# 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_09050 _database_code_depnum_ccdc_archive 'CCDC 919243' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: ...Due to the Squeeze option in Platon, reported sum formula does not agree with the calculated sum formula. 'see_platon_squeeze_details' ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C30 H30 N2 O)2(CH3 CH2)O' _chemical_formula_sum 'C34 H40 N2 O2' _chemical_formula_weight 508.68 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' _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 8.9542(16) _cell_length_b 12.028(2) _cell_length_c 14.082(3) _cell_angle_alpha 89.451(3) _cell_angle_beta 85.613(4) _cell_angle_gamma 81.432(4) _cell_volume 1495.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 653 _cell_measurement_theta_min 3.071 _cell_measurement_theta_max 21.739 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9828 _exptl_absorpt_correction_T_max 0.9917 _exptl_absorpt_process_details ; absorption correction based on 2730 reflections(SADABS);Rint 0.1006 before corrrection and 0.0329 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10849 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.1277 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5210 _reflns_number_gt 2537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Disordered diethyl ether was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 373.2 3 with an estimated 106e/cell to be added. Two solvent diethyl ether molecules/unit cell accounting for 84e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0645P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5210 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 341 104 ' ' _platon_squeeze_details ; Disordered diethyl ether was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 345.2 3 with an estimated 104e/cell to be added. Two solvent diethyl ether molecules/unit cell accounting for 84e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. ; 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 O1 O 0.2939(2) 0.29147(14) 0.77823(12) 0.0374(5) Uani 1 1 d . . . H1 H 0.2343 0.3524 0.7784 0.056 Uiso 1 1 calc R . . N1 N 0.1449(2) 0.47546(17) 0.84173(14) 0.0299(5) Uani 1 1 d . . . N2 N -0.1296(2) 0.64953(17) 0.71652(14) 0.0299(5) Uani 1 1 d . . . C1 C 0.5436(3) 0.1319(2) 0.6956(2) 0.0455(8) Uani 1 1 d . . . H1A H 0.5331 0.2088 0.6776 0.055 Uiso 1 1 calc R . . C2 C 0.5831(3) 0.0491(3) 0.6260(2) 0.0551(9) Uani 1 1 d . . . H2 H 0.5975 0.0699 0.5611 0.066 Uiso 1 1 calc R . . C3 C 0.6015(3) -0.0627(3) 0.6508(2) 0.0563(9) Uani 1 1 d . . . H3 H 0.6304 -0.1192 0.6035 0.068 Uiso 1 1 calc R . . C4 C 0.5774(3) -0.0917(3) 0.7451(2) 0.0532(9) Uani 1 1 d . . . H4 H 0.5890 -0.1687 0.7630 0.064 Uiso 1 1 calc R . . C5 C 0.5363(3) -0.0088(2) 0.8140(2) 0.0427(7) Uani 1 1 d . . . H5 H 0.5195 -0.0299 0.8787 0.051 Uiso 1 1 calc R . . C6 C 0.5193(3) 0.1042(2) 0.7902(2) 0.0350(7) Uani 1 1 d . . . C7 C 0.4819(3) 0.1911(2) 0.86644(18) 0.0339(7) Uani 1 1 d . . . C8 C 0.5583(3) 0.1809(2) 0.94885(19) 0.0391(7) Uani 1 1 d . . . H8 H 0.6346 0.1181 0.9558 0.047 Uiso 1 1 calc R . . C9 C 0.5267(3) 0.2594(2) 1.0208(2) 0.0445(8) Uani 1 1 d . . . H9 H 0.5809 0.2503 1.0765 0.053 Uiso 1 1 calc R . . C10 C 0.4172(3) 0.3505(2) 1.01227(19) 0.0398(7) Uani 1 1 d . . . H10 H 0.3961 0.4042 1.0624 0.048 Uiso 1 1 calc R . . C11 C 0.3352(3) 0.3662(2) 0.93061(17) 0.0299(6) Uani 1 1 d . . . C12 C 0.3689(3) 0.2843(2) 0.85807(18) 0.0303(6) Uani 1 1 d . . . C13 C 0.2198(3) 0.4671(2) 0.92212(17) 0.0303(6) Uani 1 1 d . . . C14 C 0.1910(3) 0.5535(2) 0.98928(18) 0.0378(7) Uani 1 1 d . . . H14 H 0.2442 0.5482 1.0454 0.045 Uiso 1 1 calc R . . C15 C 0.0864(3) 0.6459(2) 0.97470(19) 0.0433(7) Uani 1 1 d . . . H15 H 0.0661 0.7045 1.0208 0.052 Uiso 1 1 calc R . . C16 C 0.0098(3) 0.6537(2) 0.89193(18) 0.0368(7) Uani 1 1 d . . . H16 H -0.0635 0.7171 0.8805 0.044 Uiso 1 1 calc R . . C17 C 0.0431(3) 0.5671(2) 0.82727(17) 0.0283(6) Uani 1 1 d . . . C18 C -0.0284(3) 0.5702(2) 0.73715(17) 0.0307(6) Uani 1 1 d . . . H18 H 0.0022 0.5107 0.6927 0.037 Uiso 1 1 calc R . . C19 C -0.1936(3) 0.6480(2) 0.62674(17) 0.0276(6) Uani 1 1 d . . . C20 C -0.1175(3) 0.6816(2) 0.54307(18) 0.0336(7) Uani 1 1 d . . . C21 C -0.1900(3) 0.6810(2) 0.45948(19) 0.0403(7) Uani 1 1 d . . . H21 H -0.1411 0.7038 0.4019 0.048 Uiso 1 1 calc R . . C22 C -0.3298(3) 0.6486(2) 0.45762(19) 0.0401(7) Uani 1 1 d . . . H22 H -0.3745 0.6458 0.3988 0.048 Uiso 1 1 calc R . . C23 C -0.4057(3) 0.6200(2) 0.54099(19) 0.0377(7) Uani 1 1 d . . . H23 H -0.5041 0.5999 0.5393 0.045 Uiso 1 1 calc R . . C24 C -0.3404(3) 0.6201(2) 0.62768(18) 0.0306(6) Uani 1 1 d . . . C25 C -0.4221(3) 0.5898(2) 0.71993(18) 0.0362(7) Uani 1 1 d . . . H25 H -0.3838 0.6314 0.7719 0.043 Uiso 1 1 calc R . . C26 C -0.5938(3) 0.6269(3) 0.7227(2) 0.0542(9) Uani 1 1 d . . . H26A H -0.6147 0.7059 0.7037 0.081 Uiso 1 1 calc R . . H26B H -0.6389 0.6180 0.7875 0.081 Uiso 1 1 calc R . . H26C H -0.6377 0.5803 0.6787 0.081 Uiso 1 1 calc R . . C27 C -0.3842(3) 0.4646(2) 0.7417(2) 0.0478(8) Uani 1 1 d . . . H27A H -0.4204 0.4208 0.6922 0.072 Uiso 1 1 calc R . . H27B H -0.4336 0.4484 0.8037 0.072 Uiso 1 1 calc R . . H27C H -0.2742 0.4442 0.7430 0.072 Uiso 1 1 calc R . . C28 C 0.0325(3) 0.7259(2) 0.54459(19) 0.0391(7) Uani 1 1 d . . . H28 H 0.0681 0.7155 0.6101 0.047 Uiso 1 1 calc R . . C29 C 0.1525(3) 0.6636(3) 0.4747(2) 0.0599(9) Uani 1 1 d . . . H29A H 0.1686 0.5835 0.4910 0.090 Uiso 1 1 calc R . . H29B H 0.2476 0.6942 0.4778 0.090 Uiso 1 1 calc R . . H29C H 0.1191 0.6728 0.4100 0.090 Uiso 1 1 calc R . . C30 C 0.0106(4) 0.8518(3) 0.5214(3) 0.0681(10) Uani 1 1 d . . . H30A H -0.0271 0.8636 0.4580 0.102 Uiso 1 1 calc R . . H30B H 0.1076 0.8800 0.5225 0.102 Uiso 1 1 calc R . . H30C H -0.0628 0.8923 0.5689 0.102 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 O1 0.0413(12) 0.0379(12) 0.0325(11) 0.0003(9) -0.0117(9) 0.0009(9) N1 0.0284(12) 0.0369(14) 0.0260(13) 0.0034(10) -0.0021(10) -0.0096(10) N2 0.0291(12) 0.0342(13) 0.0267(13) 0.0009(10) -0.0039(10) -0.0054(10) C1 0.054(2) 0.0340(17) 0.0447(19) 0.0051(15) 0.0013(15) 0.0015(14) C2 0.058(2) 0.054(2) 0.049(2) -0.0049(17) 0.0042(16) 0.0016(17) C3 0.060(2) 0.042(2) 0.064(2) -0.0135(17) -0.0053(18) 0.0030(16) C4 0.055(2) 0.0336(18) 0.072(2) 0.0056(17) -0.0117(18) -0.0059(15) C5 0.0440(18) 0.0359(17) 0.0489(19) 0.0031(15) -0.0081(14) -0.0062(14) C6 0.0336(16) 0.0324(16) 0.0393(17) 0.0049(13) -0.0067(13) -0.0040(13) C7 0.0323(16) 0.0364(16) 0.0342(17) 0.0066(13) -0.0003(13) -0.0102(13) C8 0.0392(17) 0.0333(17) 0.0457(19) 0.0078(14) -0.0129(14) -0.0038(13) C9 0.0523(19) 0.0436(19) 0.0395(18) 0.0078(15) -0.0189(15) -0.0059(16) C10 0.0474(18) 0.0406(18) 0.0323(17) 0.0004(13) -0.0069(14) -0.0074(15) C11 0.0322(15) 0.0353(16) 0.0234(15) 0.0047(12) -0.0020(12) -0.0087(13) C12 0.0289(15) 0.0330(16) 0.0303(16) 0.0095(12) -0.0045(12) -0.0083(12) C13 0.0281(15) 0.0389(16) 0.0247(15) 0.0030(12) -0.0009(12) -0.0084(13) C14 0.0350(16) 0.0485(19) 0.0295(16) -0.0019(14) -0.0070(13) -0.0026(14) C15 0.0467(19) 0.0486(19) 0.0331(17) -0.0131(14) -0.0028(14) -0.0018(15) C16 0.0328(16) 0.0440(18) 0.0316(16) -0.0006(14) 0.0014(13) -0.0011(13) C17 0.0276(15) 0.0326(15) 0.0246(15) 0.0006(12) 0.0010(12) -0.0058(12) C18 0.0299(15) 0.0344(16) 0.0278(15) -0.0010(12) 0.0007(12) -0.0067(13) C19 0.0292(15) 0.0258(14) 0.0271(15) 0.0015(11) -0.0046(12) -0.0011(12) C20 0.0330(16) 0.0370(16) 0.0307(16) 0.0022(13) -0.0021(13) -0.0053(13) C21 0.0440(18) 0.0458(18) 0.0313(17) 0.0079(14) -0.0073(14) -0.0057(15) C22 0.0445(19) 0.0438(18) 0.0329(17) 0.0004(13) -0.0141(14) -0.0038(15) C23 0.0322(16) 0.0402(17) 0.0415(18) -0.0002(14) -0.0091(14) -0.0047(13) C24 0.0304(15) 0.0303(15) 0.0309(16) -0.0017(12) -0.0018(12) -0.0044(12) C25 0.0346(16) 0.0417(17) 0.0340(17) -0.0054(13) 0.0020(13) -0.0133(13) C26 0.0388(18) 0.072(2) 0.054(2) -0.0172(17) 0.0079(15) -0.0176(17) C27 0.054(2) 0.052(2) 0.0406(18) 0.0019(15) 0.0046(15) -0.0234(16) C28 0.0344(16) 0.0483(19) 0.0348(17) 0.0071(14) 0.0017(13) -0.0092(14) C29 0.0405(19) 0.061(2) 0.077(3) -0.0121(19) 0.0052(17) -0.0091(16) C30 0.058(2) 0.055(2) 0.093(3) -0.0037(19) 0.0085(19) -0.0204(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 O1 C12 1.348(3) . ? O1 H1 0.8400 . ? N1 C17 1.346(3) . ? N1 C13 1.355(3) . ? N2 C18 1.262(3) . ? N2 C19 1.429(3) . ? C1 C6 1.379(4) . ? C1 C2 1.392(4) . ? C1 H1A 0.9500 . ? C2 C3 1.375(4) . ? C2 H2 0.9500 . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 C7 1.489(4) . ? C7 C8 1.387(3) . ? C7 C12 1.404(3) . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 C10 1.369(4) . ? C9 H9 0.9500 . ? C10 C11 1.407(3) . ? C10 H10 0.9500 . ? C11 C12 1.410(3) . ? C11 C13 1.482(3) . ? C13 C14 1.394(3) . ? C14 C15 1.367(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 C17 1.374(3) . ? C16 H16 0.9500 . ? C17 C18 1.462(3) . ? C18 H18 0.9500 . ? C19 C20 1.402(3) . ? C19 C24 1.404(3) . ? C20 C21 1.388(3) . ? C20 C28 1.518(3) . ? C21 C22 1.368(4) . ? C21 H21 0.9500 . ? C22 C23 1.378(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(3) . ? C23 H23 0.9500 . ? C24 C25 1.510(3) . ? C25 C27 1.527(4) . ? C25 C26 1.534(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.516(4) . ? C28 C30 1.533(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 C12 O1 H1 109.5 . . ? C17 N1 C13 119.8(2) . . ? C18 N2 C19 119.2(2) . . ? C6 C1 C2 121.2(3) . . ? C6 C1 H1A 119.4 . . ? C2 C1 H1A 119.4 . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C1 C6 C5 117.9(3) . . ? C1 C6 C7 122.3(2) . . ? C5 C6 C7 119.8(2) . . ? C8 C7 C12 118.1(3) . . ? C8 C7 C6 120.2(2) . . ? C12 C7 C6 121.8(2) . . ? C9 C8 C7 121.8(3) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 117.8(2) . . ? C10 C11 C13 120.1(2) . . ? C12 C11 C13 122.1(2) . . ? O1 C12 C7 117.2(2) . . ? O1 C12 C11 121.7(2) . . ? C7 C12 C11 121.1(2) . . ? N1 C13 C14 119.7(2) . . ? N1 C13 C11 116.5(2) . . ? C14 C13 C11 123.7(2) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 118.1(3) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? N1 C17 C16 122.5(2) . . ? N1 C17 C18 115.9(2) . . ? C16 C17 C18 121.6(2) . . ? N2 C18 C17 122.0(2) . . ? N2 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C20 C19 C24 121.8(2) . . ? C20 C19 N2 121.1(2) . . ? C24 C19 N2 116.9(2) . . ? C21 C20 C19 117.4(2) . . ? C21 C20 C28 120.9(2) . . ? C19 C20 C28 121.6(2) . . ? C22 C21 C20 121.9(3) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 117.7(2) . . ? C23 C24 C25 121.9(2) . . ? C19 C24 C25 120.4(2) . . ? C24 C25 C27 111.4(2) . . ? C24 C25 C26 112.8(2) . . ? C27 C25 C26 111.2(2) . . ? C24 C25 H25 107.0 . . ? C27 C25 H25 107.0 . . ? C26 C25 H25 107.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C20 111.8(2) . . ? C29 C28 C30 109.7(2) . . ? C20 C28 C30 109.8(2) . . ? C29 C28 H28 108.5 . . ? C20 C28 H28 108.5 . . ? C30 C28 H28 108.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 C6 C1 C2 C3 -1.1(5) . . . . ? C1 C2 C3 C4 1.2(5) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? C2 C1 C6 C7 177.9(3) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C4 C5 C6 C7 -177.3(3) . . . . ? C1 C6 C7 C8 -132.3(3) . . . . ? C5 C6 C7 C8 45.3(4) . . . . ? C1 C6 C7 C12 48.3(4) . . . . ? C5 C6 C7 C12 -134.1(3) . . . . ? C12 C7 C8 C9 -0.4(4) . . . . ? C6 C7 C8 C9 -179.9(3) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C9 C10 C11 C13 -178.5(2) . . . . ? C8 C7 C12 O1 -178.8(2) . . . . ? C6 C7 C12 O1 0.7(4) . . . . ? C8 C7 C12 C11 0.8(4) . . . . ? C6 C7 C12 C11 -179.7(2) . . . . ? C10 C11 C12 O1 178.7(2) . . . . ? C13 C11 C12 O1 -2.3(4) . . . . ? C10 C11 C12 C7 -0.8(4) . . . . ? C13 C11 C12 C7 178.1(2) . . . . ? C17 N1 C13 C14 -0.1(3) . . . . ? C17 N1 C13 C11 -177.2(2) . . . . ? C10 C11 C13 N1 -179.5(2) . . . . ? C12 C11 C13 N1 1.6(3) . . . . ? C10 C11 C13 C14 3.5(4) . . . . ? C12 C11 C13 C14 -175.4(2) . . . . ? N1 C13 C14 C15 0.7(4) . . . . ? C11 C13 C14 C15 177.6(2) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C13 N1 C17 C16 -0.7(4) . . . . ? C13 N1 C17 C18 178.1(2) . . . . ? C15 C16 C17 N1 0.8(4) . . . . ? C15 C16 C17 C18 -178.0(2) . . . . ? C19 N2 C18 C17 179.3(2) . . . . ? N1 C17 C18 N2 177.4(2) . . . . ? C16 C17 C18 N2 -3.7(4) . . . . ? C18 N2 C19 C20 -79.6(3) . . . . ? C18 N2 C19 C24 105.3(3) . . . . ? C24 C19 C20 C21 -3.1(4) . . . . ? N2 C19 C20 C21 -178.0(2) . . . . ? C24 C19 C20 C28 172.1(2) . . . . ? N2 C19 C20 C28 -2.8(4) . . . . ? C19 C20 C21 C22 -0.3(4) . . . . ? C28 C20 C21 C22 -175.6(2) . . . . ? C20 C21 C22 C23 2.9(4) . . . . ? C21 C22 C23 C24 -2.0(4) . . . . ? C22 C23 C24 C19 -1.3(4) . . . . ? C22 C23 C24 C25 179.6(2) . . . . ? C20 C19 C24 C23 3.9(4) . . . . ? N2 C19 C24 C23 179.0(2) . . . . ? C20 C19 C24 C25 -177.0(2) . . . . ? N2 C19 C24 C25 -1.9(3) . . . . ? C23 C24 C25 C27 92.0(3) . . . . ? C19 C24 C25 C27 -87.1(3) . . . . ? C23 C24 C25 C26 -34.0(3) . . . . ? C19 C24 C25 C26 146.9(2) . . . . ? C21 C20 C28 C29 -57.6(3) . . . . ? C19 C20 C28 C29 127.4(3) . . . . ? C21 C20 C28 C30 64.4(3) . . . . ? C19 C20 C28 C30 -110.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.84 1.79 2.540(3) 148.4 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.291 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.061 data_09056 _database_code_depnum_ccdc_archive 'CCDC 919244' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 N2 O' _chemical_formula_sum 'C31 H34 N2 O' _chemical_formula_weight 450.60 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' _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 9.6467(12) _cell_length_b 24.689(3) _cell_length_c 11.3413(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.409(3) _cell_angle_gamma 90.00 _cell_volume 2531.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 708 _cell_measurement_theta_min 2.253 _cell_measurement_theta_max 23.377 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9852 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details ; absorption correction based on 2097 reflections(SADABS);Rint 0.1394 before correction and 0.0535 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18269 _diffrn_reflns_av_R_equivalents 0.1632 _diffrn_reflns_av_sigmaI/netI 0.1699 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4462 _reflns_number_gt 1873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0363P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4462 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.1722(3) 0.06800(9) 0.0471(2) 0.0442(7) Uani 1 1 d . . . H1 H 0.1490 0.0915 0.0905 0.066 Uiso 1 1 calc R . . N1 N 0.1435(3) 0.11186(11) 0.2402(3) 0.0345(7) Uani 1 1 d . . . N2 N 0.0633(3) 0.22521(11) 0.1294(2) 0.0377(8) Uani 1 1 d . . . H2 H 0.1069 0.1985 0.0856 0.045 Uiso 1 1 d R . . C1 C 0.2433(4) 0.02609(14) 0.1227(3) 0.0341(9) Uani 1 1 d . . . C2 C 0.2843(4) -0.01735(13) 0.0629(3) 0.0340(9) Uani 1 1 d . . . C3 C 0.3562(4) -0.06017(14) 0.1379(3) 0.0405(10) Uani 1 1 d . . . H3 H 0.3834 -0.0906 0.0996 0.049 Uiso 1 1 calc R . . C4 C 0.3901(4) -0.06026(15) 0.2673(3) 0.0425(10) Uani 1 1 d . . . H4 H 0.4408 -0.0900 0.3168 0.051 Uiso 1 1 calc R . . C5 C 0.3491(4) -0.01657(14) 0.3228(3) 0.0400(10) Uani 1 1 d . . . H5 H 0.3715 -0.0167 0.4113 0.048 Uiso 1 1 calc R . . C6 C 0.2758(4) 0.02799(13) 0.2533(3) 0.0335(9) Uani 1 1 d . . . C7 C 0.2329(4) 0.07388(14) 0.3157(3) 0.0365(9) Uani 1 1 d . . . C8 C 0.2758(4) 0.07942(14) 0.4460(3) 0.0438(10) Uani 1 1 d . . . H8 H 0.3397 0.0534 0.4997 0.053 Uiso 1 1 calc R . . C9 C 0.2261(4) 0.12226(16) 0.4967(3) 0.0524(11) Uani 1 1 d . . . H9 H 0.2556 0.1262 0.5854 0.063 Uiso 1 1 calc R . . C10 C 0.1321(4) 0.15979(15) 0.4172(3) 0.0443(10) Uani 1 1 d . . . H10 H 0.0954 0.1896 0.4505 0.053 Uiso 1 1 calc R . . C11 C 0.0932(4) 0.15305(14) 0.2895(3) 0.0342(9) Uani 1 1 d . . . C12 C -0.0116(4) 0.19140(13) 0.1972(3) 0.0362(9) Uani 1 1 d . . . H12 H -0.0523 0.2164 0.2464 0.043 Uiso 1 1 calc R . . C13 C 0.1525(4) 0.26793(14) 0.2013(3) 0.0352(9) Uani 1 1 d . . . C14 C 0.0800(4) 0.31296(14) 0.2282(3) 0.0379(9) Uani 1 1 d . . . C15 C 0.1622(4) 0.35456(15) 0.2996(3) 0.0447(10) Uani 1 1 d . . . H15 H 0.1133 0.3846 0.3201 0.054 Uiso 1 1 calc R . . C16 C 0.3155(5) 0.35339(16) 0.3420(3) 0.0508(11) Uani 1 1 d . . . H16 H 0.3713 0.3824 0.3907 0.061 Uiso 1 1 calc R . . C17 C 0.3862(4) 0.30953(15) 0.3126(3) 0.0451(10) Uani 1 1 d . . . H17 H 0.4911 0.3095 0.3389 0.054 Uiso 1 1 calc R . . C18 C 0.3082(4) 0.26550(14) 0.2457(3) 0.0377(9) Uani 1 1 d . . . C19 C -0.0884(4) 0.31864(14) 0.1757(3) 0.0407(10) Uani 1 1 d . . . H19 H -0.1304 0.2856 0.1248 0.049 Uiso 1 1 calc R . . C20 C -0.1506(4) 0.32220(14) 0.2821(3) 0.0533(11) Uani 1 1 d . . . H20A H -0.1164 0.2911 0.3383 0.080 Uiso 1 1 calc R . . H20B H -0.2589 0.3221 0.2467 0.080 Uiso 1 1 calc R . . H20C H -0.1165 0.3557 0.3295 0.080 Uiso 1 1 calc R . . C21 C -0.1360(4) 0.36801(14) 0.0895(3) 0.0527(11) Uani 1 1 d . . . H21A H -0.0997 0.4011 0.1384 0.079 Uiso 1 1 calc R . . H21B H -0.2442 0.3692 0.0527 0.079 Uiso 1 1 calc R . . H21C H -0.0946 0.3654 0.0221 0.079 Uiso 1 1 calc R . . C22 C 0.3928(4) 0.21858(15) 0.2180(3) 0.0477(10) Uani 1 1 d . . . H22 H 0.3210 0.1885 0.1828 0.057 Uiso 1 1 calc R . . C23 C 0.5126(5) 0.19740(18) 0.3351(4) 0.0843(16) Uani 1 1 d . . . H23A H 0.5887 0.2252 0.3682 0.126 Uiso 1 1 calc R . . H23B H 0.5573 0.1649 0.3140 0.126 Uiso 1 1 calc R . . H23C H 0.4691 0.1884 0.3989 0.126 Uiso 1 1 calc R . . C24 C 0.4591(5) 0.23377(17) 0.1196(4) 0.0774(14) Uani 1 1 d . . . H24A H 0.3803 0.2457 0.0428 0.116 Uiso 1 1 calc R . . H24B H 0.5094 0.2022 0.1007 0.116 Uiso 1 1 calc R . . H24C H 0.5304 0.2632 0.1516 0.116 Uiso 1 1 calc R . . C25 C 0.2544(4) -0.01924(13) -0.0748(3) 0.0349(9) Uani 1 1 d . . . C26 C 0.1183(4) -0.00507(13) -0.1627(3) 0.0400(10) Uani 1 1 d . . . H26 H 0.0425 0.0083 -0.1350 0.048 Uiso 1 1 calc R . . C27 C 0.0918(4) -0.01025(14) -0.2900(3) 0.0435(10) Uani 1 1 d . . . H27 H -0.0022 -0.0006 -0.3489 0.052 Uiso 1 1 calc R . . C28 C 0.2004(4) -0.02924(14) -0.3324(4) 0.0494(11) Uani 1 1 d . . . H28 H 0.1818 -0.0328 -0.4200 0.059 Uiso 1 1 calc R . . C29 C 0.3366(4) -0.04308(14) -0.2458(4) 0.0469(10) Uani 1 1 d . . . H29 H 0.4127 -0.0559 -0.2739 0.056 Uiso 1 1 calc R . . C30 C 0.3629(4) -0.03836(13) -0.1173(3) 0.0423(10) Uani 1 1 d . . . H30 H 0.4565 -0.0484 -0.0584 0.051 Uiso 1 1 calc R . . C31 C -0.1416(4) 0.16174(14) 0.1034(3) 0.0483(11) Uani 1 1 d . . . H31A H -0.2107 0.1881 0.0492 0.073 Uiso 1 1 calc R . . H31B H -0.1924 0.1404 0.1489 0.073 Uiso 1 1 calc R . . H31C H -0.1056 0.1376 0.0518 0.073 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 O1 0.0603(18) 0.0358(15) 0.0344(15) 0.0010(13) 0.0138(13) 0.0095(14) N1 0.0395(19) 0.0304(17) 0.0332(18) -0.0008(15) 0.0122(15) -0.0018(15) N2 0.048(2) 0.0320(17) 0.0324(18) -0.0052(15) 0.0134(15) -0.0038(16) C1 0.030(2) 0.033(2) 0.035(2) 0.0061(19) 0.0069(18) 0.0002(18) C2 0.032(2) 0.032(2) 0.035(2) -0.0014(19) 0.0074(18) -0.0022(18) C3 0.036(2) 0.035(2) 0.046(3) -0.004(2) 0.0093(19) -0.0018(19) C4 0.038(2) 0.040(2) 0.042(3) 0.002(2) 0.005(2) -0.001(2) C5 0.039(2) 0.044(2) 0.032(2) 0.002(2) 0.0073(19) -0.006(2) C6 0.034(2) 0.031(2) 0.032(2) 0.0040(18) 0.0063(18) -0.0029(18) C7 0.038(2) 0.036(2) 0.031(2) -0.0012(19) 0.0080(18) -0.0079(19) C8 0.046(3) 0.046(2) 0.033(2) 0.002(2) 0.006(2) 0.002(2) C9 0.062(3) 0.060(3) 0.032(2) -0.006(2) 0.013(2) 0.003(2) C10 0.051(3) 0.047(2) 0.035(2) -0.006(2) 0.016(2) -0.001(2) C11 0.036(2) 0.033(2) 0.035(2) -0.0055(18) 0.0136(19) -0.0081(18) C12 0.042(2) 0.031(2) 0.035(2) -0.0044(18) 0.0121(19) -0.0057(19) C13 0.043(2) 0.037(2) 0.023(2) -0.0035(18) 0.0095(18) -0.007(2) C14 0.049(3) 0.032(2) 0.033(2) -0.0024(18) 0.0143(19) -0.005(2) C15 0.052(3) 0.042(2) 0.036(2) -0.005(2) 0.010(2) -0.001(2) C16 0.061(3) 0.047(3) 0.040(3) -0.002(2) 0.011(2) -0.019(2) C17 0.041(3) 0.054(3) 0.039(2) 0.000(2) 0.012(2) -0.007(2) C18 0.044(3) 0.038(2) 0.029(2) 0.0021(19) 0.0107(19) -0.003(2) C19 0.042(2) 0.039(2) 0.040(2) 0.0001(19) 0.013(2) 0.001(2) C20 0.060(3) 0.050(3) 0.058(3) 0.000(2) 0.031(2) 0.008(2) C21 0.055(3) 0.053(3) 0.050(3) 0.002(2) 0.018(2) 0.009(2) C22 0.044(3) 0.053(3) 0.048(3) -0.004(2) 0.019(2) -0.003(2) C23 0.095(4) 0.098(4) 0.059(3) 0.011(3) 0.026(3) 0.053(3) C24 0.093(4) 0.090(4) 0.067(3) -0.005(3) 0.050(3) 0.008(3) C25 0.036(2) 0.028(2) 0.038(2) -0.0046(18) 0.0105(19) -0.0023(18) C26 0.038(2) 0.042(2) 0.036(2) -0.0025(19) 0.0077(19) 0.0003(19) C27 0.044(3) 0.041(2) 0.040(2) -0.006(2) 0.008(2) -0.001(2) C28 0.060(3) 0.045(3) 0.041(3) -0.005(2) 0.016(2) -0.006(2) C29 0.048(3) 0.049(3) 0.051(3) -0.013(2) 0.027(2) -0.008(2) C30 0.040(2) 0.039(2) 0.045(3) -0.009(2) 0.011(2) -0.0026(19) C31 0.043(2) 0.048(2) 0.049(3) -0.001(2) 0.011(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 O1 C1 1.366(3) . ? O1 H1 0.8400 . ? N1 C11 1.331(4) . ? N1 C7 1.357(4) . ? N2 C13 1.425(4) . ? N2 C12 1.482(4) . ? N2 H2 1.0024 . ? C1 C2 1.398(4) . ? C1 C6 1.404(4) . ? C2 C3 1.383(4) . ? C2 C25 1.486(5) . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C7 1.470(4) . ? C7 C8 1.396(4) . ? C8 C9 1.368(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 C11 1.374(4) . ? C10 H10 0.9500 . ? C11 C12 1.509(4) . ? C12 C31 1.520(4) . ? C12 H12 1.0000 . ? C13 C14 1.403(4) . ? C13 C18 1.409(4) . ? C14 C15 1.375(4) . ? C14 C19 1.529(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C22 1.512(5) . ? C19 C20 1.526(4) . ? C19 C21 1.529(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.513(5) . ? C22 C23 1.518(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.380(4) . ? C25 C26 1.388(4) . ? C26 C27 1.381(4) . ? C26 H26 0.9500 . ? C27 C28 1.378(5) . ? C27 H27 0.9500 . ? C28 C29 1.382(4) . ? C28 H28 0.9500 . ? C29 C30 1.394(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 O1 H1 109.5 . . ? C11 N1 C7 120.5(3) . . ? C13 N2 C12 115.2(3) . . ? C13 N2 H2 119.8 . . ? C12 N2 H2 104.6 . . ? O1 C1 C2 116.2(3) . . ? O1 C1 C6 121.0(3) . . ? C2 C1 C6 122.7(3) . . ? C3 C2 C1 117.0(3) . . ? C3 C2 C25 119.6(3) . . ? C1 C2 C25 123.4(3) . . ? C2 C3 C4 122.3(3) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 116.9(3) . . ? C5 C6 C7 120.6(3) . . ? C1 C6 C7 122.5(3) . . ? N1 C7 C8 119.3(3) . . ? N1 C7 C6 116.9(3) . . ? C8 C7 C6 123.8(3) . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 118.7(4) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? N1 C11 C10 122.0(3) . . ? N1 C11 C12 116.2(3) . . ? C10 C11 C12 121.7(3) . . ? N2 C12 C11 112.5(3) . . ? N2 C12 C31 109.9(3) . . ? C11 C12 C31 111.9(3) . . ? N2 C12 H12 107.4 . . ? C11 C12 H12 107.4 . . ? C31 C12 H12 107.4 . . ? C14 C13 C18 120.4(3) . . ? C14 C13 N2 117.6(3) . . ? C18 C13 N2 121.9(3) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 C19 118.5(3) . . ? C13 C14 C19 122.1(3) . . ? C14 C15 C16 121.0(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 121.8(4) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 117.9(3) . . ? C17 C18 C22 119.0(3) . . ? C13 C18 C22 123.0(3) . . ? C20 C19 C21 110.3(3) . . ? C20 C19 C14 110.7(3) . . ? C21 C19 C14 111.3(3) . . ? C20 C19 H19 108.1 . . ? C21 C19 H19 108.1 . . ? C14 C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 111.1(3) . . ? C18 C22 C23 112.5(3) . . ? C24 C22 C23 110.0(3) . . ? C18 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 118.5(3) . . ? C30 C25 C2 119.0(3) . . ? C26 C25 C2 122.4(3) . . ? C27 C26 C25 120.8(4) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.6(4) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 120.2(4) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.7(4) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C12 C31 H31A 109.5 . . ? C12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 O1 C1 C2 C3 -179.9(3) . . . . ? C6 C1 C2 C3 1.7(5) . . . . ? O1 C1 C2 C25 0.1(5) . . . . ? C6 C1 C2 C25 -178.2(3) . . . . ? C1 C2 C3 C4 -1.4(5) . . . . ? C25 C2 C3 C4 178.6(3) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C4 C5 C6 C1 0.9(5) . . . . ? C4 C5 C6 C7 179.6(3) . . . . ? O1 C1 C6 C5 -179.7(3) . . . . ? C2 C1 C6 C5 -1.5(5) . . . . ? O1 C1 C6 C7 1.5(5) . . . . ? C2 C1 C6 C7 179.8(3) . . . . ? C11 N1 C7 C8 -2.2(5) . . . . ? C11 N1 C7 C6 176.3(3) . . . . ? C5 C6 C7 N1 -170.6(3) . . . . ? C1 C6 C7 N1 8.0(5) . . . . ? C5 C6 C7 C8 7.7(5) . . . . ? C1 C6 C7 C8 -173.6(3) . . . . ? N1 C7 C8 C9 1.0(5) . . . . ? C6 C7 C8 C9 -177.3(3) . . . . ? C7 C8 C9 C10 0.4(6) . . . . ? C8 C9 C10 C11 -0.7(6) . . . . ? C7 N1 C11 C10 1.9(5) . . . . ? C7 N1 C11 C12 -177.0(3) . . . . ? C9 C10 C11 N1 -0.4(5) . . . . ? C9 C10 C11 C12 178.4(3) . . . . ? C13 N2 C12 C11 -74.7(4) . . . . ? C13 N2 C12 C31 159.9(3) . . . . ? N1 C11 C12 N2 -70.8(4) . . . . ? C10 C11 C12 N2 110.4(4) . . . . ? N1 C11 C12 C31 53.6(4) . . . . ? C10 C11 C12 C31 -125.3(4) . . . . ? C12 N2 C13 C14 -73.0(4) . . . . ? C12 N2 C13 C18 106.4(4) . . . . ? C18 C13 C14 C15 -0.7(5) . . . . ? N2 C13 C14 C15 178.7(3) . . . . ? C18 C13 C14 C19 176.4(3) . . . . ? N2 C13 C14 C19 -4.1(5) . . . . ? C13 C14 C15 C16 2.0(5) . . . . ? C19 C14 C15 C16 -175.3(3) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C15 C16 C17 C18 -2.5(6) . . . . ? C16 C17 C18 C13 3.7(5) . . . . ? C16 C17 C18 C22 -179.3(3) . . . . ? C14 C13 C18 C17 -2.0(5) . . . . ? N2 C13 C18 C17 178.6(3) . . . . ? C14 C13 C18 C22 -178.9(3) . . . . ? N2 C13 C18 C22 1.7(5) . . . . ? C15 C14 C19 C20 -63.1(4) . . . . ? C13 C14 C19 C20 119.7(3) . . . . ? C15 C14 C19 C21 60.0(4) . . . . ? C13 C14 C19 C21 -117.2(4) . . . . ? C17 C18 C22 C24 -71.9(4) . . . . ? C13 C18 C22 C24 105.0(4) . . . . ? C17 C18 C22 C23 52.0(5) . . . . ? C13 C18 C22 C23 -131.1(4) . . . . ? C3 C2 C25 C30 -41.9(5) . . . . ? C1 C2 C25 C30 138.0(3) . . . . ? C3 C2 C25 C26 134.7(3) . . . . ? C1 C2 C25 C26 -45.4(5) . . . . ? C30 C25 C26 C27 0.3(5) . . . . ? C2 C25 C26 C27 -176.3(3) . . . . ? C25 C26 C27 C28 -0.5(5) . . . . ? C26 C27 C28 C29 0.0(5) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C26 C25 C30 C29 0.3(5) . . . . ? C2 C25 C30 C29 177.1(3) . . . . ? C28 C29 C30 C25 -0.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.84 1.79 2.543(3) 148.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.185 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.050 data_09097 _database_code_depnum_ccdc_archive 'CCDC 919245' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C32 H32 N2 O3 Pd), C H2 Cl2' _chemical_formula_sum 'C65 H66 Cl2 N4 O6 Pd2' _chemical_formula_weight 1282.92 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 15.311(2) _cell_length_b 11.6253(17) _cell_length_c 32.923(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.364(4) _cell_angle_gamma 90.00 _cell_volume 5860.