Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Coles, Simon J.' 'Danopoulos, Andreas' 'Hay-Motherwell, Robyn S.' 'Hursthouse, Michael B.' 'Motherwell, W.' 'Tizzard, Graham J.' 'Tulloch, Arran A. D.' _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Dr Andreas Danopoulos Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'AD1@SOTON.AC.UK' data_s92 _database_code_CSD 162457 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H45 Ag Cl9 N5 Pd' _chemical_formula_weight 1129.13 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' '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.559(2) _cell_length_b 42.043(8) _cell_length_c 10.631(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.51(3) _cell_angle_gamma 90.00 _cell_volume 4772.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ?28393 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5571 _exptl_absorpt_correction_T_max 0.9740 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28393 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10436 _reflns_number_gt 7019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10436 _refine_ls_number_parameters 581 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 4.156 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5696(4) 0.16143(10) 0.2695(4) 0.0264(9) Uani 1 1 d . . . C01' C 0.458(2) 0.1772(11) 0.668(2) 0.013(12) Uani 0.21(8) 1 d PU . . C01 C 0.4666(11) 0.1680(7) 0.6643(10) 0.062(3) Uani 0.79(8) 1 d PU . . C2 C -0.6701(4) 0.14754(10) 0.2918(4) 0.0301(10) Uani 1 1 d . . . C02 C 0.9616(6) 0.29270(17) 0.0668(6) 0.083(2) Uani 1 1 d . . . C3 C -0.6959(4) 0.11227(10) 0.2769(4) 0.0326(10) Uani 1 1 d . . . H3 H -0.6293 0.1022 0.2519 0.039 Uiso 1 1 calc R . . C03 C -0.0318(7) -0.00091(17) 0.7522(8) 0.089(2) Uani 1 1 d . . . C4 C -0.6899(8) 0.09740(16) 0.4079(6) 0.094(2) Uani 1 1 d . . . H4A H -0.7645 0.1034 0.4251 0.140 Uiso 1 1 calc R . . H4B H -0.6148 0.1049 0.4831 0.140 Uiso 1 1 calc R . . H4C H -0.6866 0.0742 0.4010 0.140 Uiso 1 1 calc R . . C5 C -0.8199(7) 0.10470(14) 0.1660(7) 0.123(4) Uani 1 1 d . . . H5A H -0.8334 0.0816 0.1616 0.184 Uiso 1 1 calc R . . H5B H -0.8204 0.1123 0.0786 0.184 Uiso 1 1 calc R . . H5C H -0.8869 0.1152 0.1853 0.184 Uiso 1 1 calc R . . C6 C -0.7494(4) 0.16792(11) 0.3243(4) 0.0365(11) Uani 1 1 d . . . H6 H -0.8183 0.1593 0.3406 0.044 Uiso 1 1 calc R . . C7 C -0.7304(4) 0.20019(12) 0.3332(4) 0.0404(11) Uani 1 1 d . . . H7 H -0.7856 0.2136 0.3561 0.049 Uiso 1 1 calc R . . C8 C -0.6318(4) 0.21317(11) 0.3093(4) 0.0392(11) Uani 1 1 d . . . H8 H -0.6202 0.2356 0.3147 0.047 Uiso 1 1 calc R . . C9 C -0.5477(4) 0.19391(11) 0.2769(4) 0.0345(10) Uani 1 1 d . . . C10 C -0.4417(5) 0.20858(11) 0.2465(5) 0.0442(12) Uani 1 1 d . . . H10 H -0.3806 0.1914 0.2510 0.053 Uiso 1 1 calc R . . C11 C -0.3724(5) 0.23415(12) 0.3501(5) 0.0524(13) Uani 1 1 d . . . H11A H -0.4274 0.2525 0.3395 0.079 Uiso 1 1 calc R . . H11B H -0.2974 0.2408 0.3349 0.079 Uiso 1 1 calc R . . H11C H -0.3477 0.2256 0.4424 0.079 Uiso 1 1 calc R . . C12 C -0.4894(6) 0.22282(14) 0.1034(5) 0.0704(17) Uani 1 1 d . . . H12A H -0.5240 0.2059 0.0361 0.106 Uiso 1 1 calc R . . H12B H -0.4200 0.2332 0.0881 0.106 Uiso 1 1 calc R . . H12C H -0.5548 0.2385 0.0942 0.106 Uiso 1 1 calc R . . C13 C -0.5157(4) 0.13676(10) 0.0884(4) 0.0360(11) Uani 1 1 d . . . H13 H -0.5767 0.1476 0.0141 0.043 Uiso 1 1 calc R . . C14 C -0.4363(4) 0.11430(11) 0.0804(4) 0.0366(11) Uani 1 1 d . . . H14 H -0.4299 0.1062 -0.0001 0.044 Uiso 1 1 calc R . . C15 C -0.3989(4) 0.12177(10) 0.3020(4) 0.0264(9) Uani 1 1 d . . . C16 C -0.2709(4) 0.08067(10) 0.2530(4) 0.0335(10) Uani 1 1 d . . . H16A H -0.1891 0.0902 0.3089 0.040 Uiso 1 1 calc R . . H16B H -0.2638 0.0713 0.1708 0.040 Uiso 1 1 calc R . . C17 C -0.3012(3) 0.05504(10) 0.3328(4) 0.0257(9) Uani 1 1 d . . . C18 C -0.3045(4) 0.02339(10) 0.2939(4) 0.0330(10) Uani 1 1 d . . . H18 H -0.2898 0.0180 0.2145 0.040 Uiso 1 1 calc R . . C19 C -0.3289(4) -0.00016(11) 0.3696(4) 0.0374(11) Uani 1 1 d . . . H19 H -0.3272 -0.0219 0.3464 0.045 Uiso 1 1 calc R . . C20 C -0.3560(4) 0.00861(10) 0.4802(4) 0.0320(10) Uani 1 1 d . . . H20 H -0.3752 -0.0071 0.5333 0.038 Uiso 1 1 calc R . . C21 C -0.3551(3) 0.04014(10) 0.5134(4) 0.0256(9) Uani 1 1 d . . . C22 C -0.3843(4) 0.05046(10) 0.6342(4) 0.0276(9) Uani 1 1 d . . . H22A H -0.4598 0.0641 0.6028 0.033 Uiso 1 1 calc R . . H22B H -0.4020 0.0315 0.6793 0.033 Uiso 1 1 calc R . . C23 C -0.2082(4) 0.05886(10) 0.8616(4) 0.0309(10) Uani 1 1 d . . . H23 H -0.2209 0.0405 0.9071 0.037 Uiso 1 1 calc R . . C24 C -0.1182(4) 0.08051(11) 0.9126(4) 0.0337(10) Uani 1 1 d . . . H24 H -0.0547 0.0806 1.0016 0.040 Uiso 1 1 calc R . . C25 