3(4) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 119.4(4) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C47 C48 C43 121.9(4) . . ? C47 C48 H48 119.0 . . ? C43 C48 H48 119.0 . . ? Si2 C49 H49A 109.5 . . ? Si2 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si2 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si2 C50 H50A 109.5 . . ? Si2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 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 C1 Pd1 P1 O1 -8.81(14) . . . . ? Cl1 Pd1 P1 O1 171.86(10) 2_757 . . . ? Cl1 Pd1 P1 O1 29.8(4) . . . . ? C1 Pd1 P1 O2 -121.42(14) . . . . ? Cl1 Pd1 P1 O2 59.25(10) 2_757 . . . ? Cl1 Pd1 P1 O2 -82.9(3) . . . . ? C1 Pd1 P1 O3 112.24(13) . . . . ? Cl1 Pd1 P1 O3 -67.09(9) 2_757 . . . ? Cl1 Pd1 P1 O3 150.8(3) . . . . ? C1 Pd1 Cl1 Pd1 166.32(9) . . . 2_757 ? P1 Pd1 Cl1 Pd1 128.3(3) . . . 2_757 ? Cl1 Pd1 Cl1 Pd1 -14.26(4) 2_757 . . 2_757 ? O2 P1 O1 C2 136.4(2) . . . . ? O3 P1 O1 C2 -115.2(2) . . . . ? Pd1 P1 O1 C2 8.0(2) . . . . ? O1 P1 O2 C15 167.2(2) . . . . ? O3 P1 O2 C15 55.6(2) . . . . ? Pd1 P1 O2 C15 -74.1(2) . . . . ? O1 P1 O3 C34 -71.0(2) . . . . ? O2 P1 O3 C34 32.1(2) . . . . ? Pd1 P1 O3 C34 167.52(19) . . . . ? P1 Pd1 C1 C2 9.5(3) . . . . ? Cl1 Pd1 C1 C2 35(4) 2_757 . . . ? Cl1 Pd1 C1 C2 -167.1(3) . . . . ? P1 Pd1 C1 C6 -173.8(3) . . . . ? Cl1 Pd1 C1 C6 -148(3) 2_757 . . . ? Cl1 Pd1 C1 C6 9.7(3) . . . . ? C6 C1 C2 C3 -3.9(5) . . . . ? Pd1 C1 C2 C3 172.9(3) . . . . ? C6 C1 C2 O1 175.8(3) . . . . ? Pd1 C1 C2 O1 -7.4(4) . . . . ? P1 O1 C2 C1 -1.2(4) . . . . ? P1 O1 C2 C3 178.5(2) . . . . ? C1 C2 C3 C4 4.5(5) . . . . ? O1 C2 C3 C4 -175.2(3) . . . . ? C1 C2 C3 C7 -170.5(3) . . . . ? O1 C2 C3 C7 9.8(5) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C7 C3 C4 C5 173.9(3) . . . . ? C3 C4 C5 C6 -2.3(5) . . . . ? C3 C4 C5 C11 -178.7(3) . . . . ? C4 C5 C6 C1 3.0(5) . . . . ? C11 C5 C6 C1 179.4(4) . . . . ? C2 C1 C6 C5 -0.1(5) . . . . ? Pd1 C1 C6 C5 -176.9(3) . . . . ? C2 C3 C7 C10 -62.3(4) . . . . ? C4 C3 C7 C10 123.0(3) . . . . ? C2 C3 C7 C9 58.8(4) . . . . ? C4 C3 C7 C9 -115.9(3) . . . . ? C2 C3 C7 C8 177.9(3) . . . . ? C4 C3 C7 C8 3.2(5) . . . . ? C6 C5 C11 C14 136.5(4) . . . . ? C4 C5 C11 C14 -47.3(5) . . . . ? C6 C5 C11 C12 15.9(5) . . . . ? C4 C5 C11 C12 -167.8(4) . . . . ? C6 C5 C11 C13 -102.9(4) . . . . ? C4 C5 C11 C13 73.3(4) . . . . ? P1 O2 C15 C24 -67.3(3) . . . . ? P1 O2 C15 C16 116.5(3) . . . . ? C24 C15 C16 C17 4.4(5) . . . . ? O2 C15 C16 C17 -179.7(3) . . . . ? C24 C15 C16 Si1 -166.2(3) . . . . ? O2 C15 C16 Si1 9.6(4) . . . . ? C42 Si1 C16 C17 157.2(3) . . . . ? C41 Si1 C16 C17 -80.6(3) . . . . ? C35 Si1 C16 C17 36.2(3) . . . . ? C42 Si1 C16 C15 -32.4(4) . . . . ? C41 Si1 C16 C15 89.9(3) . . . . ? C35 Si1 C16 C15 -153.3(3) . . . . ? C15 C16 C17 C18 3.7(5) . . . . ? Si1 C16 C17 C18 175.3(3) . . . . ? C16 C17 C18 C19 176.7(3) . . . . ? C16 C17 C18 C23 -5.0(5) . . . . ? C17 C18 C19 C20 -179.9(3) . . . . ? C23 C18 C19 C20 1.9(5) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 -1.0(5) . . . . ? C20 C21 C22 C23 -0.1(5) . . . . ? C21 C22 C23 C18 2.0(5) . . . . ? C21 C22 C23 C24 -177.7(3) . . . . ? C17 C18 C23 C22 178.8(3) . . . . ? C19 C18 C23 C22 -2.9(5) . . . . ? C17 C18 C23 C24 -1.4(5) . . . . ? C19 C18 C23 C24 176.9(3) . . . . ? C16 C15 C24 C23 -10.6(5) . . . . ? O2 C15 C24 C23 173.5(3) . . . . ? C16 C15 C24 C25 163.1(3) . . . . ? O2 C15 C24 C25 -12.8(4) . . . . ? C22 C23 C24 C15 -171.6(3) . . . . ? C18 C23 C24 C15 8.6(4) . . . . ? C22 C23 C24 C25 14.8(5) . . . . ? C18 C23 C24 C25 -165.0(3) . . . . ? C15 C24 C25 C34 56.8(5) . . . . ? C23 C24 C25 C34 -129.8(3) . . . . ? C15 C24 C25 C26 -120.2(4) . . . . ? C23 C24 C25 C26 53.2(5) . . . . ? C34 C25 C26 C31 2.7(5) . . . . ? C24 C25 C26 C31 179.8(3) . . . . ? C34 C25 C26 C27 -174.5(3) . . . . ? C24 C25 C26 C27 2.6(5) . . . . ? C31 C26 C27 C28 1.9(5) . . . . ? C25 C26 C27 C28 179.1(4) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C27 C28 C29 C30 -1.2(6) . . . . ? C28 C29 C30 C31 1.2(6) . . . . ? C27 C26 C31 C32 179.1(3) . . . . ? C25 C26 C31 C32 1.8(5) . . . . ? C27 C26 C31 C30 -1.8(5) . . . . ? C25 C26 C31 C30 -179.1(3) . . . . ? C29 C30 C31 C32 179.3(4) . . . . ? C29 C30 C31 C26 0.3(5) . . . . ? C26 C31 C32 C33 -3.2(6) . . . . ? C30 C31 C32 C33 177.8(4) . . . . ? C31 C32 C33 C34 -0.1(5) . . . . ? C31 C32 C33 Si2 177.3(3) . . . . ? C50 Si2 C33 C32 -177.3(3) . . . . ? C49 Si2 C33 C32 58.5(3) . . . . ? C43 Si2 C33 C32 -54.3(3) . . . . ? C50 Si2 C33 C34 -0.3(4) . . . . ? C49 Si2 C33 C34 -124.5(4) . . . . ? C43 Si2 C33 C34 122.7(3) . . . . ? C26 C25 C34 O3 176.5(3) . . . . ? C24 C25 C34 O3 -0.6(5) . . . . ? C26 C25 C34 C33 -6.3(5) . . . . ? C24 C25 C34 C33 176.6(3) . . . . ? P1 O3 C34 C25 -64.8(4) . . . . ? P1 O3 C34 C33 117.8(3) . . . . ? C32 C33 C34 C25 5.0(5) . . . . ? Si2 C33 C34 C25 -171.9(3) . . . . ? C32 C33 C34 O3 -177.8(3) . . . . ? Si2 C33 C34 O3 5.3(5) . . . . ? C42 Si1 C35 C36 85.7(3) . . . . ? C41 Si1 C35 C36 -34.6(3) . . . . ? C16 Si1 C35 C36 -151.3(3) . . . . ? C42 Si1 C35 C40 -90.1(3) . . . . ? C41 Si1 C35 C40 149.6(3) . . . . ? C16 Si1 C35 C40 32.9(3) . . . . ? C40 C35 C36 C37 -0.5(5) . . . . ? Si1 C35 C36 C37 -176.6(3) . . . . ? C35 C36 C37 C38 -0.3(6) . . . . ? C36 C37 C38 C39 0.9(6) . . . . ? C37 C38 C39 C40 -0.5(6) . . . . ? C38 C39 C40 C35 -0.4(5) . . . . ? C36 C35 C40 C39 0.9(5) . . . . ? Si1 C35 C40 C39 176.9(3) . . . . ? C50 Si2 C43 C44 22.4(4) . . . . ? C49 Si2 C43 C44 144.0(3) . . . . ? C33 Si2 C43 C44 -102.3(3) . . . . ? C50 Si2 C43 C48 -159.4(3) . . . . ? C49 Si2 C43 C48 -37.7(4) . . . . ? C33 Si2 C43 C48 75.9(3) . . . . ? C48 C43 C44 C45 0.5(5) . . . . ? Si2 C43 C44 C45 178.8(3) . . . . ? C43 C44 C45 C46 -1.7(6) . . . . ? C44 C45 C46 C47 1.5(7) . . . . ? C45 C46 C47 C48 -0.2(6) . . . . ? C46 C47 C48 C43 -1.0(6) . . . . ? C44 C43 C48 C47 0.8(5) . . . . ? Si2 C43 C48 C47 -177.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 65.11 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.544 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.062 # Attachment '- 9d.cif' data_yc_3_5_5_0m _database_code_depnum_ccdc_archive 'CCDC 815809' #TrackingRef '- 9d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C140 H120 Cl2 O8 P2 Pd2 Si4, C5 H12' _chemical_formula_sum 'C145 H132 Cl2 O8 P2 Pd2 Si4' _chemical_formula_weight 2460.51 _chemical_absolute_configuration ad 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.4938(6) _cell_length_b 30.6692(13) _cell_length_c 14.4991(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.461(3) _cell_angle_gamma 90.00 _cell_volume 6180.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 73502 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.58 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2556 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9669 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _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 Apex II kappa with CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 73461 _diffrn_reflns_av_R_equivalents 0.1448 _diffrn_reflns_av_sigmaI/netI 0.1903 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.58 _reflns_number_total 27759 _reflns_number_gt 16932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+39.1891P] 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 0.01(3) _refine_ls_number_reflns 27759 _refine_ls_number_parameters 1484 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1736 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _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 0.27632(5) 0.75462(3) 0.90395(5) 0.01975(17) Uani 1 1 d . . . Pd2 Pd 0.39545(5) 0.81909(2) 0.78638(5) 0.01916(17) Uani 1 1 d . . . P1 P 0.22706(18) 0.68880(9) 0.87533(18) 0.0208(6) Uani 1 1 d . . . P2 P 0.36373(18) 0.88535(9) 0.74249(19) 0.0202(6) Uani 1 1 d . . . Si1 Si -0.0085(2) 0.66100(10) 0.6063(2) 0.0260(7) Uani 1 1 d . . . Si2 Si 0.4848(2) 0.66482(10) 1.09441(19) 0.0211(6) Uani 1 1 d . . . Si3 Si 0.0798(2) 0.90012(12) 0.5323(2) 0.0320(8) Uani 1 1 d . . . Si4 Si 0.5901(2) 0.90847(10) 0.9976(2) 0.0231(6) Uani 1 1 d . . . Cl1 Cl 0.41865(17) 0.74458(8) 0.84683(17) 0.0235(6) Uani 1 1 d . . . Cl2 Cl 0.34187(17) 0.82812(8) 0.92995(17) 0.0229(6) Uani 1 1 d . . . O1 O 0.1388(4) 0.6794(2) 0.9146(5) 0.0224(16) Uani 1 1 d . . . O2 O 0.1975(5) 0.6788(2) 0.7624(5) 0.0254(16) Uani 1 1 d . . . O3 O 0.2936(5) 0.6485(2) 0.9239(5) 0.0208(16) Uani 1 1 d . . . O4 O 0.1570(5) 0.8334(2) 0.9802(5) 0.0303(18) Uani 1 1 d . . . H4 H 0.1940 0.8328 0.9449 0.045 Uiso 1 1 calc R . . O5 O 0.3927(5) 0.8955(2) 0.6474(4) 0.0210(15) Uani 1 1 d . . . O6 O 0.2527(5) 0.8938(2) 0.7258(5) 0.0241(16) Uani 1 1 d . . . O7 O 0.4152(5) 0.9260(2) 0.8061(5) 0.0222(16) Uani 1 1 d . . . O8 O 0.4683(5) 0.7420(2) 0.6597(5) 0.0262(17) Uani 1 1 d . . . H8 H 0.4411 0.7421 0.7038 0.039 Uiso 1 1 calc R . . C1 C 0.1538(6) 0.7562(4) 0.9496(6) 0.019(2) Uani 1 1 d . . . C2 C 0.1044(6) 0.7171(3) 0.9515(6) 0.015(2) Uani 1 1 d . . . C3 C 0.0267(7) 0.7110(4) 0.9884(7) 0.025(2) Uani 1 1 d . . . C4 C -0.0030(7) 0.7501(4) 1.0215(8) 0.031(3) Uani 1 1 d . . . H4A H -0.0574 0.7484 1.0455 0.037 Uiso 1 1 calc R . . C5 C 0.0387(8) 0.7909(4) 1.0231(8) 0.031(3) Uani 1 1 d . . . C6 C 0.1183(7) 0.7926(3) 0.9828(7) 0.021(2) Uani 1 1 d . . . C7 C -0.0210(8) 0.6673(4) 0.9974(8) 0.032(3) Uani 1 1 d . . . C8 C 0.0519(8) 0.6377(4) 1.0718(9) 0.040(3) Uani 1 1 d . . . H8A H 0.0732 0.6528 1.1338 0.060 Uiso 1 1 calc R . . H8B H 0.1076 0.6316 1.0483 0.060 Uiso 1 1 calc R . . H8C H 0.0204 0.6103 1.0799 0.060 Uiso 1 1 calc R . . C9 C -0.1083(10) 0.6726(4) 1.0357(11) 0.059(4) Uani 1 1 d . . . H9A H -0.0869 0.6815 1.1034 0.089 Uiso 1 1 calc R . . H9B H -0.1427 0.6448 1.0303 0.089 Uiso 1 1 calc R . . H9C H -0.1514 0.6949 0.9981 0.089 Uiso 1 1 calc R . . C10 C -0.0549(8) 0.6440(4) 0.8991(9) 0.042(3) Uani 1 1 d . . . H10A H -0.0810 0.6153 0.9075 0.063 Uiso 1 1 calc R . . H10B H -0.0002 0.6405 0.8726 0.063 Uiso 1 1 calc R . . H10C H -0.1048 0.6615 0.8549 0.063 Uiso 1 1 calc R . . C11 C 0.0045(8) 0.8319(4) 1.0630(9) 0.035(3) Uani 1 1 d . . . C12 C 0.0829(9) 0.8490(4) 1.1503(10) 0.048(4) Uani 1 1 d . . . H12A H 0.0596 0.8751 1.1754 0.072 Uiso 1 1 calc R . . H12B H 0.1406 0.8562 1.1309 0.072 Uiso 1 1 calc R . . H12C H 0.0987 0.8265 1.2003 0.072 Uiso 1 1 calc R . . C13 C -0.0301(8) 0.8674(4) 0.9814(9) 0.041(3) Uani 1 1 d . . . H13A H -0.0634 0.8909 1.0046 0.061 Uiso 1 1 calc R . . H13B H -0.0741 0.8539 0.9245 0.061 Uiso 1 1 calc R . . H13C H 0.0258 0.8792 0.9645 0.061 Uiso 1 1 calc R . . C14 C -0.0858(9) 0.8211(5) 1.0957(11) 0.057(4) Uani 1 1 d . . . H14A H -0.0804 0.7915 1.1218 0.086 Uiso 1 1 calc R . . H14B H -0.1433 0.8232 1.0405 0.086 Uiso 1 1 calc R . . H14C H -0.0910 0.8419 1.1454 0.086 Uiso 1 1 calc R . . C15 C 0.1883(7) 0.6356(4) 0.7262(6) 0.022(2) Uani 1 1 d . . . C16 C 0.0965(7) 0.6240(4) 0.6660(7) 0.026(2) Uani 1 1 d . . . C17 C 0.0921(8) 0.5813(4) 0.6322(8) 0.030(3) Uani 1 1 d . . . H17 H 0.0318 0.5714 0.5925 0.036 Uiso 1 1 calc R . . C18 C 0.1673(7) 0.5522(4) 0.6513(7) 0.026(2) Uani 1 1 d . . . C19 C 0.1576(8) 0.5092(4) 0.6154(9) 0.038(3) Uani 1 1 d . . . H19 H 0.0965 0.4995 0.5771 0.045 Uiso 1 1 calc R . . C20 C 0.2337(8) 0.4813(4) 0.6344(8) 0.034(3) Uani 1 1 d . . . H20 H 0.2255 0.4526 0.6085 0.041 Uiso 1 1 calc R . . C21 C 0.3243(7) 0.4948(4) 0.6922(7) 0.027(2) Uani 1 1 d . . . H21 H 0.3772 0.4752 0.7057 0.032 Uiso 1 1 calc R . . C22 C 0.3362(7) 0.5357(4) 0.7286(7) 0.025(2) Uani 1 1 d . . . H22 H 0.3971 0.5441 0.7697 0.030 Uiso 1 1 calc R . . C23 C 0.2599(7) 0.5663(4) 0.7068(7) 0.025(2) Uani 1 1 d . . . C24 C 0.2706(7) 0.6110(3) 0.7437(6) 0.017(2) Uani 1 1 d . . . C25 C 0.3675(7) 0.6267(3) 0.8054(7) 0.019(2) Uani 1 1 d . . . C26 C 0.4510(7) 0.6250(4) 0.7686(7) 0.028(3) Uani 1 1 d . . . C27 C 0.4459(8) 0.6163(4) 0.6715(8) 0.034(3) Uani 1 1 d . . . H27 H 0.3858 0.6094 0.6269 0.041 Uiso 1 1 calc R . . C28 C 0.5257(10) 0.6178(5) 0.6425(9) 0.047(4) Uani 1 1 d . . . H28 H 0.5210 0.6124 0.5768 0.057 Uiso 1 1 calc R . . C29 C 0.6170(8) 0.6273(4) 0.7071(8) 0.042(3) Uani 1 1 d U . . H29 H 0.6729 0.6285 0.6853 