# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2a _database_code_depnum_ccdc_archive 'CCDC 871882' #TrackingRef '10170_web_deposit_cif_file_0_CatherineS.J.Cazin_1331897901.2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety 'C45 H51 Cl2 N2 P Pd' _chemical_formula_sum 'C45 H51 Cl2 N2 P Pd' _chemical_formula_weight 828.15 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' 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 P2(1)2(1)2(1) 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' _cell_length_a 12.7651(7) _cell_length_b 13.7447(9) _cell_length_c 47.075(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8259.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8002 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 23.36 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8295 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81368 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0458 _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 -52 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.75 _reflns_number_total 17555 _reflns_number_gt 16904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+30.6636P] 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 0.04(2) _refine_ls_number_reflns 17555 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63618(3) 0.01115(3) 0.594219(8) 0.02058(8) Uani 1 1 d . . . Cl1 Cl 0.49495(11) 0.10791(10) 0.58473(3) 0.0331(3) Uani 1 1 d . . . Cl2 Cl 0.77934(11) -0.08392(11) 0.60335(3) 0.0353(3) Uani 1 1 d . . . C1 C 0.6220(4) -0.0410(3) 0.55401(10) 0.0195(9) Uani 1 1 d . . . N2 N 0.6846(3) -0.0215(3) 0.53177(8) 0.0192(8) Uani 1 1 d . . . C3 C 0.6418(4) -0.0577(4) 0.50679(10) 0.0227(9) Uani 1 1 d . . . H3A H 0.6704 -0.0526 0.4882 0.027 Uiso 1 1 calc R . . C4 C 0.5519(4) -0.1014(4) 0.51416(11) 0.0246(11) Uani 1 1 d . . . H4A H 0.5048 -0.1338 0.5017 0.029 Uiso 1 1 calc R . . N5 N 0.5405(3) -0.0907(3) 0.54316(8) 0.0197(8) Uani 1 1 d . . . C6 C 0.7861(4) 0.0249(4) 0.53300(10) 0.0206(10) Uani 1 1 d . . . C7 C 0.8736(4) -0.0353(4) 0.53405(10) 0.0238(10) Uani 1 1 d . . . C8 C 0.9711(4) 0.0102(5) 0.53402(14) 0.0360(14) Uani 1 1 d . . . H8A H 1.0331 -0.0280 0.5345 0.043 Uiso 1 1 calc R . . C9 C 0.9784(5) 0.1101(4) 0.53331(14) 0.0369(14) Uani 1 1 d . . . H9A H 1.0455 0.1399 0.5335 0.044 Uiso 1 1 calc R . . C10 C 0.8905(4) 0.1671(4) 0.53236(13) 0.0312(13) Uani 1 1 d . . . H10A H 0.8978 0.2359 0.5319 0.037 Uiso 1 1 calc R . . C11 C 0.7909(4) 0.1265(4) 0.53208(11) 0.0238(11) Uani 1 1 d . . . C12 C 0.8656(5) -0.1444(4) 0.53549(13) 0.0337(13) Uani 1 1 d . . . H12A H 0.7963 -0.1608 0.5442 0.040 Uiso 1 1 calc R . . C13 C 0.8683(6) -0.1891(5) 0.50561(15) 0.0472(16) Uani 1 1 d . . . H13A H 0.8138 -0.1590 0.4939 0.071 Uiso 1 1 calc R . . H13B H 0.8556 -0.2593 0.5069 0.071 Uiso 1 1 calc R . . H13C H 0.9370 -0.1775 0.4970 0.071 Uiso 1 1 calc R . . C14 C 0.9503(5) -0.1921(5) 0.55352(17) 0.0485(18) Uani 1 1 d . . . H14A H 0.9495 -0.1638 0.5726 0.073 Uiso 1 1 calc R . . H14B H 1.0190 -0.1809 0.5448 0.073 Uiso 1 1 calc R . . H14C H 0.9371 -0.2622 0.5548 0.073 Uiso 1 1 calc R . . C15 C 0.6943(5) 0.1883(4) 0.53090(13) 0.0326(13) Uani 1 1 d . . . H15A H 0.6383 0.1529 0.5416 0.039 Uiso 1 1 calc R . . C16 C 0.6575(8) 0.1979(6) 0.50066(19) 0.085(3) Uani 1 1 d . . . H16A H 0.6508 0.1331 0.4922 0.127 Uiso 1 1 calc R . . H16B H 0.7085 0.2361 0.4898 0.127 Uiso 1 1 calc R . . H16C H 0.5894 0.2307 0.5003 0.127 Uiso 1 1 calc R . . C17 C 0.7052(6) 0.2858(5) 0.54420(18) 0.0565(19) Uani 1 1 d . . . H17A H 0.7271 0.2783 0.5640 0.085 Uiso 1 1 calc R . . H17B H 0.6377 0.3198 0.5435 0.085 Uiso 1 1 calc R . . H17C H 0.7579 0.3237 0.5339 0.085 Uiso 1 1 calc R . . C18 C 0.4563(4) -0.1362(3) 0.55891(10) 0.0188(9) Uani 1 1 d . . . C19 C 0.3549(4) -0.0987(4) 0.55618(10) 0.0250(10) Uani 1 1 d . . . C20 C 0.2767(4) -0.1476(4) 0.57078(13) 0.0333(13) Uani 1 1 d . . . H20A H 0.2068 -0.1242 0.5695 0.040 Uiso 1 1 calc R . . C21 C 0.2967(5) -0.2281(5) 0.58690(14) 0.0417(15) Uani 1 1 d . . . H21A H 0.2410 -0.2602 0.5965 0.050 Uiso 1 1 calc R . . C22 C 0.3982(5) -0.2627(4) 0.58930(13) 0.0346(13) Uani 1 1 d . . . H22A H 0.4119 -0.3179 0.6009 0.042 Uiso 1 1 calc R . . C23 C 0.4804(4) -0.2177(4) 0.57494(12) 0.0261(11) Uani 1 1 d . . . C24 C 0.3286(4) -0.0097(4) 0.53834(11) 0.0269(11) Uani 1 1 d . . . H24A H 0.3955 0.0240 0.5332 0.032 Uiso 1 1 calc R . . C25 C 0.2730(5) -0.0402(5) 0.51086(12) 0.0362(13) Uani 1 1 d . . . H25A H 0.3175 -0.0857 0.5003 0.054 Uiso 1 1 calc R . . H25B H 0.2595 0.0175 0.4992 0.054 Uiso 1 1 calc R . . H25C H 0.2064 -0.0719 0.5155 0.054 Uiso 1 1 calc R . . C26 C 0.2595(4) 0.0617(4) 0.55465(14) 0.0361(13) Uani 1 1 d . . . H26A H 0.2952 0.0817 0.5721 0.054 Uiso 1 1 calc R . . H26B H 0.1929 0.0302 0.5595 0.054 Uiso 1 1 calc R . . H26C H 0.2459 0.1191 0.5428 0.054 Uiso 1 1 calc R . . C27 C 0.5894(5) -0.2581(4) 0.57660(13) 0.0315(12) Uani 1 1 d . . . H27A H 0.6388 -0.2018 0.5749 0.038 Uiso 1 1 calc R . . C28 C 0.6116(6) -0.3263(6) 0.55143(18) 0.061(2) Uani 1 1 d . . . H28A H 0.5958 -0.2926 0.5336 0.091 Uiso 1 1 calc R . . H28B H 0.5675 -0.3845 0.5530 0.091 Uiso 1 1 calc R . . H28C H 0.6855 -0.3455 0.5516 0.091 Uiso 1 1 calc R . . C29 C 0.6132(7) -0.3081(7) 0.60479(18) 0.075(3) Uani 1 1 d . . . H29A H 0.5996 -0.2629 0.6205 0.112 Uiso 1 1 calc R . . H29B H 0.6869 -0.3280 0.6052 0.112 Uiso 1 1 calc R . . H29C H 0.5685 -0.3656 0.6068 0.112 Uiso 1 1 calc R . . P1 P 0.63400(11) 0.07523(9) 0.63947(3) 0.0240(3) Uani 1 1 d . . . C31 C 0.6042(5) 0.2051(4) 0.63935(12) 0.0324(13) Uani 1 1 d . . . C32 C 0.5106(5) 0.2405(4) 0.65031(13) 0.0406(15) Uani 1 1 d . . . H32A H 0.4649 0.1981 0.6603 0.049 Uiso 1 1 calc R . . C33 C 0.4840(7) 0.3362(5) 0.64675(15) 0.0538(19) Uani 1 1 d . . . H33A H 0.4198 0.3602 0.6541 0.065 Uiso 1 1 calc R . . C34 C 0.5507(8) 0.3972(5) 0.63248(17) 0.063(2) Uani 1 1 d . . . H34A H 0.5321 0.4635 0.6300 0.075 Uiso 1 1 calc R . . C35 C 0.6433(8) 0.3639(5) 0.62185(17) 0.065(2) Uani 1 1 d . . . H35A H 0.6899 0.4072 0.6125 0.078 Uiso 1 1 calc R . . C36 C 0.6689(6) 0.2663(5) 0.62478(14) 0.0475(17) Uani 1 1 d . . . H36A H 0.7318 0.2420 0.6166 0.057 Uiso 1 1 calc R . . C37 C 0.7509(4) 0.0584(4) 0.66125(10) 0.0255(11) Uani 1 1 d . . . C38 C 0.8222(5) 0.1315(4) 0.66672(13) 0.0363(13) Uani 1 1 d . . . H38A H 0.8080 0.1961 0.6606 0.044 Uiso 1 1 calc R . . C39 C 0.9138(5) 0.1113(5) 0.68091(14) 0.0422(15) Uani 1 1 d . . . H39A H 0.9625 0.1620 0.6845 0.051 Uiso 1 1 calc R . . C40 C 0.9351(4) 0.0190(4) 0.68984(12) 0.0336(13) Uani 1 1 d . . . H40A H 0.9986 0.0056 0.6996 0.040 Uiso 1 1 calc R . . C41 C 0.8647(5) -0.0545(4) 0.68470(11) 0.0339(12) Uani 1 1 d . . . H41A H 0.8790 -0.1187 0.6911 0.041 Uiso 1 1 calc R . . C42 C 0.7731(5) -0.0349(4) 0.67021(12) 0.0301(12) Uani 1 1 d . . . H42A H 0.7251 -0.0860 0.6664 0.036 Uiso 1 1 calc R . . C43 C 0.5329(4) 0.0177(4) 0.66061(11) 0.0283(11) Uani 1 1 d . . . C44 C 0.4606(4) -0.0423(4) 0.64760(12) 0.0324(12) Uani 1 1 d . . . H44A H 0.4628 -0.0515 0.6276 0.039 Uiso 1 1 calc R . . C45 C 0.3844(5) -0.0894(5) 0.66377(14) 0.0441(15) Uani 1 1 d . . . H45A H 0.3352 -0.1315 0.6549 0.053 Uiso 1 1 calc R . . C46 C 0.3814(5) -0.0744(5) 0.69246(14) 0.0456(16) Uani 1 1 d . . . H46A H 0.3297 -0.1065 0.7035 0.055 Uiso 1 1 calc R . . C47 C 0.4515(6) -0.0141(6) 0.70541(15) 0.0495(16) Uani 1 1 d . . . H47A H 0.4473 -0.0036 0.7253 0.059 Uiso 1 1 calc R . . C48 C 0.5278(5) 0.0313(5) 0.68991(13) 0.0405(15) Uani 1 1 d . . . H48A H 0.5773 0.0722 0.6991 0.049 Uiso 1 1 calc R . . Pd51 Pd 0.15874(3) 0.44944(3) 0.655690(7) 0.01893(8) Uani 1 1 d . . . Cl51 Cl 0.28793(10) 0.55620(10) 0.64262(3) 0.0294(3) Uani 1 1 d . . . Cl52 Cl 0.02849(11) 0.34465(10) 0.66845(3) 0.0324(3) Uani 1 1 d . . . C51 C 0.1467(4) 0.5078(3) 0.69526(10) 0.0202(9) Uani 1 1 d . . . N52 N 0.2145(3) 0.4986(3) 0.71692(9) 0.0238(9) Uani 1 1 d . . . C53 C 0.1744(4) 0.5379(4) 0.74171(11) 0.0325(13) Uani 1 1 d . . . H53A H 0.2074 0.5400 0.7598 0.039 Uiso 1 1 calc R . . C54 C 0.0798(4) 0.5725(4) 0.73497(11) 0.0320(13) Uani 1 1 d . . . H54A H 0.0324 0.6039 0.7475 0.038 Uiso 1 1 calc R . . N55 N 0.0636(3) 0.5543(3) 0.70648(9) 0.0238(9) Uani 1 1 d . . . C56 C 0.3147(4) 0.4511(4) 0.71577(11) 0.0257(11) Uani 1 1 d . . . C57 C 0.3163(4) 0.3496(4) 0.72024(11) 0.0304(12) Uani 1 1 d . . . C58 C 0.4137(5) 0.3054(5) 0.72072(14) 0.0380(14) Uani 1 1 d . . . H58A H 0.4179 0.2371 0.7235 0.046 Uiso 1 1 calc R . . C59 C 0.5045(5) 0.3580(5) 0.71735(13) 0.0437(16) Uani 1 1 d . . . H59A H 0.5706 0.3261 0.7178 0.052 Uiso 1 1 calc R . . C60 C 0.4990(4) 0.4568(5) 0.71336(13) 0.0370(13) Uani 1 1 d . . . H60A H 0.5623 0.4926 0.7115 0.044 Uiso 1 1 calc R . . C61 C 0.4041(4) 0.5066(5) 0.71186(11) 0.0304(12) Uani 1 1 d . . . C62 C 0.4005(4) 0.6152(4) 0.70746(12) 0.0311(12) Uani 1 1 d . . . H62A H 0.3310 0.6318 0.6989 0.037 Uiso 1 1 calc R . . C63 C 0.4088(7) 0.6673(6) 0.73585(15) 0.056(2) Uani 1 1 d . . . H63A H 0.3531 0.6445 0.7485 0.084 Uiso 1 1 calc R . . H63B H 0.4016 0.7376 0.7329 0.084 Uiso 1 1 calc R . . H63C H 0.4772 0.6535 0.7444 0.084 Uiso 1 1 calc R . . C64 C 0.4859(5) 0.6502(5) 0.68716(16) 0.0475(16) Uani 1 1 d . . . H64A H 0.4789 0.6163 0.6689 0.071 Uiso 1 1 calc R . . H64B H 0.5548 0.6362 0.6954 0.071 Uiso 1 1 calc R . . H64C H 0.4787 0.7204 0.6842 0.071 Uiso 1 1 calc R . . C65 C 0.2194(5) 0.2905(4) 0.72562(13) 0.0344(13) Uani 1 1 d . . . H65A H 0.1572 0.3321 0.7212 0.041 Uiso 1 1 calc R . . C66 C 0.2143(7) 0.2630(6) 0.75718(15) 0.0540(19) Uani 1 1 d . . . H66A H 0.2176 0.3221 0.7688 0.081 Uiso 1 1 calc R . . H66B H 0.2736 0.2206 0.7619 0.081 Uiso 1 1 calc R . . H66C H 0.1486 0.2286 0.7610 0.081 Uiso 1 1 calc R . . C67 C 0.2136(6) 0.2004(5) 0.70709(15) 0.0504(17) Uani 1 1 d . . . H67A H 0.2161 0.2195 0.6870 0.076 Uiso 1 1 calc R . . H67B H 0.1479 0.1658 0.7109 0.076 Uiso 1 1 calc R . . H67C H 0.2729 0.1576 0.7114 0.076 Uiso 1 1 calc R . . C68 C -0.0313(4) 0.5815(4) 0.69205(10) 0.0226(10) Uani 1 1 d . . . C69 C -0.1232(4) 0.5300(4) 0.69797(11) 0.0290(11) Uani 1 1 d . . . C70 C -0.2145(4) 0.5612(5) 0.68479(14) 0.0408(15) Uani 1 1 d . . . H70A H -0.2784 0.5280 0.6884 0.049 Uiso 1 1 calc R . . C71 C -0.2141(5) 0.6395(6) 0.66652(13) 0.0435(16) Uani 1 1 d . . . H71A H -0.2777 0.6606 0.6581 0.052 Uiso 1 1 calc R . . C72 C -0.1224(5) 0.6874(5) 0.66039(12) 0.0370(13) Uani 1 1 d . . . H72A H -0.1230 0.7398 0.6472 0.044 Uiso 1 1 calc R . . C73 C -0.0288(4) 0.6603(4) 0.67317(11) 0.0274(11) Uani 1 1 d . . . C74 C -0.1269(4) 0.4456(4) 0.71868(13) 0.0361(12) Uani 1 1 d . . . H74A H -0.0536 0.4222 0.7219 0.043 Uiso 1 1 calc R . . C75 C -0.1719(6) 0.4787(5) 0.74745(14) 0.0525(19) Uani 1 1 d . . . H75A H -0.1302 0.5329 0.7548 0.079 Uiso 1 1 calc R . . H75B H -0.1696 0.4244 0.7609 0.079 Uiso 1 1 calc R . . H75C H -0.2447 0.4998 0.7449 0.079 Uiso 1 1 calc R . . C76 C -0.1911(6) 0.3612(5) 0.7073(2) 0.062(2) Uani 1 1 d . . . H76A H -0.1621 0.3397 0.6891 0.094 Uiso 1 1 calc R . . H76B H -0.2638 0.3821 0.7046 0.094 Uiso 1 1 calc R . . H76C H -0.1890 0.3073 0.7209 0.094 Uiso 1 1 calc R . . C77 C 0.0722(5) 0.7140(4) 0.66698(15) 0.0375(14) Uani 1 1 d . . . H77A H 0.1283 0.6638 0.6646 0.045 Uiso 1 1 calc R . . C78 C 0.1046(5) 0.7789(5) 0.69183(19) 0.057(2) Uani 1 1 d . . . H78A H 0.1071 0.7402 0.7093 0.085 Uiso 1 1 calc R . . H78B H 0.0534 0.8315 0.6941 0.085 Uiso 1 1 calc R . . H78C H 0.1739 0.8067 0.6881 0.085 Uiso 1 1 calc R . . C79 C 0.0677(7) 0.7720(5) 0.63948(19) 0.064(2) Uani 1 1 d . . . H79A H 0.0469 0.7290 0.6238 0.095 Uiso 1 1 calc R . . H79B H 0.1368 0.7997 0.6355 0.095 Uiso 1 1 calc R . . H79C H 0.0163 0.8246 0.6414 0.095 Uiso 1 1 calc R . . P51 P 0.15076(10) 0.37858(9) 0.61132(3) 0.0212(2) Uani 1 1 d . . . C81 C 0.1273(5) 0.2490(4) 0.61275(11) 0.0301(12) Uani 1 1 d . . . C82 C 0.0366(5) 0.2062(4) 0.60337(14) 0.0396(15) Uani 1 1 d . . . H82A H -0.0150 0.2447 0.5942 0.047 Uiso 1 1 calc R . . C83 C 0.0193(7) 0.1071(5) 0.60715(14) 0.0506(19) Uani 1 1 d . . . H83A H -0.0434 0.0779 0.6004 0.061 Uiso 1 1 calc R . . C84 C 0.0927(8) 0.0522(5) 0.62063(16) 0.068(3) Uani 1 1 d . . . H84A H 0.0804 -0.0152 0.6234 0.081 Uiso 1 1 calc R . . C85 C 0.1835(8) 0.0926(5) 0.63014(15) 0.059(2) Uani 1 1 d . . . H85A H 0.2342 0.0532 0.6394 0.071 Uiso 1 1 calc R . . C86 C 0.2023(6) 0.1915(5) 0.62631(13) 0.0427(15) Uani 1 1 d . . . H86A H 0.2657 0.2196 0.6329 0.051 Uiso 1 1 calc R . . C87 C 0.2569(4) 0.3956(4) 0.58579(11) 0.0246(11) Uani 1 1 d . . . C88 C 0.3196(5) 0.3210(4) 0.57689(12) 0.0321(12) Uani 1 1 d . . . H88A H 0.3098 0.2574 0.5843 0.039 Uiso 1 1 calc R . . C89 C 0.3979(5) 0.3383(5) 0.55688(14) 0.0420(15) Uani 1 1 d . . . H89A H 0.4414 0.2864 0.5506 0.050 Uiso 1 1 calc R . . C90 C 0.4123(5) 0.4299(5) 0.54622(13) 0.0430(15) Uani 1 1 d . . . H90A H 0.4655 0.4411 0.5325 0.052 Uiso 1 1 calc R . . C91 C 0.3506(5) 0.5057(5) 0.55511(11) 0.0372(12) Uani 1 1 d . . . H91A H 0.3608 0.5692 0.5476 0.045 Uiso 1 1 calc R . . C92 C 0.2723(4) 0.4884(4) 0.57544(11) 0.0290(11) Uani 1 1 d . . . H92A H 0.2299 0.5405 0.5820 0.035 Uiso 1 1 calc R . . C93 C 0.0403(4) 0.4289(3) 0.59237(11) 0.0232(10) Uani 1 1 d . . . C94 C -0.0335(5) 0.4850(4) 0.60626(12) 0.0354(13) Uani 1 1 d . . . H94A H -0.0260 0.4965 0.6261 0.042 Uiso 1 1 calc R . . C95 C -0.1177(5) 0.5245(5) 0.59201(14) 0.0489(17) Uani 1 1 d . . . H95A H -0.1681 0.5625 0.6019 0.059 Uiso 1 1 calc R . . C96 C -0.1281(5) 0.5084(5) 0.56317(13) 0.0433(15) Uani 1 1 d . . . H96A H -0.1857 0.5355 0.5532 0.052 Uiso 1 1 calc R . . C97 C -0.0555(4) 0.4534(5) 0.54899(12) 0.0349(12) Uani 1 1 d . . . H97A H -0.0631 0.4425 0.5292 0.042 Uiso 1 1 calc R . . C98 C 0.0277(5) 0.4141(4) 0.56321(12) 0.0312(12) Uani 1 1 d . . . H98A H 0.0777 0.3762 0.5531 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02116(17) 0.02053(17) 0.02005(16) -0.00084(14) -0.00154(14) -0.00077(14) Cl1 0.0355(7) 0.0304(7) 0.0335(7) -0.0064(5) -0.0087(6) 0.0113(6) Cl2 0.0305(7) 0.0452(8) 0.0301(7) -0.0073(6) -0.0080(5) 0.0116(6) C1 0.021(2) 0.017(2) 0.021(2) -0.0007(18) -0.0038(18) 0.0013(18) N2 0.0179(19) 0.023(2) 0.0167(18) -0.0021(15) 0.0016(15) -0.0016(16) C3 0.022(2) 0.025(2) 0.020(2) -0.0010(19) 0.0055(19) -0.004(2) C4 0.026(3) 0.026(3) 0.022(2) -0.004(2) 0.001(2) -0.004(2) N5 0.0170(19) 0.022(2) 0.020(2) -0.0016(16) 0.0000(16) 0.0008(16) C6 0.017(2) 0.025(3) 0.020(2) 0.0027(19) -0.0032(18) -0.0052(19) C7 0.022(2) 0.023(3) 0.026(2) 0.0031(19) 0.006(2) 0.002(2) C8 0.015(2) 0.041(3) 0.051(4) 0.004(3) 0.002(2) 0.003(2) C9 0.025(3) 0.034(3) 0.052(4) 0.014(3) -0.006(3) -0.009(2) C10 0.029(3) 0.028(3) 0.036(3) 0.005(2) -0.005(2) -0.006(2) C11 0.026(3) 0.024(3) 0.021(2) 0.001(2) -0.002(2) -0.005(2) C12 0.023(3) 0.026(3) 0.052(4) 0.001(2) 0.006(3) 0.005(2) C13 0.046(4) 0.038(3) 0.058(4) -0.007(3) 0.015(3) 0.008(3) C14 0.040(4) 0.031(3) 0.074(5) 0.013(3) 0.009(3) 0.011(3) C15 0.031(3) 0.026(3) 0.040(3) 0.008(2) -0.002(2) 0.001(2) C16 0.107(8) 0.070(5) 0.078(6) -0.009(5) -0.064(6) 0.040(6) C17 0.051(4) 0.042(4) 0.076(5) -0.006(4) 0.000(4) 0.008(3) C18 0.024(2) 0.017(2) 0.016(2) -0.0012(17) 0.0038(18) -0.0036(18) C19 0.024(2) 0.023(2) 0.028(2) -0.0012(19) 0.002(2) -0.003(2) C20 0.019(3) 0.040(3) 0.041(3) -0.001(3) 0.009(2) -0.003(2) C21 0.041(3) 0.039(3) 0.045(4) 0.009(3) 0.015(3) -0.013(3) C22 0.043(3) 0.023(3) 0.038(3) 0.012(2) 0.004(3) -0.003(2) C23 0.026(3) 0.023(3) 0.030(3) -0.002(2) 0.002(2) -0.002(2) C24 0.022(2) 0.023(2) 0.036(3) 0.001(2) -0.004(2) 0.003(2) C25 0.036(3) 0.039(3) 0.034(3) 0.002(3) -0.003(2) 0.007(3) C26 0.025(3) 0.032(3) 0.051(4) -0.008(3) -0.002(2) 0.008(2) C27 0.031(3) 0.025(3) 0.038(3) 0.008(2) -0.005(2) 0.006(2) C28 0.046(4) 0.056(5) 0.081(6) -0.022(4) -0.008(4) 0.019(3) C29 0.065(6) 0.098(7) 0.061(5) 0.048(5) -0.010(4) 0.012(5) P1 0.0298(7) 0.0217(6) 0.0204(6) -0.0022(5) -0.0017(5) -0.0008(5) C31 0.044(3) 0.027(3) 0.026(3) -0.004(2) -0.010(2) -0.002(2) C32 0.053(4) 0.034(3) 0.035(3) -0.005(2) 0.002(3) 0.006(3) C33 0.075(5) 0.036(4) 0.051(4) -0.003(3) 0.006(4) 0.023(4) C34 0.106(7) 0.028(4) 0.053(4) -0.005(3) 0.004(5) 0.010(4) C35 0.101(7) 0.028(3) 0.065(5) 0.009(3) 0.015(5) -0.005(4) C36 0.066(5) 0.034(3) 0.043(4) 0.004(3) 0.014(3) 0.001(3) C37 0.033(3) 0.026(3) 0.017(2) -0.009(2) -0.0002(19) -0.006(2) C38 0.041(3) 0.030(3) 0.038(3) -0.001(2) -0.010(3) -0.003(2) C39 0.040(3) 0.040(4) 0.046(4) -0.006(3) -0.010(3) -0.008(3) C40 0.032(3) 0.043(3) 0.027(3) -0.006(2) -0.005(2) -0.002(2) C41 0.039(3) 0.035(3) 0.027(3) 0.001(2) 0.004(2) 0.003(3) C42 0.037(3) 0.024(3) 0.030(3) 0.002(2) -0.004(2) -0.008(2) C43 0.031(3) 0.027(3) 0.027(3) 0.001(2) 0.001(2) 0.003(2) C44 0.032(3) 0.033(3) 0.032(3) 0.001(2) 0.001(2) -0.002(2) C45 0.040(3) 0.046(4) 0.046(4) 0.004(3) 0.003(3) -0.008(3) C46 0.042(4) 0.053(4) 0.041(3) 0.016(3) 0.013(3) 0.000(3) C47 0.053(4) 0.055(4) 0.040(4) 0.001(3) 0.009(3) 0.004(3) C48 0.038(3) 0.053(4) 0.030(3) -0.006(3) 0.002(2) -0.001(3) Pd51 0.01962(17) 0.01911(16) 0.01805(16) -0.00021(14) 0.00139(14) 0.00105(14) Cl51 0.0289(6) 0.0295(6) 0.0296(6) -0.0021(5) 0.0054(5) -0.0082(6) Cl52 0.0364(7) 0.0303(7) 0.0304(7) -0.0032(5) 0.0104(6) -0.0104(6) C51 0.019(2) 0.014(2) 0.028(2) 0.0016(17) 0.0007(19) -0.0041(19) N52 0.0186(19) 0.030(2) 0.022(2) -0.0017(19) -0.0031(16) -0.0002(19) C53 0.030(3) 0.049(4) 0.018(2) -0.012(2) -0.006(2) 0.005(3) C54 0.033(3) 0.047(4) 0.015(2) -0.008(2) 0.003(2) 0.010(3) N55 0.024(2) 0.025(2) 0.022(2) -0.0039(18) -0.0001(16) 0.0003(18) C56 0.024(2) 0.027(2) 0.026(2) 0.005(2) -0.002(2) 0.010(2) C57 0.027(3) 0.040(3) 0.024(3) 0.006(2) -0.002(2) 0.007(2) C58 0.035(3) 0.037(3) 0.042(4) 0.016(3) 0.007(3) 0.008(3) C59 0.034(3) 0.060(4) 0.037(3) 0.020(3) 0.007(3) 0.021(3) C60 0.022(3) 0.046(4) 0.043(3) 0.006(3) -0.002(2) 0.000(3) C61 0.030(3) 0.041(3) 0.020(2) 0.001(2) -0.004(2) 0.005(3) C62 0.028(3) 0.030(3) 0.035(3) 0.000(2) -0.007(2) -0.003(2) C63 0.076(5) 0.049(4) 0.043(4) -0.014(3) -0.001(4) -0.011(4) C64 0.032(3) 0.049(4) 0.061(4) 0.003(3) 0.000(3) -0.006(3) C65 0.036(3) 0.031(3) 0.036(3) 0.005(2) 0.001(3) 0.002(2) C66 0.068(5) 0.049(4) 0.044(4) -0.002(3) 0.016(4) -0.002(4) C67 0.065(5) 0.041(4) 0.046(4) 0.007(3) -0.005(4) -0.004(3) C68 0.021(2) 0.026(3) 0.021(2) -0.0030(19) 0.0007(19) 0.0029(19) C69 0.031(3) 0.028(3) 0.028(3) -0.005(2) 0.005(2) 0.000(2) C70 0.018(3) 0.055(4) 0.049(4) -0.015(3) 0.002(2) -0.001(3) C71 0.031(3) 0.069(5) 0.031(3) -0.004(3) -0.002(3) 0.011(3) C72 0.042(3) 0.046(3) 0.023(3) 0.004(2) 0.001(2) 0.011(3) C73 0.032(3) 0.026(3) 0.024(3) -0.005(2) 0.002(2) 0.005(2) C74 0.029(3) 0.035(3) 0.045(3) 0.004(3) 0.016(2) 0.004(3) C75 0.057(4) 0.055(4) 0.046(4) 0.016(3) 0.026(3) 0.020(3) C76 0.044(4) 0.037(4) 0.107(7) -0.008(4) 0.034(4) -0.012(3) C77 0.031(3) 0.020(3) 0.062(4) 0.006(3) 0.017(3) 0.003(2) C78 0.035(4) 0.037(4) 0.097(6) -0.006(4) -0.001(4) -0.006(3) C79 0.071(5) 0.037(4) 0.083(6) 0.023(4) 0.029(5) 0.008(4) P51 0.0233(6) 0.0200(6) 0.0202(6) -0.0013(4) 0.0021(5) 0.0011(5) C81 0.041(3) 0.026(3) 0.022(2) 0.004(2) 0.012(2) 0.000(2) C82 0.045(4) 0.033(3) 0.041(3) -0.008(3) 0.010(3) -0.013(3) C83 0.084(5) 0.028(3) 0.039(4) -0.014(3) 0.024(4) -0.021(3) C84 0.131(8) 0.023(3) 0.049(4) 0.006(3) 0.030(5) -0.004(5) C85 0.106(7) 0.034(4) 0.037(4) 0.008(3) 0.014(4) 0.024(4) C86 0.064(4) 0.033(3) 0.031(3) 0.004(3) 0.005(3) 0.013(3) C87 0.028(3) 0.024(3) 0.022(3) 0.001(2) 0.000(2) 0.001(2) C88 0.040(3) 0.022(3) 0.034(3) -0.001(2) 0.008(2) 0.005(2) C89 0.040(3) 0.041(4) 0.045(4) -0.010(3) 0.019(3) -0.002(3) C90 0.038(3) 0.055(4) 0.036(3) -0.004(3) 0.015(3) -0.002(3) C91 0.040(3) 0.039(3) 0.032(3) 0.005(2) 0.006(3) -0.007(3) C92 0.037(3) 0.028(3) 0.022(2) -0.003(2) 0.002(2) 0.003(2) C93 0.026(2) 0.020(2) 0.023(2) 0.002(2) -0.004(2) -0.0040(18) C94 0.035(3) 0.041(3) 0.030(3) -0.007(3) -0.005(2) 0.009(3) C95 0.039(3) 0.064(4) 0.043(3) -0.013(3) -0.007(3) 0.025(3) C96 0.036(3) 0.053(4) 0.041(3) -0.001(3) -0.011(3) 0.014(3) C97 0.035(3) 0.039(3) 0.030(3) 0.001(3) -0.002(2) 0.002(3) C98 0.033(3) 0.033(3) 0.028(3) -0.001(2) -0.001(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.032(5) . ? Pd1 Cl1 2.2845(13) . ? Pd1 Cl2 2.2873(14) . ? Pd1 P1 2.3054(13) . ? C1 N2 1.344(6) . ? C1 N5 1.345(6) . ? N2 C3 1.389(6) . ? N2 C6 1.446(6) . ? C3 C4 1.340(7) . ? C3 H3A 0.9500 . ? C4 N5 1.381(6) . ? C4 H4A 0.9500 . ? N5 C18 1.449(6) . ? C6 C7 1.391(7) . ? C6 C11 1.398(7) . ? C7 C8 1.393(7) . ? C7 C12 1.505(7) . ? C8 C9 1.375(9) . ? C8 H8A 0.9500 . ? C9 C10 1.370(9) . ? C9 H9A 0.9500 . ? C10 C11 1.389(7) . ? C10 H10A 0.9500 . ? C11 C15 1.499(8) . ? C12 C14 1.523(9) . ? C12 C13 1.535(9) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.486(9) . ? C15 C16 1.505(9) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.385(7) . ? C18 C19 1.398(7) . ? C19 C20 1.386(7) . ? C19 C24 1.522(7) . ? C20 C21 1.366(9) . ? C20 H20A 0.9500 . ? C21 C22 1.385(9) . ? C21 H21A 0.9500 . ? C22 C23 1.394(8) . ? C22 H22A 0.9500 . ? C23 C27 1.500(8) . ? C24 C26 1.527(7) . ? C24 C25 1.534(7) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.525(8) . ? C27 C28 1.538(9) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C43 1.812(6) . ? P1 C37 1.825(5) . ? P1 C31 1.826(6) . ? C31 C36 1.364(9) . ? C31 C32 1.389(9) . ? C32 C33 1.369(9) . ? C32 H32A 0.9500 . ? C33 C34 1.371(11) . ? C33 H33A 0.9500 . ? C34 C35 1.363(12) . ? C34 H34A 0.9500 . ? C35 C36 1.387(9) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.380(7) . ? C37 C38 1.380(8) . ? C38 C39 1.374(9) . ? C38 H38A 0.9500 . ? C39 C40 1.363(9) . ? C39 H39A 0.9500 . ? C40 C41 1.374(8) . ? C40 H40A 0.9500 . ? C41 C42 1.380(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.381(8) . ? C43 C48 1.394(8) . ? C44 C45 1.394(8) . ? C44 H44A 0.9500 . ? C45 C46 1.366(9) . ? C45 H45A 0.9500 . ? C46 C47 1.363(10) . ? C46 H46A 0.9500 . ? C47 C48 1.368(9) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? Pd51 C51 2.034(5) . ? Pd51 Cl52 2.2803(14) . ? Pd51 Cl51 2.2915(13) . ? Pd51 P51 2.3069(12) . ? C51 N52 1.343(6) . ? C51 N55 1.347(6) . ? N52 C53 1.384(6) . ? N52 C56 1.436(6) . ? C53 C54 1.335(8) . ? C53 H53A 0.9500 . ? C54 N55 1.380(6) . ? C54 H54A 0.9500 . ? N55 C68 1.438(6) . ? C56 C61 1.385(8) . ? C56 C57 1.411(8) . ? C57 C58 1.383(8) . ? C57 C65 1.502(8) . ? C58 C59 1.375(9) . ? C58 H58A 0.9500 . ? C59 C60 1.374(9) . ? C59 H59A 0.9500 . ? C60 C61 1.392(8) . ? C60 H60A 0.9500 . ? C61 C62 1.508(8) . ? C62 C63 1.520(9) . ? C62 C64 1.527(9) . ? C62 H62A 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C67 1.517(9) . ? C65 C66 1.534(9) . ? C65 H65A 1.0000 . ? 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 C69 1.397(7) . ? C68 C73 1.402(7) . ? C69 C70 1.389(8) . ? C69 C74 1.516(8) . ? C70 C71 1.378(10) . ? C70 H70A 0.9500 . ? C71 C72 1.373(9) . ? C71 H71A 0.9500 . ? C72 C73 1.388(8) . ? C72 H72A 0.9500 . ? C73 C77 1.514(8) . ? C74 C76 1.517(9) . ? C74 C75 1.540(8) . ? C74 H74A 1.0000 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C79 1.522(10) . ? C77 C78 1.529(10) . ? C77 H77A 1.0000 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? P51 C93 1.807(5) . ? P51 C81 1.808(5) . ? P51 C87 1.826(5) . ? C81 C82 1.371(9) . ? C81 C86 1.396(9) . ? C82 C83 1.391(9) . ? C82 H82A 0.9500 . ? C83 C84 1.359(12) . ? C83 H83A 0.9500 . ? C84 C85 1.361(13) . ? C84 H84A 0.9500 . ? C85 C86 1.391(10) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C87 C88 1.366(7) . ? C87 C92 1.379(8) . ? C88 C89 1.394(8) . ? C88 H88A 0.9500 . ? C89 C90 1.368(9) . ? C89 H89A 0.9500 . ? C90 C91 1.371(9) . ? C90 H90A 0.9500 . ? C91 C92 1.405(8) . ? C91 H91A 0.9500 . ? C92 H92A 0.9500 . ? C93 C94 1.381(7) . ? C93 C98 1.397(7) . ? C94 C95 1.379(8) . ? C94 H94A 0.9500 . ? C95 C96 1.382(9) . ? C95 H95A 0.9500 . ? C96 C97 1.369(8) . ? C96 H96A 0.9500 . ? C97 C98 1.367(8) . ? C97 H97A 0.9500 . ? C98 H98A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl1 87.30(13) . . ? C1 Pd1 Cl2 92.57(13) . . ? Cl1 Pd1 Cl2 179.06(6) . . ? C1 Pd1 P1 173.95(14) . . ? Cl1 Pd1 P1 87.06(5) . . ? Cl2 Pd1 P1 93.11(5) . . ? N2 C1 N5 105.3(4) . . ? N2 C1 Pd1 127.1(3) . . ? N5 C1 Pd1 127.0(3) . . ? C1 N2 C3 110.8(4) . . ? C1 N2 C6 126.1(4) . . ? C3 N2 C6 123.0(4) . . ? C4 C3 N2 106.1(4) . . ? C4 C3 H3A 126.9 . . ? N2 C3 H3A 126.9 . . ? C3 C4 N5 107.4(4) . . ? C3 C4 H4A 126.3 . . ? N5 C4 H4A 126.3 . . ? C1 N5 C4 110.4(4) . . ? C1 N5 C18 126.8(4) . . ? C4 N5 C18 122.6(4) . . ? C7 C6 C11 124.1(5) . . ? C7 C6 N2 117.3(4) . . ? C11 C6 N2 118.6(5) . . ? C6 C7 C8 116.7(5) . . ? C6 C7 C12 122.7(5) . . ? C8 C7 C12 120.6(5) . . ? C9 C8 C7 120.6(5) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 121.3(5) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C6 116.2(5) . . ? C10 C11 C15 121.7(5) . . ? C6 C11 C15 122.1(5) . . ? C7 C12 C14 113.9(5) . . ? C7 C12 C13 110.8(5) . . ? C14 C12 C13 108.9(5) . . ? C7 C12 H12A 107.7 . . ? C14 C12 H12A 107.7 . . ? C13 C12 H12A 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 114.8(5) . . ? C17 C15 C16 110.4(6) . . ? C11 C15 C16 110.0(6) . . ? C17 C15 H15A 107.1 . . ? C11 C15 H15A 107.1 . . ? C16 C15 H15A 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 123.6(5) . . ? C23 C18 N5 117.6(4) . . ? C19 C18 N5 118.7(4) . . ? C20 C19 C18 116.3(5) . . ? C20 C19 C24 120.3(5) . . ? C18 C19 C24 123.4(4) . . ? C21 C20 C19 122.2(5) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C20 C21 C22 119.9(5) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C18 C23 C22 117.1(5) . . ? C18 C23 C27 122.3(5) . . ? C22 C23 C27 120.6(5) . . ? C19 C24 C26 111.5(5) . . ? C19 C24 C25 110.3(4) . . ? C26 C24 C25 109.4(4) . . ? C19 C24 H24A 108.5 . . ? C26 C24 H24A 108.5 . . ? C25 C24 H24A 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 113.4(6) . . ? C23 C27 C28 110.9(5) . . ? C29 C27 C28 111.0(6) . . ? C23 C27 H27A 107.1 . . ? C29 C27 H27A 107.1 . . ? C28 C27 H27A 107.1 . . ? 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 . . ? C43 P1 C37 102.6(2) . . ? C43 P1 C31 106.3(3) . . ? C37 P1 C31 107.2(3) . . ? C43 P1 Pd1 110.44(18) . . ? C37 P1 Pd1 117.44(17) . . ? C31 P1 Pd1 111.92(18) . . ? C36 C31 C32 119.5(6) . . ? C36 C31 P1 118.6(5) . . ? C32 C31 P1 121.3(5) . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 119.6(7) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C35 C34 C33 120.9(7) . . ? C35 C34 H34A 119.6 . . ? C33 C34 H34A 119.6 . . ? C34 C35 C36 119.5(8) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C31 C36 C35 120.2(7) . . ? C31 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C42 C37 C38 118.9(5) . . ? C42 C37 P1 117.2(4) . . ? C38 C37 P1 123.5(4) . . ? C39 C38 C37 120.3(6) . . ? C39 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C40 C39 C38 120.5(6) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C39 C40 C41 119.9(6) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C40 C41 C42 119.8(5) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? C37 C42 C41 120.5(5) . . ? C37 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C44 C43 C48 119.2(5) . . ? C44 C43 P1 119.6(4) . . ? C48 C43 P1 121.2(5) . . ? C43 C44 C45 120.1(6) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C46 C45 C44 119.3(6) . . ? C46 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C47 C46 C45 121.0(6) . . ? C47 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? C46 C47 C48 120.4(6) . . ? C46 C47 H47A 119.8 . . ? C48 C47 H47A 119.8 . . ? C47 C48 C43 120.0(6) . . ? C47 C48 H48A 120.0 . . ? C43 C48 H48A 120.0 . . ? C51 Pd51 Cl52 87.31(13) . . ? C51 Pd51 Cl51 92.72(13) . . ? Cl52 Pd51 Cl51 179.21(6) . . ? C51 Pd51 P51 172.94(14) . . ? Cl52 Pd51 P51 86.54(5) . . ? Cl51 Pd51 P51 93.39(5) . . ? N52 C51 N55 104.8(4) . . ? N52 C51 Pd51 127.5(4) . . ? N55 C51 Pd51 127.3(3) . . ? C51 N52 C53 111.4(4) . . ? C51 N52 C56 126.0(4) . . ? C53 N52 C56 122.6(4) . . ? C54 C53 N52 105.8(4) . . ? C54 C53 H53A 127.1 . . ? N52 C53 H53A 127.1 . . ? C53 C54 N55 107.6(5) . . ? C53 C54 H54A 126.2 . . ? N55 C54 H54A 126.2 . . ? C51 N55 C54 110.4(4) . . ? C51 N55 C68 127.0(4) . . ? C54 N55 C68 122.6(4) . . ? C61 C56 C57 123.5(5) . . ? C61 C56 N52 119.3(5) . . ? C57 C56 N52 117.2(5) . . ? C58 C57 C56 116.8(5) . . ? C58 C57 C65 120.0(5) . . ? C56 C57 C65 123.2(5) . . ? C59 C58 C57 121.7(6) . . ? C59 C58 H58A 119.2 . . ? C57 C58 H58A 119.2 . . ? C60 C59 C58 119.4(6) . . ? C60 C59 H59A 120.3 . . ? C58 C59 H59A 120.3 . . ? C59 C60 C61 122.5(6) . . ? C59 C60 H60A 118.7 . . ? C61 C60 H60A 118.7 . . ? C56 C61 C60 116.1(5) . . ? C56 C61 C62 122.5(5) . . ? C60 C61 C62 121.3(5) . . ? C61 C62 C63 110.1(5) . . ? C61 C62 C64 112.1(5) . . ? C63 C62 C64 110.6(5) . . ? C61 C62 H62A 108.0 . . ? C63 C62 H62A 108.0 . . ? C64 C62 H62A 108.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C57 C65 C67 112.7(5) . . ? C57 C65 C66 109.4(5) . . ? C67 C65 C66 110.7(5) . . ? C57 C65 H65A 108.0 . . ? C67 C65 H65A 108.0 . . ? C66 C65 H65A 108.0 . . ? 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 . . ? C69 C68 C73 122.5(5) . . ? C69 C68 N55 118.8(5) . . ? C73 C68 N55 118.7(5) . . ? C70 C69 C68 117.4(5) . . ? C70 C69 C74 119.8(5) . . ? C68 C69 C74 122.8(5) . . ? C71 C70 C69 121.1(6) . . ? C71 C70 H70A 119.5 . . ? C69 C70 H70A 119.5 . . ? C72 C71 C70 120.6(6) . . ? C72 C71 H71A 119.7 . . ? C70 C71 H71A 119.7 . . ? C71 C72 C73 120.9(6) . . ? C71 C72 H72A 119.5 . . ? C73 C72 H72A 119.5 . . ? C72 C73 C68 117.5(5) . . ? C72 C73 C77 121.3(5) . . ? C68 C73 C77 121.2(5) . . ? C69 C74 C76 112.1(6) . . ? C69 C74 C75 110.6(5) . . ? C76 C74 C75 109.5(5) . . ? C69 C74 H74A 108.2 . . ? C76 C74 H74A 108.2 . . ? C75 C74 H74A 108.2 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C73 C77 C79 112.7(6) . . ? C73 C77 C78 111.5(5) . . ? C79 C77 C78 110.8(6) . . ? C73 C77 H77A 107.1 . . ? C79 C77 H77A 107.1 . . ? C78 C77 H77A 107.1 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C93 P51 C81 105.4(3) . . ? C93 P51 C87 101.9(2) . . ? C81 P51 C87 105.9(2) . . ? C93 P51 Pd51 108.65(17) . . ? C81 P51 Pd51 112.94(17) . . ? C87 P51 Pd51 120.60(18) . . ? C82 C81 C86 118.9(6) . . ? C82 C81 P51 123.4(5) . . ? C86 C81 P51 117.5(5) . . ? C81 C82 C83 120.8(7) . . ? C81 C82 H82A 119.6 . . ? C83 C82 H82A 119.6 . . ? C84 C83 C82 119.6(8) . . ? C84 C83 H83A 120.2 . . ? C82 C83 H83A 120.2 . . ? C83 C84 C85 120.9(7) . . ? C83 C84 H84A 119.5 . . ? C85 C84 H84A 119.5 . . ? C84 C85 C86 120.1(8) . . ? C84 C85 H85A 119.9 . . ? C86 C85 H85A 119.9 . . ? C85 C86 C81 119.6(7) . . ? C85 C86 H86A 120.2 . . ? C81 C86 H86A 120.2 . . ? C88 C87 C92 120.1(5) . . ? C88 C87 P51 122.7(4) . . ? C92 C87 P51 117.2(4) . . ? C87 C88 C89 120.0(5) . . ? C87 C88 H88A 120.0 . . ? C89 C88 H88A 120.0 . . ? C90 C89 C88 120.0(6) . . ? C90 C89 H89A 120.0 . . ? C88 C89 H89A 120.0 . . ? C89 C90 C91 120.7(6) . . ? C89 C90 H90A 119.6 . . ? C91 C90 H90A 119.6 . . ? C90 C91 C92 119.2(6) . . ? C90 C91 H91A 120.4 . . ? C92 C91 H91A 120.4 . . ? C87 C92 C91 119.9(5) . . ? C87 C92 H92A 120.0 . . ? C91 C92 H92A 120.0 . . ? C94 C93 C98 117.9(5) . . ? C94 C93 P51 120.8(4) . . ? C98 C93 P51 121.2(4) . . ? C95 C94 C93 121.4(5) . . ? C95 C94 H94A 119.3 . . ? C93 C94 H94A 119.3 . . ? C94 C95 C96 119.3(6) . . ? C94 C95 H95A 120.4 . . ? C96 C95 H95A 120.4 . . ? C97 C96 C95 120.2(5) . . ? C97 C96 H96A 119.9 . . ? C95 C96 H96A 119.9 . . ? C98 C97 C96 120.4(5) . . ? C98 C97 H97A 119.8 . . ? C96 C97 H97A 119.8 . . ? C97 C98 C93 120.8(5) . . ? C97 C98 H98A 119.6 . . ? C93 C98 H98A 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 C1 N2 106.7(4) . . . . ? Cl2 Pd1 C1 N2 -72.4(4) . . . . ? P1 Pd1 C1 N2 128.0(12) . . . . ? Cl1 Pd1 C1 N5 -63.1(4) . . . . ? Cl2 Pd1 C1 N5 117.8(4) . . . . ? P1 Pd1 C1 N5 -41.8(16) . . . . ? N5 C1 N2 C3 0.9(5) . . . . ? Pd1 C1 N2 C3 -170.7(3) . . . . ? N5 C1 N2 C6 -175.4(4) . . . . ? Pd1 C1 N2 C6 13.0(7) . . . . ? C1 N2 C3 C4 -0.9(6) . . . . ? C6 N2 C3 C4 175.5(5) . . . . ? N2 C3 C4 N5 0.6(6) . . . . ? N2 C1 N5 C4 -0.5(5) . . . . ? Pd1 C1 N5 C4 171.1(3) . . . . ? N2 C1 N5 C18 173.8(4) . . . . ? Pd1 C1 N5 C18 -14.6(7) . . . . ? C3 C4 N5 C1 0.0(6) . . . . ? C3 C4 N5 C18 -174.6(4) . . . . ? C1 N2 C6 C7 94.8(6) . . . . ? C3 N2 C6 C7 -81.0(6) . . . . ? C1 N2 C6 C11 -87.3(6) . . . . ? C3 N2 C6 C11 96.9(6) . . . . ? C11 C6 C7 C8 -0.3(8) . . . . ? N2 C6 C7 C8 177.4(5) . . . . ? C11 C6 C7 C12 179.0(5) . . . . ? N2 C6 C7 C12 -3.3(7) . . . . ? C6 C7 C8 C9 0.8(9) . . . . ? C12 C7 C8 C9 -178.6(6) . . . . ? C7 C8 C9 C10 -0.6(10) . . . . ? C8 C9 C10 C11 0.0(10) . . . . ? C9 C10 C11 C6 0.4(9) . . . . ? C9 C10 C11 C15 -179.7(6) . . . . ? C7 C6 C11 C10 -0.2(8) . . . . ? N2 C6 C11 C10 -177.9(5) . . . . ? C7 C6 C11 C15 179.9(5) . . . . ? N2 C6 C11 C15 2.2(7) . . . . ? C6 C7 C12 C14 -144.6(5) . . . . ? C8 C7 C12 C14 34.8(8) . . . . ? C6 C7 C12 C13 92.2(6) . . . . ? C8 C7 C12 C13 -88.4(7) . . . . ? C10 C11 C15 C17 -29.4(8) . . . . ? C6 C11 C15 C17 150.4(6) . . . . ? C10 C11 C15 C16 95.7(7) . . . . ? C6 C11 C15 C16 -84.4(7) . . . . ? C1 N5 C18 C23 -69.7(6) . . . . ? C4 N5 C18 C23 103.9(6) . . . . ? C1 N5 C18 C19 113.1(5) . . . . ? C4 N5 C18 C19 -73.3(6) . . . . ? C23 C18 C19 C20 0.4(8) . . . . ? N5 C18 C19 C20 177.4(5) . . . . ? C23 C18 C19 C24 -179.5(5) . . . . ? N5 C18 C19 C24 -2.5(7) . . . . ? C18 C19 C20 C21 -0.2(8) . . . . ? C24 C19 C20 C21 179.6(6) . . . . ? C19 C20 C21 C22 0.7(10) . . . . ? C20 C21 C22 C23 -1.4(10) . . . . ? C19 C18 C23 C22 -1.0(8) . . . . ? N5 C18 C23 C22 -178.0(5) . . . . ? C19 C18 C23 C27 177.8(5) . . . . ? N5 C18 C23 C27 0.8(7) . . . . ? C21 C22 C23 C18 1.4(9) . . . . ? C21 C22 C23 C27 -177.3(6) . . . . ? C20 C19 C24 C26 47.8(7) . . . . ? C18 C19 C24 C26 -132.4(5) . . . . ? C20 C19 C24 C25 -74.0(6) . . . . ? C18 C19 C24 C25 105.8(6) . . . . ? C18 C23 C27 C29 149.9(6) . . . . ? C22 C23 C27 C29 -31.4(8) . . . . ? C18 C23 C27 C28 -84.5(7) . . . . ? C22 C23 C27 C28 94.2(7) . . . . ? C1 Pd1 P1 C43 57.4(13) . . . . ? Cl1 Pd1 P1 C43 78.74(19) . . . . ? Cl2 Pd1 P1 C43 -102.19(19) . . . . ? C1 Pd1 P1 C37 174.6(13) . . . . ? Cl1 Pd1 P1 C37 -164.1(2) . . . . ? Cl2 Pd1 P1 C37 15.0(2) . . . . ? C1 Pd1 P1 C31 -60.8(13) . . . . ? Cl1 Pd1 P1 C31 -39.4(2) . . . . ? Cl2 Pd1 P1 C31 139.6(2) . . . . ? C43 P1 C31 C36 180.0(5) . . . . ? C37 P1 C31 C36 70.8(5) . . . . ? Pd1 P1 C31 C36 -59.4(5) . . . . ? C43 P1 C31 C32 -8.9(6) . . . . ? C37 P1 C31 C32 -118.1(5) . . . . ? Pd1 P1 C31 C32 111.7(5) . . . . ? C36 C31 C32 C33 -0.6(10) . . . . ? P1 C31 C32 C33 -171.6(5) . . . . ? C31 C32 C33 C34 -0.5(11) . . . . ? C32 C33 C34 C35 -0.2(13) . . . . ? C33 C34 C35 C36 1.9(13) . . . . ? C32 C31 C36 C35 2.4(10) . . . . ? P1 C31 C36 C35 173.6(6) . . . . ? C34 C35 C36 C31 -3.0(12) . . . . ? C43 P1 C37 C42 52.6(5) . . . . ? C31 P1 C37 C42 164.3(4) . . . . ? Pd1 P1 C37 C42 -68.8(5) . . . . ? C43 P1 C37 C38 -134.0(5) . . . . ? C31 P1 C37 C38 -22.2(6) . . . . ? Pd1 P1 C37 C38 104.7(5) . . . . ? C42 C37 C38 C39 -0.1(9) . . . . ? P1 C37 C38 C39 -173.5(5) . . . . ? C37 C38 C39 C40 -0.2(10) . . . . ? C38 C39 C40 C41 -0.1(10) . . . . ? C39 C40 C41 C42 0.8(9) . . . . ? C38 C37 C42 C41 0.8(8) . . . . ? P1 C37 C42 C41 174.5(4) . . . . ? C40 C41 C42 C37 -1.1(8) . . . . ? C37 P1 C43 C44 -136.2(5) . . . . ? C31 P1 C43 C44 111.4(5) . . . . ? Pd1 P1 C43 C44 -10.2(5) . . . . ? C37 P1 C43 C48 42.6(5) . . . . ? C31 P1 C43 C48 -69.8(5) . . . . ? Pd1 P1 C43 C48 168.6(4) . . . . ? C48 C43 C44 C45 -0.8(9) . . . . ? P1 C43 C44 C45 178.0(5) . . . . ? C43 C44 C45 C46 0.9(10) . . . . ? C44 C45 C46 C47 0.1(10) . . . . ? C45 C46 C47 C48 -1.3(11) . . . . ? C46 C47 C48 C43 1.3(10) . . . . ? C44 C43 C48 C47 -0.3(9) . . . . ? P1 C43 C48 C47 -179.1(5) . . . . ? Cl52 Pd51 C51 N52 107.5(4) . . . . ? Cl51 Pd51 C51 N52 -73.3(4) . . . . ? P51 Pd51 C51 N52 136.9(9) . . . . ? Cl52 Pd51 C51 N55 -63.9(4) . . . . ? Cl51 Pd51 C51 N55 115.3(4) . . . . ? P51 Pd51 C51 N55 -34.5(14) . . . . ? N55 C51 N52 C53 0.5(6) . . . . ? Pd51 C51 N52 C53 -172.4(4) . . . . ? N55 C51 N52 C56 178.3(5) . . . . ? Pd51 C51 N52 C56 5.3(7) . . . . ? C51 N52 C53 C54 -0.2(7) . . . . ? C56 N52 C53 C54 -178.0(5) . . . . ? N52 C53 C54 N55 -0.2(7) . . . . ? N52 C51 N55 C54 -0.6(6) . . . . ? Pd51 C51 N55 C54 172.3(4) . . . . ? N52 C51 N55 C68 -179.6(5) . . . . ? Pd51 C51 N55 C68 -6.7(7) . . . . ? C53 C54 N55 C51 0.5(7) . . . . ? C53 C54 N55 C68 179.6(5) . . . . ? C51 N52 C56 C61 97.4(6) . . . . ? C53 N52 C56 C61 -85.1(7) . . . . ? C51 N52 C56 C57 -85.9(6) . . . . ? C53 N52 C56 C57 91.6(7) . . . . ? C61 C56 C57 C58 0.2(9) . . . . ? N52 C56 C57 C58 -176.4(5) . . . . ? C61 C56 C57 C65 177.5(5) . . . . ? N52 C56 C57 C65 0.9(8) . . . . ? C56 C57 C58 C59 0.7(9) . . . . ? C65 C57 C58 C59 -176.6(6) . . . . ? C57 C58 C59 C60 -0.1(10) . . . . ? C58 C59 C60 C61 -1.6(10) . . . . ? C57 C56 C61 C60 -1.7(8) . . . . ? N52 C56 C61 C60 174.8(5) . . . . ? C57 C56 C61 C62 -179.3(5) . . . . ? N52 C56 C61 C62 -2.8(8) . . . . ? C59 C60 C61 C56 2.5(9) . . . . ? C59 C60 C61 C62 -180.0(6) . . . . ? C56 C61 C62 C63 91.2(7) . . . . ? C60 C61 C62 C63 -86.2(7) . . . . ? C56 C61 C62 C64 -145.3(5) . . . . ? C60 C61 C62 C64 37.3(8) . . . . ? C58 C57 C65 C67 -51.5(8) . . . . ? C56 C57 C65 C67 131.3(6) . . . . ? C58 C57 C65 C66 72.0(7) . . . . ? C56 C57 C65 C66 -105.1(6) . . . . ? C51 N55 C68 C69 107.5(6) . . . . ? C54 N55 C68 C69 -71.4(7) . . . . ? C51 N55 C68 C73 -74.3(7) . . . . ? C54 N55 C68 C73 106.8(6) . . . . ? C73 C68 C69 C70 -1.4(8) . . . . ? N55 C68 C69 C70 176.8(5) . . . . ? C73 C68 C69 C74 -179.1(5) . . . . ? N55 C68 C69 C74 -1.0(7) . . . . ? C68 C69 C70 C71 0.3(9) . . . . ? C74 C69 C70 C71 178.1(5) . . . . ? C69 C70 C71 C72 1.5(10) . . . . ? C70 C71 C72 C73 -2.3(10) . . . . ? C71 C72 C73 C68 1.2(8) . . . . ? C71 C72 C73 C77 -178.8(6) . . . . ? C69 C68 C73 C72 0.7(8) . . . . ? N55 C68 C73 C72 -177.5(5) . . . . ? C69 C68 C73 C77 -179.4(5) . . . . ? N55 C68 C73 C77 2.4(7) . . . . ? C70 C69 C74 C76 45.7(7) . . . . ? C68 C69 C74 C76 -136.6(5) . . . . ? C70 C69 C74 C75 -76.8(7) . . . . ? C68 C69 C74 C75 100.9(6) . . . . ? C72 C73 C77 C79 -19.6(8) . . . . ? C68 C73 C77 C79 160.5(5) . . . . ? C72 C73 C77 C78 105.8(7) . . . . ? C68 C73 C77 C78 -74.1(7) . . . . ? C51 Pd51 P51 C93 49.7(11) . . . . ? Cl52 Pd51 P51 C93 79.15(17) . . . . ? Cl51 Pd51 P51 C93 -100.06(17) . . . . ? C51 Pd51 P51 C81 -66.9(11) . . . . ? Cl52 Pd51 P51 C81 -37.5(2) . . . . ? Cl51 Pd51 P51 C81 143.3(2) . . . . ? C51 Pd51 P51 C87 166.6(11) . . . . ? Cl52 Pd51 P51 C87 -164.0(2) . . . . ? Cl51 Pd51 P51 C87 16.8(2) . . . . ? C93 P51 C81 C82 -5.9(5) . . . . ? C87 P51 C81 C82 -113.4(5) . . . . ? Pd51 P51 C81 C82 112.6(5) . . . . ? C93 P51 C81 C86 179.6(4) . . . . ? C87 P51 C81 C86 72.2(5) . . . . ? Pd51 P51 C81 C86 -61.9(5) . . . . ? C86 C81 C82 C83 -0.2(9) . . . . ? P51 C81 C82 C83 -174.6(5) . . . . ? C81 C82 C83 C84 0.8(10) . . . . ? C82 C83 C84 C85 -0.9(11) . . . . ? C83 C84 C85 C86 0.4(11) . . . . ? C84 C85 C86 C81 0.2(10) . . . . ? C82 C81 C86 C85 -0.3(9) . . . . ? P51 C81 C86 C85 174.4(5) . . . . ? C93 P51 C87 C88 -125.8(5) . . . . ? C81 P51 C87 C88 -15.8(5) . . . . ? Pd51 P51 C87 C88 113.9(5) . . . . ? C93 P51 C87 C92 54.0(5) . . . . ? C81 P51 C87 C92 164.1(4) . . . . ? Pd51 P51 C87 C92 -66.2(5) . . . . ? C92 C87 C88 C89 -1.3(9) . . . . ? P51 C87 C88 C89 178.6(5) . . . . ? C87 C88 C89 C90 0.2(10) . . . . ? C88 C89 C90 C91 0.3(10) . . . . ? C89 C90 C91 C92 0.2(10) . . . . ? C88 C87 C92 C91 1.8(8) . . . . ? P51 C87 C92 C91 -178.1(4) . . . . ? C90 C91 C92 C87 -1.2(9) . . . . ? C81 P51 C93 C94 110.0(5) . . . . ? C87 P51 C93 C94 -139.7(5) . . . . ? Pd51 P51 C93 C94 -11.4(5) . . . . ? C81 P51 C93 C98 -71.3(5) . . . . ? C87 P51 C93 C98 39.1(5) . . . . ? Pd51 P51 C93 C98 167.4(4) . . . . ? C98 C93 C94 C95 0.7(9) . . . . ? P51 C93 C94 C95 179.4(5) . . . . ? C93 C94 C95 C96 -0.5(11) . . . . ? C94 C95 C96 C97 0.2(11) . . . . ? C95 C96 C97 C98 0.0(10) . . . . ? C96 C97 C98 C93 0.2(9) . . . . ? C94 C93 C98 C97 -0.5(8) . . . . ? P51 C93 C98 C97 -179.