# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Martin Albrecht' 'Helen Stoeckli-Evans' _publ_contact_author_name 'ProfD Martin Albrecht' _publ_contact_author_address ; Chemistry Department University of Fribourg Organometallic Synthesis Lab Chemin du Musee 9 Fribourg 1700 SWITZERLAND ; _publ_contact_author_email MARTIN.ALBRECHT@UNIFR.CH _publ_requested_journal 'Chemical Communications' _publ_section_title ; Catalytically active palladium pyridylidene complexes: Pyridinium ionic liquids as N-heterocyclic carbene precursors ; #================================================= data_cpd2 _database_code_depnum_ccdc_archive 'CCDC 275134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 I2 N2 Pd' _chemical_formula_sum 'C13 H20 I2 N2 Pd' _chemical_formula_weight 564.51 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' I I -0.4742 1.8119 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.7386(6) _cell_length_b 16.3024(8) _cell_length_c 31.923(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6629.4(6) _cell_formula_units_Z 16 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 36053 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 25.90 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 4.832 _exptl_absorpt_correction_type empircal _exptl_absorpt_correction_T_min 0.285 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details 'refined from \DF (DELABS in PLATON; Spek, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50877 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.11 _reflns_number_total 13031 _reflns_number_gt 9801 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'X-Area V2.1 (STOE, 2003)' _computing_cell_refinement 'X-Area V2.1' _computing_data_reduction 'X-RED32 V1.05 (STOE, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL-97 _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^)+(0.0397P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 13031 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 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 I1 I -0.11971(5) 1.06046(5) 0.12470(2) 0.06051(18) Uani 1 1 d . . . I2 I -0.03681(6) 1.19432(5) 0.21553(2) 0.06686(19) Uani 1 1 d . . . Pd1 Pd 0.00781(6) 1.04340(5) 0.18715(2) 0.05055(18) Uani 1 1 d . . . N1 N 0.1258(6) 1.0251(5) 0.2334(3) 0.060(2) Uani 1 1 d . . . N2 N 0.1528(7) 0.7804(5) 0.1544(3) 0.056(2) Uani 1 1 d . . . C1 C 0.2237(8) 1.0594(8) 0.2167(4) 0.078(3) Uani 1 1 d . . . H1A H 0.2184 1.1193 0.2157 0.117 Uiso 1 1 calc R . . H1B H 0.2358 1.0380 0.1884 0.117 Uiso 1 1 calc R . . H1C H 0.2824 1.0437 0.2349 0.117 Uiso 1 1 calc R . . C2 C 0.1076(9) 1.0567(8) 0.2769(3) 0.067(3) Uani 1 1 d . . . H2A H 0.0842 1.1146 0.2765 0.080 Uiso 1 1 calc R . . H2B H 0.1716 1.0519 0.2943 0.080 Uiso 1 1 calc R . . C3 C 0.0219(9) 1.0005(7) 0.2922(3) 0.065(3) Uani 1 1 d . . . H3A H -0.0479 1.0208 0.2834 0.077 Uiso 1 1 calc R . . H3B H 0.0232 0.9964 0.3232 0.077 Uiso 1 1 calc R . . C4 C 0.0462(11) 0.9163(7) 0.2719(3) 0.076(3) Uani 1 1 d . . . H4B H -0.0167 0.8938 0.2577 0.091 Uiso 1 1 calc R . . H4A H 0.0707 0.8764 0.2931 0.091 Uiso 1 1 calc R . . C5 C 0.1336(8) 0.9350(6) 0.2399(3) 0.058(3) Uani 1 1 d . . . H5A H 0.2036 0.9208 0.2521 0.070 Uiso 1 1 calc R . . C6 C 0.1194(8) 0.8925(7) 0.1989(3) 0.057(3) Uani 1 1 d . . . C7 C 0.0496(8) 0.9304(7) 0.1700(3) 0.054(2) Uani 1 1 d . . . C8 C 0.0321(8) 0.8862(7) 0.1341(3) 0.058(3) Uani 1 1 d . . . H8A H -0.0151 0.9075 0.1137 0.070 Uiso 1 1 calc R . . C9 C 0.0805(9) 0.8121(8) 0.1264(3) 0.068(3) Uani 1 1 d . . . H9A H 0.0641 0.7824 0.1017 0.082 Uiso 1 1 calc R . . C10 C 0.1679(9) 0.8207(8) 0.1906(3) 0.067(3) Uani 1 1 d . . . H10A H 0.2141 0.7981 0.2109 0.080 Uiso 1 1 calc R . . C11 C 0.2115(11) 0.7026(7) 0.1453(4) 0.075(3) Uani 1 1 d . . . H11A H 0.2682 0.6989 0.1669 0.091 Uiso 1 1 calc R . . C12 C 0.1439(14) 0.6345(8) 0.1526(6) 0.109(6) Uani 1 1 d . . . H12C H 0.1851 0.5838 0.1525 0.164 Uiso 1 1 calc R . . H12B H 0.0905 0.6321 0.1306 0.164 Uiso 1 1 calc R . . H12A H 0.1095 0.6409 0.1799 0.164 Uiso 1 1 calc R . . C13 C 0.2664(10) 0.7064(8) 0.1035(4) 0.080(4) Uani 1 1 d . . . H13A H 0.3165 0.7520 0.1035 0.120 Uiso 1 1 calc R . . H13B