# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Joel Rosenthal' _publ_contact_author_email rosenthal@mail.chem.udel.edu loop_ _publ_author_name 'Piyal Ariyananda' 'Glenn Yap' 'Joel Rosenthal' data_joer011 _database_code_depnum_ccdc_archive 'CCDC 871921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H50 N4 O2 Pd' _chemical_formula_weight 665.19 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 14.176(4) _cell_length_b 8.709(2) _cell_length_c 27.584(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.076(5) _cell_angle_gamma 90.00 _cell_volume 3400.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 20.05 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 0.9693 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 42760 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8436 _reflns_number_gt 5817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. The 90 restraints arise from modeling the disorder from the two solvent molecules in the asymmetric unit. ; _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^)+(0.0598P)^2^+1.1016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8436 _refine_ls_number_parameters 387 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.004 _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 Pd Pd 0.22561(2) 0.41881(3) 0.154585(10) 0.03548(10) Uani 1 1 d . . . N1 N 0.4210(2) 0.2412(4) 0.17734(12) 0.0462(8) Uani 1 1 d . . . N2 N 0.3339(2) 0.2634(4) 0.23751(12) 0.0411(8) Uani 1 1 d . . . N3 N 0.0514(2) 0.2250(4) 0.19259(13) 0.0448(8) Uani 1 1 d . . . N4 N 0.1662(2) 0.2589(4) 0.24457(12) 0.0407(8) Uani 1 1 d . . . C1 C 0.3370(3) 0.3049(5) 0.18994(15) 0.0400(9) Uani 1 1 d . . . C2 C 0.4657(3) 0.1643(6) 0.21629(18) 0.0598(13) Uani 1 1 d . . . H2A H 0.5237 0.1121 0.2161 0.072 Uiso 1 1 calc R . . C3 C 0.4109(3) 0.1784(6) 0.25411(18) 0.0551(12) Uani 1 1 d . . . H3A H 0.4226 0.1384 0.2855 0.066 Uiso 1 1 calc R . . C4 C 0.4178(3) 0.1453(6) 0.09453(17) 0.0494(11) Uani 1 1 d . . . C5 C 0.4496(3) 0.1546(6) 0.04755(18) 0.0547(12) Uani 1 1 d . . . H5A H 0.4237 0.0880 0.0235 0.066 Uiso 1 1 calc R . . C6 C 0.5183(3) 0.2592(6) 0.03527(17) 0.0535(12) Uani 1 1 d . . . C7 C 0.5588(3) 0.3493(6) 0.07196(19) 0.0560(12) Uani 1 1 d . . . H7A H 0.6081 0.4165 0.0647 0.067 Uiso 1 1 calc R . . C8 C 0.5293(3) 0.3442(6) 0.11942(18) 0.0513(11) Uani 1 1 d . . . C9 C 0.4566(3) 0.2438(5) 0.12907(16) 0.0460(10) Uani 1 1 d . . . C10 C 0.3434(4) 0.0291(7) 0.1067(2) 0.0777(18) Uani 1 1 d . . . H10A H 0.2866 0.0823 0.1154 0.117 Uiso 1 1 calc R . . H10B H 0.3669 -0.0339 0.1337 0.117 Uiso 1 1 calc R . . H10C H 0.3289 -0.0357 0.0786 0.117 Uiso 1 1 calc R . . C11 C 0.5465(4) 0.2751(7) -0.01660(19) 0.0717(16) Uani 1 1 d . . . H11A H 0.5122 0.2005 -0.0368 0.108 Uiso 1 1 calc R . . H11B H 0.6138 0.2571 -0.0180 0.108 Uiso 1 1 calc R . . H11C H 0.5316 0.3778 -0.0282 0.108 Uiso 1 1 calc R . . C12 C 0.5756(4) 0.4475(7) 0.1578(2) 0.0743(17) Uani 1 1 d . . . H12A H 0.6290 0.4996 0.1446 0.111 Uiso 1 1 calc R . . H12B H 0.5973 0.3863 0.1856 0.111 Uiso 1 1 calc R . . H12C H 0.5303 0.5229 0.1678 0.111 Uiso 1 1 calc R . . C13 C 0.2561(3) 0.3096(5) 0.26684(15) 0.0434(10) Uani 1 1 d . . . H13A H 0.2650 0.2649 0.2994 0.052 Uiso 1 1 calc R . . H13B H 0.2557 0.4216 0.2702 0.052 Uiso 1 1 calc R . . C14 C 0.1379(3) 0.2947(5) 0.19781(14) 0.0384(9) Uani 1 1 d . . . C15 C 0.0294(3) 0.1493(6) 0.23489(17) 0.0558(12) Uani 1 1 d . . . H15A H -0.0261 0.0936 0.2397 0.067 Uiso 1 1 calc R . . C16 C 0.1014(3) 0.1700(6) 0.26738(17) 0.0525(12) Uani 1 1 d . . . H16A H 0.1068 0.1318 0.2993 0.063 Uiso 1 1 calc R . . C17 C 0.0100(3) 0.1108(5) 0.11355(19) 0.0524(11) Uani 1 1 d . . . C18 C -0.0499(4) 0.1067(6) 0.07191(19) 0.0596(13) Uani 1 1 d . . . H18A H -0.0367 0.0375 0.0470 0.072 Uiso 1 1 calc R . . C19 C -0.1277(4) 0.2007(6) 0.06599(19) 0.0589(13) Uani 1 1 d . . . C20 C -0.1463(3) 0.3017(6) 0.10235(19) 0.0583(12) Uani 1 1 d . . . H20A H -0.1997 0.3654 0.0987 0.070 Uiso 1 1 calc R . . C21 C -0.0878(3) 0.3128(5) 0.14500(17) 0.0489(11) Uani 1 1 d . . . C22 C -0.0085(3) 0.2189(5) 0.14916(15) 0.0436(10) Uani 1 1 d . . . C23 C 0.0923(4) 0.0004(7) 0.1209(2) 0.0802(18) Uani 1 1 d . . . H23A H 0.1499 0.0579 0.1281 0.120 Uiso 1 1 calc R . . H23B H 0.0986 -0.0593 0.0916 0.120 Uiso 1 1 calc R . . H23C H 0.0809 -0.0681 0.1477 0.120 Uiso 1 1 calc R . . C24 C -0.1913(5) 0.1960(8) 0.0198(2) 0.0866(19) Uani 1 1 d . . . H24A H -0.2212 0.2953 0.0146 0.130 Uiso 1 1 calc R . . H24B H -0.2395 0.1181 0.0229 0.130 Uiso 1 1 calc R . . H24C H -0.1539 0.1716 -0.0076 0.130 Uiso 1 1 calc R . . C25 C -0.1114(4) 0.4254(6) 0.1840(2) 0.0651(14) Uani 1 1 d . . . H25A H -0.1050 0.3754 0.2154 0.098 Uiso 1 1 calc R . . H25B H -0.1759 0.4609 0.1782 0.098 Uiso 1 1 calc R . . H25C H -0.0686 0.5122 0.1835 0.098 Uiso 1 1 calc R . . C26 C 0.1147(3) 0.5380(6) 0.11947(16) 0.0516(11) Uani 1 1 d . . . H26A H 0.0596 0.5332 0.1388 0.077 Uiso 1 1 calc R . . H26B H 0.0999 0.4920 0.0880 0.077 Uiso 1 1 calc R . . H26C H 0.1329 0.6443 0.1153 0.077 Uiso 1 1 calc R . . C27 C 0.3105(3) 0.5517(5) 0.11217(16) 0.0489(11) Uani 1 1 d . . . H27A H 0.3758 0.5426 0.1242 0.073 Uiso 1 1 calc R . . H27B H 0.2909 0.6582 0.1137 0.073 Uiso 1 1 calc R . . H27C H 0.3045 0.5162 0.0788 0.073 Uiso 1 1 calc R . . O1 O -0.2204(3) 0.6405(6) 0.06492(18) 0.1023(15) Uani 1 1 d DU . . C28 C -0.1217(5) 0.6774(9) 0.0663(3) 0.103(2) Uani 1 1 d DU . . H28A H -0.0848 0.6018 0.0856 0.124 Uiso 1 1 calc R . . H28B H -0.1102 0.7796 0.0803 0.124 Uiso 1 1 calc R . . C29 C -0.0971(6) 0.6731(10) 0.0151(3) 0.115(2) Uani 1 1 d DU . . H29A H -0.0821 0.5683 0.0051 0.138 Uiso 1 1 calc R . . H29B H -0.0430 0.7399 0.0097 0.138 Uiso 1 1 calc R . . C30 C -0.1844(6) 0.7306(9) -0.0118(3) 0.102(2) Uani 1 1 d DU . . H30A H -0.1830 0.8426 -0.0153 0.123 Uiso 1 1 calc R . . H30B H -0.1922 0.6837 -0.0441 0.123 Uiso 1 1 calc R . . C31 C -0.2590(6) 0.6826(12) 0.0191(3) 0.126(3) Uani 1 1 d DU . . H31A H -0.3039 0.7670 0.0225 0.151 Uiso 1 1 calc R . . H31B H -0.2932 0.5954 0.0042 0.151 Uiso 1 1 calc R . . O2 O 0.6878(10) 0.0471(14) 0.1908(5) 0.281(6) Uani 1 1 d DU . . C32 C 0.7809(9) 0.0140(14) 0.2121(5) 0.184(4) Uani 1 1 d DU . . H32A H 0.8278 0.0892 0.2024 0.221 Uiso 1 1 calc R . . H32B H 0.7815 0.0082 0.2476 0.221 Uiso 1 1 calc R . . C33 C 0.7947(11) -0.1304(17) 0.1909(6) 0.240(6) Uani 1 1 d DU . . H33A H 0.8229 -0.2017 0.2151 0.287 Uiso 1 1 calc R . . H33B H 0.8371 -0.1214 0.1642 0.287 Uiso 1 1 calc R . . C34 C 0.7003(14) -0.1874(17) 0.1726(7) 0.287(8) Uani 1 1 d DU . . H34A H 0.7053 -0.2743 0.1503 0.344 Uiso 1 1 calc R . . H34B H 0.6601 -0.2154 0.1990 0.344 Uiso 1 1 calc R . . C35 C 0.6685(13) -0.052(2) 0.1482(7) 0.302(9) Uani 1 1 d DU . . H35A H 0.6013 -0.0554 0.1378 0.362 Uiso 1 1 calc R . . H35B H 0.7065 -0.0248 0.1208 0.362 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 Pd 0.04093(18) 0.03604(17) 0.02997(16) 0.00156(13) 0.00644(11) -0.00141(14) N1 0.0419(19) 0.057(2) 0.0405(19) 0.0065(17) 0.0098(15) 0.0051(17) N2 0.0395(18) 0.048(2) 0.0361(17) 0.0023(15) 0.0063(14) 0.0009(16) N3 0.0418(19) 0.050(2) 0.043(2) 0.0115(16) 0.0064(15) -0.0042(16) N4 0.0391(18) 0.047(2) 0.0363(17) 0.0059(15) 0.0086(14) 0.0005(16) C1 