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.431 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.088 data_2b _database_code_depnum_ccdc_archive 'CCDC 871883' #TrackingRef '10171_web_deposit_cif_file_1_CatherineS.J.Cazin_1331897901.2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H69 Cl2 N2 P Pd' _chemical_formula_sum 'C45 H69 Cl2 N2 P Pd' _chemical_formula_weight 846.29 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' 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.687(2) _cell_length_b 14.147(3) _cell_length_c 15.029(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.572(6) _cell_angle_gamma 90.00 _cell_volume 2261.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8380 _cell_measurement_theta_min 2.2391 _cell_measurement_theta_max 28.6268 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1200 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7527 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14317 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.33 _reflns_number_total 7509 _reflns_number_gt 6636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0323P] 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 -0.02(3) _refine_ls_number_reflns 7509 _refine_ls_number_parameters 460 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.52965(3) 0.39413(2) 0.743059(19) 0.02070(11) Uani 1 1 d . . . Cl1 Cl 0.48492(14) 0.49800(9) 0.62597(8) 0.0331(3) Uani 1 1 d . . . Cl2 Cl 0.57013(13) 0.28500(9) 0.85687(7) 0.0294(3) Uani 1 1 d . . . C1 C 0.5779(4) 0.2958(3) 0.6537(3) 0.0205(10) Uani 1 1 d . . . N2 N 0.5020(4) 0.2403(3) 0.5974(2) 0.0230(9) Uani 1 1 d . . . C3 C 0.5734(5) 0.1833(3) 0.5470(3) 0.0271(11) Uani 1 1 d . . . H3A H 0.5419 0.1394 0.5026 0.032 Uiso 1 1 calc R . . C4 C 0.6945(5) 0.2012(4) 0.5720(3) 0.0302(12) Uani 1 1 d . . . H4A H 0.7651 0.1724 0.5492 0.036 Uiso 1 1 calc R . . N5 N 0.6967(4) 0.2701(3) 0.6379(2) 0.0237(9) Uani 1 1 d . . . C6 C 0.3674(4) 0.2387(3) 0.5906(3) 0.0219(10) Uani 1 1 d . . . C7 C 0.3085(5) 0.1836(3) 0.6516(3) 0.0238(11) Uani 1 1 d . . . C8 C 0.1770(5) 0.1791(4) 0.6419(3) 0.0304(12) Uani 1 1 d . . . H8A H 0.1348 0.1425 0.6828 0.036 Uiso 1 1 calc R . . C9 C 0.1079(5) 0.2267(4) 0.5741(3) 0.0297(12) Uani 1 1 d . . . H9A H 0.0187 0.2231 0.5687 0.036 Uiso 1 1 calc R . . C10 C 0.1673(5) 0.2792(4) 0.5145(3) 0.0295(11) Uani 1 1 d . . . H10A H 0.1183 0.3117 0.4681 0.035 Uiso 1 1 calc R . . C11 C 0.2972(4) 0.2863(4) 0.5199(3) 0.0249(10) Uani 1 1 d . . . C12 C 0.3852(5) 0.1242(4) 0.7227(3) 0.0354(13) Uani 1 1 d . . . H12A H 0.4682 0.1558 0.7376 0.042 Uiso 1 1 calc R . . C13 C 0.4090(7) 0.0263(4) 0.6856(4) 0.0579(18) Uani 1 1 d . . . H13A H 0.4529 0.0324 0.6316 0.087 Uiso 1 1 calc R . . H13B H 0.3286 -0.0061 0.6709 0.087 Uiso 1 1 calc R . . H13C H 0.4609 -0.0104 0.7305 0.087 Uiso 1 1 calc R . . C14 C 0.3197(6) 0.1159(6) 0.8090(4) 0.063(2) Uani 1 1 d . . . H14A H 0.3716 0.0778 0.8527 0.094 Uiso 1 1 calc R . . H14B H 0.2375 0.0856 0.7957 0.094 Uiso 1 1 calc R . . H14C H 0.3081 0.1792 0.8335 0.094 Uiso 1 1 calc R . . C15 C 0.3610(5) 0.3416(4) 0.4500(3) 0.0321(12) Uani 1 1 d . . . H15A H 0.4491 0.3563 0.4749 0.038 Uiso 1 1 calc R . . C16 C 0.3658(6) 0.2836(4) 0.3654(3) 0.0421(14) Uani 1 1 d . . . H16A H 0.4112 0.2245 0.3797 0.063 Uiso 1 1 calc R . . H16B H 0.4092 0.3197 0.3220 0.063 Uiso 1 1 calc R . . H16C H 0.2800 0.2692 0.3399 0.063 Uiso 1 1 calc R . . C17 C 0.2924(6) 0.4352(4) 0.4268(4) 0.0451(15) Uani 1 1 d . . . H17A H 0.2911 0.4735 0.4810 0.068 Uiso 1 1 calc R . . H17B H 0.2059 0.4219 0.4020 0.068 Uiso 1 1 calc R . . H17C H 0.3363 0.4697 0.3826 0.068 Uiso 1 1 calc R . . C18 C 0.8145(4) 0.3113(3) 0.6775(3) 0.0196(10) Uani 1 1 d . . . C19 C 0.8801(5) 0.2664(3) 0.7493(3) 0.0245(11) Uani 1 1 d . . . C20 C 0.9974(5) 0.3043(4) 0.7803(3) 0.0292(12) Uani 1 1 d . . . H20A H 1.0458 0.2751 0.8292 0.035 Uiso 1 1 calc R . . C21 C 1.0437(4) 0.3835(5) 0.7408(3) 0.0289(12) Uani 1 1 d . . . H21A H 1.1228 0.4089 0.7631 0.035 Uiso 1 1 calc R . . C22 C 0.9749(5) 0.4258(3) 0.6685(3) 0.0279(11) Uani 1 1 d . . . H22A H 1.0083 0.4796 0.6413 0.033 Uiso 1 1 calc R . . C23 C 0.8587(4) 0.3913(4) 0.6353(3) 0.0244(9) Uani 1 1 d . . . C24 C 0.8356(5) 0.1766(4) 0.7919(3) 0.0295(11) Uani 1 1 d . . . H24A H 0.7426 0.1716 0.7769 0.035 Uiso 1 1 calc R . . C25 C 0.8960(6) 0.0895(4) 0.7550(4) 0.0389(14) Uani 1 1 d . . . H25A H 0.8789 0.0885 0.6897 0.058 Uiso 1 1 calc R . . H25B H 0.8609 0.0325 0.7802 0.058 Uiso 1 1 calc R . . H25C H 0.9870 0.0913 0.7712 0.058 Uiso 1 1 calc R . . C26 C 0.8617(6) 0.1790(5) 0.8946(4) 0.0422(15) Uani 1 1 d . . . H26A H 0.8314 0.1204 0.9198 0.063 Uiso 1 1 calc R . . H26B H 0.8181 0.2331 0.9182 0.063 Uiso 1 1 calc R . . H26C H 0.9524 0.1851 0.9111 0.063 Uiso 1 1 calc R . . C27 C 0.7894(5) 0.4357(4) 0.5523(3) 0.0319(12) Uani 1 1 d . . . H27A H 0.7011 0.4116 0.5447 0.038 Uiso 1 1 calc R . . C28 C 0.8570(6) 0.4074(6) 0.4708(3) 0.0567(19) Uani 1 1 d . . . H28A H 0.8577 0.3384 0.4655 0.085 Uiso 1 1 calc R . . H28B H 0.9436 0.4310 0.4782 0.085 Uiso 1 1 calc R . . H28C H 0.8128 0.4348 0.4166 0.085 Uiso 1 1 calc R . . C29 C 0.7878(6) 0.5437(4) 0.5605(4) 0.0415(14) Uani 1 1 d . . . H29A H 0.7433 0.5618 0.6119 0.062 Uiso 1 1 calc R . . H29B H 0.7448 0.5710 0.5059 0.062 Uiso 1 1 calc R . . H29C H 0.8743 0.5674 0.5689 0.062 Uiso 1 1 calc R . . P1 P 0.49362(13) 0.50914(9) 0.84899(8) 0.0240(3) Uani 1 1 d . . . C31 C 0.4056(5) 0.6139(3) 0.8044(3) 0.0276(11) Uani 1 1 d . . . H31A H 0.4471 0.6331 0.7503 0.033 Uiso 1 1 calc R . . C32 C 0.4079(6) 0.7026(4) 0.8632(4) 0.0403(14) Uani 1 1 d . . . H32A H 0.3649 0.6892 0.9173 0.048 Uiso 1 1 calc R . . H32B H 0.4961 0.7199 0.8826 0.048 Uiso 1 1 calc R . . C33 C 0.3422(6) 0.7858(4) 0.8118(4) 0.0462(15) Uani 1 1 d . . . H33A H 0.3406 0.8411 0.8521 0.055 Uiso 1 1 calc R . . H33B H 0.3906 0.8036 0.7614 0.055 Uiso 1 1 calc R . . C34 C 0.2097(6) 0.7606(4) 0.7762(4) 0.0499(16) Uani 1 1 d . . . H34A H 0.1718 0.8142 0.7409 0.060 Uiso 1 1 calc R . . H34B H 0.1589 0.7496 0.8270 0.060 Uiso 1 1 calc R . . C35 C 0.2058(6) 0.6720(4) 0.7174(4) 0.0460(15) Uani 1 1 d . . . H35A H 0.2492 0.6848 0.6634 0.055 Uiso 1 1 calc R . . H35B H 0.1173 0.6555 0.6979 0.055 Uiso 1 1 calc R . . C36 C 0.2697(5) 0.5892(4) 0.7693(4) 0.0349(12) Uani 1 1 d . . . H36A H 0.2216 0.5729 0.8202 0.042 Uiso 1 1 calc R . . H36B H 0.2698 0.5333 0.7297 0.042 Uiso 1 1 calc R . . C37 C 0.4229(5) 0.4581(3) 0.9447(3) 0.0253(11) Uani 1 1 d . . . H37A H 0.4862 0.4118 0.9719 0.030 Uiso 1 1 calc R . . C38 C 0.3968(5) 0.5256(4) 1.0212(3) 0.0324(12) Uani 1 1 d . . . H38A H 0.4724 0.5645 1.0383 0.039 Uiso 1 1 calc R . . H38B H 0.3269 0.5687 1.0008 0.039 Uiso 1 1 calc R . . C39 C 0.3624(5) 0.4686(4) 1.1022(3) 0.0366(14) Uani 1 1 d . . . H39A H 0.3426 0.5126 1.1501 0.044 Uiso 1 1 calc R . . H39B H 0.4354 0.4298 1.1255 0.044 Uiso 1 1 calc R . . C40 C 0.2490(5) 0.4039(5) 1.0775(3) 0.0389(13) Uani 1 1 d . . . H40A H 0.2350 0.3636 1.1294 0.047 Uiso 1 1 calc R . . H40B H 0.1730 0.4432 1.0634 0.047 Uiso 1 1 calc R . . C41 C 0.2688(6) 0.3417(4) 0.9978(3) 0.0358(13) Uani 1 1 d . . . H41A H 0.3370 0.2959 1.0150 0.043 Uiso 1 1 calc R . . H41B H 0.1910 0.3055 0.9806 0.043 Uiso 1 1 calc R . . C42 C 0.3028(4) 0.3992(5) 0.9180(3) 0.0299(10) Uani 1 1 d . . . H42A H 0.2324 0.4419 0.8976 0.036 Uiso 1 1 calc R . . H42B H 0.3176 0.3562 0.8681 0.036 Uiso 1 1 calc R . . C43 C 0.6484(5) 0.5569(4) 0.8959(3) 0.0286(11) Uani 1 1 d . . . H43A H 0.6324 0.6131 0.9335 0.034 Uiso 1 1 calc R . . C44 C 0.7269(5) 0.4860(4) 0.9546(4) 0.0403(14) Uani 1 1 d . . . H44A H 0.6812 0.4685 1.0065 0.048 Uiso 1 1 calc R . . H44B H 0.7394 0.4280 0.9198 0.048 Uiso 1 1 calc R . . C45 C 0.8538(5) 0.5279(5) 0.9876(4) 0.0449(15) Uani 1 1 d . . . H45A H 0.9040 0.4799 1.0233 0.054 Uiso 1 1 calc R . . H45B H 0.8411 0.5823 1.0271 0.054 Uiso 1 1 calc R . . C46 C 0.9263(6) 0.5605(5) 0.9100(4) 0.0452(15) Uani 1 1 d . . . H46A H 1.0066 0.5900 0.9340 0.054 Uiso 1 1 calc R . . H46B H 0.9461 0.5051 0.8736 0.054 Uiso 1 1 calc R . . C47 C 0.8501(6) 0.6303(5) 0.8525(4) 0.0457(17) Uani 1 1 d . . . H47A H 0.8961 0.6475 0.8007 0.055 Uiso 1 1 calc R . . H47B H 0.8385 0.6885 0.8873 0.055 Uiso 1 1 calc R . . C48 C 0.7220(5) 0.5903(5) 0.8190(4) 0.0427(14) Uani 1 1 d . . . H48A H 0.7335 0.5364 0.7786 0.051 Uiso 1 1 calc R . . H48B H 0.6728 0.6394 0.7842 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0217(2) 0.02048(18) 0.01990(17) -0.00282(15) 0.00167(13) 0.00038(16) Cl1 0.0475(9) 0.0251(6) 0.0271(6) 0.0035(5) 0.0055(6) 0.0059(6) Cl2 0.0348(8) 0.0299(7) 0.0233(6) -0.0009(5) 0.0013(5) 0.0064(6) C1 0.018(3) 0.019(2) 0.024(2) 0.007(2) 0.0016(19) -0.003(2) N2 0.018(2) 0.029(2) 0.023(2) 0.0041(17) 0.0031(16) 0.0027(18) C3 0.034(3) 0.024(3) 0.024(2) -0.009(2) 0.004(2) 0.006(2) C4 0.024(3) 0.028(3) 0.039(3) -0.013(2) 0.005(2) 0.001(2) N5 0.020(2) 0.018(2) 0.033(2) -0.0035(17) 0.0019(17) 0.0017(17) C6 0.020(3) 0.020(2) 0.025(2) -0.012(2) -0.0001(19) -0.002(2) C7 0.032(3) 0.023(2) 0.016(2) -0.0066(19) 0.001(2) -0.008(2) C8 0.028(3) 0.035(3) 0.029(3) 0.004(2) 0.005(2) -0.003(2) C9 0.024(3) 0.037(3) 0.030(3) -0.010(2) 0.010(2) -0.004(2) C10 0.022(3) 0.031(3) 0.033(3) -0.001(2) -0.007(2) 0.001(2) C11 0.021(3) 0.025(2) 0.029(2) 0.001(2) 0.002(2) 0.004(2) C12 0.030(3) 0.045(3) 0.030(3) 0.006(2) -0.004(2) -0.013(3) C13 0.058(4) 0.045(4) 0.065(4) 0.021(3) -0.025(3) 0.009(3) C14 0.041(4) 0.108(6) 0.037(3) 0.018(4) -0.006(3) -0.027(4) C15 0.032(3) 0.032(3) 0.031(3) 0.005(2) 0.002(2) -0.002(2) C16 0.052(4) 0.043(3) 0.032(3) 0.000(3) 0.011(3) -0.011(3) C17 0.044(4) 0.027(3) 0.063(4) 0.021(3) 0.001(3) 0.002(3) C18 0.021(3) 0.019(2) 0.019(2) -0.0017(18) 0.0006(18) -0.0011(19) C19 0.025(3) 0.020(2) 0.030(3) -0.003(2) 0.010(2) -0.004(2) C20 0.030(3) 0.030(3) 0.027(2) 0.001(2) 0.000(2) -0.004(2) C21 0.028(3) 0.027(3) 0.029(2) 0.003(2) -0.0077(19) -0.010(2) C22 0.032(3) 0.024(3) 0.027(2) -0.0011(19) 0.000(2) -0.009(2) C23 0.026(2) 0.020(2) 0.027(2) -0.003(2) -0.0001(17) -0.003(3) C24 0.022(3) 0.035(3) 0.033(3) -0.001(2) 0.005(2) -0.005(2) C25 0.043(4) 0.025(3) 0.051(3) 0.012(3) 0.014(3) 0.005(3) C26 0.031(3) 0.061(4) 0.035(3) 0.008(3) 0.006(3) 0.001(3) C27 0.029(3) 0.036(3) 0.032(3) 0.005(2) 0.006(2) 0.004(2) C28 0.067(4) 0.079(5) 0.023(2) 0.014(3) 0.000(2) 0.038(4) C29 0.046(4) 0.034(3) 0.045(3) 0.006(3) 0.003(3) 0.004(3) P1 0.0241(7) 0.0235(7) 0.0245(6) -0.0090(5) 0.0028(5) -0.0005(6) C31 0.024(3) 0.021(3) 0.037(3) 0.003(2) 0.000(2) 0.004(2) C32 0.036(3) 0.031(3) 0.054(3) -0.014(3) 0.004(3) 0.006(3) C33 0.054(4) 0.022(3) 0.065(4) -0.003(3) 0.015(3) 0.004(3) C34 0.039(4) 0.035(3) 0.076(4) 0.011(3) 0.007(3) 0.009(3) C35 0.034(4) 0.038(3) 0.064(4) 0.014(3) -0.007(3) 0.005(3) C36 0.029(3) 0.030(3) 0.045(3) -0.001(2) 0.002(2) 0.004(2) C37 0.024(3) 0.028(3) 0.023(2) -0.007(2) 0.0013(19) -0.002(2) C38 0.033(3) 0.033(3) 0.032(3) -0.018(2) 0.007(2) -0.004(2) C39 0.032(3) 0.057(4) 0.021(2) 0.004(2) 0.001(2) 0.006(3) C40 0.039(3) 0.053(4) 0.025(2) 0.011(3) 0.002(2) 0.001(3) C41 0.038(3) 0.037(3) 0.032(3) 0.001(2) 0.005(2) -0.003(3) C42 0.026(2) 0.036(3) 0.028(2) -0.010(3) 0.0009(18) -0.005(3) C43 0.025(3) 0.035(3) 0.027(3) -0.007(2) 0.003(2) -0.003(2) C44 0.033(3) 0.047(4) 0.040(3) -0.010(3) 0.001(2) -0.008(3) C45 0.032(3) 0.059(4) 0.041(3) -0.008(3) -0.007(2) -0.012(3) C46 0.026(3) 0.062(4) 0.048(3) -0.021(3) 0.004(3) -0.007(3) C47 0.030(3) 0.058(4) 0.052(4) -0.011(3) 0.018(3) -0.019(3) C48 0.028(3) 0.055(4) 0.045(3) -0.003(3) 0.005(2) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.034(5) . ? Pd1 Cl1 2.3067(13) . ? Pd1 Cl2 2.3136(13) . ? Pd1 P1 2.3344(12) . ? C1 N5 1.364(6) . ? C1 N2 1.363(6) . ? N2 C3 1.385(6) . ? N2 C6 1.433(6) . ? C3 C4 1.336(7) . ? C3 H3A 0.9500 . ? C4 N5 1.388(6) . ? C4 H4A 0.9500 . ? N5 C18 1.461(6) . ? C6 C7 1.398(6) . ? C6 C11 1.410(6) . ? C7 C8 1.400(7) . ? C7 C12 1.534(7) . ? C8 C9 1.374(7) . ? C8 H8A 0.9500 . ? C9 C10 1.366(7) . ? C9 H9A 0.9500 . ? C10 C11 1.386(7) . ? C10 H10A 0.9500 . ? C11 C15 1.523(7) . ? C12 C13 1.523(8) . ? C12 C14 1.536(7) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.519(7) . ? C15 C17 1.536(7) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.383(6) . ? C18 C23 1.402(7) . ? C19 C20 1.401(7) . ? C19 C24 1.520(7) . ? C20 C21 1.382(8) . ? C20 H20A 0.9500 . ? C21 C22 1.387(7) . ? C21 H21A 0.9500 . ? C22 C23 1.382(6) . ? C22 H22A 0.9500 . ? C23 C27 1.523(6) . ? C24 C25 1.520(7) . ? C24 C26 1.541(7) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.535(7) . ? C27 C29 1.533(7) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C37 1.837(5) . ? P1 C31 1.846(5) . ? P1 C43 1.861(5) . ? C31 C36 1.536(7) . ? C31 C32 1.534(7) . ? C31 H31A 1.0000 . ? C32 C33 1.540(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.507(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.532(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.531(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.541(6) . ? C37 C42 1.550(7) . ? C37 H37A 1.0000 . ? C38 C39 1.536(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.535(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.518(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.522(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.531(7) . ? C43 C48 1.535(7) . ? C43 H43A 1.0000 . ? C44 C45 1.518(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.533(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.500(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.521(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl1 88.79(13) . . ? C1 Pd1 Cl2 89.47(13) . . ? Cl1 Pd1 Cl2 177.58(5) . . ? C1 Pd1 P1 174.84(14) . . ? Cl1 Pd1 P1 92.32(5) . . ? Cl2 Pd1 P1 89.56(4) . . ? N5 C1 N2 104.2(4) . . ? N5 C1 Pd1 126.7(3) . . ? N2 C1 Pd1 129.1(3) . . ? C1 N2 C3 110.4(4) . . ? C1 N2 C6 125.9(4) . . ? C3 N2 C6 123.7(4) . . ? C4 C3 N2 107.9(4) . . ? C4 C3 H3A 126.1 . . ? N2 C3 H3A 126.1 . . ? C3 C4 N5 106.4(4) . . ? C3 C4 H4A 126.8 . . ? N5 C4 H4A 126.8 . . ? C1 N5 C4 111.1(4) . . ? C1 N5 C18 127.0(4) . . ? C4 N5 C18 121.7(4) . . ? C7 C6 C11 121.3(4) . . ? C7 C6 N2 118.4(4) . . ? C11 C6 N2 120.2(4) . . ? C8 C7 C6 117.9(4) . . ? C8 C7 C12 120.7(4) . . ? C6 C7 C12 121.2(4) . . ? C7 C8 C9 121.0(5) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 121.8(5) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C6 117.8(4) . . ? C10 C11 C15 120.6(4) . . ? C6 C11 C15 121.6(4) . . ? C13 C12 C7 109.9(4) . . ? C13 C12 C14 110.3(5) . . ? C7 C12 C14 111.9(5) . . ? C13 C12 H12A 108.2 . . ? C7 C12 H12A 108.2 . . ? C14 C12 H12A 108.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 110.7(4) . . ? C11 C15 C17 111.3(5) . . ? C16 C15 C17 109.2(5) . . ? C11 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? C17 C15 H15A 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.8(4) . . ? C19 C18 N5 119.1(4) . . ? C23 C18 N5 116.9(4) . . ? C20 C19 C18 116.9(4) . . ? C20 C19 C24 119.1(4) . . ? C18 C19 C24 123.9(4) . . ? C19 C20 C21 120.9(5) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 121.4(5) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C18 116.9(4) . . ? C22 C23 C27 119.9(5) . . ? C18 C23 C27 123.1(4) . . ? C25 C24 C19 111.2(4) . . ? C25 C24 C26 110.0(5) . . ? C19 C24 C26 111.7(4) . . ? C25 C24 H24A 107.9 . . ? C19 C24 H24A 107.9 . . ? C26 C24 H24A 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 108.5(4) . . ? C23 C27 C29 110.7(4) . . ? C28 C27 C29 109.5(5) . . ? C23 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C29 C27 H27A 109.4 . . ? 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 . . ? C37 P1 C31 111.5(2) . . ? C37 P1 C43 105.3(2) . . ? C31 P1 C43 104.4(2) . . ? C37 P1 Pd1 111.56(16) . . ? C31 P1 Pd1 115.07(16) . . ? C43 P1 Pd1 108.19(17) . . ? C36 C31 C32 110.2(4) . . ? C36 C31 P1 112.0(3) . . ? C32 C31 P1 117.9(4) . . ? C36 C31 H31A 105.2 . . ? C32 C31 H31A 105.2 . . ? P1 C31 H31A 105.2 . . ? C33 C32 C31 110.8(4) . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 111.4(5) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.7(5) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 110.3(5) . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C31 C36 C35 111.2(4) . . ? C31 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? C31 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C42 108.8(4) . . ? C38 C37 P1 117.2(3) . . ? C42 C37 P1 113.7(3) . . ? C38 C37 H37A 105.3 . . ? C42 C37 H37A 105.3 . . ? P1 C37 H37A 105.3 . . ? C39 C38 C37 109.9(4) . . ? C39 C38 H38A 109.7 . . ? C37 C38 H38A 109.7 . . ? C39 C38 H38B 109.7 . . ? C37 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C38 C39 C40 111.4(4) . . ? C38 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? C38 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C39 111.7(4) . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C42 C41 C40 112.0(5) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 C37 109.8(4) . . ? C41 C42 H42A 109.7 . . ? C37 C42 H42A 109.7 . . ? C41 C42 H42B 109.7 . . ? C37 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C48 110.1(5) . . ? C44 C43 P1 113.5(4) . . ? C48 C43 P1 109.1(3) . . ? C44 C43 H43A 108.0 . . ? C48 C43 H43A 108.0 . . ? P1 C43 H43A 108.0 . . ? C45 C44 C43 110.8(5) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C44 C45 C46 111.7(4) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 107.9 . . ? C47 C46 C45 110.5(5) . . ? C47 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? C46 C47 C48 111.5(5) . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? C47 C48 C43 112.1(4) . . ? C47 C48 H48A 109.2 . . ? C43 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C43 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 C1 N5 102.8(4) . . . . ? Cl2 Pd1 C1 N5 -78.9(4) . . . . ? P1 Pd1 C1 N5 0.3(17) . . . . ? Cl1 Pd1 C1 N2 -78.1(4) . . . . ? Cl2 Pd1 C1 N2 100.2(4) . . . . ? P1 Pd1 C1 N2 179(43) . . . . ? N5 C1 N2 C3 -1.2(5) . . . . ? Pd1 C1 N2 C3 179.5(3) . . . . ? N5 C1 N2 C6 178.0(4) . . . . ? Pd1 C1 N2 C6 -1.3(7) . . . . ? C1 N2 C3 C4 1.0(6) . . . . ? C6 N2 C3 C4 -178.2(4) . . . . ? N2 C3 C4 N5 -0.3(5) . . . . ? N2 C1 N5 C4 1.0(5) . . . . ? Pd1 C1 N5 C4 -179.7(3) . . . . ? N2 C1 N5 C18 176.7(4) . . . . ? Pd1 C1 N5 C18 -4.0(6) . . . . ? C3 C4 N5 C1 -0.4(5) . . . . ? C3 C4 N5 C18 -176.4(4) . . . . ? C1 N2 C6 C7 -83.0(6) . . . . ? C3 N2 C6 C7 96.1(5) . . . . ? C1 N2 C6 C11 101.4(5) . . . . ? C3 N2 C6 C11 -79.5(6) . . . . ? C11 C6 C7 C8 -1.6(7) . . . . ? N2 C6 C7 C8 -177.2(4) . . . . ? C11 C6 C7 C12 173.9(4) . . . . ? N2 C6 C7 C12 -1.6(7) . . . . ? C6 C7 C8 C9 0.4(7) . . . . ? C12 C7 C8 C9 -175.2(4) . . . . ? C7 C8 C9 C10 0.4(8) . . . . ? C8 C9 C10 C11 0.0(8) . . . . ? C9 C10 C11 C6 -1.2(7) . . . . ? C9 C10 C11 C15 177.2(5) . . . . ? C7 C6 C11 C10 2.0(7) . . . . ? N2 C6 C11 C10 177.4(4) . . . . ? C7 C6 C11 C15 -176.3(4) . . . . ? N2 C6 C11 C15 -0.9(7) . . . . ? C8 C7 C12 C13 86.3(6) . . . . ? C6 C7 C12 C13 -89.1(6) . . . . ? C8 C7 C12 C14 -36.5(7) . . . . ? C6 C7 C12 C14 148.0(5) . . . . ? C10 C11 C15 C16 -79.0(6) . . . . ? C6 C11 C15 C16 99.3(6) . . . . ? C10 C11 C15 C17 42.7(7) . . . . ? C6 C11 C15 C17 -139.0(5) . . . . ? C1 N5 C18 C19 98.6(5) . . . . ? C4 N5 C18 C19 -86.2(5) . . . . ? C1 N5 C18 C23 -86.0(6) . . . . ? C4 N5 C18 C23 89.2(5) . . . . ? C23 C18 C19 C20 -0.1(7) . . . . ? N5 C18 C19 C20 174.9(4) . . . . ? C23 C18 C19 C24 -176.5(4) . . . . ? N5 C18 C19 C24 -1.5(7) . . . . ? C18 C19 C20 C21 0.6(7) . . . . ? C24 C19 C20 C21 177.2(4) . . . . ? C19 C20 C21 C22 -1.0(8) . . . . ? C20 C21 C22 C23 1.0(8) . . . . ? C21 C22 C23 C18 -0.6(7) . . . . ? C21 C22 C23 C27 -176.2(5) . . . . ? C19 C18 C23 C22 0.1(7) . . . . ? N5 C18 C23 C22 -175.0(4) . . . . ? C19 C18 C23 C27 175.6(4) . . . . ? N5 C18 C23 C27 0.4(7) . . . . ? C20 C19 C24 C25 -80.0(6) . . . . ? C18 C19 C24 C25 96.4(6) . . . . ? C20 C19 C24 C26 43.4(6) . . . . ? C18 C19 C24 C26 -140.3(5) . . . . ? C22 C23 C27 C28 72.0(6) . . . . ? C18 C23 C27 C28 -103.3(6) . . . . ? C22 C23 C27 C29 -48.2(6) . . . . ? C18 C23 C27 C29 136.5(5) . . . . ? C1 Pd1 P1 C37 -112.5(14) . . . . ? Cl1 Pd1 P1 C37 145.15(18) . . . . ? Cl2 Pd1 P1 C37 -33.33(18) . . . . ? C1 Pd1 P1 C31 119.2(14) . . . . ? Cl1 Pd1 P1 C31 16.86(19) . . . . ? Cl2 Pd1 P1 C31 -161.62(19) . . . . ? C1 Pd1 P1 C43 2.9(14) . . . . ? Cl1 Pd1 P1 C43 -99.46(18) . . . . ? Cl2 Pd1 P1 C43 82.06(18) . . . . ? C37 P1 C31 C36 -62.0(4) . . . . ? C43 P1 C31 C36 -175.3(3) . . . . ? Pd1 P1 C31 C36 66.3(4) . . . . ? C37 P1 C31 C32 67.4(4) . . . . ? C43 P1 C31 C32 -45.8(4) . . . . ? Pd1 P1 C31 C32 -164.3(3) . . . . ? C36 C31 C32 C33 -56.0(6) . . . . ? P1 C31 C32 C33 173.8(4) . . . . ? C31 C32 C33 C34 55.8(6) . . . . ? C32 C33 C34 C35 -55.9(6) . . . . ? C33 C34 C35 C36 56.2(7) . . . . ? C32 C31 C36 C35 57.1(6) . . . . ? P1 C31 C36 C35 -169.6(4) . . . . ? C34 C35 C36 C31 -56.6(6) . . . . ? C31 P1 C37 C38 -51.3(4) . . . . ? C43 P1 C37 C38 61.4(4) . . . . ? Pd1 P1 C37 C38 178.5(3) . . . . ? C31 P1 C37 C42 77.1(4) . . . . ? C43 P1 C37 C42 -170.2(4) . . . . ? Pd1 P1 C37 C42 -53.1(4) . . . . ? C42 C37 C38 C39 60.2(6) . . . . ? P1 C37 C38 C39 -169.1(4) . . . . ? C37 C38 C39 C40 -56.8(6) . . . . ? C38 C39 C40 C41 53.1(6) . . . . ? C39 C40 C41 C42 -53.8(6) . . . . ? C40 C41 C42 C37 57.6(6) . . . . ? C38 C37 C42 C41 -60.5(6) . . . . ? P1 C37 C42 C41 166.9(4) . . . . ? C37 P1 C43 C44 49.9(4) . . . . ? C31 P1 C43 C44 167.5(4) . . . . ? Pd1 P1 C43 C44 -69.5(4) . . . . ? C37 P1 C43 C48 173.0(4) . . . . ? C31 P1 C43 C48 -69.4(4) . . . . ? Pd1 P1 C43 C48 53.6(4) . . . . ? C48 C43 C44 C45 55.1(6) . . . . ? P1 C43 C44 C45 177.7(4) . . . . ? C43 C44 C45 C46 -56.6(7) . . . . ? C44 C45 C46 C47 56.6(7) . . . . ? C45 C46 C47 C48 -55.5(6) . . . . ? C46 C47 C48 C43 55.8(7) . . . . ? C44 C43 C48 C47 -54.9(7) . . . . ? P1 C43 C48 C47 -180.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.130 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.078 data_2c _database_code_depnum_ccdc_archive 'CCDC 871884' #TrackingRef '10172_web_deposit_cif_file_2_CatherineS.J.Cazin_1331897901.2c.cif' # start Validation Reply Form _vrf_PLAT602_2c ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: No observable solvent - greatest peak only 0.99eA-3 at 0.07 A from PD1 ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H57 Cl2 N2 P Pd' _chemical_formula_sum 'C48 H57 Cl2 N2 P Pd' _chemical_formula_weight 870.23 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' 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 I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 24.122(4) _cell_length_b 24.122(4) _cell_length_c 18.253(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10620(3) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 17840 _cell_measurement_theta_min 1.1938 _cell_measurement_theta_max 28.6226 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7469 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33423 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.32 _reflns_number_total 9699 _reflns_number_gt 8227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 9699 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.789331(16) 0.461483(16) 0.52252(2) 0.03116(14) Uani 1 1 d . . . Cl1 Cl 0.85610(6) 0.51877(6) 0.57115(9) 0.0424(4) Uani 1 1 d . . . Cl2 Cl 0.71646(6) 0.40525(6) 0.48707(10) 0.0456(4) Uani 1 1 d . . . C1 C 0.7461(2) 0.5281(2) 0.4854(3) 0.0315(12) Uani 1 1 d . . . N2 N 0.74078(19) 0.54306(19) 0.4137(3) 0.0352(11) Uani 1 1 d . . . C3 C 0.7061(2) 0.5887(3) 0.4069(4) 0.0405(14) Uani 1 1 d . . . H3A H 0.6956 0.6064 0.3625 0.049 Uiso 1 1 calc R . . C4 C 0.6904(2) 0.6031(3) 0.4743(4) 0.0437(15) Uani 1 1 d . . . H4A H 0.6670 0.6332 0.4870 0.052 Uiso 1 1 calc R . . N5 N 0.71498(18) 0.56546(18) 0.5227(3) 0.0343(10) Uani 1 1 d . . . C6 C 0.7694(3) 0.5191(2) 0.3515(4) 0.0429(15) Uani 1 1 d . . . C7 C 0.8246(3) 0.5353(3) 0.3391(5) 0.060(2) Uani 1 1 d . . . C8 C 0.8499(4) 0.5146(5) 0.2773(7) 0.089(3) Uani 1 1 d . . . H8A H 0.8872 0.5246 0.2674 0.107 Uiso 1 1 calc R . . C9 C 0.8238(6) 0.4812(5) 0.2311(7) 0.112(5) Uani 1 1 d . . . H9A H 0.8434 0.4671 0.1900 0.135 Uiso 1 1 calc R . . C10 C 0.7687(5) 0.4662(4) 0.2412(5) 0.081(3) Uani 1 1 d . . . H10A H 0.7500 0.4441 0.2059 0.097 Uiso 1 1 calc R . . C11 C 0.7412(3) 0.4842(3) 0.3044(4) 0.0544(18) Uani 1 1 d . . . C12 C 0.8553(3) 0.5753(4) 0.3895(5) 0.076(3) Uani 1 1 d . . . H12A H 0.8393 0.5696 0.4395 0.092 Uiso 1 1 calc R . . C13 C 0.8442(4) 0.6347(4) 0.3703(6) 0.086(3) Uani 1 1 d . . . H13A H 0.8640 0.6589 0.4045 0.129 Uiso 1 1 calc R . . H13B H 0.8043 0.6420 0.3736 0.129 Uiso 1 1 calc R . . H13C H 0.8569 0.6420 0.3202 0.129 Uiso 1 1 calc R . . C14 C 0.9170(3) 0.5675(5) 0.3971(8) 0.150(7) Uani 1 1 d . . . H14A H 0.9318 0.5953 0.4311 0.225 Uiso 1 1 calc R . . H14B H 0.9346 0.5719 0.3492 0.225 Uiso 1 1 calc R . . H14C H 0.9246 0.5303 0.4161 0.225 Uiso 1 1 calc R . . C15 C 0.6817(3) 0.4658(3) 0.3168(4) 0.062(2) Uani 1 1 d . . . H15A H 0.6717 0.4739 0.3690 0.074 Uiso 1 1 calc R . . C16 C 0.6422(4) 0.5008(5) 0.2658(5) 0.097(3) Uani 1 1 d . . . H16A H 0.6037 0.4892 0.2737 0.146 Uiso 1 1 calc R . . H16B H 0.6523 0.4946 0.2144 0.146 Uiso 1 1 calc R . . H16C H 0.6459 0.5402 0.2775 0.146 Uiso 1 1 calc R . . C17 C 0.6734(4) 0.4049(4) 0.3034(5) 0.084(3) Uani 1 1 d . . . H17A H 0.6973 0.3836 0.3364 0.126 Uiso 1 1 calc R . . H17B H 0.6829 0.3962 0.2525 0.126 Uiso 1 1 calc R . . H17C H 0.6345 0.3952 0.3125 0.126 Uiso 1 1 calc R . . C18 C 0.7108(2) 0.5695(2) 0.6015(3) 0.0346(13) Uani 1 1 d . . . C19 C 0.6736(3) 0.5360(3) 0.6383(4) 0.0472(16) Uani 1 1 d . . . C20 C 0.6716(3) 0.5405(3) 0.7150(4) 0.0526(18) Uani 1 1 d . . . H20A H 0.6469 0.5179 0.7425 0.063 Uiso 1 1 calc R . . C21 C 0.7055(3) 0.5778(3) 0.7499(4) 0.058(2) Uani 1 1 d . . . H21A H 0.7048 0.5794 0.8019 0.070 Uiso 1 1 calc R . . C22 C 0.7402(3) 0.6127(3) 0.7127(4) 0.0506(18) Uani 1 1 d . . . H22A H 0.7615 0.6394 0.7387 0.061 Uiso 1 1 calc R . . C23 C 0.7442(2) 0.6091(3) 0.6360(4) 0.0425(15) Uani 1 1 d . . . C24 C 0.6332(3) 0.4983(3) 0.5965(4) 0.0512(17) Uani 1 1 d . . . H24A H 0.6505 0.4891 0.5482 0.061 Uiso 1 1 calc R . . C25 C 0.5791(3) 0.5301(4) 0.5814(6) 0.083(3) Uani 1 1 d . . . H25A H 0.5875 0.5645 0.5552 0.125 Uiso 1 1 calc R . . H25B H 0.5608 0.5388 0.6279 0.125 Uiso 1 1 calc R . . H25C H 0.5544 0.5071 0.5514 0.125 Uiso 1 1 calc R . . C26 C 0.6205(4) 0.4438(3) 0.6359(5) 0.077(3) Uani 1 1 d . . . H26A H 0.6551 0.4236 0.6447 0.115 Uiso 1 1 calc R . . H26B H 0.5958 0.4212 0.6053 0.115 Uiso 1 1 calc R . . H26C H 0.6023 0.4517 0.6827 0.115 Uiso 1 1 calc R . . C27 C 0.7809(3) 0.6490(3) 0.5948(4) 0.0485(16) Uani 1 1 d . . . H27A H 0.7863 0.6342 0.5442 0.058 Uiso 1 1 calc R . . C28 C 0.7528(4) 0.7058(3) 0.5887(5) 0.073(2) Uani 1 1 d . . . H28A H 0.7161 0.7014 0.5664 0.110 Uiso 1 1 calc R . . H28B H 0.7755 0.7303 0.5582 0.110 Uiso 1 1 calc R . . H28C H 0.7488 0.7220 0.6377 0.110 Uiso 1 1 calc R . . C29 C 0.8392(3) 0.6567(3) 0.6305(5) 0.0582(19) Uani 1 1 d . . . H29A H 0.8577 0.6206 0.6342 0.087 Uiso 1 1 calc R . . H29B H 0.8350 0.6726 0.6796 0.087 Uiso 1 1 calc R . . H29C H 0.8616 0.6816 0.6002 0.087 Uiso 1 1 calc R . . P1 P 0.83819(6) 0.38108(6) 0.55694(9) 0.0317(3) Uani 1 1 d . . . C31 C 0.9043(2) 0.3891(2) 0.6039(3) 0.0375(14) Uani 1 1 d . . . C32 C 0.9501(3) 0.4128(3) 0.5667(4) 0.0437(15) Uani 1 1 d . . . C33 C 0.9998(3) 0.4185(3) 0.6048(5) 0.058(2) Uani 1 1 d . . . H33A H 1.0307 0.4352 0.5811 0.070 Uiso 1 1 calc R . . C34 C 1.0054(3) 0.4000(3) 0.6773(5) 0.062(2) Uani 1 1 d . . . H34A H 1.0400 0.4035 0.7017 0.074 Uiso 1 1 calc R . . C35 C 0.9607(3) 0.3768(3) 0.7134(4) 0.0531(18) Uani 1 1 d . . . H35A H 0.9644 0.3645 0.7626 0.064 Uiso 1 1 calc R . . C36 C 0.9108(3) 0.3715(3) 0.6773(4) 0.0425(15) Uani 1 1 d . . . H36A H 0.8801 0.3556 0.7022 0.051 Uiso 1 1 calc R . . C37 C 0.9476(3) 0.4307(3) 0.4872(4) 0.0530(18) Uani 1 1 d . . . H37A H 0.9101 0.4246 0.4682 0.079 Uiso 1 1 calc R . . H37B H 0.9741 0.4089 0.4585 0.079 Uiso 1 1 calc R . . H37C H 0.9569 0.4701 0.4835 0.079 Uiso 1 1 calc R . . C38 C 0.8556(2) 0.3373(2) 0.4784(4) 0.0375(13) Uani 1 1 d . . . C39 C 0.8902(3) 0.2907(2) 0.4798(5) 0.0460(15) Uani 1 1 d . . . C40 C 0.9040(4) 0.2647(4) 0.4136(5) 0.072(2) Uani 1 1 d . . . H40A H 0.9275 0.2332 0.4145 0.086 Uiso 1 1 calc R . . C41 C 0.8840(3) 0.2838(4) 0.3460(5) 0.066(2) Uani 1 1 d . . . H41A H 0.8949 0.2664 0.3017 0.079 Uiso 1 1 calc R . . C42 C 0.8489(3) 0.3276(4) 0.3451(4) 0.064(2) Uani 1 1 d . . . H42A H 0.8334 0.3395 0.2999 0.076 Uiso 1 1 calc R . . C43 C 0.8350(3) 0.3556(3) 0.4098(4) 0.0521(18) Uani 1 1 d . . . H43A H 0.8116 0.3872 0.4076 0.062 Uiso 1 1 calc R . . C44 C 0.9164(4) 0.2686(3) 0.5496(5) 0.069(2) Uani 1 1 d . . . H44A H 0.9387 0.2358 0.5382 0.103 Uiso 1 1 calc R . . H44B H 0.8873 0.2586 0.5846 0.103 Uiso 1 1 calc R . . H44C H 0.9403 0.2972 0.5711 0.103 Uiso 1 1 calc R . . C45 C 0.7949(2) 0.3393(3) 0.6178(3) 0.0377(14) Uani 1 1 d . . . C46 C 0.7710(2) 0.3633(3) 0.6801(4) 0.0448(16) Uani 1 1 d . . . C47 C 0.7360(3) 0.3287(4) 0.7223(4) 0.061(2) Uani 1 1 d . . . H47A H 0.7190 0.3438 0.7649 0.073 Uiso 1 1 calc R . . C48 C 0.7255(4) 0.2755(4) 0.7053(5) 0.075(3) Uani 1 1 d . . . H48A H 0.7017 0.2538 0.7353 0.090 Uiso 1 1 calc R . . C49 C 0.7496(4) 0.2526(4) 0.6436(5) 0.075(3) Uani 1 1 d . . . H49A H 0.7433 0.2147 0.6318 0.090 Uiso 1 1 calc R . . C50 C 0.7828(3) 0.2849(3) 0.5993(4) 0.0564(18) Uani 1 1 d . . . H50A H 0.7977 0.2696 0.5555 0.068 Uiso 1 1 calc R . . C51 C 0.7808(3) 0.4224(3) 0.7023(4) 0.0546(18) Uani 1 1 d . . . H51A H 0.8062 0.4400 0.6674 0.082 Uiso 1 1 calc R . . H51B H 0.7971 0.4234 0.7514 0.082 Uiso 1 1 calc R . . H51C H 0.7455 0.4425 0.7025 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0270(2) 0.0288(2) 0.0377(2) 0.0020(2) -0.00308(19) -0.00121(17) Cl1 0.0351(8) 0.0367(8) 0.0553(10) -0.0008(7) -0.0120(7) -0.0055(6) Cl2 0.0343(7) 0.0397(8) 0.0629(10) -0.0021(8) -0.0080(8) -0.0101(6) C1 0.024(3) 0.030(3) 0.040(3) -0.002(3) 0.003(3) -0.005(2) N2 0.032(3) 0.033(3) 0.041(3) 0.001(2) -0.002(2) 0.005(2) C3 0.032(3) 0.049(4) 0.041(4) 0.005(3) -0.002(3) 0.009(3) C4 0.032(3) 0.042(3) 0.058(4) -0.001(3) -0.014(3) 0.012(2) N5 0.031(2) 0.032(2) 0.039(3) -0.002(2) -0.009(2) 0.0036(19) C6 0.045(4) 0.030(3) 0.054(4) 0.005(3) 0.008(3) 0.008(3) C7 0.041(4) 0.067(5) 0.073(5) 0.027(4) 0.011(4) 0.012(4) C8 0.070(6) 0.091(7) 0.107(8) 0.019(7) 0.048(6) 0.024(6) C9 0.140(12) 0.092(8) 0.104(9) 0.010(7) 0.075(9) 0.039(8) C10 0.116(8) 0.062(5) 0.065(5) -0.013(5) 0.038(5) 0.014(5) C11 0.065(5) 0.051(4) 0.047(4) -0.002(3) 0.015(4) 0.014(4) C12 0.030(4) 0.115(7) 0.083(6) 0.053(6) 0.002(4) -0.016(4) C13 0.062(5) 0.086(7) 0.110(8) 0.001(6) -0.024(5) 0.007(5) C14 0.037(4) 0.162(11) 0.252(16) 0.153(12) -0.018(7) -0.008(6) C15 0.065(5) 0.069(5) 0.052(5) -0.017(4) 0.007(4) -0.010(4) C16 0.081(7) 0.152(11) 0.059(6) -0.014(6) -0.004(5) 0.010(7) C17 0.104(7) 0.070(6) 0.078(6) -0.023(5) -0.002(6) -0.029(5) C18 0.029(3) 0.036(3) 0.039(3) -0.005(3) -0.006(3) 0.005(2) C19 0.041(4) 0.051(4) 0.050(4) -0.008(3) -0.003(3) 0.013(3) C20 0.047(4) 0.059(4) 0.052(5) 0.003(4) 0.004(3) 0.007(3) C21 0.064(5) 0.067(5) 0.043(4) -0.009(4) -0.016(4) 0.014(4) C22 0.048(4) 0.064(5) 0.040(4) -0.011(4) -0.012(3) 0.007(3) C23 0.036(3) 0.044(4) 0.048(4) -0.007(3) -0.005(3) 0.006(3) C24 0.043(4) 0.050(4) 0.061(5) -0.014(3) 0.002(3) -0.011(3) C25 0.051(5) 0.095(7) 0.104(7) -0.029(6) -0.022(5) -0.006(4) C26 0.079(6) 0.070(5) 0.082(6) -0.010(5) 0.012(5) -0.037(5) C27 0.049(4) 0.041(4) 0.054(4) -0.004(3) -0.007(3) -0.005(3) C28 0.076(5) 0.052(4) 0.092(6) 0.007(4) -0.034(5) -0.006(4) C29 0.043(4) 0.056(4) 0.075(5) -0.008(4) -0.014(4) -0.005(3) P1 0.0303(8) 0.0302(7) 0.0347(8) 0.0044(7) -0.0008(7) 0.0001(6) C31 0.037(3) 0.034(3) 0.042(4) 0.000(3) -0.001(3) 0.001(2) C32 0.037(3) 0.041(3) 0.053(4) -0.002(3) -0.001(3) 0.000(3) C33 0.031(3) 0.060(4) 0.083(6) -0.006(4) -0.004(4) -0.004(3) C34 0.038(4) 0.079(5) 0.069(5) -0.006(4) -0.023(4) 0.002(4) C35 0.040(4) 0.067(5) 0.053(4) -0.007(4) -0.017(3) 0.012(3) C36 0.040(3) 0.044(4) 0.043(4) -0.005(3) -0.002(3) 0.010(3) C37 0.037(3) 0.054(4) 0.069(5) 0.017(4) 0.017(3) -0.001(3) C38 0.038(3) 0.037(3) 0.037(3) -0.005(3) 0.002(3) 0.001(2) C39 0.049(4) 0.034(3) 0.055(4) -0.011(3) 0.002(4) 0.006(3) C40 0.071(5) 0.060(5) 0.086(6) -0.025(5) 0.001(5) 0.011(4) C41 0.067(5) 0.077(5) 0.055(5) -0.022(4) -0.002(4) 0.014(4) C42 0.070(5) 0.087(6) 0.034(4) -0.010(4) -0.003(4) 0.003(5) C43 0.044(4) 0.059(4) 0.053(4) 0.001(3) -0.004(3) 0.006(3) C44 0.083(6) 0.052(4) 0.072(6) -0.001(4) -0.009(5) 0.023(4) C45 0.033(3) 0.042(3) 0.037(3) 0.011(3) -0.007(3) -0.005(2) C46 0.030(3) 0.052(4) 0.052(4) 0.007(3) 0.002(3) -0.005(3) C47 0.044(4) 0.095(6) 0.044(4) 0.015(4) 0.009(3) -0.006(4) C48 0.078(6) 0.079(6) 0.069(6) 0.032(5) -0.005(5) -0.040(5) C49 0.092(6) 0.063(5) 0.070(6) 0.011(5) -0.003(5) -0.045(5) C50 0.058(4) 0.054(4) 0.057(4) 0.006(4) -0.001(4) -0.014(3) C51 0.047(4) 0.070(5) 0.046(4) 0.003(4) 0.004(3) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.032(6) . ? Pd1 Cl1 2.3002(15) . ? Pd1 Cl2 2.3127(15) . ? Pd1 P1 2.3547(15) . ? C1 N5 1.357(7) . ? C1 N2 1.362(8) . ? N2 C3 1.388(8) . ? N2 C6 1.450(8) . ? C3 C4 1.333(10) . ? C3 H3A 0.9500 . ? C4 N5 1.398(8) . ? C4 H4A 0.9500 . ? N5 C18 1.445(8) . ? C6 C11 1.383(10) . ? C6 C7 1.406(9) . ? C7 C8 1.375(13) . ? C7 C12 1.525(13) . ? C8 C9 1.324(16) . ? C8 H8A 0.9500 . ? C9 C10 1.392(16) . ? C9 H9A 0.9500 . ? C10 C11 1.399(10) . ? C10 H10A 0.9500 . ? C11 C15 1.520(11) . ? C12 C13 1.498(12) . ? C12 C14 1.507(10) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.504(11) . ? C15 C16 1.577(13) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.382(9) . ? C18 C23 1.401(9) . ? C19 C20 1.404(10) . ? C19 C24 1.536(9) . ? C20 C21 1.372(11) . ? C20 H20A 0.9500 . ? C21 C22 1.368(11) . ? C21 H21A 0.9500 . ? C22 C23 1.405(9) . ? C22 H22A 0.9500 . ? C23 C27 1.507(10) . ? C24 C26 1.531(11) . ? C24 C25 1.539(11) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.533(10) . ? C27 C29 1.561(9) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C31 1.821(6) . ? P1 C45 1.827(6) . ? P1 C38 1.829(6) . ? C31 C36 1.414(9) . ? C31 C32 1.417(9) . ? C32 C33 1.393(9) . ? C32 C37 1.515(10) . ? C33 C34 1.402(12) . ? C33 H33A 0.9500 . ? C34 C35 1.382(11) . ? C34 H34A 0.9500 . ? C35 C36 1.379(9) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.400(8) . ? C38 C43 1.419(9) . ? C39 C40 1.401(11) . ? C39 C44 1.519(11) . ? C40 C41 1.402(12) . ? C40 H40A 0.9500 . ? C41 C42 1.355(11) . ? C41 H41A 0.9500 . ? C42 C43 1.399(10) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.387(9) . ? C45 C46 1.400(9) . ? C46 C47 1.416(9) . ? C46 C51 1.502(10) . ? C47 C48 1.344(12) . ? C47 H47A 0.9500 . ? C48 C49 1.382(13) . ? C48 H48A 0.9500 . ? C49 C50 1.381(10) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl1 90.73(15) . . ? C1 Pd1 Cl2 88.89(15) . . ? Cl1 Pd1 Cl2 172.97(7) . . ? C1 Pd1 P1 175.67(18) . . ? Cl1 Pd1 P1 92.37(5) . . ? Cl2 Pd1 P1 88.40(5) . . ? N5 C1 N2 104.7(5) . . ? N5 C1 Pd1 129.9(5) . . ? N2 C1 Pd1 125.3(4) . . ? C1 N2 C3 110.7(5) . . ? C1 N2 C6 127.0(5) . . ? C3 N2 C6 122.2(5) . . ? C4 C3 N2 107.1(6) . . ? C4 C3 H3A 126.4 . . ? N2 C3 H3A 126.4 . . ? C3 C4 N5 107.1(5) . . ? C3 C4 H4A 126.4 . . ? N5 C4 H4A 126.4 . . ? C1 N5 C4 110.3(5) . . ? C1 N5 C18 125.7(5) . . ? C4 N5 C18 123.8(5) . . ? C11 C6 C7 122.3(7) . . ? C11 C6 N2 119.6(6) . . ? C7 C6 N2 117.9(6) . . ? C8 C7 C6 116.8(9) . . ? C8 C7 C12 120.7(8) . . ? C6 C7 C12 122.5(7) . . ? C9 C8 C7 122.2(10) . . ? C9 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? C8 C9 C10 121.8(10) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C9 C10 C11 118.8(10) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C6 C11 C10 117.9(8) . . ? C6 C11 C15 123.4(6) . . ? C10 C11 C15 118.7(8) . . ? C13 C12 C14 108.5(7) . . ? C13 C12 C7 112.2(7) . . ? C14 C12 C7 117.1(10) . . ? C13 C12 H12A 106.1 . . ? C14 C12 H12A 106.1 . . ? C7 C12 H12A 106.