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 691 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 23.382 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 4744 reflections(SADABS);Rint 0.1085 before correction and 0.0546 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45009 _diffrn_reflns_av_R_equivalents 0.2017 _diffrn_reflns_av_sigmaI/netI 0.2406 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11515 _reflns_number_gt 5339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0186P)^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 11515 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _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 0.22857(4) 0.39545(5) 0.159200(17) 0.02245(16) Uani 1 1 d . . . O1 O 0.3040(3) 0.2735(4) 0.17863(14) 0.0302(14) Uani 1 1 d . . . O2 O 0.3123(3) 0.4162(4) 0.11353(13) 0.0237(13) Uani 1 1 d . . . O3 O 0.4179(3) 0.4883(5) 0.15476(15) 0.0337(15) Uani 1 1 d . . . N1 N 0.1412(4) 0.3737(5) 0.20168(17) 0.0227(16) Uani 1 1 d . . . N2 N 0.1441(4) 0.5105(5) 0.13902(17) 0.0229(16) Uani 1 1 d . . . C1 C 0.2798(5) 0.1949(7) 0.2041(2) 0.026(2) Uani 1 1 d . . . C2 C 0.2123(5) 0.2040(7) 0.2335(2) 0.0265(19) Uani 1 1 d . . . C3 C 0.2035(5) 0.1162(7) 0.2625(2) 0.032(2) Uani 1 1 d . . . H3 H 0.1612 0.1238 0.2833 0.038 Uiso 1 1 calc R . . C4 C 0.2546(6) 0.0201(7) 0.2614(2) 0.035(2) Uani 1 1 d . . . H4 H 0.2473 -0.0383 0.2812 0.042 Uiso 1 1 calc R . . C5 C 0.3174(5) 0.0073(7) 0.2313(2) 0.035(2) Uani 1 1 d . . . H5 H 0.3517 -0.0607 0.2306 0.042 Uiso 1 1 calc R . . C6 C 0.3306(5) 0.0899(7) 0.2030(2) 0.028(2) Uani 1 1 d . . . C7 C 0.3938(5) 0.0788(6) 0.1693(2) 0.027(2) Uani 1 1 d . . . C8 C 0.4791(6) 0.0504(7) 0.1765(2) 0.041(2) Uani 1 1 d . . . H8 H 0.4977 0.0369 0.2037 0.049 Uiso 1 1 calc R . . C9 C 0.5396(6) 0.0406(7) 0.1452(3) 0.048(3) Uani 1 1 d . . . H9 H 0.5992 0.0243 0.1510 0.057 Uiso 1 1 calc R . . C10 C 0.5112(6) 0.0550(7) 0.1059(3) 0.048(3) Uani 1 1 d . . . H10 H 0.5516 0.0477 0.0843 0.058 Uiso 1 1 calc R . . C11 C 0.4244(7) 0.0801(8) 0.0973(3) 0.053(3) Uani 1 1 d . . . H11 H 0.4052 0.0880 0.0699 0.063 Uiso 1 1 calc R . . C12 C 0.3666(6) 0.0933(8) 0.1284(3) 0.046(3) Uani 1 1 d . . . H12 H 0.3075 0.1123 0.1226 0.055 Uiso 1 1 calc R . . C13 C 0.1464(5) 0.3000(7) 0.2333(2) 0.0249(19) Uani 1 1 d . . . C14 C 0.0838(5) 0.3117(7) 0.2650(2) 0.032(2) Uani 1 1 d . . . H14 H 0.0891 0.2659 0.2888 0.039 Uiso 1 1 calc R . . C15 C 0.0181(5) 0.3859(7) 0.2617(2) 0.035(2) Uani 1 1 d . . . H15 H -0.0239 0.3905 0.2828 0.042 Uiso 1 1 calc R . . C16 C 0.0100(5) 0.4564(7) 0.2283(2) 0.033(2) Uani 1 1 d . . . H16 H -0.0381 0.5075 0.2255 0.039 Uiso 1 1 calc R . . C17 C 0.0745(5) 0.4504(7) 0.1986(2) 0.027(2) Uani 1 1 d . . . C18 C 0.0771(5) 0.5213(6) 0.1623(2) 0.029(2) Uani 1 1 d . . . H18 H 0.0313 0.5735 0.1560 0.035 Uiso 1 1 calc R . . C19 C 0.1528(5) 0.5759(7) 0.1019(2) 0.027(2) Uani 1 1 d . . . C20 C 0.1394(5) 0.5179(7) 0.0651(2) 0.028(2) Uani 1 1 d . . . C21 C 0.1496(5) 0.5812(7) 0.0303(2) 0.032(2) Uani 1 1 d . . . H21 H 0.1402 0.5447 0.0048 0.039 Uiso 1 1 calc R . . C22 C 0.1733(5) 0.6969(8) 0.0309(2) 0.041(2) Uani 1 1 d . . . H22 H 0.1800 0.7387 0.0064 0.050 Uiso 1 1 calc R . . C23 C 0.1866(5) 0.7489(7) 0.0677(2) 0.042(2) Uani 1 1 d . . . H23 H 0.2026 0.8279 0.0682 0.050 Uiso 1 1 calc R . . C24 C 0.1778(5) 0.6915(7) 0.1041(2) 0.031(2) Uani 1 1 d . . . C25 C 0.1170(5) 0.3911(7) 0.0632(2) 0.034(2) Uani 1 1 d . . . H25 H 0.1160 0.3604 0.0915 0.040 Uiso 1 1 calc R . . C26 C 0.0267(5) 0.3746(7) 0.0446(2) 0.044(2) Uani 1 1 d . . . H26D H 0.0250 0.4094 0.0175 0.067 Uiso 1 1 calc R . . H26E H -0.0169 0.4115 0.0619 0.067 Uiso 1 1 calc R . . H26F H 0.0139 0.2922 0.0425 0.067 Uiso 1 1 calc R . . C27 C 0.1852(6) 0.3240(7) 0.0395(2) 0.050(3) Uani 1 1 d . . . H27D H 0.1880 0.3536 0.0116 0.075 Uiso 1 1 calc R . . H27E H 0.1692 0.2424 0.0389 0.075 Uiso 1 1 calc R . . H27F H 0.2424 0.3329 0.0526 0.075 Uiso 1 1 calc R . . C28 C 0.2003(5) 0.7522(7) 0.1436(2) 0.039(2) Uani 1 1 d . . . H28 H 0.1836 0.7000 0.1663 0.047 Uiso 1 1 calc R . . C29 C 0.2978(6) 0.7712(7) 0.1462(3) 0.059(3) Uani 1 1 d . . . H29A H 0.3277 0.6967 0.1470 0.088 Uiso 1 1 calc R . . H29B H 0.3118 0.8145 0.1710 0.088 Uiso 1 1 calc R . . H29C H 0.3172 0.8148 0.1225 0.088 Uiso 1 1 calc R . . C30 C 0.1490(6) 0.8636(8) 0.1485(3) 0.067(3) Uani 1 1 d . . . H30A H 0.1660 0.9180 0.1272 0.101 Uiso 1 1 calc R . . H30B H 0.1616 0.8970 0.1752 0.101 Uiso 1 1 calc R . . H30C H 0.0863 0.8473 0.1462 0.101 Uiso 1 1 calc R . . C31 C 0.3923(6) 0.4439(7) 0.1231(2) 0.033(2) Uani 1 1 d . . . C32 C 0.4549(5) 0.4148(7) 0.0892(2) 0.044(2) Uani 1 1 d . . . H32D H 0.4525 0.4750 0.0684 0.065 Uiso 1 1 calc R . . H32E H 0.4384 0.3408 0.0771 0.065 Uiso 1 1 calc R . . H32F H 0.5144 0.4096 0.1002 0.065 Uiso 1 1 calc R . . Pd1A Pd 0.72714(4) 0.79012(5) 0.148316(17) 0.02406(17) Uani 1 1 d . . . O1A O 0.8014(3) 0.9159(4) 0.16688(15) 0.0325(14) Uani 1 1 d . . . O2A O 0.8090(3) 0.7668(4) 0.10179(14) 0.0271(13) Uani 1 1 d . . . O3A O 0.9058(3) 0.6803(5) 0.14354(16) 0.0379(16) Uani 1 1 d . . . N1A N 0.6441(4) 0.8115(5) 0.19266(17) 0.0246(16) Uani 1 1 d . . . N2A N 0.6449(4) 0.6662(5) 0.13114(18) 0.0258(16) Uani 1 1 d . . . C1A C 0.7802(5) 0.9909(7) 0.1939(2) 0.030(2) Uani 1 1 d . . . C2A C 0.7114(5) 0.9830(7) 0.2229(2) 0.032(2) Uani 1 1 d . . . C3A C 0.7022(6) 1.0707(7) 0.2514(2) 0.040(2) Uani 1 1 d . . . H3A H 0.6573 1.0648 0.2711 0.047 Uiso 1 1 calc R . . C4A C 0.7553(6) 1.1641(9) 0.2521(3) 0.048(3) Uani 1 1 d . . . H4A H 0.7465 1.2239 0.2713 0.057 Uiso 1 1 calc R . . C5A C 0.8230(6) 1.1708(7) 0.2242(3) 0.042(2) Uani 1 1 d . . . H5A H 0.8618 1.2345 0.2255 0.051 Uiso 1 1 calc R . . C6A C 0.8358(5) 1.0891(7) 0.1948(2) 0.035(2) Uani 1 1 d . . . C7A C 0.9098(6) 1.0982(7) 0.1652(2) 0.035(2) Uani 1 1 d . . . C8A C 0.9929(6) 1.1316(6) 0.1780(3) 0.037(2) Uani 1 1 d . . . H8A H 1.0034 1.1477 0.2059 0.045 Uiso 1 1 calc R . . C9A C 1.0595(6) 1.1413(7) 0.1508(3) 0.042(2) Uani 1 1 d . . . H9A H 1.1162 1.1619 0.1601 0.050 Uiso 1 1 calc R . . C10A C 1.0457(6) 1.1221(7) 0.1107(3) 0.051(3) Uani 1 1 d . . . H10A H 1.0927 1.1280 0.0921 0.061 Uiso 1 1 calc R . . C11A C 0.9649(7) 1.0947(8) 0.0974(3) 0.053(3) Uani 1 1 d . . . H11A H 0.9547 1.0840 0.0691 0.063 Uiso 1 1 calc R . . C12A C 0.8963(6) 1.0818(7) 0.1246(3) 0.048(3) Uani 1 1 d . . . H12A H 0.8398 1.0616 0.1148 0.058 Uiso 1 1 calc R . . C13A C 0.6466(5) 0.8867(7) 0.2232(2) 0.028(2) Uani 1 1 d . . . C14A C 0.5875(5) 0.8767(7) 0.2553(2) 0.032(2) Uani 1 1 d . . . H14A H 0.5910 0.9280 0.2777 0.038 Uiso 1 1 calc R . . C15A C 0.5247(5) 0.7933(8) 0.2544(2) 0.037(2) Uani 1 1 d . . . H15A H 0.4847 0.7868 0.2762 0.044 Uiso 1 1 calc R . . C16A C 0.5190(5) 0.7183(7) 0.2220(2) 0.036(2) Uani 1 1 d . . . H16A H 0.4741 0.6620 0.2206 0.043 Uiso 1 1 calc R . . C17A C 0.5803(5) 0.7277(7) 0.1919(2) 0.028(2) Uani 1 1 d . . . C18A C 0.5830(5) 0.6516(7) 0.1573(2) 0.032(2) Uani 1 1 d . . . H18A H 0.5407 0.5926 0.1539 0.039 Uiso 1 1 calc R . . C19A C 0.6486(5) 0.5993(8) 0.0941(2) 0.029(2) Uani 1 1 d . . . C20A C 0.6905(5) 0.4935(7) 0.0948(2) 0.032(2) Uani 1 1 d . . . C21A C 0.6931(5) 0.4303(8) 0.0592(3) 0.044(3) Uani 1 1 d . . . H21A H 0.7213 0.3576 0.0587 0.053 Uiso 1 1 calc R . . C22A C 0.6550(6) 0.4727(9) 0.0248(3) 0.052(3) Uani 1 1 d . . . H22A H 0.6570 0.4291 0.0004 0.062 Uiso 1 1 calc R . . C23A C 0.6136(6) 0.5779(8) 0.0248(2) 0.043(3) Uani 1 1 d . . . H23A H 0.5862 0.6050 0.0007 0.052 Uiso 1 1 calc R . . C24A C 0.6114(5) 0.6447(7) 0.0596(2) 0.032(2) Uani 1 1 d . . . C25A C 0.7312(5) 0.4448(7) 0.1329(2) 0.035(2) Uani 1 1 d . . . H25A H 0.7338 0.5071 0.1539 0.042 Uiso 1 1 calc R . . C26A C 0.6760(6) 0.3487(7) 0.1490(3) 0.057(3) Uani 1 1 d . . . H26A H 0.6190 0.3789 0.1571 0.086 Uiso 1 1 calc R . . H26B H 0.7050 0.3138 0.1726 0.086 Uiso 1 1 calc R . . H26C H 0.6679 0.2904 0.1278 0.086 Uiso 1 1 calc R . . C27A C 0.8233(6) 0.3978(8) 0.1269(3) 0.066(3) Uani 1 1 d . . . H27A H 0.8213 0.3332 0.1078 0.099 Uiso 1 1 calc R . . H27B H 0.8470 0.3715 0.1530 0.099 Uiso 1 1 calc R . . H27C H 0.8608 0.4586 0.1160 0.099 Uiso 1 1 calc R . . C28A C 0.5631(6) 0.7606(8) 0.0594(3) 0.048(3) Uani 1 1 d . . . H28A H 0.5918 0.8113 0.0801 0.058 Uiso 1 1 calc R . . C29A C 0.5654(7) 0.8233(7) 0.0185(3) 0.069(3) Uani 1 1 d . . . H29D H 0.6261 0.8332 0.0100 0.104 Uiso 1 1 calc R . . H29E H 0.5377 0.8989 0.0212 0.104 Uiso 1 1 calc R . . H29F H 0.5337 0.7780 -0.0020 0.104 Uiso 1 1 calc R . . C30A C 0.4666(6) 0.7464(8) 0.0716(3) 0.074(3) Uani 1 1 d . . . H30D H 0.4351 0.7048 0.0502 0.111 Uiso 1 1 calc R . . H30E H 0.4402 0.8224 0.0753 0.111 Uiso 1 1 calc R . . H30F H 0.4633 0.7030 0.0971 0.111 Uiso 1 1 calc R . . C31A C 0.8834(5) 0.7203(7) 0.1107(2) 0.031(2) Uani 1 1 d . . . C32A C 0.9460(5) 0.7196(8) 0.0748(2) 0.059(3) Uani 1 1 d . . . H32A H 0.9745 0.7949 0.0726 0.089 Uiso 1 1 calc R . . H32B H 0.9134 0.7036 0.0497 0.089 Uiso 1 1 calc R . . H32C H 0.9904 0.6600 0.0789 0.089 Uiso 1 1 calc R . . C33 C 0.7931(6) 0.9486(8) 0.0288(3) 0.080(4) Uani 1 1 d . . . H33A H 0.7595 0.8837 0.0170 0.096 Uiso 1 1 calc R . . H33B H 0.8188 0.9224 0.0548 0.096 Uiso 1 1 calc R . . Cl1 Cl 0.87760(19) 0.9872(2) -0.00470(8) 0.0771(9) Uani 1 1 d . . . Cl2 Cl 0.7227(2) 1.0638(3) 0.03773(10) 0.0994(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0210(4) 0.0252(4) 0.0212(3) 0.0034(3) 0.0015(3) -0.0019(3) O1 0.033(3) 0.029(3) 0.029(3) 0.016(3) 0.005(3) 0.006(3) O2 0.018(3) 0.032(4) 0.022(3) 0.008(3) -0.001(2) -0.001(3) O3 0.033(4) 0.043(4) 0.026(3) -0.005(3) 0.006(3) -0.013(3) N1 0.032(4) 0.016(4) 0.021(4) -0.003(3) 0.003(3) -0.008(3) N2 0.026(4) 0.027(4) 0.016(3) 0.002(3) 0.001(3) 0.002(3) C1 0.027(5) 0.033(5) 0.017(4) 0.003(4) -0.009(3) -0.005(4) C2 0.036(5) 0.029(5) 0.015(4) 0.004(4) -0.002(4) -0.015(4) C3 0.028(5) 0.039(6) 0.027(5) 0.004(4) 0.004(4) -0.012(5) C4 0.049(6) 0.030(6) 0.027(5) 0.009(4) -0.002(4) -0.003(5) C5 0.048(6) 0.025(5) 0.031(5) 0.004(4) -0.009(4) 0.004(5) C6 0.027(5) 0.028(5) 0.030(5) 0.007(4) -0.008(4) -0.006(4) C7 0.038(6) 0.011(5) 0.031(5) 0.001(4) -0.006(4) 0.004(4) C8 0.051(7) 0.041(6) 0.031(5) 0.000(4) 0.002(5) 0.010(5) C9 0.056(7) 0.039(6) 0.048(6) 0.008(5) 0.012(5) 0.029(5) C10 0.052(7) 0.049(7) 0.044(6) -0.001(5) 0.022(5) 0.011(5) C11 0.068(8) 0.048(7) 0.041(6) 0.006(5) -0.004(6) 0.012(6) C12 0.039(6) 0.060(7) 0.038(6) 0.004(5) 0.001(5) 0.003(5) C13 0.025(5) 0.024(5) 0.026(5) -0.009(4) 0.004(4) -0.013(4) C14 0.043(6) 0.029(5) 0.025(5) 0.001(4) 0.009(4) -0.017(5) C15 0.044(6) 0.034(6) 0.027(5) 0.002(4) 0.016(4) -0.008(5) C16 0.030(5) 0.037(6) 0.031(5) -0.005(4) 0.012(4) 0.001(4) C17 0.035(5) 0.021(5) 0.024(5) -0.009(4) 0.009(4) -0.004(4) C18 0.028(5) 0.024(5) 0.034(5) 0.002(4) -0.002(4) -0.004(4) C19 0.025(5) 0.030(5) 0.028(5) 0.013(4) 0.006(4) 0.007(4) C20 0.030(5) 0.029(5) 0.026(5) -0.002(4) -0.003(4) 0.014(4) C21 0.034(5) 0.040(6) 0.024(5) 0.004(4) 0.002(4) 0.003(4) C22 0.045(6) 0.049(7) 0.031(5) 0.014(5) 0.009(4) 0.010(5) C23 0.057(7) 0.030(6) 0.038(6) 0.009(5) 0.016(5) 0.006(5) C24 0.034(5) 0.027(5) 0.032(5) 0.002(4) 0.003(4) 0.003(4) C25 0.039(6) 0.036(6) 0.025(5) -0.001(4) -0.003(4) 0.006(5) C26 0.050(6) 0.038(6) 0.046(6) -0.002(5) -0.002(5) -0.005(5) C27 0.052(7) 0.051(7) 0.047(6) -0.017(5) -0.001(5) 0.005(5) C28 0.045(6) 0.036(6) 0.036(5) 0.006(4) 0.014(5) 0.006(5) C29 0.073(8) 0.038(6) 0.065(7) -0.027(5) 0.015(6) -0.023(6) C30 0.086(9) 0.066(8) 0.050(7) -0.012(6) 0.021(6) 0.021(6) C31 0.042(6) 0.032(6) 0.026(5) 0.012(4) 0.005(4) 0.008(5) C32 0.031(5) 0.063(7) 0.037(5) -0.010(5) 0.012(4) -0.011(5) Pd1A 0.0227(4) 0.0270(4) 0.0225(3) -0.0033(3) 0.0015(3) 0.0005(3) O1A 0.029(3) 0.035(4) 0.033(3) -0.011(3) 0.004(3) -0.009(3) O2A 0.025(3) 0.027(3) 0.030(3) -0.003(3) 0.007(3) -0.002(3) O3A 0.041(4) 0.045(4) 0.027(3) 0.002(3) 0.007(3) 0.015(3) N1A 0.023(4) 0.031(4) 0.019(4) -0.005(3) 0.003(3) 0.008(3) N2A 0.034(4) 0.021(4) 0.022(4) 0.002(3) 0.002(3) 0.000(3) C1A 0.039(6) 0.029(6) 0.023(5) -0.002(4) 0.000(4) 0.007(5) C2A 0.040(6) 0.031(5) 0.024(5) -0.014(4) -0.011(4) 0.020(5) C3A 0.036(6) 0.042(6) 0.040(6) -0.011(5) -0.005(4) 0.011(5) C4A 0.046(6) 0.056(7) 0.041(6) -0.024(5) -0.004(5) 0.026(5) C5A 0.049(7) 0.029(6) 0.049(6) -0.013(5) -0.018(5) 0.003(5) C6A 0.039(6) 0.029(6) 0.037(5) -0.007(5) -0.009(4) 0.013(5) C7A 0.045(6) 0.026(5) 0.034(5) -0.008(5) -0.005(4) -0.007(5) C8A 0.054(7) 0.018(5) 0.039(6) -0.006(4) -0.009(5) -0.008(5) C9A 0.039(6) 0.039(6) 0.048(6) -0.013(5) -0.004(5) -0.013(5) C10A 0.061(7) 0.046(7) 0.045(6) -0.003(5) 0.008(5) -0.016(6) C11A 0.067(8) 0.054(7) 0.037(6) -0.001(5) -0.008(5) -0.032(6) C12A 0.058(7) 0.040(6) 0.046(6) 0.003(5) -0.025(5) -0.023(5) C13A 0.023(5) 0.031(5) 0.029(5) 0.005(4) -0.009(4) 0.009(4) C14A 0.037(6) 0.039(6) 0.019(4) 0.005(4) 0.010(4) 0.016(5) C15A 0.039(6) 0.055(7) 0.018(5) 0.014(5) 0.014(4) 0.026(5) C16A 0.038(6) 0.043(6) 0.026(5) 0.014(5) 0.011(4) -0.001(5) C17A 0.042(6) 0.027(5) 0.015(4) 0.003(4) 0.004(4) 0.006(4) C18A 0.029(5) 0.034(5) 0.034(5) 0.001(4) 0.002(4) -0.002(4) C19A 0.028(5) 0.037(6) 0.022(5) -0.002(4) 0.006(4) -0.015(5) C20A 0.031(5) 0.026(5) 0.039(5) -0.006(4) 0.008(4) -0.007(4) C21A 0.039(6) 0.055(7) 0.039(6) -0.022(5) 0.005(5) 0.002(5) C22A 0.044(7) 0.072(8) 0.040(6) -0.032(6) 0.009(5) -0.018(6) C23A 0.042(6) 0.064(7) 0.024(5) -0.007(5) 0.002(4) -0.010(5) C24A 0.029(5) 0.045(6) 0.021(5) 0.005(4) 0.005(4) -0.004(4) C25A 0.039(6) 0.030(5) 0.037(5) 0.012(4) 0.001(4) 0.008(5) C26A 0.054(7) 0.062(7) 0.055(7) 0.014(6) -0.012(5) -0.004(6) C27A 0.049(7) 0.065(7) 0.084(8) -0.010(7) -0.014(6) 0.013(6) C28A 0.065(8) 0.043(6) 0.037(6) -0.005(5) -0.014(5) 0.006(6) C29A 0.104(10) 0.054(7) 0.049(7) 0.014(6) -0.015(6) 0.005(7) C30A 0.072(9) 0.065(8) 0.086(8) 0.010(6) 0.008(7) 0.016(7) C31A 0.031(6) 0.030(6) 0.032(5) 0.001(5) 0.006(4) -0.005(4) C32A 0.043(6) 0.100(9) 0.036(6) 0.004(6) 0.015(5) 0.023(6) C33 0.070(8) 0.064(8) 0.107(9) 0.006(7) 0.041(7) -0.002(7) Cl1 0.093(2) 0.077(2) 0.0613(18) 0.0016(16) 0.0123(16) -0.0158(18) Cl2 0.082(2) 0.080(2) 0.136(3) -0.003(2) 0.013(2) 0.0092(19) _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 O1 1.934(5) . ? Pd1 N1 1.958(6) . ? Pd1 N2 1.973(6) . ? Pd1 O2 1.997(5) . ? O1 C1 1.296(8) . ? O2 C31 1.303(9) . ? O3 C31 1.225(9) . ? N1 C13 1.350(8) . ? N1 C17 1.359(9) . ? N2 C18 1.292(8) . ? N2 C19 1.447(8) . ? C1 C2 1.424(10) . ? C1 C6 1.448(10) . ? C2 C3 1.406(9) . ? C2 C13 1.503(10) . ? C3 C4 1.364(10) . ? C3 H3 0.9500 . ? C4 C5 1.392(10) . ? C4 H4 0.9500 . ? C5 C6 1.354(9) . ? C5 H5 0.9500 . ? C6 C7 1.483(10) . ? C7 C8 1.365(10) . ? C7 C12 1.416(10) . ? C8 C9 1.396(10) . ? C8 H8 0.9500 . ? C9 C10 1.372(11) . ? C9 H9 0.9500 . ? C10 C11 1.389(11) . ? C10 H10 0.9500 . ? C11 C12 1.367(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.429(9) . ? C14 C15 1.328(10) . ? C14 H14 0.9500 . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 C17 1.396(9) . ? C16 H16 0.9500 . ? C17 C18 1.451(9) . ? C18 H18 0.9500 . ? C19 C20 1.399(10) . ? C19 C24 1.399(10) . ? C20 C21 1.372(9) . ? C20 C25 1.515(10) . ? C21 C22 1.394(10) . ? C21 H21 0.9500 . ? C22 C23 1.368(10) . ? C22 H22 0.9500 . ? C23 C24 1.378(10) . ? C23 H23 0.9500 . ? C24 C28 1.516(10) . ? C25 C26 1.520(10) . ? C25 C27 1.522(10) . ? C25 H25 1.0000 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C28 C29 1.512(11) . ? C28 C30 1.523(10) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.514(10) . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? Pd1A O1A 1.948(5) . ? Pd1A N1A 1.958(6) . ? Pd1A N2A 1.993(6) . ? Pd1A O2A 2.004(5) . ? O1A C1A 1.287(8) . ? O2A C31A 1.293(9) . ? O3A C31A 1.224(8) . ? N1A C13A 1.333(9) . ? N1A C17A 1.379(9) . ? N2A C18A 1.297(8) . ? N2A C19A 1.449(9) . ? C1A C6A 1.425(10) . ? C1A C2A 1.430(10) . ? C2A C3A 1.395(10) . ? C2A C13A 1.495(10) . ? C3A C4A 1.357(11) . ? C3A H3A 0.9500 . ? C4A C5A 1.392(11) . ? C4A H4A 0.9500 . ? C5A C6A 1.369(10) . ? C5A H5A 0.9500 . ? C6A C7A 1.503(11) . ? C7A C12A 1.366(10) . ? C7A C8A 1.393(10) . ? C8A C9A 1.366(10) . ? C8A H8A 0.9500 . ? C9A C10A 1.353(10) . ? C9A H9A 0.9500 . ? C10A C11A 1.349(11) . ? C10A H10A 0.9500 . ? C11A C12A 1.394(11) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C14A 1.400(9) . ? C14A C15A 1.366(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.380(10) . ? C15A H15A 0.9500 . ? C16A C17A 1.374(9) . ? C16A H16A 0.9500 . ? C17A C18A 1.441(10) . ? C18A H18A 0.9500 . ? C19A C24A 1.373(10) . ? C19A C20A 1.387(10) . ? C20A C21A 1.386(10) . ? C20A C25A 1.507(10) . ? C21A C22A 1.364(11) . ? C21A H21A 0.9500 . ? C22A C23A 1.378(11) . ? C22A H22A 0.9500 . ? C23A C24A 1.383(10) . ? C23A H23A 0.9500 . ? C24A C28A 1.537(11) . ? C25A C26A 1.500(10) . ? C25A C27A 1.526(10) . ? C25A H25A 1.0000 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A C29A 1.534(10) . ? C28A C30A 1.541(11) . ? C28A H28A 1.0000 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31A C32A 1.527(10) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33 Cl2 1.746(9) . ? C33 Cl1 1.763(9) . ? C33 H33A 0.9900 . ? C33 H33B 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 O1 Pd1 N1 94.5(2) . . ? O1 Pd1 N2 175.4(2) . . ? N1 Pd1 N2 83.1(3) . . ? O1 Pd1 O2 87.3(2) . . ? N1 Pd1 O2 176.8(2) . . ? N2 Pd1 O2 95.0(2) . . ? C1 O1 Pd1 124.0(5) . . ? C31 O2 Pd1 117.1(5) . . ? C13 N1 C17 121.0(7) . . ? C13 N1 Pd1 126.6(5) . . ? C17 N1 Pd1 112.2(5) . . ? C18 N2 C19 121.9(6) . . ? C18 N2 Pd1 112.8(5) . . ? C19 N2 Pd1 125.3(5) . . ? O1 C1 C2 126.7(7) . . ? O1 C1 C6 115.0(7) . . ? C2 C1 C6 118.2(7) . . ? C3 C2 C1 118.7(8) . . ? C3 C2 C13 118.3(7) . . ? C1 C2 C13 122.9(7) . . ? C4 C3 C2 121.3(8) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.3(8) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 121.4(8) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 119.8(8) . . ? C5 C6 C7 123.7(8) . . ? C1 C6 C7 116.5(7) . . ? C8 C7 C12 118.0(8) . . ? C8 C7 C6 121.3(7) . . ? C12 C7 C6 120.7(7) . . ? C7 C8 C9 122.0(8) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 118.6(9) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 121.0(8) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.6(9) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 120.7(9) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? N1 C13 C14 117.8(7) . . ? N1 C13 C2 120.6(7) . . ? C14 C13 C2 121.4(7) . . ? C15 C14 C13 120.9(8) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 121.1(8) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 118.0(8) . . ? C15 C16 H16 121.0 . . ? C17 C16 H16 121.0 . . ? N1 C17 C16 121.0(7) . . ? N1 C17 C18 114.2(7) . . ? C16 C17 C18 124.8(8) . . ? N2 C18 C17 117.4(7) . . ? N2 C18 H18 121.3 . . ? C17 C18 H18 121.3 . . ? C20 C19 C24 123.2(7) . . ? C20 C19 N2 117.6(7) . . ? C24 C19 N2 119.1(7) . . ? C21 C20 C19 116.6(8) . . ? C21 C20 C25 120.8(7) . . ? C19 C20 C25 122.6(7) . . ? C20 C21 C22 122.5(8) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 118.5(8) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C22 C23 C24 122.7(8) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C19 116.6(8) . . ? C23 C24 C28 119.7(8) . . ? C19 C24 C28 123.6(7) . . ? C20 C25 C26 110.2(7) . . ? C20 C25 C27 111.4(7) . . ? C26 C25 C27 110.8(7) . . ? C20 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? C27 C25 H25 108.1 . . ? C25 C26 H26D 109.5 . . ? C25 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C25 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C25 C27 H27D 109.5 . . ? C25 C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? C25 C27 H27F 109.5 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C29 C28 C24 109.7(7) . . ? C29 C28 C30 112.3(8) . . ? C24 C28 C30 111.9(7) . . ? C29 C28 H28 107.6 . . ? C24 C28 H28 107.6 . . ? C30 C28 H28 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 O2 127.2(8) . . ? O3 C31 C32 121.4(8) . . ? O2 C31 C32 111.4(7) . . ? C31 C32 H32D 109.5 . . ? C31 C32 H32E 109.5 . . ? H32D C32 H32E 109.5 . . ? C31 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? O1A Pd1A N1A 92.9(2) . . ? O1A Pd1A N2A 176.4(2) . . ? N1A Pd1A N2A 83.8(3) . . ? O1A Pd1A O2A 88.6(2) . . ? N1A Pd1A O2A 178.2(2) . . ? N2A Pd1A O2A 94.7(2) . . ? C1A O1A Pd1A 125.2(5) . . ? C31A O2A Pd1A 115.9(5) . . ? C13A N1A C17A 119.7(7) . . ? C13A N1A Pd1A 129.0(6) . . ? C17A N1A Pd1A 111.1(5) . . ? C18A N2A C19A 121.5(7) . . ? C18A N2A Pd1A 111.6(5) . . ? C19A N2A Pd1A 126.8(5) . . ? O1A C1A C6A 113.9(7) . . ? O1A C1A C2A 127.4(8) . . ? C6A C1A C2A 118.6(8) . . ? C3A C2A C1A 118.8(8) . . ? C3A C2A C13A 118.2(8) . . ? C1A C2A C13A 123.0(7) . . ? C4A C3A C2A 122.1(9) . . ? C4A C3A H3A 118.9 . . ? C2A C3A H3A 118.9 . . ? C3A C4A C5A 118.9(9) . . ? C3A C4A H4A 120.5 . . ? C5A C4A H4A 120.5 . . ? C6A C5A C4A 122.5(9) . . ? C6A C5A H5A 118.8 . . ? C4A C5A H5A 118.8 . . ? C5A C6A C1A 118.9(8) . . ? C5A C6A C7A 121.4(8) . . ? C1A C6A C7A 119.6(7) . . ? C12A C7A C8A 117.9(8) . . ? C12A C7A C6A 121.0(8) . . ? C8A C7A C6A 121.0(8) . . ? C9A C8A C7A 120.6(8) . . ? C9A C8A H8A 119.7 . . ? C7A C8A H8A 119.7 . . ? C10A C9A C8A 120.9(9) . . ? C10A C9A H9A 119.5 . . ? C8A C9A H9A 119.5 . . ? C11A C10A C9A 119.6(9) . . ? C11A C10A H10A 120.2 . . ? C9A C10A H10A 120.2 . . ? C10A C11A C12A 120.6(9) . . ? C10A C11A H11A 119.7 . . ? C12A C11A H11A 119.7 . . ? C7A C12A C11A 120.3(8) . . ? C7A C12A H12A 119.8 . . ? C11A C12A H12A 119.8 . . ? N1A C13A C14A 119.9(8) . . ? N1A C13A C2A 120.1(7) . . ? C14A C13A C2A 120.0(8) . . ? C15A C14A C13A 120.2(8) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C14A C15A C16A 120.3(7) . . ? C14A C15A H15A 119.8 . . ? C16A C15A H15A 119.8 . . ? C17A C16A C15A 117.9(8) . . ? C17A C16A H16A 121.0 . . ? C15A C16A H16A 121.0 . . ? C16A C17A N1A 121.9(7) . . ? C16A C17A C18A 122.9(8) . . ? N1A C17A C18A 115.1(7) . . ? N2A C18A C17A 118.0(8) . . ? N2A C18A H18A 121.0 . . ? C17A C18A H18A 121.0 . . ? C24A C19A C20A 123.1(8) . . ? C24A C19A N2A 118.1(8) . . ? C20A C19A N2A 118.7(7) . . ? C21A C20A C19A 118.0(8) . . ? C21A C20A C25A 119.5(8) . . ? C19A C20A C25A 122.5(7) . . ? C22A C21A C20A 119.9(9) . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? C21A C22A C23A 120.9(9) . . ? C21A C22A H22A 119.5 . . ? C23A C22A H22A 119.5 . . ? C22A C23A C24A 120.9(9) . . ? C22A C23A H23A 119.5 . . ? C24A C23A H23A 119.5 . . ? C19A C24A C23A 117.1(8) . . ? C19A C24A C28A 122.5(8) . . ? C23A C24A C28A 120.2(8) . . ? C26A C25A C20A 110.0(7) . . ? C26A C25A C27A 107.6(7) . . ? C20A C25A C27A 113.7(7) . . ? C26A C25A H25A 108.4 . . ? C20A C25A H25A 108.4 . . ? C27A C25A H25A 108.4 . . ? C25A C26A H26A 109.5 . . ? C25A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25A C27A H27A 109.5 . . ? C25A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C29A C28A C24A 114.0(7) . . ? C29A C28A C30A 107.9(8) . . ? C24A C28A C30A 111.5(7) . . ? C29A C28A H28A 107.7 . . ? C24A C28A H28A 107.7 . . ? C30A C28A H28A 107.7 . . ? C28A C29A H29D 109.5 . . ? C28A C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C28A C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C28A C30A H30D 109.5 . . ? C28A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C28A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? O3A C31A O2A 126.9(8) . . ? O3A C31A C32A 120.6(8) . . ? O2A C31A C32A 112.5(7) . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? Cl2 C33 Cl1 111.5(5) . . ? Cl2 C33 H33A 109.3 . . ? Cl1 C33 H33A 109.3 . . ? Cl2 C33 H33B 109.3 . . ? Cl1 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 O1 C1 15.7(6) . . . . ? O2 Pd1 O1 C1 -161.6(6) . . . . ? O1 Pd1 O2 C31 -60.7(5) . . . . ? N2 Pd1 O2 C31 123.3(5) . . . . ? O1 Pd1 N1 C13 4.3(6) . . . . ? N2 Pd1 N1 C13 -179.6(6) . . . . ? O1 Pd1 N1 C17 178.5(5) . . . . ? N2 Pd1 N1 C17 -5.4(5) . . . . ? N1 Pd1 N2 C18 2.7(5) . . . . ? O2 Pd1 N2 C18 -179.9(5) . . . . ? N1 Pd1 N2 C19 -176.0(6) . . . . ? O2 Pd1 N2 C19 1.4(6) . . . . ? Pd1 O1 C1 C2 -25.7(10) . . . . ? Pd1 O1 C1 C6 157.2(5) . . . . ? O1 C1 C2 C3 -170.9(7) . . . . ? C6 C1 C2 C3 6.2(10) . . . . ? O1 C1 C2 C13 12.9(12) . . . . ? C6 C1 C2 C13 -170.0(6) . . . . ? C1 C2 C3 C4 -4.1(11) . . . . ? C13 C2 C3 C4 172.3(7) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? C3 C4 C5 C6 1.2(12) . . . . ? C4 C5 C6 C1 1.1(12) . . . . ? C4 C5 C6 C7 -177.3(7) . . . . ? O1 C1 C6 C5 172.6(7) . . . . ? C2 C1 C6 C5 -4.8(11) . . . . ? O1 C1 C6 C7 -8.9(10) . . . . ? C2 C1 C6 C7 173.8(7) . . . . ? C5 C6 C7 C8 -52.6(11) . . . . ? C1 C6 C7 C8 128.9(8) . . . . ? C5 C6 C7 C12 125.0(9) . . . . ? C1 C6 C7 C12 -53.4(10) . . . . ? C12 C7 C8 C9 2.9(12) . . . . ? C6 C7 C8 C9 -179.4(8) . . . . ? C7 C8 C9 C10 -3.0(13) . . . . ? C8 C9 C10 C11 0.7(14) . . . . ? C9 C10 C11 C12 1.5(14) . . . . ? C10 C11 C12 C7 -1.6(14) . . . . ? C8 C7 C12 C11 -0.6(13) . . . . ? C6 C7 C12 C11 -178.3(8) . . . . ? C17 N1 C13 C14 -5.1(10) . . . . ? Pd1 N1 C13 C14 168.7(5) . . . . ? C17 N1 C13 C2 170.8(7) . . . . ? Pd1 N1 C13 C2 -15.4(10) . . . . ? C3 C2 C13 N1 -167.0(6) . . . . ? C1 C2 C13 N1 9.2(11) . . . . ? C3 C2 C13 C14 8.8(11) . . . . ? C1 C2 C13 C14 -175.0(7) . . . . ? N1 C13 C14 C15 5.8(11) . . . . ? C2 C13 C14 C15 -170.1(7) . . . . ? C13 C14 C15 C16 -2.1(12) . . . . ? C14 C15 C16 C17 -2.3(12) . . . . ? C13 N1 C17 C16 0.8(11) . . . . ? Pd1 N1 C17 C16 -173.8(6) . . . . ? C13 N1 C17 C18 -178.4(6) . . . . ? Pd1 N1 C17 C18 7.0(8) . . . . ? C15 C16 C17 N1 3.0(11) . . . . ? C15 C16 C17 C18 -177.8(7) . . . . ? C19 N2 C18 C17 179.2(7) . . . . ? Pd1 N2 C18 C17 0.4(8) . . . . ? N1 C17 C18 N2 -5.0(10) . . . . ? C16 C17 C18 N2 175.7(7) . . . . ? C18 N2 C19 C20 -105.6(8) . . . . ? Pd1 N2 C19 C20 73.0(8) . . . . ? C18 N2 C19 C24 77.3(9) . . . . ? Pd1 N2 C19 C24 -104.1(7) . . . . ? C24 C19 C20 C21 -1.8(11) . . . . ? N2 C19 C20 C21 -178.8(6) . . . . ? C24 C19 C20 C25 176.7(7) . . . . ? N2 C19 C20 C25 -0.3(11) . . . . ? C19 C20 C21 C22 0.9(11) . . . . ? C25 C20 C21 C22 -177.6(7) . . . . ? C20 C21 C22 C23 -0.1(12) . . . . ? C21 C22 C23 C24 0.2(13) . . . . ? C22 C23 C24 C19 -1.0(12) . . . . ? C22 C23 C24 C28 175.3(8) . . . . ? C20 C19 C24 C23 1.9(12) . . . . ? N2 C19 C24 C23 178.8(7) . . . . ? C20 C19 C24 C28 -174.3(7) . . . . ? N2 C19 C24 C28 2.6(11) . . . . ? C21 C20 C25 C26 -65.3(9) . . . . ? C19 C20 C25 C26 116.3(8) . . . . ? C21 C20 C25 C27 58.1(10) . . . . ? C19 C20 C25 C27 -120.4(8) . . . . ? C23 C24 C28 C29 -69.3(10) . . . . ? C19 C24 C28 C29 106.8(9) . . . . ? C23 C24 C28 C30 56.0(10) . . . . ? C19 C24 C28 C30 -127.9(8) . . . . ? Pd1 O2 C31 O3 -21.1(11) . . . . ? Pd1 O2 C31 C32 159.0(5) . . . . ? N1A Pd1A O1A C1A -12.4(6) . . . . ? O2A Pd1A O1A C1A 166.5(6) . . . . ? O1A Pd1A O2A C31A 73.3(5) . . . . ? N2A Pd1A O2A C31A -108.2(5) . . . . ? O1A Pd1A N1A C13A -1.4(6) . . . . ? N2A Pd1A N1A C13A -179.9(7) . . . . ? O1A Pd1A N1A C17A -175.5(5) . . . . ? N2A Pd1A N1A C17A 6.0(5) . . . . ? N1A Pd1A N2A C18A -5.2(5) . . . . ? O2A Pd1A N2A C18A 175.8(5) . . . . ? N1A Pd1A N2A C19A 173.4(6) . . . . ? O2A Pd1A N2A C19A -5.6(6) . . . . ? Pd1A O1A C1A C6A -165.2(5) . . . . ? Pd1A O1A C1A C2A 17.5(11) . . . . ? O1A C1A C2A C3A 176.0(7) . . . . ? C6A C1A C2A C3A -1.1(11) . . . . ? O1A C1A C2A C13A -6.1(13) . . . . ? C6A C1A C2A C13A 176.8(7) . . . . ? C1A C2A C3A C4A 1.3(12) . . . . ? C13A C2A C3A C4A -176.7(8) . . . . ? C2A C3A C4A C5A -2.2(13) . . . . ? C3A C4A C5A C6A 3.0(13) . . . . ? C4A C5A C6A C1A -2.8(12) . . . . ? C4A C5A C6A C7A -179.6(8) . . . . ? O1A C1A C6A C5A -175.6(7) . . . . ? C2A C1A C6A C5A 1.9(11) . . . . ? O1A C1A C6A C7A 1.2(11) . . . . ? C2A C1A C6A C7A 178.7(7) . . . . ? C5A C6A C7A C12A -132.9(9) . . . . ? C1A C6A C7A C12A 50.4(12) . . . . ? C5A C6A C7A C8A 42.5(12) . . . . ? C1A C6A C7A C8A -134.3(8) . . . . ? C12A C7A C8A C9A -3.5(13) . . . . ? C6A C7A C8A C9A -179.0(8) . . . . ? C7A C8A C9A C10A 1.9(13) . . . . ? C8A C9A C10A C11A 1.0(14) . . . . ? C9A C10A C11A C12A -2.3(15) . . . . ? C8A C7A C12A C11A 2.1(13) . . . . ? C6A C7A C12A C11A 177.6(8) . . . . ? C10A C11A C12A C7A 0.7(15) . . . . ? C17A N1A C13A C14A 3.3(11) . . . . ? Pd1A N1A C13A C14A -170.4(5) . . . . ? C17A N1A C13A C2A -175.6(7) . . . . ? Pd1A N1A C13A C2A 10.7(10) . . . . ? C3A C2A C13A N1A 169.1(7) . . . . ? C1A C2A C13A N1A -8.8(11) . . . . ? C3A C2A C13A C14A -9.8(11) . . . . ? C1A C2A C13A C14A 172.3(7) . . . . ? N1A C13A C14A C15A -3.0(11) . . . . ? C2A C13A C14A C15A 175.9(7) . . . . ? C13A C14A C15A C16A 0.0(12) . . . . ? C14A C15A C16A C17A 2.6(12) . . . . ? C15A C16A C17A N1A -2.3(12) . . . . ? C15A C16A C17A C18A 177.7(7) . . . . ? C13A N1A C17A C16A -0.6(11) . . . . ? Pd1A N1A C17A C16A 174.1(6) . . . . ? C13A N1A C17A C18A 179.4(6) . . . . ? Pd1A N1A C17A C18A -5.8(8) . . . . ? C19A N2A C18A C17A -175.3(7) . . . . ? Pd1A N2A C18A C17A 3.4(9) . . . . ? C16A C17A C18A N2A -178.3(7) . . . . ? N1A C17A C18A N2A 1.7(10) . . . . ? C18A N2A C19A C24A 94.0(9) . . . . ? Pd1A N2A C19A C24A -84.5(8) . . . . ? C18A N2A C19A C20A -86.9(9) . . . . ? Pd1A N2A C19A C20A 94.6(8) . . . . ? C24A C19A C20A C21A -1.3(12) . . . . ? N2A C19A C20A C21A 179.6(7) . . . . ? C24A C19A C20A C25A 179.9(7) . . . . ? N2A C19A C20A C25A 0.9(11) . . . . ? C19A C20A C21A C22A -0.1(12) . . . . ? C25A C20A C21A C22A 178.7(8) . . . . ? C20A C21A C22A C23A -0.1(13) . . . . ? C21A C22A C23A C24A 1.6(14) . . . . ? C20A C19A C24A C23A 2.7(12) . . . . ? N2A C19A C24A C23A -178.2(7) . . . . ? C20A C19A C24A C28A 178.4(8) . . . . ? N2A C19A C24A C28A -2.6(11) . . . . ? C22A C23A C24A C19A -2.8(12) . . . . ? C22A C23A C24A C28A -178.6(8) . . . . ? C21A C20A C25A C26A -72.5(10) . . . . ? C19A C20A C25A C26A 106.2(9) . . . . ? C21A C20A C25A C27A 48.3(11) . . . . ? C19A C20A C25A C27A -132.9(8) . . . . ? C19A C24A C28A C29A 151.9(8) . . . . ? C23A C24A C28A C29A -32.5(11) . . . . ? C19A C24A C28A C30A -85.6(10) . . . . ? C23A C24A C28A C30A 89.9(9) . . . . ? Pd1A O2A C31A O3A 6.8(11) . . . . ? Pd1A O2A C31A C32A -172.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.740 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.123 data_10001 _database_code_depnum_ccdc_archive 'CCDC 919246' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 N2 O3 Pd, C H2 Cl2' _chemical_formula_sum 'C33 H36 Cl2 N2 O3 Pd' _chemical_formula_weight 685.94 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.471(3) _cell_length_b 14.913(3) _cell_length_c 16.595(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.732(4) _cell_angle_gamma 90.00 _cell_volume 3157.