# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email yusy@ruc.edu.cn _publ_contact_author_name 'Dr Shu-Yan Yu' _publ_section_title ; Programmable Self-Assembly of Homo- or Hetero- Metallomacrocycles using 4-(1H-pyrazolyl-4-yl)pyridine ; loop_ _publ_author_name 'Shu-Yan Yu' 'Hui Li' 'Jin Tong' # Attachment '- 1.cif' data_42 _database_code_depnum_ccdc_archive 'CCDC 843501' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H73.20 N24 O0.60 Pd6, 0.4(H4 O2), 8.6(H2 O)' _chemical_formula_sum 'C92 H92 N24 O10 Pd6' _chemical_formula_weight 2332.30 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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6289(6) _cell_length_b 16.3546(8) _cell_length_c 17.1424(6) _cell_angle_alpha 75.0190(10) _cell_angle_beta 86.462(2) _cell_angle_gamma 77.0910(10) _cell_volume 3333.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3175 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.12 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20902 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13113 _reflns_number_gt 9144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0519P)^2^+1.3779P] 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 13113 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 C1 C 0.3342(3) -0.0452(3) 0.0685(2) 0.0473(9) Uani 1 1 d . . . H1 H 0.3702 0.0003 0.0543 0.057 Uiso 1 1 calc R . . C2 C 0.3700(3) -0.1142(3) 0.0345(2) 0.0516(10) Uani 1 1 d . . . H2 H 0.4290 -0.1175 -0.0007 0.062 Uiso 1 1 calc R . . C3 C 0.3090(3) -0.1797(3) 0.0576(2) 0.0502(9) Uani 1 1 d . . . H3 H 0.3268 -0.2281 0.0365 0.060 Uiso 1 1 calc R . . C4 C 0.2219(3) -0.1721(3) 0.1122(3) 0.0550(10) Uani 1 1 d . . . H4 H 0.1823 -0.2153 0.1277 0.066 Uiso 1 1 calc R . . C5 C 0.1969(3) -0.1022(3) 0.1414(3) 0.0519(10) Uani 1 1 d . . . C6 C 0.1141(3) -0.0930(3) 0.2060(2) 0.0543(10) Uani 1 1 d . . . C7 C 0.0534(3) -0.1530(3) 0.2389(2) 0.0498(9) Uani 1 1 d . . . H7 H 0.0555 -0.2001 0.2174 0.060 Uiso 1 1 calc R . . C8 C -0.0124(3) -0.1416(3) 0.3059(2) 0.0536(10) Uani 1 1 d . . . H8 H -0.0527 -0.1823 0.3310 0.064 Uiso 1 1 calc R . . C9 C -0.0166(4) -0.0682(3) 0.3347(3) 0.0582(11) Uani 1 1 d . . . H9 H -0.0583 -0.0600 0.3798 0.070 Uiso 1 1 calc R . . C10 C 0.0402(3) -0.0107(3) 0.2963(2) 0.0475(9) Uani 1 1 d . . . H10 H 0.0343 0.0393 0.3140 0.057 Uiso 1 1 calc R . . C11 C 0.2631(3) 0.1434(3) 0.4331(2) 0.0468(9) Uani 1 1 d . . . H11 H 0.1931 0.1531 0.4136 0.056 Uiso 1 1 calc R . . C12 C 0.2832(3) 0.1301(3) 0.5184(2) 0.0514(10) Uani 1 1 d . . . H12 H 0.2240 0.1367 0.5530 0.062 Uiso 1 1 calc R . . C13 C 0.3820(4) 0.1090(3) 0.5489(3) 0.0516(10) Uani 1 1 d . . . H13 H 0.3924 0.0961 0.6044 0.062 Uiso 1 1 calc R . . C14 C 0.4660(3) 0.1066(2) 0.4984(2) 0.0459(9) Uani 1 1 d . . . H14 H 0.5361 0.0944 0.5184 0.055 Uiso 1 1 calc R . . C15 C 0.4496(3) 0.1228(2) 0.4133(2) 0.0438(8) Uani 1 1 d . . . C16 C 0.5376(3) 0.1216(2) 0.3540(2) 0.0465(9) Uani 1 1 d . . . C17 C 0.6453(4) 0.1086(3) 0.3740(3) 0.0562(10) Uani 1 1 d . . . H17 H 0.6659 0.1064 0.4258 0.067 Uiso 1 1 calc R . . C18 C 0.7221(3) 0.0990(3) 0.3127(2) 0.0500(9) Uani 1 1 d . . . H18 H 0.7960 0.0875 0.3233 0.060 Uiso 1 1 calc R . . C19 C 0.6874(3) 0.1065(3) 0.2404(3) 0.0509(10) Uani 1 1 d . . . H19 H 0.7380 0.1049 0.1987 0.061 Uiso 1 1 calc R . . C20 C 0.5794(3) 0.1166(2) 0.2229(2) 0.0477(9) Uani 1 1 d . . . H20 H 0.5584 0.1166 0.1719 0.057 Uiso 1 1 calc R . . C21 C -0.3976(3) 0.3453(2) 0.4502(2) 0.0460(9) Uani 1 1 d . . . H21 H -0.3281 0.3318 0.4291 0.055 Uiso 1 1 calc R . . C22 C -0.4300(3) 0.2846(3) 0.5166(2) 0.0459(9) Uani 1 1 d . . . H22 H -0.3835 0.2316 0.5377 0.055 Uiso 1 1 calc R . . C23 C -0.5275(3) 0.3044(3) 0.5485(2) 0.0526(10) Uani 1 1 d . . . H23 H -0.5491 0.2671 0.5943 0.063 Uiso 1 1 calc R . . C24 C -0.6000(3) 0.3853(3) 0.5106(2) 0.0490(9) Uani 1 1 d . . . H24 H -0.6711 0.3986 0.5290 0.059 Uiso 1 1 calc R . . C25 C -0.5625(3) 0.4413(3) 0.4477(3) 0.0497(9) Uani 1 1 d . . . C26 C -0.6252(3) 0.5270(2) 0.4055(2) 0.0434(8) Uani 1 1 d . . . C27 C -0.7346(3) 0.5591(3) 0.4297(2) 0.0501(9) Uani 1 1 d . . . H27 H -0.7705 0.5253 0.4701 0.060 Uiso 1 1 calc R . . C28 C -0.7812(3) 0.6389(3) 0.3915(2) 0.0473(9) Uani 1 1 d . . . H28 H -0.8535 0.6608 0.4024 0.057 Uiso 1 1 calc R . . C29 C -0.7238(3) 0.6913(3) 0.3348(2) 0.0466(9) Uani 1 1 d . . . H29 H -0.7530 0.7501 0.3147 0.056 Uiso 1 1 calc R . . C30 C -0.6234(3) 0.6541(3) 0.3094(2) 0.0513(10) Uani 1 1 d . . . H30 H -0.5898 0.6860 0.2661 0.062 Uiso 1 1 calc R . . C31 C 0.0210(3) 0.1971(3) 0.2161(3) 0.0512(9) Uani 1 1 d . . . H31 H -0.0343 0.1804 0.1948 0.061 Uiso 1 1 calc R . . C32 C 0.0080(3) 0.2672(3) 0.2512(2) 0.0459(9) Uani 1 1 d . . . C33 C 0.1145(3) 0.2654(3) 0.2777(2) 0.0478(9) Uani 1 1 d . . . H33 H 0.1327 0.3028 0.3048 0.057 Uiso 1 1 calc R . . C34 C -0.2853(3) 0.3687(3) 0.2581(3) 0.0513(10) Uani 1 1 d . . . H34 H -0.3511 0.3593 0.2448 0.062 Uiso 1 1 calc R . . C35 C -0.1926(3) 0.3168(2) 0.2418(2) 0.0482(9) Uani 1 1 d . . . H35 H -0.1949 0.2738 0.2159 0.058 Uiso 1 1 calc R . . C36 C -0.0909(3) 0.3279(2) 0.2640(2) 0.0453(8) Uani 1 1 d . . . C37 C -0.0930(3) 0.3958(3) 0.2995(3) 0.0509(9) Uani 1 1 d . . . H37 H -0.0280 0.4063 0.3132 0.061 Uiso 1 1 calc R . . C38 C -0.1909(3) 0.4482(3) 0.3146(2) 0.0483(9) Uani 1 1 d . . . H38 H -0.1904 0.4925 0.3393 0.058 Uiso 1 1 calc R . . C39 C 0.2891(3) 0.1743(3) 0.0274(2) 0.0499(9) Uani 1 1 d . . . H39 H 0.2544 0.1589 -0.0112 0.060 Uiso 1 1 calc R . . C40 C 0.3536(3) 0.2364(2) 0.0111(2) 0.0442(8) Uani 1 1 d . . . C41 C 0.3859(3) 0.2380(2) 0.0871(2) 0.0458(9) Uani 1 1 d . . . H41 H 0.4293 0.2735 0.0965 0.055 Uiso 1 1 calc R . . C42 C 0.3539(3) 0.3424(2) -0.2100(2) 0.0452(9) Uani 1 1 d . . . H42 H 0.3275 0.3358 -0.2570 0.054 Uiso 1 1 calc R . . C43 C 0.3333(3) 0.2867(3) -0.1372(3) 0.0532(10) Uani 1 1 d . . . H43 H 0.2902 0.2471 -0.1359 0.064 Uiso 1 1 calc R . . C44 C 0.3773(3) 0.2906(3) -0.0669(2) 0.0482(9) Uani 1 1 d . . . C45 C 0.4357(3) 0.3513(3) -0.0742(2) 0.0482(9) Uani 1 1 d . . . H45 H 0.4653 0.3563 -0.0277 0.058 Uiso 1 1 calc R . . C46 C 0.4546(3) 0.4074(3) -0.1476(2) 0.0511(9) Uani 1 1 d . . . H46 H 0.4983 0.4467 -0.1495 0.061 Uiso 1 1 calc R . . N1 N 0.2530(3) -0.0393(2) 0.1195(2) 0.0533(8) Uani 1 1 d . . . N2 N 0.1052(3) -0.0206(2) 0.2337(2) 0.0523(8) Uani 1 1 d . . . N3 N 0.3505(2) 0.1412(2) 0.38302(18) 0.0416(7) Uani 1 1 d . . . N4 N 0.5075(3) 0.1263(2) 0.27929(19) 0.0449(7) Uani 1 1 d . . . N5 N -0.4613(3) 0.4201(2) 0.41673(19) 0.0470(7) Uani 1 1 d . . . N6 N -0.5732(3) 0.5737(2) 0.34515(18) 0.0423(7) Uani 1 1 d . . . N7 N 0.1262(3) 0.1583(2) 0.2185(2) 0.0543(8) Uani 1 1 d . . . N8 N 0.1838(3) 0.1979(2) 0.25533(19) 0.0477(7) Uani 1 1 d . . . N9 N -0.2862(3) 0.4362(2) 0.2943(2) 0.0487(8) Uani 1 1 d . . . N10 N 0.2852(3) 0.1408(2) 0.10697(19) 0.0451(7) Uani 1 1 d . . . N11 N 0.3446(3) 0.1806(2) 0.1442(2) 0.0511(8) Uani 1 1 d . . . N12 N 0.4086(3) 0.4044(2) -0.21687(19) 0.0474(7) Uani 1 1 d . . . O1W O 0.9662(5) 1.0066(4) 0.0446(4) 0.0450(14) Uani 0.40 1 d P . . H1X H 1.0059 0.9604 0.0723 0.054 Uiso 0.40 1 d PR . . H1Y H 0.9876 1.0157 -0.0043 0.054 Uiso 0.40 1 d PR . . O2W O 0.8364(8) 0.2589(6) 0.0596(6) 0.058(2) Uani 0.30 1 d P . . H2X H 0.8871 0.2858 0.0585 0.069 Uiso 0.30 1 d PR . . H2Y H 0.7942 0.2847 0.0198 0.069 Uiso 0.30 1 d PR . . O3W O 0.1437(8) 0.4059(7) 0.0712(6) 0.058(2) Uani 0.30 1 d P . . H3X H 0.1245 0.4583 0.0741 0.069 Uiso 0.30 1 d PR . . H3Y H 0.1180 0.4007 0.0285 0.069 Uiso 0.30 1 d PR . . O4W O 0.3976(6) 0.3791(5) 0.2859(4) 0.0624(19) Uani 0.40 1 d P . . H4X H 0.4580 0.3516 0.2718 0.075 Uiso 0.40 1 d PR . . H4Y H 0.3679 0.3446 0.3216 0.075 Uiso 0.40 1 d PR . . O5W O 0.1951(8) 0.3218(6) 0.6410(6) 0.055(2) Uani 0.30 1 d P . . H5X H 0.2497 0.3041 0.6135 0.066 Uiso 0.30 1 d PR . . H5Y H 0.1922 0.2836 0.6850 0.066 Uiso 0.30 1 d PR . . O6W O 0.0887(7) 0.3377(6) 0.5023(5) 0.047(2) Uani 0.30 1 d P . . H6X H 0.0214 0.3568 0.5089 0.057 Uiso 0.30 1 d PR . . H6Y H 0.1126 0.3729 0.4633 0.057 Uiso 0.30 1 d PR . . O7W O 0.2623(6) 0.6066(5) 0.1462(5) 0.0607(19) Uani 0.40 1 d P . . H7X H 0.2639 0.5823 0.1964 0.073 Uiso 0.40 1 d PR . . H7Y H 0.3095 0.6378 0.1350 0.073 Uiso 0.40 1 d PR . . O8W O 0.9676(8) 0.7119(7) 0.1228(7) 0.068(3) Uani 0.30 1 d P . . H8X H 0.9347 0.6727 0.1200 0.081 Uiso 0.30 1 d PR . . H8Y H 0.9821 0.7391 0.0754 0.081 Uiso 0.30 1 d PR . . O9W O 1.0014(9) 0.3852(7) 0.7452(6) 0.062(3) Uani 0.30 1 d P . . H9X H 1.0338 0.4103 0.7710 0.074 Uiso 0.30 1 d PR . . H9Y H 0.9371 0.3860 0.7635 0.074 Uiso 0.30 1 d PR . . O10W O 0.1640(6) 0.4845(5) 0.9320(4) 0.061(2) Uani 0.40 1 d P . . H10X H 0.2302 0.4767 0.9172 0.073 Uiso 0.40 1 d PR . . H10Y H 0.1287 0.4631 0.9047 0.073 Uiso 0.40 1 d PR . . O11W O 0.4610(9) 0.5977(7) 0.9237(6) 0.063(3) Uani 0.30 1 d P . . H11X H 0.4557 0.5709 0.8882 0.075 Uiso 0.30 1 d PR . . H11Y H 0.4369 0.6517 0.9046 0.075 Uiso 0.30 1 d PR . . O12W O 0.8105(9) 0.9058(7) 0.1211(6) 0.063(3) Uani 0.30 1 d P . . H12X H 0.7895 0.8874 0.1692 0.075 Uiso 0.30 1 d PR . . H12Y H 0.8347 0.9512 0.1174 0.075 Uiso 0.30 1 d PR . . O13W O 0.9189(7) 0.1159(6) 0.4224(5) 0.052(2) Uani 0.30 1 d P . . H13X H 0.8882 0.1593 0.4402 0.062 Uiso 0.30 1 d PR . . H13Y H 0.9724 0.1280 0.3926 0.062 Uiso 0.30 1 d PR . . H14X H 0.2834 -0.0519 0.2655 0.062 Uiso 0.30 1 d PR . . H14Y H 0.2266 -0.0800 0.3356 0.062 Uiso 0.30 1 d PR . . O14W O 0.2893(8) -0.0766(7) 0.3156(5) 0.064(3) Uani 0.30 1 d P . . O15W O 0.4351(6) 0.8849(5) 0.2747(4) 0.0545(17) Uani 0.40 1 d P . . H15X H 0.4573 0.9285 0.2457 0.065 Uiso 0.40 1 d PR . . H15Y H 0.4323 0.8499 0.2463 0.065 Uiso 0.40 1 d PR . . Pd1 Pd 0.19594(3) 0.06088(2) 0.170560(19) 0.05016(9) Uani 1 1 d . . . Pd2 Pd 0.34394(3) 0.16041(2) 0.263884(19) 0.04838(9) Uani 1 1 d . . . Pd3 Pd -0.42908(3) 0.50785(2) 0.317665(18) 0.04775(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 0.049(2) 0.046(2) 0.046(2) -0.0026(17) -0.0092(17) -0.0148(17) C2 0.047(2) 0.054(2) 0.046(2) -0.0137(18) -0.0144(17) 0.0107(18) C3 0.055(2) 0.048(2) 0.050(2) -0.0234(18) -0.0093(18) 0.0019(18) C4 0.048(2) 0.055(2) 0.066(3) -0.014(2) 0.0060(19) -0.0208(19) C5 0.050(2) 0.043(2) 0.057(2) -0.0118(18) -0.0217(19) 0.0053(18) C6 0.049(2) 0.062(3) 0.047(2) -0.0075(19) -0.0115(18) -0.006(2) C7 0.044(2) 0.050(2) 0.050(2) -0.0118(18) -0.0152(17) 0.0031(17) C8 0.044(2) 0.057(2) 0.049(2) 0.0131(19) -0.0068(17) -0.0169(18) C9 0.061(3) 0.051(2) 0.053(2) -0.001(2) 0.005(2) -0.009(2) C10 0.053(2) 0.046(2) 0.0404(19) -0.0138(17) -0.0108(17) 0.0018(17) C11 0.044(2) 0.048(2) 0.050(2) -0.0146(17) 0.0101(17) -0.0136(17) C12 0.046(2) 0.055(2) 0.051(2) -0.0132(19) 0.0160(18) -0.0131(18) C13 0.065(3) 0.051(2) 0.046(2) -0.0207(18) 0.0063(19) -0.019(2) C14 0.044(2) 0.044(2) 0.047(2) -0.0083(17) -0.0005(17) -0.0080(16) C15 0.049(2) 0.043(2) 0.0415(19) -0.0049(16) -0.0033(16) -0.0190(17) C16 0.049(2) 0.043(2) 0.045(2) -0.0088(16) -0.0012(17) -0.0071(17) C17 0.053(2) 0.059(3) 0.056(2) -0.020(2) 0.0069(19) -0.006(2) C18 0.047(2) 0.051(2) 0.053(2) -0.0123(18) 0.0106(18) -0.0146(18) C19 0.051(2) 0.048(2) 0.052(2) -0.0134(18) 0.0192(19) -0.0128(18) C20 0.056(2) 0.046(2) 0.045(2) -0.0181(17) 0.0074(18) -0.0144(18) C21 0.047(2) 0.044(2) 0.049(2) -0.0167(17) -0.0076(17) -0.0058(17) C22 0.053(2) 0.049(2) 0.042(2) -0.0102(17) -0.0126(17) -0.0221(18) C23 0.049(2) 0.049(2) 0.049(2) 0.0132(18) -0.0090(18) -0.0153(18) C24 0.052(2) 0.046(2) 0.047(2) -0.0118(17) -0.0030(18) -0.0051(18) C25 0.047(2) 0.046(2) 0.059(2) -0.0163(19) 0.0042(18) -0.0135(17) C26 0.046(2) 0.0387(19) 0.046(2) -0.0120(16) -0.0007(16) -0.0077(16) C27 0.049(2) 0.051(2) 0.044(2) 0.0067(17) -0.0081(17) -0.0157(18) C28 0.042(2) 0.050(2) 0.050(2) -0.0169(18) -0.0053(17) -0.0044(17) C29 0.044(2) 0.044(2) 0.049(2) -0.0145(17) -0.0109(17) 0.0021(16) C30 0.040(2) 