0.042(2) 0.042(2) 0.037(2) 0.0026(17) 0.0091(17) -0.0049(18) C2 0.047(3) 0.077(4) 0.057(3) 0.015(3) 0.008(2) 0.016(3) C3 0.047(3) 0.069(3) 0.050(3) 0.015(2) 0.004(2) 0.010(2) C4 0.045(2) 0.052(3) 0.053(3) 0.001(2) 0.011(2) -0.001(2) C5 0.055(3) 0.058(3) 0.052(3) 0.000(2) 0.014(2) 0.002(2) C6 0.055(3) 0.055(3) 0.052(3) 0.008(2) 0.020(2) 0.009(2) C7 0.050(3) 0.051(3) 0.070(3) 0.006(2) 0.028(2) -0.001(2) C8 0.046(3) 0.050(3) 0.059(3) 0.001(2) 0.016(2) 0.004(2) C9 0.042(2) 0.051(3) 0.046(2) 0.007(2) 0.0146(19) 0.004(2) C10 0.078(4) 0.079(4) 0.079(4) -0.013(3) 0.028(3) -0.031(3) C11 0.073(4) 0.091(4) 0.054(3) 0.011(3) 0.025(3) 0.007(3) C12 0.055(3) 0.085(4) 0.085(4) -0.021(3) 0.023(3) -0.016(3) C13 0.043(2) 0.056(3) 0.0309(19) 0.0014(18) 0.0058(17) 0.002(2) C14 0.036(2) 0.043(2) 0.036(2) 0.0028(17) 0.0061(16) 0.0040(17) C15 0.046(3) 0.068(3) 0.055(3) 0.022(2) 0.008(2) -0.011(2) C16 0.047(3) 0.068(3) 0.044(3) 0.018(2) 0.010(2) -0.002(2) C17 0.051(3) 0.047(3) 0.060(3) 0.003(2) 0.009(2) -0.003(2) C18 0.073(4) 0.051(3) 0.055(3) -0.010(2) 0.006(3) -0.010(3) C19 0.060(3) 0.055(3) 0.060(3) -0.001(2) -0.008(2) -0.012(2) C20 0.049(3) 0.056(3) 0.070(3) 0.001(2) -0.005(2) -0.004(2) C21 0.042(2) 0.052(3) 0.053(3) 0.000(2) 0.006(2) -0.001(2) C22 0.042(2) 0.047(2) 0.042(2) 0.0065(19) 0.0034(18) -0.0055(19) C23 0.074(4) 0.075(4) 0.092(5) -0.009(3) 0.005(3) 0.023(3) C24 0.096(5) 0.085(4) 0.075(4) -0.010(3) -0.028(4) -0.006(4) C25 0.060(3) 0.074(4) 0.062(3) -0.013(3) 0.005(2) 0.009(3) C26 0.055(3) 0.058(3) 0.042(2) 0.009(2) 0.008(2) 0.009(2) C27 0.055(3) 0.054(3) 0.038(2) 0.0085(19) 0.0068(19) -0.008(2) O1 0.085(3) 0.118(4) 0.104(3) 0.042(3) 0.004(3) 0.005(3) C28 0.096(5) 0.101(5) 0.111(5) 0.039(5) -0.012(4) -0.015(4) C29 0.116(5) 0.108(6) 0.125(6) 0.002(5) 0.032(5) 0.003(5) C30 0.146(6) 0.088(5) 0.073(4) -0.004(4) 0.010(4) -0.004(5) C31 0.115(5) 0.165(8) 0.095(5) 0.036(6) -0.014(4) -0.010(6) O2 0.304(12) 0.245(10) 0.292(13) -0.078(9) -0.007(11) 0.118(10) C32 0.184(10) 0.140(9) 0.238(12) -0.037(8) 0.106(8) -0.049(8) C33 0.256(14) 0.182(12) 0.280(16) -0.064(11) 0.007(12) 0.065(10) C34 0.37(2) 0.150(9) 0.34(2) -0.052(11) -0.037(16) -0.068(12) C35 0.320(15) 0.256(15) 0.323(19) -0.123(12) -0.046(12) 0.199(13) _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 Pd C1 2.065(4) . ? Pd C14 2.072(4) . ? Pd C27 2.075(4) . ? Pd C26 2.079(4) . ? N1 C1 1.374(5) . ? N1 C2 1.390(6) . ? N1 C9 1.449(5) . ? N2 C1 1.364(5) . ? N2 C3 1.377(6) . ? N2 C13 1.460(5) . ? N3 C14 1.369(5) . ? N3 C15 1.390(5) . ? N3 C22 1.431(5) . ? N4 C14 1.367(5) . ? N4 C16 1.379(5) . ? N4 C13 1.452(5) . ? C2 C3 1.339(6) . ? C4 C9 1.374(6) . ? C4 C5 1.397(6) . ? C4 C10 1.513(7) . ? C5 C6 1.389(7) . ? C6 C7 1.382(7) . ? C6 C11 1.513(6) . ? C7 C8 1.396(6) . ? C8 C9 1.389(6) . ? C8 C12 1.512(7) . ? C15 C16 1.334(7) . ? C17 C18 1.392(7) . ? C17 C22 1.395(6) . ? C17 C23 1.517(7) . ? C18 C19 1.377(7) . ? C19 C20 1.370(7) . ? C19 C24 1.522(7) . ? C20 C21 1.406(7) . ? C21 C22 1.390(6) . ? C21 C25 1.506(7) . ? O1 C31 1.399(8) . ? O1 C28 1.433(7) . ? C28 C29 1.474(9) . ? C29 C30 1.495(9) . ? C30 C31 1.455(9) . ? O2 C32 1.444(12) . ? O2 C35 1.471(14) . ? C32 C33 1.404(13) . ? C33 C34 1.490(14) . ? C34 C35 1.422(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd C14 86.86(15) . . ? C1 Pd C27 94.71(17) . . ? C14 Pd C27 177.52(17) . . ? C1 Pd C26 178.76(18) . . ? C14 Pd C26 93.80(17) . . ? C27 Pd C26 84.60(19) . . ? C1 N1 C2 111.3(3) . . ? C1 N1 C9 125.1(4) . . ? C2 N1 C9 123.4(4) . . ? C1 N2 C3 113.3(3) . . ? C1 N2 C13 121.7(3) . . ? C3 N2 C13 125.0(4) . . ? C14 N3 C15 111.2(4) . . ? C14 N3 C22 126.3(3) . . ? C15 N3 C22 122.4(4) . . ? C14 N4 C16 112.9(4) . . ? C14 N4 C13 122.5(3) . . ? C16 N4 C13 124.6(4) . . ? N2 C1 N1 102.1(3) . . ? N2 C1 Pd 121.2(3) . . ? N1 C1 Pd 136.5(3) . . ? C3 C2 N1 107.4(4) . . ? C2 C3 N2 105.8(4) . . ? C9 C4 C5 118.1(4) . . ? C9 C4 C10 121.5(4) . . ? C5 C4 C10 120.5(5) . . ? C6 C5 C4 121.9(5) . . ? C7 C6 C5 117.6(4) . . ? C7 C6 C11 121.3(5) . . ? C5 C6 C11 121.0(5) . . ? C6 C7 C8 122.3(4) . . ? C9 C8 C7 117.6(5) . . ? C9 C8 C12 122.6(4) . . ? C7 C8 C12 119.8(5) . . ? C4 C9 C8 122.2(4) . . ? C4 C9 N1 118.8(4) . . ? C8 C9 N1 119.0(4) . . ? N4 C13 N2 110.7(3) . . ? N4 C14 N3 102.4(3) . . ? N4 C14 Pd 120.5(3) . . ? N3 C14 Pd 137.1(3) . . ? C16 C15 N3 107.6(4) . . ? C15 C16 N4 105.9(4) . . ? C18 C17 C22 118.0(5) . . ? C18 C17 C23 121.6(5) . . ? C22 C17 C23 120.4(5) . . ? C19 C18 C17 122.2(5) . . ? C20 C19 C18 118.6(5) . . ? C20 C19 C24 120.2(5) . . ? C18 C19 C24 121.2(5) . . ? C19 C20 C21 122.0(5) . . ? C22 C21 C20 117.8(4) . . ? C22 C21 C25 122.2(4) . . ? C20 C21 C25 120.0(4) . . ? C21 C22 C17 121.3(4) . . ? C21 C22 N3 119.2(4) . . ? C17 C22 N3 119.3(4) . . ? C31 O1 C28 107.4(5) . . ? O1 C28 C29 104.4(6) . . ? C28 C29 C30 103.7(6) . . ? C31 C30 C29 102.7(6) . . ? O1 C31 C30 110.1(6) . . ? C32 O2 C35 109.6(10) . . ? C33 C32 O2 98.9(10) . . ? C32 C33 C34 107.3(12) . . ? C35 C34 C33 98.1(13) . . ? C34 C35 O2 93.9(13) . . ? 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 C3 N2 C1 N1 -0.1(5) . . . . ? C13 N2 C1 N1 178.8(4) . . . . ? C3 N2 C1 Pd 175.3(3) . . . . ? C13 N2 C1 Pd -5.7(5) . . . . ? C2 N1 C1 N2 0.1(5) . . . . ? C9 N1 C1 N2 176.4(4) . . . . ? C2 N1 C1 Pd -174.2(4) . . . . ? C9 N1 C1 Pd 2.0(7) . . . . ? C14 Pd C1 N2 -33.2(3) . . . . ? C27 Pd C1 N2 144.9(3) . . . . ? C26 Pd C1 N2 89(8) . . . . ? C14 Pd C1 N1 140.3(5) . . . . ? C27 Pd C1 N1 -41.6(5) . . . . ? C26 Pd C1 N1 -97(8) . . . . ? C1 N1 C2 C3 -0.1(6) . . . . ? C9 N1 C2 C3 -176.4(4) . . . . ? N1 C2 C3 N2 0.0(6) . . . . ? C1 N2 C3 C2 0.1(6) . . . . ? C13 N2 C3 C2 -178.9(4) . . . . ? C9 C4 C5 C6 0.0(7) . . . . ? C10 C4 C5 C6 -179.6(5) . . . . ? C4 C5 C6 C7 3.7(7) . . . . ? C4 C5 C6 C11 -175.5(5) . . . . ? C5 C6 C7 C8 -3.7(7) . . . . ? C11 C6 C7 C8 175.5(5) . . . . ? C6 C7 C8 C9 0.1(7) . . . . ? C6 C7 C8 C12 -179.1(5) . . . . ? C5 C4 C9 C8 -3.9(7) . . . . ? C10 C4 C9 C8 175.7(5) . . . . ? C5 C4 C9 N1 176.9(4) . . . . ? C10 C4 C9 N1 -3.6(7) . . . . ? C7 C8 C9 C4 3.9(7) . . . . ? C12 C8 C9 C4 -177.0(5) . . . . ? C7 C8 C9 N1 -176.9(4) . . . . ? C12 C8 C9 N1 2.2(7) . . . . ? C1 N1 C9 C4 -76.4(6) . . . . ? C2 N1 C9 C4 99.4(6) . . . . ? C1 N1 C9 C8 104.3(5) . . . . ? C2 N1 C9 C8 -79.9(6) . . . . ? C14 N4 C13 N2 -54.6(5) . . . . ? C16 N4 C13 N2 124.8(4) . . . . ? C1 N2 C13 N4 56.5(5) . . . . ? C3 N2 C13 N4 -124.6(4) . . . . ? C16 N4 C14 N3 0.6(5) . . . . ? C13 N4 C14 N3 -179.9(4) . . . . ? C16 N4 C14 Pd -177.1(3) . . . . ? C13 N4 C14 Pd 2.3(5) . . . . ? C15 N3 C14 N4 -0.4(5) . . . . ? C22 N3 C14 N4 -176.5(4) . . . . ? C15 N3 C14 Pd 176.7(4) . . . . ? C22 N3 C14 Pd 0.6(7) . . . . ? C1 Pd C14 N4 34.8(3) . . . . ? C27 Pd C14 N4 -95(4) . . . . ? C26 Pd C14 N4 -144.1(3) . . . . ? C1 Pd C14 N3 -141.9(4) . . . . ? C27 Pd C14 N3 89(4) . . . . ? C26 Pd C14 N3 39.1(5) . . . . ? C14 N3 C15 C16 0.1(6) . . . . ? C22 N3 C15 C16 176.3(4) . . . . ? N3 C15 C16 N4 0.3(6) . . . . ? C14 N4 C16 C15 -0.6(6) . . . . ? C13 N4 C16 C15 179.9(4) . . . . ? C22 C17 C18 C19 -2.7(7) . . . . ? C23 C17 C18 C19 176.4(5) . . . . ? C17 C18 C19 C20 0.2(8) . . . . ? C17 C18 C19 C24 179.0(5) . . . . ? C18 C19 C20 C21 