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 736 _cell_measurement_theta_min 2.724 _cell_measurement_theta_max 25.817 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 0.802 _exptl_absorpt_process_details ; aborption correction based on 4074 reflections(SADABS);Rint 0.1438 before correction and 0.0600 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24097 _diffrn_reflns_av_R_equivalents 0.1722 _diffrn_reflns_av_sigmaI/netI 0.1923 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6204 _reflns_number_gt 3294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0199P)^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 6204 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.45538(3) 0.94864(3) 0.56889(3) 0.02789(14) Uani 1 1 d . . . O1 O 0.6064(3) 0.9248(3) 0.6291(2) 0.0352(11) Uani 1 1 d . . . O2 O 0.4523(3) 0.8437(3) 0.4912(2) 0.0346(11) Uani 1 1 d . . . O3 O 0.3871(4) 0.7577(3) 0.5711(3) 0.0526(13) Uani 1 1 d . . . N1 N 0.4610(4) 1.0552(3) 0.6389(3) 0.0338(12) Uani 1 1 d . . . N2 N 0.3056(3) 0.9933(3) 0.5013(3) 0.0286(12) Uani 1 1 d . . . H2 H 0.3171 0.9971 0.4605 0.034 Uiso 1 1 d R . . C1 C 0.6433(5) 0.9333(4) 0.7126(4) 0.0349(16) Uani 1 1 d . . . C2 C 0.6101(5) 1.0005(4) 0.7571(4) 0.0387(17) Uani 1 1 d . . . C3 C 0.6572(6) 1.0026(5) 0.8472(4) 0.052(2) Uani 1 1 d . . . H3 H 0.6333 1.0449 0.8796 0.062 Uiso 1 1 calc R . . C4 C 0.7365(6) 0.9446(6) 0.8881(4) 0.059(2) Uani 1 1 d . . . H4 H 0.7672 0.9476 0.9482 0.071 Uiso 1 1 calc R . . C5 C 0.7715(5) 0.8826(5) 0.8431(5) 0.053(2) Uani 1 1 d . . . H5 H 0.8283 0.8448 0.8725 0.064 Uiso 1 1 calc R . . C6 C 0.7272(5) 0.8730(4) 0.7565(4) 0.0403(18) Uani 1 1 d . . . C7 C 0.7659(5) 0.8056(4) 0.7086(4) 0.0376(17) Uani 1 1 d . . . C8 C 0.8741(5) 0.7986(5) 0.7205(5) 0.061(2) Uani 1 1 d . . . H8 H 0.9222 0.8355 0.7615 0.074 Uiso 1 1 calc R . . C9 C 0.9103(6) 0.7394(5) 0.6737(6) 0.074(3) Uani 1 1 d . . . H9 H 0.9832 0.7373 0.6814 0.089 Uiso 1 1 calc R . . C10 C 0.8445(6) 0.6832(5) 0.6161(6) 0.069(3) Uani 1 1 d . . . H10 H 0.8712 0.6417 0.5848 0.083 Uiso 1 1 calc R . . C11 C 0.7382(6) 0.6873(5) 0.6040(5) 0.051(2) Uani 1 1 d . . . H11 H 0.6916 0.6483 0.5642 0.062 Uiso 1 1 calc R . . C12 C 0.6989(5) 0.7482(4) 0.6495(4) 0.0434(18) Uani 1 1 d . . . H12 H 0.6256 0.7507 0.6402 0.052 Uiso 1 1 calc R . . C13 C 0.5348(5) 1.0720(4) 0.7156(4) 0.0358(17) Uani 1 1 d . . . C14 C 0.5372(5) 1.1547(5) 0.7540(4) 0.0458(19) Uani 1 1 d . . . H14 H 0.5905 1.1677 0.8061 0.055 Uiso 1 1 calc R . . C15 C 0.4619(6) 1.2186(5) 0.7164(5) 0.056(2) Uani 1 1 d . . . H15 H 0.4640 1.2755 0.7426 0.068 Uiso 1 1 calc R . . C16 C 0.3846(5) 1.1999(4) 0.6417(5) 0.0447(19) Uani 1 1 d . . . H16 H 0.3312 1.2423 0.6161 0.054 Uiso 1 1 calc R . . C17 C 0.3869(5) 1.1167(4) 0.6047(4) 0.0330(16) Uani 1 1 d . . . C18 C 0.3059(5) 1.0916(4) 0.5222(4) 0.0356(17) Uani 1 1 d . . . H18A H 0.3186 1.1266 0.4757 0.043 Uiso 1 1 calc R . . H18B H 0.2358 1.1083 0.5246 0.043 Uiso 1 1 calc R . . C19 C 0.2074(4) 0.9473(4) 0.4979(4) 0.0295(14) Uani 1 1 d . . . C20 C 0.1349(4) 0.9283(4) 0.4170(4) 0.0333(16) Uani 1 1 d . . . C21 C 0.0407(5) 0.8893(4) 0.4148(4) 0.0401(18) Uani 1 1 d . . . H21 H -0.0087 0.8748 0.3611 0.048 Uiso 1 1 calc R . . C22 C 0.0159(5) 0.8710(4) 0.4866(5) 0.0439(19) Uani 1 1 d . . . H22 H -0.0502 0.8455 0.4823 0.053 Uiso 1 1 calc R . . C23 C 0.0881(5) 0.8897(4) 0.5666(4) 0.0405(18) Uani 1 1 d . . . H23 H 0.0704 0.8770 0.6164 0.049 Uiso 1 1 calc R . . C24 C 0.1860(4) 0.9268(4) 0.5742(4) 0.0312(16) Uani 1 1 d . . . C25 C 0.1586(4) 0.9468(4) 0.3352(3) 0.0369(15) Uani 1 1 d . . . H25 H 0.2071 0.9994 0.3454 0.044 Uiso 1 1 calc R . . C26 C 0.0604(4) 0.9703(4) 0.2602(4) 0.0418(18) Uani 1 1 d . . . H26A H 0.0153 0.9173 0.2442 0.063 Uiso 1 1 calc R . . H26B H 0.0814 0.9899 0.2117 0.063 Uiso 1 1 calc R . . H26C H 0.0219 1.0187 0.2771 0.063 Uiso 1 1 calc R . . C27 C 0.2151(5) 0.8668(4) 0.3124(4) 0.0482(19) Uani 1 1 d . . . H27A H 0.1729 0.8126 0.3088 0.072 Uiso 1 1 calc R . . H27B H 0.2834 0.8589 0.3564 0.072 Uiso 1 1 calc R . . H27C H 0.2255 0.8777 0.2574 0.072 Uiso 1 1 calc R . . C28 C 0.2618(5) 0.9399(5) 0.6623(4) 0.0438(17) Uani 1 1 d . . . H28 H 0.3315 0.9551 0.6565 0.053 Uiso 1 1 calc R . . C29 C 0.2307(5) 1.0166(4) 0.7094(4) 0.060(2) Uani 1 1 d . . . H29A H 0.2233 1.0717 0.6758 0.090 Uiso 1 1 calc R . . H29B H 0.2849 1.0251 0.7647 0.090 Uiso 1 1 calc R . . H29C H 0.1638 1.0026 0.7181 0.090 Uiso 1 1 calc R . . C30 C 0.2757(5) 0.8547(5) 0.7157(4) 0.059(2) Uani 1 1 d . . . H30A H 0.2129 0.8446 0.7321 0.088 Uiso 1 1 calc R . . H30B H 0.3368 0.8612 0.7670 0.088 Uiso 1 1 calc R . . H30C H 0.2863 0.8035 0.6824 0.088 Uiso 1 1 calc R . . C31 C 0.4229(5) 0.7703(5) 0.5131(4) 0.0309(16) Uani 1 1 d . . . C32 C 0.4329(5) 0.6900(4) 0.4585(4) 0.053(2) Uani 1 1 d . . . H32A H 0.4444 0.6352 0.4929 0.080 Uiso 1 1 calc R . . H32B H 0.4923 0.6995 0.4376 0.080 Uiso 1 1 calc R . . H32C H 0.3684 0.6839 0.4101 0.080 Uiso 1 1 calc R . . C33 C 0.1524(5) 0.6669(5) 0.4879(5) 0.062(2) Uani 1 1 d . . . H33A H 0.2245 0.6675 0.5288 0.074 Uiso 1 1 calc R . . H33B H 0.1336 0.7293 0.4686 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.14996(18) 0.60122(16) 0.40113(14) 0.0906(8) Uani 1 1 d . . . Cl2 Cl 0.0673(2) 0.62885(15) 0.53898(17) 0.1021(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0208(2) 0.0351(3) 0.0252(3) -0.0028(3) 0.00399(18) 0.0022(3) O1 0.022(2) 0.054(3) 0.025(2) -0.003(2) 0.0007(19) 0.004(2) O2 0.027(3) 0.038(3) 0.036(3) 0.000(2) 0.005(2) 0.004(2) O3 0.069(4) 0.053(3) 0.039(3) 0.001(3) 0.022(3) -0.006(3) N1 0.029(3) 0.037(3) 0.034(3) -0.004(3) 0.008(2) 0.001(3) N2 0.022(3) 0.036(3) 0.029(3) 0.003(3) 0.009(2) 0.001(2) C1 0.028(4) 0.046(5) 0.028(4) -0.001(3) 0.005(3) -0.015(3) C2 0.043(4) 0.046(4) 0.024(4) -0.003(3) 0.005(3) -0.019(4) C3 0.052(5) 0.066(5) 0.036(5) -0.011(4) 0.013(4) -0.035(4) C4 0.058(5) 0.074(6) 0.030(4) 0.001(5) -0.009(4) -0.030(5) C5 0.043(5) 0.058(5) 0.038(5) 0.013(4) -0.018(4) -0.018(4) C6 0.036(4) 0.043(4) 0.033(4) 0.009(4) 0.000(3) -0.016(3) C7 0.030(4) 0.033(4) 0.042(4) 0.015(3) 0.001(3) 0.006(3) C8 0.033(5) 0.042(5) 0.095(7) 0.019(5) 0.001(5) 0.005(4) C9 0.033(5) 0.043(5) 0.136(9) 0.018(5) 0.011(5) 0.014(4) C10 0.054(6) 0.060(6) 0.103(8) 0.021(5) 0.038(6) 0.016(5) C11 0.044(5) 0.049(5) 0.054(5) 0.008(4) 0.008(4) 0.008(4) C12 0.036(4) 0.047(5) 0.038(4) 0.015(4) -0.001(4) -0.001(4) C13 0.035(4) 0.043(5) 0.036(4) -0.007(3) 0.020(3) -0.014(3) C14 0.044(5) 0.058(5) 0.041(5) -0.020(4) 0.022(4) -0.015(4) C15 0.059(6) 0.049(5) 0.081(6) -0.027(5) 0.050(5) -0.015(4) C16 0.040(5) 0.037(4) 0.063(5) -0.007(4) 0.025(4) 0.002(4) C17 0.033(4) 0.035(4) 0.035(4) -0.006(3) 0.017(3) 0.003(3) C18 0.035(4) 0.031(4) 0.048(5) 0.004(3) 0.024(4) 0.001(3) C19 0.023(3) 0.033(3) 0.032(4) 0.009(4) 0.008(3) 0.009(3) C20 0.021(3) 0.030(4) 0.047(4) 0.010(3) 0.008(3) 0.004(3) C21 0.025(4) 0.047(4) 0.045(5) 0.004(3) 0.007(4) -0.001(3) C22 0.020(4) 0.047(4) 0.066(5) 0.006(4) 0.016(4) -0.002(3) C23 0.032(4) 0.045(4) 0.053(5) 0.013(4) 0.025(4) 0.007(3) C24 0.022(3) 0.026(4) 0.045(4) 0.008(3) 0.010(3) 0.013(3) C25 0.029(3) 0.049(4) 0.029(4) 0.011(4) 0.002(3) -0.007(4) C26 0.040(4) 0.037(4) 0.042(4) 0.004(3) 0.005(3) -0.006(3) C27 0.032(4) 0.066(5) 0.048(5) 0.009(4) 0.015(4) 0.007(4) C28 0.036(4) 0.055(5) 0.041(4) 0.007(4) 0.013(3) 0.003(4) C29 0.057(5) 0.074(6) 0.042(5) -0.010(4) 0.005(4) 0.000(4) C30 0.061(5) 0.079(6) 0.037(5) 0.013(4) 0.017(4) 0.018(4) C31 0.022(4) 0.045(5) 0.022(4) -0.002(3) 0.000(3) 0.004(3) C32 0.058(5) 0.045(5) 0.057(5) -0.002(4) 0.019(4) -0.007(4) C33 0.057(5) 0.051(5) 0.079(6) 0.002(4) 0.024(5) 0.005(4) Cl1 0.0888(18) 0.116(2) 0.0594(15) -0.0214(14) 0.0135(13) -0.0085(15) Cl2 0.107(2) 0.0933(18) 0.137(2) 0.0348(17) 0.0818(19) 0.0254(15) _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 N1 1.955(5) . ? Pd1 O1 1.990(4) . ? Pd1 O2 2.019(4) . ? Pd1 N2 2.078(4) . ? O1 C1 1.319(6) . ? O2 C31 1.257(7) . ? O3 C31 1.221(7) . ? N1 C17 1.340(7) . ? N1 C13 1.364(7) . ? N2 C19 1.476(7) . ? N2 C18 1.505(6) . ? N2 H2 0.7442 . ? C1 C2 1.401(8) . ? C1 C6 1.445(8) . ? C2 C3 1.424(8) . ? C2 C13 1.480(8) . ? C3 C4 1.373(9) . ? C3 H3 0.9500 . ? C4 C5 1.364(9) . ? C4 H4 0.9500 . ? C5 C6 1.375(8) . ? C5 H5 0.9500 . ? C6 C7 1.477(8) . ? C7 C12 1.393(8) . ? C7 C8 1.410(8) . ? C8 C9 1.366(10) . ? C8 H8 0.9500 . ? C9 C10 1.363(10) . ? C9 H9 0.9500 . ? C10 C11 1.381(9) . ? C10 H10 0.9500 . ? C11 C12 1.390(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.383(8) . ? C14 C15 1.385(8) . ? C14 H14 0.9500 . ? C15 C16 1.367(9) . ? C15 H15 0.9500 . ? C16 C17 1.389(8) . ? C16 H16 0.9500 . ? C17 C18 1.500(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.411(7) . ? C19 C24 1.418(7) . ? C20 C21 1.386(7) . ? C20 C25 1.516(8) . ? C21 C22 1.364(8) . ? C21 H21 0.9500 . ? C22 C23 1.399(8) . ? C22 H22 0.9500 . ? C23 C24 1.398(7) . ? C23 H23 0.9500 . ? C24 C28 1.504(8) . ? C25 C27 1.527(8) . ? C25 C26 1.537(7) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.519(8) . ? C28 C30 1.526(8) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.534(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Cl2 1.727(7) . ? C33 Cl1 1.733(7) . ? C33 H33A 0.9900 . ? C33 H33B 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 N1 Pd1 O1 90.48(18) . . ? N1 Pd1 O2 176.25(19) . . ? O1 Pd1 O2 89.43(15) . . ? N1 Pd1 N2 84.59(19) . . ? O1 Pd1 N2 170.82(17) . . ? O2 Pd1 N2 94.99(17) . . ? C1 O1 Pd1 119.3(4) . . ? C31 O2 Pd1 115.7(4) . . ? C17 N1 C13 119.3(6) . . ? C17 N1 Pd1 115.1(4) . . ? C13 N1 Pd1 125.6(4) . . ? C19 N2 C18 113.5(5) . . ? C19 N2 Pd1 125.1(3) . . ? C18 N2 Pd1 104.9(4) . . ? C19 N2 H2 116.5 . . ? C18 N2 H2 98.7 . . ? Pd1 N2 H2 93.7 . . ? O1 C1 C2 123.1(6) . . ? O1 C1 C6 116.1(6) . . ? C2 C1 C6 120.6(6) . . ? C1 C2 C3 117.3(6) . . ? C1 C2 C13 123.9(6) . . ? C3 C2 C13 118.7(6) . . ? C4 C3 C2 121.3(7) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 122.2(7) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 118.0(7) . . ? C5 C6 C7 121.5(7) . . ? C1 C6 C7 120.5(6) . . ? C12 C7 C8 117.4(7) . . ? C12 C7 C6 122.4(6) . . ? C8 C7 C6 120.2(7) . . ? C9 C8 C7 120.7(8) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 121.7(8) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 119.0(8) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 120.5(7) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.6(7) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? N1 C13 C14 119.8(6) . . ? N1 C13 C2 119.1(6) . . ? C14 C13 C2 121.1(6) . . ? C13 C14 C15 120.0(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.2(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 117.6(7) . . ? C15 C16 H16 121.2 . . ? C17 C16 H16 121.2 . . ? N1 C17 C16 123.0(6) . . ? N1 C17 C18 116.1(5) . . ? C16 C17 C18 120.9(6) . . ? C17 C18 N2 113.6(5) . . ? C17 C18 H18A 108.8 . . ? N2 C18 H18A 108.8 . . ? C17 C18 H18B 108.8 . . ? N2 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C24 121.9(5) . . ? C20 C19 N2 117.9(5) . . ? C24 C19 N2 120.1(5) . . ? C21 C20 C19 117.2(6) . . ? C21 C20 C25 120.4(6) . . ? C19 C20 C25 122.3(5) . . ? C22 C21 C20 122.7(6) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.8(6) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C19 117.4(6) . . ? C23 C24 C28 117.7(6) . . ? C19 C24 C28 124.9(5) . . ? C20 C25 C27 110.2(5) . . ? C20 C25 C26 113.1(5) . . ? C27 C25 C26 110.2(5) . . ? C20 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 112.6(5) . . ? C24 C28 C30 112.0(6) . . ? C29 C28 C30 109.3(5) . . ? C24 C28 H28 107.5 . . ? C29 C28 H28 107.5 . . ? C30 C28 H28 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 O2 127.1(6) . . ? O3 C31 C32 118.5(6) . . ? O2 C31 C32 114.4(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl2 C33 Cl1 112.6(4) . . ? Cl2 C33 H33A 109.1 . . ? Cl1 C33 H33A 109.1 . . ? Cl2 C33 H33B 109.1 . . ? Cl1 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? 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 N1 Pd1 O1 C1 43.2(4) . . . . ? O2 Pd1 O1 C1 -140.5(4) . . . . ? O1 Pd1 O2 C31 94.5(4) . . . . ? N2 Pd1 O2 C31 -93.5(4) . . . . ? O1 Pd1 N1 C17 157.0(4) . . . . ? N2 Pd1 N1 C17 -15.3(4) . . . . ? O1 Pd1 N1 C13 -20.5(5) . . . . ? N2 Pd1 N1 C13 167.3(5) . . . . ? N1 Pd1 N2 C19 -113.1(5) . . . . ? O2 Pd1 N2 C19 70.7(5) . . . . ? N1 Pd1 N2 C18 20.7(3) . . . . ? O2 Pd1 N2 C18 -155.6(3) . . . . ? Pd1 O1 C1 C2 -37.6(7) . . . . ? Pd1 O1 C1 C6 147.0(4) . . . . ? O1 C1 C2 C3 -179.4(5) . . . . ? C6 C1 C2 C3 -4.1(9) . . . . ? O1 C1 C2 C13 -3.5(10) . . . . ? C6 C1 C2 C13 171.7(5) . . . . ? C1 C2 C3 C4 3.9(9) . . . . ? C13 C2 C3 C4 -172.2(6) . . . . ? C2 C3 C4 C5 -0.7(11) . . . . ? C3 C4 C5 C6 -2.5(11) . . . . ? C4 C5 C6 C1 2.2(10) . . . . ? C4 C5 C6 C7 180.0(6) . . . . ? O1 C1 C6 C5 176.8(5) . . . . ? C2 C1 C6 C5 1.2(9) . . . . ? O1 C1 C6 C7 -1.0(8) . . . . ? C2 C1 C6 C7 -176.6(6) . . . . ? C5 C6 C7 C12 132.4(7) . . . . ? C1 C6 C7 C12 -49.9(9) . . . . ? C5 C6 C7 C8 -48.9(9) . . . . ? C1 C6 C7 C8 128.8(7) . . . . ? C12 C7 C8 C9 1.8(10) . . . . ? C6 C7 C8 C9 -176.9(7) . . . . ? C7 C8 C9 C10 -2.1(12) . . . . ? C8 C9 C10 C11 1.0(12) . . . . ? C9 C10 C11 C12 0.3(11) . . . . ? C10 C11 C12 C7 -0.5(10) . . . . ? C8 C7 C12 C11 -0.5(9) . . . . ? C6 C7 C12 C11 178.2(6) . . . . ? C17 N1 C13 C14 -5.0(8) . . . . ? Pd1 N1 C13 C14 172.4(4) . . . . ? C17 N1 C13 C2 174.0(5) . . . . ? Pd1 N1 C13 C2 -8.6(8) . . . . ? C1 C2 C13 N1 28.9(9) . . . . ? C3 C2 C13 N1 -155.2(5) . . . . ? C1 C2 C13 C14 -152.1(6) . . . . ? C3 C2 C13 C14 23.8(9) . . . . ? N1 C13 C14 C15 3.0(9) . . . . ? C2 C13 C14 C15 -176.0(6) . . . . ? C13 C14 C15 C16 0.5(10) . . . . ? C14 C15 C16 C17 -1.9(10) . . . . ? C13 N1 C17 C16 3.6(9) . . . . ? Pd1 N1 C17 C16 -174.0(5) . . . . ? C13 N1 C17 C18 -177.4(5) . . . . ? Pd1 N1 C17 C18 5.0(7) . . . . ? C15 C16 C17 N1 -0.1(10) . . . . ? C15 C16 C17 C18 -179.1(6) . . . . ? N1 C17 C18 N2 13.9(8) . . . . ? C16 C17 C18 N2 -167.1(5) . . . . ? C19 N2 C18 C17 116.3(5) . . . . ? Pd1 N2 C18 C17 -23.5(6) . . . . ? C18 N2 C19 C20 102.6(6) . . . . ? Pd1 N2 C19 C20 -127.0(5) . . . . ? C18 N2 C19 C24 -74.7(7) . . . . ? Pd1 N2 C19 C24 55.7(7) . . . . ? C24 C19 C20 C21 0.6(9) . . . . ? N2 C19 C20 C21 -176.7(5) . . . . ? C24 C19 C20 C25 -177.7(5) . . . . ? N2 C19 C20 C25 5.0(8) . . . . ? C19 C20 C21 C22 1.3(9) . . . . ? C25 C20 C21 C22 179.6(6) . . . . ? C20 C21 C22 C23 -1.5(10) . . . . ? C21 C22 C23 C24 -0.3(10) . . . . ? C22 C23 C24 C19 2.0(9) . . . . ? C22 C23 C24 C28 -176.4(6) . . . . ? C20 C19 C24 C23 -2.2(9) . . . . ? N2 C19 C24 C23 175.0(5) . . . . ? C20 C19 C24 C28 176.1(6) . . . . ? N2 C19 C24 C28 -6.7(9) . . . . ? C21 C20 C25 C27 -91.2(6) . . . . ? C19 C20 C25 C27 87.1(7) . . . . ? C21 C20 C25 C26 32.7(8) . . . . ? C19 C20 C25 C26 -149.1(6) . . . . ? C23 C24 C28 C29 -72.7(7) . . . . ? C19 C24 C28 C29 108.9(7) . . . . ? C23 C24 C28 C30 51.0(7) . . . . ? C19 C24 C28 C30 -127.3(6) . . . . ? Pd1 O2 C31 O3 7.3(8) . . . . ? Pd1 O2 C31 C32 -173.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O1 0.74 2.37 3.037(6) 150.2 3_676 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.546 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.101 data_10016 _database_code_depnum_ccdc_archive 'CCDC 919247' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: ...Due to the Squeeze option in Platon,reported sum formula does not agree with the calculated sum formula. 'see_platon_squeeze_details' ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 Cl N2 O Pd ,C9 H21,H2 O' _chemical_formula_sum 'C39 H54 Cl N2 O2 Pd' _chemical_formula_weight 724.69 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' 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 10.5900(16) _cell_length_b 10.9142(16) _cell_length_c 14.160(2) _cell_angle_alpha 92.595(3) _cell_angle_beta 95.184(3) _cell_angle_gamma 105.297(3) _cell_volume 1568.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 663 _cell_measurement_theta_min 2.336 _cell_measurement_theta_max 23.280 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 3620 reflections(SADABS);Rint 0.1385 before correction and 0.0480 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12345 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.1607 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6069 _reflns_number_gt 3959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0424P)^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 6069 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.001 0.500 0.000 377 169 ' ' _platon_squeeze_details ; Disordered C6H14 and H2O were omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 380.1 3 with an estimated 169e/cell to be added. Three solvent C6H14 and two H2O molecules/unit cell accounting for 169e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. ; 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 0.96438(4) 0.85194(4) 0.52445(3) 0.02224(14) Uani 1 1 d . . . Cl1 Cl 1.18222(13) 0.85959(13) 0.51716(10) 0.0285(3) Uani 1 1 d . . . O1 O 1.0004(4) 0.9303(3) 0.6580(3) 0.0275(9) Uani 1 1 d . . . N1 N 0.7744(4) 0.8350(4) 0.5256(3) 0.0275(11) Uani 1 1 d . . . N2 N 0.9162(4) 0.7983(4) 0.3817(3) 0.0247(11) Uani 1 1 d . . . H2 H 0.9666 0.8967 0.3779 0.030 Uiso 1 1 d R . . C1 C 0.9234(6) 0.8720(5) 0.7186(4) 0.0320(14) Uani 1 1 d . . . C2 C 0.7834(6) 0.8257(5) 0.6991(4) 0.0340(15) Uani 1 1 d . . . C3 C 0.7082(7) 0.7677(6) 0.7698(5) 0.0474(18) Uani 1 1 d . . . H3 H 0.6152 0.7376 0.7564 0.057 Uiso 1 1 calc R . . C4 C 0.7666(8) 0.7538(6) 0.8577(5) 0.053(2) Uani 1 1 d . . . H4 H 0.7138 0.7125 0.9039 0.063 Uiso 1 1 calc R . . C5 C 0.9010(7) 0.7991(6) 0.8801(5) 0.0463(18) Uani 1 1 d . . . H5 H 0.9392 0.7898 0.9418 0.056 Uiso 1 1 calc R . . C6 C 0.9823(6) 0.8586(6) 0.8131(4) 0.0370(16) Uani 1 1 d . . . C7 C 1.1264(6) 0.9123(6) 0.8370(4) 0.0352(15) Uani 1 1 d . . . C8 C 1.1740(7) 0.9798(6) 0.9239(5) 0.0465(18) Uani 1 1 d . . . H8 H 1.1132 0.9918 0.9665 0.056 Uiso 1 1 calc R . . C9 C 1.3064(8) 1.0298(8) 0.9504(5) 0.062(2) Uani 1 1 d . . . H9 H 1.3370 1.0756 1.0103 0.075 Uiso 1 1 calc R . . C10 C 1.3946(8) 1.0120(7) 0.8878(5) 0.064(2) Uani 1 1 d . . . H10 H 1.4864 1.0465 0.9052 0.077 Uiso 1 1 calc R . . C11 C 1.3517(7) 0.9456(7) 0.8014(5) 0.054(2) Uani 1 1 d . . . H11 H 1.4128 0.9334 0.7591 0.065 Uiso 1 1 calc R . . C12 C 1.2170(7) 0.8964(6) 0.7767(4) 0.0428(17) Uani 1 1 d . . . H12 H 1.1866 0.8507 0.7167 0.051 Uiso 1 1 calc R . . C13 C 0.7151(6) 0.8380(5) 0.6061(5) 0.0327(15) Uani 1 1 d . . . C14 C 0.5842(6) 0.8475(6) 0.5980(5) 0.0417(17) Uani 1 1 d . . . H14 H 0.5418 0.8552 0.6534 0.050 Uiso 1 1 calc R . . C15 C 0.5181(6) 0.8454(6) 0.5090(6) 0.0473(19) Uani 1 1 d . . . H15 H 0.4301 0.8519 0.5035 0.057 Uiso 1 1 calc R . . C16 C 0.5785(6) 0.8342(5) 0.4283(5) 0.0381(16) Uani 1 1 d . . . H16 H 0.5327 0.8290 0.3667 0.046 Uiso 1 1 calc R . . C17 C 0.7085(5) 0.8307(5) 0.4403(4) 0.0291(14) Uani 1 1 d . . . C18 C 0.7821(5) 0.8181(5) 0.3550(4) 0.0312(14) Uani 1 1 d . . . H18A H 0.7291 0.7453 0.3118 0.037 Uiso 1 1 calc R . . H18B H 0.7926 0.8960 0.3200 0.037 Uiso 1 1 calc R . . C19 C 0.9396(6) 0.6824(5) 0.3429(4) 0.0306(14) Uani 1 1 d . . . C20 C 1.0410(6) 0.6913(5) 0.2859(4) 0.0301(14) Uani 1 1 d . . . C21 C 1.0630(7) 0.5778(6) 0.2483(5) 0.0476(18) Uani 1 1 d . . . H21 H 1.1321 0.5826 0.2091 0.057 Uiso 1 1 calc R . . C22 C 0.9884(8) 0.4633(7) 0.2665(6) 0.073(3) Uani 1 1 d . . . H22 H 1.0039 0.3879 0.2395 0.088 Uiso 1 1 calc R . . C23 C 0.8884(8) 0.4551(7) 0.3252(5) 0.066(2) Uani 1 1 d . . . H23 H 0.8367 0.3734 0.3378 0.079 Uiso 1 1 calc R . . C24 C 0.8615(6) 0.5622(5) 0.3659(4) 0.0384(16) Uani 1 1 d . . . C25 C 1.1261(5) 0.8174(5) 0.2577(4) 0.0311(14) Uani 1 1 d . . . H25 H 1.1157 0.8862 0.3030 0.037 Uiso 1 1 calc R . . C26 C 1.0788(7) 0.8452(7) 0.1579(5) 0.061(2) Uani 1 1 d . . . H26A H 1.0806 0.7754 0.1125 0.092 Uiso 1 1 calc R . . H26B H 1.1368 0.9249 0.1404 0.092 Uiso 1 1 calc R . . H26C H 0.9887 0.8532 0.1568 0.092 Uiso 1 1 calc R . . C27 C 1.2721(6) 0.8211(7) 0.2665(5) 0.060(2) Uani 1 1 d . . . H27A H 1.2962 0.7902 0.3277 0.091 Uiso 1 1 calc R . . H27B H 1.3251 0.9088 0.2628 0.091 Uiso 1 1 calc R . . H27C H 1.2885 0.7666 0.2147 0.091 Uiso 1 1 calc R . . C28 C 0.7544(7) 0.5433(6) 0.4312(5) 0.0498(19) Uani 1 1 d . . . H28 H 0.7463 0.6300 0.4504 0.060 Uiso 1 1 calc R . . C29 C 0.6192(8) 0.4682(8) 0.3800(7) 0.107(4) Uani 1 1 d . . . H29A H 0.6042 0.5038 0.3190 0.161 Uiso 1 1 calc R . . H29B H 0.5497 0.4745 0.4197 0.161 Uiso 1 1 calc R . . H29C H 0.6179 0.3786 0.3689 0.161 Uiso 1 1 calc R . . C30 C 0.7907(9) 0.4853(8) 0.5229(6) 0.096(3) Uani 1 1 d . . . H30A H 0.8085 0.4035 0.5071 0.143 Uiso 1 1 calc R . . H30B H 0.7175 0.4719 0.5623 0.143 Uiso 1 1 calc R . . H30C H 0.8694 0.5434 0.5579 0.143 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 0.0198(2) 0.0180(2) 0.0293(3) 0.00276(17) 0.00457(18) 0.00481(17) Cl1 0.0199(7) 0.0300(8) 0.0373(9) 0.0050(7) 0.0050(6) 0.0086(6) O1 0.029(2) 0.021(2) 0.032(2) 0.0031(17) 0.0089(19) 0.0040(17) N1 0.024(3) 0.027(3) 0.033(3) 0.004(2) 0.006(2) 0.009(2) N2 0.025(3) 0.015(2) 0.032(3) 0.002(2) -0.001(2) 0.004(2) C1 0.037(4) 0.024(3) 0.037(4) -0.002(3) 0.011(3) 0.010(3) C2 0.044(4) 0.022(3) 0.035(4) -0.001(3) 0.011(3) 0.006(3) C3 0.047(4) 0.037(4) 0.053(5) 0.001(3) 0.019(4) -0.004(3) C4 0.071(6) 0.036(4) 0.046(5) 0.001(3) 0.036(4) -0.004(4) C5 0.076(6) 0.033(4) 0.034(4) 0.005(3) 0.026(4) 0.015(4) C6 0.047(4) 0.031(4) 0.039(4) 0.002(3) 0.013(3) 0.019(3) C7 0.049(4) 0.037(4) 0.027(3) 0.009(3) 0.007(3) 0.021(3) C8 0.060(5) 0.054(5) 0.034(4) 0.001(3) 0.003(4) 0.031(4) C9 0.066(6) 0.085(6) 0.040(4) -0.004(4) -0.012(4) 0.036(5) C10 0.056(5) 0.080(6) 0.056(5) -0.007(4) -0.017(4) 0.028(5) C11 0.044(5) 0.079(6) 0.048(5) -0.009(4) 0.009(4) 0.032(4) C12 0.061(5) 0.043(4) 0.032(4) -0.004(3) 0.003(3) 0.028(4) C13 0.029(4) 0.014(3) 0.054(4) 0.001(3) 0.019(3) -0.001(3) C14 0.028(4) 0.032(4) 0.066(5) -0.004(3) 0.024(4) 0.005(3) C15 0.018(3) 0.031(4) 0.092(6) 0.009(4) 0.011(4) 0.002(3) C16 0.020(3) 0.030(4) 0.059(5) -0.003(3) -0.002(3) 0.000(3) C17 0.026(3) 0.011(3) 0.052(4) 0.003(3) 0.007(3) 0.005(2) C18 0.019(3) 0.027(3) 0.041(4) 0.003(3) -0.002(3) -0.002(3) C19 0.040(4) 0.020(3) 0.035(4) 0.005(3) 0.006(3) 0.013(3) C20 0.035(4) 0.022(3) 0.031(3) -0.003(3) 0.003(3) 0.005(3) C21 0.066(5) 0.038(4) 0.046(4) 0.005(3) 0.028(4) 0.021(4) C22 0.113(7) 0.027(4) 0.089(6) 0.000(4) 0.047(6) 0.024(4) C23 0.100(7) 0.026(4) 0.069(5) -0.005(4) 0.034(5) 0.002(4) C24 0.052(4) 0.019(3) 0.044(4) -0.003(3) 0.015(3) 0.006(3) C25 0.031(3) 0.033(4) 0.030(3) -0.004(3) 0.007(3) 0.010(3) C26 0.084(6) 0.051(5) 0.052(5) 0.014(4) 0.003(4) 0.024(4) C27 0.033(4) 0.065(5) 0.083(6) -0.013(4) 0.011(4) 0.015(4) C28 0.063(5) 0.018(3) 0.062(5) -0.001(3) 0.019(4) -0.004(3) C29 0.079(7) 0.091(7) 0.123(8) -0.032(6) 0.051(6) -0.035(6) C30 0.144(9) 0.098(7) 0.084(7) 0.047(6) 0.067(7) 0.076(7) _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 N1 1.973(4) . ? Pd1 O1 2.001(4) . ? Pd1 N2 2.058(4) . ? Pd1 Cl1 2.2982(14) . ? Pd1 Pd1 3.2412(10) 2_776 ? Pd1 H2 2.1539 . ? O1 C1 1.307(6) . ? N1 C17 1.332(7) . ? N1 C13 1.353(7) . ? N2 C19 1.446(6) . ? N2 C18 1.510(7) . ? N2 H2 1.0721 . ? C1 C2 1.431(8) . ? C1 C6 1.454(8) . ? C2 C3 1.404(8) . ? C2 C13 1.474(8) . ? C3 C4 1.373(9) . ? C3 H3 0.9500 . ? C4 C5 1.380(9) . ? C4 H4 0.9500 . ? C5 C6 1.404(8) . ? C5 H5 0.9500 . ? C6 C7 1.485(8) . ? C7 C12 1.380(8) . ? C7 C8 1.386(8) . ? C8 C9 1.374(9) . ? C8 H8 0.9500 . ? C9 C10 1.387(10) . ? C9 H9 0.9500 . ? C10 C11 1.369(9) . ? C10 H10 0.9500 . ? C11 C12 1.391(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.412(8) . ? C14 C15 1.382(9) . ? C14 H14 0.9500 . ? C15 C16 1.375(8) . ? C15 H15 0.9500 . ? C16 C17 1.382(7) . ? C16 H16 0.9500 . ? C17 C18 1.515(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.387(8) . ? C19 C24 1.423(8) . ? C20 C21 1.410(8) . ? C20 C25 1.524(8) . ? C21 C22 1.341(9) . ? C21 H21 0.9500 . ? C22 C23 1.392(9) . ? C22 H22 0.9500 . ? C23 C24 1.387(8) . ? C23 H23 0.9500 . ? C24 C28 1.506(8) . ? C25 C26 1.527(8) . ? C25 C27 1.530(8) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.532(9) . ? C28 C29 1.545(10) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 O1 90.92(17) . . ? N1 Pd1 N2 84.59(18) . . ? O1 Pd1 N2 170.17(16) . . ? N1 Pd1 Cl1 176.34(14) . . ? O1 Pd1 Cl1 92.07(11) . . ? N2 Pd1 Cl1 92.77(13) . . ? N1 Pd1 Pd1 94.55(13) . 2_776 ? O1 Pd1 Pd1 82.10(10) . 2_776 ? N2 Pd1 Pd1 89.52(12) . 2_776 ? Cl1 Pd1 Pd1 87.95(4) . 2_776 ? N1 Pd1 H2 94.1 . . ? O1 Pd1 H2 143.1 . . ? N2 Pd1 H2 29.4 . . ? Cl1 Pd1 H2 84.7 . . ? Pd1 Pd1 H2 61.1 2_776 . ? C1 O1 Pd1 116.0(3) . . ? C17 N1 C13 121.3(5) . . ? C17 N1 Pd1 114.9(4) . . ? C13 N1 Pd1 123.7(4) . . ? C19 N2 C18 116.8(4) . . ? C19 N2 Pd1 119.9(3) . . ? C18 N2 Pd1 106.9(3) . . ? C19 N2 H2 132.0 . . ? C18 N2 H2 93.6 . . ? Pd1 N2 H2 80.3 . . ? O1 C1 C2 123.9(5) . . ? O1 C1 C6 118.3(5) . . ? C2 C1 C6 117.8(6) . . ? C3 C2 C1 119.9(6) . . ? C3 C2 C13 118.6(6) . . ? C1 C2 C13 121.5(5) . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.9(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 121.0(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.3(6) . . ? C5 C6 C7 121.8(6) . . ? C1 C6 C7 118.9(5) . . ? C12 C7 C8 117.7(6) . . ? C12 C7 C6 122.8(6) . . ? C8 C7 C6 119.6(6) . . ? C9 C8 C7 122.0(7) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 118.7(7) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C11 C10 C9 121.1(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 118.7(7) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C7 C12 C11 121.8(6) . . ? C7 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N1 C13 C14 118.2(6) . . ? N1 C13 C2 120.8(5) . . ? C14 C13 C2 121.0(6) . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 117.4(6) . . ? C15 C16 H16 121.3 . . ? C17 C16 H16 121.3 . . ? N1 C17 C16 122.7(6) . . ? N1 C17 C18 116.6(5) . . ? C16 C17 C18 120.7(6) . . ? N2 C18 C17 113.0(5) . . ? N2 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? N2 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C24 121.4(5) . . ? C20 C19 N2 118.8(5) . . ? C24 C19 N2 119.7(5) . . ? C19 C20 C21 118.4(5) . . ? C19 C20 C25 123.5(5) . . ? C21 C20 C25 118.0(5) . . ? C22 C21 C20 121.5(6) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 119.7(7) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 122.3(7) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C23 C24 C19 116.6(6) . . ? C23 C24 C28 118.3(6) . . ? C19 C24 C28 125.1(5) . . ? C20 C25 C26 110.9(5) . . ? C20 C25 C27 111.8(5) . . ? C26 C25 C27 111.4(5) . . ? C20 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C30 112.0(6) . . ? C24 C28 C29 112.0(6) . . ? C30 C28 C29 112.6(7) . . ? C24 C28 H28 106.6 . . ? C30 C28 H28 106.6 . . ? C29 C28 H28 106.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 N1 Pd1 O1 C1 47.1(4) . . . . ? Cl1 Pd1 O1 C1 -130.8(4) . . . . ? Pd1 Pd1 O1 C1 141.6(4) 2_776 . . . ? O1 Pd1 N1 C17 155.5(4) . . . . ? N2 Pd1 N1 C17 -15.8(4) . . . . ? Pd1 Pd1 N1 C17 73.3(4) 2_776 . . . ? O1 Pd1 N1 C13 -19.3(4) . . . . ? N2 Pd1 N1 C13 169.5(4) . . . . ? Pd1 Pd1 N1 C13 -101.4(4) 2_776 . . . ? N1 Pd1 N2 C19 -118.4(4) . . . . ? Cl1 Pd1 N2 C19 59.0(4) . . . . ? Pd1 Pd1 N2 C19 146.9(4) 2_776 . . . ? N1 Pd1 N2 C18 17.5(3) . . . . ? Cl1 Pd1 N2 C18 -165.0(3) . . . . ? Pd1 Pd1 N2 C18 -77.1(3) 2_776 . . . ? Pd1 O1 C1 C2 -44.7(6) . . . . ? Pd1 O1 C1 C6 138.3(4) . . . . ? O1 C1 C2 C3 -178.0(5) . . . . ? C6 C1 C2 C3 -1.0(8) . . . . ? O1 C1 C2 C13 1.6(8) . . . . ? C6 C1 C2 C13 178.6(5) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C13 C2 C3 C4 -179.9(6) . . . . ? C2 C3 C4 C5 1.5(10) . . . . ? C3 C4 C5 C6 -1.1(10) . . . . ? C4 C5 C6 C1 -0.3(9) . . . . ? C4 C5 C6 C7 177.6(6) . . . . ? O1 C1 C6 C5 178.4(5) . . . . ? C2 C1 C6 C5 1.3(8) . . . . ? O1 C1 C6 C7 0.5(8) . . . . ? C2 C1 C6 C7 -176.6(5) . . . . ? C5 C6 C7 C12 137.0(6) . . . . ? C1 C6 C7 C12 -45.1(8) . . . . ? C5 C6 C7 C8 -41.9(8) . . . . ? C1 C6 C7 C8 136.0(6) . . . . ? C12 C7 C8 C9 -0.1(10) . . . . ? C6 C7 C8 C9 178.9(6) . . . . ? C7 C8 C9 C10 0.1(11) . . . . ? C8 C9 C10 C11 -0.3(12) . . . . ? C9 C10 C11 C12 0.4(12) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? C6 C7 C12 C11 -178.8(6) . . . . ? C10 C11 C12 C7 -0.3(11) . . . . ? C17 N1 C13 C14 -5.4(8) . . . . ? Pd1 N1 C13 C14 169.0(4) . . . . ? C17 N1 C13 C2 171.9(5) . . . . ? Pd1 N1 C13 C2 -13.7(7) . . . . ? C3 C2 C13 N1 -148.9(5) . . . . ? C1 C2 C13 N1 31.5(8) . . . . ? C3 C2 C13 C14 28.3(8) . . . . ? C1 C2 C13 C14 -151.3(5) . . . . ? N1 C13 C14 C15 4.0(8) . . . . ? C2 C13 C14 C15 -173.2(5) . . . . ? C13 C14 C15 C16 0.1(9) . . . . ? C14 C15 C16 C17 -2.8(9) . . . . ? C13 N1 C17 C16 2.7(8) . . . . ? Pd1 N1 C17 C16 -172.2(4) . . . . ? C13 N1 C17 C18 -175.7(5) . . . . ? Pd1 N1 C17 C18 9.4(6) . . . . ? C15 C16 C17 N1 1.5(8) . . . . ? C15 C16 C17 C18 179.8(5) . . . . ? C19 N2 C18 C17 120.3(5) . . . . ? Pd1 N2 C18 C17 -17.3(5) . . . . ? N1 C17 C18 N2 6.2(7) . . . . ? C16 C17 C18 N2 -172.3(5) . . . . ? C18 N2 C19 C20 120.3(6) . . . . ? Pd1 N2 C19 C20 -107.8(5) . . . . ? C18 N2 C19 C24 -61.6(7) . . . . ? Pd1 N2 C19 C24 70.2(6) . . . . ? C24 C19 C20 C21 2.0(9) . . . . ? N2 C19 C20 C21 -180.0(5) . . . . ? C24 C19 C20 C25 179.0(5) . . . . ? N2 C19 C20 C25 -3.0(8) . . . . ? C19 C20 C21 C22 0.0(10) . . . . ? C25 C20 C21 C22 -177.2(7) . . . . ? C20 C21 C22 C23 -1.1(12) . . . . ? C21 C22 C23 C24 0.3(13) . . . . ? C22 C23 C24 C19 1.5(11) . . . . ? C22 C23 C24 C28 -177.8(8) . . . . ? C20 C19 C24 C23 -2.7(9) . . . . ? N2 C19 C24 C23 179.3(6) . . . . ? C20 C19 C24 C28 176.6(6) . . . . ? N2 C19 C24 C28 -1.5(9) . . . . ? C19 C20 C25 C26 -99.1(7) . . . . ? C21 C20 C25 C26 77.9(7) . . . . ? C19 C20 C25 C27 136.0(6) . . . . ? C21 C20 C25 C27 -47.1(7) . . . . ? C23 C24 C28 C30 66.8(9) . . . . ? C19 C24 C28 C30 -112.4(8) . . . . ? C23 C24 C28 C29 -60.8(9) . . . . ? C19 C24 C28 C29 119.9(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O1 1.07 1.93 2.956(6) 159.3 2_776 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.984 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.132 data_10031 _database_code_depnum_ccdc_archive 'CCDC 919248' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 Cl N2 O Pd' _chemical_formula_sum 'C30 H29 Cl N2 O Pd' _chemical_formula_weight 575.40 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.941(4) _cell_length_b 12.678(5) _cell_length_c 20.671(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.076(7) _cell_angle_gamma 90.00 _cell_volume 2585.