# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Carlos Peinador' _publ_contact_author_email capeveqo@udc.es loop_ _publ_author_name D.Abella V.Blanco E.Pia M.Chas C.Platas-Iglesias C.Peinador ; J.M.Quintela ; data_0620762_0s _database_code_depnum_ccdc_archive 'CCDC 675724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H74 N16 O30 Pd2' _chemical_formula_weight 1592.05 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 8.684(5) _cell_length_b 13.421(5) _cell_length_c 14.573(5) _cell_angle_alpha 95.949(5) _cell_angle_beta 101.272(5) _cell_angle_gamma 106.982(5) _cell_volume 1569.5(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14503 _cell_measurement_theta_min 5.189 _cell_measurement_theta_max 56.750 _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8598 _exptl_absorpt_correction_T_max 0.9292 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21542 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.38 _reflns_number_total 7715 _reflns_number_gt 7190 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+4.8449P] 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 7715 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 C1 C 0.2077(4) 0.2947(3) 0.9086(2) 0.0175(6) Uani 1 1 d . . . H1 H 0.2876 0.2842 0.8757 0.021 Uiso 1 1 calc R . . C2 C 0.2158(4) 0.2709(3) 0.9990(2) 0.0168(6) Uani 1 1 d . . . H2 H 0.3003 0.2444 1.0277 0.020 Uiso 1 1 calc R . . C3 C 0.0997(4) 0.2859(3) 1.0478(2) 0.0160(6) Uani 1 1 d . . . C4 C -0.0217(5) 0.3253(3) 1.0028(2) 0.0217(7) Uani 1 1 d . . . H4 H -0.1029 0.3366 1.0342 0.026 Uiso 1 1 calc R . . C5 C -0.0229(5) 0.3478(3) 0.9119(2) 0.0214(7) Uani 1 1 d . . . H5 H -0.1057 0.3747 0.8817 0.026 Uiso 1 1 calc R . . C6 C 0.1035(4) 0.2551(3) 1.1430(2) 0.0159(6) Uani 1 1 d . . . C7 C -0.0407(4) 0.2216(3) 1.1754(2) 0.0179(6) Uani 1 1 d . . . H7 H -0.1424 0.2240 1.1388 0.021 Uiso 1 1 calc R . . C8 C -0.0358(4) 0.1847(3) 1.2607(2) 0.0175(6) Uani 1 1 d . . . H8 H -0.1348 0.1606 1.2821 0.021 Uiso 1 1 calc R . . C9 C 0.2516(4) 0.2185(3) 1.2861(2) 0.0184(6) Uani 1 1 d . . . H9 H 0.3527 0.2185 1.3255 0.022 Uiso 1 1 calc R . . C10 C 0.2519(4) 0.2549(3) 1.2014(2) 0.0178(6) Uani 1 1 d . . . H10 H 0.3531 0.2799 1.1825 0.021 Uiso 1 1 calc R . . C11 C 0.1094(4) 0.1345(3) 1.4014(2) 0.0183(6) Uani 1 1 d . . . H11A H 0.0332 0.1551 1.4362 0.022 Uiso 1 1 calc R . . H11B H 0.2222 0.1605 1.4436 0.022 Uiso 1 1 calc R . . C12 C 0.1663(4) -0.0310(3) 1.3501(2) 0.0192(6) Uani 1 1 d . . . H12 H 0.2766 0.0114 1.3534 0.023 Uiso 1 1 calc R . . C13 C -0.1173(4) 0.1405(3) 0.6797(2) 0.0202(6) Uani 1 1 d . . . H13 H -0.1961 0.1710 0.6962 0.024 Uiso 1 1 calc R . . N10 N 0.0362(3) 0.2035(2) 0.68579(19) 0.0147(5) Uani 1 1 d . . . C15 C 0.1518(4) 0.1605(3) 0.6620(2) 0.0150(6) Uani 1 1 d . . . C16 C 0.3154(4) 0.2277(3) 0.6712(2) 0.0195(6) Uani 1 1 d . . . H16 H 0.3448 0.3008 0.6961 0.023 Uiso 1 1 calc R . . C17 C 0.4308(5) 0.1883(3) 0.6446(3) 0.0247(7) Uani 1 1 d . . . H17 H 0.5402 0.2340 0.6506 0.030 Uiso 1 1 calc R . . C18 C 0.3883(5) 0.0795(3) 0.6082(3) 0.0246(7) Uani 1 1 d . . . H18 H 0.4684 0.0531 0.5877 0.029 Uiso 1 1 calc R . . C19 C 0.2328(5) 0.0117(3) 0.6020(2) 0.0214(7) Uani 1 1 d . . . H19 H 0.2077 -0.0616 0.5795 0.026 Uiso 1 1 calc R . . C020 C 0.1084(4) 0.0497(3) 0.6289(2) 0.0157(6) Uani 1 1 d . . . C20 C 0.1420(5) 0.5147(3) 0.6033(2) 0.0233(7) Uani 1 1 d . . . H20A H 0.0349 0.5285 0.5863 0.028 Uiso 1 1 calc R . . H20B H 0.2072 0.5400 0.5568 0.028 Uiso 1 1 calc R . . C21 C 0.2360(5) 0.5723(3) 0.7026(3) 0.0245(7) Uani 1 1 d . . . H21A H 0.3500 0.5682 0.7162 0.029 Uiso 1 1 calc R . . H21B H 0.2425 0.6477 0.7092 0.029 Uiso 1 1 calc R . . C22 C 0.9225(5) 0.9793(3) 0.0742(2) 0.0213(7) Uani 1 1 d . . . C23 C 1.0814(4) 0.9754(3) 0.0819(2) 0.0213(7) Uani 1 1 d . . . H23 H 1.1377 0.9589 0.1381 0.026 Uiso 1 1 calc R . . C24 C 0.8402(4) 1.0045(3) -0.0077(3) 0.0217(7) Uani 1 1 d . . . H24 H 0.7312 1.0080 -0.0131 0.026 Uiso 1 1 calc R . . N1 N 0.0897(4) 0.3325(2) 0.8656(2) 0.0171(5) Uani 1 1 d . . . N2 N 0.1087(4) 0.1828(2) 1.31377(19) 0.0159(5) Uani 1 1 d . . . C56 C 0.0549(4) 0.0151(3) 1.3746(2) 0.0165(6) Uani 1 1 