Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Andreas Danopoulos' 'Jennifer C. Green' 'Michael B. Hursthouse' 'Nikolaos Tsoureas' _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email AD1@SOTON.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Migratory Insertion in N-heterocyclic Carbene Complexes of Palladium; an Experimental and DFT Study ; data_1 _database_code_CSD 200426 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_melting_point ? _chemical_formula_moiety 'C41 H57 N5 O Pd' _chemical_formula_sum 'C41 H57 N5 O Pd' _chemical_formula_weight 742.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.65920(10) _cell_length_b 21.2788(3) _cell_length_c 21.3929(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.5780(10) _cell_angle_gamma 90.00 _cell_volume 3934.12(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18355 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9653 _exptl_absorpt_correction_T_max 0.9849 _exptl_absorpt_process_details 'Sortav (Blessing, 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 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 44801 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.26 _reflns_number_total 8719 _reflns_number_gt 5677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1998)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0410P)^2^+0.7668P] 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 8719 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 C35 C 0.2580(4) -0.01924(17) 0.20493(15) 0.0579(9) Uani 1 1 d . . . H35 H 0.3543 -0.0112 0.1827 0.069 Uiso 1 1 calc R . . C44 C 0.3700(4) 0.16779(16) 0.20382(15) 0.0595(9) Uani 1 1 d . . . H10A H 0.3872 0.1501 0.2460 0.089 Uiso 1 1 calc R . . H10B H 0.2592 0.1668 0.1913 0.089 Uiso 1 1 calc R . . H10C H 0.4067 0.2114 0.2037 0.089 Uiso 1 1 calc R . . O1 O 0.4025(5) 0.24622(18) 0.82082(14) 0.1118(11) Uani 1 1 d . . . C39 C 0.6069(5) 0.0664(2) 0.38583(16) 0.0808(13) Uani 1 1 d . . . H39 H 0.6798 0.0662 0.3514 0.097 Uiso 1 1 calc R . . C37 C 0.1245(5) 0.0106(2) 0.16677(19) 0.0939(15) Uani 1 1 d . . . H37A H 0.1147 -0.0089 0.1252 0.141 Uiso 1 1 calc R . . H37B H 0.1438 0.0557 0.1624 0.141 Uiso 1 1 calc R . . H37C H 0.0286 0.0042 0.1879 0.141 Uiso 1 1 calc R . . C38 C 0.6662(6) 0.0182(3) 0.4342(3) 0.1176(18) Uani 1 1 d . . . H38A H 0.7696 0.0305 0.4511 0.176 Uiso 1 1 calc R . . H38B H 0.6714 -0.0232 0.4143 0.176 Uiso 1 1 calc R . . H38C H 0.5957 0.0163 0.4682 