C -0.2336(3) 0.09499(10) 0.6968(4) 0.0247(9) Uani 1 1 d . . . C26 C -0.0487(4) 0.12920(10) 0.8329(4) 0.0295(10) Uani 1 1 d . . . C27 C -0.0610(4) 0.15504(10) 0.9094(4) 0.0349(10) Uani 1 1 d . . . C28 C -0.1700(4) 0.15764(12) 0.9572(5) 0.0445(12) Uani 1 1 d . . . H28 H -0.2355 0.1419 0.9044 0.053 Uiso 1 1 calc R . . C29 C -0.1287(5) 0.14969(15) 1.1076(5) 0.0615(16) Uani 1 1 d . . . H29A H -0.1046 0.1272 1.1222 0.092 Uiso 1 1 calc R . . H29B H -0.1979 0.1537 1.1372 0.092 Uiso 1 1 calc R . . H29C H -0.0569 0.1630 1.1605 0.092 Uiso 1 1 calc R . . C30 C -0.2289(5) 0.19109(13) 0.9278(6) 0.0620(16) Uani 1 1 d . . . H30A H -0.1700 0.2066 0.9875 0.093 Uiso 1 1 calc R . . H30B H -0.3065 0.1913 0.9447 0.093 Uiso 1 1 calc R . . H30C H -0.2475 0.1967 0.8325 0.093 Uiso 1 1 calc R . . C31 C 0.0318(4) 0.17819(11) 0.9430(5) 0.0449(12) Uani 1 1 d . . . H31 H 0.0268 0.1961 0.9954 0.054 Uiso 1 1 calc R . . C32 C 0.1296(5) 0.17578(13) 0.9024(5) 0.0518(14) Uani 1 1 d . . . H32 H 0.1930 0.1916 0.9291 0.062 Uiso 1 1 calc R . . C33 C 0.1380(4) 0.15070(13) 0.8231(5) 0.0474(13) Uani 1 1 d . . . H33 H 0.2048 0.1498 0.7921 0.057 Uiso 1 1 calc R . . C34 C 0.0483(4) 0.12654(12) 0.7883(4) 0.0384(11) Uani 1 1 d . . . C35 C 0.0602(5) 0.09921(14) 0.7020(6) 0.0588(15) Uani 1 1 d . . . H35 H -0.0074 0.0836 0.6942 0.071 Uiso 1 1 calc R . . C36 C 0.0382(6) 0.11085(18) 0.5573(6) 0.089(2) Uani 1 1 d . . . H36A H -0.0457 0.1202 0.5158 0.133 Uiso 1 1 calc R . . H36B H 0.0452 0.0929 0.5021 0.133 Uiso 1 1 calc R . . H36C H 0.1010 0.1269 0.5619 0.133 Uiso 1 1 calc R . . C37 C 0.1885(5) 0.08184(16) 0.7716(8) 0.100(3) Uani 1 1 d . . . H37A H 0.1900 0.0628 0.7191 0.149 Uiso 1 1 calc R . . H37B H 0.1993 0.0757 0.8643 0.149 Uiso 1 1 calc R . . H37C H 0.2565 0.0962 0.7751 0.149 Uiso 1 1 calc R . . N1 N -0.4921(3) 0.14115(8) 0.2246(3) 0.0262(8) Uani 1 1 d . . . N2 N -0.3663(3) 0.10539(8) 0.2120(3) 0.0280(8) Uani 1 1 d . . . N3 N -0.3272(3) 0.06316(8) 0.4416(3) 0.0242(7) Uani 1 1 d . . . N4 N -0.2786(3) 0.06804(8) 0.7316(3) 0.0245(7) Uani 1 1 d . . . N5 N -0.1347(3) 0.10296(7) 0.8108(3) 0.0242(7) Uani 1 1 d . . . Cl1 Cl -0.29508(10) 0.16235(2) 0.56640(10) 0.0331(3) Uani 1 1 d . . . Pd1 Pd -0.31530(3) 0.110385(7) 0.50167(3) 0.02218(11) Uani 1 1 d . . . Cl2 Cl 0.35477(18) 0.19466(4) 0.70267(19) 0.0884(6) Uani 1 1 d . . . Cl3 Cl 0.47689(14) 0.13279(5) 0.74202(14) 0.0813(5) Uani 1 1 d . . . Cl4 Cl 1.0592(5) 0.26075(7) 0.1325(4) 0.0952(19) Uani 0.640(10) 1 d P . . Cl4' Cl 0.9625(14) 0.25914(15) 0.1698(8) 0.133(6) Uani 0.360(10) 1 d P . . Cl5 Cl 0.9486(3) 0.3023(2) -0.0993(3) 0.115(3) Uani 0.673(12) 1 d P . . Cl5' Cl 0.9834(12) 0.2762(4) -0.0843(15) 0.156(5) Uani 0.327(12) 1 d P . . Cl6 Cl 0.52513(11) 0.04197(3) 0.92079(11) 0.0377(3) Uani 1 1 d . . . Cl7 Cl 0.3136(11) 0.02639(11) 1.2120(10) 0.0472(17) Uani 0.71(3) 1 d P . . Cl7' Cl 0.255(3) 0.0224(2) 1.152(3) 0.050(4) Uani 0.29(3) 1 d P . . Cl8 Cl 0.0924(2) 0.00743(6) 0.8864(2) 0.0445(6) Uani 0.50 1 d P A 1 Cl9 Cl -0.0205(11) -0.0374(3) 0.6766(8) 0.0289(18) Uani 0.20 1 d P A 1 Cl9' Cl -0.0315(11) -0.0327(3) 0.6271(8) 0.081(3) Uani 0.30 1 d P A 1 Cl8A Cl -0.0239(4) 0.01707(10) 0.6337(5) 0.1170(16) Uani 0.50 1 d P A 2 Cl9A Cl 0.0138(4) -0.04255(9) 0.7620(6) 0.0922(14) Uani 0.50 1 d P A 2 Ag1 Ag 0.41755(4) 0.026519(10) 1.06132(4) 0.04962(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(2) 0.024(2) 0.021(2) -0.0006(17) 0.0065(17) 0.0053(19) C01' 0.014(12) 0.014(12) 0.013(12) 0.0000(10) 0.005(5) 0.0002(10) C01 0.063(3) 0.063(3) 0.062(3) 0.0001(10) 0.0244(15) 0.0003(10) C2 0.030(2) 0.027(2) 0.022(2) 0.0007(18) -0.0027(17) 0.006(2) C02 0.093(5) 0.077(5) 0.065(4) 0.004(4) 0.013(3) 0.024(4) C3 0.027(2) 0.030(2) 0.035(2) -0.001(2) 0.0067(19) -0.001(2) C03 0.088(5) 0.055(4) 0.137(6) -0.014(4) 0.057(5) 0.002(4) C4 0.168(7) 0.046(4) 0.074(4) 0.003(3) 0.053(5) -0.014(4) C5 0.114(6) 0.032(4) 0.113(6) -0.010(4) -0.079(5) 0.003(4) C6 0.028(2) 0.041(3) 0.038(3) -0.002(2) 0.0092(19) 0.008(2) C7 0.041(3) 0.038(3) 0.041(3) -0.003(2) 0.014(2) 0.015(2) C8 0.050(3) 0.025(2) 0.040(3) -0.001(2) 0.014(2) 0.008(2) C9 0.037(2) 0.029(3) 0.035(2) 0.002(2) 0.011(2) 0.007(2) C10 0.056(3) 0.024(3) 0.061(3) -0.001(2) 0.032(3) 0.000(2) C11 0.056(3) 0.029(3) 0.074(4) -0.005(3) 0.026(3) -0.010(2) C12 0.112(5) 0.052(4) 0.059(4) 0.006(3) 0.045(4) 0.000(4) C13 0.046(3) 0.028(3) 0.027(2) 0.0016(19) 0.006(2) 0.007(2) C14 0.050(3) 0.035(3) 0.023(2) 0.0020(19) 0.012(2) 0.006(2) C15 0.026(2) 0.024(2) 0.026(2) -0.0016(18) 0.0071(18) 0.0017(18) C16 0.035(2) 0.029(3) 0.038(2) 0.002(2) 0.016(2) 0.010(2) C17 0.0193(19) 0.024(2) 0.033(2) 0.0031(18) 0.0085(17) 0.0065(18) C18 0.030(2) 0.030(3) 