# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2140 data_codp _audit_creation_method SHELXL _chemical_name_systematic ; bis[1,3-(diphenylphosphino)propane]- [eta-3-(1-methoxy-2-cicloocten-1-yl]-palladium(II) exafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety '([(CH2)3 (P(C6H5)2)2] (C9 H15 O) Pd 1+ ) (P F6 1-)' _chemical_formula_structural '[(P(Ph)2)-(CH2)3-(P(Ph)2) (C8 H12 (O C H3)) Pd] (P F6)' _chemical_formula_analytical ? _chemical_formula_sum 'C36 H41 F6 O P3 Pd' _chemical_formula_weight 803.00 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pd' 'Pd' -0.9988 1.0072 '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' 'F' 'F' 0.0171 0.0103 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 10.716(2) _cell_length_b 18.008(2) _cell_length_c 18.978(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.01(1) _cell_angle_gamma 90.00 _cell_volume 3626.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 16.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method ? _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 300 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.022 _diffrn_standards_decay_corr_min 0.943 _diffrn_reflns_number 8741 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.05 _reflns_number_total 8213 _reflns_number_observed 4692 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CELDIM (Enraf-Nonius)' _computing_data_reduction 'WinGX 1.63 (Farrugia, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8213 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_obs 0.0490 _refine_ls_wR_factor_all 0.1389 _refine_ls_wR_factor_obs 0.1256 _refine_ls_goodness_of_fit_all 0.975 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_restrained_S_all 0.975 _refine_ls_restrained_S_obs 1.189 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.22889(3) 0.25958(2) 0.41182(2) 0.04861(12) Uani 1 d . . P1 P 0.11998(10) 0.36309(6) 0.43745(6) 0.0495(3) Uani 1 d . . P2 P 0.39118(11) 0.32534(7) 0.37292(6) 0.0548(3) Uani 1 d . . O1 O 0.3996(4) 0.1028(2) 0.3833(2) 0.0827(10) Uani 1 d . . C1 C 0.1912(5) 0.1416(2) 0.4006(3) 0.0633(12) Uani 1 d . . H1 H 0.1609(5) 0.1269(2) 0.3544(3) 0.076 Uiso 1 calc R . C2 C 0.1050(5) 0.1736(3) 0.4410(3) 0.0713(14) Uani 1 d . . H2 