Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Robin Bedford' 'Michael Betham' 'Michael E. Blake' 'Robert M. Forst' 'Peter N. Horton' 'Michael B. Hursthouse' 'Rosa-Maria Lopez-Nicolas' _publ_contact_author_name 'Dr Robin Bedford' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email R.BEDFORD@BRISTOL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; N-Heterocyclic carbene adducts of orthopalladated triarylphosphite complexes. ; data_2005src0244 _database_code_depnum_ccdc_archive 'CCDC 271192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. R. B. Bedford ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H100 Cl N2 O3 P Pd' _chemical_formula_sum 'C69 H100 Cl N2 O3 P Pd' _chemical_formula_weight 1178.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 21.0783(16) _cell_length_b 21.0783(16) _cell_length_c 29.741(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13214(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15462 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Cut Shard' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5040 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9122 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BrukerNonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91295 _diffrn_reflns_av_R_equivalents 0.1204 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15144 _reflns_number_gt 11568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+4.9833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(16) _refine_ls_number_reflns 15144 _refine_ls_number_parameters 760 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.65650(4) 0.07535(4) -0.00522(3) 0.02558(19) Uani 1 1 d . . . Pd1 Pd 0.624689(11) 0.171855(11) 0.029545(8) 0.01830(6) Uani 1 1 d . . . C1 C 0.61291(14) 0.31181(14) 0.02397(11) 0.0229(8) Uani 1 1 d . . . C2 C 0.58923(15) 0.25913(14) 0.04612(10) 0.0201(7) Uani 1 1 d . . . C3 C 0.53762(15) 0.26966(15) 0.07439(10) 0.0219(7) Uani 1 1 d . . . H3 H 0.5202 0.2347 0.0903 0.026 Uiso 1 1 calc R . . C4 C 0.51054(15) 0.32949(16) 0.08024(11) 0.0274(8) Uani 1 1 d . . . C5 C 0.54009(16) 0.38013(17) 0.05982(12) 0.0319(9) Uani 1 1 d . . . H5 H 0.5239 0.4215 0.0654 0.038 Uiso 1 1 calc R . . C6 C 0.59215(15) 0.37414(16) 0.03161(12) 0.0317(8) Uani 1 1 d . . . C7 C 0.44930(15) 0.33999(16) 0.10751(11) 0.0298(8) Uani 1 1 d . . . C8 C 0.42320(16) 0.27878(17) 0.12825(12) 0.0358(9) Uani 1 1 d . . . H8A H 0.4551 0.2603 0.1483 0.054 Uiso 1 1 calc R . . H8B H 0.4131 0.2485 0.1043 0.054 Uiso 1 1 calc R . . H8C H 0.3847 0.2884 0.1454 0.054 Uiso 1 1 calc R . . C9 C 0.39794(16) 0.36827(17) 0.07629(13) 0.0425(10) Uani 1 1 d . . . H9A H 0.3591 0.3758 0.0936 0.064 Uiso 1 1 calc R . . H9B H 0.3890 0.3385 0.0518 0.064 Uiso 1 1 calc R . . H9C H 0.4131 0.4085 0.0637 0.064 Uiso 1 1 calc R . . C10 C 0.46139(17) 0.38671(18) 0.14598(13) 0.0436(11) Uani 1 1 d . . . H10A H 0.4958 0.3707 0.1650 0.065 Uiso 1 1 calc R . . H10B H 0.4227 0.3912 0.1640 0.065 Uiso 1 1 calc R . . H10C H 0.4733 0.4281 0.1336 0.065 Uiso 1 1 calc R . . C11 C 0.6236(2) 0.43186(17) 0.00866(14) 0.0488(11) Uani 1 1 d . . . C12 C 0.6012(3) 0.49433(18) 0.03156(19) 0.0856(18) Uani 1 1 d . . . H12A H 0.6087 0.4917 0.0640 0.128 Uiso 1 1 calc R . . H12B H 0.5558 0.5005 0.0259 0.128 Uiso 1 1 calc R . . H12C H 0.6249 0.5302 0.0191 0.128 Uiso 1 1 calc R . . C13 C 0.60457(19) 0.4319(2) -0.04054(15) 0.0642(15) Uani 1 1 d . . . H13A H 0.6285 0.4648 -0.0565 0.096 Uiso 1 1 calc R . . H13B H 0.5590 0.4406 -0.0431 0.096 Uiso 1 1 calc R . . H13C H 0.6139 0.3904 -0.0538 0.096 Uiso 1 1 calc R . . C14 C 0.69562(19) 0.43112(18) 0.01411(15) 0.0570(13) Uani 1 1 d . . . H14A H 0.7133 0.3951 -0.0025 0.086 Uiso 1 1 calc R . . H14B H 0.7064 0.4271 0.0460 0.086 Uiso 1 1 calc R . . H14C H 0.7134 0.4707 0.0023 0.086 Uiso 1 1 calc R . . C21 C 0.65689(14) 0.22907(14) -0.09589(10) 0.0210(8) Uani 1 1 d . . . C22 C 0.60424(15) 0.19126(15) -0.09210(10) 0.0248(8) Uani 1 1 d . . . H22 H 0.6019 0.1607 -0.0687 0.030 Uiso 1 1 calc R . . C23 C 0.55467(15) 0.19743(15) -0.12211(11) 0.0238(8) Uani 1 1 d . . . H23 H 0.5183 0.1711 -0.1193 0.029 Uiso 1 1 calc R . . C24 C 0.55774(15) 0.24185(15) -0.15627(10) 0.0228(7) Uani 1 1 d . . . C25 C 0.61376(15) 0.27643(15) -0.16037(11) 0.0228(8) Uani 1 1 d . . . H25 H 0.6171 0.3053 -0.1848 0.027 Uiso 1 1 calc R . . C26 C 0.66509(15) 0.27180(14) -0.13133(10) 0.0207(7) Uani 1 1 d . . . C27 C 0.50336(15) 0.25364(16) -0.18893(11) 0.0265(8) Uani 1 1 d D . . C28 C 0.52225(18) 0.2365(2) -0.23656(11) 0.0463(11) Uani 1 1 d D . . H28A H 0.5316 0.1911 -0.2382 0.069 Uiso 1 1 calc R . . H28B H 0.5600 0.2608 -0.2452 0.069 Uiso 1 1 calc R . . H28C H 0.4873 0.2467 -0.2571 0.069 Uiso 1 1 calc R . . C29 C 0.4846(2) 0.32391(19) -0.18688(15) 0.0645(14) Uani 1 1 d D . . H29A H 0.4468 0.3309 -0.2054 0.097 Uiso 1 1 calc R . . H29B H 0.5196 0.3500 -0.1983 0.097 Uiso 1 1 calc R . . H29C H 0.4755 0.3357 -0.1557 0.097 Uiso 1 1 calc R . . C30 C 0.44401(17) 0.2156(2) -0.17702(13) 0.0586(13) Uani 1 1 d D . . H30A H 0.4098 0.2263 -0.1980 0.088 Uiso 1 1 calc R . . H30B H 0.4308 0.2258 -0.1463 0.088 Uiso 1 1 calc R . . H30C H 0.4534 0.1701 -0.1791 0.088 Uiso 1 1 calc R . . C31 C 0.72741(15) 0.30840(15) -0.13956(11) 0.0267(8) Uani 1 1 d . . . C32 C 0.72363(17) 0.34857(17) -0.18230(12) 0.0376(10) Uani 1 1 d . . . H32A H 0.7634 0.3720 -0.1862 0.056 Uiso 1 1 calc R . . H32B H 0.6883 0.3786 -0.1798 0.056 Uiso 1 1 calc R . . H32C H 0.7168 0.3208 -0.2083 0.056 Uiso 1 1 calc R . . C33 C 0.78203(15) 0.26150(16) -0.14503(12) 0.0336(9) Uani 1 1 d . . . H33A H 0.8211 0.2847 -0.1520 0.050 Uiso 1 1 calc R . . H33B H 0.7723 0.2320 -0.1695 0.050 Uiso 1 1 calc R . . H33C H 0.7877 0.2377 -0.1170 0.050 Uiso 1 1 calc R . . C34 C 0.74338(17) 0.35383(16) -0.10078(12) 0.0412(10) Uani 1 1 d . . . H34A H 0.7469 0.3297 -0.0727 0.062 Uiso 1 1 calc R . . H34B H 0.7097 0.3856 -0.0979 0.062 Uiso 1 1 calc R . . H34C H 0.7838 0.3751 -0.1070 0.062 Uiso 1 1 calc R . . C41 C 0.80318(14) 0.20373(14) 0.02082(10) 0.0205(8) Uani 1 1 d . A . C42 C 0.80499(15) 0.14439(15) 0.00200(11) 0.0258(8) Uani 1 1 d . . . H42 H 0.7757 0.1332 -0.0209 0.031 Uiso 1 1 calc R . . C43 C 0.84953(15) 0.10103(15) 0.01642(11) 0.0281(9) Uani 1 1 d . A . H43 H 0.8507 0.0600 0.0033 0.034 Uiso 1 1 calc R . . C44 C 0.89251(15) 0.11661(16) 0.04987(11) 0.0259(8) Uani 1 1 d D . . C45 C 0.88974(14) 0.17753(16) 0.06705(11) 0.0276(8) Uani 1 1 d . A . H45 H 0.9195 0.1888 0.0896 0.033 Uiso 1 1 calc R . . C46 C 0.84652(14) 0.22334(16) 0.05361(11) 0.0241(8) Uani 1 1 d . . . C47 C 0.9429(7) 0.0702(7) 0.0675(5) 0.0356(11) Uani 0.422(16) 1 d PDU A 1 C48 C 0.9650(10) 0.0849(6) 0.1155(4) 0.063(6) Uani 0.422(16) 1 d PD A 1 H48A H 0.9930 0.0509 0.1260 0.095 Uiso 0.422(16) 1 calc PR A 1 H48B H 0.9280 0.0879 0.1354 0.095 Uiso 0.422(16) 1 calc PR A 1 H48C H 0.9880 0.1252 0.1157 0.095 Uiso 0.422(16) 1 calc PR A 1 C49 C 0.9162(7) 0.0023(6) 0.0676(7) 0.051(5) Uani 0.422(16) 1 d PD A 1 H49A H 0.9064 -0.0106 0.0367 0.076 Uiso 0.422(16) 1 calc PR A 1 H49B H 0.8775 0.0008 0.0858 0.076 Uiso 0.422(16) 1 calc PR A 1 H49C H 0.9478 -0.0267 0.0803 0.076 Uiso 0.422(16) 1 calc PR A 1 C50 C 0.9992(6) 0.0724(8) 0.0354(6) 0.057(5) Uani 0.422(16) 1 d PD A 1 H50A H 1.0315 0.0420 0.0453 0.085 Uiso 0.422(16) 1 calc PR A 1 H50B H 1.0173 0.1152 0.0352 0.085 Uiso 0.422(16) 1 calc PR A 1 H50C H 0.9850 0.0612 0.0050 0.085 Uiso 0.422(16) 1 calc PR A 1 C147 C 0.9399(5) 0.0675(6) 0.0669(4) 0.0356(10) Uani 0.578(16) 1 d PDU A 2 C148 C 0.9264(5) 0.0564(6) 0.1168(3) 0.055(3) Uani 0.578(16) 1 d PD A 2 H14D H 0.9580 0.0272 0.1292 0.082 Uiso 0.578(16) 1 calc PR A 2 H14E H 0.8839 0.0380 0.1203 0.082 Uiso 0.578(16) 1 calc PR A 2 H14F H 0.9284 0.0969 0.1329 0.082 Uiso 0.578(16) 1 calc PR A 2 C149 C 0.9330(8) 0.0037(6) 0.0426(5) 0.089(5) Uani 0.578(16) 1 d PD A 2 H14G H 0.9421 0.0093 0.0105 0.134 Uiso 0.578(16) 1 calc PR A 2 H14H H 0.8896 -0.0121 0.0463 0.134 Uiso 0.578(16) 1 calc PR A 2 H14I H 0.9629 -0.0269 0.0555 0.134 Uiso 0.578(16) 1 calc PR A 2 C150 C 1.0072(4) 0.0932(6) 0.0632(5) 0.069(4) Uani 0.578(16) 1 d PD A 2 H15A H 1.0197 0.0949 0.0315 0.104 Uiso 0.578(16) 1 calc PR A 2 H15B H 1.0363 0.0652 0.0796 0.104 Uiso 0.578(16) 1 calc PR A 2 H15C H 1.0089 0.1359 0.0762 0.104 Uiso 0.578(16) 1 calc PR A 2 C51 C 0.84590(15) 0.29054(15) 0.07351(11) 0.0287(8) Uani 1 1 d . A . C52 C 0.85794(15) 0.33927(14) 0.03637(12) 0.0347(9) Uani 1 1 d . . . H52A H 0.9004 0.3327 0.0238 0.052 Uiso 1 1 calc R A . H52B H 0.8550 0.3821 0.0489 0.052 Uiso 1 1 calc R . . H52C H 0.8261 0.3342 0.0126 0.052 Uiso 1 1 calc R . . C53 C 0.78265(16) 0.30319(16) 0.09712(12) 0.0340(9) Uani 1 1 d . . . H53A H 0.7485 0.3043 0.0748 0.051 Uiso 1 1 calc R A . H53B H 0.7847 0.3441 0.1128 0.051 Uiso 1 1 calc R . . H53C H 0.7743 0.2694 0.1189 0.051 Uiso 1 1 calc R . . C54 C 0.89886(18) 0.29802(18) 0.10863(14) 0.0517(12) Uani 1 1 d . . . H54A H 0.8911 0.2690 0.1338 0.078 Uiso 1 1 calc R A . H54B H 0.8993 0.3418 0.1197 0.078 Uiso 1 1 calc R . . H54C H 0.9399 0.2881 0.0948 0.078 Uiso 1 1 calc R . . O1 O 0.65993(10) 0.30312(9) -0.00924(7) 0.0239(5) Uani 1 1 d . . . O21 O 0.70485(10) 0.22462(10) -0.06289(7) 0.0225(5) Uani 1 1 d . . . O41 O 0.75785(9) 0.24775(9) 0.00665(7) 0.0229(5) Uani 1 1 d . . . P1 P 0.68817(4) 0.23300(4) -0.01084(3) 0.02039(19) Uani 1 1 d . A . C61 C 0.56778(14) 0.13039(14) 0.07764(10) 0.0178(7) Uani 1 1 d . . . C62 C 0.47772(15) 0.09226(16) 0.11549(10) 0.0254(8) Uani 1 1 d . . . H62A H 0.4678 0.0467 0.1195 0.030 Uiso 1 1 calc R . . H62B H 0.4380 0.1171 0.1173 0.030 Uiso 1 1 calc R . . C63 C 0.52599(14) 0.11487(16) 0.15008(11) 0.0262(8) Uani 1 1 d . . . H63A H 