d . . . N4 N 0.1126(4) 0.3993(2) 0.6011(2) 0.0204(6) Uani 1 1 d . . . H4A H 0.1989 0.3815 0.5841 0.024 Uiso 1 1 calc R . . H4B H 0.0167 0.3615 0.5565 0.024 Uiso 1 1 calc R . . N5 N 0.1431(4) 0.5192(2) 0.7693(2) 0.0212(6) Uani 1 1 d . . . H5A H 0.0462 0.5352 0.7655 0.025 Uiso 1 1 calc R . . H5B H 0.2058 0.5416 0.8307 0.025 Uiso 1 1 calc R . . N6 N 0.2729(4) 0.4842(3) 0.2997(2) 0.0268(7) Uani 1 1 d . . . N7 N 0.7023(4) 0.2493(2) 0.4770(2) 0.0216(6) Uani 1 1 d . . . N8 N 0.5649(5) 0.1410(3) 0.8628(3) 0.0333(8) Uani 1 1 d . . . O1 O 0.8517(3) 0.9585(2) 0.14974(19) 0.0266(6) Uani 1 1 d . . . H1A H 0.7547 0.9614 0.1367 0.040 Uiso 1 1 calc R . . O2 O 0.2176(4) 0.5088(3) 0.2224(2) 0.0357(7) Uani 1 1 d . . . O3 O 0.4247(4) 0.5047(3) 0.3305(3) 0.0468(9) Uani 1 1 d . . . O4 O 0.1736(4) 0.4365(2) 0.3442(2) 0.0341(7) Uani 1 1 d . . . O5 O 0.8317(3) 0.2483(2) 0.4514(2) 0.0271(6) Uani 1 1 d . . . O6 O 0.5655(4) 0.1816(2) 0.4349(2) 0.0322(6) Uani 1 1 d . . . O7 O 0.7110(4) 0.3171(3) 0.5439(2) 0.0414(8) Uani 1 1 d . . . O8 O 0.4825(4) 0.0731(3) 0.9064(2) 0.0379(7) Uani 1 1 d . . . O9 O 0.6271(4) 0.1086(3) 0.8023(2) 0.0430(8) Uani 1 1 d . . . O10 O 0.5802(5) 0.2366(3) 0.8829(3) 0.0478(8) Uani 1 1 d . . . O21 O 0.3466(4) 0.3587(2) 0.49427(19) 0.0299(6) Uani 1 1 d . . . H21C H 0.3544 0.3913 0.4568 0.045 Uiso 1 1 d R . . H21D H 0.4511 0.4011 0.5292 0.045 Uiso 1 1 d R . . O22 O 0.5633(4) 0.2024(3) 0.0862(2) 0.0413(8) Uani 1 1 d . . . H22A H 0.5524 0.1715 0.0304 0.062 Uiso 1 1 d R . . H22B H 0.6217 0.2739 0.0894 0.062 Uiso 1 1 d R . . O23 O 0.5578(5) 0.1145(3) 0.2447(3) 0.0474(8) Uani 1 1 d . . . H35B H 0.5829 0.1341 0.3048 0.071 Uiso 1 1 d R . . H35A H 0.5615 0.1483 0.2039 0.071 Uiso 1 1 d R . . O34 O 0.6266(4) 0.4046(3) 0.0553(2) 0.0401(7) Uani 1 1 d . . . H34A H 0.6313 0.4210 0.0019 0.060 Uiso 1 1 d R . . H34B H 0.5596 0.4536 0.0493 0.060 Uiso 1 1 d R . . O40 O 0.5293(4) 0.4540(3) -0.1192(3) 0.0429(8) Uani 1 1 d . . . H40B H 0.6187 0.4858 -0.0820 0.064 Uiso 1 1 d R . . H40A H 0.5066 0.5173 -0.1226 0.064 Uiso 1 1 d R . . Pd1 Pd 0.09279(3) 0.361612(19) 0.731349(16) 0.01480(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0184(15) 0.0195(16) 0.0161(14) 0.0050(12) 0.0045(12) 0.0076(13) C2 0.0165(14) 0.0169(15) 0.0161(14) 0.0039(12) 0.0017(11) 0.0052(12) C3 0.0194(15) 0.0135(14) 0.0135(13) 0.0019(11) 0.0021(11) 0.0042(12) C4 0.0269(17) 0.0270(18) 0.0188(15) 0.0083(13) 0.0094(13) 0.0159(15) C5 0.0264(17) 0.0275(18) 0.0181(15) 0.0099(13) 0.0082(13) 0.0164(15) C6 0.0203(15) 0.0146(14) 0.0141(13) 0.0034(11) 0.0040(12) 0.0072(12) C7 0.0205(15) 0.0183(15) 0.0161(14) 0.0044(12) 0.0027(12) 0.0088(13) C8 0.0187(15) 0.0157(15) 0.0180(15) 0.0046(12) 0.0043(12) 0.0048(12) C9 0.0186(15) 0.0185(16) 0.0163(14) 0.0039(12) 0.0008(12) 0.0052(13) C10 0.0187(15) 0.0181(15) 0.0161(14) 0.0047(12) 0.0038(12) 0.0047(13) C11 0.0262(17) 0.0148(15) 0.0127(14) 0.0056(11) 0.0031(12) 0.0046(13) C12 0.0174(15) 0.0159(15) 0.0217(15) 0.0052(12) 0.0037(12) 0.0014(13) C13 0.0213(16) 0.0227(17) 0.0213(15) 0.0074(13) 0.0070(13) 0.0114(14) N10 0.0169(12) 0.0126(12) 0.0138(12) 0.0041(9) 0.0045(10) 0.0025(10) C15 0.0183(15) 0.0167(15) 0.0104(13) 0.0054(11) 0.0034(11) 0.0050(12) C16 0.0191(15) 0.0194(16) 0.0185(15) 0.0060(12) 0.0038(12) 0.0034(13) C17 0.0209(16) 0.0281(19) 0.0270(18) 0.0121(15) 0.0077(14) 0.0070(15) C18 0.0244(17) 0.0283(19) 0.0267(17) 0.0098(15) 0.0100(14) 0.0127(15) C19 0.0289(18) 0.0219(17) 0.0191(15) 0.0085(13) 0.0094(13) 0.0125(15) C020 0.0220(15) 0.0162(15) 0.0111(13) 0.0069(11) 0.0046(11) 0.0071(13) C20 0.0343(19) 0.0174(16) 0.0194(16) 0.0097(13) 0.0053(14) 0.0084(15) C21 0.0327(19) 0.0139(16) 0.0239(17) 0.0050(13) 0.0035(14) 0.0047(14) C22 0.0268(17) 0.0165(16) 0.0190(15) 0.0028(12) 0.0067(13) 0.0041(14) C23 0.0237(16) 0.0193(16) 0.0173(15) 0.0031(12) -0.0005(13) 0.0052(14) C24 0.0186(15) 0.0217(17) 0.0239(17) 0.0050(13) 0.0040(13) 0.0053(13) N1 0.0223(14) 0.0166(13) 0.0144(12) 0.0053(10) 0.0045(10) 0.0081(11) N2 0.0221(14) 0.0125(12) 0.0127(12) 0.0040(10) 0.0029(10) 0.0050(11) C56 0.0229(16) 0.0148(15) 0.0101(13) 0.0046(11) 0.0002(11) 0.0050(13) N4 