H 0.0405(5) 0.2018(3) 0.4163(3) 0.086 Uiso 1 calc R . C3 C 0.1060(6) 0.1671(3) 0.5196(3) 0.093(2) Uani 1 d . . H3A H 0.0326(6) 0.1927(3) 0.5322(3) 0.112 Uiso 1 calc R . H3B H 0.1800(6) 0.1926(3) 0.5432(3) 0.112 Uiso 1 calc R . C4 C 0.1063(8) 0.0884(4) 0.5486(4) 0.117(3) Uani 1 d . . H4A H 0.1163(8) 0.0913(4) 0.6001(4) 0.141 Uiso 1 calc R . H4B H 0.0241(8) 0.0667(4) 0.5331(4) 0.141 Uiso 1 calc R . C5 C 0.2038(8) 0.0365(4) 0.5284(4) 0.123(3) Uani 1 d . . H5A H 0.1967(8) -0.0093(4) 0.5545(4) 0.147 Uiso 1 calc R . H5B H 0.1808(8) 0.0250(4) 0.4784(4) 0.147 Uiso 1 calc R . C6 C 0.3393(7) 0.0577(4) 0.5388(4) 0.106(2) Uani 1 d . . H6A H 0.3870(7) 0.0165(4) 0.5232(4) 0.127 Uiso 1 calc R . H6B H 0.3661(7) 0.0640(4) 0.5894(4) 0.127 Uiso 1 calc R . C7 C 0.3747(5) 0.1280(3) 0.5007(3) 0.082(2) Uani 1 d . . H7A H 0.3475(5) 0.1711(3) 0.5251(3) 0.098 Uiso 1 calc R . H7B H 0.4656(5) 0.1304(3) 0.5033(3) 0.098 Uiso 1 calc R . C8 C 0.3165(5) 0.1304(3) 0.4241(3) 0.0623(12) Uani 1 d . . C9 C 0.3637(7) 0.0989(4) 0.3086(3) 0.107(2) Uani 1 d . . H9A H 0.4319(19) 0.0787(26) 0.2868(4) 0.161 Uiso 1 calc R . H9B H 0.3440(45) 0.1478(5) 0.2903(5) 0.161 Uiso 1 calc R . H9C H 0.2910(29) 0.0676(22) 0.2982(3) 0.161 Uiso 1 calc R . C10 C 0.4315(4) 0.4095(3) 0.4242(3) 0.0653(13) Uani 1 d . . H10A H 0.4612(4) 0.3959(3) 0.4731(3) 0.078 Uiso 1 calc R . H10B H 0.4999(4) 0.4344(3) 0.4054(3) 0.078 Uiso 1 calc R . C11 C 0.3212(5) 0.4636(3) 0.4231(3) 0.0657(13) Uani 1 d . . H11A H 0.2801(5) 0.4686(3) 0.3745(3) 0.079 Uiso 1 calc R . H11B H 0.3541(5) 0.5119(3) 0.4387(3) 0.079 Uiso 1 calc R . C12 C 0.2227(4) 0.4403(2) 0.4700(3) 0.0595(11) Uani 1 d . . H12A H 0.1701(4) 0.4831(2) 0.4761(3) 0.071 Uiso 1 calc R . H12B H 0.2663(4) 0.4272(2) 0.5165(3) 0.071 Uiso 1 calc R . C13 C 0.0118(4) 0.3978(3) 0.3625(2) 0.0572(11) Uani 1 d . . C14 C -0.0319(6) 0.3506(3) 0.3087(3) 0.082(2) Uani 1 d . . H14 H 0.0014(6) 0.3030(3) 0.3077(3) 0.098 Uiso 1 calc R . C15 C -0.1264(7) 0.3734(4) 0.2551(3) 0.110(2) Uani 1 d . . H15 H -0.1585(7) 0.3402(4) 0.2195(3) 0.132 Uiso 1 calc R . C16 C -0.1713(7) 0.4430(4) 0.2546(4) 0.109(2) Uani 1 d . . H16 H -0.2331(7) 0.4584(4) 0.2182(4) 0.130 Uiso 1 calc R . C17 C -0.1259(6) 0.4914(4) 0.3079(3) 0.097(2) Uani 1 d . . H17 H -0.1569(6) 0.5397(4) 0.3075(3) 0.116 Uiso 1 calc R . C18 C -0.0353(6) 0.4690(3) 0.3613(3) 0.079(2) Uani 1 d . . H18 H -0.0052(6) 0.5021(3) 0.3973(3) 0.095 Uiso 1 calc R . C19 C 0.0218(4) 0.3546(2) 0.5078(2) 0.0518(10) Uani 1 d . . C20 C -0.1079(5) 0.3577(3) 0.4956(3) 0.0702(13) Uani 1 d . . H20 H -0.1496(5) 0.3654(3) 0.4498(3) 0.084 Uiso 1 calc R . C21 C -0.1755(6) 0.3492(3) 0.5522(3) 0.086(2) Uani 1 d . . H21 H -0.2630(6) 0.3523(3) 0.5438(3) 0.103 Uiso 1 calc R . C22 C -0.1190(7) 0.3365(4) 0.6184(4) 0.099(2) Uani 1 d . . H22 H -0.1665(7) 0.3303(4) 0.6554(4) 0.119 Uiso 1 calc R . C23 C 0.0084(7) 0.3329(4) 0.6308(3) 0.091(2) Uani 1 d . . H23 H 0.0484(7) 0.3244(4) 0.6768(3) 0.109 Uiso 1 calc R . C24 C 0.0796(5) 0.3417(3) 0.5759(3) 0.0720(13) Uani 1 d . . H24 H 0.1670(5) 0.3388(3) 0.5852(3) 0.086 Uiso 1 calc R . C25 C 0.3552(5) 0.3570(3) 0.2824(2) 0.0614(12) Uani 1 d . . C26 C 0.2595(6) 0.3240(3) 0.2382(3) 0.0795(15) Uani 1 d . . H26 H 0.2134(6) 0.2860(3) 0.2555(3) 0.095 Uiso 1 calc R . C27 C 0.2302(7) 0.3464(4) 0.1680(3) 0.107(2) Uani 1 d . . H27 H 0.1678(7) 0.3218(4) 0.1378(3) 0.128 Uiso 1 calc R . C28 C 0.2921(9) 0.4039(4) 0.1433(4) 0.122(3) Uani 1 d . . H28 H 0.2692(9) 0.4205(4) 0.0969(4) 0.147 Uiso 1 calc R . C29 C 0.3887(8) 0.4383(4) 0.1863(4) 0.109(2) Uani 1 d . . H29 H 0.4325(8) 0.4772(4) 0.1687(4) 0.131 Uiso 1 calc R . C30 C 0.4206(6) 0.4150(3) 0.2555(3) 0.085(2) Uani 1 d . . H30 H 0.4862(6) 0.4381(3) 0.2846(3) 0.102 Uiso 1 calc R . C31 C 0.5388(4) 0.2748(3) 0.3774(3) 0.0635(12) Uani 1 d . . C32 C 0.5909(6) 0.2557(4) 0.3178(4) 0.100(2) Uani 1 d . . H32 H 0.5573(6) 0.2741(4) 0.2735(4) 0.120 Uiso 1 calc R . C33 C 0.6955(7) 0.2080(5) 0.3246(5) 0.120(3) Uani 1 d . . H33 H 0.7302(7) 0.1946(5) 0.2842(5) 0.144 Uiso 1 calc R . C34 C 0.7464(6) 0.1815(4) 0.3880(6) 0.113(3) Uani 1 d . . H34 H 0.8150(6) 0.1494(4) 0.3912(6) 0.136 Uiso 1 calc R . C35 C 0.6991(6) 0.2009(4) 0.4462(5) 0.115(2) Uani 1 d . . H35 H 0.7360(6) 0.1835(4) 0.4904(5) 0.138 Uiso 1 calc R . C36 C 0.5938(5) 0.2475(3) 0.4413(4) 0.089(2) Uani 1 d . . H36 H 0.5607(5) 0.2601(3) 0.4825(4) 0.106 Uiso 1 calc R . P3 P -0.02441(12) 0.14262(9) 0.17424(8) 0.0753(4) Uani 1 d . . F1 F 0.0289(6) 0.2001(3) 0.2263(4) 0.224(4) Uani 1 d . . F2 F 