0.050 Uiso 1 1 calc R . . C30 C 0.6226(8) 0.6345(4) 0.8004(8) 0.035(3) Uani 1 1 d . . . H30 H 0.6838 0.6396 0.8448 0.042 Uiso 1 1 calc R . . C31 C 0.5398(8) 0.6348(4) 0.8338(8) 0.031(3) Uani 1 1 d . . . C32 C 0.5458(7) 0.6449(4) 0.9301(8) 0.027(3) Uani 1 1 d . . . H32 H 0.6081 0.6485 0.9738 0.033 Uiso 1 1 calc R . . C33 C 0.4663(7) 0.6502(3) 0.9660(7) 0.022(2) Uani 1 1 d . . . C34 C 0.3781(7) 0.6415(3) 0.8952(7) 0.018(2) Uani 1 1 d . . . C35 C -0.1171(7) 0.6255(4) 0.5632(8) 0.038(3) Uani 1 1 d . . . C36 C -0.1515(8) 0.5994(4) 0.6270(9) 0.038(3) Uani 1 1 d . . . H36 H -0.1194 0.6000 0.6939 0.046 Uiso 1 1 calc R . . C37 C -0.2316(8) 0.5730(4) 0.5928(10) 0.043(3) Uani 1 1 d . . . H37 H -0.2517 0.5552 0.6372 0.052 Uiso 1 1 calc R . . C38 C -0.2814(9) 0.5715(5) 0.5004(10) 0.046(3) Uani 1 1 d . . . H38 H -0.3378 0.5541 0.4800 0.055 Uiso 1 1 calc R . . C39 C -0.2503(8) 0.5953(4) 0.4345(9) 0.042(3) Uani 1 1 d . . . H39 H -0.2841 0.5934 0.3682 0.051 Uiso 1 1 calc R . . C40 C -0.1700(9) 0.6223(4) 0.4639(8) 0.039(3) Uani 1 1 d . . . H40 H -0.1501 0.6388 0.4174 0.046 Uiso 1 1 calc R . . C41 C -0.0418(7) 0.7078(4) 0.6764(7) 0.026(2) Uani 1 1 d . . . C42 C 0.0149(8) 0.7433(3) 0.7020(8) 0.032(3) Uani 1 1 d . . . H42 H 0.0744 0.7446 0.6868 0.038 Uiso 1 1 calc R . . C43 C -0.0125(9) 0.7780(4) 0.7505(8) 0.038(3) Uani 1 1 d . . . H43 H 0.0289 0.8024 0.7698 0.046 Uiso 1 1 calc R . . C44 C -0.0996(8) 0.7768(4) 0.7703(9) 0.045(3) Uani 1 1 d . . . H44 H -0.1184 0.8009 0.8020 0.054 Uiso 1 1 calc R . . C45 C -0.1607(9) 0.7415(4) 0.7453(8) 0.039(3) Uani 1 1 d . . . H45 H -0.2199 0.7404 0.7610 0.046 Uiso 1 1 calc R . . C46 C -0.1311(9) 0.7066(4) 0.6946(8) 0.038(3) Uani 1 1 d . . . H46 H -0.1727 0.6825 0.6732 0.046 Uiso 1 1 calc R . . C47 C 0.0219(7) 0.6855(3) 0.4991(9) 0.029(3) Uani 1 1 d U . . C48 C -0.0152(8) 0.7256(4) 0.4626(8) 0.039(3) Uani 1 1 d . . . H48 H -0.0527 0.7419 0.4945 0.046 Uiso 1 1 calc R . . C49 C 0.0020(8) 0.7421(4) 0.3800(8) 0.038(3) Uani 1 1 d . . . H49 H -0.0260 0.7693 0.3558 0.045 Uiso 1 1 calc R . . C50 C 0.0581(8) 0.7208(4) 0.3309(8) 0.037(3) Uani 1 1 d . . . H50 H 0.0703 0.7331 0.2754 0.045 Uiso 1 1 calc R . . C51 C 0.0961(9) 0.6801(4) 0.3672(9) 0.045(3) Uani 1 1 d . . . H51 H 0.1335 0.6639 0.3349 0.054 Uiso 1 1 calc R . . C52 C 0.0791(8) 0.6632(4) 0.4520(8) 0.033(3) Uani 1 1 d . . . H52 H 0.1071 0.6361 0.4770 0.040 Uiso 1 1 calc R . . C53 C 0.4922(7) 0.6137(4) 1.1656(7) 0.027(2) Uani 1 1 d . . . C54 C 0.5178(9) 0.5739(4) 1.1368(9) 0.045(3) Uani 1 1 d . . . H54 H 0.5260 0.5722 1.0742 0.054 Uiso 1 1 calc R . . C55 C 0.5322(10) 0.5373(4) 1.1897(10) 0.054(4) Uani 1 1 d . . . H55 H 0.5542 0.5116 1.1662 0.065 Uiso 1 1 calc R . . C56 C 0.5144(8) 0.5374(4) 1.2802(9) 0.039(3) Uani 1 1 d . . . H56 H 0.5192 0.5113 1.3167 0.047 Uiso 1 1 calc R . . C57 C 0.4890(9) 0.5774(5) 1.3154(9) 0.046(3) Uani 1 1 d . . . H57 H 0.4798 0.5792 1.3776 0.056 Uiso 1 1 calc R . . C58 C 0.4779(9) 0.6139(4) 1.2566(8) 0.041(3) Uani 1 1 d . . . H58 H 0.4595 0.6406 1.2798 0.049 Uiso 1 1 calc R . . C59 C 0.6027(7) 0.6943(3) 1.1305(7) 0.022(2) Uani 1 1 d . . . C60 C 0.6664(7) 0.6847(4) 1.2260(8) 0.034(3) Uani 1 1 d . . . H60 H 0.6488 0.6649 1.2685 0.041 Uiso 1 1 calc R . . C61 C 0.7571(8) 0.7071(4) 1.2521(9) 0.051(4) Uani 1 1 d . . . H61 H 0.8029 0.6996 1.3111 0.061 Uiso 1 1 calc R . . C62 C 0.7797(8) 0.7371(4) 1.1988(8) 0.036(3) Uani 1 1 d . . . H62 H 0.8395 0.7520 1.2204 0.043 Uiso 1 1 calc R . . C63 C 0.7165(7) 0.7473(4) 1.1109(8) 0.035(3) Uani 1 1 d . . . H63 H 0.7326 0.7699 1.0734 0.042 Uiso 1 1 calc R . . C64 C 0.6299(7) 0.7253(4) 1.0757(7) 0.027(3) Uani 1 1 d . . . H64 H 0.5893 0.7318 1.0133 0.033 Uiso 1 1 calc R . . C65 C 0.3934(7) 0.7017(4) 1.1217(7) 0.024(2) Uani 1 1 d . . . C66 C 0.3135(7) 0.6858(4) 1.1484(7) 0.027(2) Uani 1 1 d . . . H66 H 0.3003 0.6554 1.1443 0.032 Uiso 1 1 calc R . . C67 C 0.2531(8) 0.7136(4) 1.1808(8) 0.037(3) Uani 1 1 d . . . H67 H 0.2011 0.7022 1.2010 0.044 Uiso 1 1 calc R . . C68 C 0.2707(7) 0.7592(4) 1.1829(7) 0.033(3) Uani 1 1 d . . . H68 H 0.2296 0.7788 1.2035 0.039 Uiso 1 1 calc R . . C69 C 0.3469(7) 0.7746(4) 1.1553(8) 0.033(3) Uani 1 1 d . . . H69 H 0.3592 0.8050 1.1576 0.040 Uiso 1 1 calc R . . C70 C 0.4069(7) 0.7468(3) 1.1238(7) 0.027(2) Uani 1 1 d . . . H70 H 0.4583 0.7587 1.1032 0.032 Uiso 1 1 calc R . . C71 C 0.4333(6) 0.8195(4) 0.6602(7) 0.023(2) Uani 1 1 d . . . C72 C 0.4270(8) 0.8596(4) 0.6110(7) 0.028(3) Uani 1 1 d . . . C73 C 0.4572(8) 0.8641(4) 0.5291(7) 0.028(3) Uani 1 1 d . . . C74 C 0.4893(8) 0.8266(4) 0.4939(8) 0.034(3) Uani 1 1 d . . . H74 H 0.5094 0.8290 0.4371 0.041 Uiso 1 1 calc R . . C75 C 0.4937(7) 0.7857(4) 0.5373(7) 0.024(2) Uani 1 1 d . . . C76 C 0.4642(7) 0.7835(3) 0.6202(7) 0.021(2) Uani 1 1 d . . . C77 C 0.4558(9) 0.9091(4) 0.4779(8) 0.036(3) Uani 1 1 d . . . C78 C 0.3551(8) 0.9279(4) 0.4448(8) 0.037(3) Uani 1 1 d . . . H78A H 0.3118 0.9067 0.4036 0.055 Uiso 1 1 calc R . . H78B H 0.3559 0.9548 0.4086 0.055 Uiso 1 1 calc R . . H78C H 0.3325 0.9343 0.5010 0.055 Uiso 1 1 calc R . . C79 C 0.5223(9) 0.9408(4) 0.5486(8) 0.038(3) Uani 1 1 d . . . H79A H 0.5210 0.9694 0.5177 0.057 Uiso 1 1 calc R . . H79B H 0.5882 0.9295 0.5669 0.057 Uiso 1 1 calc R . . H79C H 0.5001 0.9439 0.6061 0.057 Uiso 1 1 calc R . . C80 C 0.4995(9) 0.9055(4) 0.3914(8) 0.040(3) Uani 1 1 d . . . H80A H 0.4562 0.8885 0.3398 0.060 Uiso 1 1 calc R . . H80B H 0.5622 0.8910 0.4125 0.060 Uiso 1 1 calc R . . H80C H 0.5076 0.9348 0.3678 0.060 Uiso 1 1 calc R . . C81 C 0.5276(8) 0.7445(4) 0.4907(8) 0.032(3) Uani 1 1 d . . . C82 C 0.5522(10) 0.7568(5) 0.3968(8) 0.049(3) Uani 1 1 d . . . H82A H 0.5735 0.7307 0.3696 0.073 Uiso 1 1 calc R . . H82B H 0.6036 0.7786 0.4110 0.073 Uiso 1 1 calc R . . H82C H 0.4949 0.7688 0.3505 0.073 Uiso 1 1 calc R . . C83 C 0.6190(9) 0.7254(4) 0.5630(9) 0.040(3) Uani 1 1 d . . . H83A H 0.6407 0.6997 0.5347 0.061 Uiso 1 1 calc R . . H83B H 0.6041 0.7170 0.6224 0.061 Uiso 1 1 calc R . . H83C H 0.6700 0.7475 0.5775 0.061 Uiso 1 1 calc R . . C84 C 0.4455(9) 0.7097(4) 0.4640(8) 0.038(3) Uani 1 1 d . . . H84A H 0.3982 0.7180 0.4037 0.057 Uiso 1 1 calc R . . H84B H 0.4140 0.7080 0.5154 0.057 Uiso 1 1 calc R . . H84C H 0.4728 0.6812 0.4562 0.057 Uiso 1 1 calc R . . C85 C 0.2072(7) 0.9350(4) 0.7150(7) 0.023(2) Uani 1 1 d . . . C86 C 0.1342(7) 0.9413(4) 0.6287(7) 0.025(2) Uani 1 1 d . . . C87 C 0.0911(8) 0.9832(4) 0.6193(8) 0.035(3) Uani 1 1 d . . . H87 H 0.0404 0.9895 0.5630 0.042 Uiso 1 1 calc R . . C88 C 0.1208(8) 1.0163(4) 0.6908(8) 0.031(3) Uani 1 1 d . . . C89 C 0.0784(9) 1.0584(4) 0.6776(8) 0.039(3) Uani 1 1 d . . . H89 H 0.0263 1.0643 0.6224 0.047 Uiso 1 1 calc R . . C90 C 0.1113(9) 1.0899(4) 0.7423(8) 0.038(3) Uani 1 1 d . . . H90 H 0.0828 1.1181 0.7316 0.045 Uiso 1 1 calc R . . C91 C 0.1882(9) 1.0821(4) 0.8269(8) 0.037(3) Uani 1 1 d . . . H91 H 0.2121 1.1046 0.8724 0.044 Uiso 1 1 calc R . . C92 C 0.2268(8) 1.0407(4) 0.8408(8) 0.036(3) Uani 1 1 d . . . H92 H 0.2779 1.0353 0.8973 0.043 Uiso 1 1 calc R . . C93 C 0.1955(7) 1.0063(3) 0.7768(7) 0.023(2) Uani 1 1 d . . . C94 C 0.2343(7) 0.9638(4) 0.7906(8) 0.028(3) Uani 1 1 d . . . C95 C 0.2990(7) 0.9508(4) 0.8850(8) 0.025(2) Uani 1 1 d . . . C96 C 0.2704(8) 0.9542(4) 0.9701(8) 0.030(3) Uani 1 1 d . . . C97 C 0.1732(8) 0.9647(4) 0.9690(9) 0.040(3) Uani 1 1 d . . . H97 H 0.1263 0.9704 0.9096 0.048 Uiso 1 1 calc R . . C98 C 0.1479(9) 0.9664(5) 1.0539(9) 0.046(3) Uani 1 1 d . . . H98 H 0.0835 0.9729 1.0525 0.055 Uiso 1 1 calc R . . C99 C 0.2165(9) 0.9585(5) 1.1421(9) 0.056(4) Uani 1 1 d . . . H99 H 0.1989 0.9613 1.2002 0.067 Uiso 1 1 calc R . . C100 C 0.3097(9) 0.9468(4) 1.1456(8) 0.041(3) Uani 1 1 d . . . H100 H 0.3550 0.9405 1.2056 0.049 Uiso 1 1 calc R . . C101 C 0.3373(7) 0.9442(4) 1.0596(8) 0.031(3) Uani 1 1 d . . . C102 C 0.4320(7) 0.9320(4) 1.0608(8) 0.027(2) Uani 1 1 d . . . H102 H 0.4782 0.9281 1.1215 0.032 Uiso 1 1 calc R . . C103 C 0.4601(7) 0.9257(3) 0.9814(7) 0.022(2) Uani 1 1 d . . . C104 C 0.3884(7) 0.9336(3) 0.8913(7) 0.022(2) Uani 1 1 d . . . C105 C -0.0383(9) 0.8825(4) 0.5491(8) 0.039(3) Uani 1 1 d . . . C106 C -0.0719(8) 0.8393(4) 0.5326(8) 0.034(3) Uani 1 1 d . . . H106 H -0.0299 0.8182 0.5185 0.040 Uiso 1 1 calc R . . C107 C -0.1605(7) 0.8258(4) 0.5354(7) 0.034(3) Uani 1 1 d . . . H107 H -0.1783 0.7960 0.5244 0.040 Uiso 1 1 calc R . . C108 C -0.2243(9) 0.8554(4) 0.5544(8) 0.041(3) Uani 1 1 d . . . H108 H -0.2862 0.8464 0.5571 0.049 Uiso 1 1 calc R . . C109 C -0.1953(9) 0.8994(5) 0.5697(10) 0.049(3) Uani 1 1 d . . . H109 H -0.2381 0.9206 0.5822 0.059 Uiso 1 1 calc R . . C110 C -0.1057(10) 0.9115(4) 0.5666(9) 0.046(3) Uani 1 1 d . . . H110 H -0.0882 0.9414 0.5769 0.055 Uiso 1 1 calc R . . C111 C 0.0538(7) 0.9301(4) 0.4156(8) 0.032(3) Uani 1 1 d . . . C112 C -0.0203(8) 0.9132(4) 0.3365(8) 0.037(3) Uani 1 1 d . . . H112 H -0.0522 0.8869 0.3441 0.045 Uiso 1 1 calc R . . C113 C -0.0458(8) 0.9344(4) 0.2501(9) 0.038(3) Uani 1 1 d . . . H113 H -0.0931 0.9218 0.1977 0.046 Uiso 1 1 calc R . . C114 C -0.0047(9) 0.9737(4) 0.2368(9) 0.040(3) Uani 1 1 d . . . H114 H -0.0284 0.9897 0.1788 0.048 Uiso 1 1 calc R . . C115 C 0.0717(8) 0.9893(4) 0.3101(8) 0.034(3) Uani 1 1 d . . . H115 H 0.1060 1.0145 0.3005 0.041 Uiso 1 1 calc R . . C116 C 0.0981(8) 0.9672(4) 0.3994(8) 0.030(3) Uani 1 1 d . . . H116 H 0.1490 0.9787 0.4501 0.036 Uiso 1 1 calc R . . C117 C 0.1513(8) 0.8500(4) 0.5283(8) 0.034(3) Uani 1 1 d . . . C118 C 0.1631(7) 0.8173(4) 0.6023(8) 0.034(3) Uani 1 1 d . . . H118 H 0.1410 0.8227 0.6569 0.040 Uiso 1 1 calc R . . C119 C 0.2078(7) 0.7770(3) 0.5935(8) 0.031(3) Uani 1 1 d . . . H119 H 0.2152 0.7552 0.6416 0.037 Uiso 1 1 calc R . . C120 C 0.2408(8) 0.7698(4) 0.5131(8) 0.040(3) Uani 1 1 d . . . H120 H 0.2712 0.7429 0.5070 0.048 Uiso 1 1 calc R . . C121 C 0.2298(9) 0.8011(4) 0.4425(9) 0.039(3) Uani 1 1 d . . . H121 H 0.2542 0.7959 0.3893 0.046 Uiso 1 1 calc R . . C122 C 0.1837(7) 0.8399(4) 0.4485(9) 0.035(3) Uani 1 1 d . . . H122 H 0.1738 0.8604 0.3973 0.042 Uiso 1 1 calc R . . C123 C 0.6270(7) 0.8797(4) 1.1146(7) 0.023(2) Uani 1 1 d . . . C124 C 0.7044(7) 0.8927(4) 1.1915(7) 0.028(3) Uani 1 1 d . . . H124 H 0.7378 0.9187 1.1848 0.034 Uiso 1 1 calc R . . C125 C 0.7348(9) 0.8698(4) 1.2770(9) 0.038(3) Uani 1 1 d . . . H125 H 0.7892 0.8793 1.3266 0.045 Uiso 1 1 calc R . . C126 C 0.6861(7) 0.8336(4) 1.2892(8) 0.027(3) Uani 1 1 d . . . H126 H 0.7078 0.8172 1.3469 0.033 Uiso 1 1 calc R . . C127 C 0.6047(7) 0.8202(5) 1.2184(7) 0.030(2) Uani 1 1 d . . . H127 H 0.5693 0.7955 1.2288 0.036 Uiso 1 1 calc R . . C128 C 0.5763(8) 0.8424(4) 1.1345(8) 0.035(3) Uani 1 1 d . . . H128 H 0.5203 0.8329 1.0868 0.042 Uiso 1 1 calc R . . C129 C 0.6149(7) 0.8738(4) 0.9021(6) 0.022(2) Uani 1 1 d . . . C130 C 0.6226(7) 0.8279(3) 0.9093(7) 0.025(2) Uani 1 1 d . . . H130 H 0.6084 0.8139 0.9622 0.030 Uiso 1 1 calc R . . C131 C 0.6493(7) 0.8028(4) 0.8440(7) 0.024(2) Uani 1 1 d . . . H131 H 0.6533 0.7720 0.8512 0.029 Uiso 1 1 calc R . . C132 C 0.6706(7) 0.8229(4) 0.7664(7) 0.036(3) Uani 1 1 d . . . H132 H 0.6903 0.8057 0.7209 0.044 Uiso 1 1 calc R . . C133 C 0.6634(8) 0.8672(4) 0.7548(8) 0.032(3) Uani 1 1 d . . . H133 H 0.6780 0.8805 0.7014 0.039 Uiso 1 1 calc R . . C134 C 0.6346(7) 0.8931(4) 0.8221(7) 0.025(2) Uani 1 1 d . . . H134 H 0.6284 0.9238 0.8131 0.030 Uiso 1 1 calc R . . C135 C 0.6639(7) 0.9588(3) 1.0054(7) 0.023(2) Uani 1 1 d . . . C136 C 0.6328(9) 1.0003(4) 1.0258(9) 0.037(3) Uani 1 1 d . . . H136 H 0.5703 1.0036 1.0337 0.045 Uiso 1 1 calc R . . C137 C 0.6921(10) 1.0363(4) 1.0345(9) 0.045(3) Uani 1 1 d . . . H137 H 0.6688 1.0640 1.0472 0.054 Uiso 1 1 calc R . . C138 C 0.7828(8) 1.0333(4) 1.0254(8) 0.036(3) Uani 1 1 d . . . H138 H 0.8227 1.0583 1.0327 0.043 Uiso 1 1 calc R . . C139 C 0.8154(8) 0.9939(4) 1.0058(8) 0.034(3) Uani 1 1 d . . . H139 H 0.8780 0.9918 0.9978 0.041 Uiso 1 1 calc R . . C140 C 0.7591(7) 0.9564(4) 0.9970(7) 0.025(2) Uani 1 1 d . . . H140 H 0.7846 0.9291 0.9853 0.030 Uiso 1 1 calc R . . C141 C 0.7270(12) 0.0763(8) 0.5654(13) 0.114(8) Uani 1 1 d . . . H14D H 0.7686 0.0781 0.5228 0.171 Uiso 1 1 calc R . . H14E H 0.6962 0.1046 