# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Stephen Foley' 'Jackson M Chitanda' 'Demyan E Prokopchuk' 'J.Wilson Quail' _publ_contact_author_name 'Stephen Foley' _publ_contact_author_email STEPHEN.FOLEY@USASK.CA _publ_section_title ; A facile route into the synthesis of palladacycles employing iminoisoindolines as monoanionic bidentate ligands ; # Attachment 'Crystal_structure_data.cif' data_1008 _database_code_depnum_ccdc_archive 'CCDC 687003' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 N4 O4 Pd2, C H2 Cl2' _chemical_formula_sum 'C45 H38 Cl2 N4 O4 Pd2' _chemical_formula_weight 982.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 12.5421(2) _cell_length_b 16.7665(3) _cell_length_c 18.9026(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.3617(13) _cell_angle_gamma 90.00 _cell_volume 3973.85(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9335 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description chip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'Shelxtl 6.10 (Bruker-AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57938 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8109 _reflns_number_gt 6475 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+4.6568P] 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 8109 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.22352(2) 0.417634(15) 0.314784(14) 0.02146(8) Uani 1 1 d . . . Pd2 Pd 0.17076(2) 0.565609(15) 0.232134(15) 0.02391(8) Uani 1 1 d . . . O1 O 0.36191(19) 0.49219(15) 0.33180(14) 0.0307(6) Uani 1 1 d . . . O2 O 0.2989(2) 0.60857(15) 0.28929(15) 0.0345(6) Uani 1 1 d . . . O3 O 0.1659(2) 0.48431(14) 0.39653(13) 0.0284(6) Uani 1 1 d . . . O4 O 0.0890(2) 0.58062(15) 0.33017(14) 0.0310(6) Uani 1 1 d . . . N1 N 0.1311(2) 0.28613(16) 0.19765(16) 0.0228(6) Uani 1 1 d . . . N2 N 0.2871(2) 0.35224(16) 0.23769(16) 0.0221(6) Uani 1 1 d . . . N3 N 0.1382(2) 0.46679(18) 0.08366(16) 0.0271(7) Uani 1 1 d . . . N4 N 0.0440(2) 0.52573(17) 0.17621(16) 0.0242(6) Uani 1 1 d . . . C1 C 0.2360(3) 0.30725(18) 0.19207(19) 0.0207(7) Uani 1 1 d . . . C2 C 0.2745(3) 0.2725(2) 0.12486(19) 0.0256(8) Uani 1 1 d . . . C3 C 0.3693(3) 0.2816(2) 0.0890(2) 0.0317(8) Uani 1 1 d . . . H3 H 0.4262 0.3125 0.1086 0.038 Uiso 1 1 calc R . . C4 C 0.3786(3) 0.2445(3) 0.0238(2) 0.0402(10) Uani 1 1 d . . . H4 H 0.4430 0.2500 -0.0012 0.048 Uiso 1 1 calc R . . C5 C 0.2963(4) 0.1995(3) -0.0057(2) 0.0436(11) Uani 1 1 d . . . H5 H 0.3049 0.1745 -0.0503 0.052 Uiso 1 1 calc R . . C6 C 0.2018(3) 0.1908(2) 0.0296(2) 0.0382(10) Uani 1 1 d . . . H6 H 0.1448 0.1603 0.0097 0.046 Uiso 1 1 calc R . . C7 C 0.1920(3) 0.2277(2) 0.0948(2) 0.0271(8) Uani 1 1 d . . . C8 C 0.0972(3) 0.2311(2) 0.1408(2) 0.0274(8) Uani 1 1 d . . . H8A H 0.0340 0.2519 0.1144 0.033 Uiso 1 1 calc R . . H8B H 0.0803 0.1777 0.1600 0.033 Uiso 1 1 calc R . . C9 C 0.0640(3) 0.30129(19) 0.25476(19) 0.0218(7) Uani 1 1 d . . . C10 C 0.0943(3) 0.3507(2) 0.31152(19) 0.0232(7) Uani 1 1 d . . . C11 C 0.0222(3) 0.3564(2) 0.3671(2) 0.0279(8) Uani 1 1 d . . . H11 H 0.0426 0.3866 0.4077 0.033 Uiso 1 1 calc R . . C12 C -0.0770(3) 0.3202(2) 0.3655(2) 0.0317(9) Uani 1 1 d . . . H12 H -0.1242 0.3269 0.4036 0.038 Uiso 1 1 calc R . . C13 C -0.1061(3) 0.2740(2) 0.3075(2) 0.0318(9) Uani 1 1 d . . . H13 H -0.1742 0.2491 0.3054 0.038 Uiso 1 1 calc R . . C14 C -0.0367(3) 0.2642(2) 0.2527(2) 0.0294(8) Uani 1 1 d . . . H14 H -0.0570 0.2320 0.2133 0.035 Uiso 1 1 calc R . . C15 C 0.4011(3) 0.3590(2) 0.23142(19) 0.0234(7) Uani 1 1 d . . . C16 C 0.4653(3) 0.2972(2) 0.2554(2) 0.0329(9) Uani 1 1 d . . . H16 H 0.4350 0.2513 0.2765 0.039 Uiso 1 1 calc R . . C17 C 0.5753(3) 0.3034(3) 0.2481(3) 0.0449(11) Uani 1 1 d . . . H17 H 0.6200 0.2603 0.2624 0.054 Uiso 1 1 calc R . . C18 C 0.6197(3) 0.3707(3) 0.2205(2) 0.0403(10) Uani 1 1 d . . . H18 H 0.6950 0.3749 0.2174 0.048 Uiso 1 1 calc R . . C19 C 0.5552(3) 0.4328(2) 0.1972(2) 0.0367(9) Uani 1 1 d . . . H19 H 0.5857 0.4791 0.1770 0.044 Uiso 1 1 calc R . . C20 C 0.4455(3) 0.4266(2) 0.2036(2) 0.0301(8) Uani 1 1 d . . . H20 H 0.4008 0.4695 0.1887 0.036 Uiso 1 1 calc R . . C21 C 0.0484(3) 0.4777(2) 0.12189(19) 0.0246(7) Uani 1 1 d . . . C22 C -0.0353(3) 0.42608(19) 0.0906(2) 0.0264(8) Uani 1 1 d . . . C23 C -0.1387(3) 0.4078(2) 0.1120(2) 0.0340(9) Uani 1 1 d . . . H23 H -0.1689 0.4334 0.1516 0.041 Uiso 1 1 calc R . . C24 C -0.1955(4) 0.3507(2) 0.0731(2) 0.0416(10) Uani 1 1 d . . . H24 H -0.2656 0.3369 0.0868 0.050 Uiso 1 1 calc R . . C25 C -0.1520(4) 0.3135(2) 0.0148(2) 0.0422(11) Uani 1 1 d . . . H25 H -0.1927 0.2749 -0.0108 0.051 Uiso 1 1 calc R . . C26 C -0.0508(4) 0.3319(2) -0.0063(2) 0.0378(10) Uani 1 1 d . . . H26 H -0.0215 0.3072 -0.0466 0.045 Uiso 1 1 calc R . . C27 C 0.0070(3) 0.3871(2) 0.0329(2) 0.0322(9) Uani 1 1 d . . . C28 C 0.1191(3) 0.4138(2) 0.0230(2) 0.0319(9) Uani 1 1 d . . . H28A H 0.1690 0.3681 0.0242 0.038 Uiso 1 1 calc R . . H28B H 0.1264 0.4428 -0.0222 0.038 Uiso 1 1 calc R . . C29 C 0.2318(3) 0.5147(2) 0.0872(2) 0.0278(8) Uani 1 1 d . . . C30 C 0.2528(3) 0.5652(2) 0.1448(2) 0.0282(8) Uani 1 1 d . . . C31 C 0.3425(3) 0.6148(2) 0.1411(2) 0.0360(9) Uani 1 1 d . . . H31 H 0.3565 0.6518 0.1782 0.043 Uiso 1 1 calc R . . C32 C 0.4118(3) 0.6114(3) 0.0847(3) 0.0455(11) Uani 1 1 d . . . H32 H 0.4724 0.6453 0.0837 0.055 Uiso 1 1 calc R . . C33 C 0.3914(3) 0.5585(3) 0.0304(3) 0.0443(11) Uani 1 1 d . . . H33 H 0.4384 0.5557 -0.0082 0.053 Uiso 1 1 calc R . . C34 C 0.3035(3) 0.5096(2) 0.0317(2) 0.0380(10) Uani 1 1 d . . . H34 H 0.2913 0.4721 -0.0053 0.046 Uiso 1 1 calc R . . C35 C -0.0584(3) 0.5463(2) 0.20401(19) 0.0243(7) Uani 1 1 d . . . C36 C -0.1135(3) 0.6104(2) 0.1738(2) 0.0311(8) Uani 1 1 d . . . H36 H -0.0843 0.6390 0.1354 0.037 Uiso 1 1 calc R . . C37 C -0.2118(3) 0.6320(3) 0.2005(3) 0.0426(11) Uani 1 1 d . . . H37 H -0.2505 0.6749 0.1794 0.051 Uiso 1 1 calc R . . C38 C -0.2538(3) 0.5918(3) 0.2572(3) 0.0468(12) Uani 1 1 d . . . H38 H -0.3212 0.6066 0.2750 0.056 Uiso 1 1 calc R . . C39 C -0.1967(3) 0.5299(3) 0.2877(2) 0.0426(10) Uani 1 1 d . . . H39 H -0.2247 0.5025 0.3272 0.051 Uiso 1 1 calc R . . C40 C -0.0989(3) 0.5071(2) 0.2615(2) 0.0336(9) Uani 1 1 d . . . H40 H -0.0600 0.4647 0.2832 0.040 Uiso 1 1 calc R . . C41 C 0.3641(3) 0.5664(2) 0.3245(2) 0.0286(8) Uani 1 1 d . . . C42 C 0.4537(3) 0.6116(3) 0.3613(3) 0.0456(11) Uani 1 1 d . . . H42A H 0.4522 0.6014 0.4124 0.055 Uiso 1 1 calc R . . H42B H 0.4449 0.6689 0.3525 0.055 Uiso 1 1 calc R . . H42C H 0.5222 0.5939 0.3430 0.055 Uiso 1 1 calc R . . C43 C 0.1135(3) 0.5483(2) 0.3880(2) 0.0260(8) Uani 1 1 d . . . C44 C 0.0769(4) 0.5871(3) 0.4545(2) 0.0471(12) Uani 1 1 d . . . H44A H 0.0882 0.6448 0.4515 0.057 Uiso 1 1 calc R . . H44B H 0.1177 0.5656 0.4950 0.057 Uiso 1 1 calc R . . H44C H 0.0009 0.5761 0.4604 0.057 Uiso 1 1 calc R . . C45 C 0.5752(4) 0.4162(3) 0.4188(3) 0.0610(15) Uani 1 1 d . . . H45A H 0.5007 0.4189 0.4347 0.073 Uiso 1 1 calc R . . H45B H 0.5751 0.4296 0.3678 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.62349(10) 0.31889(7) 0.43071(8) 0.0565(3) Uani 1 1 d . . . Cl2 Cl 0.65272(10) 0.48629(8) 0.46591(8) 0.0592(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 0.02219(14) 0.01871(13) 0.02341(15) -0.00147(10) -0.00112(10) 0.00041(10) Pd2 0.02696(15) 0.02053(14) 0.02412(15) -0.00076(10) -0.00190(11) 0.00133(10) O1 0.0265(13) 0.0264(13) 0.0389(16) -0.0058(11) -0.0028(11) -0.0028(10) O2 0.0366(15) 0.0256(13) 0.0409(17) 0.0014(12) -0.0105(13) -0.0039(11) O3 0.0346(14) 0.0242(13) 0.0265(14) -0.0016(10) -0.0010(11) 0.0023(11) O4 0.0370(15) 0.0322(14) 0.0237(14) -0.0034(11) -0.0002(11) 0.0081(11) N1 0.0217(14) 0.0202(14) 0.0263(16) -0.0022(12) -0.0001(12) -0.0039(11) N2 0.0182(14) 0.0169(14) 0.0311(17) -0.0007(12) 0.0004(12) 0.0010(11) N3 0.0322(16) 0.0268(16) 0.0221(16) -0.0041(12) -0.0004(13) 0.0054(13) N4 0.0264(15) 0.0228(15) 0.0235(16) 0.0010(12) 0.0002(12) 0.0038(12) C1 0.0211(16) 0.0152(15) 0.0260(19) 0.0029(13) 0.0012(14) 0.0013(12) C2 0.0329(19) 0.0188(17) 0.0249(19) 0.0042(14) -0.0005(15) 0.0009(14) C3 0.032(2) 0.030(2) 0.033(2) -0.0015(16) 0.0052(17) 0.0002(16) C4 0.039(2) 0.045(2) 0.037(2) -0.0071(19) 0.0082(19) 0.0038(18) C5 0.057(3) 0.047(3) 0.026(2) -0.0121(19) 0.004(2) 0.003(2) C6 0.044(2) 0.037(2) 0.033(2) -0.0087(18) -0.0015(19) -0.0053(18) C7 0.034(2) 0.0233(18) 0.0244(19) 0.0002(15) -0.0015(15) -0.0027(15) C8 0.0287(19) 0.0266(18) 0.027(2) -0.0039(15) -0.0036(15) -0.0034(14) C9 0.0247(17) 0.0172(16) 0.0234(18) 0.0045(13) 0.0003(14) 0.0000(13) C10 0.0245(17) 0.0200(17) 0.0250(19) 0.0062(14) -0.0002(14) 0.0020(13) C11 0.034(2) 0.0267(18) 0.0226(19) 0.0053(15) 0.0024(16) 0.0022(15) C12 0.031(2) 0.031(2) 0.034(2) 0.0094(16) 0.0089(17) -0.0011(15) C13 0.0223(18) 0.0287(19) 0.045(2) 0.0066(17) 0.0030(17) -0.0047(15) C14 0.0263(19) 0.0257(18) 0.036(2) 0.0003(16) -0.0010(16) -0.0028(14) C15 0.0213(17) 0.0219(17) 0.0272(19) -0.0030(14) 0.0018(14) -0.0010(13) C16 0.0280(19) 0.0215(18) 0.049(3) 0.0059(17) -0.0013(18) 0.0019(15) C17 0.028(2) 0.042(2) 0.064(3) 0.008(2) -0.006(2) 0.0088(18) C18 0.023(2) 0.043(2) 0.056(3) -0.003(2) 0.0045(19) -0.0035(17) C19 0.033(2) 0.031(2) 0.046(3) 0.0013(18) 0.0018(18) -0.0080(16) C20 0.0253(18) 0.0209(18) 0.044(2) 0.0010(16) -0.0007(17) 0.0011(14) C21 0.0318(19) 0.0214(17) 0.0205(18) 0.0008(14) -0.0035(15) 0.0054(14) C22 0.039(2) 0.0174(16) 0.0229(19) 0.0024(14) -0.0043(16) 0.0029(14) C23 0.038(2) 0.032(2) 0.032(2) -0.0022(17) -0.0029(17) -0.0029(17) C24 0.043(2) 0.035(2) 0.046(3) -0.0019(19) -0.008(2) -0.0022(18) C25 0.058(3) 0.030(2) 0.037(3) -0.0082(18) -0.017(2) -0.0001(19) C26 0.055(3) 0.029(2) 0.028(2) -0.0061(17) -0.0044(19) 0.0011(18) C27 0.047(2) 0.0225(18) 0.027(2) -0.0005(15) -0.0050(17) 0.0090(16) C28 0.045(2) 0.0272(19) 0.023(2) -0.0045(15) -0.0001(17) 0.0093(16) C29 0.0316(19) 0.0246(18) 0.027(2) 0.0040(15) 0.0044(16) 0.0052(15) C30 0.0309(19) 0.0187(17) 0.035(2) 0.0069(15) 0.0011(16) 0.0070(14) C31 0.038(2) 0.0225(19) 0.048(3) 0.0064(17) 0.0072(19) 0.0000(16) C32 0.039(2) 0.032(2) 0.066(3) 0.018(2) 0.018(2) -0.0005(18) C33 0.039(2) 0.044(2) 0.051(3) 0.014(2) 0.021(2) 0.0080(19) C34 0.041(2) 0.039(2) 0.034(2) 0.0008(18) 0.0103(19) 0.0126(18) C35 0.0250(18) 0.0233(17) 0.0245(19) -0.0068(14) -0.0018(15) 0.0002(14) C36 0.033(2) 0.0295(19) 0.031(2) -0.0047(16) -0.0021(16) 0.0034(16) C37 0.031(2) 0.035(2) 0.062(3) -0.015(2) -0.007(2) 0.0102(17) C38 0.027(2) 0.054(3) 0.061(3) -0.021(2) 0.008(2) -0.0049(19) C39 0.040(2) 0.050(3) 0.039(3) -0.006(2) 0.014(2) -0.011(2) C40 0.036(2) 0.034(2) 0.031(2) 0.0002(17) 0.0025(17) -0.0028(16) C41 0.0276(19) 0.0272(19) 0.031(2) -0.0047(15) 0.0033(16) -0.0060(15) C42 0.042(2) 0.038(2) 0.056(3) 0.003(2) -0.015(2) -0.0163(19) C43 0.0228(17) 0.0267(18) 0.029(2) -0.0047(15) 0.0006(15) -0.0020(14) C44 0.068(3) 0.044(3) 0.029(2) -0.0044(19) 0.007(2) 0.023(2) C45 0.057(3) 0.046(3) 0.078(4) -0.011(3) -0.018(3) 0.007(2) Cl1 0.0526(7) 0.0455(7) 0.0718(9) 0.0063(6) 0.0090(6) 0.0055(5) Cl2 0.0577(7) 0.0568(7) 0.0630(9) -0.0094(6) -0.0037(6) -0.0099(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 C10 1.972(3) . ? Pd1 N2 2.004(3) . ? Pd1 O3 2.053(3) . ? Pd1 O1 2.157(2) . ? Pd1 Pd2 2.9975(4) . ? Pd2 C30 1.965(4) . ? Pd2 N4 2.003(3) . ? Pd2 O2 2.046(3) . ? Pd2 O4 2.154(3) . ? O1 C41 1.253(4) . ? O2 C41 1.259(5) . ? O3 C43 1.267(4) . ? O4 C43 1.251(4) . ? N1 C1 1.368(4) . ? N1 C9 1.408(4) . ? N1 C8 1.472(4) . ? N2 C1 1.303(4) . ? N2 C15 1.441(4) . ? N3 C21 1.365(5) . ? N3 C29 1.422(5) . ? N3 C28 1.465(5) . ? N4 C21 1.307(5) . ? N4 C35 1.441(4) . ? C1 C2 1.489(5) . ? C2 C7 1.389(5) . ? C2 C3 1.391(5) . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C5 C6 1.382(6) . ? C5 H5 0.9500 . ? C6 C7 1.387(5) . ? C6 H6 0.9500 . ? C7 C8 1.490(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.400(5) . ? C9 C14 1.408(5) . ? C10 C11 1.405(5) . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C13 1.385(6) . ? C12 H12 0.9500 . ? C13 C14 1.378(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.373(5) . ? C15 C16 1.383(5) . ? C16 C17 1.393(6) . ? C16 H16 0.9500 . ? C17 C18 1.366(6) . ? C17 H17 0.9500 . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 C20 1.388(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.474(5) . ? C22 C27 1.388(5) . ? C22 C23 1.401(5) . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C24 C25 1.389(6) . ? C24 H24 0.9500 . ? C25 C26 1.373(6) . ? C25 H25 0.9500 . ? C26 C27 1.381(5) . ? C26 H26 0.9500 . ? C27 C28 1.492(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.400(5) . ? C29 C30 1.401(5) . ? C30 C31 1.401(5) . ? C31 C32 1.392(6) . ? C31 H31 0.9500 . ? C32 C33 1.375(7) . ? C32 H32 0.9500 . ? C33 C34 1.375(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.378(5) . ? C35 C36 1.393(5) . ? C36 C37 1.392(5) . ? C36 H36 0.9500 . ? C37 C38 1.382(7) . ? C37 H37 0.9500 . ? C38 C39 1.380(7) . ? C38 H38 0.9500 . ? C39 C40 1.388(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.511(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.496(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 Cl1 1.753(5) . ? C45 Cl2 1.755(5) . ? C45 H45A 0.9900 . ? C45 H45B 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 C10 Pd1 N2 90.40(13) . . ? C10 Pd1 O3 91.70(13) . . ? N2 Pd1 O3 177.01(10) . . ? C10 Pd1 O1 173.12(13) . . ? N2 Pd1 O1 95.31(10) . . ? O3 Pd1 O1 82.46(10) . . ? C10 Pd1 Pd2 106.49(9) . . ? N2 Pd1 Pd2 99.24(8) . . ? O3 Pd1 Pd2 82.20(7) . . ? O1 Pd1 Pd2 76.40(7) . . ? C30 Pd2 N4 88.89(14) . . ? C30 Pd2 O2 91.38(14) . . ? N4 Pd2 O2 178.86(11) . . ? C30 Pd2 O4 172.86(13) . . ? N4 Pd2 O4 96.03(11) . . ? O2 Pd2 O4 83.61(11) . . ? C30 Pd2 Pd1 108.73(9) . . ? N4 Pd2 Pd1 99.29(8) . . ? O2 Pd2 Pd1 81.68(7) . . ? O4 Pd2 Pd1 75.64(7) . . ? C41 O1 Pd1 125.4(2) . . ? C41 O2 Pd2 125.0(2) . . ? C43 O3 Pd1 123.8(2) . . ? C43 O4 Pd2 126.1(2) . . ? C1 N1 C9 127.3(3) . . ? C1 N1 C8 111.6(3) . . ? C9 N1 C8 120.4(3) . . ? C1 N2 C15 117.7(3) . . ? C1 N2 Pd1 126.8(2) . . ? C15 N2 Pd1 115.4(2) . . ? C21 N3 C29 126.1(3) . . ? C21 N3 C28 111.9(3) . . ? C29 N3 C28 119.9(3) . . ? C21 N4 C35 119.3(3) . . ? C21 N4 Pd2 124.9(2) . . ? C35 N4 Pd2 115.5(2) . . ? N2 C1 N1 123.9(3) . . ? N2 C1 C2 128.8(3) . . ? N1 C1 C2 107.2(3) . . ? C7 C2 C3 119.9(4) . . ? C7 C2 C1 107.8(3) . . ? C3 C2 C1 132.2(3) . . ? C4 C3 C2 118.3(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 121.6(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 118.6(4) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C6 C7 C2 121.5(4) . . ? C6 C7 C8 128.6(3) . . ? C2 C7 C8 109.8(3) . . ? N1 C8 C7 103.2(3) . . ? N1 C8 H8A 111.1 . . ? C7 C8 H8A 111.1 . . ? N1 C8 H8B 111.1 . . ? C7 C8 H8B 111.1 . . ? H8A C8 H8B 109.1 . . ? C10 C9 N1 122.6(3) . . ? C10 C9 C14 120.6(3) . . ? N1 C9 C14 116.9(3) . . ? C9 C10 C11 116.5(3) . . ? C9 C10 Pd1 124.6(3) . . ? C11 C10 Pd1 118.7(3) . . ? C12 C11 C10 123.2(4) . . ? C12 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C11 C12 C13 118.9(4) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.6(4) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? C20 C15 C16 120.3(3) . . ? C20 C15 N2 120.6(3) . . ? C16 C15 N2 119.0(3) . . ? C15 C16 C17 118.8(4) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 120.8(4) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C15 C20 C19 120.5(3) . . ? C15 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N4 C21 N3 123.4(3) . . ? N4 C21 C22 129.3(3) . . ? N3 C21 C22 107.3(3) . . ? C27 C22 C23 119.8(3) . . ? C27 C22 C21 108.1(3) . . ? C23 C22 C21 131.9(3) . . ? C24 C23 C22 117.7(4) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? C25 C24 C23 121.4(4) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 120.9(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 118.1(4) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C26 C27 C22 122.1(4) . . ? C26 C27 C28 128.3(4) . . ? C22 C27 C28 109.6(3) . . ? N3 C28 C27 102.8(3) . . ? N3 C28 H28A 111.2 . . ? C27 C28 H28A 111.2 . . ? N3 C28 H28B 111.2 . . ? C27 C28 H28B 111.2 . . ? H28A C28 H28B 109.1 . . ? C34 C29 C30 120.5(4) . . ? C34 C29 N3 118.4(3) . . ? C30 C29 N3 121.2(3) . . ? C29 C30 C31 117.1(4) . . ? C29 C30 Pd2 124.3(3) . . ? C31 C30 Pd2 118.5(3) . . ? C32 C31 C30 122.1(4) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C33 C32 C31 119.3(4) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C29 120.4(4) . . ? C33 C34 H34 119.8 . . ? C29 C34 H34 119.8 . . ? C40 C35 C36 120.2(3) . . ? C40 C35 N4 121.5(3) . . ? C36 C35 N4 118.2(3) . . ? C37 C36 C35 119.2(4) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C38 C37 C36 120.8(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C39 C38 C37 119.2(4) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 120.8(4) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C35 C40 C39 119.8(4) . . ? C35 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? O1 C41 O2 126.8(3) . . ? O1 C41 C42 117.8(3) . . ? O2 C41 C42 115.4(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 O3 126.4(3) . . ? O4 C43 C44 118.1(3) . . ? O3 C43 C44 115.4(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Cl1 C45 Cl2 111.8(3) . . ? Cl1 C45 H45A 109.2 . . ? Cl2 C45 H45A 109.2 . . ? Cl1 C45 H45B 109.2 . . ? Cl2 C45 H45B 109.2 . . ? H45A C45 H45B 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 C10 Pd1 Pd2 C30 -111.11(16) . . . . ? N2 Pd1 Pd2 C30 -17.93(14) . . . . ? O3 Pd1 Pd2 C30 159.42(14) . . . . ? O1 Pd1 Pd2 C30 75.34(14) . . . . ? C10 Pd1 Pd2 N4 -19.12(14) . . . . ? N2 Pd1 Pd2 N4 74.06(12) . . . . ? O3 Pd1 Pd2 N4 -108.59(11) . . . . ? O1 Pd1 Pd2 N4 167.33(11) . . . . ? C10 Pd1 Pd2 O2 160.26(14) . . . . ? N2 Pd1 Pd2 O2 -106.56(11) . . . . ? O3 Pd1 Pd2 O2 70.79(11) . . . . ? O1 Pd1 Pd2 O2 -13.28(11) . . . . ? C10 Pd1 Pd2 O4 74.77(13) . . . . ? N2 Pd1 Pd2 O4 167.95(11) . . . . ? O3 Pd1 Pd2 O4 -14.69(10) . . . . ? O1 Pd1 Pd2 O4 -98.77(10) . . . . ? N2 Pd1 O1 C41 119.5(3) . . . . ? O3 Pd1 O1 C41 -62.5(3) . . . . ? Pd2 Pd1 O1 C41 21.3(3) . . . . ? C30 Pd2 O2 C41 -95.8(3) . . . . ? O4 Pd2 O2 C41 89.3(3) . . . . ? Pd1 Pd2 O2 C41 13.0(3) . . . . ? C10 Pd1 O3 C43 -92.6(3) . . . . ? O1 Pd1 O3 C43 91.0(3) . . . . ? Pd2 Pd1 O3 C43 13.8(3) . . . . ? N4 Pd2 O4 C43 122.3(3) . . . . ? O2 Pd2 O4 C43 -58.8(3) . . . . ? Pd1 Pd2 O4 C43 24.2(3) . . . . ? C10 Pd1 N2 C1 21.2(3) . . . . ? O1 Pd1 N2 C1 -162.6(3) . . . . ? Pd2 Pd1 N2 C1 -85.6(3) . . . . ? C10 Pd1 N2 C15 -161.3(2) . . . . ? O1 Pd1 N2 C15 14.9(2) . . . . ? Pd2 Pd1 N2 C15 91.9(2) . . . . ? C30 Pd2 N4 C21 33.5(3) . . . . ? O4 Pd2 N4 C21 -151.7(3) . . . . ? Pd1 Pd2 N4 C21 -75.3(3) . . . . ? C30 Pd2 N4 C35 -153.1(2) . . . . ? O4 Pd2 N4 C35 21.8(2) . . . . ? Pd1 Pd2 N4 C35 98.1(2) . . . . ? C15 N2 C1 N1 170.2(3) . . . . ? Pd1 N2 C1 N1 -12.4(5) . . . . ? C15 N2 C1 C2 -12.6(5) . . . . ? Pd1 N2 C1 C2 164.8(3) . . . . ? C9 N1 C1 N2 -6.8(5) . . . . ? C8 N1 C1 N2 -176.5(3) . . . . ? C9 N1 C1 C2 175.5(3) . . . . ? C8 N1 C1 C2 5.8(4) . . . . ? N2 C1 C2 C7 179.1(3) . . . . ? N1 C1 C2 C7 -3.4(4) . . . . ? N2 C1 C2 C3 -5.5(6) . . . . ? N1 C1 C2 C3 172.1(4) . . . . ? C7 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C4 -175.7(4) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C4 C5 C6 C7 -0.3(6) . . . . ? C5 C6 C7 C2 -0.1(6) . . . . ? C5 C6 C7 C8 176.3(4) . . . . ? C3 C2 C7 C6 0.6(5) . . . . ? C1 C2 C7 C6 176.8(3) . . . . ? C3 C2 C7 C8 -176.4(3) . . . . ? C1 C2 C7 C8 -0.2(4) . . . . ? C1 N1 C8 C7 -5.8(4) . . . . ? C9 N1 C8 C7 -176.3(3) . . . . ? C6 C7 C8 N1 -173.3(4) . . . . ? C2 C7 C8 N1 3.5(4) . . . . ? C1 N1 C9 C10 8.5(5) . . . . ? C8 N1 C9 C10 177.4(3) . . . . ? C1 N1 C9 C14 -171.4(3) . . . . ? C8 N1 C9 C14 -2.5(5) . . . . ? N1 C9 C10 C11 -176.0(3) . . . . ? C14 C9 C10 C11 4.0(5) . . . . ? N1 C9 C10 Pd1 8.9(5) . . . . ? C14 C9 C10 Pd1 -171.1(3) . . . . ? N2 Pd1 C10 C9 -18.8(3) . . . . ? O3 Pd1 C10 C9 163.3(3) . . . . ? Pd2 Pd1 C10 C9 81.0(3) . . . . ? N2 Pd1 C10 C11 166.2(3) . . . . ? O3 Pd1 C10 C11 -11.7(3) . . . . ? Pd2 Pd1 C10 C11 -94.0(3) . . . . ? C9 C10 C11 C12 -4.2(5) . . . . ? Pd1 C10 C11 C12 171.3(3) . . . . ? C10 C11 C12 C13 2.0(5) . . . . ? C11 C12 C13 C14 0.5(6) . . . . ? C12 C13 C14 C9 -0.6(6) . . . . ? C10 C9 C14 C13 -1.8(5) . . . . ? N1 C9 C14 C13 178.2(3) . . . . ? C1 N2 C15 C20 104.1(4) . . . . ? Pd1 N2 C15 C20 -73.6(4) . . . . ? C1 N2 C15 C16 -77.4(4) . . . . ? Pd1 N2 C15 C16 104.9(3) . . . . ? C20 C15 C16 C17 -2.7(6) . . . . ? N2 C15 C16 C17 178.9(4) . . . . ? C15 C16 C17 C18 2.8(7) . . . . ? C16 C17 C18 C19 -2.3(7) . . . . ? C17 C18 C19 C20 1.5(7) . . . . ? C16 C15 C20 C19 2.0(6) . . . . ? N2 C15 C20 C19 -179.5(4) . . . . ? C18 C19 C20 C15 -1.4(6) . . . . ? C35 N4 C21 N3 167.1(3) . . . . ? Pd2 N4 C21 N3 -19.7(5) . . . . ? C35 N4 C21 C22 -13.8(5) . . . . ? Pd2 N4 C21 C22 159.5(3) . . . . ? C29 N3 C21 N4 -12.7(5) . . . . ? C28 N3 C21 N4 -176.3(3) . . . . ? C29 N3 C21 C22 168.0(3) . . . . ? C28 N3 C21 C22 4.3(4) . . . . ? N4 C21 C22 C27 179.2(4) . . . . ? N3 C21 C22 C27 -1.6(4) . . . . ? N4 C21 C22 C23 -6.1(6) . . . . ? N3 C21 C22 C23 173.1(4) . . . . ? C27 C22 C23 C24 -0.6(5) . . . . ? C21 C22 C23 C24 -174.8(4) . . . . ? C22 C23 C24 C25 -0.5(6) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C24 C25 C26 C27 1.2(6) . . . . ? C25 C26 C27 C22 -2.3(6) . . . . ? C25 C26 C27 C28 176.7(4) . . . . ? C23 C22 C27 C26 2.0(6) . . . . ? C21 C22 C27 C26 177.5(3) . . . . ? C23 C22 C27 C28 -177.2(3) . . . . ? C21 C22 C27 C28 -1.7(4) . . . . ? C21 N3 C28 C27 -5.2(4) . . . . ? C29 N3 C28 C27 -170.0(3) . . . . ? C26 C27 C28 N3 -175.1(4) . . . . ? C22 C27 C28 N3 4.0(4) . . . . ? C21 N3 C29 C34 -162.4(3) . . . . ? C28 N3 C29 C34 0.1(5) . . . . ? C21 N3 C29 C30 18.3(5) . . . . ? C28 N3 C29 C30 -179.3(3) . . . . ? C34 C29 C30 C31 5.6(5) . . . . ? N3 C29 C30 C31 -175.1(3) . . . . ? C34 C29 C30 Pd2 -170.2(3) . . . . ? N3 C29 C30 Pd2 9.1(5) . . . . ? N4 Pd2 C30 C29 -27.3(3) . . . . ? O2 Pd2 C30 C29 153.8(3) . . . . ? Pd1 Pd2 C30 C29 72.1(3) . . . . ? N4 Pd2 C30 C31 156.9(3) . . . . ? O2 Pd2 C30 C31 -22.0(3) . . . . ? Pd1 Pd2 C30 C31 -103.7(3) . . . . ? C29 C30 C31 C32 -3.6(5) . . . . ? Pd2 C30 C31 C32 172.5(3) . . . . ? C30 C31 C32 C33 0.7(6) . . . . ? C31 C32 C33 C34 0.2(6) . . . . ? C32 C33 C34 C29 1.9(6) . . . . ? C30 C29 C34 C33 -5.0(6) . . . . ? N3 C29 C34 C33 175.7(4) . . . . ? C21 N4 C35 C40 97.3(4) . . . . ? Pd2 N4 C35 C40 -76.6(4) . . . . ? C21 N4 C35 C36 -86.4(4) . . . . ? Pd2 N4 C35 C36 99.8(3) . . . . ? C40 C35 C36 C37 -2.7(5) . . . . ? N4 C35 C36 C37 -179.1(3) . . . . ? C35 C36 C37 C38 1.3(6) . . . . ? C36 C37 C38 C39 0.4(6) . . . . ? C37 C38 C39 C40 -0.9(6) . . . . ? C36 C35 C40 C39 2.3(6) . . . . ? N4 C35 C40 C39 178.6(3) . . . . ? C38 C39 C40 C35 -0.5(6) . . . . ? Pd1 O1 C41 O2 -20.4(6) . . . . ? Pd1 O1 C41 C42 159.7(3) . . . . ? Pd2 O2 C41 O1 -1.0(6) . . . . ? Pd2 O2 C41 C42 178.9(3) . . . . ? Pd2 O4 C43 O3 -23.7(5) . . . . ? Pd2 O4 C43 C44 157.2(3) . . . . ? Pd1 O3 C43 O4 -0.1(5) . . . . ? Pd1 O3 C43 C44 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.533 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.103 #===END data_1066 _database_code_depnum_ccdc_archive 'CCDC 687004' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 N4 O8 Pd2, C H2 Cl2' _chemical_formula_sum 'C53 H46 Cl2 N4 O8 Pd2' _chemical_formula_weight 1150.64 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6888(8) _cell_length_b 13.9845(11) _cell_length_c 21.6903(11) _cell_angle_alpha 90.00 _cell_angle_beta 124.159(3) _cell_angle_gamma 90.00 _cell_volume 4690.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19844 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'Shelxtl 6.10 (Bruker-AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 55029 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8577 _reflns_number_gt 6852 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+19.8645P] 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 8577 _refine_ls_number_parameters 628 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.051 _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 -0.04211(3) 0.17795(3) 0.04062(2) 0.02391(11) Uani 1 1 d . . . Pd2 Pd -0.00082(3) 0.29628(3) 0.17034(2) 0.02287(11) Uani 1 1 d . . . O1 O -0.1383(2) 0.2887(3) -0.0077(2) 0.0298(8) Uani 1 1 d . . . O2 O -0.1236(2) 0.3467(3) 0.0957(2) 0.0282(8) Uani 1 1 d . . . O3 O 0.0321(2) 0.2813(3) 0.0340(2) 0.0313(9) Uani 1 1 d . . . O4 O 0.0373(2) 0.3885(3) 0.1138(2) 0.0301(8) Uani 1 1 d . . . O21 O -0.5137(3) 0.2305(5) -0.1338(3) 0.0736(17) Uani 1 1 d . . . O23 O 0.2970(3) 0.1900(4) 0.1573(3) 0.0458(11) Uani 1 1 d . . . O51 O 0.4428(6) 0.5397(7) 0.4029(5) 0.166(4) Uani 1 1 d DU . . O53 O -0.2791(3) 0.2699(4) 0.1959(3) 0.0542(13) Uani 1 1 d . . . N1 N -0.0306(3) -0.0539(3) 0.0847(2) 0.0284(10) Uani 1 1 d . . . N2 N -0.1243(3) 0.0779(3) 0.0321(2) 0.0265(10) Uani 1 1 d . . . N31 N 0.0851(3) 0.1084(3) 0.2753(2) 0.0271(10) Uani 1 1 d . . . N32 N 0.1213(3) 0.2549(3) 0.2466(2) 0.0244(9) Uani 1 1 d . . . C1 C -0.1106(3) -0.0127(4) 0.0484(3) 0.0261(11) Uani 1 1 d . . . C2 C -0.1743(4) -0.0899(4) 0.0316(3) 0.0298(12) Uani 1 1 d . . . C3 C -0.2645(4) -0.0906(5) -0.0053(3) 0.0364(13) Uani 1 1 d . . . H3 H -0.2973 -0.0336 -0.0257 0.044 Uiso 1 1 calc R . . C4 C -0.3043(4) -0.1764(5) -0.0110(3) 0.0463(16) Uani 1 1 d . . . H4 H -0.3653 -0.1783 -0.0355 0.056 Uiso 1 1 calc R . . C5 C -0.2568(5) -0.2602(5) 0.0185(3) 0.0476(17) Uani 1 1 d . . . H5 H -0.2859 -0.3181 0.0143 0.057 Uiso 1 1 calc R . . C6 C -0.1684(5) -0.2606(4) 0.0537(3) 0.0406(15) Uani 1 1 d . . . H6 H -0.1362 -0.3182 0.0731 0.049 Uiso 1 1 calc R . . C7 C -0.1278(4) -0.1752(4) 0.0602(3) 0.0316(12) Uani 1 1 d . . . C8 C -0.0338(4) -0.1576(4) 0.0954(3) 0.0327(13) Uani 1 1 d . . . H8A H 0.0005 -0.1745 0.1490 0.039 Uiso 1 1 calc R . . H8B H -0.0121 -0.1946 0.0702 0.039 Uiso 1 1 calc R . . C9 C 0.0487(4) -0.0097(4) 0.1077(3) 0.0267(11) Uani 1 1 d . . . C10 C 0.0535(3) 