0.0275(15) 0.0167(14) 0.0145(12) 0.0059(10) 0.0023(11) 0.0039(12) N5 0.0295(15) 0.0160(13) 0.0172(13) 0.0022(11) 0.0013(11) 0.0090(12) N6 0.0297(16) 0.0207(15) 0.0275(16) 0.0007(12) 0.0003(13) 0.0097(13) N7 0.0261(15) 0.0186(14) 0.0203(14) 0.0075(11) 0.0071(12) 0.0049(12) N8 0.0305(18) 0.042(2) 0.0289(17) 0.0088(15) 0.0058(14) 0.0133(16) O1 0.0267(13) 0.0341(15) 0.0210(12) 0.0093(11) 0.0098(10) 0.0087(12) O2 0.0377(16) 0.0396(17) 0.0333(16) 0.0156(13) 0.0054(13) 0.0163(14) O3 0.0282(16) 0.052(2) 0.051(2) -0.0020(17) -0.0076(14) 0.0137(15) O4 0.0465(18) 0.0307(15) 0.0311(15) 0.0088(12) 0.0125(13) 0.0178(14) O5 0.0243(13) 0.0236(13) 0.0336(14) 0.0024(11) 0.0071(11) 0.0089(11) O6 0.0247(14) 0.0326(16) 0.0350(15) 0.0013(12) 0.0050(12) 0.0056(12) O7 0.0475(19) 0.0329(16) 0.0351(16) -0.0091(13) 0.0250(15) -0.0050(14) O8 0.0328(16) 0.051(2) 0.0372(16) 0.0180(15) 0.0151(13) 0.0159(15) O9 0.0365(17) 0.067(2) 0.0394(17) 0.0196(16) 0.0166(14) 0.0284(17) O10 0.052(2) 0.042(2) 0.047(2) 0.0074(16) 0.0073(17) 0.0145(17) O21 0.0346(15) 0.0258(14) 0.0203(12) 0.0053(11) 0.0020(11) -0.0011(12) O22 0.0367(17) 0.051(2) 0.0375(17) 0.0092(15) 0.0039(13) 0.0184(15) O23 0.062(2) 0.047(2) 0.0354(17) 0.0098(15) 0.0097(16) 0.0215(18) O34 0.0347(16) 0.0446(19) 0.0338(16) -0.0037(14) -0.0037(13) 0.0131(15) O40 0.0395(18) 0.0409(19) 0.0473(19) 0.0035(15) 0.0134(15) 0.0109(15) Pd1 0.02025(14) 0.01279(13) 0.01175(13) 0.00410(8) 0.00268(9) 0.00594(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.348(4) . ? C1 C2 1.381(4) . ? C2 C3 1.391(5) . ? C3 C4 1.396(5) . ? C3 C6 1.485(4) . ? C4 C5 1.387(5) . ? C5 N1 1.343(4) . ? C6 C7 1.392(5) . ? C6 C10 1.400(5) . ? C7 C8 1.383(4) . ? C8 N2 1.348(4) . ? C9 N2 1.349(5) . ? C9 C10 1.374(5) . ? C11 N2 1.491(4) . ? C11 C56 1.516(5) . ? C12 C56 1.374(5) . ? C12 C13 1.399(5) 2_557 ? C13 N10 1.334(5) . ? C13 C12 1.399(5) 2_557 ? N10 C15 1.377(4) . ? N10 Pd1 2.038(3) . ? C15 C16 1.415(5) . ? C15 C020 1.427(5) . ? C16 C17 1.362(5) . ? C17 C18 1.413(6) . ? C18 C19 1.370(5) . ? C19 C020 1.424(5) . ? C020 C56 1.418(5) 2_557 ? C20 N4 1.490(4) . ? C20 C21 1.516(5) . ? C21 N5 1.489(5) . ? C22 O1 1.377(4) . ? C22 C23 1.379(5) . ? C22 C24 1.394(5) . ? C23 C24 1.395(5) 2_775 ? C24 C23 1.395(5) 2_775 ? N1 Pd1 2.038(3) . ? C56 C020 1.418(5) 2_557 ? N4 Pd1 2.041(3) . ? N5 Pd1 2.024(3) . ? N6 O3 1.244(5) . ? N6 O4 1.247(5) . ? N6 O2 1.252(4) . ? N7 O7 1.238(4) . ? N7 O5 1.255(4) . ? N7 O6 1.258(4) . ? N8 O9 1.226(5) . ? N8 O10 1.248(5) . ? N8 O8 1.290(5) . ? 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 N1 C1 C2 121.9(3) . . ? C1 C2 C3 119.6(3) . . ? C2 C3 C4 118.0(3) . . ? C2 C3 C6 119.5(3) . . ? C4 C3 C6 122.4(3) . . ? C5 C4 C3 119.5(3) . . ? N1 C5 C4 121.8(3) . . ? C7 C6 C10 118.0(3) . . ? C7 C6 C3 121.2(3) . . ? C10 C6 C3 120.7(3) . . ? C8 C7 C6 120.0(3) . . ? N2 C8 C7 120.3(3) . . ? N2 C9 C10 120.4(3) . . ? C9 C10 C6 120.1(3) . . ? N2 C11 C56 109.5(3) . . ? C56 C12 C13 120.0(3) . 2_557 ? N10 C13 C12 122.4(3) . 2_557 ? C13 N10 C15 119.5(3) . . ? C13 N10 Pd1 118.6(2) . . ? C15 N10 Pd1 121.9(2) . . ? N10 C15 C16 119.0(3) . . ? N10 C15 C020 120.8(3) . . ? C16 C15 C020 120.2(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 120.1(3) . . ? C19 C18 C17 120.8(3) . . ? C18 C19 C020 120.8(3) . . ? C56 C020 C19 124.3(3) 2_557 . ? C56 C020 C15 118.1(3) 2_557 . ? C19 C020 C15 117.6(3) . . ? N4 C20 C21 108.4(3) . . ? N5 C21 C20 106.8(3) . . ? O1 C22 C23 117.6(3) . . ? O1 C22 C24 122.5(3) . . ? C23 C22 C24 119.9(3) . . ? C22 C23 C24 120.4(3) . 2_775 ? C22 C24 C23 119.7(3) . 2_775 ? C5 N1 C1 119.2(3) . . ? C5 N1 Pd1 123.8(2) . . ? C1 N1 Pd1 117.0(2) . . ? C8 N2 C9 121.1(3) . . ? C8 N2 C11 119.5(3) . . ? C9 N2 C11 119.3(3) . . ? C12 C56 C020 119.1(3) . 2_557 ? C12 C56 C11 118.6(3) . . ? C020 C56 C11 122.2(3) 2_557 . ? C20 N4 Pd1 110.2(2) . . ? C21 N5 Pd1 107.4(2) . . ? O3 N6 O4 120.4(4) . . ? O3 N6 O2 120.4(4) . . ? O4 N6 O2 119.2(3) . . ? O7 N7 O5 119.4(3) . . ? O7 N7 O6 120.7(3) . . ? O5 N7 O6 119.9(3) . . ? O9 N8 O10 122.0(4) . . ? O9 N8 O8 118.0(4) . . ? O10 N8 O8 120.1(4) . . ? N5 Pd1 N1 93.64(12) . . ? N5 Pd1 N10 176.85(11) . . ? N1 Pd1 N10 89.18(11) . . ? N5 Pd1 N4 83.67(12) . . ? N1 Pd1 N4 175.73(12) . . ? N10 Pd1 N4 93.60(11) . . ? 