0.6(8) . . . . ? C24 C19 C20 C21 -178.1(5) . . . . ? C19 C20 C21 C22 1.0(7) . . . . ? C19 C20 C21 C25 -179.8(5) . . . . ? C20 C21 C22 C17 -3.6(7) . . . . ? C25 C21 C22 C17 177.2(4) . . . . ? C20 C21 C22 N3 -178.6(4) . . . . ? C25 C21 C22 N3 2.2(7) . . . . ? C18 C17 C22 C21 4.4(7) . . . . ? C23 C17 C22 C21 -174.7(5) . . . . ? C18 C17 C22 N3 179.4(4) . . . . ? C23 C17 C22 N3 0.3(7) . . . . ? C14 N3 C22 C21 -104.4(5) . . . . ? C15 N3 C22 C21 79.9(6) . . . . ? C14 N3 C22 C17 80.4(6) . . . . ? C15 N3 C22 C17 -95.3(5) . . . . ? C31 O1 C28 C29 -25.7(9) . . . . ? O1 C28 C29 C30 34.3(8) . . . . ? C28 C29 C30 C31 -29.7(9) . . . . ? C28 O1 C31 C30 6.7(10) . . . . ? C29 C30 C31 O1 14.7(10) . . . . ? C35 O2 C32 C33 -18(2) . . . . ? O2 C32 C33 C34 -17.1(19) . . . . ? C32 C33 C34 C35 47.6(19) . . . . ? C33 C34 C35 O2 -52.5(17) . . . . ? C32 O2 C35 C34 47(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.850 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.094 #===END data_joer049s _database_code_depnum_ccdc_archive 'CCDC 871922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 N4 O3 Pd, 2.5(C2 H3 N)' _chemical_formula_sum 'C31 H35.50 N6.50 O3 Pd' _chemical_formula_weight 653.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.015(7) _cell_length_b 16.141(9) _cell_length_c 17.230(9) _cell_angle_alpha 101.769(18) _cell_angle_beta 110.124(17) _cell_angle_gamma 102.20(2) _cell_volume 3411(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 993 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.65 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9004 _exptl_absorpt_correction_T_max 0.9637 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 42475 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1313 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.26 _reflns_number_total 16756 _reflns_number_gt 9806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. Data-set was treated with SQUEEZE (see _platon_squeeze_details) to model 10 acetonitrile molecules located near the inversion center as diffused contributions. ; _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^)+(0.0529P)^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_number_reflns 16756 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.90201(3) 0.85334(2) 0.48627(2) 0.02877(11) Uani 1 1 d . . . Pd2 Pd 0.58643(3) 0.15722(2) 0.02809(2) 0.02899(11) Uani 1 1 d . . . O1 O 1.0495(3) 0.8893(2) 0.5878(2) 0.0341(8) Uani 1 1 d . . . O2 O 0.8995(3) 0.8747(2) 0.6080(2) 0.0385(8) Uani 1 1 d . . . O3 O 1.0578(3) 0.9300(3) 0.7243(2) 0.0460(10) Uani 1 1 d . . . O4 O 0.4685(3) 0.1173(2) -0.0960(2) 0.0358(8) Uani 1 1 d . . . O5 O 0.4687(3) 0.2171(2) 0.0126(2) 0.0379(9) Uani 1 1 d . . . O6 O 0.3285(3) 0.1708(3) -0.1170(2) 0.0501(10) Uani 1 1 d . . . N1 N 1.0032(3) 0.8124(3) 0.3579(3) 0.0334(10) Uani 1 1 d . . . N2 N 0.8737(3) 0.8663(3) 0.3102(3) 0.0352(10) Uani 1 1 d . . . N3 N 0.7173(3) 0.8530(3) 0.3358(3) 0.0318(9) Uani 1 1 d . . . N4 N 0.6595(3) 0.7751(3) 0.4072(3) 0.0362(10) Uani 1 1 d . . . N5 N 0.7143(3) 0.0517(3) -0.0375(3) 0.0354(10) Uani 1 1 d . . . N6 N 0.7296(3) 0.0518(3) 0.0900(3) 0.0325(9) Uani 1 1 d . . . N7 N 0.7267(3) 0.1619(3) 0.2044(2) 0.0336(10) Uani 1 1 d . . . N8 N 0.7132(3) 0.2927(3) 0.2075(3) 0.0388(11) Uani 1 1 d . . . C1 C 1.0696(5) 0.6937(4) 0.4020(4) 0.0458(14) Uani 1 1 d . . . C2 C 1.1553(5) 0.6683(4) 0.4512(4) 0.0518(15) Uani 1 1 d . . . H2A H 1.1455 0.6071 0.4463 0.062 Uiso 1 1 calc R . . C3 C 1.2521(5) 0.7288(4) 0.5057(4) 0.0475(14) Uani 1 1 d . . . C4 C 1.2655(4) 0.8191(4) 0.5157(3) 0.0441(14) Uani 1 1 d . . . H4A H 1.3318 0.8616 0.5552 0.053 Uiso 1 1 calc R . . C5 C 1.1830(4) 0.8481(3) 0.4688(3) 0.0362(12) Uani 1 1 d . . . C6 C 1.0866(4) 0.7840(3) 0.4118(3) 0.0351(12) Uani 1 1 d . . . C7 C 0.9647(5) 0.6261(4) 0.3384(5) 0.074(2) Uani 1 1 d . . . H7A H 0.9064 0.6402 0.3519 0.110 Uiso 1 1 calc R . . H7B H 0.9659 0.5667 0.3425 0.110 Uiso 1 1 calc R . . H7C H 0.9537 0.6277 0.2794 0.110 Uiso 1 1 calc R . . C8 C 1.3449(6) 0.6978(5) 0.5529(5) 0.073(2) Uani 1 1 d . . . H8A H 1.3173 0.6409 0.5615 0.109 Uiso 1 1 calc R . . H8B H 1.3902 0.7422 0.6094 0.109 Uiso 1 1 calc R . . H8C H 1.3870 0.6904 0.5183 0.109 Uiso 1 1 calc R . . C9 C 1.1993(5) 0.9462(4) 0.4802(4) 0.0570(16) Uani 1 1 d . . . H9A H 1.1850 0.9570 0.4240 0.086 Uiso 1 1 calc R . . H9B H 1.2731 0.9800 0.5203 0.086 Uiso 1 1 calc R . . H9C H 1.1503 0.9652 0.5038 0.086 Uiso 1 1 calc R . . C10 C 0.9314(4) 0.8448(3) 0.3809(3) 0.0341(11) Uani 1 1 d . . . C11 C 0.9898(5) 0.8152(4) 0.2739(4) 0.0467(14) Uani 1 1 d . . . H11A H 1.0307 0.7972 0.2434 0.056 Uiso 1 1 calc R . . C12 C 0.9093(4) 0.8477(4) 0.2452(3) 0.0433(13) Uani 1 1 d . . . H12A H 0.8813 0.8565 0.1899 0.052 Uiso 1 1 calc R . . C13 C 0.7905(4) 0.9071(3) 0.3100(3) 0.0343(11) Uani 1 1 d . . . H13A H 0.8225 0.9680 0.3509 0.041 Uiso 1 1 calc R . . H13B H 0.7519 0.9107 0.2513 0.041 Uiso 1 1 calc R . . C14 C 0.7504(4) 0.8236(3) 0.4055(3) 0.0310(11) Uani 1 1 d . . . C15 C 0.6063(4) 0.8230(4) 0.2938(4) 0.0453(14) Uani 1 1 d . . . H15A H 0.5644 0.8356 0.2438 0.054 Uiso 1 1 calc R . . C16 C 0.5697(4) 0.7734(4) 0.3366(4) 0.0472(14) Uani 1 1 d . . . H16A H 0.4972 0.7429 0.3223 0.057 Uiso 1 1 calc R . . C17 C 0.6489(5) 0.6340(4) 0.4425(4) 0.0441(14) Uani 1 1 d . . . C18 C 0.6418(5) 0.5856(4) 0.4982(4) 0.0567(17) Uani 1 1 d . . . H18A H 0.6405 0.5253 0.4833 0.068 Uiso 1 1 calc R . . C19 C 0.6362(5) 0.6243(4) 0.5784(4) 0.0525(16) Uani 1 1 d . . . C20 C 0.6398(4) 0.7114(4) 0.5978(4) 0.0489(15) Uani 1 1 d . . . H20A H 0.6372 0.7379 0.6513 0.059 Uiso 1 1 calc R . . C21 C 0.6470(4) 0.7643(4) 0.5435(3) 0.0365(12) Uani 1 1 d . . . C22 C 0.6526(4) 0.7230(4) 0.4662(3) 0.0360(12) Uani 1 1 d . . . C23 C 0.6502(6) 0.5912(4) 0.3557(4) 0.0604(18) Uani 1 1 d . . . H23A H 0.6505 0.5297 0.3511 0.091 Uiso 1 1 calc R . . H23B H 0.7144 0.6247 0.3516 0.091 Uiso 1 1 calc R . . H23C H 0.5867 0.5917 0.3086 0.091 Uiso 1 1 calc R . . C24 C 0.6276(7) 0.5690(6) 0.6382(5) 0.087(3) Uani 1 1 d . . . H24A H 0.5640 0.5697 0.6498 0.130 Uiso 1 1 calc R . . H24B H 0.6912 0.5939 0.6929 0.130 Uiso 1 1 calc R . . H24C H 0.6220 0.5077 0.6108 0.130 Uiso 1 1 calc R . . C25 C 0.6484(5) 0.8587(4) 0.5662(4) 0.0548(16) Uani 1 1 d . . . H25A H 0.5914 0.8672 0.5192 0.082 Uiso 1 1 calc R . . H25B H 0.7176 0.8974 0.5747 0.082 Uiso 1 1 calc R . . H25C H 0.6373 0.8737 0.6198 0.082 Uiso 1 1 calc R . . C26 C 1.0069(4) 0.9001(3) 0.6443(3) 0.0344(12) Uani 1 1 d . . . C27 C 0.7375(5) 0.1443(4) -0.1307(4) 0.0446(14) Uani 1 1 d . . . C28 C 0.7088(6) 0.1545(4) -0.2134(4) 0.0585(18) Uani 1 1 d . . . H28A H 0.7452 0.2070 -0.2208 0.070 Uiso 1 1 calc R . . C29 C 0.6266(5) 0.0881(5) -0.2858(4) 0.0532(17) Uani 1 1 d . . . C30 C 0.5751(5) 0.0134(4) -0.2734(4) 0.0504(15) Uani 1 1 d . . . H30A H 0.5193 -0.0313 -0.3223 0.061 Uiso 1 1 calc R . . C31 C 0.6006(4) -0.0001(4) -0.1929(3) 0.0383(12) Uani 1 1 d . . . C32 C 0.6829(4) 0.0674(4) -0.1226(3) 0.0357(12) Uani 1 1 d . . . C33 C 0.8279(6) 0.2162(4) -0.0537(4) 0.070(2) Uani 1 1 d . . . H33A H 0.8050 0.2304 -0.0063 0.106 Uiso 1 1 calc R . . H33B H 0.8470 0.2696 -0.0708 0.106 Uiso 1 1 calc R . . H33C H 0.8901 0.1950 -0.0345 0.106 