H 0.2145 0.7148 0.0813 0.120 Uiso 1 1 calc R . . H13C H 0.3039 0.6548 0.0986 0.120 Uiso 1 1 calc R . . I21 I 0.39578(5) -0.06040(5) 0.12708(2) 0.06443(19) Uani 1 1 d . . . I22 I 0.45254(6) -0.17474(5) 0.22723(2) 0.0691(2) Uani 1 1 d . . . Pd2 Pd 0.49259(6) -0.02377(5) 0.19572(2) 0.04994(18) Uani 1 1 d . . . N21 N 0.5666(6) 0.0230(5) 0.2509(2) 0.057(2) Uani 1 1 d . . . N22 N 0.6393(9) 0.2314(7) 0.1501(3) 0.074(3) Uani 1 1 d . . . C21 C 0.4890(10) 0.0750(9) 0.2747(3) 0.083(4) Uani 1 1 d . . . H21A H 0.4315 0.0404 0.2848 0.125 Uiso 1 1 calc R . . H21B H 0.4608 0.1175 0.2561 0.125 Uiso 1 1 calc R . . H21C H 0.5243 0.1009 0.2985 0.125 Uiso 1 1 calc R . . C22 C 0.6180(8) -0.0336(7) 0.2805(3) 0.063(3) Uani 1 1 d . . . H22A H 0.5721 -0.0810 0.2870 0.076 Uiso 1 1 calc R . . H22B H 0.6364 -0.0053 0.3070 0.076 Uiso 1 1 calc R . . C23 C 0.7179(8) -0.0614(8) 0.2567(4) 0.069(3) Uani 1 1 d . . . H23A H 0.7768 -0.0708 0.2764 0.083 Uiso 1 1 calc R . . H23B H 0.7046 -0.1126 0.2409 0.083 Uiso 1 1 calc R . . C24 C 0.7418(8) 0.0090(7) 0.2274(4) 0.066(3) Uani 1 1 d . . . H24B H 0.7400 -0.0098 0.1979 0.079 Uiso 1 1 calc R . . H24A H 0.8122 0.0318 0.2333 0.079 Uiso 1 1 calc R . . C25 C 0.6564(9) 0.0744(7) 0.2351(4) 0.067(3) Uani 1 1 d . . . H25A H 0.6796 0.1141 0.2571 0.080 Uiso 1 1 calc R . . C26 C 0.6191(9) 0.1195(7) 0.1966(3) 0.060(3) Uani 1 1 d . . . C27 C 0.5400(8) 0.0823(7) 0.1730(3) 0.055(2) Uani 1 1 d . . . C28 C 0.5094(9) 0.1289(7) 0.1381(3) 0.066(3) Uani 1 1 d . . . H28A H 0.4528 0.1108 0.1211 0.080 Uiso 1 1 calc R . . C29 C 0.5625(11) 0.2026(9) 0.1281(4) 0.083(4) Uani 1 1 d . . . H29A H 0.5406 0.2324 0.1041 0.099 Uiso 1 1 calc R . . C30 C 0.6689(10) 0.1907(7) 0.1845(4) 0.067(3) Uani 1 1 d . . . H30A H 0.7253 0.2112 0.2009 0.081 Uiso 1 1 calc R . . C31 C 0.6933(15) 0.3088(9) 0.1359(5) 0.112(6) Uani 1 1 d . . . H31A H 0.7552 0.3041 0.1550 0.134 Uiso 1 1 calc R . . C32 C 0.6531(15) 0.3772(8) 0.1532(5) 0.114(6) Uani 1 1 d . . . H32C H 0.6946 0.4248 0.1443 0.170 Uiso 1 1 calc R . . H32B H 0.6553 0.3725 0.1838 0.170 Uiso 1 1 calc R . . H32A H 0.5803 0.3842 0.1440 0.170 Uiso 1 1 calc R . . C33 C 0.7483(10) 0.2978(8) 0.0988(5) 0.083(4) Uani 1 1 d . . . H33A H 0.6993 0.2996 0.0751 0.124 Uiso 1 1 calc R . . H33B H 0.7838 0.2444 0.0993 0.124 Uiso 1 1 calc R . . H33C H 0.8005 0.3415 0.0957 0.124 Uiso 1 1 calc R . . I31 I 0.47149(6) 0.31712(5) 0.01666(2) 0.0683(2) Uani 1 1 d . . . I32 I 0.38205(6) 0.46420(5) 0.09864(2) 0.0683(2) Uani 1 1 d . . . Pd3 Pd 0.32500(6) 0.31356(5) 0.07276(2) 0.04995(18) Uani 1 1 d . . . N31 N 0.2210(6) 0.2918(5) 0.1242(3) 0.055(2) Uani 1 1 d . . . N32 N 0.1925(6) 0.0456(5) 0.0427(3) 0.060(2) Uani 1 1 d . . . C41 C 0.2861(9) 0.2638(7) 0.1594(3) 0.063(3) Uani 1 1 d . . . H41A H 0.3367 0.3068 0.1668 0.094 Uiso 1 1 calc R . . H41B H 0.3240 0.2139 0.1513 0.094 Uiso 1 1 calc R . . H41C H 0.2412 0.2521 0.1836 0.094 Uiso 1 1 calc R . . C42 C 0.1536(9) 0.3588(8) 0.1386(4) 0.068(3) Uani 1 1 d . . . H42A H 0.1939 0.4106 0.1402 0.082 Uiso 1 1 calc R . . H42B H 0.1248 0.3464 0.1667 0.082 Uiso 1 1 calc R . . C43 C 0.0672(11) 0.3662(9) 0.1074(4) 0.086(4) Uani 1 1 d . . . H43A H 0.0876 0.4022 0.0838 0.104 Uiso 1 1 calc R . . H43B H 0.0025 0.3879 0.1205 0.104 Uiso 1 1 calc R . . C44 C 0.0519(9) 0.2768(8) 0.0926(4) 0.081(4) Uani 1 1 d . . . H44B H -0.0159 0.2549 0.1029 0.098 Uiso 1 1 calc R . . H44A H 0.0525 0.2739 0.0617 0.098 Uiso 1 1 calc R . . C45 C 0.1428(8) 0.2278(7) 0.1107(3) 0.056(3) Uani 1 1 d . . . H45A H 0.1186 0.1954 0.1355 0.067 Uiso 1 1 calc R . . C46 C 0.1919(7) 0.1724(6) 0.0793(3) 0.053(2) Uani 1 1 d . . . C47 C 0.2746(8) 0.2056(6) 0.0543(3) 0.051(2) Uani 1 1 d . . . C48 C 0.3031(9) 0.1547(7) 0.0216(4) 0.066(3) Uani 1 1 d . . . H48A H 0.3523 0.1746 0.0017 0.080 Uiso 1 1 calc R . . C49 C 0.2638(9) 0.0762(6) 0.0164(3) 0.061(3) Uani 1 1 d . . . H49A H 0.2878 0.0437 -0.0064 0.073 Uiso 1 1 calc R . . C50 C 0.1578(9) 0.0941(7) 0.0741(3) 0.061(3) Uani 1 1 d . . . H50A H 0.1077 0.0726 0.0933 0.073 Uiso 1 1 calc R . . C51 C 0.1493(9) -0.0401(8) 0.0391(4) 0.076(3) Uani 1 1 d . . . H51A H 0.1293 -0.0561 0.0683 0.092 Uiso 1 1 calc R . . C52 C 0.0537(10) -0.0387(8) 0.0163(5) 