Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Steyer, Stephane' ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513 Universite Louis Pasteur, 1 rue Blaise Pascal, F67008 Strasbourg France ; 'Jeunesse, Catherine' ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513, Universite Louis Pasteur, 1 rue Blaise Pascal, F67008 Strasbourg France ; 'Matt, Dominique' ; Laboratoire de Chimie Inorganique Moleculaire, UMR CNRS 7513, Universite Louis Pasteur, 1 rue Blaise Pascal, F67008 Strasbourg France ; 'Welter, Richard' ; Laboratoire DECMET, UMR CNRS 7513 Universite Louis Pasteur, 4 rue Blaise Pascal Strasbourg France ; 'Wesolek, Marcel' ; Laboratoire de catalyse, Universite Louis Pasteur, UMR 7513 CNRS, 4 rue Blaise Pascal, F-67008 Strasbourg Cedex France. ; _publ_contact_author_name ; Prof Dominique Matt ; _publ_contact_author_address ; Laboratoire de Chimie Inorganique Moleculaire, Universite Louis Pasteur, UMR 7513, 1 rue Blaise Pascal, F67008 Strasbourg cedex France ; _publ_contact_author_phone '+33 390241719' _publ_contact_author_fax '+33 390241719' _publ_contact_author_email dmatt@chimie.u-strasbg.fr _publ_requested_journal 'J. Chem. Soc, Dalton Trans' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in J. Chem. Soc, Dalton Trans. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Heterofunctionalized phosphites built on a caliz[4] arene scaffold and their use in 1-octene hydroformylation. Formation of 12-membered P, O-chelate rings ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; data_st564 _database_code_CSD 184801 _audit_creation_date 19-04-02 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C124 H145 Cl2 N5 O11 P4 Pt' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C124 H145 Cl2 N5 O11 P4 Pt' _chemical_formula_weight 2271.46 _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 C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pt ? -2.352 8.388 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 16.3979(1) _cell_length_b 17.5637(1) _cell_length_c 24.1629(1) _cell_angle_alpha 71.905(6) _cell_angle_beta 84.340(6) _cell_angle_gamma 65.213(6) _cell_volume 6001.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 37630 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9530 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 17630 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 0.3 deg 1 scans of 50 sec per frame. Data collection was divided into 3 set(s) with the following starting angles and number of frames : Set 1 Theta = 6.40 Omega = 0.00 Kappa = 0.00 610 frames Set 2 Theta = -1.70 Kappa = -168.00 Phi = 0.00 162 frames Set 3 Theta = -3.70 Kappa = 0.00 Phi = 0.00 150 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 37630 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.53 _reflns_number_total 27279 _reflns_number_gt 22183 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 22183 _refine_ls_number_parameters 1256 _refine_ls_number_restraints 0 _refine_ls_number_constraints 18 _refine_ls_R_factor_all 0.077 _refine_ls_R_factor_gt 0.060 _refine_ls_wR_factor_all 0.624 _refine_ls_wR_factor_ref 0.075 _refine_ls_goodness_of_fit_all 9.793 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/esd_mean 0.010 _refine_diff_density_max 1.341 _refine_diff_density_min -0.102 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PT 0.14193(1) 0.47028(1) 0.16510(1) 0.02541(7) Uani ? ? Pt CL1 0.0600(1) 0.44807(9) 0.10206(6) 0.0430(6) Uani ? ? Cl CL2 0.1689(1) 0.57363(9) 0.08637(6) 0.0518(7) Uani ? ? Cl P1 0.20936(9) 0.50583(8) 0.22200(5) 0.0265(5) Uani ? ? P O1 0.1713(2) 0.4936(2) 0.2851(1) 0.029(1) Uani ? ? O O2 0.3152(2) 0.4456(2) 0.2275(2) 0.031(2) Uani ? ? O O3 0.2021(2) 0.6039(2) 0.2048(2) 0.029(1) Uani ? ? O C1 0.1091(4) 0.5275(3) 0.3729(2) 0.036(2) Uani ? ? C C2 0.1183(4) 0.5139(4) 0.4324(2) 0.043(2) Uani ? ? C C3 0.1971(4) 0.4565(4) 0.4654(2) 0.046(3) Uani ? ? C C4 0.2694(4) 0.4116(4) 0.4358(2) 0.042(2) Uani ? ? C C5 0.2649(4) 0.4227(3) 0.3761(2) 0.034(2) Uani ? ? C C6 0.1851(3) 0.4835(3) 0.3449(2) 0.032(2) Uani ? ? C C7 0.2026(5) 0.4365(5) 0.5316(3) 0.055(3) Uani ? ? C C8 0.2974(7) 0.413(1) 0.5522(4) 0.136(6) Uani ? ? C C9 0.1800(7) 0.3558(6) 0.5594(3) 0.064(5) Uani ? ? C C10 0.1332(8) 0.5107(5) 0.5529(3) 0.081(5) Uani ? ? C C11 0.3466(4) 0.3680(3) 0.3488(2) 0.035(2) Uani ? ? C C12 0.3951(4) 0.4226(3) 0.3137(2) 0.033(2) Uani ? ? C C13 0.4563(4) 0.4387(3) 0.3395(3) 0.037(2) Uani ? ? C C14 0.4978(4) 0.4926(4) 0.3081(3) 0.042(3) Uani ? ? C C15 0.4765(4) 0.5307(4) 0.2479(3) 0.040(3) Uani ? ? C C16 0.4152(4) 0.5164(4) 0.2202(3) 0.034(2) Uani ? ? C C17 0.3760(3) 0.4627(3) 0.2549(2) 0.030(2) Uani ? ? C C18 0.5666(4) 0.5091(4) 0.3364(3) 0.053(3) Uani ? ? C C19 0.5644(6) 0.4786(6) 0.4028(4) 0.108(5) Uani ? ? C C20 0.6613(5) 0.4561(6) 0.3188(5) 0.079(5) Uani ? ? C C21 0.5487(5) 0.6063(4) 0.3152(4) 0.076(4) Uani ? ? C C22 0.3898(4) 0.5586(4) 0.1565(3) 0.039(3) Uani ? ? C C23 0.3121(3) 0.6498(3) 0.1420(2) 0.033(2) Uani ? ? C C24 0.3298(4) 0.7198(4) 0.1050(3) 0.039(2) Uani ? ? C C25 0.2640(4) 0.8045(3) 0.0843(2) 0.038(2) Uani ? ? C C26 0.1756(4) 0.8163(3) 0.0995(2) 0.033(2) Uani ? ? C C27 0.1537(3) 0.7491(3) 0.1359(2) 0.032(2) Uani ? ? C C28 0.2243(3) 0.6660(3) 0.1591(2) 0.031(2) Uani ? ? C C29 0.2855(4) 0.8820(3) 0.0470(3) 0.044(2) Uani ? ? C C30 0.3827(5) 0.8532(4) 0.0289(4) 0.070(4) Uani ? ? C C31 0.2683(5) 0.9459(4) 0.0828(3) 0.065(3) Uani ? ? C C32 0.2239(5) 0.9319(5) -0.0076(4) 0.077(4) Uani ? ? C C33 0.0560(4) 0.7664(3) 0.1459(2) 0.034(2) Uani ? ? C C34 0.0304(3) 0.7612(3) 0.2083(2) 0.033(2) Uani ? ? C C35 0.0302(4) 0.8226(4) 0.2335(3) 0.040(3) Uani ? ? C C36 0.0178(4) 0.8135(4) 0.2932(3) 0.047(3) Uani ? ? C C37 0.0122(4) 0.7358(4) 0.3275(3) 0.044(3) Uani ? ? C C38 0.0124(4) 0.6721(3) 0.3040(2) 0.035(2) Uani ? ? C C39 0.0142(3) 0.6897(3) 0.2440(2) 0.030(2) Uani ? ? C C40 0.0117(5) 0.8852(4) 0.3194(3) 0.064(3) Uani ? ? C C41 0.028(1) 0.8514(6) 0.3842(4) 0.138(6) Uani ? ? C C42 0.0743(8) 0.9269(6) 0.2893(6) 0.254(6) Uani ? ? C C43 -0.0830(8) 0.9550(6) 0.3082(5) 0.108(6) Uani ? ? C O4 0.0110(2) 0.6274(2) 0.2202(2) 0.030(1) Uani ? ? O C44 -0.0708(3) 0.6508(3) 0.1902(2) 0.033(2) Uani ? ? C P2 -0.17456(9) 0.6806(1) 0.23184(6) 0.0341(6) Uani ? ? P O5 -0.1668(3) 0.6213(3) 0.2918(2) 0.047(2) Uani ? ? O C45 -0.2528(4) 0.6779(4) 0.1851(3) 0.038(3) Uani ? ? C C46 -0.2563(5) 0.5967(5) 0.1953(3) 0.059(3) Uani ? ? C C47 -0.3141(5) 0.5876(5) 0.1617(4) 0.076(4) Uani ? ? C C48 -0.3694(5) 0.6615(5) 0.1184(3) 0.070(4) Uani ? ? C C49 -0.3655(6) 0.7392(6) 0.1087(4) 0.072(4) Uani ? ? C C50 -0.3068(5) 0.7479(5) 0.1417(3) 0.061(4) Uani ? ? C C51 -0.2122(4) 0.7951(4) 0.2289(3) 0.043(3) Uani ? ? C C52 -0.2566(6) 0.8194(5) 0.2772(3) 0.064(4) Uani ? ? C C53 -0.2889(7) 0.9077(6) 0.2770(4) 0.094(5) Uani ? ? C C54 -0.2768(7) 0.9687(6) 0.2301(4) 0.092(5) Uani ? ? C C55 -0.2337(6) 0.9462(5) 0.1827(5) 0.076(4) Uani ? ? C C56 -0.2014(5) 0.8591(4) 0.1818(4) 0.057(4) Uani ? ? C C57 0.0175(4) 0.5840(4) 0.3427(2) 0.037(2) Uani ? ? C P3 0.12110(8) 0.36340(8) 0.23496(5) 0.0248(5) Uani ? ? P O6 0.1977(2) 0.3165(2) 0.2846(1) 0.028(1) Uani ? ? O O7 0.0274(2) 0.4038(2) 0.2643(1) 0.028(1) Uani ? ? O O8 0.1192(2) 0.2828(2) 0.2188(1) 0.029(1) Uani ? ? O C58 0.3110(3) 0.1920(3) 0.3508(2) 0.030(2) Uani ? ? C C59 0.2229(3) 0.2567(3) 0.3420(2) 0.027(2) Uani ? ? C C60 0.1675(3) 0.2693(3) 0.3888(2) 0.031(2) Uani ? ? C C61 0.1980(4) 0.2088(4) 0.4440(2) 0.036(2) Uani ? ? C C62 0.2821(4) 0.1395(4) 0.4544(2) 0.037(2) Uani ? ? C C63 0.3388(4) 0.1341(4) 0.4068(2) 0.035(2) Uani ? ? C C64 0.3160(5) 0.0728(5) 0.5156(3) 0.046(3) Uani ? ? C C65 0.3830(7) 0.0958(7) 0.5398(4) 0.082(5) Uani ? ? C C66 0.3613(8) -0.0200(6) 0.5112(4) 0.071(5) Uani ? ? C C67 0.2391(6) 0.0789(7) 0.5572(4) 0.068(5) Uani ? ? C C68 0.0753(4) 0.3440(3) 0.3837(2) 0.032(2) Uani ? ? C C69 0.0060(3) 0.3238(3) 0.3621(2) 0.028(2) Uani ? ? C C70 -0.0353(4) 0.2730(3) 0.3984(2) 0.033(2) Uani ? ? C C71 -0.0940(4) 0.2486(3) 0.3775(2) 0.033(2) Uani ? ? C C72 -0.1112(4) 0.2775(3) 0.3174(3) 0.036(2) Uani ? ? C C73 -0.0708(3) 0.3292(3) 0.2786(2) 0.030(2) Uani ? ? C C74 -0.0130(3) 0.3504(3) 0.3023(2) 0.027(2) Uani ? ? C C75 -0.1350(4) 0.1893(4) 0.4202(3) 0.045(3) Uani ? ? C C76 -0.0609(7) 0.0999(6) 0.4469(6) 0.089(6) Uani ? ? C C77 -0.2056(6) 0.1782(5) 0.3904(5) 0.086(5) Uani ? ? C C78 -0.1831(6) 0.2308(6) 0.4669(4) 0.092(5) Uani ? ? C C79 -0.0859(4) 0.3577(3) 0.2136(2) 0.033(2) Uani ? ? C C80 -0.0230(3) 0.2896(3) 0.1856(2) 0.031(2) Uani ? ? C C81 -0.0618(4) 0.2534(3) 0.1575(2) 0.034(2) Uani ? ? C C82 -0.0129(4) 0.1935(3) 0.1271(2) 0.036(2) Uani ? ? C C83 0.0781(4) 0.1749(3) 0.1223(2) 0.036(2) Uani ? ? C C84 0.1214(4) 0.2094(3) 0.1489(2) 0.030(2) Uani ? ? C C85 0.0705(3) 0.2630(3) 0.1833(2) 0.029(2) Uani ? ? C C86 -0.0602(4) 0.1568(4) 0.0970(3) 0.046(3) Uani ? ? C C87 -0.0993(5) 0.2229(5) 0.0384(3) 0.080(4) Uani ? ? C C88 -0.1379(5) 0.1426(5) 0.1334(4) 0.085(4) Uani ? ? C C89 0.0035(6) 0.0697(5) 0.0885(5) 0.100(4) Uani ? ? C C90 0.2183(4) 0.1940(3) 0.1333(2) 0.036(2) Uani ? ? C C91 0.2856(4) 0.1389(3) 0.1840(2) 0.033(2) Uani ? ? C C92 0.3124(4) 0.0487(3) 0.2063(3) 0.041(2) Uani ? ? C C93 0.3688(4) -0.0018(4) 0.2560(3) 0.040(3) Uani ? ? C C94 0.3912(4) 0.0435(4) 0.2860(2) 0.037(3) Uani ? ? C C95 0.3656(4) 0.1342(3) 0.2652(2) 0.033(2) Uani ? ? C C96 0.3196(4) 0.1793(3) 0.2118(2) 0.031(2) Uani ? ? C C97 0.4041(5) -0.1032(4) 0.2771(3) 0.047(3) Uani ? ? C C98 0.3324(8) -0.1307(6) 0.290(1) 0.108(9) Uani ? ? C C99 0.4714(8) -0.1446(6) 0.3271(7) 0.097(7) Uani ? ? C C100 0.464(1) -0.1394(6) 0.2295(5) 0.104(8) Uani ? ? C O9 0.2992(3) 0.2689(2) 0.1882(2) 0.034(2) Uani ? ? O C101 0.3585(6) 0.2949(4) 0.1510(4) 0.075(4) Uani ? ? C P4 0.4656(1) 0.2251(1) 0.1426(1) 0.077(1) Uani ? ? P O10 0.5188(5) 0.1889(5) 0.1998(3) 0.102(4) Uani ? ? O C102 0.4661(5) 0.1449(5) 0.1101(4) 0.118(4) Uani ? ? C C103 0.4130(5) 0.1607(5) 0.0630(4) 0.072(4) Uani ? ? C C104 0.4184(5) 0.0899(6) 0.0466(3) 0.075(4) Uani ? ? C C105 0.4819(6) 0.0060(5) 0.0775(4) 0.105(4) Uani ? ? C C106 0.5347(8) 0.0000(9) 0.1217(5) 0.097(7) Uani ? ? C C107 0.5231(7) 0.0692(8) 0.1364(5) 0.119(6) Uani ? ? C C108 0.5251(8) 0.2896(9) 0.0902(8) 0.071(2) Uiso ? ? C C109 0.4651(8) 0.3445(9) 0.0362(8) 0.094(3) Uiso ? ? C C110 0.4977(8) 0.4014(9) -0.0112(8) 0.102(4) Uiso ? ? C C111 0.5937(8) 0.3852(9) 0.0019(8) 0.090(3) Uiso ? ? C C112 0.6272(8) 0.3139(9) 0.0603(8) 0.151(6) Uiso ? ? C C113 0.5903(8) 0.2805(9) 0.0947(8) 0.133(5) Uiso ? ? C C114 0.3793(4) 0.1828(3) 0.3025(2) 0.032(2) Uani ? ? C C115 0.1427(5) 0.1033(4) 0.3252(4) 0.060(4) Uani ? ? C C116 0.1759(6) 0.0289(5) 0.3778(4) 0.087(5) Uani ? ? C N1 0.2023(7) -0.0300(7) 0.4185(5) 0.138(7) Uani ? ? N C117 0.1523(8) 0.5343(8) -0.0502(6) 0.114(4) Uiso ? ? C C118 0.2084(9) 0.4521(8) -0.0192(6) 0.119(4) Uiso ? ? C N2 0.257(1) 0.370(1) 0.0090(7) 0.187(6) Uiso ? ? N C119 0.085(1) 0.3302(6) 0.9830(5) 0.095(7) Uani ? ? C C120 0.1324(7) 0.2443(6) 0.9735(4) 0.069(5) Uani ? ? C N3 0.1674(8) 0.1783(5) 0.9659(4) 0.099(6) Uani ? ? N C121 0.2598(6) 0.6617(5) 0.3086(4) 0.078(4) Uani ? ? C C122 0.2781(8) 0.6494(7) 0.3677(6) 0.114(7) Uani ? ? C N4 0.294(1) 0.638(1) 0.4157(6) 0.19(1) Uani ? ? N C123 0.398(1) 0.722(1) 0.4609(7) 0.17(1) Uani ? ? C C124 0.4471(8) 0.7382(7) 0.4969(6) 0.109(8) Uani ? ? C N5 0.4825(9) 0.7501(7) 0.5296(8) 0.19(1) Uani ? ? N O11 0.369(1) 0.710(1) -0.2411(8) 0.279(9) Uiso ? ? O H1 0.0679 0.5456 0.4515 0.0544 Uiso calc C2 H H2 0.3242 0.3716 0.4571 0.0539 Uiso calc C4 H H3 0.2995 0.4006 0.5933 0.2368 Uiso calc C8 H H4 0.3382 0.3623 0.5418 0.2368 Uiso calc C8 H H5 0.3137 0.4605 0.5342 0.2368 Uiso calc C8 H H6 0.1829 0.3417 0.6007 0.1105 Uiso calc C9 H H7 0.1212 0.3690 0.5469 0.1105 Uiso calc C9 H H8 0.2222 0.3071 0.5478 0.1105 Uiso calc C9 H H9 0.1392 0.4953 0.5941 0.1286 Uiso calc C10 H H10 0.1424 0.5629 0.5355 0.1286 Uiso calc C10 H H11 0.0745 0.5204 0.5424 0.1286 Uiso calc C10 H H12 0.3279 0.3452 0.3240 0.0466 Uiso calc C11 H H13 0.3863 0.3209 0.3788 0.0466 Uiso calc C11 H H14 0.4701 0.4118 0.3801 0.0511 Uiso calc C13 H H15 0.5046 0.5672 0.2252 0.0578 Uiso calc C15 H H16 0.6074 0.4895 0.4192 0.1285 Uiso calc C19 H H17 0.5061 0.5100 0.4148 0.1285 Uiso calc C19 H H18 0.5783 0.4175 0.4159 0.1285 Uiso calc C19 H H19 0.7043 0.4658 0.3360 0.1203 Uiso calc C20 H H20 0.6735 0.3953 0.3319 0.1203 Uiso calc C20 H H21 0.6646 0.4743 0.2776 0.1203 Uiso calc C20 H H22 0.5916 0.6154 0.3330 0.1076 Uiso calc C21 H H23 0.5533 0.6241 0.2740 0.1076 Uiso calc C21 H H24 0.4900 0.6400 0.3253 0.1076 Uiso calc C21 H H25 0.3730 0.5215 0.1432 0.0541 Uiso calc C22 H H26 0.4409 0.5639 0.1365 0.0541 Uiso calc C22 H H27 0.3898 0.7087 0.0934 0.0495 Uiso calc C24 H H28 0.1284 0.8727 0.0842 0.0451 Uiso calc C26 H H29 0.3925 0.9032 0.0061 0.0891 Uiso calc C30 H H30 0.4215 0.8247 0.0627 0.0891 Uiso calc C30 H H31 0.3948 0.8138 0.0067 0.0891 Uiso calc C30 H H32 0.2814 0.9941 0.0602 0.0755 Uiso calc C31 H H33 0.2071 0.9668 0.0931 0.0755 Uiso calc C31 H H34 0.3058 0.9161 0.1172 0.0755 Uiso calc C31 H H35 0.2380 0.9795 -0.0302 0.0977 Uiso calc C32 H H36 0.2323 0.8935 -0.0300 0.0977 Uiso calc C32 H H37 0.1631 0.9539 0.0034 0.0977 Uiso calc C32 H H38 0.0441 0.7242 0.1353 0.0464 Uiso calc C33 H H39 0.0202 0.8236 0.1218 0.0464 Uiso calc C33 H H40 0.0388 0.8727 0.2094 0.0529 Uiso calc C35 H H41 0.0080 0.7257 0.3684 0.0556 Uiso calc C37 H H42 0.0238 0.8976 0.3984 0.2215 Uiso calc C41 H H43 -0.0153 0.8298 0.4019 0.2215 Uiso calc C41 H H44 0.0866 0.8052 0.3933 0.2215 Uiso calc C41 H H45 0.0700 0.9710 0.3057 0.2493 Uiso calc C42 H H46 0.1343 0.8834 0.2941 0.2493 Uiso calc C42 H H47 0.0580 0.9527 0.2489 0.2493 Uiso calc C42 H H48 -0.0889 1.0003 0.3239 0.1430 Uiso calc C43 H H49 -0.0960 0.9789 0.2674 0.1430 Uiso calc C43 H H50 -0.1238 0.9299 0.3262 0.1430 Uiso calc C43 H H51 -0.0648 0.6022 0.1781 0.0428 Uiso calc C44 H H52 -0.0781 0.6997 0.1569 0.0428 Uiso calc C44 H H53 -0.3042 0.8033 0.1340 0.0810 Uiso calc C50 H H54 -0.4031 0.7888 0.0790 0.0974 Uiso calc C49 H H55 -0.4101 0.6566 0.0957 0.0870 Uiso calc C48 H H56 -0.3159 0.5321 0.1680 0.0930 Uiso calc C47 H H57 -0.2192 0.5474 0.2254 0.0775 Uiso calc C46 H H58 -0.2650 0.7768 0.3099 0.0913 Uiso calc C52 H H59 -0.3192 0.9246 0.3096 0.1295 Uiso calc C53 H H60 -0.2987 1.0279 0.2304 0.1261 Uiso calc C54 H H61 -0.2256 0.9894 0.1503 0.1056 Uiso calc C55 H H62 -0.1717 0.8436 0.1486 0.0768 Uiso calc C56 H H63 -0.0267 0.5932 0.3713 0.0496 Uiso calc C57 H H64 0.0060 0.5544 0.3195 0.0496 Uiso calc C57 H H65 0.1593 0.2156 0.4757 0.0494 Uiso calc C61 H H66 0.3983 0.0895 0.4131 0.0477 Uiso calc C63 H H67 0.4049 0.0559 0.5774 0.1265 Uiso calc C65 H H68 0.4318 0.0918 0.5145 0.1265 Uiso calc C65 H H69 0.3537 0.1540 0.5425 0.1265 Uiso calc C65 H H70 0.3818 -0.0603 0.5489 0.1222 Uiso calc C66 H H71 0.3196 -0.0330 0.4954 0.1222 Uiso calc C66 H H72 0.4110 -0.0250 0.4866 0.1222 Uiso calc C66 H H73 0.2618 0.0375 0.5942 0.1206 Uiso calc C67 H H74 0.2115 0.1364 0.5611 0.1206 Uiso calc C67 H H75 0.1960 0.0667 0.5422 0.1206 Uiso calc C67 H H76 0.0770 0.3961 0.3571 0.0419 Uiso calc C68 H H77 0.0593 0.3526 0.4208 0.0419 Uiso calc C68 H H78 -0.0231 0.2542 0.4392 0.0459 Uiso calc C70 H H79 -0.1512 0.2620 0.3021 0.0462 Uiso calc C72 H H80 -0.0858 0.0632 0.4732 0.1613 Uiso calc C76 H H81 -0.0320 0.0745 0.4170 0.1613 Uiso calc C76 H H82 -0.0184 0.1060 0.4672 0.1613 Uiso calc C76 H H83 -0.2289 0.1414 0.4182 0.1126 Uiso calc C77 H H84 -0.2530 0.2341 0.3742 0.1126 Uiso calc C77 H H85 -0.1787 0.1523 0.3604 0.1126 Uiso calc C77 H H86 -0.2082 0.1942 0.4931 0.1153 Uiso calc C78 H H87 -0.1416 0.2378 0.4876 0.1153 Uiso calc C78 H H88 -0.2297 0.2867 0.4494 0.1153 Uiso calc C78 H H89 -0.0772 0.4103 0.1973 0.0441 Uiso calc C79 H H90 -0.1460 0.3686 0.2055 0.0441 Uiso calc C79 H H91 -0.1250 0.2707 0.1592 0.0458 Uiso calc C81 H H92 0.1128 0.1370 0.0999 0.0466 Uiso calc C83 H H93 -0.1287 0.2008 0.0194 0.0991 Uiso calc C87 H H94 -0.1414 0.2767 0.0439 0.0991 Uiso calc C87 H H95 -0.0524 0.2324 0.0151 0.0991 Uiso calc C87 H H96 -0.1662 0.1200 0.1141 0.0975 Uiso calc C88 H H97 -0.1150 0.1020 0.1706 0.0975 Uiso calc C88 H H98 -0.1804 0.1970 0.1379 0.0975 Uiso calc C88 H H99 -0.0279 0.0491 0.0699 0.1344 Uiso calc C89 H H100 0.0513 0.0771 0.0651 0.1344 Uiso calc C89 H H101 0.0273 0.0282 0.1254 0.1344 Uiso calc C89 H H102 0.2214 0.2495 0.1185 0.0462 Uiso calc C90 H H103 0.2345 0.1652 0.1040 0.0462 Uiso calc C90 H H104 0.2916 0.0202 0.1871 0.0512 Uiso calc C92 H H105 0.4250 0.0116 0.3219 0.0525 Uiso calc C94 H H106 0.3562 -0.1930 0.3033 0.2987 Uiso calc C98 H H107 0.2983 -0.1083 0.3204 0.2987 Uiso calc C98 H H108 0.2948 -0.1090 0.2566 0.2987 Uiso calc C98 H H109 0.4911 -0.2066 0.3385 0.1835 Uiso calc C99 H H110 0.5214 -0.1300 0.3155 0.1835 Uiso calc C99 H H111 0.4443 -0.1233 0.3590 0.1835 Uiso calc C99 H H112 0.4866 -0.2017 0.2416 0.2121 Uiso calc C100 H H113 0.4296 -0.1162 0.1941 0.2121 Uiso calc C100 H H114 0.5130 -0.1224 0.2236 0.2121 Uiso calc C100 H H115 0.4383 0.1514 0.3197 0.0437 Uiso calc C114 H H116 0.3724 0.2397 0.2787 0.0437 Uiso calc C114 H H117 0.3640 0.3391 0.1631 0.1061 Uiso calc C101 H H118 0.3300 0.3201 0.1134 0.1061 Uiso calc C101 H H119 0.3737 0.2189 0.0424 0.1017 Uiso calc C103 H H120 0.3810 0.0973 0.0160 0.0931 Uiso calc C104 H H121 0.4885 -0.0450 0.0682 0.1204 Uiso calc C105 H H122 0.5800 -0.0554 0.1415 0.1514 Uiso calc C106 H H123 0.5585 0.0624 0.1678 0.1739 Uiso calc C107 H H124 0.4087 0.3429 0.0326 0.1216 Uiso calc C109 H H125 0.4631 0.4426 -0.0453 0.1329 Uiso calc C110 H H126 0.6273 0.4147 -0.0224 0.1169 Uiso calc C111 H H127 0.6892 0.2941 0.0694 0.1957 Uiso calc C112 H H128 0.6223 0.2414 0.1301 0.1727 Uiso