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C11 112.7(7) . . ? C17 C15 C16 110.2(8) . . ? C11 C15 C16 109.1(7) . . ? C17 C15 H15A 108.2 . . ? C11 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.6(6) . . ? C19 C18 N5 119.3(5) . . ? C23 C18 N5 117.0(6) . . ? C18 C19 C20 117.5(6) . . ? C18 C19 C24 121.1(6) . . ? C20 C19 C24 121.3(7) . . ? C21 C20 C19 119.5(7) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C22 C21 C20 122.6(7) . . ? C22 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? C21 C22 C23 119.9(7) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C18 C23 C22 116.8(6) . . ? C18 C23 C27 123.3(6) . . ? C22 C23 C27 119.9(6) . . ? C26 C24 C19 113.7(7) . . ? C26 C24 C25 109.9(7) . . ? C19 C24 C25 109.5(6) . . ? C26 C24 H24A 107.8 . . ? C19 C24 H24A 107.8 . . ? C25 C24 H24A 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 110.3(6) . . ? C23 C27 C29 113.3(6) . . ? C28 C27 C29 108.9(6) . . ? C23 C27 H27A 108.1 . . ? C28 C27 H27A 108.1 . . ? C29 C27 H27A 108.1 . . ? 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 . . ? C31 P1 C45 105.8(3) . . ? C31 P1 C38 103.2(3) . . ? C45 P1 C38 106.8(3) . . ? C31 P1 Pd1 118.4(2) . . ? C45 P1 Pd1 109.3(2) . . ? C38 P1 Pd1 112.4(2) . . ? C36 C31 C32 119.3(6) . . ? C36 C31 P1 120.7(5) . . ? C32 C31 P1 120.0(5) . . ? C33 C32 C31 118.1(7) . . ? C33 C32 C37 119.0(6) . . ? C31 C32 C37 122.8(6) . . ? C32 C33 C34 121.5(7) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C35 C34 C33 120.3(6) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C36 C35 C34 119.4(7) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? C35 C36 C31 121.4(7) . . ? C35 C36 H36A 119.3 . . ? C31 C36 H36A 119.3 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C43 118.3(6) . . ? C39 C38 P1 125.9(6) . . ? C43 C38 P1 115.6(4) . . ? C38 C39 C40 119.0(7) . . ? C38 C39 C44 123.0(7) . . ? C40 C39 C44 117.9(6) . . ? C39 C40 C41 122.0(7) . . ? C39 C40 H40A 119.0 . . ? C41 C40 H40A 119.0 . . ? C42 C41 C40 118.8(7) . . ? C42 C41 H41A 120.6 . . ? C40 C41 H41A 120.6 . . ? C41 C42 C43 121.0(7) . . ? C41 C42 H42A 119.5 . . ? C43 C42 H42A 119.5 . . ? C42 C43 C38 120.8(6) . . ? C42 C43 H43A 119.6 . . ? C38 C43 H43A 119.6 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 120.2(6) . . ? C50 C45 P1 119.6(5) . . ? C46 C45 P1 120.1(5) . . ? C45 C46 C47 116.4(7) . . ? C45 C46 C51 123.1(6) . . ? C47 C46 C51 120.5(7) . . ? C48 C47 C46 123.3(8) . . ? C48 C47 H47A 118.4 . . ? C46 C47 H47A 118.4 . . ? C47 C48 C49 119.4(7) . . ? C47 C48 H48A 120.3 . . ? C49 C48 H48A 120.3 . . ? C50 C49 C48 119.7(8) . . ? C50 C49 H49A 120.1 . . ? C48 C49 H49A 120.1 . . ? C49 C50 C45 120.9(7) . . ? C49 C50 H50A 119.6 . . ? C45 C50 H50A 119.6 . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 C1 N5 -73.8(5) . . . . ? Cl2 Pd1 C1 N5 99.1(5) . . . . ? P1 Pd1 C1 N5 150.4(18) . . . . ? Cl1 Pd1 C1 N2 109.3(4) . . . . ? Cl2 Pd1 C1 N2 -77.7(4) . . . . ? P1 Pd1 C1 N2 -26(2) . . . . ? N5 C1 N2 C3 -0.8(6) . . . . ? Pd1 C1 N2 C3 176.7(4) . . . . ? N5 C1 N2 C6 174.7(5) . . . . ? Pd1 C1 N2 C6 -7.8(8) . . . . ? C1 N2 C3 C4 1.0(7) . . . . ? C6 N2 C3 C4 -174.7(5) . . . . ? N2 C3 C4 N5 -0.8(7) . . . . ? N2 C1 N5 C4 0.2(6) . . . . ? Pd1 C1 N5 C4 -177.1(4) . . . . ? N2 C1 N5 C18 -175.0(5) . . . . ? Pd1 C1 N5 C18 7.7(8) . . . . ? C3 C4 N5 C1 0.4(6) . . . . ? C3 C4 N5 C18 175.7(5) . . . . ? C1 N2 C6 C11 105.4(7) . . . . ? C3 N2 C6 C11 -79.6(8) . . . . ? C1 N2 C6 C7 -78.4(8) . . . . ? C3 N2 C6 C7 96.6(7) . . . . ? C11 C6 C7 C8 -0.1(11) . . . . ? N2 C6 C7 C8 -176.2(7) . . . . ? C11 C6 C7 C12 177.8(7) . . . . ? N2 C6 C7 C12 1.7(10) . . . . ? C6 C7 C8 C9 0.3(14) . . . . ? C12 C7 C8 C9 -177.7(10) . . . . ? C7 C8 C9 C10 1.9(18) . . . . ? C8 C9 C10 C11 -4.1(17) . . . . ? C7 C6 C11 C10 -2.1(11) . . . . ? N2 C6 C11 C10 174.0(7) . . . . ? C7 C6 C11 C15 179.6(7) . . . . ? N2 C6 C11 C15 -4.3(10) . . . . ? C9 C10 C11 C6 4.1(13) . . . . ? C9 C10 C11 C15 -177.5(9) . . . . ? C8 C7 C12 C13 93.0(10) . . . . ? C6 C7 C12 C13 -84.9(9) . . . . ? C8 C7 C12 C14 -33.5(11) . . . . ? C6 C7 C12 C14 148.6(7) . . . . ? C6 C11 C15 C17 -135.6(8) . . . . ? C10 C11 C15 C17 46.1(11) . . . . ? C6 C11 C15 C16 101.7(9) . . . . ? C10 C11 C15 C16 -76.6(9) . . . . ? C1 N5 C18 C19 -84.3(7) . . . . ? C4 N5 C18 C19 101.1(7) . . . . ? C1 N5 C18 C23 97.6(7) . . . . ? C4 N5 C18 C23 -77.0(7) . . . . ? C23 C18 C19 C20 -3.2(10) . . . . ? N5 C18 C19 C20 178.9(6) . . . . ? C23 C18 C19 C24 172.5(6) . . . . ? N5 C18 C19 C24 -5.4(9) . . . . ? C18 C19 C20 C21 0.8(10) . . . . ? C24 C19 C20 C21 -174.9(6) . . . . ? C19 C20 C21 C22 2.6(11) . . . . ? C20 C21 C22 C23 -3.5(11) . . . . ? C19 C18 C23 C22 2.2(9) . . . . ? N5 C18 C23 C22 -179.8(5) . . . . ? C19 C18 C23 C27 -174.3(6) . . . . ? N5 C18 C23 C27 3.7(8) . . . . ? C21 C22 C23 C18 1.1(10) . . . . ? C21 C22 C23 C27 177.8(6) . . . . ? C18 C19 C24 C26 146.5(7) . . . . ? C20 C19 C24 C26 -37.9(9) . . . . ? C18 C19 C24 C25 -90.0(8) . . . . ? C20 C19 C24 C25 85.5(9) . . . . ? C18 C23 C27 C28 99.8(7) . . . . ? C22 C23 C27 C28 -76.7(8) . . . . ? C18 C23 C27 C29 -137.9(6) . . . . ? C22 C23 C27 C29 45.6(9) . . . . ? C1 Pd1 P1 C31 135(2) . . . . ? Cl1 Pd1 P1 C31 -0.4(2) . . . . ? Cl2 Pd1 P1 C31 -173.4(2) . . . . ? C1 Pd1 P1 C45 -103(2) . . . . ? Cl1 Pd1 P1 C45 120.8(2) . . . . ? Cl2 Pd1 P1 C45 -52.2(2) . . . . ? C1 Pd1 P1 C38 15(2) . . . . ? Cl1 Pd1 P1 C38 -120.8(2) . . . . ? Cl2 Pd1 P1 C38 66.2(2) . . . . ? C45 P1 C31 C36 -8.5(6) . . . . ? C38 P1 C31 C36 -120.6(5) . . . . ? Pd1 P1 C31 C36 114.4(5) . . . . ? C45 P1 C31 C32 170.9(5) . . . . ? C38 P1 C31 C32 58.9(5) . . . . ? Pd1 P1 C31 C32 -66.1(5) . . . . ? C36 C31 C32 C33 -0.9(9) . . . . ? P1 C31 C32 C33 179.7(5) . . . . ? C36 C31 C32 C37 177.4(6) . . . . ? P1 C31 C32 C37 -2.1(8) . . . . ? C31 C32 C33 C34 1.7(11) . . . . ? C37 C32 C33 C34 -176.7(7) . . . . ? C32 C33 C34 C35 -1.5(12) . . . . ? C33 C34 C35 C36 0.5(11) . . . . ? C34 C35 C36 C31 0.3(10) . . . . ? C32 C31 C36 C35 -0.1(9) . . . . ? P1 C31 C36 C35 179.4(5) . . . . ? C31 P1 C38 C39 42.7(6) . . . . ? C45 P1 C38 C39 -68.6(6) . . . . ? Pd1 P1 C38 C39 171.5(5) . . . . ? C31 P1 C38 C43 -132.3(5) . . . . ? C45 P1 C38 C43 116.4(5) . . . . ? Pd1 P1 C38 C43 -3.5(5) . . . . ? C43 C38 C39 C40 1.2(10) . . . . ? P1 C38 C39 C40 -173.7(5) . . . . ? C43 C38 C39 C44 177.7(7) . . . . ? P1 C38 C39 C44 2.8(10) . . . . ? C38 C39 C40 C41 -0.2(12) . . . . ? C44 C39 C40 C41 -176.8(8) . . . . ? C39 C40 C41 C42 -2.3(13) . . . . ? C40 C41 C42 C43 3.7(13) . . . . ? C41 C42 C43 C38 -2.7(12) . . . . ? C39 C38 C43 C42 0.2(10) . . . . ? P1 C38 C43 C42 175.6(6) . . . . ? C31 P1 C45 C50 -108.5(5) . . . . ? C38 P1 C45 C50 1.0(6) . . . . ? Pd1 P1 C45 C50 122.9(5) . . . . ? C31 P1 C45 C46 76.0(5) . . . . ? C38 P1 C45 C46 -174.5(5) . . . . ? Pd1 P1 C45 C46 -52.6(5) . . . . ? C50 C45 C46 C47 1.6(9) . . . . ? P1 C45 C46 C47 177.1(5) . . . . ? C50 C45 C46 C51 -178.1(6) . . . . ? P1 C45 C46 C51 -2.6(9) . . . . ? C45 C46 C47 C48 0.1(11) . . . . ? C51 C46 C47 C48 179.9(7) . . . . ? C46 C47 C48 C49 0.0(13) . . . . ? C47 C48 C49 C50 -1.8(14) . . . . ? C48 C49 C50 C45 3.6(13) . . . . ? C46 C45 C50 C49 -3.5(11) . . . . ? P1 C45 C50 C49 -179.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.990 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.113 data_2d _database_code_depnum_ccdc_archive 'CCDC 871885' #TrackingRef '10173_web_deposit_cif_file_3_CatherineS.J.Cazin_1331897901.2d.cif' # start Validation Reply Form _vrf_PLAT221_2d ; PROBLEM: Large Solvent/Anion C Ueq(max)/Ueq(min) ... 6.25 Ratio RESPONSE: Disordered solvent-see _refine_special_details. ; _vrf_PLAT973_2d ; PROBLEM: Large Calcd. Positive Residual Density on Pd61 5.48 eA-3 RESPONSE: Highest residual electron density in res file near disordered solvent. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H75 Cl2 N2 P Pd,0.5(C H2 Cl2)' _chemical_formula_sum 'C51.50 H76 Cl3 N2 P Pd' _chemical_formula_weight 966.86 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.854(3) _cell_length_b 16.741(4) _cell_length_c 21.852(4) _cell_angle_alpha 93.602(5) _cell_angle_beta 91.002(6) _cell_angle_gamma 92.724(7) _cell_volume 5051.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 18433 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 26.4 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39296 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.35 _reflns_number_total 18263 _reflns_number_gt 13272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is a partial weight dichloromethane diordered into 3 loactions which was refined isotropically without hydrogen atoms. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18263 _refine_ls_number_parameters 1059 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.3680 _refine_ls_wR_factor_gt 0.2788 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_restrained_S_all 1.340 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.08044(4) 0.21053(3) 0.78097(2) 0.0258(2) Uani 1 1 d . . . Cl1 Cl -0.03226(13) 0.10326(11) 0.76685(9) 0.0319(4) Uani 1 1 d . . . Cl2 Cl 0.19894(14) 0.31122(12) 0.78631(10) 0.0391(5) Uani 1 1 d . . . C1 C 0.1801(5) 0.1399(5) 0.7403(4) 0.0303(17) Uani 1 1 d . . . N2 N 0.2360(5) 0.0894(4) 0.7697(3) 0.0327(15) Uani 1 1 d . . . C3 C 0.2953(6) 0.0490(5) 0.7276(4) 0.038(2) Uani 1 1 d . . . H3A H 0.3407 0.0103 0.7367 0.046 Uiso 1 1 calc R . . C4 C 0.2763(6) 0.0748(5) 0.6740(4) 0.0339(18) Uani 1 1 d . . . H4A H 0.3056 0.0585 0.6366 0.041 Uiso 1 1 calc R . . N5 N 0.2047(4) 0.1310(4) 0.6813(3) 0.0307(15) Uani 1 1 d . . . C6 C 0.2411(5) 0.0839(5) 0.8350(4) 0.0328(18) Uani 1 1 d . . . C7 C 0.1786(5) 0.0259(5) 0.8618(4) 0.0320(17) Uani 1 1 d . . . C8 C 0.1828(7) 0.0265(6) 0.9259(4) 0.044(2) Uani 1 1 d . . . H8A H 0.1425 -0.0109 0.9459 0.053 Uiso 1 1 calc R . . C9 C 0.2433(7) 0.0793(6) 0.9611(4) 0.048(2) Uani 1 1 d . . . H9A H 0.2416 0.0796 1.0045 0.058 Uiso 1 1 calc R . . C10 C 0.3051(7) 0.1306(6) 0.9344(4) 0.051(2) Uani 1 1 d . . . H10A H 0.3493 0.1637 0.9596 0.061 Uiso 1 1 calc R . . C11 C 0.3061(6) 0.1367(5) 0.8699(4) 0.0357(18) Uani 1 1 d . . . C12 C 0.1153(6) -0.0344(6) 0.8228(5) 0.043(2) Uani 1 1 d . . . H12A H 0.0979 -0.0094 0.7840 0.052 Uiso 1 1 calc R . . C13 C 0.0224(7) -0.0580(7) 0.8541(5) 0.061(3) Uani 1 1 d . . . H13A H -0.0159 -0.0970 0.8273 0.091 Uiso 1 1 calc R . . H13B H -0.0148 -0.0103 0.8626 0.091 Uiso 1 1 calc R . . H13C H 0.0378 -0.0818 0.8927 0.091 Uiso 1 1 calc R . . C14 C 0.1703(7) -0.1081(6) 0.8061(6) 0.055(3) Uani 1 1 d . . . H14A H 0.1286 -0.1468 0.7812 0.082 Uiso 1 1 calc R . . H14B H 0.1906 -0.1323 0.8437 0.082 Uiso 1 1 calc R . . H14C H 0.2274 -0.0930 0.7828 0.082 Uiso 1 1 calc R . . C15 C 0.3774(7) 0.1917(5) 0.8394(4) 0.044(2) Uani 1 1 d . . . H15A H 0.3495 0.2040 0.7988 0.053 Uiso 1 1 calc R . . C16 C 0.4717(7) 0.1501(7) 0.8287(5) 0.063(3) Uani 1 1 d . . . H16A H 0.4588 0.1004 0.8031 0.094 Uiso 1 1 calc R . . H16B H 0.4999 0.1375 0.8682 0.094 Uiso 1 1 calc R . . H16C H 0.5170 0.1856 0.8080 0.094 Uiso 1 1 calc R . . C17 C 0.3963(9) 0.2710(6) 0.8783(6) 0.071(3) Uani 1 1 d . . . H17A H 0.4427 0.3055 0.8576 0.106 Uiso 1 1 calc R . . H17B H 0.4228 0.2598 0.9186 0.106 Uiso 1 1 calc R . . H17C H 0.3355 0.2980 0.8835 0.106 Uiso 1 1 calc R . . C18 C 0.1660(6) 0.1772(5) 0.6340(3) 0.0319(17) Uani 1 1 d . . . C19 C 0.0797(5) 0.1481(5) 0.6039(4) 0.0343(19) Uani 1 1 d . . . C20 C 0.0441(7) 0.1945(6) 0.5584(4) 0.048(2) Uani 1 1 d . . . H20A H -0.0138 0.1769 0.5367 0.057 Uiso 1 1 calc R . . C21 C 0.0925(9) 0.2674(7) 0.5438(4) 0.057(3) Uani 1 1 d . . . H21A H 0.0652 0.2994 0.5143 0.069 Uiso 1 1 calc R . . C22 C 0.1770(8) 0.2908(5) 0.5721(5) 0.051(3) Uani 1 1 d . . . H22A H 0.2107 0.3379 0.5600 0.061 Uiso 1 1 calc R . . C23 C 0.2177(6) 0.2477(6) 0.6192(4) 0.042(2) Uani 1 1 d . . . C24 C 0.0339(6) 0.0684(6) 0.6152(4) 0.040(2) Uani 1 1 d . . . H24A H 0.0496 0.0566 0.6584 0.048 Uiso 1 1 calc R . . C25 C 0.0775(6) 0.0038(5) 0.5724(5) 0.045(2) Uani 1 1 d . . . H25A H 0.1478 0.0058 0.5786 0.068 Uiso 1 1 calc R . . H25B H 0.0620 0.0135 0.5297 0.068 Uiso 1 1 calc R . . H25C H 0.0505 -0.0491 0.5818 0.068 Uiso 1 1 calc R . . C26 C -0.0767(6) 0.0648(7) 0.6071(4) 0.053(3) Uani 1 1 d . . . H26A H -0.1039 0.1055 0.6351 0.079 Uiso 1 1 calc R . . H26B H -0.1028 0.0116 0.6164 0.079 Uiso 1 1 calc R . . H26C H -0.0939 0.0751 0.5647 0.079 Uiso 1 1 calc R . . C27 C 0.3174(7) 0.2727(6) 0.6462(4) 0.047(2) Uani 1 1 d . . . H27A H 0.3247 0.2472 0.6861 0.056 Uiso 1 1 calc R . . C28 C 0.3978(7) 0.2419(6) 0.6027(5) 0.059(3) Uani 1 1 d . . . H28A H 0.4615 0.2577 0.6209 0.089 Uiso 1 1 calc R . . H28B H 0.3912 0.2653 0.5629 0.089 Uiso 1 1 calc R . . H28C H 0.3910 0.1833 0.5968 0.089 Uiso 1 1 calc R . . C29 C 0.3311(11) 0.3625(7) 0.6586(5) 0.077(4) Uani 1 1 d . . . H29A H 0.2810 0.3815 0.6863 0.115 Uiso 1 1 calc R . . H29B H 0.3263 0.3887 0.6199 0.115 Uiso 1 1 calc R . . H29C H 0.3950 0.3755 0.6777 0.115 Uiso 1 1 calc R . . P30 P -0.03020(13) 0.29800(12) 0.82736(9) 0.0266(4) Uani 1 1 d . . . C31 C -0.1167(5) 0.2535(5) 0.8821(4) 0.0339(18) Uani 1 1 d . . . C32 C -0.1602(6) 0.3150(5) 0.9276(4) 0.043(2) Uani 1 1 d . . . H32A H -0.1993 0.3516 0.9047 0.052 Uiso 1 1 calc R . . H32B H -0.1073 0.3475 0.9496 0.052 Uiso 1 1 calc R . . C33 C -0.2246(6) 0.2736(6) 0.9749(4) 0.044(2) Uani 1 1 d . . . H33A H -0.2517 0.3147 1.0041 0.053 Uiso 1 1 calc R . . C34 C -0.3080(6) 0.2249(6) 0.9388(4) 0.049(2) Uani 1 1 d . . . H34A H -0.3515 0.1987 0.9678 0.059 Uiso 1 1 calc R . . H34B H -0.3462 0.2613 0.9152 0.059 Uiso 1 1 calc R . . C35A C -0.2655(6) 0.1612(5) 0.8950(4) 0.039(2) Uani 1 1 d . . . H35A H -0.3194 0.1291 0.8727 0.047 Uiso 1 1 calc R . . C36 C -0.2034(5) 0.2049(4) 0.8484(4) 0.0304(17) Uani 1 1 d . . . H36A H -0.2436 0.2418 0.8265 0.036 Uiso 1 1 calc R . . H36B H -0.1785 0.1654 0.8177 0.036 Uiso 1 1 calc R . . C37 C -0.0586(6) 0.1956(5) 0.9185(4) 0.0333(18) Uani 1 1 d . . . H37A H -0.0031 0.2255 0.9399 0.040 Uiso 1 1 calc R . . H37B H -0.0329 0.1540 0.8899 0.040 Uiso 1 1 calc R . . C38 C -0.1231(6) 0.1549(5) 0.9664(4) 0.0367(19) Uani 1 1 d . . . H38A H -0.0840 0.1187 0.9905 0.044 Uiso 1 1 calc R . . C39 C -0.1645(8) 0.2188(6) 1.0089(4) 0.052(3) Uani 1 1 d . . . H39A H -0.2047 0.1929 1.0398 0.063 Uiso 1 1 calc R . . H39B H -0.1110 0.2504 1.0309 0.063 Uiso 1 1 calc R . . C40 C -0.2068(6) 0.1063(5) 0.9319(4) 0.042(2) Uani 1 1 d . . . H40A H -0.1805 0.0641 0.9041 0.051 Uiso 1 1 calc R . . H40B H -0.2489 0.0800 0.9616 0.051 Uiso 1 1 calc R . . C41 C -0.0930(5) 0.3465(5) 0.7631(4) 0.0305(17) Uani 1 1 d . . . C42 C -0.1781(6) 0.4003(5) 0.7840(4) 0.0370(19) Uani 1 1 d . . . H42A H -0.2280 0.3673 0.8041 0.044 Uiso 1 1 calc R . . H42B H -0.1533 0.4433 0.8141 0.044 Uiso 1 1 calc R . . C43 C -0.2221(7) 0.4367(5) 0.7296(4) 0.046(2) Uani 1 1 d . . . H43A H -0.2769 0.4696 0.7437 0.055 Uiso 1 1 calc R . . C44 C -0.1470(7) 0.4907(5) 0.6990(4) 0.046(2) Uani 1 1 d . . . H44A H -0.1767 0.5139 0.6630 0.055 Uiso 1 1 calc R . . H44B H -0.1236 0.5352 0.7283 0.055 Uiso 1 1 calc R . . C45 C -0.0619(7) 0.4404(5) 0.6785(4) 0.041(2) Uani 1 1 d . . . H45A H -0.0114 0.4751 0.6596 0.050 Uiso 1 1 calc R . . C46 C -0.0191(6) 0.4030(5) 0.7346(4) 0.0377(19) Uani 1 1 d . . . H46A H 0.0379 0.3729 0.7221 0.045 Uiso 1 1 calc R . . H46B H 0.0028 0.4461 0.7655 0.045 Uiso 1 1 calc R . . C47 C -0.1759(7) 0.3215(5) 0.6610(4) 0.045(2) Uani 1 1 d . . . H47A H -0.1996 0.2783 0.6299 0.054 Uiso 1 1 calc R . . C48 C -0.2615(7) 0.3689(6) 0.6828(5) 0.050(2) Uani 1 1 d . . . H48A H -0.2935 0.3920 0.6476 0.060 Uiso 1 1 calc R . . H48B H -0.3093 0.3334 0.7024 0.060 Uiso 1 1 calc R . . C49 C -0.0998(6) 0.3742(5) 0.6321(4) 0.040(2) Uani 1 1 d . . . H49A H -0.1280 0.3982 0.5960 0.048 Uiso 1 1 calc R . . H49B H -0.0458 0.3415 0.6180 0.048 Uiso 1 1 calc R . . C50 C -0.1304(6) 0.2831(5) 0.7147(4) 0.0334(18) Uani 1 1 d . . . H50A H -0.0763 0.2508 0.7002 0.040 Uiso 1 1 calc R . . H50B H -0.1789 0.2468 0.7329 0.040 Uiso 1 1 calc R . . C51 C 0.0322(6) 0.3815(5) 0.8739(4) 0.0346(18) Uani 1 1 d . . . H51A H 0.0720 0.4137 0.8463 0.042 Uiso 1 1 calc R . . H51B H -0.0173 0.4166 0.8915 0.042 Uiso 1 1 calc R . . C52 C 0.0990(6) 0.3570(5) 0.9276(4) 0.041(2) Uani 1 1 d . . . H52A H 0.0588 0.3463 0.9635 0.049 Uiso 1 1 calc R . . H52B H 0.1300 0.3068 0.9147 0.049 Uiso 1 1 calc R . . C53 C 0.1773(6) 0.4216(6) 0.9466(5) 0.048(2) Uani 1 1 d . . . H53A H 0.2212 0.4007 0.9774 0.058 Uiso 1 1 calc R . . H53B H 0.2159 0.4337 0.9103 0.058 Uiso 1 1 calc R . . C54 C 0.1370(8) 0.4971(6) 0.9729(5) 0.055(3) Uani 1 1 d . . . H54A H 0.1900 0.5365 0.9839 0.082 Uiso 1 1 calc R . . H54B H 0.1004 0.4859 1.0096 0.082 Uiso 1 1 calc R . . H54C H 0.0941 0.5185 0.9425 0.082 Uiso 1 1 calc R . . Pd61 Pd 0.55183(4) 0.77194(3) 0.72256(3) 0.0266(2) Uani 1 1 d . . . Cl61 Cl 0.45836(13) 0.88343(11) 0.72561(9) 0.0323(4) Uani 1 1 d . . . Cl62 Cl 0.64819(15) 0.66479(12) 0.73176(10) 0.0400(5) Uani 1 1 d . . . C61 C 0.6597(5) 0.8431(5) 0.7649(4) 0.0301(17) Uani 1 1 d . . . N62 N 0.6874(4) 0.8513(4) 0.8240(3) 0.0255(13) Uani 1 1 d . . . C63 C 0.7611(5) 0.9094(4) 0.8336(4) 0.0286(16) Uani 1 1 d . . . H63A H 0.7919 0.9261 0.8718 0.034 Uiso 1 1 calc R . . C64 C 0.7811(5) 0.9381(5) 0.7788(4) 0.0319(18) Uani 1 1 d . . . H64A H 0.8294 0.9781 0.7709 0.038 Uiso 1 1 calc R . . N65 N 0.7170(4) 0.8977(3) 0.7355(3) 0.0246(13) Uani 1 1 d . . . C66 C 0.6480(5) 0.8028(4) 0.8700(4) 0.0314(17) Uani 1 1 d . . . C67 C 0.6983(6) 0.7384(5) 0.8858(4) 0.0383(19) Uani 1 1 d . . . C68 C 0.6522(7) 0.6852(5) 0.9270(4) 0.045(2) Uani 1 1 d . . . H68A H 0.6841 0.6393 0.9386 0.054 Uiso 1 1 calc R . . C69 C 0.5631(7) 0.7000(6) 0.9494(4) 0.043(2) Uani 1 1 d . . . H69A H 0.5315 0.6630 0.9746 0.052 Uiso 1 1 calc R . . C70 C 0.5185(7) 0.7700(5) 0.9352(4) 0.043(2) Uani 1 1 d . . . H70A H 0.4584 0.7815 0.9532 0.052 Uiso 1 1 calc R . . C71 C 0.5586(5) 0.8221(4) 0.8964(4) 0.0309(17) Uani 1 1 d . . . C72 C 0.7993(7) 0.7215(6) 0.8645(4) 0.045(2) Uani 1 1 d . . . H72A H 0.8102 0.7492 0.8258 0.053 Uiso 1 1 calc R . . C73 C 0.8184(8) 0.6310(6) 0.8510(5) 0.063(3) Uani 1 1 d . . . H73A H 0.7717 0.6075 0.8200 0.094 Uiso 1 1 calc R . . H73B H 0.8115 0.6029 0.8888 0.094 Uiso 1 1 calc R . . H73C H 0.8841 0.6258 0.8358 0.094 Uiso 1 1 calc R . . C74 C 0.8744(7) 0.7573(7) 0.9130(5) 0.058(3) Uani 1 1 d . . . H74A H 0.8637 0.8143 0.9216 0.087 Uiso 1 1 calc R . . H74B H 0.9396 0.7512 0.8973 0.087 Uiso 1 1 calc R . . H74C H 0.8674 0.7292 0.9508 0.087 Uiso 1 1 calc R . . C75 C 0.5143(5) 0.9016(5) 0.8850(4) 0.0324(17) Uani 1 1 d . . . H75A H 0.5261 0.9128 0.8413 0.039 Uiso 1 1 calc R . . C76 C 0.5661(7) 0.9693(6) 0.9250(5) 0.046(2) Uani 1 1 d . . . H76A H 0.5376 1.0203 0.9172 0.069 Uiso 1 1 calc R . . H76B H 0.6348 0.9723 0.9151 0.069 Uiso 1 1 calc R . . H76C H 0.5590 0.9587 0.9683 0.069 Uiso 1 1 calc R . . C77 C 0.4050(6) 0.9010(6) 0.8941(5) 0.051(2) Uani 1 1 d . . . H77A H 0.3734 0.8575 0.8679 0.077 Uiso 1 1 calc R . . H77B H 0.3806 0.9523 0.8832 0.077 Uiso 1 1 calc R . . H77C H 0.3910 0.8928 0.9371 0.077 Uiso 1 1 calc R . . C78 C 0.7219(5) 0.9030(5) 0.6708(4) 0.0323(18) Uani 1 1 d . . . C79 C 0.7763(6) 0.8486(5) 0.6368(4) 0.0368(19) Uani 1 1 d . . . C80 C 0.7763(7) 0.8517(6) 0.5734(4) 0.047(2) Uani 1 1 d . . . H80A H 0.8134 0.8157 0.5493 0.057 Uiso 1 1 calc R . . C81 C 0.7226(7) 0.9071(5) 0.5449(4) 0.045(2) Uani 1 1 d . . . H81A H 0.7198 0.9066 0.5015 0.054 Uiso 1 1 calc R . . C82 C 0.6723(7) 0.9637(6) 0.5801(4) 0.046(2) Uani 1 1 d . . . H82A H 0.6382 1.0031 0.5603 0.055 Uiso 1 1 calc R . . C83 C 0.6719(5) 0.9627(5) 0.6437(4) 0.0306(17) Uani 1 1 d . . . C84 C 0.8411(6) 0.7929(5) 0.6696(4) 0.041(2) Uani 1 1 d . . . H84A H 0.8132 0.7838 0.7107 0.049 Uiso 1 1 calc R . . C85 C 0.8459(9) 0.7097(6) 0.6330(5) 0.063(3) Uani 1 1 d . . . H85A H 0.8877 0.6753 0.6553 0.095 Uiso 1 1 calc R . . H85B H 0.8723 0.7175 0.5924 0.095 Uiso 1 1 calc R . . H85C H 0.7808 0.6842 0.6285 0.095 Uiso 1 1 calc R . . C86 C 0.9423(8) 0.8305(7) 0.6796(6) 0.068(3) Uani 1 1 d . . . H86A H 0.9392 0.8819 0.7034 0.102 Uiso 1 1 calc R . . H86B H 0.9711 0.8393 0.6398 0.102 Uiso 1 1 calc R . . H86C H 0.9819 0.7947 0.7020 0.102 Uiso 1 1 calc R . . C87 C 0.6217(5) 1.0288(5) 0.6801(4) 0.0345(18) Uani 1 1 d . . . H87A H 0.6032 1.0074 0.7203 0.041 Uiso 1 1 calc R . . C88 C 0.6917(6) 1.1014(5) 0.6942(4) 0.041(2) Uani 1 1 d . . . H88A H 0.7507 1.0841 0.7137 0.061 Uiso 1 1 calc R . . H88B H 0.6612 1.1405 0.7219 0.061 Uiso 1 1 calc R . . H88C H 0.7079 1.1260 0.6559 0.061 Uiso 1 1 calc R . . C89 C 0.5302(6) 1.0558(5) 0.6502(5) 0.045(2) Uani 1 1 d . . . H89A H 0.4849 1.0096 0.6417 0.067 Uiso 1 1 calc R . . H89B H 0.5463 1.0799 0.6117 0.067 Uiso 1 1 calc R . . H89C H 0.5005 1.0955 0.6778 0.067 Uiso 1 1 calc R . . P90 P 0.42907(14) 0.68888(12) 0.67122(9) 0.0276(4) Uani 1 1 d . . . C91 C 0.3676(5) 0.7354(5) 0.6055(4) 0.0314(17) Uani 1 1 d . . . C92 C 0.2854(6) 0.7896(5) 0.6263(4) 0.0379(19) Uani 1 1 d . . . H92A H 0.2348 0.7572 0.6464 0.045 Uiso 1 1 calc R . . H92B H 0.3113 0.8319 0.6567 0.045 Uiso 1 1 calc R . . C93 C 0.2412(6) 0.8280(6) 0.5719(5) 0.053(3) Uani 1 1 d . . . H93A H 0.1886 0.8632 0.5863 0.063 Uiso 1 1 calc R . . C94 C 0.1985(6) 0.7613(7) 0.5238(5) 0.055(3) Uani 1 1 d . . . H94A H 0.1471 0.7285 0.5425 0.067 Uiso 1 1 calc R . . H94B H 0.1702 0.7863 0.4881 0.067 Uiso 1 1 calc R . . C95 C 0.2783(6) 0.7101(6) 0.5035(5) 0.048(2) Uani 1 1 d . . . H95A H 0.2517 0.6668 0.4734 0.058 Uiso 1 1 calc R . . C96 C 0.3241(6) 0.6721(5) 0.5572(4) 0.0378(19) Uani 1 1 d . . . H96A H 0.3756 0.6373 0.5421 0.045 Uiso 1 1 calc R . . H96B H 0.2747 0.6379 0.5767 0.045 Uiso 1 1 calc R . . C97 C 0.4434(6) 0.7873(5) 0.5743(3) 0.0309(17) Uani 1 1 d . . . H97A H 0.4968 0.7539 0.5603 0.037 Uiso 1 1 calc R . . H97B H 0.4707 0.8297 0.6043 0.037 Uiso 1 1 calc R . . C98 C 0.3990(6) 0.8263(6) 0.5192(4) 0.042(2) Uani 1 1 d . . . H98A H 0.4499 0.8598 0.4996 0.050 Uiso 1 1 calc R . . C99 C 0.3192(7) 0.8781(5) 0.5405(5) 0.047(2) Uani 1 1 d . . . H99A H 0.2902 0.9028 0.5050 0.056 Uiso 1 1 calc R . . H99B H 0.3458 0.9216 0.5696 0.056 Uiso 1 1 calc R . . C100 C 0.3576(7) 0.7609(6) 0.4721(4) 0.051(2) Uani 1 1 d . . . H10E H 0.3294 0.7858 0.4363 0.061 Uiso 1 1 calc R . . H10F H 0.4095 0.7264 0.4574 0.061 Uiso 1 1 calc R . . C101 C 0.3406(6) 0.6502(5) 0.7274(4) 0.0350(18) Uani 1 1 d . . . C102 C 0.2521(8) 0.6032(6) 0.6989(5) 0.055(3) Uani 1 1 d . . . H10G H 0.2162 0.6376 0.6722 0.066 Uiso 1 1 calc R . . H10H H 0.2727 0.5562 0.6736 0.066 Uiso 1 1 calc R . . C103 C 0.1864(11) 0.5752(9) 0.7500(6) 0.094(5) Uani 1 1 d . . . H10B H 0.1283 0.5450 0.7309 0.113 Uiso 1 1 calc R . . C104 C 0.1536(8) 0.6455(10) 0.7904(6) 0.086(4) Uani 1 1 d . . . H10I H 0.1196 0.6829 0.7651 0.103 Uiso 1 1 calc R . . H10J H 0.1082 0.6261 0.8213 0.103 Uiso 1 1 calc R . . C105 C 0.2413(8) 0.6880(7) 0.8219(5) 0.060(3) Uani 1 1 d . . . H10C H 0.2202 0.7345 0.8484 0.072 Uiso 1 1 calc R . . C106 C 0.3083(7) 0.7195(5) 0.7712(4) 0.045(2) Uani 1 1 d . . . H10K H 0.2734 0.7579 0.7474 0.054 Uiso 1 1 calc R . . H10L H 0.3660 0.7483 0.7908 0.054 Uiso 1 1 calc R . . C107 C 0.2955(9) 0.6363(6) 0.8592(5) 0.059(3) Uani 1 1 d . . . H10M H 0.2543 0.6173 0.8924 0.070 Uiso 1 1 calc R . . H10N H 0.3524 0.6669 0.8783 0.070 Uiso 1 1 calc R . . C108 C 0.3284(9) 0.5655(7) 0.8205(5) 0.064(3) Uani 1 1 d . . . H10D H 0.3637 0.5292 0.8467 0.077 Uiso 1 1 calc R . . C109 C 0.2405(11) 0.5201(6) 0.7896(6) 0.081(4) Uani 1 1 d . . . H10O H 0.2618 0.4736 0.7640 0.098 Uiso 1 1 calc R . . H10P H 0.1971 0.4999 0.8213 0.098 Uiso 1 1 calc R . . C110 C 0.3942(8) 0.5937(6) 0.7694(4) 0.052(3) Uani 1 1 d . . . H11J H 0.4150 0.5465 0.7443 0.063 Uiso 1 1 calc R . . H11K H 0.4527 0.6225 0.7879 0.063 Uiso 1 1 calc R . . C111 C 0.4769(5) 0.5960(4) 0.6369(4) 0.0300(17) Uani 1 1 d . . . H11D H 0.5036 0.5658 0.6703 0.036 Uiso 1 1 calc R . . H11E H 0.4223 0.5628 0.6174 0.036 Uiso 1 1 calc R . . C112 C 0.5562(6) 0.6066(5) 0.5883(4) 0.0352(18) Uani 1 1 d . . . H11F H 0.5260 0.6208 0.5493 0.042 Uiso 1 1 calc R . . H11G H 0.6024 0.6510 0.6026 0.042 Uiso 1 1 calc R . . C113 C 0.6109(7) 0.5289(5) 0.5772(5) 0.050(2) Uani 1 1 d . . . H11H H 0.6430 0.5165 0.6161 0.059 Uiso 1 1 calc R . . H11I H 0.5636 0.4842 0.5654 0.059 Uiso 1 1 calc R . . C114 C 0.6859(7) 0.5337(7) 0.5282(5) 0.054(3) Uani 1 1 d . . . H11A H 0.7183 0.4829 0.5239 0.081 Uiso 1 1 calc R . . H11B H 0.7337 0.5773 0.5398 0.081 Uiso 1 1 calc R . . H11C H 0.6545 0.5439 0.4891 0.081 Uiso 1 1 calc R . . C201 C 0.038(3) 0.470(2) 0.5011(18) 0.112(11) Uiso 0.50 1 d P . . Cl4 Cl 0.0764(8) 0.5331(7) 0.5393(5) 0.116(3) Uiso 0.50 1 d P . . Cl5 Cl -0.0403(7) 0.4319(6) 0.4552(5) 0.107(3) Uiso 0.50 1 d P . . C202 C 0.6442 0.4691 0.8993 0.100 Uiso 0.25 1 d PD A 1 Cl6 Cl 0.5982(15) 0.4653(13) 0.9682(8) 0.125(6) Uiso 0.25 1 d PD A 1 Cl7 Cl 0.5733(17) 0.4516(16) 0.8371(10) 0.151(8) Uiso 0.25 1 d PD A 1 C203 C 0.5809(16) 0.4924(12) 0.8520(8) 0.016(5) Uiso 0.25 1 d PD B 2 Cl8 Cl 0.6307(8) 0.4598(7) 0.9141(5) 0.063(3) Uiso 0.25 1 d PD B 2 Cl9 Cl 0.5424(4) 0.4250(4) 0.7937(3) 0.0180(12) Uiso 0.25 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0275(4) 0.0268(4) 0.0226(4) -0.0026(2) 0.0040(2) -0.0018(2) Cl1 0.0320(9) 0.0311(10) 0.0316(10) -0.0051(8) 0.0024(8) -0.0007(7) Cl2 0.0358(10) 0.0380(11) 0.0423(12) -0.0036(9) 0.0101(9) -0.0078(8) C1 0.025(4) 0.040(4) 0.025(4) -0.002(3) -0.002(3) -0.002(3) N2 0.033(3) 0.033(4) 0.032(4) 0.001(3) -0.003(3) 0.006(3) C3 0.033(4) 0.044(5) 0.037(5) -0.001(4) -0.003(3) 0.006(4) C4 0.034(4) 0.031(4) 0.036(5) -0.009(4) 0.008(3) 0.005(3) N5 0.023(3) 0.045(4) 0.023(3) -0.011(3) 0.000(2) 0.009(3) C6 0.026(4) 0.039(5) 0.032(4) -0.007(4) -0.004(3) -0.003(3) C7 0.033(4) 0.034(4) 0.031(4) 0.009(3) 0.002(3) 0.009(3) C8 0.050(5) 0.049(5) 0.035(5) 0.015(4) 0.006(4) -0.003(4) C9 0.059(6) 0.054(6) 0.033(5) 0.012(4) 0.004(4) 0.007(5) C10 0.061(6) 0.066(7) 0.024(5) -0.002(4) -0.011(4) 0.006(5) C11 0.047(5) 0.028(4) 0.032(4) 0.003(3) -0.006(4) -0.001(3) C12 0.038(4) 0.048(5) 0.046(5) 0.019(4) -0.004(4) 0.000(4) C13 0.036(5) 0.074(7) 0.073(8) 0.020(6) -0.015(5) -0.014(5) C14 0.041(5) 0.038(5) 0.083(8) -0.013(5) -0.007(5) -0.001(4) C15 0.052(5) 0.037(5) 0.041(5) 0.008(4) -0.020(4) -0.014(4) C16 0.040(5) 0.088(8) 0.059(7) 0.011(6) -0.016(5) 0.008(5) C17 0.083(8) 0.050(6) 0.074(8) -0.001(6) -0.038(6) -0.021(6) C18 0.049(5) 0.027(4) 0.021(4) 0.004(3) 0.006(3) 0.003(3) C19 0.029(4) 0.045(5) 0.029(4) -0.008(4) 0.003(3) 0.018(3) C20 0.052(5) 0.066(7) 0.028(5) 0.008(4) 0.003(4) 0.021(5) C21 0.086(8) 0.063(7) 0.031(5) 0.019(5) 0.023(5) 0.047(6) C22 0.079(7) 0.032(5) 0.044(6) 0.010(4) 0.035(5) 0.012(5) C23 0.053(5) 0.049(5) 0.025(4) 0.004(4) 0.021(4) 0.008(4) C24 0.037(4) 0.057(6) 0.026(4) -0.006(4) 0.004(3) 0.009(4) C25 0.044(5) 0.042(5) 0.049(6) -0.010(4) 0.009(4) 0.011(4) C26 0.040(5) 0.081(7) 0.034(5) -0.020(5) 0.000(4) 0.004(5) C27 0.069(6) 0.043(5) 0.028(5) 0.002(4) 0.009(4) -0.020(4) C28 0.045(5) 0.058(6) 0.074(8) 0.005(6) 0.013(5) -0.012(5) C29 0.120(11) 0.054(7) 0.051(7) -0.002(5) 0.011(7) -0.037(7) P30 0.0301(10) 0.0289(10) 0.0198(9) -0.0041(8) 0.0068(7) -0.0041(8) C31 0.028(4) 0.040(5) 0.032(4) -0.012(4) 0.002(3) -0.001(3) C32 0.036(4) 0.037(5) 0.053(6) -0.020(4) 0.014(4) -0.010(4) C33 0.042(5) 0.047(5) 0.041(5) -0.016(4) 0.015(4) -0.007(4) C34 0.046(5) 0.057(6) 0.042(5) -0.008(4) 0.026(4) -0.015(4) C35A 0.037(4) 0.035(5) 0.044(5) -0.002(4) 0.006(4) -0.012(4) C36 0.034(4) 0.024(4) 0.033(4) 0.002(3) 0.006(3) -0.005(3) C37 0.042(4) 0.033(4) 0.023(4) 0.001(3) 0.002(3) -0.019(3) C38 0.043(4) 0.042(5) 0.025(4) 0.007(3) 0.006(3) -0.010(4) C39 0.066(6) 0.061(6) 0.028(5) 0.006(4) 0.012(4) -0.018(5) C40 0.050(5) 0.047(5) 0.028(4) 0.004(4) 0.005(4) -0.023(4) C41 0.032(4) 0.034(4) 0.025(4) -0.001(3) 0.000(3) 0.006(3) C42 0.055(5) 0.030(4) 0.026(4) 0.000(3) 0.015(4) 0.010(4) C43 0.057(5) 0.031(5) 0.050(6) -0.007(4) 0.008(4) 0.021(4) C44 0.069(6) 0.023(4) 0.046(5) 0.004(4) -0.011(5) 0.007(4) C45 0.056(5) 0.029(4) 0.038(5) 0.002(4) 0.003(4) -0.008(4) C46 0.043(4) 0.024(4) 0.045(5) -0.002(4) -0.001(4) -0.005(3) C47 0.052(5) 0.039(5) 0.042(5) -0.014(4) -0.010(4) 0.005(4) C48 0.049(5) 0.041(5) 0.062(7) 0.007(5) -0.008(5) 0.011(4) C49 0.055(5) 0.042(5) 0.024(4) 0.001(4) -0.001(4) 0.012(4) C50 0.035(4) 0.032(4) 0.031(4) -0.004(3) -0.002(3) -0.003(3) C51 0.044(4) 0.025(4) 0.034(4) -0.005(3) 0.006(4) -0.002(3) C52 0.046(5) 0.037(5) 0.037(5) -0.005(4) 0.006(4) -0.014(4) C53 0.043(5) 0.046(5) 0.054(6) -0.012(4) -0.002(4) -0.015(4) C54 0.064(6) 0.050(6) 0.049(6) -0.009(5) 0.011(5) -0.010(5) Pd61 0.0297(4) 0.0257(4) 0.0234(4) -0.0030(2) 0.0016(2) -0.0021(2) Cl61 0.0342(9) 0.0256(9) 0.0366(11) -0.0025(8) 0.0031(8) 0.0005(7) Cl62 0.0456(11) 0.0325(11) 0.0412(12) -0.0015(9) -0.0086(9) 0.0053(9) C61 0.028(4) 0.033(4) 0.028(4) -0.012(3) 0.002(3) 0.008(3) N62 0.017(3) 0.029(3) 0.030(3) 0.000(3) 0.003(2) -0.001(2) C63 0.033(4) 0.025(4) 0.027(4) -0.004(3) 0.005(3) -0.004(3) C64 0.031(4) 0.032(4) 0.031(4) -0.014(3) 0.004(3) -0.002(3) N65 0.040(3) 0.016(3) 0.018(3) 0.007(2) 0.011(3) 0.000(2) C66 0.036(4) 0.025(4) 0.032(4) -0.009(3) -0.006(3) 0.000(3) C67 0.046(5) 0.032(4) 0.037(5) -0.001(4) -0.005(4) 0.003(4) C68 0.070(6) 0.032(5) 0.032(5) -0.001(4) -0.005(4) -0.004(4) C69 0.061(6) 0.044(5) 0.025(4) 0.013(4) 0.001(4) -0.015(4) C70 0.051(5) 0.040(5) 0.036(5) -0.010(4) 0.012(4) -0.011(4) C71 0.035(4) 0.020(4) 0.037(5) -0.001(3) -0.002(3) -0.008(3) C72 0.049(5) 0.047(5) 0.038(5) 0.000(4) 0.006(4) 0.007(4) C73 0.061(6) 0.061(7) 0.064(7) -0.016(6) -0.021(5) 0.021(5) C74 0.043(5) 0.076(8) 0.056(7) 0.002(5) -0.005(5) 0.018(5) C75 0.032(4) 0.041(5) 0.025(4) 0.002(3) 0.008(3) 0.001(3) C76 0.045(5) 0.042(5) 0.051(6) -0.007(4) 0.010(4) -0.003(4) C77 0.038(5) 0.067(7) 0.047(6) -0.007(5) -0.005(4) 0.009(4) C78 0.028(4) 0.043(5) 0.024(4) -0.006(3) 0.003(3) -0.004(3) C79 0.040(4) 0.031(4) 0.039(5) -0.005(4) 0.010(4) -0.006(3) C80 0.055(5) 0.041(5) 0.044(6) -0.017(4) 0.017(4) -0.001(4) C81 0.064(6) 0.043(5) 0.027(5) 0.004(4) 0.013(4) 0.002(4) C82 0.051(5) 0.046(5) 0.039(5) -0.002(4) -0.010(4) -0.009(4) C83 0.023(3) 0.034(4) 0.033(4) -0.001(3) 0.004(3) -0.006(3) C84 0.045(5) 0.043(5) 0.037(5) 0.007(4) 0.013(4) 0.011(4) C85 0.087(8) 0.039(6) 0.067(7) 0.008(5) 0.019(6) 0.023(5) C86 0.069(7) 0.059(7) 0.077(8) 0.004(6) -0.006(6) 0.020(6) C87 0.029(4) 0.042(5) 0.032(4) 0.007(4) 0.009(3) -0.008(3) C88 0.037(4) 0.039(5) 0.046(5) 0.007(4) -0.005(4) 0.003(4) C89 0.039(4) 0.038(5) 0.056(6) 0.005(4) 0.002(4) -0.008(4) P90 0.0330(10) 0.0241(10) 0.0247(10) -0.0038(8) 0.0029(8) -0.0033(8) C91 0.033(4) 0.030(4) 0.031(4) 0.001(3) 0.004(3) 0.001(3) C92 0.037(4) 0.026(4) 0.052(6) 0.010(4) 0.006(4) 0.002(3) C93 0.034(4) 0.061(6) 0.065(7) 0.024(5) 0.000(4) 0.003(4) C94 0.032(4) 0.076(7) 0.061(7) 0.037(6) -0.012(4) 0.004(5) C95 0.039(5) 0.058(6) 0.046(6) 0.012(4) -0.017(4) -0.009(4) C96 0.036(4) 0.046(5) 0.031(5) 0.006(4) -0.005(3) -0.003(4) C97 0.038(4) 0.031(4) 0.023(4) 0.003(3) 0.004(3) -0.006(3) C98 0.037(4) 0.057(6) 0.034(5) 0.022(4) -0.007(4) 0.000(4) C99 0.055(5) 0.027(4) 0.062(6) 0.030(4) -0.001(5) 0.006(4) C100 0.062(6) 0.059(6) 0.032(5) 0.002(4) -0.016(4) -0.004(5) C101 0.040(4) 0.031(4) 0.033(4) 0.002(3) 0.002(3) -0.009(3) C102 0.068(6) 0.057(6) 0.039(5) 0.014(5) -0.008(5) -0.021(5) C103 0.106(10) 0.107(11) 0.062(8) 0.000(8) 0.020(7) -0.084(9) C104 0.054(7) 0.146(13) 0.057(8) 0.012(8) 0.026(6) -0.021(8) C105 0.066(7) 0.049(6) 0.064(7) -0.008(5) 0.035(6) -0.008(5) C106 0.058(5) 0.038(5) 0.039(5) 0.001(4) 0.024(4) -0.006(4) C107 0.085(7) 0.043(6) 0.044(6) -0.009(5) 0.022(5) -0.031(5) C108 0.110(9) 0.057(7) 0.030(5) 0.018(5) 0.034(6) 0.012(6) C109 0.150(12) 0.026(5) 0.066(8) -0.005(5) 0.043(8) -0.025(7) C110 0.076(6) 0.050(6) 0.036(5) 0.021(4) 0.022(5) 0.022(5) C111 0.038(4) 0.020(4) 0.032(4) -0.004(3) 0.001(3) 0.000(3) C112 0.041(4) 0.027(4) 0.038(5) -0.004(3) 0.002(4) 0.007(3) C113 0.054(5) 0.032(5) 0.063(7) -0.001(4) 0.007(5) 0.011(4) C114 0.056(6) 0.068(7) 0.039(5) 0.003(5) 0.012(4) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.040(8) . ? Pd1 Cl2 2.293(2) . ? Pd1 Cl1 2.3248(19) . ? Pd1 P30 2.3671(19) . ? C1 N5 1.340(10) . ? C1 N2 1.356(10) . ? N2 C3 1.407(10) . ? N2 C6 1.436(10) . ? C3 C4 1.301(12) . ? C3 H3A 0.9500 . ? C4 N5 1.403(10) . ? C4 H4A 0.9500 . ? N5 C18 1.440(10) . ? C6 C7 1.431(12) . ? C6 C11 1.410(10) . ? C7 C8 1.402(12) . ? C7 C12 1.515(12) . ? C8 C9 1.377(13) . ? C8 H8A 0.9500 . ? C9 C10 1.349(14) . ? C9 H9A 0.9500 . ? C10 C11 1.421(12) . ? C10 H10A 0.9500 . ? C11 C15 1.509(12) . ? C12 C14 1.509(13) . ? C12 C13 1.516(13) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.524(14) . ? C15 C17 1.539(13) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.406(11) . ? C18 C23 1.409(12) . ? C19 C20 1.397(12) . ? C19 C24 1.486(13) . ? C20 C21 1.420(15) . ? C20 H20A 0.9500 . ? C21 C22 1.345(15) . ? C21 H21A 0.9500 . ? C22 C23 1.419(14) . ? C22 H22A 0.9500 . ? C23 C27 1.522(13) . ? C24 C26 1.537(12) . ? C24 C25 1.537(11) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.514(14) . ? C27 C28 1.562(14) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P30 C51 1.848(7) . ? P30 C31 1.871(8) . ? P30 C41 1.886(8) . ? C31 C37 1.539(12) . ? C31 C32 1.537(10) . ? C31 C36 1.565(10) . ? C32 C33 1.552(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C39 1.491(14) . ? C33 C34 1.555(12) . ? C33 H33A 1.0000 . ? C34 C35A 1.533(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35A C40 1.515(13) . ? C35A C36 1.542(11) . ? C35A H35A 1.0000 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.556(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.512(13) . ? C38 C40 1.543(11) . ? C38 H38A 1.0000 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.528(11) . ? C41 C50 1.517(10) . ? C41 C42 1.573(10) . ? C42 C43 1.502(13) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.552(13) . ? C43 C44 1.537(14) . ? C43 H43A 1.0000 . ? C44 C45 1.536(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C49 1.523(11) . ? C45 C46 1.533(13) . ? C45 H45A 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C49 1.515(13) . ? C47 C50 1.516(12) . ? C47 C48 1.525(13) . ? C47 H47A 1.0000 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.569(13) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.529(11) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.492(13) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Pd61 C61 2.037(7) . ? Pd61 Cl62 2.303(2) . ? Pd61 Cl61 2.320(2) . ? Pd61 P90 2.3659(19) . ? C61 N62 1.339(10) . ? C61 N65 1.379(10) . ? N62 C63 1.380(9) . ? N62 C66 1.431(10) . ? C63 C64 1.348(12) . ? C63 H63A 0.9500 . ? C64 N65 1.405(9) . ? C64 H64A 0.9500 . ? N65 C78 1.424(10) . ? C66 C67 1.371(12) . ? C66 C71 1.418(11) . ? C67 C68 1.442(13) . ? C67 C72 1.516(12) . ? C68 C69 1.364(14) . ? C68 H68A 0.9500 . ? C69 C70 1.400(14) . ? C69 H69A 0.9500 . ? C70 C71 1.361(12) . ? C70 H70A 0.9500 . ? C71 C75 1.525(11) . ? C72 C74 1.544(13) . ? C72 C73 1.560(13) . ? C72 H72A 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C77 1.530(11) . ? C75 C76 1.529(11) . ? C75 H75A 1.0000 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C83 1.400(12) . ? C78 C79 1.397(11) . ? C79 C80 1.390(13) . ? C79 C84 1.528(13) . ? C80 C81 1.386(14) . ? C80 H80A 0.9500 . ? C81 C82 1.402(13) . ? C81 H81A 0.9500 . ? C82 C83 1.390(12) . ? C82 H82A 0.9500 . ? C83 C87 1.524(11) . ? C84 C86 1.516(15) . ? C84 C85 1.567(13) . ? C84 H84A 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C89 1.517(12) . ? C87 C88 1.531(11) . ? C87 H87A 1.0000 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? P90 C111 1.841(7) . ? P90 C101 1.873(8) . ? P90 C91 1.886(8) . ? C91 C97 1.527(11) . ? C91 C96 1.542(11) . ? C91 C92 1.547(11) . ? C92 C93 1.520(13) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C99 1.534(13) . ? C93 C94 1.573(15) . ? C93 H93A 1.0000 . ? C94 C95 1.487(14) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.514(12) . ? C95 C100 1.554(14) . ? C95 H95A 1.0000 . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.539(11) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.501(13) . ? C98 C100 1.537(12) . ? C98 H98A 1.0000 . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H10E 0.9900 . ? C100 H10F 0.9900 . ? C101 C102 1.527(12) . ? C101 C106 1.545(11) . ? C101 C110 1.561(13) . ? C102 C103 1.533(15) . ? C102 H10G 0.9900 . ? C102 H10H 0.9900 . ? C103 C109 1.52(2) . ? C103 C104 1.52(2) . ? C103 H10B 1.0000 . ? C104 C105 1.512(16) . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 C107 1.450(17) . ? C105 C106 1.558(13) . ? C105 H10C 1.0000 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.506(14) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 C110 1.538(13) . ? C108 C109 1.527(18) . ? C108 H10D 1.0000 . ? C109 H10O 0.9900 . ? C109 H10P 0.9900 . ? C110 H11J 0.9900 . ? C110 H11K 0.9900 . ? C111 C112 1.553(11) . ? C111 H11D 0.9900 . ? C111 H11E 0.9900 . ? C112 C113 1.545(11) . ? C112 H11F 0.9900 . ? C112 H11G 0.9900 . ? C113 C114 1.507(13) . ? C113 H11H 0.9900 . ? C113 H11I 0.9900 . ? C114 H11A 0.9800 . ? C114 H11B 0.9800 . ? C114 H11C 0.9800 . ? C201 Cl4 1.38(4) . ? C201 C201 1.47(7) 2_566 ? C201 Cl5 1.55(4) . ? C201 Cl5 1.84(4) 2_566 ? C201 Cl4 1.79(4) 2_566 ? Cl4 Cl5 0.793(12) 2_566 ? Cl4 C201 1.79(4) 2_566 ? Cl5 Cl4 0.793(12) 2_566 ? Cl5 C201 1.84(4) 2_566 ? C202 Cl7 1.666(16) . ? C202 Cl6 1.649(15) . ? C203 Cl9 1.709(16) . ? C203 Cl8 1.647(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl2 86.6(2) . . ? C1 Pd1 Cl1 88.4(2) . . ? Cl2 Pd1 Cl1 174.28(7) . . ? C1 Pd1 P30 177.2(2) . . ? Cl2 Pd1 P30 90.69(7) . . ? Cl1 Pd1 P30 94.26(7) . . ? N5 C1 N2 105.0(6) . . ? N5 C1 Pd1 129.9(6) . . ? N2 C1 Pd1 125.1(6) . . ? C1 N2 C3 110.1(7) . . ? C1 N2 C6 125.0(7) . . ? C3 N2 C6 124.6(7) . . ? C4 C3 N2 106.8(7) . . ? C4 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? C3 C4 N5 107.8(7) . . ? C3 C4 H4A 126.1 . . ? N5 C4 H4A 126.1 . . ? C1 N5 C4 110.2(7) . . ? C1 N5 C18 123.5(6) . . ? C4 N5 C18 126.2(6) . . ? C7 C6 C11 123.0(8) . . ? C7 C6 N2 118.3(6) . . ? C11 C6 N2 118.7(7) . . ? C8 C7 C6 115.7(7) . . ? C8 C7 C12 122.5(8) . . ? C6 C7 C12 121.7(7) . . ? C7 C8 C9 122.3(8) . . ? C7 C8 H8A 118.8 . . ? C9 C8 H8A 118.8 . . ? C10 C9 C8 120.7(9) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 122.1(9) . . ? C9 C10 H10A 119.0 . . ? C11 C10 H10A 119.0 . . ? C6 C11 C10 116.1(8) . . ? C6 C11 C15 121.3(7) . . ? C10 C11 C15 122.4(8) . . ? C14 C12 C13 109.9(8) . . ? C14 C12 C7 110.2(7) . . ? C13 C12 C7 112.5(8) . . ? C14 C12 H12A 108.1 . . ? C13 C12 H12A 108.1 . . ? C7 C12 H12A 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 109.9(8) . . ? C16 C15 C17 110.3(8) . . ? C11 C15 C17 111.1(9) . . ? C16 C15 H15A 108.5 . . ? C11 C15 H15A 108.5 . . ? C17 C15 H15A 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.5(8) . . ? C19 C18 N5 117.9(7) . . ? C23 C18 N5 118.5(7) . . ? C18 C19 C20 116.4(8) . . ? C18 C19 C24 122.0(8) . . ? C20 C19 C24 121.3(8) . . ? C19 C20 C21 121.5(9) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C22 C21 C20 119.7(9) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 122.3(9) . . ? C21 C22 H22A 118.9 . . ? C23 C22 H22A 118.9 . . ? C22 C23 C18 116.4(8) . . ? C22 C23 C27 120.3(8) . . ? C18 C23 C27 122.9(8) . . ? C19 C24 C26 113.3(8) . . ? C19 C24 C25 109.4(7) . . ? C26 C24 C25 110.1(7) . . ? C19 C24 H24A 108.0 . . ? C26 C24 H24A 108.0 . . ? C25 C24 H24A 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 112.4(10) . . ? C29 C27 C28 109.8(8) . . ? C23 C27 C28 110.4(7) . . ? C29 C27 H27A 108.1 . . ? C23 C27 H27A 108.1 . . ? C28 C27 H27A 108.1 . . ? 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 . . ? C51 P30 C31 103.5(4) . . ? C51 P30 C41 105.2(4) . . ? C31 P30 C41 112.7(4) . . ? C51 P30 Pd1 111.8(3) . . ? C31 P30 Pd1 116.5(3) . . ? C41 P30 Pd1 106.6(2) . . ? C37 C31 C32 108.6(7) . . ? C37 C31 C36 108.6(7) . . ? C32 C31 C36 106.9(6) . . ? C37 C31 P30 106.0(5) . . ? C32 C31 P30 114.3(6) . . ? C36 C31 P30 112.3(5) . . ? C31 C32 C33 111.6(7) . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C39 C33 C32 108.6(7) . . ? C39 C33 C34 110.2(8) . . ? C32 C33 C34 107.8(7) . . ? C39 C33 H33A 110.1 . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? C35A C34 C33 109.5(7) . . ? C35A C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? C35A C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C40 C35A C36 112.1(7) . . ? C40 C35A C34 109.1(8) . . ? C36 C35A C34 107.8(7) . . ? C40 C35A H35A 109.3 . . ? C36 C35A H35A 109.3 . . ? C34 C35A H35A 109.3 . . ? C35A C36 C31 110.2(7) . . ? C35A C36 H36A 109.6 . . ? C31 C36 H36A 109.6 . . ? C35A C36 H36B 109.6 . . ? C31 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C31 C37 C38 110.9(7) . . ? C31 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C40 109.0(7) . . ? C39 C38 C37 109.2(7) . . ? C40 C38 C37 108.4(6) . . ? C39 C38 H38A 110.1 . . ? C40 C38 H38A 110.1 . . ? C37 C38 H38A 110.1 . . ? C33 C39 C38 111.8(8) . . ? C33 C39 H39A 109.3 . . ? C38 C39 H39A 109.3 . . ? C33 C39 H39B 109.3 . . ? C38 C39 H39B 109.3 . . ? H39A C39 H39B 107.9 . . ? C35A C40 C38 110.0(7) . . ? C35A C40 H40A 109.7 . . ? C38 C40 H40A 109.7 . . ? C35A C40 H40B 109.7 . . ? C38 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C46 C41 C50 109.3(7) . . ? C46 C41 C42 105.5(7) . . ? C50 C41 C42 109.4(6) . . ? C46 C41 P30 107.8(5) . . ? C50 C41 P30 110.0(6) . . ? C42 C41 P30 114.6(5) . . ? C43 C42 C41 110.2(6) . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C48 109.4(7) . . ? C42 C43 C44 110.6(8) . . ? C48 C43 C44 109.7(8) . . ? C42 C43 H43A 109.0 . . ? C48 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C45 C44 C43 109.0(7) . . ? C45 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? C45 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C49 C45 C44 108.5(7) . . ? C49 C45 C46 109.4(7) . . ? C44 C45 C46 108.9(7) . . ? C49 C45 H45A 110.0 . . ? C44 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? C41 C46 C45 111.5(7) . . ? C41 C46 H46A 109.3 . . ? C45 C46 H46A 109.3 . . ? C41 C46 H46B 109.3 . . ? C45 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? C49 C47 C50 108.9(7) . . ? C49 C47 C48 111.8(8) . . ? C50 C47 C48 109.7(8) . . ? C49 C47 H47A 108.8 . . ? C50 C47 H47A 108.8 . . ? C48 C47 H47A 108.8 . . ? C43 C48 C47 107.6(7) . . ? C43 C48 H48A 110.2 . . ? C47 C48 H48A 110.2 . . ? C43 C48 H48B 110.2 . . ? C47 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? C47 C49 C45 110.0(7) . . ? C47 C49 H49A 109.7 . . ? C45 C49 H49A 109.7 . . ? C47 C49 H49B 109.7 . . ? C45 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C47 C50 C41 110.7(7) . . ? C47 C50 H50A 109.5 . . ? C41 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? C41 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C52 C51 P30 115.8(6) . . ? C52 C51 H51A 108.3 . . ? P30 C51 H51A 108.3 . . ? C52 C51 H51B 108.3 . . ? P30 C51 H51B 108.3 . . ? H51A C51 H51B 107.4 . . ? C53 C52 C51 112.6(8) . . ? C53 C52 H52A 109.1 . . ? C51 C52 H52A 109.1 . . ? C53 C52 H52B 109.1 . . ? C51 C52 H52B 109.1 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C52 112.8(8) . . ? C54 C53 H53A 109.0 . . ? C52 C53 H53A 109.0 . . ? C54 C53 H53B 109.0 . . ? C52 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 Pd61 Cl62 88.1(2) . . ? C61 Pd61 Cl61 87.6(2) . . ? Cl62 Pd61 Cl61 173.20(7) . . ? C61 Pd61 P90 178.5(2) . . ? Cl62 Pd61 P90 91.43(7) . . ? Cl61 Pd61 P90 93.01(7) . . ? N62 C61 N65 105.8(6) . . ? N62 C61 Pd61 130.1(6) . . ? N65 C61 Pd61 124.0(5) . . ? C61 N62 C63 111.2(7) . . ? C61 N62 C66 123.5(6) . . ? C63 N62 C66 125.2(6) . . ? C64 C63 N62 107.2(7) . . ? C64 C63 H63A 126.4 . . ? N62 C63 H63A 126.4 . . ? C63 C64 N65 107.1(7) . . ? C63 C64 H64A 126.5 . . ? N65 C64 H64A 126.5 . . ? C61 N65 C64 108.8(6) . . ? C61 N65 C78 125.5(6) . . ? C64 N65 C78 125.0(6) . . ? C67 C66 N62 117.9(7) . . ? C67 C66 C71 122.8(8) . . ? N62 C66 C71 119.2(7) . . ? C66 C67 C68 117.0(8) . . ? C66 C67 C72 124.4(8) . . ? C68 C67 C72 118.6(8) . . ? C69 C68 C67 120.7(9) . . ? C69 C68 H68A 119.7 . . ? C67 C68 H68A 119.7 . . ? C68 C69 C70 119.7(8) . . ? C68 C69 H69A 120.2 . . ? C70 C69 H69A 120.2 . . ? C71 C70 C69 122.0(8) . . ? C71 C70 H70A 119.0 . . ? C69 C70 H70A 119.0 . . ? C70 C71 C66 117.5(8) . . ? C70 C71 C75 122.0(8) . . ? C66 C71 C75 120.3(7) . . ? C67 C72 C74 109.6(7) . . ? C67 C72 C73 115.0(8) . . ? C74 C72 C73 108.5(8) . . ? C67 C72 H72A 107.8 . . ? C74 C72 H72A 107.8 . . ? C73 C72 H72A 107.8 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C77 C75 C71 113.8(7) . . ? C77 C75 C76 111.0(7) . . ? C71 C75 C76 109.9(7) . . ? C77 C75 H75A 107.3 . . ? C71 C75 H75A 107.3 . . ? C76 C75 H75A 107.3 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C83 C78 C79 122.3(8) . . ? C83 C78 N65 118.7(7) . . ? C79 C78 N65 119.0(8) . . ? C80 C79 C78 118.4(8) . . ? C80 C79 C84 121.4(8) . . ? C78 C79 C84 119.9(8) . . ? C79 C80 C81 120.4(8) . . ? C79 C80 H80A 119.8 . . ? C81 C80 H80A 119.8 . . ? C80 C81 C82 120.3(9) . . ? C80 C81 H81A 119.9 . . ? C82 C81 H81A 119.9 . . ? C83 C82 C81 120.5(9) . . ? C83 C82 H82A 119.7 . . ? C81 C82 H82A 119.7 . . ? C78 C83 C82 117.8(7) . . ? C78 C83 C87 123.5(7) . . ? C82 C83 C87 118.6(8) . . ? C86 C84 C79 110.9(8) . . ? C86 C84 C85 109.6(8) . . ? C79 C84 C85 111.4(8) . . ? C86 C84 H84A 108.3 . . ? C79 C84 H84A 108.3 . . ? C85 C84 H84A 108.3 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C83 C87 C89 114.9(7) . . ? C83 C87 C88 110.3(6) . . ? C89 C87 C88 109.3(7) . . ? C83 C87 H87A 107.3 . . ? C89 C87 H87A 107.3 . . ? C88 C87 H87A 107.3 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C111 P90 C101 102.3(4) . . ? C111 P90 C91 104.7(4) . . ? C101 P90 C91 112.3(4) . . ? C111 P90 Pd61 111.7(3) . . ? C101 P90 Pd61 110.4(3) . . ? C91 P90 Pd61 114.5(2) . . ? C97 C91 C96 108.2(7) . . ? C97 C91 C92 107.9(6) . . ? C96 C91 C92 107.4(6) . . ? C97 C91 P90 107.9(5) . . ? C96 C91 P90 112.4(6) . . ? C92 C91 P90 112.9(6) . . ? C93 C92 C91 110.7(7) . . ? C93 C92 H92A 109.5 . . ? C91 C92 H92A 109.5 . . ? C93 C92 H92B 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 108.1 . . ? C92 C93 C99 109.8(7) . . ? C92 C93 C94 110.0(8) . . ? C99 C93 C94 108.1(9) . . ? C92 C93 H93A 109.6 . . ? C99 C93 H93A 109.6 . . ? C94 C93 H93A 109.6 . . ? C95 C94 C93 108.3(7) . . ? C95 C94 H94A 110.0 . . ? C93 C94 H94A 110.0 . . ? C95 C94 H94B 110.0 . . ? C93 C94 H94B 110.0 . . ? H94A C94 H94B 108.4 . . ? C96 C95 C94 111.3(8) . . ? C96 C95 C100 108.6(7) . . ? C94 C95 C100 110.2(8) . . ? C96 C95 H95A 108.9 . . ? C94 C95 H95A 108.9 . . ? C100 C95 H95A 108.9 . . ? C95 C96 C91 111.9(7) . . ? C95 C96 H96A 109.2 . . ? C91 C96 H96A 109.2 . . ? C95 C96 H96B 109.2 . . ? C91 C96 H96B 109.2 . . ? H96A C96 H96B 107.9 . . ? C91 C97 C98 111.0(7) . . ? C91 C97 H97A 109.4 . . ? C98 C97 H97A 109.4 . . ? C91 C97 H97B 109.4 . . ? C98 C97 H97B 109.4 . . ? H97A C97 H97B 108.0 . . ? C99 C98 C97 109.5(7) . . ? C99 C98 C100 109.1(8) . . ? C97 C98 C100 109.9(8) . . ? C99 C98 H98A 109.4 . . ? C97 C98 H98A 109.4 . . ? C100 C98 H98A 109.4 . . ? C98 C99 C93 110.3(7) . . ? C98 C99 H99A 109.6 . . ? C93 C99 H99A 109.6 . . ? C98 C99 H99B 109.6 . . ? C93 C99 H99B 109.6 . . ? H99A C99 H99B 108.1 . . ? C95 C100 C98 108.3(8) . . ? C95 C100 H10E 110.0 . . ? C98 C100 H10E 110.0 . . ? C95 C100 H10F 110.0 . . ? C98 C100 H10F 110.0 . . ? H10E C100 H10F 108.4 . . ? C102 C101 C106 109.8(8) . . ? C102 C101 C110 107.8(8) . . ? C106 C101 C110 105.1(7) . . ? C102 C101 P90 115.1(6) . . ? C106 C101 P90 110.3(5) . . ? C110 C101 P90 108.1(6) . . ? C103 C102 C101 109.5(8) . . ? C103 C102 H10G 109.8 . . ? C101 C102 H10G 109.8 . . ? C103 C102 H10H 109.8 . . ? C101 C102 H10H 109.8 . . ? H10G C102 H10H 108.2 . . ? C109 C103 C102 109.6(12) . . ? C109 C103 C104 108.7(11) . . ? C102 C103 C104 111.6(11) . . ? C109 C103 H10B 109.0 . . ? C102 C103 H10B 109.0 . . ? C104 C103 H10B 109.0 . . ? C105 C104 C103 108.7(10) . . ? C105 C104 H10I 110.0 . . ? C103 C104 H10I 110.0 . . ? C105 C104 H10J 110.0 . . ? C103 C104 H10J 110.0 . . ? H10I C104 H10J 108.3 . . ? C107 C105 C104 113.0(10) . . ? C107 C105 C106 108.8(9) . . ? C104 C105 C106 107.7(9) . . ? C107 C105 H10C 109.1 . . ? C104 C105 H10C 109.1 . . ? C106 C105 H10C 109.1 . . ? C101 C106 C105 111.4(7) . . ? C101 C106 H10K 109.4 . . ? C105 C106 H10K 109.4 . . ? C101 C106 H10L 109.4 . . ? C105 C106 H10L 109.4 . . ? H10K C106 H10L 108.0 . . ? C105 C107 C108 110.3(9) . . ? C105 C107 H10M 109.6 . . ? C108 C107 H10M 109.6 . . ? C105 C107 H10N 109.6 . . ? C108 C107 H10N 109.6 . . ? H10M C107 H10N 108.1 . . ? C107 C108 C110 110.4(9) . . ? C107 C108 C109 109.3(10) . . ? C110 C108 C109 107.4(9) . . ? C107 C108 H10D 109.9 . . ? C110 C108 H10D 109.9 . . ? C109 C108 H10D 109.9 . . ? C103 C109 C108 110.0(9) . . ? C103 C109 H10O 109.7 . . ? C108 C109 H10O 109.7 . . ? C103 C109 H10P 109.7 . . ? C108 C109 H10P 109.7 . . ? H10O C109 H10P 108.2 . . ? C108 C110 C101 111.1(8) . . ? C108 C110 H11J 109.4 . . ? C101 C110 H11J 109.4 . . ? C108 C110 H11K 109.4 . . ? C101 C110 H11K 109.4 . . ? H11J C110 H11K 108.0 . . ? C112 C111 P90 116.0(5) . . ? C112 C111 H11D 108.3 . . ? P90 C111 H11D 108.3 . . ? C112 C111 H11E 108.3 . . ? P90 C111 H11E 108.3 . . ? H11D C111 H11E 107.4 . . ? C113 C112 C111 110.9(7) . . ? C113 C112 H11F 109.5 . . ? C111 C112 H11F 109.5 . . ? C113 C112 H11G 109.5 . . ? C111 C112 H11G 109.5 . . ? H11F C112 H11G 108.0 . . ? C114 C113 C112 113.7(8) . . ? C114 C113 H11H 108.8 . . ? C112 C113 H11H 108.8 . . ? C114 C113 H11I 108.8 . . ? C112 C113 H11I 108.8 . . ? H11H C113 H11I 107.7 . . ? C113 C114 H11A 109.5 . . ? C113 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C113 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? Cl4 C201 C201 78(3) . 2_566 ? Cl4 C201 Cl5 152(3) . . ? C201 C201 Cl5 75(3) 2_566 . ? Cl4 C201 Cl5 23.4(8) . 2_566 ? C201 C201 Cl5 54(2) 2_566 2_566 ? Cl5 C201 Cl5 129(2) . 2_566 ? Cl4 C201 Cl4 127(2) . 2_566 ? C201 C201 Cl4 49(2) 2_566 2_566 ? Cl5 C201 Cl4 26.2(7) . 2_566 ? Cl5 C201 Cl4 103.2(18) 2_566 2_566 ? Cl5 Cl4 C201 113(2) 2_566 . ? Cl5 Cl4 C201 59.6(15) 2_566 2_566 ? C201 Cl4 C201 53(2) . 2_566 ? Cl4 Cl5 C201 94.2(17) 2_566 . ? Cl4 Cl5 C201 43.8(14) 2_566 2_566 ? C201 Cl5 C201 51(2) . 2_566 ? Cl7 C202 Cl6 120.2(12) . . ? Cl9 C203 Cl8 119.3(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pd1 C1 N5 -85.1(7) . . . . ? Cl1 Pd1 C1 N5 92.1(7) . . . . ? P30 Pd1 C1 N5 -71(5) . . . . ? Cl2 Pd1 C1 N2 95.9(6) . . . . ? Cl1 Pd1 C1 N2 -86.9(6) . . . . ? P30 Pd1 C1 N2 110(5) . . . . ? N5 C1 N2 C3 -0.2(8) . . . . ? Pd1 C1 N2 C3 179.0(5) . . . . ? N5 C1 N2 C6 174.0(7) . . . . ? Pd1 C1 N2 C6 -6.8(11) . . . . ? C1 N2 C3 C4 0.4(9) . . . . ? C6 N2 C3 C4 -173.8(7) . . . . ? N2 C3 C4 N5 -0.4(9) . . . . ? N2 C1 N5 C4 -0.1(8) . . . . ? Pd1 C1 N5 C4 -179.2(6) . . . . ? N2 C1 N5 C18 -176.5(7) . . . . ? Pd1 C1 N5 C18 4.4(11) . . . . ? C3 C4 N5 C1 0.3(9) . . . . ? C3 C4 N5 C18 176.6(7) . . . . ? C1 N2 C6 C7 92.9(9) . . . . ? C3 N2 C6 C7 -93.7(9) . . . . ? C1 N2 C6 C11 -85.9(10) . . . . ? C3 N2 C6 C11 87.4(10) . . . . ? C11 C6 C7 C8 2.4(12) . . . . ? N2 C6 C7 C8 -176.4(7) . . . . ? C11 C6 C7 C12 -175.1(7) . . . . ? N2 C6 C7 C12 6.1(11) . . . . ? C6 C7 C8 C9 -0.1(13) . . . . ? C12 C7 C8 C9 177.3(8) . . . . ? C7 C8 C9 C10 -3.3(15) . . . . ? C8 C9 C10 C11 4.5(16) . . . . ? C7 C6 C11 C10 -1.3(12) . . . . ? N2 C6 C11 C10 177.5(8) . . . . ? C7 C6 C11 C15 174.2(7) . . . . ? N2 C6 C11 C15 -7.0(12) . . . . ? C9 C10 C11 C6 -2.2(14) . . . . ? C9 C10 C11 C15 -177.7(9) . . . . ? C8 C7 C12 C14 -89.7(10) . . . . ? C6 C7 C12 C14 87.6(10) . . . . ? C8 C7 C12 C13 33.2(11) . . . . ? C6 C7 C12 C13 -149.5(8) . . . . ? C6 C11 C15 C16 -90.3(10) . . . . ? C10 C11 C15 C16 84.9(11) . . . . ? C6 C11 C15 C17 147.2(8) . . . . ? C10 C11 C15 C17 -37.5(12) . . . . ? C1 N5 C18 C19 -88.3(9) . . . . ? C4 N5 C18 C19 95.9(9) . . . . ? C1 N5 C18 C23 93.5(9) . . . . ? C4 N5 C18 C23 -82.3(10) . . . . ? C23 C18 C19 C20 -2.0(11) . . . . ? N5 C18 C19 C20 179.9(7) . . . . ? C23 C18 C19 C24 172.1(7) . . . . ? N5 C18 C19 C24 -6.0(11) . . . . ? C18 C19 C20 C21 -0.3(12) . . . . ? C24 C19 C20 C21 -174.5(8) . . . . ? C19 C20 C21 C22 3.4(13) . . . . ? C20 C21 C22 C23 -4.0(13) . . . . ? C21 C22 C23 C18 1.7(12) . . . . ? C21 C22 C23 C27 175.0(8) . . . . ? C19 C18 C23 C22 1.4(11) . . . . ? N5 C18 C23 C22 179.5(7) . . . . ? C19 C18 C23 C27 -171.6(7) . . . . ? N5 C18 C23 C27 6.5(11) . . . . ? C18 C19 C24 C26 149.8(7) . . . . ? C20 C19 C24 C26 -36.4(10) . . . . ? C18 C19 C24 C25 -86.9(9) . . . . ? C20 C19 C24 C25 86.9(9) . . . . ? C22 C23 C27 C29 43.9(11) . . . . ? C18 C23 C27 C29 -143.4(9) . . . . ? C22 C23 C27 C28 -79.1(11) . . . . ? C18 C23 C27 C28 93.7(10) . . . . ? C1 Pd1 P30 C51 -39(5) . . . . ? Cl2 Pd1 P30 C51 -24.2(3) . . . . ? Cl1 Pd1 P30 C51 158.7(3) . . . . ? C1 Pd1 P30 C31 -157(5) . . . . ? Cl2 Pd1 P30 C31 -142.9(3) . . . . ? Cl1 Pd1 P30 C31 40.0(3) . . . . ? C1 Pd1 P30 C41 76(5) . . . . ? Cl2 Pd1 P30 C41 90.2(3) . . . . ? Cl1 Pd1 P30 C41 -86.9(3) . . . . ? C51 P30 C31 C37 -83.9(5) . . . . ? C41 P30 C31 C37 163.0(5) . . . . ? Pd1 P30 C31 C37 39.3(5) . . . . ? C51 P30 C31 C32 35.7(7) . . . . ? C41 P30 C31 C32 -77.4(7) . . . . ? Pd1 P30 C31 C32 158.9(5) . . . . ? C51 P30 C31 C36 157.8(6) . . . . ? C41 P30 C31 C36 44.7(7) . . . . ? Pd1 P30 C31 C36 -79.1(6) . . . . ? C37 C31 C32 C33 -57.3(9) . . . . ? C36 C31 C32 C33 59.7(10) . . . . ? P30 C31 C32 C33 -175.4(6) . . . . ? C31 C32 C33 C39 59.0(9) . . . . ? C31 C32 C33 C34 -60.3(10) . . . . ? C39 C33 C34 C35A -57.5(10) . . . . ? C32 C33 C34 C35A 60.9(10) . . . . ? C33 C34 C35A C40 59.1(10) . . . . ? C33 C34 C35A C36 -62.8(10) . . . . ? C40 C35A C36 C31 -57.0(9) . . . . ? C34 C35A C36 C31 63.1(9) . . . . ? C37 C31 C36 C35A 56.3(8) . . . . ? C32 C31 C36 C35A -60.7(9) . . . . ? P30 C31 C36 C35A 173.1(6) . . . . ? C32 C31 C37 C38 56.3(8) . . . . ? C36 C31 C37 C38 -59.6(8) . . . . ? P30 C31 C37 C38 179.6(5) . . . . ? C31 C37 C38 C39 -57.5(9) . . . . ? C31 C37 C38 C40 61.2(9) . . . . ? C32 C33 C39 C38 -60.1(9) . . . . ? C34 C33 C39 C38 57.7(9) . . . . ? C40 C38 C39 C33 -58.4(10) . . . . ? C37 C38 C39 C33 59.9(9) . . . . ? C36 C35A C40 C38 58.5(9) . . . . ? C34 C35A C40 C38 -60.8(9) . . . . ? C39 C38 C40 C35A 59.6(9) . . . . ? C37 C38 C40 C35A -59.2(9) . . . . ? C51 P30 C41 C46 49.7(6) . . . . ? C31 P30 C41 C46 161.7(5) . . . . ? Pd1 P30 C41 C46 -69.2(5) . . . . ? C51 P30 C41 C50 168.8(5) . . . . ? C31 P30 C41 C50 -79.2(6) . . . . ? Pd1 P30 C41 C50 49.9(6) . . . . ? C51 P30 C41 C42 -67.5(6) . . . . ? C31 P30 C41 C42 44.6(7) . . . . ? Pd1 P30 C41 C42 173.7(5) . . . . ? C46 C41 C42 C43 60.9(8) . . . . ? C50 C41 C42 C43 -56.6(9) . . . . ? P30 C41 C42 C43 179.3(6) . . . . ? C41 C42 C43 C48 59.6(10) . . . . ? C41 C42 C43 C44 -61.4(9) . . . . ? C42 C43 C44 C45 59.0(9) . . . . ? C48 C43 C44 C45 -61.8(9) . . . . ? C43 C44 C45 C49 61.3(9) . . . . ? C43 C44 C45 C46 -57.8(9) . . . . ? C50 C41 C46 C45 56.1(9) . . . . ? C42 C41 C46 C45 -61.5(8) . . . . ? P30 C41 C46 C45 175.6(5) . . . . ? C49 C45 C46 C41 -56.5(9) . . . . ? C44 C45 C46 C41 62.0(9) . . . . ? C42 C43 C48 C47 -62.5(10) . . . . ? C44 C43 C48 C47 59.1(10) . . . . ? C49 C47 C48 C43 -58.4(10) . . . . ? C50 C47 C48 C43 62.5(10) . . . . ? C50 C47 C49 C45 -61.3(9) . . . . ? C48 C47 C49 C45 60.1(10) . . . . ? C44 C45 C49 C47 -60.0(9) . . . . ? C46 C45 C49 C47 58.8(9) . . . . ? C49 C47 C50 C41 61.4(9) . . . . ? C48 C47 C50 C41 -61.2(9) . . . . ? C46 C41 C50 C47 -58.4(9) . . . . ? C42 C41 C50 C47 56.6(9) . . . . ? P30 C41 C50 C47 -176.7(6) . . . . ? C31 P30 C51 C52 67.1(7) . . . . ? C41 P30 C51 C52 -174.4(6) . . . . ? Pd1 P30 C51 C52 -59.1(6) . . . . ? P30 C51 C52 C53 156.5(6) . . . . ? C51 C52 C53 C54 64.6(11) . . . . ? Cl62 Pd61 C61 N62 -75.4(7) . . . . ? Cl61 Pd61 C61 N62 99.3(7) . . . . ? P90 Pd61 C61 N62 -145(9) . . . . ? Cl62 Pd61 C61 N65 108.4(6) . . . . ? Cl61 Pd61 C61 N65 -76.9(6) . . . . ? P90 Pd61 C61 N65 39(10) . . . . ? N65 C61 N62 C63 -0.2(8) . . . . ? Pd61 C61 N62 C63 -176.9(5) . . . . ? N65 C61 N62 C66 -177.3(6) . . . . ? Pd61 C61 N62 C66 5.9(10) . . . . ? C61 N62 C63 C64 -0.6(8) . . . . ? C66 N62 C63 C64 176.5(7) . . . . ? N62 C63 C64 N65 1.2(8) . . . . ? N62 C61 N65 C64 0.9(8) . . . . ? Pd61 C61 N65 C64 177.9(5) . . . . ? N62 C61 N65 C78 171.3(7) . . . . ? Pd61 C61 N65 C78 -11.8(10) . . . . ? C63 C64 N65 C61 -1.3(8) . . . . ? C63 C64 N65 C78 -171.7(7) . . . . ? C61 N62 C66 C67 97.3(9) . . . . ? C63 N62 C66 C67 -79.4(9) . . . . ? C61 N62 C66 C71 -81.6(9) . . . . ? C63 N62 C66 C71 101.6(8) . . . . ? N62 C66 C67 C68 -173.1(7) . . . . ? C71 C66 C67 C68 5.8(11) . . . . ? N62 C66 C67 C72 8.8(11) . . . . ? C71 C66 C67 C72 -172.3(7) . . . . ? C66 C67 C68 C69 -1.1(12) . . . . ? C72 C67 C68 C69 177.1(8) . . . . ? C67 C68 C69 C70 -3.7(13) . . . . ? C68 C69 C70 C71 4.0(13) . . . . ? C69 C70 C71 C66 0.5(12) . . . . ? C69 C70 C71 C75 -174.9(7) . . . . ? C67 C66 C71 C70 -5.6(11) . . . . ? N62 C66 C71 C70 173.3(7) . . . . ? C67 C66 C71 C75 169.9(7) . . . . ? N62 C66 C71 C75 -11.2(10) . . . . ? C66 C67 C72 C74 94.1(11) . . . . ? C68 C67 C72 C74 -84.0(10) . . . . ? C66 C67 C72 C73 -143.4(9) . . . . ? C68 C67 C72 C73 38.6(11) . . . . ? C70 C71 C75 C77 -27.3(11) . . . . ? C66 C71 C75 C77 157.5(7) . . . . ? C70 C71 C75 C76 97.8(9) . . . . ? C66 C71 C75 C76 -77.4(9) . . . . ? C61 N65 C78 C83 101.4(9) . . . . ? C64 N65 C78 C83 -89.7(9) . . . . ? C61 N65 C78 C79 -78.5(9) . . . . ? C64 N65 C78 C79 90.4(9) . . . . ? C83 C78 C79 C80 -3.2(12) . . . . ? N65 C78 C79 C80 176.6(7) . . . . ? C83 C78 C79 C84 171.0(7) . . . . ? N65 C78 C79 C84 -9.1(11) . . . . ? C78 C79 C80 C81 -0.8(12) . . . . ? C84 C79 C80 C81 -175.0(8) . . . . ? C79 C80 C81 C82 3.9(14) . . . . ? C80 C81 C82 C83 -3.1(13) . . . . ? C79 C78 C83 C82 4.0(11) . . . . ? N65 C78 C83 C82 -175.9(7) . . . . ? C79 C78 C83 C87 -172.7(7) . . . . ? N65 C78 C83 C87 7.4(11) . . . . ? C81 C82 C83 C78 -0.8(12) . . . . ? C81 C82 C83 C87 176.1(7) . . . . ? C80 C79 C84 C86 82.8(10) . . . . ? C78 C79 C84 C86 -91.3(10) . . . . ? C80 C79 C84 C85 -39.6(11) . . . . ? C78 C79 C84 C85 146.3(8) . . . . ? C78 C83 C87 C89 -146.5(8) . . . . ? C82 C83 C87 C89 36.8(10) . . . . ? C78 C83 C87 C88 89.4(9) . . . . ? C82 C83 C87 C88 -87.3(9) . . . . ? C61 Pd61 P90 C111 48(9) . . . . ? Cl62 Pd61 P90 C111 -21.4(3) . . . . ? Cl61 Pd61 P90 C111 163.8(3) . . . . ? C61 Pd61 P90 C101 162(9) . . . . ? Cl62 Pd61 P90 C101 91.8(3) . . . . ? Cl61 Pd61 P90 C101 -83.0(3) . . . . ? C61 Pd61 P90 C91 -71(9) . . . . ? Cl62 Pd61 P90 C91 -140.2(3) . . . . ? Cl61 Pd61 P90 C91 44.9(3) . . . . ? C111 P90 C91 C97 -87.3(6) . . . . ? C101 P90 C91 C97 162.4(5) . . . . ? Pd61 P90 C91 C97 35.4(6) . . . . ? C111 P90 C91 C96 31.9(6) . . . . ? C101 P90 C91 C96 -78.4(6) . . . . ? Pd61 P90 C91 C96 154.6(5) . . . . ? C111 P90 C91 C92 153.5(5) . . . . ? C101 P90 C91 C92 43.3(6) . . . . ? Pd61 P90 C91 C92 -83.7(6) . . . . ? C97 C91 C92 C93 58.6(8) . . . . ? C96 C91 C92 C93 -57.8(9) . . . . ? P90 C91 C92 C93 177.7(6) . . . . ? C91 C92 C93 C99 -58.9(10) . . . . ? C91 C92 C93 C94 59.9(9) . . . . ? C92 C93 C94 C95 -59.2(10) . . . . ? C99 C93 C94 C95 60.7(10) . . . . ? C93 C94 C95 C96 58.9(10) . . . . ? C93 C94 C95 C100 -61.6(10) . . . . ? C94 C95 C96 C91 -60.4(10) . . . . ? C100 C95 C96 C91 61.0(10) . . . . ? C97 C91 C96 C95 -58.9(9) . . . . ? C92 C91 C96 C95 57.4(9) . . . . ? P90 C91 C96 C95 -177.9(6) . . . . ? C96 C91 C97 C98 57.1(9) . . . . ? C92 C91 C97 C98 -58.8(9) . . . . ? P90 C91 C97 C98 178.9(6) . . . . ? C91 C97 C98 C99 60.1(9) . . . . ? C91 C97 C98 C100 -59.8(9) . . . . ? C97 C98 C99 C93 -58.8(10) . . . . ? C100 C98 C99 C93 61.5(10) . . . . ? C92 C93 C99 C98 59.0(11) . . . . ? C94 C93 C99 C98 -61.0(9) . . . . ? C96 C95 C100 C98 -60.5(10) . . . . ? C94 C95 C100 C98 61.6(10) . . . . ? C99 C98 C100 C95 -59.9(10) . . . . ? C97 C98 C100 C95 60.2(10) . . . . ? C111 P90 C101 C102 -67.3(8) . . . . ? C91 P90 C101 C102 44.5(8) . . . . ? Pd61 P90 C101 C102 173.7(6) . . . . ? C111 P90 C101 C106 167.8(6) . . . . ? C91 P90 C101 C106 -80.5(7) . . . . ? Pd61 P90 C101 C106 48.7(7) . . . . ? C111 P90 C101 C110 53.3(7) . . . . ? C91 P90 C101 C110 165.1(6) . . . . ? Pd61 P90 C101 C110 -65.8(6) . . . . ? C106 C101 C102 C103 -54.8(12) . . . . ? C110 C101 C102 C103 59.1(12) . . . . ? P90 C101 C102 C103 179.9(9) . . . . ? C101 C102 C103 C109 -61.4(12) . . . . ? C101 C102 C103 C104 59.1(15) . . . . ? C109 C103 C104 C105 58.0(13) . . . . ? C102 C103 C104 C105 -63.0(16) . . . . ? C103 C104 C105 C107 -58.9(13) . . . . ? C103 C104 C105 C106 61.4(14) . . . . ? C102 C101 C106 C105 56.8(11) . . . . ? C110 C101 C106 C105 -58.9(10) . . . . ? P90 C101 C106 C105 -175.3(7) . . . . ? C107 C105 C106 C101 63.0(11) . . . . ? C104 C105 C106 C101 -59.9(12) . . . . ? C104 C105 C107 C108 58.5(12) . . . . ? C106 C105 C107 C108 -61.1(11) . . . . ? C105 C107 C108 C110 60.4(13) . . . . ? C105 C107 C108 C109 -57.4(11) . . . . ? C102 C103 C109 C108 62.2(12) . . . . ? C104 C103 C109 C108 -60.0(12) . . . . ? C107 C108 C109 C103 59.1(12) . . . . ? C110 C108 C109 C103 -60.7(12) . . . . ? C107 C108 C110 C101 -58.9(13) . . . . ? C109 C108 C110 C101 60.2(11) . . . . ? C102 C101 C110 C108 -60.0(11) . . . . ? C106 C101 C110 C108 57.1(10) . . . . ? P90 C101 C110 C108 174.9(7) . . . . ? C101 P90 C111 C112 -178.3(6) . . . . ? C91 P90 C111 C112 64.4(6) . . . . ? Pd61 P90 C111 C112 -60.2(6) . . . . ? P90 C111 C112 C113 163.3(6) . . . . ? C111 C112 C113 C114 177.2(8) . . . . ? C201 C201 Cl4 Cl5 6(4) 2_566 . . 2_566 ? Cl5 C201 Cl4 Cl5 11(8) . . . 2_566 ? Cl4 C201 Cl4 Cl5 6(4) 2_566 . . 2_566 ? Cl5 C201 Cl4 C201 6(4) . . . 2_566 ? Cl5 C201 Cl4 C201 -6(4) 2_566 . . 2_566 ? Cl4 C201 Cl4 C201 0.000(6) 2_566 . . 2_566 ? Cl4 C201 Cl5 Cl4 -11(7) . . . 2_566 ? C201 C201 Cl5 Cl4 -5(3) 2_566 . . 2_566 ? Cl5 C201 Cl5 Cl4 -5(3) 2_566 . . 2_566 ? Cl4 C201 Cl5 C201 -6(4) . . . 2_566 ? Cl5 C201 Cl5 C201 0.000(6) 2_566 . . 2_566 ? Cl4 C201 Cl5 C201 5(3) 2_566 . . 2_566 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.829 _refine_diff_density_min -2.955 _refine_diff_density_rms 0.337 data_2f _database_code_depnum_ccdc_archive 'CCDC 871887' #TrackingRef '10175_web_deposit_cif_file_5_CatherineS.J.Cazin_1331897901.2f.cif' # start Validation Reply Form _vrf_PLAT971_2f ; PROBLEM: Large Calcd. Non-Metal Positive Residual Density 3.98 eA-3 RESPONSE: Near the partial weight disordered solvent. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H85 Cl2 N2 P Pd,1.5(C H2 Cl2)' _chemical_formula_sum 'C61.50 H88 Cl5 N2 P Pd' _chemical_formula_weight 1169.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.320(3) _cell_length_b 12.759(2) _cell_length_c 21.547(5) _cell_angle_alpha 103.505(8) _cell_angle_beta 104.578(7) _cell_angle_gamma 93.875(9) _cell_volume 3158.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8336 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1234 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32216 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.39 _reflns_number_total 11488 _reflns_number_gt 9811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1520P)^2^+9.6603P] 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 11488 _refine_ls_number_parameters 639 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2344 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.64254(3) 0.69189(3) 0.766083(17) 0.02333(17) Uani 1 1 d . . . Cl1 Cl 0.75455(12) 0.57173(11) 0.80737(7) 0.0342(3) Uani 1 1 d . . . Cl2 Cl 0.53187(11) 0.81448(10) 0.72802(6) 0.0288(3) Uani 1 1 d . . . C1 C 0.5459(4) 0.6837(4) 0.8303(2) 0.0242(10) Uani 1 1 d . . . N2 N 0.4649(4) 0.6030(3) 0.8254(2) 0.0275(9) Uani 1 1 d . . . C3 C 0.4148(5) 0.6305(4) 0.8761(3) 0.0347(12) Uani 1 1 d . . . H3A H 0.3555 0.5873 0.8832 0.042 Uiso 1 1 calc R . . C4 C 0.4650(5) 0.7293(4) 0.9137(3) 0.0321(12) Uani 1 1 d . . . H4A H 0.4485 0.7695 0.9525 0.039 Uiso 1 1 calc R . . N5 N 0.5464(4) 0.7616(3) 0.8847(2) 0.0278(9) Uani 1 1 d . . . C6 C 0.4403(4) 0.4970(4) 0.7779(3) 0.0294(11) Uani 1 1 d . . . C7 C 0.4850(5) 0.4097(4) 0.8001(3) 0.0328(12) Uani 1 1 d . . . C8 C 0.4587(5) 0.3077(5) 0.7547(3) 0.0394(13) Uani 1 1 d . . . H8A H 0.4862 0.2464 0.7681 0.047 Uiso 1 1 calc R . . C9 C 0.3931(6) 0.2948(5) 0.6906(3) 0.0452(15) Uani 1 1 d . . . H9A H 0.3769 0.2249 0.6602 0.054 Uiso 1 1 calc R . . C10 C 0.3508(5) 0.3820(5) 0.6700(3) 0.0404(14) Uani 1 1 d . . . H10A H 0.3064 0.3712 0.6254 0.048 Uiso 1 1 calc R . . C11 C 0.3717(5) 0.4859(4) 0.7131(3) 0.0329(12) Uani 1 1 d . . . C12 C 0.5554(6) 0.4222(5) 0.8710(3) 0.0413(14) Uani 1 1 d . . . H12A H 0.5831 0.5013 0.8914 0.050 Uiso 1 1 calc R . . C13 C 0.4833(7) 0.3845(6) 0.9118(4) 0.0562(19) Uani 1 1 d . . . H13A H 0.4176 0.4242 0.9097 0.084 Uiso 1 1 calc R . . H13B H 0.5285 0.3988 0.9581 0.084 Uiso 1 1 calc R . . H13C H 0.4574 0.3063 0.8939 0.084 Uiso 1 1 calc R . . C14 C 0.6594(6) 0.3613(5) 0.8744(4) 0.0537(18) Uani 1 1 d . . . H14A H 0.7059 0.3870 0.8488 0.081 Uiso 1 1 calc R . . H14B H 0.6345 0.2831 0.8559 0.081 Uiso 1 1 calc R . . H14C H 0.7040 0.3751 0.9208 0.081 Uiso 1 1 calc R . . C15 C 0.3215(5) 0.5811(5) 0.6920(3) 0.0426(15) Uani 1 1 d . . . H15A H 0.3804 0.6464 0.7121 0.051 Uiso 1 1 calc R . . C16 C 0.2191(6) 0.6052(6) 0.7187(4) 0.0574(19) Uani 1 1 d . . . H16A H 0.2411 0.6156 0.7670 0.086 Uiso 1 1 calc R . . H16B H 0.1582 0.5441 0.6980 0.086 Uiso 1 1 calc R . . H16C H 0.1925 0.6715 0.7083 0.086 Uiso 1 1 calc R . . C17 C 0.2878(6) 0.5647(7) 0.6167(4) 0.059(2) Uani 1 1 d . . . H17A H 0.3537 0.5500 0.5999 0.088 Uiso 1 1 calc R . . H17B H 0.2607 0.6307 0.6061 0.088 Uiso 1 1 calc R . . H17C H 0.2275 0.5031 0.5958 0.088 Uiso 1 1 calc R . . C18 C 0.6234(4) 0.8626(4) 0.9106(2) 0.0277(11) Uani 1 1 d . . . C19 C 0.5825(4) 0.9580(4) 0.8998(3) 0.0290(11) Uani 1 1 d . . . C20 C 0.6603(5) 1.0538(5) 0.9234(3) 0.0373(13) Uani 1 1 d . . . H20A H 0.6360 1.1204 0.9167 0.045 Uiso 1 1 calc R . . C21 C 0.7705(5) 1.0520(5) 0.9558(3) 0.0420(14) Uani 1 1 d . . . H21A H 0.8222 1.1173 0.9710 0.050 Uiso 1 1 calc R . . C22 C 0.8075(5) 0.9571(5) 0.9668(3) 0.0371(13) Uani 1 1 d . . . H22A H 0.8845 0.9582 0.9896 0.045 Uiso 1 1 calc R . . C23 C 0.7347(5) 0.8590(5) 0.9454(3) 0.0322(12) Uani 1 1 d . . . C24 C 0.4578(5) 0.9617(4) 0.8663(3) 0.0326(12) Uani 1 1 d . . . H24A H 0.4237 0.8867 0.8386 0.039 Uiso 1 1 calc R . . C25 C 0.3935(6) 0.9945(6) 0.9180(3) 0.0467(15) Uani 1 1 d . . . H25A H 0.4029 0.9450 0.9470 0.070 Uiso 1 1 calc R . . H25B H 0.3129 0.9906 0.8956 0.070 Uiso 1 1 calc R . . H25C H 0.4231 1.0691 0.9446 0.070 Uiso 1 1 calc R . . C26 C 0.4422(6) 1.0385(5) 0.8209(3) 0.0469(16) Uani 1 1 d . . . H26A H 0.4835 1.0174 0.7875 0.070 Uiso 1 1 calc R . . H26B H 0.4717 1.1132 0.8474 0.070 Uiso 1 1 calc R . . H26C H 0.3616 1.0342 0.7987 0.070 Uiso 1 1 calc R . . C27 C 0.7737(5) 0.7565(5) 0.9631(3) 0.0357(13) Uani 1 1 d . . . H27A H 0.7314 0.6930 0.9259 0.043 Uiso 1 1 calc R . . C28 C 0.7426(7) 0.7452(6) 1.0263(3) 0.0526(17) Uani 1 1 d . . . H28A H 0.6615 0.7488 1.0203 0.079 Uiso 1 1 calc R . . H28B H 0.7861 0.8044 1.0642 0.079 Uiso 1 1 calc R . . H28C H 0.7603 0.6752 1.0347 0.079 Uiso 1 1 calc R . . C29 C 0.8995(6) 0.7504(6) 0.9721(4) 0.0527(17) Uani 1 1 d . . . H29A H 0.9191 0.7573 0.9318 0.079 Uiso 1 1 calc R . . H29B H 0.9171 0.6805 0.9806 0.079 Uiso 1 1 calc R . . H29C H 0.9434 0.8097 1.0098 0.079 Uiso 1 1 calc R . . P1 P 0.75380(11) 0.70660(10) 0.69535(6) 0.0231(3) Uani 1 1 d . . . C31 C 0.8837(4) 0.8025(4) 0.7405(2) 0.0267(11) Uani 1 1 d . . . H31A H 0.9085 0.8368 0.7083 0.032 Uiso 1 1 calc R . . C32 C 0.8547(5) 0.8924(4) 0.7928(3) 0.0315(12) Uani 1 1 d . . . H32A H 0.7911 0.9264 0.7708 0.038 Uiso 1 1 calc R . . H32B H 0.8302 0.8599 0.8254 0.038 Uiso 1 1 calc R . . C33 C 0.9575(5) 0.9799(5) 0.8292(3) 0.0389(13) Uani 1 1 d . . . H33A H 0.9783 1.0164 0.7973 0.047 Uiso 1 1 calc R . . H33B H 0.9378 1.0354 0.8636 0.047 Uiso 1 1 calc R . . C34 C 1.0576(5) 0.9293(5) 0.8615(3) 0.0425(14) Uani 1 1 d . . . H34A H 1.0400 0.9010 0.8974 0.051 Uiso 1 1 calc R . . H34B H 1.1244 0.9858 0.8816 0.051 Uiso 1 1 calc R . . C35 C 1.0856(5) 0.8370(5) 0.8114(3) 0.0446(15) Uani 1 1 d . . . H35A H 1.1477 0.8031 0.8348 0.054 Uiso 1 1 calc R . . H35B H 1.1123 0.8670 0.7786 0.054 Uiso 1 1 calc R . . C36 C 0.9829(4) 0.7499(4) 0.7749(3) 0.0334(12) Uani 1 1 d . . . H36A H 0.9600 0.7148 0.8068 0.040 Uiso 1 1 calc R . . H36B H 1.0032 0.6932 0.7413 0.040 Uiso 1 1 calc R . . C37 C 0.8014(4) 0.5759(4) 0.6623(2) 0.0272(11) Uani 1 1 d . . . H37A H 0.8569 0.5606 0.7007 0.033 Uiso 1 1 calc R . . C38 C 0.8657(5) 0.5802(4) 0.6103(3) 0.0324(12) Uani 1 1 d . . . H38A H 0.9264 0.6431 0.6279 0.039 Uiso 1 1 calc R . . H38B H 0.8132 0.5904 0.5697 0.039 Uiso 1 1 calc R . . C39 C 0.9180(5) 0.4745(5) 0.5927(3) 0.0382(13) Uani 1 1 d . . . H39A H 0.9555 0.4773 0.5574 0.046 Uiso 1 1 calc R . . H39B H 0.9762 0.4681 0.6323 0.046 Uiso 1 1 calc R . . C40 C 0.8277(5) 0.3756(5) 0.5690(3) 0.0389(13) Uani 1 1 d . . . H40A H 0.8641 0.3086 0.5622 0.047 Uiso 1 1 calc R . . H40B H 0.7758 0.3767 0.5259 0.047 Uiso 1 1 calc R . . C41 C 0.7598(5) 0.3740(4) 0.6195(3) 0.0372(13) Uani 1 1 d . . . H41A H 0.6988 0.3114 0.6014 0.045 Uiso 1 1 calc R . . H41B H 0.8102 0.3638 0.6608 0.045 Uiso 1 1 calc R . . C42 C 0.7075(5) 0.4789(4) 0.6361(3) 0.0327(12) Uani 1 1 d . . . H42A H 0.6523 0.4869 0.5958 0.039 Uiso 1 1 calc R . . H42B H 0.6670 0.4760 0.6701 0.039 Uiso 1 1 calc R . . C43 C 0.6808(4) 0.7456(4) 0.6204(2) 0.0264(11) Uani 1 1 d . . . C44 C 0.7126(4) 0.8254(4) 0.5898(3) 0.0280(11) Uani 1 1 d . . . C45 C 0.6431(5) 0.8250(5) 0.5267(3) 0.0364(13) Uani 1 1 d . . . H45A H 0.6634 0.8778 0.5055 0.044 Uiso 1 1 calc R . . C46 C 0.5469(5) 0.7510(5) 0.4945(3) 0.0384(13) Uani 1 1 d . . . H46A H 0.5043 0.7511 0.4511 0.046 Uiso 1 1 calc R . . C47 C 0.5127(5) 0.6766(4) 0.5257(3) 0.0331(12) Uani 1 1 d . . . H47A H 0.4452 0.6269 0.5047 0.040 Uiso 1 1 calc R . . C48 C 0.5784(4) 0.6758(4) 0.5878(3) 0.0282(11) Uani 1 1 d . . . H48A H 0.5535 0.6260 0.6095 0.034 Uiso 1 1 calc R . . C49 C 0.8107(5) 0.9162(4) 0.6190(3) 0.0293(11) Uani 1 1 d . . . C50 C 0.7982(4) 1.0143(4) 0.6617(3) 0.0300(11) Uani 1 1 d . . . C51 C 0.8901(5) 1.0975(4) 0.6853(3) 0.0329(12) Uani 1 1 d . . . H51A H 0.8832 1.1641 0.7140 0.039 Uiso 1 1 calc R . . C52 C 0.9910(5) 1.0863(4) 0.6683(3) 0.0314(12) Uani 1 1 d . . . C53 C 0.9980(5) 0.9917(4) 0.6242(3) 0.0302(11) Uani 1 1 d . . . H53A H 1.0656 0.9842 0.6109 0.036 Uiso 1 1 calc R . . C54 C 0.9094(5) 0.9065(4) 0.5983(3) 0.0286(11) Uani 1 1 d . . . C55 C 0.6876(5) 1.0335(4) 0.6796(3) 0.0358(13) Uani 1 1 d . . . H55A H 0.6507 0.9622 0.6811 0.043 Uiso 1 1 calc R . . C56 C 0.7043(6) 1.1133(5) 0.7464(3) 0.0441(15) Uani 1 1 d . . . H56A H 0.7557 1.0878 0.7809 0.066 Uiso 1 1 calc R . . H56B H 0.6312 1.1188 0.7563 0.066 Uiso 1 1 calc R . . H56C H 0.7370 1.1849 0.7454 0.066 Uiso 1 1 calc R . . C57 C 0.6077(5) 1.0732(5) 0.6259(4) 0.0474(16) Uani 1 1 d . . . H57A H 0.5369 1.0850 0.6377 0.071 Uiso 1 1 calc R . . H57B H 0.5916 1.0185 0.5832 0.071 Uiso 1 1 calc R . . H57C H 0.6434 1.1417 0.6222 0.071 Uiso 1 1 calc R . . C58 C 1.0939(5) 1.1743(5) 0.6991(3) 0.0374(13) Uani 1 1 d . . . H58A H 1.1470 1.1591 0.6708 0.045 Uiso 1 1 calc R . . C59 C 1.1566(6) 1.1667(6) 0.7687(4) 0.0549(18) Uani 1 1 d . . . H59A H 1.2225 1.2231 0.7874 0.082 Uiso 1 1 calc R . . H59B H 1.1818 1.0949 0.7659 0.082 Uiso 1 1 calc R . . H59C H 1.1057 1.1772 0.7973 0.082 Uiso 1 1 calc R . . C60 C 1.0654(5) 1.2888(5) 0.7003(4) 0.0450(15) Uani 1 1 d . . . H60A H 1.0262 1.2919 0.6553 0.068 Uiso 1 1 calc R . . H60B H 1.1353 1.3403 0.7170 0.068 Uiso 1 1 calc R . . H60C H 1.0162 1.3080 0.7295 0.068 Uiso 1 1 calc R . . C61 C 0.9235(5) 0.8058(4) 0.5473(3) 0.0343(12) Uani 1 1 d . . . H61A H 0.8639 0.7456 0.5435 0.041 Uiso 1 1 calc R . . C62 C 1.0397(6) 0.7672(5) 0.5688(4) 0.0464(15) Uani 1 1 d . . . H62A H 1.0498 0.7524 0.6124 0.070 Uiso 1 1 calc R . . H62B H 1.0996 0.8240 0.5715 0.070 Uiso 1 1 calc R . . H62C H 1.0436 0.7007 0.5362 0.070 Uiso 1 1 calc R . . C63 C 0.9058(7) 0.8282(6) 0.4790(3) 0.0506(17) Uani 1 1 d . . . H63A H 0.8316 0.8525 0.4659 0.076 Uiso 1 1 calc R . . H63B H 0.9091 0.7615 0.4464 0.076 Uiso 1 1 calc R . . H63C H 0.9652 0.8850 0.4810 0.076 Uiso 1 1 calc R . . C71 C 0.3534(6) 0.8818(6) 0.5899(4) 0.0503(16) Uani 1 1 d . . . H71A H 0.4367 0.8868 0.5992 0.060 Uiso 1 1 calc R . . H71B H 0.3240 0.8080 0.5906 0.060 Uiso 1 1 calc R . . Cl3 Cl 0.31888(16) 0.97853(17) 0.65179(9) 0.0628(5) Uani 1 1 d . . . Cl4 Cl 0.2969(2) 0.90168(15) 0.51232(9) 0.0675(6) Uani 1 1 d . . . C72 C 1.057(3) 0.4930(15) 0.8687(5) 0.170(17) Uani 0.50 1 d PD . . H72A H 1.1057 0.4623 0.8407 0.204 Uiso 0.50 1 calc PR . . H72B H 0.9987 0.5235 0.8399 0.204 Uiso 0.50 1 calc PR . . Cl5 Cl 0.9819(5) 0.3771(5) 0.8781(3) 0.1056(17) Uiso 0.50 1 d PD . . Cl6 Cl 1.1437(6) 0.6091(5) 0.9262(3) 0.1113(19) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0239(3) 0.0226(2) 0.0238(2) 0.00583(17) 0.00729(17) 0.00281(16) Cl1 0.0397(8) 0.0382(7) 0.0339(7) 0.0180(6) 0.0155(6) 0.0177(6) Cl2 0.0308(7) 0.0275(6) 0.0330(7) 0.0118(5) 0.0124(5) 0.0094(5) C1 0.025(2) 0.018(2) 0.025(2) 0.0018(19) 0.003(2) 0.0040(19) N2 0.028(2) 0.023(2) 0.033(2) 0.0057(18) 0.0138(19) 0.0013(17) C3 0.040(3) 0.030(3) 0.040(3) 0.006(2) 0.025(3) 0.000(2) C4 0.033(3) 0.032(3) 0.034(3) 0.004(2) 0.019(2) 0.002(2) N5 0.028(2) 0.025(2) 0.031(2) 0.0055(18) 0.0107(19) 0.0034(17) C6 0.029(3) 0.026(3) 0.035(3) 0.006(2) 0.014(2) 0.001(2) C7 0.035(3) 0.028(3) 0.038(3) 0.009(2) 0.016(2) 0.001(2) C8 0.049(4) 0.026(3) 0.044(3) 0.006(2) 0.018(3) 0.006(2) C9 0.054(4) 0.031(3) 0.044(3) -0.006(3) 0.017(3) 0.003(3) C10 0.039(3) 0.042(3) 0.034(3) 0.003(3) 0.009(3) -0.003(3) C11 0.026(3) 0.032(3) 0.038(3) 0.007(2) 0.009(2) -0.003(2) C12 0.056(4) 0.029(3) 0.037(3) 0.011(2) 0.009(3) 0.003(3) C13 0.087(6) 0.044(4) 0.050(4) 0.020(3) 0.032(4) 0.013(4) C14 0.065(5) 0.041(4) 0.057(4) 0.025(3) 0.009(3) 0.011(3) C15 0.031(3) 0.040(3) 0.052(4) 0.015(3) 0.002(3) -0.003(2) C16 