0.034(2) -0.001(2) 0.0068(19) 0.009(2) C19 0.038(3) 0.022(2) 0.046(3) -0.006(2) 0.009(2) 0.005(2) C20 0.027(2) 0.018(2) 0.045(3) -0.0046(19) 0.007(2) -0.0034(18) C21 0.0139(18) 0.024(2) 0.033(2) -0.0004(18) 0.0024(16) -0.0018(17) C22 0.024(2) 0.023(2) 0.035(2) -0.0033(18) 0.0109(18) -0.0093(18) C23 0.038(2) 0.026(2) 0.028(2) 0.0083(19) 0.0118(19) 0.000(2) C24 0.033(2) 0.033(3) 0.028(2) 0.005(2) 0.0032(19) 0.003(2) C25 0.021(2) 0.022(2) 0.029(2) -0.0021(18) 0.0070(17) 0.0031(17) C26 0.022(2) 0.025(2) 0.030(2) -0.0001(18) -0.0033(17) -0.0047(18) C27 0.032(2) 0.020(2) 0.038(2) 0.0001(19) -0.0035(19) 0.0019(19) C28 0.038(3) 0.034(3) 0.051(3) -0.018(2) 0.005(2) -0.002(2) C29 0.056(3) 0.069(4) 0.062(4) -0.006(3) 0.026(3) 0.004(3) C30 0.057(3) 0.047(4) 0.067(4) -0.018(3) 0.008(3) 0.015(3) C31 0.042(3) 0.028(3) 0.047(3) -0.003(2) -0.003(2) -0.001(2) C32 0.038(3) 0.041(3) 0.059(3) 0.002(3) -0.002(2) -0.016(2) C33 0.033(3) 0.047(3) 0.053(3) 0.001(3) 0.005(2) -0.012(2) C34 0.027(2) 0.038(3) 0.041(3) -0.001(2) 0.002(2) -0.004(2) C35 0.033(3) 0.052(4) 0.092(4) -0.024(3) 0.024(3) -0.011(3) C36 0.083(5) 0.120(7) 0.079(5) -0.040(4) 0.049(4) -0.006(4) C37 0.040(3) 0.071(5) 0.178(8) -0.036(5) 0.032(4) 0.009(3) N1 0.0328(19) 0.0199(18) 0.0217(17) -0.0022(14) 0.0059(15) 0.0016(15) N2 0.0330(19) 0.026(2) 0.0245(18) 0.0035(15) 0.0105(15) 0.0057(16) N3 0.0213(17) 0.0217(19) 0.0271(18) -0.0016(15) 0.0062(14) 0.0017(14) N4 0.0261(17) 0.0207(18) 0.0266(18) -0.0020(14) 0.0100(14) -0.0046(15) N5 0.0257(18) 0.0179(18) 0.0231(17) 0.0007(14) 0.0026(14) 0.0001(14) Cl1 0.0377(6) 0.0187(5) 0.0359(6) -0.0017(4) 0.0061(5) -0.0009(5) Pd1 0.02139(17) 0.01813(17) 0.02476(18) -0.00001(13) 0.00633(13) 0.00033(13) Cl2 0.1099(13) 0.0818(12) 0.1059(13) -0.0356(10) 0.0776(11) -0.0376(11) Cl3 0.0697(10) 0.1250(16) 0.0447(8) 0.0160(9) 0.0170(7) -0.0020(10) Cl4 0.094(3) 0.0515(17) 0.108(2) -0.0162(16) 0.003(2) 0.0157(17) Cl4' 0.155(11) 0.062(4) 0.120(5) -0.033(4) -0.018(5) 0.012(4) Cl5 0.094(2) 0.182(7) 0.076(2) 0.019(2) 0.0384(16) -0.014(3) Cl5' 0.137(8) 0.128(11) 0.268(12) -0.067(8) 0.151(8) -0.048(7) Cl6 0.0460(6) 0.0313(6) 0.0419(6) -0.0073(5) 0.0238(5) -0.0058(5) Cl7 0.060(4) 0.0377(13) 0.057(3) 0.0094(15) 0.037(3) 0.0113(16) Cl7' 0.060(9) 0.037(3) 0.068(9) 0.010(4) 0.041(8) 0.006(4) Cl8 0.0337(12) 0.0552(17) 0.0427(13) 0.0078(12) 0.0126(10) 0.0120(12) Cl9 0.028(4) 0.030(4) 0.016(4) 0.009(4) -0.005(4) 0.010(3) Cl9' 0.064(4) 0.101(7) 0.063(6) -0.004(5) 0.007(5) 0.023(4) Cl8A 0.073(2) 0.078(3) 0.177(4) 0.047(3) 0.022(3) 0.006(2) Cl9A 0.078(3) 0.052(2) 0.173(5) 0.034(3) 0.077(3) 0.023(2) Ag1 0.0544(3) 0.0527(3) 0.0508(3) 0.00168(19) 0.0302(2) 0.0019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C9 1.386(6) . ? C1 C2 1.399(6) . ? C1 N1 1.445(5) . ? C01' Cl2 1.56(4) . ? C01' Cl3 2.00(4) . ? C01 Cl3 1.68(2) . ? C01 Cl2 1.87(3) . ? C2 C6 1.391(6) . ? C2 C3 1.509(6) . ? C02 Cl4 1.721(7) . ? C02 Cl5 1.761(7) . ? C02 Cl4' 1.784(12) . ? C02 Cl5' 1.853(11) . ? C3 C5 1.501(7) . ? C3 C4 1.504(7) . ? C03 Cl8A 1.501(8) . ? C03 Cl8 1.628(8) . ? C03 Cl9 1.760(13) . ? C03 Cl9A 1.820(8) . ? C03 Cl9' 1.886(13) . ? C6 C7 1.372(7) . ? C7 C8 1.372(6) . ? C8 C9 1.406(6) . ? C9 C10 1.513(6) . ? C10 C12 1.528(7) . ? C10 C11 1.528(6) . ? C13 C14 1.341(6) . ? C13 N1 1.379(5) . ? C14 N2 1.373(5) . ? C15 N2 1.345(5) . ? C15 N1 1.350(5) . ? C15 Pd1 2.025(4) . ? C16 N2 1.455(5) . ? C16 C17 1.493(6) . ? C17 N3 1.347(5) . ? C17 C18 1.389(6) . ? C18 C19 1.371(6) . ? C19 C20 1.378(6) . ? C20 C21 1.371(5) . ? C21 N3 1.346(5) . ? C21 C22 1.512(5) . ? C22 N4 1.464(5) . ? C23 C24 1.331(6) . ? C23 N4 1.364(5) . ? C24 N5 1.393(5) . ? C25 N5 1.351(5) . ? C25 N4 1.356(5) . ? C25 Pd1 2.029(4) . ? C26 C34 1.378(6) . ? C26 C27 1.397(6) . ? C26 N5 1.443(5) . ? C27 C31 1.391(6) . ? C27 C28 1.531(6) . ? C28 C29 1.521(7) . ? C28 C30 1.541(7) . ? C31 C32 1.359(7) . ? C32 C33 1.376(7) . ? C33 C34 1.396(6) . ? C34 C35 1.509(7) . ? C35 C36 1.539(8) . ? C35 C37 1.562(7) . ? N3 Pd1 2.074(3) . ? Cl1 Pd1 2.2756(11) . ? Cl4 Cl4' 1.323(13) . ? Cl4 Cl5' 2.226(18) . ? Cl5 Cl5' 1.158(13) . ? Cl6 Ag1 2.3712(12) . ? Cl7 Cl7' 0.75(2) . ? Cl7 Ag1 2.341(3) . ? Cl7' Ag1 2.422(9) . ? Cl9 Cl9' 0.529(10) . ? 