0.0844(4) 0.0868(3) 0.0276(11) Uani 1 1 d . . . C11 C 0.1352(4) 0.1158(4) 0.1079(3) 0.0296(12) Uani 1 1 d . . . H11 H 0.1395 0.1767 0.0909 0.036 Uiso 1 1 calc R . . C12 C 0.2108(4) 0.0628(4) 0.1526(3) 0.0342(13) Uani 1 1 d . . . C13 C 0.2044(4) -0.0275(4) 0.1763(3) 0.0335(13) Uani 1 1 d . . . H13 H 0.2550 -0.0640 0.2086 0.040 Uiso 1 1 calc R . . C14 C 0.1246(4) -0.0635(4) 0.1526(3) 0.0334(13) Uani 1 1 d . . . H14 H 0.1205 -0.1264 0.1669 0.040 Uiso 1 1 calc R . . C15 C -0.2085(3) 0.1137(4) 0.0070(3) 0.0261(11) Uani 1 1 d . . . C16 C -0.2674(4) 0.1405(4) -0.0673(3) 0.0314(12) Uani 1 1 d . . . H16 H -0.2514 0.1370 -0.1018 0.038 Uiso 1 1 calc R . . C17 C -0.3484(4) 0.1720(4) -0.0901(3) 0.0359(13) Uani 1 1 d . . . H17 H -0.3887 0.1892 -0.1407 0.043 Uiso 1 1 calc R . . C18 C -0.3721(4) 0.1791(4) -0.0395(4) 0.0360(13) Uani 1 1 d . . . C19 C -0.3122(4) 0.1558(4) 0.0348(3) 0.0374(14) Uani 1 1 d . . . H19 H -0.3273 0.1622 0.0697 0.045 Uiso 1 1 calc R . . C20 C -0.2309(4) 0.1233(4) 0.0581(3) 0.0324(13) Uani 1 1 d . . . H20 H -0.1903 0.1075 0.1090 0.039 Uiso 1 1 calc R . . C21 C -0.4625(4) 0.2122(5) -0.0685(5) 0.0507(17) Uani 1 1 d . . . C22 C -0.4871(6) 0.2214(7) -0.0133(6) 0.080(3) Uani 1 1 d . . . H22A H -0.5413 0.2573 -0.0360 0.119 Uiso 1 1 calc R . . H22B H -0.4413 0.2553 0.0312 0.119 Uiso 1 1 calc R . . H22C H -0.4948 0.1576 0.0009 0.119 Uiso 1 1 calc R . . C23 C 0.2947(4) 0.1073(5) 0.1744(3) 0.0373(14) Uani 1 1 d . . . C24 C 0.3758(4) 0.0484(6) 0.2166(4) 0.0521(18) Uani 1 1 d . . . H24A H 0.4263 0.0907 0.2401 0.078 Uiso 1 1 calc R . . H24B H 0.3778 0.0048 0.1822 0.078 Uiso 1 1 calc R . . H24C H 0.3762 0.0112 0.2551 0.078 Uiso 1 1 calc R . . C31 C 0.1438(3) 0.1707(4) 0.2782(3) 0.0238(11) Uani 1 1 d . . . C32 C 0.2290(4) 0.1231(4) 0.3199(3) 0.0295(12) Uani 1 1 d . . . C33 C 0.3109(4) 0.1514(4) 0.3395(3) 0.0357(13) Uani 1 1 d . . . H33 H 0.3203 0.2134 0.3274 0.043 Uiso 1 1 calc R . . C34 C 0.3781(4) 0.0861(5) 0.3770(4) 0.0429(15) Uani 1 1 d . . . H34 H 0.4343 0.1041 0.3908 0.051 Uiso 1 1 calc R . . C35 C 0.3652(4) -0.0052(5) 0.3950(4) 0.0491(17) Uani 1 1 d . . . H35 H 0.4123 -0.0486 0.4203 0.059 Uiso 1 1 calc R . . C36 C 0.2850(4) -0.0328(4) 0.3763(3) 0.0391(14) Uani 1 1 d . . . H36 H 0.2761 -0.0944 0.3893 0.047 Uiso 1 1 calc R . . C37 C 0.2174(4) 0.0313(4) 0.3381(3) 0.0319(12) Uani 1 1 d . . . C38 C 0.1259(4) 0.0172(4) 0.3126(3) 0.0328(13) Uani 1 1 d . . . H38A H 0.0995 -0.0372 0.2774 0.039 Uiso 1 1 calc R . . H38B H 0.1212 0.0058 0.3552 0.039 Uiso 1 1 calc R . . C39 C 0.0033(3) 0.1336(4) 0.2602(3) 0.0275(11) Uani 1 1 d . . . C40 C -0.0400(3) 0.2173(4) 0.2212(3) 0.0252(11) Uani 1 1 d . . . C41 C -0.1157(3) 0.2404(4) 0.2166(3) 0.0254(11) Uani 1 1 d . . . H41 H -0.1462 0.2969 0.1909 0.030 Uiso 1 1 calc R . . C42 C -0.1484(3) 0.1830(4) 0.2486(3) 0.0282(12) Uani 1 1 d . . . C43 C -0.1068(4) 0.0983(4) 0.2830(3) 0.0334(13) Uani 1 1 d . . . H43 H -0.1292 0.0578 0.3035 0.040 Uiso 1 1 calc R . . C44 C -0.0324(4) 0.0726(4) 0.2875(3) 0.0345(13) Uani 1 1 d . . . H44 H -0.0053 0.0132 0.3093 0.041 Uiso 1 1 calc R . . C45 C 0.1893(3) 0.3213(4) 0.2651(3) 0.0261(11) Uani 1 1 d . . . C46 C 0.2206(4) 0.3792(4) 0.3270(3) 0.0356(13) Uani 1 1 d . . . H46 H 0.1942 0.3784 0.3538 0.043 Uiso 1 1 calc R . . C47 C 0.2905(4) 0.4384(5) 0.3496(4) 0.0462(16) Uani 1 1 d . . . H47 H 0.3131 0.4768 0.3928 0.055 Uiso 1 1 calc R . . C48 C 0.3277(3) 0.4421(4) 0.3099(4) 0.0446(16) Uani 1 1 d D . . C49 C 0.2935(4) 0.3882(5) 0.2464(4) 0.0412(15) Uani 1 1 d . . . H49 H 0.3178 0.3924 0.2181 0.049 Uiso 1 1 calc R . . C50 C 0.2239(4) 0.3277(4) 0.2230(3) 0.0336(13) Uani 1 1 d . . . H50 H 0.2002 0.2911 0.1787 0.040 Uiso 1 1 calc R . . C51 C 0.4085(3) 0.5007(4) 0.3426(4) 0.095(3) Uani 1 1 d D . . C52 C 0.4448(6) 0.5083(7) 0.2962(5) 0.081(3) Uani 1 1 d DU . . H52A H 0.4896 0.5578 0.3170 0.122 Uiso 1 1 calc R . . H52B H 0.3985 0.5253 0.2450 0.122 Uiso 1 1 calc R . . H52C H 0.4700 0.4468 0.2964 0.122 Uiso 1 1 calc R . . C53 C -0.2285(4) 0.2138(4) 0.2435(3) 0.0333(13) Uani 1 1 d . . . C54 C -0.2430(4) 0.1755(5) 0.3001(4) 0.0413(15) Uani 1 1 d . . . H54A H -0.2955 0.2040 0.2922 0.062 Uiso 1 1 calc R . . H54B H -0.1933 0.1915 0.3503 0.062 Uiso 1 1 calc R . . H54C H -0.2497 0.1059 0.2951 0.062 Uiso 1 1 calc R . . C55 C -0.1605(3) 0.3415(4) 0.0256(3) 0.0265(11) Uani 1 1 d . . . C56 C -0.2380(4) 0.4047(4) -0.0215(3) 0.0378(14) Uani 1 1 d . . . H56A H -0.2455 0.4173 -0.0692 0.057 Uiso 1 1 calc R . . H56B H -0.2294 0.4653 0.0046 0.057 Uiso 1 1 calc R . . H56C H -0.2898 0.3728 -0.0304 0.057 Uiso 1 1 calc R . . C57 C 0.0497(3) 0.3627(4) 0.0653(3) 0.0291(12) Uani 1 1 d . . . C58 C 0.0930(4) 0.4317(4) 0.0425(4) 0.0413(15) Uani 1 1 d . . . H58A H 0.0957 0.4952 0.0628 0.062 Uiso 1 1 calc R . . H58B H 0.0597 0.4353 -0.0120 0.062 Uiso 1 1 calc R . . H58C H 0.1517 0.4094 0.0619 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.53910(15) 0.29500(18) 0.18088(16) 0.0829(7) Uani 1 1 d D . . Cl2 Cl 0.4060(2) 0.4365(2) 0.1224(2) 0.1475(17) Uani 1 1 d D . . C60 C 0.4466(4) 0.3317(4) 0.1775(4) 0.085(3) Uani 1 1 d D . . H60A H 0.4620 0.3450 0.2284 0.102 Uiso 1 1 calc R . . H60B H 0.4022 0.2807 0.1553 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 Pd1 0.0274(2) 0.0249(2) 0.0237(2) -0.00047(16) 0.01689(18) 0.00172(16) Pd2 0.0270(2) 0.0228(2) 0.0231(2) 0.00006(15) 0.01669(18) -0.00069(16) O1 0.034(2) 0.030(2) 0.0271(19) -0.0011(16) 0.0182(18) 0.0028(16) O2 0.031(2) 0.029(2) 0.030(2) 0.0036(16) 0.0206(18) 0.0054(16) O3 0.040(2) 0.028(2) 0.037(2) 0.0010(17) 0.0285(19) 0.0021(17) O4 0.041(2) 0.0255(19) 0.033(2) 0.0006(16) 0.0262(19) -0.0026(17) O21 0.033(3) 0.098(5) 0.074(4) 0.004(3) 0.020(3) 0.021(3) O23 0.038(2) 0.058(3) 0.050(3) -0.011(2) 0.030(2) -0.009(2) O51 0.158(5) 0.169(5) 0.168(5) -0.028(4) 0.090(4) -0.020(4) O53 0.047(3) 0.066(3) 0.065(3) 0.021(3) 0.041(3) 0.015(2) N1 0.036(3) 0.026(2) 0.025(2) 0.0013(18) 0.018(2) 0.003(2) N2 0.026(2) 0.030(2) 0.023(2) -0.0003(18) 0.013(2) 0.0029(19) N31 0.032(2) 0.023(2) 0.030(2) 0.0026(18) 0.020(2) -0.0022(19) N32 0.027(2) 0.025(2) 0.026(2) -0.0012(18) 0.018(2) -0.0043(18) C1 0.031(3) 0.033(3) 0.018(2) -0.004(2) 0.016(2) 0.000(2) C2 0.037(3) 0.034(3) 0.024(3) -0.004(2) 0.020(3) -0.005(2) C3 0.043(4) 0.040(3) 0.028(3) -0.002(2) 0.022(3) -0.008(3) C4 0.047(4) 0.054(4) 0.030(3) -0.006(3) 0.017(3) -0.020(3) C5 0.067(5) 0.042(4) 0.033(3) -0.008(3) 0.028(3) -0.021(3) C6 0.064(4) 0.031(3) 0.032(3) -0.001(2) 0.030(3) -0.006(3) C7 0.046(3) 0.030(3) 0.025(3) -0.004(2) 0.024(3) -0.003(3) C8 0.050(4) 0.026(3) 0.032(3) 0.002(2) 0.029(3) 0.003(3) C9 0.032(3) 0.028(3) 0.025(3) -0.004(2) 0.019(2) 0.001(2) C10 0.030(3) 0.033(3) 0.022(3) -0.006(2) 0.016(2) 0.000(2) C11 0.035(3) 0.031(3) 0.029(3) -0.006(2) 0.022(3) 0.001(2) C12 0.034(3) 0.042(3) 0.031(3) -0.006(3) 0.021(3) 0.004(3) C13 0.034(3) 0.043(3) 0.026(3) -0.001(2) 0.018(3) 0.010(3) C14 0.037(3) 0.038(3) 0.028(3) 0.001(2) 0.021(3) 0.008(3) C15 0.023(3) 0.026(3) 0.029(3) -0.006(2) 0.015(2) -0.002(2) C16 0.032(3) 0.033(3) 0.029(3) -0.002(2) 0.018(3) -0.001(2) C17 0.030(3) 0.035(3) 0.031(3) -0.005(2) 0.010(3) 0.000(2) C18 0.028(3) 0.030(3) 0.048(4) -0.007(3) 0.021(3) -0.001(2) C19 0.037(3) 0.040(3) 0.046(4) -0.011(3) 0.029(3) -0.003(3) C20 0.025(3) 0.041(3) 0.028(3) -0.006(2) 0.013(2) -0.005(2) C21 0.038(4) 0.040(4) 0.072(5) 0.000(3) 0.030(4) 0.005(3) C22 0.064(5) 0.089(7) 0.116(8) 0.039(6) 0.068(6) 0.033(5) C23 0.030(3) 0.055(4) 0.032(3) -0.016(3) 0.021(3) -0.002(3) C24 0.028(3) 0.069(5) 0.058(4) -0.009(4) 0.024(3) 0.007(3) C31 0.026(3) 0.025(3) 0.023(3) -0.002(2) 0.016(2) -0.002(2) C32 0.038(3) 0.027(3) 0.030(3) -0.003(2) 0.023(3) 0.002(2) C33 0.034(3) 0.037(3) 0.037(3) -0.002(3) 0.021(3) -0.001(3) C34 0.030(3) 0.040(4) 0.053(4) 0.004(3) 0.020(3) 0.006(3) C35 0.039(4) 0.044(4) 0.056(4) 0.009(3) 0.021(3) 0.014(3) C36 0.039(3) 0.032(3) 0.041(3) 0.002(3) 0.020(3) 0.002(3) C37 0.037(3) 0.030(3) 0.030(3) 0.000(2) 0.020(3) 0.001(2) C38 0.040(3) 0.024(3) 0.040(3) 0.004(2) 0.026(3) 0.002(2) C39 0.029(3) 0.028(3) 0.029(3) 0.000(2) 0.019(2) -0.003(2) C40 0.030(3) 0.024(3) 0.022(3) -0.005(2) 0.015(2) -0.007(2) C41 0.029(3) 0.026(3) 0.024(3) -0.004(2) 0.016(2) -0.004(2) C42 0.029(3) 0.035(3) 0.022(3) -0.005(2) 0.016(2) -0.008(2) C43 0.037(3) 0.036(3) 0.036(3) 0.002(3) 0.026(3) -0.006(3) C44 0.037(3) 0.028(3) 0.040(3) 0.007(2) 0.023(3) -0.004(2) C45 0.025(3) 0.026(3) 0.028(3) 0.001(2) 0.015(2) 0.001(2) C46 0.036(3) 0.039(3) 0.033(3) -0.006(3) 0.020(3) -0.003(3) C47 0.039(4) 0.047(4) 0.043(4) -0.020(3) 0.017(3) -0.012(3) C48 0.031(3) 0.039(4) 0.060(4) -0.002(3) 0.023(3) -0.005(3) C49 0.038(3) 0.046(4) 0.054(4) 0.011(3) 0.035(3) 0.002(3) C50 0.032(3) 0.042(3) 0.033(3) -0.001(3) 0.022(3) 0.000(3) C51 0.069(6) 0.081(7) 0.130(10) -0.027(6) 0.053(7) -0.030(5) C52 0.068(4) 0.087(4) 0.103(4) 0.012(3) 0.057(3) -0.008(3) C53 0.029(3) 0.036(3) 0.039(3) -0.008(3) 0.021(3) -0.008(3) C54 0.038(3) 0.055(4) 0.043(4) -0.004(3) 0.030(3) -0.005(3) C55 0.032(3) 0.022(3) 0.031(3) 0.005(2) 0.021(3) 0.000(2) C56 0.041(3) 0.038(3) 0.035(3) 0.005(3) 0.021(3) 0.011(3) C57 0.029(3) 0.031(3) 0.032(3) 0.005(2) 0.020(3) 0.002(2) C58 0.055(4) 0.035(3) 0.052(4) 0.006(3) 0.041(4) 0.002(3) Cl1 0.0717(15) 0.0811(16) 0.1060(19) -0.0020(13) 0.0560(14) 0.0165(12) Cl2 0.096(2) 0.0748(18) 0.137(3) -0.0160(18) -0.0171(19) 0.0252(16) C60 0.076(6) 0.121(8) 0.075(6) -0.044(6) 0.053(5) -0.033(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 C10 1.975(5) . ? Pd1 N2 2.008(4) . ? Pd1 O3 2.064(4) . ? Pd1 O1 2.147(4) . ? Pd1 Pd2 2.9685(6) . ? Pd2 C40 1.970(5) . ? Pd2 N32 2.011(4) . ? Pd2 O2 2.052(4) . ? Pd2 O4 2.158(3) . ? O1 C55 1.255(6) . ? O2 C55 1.272(6) . ? O3 C57 1.271(7) . ? O4 C57 1.251(6) . ? O21 C21 1.211(9) . ? O23 C23 1.222(8) . ? N1 C1 1.366(7) . ? N1 C9 1.413(7) . ? N1 C8 1.476(7) . ? N2 C1 1.301(7) . ? N2 C15 1.435(7) . ? C1 C2 1.493(8) . ? C2 C7 1.399(8) . ? C2 C3 1.402(8) . ? C3 C4 1.381(9) . ? C3 H3 0.9500 . ? C4 C5 1.389(10) . ? C4 H4 0.9500 . ? C5 C6 1.378(10) . ? C5 H5 0.9500 . ? C6 C7 1.380(8) . ? C6 H6 0.9500 . ? C7 C8 1.491(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.405(8) . ? C9 C10 1.411(8) . ? C10 C11 1.395(8) . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C12 C13 1.394(8) . ? C12 C23 1.495(8) . ? C13 C14 1.372(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.395(7) . ? C15 C16 1.398(8) . ? C16 C17 1.375(8) . ? C16 H16 0.9500 . ? C17 C18 1.398(8) . ? C17 H17 0.9500 . ? C18 C19 1.389(9) . ? C18 C21 1.506(8) . ? C19 C20 1.381(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.511(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.502(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O51 C51 1.216(11) . ? O53 C53 1.217(7) . ? N31 C31 1.375(7) . ? N31 C39 1.417(7) . ? N31 C38 1.473(7) . ? N32 C31 1.307(7) . ? N32 C45 1.436(7) . ? C31 C32 1.475(7) . ? C32 C37 1.396(8) . ? C32 C33 1.397(8) . ? C33 C34 1.387(8) . ? C33 H33 0.9500 . ? C34 C35 1.396(9) . ? C34 H34 0.9500 . ? C35 C36 1.369(9) . ? C35 H35 0.9500 . ? C36 C37 1.382(8) . ? C36 H36 0.9500 . ? C37 C38 1.485(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.403(7) . ? C39 C40 1.405(8) . ? C40 C41 1.399(7) . ? C41 C42 1.405(7) . ? C41 H41 0.9500 . ? C42 C43 1.383(8) . ? C42 C53 1.503(8) . ? C43 C44 1.385(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.385(8) . ? C45 C50 1.387(7) . ? C46 C47 1.383(8) . ? C46 H46 0.9500 . ? C47 C48 1.377(9) . ? C47 H47 0.9500 . ? C48 C49 1.373(9) . ? C48 C51 1.501(10) . ? C49 C50 1.387(8) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.500(14) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.496(8) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.504(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.510(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C60 Cl1 1.764(14) . ? C60 Cl2 1.769(7) . ? C60 H60A 0.9900 . ? C60 H60B 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 C10 Pd1 N2 90.7(2) . . ? C10 Pd1 O3 92.70(19) . . ? N2 Pd1 O3 172.28(16) . . ? C10 Pd1 O1 175.23(19) . . ? N2 Pd1 O1 94.02(16) . . ? O3 Pd1 O1 82.65(15) . . ? C10 Pd1 Pd2 102.09(14) . . ? N2 Pd1 Pd2 104.74(12) . . ? O3 Pd1 Pd2 81.29(10) . . ? O1 Pd1 Pd2 76.20(10) . . ? C40 Pd2 N32 89.2(2) . . ? C40 Pd2 O2 91.78(19) . . ? N32 Pd2 O2 176.43(16) . . ? C40 Pd2 O4 176.96(19) . . ? N32 Pd2 O4 93.17(16) . . ? O2 Pd2 O4 85.78(14) . . ? C40 Pd2 Pd1 103.75(14) . . ? N32 Pd2 Pd1 100.97(12) . . ? O2 Pd2 Pd1 82.15(10) . . ? O4 Pd2 Pd1 77.73(10) . . ? C55 O1 Pd1 126.9(3) . . ? C55 O2 Pd2 122.6(3) . . ? C57 O3 Pd1 124.9(3) . . ? C57 O4 Pd2 125.6(3) . . ? C1 N1 C9 127.7(5) . . ? C1 N1 C8 112.1(5) . . ? C9 N1 C8 120.1(4) . . ? C1 N2 C15 116.7(4) . . ? C1 N2 Pd1 129.0(4) . . ? C15 N2 Pd1 114.2(3) . . ? N2 C1 N1 123.5(5) . . ? N2 C1 C2 129.0(5) . . ? N1 C1 C2 107.5(5) . . ? C7 C2 C3 119.7(5) . . ? C7 C2 C1 107.2(5) . . ? C3 C2 C1 133.1(5) . . ? C4 C3 C2 118.1(6) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.3(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 121.1(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 118.2(6) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C6 C7 C2 121.6(6) . . ? C6 C7 C8 128.1(6) . . ? C2 C7 C8 110.3(5) . . ? N1 C8 C7 102.8(5) . . ? N1 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? N1 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? C14 C9 C10 120.1(5) . . ? C14 C9 N1 117.4(5) . . ? C10 C9 N1 122.5(5) . . ? C11 C10 C9 116.3(5) . . ? C11 C10 Pd1 118.0(4) . . ? C9 C10 Pd1 125.3(4) . . ? C10 C11 C12 123.7(5) . . ? C10 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C13 C12 C11 118.3(5) . . ? C13 C12 C23 123.5(6) . . ? C11 C12 C23 118.1(6) . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 121.6(6) . . ? C13 C14 H14 119.2 . . ? C9 C14 H14 119.2 . . ? C20 C15 C16 119.7(5) . . ? C20 C15 N2 119.2(5) . . ? C16 C15 N2 121.1(5) . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.3(5) . . ? C19 C18 C21 122.7(6) . . ? C17 C18 C21 118.0(6) . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C15 120.0(5) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? O21 C21 C18 121.1(7) . . ? O21 C21 C22 121.1(7) . . ? C18 C21 C22 117.7(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O23 C23 C12 120.5(6) . . ? O23 C23 C24 120.5(6) . . ? C12 C23 C24 119.0(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 N31 C39 125.6(4) . . ? C31 N31 C38 111.7(4) . . ? C39 N31 C38 120.1(4) . . ? C31 N32 C45 117.5(4) . . ? C31 N32 Pd2 125.0(3) . . ? C45 N32 Pd2 117.4(3) . . ? N32 C31 N31 122.3(5) . . ? N32 C31 C32 130.3(5) . . ? N31 C31 C32 107.5(4) . . ? C37 C32 C33 119.4(5) . . ? C37 C32 C31 107.7(5) . . ? C33 C32 C31 132.8(5) . . ? C34 C33 C32 118.0(6) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 121.6(6) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C36 C35 C34 120.5(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 118.4(6) . . ? C35 C36 H36 120.8 . . ? C37 C36 H36 120.8 . . ? C36 C37 C32 122.1(5) . . ? C36 C37 C38 127.7(5) . . ? C32 C37 C38 110.2(5) . . ? N31 C38 C37 102.9(4) . . ? N31 C38 H38A 111.2 . . ? C37 C38 H38A 111.2 . . ? N31 C38 H38B 111.2 . . ? C37 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? C44 C39 C40 120.7(5) . . ? C44 C39 N31 117.3(5) . . ? C40 C39 N31 122.0(5) . . ? C41 C40 C39 117.0(5) . . ? C41 C40 Pd2 120.7(4) . . ? C39 C40 Pd2 122.3(4) . . ? C40 C41 C42 122.3(5) . . ? C40 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C43 C42 C41 119.2(5) . . ? C43 C42 C53 121.3(5) . . ? C41 C42 C53 119.5(5) . . ? C42 C43 C44 119.9(5) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C39 120.6(5) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? C46 C45 C50 120.0(5) . . ? C46 C45 N32 118.4(5) . . ? C50 C45 N32 121.6(5) . . ? C47 C46 C45 119.6(6) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C48 C47 C46 120.6(6) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C49 C48 C47 119.4(5) . . ? C49 C48 C51 123.5(6) . . ? C47 C48 C51 116.9(6) . . ? C48 C49 C50 121.0(5) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C45 C50 C49 119.1(5) . . ? C45 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? O51 C51 C52 121.7(6) . . ? O51 C51 C48 122.4(7) . . ? C52 C51 C48 115.8(6) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O53 C53 C54 121.0(5) . . ? O53 C53 C42 121.0(5) . . ? C54 C53 C42 118.0(5) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1 C55 O2 126.1(5) . . ? O1 C55 C56 117.4(5) . . ? O2 C55 C56 116.5(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O4 C57 O3 126.4(5) . . ? O4 C57 C58 118.5(5) . . ? O3 C57 C58 115.0(5) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? Cl1 C60 Cl2 107.9(5) . . ? Cl1 C60 H60A 110.1 . . ? Cl2 C60 H60A 110.1 . . ? Cl1 C60 H60B 110.1 . . ? Cl2 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Pd1 O1 C55 85.5(4) . . . . ? O3 Pd1 O1 C55 -101.4(4) . . . . ? Pd2 Pd1 O1 C55 -18.7(4) . . . . ? C40 Pd2 O2 C55 -126.3(4) . . . . ? O4 Pd2 O2 C55 55.5(4) . . . . ? Pd1 Pd2 O2 C55 -22.7(4) . . . . ? C10 Pd1 O3 C57 -119.8(4) . . . . ? O1 Pd1 O3 C57 59.1(4) . . . . ? Pd2 Pd1 O3 C57 -18.0(4) . . . . ? N32 Pd2 O4 C57 84.1(4) . . . . ? O2 Pd2 O4 C57 -99.4(4) . . . . ? Pd1 Pd2 O4 C57 -16.5(4) . . . . ? C10 Pd1 N2 C1 -4.1(5) . . . . ? O1 Pd1 N2 C1 176.4(4) . . . . ? Pd2 Pd1 N2 C1 -106.8(4) . . . . ? C10 Pd1 N2 C15 173.2(4) . . . . ? O1 Pd1 N2 C15 -6.2(3) . . . . ? Pd2 Pd1 N2 C15 70.5(3) . . . . ? C40 Pd2 Pd1 C10 -78.5(2) . . . . ? N32 Pd2 Pd1 C10 13.3(2) . . . . ? O2 Pd2 Pd1 C10 -168.41(19) . . . . ? O4 Pd2 Pd1 C10 104.24(19) . . . . ? C40 Pd2 Pd1 N2 15.5(2) . . . . ? N32 Pd2 Pd1 N2 107.35(17) . . . . ? O2 Pd2 Pd1 N2 -74.40(16) . . . . ? O4 Pd2 Pd1 N2 -161.76(17) . . . . ? C40 Pd2 Pd1 O3 -169.40(19) . . . . ? N32 Pd2 Pd1 O3 -77.56(16) . . . . ? O2 Pd2 Pd1 O3 100.68(15) . . . . ? O4 Pd2 Pd1 O3 13.32(15) . . . . ? C40 Pd2 Pd1 O1 106.08(19) . . . . ? N32 Pd2 Pd1 O1 -162.08(16) . . . . ? O2 Pd2 Pd1 O1 16.17(14) . . . . ? O4 Pd2 Pd1 O1 -71.19(15) . . . . ? C15 N2 C1 N1 -168.4(4) . . . . ? Pd1 N2 C1 N1 9.0(7) . . . . ? C15 N2 C1 C2 12.9(8) . . . . ? Pd1 N2 C1 C2 -169.8(4) . . . . ? C9 N1 C1 N2 -2.9(8) . . . . ? C8 N1 C1 N2 -179.4(5) . . . . ? C9 N1 C1 C2 176.1(5) . . . . ? C8 N1 C1 C2 -0.4(5) . . . . ? N2 C1 C2 C7 179.5(5) . . . . ? N1 C1 C2 C7 0.6(5) . . . . ? N2 C1 C2 C3 0.3(9) . . . . ? N1 C1 C2 C3 -178.6(5) . . . . ? C7 C2 C3 C4 1.0(8) . . . . ? C1 C2 C3 C4 -179.8(5) . . . . ? C2 C3 C4 C5 -0.3(9) . . . . ? C3 C4 C5 C6 -0.8(10) . . . . ? C4 C5 C6 C7 1.1(9) . . . . ? C5 C6 C7 C2 -0.4(8) . . . . ? C5 C6 C7 C8 -179.8(5) . . . . ? C3 C2 C7 C6 -0.7(8) . . . . ? C1 C2 C7 C6 180.0(5) . . . . ? C3 C2 C7 C8 178.8(5) . . . . ? C1 C2 C7 C8 -0.5(6) . . . . ? C1 N1 C8 C7 0.1(5) . . . . ? C9 N1 C8 C7 -176.7(4) . . . . ? C6 C7 C8 N1 179.8(5) . . . . ? C2 C7 C8 N1 0.3(6) . . . . ? C1 N1 C9 C14 172.1(5) . . . . ? C8 N1 C9 C14 -11.6(7) . . . . ? C1 N1 C9 C10 -8.5(8) . . . . ? C8 N1 C9 C10 167.8(5) . . . . ? C14 C9 C10 C11 4.9(7) . . . . ? N1 C9 C10 C11 -174.4(5) . . . . ? C14 C9 C10 Pd1 -167.9(4) . . . . ? N1 C9 C10 Pd1 12.7(7) . . . . ? N2 Pd1 C10 C11 -179.1(4) . . . . ? O3 Pd1 C10 C11 7.8(4) . . . . ? Pd2 Pd1 C10 C11 -73.9(4) . . . . ? N2 Pd1 C10 C9 -6.4(4) . . . . ? O3 Pd1 C10 C9 -179.5(4) . . . . ? Pd2 Pd1 C10 C9 98.8(4) . . . . ? C9 C10 C11 C12 -5.3(8) . . . . ? Pd1 C10 C11 C12 168.1(4) . . . . ? C10 C11 C12 C13 1.5(8) . . . . ? C10 C11 C12 C23 -176.8(5) . . . . ? C11 C12 C13 C14 2.9(8) . . . . ? C23 C12 C13 C14 -178.9(5) . . . . ? C12 C13 C14 C9 -3.1(8) . . . . ? C10 C9 C14 C13 -0.9(8) . . . . ? N1 C9 C14 C13 178.5(5) . . . . ? C1 N2 C15 C20 72.0(6) . . . . ? Pd1 N2 C15 C20 -105.7(5) . . . . ? C1 N2 C15 C16 -109.1(6) . . . . ? Pd1 N2 C15 C16 73.2(6) . . . . ? C20 C15 C16 C17 -3.0(8) . . . . ? N2 C15 C16 C17 178.2(5) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? C16 C17 C18 C19 1.4(9) . . . . ? C16 C17 C18 C21 -178.8(6) . . . . ? C17 C18 C19 C20 -1.9(9) . . . . ? C21 C18 C19 C20 178.3(6) . . . . ? C18 C19 C20 C15 0.0(9) . . . . ? C16 C15 C20 C19 2.4(8) . . . . ? N2 C15 C20 C19 -178.7(5) . . . . ? C19 C18 C21 O21 -178.8(7) . . . . ? C17 C18 C21 O21 1.4(10) . . . . ? C19 C18 C21 C22 1.0(10) . . . . ? C17 C18 C21 C22 -178.9(7) . . . . ? C13 C12 C23 O23 -173.6(5) . . . . ? C11 C12 C23 O23 4.7(8) . . . . ? C13 C12 C23 C24 7.3(8) . . . . ? C11 C12 C23 C24 -174.5(5) . . . . ? C40 Pd2 N32 C31 34.1(4) . . . . ? O4 Pd2 N32 C31 -147.8(4) . . . . ? Pd1 Pd2 N32 C31 -69.7(4) . . . . ? C40 Pd2 N32 C45 -149.1(4) . . . . ? O4 Pd2 N32 C45 29.0(4) . . . . ? Pd1 Pd2 N32 C45 107.1(3) . . . . ? C45 N32 C31 N31 168.0(5) . . . . ? Pd2 N32 C31 N31 -15.2(7) . . . . ? C45 N32 C31 C32 -13.4(8) . . . . ? Pd2 N32 C31 C32 163.4(4) . . . . ? C39 N31 C31 N32 -20.4(8) . . . . ? C38 N31 C31 N32 177.9(5) . . . . ? C39 N31 C31 C32 160.7(5) . . . . ? C38 N31 C31 C32 -1.1(6) . . . . ? N32 C31 C32 C37 -176.4(5) . . . . ? N31 C31 C32 C37 2.4(6) . . . . ? N32 C31 C32 C33 0.7(10) . . . . ? N31 C31 C32 C33 179.6(6) . . . . ? C37 C32 C33 C34 -0.3(8) . . . . ? C31 C32 C33 C34 -177.2(6) . . . . ? C32 C33 C34 C35 0.1(10) . . . . ? C33 C34 C35 C36 -0.6(11) . . . . ? C34 C35 C36 C37 1.3(10) . . . . ? C35 C36 C37 C32 -1.6(9) . . . . ? C35 C36 C37 C38 -179.8(6) . . . . ? C33 C32 C37 C36 1.1(8) . . . . ? C31 C32 C37 C36 178.7(5) . . . . ? C33 C32 C37 C38 179.6(5) . . . . ? C31 C32 C37 C38 -2.8(6) . . . . ? C31 N31 C38 C37 -0.6(6) . . . . ? C39 N31 C38 C37 -163.5(5) . . . . ? C36 C37 C38 N31 -179.6(6) . . . . ? C32 C37 C38 N31 2.1(6) . . . . ? C31 N31 C39 C44 -155.3(5) . . . . ? C38 N31 C39 C44 5.1(7) . . . . ? C31 N31 C39 C40 23.2(8) . . . . ? C38 N31 C39 C40 -176.4(5) . . . . ? C44 C39 C40 C41 5.2(8) . . . . ? N31 C39 C40 C41 -173.2(5) . . . . ? C44 C39 C40 Pd2 -171.7(4) . . . . ? N31 C39 C40 Pd2 9.9(7) . . . . ? N32 Pd2 C40 C41 153.3(4) . . . . ? O2 Pd2 C40 C41 -23.3(4) . . . . ? Pd1 Pd2 C40 C41 -105.7(4) . . . . ? N32 Pd2 C40 C39 -29.9(4) . . . . ? O2 Pd2 C40 C39 153.5(4) . . . . ? Pd1 Pd2 C40 C39 71.2(4) . . . . ? C39 C40 C41 C42 -0.5(7) . . . . ? Pd2 C40 C41 C42 176.4(4) . . . . ? C40 C41 C42 C43 -3.1(8) . . . . ? C40 C41 C42 C53 178.1(5) . . . . ? C41 C42 C43 C44 2.0(8) . . . . ? C53 C42 C43 C44 -179.2(5) . . . . ? C42 C43 C44 C39 2.7(9) . . . . ? C40 C39 C44 C43 -6.4(8) . . . . ? N31 C39 C44 C43 172.1(5) . . . . ? C31 N32 C45 C46 -87.3(6) . . . . ? Pd2 N32 C45 C46 95.6(5) . . . . ? C31 N32 C45 C50 92.2(6) . . . . ? Pd2 N32 C45 C50 -84.8(6) . . . . ? C50 C45 C46 C47 -4.6(9) . . . . ? N32 C45 C46 C47 174.9(6) . . . . ? C45 C46 C47 C48 1.8(10) . . . . ? C46 C47 C48 C49 1.6(10) . . . . ? C46 C47 C48 C51 -174.1(6) . . . . ? C47 C48 C49 C50 -2.1(10) . . . . ? C51 C48 C49 C50 173.2(5) . . . . ? C46 C45 C50 C49 4.1(9) . . . . ? N32 C45 C50 C49 -175.5(5) . . . . ? C48 C49 C50 C45 -0.7(9) . . . . ? C49 C48 C51 O51 -171.9(7) . . . . ? C47 C48 C51 O51 3.5(7) . . . . ? C49 C48 C51 C52 7.9(7) . . . . ? C47 C48 C51 C52 -176.6(6) . . . . ? C43 C42 C53 O53 -157.5(6) . . . . ? C41 C42 C53 O53 21.3(8) . . . . ? C43 C42 C53 C54 24.2(8) . . . . ? C41 C42 C53 C54 -156.9(5) . . . . ? Pd1 O1 C55 O2 8.4(8) . . . . ? Pd1 O1 C55 C56 -171.6(4) . . . . ? Pd2 O2 C55 O1 17.0(7) . . . . ? Pd2 O2 C55 C56 -163.0(4) . . . . ? Pd2 O4 C57 O3 9.3(8) . . . . ? Pd2 O4 C57 C58 -168.0(4) . . . . ? Pd1 O3 C57 O4 11.9(8) . . . . ? Pd1 O3 C57 C58 -170.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.611 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.112 #===END data_1176 _database_code_depnum_ccdc_archive 'CCDC 687005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H44 N4 O4 Pd2, C H Cl3' _chemical_formula_sum 'C49 H45 Cl3 N4 O4 Pd2' _chemical_formula_weight 1073.04 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 23.1864(3) _cell_length_b 9.6437(1) _cell_length_c 20.2415(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.026(1) _cell_angle_gamma 90.00 _cell_volume 4371.30(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11780 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 28.700 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details 'Shelxtl 6.10 (Bruker-AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 77979 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.71 _reflns_number_total 11273 _reflns_number_gt 8852 _reflns_threshold_expression >/2(I) _computing_data_collection 'Collect (Nonius BV, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON. (Spek, 2003)' _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^)+(0.0279P)^2^+7.6740P] 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 11273 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.196278(10) 0.15406(2) 0.136423(11) 0.02188(6) Uani 1 1 d . . . Pd2 Pd 0.235276(10) 0.38922(2) 0.060686(11) 0.02093(6) Uani 1 1 d . . . O1 O 0.11961(10) 0.1999(3) 0.05960(11) 0.0334(5) Uani 1 1 d . . . O2 O 0.15667(10) 0.3213(2) -0.01380(11) 0.0308(5) Uani 1 1 d . . . O3 O 0.22669(10) 0.0614(2) 0.05436(11) 0.0286(5) Uani 1 1 d . . . O4 O 0.27823(10) 0.2314(2) 0.02235(11) 0.0306(5) Uani 1 1 d . . . N1 N 0.22437(12) 0.1098(3) 0.30495(13) 0.0262(5) Uani 1 1 d . . . N2 N 0.26318(11) 0.0722(3) 0.21036(12) 0.0234(5) Uani 1 1 d . . . N31 N 0.25010(11) 0.5499(3) 0.20299(12) 0.0217(5) Uani 1 1 d . . . N32 N 0.19601(11) 0.5581(3) 0.08826(12) 0.0215(5) Uani 1 1 d . . . C1 C 0.26419(13) 0.0516(3) 0.27420(15) 0.0226(6) Uani 1 1 d . . . C2 C 0.30432(14) -0.0391(3) 0.32602(15) 0.0256(6) Uani 1 1 d . . . C3 C 0.35319(14) -0.1234(3) 0.32415(16) 0.0290(7) Uani 1 1 d . . . H3 H 0.3679 -0.1274 0.2846 0.035 Uiso 1 1 calc R . . C4 C 0.37938(15) -0.2011(4) 0.38214(17) 0.0326(7) Uani 1 1 d . . . H4 H 0.4125 -0.2588 0.3818 0.039 Uiso 1 1 calc R . . C5 C 0.35854(16) -0.1966(4) 0.44018(18) 0.0372(8) Uani 1 1 d . . . H5 H 0.3767 -0.2527 0.4785 0.045 Uiso 1 1 calc R . . C6 C 0.31104(16) -0.1105(4) 0.44283(17) 0.0370(8) Uani 1 1 d . . . H6 H 0.2970 -0.1052 0.4829 0.044 Uiso 1 1 