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 N1 C1 C2 C3 0.0(5) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C1 C2 C3 C6 176.9(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C6 C3 C4 C5 -176.9(3) . . . . ? C3 C4 C5 N1 0.1(6) . . . . ? C2 C3 C6 C7 -149.8(3) . . . . ? C4 C3 C6 C7 27.1(5) . . . . ? C2 C3 C6 C10 27.6(5) . . . . ? C4 C3 C6 C10 -155.4(3) . . . . ? C10 C6 C7 C8 -3.1(5) . . . . ? C3 C6 C7 C8 174.4(3) . . . . ? C6 C7 C8 N2 1.2(5) . . . . ? N2 C9 C10 C6 -0.1(5) . . . . ? C7 C6 C10 C9 2.5(5) . . . . ? C3 C6 C10 C9 -175.0(3) . . . . ? C12 C13 N10 C15 0.1(5) 2_557 . . . ? C12 C13 N10 Pd1 -179.5(3) 2_557 . . . ? C13 N10 C15 C16 -178.3(3) . . . . ? Pd1 N10 C15 C16 1.2(4) . . . . ? C13 N10 C15 C020 1.4(4) . . . . ? Pd1 N10 C15 C020 -179.1(2) . . . . ? N10 C15 C16 C17 -177.3(3) . . . . ? C020 C15 C16 C17 3.0(5) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C19 -2.2(6) . . . . ? C17 C18 C19 C020 2.3(5) . . . . ? C18 C19 C020 C56 -179.6(3) . . . 2_557 ? C18 C19 C020 C15 0.2(5) . . . . ? N10 C15 C020 C56 -2.7(4) . . . 2_557 ? C16 C15 C020 C56 176.9(3) . . . 2_557 ? N10 C15 C020 C19 177.5(3) . . . . ? C16 C15 C020 C19 -2.8(4) . . . . ? N4 C20 C21 N5 -51.3(4) . . . . ? O1 C22 C23 C24 179.8(3) . . . 2_775 ? C24 C22 C23 C24 -0.6(6) . . . 2_775 ? O1 C22 C24 C23 -179.9(3) . . . 2_775 ? C23 C22 C24 C23 0.6(6) . . . 2_775 ? C4 C5 N1 C1 -0.3(6) . . . . ? C4 C5 N1 Pd1 179.0(3) . . . . ? C2 C1 N1 C5 0.3(5) . . . . ? C2 C1 N1 Pd1 -179.1(3) . . . . ? C7 C8 N2 C9 1.3(5) . . . . ? C7 C8 N2 C11 -174.9(3) . . . . ? C10 C9 N2 C8 -1.9(5) . . . . ? C10 C9 N2 C11 174.3(3) . . . . ? C56 C11 N2 C8 79.2(4) . . . . ? C56 C11 N2 C9 -97.1(3) . . . . ? C13 C12 C56 C020 1.2(5) 2_557 . . 2_557 ? C13 C12 C56 C11 -176.7(3) 2_557 . . . ? N2 C11 C56 C12 77.2(4) . . . . ? N2 C11 C56 C020 -100.7(3) . . . 2_557 ? C21 C20 N4 Pd1 30.2(4) . . . . ? C20 C21 N5 Pd1 47.9(3) . . . . ? C21 N5 Pd1 N1 151.6(2) . . . . ? C21 N5 Pd1 N10 -55(2) . . . . ? C21 N5 Pd1 N4 -25.0(2) . . . . ? C5 N1 Pd1 N5 65.3(3) . . . . ? C1 N1 Pd1 N5 -115.4(3) . . . . ? C5 N1 Pd1 N10 -113.3(3) . . . . ? C1 N1 Pd1 N10 66.0(3) . . . . ? C5 N1 Pd1 N4 116.0(15) . . . . ? C1 N1 Pd1 N4 -64.6(16) . . . . ? C13 N10 Pd1 N5 -81(2) . . . . ? C15 N10 Pd1 N5 100(2) . . . . ? C13 N10 Pd1 N1 73.1(3) . . . . ? C15 N10 Pd1 N1 -106.4(2) . . . . ? C13 N10 Pd1 N4 -110.1(3) . . . . ? C15 N10 Pd1 N4 70.3(2) . . . . ? C20 N4 Pd1 N5 -3.0(2) . . . . ? C20 N4 Pd1 N1 -54.1(16) . . . . ? C20 N4 Pd1 N10 175.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.195 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.189 # Attachment 'NPH.cif' data_0620086s _database_code_depnum_ccdc_archive 'CCDC 675725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H72 N16 O24 Pd2' _chemical_formula_weight 1638.16 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 11.818(2) _cell_length_b 12.632(2) _cell_length_c 12.814(2) _cell_angle_alpha 109.691(3) _cell_angle_beta 97.742(3) _cell_angle_gamma 99.527(3) _cell_volume 1738.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4753 _cell_measurement_theta_min 4.408 _cell_measurement_theta_max 42.905 _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8482 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23236 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.1308 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.34 _reflns_number_total 8549 _reflns_number_gt 4024 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to the disorder in the pendant chains of the 1,5-bis[2-(2-hydroxyethoxy)ethoxy]naphtalene moiety and one of the nitrate counterion, 239 restraints were used in the refinement. These restraints are dfix, sadi, simu and delu instructions ; _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^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8549 _refine_ls_number_parameters 525 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.1548 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.40861(4) 0.48263(4) 0.23996(4) 