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 714 _cell_measurement_theta_min 2.616 _cell_measurement_theta_max 23.329 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 4932 reflections(SADABS);Rint 0.2709 before correction and 0.0661 after. ; _exptl_special_details ; Gemini (the Twinning Program) was used to find the cell. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19633 _diffrn_reflns_av_R_equivalents 0.1370 _diffrn_reflns_av_sigmaI/netI 0.1206 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5077 _reflns_number_gt 3225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0767P)^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 5077 _refine_ls_number_parameters 429 _refine_ls_number_restraints 679 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.43210(5) 0.92607(3) 0.31555(2) 0.03284(17) Uani 1 1 d U . . Cl1 Cl 0.20682(17) 0.97102(14) 0.30899(9) 0.0512(5) Uani 1 1 d U A . N1 N 0.6241(5) 0.8811(4) 0.3186(2) 0.0349(11) Uani 1 1 d U A . N2 N 0.4014(5) 0.7988(4) 0.2576(2) 0.0353(12) Uani 1 1 d U A . O1A O 0.4814(4) 1.0540(3) 0.3678(2) 0.0386(10) Uani 0.50 1 d PDU A 1 C1A C 0.5831(15) 1.0467(19) 0.4153(8) 0.032(5) Uani 0.50 1 d PDU A 1 C2A C 0.7202(15) 1.0180(16) 0.4019(9) 0.035(4) Uani 0.50 1 d PDU A 1 C3A C 0.8339(13) 1.0459(10) 0.4462(6) 0.034(3) Uani 0.50 1 d PDU A 1 H3A H 0.9198 1.0167 0.4408 0.040 Uiso 0.50 1 calc PR A 1 C4A C 0.8239(13) 1.1135(10) 0.4964(6) 0.039(3) Uani 0.50 1 d PDU A 1 H4A H 0.9015 1.1307 0.5262 0.047 Uiso 0.50 1 calc PR A 1 C5A C 0.7002(13) 1.1562(9) 0.5034(7) 0.039(3) Uani 0.50 1 d PDU A 1 H5A H 0.6935 1.2007 0.5399 0.047 Uiso 0.50 1 calc PR A 1 C6A C 0.5834(13) 1.1383(10) 0.4603(6) 0.035(3) Uani 0.50 1 d PDU A 1 C7A C 0.4546(14) 1.1935(13) 0.4694(7) 0.043(4) Uani 0.50 1 d PDU A 1 C8A C 0.4386(17) 1.2252(13) 0.5336(7) 0.048(4) Uani 0.50 1 d PDU A 1 H8A H 0.5049 1.2057 0.5687 0.058 Uiso 0.50 1 calc PR A 1 C9A C 0.326(2) 1.2847(17) 0.5463(10) 0.061(6) Uani 0.50 1 d PDU A 1 H9A H 0.3130 1.3020 0.5898 0.073 Uiso 0.50 1 calc PR A 1 C10A C 0.2333(18) 1.3184(14) 0.4940(8) 0.063(4) Uani 0.50 1 d PDU A 1 H10A H 0.1545 1.3561 0.5022 0.076 Uiso 0.50 1 calc PR A 1 C11A C 0.2554(16) 1.2972(13) 0.4307(7) 0.069(4) Uani 0.50 1 d PDU A 1 H11A H 0.1981 1.3279 0.3955 0.083 Uiso 0.50 1 calc PR A 1 C12A C 0.3608(14) 1.2315(11) 0.4180(7) 0.058(4) Uani 0.50 1 d PDU A 1 H12A H 0.3698 1.2120 0.3744 0.070 Uiso 0.50 1 calc PR A 1 O1B O 0.4814(4) 1.0540(3) 0.3678(2) 0.0386(10) Uani 0.50 1 d PDU A 2 C1B C 0.5972(15) 1.066(2) 0.4064(8) 0.035(5) Uani 0.50 1 d PDU A 2 C2B C 0.7083(14) 0.9897(16) 0.4069(9) 0.035(5) Uani 0.50 1 d PDU A 2 C3B C 0.8175(13) 0.9891(13) 0.4579(7) 0.051(4) Uani 0.50 1 d PDU A 2 H3B H 0.8986 0.9517 0.4533 0.061 Uiso 0.50 1 calc PR A 2 C4B C 0.8038(15) 1.0429(16) 0.5133(8) 0.073(5) Uani 0.50 1 d PDU A 2 H4B H 0.8789 1.0473 0.5464 0.087 Uiso 0.50 1 calc PR A 2 C5B C 0.6846(14) 1.0910(14) 0.5228(7) 0.061(4) Uani 0.50 1 d PDU A 2 H5B H 0.6749 1.1186 0.5647 0.073 Uiso 0.50 1 calc PR A 2 C6B C 0.5772(12) 1.1010(11) 0.4732(6) 0.036(3) Uani 0.50 1 d PDU A 2 C7B C 0.4547(13) 1.1609(12) 0.4854(7) 0.039(4) Uani 0.50 1 d PDU A 2 C8B C 0.4662(17) 1.2568(14) 0.5214(9) 0.058(5) Uani 0.50 1 d PDU A 2 H8B H 0.5537 1.2851 0.5346 0.070 Uiso 0.50 1 calc PR A 2 C9B C 0.3526(18) 1.3105(19) 0.5379(11) 0.062(6) Uani 0.50 1 d PDU A 2 H9B H 0.3628 1.3742 0.5623 0.074 Uiso 0.50 1 calc PR A 2 C10B C 0.2229(16) 1.2691(11) 0.5180(8) 0.050(4) Uani 0.50 1 d PDU A 2 H10B H 0.1450 1.2989 0.5332 0.059 Uiso 0.50 1 calc PR A 2 C11B C 0.2111(13) 1.1853(10) 0.4763(6) 0.039(3) Uani 0.50 1 d PDU A 2 H11B H 0.1233 1.1635 0.4577 0.047 Uiso 0.50 1 calc PR A 2 C12B C 0.3227(11) 1.1313(9) 0.4604(5) 0.033(2) Uani 0.50 1 d PDU A 2 H12B H 0.3099 1.0726 0.4317 0.039 Uiso 0.50 1 calc PR A 2 C13 C 0.7322(6) 0.9274(5) 0.3527(3) 0.0392(14) Uani 1 1 d U . . C14 C 0.8607(7) 0.8968(5) 0.3381(3) 0.0431(16) Uani 1 1 d U A . H14 H 0.9382 0.9330 0.3585 0.052 Uiso 1 1 calc R . . C15 C 0.8783(7) 0.8175(5) 0.2960(4) 0.0485(17) Uani 1 1 d U . . H15 H 0.9668 0.7978 0.2877 0.058 Uiso 1 1 calc R A . C16 C 0.7644(7) 0.7650(5) 0.2647(4) 0.0496(18) Uani 1 1 d U A . H16 H 0.7738 0.7070 0.2365 0.060 Uiso 1 1 calc R . . C17 C 0.6396(7) 0.7996(5) 0.2760(3) 0.0416(16) Uani 1 1 d U . . C18 C 0.5129(7) 0.7555(5) 0.2456(3) 0.0412(16) Uani 1 1 d U A . H18 H 0.5121 0.6961 0.2175 0.049 Uiso 1 1 calc R . . C19 C 0.2733(6) 0.7547(5) 0.2302(3) 0.0341(13) Uani 1 1 d U . . C20 C 0.2075(7) 0.8020(5) 0.1734(3) 0.0443(16) Uani 1 1 d U A . C21 C 0.0891(7) 0.7540(6) 0.1463(4) 0.0522(19) Uani 1 1 d U . . H21 H 0.0432 0.7809 0.1067 0.063 Uiso 1 1 calc R A . C22 C 0.0349(7) 0.6675(5) 0.1754(3) 0.0451(17) Uani 1 1 d U A . H22 H -0.0460 0.6353 0.1554 0.054 Uiso 1 1 calc R . . C23 C 0.1000(7) 0.6288(5) 0.2337(3) 0.0402(15) Uani 1 1 d U . . H23 H 0.0617 0.5708 0.2540 0.048 Uiso 1 1 calc R A . C24 C 0.2197(6) 0.6730(5) 0.2629(3) 0.0335(13) Uani 1 1 d U A . C25 C 0.2616(8) 0.8994(6) 0.1427(4) 0.0572(19) Uani 1 1 d U . . H25 H 0.3319 0.9314 0.1757 0.069 Uiso 1 1 calc R A . C26 C 0.3286(11) 0.8738(8) 0.0840(5) 0.096(3) Uani 1 1 d U A . H26A H 0.4022 0.8233 0.0959 0.144 Uiso 1 1 calc R . . H26B H 0.3658 0.9384 0.0671 0.144 Uiso 1 1 calc R . . H26C H 0.2621 0.8429 0.0504 0.144 Uiso 1 1 calc R . . C27 C 0.1483(10) 0.9806(7) 0.1279(5) 0.103(4) Uani 1 1 d U A . H27A H 0.0855 0.9569 0.0905 0.155 Uiso 1 1 calc R . . H27B H 0.1875 1.0487 0.1179 0.155 Uiso 1 1 calc R . . H27C H 0.0993 0.9882 0.1660 0.155 Uiso 1 1 calc R . . C28 C 0.2856(7) 0.6338(5) 0.3287(3) 0.0407(15) Uani 1 1 d U . . H28 H 0.3580 0.6855 0.3448 0.049 Uiso 1 1 calc R A . C29 C 0.3533(11) 0.5283(7) 0.3231(4) 0.089(3) Uani 1 1 d U A . H29A H 0.4060 0.5103 0.3649 0.134 Uiso 1 1 calc R . . H29B H 0.4138 0.5319 0.2891 0.134 Uiso 1 1 calc R . . H29C H 0.2841 0.4742 0.3116 0.134 Uiso 1 1 calc R . . C30 C 0.1863(9) 0.6304(8) 0.3782(4) 0.082(3) Uani 1 1 d U A . H30A H 0.1098 0.5848 0.3622 0.123 Uiso 1 1 calc R . . H30B H 0.1531 0.7018 0.3851 0.123 Uiso 1 1 calc R . . H30C H 0.2314 0.6025 0.4195 0.123 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 0.0251(3) 0.0286(2) 0.0445(3) -0.0015(2) 0.00300(19) 0.0011(2) Cl1 0.0286(9) 0.0491(9) 0.0744(13) -0.0157(9) 0.0000(9) 0.0059(8) N1 0.027(3) 0.035(3) 0.043(3) 0.006(2) 0.005(2) 0.004(2) N2 0.033(3) 0.031(3) 0.042(3) -0.003(2) 0.006(2) -0.001(2) O1A 0.035(2) 0.036(2) 0.043(2) -0.0009(18) -0.0048(19) 0.0025(18) C1A 0.025(6) 0.036(9) 0.033(7) 0.011(6) 0.002(5) -0.012(6) C2A 0.029(6) 0.037(9) 0.040(7) 0.006(6) 0.007(5) -0.010(6) C3A 0.021(6) 0.033(7) 0.047(7) 0.005(5) 0.008(5) -0.006(5) C4A 0.042(6) 0.031(6) 0.044(7) 0.001(5) 0.004(6) -0.005(6) C5A 0.050(6) 0.022(6) 0.044(8) -0.007(5) 0.005(5) -0.004(6) C6A 0.046(6) 0.026(7) 0.031(7) 0.013(5) 0.004(5) -0.004(5) C7A 0.053(7) 0.043(8) 0.035(7) 0.006(7) 0.012(6) -0.002(6) C8A 0.066(10) 0.042(8) 0.038(6) 0.013(7) 0.011(7) 0.005(7) C9A 0.085(12) 0.039(10) 0.059(8) -0.012(8) 0.014(8) 0.011(10) C10A 0.072(10) 0.052(9) 0.065(9) -0.019(8) 0.008(7) 0.019(8) C11A 0.071(11) 0.072(10) 0.065(7) -0.014(8) 0.003(8) 0.023(8) C12A 0.060(9) 0.063(9) 0.051(7) -0.010(7) 0.003(6) 0.017(7) O1B 0.035(2) 0.036(2) 0.043(2) -0.0009(18) -0.0048(19) 0.0025(18) C1B 0.031(6) 0.035(9) 0.041(6) 0.007(7) 0.012(5) -0.015(5) C2B 0.015(6) 0.050(11) 0.038(7) 0.003(7) 0.003(5) -0.017(5) C3B 0.013(6) 0.085(11) 0.054(8) -0.017(8) 0.005(5) -0.013(7) C4B 0.031(7) 0.127(13) 0.057(9) -0.036(9) -0.006(7) 0.006(8) C5B 0.041(7) 0.093(11) 0.046(7) -0.015(8) -0.002(6) 0.005(8) C6B 0.030(5) 0.048(9) 0.031(6) 0.010(6) 0.007(5) -0.011(5) C7B 0.045(6) 0.056(9) 0.015(7) 0.006(6) 0.007(5) 0.000(6) C8B 0.049(7) 0.081(11) 0.047(10) -0.027(9) 0.021(7) -0.028(7) C9B 0.068(9) 0.063(12) 0.056(10) -0.026(9) 0.018(9) -0.011(7) C10B 0.060(7) 0.042(8) 0.047(9) 0.002(6) 0.009(8) 0.010(7) C11B 0.042(6) 0.050(7) 0.026(6) -0.008(5) 0.007(6) 0.001(6) C12B 0.038(6) 0.037(6) 0.023(6) 0.000(5) 0.004(5) 0.003(5) C13 0.028(3) 0.047(4) 0.042(3) 0.008(3) 0.003(3) 0.001(3) C14 0.027(3) 0.053(4) 0.049(4) 0.007(3) 0.001(3) -0.001(3) C15 0.030(4) 0.045(4) 0.072(5) 0.010(3) 0.012(3) 0.004(3) C16 0.037(4) 0.039(4) 0.075(5) -0.001(3) 0.016(4) 0.004(3) C17 0.031(3) 0.032(3) 0.062(4) -0.002(3) 0.009(3) 0.004(3) C18 0.034(3) 0.029(3) 0.061(4) -0.002(3) 0.008(3) 0.003(3) C19 0.027(3) 0.033(3) 0.043(3) -0.007(2) 0.006(3) 0.000(2) C20 0.039(4) 0.043(4) 0.050(4) 0.004(3) 0.001(3) -0.004(3) C21 0.043(4) 0.061(5) 0.050(4) 0.008(3) -0.007(3) -0.009(3) C22 0.040(4) 0.049(4) 0.044(4) -0.008(3) -0.003(3) -0.010(3) C23 0.036(4) 0.034(3) 0.051(4) -0.006(3) 0.008(3) -0.003(3) C24 0.029(3) 0.029(3) 0.043(3) -0.007(3) 0.010(3) 0.000(2) C25 0.049(5) 0.058(5) 0.062(5) 0.020(4) -0.001(4) -0.015(3) C26 0.111(8) 0.105(8) 0.074(6) 0.015(6) 0.023(5) -0.044(6) C27 0.087(7) 0.077(6) 0.143(9) 0.067(6) 0.003(6) 0.003(5) C28 0.043(4) 0.035(3) 0.043(4) -0.004(3) -0.002(3) -0.008(3) C29 0.117(9) 0.074(6) 0.070(6) 0.001(5) -0.011(5) 0.040(6) C30 0.058(6) 0.147(9) 0.041(4) 0.002(5) 0.006(4) -0.017(6) _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 O1A 1.976(4) . ? Pd1 N1 1.986(5) . ? Pd1 N2 2.010(5) . ? Pd1 Cl1 2.2986(19) . ? N1 C13 1.345(8) . ? N1 C17 1.378(8) . ? N2 C18 1.289(7) . ? N2 C19 1.441(8) . ? O1A C1A 1.324(12) . ? C1A C2A 1.469(17) . ? C1A C6A 1.487(16) . ? C2A C3A 1.409(14) . ? C2A C13 1.549(16) . ? C3A C4A 1.359(14) . ? C3A H3A 0.9500 . ? C4A C5A 1.368(15) . ? C4A H4A 0.9500 . ? C5A C6A 1.392(14) . ? C5A H5A 0.9500 . ? C6A C7A 1.492(14) . ? C7A C12A 1.408(15) . ? C7A C8A 1.416(15) . ? C8A C9A 1.400(15) . ? C8A H8A 0.9500 . ? C9A C10A 1.397(19) . ? C9A H9A 0.9500 . ? C10A C11A 1.381(16) . ? C10A H10A 0.9500 . ? C11A C12A 1.389(15) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C1B C2B 1.469(17) . ? C1B C6B 1.487(16) . ? C2B C13 1.414(16) . ? C2B C3B 1.417(14) . ? C3B C4B 1.353(15) . ? C3B H3B 0.9500 . ? C4B C5B 1.369(16) . ? C4B H4B 0.9500 . ? C5B C6B 1.392(14) . ? C5B H5B 0.9500 . ? C6B C7B 1.484(14) . ? C7B C12B 1.401(15) . ? C7B C8B 1.422(15) . ? C8B C9B 1.397(15) . ? C8B H8B 0.9500 . ? C9B C10B 1.406(19) . ? C9B H9B 0.9500 . ? C10B C11B 1.364(15) . ? C10B H10B 0.9500 . ? C11B C12B 1.377(14) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13 C14 1.403(9) . ? C14 C15 1.355(9) . ? C14 H14 0.9500 . ? C15 C16 1.401(10) . ? C15 H15 0.9500 . ? C16 C17 1.362(9) . ? C16 H16 0.9500 . ? C17 C18 1.449(9) . ? C18 H18 0.9500 . ? C19 C24 1.380(8) . ? C19 C20 1.405(9) . ? C20 C21 1.381(9) . ? C20 C25 1.518(9) . ? C21 C22 1.389(9) . ? C21 H21 0.9500 . ? C22 C23 1.386(9) . ? C22 H22 0.9500 . ? C23 C24 1.385(8) . ? C23 H23 0.9500 . ? C24 C28 1.520(9) . ? C25 C26 1.490(11) . ? C25 C27 1.528(11) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.506(10) . ? C28 C29 1.508(10) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O1A Pd1 N1 92.6(2) . . ? O1A Pd1 N2 173.40(19) . . ? N1 Pd1 N2 82.1(2) . . ? O1A Pd1 Cl1 90.18(13) . . ? N1 Pd1 Cl1 177.21(16) . . ? N2 Pd1 Cl1 95.08(16) . . ? C13 N1 C17 121.2(5) . . ? C13 N1 Pd1 126.4(4) . . ? C17 N1 Pd1 112.2(4) . . ? C18 N2 C19 119.8(5) . . ? C18 N2 Pd1 112.7(4) . . ? C19 N2 Pd1 127.4(4) . . ? C1A O1A Pd1 117.7(9) . . ? O1A C1A C2A 121.2(14) . . ? O1A C1A C6A 110.7(12) . . ? C2A C1A C6A 112.4(14) . . ? C3A C2A C1A 120.2(12) . . ? C3A C2A C13 119.5(11) . . ? C1A C2A C13 117.1(13) . . ? C4A C3A C2A 121.7(12) . . ? C4A C3A H3A 119.1 . . ? C2A C3A H3A 119.1 . . ? C3A C4A C5A 118.8(11) . . ? C3A C4A H4A 120.6 . . ? C5A C4A H4A 120.6 . . ? C4A C5A C6A 123.9(11) . . ? C4A C5A H5A 118.1 . . ? C6A C5A H5A 118.1 . . ? C5A C6A C1A 117.7(10) . . ? C5A C6A C7A 120.3(11) . . ? C1A C6A C7A 120.6(11) . . ? C12A C7A C8A 118.0(12) . . ? C12A C7A C6A 124.4(12) . . ? C8A C7A C6A 116.6(12) . . ? C9A C8A C7A 120.8(14) . . ? C9A C8A H8A 119.6 . . ? C7A C8A H8A 119.6 . . ? C10A C9A C8A 119.2(15) . . ? C10A C9A H9A 120.4 . . ? C8A C9A H9A 120.4 . . ? C11A C10A C9A 120.4(14) . . ? C11A C10A H10A 119.8 . . ? C9A C10A H10A 119.8 . . ? C10A C11A C12A 120.5(14) . . ? C10A C11A H11A 119.7 . . ? C12A C11A H11A 119.7 . . ? C11A C12A C7A 120.5(12) . . ? C11A C12A H12A 119.8 . . ? C7A C12A H12A 119.8 . . ? C2B C1B C6B 112.1(15) . . ? C13 C2B C3B 113.5(11) . . ? C13 C2B C1B 124.2(12) . . ? C3B C2B C1B 121.0(12) . . ? C4B C3B C2B 118.7(12) . . ? C4B C3B H3B 120.7 . . ? C2B C3B H3B 120.7 . . ? C3B C4B C5B 121.7(13) . . ? C3B C4B H4B 119.2 . . ? C5B C4B H4B 119.2 . . ? C4B C5B C6B 122.2(12) . . ? C4B C5B H5B 118.9 . . ? C6B C5B H5B 118.9 . . ? C5B C6B C7B 119.5(11) . . ? C5B C6B C1B 118.7(10) . . ? C7B C6B C1B 121.1(11) . . ? C12B C7B C8B 115.7(11) . . ? C12B C7B C6B 123.4(11) . . ? C8B C7B C6B 120.8(12) . . ? C9B C8B C7B 122.0(14) . . ? C9B C8B H8B 119.0 . . ? C7B C8B H8B 119.0 . . ? C8B C9B C10B 119.0(15) . . ? C8B C9B H9B 120.5 . . ? C10B C9B H9B 120.5 . . ? C11B C10B C9B 118.8(13) . . ? C11B C10B H10B 120.6 . . ? C9B C10B H10B 120.6 . . ? C10B C11B C12B 121.9(12) . . ? C10B C11B H11B 119.0 . . ? C12B C11B H11B 119.0 . . ? C11B C12B C7B 121.6(11) . . ? C11B C12B H12B 119.2 . . ? C7B C12B H12B 119.2 . . ? N1 C13 C14 117.1(6) . . ? N1 C13 C2B 117.3(8) . . ? C14 C13 C2B 124.8(8) . . ? N1 C13 C2A 123.2(7) . . ? C14 C13 C2A 119.5(8) . . ? C2B C13 C2A 14.4(18) . . ? C15 C14 C13 122.5(7) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 119.2(7) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 118.0(7) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 N1 121.7(6) . . ? C16 C17 C18 124.2(6) . . ? N1 C17 C18 114.0(6) . . ? N2 C18 C17 118.3(6) . . ? N2 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? C24 C19 C20 124.1(6) . . ? C24 C19 N2 118.3(6) . . ? C20 C19 N2 117.4(6) . . ? C21 C20 C19 115.9(6) . . ? C21 C20 C25 121.2(6) . . ? C19 C20 C25 123.0(6) . . ? C20 C21 C22 121.9(7) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C23 C22 C21 119.4(6) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 121.3(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C19 C24 C23 117.0(6) . . ? C19 C24 C28 122.3(6) . . ? C23 C24 C28 120.7(6) . . ? C26 C25 C20 112.3(7) . . ? C26 C25 C27 112.1(8) . . ? C20 C25 C27 110.0(7) . . ? C26 C25 H25 107.4 . . ? C20 C25 H25 107.4 . . ? C27 C25 H25 107.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 111.3(7) . . ? C30 C28 C24 111.8(6) . . ? C29 C28 C24 111.6(6) . . ? C30 C28 H28 107.3 . . ? C29 C28 H28 107.3 . . ? C24 C28 H28 107.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 O1A Pd1 N1 C13 5.7(5) . . . . ? N2 Pd1 N1 C13 -178.3(5) . . . . ? Cl1 Pd1 N1 C13 -176(36) . . . . ? O1A Pd1 N1 C17 -168.8(4) . . . . ? N2 Pd1 N1 C17 7.2(4) . . . . ? Cl1 Pd1 N1 C17 10(3) . . . . ? O1A Pd1 N2 C18 32.2(18) . . . . ? N1 Pd1 N2 C18 -5.2(5) . . . . ? Cl1 Pd1 N2 C18 174.9(4) . . . . ? O1A Pd1 N2 C19 -147.9(14) . . . . ? N1 Pd1 N2 C19 174.7(5) . . . . ? Cl1 Pd1 N2 C19 -5.2(5) . . . . ? N1 Pd1 O1A C1A -36.9(12) . . . . ? N2 Pd1 O1A C1A -74(2) . . . . ? Cl1 Pd1 O1A C1A 143.2(12) . . . . ? Pd1 O1A C1A C2A 60(3) . . . . ? Pd1 O1A C1A C6A -164.7(12) . . . . ? O1A C1A C2A C3A 157.4(17) . . . . ? C6A C1A C2A C3A 23(3) . . . . ? O1A C1A C2A C13 -43(4) . . . . ? C6A C1A C2A C13 -176.9(14) . . . . ? C1A C2A C3A C4A -11(3) . . . . ? C13 C2A C3A C4A -170.0(14) . . . . ? C2A C3A C4A C5A -1(2) . . . . ? C3A C4A C5A C6A -3(2) . . . . ? C4A C5A C6A C1A 17(2) . . . . ? C4A C5A C6A C7A -176.1(13) . . . . ? O1A C1A C6A C5A -165.0(15) . . . . ? C2A C1A C6A C5A -26(3) . . . . ? O1A C1A C6A C7A 28(3) . . . . ? C2A C1A C6A C7A 167.4(17) . . . . ? C5A C6A C7A C12A 142.3(16) . . . . ? C1A C6A C7A C12A -51(2) . . . . ? C5A C6A C7A C8A -26(2) . . . . ? C1A C6A C7A C8A 139.9(19) . . . . ? C12A C7A C8A C9A 6(3) . . . . ? C6A C7A C8A C9A 175.0(17) . . . . ? C7A C8A C9A C10A -4(3) . . . . ? C8A C9A C10A C11A -3(3) . . . . ? C9A C10A C11A C12A 8(3) . . . . ? C10A C11A C12A C7A -6(3) . . . . ? C8A C7A C12A C11A -1(3) . . . . ? C6A C7A C12A C11A -169.1(15) . . . . ? C6B C1B C2B C13 166.5(17) . . . . ? C6B C1B C2B C3B -27(3) . . . . ? C13 C2B C3B C4B -177.5(17) . . . . ? C1B C2B C3B C4B 15(3) . . . . ? C2B C3B C4B C5B 5(3) . . . . ? C3B C4B C5B C6B -9(3) . . . . ? C4B C5B C6B C7B -175.5(18) . . . . ? C4B C5B C6B C1B -5(3) . . . . ? C2B C1B C6B C5B 22(3) . . . . ? C2B C1B C6B C7B -167.7(17) . . . . ? C5B C6B C7B C12B -142.4(16) . . . . ? C1B C6B C7B C12B 48(2) . . . . ? C5B C6B C7B C8B 41(2) . . . . ? C1B C6B C7B C8B -129(2) . . . . ? C12B C7B C8B C9B 8(3) . . . . ? C6B C7B C8B C9B -175.0(18) . . . . ? C7B C8B C9B C10B 0(3) . . . . ? C8B C9B C10B C11B -8(3) . . . . ? C9B C10B C11B C12B 9(3) . . . . ? C10B C11B C12B C7B -1(2) . . . . ? C8B C7B C12B C11B -7(2) . . . . ? C6B C7B C12B C11B 175.8(12) . . . . ? C17 N1 C13 C14 6.6(9) . . . . ? Pd1 N1 C13 C14 -167.5(4) . . . . ? C17 N1 C13 C2B -163.8(12) . . . . ? Pd1 N1 C13 C2B 22.2(13) . . . . ? C17 N1 C13 C2A -179.0(12) . . . . ? Pd1 N1 C13 C2A 6.9(14) . . . . ? C3B C2B C13 N1 148.5(14) . . . . ? C1B C2B C13 N1 -44(3) . . . . ? C3B C2B C13 C14 -21(2) . . . . ? C1B C2B C13 C14 146(2) . . . . ? C3B C2B C13 C2A -94(4) . . . . ? C1B C2B C13 C2A 73(4) . . . . ? C3A C2A C13 N1 165.6(13) . . . . ? C1A C2A C13 N1 6(3) . . . . ? C3A C2A C13 C14 -20(2) . . . . ? C1A C2A C13 C14 180.0(17) . . . . ? C3A C2A C13 C2B 96(4) . . . . ? C1A C2A C13 C2B -64(3) . . . . ? N1 C13 C14 C15 -6.0(10) . . . . ? C2B C13 C14 C15 163.5(13) . . . . ? C2A C13 C14 C15 179.4(12) . . . . ? C13 C14 C15 C16 1.2(11) . . . . ? C14 C15 C16 C17 3.0(10) . . . . ? C15 C16 C17 N1 -2.4(10) . . . . ? C15 C16 C17 C18 177.9(6) . . . . ? C13 N1 C17 C16 -2.5(10) . . . . ? Pd1 N1 C17 C16 172.3(5) . . . . ? C13 N1 C17 C18 177.1(6) . . . . ? Pd1 N1 C17 C18 -8.1(7) . . . . ? C19 N2 C18 C17 -177.7(6) . . . . ? Pd1 N2 C18 C17 2.2(8) . . . . ? C16 C17 C18 N2 -176.4(6) . . . . ? N1 C17 C18 N2 3.9(9) . . . . ? C18 N2 C19 C24 84.8(7) . . . . ? Pd1 N2 C19 C24 -95.1(6) . . . . ? C18 N2 C19 C20 -98.5(7) . . . . ? Pd1 N2 C19 C20 81.5(7) . . . . ? C24 C19 C20 C21 -7.2(10) . . . . ? N2 C19 C20 C21 176.4(6) . . . . ? C24 C19 C20 C25 173.0(6) . . . . ? N2 C19 C20 C25 -3.4(10) . . . . ? C19 C20 C21 C22 3.1(11) . . . . ? C25 C20 C21 C22 -177.1(7) . . . . ? C20 C21 C22 C23 1.0(11) . . . . ? C21 C22 C23 C24 -1.5(10) . . . . ? C20 C19 C24 C23 6.7(9) . . . . ? N2 C19 C24 C23 -176.9(5) . . . . ? C20 C19 C24 C28 -171.8(6) . . . . ? N2 C19 C24 C28 4.6(9) . . . . ? C22 C23 C24 C19 -2.1(9) . . . . ? C22 C23 C24 C28 176.4(6) . . . . ? C21 C20 C25 C26 -77.0(10) . . . . ? C19 C20 C25 C26 102.8(9) . . . . ? C21 C20 C25 C27 48.6(10) . . . . ? C19 C20 C25 C27 -131.6(8) . . . . ? C19 C24 C28 C30 127.7(7) . . . . ? C23 C24 C28 C30 -50.8(8) . . . . ? C19 C24 C28 C29 -106.9(8) . . . . ? C23 C24 C28 C29 74.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.459 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.134 data_10066 _database_code_depnum_ccdc_archive 'CCDC 919249' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '5(C27 H23 Cl N2 O Pd), 3(C H2 Cl2)' _chemical_formula_sum 'C138 H121 Cl11 N10 O5 Pd5' _chemical_formula_weight 2921.40 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' 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 13.427(8) _cell_length_b 17.856(11) _cell_length_c 26.730(16) _cell_angle_alpha 76.396(13) _cell_angle_beta 86.289(14) _cell_angle_gamma 86.280(15) _cell_volume 6208(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 947 _cell_measurement_theta_min 2.242 _cell_measurement_theta_max 23.323 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 5866 reflections(SADABS);Rint 0.1492 before correction and 0.0511 after. ; _exptl_special_details ; The crystal data was weak due to crystal quality. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48941 _diffrn_reflns_av_R_equivalents 0.1753 _diffrn_reflns_av_sigmaI/netI 0.3590 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 24098 _reflns_number_gt 8225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0036P)^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 24098 _refine_ls_number_parameters 1536 _refine_ls_number_restraints 1475 _refine_ls_R_factor_all 0.2329 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.775 _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 0.35500(6) 0.26294(4) 0.01394(3) 0.0331(2) Uani 1 1 d U . . Cl1 Cl 0.4230(2) 0.37737(14) -0.02570(9) 0.0374(7) Uani 1 1 d U . . O1 O 0.4373(5) 0.2578(3) 0.0719(2) 0.0343(17) Uani 1 1 d U . . N1 N 0.3015(6) 0.1615(4) 0.0432(3) 0.029(2) Uani 1 1 d U . . N2 N 0.2680(6) 0.2608(5) -0.0428(3) 0.035(2) Uani 1 1 d U . . C1 C 0.4188(7) 0.2116(5) 0.1195(4) 0.028(2) Uani 1 1 d U . . C2 C 0.3678(7) 0.1425(6) 0.1284(4) 0.033(2) Uani 1 1 d U . . C3 C 0.3599(8) 0.0999(5) 0.1807(4) 0.038(3) Uani 1 1 d U . . H3 H 0.3247 0.0537 0.1886 0.046 Uiso 1 1 calc R . . C4 C 0.3995(8) 0.1220(6) 0.2192(4) 0.040(3) Uani 1 1 d U . . H4 H 0.3955 0.0906 0.2532 0.048 Uiso 1 1 calc R . . C5 C 0.4463(7) 0.1907(6) 0.2089(4) 0.038(3) Uani 1 1 d U . . H5 H 0.4724 0.2066 0.2367 0.046 Uiso 1 1 calc R . . C6 C 0.4569(7) 0.2368(6) 0.1607(4) 0.032(2) Uani 1 1 d U . . C7 C 0.5099(8) 0.3103(6) 0.1517(3) 0.029(2) Uani 1 1 d U . . C8 C 0.5914(8) 0.3156(6) 0.1775(4) 0.045(3) Uani 1 1 d U . . H8 H 0.6151 0.2721 0.2025 0.054 Uiso 1 1 calc R . . C9 C 0.6405(9) 0.3827(7) 0.1682(4) 0.058(3) Uani 1 1 d U . . H9 H 0.6979 0.3845 0.1867 0.070 Uiso 1 1 calc R . . C10 C 0.6092(9) 0.4472(7) 0.1329(4) 0.058(3) Uani 1 1 d U . . H10 H 0.6453 0.4929 0.1257 0.069 Uiso 1 1 calc R . . C11 C 0.5237(8) 0.4435(6) 0.1084(4) 0.041(3) Uani 1 1 d U . . H11 H 0.4981 0.4883 0.0851 0.049 Uiso 1 1 calc R . . C12 C 0.4744(7) 0.3763(5) 0.1169(3) 0.033(3) Uani 1 1 d U . . H12 H 0.4159 0.3747 0.0990 0.040 Uiso 1 1 calc R . . C13 C 0.3184(8) 0.1155(6) 0.0892(4) 0.035(2) Uani 1 1 d U . . C14 C 0.2869(8) 0.0382(6) 0.0976(4) 0.041(3) Uani 1 1 d U . . H14 H 0.3027 0.0029 0.1290 0.049 Uiso 1 1 calc R . . C15 C 0.2365(8) 0.0132(6) 0.0638(4) 0.046(3) Uani 1 1 d U . . H15 H 0.2179 -0.0389 0.0708 0.055 Uiso 1 1 calc R . . C16 C 0.2124(8) 0.0635(6) 0.0193(4) 0.054(3) Uani 1 1 d U . . H16 H 0.1722 0.0488 -0.0044 0.065 Uiso 1 1 calc R . . C17 C 0.2481(8) 0.1369(6) 0.0092(4) 0.043(3) Uani 1 1 d U . . C18 C 0.2278(8) 0.1974(6) -0.0364(4) 0.046(3) Uani 1 1 d U . . H18 H 0.1847 0.1891 -0.0612 0.055 Uiso 1 1 calc R . . C19 C 0.2487(8) 0.3212(6) -0.0875(4) 0.041(3) Uani 1 1 d U . . C20 C 0.3014(8) 0.3230(6) -0.1336(4) 0.039(3) Uani 1 1 d U . . C21 C 0.2770(8) 0.3819(6) -0.1759(4) 0.043(3) Uani 1 1 d U . . H21 H 0.3144 0.3845 -0.2076 0.052 Uiso 1 1 calc R . . C22 C 0.2000(8) 0.4368(6) -0.1734(4) 0.043(3) Uani 1 1 d U . . C23 C 0.1518(8) 0.4339(6) -0.1261(4) 0.045(3) Uani 1 1 d U . . H23 H 0.1018 0.4730 -0.1233 0.054 Uiso 1 1 calc R . . C24 C 0.1718(8) 0.3776(6) -0.0824(4) 0.040(3) Uani 1 1 d U . . C25 C 0.3846(8) 0.2658(6) -0.1377(4) 0.057(3) Uani 1 1 d U . . H25A H 0.4392 0.2732 -0.1170 0.085 Uiso 1 1 calc R . . H25B H 0.4087 0.2728 -0.1738 0.085 Uiso 1 1 calc R . . H25C H 0.3610 0.2136 -0.1250 0.085 Uiso 1 1 calc R . . C26 C 0.1725(8) 0.4980(6) -0.2202(4) 0.065(4) Uani 1 1 d U . . H26A H 0.1039 0.5183 -0.2151 0.097 Uiso 1 1 calc R . . H26B H 0.1771 0.4756 -0.2505 0.097 Uiso 1 1 calc R . . H26C H 0.2184 0.5399 -0.2255 0.097 Uiso 1 1 calc R . . C27 C 0.1143(8) 0.3751(6) -0.0321(4) 0.055(3) Uani 1 1 d U . . H27A H 0.1607 0.3639 -0.0041 0.082 Uiso 1 1 calc R . . H27B H 0.0660 0.3347 -0.0261 0.082 Uiso 1 1 calc R . . H27C H 0.0788 0.4251 -0.0331 0.082 Uiso 1 1 calc R . . Pd1A Pd 0.89673(6) 0.33026(5) 0.30479(3) 0.0372(2) Uani 1 1 d U . . Cl1A Cl 0.8001(2) 0.25364(16) 0.27261(10) 0.0465(8) Uani 1 1 d U . . O1A O 0.9922(5) 0.3270(4) 0.2479(2) 0.0430(19) Uani 1 1 d U . . N1A N 0.9796(6) 0.3927(4) 0.3357(3) 0.0329(19) Uani 1 1 d U . . N2A N 0.8020(6) 0.3406(5) 0.3639(3) 0.038(2) Uani 1 1 d U . . C1A C 1.0794(8) 0.3572(5) 0.2402(4) 0.034(2) Uani 1 1 d U . . C2A C 1.1238(8) 0.3969(5) 0.2729(4) 0.037(2) Uani 1 1 d U . . C3A C 1.2266(8) 0.4167(6) 0.2599(4) 0.045(3) Uani 1 1 d U . . H3A H 1.2599 0.4411 0.2815 0.055 Uiso 1 1 calc R . . C4A C 1.2759(8) 0.4013(6) 0.2180(4) 0.045(3) Uani 1 1 d U . . H4A H 1.3438 0.4142 0.2110 0.054 Uiso 1 1 calc R . . C5A C 1.2321(8) 0.3680(6) 0.1855(4) 0.038(3) Uani 1 1 d U . . H5A H 1.2693 0.3587 0.1559 0.046 Uiso 1 1 calc R . . C6A C 1.1334(8) 0.3470(5) 0.1944(4) 0.036(2) Uani 1 1 d U . . C7A C 1.0878(8) 0.3141(6) 0.1572(4) 0.042(3) Uani 1 1 d U . . C8A C 1.1331(8) 0.2547(6) 0.1377(4) 0.051(3) Uani 1 1 d U . . H8A H 1.1962 0.2329 0.1495 0.062 Uiso 1 1 calc R . . C9A C 1.0889(10) 0.2265(8) 0.1014(4) 0.070(4) Uani 1 1 d U . . H9A H 1.1233 0.1865 0.0882 0.084 Uiso 1 1 calc R . . C10A C 0.9959(10) 0.2541(8) 0.0835(4) 0.068(4) Uani 1 1 d U . . H10A H 0.9645 0.2326 0.0597 0.082 Uiso 1 1 calc R . . C11A C 0.9520(10) 0.3138(7) 0.1019(4) 0.067(4) Uani 1 1 d U . . H11A H 0.8911 0.3378 0.0884 0.080 Uiso 1 1 calc R . . C12A C 0.9947(9) 0.3399(6) 0.1398(4) 0.050(3) Uani 1 1 d U . . H12A H 0.9580 0.3775 0.1546 0.060 Uiso 1 1 calc R . . C13A C 1.0711(8) 0.4184(5) 0.3169(4) 0.037(2) Uani 1 1 d U . . C14A C 1.1139(9) 0.4658(6) 0.3448(4) 0.053(3) Uani 1 1 d U . . H14A H 1.1771 0.4860 0.3328 0.064 Uiso 1 1 calc R . . C15A C 1.0688(9) 0.4837(6) 0.3879(4) 0.056(3) Uani 1 1 d U . . H15A H 1.0995 0.5166 0.4049 0.067 Uiso 1 1 calc R . . C16A C 0.9775(8) 0.4535(6) 0.4067(4) 0.046(3) Uani 1 1 d U . . H16A H 0.9456 0.4620 0.4378 0.055 Uiso 1 1 calc R . . C17A C 0.9366(9) 0.4116(6) 0.3785(4) 0.040(3) Uani 1 1 d U . . C18A C 0.8395(8) 0.3820(5) 0.3916(4) 0.038(3) Uani 1 1 d U . . H18A H 0.8020 0.3927 0.4207 0.045 Uiso 1 1 calc R . . C19A C 0.7078(8) 0.3047(6) 0.3794(4) 0.037(2) Uani 1 1 d U . . C20A C 0.7070(8) 0.2412(6) 0.4212(4) 0.041(3) Uani 1 1 d U . . C21A C 0.6204(9) 0.2045(7) 0.4343(4) 0.052(3) Uani 1 1 d U . . H21A H 0.6193 0.1613 0.4628 0.062 Uiso 1 1 calc R . . C22A C 0.5333(9) 0.2270(8) 0.4080(4) 0.058(3) Uani 1 1 d U . . C23A C 0.5401(9) 0.2922(7) 0.3687(4) 0.060(3) Uani 1 1 d U . . H23A H 0.4809 0.3111 0.3513 0.072 Uiso 1 1 calc R . . C24A C 0.6234(9) 0.3318(7) 0.3526(4) 0.054(3) Uani 1 1 d U . . C25A C 0.8001(8) 0.2107(6) 0.4483(4) 0.053(3) Uani 1 1 d U . . H25D H 0.8198 0.2475 0.4674 0.080 Uiso 1 1 calc R . . H25E H 0.8538 0.2035 0.4229 0.080 Uiso 1 1 calc R . . H25F H 0.7879 0.1612 0.4723 0.080 Uiso 1 1 calc R . . C26A C 0.4412(8) 0.1836(7) 0.4229(4) 0.084(4) Uani 1 1 d U . . H26D H 0.3835 0.2200 0.4234 0.126 Uiso 1 1 calc R . . H26E H 0.4473 0.1494 0.4572 0.126 Uiso 1 1 calc R . . H26F H 0.4320 0.1528 0.3978 0.126 Uiso 1 1 calc R . . C27A C 0.6220(8) 0.4008(6) 0.3087(4) 0.067(4) Uani 1 1 d U . . H27D H 0.6285 0.3842 0.2761 0.100 Uiso 1 1 calc R . . H27E H 0.6777 0.4326 0.3106 0.100 Uiso 1 1 calc R . . H27F H 0.5587 0.4310 0.3104 0.100 Uiso 1 1 calc R . . Pd1B Pd 0.79507(6) 0.97583(5) 0.69243(3) 0.0386(2) Uani 1 1 d U . . Cl1B Cl 0.6922(2) 0.98512(16) 0.62554(10) 0.0473(8) Uani 1 1 d U . . O1B O 0.7109(5) 1.0569(3) 0.7140(2) 0.0359(17) Uani 1 1 d U . . N1B N 0.8875(6) 0.9662(5) 0.7480(3) 0.035(2) Uani 1 1 d U . . N2B N 0.8808(6) 0.8862(5) 0.6781(3) 0.037(2) Uani 1 1 d U . . C1B C 0.7286(8) 1.0908(5) 0.7505(4) 0.030(2) Uani 1 1 d U . . C2B C 0.8137(8) 1.0745(6) 0.7810(4) 0.035(2) Uani 1 1 d U . . C3B C 0.8229(8) 1.1244(5) 0.8153(4) 0.040(3) Uani 1 1 d U . . H3B H 0.8812 1.1166 0.8346 0.048 Uiso 1 1 calc R . . C4B C 0.7568(9) 1.1809(6) 0.8225(4) 0.051(3) Uani 1 1 d U . . H4B H 0.7700 1.2140 0.8441 0.061 Uiso 1 1 calc R . . C5B C 0.6680(8) 1.1893(6) 0.7970(4) 0.042(3) Uani 1 1 d U . . H5B H 0.6168 1.2251 0.8043 0.050 Uiso 1 1 calc R . . C6B C 0.6523(8) 1.1466(6) 0.7612(4) 0.037(2) Uani 1 1 d U . . C7B C 0.5567(8) 1.1603(6) 0.7348(4) 0.038(3) Uani 1 1 d U . . C8B C 0.5127(8) 1.2349(6) 0.7206(4) 0.048(3) Uani 1 1 d U . . H8B H 0.5480 1.2775 0.7243 0.057 Uiso 1 1 calc R . . C9B C 0.4208(9) 1.2471(7) 0.7017(4) 0.062(4) Uani 1 1 d U . . H9B H 0.3930 1.2985 0.6918 0.075 Uiso 1 1 calc R . . C10B C 0.3663(8) 1.1871(7) 0.6963(4) 0.056(3) Uani 1 1 d U . . H10B H 0.3010 1.1958 0.6837 0.067 Uiso 1 1 calc R . . C11B C 0.4100(9) 1.1143(7) 0.7099(4) 0.056(3) Uani 1 1 d U . . H11B H 0.3745 1.0718 0.7060 0.067 Uiso 1 1 calc R . . C12B C 0.5024(8) 1.1010(6) 0.7288(4) 0.042(3) Uani 1 1 d U . . H12B H 0.5300 1.0495 0.7380 0.050 Uiso 1 1 calc R . . C13B C 0.8855(8) 1.0107(6) 0.7819(4) 0.032(2) Uani 1 1 d U . . C14B C 0.9562(8) 0.9894(6) 0.8207(4) 0.052(3) Uani 1 1 d U . . H14B H 0.9551 1.0189 0.8460 0.063 Uiso 1 1 calc R . . C15B C 1.0250(9) 0.9298(7) 0.8242(4) 0.060(3) Uani 1 1 d U . . H15B H 1.0712 0.9174 0.8507 0.072 Uiso 1 1 calc R . . C16B C 1.0241(9) 0.8876(6) 0.7864(4) 0.058(3) Uani 1 1 d U . . H16B H 1.0705 0.8449 