calc C113 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PT 0.03362(8) 0.02530(6) 0.01930(7) -0.01295(5) -0.00013(6) -0.00394(5) Pt CL1 0.0672(7) 0.0400(5) 0.0296(6) -0.0290(4) -0.0146(5) -0.0013(4) Cl CL2 0.1017(9) 0.0593(6) 0.0231(6) -0.0562(5) -0.0008(6) -0.0002(5) Cl P1 0.0307(5) 0.0278(5) 0.0219(5) -0.0140(4) 0.0016(4) -0.0052(4) P O1 0.035(2) 0.032(1) 0.021(1) -0.015(1) -0.000(1) -0.006(1) O O2 0.031(2) 0.032(1) 0.030(2) -0.012(1) -0.001(1) -0.008(1) O O3 0.030(1) 0.029(1) 0.028(2) -0.014(1) 0.004(1) -0.006(1) O C1 0.043(2) 0.040(2) 0.026(2) -0.024(2) 0.003(2) -0.009(2) C C2 0.047(3) 0.058(3) 0.030(2) -0.027(2) 0.007(2) -0.020(2) C C3 0.056(3) 0.063(3) 0.028(2) -0.035(2) -0.000(2) -0.013(2) C C4 0.049(3) 0.051(2) 0.029(2) -0.027(2) -0.007(2) -0.007(2) C C5 0.041(2) 0.035(2) 0.028(2) -0.021(2) -0.002(2) -0.006(2) C C6 0.042(2) 0.038(2) 0.020(2) -0.023(1) 0.002(2) -0.008(2) C C7 0.061(4) 0.101(4) 0.027(2) -0.031(3) -0.002(2) -0.024(2) C C8 0.110(5) 0.45(1) 0.051(4) -0.157(5) 0.013(3) -0.099(4) C C9 0.110(7) 0.072(5) 0.033(3) -0.010(5) 0.007(4) -0.003(3) C C10 0.197(9) 0.079(4) 0.034(3) -0.064(4) 0.004(4) -0.022(3) C C11 0.043(3) 0.031(2) 0.034(2) -0.016(2) -0.005(2) -0.006(2) C C12 0.031(2) 0.028(2) 0.039(3) -0.009(2) -0.002(2) -0.008(2) C C13 0.037(3) 0.030(2) 0.046(3) -0.011(2) -0.008(2) -0.006(2) C C14 0.037(3) 0.033(2) 0.061(3) -0.013(2) -0.011(2) -0.010(2) C C15 0.031(2) 0.034(2) 0.062(4) -0.013(2) -0.003(3) -0.004(2) C C16 0.026(2) 0.034(2) 0.043(3) -0.010(2) 0.000(2) -0.004(2) C C17 0.025(2) 0.028(2) 0.040(3) -0.010(2) -0.002(2) -0.008(2) C C18 0.053(3) 0.034(2) 0.080(4) -0.019(2) -0.027(3) -0.001(3) C C19 0.129(4) 0.116(4) 0.083(5) -0.087(3) -0.036(4) -0.008(4) C C20 0.044(3) 0.070(4) 0.162(8) -0.018(3) -0.032(4) -0.029(4) C C21 0.082(4) 0.042(3) 0.127(6) -0.026(2) -0.045(4) -0.014(3) C C22 0.032(2) 0.044(3) 0.041(3) -0.015(2) 0.008(2) -0.005(2) C C23 0.032(2) 0.035(2) 0.031(2) -0.015(2) 0.004(2) -0.006(2) C C24 0.037(2) 0.045(2) 0.036(3) -0.023(2) 0.006(2) -0.008(2) C C25 0.043(2) 0.039(2) 0.032(2) -0.025(2) 0.006(2) -0.009(2) C C26 0.040(2) 0.029(2) 0.032(2) -0.014(2) 0.001(2) -0.005(2) C C27 0.032(2) 0.033(2) 0.030(2) -0.016(2) 0.003(2) -0.008(2) C C28 0.036(2) 0.032(2) 0.027(2) -0.019(1) 0.002(2) -0.005(2) C C29 0.051(3) 0.040(2) 0.043(3) -0.031(2) 0.008(2) -0.010(2) C C30 0.074(3) 0.057(3) 0.083(5) -0.044(2) 0.039(3) -0.018(3) C C31 0.062(3) 0.058(2) 0.075(4) -0.040(2) 0.015(3) -0.030(2) C C32 0.106(4) 0.077(3) 0.055(4) -0.068(2) -0.011(3) 0.010(3) C C33 0.035(2) 0.031(2) 0.036(3) -0.014(2) -0.002(2) -0.003(2) C C34 0.027(2) 0.034(2) 0.039(3) -0.012(2) 0.001(2) -0.010(2) C C35 0.033(2) 0.037(2) 0.052(3) -0.015(2) 0.003(2) -0.014(2) C C36 0.040(3) 0.047(2) 0.055(3) -0.017(2) 0.001(2) -0.027(2) C C37 0.041(3) 0.051(3) 0.040(3) -0.016(2) 0.005(2) -0.024(2) C C38 0.030(2) 0.041(2) 0.036(2) -0.014(2) 0.005(2) -0.015(2) C C39 0.024(2) 0.032(2) 0.033(2) -0.009(2) 0.002(2) -0.012(2) C C40 0.067(4) 0.053(3) 0.075(4) -0.025(2) 0.004(3) -0.039(2) C C41 0.32(1) 0.075(4) 0.110(5) -0.040(5) -0.095(5) -0.043(3) C C42 0.208(6) 0.263(4) 0.299(8) -0.200(3) 0.142(6) -0.235(3) C C43 0.108(8) 0.076(4) 0.153(6) -0.012(4) -0.007(6) -0.078(3) C O4 0.028(2) 0.031(1) 0.031(2) -0.012(1) 0.002(1) -0.010(1) O C44 0.034(2) 0.038(2) 0.029(2) -0.017(2) -0.000(2) -0.010(2) C P2 0.0294(6) 0.0469(6) 0.0288(6) -0.0169(4) 0.0026(5) -0.0066(5) P O5 0.044(2) 0.067(2) 0.035(2) -0.027(2) 0.001(2) 0.002(2) O C45 0.032(2) 0.048(3) 0.037(3) -0.015(2) 0.005(2) -0.010(2) C C46 0.055(3) 0.058(3) 0.066(4) -0.027(2) -0.009(3) -0.009(3) C C47 0.070(4) 0.076(3) 0.084(5) -0.039(3) -0.007(3) -0.029(3) C C48 0.060(3) 0.098(4) 0.059(4) -0.040(3) -0.001(3) -0.033(3) C C49 0.074(4) 0.080(4) 0.064(4) -0.027(3) -0.030(3) -0.009(3) C C50 0.062(4) 0.060(3) 0.059(4) -0.023(3) -0.019(3) -0.007(3) C C51 0.032(3) 0.054(3) 0.045(3) -0.009(2) -0.002(2) -0.022(2) C C52 0.059(4) 0.075(4) 0.059(3) 0.001(4) -0.007(3) -0.035(3) C C53 0.080(6) 0.108(5) 0.096(4) 0.014(4) -0.022(4) -0.077(3) C C54 0.090(6) 0.069(4) 0.124(5) 0.002(4) -0.046(4) -0.052(3) C C55 0.071(4) 0.049(3) 0.123(6) -0.017(3) -0.024(4) -0.028(3) C C56 0.056(4) 0.045(3) 0.074(4) -0.018(2) -0.001(3) -0.017(3) C C57 0.036(2) 0.050(2) 0.028(2) -0.020(2) 0.006(2) -0.009(2) C P3 0.0299(5) 0.0231(4) 0.0221(5) -0.0110(4) -0.0009(4) -0.0039(4) P O6 0.033(2) 0.028(1) 0.023(1) -0.012(1) -0.003(1) -0.003(1) O O7 0.031(2) 0.026(1) 0.027(2) -0.011(1) 0.002(1) -0.006(1) O O8 0.034(2) 0.026(1) 0.028(2) -0.012(1) -0.001(1) -0.008(1) O C58 0.034(2) 0.029(2) 0.028(2) -0.014(1) -0.001(2) -0.007(2) C C59 0.036(2) 0.025(2) 0.021(2) -0.013(1) -0.003(2) -0.003(2) C C60 0.035(2) 0.032(2) 0.027(2) -0.015(2) -0.000(2) -0.008(2) C C61 0.040(2) 0.047(2) 0.025(2) -0.019(2) 0.000(2) -0.005(2) C C62 0.040(3) 0.046(3) 0.028(2) -0.018(2) -0.006(2) -0.002(2) C C63 0.035(2) 0.035(2) 0.034(2) -0.012(2) -0.007(2) -0.005(2) C C64 0.053(4) 0.064(4) 0.030(3) -0.014(3) -0.007(3) 0.007(3) C C65 0.091(5) 0.131(7) 0.046(4) -0.040(5) -0.032(4) 0.008(5) C C66 0.109(7) 0.062(5) 0.053(5) -0.005(5) -0.006(5) 0.019(4) C C67 0.074(5) 0.101(6) 0.042(4) -0.011(5) 0.003(4) 0.024(4) C C68 0.037(2) 0.034(2) 0.026(2) -0.014(2) 0.004(2) -0.011(2) C C69 0.027(2) 0.028(2) 0.030(2) -0.009(2) 0.003(2) -0.008(2) C C70 0.036(2) 0.031(2) 0.031(2) -0.010(2) 0.004(2) -0.006(2) C C71 0.031(2) 0.031(2) 0.039(3) -0.009(2) 0.008(2) -0.006(2) C C72 0.030(2) 0.036(2) 0.043(3) -0.015(2) 0.001(2) -0.013(2) C C73 0.028(2) 0.030(2) 0.033(2) -0.010(2) 0.003(2) -0.009(2) C C74 0.027(2) 0.024(2) 0.030(2) -0.009(1) 0.004(2) -0.005(2) C C75 0.045(3) 0.040(2) 0.050(3) -0.021(2) 0.008(3) -0.002(2) C C76 0.072(5) 0.054(4) 0.18(1) -0.024(3) 0.010(6) 0.044(5) C C77 0.082(4) 0.080(4) 0.099(7) -0.056(3) 0.006(4) 0.004(4) C C78 0.097(4) 0.113(5) 0.070(5) -0.067(3) 0.041(4) -0.024(4) C C79 0.030(2) 0.035(2) 0.034(2) -0.011(2) -0.002(2) -0.010(2) C C80 0.035(2) 0.031(2) 0.028(2) -0.015(2) -0.004(2) -0.003(2) C C81 0.035(2) 0.031(2) 0.036(3) -0.013(2) -0.006(2) -0.005(2) C C82 0.045(3) 0.030(2) 0.035(2) -0.017(2) -0.008(2) -0.003(2) C C83 0.046(3) 0.031(2) 0.034(2) -0.016(2) -0.002(2) -0.012(2) C C84 0.037(2) 0.027(2) 0.026(2) -0.013(2) -0.002(2) -0.006(2) C C85 0.035(2) 0.025(2) 0.027(2) -0.013(1) -0.004(2) -0.004(2) C C86 0.049(3) 0.039(2) 0.049(3) -0.022(2) -0.008(2) -0.014(2) C C87 0.110(4) 0.093(3) 0.050(3) -0.068(2) -0.021(3) -0.009(3) C C88 0.092(4) 0.099(3) 0.068(4) -0.070(2) 0.002(3) -0.026(3) C C89 0.066(4) 0.078(3) 0.197(6) -0.020(2) -0.030(4) -0.083(3) C C90 0.039(2) 0.039(2) 0.030(2) -0.016(2) 0.000(2) -0.012(2) C C91 0.034(2) 0.035(2) 0.030(2) -0.013(2) 0.004(2) -0.013(2) C C92 0.046(3) 0.036(2) 0.040(3) -0.019(2) 0.007(2) -0.016(2) C C93 0.049(3) 0.033(2) 0.039(3) -0.015(2) 0.007(2) -0.012(2) C C94 0.047(3) 0.032(2) 0.034(3) -0.010(2) -0.003(2) -0.007(2) C C95 0.036(2) 0.032(2) 0.032(2) -0.010(2) 0.001(2) -0.010(2) C C96 0.032(2) 0.029(2) 0.031(2) -0.009(2) 0.001(2) -0.009(2) C C97 0.074(4) 0.028(2) 0.052(3) -0.017(2) -0.001(3) -0.008(2) C C98 0.076(6) 0.033(4) 0.51(3) -0.028(3) -0.02(1) 0.032(9) C C99 0.117(7) 0.031(4) 0.25(1) -0.013(4) -0.090(7) -0.002(6) C C100 0.29(2) 0.040(4) 0.099(7) -0.015(8) 0.051(9) -0.023(4) C O9 0.039(2) 0.026(1) 0.040(2) -0.009(1) -0.006(2) -0.006(1) O C101 0.109(4) 0.041(3) 0.094(4) -0.037(3) 0.073(3) -0.032(3) C P4 0.071(1) 0.083(1) 0.077(1) -0.0320(9) 0.006(1) -0.027(1) P O10 0.107(4) 0.125(5) 0.080(4) -0.050(3) -0.017(3) -0.012(4) O C102 0.074(4) 0.154(4) 0.144(4) -0.074(3) 0.065(3) -0.125(3) C C103 0.054(3) 0.061(4) 0.112(5) -0.022(3) 0.047(3) -0.031(4) C C104 0.064(3) 0.118(4) 0.055(4) -0.057(3) 0.022(3) -0.033(3) C C105 0.119(5) 0.088(3) 0.111(5) -0.064(3) 0.068(4) -0.070(3) C C106 0.071(6) 0.139(9) 0.093(6) 0.005(6) 0.012(5) -0.043(6) C C107 0.050(5) 0.233(8) 0.144(6) -0.028(5) 0.018(5) -0.139(4) C C114 0.032(2) 0.034(2) 0.032(2) -0.009(2) -0.002(2) -0.010(2) C C115 0.072(4) 0.043(3) 0.067(4) -0.030(2) 0.002(3) -0.009(3) C C116 0.092(4) 0.089(4) 0.081(6) -0.063(3) -0.002(4) -0.006(4) C N1 0.161(7) 0.147(6) 0.111(7) -0.097(4) -0.040(6) 0.048(6) N C119 0.17(1) 0.049(4) 0.105(8) -0.027(5) -0.002(8) -0.011(5) C C120 0.117(6) 0.060(4) 0.046(4) -0.031(4) -0.002(4) 0.005(3) C N3 0.191(9) 0.067(4) 0.076(5) -0.038(5) 0.038(5) -0.021(4) N C121 0.066(4) 0.073(4) 0.100(5) -0.025(3) 0.002(4) -0.041(3) C C122 0.107(7) 0.100(6) 0.137(9) -0.045(5) 0.006(7) -0.048(5) C N4 0.24(1) 0.21(1) 0.128(8) -0.074(9) -0.021(9) -0.068(7) N C123 0.21(1) 0.23(1) 0.099(9) -0.153(7) 0.013(8) -0.011(9) C C124 0.115(8) 0.091(6) 0.13(1) -0.045(5) 0.002(7) -0.001(7) C N5 0.24(1) 0.086(6) 0.33(2) -0.074(6) -0.176(9) 0.060(8) N # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT CL1 2.342(1) . . ? PT CL2 2.339(1) . . ? PT P1 2.217(1) . . ? PT P3 2.224(1) . . ? P1 