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 C9 C1 C2 123.2(4) . . ? C9 C1 N1 118.5(4) . . ? C2 C1 N1 118.1(4) . . ? Cl2 C01' Cl3 108.9(12) . . ? Cl3 C01 Cl2 110.2(5) . . ? C6 C2 C1 117.0(4) . . ? C6 C2 C3 120.6(4) . . ? C1 C2 C3 122.4(4) . . ? Cl4 C02 Cl5 112.1(5) . . ? Cl4 C02 Cl4' 44.3(4) . . ? Cl5 C02 Cl4' 140.8(6) . . ? Cl4 C02 Cl5' 76.9(7) . . ? Cl5 C02 Cl5' 37.3(5) . . ? Cl4' C02 Cl5' 105.4(8) . . ? C5 C3 C4 109.3(5) . . ? C5 C3 C2 112.5(4) . . ? C4 C3 C2 112.0(4) . . ? Cl8A C03 Cl8 108.1(5) . . ? Cl8A C03 Cl9 90.9(5) . . ? Cl8 C03 Cl9 113.1(5) . . ? Cl8A C03 Cl9A 115.0(5) . . ? Cl8 C03 Cl9A 91.0(4) . . ? Cl9 C03 Cl9A 28.0(3) . . ? Cl8A C03 Cl9' 75.4(5) . . ? Cl8 C03 Cl9' 122.1(5) . . ? Cl9 C03 Cl9' 16.2(4) . . ? Cl9A C03 Cl9' 44.0(3) . . ? C7 C6 C2 121.6(4) . . ? C8 C7 C6 120.2(4) . . ? C7 C8 C9 121.2(4) . . ? C1 C9 C8 116.9(4) . . ? C1 C9 C10 122.4(4) . . ? C8 C9 C10 120.7(4) . . ? C9 C10 C12 111.1(4) . . ? C9 C10 C11 112.2(4) . . ? C12 C10 C11 109.4(4) . . ? C14 C13 N1 107.2(4) . . ? C13 C14 N2 106.1(4) . . ? N2 C15 N1 104.5(3) . . ? N2 C15 Pd1 118.3(3) . . ? N1 C15 Pd1 137.0(3) . . ? N2 C16 C17 111.8(3) . . ? N3 C17 C18 120.6(4) . . ? N3 C17 C16 118.9(4) . . ? C18 C17 C16 120.6(4) . . ? C19 C18 C17 120.4(4) . . ? C18 C19 C20 118.2(4) . . ? C21 C20 C19 119.8(4) . . ? N3 C21 C20 122.0(4) . . ? N3 C21 C22 117.1(4) . . ? C20 C21 C22 120.9(4) . . ? N4 C22 C21 110.4(3) . . ? C24 C23 N4 106.8(4) . . ? C23 C24 N5 107.1(4) . . ? N5 C25 N4 104.1(3) . . ? N5 C25 Pd1 137.8(3) . . ? N4 C25 Pd1 117.9(3) . . ? C34 C26 C27 122.8(4) . . ? C34 C26 N5 118.9(4) . . ? C27 C26 N5 118.1(4) . . ? C31 C27 C26 116.9(4) . . ? C31 C27 C28 121.1(4) . . ? C26 C27 C28 121.9(4) . . ? C29 C28 C27 111.5(4) . . ? C29 C28 C30 110.5(4) . . ? C27 C28 C30 110.7(4) . . ? C32 C31 C27 121.4(5) . . ? C31 C32 C33 120.9(5) . . ? C32 C33 C34 120.0(5) . . ? C26 C34 C33 117.9(4) . . ? C26 C34 C35 123.1(4) . . ? C33 C34 C35 118.9(4) . . ? C34 C35 C36 110.3(5) . . ? C34 C35 C37 111.0(4) . . ? C36 C35 C37 112.7(5) . . ? C15 N1 C13 110.5(3) . . ? C15 N1 C1 127.3(3) . . ? C13 N1 C1 121.9(3) . . ? C15 N2 C14 111.6(3) . . ? C15 N2 C16 122.6(3) . . ? C14 N2 C16 125.7(3) . . ? C21 N3 C17 119.0(4) . . ? C21 N3 Pd1 121.1(3) . . ? C17 N3 Pd1 119.8(3) . . ? C25 N4 C23 111.7(3) . . ? C25 N4 C22 122.2(3) . . ? C23 N4 C22 125.9(3) . . ? C25 N5 C24 110.2(3) . . ? C25 N5 C26 128.9(3) . . ? C24 N5 C26 120.8(3) . . ? C15 Pd1 C25 175.07(16) . . ? C15 Pd1 N3 87.41(14) . . ? C25 Pd1 N3 87.67(14) . . ? C15 Pd1 Cl1 92.44(12) . . ? C25 Pd1 Cl1 92.48(12) . . ? N3 Pd1 Cl1 177.78(9) . . ? C01' Cl2 C01 8.8(11) . . ? C01 Cl3 C01' 7.5(8) . . ? Cl4' Cl4 C02 70.3(4) . . ? Cl4' Cl4 Cl5' 106.4(4) . . ? C02 Cl4 Cl5' 54.2(4) . . ? Cl4 Cl4' C02 65.3(7) . . ? Cl5' Cl5 C02 75.7(6) . . ? Cl5 Cl5' C02 67.0(5) . . ? Cl5 Cl5' Cl4 113.4(7) . . ? C02 Cl5' Cl4 48.9(4) . . ? Cl7' Cl7 Ag1 87.2(7) . . ? Cl7 Cl7' Ag1 74.9(8) . . ? Cl9' Cl9 C03 96(2) . . ? Cl9 Cl9' C03 68(2) . . ? Cl7 Ag1 Cl6 164.12(15) . . ? Cl7 Ag1 Cl7' 17.9(5) . . ? Cl6 Ag1 Cl7' 160.7(5) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.943 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.112 data_00skl044 _database_code_CSD 162458 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H41 Cl4.50 N5 Pd1' _chemical_formula_sum 'C36 H41 Cl4.50 N5 Pd' _chemical_formula_weight 809.66 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4782(4) _cell_length_b 11.8790(6) _cell_length_c 20.8146(11) _cell_angle_alpha 75.077(3) _cell_angle_beta 83.364(3) _cell_angle_gamma 71.322(2) _cell_volume 1917.65(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14147 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 25.02 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 829 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9597 _exptl_absorpt_correction_T_max 0.9836 _exptl_absorpt_process_details ; SORTAV (Blessing, 1995-1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% n/a _diffrn_reflns_number 14147 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.1279 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6524 _reflns_number_gt 4241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1574P)^2^+7.8887P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6524 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.2213 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 14.249 _refine_ls_shift/su_mean 0.325 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 0.13863(10) 0.17003(6) 0.25573(3) 0.0289(3) Uani 1 1 d . . . Cl2 Cl -0.0231(3) 0.2130(2) 0.34717(11) 0.0365(6) Uani 1 1 d . . . N5 N 0.0813(10) -0.0936(7) 0.2972(4) 0.0278(17) Uani 1 1 d . . . N1 N 0.1644(10) 0.4430(7) 0.2269(4) 0.0322(19) Uani 1 1 d . . . N4 N 0.2318(10) -0.0493(7) 0.2106(4) 0.0295(18) Uani 1 1 d . . . N3 N 0.2775(9) 0.1346(7) 0.1761(3) 0.0269(17) Uani 1 1 d . . . N2 N 0.2842(10) 0.3289(7) 0.1614(4) 0.0318(19) Uani 1 1 d . . . C3 C 0.2244(13) -0.1644(9) 0.2126(5) 0.036(2) Uani 1 1 d . . . H3 H 0.2757 -0.2135 0.1819 0.043 Uiso 1 1 calc R . . C2 C 0.1300(12) -0.1927(8) 0.2667(5) 0.032(2) Uani 1 1 d . . . H2 H 0.1011 -0.2664 0.2818 