Uiso 1 1 calc R . . C34 C 0.5990(7) 0.0971(6) -0.3771(4) 0.084(3) Uani 1 1 d . . . H34A H 0.5216 0.0842 -0.4067 0.126 Uiso 1 1 calc R . . H34B H 0.6227 0.0550 -0.4099 0.126 Uiso 1 1 calc R . . H34C H 0.6349 0.1578 -0.3732 0.126 Uiso 1 1 calc R . . C35 C 0.5436(5) -0.0836(4) -0.1812(4) 0.0633(18) Uani 1 1 d . . . H35A H 0.5225 -0.0681 -0.1329 0.095 Uiso 1 1 calc R . . H35B H 0.5913 -0.1202 -0.1688 0.095 Uiso 1 1 calc R . . H35C H 0.4799 -0.1171 -0.2344 0.095 Uiso 1 1 calc R . . C36 C 0.6811(4) 0.0824(3) 0.0244(3) 0.0303(11) Uani 1 1 d . . . C37 C 0.7821(5) 0.0017(4) -0.0105(4) 0.0452(14) Uani 1 1 d . . . H37A H 0.8147 -0.0273 -0.0430 0.054 Uiso 1 1 calc R . . C38 C 0.7925(5) 0.0024(4) 0.0699(4) 0.0430(14) Uani 1 1 d . . . H38A H 0.8344 -0.0253 0.1059 0.052 Uiso 1 1 calc R . . C39 C 0.7144(4) 0.0680(3) 0.1717(3) 0.0338(11) Uani 1 1 d . . . H39A H 0.6423 0.0317 0.1614 0.041 Uiso 1 1 calc R . . H39B H 0.7678 0.0508 0.2150 0.041 Uiso 1 1 calc R . . C40 C 0.6815(4) 0.2085(3) 0.1534(3) 0.0329(11) Uani 1 1 d . . . C41 C 0.7867(4) 0.2157(4) 0.2891(3) 0.0385(13) Uani 1 1 d . . . H41A H 0.8269 0.1982 0.3363 0.046 Uiso 1 1 calc R . . C42 C 0.7772(4) 0.2960(4) 0.2918(3) 0.0426(14) Uani 1 1 d . . . H42A H 0.8081 0.3466 0.3417 0.051 Uiso 1 1 calc R . . C43 C 0.7730(5) 0.4193(4) 0.1602(3) 0.0475(15) Uani 1 1 d . . . C44 C 0.7554(6) 0.4933(4) 0.1353(4) 0.0555(17) Uani 1 1 d . . . H44A H 0.8071 0.5280 0.1212 0.067 Uiso 1 1 calc R . . C45 C 0.6653(6) 0.5186(4) 0.1302(4) 0.0576(18) Uani 1 1 d . . . C46 C 0.5894(5) 0.4668(4) 0.1499(4) 0.0539(16) Uani 1 1 d . . . H46A H 0.5262 0.4822 0.1448 0.065 Uiso 1 1 calc R . . C47 C 0.6037(5) 0.3918(3) 0.1774(3) 0.0412(13) Uani 1 1 d . . . C48 C 0.6957(4) 0.3697(3) 0.1799(3) 0.0360(12) Uani 1 1 d . . . C49 C 0.8725(5) 0.3944(4) 0.1647(4) 0.0605(17) Uani 1 1 d . . . H49A H 0.8526 0.3313 0.1332 0.091 Uiso 1 1 calc R . . H49B H 0.9195 0.4054 0.2254 0.091 Uiso 1 1 calc R . . H49C H 0.9100 0.4304 0.1384 0.091 Uiso 1 1 calc R . . C50 C 0.6489(7) 0.5992(5) 0.1026(6) 0.094(3) Uani 1 1 d . . . H50A H 0.5954 0.6180 0.1203 0.141 Uiso 1 1 calc R . . H50B H 0.6241 0.5843 0.0395 0.141 Uiso 1 1 calc R . . H50C H 0.7165 0.6476 0.1302 0.141 Uiso 1 1 calc R . . C51 C 0.5222(5) 0.3396(4) 0.1997(4) 0.0534(16) Uani 1 1 d . . . H51A H 0.5559 0.3359 0.2585 0.080 Uiso 1 1 calc R . . H51B H 0.4896 0.2796 0.1585 0.080 Uiso 1 1 calc R . . H51C H 0.4670 0.3688 0.1969 0.080 Uiso 1 1 calc R . . C52 C 0.4173(4) 0.1679(4) -0.0692(3) 0.0383(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0306(2) 0.0323(2) 0.01779(19) 0.00476(15) 0.00500(16) 0.00917(16) Pd2 0.0334(2) 0.0299(2) 0.01830(19) 0.00344(15) 0.00556(16) 0.01115(16) O1 0.0280(17) 0.051(2) 0.0177(16) 0.0083(15) 0.0033(14) 0.0122(16) O2 0.038(2) 0.053(2) 0.0271(19) 0.0110(16) 0.0142(16) 0.0175(17) O3 0.046(2) 0.068(3) 0.0154(18) 0.0056(17) 0.0053(16) 0.019(2) O4 0.0374(19) 0.0354(19) 0.0232(18) -0.0006(14) 0.0035(15) 0.0126(16) O5 0.039(2) 0.046(2) 0.0188(17) -0.0008(15) 0.0023(15) 0.0195(17) O6 0.042(2) 0.072(3) 0.0244(19) 0.0081(19) -0.0013(17) 0.023(2) N1 0.041(2) 0.044(2) 0.023(2) 0.0123(18) 0.0155(19) 0.020(2) N2 0.043(2) 0.042(2) 0.020(2) 0.0090(18) 0.0100(19) 0.018(2) N3 0.032(2) 0.037(2) 0.021(2) 0.0050(17) 0.0063(18) 0.0117(18) N4 0.036(2) 0.046(3) 0.024(2) 0.0076(19) 0.0103(19) 0.016(2) N5 0.050(3) 0.038(2) 0.022(2) 0.0079(18) 0.014(2) 0.021(2) N6 0.039(2) 0.033(2) 0.027(2) 0.0107(18) 0.0128(19) 0.0138(19) N7 0.039(2) 0.035(2) 0.019(2) 0.0039(17) 0.0044(18) 0.0101(19) N8 0.047(3) 0.041(2) 0.017(2) 0.0006(18) 0.0000(19) 0.022(2) C1 0.045(3) 0.038(3) 0.047(3) 0.009(3) 0.013(3) 0.011(3) C2 0.059(4) 0.042(3) 0.056(4) 0.022(3) 0.017(3) 0.023(3) C3 0.046(3) 0.071(4) 0.042(3) 0.026(3) 0.022(3) 0.033(3) C4 0.040(3) 0.060(4) 0.029(3) 0.008(3) 0.011(2) 0.019(3) C5 0.046(3) 0.043(3) 0.030(3) 0.012(2) 0.024(2) 0.018(2) C6 0.043(3) 0.040(3) 0.021(2) 0.006(2) 0.011(2) 0.018(2) C7 0.065(4) 0.046(4) 0.084(5) 0.013(4) 0.008(4) 0.010(3) C8 0.074(5) 0.106(6) 0.056(4) 0.039(4) 0.021(4) 0.060(5) C9 0.070(4) 0.048(4) 0.053(4) 0.008(3) 0.027(3) 0.021(3) C10 0.032(3) 0.039(3) 0.024(3) 0.007(2) 0.007(2) 0.008(2) C11 0.054(4) 0.064(4) 0.031(3) 0.017(3) 0.019(3) 0.030(3) C12 0.047(3) 0.063(4) 0.024(3) 0.017(3) 0.011(2) 0.025(3) C13 0.034(3) 0.043(3) 0.025(3) 0.010(2) 0.007(2) 0.018(2) C14 0.037(3) 0.030(2) 0.020(2) 0.0030(19) 0.007(2) 0.011(2) C15 0.039(3) 0.062(4) 0.033(3) 0.014(3) 0.008(3) 0.024(3) C16 0.032(3) 0.059(4) 0.034(3) 0.006(3) 0.005(3) 0.005(3) C17 0.049(3) 0.037(3) 0.035(3) 0.002(2) 0.013(3) 0.005(3) C18 0.062(4) 0.040(3) 0.060(4) 0.011(3) 0.022(4) 0.008(3) C19 0.048(4) 0.060(4) 0.045(4) 0.022(3) 0.015(3) 0.007(3) C20 0.046(3) 0.059(4) 0.032(3) 0.004(3) 0.016(3) 0.008(3) C21 0.038(3) 0.047(3) 0.024(3) 0.006(2) 0.014(2) 0.014(2) C22 0.026(3) 0.047(3) 0.031(3) 0.013(2) 0.010(2) 0.005(2) C23 0.079(5) 0.052(4) 0.041(4) -0.001(3) 0.023(3) 0.021(3) C24 0.099(6) 0.092(6) 0.066(5) 0.041(5) 0.031(5) 0.012(5) C25 0.068(4) 0.064(4) 0.034(3) 0.005(3) 0.022(3) 0.028(3) C26 0.038(3) 0.035(3) 0.027(3) 0.013(2) 0.005(2) 0.012(2) C27 0.068(4) 0.041(3) 0.036(3) 0.010(2) 0.028(3) 0.027(3) C28 0.087(5) 0.060(4) 0.066(5) 0.038(4) 0.053(4) 0.039(4) C29 0.067(4) 0.083(5) 0.030(3) 0.022(3) 0.021(3) 0.054(4) C30 0.048(4) 0.070(4) 0.033(3) 0.009(3) 0.017(3) 0.025(3) C31 0.037(3) 0.053(3) 0.033(3) 0.011(2) 0.019(2) 0.024(3) C32 0.045(3) 0.048(3) 0.028(3) 0.019(2) 0.022(2) 0.023(3) C33 0.102(6) 0.045(4) 0.056(4) 0.008(3) 0.033(4) 0.010(4) C34 0.122(7) 0.133(7) 0.039(4) 0.039(4) 0.044(4) 0.088(6) C35 0.050(4) 0.067(4) 0.058(4) 0.009(3) 0.020(3) 0.002(3) C36 0.035(3) 0.034(3) 0.021(2) 0.009(2) 0.008(2) 0.015(2) C37 0.063(4) 0.055(4) 0.034(3) 0.017(3) 0.024(3) 0.041(3) C38 0.064(4) 0.048(3) 0.036(3) 0.021(3) 0.024(3) 0.037(3) C39 0.042(3) 0.034(3) 0.025(3) 0.009(2) 0.012(2) 0.013(2) C40 0.029(3) 0.035(3) 0.027(3) 0.006(2) 0.001(2) 0.013(2) C41 0.043(3) 0.048(3) 0.015(2) 0.003(2) 0.003(2) 0.018(3) C42 0.055(3) 0.040(3) 0.016(2) -0.001(2) 0.001(2) 0.013(3) C43 0.056(4) 0.039(3) 0.027(3) -0.003(2) 0.005(3) 0.009(3) C44 0.073(4) 0.036(3) 0.042(3) 0.010(3) 0.013(3) 0.004(3) C45 0.083(5) 0.036(3) 0.039(3) 0.009(3) 0.006(3) 0.023(3) C46 0.066(4) 0.042(3) 0.038(3) -0.002(3) 0.006(3) 0.025(3) C47 0.054(3) 0.034(3) 0.021(3) -0.003(2) 0.004(2) 0.016(3) C48 0.053(3) 0.028(3) 0.017(2) -0.0005(19) 0.006(2) 0.014(2) C49 0.055(4) 0.055(4) 0.061(4) 0.009(3) 0.019(3) 0.013(3) C50 0.129(8) 0.074(6) 0.095(7) 0.044(5) 0.040(6) 0.052(5) C51 0.061(4) 0.064(4) 0.033(3) 0.003(3) 0.017(3) 0.030(3) C52 0.032(3) 0.047(3) 0.028(3) 0.009(2) 0.007(2) 0.006(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 Pd1 C10 1.980(5) . ? Pd1 C14 1.986(5) . ? Pd1 O1 2.064(3) . ? Pd1 O2 2.069(4) . ? Pd1 C26 2.466(5) . ? Pd2 C36 1.981(5) . ? Pd2 C40 1.988(5) . ? Pd2 O5 2.051(3) . ? Pd2 O4 2.067(3) . ? Pd2 C52 2.453(5) . ? O1 C26 1.307(6) . ? O2 C26 1.346(6) . ? O3 C26 1.244(6) . ? O4 C52 1.310(6) . ? O5 C52 1.319(6) . ? O6 C52 1.250(6) . ? N1 C10 1.363(6) . ? N1 C11 1.405(7) . ? N1 C6 1.446(6) . ? N2 C10 1.368(6) . ? N2 C12 1.379(7) . ? N2 C13 1.455(6) . ? N3 C14 1.352(6) . ? N3 C15 1.393(6) . ? N3 C13 1.451(6) . ? N4 