0.5672 0.171 Uiso 1 1 calc R . . H14F H 0.6775 0.0541 0.5411 0.171 Uiso 1 1 calc R . . C142 C 0.7899(13) 0.0634(6) 0.6711(11) 0.080(5) Uani 1 1 d . . . H14G H 0.8474 0.0825 0.6879 0.097 Uiso 1 1 calc R . . H14H H 0.7519 0.0707 0.7160 0.097 Uiso 1 1 calc R . . C143 C 0.8229(10) 0.0185(5) 0.6901(9) 0.049(4) Uani 1 1 d . . . H14I H 0.7657 -0.0005 0.6797 0.059 Uiso 1 1 calc R . . H14J H 0.8565 0.0102 0.6421 0.059 Uiso 1 1 calc R . . C144 C 0.8844(14) 0.0099(6) 0.7821(11) 0.080(6) Uani 1 1 d . . . H14K H 0.8534 0.0202 0.8307 0.096 Uiso 1 1 calc R . . H14L H 0.9445 0.0267 0.7908 0.096 Uiso 1 1 calc R . . C145 C 0.9094(12) -0.0370(6) 0.8003(12) 0.078(5) Uani 1 1 d . . . H14M H 0.8519 -0.0548 0.7738 0.117 Uiso 1 1 calc R . . H14N H 0.9338 -0.0420 0.8697 0.117 Uiso 1 1 calc R . . H14O H 0.9589 -0.0449 0.7693 0.117 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 Pd1 0.0202(4) 0.0198(4) 0.0186(4) -0.0019(4) 0.0044(3) -0.0004(3) Pd2 0.0186(4) 0.0195(4) 0.0184(4) 0.0002(4) 0.0036(3) 0.0007(3) P1 0.0215(13) 0.0217(16) 0.0188(13) 0.0013(11) 0.0050(10) 0.0039(11) P2 0.0200(13) 0.0182(15) 0.0207(13) -0.0008(11) 0.0031(10) 0.0023(11) Si1 0.0262(15) 0.0268(18) 0.0226(15) -0.0038(14) 0.0028(12) 0.0066(13) Si2 0.0212(14) 0.0224(17) 0.0179(14) 0.0022(12) 0.0023(11) -0.0015(12) Si3 0.0253(16) 0.035(2) 0.0338(18) -0.0070(15) 0.0063(13) 0.0054(14) Si4 0.0222(14) 0.0216(17) 0.0236(15) 0.0006(13) 0.0033(12) -0.0004(12) Cl1 0.0247(12) 0.0236(16) 0.0235(12) 0.0028(11) 0.0090(10) 0.0024(10) Cl2 0.0245(12) 0.0219(16) 0.0235(12) -0.0010(11) 0.0089(10) -0.0032(10) O1 0.019(3) 0.021(4) 0.024(4) -0.001(3) 0.000(3) 0.000(3) O2 0.040(4) 0.016(4) 0.016(4) 0.000(3) 0.000(3) 0.000(3) O3 0.020(4) 0.012(4) 0.028(4) 0.004(3) 0.004(3) -0.001(3) O4 0.039(5) 0.021(4) 0.037(5) -0.002(3) 0.021(4) -0.008(3) O5 0.033(4) 0.020(4) 0.013(3) -0.006(3) 0.011(3) -0.002(3) O6 0.020(4) 0.022(4) 0.028(4) 0.004(3) 0.004(3) 0.010(3) O7 0.019(4) 0.020(4) 0.026(4) 0.001(3) 0.004(3) -0.002(3) O8 0.035(4) 0.023(4) 0.024(4) -0.003(3) 0.013(3) 0.000(3) C1 0.012(4) 0.026(6) 0.017(4) 0.003(5) 0.000(3) -0.005(5) C2 0.017(5) 0.012(5) 0.014(5) -0.004(4) 0.001(4) 0.007(4) C3 0.015(5) 0.028(7) 0.035(6) 0.004(5) 0.010(4) 0.008(4) C4 0.019(5) 0.022(6) 0.051(7) 0.006(6) 0.008(4) 0.007(5) C5 0.034(6) 0.024(6) 0.042(7) 0.000(5) 0.024(5) 0.008(5) C6 0.024(5) 0.019(6) 0.018(5) -0.008(4) 0.004(4) -0.012(4) C7 0.037(6) 0.025(7) 0.041(7) 0.002(6) 0.022(5) 0.006(5) C8 0.044(7) 0.024(7) 0.054(8) -0.001(6) 0.017(6) -0.013(6) C9 0.060(9) 0.042(9) 0.098(12) -0.004(8) 0.059(9) -0.014(7) C10 0.030(6) 0.034(8) 0.068(9) 0.007(7) 0.022(6) 0.001(5) C11 0.047(7) 0.016(6) 0.056(8) 0.004(5) 0.036(6) 0.002(5) C12 0.044(8) 0.037(8) 0.073(10) -0.007(7) 0.035(7) 0.001(6) C13 0.038(7) 0.028(7) 0.055(8) -0.004(6) 0.010(6) 0.007(5) C14 0.053(8) 0.038(8) 0.103(11) 0.000(9) 0.059(8) 0.006(7) C15 0.032(6) 0.029(6) 0.007(5) -0.007(4) 0.007(4) -0.002(5) C16 0.021(5) 0.031(7) 0.021(5) -0.001(5) 0.001(4) 0.002(5) C17 0.027(6) 0.029(7) 0.029(6) 0.000(5) 0.000(5) 0.004(5) C18 0.026(6) 0.023(6) 0.026(6) 0.003(5) 0.001(4) 0.003(5) C19 0.028(6) 0.030(7) 0.053(8) -0.007(6) 0.007(6) -0.004(5) C20 0.039(7) 0.019(7) 0.040(7) -0.004(6) 0.002(5) 0.009(5) C21 0.025(5) 0.023(6) 0.030(6) -0.008(5) 0.005(5) 0.003(5) C22 0.026(5) 0.026(6) 0.020(5) -0.009(5) 0.002(4) -0.002(5) C23 0.026(5) 0.025(6) 0.020(5) -0.006(5) -0.001(4) -0.006(5) C24 0.020(5) 0.019(6) 0.010(5) -0.004(4) 0.000(4) -0.002(4) C25 0.026(5) 0.019(6) 0.011(5) -0.007(4) 0.002(4) 0.001(4) C26 0.026(6) 0.044(8) 0.018(5) -0.007(5) 0.017(4) -0.003(5) C27 0.023(6) 0.048(8) 0.031(6) 0.002(6) 0.008(5) -0.009(5) C28 0.053(8) 0.053(10) 0.032(7) -0.013(7) 0.005(6) 0.004(7) C29 0.030(6) 0.070(9) 0.037(7) -0.016(7) 0.031(5) -0.014(6) C30 0.031(6) 0.045(8) 0.030(6) -0.001(6) 0.009(5) 0.000(5) C31 0.029(6) 0.033(7) 0.035(6) -0.019(5) 0.014(5) -0.007(5) C32 0.017(5) 0.027(7) 0.039(7) -0.002(5) 0.009(5) 0.005(4) C33 0.032(6) 0.019(6) 0.017(5) -0.005(4) 0.009(4) 0.002(4) C34 0.023(5) 0.015(5) 0.019(5) 0.005(4) 0.013(4) 0.002(4) C35 0.018(5) 0.067(9) 0.025(6) -0.014(6) -0.002(4) 0.004(6) C36 0.035(7) 0.045(8) 0.036(7) -0.002(6) 0.013(5) -0.001(6) C37 0.026(6) 0.041(8) 0.062(9) 0.002(7) 0.012(6) 0.005(6) C38 0.037(7) 0.051(9) 0.055(9) 0.016(7) 0.022(6) 0.003(6) C39 0.027(6) 0.047(8) 0.049(8) 0.007(7) 0.004(5) -0.009(6) C40 0.048(7) 0.036(8) 0.029(6) -0.002(6) 0.008(5) -0.017(6) C41 0.028(6) 0.025(6) 0.025(6) -0.009(5) 0.010(4) 0.005(5) C42 0.046(7) 0.021(7) 0.032(6) 0.000(5) 0.017(5) 0.008(5) C43 0.052(8) 0.031(7) 0.032(7) -0.004(5) 0.012(6) 0.009(6) C44 0.031(6) 0.050(9) 0.045(8) -0.016(6) -0.001(6) -0.003(6) C45 0.045(7) 0.045(8) 0.030(6) -0.003(6) 0.018(5) 0.003(6) C46 0.051(8) 0.029(7) 0.037(7) -0.008(6) 0.015(6) -0.006(6) C47 0.014(5) 0.009(5) 0.059(8) -0.012(5) 0.002(5) 0.005(4) C48 0.036(7) 0.045(8) 0.031(6) -0.001(6) 0.004(5) -0.001(6) C49 0.040(7) 0.031(8) 0.039(7) -0.012(6) 0.007(6) 0.006(5) C50 0.020(6) 0.049(8) 0.039(7) 0.009(6) 0.001(5) -0.009(5) C51 0.042(7) 0.050(9) 0.049(8) 0.000(7) 0.019(6) 0.005(6) C52 0.045(7) 0.023(6) 0.037(7) 0.006(5) 0.022(6) 0.002(5) C53 0.027(6) 0.024(6) 0.024(6) -0.002(5) 0.000(4) 0.004(5) C54 0.058(9) 0.035(8) 0.039(7) 0.021(6) 0.012(6) 0.007(7) C55 0.064(9) 0.032(8) 0.051(9) -0.004(7) -0.007(7) 0.011(7) C56 0.038(7) 0.039(8) 0.037(7) 0.019(6) 0.004(5) -0.010(6) C57 0.052(8) 0.054(10) 0.033(7) 0.019(7) 0.013(6) 0.009(7) C58 0.052(8) 0.040(8) 0.032(7) 0.010(6) 0.012(6) 0.008(6) C59 0.021(5) 0.021(6) 0.021(5) -0.005(4) 0.003(4) 0.005(4) C60 0.020(5) 0.039(7) 0.036(7) -0.001(6) -0.005(5) -0.005(5) C61 0.032(7) 0.049(9) 0.051(8) 0.009(7) -0.023(6) -0.019(6) C62 0.022(6) 0.043(8) 0.033(6) 0.006(6) -0.007(5) -0.008(5) C63 0.021(5) 0.043(9) 0.040(7) 0.014(6) 0.006(5) -0.005(5) C64 0.012(5) 0.047(7) 0.019(5) 0.005(5) -0.001(4) -0.007(4) C65 0.023(5) 0.029(6) 0.016(5) -0.001(5) -0.002(4) -0.003(4) C66 0.030(6) 0.029(7) 0.018(5) 0.011(5) -0.001(4) 0.003(5) C67 0.026(6) 0.056(9) 0.028(6) 0.007(6) 0.008(5) 0.006(6) C68 0.031(6) 0.041(8) 0.024(5) 0.007(6) 0.006(4) 0.019(6) C69 0.024(6) 0.032(7) 0.039(7) -0.004(5) 0.002(5) 0.000(5) C70 0.029(5) 0.023(7) 0.020(5) -0.007(5) -0.009(4) 0.004(5) C71 0.023(5) 0.019(5) 0.026(5) 0.004(5) 0.005(4) -0.007(5) C72 0.031(6) 0.030(7) 0.020(6) -0.005(5) 0.002(5) 0.004(5) C73 0.030(6) 0.027(7) 0.023(6) -0.002(5) 0.000(5) 0.000(5) C74 0.040(6) 0.036(8) 0.025(5) 0.001(5) 0.005(5) 0.003(5) C75 0.020(5) 0.025(6) 0.029(6) -0.013(5) 0.012(4) -0.006(4) C76 0.020(5) 0.013(5) 0.024(5) 0.010(4) -0.002(4) 0.002(4) C77 0.066(8) 0.024(7) 0.023(6) 0.002(5) 0.018(6) 0.004(6) C78 0.041(7) 0.038(8) 0.038(7) 0.013(6) 0.022(6) 0.011(6) C79 0.061(8) 0.035(7) 0.025(6) -0.004(5) 0.024(6) -0.006(6) C80 0.059(8) 0.031(7) 0.041(7) 0.005(6) 0.032(6) -0.011(6) C81 0.045(7) 0.027(7) 0.034(6) -0.010(5) 0.026(5) 0.000(5) C82 0.083(9) 0.041(8) 0.037(7) -0.006(7) 0.041(7) -0.004(8) C83 0.051(8) 0.026(7) 0.055(8) -0.014(6) 0.032(7) 0.002(6) C84 0.051(8) 0.041(8) 0.028(6) -0.001(6) 0.021(6) -0.002(6) C85 0.019(5) 0.022(6) 0.029(6) -0.001(5) 0.007(4) 0.003(4) C86 0.032(6) 0.026(6) 0.017(5) 0.002(5) 0.007(4) -0.002(5) C87 0.035(6) 0.040(8) 0.025(6) -0.011(6) 0.003(5) 0.003(5) C88 0.033(6) 0.025(7) 0.039(7) -0.002(5) 0.018(5) 0.005(5) C89 0.052(8) 0.025(7) 0.032(7) 0.009(6) 0.000(6) 0.007(6) C90 0.060(8) 0.033(8) 0.021(6) 0.000(5) 0.014(6) 0.018(6) C91 0.054(8) 0.027(7) 0.023(6) -0.007(5) 0.001(5) 0.023(6) C92 0.031(6) 0.052(9) 0.021(6) -0.007(6) 0.000(5) 0.007(6) C93 0.023(5) 0.027(6) 0.019(5) 0.008(5) 0.009(4) 0.005(4) C94 0.021(5) 0.025(6) 0.035(6) 0.000(5) 0.005(5) -0.004(4) C95 0.015(5) 0.023(6) 0.036(6) -0.006(5) 0.005(5) 0.004(4) C96 0.026(6) 0.039(7) 0.032(6) 0.008(5) 0.021(5) 0.004(5) C97 0.031(7) 0.041(8) 0.045(8) -0.003(6) 0.007(6) 0.015(6) C98 0.032(7) 0.062(10) 0.047(8) -0.001(7) 0.019(6) 0.012(6) C99 0.043(8) 0.099(13) 0.029(7) 0.019(8) 0.018(6) 0.023(8) C100 0.038(7) 0.060(9) 0.027(6) 0.006(6) 0.015(5) 0.013(6) C101 0.025(6) 0.032(7) 0.035(6) 0.007(5) 0.006(5) 0.010(5) C102 0.027(6) 0.025(6) 0.024(6) 0.010(5) 0.002(4) 0.004(5) C103 0.013(5) 0.027(6) 0.024(5) 0.001(5) 0.003(4) 0.004(4) C104 0.036(6) 0.020(6) 0.014(5) -0.007(4) 0.012(4) -0.009(5) C105 0.044(7) 0.044(8) 0.016(6) 0.009(5) -0.016(5) 0.010(6) C106 0.035(6) 0.023(7) 0.038(7) 0.002(5) 0.002(5) 0.011(5) C107 0.024(5) 0.044(8) 0.033(6) 0.003(6) 0.009(4) 0.003(5) C108 0.055(8) 0.041(8) 0.024(6) 0.005(6) 0.007(6) -0.015(6) C109 0.047(8) 0.042(9) 0.065(9) -0.005(7) 0.027(7) 0.002(6) C110 0.059(9) 0.029(8) 0.056(8) -0.016(7) 0.026(7) -0.010(6) C111 0.023(5) 0.047(8) 0.023(6) -0.007(5) 0.004(4) 0.007(5) C112 0.039(7) 0.038(8) 0.029(6) -0.001(6) -0.001(5) -0.007(6) C113 0.026(6) 0.058(9) 0.036(7) 0.008(6) 0.016(5) 0.001(6) C114 0.044(7) 0.045(8) 0.035(7) -0.007(6) 0.017(6) 0.002(6) C115 0.036(6) 0.029(7) 0.040(7) -0.010(6) 0.012(5) 0.000(5) C116 0.031(6) 0.033(7) 0.023(6) -0.003(5) 0.002(5) -0.006(5) C117 0.039(7) 0.023(6) 0.036(7) -0.003(5) 0.004(5) -0.003(5) C118 0.027(5) 0.027(6) 0.045(6) -0.003(6) 0.007(5) 0.015(5) C119 0.035(6) 0.014(6) 0.041(7) -0.008(5) 0.005(5) 0.004(5) C120 0.028(6) 0.048(9) 0.040(7) -0.017(6) 0.003(5) 0.002(5) C121 0.046(7) 0.026(7) 0.043(7) -0.019(6) 0.011(6) -0.004(6) C122 0.009(5) 0.046(8) 0.051(7) -0.017(6) 0.012(5) -0.008(5) C123 0.018(5) 0.030(6) 0.015(5) -0.003(4) -0.002(4) 0.005(4) C124 0.019(5) 0.035(7) 0.024(5) -0.004(5) -0.008(4) -0.003(5) C125 0.046(7) 0.021(7) 0.041(7) -0.005(6) 0.004(6) 0.002(5) C126 0.031(6) 0.026(7) 0.024(6) -0.001(5) 0.007(5) 0.000(5) C127 0.036(5) 0.041(7) 0.014(5) 0.007(6) 0.009(4) -0.005(6) C128 0.023(6) 0.040(8) 0.031(6) -0.005(6) -0.007(5) -0.006(5) C129 0.021(5) 0.034(7) 0.004(4) 0.002(4) -0.005(4) 0.000(4) C130 0.026(5) 0.025(7) 0.022(5) 0.003(5) 0.004(4) 0.001(4) C131 0.021(5) 0.028(6) 0.021(5) 0.002(4) 0.003(4) 0.003(4) C132 0.026(5) 0.050(8) 0.033(6) -0.018(6) 0.007(4) 0.007(6) C133 0.033(6) 0.040(8) 0.026(6) -0.010(6) 0.011(5) -0.001(5) C134 0.020(5) 0.030(7) 0.025(5) -0.001(5) 0.004(4) -0.005(4) C135 0.031(6) 0.017(6) 0.024(5) 0.005(4) 0.013(4) -0.007(4) C136 0.038(7) 0.026(7) 0.044(7) -0.001(6) 0.005(6) 0.005(6) C137 0.066(9) 0.021(7) 0.060(9) -0.007(6) 0.036(7) -0.009(6) C138 0.042(7) 0.025(7) 0.039(7) -0.008(5) 0.008(6) -0.020(5) C139 0.036(6) 0.037(8) 0.029(6) -0.010(6) 0.009(5) -0.014(5) C140 0.025(5) 0.028(6) 0.020(5) 0.001(5) 0.002(4) 0.001(5) C141 0.048(10) 0.18(2) 0.084(13) -0.034(15) -0.024(9) 0.015(13) C142 0.112(15) 0.082(14) 0.046(10) -0.011(9) 0.020(9) -0.001(11) C143 0.064(9) 0.061(10) 0.035(7) 0.002(7) 0.033(7) -0.010(7) C144 0.114(15) 0.072(13) 0.057(10) 0.028(9) 0.031(10) 0.042(11) C145 0.068(11) 0.089(14) 0.069(11) 0.024(10) 0.007(9) -0.004(10) _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 C1 2.064(8) . ? Pd1 P1 2.142(3) . ? Pd1 Cl2 2.434(3) . ? Pd1 Cl1 2.450(2) . ? Pd2 C71 2.053(9) . ? Pd2 P2 2.140(3) . ? Pd2 Cl2 2.435(2) . ? Pd2 Cl1 2.436(3) . ? P1 O1 1.567(7) . ? P1 O2 1.600(7) . ? P1 O3 1.602(7) . ? P2 O6 1.579(7) . ? P2 O5 1.581(7) . ? P2 O7 1.604(7) . ? Si1 C35 1.870(12) . ? Si1 C47 1.887(13) . ? Si1 C16 1.898(11) . ? Si1 C41 1.900(10) . ? Si2 C33 1.860(10) . ? Si2 C53 1.864(11) . ? Si2 C65 1.867(11) . ? Si2 C59 1.872(10) . ? Si3 C117 1.865(12) . ? Si3 C111 1.869(12) . ? Si3 C105 1.875(14) . ? Si3 C86 1.883(11) . ? Si4 C123 1.851(10) . ? Si4 C129 1.860(10) . ? Si4 C135 1.864(10) . ? Si4 C103 1.906(10) . ? O1 C2 1.423(11) . ? O2 C15 1.417(12) . ? O3 C34 1.417(11) . ? O4 C6 1.376(11) . ? O4 H4 0.8400 . ? O5 C72 1.373(12) . ? O6 C85 1.411(12) . ? O7 C104 1.416(11) . ? O8 C76 1.392(11) . ? O8 H8 0.8400 . ? C1 C6 1.374(14) . ? C1 C2 1.399(14) . ? C2 C3 1.389(13) . ? C3 C4 1.404(15) . ? C3 C7 1.531(15) . ? C4 C5 1.387(16) . ? C4 H4A 0.9500 . ? C5 C6 1.434(14) . ? C5 C11 1.524(15) . ? C7 C9 1.528(15) . ? C7 C10 1.544(16) . ? C7 C8 1.568(16) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.534(17) . ? C11 C14 1.549(14) . ? C11 C13 1.580(16) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C24 1.373(14) . ? C15 C16 1.415(13) . ? C16 C17 1.395(15) . ? C17 