0.039 Uiso 1 1 calc R . . C5 C 0.4036(12) -0.0038(9) 0.1084(4) 0.032(2) Uani 1 1 d . . . H5 H 0.4231 -0.0810 0.0986 0.039 Uiso 1 1 calc R . . C27 C -0.1242(16) 0.6004(10) 0.3762(5) 0.049(3) Uani 1 1 d . . . H27 H -0.1886 0.6400 0.4091 0.059 Uiso 1 1 calc R . . C16 C -0.0900(14) -0.1411(9) 0.4700(5) 0.041(3) Uani 1 1 d . . . H16 H -0.0543 -0.1802 0.5141 0.049 Uiso 1 1 calc R . . C17 C 0.0248(13) -0.1470(9) 0.4180(5) 0.036(2) Uani 1 1 d . . . C1 C 0.1416(12) -0.0030(8) 0.2629(4) 0.028(2) Uani 1 1 d . . . C10 C 0.2425(13) 0.5101(9) 0.1758(5) 0.039(2) Uani 1 1 d . . . H10 H 0.2407 0.5922 0.1709 0.047 Uiso 1 1 calc R . . C9 C 0.3208(14) 0.4374(9) 0.1346(5) 0.037(2) Uani 1 1 d . . . H9 H 0.3868 0.4563 0.0956 0.044 Uiso 1 1 calc R . . C26 C 0.0410(15) 0.5347(10) 0.3861(5) 0.043(3) Uani 1 1 d . . . H26 H 0.0876 0.5263 0.4271 0.051 Uiso 1 1 calc R . . C34 C 0.4152(15) 0.4875(11) 0.3691(6) 0.054(3) Uani 1 1 d . . . H34A H 0.4043 0.5629 0.3344 0.081 Uiso 1 1 calc R . . H34B H 0.5333 0.4406 0.3740 0.081 Uiso 1 1 calc R . . H34C H 0.3678 0.5080 0.4113 0.081 Uiso 1 1 calc R . . C24 C 0.0639(13) 0.4947(8) 0.2796(5) 0.034(2) Uani 1 1 d . . . C18 C -0.2593(13) 0.0436(9) 0.2723(5) 0.039(2) Uani 1 1 d . . . H18 H -0.1596 0.0534 0.2434 0.047 Uiso 1 1 calc R . . C25 C 0.1417(13) 0.4803(9) 0.3378(5) 0.034(2) Uani 1 1 d . . . C13 C -0.2004(13) -0.0204(9) 0.3414(5) 0.036(2) Uani 1 1 d . . . C21 C 0.2095(13) -0.2121(10) 0.4285(5) 0.039(2) Uani 1 1 d . . . H21 H 0.2545 -0.2531 0.3910 0.047 Uiso 1 1 calc R . . C15 C -0.2577(14) -0.0790(10) 0.4595(5) 0.042(3) Uani 1 1 d . . . H15 H -0.3354 -0.0764 0.4963 0.050 Uiso 1 1 calc R . . C30 C -0.1825(15) 0.5693(10) 0.2028(6) 0.047(3) Uani 1 1 d . . . H30 H -0.0943 0.5255 0.1738 0.056 Uiso 1 1 calc R . . C11 C 0.1901(12) 0.3306(8) 0.2175(4) 0.030(2) Uani 1 1 d . . . C12 C -0.0347(12) -0.0857(9) 0.3543(4) 0.030(2) Uani 1 1 d . . . C29 C -0.1032(13) 0.5578(9) 0.2677(5) 0.038(2) Uani 1 1 d . . . C14 C -0.3120(14) -0.0208(9) 0.3956(5) 0.041(3) Uani 1 1 d . . . H14 H -0.4274 0.0194 0.3889 0.049 Uiso 1 1 calc R . . C4 C 0.3074(13) 0.0271(8) 0.1621(4) 0.031(2) Uani 1 1 d . . . C22 C 0.2460(16) -0.3095(11) 0.4930(6) 0.056(3) Uani 1 1 d . . . H22A H 0.3666 -0.3475 0.4964 0.085 Uiso 1 1 calc R . . H22B H 0.1929 -0.3718 0.4934 0.085 Uiso 1 1 calc R . . H22C H 0.2019 -0.2720 0.5307 0.085 Uiso 1 1 calc R . . C35 C 0.3402(16) 0.2955(11) 0.4022(6) 0.054(3) Uani 1 1 d . . . H35A H 0.2825 0.2463 0.3887 0.081 Uiso 1 1 calc R . . H35B H 0.2906 0.3148 0.4445 0.081 Uiso 1 1 calc R . . H35C H 0.4584 0.2493 0.4077 0.081 Uiso 1 1 calc R . . C28 C -0.1966(15) 0.6084(10) 0.3174(6) 0.046(3) Uani 1 1 d . . . H28 H -0.3122 0.6495 0.3118 0.055 Uiso 1 1 calc R . . C33 C 0.3232(13) 0.4122(9) 0.3497(5) 0.040(2) Uani 1 1 d . . . H33 H 0.3763 0.3901 0.3073 0.048 Uiso 1 1 calc R . . C7 C 0.4356(14) 0.1995(10) 0.0816(5) 0.039(3) Uani 1 1 d . . . H7 H 0.4774 0.2609 0.0531 0.047 Uiso 1 1 calc R . . C23 C 0.3068(17) -0.1208(13) 0.4268(7) 0.066(4) Uani 1 1 d . . . H23A H 0.4251 -0.1656 0.4336 0.099 Uiso 1 1 calc R . . H23B H 0.2626 -0.0770 0.4621 0.099 Uiso 1 1 calc R . . H23C H 0.2944 -0.0621 0.3835 0.099 Uiso 1 1 calc R . . C20 C -0.3815(15) 0.1697(10) 0.2687(6) 0.051(3) Uani 1 1 d . . . H20A H -0.4161 0.2072 0.2227 0.077 Uiso 1 1 calc R . . H20B H -0.3283 0.2205 0.2832 0.077 Uiso 1 1 calc R . . H20C H -0.4794 0.1632 0.2977 0.077 Uiso 1 1 calc R . . C6 C 0.4718(13) 0.0845(9) 0.0687(4) 0.036(2) Uani 1 1 d . . . H6 H 0.5444 0.0656 0.0320 0.044 Uiso 1 1 calc R . . C19 C -0.3326(18) -0.0341(12) 0.2456(6) 0.064(4) Uani 1 1 d . . . H19A H -0.3697 0.0080 0.2003 0.096 Uiso 1 1 calc R . . H19B H -0.4278 -0.0485 0.2742 0.096 Uiso 1 1 calc R . . H19C H -0.2480 -0.1126 0.2447 0.096 Uiso 1 1 calc R . . Cl1 Cl 0.3729(4) 0.7272(2) 0.06897(12) 0.0458(7) Uani 1 1 d . . . C8 C 0.3386(13) 0.2210(9) 0.1364(4) 0.034(2) Uani 1 1 d . . . C31 C -0.250(2) 0.7020(12) 0.1652(7) 0.075(4) Uani 1 1 d . . . H31A H -0.1594 0.7394 0.1559 0.112 Uiso 1 1 calc R . . H31B H -0.3380 0.7464 0.1923 0.112 Uiso 1 1 calc R . . H31C H -0.2951 0.7055 0.1232 0.112 Uiso 1 1 calc R . . C32 C -0.320(2) 0.5098(14) 0.2160(8) 0.082(5) Uani 1 1 d . . . H32A H -0.2761 0.4241 0.2397 0.123 Uiso 1 1 calc R . . H32B H -0.3642 0.5139 0.1736 0.123 Uiso 1 1 calc R . . H32C H -0.4101 0.5529 0.2431 0.123 Uiso 1 1 calc R . . Cl42 Cl 0.6935(8) 0.5083(6) 0.0386(3) 0.0638(15) Uiso 0.50 1 d P . . Cl43 Cl 0.8629(9) 0.2772(7) 0.1087(3) 0.0759(18) Uiso 0.50 1 d P . . Cl40 Cl 0.9448(9) 0.0363(7) 0.0859(4) 0.0935(18) Uiso 0.50 1 d P . . Cl44 Cl 1.0783(10) 0.2309(7) 0.0037(4) 0.1000(19) Uiso 0.50 1 d P . . Cl41 Cl 1.0316(10) 0.4093(7) -0.0061(4) 