0.0982(5) 0.0977(4) 0.1876(4) 0.204(3) Uani 1 d . . F3 F -0.0795(6) 0.0773(4) 0.1290(4) 0.221(3) Uani 1 d . . F4 F -0.1493(5) 0.1785(5) 0.1695(4) 0.247(4) Uani 1 d . . F5 F -0.0564(9) 0.1017(6) 0.2403(5) 0.278(4) Uani 1 d . . F6 F 0.0061(12) 0.1763(6) 0.1118(4) 0.335(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0479(2) 0.0494(2) 0.0500(2) -0.0017(2) 0.01202(13) -0.0008(2) P1 0.0521(6) 0.0509(6) 0.0466(6) -0.0033(5) 0.0110(5) 0.0023(5) P2 0.0530(6) 0.0589(7) 0.0554(7) -0.0059(5) 0.0177(5) -0.0059(5) O1 0.087(3) 0.086(3) 0.081(3) -0.005(2) 0.032(2) 0.012(2) C1 0.076(3) 0.050(3) 0.062(3) -0.005(2) 0.003(2) -0.010(2) C2 0.060(3) 0.056(3) 0.102(4) 0.005(3) 0.023(3) -0.005(2) C3 0.114(5) 0.071(3) 0.109(5) 0.012(3) 0.066(4) 0.001(3) C4 0.152(7) 0.094(5) 0.123(6) 0.011(4) 0.080(5) -0.015(5) C5 0.167(8) 0.069(4) 0.144(7) 0.034(4) 0.063(6) 0.001(5) C6 0.126(6) 0.098(5) 0.097(5) 0.032(4) 0.030(4) 0.024(4) C7 0.083(4) 0.092(4) 0.068(3) 0.007(3) 0.005(3) -0.003(3) C8 0.066(3) 0.065(3) 0.058(3) -0.003(2) 0.017(2) -0.001(2) C9 0.135(6) 0.119(5) 0.079(4) -0.017(4) 0.052(4) 0.003(4) C10 0.064(3) 0.068(3) 0.068(3) -0.014(2) 0.023(2) -0.015(2) C11 0.075(3) 0.052(3) 0.074(3) -0.013(2) 0.025(3) -0.012(2) C12 0.067(3) 0.054(3) 0.060(3) -0.012(2) 0.021(2) -0.006(2) C13 0.061(3) 0.064(3) 0.047(2) 0.003(2) 0.010(2) 0.006(2) C14 0.104(4) 0.072(3) 0.064(3) -0.015(3) -0.008(3) 0.021(3) C15 0.130(6) 0.115(6) 0.073(4) -0.021(4) -0.024(4) 0.024(5) C16 0.125(6) 0.107(5) 0.084(4) 0.007(4) -0.024(4) 0.034(4) C17 0.118(5) 0.085(4) 0.082(4) -0.002(3) -0.008(4) 0.031(4) C18 0.097(4) 0.068(3) 0.067(3) -0.010(3) -0.007(3) 0.023(3) C19 0.052(2) 0.054(2) 0.050(2) -0.003(2) 0.011(2) 0.002(2) C20 0.063(3) 0.075(3) 0.075(3) -0.005(3) 0.018(3) -0.005(2) C21 0.075(4) 0.101(4) 0.088(4) -0.014(3) 0.039(3) -0.015(3) C22 0.129(6) 0.101(5) 0.079(4) -0.016(4) 0.054(4) -0.030(4) C23 0.113(5) 0.115(5) 0.045(3) 0.004(3) 0.015(3) -0.017(4) C24 0.072(3) 0.087(4) 0.058(3) 0.002(3) 0.014(2) -0.003(3) C25 0.072(3) 0.061(3) 0.056(3) -0.005(2) 0.028(2) -0.001(2) C26 0.098(4) 0.086(4) 0.055(3) 0.008(3) 0.014(3) -0.015(3) C27 0.134(6) 0.120(5) 0.062(4) 0.000(4) -0.001(4) -0.029(5) C28 0.206(9) 0.107(6) 0.059(4) 0.019(4) 0.039(5) -0.001(6) C29 