0.041(4) 0.057(4) 0.071(5) 0.016(4) 0.008(3) 0.018(3) C17 0.048(4) 0.072(5) 0.056(4) 0.034(4) 0.000(3) 0.002(3) C18 0.030(3) 0.028(3) 0.024(2) 0.002(2) 0.012(2) -0.002(2) C19 0.030(3) 0.030(3) 0.026(3) 0.004(2) 0.010(2) 0.002(2) C20 0.052(4) 0.027(3) 0.033(3) 0.004(2) 0.017(3) 0.000(2) C21 0.043(3) 0.040(3) 0.036(3) -0.001(3) 0.011(3) -0.012(3) C22 0.030(3) 0.049(3) 0.025(3) 0.000(2) 0.006(2) -0.005(2) C23 0.034(3) 0.040(3) 0.023(3) 0.005(2) 0.011(2) 0.006(2) C24 0.032(3) 0.032(3) 0.032(3) 0.004(2) 0.009(2) 0.009(2) C25 0.044(4) 0.052(4) 0.041(3) 0.000(3) 0.016(3) 0.012(3) C26 0.056(4) 0.042(3) 0.046(4) 0.013(3) 0.014(3) 0.019(3) C27 0.034(3) 0.041(3) 0.032(3) 0.008(2) 0.011(2) 0.007(2) C28 0.064(4) 0.062(4) 0.045(4) 0.026(3) 0.024(3) 0.023(4) C29 0.040(4) 0.073(5) 0.050(4) 0.021(4) 0.012(3) 0.021(3) P1 0.0236(6) 0.0226(6) 0.0213(6) 0.0039(5) 0.0051(5) 0.0016(5) C31 0.027(3) 0.027(3) 0.024(2) 0.005(2) 0.007(2) 0.000(2) C32 0.028(3) 0.028(3) 0.036(3) 0.003(2) 0.011(2) 0.000(2) C33 0.038(3) 0.035(3) 0.037(3) 0.002(2) 0.009(3) -0.009(2) C34 0.039(3) 0.044(3) 0.033(3) -0.001(3) 0.002(3) -0.007(3) C35 0.031(3) 0.046(4) 0.044(3) 0.002(3) -0.003(3) 0.002(3) C36 0.028(3) 0.033(3) 0.034(3) 0.004(2) 0.002(2) 0.004(2) C37 0.029(3) 0.026(2) 0.026(2) 0.005(2) 0.008(2) 0.005(2) C38 0.035(3) 0.028(3) 0.035(3) 0.005(2) 0.015(2) 0.005(2) C39 0.036(3) 0.039(3) 0.041(3) 0.002(3) 0.019(3) 0.008(2) C40 0.038(3) 0.033(3) 0.039(3) -0.002(2) 0.010(3) 0.006(2) C41 0.032(3) 0.028(3) 0.047(3) 0.004(2) 0.009(3) 0.000(2) C42 0.029(3) 0.031(3) 0.035(3) 0.004(2) 0.007(2) 0.001(2) C43 0.025(3) 0.029(3) 0.025(2) 0.005(2) 0.007(2) 0.009(2) C44 0.026(3) 0.031(3) 0.028(3) 0.007(2) 0.010(2) 0.004(2) C45 0.035(3) 0.048(3) 0.030(3) 0.020(3) 0.008(2) 0.003(3) C46 0.035(3) 0.048(3) 0.029(3) 0.010(2) 0.001(2) 0.009(3) C47 0.030(3) 0.034(3) 0.030(3) 0.003(2) 0.004(2) 0.001(2) C48 0.026(3) 0.027(3) 0.031(3) 0.007(2) 0.008(2) 0.000(2) C49 0.034(3) 0.026(3) 0.029(3) 0.012(2) 0.008(2) 0.002(2) C50 0.030(3) 0.027(3) 0.038(3) 0.012(2) 0.014(2) 0.004(2) C51 0.034(3) 0.026(3) 0.042(3) 0.008(2) 0.017(2) 0.005(2) C52 0.031(3) 0.032(3) 0.036(3) 0.014(2) 0.012(2) 0.007(2) C53 0.029(3) 0.032(3) 0.037(3) 0.016(2) 0.016(2) 0.008(2) C54 0.032(3) 0.028(3) 0.031(3) 0.013(2) 0.013(2) 0.005(2) C55 0.039(3) 0.025(3) 0.050(3) 0.012(2) 0.022(3) 0.007(2) C56 0.050(4) 0.028(3) 0.059(4) 0.005(3) 0.030(3) 0.007(3) C57 0.038(3) 0.045(4) 0.066(4) 0.024(3) 0.015(3) 0.010(3) C58 0.034(3) 0.035(3) 0.044(3) 0.010(3) 0.013(3) 0.000(2) C59 0.036(3) 0.056(4) 0.061(4) 0.019(3) -0.007(3) -0.008(3) C60 0.038(3) 0.036(3) 0.062(4) 0.015(3) 0.014(3) 0.001(3) C61 0.037(3) 0.029(3) 0.041(3) 0.008(2) 0.019(3) 0.002(2) C62 0.046(4) 0.035(3) 0.066(4) 0.011(3) 0.031(3) 0.007(3) C63 0.068(5) 0.051(4) 0.039(3) 0.012(3) 0.026(3) 0.007(3) C71 0.046(4) 0.045(4) 0.064(4) 0.012(3) 0.021(3) 0.011(3) Cl3 0.0519(10) 0.0775(13) 0.0489(10) -0.0011(9) 0.0102(8) 0.0172(9) Cl4 0.1004(16) 0.0518(10) 0.0490(10) 0.0138(8) 0.0219(10) -0.0059(10) C72 0.24(4) 0.18(3) 0.067(15) 0.034(17) 0.020(19) -0.10(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.055(5) . ? Pd1 Cl2 2.3027(12) . ? Pd1 Cl1 2.3133(13) . ? Pd1 P1 2.3211(14) . ? C1 N5 1.346(7) . ? C1 N2 1.351(6) . ? N2 C3 1.373(7) . ? N2 C6 1.453(7) . ? C3 C4 1.339(8) . ? C3 H3A 0.9500 . ? C4 N5 1.395(7) . ? C4 H4A 0.9500 . ? N5 C18 1.450(7) . ? C6 C7 1.404(8) . ? C6 C11 1.406(8) . ? C7 C8 1.395(8) . ? C7 C12 1.521(8) . ? C8 C9 1.379(9) . ? C8 H8A 0.9500 . ? C9 C10 1.378(9) . ? C9 H9A 0.9500 . ? C10 C11 1.394(8) . ? C10 H10A 0.9500 . ? C11 C15 1.511(8) . ? C12 C13 1.526(9) . ? C12 C14 1.537(9) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.530(9) . ? C15 C16 1.534(10) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.396(8) . ? C18 C23 1.397(8) . ? C19 C20 1.405(8) . ? C19 C24 1.533(7) . ? C20 C21 1.366(9) . ? C20 H20A 0.9500 . ? C21 C22 1.372(9) . ? C21 H21A 0.9500 . ? C22 C23 1.399(8) . ? C22 H22A 0.9500 . ? C23 C27 1.520(8) . ? C24 C25 1.520(9) . ? C24 C26 1.528(8) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.522(8) . ? C27 C28 1.541(9) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C43 1.836(5) . ? P1 C31 1.844(5) . ? P1 C37 1.850(5) . ? C31 C32 1.538(7) . ? C31 C36 1.543(7) . ? C31 H31A 1.0000 . ? C32 C33 1.539(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.522(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.535(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.530(7) . ? C37 C38 1.534(8) . ? C37 H37A 1.0000 . ? C38 C39 1.543(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.521(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.533(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.531(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.410(7) . ? C43 C44 1.419(7) . ? C44 C45 1.411(7) . ? C44 C49 1.512(7) . ? C45 C46 1.382(8) . ? C45 H45A 0.9500 . ? C46 C47 1.384(8) . ? C46 H46A 0.9500 . ? C47 C48 1.381(7) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C54 1.400(8) . ? C49 C50 1.412(8) . ? C50 C51 1.402(7) . ? C50 C55 1.526(8) . ? C51 C52 1.388(8) . ? C51 H51A 0.9500 . ? C52 C53 1.374(8) . ? C52 C58 1.531(8) . ? C53 C54 1.391(8) . ? C53 H53A 0.9500 . ? C54 C61 1.534(8) . ? C55 C56 1.514(8) . ? C55 C57 1.528(8) . ? C55 H55A 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 . ? C58 C60 1.522(8) . ? C58 C59 1.533(9) . ? C58 H58A 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.530(8) . ? C61 C62 1.540(8) . ? C61 H61A 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C71 Cl4 1.726(7) . ? C71 Cl3 1.752(7) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 Cl6 1.7700(11) . ? C72 Cl5 1.7703(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl2 88.24(13) . . ? C1 Pd1 Cl1 90.76(13) . . ? Cl2 Pd1 Cl1 178.38(5) . . ? C1 Pd1 P1 178.24(14) . . ? Cl2 Pd1 P1 91.08(5) . . ? Cl1 Pd1 P1 89.89(5) . . ? N5 C1 N2 105.5(4) . . ? N5 C1 Pd1 126.6(4) . . ? N2 C1 Pd1 127.9(4) . . ? C1 N2 C3 110.5(4) . . ? C1 N2 C6 125.7(4) . . ? C3 N2 C6 123.5(4) . . ? C4 C3 N2 107.5(5) . . ? C4 C3 H3A 126.3 . . ? N2 C3 H3A 126.3 . . ? C3 C4 N5 106.4(5) . . ? C3 C4 H4A 126.8 . . ? N5 C4 H4A 126.8 . . ? C1 N5 C4 110.2(4) . . ? C1 N5 C18 124.7(4) . . ? C4 N5 C18 125.1(4) . . ? C7 C6 C11 123.3(5) . . ? C7 C6 N2 117.5(5) . . ? C11 C6 N2 119.2(5) . . ? C8 C7 C6 117.1(5) . . ? C8 C7 C12 120.1(5) . . ? C6 C7 C12 122.7(5) . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C10 C9 C8 120.9(5) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 121.4(6) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C6 116.5(5) . . ? C10 C11 C15 121.9(5) . . ? C6 C11 C15 121.7(5) . . ? C7 C12 C13 110.8(5) . . ? C7 C12 C14 112.6(5) . . ? C13 C12 C14 110.0(5) . . ? C7 C12 H12A 107.7 . . ? C13 C12 H12A 107.7 . . ? C14 C12 H12A 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 113.0(6) . . ? C11 C15 C16 110.8(5) . . ? C17 C15 C16 109.8(5) . . ? C11 C15 H15A 107.7 . . ? C17 C15 H15A 107.7 . . ? C16 C15 H15A 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.5(5) . . ? C19 C18 N5 118.5(5) . . ? C23 C18 N5 118.0(5) . . ? C18 C19 C20 117.1(5) . . ? C18 C19 C24 122.6(5) . . ? C20 C19 C24 120.3(5) . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 120.9(5) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C21 C22 C23 121.7(5) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C18 C23 C22 116.2(5) . . ? C18 C23 C27 122.4(5) . . ? C22 C23 C27 121.3(5) . . ? C25 C24 C26 109.3(5) . . ? C25 C24 C19 110.8(5) . . ? C26 C24 C19 112.8(5) . . ? C25 C24 H24A 107.9 . . ? C26 C24 H24A 107.9 . . ? C19 C24 H24A 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 114.4(5) . . ? C23 C27 C28 109.8(5) . . ? C29 C27 C28 109.6(5) . . ? C23 C27 H27A 107.6 . . ? C29 C27 H27A 107.6 . . ? C28 C27 H27A 107.6 . . ? 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 . . ? C43 P1 C31 110.1(2) . . ? C43 P1 C37 103.6(2) . . ? C31 P1 C37 106.0(2) . . ? C43 P1 Pd1 114.20(18) . . ? C31 P1 Pd1 110.16(17) . . ? C37 P1 Pd1 112.35(17) . . ? C32 C31 C36 109.4(4) . . ? C32 C31 P1 108.2(4) . . ? C36 C31 P1 114.3(4) . . ? C32 C31 H31A 108.3 . . ? C36 C31 H31A 108.3 . . ? P1 C31 H31A 108.3 . . ? C33 C32 C31 111.0(5) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 110.6(5) . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C33 C34 C35 111.6(5) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 112.0(5) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 109.8(4) . . ? C35 C36 H36A 109.7 . . ? C31 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C31 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C42 C37 C38 110.2(4) . . ? C42 C37 P1 114.1(4) . . ? C38 C37 P1 113.6(4) . . ? C42 C37 H37A 106.1 . . ? C38 C37 H37A 106.1 . . ? P1 C37 H37A 106.1 . . ? C37 C38 C39 110.8(4) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 110.9(5) . . ? C40 C39 H39A 109.5 . . ? C38 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C39 C40 C41 111.2(5) . . ? C39 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? C39 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C40 112.2(5) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C37 C42 C41 109.2(4) . . ? C37 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? C37 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C48 C43 C44 118.0(4) . . ? C48 C43 P1 110.0(4) . . ? C44 C43 P1 131.9(4) . . ? C45 C44 C43 117.7(5) . . ? C45 C44 C49 115.2(5) . . ? C43 C44 C49 127.0(4) . . ? C46 C45 C44 122.6(5) . . ? C46 C45 H45A 118.7 . . ? C44 C45 H45A 118.7 . . ? C45 C46 C47 119.8(5) . . ? C45 C46 H46A 120.1 . . ? C47 C46 H46A 120.1 . . ? C48 C47 C46 118.9(5) . . ? C48 C47 H47A 120.6 . . ? C46 C47 H47A 120.6 . . ? C47 C48 C43 122.9(5) . . ? C47 C48 H48A 118.5 . . ? C43 C48 H48A 118.5 . . ? C54 C49 C50 120.4(5) . . ? C54 C49 C44 119.5(5) . . ? C50 C49 C44 119.9(5) . . ? C51 C50 C49 117.6(5) . . ? C51 C50 C55 120.0(5) . . ? C49 C50 C55 122.4(5) . . ? C52 C51 C50 122.5(5) . . ? C52 C51 H51A 118.7 . . ? C50 C51 H51A 118.7 . . ? C53 C52 C51 118.1(5) . . ? C53 C52 C58 120.1(5) . . ? C51 C52 C58 121.8(5) . . ? C52 C53 C54 122.2(5) . . ? C52 C53 H53A 118.9 . . ? C54 C53 H53A 118.9 . . ? C53 C54 C49 119.0(5) . . ? C53 C54 C61 118.4(5) . . ? C49 C54 C61 122.6(5) . . ? C56 C55 C57 109.5(5) . . ? C56 C55 C50 113.3(5) . . ? C57 C55 C50 110.1(5) . . ? C56 C55 H55A 107.9 . . ? C57 C55 H55A 107.9 . . ? C50 C55 H55A 107.9 . . ? 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 . . ? C60 C58 C52 113.5(5) . . ? C60 C58 C59 111.0(6) . . ? C52 C58 C59 110.7(5) . . ? C60 C58 H58A 107.1 . . ? C52 C58 H58A 107.1 . . ? C59 C58 H58A 107.1 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 C54 110.6(5) . . ? C63 C61 C62 110.2(5) . . ? C54 C61 C62 112.2(5) . . ? C63 C61 H61A 107.9 . . ? C54 C61 H61A 107.9 . . ? C62 C61 H61A 107.9 . . ? 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 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Cl4 C71 Cl3 111.3(4) . . ? Cl4 C71 H71A 109.4 . . ? Cl3 C71 H71A 109.4 . . ? Cl4 C71 H71B 109.4 . . ? Cl3 C71 H71B 109.4 . . ? H71A C71 H71B 108.0 . . ? Cl6 C72 Cl5 133.0(7) . . ? Cl6 C72 H72A 104.0 . . ? Cl5 C72 H72A 104.0 . . ? Cl6 C72 H72B 104.0 . . ? Cl5 C72 H72B 104.0 . . ? H72A C72 H72B 105.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pd1 C1 N5 -71.6(4) . . . . ? Cl1 Pd1 C1 N5 107.1(4) . . . . ? P1 Pd1 C1 N5 -4(5) . . . . ? Cl2 Pd1 C1 N2 104.4(4) . . . . ? Cl1 Pd1 C1 N2 -76.9(4) . . . . ? P1 Pd1 C1 N2 172(4) . . . . ? N5 C1 N2 C3 0.3(6) . . . . ? Pd1 C1 N2 C3 -176.4(4) . . . . ? N5 C1 N2 C6 -173.8(4) . . . . ? Pd1 C1 N2 C6 9.5(7) . . . . ? C1 N2 C3 C4 -0.3(6) . . . . ? C6 N2 C3 C4 173.9(5) . . . . ? N2 C3 C4 N5 0.2(6) . . . . ? N2 C1 N5 C4 -0.1(5) . . . . ? Pd1 C1 N5 C4 176.6(4) . . . . ? N2 C1 N5 C18 177.8(4) . . . . ? Pd1 C1 N5 C18 -5.5(7) . . . . ? C3 C4 N5 C1 -0.1(6) . . . . ? C3 C4 N5 C18 -177.9(5) . . . . ? C1 N2 C6 C7 99.3(6) . . . . ? C3 N2 C6 C7 -74.0(7) . . . . ? C1 N2 C6 C11 -82.2(7) . . . . ? C3 N2 C6 C11 104.5(6) . . . . ? C11 C6 C7 C8 0.0(8) . . . . ? N2 C6 C7 C8 178.4(5) . . . . ? C11 C6 C7 C12 -177.6(6) . . . . ? N2 C6 C7 C12 0.8(8) . . . . ? C6 C7 C8 C9 1.1(9) . . . . ? C12 C7 C8 C9 178.8(6) . . . . ? C7 C8 C9 C10 -0.8(10) . . . . ? C8 C9 C10 C11 -0.6(10) . . . . ? C9 C10 C11 C6 1.6(9) . . . . ? C9 C10 C11 C15 -177.3(6) . . . . ? C7 C6 C11 C10 -1.3(8) . . . . ? N2 C6 C11 C10 -179.7(5) . . . . ? C7 C6 C11 C15 177.5(5) . . . . ? N2 C6 C11 C15 -0.9(8) . . . . ? C8 C7 C12 C13 -78.2(7) . . . . ? C6 C7 C12 C13 99.4(6) . . . . ? C8 C7 C12 C14 45.5(8) . . . . ? C6 C7 C12 C14 -136.9(6) . . . . ? C10 C11 C15 C17 -22.3(8) . . . . ? C6 C11 C15 C17 159.0(6) . . . . ? C10 C11 C15 C16 101.5(7) . . . . ? C6 C11 C15 C16 -77.3(7) . . . . ? C1 N5 C18 C19 103.9(6) . . . . ? C4 N5 C18 C19 -78.5(7) . . . . ? C1 N5 C18 C23 -76.4(6) . . . . ? C4 N5 C18 C23 101.2(6) . . . . ? C23 C18 C19 C20 2.6(8) . . . . ? N5 C18 C19 C20 -177.8(5) . . . . ? C23 C18 C19 C24 -174.9(5) . . . . ? N5 C18 C19 C24 4.7(8) . . . . ? C18 C19 C20 C21 -0.5(8) . . . . ? C24 C19 C20 C21 177.1(5) . . . . ? C19 C20 C21 C22 -0.8(9) . . . . ? C20 C21 C22 C23 0.1(9) . . . . ? C19 C18 C23 C22 -3.2(8) . . . . ? N5 C18 C23 C22 177.1(5) . . . . ? C19 C18 C23 C27 173.1(5) . . . . ? N5 C18 C23 C27 -6.5(8) . . . . ? C21 C22 C23 C18 1.8(8) . . . . ? C21 C22 C23 C27 -174.6(5) . . . . ? C18 C19 C24 C25 94.3(6) . . . . ? C20 C19 C24 C25 -83.1(7) . . . . ? C18 C19 C24 C26 -142.8(5) . . . . ? C20 C19 C24 C26 39.8(7) . . . . ? C18 C23 C27 C29 154.2(6) . . . . ? C22 C23 C27 C29 -29.7(8) . . . . ? C18 C23 C27 C28 -82.1(7) . . . . ? C22 C23 C27 C28 94.0(7) . . . . ? C1 Pd1 P1 C43 -94(4) . . . . ? Cl2 Pd1 P1 C43 -26.54(19) . . . . ? Cl1 Pd1 P1 C43 154.77(19) . . . . ? C1 Pd1 P1 C31 31(4) . . . . ? Cl2 Pd1 P1 C31 97.96(18) . . . . ? Cl1 Pd1 P1 C31 -80.74(18) . . . . ? C1 Pd1 P1 C37 149(4) . . . . ? Cl2 Pd1 P1 C37 -144.15(18) . . . . ? Cl1 Pd1 P1 C37 37.16(18) . . . . ? C43 P1 C31 C32 93.0(4) . . . . ? C37 P1 C31 C32 -155.6(3) . . . . ? Pd1 P1 C31 C32 -33.8(4) . . . . ? C43 P1 C31 C36 -145.0(4) . . . . ? C37 P1 C31 C36 -33.5(5) . . . . ? Pd1 P1 C31 C36 88.2(4) . . . . ? C36 C31 C32 C33 58.9(6) . . . . ? P1 C31 C32 C33 -176.0(4) . . . . ? C31 C32 C33 C34 -57.2(6) . . . . ? C32 C33 C34 C35 54.7(7) . . . . ? C33 C34 C35 C36 -55.2(7) . . . . ? C34 C35 C36 C31 56.6(7) . . . . ? C32 C31 C36 C35 -57.9(6) . . . . ? P1 C31 C36 C35 -179.4(4) . . . . ? C43 P1 C37 C42 -76.7(4) . . . . ? C31 P1 C37 C42 167.3(4) . . . . ? Pd1 P1 C37 C42 47.0(4) . . . . ? C43 P1 C37 C38 50.8(4) . . . . ? C31 P1 C37 C38 -65.1(4) . . . . ? Pd1 P1 C37 C38 174.5(3) . . . . ? C42 C37 C38 C39 -58.9(6) . . . . ? P1 C37 C38 C39 171.6(4) . . . . ? C37 C38 C39 C40 56.1(6) . . . . ? C38 C39 C40 C41 -53.7(7) . . . . ? C39 C40 C41 C42 55.2(6) . . . . ? C38 C37 C42 C41 58.8(6) . . . . ? P1 C37 C42 C41 -172.0(4) . . . . ? C40 C41 C42 C37 -57.2(6) . . . . ? C31 P1 C43 C48 -176.8(4) . . . . ? C37 P1 C43 C48 70.2(4) . . . . ? Pd1 P1 C43 C48 -52.3(4) . . . . ? C31 P1 C43 C44 7.6(6) . . . . ? C37 P1 C43 C44 -105.4(5) . . . . ? Pd1 P1 C43 C44 132.1(5) . . . . ? C48 C43 C44 C45 -4.0(8) . . . . ? P1 C43 C44 C45 171.3(4) . . . . ? C48 C43 C44 C49 172.6(5) . . . . ? P1 C43 C44 C49 -12.1(9) . . . . ? C43 C44 C45 C46 0.2(9) . . . . ? C49 C44 C45 C46 -176.8(5) . . . . ? C44 C45 C46 C47 3.0(9) . . . . ? C45 C46 C47 C48 -2.2(9) . . . . ? C46 C47 C48 C43 -1.7(9) . . . . ? C44 C43 C48 C47 4.9(8) . . . . ? P1 C43 C48 C47 -171.4(5) . . . . ? C45 C44 C49 C54 -80.6(6) . . . . ? C43 C44 C49 C54 102.8(6) . . . . ? C45 C44 C49 C50 93.2(6) . . . . ? C43 C44 C49 C50 -83.4(7) . . . . ? C54 C49 C50 C51 -3.8(7) . . . . ? C44 C49 C50 C51 -177.5(5) . . . . ? C54 C49 C50 C55 173.1(5) . . . . ? C44 C49 C50 C55 -0.6(7) . . . . ? C49 C50 C51 C52 -0.1(8) . . . . ? C55 C50 C51 C52 -177.1(5) . . . . ? C50 C51 C52 C53 3.2(8) . . . . ? C50 C51 C52 C58 -174.7(5) . . . . ? C51 C52 C53 C54 -2.3(8) . . . . ? C58 C52 C53 C54 175.6(5) . . . . ? C52 C53 C54 C49 -1.5(8) . . . . ? C52 C53 C54 C61 177.7(5) . . . . ? C50 C49 C54 C53 4.6(7) . . . . ? C44 C49 C54 C53 178.3(4) . . . . ? C50 C49 C54 C61 -174.6(5) . . . . ? C44 C49 C54 C61 -0.9(7) . . . . ? C51 C50 C55 C56 -30.3(7) . . . . ? C49 C50 C55 C56 152.9(5) . . . . ? C51 C50 C55 C57 92.7(6) . . . . ? C49 C50 C55 C57 -84.2(6) . . . . ? C53 C52 C58 C60 135.9(6) . . . . ? C51 C52 C58 C60 -46.2(7) . . . . ? C53 C52 C58 C59 -98.5(7) . . . . ? C51 C52 C58 C59 79.4(7) . . . . ? C53 C54 C61 C63 -77.7(6) . . . . ? C49 C54 C61 C63 101.5(6) . . . . ? C53 C54 C61 C62 45.7(7) . . . . ? C49 C54 C61 C62 -135.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.902 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.138 data_2g _database_code_depnum_ccdc_archive 'CCDC 871888' #TrackingRef '10176_web_deposit_cif_file_6_CatherineS.J.Cazin_1331897901.2g.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H71 Cl2 N2 O2 P Pd' _chemical_formula_sum 'C53 H71 Cl2 N2 O2 P Pd' _chemical_formula_weight 976.39 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.580(3) _cell_length_b 14.0874(19) _cell_length_c 19.401(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.472(3) _cell_angle_gamma 90.00 _cell_volume 5077.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 12657 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50611 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.36 _reflns_number_total 9288 _reflns_number_gt 8133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+2.7939P] 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 9288 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.221164(12) 0.101852(17) 0.229758(12) 0.02521(11) Uani 1 1 d . . . Cl1 Cl 0.13555(4) 0.21581(6) 0.25518(5) 0.0342(2) Uani 1 1 d . . . Cl2 Cl 0.30605(4) -0.01076(6) 0.20441(5) 0.0357(2) Uani 1 1 d . . . C1 C 0.13906(17) 0.0108(2) 0.20342(16) 0.0258(7) Uani 1 1 d . . . N2 N 0.09900(15) -0.04079(19) 0.24778(13) 0.0289(6) Uani 1 1 d . . . C3 C 0.0441(2) -0.0880(3) 0.21373(19) 0.0359(8) Uani 1 1 d . . . H3A H 0.0091 -0.1284 0.2339 0.043 Uiso 1 1 calc R . . C4 C 0.04952(19) -0.0660(2) 0.14691(18) 0.0345(8) Uani 1 1 d . . . H4A H 0.0187 -0.0866 0.1105 0.041 Uiso 1 1 calc R . . N5 N 0.10901(14) -0.00697(18) 0.14114(13) 0.0259(6) Uani 1 1 d . . . C6 C 0.11202(17) -0.0503(2) 0.32097(16) 0.0271(7) Uani 1 1 d . . . C7 C 0.16322(19) -0.1160(2) 0.34370(19) 0.0323(8) Uani 1 1 d . . . C8 C 0.1736(2) -0.1241(3) 0.41446(19) 0.0377(9) Uani 1 1 d . . . H8A H 0.2086 -0.1674 0.4316 0.045 Uiso 1 1 calc R . . C9 C 0.1342(2) -0.0708(3) 0.46038(19) 0.0393(9) Uani 1 1 d . . . H9A H 0.1424 -0.0774 0.5085 0.047 Uiso 1 1 calc R . . C10 C 0.08301(19) -0.0081(3) 0.43630(18) 0.0357(8) Uani 1 1 d . . . H10A H 0.0556 0.0274 0.4684 0.043 Uiso 1 1 calc R . . C11 C 0.07052(17) 0.0043(2) 0.36608(17) 0.0274(7) Uani 1 1 d . . . C12 C 0.2033(2) -0.1803(3) 0.2940(2) 0.0421(9) Uani 1 1 d . . . H12A H 0.2070 -0.1457 0.2491 0.051 Uiso 1 1 calc R . . C13 C 0.2795(2) -0.2038(3) 0.3178(2) 0.0552(11) Uani 1 1 d . . . H13A H 0.3065 -0.1449 0.3250 0.083 Uiso 1 1 calc R . . H13B H 0.3033 -0.2422 0.2826 0.083 Uiso 1 1 calc R . . H13C H 0.2776 -0.2395 0.3611 0.083 Uiso 1 1 calc R . . C14 C 0.1594(3) -0.2714(3) 0.2806(3) 0.0641(13) Uani 1 1 d . . . H14A H 0.1856 -0.3124 0.2486 0.096 Uiso 1 1 calc R . . H14B H 0.1126 -0.2546 0.2605 0.096 Uiso 1 1 calc R . . H14C H 0.1523 -0.3050 0.3242 0.096 Uiso 1 1 calc R . . C15 C 0.01230(18) 0.0713(2) 0.34076(18) 0.0322(8) Uani 1 1 d . . . H15A H 0.0225 0.0870 0.2915 0.039 Uiso 1 1 calc R . . C16 C 0.0100(2) 0.1643(3) 0.3811(2) 0.0422(9) Uani 1 1 d . . . H16A H 0.0572 0.1953 0.3792 0.063 Uiso 1 1 calc R . . H16B H -0.0021 0.1511 0.4292 0.063 Uiso 1 1 calc R . . H16C H -0.0266 0.2062 0.3608 0.063 Uiso 1 1 calc R . . C17 C -0.0621(2) 0.0237(3) 0.3435(2) 0.0452(10) Uani 1 1 d . . . H17A H -0.0612 -0.0356 0.3170 0.068 Uiso 1 1 calc R . . H17B H -0.0984 0.0664 0.3236 0.068 Uiso 1 1 calc R . . H17C H -0.0743 0.0098 0.3915 0.068 Uiso 1 1 calc R . . C18 C 0.13219(17) 0.0266(3) 0.07443(17) 0.0310(8) Uani 1 1 d . . . C19 C 0.0999(2) 0.1076(2) 0.04743(19) 0.0378(9) Uani 1 1 d . . . C20 C 0.1175(3) 0.1290(3) -0.0224(2) 0.0571(12) Uani 1 1 d . . . H20A H 0.0974 0.1834 -0.0441 0.069 Uiso 1 1 calc R . . C21 C 0.1635(3) 0.0710(4) -0.0582(2) 0.0618(13) Uani 1 1 d . . . H21A H 0.1742 0.0863 -0.1047 0.074 Uiso 1 1 calc R . . C22 C 0.1941(2) -0.0070(4) -0.0297(2) 0.0577(12) Uani 1 1 d . . . H22A H 0.2253 -0.0454 -0.0564 0.069 Uiso 1 1 calc R . . C23 C 0.18044(19) -0.0311(3) 0.03773(19) 0.0409(9) Uani 1 1 d . . . C24 C 0.0482(2) 0.1677(3) 0.0875(2) 0.0487(10) Uani 1 1 d . . . H24A H 0.0490 0.1461 0.1366 0.058 Uiso 1 1 calc R . . C25 C 0.0697(4) 0.2735(3) 0.0854(3) 0.0791(17) Uani 1 1 d . . . H25A H 0.1183 0.2811 0.1048 0.119 Uiso 1 1 calc R . . H25B H 0.0356 0.3107 0.1125 0.119 Uiso 1 1 calc R . . H25C H 0.0690 0.2958 0.0376 0.119 Uiso 1 1 calc R . . C26 C -0.0270(3) 0.1537(4) 0.0587(3) 0.0772(16) Uani 1 1 d . . . H26A H -0.0399 0.0864 0.0613 0.116 Uiso 1 1 calc R . . H26B H -0.0286 0.1746 0.0105 0.116 Uiso 1 1 calc R . . H26C H -0.0612 0.1911 0.0857 0.116 Uiso 1 1 calc R . . C27 C 0.2150(2) -0.1175(3) 0.0697(2) 0.0517(11) Uani 1 1 d . . . H27A H 0.2189 -0.1054 0.1204 0.062 Uiso 1 1 calc R . . C28 C 0.2910(3) -0.1368(5) 0.0438(3) 0.0837(18) Uani 1 1 d . . . H28A H 0.3206 -0.0798 0.0499 0.126 Uiso 1 1 calc R . . H28B H 0.2890 -0.1536 -0.0052 0.126 Uiso 1 1 calc R . . H28C H 0.3123 -0.1894 0.0700 0.126 Uiso 1 1 calc R . . C29 C 0.1698(3) -0.2086(3) 0.0602(3) 0.0658(13) Uani 1 1 d . . . H29A H 0.1209 -0.1976 0.0771 0.099 Uiso 1 1 calc R . . H29B H 0.1920 -0.2607 0.0862 0.099 Uiso 1 1 calc R . . H29C H 0.1677 -0.2254 0.0112 0.099 Uiso 1 1 calc R . . P1 P 0.31334(4) 0.20011(6) 0.27003(4) 0.02445(19) Uani 1 1 d . . . C31 C 0.29243(18) 0.3279(2) 0.26422(16) 0.0286(7) Uani 1 1 d . . . H31A H 0.2470 0.3375 0.2907 0.034 Uiso 1 1 calc R . . C32 C 0.27625(19) 0.3609(2) 0.19039(18) 0.0337(8) Uani 1 1 d . . . H32A H 0.3201 0.3549 0.1621 0.040 Uiso 1 1 calc R . . H32B H 0.2384 0.3202 0.1697 0.040 Uiso 1 1 calc R . . C33 C 0.2511(2) 0.4641(3) 0.19071(19) 0.0395(9) Uani 1 1 d . . . H33A H 0.2421 0.4853 0.1427 0.047 Uiso 1 1 calc R . . H33B H 0.2053 0.4690 0.2162 0.047 Uiso 1 1 calc R . . C34 C 0.3072(2) 0.5286(3) 0.2243(2) 0.0473(10) Uani 1 1 d . . . H34A H 0.3517 0.5278 0.1966 0.057 Uiso 1 1 calc R . . H34B H 0.2888 0.5945 0.2253 0.057 Uiso 1 1 calc R . . C35 C 0.3240(2) 0.4963(3) 0.2967(2) 0.0435(9) Uani 1 1 d . . . H35A H 0.2806 0.5032 0.3255 0.052 Uiso 1 1 calc R . . H35B H 0.3623 0.5370 0.3166 0.052 Uiso 1 1 calc R . . C36 C 0.34881(19) 0.3926(2) 0.2978(2) 0.0340(8) Uani 1 1 d . . . H36A H 0.3572 0.3724 0.3461 0.041 Uiso 1 1 calc R . . H36B H 0.3948 0.3868 0.2728 0.041 Uiso 1 1 calc R . . C37 C 0.32597(17) 0.1753(2) 0.36310(16) 0.0294(7) Uani 1 1 d . . . H37A H 0.3743 0.1999 0.3775 0.035 Uiso 1 1 calc R . . C38 C 0.26868(19) 0.2245(3) 0.40711(17) 0.0346(8) Uani 1 1 d . . . H38A H 0.2701 0.2939 0.3990 0.042 Uiso 1 1 calc R . . H38B H 0.2203 0.2012 0.3939 0.042 Uiso 1 1 calc R . . C39 C 0.2831(2) 0.2037(3) 0.48348(18) 0.0438(9) Uani 1 1 d . . . H39A H 0.3300 0.2315 0.4972 0.053 Uiso 1 1 calc R . . H39B H 0.2453 0.2339 0.5116 0.053 Uiso 1 1 calc R . . C40 C 0.2842(2) 0.0976(3) 0.4979(2) 0.0486(11) Uani 1 1 d . . . H40A H 0.2972 0.0868 0.5468 0.058 Uiso 1 1 calc R . . H40B H 0.2355 0.0712 0.4899 0.058 Uiso 1 1 calc R . . C41 C 0.3373(2) 0.0465(3) 0.45255(18) 0.0461(10) Uani 1 1 d . . . H41A H 0.3329 -0.0228 0.4600 0.055 Uiso 1 1 calc R . . H41B H 0.3868 0.0657 0.4656 0.055 Uiso 1 1 calc R . . C42 C 0.3244(2) 0.0685(3) 0.37645(18) 0.0358(8) Uani 1 1 d . . . H42A H 0.3619 0.0372 0.3486 0.043 Uiso 1 1 calc R . . H42B H 0.2770 0.0428 0.3620 0.043 Uiso 1 1 calc R . . C43 C 0.39911(16) 0.1884(2) 0.22327(15) 0.0235(6) Uani 1 1 d . . . C44 C 0.47035(17) 0.1863(2) 0.24771(15) 0.0235(7) Uani 1 1 d . . . C45 C 0.52616(17) 0.1844(2) 0.20003(16) 0.0267(7) Uani 1 1 d . . . H45A H 0.5744 0.1832 0.2165 0.032 Uiso 1 1 calc R . . C46 C 0.51369(18) 0.1842(2) 0.12934(17) 0.0299(7) Uani 1 1 d . . . H46A H 0.5528 0.1839 0.0981 0.036 Uiso 1 1 calc R . . C47 C 0.44400(19) 0.1843(2) 0.10515(16) 0.0304(7) Uani 1 1 d . . . H47A H 0.4346 0.1834 0.0569 0.036 Uiso 1 1 calc R . . C48 C 0.38749(18) 0.1857(2) 0.15131(16) 0.0286(7) Uani 1 1 d . . . H48A H 0.3395 0.1848 0.1340 0.034 Uiso 1 1 calc R . . C49 C 0.49426(16) 0.1821(2) 0.32144(16) 0.0237(7) Uani 1 1 d . . . C50 C 0.51309(17) 0.2640(2) 0.35776(16) 0.0260(7) Uani 1 1 d . . . C51 C 0.53554(18) 0.2592(2) 0.42702(17) 0.0326(8) Uani 1 1 d . . . H51A H 0.5454 0.3154 0.4525 0.039 Uiso 1 1 calc R . . C52 C 0.5430(2) 0.1713(3) 0.45715(18) 0.0378(8) Uani 1 1 d . . . H52A H 0.5577 0.1676 0.5041 0.045 Uiso 1 1 calc R . . C53 C 0.5298(2) 0.0886(3) 0.42137(18) 0.0350(8) Uani 1 1 d . . . H53A H 0.5373 0.0287 0.4426 0.042 Uiso 1 1 calc R . . C54 C 0.50498(18) 0.0944(2) 0.35304(17) 0.0278(7) Uani 1 1 d . . . O50 O 0.50968(12) 0.34647(15) 0.32130(11) 0.0305(5) Uani 1 1 d . . . C55 C 0.5212(2) 0.4346(2) 0.35641(19) 0.0353(8) Uani 1 1 d . . . H55A H 0.5171 0.4871 0.3235 0.053 Uiso 1 1 calc R . . H55B H 0.5693 0.4349 0.3774 0.053 Uiso 1 1 calc R . . H55C H 0.4850 0.4422 0.3924 0.053 Uiso 1 1 calc R . . O54 O 0.49123(13) 0.01779(15) 0.31250(12) 0.0325(5) Uani 1 1 d . . . C56 C 0.4926(2) -0.0741(2) 0.3432(2) 0.0416(9) Uani 1 1 d . . . H56A H 0.4817 -0.1221 0.3081 0.062 Uiso 1 1 calc R . . H56B H 0.4566 -0.0773 0.3798 0.062 Uiso 1 1 calc R . . H56C H 0.5405 -0.0862 0.3629 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02331(17) 0.02925(17) 0.02303(16) -0.00199(9) -0.00149(11) -0.00185(10) Cl1 0.0246(4) 0.0352(4) 0.0427(5) -0.0060(4) -0.0003(4) 0.0004(3) Cl2 0.0299(4) 0.0341(4) 0.0432(5) -0.0091(4) 0.0003(4) 0.0007(4) C1 0.0257(16) 0.0257(16) 0.0262(16) -0.0026(13) 0.0007(13) 0.0049(13) N2 0.0319(15) 0.0290(14) 0.0256(14) -0.0017(11) -0.0016(12) -0.0010(12) C3 0.037(2) 0.0366(19) 0.035(2) -0.0031(15) -0.0010(16) -0.0135(16) C4 0.036(2) 0.0357(19) 0.0321(18) -0.0058(15) -0.0060(15) -0.0105(16) N5 0.0281(14) 0.0259(13) 0.0236(13) -0.0041(11) -0.0006(11) -0.0031(12) C6 0.0281(17) 0.0277(16) 0.0254(16) 0.0009(13) -0.0016(13) -0.0061(14) C7 0.0317(19) 0.0287(17) 0.0366(19) 0.0051(15) 0.0037(15) -0.0020(15) C8 0.033(2) 0.040(2) 0.040(2) 0.0163(17) -0.0003(16) 0.0017(17) C9 0.039(2) 0.048(2) 0.0299(18) 0.0068(17) -0.0026(16) -0.0016(18) C10 0.0364(19) 0.041(2) 0.0299(18) -0.0018(15) 0.0033(15) -0.0035(17) C11 0.0264(17) 0.0256(16) 0.0301(17) -0.0002(13) 0.0005(14) -0.0061(14) C12 0.042(2) 0.037(2) 0.047(2) 0.0007(17) 0.0093(18) 0.0093(18) C13 0.047(2) 0.050(2) 0.068(3) 0.007(2) 0.007(2) 0.018(2) C14 0.060(3) 0.044(2) 0.088(4) -0.024(2) 0.006(3) 0.004(2) C15 0.0312(19) 0.0302(17) 0.0353(19) -0.0033(15) 0.0002(15) 0.0024(15) C16 0.044(2) 0.035(2) 0.048(2) -0.0070(17) 0.0081(18) 0.0041(17) C17 0.032(2) 0.039(2) 0.065(3) 0.0010(19) -0.0037(18) 0.0011(17) C18 0.0261(17) 0.042(2) 0.0253(16) -0.0036(15) -0.0016(13) -0.0083(15) C19 0.046(2) 0.0327(19) 0.034(2) 0.0025(15) -0.0109(17) -0.0118(16) C20 0.064(3) 0.053(2) 0.054(3) 0.017(2) -0.015(2) -0.024(2) C21 0.066(3) 0.077(3) 0.043(2) -0.007(2) 0.017(2) -0.033(3) C22 0.046(2) 0.083(3) 0.045(2) -0.014(2) 0.011(2) -0.019(2) C23 0.0272(18) 0.062(3) 0.0337(19) -0.0156(18) 0.0003(15) -0.0089(18) C24 0.062(3) 0.041(2) 0.043(2) -0.0081(18) -0.0199(19) 0.013(2) C25 0.139(5) 0.034(2) 0.064(3) -0.003(2) -0.030(3) 0.005(3) C26 0.058(3) 0.093(4) 0.080(4) -0.032(3) -0.019(3) 0.027(3) C27 0.040(2) 0.066(3) 0.049(2) -0.025(2) -0.0088(19) 0.014(2) C28 0.049(3) 0.124(5) 0.078(4) -0.039(4) -0.001(3) 0.025(3) C29 0.061(3) 0.053(3) 0.084(4) -0.019(2) -0.011(3) 0.012(2) P1 0.0230(4) 0.0290(4) 0.0213(4) -0.0013(3) -0.0008(3) -0.0016(3) C31 0.0296(17) 0.0277(17) 0.0284(17) -0.0009(13) -0.0012(14) 0.0012(14) C32 0.0322(19) 0.0350(19) 0.0339(18) 0.0026(15) 0.0003(15) 0.0053(16) C33 0.040(2) 0.043(2) 0.0356(19) 0.0068(16) 0.0047(16) 0.0110(18) C34 0.050(2) 0.0318(19) 0.061(3) 0.0046(18) 0.017(2) 0.0056(18) C35 0.046(2) 0.0301(19) 0.055(2) -0.0093(17) 0.0010(19) -0.0064(17) C36 0.0293(19) 0.0338(19) 0.039(2) -0.0030(15) -0.0029(16) -0.0054(15) C37 0.0250(17) 0.0395(19) 0.0236(16) -0.0001(14) -0.0002(13) -0.0026(15) C38 0.0301(18) 0.049(2) 0.0249(17) -0.0047(15) 0.0008(14) 0.0007(16) C39 0.042(2) 0.067(3) 0.0230(17) -0.0047(17) 0.0017(16) -0.005(2) C40 0.052(3) 0.070(3) 0.0233(19) 0.0084(17) -0.0006(18) -0.013(2) C41 0.053(2) 0.055(2) 0.0301(19) 0.0123(18) -0.0057(17) -0.002(2) C42 0.038(2) 0.041(2) 0.0278(18) 0.0024(15) -0.0028(15) -0.0018(17) C43 0.0235(16) 0.0239(15) 0.0233(15) 0.0005(12) -0.0003(12) -0.0006(13) C44 0.0285(17) 0.0185(14) 0.0236(15) 0.0009(12) 0.0028(13) -0.0021(13) C45 0.0250(16) 0.0250(16) 0.0301(17) 0.0008(13) 0.0008(13) -0.0002(13) C46 0.0330(18) 0.0270(17) 0.0297(17) 0.0009(14) 0.0089(14) 0.0027(15) C47 0.040(2) 0.0305(17) 0.0211(16) -0.0015(13) 0.0004(14) 0.0020(15) C48 0.0300(17) 0.0287(17) 0.0272(17) -0.0012(13) -0.0023(14) 0.0039(14) C49 0.0200(15) 0.0257(16) 0.0256(16) 0.0017(13) 0.0017(12) 0.0004(13) C50 0.0223(16) 0.0247(16) 0.0310(17) 0.0012(13) -0.0008(13) 0.0002(13) C51 0.0334(18) 0.0362(19) 0.0280(17) -0.0027(15) -0.0063(14) -0.0053(16) C52 0.040(2) 0.047(2) 0.0260(17) 0.0026(16) -0.0074(15) -0.0037(17) C53 0.040(2) 0.0333(18) 0.0314(19) 0.0080(15) -0.0052(16) -0.0003(16) C54 0.0270(18) 0.0272(17) 0.0293(18) -0.0019(13) 0.0000(14) -0.0008(14) O50 0.0366(13) 0.0214(11) 0.0334(12) -0.0012(10) -0.0061(10) -0.0033(10) C55 0.038(2) 0.0264(17) 0.042(2) -0.0075(15) -0.0024(16) -0.0057(15) O54 0.0445(14) 0.0208(11) 0.0323(13) 0.0024(9) 0.0001(11) 0.0012(10) C56 0.059(3) 0.0235(17) 0.043(2) 0.0074(16) 0.0058(19) 0.0020(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.054(3) . ? Pd1 Cl2 2.2932(9) . ? Pd1 Cl1 2.3160(9) . ? Pd1 P1 2.3319(9) . ? C1 N5 1.350(4) . ? C1 N2 1.354(4) . ? N2 C3 1.382(4) . ? N2 C6 1.445(4) . ? C3 C4 1.338(5) . ? C3 H3A 0.9500 . ? C4 N5 1.388(4) . ? C4 H4A 0.9500 . ? N5 C18 1.447(4) . ? C6 C7 1.396(5) . ? C6 C11 1.401(5) . ? C7 C8 1.389(5) . ? C7 C12 1.522(5) . ? C8 C9 1.380(5) . ? C8 H8A 0.9500 . ? C9 C10 1.377(5) . ? C9 H9A 0.9500 . ? C10 C11 1.391(5) . ? C10 H10A 0.9500 . ? C11 C15 1.515(5) . ? C12 C13 1.521(6) . ? C12 C14 1.541(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.526(5) . ? C15 C17 1.539(5) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.390(5) . ? C18 C23 1.408(5) . ? C19 C20 1.428(6) . ? C19 C24 1.502(6) . ? C20 C21 1.375(7) . ? C20 H20A 0.9500 . ? C21 C22 1.353(7) . ? C21 H21A 0.9500 . ? C22 C23 1.377(6) . ? C22 H22A 0.9500 . ? C23 C27 1.507(6) . ? C24 C26 1.514(6) . ? C24 C25 1.543(6) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.528(6) . ? C27 C29 1.546(6) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C31 1.845(3) . ? P1 C43 1.847(3) . ? P1 C37 1.852(3) . ? C31 C36 1.530(5) . ? C31 C32 1.533(4) . ? C31 H31A 1.0000 . ? C32 C33 1.527(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.507(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.532(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.527(5) . ? C37 C38 1.536(5) . ? C37 H37A 1.0000 . ? C38 C39 1.532(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.520(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.509(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.526(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.403(4) . ? C43 C48 1.411(4) . ? C44 C45 1.395(4) . ? C44 C49 1.495(4) . ? C45 C46 1.389(5) . ? C45 H45A 0.9500 . ? C46 C47 1.374(5) . ? C46 H46A 0.9500 . ? C47 C48 1.386(5) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C54 1.394(4) . ? C49 C50 1.395(4) . ? C50 O50 1.361(4) . ? C50 C51 1.405(5) . ? C51 C52 1.375(5) . ? C51 H51A 0.9500 . ? C52 C53 1.378(5) . ? C52 H52A 0.9500 . ? C53 C54 1.402(5) . ? C53 H53A 0.9500 . ? C54 O54 1.358(4) . ? O50 C55 1.431(4) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? O54 C56 1.426(4) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 Cl2 91.46(9) . . ? C1 Pd1 Cl1 88.61(9) . . ? Cl2 Pd1 Cl1 179.87(4) . . ? C1 Pd1 P1 174.73(9) . . ? Cl2 Pd1 P1 88.74(3) . . ? Cl1 Pd1 P1 91.20(3) . . ? N5 C1 N2 104.1(3) . . ? N5 C1 Pd1 129.7(2) . . ? N2 C1 Pd1 126.0(2) . . ? C1 N2 C3 111.3(3) . . ? C1 N2 C6 125.9(3) . . ? C3 N2 C6 122.8(3) . . ? C4 C3 N2 106.8(3) . . ? C4 C3 H3A 126.6 . . ? N2 C3 H3A 126.6 . . ? C3 C4 N5 106.5(3) . . ? C3 C4 H4A 126.8 . . ? N5 C4 H4A 126.8 . . ? C1 N5 C4 111.3(3) . . ? C1 N5 C18 128.0(3) . . ? C4 N5 C18 120.7(3) . . ? C7 C6 C11 122.9(3) . . ? C7 C6 N2 118.7(3) . . ? C11 C6 N2 118.3(3) . . ? C8 C7 C6 117.1(3) . . ? C8 C7 C12 120.8(3) . . ? C6 C7 C12 122.0(3) . . ? C9 C8 C7 121.5(3) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 121.5(3) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C6 117.0(3) . . ? C10 C11 C15 120.6(3) . . ? C6 C11 C15 122.3(3) . . ? C13 C12 C7 113.3(4) . . ? C13 C12 C14 111.0(3) . . ? C7 C12 C14 109.9(3) . . ? C13 C12 H12A 107.4 . . ? C7 C12 H12A 107.4 . . ? C14 C12 H12A 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 113.0(3) . . ? C11 C15 C17 110.9(3) . . ? C16 C15 C17 109.1(3) . . ? C11 C15 H15A 107.9 . . ? C16 C15 H15A 107.9 . . ? C17 C15 H15A 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 123.9(3) . . ? C19 C18 N5 118.3(3) . . ? C23 C18 N5 117.4(3) . . ? C18 C19 C20 115.4(4) . . ? C18 C19 C24 122.9(3) . . ? C20 C19 C24 121.6(4) . . ? C21 C20 C19 120.1(4) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 122.5(4) . . ? C22 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C22 C23 C18 117.5(4) . . ? C22 C23 C27 120.6(4) . . ? C18 C23 C27 121.9(3) . . ? C19 C24 C26 109.1(3) . . ? C19 C24 C25 111.4(4) . . ? C26 C24 C25 110.8(4) . . ? C19 C24 H24A 108.5 . . ? C26 C24 H24A 108.5 . . ? C25 C24 H24A 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 113.6(4) . . ? C23 C27 C29 113.0(3) . . ? C28 C27 C29 108.4(4) . . ? C23 C27 H27A 107.1 . . ? C28 C27 H27A 107.1 . . ? C29 C27 H27A 107.1 . . ? 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 . . ? C31 P1 C43 103.83(15) . . ? C31 P1 C37 105.58(15) . . ? C43 P1 C37 111.04(14) . . ? C31 P1 Pd1 113.89(11) . . ? C43 P1 Pd1 114.62(10) . . ? C37 P1 Pd1 107.55(11) . . ? C36 C31 C32 110.2(3) . . ? C36 C31 P1 114.3(2) . . ? C32 C31 P1 113.1(2) . . ? C36 C31 H31A 106.2 . . ? C32 C31 H31A 106.2 . . ? P1 C31 H31A 106.2 . . ? C33 C32 C31 110.0(3) . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 111.2(3) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.7(3) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.2(3) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 110.9(3) . . ? C35 C36 H36A 109.5 . . ? C31 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 108.0 . . ? C42 C37 C38 109.6(3) . . ? C42 C37 P1 110.4(2) . . ? C38 C37 P1 112.0(2) . . ? C42 C37 H37A 108.2 . . ? C38 C37 H37A 108.2 . . ? P1 C37 H37A 108.2 . . ? C39 C38 C37 109.5(3) . . ? C39 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? C39 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? C40 C39 C38 111.6(3) . . ? C40 C39 H39A 109.3 . . ? C38 C39 H39A 109.3 . . ? C40 C39 H39B 109.3 . . ? C38 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C39 111.7(3) . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C40 C41 C42 111.6(3) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 111.2(3) . . ? C37 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? C37 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C48 118.0(3) . . ? C44 C43 P1 130.6(2) . . ? C48 C43 P1 111.3(2) . . ? C45 C44 C43 118.7(3) . . ? C45 C44 C49 114.6(3) . . ? C43 C44 C49 126.6(3) . . ? C46 C45 C44 122.4(3) . . ? C46 C45 H45A 118.8 . . ? C44 C45 H45A 118.8 . . ? C47 C46 C45 119.1(3) . . ? C47 C46 H46A 120.4 . . ? C45 C46 H46A 120.4 . . ? C46 C47 C48 119.8(3) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C47 C48 C43 122.0(3) . . ? C47 C48 H48A 119.0 . . ? C43 C48 H48A 119.0 . . ? C54 C49 C50 118.5(3) . . ? C54 C49 C44 119.7(3) . . ? C50 C49 C44 121.5(3) . . ? O50 C50 C49 115.6(3) . . ? O50 C50 C51 123.4(3) . . ? C49 C50 C51 120.9(3) . . ? C52 C51 C50 118.5(3) . . ? C52 C51 H51A 120.7 . . ? C50 C51 H51A 120.7 . . ? C51 C52 C53 122.0(3) . . ? C51 C52 H52A 119.0 . . ? C53 C52 H52A 119.0 . . ? C52 C53 C54 118.9(3) . . ? C52 C53 H53A 120.5 . . ? C54 C53 H53A 120.5 . . ? O54 C54 C49 115.1(3) . . ? O54 C54 C53 124.1(3) . . ? C49 C54 C53 120.8(3) . . ? C50 O50 C55 119.1(3) . . ? O50 C55 H55A 109.5 . . ? O50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 O54 C56 118.5(3) . . ? O54 C56 H56A 109.5 . . ? O54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pd1 C1 N5 -85.8(3) . . . . ? Cl1 Pd1 C1 N5 94.1(3) . . . . ? P1 Pd1 C1 N5 -177.9(7) . . . . ? Cl2 Pd1 C1 N2 99.4(3) . . . . ? Cl1 Pd1 C1 N2 -80.7(3) . . . . ? P1 Pd1 C1 N2 7.3(12) . . . . ? N5 C1 N2 C3 -1.4(4) . . . . ? Pd1 C1 N2 C3 174.5(2) . . . . ? N5 C1 N2 C6 176.2(3) . . . . ? Pd1 C1 N2 C6 -7.9(4) . . . . ? C1 N2 C3 C4 0.0(4) . . . . ? C6 N2 C3 C4 -177.6(3) . . . . ? N2 C3 C4 N5 1.3(4) . . . . ? N2 C1 N5 C4 2.2(4) . . . . ? Pd1 C1 N5 C4 -173.5(2) . . . . ? N2 C1 N5 C18 -177.1(3) . . . . ? Pd1 C1 N5 C18 7.2(5) . . . . ? C3 C4 N5 C1 -2.2(4) . . . . ? C3 C4 N5 C18 177.1(3) . . . . ? C1 N2 C6 C7 -81.8(4) . . . . ? C3 N2 C6 C7 95.4(4) . . . . ? C1 N2 C6 C11 100.7(4) . . . . ? C3 N2 C6 C11 -82.0(4) . . . . ? C11 C6 C7 C8 -1.8(5) . . . . ? N2 C6 C7 C8 -179.1(3) . . . . ? C11 C6 C7 C12 174.9(3) . . . . ? N2 C6 C7 C12 -2.4(5) . . . . ? C6 C7 C8 C9 1.1(5) . . . . ? C12 C7 C8 C9 -175.6(3) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C8 C9 C10 C11 -1.1(6) . . . . ? C9 C10 C11 C6 0.4(5) . . . . ? C9 C10 C11 C15 178.0(3) . . . . ? C7 C6 C11 C10 1.0(5) . . . . ? N2 C6 C11 C10 178.4(3) . . . . ? C7 C6 C11 C15 -176.5(3) . . . . ? N2 C6 C11 C15 0.9(5) . . . . ? C8 C7 C12 C13 -35.5(5) . . . . ? C6 C7 C12 C13 147.9(4) . . . . ? C8 C7 C12 C14 89.4(4) . . . . ? C6 C7 C12 C14 -87.2(4) . . . . ? C10 C11 C15 C16 42.0(4) . . . . ? C6 C11 C15 C16 -140.5(3) . . . . ? C10 C11 C15 C17 -80.9(4) . . . . ? C6 C11 C15 C17 96.6(4) . . . . ? C1 N5 C18 C19 -95.5(4) . . . . ? C4 N5 C18 C19 85.3(4) . . . . ? C1 N5 C18 C23 91.4(4) . . . . ? C4 N5 C18 C23 -87.8(4) . . . . ? C23 C18 C19 C20 1.4(5) . . . . ? N5 C18 C19 C20 -171.3(3) . . . . ? C23 C18 C19 C24 179.7(3) . . . . ? N5 C18 C19 C24 7.0(5) . . . . ? C18 C19 C20 C21 0.0(6) . . . . ? C24 C19 C20 C21 -178.3(4) . . . . ? C19 C20 C21 C22 -0.5(7) . . . . ? C20 C21 C22 C23 -0.5(7) . . . . ? C21 C22 C23 C18 1.8(6) . . . . ? C21 C22 C23 C27 -179.4(4) . . . . ? C19 C18 C23 C22 -2.3(5) . . . . ? N5 C18 C23 C22 170.4(3) . . . . ? C19 C18 C23 C27 179.0(3) . . . . ? N5 C18 C23 C27 -8.3(5) . . . . ? C18 C19 C24 C26 -108.3(5) . . . . ? C20 C19 C24 C26 69.9(5) . . . . ? C18 C19 C24 C25 129.2(4) . . . . ? C20 C19 C24 C25 -52.6(5) . . . . ? C22 C23 C27 C28 34.4(5) . . . . ? C18 C23 C27 C28 -147.0(4) . . . . ? C22 C23 C27 C29 -89.8(5) . . . . ? C18 C23 C27 C29 88.9(4) . . . . ? C1 Pd1 P1 C31 -114.6(9) . . . . ? Cl2 Pd1 P1 C31 153.17(12) . . . . ? Cl1 Pd1 P1 C31 -26.71(12) . . . . ? C1 Pd1 P1 C43 126.0(9) . . . . ? Cl2 Pd1 P1 C43 33.79(11) . . . . ? Cl1 Pd1 P1 C43 -146.09(11) . . . . ? C1 Pd1 P1 C37 2.0(10) . . . . ? Cl2 Pd1 P1 C37 -90.20(11) . . . . ? Cl1 Pd1 P1 C37 89.91(11) . . . . ? C43 P1 C31 C36 -61.2(3) . . . . ? C37 P1 C31 C36 55.7(3) . . . . ? Pd1 P1 C31 C36 173.5(2) . . . . ? C43 P1 C31 C32 66.1(3) . . . . ? C37 P1 C31 C32 -177.0(2) . . . . ? Pd1 P1 C31 C32 -59.3(3) . . . . ? C36 C31 C32 C33 -57.1(4) . . . . ? P1 C31 C32 C33 173.5(2) . . . . ? C31 C32 C33 C34 57.5(4) . . . . ? C32 C33 C34 C35 -57.2(4) . . . . ? C33 C34 C35 C36 56.2(4) . . . . ? C34 C35 C36 C31 -56.4(4) . . . . ? C32 C31 C36 C35 56.6(4) . . . . ? P1 C31 C36 C35 -174.7(3) . . . . ? C31 P1 C37 C42 165.4(2) . . . . ? C43 P1 C37 C42 -82.7(3) . . . . ? Pd1 P1 C37 C42 43.5(2) . . . . ? C31 P1 C37 C38 43.0(3) . . . . ? C43 P1 C37 C38 154.9(2) . . . . ? Pd1 P1 C37 C38 -79.0(2) . . . . ? C42 C37 C38 C39 58.6(4) . . . . ? P1 C37 C38 C39 -178.5(2) . . . . ? C37 C38 C39 C40 -57.3(4) . . . . ? C38 C39 C40 C41 54.8(4) . . . . ? C39 C40 C41 C42 -53.3(5) . . . . ? C38 C37 C42 C41 -58.1(4) . . . . ? P1 C37 C42 C41 178.0(3) . . . . ? C40 C41 C42 C37 55.5(4) . . . . ? C31 P1 C43 C44 96.5(3) . . . . ? C37 P1 C43 C44 -16.5(3) . . . . ? Pd1 P1 C43 C44 -138.6(3) . . . . ? C31 P1 C43 C48 -80.4(2) . . . . ? C37 P1 C43 C48 166.6(2) . . . . ? Pd1 P1 C43 C48 44.5(2) . . . . ? C48 C43 C44 C45 1.8(4) . . . . ? P1 C43 C44 C45 -174.9(2) . . . . ? C48 C43 C44 C49 -175.7(3) . . . . ? P1 C43 C44 C49 7.6(5) . . . . ? C43 C44 C45 C46 -0.2(5) . . . . ? C49 C44 C45 C46 177.6(3) . . . . ? C44 C45 C46 C47 -1.1(5) . . . . ? C45 C46 C47 C48 0.7(5) . . . . ? C46 C47 C48 C43 1.0(5) . . . . ? C44 C43 C48 C47 -2.2(5) . . . . ? P1 C43 C48 C47 175.1(3) . . . . ? C45 C44 C49 C54 -87.3(4) . . . . ? C43 C44 C49 C54 90.2(4) . . . . ? C45 C44 C49 C50 86.2(4) . . . . ? C43 C44 C49 C50 -96.2(4) . . . . ? C54 C49 C50 O50 172.3(3) . . . . ? C44 C49 C50 O50 -1.4(4) . . . . ? C54 C49 C50 C51 -6.3(5) . . . . ? C44 C49 C50 C51 -179.9(3) . . . . ? O50 C50 C51 C52 -174.4(3) . . . . ? C49 C50 C51 C52 4.1(5) . . . . ? C50 C51 C52 C53 0.6(5) . . . . ? C51 C52 C53 C54 -2.8(6) . . . . ? C50 C49 C54 O54 -174.6(3) . . . . ? C44 C49 C54 O54 -0.9(4) . . . . ? C50 C49 C54 C53 4.0(5) . . . . ? C44 C49 C54 C53 177.8(3) . . . . ? C52 C53 C54 O54 178.9(3) . . . . ? C52 C53 C54 C49 0.4(5) . . . . ? C49 C50 O50 C55 173.8(3) . . . . ? C51 C50 O50 C55 -7.6(4) . . . . ? C49 C54 O54 C56 -172.6(3) . . . . ? C53 C54 O54 C56 8.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.044 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.100 data_6 _database_code_depnum_ccdc_archive 'CCDC 871889' #TrackingRef '10177_web_deposit_cif_file_7_CatherineS.J.Cazin_1331897901.6.cif' # start Validation Reply Form _vrf_PLAT973_6 ; PROBLEM: Large Calcd. Positive Residual Density on Pd1 2.11 eA-3 RESPONSE: Poor quality crystal. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H71 N2 O2 P Pd' _chemical_formula_sum 'C53 H71 N2 O2 P Pd' _chemical_formula_weight 905.49 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' 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 17.831(2) _cell_length_b 14.5302(19) _cell_length_c 18.802(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.784(5) _cell_angle_gamma 90.00 _cell_volume 4800.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 16525 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 28.49 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5095 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25152 _diffrn_reflns_av_R_equivalents 0.2327 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8670 _reflns_number_gt 6800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+48.3915P] 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 8670 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2548 _refine_ls_wR_factor_gt 0.2141 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.53816(4) 0.20324(3) 0.23687(3) 0.0224(2) Uani 1 1 d . . . C1 C 0.5961(5) 0.3035(4) 0.1950(4) 0.0244(17) Uani 1 1 d . . . N2 N 0.6210(4) 0.3138(4) 0.1304(3) 0.0230(14) Uani 1 1 d . . . C3 C 0.6582(5) 0.3964(5) 0.1248(4) 0.0285(18) Uani 1 1 d . . . H3A H 0.6784 0.4179 0.0842 0.034 Uiso 1 1 calc R . . C4 C 0.6601(5) 0.4402(5) 0.1876(4) 0.0288(18) Uani 1 1 d . . . H4A H 0.6823 0.4985 0.2008 0.035 Uiso 1 1 calc R . . N5 N 0.6231(3) 0.3835(4) 0.2297(3) 0.0170(12) Uani 1 1 d . . . C6 C 0.6083(5) 0.2449(5) 0.0738(3) 0.0235(16) Uani 1 1 d . . . C7 C 0.5434(5) 0.2516(5) 0.0222(4) 0.0273(17) Uani 1 1 d . . . C8 C 0.5302(5) 0.1800(6) -0.0288(4) 0.037(2) Uani 1 1 d . . . H8A H 0.4859 0.1812 -0.0649 0.044 Uiso 1 1 calc R . . C9 C 0.5810(6) 0.1080(6) -0.0268(4) 0.043(2) Uani 1 1 d . . . H9A H 0.5702 0.0587 -0.0602 0.051 Uiso 1 1 calc R . . C10 C 0.6469(6) 0.1068(5) 0.0228(4) 0.037(2) Uani 1 1 d . . . H10A H 0.6824 0.0584 0.0219 0.044 Uiso 1 1 calc R . . C11 C 0.6623(5) 0.1760(5) 0.0746(4) 0.0275(18) Uani 1 1 d . . . C12 C 0.4882(5) 0.3320(6) 0.0194(5) 0.035(2) Uani 1 1 d . . . H12A H 0.5135 0.3801 0.0533 0.042 Uiso 1 1 calc R . . C13 C 0.4712(7) 0.3760(7) -0.0559(5) 0.057(3) Uani 1 1 d . . . H13A H 0.5191 0.3931 -0.0714 0.085 Uiso 1 1 calc R . . H13B H 0.4399 0.4312 -0.0542 0.085 Uiso 1 1 calc R . . H13C H 0.4438 0.3319 -0.0903 0.085 Uiso 1 1 calc R . . C14 C 0.4133(6) 0.3041(7) 0.0461(5) 0.046(2) Uani 1 1 d . . . H14A H 0.4256 0.2765 0.0942 0.069 Uiso 1 1 calc R . . H14B H 0.3855 0.2593 0.0125 0.069 Uiso 1 1 calc R . . H14C H 0.3816 0.3588 0.0482 0.069 Uiso 1 1 calc R . . C15 C 0.7367(5) 0.1761(5) 0.1298(4) 0.0288(18) Uani 1 1 d . . . H15A H 0.7459 0.2408 0.1472 0.035 Uiso 1 1 calc R . . C16 C 0.8047(6) 0.1470(8) 0.0980(6) 0.053(3) Uani 1 1 d . . . H16A H 0.8091 0.1861 0.0565 0.080 Uiso 1 1 calc R . . H16B H 0.7986 0.0827 0.0824 0.080 Uiso 1 1 calc R . . H16C H 0.8507 0.1531 0.1345 0.080 Uiso 1 1 calc R . . C17 C 0.7274(7) 0.1170(6) 0.1956(5) 0.047(3) Uani 1 1 d . . . H17A H 0.7749 0.1177 0.2305 0.070 Uiso 1 1 calc R . . H17B H 0.7152 0.0536 0.1800 0.070 Uiso 1 1 calc R . . H17C H 0.6861 0.1420 0.2182 0.070 Uiso 1 1 calc R . . C18 C 0.6074(5) 0.4055(4) 0.3013(4) 0.0236(16) Uani 1 1 d . . . C19 C 0.6582(5) 0.3708(5) 0.3608(4) 0.0298(18) Uani 1 1 d . . . C20 C 0.6426(6) 0.3930(6) 0.4290(4) 0.037(2) Uani 1 1 d . . . H20A H 0.6750 0.3705 0.4707 0.044 Uiso 1 1 calc R . . C21 C 0.5802(6) 0.4476(5) 0.4368(4) 0.037(2) Uani 1 1 d . . . H21A H 0.5710 0.4627 0.4837 0.044 Uiso 1 1 calc R . . C22 C 0.5320(5) 0.4797(5) 0.3768(4) 0.0334(19) Uani 1 1 d . . . H22A H 0.4894 0.5162 0.3830 0.040 Uiso 1 1 calc R . . C23 C 0.5445(5) 0.4595(5) 0.3070(4) 0.0302(18) Uani 1 1 d . . . C24 C 0.7251(6) 0.3105(5) 0.3531(4) 0.035(2) Uani 1 1 d . . . H24A H 0.7278 0.3063 0.3005 0.042 Uiso 1 1 calc R . . C25 C 0.8004(5) 0.3508(6) 0.3914(5) 0.041(2) Uani 1 1 d . . . H25A H 0.8065 0.4132 0.3734 0.061 Uiso 1 1 calc R . . H25B H 0.8425 0.3121 0.3818 0.061 Uiso 1 1 calc R . . H25C H 0.8003 0.3531 0.4435 0.061 Uiso 1 1 calc R . . C26 C 0.7148(6) 0.2130(6) 0.3802(5) 0.043(2) Uani 1 1 d . . . H26A H 0.6664 0.1877 0.3553 0.064 Uiso 1 1 calc R . . H26B H 0.7145 0.2146 0.4323 0.064 Uiso 1 1 calc R . . H26C H 0.7568 0.1741 0.3705 0.064 Uiso 1 1 calc R . . C27 C 0.4887(5) 0.4884(5) 0.2404(5) 0.0349(19) Uani 1 1 d . . . H27A H 0.5148 0.4828 0.1976 0.042 Uiso 1 1 calc R . . C28 C 0.4635(6) 0.5878(6) 0.2456(6) 0.047(2) Uani 1 1 d . . . H28A H 0.5081 0.6283 0.2512 0.071 Uiso 1 1 calc R . . H28B H 0.4377 0.5948 0.2873 0.071 Uiso 1 1 calc R . . H28C H 0.4284 0.6044 0.2015 0.071 Uiso 1 1 calc R . . C29 C 0.4209(6) 0.4220(5) 0.2302(5) 0.041(2) Uani 1 1 d . . . H29A H 0.4392 0.3589 0.2264 0.062 Uiso 1 1 calc R . . H29B H 0.3858 0.4380 0.1859 0.062 Uiso 1 1 calc R . . H29C H 0.3944 0.4266 0.2716 0.062 Uiso 1 1 calc R . . P1 P 0.46592(12) 0.10592(12) 0.28907(9) 0.0226(4) Uani 1 1 d . . . C31 C 0.4978(5) -0.0165(5) 0.2996(4) 0.0253(17) Uani 1 1 d . . . H31A H 0.4754 -0.0447 0.3398 0.030 Uiso 1 1 calc R . . C32 C 0.4722(5) -0.0726(5) 0.2310(4) 0.0325(19) Uani 1 1 d . . . H32A H 0.4918 -0.0436 0.1901 0.039 Uiso 1 1 calc R . . H32B H 0.4160 -0.0730 0.2194 0.039 Uiso 1 1 calc R . . C33 C 0.5014(6) -0.1718(5) 0.2404(5) 0.040(2) Uani 1 1 d . . . H33A H 0.4785 -0.2022 0.2787 0.048 Uiso 1 1 calc R . . H33B H 0.4854 -0.2061 0.1949 0.048 Uiso 1 1 calc R . . C34 C 0.5868(6) -0.1752(6) 0.2603(5) 0.044(2) Uani 1 1 d . . . H34A H 0.6098 -0.1510 0.2197 0.052 Uiso 1 1 calc R . . H34B H 0.6032 -0.2399 0.2686 0.052 Uiso 1 1 calc R . . C35 C 0.6155(5) -0.1192(5) 0.3278(5) 0.037(2) Uani 1 1 d . . . H35A H 0.6718 -0.1180 0.3365 0.044 Uiso 1 1 calc R . . H35B H 0.5988 -0.1485 0.3700 0.044 Uiso 1 1 calc R . . C36 C 0.5848(5) -0.0205(5) 0.3194(5) 0.0328(19) Uani 1 1 d . . . H36A H 0.6074 0.0110 0.2814 0.039 Uiso 1 1 calc R . . H36B H 0.6010 0.0131 0.3652 0.039 Uiso 1 1 calc R . . C37 C 0.4510(5) 0.1396(5) 0.3807(4) 0.0226(15) Uani 1 1 d . . . H37A H 0.4063 0.1046 0.3922 0.027 Uiso 1 1 calc R . . C38 C 0.4317(5) 0.2428(5) 0.3803(4) 0.0297(18) Uani 1 1 d . . . H38A H 0.3862 0.2547 0.3433 0.036 Uiso 1 1 calc R . . H38B H 0.4746 0.2785 0.3672 0.036 Uiso 1 1 calc R . . C39 C 0.4160(7) 0.2758(6) 0.4546(4) 0.043(2) Uani 1 1 d . . . H39A H 0.4070 0.3431 0.4532 0.051 Uiso 1 1 calc R . . H39B H 0.3697 0.2453 0.4656 0.051 Uiso 1 1 calc R . . C40 C 0.4835(6) 0.2533(6) 0.5137(4) 0.039(2) Uani 1 1 d . . . H40A H 0.5284 0.2896 0.5058 0.047 Uiso 1 1 calc R . . H40B H 0.4711 0.2707 0.5613 0.047 Uiso 1 1 calc R . . C41 C 0.5024(6) 0.1509(6) 0.5135(4) 0.037(2) Uani 1 1 d . . . H41A H 0.4590 0.1151 0.5256 0.045 Uiso 1 1 calc R . . H41B H 0.5473 0.1383 0.5510 0.045 Uiso 1 1 calc R . . C42 C 0.5190(5) 0.1199(5) 0.4397(4) 0.0301(18) Uani 1 1 d . . . H42A H 0.5643 0.1530 0.4288 0.036 Uiso 1 1 calc R . . H42B H 0.5303 0.0532 0.4410 0.036 Uiso 1 1 calc R . . C43 C 0.3693(4) 0.0927(4) 0.2345(4) 0.0205(15) Uani 1 1 d . . . C44 C 0.3000(5) 0.0630(5) 0.2531(4) 0.0266(17) Uani 1 1 d . . . C45 C 0.2380(5) 0.0485(6) 0.1995(4) 0.038(2) Uani 1 1 d . . . H45A H 0.1917 0.0280 0.2126 0.045 Uiso 1 1 calc R . . C46 C 0.2409(5) 0.0625(6) 0.1273(4) 0.038(2) Uani 1 1 d . . . H46A H 0.1972 0.0519 0.0917 0.046 Uiso 1 1 calc R . . C47 C 0.3078(6) 0.0922(6) 0.1077(4) 0.036(2) Uani 1 1 d . . . H47A H 0.3106 0.1017 0.0583 0.043 Uiso 1 1 calc R . . C48 C 0.3708(6) 0.1082(5) 0.1601(4) 0.0326(19) Uani 1 1 d . . . H48A H 0.4163 0.1301 0.1460 0.039 Uiso 1 1 calc R . . C49 C 0.2858(4) 0.0432(5) 0.3287(4) 0.0240(16) Uani 1 1 d . . . C50 C 0.2561(5) 0.1106(5) 0.3682(4) 0.0325(18) Uani 1 1 d . . . O50 O 0.2428(4) 0.1934(4) 0.3339(3) 0.0387(15) Uani 1 1 d . . . C51 C 0.2418(6) 0.0929(6) 0.4370(5) 0.047(3) Uani 1 1 d . . . H51A H 0.2218 0.1395 0.4639 0.057 Uiso 1 1 calc R . . C52 C 0.2572(7) 0.0054(7) 0.4661(5) 0.053(3) Uani 1 1 d . . . H52A H 0.2492 -0.0067 0.5139 0.063 Uiso 1 1 calc R . . C53 C 0.2837(6) -0.0635(6) 0.4272(4) 0.039(2) Uani 1 1 d . . . H53A H 0.2927 -0.1233 0.4474 0.047 Uiso 1 1 calc R . . C54 C 0.2972(5) -0.0453(5) 0.3579(4) 0.034(2) Uani 1 1 d . . . O54 O 0.3220(4) -0.1101(3) 0.3147(3) 0.0322(13) Uani 1 1 d . . . C55 C 0.2081(6) 0.2648(6) 0.3702(5) 0.044(2) Uani 1 1 d . . . H55A H 0.2018 0.3202 0.3401 0.066 Uiso 1 1 calc R . . H55B H 0.2407 0.2788 0.4164 0.066 Uiso 1 1 calc R . . H55C H 0.1582 0.2439 0.3790 0.066 Uiso 1 1 calc R . . C56 C 0.3124(7) -0.2048(5) 0.3337(5) 0.046(3) Uani 1 1 d . . . H56A H 0.3321 -0.2449 0.2992 0.070 Uiso 1 1 calc R . . H56B H 0.2583 -0.2175 0.3324 0.070 Uiso 1 1 calc R . . H56C H 0.3404 -0.2164 0.3824 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0324(4) 0.0151(3) 0.0191(3) 0.00072(19) 0.0025(2) -0.0035(2) C1 0.039(5) 0.012(3) 0.018(3) 0.001(2) -0.008(3) 0.001(3) N2 0.032(4) 0.015(3) 0.019(3) -0.001(2) -0.001(3) 0.000(2) C3 0.040(5) 0.017(3) 0.026(4) 0.005(3) -0.002(3) -0.005(3) C4 0.040(5) 0.019(3) 0.026(4) 0.000(3) 0.001(3) -0.006(3) N5 0.007(3) 0.019(3) 0.025(3) 0.002(2) 0.004(2) -0.002(2) C6 0.040(5) 0.020(3) 0.012(3) -0.001(3) 0.007(3) -0.004(3) C7 0.034(5) 0.027(4) 0.021(3) 0.004(3) 0.005(3) -0.004(3) C8 0.036(5) 0.043(5) 0.029(4) -0.002(3) -0.006(4) -0.007(4) C9 0.064(7) 0.031(4) 0.030(4) -0.015(3) -0.001(4) 0.000(4) C10 0.058(6) 0.023(4) 0.028(4) -0.005(3) 0.006(4) 0.004(4) C11 0.039(5) 0.017(3) 0.025(4) 0.003(3) 0.000(3) 0.000(3) C12 0.031(5) 0.031(4) 0.039(5) 0.006(3) -0.007(4) 0.000(3) C13 0.066(8) 0.050(6) 0.050(6) 0.022(5) -0.004(5) 0.019(5) C14 0.043(6) 0.046(5) 0.048(5) -0.002(4) 0.007(5) 0.003(4) C15 0.033(5) 0.022(3) 0.029(4) 0.000(3) 0.000(3) 0.008(3) C16 0.044(6) 0.067(7) 0.047(5) -0.003(5) 0.005(5) 0.012(5) C17 0.067(7) 0.032(4) 0.036(5) 0.006(4) -0.006(5) 0.008(4) C18 0.036(5) 0.016(3) 0.020(3) -0.003(3) 0.008(3) -0.001(3) C19 0.043(5) 0.020(3) 0.023(4) -0.004(3) -0.003(3) -0.003(3) C20 0.049(6) 0.033(4) 0.024(4) -0.004(3) -0.005(4) -0.003(4) C21 0.053(6) 0.031(4) 0.027(4) -0.008(3) 0.006(4) -0.008(4) C22 0.039(5) 0.026(4) 0.039(4) -0.006(3) 0.017(4) -0.003(3) C23 0.045(5) 0.016(3) 0.031(4) -0.002(3) 0.011(4) -0.001(3) C24 0.053(6) 0.030(4) 0.018(3) 0.001(3) -0.004(4) 0.007(4) C25 0.036(5) 0.046(5) 0.037(4) -0.004(4) -0.001(4) 0.002(4) C26 0.045(6) 0.034(4) 0.048(5) 0.006(4) 0.005(4) 0.002(4) C27 0.033(5) 0.028(4) 0.042(5) 0.002(3) 0.002(4) 0.014(3) C28 0.039(6) 0.026(4) 0.075(7) 0.010(4) 0.005(5) 0.009(4) C29 0.043(6) 0.024(4) 0.054(5) -0.008(4) 0.000(4) 0.013(4) P1 0.0333(11) 0.0157(8) 0.0176(8) 0.0007(6) 0.0006(8) -0.0032(7) C31 0.037(5) 0.019(3) 0.019(3) 0.000(3) 0.003(3) -0.002(3) C32 0.046(5) 0.023(4) 0.025(4) -0.003(3) -0.003(4) 0.000(3) C33 0.063(7) 0.023(4) 0.032(4) -0.006(3) 0.006(4) 0.004(4) C34 0.062(7) 0.028(4) 0.045(5) 0.003(4) 0.018(5) 0.015(4) C35 0.035(5) 0.026(4) 0.051(5) 0.006(4) 0.010(4) 0.009(3) C36 0.028(5) 0.025(4) 0.043(5) 0.001(3) 0.000(4) 0.004(3) C37 0.029(4) 0.024(3) 0.016(3) -0.003(3) 0.008(3) -0.004(3) C38 0.039(5) 0.026(4) 0.024(4) -0.002(3) 0.004(3) 0.002(3) C39 0.068(7) 0.031(4) 0.029(4) -0.009(3) 0.010(4) 0.004(4) C40 0.055(6) 0.042(5) 0.021(4) -0.009(3) 0.011(4) -0.017(4) C41 0.052(6) 0.039(4) 0.019(4) 0.002(3) 0.001(4) -0.014(4) C42 0.037(5) 0.028(4) 0.025(4) 0.004(3) 0.005(3) -0.008(3) C43 0.019(4) 0.017(3) 0.025(3) 0.001(3) 0.004(3) -0.001(3) C44 0.037(5) 0.020(3) 0.022(4) -0.001(3) 0.001(3) 0.000(3) C45 0.035(5) 0.041(5) 0.034(4) 0.005(4) -0.003(4) -0.008(4) C46 0.031(5) 0.049(5) 0.029(4) 0.007(4) -0.010(4) -0.007(4) C47 0.048(6) 0.039(4) 0.018(4) 0.004(3) -0.003(4) -0.005(4) C48 0.051(6) 0.022(3) 0.022(4) 0.003(3) -0.001(4) 0.001(3) C49 0.020(4) 0.030(4) 0.023(3) 0.003(3) 0.006(3) -0.008(3) C50 0.038(5) 0.027(4) 0.031(4) 0.001(3) 0.002(4) 0.001(3) O50 0.054(4) 0.027(3) 0.034(3) 0.003(2) 0.006(3) 0.011(3) C51 0.068(7) 0.037(5) 0.038(5) -0.001(4) 0.012(5) 0.010(5) C52 0.081(8) 0.046(5) 0.032(5) 0.010(4) 0.012(5) 0.007(5) C53 0.054(6) 0.031(4) 0.031(4) 0.009(3) 0.006(4) 0.002(4) C54 0.038(5) 0.026(4) 0.032(4) 0.000(3) -0.009(4) -0.002(3) O54 0.046(4) 0.024(3) 0.029(3) 0.003(2) 0.012(3) -0.004(2) C55 0.046(6) 0.038(5) 0.044(5) -0.007(4) -0.001(4) 0.016(4) C56 0.078(8) 0.020(4) 0.036(4) 0.001(3) -0.007(5) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.022(8) . ? Pd1 P1 2.248(2) . ? C1 N2 1.371(10) . ? C1 N5 1.379(8) . ? N2 C3 1.384(9) . ? N2 C6 1.451(8) . ? C3 C4 1.338(11) . ? C3 H3A 0.9500 . ? C4 N5 1.385(10) . ? C4 H4A 0.9500 . ? N5 C18 1.456(9) . ? C6 C11 1.387(11) . ? C6 C7 1.382(11) . ? C7 C8 1.407(11) . ? C7 C12 1.523(12) . ? C8 C9 1.380(13) . ? C8 H8A 0.9500 . ? C9 C10 1.369(13) . ? C9 H9A 0.9500 . ? C10 C11 1.394(10) . ? C10 H10A 0.9500 . ? C11 C15 1.539(11) . ? C12 C13 1.536(12) . ? C12 C14 1.559(14) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.501(14) . ? C15 C17 1.539(12) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.388(12) . ? C18 C19 1.407(10) . ? C19 C20 1.394(12) . ? C19 C24 1.506(12) . ? C20 C21 1.394(13) . ? C20 H20A 0.9500 . ? C21 C22 1.378(12) . ? C21 H21A 0.9500 . ? C22 C23 1.399(11) . ? C22 H22A 0.9500 . ? C23 C27 1.520(11) . ? C24 C25 1.528(12) . ? C24 C26 1.528(11) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.520(11) . ? C27 C29 1.533(13) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 C37 1.854(7) . ? P1 C43 1.859(7) . ? P1 C31 1.867(7) . ? C31 C32 1.530(9) . ? C31 C36 1.533(11) . ? C31 H31A 1.0000 . ? C32 C33 1.531(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.505(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.521(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.533(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.537(10) . ? C37 C42 1.525(10) . ? C37 H37A 1.0000 . ? C38 C39 1.547(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.528(13) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.525(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.536(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.410(11) . ? C43 C48 1.420(10) . ? C44 C45 1.379(11) . ? C44 C49 1.511(10) . ? C45 C46 1.381(12) . ? C45 H45A 0.9500 . ? C46 C47 1.376(14) . ? C46 H46A 0.9500 . ? C47 C48 1.382(11) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.387(12) . ? C49 C54 1.400(10) . ? C50 O50 1.368(9) . ? C50 C51 1.385(13) . ? O50 C55 1.438(11) . ? C51 C52 1.392(13) . ? C51 H51A 0.9500 . ? C52 C53 1.370(14) . ? C52 H52A 0.9500 . ? C53 C54 1.390(12) . ? C53 H53A 0.9500 . ? C54 O54 1.365(11) . ? O54 C56 1.439(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 172.9(2) . . ? N2 C1 N5 100.8(6) . . ? N2 C1 Pd1 133.5(5) . . ? N5 C1 Pd1 125.7(5) . . ? C1 N2 C3 113.2(6) . . ? C1 N2 C6 122.7(6) . . ? C3 N2 C6 124.1(6) . . ? C4 C3 N2 106.6(7) . . ? C4 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? C3 C4 N5 106.2(6) . . ? C3 C4 H4A 126.9 . . ? N5 C4 H4A 126.9 . . ? C1 N5 C4 113.1(6) . . ? C1 N5 C18 121.1(6) . . ? C4 N5 C18 125.6(6) . . ? C11 C6 C7 123.7(6) . . ? C11 C6 N2 117.9(6) . . ? C7 C6 N2 118.4(7) . . ? C6 C7 C8 116.7(7) . . ? C6 C7 C12 122.5(7) . . ? C8 C7 C12 120.8(7) . . ? C9 C8 C7 120.6(7) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.7(7) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C11 120.7(8) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C6 C11 C10 117.3(7) . . ? C6 C11 C15 121.6(6) . . ? C10 C11 C15 121.1(7) . . ? C7 C12 C13 112.1(8) . . ? C7 C12 C14 111.9(7) . . ? C13 C12 C14 111.1(8) . . ? C7 C12 H12A 107.2 . . ? C13 C12 H12A 107.2 . . ? C14 C12 H12A 107.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 113.2(7) . . ? C16 C15 C17 111.5(7) . . ? C11 C15 C17 110.1(7) . . ? C16 C15 H15A 107.2 . . ? C11 C15 H15A 107.2 . . ? C17 C15 H15A 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 124.1(7) . . ? C23 C18 N5 118.7(6) . . ? C19 C18 N5 117.2(7) . . ? C20 C19 C18 116.5(8) . . ? C20 C19 C24 120.5(7) . . ? C18 C19 C24 123.0(7) . . ? C21 C20 C19 121.0(7) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C22 C21 C20 120.3(8) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 121.4(8) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C18 C23 C22 116.8(7) . . ? C18 C23 C27 121.1(7) . . ? C22 C23 C27 121.9(8) . . ? C19 C24 C25 112.3(7) . . ? C19 C24 C26 111.4(8) . . ? C25 C24 C26 110.1(7) . . ? C19 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C26 C24 H24A 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 111.7(7) . . ? C23 C27 C29 108.7(7) . . ? C28 C27 C29 111.8(7) . . ? C23 C27 H27A 108.2 . . ? C28 C27 H27A 108.2 . . ? C29 C27 H27A 108.2 . . ? 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 . . ? C37 P1 C43 106.0(4) . . ? C37 P1 C31 104.0(3) . . ? C43 P1 C31 101.4(3) . . ? C37 P1 Pd1 115.0(2) . . ? C43 P1 Pd1 111.7(2) . . ? C31 P1 Pd1 117.3(3) . . ? C32 C31 C36 109.2(7) . . ? C32 C31 P1 112.1(5) . . ? C36 C31 P1 109.8(5) . . ? C32 C31 H31A 108.5 . . ? C36 C31 H31A 108.5 . . ? P1 C31 H31A 108.5 . . ? C31 C32 C33 110.9(6) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 111.7(7) . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C33 C34 C35 111.9(8) . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34B 109.2 . . ? C35 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 C36 110.5(7) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C31 112.9(7) . . ? C35 C36 H36A 109.0 . . ? C31 C36 H36A 109.0 . . ? C35 C36 H36B 109.0 . . ? C31 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? C38 C37 C42 109.6(6) . . ? C38 C37 P1 108.7(5) . . ? C42 C37 P1 113.8(6) . . ? C38 C37 H37A 108.2 . . ? C42 C37 H37A 108.2 . . ? P1 C37 H37A 108.2 . . ? C37 C38 C39 111.9(6) . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C39 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 110.5(8) . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? C38 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C41 C40 C39 110.7(6) . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 111.4(6) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C37 C42 C41 110.5(7) . . ? C37 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C37 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C48 117.2(7) . . ? C44 C43 P1 131.6(5) . . ? C48 C43 P1 110.9(6) . . ? C45 C44 C43 119.5(7) . . ? C45 C44 C49 114.7(8) . . ? C43 C44 C49 125.9(6) . . ? C44 C45 C46 122.5(9) . . ? C44 C45 H45A 118.8 . . ? C46 C45 H45A 118.8 . . ? C47 C46 C45 119.2(7) . . ? C47 C46 H46A 120.4 . . ? C45 C46 H46A 120.4 . . ? C46 C47 C48 119.9(8) . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C47 C48 C43 121.7(9) . . ? C47 C48 H48A 119.1 . . ? C43 C48 H48A 119.1 . . ? C50 C49 C54 118.7(7) . . ? C50 C49 C44 120.6(7) . . ? C54 C49 C44 120.5(7) . . ? O50 C50 C51 124.0(8) . . ? O50 C50 C49 114.8(7) . . ? C51 C50 C49 121.2(7) . . ? C50 O50 C55 117.7(7) . . ? C52 C51 C50 118.7(9) . . ? C52 C51 H51A 120.7 . . ? C50 C51 H51A 120.7 . . ? C53 C52 C51 121.4(9) . . ? C53 C52 H52A 119.3 . . ? C51 C52 H52A 119.3 . . ? C52 C53 C54 119.4(8) . . ? C52 C53 H53A 120.3 . . ? C54 C53 H53A 120.3 . . ? O54 C54 C53 123.5(7) . . ? O54 C54 C49 116.1(7) . . ? C53 C54 C49 120.4(8) . . ? C54 O54 C56 116.5(7) . . ? O50 C55 H55A 109.5 . . ? O50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O54 C56 H56A 109.5 . . ? O54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 C1 N2 -140.2(12) . . . . ? P1 Pd1 C1 N5 41.5(19) . . . . ? N5 C1 N2 C3 -2.4(8) . . . . ? Pd1 C1 N2 C3 179.0(6) . . . . ? N5 C1 N2 C6 178.5(6) . . . . ? Pd1 C1 N2 C6 -0.1(11) . . . . ? C1 N2 C3 C4 2.0(9) . . . . ? C6 N2 C3 C4 -178.8(7) . . . . ? N2 C3 C4 N5 -0.7(9) . . . . ? N2 C1 N5 C4 1.9(8) . . . . ? Pd1 C1 N5 C4 -179.3(5) . . . . ? N2 C1 N5 C18 177.4(6) . . . . ? Pd1 C1 N5 C18 -3.8(9) . . . . ? C3 C4 N5 C1 -0.8(9) . . . . ? C3 C4 N5 C18 -176.1(7) . . . . ? C1 N2 C6 C11 -89.1(9) . . . . ? C3 N2 C6 C11 91.8(9) . . . . ? C1 N2 C6 C7 91.1(8) . . . . ? C3 N2 C6 C7 -87.9(10) . . . . ? C11 C6 C7 C8 4.6(12) . . . . ? N2 C6 C7 C8 -175.6(7) . . . . ? C11 C6 C7 C12 -175.1(8) . . . . ? N2 C6 C7 C12 4.6(11) . . . . ? C6 C7 C8 C9 -0.9(13) . . . . ? C12 C7 C8 C9 178.9(9) . . . . ? C7 C8 C9 C10 -2.9(15) . . . . ? C8 C9 C10 C11 3.1(15) . . . . ? C7 C6 C11 C10 -4.4(12) . . . . ? N2 C6 C11 C10 175.8(7) . . . . ? C7 C6 C11 C15 175.1(7) . . . . ? N2 C6 C11 C15 -4.7(11) . . . . ? C9 C10 C11 C6 0.4(13) . . . . ? C9 C10 C11 C15 -179.1(8) . . . . ? C6 C7 C12 C13 128.4(9) . . . . ? C8 C7 C12 C13 -51.4(11) . . . . ? C6 C7 C12 C14 -106.1(9) . . . . ? C8 C7 C12 C14 74.2(10) . . . . ? C6 C11 C15 C16 -140.0(8) . . . . ? C10 C11 C15 C16 39.4(11) . . . . ? C6 C11 C15 C17 94.4(9) . . . . ? C10 C11 C15 C17 -86.1(10) . . . . ? C1 N5 C18 C23 -93.3(8) . . . . ? C4 N5 C18 C23 81.6(9) . . . . ? C1 N5 C18 C19 87.3(8) . . . . ? C4 N5 C18 C19 -97.7(8) . . . . ? C23 C18 C19 C20 0.2(11) . . . . ? N5 C18 C19 C20 179.6(7) . . . . ? C23 C18 C19 C24 178.6(8) . . . . ? N5 C18 C19 C24 -2.0(11) . . . . ? C18 C19 C20 C21 -0.6(12) . . . . ? C24 C19 C20 C21 -179.1(8) . . . . ? C19 C20 C21 C22 0.9(13) . . . . ? C20 C21 C22 C23 -0.7(13) . . . . ? C19 C18 C23 C22 0.0(11) . . . . ? N5 C18 C23 C22 -179.4(7) . . . . ? C19 C18 C23 C27 -175.2(7) . . . . ? N5 C18 C23 C27 5.4(11) . . . . ? C21 C22 C23 C18 0.3(12) . . . . ? C21 C22 C23 C27 175.4(8) . . . . ? C20 C19 C24 C25 -58.4(10) . . . . ? C18 C19 C24 C25 123.2(8) . . . . ? C20 C19 C24 C26 65.6(10) . . . . ? C18 C19 C24 C26 -112.7(8) . . . . ? C18 C23 C27 C28 -139.2(8) . . . . ? C22 C23 C27 C28 45.8(12) . . . . ? C18 C23 C27 C29 97.0(9) . . . . ? C22 C23 C27 C29 -78.0(9) . . . . ? C1 Pd1 P1 C37 -41.2(16) . . . . ? C1 Pd1 P1 C43 79.7(15) . . . . ? C1 Pd1 P1 C31 -164.0(15) . . . . ? C37 P1 C31 C32 148.3(6) . . . . ? C43 P1 C31 C32 38.5(7) . . . . ? Pd1 P1 C31 C32 -83.4(6) . . . . ? C37 P1 C31 C36 -90.1(6) . . . . ? C43 P1 C31 C36 160.1(5) . . . . ? Pd1 P1 C31 C36 38.2(6) . . . . ? C36 C31 C32 C33 56.2(9) . . . . ? P1 C31 C32 C33 178.1(7) . . . . ? C31 C32 C33 C34 -57.4(10) . . . . ? C32 C33 C34 C35 55.9(10) . . . . ? C33 C34 C35 C36 -53.6(10) . . . . ? C34 C35 C36 C31 54.4(10) . . . . ? C32 C31 C36 C35 -55.7(9) . . . . ? P1 C31 C36 C35 -179.1(6) . . . . ? C43 P1 C37 C38 -78.9(6) . . . . ? C31 P1 C37 C38 174.7(5) . . . . ? Pd1 P1 C37 C38 45.0(6) . . . . ? C43 P1 C37 C42 158.6(5) . . . . ? C31 P1 C37 C42 52.2(6) . . . . ? Pd1 P1 C37 C42 -77.5(5) . . . . ? C42 C37 C38 C39 -56.7(9) . . . . ? P1 C37 C38 C39 178.3(6) . . . . ? C37 C38 C39 C40 55.7(10) . . . . ? C38 C39 C40 C41 -55.1(10) . . . . ? C39 C40 C41 C42 57.0(10) . . . . ? C38 C37 C42 C41 57.3(8) . . . . ? P1 C37 C42 C41 179.3(5) . . . . ? C40 C41 C42 C37 -58.4(9) . . . . ? C37 P1 C43 C44 -32.9(7) . . . . ? C31 P1 C43 C44 75.4(7) . . . . ? Pd1 P1 C43 C44 -158.9(6) . . . . ? C37 P1 C43 C48 153.6(5) . . . . ? C31 P1 C43 C48 -98.1(5) . . . . ? Pd1 P1 C43 C48 27.6(5) . . . . ? C48 C43 C44 C45 1.4(10) . . . . ? P1 C43 C44 C45 -171.8(6) . . . . ? C48 C43 C44 C49 -179.5(7) . . . . ? P1 C43 C44 C49 7.3(11) . . . . ? C43 C44 C45 C46 -0.5(13) . . . . ? C49 C44 C45 C46 -179.6(8) . . . . ? C44 C45 C46 C47 0.0(14) . . . . ? C45 C46 C47 C48 -0.5(13) . . . . ? C46 C47 C48 C43 1.6(13) . . . . ? C44 C43 C48 C47 -2.0(11) . . . . ? P1 C43 C48 C47 172.6(6) . . . . ? C45 C44 C49 C50 -86.8(9) . . . . ? C43 C44 C49 C50 94.1(10) . . . . ? C45 C44 C49 C54 88.6(9) . . . . ? C43 C44 C49 C54 -90.5(9) . . . . ? C54 C49 C50 O50 -176.5(7) . . . . ? C44 C49 C50 O50 -1.0(11) . . . . ? C54 C49 C50 C51 3.5(13) . . . . ? C44 C49 C50 C51 179.0(8) . . . . ? C51 C50 O50 C55 -3.4(13) . . . . ? C49 C50 O50 C55 176.6(8) . . . . ? O50 C50 C51 C52 179.5(9) . . . . ? C49 C50 C51 C52 -0.5(15) . . . . ? C50 C51 C52 C53 -2.2(17) . . . . ? C51 C52 C53 C54 1.6(17) . . . . ? C52 C53 C54 O54 -178.6(9) . . . . ? C52 C53 C54 C49 1.6(14) . . . . ? C50 C49 C54 O54 176.0(7) . . . . ? C44 C49 C54 O54 0.6(11) . . . . ? C50 C49 C54 C53 -4.0(12) . . . . ? C44 C49 C54 C53 -179.5(8) . . . . ? C53 C54 O54 C56 18.2(12) . . . . ? C49 C54 O54 C56 -161.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.118 _refine_diff_density_min -4.074 _refine_diff_density_rms 0.157 data_2e. _database_code_depnum_ccdc_archive 'CCDC 910518' #TrackingRef 'web_deposit_cif_file_0_ThibaultSchmid_1352721592.2e.cif' _chemical_formula_sum 'C51 H67 Cl2 N2 P Pd' _chemical_formula_moiety 'C51 H67 Cl2 N2 P Pd' _chemical_formula_weight 916.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.928(2) _cell_length_b 13.362(3) _cell_length_c 30.789(5) _cell_angle_alpha 90.0000 _cell_angle_beta 92.804(5) _cell_angle_gamma 90.0000 _cell_volume 4901.3(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13484 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.35 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928.00 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.946 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_reflns_number 29822 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_theta_max 25.35 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8941 _reflns_number_gt 6424 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0904 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 8941 _refine_ls_number_parameters 514 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.440 _refine_diff_density_min -0.510 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.9988 1.0072 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.755306(19) 0.192652(17) 0.127728(7) 0.03592(9) Uani 1.0 4 d . . . Cl1 Cl 0.77709(8) 0.30437(6) 0.18491(3) 0.0531(3) Uani 1.0 4 d . . . Cl2 Cl 0.73341(8) 0.07851(7) 0.07235(3) 0.0610(3) Uani 1.0 4 d . . . P30 P 0.70476(7) 0.32910(6) 0.08356(3) 0.0373(2) Uani 1.0 4 d . . . N2 N 0.9097(2) 0.06825(17) 0.18738(7) 0.0353(6) Uani 1.0 4 d . . . N5 N 0.73821(19) 0.03197(17) 0.19791(7) 0.0346(6) Uani 1.0 4 d . . . C1 C 0.8027(3) 0.0857(2) 0.17203(9) 0.0342(7) Uani 1.0 4 d . . . C3 C 0.9099(3) 0.0059(3) 0.22330(10) 0.0437(9) Uani 1.0 4 d . . . C4 C 0.8033(3) -0.0164(3) 0.23005(10) 0.0446(9) Uani 1.0 4 d . . . C6 C 1.0090(3) 0.1027(3) 0.16663(10) 0.0402(8) Uani 1.0 4 d . . . C7 C 1.0714(3) 0.1817(3) 0.18497(11) 0.0437(9) Uani 1.0 4 d . . . C8 C 1.1636(3) 0.2132(3) 0.16283(13) 0.0606(10) Uani 1.0 4 d . . . C9 C 1.1930(4) 0.1690(4) 0.12519(13) 0.0719(12) Uani 1.0 4 d . . . C10 C 1.1317(3) 0.0891(3) 0.10828(12) 0.0653(11) Uani 1.0 4 d . . . C11 C 1.0394(3) 0.0532(3) 0.12876(11) 0.0490(9) Uani 1.0 4 d . . . C12 C 1.0460(3) 0.2290(3) 0.22794(10) 0.0526(9) Uani 1.0 4 d . . . C13 C 1.1282(4) 0.1895(3) 0.26410(12) 0.0816(13) Uani 1.0 4 d . . . C14 C 1.0515(4) 0.3432(3) 0.22692(13) 0.0772(13) Uani 1.0 4 d . . . C15 C 0.9802(4) -0.0405(3) 0.11203(11) 0.0618(11) Uani 1.0 4 d . . . C16 C 1.0301(4) -0.1323(3) 0.13585(14) 0.0955(16) Uani 1.0 4 d . . . C17 C 0.9846(4) -0.0564(4) 0.06259(12) 0.0931(15) Uani 1.0 4 d . . . C18 C 0.6198(3) 0.0125(3) 0.18804(9) 0.0397(8) Uani 1.0 4 d . . . C19 C 0.5932(3) -0.0706(3) 0.16223(10) 0.0462(9) Uani 1.0 4 d . . . C20 C 0.4804(4) -0.0858(3) 0.15089(12) 0.0626(11) Uani 1.0 4 d . . . C21 C 0.3995(4) -0.0237(4) 0.16508(13) 0.0719(12) Uani 1.0 4 d . . . C22 C 0.4277(3) 0.0556(3) 0.19228(12) 0.0619(11) Uani 1.0 4 d . . . C23 C 0.5396(3) 0.0749(3) 0.20485(10) 0.0462(9) Uani 1.0 4 d . . . C24 C 0.6803(4) -0.1455(3) 0.14922(11) 0.0605(10) Uani 1.0 4 d . . . C25 C 0.6815(4) -0.2350(3) 0.18027(13) 0.0846(14) Uani 1.0 4 d . . . C26 C 0.6642(5) -0.1822(4) 0.10270(12) 0.0992(16) Uani 1.0 4 d . . . C27 C 0.5678(3) 0.1580(3) 0.23678(12) 0.0585(10) Uani 1.0 4 d . . . C28 C 0.5454(4) 0.1211(4) 0.28281(12) 0.1011(16) Uani 1.0 4 d . . . C29 C 0.5050(4) 0.2542(3) 0.22635(15) 0.0990(16) Uani 1.0 4 d . . . C31 C 0.6689(3) 0.3075(3) 0.02541(9) 0.0409(8) Uani 1.0 4 d . . . C32 C 0.6050(3) 0.3918(3) 0.00104(9) 0.0462(9) Uani 1.0 4 d . . . C33 C 0.5638(3) 0.3563(3) -0.04402(10) 0.0546(10) Uani 1.0 4 d . . . C34 C 0.6607(4) 0.3201(3) -0.06979(11) 0.0664(11) Uani 1.0 4 d . . . C35 C 0.7281(4) 0.2394(3) -0.04574(11) 0.0721(12) Uani 1.0 4 d . . . C36 C 0.7694(3) 0.2757(3) -0.00053(10) 0.0548(10) Uani 1.0 4 d . . . C37 C 0.8207(3) 0.4210(3) 0.08937(10) 0.0453(9) Uani 1.0 4 d . . . C38 C 0.8101(3) 0.5175(3) 0.06278(11) 0.0573(10) Uani 1.0 4 d . . . C39 C 0.9032(4) 0.5902(3) 0.07638(14) 0.0830(14) Uani 1.0 4 d . . . C40 C 1.0179(4) 0.5442(4) 0.07204(15) 0.0975(17) Uani 1.0 4 d . . . C41 C 1.0291(4) 0.4465(4) 0.09759(14) 0.0856(14) Uani 1.0 4 d . . . C42 C 0.9361(3) 0.3718(3) 0.08416(12) 0.0628(11) Uani 1.0 4 d . . . C43 C 0.5817(3) 0.3911(3) 0.10578(9) 0.0373(8) Uani 1.0 4 d . . . C44 C 0.4701(3) 0.3583(3) 0.09824(9) 0.0411(8) Uani 1.0 4 d . . . C45 C 0.3850(3) 0.4083(3) 0.11868(10) 0.0527(9) Uani 1.0 4 d . . . C46 C 0.4050(3) 0.4859(3) 0.14698(11) 0.0595(10) Uani 1.0 4 d . . . C47 C 0.5137(4) 0.5171(3) 0.15520(11) 0.0567(10) Uani 1.0 4 d . . . C48 C 0.6002(3) 0.4714(3) 0.13479(10) 0.0479(9) Uani 1.0 4 d . . . C49 C 0.4341(3) 0.2724(3) 0.07010(10) 0.0444(8) Uani 1.0 4 d . . . C50 C 0.4701(3) 0.1760(3) 0.07860(11) 0.0517(9) Uani 1.0 4 d . . . C51 C 0.4301(4) 0.0965(3) 0.05361(13) 0.0699(12) Uani 1.0 4 d . . . C52 C 0.3525(4) 0.1115(4) 0.01997(13) 0.0796(14) Uani 1.0 4 d . . . C53 C 0.3143(4) 0.2069(4) 0.01199(12) 0.0778(13) Uani 1.0 4 d . . . C54 C 0.3540(3) 0.2868(3) 0.03628(11) 0.0584(10) Uani 1.0 4 d . . . H3 H 0.9740 -0.0167 0.2400 0.0524 Uiso 1.0 4 calc R . . H4 H 0.7769 -0.0576 0.2525 0.0535 Uiso 1.0 4 calc R . . H8 H 1.2075 0.2673 0.1743 0.0727 Uiso 1.0 4 calc R . . H9 H 1.2558 0.1932 0.1105 0.0862 Uiso 1.0 4 calc R . . H10 H 1.1533 0.0585 0.0822 0.0784 Uiso 1.0 4 calc R . . H12 H 0.9683 0.2091 0.2352 0.0631 Uiso 1.0 4 calc R . . H13A H 1.2052 0.2065 0.2572 0.0980 Uiso 1.0 4 calc R . . H13B H 1.1209 0.1166 0.2662 0.0980 Uiso 1.0 4 calc R . . H13C H 1.1108 0.2201 0.2919 0.0980 Uiso 1.0 4 calc R . . H14A H 0.9970 0.3686 0.2047 0.0926 Uiso 1.0 4 calc R . . H14B H 1.1272 0.3644 0.2200 0.0926 Uiso 1.0 4 calc R . . H14C H 1.0336 0.3699 0.2554 0.0926 Uiso 1.0 4 calc R . . H15 H 0.8995 -0.0354 0.1192 0.0741 Uiso 1.0 4 calc R . . H16A H 1.0219 -0.1247 0.1672 0.1146 Uiso 1.0 4 calc R . . H16B H 1.1099 -0.1380 0.1300 0.1146 Uiso 1.0 4 calc R . . H16C H 0.9905 -0.1926 0.1255 0.1146 Uiso 1.0 4 calc R . . H17A H 1.0629 -0.0628 0.0548 0.1117 Uiso 1.0 4 calc R . . H17B H 0.9501 0.0011 0.0473 0.1117 Uiso 1.0 4 calc R . . H17C H 0.9435 -0.1175 0.0542 0.1117 Uiso 1.0 4 calc R . . H20 H 0.4593 -0.1410 0.1328 0.0751 Uiso 1.0 4 calc R . . H21 H 0.3231 -0.0348 0.1562 0.0863 Uiso 1.0 4 calc R . . H22 H 0.3703 0.0974 0.2026 0.0743 Uiso 1.0 4 calc R . . H24 H 0.7554 -0.1123 0.1523 0.0727 Uiso 1.0 4 calc R . . H25A H 0.6074 -0.2668 0.1791 0.1015 Uiso 1.0 4 calc R . . H25B H 0.7001 -0.2121 0.2100 0.1015 Uiso 1.0 4 calc R . . H25C H 0.7379 -0.2836 0.1717 0.1015 Uiso 1.0 4 calc R . . H26A H 0.6684 -0.1254 0.0827 0.1190 Uiso 1.0 4 calc R . . H26B H 0.5906 -0.2144 0.0987 0.1190 Uiso 1.0 4 calc R . . H26C H 0.7232 -0.2306 0.0967 0.1190 Uiso 1.0 4 calc R . . H27 H 0.6499 0.1723 0.2357 0.0702 Uiso 1.0 4 calc R . . H28A H 0.5919 0.0622 0.2897 0.1213 Uiso 1.0 4 calc R . . H28B H 0.4660 0.1032 0.2843 0.1213 Uiso 1.0 4 calc R . . H28C H 0.5639 0.1743 0.3039 0.1213 Uiso 1.0 4 calc R . . H29A H 0.4240 0.2422 0.2270 0.1188 Uiso 1.0 4 calc R . . H29B H 0.5232 0.2776 0.1974 0.1188 Uiso 1.0 4 calc R . . H29C H 0.5271 0.3053 0.2480 0.1188 Uiso 1.0 4 calc R . . H31 H 0.6168 0.2488 0.0244 0.0491 Uiso 1.0 4 calc R . . H32A H 0.5401 0.4128 0.0177 0.0554 Uiso 1.0 4 calc R . . H32B H 0.6550 0.4503 -0.0018 0.0554 Uiso 1.0 4 calc R . . H33A H 0.5091 0.3012 -0.0411 0.0655 Uiso 1.0 4 calc R . . H33B H 0.5251 0.4120 -0.0598 0.0655 Uiso 1.0 4 calc R . . H34A H 0.7105 0.3773 -0.0757 0.0797 Uiso 1.0 4 calc R . . H34B H 0.6312 0.2933 -0.0981 0.0797 Uiso 1.0 4 calc R . . H35A H 0.7933 0.2208 -0.0627 0.0865 Uiso 1.0 4 calc R . . H35B H 0.6808 0.1791 -0.0428 0.0865 Uiso 1.0 4 calc R . . H36A H 0.8210 0.3331 -0.0034 0.0658 Uiso 1.0 4 calc R . . H36B H 0.8110 0.2213 0.0150 0.0658 Uiso 1.0 4 calc R . . H37 H 0.8214 0.4430 0.1204 0.0544 Uiso 1.0 4 calc R . . H38A H 0.8143 0.5017 0.0315 0.0687 Uiso 1.0 4 calc R . . H38B H 0.7364 0.5489 0.0672 0.0687 Uiso 1.0 4 calc R . . H39A H 0.8965 0.6510 0.0581 0.0996 Uiso 1.0 4 calc R . . H39B H 0.8947 0.6105 0.1070 0.0996 Uiso 1.0 4 calc R . . H40A H 1.0762 0.5919 0.0830 0.1170 Uiso 1.0 4 calc R . . H40B H 1.0299 0.5311 0.0410 0.1170 Uiso 1.0 4 calc R . . H41A H 1.0259 0.4610 0.1290 0.1027 Uiso 1.0 4 calc R . . H41B H 1.1031 0.4160 0.0926 0.1027 Uiso 1.0 4 calc R . . H42A H 0.9435 0.3514 0.0535 0.0754 Uiso 1.0 4 calc R . . H42B H 0.9429 0.3112 0.1026 0.0754 Uiso 1.0 4 calc R . . H45 H 0.3096 0.3876 0.1127 0.0632 Uiso 1.0 4 calc R . . H46 H 0.3449 0.5177 0.1607 0.0714 Uiso 1.0 4 calc R . . H47 H 0.5292 0.5704 0.1750 0.0680 Uiso 1.0 4 calc R . . H48 H 0.6747 0.4947 0.1405 0.0574 Uiso 1.0 4 calc R . . H50 H 0.5232 0.1640 0.1020 0.0620 Uiso 