C18 1.375(14) . ? C17 H17 0.9500 . ? C18 C19 1.410(15) . ? C18 C23 1.423(13) . ? C19 C20 1.361(16) . ? C19 H19 0.9500 . ? C20 C21 1.406(15) . ? C20 H20 0.9500 . ? C21 C22 1.353(14) . ? C21 H21 0.9500 . ? C22 C23 1.415(15) . ? C22 H22 0.9500 . ? C23 C24 1.464(14) . ? C24 C25 1.513(13) . ? C25 C34 1.346(13) . ? C25 C26 1.456(13) . ? C26 C31 1.396(14) . ? C26 C27 1.414(14) . ? C27 C28 1.339(16) . ? C27 H27 0.9500 . ? C28 C29 1.418(17) . ? C28 H28 0.9500 . ? C29 C30 1.350(15) . ? C29 H29 0.9500 . ? C30 C31 1.417(14) . ? C30 H30 0.9500 . ? C31 C32 1.409(15) . ? C32 C33 1.400(14) . ? C32 H32 0.9500 . ? C33 C34 1.420(14) . ? C35 C36 1.416(17) . ? C35 C40 1.430(15) . ? C36 C37 1.387(16) . ? C36 H36 0.9500 . ? C37 C38 1.331(17) . ? C37 H37 0.9500 . ? C38 C39 1.376(16) . ? C38 H38 0.9500 . ? C39 C40 1.393(15) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.350(15) . ? C41 C46 1.392(15) . ? C42 C43 1.395(15) . ? C42 H42 0.9500 . ? C43 C44 1.372(16) . ? C43 H43 0.9500 . ? C44 C45 1.380(16) . ? C44 H44 0.9500 . ? C45 C46 1.430(16) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.388(16) . ? C47 C52 1.394(14) . ? C48 C49 1.387(16) . ? C48 H48 0.9500 . ? C49 C50 1.387(16) . ? C49 H49 0.9500 . ? C50 C51 1.404(17) . ? C50 H50 0.9500 . ? C51 C52 1.419(16) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.373(16) . ? C53 C58 1.392(15) . ? C54 C55 1.342(17) . ? C54 H54 0.9500 . ? C55 C56 1.407(18) . ? C55 H55 0.9500 . ? C56 C57 1.418(18) . ? C56 H56 0.9500 . ? C57 C58 1.389(16) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.366(14) . ? C59 C60 1.460(14) . ? C60 C61 1.436(15) . ? C60 H60 0.9500 . ? C61 C62 1.302(16) . ? C61 H61 0.9500 . ? C62 C63 1.378(14) . ? C62 H62 0.9500 . ? C63 C64 1.389(14) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.397(14) . ? C65 C66 1.409(14) . ? C66 C67 1.395(15) . ? C66 H66 0.9500 . ? C67 C68 1.420(17) . ? C67 H67 0.9500 . ? C68 C69 1.363(15) . ? C68 H68 0.9500 . ? C69 C70 1.384(14) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C76 1.378(15) . ? C71 C72 1.412(15) . ? C72 C73 1.384(15) . ? C73 C74 1.390(15) . ? C73 C77 1.565(16) . ? C74 C75 1.398(15) . ? C74 H74 0.9500 . ? C75 C76 1.388(14) . ? C75 C81 1.577(14) . ? C77 C78 1.514(16) . ? C77 C79 1.539(16) . ? C77 C80 1.560(15) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.548(14) . ? C81 C83 1.551(16) . ? C81 C84 1.563(15) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C94 1.377(14) . ? C85 C86 1.406(14) . ? C86 C87 1.418(15) . ? C87 C88 1.426(15) . ? C87 H87 0.9500 . ? C88 C89 1.421(15) . ? C88 C93 1.434(15) . ? C89 C90 1.337(16) . ? C89 H89 0.9500 . ? C90 C91 1.425(15) . ? C90 H90 0.9500 . ? C91 C92 1.379(16) . ? C91 H91 0.9500 . ? C92 C93 1.394(15) . ? C92 H92 0.9500 . ? C93 C94 1.410(15) . ? C94 C95 1.478(15) . ? C95 C104 1.377(14) . ? C95 C96 1.412(14) . ? C96 C101 1.416(15) . ? C96 C97 1.441(14) . ? C97 C98 1.381(17) . ? C97 H97 0.9500 . ? C98 C99 1.400(17) . ? C98 H98 0.9500 . ? C99 C100 1.385(16) . ? C99 H99 0.9500 . ? C100 C101 1.416(15) . ? C100 H100 0.9500 . ? C101 C102 1.417(14) . ? C102 C103 1.340(14) . ? C102 H102 0.9500 . ? C103 C104 1.440(13) . ? C105 C110 1.399(17) . ? C105 C106 1.407(17) . ? C106 C107 1.362(15) . ? C106 H106 0.9500 . ? C107 C108 1.379(16) . ? C107 H107 0.9500 . ? C108 C109 1.413(18) . ? C108 H108 0.9500 . ? C109 C110 1.363(17) . ? C109 H109 0.9500 . ? C110 H110 0.9500 . ? C111 C116 1.357(16) . ? C111 C112 1.428(15) . ? C112 C113 1.367(15) . ? C112 H112 0.9500 . ? C113 C114 1.381(17) . ? C113 H113 0.9500 . ? C114 C115 1.384(15) . ? C114 H114 0.9500 . ? C115 C116 1.415(15) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C117 C122 1.401(15) . ? C117 C118 1.443(16) . ? C118 C119 1.418(14) . ? C118 H118 0.9500 . ? C119 C120 1.397(15) . ? C119 H119 0.9500 . ? C120 C121 1.379(17) . ? C120 H120 0.9500 . ? C121 C122 1.381(15) . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 C124 1.397(13) . ? C123 C128 1.432(15) . ? C124 C125 1.385(15) . ? C124 H124 0.9500 . ? C125 C126 1.354(15) . ? C125 H125 0.9500 . ? C126 C127 1.388(14) . ? C126 H126 0.9500 . ? C127 C128 1.354(15) . ? C127 H127 0.9500 . ? C128 H128 0.9500 . ? C129 C134 1.401(13) . ? C129 C130 1.416(14) . ? C130 C131 1.358(13) . ? C130 H130 0.9500 . ? C131 C132 1.392(15) . ? C131 H131 0.9500 . ? C132 C133 1.369(17) . ? C132 H132 0.9500 . ? C133 C134 1.411(14) . ? C133 H133 0.9500 . ? C134 H134 0.9500 . ? C135 C136 1.409(15) . ? C135 C140 1.422(14) . ? C136 C137 1.383(17) . ? C136 H136 0.9500 . ? C137 C138 1.363(16) . ? C137 H137 0.9500 . ? C138 C139 1.354(16) . ? C138 H138 0.9500 . ? C139 C140 1.396(15) . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C141 C142 1.60(2) . ? C141 H14D 0.9800 . ? C141 H14E 0.9800 . ? C141 H14F 0.9800 . ? C142 C143 1.46(2) . ? C142 H14G 0.9900 . ? C142 H14H 0.9900 . ? C143 C144 1.403(19) . ? C143 H14I 0.9900 . ? C143 H14J 0.9900 . ? C144 C145 1.49(2) . ? C144 H14K 0.9900 . ? C144 H14L 0.9900 . ? C145 H14M 0.9800 . ? C145 H14N 0.9800 . ? C145 H14O 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 Pd1 P1 79.3(3) . . ? C1 Pd1 Cl2 105.2(3) . . ? P1 Pd1 Cl2 175.46(10) . . ? C1 Pd1 Cl1 174.0(3) . . ? P1 Pd1 Cl1 94.73(10) . . ? Cl2 Pd1 Cl1 80.77(8) . . ? C71 Pd2 P2 79.6(3) . . ? C71 Pd2 Cl2 172.5(3) . . ? P2 Pd2 Cl2 93.01(10) . . ? C71 Pd2 Cl1 106.3(3) . . ? P2 Pd2 Cl1 173.56(10) . . ? Cl2 Pd2 Cl1 81.03(8) . . ? O1 P1 O2 109.1(4) . . ? O1 P1 O3 98.6(4) . . ? O2 P1 O3 104.8(4) . . ? O1 P1 Pd1 111.4(3) . . ? O2 P1 Pd1 110.9(3) . . ? O3 P1 Pd1 121.0(3) . . ? O6 P2 O5 110.2(4) . . ? O6 P2 O7 104.3(4) . . ? O5 P2 O7 98.9(4) . . ? O6 P2 Pd2 109.0(3) . . ? O5 P2 Pd2 111.0(3) . . ? O7 P2 Pd2 122.8(3) . . ? C35 Si1 C47 109.1(5) . . ? C35 Si1 C16 107.1(5) . . ? C47 Si1 C16 105.6(5) . . ? C35 Si1 C41 107.6(5) . . ? C47 Si1 C41 107.1(5) . . ? C16 Si1 C41 120.0(5) . . ? C33 Si2 C53 108.7(5) . . ? C33 Si2 C65 116.7(5) . . ? C53 Si2 C65 109.0(5) . . ? C33 Si2 C59 104.9(5) . . ? C53 Si2 C59 110.3(5) . . ? C65 Si2 C59 107.2(5) . . ? C117 Si3 C111 110.4(5) . . ? C117 Si3 C105 107.6(6) . . ? C111 Si3 C105 107.6(5) . . ? C117 Si3 C86 117.2(5) . . ? C111 Si3 C86 106.0(5) . . ? C105 Si3 C86 107.6(5) . . ? C123 Si4 C129 110.1(5) . . ? C123 Si4 C135 109.1(5) . . ? C129 Si4 C135 106.8(5) . . ? C123 Si4 C103 105.3(5) . . ? C129 Si4 C103 117.4(4) . . ? C135 Si4 C103 108.0(5) . . ? Pd2 Cl1 Pd1 87.72(8) . . ? Pd1 Cl2 Pd2 88.13(8) . . ? C2 O1 P1 113.3(6) . . ? C15 O2 P1 121.9(6) . . ? C34 O3 P1 116.8(6) . . ? C6 O4 H4 109.5 . . ? C72 O5 P2 113.1(7) . . ? C85 O6 P2 126.0(6) . . ? C104 O7 P2 115.6(6) . . ? C76 O8 H8 109.5 . . ? C6 C1 C2 116.4(8) . . ? C6 C1 Pd1 124.9(8) . . ? C2 C1 Pd1 118.6(8) . . ? C3 C2 C1 126.7(9) . . ? C3 C2 O1 116.3(9) . . ? C1 C2 O1 116.9(8) . . ? C2 C3 C4 112.2(10) . . ? C2 C3 C7 125.9(9) . . ? C4 C3 C7 121.9(9) . . ? C5 C4 C3 127.0(10) . . ? C5 C4 H4A 116.5 . . ? C3 C4 H4A 116.5 . . ? C4 C5 C6 115.0(10) . . ? C4 C5 C11 124.3(10) . . ? C6 C5 C11 120.6(10) . . ? C1 C6 O4 122.3(9) . . ? C1 C6 C5 122.5(9) . . ? O4 C6 C5 115.2(9) . . ? C9 C7 C3 112.3(9) . . ? C9 C7 C10 107.8(10) . . ? C3 C7 C10 111.1(9) . . ? C9 C7 C8 106.1(10) . . ? C3 C7 C8 109.4(9) . . ? C10 C7 C8 110.1(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 C12 110.5(10) . . ? C5 C11 C14 109.5(10) . . ? C12 C11 C14 108.2(10) . . ? C5 C11 C13 110.6(9) . . ? C12 C11 C13 112.7(10) . . ? C14 C11 C13 105.0(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C15 C16 126.3(10) . . ? C24 C15 O2 117.4(9) . . ? C16 C15 O2 115.9(9) . . ? C17 C16 C15 113.2(10) . . ? C17 C16 Si1 116.8(7) . . ? C15 C16 Si1 128.6(9) . . ? C18 C17 C16 125.8(10) . . ? C18 C17 H17 117.1 . . ? C16 C17 H17 117.1 . . ? C17 C18 C19 122.8(10) . . ? C17 C18 C23 118.9(10) . . ? C19 C18 C23 118.2(10) . . ? C20 C19 C18 121.6(11) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 120.1(11) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.1(10) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.5(10) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C18 118.5(10) . . ? C22 C23 C24 122.9(9) . . ? C18 C23 C24 118.5(9) . . ? C15 C24 C23 116.8(9) . . ? C15 C24 C25 123.1(9) . . ? C23 C24 C25 119.9(9) . . ? C34 C25 C26 119.1(9) . . ? C34 C25 C24 120.8(9) . . ? C26 C25 C24 120.1(8) . . ? C31 C26 C27 119.6(9) . . ? C31 C26 C25 116.6(9) . . ? C27 C26 C25 123.8(9) . . ? C28 C27 C26 120.0(11) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 121.8(11) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 118.4(10) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C29 C30 C31 121.8(10) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C26 C31 C32 120.3(9) . . ? C26 C31 C30 118.4(10) . . ? C32 C31 C30 121.3(10) . . ? C33 C32 C31 124.5(10) . . ? C33 C32 H32 117.8 . . ? C31 C32 H32 117.8 . . ? C32 C33 C34 112.2(9) . . ? C32 C33 Si2 119.9(8) . . ? C34 C33 Si2 127.8(7) . . ? C25 C34 O3 117.6(8) . . ? C25 C34 C33 126.5(9) . . ? O3 C34 C33 115.8(8) . . ? C36 C35 C40 115.6(11) . . ? C36 C35 Si1 122.0(8) . . ? C40 C35 Si1 122.4(10) . . ? C37 C36 C35 120.8(11) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C38 C37 C36 122.7(13) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C37 C38 C39 119.3(13) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C40 120.9(12) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 120.7(11) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? C42 C41 C46 119.7(10) . . ? C42 C41 Si1 121.9(8) . . ? C46 C41 Si1 118.2(8) . . ? C41 C42 C43 121.0(11) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 119.6(12) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 121.8(12) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C45 C46 117.3(11) . . ? C44 C45 H45 121.4 . . ? C46 C45 H45 121.4 . . ? C41 C46 C45 120.5(11) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C52 118.0(11) . . ? C48 C47 Si1 120.8(9) . . ? C52 C47 Si1 121.2(8) . . ? C49 C48 C47 120.6(12) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C50 C49 C48 123.0(12) . . ? C50 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? C49 C50 C51 116.9(11) . . ? C49 C50 H50 121.6 . . ? C51 C50 H50 121.6 . . ? C50 C51 C52 120.3(12) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C47 C52 C51 121.2(11) . . ? C47 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C54 C53 C58 114.7(11) . . ? C54 C53 Si2 123.8(9) . . ? C58 C53 Si2 121.3(9) . . ? C55 C54 C53 125.5(13) . . ? C55 C54 H54 117.2 . . ? C53 C54 H54 117.2 . . ? C54 C55 C56 119.4(13) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C55 C56 C57 118.2(11) . . ? C55 C56 H56 120.9 . . ? C57 C56 H56 120.9 . . ? C58 C57 C56 118.3(12) . . ? C58 C57 H57 120.9 . . ? C56 C57 H57 120.9 . . ? C57 C58 C53 123.7(12) . . ? C57 C58 H58 118.1 . . ? C53 C58 H58 118.1 . . ? C64 C59 C60 118.8(9) . . ? C64 C59 Si2 124.3(7) . . ? C60 C59 Si2 116.7(8) . . ? C61 C60 C59 116.1(11) . . ? C61 C60 H60 122.0 . . ? C59 C60 H60 122.0 . . ? C62 C61 C60 123.2(11) . . ? C62 C61 H61 118.4 . . ? C60 C61 H61 118.4 . . ? C61 C62 C63 119.7(11) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C62 C63 C64 121.7(11) . . ? C62 C63 H63 119.2 . . ? C64 C63 H63 119.2 . . ? C59 C64 C63 120.3(9) . . ? C59 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C70 C65 C66 117.3(10) . . ? C70 C65 Si2 120.1(8) . . ? C66 C65 Si2 122.5(8) . . ? C67 C66 C65 121.6(11) . . ? C67 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? C66 C67 C68 119.0(11) . . ? C66 C67 H67 120.5 . . ? C68 C67 H67 120.5 . . ? C69 C68 C67 119.3(11) . . ? C69 C68 H68 120.4 . . ? C67 C68 H68 120.4 . . ? C68 C69 C70 121.5(11) . . ? C68 C69 H69 119.3 . . ? C70 C69 H69 119.3 . . ? C69 C70 C65 121.3(11) . . ? C69 C70 H70 119.3 . . ? C65 C70 H70 119.3 . . ? C76 C71 C72 117.8(9) . . ? C76 C71 Pd2 124.8(8) . . ? C72 C71 Pd2 117.4(8) . . ? O5 C72 C73 119.2(10) . . ? O5 C72 C71 118.8(9) . . ? C73 C72 C71 122.0(10) . . ? C72 C73 C74 117.0(11) . . ? C72 C73 C77 122.0(10) . . ? C74 C73 C77 121.0(10) . . ? C73 C74 C75 123.6(10) . . ? C73 C74 H74 118.2 . . ? C75 C74 H74 118.2 . . ? C76 C75 C74 116.6(10) . . ? C76 C75 C81 122.8(10) . . ? C74 C75 C81 120.5(9) . . ? C71 C76 C75 