C14 1.360(6) . ? N4 C16 1.408(7) . ? N4 C22 1.460(7) . ? N5 C36 1.350(6) . ? N5 C37 1.394(6) . ? N5 C32 1.470(6) . ? N6 C36 1.350(6) . ? N6 C38 1.387(6) . ? N6 C39 1.475(6) . ? N7 C40 1.350(6) . ? N7 C41 1.386(6) . ? N7 C39 1.456(6) . ? N8 C40 1.363(6) . ? N8 C42 1.404(6) . ? N8 C48 1.455(6) . ? C1 C6 1.392(7) . ? C1 C2 1.406(8) . ? C1 C7 1.509(8) . ? C2 C3 1.366(8) . ? C3 C4 1.397(8) . ? C3 C8 1.522(8) . ? C4 C5 1.396(7) . ? C5 C6 1.393(7) . ? C5 C9 1.512(8) . ? C11 C12 1.329(8) . ? C15 C16 1.332(8) . ? C17 C18 1.371(8) . ? C17 C22 1.395(7) . ? C17 C23 1.523(8) . ? C18 C19 1.431(9) . ? C19 C20 1.363(8) . ? C19 C24 1.513(9) . ? C20 C21 1.404(8) . ? C21 C22 1.398(7) . ? C21 C25 1.487(8) . ? C27 C32 1.375(8) . ? C27 C28 1.395(8) . ? C27 C33 1.518(8) . ? C28 C29 1.406(9) . ? C29 C30 1.365(9) . ? C29 C34 1.531(8) . ? C30 C31 1.383(8) . ? C31 C32 1.398(7) . ? C31 C35 1.505(8) . ? C37 C38 1.341(7) . ? C41 C42 1.325(7) . ? C43 C48 1.389(8) . ? C43 C44 1.391(8) . ? C43 C49 1.513(8) . ? C44 C45 1.388(9) . ? C45 C46 1.391(9) . ? C45 C50 1.508(9) . ? C46 C47 1.415(8) . ? C47 C48 1.397(7) . ? C47 C51 1.480(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Pd1 C14 84.9(2) . . ? C10 Pd1 O1 105.44(18) . . ? C14 Pd1 O1 169.49(17) . . ? C10 Pd1 O2 169.94(17) . . ? C14 Pd1 O2 104.63(17) . . ? O1 Pd1 O2 64.96(14) . . ? C10 Pd1 C26 137.09(19) . . ? C14 Pd1 C26 137.50(19) . . ? O1 Pd1 C26 32.01(15) . . ? O2 Pd1 C26 33.08(15) . . ? C36 Pd2 C40 85.25(19) . . ? C36 Pd2 O5 169.81(16) . . ? C40 Pd2 O5 104.08(17) . . ? C36 Pd2 O4 105.81(17) . . ? C40 Pd2 O4 168.74(17) . . ? O5 Pd2 O4 64.74(13) . . ? C36 Pd2 C52 137.74(19) . . ? C40 Pd2 C52 136.49(19) . . ? O5 Pd2 C52 32.54(15) . . ? O4 Pd2 C52 32.28(15) . . ? C26 O1 Pd1 91.2(3) . . ? C26 O2 Pd1 89.9(3) . . ? C52 O4 Pd2 90.3(3) . . ? C52 O5 Pd2 90.7(3) . . ? C10 N1 C11 110.1(4) . . ? C10 N1 C6 126.5(4) . . ? C11 N1 C6 123.3(4) . . ? C10 N2 C12 110.9(4) . . ? C10 N2 C13 121.7(4) . . ? C12 N2 C13 127.3(4) . . ? C14 N3 C15 110.6(4) . . ? C14 N3 C13 122.9(4) . . ? C15 N3 C13 126.5(4) . . ? C14 N4 C16 110.1(4) . . ? C14 N4 C22 126.6(4) . . ? C16 N4 C22 123.0(4) . . ? C36 N5 C37 110.9(4) . . ? C36 N5 C32 125.2(4) . . ? C37 N5 C32 123.9(4) . . ? C36 N6 C38 111.8(4) . . ? C36 N6 C39 123.2(4) . . ? C38 N6 C39 124.9(4) . . ? C40 N7 C41 111.2(4) . . ? C40 N7 C39 123.0(4) . . ? C41 N7 C39 125.8(4) . . ? C40 N8 C42 109.5(4) . . ? C40 N8 C48 125.1(4) . . ? C42 N8 C48 125.0(4) . . ? C6 C1 C2 117.1(5) . . ? C6 C1 C7 120.9(5) . . ? C2 C1 C7 121.9(5) . . ? C3 C2 C1 122.2(6) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 C8 120.4(6) . . ? C4 C3 C8 120.5(6) . . ? C5 C4 C3 121.2(5) . . ? C6 C5 C4 117.9(5) . . ? C6 C5 C9 121.8(5) . . ? C4 C5 C9 120.3(5) . . ? C1 C6 C5 122.5(5) . . ? C1 C6 N1 118.9(5) . . ? C5 C6 N1 118.5(5) . . ? N1 C10 N2 104.4(4) . . ? N1 C10 Pd1 130.8(4) . . ? N2 C10 Pd1 124.7(4) . . ? C12 C11 N1 107.1(5) . . ? C11 C12 N2 107.5(5) . . ? N3 C13 N2 108.4(4) . . ? N3 C14 N4 105.2(4) . . ? N3 C14 Pd1 124.3(4) . . ? N4 C14 Pd1 130.5(4) . . ? C16 C15 N3 107.5(5) . . ? C15 C16 N4 106.6(5) . . ? C18 C17 C22 118.6(5) . . ? C18 C17 C23 120.8(6) . . ? C22 C17 C23 120.6(5) . . ? C17 C18 C19 121.2(6) . . ? C20 C19 C18 117.4(6) . . ? C20 C19 C24 122.5(6) . . ? C18 C19 C24 120.1(6) . . ? C19 C20 C21 124.0(5) . . ? C22 C21 C20 116.0(5) . . ? C22 C21 C25 121.7(5) . . ? C20 C21 C25 122.3(5) . . ? C17 C22 C21 122.8(5) . . ? C17 C22 N4 119.1(5) . . ? C21 C22 N4 118.1(5) . . ? O3 C26 O1 125.0(5) . . ? O3 C26 O2 121.5(5) . . ? O1 C26 O2 113.5(4) . . ? O3 C26 Pd1 174.9(4) . . ? O1 C26 Pd1 56.8(2) . . ? O2 C26 Pd1 57.0(2) . . ? C32 C27 C28 117.9(6) . . ? C32 C27 C33 122.2(5) . . ? C28 C27 C33 119.9(6) . . ? C27 C28 C29 120.9(6) . . ? C30 C29 C28 118.5(6) . . ? C30 C29 C34 120.5(6) . . ? C28 C29 C34 120.9(7) . . ? C29 C30 C31 122.9(6) . . ? C30 C31 C32 116.9(5) . . ? C30 C31 C35 121.9(5) . . ? C32 C31 C35 121.3(5) . . ? C27 C32 C31 123.0(5) . . ? C27 C32 N5 119.7(5) . . ? C31 C32 N5 117.3(5) . . ? N5 C36 N6 104.2(4) . . ? N5 C36 Pd2 131.4(4) . . ? N6 C36 Pd2 124.4(3) . . ? C38 C37 N5 107.0(5) . . ? C37 C38 N6 106.0(5) . . ? N7 C39 N6 109.1(4) . . ? N7 C40 N8 104.9(4) . . ? N7 C40 Pd2 124.8(3) . . ? N8 C40 Pd2 130.3(4) . . ? C42 C41 N7 106.9(5) . . ? C41 C42 N8 107.6(4) . . ? C48 C43 C44 117.4(6) . . ? C48 C43 C49 122.0(5) . . ? C44 C43 C49 120.7(6) . . ? C45 C44 C43 122.6(6) . . ? C44 C45 C46 118.3(6) . . ? C44 C45 C50 121.0(7) . . ? C46 C45 C50 120.7(7) . . ? C45 C46 C47 121.8(6) . . ? C48 C47 C46 116.7(6) . . ? C48 C47 C51 123.2(5) . . ? C46 C47 C51 120.1(5) . . ? C43 C48 C47 123.2(5) . . ? C43 C48 N8 118.3(5) . . ? C47 C48 N8 118.5(5) . . ? O6 C52 O4 123.3(5) . . ? O6 C52 O5 122.7(5) . . ? O4 C52 O5 114.0(4) . . ? O6 C52 Pd2 176.9(4) . . ? O4 C52 Pd2 57.4(2) . . ? O5 C52 Pd2 56.7(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 C10 Pd1 O1 C26 172.6(3) . . . . ? C14 Pd1 O1 C26 3.6(11) . . . . ? O2 Pd1 O1 C26 -4.2(3) . . . . ? C10 Pd1 O2 C26 -13.8(11) . . . . ? C14 Pd1 O2 C26 -174.5(3) . . . . ? O1 Pd1 O2 C26 4.0(3) . . . . ? C36 Pd2 O4 C52 172.8(3) . . . . ? C40 Pd2 O4 C52 4.1(10) . . . . ? O5 Pd2 O4 C52 -3.1(3) . . . . ? C36 Pd2 O5 C52 -19.6(11) . . . . ? C40 Pd2 O5 C52 -175.4(3) . . . . ? O4 Pd2 O5 C52 3.1(3) . . . . ? C6 C1 C2 C3 -0.9(9) . . . . ? C7 C1 C2 C3 176.7(6) . . . . ? C1 C2 C3 C4 2.6(9) . . . . ? C1 C2 C3 C8 -175.8(6) . . . . ? C2 C3 C4 C5 -2.3(8) . . . . ? C8 C3 C4 C5 176.1(5) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C3 C4 C5 C9 -179.6(5) . . . . ? C2 C1 C6 C5 -1.2(8) . . . . ? C7 C1 C6 C5 -178.9(6) . . . . ? C2 C1 C6 N1 175.6(5) . . . . ? C7 C1 C6 N1 -2.1(8) . . . . ? C4 C5 C6 C1 1.5(8) . . . . ? C9 C5 C6 C1 -178.6(5) . . . . ? C4 C5 C6 N1 -175.3(4) . . . . ? C9 C5 C6 N1 4.6(7) . . . . ? C10 N1 C6 C1 99.4(6) . . . . ? C11 N1 C6 C1 -84.8(7) . . . . ? C10 N1 C6 C5 -83.7(6) . . . . ? C11 N1 C6 C5 92.2(6) . . . . ? C11 N1 C10 N2 0.6(6) . . . . ? C6 N1 C10 N2 176.9(4) . . . . ? C11 N1 C10 Pd1 176.2(4) . . . . ? C6 N1 C10 Pd1 -7.5(8) . . . . ? C12 N2 C10 N1 0.0(6) . . . . ? C13 N2 C10 N1 -177.4(4) . . . . ? C12 N2 C10 Pd1 -176.0(4) . . . . ? C13 N2 C10 Pd1 6.6(7) . . . . ? C14 Pd1 C10 N1 -142.6(5) . . . . ? O1 Pd1 C10 N1 39.4(5) . . . . ? O2 Pd1 C10 N1 56.1(13) . . . . ? C26 Pd1 C10 N1 45.1(6) . . . . ? C14 Pd1 C10 N2 32.2(4) . . . . ? O1 Pd1 C10 N2 -145.8(4) . . . . ? O2 Pd1 C10 N2 -129.0(9) . . . . ? C26 Pd1 C10 N2 -140.1(4) . . . . ? C10 N1 C11 C12 -1.0(6) . . . . ? C6 N1 C11 C12 -177.4(5) . . . . ? N1 C11 C12 N2 0.9(7) . . . . ? C10 N2 C12 C11 -0.6(7) . . . . ? C13 N2 C12 C11 176.6(5) . . . . ? C14 N3 C13 N2 47.6(6) . . . . ? C15 N3 C13 N2 -131.2(5) . . . . ? C10 N2 C13 N3 -52.6(6) . . . . ? C12 N2 C13 N3 130.5(5) . . . . ? C15 N3 C14 N4 -0.2(5) . . . . ? C13 N3 C14 N4 -179.1(4) . . . . ? C15 N3 C14 Pd1 -178.1(4) . . . . ? C13 N3 C14 Pd1 2.9(6) . . . . ? C16 N4 C14 N3 1.1(5) . . . . ? C22 N4 C14 N3 174.7(4) . . . . ? C16 N4 C14 Pd1 178.9(4) . . . . ? C22 N4 C14 Pd1 -7.6(7) . . . . ? C10 Pd1 C14 N3 -37.0(4) . . . . ? O1 Pd1 C14 N3 132.3(8) . . . . ? O2 Pd1 C14 N3 139.6(4) . . . . ? C26 Pd1 C14 N3 135.2(4) . . . . ? C10 Pd1 C14 N4 145.5(5) . . . . ? O1 Pd1 