0.054(2) 0.049(2) 0.0083(18) -0.0143(17) -0.0080(17) C31 0.037(2) 0.054(2) 0.063(3) -0.014(2) 0.0054(18) -0.0151(17) C32 0.050(2) 0.046(2) 0.043(2) -0.0090(16) 0.0081(17) -0.0176(17) C33 0.052(2) 0.046(2) 0.047(2) -0.0126(17) 0.0060(17) -0.0155(18) C34 0.039(2) 0.056(2) 0.065(3) -0.018(2) 0.0061(18) -0.0219(18) C35 0.051(2) 0.0395(19) 0.053(2) -0.0143(17) 0.0049(18) -0.0061(17) C36 0.0398(19) 0.046(2) 0.049(2) -0.0149(17) -0.0038(16) -0.0016(16) C37 0.037(2) 0.058(2) 0.063(2) -0.017(2) -0.0006(17) -0.0196(18) C38 0.051(2) 0.044(2) 0.050(2) -0.0109(17) 0.0009(18) -0.0096(17) C39 0.052(2) 0.053(2) 0.047(2) -0.0170(18) -0.0123(18) -0.0077(18) C40 0.052(2) 0.046(2) 0.0381(19) -0.0170(16) 0.0109(16) -0.0136(17) C41 0.043(2) 0.044(2) 0.053(2) -0.0151(17) 0.0093(17) -0.0147(16) C42 0.051(2) 0.048(2) 0.0358(18) -0.0147(16) -0.0100(16) -0.0011(17) C43 0.042(2) 0.061(3) 0.061(3) -0.014(2) 0.0041(18) -0.0236(19) C44 0.045(2) 0.045(2) 0.046(2) 0.0075(17) -0.0103(16) -0.0107(17) C45 0.053(2) 0.049(2) 0.041(2) -0.0118(17) -0.0107(17) -0.0026(18) C46 0.042(2) 0.061(3) 0.056(2) -0.017(2) 0.0026(18) -0.0223(19) N1 0.0479(19) 0.052(2) 0.0490(19) -0.0102(15) -0.0025(15) 0.0091(16) N2 0.058(2) 0.0471(19) 0.0455(18) -0.0028(15) -0.0009(15) -0.0079(16) N3 0.0410(16) 0.0426(16) 0.0467(17) -0.0154(14) 0.0023(13) -0.0158(13) N4 0.0438(17) 0.0423(17) 0.0477(18) -0.0100(14) 0.0054(14) -0.0103(13) N5 0.0459(18) 0.0537(19) 0.0430(17) -0.0115(15) -0.0050(14) -0.0132(15) N6 0.0495(18) 0.0475(17) 0.0374(15) -0.0172(14) -0.0074(13) -0.0165(14) N7 0.054(2) 0.058(2) 0.0509(19) -0.0140(16) 0.0049(16) -0.0125(17) N8 0.0455(18) 0.0522(19) 0.0460(17) -0.0160(15) 0.0068(14) -0.0098(15) N9 0.0459(18) 0.0542(19) 0.0484(18) -0.0181(15) 0.0066(14) -0.0112(15) N10 0.0464(18) 0.0409(17) 0.0492(18) -0.0144(14) 0.0031(14) -0.0092(14) N11 0.054(2) 0.0487(19) 0.0535(19) -0.0178(16) 0.0048(16) -0.0122(15) N12 0.0471(18) 0.0482(18) 0.0412(17) -0.0025(14) -0.0038(14) -0.0077(15) O1W 0.047(4) 0.047(4) 0.046(4) -0.019(3) 0.006(3) -0.013(3) O2W 0.059(6) 0.064(6) 0.047(5) -0.008(5) -0.001(4) -0.012(5) O3W 0.052(6) 0.069(6) 0.051(5) -0.020(5) -0.008(4) -0.003(5) O4W 0.055(4) 0.075(5) 0.053(4) -0.012(4) 0.003(3) -0.013(4) O5W 0.057(6) 0.063(6) 0.054(5) -0.023(5) -0.015(4) -0.016(5) O6W 0.044(5) 0.059(5) 0.048(5) -0.022(4) 0.016(4) -0.022(4) O7W 0.058(4) 0.058(4) 0.064(5) -0.014(4) 0.013(4) -0.014(4) O8W 0.057(6) 0.062(6) 0.091(8) -0.029(6) 0.008(6) -0.015(5) O9W 0.058(6) 0.061(6) 0.064(6) -0.014(5) 0.004(5) -0.008(5) O10W 0.041(4) 0.059(4) 0.065(5) 0.015(4) -0.014(3) -0.008(3) O11W 0.068(7) 0.079(7) 0.048(5) -0.021(5) 0.008(5) -0.026(5) O12W 0.068(7) 0.070(7) 0.052(6) -0.009(5) -0.012(5) -0.020(5) O13W 0.046(5) 0.050(5) 0.054(5) -0.005(4) 0.008(4) -0.014(4) O14W 0.058(6) 0.083(7) 0.042(5) 0.021(5) -0.014(4) -0.034(5) O15W 0.050(4) 0.053(4) 0.056(4) -0.014(3) 0.006(3) -0.004(3) Pd1 0.04923(18) 0.04997(18) 0.04854(17) -0.01211(14) 0.00553(13) -0.00689(14) Pd2 0.04822(18) 0.04762(17) 0.04922(17) -0.01264(13) 0.00558(13) -0.01118(13) Pd3 0.04591(17) 0.04844(17) 0.04362(16) -0.00389(13) -0.00328(13) -0.00744(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 C1 N1 1.309(5) . ? C1 C2 1.378(6) . ? C1 H1 0.9300 . ? C2 C3 1.417(6) . ? C2 H2 0.9300 . ? C3 C4 1.405(6) . ? C3 H3 0.9300 . ? C4 C5 1.331(6) . ? C4 H4 0.9300 . ? C5 N1 1.339(6) . ? C5 C6 1.489(6) . ? C6 C7 1.366(6) . ? C6 N2 1.366(6) . ? C7 C8 1.403(6) . ? C7 H7 0.9300 . ? C8 C9 1.400(6) . ? C8 H8 0.9300 . ? C9 C10 1.324(6) . ? C9 H9 0.9300 . ? C10 N2 1.332(5) . ? C10 H10 0.9300 . ? C11 N3 1.356(5) . ? C11 C12 1.451(6) . ? C11 H11 0.9300 . ? C12 C13 1.321(6) . ? C12 H12 0.9300 . ? C13 C14 1.327(6) . ? C13 H13 0.9300 . ? C14 C15 1.434(5) . ? C14 H14 0.9300 . ? C15 N3 1.325(5) . ? C15 C16 1.460(5) . ? C16 N4 1.336(5) . ? C16 C17 1.380(6) . ? C17 C18 1.400(6) . ? C17 H17 0.9300 . ? C18 C19 1.307(6) . ? C18 H18 0.9300 . ? C19 C20 1.379(6) . ? C19 H19 0.9300 . ? C20 N4 1.300(5) . ? C20 H20 0.9300 . ? C21 N5 1.313(5) . ? C21 C22 1.410(5) . ? C21 H21 0.9300 . ? C22 C23 1.323(6) . ? C22 H22 0.9300 . ? C23 C24 1.448(5) . ? C23 H23 0.9300 . ? C24 C25 1.359(6) . ? C24 H24 0.9300 . ? C25 N5 1.360(5) . ? C25 C26 1.471(5) . ? C26 N6 1.348(5) . ? C26 C27 1.440(5) . ? C27 C28 1.320(5) . ? C27 H27 0.9300 . ? C28 C29 1.402(6) . ? C28 H28 0.9300 . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 N6 1.328(5) . ? C30 H30 0.9300 . ? C31 N7 1.336(5) . ? C31 C32 1.401(6) . ? C31 H31 0.9300 . ? C32 C33 1.437(6) . ? C32 C36 1.456(5) . ? C33 N8 1.370(5) . ? C33 H33 0.9300 . ? C34 C35 1.344(5) . ? C34 N9 1.398(5) . ? C34 H34 0.9300 . ? C35 C36 1.424(6) . ? C35 H35 0.9300 . ? C36 C37 1.393(6) . ? C37 C38 1.390(6) . ? C37 H37 0.9300 . ? C38 N9 1.341(5) . ? C38 H38 0.9300 . ? C39 N10 1.334(5) . ? C39 C40 1.403(6) . ? C39 H39 0.9300 . ? C40 C41 1.397(5) . ? C40 C44 1.455(5) . ? C41 N11 1.339(5) . ? C41 H41 0.9300 . ? C42 N12 1.327(5) . ? C42 C43 1.391(6) . ? C42 H42 0.9300 . ? C43 C44 1.379(6) . ? C43 H43 0.9300 . ? C44 C45 1.341(6) . ? C45 C46 1.394(6) . ? C45 H45 0.9300 . ? C46 N12 1.371(5) . ? C46 H46 0.9300 . ? N1 Pd1 2.026(3) . ? N2 Pd1 2.010(3) . ? N3 Pd2 1.988(3) . ? N4 Pd2 2.031(3) . ? N5 Pd3 2.006(3) . ? N6 Pd3 1.994(3) . ? N7 N8 1.352(5) . ? N7 Pd1 1.987(4) . ? N8 Pd2 1.980(3) . ? N9 Pd3 2.000(3) . ? N10 N11 1.372(5) . ? N10 Pd1 1.985(3) . ? N11 Pd2 1.992(3) . ? N12 Pd3 1.985(3) 2_565 ? O1W O1W 1.742(12) 2_775 ? O1W H1X 0.8500 . ? O1W H1Y 0.8499 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8500 . ? O3W H3X 0.8501 . ? O3W H3Y 0.8500 . ? O4W H4X 0.8500 . ? O4W H4Y 0.8500 . ? O5W H5X 0.8500 . ? O5W H5Y 0.8500 . ? O6W H6X 0.8500 . ? O6W H6Y 0.8499 . ? O7W H7X 0.8501 . ? O7W H7Y 0.8499 . ? O8W H8X 0.8501 . ? O8W H8Y 0.8500 . ? O9W H9X 0.8499 . ? O9W H9Y 0.8500 . ? O10W H10X 0.8500 . ? O10W H10Y 0.8500 . ? O11W H11X 0.8500 . ? O11W H11Y 0.8500 . ? O12W H12X 0.8500 . ? O12W H12Y 0.8500 . ? O13W H13X 0.8500 . ? O13W H13Y 0.8500 . ? O14W H14X 0.8499 . ? O14W H14Y 0.8501 . ? O15W H15X 0.8500 . ? O15W H15Y 0.8499 . ? Pd3 N12 1.985(3) 2_565 ? 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 124.6(4) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 114.2(4) . . ? C1 C2 H2 122.9 . . ? C3 C2 H2 122.9 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 N1 121.2(4) . . ? C4 C5 C6 122.7(4) . . ? N1 C5 C6 115.7(4) . . ? C7 C6 N2 121.0(4) . . ? C7 C6 C5 123.9(4) . . ? N2 C6 C5 115.0(4) . . ? C6 C7 C8 118.1(4) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 118.5(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 N2 123.6(4) . . ? C9 C10 H10 118.2 . . ? N2 C10 H10 118.2 . . ? N3 C11 C12 117.3(4) . . ? N3 C11 H11 121.3 . . ? C12 C11 H11 121.3 . . ? C13 C12 C11 122.7(4) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 118.3(4) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N3 C15 C14 121.0(3) . . ? N3 C15 C16 115.1(3) . . ? C14 C15 C16 123.8(3) . . ? N4 C16 C17 121.7(4) . . ? N4 C16 C15 114.9(3) . . ? C17 C16 C15 123.1(4) . . ? C16 C17 C18 116.9(4) . . ? C16 C17 H17 121.5 . . ? C18 C17 H17 121.5 . . ? C19 C18 C17 118.5(4) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 123.1(4) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? N4 C20 C19 118.6(4) . . ? N4 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N5 C21 C22 122.9(4) . . ? N5 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 118.9(4) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 118.8(4) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 118.9(4) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 N5 121.1(4) . . ? C24 C25 C26 124.9(4) . . ? N5 C25 C26 114.0(3) . . ? N6 C26 C27 122.7(3) . . ? N6 C26 C25 116.1(3) . . ? C27 C26 C25 121.2(3) . . ? C28 C27 C26 116.4(4) . . ? C28 C27 H27 121.8 . . ? C26 C27 H27 121.8 . . ? C27 C28 C29 121.3(4) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 118.7(4) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? N6 C30 C29 121.8(4) . . ? N6 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? N7 C31 C32 108.5(4) . . ? N7 C31 H31 125.7 . . ? C32 C31 H31 125.7 . . ? C31 C32 C33 105.6(4) . . ? C31 C32 C36 129.2(4) . . ? C33 C32 C36 125.2(4) . . ? N8 C33 C32 106.7(3) . . ? N8 C33 H33 126.7 . . ? C32 C33 H33 126.7 . . ? C35 C34 N9 122.3(4) . . ? C35 C34 H34 118.9 . . ? N9 C34 H34 118.9 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 117.1(3) . . ? C37 C36 C32 123.6(4) . . ? C35 C36 C32 119.2(3) . . ? C38 C37 C36 120.8(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? N9 C38 C37 121.4(4) . . ? N9 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? N10 C39 C40 109.4(3) . . ? N10 C39 H39 125.3 . . ? C40 C39 H39 125.3 . . ? C41 C40 C39 104.5(3) . . ? C41 C40 C44 127.4(4) . . ? C39 C40 C44 128.1(4) . . ? N11 C41 C40 109.5(3) . . ? N11 C41 H41 125.3 . . ? C40 C41 H41 125.3 . . ? N12 C42 C43 124.3(3) . . ? N12 C42 H42 117.8 . . ? C43 C42 H42 117.8 . . ? C44 C43 C42 119.5(4) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 116.1(4) . . ? C45 C44 C40 122.4(4) . . ? C43 C44 C40 121.4(4) . . ? C44 C45 C46 123.7(4) . . ? C44 C45 H45 118.1 . . ? C46 C45 H45 118.1 . . ? N12 C46 C45 119.8(4) . . ? N12 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C1 N1 C5 120.5(4) . . ? C1 N1 Pd1 126.3(3) . . ? C5 N1 Pd1 113.2(3) . . ? C10 N2 C6 119.2(4) . . ? C10 N2 Pd1 127.6(3) . . ? C6 N2 Pd1 113.2(3) . . ? C15 N3 C11 119.8(3) . . ? C15 N3 Pd2 115.3(2) . . ? C11 N3 Pd2 124.9(3) . . ? C20 N4 C16 120.9(4) . . ? C20 N4 Pd2 125.8(3) . . ? C16 N4 Pd2 113.1(3) . . ? C21 N5 C25 119.2(3) . . ? C21 N5 Pd3 126.7(3) . . ? C25 N5 Pd3 114.0(3) . . ? C30 N6 C26 118.3(3) . . ? C30 N6 Pd3 128.1(3) . . ? C26 N6 Pd3 113.5(2) . . ? C31 N7 N8 110.3(3) . . ? C31 N7 Pd1 127.2(3) . . ? N8 N7 Pd1 122.5(3) . . ? N7 N8 C33 108.9(3) . . ? N7 N8 Pd2 120.8(3) . . ? C33 N8 Pd2 130.2(3) . . ? C38 N9 C34 118.4(3) . . ? C38 N9 Pd3 122.7(3) . . ? C34 N9 Pd3 118.8(3) . . ? C39 N10 N11 108.4(3) . . ? C39 N10 Pd1 129.9(3) . . ? N11 N10 Pd1 121.2(2) . . ? C41 N11 N10 108.3(3) . . ? C41 N11 Pd2 130.0(3) . . ? N10 N11 Pd2 121.2(2) . . ? C42 N12 C46 116.3(3) . . ? C42 N12 Pd3 125.9(3) . 2_565 ? C46 N12 Pd3 117.8(3) . 2_565 ? O1W O1W H1X 92.1 2_775 . ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 109.