calc R . . C7 C 0.28495(14) -0.0330(3) 0.38559(16) 0.0281(7) Uani 1 1 d . . . C8 C 0.23457(15) 0.0668(4) 0.37685(15) 0.0305(7) Uani 1 1 d . . . H8A H 0.1987 0.0215 0.3850 0.037 Uiso 1 1 calc R . . H8B H 0.2457 0.1469 0.4082 0.037 Uiso 1 1 calc R . . C9 C 0.17986(14) 0.2088(3) 0.27625(15) 0.0260(6) Uani 1 1 d . . . C10 C 0.16303(13) 0.2406(3) 0.20662(15) 0.0245(6) Uani 1 1 d . . . C11 C 0.11864(14) 0.3408(3) 0.18518(16) 0.0256(6) Uani 1 1 d . . . H11 H 0.1075 0.3649 0.1381 0.031 Uiso 1 1 calc R . . C12 C 0.08969(15) 0.4076(3) 0.22859(17) 0.0303(7) Uani 1 1 d . . . C13 C 0.10772(18) 0.3731(4) 0.29694(19) 0.0411(9) Uani 1 1 d . . . H13 H 0.0894 0.4176 0.3281 0.049 Uiso 1 1 calc R . . C14 C 0.15168(17) 0.2754(4) 0.32132(18) 0.0386(8) Uani 1 1 d . . . H14 H 0.1629 0.2531 0.3686 0.046 Uiso 1 1 calc R . . C15 C 0.31101(13) 0.0119(3) 0.18619(15) 0.0224(6) Uani 1 1 d . . . C16 C 0.36357(14) 0.0843(3) 0.19261(16) 0.0264(6) Uani 1 1 d . . . H16 H 0.3677 0.1757 0.2107 0.032 Uiso 1 1 calc R . . C17 C 0.41016(14) 0.0222(3) 0.17243(17) 0.0293(7) Uani 1 1 d . . . H17 H 0.4462 0.0725 0.1766 0.035 Uiso 1 1 calc R . . C18 C 0.40550(14) -0.1123(4) 0.14612(16) 0.0286(7) Uani 1 1 d . . . C19 C 0.35144(15) -0.1806(3) 0.13814(16) 0.0287(7) Uani 1 1 d . . . H19 H 0.3467 -0.2711 0.1190 0.034 Uiso 1 1 calc R . . C20 C 0.30441(14) -0.1200(3) 0.15740(16) 0.0264(6) Uani 1 1 d . . . H20 H 0.2676 -0.1682 0.1510 0.032 Uiso 1 1 calc R . . C21 C 0.04056(16) 0.5104(4) 0.2017(2) 0.0389(8) Uani 1 1 d . . . H21A H 0.0019 0.4673 0.1999 0.058 Uiso 1 1 calc R . . H21B H 0.0415 0.5399 0.1557 0.058 Uiso 1 1 calc R . . H21C H 0.0462 0.5913 0.2320 0.058 Uiso 1 1 calc R . . C22 C 0.45762(16) -0.1821(4) 0.1282(2) 0.0401(9) Uani 1 1 d . . . H22A H 0.4855 -0.2166 0.1700 0.060 Uiso 1 1 calc R . . H22B H 0.4781 -0.1153 0.1057 0.060 Uiso 1 1 calc R . . H22C H 0.4431 -0.2599 0.0972 0.060 Uiso 1 1 calc R . . C31 C 0.20400(13) 0.5992(3) 0.15105(15) 0.0218(6) Uani 1 1 d . . . C32 C 0.16868(13) 0.6958(3) 0.18207(16) 0.0240(6) Uani 1 1 d . . . C33 C 0.12339(15) 0.7904(4) 0.15401(18) 0.0325(7) Uani 1 1 d . . . H33 H 0.1089 0.8006 0.1059 0.039 Uiso 1 1 calc R . . C34 C 0.10004(16) 0.8694(4) 0.1984(2) 0.0392(8) Uani 1 1 d . . . H34 H 0.0699 0.9360 0.1804 0.047 Uiso 1 1 calc R . . C35 C 0.12024(16) 0.8523(4) 0.2687(2) 0.0432(9) Uani 1 1 d . . . H35 H 0.1026 0.9048 0.2980 0.052 Uiso 1 1 calc R . . C36 C 0.16565(15) 0.7602(4) 0.29684(18) 0.0351(8) Uani 1 1 d . . . H36 H 0.1795 0.7491 0.3450 0.042 Uiso 1 1 calc R . . C37 C 0.19027(14) 0.6846(3) 0.25278(17) 0.0275(7) Uani 1 1 d . . . C38 C 0.24255(14) 0.5878(3) 0.27040(16) 0.0279(7) Uani 1 1 d . . . H38A H 0.2786 0.6347 0.2985 0.033 Uiso 1 1 calc R . . H38B H 0.2338 0.5053 0.2953 0.033 Uiso 1 1 calc R . . C39 C 0.30475(13) 0.5007(3) 0.19264(15) 0.0210(6) Uani 1 1 d . . . C40 C 0.30764(13) 0.4416(3) 0.13021(15) 0.0219(6) Uani 1 1 d . . . C41 C 0.36444(14) 0.4117(3) 0.12141(16) 0.0267(6) Uani 1 1 d . . . H41 H 0.3670 0.3744 0.0789 0.032 Uiso 1 1 calc R . . C42 C 0.41707(13) 0.4341(3) 0.17189(17) 0.0280(7) Uani 1 1 d . . . C43 C 0.41203(14) 0.4883(3) 0.23390(17) 0.0297(7) Uani 1 1 d . . . H43 H 0.4471 0.5031 0.2697 0.036 Uiso 1 1 calc R . . C44 C 0.35716(14) 0.5208(3) 0.24434(16) 0.0266(6) Uani 1 1 d . . . H44 H 0.3550 0.5574 0.2872 0.032 Uiso 1 1 calc R . . C45 C 0.15181(13) 0.6292(3) 0.03597(15) 0.0225(6) Uani 1 1 d . . . C46 C 0.09371(13) 0.5787(3) 0.01444(16) 0.0273(7) Uani 1 1 d . . . H46 H 0.0830 0.4956 0.0335 0.033 Uiso 1 1 calc R . . C47 C 0.05176(14) 0.6496(4) -0.03461(17) 0.0303(7) Uani 1 1 d . . . H47 H 0.0123 0.6138 -0.0491 0.036 Uiso 1 1 calc R . . C48 C 0.06540(14) 0.7718(4) -0.06348(17) 0.0313(7) Uani 1 1 d . . . C49 C 0.12377(14) 0.8212(4) -0.04112(18) 0.0324(7) Uani 1 1 d . . . H49 H 0.1343 0.9053 -0.0596 0.039 Uiso 1 1 calc R . . C50 C 0.16698(14) 0.7498(3) 0.00769(16) 0.0282(7) Uani 1 1 d . . . H50 H 0.2067 0.7840 0.0215 0.034 Uiso 1 1 calc R . . C51 C 0.47727(15) 0.3995(4) 0.1605(2) 0.0394(8) Uani 1 1 d . . . H51A H 0.4724 0.3292 0.1245 0.059 Uiso 1 1 calc R . . H51B H 0.5035 0.3635 0.2030 0.059 Uiso 1 1 calc R . . H51C H 0.4950 0.4833 0.1466 0.059 Uiso 1 1 calc R . . C52 C 0.01818(17) 0.8475(4) -0.1161(2) 0.0492(11) Uani 1 1 d . . . H52A H 0.0118 0.8006 -0.1604 0.074 Uiso 1 1 calc R . . H52B H 0.0312 0.9431 -0.1203 0.074 Uiso 1 1 calc R . . H52C H -0.0192 0.8482 -0.1021 0.074 Uiso 1 1 calc R . . C61 C 0.11686(15) 0.2520(4) 0.00205(16) 0.0306(7) Uani 1 1 d . . . C62 C 0.05866(16) 0.2320(5) -0.05193(19) 0.0451(10) Uani 1 1 d . . . H62A H 0.0293 0.2995 -0.0448 0.068 Uiso 1 1 calc R . . H62B H 0.0437 0.1379 -0.0486 0.068 Uiso 1 1 calc R . . H62C H 0.0653 0.2455 -0.0974 0.068 Uiso 1 1 calc R . . C63 C 0.25859(14) 0.1093(3) 0.02021(16) 0.0280(7) Uani 1 1 d . . . C64 C 0.27751(19) 0.0122(4) -0.0296(2) 0.0452(9) Uani 1 1 d . . . H64A H 0.2475 -0.0608 -0.0440 0.068 Uiso 1 1 calc R . . H64B H 0.3161 -0.0299 -0.0072 0.068 Uiso 1 1 calc R . . H64C H 0.2812 0.0648 -0.0698 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.37055(5) 0.30044(12) 0.36929(5) 0.0539(3) Uani 1 1 d . . . Cl2 Cl 0.43874(6) 0.39457(13) 0.50153(7) 0.0658(3) Uani 1 1 d . . . Cl3 Cl 0.44435(5) 0.10954(11) 0.46294(6) 0.0559(3) Uani 1 1 d . . . C65 C 0.39860(17) 0.2560(4) 0.45533(18) 0.0378(8) Uani 1 1 d . . . H65 H 0.3643 0.2337 0.4749 0.045 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 0.02341(12) 0.02443(12) 0.01922(11) -0.00104(9) 0.00809(9) -0.00190(9) Pd2 0.02268(11) 0.02213(12) 0.01792(11) -0.00120(8) 0.00518(8) 0.00092(9) O1 0.0287(12) 0.0441(14) 0.0274(12) -0.0022(10) 0.0071(9) 0.0006(10) O2 0.0285(12) 0.0353(13) 0.0258(12) -0.0068(9) 0.0022(9) -0.0005(10) O3 0.0383(12) 0.0291(12) 0.0215(11) -0.0012(9) 0.0132(9) 0.0006(10) O4 0.0310(12) 0.0292(13) 0.0307(12) -0.0037(9) 0.0066(10) 0.0008(10) N1 0.0302(14) 0.0297(14) 0.0206(13) -0.0013(10) 0.0097(10) 0.0032(11) N2 0.0252(13) 0.0247(13) 0.0217(13) -0.0005(10) 0.0087(10) 0.0005(10) N31 0.0227(12) 0.0249(13) 0.0180(12) -0.0013(10) 0.0059(9) 0.0007(10) N32 0.0222(12) 0.0212(12) 0.0210(12) 0.0007(9) 0.0053(10) 0.0017(10) C1 0.0254(14) 0.0214(15) 0.0218(15) -0.0014(11) 0.0074(12) -0.0043(12) C2 0.0298(16) 0.0243(16) 0.0224(15) -0.0020(12) 0.0062(12) -0.0059(13) C3 0.0314(16) 0.0269(17) 0.0272(16) 0.0004(12) 0.0050(13) 0.0002(13) C4 0.0308(17) 0.0308(18) 0.0327(18) 0.0010(14) 0.0023(14) 0.0015(14) C5 0.041(2) 0.037(2) 0.0289(18) 0.0083(14) 0.0018(15) -0.0014(16) C6 0.0392(19) 0.046(2) 0.0239(17) 0.0050(15) 0.0059(14) -0.0018(16) C7 0.0320(17) 0.0274(17) 0.0243(16) -0.0004(12) 0.0065(13) -0.0040(13) C8 0.0374(18) 0.0359(18) 0.0197(15) 0.0002(13) 0.0102(13) 0.0004(14) C9 0.0325(16) 0.0259(16) 0.0222(15) -0.0028(12) 0.0118(13) -0.0001(13) C10 0.0262(15) 0.0258(16) 0.0243(15) -0.0004(12) 0.0114(12) -0.0034(12) C11 0.0268(15) 0.0296(17) 0.0223(15) 0.0002(12) 0.0098(12) -0.0021(13) C12 0.0313(17) 0.0249(17) 0.0373(18) 0.0025(13) 0.0136(14) 0.0034(13) C13 0.054(2) 0.043(2) 0.0328(19) 0.0011(15) 0.0238(17) 0.0136(18) C14 0.051(2) 0.044(2) 0.0252(17) 0.0021(15) 0.0177(16) 0.0129(17) C15 0.0236(14) 0.0239(15) 0.0211(14) 0.0032(11) 0.0084(11) 0.0008(12) C16 0.0293(16) 0.0224(16) 0.0271(16) 0.0015(12) 0.0068(13) -0.0010(12) C17 0.0241(15) 0.0309(17) 0.0338(18) 0.0032(13) 0.0091(13) 0.0001(13) C18 0.0307(16) 0.0331(18) 0.0226(15) 0.0034(13) 0.0081(13) 0.0059(14) C19 0.0359(17) 0.0251(17) 0.0261(16) -0.0011(12) 0.0099(13) 0.0026(13) C20 0.0295(15) 0.0250(16) 0.0262(16) 0.0002(12) 0.0097(12) -0.0058(13) C21 0.0355(19) 0.038(2) 0.047(2) 0.0015(16) 0.0175(16) 0.0074(16) C22 0.0359(19) 0.043(2) 0.043(2) -0.0024(16) 0.0136(16) 0.0111(16) C31 0.0210(14) 0.0220(15) 0.0243(15) -0.0002(11) 0.0096(11) -0.0026(11) C32 0.0217(14) 0.0215(15) 0.0300(16) -0.0042(12) 0.0091(12) -0.0025(12) C33 0.0326(17) 0.0295(18) 0.0362(18) -0.0008(14) 0.0103(14) 0.0046(14) C34 0.0318(18) 0.034(2) 0.052(2) -0.0065(16) 0.0104(16) 0.0085(15) C35 0.0363(19) 0.045(2) 0.052(2) -0.0186(18) 0.0187(17) 0.0041(17) C36 0.0316(17) 0.044(2) 0.0324(18) -0.0106(15) 0.0127(14) -0.0035(15) C37 0.0244(15) 0.0270(17) 0.0329(17) -0.0053(13) 0.0108(13) -0.0046(12) C38 0.0303(16) 0.0317(18) 0.0229(15) -0.0029(12) 0.0090(12) -0.0020(13) C39 0.0210(14) 0.0188(14) 0.0225(14) 0.0013(11) 0.0045(11) -0.0017(11) C40 0.0218(14) 0.0203(14) 0.0237(15) 0.0017(11) 0.0063(11) -0.0002(11) C41 0.0276(16) 0.0241(16) 0.0293(16) 0.0001(12) 0.0089(13) 0.0022(12) C42 0.0208(14) 0.0288(17) 0.0337(17) 0.0020(13) 0.0060(13) 0.0011(13) C43 0.0232(15) 0.0312(17) 0.0317(17) -0.0002(13) 0.0016(13) 0.0002(13) C44 0.0278(15) 0.0276(16) 0.0223(15) -0.0010(12) 0.0030(12) -0.0002(13) C45 0.0231(14) 0.0228(15) 0.0220(14) -0.0004(11) 0.0066(11) 0.0018(12) C46 0.0231(15) 0.0275(17) 0.0311(17) 0.0066(13) 0.0066(13) -0.0025(12) C47 0.0204(15) 0.0346(18) 0.0332(17) 0.0051(14) 0.0019(13) -0.0021(13) C48 0.0262(16) 0.0329(18) 0.0331(18) 0.0081(14) 0.0045(13) 0.0014(13) C49 0.0277(16) 0.0315(18) 0.0373(19) 0.0119(14) 0.0070(14) -0.0027(14) C50 0.0235(15) 0.0290(17) 0.0313(17) 0.0033(13) 0.0057(13) -0.0050(13) C51 0.0258(17) 0.047(2) 0.046(2) -0.0013(17) 0.0091(15) 0.0035(15) C52 0.0334(19) 0.050(2) 0.054(2) 0.026(2) -0.0070(17) -0.0040(17) C61 0.0304(17) 0.0341(18) 0.0265(17) -0.0104(13) 0.0061(13) 0.0076(14) C62 0.0287(18) 0.067(3) 0.036(2) -0.0134(18) 0.0023(15) 0.0001(18) C63 0.0305(16) 0.0309(17) 0.0227(15) 0.0020(12) 0.0074(13) 0.0012(13) C64 0.059(2) 0.038(2) 0.048(2) -0.0088(17) 0.031(2) -0.0036(18) Cl1 0.0708(7) 0.0561(6) 0.0366(5) 0.0070(4) 0.0173(5) 0.0027(5) Cl2 0.0694(7) 0.0551(7) 0.0707(8) -0.0284(6) 0.0140(6) -0.0120(6) Cl3 0.0632(7) 0.0444(6) 0.0605(7) -0.0010(5) 0.0167(5) 0.0084(5) C65 0.041(2) 0.039(2) 0.0370(19) -0.0009(15) 0.0159(16) -0.0062(16) _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 C10 1.969(3) . ? Pd1 N2 2.016(3) . ? Pd1 O1 2.083(2) . ? Pd1 O3 2.159(2) . ? Pd1 Pd2 3.0049(3) . ? Pd2 C40 1.956(3) . ? Pd2 N32 2.014(2) . ? Pd2 O4 2.077(2) . ? Pd2 O2 2.145(2) . ? O1 C61 1.255(4) . ? O2 C61 1.247(4) . ? O3 C63 1.226(4) . ? O4 C63 1.259(4) . ? N1 C1 1.361(4) . ? N1 C9 1.416(4) . ? N1 C8 1.472(4) . ? N2 C1 1.302(4) . ? N2 C15 1.445(4) . ? N31 C31 1.375(4) . ? N31 C39 1.418(4) . ? N31 C38 1.466(4) . ? N32 C31 1.298(4) . ? N32 C45 1.441(4) . ? C1 C2 1.492(4) . ? C2 C7 1.393(4) . ? C2 C3 1.404(5) . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 C8 1.488(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.395(4) . ? C9 C14 1.407(4) . ? C10 C11 1.397(4) . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 C21 1.502(5) . ? C13 C14 1.381(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C15 C20 1.391(4) . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C17 C18 1.396(5) . ? C17 H17 0.9500 . ? C18 C19 1.388(5) . ? C18 C22 1.508(5) . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.483(4) . ? C32 C37 1.393(5) . ? C32 C33 1.396(4) . ? C33 C34 1.391(5) . ? C33 H33 0.9500 . ? C34 C35 1.387(6) . ? C34 H34 0.9500 . ? C35 C36 1.382(5) . ? C35 H35 0.9500 . ? C36 C37 1.384(4) . ? C36 H36 0.9500 . ? C37 C38 1.498(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.397(4) . ? C39 C40 1.403(4) . ? C40 C41 1.404(4) . ? C41 C42 1.390(4) . ? C41 H41 0.9500 . ? C42 C43 1.392(5) . ? C42 C51 1.510(4) . ? C43 C44 1.379(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.382(4) . ? C45 C46 1.392(4) . ? C46 C47 1.378(4) . ? C46 H46 0.9500 . ? C47 C48 1.388(5) . ? C47 H47 0.9500 . ? C48 C49 1.395(4) . ? C48 C52 1.504(5) . ? C49 C50 1.393(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C61 C62 1.513(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.522(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? Cl1 C65 1.747(4) . ? Cl2 C65 1.754(4) . ? Cl3 C65 1.749(4) . ? C65 H65 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 C10 Pd1 N2 90.00(11) . . ? C10 Pd1 O1 91.77(11) . . ? N2 Pd1 O1 168.66(10) . . ? C10 Pd1 O3 175.96(11) . . ? N2 Pd1 O3 93.85(9) . . ? O1 Pd1 O3 84.22(9) . . ? C10 Pd1 Pd2 105.92(9) . . ? N2 Pd1 Pd2 113.50(7) . . ? O1 Pd1 Pd2 76.74(7) . . ? O3 Pd1 Pd2 73.65(6) . . ? C40 Pd2 N32 87.52(11) . . ? C40 Pd2 O4 93.05(11) . . ? N32 Pd2 O4 172.48(10) . . ? C40 Pd2 O2 177.13(11) . . ? N32 Pd2 O2 94.54(9) . . ? O4 Pd2 O2 85.17(9) . . ? C40 Pd2 Pd1 98.24(9) . . ? N32 Pd2 Pd1 104.57(7) . . ? O4 Pd2 Pd1 82.78(6) . . ? O2 Pd2 Pd1 79.33(6) . . ? C61 O1 Pd1 127.3(2) . . ? C61 O2 Pd2 122.3(2) . . ? C63 O3 Pd1 130.0(2) . . ? C63 O4 Pd2 119.6(2) . . ? C1 N1 C9 126.8(3) . . ? C1 N1 C8 112.5(3) . . ? C9 N1 C8 120.6(2) . . ? C1 N2 C15 117.2(3) . . ? C1 N2 Pd1 127.5(2) . . ? C15 N2 Pd1 114.62(18) . . ? C31 N31 C39 123.3(2) . . ? C31 N31 C38 111.6(2) . . ? C39 N31 C38 123.2(2) . . ? C31 N32 C45 117.9(2) . . ? C31 N32 Pd2 123.9(2) . . ? C45 N32 Pd2 117.87(18) . . ? N2 C1 N1 123.5(3) . . ? N2 C1 C2 129.4(3) . . ? N1 C1 C2 107.1(2) . . ? C7 C2 C3 119.4(3) . . ? C7 C2 C1 107.6(3) . . ? C3 C2 C1 133.0(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C5 