0.176 Uiso 1 1 calc R . . C41 C -0.0669(7) 0.1975(3) -0.0216(2) 0.134(2) Uani 1 1 d . . . H41A H -0.0077 0.2167 -0.0542 0.201 Uiso 1 1 calc R . . H41B H -0.1505 0.2260 -0.0111 0.201 Uiso 1 1 calc R . . H41C H -0.1111 0.1576 -0.0369 0.201 Uiso 1 1 calc R . . C46 C 0.2916(8) 0.2238(2) 0.7776(2) 0.1054(17) Uani 1 1 d . . . H20A H 0.3277 0.1841 0.7592 0.126 Uiso 1 1 calc R . . H20B H 0.2736 0.2548 0.7434 0.126 Uiso 1 1 calc R . . C47 C 0.5404(7) 0.2649(3) 0.7952(3) 0.125(2) Uani 1 1 d . . . H20C H 0.5202 0.3025 0.7686 0.149 Uiso 1 1 calc R . . H20D H 0.5769 0.2309 0.7683 0.149 Uiso 1 1 calc R . . C36 C 0.2370(7) -0.0904(2) 0.2090(2) 0.1074(17) Uani 1 1 d . . . H36A H 0.2230 -0.1080 0.1667 0.161 Uiso 1 1 calc R . . H36B H 0.1457 -0.0998 0.2322 0.161 Uiso 1 1 calc R . . H36C H 0.3288 -0.1091 0.2307 0.161 Uiso 1 1 calc R . . C45 C 0.1455(7) 0.2125(3) 0.8085(3) 0.1182(18) Uani 1 1 d . . . H20E H 0.0668 0.1964 0.7777 0.177 Uiso 1 1 calc R . . H20F H 0.1095 0.2520 0.8261 0.177 Uiso 1 1 calc R . . H20G H 0.1638 0.1817 0.8422 0.177 Uiso 1 1 calc R . . C48 C 0.6609(8) 0.2795(3) 0.8438(3) 0.154(3) Uani 1 1 d . . . H20H H 0.7550 0.2927 0.8242 0.231 Uiso 1 1 calc R . . H20I H 0.6830 0.2422 0.8695 0.231 Uiso 1 1 calc R . . H20J H 0.6256 0.3136 0.8702 0.231 Uiso 1 1 calc R . . C40 C 0.6140(9) 0.1314(3) 0.4151(3) 0.157(3) Uani 1 1 d . . . H40A H 0.7196 0.1397 0.4323 0.236 Uiso 1 1 calc R . . H40B H 0.5426 0.1334 0.4489 0.236 Uiso 1 1 calc R . . H40C H 0.5845 0.1629 0.3832 0.236 Uiso 1 1 calc R . . C42 C -0.0480(6) 0.1543(3) 0.0864(2) 0.1151(19) Uani 1 1 d . . . H42A H -0.0942 0.1152 0.0699 0.173 Uiso 1 1 calc R . . H42B H -0.1299 0.1825 0.0992 0.173 Uiso 1 1 calc R . . H42C H 0.0230 0.1449 0.1227 0.173 Uiso 1 1 calc R . . Pd1 Pd 0.48861(3) 0.115888(10) 0.142134(10) 0.03694(9) Uani 1 1 d . . . N5 N 0.6063(3) 0.06227(11) 0.08275(11) 0.0377(6) Uani 1 1 d . . . N1 N 0.5085(3) 0.12961(11) 0.00894(10) 0.0388(6) Uani 1 1 d . . . N4 N 0.5598(3) 0.01848(11) 0.25958(11) 0.0437(6) Uani 1 1 d . . . C12 C 0.6727(4) 0.04004(15) -0.02076(15) 0.0489(8) Uani 1 1 d . . . H12 H 0.6660 0.0497 -0.0642 0.059 Uiso 1 1 calc R . . C1 C 0.4382(3) 0.15967(14) 0.05704(13) 0.0379(7) Uani 1 1 d . . . C2 C 0.6100(3) 0.05903(14) 0.20764(13) 0.0401(7) Uani 1 1 d . . . C6 C 0.6363(4) -0.03842(16) 0.25756(16) 0.0562(9) Uani 1 1 d . . . H6 H 0.6340 -0.0693 0.2895 0.067 Uiso 1 1 calc R . . C9 C 0.6891(3) 0.01313(14) 0.10662(14) 0.0410(7) Uani 1 1 