O1 1.575(4) . . ? P1 O2 1.603(4) . . ? P1 O3 1.595(4) . . ? O1 C6 1.430(6) . . ? O2 C17 1.423(7) . . ? O3 C28 1.432(6) . . ? C1 C2 1.395(8) . . ? C1 C6 1.398(8) . . ? C1 C57 1.514(9) . . ? C2 C3 1.391(9) . . ? C3 C4 1.39(1) . . ? C3 C7 1.531(8) . . ? C4 C5 1.400(8) . . ? C5 C6 1.394(8) . . ? C5 C11 1.513(9) . . ? C7 C8 1.52(1) . . ? C7 C9 1.55(1) . . ? C7 C10 1.52(1) . . ? C11 C12 1.508(8) . . ? C12 C13 1.396(8) . . ? C12 C17 1.376(8) . . ? C13 C14 1.388(9) . . ? C14 C15 1.41(1) . . ? C14 C18 1.540(9) . . ? C15 C16 1.402(9) . . ? C16 C17 1.385(8) . . ? C16 C22 1.500(9) . . ? C18 C19 1.53(1) . . ? C18 C20 1.54(1) . . ? C18 C21 1.53(1) . . ? C22 C23 1.530(8) . . ? C23 C24 1.400(8) . . ? C23 C28 1.391(8) . . ? C24 C25 1.389(9) . . ? C25 C26 1.404(8) . . ? C25 C29 1.538(8) . . ? C26 C27 1.394(8) . . ? C27 C28 1.409(8) . . ? C27 C33 1.510(8) . . ? C29 C30 1.52(1) . . ? C29 C31 1.54(1) . . ? C29 C32 1.53(1) . . ? C33 C34 1.510(8) . . ? C34 C35 1.394(9) . . ? C34 C39 1.397(8) . . ? C35 C36 1.404(9) . . ? C36 C37 1.39(1) . . ? C36 C40 1.542(9) . . ? C37 C38 1.402(9) . . ? C38 C39 1.385(8) . . ? C38 C57 1.511(8) . . ? C39 O4 1.406(7) . . ? C40 C41 1.50(1) . . ? C40 C42 1.51(2) . . ? C40 C43 1.51(1) . . ? O4 C44 1.428(7) . . ? C44 P2 1.850(6) . . ? P2 O5 1.479(4) . . ? P2 C45 1.816(7) . . ? P2 C51 1.819(7) . . ? C45 C46 1.39(1) . . ? C45 C50 1.37(1) . . ? C46 C47 1.39(1) . . ? C47 C48 1.40(1) . . ? C48 C49 1.34(1) . . ? C49 C50 1.39(1) . . ? C51 C52 1.40(1) . . ? C51 C56 1.39(1) . . ? C52 C53 1.41(1) . . ? C53 C54 1.36(2) . . ? C54 C55 1.36(2) . . ? C55 C56 1.40(1) . . ? P3 O6 1.585(4) . . ? P3 O7 1.597(4) . . ? P3 O8 1.594(4) . . ? O6 C59 1.428(6) . . ? O7 C74 1.423(6) . . ? O8 C85 1.430(6) . . ? C58 C59 1.399(8) . . ? C58 C63 1.398(8) . . ? C58 C114 1.533(8) . . ? C59 C60 1.392(8) . . ? C60 C61 1.402(8) . . ? C60 C68 1.515(8) . . ? C61 C62 1.385(9) . . ? C62 C63 1.406(9) . . ? C62 C64 1.551(8) . . ? C64 C65 1.54(1) . . ? C64 C66 1.52(1) . . ? C64 C67 1.52(1) . . ? C68 C69 1.504(8) . . ? C69 C70 1.387(8) . . ? C69 C74 1.396(7) . . ? C70 C71 1.394(9) . . ? C71 C72 1.396(8) . . ? C71 C75 1.546(8) . . ? C72 C73 1.413(8) . . ? C73 C74 1.379(8) . . ? C73 C79 1.504(8) . . ? C75 C76 1.51(1) . . ? C75 C77 1.53(1) . . ? C75 C78 1.51(1) . . ? C79 C80 1.512(8) . . ? C80 C81 1.401(8) . . ? C80 C85 1.403(8) . . ? C81 C82 1.396(9) . . ? C82 C83 1.388(9) . . ? C82 C86 1.539(8) . . ? C83 C84 1.406(8) . . ? C84 C85 1.402(8) . . ? C84 C90 1.526(8) . . ? C86 C87 1.52(1) . . ? C86 C88 1.54(1) . . ? C86 C89 1.51(1) . . ? C90 C91 1.513(8) . . ? C91 C92 1.387(8) . . ? C91 C96 1.402(8) . . ? C92 C93 1.397(9) . . ? C93 C94 1.398(9) . . ? C93 C97 1.548(9) . . ? C94 C95 1.396(8) . . ? C95 C96 1.386(8) . . ? C95 C114 1.507(8) . . ? C96 O9 1.397(7) . . ? C97 C98 1.42(1) . . ? C97 C99 1.50(1) . . ? C97 C100 1.55(1) . . ? O9 C101 1.381(8) . . ? C101 P4 1.705(9) . . ? P4 O10 1.517(7) . . ? P4 C102 1.809(9) . . ? P4 C108 1.905(17) . . ? C102 C103 1.39(2) . . ? C102 C107 1.26(2) . . ? C103 C104 1.39(1) . . ? C104 C105 1.41(2) . . ? C105 C106 1.39(2) . . ? C106 C107 1.30(2) . . ? C108 C109 1.51(2) . . ? C108 C112 1.92(2) . . ? C108 C113 1.02(2) . . ? C109 C110 1.49(2) . . ? C110 C111 1.53(2) . . ? C111 C112 1.53(3) . . ? C112 C113 1.14(2) . . ? C115 C116 1.46(1) . . ? C116 N1 1.14(1) . . ? C117 C118 1.36(2) . . ? C118 N2 1.30(2) . . ? C119 C120 1.46(1) . . ? C120 N3 1.12(1) . . ? C121 C122 1.42(2) . . ? C122 N4 1.15(2) . . ? C123 C124 1.40(2) . . ? C124 N5 1.14(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 PT CL2 89.39(6) . . . ? CL1 PT P1 174.04(6) . . . ? CL1 PT P3 87.32(5) . . . ? CL2 PT P1 87.54(5) . . . ? CL2 PT P3 174.65(6) . . . ? P1 PT P3 96.11(5) . . . ? O1 P1 O2 108.3(2) . . . ? O1 P1 O3 101.9(2) . . . ? O2 P1 O3 104.5(2) . . . ? P1 O1 C6 147.1(4) . . . ? P1 O2 C17 121.7(3) . . . ? P1 O3 C28 140.8(4) . . . ? C2 C1 C6 117.5(6) . . . ? C2 C1 C57 119.1(5) . . . ? C6 C1 C57 123.3(5) . . . ? C1 C2 C3 123.6(6) . . . ? C2 C3 C4 116.3(5) . . . ? C2 C3 C7 122.4(6) . . . ? C4 C3 C7 121.1(6) . . . ? C3 C4 C5 122.9(6) . . . ? C4 C5 C6 118.1(6) . . . ? C4 C5 C11 118.4(5) . . . ? C6 C5 C11 123.5(5) . . . ? O1 C6 C1 115.8(5) . . . ? O1 C6 C5 122.0(5) . . . ? C1 C6 C5 121.3(5) . . . ? C3 C7 C8 110.7(7) . . . ? C3 C7 C9 107.4(6) . . . ? C3 C7 C10 112.6(7) . . . ? C8 C7 C9 108(1) . . . ? C8 C7 C10 111(1) . . . ? C9 C7 C10 106.2(7) . . . ? C5 C11 C12 110.9(5) . . . ? C11 C12 C13 122.0(5) . . . ? C11 C12 C17 120.3(5) . . . ? C13 C12 C17 117.6(5) . . . ? C12 C13 C14 122.5(6) . . . ? C13 C14 C15 117.2(6) . . . ? C13 C14 C18 122.5(6) . . . ? C15 C14 C18 120.3(6) . . . ? C14 C15 C16 122.2(6) . . . ? C15 C16 C17 116.8(6) . . . ? C15 C16 C22 122.8(6) . . . ? C17 C16 C22 120.4(6) . . . ? O2 C17 C12 118.5(5) . . . ? O2 C17 C16 117.8(5) . . . ? C12 C17 C16 123.7(6) . . . ? C14 C18 C19 111.2(7) . . . ? C14 C18 C20 108.7(7) . . . ? C14 C18 C21 110.5(6) . . . ? C19 C18 C20 107.9(8) . . . ? C19 C18 C21 109.9(8) . . . ? C20 C18 C21 108.6(8) . . . ? C16 C22 C23 114.3(5) . . . ? C22 C23 C24 117.0(5) . . . ? C22 C23 C28 124.3(5) . . . ? C24 C23 C28 118.5(5) . . . ? C23 C24 C25 123.2(5) . . . ? C24 C25 C26 116.2(5) . . . ? C24 C25 C29 122.6(5) . . . ? C26 C25 C29 121.2(6) . . . ? C25 C26 C27 123.1(5) . . . ? C26 C27 C28 118.0(5) . . . ? C26 C27 C33 119.0(5) . . . ? C28 C27 C33 122.9(5) . . . ? O3 C28 C23 122.6(5) . . . ? O3 C28 C27 116.4(5) . . . ? C23 C28 C27 120.7(5) . . . ? C25 C29 C30 112.7(6) . . . ? C25 C29 C31 108.7(5) . . . ? C25 C29 C32 110.5(5) . . . ? C30 C29 C31 108.0(6) . . . ? C30 C29 C32 108.9(7) . . . ? C31 C29 C32 107.9(7) . . . ? C27 C33 C34 113.3(5) . . . ? C33 C34 C35 121.3(5) . . . ? C33 C34 C39 120.5(5) . . . ? C35 C34 C39 117.9(5) . . . ? C34 C35 C36 122.6(6) . . . ? C35 C36 C37 116.5(6) . . . ? C35 C36 C40 121.7(6) . . . ? C37 C36 C40 121.8(6) . . . ? C36 C37 C38 122.7(6) . . . ? C37 C38 C39 118.0(6) . . . ? C37 C38 C57 121.4(5) . . . ? C39 C38 C57 120.5(5) . . . ? C34 C39 C38 121.4(5) . . . ? C34 C39 O4 120.1(5) . . . ? C38 C39 O4 118.1(5) . . . ? C36 C40 C41 112.4(7) . . . ? C36 C40 C42 110.2(7) . . . ? C36 C40 C43 107.5(7) . . . ? C41 C40 C42 111(1) . . . ? C41 C40 C43 106(1) . . . ? C42 C40 C43 108(1) . . . ? C39 O4 C44 116.5(4) . . . ? O4 C44 P2 116.5(4) . . . ? C44 P2 O5 114.8(3) . . . ? C44 P2 C45 100.9(3) . . . ? C44 P2 C51 107.8(3) . . . ? O5 P2 C45 112.9(3) . . . ? O5 P2 C51 113.2(3) . . . ? C45 P2 C51 106.2(3) . . . ? P2 C45 C46 115.9(5) . . . ? P2 C45 C50 125.2(6) . . . ? C46 C45 C50 118.9(7) . . . ? C45 C46 C47 120.3(7) . . . ? C46 C47 C48 118.8(8) . . . ? C47 C48 C49 120.5(8) . . . ? C48 C49 C50 120.6(8) . . . ? C45 C50 C49 120.8(8) . . . ? P2 C51 C52 117.0(6) . . . ? P2 C51 C56 124.3(5) . . . ? C52 C51 C56 118.7(7) . . . ? C51 C52 C53 119(1) . . . ? C52 C53 C54 120.2(9) . . . ? C53 C54 C55 121(1) . . . ? C54 C55 C56 119(1) . . . ? C51 C56 C55 120.7(9) . . . ? C1 C57 C38 111.6(5) . . . ? O6 P3 O7 107.7(2) . . . ? O6 P3 O8 102.7(2) . . . ? O7 P3 O8 105.3(2) . . . ? P3 O6 C59 143.8(4) . . . ? P3 O7 C74 122.5(3) . . . ? P3 O8 C85 141.5(3) . . . ? C59 C58 C63 118.2(5) . . . ? C59 C58 C114 123.4(5) . . . ? C63 C58 C114 118.3(5) . . . ? O6 C59 C58 116.7(5) . . . ? O6 C59 C60 121.8(5) . . . ? C58 C59 C60 120.9(5) . . . ? C59 C60 C61 118.3(5) . . . ? C59 C60 C68 124.0(5) . . . ? C61 C60 C68 117.7(5) . . . ? C60 C61 C62 122.9(5) . . . ? C61 C62 C63 116.6(5) . . . ? C61 C62 C64 122.9(6) . . . ? C63 C62 C64 120.4(6) . . . ? C58 C63 C62 122.5(5) . . . ? C62 C64 C65 107.6(7) . . . ? C62 C64 C66 110.2(6) . . . ? C62 C64 C67 111.4(6) . . . ? C65 C64 C66 110.3(8) . . . ? C65 C64 C67 108.4(8) . . . ? C66 C64 C67 109.0(8) . . . ? C60 C68 C69 110.8(5) . . . ? C68 C69 C70 123.0(5) . . . ? C68 C69 C74 119.2(5) . . . ? C70 C69 C74 117.5(5) . . . ? C69 C70 C71 122.7(5) . . . ? C70 C71 C72 117.5(5) . . . ? C70 C71 C75 119.9(5) . . . ? C72 C71 C75 122.5(6) . . . ? C71 C72 C73 121.9(5) . . . ? C72 C73 C74 117.4(5) . . . ? C72 C73 C79 122.3(5) . . . ? C74 C73 C79 120.2(5) . . . ? O7 C74 C69 118.4(5) . . . ? O7 C74 C73 118.6(5) . . . ? C69 C74 C73 122.9(5) . . . ? C71 C75 C76 109.1(6) . . . ? C71 C75 C77 112.3(6) . . . ? C71 C75 C78 109.7(6) . . . ? C76 C75 C77 109.0(8) . . . ? C76 C75 C78 110.6(9) . . . ? C77 C75 C78 106.0(7) . . . ? C73 C79 C80 112.9(5) . . . ? C79 C80 C81 117.1(5) . . . ? C79 C80 C85 125.1(5) . . . ? C81 C80 C85 117.8(5) . . . ? C80 C81 C82 123.7(6) . . . ? C81 C82 C83 116.1(5) . . . ? C81 C82 C86 120.8(6) . . . ? C83 C82 C86 122.9(6) . . . ? C82 C83 C84 123.2(5) . . . ? C83 C84 C85 118.2(5) . . . ? C83 C84 C90 117.7(5) . . . ? C85 C84 C90 123.8(5) . . . ? O8 C85 C80 122.5(5) . . . ? O8 C85 C84 116.8(5) . . . ? C80 C85 C84 120.6(5) . . . ? C82 C86 C87 108.8(5) . . . ? C82 C86 C88 110.7(6) . . . ? C82 C86 C89 111.8(6) . . . ? C87 C86 