0.099(5) Uani 1 1 d . . . H52C H 0.0198 -0.0925 0.0182 0.148 Uiso 1 1 calc R . . H52B H 0.0681 -0.0257 -0.0131 0.148 Uiso 1 1 calc R . . H52A H 0.0071 0.0031 0.0282 0.148 Uiso 1 1 calc R . . C53 C 0.2275(9) -0.0990(7) 0.0265(4) 0.070(3) Uani 1 1 d . . . H53A H 0.2913 -0.0910 0.0432 0.105 Uiso 1 1 calc R . . H53B H 0.2439 -0.0914 -0.0032 0.105 Uiso 1 1 calc R . . H53C H 0.2006 -0.1546 0.0310 0.105 Uiso 1 1 calc R . . I41 I 0.01009(5) 0.19779(4) 0.47535(2) 0.05798(17) Uani 1 1 d . . . I42 I 0.14775(6) 0.04648(4) 0.40432(2) 0.06130(17) Uani 1 1 d . . . Pd4 Pd 0.18011(5) 0.20113(5) 0.43043(2) 0.04609(17) Uani 1 1 d . . . N41 N 0.3182(6) 0.2175(5) 0.3933(2) 0.056(2) Uani 1 1 d . . . N42 N 0.3065(7) 0.4605(6) 0.4763(3) 0.060(2) Uani 1 1 d . . . C61 C 0.4092(9) 0.1805(8) 0.4156(4) 0.078(3) Uani 1 1 d . . . H61A H 0.3999 0.1210 0.4173 0.117 Uiso 1 1 calc R . . H61B H 0.4137 0.2034 0.4439 0.117 Uiso 1 1 calc R . . H61C H 0.4740 0.1929 0.4003 0.117 Uiso 1 1 calc R . . C62 C 0.3113(10) 0.1890(8) 0.3490(3) 0.072(3) Uani 1 1 d . . . H62A H 0.2827 0.1326 0.3476 0.087 Uiso 1 1 calc R . . H62B H 0.3814 0.1895 0.3356 0.087 Uiso 1 1 calc R . . C63 C 0.2401(12) 0.2475(9) 0.3281(4) 0.085(4) Uani 1 1 d . . . H63A H 0.1658 0.2314 0.3320 0.102 Uiso 1 1 calc R . . H63B H 0.2553 0.2509 0.2977 0.102 Uiso 1 1 calc R . . C64 C 0.2640(11) 0.3300(8) 0.3502(3) 0.075(3) Uani 1 1 d . . . H64A H 0.1980 0.3573 0.3588 0.090 Uiso 1 1 calc R . . H64B H 0.3027 0.3672 0.3311 0.090 Uiso 1 1 calc R . . C65 C 0.3324(8) 0.3085(6) 0.3894(3) 0.062(3) Uani 1 1 d . . . H65A H 0.4078 0.3221 0.3840 0.074 Uiso 1 1 calc R . . C66 C 0.2951(9) 0.3499(7) 0.4279(3) 0.061(3) Uani 1 1 d . . . C67 C 0.2197(7) 0.3101(6) 0.4519(3) 0.049(2) Uani 1 1 d . . . C68 C 0.1924(8) 0.3494(7) 0.4889(3) 0.057(3) Uani 1 1 d . . . H68A H 0.1431 0.3239 0.5070 0.069 Uiso 1 1 calc R . . C69 C 0.2342(9) 0.4237(8) 0.5002(3) 0.065(3) Uani 1 1 d . . . H69A H 0.2117 0.4494 0.5254 0.078 Uiso 1 1 calc R . . C70 C 0.3385(8) 0.4222(7) 0.4407(4) 0.064(3) Uani 1 1 d . . . H70A H 0.3926 0.4463 0.4243 0.077 Uiso 1 1 calc R . . C71 C 0.3492(9) 0.5400(7) 0.4901(4) 0.068(3) Uani 1 1 d . . . H71A H 0.3199 0.5490 0.5188 0.081 Uiso 1 1 calc R . . C72 C 0.3092(10) 0.6098(8) 0.4642(5) 0.083(4) Uani 1 1 d . . . H72C H 0.3409 0.6612 0.4739 0.125 Uiso 1 1 calc R . . H72B H 0.2327 0.6133 0.4669 0.125 Uiso 1 1 calc R . . H72A H 0.3278 0.6008 0.4347 0.125 Uiso 1 1 calc R . . C73 C 0.4648(10) 0.5391(8) 0.4954(4) 0.088(4) Uani 1 1 d . . . H73A H 0.4984 0.5307 0.4682 0.131 Uiso 1 1 calc R . . H73B H 0.4845 0.4945 0.5144 0.131 Uiso 1 1 calc R . . H73C H 0.4878 0.5916 0.5073 0.131 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 I1 0.0555(4) 0.0683(5) 0.0578(4) 0.0062(3) 0.0014(3) 0.0072(3) I2 0.0726(4) 0.0515(4) 0.0765(4) -0.0022(3) 0.0108(4) 0.0066(4) Pd1 0.0503(4) 0.0475(4) 0.0538(4) 0.0008(3) 0.0040(3) 0.0030(4) N1 0.055(5) 0.054(5) 0.070(5) -0.007(4) -0.004(4) -0.002(4) N2 0.064(5) 0.041(5) 0.064(5) 0.000(4) 0.010(4) 0.008(4) C1 0.050(6) 0.086(9) 0.099(9) -0.001(7) 0.000(6) -0.015(6) C2 0.067(6) 0.079(8) 0.055(6) -0.018(6) -0.011(5) 0.009(6) C3 0.069(7) 0.066(7) 0.059(6) -0.002(5) -0.002(5) 0.002(6) C4 0.117(10) 0.061(7) 0.050(6) 0.005(5) 0.009(6) -0.029(7) C5 0.057(6) 0.047(6) 0.069(6) -0.005(5) -0.008(5) 0.021(5) C6 0.053(6) 0.056(6) 0.061(6) -0.006(5) 0.009(5) -0.005(5) C7 0.049(5) 0.059(6) 0.052(5) -0.001(5) 0.022(5) 0.000(5) C8 0.054(6) 0.066(7) 0.055(6) -0.009(5) 0.007(5) -0.003(5) C9 0.084(8) 0.067(8) 0.054(6) -0.004(6) 0.007(6) -0.011(6) C10 0.065(7) 0.076(8) 0.059(6) -0.003(6) 0.009(5) -0.007(6) C11 0.103(9) 0.054(7) 0.069(7) -0.011(6) 0.014(7) 0.013(7) C12 0.123(13) 0.056(8) 0.148(15) 0.016(8) 0.039(11) -0.008(9) C13 0.079(8) 0.055(7) 0.108(10) -0.005(7) 0.036(7) 0.011(6) I21 0.0578(4) 0.0775(5) 0.0580(4) -0.0078(4) -0.0017(3) -0.0001(4) I22 0.0712(4) 0.0603(5) 0.0758(5) 0.0068(4) 0.0040(4) -0.0089(4) Pd2 0.0469(4) 0.0524(4) 0.0506(4) -0.0013(3) 0.0048(3) -0.0021(3) N21 0.059(5) 0.064(6) 0.048(4) 0.001(4) 0.014(4) -0.008(4) N22 0.084(7) 0.073(7) 0.066(6) 0.001(5) 0.016(6) -0.005(6) C21 0.086(8) 0.099(10) 0.064(7) -0.028(6) 0.018(6) -0.017(8) C22 