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 109.5 . . ? H5X O5W H5Y 109.5 . . ? H6X O6W H6Y 109.5 . . ? H7X O7W H7Y 109.5 . . ? H8X O8W H8Y 109.5 . . ? H9X O9W H9Y 109.5 . . ? H10X O10W H10Y 109.5 . . ? H11X O11W H11Y 109.5 . . ? H12X O12W H12Y 109.5 . . ? H13X O13W H13Y 109.5 . . ? H14X O14W H14Y 109.5 . . ? H15X O15W H15Y 109.5 . . ? N10 Pd1 N7 85.88(13) . . ? N10 Pd1 N2 179.26(14) . . ? N7 Pd1 N2 94.65(14) . . ? N10 Pd1 N1 97.47(14) . . ? N7 Pd1 N1 174.68(15) . . ? N2 Pd1 N1 81.97(15) . . ? N8 Pd2 N3 96.23(13) . . ? N8 Pd2 N11 86.26(14) . . ? N3 Pd2 N11 177.25(13) . . ? N8 Pd2 N4 175.81(13) . . ? N3 Pd2 N4 80.35(13) . . ? N11 Pd2 N4 97.11(14) . . ? N12 Pd3 N6 95.29(13) 2_565 . ? N12 Pd3 N9 87.64(13) 2_565 . ? N6 Pd3 N9 176.96(13) . . ? N12 Pd3 N5 175.65(13) 2_565 . ? N6 Pd3 N5 81.74(13) . . ? N9 Pd3 N5 95.29(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 N1 C1 C2 C3 1.6(6) . . . . ? C1 C2 C3 C4 -1.3(5) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C3 C4 C5 N1 0.2(6) . . . . ? C3 C4 C5 C6 -173.2(4) . . . . ? C4 C5 C6 C7 -2.7(6) . . . . ? N1 C5 C6 C7 -176.4(4) . . . . ? C4 C5 C6 N2 174.6(4) . . . . ? N1 C5 C6 N2 0.9(5) . . . . ? N2 C6 C7 C8 -4.8(6) . . . . ? C5 C6 C7 C8 172.4(4) . . . . ? C6 C7 C8 C9 2.4(6) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C8 C9 C10 N2 -3.1(7) . . . . ? N3 C11 C12 C13 -5.9(6) . . . . ? C11 C12 C13 C14 5.5(6) . . . . ? C12 C13 C14 C15 -2.8(6) . . . . ? C13 C14 C15 N3 0.6(6) . . . . ? C13 C14 C15 C16 179.9(4) . . . . ? N3 C15 C16 N4 -9.5(5) . . . . ? C14 C15 C16 N4 171.2(3) . . . . ? N3 C15 C16 C17 176.1(4) . . . . ? C14 C15 C16 C17 -3.1(6) . . . . ? N4 C16 C17 C18 -1.2(6) . . . . ? C15 C16 C17 C18 172.8(4) . . . . ? C16 C17 C18 C19 2.9(6) . . . . ? C17 C18 C19 C20 -5.3(6) . . . . ? C18 C19 C20 N4 5.8(6) . . . . ? N5 C21 C22 C23 -1.9(6) . . . . ? C21 C22 C23 C24 4.0(6) . . . . ? C22 C23 C24 C25 -5.3(6) . . . . ? C23 C24 C25 N5 4.5(6) . . . . ? C23 C24 C25 C26 -177.5(4) . . . . ? C24 C25 C26 N6 179.1(4) . . . . ? N5 C25 C26 N6 -2.8(5) . . . . ? C24 C25 C26 C27 1.0(6) . . . . ? N5 C25 C26 C27 179.1(3) . . . . ? N6 C26 C27 C28 -2.3(6) . . . . ? C25 C26 C27 C28 175.6(4) . . . . ? C26 C27 C28 C29 -4.7(6) . . . . ? C27 C28 C29 C30 10.6(6) . . . . ? C28 C29 C30 N6 -9.8(6) . . . . ? N7 C31 C32 C33 -2.0(4) . . . . ? N7 C31 C32 C36 -178.7(4) . . . . ? C31 C32 C33 N8 1.9(4) . . . . ? C36 C32 C33 N8 178.7(4) . . . . ? N9 C34 C35 C36 2.2(6) . . . . ? C34 C35 C36 C37 -2.6(6) . . . . ? C34 C35 C36 C32 175.6(4) . . . . ? C31 C32 C36 C37 -179.6(4) . . . . ? C33 C32 C36 C37 4.3(6) . . . . ? C31 C32 C36 C35 2.4(6) . . . . ? C33 C32 C36 C35 -173.7(4) . . . . ? C35 C36 C37 C38 2.1(6) . . . . ? C32 C36 C37 C38 -176.0(4) . . . . ? C36 C37 C38 N9 -1.2(6) . . . . ? N10 C39 C40 C41 -1.0(4) . . . . ? N10 C39 C40 C44 -178.0(4) . . . . ? C39 C40 C41 N11 0.6(4) . . . . ? C44 C40 C41 N11 177.7(4) . . . . ? N12 C42 C43 C44 -4.4(6) . . . . ? C42 C43 C44 C45 1.9(6) . . . . ? C42 C43 C44 C40 177.0(4) . . . . ? C41 C40 C44 C45 -0.2(7) . . . . ? C39 C40 C44 C45 176.2(4) . . . . ? C41 C40 C44 C43 -175.0(4) . . . . ? C39 C40 C44 C43 1.4(7) . . . . ? C43 C44 C45 C46 -1.2(6) . . . . ? C40 C44 C45 C46 -176.3(4) . . . . ? C44 C45 C46 N12 2.7(6) . . . . ? C2 C1 N1 C5 -1.0(6) . . . . ? C2 C1 N1 Pd1 -179.3(3) . . . . ? C4 C5 N1 C1 0.0(6) . . . . ? C6 C5 N1 C1 173.9(3) . . . . ? C4 C5 N1 Pd1 178.6(3) . . . . ? C6 C5 N1 Pd1 -7.6(4) . . . . ? C9 C10 N2 C6 0.8(6) . . . . ? C9 C10 N2 Pd1 -179.7(3) . . . . ? C7 C6 N2 C10 3.3(6) . . . . ? C5 C6 N2 C10 -174.1(3) . . . . ? C7 C6 N2 Pd1 -176.3(3) . . . . ? C5 C6 N2 Pd1 6.3(4) . . . . ? C14 C15 N3 C11 -1.1(5) . . . . ? C16 C15 N3 C11 179.6(3) . . . . ? C14 C15 N3 Pd2 -179.4(3) . . . . ? C16 C15 N3 Pd2 1.3(4) . . . . ? C12 C11 N3 C15 3.5(5) . . . . ? C12 C11 N3 Pd2 -178.4(3) . . . . ? C19 C20 N4 C16 -3.9(6) . . . . ? C19 C20 N4 Pd2 170.1(3) . . . . ? C17 C16 N4 C20 1.8(6) . . . . ? C15 C16 N4 C20 -172.6(3) . . . . ? C17 C16 N4 Pd2 -172.9(3) . . . . ? C15 C16 N4 Pd2 12.7(4) . . . . ? C22 C21 N5 C25 1.0(6) . . . . ? C22 C21 N5 Pd3 -175.3(3) . . . . ? C24 C25 N5 C21 -2.4(6) . . . . ? C26 C25 N5 C21 179.4(3) . . . . ? C24 C25 N5 Pd3 174.4(3) . . . . ? C26 C25 N5 Pd3 -3.8(4) . . . . ? C29 C30 N6 C26 3.0(6) . . . . ? C29 C30 N6 Pd3 179.6(3) . . . . ? C27 C26 N6 C30 3.2(5) . . . . ? C25 C26 N6 C30 -174.8(4) . . . . ? C27 C26 N6 Pd3 -173.9(3) . . . . ? C25 C26 N6 Pd3 8.1(4) . . . . ? C32 C31 N7 N8 1.5(5) . . . . ? C32 C31 N7 Pd1 -175.0(3) . . . . ? C31 N7 N8 C33 -0.2(4) . . . . ? Pd1 N7 N8 C33 176.4(3) . . . . ? C31 N7 N8 Pd2 -176.8(3) . . . . ? Pd1 N7 N8 Pd2 -0.1(4) . . . . ? C32 C33 N8 N7 -1.0(4) . . . . ? C32 C33 N8 Pd2 175.0(3) . . . . ? C37 C38 N9 C34 0.7(6) . . . . ? C37 C38 N9 Pd3 178.3(3) . . . . ? C35 C34 N9 C38 -1.2(6) . . . . ? C35 C34 N9 Pd3 -178.9(3) . . . . ? C40 C39 N10 N11 1.0(4) . . . . ? C40 C39 N10 Pd1 172.3(3) . . . . ? C40 C41 N11 N10 0.0(4) . . . . ? C40 C41 N11 Pd2 -171.7(3) . . . . ? C39 N10 N11 C41 -0.6(4) . . . . ? Pd1 N10 N11 C41 -172.8(2) . . . . ? C39 N10 N11 Pd2 172.0(3) . . . . ? Pd1 N10 N11 Pd2 -0.2(4) . . . . ? C43 C42 N12 C46 5.7(6) . . . . ? C43 C42 N12 Pd3 -174.2(3) . . . 2_565 ? C45 C46 N12 C42 -4.7(6) . . . . ? C45 C46 N12 Pd3 175.2(3) . . . 2_565 ? C39 N10 Pd1 N7 -115.4(4) . . . . ? N11 N10 Pd1 N7 54.8(3) . . . . ? C39 N10 Pd1 N1 60.4(4) . . . . ? N11 N10 Pd1 N1 -129.3(3) . . . . ? C31 N7 Pd1 N10 120.6(4) . . . . ? N8 N7 Pd1 N10 -55.5(3) . . . . ? C31 N7 Pd1 N2 -58.9(4) . . . . ? N8 N7 Pd1 N2 125.0(3) . . . . ? C10 N2 Pd1 N7 -11.7(4) . . . . ? C6 N2 Pd1 N7 167.8(3) . . . . ? C10 N2 Pd1 N1 172.4(4) . . . . ? C6 N2 Pd1 N1 -8.0(3) . . . . ? C1 N1 Pd1 N10 7.5(3) . . . . ? C5 N1 Pd1 N10 -170.9(3) . . . . ? C1 N1 Pd1 N2 -173.0(4) . . . . ? C5 N1 Pd1 N2 8.6(3) . . . . ? N7 N8 Pd2 N3 -125.8(3) . . . . ? C33 N8 Pd2 N3 58.5(3) . . . . ? N7 N8 Pd2 N11 55.4(3) . . . . ? C33 N8 Pd2 N11 -120.3(3) . . . . ? C15 N3 Pd2 N8 -173.4(3) . . . . ? C11 N3 Pd2 N8 8.4(3) . . . . ? C15 N3 Pd2 N4 4.2(3) . . . . ? C11 N3 Pd2 N4 -174.0(3) . . . . ? C41 N11 Pd2 N8 115.5(4) . . . . ? N10 N11 Pd2 N8 -55.3(3) . . . . ? C41 N11 Pd2 N4 -62.0(4) . . . . ? N10 N11 Pd2 N4 127.2(3) . . . . ? C20 N4 Pd2 N3 176.3(3) . . . . ? C16 N4 Pd2 N3 -9.4(3) . . . . ? C20 N4 Pd2 N11 -4.8(3) . . . . ? C16 N4 Pd2 N11 169.6(3) . . . . ? C30 N6 Pd3 N12 -7.8(3) . . . 2_565 ? C26 N6 Pd3 N12 169.0(3) . . . 2_565 ? C30 N6 Pd3 N5 175.4(3) . . . . ? C26 N6 Pd3 N5 -7.8(2) . . . . ? C38 N9 Pd3 N12 83.6(3) . . . 2_565 ? C34 N9 Pd3 N12 -98.8(3) . . . 2_565 ? C38 N9 Pd3 N5 -99.6(3) . . . . ? C34 N9 Pd3 N5 78.0(3) . . . . ? C21 N5 Pd3 N6 -177.2(3) . . . . ? C25 N5 Pd3 N6 6.3(3) . . . . ? C21 N5 Pd3 N9 3.5(3) . . . . ? C25 N5 Pd3 N9 -173.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.358 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.073 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 843502' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H72 N24 Pd2 Pt4, H1.20 O0.60, 8(N O3), 7.4(H2 O)' _chemical_formula_sum 'C92 H88 N32 O32 Pd2 Pt4' _chemical_formula_weight 3147.10 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' Pt Pt -1.7033 8.3905 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2067(15) _cell_length_b 15.8034(16) _cell_length_c 17.2256(19) _cell_angle_alpha 116.487(2) _cell_angle_beta 102.313(4) _cell_angle_gamma 96.752(2) _cell_volume 3511.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 7173 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.93 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 4.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3795 _exptl_absorpt_correction_T_max 0.4257 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31419 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13629 _reflns_number_gt 9250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0505P)^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 13629 _refine_ls_number_parameters 808 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 C1 C 0.2109(4) 0.4379(5) -0.0086(5) 0.0447(16) Uani 1 1 d . . . H1 H 0.1914 0.4505 0.0423 0.054 Uiso 1 1 calc R . . C2 C 0.1803(5) 0.4791(4) -0.0622(4) 0.0423(16) Uani 1 1 d . . . H2 H 0.1406 0.5201 -0.0461 0.051 Uiso 1 1 calc R . . C3 C 0.2063(4) 0.4617(4) -0.1369(4) 0.0390(14) Uani 1 1 d . . . H3 H 0.1866 0.4922 -0.1704 0.047 Uiso 1 1 calc R . . C4 C 0.2611(4) 0.3996(5) -0.1626(4) 0.0420(15) Uani 1 1 d . . . H4 H 0.2778 0.3852 -0.2152 0.050 Uiso 1 1 calc R . . C5 C 0.2927(4) 0.3571(4) -0.1095(4) 0.0405(15) Uani 1 1 d . . . C6 C 0.3518(4) 0.2869(5) -0.1286(4) 0.0423(15) Uani 1 1 d . . . C7 C 0.3800(5) 0.2501(5) -0.2089(5) 0.0482(17) Uani 1 1 d . . . H7 H 0.3648 0.2716 -0.2512 0.058 Uiso 1 1 calc R . . C8 C 0.4298(4) 0.1827(5) -0.2206(5) 0.0446(17) Uani 1 1 d . . . H8 H 0.4524 0.1611 -0.2705 0.054 Uiso 1 1 calc R . . C9 C 0.4485(5) 0.1454(5) -0.1662(5) 0.0505(17) Uani 1 1 d . . . H9 H 0.4748 0.0921 -0.1822 0.061 Uiso 1 1 calc R . . C10 C 0.4272(5) 0.1893(5) -0.0804(5) 0.0458(16) Uani 1 1 d . . . H10 H 0.4474 0.1720 -0.0358 0.055 Uiso 1 1 calc R . . C11 C 0.2303(4) -0.0279(5) -0.0367(4) 0.0452(17) Uani 1 1 d . . . H11 H 0.2908 0.0002 0.0018 0.054 Uiso 1 1 calc R . . C12 C 0.2083(4) -0.1255(4) -0.1050(4) 0.0409(15) Uani 1 1 d . . . H12 H 0.2531 -0.1614 -0.1106 0.049 Uiso 1 1 calc R . . C13 C 0.1178(5) -0.1683(4) -0.1647(5) 0.0476(18) Uani 1 1 d . . . H13 H 0.1020 -0.2303 -0.2148 0.057 Uiso 1 1 calc R . . C14 C 0.0535(5) -0.1134(4) -0.1452(4) 0.0459(17) Uani 1 1 d . . . H14 H -0.0091 -0.1420 -0.1767 0.055 Uiso 1 1 calc R . . C15 C 0.0820(4) -0.0129(4) -0.0771(4) 0.0346(13) Uani 1 1 d . . . C16 C 0.0164(5) 0.0521(5) -0.0661(5) 0.0495(17) Uani 1 1 d . . . C17 C -0.0741(5) 0.0266(5) -0.1176(5) 0.0445(16) Uani 1 1 d . . . H17 H -0.1014 -0.0380 -0.1615 0.053 Uiso 1 1 calc R . . C18 C -0.1254(4) 0.0956(5) -0.1051(5) 0.0457(16) Uani 1 1 d . . . H18 H -0.1866 0.0780 -0.1409 0.055 Uiso 1 1 calc R . . C19 C -0.0847(4) 0.1911(5) -0.0387(5) 0.0503(19) Uani 1 1 d . . . H19 H -0.1173 0.2393 -0.0302 0.060 Uiso 1 1 calc R . . C20 C 0.0080(5) 0.2142(5) 0.0162(5) 0.0504(18) Uani 1 1 d . . . H20 H 0.0365 0.2776 0.0624 0.060 Uiso 1 1 calc R . . C21 C 0.1806(4) 0.3598(4) 0.2224(4) 0.0404(15) Uani 1 1 d . . . H21 H 0.1404 0.3352 0.2453 0.049 Uiso 1 1 calc R . . C22 C 0.2211(5) 0.4587(4) 0.2564(4) 0.0410(15) Uani 1 1 d . . . C23 C 0.2776(4) 0.4633(4) 0.2043(4) 0.0338(13) Uani 1 1 d . . . H23 H 0.3144 0.5199 0.2129 0.041 Uiso 1 1 calc R . . C24 C 0.2327(5) 0.7194(5) 0.4304(5) 0.0485(17) Uani 1 1 d . . . H24 H 0.2583 0.7824 0.4434 0.058 Uiso 1 1 calc R . . C25 C 0.2462(4) 0.6349(4) 0.3536(4) 0.0417(16) Uani 1 1 d . . . H25 H 0.2824 0.6446 0.3197 0.050 Uiso 1 1 calc R . . C26 C 0.2052(5) 0.5413(5) 0.3322(5) 0.0447(16) Uani 1 1 d . . . C27 C 0.1564(4) 0.5327(5) 0.3892(4) 0.0393(14) Uani 1 1 d . . . H27 H 0.1324 0.4711 0.3805 0.047 Uiso 1 1 calc R . . C28 C 0.1433(4) 0.6105(5) 0.4558(4) 0.0390(14) Uani 1 1 d . . . H28 H 0.1049 0.6015 0.4883 0.047 Uiso 1 1 calc R . . C29 C 0.0019(4) 0.7621(5) 0.4082(4) 0.0452(17) Uani 1 1 d . . . H29 H 0.0298 0.7146 0.3752 0.054 Uiso 1 1 calc R . . C30 C -0.0801(4) 0.7678(4) 0.3647(5) 0.054(2) Uani 1 1 d . . . H30 H -0.1075 0.7231 0.3034 0.065 Uiso 1 1 calc R . . C31 C -0.1248(5) 0.8381(5) 0.4084(5) 0.0462(16) Uani 1 1 d . . . H31 H -0.1807 0.8425 0.3775 0.055 Uiso 1 1 calc R . . C32 C -0.0823(4) 0.9023(5) 0.5010(5) 0.0510(19) Uani 1 1 d . . . H32 H -0.1108 0.9492 0.5340 0.061 Uiso 1 1 calc R . . C33 C 0.0045(5) 0.8950(5) 0.5437(4) 0.0461(16) Uani 1 1 d . . . C34 C 0.0567(4) 0.9634(4) 0.6376(4) 0.0396(14) Uani 1 1 d . . . C35 C 0.0256(5) 1.0410(5) 0.6944(4) 0.0441(16) Uani 1 1 d . . . H35 H -0.0341 1.0469 0.6747 0.053 Uiso 1 1 calc R . . C36 C 0.0812(5) 1.1063(5) 0.7766(4) 0.0445(16) Uani 1 1 d . . . H36 H 0.0664 1.1641 0.8116 0.053 Uiso 1 1 calc R . . C37 C 0.1693(5) 1.0819(5) 0.8103(5) 0.0519(19) Uani 1 1 d . . . H37 H 0.2069 1.1208 0.8700 0.062 Uiso 1 1 calc R . . C38 C 0.1918(4) 1.0077(4) 0.7560(4) 0.0372(14) Uani 1 1 d . . . H38 H 0.2492 0.9973 0.7761 0.045 Uiso 1 1 calc R . . C39 C 0.2756(4) 0.7631(4) 0.6915(4) 0.0344(13) Uani 1 1 d . . . H39 H 0.2182 0.7252 0.6810 0.041 Uiso 1 1 calc R . . C40 C 0.3556(4) 0.7548(4) 0.7420(4) 0.0409(15) Uani 1 1 d . . . H40 H 0.3506 0.7119 0.7651 0.049 Uiso 1 1 calc R . . C41 C 0.4415(4) 0.8089(4) 0.7583(4) 0.0342(13) Uani 1 1 d . . . C42 C 0.4435(4) 0.8694(4) 0.7212(4) 0.0394(15) Uani 1 1 d . . . H42 H 0.5004 0.9063 0.7294 0.047 Uiso 1 1 calc R . . C43 C 0.3660(4) 0.8770(4) 0.6737(4) 0.0410(15) Uani 1 1 d . . . H43 H 0.3709 0.9197 0.6504 0.049 Uiso 1 1 calc R . . C44 C 0.5287(5) 0.7432(5) 0.8550(4) 0.0403(15) Uani 1 1 d . . . H44 H 0.4770 0.7074 0.8572 0.048 Uiso 1 1 calc R . . C45 C 0.5256(4) 0.7951(4) 0.8097(4) 0.0412(15) Uani 1 1 d . . . C46 C 0.6220(4) 0.8395(5) 0.8284(4) 0.0435(16) Uani 1 1 d . . . H46 H 0.6433 0.8801 0.8071 0.052 Uiso 1 1 calc R . . N1 N 0.2694(4) 0.3790(4) -0.0312(3) 0.0401(12) Uani 1 1 d . . . N2 N 0.3754(4) 0.2579(4) -0.0683(4) 0.0438(13) Uani 1 1 d . . . N3 N 0.1690(3) 0.0261(3) -0.0246(3) 0.0374(12) Uani 1 1 d . . . N4 N 0.0545(3) 0.1429(4) 0.0006(3) 0.0394(12) Uani 1 1 d . . . N5 N 0.2102(4) 0.3057(4) 0.1498(3) 0.0382(12) Uani 1 1 d . . . N6 N 0.2702(3) 0.3712(4) 0.1384(4) 