C4 C3 121.8(3) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 118.0(3) . . ? C7 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? C6 C7 C2 122.3(3) . . ? C6 C7 C8 127.6(3) . . ? C2 C7 C8 110.1(3) . . ? N1 C8 C7 102.7(2) . . ? N1 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? N1 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? C10 C9 C14 120.0(3) . . ? C10 C9 N1 123.1(3) . . ? C14 C9 N1 117.0(3) . . ? C9 C10 C11 117.1(3) . . ? C9 C10 Pd1 125.2(2) . . ? C11 C10 Pd1 117.6(2) . . ? C12 C11 C10 124.1(3) . . ? C12 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? C13 C12 C11 116.8(3) . . ? C13 C12 C21 121.8(3) . . ? C11 C12 C21 121.4(3) . . ? C12 C13 C14 121.8(3) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C16 C15 C20 120.0(3) . . ? C16 C15 N2 120.0(3) . . ? C20 C15 N2 119.9(3) . . ? C15 C16 C17 119.4(3) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 121.6(3) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 117.6(3) . . ? C19 C18 C22 121.1(3) . . ? C17 C18 C22 121.3(3) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C15 119.8(3) . . ? C19 C20 H20 120.1 . . ? C15 C20 H20 120.1 . . ? C12 C21 H21A 109.5 . . ? C12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N32 C31 N31 121.9(3) . . ? N32 C31 C32 130.7(3) . . ? N31 C31 C32 107.4(2) . . ? C37 C32 C33 120.0(3) . . ? C37 C32 C31 107.2(3) . . ? C33 C32 C31 132.7(3) . . ? C34 C33 C32 118.2(3) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 121.2(3) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 118.0(3) . . ? C35 C36 H36 121.0 . . ? C37 C36 H36 121.0 . . ? C36 C37 C32 121.5(3) . . ? C36 C37 C38 128.2(3) . . ? C32 C37 C38 110.2(3) . . ? N31 C38 C37 102.6(2) . . ? N31 C38 H38A 111.2 . . ? C37 C38 H38A 111.2 . . ? N31 C38 H38B 111.2 . . ? C37 C38 H38B 111.2 . . ? H38A C38 H38B 109.2 . . ? C44 C39 C40 119.7(3) . . ? C44 C39 N31 118.7(3) . . ? C40 C39 N31 121.5(3) . . ? C39 C40 C41 117.6(3) . . ? C39 C40 Pd2 121.3(2) . . ? C41 C40 Pd2 120.9(2) . . ? C42 C41 C40 123.3(3) . . ? C42 C41 H41 118.4 . . ? C40 C41 H41 118.4 . . ? C41 C42 C43 117.3(3) . . ? C41 C42 C51 121.6(3) . . ? C43 C42 C51 121.2(3) . . ? C44 C43 C42 121.3(3) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C39 120.8(3) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C50 C45 C46 119.6(3) . . ? C50 C45 N32 119.7(3) . . ? C46 C45 N32 120.7(3) . . ? C47 C46 C45 119.8(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 122.0(3) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C47 C48 C49 117.5(3) . . ? C47 C48 C52 120.5(3) . . ? C49 C48 C52 122.1(3) . . ? C50 C49 C48 121.3(3) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C45 C50 C49 119.8(3) . . ? C45 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C42 C51 H51A 109.5 . . ? C42 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C42 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52A 109.5 . . ? C48 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C48 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O2 C61 O1 126.2(3) . . ? O2 C61 C62 117.6(3) . . ? O1 C61 C62 116.1(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O3 C63 O4 126.8(3) . . ? O3 C63 C64 117.5(3) . . ? O4 C63 C64 115.7(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Cl1 C65 Cl3 110.3(2) . . ? Cl1 C65 Cl2 110.7(2) . . ? Cl3 C65 Cl2 110.0(2) . . ? Cl1 C65 H65 108.6 . . ? Cl3 C65 H65 108.6 . . ? Cl2 C65 H65 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 C10 Pd1 Pd2 C40 75.11(13) . . . . ? N2 Pd1 Pd2 C40 -22.02(12) . . . . ? O1 Pd1 Pd2 C40 163.14(11) . . . . ? O3 Pd1 Pd2 C40 -109.08(11) . . . . ? C10 Pd1 Pd2 N32 -14.46(12) . . . . ? N2 Pd1 Pd2 N32 -111.59(10) . . . . ? O1 Pd1 Pd2 N32 73.57(10) . . . . ? O3 Pd1 Pd2 N32 161.35(9) . . . . ? C10 Pd1 Pd2 O4 167.16(11) . . . . ? N2 Pd1 Pd2 O4 70.03(10) . . . . ? O1 Pd1 Pd2 O4 -104.81(9) . . . . ? O3 Pd1 Pd2 O4 -17.03(9) . . . . ? C10 Pd1 Pd2 O2 -106.43(11) . . . . ? N2 Pd1 Pd2 O2 156.45(10) . . . . ? O1 Pd1 Pd2 O2 -18.39(9) . . . . ? O3 Pd1 Pd2 O2 69.39(9) . . . . ? C10 Pd1 O1 C61 133.4(3) . . . . ? N2 Pd1 O1 C61 -127.8(5) . . . . ? O3 Pd1 O1 C61 -47.1(3) . . . . ? Pd2 Pd1 O1 C61 27.4(3) . . . . ? N32 Pd2 O2 C61 -83.3(3) . . . . ? O4 Pd2 O2 C61 104.2(3) . . . . ? Pd1 Pd2 O2 C61 20.7(2) . . . . ? N2 Pd1 O3 C63 -94.7(3) . . . . ? O1 Pd1 O3 C63 96.5(3) . . . . ? Pd2 Pd1 O3 C63 18.7(3) . . . . ? C40 Pd2 O4 C63 123.2(2) . . . . ? O2 Pd2 O4 C63 -54.6(2) . . . . ? Pd1 Pd2 O4 C63 25.3(2) . . . . ? C10 Pd1 N2 C1 20.7(3) . . . . ? O1 Pd1 N2 C1 -78.4(6) . . . . ? O3 Pd1 N2 C1 -158.1(3) . . . . ? Pd2 Pd1 N2 C1 128.1(2) . . . . ? C10 Pd1 N2 C15 -169.2(2) . . . . ? O1 Pd1 N2 C15 91.8(5) . . . . ? O3 Pd1 N2 C15 12.0(2) . . . . ? Pd2 Pd1 N2 C15 -61.8(2) . . . . ? C40 Pd2 N32 C31 -39.8(2) . . . . ? O2 Pd2 N32 C31 138.2(2) . . . . ? Pd1 Pd2 N32 C31 58.1(2) . . . . ? C40 Pd2 N32 C45 146.9(2) . . . . ? O2 Pd2 N32 C45 -35.1(2) . . . . ? Pd1 Pd2 N32 C45 -115.25(19) . . . . ? C15 N2 C1 N1 175.5(3) . . . . ? Pd1 N2 C1 N1 -14.6(4) . . . . ? C15 N2 C1 C2 -7.4(5) . . . . ? Pd1 N2 C1 C2 162.5(2) . . . . ? C9 N1 C1 N2 -5.9(5) . . . . ? C8 N1 C1 N2 178.6(3) . . . . ? C9 N1 C1 C2 176.4(3) . . . . ? C8 N1 C1 C2 0.9(3) . . . . ? N2 C1 C2 C7 -175.9(3) . . . . ? N1 C1 C2 C7 1.6(3) . . . . ? N2 C1 C2 C3 2.9(6) . . . . ? N1 C1 C2 C3 -179.6(3) . . . . ? C7 C2 C3 C4 1.7(5) . . . . ? C1 C2 C3 C4 -176.9(3) . . . . ? C2 C3 C4 C5 0.0(5) . . . . ? C3 C4 C5 C6 -1.6(6) . . . . ? C4 C5 C6 C7 1.4(5) . . . . ? C5 C6 C7 C2 0.3(5) . . . . ? C5 C6 C7 C8 -179.1(3) . . . . ? C3 C2 C7 C6 -1.9(5) . . . . ? C1 C2 C7 C6 177.1(3) . . . . ? C3 C2 C7 C8 177.6(3) . . . . ? C1 C2 C7 C8 -3.4(4) . . . . ? C1 N1 C8 C7 -2.8(4) . . . . ? C9 N1 C8 C7 -178.6(3) . . . . ? C6 C7 C8 N1 -176.7(3) . . . . ? C2 C7 C8 N1 3.8(4) . . . . ? C1 N1 C9 C10 13.2(5) . . . . ? C8 N1 C9 C10 -171.6(3) . . . . ? C1 N1 C9 C14 -167.5(3) . . . . ? C8 N1 C9 C14 7.6(5) . . . . ? C14 C9 C10 C11 1.0(5) . . . . ? N1 C9 C10 C11 -179.8(3) . . . . ? C14 C9 C10 Pd1 -178.4(3) . . . . ? N1 C9 C10 Pd1 0.9(5) . . . . ? N2 Pd1 C10 C9 -13.2(3) . . . . ? O1 Pd1 C10 C9 155.6(3) . . . . ? Pd2 Pd1 C10 C9 -127.7(3) . . . . ? N2 Pd1 C10 C11 167.5(2) . . . . ? O1 Pd1 C10 C11 -23.7(2) . . . . ? Pd2 Pd1 C10 C11 53.0(2) . . . . ? C9 C10 C11 C12 -1.5(5) . . . . ? Pd1 C10 C11 C12 177.9(3) . . . . ? C10 C11 C12 C13 1.5(5) . . . . ? C10 C11 C12 C21 -177.5(3) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? C21 C12 C13 C14 178.0(4) . . . . ? C12 C13 C14 C9 0.6(6) . . . . ? C10 C9 C14 C13 -0.6(6) . . . . ? N1 C9 C14 C13 -179.9(3) . . . . ? C1 N2 C15 C16 -87.5(4) . . . . ? Pd1 N2 C15 C16 101.3(3) . . . . ? C1 N2 C15 C20 91.5(3) . . . . ? Pd1 N2 C15 C20 -79.7(3) . . . . ? C20 C15 C16 C17 -2.3(4) . . . . ? N2 C15 C16 C17 176.7(3) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C16 C17 C18 C19 2.5(5) . . . . ? C16 C17 C18 C22 -176.4(3) . . . . ? C17 C18 C19 C20 -2.0(5) . . . . ? C22 C18 C19 C20 176.9(3) . . . . ? C18 C19 C20 C15 -0.7(5) . . . . ? C16 C15 C20 C19 2.9(4) . . . . ? N2 C15 C20 C19 -176.1(3) . . . . ? C45 N32 C31 N31 -171.6(3) . . . . ? Pd2 N32 C31 N31 15.1(4) . . . . ? C45 N32 C31 C32 10.8(5) . . . . ? Pd2 N32 C31 C32 -162.6(2) . . . . ? C39 N31 C31 N32 27.1(4) . . . . ? C38 N31 C31 N32 -167.8(3) . . . . ? C39 N31 C31 C32 -154.7(3) . . . . ? C38 N31 C31 C32 10.3(3) . . . . ? N32 C31 C32 C37 169.5(3) . . . . ? N31 C31 C32 C37 -8.4(3) . . . . ? N32 C31 C32 C33 -13.3(6) . . . . ? N31 C31 C32 C33 168.8(3) . . . . ? C37 C32 C33 C34 -1.5(5) . . . . ? C31 C32 C33 C34 -178.4(3) . . . . ? C32 C33 C34 C35 -1.5(5) . . . . ? C33 C34 C35 C36 2.5(6) . . . . ? C34 C35 C36 C37 -0.4(6) . . . . ? C35 C36 C37 C32 -2.7(5) . . . . ? C35 C36 C37 C38 174.7(3) . . . . ? C33 C32 C37 C36 3.6(5) . . . . ? C31 C32 C37 C36 -178.7(3) . . . . ? C33 C32 C37 C38 -174.2(3) . . . . ? C31 C32 C37 C38 3.5(3) . . . . ? C31 N31 C38 C37 -7.9(3) . . . . ? C39 N31 C38 C37 157.1(3) . . . . ? C36 C37 C38 N31 -175.3(3) . . . . ? C32 C37 C38 N31 2.3(3) . . . . ? C31 N31 C39 C44 146.9(3) . . . . ? C38 N31 C39 C44 -16.4(4) . . . . ? C31 N31 C39 C40 -28.6(4) . . . . ? C38 N31 C39 C40 168.1(3) . . . . ? C44 C39 C40 C41 -3.3(4) . . . . ? N31 C39 C40 C41 172.2(3) . . . . ? C44 C39 C40 Pd2 172.1(2) . . . . ? N31 C39 C40 Pd2 -12.5(4) . . . . ? N32 Pd2 C40 C39 36.5(2) . . . . ? O4 Pd2 C40 C39 -151.0(2) . . . . ? Pd1 Pd2 C40 C39 -67.9(2) . . . . ? N32 Pd2 C40 C41 -148.3(3) . . . . ? O4 Pd2 C40 C41 24.2(3) . . . . ? Pd1 Pd2 C40 C41 107.3(2) . . . . ? C39 C40 C41 C42 1.9(5) . . . . ? Pd2 C40 C41 C42 -173.4(2) . . . . ? C40 C41 C42 C43 0.3(5) . . . . ? C40 C41 C42 C51 179.5(3) . . . . ? C41 C42 C43 C44 -1.2(5) . . . . ? C51 C42 C43 C44 179.6(3) . . . . ? C42 C43 C44 C39 -0.2(5) . . . . ? C40 C39 C44 C43 2.5(5) . . . . ? N31 C39 C44 C43 -173.1(3) . . . . ? C31 N32 C45 C50 84.8(4) . . . . ? Pd2 N32 C45 C50 -101.5(3) . . . . ? C31 N32 C45 C46 -94.2(4) . . . . ? Pd2 N32 C45 C46 79.6(3) . . . . ? C50 C45 C46 C47 -0.3(5) . . . . ? N32 C45 C46 C47 178.7(3) . . . . ? C45 C46 C47 C48 -0.4(5) . . . . ? C46 C47 C48 C49 0.2(5) . . . . ? C46 C47 C48 C52 -179.1(4) . . . . ? C47 C48 C49 C50 0.8(5) . . . . ? C52 C48 C49 C50 -180.0(4) . . . . ? C46 C45 C50 C49 1.2(5) . . . . ? N32 C45 C50 C49 -177.8(3) . . . . ? C48 C49 C50 C45 -1.5(5) . . . . ? Pd2 O2 C61 O1 -8.7(5) . . . . ? Pd2 O2 C61 C62 169.1(2) . . . . ? Pd1 O1 C61 O2 -21.4(5) . . . . ? Pd1 O1 C61 C62 160.7(2) . . . . ? Pd1 O3 C63 O4 -5.4(5) . . . . ? Pd1 O3 C63 C64 173.8(2) . . . . ? Pd2 O4 C63 O3 -21.5(4) . . . . ? Pd2 O4 C63 C64 159.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.221 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.102 _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Crystallogr. 32, 115-119. Bruker-AXS (2000). SHELXTL 6.10. Bruker-AXS, Madison, USA. Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands. Osborne, A. G. & Whiteley, R. H. (1975). J. Organomet. Chem. 101, C27-C28. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology , Vol. 276, Macromolecular Crystallography, Part A, edited by C.W. Carter & R.M. Sweet, London: Academic Press, pp. 307-326. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen. Germany. Spek, A. L. (2001). J. Applied Cryst, 36, 7-13. ; #===END data_1226 _database_code_depnum_ccdc_archive 'CCDC 687006' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H60 N4 O4 Pd2, C3 H6 O' _chemical_formula_sum 'C59 H66 N4 O5 Pd2' _chemical_formula_weight 1123.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.7107(2) _cell_length_b 19.1758(3) _cell_length_c 21.3745(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.8830(10) _cell_angle_gamma 90.00 _cell_volume 5377.44(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12603 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description chip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details 'Shelxtl 6.10 (Bruker-AXS, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 77135 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12313 _reflns_number_gt 9169 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 2003)' _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^+6.1477P] 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 SHELXL _refine_ls_extinction_coef 0.00130(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12313 _refine_ls_number_parameters 644 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.083228(19) 0.306371(12) 0.111811(12) 0.02220(7) Uani 1 1 d . . . Pd2 Pd 0.037827(19) 0.430524(12) 0.192956(11) 0.02292(8) Uani 1 1 d . . . O1 O 0.19809(18) 0.37177(11) 0.10443(11) 0.0277(5) Uani 1 1 d . . . O2 O 0.18166(18) 0.45305(12) 0.17638(11) 0.0289(5) Uani 1 1 d . . . C61 C 0.2257(2) 0.42545(16) 0.13930(15) 0.0237(7) Uani 1 1 d . . . C62 C 0.3246(3) 0.4580(2) 0.13607(19) 0.0387(9) Uani 1 1 d . . . H62A H 0.3200 0.5088 0.1388 0.058 Uiso 1 1 calc R . . H62B H 0.3372 0.4452 0.0947 0.058 Uiso 1 1 calc R . . H62C H 0.3807 0.4409 0.1726 0.058 Uiso 1 1 calc R . . O3 O -0.02161(18) 0.37355(12) 0.04489(11) 0.0285(5) Uani 1 1 d . . . O4 O -0.02801(19) 0.47154(12) 0.10163(11) 0.0303(5) Uani 1 1 d . . . C63 C -0.0510(3) 0.43412(17) 0.04987(15) 0.0254(7) Uani 1 1 d . . . C64 C -0.1237(3) 0.4667(2) -0.00929(17) 0.0352(8) Uani 1 1 d . . . H64A H -0.1029 0.4549 -0.0482 0.053 Uiso 1 1 calc R . . H64B H -0.1230 0.5174 -0.0039 0.053 Uiso 1 1 calc R . . H64C H -0.1927 0.4490 -0.0144 0.053 Uiso 1 1 calc R . . N1 N 0.0727(2) 0.18351(14) 0.21508(13) 0.0266(6) Uani 1 1 d . . . N2 N -0.0255(2) 0.24076(13) 0.12099(13) 0.0243(6) Uani 1 1 d . . . C1 C -0.0188(3) 0.20122(16) 0.17143(16) 0.0244(7) Uani 1 1 d . . . C2 C -0.0998(3) 0.16898(17) 0.19463(18) 0.0312(8) Uani 1 1 d . . . C3 C -0.2055(3) 0.1685(2) 0.1691(2) 0.0429(10) Uani 1 1 d . . . H3 H -0.2383 0.1908 0.1288 0.051 Uiso 1 1 calc R . . C4 C -0.2612(3) 0.1344(2) 0.2045(3) 0.0573(13) Uani 1 1 d . . . H4 H -0.3335 0.1335 0.1880 0.069 Uiso 