1.0 4 calc R . . H51 H 0.4566 0.0307 0.0599 0.0839 Uiso 1.0 4 calc R . . H52 H 0.3257 0.0571 0.0025 0.0956 Uiso 1.0 4 calc R . . H53 H 0.2592 0.2180 -0.0108 0.0933 Uiso 1.0 4 calc R . . H54 H 0.3266 0.3522 0.0300 0.0700 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.03509(15) 0.03815(17) 0.03481(15) 0.00011(11) 0.00474(11) 0.00385(11) Cl1 0.0715(6) 0.0467(6) 0.0405(5) 0.0026(5) -0.0017(5) -0.0028(4) Cl2 0.0798(7) 0.0523(6) 0.0500(5) 0.0091(5) -0.0053(5) -0.0090(5) P30 0.0331(5) 0.0421(5) 0.0370(5) -0.0014(4) 0.0045(4) 0.0070(4) N2 0.0345(15) 0.0354(15) 0.0368(14) 0.0005(12) 0.0084(12) 0.0042(12) N5 0.0359(15) 0.0375(15) 0.0308(14) -0.0024(12) 0.0062(12) 0.0005(12) C1 0.0361(18) 0.0316(18) 0.0351(17) 0.0011(15) 0.0032(14) -0.0026(14) C3 0.043(2) 0.047(2) 0.0410(19) -0.0005(17) -0.0016(16) 0.0138(17) C4 0.051(3) 0.047(3) 0.0356(18) -0.0046(17) 0.0042(16) 0.0112(16) C6 0.0317(18) 0.043(2) 0.0467(19) 0.0040(16) 0.0073(16) 0.0071(16) C7 0.0339(19) 0.045(2) 0.052(2) 0.0059(16) 0.0073(16) 0.0100(17) C8 0.041(3) 0.065(3) 0.076(3) -0.0094(19) 0.012(2) 0.000(3) C9 0.051(3) 0.087(4) 0.081(3) -0.004(3) 0.033(3) 0.015(3) C10 0.057(3) 0.080(3) 0.061(3) 0.006(3) 0.029(2) -0.001(3) C11 0.041(2) 0.053(3) 0.054(2) 0.0059(18) 0.0115(17) 0.0083(19) C12 0.047(3) 0.055(3) 0.057(3) -0.0081(18) 0.0055(18) -0.0011(19) C13 0.079(3) 0.097(4) 0.068(3) -0.012(3) -0.003(3) 0.008(3) C14 0.081(3) 0.064(3) 0.087(3) -0.012(3) 0.008(3) -0.015(3) C15 0.058(3) 0.065(3) 0.063(3) 0.005(2) 0.019(2) -0.014(2) C16 0.125(5) 0.060(3) 0.104(4) 0.002(3) 0.025(4) -0.012(3) C17 0.088(4) 0.119(4) 0.074(3) 0.007(3) 0.018(3) -0.031(3) C18 0.038(2) 0.044(2) 0.0373(18) -0.0065(16) 0.0046(15) 0.0056(16) C19 0.048(3) 0.047(3) 0.0438(19) -0.0123(18) 0.0065(17) -0.0002(17) C20 0.061(3) 0.064(3) 0.062(3) -0.017(3) -0.003(2) -0.002(2) C21 0.047(3) 0.081(4) 0.086(3) -0.018(3) -0.010(3) 0.008(3) C22 0.044(3) 0.060(3) 0.082(3) 0.0030(19) 0.006(2) 0.014(3) C23 0.042(2) 0.044(2) 0.053(2) -0.0036(17) 0.0095(17) 0.0073(18) C24 0.067(3) 0.056(3) 0.060(3) -0.017(2) 0.014(2) -0.016(2) C25 0.100(4) 0.060(3) 0.095(4) 0.009(3) 0.015(3) -0.000(3) C26 0.142(5) 0.088(4) 0.069(3) 0.002(4) 0.018(3) -0.026(3) C27 0.052(3) 0.049(3) 0.076(3) -0.0037(19) 0.022(2) -0.008(2) C28 0.124(5) 0.110(4) 0.072(3) -0.029(4) 0.030(3) -0.030(3) C29 0.077(4) 0.057(3) 0.165(5) 0.005(3) 0.032(4) -0.022(3) C31 0.046(2) 0.044(2) 0.0336(17) 0.0012(16) 0.0047(15) 0.0047(15) C32 0.048(2) 0.051(3) 0.0408(19) 0.0011(17) 0.0045(16) 0.0052(16) C33 0.056(3) 0.069(3) 0.0387(19) -0.001(2) -0.0015(18) 0.0056(18) C34 0.078(3) 0.084(3) 0.038(2) -0.004(3) 0.008(2) -0.001(2) C35 0.088(3) 0.076(3) 0.054(3) 0.010(3) 0.029(3) -0.006(3) C36 0.057(3) 0.063(3) 0.046(2) 0.0131(19) 0.0152(18) 0.0088(18) C37 0.0375(19) 0.051(2) 0.0473(19) -0.0055(16) 0.0043(16) 0.0084(17) C38 0.055(3) 0.056(3) 0.060(3) -0.0185(19) -0.0014(19) 0.0133(19) C39 0.086(4) 0.069(3) 0.093(4) -0.036(3) -0.002(3) 0.018(3) C40 0.070(4) 0.118(5) 0.104(4) -0.053(3) 0.003(3) 0.024(4) C41 0.044(3) 0.118(4) 0.094(4) -0.019(3) -0.003(3) 0.016(3) C42 0.038(3) 0.076(3) 0.075(3) -0.006(2) 0.0063(19) 0.009(3) C43 0.0377(19) 0.041(2) 0.0336(17) 0.0011(15) 0.0022(14) 0.0062(16) C44 0.041(2) 0.044(2) 0.0388(18) 0.0013(16) 0.0050(16) 0.0075(16) C45 0.043(3) 0.062(3) 0.055(3) 0.0023(19) 0.0140(18) -0.001(2) C46 0.058(3) 0.064(3) 0.058(3) 0.014(2) 0.018(2) -0.008(2) C47 0.068(3) 0.048(3) 0.054(3) 0.002(2) 0.008(2) -0.0069(19) C48 0.045(3) 0.048(3) 0.050(2) -0.0018(17) 0.0000(18) 0.0012(18) C49 0.0366(19) 0.056(3) 0.0414(19) -0.0099(17) 0.0126(15) -0.0029(18) C50 0.043(2) 0.059(3) 0.054(3) -0.0103(19) 0.0150(17) -0.008(2) C51 0.073(3) 0.059(3) 0.080(3) -0.013(3) 0.024(3) -0.010(3) C52 0.084(4) 0.097(4) 0.060(3) -0.043(3) 0.019(3) -0.027(3) C53 0.072(3) 0.112(4) 0.048(3) -0.023(3) -0.003(3) -0.003(3) C54 0.050(3) 0.074(3) 0.050(3) -0.012(2) -0.0008(18) 0.003(2) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13' _computing_structure_solution 'DIRDIF99-PATTY (Gould, et al., 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd1 Cl1 2.3132(10) yes . . Pd1 Cl2 2.2930(10) yes . . Pd1 P30 2.3359(10) yes . . Pd1 C1 2.036(3) yes . . P30 C31 1.843(3) yes . . P30 C37 1.851(4) yes . . P30 C43 1.846(3) yes . . N2 C1 1.360(4) yes . . N2 C3 1.384(4) yes . . N2 C6 1.449(4) yes . . N5 C1 1.342(4) yes . . N5 C4 1.387(4) yes . . N5 C18 1.454(4) yes . . C3 C4 1.333(5) yes . . C6 C7 1.395(5) yes . . C6 C11 1.403(5) yes . . C7 C8 1.387(5) yes . . C7 C12 1.510(5) yes . . C8 C9 1.362(6) yes . . C9 C10 1.381(6) yes . . C10 C11 1.382(6) yes . . C11 C15 1.515(5) yes . . C12 C13 1.541(5) yes . . C12 C14 1.527(5) yes . . C15 C16 1.533(6) yes . . C15 C17 1.540(5) yes . . C18 C19 1.392(5) yes . . C18 C23 1.388(5) yes . . C19 C20 1.388(5) yes . . C19 C24 1.511(5) yes . . C20 C21 1.362(6) yes . . C21 C22 1.381(6) yes . . C22 C23 1.396(5) yes . . C23 C27 1.510(5) yes . . C24 C25 1.531(6) yes . . C24 C26 1.517(5) yes . . C27 C28 1.536(6) yes . . C27 C29 1.515(6) yes . . C31 C32 1.535(5) yes . . C31 C36 1.533(5) yes . . C32 C33 1.525(5) yes . . C33 C34 1.513(6) yes . . C34 C35 1.516(6) yes . . C35 C36 1.533(5) yes . . C37 C38 1.530(5) yes . . C37 C42 1.540(5) yes . . C38 C39 1.518(6) yes . . C39 C40 1.511(7) yes . . C40 C41 1.527(7) yes . . C41 C42 1.534(6) yes . . C43 C44 1.410(5) yes . . C43 C48 1.406(5) yes . . C44 C45 1.391(5) yes . . C44 C49 1.489(5) yes . . C45 C46 1.368(5) yes . . C46 C47 1.373(6) yes . . C47 C48 1.378(5) yes . . C49 C50 1.379(5) yes . . C49 C54 1.392(5) yes . . C50 C51 1.383(6) yes . . C51 C52 1.369(6) yes . . C52 C53 1.372(7) yes . . C53 C54 1.374(6) yes . . C3 H3 0.950 no . . C4 H4 0.950 no . . C8 H8 0.950 no . . C9 H9 0.950 no . . C10 H10 0.950 no . . C12 H12 1.000 no . . C13 H13A 0.980 no . . C13 H13B 0.980 no . . C13 H13C 0.980 no . . C14 H14A 0.980 no . . C14 H14B 0.980 no . . C14 H14C 0.980 no . . C15 H15 1.000 no . . C16 H16A 0.980 no . . C16 H16B 0.980 no . . C16 H16C 0.980 no . . C17 H17A 0.980 no . . C17 H17B 0.980 no . . C17 H17C 0.980 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C24 H24 1.000 no . . C25 H25A 0.980 no . . C25 H25B 0.980 no . . C25 H25C 0.980 no . . C26 H26A 0.980 no . . C26 H26B 0.980 no . . C26 H26C 0.980 no . . C27 H27 1.000 no . . C28 H28A 0.980 no . . C28 H28B 0.980 no . . C28 H28C 0.980 no . . C29 H29A 0.980 no . . C29 H29B 0.980 no . . C29 H29C 0.980 no . . C31 H31 1.000 no . . C32 H32A 0.990 no . . C32 H32B 0.990 no . . C33 H33A 0.990 no . . C33 H33B 0.990 no . . C34 H34A 0.990 no . . C34 H34B 0.990 no . . C35 H35A 0.990 no . . C35 H35B 0.990 no . . C36 H36A 0.990 no . . C36 H36B 0.990 no . . C37 H37 1.000 no . . C38 H38A 0.990 no . . C38 H38B 0.990 no . . C39 H39A 0.990 no . . C39 H39B 0.990 no . . C40 H40A 0.990 no . . C40 H40B 0.990 no . . C41 H41A 0.990 no . . C41 H41B 0.990 no . . C42 H42A 0.990 no . . C42 H42B 0.990 no . . C45 H45 0.950 no . . C46 H46 0.950 no . . C47 H47 0.950 no . . C48 H48 0.950 no . . C50 H50 0.950 no . . C51 H51 0.950 no . . C52 H52 0.950 no . . C53 H53 0.950 no . . C54 H54 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl1 Pd1 Cl2 178.48(4) yes . . . Cl1 Pd1 P30 87.46(4) yes . . . Cl1 Pd1 C1 85.75(9) yes . . . Cl2 Pd1 P30 93.98(4) yes . . . Cl2 Pd1 C1 92.82(9) yes . . . P30 Pd1 C1 173.19(9) yes . . . Pd1 P30 C31 118.96(10) yes . . . Pd1 P30 C37 106.91(11) yes . . . Pd1 P30 C43 108.78(10) yes . . . C31 P30 C37 109.55(15) yes . . . C31 P30 C43 106.22(14) yes . . . C37 P30 C43 105.68(14) yes . . . C1 N2 C3 110.2(3) yes . . . C1 N2 C6 124.5(3) yes . . . C3 N2 C6 125.0(3) yes . . . C1 N5 C4 110.9(3) yes . . . C1 N5 C18 123.4(3) yes . . . C4 N5 C18 124.7(3) yes . . . Pd1 C1 N2 125.3(2) yes . . . Pd1 C1 N5 128.7(2) yes . . . N2 C1 N5 104.9(3) yes . . . N2 C3 C4 107.2(3) yes . . . N5 C4 C3 106.8(3) yes . . . N2 C6 C7 119.6(3) yes . . . N2 C6 C11 117.8(3) yes . . . C7 C6 C11 122.6(3) yes . . . C6 C7 C8 116.8(4) yes . . . C6 C7 C12 123.1(3) yes . . . C8 C7 C12 120.1(3) yes . . . C7 C8 C9 122.0(4) yes . . . C8 C9 C10 120.2(4) yes . . . C9 C10 C11 121.1(4) yes . . . C6 C11 C10 117.3(3) yes . . . C6 C11 C15 122.5(3) yes . . . C10 C11 C15 120.1(4) yes . . . C7 C12 C13 110.0(3) yes . . . C7 C12 C14 112.9(3) yes . . . C13 C12 C14 109.3(3) yes . . . C11 C15 C16 109.5(3) yes . . . C11 C15 C17 114.3(4) yes . . . C16 C15 C17 109.4(4) yes . . . N5 C18 C19 117.0(3) yes . . . N5 C18 C23 119.6(3) yes . . . C19 C18 C23 123.3(3) yes . . . C18 C19 C20 116.9(3) yes . . . C18 C19 C24 122.6(3) yes . . . C20 C19 C24 120.4(3) yes . . . C19 C20 C21 121.5(4) yes . . . C20 C21 C22 120.4(4) yes . . . C21 C22 C23 120.8(4) yes . . . C18 C23 C22 116.9(3) yes . . . C18 C23 C27 123.3(3) yes . . . C22 C23 C27 119.7(3) yes . . . C19 C24 C25 109.7(3) yes . . . C19 C24 C26 114.0(3) yes . . . C25 C24 C26 109.5(3) yes . . . C23 C27 C28 108.8(3) yes . . . C23 C27 C29 113.2(3) yes . . . C28 C27 C29 111.2(4) yes . . . P30 C31 C32 116.5(2) yes . . . P30 C31 C36 113.5(2) yes . . . C32 C31 C36 109.3(3) yes . . . C31 C32 C33 110.3(3) yes . . . C32 C33 C34 110.9(3) yes . . . C33 C34 C35 111.8(3) yes . . . C34 C35 C36 111.0(3) yes . . . C31 C36 C35 109.6(3) yes . . . P30 C37 C38 117.8(3) yes . . . P30 C37 C42 112.0(3) yes . . . C38 C37 C42 110.8(3) yes . . . C37 C38 C39 110.6(3) yes . . . C38 C39 C40 111.6(4) yes . . . C39 C40 C41 111.0(4) yes . . . C40 C41 C42 111.9(4) yes . . . C37 C42 C41 109.4(3) yes . . . P30 C43 C44 124.1(3) yes . . . P30 C43 C48 118.3(3) yes . . . C44 C43 C48 117.3(3) yes . . . C43 C44 C45 118.7(3) yes . . . C43 C44 C49 125.3(3) yes . . . C45 C44 C49 116.0(3) yes . . . C44 C45 C46 122.9(4) yes . . . C45 C46 C47 118.8(4) yes . . . C46 C47 C48 120.2(4) yes . . . C43 C48 C47 122.0(3) yes . . . C44 C49 C50 122.1(3) yes . . . C44 C49 C54 119.8(3) yes . . . C50 C49 C54 117.8(4) yes . . . C49 C50 C51 121.1(4) yes . . . C50 C51 C52 120.6(4) yes . . . C51 C52 C53 118.6(4) yes . . . C52 C53 C54 121.4(4) yes . . . C49 C54 C53 120.4(4) yes . . . N2 C3 H3 126.410 no . . . C4 C3 H3 126.418 no . . . N5 C4 H4 126.603 no . . . C3 C4 H4 126.602 no . . . C7 C8 H8 119.005 no . . . C9 C8 H8 118.996 no . . . C8 C9 H9 119.922 no . . . C10 C9 H9 119.923 no . . . C9 C10 H10 119.469 no . . . C11 C10 H10 119.476 no . . . C7 C12 H12 108.162 no . . . C13 C12 H12 108.161 no . . . C14 C12 H12 108.158 no . . . C12 C13 H13A 109.462 no . . . C12 C13 H13B 109.465 no . . . C12 C13 H13C 109.466 no . . . H13A C13 H13B 109.470 no . . . H13A C13 H13C 109.487 no . . . H13B C13 H13C 109.477 no . . . C12 C14 H14A 109.459 no . . . C12 C14 H14B 109.472 no . . . C12 C14 H14C 109.472 no . . . H14A C14 H14B 109.465 no . . . H14A C14 H14C 109.478 no . . . H14B C14 H14C 109.482 no . . . C11 C15 H15 107.806 no . . . C16 C15 H15 107.805 no . . . C17 C15 H15 107.800 no . . . C15 C16 H16A 109.465 no . . . C15 C16 H16B 109.467 no . . . C15 C16 H16C 109.475 no . . . H16A C16 H16B 109.473 no . . . H16A C16 H16C 109.479 no . . . H16B C16 H16C 109.469 no . . . C15 C17 H17A 109.471 no . . . C15 C17 H17B 109.465 no . . . C15 C17 H17C 109.465 no . . . H17A C17 H17B 109.473 no . . . H17A C17 H17C 109.478 no . . . H17B C17 H17C 109.476 no . . . C19 C20 H20 119.231 no . . . C21 C20 H20 119.231 no . . . C20 C21 H21 119.806 no . . . C22 C21 H21 119.790 no . . . C21 C22 H22 119.620 no . . . C23 C22 H22 119.604 no . . . C19 C24 H24 107.794 no . . . C25 C24 H24 107.790 no . . . C26 C24 H24 107.785 no . . . C24 C25 H25A 109.483 no . . . C24 C25 H25B 109.469 no . . . C24 C25 H25C 109.477 no . . . H25A C25 H25B 109.457 no . . . H25A C25 H25C 109.477 no . . . H25B C25 H25C 109.465 no . . . C24 C26 H26A 109.480 no . . . C24 C26 H26B 109.466 no . . . C24 C26 H26C 109.465 no . . . H26A C26 H26B 109.473 no . . . H26A C26 H26C 109.474 no . . . H26B C26 H26C 109.468 no . . . C23 C27 H27 107.824 no . . . C28 C27 H27 107.835 no . . . C29 C27 H27 107.833 no . . . C27 C28 H28A 109.491 no . . . C27 C28 H28B 109.487 no . . . C27 C28 H28C 109.475 no . . . H28A C28 H28B 109.461 no . . . H28A C28 H28C 109.455 no . . . H28B C28 H28C 109.459 no . . . C27 C29 H29A 109.474 no . . . C27 C29 H29B 109.476 no . . . C27 C29 H29C 109.468 no . . . H29A C29 H29B 109.466 no . . . H29A C29 H29C 109.478 no . . . H29B C29 H29C 109.466 no . . . P30 C31 H31 105.516 no . . . C32 C31 H31 105.512 no . . . C36 C31 H31 105.504 no . . . C31 C32 H32A 109.608 no . . . C31 C32 H32B 109.609 no . . . C33 C32 H32A 109.592 no . . . C33 C32 H32B 109.591 no . . . H32A C32 H32B 108.141 no . . . C32 C33 H33A 109.481 no . . . C32 C33 H33B 109.472 no . . . C34 C33 H33A 109.467 no . . . C34 C33 H33B 109.466 no . . . H33A C33 H33B 108.051 no . . . C33 C34 H34A 109.248 no . . . C33 C34 H34B 109.245 no . . . C35 C34 H34A 109.253 no . . . C35 C34 H34B 109.255 no . . . H34A C34 H34B 107.927 no . . . C34 C35 H35A 109.445 no . . . C34 C35 H35B 109.437 no . . . C36 C35 H35A 109.445 no . . . C36 C35 H35B 109.449 no . . . H35A C35 H35B 108.044 no . . . C31 C36 H36A 109.740 no . . . C31 C36 H36B 109.747 no . . . C35 C36 H36A 109.749 no . . . C35 C36 H36B 109.748 no . . . H36A C36 H36B 108.215 no . . . P30 C37 H37 105.035 no . . . C38 C37 H37 105.036 no . . . C42 C37 H37 105.036 no . . . C37 C38 H38A 109.520 no . . . C37 C38 H38B 109.535 no . . . C39 C38 H38A 109.526 no . . . C39 C38 H38B 109.531 no . . . H38A C38 H38B 108.086 no . . . C38 C39 H39A 109.303 no . . . C38 C39 H39B 109.291 no . . . C40 C39 H39A 109.297 no . . . C40 C39 H39B 109.293 no . . . H39A C39 H39B 107.947 no . . . C39 C40 H40A 109.435 no . . . C39 C40 H40B 109.429 no . . . C41 C40 H40A 109.434 no . . . C41 C40 H40B 109.430 no . . . H40A C40 H40B 108.034 no . . . C40 C41 H41A 109.225 no . . . C40 C41 H41B 109.214 no . . . C42 C41 H41A 109.236 no . . . C42 C41 H41B 109.229 no . . . H41A C41 H41B 107.934 no . . . C37 C42 H42A 109.781 no . . . C37 C42 H42B 109.789 no . . . C41 C42 H42A 109.790 no . . . C41 C42 H42B 109.778 no . . . H42A C42 H42B 108.245 no . . . C44 C45 H45 118.516 no . . . C46 C45 H45 118.540 no . . . C45 C46 H46 120.611 no . . . C47 C46 H46 120.627 no . . . C46 C47 H47 119.915 no . . . C48 C47 H47 119.900 no . . . C43 C48 H48 118.972 no . . . C47 C48 H48 119.001 no . . . C49 C50 H50 119.452 no . . . C51 C50 H50 119.458 no . . . C50 C51 H51 119.667 no . . . C52 C51 H51 119.683 no . . . C51 C52 H52 120.716 no . . . C53 C52 H52 120.720 no . . . C52 C53 H53 119.280 no . . . C54 C53 H53 119.275 no . . . C49 C54 H54 119.808 no . . . C53 C54 H54 119.812 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl1 Pd1 P30 C31 179.92(5) no . . . . Cl1 Pd1 P30 C37 55.30(5) no . . . . Cl1 Pd1 P30 C43 -58.39(5) no . . . . Cl1 Pd1 C1 N2 -77.2(2) no . . . . Cl1 Pd1 C1 N5 89.0(3) no . . . . Cl2 Pd1 P30 C31 -0.57(5) no . . . . Cl2 Pd1 P30 C37 -125.19(5) no . . . . Cl2 Pd1 P30 C43 121.12(5) no . . . . Cl2 Pd1 C1 N2 103.3(2) no . . . . Cl2 Pd1 C1 N5 -90.5(3) no . . . . Pd1 P30 C31 C32 163.06(13) no . . . . Pd1 P30 C31 C36 -68.6(2) no . . . . Pd1 P30 C37 C38 178.65(16) no . . . . Pd1 P30 C37 C42 48.53(19) no . . . . Pd1 P30 C43 C44 -81.7(2) no . . . . Pd1 P30 C43 C48 93.05(19) no . . . . C31 P30 C37 C38 48.5(3) no . . . . C31 P30 C37 C42 -81.6(2) no . . . . C37 P30 C31 C32 -73.6(3) no . . . . C37 P30 C31 C36 54.7(2) no . . . . C31 P30 C43 C44 47.4(3) no . . . . C31 P30 C43 C48 -137.79(19) no . . . . C43 P30 C31 C32 40.1(3) no . . . . C43 P30 C31 C36 168.40(17) no . . . . C37 P30 C43 C44 163.8(2) no . . . . C37 P30 C43 C48 -21.4(3) no . . . . C43 P30 C37 C38 -65.6(3) no . . . . C43 P30 C37 C42 164.31(17) no . . . . C1 N2 C3 C4 0.7(3) no . . . . C3 N2 C1 Pd1 167.3(2) no . . . . C3 N2 C1 N5 -1.6(3) no . . . . C1 N2 C6 C7 106.6(3) no . . . . C1 N2 C6 C11 -74.4(4) no . . . . C6 N2 C1 Pd1 -17.8(4) no . . . . C6 N2 C1 N5 173.3(3) no . . . . C3 N2 C6 C7 -79.4(4) no . . . . C3 N2 C6 C11 99.7(3) no . . . . C6 N2 C3 C4 -174.1(3) no . . . . C1 N5 C4 C3 -1.4(3) no . . . . C4 N5 C1 Pd1 -166.6(3) no . . . . C4 N5 C1 N2 1.8(3) no . . . . C1 N5 C18 C19 86.8(4) no . . . . C1 N5 C18 C23 -94.2(3) no . . . . C18 N5 C1 Pd1 24.4(4) no . . . . C18 N5 C1 N2 -167.2(3) no . . . . C4 N5 C18 C19 -80.7(4) no . . . . C4 N5 C18 C23 98.4(4) no . . . . C18 N5 C4 C3 167.4(3) no . . . . N2 C3 C4 N5 0.4(4) no . . . . N2 C6 C7 C8 -178.0(3) no . . . . N2 C6 C7 C12 5.0(5) no . . . . N2 C6 C11 C10 177.5(3) no . . . . N2 C6 C11 C15 -6.8(5) no . . . . C7 C6 C11 C10 -3.5(5) no . . . . C7 C6 C11 C15 172.2(3) no . . . . C11 C6 C7 C8 2.9(5) no . . . . C11 C6 C7 C12 -174.0(3) no . . . . C6 C7 C8 C9 -0.6(5) no . . . . C6 C7 C12 C13 101.3(4) no . . . . C6 C7 C12 C14 -136.2(3) no . . . . C8 C7 C12 C13 -75.5(4) no . . . . C8 C7 C12 C14 46.9(4) no . . . . C12 C7 C8 C9 176.5(3) no . . . . C7 C8 C9 C10 -1.2(6) no . . . . C8 C9 C10 C11 0.6(6) no . . . . C9 C10 C11 C6 1.6(5) no . . . . C9 C10 C11 C15 -174.1(3) no . . . . C6 C11 C15 C16 -83.5(4) no . . . . C6 C11 C15 C17 153.4(3) no . . . . C10 C11 C15 C16 92.1(4) no . . . . C10 C11 C15 C17 -31.0(5) no . . . . N5 C18 C19 C20 -176.6(3) no . . . . N5 C18 C19 C24 7.4(4) no . . . . N5 C18 C23 C22 176.6(3) no . . . . N5 C18 C23 C27 -5.9(5) no . . . . C19 C18 C23 C22 -4.4(5) no . . . . C19 C18 C23 C27 173.0(3) no . . . . C23 C18 C19 C20 4.4(5) no . . . . C23 C18 C19 C24 -171.5(3) no . . . . C18 C19 C20 C21 -1.3(5) no . . . . C18 C19 C24 C25 96.5(4) no . . . . C18 C19 C24 C26 -140.3(3) no . . . . C20 C19 C24 C25 -79.4(4) no . . . . C20 C19 C24 C26 43.9(5) no . . . . C24 C19 C20 C21 174.8(3) no . . . . C19 C20 C21 C22 -1.6(6) no . . . . C20 C21 C22 C23 1.6(6) no . . . . C21 C22 C23 C18 1.3(5) no . . . . C21 C22 C23 C27 -176.2(3) no . . . . C18 C23 C27 C28 -99.4(4) no . . . . C18 C23 C27 C29 136.5(3) no . . . . C22 C23 C27 C28 78.0(4) no . . . . C22 C23 C27 C29 -46.1(5) no . . . . P30 C31 C32 C33 -170.17(17) no . . . . P30 C31 C36 C35 168.71(18) no . . . . C32 C31 C36 C35 -59.4(3) no . . . . C36 C31 C32 C33 59.5(3) no . . . . C31 C32 C33 C34 -57.2(4) no . . . . C32 C33 C34 C35 55.2(4) no . . . . C33 C34 C35 C36 -55.5(4) no . . . . C34 C35 C36 C31 57.5(4) no . . . . P30 C37 C38 C39 171.65(18) no . . . . P30 C37 C42 C41 -169.54(18) no . . . . C38 C37 C42 C41 56.8(4) no . . . . C42 C37 C38 C39 -57.7(4) no . . . . C37 C38 C39 C40 56.8(4) no . . . . C38 C39 C40 C41 -55.4(5) no . . . . C39 C40 C41 C42 55.4(5) no . . . . C40 C41 C42 C37 -55.8(4) no . . . . P30 C43 C44 C45 176.64(18) no . . . . P30 C43 C44 C49 -2.7(4) no . . . . P30 C43 C48 C47 -175.34(19) no . . . . C44 C43 C48 C47 -0.2(5) no . . . . C48 C43 C44 C45 1.8(4) no . . . . C48 C43 C44 C49 -177.5(3) no . . . . C43 C44 C45 C46 -2.3(5) no . . . . C43 C44 C49 C50 61.4(5) no . . . . C43 C44 C49 C54 -124.5(3) no . . . . C45 C44 C49 C50 -118.0(3) no . . . . C45 C44 C49 C54 56.2(4) no . . . . C49 C44 C45 C46 177.1(3) no . . . . C44 C45 C46 C47 1.0(5) no . . . . C45 C46 C47 C48 0.7(5) no . . . . C46 C47 C48 C43 -1.1(5) no . . . . C44 C49 C50 C51 175.9(3) no . . . . C44 C49 C54 C53 -175.5(3) no . . . . C50 C49 C54 C53 -1.1(5) no . . . . C54 C49 C50 C51 1.7(5) no . . . . C49 C50 C51 C52 -0.7(6) no . . . . C50 C51 C52 C53 -0.9(6) no . . . . C51 C52 C53 C54 1.4(6) no . . . . C52 C53 C54 C49 -0.5(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Pd1 C6 3.418(3) no . . Pd1 C18 3.486(3) no . . Pd1 C42 3.530(4) no . . Cl1 N2 3.528(3) no . . Cl1 C12 3.556(4) no . . Cl1 C14 3.498(5) no . . Cl1 C37 3.391(4) no . . Cl1 C43 3.487(3) no . . Cl1 C48 3.390(4) no . . Cl2 C15 3.512(4) no . . Cl2 C17 3.522(5) no . . Cl2 C31 3.454(3) no . . Cl2 C36 3.501(4) no . . Cl2 C50 3.414(4) no . . P30 C49 3.322(4) no . . P30 C50 3.464(4) no . . N2 C12 2.936(4) no . . N2 C15 2.897(5) no . . N2 C16 3.461(5) no . . N2 C18 3.538(4) no . . N5 C6 3.544(4) no . . N5 C24 2.872(5) no . . N5 C27 2.939(5) no . . C1 C7 3.458(5) no . . C1 C11 3.210(5) no . . C1 C15 3.335(5) no . . C1 C19 3.259(5) no . . C1 C23 3.346(5) no . . C1 C24 3.474(5) no . . C3 C7 3.293(5) no . . C3 C11 3.420(5) no . . C3 C12 3.394(5) no . . C3 C18 3.576(5) no . . C4 C6 3.583(5) no . . C4 C19 3.263(5) no . . C4 C23 3.427(5) no . . C4 C24 3.311(5) no . . C4 C25 3.574(5) no . . C6 C9 2.739(5) no . . C6 C13 3.457(5) no . . C6 C16 3.292(5) no . . C7 C10 2.791(5) no . . C8 C11 2.778(5) no . . C8 C13 3.183(6) no . . C8 C14 2.993(6) no . . C10 C16 3.322(6) no . . C10 C17 2.932(6) no . . C18 C21 2.731(5) no . . C18 C25 3.399(5) no . . C18 C28 3.415(5) no . . C19 C22 2.788(5) no . . C20 C23 2.785(5) no . . C20 C25 3.214(6) no . . C20 C26 2.997(6) no . . C22 C28 3.182(6) no . . C22 C29 2.984(6) no . . C31 C34 2.933(5) no . . C31 C38 3.442(5) no . . C31 C44 3.411(5) no . . C31 C49 3.214(5) no . . C31 C50 3.431(5) no . . C32 C35 2.930(5) no . . C32 C38 3.459(5) no . . C32 C43 3.250(4) no . . C32 C44 3.495(5) no . . C32 C49 3.413(5) no . . C32 C54 3.525(5) no . . C33 C36 2.941(5) no . . C36 C37 3.411(5) no . . C36 C42 3.448(5) no . . C37 C40 2.941(6) no . . C37 C48 3.112(5) no . . C38 C41 2.932(6) no . . C38 C43 3.519(5) no . . C38 C48 3.480(5) no . . C39 C42 2.952(6) no . . C43 C46 2.814(5) no . . C43 C50 3.260(5) no . . C44 C47 2.785(5) no . . C45 C48 2.724(5) no . . C45 C50 3.509(5) no . . C45 C54 3.020(5) no . . C49 C52 2.793(6) no . . C50 C53 2.731(5) no . . C51 C54 2.743(6) no . . C26 C53 3.568(6) no . 3_655 C34 C46 3.578(5) no . 3_665 C46 C34 3.578(5) no . 3_665 C53 C26 3.568(6) no . 3_655 Pd1 H15 3.5151 no . . Pd1 H31 3.5916 no . . Pd1 H36B 3.5858 no . . Pd1 H37 3.4471 no . . Pd1 H42B 2.8787 no . . Pd1 H50 2.8672 no . . Cl1 H12 2.9788 no . . Cl1 H14A 2.7993 no . . Cl1 H27 2.8455 no . . Cl1 H29B 3.0919 no . . Cl1 H37 2.7853 no . . Cl1 H42B 3.2915 no . . Cl1 H48 3.1096 no . . Cl2 H15 2.8351 no . . Cl2 H17B 2.9224 no . . Cl2 H24 3.5458 no . . Cl2 H26A 2.8550 no . . Cl2 H31 3.0150 no . . Cl2 H36B 2.7883 no . . Cl2 H50 2.9405 no . . Cl2 H51 3.3662 no . . P30 H32A 2.9704 no . . P30 H32B 3.1187 no . . P30 H36A 3.0755 no . . P30 H36B 2.8978 no . . P30 H38A 3.1307 no . . P30 H38B 3.0065 no . . P30 H42A 3.0511 no . . P30 H42B 2.8828 no . . P30 H48 2.8565 no . . P30 H50 3.1619 no . . N2 H4 3.1102 no . . N2 H12 2.4688 no . . N2 H13B 3.4724 no . . N2 H15 2.5139 no . . N2 H16A 2.9840 no . . N2 H24 3.1903 no . . N5 H3 3.1076 no . . N5 H15 3.2937 no . . N5 H24 2.3996 no . . N5 H25B 3.3159 no . . N5 H27 2.4695 no . . N5 H28A 3.4162 no . . C1 H3 3.1639 no . . C1 H4 3.1592 no . . C1 H12 3.1663 no . . C1 H15 2.6051 no . . C1 H24 2.7667 no . . C1 H27 2.9753 no . . C3 H12 2.8217 no . . C3 H13B 3.1530 no . . C3 H15 3.2502 no . . C3 H16A 2.8357 no . . C3 H24 3.2050 no . . C4 H12 3.5985 no . . C4 H24 2.7496 no . . C4 H25B 2.9421 no . . C4 H27 3.1248 no . . C4 H28A 3.3586 no . . C6 H3 2.8131 no . . C6 H8 3.2314 no . . C6 H10 3.2425 no . . C6 H12 2.6100 no . . C6 H13B 3.2888 no . . C6 H15 2.6570 no . . C6 H16A 3.0419 no . . C6 H42B 3.4812 no . . C7 H3 3.3820 no . . C7 H9 3.2565 no . . C7 H13A 2.6930 no . . C7 H13B 2.6868 no . . C7 H13C 3.3421 no . . C7 H14A 2.7290 no . . C7 H14B 2.7367 no . . C7 H14C 3.3652 no . . C7 H42B 3.3754 no . . C8 H10 3.2298 no . . C8 H12 3.3011 no . . C8 H13A 2.9242 no . . C8 H13B 3.4954 no . . C8 H14A 3.1892 no . . C8 H14B 2.7269 no . . C8 H41B 3.5184 no . . C8 H42B 3.4059 no . . C9 H41B 3.5971 no . . C9 H42B 3.5754 no . . C10 H8 3.2298 no . . C10 H15 3.2617 no . . C10 H16B 3.1218 no . . C10 H17A 2.7152 no . . C10 H17B 3.0334 no . . C11 H9 3.2589 no . . C11 H16A 2.6673 no . . C11 H16B 2.6890 no . . C11 H16C 3.3361 no . . C11 H17A 2.7799 no . . C11 H17B 2.7651 no . . C11 H17C 3.3930 no . . C12 H3 3.4179 no . . C12 H8 2.6486 no . . C13 H3 3.3740 no . . C13 H8 3.1434 no . . C13 H14A 3.3532 no . . C13 H14B 2.7032 no . . C13 H14C 2.6694 no . . C14 H8 2.7236 no . . C14 H13A 2.7204 no . . C14 H13B 3.3498 no . . C14 H13C 2.6591 no . . C14 H41A 3.4008 no . . C15 H10 2.6544 no . . C15 H24 3.1579 no . . C16 H10 3.4094 no . . C16 H17A 2.7095 no . . C16 H17B 3.3558 no . . C16 H17C 2.6772 no . . C16 H24 3.3504 no . . C17 H10 2.5785 no . . C17 H16A 3.3561 no . . C17 H16B 2.7263 no . . C17 H16C 2.6580 no . . C18 H4 2.8226 no . . C18 H20 3.2318 no . . C18 H22 3.2363 no . . C18 H24 2.6043 no . . C18 H25B 3.2115 no . . C18 H27 2.6058 no . . C18 H28A 3.2316 no . . C18 H50 3.4846 no . . C19 H4 3.4592 no . . C19 H21 3.2535 no . . C19 H25A 2.6762 no . . C19 H25B 2.6796 no . . C19 H25C 3.3339 no . . C19 H26A 2.7473 no . . C19 H26B 2.7425 no . . C19 H26C 3.3704 no . . C20 H22 3.2334 no . . C20 H24 3.2974 no . . C20 H25A 2.9595 no . . C20 H25B 3.5430 no . . C20 H26A 3.1889 no . . C20 H26B 2.7331 no . . C20 H51 3.2073 no . . C21 H50 3.5381 no . . C21 H51 3.4215 no . . C22 H20 3.2339 no . . C22 H27 3.3013 no . . C22 H28A 3.5014 no . . C22 H28B 2.9180 no . . C22 H29A 2.7140 no . . C22 H29B 3.1784 no . . C22 H50 3.3812 no . . C23 H4 3.5907 no . . C23 H21 3.2689 no . . C23 H28A 2.6603 no . . C23 H28B 2.6664 no . . C23 H28C 3.3250 no . . C23 H29A 2.7299 no . . C23 H29B 2.7238 no . . C23 H29C 3.3587 no . . C23 H50 3.3794 no . . C24 H4 3.5309 no . . C24 H15 3.1772 no . . C24 H20 2.6612 no . . C25 H4 3.4085 no . . C25 H20 3.2193 no . . C25 H26A 3.3382 no . . C25 H26B 2.7017 no . . C25 H26C 2.6459 no . . C26 H15 3.4420 no . . C26 H20 2.7130 no . . C26 H25A 2.7237 no . . C26 H25B 3.3341 no . . C26 H25C 2.6324 no . . C27 H22 2.6594 no . . C28 H22 3.1720 no . . C28 H29A 2.7242 no . . C28 H29B 3.3607 no . . C28 H29C 2.6894 no . . C29 H22 2.7196 no . . C29 H28A 3.3556 no . . C29 H28B 2.7482 no . . C29 H28C 2.6768 no . . C31 H33A 2.7299 no . . C31 H33B 3.3660 no . . C31 H34A 3.3097 no . . C31 H35A 3.3618 no . . C31 H35B 2.7201 no . . C31 H38A 3.1220 no . . C31 H38B 3.5502 no . . C31 H42A 3.3976 no . . C31 H50 3.5576 no . . C32 H34A 2.7370 no . . C32 H34B 3.3522 no . . C32 H35B 3.2918 no . . C32 H36A 2.7040 no . . C32 H36B 3.3633 no . . C32 H38A 3.0067 no . . C32 H38B 3.2702 no . . C32 H54 3.5196 no . . C33 H31 2.6020 no . . C33 H35A 3.3561 no . . C33 H35B 2.7480 no . . C33 H36A 3.2716 no . . C34 H31 3.1209 no . . C34 H32A 3.3531 no . . C34 H32B 2.7266 no . . C34 H36A 2.7359 no . . C34 H36B 3.3639 no . . C35 H31 2.5929 no . . C35 H32B 3.2640 no . . C35 H33A 2.7503 no . . C35 H33B 3.3568 no . . C36 H32A 3.3618 no . . C36 H32B 2.7028 no . . C36 H33A 3.3076 no . . C36 H34A 2.7443 no . . C36 H34B 3.3629 no . . C36 H38A 3.2134 no . . C36 H42A 2.7864 no . . C37 H32B 3.3753 no . . C37 H36A 3.0884 no . . C37 H36B 3.5136 no . . C37 H39A 3.3581 no . . C37 H39B 2.7271 no . . C37 H40B 3.3136 no . . C37 H41A 2.7348 no . . C37 H41B 3.3654 no . . C37 H48 2.5978 no . . C38 H32B 2.7965 no . . C38 H36A 3.2042 no . . C38 H40A 3.3545 no . . C38 H40B 2.7442 no . . C38 H41A 3.2928 no . . C38 H42A 2.7531 no . . C38 H42B 3.3795 no . . C38 H48 2.9671 no . . C39 H37 2.6044 no . . C39 H41A 2.7419 no . . C39 H41B 3.3519 no . . C39 H42A 3.3069 no . . C40 H37 3.1433 no . . C40 H38A 2.7352 no . . C40 H38B 3.3545 no . . C40 H42A 2.7750 no . . C40 H42B 3.3853 no . . C41 H14A 3.4970 no . . C41 H37 2.6085 no . . C41 H38A 3.2774 no . . C41 H39A 3.3555 no . . C41 H39B 2.7387 no . . C42 H36A 3.0092 no . . C42 H36B 3.2388 no . . C42 H38A 2.7424 no . . C42 H38B 3.3799 no . . C42 H39B 3.3075 no . . C42 H40A 3.3840 no . . C42 H40B 2.7745 no . . C43 H29B 3.3063 no . . C43 H31 3.1896 no . . C43 H32A 2.7469 no . . C43 H32B 3.5550 no . . C43 H37 2.9553 no . . C43 H38B 3.0779 no . . C43 H45 3.2630 no . . C43 H47 3.2867 no . . C43 H50 3.1151 no . . C44 H29B 3.2694 no . . C44 H31 3.2806 no . . C44 H32A 2.7519 no . . C44 H46 3.2773 no . . C44 H48 3.2649 no . . C44 H50 2.6743 no . . C44 H54 2.6464 no . . C45 H29B 3.3536 no . . C45 H47 3.2195 no . . C45 H54 2.8850 no . . C46 H29B 3.4541 no . . C46 H48 3.2350 no . . C47 H29B 3.4539 no . . C47 H45 3.2121 no . . C48 H29B 3.3813 no . . C48 H37 2.7229 no . . C48 H38B 2.8940 no . . C48 H46 3.2456 no . . C49 H31 2.6696 no . . C49 H32A 2.8136 no . . C49 H45 2.5474 no . . C49 H51 3.2565 no . . C49 H53 3.2527 no . . C50 H31 2.6606 no . . C50 H52 3.2526 no . . C50 H54 3.2348 no . . C51 H31 3.1794 no . . C51 H53 3.2143 no . . C52 H50 3.2429 no . . C52 H54 3.2465 no . . C53 H33A 3.1669 no . . C53 H51 3.2171 no . . C54 H31 3.2138 no . . C54 H32A 2.8659 no . . C54 H33A 3.0933 no . . C54 H45 2.7851 no . . C54 H50 3.2346 no . . C54 H52 3.2522 no . . H3 H4 2.4631 no . . H3 H12 3.0204 no . . H3 H13B 2.5983 no . . H3 H16A 2.7499 no . . H4 H24 3.1690 no . . H4 H25B 2.5882 no . . H4 H27 3.4523 no . . H4 H28A 2.9972 no . . H8 H9 2.2962 no . . H8 H12 3.5759 no . . H8 H13A 2.6798 no . . H8 H14A 3.0407 no . . H8 H14B 2.1709 no . . H8 H14C 3.5960 no . . H8 H41B 3.3928 no . . H9 H10 2.3223 no . . H9 H41B 3.5194 no . . H10 H15 3.5174 no . . H10 H16B 3.0673 no . . H10 H17A 2.0992 no . . H10 H17B 2.7130 no . . H10 H17C 3.5094 no . . H12 H13A 2.8740 no . . H12 H13B 2.3630 no . . H12 H13C 2.3814 no . . H12 H14A 2.3609 no . . H12 H14B 2.8640 no . . H12 H14C 2.3587 no . . H13A H14B 2.5542 no . . H13A H14C 2.9909 no . . H13B H14C 3.5515 no . . H13C H14A 3.5540 no . . H13C H14B 2.9498 no . . H13C H14C 2.4522 no . . H14A H37 3.4031 no . . H14A H41A 2.6741 no . . H14A H42B 3.2693 no . . H14B H41A 3.2609 no . . H15 H16A 2.3518 no . . H15 H16B 2.8652 no . . H15 H16C 2.3689 no . . H15 H17A 2.8704 no . . H15 H17B 2.3715 no . . H15 H17C 2.3614 no . . H15 H24 2.2860 no . . H15 H26A 3.1626 no . . H15 H26C 3.4013 no . . H16A H17C 3.5582 no . . H16A H24 3.1927 no . . H16B H17A 2.5625 no . . H16B H17C 3.0014 no . . H16C H17A 2.9479 no . . H16C H17B 3.5526 no . . H16C H17C 2.4546 no . . H16C H24 3.1493 no . . H16C H26C 3.3076 no . . H17B H36B 3.4985 no . . H17C H26A 3.4398 no . . H17C H26C 3.3525 no . . H20 H21 2.2986 no . . H20 H24 3.5752 no . . H20 H25A 2.7797 no . . H20 H26A 3.0033 no . . H20 H26B 2.1642 no . . H20 H26C 3.5951 no . . H20 H51 3.2101 no . . H21 H22 2.3228 no . . H21 H51 3.5457 no . . H22 H27 3.5825 no . . H22 H28B 2.7131 no . . H22 H29A 2.1617 no . . H22 H29B 3.0293 no . . H22 H29C 3.5936 no . . H24 H25A 2.8631 no . . H24 H25B 2.3407 no . . H24 H25C 2.3757 no . . H24 H26A 2.3416 no . . H24 H26B 2.8531 no . . H24 H26C 2.3493 no . . H25A H26B 2.5707 no . . H25A H26C 2.9864 no . . H25B H26C 3.5220 no . . H25C H26A 3.5251 no . . H25C H26B 2.9334 no . . H25C H26C 2.4126 no . . H26A H51 3.3249 no . . H27 H28A 2.3474 no . . H27 H28B 2.8676 no . . H27 H28C 2.3802 no . . H27 H29A 2.8518 no . . H27 H29B 2.3419 no . . H27 H29C 2.3459 no . . H28A H29C 3.5635 no . . H28B H29A 2.5929 no . . H28B H29C 3.0253 no . . H28C H29A 2.9699 no . . H28C H29B 3.5687 no . . H28C H29C 2.4786 no . . H29B H50 3.3044 no . . H31 H32A 2.3791 no . . H31 H32B 2.8540 no . . H31 H33A 2.4404 no . . H31 H33B 3.5200 no . . H31 H35A 3.5101 no . . H31 H35B 2.4254 no . . H31 H36A 2.8534 no . . H31 H36B 2.3773 no . . H31 H50 2.9154 no . . H32A H33A 2.3614 no . . H32A H33B 2.3845 no . . H32A H38A 3.4857 no . . H32A H38B 3.2792 no . . H32A H54 2.7162 no . . H32B H33A 2.8739 no . . H32B H33B 2.3626 no . . H32B H34A 2.5917 no . . H32B H36A 2.5279 no . . H32B H38A 2.2227 no . . H32B H38B 2.6419 no . . H33A H34A 2.8609 no . . H33A H34B 2.3368 no . . H33A H35B 2.6215 no . . H33A H53 3.3553 no . . H33A H54 3.2336 no . . H33B H34A 2.3347 no . . H33B H34B 2.3781 no . . H34A H35A 2.3392 no . . H34A H35B 2.8632 no . . H34A H36A 2.5988 no . . H34B H35A 2.3787 no . . H34B H35B 2.3410 no . . H35A H36A 2.3745 no . . H35A H36B 2.3919 no . . H35B H36A 2.8812 no . . H35B H36B 2.3714 no . . H36A H38A 2.4989 no . . H36A H42A 2.2390 no . . H36A H42B 3.5198 no . . H36B H42A 2.5963 no . . H36B H42B 3.2831 no . . H37 H38A 2.8453 no . . H37 H38B 2.3568 no . . H37 H39A 3.5179 no . . H37 H39B 2.4444 no . . H37 H41A 2.4529 no . . H37 H41B 3.5255 no . . H37 H42A 2.8556 no . . H37 H42B 2.3627 no . . H37 H48 2.0066 no . . H38A H39A 2.3516 no . . H38A H39B 2.8660 no . . H38A H40B 2.6044 no . . H38A H42A 2.6007 no . . H38B H39A 2.3750 no . . H38B H39B 2.3492 no . . H38B H48 2.5142 no . . H39A H40A 2.3756 no . . H39A H40B 2.3363 no . . H39B H40A 2.3349 no . . H39B H40B 2.8598 no . . H39B H41A 2.6069 no . . H39B H48 3.2565 no . . H40A H41A 2.3478 no . . H40A H41B 2.3889 no . . H40B H41A 2.8710 no . . H40B H41B 2.3497 no . . H40B H42A 2.6487 no . . H41A H42A 2.8799 no . . H41A H42B 2.3599 no . . H41B H42A 2.3656 no . . H41B H42B 2.3998 no . . H45 H46 2.3055 no . . H45 H54 2.6091 no . . H46 H47 2.3309 no . . H47 H48 2.3116 no . . H50 H51 2.3207 no . . H51 H52 2.3252 no . . H52 H53 2.3218 no . . H53 H54 2.3105 no . . Cl1 H4 2.7652 no . 2_655 Cl1 H25B 3.2415 no . 2_655 Cl2 H52 2.9896 no . 3_655 C3 H29C 2.9104 no . 2_645 C3 H47 3.2939 no . 2_645 C4 H29C 3.1771 no . 2_645 C8 H22 3.1110 no . 1_655 C8 H45 3.3336 no . 1_655 C9 H21 3.2554 no . 1_655 C9 H22 3.2517 no . 1_655 C9 H45 3.2666 no . 1_655 C10 H21 3.1316 no . 1_655 C12 H25A 3.4729 no . 2_655 C13 H25A 3.4327 no . 2_655 C13 H46 3.2653 no . 2_645 C13 H47 3.1492 no . 2_645 C14 H28A 3.4155 no . 2_655 C14 H28B 3.4969 no . 2_655 C16 H28C 3.4038 no . 2_645 C16 H35A 3.3717 no . 3_755 C17 H17B 3.5862 no . 3_755 C17 H35A 3.4412 no . 3_755 C18 H14C 3.2130 no . 2_645 C19 H14C 3.1188 no . 2_645 C20 H13C 3.3469 no . 2_645 C20 H14C 2.9575 no . 2_645 C20 H34B 3.4483 no . 3_655 C21 H14C 2.9088 no . 2_645 C22 H14C 2.9815 no . 2_645 C23 H14C 3.1417 no . 2_645 C25 H12 3.3141 no . 2_645 C25 H27 3.4292 no . 2_645 C25 H28C 3.2834 no . 2_645 C25 H47 3.1711 no . 1_545 C26 H33A 3.1643 no . 3_655 C26 H53 3.0520 no . 3_655 C27 H25B 3.5948 no . 2_655 C28 H14A 3.4356 no . 2_645 C28 H25C 3.1492 no . 2_655 C28 H39B 3.4366 no . 2_645 C28 H41A 3.5907 no . 2_645 C29 H3 3.2374 no . 2_655 C32 H32A 3.1703 no . 3_665 C32 H33B 3.5810 no . 3_665 C33 H26B 3.0838 no . 3_655 C33 H32A 3.4368 no . 3_665 C34 H20 3.3565 no . 3_655 C34 H26B 3.3920 no . 3_655 C34 H40A 3.3947 no . 3_765 C34 H46 3.5385 no . 3_665 C35 H16B 3.5769 no . 3_755 C35 H17A 3.4539 no . 3_755 C35 H40A 3.4794 no . 3_765 C39 H16C 3.4125 no . 1_565 C39 H26C 3.2962 no . 1_565 C40 H34A 3.4027 no . 3_765 C40 H36A 3.3530 no . 3_765 C41 H45 3.4465 no . 1_655 C43 H33B 3.2206 no . 3_665 C44 H9 3.4122 no . 1_455 C44 H33B 3.2910 no . 3_665 C45 H8 3.3644 no . 1_455 C45 H9 3.2658 no . 1_455 C45 H33B 3.2240 no . 3_665 C45 H34A 3.3330 no . 3_665 C45 H41B 3.4205 no . 1_455 C46 H13B 3.2196 no . 2_655 C46 H33B 3.1598 no . 3_665 C46 H34A 3.1244 no . 3_665 C46 H34B 3.3303 no . 3_665 C47 H3 3.2540 no . 2_655 C47 H13B 3.2522 no . 2_655 C47 H13C 3.5287 no . 2_655 C47 H25A 3.1697 no . 1_565 C47 H33B 3.1002 no . 3_665 C47 H34B 3.4929 no . 3_665 C48 H33B 3.1082 no . 3_665 C49 H9 2.7303 no . 1_455 C50 H9 2.7931 no . 1_455 C51 H9 3.0693 no . 1_455 C51 H10 3.4945 no . 1_455 C52 H9 3.2575 no . 1_455 C52 H10 3.2029 no . 1_455 C52 H26A 3.1651 no . 3_655 C53 H9 3.1518 no . 1_455 C53 H10 3.5633 no . 1_455 C53 H26A 3.1294 no . 3_655 C53 H26C 3.3685 no . 3_655 C54 H9 2.9026 no . 1_455 H3 C29 3.2374 no . 2_645 H3 C47 3.2540 no . 2_645 H3 H29A 3.5742 no . 2_645 H3 H29B 3.3580 no . 2_645 H3 H29C 2.4078 no . 2_645 H3 H47 2.8653 no . 2_645 H4 Cl1 2.7652 no . 2_645 H4 H29B 3.5439 no . 2_645 H4 H29C 2.9712 no . 2_645 H4 H47 3.5700 no . 2_645 H4 H48 3.3891 no . 2_645 H8 C45 3.3644 no . 1_655 H8 H22 3.0848 no . 1_655 H8 H29A 3.0012 no . 1_655 H8 H45 2.8088 no . 1_655 H9 C44 3.4122 no . 1_655 H9 C45 3.2658 no . 1_655 H9 C49 2.7303 no . 1_655 H9 C50 2.7931 no . 1_655 H9 C51 3.0693 no . 1_655 H9 C52 3.2575 no . 1_655 H9 C53 3.1518 no . 1_655 H9 C54 2.9026 no . 1_655 H9 H21 3.4347 no . 1_655 H9 H22 3.3401 no . 1_655 H9 H45 2.6766 no . 1_655 H9 H50 3.2378 no . 1_655 H9 H54 3.4039 no . 1_655 H10 C51 3.4945 no . 1_655 H10 C52 3.2029 no . 1_655 H10 C53 3.5633 no . 1_655 H10 H21 3.2256 no . 1_655 H10 H52 3.2757 no . 1_655 H12 C25 3.3141 no . 2_655 H12 H25A 2.8503 no . 2_655 H12 H25B 2.8854 no . 2_655 H12 H47 3.3276 no . 2_645 H13A H22 3.0256 no . 1_655 H13A H28B 3.4669 no . 1_655 H13A H29A 2.8529 no . 1_655 H13B C46 3.2196 no . 2_645 H13B C47 3.2522 no . 2_645 H13B H46 2.6246 no . 2_645 H13B H47 2.6793 no . 2_645 H13C C20 3.3469 no . 2_655 H13C C47 3.5287 no . 2_645 H13C H20 3.1162 no . 2_655 H13C H25A 2.7988 no . 2_655 H13C H34B 3.3893 no . 4_555 H13C H46 3.1067 no . 2_645 H13C H47 2.8280 no . 2_645 H14A C28 3.4356 no . 2_655 H14A H28A 2.8047 no . 2_655 H14A H28B 3.1814 no . 2_655 H14B H28B 3.3801 no . 2_655 H14C C18 3.2130 no . 2_655 H14C C19 3.1188 no . 2_655 H14C C20 2.9575 no . 2_655 H14C C21 2.9088 no . 2_655 H14C C22 2.9815 no . 2_655 H14C C23 3.1417 no . 2_655 H14C H20 3.4412 no . 2_655 H14C H21 3.3895 no . 2_655 H14C H22 3.4760 no . 2_655 H14C H25A 3.2500 no . 2_655 H14C H25B 3.2242 no . 2_655 H14C H28A 3.2517 no . 2_655 H14C H28B 3.3497 no . 2_655 H16A H28C 3.0235 no . 2_645 H16A H29C 2.8618 no . 2_645 H16B C35 3.5769 no . 3_755 H16B H21 2.9692 no . 1_655 H16B H35A 2.6617 no . 3_755 H16C C39 3.4125 no . 1_545 H16C H28C 2.9055 no . 2_645 H16C H35A 3.3198 no . 3_755 H16C H39A 3.1167 no . 1_545 H16C H39B 2.9140 no . 1_545 H16C H40A 3.3439 no . 1_545 H17A C35 3.4539 no . 3_755 H17A H17B 3.2459 no . 3_755 H17A H35A 2.7232 no . 3_755 H17A H35B 3.4649 no . 3_755 H17A H36B 3.4180 no . 3_755 H17B C17 3.5862 no . 3_755 H17B H17A 3.2459 no . 3_755 H17B H17B 3.2008 no . 3_755 H17C H35A 3.4273 no . 3_755 H17C H39A 3.1480 no . 1_545 H17C H53 3.0206 no . 3_655 H20 C34 3.3565 no . 3_655 H20 H13C 3.1162 no . 2_645 H20 H14C 3.4412 no . 2_645 H20 H33A 3.5780 no . 3_655 H20 H34B 2.5177 no . 3_655 H20 H35B 3.2070 no . 