0.7870 0.070 Uiso 1 1 calc R . . C17B C 0.9565(8) 0.9073(6) 0.7484(4) 0.043(3) Uani 1 1 d U . . C18B C 0.9487(8) 0.8656(6) 0.7106(4) 0.047(3) Uani 1 1 d U . . H18B H 0.9933 0.8225 0.7093 0.057 Uiso 1 1 calc R . . C19B C 0.8751(8) 0.8440(6) 0.6394(4) 0.049(3) Uani 1 1 d U . . C20B C 0.9384(9) 0.8590(7) 0.5963(4) 0.051(3) Uani 1 1 d U . . C21B C 0.9334(9) 0.8167(7) 0.5614(4) 0.055(3) Uani 1 1 d U . . H21B H 0.9770 0.8279 0.5315 0.066 Uiso 1 1 calc R . . C22B C 0.8694(9) 0.7586(7) 0.5661(4) 0.051(3) Uani 1 1 d U . . C23B C 0.8036(8) 0.7449(6) 0.6104(4) 0.052(3) Uani 1 1 d U . . H23B H 0.7584 0.7046 0.6158 0.063 Uiso 1 1 calc R . . C24B C 0.8047(8) 0.7906(6) 0.6467(4) 0.044(3) Uani 1 1 d U . . C25B C 1.0139(8) 0.9212(7) 0.5885(4) 0.082(4) Uani 1 1 d U . . H25G H 1.0616 0.9076 0.6158 0.123 Uiso 1 1 calc R . . H25H H 0.9789 0.9707 0.5896 0.123 Uiso 1 1 calc R . . H25I H 1.0499 0.9254 0.5549 0.123 Uiso 1 1 calc R . . C26B C 0.8620(8) 0.7111(6) 0.5256(4) 0.060(4) Uani 1 1 d U . . H26G H 0.8169 0.7386 0.4992 0.090 Uiso 1 1 calc R . . H26H H 0.8360 0.6608 0.5422 0.090 Uiso 1 1 calc R . . H26I H 0.9284 0.7037 0.5095 0.090 Uiso 1 1 calc R . . C27B C 0.7294(7) 0.7775(6) 0.6919(4) 0.052(3) Uani 1 1 d U . . H27G H 0.7644 0.7600 0.7240 0.078 Uiso 1 1 calc R . . H27H H 0.6842 0.7381 0.6887 0.078 Uiso 1 1 calc R . . H27I H 0.6907 0.8258 0.6924 0.078 Uiso 1 1 calc R . . Pd1C Pd 0.82385(6) 0.23661(4) 0.98205(3) 0.0363(2) Uani 1 1 d U . . Cl1C Cl 0.8715(2) 0.10952(14) 1.01221(10) 0.0498(8) Uani 1 1 d U . . O1C O 0.9480(5) 0.2534(3) 0.9402(2) 0.0348(17) Uani 1 1 d U . . N1C N 0.7809(6) 0.3469(4) 0.9617(3) 0.035(2) Uani 1 1 d U . . N2C N 0.6974(6) 0.2345(5) 1.0254(3) 0.035(2) Uani 1 1 d U . . C1C C 0.9478(7) 0.3018(6) 0.8933(4) 0.034(2) Uani 1 1 d U . . C2C C 0.8938(7) 0.3749(5) 0.8849(4) 0.029(2) Uani 1 1 d U . . C3C C 0.8995(7) 0.4224(6) 0.8354(4) 0.041(3) Uani 1 1 d U . . H3C H 0.8649 0.4715 0.8292 0.049 Uiso 1 1 calc R . . C4C C 0.9532(8) 0.4008(6) 0.7954(4) 0.039(3) Uani 1 1 d U . . H4C H 0.9531 0.4330 0.7616 0.047 Uiso 1 1 calc R . . C5C C 1.0076(8) 0.3309(6) 0.8053(4) 0.039(3) Uani 1 1 d U . . H5C H 1.0498 0.3177 0.7784 0.047 Uiso 1 1 calc R . . C6C C 1.0031(7) 0.2803(6) 0.8522(4) 0.032(2) Uani 1 1 d U . . C7C C 1.0623(8) 0.2053(6) 0.8602(4) 0.034(2) Uani 1 1 d U . . C8C C 1.1531(8) 0.1981(6) 0.8338(4) 0.044(3) Uani 1 1 d U . . H8C H 1.1787 0.2420 0.8104 0.052 Uiso 1 1 calc R . . C9C C 1.2068(8) 0.1288(7) 0.8408(4) 0.055(3) Uani 1 1 d U . . H9C H 1.2688 0.1255 0.8220 0.065 Uiso 1 1 calc R . . C10C C 1.1728(9) 0.0645(7) 0.8743(4) 0.056(3) Uani 1 1 d U . . H10C H 1.2110 0.0169 0.8793 0.068 Uiso 1 1 calc R . . C11C C 1.0834(9) 0.0696(6) 0.9005(4) 0.051(3) Uani 1 1 d U . . H11C H 1.0584 0.0253 0.9239 0.061 Uiso 1 1 calc R . . C12C C 1.0291(8) 0.1390(6) 0.8932(4) 0.040(3) Uani 1 1 d U . . H12C H 0.9664 0.1413 0.9115 0.048 Uiso 1 1 calc R . . C13C C 0.8283(7) 0.3987(6) 0.9246(4) 0.032(2) Uani 1 1 d U . . C14C C 0.8049(8) 0.4779(5) 0.9244(4) 0.039(3) Uani 1 1 d U . . H14C H 0.8401 0.5165 0.9005 0.047 Uiso 1 1 calc R . . C15C C 0.7337(8) 0.4999(6) 0.9576(4) 0.042(3) Uani 1 1 d U . . H15C H 0.7210 0.5527 0.9579 0.050 Uiso 1 1 calc R . . C16C C 0.6803(8) 0.4428(5) 0.9908(3) 0.036(3) Uani 1 1 d U . . H16C H 0.6249 0.4564 1.0115 0.043 Uiso 1 1 calc R . . C17C C 0.7082(8) 0.3667(6) 0.9937(4) 0.035(3) Uani 1 1 d U . . C18C C 0.6581(8) 0.3015(6) 1.0268(3) 0.037(3) Uani 1 1 d U . . H18C H 0.6001 0.3082 1.0480 0.045 Uiso 1 1 calc R . . C19C C 0.6486(8) 0.1660(6) 1.0535(4) 0.036(2) Uani 1 1 d U . . C20C C 0.6659(8) 0.1390(6) 1.1045(4) 0.038(3) Uani 1 1 d U . . C21C C 0.6245(7) 0.0702(6) 1.1304(4) 0.040(3) Uani 1 1 d U . . H21C H 0.6355 0.0497 1.1659 0.048 Uiso 1 1 calc R . . C22C C 0.5680(8) 0.0321(6) 1.1045(4) 0.045(3) Uani 1 1 d U . . C23C C 0.5538(8) 0.0598(6) 1.0539(4) 0.047(3) Uani 1 1 d U . . H23C H 0.5154 0.0318 1.0366 0.057 Uiso 1 1 calc R . . C24C C 0.5938(8) 0.1283(6) 1.0262(4) 0.039(3) Uani 1 1 d U . . C25C C 0.7332(8) 0.1758(6) 1.1328(3) 0.051(3) Uani 1 1 d U . . H25J H 0.8004 0.1772 1.1161 0.076 Uiso 1 1 calc R . . H25K H 0.7361 0.1459 1.1685 0.076 Uiso 1 1 calc R . . H25L H 0.7074 0.2286 1.1325 0.076 Uiso 1 1 calc R . . C26C C 0.5242(8) -0.0437(6) 1.1327(4) 0.068(4) Uani 1 1 d U . . H26J H 0.4753 -0.0580 1.1114 0.102 Uiso 1 1 calc R . . H26K H 0.4914 -0.0379 1.1654 0.102 Uiso 1 1 calc R . . H26L H 0.5779 -0.0841 1.1393 0.102 Uiso 1 1 calc R . . C27C C 0.5791(8) 0.1603(6) 0.9700(4) 0.057(3) Uani 1 1 d U . . H27J H 0.5305 0.1303 0.9583 0.085 Uiso 1 1 calc R . . H27K H 0.6430 0.1571 0.9505 0.085 Uiso 1 1 calc R . . H27L H 0.5544 0.2143 0.9644 0.085 Uiso 1 1 calc R . . Pd1D Pd 0.27130(6) 0.66589(5) 0.45774(3) 0.0349(2) Uani 1 1 d U . . Cl1D Cl 0.11138(19) 0.62638(15) 0.46177(9) 0.0421(7) Uani 1 1 d U . . O1D O 0.2998(5) 0.5815(4) 0.5162(2) 0.0390(18) Uani 1 1 d U . . N1D N 0.4046(6) 0.7076(5) 0.4550(3) 0.035(2) Uani 1 1 d U . . N2D N 0.2516(7) 0.7572(5) 0.3994(3) 0.040(2) Uani 1 1 d U . . C1D C 0.3884(8) 0.5618(6) 0.5355(4) 0.036(2) Uani 1 1 d U . . C2D C 0.4762(8) 0.6026(6) 0.5218(4) 0.037(2) Uani 1 1 d U . . C3D C 0.5612(8) 0.5702(6) 0.5471(4) 0.047(3) Uani 1 1 d U . . H3D H 0.6210 0.5970 0.5380 0.056 Uiso 1 1 calc R . . C4D C 0.5656(9) 0.5034(7) 0.5836(4) 0.053(3) Uani 1 1 d U . . H4D H 0.6271 0.4836 0.5985 0.064 Uiso 1 1 calc R . . C5D C 0.4803(8) 0.4648(6) 0.5987(4) 0.048(3) Uani 1 1 d U . . H5D H 0.4821 0.4189 0.6252 0.058 Uiso 1 1 calc R . . C6D C 0.3906(8) 0.4919(6) 0.5758(4) 0.039(3) Uani 1 1 d U . . C7D C 0.2988(8) 0.4476(6) 0.5939(4) 0.038(3) Uani 1 1 d U . . C8D C 0.2758(8) 0.4227(6) 0.6449(4) 0.051(3) Uani 1 1 d U . . H8D H 0.3174 0.4348 0.6690 0.061 Uiso 1 1 calc R . . C9D C 0.1916(10) 0.3792(6) 0.6630(5) 0.064(4) Uani 1 1 d U . . H9D H 0.1754 0.3630 0.6989 0.076 Uiso 1 1 calc R . . C10D C 0.1335(9) 0.3606(6) 0.6277(5) 0.063(4) Uani 1 1 d U . . H10D H 0.0771 0.3304 0.6388 0.076 Uiso 1 1 calc R . . C11D C 0.1577(9) 0.3858(6) 0.5770(5) 0.058(3) Uani 1 1 d U . . H11D H 0.1178 0.3724 0.5527 0.069 Uiso 1 1 calc R . . C12D C 0.2377(8) 0.4301(6) 0.5594(4) 0.042(3) Uani 1 1 d U . . H12D H 0.2511 0.4486 0.5234 0.051 Uiso 1 1 calc R . . C13D C 0.4820(8) 0.6761(6) 0.4831(4) 0.038(3) Uani 1 1 d U . . C14D C 0.5677(8) 0.7184(7) 0.4766(4) 0.059(3) Uani 1 1 d U . . H14D H 0.6241 0.6974 0.4959 0.071 Uiso 1 1 calc R . . C15D C 0.5727(9) 0.7889(7) 0.4434(4) 0.061(4) Uani 1 1 d U . . H15D H 0.6320 0.8165 0.4398 0.073 Uiso 1 1 calc R . . C16D C 0.4919(9) 0.8202(7) 0.4150(4) 0.061(3) Uani 1 1 d U . . H16D H 0.4929 0.8700 0.3924 0.073 Uiso 1 1 calc R . . C17D C 0.4101(8) 0.7769(6) 0.4207(4) 0.039(3) Uani 1 1 d U . . C18D C 0.3242(8) 0.8015(6) 0.3913(4) 0.040(3) Uani 1 1 d U . . H18D H 0.3212 0.8494 0.3665 0.048 Uiso 1 1 calc R . . C19D C 0.1646(8) 0.7804(6) 0.3694(4) 0.037(2) Uani 1 1 d U . . C20D C 0.1510(8) 0.7458(6) 0.3296(4) 0.042(3) Uani 1 1 d U . . C21D C 0.0678(8) 0.7706(7) 0.2989(4) 0.051(3) Uani 1 1 d U . . H21D H 0.0569 0.7475 0.2713 0.061 Uiso 1 1 calc R . . C22D C 0.0036(9) 0.8278(7) 0.3092(4) 0.051(3) Uani 1 1 d U . . C23D C 0.0153(8) 0.8612(6) 0.3499(4) 0.048(3) Uani 1 1 d U . . H23D H -0.0321 0.8999 0.3566 0.058 Uiso 1 1 calc R . . C24D C 0.0955(8) 0.8388(6) 0.3812(4) 0.041(3) Uani 1 1 d U . . C25D C 0.2189(7) 0.6802(6) 0.3204(4) 0.050(3) Uani 1 1 d U . . H25M H 0.2882 0.6957 0.3165 0.075 Uiso 1 1 calc R . . H25N H 0.2012 0.6660 0.2890 0.075 Uiso 1 1 calc R . . H25O H 0.2120 0.6358 0.3498 0.075 Uiso 1 1 calc R . . C26D C -0.0833(9) 0.8543(7) 0.2754(4) 0.090(5) Uani 1 1 d U . . H26M H -0.0614 0.8566 0.2394 0.134 Uiso 1 1 calc R . . H26N H -0.1085 0.9056 0.2790 0.134 Uiso 1 1 calc R . . H26O H -0.1365 0.8179 0.2858 0.134 Uiso 1 1 calc R . . C27D C 0.1084(8) 0.8709(6) 0.4257(3) 0.048(3) Uani 1 1 d U . . H27M H 0.0507 0.9055 0.4303 0.072 Uiso 1 1 calc R . . H27N H 0.1693 0.8997 0.4200 0.072 Uiso 1 1 calc R . . H27O H 0.1138 0.8288 0.4566 0.072 Uiso 1 1 calc R . . C28 C 0.7447(9) 0.9496(7) 0.5037(4) 0.083(4) Uani 1 1 d U . . H28A H 0.7357 0.9036 0.5324 0.100 Uiso 1 1 calc R . . H28B H 0.7846 0.9860 0.5158 0.100 Uiso 1 1 calc R . . Cl2 Cl 0.6306(3) 0.9926(2) 0.48650(16) 0.1400(19) Uani 1 1 d U . . Cl3 Cl 0.8078(3) 0.9223(2) 0.45204(14) 0.1099(14) Uani 1 1 d U . . C29 C 0.5595(12) 0.4221(9) 0.8224(7) 0.143(6) Uani 1 1 d U . . H29A H 0.5705 0.4736 0.8283 0.172 Uiso 1 1 calc R . . H29B H 0.4913 0.4084 0.8365 0.172 Uiso 1 1 calc R . . Cl4 Cl 0.5632(4) 0.4300(2) 0.75481(19) 0.1400(18) Uani 1 1 d U . . Cl5 Cl 0.6372(3) 0.3614(3) 0.85475(19) 0.148(2) Uani 1 1 d U . . C30 C 0.6864(9) 0.0907(7) 0.3411(5) 0.094(5) Uani 1 1 d U . . H30A H 0.7023 0.0831 0.3776 0.112 Uiso 1 1 calc R . . H30B H 0.6917 0.1462 0.3246 0.112 Uiso 1 1 calc R . . Cl6 Cl 0.5646(3) 0.0664(2) 0.33856(18) 0.1315(17) Uani 1 1 d U . . Cl7 Cl 0.7757(3) 0.0376(2) 0.31088(17) 0.1276(17) Uani 1 1 d U . . 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 0.0453(6) 0.0239(5) 0.0284(5) -0.0007(4) -0.0028(4) -0.0073(4) Cl1 0.053(2) 0.0242(15) 0.0322(16) 0.0003(12) -0.0003(14) -0.0128(14) O1 0.037(4) 0.031(4) 0.032(4) -0.002(3) 0.005(3) -0.016(3) N1 0.044(6) 0.018(4) 0.022(4) 0.006(3) -0.003(4) -0.008(4) N2 0.048(6) 0.028(5) 0.025(4) 0.005(3) 0.000(4) -0.013(4) C1 0.024(6) 0.025(5) 0.032(5) -0.005(4) 0.009(5) 0.001(4) C2 0.037(7) 0.034(6) 0.027(5) -0.003(4) 0.004(5) -0.007(5) C3 0.059(8) 0.017(6) 0.038(5) -0.007(4) 0.007(6) -0.006(5) C4 0.058(8) 0.037(6) 0.025(6) -0.007(5) 0.009(5) -0.011(6) C5 0.051(8) 0.031(6) 0.032(5) -0.004(5) 0.001(6) -0.009(5) C6 0.039(7) 0.031(5) 0.023(5) -0.003(4) 0.001(5) 0.003(5) C7 0.039(7) 0.030(5) 0.021(6) -0.009(4) -0.001(5) -0.001(5) C8 0.060(8) 0.045(7) 0.035(7) -0.018(5) -0.010(5) -0.004(5) C9 0.063(9) 0.071(8) 0.047(8) -0.017(6) -0.019(6) -0.020(6) C10 0.083(9) 0.060(7) 0.035(8) -0.011(5) -0.003(6) -0.030(7) C11 0.063(8) 0.029(6) 0.027(6) 0.003(5) -0.002(5) -0.012(6) C12 0.041(7) 0.031(6) 0.026(6) -0.003(4) 0.005(5) -0.007(5) C13 0.040(7) 0.021(5) 0.040(5) 0.003(4) -0.006(5) -0.006(5) C14 0.053(8) 0.028(6) 0.036(6) 0.004(5) -0.003(5) -0.012(5) C15 0.078(9) 0.024(6) 0.035(7) -0.004(4) -0.007(6) -0.018(6) C16 0.076(9) 0.039(6) 0.048(7) 0.002(5) -0.030(6) -0.023(6) C17 0.065(8) 0.028(5) 0.034(6) 0.004(4) -0.006(5) -0.017(5) C18 0.063(8) 0.039(6) 0.033(6) 0.002(5) -0.016(6) -0.012(6) C19 0.051(7) 0.030(6) 0.035(5) 0.009(4) -0.012(5) -0.011(5) C20 0.041(7) 0.035(6) 0.039(6) 0.001(5) -0.004(5) -0.012(5) C21 0.060(8) 0.039(7) 0.028(6) -0.003(5) 0.007(5) -0.014(5) C22 0.055(8) 0.028(6) 0.042(6) 0.003(5) -0.005(6) -0.015(5) C23 0.046(8) 0.029(6) 0.054(6) 0.002(5) -0.005(6) 0.002(5) C24 0.047(7) 0.025(6) 0.046(6) -0.001(5) -0.007(5) -0.010(5) C25 0.061(9) 0.048(8) 0.054(8) 0.005(6) -0.005(6) -0.004(6) C26 0.086(10) 0.041(8) 0.058(7) 0.010(6) -0.005(7) -0.016(7) C27 0.072(9) 0.048(8) 0.040(6) -0.003(6) -0.004(6) -0.004(7) Pd1A 0.0444(6) 0.0318(5) 0.0325(5) -0.0045(4) 0.0062(5) 0.0006(5) Cl1A 0.047(2) 0.051(2) 0.0424(18) -0.0145(15) 0.0020(15) -0.0040(15) O1A 0.046(5) 0.039(5) 0.043(4) -0.012(4) 0.017(4) -0.004(4) N1A 0.047(5) 0.023(5) 0.024(5) 0.003(4) -0.001(4) 0.007(4) N2A 0.047(5) 0.036(6) 0.026(5) 0.001(4) 0.004(4) 0.002(4) C1A 0.042(6) 0.020(6) 0.034(6) 0.002(5) 0.003(5) 0.010(5) C2A 0.046(6) 0.023(6) 0.036(6) 0.002(5) -0.002(5) 0.006(5) C3A 0.053(7) 0.037(7) 0.047(7) -0.014(6) 0.006(6) 0.004(6) C4A 0.055(7) 0.036(7) 0.042(7) -0.005(5) 0.010(5) -0.008(6) C5A 0.051(7) 0.035(7) 0.023(6) 0.002(5) 0.009(5) -0.001(6) C6A 0.051(6) 0.022(6) 0.029(6) 0.006(4) 0.009(5) -0.002(5) C7A 0.043(6) 0.048(7) 0.031(6) -0.003(5) 0.013(5) -0.005(5) C8A 0.041(7) 0.081(9) 0.041(7) -0.038(6) 0.013(5) 0.004(6) C9A 0.077(9) 0.099(10) 0.043(8) -0.036(7) 0.010(7) -0.002(8) C10A 0.071(9) 0.100(11) 0.036(8) -0.021(7) 0.009(7) -0.021(8) C11A 0.065(9) 0.080(10) 0.046(9) 0.004(7) -0.008(6) -0.002(7) C12A 0.050(7) 0.055(8) 0.038(7) -0.002(6) 0.009(5) 0.008(6) C13A 0.054(6) 0.011(6) 0.042(6) 0.000(4) 0.002(5) 0.001(5) C14A 0.072(8) 0.038(7) 0.046(7) -0.002(5) 0.008(6) -0.019(6) C15A 0.071(9) 0.050(8) 0.052(8) -0.019(6) -0.005(6) -0.015(6) C16A 0.062(8) 0.025(7) 0.047(7) -0.005(5) 0.002(6) -0.005(6) C17A 0.062(7) 0.028(6) 0.027(6) -0.002(5) 0.010(5) -0.010(5) C18A 0.053(7) 0.022(6) 0.035(6) -0.004(5) 0.005(5) 0.007(5) C19A 0.047(6) 0.041(7) 0.024(6) -0.009(4) 0.003(4) 0.000(5) C20A 0.046(6) 0.040(7) 0.035(7) -0.008(5) -0.001(5) -0.002(5) C21A 0.055(7) 0.058(8) 0.046(7) -0.016(6) -0.003(6) -0.013(6) C22A 0.040(6) 0.087(9) 0.048(8) -0.020(6) 0.011(6) -0.009(7) C23A 0.041(7) 0.083(9) 0.054(8) -0.015(6) 0.004(6) 0.007(6) C24A 0.051(7) 0.060(8) 0.044(7) -0.003(5) 0.001(6) 0.007(6) C25A 0.057(7) 0.048(8) 0.050(8) 0.001(6) -0.008(6) -0.012(6) C26A 0.048(8) 0.116(12) 0.088(10) -0.023(8) 0.011(8) -0.027(8) C27A 0.073(10) 0.072(9) 0.046(8) 0.002(5) -0.007(7) 0.015(7) Pd1B 0.0428(6) 0.0303(5) 0.0402(6) -0.0048(4) -0.0001(5) 0.0016(4) Cl1B 0.051(2) 0.0458(19) 0.0465(19) -0.0132(15) -0.0090(15) 0.0047(15) O1B 0.041(5) 0.025(4) 0.038(4) -0.001(3) 0.002(3) 0.001(3) N1B 0.027(5) 0.034(5) 0.046(5) -0.011(4) 0.007(4) -0.010(4) N2B 0.035(6) 0.036(5) 0.039(5) -0.006(4) 0.008(4) -0.005(4) C1B 0.035(6) 0.017(5) 0.032(6) 0.007(4) 0.011(4) -0.010(4) C2B 0.033(6) 0.031(6) 0.036(6) -0.005(5) 0.015(4) -0.006(4) C3B 0.057(7) 0.025(6) 0.033(6) 0.004(5) -0.001(5) -0.006(5) C4B 0.065(8) 0.036(7) 0.053(8) -0.012(6) -0.007(6) -0.005(6) C5B 0.042(7) 0.033(7) 0.049(7) -0.010(5) 0.010(5) 0.002(5) C6B 0.045(6) 0.025(6) 0.035(6) 0.002(4) 0.009(5) -0.010(4) C7B 0.036(6) 0.027(6) 0.048(7) -0.004(5) 0.008(5) 0.003(4) C8B 0.043(7) 0.032(6) 0.062(8) -0.001(6) 0.005(6) -0.001(5) C9B 0.040(7) 0.048(7) 0.088(10) -0.001(7) 0.006(7) 0.012(6) C10B 0.028(7) 0.062(8) 0.068(8) 0.001(7) -0.004(6) 0.005(5) C11B 0.043(7) 0.060(7) 0.064(8) -0.011(7) -0.002(6) 0.001(6) C12B 0.048(7) 0.026(6) 0.050(7) -0.009(5) -0.003(6) 0.007(5) C13B 0.030(6) 0.025(6) 0.040(6) -0.001(5) 0.007(4) -0.011(4) C14B 0.053(8) 0.049(8) 0.061(8) -0.023(6) -0.018(6) 0.001(5) C15B 0.053(8) 0.065(9) 0.063(8) -0.018(6) -0.022(7) 0.016(6) C16B 0.054(8) 0.045(8) 0.074(9) -0.013(6) -0.013(6) 0.016(6) C17B 0.040(7) 0.039(7) 0.050(7) -0.013(5) 0.002(5) -0.004(5) C18B 0.045(8) 0.042(7) 0.053(8) -0.013(6) 0.009(5) 0.008(5) C19B 0.045(8) 0.045(7) 0.058(7) -0.017(6) 0.008(5) 0.000(5) C20B 0.048(8) 0.053(8) 0.055(7) -0.024(6) 0.010(6) 0.017(5) C21B 0.050(8) 0.065(9) 0.052(7) -0.021(6) 0.006(6) 0.008(6) C22B 0.045(8) 0.061(8) 0.045(7) -0.015(6) -0.007(6) 0.020(6) C23B 0.050(8) 0.057(8) 0.049(7) -0.012(6) -0.016(5) 0.005(6) C24B 0.049(8) 0.041(7) 0.042(7) -0.010(5) -0.011(5) 0.009(5) C25B 0.064(10) 0.091(11) 0.098(11) -0.039(8) 0.033(8) -0.023(7) C26B 0.061(9) 0.056(8) 0.067(8) -0.029(6) 0.009(7) 0.005(7) C27B 0.060(8) 0.036(7) 0.052(7) 0.004(6) 0.002(6) -0.007(6) Pd1C 0.0466(6) 0.0240(5) 0.0350(5) -0.0021(4) 0.0022(5) 0.0006(4) Cl1C 0.065(2) 0.0229(16) 0.0541(19) 0.0010(14) 0.0081(16) 0.0039(15) O1C 0.035(4) 0.032(4) 0.034(4) -0.003(3) 0.001(3) 0.008(3) N1C 0.041(6) 0.024(4) 0.035(5) 0.000(4) 0.005(4) 0.010(4) N2C 0.049(5) 0.024(4) 0.029(5) -0.002(4) 0.001(4) -0.001(4) C1C 0.042(7) 0.022(5) 0.038(5) -0.008(4) 0.001(5) -0.001(5) C2C 0.038(7) 0.023(5) 0.025(5) -0.004(4) 0.001(4) -0.004(4) C3C 0.051(8) 0.029(6) 0.039(6) -0.003(5) -0.001(5) -0.003(5) C4C 0.060(8) 0.035(6) 0.023(6) -0.008(5) -0.007(5) 0.000(6) C5C 0.042(7) 0.037(6) 0.041(6) -0.014(5) 0.008(6) -0.010(5) C6C 0.035(6) 0.025(5) 0.039(6) -0.012(4) -0.003(5) -0.009(4) C7C 0.039(7) 0.039(5) 0.031(6) -0.020(4) -0.010(5) 0.000(5) C8C 0.042(7) 0.055(7) 0.044(7) -0.033(6) -0.003(5) 0.007(5) C9C 0.036(7) 0.068(8) 0.069(9) -0.036(7) -0.014(6) 0.013(6) C10C 0.051(8) 0.056(7) 0.069(10) -0.029(6) -0.028(6) 0.024(7) C11C 0.064(8) 0.046(6) 0.043(7) -0.008(6) -0.020(6) 0.013(6) C12C 0.049(7) 0.033(6) 0.042(7) -0.012(5) -0.014(5) 0.009(5) C13C 0.033(6) 0.027(5) 0.036(6) -0.006(4) -0.005(4) 0.002(5) C14C 0.056(8) 0.027(5) 0.031(6) -0.002(5) 0.010(5) -0.004(5) C15C 0.060(8) 0.028(6) 0.037(7) -0.008(5) 0.000(5) -0.002(5) C16C 0.049(7) 0.030(5) 0.027(6) -0.008(5) 0.004(5) 0.004(5) C17C 0.044(7) 0.030(5) 0.030(6) -0.005(5) -0.003(5) 0.008(5) C18C 0.047(7) 0.039(5) 0.023(6) -0.002(5) 0.005(5) 0.002(5) C19C 0.045(7) 0.027(5) 0.032(5) 0.000(4) 0.005(5) 0.008(5) C20C 0.048(8) 0.034(6) 0.031(5) -0.007(5) 0.007(5) 0.003(5) C21C 0.037(7) 0.030(6) 0.041(6) 0.013(5) -0.007(5) 0.017(5) C22C 0.040(8) 0.034(7) 0.051(7) 0.007(5) 0.008(6) 0.003(5) C23C 0.050(8) 0.035(6) 0.053(6) -0.005(5) -0.001(6) -0.001(5) C24C 0.047(8) 0.027(6) 0.041(6) -0.005(5) 0.003(5) 0.002(5) C25C 0.066(9) 0.042(7) 0.038(7) 0.001(6) -0.003(6) 0.001(6) C26C 0.061(9) 0.035(7) 0.093(9) 0.008(6) 0.009(8) 0.004(6) C27C 0.074(9) 0.050(8) 0.048(6) -0.010(6) -0.013(7) -0.010(7) Pd1D 0.0366(6) 0.0343(5) 0.0324(5) -0.0050(4) 0.0030(4) -0.0065(4) Cl1D 0.0390(18) 0.0467(19) 0.0376(17) -0.0012(14) -0.0011(14) -0.0124(15) O1D 0.031(4) 0.031(4) 0.050(5) 0.001(3) 0.003(3) -0.007(3) N1D 0.027(4) 0.042(5) 0.039(5) -0.016(4) 0.012(4) 0.001(4) N2D 0.050(5) 0.029(5) 0.037(5) 0.000(4) 0.003(4) -0.012(4) C1D 0.037(6) 0.035(6) 0.036(6) -0.011(4) 0.001(5) 0.001(5) C2D 0.032(6) 0.053(7) 0.029(6) -0.014(4) 0.003(5) -0.007(5) C3D 0.028(6) 0.048(7) 0.062(8) -0.013(5) 0.005(5) 0.009(5) C4D 0.046(7) 0.061(8) 0.052(8) -0.012(6) -0.006(6) 0.005(6) C5D 0.058(7) 0.045(7) 0.038(7) 0.000(5) -0.011(6) 0.002(6) C6D 0.049(6) 0.035(6) 0.030(6) -0.002(4) -0.001(5) 0.001(5) C7D 0.048(6) 0.030(6) 0.034(6) -0.005(5) 0.003(5) 0.006(5) C8D 0.058(8) 0.048(8) 0.039(6) 0.002(6) 0.009(6) 0.010(6) C9D 0.085(10) 0.040(8) 0.056(7) 0.004(6) 0.018(6) -0.004(7) C10D 0.072(9) 0.032(7) 0.078(8) -0.001(7) 0.020(7) -0.012(6) C11D 0.062(8) 0.043(8) 0.072(7) -0.024(7) 0.012(7) -0.008(6) C12D 0.043(7) 0.036(7) 0.044(6) -0.007(6) 0.008(5) 0.003(5) C13D 0.032(6) 0.053(7) 0.029(6) -0.010(4) 0.010(5) -0.005(5) C14D 0.028(6) 0.070(8) 0.074(9) -0.009(6) 0.003(6) -0.008(6) C15D 0.041(7) 0.073(9) 0.068(9) -0.010(6) 0.005(6) -0.036(7) C16D 0.058(8) 0.058(8) 0.062(9) 0.001(6) 0.003(6) -0.020(6) C17D 0.050(6) 0.035(6) 0.032(6) -0.006(5) -0.002(5) -0.009(5) C18D 0.048(6) 0.039(6) 0.036(7) -0.011(5) 0.005(5) -0.013(5) C19D 0.046(6) 0.039(7) 0.023(6) 0.003(4) 0.006(4) -0.013(5) C20D 0.048(7) 0.040(7) 0.034(7) 0.001(5) 0.012(5) -0.024(5) C21D 0.052(8) 0.061(8) 0.034(7) 0.005(6) 0.006(5) -0.029(5) C22D 0.039(7) 0.075(9) 0.031(7) 0.009(6) -0.007(5) -0.023(5) C23D 0.049(7) 0.050(7) 0.037(7) 0.010(5) -0.010(5) -0.008(6) C24D 0.042(7) 0.046(7) 0.033(6) -0.001(5) -0.005(5) -0.014(5) C25D 0.059(8) 0.054(8) 0.043(7) -0.022(6) 0.010(6) -0.021(5) C26D 0.063(9) 0.123(13) 0.079(10) -0.006(9) -0.033(7) -0.013(8) C27D 0.063(9) 0.045(8) 0.036(7) -0.008(5) -0.011(6) 0.007(6) C28 0.073(9) 0.088(11) 0.081(10) -0.013(8) 0.006(7) 0.013(8) Cl2 0.120(4) 0.111(4) 0.146(4) 0.036(3) 0.015(3) 0.047(3) Cl3 0.096(3) 0.134(4) 0.086(3) -0.005(3) 0.013(2) 0.001(3) C29 0.104(14) 0.136(16) 0.221(11) -0.119(13) 0.024(12) 0.017(10) Cl4 0.169(5) 0.075(3) 0.186(5) -0.044(3) -0.036(4) 0.002(3) Cl5 0.100(4) 0.189(6) 0.196(5) -0.119(4) -0.049(4) 0.005(4) C30 0.103(9) 0.076(10) 0.111(12) -0.045(9) 0.068(9) -0.053(8) Cl6 0.111(4) 0.116(4) 0.192(5) -0.081(4) -0.036(3) 0.008(3) Cl7 0.135(4) 0.099(4) 0.159(4) -0.059(3) 0.052(3) -0.035(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 O1 1.943(6) . ? Pd1 N1 1.959(7) . ? Pd1 N2 1.981(8) . ? Pd1 Cl1 2.287(3) . ? O1 C1 1.359(10) . ? N1 C13 1.332(10) . ? N1 C17 1.358(11) . ? N2 C18 1.257(11) . ? N2 C19 1.435(11) . ? C1 C2 1.413(12) . ? C1 C6 1.422(12) . ? C2 C3 1.428(12) . ? C2 C13 1.463(12) . ? C3 C4 1.336(11) . ? C3 H3 0.9500 . ? C4 C5 1.377(12) . ? C4 H4 0.9500 . ? C5 C6 1.360(11) . ? C5 H5 0.9500 . ? C6 C7 1.494(12) . ? C7 C8 1.352(12) . ? C7 C12 1.397(12) . ? C8 C9 1.368(13) . ? C8 H8 0.9500 . ? C9 C10 1.367(14) . ? C9 H9 0.9500 . ? C10 C11 1.371(13) . ? C10 H10 0.9500 . ? C11 C12 1.374(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.432(12) . ? C14 C15 1.336(12) . ? C14 H14 0.9500 . ? C15 C16 1.356(12) . ? C15 H15 0.9500 . ? C16 C17 1.386(12) . ? C16 H16 0.9500 . ? C17 C18 1.455(12) . ? C18 H18 0.9500 . ? C19 C20 1.375(12) . ? C19 C24 1.418(13) . ? C20 C21 1.390(12) . ? C20 C25 1.481(13) . ? C21 C22 1.389(13) . ? C21 H21 0.9500 . ? C22 C23 1.375(12) . ? C22 C26 1.502(12) . ? C23 C24 1.378(12) . ? C23 H23 0.9500 . ? C24 C27 1.500(12) . ? 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 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Pd1A O1A 1.934(6) . ? Pd1A N1A 1.969(8) . ? Pd1A N2A 1.999(8) . ? Pd1A Cl1A 2.285(3) . ? O1A C1A 1.306(11) . ? N1A C17A 1.353(11) . ? N1A C13A 1.363(11) . ? N2A C18A 1.305(11) . ? N2A C19A 1.446(12) . ? C1A C2A 1.426(13) . ? C1A C6A 1.427(12) . ? C2A C13A 1.448(12) . ? C2A C3A 1.448(13) . ? C3A C4A 1.340(11) . ? C3A H3A 0.9500 . ? C4A C5A 1.344(12) . ? C4A H4A 0.9500 . ? C5A C6A 1.391(13) . ? C5A H5A 0.9500 . ? C6A C7A 1.451(13) . ? C7A C12A 1.376(13) . ? C7A C8A 1.379(13) . ? C8A C9A 1.375(13) . ? C8A H8A 0.9500 . ? C9A C10A 1.385(15) . ? C9A H9A 0.9500 . ? C10A C11A 1.360(15) . ? C10A H10A 0.9500 . ? C11A C12A 1.381(14) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C14A 1.423(13) . ? C14A C15A 1.361(12) . ? C14A H14A 0.9500 . ? C15A C16A 1.388(13) . ? C15A H15A 0.9500 . ? C16A C17A 1.340(13) . ? C16A H16A 0.9500 . ? C17A C18A 1.430(13) . ? C18A H18A 0.9500 . ? C19A C24A 1.380(13) . ? C19A C20A 1.392(13) . ? C20A C21A 1.357(13) . ? C20A C25A 1.493(13) . ? C21A C22A 1.390(14) . ? C21A H21A 0.9500 . ? C22A C23A 1.376(14) . ? C22A C26A 1.484(14) . ? C23A C24A 1.354(14) . ? C23A H23A 0.9500 . ? C24A C27A 1.489(13) . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? Pd1B O1B 1.950(6) . ? Pd1B N1B 1.966(8) . ? Pd1B N2B 2.006(8) . ? Pd1B Cl1B 2.298(3) . ? O1B C1B 1.303(10) . ? N1B C13B 1.338(11) . ? N1B C17B 1.354(12) . ? N2B C18B 1.276(11) . ? N2B C19B 1.425(12) . ? C1B C2B 1.422(13) . ? C1B C6B 1.445(13) . ? C2B C3B 1.436(12) . ? C2B C13B 1.439(13) . ? C3B C4B 1.340(13) . ? C3B H3B 0.9500 . ? C4B C5B 1.394(13) . ? C4B H4B 0.9500 . ? C5B C6B 1.390(12) . ? C5B H5B 0.9500 . ? C6B C7B 1.484(13) . ? C7B C12B 1.369(13) . ? C7B C8B 1.399(12) . ? C8B C9B 1.349(13) . ? C8B H8B 0.9500 . ? C9B C10B 1.375(14) . ? C9B H9B 0.9500 . ? C10B C11B 1.369(13) . ? C10B H10B 0.9500 . ? C11B C12B 1.355(13) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.420(13) . ? C14B C15B 1.354(13) . ? C14B H14B 0.9500 . ? C15B C16B 1.394(13) . ? C15B H15B 0.9500 . ? C16B C17B 1.376(13) . ? C16B H16B 0.9500 . ? C17B C18B 1.400(13) . ? C18B H18B 0.9500 . ? C19B C24B 1.360(14) . ? C19B C20B 1.370(13) . ? C20B C21B 1.338(13) . ? C20B C25B 1.522(14) . ? C21B C22B 1.369(14) . ? C21B H21B 0.9500 . ? C22B C23B 1.415(13) . ? C22B C26B 1.534(13) . ? C23B C24B 1.408(13) . ? C23B H23B 0.9500 . ? C24B C27B 1.508(12) . ? C25B H25G 0.9800 . ? C25B H25H 0.9800 . ? C25B H25I 0.9800 . ? C26B H26G 0.9800 . ? C26B H26H 0.9800 . ? C26B H26I 0.9800 . ? C27B H27G 0.9800 . ? C27B H27H 0.9800 . ? C27B H27I 0.9800 . ? Pd1C O1C 1.946(6) . ? Pd1C N1C 1.973(8) . ? Pd1C N2C 1.990(8) . ? Pd1C Cl1C 2.286(3) . ? O1C C1C 1.346(10) . ? N1C C17C 1.342(11) . ? N1C C13C 1.345(11) . ? N2C C18C 1.283(11) . ? N2C C19C 1.449(11) . ? C1C C6C 1.399(12) . ? C1C C2C 1.429(12) . ? C2C C3C 1.395(11) . ? C2C C13C 1.456(12) . ? C3C C4C 1.367(11) . ? C3C H3C 0.9500 . ? C4C C5C 1.382(12) . ? C4C H4C 0.9500 . ? C5C C6C 1.362(12) . ? C5C H5C 0.9500 . ? C6C C7C 1.491(13) . ? C7C C12C 1.380(12) . ? C7C C8C 1.382(12) . ? C8C C9C 1.371(13) . ? C8C H8C 0.9500 . ? C9C C10C 1.364(14) . ? C9C H9C 0.9500 . ? C10C C11C 1.359(13) . ? C10C H10C 0.9500 . ? C11C C12C 1.375(12) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C C14C 1.428(12) . ? C14C C15C 1.362(11) . ? C14C H14C 0.9500 . ? C15C C16C 1.390(12) . ? C15C H15C 0.9500 . ? C16C C17C 1.372(12) . ? C16C H16C 0.9500 . ? C17C C18C 1.460(12) . ? C18C H18C 0.9500 . ? C19C C20C 1.364(12) . ? C19C C24C 1.376(13) . ? C20C C21C 1.392(12) . ? C20C C25C 1.490(12) . ? C21C C22C 1.370(13) . ? C21C H21C 0.9500 . ? C22C C23C 1.348(13) . ? C22C C26C 1.521(13) . ? C23C C24C 1.392(12) . ? C23C H23C 0.9500 . ? C24C C27C 1.497(12) . ? C25C H25J 0.9800 . ? C25C H25K 0.9800 . ? C25C H25L 0.9800 . ? C26C H26J 0.9800 . ? C26C H26K 0.9800 . ? C26C H26L 0.9800 . ? C27C H27J 0.9800 . ? C27C H27K 0.9800 . ? C27C H27L 0.9800 . ? Pd1D O1D 1.937(6) . ? Pd1D N1D 1.973(8) . ? Pd1D N2D 1.990(8) . ? Pd1D Cl1D 2.291(3) . ? O1D C1D 1.322(11) . ? N1D C13D 1.336(11) . ? N1D C17D 1.359(11) . ? N2D C18D 1.271(11) . ? N2D C19D 1.442(12) . ? C1D C2D 1.409(13) . ? C1D C6D 1.445(12) . ? C2D C3D 1.387(12) . ? C2D C13D 1.469(13) . ? C3D C4D 1.353(13) . ? C3D H3D 0.9500 . ? C4D C5D 1.364(13) . ? C4D H4D 0.9500 . ? C5D C6D 1.392(13) . ? C5D H5D 0.9500 . ? C6D C7D 1.500(13) . ? C7D C8D 1.351(12) . ? C7D C12D 1.374(13) . ? C8D C9D 1.408(14) . ? C8D H8D 0.9500 . ? C9D C10D 1.374(14) . ? C9D H9D 0.9500 . ? C10D C11D 1.348(13) . ? C10D H10D 0.9500 . ? C11D C12D 1.367(13) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D C14D 1.397(13) . ? C14D C15D 1.363(14) . ? C14D H14D 0.9500 . ? C15D C16D 1.377(14) . ? C15D H15D 0.9500 . ? C16D C17D 1.364(13) . ? C16D H16D 0.9500 . ? C17D C18D 1.426(13) . ? C18D H18D 0.9500 . ? C19D C20D 1.378(13) . ? C19D C24D 1.427(13) . ? C20D C21D 1.414(13) . ? C20D C25D 1.494(13) . ? C21D C22D 1.360(14) . ? C21D H21D 0.9500 . ? C22D C23D 1.379(13) . ? C22D C26D 1.505(13) . ? C23D C24D 1.386(13) . ? C23D H23D 0.9500 . ? C24D C27D 1.461(12) . ? C25D H25M 0.9800 . ? C25D H25N 0.9800 . ? C25D H25O 0.9800 . ? C26D H26M 0.9800 . ? C26D H26N 0.9800 . ? C26D H26O 0.9800 . ? C27D H27M 0.9800 . ? C27D H27N 0.9800 . ? C27D H27O 0.9800 . ? C28 Cl2 1.709(11) . ? C28 Cl3 1.724(11) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 Cl5 1.593(16) . ? C29 Cl4 1.778(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 Cl6 1.729(12) . ? C30 Cl7 1.754(11) . ? C30 H30A 0.9900 . ? C30 H30B 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 O1 Pd1 N1 93.5(3) . . ? O1 Pd1 N2 176.0(3) . . ? N1 Pd1 N2 82.5(3) . . ? O1 Pd1 Cl1 88.66(19) . . ? N1 Pd1 Cl1 175.3(2) . . ? N2 Pd1 Cl1 95.4(2) . . ? C1 O1 Pd1 123.3(6) . . ? C13 N1 C17 120.1(8) . . ? C13 N1 Pd1 127.2(7) . . ? C17 N1 Pd1 112.5(6) . . ? C18 N2 C19 120.0(9) . . ? C18 N2 Pd1 112.3(7) . . ? C19 N2 Pd1 127.7(7) . . ? O1 C1 C2 123.9(9) . . ? O1 C1 C6 114.9(9) . . ? C2 C1 C6 121.2(9) . . ? C1 C2 C3 115.8(9) . . ? C1 C2 C13 125.0(9) . . ? C3 C2 C13 119.1(9) . . ? C4 C3 C2 123.0(10) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 119.3(10) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 123.0(10) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 117.7(10) . . ? C5 C6 C7 120.8(9) . . ? C1 C6 C7 121.5(9) . . ? C8 C7 C12 118.0(10) . . ? C8 C7 C6 121.5(10) . . ? C12 C7 C6 120.5(9) . . ? C7 C8 C9 121.0(11) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 121.9(12) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 117.5(12) . . ? C11 C10 H10 121.3 . . ? C9 C10 H10 121.3 . . ? C10 C11 C12 121.2(11) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 120.2(10) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? N1 C13 C14 116.3(9) . . ? N1 C13 C2 121.5(9) . . ? C14 C13 C2 122.2(9) . . ? C15 C14 C13 123.6(10) . . ? C15 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C14 C15 C16 118.7(10) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C16 C17 118.2(10) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? N1 C17 C16 122.8(9) . . ? N1 C17 C18 112.4(9) . . ? C16 C17 C18 124.7(10) . . ? N2 C18 C17 119.3(10) . . ? N2 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C24 121.7(10) . . ? C20 C19 N2 121.1(10) . . ? C24 C19 N2 117.2(10) . . ? C19 C20 C21 118.2(10) . . ? C19 C20 C25 121.0(10) . . ? C21 C20 C25 120.7(10) . . ? C22 C21 C20 122.4(10) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C23 C22 C21 117.0(10) . . ? C23 C22 C26 121.6(11) . . ? C21 C22 C26 121.3(10) . . ? C22 C23 C24 124.0(11) . . ? C22 C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? C23 C24 C19 116.6(10) . . ? C23 C24 C27 121.9(10) . . ? C19 C24 C27 121.4(10) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O1A Pd1A N1A 93.9(3) . . ? O1A Pd1A N2A 176.0(3) . . ? N1A Pd1A N2A 82.5(3) . . ? O1A Pd1A Cl1A 87.7(2) . . ? N1A Pd1A Cl1A 177.3(2) . . ? N2A Pd1A Cl1A 95.9(3) . . ? C1A O1A Pd1A 126.4(7) . . ? C17A N1A C13A 120.2(9) . . ? C17A N1A Pd1A 113.9(7) . . ? C13A N1A Pd1A 125.8(7) . . ? C18A N2A C19A 121.1(9) . . ? C18A N2A Pd1A 110.3(7) . . ? C19A N2A Pd1A 128.4(7) . . ? O1A C1A C2A 126.6(10) . . ? O1A C1A C6A 114.2(10) . . ? C2A C1A C6A 119.2(10) . . ? C1A C2A C13A 123.5(10) . . ? C1A C2A C3A 116.6(10) . . ? C13A C2A C3A 119.9(10) . . ? C4A C3A C2A 121.5(11) . . ? C4A C3A H3A 119.3 . . ? C2A C3A H3A 119.3 . . ? C3A C4A C5A 121.8(11) . . ? C3A C4A H4A 119.1 . . ? C5A C4A H4A 119.1 . . ? C4A C5A C6A 121.3(10) . . ? C4A C5A H5A 119.3 . . ? C6A C5A H5A 119.3 . . ? C5A C6A C1A 119.2(10) . . ? C5A C6A C7A 119.5(10) . . ? C1A