0.05132(19) Uani 1 1 d . . . O1 O 0.1442(5) 0.0586(5) 0.2281(4) 0.0919(15) Uani 1 1 d DU . . O3A O 0.470(2) -0.1433(17) 0.3001(18) 0.190(7) Uani 0.50 1 d PDU A 1 H3A H 0.4224 -0.1520 0.2414 0.285 Uiso 0.50 1 calc PR A 1 O2A O 0.3826(19) 0.089(2) 0.357(2) 0.172(8) Uani 0.50 1 d PDU A 1 O3B O 0.4793(16) -0.0309(14) 0.1653(14) 0.153(5) Uani 0.50 1 d PDU B 2 H3B H 0.4455 -0.1008 0.1314 0.230 Uiso 0.50 1 calc PR B 2 O2B O 0.3738(17) 0.081(2) 0.321(2) 0.145(6) Uani 0.50 1 d PDU B 2 N1 N -0.3631(4) -0.3223(4) -0.1155(4) 0.0557(12) Uani 1 1 d . . . N2 N -0.1258(4) 0.2279(4) 0.3065(4) 0.0521(12) Uani 1 1 d . . . N3 N 0.2552(4) 0.4505(4) 0.2917(4) 0.0528(12) Uani 1 1 d . . . N4 N 0.4608(5) 0.6470(4) 0.3546(5) 0.0721(15) Uani 1 1 d . . . H4B H 0.4183 0.6866 0.3087 0.086 Uiso 1 1 d R . . H4A H 0.4484 0.6433 0.4156 0.086 Uiso 1 1 d R . . N5 N 0.5700(5) 0.5171(5) 0.2035(4) 0.0645(14) Uani 1 1 d . . . H5A H 0.5541 0.4860 0.1146 0.077 Uiso 1 1 d R . . H5B H 0.5989 0.4519 0.2335 0.077 Uiso 1 1 d R . . C1 C -0.1036(6) 0.1324(6) 0.3202(5) 0.0612(16) Uani 1 1 d . . . H1 H -0.0516 0.1398 0.3869 0.073 Uiso 1 1 calc R . . C2 C -0.2002(6) 0.2180(6) 0.2136(5) 0.0655(17) Uani 1 1 d . . . H2 H -0.2169 0.2856 0.2042 0.079 Uiso 1 1 calc R . . C3 C 0.0640(8) -0.1346(7) 0.0886(7) 0.090(2) Uani 1 1 d . . . H3 H 0.0964 -0.1693 0.1372 0.108 Uiso 1 1 calc R A . C4 C -0.1527(6) 0.0257(5) 0.2420(5) 0.0614(16) Uani 1 1 d . . . H4 H -0.1351 -0.0403 0.2546 0.074 Uiso 1 1 calc R . . C5 C -0.2286(5) 0.0124(5) 0.1438(5) 0.0495(14) Uani 1 1 d . . . C6 C -0.2820(5) -0.1031(5) 0.0547(4) 0.0488(14) Uani 1 1 d . . . C7 C -0.3347(6) -0.1174(5) -0.0542(5) 0.0644(17) Uani 1 1 d . . . H7 H -0.3445 -0.0520 -0.0722 0.077 Uiso 1 1 calc R . . C8 C -0.3725(6) -0.2261(6) -0.1356(5) 0.0665(17) Uani 1 1 d . . . H8 H -0.4071 -0.2337 -0.2099 0.080 Uiso 1 1 calc R . . C9 C -0.3147(6) -0.3076(6) -0.0099(5) 0.0684(18) Uani 1 1 d . . . H9 H -0.3089 -0.3744 0.0072 0.082 Uiso 1 1 calc R . . C10 C -0.2734(6) -0.2033(5) 0.0741(5) 0.0644(17) Uani 1 1 d . . . H10 H -0.2382 -0.1986 0.1472 0.077 Uiso 1 1 calc R . . C11 C -0.0646(5) 0.3444(5) 0.3934(5) 0.0572(15) Uani 1 1 d . . . H11A H -0.0458 0.3384 0.4686 0.069 Uiso 1 1 calc R . . H11B H -0.1169 0.3988 0.3983 0.069 Uiso 1 1 calc R . . C12 C 0.0473(5) 0.3897(5) 0.3614(4) 0.0505(14) Uani 1 1 d . . . C13 C 0.1483(5) 0.3623(5) 0.3975(4) 0.0536(14) Uani 1 1 d . . . H13 H 0.1491 0.3211 0.4473 0.064 Uiso 1 1 calc R . . C14 C 0.2503(5) 0.3942(5) 0.3618(5) 0.0562(15) Uani 1 1 d . . . H14 H 0.3196 0.3747 0.3891 0.067 Uiso 1 1 calc R . . C15 C 0.1566(5) 0.4826(5) 0.2553(5) 0.0549(15) Uani 1 1 d . . . C16 C 0.1597(7) 0.5433(6) 0.1812(6) 0.075(2) Uani 1 1 d . . . H16 H 0.2301 0.5615 0.1565 0.090 Uiso 1 1 calc R . . C17 C 0.0633(9) 0.5758(7) 0.1451(7) 0.095(3) Uani 1 1 d . . . H17 H 0.0663 0.6161 0.0945 0.114 Uiso 1 1 calc R . . C18 C -0.0388(8) 0.5514(7) 0.1806(8) 0.094(3) Uani 1 1 d . . . H18 H -0.1051 0.5761 0.1549 0.113 Uiso 1 1 calc R . . C19 C -0.0477(6) 0.4923(6) 0.2523(6) 0.0721(19) Uani 1 1 d . . . H19 H -0.1195 0.4765 0.2757 0.086 Uiso 1 1 calc R . . C20 C 0.0497(5) 0.4552(5) 0.2913(5) 0.0558(15) Uani 1 1 d . . . C21 C 0.0496(6) 0.1574(5) 0.0894(5) 0.0626(16) Uani 1 1 d . . . H21 H 0.0939 0.2057 0.1626 0.075 Uiso 1 1 calc R . . C22 C -0.0019(8) -0.2035(7) -0.0200(7) 0.087(2) Uani 1 1 d . . . H22 H -0.0129 -0.2850 -0.0445 0.105 Uiso 1 1 calc R . . C23 C -0.2529(6) 0.1124(6) 0.1319(5) 0.0640(17) Uani 1 1 d . . . H23 H -0.3061 0.1072 0.0669 0.077 Uiso 1 1 calc R . . C24 C 0.0813(6) -0.0192(7) 0.1234(5) 0.0675(18) Uani 1 1 d . . . C25 C 0.0340(5) 0.0350(5) 0.0537(5) 0.0554(15) Uani 1 1 d . . . C26A C 0.1753(17) 0.0350(18) 0.3321(11) 0.092(5) Uani 0.50 1 d PDU A 1 H26A H 0.1110 -0.0205 0.3407 0.110 Uiso 0.50 1 calc PR A 1 H26B H 0.1965 0.1067 0.4004 0.110 Uiso 0.50 1 calc PR A 1 C27A C 0.2819(15) -0.0174(17) 0.308(2) 0.119(5) Uani 0.50 1 d PDU A 1 H27A H 0.2907 -0.0725 0.3464 0.142 Uiso 0.50 1 calc PR A 1 H27B H 0.2758 -0.0571 0.2255 0.142 Uiso 0.50 1 calc PR A 1 C28A C 0.488(2) 0.055(3) 0.306(3) 0.170(7) Uani 0.50 1 d PDU A 1 H28A H 0.4613 0.0190 