0.064(6) 0.076(8) 0.049(6) 0.012(5) 0.000(5) -0.020(6) C23 0.066(6) 0.074(8) 0.069(7) 0.009(6) -0.010(6) 0.003(6) C24 0.061(6) 0.073(8) 0.063(7) 0.006(6) 0.002(5) -0.002(6) C25 0.069(7) 0.064(7) 0.068(7) -0.006(6) 0.004(6) -0.006(6) C26 0.065(7) 0.058(7) 0.057(6) -0.006(5) 0.011(5) 0.002(5) C27 0.046(5) 0.059(6) 0.060(6) -0.005(5) 0.003(5) 0.001(5) C28 0.067(7) 0.075(8) 0.057(6) 0.002(5) 0.003(5) 0.009(6) C29 0.096(9) 0.072(9) 0.079(8) 0.033(7) 0.021(8) 0.030(8) C30 0.082(7) 0.046(6) 0.075(7) -0.007(6) 0.016(6) -0.014(6) C31 0.165(15) 0.060(9) 0.110(11) -0.004(8) 0.080(11) -0.036(10) C32 0.149(15) 0.051(8) 0.142(14) -0.007(8) 0.079(12) -0.028(9) C33 0.078(8) 0.054(7) 0.117(10) -0.002(7) 0.040(8) -0.015(6) I31 0.0747(5) 0.0627(5) 0.0675(4) -0.0021(3) 0.0212(4) -0.0072(4) I32 0.0918(5) 0.0561(4) 0.0571(4) -0.0043(3) 0.0031(4) -0.0071(4) Pd3 0.0540(4) 0.0479(4) 0.0480(4) 0.0000(3) 0.0026(3) 0.0018(4) N31 0.061(5) 0.046(5) 0.057(5) -0.008(4) 0.003(4) 0.003(4) N32 0.059(5) 0.050(5) 0.071(5) -0.014(4) 0.010(4) -0.001(4) C41 0.077(7) 0.064(7) 0.048(6) -0.002(5) -0.002(5) 0.008(6) C42 0.063(6) 0.076(8) 0.065(7) -0.010(6) 0.010(6) 0.009(6) C43 0.085(9) 0.084(10) 0.091(9) 0.001(7) -0.009(7) 0.017(7) C44 0.064(7) 0.093(10) 0.087(8) -0.030(7) -0.011(7) 0.021(7) C45 0.054(6) 0.052(6) 0.061(6) -0.003(5) 0.010(5) 0.006(5) C46 0.053(6) 0.050(6) 0.057(6) 0.009(5) 0.009(5) 0.007(5) C47 0.056(5) 0.048(6) 0.049(5) -0.005(4) 0.003(4) 0.007(5) C48 0.075(7) 0.056(7) 0.068(7) -0.007(5) 0.021(6) -0.012(6) C49 0.075(7) 0.042(6) 0.065(6) -0.014(5) 0.015(6) 0.014(5) C50 0.060(6) 0.059(7) 0.065(7) 0.008(5) 0.013(5) 0.016(5) C51 0.063(7) 0.066(8) 0.100(9) -0.023(7) 0.013(6) -0.002(6) C52 0.074(8) 0.050(7) 0.172(14) -0.020(8) -0.033(9) 0.001(7) C53 0.064(7) 0.046(6) 0.099(9) 0.002(6) -0.014(6) 0.007(5) I41 0.0530(3) 0.0524(4) 0.0685(4) 0.0048(3) 0.0107(3) -0.0009(3) I42 0.0708(4) 0.0502(4) 0.0629(4) -0.0056(3) 0.0015(3) -0.0092(3) Pd4 0.0464(4) 0.0426(4) 0.0492(4) 0.0002(3) 0.0003(3) -0.0041(3) N41 0.056(5) 0.055(5) 0.056(5) -0.007(4) 0.006(4) -0.003(4) N42 0.059(5) 0.060(6) 0.061(5) -0.018(4) -0.015(4) 0.007(5) C61 0.056(6) 0.082(9) 0.096(9) -0.018(7) -0.005(6) -0.007(6) C62 0.085(8) 0.071(8) 0.061(7) -0.005(6) 0.016(6) -0.019(7) C63 0.115(10) 0.091(10) 0.049(6) -0.005(6) 0.013(7) -0.024(9) C64 0.105(9) 0.076(8) 0.044(6) -0.002(5) 0.014(6) 0.017(7) C65 0.057(6) 0.045(6) 0.083(7) -0.009(5) 0.020(5) -0.015(5) C66 0.068(7) 0.051(6) 0.065(7) 0.000(5) -0.006(5) 0.002(6) C67 0.043(5) 0.047(6) 0.056(6) -0.003(5) -0.005(4) 0.002(5) C68 0.057(6) 0.057(7) 0.058(6) -0.008(5) 0.003(5) -0.008(5) C69 0.061(6) 0.070(8) 0.065(7) -0.005(6) -0.001(5) -0.010(6) C70 0.052(6) 0.069(7) 0.071(7) 0.007(6) 0.004(5) -0.008(5) C71 0.075(7) 0.060(7) 0.068(7) -0.013(6) -0.006(6) -0.014(6) C72 0.076(8) 0.067(8) 0.107(10) 0.003(7) -0.012(7) 0.001(7) C73 0.084(8) 0.064(8) 0.115(10) 0.001(7) -0.034(7) 0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.5867(10) . ? I2 Pd1 2.6827(10) . ? Pd1 C7 1.994(10) . ? Pd1 N1 2.129(8) . ? N1 C1 1.468(13) . ? N1 C5 1.486(14) . ? N1 C2 1.498(13) . ? N2 C10 1.341(14) . ? N2 C9 1.384(14) . ? N2 C11 1.499(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.507(16) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.551(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.541(15) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 C6 1.493(15) . ? C5 H5A 1.0000 . ? C6 C10 1.350(16) . ? C6 C7 1.421(15) . ? C7 C8 1.374(14) . ? C8 C9 1.379(16) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.424(18) . ? C11 C13 1.507(16) . ? C11 H11A 1.0000 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? I21 Pd2 2.5841(10) . ? I22 Pd2 2.7074(11) . ? Pd2 C27 1.971(11) . ? Pd2 N21 2.138(8) . ? N21 C22 1.475(14) . ? N21 C21 1.508(14) . ? N21 C25 1.506(14) . ? N22 C29 1.291(17) . ? N22 C30 1.337(15) . ? N22 C31 1.506(16) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.551(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.512(15) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.543(16) . ? C24 H24B 0.9900 . ? C24 H24A 0.9900 . ? C25 C26 1.508(16) . ? C25 H25A 1.0000 . ? C26 C30 