d . . . C13 C 0.5993(3) 0.07539(13) 0.02180(13) 0.0389(7) Uani 1 1 d . . . C22 C 0.2760(3) 0.25653(14) 0.05633(13) 0.0405(7) Uani 1 1 d . . . N2 N 0.3666(3) 0.20865(11) 0.02722(11) 0.0394(6) Uani 1 1 d . . . N3 N 0.6848(3) 0.00841(12) 0.16908(12) 0.0462(6) Uani 1 1 d . . . C7 C 0.4779(4) 0.15968(16) -0.04782(13) 0.0471(8) Uani 1 1 d . . . H7 H 0.5129 0.1473 -0.0872 0.057 Uiso 1 1 calc R . . C10 C 0.7680(4) -0.02548(15) 0.06566(16) 0.0497(8) Uani 1 1 d . . . H10 H 0.8266 -0.0606 0.0810 0.060 Uiso 1 1 calc R . . C27 C 0.3495(4) 0.31153(15) 0.07703(15) 0.0500(8) Uani 1 1 d . . . C16 C 0.4270(4) 0.02693(14) 0.29514(14) 0.0461(8) Uani 1 1 d . . . C43 C 0.7436(4) 0.10028(16) 0.23499(16) 0.0549(9) Uani 1 1 d . . . H0A H 0.7801 0.1276 0.2021 0.082 Uiso 1 1 calc R . . H0B H 0.8287 0.0734 0.2513 0.082 Uiso 1 1 calc R . . H0C H 0.7072 0.1262 0.2690 0.082 Uiso 1 1 calc R . . C5 C 0.7132(4) -0.04530(16) 0.20651(17) 0.0604(9) Uani 1 1 d . . . H5 H 0.7761 -0.0801 0.1968 0.073 Uiso 1 1 calc R . . C8 C 0.3905(4) 0.20898(16) -0.03688(14) 0.0483(8) Uani 1 1 d . . . H8 H 0.3514 0.2389 -0.0668 0.058 Uiso 1 1 calc R . . C23 C 0.1176(4) 0.24608(16) 0.05945(16) 0.0564(9) Uani 1 1 d . . . C21 C 0.2809(4) 0.00879(15) 0.26988(14) 0.0484(8) Uani 1 1 d . . . C28 C 0.5225(4) 0.32190(17) 0.07299(18) 0.0638(10) Uani 1 1 d . . . H28 H 0.5687 0.2808 0.0611 0.077 Uiso 1 1 calc R . . C11 C 0.7582(4) -0.01130(15) 0.00346(16) 0.0532(9) Uani 1 1 d . . . H11 H 0.8112 -0.0371 -0.0244 0.064 Uiso 1 1 calc R . . C25 C 0.1008(5) 0.3482(2) 0.1059(2) 0.0836(13) Uani 1 1 d . . . H25 H 0.0393 0.3803 0.1226 0.100 Uiso 1 1 calc R . . C18 C 0.3172(6) 0.05405(19) 0.39170(18) 0.0784(12) Uani 1 1 d . . . H18 H 0.3280 0.0693 0.4335 0.094 Uiso 1 1 calc R . . C17 C 0.4486(5) 0.04927(16) 0.35708(15) 0.0593(9) Uani 1 1 d . . . C29 C 0.5997(6) 0.3410(3) 0.1349(2) 0.127(2) Uani 1 1 d . . . H29A H 0.7107 0.3469 0.1304 0.190 Uiso 1 1 calc R . . H29B H 0.5842 0.3082 0.1660 0.190 Uiso 1 1 calc R . . H29C H 0.5545 0.3805 0.1487 0.190 Uiso 1 1 calc R . . C26 C 0.2567(5) 0.35719(18) 0.10247(18) 0.0707(11) Uani 1 1 d . . . H26 H 0.3023 0.3953 0.1177 0.085 Uiso 1 1 calc R . . C19 C 0.1734(5) 0.0373(2) 0.3670(2) 0.0778(12) Uani 1 1 d . . . H19 H 0.0862 0.0411 0.3916 0.093 Uiso 1 1 calc R . . C31 C 0.0396(4) 0.18565(19) 0.0365(2) 0.0764(12) Uani 1 1 d . . . H31 H 0.1225 0.1560 0.0245 0.092 Uiso 1 1 calc R . . C24 C 0.0334(5) 0.2937(2) 0.0856(2) 0.0787(12) Uani 1 