0.0403(12) Uani 1 1 d . . . N7 N 0.1855(4) 0.7056(4) 0.4788(4) 0.0435(13) Uani 1 1 d . . . N8 N 0.0462(4) 0.8233(3) 0.4992(4) 0.0388(12) Uani 1 1 d . . . N9 N 0.1363(3) 0.9417(4) 0.6694(4) 0.0432(13) Uani 1 1 d . . . N10 N 0.2798(3) 0.8246(4) 0.6577(4) 0.0390(12) Uani 1 1 d . . . N11 N 0.6180(4) 0.7512(4) 0.8965(4) 0.0437(13) Uani 1 1 d . . . N12 N 0.6731(4) 0.8133(4) 0.8793(3) 0.0373(12) Uani 1 1 d . . . N13 N 0.3164(4) 0.6889(4) 0.9573(4) 0.0434(13) Uani 1 1 d . . . N14 N 0.1707(4) 0.8587(4) 0.3212(4) 0.0484(14) Uani 1 1 d . . . N15 N 0.4989(4) 0.7270(5) 0.4988(4) 0.0532(16) Uani 1 1 d . . . N16 N 0.9484(5) 0.6804(5) 0.5992(4) 0.0564(16) Uani 1 1 d . . . O1 O 0.3705(3) 0.6788(3) 1.0184(3) 0.0505(12) Uani 1 1 d . . . O2 O 0.2491(3) 0.7251(3) 0.9736(3) 0.0519(12) Uani 1 1 d . . . O3 O 0.3269(3) 0.6585(3) 0.8806(3) 0.0448(11) Uani 1 1 d . . . O4 O 0.1491(3) 0.9056(4) 0.3902(3) 0.0531(13) Uani 1 1 d . . . O5 O 0.1107(3) 0.8239(3) 0.2438(3) 0.0512(12) Uani 1 1 d . . . O6 O 0.2479(3) 0.8399(3) 0.3262(3) 0.0505(12) Uani 1 1 d . . . O7 O 0.4706(3) 0.8028(4) 0.5080(4) 0.0629(15) Uani 1 1 d . . . O8 O 0.5719(4) 0.7176(4) 0.4740(3) 0.0587(14) Uani 1 1 d . . . O9 O 0.4549(3) 0.6640(4) 0.5107(3) 0.0510(12) Uani 1 1 d . . . O10 O 0.9019(3) 0.6756(4) 0.5275(3) 0.0569(13) Uani 1 1 d . . . O11 O 1.0302(4) 0.6681(4) 0.6057(4) 0.0668(15) Uani 1 1 d . . . O12 O 0.9177(3) 0.6985(3) 0.6638(3) 0.0480(11) Uani 1 1 d . . . O1W O 0.6385(8) 0.6505(8) 0.6188(8) 0.031(3) Uani 0.30 1 d P . . H1X H 0.6934 0.6737 0.6224 0.037 Uiso 0.30 1 d PR . . H1Y H 0.6206 0.6938 0.6589 0.037 Uiso 0.30 1 d PR . . O2W O 0.2577(13) 0.4049(14) 0.6335(12) 0.080(6) Uani 0.30 1 d P . . H2X H 0.2871 0.3626 0.6344 0.095 Uiso 0.30 1 d PR . . H2Y H 0.2033 0.3890 0.6357 0.095 Uiso 0.30 1 d PR . . O3W O 0.4828(10) 0.5502(10) 0.9312(10) 0.047(4) Uani 0.30 1 d P . . H3X H 0.4614 0.5356 0.9665 0.056 Uiso 0.30 1 d PR . . H3Y H 0.5379 0.5430 0.9361 0.056 Uiso 0.30 1 d PR . . O4W O 0.3397(9) 0.5162(10) 0.5415(8) 0.040(4) Uani 0.30 1 d P . . H4X H 0.3596 0.5212 0.5937 0.048 Uiso 0.30 1 d PR . . H4Y H 0.2809 0.5048 0.5258 0.048 Uiso 0.30 1 d PR . . O5W O 0.2614(8) 0.0621(10) 0.3606(9) 0.040(3) Uani 0.30 1 d P . . H5X H 0.2713 0.1238 0.3854 0.047 Uiso 0.30 1 d PR . . H5Y H 0.3121 0.0465 0.3730 0.047 Uiso 0.30 1 d PR . . O6W O 0.3654(9) 0.9131(10) 0.0828(10) 0.041(3) Uani 0.30 1 d P . . H6X H 0.3591 0.8845 0.1137 0.049 Uiso 0.30 1 d PR . . H6Y H 0.3876 0.9739 0.1184 0.049 Uiso 0.30 1 d PR . . O7W O 0.5164(9) 0.5417(10) 0.2309(10) 0.043(4) Uani 0.30 1 d P . . H7X H 0.5170 0.5823 0.2111 0.052 Uiso 0.30 1 d PR . . H7Y H 0.4886 0.5576 0.2713 0.052 Uiso 0.30 1 d PR . . O8W O 0.6694(9) 0.8247(9) 0.4569(9) 0.039(3) Uani 0.30 1 d P . . H8X H 0.6387 0.7691 0.4130 0.047 Uiso 0.30 1 d PR . . H8Y H 0.6885 0.8200 0.5046 0.047 Uiso 0.30 1 d PR . . O9W O 0.0221(10) 0.4345(10) 0.0744(11) 0.049(4) Uani 0.30 1 d P . . H9X H 0.0771 0.4675 0.1069 0.058 Uiso 0.30 1 d PR . . H9Y H 0.0169 0.4176 0.0190 0.058 Uiso 0.30 1 d PR . . O10W O 0.4812(8) -0.0200(10) 0.5826(10) 0.040(4) Uani 0.30 1 d P . . H10X H 0.4544 0.0191 0.6162 0.048 Uiso 0.30 1 d PR . . H10Y H 0.5144 0.0095 0.5639 0.048 Uiso 0.30 1 d PR . . O11W O 0.3260(11) 0.7307(13) 0.1487(11) 0.058(5) Uani 0.30 1 d P . . H11X H 0.3016 0.6699 0.1162 0.070 Uiso 0.30 1 d PR . . H11Y H 0.3606 0.7488 0.1234 0.070 Uiso 0.30 1 d PR . . O12W O 0.5000 0.0000 1.0000 0.050(3) Uani 0.60 2 d SP . . H12X H 0.5094 -0.0154 0.9490 0.060 Uiso 0.30 1 d PR . . H12Y H 0.4653 0.0398 1.0098 0.060 Uiso 0.30 1 d PR . . O13W O 0.8543(9) 0.4112(9) 0.2737(9) 0.060(3) Uani 0.40 1 d P . . H13X H 0.8590 0.3789 0.2206 0.071 Uiso 0.40 1 d PR . . H13Y H 0.8998 0.4609 0.3051 0.071 Uiso 0.40 1 d PR . . Pd1 Pd 0.16250(3) 0.82297(3) 0.57610(3) 0.04070(13) Uani 1 1 d . . . Pt1 Pt 0.32439(2) 0.31315(2) 0.03666(2) 0.05375(10) Uani 1 1 d . . . Pt2 Pt 0.19152(2) 0.16752(2) 0.06568(2) 0.05119(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 0.031(3) 0.050(4) 0.040(4) 0.013(3) 0.010(3) 0.000(3) C2 0.050(4) 0.029(3) 0.038(4) 0.009(3) 0.012(3) 0.009(3) C3 0.033(3) 0.041(3) 0.030(3) 0.014(3) -0.006(3) 0.001(3) C4 0.029(3) 0.045(4) 0.033(3) 0.008(3) 0.005(3) 0.002(3) C5 0.038(3) 0.036(3) 0.025(3) 0.001(2) 0.002(3) 0.005(3) C6 0.034(3) 0.043(3) 0.034(3) 0.013(3) -0.003(3) 0.005(3) C7 0.046(4) 0.050(4) 0.042(4) 0.021(3) 0.009(3) 0.003(3) C8 0.023(3) 0.056(4) 0.041(4) 0.012(3) 0.012(3) 0.008(3) C9 0.046(4) 0.045(4) 0.046(4) 0.014(3) 0.006(3) 0.008(3) C10 0.052(4) 0.037(3) 0.039(4) 0.017(3) 0.004(3) 0.004(3) C11 0.030(3) 0.054(4) 0.029(3) 0.002(3) 0.012(3) 0.003(3) C12 0.044(4) 0.035(3) 0.041(4) 0.014(3) 0.015(3) 0.014(3) C13 0.049(4) 0.021(3) 0.047(4) 0.005(3) -0.005(3) 0.003(3) C14 0.050(4) 0.027(3) 0.035(4) -0.006(3) 0.012(3) 0.006(3) C15 0.041(3) 0.035(3) 0.023(3) 0.006(2) 0.018(3) 0.011(3) C16 0.038(4) 0.054(4) 0.049(4) 0.019(3) 0.018(3) 0.005(3) C17 0.046(4) 0.037(3) 0.058(4) 0.025(3) 0.023(3) 0.014(3) C18 0.028(3) 0.047(4) 0.060(4) 0.023(3) 0.013(3) 0.015(3) C19 0.031(3) 0.043(4) 0.050(4) 0.007(3) -0.006(3) 0.013(3) C20 0.043(4) 0.038(3) 0.056(4) 0.016(3) 0.006(3) 0.008(3) C21 0.045(4) 0.038(3) 0.040(3) 0.020(3) 0.021(3) -0.007(3) C22 0.049(4) 0.024(3) 0.038(3) 0.006(3) 0.011(3) 0.009(3) C23 0.028(3) 0.042(3) 0.028(3) 0.012(3) 0.009(2) 0.020(3) C24 0.039(4) 0.045(4) 0.045(4) 0.018(3) -0.002(3) -0.001(3) C25 0.036(3) 0.038(3) 0.039(3) 0.015(3) 0.011(3) -0.019(3) C26 0.056(4) 0.034(3) 0.046(4) 0.016(3) 0.028(3) 0.009(3) C27 0.041(3) 0.038(3) 0.038(3) 0.017(3) 0.016(3) 0.006(3) C28 0.034(3) 0.047(4) 0.027(3) 0.012(3) 0.008(3) 0.009(3) C29 0.041(4) 0.048(4) 0.032(3) 0.001(3) 0.021(3) 0.014(3) C30 0.030(3) 0.030(3) 0.059(5) 0.001(3) -0.011(3) -0.009(3) C31 0.047(4) 0.055(4) 0.039(4) 0.026(3) 0.013(3) 0.014(3) C32 0.032(3) 0.054(4) 0.041(4) 0.002(3) 0.010(3) 0.013(3) C33 0.057(4) 0.043(4) 0.037(4) 0.018(3) 0.011(3) 0.022(3) C34 0.040(3) 0.032(3) 0.036(3) 0.010(3) 0.011(3) 0.002(3) C35 0.041(4) 0.043(4) 0.046(4) 0.024(3) 0.004(3) 0.011(3) C36 0.048(4) 0.038(3) 0.042(4) 0.011(3) 0.024(3) 0.008(3) C37 0.033(3) 0.047(4) 0.038(4) 0.002(3) -0.006(3) -0.011(3) C38 0.034(3) 0.037(3) 0.037(3) 0.018(3) 0.006(3) 0.006(3) C39 0.039(3) 0.038(3) 0.032(3) 0.019(3) 0.017(3) 0.015(3) C40 0.034(3) 0.037(3) 0.040(3) 0.013(3) 0.002(3) 0.008(3) C41 0.029(3) 0.029(3) 0.038(3) 0.010(2) 0.011(3) 0.011(2) C42 0.032(3) 0.037(3) 0.046(4) 0.017(3) 0.012(3) 0.015(3) C43 0.038(3) 0.037(3) 0.042(4) 0.015(3) 0.008(3) 0.013(3) C44 0.043(4) 0.042(3) 0.043(4) 0.022(3) 0.020(3) 0.020(3) C45 0.038(3) 0.035(3) 0.046(4) 0.012(3) 0.016(3) 0.016(3) C46 0.030(3) 0.052(4) 0.034(3) 0.007(3) 0.008(3) 0.016(3) N1 0.042(3) 0.043(3) 0.030(3) 0.014(2) 0.015(2) 0.000(2) N2 0.044(3) 0.038(3) 0.031(3) 0.010(2) -0.003(2) 0.003(2) N3 0.036(3) 0.032(3) 0.031(3) 0.009(2) 0.004(2) -0.001(2) N4 0.034(3) 0.040(3) 0.035(3) 0.007(2) 0.016(2) 0.014(2) N5 0.042(3) 0.040(3) 0.030(3) 0.015(2) 0.007(2) 0.015(2) N6 0.031(3) 0.042(3) 0.039(3) 0.015(2) 0.004(2) 0.013(2) N7 0.034(3) 0.042(3) 0.042(3) 0.013(3) 0.006(2) 0.004(2) N8 0.040(3) 0.031(3) 0.044(3) 0.019(2) 0.006(2) 0.011(2) N9 0.034(3) 0.040(3) 0.038(3) 0.004(2) 0.013(2) 0.008(2) N10 0.036(3) 0.031(3) 0.047(3) 0.013(2) 0.017(2) 0.015(2) N11 0.042(3) 0.038(3) 0.043(3) 0.013(2) 0.013(3) 0.008(2) N12 0.039(3) 0.043(3) 0.026(3) 0.010(2) 0.019(2) 0.011(2) N13 0.052(3) 0.038(3) 0.035(3) 0.011(2) 0.017(3) 0.008(3) N14 0.054(4) 0.043(3) 0.039(3) 0.014(3) 0.010(3) 0.009(3) N15 0.053(4) 0.047(4) 0.053(4) 0.012(3) 0.022(3) 0.029(3) N16 0.056(4) 0.059(4) 0.043(4) 0.017(3) 0.013(3) 0.013(3) O1 0.044(3) 0.051(3) 0.040(3) 0.009(2) 0.013(2) 0.010(2) O2 0.060(3) 0.045(3) 0.046(3) 0.013(2) 0.025(2) 0.015(2) O3 0.045(3) 0.037(2) 0.046(3) 0.013(2) 0.018(2) 0.010(2) O4 0.041(3) 0.059(3) 0.041(3) 0.012(2) 0.000(2) 0.023(2) O5 0.052(3) 0.046(3) 0.047(3) 0.015(2) 0.013(2) 0.018(2) O6 0.036(2) 0.054(3) 0.058(3) 0.022(2) 0.012(2) 0.023(2) O7 0.045(3) 0.059(3) 0.059(3) 0.016(3) 0.010(3) -0.018(3) O8 0.060(3) 0.058(3) 0.041(3) 0.014(2) 0.017(2) -0.008(3) O9 0.047(3) 0.046(3) 0.053(3) 0.020(2) 0.010(2) 0.017(2) O10 0.051(3) 0.058(3) 0.047(3) 0.015(2) 0.008(2) 0.016(2) O11 0.089(4) 0.069(4) 0.064(4) 0.041(3) 0.038(3) 0.026(3) O12 0.054(3) 0.043(3) 0.045(3) 0.015(2) 0.022(2) 0.016(2) O1W 0.026(6) 0.021(6) 0.029(7) -0.001(5) 0.005(5) 0.010(5) O2W 0.065(12) 0.071(12) 0.048(11) -0.004(9) -0.007(9) 0.010(10) O3W 0.030(7) 0.038(8) 0.050(9) 0.012(7) 0.004(7) -0.014(6) O4W 0.038(8) 0.040(7) 0.020(6) 0.004(6) -0.012(6) 0.013(6) O5W 0.011(6) 0.039(7) 0.043(8) 0.011(6) -0.013(6) -0.004(5) O6W 0.037(8) 0.030(7) 0.048(9) 0.019(6) 0.001(6) 0.009(6) O7W 0.025(7) 0.033(7) 0.060(10) 0.014(7) 0.004(6) 0.012(6) O8W 0.041(8) 0.026(6) 0.026(7) -0.001(5) 0.001(6) -0.004(6) O9W 0.036(8) 0.034(8) 0.064(10) 0.013(7) 0.014(7) 0.012(6) O10W 0.012(6) 0.039(7) 0.067(10) 0.023(7) 0.016(6) 0.008(5) O11W 0.045(9) 0.065(10) 0.041(9) 0.015(8) -0.009(7) 0.013(8) O12W 0.044(6) 0.035(5) 0.048(6) -0.002(5) 0.015(5) 0.020(5) O13W 0.078(9) 0.045(7) 0.069(9) 0.032(6) 0.038(7) 0.014(6) Pd1 0.0303(2) 0.0351(2) 0.0343(3) 0.0021(2) 0.00103(19) 0.00788(19) Pt1 0.05035(18) 0.04912(17) 0.04838(18) 0.01211(13) 0.01406(13) 0.01512(13) Pt2 0.04994(17) 0.04281(15) 0.04733(17) 0.01109(12) 0.01289(13) 0.01255(12) _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 1.352(8) . ? C1 C2 1.385(10) . ? C1 H1 0.9300 . ? C2 C3 1.346(9) . ? C2 H2 0.9300 . ? C3 C4 1.347(9) . ? C3 H3 0.9300 . ? C4 C5 1.399(10) . ? C4 H4 0.9300 . ? C5 N1 1.370(8) . ? C5 C6 1.477(9) . ? C6 N2 1.314(8) . ? C6 C7 1.424(9) . ? C7 C8 1.346(9) . ? C7 H7 0.9300 . ? C8 C9 1.315(10) . ? C8 H8 0.9300 . ? C9 C10 1.454(10) . ? C9 H9 0.9300 . ? C10 N2 1.381(9) . ? C10 H10 0.9300 . ? C11 N3 1.324(8) . ? C11 C12 1.403(8) . ? C11 H11 0.9300 . ? C12 C13 1.402(9) . ? C12 H12 0.9300 . ? C13 C14 1.379(9) . ? C13 H13 0.9300 . ? C14 C15 1.430(8) . ? C14 H14 0.9300 . ? C15 N3 1.322(8) . ? C15 C16 1.495(9) . ? C16 N4 1.328(8) . ? C16 C17 1.369(10) . ? C17 C18 1.381(9) . ? C17 H17 0.9300 . ? C18 C19 1.381(9) . ? C18 H18 0.9300 . ? C19 C20 1.420(9) . ? C19 H19 0.9300 . ? C20 N4 1.357(8) . ? C20 H20 0.9300 . ? C21 N5 1.369(8) . ? C21 C22 1.403(8) . ? C21 H21 0.9300 . ? C22 C23 1.386(9) . ? C22 C26 1.469(8) . ? C23 N6 1.361(7) . ? C23 H23 0.9300 . ? C24 N7 1.281(9) . ? C24 C25 1.476(9) . ? C24 H24 0.9300 . ? C25 C26 1.381(8) . ? C25 H25 0.9300 . ? C26 C27 1.393(9) . ? C27 C28 1.328(8) . ? C27 H27 0.9300 . ? C28 N7 1.400(8) . ? C28 H28 0.9300 . ? C29 C30 1.347(9) . ? C29 N8 1.374(8) . ? C29 H29 0.9300 . ? C30 C31 1.383(9) . ? C30 H30 0.9300 . ? C31 C32 1.397(9) . ? C31 H31 0.9300 . ? C32 C33 1.412(9) . ? C32 H32 0.9300 . ? C33 N8 1.369(8) . ? C33 C34 1.451(9) . ? C34 N9 1.366(8) . ? C34 C35 1.396(9) . ? C35 C36 1.329(9) . ? C35 H35 0.9300 . ? C36 C37 1.506(10) . ? C36 H36 0.9300 . ? C37 C38 1.273(9) . ? C37 H37 0.9300 . ? C38 N9 1.376(8) . ? C38 H38 0.9300 . ? C39 N10 1.338(8) . ? C39 C40 1.394(8) . ? C39 H39 0.9300 . ? C40 C41 1.373(8) . ? C40 H40 0.9300 . ? C41 C42 1.367(9) . ? C41 C45 1.491(9) . ? C42 C43 1.335(8) . ? C42 H42 0.9300 . ? C43 N10 1.367(8) . ? C43 H43 0.9300 . ? C44 N11 1.354(8) . ? C44 C45 1.359(9) . ? C44 H44 0.9300 . ? C45 C46 1.449(9) . ? C46 N12 1.286(8) . ? C46 H46 0.9300 . ? N1 Pt1 2.006(6) . ? N2 Pt1 1.995(6) . ? N3 Pt2 2.006(5) . ? N4 Pt2 2.043(5) . ? N5 N6 1.407(8) . ? N5 Pt2 1.950(5) . ? N6 Pt1 1.988(5) . ? N7 Pd1 2.000(5) . ? N8 Pd1 1.973(5) . ? N9 Pd1 2.005(5) . ? N10 Pd1 2.012(5) . ? N11 N12 1.387(7) . ? N11 Pt1 1.988(6) 2_666 ? N12 Pt2 1.998(5) 2_666 ? N13 O3 1.243(7) . ? N13 O2 1.253(7) . ? N13 O1 1.275(7) . ? N14 O4 1.228(7) . ? N14 O6 1.240(7) . ? N14 O5 1.274(7) . ? N15 O9 1.250(8) . ? N15 O8 1.274(7) . ? N15 O7 1.275(8) . ? N16 O12 1.228(7) . ? N16 O10 1.251(8) . ? N16 O11 1.270(8) . ? O1W H1X 0.8499 . ? O1W H1Y 0.8501 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8501 . ? O3W H3X 0.8500 . ? O3W H3Y 0.8500 . ? O4W H4X 0.8500 . ? O4W H4Y 0.8500 . ? O5W H5X 0.8500 . ? O5W H5Y 0.8500 . ? O6W H6X 0.8500 . ? O6W H6Y 0.8500 . ? O7W H7X 0.8500 . ? O7W H7Y 0.8500 . ? O8W H8X 0.8500 . ? O8W H8Y 0.8499 . ? O9W H9X 0.8499 . ? O9W H9Y 0.8499 . ? O10W H10X 0.8500 . ? O10W H10Y 0.8500 . ? O11W H11X 0.8500 . ? O11W H11Y 0.8500 . ? O12W H12X 0.8500 . ? O12W H12Y 0.8500 . ? O13W H13X 0.8499 . ? O13W H13Y 0.8500 . ? Pt1 N11 1.988(6) 2_666 ? Pt1 Pt2 3.1612(5) . ? Pt2 N12 1.998(5) 2_666 ? 