1.377(15) . ? C26 C27 1.396(15) . ? C27 C28 1.403(15) . ? C28 C29 1.416(18) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.345(19) . ? C31 C33 1.389(17) . ? C31 H31A 1.0000 . ? C32 H32C 0.9800 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? I31 Pd3 2.5872(10) . ? I32 Pd3 2.6911(11) . ? Pd3 C47 1.964(10) . ? Pd3 N31 2.139(8) . ? N31 C42 1.464(13) . ? N31 C41 1.470(13) . ? N31 C45 1.505(13) . ? N32 C49 1.334(13) . ? N32 C50 1.351(13) . ? N32 C51 1.507(14) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.488(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.543(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.520(15) . ? C44 H44B 0.9900 . ? C44 H44A 0.9900 . ? C45 C46 1.488(14) . ? C45 H45A 1.0000 . ? C46 C50 1.359(15) . ? C46 C47 1.428(13) . ? C47 C48 1.382(14) . ? C48 C49 1.384(15) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C53 1.441(15) . ? C51 C52 1.418(17) . ? C51 H51A 1.0000 . ? C52 H52C 0.9800 . ? C52 H52B 0.9800 . ? C52 H52A 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? I41 Pd4 2.5982(9) . ? I42 Pd4 2.6871(10) . ? Pd4 C67 1.969(10) . ? Pd4 N41 2.138(8) . ? N41 C62 1.491(13) . ? N41 C65 1.499(13) . ? N41 C61 1.488(14) . ? N42 C69 1.339(14) . ? N42 C70 1.359(14) . ? N42 C71 1.473(14) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.477(19) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.550(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.565(16) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.481(15) . ? C65 H65A 1.0000 . ? C66 C70 1.364(16) . ? C66 C67 1.389(14) . ? C67 C68 1.389(14) . ? C68 C69 1.372(15) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C73 1.482(17) . ? C71 C72 1.498(17) . ? C71 H71A 1.0000 . ? C72 H72C 0.9800 . ? C72 H72B 0.9800 . ? C72 H72A 0.9800 . ? 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 C7 Pd1 N1 82.6(4) . . ? C7 Pd1 I1 93.2(3) . . ? N1 Pd1 I1 173.5(2) . . ? C7 Pd1 I2 175.2(3) . . ? N1 Pd1 I2 92.5(2) . . ? I1 Pd1 I2 91.64(3) . . ? C1 N1 C5 111.7(9) . . ? C1 N1 C2 109.7(9) . . ? C5 N1 C2 102.9(8) . . ? C1 N1 Pd1 107.1(7) . . ? C5 N1 Pd1 106.4(6) . . ? C2 N1 Pd1 119.0(6) . . ? C10 N2 C9 117.9(10) . . ? C10 N2 C11 120.7(10) . . ? C9 N2 C11 121.5(9) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 101.7(8) . . ? N1 C2 H2A 111.4 . . ? C3 C2 H2A 111.4 . . ? N1 C2 H2B 111.4 . . ? C3 C2 H2B 111.4 . . ? H2A C2 H2B 109.3 . . ? C2 C3 C4 104.9(9) . . ? C2 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? C2 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.8 . . ? C3 C4 C5 104.2(9) . . ? C3 C4 H4B 110.9 . . ? C5 C4 H4B 110.9 . . ? C3 C4 H4A 110.9 . . ? C5 C4 H4A 110.9 . . ? H4B C4 H4A 108.9 . . ? C6 C5 N1 109.2(9) . . ? C6 C5 C4 113.6(9) . . ? N1 C5 C4 103.9(8) . . ? C6 C5 H5A 110.0 . . ? N1 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? C10 C6 C7 122.4(10) . . ? C10 C6 C5 121.3(10) . . ? C7 C6 C5 116.3(9) . . ? C8 C7 C6 114.5(10) . . ? C8 C7 Pd1 132.1(8) . . ? C6 C7 Pd1 113.0(7) . . ? C9 C8 C7 122.3(11) . . ? C9 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? C8 C9 N2 120.8(10) . . ? C8 C9 H9A 119.6 . . ? N2 C9 H9A 119.6 . . ? C6 C10 N2 121.9(11) . . ? C6 C10 H10A 119.0 . . ? N2 C10 H10A 119.0 . . ? C12 C11 C13 117.2(12) . . ? C12 C11 N2 109.0(11) . . ? C13 C11 N2 111.7(10) . . ? C12 C11 H11A 106.1 . . ? C13 C11 H11A 106.1 . . ? N2 C11 H11A 106.1 . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C27 Pd2 N21 81.7(4) . . ? C27 Pd2 I21 92.1(3) . . ? N21 Pd2 I21 172.4(2) . . ? C27 Pd2 I22 173.0(3) . . ? N21 Pd2 I22 95.8(2) . . ? I21 Pd2 I22 90.87(3) . . ? C22 N21 C21 108.6(8) . . ? C22 N21 C25 103.1(8) . . ? C21 N21 C25 110.7(9) . . ? C22 N21 Pd2 120.1(7) . . ? C21 N21 Pd2 109.1(6) . . ? C25 N21 Pd2 104.9(6) . . ? C29 N22 C30 118.5(11) . . ? C29 N22 C31 119.2(13) . . ? C30 N22 C31 122.3(13) . . ? N21 C21 H21A 109.5 . . ? N21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 C23 103.4(8) . . ? N21 C22 H22A 111.1 . . ? C23 C22 H22A 111.1 . . ? N21 C22 H22B 111.1 . . ? C23 C22 H22B 111.1 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 104.3(9) . . ? C24 C23 H23A 110.9 . . ? C22 C23 H23A 110.9 . . ? C24 C23 H23B 110.9 . . ? C22 