1 d . . . H24 H -0.0744 0.2880 0.0895 0.094 Uiso 1 1 calc R . . C20 C 0.1549(4) 0.01512(18) 0.30690(18) 0.0671(10) Uani 1 1 d . . . H20 H 0.0545 0.0038 0.2902 0.081 Uiso 1 1 calc R . . C30 C 0.5555(6) 0.3688(3) 0.0224(3) 0.134(2) Uani 1 1 d . . . H30A H 0.6676 0.3740 0.0206 0.201 Uiso 1 1 calc R . . H30B H 0.5085 0.4093 0.0318 0.201 Uiso 1 1 calc R . . H30C H 0.5117 0.3534 -0.0181 0.201 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 C35 0.049(2) 0.072(3) 0.053(2) -0.0010(18) 0.0055(16) -0.0075(18) C44 0.074(2) 0.058(2) 0.0475(19) -0.0002(17) 0.0177(17) 0.0198(19) O1 0.143(3) 0.128(3) 0.0648(19) 0.0127(19) 0.007(2) -0.031(2) C39 0.114(4) 0.089(3) 0.038(2) -0.001(2) -0.002(2) -0.030(3) C37 0.067(3) 0.143(4) 0.070(3) 0.005(3) -0.012(2) 0.003(3) C38 0.109(4) 0.112(4) 0.127(4) 0.014(4) -0.031(3) -0.004(3) C41 0.169(6) 0.133(5) 0.097(4) 0.001(4) -0.010(4) -0.075(4) C46 0.157(5) 0.079(3) 0.078(3) 0.004(3) -0.010(4) 0.000(3) C47 0.132(5) 0.152(5) 0.093(4) 0.028(4) 0.036(4) -0.007(4) C36 0.152(5) 0.080(3) 0.088(3) -0.020(3) -0.003(3) -0.015(3) C45 0.142(5) 0.099(4) 0.111(4) -0.013(3) -0.016(4) 0.002(4) C48 0.153(6) 0.197(7) 0.113(5) 0.022(5) 0.024(4) -0.073(5) C40 0.234(8) 0.086(4) 0.142(5) -0.011(4) -0.073(5) -0.028(4) C42 0.111(4) 0.110(4) 0.121(4) 0.042(3) -0.019(3) -0.051(3) Pd1 0.04010(14) 0.03579(14) 0.03540(12) -0.00022(10) 0.00620(9) 0.00334(11) N5 0.0377(14) 0.0350(14) 0.0410(14) -0.0047(11) 0.0064(11) 0.0010(11) N1 0.0417(14) 0.0413(15) 0.0336(13) -0.0018(11) 0.0045(10) -0.0003(11) N4 0.0444(15) 0.0410(15) 0.0456(14) 0.0084(12) 0.0023(12) 0.0032(12) C12 0.052(2) 0.052(2) 0.0441(18) -0.0101(15) 0.0110(15) -0.0042(16) C1 0.0352(16) 0.0365(17) 0.0422(16) 0.0029(13) 0.0035(13) -0.0030(13) C2 0.0408(17) 0.0393(17) 0.0405(16) 0.0026(13) 0.0052(13) 0.0045(14) C6 0.062(2) 0.047(2) 0.060(2) 0.0147(17) 0.0065(18) 0.0120(17) C9 0.0370(17) 0.0369(18) 0.0497(18) -0.0042(14) 0.0072(14) -0.0011(14) C13 0.0396(17) 0.0357(17) 0.0421(17) -0.0059(13) 0.0078(13) -0.0079(14) C22 0.0423(18) 0.0402(18) 0.0392(16) 0.0083(14) 0.0044(13) 0.0066(14) N2 0.0392(14) 0.0403(15) 0.0388(14) 0.0036(11) 0.0033(11) -0.0023(11) N3 0.0508(16) 0.0397(15) 0.0487(16) 0.0039(12) 0.0077(12) 0.0094(12) C7 0.055(2) 0.053(2) 0.0340(16) 0.0013(14) 0.0080(14) -0.0046(17) C10 0.0458(19) 0.0403(19) 0.064(2) -0.0069(16) 0.0094(16) 0.0053(15) C27 0.053(2) 0.047(2) 0.0495(18) -0.0013(15) 0.0011(15) 0.0014(16) C16 0.057(2) 0.0390(18) 