C88 108.1(7) . . . ? C87 C86 C89 109.7(8) . . . ? C88 C86 C89 107.7(7) . . . ? C84 C90 C91 114.2(5) . . . ? C90 C91 C92 122.1(5) . . . ? C90 C91 C96 119.9(5) . . . ? C92 C91 C96 117.9(5) . . . ? C91 C92 C93 122.6(6) . . . ? C92 C93 C94 116.8(6) . . . ? C92 C93 C97 121.6(6) . . . ? C94 C93 C97 121.5(6) . . . ? C93 C94 C95 122.2(6) . . . ? C94 C95 C96 118.2(5) . . . ? C94 C95 C114 120.7(5) . . . ? C96 C95 C114 120.8(5) . . . ? C91 C96 C95 121.1(5) . . . ? C91 C96 O9 119.6(5) . . . ? C95 C96 O9 119.0(5) . . . ? C93 C97 C98 111.5(7) . . . ? C93 C97 C99 112.5(7) . . . ? C93 C97 C100 108.1(6) . . . ? C98 C97 C99 111(1) . . . ? C98 C97 C100 112(1) . . . ? C99 C97 C100 100(1) . . . ? C96 O9 C101 119.0(5) . . . ? O9 C101 P4 123.7(6) . . . ? C101 P4 O10 109.1(5) . . . ? C101 P4 C102 111.1(6) . . . ? C101 P4 C108 109.5(3) . . . ? O10 P4 C102 116.3(7) . . . ? O10 P4 C108 104.1(3) . . . ? C102 P4 C108 106.3(4) . . . ? P4 C102 C103 126.9(7) . . . ? P4 C102 C107 110(1) . . . ? C103 C102 C107 122(1) . . . ? C102 C103 C104 118(1) . . . ? C103 C104 C105 117.0(9) . . . ? C104 C105 C106 118(1) . . . ? C105 C106 C107 121(1) . . . ? C102 C107 C106 121(1) . . . ? P4 C108 C109 107.6(17) . . . ? P4 C108 C112 154.6(10) . . . ? P4 C108 C113 125.9(11) . . . ? C109 C108 C112 96.5(12) . . . ? C109 C108 C113 125.6(19) . . . ? C108 C109 C110 117.3(17) . . . ? C109 C110 C111 111.4(14) . . . ? C110 C111 C112 109.1(13) . . . ? C108 C112 C111 104.9(11) . . . ? C111 C112 C113 130.8(16) . . . ? C108 C113 C112 125(2) . . . ? C58 C114 C95 111.1(5) . . . ? C115 C116 N1 179(1) . . . ? C117 C118 N2 174(1) . . . ? C119 C120 N3 178(1) . . . ? C121 C122 N4 178(1) . . . ? C123 C124 N5 174(2) . . . ? _______________________________________________________ data_wel4 _database_code_CSD 184802 _audit_creation_date 10-03-02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H85 B Cl6 F4 N2 O5 P Pd' _chemical_formula_sum 'C66 H85 B Cl6 F4 N2 O5 P Pd' _chemical_formula_weight 1423.24 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 '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' 'B' 'B' 0.0013 0.0007 '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 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7230(4) _cell_length_b 14.6378(4) _cell_length_c 18.4221(6) _cell_angle_alpha 87.411(2) _cell_angle_beta 88.7070(13) _cell_angle_gamma 78.6180(13) _cell_volume 3623.70(19) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 8305 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'prism' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21214 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15232 _reflns_number_gt 9432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS V6 (Dowty, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1146P)^2^+0.3622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15232 _refine_ls_number_parameters 773 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.2084 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _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 C1 C 0.5276(3) 0.1620(3) 0.7455(2) 0.0264(10) Uani 1 1 d . . . C2 C 0.5611(3) 0.0912(3) 0.7974(2) 0.0298(10) Uani 1 1 d . . . C3 C 0.5061(3) 0.0893(3) 0.8613(3) 0.0357(11) Uani 1 1 d . . . H3 H 0.5277 0.0428 0.8966 0.043 Uiso 1 1 calc . . . C4 C 0.4192(4) 0.1550(4) 0.8745(3) 0.0381(12) Uani 1 1 d . . . C5 C 0.3893(3) 0.2234(3) 0.8205(3) 0.0361(12) Uani 1 1 d . . . H5 H 0.3314 0.2674 0.8278 0.043 Uiso 1 1 calc . . . C6 C 0.4426(3) 0.2287(3) 0.7557(2) 0.0294(10) Uani 1 1 d . . . C7 C 0.3612(4) 0.1466(4) 0.9461(3) 0.0554(16) Uani 1 1 d . . . C8 C 0.3227(5) 0.0569(5) 0.9497(4) 0.0680(19) Uani 1 1 d . . . H8A H 0.3769 0.0054 0.9429 0.102 Uiso 1 1 calc . . . H8B H 0.2748 0.0588 0.9122 0.102 Uiso 1 1 calc . . . H8C H 0.2918 0.0495 0.9963 0.102 Uiso 1 1 calc . . . C9 C 0.4325(5) 0.1460(5) 1.0111(3) 0.074(2) Uani 1 1 d . . . H9A H 0.4575 0.2030 1.0092 0.111 Uiso 1 1 calc . . . H9B H 0.4871 0.0940 1.0080 0.111 Uiso 1 1 calc . . . H9C H 0.3969 0.1408 1.0561 0.111 Uiso 1 1 calc . . . C10 C 0.2763(5) 0.2302(5) 0.9557(3) 0.0626(18) Uani 1 1 d . . . H10A H 0.3024 0.2865 0.9536 0.094 Uiso 1 1 calc . . . H10B H 0.2439 0.2239 1.0018 0.094 Uiso 1 1 calc . . . H10C H 0.2292 0.2329 0.9175 0.094 Uiso 1 1 calc . . . C11 C 0.4137(3) 0.3077(3) 0.6999(2) 0.0293(11) Uani 1 1 d . . . H11A H 0.4367 0.2864 0.6523 0.035 Uiso 1 1 calc . . . H11B H 0.3418 0.3256 0.6988 0.035 Uiso 1 1 calc . . . C12 C 0.4564(3) 0.3908(3) 0.7160(2) 0.0271(10) Uani 1 1 d . . . C13 C 0.3939(3) 0.4689(3) 0.7468(2) 0.0305(11) Uani 1 1 d . . . H13 H 0.3285 0.4650 0.7587 0.037 Uiso 1 1 calc . . . C14 C 0.4254(3) 0.5499(3) 0.7599(2) 0.0310(11) Uani 1 1 d . . . C15 C 0.5226(3) 0.5553(3) 0.7395(2) 0.0300(10) Uani 1 1 d . . . H15 H 0.5446 0.6106 0.7456 0.036 Uiso 1 1 calc . . . C16 C 0.5881(3) 0.4797(3) 0.7099(2) 0.0274(10) Uani 1 1 d . . . C17 C 0.5550(3) 0.3976(3) 0.7018(2) 0.0238(10) Uani 1 1 d . . . C18 C 0.3581(4) 0.6341(4) 0.7939(3) 0.0378(12) Uani 1 1 d . . . C19 C 0.3433(7) 0.7156(5) 0.7398(5) 0.103(3) Uani 1 1 d . . . H19A H 0.3144 0.6989 0.6965 0.155 Uiso 1 1 calc . . . H19B H 0.4063 0.7320 0.7279 0.155 Uiso 1 1 calc . . . H19C H 0.2997 0.7678 0.7603 0.155 Uiso 1 1 calc . . . C20 C 0.4053(5) 0.6555(6) 0.8619(4) 0.103(3) Uani 1 1 d . . . H20A H 0.4121 0.6026 0.8955 0.155 Uiso 1 1 calc . . . H20B H 0.3643 0.7085 0.8834 0.155 Uiso 1 1 calc . . . H20C H 0.4697 0.6689 0.8504 0.155 Uiso 1 1 calc . . . C21 C 0.2548(5) 0.6154(6) 0.8119(5) 0.097(3) Uani 1 1 d . . . H21A H 0.2249 0.6006 0.7685 0.145 Uiso 1 1 calc . . . H21B H 0.2144 0.6699 0.8319 0.145 Uiso 1 1 calc . . . H21C H 0.2598 0.5640 0.8468 0.145 Uiso 1 1 calc . . . C22 C 0.6913(3) 0.4930(3) 0.6859(2) 0.0266(10) Uani 1 1 d . . . H22A H 0.7064 0.4689 0.6378 0.032 Uiso 1 1 calc . . . H22B H 0.6932 0.5589 0.6833 0.032 Uiso 1 1 calc . . . C23 C 0.7677(3) 0.4428(3) 0.7386(2) 0.0250(10) Uani 1 1 d . . . C24 C 0.8293(3) 0.3583(3) 0.7240(2) 0.0239(10) Uani 1 1 d . . . C25 C 0.8803(3) 0.3014(3) 0.7796(2) 0.0248(10) Uani 1 1 d . . . C26 C 0.8767(3) 0.3349(3) 0.8488(2) 0.0257(10) Uani 1 1 d . . . H26 H 0.9103 0.2969 0.8858 0.031 Uiso 1 1 calc . . . C27 C 0.8246(3) 0.4234(3) 0.8652(2) 0.0280(10) Uani 1 1 d . . . C28 C 0.7683(3) 0.4740(3) 0.8090(2) 0.0285(10) Uani 1 1 d . . . H28 H 0.7290 0.5315 0.8191 0.034 Uiso 1 1 calc . . . C29 C 0.8275(3) 0.4657(3) 0.9393(2) 0.0324(11) Uani 1 1 d . . . C30 C 0.8809(4) 0.5483(4) 0.9309(3) 0.0477(14) Uani 1 1 d . . . H30A H 0.8834 0.5752 0.9773 0.072 Uiso 1 1 calc . . . H30B H 0.8455 0.5945 0.8973 0.072 Uiso 1 1 calc . . . H30C H 0.9473 0.5270 0.9128 0.072 Uiso 1 1 calc . . . C31 C 0.7216(4) 0.5017(4) 0.9683(3) 0.0477(15) Uani 1 1 d . . . H31A H 0.7247 0.5271 1.0151 0.072 Uiso 1 1 calc . . . H31B H 0.6864 0.4510 0.9726 0.072 Uiso 1 1 calc . . . H31C H 0.6873 0.5492 0.9353 0.072 Uiso 1 1 calc . . . C32 C 0.8820(4) 0.3942(4) 0.9960(3) 0.0476(15) Uani 1 1 d . . . H32A H 0.8825 0.4233 1.0416 0.071 Uiso 1 1 calc . . . H32B H 0.9492 0.3721 0.9797 0.071 Uiso 1 1 calc . . . H32C H 0.8485 0.3426 1.0019 0.071 Uiso 1 1 calc . . . C33 C 0.9361(3) 0.2044(3) 0.7628(2) 0.0274(10) Uani 1 1 d . . . H33A H 0.9462 0.2018 0.7106 0.033 Uiso 1 1 calc . . . H33B H 1.0012 0.1951 0.7845 0.033 Uiso 1 1 calc . . . C34 C 0.8878(3) 0.1241(3) 0.7880(2) 0.0257(10) Uani 1 1 d . . . C35 C 0.9491(3) 0.0475(3) 0.8223(2) 0.0287(10) Uani 1 1 d . . . H35 H 1.0146 0.0514 0.8309 0.034 Uiso 1 1 calc . . . C36 C 0.9182(3) -0.0333(3) 0.8441(2) 0.0288(10) Uani 1 1 d . . . C37 C 0.8188(3) -0.0363(3) 0.8312(3) 0.0318(11) Uani 1 1 d . . . H37 H 0.7951 -0.0895 0.8463 0.038 Uiso 1 1 calc . . . C38 C 0.7535(3) 0.0374(3) 0.7965(2) 0.0275(10) Uani 1 1 d . . . C39 C 0.7884(3) 0.1178(3) 0.7754(2) 0.0253(10) Uani 1 1 d . . . C40 C 0.9858(3) -0.1170(3) 0.8824(3) 0.0350(12) Uani 1 1 d . . . C41 C 1.0962(4) -0.1089(4) 0.8763(4) 0.0589(17) Uani 1 1 d . . . H41A H 1.1046 -0.0520 0.8970 0.088 Uiso 1 1 calc . . . H41B H 1.1163 -0.1086 0.8260 0.088 Uiso 1 1 calc . . . H41C H 1.1362 -0.1610 0.9020 0.088 Uiso 1 1 calc . . . C42 C 0.9748(4) -0.2083(4) 0.8492(3) 0.0510(15) Uani 1 1 d . . . H42A H 1.0177 -0.2596 0.8737 0.076 Uiso 1 1 calc . . . H42B H 0.9929 -0.2066 0.7985 0.076 Uiso 1 1 calc . . . H42C H 0.9071 -0.2160 0.8543 0.076 Uiso 1 1 calc . . . C43 C 0.9559(4) -0.1209(4) 0.9632(3) 0.0549(16) Uani 1 1 d . . . H43A H 0.9629 -0.0641 0.9848 0.082 Uiso 1 1 calc . . . H43B H 0.9981 -0.1728 0.9876 0.082 Uiso 1 1 calc . . . H43C H 0.8880 -0.1282 0.9677 0.082 Uiso 1 1 calc . . . C44 C 0.6515(3) 0.0179(3) 0.7811(3) 0.0302(11) Uani 1 1 d . . . H44A H 0.6501 0.0050 0.7300 0.036 Uiso 1 1 calc . . . H44B H 0.6448 -0.0388 0.8084 0.036 Uiso 1 1 calc . . . C45 C 0.7657(4) 0.0466(3) 0.5930(3) 0.0387(12) Uani 1 1 d . . . H45A H 0.7950 0.0306 0.6405 0.046 Uiso 1 1 calc . . . H45B H 0.6997 