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C23 C24 C25 106.6(9) . . ? C23 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? C23 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? H24B C24 H24A 108.6 . . ? N21 C25 C26 107.8(9) . . ? N21 C25 C24 101.7(9) . . ? C26 C25 C24 115.5(9) . . ? N21 C25 H25A 110.5 . . ? C26 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? C30 C26 C27 123.1(11) . . ? C30 C26 C25 119.6(11) . . ? C27 C26 C25 117.1(10) . . ? C26 C27 C28 113.2(10) . . ? C26 C27 Pd2 113.8(8) . . ? C28 C27 Pd2 133.0(8) . . ? C27 C28 C29 120.3(11) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? N22 C29 C28 123.3(12) . . ? N22 C29 H29A 118.3 . . ? C28 C29 H29A 118.3 . . ? N22 C30 C26 121.3(12) . . ? N22 C30 H30A 119.4 . . ? C26 C30 H30A 119.4 . . ? C32 C31 C33 130.5(13) . . ? C32 C31 N22 113.5(11) . . ? C33 C31 N22 112.2(11) . . ? C32 C31 H31A 96.5 . . ? C33 C31 H31A 96.5 . . ? N22 C31 H31A 96.5 . . ? C31 C32 H32C 109.5 . . ? C31 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C47 Pd3 N31 83.0(3) . . ? C47 Pd3 I31 92.8(3) . . ? N31 Pd3 I31 169.0(2) . . ? C47 Pd3 I32 176.6(3) . . ? N31 Pd3 I32 94.8(2) . . ? I31 Pd3 I32 89.84(3) . . ? C42 N31 C41 108.8(8) . . ? C42 N31 C45 102.6(8) . . ? C41 N31 C45 112.1(8) . . ? C42 N31 Pd3 118.7(7) . . ? C41 N31 Pd3 106.7(6) . . ? C45 N31 Pd3 107.8(6) . . ? C49 N32 C50 118.2(9) . . ? C49 N32 C51 123.2(9) . . ? C50 N32 C51 118.6(9) . . ? N31 C41 H41A 109.5 . . ? N31 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N31 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N31 C42 C43 106.5(9) . . ? N31 C42 H42A 110.4 . . ? C43 C42 H42A 110.4 . . ? N31 C42 H42B 110.4 . . ? C43 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C42 C43 C44 102.8(10) . . ? C42 C43 H43A 111.2 . . ? C44 C43 H43A 111.2 . . ? C42 C43 H43B 111.2 . . ? C44 C43 H43B 111.2 . . ? H43A C43 H43B 109.1 . . ? C45 C44 C43 106.5(9) . . ? C45 C44 H44B 110.4 . . ? C43 C44 H44B 110.4 . . ? C45 C44 H44A 110.4 . . ? C43 C44 H44A 110.4 . . ? H44B C44 H44A 108.6 . . ? C46 C45 N31 109.5(8) . . ? C46 C45 C44 112.6(9) . . ? N31 C45 C44 104.3(9) . . ? C46 C45 H45A 110.1 . . ? N31 C45 H45A 110.1 . . ? C44 C45 H45A 110.1 . . ? C50 C46 C47 121.6(9) . . ? C50 C46 C45 121.2(9) . . ? C47 C46 C45 117.2(9) . . ? C48 C47 C46 112.9(10) . . ? C48 C47 Pd3 132.7(8) . . ? C46 C47 Pd3 114.4(7) . . ? C47 C48 C49 123.4(10) . . ? C47 C48 H48A 118.3 . . ? C49 C48 H48A 118.3 . . ? N32 C49 C48 121.0(9) . . ? N32 C49 H49A 119.5 . . ? C48 C49 H49A 119.5 . . ? N32 C50 C46 122.3(10) . . ? N32 C50 H50A 118.8 . . ? C46 C50 H50A 118.8 . . ? C53 C51 C52 117.5(11) . . ? C53 C51 N32 112.7(9) . . ? C52 C51 N32 109.8(11) . . ? C53 C51 H51A 105.2 . . ? C52 C51 H51A 105.2 . . ? N32 C51 H51A 105.2 . . ? C51 C52 H52C 109.5 . . ? C51 C52 H52B 109.5 . . ? H52C C52 H52B 109.5 . . ? C51 C52 H52A 109.5 . . ? H52C C52 H52A 109.5 . . ? H52B C52 H52A 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 . . ? C67 Pd4 N41 82.5(4) . . ? C67 Pd4 I41 92.3(3) . . ? N41 Pd4 I41 174.0(2) . . ? C67 Pd4 I42 173.4(3) . . ? N41 Pd4 I42 94.1(2) . . ? I41 Pd4 I42 91.36(3) . . ? C62 N41 C65 103.7(8) . . ? C62 N41 C61 111.9(9) . . ? C65 N41 C61 110.3(9) . . ? C62 N41 Pd4 116.0(7) . . ? C65 N41 Pd4 105.6(6) . . ? C61 N41 Pd4 108.9(7) . . ? C69 N42 C70 118.6(10) . . ? C69 N42 C71 118.4(9) . . ? C70 N42 C71 123.0(10) . . ? N41 C61 H61A 109.5 . . ? N41 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N41 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N41 C62 C63 105.3(10) . . ? N41 C62 H62A 110.7 . . ? C63 C62 H62A 110.7 . . ? N41 C62 H62B 110.7 . . ? C63 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? C62 C63 C64 103.5(10) . . ? C62 C63 H63A 111.1 . . ? C64 C63 H63A 111.1 . . ? C62 C63 H63B 111.1 . . ? C64 C63 H63B 111.1 . . ? H63A C63 H63B 109.0 . . ? C63 C64 C65 106.2(10) . . ? C63 C64 H64A 110.5 . . ? C65 C64 H64A 110.5 . . ? C63 C64 H64B 110.5 . . ? C65 C64 H64B 110.5 . . ? H64A C64 H64B 108.7 . . ? C66 C65 N41 110.1(8) . . ? C66 C65 C64 112.5(9) . . ? N41 C65 C64 102.8(9) . . ? C66 C65 H65A 110.4 . . ? N41 C65 H65A 110.4 . . ? C64 C65 H65A 110.4 . . ? C70 C66 C67 121.3(10) . . ? C70 