0.0433(17) 0.0112(14) 0.0093(15) 0.0070(15) C43 0.051(2) 0.056(2) 0.057(2) 0.0062(16) -0.0007(16) -0.0051(16) C5 0.068(2) 0.049(2) 0.066(2) 0.0089(18) 0.0134(19) 0.0200(18) C8 0.051(2) 0.056(2) 0.0370(17) 0.0091(15) 0.0024(14) -0.0012(17) C23 0.046(2) 0.053(2) 0.071(2) 0.0036(18) 0.0091(17) 0.0039(17) C21 0.050(2) 0.048(2) 0.0476(18) 0.0101(15) 0.0114(15) 0.0085(16) C28 0.058(2) 0.058(2) 0.076(2) -0.012(2) 0.0012(19) -0.0103(18) C11 0.054(2) 0.047(2) 0.060(2) -0.0172(17) 0.0177(17) 0.0003(17) C25 0.073(3) 0.078(3) 0.101(3) -0.016(3) 0.020(2) 0.029(3) C18 0.122(4) 0.067(3) 0.048(2) -0.0004(19) 0.029(2) 0.007(3) C17 0.085(3) 0.050(2) 0.0426(19) 0.0036(16) 0.0052(19) -0.0026(19) C29 0.076(3) 0.211(7) 0.091(3) -0.018(4) -0.019(3) -0.008(4) C26 0.080(3) 0.051(2) 0.081(3) -0.015(2) 0.001(2) 0.005(2) C19 0.082(3) 0.086(3) 0.069(3) 0.010(2) 0.036(2) 0.021(2) C31 0.041(2) 0.067(3) 0.122(4) -0.005(2) 0.016(2) -0.0099(19) C24 0.052(2) 0.080(3) 0.106(3) -0.009(3) 0.019(2) 0.008(2) C20 0.061(2) 0.077(3) 0.066(2) 0.014(2) 0.0169(19) 0.011(2) C30 0.100(4) 0.179(6) 0.124(5) 0.046(4) 0.012(3) -0.059(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C35 C37 1.512(5) . ? C35 C21 1.514(4) . ? C35 C36 1.529(6) . ? C35 H35 1.0000 . ? C44 Pd1 2.046(3) . ? C44 H10A 0.9800 . ? C44 H10B 0.9800 . ? C44 H10C 0.9800 . ? O1 C46 1.376(6) . ? O1 C47 1.402(6) . ? C39 C17 1.512(5) . ? C39 C40 1.517(6) . ? C39 C38 1.523(6) . ? C39 H39 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 C31 1.522(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C46 C45 1.483(7) . ? C46 H20A 0.9900 . ? C46 H20B 0.9900 . ? C47 C48 1.459(7) . ? C47 H20C 0.9900 . ? C47 H20D 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C45 H20E 0.9800 . ? C45 H20F 0.9800 . ? C45 H20G 0.9800 . ? C48 H20H 0.9800 . ? C48 H20I 0.9800 . ? C48 H20J 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C42 C31 1.504(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Pd1 N5 2.029(2) . ? Pd1 C1 2.067(3) . ? Pd1 C2 2.085(3) . ? N5 C13 1.331(3) . ? N5 C9 1.350(4) . ? N1 C7 1.383(4) . ? N1 C1 1.384(3) . ? N1 C13 1.413(4) . ? N4 C6 1.382(4) . ? N4 C16 1.429(4) . ? N4 C2 1.493(4) . ? C12 C13 1.368(4) . ? C12 C11 1.401(5) . ? C12 H12 0.9500 . ? C1 N2 1.352(4) . ? C2 N3 1.525(4) . ? C2 C43 1.539(4) . ? C6 C5 1.322(5) . ? C6 H6 0.9500 . ? C9 N3 1.343(4) . ? C9 C10 1.408(4) . ? C22 C27 1.391(4) . ? C22 C23 1.395(4) . ? C22 N2 1.450(4) . ? N2 C8 1.400(4) . ? N3 C5 