C6A C7A 121.3(10) . . ? C12A C7A C8A 115.6(11) . . ? C12A C7A C6A 121.4(11) . . ? C8A C7A C6A 122.9(11) . . ? C9A C8A C7A 121.3(12) . . ? C9A C8A H8A 119.3 . . ? C7A C8A H8A 119.3 . . ? C10A C9A C8A 122.4(12) . . ? C10A C9A H9A 118.8 . . ? C8A C9A H9A 118.8 . . ? C11A C10A C9A 116.4(13) . . ? C11A C10A H10A 121.8 . . ? C9A C10A H10A 121.8 . . ? C10A C11A C12A 121.0(13) . . ? C10A C11A H11A 119.5 . . ? C12A C11A H11A 119.5 . . ? C7A C12A C11A 122.9(12) . . ? C7A C12A H12A 118.5 . . ? C11A C12A H12A 118.5 . . ? N1A C13A C14A 115.2(10) . . ? N1A C13A C2A 123.1(10) . . ? C14A C13A C2A 121.7(10) . . ? C15A C14A C13A 123.2(11) . . ? C15A C14A H14A 118.4 . . ? C13A C14A H14A 118.4 . . ? C14A C15A C16A 119.3(11) . . ? C14A C15A H15A 120.3 . . ? C16A C15A H15A 120.3 . . ? C17A C16A C15A 116.4(11) . . ? C17A C16A H16A 121.8 . . ? C15A C16A H16A 121.8 . . ? C16A C17A N1A 125.6(11) . . ? C16A C17A C18A 122.0(11) . . ? N1A C17A C18A 112.5(10) . . ? N2A C18A C17A 120.8(10) . . ? N2A C18A H18A 119.6 . . ? C17A C18A H18A 119.6 . . ? C24A C19A C20A 121.9(11) . . ? C24A C19A N2A 120.7(10) . . ? C20A C19A N2A 117.4(10) . . ? C21A C20A C19A 117.9(11) . . ? C21A C20A C25A 120.8(11) . . ? C19A C20A C25A 121.1(10) . . ? C20A C21A C22A 123.4(12) . . ? C20A C21A H21A 118.3 . . ? C22A C21A H21A 118.3 . . ? C23A C22A C21A 114.6(12) . . ? C23A C22A C26A 124.0(12) . . ? C21A C22A C26A 121.4(12) . . ? C24A C23A C22A 126.0(13) . . ? C24A C23A H23A 117.0 . . ? C22A C23A H23A 117.0 . . ? C23A C24A C19A 116.1(12) . . ? C23A C24A C27A 121.1(12) . . ? C19A C24A C27A 122.8(11) . . ? C20A C25A H25D 109.5 . . ? C20A C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C20A C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C22A C26A H26D 109.5 . . ? C22A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C22A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C24A C27A H27D 109.5 . . ? C24A C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C24A C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? O1B Pd1B N1B 93.7(3) . . ? O1B Pd1B N2B 173.9(3) . . ? N1B Pd1B N2B 82.2(3) . . ? O1B Pd1B Cl1B 88.5(2) . . ? N1B Pd1B Cl1B 177.6(2) . . ? N2B Pd1B Cl1B 95.7(3) . . ? C1B O1B Pd1B 126.2(7) . . ? C13B N1B C17B 122.4(10) . . ? C13B N1B Pd1B 126.1(7) . . ? C17B N1B Pd1B 111.5(7) . . ? C18B N2B C19B 118.5(9) . . ? C18B N2B Pd1B 111.3(7) . . ? C19B N2B Pd1B 130.2(7) . . ? O1B C1B C2B 125.1(9) . . ? O1B C1B C6B 115.9(10) . . ? C2B C1B C6B 119.0(10) . . ? C1B C2B C3B 115.4(10) . . ? C1B C2B C13B 125.3(10) . . ? C3B C2B C13B 119.2(10) . . ? C4B C3B C2B 125.9(11) . . ? C4B C3B H3B 117.0 . . ? C2B C3B H3B 117.0 . . ? C3B C4B C5B 117.4(11) . . ? C3B C4B H4B 121.3 . . ? C5B C4B H4B 121.3 . . ? C6B C5B C4B 121.7(10) . . ? C6B C5B H5B 119.2 . . ? C4B C5B H5B 119.2 . . ? C5B C6B C1B 119.8(11) . . ? C5B C6B C7B 118.3(10) . . ? C1B C6B C7B 121.9(10) . . ? C12B C7B C8B 117.1(11) . . ? C12B C7B C6B 122.1(10) . . ? C8B C7B C6B 120.3(10) . . ? C9B C8B C7B 120.9(12) . . ? C9B C8B H8B 119.6 . . ? C7B C8B H8B 119.6 . . ? C8B C9B C10B 121.6(12) . . ? C8B C9B H9B 119.2 . . ? C10B C9B H9B 119.2 . . ? C11B C10B C9B 117.3(12) . . ? C11B C10B H10B 121.4 . . ? C9B C10B H10B 121.4 . . ? C12B C11B C10B 121.9(12) . . ? C12B C11B H11B 119.0 . . ? C10B C11B H11B 119.0 . . ? C11B C12B C7B 121.2(11) . . ? C11B C12B H12B 119.4 . . ? C7B C12B H12B 119.4 . . ? N1B C13B C14B 115.8(10) . . ? N1B C13B C2B 122.7(10) . . ? C14B C13B C2B 121.4(10) . . ? C15B C14B C13B 124.6(11) . . ? C15B C14B H14B 117.7 . . ? C13B C14B H14B 117.7 . . ? C14B C15B C16B 116.0(11) . . ? C14B C15B H15B 122.0 . . ? C16B C15B H15B 122.0 . . ? C17B C16B C15B 120.5(11) . . ? C17B C16B H16B 119.8 . . ? C15B C16B H16B 119.8 . . ? N1B C17B C16B 120.6(11) . . ? N1B C17B C18B 115.8(11) . . ? C16B C17B C18B 123.5(11) . . ? N2B C18B C17B 119.2(11) . . ? N2B C18B H18B 120.4 . . ? C17B C18B H18B 120.4 . . ? C24B C19B C20B 122.5(12) . . ? C24B C19B N2B 117.7(10) . . ? C20B C19B N2B 119.8(11) . . ? C21B C20B C19B 118.4(13) . . ? C21B C20B C25B 120.5(11) . . ? C19B C20B C25B 121.1(11) . . ? C20B C21B C22B 124.2(12) . . ? C20B C21B H21B 117.9 . . ? C22B C21B H21B 117.9 . . ? C21B C22B C23B 116.5(11) . . ? C21B C22B C26B 124.3(11) . . ? C23B C22B C26B 119.2(11) . . ? C24B C23B C22B 120.4(12) . . ? C24B C23B H23B 119.8 . . ? C22B C23B H23B 119.8 . . ? C19B C24B C23B 117.8(11) . . ? C19B C24B C27B 123.2(10) . . ? C23B C24B C27B 119.0(11) . . ? C20B C25B H25G 109.5 . . ? C20B C25B H25H 109.5 . . ? H25G C25B H25H 109.5 . . ? C20B C25B H25I 109.5 . . ? H25G C25B H25I 109.5 . . ? H25H C25B H25I 109.5 . . ? C22B C26B H26G 109.5 . . ? C22B C26B H26H 109.5 . . ? H26G C26B H26H 109.5 . . ? C22B C26B H26I 109.5 . . ? H26G C26B H26I 109.5 . . ? H26H C26B H26I 109.5 . . ? C24B C27B H27G 109.5 . . ? C24B C27B H27H 109.5 . . ? H27G C27B H27H 109.5 . . ? C24B C27B H27I 109.5 . . ? H27G C27B H27I 109.5 . . ? H27H C27B H27I 109.5 . . ? O1C Pd1C N1C 92.0(3) . . ? O1C Pd1C N2C 172.1(3) . . ? N1C Pd1C N2C 80.9(3) . . ? O1C Pd1C Cl1C 90.73(19) . . ? N1C Pd1C Cl1C 175.5(2) . . ? N2C Pd1C Cl1C 96.1(2) . . ? C1C O1C Pd1C 119.8(6) . . ? C17C N1C C13C 123.1(9) . . ? C17C N1C Pd1C 112.4(6) . . ? C13C N1C Pd1C 123.8(7) . . ? C18C N2C C19C 119.8(9) . . ? C18C N2C Pd1C 114.2(7) . . ? C19C N2C Pd1C 125.9(6) . . ? O1C C1C C6C 119.1(9) . . ? O1C C1C C2C 121.2(9) . . ? C6C C1C C2C 119.7(9) . . ? C3C C2C C1C 117.5(9) . . ? C3C C2C C13C 119.5(9) . . ? C1C C2C C13C 122.9(9) . . ? C4C C3C C2C 122.4(10) . . ? C4C C3C H3C 118.8 . . ? C2C C3C H3C 118.8 . . ? C3C C4C C5C 118.4(10) . . ? C3C C4C H4C 120.8 . . ? C5C C4C H4C 120.8 . . ? C6C C5C C4C 122.5(10) . . ? C6C C5C H5C 118.7 . . ? C4C C5C H5C 118.7 . . ? C5C C6C C1C 119.2(10) . . ? C5C C6C C7C 119.9(10) . . ? C1C C6C C7C 120.7(9) . . ? C12C C7C C8C 116.2(10) . . ? C12C C7C C6C 122.4(10) . . ? C8C C7C C6C 121.4(10) . . ? C9C C8C C7C 121.3(11) . . ? C9C C8C H8C 119.4 . . ? C7C C8C H8C 119.4 . . ? C10C C9C C8C 121.1(12) . . ? C10C C9C H9C 119.4 . . ? C8C C9C H9C 119.4 . . ? C11C C10C C9C 119.0(12) . . ? C11C C10C H10C 120.5 . . ? C9C C10C H10C 120.5 . . ? C10C C11C C12C 119.9(12) . . ? C10C C11C H11C 120.1 . . ? C12C C11C H11C 120.1 . . ? C11C C12C C7C 122.5(11) . . ? C11C C12C H12C 118.7 . . ? C7C C12C H12C 118.7 . . ? N1C C13C C14C 116.0(9) . . ? N1C C13C C2C 121.5(9) . . ? C14C C13C C2C 122.4(9) . . ? C15C C14C C13C 122.1(10) . . ? C15C C14C H14C 119.0 . . ? C13C C14C H14C 119.0 . . ? C14C C15C C16C 118.1(10) . . ? C14C C15C H15C 120.9 . . ? C16C C15C H15C 120.9 . . ? C17C C16C C15C 119.5(10) . . ? C17C C16C H16C 120.3 . . ? C15C C16C H16C 120.3 . . ? N1C C17C C16C 120.7(10) . . ? N1C C17C C18C 114.3(9) . . ? C16C C17C C18C 124.8(10) . . ? N2C C18C C17C 115.6(9) . . ? N2C C18C H18C 122.2 . . ? C17C C18C H18C 122.2 . . ? C20C C19C C24C 123.6(10) . . ? C20C C19C N2C 118.3(10) . . ? C24C C19C N2C 117.8(9) . . ? C19C C20C C21C 118.1(11) . . ? C19C C20C C25C 123.5(10) . . ? C21C C20C C25C 118.2(10) . . ? C22C C21C C20C 119.6(10) . . ? C22C C21C H21C 120.2 . . ? C20C C21C H21C 120.2 . . ? C23C C22C C21C 120.6(11) . . ? C23C C22C C26C 119.8(11) . . ? C21C C22C C26C 119.5(10) . . ? C22C C23C C24C 121.9(11) . . ? C22C C23C H23C 119.0 . . ? C24C C23C H23C 119.0 . . ? C19C C24C C23C 116.1(10) . . ? C19C C24C C27C 120.9(10) . . ? C23C C24C C27C 123.0(10) . . ? C20C C25C H25J 109.5 . . ? C20C C25C H25K 109.5 . . ? H25J C25C H25K 109.5 . . ? C20C C25C H25L 109.5 . . ? H25J C25C H25L 109.5 . . ? H25K C25C H25L 109.5 . . ? C22C C26C H26J 109.5 . . ? C22C C26C H26K 109.5 . . ? H26J C26C H26K 109.5 . . ? C22C C26C H26L 109.5 . . ? H26J C26C H26L 109.5 . . ? H26K C26C H26L 109.5 . . ? C24C C27C H27J 109.5 . . ? C24C C27C H27K 109.5 . . ? H27J C27C H27K 109.5 . . ? C24C C27C H27L 109.5 . . ? H27J C27C H27L 109.5 . . ? H27K C27C H27L 109.5 . . ? O1D Pd1D N1D 93.4(3) . . ? O1D Pd1D N2D 175.1(3) . . ? N1D Pd1D N2D 82.0(4) . . ? O1D Pd1D Cl1D 88.8(2) . . ? N1D Pd1D Cl1D 175.6(2) . . ? N2D Pd1D Cl1D 95.7(3) . . ? C1D O1D Pd1D 125.5(6) . . ? C13D N1D C17D 121.3(9) . . ? C13D N1D Pd1D 127.2(7) . . ? C17D N1D Pd1D 111.4(7) . . ? C18D N2D C19D 118.5(9) . . ? C18D N2D Pd1D 113.1(8) . . ? C19D N2D Pd1D 128.2(6) . . ? O1D C1D C2D 126.8(10) . . ? O1D C1D C6D 114.0(10) . . ? C2D C1D C6D 119.2(10) . . ? C3D C2D C1D 116.6(10) . . ? C3D C2D C13D 119.4(10) . . ? C1D C2D C13D 124.0(10) . . ? C4D C3D C2D 125.1(11) . . ? C4D C3D H3D 117.4 . . ? C2D C3D H3D 117.4 . . ? C3D C4D C5D 118.9(12) . . ? C3D C4D H4D 120.5 . . ? C5D C4D H4D 120.5 . . ? C4D C5D C6D 120.9(11) . . ? C4D C5D H5D 119.5 . . ? C6D C5D H5D 119.5 . . ? C5D C6D C1D 119.2(10) . . ? C5D C6D C7D 118.9(10) . . ? C1D C6D C7D 121.9(10) . . ? C8D C7D C12D 118.8(11) . . ? C8D C7D C6D 120.2(11) . . ? C12D C7D C6D 121.0(10) . . ? C7D C8D C9D 121.5(12) . . ? C7D C8D H8D 119.3 . . ? C9D C8D H8D 119.3 . . ? C10D C9D C8D 118.6(12) . . ? C10D C9D H9D 120.7 . . ? C8D C9D H9D 120.7 . . ? C11D C10D C9D 119.0(13) . . ? C11D C10D H10D 120.5 . . ? C9D C10D H10D 120.5 . . ? C10D C11D C12D 122.4(12) . . ? C10D C11D H11D 118.8 . . ? C12D C11D H11D 118.8 . . ? C11D C12D C7D 119.7(11) . . ? C11D C12D H12D 120.2 . . ? C7D C12D H12D 120.2 . . ? N1D C13D C14D 117.1(10) . . ? N1D C13D C2D 122.2(10) . . ? C14D C13D C2D 120.6(11) . . ? C15D C14D C13D 121.9(12) . . ? C15D C14D H14D 119.1 . . ? C13D C14D H14D 119.1 . . ? C14D C15D C16D 119.9(11) . . ? C14D C15D H15D 120.0 . . ? C16D C15D H15D 120.0 . . ? C17D C16D C15D 117.2(12) . . ? C17D C16D H16D 121.4 . . ? C15D C16D H16D 121.4 . . ? N1D C17D C16D 122.5(11) . . ? N1D C17D C18D 115.4(10) . . ? C16D C17D C18D 122.2(11) . . ? N2D C18D C17D 117.6(11) . . ? N2D C18D H18D 121.2 . . ? C17D C18D H18D 121.2 . . ? C20D C19D C24D 121.6(11) . . ? C20D C19D N2D 118.8(10) . . ? C24D C19D N2D 119.6(10) . . ? C19D C20D C21D 118.8(11) . . ? C19D C20D C25D 121.1(11) . . ? C21D C20D C25D 120.0(10) . . ? C22D C21D C20D 119.6(12) . . ? C22D C21D H21D 120.2 . . ? C20D C21D H21D 120.2 . . ? C21D C22D C23D 121.9(12) . . ? C21D C22D C26D 118.6(12) . . ? C23D C22D C26D 119.5(12) . . ? C24D C23D C22D 120.7(12) . . ? C24D C23D H23D 119.7 . . ? C22D C23D H23D 119.7 . . ? C23D C24D C19D 117.4(11) . . ? C23D C24D C27D 122.2(11) . . ? C19D C24D C27D 120.4(10) . . ? C20D C25D H25M 109.5 . . ? C20D C25D H25N 109.5 . . ? H25M C25D H25N 109.5 . . ? C20D C25D H25O 109.5 . . ? H25M C25D H25O 109.5 . . ? H25N C25D H25O 109.5 . . ? C22D C26D H26M 109.5 . . ? C22D C26D H26N 109.5 . . ? H26M C26D H26N 109.5 . . ? C22D C26D H26O 109.5 . . ? H26M C26D H26O 109.5 . . ? H26N C26D H26O 109.5 . . ? C24D C27D H27M 109.5 . . ? C24D C27D H27N 109.5 . . ? H27M C27D H27N 109.5 . . ? C24D C27D H27O 109.5 . . ? H27M C27D H27O 109.5 . . ? H27N C27D H27O 109.5 . . ? Cl2 C28 Cl3 110.5(7) . . ? Cl2 C28 H28A 109.6 . . ? Cl3 C28 H28A 109.6 . . ? Cl2 C28 H28B 109.6 . . ? Cl3 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? Cl5 C29 Cl4 117.0(8) . . ? Cl5 C29 H29A 108.1 . . ? Cl4 C29 H29A 108.1 . . ? Cl5 C29 H29B 108.1 . . ? Cl4 C29 H29B 108.1 . . ? H29A C29 H29B 107.3 . . ? Cl6 C30 Cl7 114.3(7) . . ? Cl6 C30 H30A 108.7 . . ? Cl7 C30 H30A 108.7 . . ? Cl6 C30 H30B 108.7 . . ? Cl7 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? 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 N1 Pd1 O1 C1 -22.0(7) . . . . ? Cl1 Pd1 O1 C1 162.1(7) . . . . ? O1 Pd1 N1 C13 4.0(9) . . . . ? N2 Pd1 N1 C13 -176.1(9) . . . . ? O1 Pd1 N1 C17 -170.8(7) . . . . ? N2 Pd1 N1 C17 9.1(7) . . . . ? N1 Pd1 N2 C18 -5.2(8) . . . . ? Cl1 Pd1 N2 C18 170.7(7) . . . . ? N1 Pd1 N2 C19 175.2(9) . . . . ? Cl1 Pd1 N2 C19 -9.0(9) . . . . ? Pd1 O1 C1 C2 26.4(12) . . . . ? Pd1 O1 C1 C6 -155.0(6) . . . . ? O1 C1 C2 C3 177.1(9) . . . . ? C6 C1 C2 C3 -1.5(14) . . . . ? O1 C1 C2 C13 -7.2(15) . . . . ? C6 C1 C2 C13 174.3(9) . . . . ? C1 C2 C3 C4 -1.5(15) . . . . ? C13 C2 C3 C4 -177.5(10) . . . . ? C2 C3 C4 C5 3.2(16) . . . . ? C3 C4 C5 C6 -1.9(16) . . . . ? C4 C5 C6 C1 -0.9(15) . . . . ? C4 C5 C6 C7 -179.0(10) . . . . ? O1 C1 C6 C5 -176.0(8) . . . . ? C2 C1 C6 C5 2.6(14) . . . . ? O1 C1 C6 C7 2.0(13) . . . . ? C2 C1 C6 C7 -179.3(9) . . . . ? C5 C6 C7 C8 37.7(14) . . . . ? C1 C6 C7 C8 -140.3(10) . . . . ? C5 C6 C7 C12 -140.7(10) . . . . ? C1 C6 C7 C12 41.3(13) . . . . ? C12 C7 C8 C9 -2.9(15) . . . . ? C6 C7 C8 C9 178.7(9) . . . . ? C7 C8 C9 C10 0.6(17) . . . . ? C8 C9 C10 C11 2.6(18) . . . . ? C9 C10 C11 C12 -3.4(16) . . . . ? C10 C11 C12 C7 1.2(15) . . . . ? C8 C7 C12 C11 2.0(14) . . . . ? C6 C7 C12 C11 -179.6(8) . . . . ? C17 N1 C13 C14 6.3(15) . . . . ? Pd1 N1 C13 C14 -168.1(7) . . . . ? C17 N1 C13 C2 -174.5(9) . . . . ? Pd1 N1 C13 C2 11.1(14) . . . . ? C1 C2 C13 N1 -12.8(16) . . . . ? C3 C2 C13 N1 162.8(9) . . . . ? C1 C2 C13 C14 166.3(10) . . . . ? C3 C2 C13 C14 -18.1(15) . . . . ? N1 C13 C14 C15 -4.9(16) . . . . ? C2 C13 C14 C15 175.9(10) . . . . ? C13 C14 C15 C16 -0.8(18) . . . . ? C14 C15 C16 C17 4.9(18) . . . . ? C13 N1 C17 C16 -2.5(16) . . . . ? Pd1 N1 C17 C16 172.7(9) . . . . ? C13 N1 C17 C18 173.7(9) . . . . ? Pd1 N1 C17 C18 -11.1(12) . . . . ? C15 C16 C17 N1 -3.5(18) . . . . ? C15 C16 C17 C18 -179.2(11) . . . . ? C19 N2 C18 C17 -179.9(10) . . . . ? Pd1 N2 C18 C17 0.4(13) . . . . ? N1 C17 C18 N2 7.3(15) . . . . ? C16 C17 C18 N2 -176.6(11) . . . . ? C18 N2 C19 C20 -83.5(13) . . . . ? Pd1 N2 C19 C20 96.1(11) . . . . ? C18 N2 C19 C24 95.2(12) . . . . ? Pd1 N2 C19 C24 -85.2(11) . . . . ? C24 C19 C20 C21 -0.5(16) . . . . ? N2 C19 C20 C21 178.2(9) . . . . ? C24 C19 C20 C25 177.1(10) . . . . ? N2 C19 C20 C25 -4.2(15) . . . . ? C19 C20 C21 C22 -1.9(16) . . . . ? C25 C20 C21 C22 -179.5(10) . . . . ? C20 C21 C22 C23 4.0(16) . . . . ? C20 C21 C22 C26 -177.6(10) . . . . ? C21 C22 C23 C24 -3.9(16) . . . . ? C26 C22 C23 C24 177.7(10) . . . . ? C22 C23 C24 C19 1.7(16) . . . . ? C22 C23 C24 C27 -177.5(10) . . . . ? C20 C19 C24 C23 0.6(16) . . . . ? N2 C19 C24 C23 -178.1(9) . . . . ? C20 C19 C24 C27 179.8(9) . . . . ? N2 C19 C24 C27 1.2(15) . . . . ? N1A Pd1A O1A C1A 1.9(8) . . . . ? Cl1A Pd1A O1A C1A -175.8(8) . . . . ? O1A Pd1A N1A C17A 177.9(7) . . . . ? N2A Pd1A N1A C17A -0.2(7) . . . . ? O1A Pd1A N1A C13A -0.1(8) . . . . ? N2A Pd1A N1A C13A -178.3(8) . . . . ? N1A Pd1A N2A C18A 0.8(7) . . . . ? Cl1A Pd1A N2A C18A 178.5(6) . . . . ? N1A Pd1A N2A C19A -174.5(9) . . . . ? Cl1A Pd1A N2A C19A 3.3(9) . . . . ? Pd1A O1A C1A C2A 1.9(14) . . . . ? Pd1A O1A C1A C6A -178.9(6) . . . . ? O1A C1A C2A C13A -8.5(16) . . . . ? C6A C1A C2A C13A 172.4(9) . . . . ? O1A C1A C2A C3A 172.2(9) . . . . ? C6A C1A C2A C3A -6.9(14) . . . . ? C1A C2A C3A C4A 2.8(15) . . . . ? C13A C2A C3A C4A -176.5(9) . . . . ? C2A C3A C4A C5A 1.2(16) . . . . ? C3A C4A C5A C6A -0.9(16) . . . . ? C4A C5A C6A C1A -3.4(15) . . . . ? C4A C5A C6A C7A 177.5(9) . . . . ? O1A C1A C6A C5A -171.9(9) . . . . ? C2A C1A C6A C5A 7.3(14) . . . . ? O1A C1A C6A C7A 7.2(14) . . . . ? C2A C1A C6A C7A -173.6(9) . . . . ? C5A C6A C7A C12A -132.6(11) . . . . ? C1A C6A C7A C12A 48.3(14) . . . . ? C5A C6A C7A C8A 48.6(15) . . . . ? C1A C6A C7A C8A -130.5(11) . . . . ? C12A C7A C8A C9A 2.9(17) . . . . ? C6A C7A C8A C9A -178.2(10) . . . . ? C7A C8A C9A C10A -1.7(19) . . . . ? C8A C9A C10A C11A 3.0(19) . . . . ? C9A C10A C11A C12A -5.6(19) . . . . ? C8A C7A C12A C11A -5.7(16) . . . . ? C6A C7A C12A C11A 175.4(10) . . . . ? C10A C11A C12A C7A 7.4(19) . . . . ? C17A N1A C13A C14A -1.0(13) . . . . ? Pd1A N1A C13A C14A 176.9(7) . . . . ? C17A N1A C13A C2A 176.6(9) . . . . ? Pd1A N1A C13A C2A -5.5(13) . . . . ? C1A C2A C13A N1A 10.2(15) . . . . ? C3A C2A C13A N1A -170.6(9) . . . . ? C1A C2A C13A C14A -172.4(10) . . . . ? C3A C2A C13A C14A 6.8(15) . . . . ? N1A C13A C14A C15A 1.2(16) . . . . ? C2A C13A C14A C15A -176.4(10) . . . . ? C13A C14A C15A C16A 1.4(17) . . . . ? C14A C15A C16A C17A -4.0(16) . . . . ? C15A C16A C17A N1A 4.4(17) . . . . ? C15A C16A C17A C18A -175.3(10) . . . . ? C13A N1A C17A C16A -1.9(15) . . . . ? Pd1A N1A C17A C16A 179.9(9) . . . . ? C13A N1A C17A C18A 177.8(9) . . . . ? Pd1A N1A C17A C18A -0.3(11) . . . . ? C19A N2A C18A C17A 174.4(9) . . . . ? Pd1A N2A C18A C17A -1.2(12) . . . . ? C16A C17A C18A N2A -179.1(10) . . . . ? N1A C17A C18A N2A 1.1(14) . . . . ? C18A N2A C19A C24A 108.8(12) . . . . ? Pd1A N2A C19A C24A -76.4(12) . . . . ? C18A N2A C19A C20A -72.9(13) . . . . ? Pd1A N2A C19A C20A 101.9(10) . . . . ? C24A C19A C20A C21A 1.8(16) . . . . ? N2A C19A C20A C21A -176.5(9) . . . . ? C24A C19A C20A C25A 177.4(10) . . . . ? N2A C19A C20A C25A -0.9(15) . . . . ? C19A C20A C21A C22A 0.3(17) . . . . ? C25A C20A C21A C22A -175.3(10) . . . . ? C20A C21A C22A C23A -2.8(17) . . . . ? C20A C21A C22A C26A 178.2(11) . . . . ? C21A C22A C23A C24A 3.7(19) . . . . ? C26A C22A C23A C24A -177.3(12) . . . . ? C22A C23A C24A C19A -1.9(19) . . . . ? C22A C23A C24A C27A 178.7(11) . . . . ? C20A C19A C24A C23A -1.1(16) . . . . ? N2A C19A C24A C23A 177.2(10) . . . . ? C20A C19A C24A C27A 178.4(10) . . . . ? N2A C19A C24A C27A -3.4(16) . . . . ? N1B Pd1B O1B C1B 5.7(7) . . . . ? Cl1B Pd1B O1B C1B -173.3(7) . . . . ? O1B Pd1B N1B C13B -5.2(8) . . . . ? N2B Pd1B N1B C13B 179.4(8) . . . . ? O1B Pd1B N1B C17B 174.9(7) . . . . ? N2B Pd1B N1B C17B -0.6(7) . . . . ? N1B Pd1B N2B C18B 1.6(7) . . . . ? Cl1B Pd1B N2B C18B -179.6(7) . . . . ? N1B Pd1B N2B C19B -179.8(9) . . . . ? Cl1B Pd1B N2B C19B -0.9(9) . . . . ? Pd1B O1B C1B C2B 0.4(13) . . . . ? Pd1B O1B C1B C6B -176.9(6) . . . . ? O1B C1B C2B C3B 173.8(9) . . . . ? C6B C1B C2B C3B -9.0(13) . . . . ? O1B C1B C2B C13B -10.0(15) . . . . ? C6B C1B C2B C13B 167.3(9) . . . . ? C1B C2B C3B C4B 3.6(15) . . . . ? C13B C2B C3B C4B -172.9(10) . . . . ? C2B C3B C4B C5B 4.3(17) . . . . ? C3B C4B C5B C6B -6.8(16) . . . . ? C4B C5B C6B C1B 1.3(15) . . . . ? C4B C5B C6B C7B -178.6(9) . . . . ? O1B C1B C6B C5B -175.6(8) . . . . ? C2B C1B C6B C5B 6.9(14) . . . . ? O1B C1B C6B C7B 4.3(13) . . . . ? C2B C1B C6B C7B -173.2(9) . . . . ? C5B C6B C7B C12B -134.8(10) . . . . ? C1B C6B C7B C12B 45.4(14) . . . . ? C5B C6B C7B C8B 37.5(14) . . . . ? C1B C6B C7B C8B -142.4(10) . . . . ? C12B C7B C8B C9B -0.2(15) . . . . ? C6B C7B C8B C9B -172.8(10) . . . . ? C7B C8B C9B C10B 0.9(18) . . . . ? C8B C9B C10B C11B -1.4(18) . . . . ? C9B C10B C11B C12B 1.1(17) . . . . ? C10B C11B C12B C7B -0.4(17) . . . . ? C8B C7B C12B C11B -0.1(15) . . . . ? C6B C7B C12B C11B 172.4(9) . . . . ? C17B N1B C13B C14B -4.1(14) . . . . ? Pd1B N1B C13B C14B 176.0(7) . . . . ? C17B N1B C13B C2B 178.5(9) . . . . ? Pd1B N1B C13B C2B -1.4(14) . . . . ? C1B C2B C13B N1B 10.3(15) . . . . ? C3B C2B C13B N1B -173.6(9) . . . . ? C1B C2B C13B C14B -166.9(9) . . . . ? C3B C2B C13B C14B 9.2(14) . . . . ? N1B C13B C14B C15B 2.0(16) . . . . ? C2B C13B C14B C15B 179.4(11) . . . . ? C13B C14B C15B C16B -0.2(18) . . . . ? C14B C15B C16B C17B 0.4(18) . . . . ? C13B N1B C17B C16B 4.5(16) . . . . ? Pd1B N1B C17B C16B -175.6(9) . . . . ? C13B N1B C17B C18B 179.6(9) . . . . ? Pd1B N1B C17B C18B -0.5(12) . . . . ? C15B C16B C17B N1B -2.4(18) . . . . ? C15B C16B C17B C18B -177.2(11) . . . . ? C19B N2B C18B C17B 178.8(10) . . . . ? Pd1B N2B C18B C17B -2.4(13) . . . . ? N1B C17B C18B N2B 2.0(15) . . . . ? C16B C17B C18B N2B 177.0(10) . . . . ? C18B N2B C19B C24B 100.4(13) . . . . ? Pd1B N2B C19B C24B -78.2(13) . . . . ? C18B N2B C19B C20B -80.5(14) . . . . ? Pd1B N2B C19B C20B 100.9(11) . . . . ? C24B C19B C20B C21B -3.0(18) . . . . ? N2B C19B C20B C21B 177.9(10) . . . . ? C24B C19B C20B C25B 177.8(11) . . . . ? N2B C19B C20B C25B -1.3(17) . . . . ? C19B C20B C21B C22B -0.7(19) . . . . ? C25B C20B C21B C22B 178.4(11) . . . . ? C20B C21B C22B C23B 1.7(18) . . . . ? C20B C21B C22B C26B 178.7(10) . . . . ? C21B C22B C23B C24B 1.0(16) . . . . ? C26B C22B C23B C24B -176.2(10) . . . . ? C20B C19B C24B C23B 5.5(17) . . . . ? N2B C19B C24B C23B -175.4(9) . . . . ? C20B C19B C24B C27B -175.4(10) . . . . ? N2B C19B C24B C27B 3.7(17) . . . . ? C22B C23B C24B C19B -4.4(16) . . . . ? C22B C23B C24B C27B 176.4(9) . . . . ? N1C Pd1C O1C C1C -40.5(7) . . . . ? Cl1C Pd1C O1C C1C 143.1(7) . . . . ? O1C Pd1C N1C C17C -162.1(7) . . . . ? N2C Pd1C N1C C17C 14.4(7) . . . . ? O1C Pd1C N1C C13C 9.0(8) . . . . ? N2C Pd1C N1C C13C -174.6(9) . . . . ? N1C Pd1C N2C C18C -10.2(7) . . . . ? Cl1C Pd1C N2C C18C 166.3(7) . . . . ? N1C Pd1C N2C C19C 168.9(8) . . . . ? Cl1C Pd1C N2C C19C -14.5(8) . . . . ? Pd1C O1C C1C C6C -137.3(8) . . . . ? Pd1C O1C C1C C2C 43.9(12) . . . . ? O1C C1C C2C C3C 178.4(9) . . . . ? C6C C1C C2C C3C -0.4(14) . . . . ? O1C C1C C2C C13C -6.2(15) . . . . ? C6C C1C C2C C13C 175.0(9) . . . . ? C1C C2C C3C C4C 0.9(15) . . . . ? C13C C2C C3C C4C -174.6(9) . . . . ? C2C C3C C4C C5C -3.4(15) . . . . ? C3C C4C C5C C6C 5.6(16) . . . . ? C4C C5C C6C C1C -5.2(16) . . . . ? C4C C5C C6C C7C 178.9(9) . . . . ? O1C C1C C6C C5C -176.3(9) . . . . ? C2C C1C C6C C5C 2.5(15) . . . . ? O1C C1C C6C C7C -0.5(14) . . . . ? C2C C1C C6C C7C 178.3(9) . . . . ? C5C C6C C7C C12C -147.0(10) . . . . ? C1C C6C C7C C12C 37.2(14) . . . . ? C5C C6C C7C C8C 31.4(15) . . . . ? C1C C6C C7C C8C -144.4(10) . . . . ? C12C C7C C8C C9C -0.7(15) . . . . ? C6C C7C C8C C9C -179.2(9) . . . . ? C7C C8C C9C C10C -0.4(17) . . . . ? C8C C9C C10C C11C 1.0(18) . . . . ? C9C C10C C11C C12C -0.4(17) . . . . ? C10C C11C C12C C7C -0.8(17) . . . . ? C8C C7C C12C C11C 1.3(15) . . . . ? C6C C7C C12C C11C 179.8(9) . . . . ? C17C N1C C13C C14C 6.8(15) . . . . ? Pd1C N1C C13C C14C -163.3(7) . . . . ? C17C N1C C13C C2C -168.9(9) . . . . ? Pd1C N1C C13C C2C 20.9(13) . . . . ? C3C C2C C13C N1C 146.4(10) . . . . ? C1C C2C C13C N1C -28.9(15) . . . . ? C3C C2C C13C C14C -29.1(14) . . . . ? C1C C2C C13C C14C 155.6(10) . . . . ? N1C C13C C14C C15C -4.5(15) . . . . ? C2C C13C C14C C15C 171.2(10) . . . . ? C13C C14C C15C C16C -2.5(16) . . . . ? C14C C15C C16C C17C 7.6(15) . . . . ? C13C N1C C17C C16C -2.0(16) . . . . ? Pd1C N1C C17C C16C 169.2(8) . . . . ? C13C N1C C17C C18C 172.7(9) . . . . ? Pd1C N1C C17C C18C -16.1(11) . . . . ? C15C C16C C17C N1C -5.6(16) . . . . ? C15C C16C C17C C18C -179.7(10) . . . . ? C19C N2C C18C C17C -174.8(9) . . . . ? Pd1C N2C C18C C17C 4.4(12) . . . . ? N1C C17C C18C N2C 7.9(14) . . . . ? C16C C17C C18C N2C -177.6(10) . . . . ? C18C N2C C19C C20C -84.2(12) . . . . ? Pd1C N2C C19C C20C 96.7(10) . . . . ? C18C N2C C19C C24C 100.8(11) . . . . ? Pd1C N2C C19C C24C -78.3(11) . . . . ? C24C C19C C20C C21C -0.9(16) . . . . ? N2C C19C C20C C21C -175.6(8) . . . . ? C24C C19C C20C C25C 173.9(10) . . . . ? N2C C19C C20C C25C -0.7(15) . . . . ? C19C C20C C21C C22C -0.3(16) . . . . ? C25C C20C C21C C22C -175.5(9) . . . . ? C20C C21C C22C C23C 1.4(17) . . . . ? C20C C21C C22C C26C 179.0(9) . . . . ? C21C C22C C23C C24C -1.3(17) . . . . ? C26C C22C C23C C24C -178.9(9) . . . . ? C20C C19C C24C C23C 1.1(16) . . . . ? N2C C19C C24C C23C 175.7(9) . . . . ? C20C C19C C24C C27C -178.9(10) . . . . ? N2C C19C C24C C27C -4.2(15) . . . . ? C22C C23C C24C C19C 0.1(16) . . . . ? C22C C23C C24C C27C 180.0(10) . . . . ? N1D Pd1D O1D C1D -9.7(8) . . . . ? Cl1D Pd1D O1D C1D 174.1(7) . . . . ? O1D Pd1D N1D C13D 6.1(8) . . . . ? N2D Pd1D N1D C13D -175.6(8) . . . . ? O1D Pd1D N1D C17D -172.2(7) . . . . ? N2D Pd1D N1D C17D 6.1(6) . . . . ? N1D Pd1D N2D C18D -6.5(7) . . . . ? Cl1D Pd1D N2D C18D 169.8(7) . . . . ? N1D Pd1D N2D C19D 178.5(9) . . . . ? Cl1D Pd1D N2D C19D -5.2(8) . . . . ? Pd1D O1D C1D C2D 7.9(14) . . . . ? Pd1D O1D C1D C6D -174.0(6) . . . . ? O1D C1D C2D C3D -179.4(9) . . . . ? C6D C1D C2D C3D 2.6(14) . . . . ? O1D C1D C2D C13D 0.9(16) . . . . ? C6D C1D C2D C13D -177.1(9) . . . . ? C1D C2D C3D C4D -0.3(16) . . . . ? C13D C2D C3D C4D 179.4(10) . . . . ? C2D C3D C4D C5D -2.2(18) . . . . ? C3D C4D C5D C6D 2.3(17) . . . . ? C4D C5D C6D C1D 0.0(16) . . . . ? C4D C5D C6D C7D -179.8(10) . . . . ? O1D C1D C6D C5D 179.2(9) . . . . ? C2D C1D C6D C5D -2.5(14) . . . . ? O1D C1D C6D C7D -1.0(14) . . . . ? C2D C1D C6D C7D 177.3(9) . . . . ? C5D C6D C7D C8D 46.2(14) . . . . ? C1D C6D C7D C8D -133.5(11) . . . . ? C5D C6D C7D C12D -132.4(11) . . . . ? C1D C6D C7D C12D 47.9(14) . . . . ? C12D C7D C8D C9D 0.4(16) . . . . ? C6D C7D C8D C9D -178.2(10) . . . . ? C7D C8D C9D C10D 1.5(18) . . . . ? C8D C9D C10D C11D -1.3(18) . . . . ? C9D C10D C11D C12D -0.6(18) . . . . ? C10D C11D C12D C7D 2.5(17) . . . . ? C8D C7D C12D C11D -2.3(16) . . . . ? C6D C7D C12D C11D 176.3(9) . . . . ? C17D N1D C13D C14D 1.6(14) . . . . ? Pd1D N1D C13D C14D -176.5(7) . . . . ? C17D N1D C13D C2D 177.8(9) . . . . ? Pd1D N1D C13D C2D -0.4(14) . . . . ? C3D C2D C13D N1D 175.4(9) . . . . ? C1D C2D C13D N1D -4.8(15) . . . . ? C3D C2D C13D C14D -8.6(15) . . . . ? C1D C2D C13D C14D 171.1(10) . . . . ? N1D C13D C14D C15D 0.3(16) . . . . ? C2D C13D C14D C15D -175.8(11) . . . . ? C13D C14D C15D C16D -0.2(18) . . . . ? C14D C15D C16D C17D -1.9(18) . . . . ? C13D N1D C17D C16D -3.9(15) . . . . ? Pd1D N1D C17D C16D 174.5(9) . . . . ? C13D N1D C17D C18D 176.6(9) . . . . ? Pd1D N1D C17D C18D -5.0(11) . . . . ? C15D C16D C17D N1D 4.0(17) . . . . ? C15D C16D C17D C18D -176.6(10) . . . . ? C19D N2D C18D C17D -178.9(9) . . . . ? Pd1D N2D C18D C17D 5.6(12) . . . . ? N1D C17D C18D N2D -0.4(14) . . . . ? C16D C17D C18D N2D -179.9(10) . . . . ? C18D N2D C19D C20D 103.4(11) . . . . ? Pd1D N2D C19D C20D -81.8(11) . . . . ? C18D N2D C19D C24D -75.9(12) . . . . ? Pd1D N2D C19D C24D 98.9(10) . . . . ? C24D C19D C20D C21D 1.7(15) . . . . ? N2D C19D C20D C21D -177.5(8) . . . . ? C24D C19D C20D C25D -174.8(9) . . . . ? N2D C19D C20D C25D 5.9(14) . . . . ? C19D C20D C21D C22D 0.1(15) . . . . ? C25D C20D C21D C22D 176.7(10) . . . . ? C20D C21D C22D C23D -1.9(17) . . . . ? C20D C21D C22D C26D 178.8(9) . . . . ? C21D C22D C23D C24D 1.9(17) . . . . ? C26D C22D C23D C24D -178.9(10) . . . . ? C22D C23D C24D C19D 0.0(15) . . . . ? C22D C23D C24D C27D -177.7(10) . . . . ? C20D C19D C24D C23D -1.8(15) . . . . ? N2D C19D C24D C23D 177.5(9) . . . . ? C20D C19D C24D C27D 176.0(9) . . . . ? N2D C19D C24D C27D -4.7(14) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.828 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.124 data_10068 _database_code_depnum_ccdc_archive 'CCDC 919250' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: ...Due to the Squeeze option in Platon,reported sum formula does not agree with the calculated sum formula.''see _platon_squeeze_details' ; _vrf_PLAT051_I ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 23.50 Perc. RESPONSE: ...Due to Platon, reported sum formula does not agree with the calculated sum formula.'see_platon_squeeze_details' ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 N2 O3 Pd,C H2 Cl2,1.5(C6 H14)' _chemical_formula_sum 'C39 H49 Cl2 N2 O3 Pd' _chemical_formula_weight 771.10 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.075(8) _cell_length_b 20.075(8) _cell_length_c 28.842(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11624(10) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 944 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 28.412 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6416 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 5597 reflections(SADABS);Rint 0.1715 before correction and 0.0694 after. ; _exptl_special_details ; The crystal data was weak due to crystal quality ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41787 _diffrn_reflns_av_R_equivalents 0.2088 _diffrn_reflns_av_sigmaI/netI 0.1566 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5124 _reflns_number_gt 3007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Disordered CH2Cl2 and C6H14 was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 2694.5 3 with an estimated 1638e/cell to be added. Sixteen solvent CH2Cl2 and twenty four C6H14 molecules/unit cell accounting for 1872e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. 