C14 N4 -45.1(12) . . . . ? O2 Pd1 C14 N4 -37.8(5) . . . . ? C26 Pd1 C14 N4 -42.2(6) . . . . ? C14 N3 C15 C16 -0.9(6) . . . . ? C13 N3 C15 C16 178.0(5) . . . . ? N3 C15 C16 N4 1.5(6) . . . . ? C14 N4 C16 C15 -1.7(6) . . . . ? C22 N4 C16 C15 -175.5(5) . . . . ? C22 C17 C18 C19 1.1(9) . . . . ? C23 C17 C18 C19 -177.5(6) . . . . ? C17 C18 C19 C20 -0.9(9) . . . . ? C17 C18 C19 C24 179.6(6) . . . . ? C18 C19 C20 C21 0.9(9) . . . . ? C24 C19 C20 C21 -179.6(6) . . . . ? C19 C20 C21 C22 -1.1(9) . . . . ? C19 C20 C21 C25 178.7(6) . . . . ? C18 C17 C22 C21 -1.4(8) . . . . ? C23 C17 C22 C21 177.2(5) . . . . ? C18 C17 C22 N4 -179.6(5) . . . . ? C23 C17 C22 N4 -1.0(8) . . . . ? C20 C21 C22 C17 1.3(8) . . . . ? C25 C21 C22 C17 -178.5(5) . . . . ? C20 C21 C22 N4 179.6(4) . . . . ? C25 C21 C22 N4 -0.2(8) . . . . ? C14 N4 C22 C17 -90.0(6) . . . . ? C16 N4 C22 C17 82.8(6) . . . . ? C14 N4 C22 C21 91.7(6) . . . . ? C16 N4 C22 C21 -95.5(6) . . . . ? Pd1 O1 C26 O3 -174.2(5) . . . . ? Pd1 O1 C26 O2 6.3(4) . . . . ? Pd1 O2 C26 O3 174.2(5) . . . . ? Pd1 O2 C26 O1 -6.3(4) . . . . ? C10 Pd1 C26 O3 102(5) . . . . ? C14 Pd1 C26 O3 -66(5) . . . . ? O1 Pd1 C26 O3 113(5) . . . . ? O2 Pd1 C26 O3 -74(5) . . . . ? C10 Pd1 C26 O1 -10.4(4) . . . . ? C14 Pd1 C26 O1 -179.0(3) . . . . ? O2 Pd1 C26 O1 173.1(5) . . . . ? C10 Pd1 C26 O2 176.5(3) . . . . ? C14 Pd1 C26 O2 7.9(4) . . . . ? O1 Pd1 C26 O2 -173.1(5) . . . . ? C32 C27 C28 C29 0.0(9) . . . . ? C33 C27 C28 C29 178.9(6) . . . . ? C27 C28 C29 C30 0.3(9) . . . . ? C27 C28 C29 C34 -176.8(5) . . . . ? C28 C29 C30 C31 -0.4(9) . . . . ? C34 C29 C30 C31 176.6(5) . . . . ? C29 C30 C31 C32 0.3(8) . . . . ? C29 C30 C31 C35 -179.1(6) . . . . ? C28 C27 C32 C31 -0.1(8) . . . . ? C33 C27 C32 C31 -179.0(5) . . . . ? C28 C27 C32 N5 176.8(5) . . . . ? C33 C27 C32 N5 -2.1(8) . . . . ? C30 C31 C32 C27 0.0(8) . . . . ? C35 C31 C32 C27 179.4(5) . . . . ? C30 C31 C32 N5 -177.0(5) . . . . ? C35 C31 C32 N5 2.4(7) . . . . ? C36 N5 C32 C27 84.8(7) . . . . ? C37 N5 C32 C27 -96.1(6) . . . . ? C36 N5 C32 C31 -98.2(6) . . . . ? C37 N5 C32 C31 81.0(6) . . . . ? C37 N5 C36 N6 0.6(6) . . . . ? C32 N5 C36 N6 179.9(4) . . . . ? C37 N5 C36 Pd2 179.4(4) . . . . ? C32 N5 C36 Pd2 -1.4(8) . . . . ? C38 N6 C36 N5 -0.1(6) . . . . ? C39 N6 C36 N5 -178.8(4) . . . . ? C38 N6 C36 Pd2 -178.9(4) . . . . ? C39 N6 C36 Pd2 2.4(6) . . . . ? C40 Pd2 C36 N5 -144.8(5) . . . . ? O5 Pd2 C36 N5 58.7(12) . . . . ? O4 Pd2 C36 N5 37.4(5) . . . . ? C52 Pd2 C36 N5 43.1(6) . . . . ? C40 Pd2 C36 N6 33.7(4) . . . . ? O5 Pd2 C36 N6 -122.8(9) . . . . ? O4 Pd2 C36 N6 -144.1(4) . . . . ? C52 Pd2 C36 N6 -138.4(4) . . . . ? C36 N5 C37 C38 -1.0(6) . . . . ? C32 N5 C37 C38 179.8(5) . . . . ? N5 C37 C38 N6 0.8(6) . . . . ? C36 N6 C38 C37 -0.5(6) . . . . ? C39 N6 C38 C37 178.2(5) . . . . ? C40 N7 C39 N6 44.9(6) . . . . ? C41 N7 C39 N6 -133.4(5) . . . . ? C36 N6 C39 N7 -48.0(6) . . . . ? C38 N6 C39 N7 133.5(5) . . . . ? C41 N7 C40 N8 -0.4(6) . . . . ? C39 N7 C40 N8 -179.0(4) . . . . ? C41 N7 C40 Pd2 -178.6(4) . . . . ? C39 N7 C40 Pd2 2.9(7) . . . . ? C42 N8 C40 N7 -0.6(6) . . . . ? C48 N8 C40 N7 171.7(5) . . . . ? C42 N8 C40 Pd2 177.4(4) . . . . ? C48 N8 C40 Pd2 -10.3(8) . . . . ? C36 Pd2 C40 N7 -36.7(4) . . . . ? O5 Pd2 C40 N7 139.2(4) . . . . ? O4 Pd2 C40 N7 132.4(8) . . . . ? C52 Pd2 C40 N7 135.6(4) . . . . ? C36 Pd2 C40 N8 145.7(5) . . . . ? O5 Pd2 C40 N8 -38.5(5) . . . . ? O4 Pd2 C40 N8 -45.2(12) . . . . ? C52 Pd2 C40 N8 -42.0(6) . . . . ? C40 N7 C41 C42 1.3(6) . . . . ? C39 N7 C41 C42 179.9(5) . . . . ? N7 C41 C42 N8 -1.6(6) . . . . ? C40 N8 C42 C41 1.4(7) . . . . ? C48 N8 C42 C41 -170.9(5) . . . . ? C48 C43 C44 C45 0.4(8) . . . . ? C49 C43 C44 C45 180.0(6) . . . . ? C43 C44 C45 C46 -0.8(9) . . . . ? C43 C44 C45 C50 -179.8(6) . . . . ? C44 C45 C46 C47 2.1(9) . . . . ? C50 C45 C46 C47 -178.9(6) . . . . ? C45 C46 C47 C48 -2.9(8) . . . . ? C45 C46 C47 C51 178.5(5) . . . . ? C44 C43 C48 C47 -1.2(8) . . . . ? C49 C43 C48 C47 179.1(5) . . . . ? C44 C43 C48 N8 -179.0(4) . . . . ? C49 C43 C48 N8 1.4(7) . . . . ? C46 C47 C48 C43 2.5(7) . . . . ? C51 C47 C48 C43 -179.0(5) . . . . ? C46 C47 C48 N8 -179.8(4) . . . . ? C51 C47 C48 N8 -1.3(7) . . . . ? C40 N8 C48 C43 -90.0(6) . . . . ? C42 N8 C48 C43 81.1(6) . . . . ? C40 N8 C48 C47 92.2(6) . . . . ? C42 N8 C48 C47 -96.7(6) . . . . ? Pd2 O4 C52 O6 -176.4(5) . . . . ? Pd2 O4 C52 O5 4.8(4) . . . . ? Pd2 O5 C52 O6 176.4(5) . . . . ? Pd2 O5 C52 O4 -4.9(5) . . . . ? C36 Pd2 C52 O6 95(8) . . . . ? C40 Pd2 C52 O6 -73(8) . . . . ? O5 Pd2 C52 O6 -80(8) . . . . ? O4 Pd2 C52 O6 105(8) . . . . ? C36 Pd2 C52 O4 -10.3(4) . . . . ? C40 Pd2 C52 O4 -178.8(3) . . . . ? O5 Pd2 C52 O4 174.7(5) . . . . ? C36 Pd2 C52 O5 174.9(3) . . . . ? C40 Pd2 C52 O5 6.4(4) . . . . ? O4 Pd2 C52 O5 -174.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.955 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.128 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.027 -0.003 1243.6 231.4 2 0.340 0.970 0.684 8.2 -1.6 3 0.660 0.030 0.315 8.1 -1.6 _platon_squeeze_details ; PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 Void space analysis consistent with 10 cocrystallized molecules of acetonitrile per unit cell. ; _vrf_CHEMW03_joer049s ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: See _platon_squeeze_details ; _vrf_PLAT043_joer049s ; PROBLEM: Check Reported Molecular Weight ................ 653.56 RESPONSE: See _platon_squeeze_details ; #===END data_joer062 _database_code_depnum_ccdc_archive 'CCDC 871923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H40 N6 O4 Pd' _chemical_formula_weight 691.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 13.403(7) _cell_length_b 19.118(10) _cell_length_c 14.849(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.089(7) _cell_angle_gamma 90.00 _cell_volume 3473(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7277 _exptl_absorpt_correction_T_max 0.8725 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 43918 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.24 _reflns_number_total 8565 _reflns_number_gt 6261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. The 9 restraints reported were applied in modeling a disordered acetonitrile solvent molecule. ; _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^)+(0.0528P)^2^+3.4967P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8565 _refine_ls_number_parameters 418 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _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 Pd Pd 0.976169(19) 0.188140(14) 0.914542(16) 0.03789(9) Uani 1 1 d . . . N1 N 1.0458(3) 0.17825(19) 0.7410(2) 0.0564(9) Uani 1 1 d . . . N2 N 0.8719(2) 0.18274(15) 0.69884(19) 0.0422(7) Uani 1 1 d . . . N3 N 0.7639(2) 0.23760(15) 0.77096(18) 0.0396(6) Uani 1 1 d . . . N4 N 0.8146(2) 0.30394(15) 0.89780(19) 0.0400(6) Uani 1 1 d . . . O1 O 1.11262(19) 0.12395(14) 0.97469(17) 0.0496(6) Uani 1 1 d . . . O2 O 1.2005(2) 0.2235(2) 1.0319(2) 0.0708(9) Uani 1 1 d . . . O3 O 0.97066(19) 0.18496(13) 1.05173(15) 0.0435(6) Uani 1 1 d . . . O4 O 0.8218(3) 0.11820(18) 0.9934(2) 0.0751(9) Uani 1 1 d . . . C1 C 1.2186(4) 0.1154(3) 0.8212(3) 0.0735(15) Uani 1 1 