0.1018(19) Uiso 0.50 1 d P . . C46 C 0.838(4) 0.376(3) 0.0299(17) 0.088(10) Uiso 0.50 1 d P . . C47 C 0.893(6) 0.203(4) 0.055(2) 0.136(15) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0379(5) 0.0248(4) 0.0268(4) -0.0059(3) 0.0025(3) -0.0148(3) Cl2 0.0503(16) 0.0334(13) 0.0321(12) -0.0122(10) 0.0111(11) -0.0221(12) N5 0.034(5) 0.023(4) 0.027(4) -0.006(3) -0.002(3) -0.011(3) N1 0.039(5) 0.024(4) 0.033(4) 0.001(3) -0.004(4) -0.014(4) N4 0.038(5) 0.029(4) 0.028(4) -0.008(3) -0.002(3) -0.018(4) N3 0.029(4) 0.024(4) 0.028(4) -0.005(3) 0.001(3) -0.011(3) N2 0.044(5) 0.027(4) 0.032(4) -0.004(3) -0.003(4) -0.022(4) C3 0.043(6) 0.035(5) 0.031(5) -0.014(4) 0.003(5) -0.010(5) C2 0.038(6) 0.022(5) 0.039(5) -0.007(4) 0.000(4) -0.012(4) C5 0.038(6) 0.031(5) 0.028(5) -0.007(4) 0.002(4) -0.012(5) C27 0.069(9) 0.038(6) 0.042(6) -0.013(5) 0.009(6) -0.021(6) C16 0.057(8) 0.034(6) 0.029(5) -0.005(4) 0.006(5) -0.013(5) C17 0.048(6) 0.033(5) 0.029(5) -0.002(4) -0.011(5) -0.016(5) C1 0.035(6) 0.028(5) 0.022(4) -0.004(4) 0.003(4) -0.016(4) C10 0.051(7) 0.030(5) 0.037(5) -0.001(4) 0.007(5) -0.022(5) C9 0.054(7) 0.034(6) 0.032(5) -0.010(4) 0.006(5) -0.028(5) C26 0.056(8) 0.040(6) 0.039(5) -0.009(5) -0.006(5) -0.023(6) C34 0.047(7) 0.045(7) 0.065(7) -0.012(6) -0.003(6) -0.009(6) C24 0.048(7) 0.022(5) 0.039(5) -0.011(4) 0.004(5) -0.021(5) C18 0.036(6) 0.040(6) 0.036(5) 0.000(5) 0.002(5) -0.011(5) C25 0.049(7) 0.027(5) 0.033(5) -0.009(4) 0.005(5) -0.020(5) C13 0.044(6) 0.028(5) 0.038(5) -0.004(4) -0.002(5) -0.015(5) C21 0.041(6) 0.044(6) 0.037(5) -0.008(5) -0.006(5) -0.018(5) C15 0.050(7) 0.046(6) 0.034(5) -0.014(5) 0.016(5) -0.024(6) C30 0.049(7) 0.040(6) 0.053(6) -0.011(5) -0.009(5) -0.014(5) C11 0.037(6) 0.027(5) 0.028(5) -0.001(4) -0.006(4) -0.016(4) C12 0.035(6) 0.030(5) 0.030(5) -0.008(4) 0.004(4) -0.018(4) C29 0.042(6) 0.026(5) 0.050(6) -0.009(5) -0.004(5) -0.016(5) C14 0.044(7) 0.034(6) 0.041(6) -0.002(5) 0.005(5) -0.016(5) C4 0.041(6) 0.030(5) 0.031(5) -0.008(4) 0.002(4) -0.020(5) C22 0.058(8) 0.057(8) 0.049(7) -0.009(6) -0.016(6) -0.008(6) C35 0.061(8) 0.048(7) 0.053(7) -0.004(6) -0.009(6) -0.021(6) C28 0.046(7) 0.036(6) 0.058(7) -0.011(5) 0.002(6) -0.016(5) C33 0.046(7) 0.041(6) 0.036(5) -0.013(5) -0.008(5) -0.014(5) C7 0.053(7) 0.041(6) 0.028(5) -0.005(4) 0.006(5) -0.025(5) C23 0.058(9) 0.071(9) 0.071(8) -0.005(7) -0.018(7) -0.028(7) C20 0.051(7) 0.040(6) 0.060(7) 0.000(6) -0.022(6) -0.012(5) C6 0.045(6) 0.046(6) 0.026(5) -0.013(4) 0.007(4) -0.023(5) C19 0.074(10) 0.056(8) 0.061(8) -0.019(7) -0.024(7) -0.007(7) Cl1 0.0650(19) 0.0399(15) 0.0372(13) -0.0077(11) 0.0094(12) -0.0273(14) C8 0.043(6) 0.031(5) 0.030(5) -0.004(4) -0.004(4) -0.015(5) C31 0.101(12) 0.051(8) 0.064(8) 0.002(7) -0.040(8) -0.011(8) C32 0.108(13) 0.078(10) 0.080(10) -0.008(8) -0.023(9) -0.057(10) _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 N3 1.975(7) . ? Pd1 C1 2.014(9) . ? Pd1 C11 2.033(9) . ? Pd1 Cl2 2.283(2) . ? N5 C1 1.342(11) . ? N5 C2 1.404(12) . ? N5 C12 1.456(12) . ? N1 C11 1.344(12) . ? N1 C10 1.395(12) . ? N1 C24 1.450(13) . ? N4 C3 1.379(12) . ? N4 C1 1.385(12) . ? N4 C4 1.416(11) . ? N3 C4 1.322(12) . ? N3 C8 1.345(12) . ? N2 C11 1.336(12) . ? N2 C9 1.384(12) . ? N2 C8 1.427(12) . ? C3 C2 1.338(13) . ? C3 H3 0.9500 . ? C2 H2 0.9500 . ? C5 C4 1.362(13) . ? C5 C6 1.396(13) . ? C5 H5 0.9500 . ? C27 C26 1.377(17) . ? C27 C28 1.401(16) . ? C27 H27 0.9500 . ? C16 C17 1.369(14) . ? C16 C15 1.390(16) . ? C16 H16 0.9500 . ? C17 C12 1.402(13) . ? C17 C21 1.521(15) . ? C10 C9 1.343(14) . ? C10 H10 0.9500 . ? C9 H9 0.9500 . ? C26 C25 1.393(15) . ? C26 H26 0.9500 . ? C34 C33 1.509(15) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C24 C25 1.392(14) . ? C24 C29 1.392(15) . ? C18 C13 1.502(14) . ? C18 C20 1.513(15) . ? C18 C19 1.504(16) . ? C18 H18 1.0000 . ? C25 C33 1.507(15) . ? C13 C12 1.389(14) . ? C13 C14 1.387(14) . ? C21 C22 1.517(15) . ? C21 C23 1.551(16) . ? C21 H21 1.0000 . ? C15 C14 1.386(15) . ? C15 H15 0.9500 . ? C30 C32 1.516(17) . ? C30 C31 1.521(16) . ? C30 C29 1.533(15) . ? C30 H30 1.0000 . ? C29 C28 1.373(15) . ? C14 H14 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C35 C33 1.506(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C28 H28 0.9500 . ? C33 H33 1.0000 . ? C7 C8 1.356(14) . ? C7 C6 1.392(14) . ? C7 H7 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C6 H6 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Cl42 C46 1.70(4) . ? Cl43 C47 1.55(5) . ? Cl43 C46 1.74(3) . ? Cl40 C47 1.84(5) . ? Cl44 C47 1.86(5) . ? Cl44 Cl41 1.987(11) . ? Cl41 C46 1.84(4) . ? Cl41 Cl41 2.122(16) 2_765 ? C46 C47 1.89(6) . ? 