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^)+(0.0853P)^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 5124 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.250 0.125 663 409 ' ' 2 0.000 0.750 -0.125 662 410 ' ' 3 0.500 0.250 0.375 662 410 ' ' 4 0.500 0.750 0.625 662 409 ' ' _platon_squeeze_details ; Disordered CH2Cl2 and C6H14 was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 2694.5 3 with an estimated 1638e/cell to be added. Sixteen solvent CH2Cl2 and twenty four C6H14 molecules/unit cell accounting for 1872e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. ; 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 0.44289(3) 0.96361(3) 0.10202(2) 0.0285(2) Uani 1 1 d . . . O1 O 0.3640(3) 0.9547(3) 0.0636(2) 0.0359(14) Uani 1 1 d . . . O2 O 0.3836(3) 1.0001(3) 0.15249(19) 0.0363(14) Uani 1 1 d . . . O3 O 0.3814(3) 1.0982(3) 0.1144(2) 0.0446(16) Uani 1 1 d . . . N1 N 0.5051(3) 0.9309(3) 0.0542(2) 0.0265(16) Uani 1 1 d . . . N2 N 0.5255(3) 0.9604(3) 0.1409(2) 0.0349(17) Uani 1 1 d . . . C1 C 0.3647(4) 0.9403(4) 0.0187(3) 0.031(2) Uani 1 1 d . . . C2 C 0.4209(4) 0.9236(4) -0.0087(3) 0.0266(19) Uani 1 1 d . . . C3 C 0.4107(5) 0.9106(4) -0.0560(3) 0.041(2) Uani 1 1 d . . . H3 H 0.4476 0.8984 -0.0748 0.049 Uiso 1 1 calc R . . C4 C 0.3493(5) 0.9150(4) -0.0756(3) 0.039(2) Uani 1 1 d . . . H4 H 0.3440 0.9060 -0.1078 0.047 Uiso 1 1 calc R . . C5 C 0.2938(4) 0.9326(4) -0.0490(3) 0.039(2) Uani 1 1 d . . . H5 H 0.2512 0.9351 -0.0632 0.046 Uiso 1 1 calc R . . C6 C 0.3002(4) 0.9461(4) -0.0034(3) 0.029(2) Uani 1 1 d . . . C7 C 0.2407(4) 0.9682(5) 0.0246(3) 0.039(2) Uani 1 1 d . . . C8 C 0.1779(5) 0.9376(5) 0.0153(4) 0.055(3) Uani 1 1 d . . . H8 H 0.1755 0.9015 -0.0060 0.066 Uiso 1 1 calc R . . C9 C 0.1195(6) 0.9604(7) 0.0373(5) 0.077(4) Uani 1 1 d . . . H9 H 0.0782 0.9385 0.0320 0.092 Uiso 1 1 calc R . . C10 C 0.1225(6) 1.0140(6) 0.0662(4) 0.060(3) Uani 1 1 d . . . H10 H 0.0829 1.0308 0.0800 0.072 Uiso 1 1 calc R . . C11 C 0.1831(7) 1.0442(6) 0.0753(4) 0.072(4) Uani 1 1 d . . . H11 H 0.1853 1.0815 0.0955 0.087 Uiso 1 1 calc R . . C12 C 0.2420(5) 1.0193(5) 0.0545(3) 0.047(3) Uani 1 1 d . . . H12 H 0.2835 1.0394 0.0620 0.057 Uiso 1 1 calc R . . C13 C 0.4893(4) 0.9181(4) 0.0091(3) 0.0254(19) Uani 1 1 d . . . C14 C 0.5429(4) 0.8995(4) -0.0197(3) 0.035(2) Uani 1 1 d . . . H14 H 0.5341 0.8904 -0.0514 0.042 Uiso 1 1 calc R . . C15 C 0.6075(4) 0.8939(4) -0.0040(3) 0.034(2) Uani 1 1 d . . . H15 H 0.6423 0.8806 -0.0244 0.041 Uiso 1 1 calc R . . C16 C 0.6204(4) 0.9081(4) 0.0419(3) 0.031(2) Uani 1 1 d . . . H16 H 0.6645 0.9052 0.0537 0.037 Uiso 1 1 calc R . . C17 C 0.5691(4) 0.9263(4) 0.0701(2) 0.0234(18) Uani 1 1 d . . . C18 C 0.5787(4) 0.9413(4) 0.1190(3) 0.0269(19) Uani 1 1 d . . . H18 H 0.6208 0.9374 0.1338 0.032 Uiso 1 1 calc R . . C19 C 0.5232(4) 0.9689(4) 0.1912(3) 0.034(2) Uani 1 1 d . . . C20 C 0.5205(4) 0.9097(5) 0.2168(3) 0.039(2) Uani 1 1 d . . . C21 C 0.5100(4) 0.9154(5) 0.2642(3) 0.045(2) Uani 1 1 d . . . H21 H 0.5076 0.8761 0.2826 0.054 Uiso 1 1 calc R . . C22 C 0.5030(5) 0.9775(6) 0.2856(3) 0.051(3) Uani 1 1 d . . . C23 C 0.5089(5) 1.0348(6) 0.2593(3) 0.054(3) Uani 1 1 d . . . H23 H 0.5066 1.0773 0.2737 0.065 Uiso 1 1 calc R . . C24 C 0.5183(4) 1.0297(5) 0.2106(3) 0.039(2) Uani 1 1 d . . . C25 C 0.5213(4) 0.8406(5) 0.1951(3) 0.047(3) Uani 1 1 d . . . H25A H 0.5106 0.8073 0.2187 0.070 Uiso 1 1 calc R . . H25B H 0.5656 0.8316 0.1823 0.070 Uiso 1 1 calc R . . H25C H 0.4881 0.8386 0.1702 0.070 Uiso 1 1 calc R . . C26 C 0.4900(6) 0.9821(6) 0.3371(4) 0.074(4) Uani 1 1 d . . . H26A H 0.4476 0.9602 0.3444 0.111 Uiso 1 1 calc R . . H26B H 0.4878 1.0290 0.3463 0.111 Uiso 1 1 calc R . . H26C H 0.5261 0.9599 0.3540 0.111 Uiso 1 1 calc R . . C27 C 0.5240(5) 1.0925(5) 0.1820(3) 0.053(3) Uani 1 1 d . . . H27A H 0.5703 1.0985 0.1722 0.080 Uiso 1 1 calc R . . H27B H 0.5101 1.1308 0.2007 0.080 Uiso 1 1 calc R . . H27C H 0.4953 1.0889 0.1547 0.080 Uiso 1 1 calc R . . C28 C 0.3653(4) 1.0625(5) 0.1473(3) 0.041(2) Uani 1 1 d . . . C29 C 0.3237(5) 1.0890(5) 0.1858(4) 0.068(3) Uani 1 1 d . . . H29A H 0.3426 1.0749 0.2156 0.101 Uiso 1 1 calc R . . H29B H 0.2782 1.0717 0.1829 0.101 Uiso 1 1 calc R . . H29C H 0.3228 1.1377 0.1843 0.101 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 0.0290(4) 0.0299(4) 0.0266(3) 0.0042(3) -0.0015(3) 0.0001(3) O1 0.029(3) 0.042(4) 0.037(4) 0.001(3) -0.001(3) 0.000(3) O2 0.041(4) 0.030(3) 0.038(4) 0.002(3) 0.012(3) 0.001(3) O3 0.051(4) 0.046(4) 0.037(4) 0.011(3) 0.011(3) 0.007(3) N1 0.031(4) 0.022(4) 0.026(4) -0.001(3) 0.000(3) -0.002(3) N2 0.033(4) 0.043(4) 0.028(4) 0.009(3) -0.008(3) 0.001(3) C1 0.032(5) 0.028(5) 0.032(5) 0.003(4) 0.000(4) -0.008(4) C2 0.030(5) 0.021(5) 0.029(5) 0.009(4) 0.002(4) -0.002(4) C3 0.050(6) 0.037(5) 0.036(5) 0.000(4) 0.007(5) -0.008(5) C4 0.049(6) 0.039(6) 0.029(5) -0.005(4) -0.013(5) 0.003(5) C5 0.032(5) 0.040(6) 0.044(6) 0.000(4) -0.005(4) -0.003(4) C6 0.018(5) 0.029(5) 0.042(5) 0.013(4) -0.007(4) -0.008(4) C7 0.035(6) 0.040(6) 0.042(6) 0.026(5) -0.009(4) -0.007(5) C8 0.055(7) 0.045(6) 0.065(7) 0.019(5) -0.009(6) -0.001(6) C9 0.047(8) 0.077(9) 0.106(11) 0.044(8) -0.014(7) -0.013(7) C10 0.042(7) 0.074(9) 0.065(8) 0.024(7) 0.005(6) -0.006(6) C11 0.103(11) 0.055(8) 0.059(8) 0.025(6) 0.009(7) 0.019(8) C12 0.038(6) 0.058(7) 0.045(6) 0.008(5) -0.005(5) -0.002(5) C13 0.031(5) 0.017(4) 0.028(5) 0.006(3) -0.002(4) -0.003(4) C14 0.050(6) 0.037(5) 0.020(5) 0.007(4) 0.005(4) 0.003(5) C15 0.031(5) 0.034(5) 0.036(5) 0.003(4) -0.004(4) 0.005(4) C16 0.025(5) 0.024(5) 0.043(6) 0.009(4) -0.004(4) -0.003(4) C17 0.032(5) 0.020(4) 0.019(4) -0.002(3) -0.009(4) -0.003(4) C18 0.021(4) 0.027(5) 0.033(5) 0.009(4) 0.001(4) 0.006(4) C19 0.031(5) 0.043(6) 0.028(5) 0.002(4) -0.006(4) 0.006(4) C20 0.034(5) 0.049(6) 0.033(5) 0.003(5) -0.002(4) -0.002(5) C21 0.039(6) 0.053(7) 0.042(6) 0.013(5) -0.001(5) -0.008(5) C22 0.047(6) 0.076(8) 0.030(6) -0.004(6) -0.007(5) -0.005(6) C23 0.053(7) 0.067(8) 0.042(6) -0.012(6) -0.002(5) 0.006(6) C24 0.037(5) 0.043(6) 0.038(5) -0.004(5) -0.004(4) 0.010(5) C25 0.036(6) 0.063(7) 0.040(6) 0.013(5) -0.009(4) -0.003(5) C26 0.063(8) 0.117(10) 0.042(7) -0.010(7) 0.001(6) -0.005(7) C27 0.046(6) 0.060(7) 0.054(7) -0.012(5) -0.005(5) 0.002(5) C28 0.039(5) 0.068(7) 0.016(4) -0.010(5) 0.004(4) -0.001(5) C29 0.066(8) 0.067(8) 0.070(8) -0.003(6) 0.031(6) 0.001(6) _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 O1 1.942(5) . ? Pd1 N1 1.973(6) . ? Pd1 N2 2.004(6) . ? Pd1 O2 2.018(5) . ? O1 C1 1.327(9) . ? O2 C28 1.313(11) . ? O3 C28 1.234(10) . ? N1 C13 1.362(9) . ? N1 C17 1.368(9) . ? N2 C18 1.299(10) . ? N2 C19 1.461(10) . ? C1 C2 1.416(11) . ? C1 C6 1.447(11) . ? C2 C3 1.406(11) . ? C2 C13 1.471(10) . ? C3 C4 1.358(11) . ? C3 H3 0.9500 . ? C4 C5 1.398(11) . ? C4 H4 0.9500 . ? C5 C6 1.350(11) . ? C5 H5 0.9500 . ? C6 C7 1.508(12) . ? C7 C12 1.341(13) . ? C7 C8 1.426(13) . ? C8 C9 1.411(15) . ? C8 H8 0.9500 . ? C9 C10 1.362(16) . ? C9 H9 0.9500 . ? C10 C11 1.386(15) . ? C10 H10 0.9500 . ? C11 C12 1.415(14) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.410(11) . ? C14 C15 1.377(11) . ? C14 H14 0.9500 . ? C15 C16 1.379(11) . ? C15 H15 0.9500 . ? C16 C17 1.363(11) . ? C16 H16 0.9500 . ? C17 C18 1.454(10) . ? C18 H18 0.9500 . ? C19 C24 1.348(11) . ? C19 C20 1.400(12) . ? C20 C21 1.389(12) . ? C20 C25 1.521(12) . ? C21 C22 1.399(13) . ? C21 H21 0.9500 . ? C22 C23 1.383(13) . ? C22 C26 1.510(13) . ? C23 C24 1.420(12) . ? C23 H23 0.9500 . ? C24 C27 1.510(12) . ? 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 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.488(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 O1 Pd1 N1 94.9(3) . . ? O1 Pd1 N2 172.8(3) . . ? N1 Pd1 N2 81.8(3) . . ? O1 Pd1 O2 88.0(2) . . ? N1 Pd1 O2 176.7(2) . . ? N2 Pd1 O2 95.5(3) . . ? C1 O1 Pd1 124.6(5) . . ? C28 O2 Pd1 115.4(5) . . ? C13 N1 C17 121.7(7) . . ? C13 N1 Pd1 125.7(5) . . ? C17 N1 Pd1 112.4(5) . . ? C18 N2 C19 122.9(7) . . ? C18 N2 Pd1 114.7(6) . . ? C19 N2 Pd1 121.7(5) . . ? O1 C1 C2 127.1(7) . . ? O1 C1 C6 113.6(7) . . ? C2 C1 C6 119.2(8) . . ? C3 C2 C1 117.9(8) . . ? C3 C2 C13 117.5(7) . . ? C1 C2 C13 124.6(7) . . ? C4 C3 C2 121.7(8) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.7(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.8(8) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.7(8) . . ? C5 C6 C7 120.4(7) . . ? C1 C6 C7 119.9(8) . . ? C12 C7 C8 117.9(10) . . ? C12 C7 C6 123.6(8) . . ? C8 C7 C6 118.2(9) . . ? C9 C8 C7 120.6(11) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 119.7(11) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.0(11) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.9(11) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 121.8(10) . . ? C7 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N1 C13 C14 115.8(7) . . ? N1 C13 C2 122.4(7) . . ? C14 C13 C2 121.8(7) . . ? C15 C14 C13 123.1(8) . . ? C15 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? C14 C15 C16 118.3(8) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 119.2(7) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 N1 121.8(7) . . ? C16 C17 C18 122.3(7) . . ? N1 C17 C18 115.9(7) . . ? N2 C18 C17 115.0(7) . . ? N2 C18 H18 122.5 . . ? C17 C18 H18 122.5 . . ? C24 C19 C20 123.2(8) . . ? C24 C19 N2 121.4(8) . . ? C20 C19 N2 115.2(8) . . ? C21 C20 C19 117.1(9) . . ? C21 C20 C25 118.9(8) . . ? C19 C20 C25 123.8(8) . . ? C20 C21 C22 121.6(9) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 119.4(9) . . ? C23 C22 C26 120.3(10) . . ? C21 C22 C26 120.4(10) . . ? C22 C23 C24 119.7(9) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 119.0(9) . . ? C19 C24 C27 121.6(8) . . ? C23 C24 C27 119.4(9) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O3 C28 O2 124.6(8) . . ? O3 C28 C29 121.0(9) . . ? O2 C28 C29 114.4(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 N1 Pd1 O1 C1 -8.3(6) . . . . ? O2 Pd1 O1 C1 170.1(6) . . . . ? O1 Pd1 O2 C28 -77.8(6) . . . . ? N2 Pd1 O2 C28 108.5(6) . . . . ? O1 Pd1 N1 C13 7.7(6) . . . . ? N2 Pd1 N1 C13 -178.7(6) . . . . ? O1 Pd1 N1 C17 -176.5(5) . . . . ? N2 Pd1 N1 C17 -2.9(5) . . . . ? N1 Pd1 N2 C18 1.3(6) . . . . ? O2 Pd1 N2 C18 -176.8(6) . . . . ? N1 Pd1 N2 C19 -169.7(6) . . . . ? O2 Pd1 N2 C19 12.2(6) . . . . ? Pd1 O1 C1 C2 5.4(11) . . . . ? Pd1 O1 C1 C6 -171.5(5) . . . . ? O1 C1 C2 C3 -179.4(7) . . . . ? C6 C1 C2 C3 -2.7(11) . . . . ? O1 C1 C2 C13 1.4(13) . . . . ? C6 C1 C2 C13 178.1(7) . . . . ? C1 C2 C3 C4 1.3(12) . . . . ? C13 C2 C3 C4 -179.4(8) . . . . ? C2 C3 C4 C5 -0.2(13) . . . . ? C3 C4 C5 C6 0.5(13) . . . . ? C4 C5 C6 C1 -2.0(12) . . . . ? C4 C5 C6 C7 177.1(8) . . . . ? O1 C1 C6 C5 -179.8(7) . . . . ? C2 C1 C6 C5 3.1(12) . . . . ? O1 C1 C6 C7 1.1(10) . . . . ? C2 C1 C6 C7 -176.0(7) . . . . ? C5 C6 C7 C12 -134.5(9) . . . . ? C1 C6 C7 C12 44.6(12) . . . . ? C5 C6 C7 C8 38.9(11) . . . . ? C1 C6 C7 C8 -142.0(8) . . . . ? C12 C7 C8 C9 -0.5(14) . . . . ? C6 C7 C8 C9 -174.2(8) . . . . ? C7 C8 C9 C10 2.9(16) . . . . ? C8 C9 C10 C11 -2.7(16) . . . . ? C9 C10 C11 C12 0.2(16) . . . . ? C8 C7 C12 C11 -2.1(14) . . . . ? C6 C7 C12 C11 171.3(8) . . . . ? C10 C11 C12 C7 2.3(15) . . . . ? C17 N1 C13 C14 0.3(10) . . . . ? Pd1 N1 C13 C14 175.8(5) . . . . ? C17 N1 C13 C2 -179.4(7) . . . . ? Pd1 N1 C13 C2 -3.9(10) . . . . ? C3 C2 C13 N1 178.6(7) . . . . ? C1 C2 C13 N1 -2.1(12) . . . . ? C3 C2 C13 C14 -1.0(11) . . . . ? C1 C2 C13 C14 178.2(8) . . . . ? N1 C13 C14 C15 0.4(11) . . . . ? C2 C13 C14 C15 -180.0(8) . . . . ? C13 C14 C15 C16 -0.9(12) . . . . ? C14 C15 C16 C17 0.7(12) . . . . ? C15 C16 C17 N1 -0.1(12) . . . . ? C15 C16 C17 C18 179.4(7) . . . . ? C13 N1 C17 C16 -0.5(11) . . . . ? Pd1 N1 C17 C16 -176.5(6) . . . . ? C13 N1 C17 C18 -180.0(7) . . . . ? Pd1 N1 C17 C18 4.0(8) . . . . ? C19 N2 C18 C17 171.4(7) . . . . ? Pd1 N2 C18 C17 0.5(9) . . . . ? C16 C17 C18 N2 177.4(7) . . . . ? N1 C17 C18 N2 -3.1(10) . . . . ? C18 N2 C19 C24 110.1(10) . . . . ? Pd1 N2 C19 C24 -79.7(10) . . . . ? C18 N2 C19 C20 -75.2(10) . . . . ? Pd1 N2 C19 C20 95.0(8) . . . . ? C24 C19 C20 C21 2.2(13) . . . . ? N2 C19 C20 C21 -172.3(7) . . . . ? C24 C19 C20 C25 175.7(8) . . . . ? N2 C19 C20 C25 1.2(12) . . . . ? C19 C20 C21 C22 -0.5(13) . . . . ? C25 C20 C21 C22 -174.3(8) . . . . ? C20 C21 C22 C23 -2.3(14) . . . . ? C20 C21 C22 C26 178.5(9) . . . . ? C21 C22 C23 C24 3.4(14) . . . . ? C26 C22 C23 C24 -177.4(9) . . . . ? C20 C19 C24 C23 -1.1(14) . . . . ? N2 C19 C24 C23 173.1(8) . . . . ? C20 C19 C24 C27 177.7(8) . . . . ? N2 C19 C24 C27 -8.1(13) . . . . ? C22 C23 C24 C19 -1.8(14) . . . . ? C22 C23 C24 C27 179.4(9) . . . . ? Pd1 O2 C28 O3 0.5(11) . . . . ? Pd1 O2 C28 C29 -177.9(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.671 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.142 data_10081 _database_code_depnum_ccdc_archive 'CCDC 919251' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: ...Due to the Squeeze option in Platon, reported sum formula does not agree with the calculated sum formula. 'see_platon_squeeze_details' ; _vrf_RINTA01_I ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: ... Due to weak data 'see _exptl_special_details' ; _vrf_PLAT020_I ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.334 RESPONSE: ...Due to weak data 'see _exptl_special_details' ; _vrf_PLAT051_I ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 31.79 Perc. RESPONSE: ... Due to the Squeeze option in Platon, reported sum formula does not agree with the calculated sum formula. 'see_platon_squeeze_details' ; _vrf_PLAT213_I ; PROBLEM: Atom C13 has ADP max/min Ratio ..... 5.7 oblat RESPONSE: ... see _exptl_special_details ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 N2 O3 Pd,C H Cl3,3(C6 H14) ' _chemical_formula_sum 'C52 H79 Cl3 N2 O3 Pd' _chemical_formula_weight 992.92 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 22.469(7) _cell_length_b 22.469(7) _cell_length_c 22.469(7) _cell_angle_alpha 115.655(6) _cell_angle_beta 115.655(6) _cell_angle_gamma 115.655(6) _cell_volume 5952(3) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 603 _cell_measurement_theta_min 2.174 _cell_measurement_theta_max 23.370 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3156 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.269 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 3153 reflections(SADABS);Rint 0.2032 before correction and 0.1767 after. ; _exptl_special_details ; The crystals and hence data were not the best. The data was weak. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46610 _diffrn_reflns_av_R_equivalents 0.3336 _diffrn_reflns_av_sigmaI/netI 0.3312 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7800 _reflns_number_gt 3035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0403P)^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 7800 _refine_ls_number_parameters 358 _refine_ls_number_restraints 351 _refine_ls_R_factor_all 0.1881 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.012 -0.012 -0.012 2020 1275 ' ' _platon_squeeze_details ; Disordered CHCl3 and C6H14 were omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 2022.3 3 with an estimated 1275e/cell to be added. Six solvent CHCl3 and eighteen C6H14 molecules/unit cell accounting for 1248e were included in the formula, FWt, (000) and density calculations. PLATON Reference:Spek, A.L. (1990), Acta Cryst. A46, C-34 ; 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 -0.00659(5) 0.55542(5) 0.47754(5) 0.02676(19) Uani 1 1 d U . . O1 O -0.1209(4) 0.4205(4) 0.3331(4) 0.0266(13) Uani 1 1 d U . . O2 O -0.0962(4) 0.5160(4) 0.4903(4) 0.0269(13) Uani 1 1 d U . . O3 O -0.1397(5) 0.5768(5) 0.4526(5) 0.0513(17) Uani 1 1 d U . . N1 N 0.0888(5) 0.6010(5) 0.4753(5) 0.0281(15) Uani 1 1 d U . . N2 N 0.1216(5) 0.6930(5) 0.6298(4) 0.0316(16) Uani 1 1 d U . . H2 H 0.1286 0.6901 0.6646 0.038 Uiso 1 1 d R . . C1 C -0.1329(6) 0.4149(6) 0.2660(6) 0.0262(18) Uani 1 1 d U . . C2 C -0.0533(7) 0.4757(6) 0.2878(6) 0.038(2) Uani 1 1 d U . . C3 C -0.0726(7) 0.4621(7) 0.2104(7) 0.036(2) Uani 1 1 d U . . H3 H -0.0171 0.5045 0.2255 0.043 Uiso 1 1 calc R . . C4 C -0.1720(7) 0.3872(7) 0.1143(7) 0.046(2) Uani 1 1 d U . . H4 H -0.1864 0.3758 0.0616 0.056 Uiso 1 1 calc R . . C5 C -0.2506(7) 0.3288(6) 0.0969(6) 0.043(2) Uani 1 1 d U . . H5 H -0.3191 0.2773 0.0309 0.051 Uiso 1 1 calc R . . C6 C -0.2346(7) 0.3417(6) 0.1702(6) 0.038(2) Uani 1 1 d U . . C7 C -0.3228(6) 0.2759(7) 0.1435(6) 0.037(2) Uani 1 1 d U . . C8 C -0.3255(7) 0.3169(6) 0.2088(6) 0.039(2) Uani 1 1 d U . . H8 H -0.2661 0.3870 0.2747 0.047 Uiso 1 1 calc R . . C9 C -0.4112(7) 0.2587(7) 0.1801(7) 0.044(2) Uani 1 1 d U . . H9 H -0.4111 0.2885 0.2258 0.053 Uiso 1 1 calc R . . C10 C -0.4993(7) 0.1557(7) 0.0840(7) 0.055(3) Uani 1 1 d U . . H10 H -0.5600 0.1158 0.0630 0.066 Uiso 1 1 calc R . . C11 C -0.4977(7) 0.1130(8) 0.0209(7) 0.055(3) Uani 1 1 d U . . H11 H -0.5559 0.0415 -0.0417 0.066 Uiso 1 1 calc R . . C12 C -0.4141(7) 0.1702(6) 0.0445(6) 0.048(2) Uani 1 1 d U . . H12 H -0.4173 0.1400 -0.0040 0.058 Uiso 1 1 calc R . . C13 C 0.0587(6) 0.5537(6) 0.3872(7) 0.0313(18) Uani 1 1 d U . . C14 C 0.1270(7) 0.5839(7) 0.3917(7) 0.045(2) Uani 1 1 d U . . H14 H 0.1044 0.5500 0.3300 0.054 Uiso 1 1 calc R . . C15 C 0.2360(7) 0.6675(7) 0.4881(7) 0.050(3) Uani 1 1 d U . . H15 H 0.2856 0.6875 0.4919 0.060 Uiso 1 1 calc R . . C16 C 0.2614(7) 0.7154(7) 0.5740(7) 0.049(2) Uani 1 1 d U . . H16 H 0.3315 0.7755 0.6398 0.058 Uiso 1 1 calc R . . C17 C 0.1878(7) 0.6780(7) 0.5665(7) 0.043(2) Uani 1 1 d U . . C18 C 0.2106(6) 0.7174(6) 0.6550(6) 0.039(2) Uani 1 1 d U . . H18 H 0.2108 0.6768 0.6625 0.047 Uiso 1 1 calc R . . C19 C 0.1400(6) 0.7768(6) 0.6799(6) 0.033(2) Uani 1 1 d U . . C20 C 0.1216(7) 0.8073(6) 0.6362(6) 0.042(2) Uani 1 1 d U . . C21 C 0.1461(6) 0.8912(6) 0.6923(7) 0.040(2) Uani 1 1 d U . . H21 H 0.1396 0.9157 0.6674 0.048 Uiso 1 1 calc R . . C22 C 0.1786(7) 0.9407(7) 0.7800(7) 0.051(3) Uani 1 1 d U . . H22 H 0.1938 0.9980 0.8149 0.061 Uiso 1 1 calc R . . C23 C 0.1900(7) 0.9080(7) 0.8196(7) 0.048(2) Uani 1 1 d U . . H23 H 0.2100 0.9405 0.8799 0.058 Uiso 1 1 calc R . . C24 C 0.1715(6) 0.8268(6) 0.7693(6) 0.035(2) Uani 1 1 d U . . C25 C 0.3136(6) 0.8278(6) 0.7562(6) 0.046(2) Uani 1 1 d U . . H25A H 0.3672 0.8388 0.7698 0.068 Uiso 1 1 calc R . . H25B H 0.3242 0.8449 0.8105 0.068 Uiso 1 1 calc R . . H25C H 0.3165 0.8715 0.7540 0.068 Uiso 1 1 calc R . . C26 C 0.0831(6) 0.7541(6) 0.5375(6) 0.037(2) Uani 1 1 d U . . H26 H 0.0494 0.6846 0.4989 0.045 Uiso 1 1 calc R . . C27 C 0.1787(7) 0.7876(6) 0.8120(6) 0.038(2) Uani 1 1 d U . . H27 H 0.1930 0.7523 0.7895 0.046 Uiso 1 1 calc R . . C28 C 0.0016(7) 0.7409(6) 0.4705(6) 0.048(2) Uani 1 1 d U . . H28A H -0.0552 0.7021 0.4572 0.071 Uiso 1 1 calc R . . H28B H -0.0242 0.7040 0.4054 0.071 Uiso 1 1 calc R . . H28C H 0.0333 0.8083 0.5069 0.071 Uiso 1 1 calc R . . C29 C 0.1730(7) 0.8134(7) 0.5576(7) 0.050(2) Uani 1 1 d U . . H29A H 0.1957 0.8740 0.5793 0.076 Uiso 1 1 calc R . . H29B H 0.1500 0.7690 0.4948 0.076 Uiso 1 1 calc R . . H29C H 0.2298 0.8345 0.6116 0.076 Uiso 1 1 calc R . . C30 C 0.2665(7) 0.8764(6) 0.9302(6) 0.046(2) Uani 1 1 d U . . H30A H 0.3242 0.9364 0.9574 0.069 Uiso 1 1 calc R . . H30B H 0.2885 0.8555 0.9549 0.069 Uiso 1 1 calc R . . H30C H 0.2424 0.8934 0.9533 0.069 Uiso 1 1 calc R . . C31 C 0.0764(7) 0.7091(7) 0.7691(7) 0.054(3) Uani 1 1 d U . . H31A H 0.0559 0.7390 0.7819 0.081 Uiso 1 1 calc R . . H31B H 0.0857 0.6920 0.8031 0.081 Uiso 1 1 calc R . . H31C H 0.0232 0.6470 0.6954 0.081 Uiso 1 1 calc R . . C32 C -0.1442(7) 0.5332(7) 0.4740(7) 0.039(2) Uani 1 1 d U . . C33 C -0.2080(7) 0.5012(7) 0.4871(8) 0.060(3) Uani 1 1 d U . . H33A H -0.1655 0.5571 0.5588 0.090 Uiso 1 1 calc R . . H33B H -0.2339 0.4406 0.4676 0.090 Uiso 1 1 calc R . . H33C H -0.2657 0.4852 0.4436 0.090 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 0.0284(4) 0.0246(4) 0.0249(4) 0.0191(3) 0.0203(3) 0.0192(3) O1 0.029(3) 0.018(3) 0.022(3) 0.016(2) 0.018(3) 0.015(3) O2 0.026(3) 0.026(3) 0.028(3) 0.019(3) 0.024(3) 0.019(3) O3 0.062(5) 0.058(5) 0.059(4) 0.051(4) 0.048(4) 0.048(4) N1 0.029(3) 0.032(4) 0.035(3) 0.027(3) 0.030(3) 0.021(3) N2 0.029(3) 0.028(4) 0.014(3) 0.012(3) 0.014(3) 0.019(3) C1 0.026(4) 0.013(4) 0.015(4) 0.008(4) 0.012(3) 0.011(4) C2 0.043(4) 0.032(5) 0.029(4) 0.023(4) 0.026(4) 0.027(4) C3 0.056(5) 0.050(6) 0.052(5) 0.048(5) 0.047(4) 0.045(5) C4 0.047(5) 0.075(7) 0.044(5) 0.050(6) 0.038(5) 0.049(6) C5 0.039(5) 0.032(5) 0.021(5) 0.019(4) 0.015(4) 0.022(5) C6 0.048(4) 0.031(5) 0.029(4) 0.024(4) 0.027(4) 0.028(4) C7 0.023(4) 0.031(5) 0.024(5) 0.017(4) 0.010(4) 0.019(4) C8 0.035(5) 0.025(5) 0.023(5) 0.014(4) 0.015(4) 0.021(4) C9 0.034(5) 0.048(5) 0.038(5) 0.033(4) 0.023(5) 0.031(5) C10 0.030(5) 0.047(6) 0.049(6) 0.037(5) 0.023(5) 0.022(4) C11 0.036(5) 0.033(5) 0.036(6) 0.020(5) 0.019(5) 0.017(5) C12 0.056(6) 0.027(5) 0.021(5) 0.013(4) 0.024(5) 0.028(4) C13 0.044(4) 0.047(5) 0.049(4) 0.045(4) 0.037(4) 0.043(4) C14 0.055(5) 0.051(6) 0.042(5) 0.035(5) 0.044(4) 0.040(5) C15 0.036(5) 0.051(6) 0.041(5) 0.037(5) 0.030(5) 0.023(5) C16 0.021(5) 0.042(6) 0.043(5) 0.028(5) 0.021(4) 0.016(5) C17 0.039(4) 0.041(5) 0.030(4) 0.024(4) 0.026(4) 0.027(4) C18 0.032(4) 0.021(4) 0.032(4) 0.016(4) 0.023(4) 0.014(4) C19 0.044(5) 0.028(4) 0.030(4) 0.024(4) 0.029(4) 0.027(4) C20 0.045(5) 0.025(5) 0.029(4) 0.019(4) 0.026(4) 0.019(5) C21 0.054(6) 0.038(5) 0.042(5) 0.034(5) 0.033(5) 0.040(5) C22 0.063(6) 0.030(5) 0.039(6) 0.025(5) 0.033(6) 0.035(5) C23 0.074(7) 0.033(5) 0.040(5) 0.029(5) 0.044(5) 0.041(5) C24 0.049(5) 0.025(5) 0.036(5) 0.025(4) 0.035(5) 0.027(5) C25 0.029(5) 0.029(5) 0.031(5) 0.016(4) 0.017(4) 0.016(4) C26 0.037(5) 0.019(5) 0.024(5) 0.014(4) 0.019(4) 0.016(4) C27 0.058(6) 0.020(5) 0.020(4) 0.013(4) 0.027(5) 0.028(5) C28 0.047(6) 0.035(6) 0.035(5) 0.025(5) 0.026(5) 0.030(5) C29 0.073(7) 0.057(7) 0.059(7) 0.052(6) 0.055(6) 0.053(6) C30 0.060(6) 0.035(5) 0.020(4) 0.020(4) 0.026(5) 0.033(5) C31 0.060(6) 0.047(6) 0.057(6) 0.042(5) 0.043(5) 0.040(5) C32 0.034(5) 0.028(5) 0.037(6) 0.022(5) 0.027(5) 0.020(5) C33 0.057(7) 0.060(7) 0.084(8) 0.057(7) 0.059(7) 0.046(6) _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 O1 1.959(5) . ? Pd1 N1 1.971(6) . ? Pd1 O2 2.025(5) . ? Pd1 N2 2.038(6) . ? Pd1 Pd1 3.1409(15) 4_566 ? O1 C1 1.350(8) . ? O2 C32 1.260(9) . ? O3 C32 1.250(9) . ? N1 C17 1.338(10) . ? N1 C13 1.378(9) . ? N2 C19 1.440(9) . ? N2 C18 1.557(10) . ? N2 H2 0.7658 . ? C1 C2 1.359(10) . ? C1 C6 1.407(11) . ? C2 C3 1.443(10) . ? C2 C13 1.523(11) . ? C3 C4 1.381(11) . ? C3 H3 0.9500 . ? C4 C5 1.395(11) . ? C4 H4 0.9500 . ? C5 C6 1.382(10) . ? C5 H5 0.9500 . ? C6 C7 1.462(11) . ? C7 C8 1.401(11) . ? C7 C12 1.432(11) . ? C8 C9 1.359(11) . ? C8 H8 0.9500 . ? C9 C10 1.394(12) . ? C9 H9 0.9500 . ? C10 C11 1.352(12) . ? C10 H10 0.9500 . ? C11 C12 1.385(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.314(10) . ? C14 C15 1.456(11) . ? C14 H14 0.9500 . ? C15 C16 1.387(11) . ? C15 H15 0.9500 . ? C16 C17 1.380(11) . ? C16 H16 0.9500 . ? C17 C18 1.484(11) . ? C18 C25 1.505(10) . ? C18 H18 1.0000 . ? C19 C24 1.386(10) . ? C19 C20 1.443(10) . ? C20 C21 1.374(10) . ? C20 C26 1.497(11) . ? C21 C22 1.344(11) . ? C21 H21 0.9500 . ? C22 C23 1.389(11) . ? C22 H22 0.9500 . ? C23 C24 1.391(10) . ? C23 H23 0.9500 . ? C24 C27 1.561(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C29 1.554(11) . ? C26 C28 1.569(10) . ? C26 H26 1.0000 . ? C27 C30 1.548(10) . ? C27 C31 1.558(11) . ? C27 H27 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 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.522(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 O1 Pd1 N1 92.5(2) . . ? O1 Pd1 O2 91.2(2) . . ? N1 Pd1 O2 176.1(2) . . ? O1 Pd1 N2 173.4(2) . . ? N1 Pd1 N2 83.4(3) . . ? O2 Pd1 N2 92.8(2) . . ? O1 Pd1 Pd1 85.34(14) . 4_566 ? N1 Pd1 Pd1 101.40(19) . 4_566 ? O2 Pd1 Pd1 77.48(15) . 4_566 ? N2 Pd1 Pd1 90.37(18) . 4_566 ? C1 O1 Pd1 118.5(4) . . ? C32 O2 Pd1 120.0(5) . . ? C17 N1 C13 120.6(7) . . ? C17 N1 Pd1 115.1(5) . . ? C13 N1 Pd1 124.1(6) . . ? C19 N2 C18 117.6(6) . . ? C19 N2 Pd1 124.2(5) . . ? C18 N2 Pd1 104.5(4) . . ? C19 N2 H2 96.0 . . ? C18 N2 H2 97.0 . . ? Pd1 N2 H2 114.2 . . ? O1 C1 C2 123.3(7) . . ? O1 C1 C6 115.5(7) . . ? C2 C1 C6 121.3(8) . . ? C1 C2 C3 120.0(8) . . ? C1 C2 C13 125.1(7) . . ? C3 C2 C13 114.7(8) . . ? C4 C3 C2 119.7(8) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 117.8(8) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 123.8(8) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C5 C6 C1 117.2(8) . . ? C5 C6 C7 119.2(8) . . ? C1 C6 C7 123.4(7) . . ? C8 C7 C12 117.6(8) . . ? C8 C7 C6 120.9(8) . . ? C12 C7 C6 121.0(8) . . ? C9 C8 C7 121.5(9) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 120.4(9) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.4(10) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 122.2(10) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 118.6(9) . . ? C11 C12 H12 120.7 . . ? C7 C12 H12 120.7 . . ? C14 C13 N1 120.4(8) . . ? C14 C13 C2 121.5(8) . . ? N1 C13 C2 117.6(7) . . ? C13 C14 C15 122.2(8) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 114.4(8) . . ? C16 C15 H15 122.8 . . ? C14 C15 H15 122.8 . . ? C17 C16 C15 121.8(9) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? N1 C17 C16 120.2(8) . . ? N1 C17 C18 115.9(8) . . ? C16 C17 C18 123.9(8) . . ? C17 C18 C25 115.5(7) . . ? C17 C18 N2 110.0(7) . . ? C25 C18 N2 112.5(7) . . ? C17 C18 H18 106.0 . . ? C25 C18 H18 106.0 . . ? N2 C18 H18 106.0 . . ? C24 C19 N2 120.1(7) . . ? C24 C19 C20 118.8(8) . . ? N2 C19 C20 121.1(7) . . ? C21 C20 C19 116.6(8) . . ? C21 C20 C26 121.3(8) . . ? C19 C20 C26 122.0(8) . . ? C22 C21 C20 124.1(8) . . ? C22 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? C21 C22 C23 120.0(9) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 118.7(8) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C19 C24 C23 121.5(8) . . ? C19 C24 C27 120.8(7) . . ? C23 C24 C27 117.5(7) . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 C29 110.7(7) . . ? C20 C26 C28 110.9(7) . . ? C29 C26 C28 110.6(7) . . ? C20 C26 H26 108.2 . . ? C29 C26 H26 108.2 . . ? C28 C26 H26 108.2 . . ? C30 C27 C31 109.2(7) . . ? C30 C27 C24 112.0(6) . . ? C31 C27 C24 111.5(7) . . ? C30 C27 H27 108.0 . . ? C31 C27 H27 108.0 . . ? C24 C27 H27 108.0 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 O2 125.4(8) . . ? O3 C32 C33 119.6(8) . . ? O2 C32 C33 115.0(8) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 N1 Pd1 O1 C1 -42.5(5) . . . . ? O2 Pd1 O1 C1 138.9(5) . . . . ? Pd1 Pd1 O1 C1 -143.7(5) 4_566 . . . ? O1 Pd1 O2 C32 -90.9(6) . . . . ? N2 Pd1 O2 C32 94.4(6) . . . . ? Pd1 Pd1 O2 C32 -175.9(6) 4_566 . . . ? O1 Pd1 N1 C17 -157.5(6) . . . . ? N2 Pd1 N1 C17 17.3(6) . . . . ? Pd1 Pd1 N1 C17 -71.7(6) 4_566 . . . ? O1 Pd1 N1 C13 17.0(6) . . . . ? N2 Pd1 N1 C13 -168.2(6) . . . . ? Pd1 Pd1 N1 C13 102.8(6) 4_566 . . . ? N1 Pd1 N2 C19 111.3(6) . . . . ? O2 Pd1 N2 C19 -69.7(6) . . . . ? Pd1 Pd1 N2 C19 -147.2(6) 4_566 . . . ? N1 Pd1 N2 C18 -27.6(5) . . . . ? O2 Pd1 N2 C18 151.4(5) . . . . ? Pd1 Pd1 N2 C18 73.9(4) 4_566 . . . ? Pd1 O1 C1 C2 38.3(9) . . . . ? Pd1 O1 C1 C6 -141.2(6) . . . . ? O1 C1 C2 C3 177.3(7) . . . . ? C6 C1 C2 C3 -3.2(12) . . . . ? O1 C1 C2 C13 3.3(12) . . . . ? C6 C1 C2 C13 -177.2(7) . . . . ? C1 C2 C3 C4 -0.1(12) . . . . ? C13 C2 C3 C4 174.5(7) . . . . ? C2 C3 C4 C5 1.7(13) . . . . ? C3 C4 C5 C6 0.0(13) . . . . ? C4 C5 C6 C1 -3.1(13) . . . . ? C4 C5 C6 C7 -179.8(8) . . . . ? O1 C1 C6 C5 -175.8(7) . . . . ? C2 C1 C6 C5 4.7(12) . . . . ? O1 C1 C6 C7 0.7(11) . . . . ? C2 C1 C6 C7 -178.8(8) . . . . ? C5 C6 C7 C8 -134.4(8) . . . . ? C1 C6 C7 C8 49.1(12) . . . . ? C5 C6 C7 C12 37.3(12) . . . . ? C1 C6 C7 C12 -139.2(9) . . . . ? C12 C7 C8 C9 0.6(12) . . . . ? C6 C7 C8 C9 172.5(7) . . . . ? C7 C8 C9 C10 0.1(13) . . . . ? C8 C9 C10 C11 2.4(14) . . . . ? C9 C10 C11 C12 -5.9(15) . . . . ? C10 C11 C12 C7 6.6(14) . . . . ? C8 C7 C12 C11 -3.8(12) . . . . ? C6 C7 C12 C11 -175.7(8) . . . . ? C17 N1 C13 C14 -0.4(12) . . . . ? Pd1 N1 C13 C14 -174.6(6) . . . . ? C17 N1 C13 C2 -172.8(7) . . . . ? Pd1 N1 C13 C2 13.0(9) . . . . ? C1 C2 C13 C14 156.3(8) . . . . ? C3 C2 C13 C14 -18.0(11) . . . . ? C1 C2 C13 N1 -31.4(12) . . . . ? C3 C2 C13 N1 154.3(7) . . . . ? N1 C13 C14 C15 -0.1(13) . . . . ? C2 C13 C14 C15 172.0(8) . . . . ? C13 C14 C15 C16 -3.3(13) . . . . ? C14 C15 C16 C17 7.3(14) . . . . ? C13 N1 C17 C16 4.5(13) . . . . ? Pd1 N1 C17 C16 179.2(7) . . . . ? C13 N1 C17 C18 -175.0(7) . . . . ? Pd1 N1 C17 C18 -0.3(10) . . . . ? C15 C16 C17 N1 -8.2(14) . . . . ? C15 C16 C17 C18 171.2(9) . . . . ? N1 C17 C18 C25 -152.4(8) . . . . ? C16 C17 C18 C25 28.1(13) . . . . ? N1 C17 C18 N2 -23.8(11) . . . . ? C16 C17 C18 N2 156.8(8) . . . . ? C19 N2 C18 C17 -107.9(8) . . . . ? Pd1 N2 C18 C17 34.3(7) . . . . ? C19 N2 C18 C25 22.4(10) . . . . ? Pd1 N2 C18 C25 164.5(6) . . . . ? C18 N2 C19 C24 -94.6(9) . . . . ? Pd1 N2 C19 C24 131.2(7) . . . . ? C18 N2 C19 C20 88.2(9) . . . . ? Pd1 N2 C19 C20 -45.9(10) . . . . ? C24 C19 C20 C21 5.8(12) . . . . ? N2 C19 C20 C21 -177.0(7) . . . . ? C24 C19 C20 C26 -177.3(8) . . . . ? N2 C19 C20 C26 -0.1(13) . . . . ? C19 C20 C21 C22 -4.8(13) . . . . ? C26 C20 C21 C22 178.3(9) . . . . ? C20 C21 C22 C23 0.5(15) . . . . ? C21 C22 C23 C24 2.8(14) . . . . ? N2 C19 C24 C23 180.0(7) . . . . ? C20 C19 C24 C23 -2.8(13) . . . . ? N2 C19 C24 C27 -5.2(12) . . . . ? C20 C19 C24 C27 172.0(8) . . . . ? C22 C23 C24 C19 -1.6(14) . . . . ? C22 C23 C24 C27 -176.5(8) . . . . ? C21 C20 C26 C29 79.5(10) . . . . ? C19 C20 C26 C29 -97.3(9) . . . . ? C21 C20 C26 C28 -43.6(11) . . . . ? C19 C20 C26 C28 139.6(8) . . . . ? C19 C24 C27 C30 147.1(8) . . . . ? C23 C24 C27 C30 -37.9(11) . . . . ? C19 C24 C27 C31 -90.2(10) . . . . ? C23 C24 C27 C31 84.8(9) . . . . ? Pd1 O2 C32 O3 -2.4(12) . . . . ? Pd1 O2 C32 C33 -179.4(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O1 0.77 2.44 3.001(8) 131.4 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.565 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.114 data_10082 _database_code_depnum_ccdc_archive 'CCDC 919252' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H25 Cl N2 O Pd, C H2 Cl2' _chemical_formula_sum 'C28 H27 Cl3 N2 O Pd' _chemical_formula_weight 620.27 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' 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 9.632(9) _cell_length_b 11.597(11) _cell_length_c 13.229(12) _cell_angle_alpha 90.567(19) _cell_angle_beta 108.415(19) _cell_angle_gamma 112.533(18) _cell_volume 1280(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 517 _cell_measurement_theta_min 2.415 _cell_measurement_theta_max 23.440 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.358 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 2947 reflections(SADABS);Rint 0.1172 before correction and 0.0663 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10113 _diffrn_reflns_av_R_equivalents 0.1186 _diffrn_reflns_av_sigmaI/netI 0.1736 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4967 _reflns_number_gt 3330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; GEMINI,the twinning program was used to find the cell. 