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 119.2(6) . . ? N1 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C3 C2 C1 122.1(6) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 119.4(6) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.4(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 120.6(6) . . ? N1 C5 C6 113.2(6) . . ? C4 C5 C6 126.2(6) . . ? N2 C6 C7 121.3(6) . . ? N2 C6 C5 116.1(6) . . ? C7 C6 C5 122.5(6) . . ? C8 C7 C6 116.7(7) . . ? C8 C7 H7 121.7 . . ? C6 C7 H7 121.7 . . ? C9 C8 C7 124.3(7) . . ? C9 C8 H8 117.9 . . ? C7 C8 H8 117.9 . . ? C8 C9 C10 118.6(7) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 116.7(6) . . ? N2 C10 H10 121.6 . . ? C9 C10 H10 121.6 . . ? N3 C11 C12 123.1(6) . . ? N3 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 119.0(6) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 116.4(5) . . ? C14 C13 H13 121.8 . . ? C12 C13 H13 121.8 . . ? C13 C14 C15 120.7(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? N3 C15 C14 120.4(6) . . ? N3 C15 C16 118.1(5) . . ? C14 C15 C16 121.5(6) . . ? N4 C16 C17 120.2(6) . . ? N4 C16 C15 113.3(6) . . ? C17 C16 C15 126.5(6) . . ? C16 C17 C18 120.8(6) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 119.2(6) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 118.5(6) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N4 C20 C19 119.4(6) . . ? N4 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? N5 C21 C22 108.5(5) . . ? N5 C21 H21 125.7 . . ? C22 C21 H21 125.7 . . ? C23 C22 C21 107.1(5) . . ? C23 C22 C26 126.8(6) . . ? C21 C22 C26 126.1(6) . . ? N6 C23 C22 108.7(6) . . ? N6 C23 H23 125.6 . . ? C22 C23 H23 125.6 . . ? N7 C24 C25 119.7(6) . . ? N7 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 120.1(6) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 116.6(6) . . ? C25 C26 C22 118.8(6) . . ? C27 C26 C22 124.5(6) . . ? C28 C27 C26 121.4(6) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 N7 122.2(6) . . ? C27 C28 H28 118.9 . . ? N7 C28 H28 118.9 . . ? C30 C29 N8 123.0(6) . . ? C30 C29 H29 118.5 . . ? N8 C29 H29 118.5 . . ? C29 C30 C31 122.0(6) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C30 C31 C32 117.1(6) . . ? C30 C31 H31 121.4 . . ? C32 C31 H31 121.4 . . ? C31 C32 C33 119.1(6) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? N8 C33 C32 122.4(6) . . ? N8 C33 C34 114.9(6) . . ? C32 C33 C34 122.6(6) . . ? N9 C34 C35 121.5(6) . . ? N9 C34 C33 114.7(5) . . ? C35 C34 C33 123.5(6) . . ? C36 C35 C34 120.0(6) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 116.7(6) . . ? C35 C36 H36 121.6 . . ? C37 C36 H36 121.6 . . ? C38 C37 C36 119.2(6) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 N9 124.0(6) . . ? C37 C38 H38 118.0 . . ? N9 C38 H38 118.0 . . ? N10 C39 C40 121.2(6) . . ? N10 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C41 C40 C39 121.1(6) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 116.2(6) . . ? C42 C41 C45 124.4(6) . . ? C40 C41 C45 119.4(6) . . ? C43 C42 C41 121.8(6) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 N10 122.8(6) . . ? C42 C43 H43 118.6 . . ? N10 C43 H43 118.6 . . ? N11 C44 C45 110.0(6) . . ? N11 C44 H44 125.0 . . ? C45 C44 H44 125.0 . . ? C44 C45 C46 104.5(6) . . ? C44 C45 C41 127.5(6) . . ? C46 C45 C41 127.9(6) . . ? N12 C46 C45 108.6(7) . . ? N12 C46 H46 125.7 . . ? C45 C46 H46 125.7 . . ? C1 N1 C5 119.2(6) . . ? C1 N1 Pt1 126.4(4) . . ? C5 N1 Pt1 114.4(4) . . ? C6 N2 C10 121.7(6) . . ? C6 N2 Pt1 115.3(5) . . ? C10 N2 Pt1 122.9(5) . . ? C15 N3 C11 119.6(5) . . ? C15 N3 Pt2 112.9(4) . . ? C11 N3 Pt2 127.5(4) . . ? C16 N4 C20 121.8(6) . . ? C16 N4 Pt2 114.2(4) . . ? C20 N4 Pt2 123.7(4) . . ? C21 N5 N6 107.3(5) . . ? C21 N5 Pt2 136.3(4) . . ? N6 N5 Pt2 116.4(4) . . ? C23 N6 N5 108.4(5) . . ? C23 N6 Pt1 135.1(5) . . ? N5 N6 Pt1 116.5(4) . . ? C24 N7 C28 119.7(6) . . ? C24 N7 Pd1 117.5(5) . . ? C28 N7 Pd1 122.4(4) . . ? C33 N8 C29 116.2(5) . . ? C33 N8 Pd1 114.6(4) . . ? C29 N8 Pd1 129.2(4) . . ? C34 N9 C38 117.1(5) . . ? C34 N9 Pd1 113.8(4) . . ? C38 N9 Pd1 128.6(4) . . ? C39 N10 C43 116.9(5) . . ? C39 N10 Pd1 118.5(4) . . ? C43 N10 Pd1 124.3(4) . . ? C44 N11 N12 106.9(5) . . ? C44 N11 Pt1 132.6(5) . 2_666 ? N12 N11 Pt1 120.3(4) . 2_666 ? C46 N12 N11 110.0(5) . . ? C46 N12 Pt2 137.4(5) . 2_666 ? N11 N12 Pt2 112.5(4) . 2_666 ? O3 N13 O2 120.1(6) . . ? O3 N13 O1 120.6(5) . . ? O2 N13 O1 119.2(5) . . ? O4 N14 O6 120.8(6) . . ? O4 N14 O5 119.3(6) . . ? O6 N14 O5 119.7(6) . . ? O9 N15 O8 122.2(6) . . ? O9 N15 O7 121.2(6) . . ? O8 N15 O7 116.5(7) . . ? O12 N16 O10 121.6(7) . . ? O12 N16 O11 119.5(7) . . ? O10 N16 O11 118.8(6) . . ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 109.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 109.5 . . ? H5X O5W H5Y 109.5 . . ? H6X O6W H6Y 109.5 . . ? H7X O7W H7Y 109.5 . . ? H8X O8W H8Y 109.5 . . ? H9X O9W H9Y 109.5 . . ? H10X O10W H10Y 109.5 . . ? H11X O11W H11Y 109.5 . . ? H12X O12W H12Y 109.5 . . ? H13X O13W H13Y 109.5 . . ? N8 Pd1 N7 96.1(2) . . ? N8 Pd1 N9 81.7(2) . . ? N7 Pd1 N9 177.5(2) . . ? N8 Pd1 N10 178.3(2) . . ? N7 Pd1 N10 85.4(2) . . ? N9 Pd1 N10 96.8(2) . . ? N6 Pt1 N11 84.7(2) . 2_666 ? N6 Pt1 N2 177.3(2) . . ? N11 Pt1 N2 98.0(2) 2_666 . ? N6 Pt1 N1 96.4(2) . . ? N11 Pt1 N1 178.5(2) 2_666 . ? N2 Pt1 N1 80.9(2) . . ? N6 Pt1 Pt2 62.90(16) . . ? N11 Pt1 Pt2 61.98(16) 2_666 . ? N2 Pt1 Pt2 118.21(15) . . ? N1 Pt1 Pt2 119.44(14) . . ? N5 Pt2 N12 86.1(2) . 2_666 ? N5 Pt2 N3 177.7(2) . . ? N12 Pt2 N3 95.7(2) 2_666 . ? N5 Pt2 N4 96.7(2) . . ? N12 Pt2 N4 175.92(19) 2_666 . ? N3 Pt2 N4 81.5(2) . . ? N5 Pt2 Pt1 64.19(16) . . ? N12 Pt2 Pt1 65.09(15) 2_666 . ? N3 Pt2 Pt1 115.22(15) . . ? N4 Pt2 Pt1 113.39(16) . . ? 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 0.7(9) . . . . ? C1 C2 C3 C4 2.4(9) . . . . ? C2 C3 C4 C5 -2.2(9) . . . . ? C3 C4 C5 N1 -0.9(9) . . . . ? C3 C4 C5 C6 179.1(6) . . . . ? N1 C5 C6 N2 -1.7(8) . . . . ? C4 C5 C6 N2 178.3(6) . . . . ? N1 C5 C6 C7 176.6(6) . . . . ? C4 C5 C6 C7 -3.5(10) . . . . ? N2 C6 C7 C8 1.6(9) . . . . ? C5 C6 C7 C8 -176.6(6) . . . . ? C6 C7 C8 C9 4.3(10) . . . . ? C7 C8 C9 C10 -9.9(10) . . . . ? C8 C9 C10 N2 9.7(9) . . . . ? N3 C11 C12 C13 1.2(11) . . . . ? C11 C12 C13 C14 -7.1(10) . . . . ? C12 C13 C14 C15 10.2(11) . . . . ? C13 C14 C15 N3 -7.7(10) . . . . ? C13 C14 C15 C16 169.1(7) . . . . ? N3 C15 C16 N4 -3.4(9) . . . . ? C14 C15 C16 N4 179.8(6) . . . . ? N3 C15 C16 C17 175.8(7) . . . . ? C14 C15 C16 C17 -1.1(11) . . . . ? N4 C16 C17 C18 4.2(11) . . . . ? C15 C16 C17 C18 -174.9(7) . . . . ? C16 C17 C18 C19 -1.0(11) . . . . ? C17 C18 C19 C20 -1.9(12) . . . . ? C18 C19 C20 N4 1.7(12) . . . . ? N5 C21 C22 C23 -1.4(8) . . . . ? N5 C21 C22 C26 177.9(6) . . . . ? C21 C22 C23 N6 2.0(7) . . . . ? C26 C22 C23 N6 -177.2(6) . . . . ? N7 C24 C25 C26 2.4(10) . . . . ? C24 C25 C26 C27 -3.5(10) . . . . ? C24 C25 C26 C22 -179.1(6) . . . . ? C23 C22 C26 C25 3.1(11) . . . . ? C21 C22 C26 C25 -176.0(7) . . . . ? C23 C22 C26 C27 -172.1(7) . . . . ? C21 C22 C26 C27 8.8(12) . . . . ? C25 C26 C27 C28 5.7(10) . . . . ? C22 C26 C27 C28 -179.0(6) . . . . ? C26 C27 C28 N7 -6.8(10) . . . . ? N8 C29 C30 C31 1.8(12) . . . . ? C29 C30 C31 C32 -1.5(11) . . . . ? C30 C31 C32 C33 2.6(11) . . . . ? C31 C32 C33 N8 -4.3(11) . . . . ? C31 C32 C33 C34 175.1(7) . . . . ? N8 C33 C34 N9 -4.7(9) . . . . ? C32 C33 C34 N9 176.0(7) . . . . ? N8 C33 C34 C35 -179.4(6) . . . . ? C32 C33 C34 C35 1.2(11) . . . . ? N9 C34 C35 C36 12.4(10) . . . . ? C33 C34 C35 C36 -173.2(7) . . . . ? C34 C35 C36 C37 -11.0(10) . . . . ? C35 C36 C37 C38 8.2(11) . . . . ? C36 C37 C38 N9 -6.1(11) . . . . ? N10 C39 C40 C41 -0.5(9) . . . . ? C39 C40 C41 C42 -0.9(9) . . . . ? C39 C40 C41 C45 -177.7(5) . . . . ? C40 C41 C42 C43 1.5(9) . . . . ? C45 C41 C42 C43 178.1(6) . . . . ? C41 C42 C43 N10 -0.7(10) . . . . ? N11 C44 C45 C46 -1.5(7) . . . . ? N11 C44 C45 C41 -177.4(5) . . . . ? C42 C41 C45 C44 173.7(6) . . . . ? C40 C41 C45 C44 -9.8(9) . . . . ? C42 C41 C45 C46 -1.2(10) . . . . ? C40 C41 C45 C46 175.3(6) . . . . ? C44 C45 C46 N12 0.3(7) . . . . ? C41 C45 C46 N12 176.1(5) . . . . ? C2 C1 N1 C5 -3.8(9) . . . . ? C2 C1 N1 Pt1 178.9(4) . . . . ? C4 C5 N1 C1 3.9(9) . . . . ? C6 C5 N1 C1 -176.1(5) . . . . ? C4 C5 N1 Pt1 -178.4(4) . . . . ? C6 C5 N1 Pt1 1.6(6) . . . . ? C7 C6 N2 C10 -1.1(9) . . . . ? C5 C6 N2 C10 177.1(5) . . . . ? C7 C6 N2 Pt1 -177.3(5) . . . . ? C5 C6 N2 Pt1 1.0(7) . . . . ? C9 C10 N2 C6 -4.4(9) . . . . ? C9 C10 N2 Pt1 171.5(4) . . . . ? C14 C15 N3 C11 1.4(9) . . . . ? C16 C15 N3 C11 -175.5(6) . . . . ? C14 C15 N3 Pt2 -179.8(5) . . . . ? C16 C15 N3 Pt2 3.3(7) . . . . ? C12 C11 N3 C15 1.7(10) . . . . ? C12 C11 N3 Pt2 -176.9(5) . . . . ? C17 C16 N4 C20 -4.4(11) . . . . ? C15 C16 N4 C20 174.8(6) . . . . ? C17 C16 N4 Pt2 -177.6(5) . . . . ? C15 C16 N4 Pt2 1.6(8) . . . . ? C19 C20 N4 C16 1.5(11) . . . . ? C19 C20 N4 Pt2 173.9(5) . . . . ? C22 C21 N5 N6 0.2(7) . . . . ? C22 C21 N5 Pt2 178.8(5) . . . . ? C22 C23 N6 N5 -1.9(6) . . . . ? C22 C23 N6 Pt1 179.2(5) . . . . ? C21 N5 N6 C23 1.0(6) . . . . ? Pt2 N5 N6 C23 -177.9(4) . . . . ? C21 N5 N6 Pt1 -179.8(4) . . . . ? Pt2 N5 N6 Pt1 1.3(5) . . . . ? C25 C24 N7 C28 -3.1(9) . . . . ? C25 C24 N7 Pd1 -175.9(5) . . . . ? C27 C28 N7 C24 5.4(10) . . . . ? C27 C28 N7 Pd1 177.8(5) . . . . ? C32 C33 N8 C29 4.3(10) . . . . ? C34 C33 N8 C29 -175.1(6) . . . . ? C32 C33 N8 Pd1 -175.7(6) . . . . ? C34 C33 N8 Pd1 5.0(8) . . . . ? C30 C29 N8 C33 -3.1(10) . . . . ? C30 C29 N8 Pd1 176.9(6) . . . . ? C35 C34 N9 C38 -9.5(9) . . . . ? C33 C34 N9 C38 175.6(6) . . . . ? C35 C34 N9 Pd1 177.0(5) . . . . ? C33 C34 N9 Pd1 2.1(7) . . . . ? C37 C38 N9 C34 6.8(10) . . . . ? C37 C38 N9 Pd1 179.1(6) . . . . ? C40 C39 N10 C43 1.3(8) . . . . ? C40 C39 N10 Pd1 174.5(4) . . . . ? C42 C43 N10 C39 -0.7(9) . . . . ? C42 C43 N10 Pd1 -173.5(5) . . . . ? C45 C44 N11 N12 2.2(7) . . . . ? C45 C44 N11 Pt1 -173.2(4) . . . 2_666 ? C45 C46 N12 N11 1.0(6) . . . . ? C45 C46 N12 Pt2 177.2(4) . . . 2_666 ? C44 N11 N12 C46 -2.0(6) . . . . ? Pt1 N11 N12 C46 174.0(4) 2_666 . . . ? C44 N11 N12 Pt2 -179.2(4) . . . 2_666 ? Pt1 N11 N12 Pt2 -3.2(5) 2_666 . . 2_666 ? C33 N8 Pd1 N7 178.1(5) . . . . ? C29 N8 Pd1 N7 -1.9(6) . . . . ? C33 N8 Pd1 N9 -3.0(5) . . . . ? C29 N8 Pd1 N9 177.0(6) . . . . ? C33 N8 Pd1 N10 26(7) . . . . ? C29 N8 Pd1 N10 -154(7) . . . . ? C24 N7 Pd1 N8 89.4(5) . . . . ? C28 N7 Pd1 N8 -83.1(5) . . . . ? C24 N7 Pd1 N9 64(5) . . . . ? C28 N7 Pd1 N9 -109(5) . . . . ? C24 N7 Pd1 N10 -91.4(5) . . . . ? C28 N7 Pd1 N10 96.1(5) . . . . ? C34 N9 Pd1 N8 0.4(5) . . . . ? C38 N9 Pd1 N8 -172.2(6) . . . . ? C34 N9 Pd1 N7 26(5) . . . . ? C38 N9 Pd1 N7 -146(5) . . . . ? C34 N9 Pd1 N10 -178.8(5) . . . . ? C38 N9 Pd1 N10 8.6(6) . . . . ? C39 N10 Pd1 N8 73(7) . . . . ? C43 N10 Pd1 N8 -115(7) . . . . ? C39 N10 Pd1 N7 -79.8(4) . . . . ? C43 N10 Pd1 N7 92.9(5) . . . . ? C39 N10 Pd1 N9 101.3(4) . . . . ? C43 N10 Pd1 N9 -86.0(5) . . . . ? C23 N6 Pt1 N11 116.9(6) . . . 2_666 ? N5 N6 Pt1 N11 -62.0(4) . . . 