0.2232 0.204 Uiso 0.50 1 calc PR A 1 H28B H 0.5467 0.1274 0.3222 0.204 Uiso 0.50 1 calc PR A 1 C29A C 0.552(2) -0.024(2) 0.343(3) 0.174(8) Uani 0.50 1 d PDU A 1 H29A H 0.5747 0.0053 0.4269 0.208 Uiso 0.50 1 calc PR A 1 H29B H 0.6238 -0.0286 0.3119 0.208 Uiso 0.50 1 calc PR A 1 C26B C 0.184(2) -0.0109(13) 0.2883(15) 0.117(6) Uani 0.50 1 d PDU B 2 H26C H 0.2104 -0.0751 0.2359 0.141 Uiso 0.50 1 calc PR B 2 H26D H 0.1180 -0.0446 0.3158 0.141 Uiso 0.50 1 calc PR B 2 C27B C 0.2827(16) 0.059(2) 0.3868(16) 0.137(6) Uani 0.50 1 d PDU B 2 H27C H 0.3054 0.0144 0.4334 0.164 Uiso 0.50 1 calc PR B 2 H27D H 0.2647 0.1312 0.4352 0.164 Uiso 0.50 1 calc PR B 2 C28B C 0.477(2) 0.052(3) 0.382(2) 0.160(7) Uani 0.50 1 d PDU B 2 H28C H 0.5333 0.1230 0.4355 0.192 Uiso 0.50 1 calc PR B 2 H28D H 0.4507 0.0023 0.4229 0.192 Uiso 0.50 1 calc PR B 2 C29B C 0.531(3) -0.010(3) 0.2860(17) 0.173(8) Uani 0.50 1 d PDU B 2 H29C H 0.6130 0.0322 0.3019 0.207 Uiso 0.50 1 calc PR B 2 H29D H 0.5325 -0.0868 0.2902 0.207 Uiso 0.50 1 calc PR B 2 C30 C 0.6206(7) 0.6400(6) 0.2575(6) 0.0750(19) Uani 1 1 d . . . H30A H 0.5905 0.6810 0.2099 0.090 Uiso 1 1 calc R . . H30B H 0.7069 0.6547 0.2666 0.090 Uiso 1 1 calc R . . C31 C 0.5883(8) 0.6835(7) 0.3712(6) 0.089(2) Uani 1 1 d . . . H31A H 0.6278 0.6512 0.4226 0.107 Uiso 1 1 calc R . . H31B H 0.6132 0.7687 0.4052 0.107 Uiso 1 1 calc R . . N6 N 0.6365(5) 0.3774(5) 0.4078(5) 0.0694(15) Uani 1 1 d . . . O4 O 0.6897(5) 0.3331(5) 0.4653(5) 0.0896(15) Uani 1 1 d . . . O5 O 0.5368(5) 0.3874(6) 0.4143(5) 0.110(2) Uani 1 1 d . . . O6 O 0.6899(5) 0.4208(5) 0.3483(5) 0.1002(17) Uani 1 1 d . . . N7 N 0.9458(8) 0.8047(7) 0.3822(6) 0.126(3) Uani 1 1 d DU . . O8 O 1.0549(8) 0.8104(14) 0.4138(8) 0.269(7) Uani 1 1 d DU . . O7 O 0.9155(6) 0.8051(5) 0.2882(5) 0.119(2) Uani 1 1 d DU . . O9 O 0.8929(7) 0.7654(7) 0.4339(6) 0.146(3) Uani 1 1 d DU . . N8 N 0.3645(8) 0.6724(7) 0.0325(8) 0.103(2) Uani 1 1 d . . . O10 O 0.3901(7) 0.5884(6) 0.0325(5) 0.122(2) Uani 1 1 d . . . O11 O 0.3575(12) 0.7019(11) -0.0395(11) 0.236(6) Uani 1 1 d . . . O12 O 0.3589(12) 0.7437(9) 0.1276(12) 0.249(6) 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 0.0591(3) 0.0527(3) 0.0406(3) 0.01606(19) 0.01615(19) 0.0060(2) O1 0.096(4) 0.110(4) 0.059(3) 0.034(3) -0.006(3) 0.008(3) O3A 0.22(2) 0.191(14) 0.187(19) 0.085(16) 0.034(15) 0.088(13) O2A 0.106(9) 0.202(13) 0.160(15) 0.026(13) -0.007(11) 0.019(8) O3B 0.162(15) 0.153(13) 0.166(11) 0.080(11) 0.057(11) 0.026(12) O2B 0.108(9) 0.202(13) 0.164(13) 0.118(11) 0.003(8) 0.048(9) N1 0.065(3) 0.058(3) 0.042(3) 0.017(2) 0.015(2) 0.006(3) N2 0.052(3) 0.053(3) 0.046(3) 0.010(2) 0.020(2) 0.009(2) N3 0.058(3) 0.055(3) 0.047(3) 0.021(2) 0.014(2) 0.011(2) N4 0.080(4) 0.067(3) 0.065(3) 0.020(3) 0.033(3) 0.000(3) N5 0.065(3) 0.075(4) 0.050(3) 0.022(3) 0.016(3) 0.006(3) C1 0.062(4) 0.074(5) 0.041(3) 0.019(3) 0.006(3) 0.007(3) C2 0.065(4) 0.061(4) 0.064(4) 0.015(3) 0.007(3) 0.018(3) C3 0.112(7) 0.083(6) 0.086(6) 0.046(5) 0.008(5) 0.029(5) C4 0.074(4) 0.058(4) 0.047(3) 0.016(3) 0.010(3) 0.010(3) C5 0.048(3) 0.058(4) 0.043(3) 0.018(3) 0.015(3) 0.011(3) C6 0.044(3) 0.061(4) 0.035(3) 0.012(3) 0.009(2) 0.005(3) C7 0.074(4) 0.054(4) 0.056(4) 0.011(3) 0.006(3) 0.018(3) C8 0.075(5) 0.072(5) 0.042(3) 0.013(3) 0.001(3) 0.015(4) C9 0.088(5) 0.065(4) 0.056(4) 0.033(3) 0.012(4) 0.004(4) C10 0.090(5) 0.056(4) 0.038(3) 0.016(3) 0.007(3) -0.005(3) C11 0.058(4) 0.057(4) 0.048(3) 0.007(3) 0.018(3) 0.013(3) C12 0.051(4) 0.051(3) 0.037(3) 0.002(3) 0.013(3) 0.007(3) C13 0.054(4) 0.062(4) 0.040(3) 0.019(3) 0.009(3) 0.002(3) C14 0.053(4) 0.070(4) 0.042(3) 0.020(3) 0.007(3) 0.008(3) C15 0.063(4) 0.051(3) 0.052(3) 0.017(3) 0.014(3) 0.016(3) C16 0.100(6) 0.062(4) 0.078(5) 0.037(4) 0.031(4) 0.021(4) C17 0.112(7) 0.088(6) 0.103(6) 0.054(5) 0.014(6) 0.039(5) C18 0.082(6) 0.089(6) 0.122(7) 0.044(5) 0.015(5) 0.044(5) C19 0.071(5) 0.062(4) 0.084(5) 0.023(4) 0.016(4) 0.026(4) C20 0.063(4) 0.042(3) 0.059(4) 0.009(3) 0.017(3) 0.019(3) C21 0.067(4) 0.057(4) 0.054(4) 0.009(3) 0.018(3) 0.007(3) C22 0.106(6) 0.065(5) 0.096(6) 0.034(5) 0.020(5) 0.023(5) C23 0.061(4) 0.064(4) 