0.0318 0.5942 0.046 Uiso 1 1 calc . . . C46 C 0.8293(4) -0.0085(3) 0.5357(3) 0.0347(12) Uani 1 1 d . . . C47 C 0.8586(4) -0.1029(4) 0.5409(3) 0.0440(13) Uani 1 1 d . . . H47 H 0.8395 -0.1367 0.5809 0.053 Uiso 1 1 calc . . . C48 C 0.9189(4) -0.1498(4) 0.4843(3) 0.0541(16) Uani 1 1 d . . . H48 H 0.9393 -0.2143 0.4887 0.065 Uiso 1 1 calc . . . C49 C 0.9470(4) -0.1044(4) 0.4255(3) 0.0548(16) Uani 1 1 d . . . H49 H 0.9851 -0.1373 0.3892 0.066 Uiso 1 1 calc . . . C50 C 0.9183(4) -0.0049(4) 0.4184(3) 0.0405(13) Uani 1 1 d . . . C51 C 0.8603(3) 0.0408(3) 0.4755(2) 0.0322(11) Uani 1 1 d . . . C52 C 0.8584(4) 0.1852(4) 0.4182(3) 0.0384(12) Uani 1 1 d . . . H52 H 0.8390 0.2498 0.4181 0.046 Uiso 1 1 calc . . . C53 C 0.9135(4) 0.1448(4) 0.3585(3) 0.0460(14) Uani 1 1 d . . . H53 H 0.9290 0.1817 0.3192 0.055 Uiso 1 1 calc . . . C54 C 0.9434(4) 0.0510(4) 0.3596(3) 0.0487(15) Uani 1 1 d . . . H54 H 0.9810 0.0232 0.3210 0.058 Uiso 1 1 calc . . . C55 C 0.7969(3) 0.3863(3) 0.5341(2) 0.0263(10) Uani 1 1 d . . . C56 C 0.8688(3) 0.3781(3) 0.5969(2) 0.0284(10) Uani 1 1 d . . . H56A H 0.9352 0.3495 0.5809 0.034 Uiso 1 1 calc . . . H56B H 0.8706 0.4395 0.6137 0.034 Uiso 1 1 calc . . . C57 C 0.7165(4) 0.4629(4) 0.4276(2) 0.0368(12) Uani 1 1 d . . . H57A H 0.7287 0.4027 0.4055 0.044 Uiso 1 1 calc . . . H57B H 0.7290 0.5090 0.3910 0.044 Uiso 1 1 calc . . . C58 C 0.6089(4) 0.4868(4) 0.4523(3) 0.0467(14) Uani 1 1 d . . . H58A H 0.5665 0.4880 0.4114 0.070 Uiso 1 1 calc . . . H58B H 0.5960 0.5469 0.4733 0.070 Uiso 1 1 calc . . . H58C H 0.5958 0.4406 0.4879 0.070 Uiso 1 1 calc . . . C59 C 0.8424(4) 0.5347(4) 0.4887(3) 0.0383(12) Uani 1 1 d . . . H59A H 0.8772 0.5380 0.4425 0.046 Uiso 1 1 calc . . . H59B H 0.8918 0.5204 0.5266 0.046 Uiso 1 1 calc . . . C60 C 0.7761(5) 0.6282(4) 0.5018(4) 0.0570(16) Uani 1 1 d . . . H60A H 0.8158 0.6755 0.5017 0.086 Uiso 1 1 calc . . . H60B H 0.7428 0.6256 0.5480 0.086 Uiso 1 1 calc . . . H60C H 0.7278 0.6430 0.4640 0.086 Uiso 1 1 calc . . . C61 C 1.0721(4) 0.4327(4) 0.7573(3) 0.0558(16) Uani 1 1 d . . . H61A H 1.0005 0.4412 0.7630 0.067 Uiso 1 1 calc . . . H61B H 1.0877 0.4912 0.7385 0.067 Uiso 1 1 calc . . . C62 C 0.6083(4) 0.3013(5) 0.8910(3) 0.0560(16) Uani 1 1 d . . . H62A H 0.5796 0.2655 0.8570 0.067 Uiso 1 1 calc . . . H62B H 0.6493 0.3377 0.8634 0.067 Uiso 1 1 calc . . . C63 C 0.7481(5) -0.2514(5) 0.7391(3) 0.0622(18) Uani 1 1 d . . . H63A H 0.7926 -0.2077 0.7409 0.075 Uiso 1 1 calc . . . H63B H 0.7879 -0.3126 0.7307 0.075 Uiso 1 1 calc . . . Pd Pd 0.75667(2) 0.18359(2) 0.568588(18) 0.02751(14) Uani 1 1 d . . . F1 F 1.0020(2) 0.6417(2) 0.55909(18) 0.0588(9) Uani 1 1 d . . . F2 F 1.0790(2) 0.6227(3) 0.66784(19) 0.0643(10) Uani 1 1 d . . . F3 F 0.9364(2) 0.5692(2) 0.65445(18) 0.0589(9) Uani 1 1 d . . . F4 F 0.9326(3) 0.7232(2) 0.6546(2) 0.0673(10) Uani 1 1 d . . . N1 N 0.8332(3) 0.1359(3) 0.47404(19) 0.0293(9) Uani 1 1 d . . . N2 N 0.7857(3) 0.4598(3) 0.4880(2) 0.0295(9) Uani 1 1 d . . . P P 0.67120(8) 0.21765(8) 0.66984(6) 0.0244(3) Uani 1 1 d . . . O1 O 0.5818(2) 0.1628(2) 0.67931(15) 0.0268(7) Uani 1 1 d . . . O2 O 0.6231(2) 0.3250(2) 0.66882(15) 0.0256(7) Uani 1 1 d . . . O3 O 0.72332(19) 0.19875(19) 0.74783(15) 0.0236(7) Uani 1 1 d . . . O4 O 0.7483(2) 0.3241(2) 0.52631(16) 0.0306(7) Uani 1 1 d . . . O5 O 0.8362(2) 0.3219(2) 0.65459(15) 0.0274(7) Uani 1 1 d . . . Cl1 Cl 1.11368(12) 0.34583(14) 0.69553(9) 0.0693(5) Uani 1 1 d . . . Cl2 Cl 1.12796(12) 0.40334(14) 0.84247(9) 0.0720(5) Uani 1 1 d . . . Cl3 Cl 0.68295(13) 0.22457(13) 0.95159(10) 0.0718(5) Uani 1 1 d . . . Cl4 Cl 0.51210(12) 0.37717(13) 0.93469(10) 0.0705(5) Uani 1 1 d . . . Cl5 Cl 0.66680(16) -0.21846(16) 0.66816(11) 0.0893(6) Uani 1 1 d . . . Cl6 Cl 0.68414(13) -0.25475(11) 0.82322(9) 0.0661(5) Uani 1 1 d . . . B B 0.9881(5) 0.6393(4) 0.6348(4) 0.0428(15) Uani 1 1 d . . . C80 C 0.2461(10) 0.0712(9) 0.7260(7) 0.091(5) Uiso 0.50 1 d PD . . H80A H 0.2209 0.1370 0.7280 0.136 Uiso 0.50 1 calc P . . H80B H 0.2804 0.0488 0.7701 0.136 Uiso 0.50 1 calc P . . H80C H 0.1918 0.0396 0.7205 0.136 Uiso 0.50 1 calc P . . C81 C 0.5034(10) -0.2122(9) 0.5075(7) 0.086(5) Uiso 0.50 1 d PD . . H81A H 0.5105 -0.2779 0.5010 0.129 Uiso 0.50 1 calc P . . H81B H 0.5674 -0.1979 0.5160 0.129 Uiso 0.50 1 calc P . . H81C H 0.4755 -0.1783 0.4646 0.129 Uiso 0.50 1 calc P . . C82 C 0.3606(12) -0.0541(7) 0.6568(6) 0.111(6) Uiso 0.50 1 d PD . . H82A H 0.3062 -0.0875 0.6611 0.133 Uiso 0.50 1 calc P . . H82B H 0.4048 -0.0745 0.6972 0.133 Uiso 0.50 1 calc P . . C83 C 0.3190(12) 0.0518(7) 0.6604(7) 0.108(6) Uiso 0.50 1 d PD . . H83A H 0.2847 0.0747 0.6157 0.129 Uiso 0.50 1 calc P . . H83B H 0.3734 0.0845 0.6654 0.129 Uiso 0.50 1 calc P . . C84 C 0.4180(12) -0.0778(7) 0.5844(7) 0.118(6) Uiso 0.50 1 d PD . . H84A H 0.4819 -0.0590 0.5855 0.142 Uiso 0.50 1 calc P . . H84B H 0.3807 -0.0439 0.5442 0.142 Uiso 0.50 1 calc P . . C85 C 0.4339(14) -0.1841(7) 0.5734(8) 0.128(7) Uiso 0.50 1 d PD . . H85A H 0.4626 -0.2179 0.6169 0.153 Uiso 0.50 1 calc P . . H85B H 0.3702 -0.2012 0.5657 0.153 Uiso 0.50 1 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(2) 0.030(3) 0.027(2) -0.001(2) -0.0005(18) -0.0092(19) C2 0.030(2) 0.028(3) 0.033(3) -0.001(2) 0.0032(19) -0.008(2) C3 0.034(3) 0.033(3) 0.037(3) 0.011(2) 0.003(2) -0.003(2) C4 0.037(3) 0.032(3) 0.043(3) 0.007(2) 0.014(2) -0.005(2) C5 0.025(2) 0.031(3) 0.050(3) 0.000(2) 0.010(2) -0.001(2) C6 0.024(2) 0.028(3) 0.036(3) 0.004(2) -0.0059(19) -0.005(2) C7 0.054(3) 0.044(4) 0.060(4) 0.009(3) 0.030(3) 0.005(3) C8 0.058(4) 0.054(4) 0.089(5) 0.011(4) 0.038(3) -0.013(3) C9 0.089(5) 0.078(5) 0.046(4) 0.014(3) 0.018(3) 0.005(4) C10 0.064(4) 0.057(4) 0.059(4) 0.009(3) 0.031(3) 0.002(3) C11 0.022(2) 0.034(3) 0.030(2) -0.001(2) -0.0019(18) -0.003(2) C12 0.026(2) 0.030(3) 0.021(2) 0.0037(19) -0.0019(17) 0.002(2) C13 0.026(2) 0.035(3) 0.028(2) 0.002(2) -0.0006(18) 0.001(2) C14 0.029(2) 0.033(3) 0.027(2) 0.000(2) -0.0021(19) 0.005(2) C15 0.036(3) 0.028(3) 0.025(2) 0.0017(19) -0.0014(19) -0.005(2) C16 0.026(2) 0.027(3) 0.025(2) 0.0017(19) -0.0035(18) 0.0044(19) C17 0.026(2) 0.022(2) 0.020(2) -0.0018(18) 0.0031(17) 0.0034(18) C18 0.036(3) 0.032(3) 0.042(3) -0.009(2) 0.007(2) 0.003(2) C19 0.139(7) 0.045(4) 0.099(6) -0.002(4) 0.026(5) 0.043(5) C20 0.079(5) 0.128(8) 0.091(6) -0.078(6) -0.010(4) 0.025(5) C21 0.067(5) 0.079(6) 0.138(8) -0.042(5) 0.045(5) 0.003(4) C22 0.026(2) 0.026(3) 0.027(2) 0.0003(19) -0.0001(18) -0.0046(19) C23 0.022(2) 0.026(2) 0.029(2) 0.0007(19) -0.0012(17) -0.0081(18) C24 0.022(2) 0.029(3) 0.022(2) -0.0026(18) 0.0025(17) -0.0067(19) C25 0.017(2) 0.025(2) 0.031(2) 0.0042(19) 0.0044(17) -0.0040(18) C26 0.022(2) 0.029(3) 0.026(2) 0.0028(19) -0.0029(17) -0.0047(19) C27 0.023(2) 0.028(3) 0.035(3) -0.005(2) -0.0009(19) -0.0083(19) C28 0.029(2) 0.028(3) 0.028(2) -0.006(2) 0.0013(18) -0.002(2) C29 0.035(3) 0.034(3) 0.028(2) -0.004(2) -0.002(2) -0.007(2) C30 0.054(3) 0.051(4) 0.041(3) -0.013(3) -0.001(3) -0.015(3) C31 0.047(3) 0.061(4) 0.035(3) -0.017(3) 0.005(2) -0.006(3) C32 0.057(3) 0.051(4) 0.035(3) -0.008(3) -0.013(2) -0.009(3) C33 0.023(2) 0.028(3) 0.031(2) 0.0017(19) 0.0032(18) -0.0041(19) C34 0.028(2) 0.021(2) 0.026(2) -0.0019(18) 0.0026(18) 0.0016(19) C35 0.027(2) 0.027(3) 0.031(2) 0.001(2) -0.0038(18) -0.001(2) C36 0.027(2) 0.027(3) 0.031(2) 0.000(2) 0.0017(19) -0.002(2) C37 0.035(3) 0.023(3) 0.036(3) -0.001(2) 0.006(2) -0.004(2) C38 0.028(2) 0.025(3) 0.027(2) -0.0033(19) 0.0026(18) 0.000(2) C39 0.028(2) 0.021(2) 0.025(2) 0.0006(18) 0.0016(18) 0.0002(19) C40 0.034(3) 0.027(3) 0.041(3) 0.003(2) -0.004(2) 0.002(2) C41 0.037(3) 0.048(4) 0.083(4) 0.021(3) -0.005(3) 0.009(3) C42 0.057(3) 0.030(3) 0.060(4) 0.000(3) -0.014(3) 0.008(3) C43 0.064(4) 0.053(4) 0.040(3) 0.009(3) 0.002(3) 0.004(3) C44 0.029(2) 0.022(2) 0.039(3) -0.002(2) 0.005(2) -0.004(2) C45 0.056(3) 0.024(3) 0.035(3) -0.002(2) 0.013(2) -0.006(2) C46 0.046(3) 0.026(3) 0.030(3) -0.004(2) 0.001(2) -0.001(2) C47 0.061(3) 0.027(3) 0.043(3) -0.002(2) 0.009(3) -0.007(3) C48 0.068(4) 0.025(3) 0.064(4) -0.006(3) 0.010(3) 0.006(3) C49 0.067(4) 0.039(3) 0.053(4) -0.014(3) 0.018(3) 0.003(3) C50 0.044(3) 0.038(3) 0.038(3) -0.007(2) 0.009(2) -0.004(2) C51 0.037(3) 0.031(3) 0.028(2) -0.008(2) 0.005(2) -0.005(2) C52 0.050(3) 0.039(3) 0.028(3) -0.005(2) 0.011(2) -0.013(2) C53 0.062(3) 0.045(4) 0.033(3) -0.004(2) 0.017(2) -0.017(3) C54 0.050(3) 0.059(4) 0.038(3) -0.014(3) 0.016(2) -0.012(3) C55 0.030(2) 0.026(3) 0.020(2) -0.0007(19) 0.0068(18) -0.001(2) C56 0.029(2) 0.029(3) 0.026(2) 0.0000(19) 0.0041(18) -0.004(2) C57 0.040(3) 0.042(3) 0.026(2) 0.006(2) -0.004(2) -0.003(2) C58 0.036(3) 0.056(4) 0.048(3) 0.011(3) -0.007(2) -0.011(3) C59 0.042(3) 0.039(3) 0.034(3) 0.008(2) -0.002(2) -0.010(2) C60 0.062(4) 0.029(3) 0.081(5) -0.002(3) 0.003(3) -0.012(3) C61 0.046(3) 0.052(4) 0.067(4) 