2_666 ? C23 N6 Pt1 N2 -67(5) . . . . ? N5 N6 Pt1 N2 114(5) . . . . ? C23 N6 Pt1 N1 -62.0(6) . . . . ? N5 N6 Pt1 N1 119.1(4) . . . . ? C23 N6 Pt1 Pt2 178.1(6) . . . . ? N5 N6 Pt1 Pt2 -0.8(3) . . . . ? C6 N2 Pt1 N6 5(5) . . . . ? C10 N2 Pt1 N6 -171(4) . . . . ? C6 N2 Pt1 N11 -179.0(5) . . . 2_666 ? C10 N2 Pt1 N11 4.9(5) . . . 2_666 ? C6 N2 Pt1 N1 -0.1(4) . . . . ? C10 N2 Pt1 N1 -176.2(5) . . . . ? C6 N2 Pt1 Pt2 118.5(4) . . . . ? C10 N2 Pt1 Pt2 -57.6(5) . . . . ? C1 N1 Pt1 N6 -3.1(5) . . . . ? C5 N1 Pt1 N6 179.4(4) . . . . ? C1 N1 Pt1 N11 -138(8) . . . 2_666 ? C5 N1 Pt1 N11 45(8) . . . 2_666 ? C1 N1 Pt1 N2 176.6(5) . . . . ? C5 N1 Pt1 N2 -0.8(4) . . . . ? C1 N1 Pt1 Pt2 59.3(5) . . . . ? C5 N1 Pt1 Pt2 -118.2(4) . . . . ? C21 N5 Pt2 N12 -115.1(6) . . . 2_666 ? N6 N5 Pt2 N12 63.3(4) . . . 2_666 ? C21 N5 Pt2 N3 105(6) . . . . ? N6 N5 Pt2 N3 -76(6) . . . . ? C21 N5 Pt2 N4 68.0(6) . . . . ? N6 N5 Pt2 N4 -113.6(4) . . . . ? C21 N5 Pt2 Pt1 -179.3(7) . . . . ? N6 N5 Pt2 Pt1 -0.8(3) . . . . ? C15 N3 Pt2 N5 -39(6) . . . . ? C11 N3 Pt2 N5 139(5) . . . . ? C15 N3 Pt2 N12 -178.9(4) . . . 2_666 ? C11 N3 Pt2 N12 -0.2(6) . . . 2_666 ? C15 N3 Pt2 N4 -1.9(4) . . . . ? C11 N3 Pt2 N4 176.8(6) . . . . ? C15 N3 Pt2 Pt1 -113.8(4) . . . . ? C11 N3 Pt2 Pt1 64.9(6) . . . . ? C16 N4 Pt2 N5 178.6(5) . . . . ? C20 N4 Pt2 N5 5.6(6) . . . . ? C16 N4 Pt2 N12 47(3) . . . 2_666 ? C20 N4 Pt2 N12 -126(3) . . . 2_666 ? C16 N4 Pt2 N3 0.0(5) . . . . ? C20 N4 Pt2 N3 -173.0(6) . . . . ? C16 N4 Pt2 Pt1 113.9(5) . . . . ? C20 N4 Pt2 Pt1 -59.1(6) . . . . ? N6 Pt1 Pt2 N5 0.6(2) . . . . ? N11 Pt1 Pt2 N5 99.5(2) 2_666 . . . ? N2 Pt1 Pt2 N5 -176.6(2) . . . . ? N1 Pt1 Pt2 N5 -81.0(2) . . . . ? N6 Pt1 Pt2 N12 -97.5(2) . . . 2_666 ? N11 Pt1 Pt2 N12 1.4(2) 2_666 . . 2_666 ? N2 Pt1 Pt2 N12 85.3(2) . . . 2_666 ? N1 Pt1 Pt2 N12 -179.1(2) . . . 2_666 ? N6 Pt1 Pt2 N3 178.2(2) . . . . ? N11 Pt1 Pt2 N3 -83.0(2) 2_666 . . . ? N2 Pt1 Pt2 N3 0.9(2) . . . . ? N1 Pt1 Pt2 N3 96.5(2) . . . . ? N6 Pt1 Pt2 N4 86.7(2) . . . . ? N11 Pt1 Pt2 N4 -174.5(2) 2_666 . . . ? N2 Pt1 Pt2 N4 -90.6(2) . . . . ? N1 Pt1 Pt2 N4 5.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.416 _refine_diff_density_min -1.429 _refine_diff_density_rms 0.111 # Attachment '- C4.cif' data_tj _database_code_depnum_ccdc_archive 'CCDC 867312' #TrackingRef '- C4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H36 N10 Pd2), 4(N O3), 5(H2 O)' _chemical_formula_sum 'C80 H82 N24 O17 Pd4' _chemical_formula_weight 2077.30 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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.397(3) _cell_length_b 16.610(3) _cell_length_c 22.239(4) _cell_angle_alpha 86.15(3) _cell_angle_beta 89.18(2) _cell_angle_gamma 89.19(3) _cell_volume 4936.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4715 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 24.79 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7 _exptl_absorpt_correction_T_max 0.8 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58300 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 19403 _reflns_number_gt 16512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.07P)^2^+1.99P] 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 19403 _refine_ls_number_parameters 1206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 C1 C 0.2218(3) -0.0851(2) 0.25124(19) 0.0360(9) Uani 1 1 d . . . H1 H 0.2477 -0.0486 0.2218 0.043 Uiso 1 1 calc R . . C2 C 0.2546(3) -0.1641(2) 0.25315(19) 0.0371(9) Uani 1 1 d . . . H2 H 0.2998 -0.1812 0.2244 0.045 Uiso 1 1 calc R . . C3 C 0.2180(3) -0.2191(2) 0.30011(18) 0.0332(8) Uani 1 1 d . . . H3 H 0.2436 -0.2714 0.3059 0.040 Uiso 1 1 calc R . . C4 C 0.1399(3) -0.1898(2) 0.33777(19) 0.0384(9) Uani 1 1 d . . . H4 H 0.1030 -0.2264 0.3622 0.046 Uiso 1 1 calc R . . C5 C 0.1201(4) -0.1155(2) 0.3386(2) 0.0474(11) Uani 1 1 d . . . C6 C 0.0337(3) -0.0794(2) 0.37143(16) 0.0306(8) Uani 1 1 d . . . C7 C -0.0175(3) -0.1236(2) 0.41289(18) 0.0349(9) Uani 1 1 d . . . H7 H 0.0022 -0.1766 0.4229 0.042 Uiso 1 1 calc R . . C8 C -0.1045(3) -0.0895(3) 0.4428(2) 0.0447(10) Uani 1 1 d . . . H8 H -0.1458 -0.1206 0.4687 0.054 Uiso 1 1 calc R . . C9 C -0.1210(3) -0.0092(3) 0.43021(18) 0.0401(10) Uani 1 1 d . . . H9 H -0.1736 0.0165 0.4492 0.048 Uiso 1 1 calc R . . C10 C -0.0615(3) 0.0341(3) 0.39005(18) 0.0404(10) Uani 1 1 d . . . H10 H -0.0741 0.0892 0.3835 0.048 Uiso 1 1 calc R . . C11 C 0.0631(3) 0.0012(2) 0.09723(16) 0.0287(7) Uani 1 1 d . . . H11 H 0.1274 0.0183 0.1044 0.034 Uiso 1 1 calc R . . C12 C 0.0485(3) -0.0615(2) 0.05819(17) 0.0361(9) Uani 1 1 d . . . H12 H 0.1034 -0.0831 0.0386 0.043 Uiso 1 1 calc R . . C13 C -0.0443(3) -0.0909(2) 0.04852(17) 0.0347(9) Uani 1 1 d . . . H13 H -0.0531 -0.1337 0.0243 0.042 Uiso 1 1 calc R . . C14 C -0.1277(3) -0.0531(2) 0.07725(16) 0.0313(8) Uani 1 1 d . . . H14 H -0.1925 -0.0688 0.0700 0.038 Uiso 1 1 calc R . . C15 C -0.1106(3) 0.0064(2) 0.11552(16) 0.0280(7) Uani 1 1 d . . . C16 C -0.1895(3) 0.0437(3) 0.1512(2) 0.0422(10) Uani 1 1 d . . . C17 C -0.2848(3) 0.0210(2) 0.15324(19) 0.0377(9) Uani 1 1 d . . . H17 H -0.3046 -0.0200 0.1297 0.045 Uiso 1 1 calc R . . C18 C -0.3556(3) 0.0575(3) 0.18997(19) 0.0424(10) Uani 1 1 d . . . H18 H -0.4226 0.0440 0.1886 0.051 Uiso 1 1 calc R . . C19 C -0.3237(3) 0.1147(3) 0.22882(19) 0.0390(9) Uani 1 1 d . . . H19 H -0.3671 0.1395 0.2551 0.047 Uiso 1 1 calc R . . C20 C -0.2189(3) 0.1320(2) 0.22497(19) 0.0361(9) Uani 1 1 d . . . H20 H -0.1944 0.1696 0.2500 0.043 Uiso 1 1 calc R . . C21 C 0.3659(3) 0.0897(3) 0.26475(19) 0.0403(10) Uani 1 1 d . . . H21A H 0.3346 0.0600 0.2983 0.060 Uiso 1 1 calc R . . H21B H 0.4010 0.1345 0.2789 0.060 Uiso 1 1 calc R . . H21C H 0.4120 0.0550 0.2451 0.060 Uiso 1 1 calc R . . C22 C 0.2888(3) 0.1197(2) 0.22152(17) 0.0320(8) Uani 1 1 d . . . C23 C 0.3027(3) 0.1591(2) 0.16413(16) 0.0299(8) Uani 1 1 d . . . C24 C 0.2135(3) 0.1654(3) 0.13981(18) 0.0374(9) Uani 1 1 d . . . C25 C 0.1720(3) 0.2065(3) 0.08186(17) 0.0380(9) Uani 1 1 d . . . H25A H 0.2053 0.2567 0.0728 0.057 Uiso 1 1 calc R . . H25B H 0.1017 0.2165 0.0870 0.057 Uiso 1 1 calc R . . H25C H 0.1827 0.1721 0.0493 0.057 Uiso 1 1 calc R . . C26 C 0.5289(3) 0.1747(3) 0.05984(18) 0.0390(9) Uani 1 1 d . . . H26 H 0.5519 0.1551 0.0239 0.047 Uiso 1 1 calc R . . C27 C 0.4321(3) 0.1578(2) 0.08205(16) 0.0304(8) Uani 1 1 d . . . H27 H 0.3887 0.1292 0.0594 0.036 Uiso 1 1 calc R . . C28 C 0.4006(3) 0.1837(3) 0.13774(16) 0.0352(9) Uani 1 1 d . . . C29 C 0.4653(3) 0.2299(2) 0.17055(18) 0.0342(9) Uani 1 1 d . . . H29 H 0.4458 0.2472 0.2079 0.041 Uiso 1 1 calc R . . C30 C 0.5588(3) 0.2491(2) 0.14607(18) 0.0363(9) Uani 1 1 d . . . H30 H 0.6012 0.2814 0.1664 0.044 Uiso 1 1 calc R . . C31 C 0.0820(3) 0.2108(3) 0.40194(17) 0.0369(9) Uani 1 1 d . . . H31A H 0.1129 0.1583 0.4056 0.055 Uiso 1 1 calc R . . H31B H 0.0305 0.2142 0.4322 0.055 Uiso 1 1 calc R . . H31C H 0.1312 0.2511 0.4073 0.055 Uiso 1 1 calc R . . C32 C 0.0376(3) 0.2247(2) 0.34117(16) 0.0288(7) Uani 1 1 d . . . C33 C -0.0115(3) 0.2911(2) 0.31453(18) 0.0328(8) Uani 1 1 d . . . C34 C -0.0406(3) 0.2742(2) 0.25810(16) 0.0277(7) Uani 1 1 d . . . C35 C -0.0897(3) 0.3178(2) 0.20641(19) 0.0387(9) Uani 1 1 d . . . H35A H -0.1579 0.3294 0.2168 0.058 Uiso 1 1 calc R . . H35B H -0.0875 0.2850 0.1725 0.058 Uiso 1 1 calc R . . H35C H -0.0555 0.3674 0.1963 0.058 Uiso 1 1 calc R . . C36 C 0.0076(3) 0.4694(2) 0.4121(2) 0.0386(9) Uani 1 1 d . . . H36 H 0.0503 0.4882 0.4405 0.046 Uiso 1 1 calc R . . C37 C 0.0290(3) 0.3951(2) 0.3847(2) 0.0384(9) Uani 1 1 d . . . H37 H 0.0870 0.3658 0.3941 0.046 Uiso 1 1 calc R . . C38 C -0.0373(3) 0.3680(2) 0.34426(18) 0.0354(9) Uani 1 1 d . . . C39 C -0.1221(3) 0.4116(2) 0.32898(19) 0.0348(9) Uani 1 1 d . . . H39 H -0.1658 0.3937 0.3008 0.042 Uiso 1 1 calc R . . C40 C -0.1424(4) 0.4871(3) 0.3580(2) 0.0442(10) Uani 1 1 d . . . H40 H -0.2002 0.5173 0.3500 0.053 Uiso 1 1 calc R . . C41 C 0.5449(3) 0.5321(2) 0.39033(17) 0.0342(8) Uani 1 1 d . . . H41 H 0.5593 0.5858 0.3797 0.041 Uiso 1 1 calc R . . C42 C 0.6031(3) 0.4889(3) 0.43317(18) 0.0381(9) Uani 1 1 d . . . H42 H 0.6520 0.5148 0.4537 0.046 Uiso 1 1 calc R . . C43 C 0.5875(3) 0.4077(2) 0.44485(16) 0.0339(8) Uani 1 1 d . . . H43 H 0.6293 0.3770 0.4707 0.041 Uiso 1 1 calc R . . C44 C 0.5073(3) 0.3717(2) 0.41706(17) 0.0272(7) Uani 1 1 d . . . H44 H 0.4925 0.3176 0.4257 0.033 Uiso 1 1 calc R . . C45 C 0.4514(3) 0.4194(2) 0.37660(15) 0.0288(8) Uani 1 1 d . . . C46 C 0.3711(3) 0.3826(2) 0.34038(17) 0.0291(8) Uani 1 1 d . . . C47 C 0.3421(3) 0.3028(2) 0.3466(2) 0.0424(10) Uani 1 1 d . . . H47 H 0.3678 0.2678 0.3770 0.051 Uiso 1 1 calc R . . C48 C 0.2744(4) 0.2765(3) 0.3067(2) 0.0418(10) Uani 1 1 d . . . H48 H 0.2559 0.2226 0.3097 0.050 Uiso 1 1 calc R . . C49 C 0.2334(3) 0.3279(2) 0.26241(18) 0.0336(8) Uani 1 1 d . . . H49 H 0.1870 0.3104 0.2356 0.040 Uiso 1 1 calc R . . C50 C 0.2650(3) 0.4077(2) 0.25995(18) 0.0334(8) Uani 1 1 d . . . H50 H 0.2406 0.4431 0.2293 0.040 Uiso 1 1 calc R . . C51 C 0.7038(3) 0.6218(2) 0.22144(17) 0.0316(8) Uani 1 1 d . . . H51 H 0.6808 0.6610 0.2464 0.038 Uiso 1 1 calc R . . C52 C 0.8051(3) 0.6010(2) 0.22272(18) 0.0365(9) Uani 1 1 d . . . H52 H 0.8479 0.6228 0.2498 0.044 Uiso 1 1 calc R . . C53 C 0.8398(4) 0.5465(3) 0.1819(2) 0.0489(11) Uani 1 1 d . . . H53 H 0.9075 0.5339 0.1788 0.059 Uiso 1 1 calc R . . C54 C 0.7733(3) 0.5128(2) 0.14739(18) 0.0337(9) Uani 1 1 d . . . H54 H 0.7952 0.4741 0.1217 0.040 Uiso 1 1 calc R . . C55 C 0.6754(3) 0.5333(2) 0.14856(16) 0.0313(8) Uani 1 1 d . . . C56 C 0.5950(3) 0.4975(2) 0.11337(17) 0.0316(8) Uani 1 1 d . . . C57 C 0.6108(3) 0.4353(2) 0.07379(18) 0.0351(9) Uani 1 1 d . . . H57 H 0.6750 0.4145 0.0688 0.042 Uiso 1 1 calc R . . C58 C 0.5369(3) 0.4061(2) 0.04383(19) 0.0372(9) Uani 1 1 d . . . H58 H 0.5505 0.3710 0.0138 0.045 Uiso 1 1 calc R . . C59 C 0.4339(3) 0.4287(2) 0.05744(17) 0.0336(8) Uani 1 1 d . . . H59 H 0.3807 0.4027 0.0410 0.040 Uiso 1 1 calc R . . C60 C 0.4181(3) 0.4906(2) 0.09607(15) 0.0315(8) Uani 1 1 d . . . H60 H 0.3542 0.5104 0.1036 0.038 Uiso 1 1 calc R . . C61 C 0.3985(3) 0.7021(3) 0.40220(18) 0.0408(10) Uani 1 1 d . . . H61A H 0.3903 0.6451 0.4104 0.061 Uiso 1 1 calc R . . H61B H 0.3348 0.7290 0.4051 0.061 Uiso 1 1 calc R . . H61C H 0.4430 0.7220 0.4310 0.061 Uiso 1 1 calc R . . C62 C 0.4428(3) 0.71886(19) 0.33743(15) 0.0270(8) Uani 1 1 d . . . C63 C 0.4947(3) 0.7846(2) 0.31122(17) 0.0320(8) Uani 1 1 d . . . C64 C 0.5223(3) 0.76405(19) 0.25301(16) 0.0233(7) Uani 1 1 d . . . C65 C 0.5714(3) 0.8078(2) 0.20429(18) 0.0350(9) Uani 1 1 d . . . H65A H 0.5796 0.7740 0.1712 0.053 Uiso 1 1 calc R . . H65B H 0.6357 0.8243 0.2170 0.053 Uiso 1 1 calc R . . H65C H 0.5320 0.8545 0.1918 0.053 Uiso 1 1 calc R . . C66 C 0.4908(3) 0.9616(3) 0.40955(17) 0.0374(9) Uani 1 1 d . . . H66 H 0.4500 0.9835 0.4386 0.045 Uiso 1 1 calc R . . C67 C 0.4627(3) 0.8939(2) 0.38342(17) 0.0324(8) Uani 1 1 d . . . H67 H 0.4023 0.8703 0.3951 0.039 Uiso 1 1 calc R . . C68 C 0.5213(3) 0.8589(2) 0.33981(16) 0.0293(8) Uani 1 1 d . . . C69 C 0.6128(3) 0.8982(2) 0.32652(17) 0.0315(8) Uani 1 1 d . . . H69 H 0.6573 0.8771 0.2991 0.038 Uiso 1 1 calc R . . C70 C 0.6353(3) 0.9634(2) 0.35216(18) 0.0357(9) Uani 1 1 d . . . H70 H 0.6951 0.9887 0.3414 0.043 Uiso 1 1 calc R . . C71 C 0.1182(3) 0.5855(2) 0.27152(16) 0.0318(8) Uani 1 1 d . . . H71A H 0.1497 0.5507 0.3021 0.048 Uiso 1 1 calc R . . H71B H 0.0669 0.5565 0.2528 0.048 Uiso 1 1 calc R . . H71C H 0.0890 0.6314 0.2895 0.048 Uiso 1 1 calc R . . C72 C 0.1924(3) 0.6127(2) 0.22618(15) 0.0242(7) Uani 1 1 d . . . C73 C 0.1779(3) 0.6517(2) 0.16611(15) 0.0252(7) Uani 1 1 d . . . C74 C 0.2785(3) 0.6600(2) 0.14129(16) 0.0336(9) Uani 1 1 d . . . C75 C 0.3108(3) 0.6959(3) 0.08016(17) 0.0389(9) Uani 1 1 d . . . H75A H 0.3813 0.7056 0.0801 0.058 Uiso 1 1 calc R . . H75B H 0.2755 0.7458 0.0713 0.058 Uiso 1 1 calc R . . H75C H 0.2963 0.6590 0.0501 0.058 Uiso 1 1 calc