1.408(4) . ? C7 C8 1.323(4) . ? C7 H7 0.9500 . ? C10 C11 1.362(4) . ? C10 H10 0.9500 . ? C27 C26 1.393(5) . ? C27 C28 1.522(5) . ? C16 C21 1.399(4) . ? C16 C17 1.409(4) . ? C43 H0A 0.9800 . ? C43 H0B 0.9800 . ? C43 H0C 0.9800 . ? C5 H5 0.9500 . ? C8 H8 0.9500 . ? C23 C24 1.386(5) . ? C23 C31 1.520(5) . ? C21 C20 1.394(5) . ? C28 C29 1.502(5) . ? C28 C30 1.512(6) . ? C28 H28 1.0000 . ? C11 H11 0.9500 . ? C25 C24 1.357(6) . ? C25 C26 1.370(6) . ? C25 H25 0.9500 . ? C18 C19 1.369(6) . ? C18 C17 1.400(5) . ? C18 H18 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C26 H26 0.9500 . ? C19 C20 1.369(5) . ? C19 H19 0.9500 . ? C31 H31 1.0000 . ? C24 H24 0.9500 . ? C20 H20 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 C35 C21 112.5(3) . . ? C37 C35 C36 110.9(4) . . ? C21 C35 C36 110.3(3) . . ? C37 C35 H35 107.6 . . ? C21 C35 H35 107.6 . . ? C36 C35 H35 107.6 . . ? Pd1 C44 H10A 109.5 . . ? Pd1 C44 H10B 109.5 . . ? H10A C44 H10B 109.5 . . ? Pd1 C44 H10C 109.5 . . ? H10A C44 H10C 109.5 . . ? H10B C44 H10C 109.5 . . ? C46 O1 C47 114.3(4) . . ? C17 C39 C40 113.6(4) . . ? C17 C39 C38 111.9(3) . . ? C40 C39 C38 109.2(4) . . ? C17 C39 H39 107.3 . . ? C40 C39 H39 107.3 . . ? C38 C39 H39 107.3 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C31 C41 H41A 109.5 . . ? C31 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C31 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O1 C46 C45 109.6(4) . . ? O1 C46 H20A 109.8 . . ? C45 C46 H20A 109.8 . . ? O1 C46 H20B 109.8 . . ? C45 C46 H20B 109.8 . . ? H20A C46 H20B 108.2 . . ? O1 C47 C48 111.7(5) . . ? O1 C47 H20C 109.3 . . ? C48 C47 H20C 109.3 . . ? O1 C47 H20D 109.3 . . ? C48 C47 H20D 109.3 . . ? H20C C47 H20D 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C46 C45 H20E 109.5 . . ? C46 C45 H20F 109.5 . . ? H20E C45 H20F 109.5 . . ? C46 C45 H20G 109.5 . . ? H20E C45 H20G 109.5 . . ? H20F C45 H20G 109.5 . . ? C47 C48 H20H 109.5 . . ? C47 C48 H20I 109.5 . . ? H20H C48 H20I 109.5 . . ? C47 C48 H20J 109.5 . . ? H20H C48 H20J 109.5 . . ? H20I C48 H20J 109.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C31 C42 H42A 109.5 . . ? C31 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C31 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 Pd1 C44 178.32(12) . . ? N5 Pd1 C1 77.79(10) . . ? C44 Pd1 C1 103.76(12) . . ? N5 Pd1 C2 80.95(10) . . ? C44 Pd1 C2 97.59(12) . . ? C1 Pd1 C2 157.38(11) . . ? C13 N5 C9 121.6(2) . . ? C13 N5 Pd1 120.09(19) . . ? C9 