122.9(9) . . ? C71 C76 O8 122.7(9) . . ? C75 C76 O8 114.4(9) . . ? C78 C77 C79 109.6(10) . . ? C78 C77 C80 110.3(10) . . ? C79 C77 C80 105.0(10) . . ? C78 C77 C73 111.6(10) . . ? C79 C77 C73 108.7(9) . . ? C80 C77 C73 111.5(9) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 C83 108.7(9) . . ? C82 C81 C84 107.3(9) . . ? C83 C81 C84 110.8(10) . . ? C82 C81 C75 110.9(10) . . ? C83 C81 C75 108.8(9) . . ? C84 C81 C75 110.2(8) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C94 C85 C86 126.3(10) . . ? C94 C85 O6 117.9(9) . . ? C86 C85 O6 115.7(9) . . ? C85 C86 C87 114.3(10) . . ? C85 C86 Si3 128.2(9) . . ? C87 C86 Si3 117.1(8) . . ? C86 C87 C88 122.6(10) . . ? C86 C87 H87 118.7 . . ? C88 C87 H87 118.7 . . ? C89 C88 C87 121.3(11) . . ? C89 C88 C93 120.1(10) . . ? C87 C88 C93 118.6(10) . . ? C90 C89 C88 120.6(11) . . ? C90 C89 H89 119.7 . . ? C88 C89 H89 119.7 . . ? C89 C90 C91 121.2(11) . . ? C89 C90 H90 119.4 . . ? C91 C90 H90 119.4 . . ? C92 C91 C90 117.9(11) . . ? C92 C91 H91 121.1 . . ? C90 C91 H91 121.1 . . ? C91 C92 C93 123.9(10) . . ? C91 C92 H92 118.0 . . ? C93 C92 H92 118.0 . . ? C92 C93 C94 124.3(10) . . ? C92 C93 C88 116.1(10) . . ? C94 C93 C88 119.6(10) . . ? C85 C94 C93 117.9(10) . . ? C85 C94 C95 121.8(10) . . ? C93 C94 C95 120.2(10) . . ? C104 C95 C96 118.3(9) . . ? C104 C95 C94 120.2(10) . . ? C96 C95 C94 121.5(9) . . ? C95 C96 C101 119.3(9) . . ? C95 C96 C97 122.4(10) . . ? C101 C96 C97 118.2(10) . . ? C98 C97 C96 120.3(11) . . ? C98 C97 H97 119.9 . . ? C96 C97 H97 119.9 . . ? C97 C98 C99 120.6(11) . . ? C97 C98 H98 119.7 . . ? C99 C98 H98 119.7 . . ? C100 C99 C98 120.7(11) . . ? C100 C99 H99 119.7 . . ? C98 C99 H99 119.7 . . ? C99 C100 C101 120.0(11) . . ? C99 C100 H100 120.0 . . ? C101 C100 H100 120.0 . . ? C100 C101 C96 120.2(10) . . ? C100 C101 C102 121.2(10) . . ? C96 C101 C102 118.6(10) . . ? C103 C102 C101 123.8(10) . . ? C103 C102 H102 118.1 . . ? C101 C102 H102 118.1 . . ? C102 C103 C104 115.9(9) . . ? C102 C103 Si4 117.7(8) . . ? C104 C103 Si4 126.4(7) . . ? C95 C104 O7 119.4(9) . . ? C95 C104 C103 123.3(9) . . ? O7 C104 C103 117.2(9) . . ? C110 C105 C106 113.8(12) . . ? C110 C105 Si3 123.4(10) . . ? C106 C105 Si3 122.3(10) . . ? C107 C106 C105 124.5(11) . . ? C107 C106 H106 117.8 . . ? C105 C106 H106 117.8 . . ? C106 C107 C108 119.8(12) . . ? C106 C107 H107 120.1 . . ? C108 C107 H107 120.1 . . ? C107 C108 C109 118.3(12) . . ? C107 C108 H108 120.8 . . ? C109 C108 H108 120.8 . . ? C110 C109 C108 119.9(13) . . ? C110 C109 H109 120.0 . . ? C108 C109 H109 120.0 . . ? C109 C110 C105 123.6(13) . . ? C109 C110 H110 118.2 . . ? C105 C110 H110 118.2 . . ? C116 C111 C112 116.8(11) . . ? C116 C111 Si3 125.8(8) . . ? C112 C111 Si3 117.4(9) . . ? C113 C112 C111 120.6(12) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C112 C113 C114 121.9(12) . . ? C112 C113 H113 119.1 . . ? C114 C113 H113 119.1 . . ? C113 C114 C115 118.5(12) . . ? C113 C114 H114 120.8 . . ? C115 C114 H114 120.8 . . ? C114 C115 C116 119.1(11) . . ? C114 C115 H115 120.4 . . ? C116 C115 H115 120.4 . . ? C111 C116 C115 122.8(10) . . ? C111 C116 H116 118.6 . . ? C115 C116 H116 118.6 . . ? C122 C117 C118 117.7(11) . . ? C122 C117 Si3 121.8(9) . . ? C118 C117 Si3 120.0(8) . . ? C119 C118 C117 120.0(10) . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C120 C119 C118 119.0(11) . . ? C120 C119 H119 120.5 . . ? C118 C119 H119 120.5 . . ? C121 C120 C119 121.0(11) . . ? C121 C120 H120 119.5 . . ? C119 C120 H120 119.5 . . ? C120 C121 C122 120.7(12) . . ? C120 C121 H121 119.7 . . ? C122 C121 H121 119.7 . . ? C121 C122 C117 121.5(12) . . ? C121 C122 H122 119.2 . . ? C117 C122 H122 119.2 . . ? C124 C123 C128 114.2(9) . . ? C124 C123 Si4 123.6(8) . . ? C128 C123 Si4 122.2(7) . . ? C125 C124 C123 123.3(11) . . ? C125 C124 H124 118.4 . . ? C123 C124 H124 118.4 . . ? C126 C125 C124 119.2(11) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C125 C126 C127 120.7(11) . . ? C125 C126 H126 119.6 . . ? C127 C126 H126 119.6 . . ? C128 C127 C126 119.6(12) . . ? C128 C127 H127 120.2 . . ? C126 C127 H127 120.2 . . ? C127 C128 C123 122.7(10) . . ? C127 C128 H128 118.7 . . ? C123 C128 H128 118.7 . . ? C134 C129 C130 116.8(9) . . ? C134 C129 Si4 120.2(8) . . ? C130 C129 Si4 122.8(7) . . ? C131 C130 C129 122.9(10) . . ? C131 C130 H130 118.5 . . ? C129 C130 H130 118.5 . . ? C130 C131 C132 119.1(11) . . ? C130 C131 H131 120.5 . . ? C132 C131 H131 120.5 . . ? C133 C132 C131 120.7(10) . . ? C133 C132 H132 119.6 . . ? C131 C132 H132 119.6 . . ? C132 C133 C134 120.1(11) . . ? C132 C133 H133 119.9 . . ? C134 C133 H133 119.9 . . ? C129 C134 C133 120.2(11) . . ? C129 C134 H134 119.9 . . ? C133 C134 H134 119.9 . . ? C136 C135 C140 116.2(10) . . ? C136 C135 Si4 123.3(8) . . ? C140 C135 Si4 120.4(8) . . ? C137 C136 C135 120.9(12) . . ? C137 C136 H136 119.6 . . ? C135 C136 H136 119.6 . . ? C138 C137 C136 121.8(12) . . ? C138 C137 H137 119.1 . . ? C136 C137 H137 119.1 . . ? C139 C138 C137 119.0(11) . . ? C139 C138 H138 120.5 . . ? C137 C138 H138 120.5 . . ? C138 C139 C140 121.6(11) . . ? C138 C139 H139 119.2 . . ? C140 C139 H139 119.2 . . ? C139 C140 C135 120.4(10) . . ? C139 C140 H140 119.8 . . ? C135 C140 H140 119.8 . . ? C142 C141 H14D 109.5 . . ? C142 C141 H14E 109.5 . . ? H14D C141 H14E 109.5 . . ? C142 C141 H14F 109.5 . . ? H14D C141 H14F 109.5 . . ? H14E C141 H14F 109.5 . . ? C143 C142 C141 118.9(14) . . ? C143 C142 H14G 107.6 . . ? C141 C142 H14G 107.6 . . ? C143 C142 H14H 107.6 . . ? C141 C142 H14H 107.6 . . ? H14G C142 H14H 107.0 . . ? C144 C143 C142 116.4(14) . . ? C144 C143 H14I 108.2 . . ? C142 C143 H14I 108.2 . . ? C144 C143 H14J 108.2 . . ? C142 C143 H14J 108.2 . . ? H14I C143 H14J 107.3 . . ? C143 C144 C145 114.1(16) . . ? C143 C144 H14K 108.7 . . ? C145 C144 H14K 108.7 . . ? C143 C144 H14L 108.7 . . ? C145 C144 H14L 108.7 . . ? H14K C144 H14L 107.6 . . ? C144 C145 H14M 109.5 . . ? C144 C145 H14N 109.5 . . ? H14M C145 H14N 109.5 . . ? C144 C145 H14O 109.5 . . ? H14M C145 H14O 109.5 . . ? H14N C145 H14O 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 C1 Pd1 P1 O1 -6.3(4) . . . . ? Cl2 Pd1 P1 O1 -179(85) . . . . ? Cl1 Pd1 P1 O1 173.2(3) . . . . ? C1 Pd1 P1 O2 115.4(4) . . . . ? Cl2 Pd1 P1 O2 -57.2(13) . . . . ? Cl1 Pd1 P1 O2 -65.1(3) . . . . ? C1 Pd1 P1 O3 -121.4(4) . . . . ? Cl2 Pd1 P1 O3 66.0(14) . . . . ? Cl1 Pd1 P1 O3 58.2(3) . . . . ? C71 Pd2 P2 O6 118.2(4) . . . . ? Cl2 Pd2 P2 O6 -60.7(3) . . . . ? Cl1 Pd2 P2 O6 -38.4(10) . . . . ? C71 Pd2 P2 O5 -3.3(4) . . . . ? Cl2 Pd2 P2 O5 177.9(3) . . . . ? Cl1 Pd2 P2 O5 -159.9(8) . . . . ? C71 Pd2 P2 O7 -119.6(4) . . . . ? Cl2 Pd2 P2 O7 61.6(3) . . . . ? Cl1 Pd2 P2 O7 83.8(10) . . . . ? C71 Pd2 Cl1 Pd1 -143.9(3) . . . . ? P2 Pd2 Cl1 Pd1 12.1(9) . . . . ? Cl2 Pd2 Cl1 Pd1 34.60(8) . . . . ? C1 Pd1 Cl1 Pd2 149(2) . . . . ? P1 Pd1 Cl1 Pd2 144.72(9) . . . . ? Cl2 Pd1 Cl1 Pd2 -34.65(8) . . . . ? C1 Pd1 Cl2 Pd2 -145.7(3) . . . . ? P1 Pd1 Cl2 Pd2 26.7(13) . . . . ? Cl1 Pd1 Cl2 Pd2 34.66(8) . . . . ? C71 Pd2 Cl2 Pd1 134(2) . . . . ? P2 Pd2 Cl2 Pd1 142.67(9) . . . . ? Cl1 Pd2 Cl2 Pd1 -34.86(8) . . . . ? O2 P1 O1 C2 -116.7(6) . . . . ? O3 P1 O1 C2 134.3(6) . . . . ? Pd1 P1 O1 C2 6.0(6) . . . . ? O1 P1 O2 C15 -74.8(8) . . . . ? O3 P1 O2 C15 30.0(8) . . . . ? Pd1 P1 O2 C15 162.2(7) . . . . ? O1 P1 O3 C34 171.7(7) . . . . ? O2 P1 O3 C34 59.2(7) . . . . ? Pd1 P1 O3 C34 -66.9(7) . . . . ? O6 P2 O5 C72 -117.7(7) . . . . ? O7 P2 O5 C72 133.4(7) . . . . ? Pd2 P2 O5 C72 3.1(7) . . . . ? O5 P2 O6 C85 -71.3(8) . . . . ? O7 P2 O6 C85 33.9(9) . . . . ? Pd2 P2 O6 C85 166.7(7) . . . . ? O6 P2 O7 C104 53.5(7) . . . . ? O5 P2 O7 C104 167.0(7) . . . . ? Pd2 P2 O7 C104 -70.9(7) . . . . ? P1 Pd1 C1 C6 -176.8(8) . . . . ? Cl2 Pd1 C1 C6 2.6(8) . . . . ? Cl1 Pd1 C1 C6 179(76) . . . . ? P1 Pd1 C1 C2 6.3(6) . . . . ? Cl2 Pd1 C1 C2 -174.3(6) . . . . ? Cl1 Pd1 C1 C2 2(3) . . . . ? C6 C1 C2 C3 -3.9(14) . . . . ? Pd1 C1 C2 C3 173.4(8) . . . . ? C6 C1 C2 O1 178.2(8) . . . . ? Pd1 C1 C2 O1 -4.6(10) . . . . ? P1 O1 C2 C3 -179.4(7) . . . . ? P1 O1 C2 C1 -1.2(10) . . . . ? C1 C2 C3 C4 3.0(14) . . . . ? O1 C2 C3 C4 -179.0(8) . . . . ? C1 C2 C3 C7 -174.6(10) . . . . ? O1 C2 C3 C7 3.4(14) . . . . ? C2 C3 C4 C5 -2.3(16) . . . . ? C7 C3 C4 C5 175.4(11) . . . . ? C3 C4 C5 C6 2.4(17) . . . . ? C3 C4 C5 C11 -178.1(11) . . . . ? C2 C1 C6 O4 -176.6(9) . . . . ? Pd1 C1 C6 O4 6.4(13) . . . . ? C2 C1 C6 C5 3.8(14) . . . . ? Pd1 C1 C6 C5 -173.2(8) . . . . ? C4 C5 C6 C1 -3.2(16) . . . . ? C11 C5 C6 C1 177.3(10) . . . . ? C4 C5 C6 O4 177.2(9) . . . . ? C11 C5 C6 O4 -2.3(15) . . . . ? C2 C3 C7 C9 -176.7(11) . . . . ? C4 C3 C7 C9 5.9(16) . . . . ? C2 C3 C7 C10 -55.9(14) . . . . ? C4 C3 C7 C10 126.7(11) . . . . ? C2 C3 C7 C8 65.7(14) . . . . ? C4 C3 C7 C8 -111.6(11) . . . . ? C4 C5 C11 C12 116.2(13) . . . . ? C6 C5 C11 C12 -64.4(14) . . . . ? C4 C5 C11 C14 -3.0(17) . . . . ? C6 C5 C11 C14 176.5(11) . . . . ? C4 C5 C11 C13 -118.3(12) . . . . ? C6 C5 C11 C13 61.2(14) . . . . ? P1 O2 C15 C24 -67.0(11) . . . . ? P1 O2 C15 C16 119.9(8) . . . . ? C24 C15 C16 C17 7.4(15) . . . . ? O2 C15 C16 C17 179.7(9) . . . . ? C24 C15 C16 Si1 -158.4(9) . . . . ? O2 C15 C16 Si1 13.9(14) . . . . ? C35 Si1 C16 C17 28.7(10) . . . . ? C47 Si1 C16 C17 -87.5(9) . . . . ? C41 Si1 C16 C17 151.6(8) . . . . ? C35 Si1 C16 C15 -165.9(9) . . . . ? C47 Si1 C16 C15 77.9(10) . . . . ? C41 Si1 C16 C15 -43.1(11) . . . . ? C15 C16 C17 C18 -1.3(16) . . . . ? Si1 C16 C17 C18 166.3(9) . . . . ? C16 C17 C18 C19 179.5(11) . . . . ? C16 C17 C18 C23 -2.9(17) . . . . ? C17 C18 C19 C20 179.0(12) . . . . ? C23 C18 C19 C20 1.4(18) . . . . ? C18 C19 C20 C21 1.0(19) . . . . ? C19 C20 C21 C22 -0.4(18) . . . . ? C20 C21 C22 C23 -2.6(17) . . . . ? C21 C22 C23 C18 4.9(16) . . . . ? C21 C22 C23 C24 -179.0(10) . . . . ? C17 C18 C23 C22 178.1(10) . . . . ? C19 C18 C23 C22 -4.1(16) . . . . ? C17 C18 C23 C24 1.8(15) . . . . ? C19 C18 C23 C24 179.5(10) . . . . ? C16 C15 C24 C23 -8.5(15) . . . . ? O2 C15 C24 C23 179.3(8) . . . . ? C16 C15 C24 C25 176.9(10) . . . . ? O2 C15 C24 C25 4.7(14) . . . . ? C22 C23 C24 C15 -172.7(10) . . . . ? C18 C23 C24 C15 3.4(14) . . . . ? C22 C23 C24 C25 2.1(15) . . . . ? C18 C23 C24 C25 178.2(9) . . . . ? C15 C24 C25 C34 53.2(14) . . . . ? C23 C24 C25 C34 -121.2(11) . . . . ? C15 C24 C25 C26 -128.0(11) . . . . ? C23 C24 C25 C26 57.5(14) . . . . ? C34 C25 C26 C31 6.6(16) . . . . ? C24 C25 C26 C31 -172.1(10) . . . . ? C34 C25 C26 C27 -170.1(11) . . . . ? C24 C25 C26 C27 11.1(17) . . . . ? C31 C26 C27 C28 -0.5(19) . . . . ? C25 C26 C27 C28 176.2(12) . . . . ? C26 C27 C28 C29 1(2) . . . . ? C27 C28 C29 C30 1(2) . . . . ? C28 C29 C30 C31 -3(2) . . . . ? C27 C26 C31 C32 177.9(11) . . . . ? C25 C26 C31 C32 1.0(17) . . . . ? C27 C26 C31 C30 -1.6(18) . . . . ? C25 C26 C31 C30 -178.5(11) . . . . ? C29 C30 C31 C26 3.3(19) . . . . ? C29 C30 C31 C32 -176.2(12) . . . . ? C26 C31 C32 C33 -6.3(19) . . . . ? C30 C31 C32 C33 173.2(11) . . . . ? C31 C32 C33 C34 3.5(16) . . . . ? C31 C32 C33 Si2 -178.6(9) . . . . ? C53 Si2 C33 C32 -91.7(10) . . . . ? C65 Si2 C33 C32 144.6(9) . . . . ? C59 Si2 C33 C32 26.2(10) . . . . ? C53 Si2 C33 C34 85.7(10) . . . . ? C65 Si2 C33 C34 -37.9(11) . . . . ? C59 Si2 C33 C34 -156.3(9) . . . . ? C26 C25 C34 O3 171.2(9) . . . . ? C24 C25 C34 O3 -10.0(14) . . . . ? C26 C25 C34 C33 -10.1(17) . . . . ? C24 C25 C34 C33 168.7(10) . . . . ? P1 O3 C34 C25 -70.5(11) . . . . ? P1 O3 C34 C33 110.6(8) . . . . ? C32 C33 C34 C25 4.9(16) . . . . ? Si2 C33 C34 C25 -172.7(9) . . . . ? C32 C33 C34 O3 -176.4(9) . . . . ? Si2 C33 C34 O3 6.0(14) . . . . ? C47 Si1 C35 C36 173.8(9) . . . . ? C16 Si1 C35 C36 60.0(11) . . . . ? C41 Si1 C35 C36 -70.3(11) . . . . ? C47 Si1 C35 C40 -5.3(12) . . . . ? C16 Si1 C35 C40 -119.1(11) . . . . ? C41 Si1 C35 C40 110.6(11) . . . . ? C40 C35 C36 C37 -0.1(18) . . . . ? Si1 C35 C36 C37 -179.3(9) . . . . ? C35 C36 C37 C38 -2(2) . . . . ? C36 C37 C38 C39 3(2) . . . . ? C37 C38 C39 C40 -3(2) . . . . ? C38 C39 C40 C35 1(2) . . . . ? C36 C35 C40 C39 0.6(18) . . . . ? Si1 C35 C40 C39 179.8(10) . . . . ? C35 Si1 C41 C42 -167.7(9) . . . . ? C47 Si1 C41 