C66 C65 120.8(10) . . ? C67 C66 C65 117.8(9) . . ? C68 C67 C66 115.3(9) . . ? C68 C67 Pd4 130.4(8) . . ? C66 C67 Pd4 114.0(7) . . ? C69 C68 C67 122.3(10) . . ? C69 C68 H68A 118.8 . . ? C67 C68 H68A 118.8 . . ? N42 C69 C68 120.8(10) . . ? N42 C69 H69A 119.6 . . ? C68 C69 H69A 119.6 . . ? C66 C70 N42 121.7(10) . . ? C66 C70 H70A 119.2 . . ? N42 C70 H70A 119.2 . . ? C73 C71 N42 113.1(10) . . ? C73 C71 C72 114.1(11) . . ? N42 C71 C72 112.2(9) . . ? C73 C71 H71A 105.5 . . ? N42 C71 H71A 105.5 . . ? C72 C71 H71A 105.5 . . ? C71 C72 H72C 109.5 . . ? C71 C72 H72B 109.5 . . ? H72C C72 H72B 109.5 . . ? C71 C72 H72A 109.5 . . ? H72C C72 H72A 109.5 . . ? H72B C72 H72A 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 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 C7 Pd1 N1 C1 93.8(8) . . . . ? I1 Pd1 N1 C1 43(3) . . . . ? I2 Pd1 N1 C1 -86.4(7) . . . . ? C7 Pd1 N1 C5 -25.8(6) . . . . ? I1 Pd1 N1 C5 -77(2) . . . . ? I2 Pd1 N1 C5 154.0(6) . . . . ? C7 Pd1 N1 C2 -141.2(8) . . . . ? I1 Pd1 N1 C2 167.9(17) . . . . ? I2 Pd1 N1 C2 38.6(8) . . . . ? C1 N1 C2 C3 -166.7(9) . . . . ? C5 N1 C2 C3 -47.7(10) . . . . ? Pd1 N1 C2 C3 69.6(10) . . . . ? N1 C2 C3 C4 34.8(11) . . . . ? C2 C3 C4 C5 -9.8(12) . . . . ? C1 N1 C5 C6 -79.5(10) . . . . ? C2 N1 C5 C6 163.0(8) . . . . ? Pd1 N1 C5 C6 37.1(9) . . . . ? C1 N1 C5 C4 159.0(9) . . . . ? C2 N1 C5 C4 41.4(10) . . . . ? Pd1 N1 C5 C4 -84.5(8) . . . . ? C3 C4 C5 C6 -137.6(9) . . . . ? C3 C4 C5 N1 -19.1(11) . . . . ? N1 C5 C6 C10 148.7(10) . . . . ? C4 C5 C6 C10 -95.9(12) . . . . ? N1 C5 C6 C7 -33.4(12) . . . . ? C4 C5 C6 C7 82.1(12) . . . . ? C10 C6 C7 C8 2.9(15) . . . . ? C5 C6 C7 C8 -175.0(9) . . . . ? C10 C6 C7 Pd1 -171.1(8) . . . . ? C5 C6 C7 Pd1 11.0(11) . . . . ? N1 Pd1 C7 C8 -163.9(10) . . . . ? I1 Pd1 C7 C8 11.0(9) . . . . ? I2 Pd1 C7 C8 -167(2) . . . . ? N1 Pd1 C7 C6 8.7(7) . . . . ? I1 Pd1 C7 C6 -176.4(7) . . . . ? I2 Pd1 C7 C6 6(4) . . . . ? C6 C7 C8 C9 -1.5(14) . . . . ? Pd1 C7 C8 C9 171.1(8) . . . . ? C7 C8 C9 N2 -2.5(16) . . . . ? C10 N2 C9 C8 5.1(15) . . . . ? C11 N2 C9 C8 -175.9(10) . . . . ? C7 C6 C10 N2 -0.3(17) . . . . ? C5 C6 C10 N2 177.5(10) . . . . ? C9 N2 C10 C6 -3.7(16) . . . . ? C11 N2 C10 C6 177.3(10) . . . . ? C10 N2 C11 C12 101.5(14) . . . . ? C9 N2 C11 C12 -77.4(14) . . . . ? C10 N2 C11 C13 -127.5(11) . . . . ? C9 N2 C11 C13 53.6(14) . . . . ? C27 Pd2 N21 C22 -147.5(7) . . . . ? I21 Pd2 N21 C22 176.9(12) . . . . ? I22 Pd2 N21 C22 25.9(6) . . . . ? C27 Pd2 N21 C21 86.3(8) . . . . ? I21 Pd2 N21 C21 50.7(18) . . . . ? I22 Pd2 N21 C21 -100.3(7) . . . . ? C27 Pd2 N21 C25 -32.3(7) . . . . ? I21 Pd2 N21 C25 -67.9(18) . . . . ? I22 Pd2 N21 C25 141.1(6) . . . . ? C21 N21 C22 C23 -161.8(9) . . . . ? C25 N21 C22 C23 -44.3(10) . . . . ? Pd2 N21 C22 C23 71.8(9) . . . . ? N21 C22 C23 C24 26.9(11) . . . . ? C22 C23 C24 C25 0.1(12) . . . . ? C22 N21 C25 C26 165.5(9) . . . . ? C21 N21 C25 C26 -78.5(10) . . . . ? Pd2 N21 C25 C26 39.0(9) . . . . ? C22 N21 C25 C24 43.7(10) . . . . ? C21 N21 C25 C24 159.7(9) . . . . ? Pd2 N21 C25 C24 -82.8(8) . . . . ? C23 C24 C25 N21 -26.3(11) . . . . ? C23 C24 C25 C26 -142.7(10) . . . . ? N21 C25 C26 C30 157.0(10) . . . . ? C24 C25 C26 C30 -90.1(13) . . . . ? N21 C25 C26 C27 -28.1(12) . . . . ? C24 C25 C26 C27 84.8(12) . . . . ? C30 C26 C27 C28 -6.0(15) . . . . ? C25 C26 C27 C28 179.3(9) . . . . ? C30 C26 C27 Pd2 174.9(9) . . . . ? C25 C26 C27 Pd2 0.2(12) . . . . ? N21 Pd2 C27 C26 18.4(7) . . . . ? I21 Pd2 C27 C26 -166.0(7) . . . . ? I22 Pd2 C27 C26 -51(3) . . . . ? N21 Pd2 C27 C28 -160.5(11) . . . . ? I21 Pd2 C27 C28 15.1(10) . . . . ? I22 Pd2 C27 C28 130(2) . . . . ? C26 C27 C28 C29 4.3(15) . . . . ? Pd2 C27 C28 C29 -176.7(9) . . . . ? C30 N22 C29 C28 -1.6(18) . . . . ? C31 N22 C29 C28 177.7(11) . . . . ? C27 C28 C29 N22 -0.8(18) . . . . ? C29 N22 C30 C26 0.0(17) . . . . ? C31 N22 C30 C26 -179.3(11) . . . . ? C27 C26 C30 N22 4.1(17) . . . . ? C25 C26 C30 N22 178.7(10) . . . . ? C29 N22 C31 C32 93.0(19) . . . . ? C30 N22 C31 C32 -88(2) . . . . ? C29 N22 C31 C33 -67.3(19) . . . . ? C30 N22 C31 C33 112.0(16) . . . . ? C47 Pd3 N31 C42 -136.3(8) . . . . ? I31 Pd3 N31 C42 155.6(9) . . . . ? I32 