0.5088 0.1503 0.1683 0.031 Uiso 1 1 calc R . . H63B H 0.5388 0.0799 0.1704 0.031 Uiso 1 1 calc R . . C64 C 0.48553(14) 0.07871(15) 0.03066(11) 0.0223(7) Uani 1 1 d . . . C65 C 0.45131(14) 0.11772(16) 0.00154(11) 0.0235(8) Uani 1 1 d . . . C66 C 0.42897(15) 0.09082(16) -0.03834(11) 0.0299(9) Uani 1 1 d . . . H66 H 0.4073 0.1169 -0.0594 0.036 Uiso 1 1 calc R . . C67 C 0.43748(16) 0.02779(17) -0.04792(11) 0.0319(9) Uani 1 1 d . . . H67 H 0.4218 0.0106 -0.0753 0.038 Uiso 1 1 calc R . . C68 C 0.46883(16) -0.01035(17) -0.01775(11) 0.0309(8) Uani 1 1 d . . . H68 H 0.4735 -0.0542 -0.0243 0.037 Uiso 1 1 calc R . . C69 C 0.49382(14) 0.01349(15) 0.02193(11) 0.0243(8) Uani 1 1 d . . . C70 C 0.43368(14) 0.18555(15) 0.01234(11) 0.0255(8) Uani 1 1 d . . . H70 H 0.4564 0.1975 0.0406 0.031 Uiso 1 1 calc R . . C71 C 0.45328(16) 0.23257(16) -0.02384(12) 0.0356(9) Uani 1 1 d . . . H71A H 0.4990 0.2290 -0.0292 0.053 Uiso 1 1 calc R . . H71B H 0.4432 0.2757 -0.0139 0.053 Uiso 1 1 calc R . . H71C H 0.4302 0.2233 -0.0517 0.053 Uiso 1 1 calc R . . C72 C 0.36208(15) 0.18962(16) 0.02193(12) 0.0370(9) Uani 1 1 d . . . H72A H 0.3506 0.2336 0.0288 0.056 Uiso 1 1 calc R . . H72B H 0.3516 0.1625 0.0477 0.056 Uiso 1 1 calc R . . H72C H 0.3384 0.1753 -0.0045 0.056 Uiso 1 1 calc R . . C73 C 0.52613(16) -0.03231(16) 0.05374(11) 0.0279(8) Uani 1 1 d . . . H73 H 0.5450 -0.0074 0.0790 0.034 Uiso 1 1 calc R . . C74 C 0.57929(16) -0.06945(16) 0.03058(13) 0.0374(9) Uani 1 1 d . . . H74A H 0.5612 -0.0964 0.0070 0.056 Uiso 1 1 calc R . . H74B H 0.6011 -0.0961 0.0527 0.056 Uiso 1 1 calc R . . H74C H 0.6096 -0.0397 0.0172 0.056 Uiso 1 1 calc R . . C75 C 0.47790(18) -0.07908(17) 0.07341(12) 0.0399(9) Uani 1 1 d . . . H75A H 0.4450 -0.0556 0.0897 0.060 Uiso 1 1 calc R . . H75B H 0.4995 -0.1081 0.0941 0.060 Uiso 1 1 calc R . . H75C H 0.4584 -0.1035 0.0490 0.060 Uiso 1 1 calc R . . C76 C 0.64171(14) 0.14619(15) 0.14169(10) 0.0212(7) Uani 1 1 d . . . C77 C 0.68834(16) 0.09906(16) 0.13601(11) 0.0258(8) Uani 1 1 d . . . C78 C 0.74624(17) 0.10803(17) 0.15788(13) 0.0358(9) Uani 1 1 d . . . H78 H 0.7790 0.0776 0.1538 0.043 Uiso 1 1 calc R . . C79 C 0.75732(18) 0.15944(18) 0.18503(13) 0.0438(11) Uani 1 1 d . . . H79 H 0.7969 0.1640 0.1999 0.053 Uiso 1 1 calc R . . C80 C 0.71102(17) 0.20392(17) 0.19050(12) 0.0360(10) Uani 1 1 d . . . H80 H 0.7191 0.2391 0.2096 0.043 Uiso 1 1 calc R . . C81 C 0.65205(16) 0.19973(16) 0.16904(11) 0.0261(8) Uani 1 1 d . . . C82 C 0.67644(16) 0.03771(14) 0.11113(11) 0.0229(7) Uani 1 1 d . . . H82 H 0.6447 0.0463 0.0869 0.028 Uiso 1 1 calc R . . C83 C 0.64776(17) -0.01069(16) 0.14328(12) 0.0361(9) Uani 1 1 d . . . H83A H 0.6769 -0.0178 0.1684 0.054 Uiso 1 1 calc R . . H83B H 0.6407 -0.0507 0.1273 0.054 Uiso 1 1 calc R . . H83C H 0.6073 0.0054 0.1548 0.054 Uiso 1 1 calc R . . C84 C 0.73620(16) 0.00939(18) 0.08906(12) 0.0397(10) Uani 1 1 d . . . H84A H 0.7580 0.0423 0.0717 0.059 Uiso 1 1 calc R . . H84B H 0.7239 -0.0254 0.0690 0.059 Uiso 1 1 calc R . . H84C H 0.7647 -0.0068 0.1124 0.059 Uiso 1 1 calc R . . C85 C 0.60508(16) 0.25258(15) 0.17624(11) 0.0270(8) Uani 1 1 d . . . H85 H 0.5674 0.2438 0.1568 0.032 Uiso 1 1 calc R . . C86 C 0.58209(17) 0.25504(17) 0.22507(12) 0.0401(10) Uani 1 1 d . . . H86A H 0.5633 0.2141 0.2332 0.060 Uiso 1 1 calc R . . H86B H 0.5502 0.2886 0.2283 0.060 Uiso 1 1 calc R . . H86C H 0.6181 0.2640 0.2449 0.060 Uiso 1 1 calc R . . C87 C 0.63273(16) 0.31676(15) 0.16173(12) 0.0339(9) Uani 1 1 d . . . H87A H 0.6703 0.3263 0.1799 0.051 Uiso 1 1 calc R . . H87B H 0.6009 0.3500 0.1661 0.051 Uiso 1 1 calc R . . H87C H 0.6446 0.3149 0.1299 0.051 Uiso 1 1 calc R . . N61 N 0.51102(12) 0.10368(12) 0.07235(8) 0.0199(6) Uani 1 1 d . . . N62 N 0.57995(11) 0.13616(12) 0.12189(8) 0.0182(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0325(5) 0.0196(4) 0.0246(5) -0.0007(4) 0.0025(4) -0.0001(3) Pd1 0.01969(13) 0.01740(12) 0.01781(11) 0.00089(11) -0.00032(11) -0.00059(11) C1 0.0185(17) 0.0260(18) 0.0241(19) 0.0035(15) -0.0015(15) 0.0012(14) C2 0.0231(18) 0.0162(16) 0.0210(19) -0.0017(14) -0.0062(15) 0.0006(14) C3 0.0242(19) 0.0202(18) 0.0213(19) -0.0005(15) -0.0053(15) -0.0012(15) C4 0.0272(18) 0.0264(18) 0.029(2) -0.0018(17) -0.0052(15) 0.0051(17) C5 0.033(2) 0.0211(19) 0.041(2) -0.0053(18) -0.0007(18) 0.0037(17) C6 0.0336(19) 0.0205(17) 0.041(2) 0.0029(19) 0.0010(18) 0.0022(16) C7 0.0266(19) 0.027(2) 0.036(2) -0.0078(17) -0.0039(17) 0.0078(16) C8 0.027(2) 0.039(2) 0.041(2) -0.0115(19) 0.0071(18) 0.0051(18) C9 0.033(2) 0.039(2) 0.055(3) -0.002(2) 0.0017(19) 0.0106(19) C10 0.034(2) 0.045(3) 0.053(3) -0.016(2) 0.0046(19) 0.0034(19) C11 0.057(3) 0.026(2) 0.064(3) 0.016(2) 0.008(3) 0.011(2) C12 0.110(4) 0.022(2) 0.125(5) 0.017(3) 0.047(4) 0.005(3) C13 0.041(3) 0.067(3) 0.085(4) 0.050(3) 0.014(2) 0.017(2) C14 0.061(3) 0.030(2) 0.081(4) 0.004(2) 0.012(3) -0.014(2) C21 0.0224(18) 0.0221(17) 0.0185(18) 0.0002(14) -0.0032(15) -0.0007(15) C22 0.0289(19) 0.0279(19) 0.0176(18) 0.0052(15) -0.0012(15) -0.0037(14) C23 0.0204(18) 0.0285(19) 0.023(2) 0.0004(16) 0.0002(15) -0.0059(15) C24 0.0221(18) 0.027(2) 0.0188(18) -0.0022(16) 0.0043(15) 0.0053(15) C25 0.0240(19) 0.0215(17) 0.0230(19) 0.0025(15) 0.0044(15) 0.0049(15) C26 0.0196(17) 0.0199(17) 0.0226(19) 0.0016(14) 0.0030(15) 0.0026(15) C27 0.0254(19) 0.032(2) 0.022(2) 0.0017(16) -0.0027(15) 0.0075(16) C28 0.038(2) 0.074(3) 0.027(2) -0.012(2) -0.0019(18) 0.004(2) C29 0.060(3) 0.051(3) 0.082(3) -0.017(3) -0.039(3) 0.026(2) C30 0.032(2) 0.101(4) 0.042(3) 0.021(3) -0.012(2) -0.011(2) C31 0.0264(18) 0.030(2) 0.024(2) 0.0072(16) 0.0024(16) -0.0033(16) C32 0.031(2) 0.045(2) 0.038(2) 0.0206(19) 0.0050(18) -0.0004(18) C33 0.0243(19) 0.036(2) 0.041(2) 0.0064(18) 0.0034(17) -0.0035(17) C34 0.043(2) 0.036(2) 0.045(3) -0.0011(19) 0.009(2) -0.0166(19) C41 0.0190(17) 0.0202(17) 0.022(2) 0.0031(15) -0.0007(15) 0.0035(14) C42 0.0275(19) 0.0249(19) 0.025(2) -0.0014(16) -0.0022(16) -0.0023(16) C43 0.035(2) 0.0147(17) 0.035(2) -0.0038(15) 0.0013(17) -0.0001(15) C44 0.0246(18) 0.029(2) 0.0237(19) 0.0022(16) 0.0012(15) 0.0010(16) C45 0.0230(19) 0.034(2) 0.0256(19) -0.0037(17) -0.0059(15) 0.0037(17) C46 0.0183(18) 0.0307(19) 0.0232(19) -0.0022(16) 0.0017(15) 0.0006(15) C47 0.034(3) 0.032(2) 0.040(3) 0.004(2) -0.001(2) 0.012(2) C48 0.091(14) 0.047(8) 0.052(8) 0.001(6) -0.047(9) 0.017(8) C49 0.042(7) 0.025(6) 0.086(14) 0.002(8) -0.016(8) 0.011(5) C50 0.026(6) 0.069(10) 0.076(11) 0.033(9) 0.014(8) 0.025(6) C147 0.034(2) 0.032(2) 0.040(3) 0.004(2) -0.001(2) 0.011(2) C148 0.047(6) 0.073(8) 0.044(5) 0.010(5) -0.012(5) 0.022(5) C149 0.120(13) 0.072(7) 0.074(10) -0.010(8) -0.030(8) 0.066(8) C150 0.038(5) 0.112(9) 0.057(9) 0.022(7) 0.005(6) 0.043(6) C51 0.026(2) 0.029(2) 0.031(2) -0.0108(17) -0.0030(16) -0.0003(15) C52 0.0303(19) 0.0198(18) 0.054(2) -0.0074(17) 0.0074(18) -0.0027(14) C53 0.036(2) 0.034(2) 0.031(2) -0.0058(17) 0.0039(17) 0.0054(18) C54 0.048(3) 0.040(2) 0.066(3) -0.029(2) -0.025(2) 0.010(2) O1 0.0232(12) 0.0193(11) 0.0292(13) 0.0066(10) 0.0008(11) 0.0004(10) O21 0.0216(12) 0.0266(12) 0.0193(13) 0.0034(10) 0.0000(10) -0.0009(10) O41 0.0211(12) 0.0204(12) 0.0272(13) 0.0008(10) -0.0071(10) -0.0004(10) P1 0.0206(5) 0.0195(5) 0.0211(5) 0.0028(4) -0.0015(4) -0.0007(3) C61 0.0243(17) 0.0109(15) 0.0180(17) -0.0014(14) -0.0006(14) 0.0029(14) C62 0.0235(18) 0.032(2) 0.0204(19) -0.0018(16) 0.0028(15) -0.0091(16) C63 0.0251(18) 0.031(2) 0.0228(19) -0.0033(16) 0.0022(15) -0.0057(16) C64 0.0193(16) 0.0310(18) 0.0164(17) -0.0014(16) 0.0009(15) -0.0062(15) C65 0.0205(17) 0.0305(19) 0.0195(18) -0.0005(16) 0.0004(14) -0.0019(16) C66 0.0283(19) 0.037(2) 0.024(2) 0.0005(17) -0.0031(16) -0.0007(17) C67 0.034(2) 0.041(2) 0.021(2) -0.0120(18) -0.0034(17) -0.0071(18) C68 0.033(2) 0.030(2) 0.029(2) -0.0068(17) -0.0002(17) -0.0037(16) C69 0.0224(17) 0.0284(19) 0.022(2) -0.0020(16) 0.0028(15) -0.0041(15) C70 0.0224(18) 0.031(2) 0.023(2) -0.0014(16) -0.0021(15) -0.0005(15) C71 0.038(2) 0.036(2) 0.033(2) 0.0028(19) -0.0031(18) 0.0042(18) C72 0.027(2) 0.040(2) 0.044(2) -0.0080(18) 0.0003(18) -0.0005(16) C73 0.030(2) 0.031(2) 0.0222(19) -0.0050(16) -0.0018(16) -0.0043(17) C74 0.041(2) 0.034(2) 0.037(2) 0.0023(19) 0.001(2) 0.0060(18) C75 0.048(3) 0.039(2) 0.033(2) 0.0030(19) 0.0030(19) -0.006(2) C76 0.0213(18) 0.0253(18) 0.0170(17) 0.0041(14) 0.0020(14) -0.0029(14) C77 0.028(2) 0.0277(19) 0.0219(19) 0.0084(16) 0.0010(16) -0.0027(15) C78 0.027(2) 0.032(2) 0.048(3) 0.0031(19) -0.0095(19) 0.0047(17) C79 0.031(2) 0.040(3) 0.060(3) 0.001(2) -0.020(2) -0.001(2) C80 0.041(2) 0.031(2) 0.036(2) -0.0032(18) -0.0132(18) -0.0062(18) C81 0.028(2) 0.0273(19) 0.0224(19) 0.0020(16) -0.0018(16) -0.0060(15) C82 0.0257(18) 0.0224(17) 0.0206(18) 0.0028(15) -0.0004(16) 0.0029(16) C83 0.046(2) 0.029(2) 0.033(2) 0.0045(17) 0.0014(19) -0.0049(18) C84 0.034(2) 0.046(2) 0.039(2) -0.0037(19) 0.0000(19) 0.0077(19) C85 0.029(2) 0.0283(19) 0.024(2) -0.0028(16) -0.0024(16) -0.0024(16) C86 0.044(2) 0.045(2) 0.031(2) -0.0131(19) 0.006(2) -0.0055(19) C87 0.032(2) 0.030(2) 0.040(2) -0.0043(17) -0.0007(18) 0.0000(18) N61 0.0201(14) 0.0253(15) 0.0141(15) -0.0018(12) 0.0011(12) -0.0046(12) N62 0.0182(14) 0.0229(15) 0.0135(14) 0.0006(12) 0.0011(11) -0.0027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Pd1 2.3784(8) . ? Pd1 C2 2.046(3) . ? Pd1 C61 2.061(3) . ? Pd1 P1 2.2124(8) . ? C1 C2 1.384(4) . ? C1 C6 1.403(4) . ? C1 O1 1.411(4) . ? C2 C3 1.393(4) . ? C3 C4 1.395(4) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 C7 1.540(4) . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? C6 C11 1.544(5) . ? C7 C10 1.531(5) . ? C7 C8 1.532(5) . ? C7 C9 1.546(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.517(6) . ? C11 C14 1.527(5) . ? C11 C12 1.556(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C22 1.371(4) . ? C21 C26 1.397(4) . ? C21 O21 1.412(3) . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 C27 1.523(4) . ? C25 C26 1.388(4) . ? C25 H25 0.9500 . ? C26 C31 1.543(4) . ? C27 C28 1.515(4) . ? C27 C30 1.528(5) . ? C27 C29 1.534(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(4) . ? C31 C32 1.529(4) . ? C31 C34 1.536(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 C42 1.371(4) . ? C41 O41 1.397(3) . ? C41 C46 1.399(4) . ? C42 C43 1.379(4) . ? C42 H42 0.9500 . ? C43 C44 1.385(4) . ? C43 H43 0.9500 . ? C44 C45 1.383(4) . ? C44 C147 1.525(12) . ? C44 C47 1.536(15) . ? C45 C46 1.386(4) . ? C45 H45 0.9500 . ? C46 C51 1.535(4) . ? C47 C50 1.525(13) . ? C47 C48 1.531(13) . ? C47 C49 1.539(13) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C147 C150 1.522(11) . ? C147 C148 1.530(10) . ? C147 C149 1.533(11) . ? C148 H14D 0.9800 . ? C148 H14E 0.9800 . ? C148 H14F 0.9800 . ? C149 H14G 0.9800 . ? C149 H14H 0.9800 . ? C149 H14I 0.9800 . ? C150 H15A 0.9800 . ? C150 H15B 0.9800 . ? C150 H15C 0.9800 . ? C51 C52 1.529(4) . ? C51 C53 1.530(4) . ? C51 C54 1.537(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O1 P1 1.594(2) . ? O21 P1 1.597(2) . ? O41 P1 1.589(2) . ? C61 N61 1.332(4) . ? C61 N62 1.346(3) . ? C62 N61 1.482(4) . ? C62 C63 1.523(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N62 1.482(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.395(4) . ? C64 C69 1.410(4) . ? C64 N61 1.450(4) . ? C65 C66 1.397(4) . ? C65 C70 1.512(4) . ? C66 C67 1.370(5) . ? C66 H66 0.9500 . ? C67 C68 1.374(4) . ? C67 H67 0.9500 . ? C68 C69 1.387(4) . ? C68 H68 0.9500 . ? C69 C73 1.514(4) . ? C70 C71 1.520(4) . ? C70 C72 1.538(4) . ? C70 H70 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.531(4) . ? C73 C75 1.532(4) . ? C73 H73 1.0000 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.407(4) . ? C76 C81 1.408(4) . ? C76 N62 1.444(4) . ? C77 C78 1.396(4) . ? C77 C82 1.511(4) . ? C78 C79 1.371(5) . ? C78 H78 0.9500 . ? C79 C80 1.363(5) . ? C79 H79 0.9500 . ? C80 C81 1.400(5) . ? C80 H80 0.9500 . ? C81 C85 1.506(5) . ? C82 C83 1.523(4) . ? C82 C84 1.541(4) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.532(4) . ? C85 C87 1.535(4) . ? C85 H85 1.0000 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 C61 90.09(12) . . ? C2 Pd1 P1 80.09(9) . . ? C61 Pd1 P1 167.36(8) . . ? C2 Pd1 Cl1 167.63(9) . . ? C61 Pd1 Cl1 95.92(8) . . ? P1 Pd1 Cl1 95.26(3) . . ? C2 C1 C6 124.2(3) . . ? C2 C1 O1 118.8(3) . . ? C6 C1 O1 117.0(3) . . ? C1 C2 C3 116.2(3) . . ? C1 C2 Pd1 118.4(2) . . ? C3 C2 Pd1 125.0(2) . . ? C2 C3 C4 122.6(3) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C7 120.0(3) . . ? C3 C4 C7 122.6(3) . . ? C4 C5 C6 123.7(3) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C1 115.5(3) . . ? C5 C6 C11 122.3(3) . . ? C1 C6 C11 122.2(3) . . ? C10 C7 C8 107.5(3) . . ? C10 C7 C4 110.3(3) . . ? C8 C7 C4 113.1(3) . . ? C10 C7 C9 108.5(3) . . ? C8 C7 C9 108.4(3) . . ? C4 C7 C9 109.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 111.4(4) . . ? C13 C11 C6 108.3(3) . . ? C14 C11 C6 111.8(3) . . ? C13 C11 C12 110.0(4) . . ? C14 C11 C12 105.3(4) . . ? C6 C11 C12 110.1(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 C21 C26 122.5(3) . . ? C22 C21 O21 118.9(3) . . ? C26 C21 O21 118.6(3) . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C25 117.3(3) . . ? C23 C24 C27 122.9(3) . . ? C25 C24 C27 119.8(3) . . ? C26 C25 C24 124.7(3) . . ? C26 C25 H25 117.6 . . ? C24 C25 H25 117.6 . . ? C25 C26 C21 114.7(3) . . ? C25 C26 C31 122.0(3) . . ? C21 C26 C31 123.2(3) . . ? C28 C27 C24 111.1(3) . . ? C28 C27 C30 107.9(3) . . ? C24 C27 C30 112.5(3) . . ? C28 C27 C29 109.5(3) . . ? C24 C27 C29 109.0(3) . . ? C30 C27 C29 106.7(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 108.0(3) . . ? C33 C31 C34 108.6(3) . . ? C32 C31 C34 106.9(3) . . ? C33 C31 C26 109.6(3) . . ? C32 C31 C26 111.4(3) . . ? C34 C31 C26 112.3(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 C41 O41 120.1(3) . . ? C42 C41 C46 122.4(3) . . ? O41 C41 C46 117.4(3) . . ? C41 C42 C43 119.8(3) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C42 C43 C44 120.8(3) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 117.2(3) . . ? C45 C44 C147 122.4(5) . . ? C43 C44 C147 120.4(5) . . ? C45 C44 C47 119.6(6) . . ? C43 C44 C47 123.2(6) . . ? C147 C44 C47 3.3(10) . . ? C44 C45 C46 124.6(3) . . ? C44 C45 H45 117.7 . . ? C46 C45 H45 117.7 . . ? C45 C46 C41 115.1(3) . . ? C45 C46 C51 122.5(3) . . ? C41 C46 C51 122.4(3) . . ? C50 C47 C48 110.0(12) . . ? C50 C47 C44 107.8(10) . . ? C48 C47 C44 113.6(10) . . ? C50 C47 C49 108.2(11) . . ? C48 C47 C49 107.3(11) . . ? C44 C47 C49 109.9(11) . . ? C150 C147 C44 110.2(8) . . ? C150 C147 C148 107.3(8) . . ? C44 C147 C148 107.6(8) . . ? C150 C147 C149 111.5(9) . . ? C44 C147 C149 112.2(9) . . ? C148 C147 C149 107.8(8) . . ? C147 C148 H14D 109.5 . . ? C147 C148 H14E 109.5 . . ? H14D C148 H14E 109.5 . . ? C147 C148 H14F 109.5 . . ? H14D C148 H14F 109.5 . . ? H14E C148 H14F 109.5 . . ? C147 C149 H14G 109.5 . . ? C147 C149 H14H 109.5 . . ? H14G C149 H14H 109.5 . . ? C147 C149 H14I 109.5 . . ? H14G C149 H14I 109.5 . . ? H14H C149 H14I 109.5 . . ? C147 C150 H15A 109.5 . . ? C147 C150 H15B 109.5 . . ? H15A C150 H15B 109.5 . . ? C147 C150 H15C 109.5 . . ? H15A C150 H15C 109.5 . . ? H15B C150 H15C 109.5 . . ? C52 C51 C53 111.0(3) . . ? C52 C51 C46 109.9(3) . . ? C53 C51 C46 110.2(3) . . ? C52 C51 C54 107.5(3) . . ? C53 C51 C54 107.6(3) . . ? C46 C51 C54 110.5(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C1 O1 P1 113.81(18) . . ? C21 O21 P1 120.57(19) . . ? C41 O41 P1 126.9(2) . . ? O41 P1 O1 98.86(11) . . ? O41 P1 O21 97.79(11) . . ? O1 P1 O21 102.35(12) . . ? O41 P1 Pd1 119.69(9) . . ? O1 P1 Pd1 107.33(9) . . ? O21 P1 Pd1 126.51(9) . . ? N61 C61 N62 109.0(3) . . ? N61 C61 Pd1 128.3(2) . . ? N62 C61 Pd1 122.0(2) . . ? N61 C62 C63 102.6(2) . . ? N61 C62 H62A 111.3 . . ? C63 C62 H62A 111.3 . . ? N61 C62 H62B 111.3 . . ? C63 C62 H62B 111.3 . . ? H62A C62 H62B 109.2 . . ? N62 C63 C62 103.0(2) . . ? N62 C63 H63A 111.2 . . ? C62 C63 H63A 111.2 . . ? N62 C63 H63B 111.2 . . ? C62 C63 H63B 111.2 . . ? H63A C63 H63B 109.1 . . ? C65 C64 C69 121.6(3) . . ? C65 C64 N61 120.6(3) . . ? C69 C64 N61 117.7(3) . . ? C64 C65 C66 117.5(3) . . ? C64 C65 C70 123.6(3) . . ? C66 C65 C70 118.8(3) . . ? C67 C66 C65 121.7(3) . . ? C67 C66 H66 119.1 . . ? C65 C66 H66 119.1 . . ? C66 C67 C68 119.6(3) . . ? C66 C67 H67 120.2 . . ? C68 C67 H67 120.2 . . ? C67 C68 C69 121.8(3) . . ? C67 C68 H68 119.1 . . ? C69 C68 H68 119.1 . . ? C68 C69 C64 117.6(3) . . ? C68 C69 C73 118.2(3) . . ? C64 C69 C73 124.2(3) . . ? C65 C70 C71 113.6(3) . . ? C65 C70 C72 109.5(3) . . ? C71 C70 C72 111.2(3) . . ? C65 C70 H70 107.4 . . ? C71 C70 H70 107.4 . . ? C72 C70 H70 107.4 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C69 C73 C74 112.0(3) . . ? C69 C73 C75 110.5(3) . . ? C74 C73 C75 109.2(3) . . ? C69 C73 H73 108.4 . . ? C74 C73 H73 108.4 . . ? C75 C73 H73 108.4 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 C81 121.8(3) . . ? C77 C76 N62 118.5(3) . . ? C81 C76 N62 119.5(3) . . ? C78 C77 C76 117.3(3) . . ? C78 C77 C82 119.3(3) . . ? C76 C77 C82 123.2(3) . . ? C79 C78 C77 122.0(3) . . ? C79 C78 H78 119.0 . . ? C77 C78 H78 119.0 . . ? C80 C79 C78 119.5(3) . . ? C80 C79 H79 120.3 . . ? C78 C79 H79 120.3 . . ? C79 C80 C81 122.5(4) . . ? C79 C80 H80 118.7 . . ? C81 C80 H80 118.7 . . ? C80 C81 C76 116.8(3) . . ? C80 C81 C85 118.2(3) . . ? C76 C81 C85 125.0(3) . . ? C77 C82 C83 109.4(3) . . ? C77 C82 C84 113.9(3) . . ? C83 C82 C84 109.4(3) . . ? C77 C82 H82 108.0 . . ? C83 C82 H82 108.0 . . ? C84 C82 H82 108.0 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C81 C85 C86 111.6(3) . . ? C81 C85 C87 111.3(3) . . ? C86 C85 C87 110.9(3) . . ? C81 C85 H85 107.6 . . ? C86 C85 H85 107.6 . . ? C87 C85 H85 107.6 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C85 C87 H87A 109.5 . . ? C85 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C85 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C61 N61 C64 126.0(2) . . ? C61 N61 C62 113.1(2) . . ? C64 N61 C62 120.4(2) . . ? C61 N62 C76 125.7(2) . . ? C61 N62 C63 112.3(2) . . ? C76 N62 C63 120.4(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.539 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.067 data_2005src0243 _database_code_depnum_ccdc_archive 'CCDC 271193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. R. Bedford ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H62 Cl N2 O4 P Pd' _chemical_formula_weight 915.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.9666(10) _cell_length_b 17.766(2) _cell_length_c 39.401(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9076.