0.173(8) 0.079(4) 0.086(5) 0.008(4) 0.053(5) -0.015(4) C30 0.111(5) 0.080(4) 0.069(4) 0.000(3) 0.034(3) -0.022(3) C31 0.050(3) 0.067(3) 0.075(3) -0.017(2) 0.013(2) -0.005(2) C32 0.080(4) 0.126(6) 0.096(5) -0.023(4) 0.023(3) 0.020(4) C33 0.074(4) 0.144(7) 0.148(8) -0.048(6) 0.037(5) 0.011(4) C34 0.054(4) 0.104(5) 0.177(9) -0.021(6) -0.004(5) 0.012(3) C35 0.070(4) 0.109(6) 0.156(8) 0.009(5) -0.016(5) 0.009(4) C36 0.062(3) 0.098(4) 0.103(5) 0.003(4) 0.003(3) -0.003(3) P3 0.0547(7) 0.0931(10) 0.0791(10) -0.0314(8) 0.0128(7) -0.0026(7) F1 0.195(6) 0.162(5) 0.287(8) -0.139(6) -0.063(5) 0.002(4) F2 0.118(4) 0.231(7) 0.256(7) -0.057(6) 0.003(4) 0.063(4) F3 0.218(6) 0.182(6) 0.235(7) -0.099(5) -0.063(6) -0.009(5) F4 0.115(4) 0.386(11) 0.222(7) -0.099(7) -0.043(4) 0.127(6) F5 0.321(10) 0.306(11) 0.235(8) 0.068(8) 0.139(8) -0.009(9) F6 0.580(17) 0.277(10) 0.196(7) 0.092(7) 0.219(10) -0.003(11) _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 Pd C2 2.162(5) . ? Pd C1 2.168(4) . ? Pd P1 2.2874(11) . ? Pd P2 2.3086(12) . ? Pd C8 2.507(5) . ? P1 C13 1.816(5) . ? P1 C19 1.817(4) . ? P1 C12 1.827(4) . ? P2 C25 1.801(5) . ? P2 C31 1.817(5) . ? P2 C10 1.820(5) . ? O1 C8 1.354(6) . ? O1 C9 1.417(7) . ? C1 C8 1.370(7) . ? C1 C2 1.403(7) . ? C2 C3 1.496(8) . ? C3 C4 1.519(8) . ? C4 C5 1.490(9) . ? C5 C6 1.487(9) . ? C6 C7 1.532(8) . ? C7 C8 1.500(7) . ? C10 C11 1.529(7) . ? C11 C12 1.530(6) . ? C13 C14 1.361(7) . ? C13 C18 1.377(7) . ? C14 C15 1.393(8) . ? C15 C16 1.343(9) . ? C16 C17 1.371(9) . ? C17 C18 1.364(7) . ? C19 C24 1.374(6) . ? C19 C20 1.378(6) . ? C20 C21 1.385(7) . ? C21 C22 1.336(9) . ? C22 C23 1.354(9) . ? C23 C24 1.383(7) . ? C25 C26 1.367(7) . ? C25 C30 1.393(7) . ? C26 C27 1.386(8) . ? C27 C28 1.349(9) . ? C28 C29 1.372(10) . ? C29 C30 1.376(8) . ? C31 C36 1.364(8) . ? C31 C32 1.373(8) . ? C32 C33 1.403(10) . ? C33 C34 1.338(10) . ? C34 C35 1.325(11) . ? C35 C36 1.399(9) . ? P3 F6 1.410(6) . ? P3 F4 1.477(5) . ? P3 F1 1.489(4) . ? P3 F3 1.526(5) . ? P3 F5 1.533(7) . ? P3 F2 1.534(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd C1 37.8(2) . . ? C2 Pd P1 100.35(14) . . ? C1 Pd P1 136.55(14) . . ? C2 Pd P2 165.10(14) . . ? C1 Pd P2 127.58(14) . . ? P1 Pd P2 94.55(4) . . ? C2 Pd C8 