Pd3 N31 C42 41.0(7) . . . . ? C47 Pd3 N31 C41 100.4(7) . . . . ? I31 Pd3 N31 C41 32.3(16) . . . . ? I32 Pd3 N31 C41 -82.3(6) . . . . ? C47 Pd3 N31 C45 -20.3(6) . . . . ? I31 Pd3 N31 C45 -88.3(13) . . . . ? I32 Pd3 N31 C45 157.0(6) . . . . ? C41 N31 C42 C43 -161.8(10) . . . . ? C45 N31 C42 C43 -42.8(12) . . . . ? Pd3 N31 C42 C43 75.9(11) . . . . ? N31 C42 C43 C44 32.4(13) . . . . ? C42 C43 C44 C45 -9.6(14) . . . . ? C42 N31 C45 C46 155.8(8) . . . . ? C41 N31 C45 C46 -87.6(10) . . . . ? Pd3 N31 C45 C46 29.7(9) . . . . ? C42 N31 C45 C44 35.1(10) . . . . ? C41 N31 C45 C44 151.7(9) . . . . ? Pd3 N31 C45 C44 -91.1(8) . . . . ? C43 C44 C45 C46 -134.1(11) . . . . ? C43 C44 C45 N31 -15.5(12) . . . . ? N31 C45 C46 C50 154.0(9) . . . . ? C44 C45 C46 C50 -90.4(13) . . . . ? N31 C45 C46 C47 -27.4(12) . . . . ? C44 C45 C46 C47 88.2(12) . . . . ? C50 C46 C47 C48 8.8(14) . . . . ? C45 C46 C47 C48 -169.8(10) . . . . ? C50 C46 C47 Pd3 -171.3(8) . . . . ? C45 C46 C47 Pd3 10.1(11) . . . . ? N31 Pd3 C47 C48 -173.9(11) . . . . ? I31 Pd3 C47 C48 -4.1(11) . . . . ? I32 Pd3 C47 C48 136(4) . . . . ? N31 Pd3 C47 C46 6.2(7) . . . . ? I31 Pd3 C47 C46 176.1(7) . . . . ? I32 Pd3 C47 C46 -44(5) . . . . ? C46 C47 C48 C49 -6.6(16) . . . . ? Pd3 C47 C48 C49 173.5(9) . . . . ? C50 N32 C49 C48 1.6(16) . . . . ? C51 N32 C49 C48 -178.4(11) . . . . ? C47 C48 C49 N32 1.7(19) . . . . ? C49 N32 C50 C46 0.8(16) . . . . ? C51 N32 C50 C46 -179.2(10) . . . . ? C47 C46 C50 N32 -6.4(16) . . . . ? C45 C46 C50 N32 172.2(10) . . . . ? C49 N32 C51 C53 38.0(16) . . . . ? C50 N32 C51 C53 -142.0(11) . . . . ? C49 N32 C51 C52 -95.0(13) . . . . ? C50 N32 C51 C52 85.0(14) . . . . ? C67 Pd4 N41 C62 -140.2(8) . . . . ? I41 Pd4 N41 C62 -110(2) . . . . ? I42 Pd4 N41 C62 45.5(8) . . . . ? C67 Pd4 N41 C65 -25.9(7) . . . . ? I41 Pd4 N41 C65 4(3) . . . . ? I42 Pd4 N41 C65 159.8(6) . . . . ? C67 Pd4 N41 C61 92.6(7) . . . . ? I41 Pd4 N41 C61 123(2) . . . . ? I42 Pd4 N41 C61 -81.7(7) . . . . ? C65 N41 C62 C63 -44.8(11) . . . . ? C61 N41 C62 C63 -163.7(10) . . . . ? Pd4 N41 C62 C63 70.5(10) . . . . ? N41 C62 C63 C64 34.1(12) . . . . ? C62 C63 C64 C65 -11.6(12) . . . . ? C62 N41 C65 C66 155.3(9) . . . . ? C61 N41 C65 C66 -84.7(11) . . . . ? Pd4 N41 C65 C66 32.8(10) . . . . ? C62 N41 C65 C64 35.3(10) . . . . ? C61 N41 C65 C64 155.3(8) . . . . ? Pd4 N41 C65 C64 -87.2(7) . . . . ? C63 C64 C65 C66 -132.9(10) . . . . ? C63 C64 C65 N41 -14.6(11) . . . . ? N41 C65 C66 C70 150.6(10) . . . . ? C64 C65 C66 C70 -95.5(12) . . . . ? N41 C65 C66 C67 -25.2(13) . . . . ? C64 C65 C66 C67 88.8(12) . . . . ? C70 C66 C67 C68 0.5(15) . . . . ? C65 C66 C67 C68 176.2(10) . . . . ? C70 C66 C67 Pd4 -173.5(9) . . . . ? C65 C66 C67 Pd4 2.2(12) . . . . ? N41 Pd4 C67 C68 -159.0(10) . . . . ? I41 Pd4 C67 C68 24.0(9) . . . . ? I42 Pd4 C67 C68 -100(2) . . . . ? N41 Pd4 C67 C66 13.8(7) . . . . ? I41 Pd4 C67 C66 -163.2(7) . . . . ? I42 Pd4 C67 C66 73(3) . . . . ? C66 C67 C68 C69 2.2(15) . . . . ? Pd4 C67 C68 C69 174.9(9) . . . . ? C70 N42 C69 C68 -0.8(16) . . . . ? C71 N42 C69 C68 -179.6(10) . . . . ? C67 C68 C69 N42 -2.1(17) . . . . ? C67 C66 C70 N42 -3.4(17) . . . . ? C65 C66 C70 N42 -179.0(10) . . . . ? C69 N42 C70 C66 3.5(16) . . . . ? C71 N42 C70 C66 -177.7(10) . . . . ? C69 N42 C71 C73 121.8(12) . . . . ? C70 N42 C71 C73 -57.0(14) . . . . ? C69 N42 C71 C72 -107.3(12) . . . . ? C70 N42 C71 C72 73.9(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C2 H2A I2 0.9899 2.8024 3.501(12) 128.08 . yes C4 H4A I2 0.9892 3.0122 3.643(11) 122.70 4_545 yes C8 H8A I1 0.9519 2.8491 3.450(11) 122.03 . yes C9 H9A I41 0.9486 2.9742 3.919(11) 173.80 4_555 yes C22 H22A I22 0.9910 2.8802 3.554(11) 125.95 . yes C28 H28A I21 0.9494 2.8903 3.427(11) 116.95 . yes C42 H42A I32 0.9896 2.8755 3.612(12) 131.91 . yes C48 H48A I31 0.9495 2.8163 3.411(11) 121.62 . yes C53 H53A I21 0.9807 3.0316 3.912(12) 149.98 . yes C62 H62A I42 0.9900 2.8644 3.586(12) 130.36 . yes C68 H68A I41 0.9493 2.8493 3.419(11) 119.58 . yes C69 H69A I32 0.9512 2.9794 3.925(11) 173.06 2_565 yes _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.919 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.114