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7653 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7984 _exptl_absorpt_correction_T_max 0.9575 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BrukerNonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32776 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9335 _reflns_number_gt 5842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+17.2850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9335 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.29576(8) -0.01597(6) 0.08317(2) 0.0290(2) Uani 1 1 d . . . Pd1 Pd 0.21363(2) 0.069463(15) 0.120791(7) 0.01579(9) Uani 1 1 d . . . C1 C 0.0950(3) 0.0812(2) 0.18471(10) 0.0179(8) Uani 1 1 d . . . C2 C 0.1398(3) 0.1241(2) 0.15898(9) 0.0165(8) Uani 1 1 d . . . C3 C 0.1325(3) 0.2020(2) 0.16408(10) 0.0194(9) Uani 1 1 d . . . H3 H 0.1615 0.2349 0.1476 0.023 Uiso 1 1 calc R . . C4 C 0.0844(3) 0.2330(2) 0.19229(10) 0.0225(9) Uani 1 1 d . . . H4 H 0.0811 0.2861 0.1948 0.027 Uiso 1 1 calc R . . C5 C 0.0415(3) 0.1868(2) 0.21669(10) 0.0257(10) Uani 1 1 d . . . H5 H 0.0086 0.2079 0.2360 0.031 Uiso 1 1 calc R . . C6 C 0.0469(3) 0.1097(2) 0.21271(10) 0.0243(10) Uani 1 1 d . . . H6 H 0.0176 0.0770 0.2292 0.029 Uiso 1 1 calc R . . C11 C 0.3222(3) -0.0758(2) 0.17982(10) 0.0183(8) Uani 1 1 d . . . C12 C 0.4106(3) -0.0642(2) 0.16106(10) 0.0265(10) Uani 1 1 d . . . H12 H 0.4087 -0.0633 0.1370 0.032 Uiso 1 1 calc R . . C13 C 0.5029(3) -0.0537(2) 0.17858(11) 0.0256(10) Uani 1 1 d . . . H13 H 0.5651 -0.0453 0.1664 0.031 Uiso 1 1 calc R . . C14 C 0.5039(3) -0.0556(2) 0.21360(11) 0.0282(10) Uani 1 1 d . . . H14 H 0.5672 -0.0489 0.2254 0.034 Uiso 1 1 calc R . . C15 C 0.4149(3) -0.0671(2) 0.23165(10) 0.0267(10) Uani 1 1 d . . . H15 H 0.4168 -0.0684 0.2557 0.032 Uiso 1 1 calc R . . C16 C 0.3222(3) -0.0767(2) 0.21483(10) 0.0226(9) Uani 1 1 d . . . H16 H 0.2599 -0.0839 0.2271 0.027 Uiso 1 1 calc R . . C21 C -0.0168(3) -0.0659(2) 0.11732(9) 0.0194(8) Uani 1 1 d . . . C22 C -0.0450(3) 0.0070(2) 0.10933(10) 0.0239(9) Uani 1 1 d . . . H22 H 0.0002 0.0479 0.1138 0.029 Uiso 1 1 calc R . . C23 C -0.1409(3) 0.0192(2) 0.09466(10) 0.0253(10) Uani 1 1 d . . . H23 H -0.1616 0.0689 0.0890 0.030 Uiso 1 1 calc R . . C24 C -0.2065(3) -0.0404(2) 0.08827(10) 0.0279(10) Uani 1 1 d . . . H24 H -0.2725 -0.0318 0.0785 0.034 Uiso 1 1 calc R . . C25 C -0.1754(3) -0.1126(2) 0.09614(11) 0.0276(10) Uani 1 1 d . . . H25 H -0.2201 -0.1536 0.0914 0.033 Uiso 1 1 calc R . . C26 C -0.0810(3) -0.1261(2) 0.11066(10) 0.0233(9) Uani 1 1 d . . . H26 H -0.0602 -0.1759 0.1160 0.028 Uiso 1 1 calc R . . O1 O 0.09832(19) 0.00138(13) 0.18230(7) 0.0216(6) Uani 1 1 d . . . O11 O 0.22966(18) -0.09352(14) 0.16259(7) 0.0201(6) Uani 1 1 d . . . O21 O 0.07709(19) -0.08464(14) 0.13254(7) 0.0213(6) Uani 1 1 d . . . P1 P 0.15748(8) -0.02794(6) 0.14925(3) 0.0181(2) Uani 1 1 d . . . C31 C 0.2523(3) 0.1683(2) 0.09624(9) 0.0159(8) Uani 1 1 d . . . C32 C 0.2312(3) 0.2842(2) 0.06822(10) 0.0216(9) Uani 1 1 d . . . H32A H 0.1897 0.3260 0.0776 0.026 Uiso 1 1 calc R . . H32B H 0.2357 0.2898 0.0433 0.026 Uiso 1 1 calc R . . C33 C 0.3372(3) 0.2820(2) 0.08407(11) 0.0225(9) Uani 1 1 d . . . H33A H 0.3918 0.2874 0.0667 0.027 Uiso 1 1 calc R . . H33B H 0.3454 0.3221 0.1013 0.027 Uiso 1 1 calc R . . C34 C 0.0938(3) 0.1853(2) 0.06096(10) 0.0182(9) Uani 1 1 d . . . C35 C 0.1005(3) 0.1340(2) 0.03387(10) 0.0202(9) Uani 1 1 d . . . C36 C 0.0108(3) 0.1158(2) 0.01685(10) 0.0230(9) Uani 1 1 d . . . H36 H 0.0135 0.0800 -0.0011 0.028 Uiso 1 1 calc R . . C37 C -0.0827(3) 0.1481(2) 0.02515(10) 0.0258(10) Uani 1 1 d . . . H37 H -0.1433 0.1350 0.0130 0.031 Uiso 1 1 calc R . . C38 C -0.0870(3) 0.1998(2) 0.05135(10) 0.0238(9) Uani 1 1 d . . . H38 H -0.1512 0.2224 0.0568 0.029 Uiso 1 1 calc R . . C39 C 0.0000(3) 0.2194(2) 0.06982(10) 0.0180(9) Uani 1 1 d . . . C40 C 0.2029(3) 0.1018(2) 0.02176(10) 0.0211(9) Uani 1 1 d . . . H40 H 0.2509 0.1000 0.0416 0.025 Uiso 1 1 calc R . . C41 C 0.1932(3) 0.0221(2) 0.00750(11) 0.0312(11) Uani 1 1 d . . . H41A H 0.1578 -0.0100 0.0240 0.047 Uiso 1 1 calc R . . H41B H 0.2621 0.0018 0.0030 0.047 Uiso 1 1 calc R . . H41C H 0.1535 0.0235 -0.0137 0.047 Uiso 1 1 calc R . . C42 C 0.2507(3) 0.1537(3) -0.00517(11) 0.0336(11) Uani 1 1 d . . . H42A H 0.2048 0.1566 -0.0249 0.050 Uiso 1 1 calc R . . H42B H 0.3177 0.1335 -0.0122 0.050 Uiso 1 1 calc R . . H42C H 0.2601 0.2041 0.0044 0.050 Uiso 1 1 calc R . . C43 C -0.0112(3) 0.2770(2) 0.09790(10) 0.0225(9) Uani 1 1 d . . . H43 H 0.0570 0.2821 0.1095 0.027 Uiso 1 1 calc R . . C44 C -0.0900(3) 0.2513(3) 0.12420(10) 0.0318(10) Uani 1 1 d . . . H44A H -0.1584 0.2484 0.1137 0.048 Uiso 1 1 calc R . . H44B H -0.0917 0.2873 0.1430 0.048 Uiso 1 1 calc R . . H44C H -0.0706 0.2015 0.1328 0.048 Uiso 1 1 calc R . . C45 C -0.0403(3) 0.3540(2) 0.08313(11) 0.0275(10) Uani 1 1 d . . . H45A H 0.0146 0.3713 0.0679 0.041 Uiso 1 1 calc R . . H45B H -0.0489 0.3903 0.1016 0.041 Uiso 1 1 calc R . . H45C H -0.1050 0.3496 0.0704 0.041 Uiso 1 1 calc R . . C46 C 0.4381(3) 0.1775(2) 0.11193(10) 0.0186(9) Uani 1 1 d . . . C47 C 0.5086(3) 0.1524(2) 0.08725(10) 0.0208(9) Uani 1 1 d . . . C48 C 0.6064(3) 0.1310(2) 0.09810(11) 0.0295(10) Uani 1 1 d . . . H48 H 0.6556 0.1144 0.0819 0.035 Uiso 1 1 calc R . . C49 C 0.6333(3) 0.1333(2) 0.13161(11) 0.0332(11) Uani 1 1 d . . . H49 H 0.7005 0.1183 0.1384 0.040 Uiso 1 1 calc R . . C50 C 0.5634(3) 0.1573(2) 0.15550(11) 0.0288(10) Uani 1 1 d . . . H50 H 0.5828 0.1581 0.1787 0.035 Uiso 1 1 calc R . . C51 C 0.4646(3) 0.1804(2) 0.14628(10) 0.0209(9) Uani 1 1 d . . . C52 C 0.4860(3) 0.1505(2) 0.04944(10) 0.0247(10) Uani 1 1 d . . . H52 H 0.4121 0.1646 0.0461 0.030 Uiso 1 1 calc R . . C53 C 0.5024(4) 0.0720(2) 0.03423(12) 0.0368(11) Uani 1 1 d . . . H53A H 0.5744 0.0567 0.0374 0.055 Uiso 1 1 calc R . . H53B H 0.4865 0.0731 0.0099 0.055 Uiso 1 1 calc R . . H53C H 0.4569 0.0359 0.0456 0.055 Uiso 1 1 calc R . . C54 C 0.5529(3) 0.2074(2) 0.03014(11) 0.0348(11) Uani 1 1 d . . . H54A H 0.5435 0.2576 0.0400 0.052 Uiso 1 1 calc R . . H54B H 0.5323 0.2082 0.0062 0.052 Uiso 1 1 calc R . . H54C H 0.6255 0.1928 0.0319 0.052 Uiso 1 1 calc R . . C55 C 0.3922(3) 0.2072(2) 0.17387(10) 0.0221(9) Uani 1 1 d . . . H55 H 0.3263 0.2234 0.1629 0.026 Uiso 1 1 calc R . . C56 C 0.3676(3) 0.1433(2) 0.19867(11) 0.0307(10) Uani 1 1 d . . . H56A H 0.3424 0.0995 0.1860 0.046 Uiso 1 1 calc R . . H56B H 0.3145 0.1600 0.2147 0.046 Uiso 1 1 calc R . . H56C H 0.4301 0.1295 0.2112 0.046 Uiso 1 1 calc R . . C57 C 0.4366(3) 0.2746(2) 0.19342(10) 0.0282(10) Uani 1 1 d . . . H57A H 0.4983 0.2587 0.2059 0.042 Uiso 1 1 calc R . . H57B H 0.3849 0.2934 0.2095 0.042 Uiso 1 1 calc R . . H57C H 0.4549 0.3146 0.1774 0.042 Uiso 1 1 calc R . . N31 N 0.1866(2) 0.21032(17) 0.07757(8) 0.0171(7) Uani 1 1 d . . . N32 N 0.3400(2) 0.20599(16) 0.10001(8) 0.0154(7) Uani 1 1 d . . . C61 C 0.7246(3) 0.3587(2) 0.18968(11) 0.0354(11) Uani 1 1 d . . . H61A H 0.7573 0.3590 0.1670 0.042 Uiso 1 1 calc R . . H61B H 0.6493 0.3524 0.1867 0.042 Uiso 1 1 calc R . . C62 C 0.7669(4) 0.2950(3) 0.21044(13) 0.0463(13) Uani 1 1 d . . . H62A H 0.8410 0.3025 0.2140 0.069 Uiso 1 1 calc R . . H62B H 0.7556 0.2474 0.1984 0.069 Uiso 1 1 calc R . . H62C H 0.7317 0.2935 0.2324 0.069 Uiso 1 1 calc R . . C63 C 0.7025(4) 0.4906(2) 0.18940(11) 0.0339(11) Uani 1 1 d . . . H63A H 0.6266 0.4854 0.1879 0.041 Uiso 1 1 calc R . . H63B H 0.7308 0.4939 0.1661 0.041 Uiso 1 1 calc R . . C64 C 0.7301(4) 0.5599(2) 0.20919(13) 0.0422(13) Uani 1 1 d . . . H64A H 0.7018 0.5560 0.2322 0.063 Uiso 1 1 calc R . . H64B H 0.7011 0.6043 0.1979 0.063 Uiso 1 1 calc R . . H64C H 0.8053 0.5647 0.2104 0.063 Uiso 1 1 calc R . . O61 O 0.7455(2) 0.42745(15) 0.20669(7) 0.0255(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0415(6) 0.0200(5) 0.0255(5) -0.0001(4) 0.0054(5) 0.0098(5) Pd1 0.01548(15) 0.01198(16) 0.01992(14) 0.00026(13) 0.00063(13) 0.00004(13) C1 0.018(2) 0.011(2) 0.025(2) -0.0037(17) 0.0003(17) -0.0016(17) C2 0.0102(18) 0.018(2) 0.021(2) -0.0001(17) -0.0018(16) 0.0016(17) C3 0.021(2) 0.012(2) 0.025(2) -0.0021(17) -0.0050(18) 0.0003(17) C4 0.027(2) 0.014(2) 0.026(2) -0.0021(18) 0.0007(19) 0.0004(19) C5 0.029(2) 0.024(2) 0.024(2) -0.0058(19) 0.0040(19) 0.006(2) C6 0.022(2) 0.024(2) 0.027(2) 0.0027(19) 0.0048(18) -0.0031(19) C11 0.0129(19) 0.011(2) 0.031(2) 0.0015(18) -0.0022(17) 0.0029(17) C12 0.027(2) 0.027(2) 0.025(2) 0.0018(19) -0.0006(18) 0.001(2) C13 0.017(2) 0.025(2) 0.035(2) 0.0020(19) 0.0050(19) -0.0010(19) C14 0.023(2) 0.029(3) 0.033(2) -0.004(2) -0.005(2) 0.001(2) C15 0.027(2) 0.028(2) 0.025(2) -0.001(2) -0.0021(18) 0.004(2) C16 0.021(2) 0.020(2) 0.027(2) -0.0001(18) 0.0020(17) 0.0042(19) C21 0.0152(19) 0.024(2) 0.0193(19) -0.0012(18) 0.0010(16) 0.0025(18) C22 0.023(2) 0.018(2) 0.031(2) 0.0010(18) 0.0012(19) 0.0002(18) C23 0.022(2) 0.022(2) 0.031(2) 0.0070(19) -0.0014(19) 0.0039(19) C24 0.022(2) 0.034(3) 0.028(2) 0.0018(19) -0.004(2) 0.002(2) C25 0.023(2) 0.029(3) 0.031(2) -0.001(2) -0.0019(19) -0.008(2) C26 0.021(2) 0.021(2) 0.027(2) 0.0023(18) -0.0005(18) -0.0023(19) O1 0.0240(15) 0.0140(15) 0.0267(15) 0.0003(12) 0.0061(13) -0.0011(12) O11 0.0172(14) 0.0132(14) 0.0299(15) 0.0017(11) -0.0041(12) 0.0020(11) O21 0.0165(14) 0.0138(15) 0.0336(16) -0.0027(12) -0.0064(12) -0.0019(12) P1 0.0163(5) 0.0135(5) 0.0244(5) 0.0008(4) 0.0006(4) -0.0006(4) C31 0.0156(18) 0.016(2) 0.0166(18) -0.0032(16) 0.0023(16) 0.0015(17) C32 0.017(2) 0.014(2) 0.033(2) 0.0051(18) -0.0020(18) -0.0056(17) C33 0.020(2) 0.012(2) 0.036(2) 0.0065(18) -0.0068(19) -0.0043(18) C34 0.018(2) 0.013(2) 0.024(2) 0.0052(17) -0.0053(17) -0.0032(17) C35 0.023(2) 0.013(2) 0.024(2) 0.0042(17) -0.0024(18) -0.0051(18) C36 0.023(2) 0.019(2) 0.028(2) -0.0046(18) -0.0020(19) -0.0004(19) C37 0.024(2) 0.020(2) 0.034(2) 0.0025(19) -0.0109(19) -0.0068(19) C38 0.016(2) 0.022(2) 0.033(2) 0.0007(19) -0.0031(18) -0.0008(19) C39 0.014(2) 0.015(2) 0.025(2) 0.0039(17) -0.0051(17) 0.0028(17) C40 0.019(2) 0.022(2) 0.022(2) -0.0033(17) -0.0031(17) -0.0010(18) C41 0.030(2) 0.024(2) 0.039(3) -0.012(2) -0.009(2) 0.002(2) C42 0.026(2) 0.041(3) 0.034(2) 0.003(2) 0.005(2) 0.000(2) C43 0.014(2) 0.028(2) 0.026(2) -0.0012(19) -0.0008(17) 0.0054(18) C44 0.027(2) 0.038(3) 0.031(2) -0.006(2) 0.001(2) 0.010(2) C45 0.021(2) 0.024(2) 0.037(3) -0.008(2) -0.007(2) 0.0071(19) C46 