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 N3 Pd1 C1 79.2(3) . . ? N3 Pd1 C11 78.9(3) . . ? C1 Pd1 C11 158.1(4) . . ? N3 Pd1 Cl2 179.4(2) . . ? C1 Pd1 Cl2 101.3(2) . . ? C11 Pd1 Cl2 100.6(3) . . ? C1 N5 C2 111.4(7) . . ? C1 N5 C12 124.6(8) . . ? C2 N5 C12 123.7(7) . . ? C11 N1 C10 110.5(8) . . ? C11 N1 C24 127.0(8) . . ? C10 N1 C24 122.4(8) . . ? C3 N4 C1 112.3(7) . . ? C3 N4 C4 129.7(8) . . ? C1 N4 C4 117.9(7) . . ? C4 N3 C8 120.9(8) . . ? C4 N3 Pd1 119.7(6) . . ? C8 N3 Pd1 119.4(6) . . ? C11 N2 C9 113.0(8) . . ? C11 N2 C8 119.9(7) . . ? C9 N2 C8 127.1(8) . . ? C2 C3 N4 105.8(8) . . ? C2 C3 H3 127.1 . . ? N4 C3 H3 127.1 . . ? C3 C2 N5 107.5(8) . . ? C3 C2 H2 126.4 . . ? N5 C2 H2 126.2 . . ? C4 C5 C6 116.3(9) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.8 . . ? C26 C27 C28 119.6(10) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C17 C16 C15 121.2(9) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.3 . . ? C16 C17 C12 116.8(9) . . ? C16 C17 C21 122.1(9) . . ? C12 C17 C21 121.1(9) . . ? N5 C1 N4 103.1(7) . . ? N5 C1 Pd1 144.7(7) . . ? N4 C1 Pd1 112.0(6) . . ? C9 C10 N1 107.5(9) . . ? C9 C10 H10 126.3 . . ? N1 C10 H10 126.3 . . ? C10 C9 N2 104.8(8) . . ? C10 C9 H9 127.7 . . ? N2 C9 H9 127.5 . . ? C27 C26 C25 121.9(10) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C33 C34 H34A 109.4 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.6 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C25 C24 C29 124.6(9) . . ? C25 C24 N1 118.0(9) . . ? C29 C24 N1 117.4(9) . . ? C13 C18 C20 112.8(9) . . ? C13 C18 C19 110.0(9) . . ? C20 C18 C19 110.9(10) . . ? C13 C18 H18 107.5 . . ? C20 C18 H18 107.6 . . ? C19 C18 H18 107.7 . . ? C26 C25 C24 115.8(10) . . ? C26 C25 C33 120.4(9) . . ? C24 C25 C33 123.8(9) . . ? C12 C13 C14 116.6(9) . . ? C12 C13 C18 122.5(9) . . ? C14 C13 C18 120.9(9) . . ? C22 C21 C17 113.9(9) . . ? C22 C21 C23 108.2(9) . . ? C17 C21 C23 111.6(9) . . ? C22 C21 H21 107.7 . . ? C17 C21 H21 107.7 . . ? C23 C21 H21 107.6 . . ? C14 C15 C16 120.2(9) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 120.0 . . ? C32 C30 C31 109.8(11) . . ? C32 C30 C29 111.1(10) . . ? C31 C30 C29 111.8(9) . . ? C32 C30 H30 108.0 . . ? C31 C30 H30 107.9 . . ? C29 C30 H30 108.1 . . ? N1 C11 N2 104.2(7) . . ? N1 C11 Pd1 143.7(7) . . ? N2 C11 Pd1 112.1(7) . . ? C13 C12 C17 124.1(9) . . ? C13 C12 N5 117.0(8) . . ? C17 C12 N5 118.9(9) . . ? C28 C29 C24 117.0(10) . . ? C28 C29 C30 120.8(10) . . ? C24 C29 C30 122.2(9) . . ? C15 C14 C13 121.0(10) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.6 . . ? N3 C4 C5 122.6(8) . . ? N3 C4 N4 111.2(8) . . ? C5 C4 N4 126.1(9) . . ? C21 C22 H22A 109.6 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.4 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C33 C35 H35A 109.2 . . ? C33 C35 H35B 109.8 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C29 C28 C27 121.0(11) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C35 C33 C34 110.1(9) . . ? C35 C33 C25 110.0(9) . . ? C34 C33 C25 112.8(9) . . ? C35 C33 H33 108.1 . . ? C34 C33 H33 107.9 . . ? C25 C33 H33 107.9 . . ? C8 C7 C6 117.7(9) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.3 . . ? C21 C23 H23A 109.7 . . ? C21 C23 H23B 109.3 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.4 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C20 H20A 109.7 . . ? C18 C20 H20B 109.3 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C6 C5 121.4(9) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.4 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.4 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C8 C7 121.0(9) . . ? N3 C8 N2 109.7(8) . . ? C7 C8 N2 129.3(9) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.7 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.6 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.3 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C47 Cl43 C46 70(2) . . ? C47 Cl44 Cl41 101.5(16) . . ? C46 Cl41 Cl44 74.4(12) . . ? C46 Cl41 Cl41 98.3(12) . 2_765 ? Cl44 Cl41 Cl41 167.4(7) . 2_765 ? Cl42 C46 Cl43 106.8(19) . . ? Cl42 C46 Cl41 108.4(19) . . ? Cl43 C46 Cl41 113.0(19) . . ? Cl42 C46 C47 145(3) . . ? Cl43 C46 C47 50.4(17) . . ? Cl41 C46 C47 106(2) . . ? Cl43 C47 Cl40 115(3) . . ? Cl43 C47 C46 60(2) . . ? Cl40 C47 C46 175(3) . . ? Cl43 C47 Cl44 106(3) . . ? Cl40 C47 Cl44 106(2) . . ? C46 C47 Cl44 76(2) . . ? 