3_655 H21 C9 3.2554 no . 1_455 H21 C10 3.1316 no . 1_455 H21 H9 3.4347 no . 1_455 H21 H10 3.2256 no . 1_455 H21 H14C 3.3895 no . 2_645 H21 H16B 2.9692 no . 1_455 H22 C8 3.1110 no . 1_455 H22 C9 3.2517 no . 1_455 H22 H8 3.0848 no . 1_455 H22 H9 3.3401 no . 1_455 H22 H13A 3.0256 no . 1_455 H22 H14C 3.4760 no . 2_645 H25A C12 3.4729 no . 2_645 H25A C13 3.4327 no . 2_645 H25A C47 3.1697 no . 1_545 H25A H12 2.8503 no . 2_645 H25A H13C 2.7988 no . 2_645 H25A H14C 3.2500 no . 2_645 H25A H47 2.3678 no . 1_545 H25A H48 3.5079 no . 1_545 H25B Cl1 3.2415 no . 2_645 H25B C27 3.5948 no . 2_645 H25B H12 2.8854 no . 2_645 H25B H14C 3.2242 no . 2_645 H25B H27 2.8446 no . 2_645 H25B H28C 3.2446 no . 2_645 H25B H29C 3.4511 no . 2_645 H25C C28 3.1492 no . 2_645 H25C H27 3.1464 no . 2_645 H25C H28A 3.0901 no . 2_645 H25C H28C 2.5100 no . 2_645 H25C H39B 3.1358 no . 1_545 H25C H47 3.1683 no . 1_545 H25C H48 3.1927 no . 1_545 H26A C52 3.1651 no . 3_655 H26A C53 3.1294 no . 3_655 H26A H33A 3.3731 no . 3_655 H26A H52 2.7837 no . 3_655 H26A H53 2.7135 no . 3_655 H26B C33 3.0838 no . 3_655 H26B C34 3.3920 no . 3_655 H26B H33A 2.3859 no . 3_655 H26B H33B 3.1851 no . 3_655 H26B H34B 2.8475 no . 3_655 H26B H53 3.3159 no . 3_655 H26C C39 3.2962 no . 1_545 H26C C53 3.3685 no . 3_655 H26C H33A 3.3207 no . 3_655 H26C H38B 3.0891 no . 1_545 H26C H39A 2.9038 no . 1_545 H26C H39B 2.9548 no . 1_545 H26C H53 2.6665 no . 3_655 H27 C25 3.4292 no . 2_655 H27 H25B 2.8446 no . 2_655 H27 H25C 3.1464 no . 2_655 H28A C14 3.4155 no . 2_645 H28A H14A 2.8047 no . 2_645 H28A H14C 3.2517 no . 2_645 H28A H25C 3.0901 no . 2_655 H28A H37 3.3151 no . 2_645 H28A H39B 3.2435 no . 2_645 H28A H41A 3.2276 no . 2_645 H28A H48 3.5499 no . 2_645 H28B C14 3.4969 no . 2_645 H28B H13A 3.4669 no . 1_455 H28B H14A 3.1814 no . 2_645 H28B H14B 3.3801 no . 2_645 H28B H14C 3.3497 no . 2_645 H28B H41A 3.2735 no . 2_645 H28C C16 3.4038 no . 2_655 H28C C25 3.2834 no . 2_655 H28C H16A 3.0235 no . 2_655 H28C H16C 2.9055 no . 2_655 H28C H25B 3.2446 no . 2_655 H28C H25C 2.5100 no . 2_655 H28C H39B 2.8944 no . 2_645 H29A H3 3.5742 no . 2_655 H29A H8 3.0012 no . 1_455 H29A H13A 2.8529 no . 1_455 H29B H3 3.3580 no . 2_655 H29B H4 3.5439 no . 2_655 H29C C3 2.9104 no . 2_655 H29C C4 3.1771 no . 2_655 H29C H3 2.4078 no . 2_655 H29C H4 2.9712 no . 2_655 H29C H16A 2.8618 no . 2_655 H29C H25B 3.4511 no . 2_655 H32A C32 3.1703 no . 3_665 H32A C33 3.4368 no . 3_665 H32A H32A 2.7280 no . 3_665 H32A H32B 2.9821 no . 3_665 H32A H33B 2.8037 no . 3_665 H32B H32A 2.9821 no . 3_665 H32B H33B 3.4620 no . 3_665 H32B H54 2.7896 no . 3_665 H33A C26 3.1643 no . 3_655 H33A H20 3.5780 no . 3_655 H33A H26A 3.3731 no . 3_655 H33A H26B 2.3859 no . 3_655 H33A H26C 3.3207 no . 3_655 H33B C32 3.5810 no . 3_665 H33B C43 3.2206 no . 3_665 H33B C44 3.2910 no . 3_665 H33B C45 3.2240 no . 3_665 H33B C46 3.1598 no . 3_665 H33B C47 3.1002 no . 3_665 H33B C48 3.1082 no . 3_665 H33B H26B 3.1851 no . 3_655 H33B H32A 2.8037 no . 3_665 H33B H32B 3.4620 no . 3_665 H33B H38B 3.1592 no . 3_665 H33B H47 3.5832 no . 3_665 H33B H48 3.5816 no . 3_665 H34A C40 3.4027 no . 3_765 H34A C45 3.3330 no . 3_665 H34A C46 3.1244 no . 3_665 H34A H40A 2.5985 no . 3_765 H34A H40B 3.4505 no . 3_765 H34A H45 3.3462 no . 3_665 H34A H46 3.0147 no . 3_665 H34B C20 3.4483 no . 3_655 H34B C46 3.3303 no . 3_665 H34B C47 3.4929 no . 3_665 H34B H13C 3.3893 no . 4_454 H34B H20 2.5177 no . 3_655 H34B H26B 2.8475 no . 3_655 H34B H46 3.1986 no . 3_665 H34B H47 3.4853 no . 3_665 H35A C16 3.3717 no . 3_755 H35A C17 3.4412 no . 3_755 H35A H16B 2.6617 no . 3_755 H35A H16C 3.3198 no . 3_755 H35A H17A 2.7232 no . 3_755 H35A H17C 3.4273 no . 3_755 H35A H40A 3.0286 no . 3_765 H35B H17A 3.4649 no . 3_755 H35B H20 3.2070 no . 3_655 H35B H51 3.2776 no . 3_655 H35B H52 3.3926 no . 3_655 H36A C40 3.3530 no . 3_765 H36A H40A 2.9669 no . 3_765 H36A H40B 2.8270 no . 3_765 H36B H17A 3.4180 no . 3_755 H37 H28A 3.3151 no . 2_655 H38A H40B 3.0043 no . 3_765 H38A H54 3.1472 no . 3_665 H38B H26C 3.0891 no . 1_565 H38B H33B 3.1592 no . 3_665 H38B H53 3.5665 no . 3_665 H38B H54 3.3219 no . 3_665 H39A H16C 3.1167 no . 1_565 H39A H17C 3.1480 no . 1_565 H39A H26C 2.9038 no . 1_565 H39A H53 2.8923 no . 3_665 H39B C28 3.4366 no . 2_655 H39B H16C 2.9140 no . 1_565 H39B H25C 3.1358 no . 1_565 H39B H26C 2.9548 no . 1_565 H39B H28A 3.2435 no . 2_655 H39B H28C 2.8944 no . 2_655 H40A C34 3.3947 no . 3_765 H40A C35 3.4794 no . 3_765 H40A H16C 3.3439 no . 1_565 H40A H34A 2.5985 no . 3_765 H40A H35A 3.0286 no . 3_765 H40A H36A 2.9669 no . 3_765 H40B H34A 3.4505 no . 3_765 H40B H36A 2.8270 no . 3_765 H40B H38A 3.0043 no . 3_765 H40B H40B 2.7182 no . 3_765 H40B H42A 3.3346 no . 3_765 H41A C28 3.5907 no . 2_655 H41A H28A 3.2276 no . 2_655 H41A H28B 3.2735 no . 2_655 H41A H45 3.5820 no . 1_655 H41B C45 3.4205 no . 1_655 H41B H45 2.5392 no . 1_655 H41B H54 3.4737 no . 1_655 H42A H40B 3.3346 no . 3_765 H45 C8 3.3336 no . 1_455 H45 C9 3.2666 no . 1_455 H45 C41 3.4465 no . 1_455 H45 H8 2.8088 no . 1_455 H45 H9 2.6766 no . 1_455 H45 H34A 3.3462 no . 3_665 H45 H41A 3.5820 no . 1_455 H45 H41B 2.5392 no . 1_455 H46 C13 3.2653 no . 2_655 H46 C34 3.5385 no . 3_665 H46 H13B 2.6246 no . 2_655 H46 H13C 3.1067 no . 2_655 H46 H34A 3.0147 no . 3_665 H46 H34B 3.1986 no . 3_665 H47 C3 3.2939 no . 2_655 H47 C13 3.1492 no . 2_655 H47 C25 3.1711 no . 1_565 H47 H3 2.8653 no . 2_655 H47 H4 3.5700 no . 2_655 H47 H12 3.3276 no . 2_655 H47 H13B 2.6793 no . 2_655 H47 H13C 2.8280 no . 2_655 H47 H25A 2.3678 no . 1_565 H47 H25C 3.1683 no . 1_565 H47 H33B 3.5832 no . 3_665 H47 H34B 3.4853 no . 3_665 H48 H4 3.3891 no . 2_655 H48 H25A 3.5079 no . 1_565 H48 H25C 3.1927 no . 1_565 H48 H28A 3.5499 no . 2_655 H48 H33B 3.5816 no . 3_665 H50 H9 3.2378 no . 1_455 H51 H35B 3.2776 no . 3_655 H51 H52 3.5066 no . 3_655 H52 Cl2 2.9896 no . 3_655 H52 H10 3.2757 no . 1_455 H52 H26A 2.7837 no . 3_655 H52 H35B 3.3926 no . 3_655 H52 H51 3.5066 no . 3_655 H53 C26 3.0520 no . 3_655 H53 H17C 3.0206 no . 3_655 H53 H26A 2.7135 no . 3_655 H53 H26B 3.3159 no . 3_655 H53 H26C 2.6665 no . 3_655 H53 H38B 3.5665 no . 3_665 H53 H39A 2.8923 no . 3_665 H54 H9 3.4039 no . 1_455 H54 H32B 2.7896 no . 3_665 H54 H38A 3.1472 no . 3_665 H54 H38B 3.3219 no . 3_665 H54 H41B 3.4737 no . 1_455 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 913234' #TrackingRef '15786_web_deposit_cif_file_0_CatherineCazin_1354182998.5.cif' _chemical_formula_sum 'C52 H70 Cl4 O4 P2 Pd2' _chemical_formula_moiety 'C52 H70 Cl4 O4 P2 Pd2' _chemical_formula_weight 1175.68 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.390(10) _cell_length_b 10.444(11) _cell_length_c 13.796(15) _cell_angle_alpha 103.695(14) _cell_angle_beta 103.287(16) _cell_angle_gamma 96.525(10) _cell_volume 1259(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3632 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.35 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604.00 _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.387 _exptl_absorpt_correction_T_max 0.950 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.257 _diffrn_reflns_number 11553 _diffrn_reflns_av_R_equivalents 0.1775 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4471 _reflns_number_gt 3998 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1309 _refine_ls_wR_factor_ref 0.3519 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4471 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.404 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.003 _refine_diff_density_max 3.780 _refine_diff_density_min -4.060 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Pd Pd -0.9988 1.0072 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.46362(5) 0.46878(5) 0.36468(3) 0.0303(4) Uani 1.0 2 d . . . Cl1 Cl 0.5320(3) 0.35048(19) 0.48637(14) 0.0302(6) Uani 1.0 2 d . . . Cl2 Cl 0.3927(3) 0.59557(19) 0.25410(14) 0.0356(6) Uani 1.0 2 d . . . P1 P 0.4634(2) 0.30662(19) 0.22459(14) 0.0290(6) Uani 1.0 2 d . . . O20 O 0.1014(6) 0.4290(5) 0.2974(4) 0.0366(12) Uani 1.0 2 d . . . O24 O 0.2061(7) 0.0007(6) 0.2715(4) 0.0370(12) Uani 1.0 2 d . . . C1 C 0.5729(8) 0.3761(7) 0.1478(5) 0.0283(15) Uani 1.0 2 d . . . C2 C 0.7109(9) 0.4823(9) 0.2153(6) 0.0398(18) Uani 1.0 2 d . . . C3 C 0.7716(9) 0.5589(9) 0.1488(6) 0.0400(18) Uani 1.0 2 d . . . C4 C 0.8161(10) 0.4636(9) 0.0623(7) 0.0421(19) Uani 1.0 2 d . . . C5 C 0.6864(9) 0.3528(9) 0.0001(6) 0.0379(18) Uani 1.0 2 d . . . C6 C 0.6228(8) 0.2769(8) 0.0669(6) 0.0314(15) Uani 1.0 2 d . . . C7 C 0.5383(8) 0.1633(7) 0.2606(5) 0.0320(16) Uani 1.0 2 d . . . C8 C 0.7051(8) 0.2022(8) 0.3157(6) 0.0373(17) Uani 1.0 2 d . . . C9 C 0.7566(9) 0.0937(8) 0.3638(6) 0.0385(18) Uani 1.0 2 d . . . C10 C 0.7243(10) -0.0400(9) 0.2797(6) 0.045(2) Uani 1.0 2 d . . . C11 C 0.5625(9) -0.0774(8) 0.2216(6) 0.0398(18) Uani 1.0 2 d . . . C12 C 0.5071(9) 0.0337(7) 0.1744(6) 0.0342(17) Uani 1.0 2 d . . . C13 C 0.2738(8) 0.2424(7) 0.1400(5) 0.0299(15) Uani 1.0 2 d . . . C14 C 0.1542(8) 0.2041(8) 0.1781(6) 0.0321(16) Uani 1.0 2 d . . . C15 C 0.0125(8) 0.1622(8) 0.1102(6) 0.0358(17) Uani 1.0 2 d . . . C16 C -0.0116(9) 0.1519(8) 0.0051(6) 0.0329(16) Uani 1.0 2 d . . . C17 C 0.1062(9) 0.1883(8) -0.0319(6) 0.0341(17) Uani 1.0 2 d . . . C18 C 0.2464(9) 0.2308(8) 0.0333(6) 0.0352(17) Uani 1.0 2 d . . . C19 C 0.1639(8) 0.2188(8) 0.2906(6) 0.0324(16) Uani 1.0 2 d . . . C20 C 0.1352(8) 0.3393(8) 0.3510(6) 0.0349(17) Uani 1.0 2 d . . . C21 C 0.1409(9) 0.3553(8) 0.4547(7) 0.0402(19) Uani 1.0 2 d . . . C22 C 0.1665(9) 0.2504(8) 0.4966(6) 0.0368(18) Uani 1.0 2 d . . . C23 C 0.1892(9) 0.1316(9) 0.4391(6) 0.0407(18) Uani 1.0 2 d . . . C24 C 0.1849(8) 0.1153(8) 0.3352(6) 0.0341(17) Uani 1.0 2 d . . . C25 C 0.0889(9) 0.5604(8) 0.3554(6) 0.0391(18) Uani 1.0 2 d . . . C26 C 0.2065(11) -0.1151(9) 0.3077(7) 0.050(3) Uani 1.0 2 d . . . H1 H 0.5064 0.4251 0.1081 0.0339 Uiso 1.0 2 calc R . . H2A H 0.6827 0.5451 0.2707 0.0478 Uiso 1.0 2 calc R . . H2B H 0.7884 0.4376 0.2483 0.0478 Uiso 1.0 2 calc R . . H3A H 0.8594 0.6267 0.1923 0.0480 Uiso 1.0 2 calc R . . H3B H 0.6952 0.6062 0.1181 0.0480 Uiso 1.0 2 calc R . . H4A H 0.8480 0.5141 0.0163 0.0505 Uiso 1.0 2 calc R . . H4B H 0.9009 0.4244 0.0928 0.0505 Uiso 1.0 2 calc R . . H5A H 0.7193 0.2890 -0.0522 0.0454 Uiso 1.0 2 calc R . . H5B H 0.6070 0.3918 -0.0374 0.0454 Uiso 1.0 2 calc R . . H6A H 0.6994 0.2329 0.1017 0.0377 Uiso 1.0 2 calc R . . H6B H 0.5372 0.2069 0.0232 0.0377 Uiso 1.0 2 calc R . . H7 H 0.4882 0.1426 0.3131 0.0384 Uiso 1.0 2 calc R . . H8A H 0.7617 0.2150 0.2654 0.0448 Uiso 1.0 2 calc R . . H8B H 0.7240 0.2878 0.3702 0.0448 Uiso 1.0 2 calc R . . H9A H 0.7042 0.0844 0.4171 0.0462 Uiso 1.0 2 calc R . . H9B H 0.8647 0.1183 0.3978 0.0462 Uiso 1.0 2 calc R . . H10A H 0.7848 -0.0328 0.2306 0.0539 Uiso 1.0 2 calc R . . H10B H 0.7533 -0.1114 0.3122 0.0539 Uiso 1.0 2 calc R . . H11A H 0.5031 -0.0950 0.2693 0.0478 Uiso 1.0 2 calc R . . H11B H 0.5471 -0.1609 0.1656 0.0478 Uiso 1.0 2 calc R . . H12A H 0.5592 0.0462 0.1216 0.0411 Uiso 1.0 2 calc R . . H12B H 0.3991 0.0083 0.1405 0.0411 Uiso 1.0 2 calc R . . H15 H -0.0696 0.1402 0.1363 0.0430 Uiso 1.0 2 calc R . . H16 H -0.1084 0.1201 -0.0405 0.0394 Uiso 1.0 2 calc R . . H17 H 0.0903 0.1840 -0.1033 0.0410 Uiso 1.0 2 calc R . . H18 H 0.3270 0.2531 0.0059 0.0423 Uiso 1.0 2 calc R . . H21 H 0.1275 0.4374 0.4960 0.0482 Uiso 1.0 2 calc R . . H22 H 0.1685 0.2603 0.5672 0.0441 Uiso 1.0 2 calc R . . H23 H 0.2078 0.0608 0.4701 0.0488 Uiso 1.0 2 calc R . . H25A H 0.1838 0.6025 0.4065 0.0470 Uiso 1.0 2 calc R . . H25B H 0.0107 0.5517 0.3909 0.0470 Uiso 1.0 2 calc R . . H25C H 0.0638 0.6159 0.3079 0.0470 Uiso 1.0 2 calc R . . H26A H 0.1107 -0.1393 0.3216 0.0603 Uiso 1.0 2 calc R . . H26B H 0.2864 -0.0971 0.3715 0.0603 Uiso 1.0 2 calc R . . H26C H 0.2227 -0.1892 0.2551 0.0603 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.0327(6) 0.0413(6) 0.0154(6) 0.0065(4) 0.0076(4) 0.0037(4) Cl1 0.0354(11) 0.0406(11) 0.0140(10) 0.0090(8) 0.0076(8) 0.0041(8) Cl2 0.0448(12) 0.0446(12) 0.0200(10) 0.0147(9) 0.0114(9) 0.0081(8) P1 0.0294(11) 0.0402(11) 0.0149(10) 0.0056(8) 0.0053(8) 0.0038(8) O20 0.044(3) 0.041(3) 0.022(3) 0.009(3) 0.010(3) 0.003(2) O24 0.048(3) 0.043(3) 0.022(3) 0.010(3) 0.014(3) 0.008(3) C1 0.034(4) 0.038(4) 0.014(3) 0.005(3) 0.012(3) 0.005(3) C2 0.035(4) 0.049(5) 0.030(4) -0.002(4) 0.008(4) 0.007(4) C3 0.037(4) 0.050(5) 0.027(4) -0.001(4) 0.001(4) 0.009(4) C4 0.043(5) 0.057(5) 0.030(4) 0.005(4) 0.015(4) 0.017(4) C5 0.039(4) 0.063(6) 0.015(4) 0.014(4) 0.013(3) 0.008(4) C6 0.037(4) 0.049(4) 0.016(4) 0.013(3) 0.019(3) 0.010(3) C7 0.037(4) 0.039(4) 0.014(4) 0.014(4) 0.000(3) -0.001(3) C8 0.029(4) 0.051(5) 0.028(4) 0.005(4) 0.004(3) 0.007(4) C9 0.041(5) 0.051(5) 0.024(4) 0.021(4) 0.009(4) 0.005(4) C10 0.058(6) 0.055(5) 0.024(4) 0.022(4) 0.012(4) 0.007(4) C11 0.051(5) 0.051(5) 0.018(4) 0.009(4) 0.010(4) 0.009(3) C12 0.037(4) 0.041(4) 0.020(4) 0.012(4) 0.002(3) 0.003(3) C13 0.029(4) 0.038(4) 0.016(4) 0.004(3) 0.002(3) -0.000(3) C14 0.034(4) 0.038(4) 0.018(4) 0.005(3) 0.007(3) -0.003(3) C15 0.032(4) 0.048(5) 0.026(4) 0.010(4) 0.009(3) 0.004(3) C16 0.032(4) 0.045(4) 0.020(4) 0.009(3) 0.007(3) 0.006(3) C17 0.042(4) 0.048(5) 0.014(4) 0.016(4) 0.008(3) 0.008(3) C18 0.034(4) 0.039(4) 0.035(4) 0.013(3) 0.016(4) 0.003(3) C19 0.031(4) 0.048(5) 0.019(4) 0.010(4) 0.014(3) 0.001(3) C20 0.027(4) 0.052(5) 0.023(4) 0.009(4) 0.002(3) 0.008(4) C21 0.040(5) 0.040(5) 0.034(5) 0.010(4) 0.012(4) -0.004(4) C22 0.037(4) 0.060(5) 0.011(4) 0.001(4) 0.012(3) 0.005(3) C23 0.036(4) 0.055(5) 0.031(5) 0.007(4) 0.006(4) 0.015(4) C24 0.032(4) 0.043(4) 0.025(4) 0.012(3) 0.011(3) -0.000(3) C25 0.042(5) 0.045(5) 0.024(4) 0.009(4) 0.008(4) -0.003(3) C26 0.067(6) 0.048(5) 0.047(6) 0.024(5) 0.021(5) 0.020(4) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd1 Cl1 2.329(3) yes . . Pd1 Cl1 2.428(3) yes . 2_666 Pd1 Cl2 2.283(3) yes . . Pd1 P1 2.247(3) yes . . P1 C1 1.845(9) yes . . P1 C7 1.848(9) yes . . P1 C13 1.839(7) yes . . O20 C20 1.347(11) yes . . O20 C25 1.448(10) yes . . O24 C24 1.371(10) yes . . O24 C26 1.414(12) yes . . C1 C2 1.551(9) yes . . C1 C6 1.530(11) yes . . C2 C3 1.514(14) yes . . C3 C4 1.533(13) yes . . C4 C5 1.513(10) yes . . C5 C6 1.526(13) yes . . C7 C8 1.536(10) yes . . C7 C12 1.523(9) yes . . C8 C9 1.514(13) yes . . C9 C10 1.537(11) yes . . C10 C11 1.503(12) yes . . C11 C12 1.543(12) yes . . C13 C14 1.403(12) yes . . C13 C18 1.408(11) yes . . C14 C15 1.392(10) yes . . C14 C19 1.502(11) yes . . C15 C16 1.391(11) yes . . C16 C17 1.373(12) yes . . C17 C18 1.368(10) yes . . C19 C20 1.426(11) yes . . C19 C24 1.376(13) yes . . C20 C21 1.387(12) yes . . C21 C22 1.374(13) yes . . C22 C23 1.373(12) yes . . C23 C24 1.395(12) yes . . C1 H1 1.000 no . . C2 H2A 0.990 no . . C2 H2B 0.990 no . . C3 H3A 0.990 no . . C3 H3B 0.990 no . . C4 H4A 0.990 no . . C4 H4B 0.990 no . . C5 H5A 0.990 no . . C5 H5B 0.990 no . . C6 H6A 0.990 no . . C6 H6B 0.990 no . . C7 H7 1.000 no . . C8 H8A 0.990 no . . C8 H8B 0.990 no . . C9 H9A 0.990 no . . C9 H9B 0.990 no . . C10 H10A 0.990 no . . C10 H10B 0.990 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C25 H25A 0.980 no . . C25 H25B 0.980 no . . C25 H25C 0.980 no . . C26 H26A 0.980 no . . C26 H26B 0.980 no . . C26 H26C 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl1 Pd1 Cl1 84.48(11) yes . . 2_666 Cl1 Pd1 Cl2 176.02(8) yes . . . Cl1 Pd1 P1 96.98(11) yes . . . Cl1 Pd1 Cl2 91.65(11) yes 2_666 . . Cl1 Pd1 P1 178.03(8) yes 2_666 . . Cl2 Pd1 P1 86.91(11) yes . . . Pd1 Cl1 Pd1 95.52(11) yes . . 2_666 Pd1 P1 C1 109.4(3) yes . . . Pd1 P1 C7 111.7(3) yes . . . Pd1 P1 C13 111.1(3) yes . . . C1 P1 C7 110.3(4) yes . . . C1 P1 C13 106.8(4) yes . . . C7 P1 C13 107.5(4) yes . . . C20 O20 C25 117.3(6) yes . . . C24 O24 C26 117.8(7) yes . . . P1 C1 C2 113.2(5) yes . . . P1 C1 C6 117.5(6) yes . . . C2 C1 C6 108.1(7) yes . . . C1 C2 C3 109.8(7) yes . . . C2 C3 C4 110.7(8) yes . . . C3 C4 C5 110.3(8) yes . . . C4 C5 C6 112.8(6) yes . . . C1 C6 C5 108.8(7) yes . . . P1 C7 C8 111.2(6) yes . . . P1 C7 C12 116.4(5) yes . . . C8 C7 C12 110.5(7) yes . . . C7 C8 C9 110.1(7) yes . . . C8 C9 C10 109.7(7) yes . . . C9 C10 C11 111.6(8) yes . . . C10 C11 C12 112.1(7) yes . . . C7 C12 C11 108.7(6) yes . . . P1 C13 C14 122.2(6) yes . . . P1 C13 C18 119.5(6) yes . . . C14 C13 C18 118.3(6) yes . . . C13 C14 C15 118.9(7) yes . . . C13 C14 C19 124.5(6) yes . . . C15 C14 C19 116.3(7) yes . . . C14 C15 C16 121.6(8) yes . . . C15 C16 C17 119.2(7) yes . . . C16 C17 C18 120.4(7) yes . . . C13 C18 C17 121.5(8) yes . . . C14 C19 C20 119.1(8) yes . . . C14 C19 C24 122.3(7) yes . . . C20 C19 C24 118.3(8) yes . . . O20 C20 C19 113.7(7) yes . . . O20 C20 C21 125.8(8) yes . . . C19 C20 C21 120.5(8) yes . . . C20 C21 C22 118.9(8) yes . . . C21 C22 C23 121.7(8) yes . . . C22 C23 C24 119.6(9) yes . . . O24 C24 C19 115.3(7) yes . . . O24 C24 C23 124.0(8) yes . . . C19 C24 C23 120.7(8) yes . . . P1 C1 H1 105.715 no . . . C2 C1 H1 105.712 no . . . C6 C1 H1 105.724 no . . . C1 C2 H2A 109.697 no . . . C1 C2 H2B 109.698 no . . . C3 C2 H2A 109.705 no . . . C3 C2 H2B 109.703 no . . . H2A C2 H2B 108.185 no . . . C2 C3 H3A 109.512 no . . . C2 C3 H3B 109.516 no . . . C4 C3 H3A 109.514 no . . . C4 C3 H3B 109.510 no . . . H3A C3 H3B 108.081 no . . . C3 C4 H4A 109.597 no . . . C3 C4 H4B 109.604 no . . . C5 C4 H4A 109.600 no . . . C5 C4 H4B 109.609 no . . . H4A C4 H4B 108.122 no . . . C4 C5 H5A 109.022 no . . . C4 C5 H5B 109.019 no . . . C6 C5 H5A 109.008 no . . . C6 C5 H5B 109.019 no . . . H5A C5 H5B 107.800 no . . . C1 C6 H6A 109.936 no . . . C1 C6 H6B 109.928 no . . . C5 C6 H6A 109.938 no . . . C5 C6 H6B 109.936 no . . . H6A C6 H6B 108.336 no . . . P1 C7 H7 105.987 no . . . C8 C7 H7 105.998 no . . . C12 C7 H7 105.998 no . . . C7 C8 H8A 109.642 no . . . C7 C8 H8B 109.643 no . . . C9 C8 H8A 109.648 no . . . C9 C8 H8B 109.656 no . . . H8A C8 H8B 108.151 no . . . C8 C9 H9A 109.718 no . . . C8 C9 H9B 109.726 no . . . C10 C9 H9A 109.718 no . . . C10 C9 H9B 109.720 no . . . H9A C9 H9B 108.195 no . . . C9 C10 H10A 109.306 no . . . C9 C10 H10B 109.313 no . . . C11 C10 H10A 109.302 no . . . C11 C10 H10B 109.308 no . . . H10A C10 H10B 107.963 no . . . C10 C11 H11A 109.191 no . . . C10 C11 H11B 109.194 no . . . C12 C11 H11A 109.197 no . . . C12 C11 H11B 109.197 no . . . H11A C11 H11B 107.894 no . . . C7 C12 H12A 109.951 no . . . C7 C12 H12B 109.954 no . . . C11 C12 H12A 109.950 no . . . C11 C12 H12B 109.952 no . . . H12A C12 H12B 108.339 no . . . C14 C15 H15 119.221 no . . . C16 C15 H15 119.224 no . . . C15 C16 H16 120.394 no . . . C17 C16 H16 120.389 no . . . C16 C17 H17 119.801 no . . . C18 C17 H17 119.794 no . . . C13 C18 H18 119.245 no . . . C17 C18 H18 119.246 no . . . C20 C21 H21 120.561 no . . . C22 C21 H21 120.550 no . . . C21 C22 H22 119.150 no . . . C23 C22 H22 119.147 no . . . C22 C23 H23 120.179 no . . . C24 C23 H23 120.175 no . . . O20 C25 H25A 109.475 no . . . O20 C25 H25B 109.472 no . . . O20 C25 H25C 109.475 no . . . H25A C25 H25B 109.467 no . . . H25A C25 H25C 109.472 no . . . H25B C25 H25C 109.466 no . . . O24 C26 H26A 109.467 no . . . O24 C26 H26B 109.470 no . . . O24 C26 H26C 109.478 no . . . H26A C26 H26B 109.473 no . . . H26A C26 H26C 109.469 no . . . H26B C26 H26C 109.471 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl1 Pd1 Cl1 Pd1 0.00(8) no . . 2_666 2_666 Cl1 Pd1 Cl1 Pd1 -0.00(8) no 2_666 . . 2_666 Cl1 Pd1 P1 C1 -130.08(11) no . . . . Cl1 Pd1 P1 C7 -7.70(11) no . . . . Cl1 Pd1 P1 C13 112.25(11) no . . . . P1 Pd1 Cl1 Pd1 178.67(7) no . . . 2_666 Cl2 Pd1 Cl1 Pd1 179.08(8) no . . 2_666 2_666 Cl2 Pd1 P1 C1 50.75(11) no . . . . Cl2 Pd1 P1 C7 173.13(11) no . . . . Cl2 Pd1 P1 C13 -66.92(11) no . . . . Pd1 P1 C1 C2 36.4(5) no . . . . Pd1 P1 C1 C6 163.5(3) no . . . . Pd1 P1 C7 C8 -67.7(5) no . . . . Pd1 P1 C7 C12 164.5(4) no . . . . Pd1 P1 C13 C14 -49.1(6) no . . . . Pd1 P1 C13 C18 130.8(5) no . . . . C1 P1 C7 C8 54.2(5) no . . . . C1 P1 C7 C12 -73.6(5) no . . . . C7 P1 C1 C2 -86.8(5) no . . . . C7 P1 C1 C6 40.3(5) no . . . . C1 P1 C13 C14 -168.4(5) no . . . . C1 P1 C13 C18 11.5(6) no . . . . C13 P1 C1 C2 156.7(5) no . . . . C13 P1 C1 C6 -76.2(5) no . . . . C7 P1 C13 C14 73.3(6) no . . . . C7 P1 C13 C18 -106.8(6) no . . . . C13 P1 C7 C8 170.2(4) no . . . . C13 P1 C7 C12 42.5(6) no . . . . C25 O20 C20 C19 -172.5(6) no . . . . C25 O20 C20 C21 8.6(10) no . . . . C26 O24 C24 C19 -170.9(6) no . . . . C26 O24 C24 C23 11.5(10) no . . . . P1 C1 C2 C3 -165.7(5) no . . . . P1 C1 C6 C5 170.0(4) no . . . . C2 C1 C6 C5 -60.4(7) no . . . . C6 C1 C2 C3 62.3(8) no . . . . C1 C2 C3 C4 -59.3(8) no . . . . C2 C3 C4 C5 54.8(9) no . . . . C3 C4 C5 C6 -54.8(10) no . . . . C4 C5 C6 C1 58.4(8) no . . . . P1 C7 C8 C9 168.3(5) no . . . . P1 C7 C12 C11 -173.7(5) no . . . . C8 C7 C12 C11 58.2(8) no . . . . C12 C7 C8 C9 -60.8(8) no . . . . C7 C8 C9 C10 58.1(8) no . . . . C8 C9 C10 C11 -56.0(9) no . . . . C9 C10 C11 C12 55.5(9) no . . . . C10 C11 C12 C7 -56.2(9) no . . . . P1 C13 C14 C15 177.1(5) no . . . . P1 C13 C14 C19 4.0(11) no . . . . P1 C13 C18 C17 -177.5(5) no . . . . C14 C13 C18 C17 2.4(11) no . . . . C18 C13 C14 C15 -2.9(11) no . . . . C18 C13 C14 C19 -175.9(7) no . . . . C13 C14 C15 C16 2.9(12) no . . . . C13 C14 C19 C20 90.3(9) no . . . . C13 C14 C19 C24 -96.3(9) no . . . . C15 C14 C19 C20 -82.9(9) no . . . . C15 C14 C19 C24 90.4(9) no . . . . C19 C14 C15 C16 176.5(7) no . . . . C14 C15 C16 C17 -2.3(12) no . . . . C15 C16 C17 C18 1.8(12) no . . . . C16 C17 C18 C13 -1.9(12) no . . . . C14 C19 C20 O20 -0.0(9) no . . . . C14 C19 C20 C21 179.0(6) no . . . . C14 C19 C24 O24 4.1(10) no . . . . C14 C19 C24 C23 -178.2(6) no . . . . C20 C19 C24 O24 177.5(6) no . . . . C20 C19 C24 C23 -4.8(10) no . . . . C24 C19 C20 O20 -173.6(6) no . . . . C24 C19 C20 C21 5.4(10) no . . . . O20 C20 C21 C22 175.3(6) no . . . . C19 C20 C21 C22 -3.6(11) no . . . . C20 C21 C22 C23 1.3(11) no . . . . C21 C22 C23 C24 -0.7(11) no . . . . C22 C23 C24 O24 -180.0(7) no . . . . C22 C23 C24 C19 2.6(11) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Pd1 O20 3.263(7) no . . Pd1 C2 3.452(10) no . . Pd1 C19 3.395(8) no . . Pd1 C20 3.169(8) no . . Cl1 C7 3.279(8) no . . Cl1 C8 3.345(9) no . . Cl1 C22 3.517(9) no . . Cl1 C23 3.559(9) no . . Cl2 O20 3.321(7) no . . Cl2 C1 3.271(8) no . . Cl2 C2 3.442(10) no . . Cl2 C13 3.583(8) no . . Cl2 C25 3.473(10) no . . P1 C19 3.250(9) no . . O20 C13 3.386(10) no . . O20 C14 2.698(10) no . . O20 C15 3.194(9) no . . O20 C24 3.580(11) no . . O24 C7 3.430(10) no . . O24 C12 3.412(11) no . . O24 C13 3.521(11) no . . O24 C14 2.766(11) no . . O24 C15 3.422(11) no . . C1 C4 2.952(13) no . . C1 C8 3.375(12) no . . C1 C18 3.127(10) no . . C2 C5 2.901(11) no . . C2 C8 3.521(14) no . . C3 C6 2.944(11) no . . C6 C7 3.383(12) no . . C6 C12 3.424(12) no . . C6 C18 3.420(12) no . . C7 C10 2.919(13) no . . C8 C11 2.919(11) no . . C9 C12 2.964(10) no . . C12 C13 3.297(11) no . . C13 C16 2.800(10) no . . C13 C20 3.442(12) no . . C13 C24 3.490(13) no . . C14 C17 2.790(11) no . . C15 C18 2.745(13) no . . C15 C20 3.261(10) no . . C15 C24 3.329(12) no . . C19 C22 2.777(12) no . . C20 C23 2.767(14) no . . C21 C24 2.786(12) no . . C21 C25 2.833(13) no . . C23 C26 2.823(13) no . . Cl2 C5 3.595(9) no . 2_665 C2 C25 3.527(11) no . 1_655 C5 Cl2 3.595(9) no . 2_665 C15 C16 3.288(11) no . 2_555 C15 C17 3.530(11) no . 2_555 C16 C15 3.288(11) no . 2_555 C16 C16 3.177(12) no . 2_555 C17 C15 3.530(11) no . 2_555 C25 C2 3.527(11) no . 1_455 Pd1 H1 3.5814 no . . Pd1 H2A 2.8083 no . . Pd1 H7 3.3573 no . . Pd1 H8B 3.2540 no . . Pd1 H25A 3.2152 no . . Cl1 H7 2.7358 no . . Cl1 H8B 2.7106 no . . Cl1 H9A 3.4242 no . . Cl1 H25A 2.6634 no . 2_666 Cl2 H1 2.8438 no . . Cl2 H2A 2.8000 no . . Cl2 H25A 3.1826 no . . Cl2 H25C 3.3558 no . . P1 H2A 2.8861 no . . P1 H2B 3.1096 no . . P1 H6A 3.1426 no . . P1 H6B 2.9942 no . . P1 H8A 3.0363 no . . P1 H8B 2.8458 no . . P1 H12A 3.0881 no . . P1 H12B 2.9930 no . . P1 H18 2.8842 no . . O20 H15 3.2713 no . . O20 H21 2.6730 no . . O24 H7 2.7472 no . . O24 H11A 3.0716 no . . O24 H12B 2.8457 no . . O24 H15 3.4960 no . . O24 H23 2.6574 no . . C1 H3A 3.3680 no . . C1 H3B 2.7055 no . . C1 H4B 3.3493 no . . C1 H5A 3.3408 no . . C1 H5B 2.6858 no . . C1 H8A 3.0425 no . . C1 H8B 3.4521 no . . C1 H12A 3.3623 no . . C1 H18 2.6214 no . . C2 H4A 3.3565 no . . C2 H4B 2.7491 no . . C2 H5B 3.2656 no . . C2 H6A 2.6798 no . . C2 H6B 3.3615 no . . C2 H8A 3.0930 no . . C2 H8B 3.2711 no . . C2 H22 3.3821 no . 2_666 C3 H1 2.5816 no . . C3 H5A 3.3512 no . . C3 H5B 2.7331 no . . C3 H6A 3.2709 no . . C4 H1 3.1176 no . . C4 H2A 3.3623 no . . C4 H2B 2.7105 no . . C4 H6A 2.7561 no . . C4 H6B 3.3777 no . . C5 H1 2.5624 no . . C5 H2B 3.2083 no . . C5 H3A 3.3506 no . . C5 H3B 2.7407 no . . C5 H18 3.4419 no . . C6 H2A 3.3551 no . . C6 H2B 2.6694 no . . C6 H3B 3.3001 no . . C6 H4A 3.3766 no . . C6 H4B 2.7780 no . . C6 H8A 3.0011 no . . C6 H12A 2.7335 no . . C6 H18 2.6750 no . . C7 H2B 3.5550 no . . C7 H6A 3.1072 no . . C7 H6B 3.4104 no . . C7 H9A 2.7116 no . . C7 H9B 3.3584 no . . C7 H10A 3.2927 no . . C7 H11A 2.7143 no . . C7 H11B 3.3471 no . . C8 H2B 2.9158 no . . C8 H6A 3.0337 no . . C8 H10A 2.7245 no . . C8 H10B 3.3480 no . . C8 H11A 3.2870 no . . C8 H12A 2.7279 no . . C8 H12B 3.3713 no . . C9 H7 2.5994 no . . C9 H11A 2.7462 no . . C9 H11B 3.3636 no . . C9 H12A 3.3176 no . . C10 H7 3.1269 no . . C10 H8A 2.7057 no . . C10 H8B 3.3554 no . . C10 H12A 2.7680 no . . C10 H12B 3.3729 no . . C11 H7 2.5992 no . . C11 H8A 3.2400 no . . C11 H9A 2.7530 no . . C11 H9B 3.3609 no . . C11 H26C 3.4413 no . . C12 H6A 3.0917 no . . C12 H6B 3.1056 no . . C12 H8A 2.7092 no . . C12 H8B 3.3665 no . . C12 H9A 3.3169 no . . C12 H10A 2.7602 no . . C12 H10B 3.3757 no . . C13 H1 2.9145 no . . C13 H6B 3.2568 no . . C13 H7 3.2073 no . . C13 H12A 3.5713 no . . C13 H12B 2.8320 no . . C13 H15 3.2642 no . . C13 H17 3.2768 no . . C14 H7 3.4724 no . . C14 H12B 3.2954 no . . C14 H16 3.2835 no . . C14 H18 3.2710 no . . C15 H17 3.2442 no . . C16 H18 3.2311 no . . C17 H15 3.2380 no . . C18 H1 2.8050 no . . C18 H6B 2.8022 no . . C18 H12B 3.3256 no . . C18 H16 3.2375 no . . C19 H7 3.1993 no . . C19 H15 2.5747 no . . C19 H21 3.3043 no . . C19 H23 3.2627 no . . C20 H15 3.2180 no . . C20 H22 3.2348 no . . C20 H25A 2.6292 no . . C20 H25B 2.6269 no . . C20 H25C 3.1974 no . . C21 H23 3.2532 no . . C21 H25A 2.8235 no . . C21 H25B 2.7221 no . . C22 H2A 3.2932 no . 2_666 C23 H21 3.2553 no . . C23 H26A 2.8246 no . . C23 H26B 2.6899 no . . C24 H7 2.9221 no . . C24 H15 3.2816 no . . C24 H22 3.2477 no . . C24 H26A 2.6216 no . . C24 H26B 2.6209 no . . C24 H26C 3.1989 no . . C25 H21 2.5511 no . . C26 H7 3.5269 no . . C26 H11A 2.9457 no . . C26 H23 2.5348 no . . H1 H2A 2.4153 no . . H1 H2B 2.8663 no . . H1 H3A 3.5009 no . . H1 H3B 2.3965 no . . H1 H5A 3.4780 no . . H1 H5B 2.3785 no . . H1 H6A 2.8534 no . . H1 H6B 2.3862 no . . H1 H18 2.2530 no . . H2A H3A 2.3648 no . . H2A H3B 2.3648 no . . H2A H6A 3.5754 no . . H2A H8A 3.5962 no . . H2A H8B 3.3158 no . . H2A H21 3.2525 no . 2_666 H2A H22 2.6171 no . 2_666 H2B H3A 2.3666 no . . H2B H3B 2.8674 no . . H2B H4B 2.5837 no . . H2B H6A 2.4759 no . . H2B H6B 3.5797 no . . H2B H8A 2.3833 no . . H2B H8B 2.6723 no . . H2B H21 3.3284 no . 2_666 H2B H22 3.4687 no . 2_666 H3A H4A 2.4064 no . . H3A H4B 2.3581 no . . H3A H22 3.3296 no . 2_666 H3B H4A 2.3571 no . . H3B H4B 2.8794 no . . H3B H5B 2.6051 no . . H4A H5A 2.3782 no . . H4A H5B 2.3290 no . . H4B H5A 2.3348 no . . H4B H5B 2.8593 no . . H4B H6A 2.6381 no . . H5A H6A 2.3727 no . . H5A H6B 2.3759 no . . H5B H6A 2.8739 no . . H5B H6B 2.3633 no . . H5B H18 3.1038 no . . H6A H8A 2.2573 no . . H6A H8B 3.5604 no . . H6A H12A 2.3338 no . . H6A H18 3.4924 no . . H6B H8A 3.4941 no . . H6B H12A 2.3943 no . . H6B H12B 3.2475 no . . H6B H18 2.0590 no . . H7 H8A 2.8589 no . . H7 H8B 2.3860 no . . H7 H9A 2.4283 no . . H7 H9B 3.5176 no . . H7 H11A 2.4390 no . . H7 H11B 3.5155 no . . H7 H12A 2.8528 no . . H7 H12B 2.3609 no . . H7 H26B 3.3292 no . . H8A H9A 2.8690 no . . H8A H9B 2.3613 no . . H8A H10A 2.5616 no . . H8A H12A 2.5507 no . . H8B H9A 2.3621 no . . H8B H9B 2.3756 no . . H8B H21 2.9983 no . 2_666 H8B H25A 2.9030 no . 2_666 H8B H25B 3.5409 no . 2_666 H9A H10A 2.8822 no . . H9A H10B 2.3687 no . . H9A H11A 2.6176 no . . H9A H25A 3.4629 no . 2_666 H9B H10A 2.3644 no . . H9B H10B 2.4011 no . . H10A H11A 2.8513 no . . H10A H11B 2.3255 no . . H10A H12A 2.6361 no . . H10B H11A 2.3244 no . . H10B H11B 2.3629 no . . H11A H12A 2.8882 no . . H11A H12B 2.3711 no . . H11A H26B 2.7298 no . . H11A H26C 2.6496 no . . H11B H12A 2.3788 no . . H11B H12B 2.4086 no . . H11B H26C 3.5481 no . . H12B H18 3.5365 no . . H12B H26C 3.3863 no . . H15 H16 2.3352 no . . H16 H17 2.3263 no . . H17 H18 2.3045 no . . H21 H22 2.3201 no . . H21 H25A 2.4249 no . . H21 H25B 2.2618 no . . H21 H25C 3.5211 no . . H22 H23 2.3136 no . . H23 H26A 2.4649 no . . H23 H26B 2.1878 no . . H23 H26C 3.4983 no . . Cl2 H5A 3.2944 no . 2_665 Cl2 H5B 3.0248 no . 2_665 Cl2 H11A 3.2220 no . 1_565 Cl2 H11B 3.3922 no . 1_565 Cl2 H26B 3.5965 no . 1_565 Cl2 H26C 2.9008 no . 1_565 O20 H2B 2.8777 no . 1_455 O20 H3A 3.5354 no . 1_455 O20 H4B 2.9983 no . 1_455 O20 H8A 3.5538 no . 1_455 O24 H16 3.0129 no . 2_555 O24 H17 3.2470 no . 2_555 C1 H5B 3.5422 no . 2_665 C2 H25B 3.1444 no . 1_655 C2 H25C 3.2741 no . 1_655 C3 H17 3.1098 no . 2_665 C3 H18 3.2804 no . 2_665 C3 H25B 3.5930 no . 1_655 C3 H25C 2.9900 no . 1_655 C4 H4A 3.5641 no . 2_765 C4 H17 3.5624 no . 2_665 C4 H25C 3.5220 no . 1_655 C5 H1 3.4980 no . 2_665 C5 H11B 2.9285 no . 2_655 C5 H16 3.2938 no . 1_655 C6 H11B 3.1099 no . 2_655 C6 H12B 3.5574 no . 2_655 C6 H15 3.4077 no . 1_655 C6 H16 3.5715 no . 1_655 C9 H23 3.0803 no . 2_656 C10 H17 3.4685 no . 2_655 C10 H22 3.5522 no . 2_656 C10 H23 3.4274 no . 2_656 C11 H5A 3.2762 no . 2_655 C11 H5B 3.5748 no . 2_655 C11 H6B 3.1948 no . 2_655 C12 H5A 3.5719 no . 2_655 C12 H6B 3.1489 no . 2_655 C14 H16 3.3917 no . 2_555 C15 H4B 3.0823 no . 1_455 C15 H6A 3.0947 no . 1_455 C15 H8A 3.5340 no . 1_455 C15 H16 3.1759 no . 2_555 C16 H4B 3.0973 no . 1_455 C16 H5A 3.0821 no . 1_455 C16 H6A 3.3915 no . 1_455 C16 H15 3.4764 no . 2_555 C16 H16 3.2721 no . 2_555 C17 H3A 3.3079 no . 2_665 C17 H3B 3.2877 no . 2_665 C17 H4A 3.0378 no . 2_665 C17 H10A 3.2793 no . 2_655 C17 H15 3.3358 no . 2_555 C17 H16 3.5919 no . 2_555 C18 H3B 3.0904 no . 2_665 C18 H4A 3.0776 no . 2_665 C20 H8A 3.4225 no . 1_455 C20 H9B 3.5103 no . 1_455 C21 H9B 3.1871 no . 1_455 C21 H21 3.5828 no . 2_566 C21 H25B 2.8698 no . 2_566 C22 H9B 2.8703 no . 1_455 C22 H10B 3.2830 no . 2_656 C22 H25B 3.1460 no . 2_566 C23 H9A 3.4269 no . 2_656 C23 H9B 2.9498 no . 1_455 C23 H10B 3.4091 no . 2_656 C24 H9B 3.3158 no . 1_455 C25 H2B 2.8557 no . 1_455 C25 H3A 3.0052 no . 1_455 C25 H4B 3.5088 no . 1_455 C25 H21 3.1995 no . 2_566 C25 H22 3.4292 no . 2_566 C25 H26A 3.2696 no . 1_565 C25 H26C 3.4784 no . 1_565 C26 H16 3.5746 no . 2_555 C26 H17 3.3479 no . 2_555 C26 H25A 3.5351 no . 1_545 C26 H25C 2.9731 no . 1_545 H1 C5 3.4980 no . 2_665 H1 H3B 3.1761 no . 2_665 H1 H4A 3.5768 no . 2_665 H1 H5B 2.5712 no . 2_665 H2A H10B 3.4566 no . 1_565 H2A H25B 3.1288 no . 1_655 H2A H25C 3.4632 no . 1_655 H2B O20 2.8777 no . 1_655 H2B C25 2.8557 no . 1_655 H2B H25B 2.4667 no . 1_655 H2B H25C 2.8347 no . 1_655 H3A O20 3.5354 no . 1_655 H3A C17 3.3079 no . 2_665 H3A C25 3.0052 no . 1_655 H3A H10B 3.2317 no . 1_565 H3A H17 2.6166 no . 2_665 H3A H18 3.4705 no . 2_665 H3A H25B 3.1012 no . 1_655 H3A H25C 2.2284 no . 1_655 H3A H26A 3.0680 no . 1_665 H3A H26C 3.5278 no . 1_665 H3B C17 3.2877 no . 2_665 H3B C18 3.0904 no . 2_665 H3B H1 3.1761 no . 2_665 H3B H5B 2.8042 no . 2_665 H3B H10B 3.3746 no . 1_565 H3B H11B 2.9510 no . 1_565 H3B H17 2.8804 no . 2_665 H3B H18 2.4945 no . 2_665 H4A C4 3.5641 no . 2_765 H4A C17 3.0378 no . 2_665 H4A C18 3.0776 no . 2_665 H4A H1 3.5768 no . 2_665 H4A H4A 3.0260 no . 2_765 H4A H4B 3.1591 no . 2_765 H4A H17 3.0321 no . 2_665 H4A H18 3.1206 no . 2_665 H4B O20 2.9983 no . 1_655 H4B C15 3.0823 no . 1_655 H4B C16 3.0973 no . 1_655 H4B C25 3.5088 no . 1_655 H4B H4A 3.1591 no . 2_765 H4B H15 3.1941 no . 1_655 H4B H16 3.2536 no . 1_655 H4B H25C 3.0912 no . 1_655 H5A Cl2 3.2944 no . 2_665 H5A C11 3.2762 no . 2_655 H5A C12 3.5719 no . 2_655 H5A C16 3.0821 no . 1_655 H5A H11A 3.2755 no . 2_655 H5A H11B 2.6355 no . 2_655 H5A H12B 3.0270 no . 2_655 H5A H16 2.5337 no . 1_655 H5A H26C 2.9443 no . 2_655 H5B Cl2 3.0248 no . 2_665 H5B C1 3.5422 no . 2_665 H5B C11 3.5748 no . 2_655 H5B H1 2.5712 no . 2_665 H5B H3B 2.8042 no . 2_665 H5B H5B 3.3298 no . 2_665 H5B H11B 2.6551 no . 2_655 H5B H18 3.5945 no . 2_665 H6A C15 3.0947 no . 1_655 H6A C16 3.3915 no . 1_655 H6A H12B 3.5254 no . 2_655 H6A H15 2.4680 no . 1_655 H6A H16 3.0832 no . 1_655 H6B C11 3.1948 no . 2_655 H6B C12 3.1489 no . 2_655 H6B H11B 2.4521 no . 2_655 H6B H12A 2.8145 no . 2_655 H6B H12B 3.0047 no . 2_655 H8A O20 3.5538 no . 1_655 H8A C15 3.5340 no . 1_655 H8A C20 3.4225 no . 1_655 H8A H15 2.6860 no . 1_655 H8B H25B 3.5371 no . 1_655 H9A C23 3.4269 no . 2_656 H9A H23 2.4940 no . 2_656 H9A H26A 3.5022 no . 2_656 H9A H26B 2.8680 no . 2_656 H9B C20 3.5103 no . 1_655 H9B C21 3.1871 no . 1_655 H9B C22 2.8703 no . 1_655 H9B C23 2.9498 no . 1_655 H9B C24 3.3158 no . 1_655 H9B H22 3.1829 no . 1_655 H9B H23 3.3142 no . 1_655 H9B H23 3.0298 no . 2_656 H10A C17 3.2793 no . 2_655 H10A H15 2.8629 no . 1_655 H10A H17 2.6472 no . 2_655 H10A H18 3.3702 no . 2_655 H10A H26A 3.4412 no . 1_655 H10B C22 3.2830 no . 2_656 H10B C23 3.4091 no . 2_656 H10B H2A 3.4566 no . 1_545 H10B H3A 3.2317 no . 1_545 H10B H3B 3.3746 no . 1_545 H10B H17 3.4931 no . 2_655 H10B H22 2.5785 no . 2_656 H10B H23 2.8529 no . 2_656 H10B H26A 3.3763 no . 1_655 H11A Cl2 3.2220 no . 1_545 H11A H5A 3.2755 no . 2_655 H11B Cl2 3.3922 no . 1_545 H11B C5 2.9285 no . 2_655 H11B C6 3.1099 no . 2_655 H11B H3B 2.9510 no . 1_545 H11B H5A 2.6355 no . 2_655 H11B H5B 2.6551 no . 2_655 H11B H6B 2.4521 no . 2_655 H11B H18 2.8959 no . 2_655 H12A H6B 2.8145 no . 2_655 H12A H12A 3.1526 no . 2_655 H12A H15 3.4586 no . 1_655 H12B C6 3.5574 no . 2_655 H12B H5A 3.0270 no . 2_655 H12B H6A 3.5254 no . 2_655 H12B H6B 3.0047 no . 2_655 H12B H16 2.7772 no . 2_555 H15 C6 3.4077 no . 1_455 H15 C16 3.4764 no . 2_555 H15 C17 3.3358 no . 2_555 H15 H4B 3.1941 no . 1_455 H15 H6A 2.4680 no . 1_455 H15 H8A 2.6860 no . 1_455 H15 H10A 2.8629 no . 1_455 H15 H12A 3.4586 no . 1_455 H15 H16 3.5032 no . 2_555 H15 H17 3.2844 no . 2_555 H16 O24 3.0129 no . 2_555 H16 C5 3.2938 no . 1_455 H16 C6 3.5715 no . 1_455 H16 C14 3.3917 no . 2_555 H16 C15 3.1759 no . 2_555 H16 C16 3.2721 no . 2_555 H16 C17 3.5919 no . 2_555 H16 C26 3.5746 no . 2_555 H16 H4B 3.2536 no . 1_455 H16 H5A 2.5337 no . 1_455 H16 H6A 3.0832 no . 1_455 H16 H12B 2.7772 no . 2_555 H16 H15 3.5032 no . 2_555 H16 H26C 3.1881 no . 2_555 H17 O24 3.2470 no . 2_555 H17 C3 3.1098 no . 2_665 H17 C4 3.5624 no . 2_665 H17 C10 3.4685 no . 2_655 H17 C26 3.3479 no . 2_555 H17 H3A 2.6166 no . 2_665 H17 H3B 2.8804 no . 2_665 H17 H4A 3.0321 no . 2_665 H17 H10A 2.6472 no . 2_655 H17 H10B 3.4931 no . 2_655 H17 H15 3.2844 no . 2_555 H17 H26A 3.0610 no . 2_555 H17 H26C 3.2071 no . 2_555 H18 C3 3.2804 no . 2_665 H18 H3A 3.4705 no . 2_665 H18 H3B 2.4945 no . 2_665 H18 H4A 3.1206 no . 2_665 H18 H5B 3.5945 no . 2_665 H18 H10A 3.3702 no . 2_655 H18 H11B 2.8959 no . 2_655 H21 C21 3.5828 no . 2_566 H21 C25 3.1995 no . 2_566 H21 H21 2.8666 no . 2_566 H21 H25A 3.5102 no . 2_566 H21 H25B 2.2380 no . 2_566 H22 C10 3.5522 no . 2_656 H22 C25 3.4292 no . 2_566 H22 H9B 3.1829 no . 1_455 H22 H10B 2.5785 no . 2_656 H22 H25B 2.7713 no . 2_566 H22 H25C 3.2731 no . 2_566 H22 H26A 3.5832 no . 2_556 H23 C9 3.0803 no . 2_656 H23 C10 3.4274 no . 2_656 H23 H9A 2.4940 no . 2_656 H23 H9B 3.3142 no . 1_455 H23 H9B 3.0298 no . 2_656 H23 H10B 2.8529 no . 2_656 H25A C26 3.5351 no . 1_565 H25A H21 3.5102 no . 2_566 H25A H26A 3.2658 no . 1_565 H25A H26B 3.3537 no . 1_565 H25A H26C 3.3989 no . 1_565 H25B C2 3.1444 no . 1_455 H25B C3 3.5930 no . 1_455 H25B C21 2.8698 no . 2_566 H25B C22 3.1460 no . 2_566 H25B H2A 3.1288 no . 1_455 H25B H2B 2.4667 no . 1_455 H25B H3A 3.1012 no . 1_455 H25B H8B 3.5371 no . 1_455 H25B H21 2.2380 no . 2_566 H25B H22 2.7713 no . 2_566 H25B H25B 3.4686 no . 2_566 H25C C2 3.2741 no . 1_455 H25C C3 2.9900 no . 1_455 H25C C4 3.5220 no . 1_455 H25C C26 2.9731 no . 1_565 H25C H2A 3.4632 no . 1_455 H25C H2B 2.8347 no . 1_455 H25C H3A 2.2284 no . 1_455 H25C H4B 3.0912 no . 1_455 H25C H22 3.2731 no . 2_566 H25C H26A 2.4992 no . 1_565 H25C H26B 3.2577 no . 1_565 H25C H26C 2.7227 no . 1_565 H26A C25 3.2696 no . 1_545 H26A H3A 3.0680 no . 1_445 H26A H9A 3.5022 no . 2_656 H26A H10A 3.4412 no . 1_455 H26A H10B 3.3763 no . 1_455 H26A H17 3.0610 no . 2_555 H26A H22 3.5832 no . 2_556 H26A H25A 3.2658 no . 1_545 H26A H25C 2.4992 no . 1_545 H26B Cl2 3.5965 no . 1_545 H26B H9A 2.8680 no . 2_656 H26B H25A 3.3537 no . 1_545 H26B H25C 3.2577 no . 1_545 H26C Cl2 2.9008 no . 1_545 H26C C25 3.4784 no . 1_545 H26C H3A 3.5278 no . 1_445 H26C H5A 2.9443 no . 2_655 H26C H16 3.1881 no . 2_555 H26C H17 3.2071 no . 2_555 H26C H25A 3.3989 no . 1_545 H26C H25C 2.7227 no . 1_545 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================