d . . . C2 C 1.3321(4) 0.1184(4) 0.8700(3) 0.096(2) Uani 1 1 d . . . H2A H 1.3723 0.0761 0.8910 0.116 Uiso 1 1 calc R . . C3 C 1.3878(5) 0.1817(5) 0.8888(5) 0.127(4) Uani 1 1 d . . . C4 C 1.3312(5) 0.2417(5) 0.8594(4) 0.113(3) Uani 1 1 d . . . H4A H 1.3698 0.2848 0.8725 0.135 Uiso 1 1 calc R . . C5 C 1.2172(5) 0.2425(4) 0.8099(4) 0.0877(18) Uani 1 1 d . . . C6 C 1.1630(4) 0.1783(3) 0.7937(3) 0.0692(14) Uani 1 1 d . . . C7 C 1.1587(4) 0.0468(3) 0.8004(4) 0.0820(15) Uani 1 1 d . . . H7A H 1.0977 0.0486 0.7352 0.123 Uiso 1 1 calc R . . H7B H 1.1305 0.0380 0.8507 0.123 Uiso 1 1 calc R . . H7C H 1.2088 0.0091 0.8017 0.123 Uiso 1 1 calc R . . C8 C 1.5125(5) 0.1832(6) 0.9443(6) 0.178(5) Uani 1 1 d . . . H8A H 1.5404 0.1352 0.9574 0.267 Uiso 1 1 calc R . . H8B H 1.5324 0.2081 1.0069 0.267 Uiso 1 1 calc R . . H8C H 1.5445 0.2072 0.9040 0.267 Uiso 1 1 calc R . . C9 C 1.1572(7) 0.3102(4) 0.7743(5) 0.117(3) Uani 1 1 d . . . H9A H 1.2097 0.3474 0.7798 0.175 Uiso 1 1 calc R . . H9B H 1.1171 0.3221 0.8145 0.175 Uiso 1 1 calc R . . H9C H 1.1057 0.3052 0.7052 0.175 Uiso 1 1 calc R . . C10 C 0.9693(3) 0.18384(18) 0.7791(2) 0.0421(8) Uani 1 1 d . . . C11 C 0.9953(4) 0.1735(2) 0.6385(3) 0.0638(12) Uani 1 1 d . . . H11A H 1.0311 0.1691 0.5952 0.077 Uiso 1 1 calc R . . C12 C 0.8868(4) 0.1763(2) 0.6122(3) 0.0557(10) Uani 1 1 d . . . H12A H 0.8313 0.1743 0.5471 0.067 Uiso 1 1 calc R . . C13 C 0.7669(3) 0.18188(19) 0.7058(2) 0.0435(8) Uani 1 1 d . . . H13A H 0.7561 0.1362 0.7318 0.052 Uiso 1 1 calc R . . H13B H 0.7074 0.1885 0.6395 0.052 Uiso 1 1 calc R . . C14 C 0.8458(3) 0.24708(18) 0.8605(2) 0.0387(7) Uani 1 1 d . . . C15 C 0.6818(3) 0.2869(2) 0.7510(2) 0.0476(8) Uani 1 1 d . . . H15A H 0.6166 0.2907 0.6926 0.057 Uiso 1 1 calc R . . C16 C 0.7135(3) 0.3284(2) 0.8314(2) 0.0481(9) Uani 1 1 d . . . H16A H 0.6742 0.3670 0.8409 0.058 Uiso 1 1 calc R . . C17 C 0.8466(3) 0.3342(2) 1.0677(2) 0.0461(8) Uani 1 1 d . . . C18 C 0.9096(3) 0.3696(2) 1.1543(2) 0.0518(9) Uani 1 1 d . . . H18A H 0.8900 0.3664 1.2089 0.062 Uiso 1 1 calc R . . C19 C 1.0000(3) 0.4095(2) 1.1641(3) 0.0496(9) Uani 1 1 d . . . C20 C 1.0279(3) 0.41411(19) 1.0844(3) 0.0479(8) Uani 1 1 d . . . H20A H 1.0890 0.4418 1.0899 0.058 Uiso 1 1 calc R . . C21 C 0.9687(3) 0.37903(18) 0.9959(2) 0.0428(8) Uani 1 1 d . . . C22 C 0.8793(3) 0.33914(19) 0.9897(2) 0.0400(7) Uani 1 1 d . . . C23 C 0.7474(3) 0.2930(3) 1.0587(3) 0.0609(11) Uani 1 1 d . . . H23A H 0.7497 0.2843 1.1246 0.091 Uiso 1 1 calc R . . H23B H 0.7465 0.2483 1.0261 0.091 Uiso 1 1 calc R . . H23C H 0.6813 0.3196 1.0196 0.091 Uiso 1 1 calc R . . C24 C 1.0666(4) 0.4471(3) 1.2602(3) 0.0732(13) Uani 1 1 d . . . H24A H 1.1145 0.4816 1.2490 0.110 Uiso 1 1 calc R . . H24B H 1.1111 0.4131 1.3096 0.110 Uiso 1 1 calc R . . H24C H 1.0172 0.4710 1.2839 0.110 Uiso 1 1 calc R . . C25 C 1.0041(4) 0.3837(2) 0.9118(3) 0.0633(11) Uani 1 1 d . . . H25A H 0.9395 0.3876 0.8493 0.095 Uiso 1 1 calc R . . H25B H 1.0452 0.3415 0.9107 0.095 Uiso 1 1 calc R . . H25C H 1.0506 0.4249 0.9207 0.095 Uiso 1 1 calc R . . C26 C 1.1966(3) 0.1591(3) 1.0278(3) 0.0552(10) Uani 1 1 d . . . C27 C 1.2964(3) 0.1161(3) 1.0910(3) 0.0869(17) Uani 1 1 d . . . H27A H 1.3628 0.1399 1.0950 0.130 Uiso 1 1 calc R . . H27B H 1.2919 0.0698 1.0614 0.130 Uiso 1 1 calc R . . H27C H 1.2986 0.1110 1.1575 0.130 Uiso 1 1 calc R . . C28 C 0.8980(3) 0.1492(2) 1.0605(3) 0.0496(9) Uani 1 1 d . . . C29 C 0.9042(4) 0.1446(3) 1.1660(3) 0.0674(12) Uani 1 1 d . . . H29A H 0.8314 0.1346 1.1635 0.101 Uiso 1 1 calc R . . H29B H 0.9305 0.1892 1.1999 0.101 Uiso 1 1 calc R . . H29C H 0.9546 0.1071 1.2018 0.101 Uiso 1 1 calc R . . N5 N 0.8175(4) 0.0080(2) 0.6890(3) 0.0820(12) Uani 1 1 d D . . C30 C 0.8606(4) 0.0043(2) 0.7724(3) 0.0631(11) Uani 1 1 d D . . C31 C 0.9142(4) 0.0010(3) 0.8794(3) 0.0674(12) Uani 1 1 d D . . H31A H 0.9908 0.0151 0.9013 0.101 Uiso 1 1 calc R . . H31B H 0.9106 -0.0469 0.9013 0.101 Uiso 1 1 calc R . . H31C H 0.8771 0.0326 0.9079 0.101 Uiso 1 1 calc R . . N6 N 0.9715(11) -0.0810(5) 0.5621(8) 0.089(3) Uani 0.580(7) 1 d PD A 1 C32 C 0.9018(8) -0.0455(5) 0.5204(6) 0.0751(19) Uani 0.580(7) 1 d PD A 1 C33 C 0.8084(12) -0.0003(11) 0.4688(11) 0.088(3) Uani 0.580(7) 1 d PD A 1 H33A H 0.7835 0.0204 0.5164 0.132 Uiso 0.580(7) 1 calc PR A 1 H33B H 0.7491 -0.0278 0.4203 0.132 Uiso 0.580(7) 1 calc PR A 1 H33C H 0.8298 0.0370 0.4349 0.132 Uiso 0.580(7) 1 calc PR A 1 N6' N 0.9640(14) 0.0896(8) 0.4272(12) 0.089(3) Uani 0.420(7) 1 d PD A 2 C32' C 0.8969(11) 0.0561(6) 0.4327(8) 0.0751(19) Uani 0.420(7) 1 d PD A 2 C33' C 0.8109(18) 0.0118(16) 0.4384(18) 0.088(3) Uani 0.420(7) 1 d PD A 2 H33D H 0.8418 -0.0336 0.4668 0.132 Uiso 0.420(7) 1 calc PR A 2 H33E H 0.7536 0.0049 0.3721 0.132 Uiso 0.420(7) 1 calc PR A 2 H33F H 0.7797 0.0345 0.4802 0.132 Uiso 0.420(7) 1 calc PR A 2 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 Pd 0.03038(13) 0.06011(18) 0.02199(12) -0.00470(10) 0.00947(9) -0.00429(11) N1 0.0513(18) 0.090(3) 0.0346(16) -0.0187(15) 0.0247(14) -0.0184(17) N2 0.0419(15) 0.0592(18) 0.0232(12) -0.0068(12) 0.0110(11) -0.0070(13) N3 0.0351(14) 0.0559(17) 0.0230(12) -0.0010(11) 0.0070(10) -0.0025(12) N4 0.0331(13) 0.0589(18) 0.0239(12) -0.0010(11) 0.0074(11) -0.0013(12) O1 0.0371(12) 0.0764(18) 0.0342(12) -0.0026(12) 0.0133(10) 0.0055(12) O2 0.0493(16) 0.108(3) 0.0512(17) -0.0281(17) 0.0164(13) -0.0186(17) O3 0.0354(12) 0.0716(16) 0.0205(10) -0.0020(10) 0.0084(9) 0.0033(11) O4 0.0679(19) 0.109(3) 0.0567(18) -0.0226(17) 0.0338(16) -0.0334(18) C1 0.045(2) 0.135(5) 0.047(2) -0.031(3) 0.0268(19) -0.016(3) C2 0.045(2) 0.197(6) 0.055(3) -0.047(3) 0.028(2) -0.019(3) C3 0.056(3) 0.262(11) 0.081(4) -0.094(6) 0.047(3) -0.062(5) C4 0.087(4) 0.204(8) 0.079(4) -0.083(5) 0.066(4) -0.088(5) C5 0.094(4) 0.133(5) 0.062(3) -0.044(3) 0.058(3) -0.055(4) C6 0.051(2) 0.130(4) 0.039(2) -0.035(2) 0.0311(19) -0.039(3) C7 0.051(2) 0.124(4) 0.075(3) -0.026(3) 0.030(2) -0.002(3) C8 0.049(3) 0.359(14) 0.131(6) -0.141(7) 0.042(4) -0.069(5) C9 0.150(7) 0.136(6) 0.104(5) -0.050(4) 0.093(5) -0.078(5) C10 0.0403(17) 0.057(2) 0.0305(16) -0.0082(14) 0.0163(14) -0.0122(15) C11 0.067(3) 0.101(3) 0.0336(19) -0.019(2) 0.0298(19) -0.021(2) C12 0.066(3) 0.076(3) 0.0253(16) -0.0085(16) 0.0189(17) -0.008(2) C13 0.0399(18) 0.058(2) 0.0263(15) -0.0058(14) 0.0070(13) -0.0069(15) C14 0.0373(16) 0.056(2) 0.0233(14) 0.0001(13) 0.0127(13) -0.0060(14) C15 0.0407(18) 0.069(2) 0.0261(16) 0.0032(15) 0.0063(14) 0.0013(17) C16 0.0405(18) 0.066(2) 0.0322(17) 0.0029(15) 0.0092(14) 0.0066(16) C17 0.0434(19) 0.062(2) 0.0327(17) -0.0060(15) 0.0153(15) -0.0019(16) C18 0.058(2) 0.071(3) 0.0286(16) -0.0055(16) 0.0195(16) -0.0007(19) C19 0.051(2) 0.055(2) 0.0347(18) -0.0067(15) 0.0082(16) -0.0003(17) C20 0.0455(19) 0.049(2) 0.0446(19) -0.0008(16) 0.0138(16) -0.0037(16) C21 0.0462(19) 0.0476(19) 0.0349(17) 0.0015(14) 0.0170(15) 0.0006(15) C22 0.0380(17) 0.0520(19) 0.0268(15) -0.0028(14) 0.0099(13) 0.0004(15) C23 0.055(2) 0.091(3) 0.044(2) -0.010(2) 0.0271(19) -0.015(2) C24 0.076(3) 0.085(3) 0.046(2) -0.022(2) 0.011(2) -0.012(3) C25 0.078(3) 0.071(3) 0.053(2) -0.007(2) 0.040(2) -0.020(2) C26 0.0367(19) 0.098(3) 0.0319(18) -0.010(2) 0.0151(15) 