N5 Pd1 118.32(19) . . ? C7 N1 C1 111.7(2) . . ? C7 N1 C13 128.5(2) . . ? C1 N1 C13 119.8(2) . . ? C6 N4 C16 122.0(3) . . ? C6 N4 C2 108.7(2) . . ? C16 N4 C2 127.2(2) . . ? C13 C12 C11 116.1(3) . . ? C13 C12 H12 122.0 . . ? C11 C12 H12 122.0 . . ? N2 C1 N1 102.4(2) . . ? N2 C1 Pd1 145.9(2) . . ? N1 C1 Pd1 111.60(19) . . ? N4 C2 N3 98.5(2) . . ? N4 C2 C43 107.1(2) . . ? N3 C2 C43 105.9(2) . . ? N4 C2 Pd1 132.6(2) . . ? N3 C2 Pd1 105.04(17) . . ? C43 C2 Pd1 105.08(19) . . ? C5 C6 N4 112.9(3) . . ? C5 C6 H6 123.5 . . ? N4 C6 H6 123.5 . . ? N3 C9 N5 112.8(3) . . ? N3 C9 C10 128.3(3) . . ? N5 C9 C10 118.9(3) . . ? N5 C13 C12 122.8(3) . . ? N5 C13 N1 110.7(2) . . ? C12 C13 N1 126.5(3) . . ? C27 C22 C23 123.4(3) . . ? C27 C22 N2 118.6(3) . . ? C23 C22 N2 117.9(3) . . ? C1 N2 C8 112.0(3) . . ? C1 N2 C22 125.7(2) . . ? C8 N2 C22 122.3(2) . . ? C9 N3 C5 127.7(3) . . ? C9 N3 C2 121.6(2) . . ? C5 N3 C2 109.3(2) . . ? C8 C7 N1 107.0(3) . . ? C8 C7 H7 126.5 . . ? N1 C7 H7 126.5 . . ? C11 C10 C9 118.4(3) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C22 C27 C26 116.6(3) . . ? C22 C27 C28 122.4(3) . . ? C26 C27 C28 121.0(3) . . ? C21 C16 C17 121.3(3) . . ? C21 C16 N4 119.9(3) . . ? C17 C16 N4 118.6(3) . . ? C2 C43 H0A 109.5 . . ? C2 C43 H0B 109.5 . . ? H0A C43 H0B 109.5 . . ? C2 C43 H0C 109.5 . . ? H0A C43 H0C 109.5 . . ? H0B C43 H0C 109.5 . . ? C6 C5 N3 107.5(3) . . ? C6 C5 H5 126.2 . . ? N3 C5 H5 126.2 . . ? C7 C8 N2 106.9(3) . . ? C7 C8 H8 126.6 . . ? N2 C8 H8 126.6 . . ? C24 C23 C22 116.5(3) . . ? C24 C23 C31 121.0(3) . . ? C22 C23 C31 122.5(3) . . ? C20 C21 C16 118.4(3) . . ? C20 C21 C35 119.8(3) . . ? C16 C21 C35 121.8(3) . . ? C29 C28 C30 111.1(4) . . ? C29 C28 C27 112.0(3) . . ? C30 C28 C27 111.5(3) . . ? C29 C28 H28 107.3 . . ? C30 C28 H28 107.3 . . ? C27 C28 H28 107.3 . . ? C10 C11 C12 122.2(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C19 C18 C17 121.8(4) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C17 C16 117.2(4) . . ? C18 C17 C39 120.9(3) . . ? C16 C17 C39 121.8(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C42 C31 C23 112.3(4) . . ? C42 C31 C41 110.3(4) . . ? C23 C31 C41 111.0(4) . . ? C42 C31 H31 107.7 . . ? C23 C31 H31 107.7 . . ? C41 C31 H31 107.7 . . ? C25 C24 C23 121.8(4) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C19 C20 C21 121.1(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.361 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.064