0.028(3) -0.009(3) -0.010(3) C62 0.061(4) 0.070(4) 0.043(3) -0.011(3) 0.003(3) -0.026(3) C63 0.060(4) 0.075(5) 0.054(4) -0.015(3) 0.008(3) -0.019(3) Pd 0.0316(2) 0.0252(2) 0.0253(2) -0.00236(14) 0.00484(14) -0.00480(15) F1 0.064(2) 0.059(2) 0.051(2) 0.0040(16) 0.0061(16) -0.0078(17) F2 0.051(2) 0.070(2) 0.075(2) 0.0222(19) -0.0169(17) -0.0224(18) F3 0.068(2) 0.051(2) 0.064(2) 0.0156(17) -0.0125(17) -0.0284(18) F4 0.073(2) 0.048(2) 0.076(2) -0.0051(18) 0.0230(19) -0.0023(18) N1 0.034(2) 0.031(2) 0.023(2) -0.0038(17) 0.0074(16) -0.0056(18) N2 0.030(2) 0.030(2) 0.027(2) 0.0024(17) 0.0023(16) -0.0030(17) P 0.0248(6) 0.0242(6) 0.0236(6) -0.0011(5) 0.0016(4) -0.0034(5) O1 0.0271(15) 0.0314(18) 0.0230(16) -0.0031(13) 0.0027(12) -0.0082(14) O2 0.0259(15) 0.0207(16) 0.0285(16) -0.0029(13) 0.0030(12) -0.0008(13) O3 0.0225(14) 0.0203(16) 0.0268(16) 0.0004(12) 0.0010(12) -0.0019(12) O4 0.0380(17) 0.0260(18) 0.0286(17) -0.0003(14) -0.0022(14) -0.0084(15) O5 0.0336(16) 0.0258(17) 0.0231(16) 0.0002(13) 0.0009(13) -0.0069(14) Cl1 0.0559(9) 0.0911(14) 0.0630(10) 0.0067(9) 0.0056(8) -0.0227(9) Cl2 0.0526(9) 0.0914(14) 0.0641(10) 0.0081(9) -0.0129(7) 0.0036(9) Cl3 0.0681(10) 0.0788(13) 0.0652(11) -0.0067(9) 0.0011(8) -0.0060(9) Cl4 0.0631(10) 0.0732(12) 0.0749(11) -0.0161(9) -0.0026(8) -0.0099(9) Cl5 0.0968(14) 0.1035(16) 0.0681(12) -0.0055(11) -0.0114(10) -0.0191(12) Cl6 0.0813(11) 0.0492(10) 0.0671(10) -0.0038(8) 0.0201(8) -0.0131(8) B 0.043(3) 0.033(4) 0.052(4) 0.008(3) 0.006(3) -0.008(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 C1 C6 1.380(6) . ? C1 C2 1.394(6) . ? C1 O1 1.414(5) . ? C2 C3 1.386(7) . ? C2 C44 1.506(6) . ? C3 C4 1.400(6) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C4 C7 1.539(7) . ? C5 C6 1.393(7) . ? C5 H5 0.9300 . ? C6 C11 1.509(7) . ? C7 C8 1.507(9) . ? C7 C10 1.528(8) . ? C7 C9 1.563(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.494(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.395(6) . ? C12 C13 1.419(6) . ? C13 C14 1.373(7) . ? C13 H13 0.9300 . ? C14 C15 1.394(7) . ? C14 C18 1.536(6) . ? C15 C16 1.403(6) . ? C15 H15 0.9300 . ? C16 C17 1.381(6) . ? C16 C22 1.520(6) . ? C17 O2 1.419(4) . ? C18 C20 1.495(8) . ? C18 C19 1.505(10) . ? C18 C21 1.524(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.503(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.387(6) . ? C23 C28 1.395(6) . ? C24 O5 1.401(5) . ? C24 C25 1.401(6) . ? C25 C26 1.382(6) . ? C25 C33 1.516(6) . ? C26 C27 1.394(6) . ? C26 H26 0.9300 . ? C27 C28 1.400(6) . ? C27 C29 1.529(6) . ? C28 H28 0.9300 . ? C29 C30 1.533(8) . ? C29 C31 1.537(7) . ? C29 C32 1.541(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.510(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.397(6) . ? C34 C39 1.410(6) . ? C35 C36 1.374(7) . ? C35 H35 0.9300 . ? C36 C37 1.400(6) . ? C36 C40 1.536(6) . ? C37 C38 1.398(6) . ? C37 H37 0.9300 . ? C38 C39 1.392(7) . ? C38 C44 1.519(6) . ? C39 O3 1.417(5) . ? C40 C42 1.530(7) . ? C40 C43 1.537(7) . ? C40 C41 1.544(8) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.512(6) . ? C45 Pd 2.016(5) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.362(7) . ? C46 C51 1.399(7) . ? C47 C48 1.429(7) . ? C47 H47 0.9300 . ? C48 C49 1.335(9) . ? C48 H48 0.9300 . ? C49 C50 1.433(8) . ? C49 H49 0.9300 . ? C50 C54 1.405(8) . ? C50 C51 1.417(6) . ? C51 N1 1.367(6) . ? C52 N1 1.309(6) . ? C52 C53 1.406(7) . ? C52 H52 0.9300 . ? C53 C54 1.352(8) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 O4 1.245(5) . ? C55 N2 1.325(6) . ? C55 C56 1.523(6) . ? C56 O5 1.432(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N2 1.473(6) . ? C57 C58 1.514(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 N2 1.465(6) . ? C59 C60 1.513(7) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 Cl1 1.747(7) . ? C61 Cl2 1.759(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 Cl3 1.744(7) . ? C62 Cl4 1.755(6) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 Cl5 1.727(7) . ? C63 Cl6 1.767(7) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? Pd N1 2.089(3) . ? Pd O4 2.148(3) . ? Pd P 2.2041(11) . ? F1 B 1.404(7) . ? F2 B 1.373(7) . ? F3 B 1.389(7) . ? F4 B 1.371(7) . ? P O2 1.579(3) . ? P O1 1.595(3) . ? P O3 1.608(3) . ? C80 C83 1.553(2) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 C85 1.546(2) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 C83 1.547(2) . ? C82 C84 1.550(2) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 C85 1.550(2) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? 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 C6 C1 C2 122.4(4) . . ? C6 C1 O1 119.5(4) . . ? C2 C1 O1 118.0(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C44 122.7(4) . . ? C1 C2 C44 119.6(4) . . ? C2 C3 C4 122.3(5) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 117.3(4) . . ? C5 C4 C7 123.7(4) . . ? C3 C4 C7 119.0(5) . . ? C4 C5 C6 122.5(4) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 117.8(4) . . ? C1 C6 C11 120.1(4) . . ? C5 C6 C11 122.0(4) . . ? C8 C7 C10 110.7(5) . . ? C8 C7 C4 110.1(5) . . ? C10 C7 C4 111.9(5) . . ? C8 C7 C9 108.9(6) . . ? C10 C7 C9 106.1(5) . . ? C4 C7 C9 108.9(5) . . ? 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 . . ? C12 C11 C6 112.1(4) . . ? C12 C11 H11A 109.2 . . ? C6 C11 H11A 109.2 . . ? C12 C11 H11B 109.2 . . ? C6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C17 C12 C13 116.9(4) . . ? C17 C12 C11 124.1(4) . . ? C13 C12 C11 119.0(4) . . ? C14 C13 C12 123.0(4) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 117.5(4) . . ? C13 C14 C18 123.1(4) . . ? C15 C14 C18 119.4(4) . . ? C14 C15 C16 121.8(4) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C17 C16 C15 118.6(4) . . ? C17 C16 C22 122.9(4) . . ? C15 C16 C22 118.5(4) . . ? C16 C17 C12 121.8(4) . . ? C16 C17 O2 116.1(4) . . ? C12 C17 O2 121.6(4) . . ? C20 C18 C19 111.8(7) . . ? C20 C18 C21 109.4(6) . . ? C19 C18 C21 106.0(6) . . ? C20 C18 C14 108.7(4) . . ? C19 C18 C14 109.3(4) . . ? C21 C18 C14 111.8(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C16 110.3(4) . . ? C23 C22 H22A 109.6 . . ? C16 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C16 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 117.3(4) . . ? C24 C23 C22 122.6(4) . . ? C28 C23 C22 119.5(4) . . ? C23 C24 O5 121.8(4) . . ? C23 C24 C25 121.2(4) . . ? O5 C24 C25 116.8(4) . . ? C26 C25 C24 118.8(4) . . ? C26 C25 C33 121.9(4) . . ? C24 C25 C33 119.3(4) . . ? C25 C26 C27 122.5(4) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C28 116.0(4) . . ? C26 C27 C29 123.6(4) . . ? C28 C27 C29 120.4(4) . . ? C23 C28 C27 123.6(4) . . ? C23 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? C27 C29 C30 108.8(4) . . ? C27 C29 C31 110.6(4) . . ? C30 C29 C31 108.4(4) . . ? C27 C29 C32 111.9(4) . . ? C30 C29 C32 109.1(4) . . ? C31 C29 C32 108.0(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C25 116.6(4) . . ? C34 C33 H33A 108.2 . . ? C25 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? C25 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? C35 C34 C39 117.8(4) . . ? C35 C34 C33 116.7(4) . . ? C39 C34 C33 125.3(4) . . ? C36 C35 C34 123.8(4) . . ? C36 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? C35 C36 C37 116.5(4) . . ? C35 C36 C40 123.6(4) . . ? C37 C36 C40 119.9(4) . . ? C38 C37 C36 122.7(5) . . ? C38 C37 H37 118.6 . . ? C36 C37 H37 118.6 . . ? C39 C38 C37 118.6(4) . . ? C39 C38 C44 126.2(4) . . ? C37 C38 C44 115.1(4) . . ? C38 C39 C34 120.5(4) . . ? C38 C39 O3 121.2(4) . . ? C34 C39 O3 117.9(4) . . ? C42 C40 C36 110.8(4) . . ? C42 C40 C43 108.7(5) . . ? C36 C40 C43 109.0(4) . . ? C42 C40 C41 108.2(4) . . ? C36 C40 C41 111.4(4) . . ? C43 C40 C41 108.8(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C2 C44 C38 118.7(4) . . ? C2 C44 H44A 107.6 . . ? C38 C44 H44A 107.6 . . ? C2 C44 H44B 107.6 . . ? C38 C44 H44B 107.6 . . ? H44A C44 H44B 107.1 . . ? C46 C45 Pd 108.5(4) . . ? C46 C45 H45A 110.0 . . ? Pd C45 H45A 110.0 . . ? C46 C45 H45B 110.0 . . ? Pd C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C47 C46 C51 119.2(4) . . ? C47 C46 C45 122.8(5) . . ? C51 C46 C45 118.0(4) . . ? C46 C47 C48 119.4(5) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 122.4(5) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C48 C49 C50 119.8(5) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C54 C50 C51 117.3(5) . . ? C54 C50 C49 125.5(5) . . ? C51 C50 C49 117.2(5) . . ? N1 C51 C46 117.3(4) . . ? N1 C51 C50 120.7(5) . . ? C46 C51 C50 121.9(5) . . ? N1 C52 C53 122.8(5) . . ? N1 C52 H52 118.6 . . ? C53 C52 H52 118.6 . . ? C54 C53 C52 118.4(5) . . ? C54 C53 H53 120.8 . . ? C52 C53 H53 120.8 . . ? C53 C54 C50 120.9(5) . . ? C53 C54 H54 119.6 . . ? C50 C54 H54 119.6 . . ? O4 C55 N2 120.2(4) . . ? O4 C55 C56 119.8(4) . . ? N2 C55 C56 120.1(4) . . ? O5 C56 C55 108.8(4) . . ? O5 C56 H56A 