0.001(2) C27 0.041(2) 0.163(5) 0.051(3) 0.002(3) 0.0123(19) 0.021(3) C28 0.050(2) 0.064(2) 0.0322(17) -0.0034(16) 0.0144(16) 0.0026(18) C29 0.065(3) 0.102(4) 0.047(2) 0.002(2) 0.035(2) -0.003(2) N5 0.102(3) 0.074(3) 0.060(2) -0.012(2) 0.023(2) 0.015(2) C30 0.066(3) 0.060(3) 0.066(3) -0.011(2) 0.030(2) 0.006(2) C31 0.063(3) 0.088(3) 0.053(2) -0.006(2) 0.026(2) 0.000(2) N6 0.122(10) 0.079(4) 0.091(5) -0.005(3) 0.068(8) -0.006(7) C32 0.108(6) 0.068(4) 0.057(4) -0.009(3) 0.042(4) -0.006(4) C33 0.111(5) 0.087(8) 0.067(10) -0.002(7) 0.039(6) -0.013(4) N6' 0.122(10) 0.079(4) 0.091(5) -0.005(3) 0.068(8) -0.006(7) C32' 0.108(6) 0.068(4) 0.057(4) -0.009(3) 0.042(4) -0.006(4) C33' 0.111(5) 0.087(8) 0.067(10) -0.002(7) 0.039(6) -0.013(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 Pd C14 1.955(3) . ? Pd C10 1.977(3) . ? Pd O3 2.069(2) . ? Pd O1 2.077(3) . ? N1 C10 1.362(4) . ? N1 C11 1.394(5) . ? N1 C6 1.442(5) . ? N2 C10 1.362(4) . ? N2 C12 1.386(4) . ? N2 C13 1.452(5) . ? N3 C14 1.347(4) . ? N3 C15 1.386(5) . ? N3 C13 1.451(4) . ? N4 C14 1.361(4) . ? N4 C16 1.391(4) . ? N4 C22 1.450(4) . ? O1 C26 1.271(5) . ? O2 C26 1.233(6) . ? O3 C28 1.241(5) . ? O4 C28 1.247(4) . ? C1 C6 1.387(7) . ? C1 C2 1.393(6) . ? C1 C7 1.502(7) . ? C2 C3 1.390(10) . ? C3 C4 1.346(11) . ? C3 C8 1.533(8) . ? C4 C5 1.399(9) . ? C5 C6 1.396(7) . ? C5 C9 1.501(9) . ? C11 C12 1.345(6) . ? C15 C16 1.350(5) . ? C17 C18 1.392(5) . ? C17 C22 1.399(5) . ? C17 C23 1.504(5) . ? C18 C19 1.388(5) . ? C19 C20 1.381(5) . ? C19 C24 1.520(5) . ? C20 C21 1.398(5) . ? C21 C22 1.391(5) . ? C21 C25 1.509(5) . ? C26 C27 1.524(6) . ? C28 C29 1.535(5) . ? N5 C30 1.135(5) . ? C30 C31 1.455(6) . ? N6 C32 1.116(10) . ? C32 C33 1.456(15) . ? N6' C32' 1.134(12) . ? C32' C33' 1.459(15) . ? 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 C14 Pd C10 86.76(14) . . ? C14 Pd O3 92.08(11) . . ? C10 Pd O3 174.08(12) . . ? C14 Pd O1 178.21(11) . . ? C10 Pd O1 94.59(13) . . ? O3 Pd O1 86.46(9) . . ? C10 N1 C11 110.3(3) . . ? C10 N1 C6 127.8(3) . . ? C11 N1 C6 121.8(3) . . ? C10 N2 C12 111.4(3) . . ? C10 N2 C13 123.2(3) . . ? C12 N2 C13 125.2(3) . . ? C14 N3 C15 112.1(3) . . ? C14 N3 C13 121.6(3) . . ? C15 N3 C13 126.4(3) . . ? C14 N4 C16 110.6(3) . . ? C14 N4 C22 126.1(3) . . ? C16 N4 C22 123.1(3) . . ? C26 O1 Pd 110.8(3) . . ? C28 O3 Pd 117.7(2) . . ? C6 C1 C2 117.3(5) . . ? C6 C1 C7 121.3(4) . . ? C2 C1 C7 121.4(6) . . ? C3 C2 C1 121.5(7) . . ? C4 C3 C2 119.4(6) . . ? C4 C3 C8 120.4(8) . . ? C2 C3 C8 120.2(9) . . ? C3 C4 C5 122.1(7) . . ? C6 C5 C4 117.4(7) . . ? C6 C5 C9 122.1(6) . . ? C4 C5 C9 120.6(6) . . ? C1 C6 C5 122.2(5) . . ? C1 C6 N1 119.6(4) . . ? C5 C6 N1 118.0(5) . . ? N1 C10 N2 104.5(3) . . ? N1 C10 Pd 134.1(3) . . ? N2 C10 Pd 121.4(2) . . ? C12 C11 N1 107.5(3) . . ? C11 C12 N2 106.4(3) . . ? N2 C13 N3 109.3(3) . . ? N3 C14 N4 104.3(3) . . ? N3 C14 Pd 124.0(2) . . ? N4 C14 Pd 131.6(2) . . ? C16 C15 N3 106.0(3) . . ? C15 C16 N4 107.0(3) . . ? C18 C17 C22 117.1(3) . . ? C18 C17 C23 121.2(3) . . ? C22 C17 C23 121.7(3) . . ? C19 C18 C17 122.5(3) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 C24 120.9(4) . . ? C18 C19 C24 120.7(4) . . ? C19 C20 C21 121.7(3) . . ? C22 C21 C20 117.9(3) . . ? C22 C21 C25 122.0(3) . . ? C20 C21 C25 120.0(3) . . ? C21 C22 C17 122.3(3) . . ? C21 C22 N4 119.1(3) . . ? C17 C22 N4 118.6(3) . . ? O2 C26 O1 124.6(4) . . ? O2 C26 C27 120.0(4) . . ? O1 C26 C27 115.4(4) . . ? O3 C28 O4 126.8(3) . . ? O3 C28 C29 114.9(3) . . ? O4 C28 C29 118.3(4) . . ? N5 C30 C31 178.6(5) . . ? N6 C32 C33 177.4(13) . . ? N6' C32' C33' 178.8(19) . . ? 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 C14 Pd O1 C26 -113(4) . . . . ? C10 Pd O1 C26 107.9(2) . . . . ? O3 Pd O1 C26 -78.0(2) . . . . ? C14 Pd O3 C28 72.6(3) . . . . ? C10 Pd O3 C28 -6.0(13) . . . . ? O1 Pd O3 C28 -106.4(3) . . . . ? C6 C1 C2 C3 -1.3(7) . . . . ? C7 C1 C2 C3 179.6(4) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? C1 C2 C3 C8 179.0(5) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C8 C3 C4 C5 -179.0(5) . . . . ? C3 C4 C5 C6 1.3(8) . . . . ? C3 C4 C5 C9 -177.3(5) . . . . ? C2 C1 C6 C5 2.6(6) . . . . ? C7 C1 C6 C5 -178.3(4) . . . . ? C2 C1 C6 N1 178.7(3) . . . . ? C7 C1 C6 N1 -2.1(6) . . . . ? C4 C5 C6 C1 -2.6(6) . . . . ? C9 C5 C6 C1 176.0(4) . . . . ? C4 C5 C6 N1 -178.8(4) . . . . ? C9 C5 C6 N1 -0.2(6) . . . . ? C10 N1 C6 C1 93.9(5) . . . . ? C11 N1 C6 C1 -87.5(5) . . . . ? C10 N1 C6 C5 -89.8(5) . . . . ? C11 N1 C6 C5 88.8(5) . . . . ? C11 N1 C10 N2 -0.2(4) . . . . ? C6 N1 C10 N2 178.5(4) . . . . ? C11 N1 C10 Pd 176.6(3) . . . . ? C6 N1 C10 Pd -4.6(7) . . . . ? C12 N2 C10 N1 0.2(4) . . . . ? C13 N2 C10 N1 174.9(3) . . . . ? C12 N2 C10 Pd -177.2(3) . . . . ? C13 N2 C10 Pd -2.4(5) . . . . ? C14 Pd C10 N1 148.5(4) . . . . ? O3 Pd C10 N1 -132.7(11) . . . . ? O1 Pd C10 N1 -32.7(4) . . . . ? C14 Pd C10 N2 -35.0(3) . . . . ? O3 Pd C10 N2 43.8(14) . . . . ? O1 Pd C10 N2 143.8(3) . . . . ? C10 N1 C11 C12 0.2(5) . . . . ? C6 N1 C11 C12 -178.6(4) . . . . ? N1 C11 C12 N2 0.0(5) . . . . ? C10 N2 C12 C11 -0.1(5) . . . . ? C13 N2 C12 C11 -174.7(4) . . . . ? C10 N2 C13 N3 50.8(4) . . . . ? C12 N2 C13 N3 -135.2(3) . . . . ? C14 N3 C13 N2 -48.9(4) . . . . ? C15 N3 C13 N2 130.0(3) . . . . ? C15 N3 C14 N4 -0.1(4) . . . . ? C13 N3 C14 N4 179.0(3) . . . . ? C15 N3 C14 Pd -179.8(2) . . . . ? C13 N3 C14 Pd -0.7(4) . . . . ? C16 N4 C14 N3 0.6(4) . . . . ? C22 N4 C14 N3 -174.5(3) . . . . ? C16 N4 C14 Pd -179.8(3) . . . . ? C22 N4 C14 Pd 5.1(5) . . . . ? C10 Pd C14 N3 37.2(3) . . . . ? O3 Pd C14 N3 -136.9(3) . . . . ? O1 Pd C14 N3 -102(4) . . . . ? C10 Pd C14 N4 -142.3(3) . . . . ? O3 Pd C14 N4 43.5(3) . . . . ? O1 Pd C14 N4 78(4) . . . . ? C14 N3 C15 C16 -0.4(4) . . . . ? C13 N3 C15 C16 -179.4(3) . . . . ? N3 C15 C16 N4 0.8(4) . . . . ? C14 N4 C16 C15 -0.9(4) . . . . ? C22 N4 C16 C15 174.4(3) . . . . ? C22 C17 C18 C19 1.3(6) . . . . ? C23 C17 C18 C19 -178.4(4) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C17 C18 C19 C24 -179.8(4) . . . . ? C18 C19 C20 C21 -0.9(6) . . . . ? C24 C19 C20 C21 179.0(4) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? C19 C20 C21 C25 -178.1(4) . . . . ? C20 C21 C22 C17 1.1(5) . . . . ? C25 C21 C22 C17 179.5(4) . . . . ? C20 C21 C22 N4 178.2(3) . . . . ? C25 C21 C22 N4 -3.4(5) . . . . ? C18 C17 C22 C21 -1.8(5) . . . . ? C23 C17 C22 C21 177.8(4) . . . . ? C18 C17 C22 N4 -179.0(3) . . . . ? C23 C17 C22 N4 0.7(5) . . . . ? C14 N4 C22 C21 71.8(5) . . . . ? C16 N4 C22 C21 -102.7(4) . . . . ? C14 N4 C22 C17 -111.0(4) . . . . ? C16 N4 C22 C17 74.5(5) . . . . ? Pd O1 C26 O2 -9.6(5) . . . . ? Pd O1 C26 C27 168.9(3) . . . . ? Pd O3 C28 O4 -5.5(5) . . . . ? Pd O3 C28 C29 175.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.032 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.077 _vrf_PLAT220_joer062 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) 4.6 RESPONSE: One of the mesityl sidearms have a slight in-plane wagging disorder that cannot be modeled because of the less than 1 Angstrom difference between disordered contributions. We prefer to depict the slight disorder rather than cosmetically apply SIMU/DELU restraints. ;