R . . C76 C -0.0735(3) 0.7457(3) 0.14788(18) 0.0365(9) Uani 1 1 d . . . H76 H -0.1168 0.7787 0.1686 0.044 Uiso 1 1 calc R . . C77 C 0.0184(3) 0.7225(2) 0.17206(17) 0.0311(8) Uani 1 1 d . . . H77 H 0.0344 0.7386 0.2100 0.037 Uiso 1 1 calc R . . C78 C 0.0886(3) 0.6754(2) 0.14119(16) 0.0294(8) Uani 1 1 d . . . C79 C 0.0575(3) 0.6514(3) 0.08243(16) 0.0330(8) Uani 1 1 d . . . H79 H 0.1004 0.6208 0.0596 0.040 Uiso 1 1 calc R . . C80 C -0.0345(3) 0.6736(3) 0.06078(17) 0.0340(9) Uani 1 1 d . . . H80 H -0.0537 0.6575 0.0234 0.041 Uiso 1 1 calc R . . N1 N 0.1519(2) -0.05843(18) 0.29151(15) 0.0316(7) Uani 1 1 d . . . N2 N 0.0156(2) 0.0009(2) 0.35902(14) 0.0335(7) Uani 1 1 d . . . N3 N -0.0150(2) 0.03581(18) 0.12377(14) 0.0292(6) Uani 1 1 d . . . N4 N -0.1566(2) 0.09895(18) 0.18920(14) 0.0277(6) Uani 1 1 d . . . N5 N 0.1908(2) 0.10365(19) 0.22998(14) 0.0297(7) Uani 1 1 d . . . N6 N 0.1420(2) 0.13547(18) 0.17938(13) 0.0268(6) Uani 1 1 d . . . N7 N 0.5882(2) 0.2211(2) 0.09296(15) 0.0335(7) Uani 1 1 d . . . N8 N 0.0407(2) 0.16657(16) 0.30056(13) 0.0231(6) Uani 1 1 d . . . N9 N -0.0055(2) 0.19685(17) 0.24856(14) 0.0286(6) Uani 1 1 d . . . N10 N -0.0747(3) 0.5106(2) 0.39606(14) 0.0370(8) Uani 1 1 d . . . N11 N 0.4689(2) 0.49737(18) 0.36436(13) 0.0268(6) Uani 1 1 d . . . N12 N 0.3271(2) 0.43602(18) 0.29820(15) 0.0304(7) Uani 1 1 d . . . N13 N 0.6369(2) 0.58771(19) 0.18565(14) 0.0300(7) Uani 1 1 d . . . N14 N 0.5031(3) 0.5224(2) 0.12352(14) 0.0366(8) Uani 1 1 d . . . N15 N 0.4390(2) 0.66134(17) 0.30124(12) 0.0230(6) Uani 1 1 d . . . N16 N 0.4848(2) 0.68789(17) 0.24752(13) 0.0255(6) Uani 1 1 d . . . N17 N 0.5762(3) 0.99600(19) 0.39358(15) 0.0353(7) Uani 1 1 d . . . N18 N 0.2931(2) 0.59566(17) 0.23183(12) 0.0237(6) Uani 1 1 d . . . N19 N 0.3405(2) 0.62428(19) 0.18051(13) 0.0293(7) Uani 1 1 d . . . N20 N -0.0995(2) 0.7196(2) 0.09354(16) 0.0368(8) Uani 1 1 d . . . N21 N 0.2756(3) 0.0559(2) 0.43451(16) 0.0406(8) Uani 1 1 d . . . N22 N 0.6121(3) 0.3815(2) 0.26184(14) 0.0375(8) Uani 1 1 d . . . N23 N 0.1984(3) 0.5757(2) 0.44409(15) 0.0376(8) Uani 1 1 d . . . N24 N 0.8669(2) 0.8950(2) 0.25541(14) 0.0309(7) Uani 1 1 d . . . O1 O 0.3157(2) 0.04175(17) 0.48634(13) 0.0375(6) Uani 1 1 d . . . O2 O 0.3026(2) 0.11802(16) 0.40697(12) 0.0370(6) Uani 1 1 d . . . O3 O 0.2116(2) 0.00928(18) 0.42020(14) 0.0469(7) Uani 1 1 d . . . O4 O 0.5354(2) 0.39417(18) 0.23440(13) 0.0426(7) Uani 1 1 d . . . O5 O 0.6589(2) 0.31615(17) 0.26587(13) 0.0378(6) Uani 1 1 d . . . O6 O 0.6555(3) 0.43990(19) 0.28429(15) 0.0505(8) Uani 1 1 d . . . O7 O 0.1782(2) 0.63281(19) 0.40815(14) 0.0451(7) Uani 1 1 d . . . O8 O 0.2434(2) 0.51824(17) 0.42103(13) 0.0372(6) Uani 1 1 d . . . O9 O 0.1741(2) 0.56809(17) 0.49645(13) 0.0396(7) Uani 1 1 d . . . O10 O 0.8007(2) 0.84512(18) 0.23982(14) 0.0458(8) Uani 1 1 d . . . O11 O 0.8386(2) 0.95263(18) 0.27965(13) 0.0425(7) Uani 1 1 d . . . O12 O 0.9488(2) 0.88208(18) 0.24031(13) 0.0393(7) Uani 1 1 d . . . O1W O 0.9184(4) 0.2122(4) 0.0446(3) 0.0272(13) Uani 0.40 1 d P . . H1X H 0.8664 0.1900 0.0601 0.033 Uiso 0.40 1 d PR . . H1Y H 0.9087 0.2629 0.0399 0.033 Uiso 0.40 1 d PR . . O2W O 0.2493(5) 0.8567(4) 0.4684(3) 0.0406(17) Uani 0.40 1 d P . . H2X H 0.1911 0.8635 0.4540 0.049 Uiso 0.40 1 d PR . . H2Y H 0.2450 0.8367 0.5045 0.049 Uiso 0.40 1 d PR . . O3W O 0.5712(5) 0.7164(4) 0.0492(3) 0.0365(16) Uani 0.40 1 d P . . H3X H 0.5453 0.7275 0.0828 0.044 Uiso 0.40 1 d PR . . H3Y H 0.6339 0.7101 0.0530 0.044 Uiso 0.40 1 d PR . . O4W O 0.4351(5) 0.1963(3) 0.4798(3) 0.0303(14) Uani 0.40 1 d P . . H4X H 0.4673 0.2094 0.5102 0.036 Uiso 0.40 1 d PR . . H4Y H 0.3732 0.1941 0.4887 0.036 Uiso 0.40 1 d PR . . O5W O 0.6321(5) 0.6961(4) 0.4379(3) 0.0353(15) Uani 0.40 1 d P . . H5X H 0.6454 0.7126 0.4722 0.042 Uiso 0.40 1 d PR . . H5Y H 0.6842 0.6986 0.4156 0.042 Uiso 0.40 1 d PR . . O6W O 0.7380(6) 0.2276(5) 0.3642(4) 0.0455(18) Uani 0.40 1 d P . . H6X H 0.7910 0.2246 0.3429 0.055 Uiso 0.40 1 d PR . . H6Y H 0.7448 0.1987 0.3969 0.055 Uiso 0.40 1 d PR . . O7W O 0.9289(5) 0.6497(4) 0.4523(3) 0.0351(15) Uani 0.40 1 d P . . H7X H 0.9918 0.6473 0.4565 0.042 Uiso 0.40 1 d PR . . H7Y H 0.9013 0.6615 0.4853 0.042 Uiso 0.40 1 d PR . . O8W O 0.5941(6) 0.9180(4) 0.0573(3) 0.0401(17) Uani 0.40 1 d P . . H8X H 0.5762 0.8698 0.0666 0.048 Uiso 0.40 1 d PR . . H8Y H 0.5453 0.9501 0.0630 0.048 Uiso 0.40 1 d PR . . O9W O 0.2802(5) 1.0058(4) 0.0360(3) 0.0392(17) Uani 0.40 1 d P . . H9X H 0.2540 0.9604 0.0458 0.047 Uiso 0.40 1 d PR . . H9Y H 0.3434 1.0012 0.0373 0.047 Uiso 0.40 1 d PR . . O10W O 0.9346(6) 0.7134(5) 0.3200(3) 0.050(2) Uani 0.40 1 d P . . H10X H 0.9710 0.6927 0.3481 0.059 Uiso 0.40 1 d PR . . H10Y H 0.8952 0.7482 0.3341 0.059 Uiso 0.40 1 d PR . . O11W O 0.8966(6) 0.4125(4) 0.0538(3) 0.0427(17) Uani 0.40 1 d P . . H11X H 0.9463 0.4194 0.0299 0.051 Uiso 0.40 1 d PR . . H11Y H 0.8429 0.4223 0.0346 0.051 Uiso 0.40 1 d PR . . O12W O 0.4004(7) 0.9533(6) 0.1405(4) 0.036(2) Uani 0.30 1 d P . . H12X H 0.3558 0.9585 0.1137 0.043 Uiso 0.30 1 d PR . . H12Y H 0.4354 0.9957 0.1393 0.043 Uiso 0.30 1 d PR . . O13W O 0.1830(7) 0.4340(6) 0.1105(4) 0.041(2) Uani 0.30 1 d P . . H13X H 0.1200 0.4329 0.1154 0.049 Uiso 0.30 1 d PR . . H13Y H 0.1985 0.4184 0.0760 0.049 Uiso 0.30 1 d PR . . Pd1 Pd 0.103266(19) 0.055361(15) 0.296763(11) 0.02245(7) Uani 1 1 d . . . Pd2 Pd -0.007919(18) 0.120664(14) 0.182913(11) 0.01905(7) Uani 1 1 d . . . Pd3 Pd 0.379192(18) 0.550271(15) 0.299288(11) 0.02026(7) Uani 1 1 d . . . Pd4 Pd 0.490801(19) 0.610348(14) 0.182592(11) 0.02141(7) 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 0.042(2) 0.0253(18) 0.042(2) -0.0141(16) 0.0101(18) -0.0044(16) C2 0.038(2) 0.0299(19) 0.045(2) -0.0162(17) 0.0079(18) 0.0042(16) C3 0.0251(19) 0.033(2) 0.042(2) -0.0038(16) -0.0115(16) -0.0002(15) C4 0.040(2) 0.0273(19) 0.047(2) 0.0047(17) 0.0085(18) -0.0107(16) C5 0.063(3) 0.0223(19) 0.057(3) -0.0073(18) 0.020(2) -0.0168(19) C6 0.031(2) 0.0330(19) 0.0270(18) 0.0089(15) -0.0056(15) -0.0017(15) C7 0.032(2) 0.032(2) 0.039(2) 0.0095(16) -0.0039(16) -0.0010(16) C8 0.032(2) 0.054(3) 0.047(2) 0.003(2) 0.0083(18) -0.0141(19) C9 0.037(2) 0.047(2) 0.034(2) 0.0031(17) 0.0181(17) -0.0011(18) C10 0.040(2) 0.044(2) 0.035(2) 0.0022(17) 0.0215(18) 0.0026(18) C11 0.032(2) 0.0290(18) 0.0255(17) -0.0035(14) 0.0008(14) -0.0036(15) C12 0.039(2) 0.037(2) 0.034(2) -0.0167(16) 0.0077(17) -0.0091(17) C13 0.043(2) 0.0322(19) 0.0291(18) 0.0011(15) 0.0044(16) -0.0223(17) C14 0.031(2) 0.0302(19) 0.0314(19) 0.0084(15) -0.0026(15) -0.0120(15) C15 0.0315(19) 0.0201(16) 0.0318(18) 0.0043(13) -0.0058(15) -0.0068(14) C16 0.035(2) 0.042(2) 0.050(2) -0.0039(19) 0.0034(18) -0.0154(18) C17 0.032(2) 0.035(2) 0.046(2) -0.0023(17) -0.0089(17) -0.0086(17) C18 0.036(2) 0.048(2) 0.042(2) 0.0108(19) -0.0004(18) -0.0094(19) C19 0.030(2) 0.043(2) 0.044(2) -0.0004(18) 0.0107(17) -0.0031(17) C20 0.028(2) 0.034(2) 0.044(2) 0.0132(17) 0.0062(17) 0.0053(16) C21 0.0208(19) 0.053(3) 0.046(2) 0.0016(19) 0.0077(16) 0.0133(17) C22 0.0210(18) 0.045(2) 0.0293(18) 0.0000(16) 0.0071(14) -0.0079(16) C23 0.0246(18) 0.036(2) 0.0288(18) -0.0017(15) 0.0099(14) -0.0083(15) C24 0.0219(18) 0.050(2) 0.038(2) 0.0163(18) 0.0041(16) -0.0152(17) C25 0.044(2) 0.039(2) 0.0294(19) 0.0110(16) 0.0001(17) -0.0090(18) C26 0.042(2) 0.047(2) 0.0269(19) 0.0048(16) 0.0143(17) -0.0126(19) C27 0.034(2) 0.0280(18) 0.0279(18) 0.0084(14) 0.0110(15) -0.0096(15) C28 0.031(2) 0.051(2) 0.0228(17) 0.0069(16) 0.0082(15) -0.0142(17) C29 0.036(2) 0.0261(18) 0.041(2) -0.0013(15) 0.0101(17) -0.0152(16) C30 0.031(2) 0.039(2) 0.037(2) 0.0069(17) 0.0025(16) -0.0092(17) C31 0.042(2) 0.041(2) 0.0285(19) -0.0077(16) -0.0098(16) 0.0104(18) C32 0.0285(19) 0.0324(19) 0.0257(17) -0.0048(14) 0.0001(14) 0.0052(15) C33 0.033(2) 0.0296(19) 0.036(2) -0.0074(15) -0.0012(16) 0.0049(15) C34 0.033(2) 0.0189(16) 0.0302(18) 0.0002(13) 0.0018(15) 0.0053(14) C35 0.039(2) 0.029(2) 0.047(2) 0.0004(17) -0.0130(18) 0.0078(17) C36 0.036(2) 0.0229(18) 0.058(3) -0.0074(17) 0.0011(19) -0.0134(16) C37 0.034(2) 0.031(2) 0.051(2) -0.0101(17) 0.0124(18) -0.0019(16) C38 0.050(2) 0.0210(17) 0.035(2) -0.0011(14) 0.0111(18) 0.0014(16) C39 0.0239(19) 0.034(2) 0.046(2) -0.0076(17) 0.0207(16) 0.0010(15) C40 0.050(3) 0.035(2) 0.048(2) -0.0038(18) -0.006(2) 0.0191(19) C41 0.038(2) 0.035(2) 0.0306(19) -0.0097(15) -0.0165(16) 0.0045(16) C42 0.037(2) 0.046(2) 0.031(2) 0.0039(17) -0.0142(17) -0.0085(18) C43 0.039(2) 0.044(2) 0.0177(16) 0.0077(15) 0.0045(15) -0.0101(17) C44 0.0213(17) 0.0198(16) 0.040(2) -0.0006(14) 0.0044(14) 0.0112(13) C45 0.0305(19) 0.0297(18) 0.0239(17) 0.0157(14) 0.0014(14) -0.0053(15) C46 0.0263(18) 0.0273(18) 0.0331(19) 0.0035(14) -0.0021(15) -0.0014(14) C47 0.054(3) 0.0216(18) 0.051(2) 0.0098(17) -0.021(2) -0.0001(17) C48 0.052(3) 0.030(2) 0.044(2) -0.0097(17) -0.0006(19) -0.0051(18) C49 0.0265(19) 0.033(2) 0.043(2) -0.0159(16) -0.0092(16) 0.0066(15) C50 0.034(2) 0.0266(18) 0.040(2) -0.0087(15) -0.0099(16) -0.0020(15) C51 0.0291(19) 0.035(2) 0.0286(18) 0.0153(15) -0.0033(15) -0.0031(15) C52 0.034(2) 0.042(2) 0.0313(19) 0.0169(16) -0.0078(16) 0.0050(17) C53 0.042(3) 0.057(3) 0.046(3) 0.012(2) -0.003(2) 0.014(2) C54 0.040(2) 0.0193(16) 0.039(2) 0.0149(15) 0.0145(17) 0.0138(15) C55 0.036(2) 0.0300(19) 0.0266(18) 0.0062(14) 0.0129(15) 0.0088(15) C56 0.042(2) 0.0145(15) 0.037(2) 0.0002(14) 0.0143(17) 0.0031(14) C57 0.044(2) 0.0228(17) 0.038(2) -0.0014(15) 0.0119(17) 0.0058(16) C58 0.038(2) 0.033(2) 0.041(2) -0.0061(16) 0.0063(17) 0.0039(17) C59 0.041(2) 0.0299(19) 0.0311(19) -0.0087(15) -0.0029(16) 0.0082(16) C60 0.051(2) 0.0216(17) 0.0216(17) -0.0017(13) 0.0026(16) 0.0002(16) C61 0.046(2) 0.042(2) 0.034(2) -0.0047(17) 0.0179(18) -0.0093(19) C62 0.045(2) 0.0136(15) 0.0213(16) 0.0027(12) 0.0064(15) 0.0065(14) C63 0.038(2) 0.0219(17) 0.036(2) -0.0019(14) 0.0054(16) 0.0028(15) C64 0.0217(17) 0.0180(15) 0.0299(17) -0.0008(13) 0.0040(13) 0.0043(12) C65 0.032(2) 0.033(2) 0.040(2) -0.0057(16) 0.0098(16) -0.0089(16) C66 0.037(2) 0.052(2) 0.0240(18) -0.0111(16) 0.0119(16) -0.0084(18) C67 0.041(2) 0.0249(17) 0.0311(19) 0.0013(14) 0.0129(16) -0.0086(15) C68 0.037(2) 0.0201(16) 0.0299(18) 0.0012(13) 0.0090(15) 0.0018(14) C69 0.032(2) 0.0316(19) 0.0299(18) 0.0034(15) 0.0089(15) -0.0008(15) C70 0.0244(19) 0.040(2) 0.043(2) -0.0035(17) 0.0110(16) -0.0077(16) C71 0.0255(18) 0.039(2) 0.0289(18) 0.0146(15) -0.0001(15) 0.0057(15) C72 0.0202(16) 0.0269(17) 0.0252(17) 0.0004(13) -0.0043(13) 0.0020(13) C73 0.0250(18) 0.0246(17) 0.0247(17) 0.0090(13) -0.0027(13) 0.0002(13) C74 0.030(2) 0.043(2) 0.0263(18) 0.0064(15) 0.0046(15) 0.0222(16) C75 0.050(3) 0.040(2) 0.0247(19) 0.0085(16) 0.0023(17) 0.0145(19) C76 0.0229(18) 0.052(2) 0.033(2) 0.0087(17) 0.0086(15) 0.0032(17) C77 0.034(2) 0.0234(17) 0.0349(19) 0.0024(14) -0.0021(16) 0.0132(15) C78 0.032(2) 0.0335(19) 0.0219(16) 0.0040(14) -0.0053(14) 0.0094(15) C79 0.0181(17) 0.058(2) 0.0236(17) -0.0038(16) -0.0001(14) 0.0017(16) C80 0.0212(18) 0.055(2) 0.0242(17) 0.0104(16) -0.0012(14) -0.0007(16) N1 0.0344(17) 0.0223(15) 0.0385(17) -0.0059(12) 0.0031(14) 0.0025(13) N2 0.0309(17) 0.0415(18) 0.0257(15) 0.0136(13) 0.0102(13) -0.0018(14) N3 0.0289(16) 0.0261(15) 0.0335(16) -0.0086(12) -0.0027(13) 0.0012(12) N4 0.0220(15) 0.0286(15) 0.0318(16) 0.0044(12) 0.0015(12) -0.0063(12) N5 0.0173(14) 0.0345(16) 0.0357(17) 0.0095(13) 0.0059(12) -0.0079(12) N6 0.0227(15) 0.0296(15) 0.0267(15) 0.0099(12) 0.0051(12) -0.0097(12) N7 0.0239(16) 0.0401(18) 0.0345(17) 0.0129(14) 0.0036(13) -0.0031(13) N8 0.0236(14) 0.0196(13) 0.0260(14) 0.0000(11) 0.0024(11) -0.0013(11) N9 0.0352(17) 0.0200(14) 0.0305(15) 0.0008(12) -0.0038(13) -0.0003(12) N10 0.048(2) 0.0359(18) 0.0264(16) -0.0024(13) 0.0189(15) 0.0033(15) N11 0.0276(16) 0.0266(15) 0.0256(14) 