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^)+(0.1217P)^2^+25.6433P] 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 4967 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.1151 _refine_ls_wR_factor_ref 0.3219 _refine_ls_wR_factor_gt 0.3053 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.51241(13) 0.87397(10) 0.55100(9) 0.0220(4) Uani 1 1 d . . . Cl1 Cl 0.7150(4) 0.8911(3) 0.4874(3) 0.0310(8) Uani 1 1 d . . . O1 O 0.6625(12) 1.0077(9) 0.6774(8) 0.026(2) Uani 1 1 d . . . N1 N 0.3333(15) 0.8413(11) 0.6036(10) 0.028(3) Uani 1 1 d . . . N2 N 0.3351(15) 0.7634(10) 0.4131(10) 0.029(3) Uani 1 1 d . . . H2 H 0.3485 0.8149 0.3604 0.035 Uiso 1 1 calc R . . C1 C 0.6551(17) 0.9844(12) 0.7734(11) 0.023(3) Uani 1 1 d . . . C2 C 0.5101(18) 0.9199(13) 0.7934(11) 0.029(3) Uani 1 1 d . . . C3 C 0.518(2) 0.8977(14) 0.8996(12) 0.034(4) Uani 1 1 d . . . H3 H 0.4215 0.8520 0.9129 0.041 Uiso 1 1 calc R . . C4 C 0.663(2) 0.9408(15) 0.9849(13) 0.036(4) Uani 1 1 d . . . H4 H 0.6657 0.9222 1.0551 0.043 Uiso 1 1 calc R . . C5 C 0.8017(19) 1.0110(13) 0.9658(12) 0.029(3) Uani 1 1 d . . . H5 H 0.8997 1.0461 1.0249 0.035 Uiso 1 1 calc R . . C6 C 0.8029(18) 1.0319(13) 0.8632(11) 0.028(3) Uani 1 1 d . . . C7 C 0.9534(17) 1.1105(13) 0.8442(11) 0.024(3) Uani 1 1 d . . . C8 C 1.058(2) 1.2249(15) 0.9131(14) 0.040(4) Uani 1 1 d . . . H8 H 1.0325 1.2505 0.9710 0.047 Uiso 1 1 calc R . . C9 C 1.200(2) 1.3013(17) 0.8962(15) 0.047(4) Uani 1 1 d . . . H9 H 1.2714 1.3778 0.9435 0.057 Uiso 1 1 calc R . . C10 C 1.236(2) 1.2649(17) 0.8097(16) 0.046(4) Uani 1 1 d . . . H10 H 1.3274 1.3188 0.7945 0.055 Uiso 1 1 calc R . . C11 C 1.1370(18) 1.1510(15) 0.7484(13) 0.036(4) Uani 1 1 d . . . H11 H 1.1653 1.1238 0.6928 0.043 Uiso 1 1 calc R . . C12 C 0.9991(18) 1.0738(14) 0.7629(11) 0.029(3) Uani 1 1 d . . . H12 H 0.9336 0.9949 0.7176 0.035 Uiso 1 1 calc R . . C13 C 0.3519(18) 0.8763(13) 0.7092(12) 0.028(3) Uani 1 1 d . . . C14 C 0.2177(19) 0.8705(14) 0.7324(13) 0.034(4) Uani 1 1 d . . . H14 H 0.2285 0.8981 0.8034 0.040 Uiso 1 1 calc R . . C15 C 0.0717(19) 0.8252(14) 0.6531(13) 0.035(4) Uani 1 1 d . . . H15 H -0.0191 0.8227 0.6686 0.041 Uiso 1 1 calc R . . C16 C 0.0544(18) 0.7826(14) 0.5496(13) 0.031(3) Uani 1 1 d . . . H16 H -0.0480 0.7475 0.4943 0.038 Uiso 1 1 calc R . . C17 C 0.1870(16) 0.7927(13) 0.5298(12) 0.028(3) Uani 1 1 d . . . C18 C 0.1799(17) 0.7488(14) 0.4169(12) 0.030(3) Uani 1 1 d . . . H18A H 0.1048 0.6588 0.3942 0.035 Uiso 1 1 calc R . . H18B H 0.1369 0.7980 0.3649 0.035 Uiso 1 1 calc R . . C19 C 0.3370(15) 0.6467(12) 0.3693(11) 0.024(3) Uani 1 1 d . . . C20 C 0.3114(17) 0.5422(12) 0.4262(11) 0.025(3) Uani 1 1 d . . . C21 C 0.3060(18) 0.4337(13) 0.3780(12) 0.032(3) Uani 1 1 d . . . H21 H 0.2850 0.3615 0.4136 0.038 Uiso 1 1 calc R . . C22 C 0.3297(17) 0.4238(13) 0.2795(12) 0.029(3) Uani 1 1 d . . . C23 C 0.3554(18) 0.5286(14) 0.2262(13) 0.032(3) Uani 1 1 d . . . H23 H 0.3688 0.5228 0.1585 0.038 Uiso 1 1 calc R . . C24 C 0.3623(16) 0.6432(13) 0.2693(12) 0.025(3) Uani 1 1 d . . . C25 C 0.2890(19) 0.5443(13) 0.5312(13) 0.032(3) Uani 1 1 d . . . H25A H 0.1766 0.5261 0.5198 0.048 Uiso 1 1 calc R . . H25B H 0.3574 0.6280 0.5741 0.048 Uiso 1 1 calc R . . H25C H 0.3180 0.4804 0.5694 0.048 Uiso 1 1 calc R . . C26 C 0.319(2) 0.3019(14) 0.2305(13) 0.039(4) Uani 1 1 d . . . H26A H 0.2073 0.2478 0.1889 0.058 Uiso 1 1 calc R . . H26B H 0.3616 0.2587 0.2878 0.058 Uiso 1 1 calc R . . H26C H 0.3826 0.3198 0.1828 0.058 Uiso 1 1 calc R . . C27 C 0.395(2) 0.7547(14) 0.2112(13) 0.034(4) Uani 1 1 d . . . H27A H 0.4912 0.8258 0.2578 0.051 Uiso 1 1 calc R . . H27B H 0.3035 0.7782 0.1922 0.051 Uiso 1 1 calc R . . H27C H 0.4122 0.7336 0.1455 0.051 Uiso 1 1 calc R . . C28 C 0.054(2) 0.5400(18) 0.8180(16) 0.054(5) Uani 1 1 d . . . H28A H -0.0331 0.5617 0.7723 0.064 Uiso 1 1 calc R . . H28B H 0.0064 0.4504 0.8275 0.064 Uiso 1 1 calc R . . Cl2 Cl 0.1420(8) 0.6336(6) 0.9422(5) 0.082(2) Uani 1 1 d . . . Cl3 Cl 0.1935(7) 0.5596(5) 0.7528(4) 0.0601(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0227(6) 0.0204(6) 0.0234(6) 0.0013(4) 0.0072(4) 0.0101(4) Cl1 0.0275(19) 0.0343(19) 0.037(2) 0.0053(16) 0.0156(16) 0.0145(16) O1 0.029(5) 0.021(5) 0.033(6) 0.006(4) 0.012(5) 0.012(4) N1 0.039(7) 0.025(6) 0.029(7) 0.005(5) 0.016(6) 0.019(6) N2 0.036(7) 0.018(6) 0.036(7) 0.005(5) 0.017(6) 0.011(5) C1 0.031(8) 0.017(6) 0.017(7) -0.006(5) 0.007(6) 0.007(6) C2 0.036(8) 0.029(8) 0.024(8) -0.003(6) 0.005(6) 0.021(7) C3 0.048(10) 0.026(8) 0.027(8) -0.006(6) 0.018(7) 0.010(7) C4 0.049(10) 0.041(9) 0.038(9) 0.014(7) 0.021(8) 0.034(8) C5 0.042(9) 0.025(7) 0.027(8) 0.002(6) 0.006(7) 0.025(7) C6 0.038(8) 0.029(7) 0.029(8) 0.004(6) 0.005(7) 0.030(7) C7 0.027(7) 0.029(7) 0.019(7) 0.003(6) 0.006(6) 0.018(6) C8 0.040(10) 0.037(9) 0.049(10) 0.005(8) 0.015(8) 0.024(8) C9 0.041(10) 0.044(10) 0.052(11) 0.011(9) 0.010(9) 0.017(8) C10 0.031(9) 0.050(11) 0.063(12) 0.016(9) 0.019(9) 0.019(8) C11 0.029(8) 0.044(9) 0.041(9) 0.007(8) 0.016(7) 0.018(7) C12 0.034(8) 0.035(8) 0.025(7) 0.005(6) 0.002(6) 0.028(7) C13 0.033(8) 0.020(7) 0.031(8) 0.004(6) 0.006(7) 0.014(6) C14 0.038(9) 0.031(8) 0.031(8) -0.005(7) 0.012(7) 0.012(7) C15 0.029(8) 0.032(8) 0.040(9) -0.001(7) 0.014(7) 0.009(7) C16 0.025(8) 0.031(8) 0.036(9) 0.000(7) 0.007(7) 0.013(6) C17 0.017(7) 0.022(7) 0.042(9) -0.003(6) 0.008(6) 0.007(6) C18 0.022(7) 0.025(7) 0.029(8) 0.003(6) 0.003(6) 0.002(6) C19 0.014(7) 0.020(7) 0.030(8) 0.001(6) 0.005(6) 0.002(5) C20 0.029(8) 0.016(6) 0.031(8) 0.006(6) 0.008(6) 0.012(6) C21 0.040(9) 0.016(7) 0.037(9) 0.008(6) 0.003(7) 0.018(6) C22 0.027(8) 0.022(7) 0.036(8) -0.002(6) 0.000(6) 0.017(6) C23 0.035(9) 0.027(8) 0.040(9) 0.004(7) 0.014(7) 0.019(7) C24 0.023(7) 0.022(7) 0.031(8) 0.001(6) 0.007(6) 0.013(6) C25 0.040(9) 0.021(7) 0.045(9) 0.008(6) 0.017(8) 0.021(7) C26 0.065(12) 0.028(8) 0.037(9) 0.005(7) 0.016(8) 0.035(8) C27 0.045(10) 0.028(8) 0.035(9) 0.007(7) 0.018(8) 0.018(7) C28 0.047(11) 0.048(11) 0.068(13) 0.006(10) 0.020(10) 0.021(9) Cl2 0.077(4) 0.089(4) 0.061(4) -0.022(3) 0.034(3) 0.007(3) Cl3 0.088(4) 0.049(3) 0.066(3) 0.015(2) 0.050(3) 0.032(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 N1 1.966(12) . ? Pd1 O1 1.999(10) . ? Pd1 N2 2.049(12) . ? Pd1 Cl1 2.302(4) . ? O1 C1 1.319(16) . ? N1 C17 1.330(18) . ? N1 C13 1.387(18) . ? N2 C18 1.456(19) . ? N2 C19 1.476(17) . ? N2 H2 0.9300 . ? C1 C2 1.42(2) . ? C1 C6 1.43(2) . ? C2 C3 1.41(2) . ? C2 C13 1.46(2) . ? C3 C4 1.39(2) . ? C3 H3 0.9500 . ? C4 C5 1.38(2) . ? C4 H4 0.9500 . ? C5 C6 1.38(2) . ? C5 H5 0.9500 . ? C6 C7 1.49(2) . ? C7 C12 1.402(19) . ? C7 C8 1.41(2) . ? C8 C9 1.40(2) . ? C8 H8 0.9500 . ? C9 C10 1.40(3) . ? C9 H9 0.9500 . ? C10 C11 1.35(2) . ? C10 H10 0.9500 . ? C11 C12 1.36(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.40(2) . ? C14 C15 1.36(2) . ? C14 H14 0.9500 . ? C15 C16 1.39(2) . ? C15 H15 0.9500 . ? C16 C17 1.35(2) . ? C16 H16 0.9500 . ? C17 C18 1.54(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.415(19) . ? C19 C24 1.42(2) . ? C20 C21 1.381(19) . ? C20 C25 1.47(2) . ? C21 C22 1.40(2) . ? C21 H21 0.9500 . ? C22 C23 1.39(2) . ? C22 C26 1.505(18) . ? C23 C24 1.410(19) . ? C23 H23 0.9500 . ? C24 C27 1.49(2) . ? 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 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Cl2 1.72(2) . ? C28 Cl3 1.760(19) . ? C28 H28A 0.9900 . ? C28 H28B 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 N1 Pd1 O1 91.3(4) . . ? N1 Pd1 N2 83.6(5) . . ? O1 Pd1 N2 167.6(4) . . ? N1 Pd1 Cl1 174.4(3) . . ? O1 Pd1 Cl1 92.3(3) . . ? N2 Pd1 Cl1 93.6(4) . . ? C1 O1 Pd1 118.0(8) . . ? C17 N1 C13 119.2(13) . . ? C17 N1 Pd1 116.5(10) . . ? C13 N1 Pd1 124.1(10) . . ? C18 N2 C19 114.1(11) . . ? C18 N2 Pd1 109.5(9) . . ? C19 N2 Pd1 120.9(9) . . ? C18 N2 H2 103.4 . . ? C19 N2 H2 103.4 . . ? Pd1 N2 H2 103.4 . . ? O1 C1 C2 124.0(13) . . ? O1 C1 C6 117.4(13) . . ? C2 C1 C6 118.5(12) . . ? C3 C2 C1 118.8(14) . . ? C3 C2 C13 118.2(14) . . ? C1 C2 C13 123.0(13) . . ? C4 C3 C2 121.8(15) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 118.8(14) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 122.1(15) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.8(14) . . ? C5 C6 C7 121.5(13) . . ? C1 C6 C7 118.6(12) . . ? C12 C7 C8 118.1(14) . . ? C12 C7 C6 123.1(13) . . ? C8 C7 C6 118.8(13) . . ? C9 C8 C7 119.8(16) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.1(17) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 118.5(16) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 123.0(16) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C7 120.3(14) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? N1 C13 C14 118.6(13) . . ? N1 C13 C2 120.0(13) . . ? C14 C13 C2 121.4(13) . . ? C15 C14 C13 119.8(14) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.4(15) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 117.9(15) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? N1 C17 C16 123.8(14) . . ? N1 C17 C18 114.5(12) . . ? C16 C17 C18 121.7(13) . . ? N2 C18 C17 113.3(12) . . ? N2 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? N2 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C24 122.3(12) . . ? C20 C19 N2 119.7(12) . . ? C24 C19 N2 118.0(12) . . ? C21 C20 C19 116.7(13) . . ? C21 C20 C25 119.9(12) . . ? C19 C20 C25 123.4(12) . . ? C20 C21 C22 123.8(13) . . ? C20 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C23 C22 C21 117.8(12) . . ? C23 C22 C26 121.0(14) . . ? C21 C22 C26 121.1(13) . . ? C22 C23 C24 122.2(14) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C23 C24 C19 117.1(13) . . ? C23 C24 C27 120.6(13) . . ? C19 C24 C27 122.3(12) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Cl2 C28 Cl3 111.8(11) . . ? Cl2 C28 H28A 109.3 . . ? Cl3 C28 H28A 109.3 . . ? Cl2 C28 H28B 109.3 . . ? Cl3 C28 H28B 109.3 . . ? H28A C28 H28B 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 N1 Pd1 O1 C1 43.4(10) . . . . ? N2 Pd1 O1 C1 109(2) . . . . ? Cl1 Pd1 O1 C1 -132.3(9) . . . . ? O1 Pd1 N1 C17 154.8(10) . . . . ? N2 Pd1 N1 C17 -13.8(10) . . . . ? Cl1 Pd1 N1 C17 -75(4) . . . . ? O1 Pd1 N1 C13 -19.1(11) . . . . ? N2 Pd1 N1 C13 172.3(11) . . . . ? Cl1 Pd1 N1 C13 111(4) . . . . ? N1 Pd1 N2 C18 14.2(9) . . . . ? O1 Pd1 N2 C18 -52(2) . . . . ? Cl1 Pd1 N2 C18 -170.8(9) . . . . ? N1 Pd1 N2 C19 -121.5(10) . . . . ? O1 Pd1 N2 C19 172.1(16) . . . . ? Cl1 Pd1 N2 C19 53.6(10) . . . . ? Pd1 O1 C1 C2 -39.1(16) . . . . ? Pd1 O1 C1 C6 143.4(9) . . . . ? O1 C1 C2 C3 178.4(12) . . . . ? C6 C1 C2 C3 -4.2(19) . . . . ? O1 C1 C2 C13 -2(2) . . . . ? C6 C1 C2 C13 175.1(12) . . . . ? C1 C2 C3 C4 2(2) . . . . ? C13 C2 C3 C4 -177.1(13) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C3 C4 C5 C6 -5(2) . . . . ? C4 C5 C6 C1 3(2) . . . . ? C4 C5 C6 C7 178.5(12) . . . . ? O1 C1 C6 C5 179.4(12) . . . . ? C2 C1 C6 C5 1.8(19) . . . . ? O1 C1 C6 C7 3.6(18) . . . . ? C2 C1 C6 C7 -174.0(12) . . . . ? C5 C6 C7 C12 133.8(14) . . . . ? C1 C6 C7 C12 -50.4(18) . . . . ? C5 C6 C7 C8 -43.9(19) . . . . ? C1 C6 C7 C8 131.9(14) . . . . ? C12 C7 C8 C9 3(2) . . . . ? C6 C7 C8 C9 -179.3(14) . . . . ? C7 C8 C9 C10 1(3) . . . . ? C8 C9 C10 C11 -5(3) . . . . ? C9 C10 C11 C12 4(3) . . . . ? C10 C11 C12 C7 0(2) . . . . ? C8 C7 C12 C11 -3(2) . . . . ? C6 C7 C12 C11 178.9(13) . . . . ? C17 N1 C13 C14 -6.1(19) . . . . ? Pd1 N1 C13 C14 167.7(10) . . . . ? C17 N1 C13 C2 174.8(13) . . . . ? Pd1 N1 C13 C2 -11.5(18) . . . . ? C3 C2 C13 N1 -150.2(13) . . . . ? C1 C2 C13 N1 31(2) . . . . ? C3 C2 C13 C14 31(2) . . . . ? C1 C2 C13 C14 -148.6(14) . . . . ? N1 C13 C14 C15 3(2) . . . . ? C2 C13 C14 C15 -177.6(14) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C17 -3(2) . . . . ? C13 N1 C17 C16 5(2) . . . . ? Pd1 N1 C17 C16 -169.5(12) . . . . ? C13 N1 C17 C18 -176.0(12) . . . . ? Pd1 N1 C17 C18 9.8(16) . . . . ? C15 C16 C17 N1 0(2) . . . . ? C15 C16 C17 C18 -179.5(14) . . . . ? C19 N2 C18 C17 126.1(13) . . . . ? Pd1 N2 C18 C17 -12.9(14) . . . . ? N1 C17 C18 N2 2.7(18) . . . . ? C16 C17 C18 N2 -177.9(13) . . . . ? C18 N2 C19 C20 -65.5(17) . . . . ? Pd1 N2 C19 C20 68.3(15) . . . . ? C18 N2 C19 C24 113.6(14) . . . . ? Pd1 N2 C19 C24 -112.6(12) . . . . ? C24 C19 C20 C21 -2(2) . . . . ? N2 C19 C20 C21 176.6(13) . . . . ? C24 C19 C20 C25 178.4(13) . . . . ? N2 C19 C20 C25 -3(2) . . . . ? C19 C20 C21 C22 2(2) . . . . ? C25 C20 C21 C22 -178.5(14) . . . . ? C20 C21 C22 C23 -2(2) . . . . ? C20 C21 C22 C26 -179.0(14) . . . . ? C21 C22 C23 C24 2(2) . . . . ? C26 C22 C23 C24 178.7(14) . . . . ? C22 C23 C24 C19 -2(2) . . . . ? C22 C23 C24 C27 178.1(14) . . . . ? C20 C19 C24 C23 2(2) . . . . ? N2 C19 C24 C23 -176.8(12) . . . . ? C20 C19 C24 C27 -177.7(13) . . . . ? N2 C19 C24 C27 3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O1 0.93 2.16 2.917(15) 138.4 2_676 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.842 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.239 #===END data_10093 _database_code_depnum_ccdc_archive 'CCDC 919253' #TrackingRef 'Revised_Cif_files_for_all_11_structures-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 Cl3 N2 O3 Pd' _chemical_formula_sum 'C30 H29 Cl3 N2 O3 Pd' _chemical_formula_weight 678.30 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.216(10) _cell_length_b 18.856(14) _cell_length_c 11.977(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.468(17) _cell_angle_gamma 90.00 _cell_volume 2935(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 612 _cell_measurement_theta_min 2.160 _cell_measurement_theta_max 23.400 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; absorption correction based on 3422 reflections(SADABS);Rint 0.1578 before correction and 0.0631 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22755 _diffrn_reflns_av_R_equivalents 0.1950 _diffrn_reflns_av_sigmaI/netI 0.2104 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5773 _reflns_number_gt 2724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0592P)^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 5773 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1757 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.46987(5) 0.01768(3) 0.11944(5) 0.0375(2) Uani 1 1 d . . . O1 O 0.5472(4) 0.1013(3) 0.0829(4) 0.0424(15) Uani 1 1 d . . . O2 O 0.3372(5) 0.0539(3) 0.0199(5) 0.0462(16) Uani 1 1 d . . . O3 O 0.2933(5) 0.1054(3) 0.1656(6) 0.0678(19) Uani 1 1 d . . . N1 N 0.5942(5) -0.0252(4) 0.2112(5) 0.0338(16) Uani 1 1 d . . . N2 N 0.4004(5) -0.0763(3) 0.1412(5) 0.0398(17) Uani 1 1 d . . . H2 H 0.3756 -0.0915 0.0674 0.048 Uiso 1 1 calc R . . C1 C 0.6202(6) 0.1279(5) 0.1625(7) 0.038(2) Uani 1 1 d . . . C2 C 0.6889(6) 0.0870(5) 0.2395(7) 0.037(2) Uani 1 1 d . . . C3 C 0.7677(7) 0.1221(5) 0.3135(8) 0.051(2) Uani 1 1 d . . . H3 H 0.8130 0.0953 0.3684 0.061 Uiso 1 1 calc R . . C4 C 0.7808(7) 0.1941(6) 0.3084(8) 0.057(3) Uani 1 1 d . . . H4 H 0.8352 0.2167 0.3585 0.068 Uiso 1 1 calc R . . C5 C 0.7151(7) 0.2332(5) 0.2310(8) 0.050(2) Uani 1 1 d . . . H5 H 0.7269 0.2827 0.2263 0.060 Uiso 1 1 calc R . . C6 C 0.6326(7) 0.2036(5) 0.1595(7) 0.041(2) Uani 1 1 d . . . C7 C 0.5617(7) 0.2445(4) 0.0767(7) 0.041(2) Uani 1 1 d . . . C8 C 0.5968(8) 0.2914(5) 0.0049(8) 0.056(3) Uani 1 1 d . . . H8 H 0.6688 0.2984 0.0105 0.067 Uiso 1 1 calc R . . C9 C 0.5290(9) 0.3286(5) -0.0757(9) 0.064(3) Uani 1 1 d . . . H9 H 0.5556 0.3607 -0.1243 0.076 Uiso 1 1 calc R . . C10 C 0.4249(10) 0.3206(5) -0.0874(8) 0.066(3) Uani 1 1 d . . . H10 H 0.3788 0.3460 -0.1435 0.079 Uiso 1 1 calc R . . C11 C 0.3893(8) 0.2740(5) -0.0140(8) 0.054(3) Uani 1 1 d . . . H11 H 0.3173 0.2678 -0.0191 0.065 Uiso 1 1 calc R . . C12 C 0.4560(7) 0.2362(5) 0.0663(8) 0.047(2) Uani 1 1 d . . . H12 H 0.4294 0.2042 0.1150 0.056 Uiso 1 1 calc R . . C13 C 0.6843(7) 0.0081(5) 0.2467(6) 0.041(2) Uani 1 1 d . . . C14 C 0.7707(7) -0.0316(5) 0.2915(7) 0.047(2) Uani 1 1 d . . . H14 H 0.8350 -0.0088 0.3162 0.057 Uiso 1 1 calc R . . C15 C 0.7629(8) -0.1032(5) 0.2999(8) 0.061(3) Uani 1 1 d . . . H15 H 0.8225 -0.1304 0.3281 0.073 Uiso 1 1 calc R . . C16 C 0.6697(7) -0.1367(5) 0.2681(7) 0.049(2) Uani 1 1 d . . . H16 H 0.6633 -0.1864 0.2775 0.058 Uiso 1 1 calc R . . C17 C 0.5873(6) -0.0966(5) 0.2230(6) 0.039(2) Uani 1 1 d . . . C18 C 0.4824(6) -0.1291(4) 0.1852(7) 0.044(2) Uani 1 1 d . . . H18A H 0.4865 -0.1643 0.1249 0.052 Uiso 1 1 calc R . . H18B H 0.4625 -0.1546 0.2501 0.052 Uiso 1 1 calc R . . C19 C 0.3106(6) -0.0792(4) 0.1954(7) 0.035(2) Uani 1 1 d . . . C20 C 0.3213(6) -0.0563(4) 0.3076(7) 0.042(2) Uani 1 1 d . . . C21 C 0.2345(7) -0.0621(5) 0.3597(8) 0.051(2) Uani 1 1 d . . . H21 H 0.2399 -0.0481 0.4368 0.061 Uiso 1 1 calc R . . C22 C 0.1420(7) -0.0876(5) 0.3023(9) 0.049(2) Uani 1 1 d . . . C23 C 0.1336(7) -0.1058(5) 0.1889(8) 0.051(2) Uani 1 1 d . . . H23 H 0.0689 -0.1205 0.1473 0.062 Uiso 1 1 calc R . . C24 C 0.2195(6) -0.1027(4) 0.1343(7) 0.037(2) Uani 1 1 d . . . C25 C 0.4186(7) -0.0269(5) 0.3776(7) 0.061(3) Uani 1 1 d . . . H25A H 0.4695 -0.0649 0.3952 0.091 Uiso 1 1 calc R . . H25B H 0.4035 -0.0070 0.4483 0.091 Uiso 1 1 calc R . . H25C H 0.4462 0.0105 0.3346 0.091 Uiso 1 1 calc R . . C26 C 0.0517(7) -0.0950(6) 0.3606(9) 0.081(4) Uani 1 1 d . . . H26A H 0.0606 -0.1372 0.4092 0.121 Uiso 1 1 calc R . . H26B H -0.0113 -0.0998 0.3037 0.121 Uiso 1 1 calc R . . H26C H 0.0467 -0.0529 0.4072 0.121 Uiso 1 1 calc R . . C27 C 0.2082(7) -0.1239(5) 0.0130(7) 0.059(3) Uani 1 1 d . . . H27A H 0.2308 -0.0850 -0.0307 0.088 Uiso 1 1 calc R . . H27B H 0.1359 -0.1348 -0.0171 0.088 Uiso 1 1 calc R . . H27C H 0.2504 -0.1660 0.0069 0.088 Uiso 1 1 calc R . . C28 C 0.2824(8) 0.0857(6) 0.0614(9) 0.054(3) Uani 1 1 d . . . C29 C 0.1787(8) 0.1073(6) -0.0126(9) 0.092(4) Uani 1 1 d . . . H29A H 0.1911 0.1273 -0.0845 0.138 Uiso 1 1 calc R . . H29B H 0.1449 0.1429 0.0277 0.138 Uiso 1 1 calc R . . H29C H 0.1343 0.0655 -0.0280 0.138 Uiso 1 1 calc R . . C30 C 0.1108(8) 0.1331(6) 0.2797(10) 0.087(4) Uani 1 1 d . . . H30 H 0.1747 0.1207 0.2502 0.104 Uiso 1 1 calc R . . Cl1 Cl 0.0108(3) 0.0803(2) 0.2115(3) 0.1160(12) Uani 1 1 d . . . Cl2 Cl 0.1319(4) 0.1180(3) 0.4222(3) 0.1551(17) Uani 1 1 d . . . Cl3 Cl 0.0795(4) 0.2210(2) 0.2456(5) 0.204(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0307(4) 0.0384(4) 0.0452(4) 0.0035(4) 0.0121(3) -0.0006(4) O1 0.047(4) 0.045(4) 0.034(3) 0.007(3) 0.006(3) -0.010(3) O2 0.034(4) 0.051(4) 0.053(4) 0.004(3) 0.007(3) -0.003(3) O3 0.056(5) 0.083(5) 0.066(5) 0.000(4) 0.018(4) 0.008(4) N1 0.024(4) 0.033(4) 0.048(4) 0.000(3) 0.014(3) -0.001(3) N2 0.032(4) 0.037(4) 0.053(5) 0.003(3) 0.012(3) 0.000(3) C1 0.029(5) 0.050(6) 0.039(5) 0.002(4) 0.016(4) -0.006(4) C2 0.026(5) 0.048(6) 0.043(5) -0.002(4) 0.020(4) 0.000(4) C3 0.039(6) 0.055(7) 0.060(6) 0.001(5) 0.016(5) -0.006(5) C4 0.045(7) 0.055(8) 0.073(7) -0.024(6) 0.014(5) -0.010(5) C5 0.053(7) 0.034(6) 0.071(7) -0.010(5) 0.029(6) -0.001(5) C6 0.039(6) 0.042(6) 0.048(6) -0.009(5) 0.023(5) -0.009(5) C7 0.053(7) 0.036(6) 0.039(6) -0.011(4) 0.019(5) -0.002(5) C8 0.062(7) 0.040(6) 0.072(7) -0.003(5) 0.028(6) -0.001(5) C9 0.085(9) 0.054(7) 0.062(7) 0.012(5) 0.041(7) -0.008(6) C10 0.092(10) 0.044(7) 0.061(7) 0.007(5) 0.013(7) 0.007(6) C11 0.054(7) 0.051(7) 0.063(7) -0.005(5) 0.022(5) 0.001(5) C12 0.051(7) 0.038(6) 0.053(6) -0.003(4) 0.017(5) 0.005(5) C13 0.035(5) 0.051(7) 0.039(5) 0.003(4) 0.016(4) 0.000(5) C14 0.032(5) 0.054(7) 0.057(6) 0.008(5) 0.009(4) 0.001(5) C15 0.049(7) 0.057(8) 0.076(7) 0.023(6) 0.009(5) 0.010(6) C16 0.035(6) 0.051(7) 0.061(6) 0.014(5) 0.013(5) -0.002(5) C17 0.030(5) 0.052(7) 0.037(5) 0.007(4) 0.014(4) 0.007(5) C18 0.033(6) 0.050(6) 0.050(6) 0.003(4) 0.015(4) 0.003(4) C19 0.031(5) 0.026(5) 0.052(6) 0.003(4) 0.016(4) 0.000(4) C20 0.035(6) 0.039(6) 0.054(6) 0.011(4) 0.017(5) 0.004(4) C21 0.046(7) 0.058(7) 0.050(6) 0.009(5) 0.017(5) 0.001(5) C22 0.034(6) 0.044(6) 0.073(7) 0.015(5) 0.023(5) 0.007(4) C23 0.035(6) 0.055(7) 0.064(7) 0.011(5) 0.007(5) 0.006(5) C24 0.026(5) 0.041(6) 0.045(6) 0.004(4) 0.007(4) -0.003(4) C25 0.064(7) 0.077(8) 0.039(6) -0.003(5) 0.005(5) -0.016(6) C26 0.051(7) 0.099(9) 0.105(9) 0.020(7) 0.044(6) 0.005(6) C27 0.046(6) 0.087(8) 0.045(6) -0.007(5) 0.011(5) -0.008(5) C28 0.046(7) 0.067(8) 0.042(7) 0.024(6) -0.011(5) -0.009(6) C29 0.072(9) 0.115(11) 0.086(9) -0.004(7) 0.006(7) 0.036(7) C30 0.057(8) 0.111(11) 0.101(10) -0.011(7) 0.038(7) 0.000(7) Cl1 0.065(2) 0.134(3) 0.148(3) 0.035(2) 0.016(2) 0.003(2) Cl2 0.165(4) 0.202(5) 0.112(3) -0.021(3) 0.062(3) -0.032(3) Cl3 0.232(6) 0.089(3) 0.334(7) 0.033(4) 0.163(6) 0.029(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 O1 1.972(5) . ? Pd1 N1 1.976(6) . ? Pd1 N2 2.033(6) . ? Pd1 O2 2.049(6) . ? Pd1 Pd1 3.177(2) 3_655 ? O1 C1 1.326(9) . ? O2 C28 1.124(11) . ? O3 C28 1.284(11) . ? N1 C13 1.345(10) . ? N1 C17 1.360(10) . ? N2 C19 1.455(9) . ? N2 C18 1.495(9) . ? N2 H2 0.9300 . ? C1 C2 1.402(11) . ? C1 C6 1.438(11) . ? C2 C3 1.403(11) . ? C2 C13 1.492(11) . ? C3 C4 1.372(11) . ? C3 H3 0.9500 . ? C4 C5 1.365(12) . ? C4 H4 0.9500 . ? C5 C6 1.377(11) . ? C5 H5 0.9500 . ? C6 C7 1.456(12) . ? C7 C8 1.372(11) . ? C7 C12 1.389(11) . ? C8 C9 1.383(13) . ? C8 H8 0.9500 . ? C9 C10 1.366(13) . ? C9 H9 0.9500 . ? C10 C11 1.385(12) . ? C10 H10 0.9500 . ? C11 C12 1.379(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(11) . ? C14 C15 1.359(11) . ? C14 H14 0.9500 . ? C15 C16 1.375(12) . ? C15 H15 0.9500 . ? C16 C17 1.355(11) . ? C16 H16 0.9500 . ? C17 C18 1.508(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.364(10) . ? C19 C20 1.394(11) . ? C20 C21 1.407(11) . ? C20 C25 1.508(11) . ? C21 C22 1.376(12) . ? C21 H21 0.9500 . ? C22 C23 1.385(11) . ? C22 C26 1.494(11) . ? C23 C24 1.410(11) . ? C23 H23 0.9500 . ? C24 C27 1.489(10) . ? 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 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.546(13) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Cl2 1.702(12) . ? C30 Cl1 1.736(11) . ? C30 Cl3 1.739(12) . ? C30 H30 1.0000 . ? 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 O1 Pd1 N1 92.2(3) . . ? O1 Pd1 N2 171.7(2) . . ? N1 Pd1 N2 85.5(3) . . ? O1 Pd1 O2 91.6(2) . . ? N1 Pd1 O2 175.3(3) . . ? N2 Pd1 O2 90.4(2) . . ? O1 Pd1 Pd1 75.09(15) . 3_655 ? N1 Pd1 Pd1 95.52(18) . 3_655 ? N2 Pd1 Pd1 97.20(18) . 3_655 ? O2 Pd1 Pd1 82.76(19) . 3_655 ? C1 O1 Pd1 118.8(5) . . ? C28 O2 Pd1 118.2(7) . . ? C13 N1 C17 120.1(7) . . ? C13 N1 Pd1 125.8(6) . . ? C17 N1 Pd1 113.5(5) . . ? C19 N2 C18 114.5(6) . . ? C19 N2 Pd1 121.0(5) . . ? C18 N2 Pd1 108.1(5) . . ? C19 N2 H2 103.7 . . ? C18 N2 H2 103.7 . . ? Pd1 N2 H2 103.7 . . ? O1 C1 C2 124.4(8) . . ? O1 C1 C6 115.4(7) . . ? C2 C1 C6 119.9(8) . . ? C1 C2 C3 118.3(8) . . ? C1 C2 C13 123.9(8) . . ? C3 C2 C13 117.8(8) . . ? C4 C3 C2 121.5(9) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.7(9) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 122.5(9) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 117.9(8) . . ? C5 C6 C7 123.2(9) . . ? C1 C6 C7 118.8(8) . . ? C8 C7 C12 117.8(9) . . ? C8 C7 C6 121.3(9) . . ? C12 C7 C6 120.9(8) . . ? C7 C8 C9 120.9(10) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 122.0(9) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 117.2(10) . . ? C9 C10 H10 121.4 . . ? C11 C10 H10 121.4 . . ? C12 C11 C10 121.6(10) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C7 120.6(9) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? N1 C13 C14 119.3(8) . . ? N1 C13 C2 119.4(7) . . ? C14 C13 C2 121.3(8) . . ? C15 C14 C13 119.7(9) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.8(9) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 118.0(9) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 N1 122.0(8) . . ? C16 C17 C18 121.5(8) . . ? N1 C17 C18 116.5(7) . . ? N2 C18 C17 113.8(7) . . ? N2 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N2 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C24 C19 C20 122.9(7) . . ? C24 C19 N2 119.1(7) . . ? C20 C19 N2 118.1(7) . . ? C19 C20 C21 117.1(8) . . ? C19 C20 C25 125.2(7) . . ? C21 C20 C25 117.7(8) . . ? C22 C21 C20 121.9(9) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 118.8(8) . . ? C21 C22 C26 120.7(9) . . ? C23 C22 C26 120.5(9) . . ? C22 C23 C24 121.1(8) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 118.1(8) . . ? C19 C24 C27 122.2(7) . . ? C23 C24 C27 119.7(8) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 O3 128.1(10) . . ? O2 C28 C29 117.5(10) . . ? O3 C28 C29 114.4(10) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Cl2 C30 Cl1 110.3(6) . . ? Cl2 C30 Cl3 112.6(7) . . ? Cl1 C30 Cl3 107.9(7) . . ? Cl2 C30 H30 108.6 . . ? Cl1 C30 H30 108.6 . . ? Cl3 C30 H30 108.6 . . ? 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 N1 Pd1 O1 C1 -38.3(6) . . . . ? O2 Pd1 O1 C1 144.5(6) . . . . ? Pd1 Pd1 O1 C1 -133.4(6) 3_655 . . . ? O1 Pd1 O2 C28 -93.9(8) . . . . ? N2 Pd1 O2 C28 94.1(8) . . . . ? Pd1 Pd1 O2 C28 -168.6(8) 3_655 . . . ? O1 Pd1 N1 C13 12.9(6) . . . . ? N2 Pd1 N1 C13 -175.0(6) . . . . ? Pd1 Pd1 N1 C13 88.2(6) 3_655 . . . ? O1 Pd1 N1 C17 -157.6(5) . . . . ? N2 Pd1 N1 C17 14.4(5) . . . . ? Pd1 Pd1 N1 C17 -82.4(5) 3_655 . . . ? N1 Pd1 N2 C19 121.0(6) . . . . ? O2 Pd1 N2 C19 -61.3(6) . . . . ? Pd1 Pd1 N2 C19 -144.0(6) 3_655 . . . ? N1 Pd1 N2 C18 -13.9(5) . . . . ? O2 Pd1 N2 C18 163.9(5) . . . . ? Pd1 Pd1 N2 C18 81.1(5) 3_655 . . . ? Pd1 O1 C1 C2 39.4(10) . . . . ? Pd1 O1 C1 C6 -146.3(5) . . . . ? O1 C1 C2 C3 175.0(7) . . . . ? C6 C1 C2 C3 1.0(11) . . . . ? O1 C1 C2 C13 -4.2(12) . . . . ? C6 C1 C2 C13 -178.2(7) . . . . ? C1 C2 C3 C4 -2.7(12) . . . . ? C13 C2 C3 C4 176.5(7) . . . . ? C2 C3 C4 C5 1.0(13) . . . . ? C3 C4 C5 C6 2.6(14) . . . . ? C4 C5 C6 C1 -4.2(12) . . . . ? C4 C5 C6 C7 179.8(8) . . . . ? O1 C1 C6 C5 -172.2(7) . . . . ? C2 C1 C6 C5 2.3(11) . . . . ? O1 C1 C6 C7 4.0(10) . . . . ? C2 C1 C6 C7 178.5(7) . . . . ? C5 C6 C7 C8 48.3(12) . . . . ? C1 C6 C7 C8 -127.7(9) . . . . ? C5 C6 C7 C12 -133.1(9) . . . . ? C1 C6 C7 C12 50.9(11) . . . . ? C12 C7 C8 C9 -0.5(13) . . . . ? C6 C7 C8 C9 178.2(8) . . . . ? C7 C8 C9 C10 0.1(15) . . . . ? C8 C9 C10 C11 0.7(15) . . . . ? C9 C10 C11 C12 -1.1(14) . . . . ? C10 C11 C12 C7 0.7(13) . . . . ? C8 C7 C12 C11 0.1(12) . . . . ? C6 C7 C12 C11 -178.5(8) . . . . ? C17 N1 C13 C14 2.3(11) . . . . ? Pd1 N1 C13 C14 -167.6(6) . . . . ? C17 N1 C13 C2 -176.4(6) . . . . ? Pd1 N1 C13 C2 13.6(9) . . . . ? C1 C2 C13 N1 -25.0(11) . . . . ? C3 C2 C13 N1 155.8(7) . . . . ? C1 C2 C13 C14 156.3(8) . . . . ? C3 C2 C13 C14 -22.9(11) . . . . ? N1 C13 C14 C15 -0.7(12) . . . . ? C2 C13 C14 C15 178.0(8) . . . . ? C13 C14 C15 C16 -2.2(13) . . . . ? C14 C15 C16 C17 3.2(13) . . . . ? C15 C16 C17 N1 -1.6(12) . . . . ? C15 C16 C17 C18 179.6(8) . . . . ? C13 N1 C17 C16 -1.2(11) . . . . ? Pd1 N1 C17 C16 169.9(6) . . . . ? C13 N1 C17 C18 177.6(7) . . . . ? Pd1 N1 C17 C18 -11.2(8) . . . . ? C19 N2 C18 C17 -126.5(7) . . . . ? Pd1 N2 C18 C17 11.6(8) . . . . ? C16 C17 C18 N2 178.1(7) . . . . ? N1 C17 C18 N2 -0.8(10) . . . . ? C18 N2 C19 C24 -110.9(8) . . . . ? Pd1 N2 C19 C24 116.9(7) . . . . ? C18 N2 C19 C20 70.5(9) . . . . ? Pd1 N2 C19 C20 -61.7(9) . . . . ? C24 C19 C20 C21 3.8(12) . . . . ? N2 C19 C20 C21 -177.6(7) . . . . ? C24 C19 C20 C25 -177.2(8) . . . . ? N2 C19 C20 C25 1.3(12) . . . . ? C19 C20 C21 C22 -1.7(13) . . . . ? C25 C20 C21 C22 179.3(8) . . . . ? C20 C21 C22 C23 -2.1(13) . . . . ? C20 C21 C22 C26 178.5(8) . . . . ? C21 C22 C23 C24 4.0(13) . . . . ? C26 C22 C23 C24 -176.6(8) . . . . ? C20 C19 C24 C23 -2.1(12) . . . . ? N2 C19 C24 C23 179.4(7) . . . . ? C20 C19 C24 C27 177.1(8) . . . . ? N2 C19 C24 C27 -1.4(12) . . . . ? C22 C23 C24 C19 -2.0(12) . . . . ? C22 C23 C24 C27 178.8(8) . . . . ? Pd1 O2 C28 O3 2.7(15) . . . . ? Pd1 O2 C28 C29 -175.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O1 0.93 2.23 2.929(8) 131.1 3_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.117 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.119