0.016(2) 0.010(2) 0.030(2) 0.0052(17) -0.0033(17) 0.0039(17) C47 0.018(2) 0.015(2) 0.029(2) 0.0031(18) 0.0004(18) -0.0009(17) C48 0.022(2) 0.034(3) 0.032(2) -0.001(2) 0.0030(19) 0.005(2) C49 0.020(2) 0.038(3) 0.041(3) 0.005(2) -0.001(2) 0.011(2) C50 0.023(2) 0.038(3) 0.025(2) 0.007(2) -0.0075(19) 0.006(2) C51 0.016(2) 0.019(2) 0.028(2) 0.0064(18) -0.0010(18) -0.0021(18) C52 0.020(2) 0.028(2) 0.027(2) -0.0018(19) 0.0024(18) 0.0000(19) C53 0.034(3) 0.037(3) 0.039(3) -0.008(2) 0.004(2) 0.004(2) C54 0.032(3) 0.036(3) 0.036(3) 0.004(2) 0.003(2) 0.001(2) C55 0.018(2) 0.025(2) 0.023(2) 0.0050(18) -0.0036(17) -0.0032(19) C56 0.024(2) 0.033(3) 0.035(2) 0.003(2) -0.002(2) -0.008(2) C57 0.030(2) 0.026(2) 0.029(2) 0.0015(19) -0.003(2) 0.001(2) N31 0.0164(17) 0.0113(17) 0.0235(17) 0.0014(14) -0.0030(14) -0.0012(14) N32 0.0143(17) 0.0099(17) 0.0220(17) 0.0014(14) -0.0004(14) -0.0033(14) C61 0.031(3) 0.039(3) 0.036(3) -0.010(2) -0.005(2) -0.003(2) C62 0.053(3) 0.030(3) 0.056(3) -0.003(2) 0.000(3) 0.003(3) C63 0.038(3) 0.035(3) 0.029(2) 0.006(2) 0.006(2) 0.006(2) C64 0.039(3) 0.034(3) 0.054(3) 0.009(2) 0.011(2) 0.002(2) O61 0.0217(14) 0.0292(17) 0.0258(14) 0.0000(14) -0.0012(12) 0.0018(13) _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 Cl1 Pd1 2.3739(10) . ? Pd1 C2 2.030(4) . ? Pd1 C31 2.066(4) . ? Pd1 P1 2.1868(10) . ? C1 C6 1.365(5) . ? C1 C2 1.395(5) . ? C1 O1 1.422(4) . ? C2 C3 1.402(5) . ? C3 C4 1.388(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.381(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C11 C16 1.380(5) . ? C11 C12 1.380(5) . ? C11 O11 1.414(4) . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 C14 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.371(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.379(5) . ? C21 C22 1.382(5) . ? C21 O21 1.397(4) . ? C22 C23 1.389(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(6) . ? C23 H23 0.9500 . ? C24 C25 1.379(6) . ? C24 H24 0.9500 . ? C25 C26 1.373(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O1 P1 1.599(3) . ? O11 P1 1.584(3) . ? O21 P1 1.592(3) . ? C31 N32 1.329(4) . ? C31 N31 1.351(5) . ? C32 N31 1.481(5) . ? C32 C33 1.509(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N32 1.489(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.403(5) . ? C34 C35 1.406(5) . ? C34 N31 1.440(5) . ? C35 C36 1.381(5) . ? C35 C40 1.522(5) . ? C36 C37 1.381(5) . ? C36 H36 0.9500 . ? C37 C38 1.383(5) . ? C37 H37 0.9500 . ? C38 C39 1.387(5) . ? C38 H38 0.9500 . ? C39 C43 1.513(5) . ? C40 C41 1.528(5) . ? C40 C42 1.536(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.525(5) . ? C43 C45 1.534(5) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C51 1.397(5) . ? C46 C47 1.408(5) . ? C46 N32 1.447(5) . ? C47 C48 1.392(5) . ? C47 C52 1.519(5) . ? C48 C49 1.366(6) . ? C48 H48 0.9500 . ? C49 C50 1.374(6) . ? C49 H49 0.9500 . ? C50 C51 1.394(5) . ? C50 H50 0.9500 . ? C51 C55 1.513(5) . ? C52 C53 1.533(5) . ? C52 C54 1.534(6) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.531(5) . ? C55 C57 1.536(5) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 O61 1.419(5) . ? C61 C62 1.499(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 O61 1.426(5) . ? C63 C64 1.500(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 C31 93.16(14) . . ? C2 Pd1 P1 80.88(11) . . ? C31 Pd1 P1 173.33(10) . . ? C2 Pd1 Cl1 168.51(11) . . ? C31 Pd1 Cl1 98.16(10) . . ? P1 Pd1 Cl1 87.91(4) . . ? C6 C1 C2 125.1(3) . . ? C6 C1 O1 116.0(3) . . ? C2 C1 O1 118.9(3) . . ? C1 C2 C3 114.0(3) . . ? C1 C2 Pd1 118.3(3) . . ? C3 C2 Pd1 127.6(3) . . ? C4 C3 C2 122.4(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.3(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C1 C6 C5 118.9(4) . . ? C1 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C16 C11 C12 122.5(4) . . ? C16 C11 O11 118.5(3) . . ? C12 C11 O11 118.8(3) . . ? C11 C12 C13 117.9(4) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 118.6(4) . . ? C11 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C26 C21 C22 121.5(4) . . ? C26 C21 O21 115.0(3) . . ? C22 C21 O21 123.5(3) . . ? C21 C22 C23 118.5(4) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.4(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 121.1(4) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 118.8(4) . . ? C25 C26 H26 120.6 . . ? C21 C26 H26 120.6 . . ? C1 O1 P1 113.2(2) . . ? C11 O11 P1 119.8(2) . . ? C21 O21 P1 126.7(2) . . ? O11 P1 O21 93.37(13) . . ? O11 P1 O1 104.66(14) . . ? O21 P1 O1 103.23(14) . . ? O11 P1 Pd1 123.74(10) . . ? O21 P1 Pd1 120.44(11) . . ? O1 P1 Pd1 108.64(10) . . ? N32 C31 N31 108.8(3) . . ? N32 C31 Pd1 125.7(3) . . ? N31 C31 Pd1 124.9(3) . . ? N31 C32 C33 103.3(3) . . ? N31 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? N31 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.1 . . ? N32 C33 C32 102.7(3) . . ? N32 C33 H33A 111.2 . . ? C32 C33 H33A 111.2 . . ? N32 C33 H33B 111.2 . . ? C32 C33 H33B 111.2 . . ? H33A C33 H33B 109.1 . . ? C39 C34 C35 121.5(3) . . ? C39 C34 N31 118.5(3) . . ? C35 C34 N31 119.6(3) . . ? C36 C35 C34 117.9(4) . . ? C36 C35 C40 119.6(3) . . ? C34 C35 C40 122.3(3) . . ? C37 C36 C35 121.8(4) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C38 119.3(4) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C37 C38 C39 121.7(4) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C38 C39 C34 117.7(3) . . ? C38 C39 C43 118.4(3) . . ? C34 C39 C43 123.9(3) . . ? C35 C40 C41 113.0(3) . . ? C35 C40 C42 110.1(3) . . ? C41 C40 C42 109.6(3) . . ? C35 C40 H40 108.0 . . ? C41 C40 H40 108.0 . . ? C42 C40 H40 108.0 . . ? 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 . . ? C39 C43 C44 111.0(3) . . ? C39 C43 C45 110.4(3) . . ? C44 C43 C45 111.1(3) . . ? C39 C43 H43 108.0 . . ? C44 C43 H43 108.0 . . ? C45 C43 H43 108.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 C46 C47 121.4(3) . . ? C51 C46 N32 121.2(3) . . ? C47 C46 N32 117.2(3) . . ? C48 C47 C46 117.8(4) . . ? C48 C47 C52 118.1(4) . . ? C46 C47 C52 124.0(3) . . ? C49 C48 C47 121.4(4) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C48 C49 C50 120.2(4) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 121.3(4) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C50 C51 C46 117.9(4) . . ? C50 C51 C55 118.4(4) . . ? C46 C51 C55 123.7(3) . . ? C47 C52 C53 112.2(3) . . ? C47 C52 C54 111.2(3) . . ? C53 C52 C54 109.1(3) . . ? C47 C52 H52 108.1 . . ? C53 C52 H52 108.1 . . ? C54 C52 H52 108.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C51 C55 C56 110.8(3) . . ? C51 C55 C57 111.9(3) . . ? C56 C55 C57 109.6(3) . . ? C51 C55 H55 108.1 . . ? C56 C55 H55 108.1 . . ? C57 C55 H55 108.1 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C31 N31 C34 127.1(3) . . ? C31 N31 C32 112.2(3) . . ? C34 N31 C32 119.2(3) . . ? C31 N32 C46 127.7(3) . . ? C31 N32 C33 112.9(3) . . ? C46 N32 C33 118.4(3) . . ? O61 C61 C62 108.8(4) . . ? O61 C61 H61A 109.9 . . ? C62 C61 H61A 109.9 . . ? O61 C61 H61B 109.9 . . ? C62 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O61 C63 C64 107.7(3) . . ? O61 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? O61 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? H63A C63 H63B 108.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C61 O61 C63 112.2(3) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.722 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.122 data_04src0834 _database_code_depnum_ccdc_archive 'CCDC 271194' _exptl_special_details ; Two of the t-butyl groups were disordered over two sites. Also the molecule of ether is also disordered over two main sites. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H98 Cl N2 O4 P Pd' _chemical_formula_weight 1168.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.9482(13) _cell_length_b 13.284(2) _cell_length_c 37.944(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.787(11) _cell_angle_gamma 90.00 _cell_volume 6480.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14763 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8350 _exptl_absorpt_correction_T_max 0.9538 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75355 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14755 _reflns_number_gt 12853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+4.1255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14755 _refine_ls_number_parameters 830 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.048 _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 0.62483(12) 0.04394(13) 0.19452(4) 0.0206(3) Uani 1 1 d . A . C2 C 0.60085(18) -0.07833(15) 0.23726(5) 0.0385(5) Uani 1 1 d . . . H2A H 0.5336 -0.1146 0.2339 0.046 Uiso 1 1 calc R . . H2B H 0.6306 -0.0830 0.2625 0.046 Uiso 1 1 calc R . . C3 C 0.67591(19) -0.11929(16) 0.21276(6) 0.0447(6) Uani 1 1 d . . . H3A H 0.7473 -0.1254 0.2252 0.054 Uiso 1 1 calc R . . H3B H 0.6529 -0.1856 0.2028 0.054 Uiso 1 1 calc R . . C4 C 0.54460(14) 0.10255(14) 0.24704(4) 0.0252(4) Uani 1 1 d . . . C5 C 0.44065(14) 0.12973(14) 0.23983(4) 0.0270(4) Uani 1 1 d . . . C6 C 0.40240(16) 0.20350(16) 0.26113(5) 0.0340(4) Uani 1 1 d . . . H6 H 0.3318 0.2238 0.2563 0.041 Uiso 1 1 calc R . . C7 C 0.46497(17) 0.24790(16) 0.28910(5) 0.0374(5) Uani 1 1 d . . . C8 C 0.56706(17) 0.21616(17) 0.29620(5) 0.0377(5) Uani 1 1 d . . . H8 H 0.6099 0.2448 0.3157 0.045 Uiso 1 1 calc R . . C9 C 0.60879(15) 0.14362(16) 0.27562(5) 0.0312(4) Uani 1 1 d . . . C10 C 0.36913(15) 0.08313(17) 0.21032(5) 0.0360(4) Uani 1 1 d . . . H10A H 0.3760 0.1186 0.1881 0.054 Uiso 1 1 calc R . . H10B H 0.2972 0.0882 0.2157 0.054 Uiso 1 1 calc R . . H10C H 0.3874 0.0121 0.2079 0.054 