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 C1 Pd1 N3 C4 1.2(7) . . . . ? C11 Pd1 N3 C4 -178.9(8) . . . . ? Cl2 Pd1 N3 C4 -141(23) . . . . ? C1 Pd1 N3 C8 -179.7(8) . . . . ? C11 Pd1 N3 C8 0.3(7) . . . . ? Cl2 Pd1 N3 C8 39(24) . . . . ? C1 N4 C3 C2 -0.5(11) . . . . ? C4 N4 C3 C2 -176.2(9) . . . . ? N4 C3 C2 N5 -0.1(11) . . . . ? C1 N5 C2 C3 0.7(11) . . . . ? C12 N5 C2 C3 174.4(8) . . . . ? C15 C16 C17 C12 1.2(15) . . . . ? C15 C16 C17 C21 178.6(10) . . . . ? C2 N5 C1 N4 -1.0(10) . . . . ? C12 N5 C1 N4 -174.6(8) . . . . ? C2 N5 C1 Pd1 173.5(10) . . . . ? C12 N5 C1 Pd1 -0.1(17) . . . . ? C3 N4 C1 N5 0.9(10) . . . . ? C4 N4 C1 N5 177.2(8) . . . . ? C3 N4 C1 Pd1 -175.7(6) . . . . ? C4 N4 C1 Pd1 0.6(10) . . . . ? N3 Pd1 C1 N5 -175.1(13) . . . . ? C11 Pd1 C1 N5 -175.2(10) . . . . ? Cl2 Pd1 C1 N5 4.6(13) . . . . ? N3 Pd1 C1 N4 -0.9(6) . . . . ? C11 Pd1 C1 N4 -1.0(14) . . . . ? Cl2 Pd1 C1 N4 178.7(6) . . . . ? C11 N1 C10 C9 -1.2(12) . . . . ? C24 N1 C10 C9 -178.3(9) . . . . ? N1 C10 C9 N2 1.4(12) . . . . ? C11 N2 C9 C10 -1.1(12) . . . . ? C8 N2 C9 C10 -179.7(9) . . . . ? C28 C27 C26 C25 3.2(16) . . . . ? C11 N1 C24 C25 91.0(11) . . . . ? C10 N1 C24 C25 -92.4(11) . . . . ? C11 N1 C24 C29 -90.4(12) . . . . ? C10 N1 C24 C29 86.1(12) . . . . ? C27 C26 C25 C24 -1.2(14) . . . . ? C27 C26 C25 C33 178.2(10) . . . . ? C29 C24 C25 C26 -0.3(14) . . . . ? N1 C24 C25 C26 178.2(8) . . . . ? C29 C24 C25 C33 -179.7(9) . . . . ? N1 C24 C25 C33 -1.2(13) . . . . ? C20 C18 C13 C12 -137.0(10) . . . . ? C19 C18 C13 C12 98.5(12) . . . . ? C20 C18 C13 C14 45.5(14) . . . . ? C19 C18 C13 C14 -78.9(13) . . . . ? C16 C17 C21 C22 23.8(14) . . . . ? C12 C17 C21 C22 -158.8(10) . . . . ? C16 C17 C21 C23 -99.0(12) . . . . ? C12 C17 C21 C23 78.4(12) . . . . ? C17 C16 C15 C14 -0.4(16) . . . . ? C10 N1 C11 N2 0.5(11) . . . . ? C24 N1 C11 N2 177.4(9) . . . . ? C10 N1 C11 Pd1 -179.0(10) . . . . ? C24 N1 C11 Pd1 -2.1(18) . . . . ? C9 N2 C11 N1 0.4(11) . . . . ? C8 N2 C11 N1 179.0(8) . . . . ? C9 N2 C11 Pd1 -179.9(7) . . . . ? C8 N2 C11 Pd1 -1.3(11) . . . . ? N3 Pd1 C11 N1 -180.0(12) . . . . ? C1 Pd1 C11 N1 -179.8(10) . . . . ? Cl2 Pd1 C11 N1 0.4(12) . . . . ? N3 Pd1 C11 N2 0.5(6) . . . . ? C1 Pd1 C11 N2 0.7(14) . . . . ? Cl2 Pd1 C11 N2 -179.1(6) . . . . ? C14 C13 C12 C17 -2.1(15) . . . . ? C18 C13 C12 C17 -179.7(10) . . . . ? C14 C13 C12 N5 175.5(8) . . . . ? C18 C13 C12 N5 -2.1(14) . . . . ? C16 C17 C12 C13 0.1(15) . . . . ? C21 C17 C12 C13 -177.4(9) . . . . ? C16 C17 C12 N5 -177.4(9) . . . . ? C21 C17 C12 N5 5.1(14) . . . . ? C1 N5 C12 C13 76.7(12) . . . . ? C2 N5 C12 C13 -96.1(11) . . . . ? C1 N5 C12 C17 -105.6(11) . . . . ? C2 N5 C12 C17 81.6(11) . . . . ? C25 C24 C29 C28 -0.3(14) . . . . ? N1 C24 C29 C28 -178.8(8) . . . . ? C25 C24 C29 C30 -179.3(9) . . . . ? N1 C24 C29 C30 2.2(13) . . . . ? C32 C30 C29 C28 -61.0(14) . . . . ? C31 C30 C29 C28 62.1(14) . . . . ? C32 C30 C29 C24 118.0(12) . . . . ? C31 C30 C29 C24 -119.0(12) . . . . ? C16 C15 C14 C13 -1.8(16) . . . . ? C12 C13 C14 C15 2.9(15) . . . . ? C18 C13 C14 C15 -179.5(10) . . . . ? C8 N3 C4 C5 1.6(14) . . . . ? Pd1 N3 C4 C5 -179.3(7) . . . . ? C8 N3 C4 N4 179.8(8) . . . . ? Pd1 N3 C4 N4 -1.1(11) . . . . ? C6 C5 C4 N3 0.7(15) . . . . ? C6 C5 C4 N4 -177.1(9) . . . . ? C3 N4 C4 N3 175.8(9) . . . . ? C1 N4 C4 N3 0.2(12) . . . . ? C3 N4 C4 C5 -6.1(17) . . . . ? C1 N4 C4 C5 178.3(9) . . . . ? C24 C29 C28 C27 2.4(15) . . . . ? C30 C29 C28 C27 -178.6(9) . . . . ? C26 C27 C28 C29 -3.8(16) . . . . ? C26 C25 C33 C35 69.9(12) . . . . ? C24 C25 C33 C35 -110.7(11) . . . . ? C26 C25 C33 C34 -53.4(13) . . . . ? C24 C25 C33 C34 126.0(10) . . . . ? C8 C7 C6 C5 3.4(15) . . . . ? C4 C5 C6 C7 -3.3(15) . . . . ? C4 N3 C8 C7 -1.5(15) . . . . ? Pd1 N3 C8 C7 179.4(8) . . . . ? C4 N3 C8 N2 178.2(8) . . . . ? Pd1 N3 C8 N2 -0.9(10) . . . . ? C6 C7 C8 N3 -1.0(15) . . . . ? C6 C7 C8 N2 179.4(9) . . . . ? C11 N2 C8 N3 1.4(12) . . . . ? C9 N2 C8 N3 179.9(9) . . . . ? C11 N2 C8 C7 -178.9(10) . . . . ? C9 N2 C8 C7 -0.5(17) . . . . ? C47 Cl44 Cl41 C46 -10.4(19) . . . . ? C47 Cl44 Cl41 Cl41 46(4) . . . 2_765 ? C47 Cl43 C46 Cl42 149(3) . . . . ? C47 Cl43 C46 Cl41 -92(3) . . . . ? Cl44 Cl41 C46 Cl42 -178.2(19) . . . . ? Cl41 Cl41 C46 Cl42 12.4(18) 2_765 . . . ? Cl44 Cl41 C46 Cl43 63.6(17) . . . . ? Cl41 Cl41 C46 Cl43 -105.8(18) 2_765 . . . ? Cl44 Cl41 C46 C47 10.4(19) . . . . ? Cl41 Cl41 C46 C47 -159(2) 2_765 . . . ? C46 Cl43 C47 Cl40 -180(3) . . . . ? C46 Cl43 C47 Cl44 63(2) . . . . ? Cl42 C46 C47 Cl43 -59(4) . . . . ? Cl41 C46 C47 Cl43 107(2) . . . . ? Cl42 C46 C47 Cl40 -55(38) . . . . ? Cl43 C46 C47 Cl40 3(35) . . . . ? Cl41 C46 C47 Cl40 110(36) . . . . ? Cl42 C46 C47 Cl44 -177(4) . . . . ? Cl43 C46 C47 Cl44 -118(2) . . . . ? Cl41 C46 C47 Cl44 -11(2) . . . . ? Cl41 Cl44 C47 Cl43 -42(3) . . . . ? Cl41 Cl44 C47 Cl40 -165.6(17) . . . . ? Cl41 Cl44 C47 C46 10.1(18) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.730 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.184