1 1 calc R . . C5 C -0.2147(3) 0.1016(2) 0.2632(2) 0.0530(12) Uani 1 1 d . . . H5 H -0.2552 0.0785 0.2861 0.064 Uiso 1 1 calc R . . C6 C -0.1099(3) 0.10198(19) 0.2888(2) 0.0432(10) Uani 1 1 d . . . H6 H -0.0776 0.0801 0.3295 0.052 Uiso 1 1 calc R . . C7 C -0.0533(3) 0.13540(17) 0.25343(18) 0.0327(8) Uani 1 1 d . . . C8 C 0.0596(3) 0.13987(18) 0.26843(17) 0.0314(8) Uani 1 1 d . . . H8A H 0.0905 0.1620 0.3115 0.038 Uiso 1 1 calc R . . H8B H 0.0901 0.0932 0.2680 0.038 Uiso 1 1 calc R . . C9 C 0.1692(2) 0.19034(17) 0.20409(15) 0.0253(7) Uani 1 1 d . . . C10 C 0.1855(2) 0.23893(17) 0.15932(15) 0.0246(7) Uani 1 1 d . . . C11 C 0.2813(3) 0.23906(18) 0.14802(17) 0.0294(7) Uani 1 1 d . . . H11 H 0.2925 0.2706 0.1165 0.035 Uiso 1 1 calc R . . C12 C 0.3606(3) 0.19523(19) 0.18072(18) 0.0333(8) Uani 1 1 d . . . C13 C 0.3426(3) 0.1496(2) 0.22652(17) 0.0355(8) Uani 1 1 d . . . H13 H 0.3960 0.1200 0.2503 0.043 Uiso 1 1 calc R . . C14 C 0.2493(3) 0.14632(19) 0.23834(17) 0.0339(8) Uani 1 1 d . . . H14 H 0.2388 0.1143 0.2697 0.041 Uiso 1 1 calc R . . C15 C -0.1224(2) 0.24664(16) 0.07139(16) 0.0244(7) Uani 1 1 d . . . C16 C -0.1902(3) 0.29945(17) 0.07427(17) 0.0302(8) Uani 1 1 d . . . H16 H -0.1750 0.3310 0.1101 0.036 Uiso 1 1 calc R . . C17 C -0.2808(3) 0.30565(18) 0.02410(18) 0.0353(8) Uani 1 1 d . . . H17 H -0.3274 0.3415 0.0263 0.042 Uiso 1 1 calc R . . C18 C -0.3049(3) 0.26077(19) -0.02925(17) 0.0317(8) Uani 1 1 d . . . C19 C -0.2357(3) 0.20834(19) -0.03041(17) 0.0329(8) Uani 1 1 d . . . H19 H -0.2510 0.1765 -0.0660 0.039 Uiso 1 1 calc R . . C20 C -0.1455(3) 0.20120(17) 0.01857(17) 0.0280(7) Uani 1 1 d . . . H20 H -0.0990 0.1652 0.0162 0.034 Uiso 1 1 calc R . . C21 C 0.4640(3) 0.1983(2) 0.1683(2) 0.0440(10) Uani 1 1 d . . . H21 H 0.5052 0.1584 0.1923 0.053 Uiso 1 1 calc R . . C22 C 0.4553(4) 0.1891(4) 0.0964(2) 0.083(2) Uani 1 1 d . . . H22A H 0.4142 0.1477 0.0795 0.124 Uiso 1 1 calc R . . H22B H 0.5235 0.1835 0.0911 0.124 Uiso 1 1 calc R . . H22C H 0.4225 0.2303 0.0720 0.124 Uiso 1 1 calc R . . C23 C 0.5211(4) 0.2650(3) 0.1951(4) 0.087(2) Uani 1 1 d . . . H23A H 0.4831 0.3053 0.1722 0.131 Uiso 1 1 calc R . . H23B H 0.5889 0.2639 0.1885 0.131 Uiso 1 1 calc R . . H23C H 0.5281 0.2688 0.2419 0.131 Uiso 1 1 calc R . . C24 C -0.4010(3) 0.2712(2) -0.0856(2) 0.0434(10) Uani 1 1 d . . . H24 H -0.4050 0.2322 -0.1173 0.052 Uiso 1 1 calc R . . C25 C -0.4970(3) 0.2691(3) -0.0642(2) 0.0601(13) Uani 1 1 d . . . H25A H -0.4942 0.3059 -0.0319 0.090 Uiso 1 1 calc R . . H25B H -0.5025 0.2235 -0.0446 0.090 Uiso 1 1 calc R . . H25C H -0.5565 0.2765 -0.1022 0.090 Uiso 1 1 calc R . . C26 C -0.3956(5) 0.3394(3) -0.1212(3) 0.092(2) Uani 1 1 d . . . H26A H -0.4584 0.3455 -0.1571 0.138 Uiso 1 1 calc R . . H26B H -0.3371 0.3381 -0.1388 0.138 Uiso 1 1 calc R . . H26C H -0.3877 0.3785 -0.0905 0.138 Uiso 1 1 calc R . . N31 N -0.0459(2) 0.34280(15) 0.29937(13) 0.0302(6) Uani 1 1 d . . . N32 N 0.1021(2) 0.39077(14) 0.28229(13) 0.0261(6) Uani 1 1 d . . . C31 C 0.0571(3) 0.34981(17) 0.31426(15) 0.0269(7) Uani 1 1 d . . . C32 C 0.1029(3) 0.30184(18) 0.36947(16) 0.0310(8) Uani 1 1 d . . . C33 C 0.2041(3) 0.2847(2) 0.40245(18) 0.0407(9) Uani 1 1 d . . . H33 H 0.2592 0.3085 0.3933 0.049 Uiso 1 1 calc R . . C34 C 0.2216(4) 0.2320(2) 0.44876(19) 0.0483(11) Uani 1 1 d . . . H34 H 0.2897 0.2189 0.4709 0.058 Uiso 1 1 calc R . . C35 C 0.1420(4) 0.1981(2) 0.46356(18) 0.0474(11) Uani 1 1 d . . . H35 H 0.1563 0.1626 0.4960 0.057 Uiso 1 1 calc R . . C36 C 0.0424(4) 0.2150(2) 0.43200(19) 0.0459(10) Uani 1 1 d . . . H36 H -0.0124 0.1915 0.4418 0.055 Uiso 1 1 calc R . . C37 C 0.0245(3) 0.26759(19) 0.38519(17) 0.0358(8) Uani 1 1 d . . . C38 C -0.0755(3) 0.29441(19) 0.34402(18) 0.0356(8) Uani 1 1 d . . . H38A H -0.1187 0.2562 0.3197 0.043 Uiso 1 1 calc R . . H38B H -0.1127 0.3190 0.3709 0.043 Uiso 1 1 calc R . . C39 C -0.1206(3) 0.38377(18) 0.25485(16) 0.0303(8) Uani 1 1 d . . . C40 C -0.0967(3) 0.42651(17) 0.20810(15) 0.0260(7) Uani 1 1 d . . . C41 C -0.1762(3) 0.46714(17) 0.16884(16) 0.0275(7) Uani 1 1 d . . . H41 H -0.1610 0.4977 0.1380 0.033 Uiso 1 1 calc R . . C42 C -0.2756(3) 0.46539(19) 0.17231(17) 0.0330(8) Uani 1 1 d . . . C43 C -0.2963(3) 0.4212(2) 0.2187(2) 0.0456(10) Uani 1 1 d . . . H43 H -0.3636 0.4187 0.2223 0.055 Uiso 1 1 calc R . . C44 C -0.2208(3) 0.3812(2) 0.2591(2) 0.0427(10) Uani 1 1 d . . . H44 H -0.2367 0.3514 0.2904 0.051 Uiso 1 1 calc R . . C45 C 0.2108(3) 0.40158(18) 0.30782(16) 0.0298(8) Uani 1 1 d . . . C46 C 0.2779(3) 0.3599(2) 0.28735(18) 0.0360(8) Uani 1 1 d . . . H46 H 0.2526 0.3233 0.2570 0.043 Uiso 1 1 calc R . . C47 C 0.3812(3) 0.3711(2) 0.31067(19) 0.0443(10) Uani 1 1 d . . . H47 H 0.4261 0.3418 0.2960 0.053 Uiso 1 1 calc R . . C48 C 0.4211(3) 0.4232(2) 0.3545(2) 0.0488(11) Uani 1 1 d . . . C49 C 0.3541(4) 0.4649(2) 0.3747(2) 0.0554(12) Uani 1 1 d . . . H49 H 0.3804 0.5015 0.4048 0.067 Uiso 1 1 calc R . . C50 C 0.2475(3) 0.4546(2) 0.35184(19) 0.0433(10) Uani 1 1 d . . . H50 H 0.2023 0.4836 0.3665 0.052 Uiso 1 1 calc R . . C51 C -0.3626(3) 0.5077(2) 0.12736(19) 0.0399(9) Uani 1 1 d . . . H51 H -0.3969 0.5334 0.1558 0.048 Uiso 1 1 calc R . . C52 C -0.3285(3) 0.5614(2) 0.0860(2) 0.0524(11) Uani 1 1 d . . . H52A H -0.2788 0.5929 0.1145 0.079 Uiso 1 1 calc R . . H52B H -0.3876 0.5882 0.0606 0.079 Uiso 1 1 calc R . . H52C H -0.2970 0.5376 0.0561 0.079 Uiso 1 1 calc R . . C53 C -0.4414(3) 0.4588(2) 0.0840(2) 0.0542(11) Uani 1 1 d . . . H53A H -0.5026 0.4853 0.0614 0.081 Uiso 1 1 calc R . . H53B H -0.4594 0.4225 0.1110 0.081 Uiso 1 1 calc R . . H53C H -0.4130 0.4370 0.0516 0.081 Uiso 1 1 calc R . . C54 C 0.5363(4) 0.4362(3) 0.3767(3) 0.0700(15) Uani 1 1 d . . . H54 H 0.5680 0.3928 0.3654 0.084 Uiso 1 1 calc R . . C55 C 0.5638(5) 0.4931(3) 0.3372(3) 0.090(2) Uani 1 1 d . . . H55A H 0.5382 0.5377 0.3484 0.135 Uiso 1 1 calc R . . H55B H 0.5332 0.4834 0.2906 0.135 Uiso 1 1 calc R . . H55C H 0.6381 0.4954 0.3468 0.135 Uiso 1 1 calc R . . C56 C 0.5793(4) 0.4447(3) 0.4485(3) 0.0782(17) Uani 1 1 d . . . H56A H 0.6539 0.4455 0.4600 0.117 Uiso 1 1 calc R . . H56B H 0.5576 0.4057 0.4708 0.117 Uiso 1 1 calc R . . H56C H 0.5549 0.4886 0.4621 0.117 Uiso 1 1 calc R . . O71 O 0.1222(4) -0.0487(2) 0.0545(2) 0.1048(16) Uani 1 1 d . . . C71 C 0.1493(5) 0.0720(3) 0.0458(3) 0.0837(18) Uani 1 1 d . . . H71A H 0.1900 0.0572 0.0173 0.126 Uiso 1 1 calc R . . H71B H 0.1925 0.0981 0.0830 0.126 Uiso 1 1 calc R . . H71C H 0.0931 0.1017 0.0212 0.126 Uiso 1 1 calc R . . C72 C 0.1074(4) 0.0097(3) 0.0700(3) 0.0629(14) Uani 1 1 d . . . C73 C 0.0450(5) 0.0223(3) 0.1159(3) 0.0825(18) Uani 1 1 d . . . H73A H 0.0152 -0.0218 0.1246 0.124 Uiso 1 1 calc R . . H73B H -0.0097 0.0555 0.0961 0.124 Uiso 1 1 calc R . . H73C H 0.0885 0.0416 0.1571 0.124 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 0.02266(14) 0.02112(13) 0.02219(13) 0.00140(9) 0.00552(9) 0.00109(10) Pd2 0.02476(14) 0.02378(13) 0.02032(13) 0.00092(10) 0.00667(10) 0.00084(10) O1 0.0306(14) 0.0261(12) 0.0285(12) -0.0001(10) 0.0118(10) -0.0029(10) O2 0.0307(14) 0.0291(12) 0.0294(12) -0.0006(10) 0.0124(10) -0.0012(10) C61 0.0207(17) 0.0242(16) 0.0260(16) 0.0066(13) 0.0065(13) 0.0009(13) C62 0.034(2) 0.040(2) 0.044(2) 0.0003(17) 0.0141(17) -0.0018(17) O3 0.0309(14) 0.0275(12) 0.0252(12) 0.0043(10) 0.0051(10) 0.0055(10) O4 0.0371(15) 0.0300(13) 0.0249(12) 0.0052(10) 0.0107(10) 0.0075(11) C63 0.0230(17) 0.0323(18) 0.0222(16) 0.0076(14) 0.0087(13) 0.0036(14) C64 0.034(2) 0.040(2) 0.0296(18) 0.0115(16) 0.0061(16) 0.0096(16) N1 0.0270(16) 0.0264(14) 0.0297(14) 0.0078(12) 0.0132(12) 0.0018(12) N2 0.0213(15) 0.0218(13) 0.0270(14) 0.0025(11) 0.0024(11) 0.0021(11) C1 0.0243(17) 0.0217(16) 0.0278(17) 0.0006(13) 0.0084(13) -0.0001(13) C2 0.0288(19) 0.0230(16) 0.044(2) 0.0062(15) 0.0143(16) 0.0031(14) C3 0.030(2) 0.038(2) 0.063(3) 0.0147(19) 0.0176(19) 0.0021(17) C4 0.033(2) 0.045(2) 0.103(4) 0.025(3) 0.034(3) 0.0068(19) C5 0.048(3) 0.037(2) 0.090(4) 0.026(2) 0.045(3) 0.0136(19) C6 0.052(3) 0.031(2) 0.057(3) 0.0137(18) 0.031(2) 0.0077(18) C7 0.038(2) 0.0232(17) 0.042(2) 0.0025(15) 0.0196(17) 0.0041(15) C8 0.034(2) 0.0308(18) 0.0310(18) 0.0073(15) 0.0115(15) 0.0049(15) C9 0.0217(17) 0.0285(17) 0.0240(16) 0.0014(13) 0.0039(13) 0.0006(13) C10 0.0224(17) 0.0265(16) 0.0222(16) -0.0007(13) 0.0022(13) -0.0021(13) C11 0.0272(19) 0.0309(18) 0.0313(18) 0.0037(14) 0.0102(15) 0.0021(14) C12 0.0236(18) 0.040(2) 0.0360(19) 0.0033(16) 0.0076(15) 0.0006(15) C13 0.026(2) 0.042(2) 0.0335(19) 0.0116(16) 0.0016(15) 0.0082(16) C14 0.029(2) 0.041(2) 0.0304(18) 0.0109(16) 0.0070(15) 0.0031(16) C15 0.0193(17) 0.0228(16) 0.0295(17) 0.0021(13) 0.0045(13) -0.0017(12) C16 0.0249(18) 0.0291(18) 0.0312(18) -0.0031(14) -0.0004(14) 0.0033(14) C17 0.0263(19) 0.0311(18) 0.043(2) 0.0008(16) 0.0014(16) 0.0080(15) C18 0.0246(19) 0.0357(19) 0.0314(18) 0.0018(15) 0.0027(15) -0.0039(15) C19 0.0258(19) 0.039(2) 0.0328(19) -0.0094(15) 0.0067(15) -0.0047(15) C20 0.0227(18) 0.0233(16) 0.0395(19) -0.0037(14) 0.0114(15) 0.0019(13) C21 0.027(2) 0.050(2) 0.058(3) 0.014(2) 0.0167(18) 0.0092(18) C22 0.049(3) 0.144(6) 0.063(3) 0.032(4) 0.029(3) 0.037(3) C23 0.039(3) 0.057(3) 0.171(7) -0.004(4) 0.040(4) -0.006(2) C24 0.031(2) 0.049(2) 0.041(2) 0.0029(18) -0.0051(17) -0.0008(18) C25 0.026(2) 0.073(3) 0.070(3) -0.011(3) -0.002(2) -0.001(2) C26 0.071(4) 0.096(4) 0.075(4) 0.041(3) -0.030(3) -0.018(3) N31 0.0311(17) 0.0346(16) 0.0269(15) 0.0052(12) 0.0118(13) -0.0004(13) N32 0.0266(16) 0.0284(15) 0.0227(14) 0.0001(11) 0.0063(11) -0.0035(12) C31 0.0285(19) 0.0304(18) 0.0218(16) 0.0024(13) 0.0073(14) 0.0002(14) C32 0.039(2) 0.0323(18) 0.0197(16) 0.0037(14) 0.0060(14) 0.0041(16) C33 0.042(2) 0.047(2) 0.0306(19) 0.0048(17) 0.0054(17) 0.0012(18) C34 0.055(3) 0.052(3) 0.034(2) 0.0107(19) 0.0063(19) 0.011(2) C35 0.070(3) 0.045(2) 0.028(2) 0.0141(17) 0.015(2) 0.011(2) C36 0.062(3) 0.047(2) 0.035(2) 0.0136(18) 0.024(2) 0.005(2) C37 0.045(2) 0.036(2) 0.0297(18) 0.0047(15) 0.0164(17) 0.0020(17) C38 0.038(2) 0.037(2) 0.037(2) 0.0110(16) 0.0189(17) -0.0003(16) C39 0.0297(19) 0.0325(18) 0.0280(17) -0.0015(14) 0.0073(15) -0.0023(15) C40 0.0286(19) 0.0275(17) 0.0220(15) -0.0042(13) 0.0076(13) -0.0014(14) C41 0.0295(19) 0.0251(17) 0.0277(17) -0.0038(14) 0.0080(14) 0.0020(14) C42 0.028(2) 0.0362(19) 0.0324(18) -0.0047(15) 0.0046(15) 0.0040(15) C43 0.026(2) 0.063(3) 0.051(2) 0.008(2) 0.0156(18) 0.0007(19) C44 0.030(2) 0.055(2) 0.046(2) 0.0127(19) 0.0148(18) -0.0022(18) C45 0.0261(19) 0.0351(19) 0.0245(17) 0.0058(14) 0.0015(14) -0.0031(15) C46 0.034(2) 0.040(2) 0.0321(19) 0.0013(16) 0.0065(16) 0.0028(16) C47 0.030(2) 0.060(3) 0.041(2) 0.008(2) 0.0058(17) 0.0048(19) C48 0.029(2) 0.055(3) 0.058(3) 0.010(2) 0.0044(19) -0.0045(19) C49 0.052(3) 0.048(3) 0.054(3) -0.012(2) -0.006(2) -0.019(2) C50 0.042(2) 0.044(2) 0.041(2) -0.0094(18) 0.0072(18) -0.0022(18) C51 0.034(2) 0.045(2) 0.039(2) -0.0019(17) 0.0081(17) 0.0107(17) C52 0.045(3) 0.047(2) 0.055(3) 0.011(2) -0.003(2) 0.007(2) C53 0.031(2) 0.066(3) 0.059(3) 0.005(2) 0.002(2) 0.000(2) C54 0.033(3) 0.067(3) 0.100(4) 0.002(3) 0.003(3) -0.004(2) C55 0.056(4) 0.109(5) 0.114(5) -0.014(4) 0.038(3) -0.033(3) C56 0.035(3) 0.102(4) 0.080(4) -0.016(3) -0.012(3) 0.001(3) O71 0.110(4) 0.060(2) 0.133(4) -0.045(3) 0.019(3) 0.021(2) C71 0.078(4) 0.080(4) 0.095(5) -0.016(3) 0.027(4) -0.006(3) C72 0.059(3) 0.057(3) 0.060(3) -0.016(2) -0.004(2) 0.010(2) C73 0.117(5) 0.057(3) 0.076(4) -0.004(3) 0.032(4) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C10 1.960(3) . ? Pd1 N2 2.004(3) . ? Pd1 O1 2.055(2) . ? Pd1 O3 2.139(2) . ? Pd1 Pd2 3.1130(3) . ? Pd2 C40 1.965(3) . ? Pd2 N32 2.006(3) . ? Pd2 O4 2.054(2) . ? Pd2 O2 2.146(2) . ? O1 C61 1.263(4) . ? O2 C61 1.245(4) . ? C61 C62 1.512(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O3 C63 1.244(4) . ? O4 C63 1.279(4) . ? C63 C64 1.500(4) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N1 C1 1.371(4) . ? N1 C9 1.415(4) . ? N1 C8 1.467(4) . ? N2 C1 1.299(4) . ? N2 C15 1.444(4) . ? C1 C2 1.477(5) . ? C2 C7 1.391(5) . ? C2 C3 1.392(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(6) . ? C4 H4 0.9500 . ? C5 C6 1.382(6) . ? C5 H5 0.9500 . ? C6 C7 1.388(5) . ? C6 H6 0.9500 . ? C7 C8 1.489(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.399(4) . ? C9 C14 1.410(5) . ? C10 C11 1.402(5) . ? C11 C12 1.392(5) . ? C11 H11 0.9500 . ? C12 C13 1.388(5) . ? C12 C21 1.516(5) . ? C13 C14 1.375(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.388(4) . ? C15 C16 1.388(5) . ? C16 C17 1.390(5) . ? C16 H16 0.9500 . ? C17 C18 1.390(5) . ? C17 H17 0.9500 . ? C18 C19 1.387(5) . ? C18 C24 1.518(5) . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.518(6) . ? C21 C23 1.524(7) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.515(6) . ? C24 C26 1.527(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N31 C31 1.360(4) . ? N31 C39 1.416(4) . ? N31 C38 1.471(4) . ? N32 C31 1.307(4) . ? N32 C45 1.446(4) . ? C31 C32 1.484(4) . ? C32 C37 1.381(5) . ? C32 C33 1.401(5) . ? C33 C34 1.385(5) . ? C33 H33 0.9500 . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.374(6) . ? C35 H35 0.9500 . ? C36 C37 1.391(5) . ? C36 H36 0.9500 . ? C37 C38 1.490(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.402(5) . ? C39 C44 1.405(5) . ? C40 C41 1.403(5) . ? C41 C42 1.387(5) . ? C41 H41 0.9500 . ? C42 C43 1.394(5) . ? C42 C51 1.529(5) . ? C43 C44 1.374(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.378(5) . ? C45 C46 1.383(5) . ? C46 C47 1.374(5) . ? C46 H46 0.9500 . ? C47 C48 1.370(6) . ? C47 H47 0.9500 . ? C48 C49 1.379(7) . ? C48 C54 1.532(6) . ? C49 C50 1.414(6) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.517(6) . ? C51 C53 1.525(6) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C56 1.485(7) . ? C54 C55 1.492(8) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? O71 C72 1.202(6) . ? C71 C72 1.482(8) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.497(8) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 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 C10 Pd1 N2 88.62(12) . . ? C10 Pd1 O1 89.63(11) . . ? N2 Pd1 O1 178.21(10) . . ? C10 Pd1 O3 169.79(11) . . ? N2 Pd1 O3 93.95(10) . . ? O1 Pd1 O3 87.84(9) . . ? C10 Pd1 Pd2 116.40(9) . . ? N2 Pd1 Pd2 98.67(8) . . ? O1 Pd1 Pd2 81.82(6) . . ? O3 Pd1 Pd2 73.01(6) . . ? C40 Pd2 N32 90.11(12) . . ? C40 Pd2 O4 89.83(12) . . ? N32 Pd2 O4 179.81(11) . . ? C40 Pd2 O2 170.63(11) . . ? N32 Pd2 O2 93.62(10) . . ? O4 Pd2 O2 86.41(9) . . ? C40 Pd2 Pd1 114.27(9) . . ? N32 Pd2 Pd1 97.83(8) . . ? O4 Pd2 Pd1 82.37(6) . . ? O2 Pd2 Pd1 73.74(6) . . ? C61 O1 Pd1 123.9(2) . . ? C61 O2 Pd2 131.2(2) . . ? O2 C61 O1 127.2(3) . . ? O2 C61 C62 117.5(3) . . ? O1 C61 C62 115.4(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C63 O3 Pd1 132.6(2) . . ? C63 O4 Pd2 122.5(2) . . ? O3 C63 O4 126.4(3) . . ? O3 C63 C64 118.0(3) . . ? O4 C63 C64 115.6(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C1 N1 C9 125.4(3) . . ? C1 N1 C8 112.1(3) . . ? C9 N1 C8 120.9(3) . . ? C1 N2 C15 118.9(3) . . ? C1 N2 Pd1 124.9(2) . . ? C15 N2 Pd1 115.6(2) . . ? N2 C1 N1 122.7(3) . . ? N2 C1 C2 130.1(3) . . ? N1 C1 C2 107.2(3) . . ? C7 C2 C3 120.1(3) . . ? C7 C2 C1 107.8(3) . . ? C3 C2 C1 132.0(3) . . ? C4 C3 C2 117.8(4) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C5 C4 C3 121.8(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 117.9(4) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C2 121.7(4) . . ? C6 C7 C8 128.3(3) . . ? C2 C7 C8 110.0(3) . . ? N1 C8 C7 102.7(3) . . ? N1 C8 H8A 111.2 . . ? C7 C8 H8A 111.2 . . ? N1 C8 H8B 111.2 . . ? C7 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? C10 C9 C14 119.9(3) . . ? C10 C9 N1 121.2(3) . . ? C14 C9 N1 118.9(3) . . ? C9 C10 C11 117.6(3) . . ? C9 C10 Pd1 124.1(2) . . ? C11 C10 Pd1 118.3(2) . . ? C12 C11 C10 123.2(3) . . ? C12 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C13 C12 C11 117.4(3) . . ? C13 C12 C21 121.0(3) . . ? C11 C12 C21 121.5(3) . . ? C14 C13 C12 121.7(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C20 C15 C16 119.8(3) . . ? C20 C15 N2 119.5(3) . . ? C16 C15 N2 120.6(3) . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 121.8(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 117.5(3) . . ? C19 C18 C24 121.4(3) . . ? C17 C18 C24 120.9(3) . . ? C20 C19 C18 121.8(3) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C15 119.9(3) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C12 C21 C22 111.8(4) . . ? C12 C21 C23 111.8(4) . . ? C22 C21 C23 111.0(5) . . ? C12 C21 H21 107.3 . . ? C22 C21 H21 107.3 . . ? C23 C21 H21 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C18 112.8(3) . . ? C25 C24 C26 110.2(4) . . ? C18 C24 C26 110.6(3) . . ? C25 C24 H24 107.7 . . ? C18 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 N31 C39 127.0(3) . . ? C31 N31 C38 112.0(3) . . ? C39 N31 C38 120.2(3) . . ? C31 N32 C45 118.7(3) . . ? C31 N32 Pd2 125.6(2) . . ? C45 N32 Pd2 115.1(2) . . ? N32 C31 N31 123.5(3) . . ? N32 C31 C32 129.3(3) . . ? N31 C31 C32 107.2(3) . . ? C37 C32 C33 119.5(3) . . ? C37 C32 C31 108.0(3) . . ? C33 C32 C31 132.4(3) . . ? C34 C33 C32 118.1(4) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C35 C34 C33 121.4(4) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 117.8(4) . . ? C35 C36 H36 121.1 . . ? C37 C36 H36 121.1 . . ? C32 C37 C36 122.2(4) . . ? C32 C37 C38 109.9(3) . . ? C36 C37 C38 127.9(4) . . ? N31 C38 C37 102.7(3) . . ? N31 C38 H38A 111.2 . . ? C37 C38 H38A 111.2 . . ? N31 C38 H38B 111.2 . . ? C37 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? C40 C39 C44 120.1(3) . . ? C40 C39 N31 122.0(3) . . ? C44 C39 N31 117.9(3) . . ? C39 C40 C41 116.7(3) . . ? C39 C40 Pd2 124.4(3) . . ? C41 C40 Pd2 118.9(2) . . ? C42 C41 C40 124.0(3) . . ? C42 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? C41 C42 C43 117.3(3) . . ? C41 C42 C51 123.6(3) . . ? C43 C42 C51 119.1(3) . . ? C44 C43 C42 121.0(4) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C39 120.8(4) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C50 C45 C46 119.9(4) . . ? C50 C45 N32 119.7(3) . . ? C46 C45 N32 120.4(3) . . ? C47 C46 C45 120.4(4) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 121.8(4) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C47 C48 C49 117.9(4) . . ? C47 C48 C54 120.1(4) . . ? C49 C48 C54 121.9(4) . . ? C48 C49 C50 121.8(4) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? C45 C50 C49 118.3(4) . . ? C45 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C52 C51 C53 110.3(3) . . ? C52 C51 C42 114.2(3) . . ? C53 C51 C42 110.0(3) . . ? C52 C51 H51 107.4 . . ? C53 C51 H51 107.4 . . ? C42 C51 H51 107.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C56 C54 C55 114.4(5) . . ? C56 C54 C48 113.8(5) . . ? C55 C54 C48 110.5(4) . . ? C56 C54 H54 105.8 . . ? C55 C54 H54 105.8 . . ? C48 C54 H54 105.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O71 C72 C71 122.7(6) . . ? O71 C72 C73 120.5(6) . . ? C71 C72 C73 116.8(5) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? 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 C10 Pd1 Pd2 C40 -109.36(15) . . . . ? N2 Pd1 Pd2 C40 -16.59(13) . . . . ? O1 Pd1 Pd2 C40 165.15(12) . . . . ? O3 Pd1 Pd2 C40 74.92(12) . . . . ? C10 Pd1 Pd2 N32 -15.68(13) . . . . ? N2 Pd1 Pd2 N32 77.09(11) . . . . ? O1 Pd1 Pd2 N32 -101.17(10) . . . . ? O3 Pd1 Pd2 N32 168.60(10) . . . . ? C10 Pd1 Pd2 O4 164.29(13) . . . . ? N2 Pd1 Pd2 O4 -102.94(10) . . . . ? O1 Pd1 Pd2 O4 78.81(10) . . . . ? O3 Pd1 Pd2 O4 -11.43(10) . . . . ? C10 Pd1 Pd2 O2 75.83(12) . . . . ? N2 Pd1 Pd2 O2 168.60(10) . . . . ? O1 Pd1 Pd2 O2 -9.66(9) . . . . ? O3 Pd1 Pd2 O2 -99.89(9) . . . . ? C10 Pd1 O1 C61 -103.2(3) . . . . ? O3 Pd1 O1 C61 86.7(2) . . . . ? Pd2 Pd1 O1 C61 13.6(2) . . . . ? N32 Pd2 O2 C61 108.8(3) . . . . ? O4 Pd2 O2 C61 -71.3(3) . . . . ? Pd1 Pd2 O2 C61 11.7(3) . . . . ? Pd2 O2 C61 O1 -5.9(5) . . . . ? Pd2 O2 C61 C62 175.7(2) . . . . ? Pd1 O1 C61 O2 -10.5(5) . . . . ? Pd1 O1 C61 C62 168.0(2) . . . . ? C10 Pd1 O3 C63 -144.8(6) . . . . ? N2 Pd1 O3 C63 110.9(3) . . . . ? O1 Pd1 O3 C63 -69.1(3) . . . . ? Pd2 Pd1 O3 C63 13.0(3) . . . . ? C40 Pd2 O4 C63 -97.8(3) . . . . ? O2 Pd2 O4 C63 90.8(3) . . . . ? Pd1 Pd2 O4 C63 16.7(2) . . . . ? Pd1 O3 C63 O4 -4.9(5) . . . . ? Pd1 O3 C63 C64 177.5(2) . . . . ? Pd2 O4 C63 O3 -14.2(5) . . . . ? Pd2 O4 C63 C64 163.5(2) . . . . ? C10 Pd1 N2 C1 35.4(3) . . . . ? O3 Pd1 N2 C1 -154.5(3) . . . . ? Pd2 Pd1 N2 C1 -81.1(3) . . . . ? C10 Pd1 N2 C15 -153.9(2) . . . . ? O3 Pd1 N2 C15 16.2(2) . . . . ? Pd2 Pd1 N2 C15 89.6(2) . . . . ? C15 N2 C1 N1 169.0(3) . . . . ? Pd1 N2 C1 N1 -20.6(4) . . . . ? C15 N2 C1 C2 -12.7(5) . . . . ? Pd1 N2 C1 C2 157.8(3) . . . . ? C9 N1 C1 N2 -16.1(5) . . . . ? C8 N1 C1 N2 178.6(3) . . . . ? C9 N1 C1 C2 165.2(3) . . . . ? C8 N1 C1 C2 0.0(4) . . . . ? N2 C1 C2 C7 -175.9(3) . . . . ? N1 C1 C2 C7 2.6(4) . . . . ? N2 C1 C2 C3 2.9(7) . . . . ? N1 C1 C2 C3 -178.6(4) . . . . ? C7 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C4 -178.1(4) . . . . ? C2 C3 C4 C5 -0.1(7) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C4 C5 C6 C7 -0.9(6) . . . . ? C5 C6 C7 C2 1.4(6) . . . . ? C5 C6 C7 C8 -176.4(4) . . . . ? C3 C2 C7 C6 -1.3(6) . . . . ? C1 C2 C7 C6 177.7(3) . . . . ? C3 C2 C7 C8 176.9(3) . . . . ? C1 C2 C7 C8 -4.1(4) . . . . ? C1 N1 C8 C7 -2.3(4) . . . . ? C9 N1 C8 C7 -168.4(3) . . . . ? C6 C7 C8 N1 -178.0(4) . . . . ? C2 C7 C8 N1 4.0(4) . . . . ? C1 N1 C9 C10 24.7(5) . . . . ? C8 N1 C9 C10 -171.2(3) . . . . ? C1 N1 C9 C14 -154.2(3) . . . . ? C8 N1 C9 C14 9.8(5) . . . . ? C14 C9 C10 C11 3.2(5) . . . . ? N1 C9 C10 C11 -175.7(3) . . . . ? C14 C9 C10 Pd1 -176.8(3) . . . . ? N1 C9 C10 Pd1 4.3(4) . . . . ? N2 Pd1 C10 C9 -26.1(3) . . . . ? O1 Pd1 C10 C9 153.5(3) . . . . ? O3 Pd1 C10 C9 -130.9(6) . . . . ? Pd2 Pd1 C10 C9 72.8(3) . . . . ? N2 Pd1 C10 C11 153.9(3) . . . . ? O1 Pd1 C10 C11 -26.5(3) . . . . ? O3 Pd1 C10 C11 49.1(8) . . . . ? Pd2 Pd1 C10 C11 -107.1(2) . . . . ? C9 C10 C11 C12 -2.3(5) . . . . ? Pd1 C10 C11 C12 177.6(3) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C10 C11 C12 C21 -178.4(3) . . . . ? C11 C12 C13 C14 1.5(6) . . . . ? C21 C12 C13 C14 180.0(4) . . . . ? C12 C13 C14 C9 -0.6(6) . . . . ? C10 C9 C14 C13 -1.9(5) . . . . ? N1 C9 C14 C13 177.1(3) . . . . ? C1 N2 C15 C20 -91.1(4) . . . . ? Pd1 N2 C15 C20 97.5(3) . . . . ? C1 N2 C15 C16 92.2(4) . . . . ? Pd1 N2 C15 C16 -79.1(3) . . . . ? C20 C15 C16 C17 0.4(5) . . . . ? N2 C15 C16 C17 177.0(3) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C16 C17 C18 C19 1.0(6) . . . . ? C16 C17 C18 C24 -176.2(4) . . . . ? C17 C18 C19 C20 -1.1(5) . . . . ? C24 C18 C19 C20 176.0(4) . . . . ? C18 C19 C20 C15 0.9(5) . . . . ? C16 C15 C20 C19 -0.5(5) . . . . ? N2 C15 C20 C19 -177.1(3) . . . . ? C13 C12 C21 C22 126.5(4) . . . . ? C11 C12 C21 C22 -55.1(5) . . . . ? C13 C12 C21 C23 -108.4(5) . . . . ? C11 C12 C21 C23 70.0(5) . . . . ? C19 C18 C24 C25 124.3(4) . . . . ? C17 C18 C24 C25 -58.7(5) . . . . ? C19 C18 C24 C26 -111.8(5) . . . . ? C17 C18 C24 C26 65.2(5) . . . . ? C40 Pd2 N32 C31 27.9(3) . . . . ? O2 Pd2 N32 C31 -160.7(3) . . . . ? Pd1 Pd2 N32 C31 -86.7(3) . . . . ? C40 Pd2 N32 C45 -161.2(2) . . . . ? O2 Pd2 N32 C45 10.3(2) . . . . ? Pd1 Pd2 N32 C45 84.3(2) . . . . ? C45 N32 C31 N31 171.5(3) . . . . ? Pd2 N32 C31 N31 -17.8(5) . . . . ? C45 N32 C31 C32 -10.8(5) . . . . ? Pd2 N32 C31 C32 159.9(3) . . . . ? C39 N31 C31 N32 -9.4(5) . . . . ? C38 N31 C31 N32 -178.9(3) . . . . ? C39 N31 C31 C32 172.5(3) . . . . ? C38 N31 C31 C32 3.0(4) . . . . ? N32 C31 C32 C37 -177.7(3) . . . . ? N31 C31 C32 C37 0.3(4) . . . . ? N32 C31 C32 C33 -1.7(6) . . . . ? N31 C31 C32 C33 176.3(4) . . . . ? C37 C32 C33 C34 1.8(5) . . . . ? C31 C32 C33 C34 -173.8(4) . . . . ? C32 C33 C34 C35 -1.5(6) . . . . ? C33 C34 C35 C36 0.8(7) . . . . ? C34 C35 C36 C37 -0.5(6) . . . . ? C33 C32 C37 C36 -1.5(6) . . . . ? C31 C32 C37 C36 175.1(3) . . . . ? C33 C32 C37 C38 -180.0(3) . . . . ? C31 C32 C37 C38 -3.4(4) . . . . ? C35 C36 C37 C32 0.8(6) . . . . ? C35 C36 C37 C38 179.0(4) . . . . ? C31 N31 C38 C37 -4.8(4) . . . . ? C39 N31 C38 C37 -175.1(3) . . . . ? C32 C37 C38 N31 4.9(4) . . . . ? C36 C37 C38 N31 -173.5(4) . . . . ? C31 N31 C39 C40 16.3(5) . . . . ? C38 N31 C39 C40 -175.0(3) . . . . ? C31 N31 C39 C44 -163.0(3) . . . . ? C38 N31 C39 C44 5.7(5) . . . . ? C44 C39 C40 C41 2.2(5) . . . . ? N31 C39 C40 C41 -177.0(3) . . . . ? C44 C39 C40 Pd2 -175.8(3) . . . . ? N31 C39 C40 Pd2 4.9(5) . . . . ? N32 Pd2 C40 C39 -20.6(3) . . . . ? O4 Pd2 C40 C39 159.6(3) . . . . ? Pd1 Pd2 C40 C39 78.0(3) . . . . ? N32 Pd2 C40 C41 161.3(3) . . . . ? O4 Pd2 C40 C41 -18.5(3) . . . . ? Pd1 Pd2 C40 C41 -100.0(2) . . . . ? C39 C40 C41 C42 -2.3(5) . . . . ? Pd2 C40 C41 C42 175.9(3) . . . . ? C40 C41 C42 C43 1.1(5) . . . . ? C40 C41 C42 C51 -177.4(3) . . . . ? C41 C42 C43 C44 0.1(6) . . . . ? C51 C42 C43 C44 178.7(4) . . . . ? C42 C43 C44 C39 0.0(7) . . . . ? C40 C39 C44 C43 -1.2(6) . . . . ? N31 C39 C44 C43 178.1(4) . . . . ? C31 N32 C45 C50 -88.7(4) . . . . ? Pd2 N32 C45 C50 99.6(3) . . . . ? C31 N32 C45 C46 92.6(4) . . . . ? Pd2 N32 C45 C46 -79.1(4) . . . . ? C50 C45 C46 C47 0.0(6) . . . . ? N32 C45 C46 C47 178.7(3) . . . . ? C45 C46 C47 C48 0.0(6) . . . . ? C46 C47 C48 C49 -0.2(6) . . . . ? C46 C47 C48 C54 -177.0(4) . . . . ? C47 C48 C49 C50 0.4(7) . . . . ? C54 C48 C49 C50 177.2(4) . . . . ? C46 C45 C50 C49 0.2(6) . . . . ? N32 C45 C50 C49 -178.5(3) . . . . ? C48 C49 C50 C45 -0.4(7) . . . . ? C41 C42 C51 C52 -9.9(5) . . . . ? C43 C42 C51 C52 171.6(4) . . . . ? C41 C42 C51 C53 114.7(4) . . . . ? C43 C42 C51 C53 -63.8(5) . . . . ? C47 C48 C54 C56 -133.5(5) . . . . ? C49 C48 C54 C56 49.9(7) . . . . ? C47 C48 C54 C55 96.2(6) . . . . ? C49 C48 C54 C55 -80.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.801 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.096 #===END