C42 -50.5(10) . . . . ? C16 Si1 C41 C42 69.6(11) . . . . ? C35 Si1 C41 C46 7.0(11) . . . . ? C47 Si1 C41 C46 124.2(9) . . . . ? C16 Si1 C41 C46 -115.6(9) . . . . ? C46 C41 C42 C43 3.0(17) . . . . ? Si1 C41 C42 C43 177.7(8) . . . . ? C41 C42 C43 C44 -1.8(17) . . . . ? C42 C43 C44 C45 1.4(18) . . . . ? C43 C44 C45 C46 -2.1(18) . . . . ? C42 C41 C46 C45 -3.7(17) . . . . ? Si1 C41 C46 C45 -178.6(8) . . . . ? C44 C45 C46 C41 3.3(17) . . . . ? C35 Si1 C47 C48 91.7(10) . . . . ? C16 Si1 C47 C48 -153.5(9) . . . . ? C41 Si1 C47 C48 -24.5(10) . . . . ? C35 Si1 C47 C52 -85.8(10) . . . . ? C16 Si1 C47 C52 29.0(10) . . . . ? C41 Si1 C47 C52 158.0(9) . . . . ? C52 C47 C48 C49 1.9(16) . . . . ? Si1 C47 C48 C49 -175.6(9) . . . . ? C47 C48 C49 C50 -1.8(18) . . . . ? C48 C49 C50 C51 1.7(18) . . . . ? C49 C50 C51 C52 -1.9(17) . . . . ? C48 C47 C52 C51 -2.2(17) . . . . ? Si1 C47 C52 C51 175.4(9) . . . . ? C50 C51 C52 C47 2.2(18) . . . . ? C33 Si2 C53 C54 23.3(11) . . . . ? C65 Si2 C53 C54 151.4(10) . . . . ? C59 Si2 C53 C54 -91.2(11) . . . . ? C33 Si2 C53 C58 -161.1(9) . . . . ? C65 Si2 C53 C58 -33.0(10) . . . . ? C59 Si2 C53 C58 84.4(10) . . . . ? C58 C53 C54 C55 -2.1(19) . . . . ? Si2 C53 C54 C55 173.7(11) . . . . ? C53 C54 C55 C56 4(2) . . . . ? C54 C55 C56 C57 -4.9(19) . . . . ? C55 C56 C57 C58 3.5(18) . . . . ? C56 C57 C58 C53 -1.3(19) . . . . ? C54 C53 C58 C57 0.5(18) . . . . ? Si2 C53 C58 C57 -175.4(10) . . . . ? C33 Si2 C59 C64 43.8(10) . . . . ? C53 Si2 C59 C64 160.7(9) . . . . ? C65 Si2 C59 C64 -80.8(10) . . . . ? C33 Si2 C59 C60 -139.8(8) . . . . ? C53 Si2 C59 C60 -22.9(9) . . . . ? C65 Si2 C59 C60 95.6(9) . . . . ? C64 C59 C60 C61 -4.3(16) . . . . ? Si2 C59 C60 C61 179.1(9) . . . . ? C59 C60 C61 C62 6(2) . . . . ? C60 C61 C62 C63 -3(2) . . . . ? C61 C62 C63 C64 -2(2) . . . . ? C60 C59 C64 C63 -0.2(16) . . . . ? Si2 C59 C64 C63 176.2(9) . . . . ? C62 C63 C64 C59 3.6(19) . . . . ? C33 Si2 C65 C70 -91.2(9) . . . . ? C53 Si2 C65 C70 145.3(8) . . . . ? C59 Si2 C65 C70 26.0(9) . . . . ? C33 Si2 C65 C66 94.2(9) . . . . ? C53 Si2 C65 C66 -29.3(9) . . . . ? C59 Si2 C65 C66 -148.7(8) . . . . ? C70 C65 C66 C67 -3.5(14) . . . . ? Si2 C65 C66 C67 171.4(8) . . . . ? C65 C66 C67 C68 2.6(16) . . . . ? C66 C67 C68 C69 -1.3(16) . . . . ? C67 C68 C69 C70 0.9(16) . . . . ? C68 C69 C70 C65 -1.8(15) . . . . ? C66 C65 C70 C69 3.0(14) . . . . ? Si2 C65 C70 C69 -171.9(8) . . . . ? P2 Pd2 C71 C76 -176.5(8) . . . . ? Cl2 Pd2 C71 C76 -167.9(16) . . . . ? Cl1 Pd2 C71 C76 0.8(8) . . . . ? P2 Pd2 C71 C72 3.2(7) . . . . ? Cl2 Pd2 C71 C72 12(3) . . . . ? Cl1 Pd2 C71 C72 -179.4(7) . . . . ? P2 O5 C72 C73 -178.4(8) . . . . ? P2 O5 C72 C71 -0.6(11) . . . . ? C76 C71 C72 O5 177.3(8) . . . . ? Pd2 C71 C72 O5 -2.5(12) . . . . ? C76 C71 C72 C73 -4.8(15) . . . . ? Pd2 C71 C72 C73 175.4(8) . . . . ? O5 C72 C73 C74 -178.6(9) . . . . ? C71 C72 C73 C74 3.6(15) . . . . ? O5 C72 C73 C77 1.4(15) . . . . ? C71 C72 C73 C77 -176.4(10) . . . . ? C72 C73 C74 C75 -1.0(16) . . . . ? C77 C73 C74 C75 179.0(10) . . . . ? C73 C74 C75 C76 -0.2(15) . . . . ? C73 C74 C75 C81 177.8(10) . . . . ? C72 C71 C76 C75 3.6(14) . . . . ? Pd2 C71 C76 C75 -176.6(7) . . . . ? C72 C71 C76 O8 -176.5(9) . . . . ? Pd2 C71 C76 O8 3.3(13) . . . . ? C74 C75 C76 C71 -1.1(14) . . . . ? C81 C75 C76 C71 -179.2(9) . . . . ? C74 C75 C76 O8 178.9(9) . . . . ? C81 C75 C76 O8 0.9(14) . . . . ? C72 C73 C77 C78 -59.8(14) . . . . ? C74 C73 C77 C78 120.3(11) . . . . ? C72 C73 C77 C79 61.2(14) . . . . ? C74 C73 C77 C79 -118.8(11) . . . . ? C72 C73 C77 C80 176.4(10) . . . . ? C74 C73 C77 C80 -3.5(15) . . . . ? C76 C75 C81 C82 177.7(10) . . . . ? C74 C75 C81 C82 -0.3(14) . . . . ? C76 C75 C81 C83 -62.7(13) . . . . ? C74 C75 C81 C83 119.3(11) . . . . ? C76 C75 C81 C84 59.0(13) . . . . ? C74 C75 C81 C84 -119.0(11) . . . . ? P2 O6 C85 C94 -61.7(12) . . . . ? P2 O6 C85 C86 121.6(9) . . . . ? C94 C85 C86 C87 4.8(16) . . . . ? O6 C85 C86 C87 -178.9(9) . . . . ? C94 C85 C86 Si3 -168.7(9) . . . . ? O6 C85 C86 Si3 7.7(14) . . . . ? C117 Si3 C86 C85 -20.3(12) . . . . ? C111 Si3 C86 C85 -144.1(10) . . . . ? C105 Si3 C86 C85 100.9(10) . . . . ? C117 Si3 C86 C87 166.4(8) . . . . ? C111 Si3 C86 C87 42.6(10) . . . . ? C105 Si3 C86 C87 -72.4(9) . . . . ? C85 C86 C87 C88 1.0(16) . . . . ? Si3 C86 C87 C88 175.2(9) . . . . ? C86 C87 C88 C89 177.8(11) . . . . ? C86 C87 C88 C93 -1.7(17) . . . . ? C87 C88 C89 C90 -175.5(12) . . . . ? C93 C88 C89 C90 3.9(18) . . . . ? C88 C89 C90 C91 -1(2) . . . . ? C89 C90 C91 C92 -0.9(19) . . . . ? C90 C91 C92 C93 0.3(19) . . . . ? C91 C92 C93 C94 -179.7(12) . . . . ? C91 C92 C93 C88 2.3(17) . . . . ? C89 C88 C93 C92 -4.3(16) . . . . ? C87 C88 C93 C92 175.1(10) . . . . ? C89 C88 C93 C94 177.6(11) . . . . ? C87 C88 C93 C94 -3.0(15) . . . . ? C86 C85 C94 C93 -9.4(17) . . . . ? O6 C85 C94 C93 174.3(9) . . . . ? C86 C85 C94 C95 168.3(10) . . . . ? O6 C85 C94 C95 -8.0(15) . . . . ? C92 C93 C94 C85 -169.9(10) . . . . ? C88 C93 C94 C85 8.1(15) . . . . ? C92 C93 C94 C95 12.4(16) . . . . ? C88 C93 C94 C95 -169.7(10) . . . . ? C85 C94 C95 C104 56.3(15) . . . . ? C93 C94 C95 C104 -126.1(12) . . . . ? C85 C94 C95 C96 -121.6(12) . . . . ? C93 C94 C95 C96 56.0(15) . . . . ? C104 C95 C96 C101 6.3(17) . . . . ? C94 C95 C96 C101 -175.7(11) . . . . ? C104 C95 C96 C97 -169.1(11) . . . . ? C94 C95 C96 C97 8.8(18) . . . . ? C95 C96 C97 C98 178.1(12) . . . . ? C101 C96 C97 C98 2.5(19) . . . . ? C96 C97 C98 C99 1(2) . . . . ? C97 C98 C99 C100 -3(2) . . . . ? C98 C99 C100 C101 2(2) . . . . ? C99 C100 C101 C96 1(2) . . . . ? C99 C100 C101 C102 -179.6(13) . . . . ? C95 C96 C101 C100 -179.1(12) . . . . ? C97 C96 C101 C100 -3.4(18) . . . . ? C95 C96 C101 C102 1.5(17) . . . . ? C97 C96 C101 C102 177.2(11) . . . . ? C100 C101 C102 C103 174.6(12) . . . . ? C96 C101 C102 C103 -6.1(18) . . . . ? C101 C102 C103 C104 2.3(17) . . . . ? C101 C102 C103 Si4 -179.1(9) . . . . ? C123 Si4 C103 C102 26.9(10) . . . . ? C129 Si4 C103 C102 149.7(9) . . . . ? C135 Si4 C103 C102 -89.6(9) . . . . ? C123 Si4 C103 C104 -154.6(9) . . . . ? C129 Si4 C103 C104 -31.7(11) . . . . ? C135 Si4 C103 C104 89.0(10) . . . . ? C96 C95 C104 O7 174.0(9) . . . . ? C94 C95 C104 O7 -3.9(15) . . . . ? C96 C95 C104 C103 -10.6(17) . . . . ? C94 C95 C104 C103 171.5(10) . . . . ? P2 O7 C104 C95 -73.1(11) . . . . ? P2 O7 C104 C103 111.2(9) . . . . ? C102 C103 C104 C95 6.3(16) . . . . ? Si4 C103 C104 C95 -172.2(9) . . . . ? C102 C103 C104 O7 -178.2(9) . . . . ? Si4 C103 C104 O7 3.2(14) . . . . ? C117 Si3 C105 C110 172.2(10) . . . . ? C111 Si3 C105 C110 -68.8(11) . . . . ? C86 Si3 C105 C110 45.1(11) . . . . ? C117 Si3 C105 C106 -16.3(10) . . . . ? C111 Si3 C105 C106 102.7(10) . . . . ? C86 Si3 C105 C106 -143.5(9) . . . . ? C110 C105 C106 C107 -1.7(17) . . . . ? Si3 C105 C106 C107 -173.9(9) . . . . ? C105 C106 C107 C108 0.8(18) . . . . ? C106 C107 C108 C109 0.4(17) . . . . ? C107 C108 C109 C110 -0.7(19) . . . . ? C108 C109 C110 C105 0(2) . . . . ? C106 C105 C110 C109 1.4(18) . . . . ? Si3 C105 C110 C109 173.5(11) . . . . ? C117 Si3 C111 C116 -104.2(11) . . . . ? C105 Si3 C111 C116 138.7(10) . . . . ? C86 Si3 C111 C116 23.8(11) . . . . ? C117 Si3 C111 C112 77.0(10) . . . . ? C105 Si3 C111 C112 -40.1(10) . . . . ? C86 Si3 C111 C112 -155.1(9) . . . . ? C116 C111 C112 C113 -1.6(17) . . . . ? Si3 C111 C112 C113 177.3(9) . . . . ? C111 C112 C113 C114 -3.0(18) . . . . ? C112 C113 C114 C115 7.3(18) . . . . ? C113 C114 C115 C116 -7.0(17) . . . . ? C112 C111 C116 C115 1.8(17) . . . . ? Si3 C111 C116 C115 -177.1(8) . . . . ? C114 C115 C116 C111 2.5(17) . . . . ? C111 Si3 C117 C122 3.8(11) . . . . ? C105 Si3 C117 C122 121.0(9) . . . . ? C86 Si3 C117 C122 -117.7(9) . . . . ? C111 Si3 C117 C118 -167.5(9) . . . . ? C105 Si3 C117 C118 -50.3(10) . . . . ? C86 Si3 C117 C118 71.0(10) . . . . ? C122 C117 C118 C119 1.1(16) . . . . ? Si3 C117 C118 C119 172.7(8) . . . . ? C117 C118 C119 C120 0.7(16) . . . . ? C118 C119 C120 C121 -0.4(16) . . . . ? C119 C120 C121 C122 -1.6(17) . . . . ? C120 C121 C122 C117 3.5(16) . . . . ? C118 C117 C122 C121 -3.2(16) . . . . ? Si3 C117 C122 C121 -174.6(8) . . . . ? C129 Si4 C123 C124 111.5(9) . . . . ? C135 Si4 C123 C124 -5.5(10) . . . . ? C103 Si4 C123 C124 -121.1(9) . . . . ? C129 Si4 C123 C128 -70.1(10) . . . . ? C135 Si4 C123 C128 173.0(9) . . . . ? C103 Si4 C123 C128 57.3(10) . . . . ? C128 C123 C124 C125 5.0(16) . . . . ? Si4 C123 C124 C125 -176.4(9) . . . . ? C123 C124 C125 C126 -2.2(17) . . . . ? C124 C125 C126 C127 -2.0(17) . . . . ? C125 C126 C127 C128 3.0(18) . . . . ? C126 C127 C128 C123 0.2(18) . . . . ? C124 C123 C128 C127 -3.9(16) . . . . ? Si4 C123 C128 C127 177.5(9) . . . . ? C123 Si4 C129 C134 -151.5(7) . . . . ? C135 Si4 C129 C134 -33.1(9) . . . . ? C103 Si4 C129 C134 88.2(9) . . . . ? C123 Si4 C129 C130 23.5(9) . . . . ? C135 Si4 C129 C130 141.8(8) . . . . ? C103 Si4 C129 C130 -96.9(9) . . . . ? C134 C129 C130 C131 1.3(14) . . . . ? Si4 C129 C130 C131 -173.9(7) . . . . ? C129 C130 C131 C132 0.2(14) . . . . ? C130 C131 C132 C133 -1.0(15) . . . . ? C131 C132 C133 C134 0.2(16) . . . . ? C130 C129 C134 C133 -2.0(14) . . . . ? Si4 C129 C134 C133 173.2(8) . . . . ? C132 C133 C134 C129 1.3(15) . . . . ? C123 Si4 C135 C136 -96.1(10) . . . . ? C129 Si4 C135 C136 144.8(9) . . . . ? C103 Si4 C135 C136 17.8(11) . . . . ? C123 Si4 C135 C140 79.6(9) . . . . ? C129 Si4 C135 C140 -39.4(9) . . . . ? C103 Si4 C135 C140 -166.5(8) . . . . ? C140 C135 C136 C137 1.5(17) . . . . ? Si4 C135 C136 C137 177.4(10) . . . . ? C135 C136 C137 C138 -1(2) . . . . ? C136 C137 C138 C139 1(2) . . . . ? C137 C138 C139 C140 -1.6(18) . . . . ? C138 C139 C140 C135 2.1(17) . . . . ? C136 C135 C140 C139 -2.0(15) . . . . ? Si4 C135 C140 C139 -178.1(8) . . . . ? C141 C142 C143 C144 175.0(16) . . . . ? C142 C143 C144 C145 175.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.523 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.138 # Attachment '- 11.cif' data_yc4_26squeeze _database_code_depnum_ccdc_archive 'CCDC 815810' #TrackingRef '- 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Cl2 O4 P Pd Si2, C6 H16 N' _chemical_formula_sum 'C46 H64 Cl2 N O4 P Pd Si2' _chemical_formula_weight 959.43 _chemical_absolute_configuration ad 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 27.1630(4) _cell_length_b 14.3800(2) _cell_length_c 14.1182(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.2860(10) _cell_angle_gamma 90.00 _cell_volume 5319.53(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 77077 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.6 _exptl_crystal_description shard _exptl_crystal_colour brown _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7015 _exptl_absorpt_correction_T_max 0.9460 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, G.M., 2008)' _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 Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 77077 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 30.60 _reflns_number_total 16225 _reflns_number_gt 14689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.713 0.000 151 33 ' ' 2 0.500 0.213 0.000 151 33 ' ' 3 0.500 0.788 0.500 164 32 ' ' 4 1.000 0.288 0.500 164 32 ' ' _platon_squeeze_details ; The discordered solvent is likely to be pentane. The electron count may not be accurate; three low angle reflections are missing. ; _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^)+(0.0397P)^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 -0.013(11) _refine_ls_number_reflns 16225 _refine_ls_number_parameters 564 _refine_ls_number_restraints 133 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.018 _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 Pd1 Pd 0.760580(5) 0.560579(11) 0.876370(9) 0.01804(4) Uani 1 1 d . . . P1 P 0.770359(18) 0.52890(4) 0.73459(3) 0.01569(10) Uani 1 1 d . . . Si1 Si 0.88363(2) 0.33716(5) 0.88643(5) 0.02768(13) Uani 1 1 d . . . Si2 Si 0.70383(2) 0.74595(4) 0.53758(4) 0.02147(11) Uani 1 1 d . . . Cl1 Cl 0.75324(2) 0.60135(4) 1.03591(4) 0.03010(12) Uani 1 1 d . . . Cl2 Cl 0.84970(2) 0.59664(4) 0.93153(4) 0.03089(12) Uani 