Uiso 1 1 calc R . . C11 C 0.4220(2) 0.32948(19) 0.31094(7) 0.0574(7) Uani 1 1 d . . . H11A H 0.4586 0.3284 0.3351 0.086 Uiso 1 1 calc R . . H11B H 0.3476 0.3178 0.3118 0.086 Uiso 1 1 calc R . . H11C H 0.4319 0.3952 0.3001 0.086 Uiso 1 1 calc R . . C12 C 0.72063(16) 0.1120(2) 0.28369(5) 0.0449(5) Uani 1 1 d . . . H12A H 0.7239 0.0400 0.2893 0.067 Uiso 1 1 calc R . . H12B H 0.7536 0.1504 0.3040 0.067 Uiso 1 1 calc R . . H12C H 0.7573 0.1249 0.2630 0.067 Uiso 1 1 calc R . . C13 C 0.73094(13) -0.05046(13) 0.15581(4) 0.0227(3) Uani 1 1 d . . . C14 C 0.69518(14) -0.11116(13) 0.12712(5) 0.0277(4) Uani 1 1 d . . . C15 C 0.75554(14) -0.11816(14) 0.09916(5) 0.0297(4) Uani 1 1 d . . . H15 H 0.7311 -0.1582 0.0792 0.036 Uiso 1 1 calc R . . C16 C 0.84949(14) -0.06905(14) 0.09946(5) 0.0286(4) Uani 1 1 d . . . C17 C 0.88522(14) -0.01355(15) 0.12918(5) 0.0317(4) Uani 1 1 d . . . H17 H 0.9506 0.0193 0.1300 0.038 Uiso 1 1 calc R . . C18 C 0.82826(14) -0.00427(15) 0.15794(5) 0.0286(4) Uani 1 1 d . . . C19 C 0.59605(18) -0.17033(17) 0.12543(8) 0.0523(7) Uani 1 1 d . . . H19A H 0.6123 -0.2418 0.1293 0.078 Uiso 1 1 calc R . . H19B H 0.5562 -0.1616 0.1020 0.078 Uiso 1 1 calc R . . H19C H 0.5549 -0.1463 0.1438 0.078 Uiso 1 1 calc R . . C20 C 0.91187(19) -0.07919(18) 0.06835(6) 0.0458(5) Uani 1 1 d . . . H20A H 0.9706 -0.0322 0.0713 0.069 Uiso 1 1 calc R . . H20B H 0.8674 -0.0637 0.0463 0.069 Uiso 1 1 calc R . . H20C H 0.9380 -0.1482 0.0673 0.069 Uiso 1 1 calc R . . C21 C 0.87308(17) 0.0500(2) 0.19085(6) 0.0579(7) Uani 1 1 d . . . H21A H 0.8390 0.1156 0.1920 0.087 Uiso 1 1 calc R . . H21B H 0.9479 0.0599 0.1903 0.087 Uiso 1 1 calc R . . H21C H 0.8616 0.0101 0.2118 0.087 Uiso 1 1 calc R . . C31 C 0.50521(12) 0.16673(11) 0.09298(4) 0.0171(3) Uani 1 1 d . A . C32 C 0.51235(12) 0.11686(11) 0.12560(4) 0.0170(3) Uani 1 1 d . A . C33 C 0.44788(13) 0.03337(12) 0.12707(4) 0.0222(3) Uani 1 1 d . A . H33 H 0.4497 -0.0026 0.1488 0.027 Uiso 1 1 calc R . . C34 C 0.38095(14) 0.00078(14) 0.09791(5) 0.0275(4) Uani 1 1 d D . . C35 C 0.38573(14) 0.04913(14) 0.06554(4) 0.0268(4) Uani 1 1 d . A . H35 H 0.3447 0.0237 0.0451 0.032 Uiso 1 1 calc R . . C36 C 0.44792(13) 0.13299(13) 0.06183(4) 0.0213(3) Uani 1 1 d . . . C37 C 0.3055(5) -0.0883(4) 0.09931(18) 0.0333(15) Uani 0.652(4) 1 d PD A 1 C38 C 0.3183(5) -0.1478(6) 0.1315(2) 0.077(3) Uani 0.652(4) 1 d PD A 1 H38A H 0.3206 -0.1031 0.1522 0.116 Uiso 0.652(4) 1 calc PR A 1 H38B H 0.3833 -0.1861 0.1327 0.116 Uiso 0.652(4) 1 calc PR A 1 H38C H 0.2596 -0.1944 0.1315 0.116 Uiso 0.652(4) 1 calc PR A 1 C39 C 0.3257(3) -0.1733(2) 0.07404(9) 0.0421(9) Uani 0.652(4) 1 d PD A 1 H39A H 0.2729 -0.2257 0.0749 0.063 Uiso 0.652(4) 1 calc PR A 1 H39B H 0.3948 -0.2019 0.0812 0.063 Uiso 0.652(4) 1 calc PR A 1 H39C H 0.3226 -0.1468 0.0498 0.063 Uiso 0.652(4) 1 calc PR A 1 C40 C 0.1974(2) -0.0474(3) 0.09181(11) 0.0487(11) Uani 0.652(4) 1 d PD A 1 H40A H 0.1471 -0.1018 0.0936 0.073 Uiso 0.652(4) 1 calc PR A 1 H40B H 0.1875 -0.0189 0.0678 0.073 Uiso 0.652(4) 1 calc PR A 1 H40C H 0.1868 0.0052 0.1091 0.073 Uiso 0.652(4) 1 calc PR A 1 C137 C 0.2879(8) -0.0698(8) 0.1038(3) 0.033(3) Uani 0.348(4) 1 d PD A 2 C138 C 0.3140(11) -0.1330(9) 0.1376(2) 0.038(3) Uani 0.348(4) 1 d PD A 2 H13A H 0.2723 -0.1947 0.1358 0.057 Uiso 0.348(4) 1 calc PR A 2 H13B H 0.2984 -0.0940 0.1583 0.057 Uiso 0.348(4) 1 calc PR A 2 H13C H 0.3881 -0.1505 0.1403 0.057 Uiso 0.348(4) 1 calc PR A 2 C139 C 0.2315(5) -0.1050(5) 0.06607(17) 0.0447(18) Uani 0.348(4) 1 d PD A 2 H13D H 0.2828 -0.1349 0.0522 0.067 Uiso 0.348(4) 1 calc PR A 2 H13E H 0.1991 -0.0467 0.0534 0.067 Uiso 0.348(4) 1 calc PR A 2 H13F H 0.1779 -0.1550 0.0695 0.067 Uiso 0.348(4) 1 calc PR A 2 C140 C 0.2010(4) -0.0109(4) 0.12005(17) 0.0347(15) Uani 0.348(4) 1 d PD A 2 H14A H 0.1422 -0.0559 0.1223 0.052 Uiso 0.348(4) 1 calc PR A 2 H14B H 0.1777 0.0457 0.1045 0.052 Uiso 0.348(4) 1 calc PR A 2 H14C H 0.2284 0.0148 0.1435 0.052 Uiso 0.348(4) 1 calc PR A 2 C41 C 0.45137(16) 0.18684(14) 0.02619(4) 0.0305(4) Uani 1 1 d . A . C42 C 0.56425(18) 0.19518(16) 0.01795(5) 0.0398(5) Uani 1 1 d . . . H42A H 0.6044 0.2358 0.0363 0.060 Uiso 1 1 calc R A . H42B H 0.5656 0.2273 -0.0052 0.060 Uiso 1 1 calc R . . H42C H 0.5948 0.1278 0.0175 0.060 Uiso 1 1 calc R . . C43 C 0.4023(2) 0.29236(16) 0.02700(5) 0.0462(6) Uani 1 1 d . . . H43A H 0.4424 0.3332 0.0453 0.069 Uiso 1 1 calc R A . H43B H 0.3304 0.2863 0.0324 0.069 Uiso 1 1 calc R . . H43C H 0.4029 0.3247 0.0038 0.069 Uiso 1 1 calc R . . C44 C 0.3907(2) 0.12826(18) -0.00447(5) 0.0485(6) Uani 1 1 d . . . H44A H 0.3974 0.1626 -0.0269 0.073 Uiso 1 1 calc R A . H44B H 0.3171 0.1249 -0.0008 0.073 Uiso 1 1 calc R . . H44C H 0.4188 0.0599 -0.0052 0.073 Uiso 1 1 calc R . . C45 C 0.75219(12) 0.35411(13) 0.10110(4) 0.0203(3) Uani 1 1 d . A . C46 C 0.78737(14) 0.25605(13) 0.10064(5) 0.0277(4) Uani 1 1 d . . . H46 H 0.7632 0.2073 0.1161 0.033 Uiso 1 1 calc R . . C47 C 0.85796(16) 0.22896(15) 0.07765(5) 0.0332(4) Uani 1 1 d . B . H47 H 0.8809 0.1611 0.0770 0.040 Uiso 1 1 calc R . . C48 C 0.89574(15) 0.29991(15) 0.05550(5) 0.0312(4) Uani 1 1 d D . . C49 C 0.86065(13) 0.39857(14) 0.05760(4) 0.0256(4) Uani 1 1 d . B . H49 H 0.8875 0.4479 0.0430 0.031 Uiso 1 1 calc R . . C50 C 0.78800(12) 0.42925(12) 0.07998(4) 0.0197(3) Uani 1 1 d . . . C51 C 0.9655(4) 0.2603(4) 0.02797(12) 0.0321(10) Uani 0.687(5) 1 d PD B 1 C52 C 0.9100(3) 0.1805(3) 0.00402(9) 0.0497(10) Uani 0.687(5) 1 d PD B 1 H52A H 0.8473 0.2095 -0.0091 0.075 Uiso 0.687(5) 1 calc PR B 1 H52B H 0.8906 0.1240 0.0185 0.075 Uiso 0.687(5) 1 calc PR B 1 H52C H 0.9565 0.1564 -0.0128 0.075 Uiso 0.687(5) 1 calc PR B 1 C53 C 0.9952(4) 0.3480(3) 0.00496(12) 0.0487(10) Uani 0.687(5) 1 d PD B 1 H53A H 1.0325 0.3992 0.0201 0.073 Uiso 0.687(5) 1 calc PR B 1 H53B H 0.9321 0.3775 -0.0077 0.073 Uiso 0.687(5) 1 calc PR B 1 H53C H 1.0401 0.3232 -0.0122 0.073 Uiso 0.687(5) 1 calc PR B 1 C54 C 1.0635(4) 0.2170(5) 0.04848(15) 0.0546(15) Uani 0.687(5) 1 d PD B 1 H54A H 1.1097 0.1921 0.0318 0.082 Uiso 0.687(5) 1 calc PR B 1 H54B H 1.0447 0.1614 0.0635 0.082 Uiso 0.687(5) 1 calc PR B 1 H54C H 1.0991 0.2696 0.0634 0.082 Uiso 0.687(5) 1 calc PR B 1 C151 C 0.9906(7) 0.2892(7) 0.0336(3) 0.029(2) Uani 0.313(5) 1 d PD B 2 C152 C 0.9497(7) 0.3082(7) -0.0053(2) 0.046(2) Uani 0.313(5) 1 d PD B 2 H15A H 1.0052 0.2954 -0.0201 0.069 Uiso 0.313(5) 1 calc PR B 2 H15B H 0.9266 0.3783 -0.0082 0.069 Uiso 0.313(5) 1 calc PR B 2 H15C H 0.8910 0.2631 -0.0124 0.069 Uiso 0.313(5) 1 calc PR B 2 C153 C 1.0855(5) 0.3613(6) 0.04320(19) 0.0408(19) Uani 0.313(5) 1 d PD B 2 H15D H 1.1137 0.3511 0.0681 0.061 Uiso 0.313(5) 1 calc PR B 2 H15E H 1.0627 0.4313 0.0397 0.061 Uiso 0.313(5) 1 calc PR B 2 H15F H 1.1394 0.3465 0.0279 0.061 Uiso 0.313(5) 1 calc PR B 2 C154 C 1.0344(12) 0.1818(8) 0.0373(4) 0.062(4) Uani 0.313(5) 1 d PD B 2 H15G H 0.9797 0.1335 0.0290 0.092 Uiso 0.313(5) 1 calc PR B 2 H15H H 1.0591 0.1684 0.0623 0.092 Uiso 0.313(5) 1 calc PR B 2 H15I H 1.0923 0.1749 0.0231 0.092 Uiso 0.313(5) 1 calc PR B 2 C55 C 0.75101(13) 0.53881(12) 0.08107(4) 0.0223(3) Uani 1 1 d . B . C56 C 0.63317(14) 0.54583(14) 0.06944(5) 0.0290(4) Uani 1 1 d . . . H56A H 0.6170 0.5154 0.0459 0.044 Uiso 1 1 calc R B . H56B H 0.6119 0.6167 0.0685 0.044 Uiso 1 1 calc R . . H56C H 0.5956 0.5098 0.0865 0.044 Uiso 1 1 calc R . . C57 C 0.80499(16) 0.60562(14) 0.05581(5) 0.0341(4) Uani 1 1 d . . . H57A H 0.7877 0.5817 0.0314 0.051 Uiso 1 1 calc R B . H57B H 0.8805 0.6026 0.0623 0.051 Uiso 1 1 calc R . . H57C H 0.7813 0.6753 0.0576 0.051 Uiso 1 1 calc R . . C58 C 0.77678(15) 0.58097(13) 0.11879(5) 0.0286(4) Uani 1 1 d . . . H58A H 0.7598 0.6529 0.1189 0.043 Uiso 1 1 calc R B . H58B H 0.8511 0.5717 0.1266 0.043 Uiso 1 1 calc R . . H58C H 0.7359 0.5452 0.1350 0.043 Uiso 1 1 calc R . . C59 C 0.40473(12) 0.37928(12) 0.14703(4) 0.0202(3) Uani 1 1 d . A . C60 C 0.34074(13) 0.30852(13) 0.12947(5) 0.0238(3) Uani 1 1 d . . . H60 H 0.3641 0.2711 0.1106 0.029 Uiso 1 1 calc R . . C61 C 0.24189(13) 0.29116(14) 0.13911(5) 0.0271(4) Uani 1 1 d . . . H61 H 0.1990 0.2409 0.1271 0.033 Uiso 1 1 calc R . . C62 C 0.20549(14) 0.34647(15) 0.16599(5) 0.0282(4) Uani 1 1 d . . . C63 C 0.27189(15) 0.41917(15) 0.18247(5) 0.0328(4) Uani 1 1 d . . . H63 H 0.2473 0.4582 0.2007 0.039 Uiso 1 1 calc R . . C64 C 0.37220(14) 0.43893(14) 0.17404(5) 0.0292(4) Uani 1 1 d . . . C65 C 0.09739(15) 0.32975(17) 0.17764(5) 0.0357(4) Uani 1 1 d . . . C66 C 0.0375(2) 0.2496(4) 0.15499(10) 0.1172(19) Uani 1 1 d . . . H66A H 0.0786 0.1875 0.1557 0.176 Uiso 1 1 calc R . . H66B H 0.0241 0.2734 0.1304 0.176 Uiso 1 1 calc R . . H66C H -0.0288 0.2364 0.1642 0.176 Uiso 1 1 calc R . . C67 C 0.0349(2) 0.4260(3) 0.17462(10) 0.0840(12) Uani 1 1 d . . . H67A H -0.0331 0.4142 0.1827 0.126 Uiso 1 1 calc R . . H67B H 0.0253 0.4482 0.1498 0.126 Uiso 1 1 calc R . . H67C H 0.0721 0.4782 0.1894 0.126 Uiso 1 1 calc R . . C68 C 0.10784(18) 0.2931(2) 0.21550(7) 0.0516(6) Uani 1 1 d . . . H68A H 0.1415 0.3451 0.2312 0.077 Uiso 1 1 calc R . . H68B H 0.1501 0.2317 0.2176 0.077 Uiso 1 1 calc R . . H68C H 0.0387 0.2786 0.2223 0.077 Uiso 1 1 calc R . . C69 C 0.44145(18) 0.51950(18) 0.19366(7) 0.0511(6) Uani 1 1 d . . . C70 C 0.53731(19) 0.4688(2) 0.21420(6) 0.0617(8) Uani 1 1 d . . . H70A H 0.5145 0.4157 0.2295 0.093 Uiso 1 1 calc R . . H70B H 0.5778 0.5191 0.2288 0.093 Uiso 1 1 calc R . . H70C H 0.5806 0.4393 0.1974 0.093 Uiso 1 1 calc R . . C71 C 0.4753(2) 0.59764(18) 0.16759(9) 0.0668(8) Uani 1 1 d . . . H71A H 0.5203 0.5655 0.1519 0.100 Uiso 1 1 calc R . . H71B H 0.5135 0.6520 0.1808 0.100 Uiso 1 1 calc R . . H71C H 0.4137 0.6254 0.1534 0.100 Uiso 1 1 calc R . . C72 C 0.3832(3) 0.5767(3) 0.22060(10) 0.1002(15) Uani 1 1 d . . . H72A H 0.3226 0.6109 0.2081 0.150 Uiso 1 1 calc R . . H72B H 0.4298 0.6266 0.2331 0.150 Uiso 1 1 calc R . . H72C H 0.3602 0.5290 0.2378 0.150 Uiso 1 1 calc R . . N1 N 0.58864(12) 0.02779(11) 0.22563(4) 0.0270(3) Uani 1 1 d . . . N2 N 0.66981(12) -0.04081(11) 0.18489(4) 0.0260(3) Uani 1 1 d . . . O1 O 0.55270(9) 0.26233(8) 0.09200(3) 0.0190(2) Uani 1 1 d . . . O2 O 0.67717(8) 0.38117(8) 0.12339(3) 0.0197(2) Uani 1 1 d . . . O3 O 0.50414(8) 0.39615(8) 0.13609(3) 0.0200(2) Uani 1 1 d . . . P1 P 0.58503(3) 0.30800(3) 0.130888(10) 0.01597(8) Uani 1 1 d . A . Cl1 Cl 0.72675(4) 0.26862(4) 0.207520(12) 0.03737(11) Uani 1 1 d . A . Pd1 Pd 0.607598(9) 0.177635(9) 0.166623(3) 0.01584(4) Uani 1 1 d . . . C81 C 0.6825(6) 0.4483(6) -0.0675(2) 0.0480(19) Uani 0.379(7) 1 d PD C 1 H81A H 0.6796 0.5200 -0.0746 0.058 Uiso 0.379(7) 1 calc PR C 1 H81B H 0.6289 0.4120 -0.0833 0.058 Uiso 0.379(7) 1 calc PR C 1 C82 C 0.6572(19) 0.4417(17) -0.0332(6) 0.085(7) Uani 0.379(7) 1 d P C 1 H82A H 0.6610 0.3712 -0.0255 0.127 Uiso 0.379(7) 1 calc PR C 1 H82B H 0.5864 0.4670 -0.0324 0.127 Uiso 0.379(7) 1 calc PR C 1 H82C H 0.7061 0.4821 -0.0174 0.127 Uiso 0.379(7) 1 calc PR C 1 C83 C 0.8048(6) 0.4160(5) -0.10792(15) 0.0444(19) Uani 0.379(7) 1 d PD C 1 H83A H 0.8064 0.4871 -0.1156 0.053 Uiso 0.379(7) 1 calc PR C 1 H83B H 0.7525 0.3790 -0.1242 0.053 Uiso 0.379(7) 1 calc PR C 1 C84 C 0.917(2) 0.3655(19) -0.1069(7) 0.064(6) Uani 0.379(7) 1 d P C 1 H84A H 0.9147 0.2974 -0.0971 0.096 Uiso 0.379(7) 1 calc PR C 1 H84B H 0.9678 0.4060 -0.0920 0.096 Uiso 0.379(7) 1 calc PR C 1 H84C H 0.9363 0.3621 -0.1311 0.096 Uiso 0.379(7) 1 calc PR C 1 C181 C 0.7303(4) 0.4819(3) -0.05512(12) 0.0461(11) Uani 0.621(7) 1 d PD C 2 H18A H 0.6912 0.5271 -0.0727 0.055 Uiso 0.621(7) 1 calc PR C 2 H18B H 0.7814 0.5231 -0.0399 0.055 Uiso 0.621(7) 1 calc PR C 2 C182 C 0.6554(7) 0.4326(9) -0.0323(2) 0.046(2) Uani 0.621(7) 1 d P C 2 H18C H 0.6031 0.3940 -0.0475 0.069 Uiso 0.621(7) 1 calc PR C 2 H18D H 0.6208 0.4847 -0.0196 0.069 Uiso 0.621(7) 1 calc PR C 2 H18E H 0.6940 0.3873 -0.0151 0.069 Uiso 0.621(7) 1 calc PR C 2 C183 C 0.8629(4) 0.4438(3) -0.09347(12) 0.0473(12) Uani 0.621(7) 1 d PD C 2 H18F H 0.9212 0.4717 -0.0771 0.057 Uiso 0.621(7) 1 calc PR C 2 H18G H 0.8344 0.4991 -0.1092 0.057 Uiso 0.621(7) 1 calc PR C 2 C184 C 0.9035(12) 0.3646(8) -0.1153(4) 0.052(3) Uani 0.621(7) 1 d P C 2 H18H H 0.9274 0.3074 -0.1001 0.078 Uiso 0.621(7) 1 calc PR C 2 H18I H 0.9618 0.3913 -0.1267 0.078 Uiso 0.621(7) 1 calc PR C 2 H18J H 0.8483 0.3423 -0.1335 0.078 Uiso 0.621(7) 1 calc PR C 2 O81 O 0.78299(13) 0.40889(13) -0.07297(5) 0.0537(4) Uani 1 1 d 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 C1 0.0204(8) 0.0237(8) 0.0178(7) 0.0041(6) 0.0024(6) 0.0019(6) C2 0.0512(12) 0.0320(10) 0.0365(10) 0.0187(8) 0.0227(9) 0.0159(9) C3 0.0647(15) 0.0359(11) 0.0387(11) 0.0224(9) 0.0279(10) 0.0248(10) C4 0.0302(9) 0.0295(9) 0.0176(7) 0.0067(7) 0.0105(6) 0.0051(7) C5 0.0290(9) 0.0316(9) 0.0219(8) 0.0026(7) 0.0092(7) 0.0022(7) C6 0.0326(10) 0.0387(11) 0.0331(10) 0.0000(8) 0.0141(8) 0.0059(8) C7 0.0481(12) 0.0377(11) 0.0303(10) -0.0033(8) 0.0209(9) -0.0023(9) C8 0.0461(12) 0.0470(12) 0.0214(9) -0.0017(8) 0.0098(8) -0.0105(10) C9 0.0307(9) 0.0419(11) 0.0220(8) 0.0088(8) 0.0067(7) -0.0020(8) C10 0.0291(10) 0.0490(12) 0.0302(9) -0.0027(9) 0.0049(8) 0.0046(9) C11 0.0787(19) 0.0483(14) 0.0517(14) -0.0169(11) 0.0344(13) -0.0046(13) C12 0.0337(11) 0.0710(16) 0.0296(10) 0.0165(10) 0.0019(8) 0.0008(11) C13 0.0266(8) 0.0222(8) 0.0202(7) 0.0053(6) 0.0068(6) 0.0068(7) C14 0.0259(9) 0.0214(8) 0.0368(9) -0.0023(7) 0.0082(7) 0.0035(7) C15 0.0318(9) 0.0293(9) 0.0279(9) -0.0078(7) 0.0033(7) 0.0048(8) C16 0.0315(9) 0.0299(9) 0.0260(8) 0.0027(7) 0.0096(7) 0.0080(8) C17 0.0233(9) 0.0380(10) 0.0349(10) -0.0026(8) 0.0084(7) -0.0016(8) C18 0.0234(9) 0.0367(10) 0.0253(8) -0.0037(7) 0.0009(7) 0.0039(7) C19 0.0405(12) 0.0382(12) 0.0833(18) -0.0286(12) 0.0283(12) -0.0113(10) C20 0.0519(13) 0.0509(13) 0.0393(11) -0.0029(10) 0.0247(10) 0.0035(11) C21 0.0288(11) 0.099(2) 0.0446(13) -0.0348(14) -0.0026(9) -0.0027(12) C31 0.0189(7) 0.0148(7) 0.0182(7) 0.0007(6) 0.0049(6) -0.0004(6) C32 0.0177(7) 0.0168(7) 0.0170(7) -0.0001(6) 0.0034(6) 0.0009(6) C33 0.0276(8) 0.0200(8) 0.0199(7) 0.0016(6) 0.0059(6) -0.0047(7) C34 0.0283(9) 0.0263(9) 0.0284(9) -0.0023(7) 0.0052(7) -0.0110(7) C35 0.0284(9) 0.0290(9) 0.0219(8) -0.0039(7) -0.0017(7) -0.0066(7) C36 0.0245(8) 0.0208(8) 0.0183(7) 0.0004(6) 0.0020(6) 0.0010(7) C37 0.038(2) 0.037(3) 0.027(2) -0.007(2) 0.0116(18) -0.018(2) C38 0.024(3) 0.049(4) 0.154(7) 0.056(4) -0.012(3) -0.019(2) C39 0.050(2) 0.0334(17) 0.0439(18) -0.0092(14) 0.0117(15) -0.0224(15) C40 0.0266(17) 0.053(2) 0.065(3) 0.0011(19) 0.0010(16) -0.0112(15) C137 0.037(5) 0.038(5) 0.027(4) -0.017(3) 0.013(3) -0.029(4) C138 0.062(6) 0.032(5) 0.025(3) -0.012(3) 0.030(4) -0.025(4) C139 0.042(4) 0.045(4) 0.047(4) -0.016(3) 0.009(3) -0.027(3) C140 0.025(3) 0.035(3) 0.046(4) 0.000(3) 0.008(2) -0.008(2) C41 0.0476(11) 0.0274(9) 0.0154(8) 0.0017(7) -0.0008(7) -0.0017(8) C42 0.0619(14) 0.0387(11) 0.0220(9) -0.0019(8) 0.0185(9) -0.0119(10) C43 0.0719(16) 0.0349(11) 0.0282(10) 0.0077(9) -0.0090(10) 0.0107(11) C44 0.0760(17) 0.0467(13) 0.0196(9) 0.0005(9) -0.0083(10) -0.0128(12) C45 0.0195(8) 0.0232(8) 0.0197(7) -0.0010(6) 0.0076(6) 0.0007(6) C46 0.0308(9) 0.0227(9) 0.0320(9) 0.0042(7) 0.0141(7) 0.0017(7) C47 0.0402(11) 0.0268(9) 0.0356(10) 0.0025(8) 0.0167(8) 0.0121(8) C48 0.0335(10) 0.0358(10) 0.0270(9) 0.0050(7) 0.0153(8) 0.0109(8) C49 0.0259(9) 0.0297(9) 0.0229(8) 0.0057(7) 0.0103(7) 0.0041(7) C50 0.0188(7) 0.0219(8) 0.0188(7) 0.0006(6) 0.0045(6) -0.0010(6) C51 0.034(2) 0.033(3) 0.034(2) -0.0023(16) 0.0195(17) 0.0051(17) C52 0.054(2) 0.057(2) 0.0429(19) -0.0186(15) 0.0250(16) -0.0041(16) C53 0.055(3) 0.050(2) 0.048(2) 0.0048(18) 0.039(2) 0.0049(18) C54 0.040(3) 0.081(4) 0.048(3) 0.008(2) 0.025(2) 0.027(3) C151 0.040(5) 0.021(5) 0.028(4) -0.003(3) 0.017(4) 0.008(3) C152 0.054(6) 0.057(6) 0.031(4) -0.003(4) 0.023(4) 0.014(4) C153 0.028(3) 0.049(4) 0.048(4) 0.003(3) 0.017(3) 0.003(3) C154 0.074(10) 0.055(7) 0.066(9) 0.020(6) 0.049(7) 0.033(6) C55 0.0258(8) 0.0190(8) 0.0236(8) 0.0035(6) 0.0095(6) 0.0002(6) C56 0.0287(9) 0.0304(9) 0.0286(9) 0.0068(7) 0.0059(7) 0.0072(7) C57 0.0438(11) 0.0255(9) 0.0368(10) 0.0082(8) 0.0202(9) -0.0008(8) C58 0.0357(10) 0.0226(9) 0.0287(9) -0.0023(7) 0.0089(7) -0.0048(7) C59 0.0194(8) 0.0207(8) 0.0223(7) 0.0028(6) 0.0093(6) 0.0004(6) C60 0.0212(8) 0.0267(9) 0.0239(8) -0.0035(7) 0.0052(6) 0.0025(7) C61 0.0203(8) 0.0311(9) 0.0299(9) -0.0030(7) 0.0031(7) -0.0014(7) C62 0.0216(8) 0.0374(10) 0.0271(9) 0.0037(7) 0.0090(7) 0.0011(7) C63 0.0309(10) 0.0379(11) 0.0326(9) -0.0094(8) 0.0171(8) -0.0018(8) C64 0.0299(9) 0.0277(9) 0.0325(9) -0.0086(7) 0.0143(7) -0.0042(7) C65 0.0227(9) 0.0534(13) 0.0330(10) 0.0020(9) 0.0120(7) -0.0017(8) C66 0.0461(16) 0.214(5) 0.101(3) -0.087(3) 0.0449(17) -0.070(2) C67 0.0418(14) 0.102(2) 0.117(3) 0.071(2) 0.0477(16) 0.0369(15) C68 0.0339(11) 0.0679(16) 0.0573(14) 0.0290(12) 0.0237(10) 0.0081(11) C69 0.0456(13) 0.0486(13) 0.0655(15) -0.0374(12) 0.0331(11) -0.0196(11) C70 0.0490(14) 0.093(2) 0.0444(13) -0.0333(14) 0.0120(11) -0.0341(14) C71 0.0673(17) 0.0275(12) 0.113(2) -0.0237(13) 0.0427(17) -0.0147(11) C72 0.076(2) 0.104(3) 0.133(3) -0.098(2) 0.065(2) -0.0447(19) N1 0.0331(8) 0.0276(8) 0.0223(7) 0.0108(6) 0.0124(6) 0.0093(6) N2 0.0333(8) 0.0235(7) 0.0230(7) 0.0092(6) 0.0107(6) 0.0093(6) O1 0.0282(6) 0.0149(5) 0.0146(5) 0.0009(4) 0.0048(4) -0.0037(4) O2 0.0215(6) 0.0166(5) 0.0229(5) -0.0017(4) 0.0110(4) -0.0028(4) O3 0.0207(6) 0.0176(5) 0.0234(5) 0.0006(4) 0.0102(4) -0.0012(4) P1 0.01929(19) 0.01451(18) 0.01501(18) 0.00036(14) 0.00581(14) -0.00197(15) Cl1 0.0475(3) 0.0394(3) 0.0226(2) -0.00230(18) -0.00689(19) -0.0172(2) Pd1 0.01872(7) 0.01632(7) 0.01271(6) 0.00118(4) 0.00279(4) -0.00141(4) C81 0.056(4) 0.037(4) 0.049(4) 0.000(3) -0.002(3) 0.013(3) C82 0.119(15) 0.031(7) 0.108(16) 0.003(8) 0.028(12) -0.011(8) C83 0.057(5) 0.037(3) 0.038(3) 0.007(3) 0.000(3) 0.002(3) C84 0.041(7) 0.102(11) 0.048(8) 0.011(6) 0.002(5) -0.012(6) C181 0.058(3) 0.033(2) 0.048(2) 0.0015(17) 0.009(2) 0.0036(19) C182 0.040(4) 0.050(5) 0.050(5) 0.008(3) 0.014(3) 0.006(3) C183 0.051(3) 0.042(2) 0.050(2) 0.0045(18) 0.013(2) -0.0107(19) C184 0.044(5) 0.041(3) 0.071(8) 0.003(3) 0.010(4) -0.010(3) O81 0.0535(10) 0.0447(9) 0.0642(11) 0.0094(8) 0.0131(8) -0.0044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.338(2) . ? C1 N2 1.338(2) . ? C1 Pd1 2.0661(16) . ? C2 N1 1.480(2) . ? C2 C3 1.523(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.480(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.389(2) . ? C4 C9 1.397(3) . ? C4 N1 1.443(2) . ? C5 C6 1.398(3) . ? C5 C10 1.500(3) . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.383(3) . ? C7 C11 1.510(3) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C12 1.504(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.389(2) . ? C13 C18 1.395(2) . ? C13 N2 1.438(2) . ? C14 C15 1.393(3) . ? C14 C19 1.500(3) . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 C20 1.513(3) . ? C17 C18 1.393(2) . ? C17 H17 0.9500 . ? C18 C21 1.498(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C36 1.393(2) . ? C31 C32 1.397(2) . ? C31 O1 1.4134(18) . ? C32 C33 1.393(2) . ? C32 Pd1 2.0352(15) . ? C33 C34 1.392(2) . ? C33 H33 0.9500 . ? C34 C35 1.394(2) . ? C34 C37 1.540(5) . ? C34 C137 1.564(7) . ? C35 C36 1.391(2) . ? C35 H35 0.9500 . ? C36 C41 1.535(2) . ? C37 C38 1.449(7) . ? C37 C40 1.497(8) . ? C37 C39 1.524(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C137 C138 1.535(12) . ? C137 C140 1.556(12) . ? C137 C139 1.599(12) . ? C138 H13A 0.9800 . ? C138 H13B 0.9800 . ? C138 H13C 0.9800 . ? C139 H13D 0.9800 . ? C139 H13E 0.9800 . ? C139 H13F 0.9800 . ? C140 H14A 0.9800 . ? C140 H14B 0.9800 . ? C140 H14C 0.9800 . ? C41 C42 1.534(3) . ? C41 C44 1.536(3) . ? C41 C43 1.541(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.381(2) . ? C45 C50 1.393(2) . ? C45 O2 1.4081(18) . ? C46 C47 1.383(2) . ? C46 H46 0.9500 . ? C47 C48 1.390(3) . ? C47 H47 0.9500 . ? C48 C49 1.392(3) . ? C48 C51 1.551(4) . ? C48 C151 1.569(7) . ? C49 C50 1.400(2) . ? C49 H49 0.9500 . ? C50 C55 1.534(2) . ? C51 C52 1.521(6) . ? C51 C54 1.521(6) . ? C51 C53 1.531(6) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C151 C152 1.526(12) . ? C151 C154 1.536(11) . ? C151 C153 1.567(10) . ? C152 H15A 0.9800 . ? C152 H15B 0.9800 . ? C152 H15C 0.9800 . ? C153 H15D 0.9800 . ? C153 H15E 0.9800 . ? C153 H15F 0.9800 . ? C154 H15G 0.9800 . ? C154 H15H 0.9800 . ? C154 H15I 0.9800 . ? C55 C57 1.534(2) . ? C55 C58 1.537(2) . ? C55 C56 1.540(2) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.372(2) . ? C59 C64 1.399(2) . ? C59 O3 1.4162(18) . ? C60 C61 1.391(2) . ? C60 H60 0.9500 . ? C61 C62 1.384(3) . ? C61 H61 0.9500 . ? C62 C63 1.391(3) . ? C62 C65 1.533(2) . ? C63 C64 1.399(2) . ? C63 H63 0.9500 . ? C64 C69 1.532(3) . ? C65 C68 1.507(3) . ? C65 C67 1.510(3) . ? C65 C66 1.522(4) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C71 1.533(4) . ? C69 C70 1.541(4) . ? C69 C72 1.541(3) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? O1 P1 1.6046(11) . ? O2 P1 1.5904(11) . ? O3 P1 1.5988(12) . ? P1 Pd1 2.1976(5) . ? Cl1 Pd1 2.3840(5) . ? C81 C82 1.38(2) . ? C81 O81 1.441(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 O81 1.391(5) . ? C83 C84 1.59(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C181 O81 1.405(4) . ? C181 C182 1.523(11) . ? C181 H18A 0.9900 . ? C181 H18B 0.9900 . ? C182 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C183 O81 1.443(4) . ? C183 C184 1.473(15) . ? C183 H18F 0.9900 . ? C183 H18G 0.9900 . ? C184 H18H 0.9800 . ? C184 H18I 0.9800 . ? C184 H18J 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 108.38(14) . . ? N1 C1 Pd1 124.19(12) . . ? N2 C1 Pd1 127.41(11) . . ? N1 C2 C3 102.22(14) . . ? N1 C2 H2A 111.3 . . ? C3 C2 H2A 111.3 . . ? N1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? N2 C3 C2 101.56(14) . . ? N2 C3 H3A 111.5 . . ? C2 C3 H3A 111.5 . . ? N2 C3 H3B 111.5 . . ? C2 C3 H3B 111.5 . . ? H3A C3 H3B 109.3 . . ? C5 C4 C9 121.68(16) . . ? C5 C4 N1 120.41(16) . . ? C9 C4 N1 117.88(16) . . ? C4 C5 C6 118.01(17) . . ? C4 C5 C10 122.56(16) . . ? C6 C5 C10 119.43(17) . . ? C7 C6 C5 121.69(19) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 118.50(18) . . ? C8 C7 C11 121.2(2) . . ? C6 C7 C11 120.3(2) . . ? C7 C8 C9 121.88(19) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C4 118.17(18) . . ? C8 C9 C12 120.56(19) . . ? C4 C9 C12 121.26(18) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 121.05(15) . . ? C14 C13 N2 119.36(16) . . ? C18 C13 N2 119.44(15) . . ? C13 C14 C15 118.05(16) . . ? C13 C14 C19 122.82(17) . . ? C15 C14 C19 119.12(18) . . ? C16 C15 C14 122.39(17) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C17 118.01(16) . . ? C15 C16 C20 120.20(18) . . ? C17 C16 C20 121.77(18) . . ? C16 C17 C18 121.99(17) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C13 118.28(16) . . ? C17 C18 C21 120.44(18) . . ? C13 C18 C21 121.22(17) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 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 . . ? C36 C31 C32 124.88(14) . . ? C36 C31 O1 117.16(13) . . ? C32 C31 O1 117.76(13) . . ? C33 C32 C31 115.83(14) . . ? C33 C32 Pd1 126.65(11) . . ? C31 C32 Pd1 117.39(11) . . ? C34 C33 C32 122.38(15) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 117.97(15) . . ? C33 C34 C37 123.4(3) . . ? C35 C34 C37 118.6(3) . . ? C33 C34 C137 119.3(5) . . ? C35 C34 C137 121.2(5) . . ? C37 C34 C137 14.4(6) . . ? C36 C35 C34 123.00(15) . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C35 C36 C31 115.36(14) . . ? C35 C36 C41 122.66(15) . . ? C31 C36 C41 121.96(15) . . ? C38 C37 C40 111.7(5) . . ? C38 C37 C39 96.7(5) . . ? C40 C37 C39 112.1(4) . . ? C38 C37 C34 116.0(5) . . ? C40 C37 C34 107.3(4) . . ? C39 C37 C34 113.0(4) . . ? C138 C137 C140 92.5(8) . . ? C138 C137 C34 110.5(9) . . ? C140 C137 C34 111.1(7) . . ? C138 C137 C139 128.3(8) . . ? C140 C137 C139 103.1(8) . . ? C34 C137 C139 108.9(7) . . ? C137 C138 H13A 109.5 . . ? C137 C138 H13B 109.5 . . ? H13A C138 H13B 109.5 . . ? C137 C138 H13C 109.5 . . ? H13A C138 H13C 109.5 . . ? H13B C138 H13C 109.5 . . ? C137 C139 H13D 109.5 . . ? C137 C139 H13E 109.5 . . ? H13D C139 H13E 109.5 . . ? C137 C139 H13F 109.5 . . ? H13D C139 H13F 109.5 . . ? H13E C139 H13F 109.5 . . ? C137 C140 H14A 109.5 . . ? C137 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? C137 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? C42 C41 C36 109.91(15) . . ? C42 C41 C44 107.25(17) . . ? C36 C41 C44 111.43(16) . . ? C42 C41 C43 110.08(17) . . ? C36 C41 C43 110.57(15) . . ? C44 C41 C43 107.52(17) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 122.41(15) . . ? C46 C45 O2 120.03(14) . . ? C50 C45 O2 117.56(14) . . ? C45 C46 C47 119.79(16) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C46 C47 C48 120.72(17) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C47 C48 C49 117.60(16) . . ? C47 C48 C51 116.9(3) . . ? C49 C48 C51 125.3(3) . . ? C47 C48 C151 127.8(4) . . ? C49 C48 C151 113.4(4) . . ? C51 C48 C151 19.6(3) . . ? C48 C49 C50 123.75(16) . . ? C48 C49 H49 118.1 . . ? C50 C49 H49 118.1 . . ? C45 C50 C49 115.68(15) . . ? C45 C50 C55 122.55(14) . . ? C49 C50 C55 121.77(14) . . ? C52 C51 C54 110.4(4) . . ? C52 C51 C53 108.8(4) . . ? C54 C51 C53 109.2(5) . . ? C52 C51 C48 111.6(3) . . ? C54 C51 C48 107.5(4) . . ? C53 C51 C48 109.4(3) . . ? C152 C151 C154 109.0(9) . . ? C152 C151 C153 107.3(7) . . ? C154 C151 C153 106.0(9) . . ? C152 C151 C48 107.0(7) . . ? C154 C151 C48 109.8(8) . . ? C153 C151 C48 117.5(6) . . ? C151 C152 H15A 109.5 . . ? C151 C152 H15B 109.5 . . ? H15A C152 H15B 109.5 . . ? C151 C152 H15C 109.5 . . ? H15A C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? C151 C153 H15D 109.5 . . ? C151 C153 H15E 109.5 . . ? H15D C153 H15E 109.5 . . ? C151 C153 H15F 109.5 . . ? H15D C153 H15F 109.5 . . ? H15E C153 H15F 109.5 . . ? C151 C154 H15G 109.5 . . ? C151 C154 H15H 109.5 . . ? H15G C154 H15H 109.5 . . ? C151 C154 H15I 109.5 . . ? H15G C154 H15I 109.5 . . ? H15H C154 H15I 109.5 . . ? C57 C55 C50 111.43(14) . . ? C57 C55 C58 107.84(15) . . ? C50 C55 C58 109.68(14) . . ? C57 C55 C56 107.16(15) . . ? C50 C55 C56 110.58(14) . . ? C58 C55 C56 110.09(14) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C64 121.79(15) . . ? C60 C59 O3 118.93(14) . . ? C64 C59 O3 119.19(15) . . ? C59 C60 C61 120.48(16) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C62 C61 C60 120.63(17) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C61 C62 C63 116.97(16) . . ? C61 C62 C65 122.51(17) . . ? C63 C62 C65 120.52(17) . . ? C62 C63 C64 124.66(17) . . ? C62 C63 H63 117.7 . . ? C64 C63 H63 117.7 . . ? C63 C64 C59 115.42(16) . . ? C63 C64 C69 121.74(16) . . ? C59 C64 C69 122.84(16) . . ? C68 C65 C67 109.4(2) . . ? C68 C65 C66 107.1(2) . . ? C67 C65 C66 108.5(3) . . ? C68 C65 C62 109.84(16) . . ? C67 C65 C62 110.75(18) . . ? C66 C65 C62 111.12(18) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C64 C69 C71 110.8(2) . . ? C64 C69 C70 109.30(19) . . ? C71 C69 C70 110.4(2) . . ? C64 C69 C72 111.27(18) . . ? C71 C69 C72 107.1(2) . . ? C70 C69 C72 108.0(3) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C1 N1 C4 126.13(14) . . ? C1 N1 C2 112.31(14) . . ? C4 N1 C2 121.55(14) . . ? C1 N2 C13 125.56(14) . . ? C1 N2 C3 112.68(14) . . ? C13 N2 C3 119.85(14) . . ? C31 O1 P1 112.50(9) . . ? C45 O2 P1 122.46(10) . . ? C59 O3 P1 123.48(10) . . ? O2 P1 O3 95.21(6) . . ? O2 P1 O1 100.74(6) . . ? O3 P1 O1 106.68(6) . . ? O2 P1 Pd1 122.96(5) . . ? O3 P1 Pd1 122.84(4) . . ? O1 P1 Pd1 105.70(4) . . ? C32 Pd1 C1 94.00(6) . . ? C32 Pd1 P1 79.42(5) . . ? C1 Pd1 P1 172.73(5) . . ? C32 Pd1 Cl1 170.41(4) . . ? C1 Pd1 Cl1 94.59(5) . . ? P1 Pd1 Cl1 91.76(2) . . ? C82 C81 O81 115.7(11) . . ? C82 C81 H81A 108.4 . . ? O81 C81 H81A 108.4 . . ? C82 C81 H81B 108.4 . . ? O81 C81 H81B 108.4 . . ? H81A C81 H81B 107.4 . . ? O81 C83 C84 103.6(10) . . ? O81 C83 H83A 111.0 . . ? C84 C83 H83A 111.0 . . ? O81 C83 H83B 111.0 . . ? C84 C83 H83B 111.0 . . ? H83A C83 H83B 109.0 . . ? O81 C181 C182 110.8(5) . . ? O81 C181 H18A 109.5 . . ? C182 C181 H18A 109.5 . . ? O81 C181 H18B 109.5 . . ? C182 C181 H18B 109.5 . . ? H18A C181 H18B 108.1 . . ? C181 C182 H18C 109.5 . . ? C181 C182 H18D 109.5 . . ? H18C C182 H18D 109.5 . . ? C181 C182 H18E 109.5 . . ? H18C C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? O81 C183 C184 113.5(6) . . ? O81 C183 H18F 108.9 . . ? C184 C183 H18F 108.9 . . ? O81 C183 H18G 108.9 . . ? C184 C183 H18G 108.9 . . ? H18F C183 H18G 107.7 . . ? C183 C184 H18H 109.5 . . ? C183 C184 H18I 109.5 . . ? H18H C184 H18I 109.5 . . ? C183 C184 H18J 109.5 . . ? H18H C184 H18J 109.5 . . ? H18I C184 H18J 109.5 . . ? C83 O81 C181 125.3(3) . . ? C83 O81 C81 113.7(4) . . ? C181 O81 C81 35.0(3) . . ? C83 O81 C183 39.2(3) . . ? C181 O81 C183 117.2(3) . . ? C81 O81 C183 132.8(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.419 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.071