63.1(2) . . ? C1 Pd C8 33.1(2) . . ? P1 Pd C8 158.73(11) . . ? P2 Pd C8 102.52(11) . . ? C13 P1 C19 103.5(2) . . ? C13 P1 C12 106.9(2) . . ? C19 P1 C12 101.5(2) . . ? C13 P1 Pd 113.8(2) . . ? C19 P1 Pd 116.91(14) . . ? C12 P1 Pd 113.0(2) . . ? C25 P2 C31 105.8(2) . . ? C25 P2 C10 104.5(2) . . ? C31 P2 C10 104.6(2) . . ? C25 P2 Pd 113.4(2) . . ? C31 P2 Pd 114.7(2) . . ? C10 P2 Pd 112.9(2) . . ? C8 O1 C9 118.8(4) . . ? C8 C1 C2 124.9(5) . . ? C8 C1 Pd 87.2(3) . . ? C2 C1 Pd 70.9(3) . . ? C1 C2 C3 126.8(5) . . ? C1 C2 Pd 71.3(3) . . ? C3 C2 Pd 113.1(4) . . ? C2 C3 C4 115.7(5) . . ? C5 C4 C3 117.2(5) . . ? C6 C5 C4 120.8(7) . . ? C5 C6 C7 116.8(5) . . ? C8 C7 C6 112.6(5) . . ? O1 C8 C1 124.1(5) . . ? O1 C8 C7 109.0(4) . . ? C1 C8 C7 125.2(5) . . ? O1 C8 Pd 123.7(3) . . ? C1 C8 Pd 59.7(2) . . ? C7 C8 Pd 102.5(3) . . ? C11 C10 P2 113.4(3) . . ? C10 C11 C12 114.4(4) . . ? C11 C12 P1 116.4(3) . . ? C14 C13 C18 118.8(5) . . ? C14 C13 P1 119.2(4) . . ? C18 C13 P1 121.7(4) . . ? C13 C14 C15 120.2(5) . . ? C16 C15 C14 120.2(6) . . ? C15 C16 C17 119.9(6) . . ? C18 C17 C16 120.2(6) . . ? C17 C18 C13 120.6(5) . . ? C24 C19 C20 118.4(4) . . ? C24 C19 P1 118.4(3) . . ? C20 C19 P1 123.2(4) . . ? C19 C20 C21 119.4(5) . . ? C22 C21 C20 122.0(6) . . ? C21 C22 C23 119.1(6) . . ? C22 C23 C24 120.8(6) . . ? C19 C24 C23 120.3(5) . . ? C26 C25 C30 118.4(5) . . ? C26 C25 P2 119.3(4) . . ? C30 C25 P2 122.3(4) . . ? C25 C26 C27 120.8(5) . . ? C28 C27 C26 120.1(6) . . ? C27 C28 C29 120.4(6) . . ? C28 C29 C30 119.7(6) . . ? C29 C30 C25 120.5(6) . . ? C36 C31 C32 117.8(5) . . ? C36 C31 P2 119.2(4) . . ? C32 C31 P2 122.5(5) . . ? C31 C32 C33 119.3(7) . . ? C34 C33 C32 121.4(7) . . ? C35 C34 C33 120.0(7) . . ? C34 C35 C36 120.1(8) . . ? C31 C36 C35 121.3(7) . . ? F6 P3 F4 94.3(6) . . ? F6 P3 F1 98.5(6) . . ? F4 P3 F1 89.8(4) . . ? F6 P3 F3 88.5(5) . . ? F4 P3 F3 91.6(4) . . ? F1 P3 F3 172.8(5) . . ? F6 P3 F5 176.7(6) . . ? F4 P3 F5 87.5(5) . . ? F1 P3 F5 84.3(5) . . ? F3 P3 F5 88.7(5) . . ? F6 P3 F2 94.1(6) . . ? F4 P3 F2 171.3(5) . . ? F1 P3 F2 90.9(3) . . ? F3 P3 F2 86.7(4) . . ? F5 P3 F2 84.0(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 C2 Pd P1 C13 -91.7(2) . . . . ? C1 Pd P1 C13 -78.8(3) . . . . ? P2 Pd P1 C13 