0.055(4) 0.009(3) 0.002(3) 0.015(3) C24 0.061(4) 0.088(5) 0.055(4) 0.031(4) 0.011(3) 0.012(4) C25 0.051(4) 0.067(4) 0.045(3) 0.017(3) 0.019(3) 0.007(3) C26A 0.107(9) 0.119(12) 0.040(8) 0.025(8) 0.016(8) 0.009(9) C27A 0.129(10) 0.127(12) 0.101(12) 0.049(10) -0.004(10) 0.037(8) C28A 0.120(11) 0.205(14) 0.201(17) 0.093(15) 0.008(12) 0.064(11) C29A 0.167(17) 0.232(17) 0.185(18) 0.139(16) 0.048(16) 0.070(11) C26B 0.131(11) 0.147(15) 0.064(11) 0.048(10) -0.014(10) 0.015(12) C27B 0.104(10) 0.191(15) 0.088(11) 0.029(10) -0.010(7) 0.034(12) C28B 0.122(11) 0.225(16) 0.159(12) 0.083(14) 0.018(11) 0.092(12) C29B 0.131(16) 0.24(2) 0.182(14) 0.099(17) 0.050(14) 0.072(13) C30 0.076(5) 0.079(5) 0.067(4) 0.030(4) 0.024(4) -0.004(4) C31 0.113(7) 0.075(5) 0.061(4) 0.015(4) 0.021(4) -0.005(5) N6 0.070(4) 0.088(4) 0.052(3) 0.023(3) 0.022(3) 0.023(3) O4 0.095(4) 0.109(4) 0.092(4) 0.058(3) 0.033(3) 0.040(3) O5 0.062(3) 0.194(7) 0.098(4) 0.071(4) 0.031(3) 0.047(4) O6 0.099(4) 0.142(5) 0.095(4) 0.068(4) 0.045(3) 0.048(4) N7 0.147(7) 0.132(6) 0.063(4) 0.046(4) -0.017(5) -0.056(6) O8 0.144(6) 0.48(2) 0.150(8) 0.147(10) -0.022(6) -0.052(10) O7 0.179(6) 0.107(4) 0.080(4) 0.056(3) 0.003(4) 0.027(4) O9 0.147(6) 0.197(7) 0.097(5) 0.081(5) 0.024(4) -0.009(5) N8 0.141(7) 0.084(5) 0.114(6) 0.045(5) 0.064(5) 0.055(5) O10 0.189(7) 0.125(5) 0.098(4) 0.064(4) 0.065(4) 0.084(5) O11 0.297(14) 0.311(14) 0.279(13) 0.231(13) 0.147(11) 0.214(12) O12 0.289(14) 0.139(8) 0.294(14) -0.002(9) 0.174(12) 0.061(9) _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 N4 2.031(5) . ? Pd1 N3 2.038(5) . ? Pd1 N5 2.037(5) . ? Pd1 N1 2.041(5) 2 ? O1 C24 1.386(8) . ? O1 C26B 1.442(5) . ? O1 C26A 1.472(11) . ? O3A C29A 1.522(17) . ? O2A C27A 1.521(17) . ? O2A C28A 1.540(17) . ? O3B C29B 1.501(16) . ? O2B C27B 1.504(16) . ? O2B C28B 1.525(16) . ? N1 C9 1.335(7) . ? N1 C8 1.343(8) . ? N1 Pd1 2.041(5) 2 ? N2 C1 1.337(8) . ? N2 C2 1.337(8) . ? N2 C11 1.502(7) . ? N3 C14 1.322(7) . ? N3 C15 1.369(7) . ? N4 C31 1.466(10) . ? N5 C30 1.451(8) . ? C1 C4 1.353(8) . ? C2 C23 1.368(8) . ? C3 C24 1.342(10) . ? C3 C22 1.403(11) . ? C4 C5 1.386(8) . ? C5 C23 1.392(8) . ? C5 C6 1.486(8) . ? C6 C10 1.387(8) . ? C6 C7 1.387(8) . ? C7 C8 1.371(8) . ? C9 C10 1.350(8) . ? C11 C12 1.516(8) . ? C12 C13 1.361(8) . ? C12 C20 1.412(8) . ? C13 C14 1.391(8) . ? C15 C16 1.407(9) . ? C15 C20 1.431(8) . ? C16 C17 1.350(10) . ? C17 C18 1.370(11) . ? C18 C19 1.369(10) . ? C19 C20 1.406(9) . ? C21 C22 1.331(10) 2 ? C21 C25 1.428(9) . ? C22 C21 1.331(10) 2 ? C24 C25 1.409(9) . ? C25 C25 1.402(11) 2 ? C26A C27A 1.538(5) . ? C28A C29A 1.503(18) . ? C26B C27B 1.499(14) . ? C28B C29B 1.497(18) . ? C30 C31 1.499(9) . ? N6 O5 1.217(7) . ? N6 O4 1.233(7) . ? N6 O6 1.256(7) . ? N7 O9 1.143(7) . ? N7 O7 1.211(7) . ? N7 O8 1.281(9) . ? N8 O11 1.105(10) . ? N8 O10 1.151(8) . ? N8 O12 1.265(11) . ? 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 N4 Pd1 N3 93.88(19) . . ? N4 Pd1 N5 83.5(2) . . ? N3 Pd1 N5 174.5(2) . . ? N4 Pd1 N1 175.15(19) . 2 ? N3 Pd1 N1 90.14(18) . 2 ? N5 Pd1 N1 92.7(2) . 2 ? C24 O1 C26B 105.4(8) . . ? C24 O1 C26A 127.3(10) . . ? C26B O1 C26A 27.4(9) . . ? C27A O2A C28A 107(2) . . ? C27B O2B C28B 100.2(18) . . ? C9 N1 C8 116.4(5) . . ? C9 N1 Pd1 120.7(4) . 2 ? C8 N1 Pd1 122.8(4) . 2 ? C1 N2 C2 119.2(5) . . ? C1 N2 C11 119.9(5) . . ? C2 N2 C11 120.9(5) . . ? C14 N3 C15 118.7(5) . . ? C14 N3 Pd1 118.3(4) . . ? C15 N3 Pd1 123.0(4) . . ? C31 N4 Pd1 108.4(4) . . ? C30 N5 Pd1 109.0(4) . . ? N2 C1 C4 122.1(6) . . ? N2 C2 C23 121.3(6) . . ? C24 C3 C22 119.7(7) . . ? C1 C4 C5 120.2(6) . . ? C4 C5 C23 117.0(5) . . ? C4 C5 C6 121.8(5) . . ? C23 C5 C6 121.2(5) . . ? C10 C6 C7 116.2(5) . . ? C10 C6 C5 121.0(5) . . ? C7 C6 C5 122.6(5) . . ? C8 C7 C6 119.8(6) . . ? N1 C8 C7 123.3(6) . . ? N1 C9 C10 123.8(6) . . ? C9 C10 C6 120.6(6) . . ? N2 C11 C12 110.1(4) . . ? C13 C12 C20 118.6(5) . . ? C13 C12 C11 119.0(5) . . ? C20 C12 C11 122.4(5) . . ? C12 C13 C14 120.5(5) . . ? N3 C14 C13 123.0(6) . . ? N3 C15 C16 119.8(6) . . ? N3 C15 C20 121.0(5) . . ? C16 C15 C20 119.1(6) . . ? C17 C16 C15 120.5(7) . . ? C16 C17 C18 