1 1 d . . . O1 O 0.71988(5) 0.48194(10) 0.66902(9) 0.0183(3) Uani 1 1 d . . . O2 O 0.80897(5) 0.45320(10) 0.71374(10) 0.0175(3) Uani 1 1 d . . . O3 O 0.78308(5) 0.62034(10) 0.68128(9) 0.0174(3) Uani 1 1 d . . . O4 O 0.64571(7) 0.58506(16) 0.92526(13) 0.0489(6) Uani 1 1 d . . . H4 H 0.6761 0.5998 0.9520 0.073 Uiso 1 1 calc R . . C1 C 0.68630(8) 0.52832(15) 0.80344(14) 0.0202(4) Uani 1 1 d . . . C2 C 0.67761(7) 0.48987(14) 0.70943(14) 0.0173(4) Uani 1 1 d . . . C3 C 0.63061(7) 0.46053(14) 0.65038(15) 0.0196(4) Uani 1 1 d . . . C4 C 0.58919(8) 0.48108(17) 0.68843(17) 0.0282(5) Uani 1 1 d . A . H4A H 0.5561 0.4629 0.6512 0.034 Uiso 1 1 calc R . . C5 C 0.59338(9) 0.52648(19) 0.77728(19) 0.0356(6) Uani 1 1 d . . . C6 C 0.64266(8) 0.54616(19) 0.83618(16) 0.0297(5) Uani 1 1 d . A . C7 C 0.62413(7) 0.41116(15) 0.55124(15) 0.0216(4) Uani 1 1 d . . . C8 C 0.65696(8) 0.32242(16) 0.56593(16) 0.0263(5) Uani 1 1 d . . . H8A H 0.6927 0.3386 0.5965 0.039 Uiso 1 1 calc R . . H8B H 0.6542 0.2930 0.5021 0.039 Uiso 1 1 calc R . . H8C H 0.6449 0.2791 0.6085 0.039 Uiso 1 1 calc R . . C9 C 0.63887(8) 0.47658(17) 0.47664(15) 0.0266(5) Uani 1 1 d . . . H9A H 0.6174 0.5324 0.4679 0.040 Uiso 1 1 calc R . . H9B H 0.6337 0.4445 0.4135 0.040 Uiso 1 1 calc R . . H9C H 0.6748 0.4944 0.5011 0.040 Uiso 1 1 calc R . . C10 C 0.56854(8) 0.38214(18) 0.50678(17) 0.0298(5) Uani 1 1 d . . . H10A H 0.5589 0.3349 0.5486 0.045 Uiso 1 1 calc R . . H10B H 0.5649 0.3564 0.4410 0.045 Uiso 1 1 calc R . . H10C H 0.5463 0.4365 0.5023 0.045 Uiso 1 1 calc R . . C11A C 0.5450(3) 0.5646(5) 0.8015(6) 0.0458(15) Uani 0.744(15) 1 d PU A 1 C12A C 0.49598(18) 0.5380(4) 0.7254(5) 0.0547(18) Uani 0.744(15) 1 d PU A 1 H12A H 0.4923 0.4701 0.7234 0.082 Uiso 0.744(15) 1 calc PR A 1 H12B H 0.4973 0.5608 0.6607 0.082 Uiso 0.744(15) 1 calc PR A 1 H12C H 0.4667 0.5659 0.7432 0.082 Uiso 0.744(15) 1 calc PR A 1 C13A C 0.5402(2) 0.5263(6) 0.8997(5) 0.065(2) Uani 0.744(15) 1 d PU A 1 H13A H 0.5706 0.5433 0.9517 0.098 Uiso 0.744(15) 1 calc PR A 1 H13B H 0.5372 0.4584 0.8957 0.098 Uiso 0.744(15) 1 calc PR A 1 H13C H 0.5098 0.5525 0.9146 0.098 Uiso 0.744(15) 1 calc PR A 1 C14A C 0.5474(2) 0.6731(4) 0.8034(7) 0.066(2) Uani 0.744(15) 1 d PU A 1 H14A H 0.5785 0.6933 0.8518 0.100 Uiso 0.744(15) 1 calc PR A 1 H14B H 0.5175 0.6978 0.8213 0.100 Uiso 0.744(15) 1 calc PR A 1 H14C H 0.5478 0.6962 0.7383 0.100 Uiso 0.744(15) 1 calc PR A 1 C11B C 0.5450(8) 0.530(2) 0.8263(14) 0.059(5) Uani 0.256(15) 1 d PU A 2 C12B C 0.4948(7) 0.476(4) 0.746(2) 0.138(11) Uani 0.256(15) 1 d PU A 2 H12D H 0.4898 0.5030 0.6804 0.207 Uiso 0.256(15) 1 calc PR A 2 H12E H 0.4638 0.4845 0.7680 0.207 Uiso 0.256(15) 1 calc PR A 2 H12F H 0.5022 0.4094 0.7435 0.207 Uiso 0.256(15) 1 calc PR A 2 C13B C 0.5478(8) 0.468(2) 0.9169(15) 0.087(6) Uani 0.256(15) 1 d PU A 2 H13D H 0.5480 0.4028 0.8983 0.131 Uiso 0.256(15) 1 calc PR A 2 H13E H 0.5182 0.4807 0.9422 0.131 Uiso 0.256(15) 1 calc PR A 2 H13F H 0.5792 0.4827 0.9679 0.131 Uiso 0.256(15) 1 calc PR A 2 C14B C 0.5440(8) 0.6375(19) 0.8486(12) 0.078(6) Uani 0.256(15) 1 d PU A 2 H14D H 0.5445 0.6729 0.7895 0.117 Uiso 0.256(15) 1 calc PR A 2 H14E H 0.5739 0.6539 0.9019 0.117 Uiso 0.256(15) 1 calc PR A 2 H14F H 0.5128 0.6525 0.8681 0.117 Uiso 0.256(15) 1 calc PR A 2 C15 C 0.86059(7) 0.47480(14) 0.72352(14) 0.0181(4) Uani 1 1 d . . . C16 C 0.89702(8) 0.42775(16) 0.79934(16) 0.0248(4) Uani 1 1 d . . . C17 C 0.94724(8) 0.45075(18) 0.80616(17) 0.0315(5) Uani 1 1 d . . . H17 H 0.9733 0.4197 0.8539 0.038 Uiso 1 1 calc R . . C18 C 0.96184(8) 0.51777(18) 0.74606(18) 0.0309(5) Uani 1 1 d . . . C19 C 1.01367(8) 0.5446(2) 0.7602(2) 0.0418(7) Uani 1 1 d . . . H19 H 1.0392 0.5155 0.8106 0.050 Uiso 1 1 calc R . . C20 C 1.02767(9) 0.6108(2) 0.7037(2) 0.0427(7) Uani 1 1 d . . . H20 H 1.0626 0.6273 0.7142 0.051 Uiso 1 1 calc R . . C21 C 0.98972(9) 0.65467(18) 0.6293(2) 0.0351(5) Uani 1 1 d . . . H21 H 0.9992 0.7021 0.5908 0.042 Uiso 1 1 calc R . . C22 C 0.93989(8) 0.63004(17) 0.61203(17) 0.0277(5) Uani 1 1 d . . . H22 H 0.9152 0.6599 0.5608 0.033 Uiso 1 1 calc R . . C23 C 0.92408(7) 0.5606(2) 0.66903(14) 0.0236(4) Uani 1 1 d . . . C24 C 0.87176(7) 0.53339(14) 0.65536(14) 0.0186(4) Uani 1 1 d . . . C25 C 0.83076(6) 0.56817(17) 0.57050(12) 0.0171(3) Uani 1 1 d . . . C26 C 0.83295(7) 0.55468(18) 0.47072(12) 0.0188(3) Uani 1 1 d . . . C27 C 0.87141(8) 0.50091(16) 0.44564(16) 0.0236(4) Uani 1 1 d . . . H27 H 0.8975 0.4730 0.4959 0.028 Uiso 1 1 calc R . . C28 C 0.87102(9) 0.48908(17) 0.34879(16) 0.0285(5) Uani 1 1 d . . . H28 H 0.8968 0.4523 0.3330 0.034 Uiso 1 1 calc R . . C29 C 0.83353(9) 0.53001(17) 0.27328(16) 0.0299(5) Uani 1 1 d . . . H29 H 0.8344 0.5220 0.2069 0.036 Uiso 1 1 calc R . . C30 C 0.79573(8) 0.58153(15) 0.29472(14) 0.0250(5) Uani 1 1 d . . . H30 H 0.7703 0.6094 0.2431 0.030 Uiso 1 1 calc R . . C31 C 0.79395(8) 0.59389(15) 0.39324(14) 0.0209(4) Uani 1 1 d . . . C32 C 0.75399(8) 0.64574(15) 0.41587(14) 0.0198(4) Uani 1 1 d . . . H32 H 0.7291 0.6738 0.3636 0.024 Uiso 1 1 calc R . . C33 C 0.74986(7) 0.65709(14) 0.51066(14) 0.0184(4) Uani 1 1 d . . . C34 C 0.78827(7) 0.61282(14) 0.58444(13) 0.0173(4) Uani 1 1 d . . . C35 C 0.91170(13) 0.3800(2) 1.0145(2) 0.0543(8) Uani 1 1 d . . . H35A H 0.8930 0.4352 1.0263 0.081 Uiso 1 1 calc R . . H35B H 0.9476 0.3962 1.0228 0.081 Uiso 1 1 calc R . . H35C H 0.9092 0.3312 1.0614 0.081 Uiso 1 1 calc R . . C36 C 0.91691(14) 0.2289(2) 0.8677(3) 0.0582(9) Uani 1 1 d . . . H36A H 0.9107 0.1804 0.9120 0.087 Uiso 1 1 calc R . . H36B H 0.9537 0.2408 0.8817 0.087 Uiso 1 1 calc R . . H36C H 0.9040 0.2081 0.7995 0.087 Uiso 1 1 calc R . . C37 C 0.81503(10) 0.31003(19) 0.8685(2) 0.0351(6) Uani 1 1 d . . . H37A H 0.8000 0.2918 0.8001 0.053 Uiso 1 1 calc R . . H37B H 0.7973 0.3651 0.8839 0.053 Uiso 1 1 calc R . . H37C H 0.8115 0.2588 0.9120 0.053 Uiso 1 1 calc R . . C38 C 0.74418(9) 0.85019(16) 0.58432(18) 0.0301(5) Uani 1 1 d . . . H38A H 0.7256 0.8921 0.6174 0.045 Uiso 1 1 calc R . . H38B H 0.7521 0.8827 0.5292 0.045 Uiso 1 1 calc R . . H38C H 0.7760 0.8303 0.6309 0.045 Uiso 1 1 calc R . . C39 C 0.65579(9) 0.77125(19) 0.41987(18) 0.0349(5) Uani 1 1 d . . . H39A H 0.6386 0.7135 0.3928 0.052 Uiso 1 1 calc R . . H39B H 0.6729 0.7981 0.3732 0.052 Uiso 1 1 calc R . . H39C H 0.6306 0.8155 0.4316 0.052 Uiso 1 1 calc R . . C40 C 0.66900(9) 0.71109(17) 0.62943(17) 0.0293(5) Uani 1 1 d . . . H40A H 0.6462 0.7616 0.6374 0.044 Uiso 1 1 calc R . . H40B H 0.6936 0.6984 0.6926 0.044 Uiso 1 1 calc R . . H40C H 0.6489 0.6550 0.6066 0.044 Uiso 1 1 calc R . . N1 N 0.81866(11) 0.80312(17) 0.95830(17) 0.0509(7) Uani 1 1 d . . . H1 H 0.8144 0.7389 0.9583 0.061 Uiso 1 1 calc R . . C44 C 0.86148(17) 0.7820(2) 1.1374(2) 0.0655(10) Uani 1 1 d . . . H44A H 0.8333 0.8106 1.1585 0.098 Uiso 1 1 calc R . . H44B H 0.8936 0.7930 1.1874 0.098 Uiso 1 1 calc R . . H44C H 0.8555 0.7149 1.1290 0.098 Uiso 1 1 calc R . . C42 C 0.72417(16) 0.8249(3) 0.8912(3) 0.0679(10) Uani 1 1 d . . . H42A H 0.7273 0.8568 0.8317 0.102 Uiso 1 1 calc R . . H42B H 0.6939 0.8479 0.9093 0.102 Uiso 1 1 calc R . . H42C H 0.7208 0.7578 0.8788 0.102 Uiso 1 1 calc R . . C41 C 0.77193(14) 0.8438(2) 0.9754(2) 0.0537(8) Uani 1 1 d . . . H41A H 0.7766 0.9119 0.9841 0.064 Uiso 1 1 calc R . . H41B H 0.7666 0.8180 1.0370 0.064 Uiso 1 1 calc R . . C45 C 0.82792(18) 0.8277(3) 0.8600(2) 0.0657(11) Uani 1 1 d . . . H45A H 0.7994 0.8032 0.8070 0.079 Uiso 1 1 calc R . . H45B H 0.8596 0.7967 0.8546 0.079 Uiso 1 1 calc R . . C43 C 0.86443(16) 0.8245(2) 1.0408(2) 0.0619(9) Uani 1 1 d . . . H43A H 0.8679 0.8928 1.0487 0.074 Uiso 1 1 calc R . . H43B H 0.8953 0.8009 1.0241 0.074 Uiso 1 1 calc R . . C46 C 0.83280(19) 0.9323(3) 0.8445(3) 0.0800(13) Uani 1 1 d . . . H46A H 0.8023 0.9640 0.8528 0.120 Uiso 1 1 calc R . . H46B H 0.8362 0.9436 0.7781 0.120 Uiso 1 1 calc R . . H46C H 0.8630 0.9562 0.8928 0.120 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 Pd1 0.02402(6) 0.01755(6) 0.01303(5) 0.00031(6) 0.00573(4) 0.00174(7) P1 0.0158(2) 0.0174(2) 0.0142(2) 0.00068(17) 0.00466(17) 0.00148(17) Si1 0.0279(3) 0.0280(3) 0.0259(3) 0.0088(3) 0.0049(2) 0.0063(3) Si2 0.0208(3) 0.0201(3) 0.0246(3) 0.0074(2) 0.0080(2) 0.0044(2) Cl1 0.0456(3) 0.0311(3) 0.0156(2) -0.0022(2) 0.0115(2) 0.0019(2) Cl2 0.0263(2) 0.0341(3) 0.0285(2) -0.0101(2) 0.0007(2) 0.0014(2) O1 0.0164(6) 0.0240(7) 0.0156(6) -0.0022(6) 0.0063(5) -0.0006(6) O2 0.0162(6) 0.0179(7) 0.0189(6) 0.0015(5) 0.0052(5) 0.0012(5) O3 0.0211(6) 0.0175(7) 0.0144(6) 0.0014(5) 0.0058(5) 0.0015(5) O4 0.0357(9) 0.0779(17) 0.0398(9) -0.0317(10) 0.0222(8) -0.0089(10) C1 0.0248(9) 0.0182(9) 0.0202(9) -0.0004(7) 0.0104(8) 0.0019(8) C2 0.0157(8) 0.0172(9) 0.0205(9) 0.0000(7) 0.0073(7) 0.0024(7) C3 0.0178(9) 0.0174(10) 0.0244(9) 0.0020(8) 0.0071(7) 0.0028(7) C4 0.0186(9) 0.0309(12) 0.0366(12) -0.0067(10) 0.0097(9) 0.0011(9) C5 0.0268(11) 0.0443(14) 0.0408(13) -0.0142(11) 0.0178(10) -0.0002(10) C6 0.0275(10) 0.0355(16) 0.0302(10) -0.0119(10) 0.0149(8) -0.0021(10) C7 0.0175(9) 0.0234(11) 0.0234(10) -0.0008(8) 0.0047(8) 0.0007(8) C8 0.0270(10) 0.0233(11) 0.0283(11) -0.0063(9) 0.0068(9) 0.0014(9) C9 0.0261(10) 0.0337(13) 0.0187(9) 0.0001(9) 0.0036(8) -0.0035(9) C10 0.0213(10) 0.0368(13) 0.0299(11) -0.0068(10) 0.0045(9) -0.0038(9) C11A 0.0280(18) 0.059(4) 0.059(3) -0.028(3) 0.027(2) -0.008(3) C12A 0.0199(16) 0.070(4) 0.082(3) -0.044(3) 0.0256(18) -0.0038(19) C13A 0.040(3) 0.111(6) 0.058(3) -0.044(3) 0.036(2) -0.027(3) C14A 0.038(2) 0.061(3) 0.101(5) -0.047(3) 0.019(3) 0.011(2) C11B 0.028(6) 0.109(13) 0.046(8) 0.004(7) 0.021(6) 0.010(9) C12B 0.029(7) 0.29(3) 0.099(12) -0.08(2) 0.021(8) -0.021(16) C13B 0.071(10) 0.143(17) 0.070(9) 0.024(12) 0.057(8) 0.021(13) C14B 0.073(10) 0.122(12) 0.037(7) 0.006(8) 0.012(7) 0.066(10) C15 0.0159(8) 0.0192(10) 0.0192(9) -0.0008(8) 0.0046(7) 0.0013(7) C16 0.0217(10) 0.0268(11) 0.0254(10) 0.0056(9) 0.0054(8) 0.0039(8) C17 0.0167(9) 0.0405(14) 0.0326(12) 0.0099(11) -0.0021(9) 0.0045(9) C18 0.0166(9) 0.0357(13) 0.0378(12) 0.0063(11) 0.0028(9) 0.0002(9) C19 0.0161(9) 0.050(2) 0.0546(15) 0.0108(14) 0.0009(9) 0.0019(11) C20 0.0189(11) 0.0446(16) 0.0629(18) 0.0073(14) 0.0079(11) -0.0051(11) C21 0.0232(11) 0.0322(13) 0.0509(15) 0.0042(12) 0.0115(10) -0.0044(10) C22 0.0215(10) 0.0303(12) 0.0314(11) 0.0049(10) 0.0070(9) -0.0010(9) C23 0.0177(8) 0.0250(9) 0.0286(9) 0.0017(12) 0.0067(7) 0.0016(11) C24 0.0153(8) 0.0210(10) 0.0198(8) -0.0004(7) 0.0051(7) 0.0014(7) C25 0.0173(7) 0.0171(10) 0.0177(7) 0.0010(8) 0.0059(6) -0.0013(8) C26 0.0201(8) 0.0174(9) 0.0207(8) 0.0009(9) 0.0086(6) -0.0028(9) C27 0.0228(10) 0.0234(11) 0.0268(10) -0.0008(8) 0.0105(8) -0.0007(8) C28 0.0312(11) 0.0285(12) 0.0321(11) -0.0075(10) 0.0197(9) -0.0057(10) C29 0.0403(12) 0.0319(12) 0.0208(9) -0.0065(9) 0.0135(9) -0.0121(10) C30 0.0338(11) 0.0249(13) 0.0168(8) -0.0008(7) 0.0075(8) -0.0076(8) C31 0.0254(10) 0.0204(9) 0.0179(8) -0.0021(8) 0.0074(7) -0.0069(8) C32 0.0222(9) 0.0187(10) 0.0166(9) 0.0030(8) 0.0017(7) -0.0045(8) C33 0.0194(9) 0.0175(10) 0.0183(9) 0.0032(7) 0.0051(7) -0.0011(7) C34 0.0189(8) 0.0183(10) 0.0156(8) 0.0011(7) 0.0063(7) -0.0014(7) C35 0.068(2) 0.054(2) 0.0305(13) 0.0117(13) -0.0052(13) -0.0060(16) C36 0.070(2) 0.0463(18) 0.067(2) 0.0228(16) 0.0337(17) 0.0322(16) C37 0.0345(12) 0.0303(13) 0.0429(15) 0.0144(11) 0.0146(11) 0.0020(11) C38 0.0300(11) 0.0218(12) 0.0404(13) 0.0017(10) 0.0127(10) 0.0025(9) C39 0.0302(12) 0.0375(14) 0.0353(12) 0.0130(11) 0.0058(10) 0.0117(10) C40 0.0296(11) 0.0275(12) 0.0364(12) 0.0095(10) 0.0186(10) 0.0091(9) N1 0.088(2) 0.0313(13) 0.0410(13) -0.0012(11) 0.0310(13) 0.0142(13) C44 0.112(3) 0.0397(18) 0.0433(17) -0.0029(15) 0.0176(19) -0.0001(19) C42 0.093(3) 0.048(2) 0.064(2) 0.0237(18) 0.023(2) 0.020(2) C41 0.092(3) 0.0317(15) 0.0476(16) 0.0038(13) 0.0355(17) 0.0150(16) C45 0.114(3) 0.052(2) 0.0427(17) 0.0058(16) 0.040(2) 0.021(2) C43 0.097(3) 0.0399(18) 0.0538(19) -0.0042(15) 0.0284(19) 0.0072(18) C46 0.134(4) 0.059(2) 0.062(2) 0.0167(19) 0.053(2) 0.017(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 Pd1 C1 2.062(2) . ? Pd1 P1 2.1366(5) . ? Pd1 Cl1 2.3862(5) . ? Pd1 Cl2 2.3961(6) . ? P1 O1 1.5886(14) . ? P1 O2 1.5919(14) . ? P1 O3 1.5975(14) . ? Si1 C36 1.854(3) . ? Si1 C37 1.855(3) . ? Si1 C35 1.872(3) . ? Si1 C16 1.891(2) . ? Si2 C39 1.858(2) . ? Si2 C40 1.864(2) . ? Si2 C38 1.871(2) . ? Si2 C33 1.895(2) . ? O1 C2 1.415(2) . ? O2 C15 1.407(2) . ? O3 C34 1.415(2) . ? O4 C6 1.359(3) . ? O4 H4 0.8400 . ? C1 C2 1.399(3) . ? C1 C6 1.405(3) . ? C2 C3 1.394(3) . ? C3 C4 1.400(3) . ? C3 C7 1.538(3) . ? C4 C5 1.392(3) . ? C4 H4A 0.9500 . ? C5 C6 1.406(3) . ? C5 C11A 1.543(6) . ? C5 C11B 1.64(2) . ? C7 C10 1.533(3) . ? C7 C8 1.539(3) . ? C7 C9 1.542(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11A C12A 1.523(8) . ? C11A C13A 1.529(8) . ? C11A C14A 1.562(8) . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C11B C13B 1.54(2) . ? C11B C14B 1.58(3) . ? C11B C12B 1.71(3) . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15 C24 1.372(3) . ? C15 C16 1.423(3) . ? C16 C17 1.382(3) . ? C17 C18 1.408(3) . ? C17 H17 0.9500 . ? C18 C19 1.422(3) . ? C18 C23 1.423(3) . ? C19 C20 1.358(4) . ? C19 H19 0.9500 . ? C20 C21 1.412(4) . ? C20 H20 0.9500 . ? C21 C22 1.357(3) . ? C21 H21 0.9500 . ? C22 C23 1.418(3) . ? C22 H22 0.9500 . ? C23 C24 1.437(3) . ? C24 C25 1.491(3) . ? C25 C34 1.380(3) . ? C25 C26 1.439(2) . ? C26 C27 1.418(3) . ? C26 C31 1.423(3) . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.396(3) . ? C28 H28 0.9500 . ? C29 C30 1.363(3) . ? C29 H29 0.9500 . ? C30 C31 1.416(3) . ? C30 H30 0.9500 . ? C31 C32 1.421(3) . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 C34 1.416(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 C41 1.475(4) . ? N1 C43 1.495(5) . ? N1 C45 1.516(4) . ? N1 H1 0.9300 . ? C44 C43 1.516(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C42 C41 1.536(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C45 C46 1.530(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 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 Pd1 P1 80.28(5) . . ? C1 Pd1 Cl1 102.26(5) . . ? P1 Pd1 Cl1 177.07(2) . . ? C1 Pd1 Cl2 169.36(5) . . ? P1 Pd1 Cl2 89.207(19) . . ? Cl1 Pd1 Cl2 88.20(2) . . ? O1 P1 O2 96.38(7) . . ? O1 P1 O3 109.63(8) . . ? O2 P1 O3 103.94(7) . . ? O1 P1 Pd1 109.58(5) . . ? O2 P1 Pd1 124.73(5) . . ? O3 P1 Pd1 111.20(5) . . ? C36 Si1 C37 108.30(16) . . ? C36 Si1 C35 108.95(16) . . ? C37 Si1 C35 109.88(15) . . ? C36 Si1 C16 107.53(13) . . ? C37 Si1 C16 114.49(11) . . ? C35 Si1 C16 107.56(13) . . ? C39 Si2 C40 108.01(11) . . ? C39 Si2 C38 111.49(12) . . ? C40 Si2 C38 109.12(11) . . ? C39 Si2 C33 107.31(10) . . ? C40 Si2 C33 116.16(9) . . ? C38 Si2 C33 104.76(10) . . ? C2 O1 P1 113.47(12) . . ? C15 O2 P1 121.27(13) . . ? C34 O3 P1 118.77(12) . . ? C6 O4 H4 109.5 . . ? C2 C1 C6 116.00(19) . . ? C2 C1 Pd1 117.43(14) . . ? C6 C1 Pd1 126.45(15) . . ? C3 C2 C1 125.86(17) . . ? C3 C2 O1 116.57(16) . . ? C1 C2 O1 117.55(16) . . ? C2 C3 C4 114.13(18) . . ? C2 C3 C7 123.45(17) . . ? C4 C3 C7 122.42(18) . . ? C5 C4 C3 124.2(2) . . ? C5 C4 H4A 117.9 . . ? C3 C4 H4A 117.9 . . ? C4 C5 C6 117.80(19) . . ? C4 C5 C11A 119.6(3) . . ? C6 C5 C11A 122.1(3) . . ? C4 C5 C11B 120.7(9) . . ? C6 C5 C11B 119.2(8) . . ? C11A C5 C11B 21.7(9) . . ? O4 C6 C1 121.9(2) . . ? O4 C6 C5 116.53(18) . . ? C1 C6 C5 121.53(19) . . ? C10 C7 C3 111.25(17) . . ? C10 C7 C8 107.62(19) . . ? C3 C7 C8 109.70(17) . . ? C10 C7 C9 106.95(17) . . ? C3 C7 C9 110.62(18) . . ? C8 C7 C9 110.63(17) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12A C11A C13A 106.3(5) . . ? C12A C11A C5 113.1(4) . . ? C13A C11A C5 110.7(5) . . ? C12A C11A C14A 106.7(5) . . ? C13A C11A C14A 111.0(5) . . ? C5 C11A C14A 108.9(4) . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C11A C13A H13A 109.5 . . ? C11A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C11A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C11A C14A H14A 109.5 . . ? C11A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C11A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13B C11B C14B 113.4(16) . . ? C13B C11B C5 117.5(16) . . ? C14B C11B C5 100.0(15) . . ? C13B C11B C12B 98(2) . . ? C14B C11B C12B 122(2) . . ? C5 C11B C12B 107.0(14) . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C11B C13B H13D 109.5 . . ? C11B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C11B C14B H14D 109.5 . . ? C11B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C11B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C24 C15 O2 117.76(16) . . ? C24 C15 C16 125.55(18) . . ? O2 C15 C16 116.50(17) . . ? C17 C16 C15 114.61(19) . . ? C17 C16 Si1 118.36(17) . . ? C15 C16 Si1 127.01(16) . . ? C16 C17 C18 123.5(2) . . ? C16 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C17 C18 C19 121.8(2) . . ? C17 C18 C23 119.72(19) . . ? C19 C18 C23 118.5(2) . . ? C20 C19 C18 121.8(2) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C21 119.2(2) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 121.0(2) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 121.2(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.24(18) . . ? C22 C23 C24 123.51(19) . . ? C18 C23 C24 118.2(2) . . ? C15 C24 C23 117.82(18) . . ? C15 C24 C25 120.89(17) . . ? C23 C24 C25 121.29(17) . . ? C34 C25 C26 117.03(17) . . ? C34 C25 C24 121.15(15) . . ? C26 C25 C24 121.80(16) . . ? C27 C26 C31 118.19(17) . . ? C27 C26 C25 122.78(18) . . ? C31 C26 C25 118.99(17) . . ? C28 C27 C26 120.2(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 121.3(2) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 120.02(19) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.6(2) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 120.85(19) . . ? C30 C31 C26 119.61(19) . . ? C32 C31 C26 119.54(17) . . ? C33 C32 C31 122.79(18) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C32 C33 C34 115.29(18) . . ? C32 C33 Si2 120.01(15) . . ? C34 C33 Si2 123.54(14) . . ? C25 C34 O3 118.26(16) . . ? C25 C34 C33 125.88(17) . . ? O3 C34 C33 115.77(16) . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C41 N1 C43 111.4(2) . . ? C41 N1 C45 114.5(3) . . ? C43 N1 C45 111.2(3) . . ? C41 N1 H1 106.4 . . ? C43 N1 H1 106.4 . . ? C45 N1 H1 106.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1 C41 C42 113.0(3) . . ? N1 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? N1 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N1 C45 C46 113.7(3) . . ? N1 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? N1 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? N1 C43 C44 112.8(3) . . ? N1 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? N1 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 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 C1 Pd1 P1 O1 -11.27(8) . . . . ? Cl1 Pd1 P1 O1 -161.6(4) . . . . ? Cl2 Pd1 P1 O1 170.39(6) . . . . ? C1 Pd1 P1 O2 -124.23(9) . . . . ? Cl1 Pd1 P1 O2 85.4(4) . . . . ? Cl2 Pd1 P1 O2 57.43(7) . . . . ? C1 Pd1 P1 O3 110.09(8) . . . . ? Cl1 Pd1 P1 O3 -40.2(5) . . . . ? Cl2 Pd1 P1 O3 -68.25(6) . . . . ? O2 P1 O1 C2 143.16(13) . . . . ? O3 P1 O1 C2 -109.55(13) . . . . ? Pd1 P1 O1 C2 12.75(14) . . . . ? O1 P1 O2 C15 156.34(14) . . . . ? O3 P1 O2 C15 44.25(15) . . . . ? Pd1 P1 O2 C15 -84.46(14) . . . . ? O1 P1 O3 C34 -55.57(14) . . . . ? O2 P1 O3 C34 46.55(14) . . . . ? Pd1 P1 O3 C34 -176.91(11) . . . . ? P1 Pd1 C1 C2 9.19(15) . . . . ? Cl1 Pd1 C1 C2 -172.29(15) . . . . ? Cl2 Pd1 C1 C2 18.2(5) . . . . ? P1 Pd1 C1 C6 -166.7(2) . . . . ? Cl1 Pd1 C1 C6 11.8(2) . . . . ? Cl2 Pd1 C1 C6 -157.7(2) . . . . ? C6 C1 C2 C3 -6.1(3) . . . . ? Pd1 C1 C2 C3 177.53(16) . . . . ? C6 C1 C2 O1 172.14(19) . . . . ? Pd1 C1 C2 O1 -4.2(2) . . . . ? P1 O1 C2 C3 172.33(15) . . . . ? P1 O1 C2 C1 -6.1(2) . . . . ? C1 C2 C3 C4 6.2(3) . . . . ? O1 C2 C3 C4 -172.04(19) . . . . ? C1 C2 C3 C7 -174.6(2) . . . . ? O1 C2 C3 C7 7.1(3) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C7 C3 C4 C5 -179.3(2) . . . . ? C3 C4 C5 C6 -5.4(4) . . . . ? C3 C4 C5 C11A 166.6(4) . . . . ? C3 C4 C5 C11B -168.2(12) . . . . ? C2 C1 C6 O4 -178.7(2) . . . . ? Pd1 C1 C6 O4 -2.8(4) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? Pd1 C1 C6 C5 175.8(2) . . . . ? C4 C5 C6 O4 -175.9(2) . . . . ? C11A C5 C6 O4 12.3(5) . . . . ? C11B C5 C6 O4 -12.8(13) . . . . ? C4 C5 C6 C1 5.5(4) . . . . ? C11A C5 C6 C1 -166.4(4) . . . . ? C11B C5 C6 C1 168.6(13) . . . . ? C2 C3 C7 C10 176.4(2) . . . . ? C4 C3 C7 C10 -4.5(3) . . . . ? C2 C3 C7 C8 57.5(3) . . . . ? C4 C3 C7 C8 -123.5(2) . . . . ? C2 C3 C7 C9 -64.8(3) . . . . ? C4 C3 C7 C9 114.2(2) . . . . ? C4 C5 C11A C12A 5.8(7) . . . . ? C6 C5 C11A C12A 177.5(4) . . . . ? C11B C5 C11A C12A -93(3) . . . . ? C4 C5 C11A C13A 125.0(5) . . . . ? C6 C5 C11A C13A -63.3(5) . . . . ? C11B C5 C11A C13A 26(3) . . . . ? C4 C5 C11A C14A -112.7(5) . . . . ? C6 C5 C11A C14A 59.0(6) . . . . ? C11B C5 C11A C14A 148(3) . . . . ? C4 C5 C11B C13B 106.5(18) . . . . ? C6 C5 C11B C13B -56(2) . . . . ? C11A C5 C11B C13B -160(4) . . . . ? C4 C5 C11B C14B -130.4(10) . . . . ? C6 C5 C11B C14B 67.0(13) . . . . ? C11A C5 C11B C14B -37(2) . . . . ? C4 C5 C11B C12B -3(2) . . . . ? C6 C5 C11B C12B -165.4(17) . . . . ? C11A C5 C11B C12B 91(3) . . . . ? P1 O2 C15 C24 -70.4(2) . . . . ? P1 O2 C15 C16 114.38(18) . . . . ? C24 C15 C16 C17 5.0(3) . . . . ? O2 C15 C16 C17 179.79(19) . . . . ? C24 C15 C16 Si1 -173.19(17) . . . . ? O2 C15 C16 Si1 1.6(3) . . . . ? C36 Si1 C16 C17 -58.2(2) . . . . ? C37 Si1 C16 C17 -178.6(2) . . . . ? C35 Si1 C16 C17 58.9(2) . . . . ? C36 Si1 C16 C15 119.9(2) . . . . ? C37 Si1 C16 C15 -0.5(3) . . . . ? C35 Si1 C16 C15 -122.9(2) . . . . ? C15 C16 C17 C18 2.3(4) . . . . ? Si1 C16 C17 C18 -179.3(2) . . . . ? C16 C17 C18 C19 175.1(3) . . . . ? C16 C17 C18 C23 -4.6(4) . . . . ? C17 C18 C19 C20 -178.5(3) . . . . ? C23 C18 C19 C20 1.3(4) . . . . ? C18 C19 C20 C21 0.5(5) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? C20 C21 C22 C23 1.1(4) . . . . ? C21 C22 C23 C18 0.7(4) . . . . ? C21 C22 C23 C24 178.5(2) . . . . ? C17 C18 C23 C22 177.9(2) . . . . ? C19 C18 C23 C22 -1.8(4) . . . . ? C17 C18 C23 C24 0.0(4) . . . . ? C19 C18 C23 C24 -179.8(2) . . . . ? O2 C15 C24 C23 175.83(18) . . . . ? C16 C15 C24 C23 -9.4(3) . . . . ? O2 C15 C24 C25 -3.7(3) . . . . ? C16 C15 C24 C25 171.1(2) . . . . ? C22 C23 C24 C15 -171.3(2) . . . . ? C18 C23 C24 C15 6.5(3) . . . . ? C22 C23 C24 C25 8.2(3) . . . . ? C18 C23 C24 C25 -174.0(2) . . . . ? C15 C24 C25 C34 54.4(3) . . . . ? C23 C24 C25 C34 -125.1(2) . . . . ? C15 C24 C25 C26 -124.0(2) . . . . ? C23 C24 C25 C26 56.6(3) . . . . ? C34 C25 C26 C27 -172.7(2) . . . . ? C24 C25 C26 C27 5.7(3) . . . . ? C34 C25 C26 C31 4.9(3) . . . . ? C24 C25 C26 C31 -176.7(2) . . . . ? C31 C26 C27 C28 1.2(3) . . . . ? C25 C26 C27 C28 178.8(2) . . . . ? C26 C27 C28 C29 0.7(3) . . . . ? C27 C28 C29 C30 -1.2(3) . . . . ? C28 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C32 -178.6(2) . . . . ? C29 C30 C31 C26 2.1(3) . . . . ? C27 C26 C31 C30 -2.6(3) . . . . ? C25 C26 C31 C30 179.7(2) . . . . ? C27 C26 C31 C32 178.1(2) . . . . ? C25 C26 C31 C32 0.4(3) . . . . ? C30 C31 C32 C33 177.91(19) . . . . ? C26 C31 C32 C33 -2.7(3) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C31 C32 C33 Si2 167.83(16) . . . . ? C39 Si2 C33 C32 20.4(2) . . . . ? C40 Si2 C33 C32 141.36(17) . . . . ? C38 Si2 C33 C32 -98.18(18) . . . . ? C39 Si2 C33 C34 -172.43(17) . . . . ? C40 Si2 C33 C34 -51.5(2) . . . . ? C38 Si2 C33 C34 68.95(19) . . . . ? C26 C25 C34 O3 174.94(19) . . . . ? C24 C25 C34 O3 -3.5(3) . . . . ? C26 C25 C34 C33 -8.7(3) . . . . ? C24 C25 C34 C33 172.91(19) . . . . ? P1 O3 C34 C25 -71.0(2) . . . . ? P1 O3 C34 C33 112.21(17) . . . . ? C32 C33 C34 C25 6.4(3) . . . . ? Si2 C33 C34 C25 -161.31(18) . . . . ? C32 C33 C34 O3 -177.17(17) . . . . ? Si2 C33 C34 O3 15.1(2) . . . . ? C43 N1 C41 C42 178.9(3) . . . . ? C45 N1 C41 C42 51.7(4) . . . . ? C41 N1 C45 C46 59.5(5) . . . . ? C43 N1 C45 C46 -67.9(4) . . . . ? C41 N1 C43 C44 63.7(4) . . . . ? C45 N1 C43 C44 -167.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.60 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.558 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.061