88.0(2) . . . . ? C8 Pd P1 C13 -128.5(4) . . . . ? C2 Pd P1 C19 28.8(2) . . . . ? C1 Pd P1 C19 41.7(3) . . . . ? P2 Pd P1 C19 -151.5(2) . . . . ? C8 Pd P1 C19 -8.0(4) . . . . ? C2 Pd P1 C12 146.1(2) . . . . ? C1 Pd P1 C12 159.0(3) . . . . ? P2 Pd P1 C12 -34.2(2) . . . . ? C8 Pd P1 C12 109.3(4) . . . . ? C2 Pd P2 C25 97.3(6) . . . . ? C1 Pd P2 C25 87.0(2) . . . . ? P1 Pd P2 C25 -81.5(2) . . . . ? C8 Pd P2 C25 111.2(2) . . . . ? C2 Pd P2 C31 -24.4(7) . . . . ? C1 Pd P2 C31 -34.7(3) . . . . ? P1 Pd P2 C31 156.7(2) . . . . ? C8 Pd P2 C31 -10.5(2) . . . . ? C2 Pd P2 C10 -144.1(7) . . . . ? C1 Pd P2 C10 -154.4(3) . . . . ? P1 Pd P2 C10 37.0(2) . . . . ? C8 Pd P2 C10 -130.2(2) . . . . ? C2 Pd C1 C8 -128.6(5) . . . . ? P1 Pd C1 C8 -149.5(2) . . . . ? P2 Pd C1 C8 47.1(3) . . . . ? C8 Pd C1 C8 0.0 . . . . ? C2 Pd C1 C2 0.0 . . . . ? P1 Pd C1 C2 -21.0(4) . . . . ? P2 Pd C1 C2 175.7(3) . . . . ? C8 Pd C1 C2 128.6(5) . . . . ? C8 C1 C2 C3 -33.1(8) . . . . ? Pd C1 C2 C3 -105.3(5) . . . . ? C8 C1 C2 Pd 72.2(5) . . . . ? Pd C1 C2 Pd 0.0 . . . . ? C1 Pd C2 C1 0.0 . . . . ? P1 Pd C2 C1 165.5(3) . . . . ? P2 Pd C2 C1 -13.3(8) . . . . ? C8 Pd C2 C1 -28.6(3) . . . . ? C1 Pd C2 C3 122.9(5) . . . . ? P1 Pd C2 C3 -71.6(4) . . . . ? P2 Pd C2 C3 109.5(6) . . . . ? C8 Pd C2 C3 94.3(4) . . . . ? C1 C2 C3 C4 -55.1(8) . . . . ? Pd C2 C3 C4 -138.5(5) . . . . ? C2 C3 C4 C5 51.7(10) . . . . ? C3 C4 C5 C6 51.8(11) . . . . ? C4 C5 C6 C7 -58.7(9) . . . . ? C5 C6 C7 C8 -47.2(8) . . . . ? C9 O1 C8 C1 13.5(8) . . . . ? C9 O1 C8 C7 179.3(5) . . . . ? C9 O1 C8 Pd -60.3(6) . . . . ? C2 C1 C8 O1 -176.6(5) . . . . ? Pd C1 C8 O1 -112.4(5) . . . . ? C2 C1 C8 C7 19.8(8) . . . . ? Pd C1 C8 C7 84.1(5) . . . . ? C2 C1 C8 Pd -64.2(4) . . . . ? Pd C1 C8 Pd 0.0 . . . . ? C6 C7 C8 O1 -94.4(6) . . . . ? C6 C7 C8 C1 71.2(7) . . . . ? C6 C7 C8 Pd 132.9(4) . . . . ? C2 Pd C8 O1 145.5(5) . . . . ? C1 Pd C8 O1 113.0(5) . . . . ? P1 Pd C8 O1 -173.1(2) . . . . ? P2 Pd C8 O1 -30.5(4) . . . . ? C2 Pd C8 C1 32.5(3) . . . . ? C1 Pd C8 C1 0.0 . . . . ? P1 Pd C8 C1 73.9(5) . . . . ? P2 Pd C8 C1 -143.5(3) . . . . ? C2 Pd C8 C7 -91.1(4) . . . . ? C1 Pd C8 C7 -123.6(5) . . . . ? P1 Pd C8 C7 -49.7(5) . . . . ? P2 Pd C8 C7 92.9(3) . . . . ? C25 P2 C10 C11 65.0(4) . . . . ? C31 