120.7(8) . . ? C19 C18 C17 121.8(7) . . ? C18 C19 C20 119.8(7) . . ? C19 C20 C12 123.7(6) . . ? C19 C20 C15 118.2(6) . . ? C12 C20 C15 118.1(5) . . ? C22 C21 C25 119.8(6) 2 . ? C21 C22 C3 121.5(7) 2 . ? C2 C23 C5 120.1(6) . . ? C3 C24 O1 125.6(7) . . ? C3 C24 C25 121.6(7) . . ? O1 C24 C25 112.8(6) . . ? C25 C25 C24 118.2(8) 2 . ? C25 C25 C21 119.2(8) 2 . ? C24 C25 C21 122.6(6) . . ? O1 C26A C27A 100.3(11) . . ? O2A C27A C26A 102.1(17) . . ? C29A C28A O2A 120(3) . . ? C28A C29A O3A 108(2) . . ? O1 C26B C27B 111.4(14) . . ? C26B C27B O2B 98(2) . . ? C29B C28B O2B 102(2) . . ? O3B C29B C28B 122(2) . . ? N5 C30 C31 108.9(5) . . ? N4 C31 C30 107.8(6) . . ? O5 N6 O4 121.3(6) . . ? O5 N6 O6 119.6(7) . . ? O4 N6 O6 118.9(6) . . ? O9 N7 O7 129.3(8) . . ? O9 N7 O8 109.5(9) . . ? O7 N7 O8 116.3(9) . . ? O11 N8 O10 125.9(10) . . ? O11 N8 O12 117.0(11) . . ? O10 N8 O12 116.4(11) . . ? 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 N4 Pd1 N3 C14 -98.6(5) . . . . ? N5 Pd1 N3 C14 -37(2) . . . . ? N1 Pd1 N3 C14 84.1(4) 2 . . . ? N4 Pd1 N3 C15 82.7(5) . . . . ? N5 Pd1 N3 C15 144(2) . . . . ? N1 Pd1 N3 C15 -94.6(5) 2 . . . ? N3 Pd1 N4 C31 158.7(5) . . . . ? N5 Pd1 N4 C31 -16.5(5) . . . . ? N1 Pd1 N4 C31 -55(3) 2 . . . ? N4 Pd1 N5 C30 -11.9(4) . . . . ? N3 Pd1 N5 C30 -74(2) . . . . ? N1 Pd1 N5 C30 165.0(4) 2 . . . ? C2 N2 C1 C4 1.0(9) . . . . ? C11 N2 C1 C4 -177.2(5) . . . . ? C1 N2 C2 C23 -0.8(9) . . . . ? C11 N2 C2 C23 177.5(5) . . . . ? N2 C1 C4 C5 0.1(9) . . . . ? C1 C4 C5 C23 -1.5(9) . . . . ? C1 C4 C5 C6 178.4(5) . . . . ? C4 C5 C6 C10 10.8(8) . . . . ? C23 C5 C6 C10 -169.4(6) . . . . ? C4 C5 C6 C7 -164.2(6) . . . . ? C23 C5 C6 C7 15.6(8) . . . . ? C10 C6 C7 C8 -1.3(9) . . . . ? C5 C6 C7 C8 173.9(6) . . . . ? C9 N1 C8 C7 0.4(9) . . . . ? Pd1 N1 C8 C7 -175.4(5) 2 . . . ? C6 C7 C8 N1 1.1(10) . . . . ? C8 N1 C9 C10 -1.7(10) . . . . ? Pd1 N1 C9 C10 174.2(5) 2 . . . ? N1 C9 C10 C6 1.5(10) . . . . ? C7 C6 C10 C9 0.1(9) . . . . ? C5 C6 C10 C9 -175.2(6) . . . . ? C1 N2 C11 C12 91.6(6) . . . . ? C2 N2 C11 C12 -86.6(6) . . . . ? N2 C11 C12 C13 -88.4(6) . . . . ? N2 C11 C12 C20 88.7(6) . . . . ? C20 C12 C13 C14 -2.6(8) . . . . ? C11 C12 C13 C14 174.6(5) . . . . ? C15 N3 C14 C13 2.4(9) . . . . ? Pd1 N3 C14 C13 -176.4(4) . . . . ? C12 C13 C14 N3 -0.7(9) . . . . ? C14 N3 C15 C16 179.6(6) . . . . ? Pd1 N3 C15 C16 -1.7(8) . . . . ? C14 N3 C15 C20 -0.6(8) . . . . ? Pd1 N3 C15 C20 178.1(4) . . . . ? N3 C15 C16 C17 -179.8(7) . . . . ? C20 C15 C16 C17 0.4(10) . . . . ? C15 C16 C17 C18 0.6(12) . . . . ? C16 C17 C18 C19 -0.9(13) . . . . ? C17 C18 C19 C20 0.0(12) . . . . ? C18 C19 C20 C12 -177.2(6) . . . . ? C18 C19 C20 C15 1.0(9) . . . . ? C13 C12 C20 C19 -177.5(6) . . . . ? C11 C12 C20 C19 5.4(9) . . . . ? C13 C12 C20 C15 4.2(8) . . . . ? C11 C12 C20 C15 -172.9(5) . . . . ? N3 C15 C20 C19 179.0(5) . . . . ? C16 C15 C20 C19 -1.2(8) . . . . ? N3 C15 C20 C12 -2.7(8) . . . . ? C16 C15 C20 C12 177.1(5) . . . . ? C24 C3 C22 C21 -0.9(13) . . . 2 ? N2 C2 C23 C5 -0.6(10) . . . . ? C4 C5 C23 C2 1.7(9) . . . . ? C6 C5 C23 C2 -178.2(5) . . . . ? C22 C3 C24 O1 179.9(7) . . . . ? C22 C3 C24 C25 0.3(12) . . . . ? C26B O1 C24 C3 -0.5(15) . . . . ? C26A O1 C24 C3 -19.2(13) . . . . ? C26B O1 C24 C25 179.1(13) . . . . ? C26A O1 C24 C25 160.4(9) . . . . ? C3 C24 C25 C25 1.1(11) . . . 2 ? O1 C24 C25 C25 -178.5(6) . . . 2 ? C3 C24 C25 C21 179.0(7) . . . . ? O1 C24 C25 C21 -0.6(8) . . . . ? C22 C21 C25 C25 -1.5(10) 2 . . 2 ? C22 C21 C25 C24 -179.4(6) 2 . . . ? C24 O1 C26A C27A 80.4(17) . . . . ? C26B O1 C26A C27A 38(3) . . . . ? C28A O2A C27A C26A -163(2) . . . . ? O1 C26A C27A O2A 90(2) . . . . ? C27A O2A C28A C29A -71(4) . . . . ? O2A C28A C29A O3A 68(4) . . . . ? C24 O1 C26B C27B 162.3(17) . . . . ? C26A O1 C26B C27B -51(2) . . . . ? O1 C26B C27B O2B -68(3) . . . . ? C28B O2B C27B C26B -133(2) . . . . ? C27B O2B C28B C29B 140(3) . . . . ? O2B C28B C29B O3B 0(4) . . . . ? Pd1 N5 C30 C31 37.7(7) . . . . ? Pd1 N4 C31 C30 41.0(7) . . . . ? N5 C30 C31 N4 -52.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.897 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.092