109.9 . . ? C55 C56 H56A 109.9 . . ? O5 C56 H56B 109.9 . . ? C55 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? N2 C57 C58 112.3(4) . . ? N2 C57 H57A 109.2 . . ? C58 C57 H57A 109.2 . . ? N2 C57 H57B 109.2 . . ? C58 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N2 C59 C60 111.9(4) . . ? N2 C59 H59A 109.2 . . ? C60 C59 H59A 109.2 . . ? N2 C59 H59B 109.2 . . ? C60 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Cl1 C61 Cl2 111.2(3) . . ? Cl1 C61 H61A 109.4 . . ? Cl2 C61 H61A 109.4 . . ? Cl1 C61 H61B 109.4 . . ? Cl2 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? Cl3 C62 Cl4 112.7(3) . . ? Cl3 C62 H62A 109.0 . . ? Cl4 C62 H62A 109.0 . . ? Cl3 C62 H62B 109.0 . . ? Cl4 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? Cl5 C63 Cl6 111.5(3) . . ? Cl5 C63 H63A 109.3 . . ? Cl6 C63 H63A 109.3 . . ? Cl5 C63 H63B 109.3 . . ? Cl6 C63 H63B 109.3 . . ? H63A C63 H63B 108.0 . . ? C45 Pd N1 83.69(17) . . ? C45 Pd O4 171.66(15) . . ? N1 Pd O4 88.83(14) . . ? C45 Pd P 89.92(14) . . ? N1 Pd P 173.27(12) . . ? O4 Pd P 97.39(8) . . ? C52 N1 C51 119.8(4) . . ? C52 N1 Pd 128.2(3) . . ? C51 N1 Pd 112.0(3) . . ? C55 N2 C59 125.4(4) . . ? C55 N2 C57 117.5(4) . . ? C59 N2 C57 116.9(4) . . ? O2 P O1 106.59(16) . . ? O2 P O3 103.56(15) . . ? O1 P O3 102.20(16) . . ? O2 P Pd 110.14(13) . . ? O1 P Pd 111.86(11) . . ? O3 P Pd 121.26(11) . . ? C1 O1 P 121.4(3) . . ? C17 O2 P 147.1(3) . . ? C39 O3 P 129.1(2) . . ? C55 O4 Pd 135.4(3) . . ? C24 O5 C56 116.5(3) . . ? F4 B F2 110.5(5) . . ? F4 B F3 108.9(5) . . ? F2 B F3 110.4(5) . . ? F4 B F1 108.8(5) . . ? F2 B F1 109.4(5) . . ? F3 B F1 108.9(5) . . ? C83 C80 H80A 109.5 . . ? C83 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C83 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C85 C81 H81A 109.5 . . ? C85 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C85 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C84 111.3(3) . . ? C83 C82 H82A 109.4 . . ? C84 C82 H82A 109.4 . . ? C83 C82 H82B 109.4 . . ? C84 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? C82 C83 C80 110.0(3) . . ? C82 C83 H83A 109.7 . . ? C80 C83 H83A 109.7 . . ? C82 C83 H83B 109.7 . . ? C80 C83 H83B 109.7 . . ? H83A C83 H83B 108.2 . . ? C82 C84 C85 109.7(3) . . ? C82 C84 H84A 109.7 . . ? C85 C84 H84A 109.7 . . ? C82 C84 H84B 109.7 . . ? C85 C84 H84B 109.7 . . ? H84A C84 H84B 108.2 . . ? C81 C85 C84 111.1(3) . . ? C81 C85 H85A 109.4 . . ? C84 C85 H85A 109.4 . . ? C81 C85 H85B 109.4 . . ? C84 C85 H85B 109.4 . . ? H85A C85 H85B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.2(7) . . . . ? O1 C1 C2 C3 -178.3(4) . . . . ? C6 C1 C2 C44 176.9(4) . . . . ? O1 C1 C2 C44 -1.2(6) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C44 C2 C3 C4 -176.6(5) . . . . ? C2 C3 C4 C5 0.0(8) . . . . ? C2 C3 C4 C7 178.6(5) . . . . ? C3 C4 C5 C6 -0.7(8) . . . . ? C7 C4 C5 C6 -179.1(5) . . . . ? C2 C1 C6 C5 -0.4(7) . . . . ? O1 C1 C6 C5 177.6(4) . . . . ? C2 C1 C6 C11 175.7(4) . . . . ? O1 C1 C6 C11 -6.3(6) . . . . ? C4 C5 C6 C1 0.8(7) . . . . ? C4 C5 C6 C11 -175.2(5) . . . . ? C5 C4 C7 C8 114.9(6) . . . . ? C3 C4 C7 C8 -63.5(7) . . . . ? C5 C4 C7 C10 -8.7(8) . . . . ? C3 C4 C7 C10 172.9(5) . . . . ? C5 C4 C7 C9 -125.7(6) . . . . ? C3 C4 C7 C9 55.9(7) . . . . ? C1 C6 C11 C12 -90.7(5) . . . . ? C5 C6 C11 C12 85.2(5) . . . . ? C6 C11 C12 C17 77.7(5) . . . . ? C6 C11 C12 C13 -103.1(5) . . . . ? C17 C12 C13 C14 2.7(7) . . . . ? C11 C12 C13 C14 -176.6(4) . . . . ? C12 C13 C14 C15 2.1(7) . . . . ? C12 C13 C14 C18 -179.4(4) . . . . ? C13 C14 C15 C16 -3.1(7) . . . . ? C18 C14 C15 C16 178.3(4) . . . . ? C14 C15 C16 C17 -0.8(7) . . . . ? C14 C15 C16 C22 177.3(4) . . . . ? C15 C16 C17 C12 5.9(6) . . . . ? C22 C16 C17 C12 -172.0(4) . . . . ? C15 C16 C17 O2 177.4(4) . . . . ? C22 C16 C17 O2 -0.6(6) . . . . ? C13 C12 C17 C16 -6.8(6) . . . . ? C11 C12 C17 C16 172.4(4) . . . . ? C13 C12 C17 O2 -177.8(4) . . . . ? C11 C12 C17 O2 1.4(6) . . . . ? C13 C14 C18 C20 121.8(6) . . . . ? C15 C14 C18 C20 -59.7(7) . . . . ? C13 C14 C18 C19 -116.0(6) . . . . ? C15 C14 C18 C19 62.5(7) . . . . ? C13 C14 C18 C21 0.9(8) . . . . ? C15 C14 C18 C21 179.4(6) . . . . ? C17 C16 C22 C23 -75.5(5) . . . . ? C15 C16 C22 C23 106.5(4) . . . . ? C16 C22 C23 C24 103.0(5) . . . . ? C16 C22 C23 C28 -67.4(5) . . . . ? C28 C23 C24 O5 -178.3(4) . . . . ? C22 C23 C24 O5 11.1(7) . . . . ? C28 C23 C24 C25 7.7(7) . . . . ? C22 C23 C24 C25 -162.8(4) . . . . ? C23 C24 C25 C26 -6.7(7) . . . . ? O5 C24 C25 C26 179.1(4) . . . . ? C23 C24 C25 C33 172.2(4) . . . . ? O5 C24 C25 C33 -2.0(6) . . . . ? C24 C25 C26 C27 -0.3(7) . . . . ? C33 C25 C26 C27 -179.1(4) . . . . ? C25 C26 C27 C28 5.6(7) . . . . ? C25 C26 C27 C29 -173.9(4) . . . . ? C24 C23 C28 C27 -2.1(7) . . . . ? C22 C23 C28 C27 168.7(4) . . . . ? C26 C27 C28 C23 -4.3(7) . . . . ? C29 C27 C28 C23 175.2(4) . . . . ? C26 C27 C29 C30 112.5(5) . . . . ? C28 C27 C29 C30 -67.0(5) . . . . ? C26 C27 C29 C31 -128.5(5) . . . . ? C28 C27 C29 C31 52.0(6) . . . . ? C26 C27 C29 C32 -8.1(7) . . . . ? C28 C27 C29 C32 172.4(5) . . . . ? C26 C25 C33 C34 74.9(5) . . . . ? C24 C25 C33 C34 -103.9(5) . . . . ? C25 C33 C34 C35 -134.7(4) . . . . ? C25 C33 C34 C39 49.9(6) . . . . ? C39 C34 C35 C36 0.2(6) . . . . ? C33 C34 C35 C36 -175.5(4) . . . . ? C34 C35 C36 C37 -0.8(6) . . . . ? C34 C35 C36 C40 -179.5(4) . . . . ? C35 C36 C37 C38 1.4(6) . . . . ? C40 C36 C37 C38 -179.9(4) . . . . ? C36 C37 C38 C39 -1.4(6) . . . . ? C36 C37 C38 C44 174.5(4) . . . . ? C37 C38 C39 C34 0.8(6) . . . . ? C44 C38 C39 C34 -174.7(4) . . . . ? C37 C38 C39 O3 -172.6(4) . . . . ? C44 C38 C39 O3 11.9(6) . . . . ? C35 C34 C39 C38 -0.2(6) . . . . ? C33 C34 C39 C38 175.2(4) . . . . ? C35 C34 C39 O3 173.4(4) . . . . ? C33 C34 C39 O3 -11.2(6) . . . . ? C35 C36 C40 C42 -134.4(5) . . . . ? C37 C36 C40 C42 47.0(6) . . . . ? C35 C36 C40 C43 106.1(5) . . . . ? C37 C36 C40 C43 -72.5(5) . . . . ? C35 C36 C40 C41 -13.9(6) . . . . ? C37 C36 C40 C41 167.4(4) . . . . ? C3 C2 C44 C38 -96.9(6) . . . . ? C1 C2 C44 C38 86.1(5) . . . . ? C39 C38 C44 C2 -49.1(6) . . . . ? C37 C38 C44 C2 135.3(4) . . . . ? Pd C45 C46 C47 172.6(4) . . . . ? Pd C45 C46 C51 -6.2(6) . . . . ? C51 C46 C47 C48 -1.0(8) . . . . ? C45 C46 C47 C48 -179.9(5) . . . . ? C46 C47 C48 C49 -0.9(9) . . . . ? C47 C48 C49 C50 1.4(10) . . . . ? C48 C49 C50 C54 179.6(6) . . . . ? C48 C49 C50 C51 -0.1(9) . . . . ? C47 C46 C51 N1 -177.0(4) . . . . ? C45 C46 C51 N1 2.0(7) . . . . ? C47 C46 C51 C50 2.4(7) . . . . ? C45 C46 C51 C50 -178.7(4) . . . . ? C54 C50 C51 N1 -2.2(7) . . . . ? C49 C50 C51 N1 177.5(5) . . . . ? C54 C50 C51 C46 178.5(5) . . . . ? C49 C50 C51 C46 -1.8(7) . . . . ? N1 C52 C53 C54 -1.4(8) . . . . ? C52 C53 C54 C50 1.2(8) . . . . ? C51 C50 C54 C53 0.5(8) . . . . ? C49 C50 C54 C53 -179.2(6) . . . . ? O4 C55 C56 O5 -26.2(5) . . . . ? N2 C55 C56 O5 153.6(4) . . . . ? C46 C45 Pd N1 5.9(3) . . . . ? C46 C45 Pd O4 32.5(14) . . . . ? C46 C45 Pd P -176.2(3) . . . . ? C53 C52 N1 C51 -0.4(7) . . . . ? C53 C52 N1 Pd 177.5(4) . . . . ? C46 C51 N1 C52 -178.5(4) . . . . ? C50 C51 N1 C52 2.2(7) . . . . ? C46 C51 N1 Pd 3.3(5) . . . . ? C50 C51 N1 Pd -176.0(4) . . . . ? C45 Pd N1 C52 176.5(4) . . . . ? O4 Pd N1 C52 0.3(4) . . . . ? P Pd N1 C52 157.9(7) . . . . ? C45 Pd N1 C51 -5.4(3) . . . . ? O4 Pd N1 C51 178.3(3) . . . . ? P Pd N1 C51 -24.1(11) . . . . ? O4 C55 N2 C59 -176.2(4) . . . . ? C56 C55 N2 C59 4.1(6) . . . . ? O4 C55 N2 C57 -1.5(6) . . . . ? C56 C55 N2 C57 178.8(4) . . . . ? C60 C59 N2 C55 -118.1(5) . . . . ? C60 C59 N2 C57 67.1(5) . . . . ? C58 C57 N2 C55 75.1(5) . . . . ? C58 C57 N2 C59 -109.6(5) . . . . ? C45 Pd P O2 -167.39(19) . . . . ? N1 Pd P O2 -148.8(9) . . . . ? O4 Pd P O2 8.58(15) . . . . ? C45 Pd P O1 -49.0(2) . . . . ? N1 Pd P O1 -30.5(9) . . . . ? O4 Pd P O1 126.94(15) . . . . ? C45 Pd P O3 71.6(2) . . . . ? N1 Pd P O3 90.2(9) . . . . ? O4 Pd P O3 -112.40(16) . . . . ? C6 C1 O1 P 91.9(4) . . . . ? C2 C1 O1 P -90.0(5) . . . . ? O2 P O1 C1 -70.1(3) . . . . ? O3 P O1 C1 38.2(3) . . . . ? Pd P O1 C1 169.4(3) . . . . ? C16 C17 O2 P 136.6(4) . . . . ? C12 C17 O2 P -51.9(7) . . . . ? O1 P O2 C17 47.4(5) . . . . ? O3 P O2 C17 -60.0(5) . . . . ? Pd P O2 C17 168.9(4) . . . . ? C38 C39 O3 P -73.6(5) . . . . ? C34 C39 O3 P 112.9(4) . . . . ? O2 P O3 C39 -171.2(3) . . . . ? O1 P O3 C39 78.2(4) . . . . ? Pd P O3 C39 -47.0(4) . . . . ? N2 C55 O4 Pd 165.3(3) . . . . ? C56 C55 O4 Pd -15.0(6) . . . . ? C45 Pd O4 C55 -123.4(11) . . . . ? N1 Pd O4 C55 -97.1(4) . . . . ? P Pd O4 C55 85.5(4) . . . . ? C23 C24 O5 C56 59.6(5) . . . . ? C25 C24 O5 C56 -126.3(4) . . . . ? C55 C56 O5 C24 -130.2(3) . . . . ? C84 C82 C83 C80 169.5(14) . . . . ? C83 C82 C84 C85 -164.9(15) . . . . ? C82 C84 C85 C81 -172.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.562 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.111