P2 C10 C11 176.0(4) . . . . ? Pd P2 C10 C11 -58.7(4) . . . . ? P2 C10 C11 C12 75.3(5) . . . . ? C10 C11 C12 P1 -73.2(5) . . . . ? C13 P1 C12 C11 -72.2(4) . . . . ? C19 P1 C12 C11 179.7(4) . . . . ? Pd P1 C12 C11 53.7(4) . . . . ? C19 P1 C13 C14 -104.4(4) . . . . ? C12 P1 C13 C14 149.0(4) . . . . ? Pd P1 C13 C14 23.5(5) . . . . ? C19 P1 C13 C18 70.1(5) . . . . ? C12 P1 C13 C18 -36.5(5) . . . . ? Pd P1 C13 C18 -162.0(4) . . . . ? C18 C13 C14 C15 -2.6(9) . . . . ? P1 C13 C14 C15 172.1(5) . . . . ? C13 C14 C15 C16 2.7(11) . . . . ? C14 C15 C16 C17 -1.4(12) . . . . ? C15 C16 C17 C18 0.0(12) . . . . ? C16 C17 C18 C13 0.2(11) . . . . ? C14 C13 C18 C17 1.1(9) . . . . ? P1 C13 C18 C17 -173.4(5) . . . . ? C13 P1 C19 C24 -168.9(4) . . . . ? C12 P1 C19 C24 -58.2(4) . . . . ? Pd P1 C19 C24 65.2(4) . . . . ? C13 P1 C19 C20 13.7(4) . . . . ? C12 P1 C19 C20 124.4(4) . . . . ? Pd P1 C19 C20 -112.2(4) . . . . ? C24 C19 C20 C21 1.3(7) . . . . ? P1 C19 C20 C21 178.7(4) . . . . ? C19 C20 C21 C22 -1.4(9) . . . . ? C20 C21 C22 C23 0.9(10) . . . . ? C21 C22 C23 C24 -0.4(10) . . . . ? C20 C19 C24 C23 -0.8(8) . . . . ? P1 C19 C24 C23 -178.3(4) . . . . ? C22 C23 C24 C19 0.3(9) . . . . ? C31 P2 C25 C26 107.4(4) . . . . ? C10 P2 C25 C26 -142.5(4) . . . . ? Pd P2 C25 C26 -19.1(5) . . . . ? C31 P2 C25 C30 -73.4(5) . . . . ? C10 P2 C25 C30 36.7(5) . . . . ? Pd P2 C25 C30 160.0(4) . . . . ? C30 C25 C26 C27 1.5(9) . . . . ? P2 C25 C26 C27 -179.3(5) . . . . ? C25 C26 C27 C28 -3.4(11) . . . . ? C26 C27 C28 C29 3.3(12) . . . . ? C27 C28 C29 C30 -1.6(12) . . . . ? C28 C29 C30 C25 -0.2(10) . . . . ? C26 C25 C30 C29 0.2(8) . . . . ? P2 C25 C30 C29 -178.9(5) . . . . ? C25 P2 C31 C36 176.3(4) . . . . ? C10 P2 C31 C36 66.3(5) . . . . ? Pd P2 C31 C36 -57.9(5) . . . . ? C25 P2 C31 C32 -11.0(5) . . . . ? C10 P2 C31 C32 -121.0(5) . . . . ? Pd P2 C31 C32 114.8(5) . . . . ? C36 C31 C32 C33 1.5(9) . . . . ? P2 C31 C32 C33 -171.3(5) . . . . ? C31 C32 C33 C34 -0.8(12) . . . . ? C32 C33 C34 C35 -0.9(13) . . . . ? C33 C34 C35 C36 1.7(12) . . . . ? C32 C31 C36 C35 -0.7(9) . . . . ? P2 C31 C36 C35 172.4(5) . . . . ? C34 C35 C36 C31 -1.0(11) . . . . ? _refine_diff_density_max 0.620 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.076