0.0028(11) -0.0050(12) -0.0003(12) N12 0.0221(15) 0.0270(15) 0.0412(18) 0.0046(13) -0.0032(13) -0.0013(12) N13 0.0248(16) 0.0333(16) 0.0309(16) 0.0019(13) 0.0059(12) 0.0068(13) N14 0.047(2) 0.0355(18) 0.0283(16) -0.0091(13) -0.0017(14) 0.0094(15) N15 0.0244(15) 0.0225(14) 0.0218(13) 0.0019(11) -0.0005(11) -0.0027(11) N16 0.0287(16) 0.0208(14) 0.0264(15) 0.0010(11) 0.0041(12) -0.0007(12) N17 0.044(2) 0.0287(16) 0.0340(17) -0.0039(13) 0.0085(14) -0.0108(14) N18 0.0195(14) 0.0285(15) 0.0227(14) 0.0016(11) -0.0011(11) -0.0016(11) N19 0.0285(16) 0.0390(17) 0.0194(14) 0.0043(12) 0.0000(12) 0.0066(13) N20 0.0247(16) 0.0408(19) 0.0433(19) 0.0086(15) 0.0029(14) -0.0002(14) N21 0.040(2) 0.0384(19) 0.045(2) -0.0070(15) -0.0041(16) 0.0000(16) N22 0.047(2) 0.0379(19) 0.0279(16) -0.0033(13) -0.0079(15) 0.0025(16) N23 0.0380(19) 0.044(2) 0.0305(17) 0.0031(15) -0.0025(14) -0.0092(16) N24 0.0196(16) 0.0426(19) 0.0317(16) -0.0101(14) -0.0074(12) -0.0009(13) O1 0.0347(15) 0.0393(15) 0.0383(15) -0.0016(12) -0.0053(12) 0.0105(12) O2 0.0519(18) 0.0335(15) 0.0269(13) -0.0093(11) -0.0004(12) -0.0110(13) O3 0.053(2) 0.0392(16) 0.0476(18) 0.0057(13) -0.0124(15) -0.0085(14) O4 0.0490(18) 0.0416(16) 0.0365(15) 0.0043(12) -0.0135(13) -0.0015(13) O5 0.0348(15) 0.0356(15) 0.0424(16) 0.0010(12) 0.0110(12) -0.0011(12) O6 0.061(2) 0.0424(17) 0.0491(18) -0.0028(14) -0.0131(16) -0.0126(15) O7 0.0474(18) 0.0434(17) 0.0436(17) 0.0028(13) -0.0054(14) 0.0073(14) O8 0.0319(15) 0.0383(15) 0.0395(15) 0.0090(12) 0.0008(12) 0.0080(12) O9 0.0329(15) 0.0400(16) 0.0446(17) 0.0075(12) 0.0024(12) -0.0039(12) O10 0.0436(18) 0.0460(17) 0.0496(18) -0.0161(14) 0.0178(14) -0.0225(14) O11 0.0456(18) 0.0448(17) 0.0388(16) -0.0150(13) -0.0055(13) 0.0059(14) O12 0.0264(15) 0.0505(17) 0.0421(16) -0.0103(13) -0.0131(12) 0.0081(12) O1W 0.014(3) 0.030(3) 0.037(3) 0.002(3) 0.007(2) 0.003(2) O2W 0.031(4) 0.046(4) 0.046(4) -0.017(3) 0.007(3) -0.014(3) O3W 0.026(3) 0.053(4) 0.030(3) -0.001(3) -0.018(3) 0.002(3) O4W 0.042(4) 0.022(3) 0.028(3) -0.002(2) -0.013(3) -0.004(3) O5W 0.028(3) 0.048(4) 0.028(3) 0.009(3) 0.005(3) -0.001(3) O6W 0.044(4) 0.045(4) 0.050(4) -0.013(3) -0.021(3) -0.010(3) O7W 0.033(4) 0.031(3) 0.042(4) -0.005(3) -0.003(3) 0.006(3) O8W 0.055(5) 0.032(4) 0.032(4) 0.002(3) -0.001(3) 0.027(3) O9W 0.043(4) 0.045(4) 0.032(3) -0.017(3) 0.019(3) -0.027(3) O10W 0.046(5) 0.064(5) 0.038(4) 0.009(4) 0.013(3) -0.013(4) O11W 0.050(5) 0.037(4) 0.042(4) -0.015(3) -0.006(3) 0.014(3) O12W 0.041(5) 0.049(5) 0.021(4) -0.017(4) 0.011(4) -0.013(4) O13W 0.038(5) 0.042(5) 0.042(5) 0.002(4) 0.002(4) -0.017(4) Pd1 0.02315(14) 0.01988(13) 0.02393(13) 0.00082(9) 0.00345(10) -0.00082(10) Pd2 0.02010(13) 0.01473(12) 0.02194(13) 0.00231(9) 0.00183(9) -0.00576(9) Pd3 0.01804(13) 0.02134(13) 0.02089(13) 0.00272(9) -0.00210(9) -0.00018(9) Pd4 0.02371(14) 0.02001(13) 0.02015(13) 0.00009(9) 0.00112(10) 0.00456(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 C2 1.375(5) . ? C1 N1 1.376(5) . ? C1 H1 0.9300 . ? C2 C3 1.427(6) . ? C2 H2 0.9300 . ? C3 C4 1.431(6) . ? C3 H3 0.9300 . ? C4 C5 1.260(6) . ? C4 H4 0.9300 . ? C5 N1 1.429(5) . ? C5 C6 1.500(6) . ? C6 C7 1.328(5) . ? C6 N2 1.362(5) . ? C7 C8 1.459(6) . ? C7 H7 0.9300 . ? C8 C9 1.360(6) . ? C8 H8 0.9300 . ? C9 C10 1.364(5) . ? C9 H9 0.9300 . ? C10 N2 1.365(5) . ? C10 H10 0.9300 . ? C11 N3 1.335(5) . ? C11 C12 1.417(5) . ? C11 H11 0.9300 . ? C12 C13 1.367(5) . ? C12 H12 0.9300 . ? C13 C14 1.437(6) . ? C13 H13 0.9300 . ? C14 C15 1.371(5) . ? C14 H14 0.9300 . ? C15 N3 1.396(5) . ? C15 C16 1.468(6) . ? C16 C17 1.335(6) . ? C16 N4 1.370(5) . ? C17 C18 1.401(6) . ? C17 H17 0.9300 . ? C18 C19 1.401(6) . ? C18 H18 0.9300 . ? C19 C20 1.438(6) . ? C19 H19 0.9300 . ? C20 N4 1.287(5) . ? C20 H20 0.9300 . ? C21 C22 1.479(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N5 1.351(5) . ? C22 C23 1.406(5) . ? C23 C24 1.318(6) . ? C23 C28 1.480(5) . ? C24 N6 1.368(4) . ? C24 C25 1.526(5) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N7 1.370(5) . ? C26 C27 1.406(5) . ? C26 H26 0.9300 . ? C27 C28 1.396(5) . ? C27 H27 0.9300 . ? C28 C29 1.409(6) . ? C29 C30 1.391(5) . ? C29 H29 0.9300 . ? C30 N7 1.349(5) . ? C30 H30 0.9300 . ? C31 C32 1.487(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N8 1.365(5) . ? C32 C33 1.380(5) . ? C33 C34 1.367(5) . ? C33 C38 1.511(5) . ? C34 N9 1.391(4) . ? C34 C35 1.474(5) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N10 1.330(6) . ? C36 C37 1.436(5) . ? C36 H36 0.9300 . ? C37 C38 1.374(6) . ? C37 H37 0.9300 . ? C38 C39 1.373(6) . ? C39 C40 1.469(5) . ? C39 H39 0.9300 . ? C40 N10 1.330(6) . ? C40 H40 0.9300 . ? C41 N11 1.335(5) . ? C41 C42 1.394(5) . ? C41 H41 0.9300 . ? C42 C43 1.375(6) . ? C42 H42 0.9300 . ? C43 C44 1.407(5) . ? C43 H43 0.9300 . ? C44 C45 1.380(5) . ? C44 H44 0.9300 . ? C45 N11 1.329(5) . ? C45 C46 1.513(5) . ? C46 N12 1.380(5) . ? C46 C47 1.384(5) . ? C47 C48 1.373(6) . ? C47 H47 0.9300 . ? C48 C49 1.375(6) . ? C48 H48 0.9300 . ? C49 C50 1.395(5) . ? C49 H49 0.9300 . ? C50 N12 1.312(5) . ? C50 H50 0.9300 . ? C51 N13 1.361(5) . ? C51 C52 1.396(5) . ? C51 H51 0.9300 . ? C52 C53 1.395(7) . ? C52 H52 0.9300 . ? C53 C54 1.337(7) . ? C53 H53 0.9300 . ? C54 C55 1.351(5) . ? C54 H54 0.9300 . ? C55 N13 1.356(5) . ? C55 C56 1.494(6) . ? C56 N14 1.315(5) . ? C56 C57 1.414(5) . ? C57 C58 1.318(6) . ? C57 H57 0.9300 . ? C58 C59 1.457(6) . ? C58 H58 0.9300 . ? C59 C60 1.396(5) . ? C59 H59 0.9300 . ? C60 N14 1.424(5) . ? C60 H60 0.9300 . ? C61 C62 1.559(5) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 N15 1.292(4) . ? C62 C63 1.393(5) . ? C63 C64 1.404(5) . ? C63 C68 1.477(5) . ? C64 N16 1.382(4) . ? C64 C65 1.421(5) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 N17 1.320(5) . ? C66 C67 1.359(6) . ? C66 H66 0.9300 . ? C67 C68 1.391(5) . ? C67 H67 0.9300 . ? C68 C69 1.415(5) . ? C69 C70 1.299(6) . ? C69 H69 0.9300 . ? C70 N17 1.343(5) . ? C70 H70 0.9300 . ? C71 C72 1.461(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N18 1.380(4) . ? C72 C73 1.460(4) . ? C73 C78 1.367(5) . ? C73 C74 1.454(5) . ? C74 N19 1.319(5) . ? C74 C75 1.507(5) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 N20 1.362(6) . ? C76 C77 1.390(5) . ? C76 H76 0.9300 . ? C77 C78 1.415(5) . ? C77 H77 0.9300 . ? C78 C79 1.460(5) . ? C79 C80 1.366(5) . ? C79 H79 0.9300 . ? C80 N20 1.382(5) . ? C80 H80 0.9300 . ? N1 Pd1 2.001(3) . ? N2 Pd1 1.983(3) . ? N3 Pd2 1.995(3) . ? N4 Pd2 2.031(3) . ? N5 N6 1.380(4) . ? N5 Pd1 2.010(3) . ? N6 Pd2 2.026(3) . ? N8 N9 1.381(4) . ? N8 Pd1 2.024(3) . ? N9 Pd2 1.996(3) . ? N11 Pd3 2.039(3) . ? N12 Pd3 2.033(3) . ? N13 Pd4 1.989(3) . ? N14 Pd4 2.033(3) . ? N15 N16 1.383(4) . ? N15 Pd3 2.025(3) . ? N16 Pd4 1.998(3) . ? N18 N19 1.358(4) . ? N18 Pd3 2.005(3) . ? N19 Pd4 2.025(3) . ? N21 O2 1.221(4) . ? N21 O3 1.223(5) . ? N21 O1 1.285(4) . ? N22 O4 1.211(4) . ? N22 O5 1.244(4) . ? N22 O6 1.273(5) . ? N23 O9 1.203(4) . ? N23 O7 1.229(4) . ? N23 O8 1.255(5) . ? N24 O12 1.165(4) . ? N24 O11 1.184(4) . ? N24 O10 1.289(4) . ? O1W H1X 0.8500 . ? O1W H1Y 0.8500 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8500 . ? O3W H3X 0.8500 . ? O3W H3Y 0.8500 . ? O4W H4X 0.8501 . ? O4W H4Y 0.8500 . ? O5W H5X 0.8500 . ? O5W H5Y 0.8500 . ? O6W H6X 0.8499 . ? O6W H6Y 0.8499 . ? O7W H7X 0.8500 . ? O7W H7Y 0.8499 . ? O8W H8X 0.8500 . ? O8W H8Y 0.8499 . ? O9W H9X 0.8500 . ? O9W H9Y 0.8500 . ? O10W H10X 0.8501 . ? O10W H10Y 0.8500 . ? O11W H11X 0.8500 . ? O11W H11Y 0.8500 . ? O12W H12X 0.8501 . ? O12W H12Y 0.8501 . ? O13W H13X 0.8500 . ? O13W H13Y 0.8500 . ? Pd1 Pd2 3.0821(10) . ? Pd3 Pd4 3.0902(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 122.2(4) . . ? C2 C1 H1 118.9 . . ? N1 C1 H1 118.9 . . ? C1 C2 C3 118.7(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 116.6(3) . . ? C2 C3 H3 121.7 . . ? C4 C3 H3 121.7 . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 N1 122.2(4) . . ? C4 C5 C6 125.5(4) . . ? N1 C5 C6 108.4(3) . . ? C7 C6 N2 122.8(4) . . ? C7 C6 C5 120.5(4) . . ? N2 C6 C5 116.5(3) . . ? C6 C7 C8 120.5(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 115.5(4) . . ? C9 C8 H8 122.3 . . ? C7 C8 H8 122.3 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 N2 123.4(4) . . ? C9 C10 H10 118.3 . . ? N2 C10 H10 118.3 . . ? N3 C11 C12 120.3(4) . . ? N3 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 121.7(4) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 117.4(4) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 N3 121.8(3) . . ? C14 C15 C16 123.5(3) . . ? N3 C15 C16 114.7(3) . . ? C17 C16 N4 120.3(4) . . ? C17 C16 C15 124.6(4) . . ? N4 C16 C15 114.7(3) . . ? C16 C17 C18 121.6(4) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 114.9(4) . . ? C18 C19 H19 122.6 . . ? C20 C19 H19 122.6 . . ? N4 C20 C19 124.4(4) . . ? N4 C20 H20 117.8 . . ? C19 C20 H20 117.8 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 108.9(3) . . ? N5 C22 C21 122.5(3) . . ? C23 C22 C21 128.1(3) . . ? C24 C23 C22 106.1(3) . . ? C24 C23 C28 129.1(4) . . ? C22 C23 C28 124.8(4) . . ? C23 C24 N6 110.8(3) . . ? C23 C24 C25 134.7(3) . . ? N6 C24 C25 114.0(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N7 C26 C27 117.7(4) . . ? N7 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 120.6(4) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.3(3) . . ? C27 C28 C23 120.8(4) . . ? C29 C28 C23 119.8(3) . . ? C30 C29 C28 118.8(4) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? N7 C30 C29 120.3(4) . . ? N7 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N8 C32 C33 107.5(3) . . ? N8 C32 C31 121.6(3) . . ? C33 C32 C31 130.9(3) . . ? C34 C33 C32 109.2(3) . . ? C34 C33 C38 124.7(4) . . ? C32 C33 C38 125.9(4) . . ? C33 C34 N9 106.9(3) . . ? C33 C34 C35 137.0(3) . . ? N9 C34 C35 115.9(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N10 C36 C37 118.5(4) . . ? N10 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C38 C37 C36 119.1(4) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 121.0(4) . . ? C39 C38 C33 120.8(4) . . ? C37 C38 C33 118.1(4) . . ? C38 C39 C40 118.7(4) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N10 C40 C39 117.3(4) . . ? N10 C40 H40 121.4 . . ? C39 C40 H40 121.4 . . ? N11 C41 C42 120.9(4) . . ? N11 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C43 C42 C41 119.4(4) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 118.9(4) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C45 C44 C43 117.9(3) . . ? C45 C44 H44 121.1 . . ? C43 C44 H44 121.1 . . ? N11 C45 C44 122.7(3) . . ? N11 C45 C46 116.7(3) . . ? C44 C45 C46 120.5(3) . . ? N12 C46 C47 120.7(3) . . ? N12 C46 C45 114.1(3) . . ? C47 C46 C45 125.3(3) . . ? C48 C47 C46 118.5(4) . . ? C48 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? C47 C48 C49 121.6(4) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C48 C49 C50 116.3(4) . . ? C48 C49 H49 121.8 . . ? C50 C49 H49 121.8 . . ? N12 C50 C49 124.1(4) . . ? N12 C50 H50 118.0 . . ? C49 C50 H50 118.0 . . ? N13 C51 C52 123.5(4) . . ? N13 C51 H51 118.2 . . ? C52 C51 H51 118.2 . . ? C53 C52 C51 117.5(4) . . ? C53 C52 H52 121.2 . . ? C51 C52 H52 121.2 . . ? C54 C53 C52 118.3(4) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? C53 C54 C55 122.1(4) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C54 C55 N13 122.8(4) . . ? C54 C55 C56 126.3(4) . . ? N13 C55 C56 110.9(3) . . ? N14 C56 C57 118.7(4) . . ? N14 C56 C55 116.9(3) . . ? C57 C56 C55 124.2(4) . . ? C58 C57 C56 121.6(4) . . ? C58 C57 H57 119.2 . . ? C56 C57 H57 119.2 . . ? C57 C58 C59 120.3(4) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C60 C59 C58 117.6(4) . . ? C60 C59 H59 121.2 . . ? C58 C59 H59 121.2 . . ? C59 C60 N14 117.7(4) . . ? C59 C60 H60 121.1 . . ? N14 C60 H60 121.1 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N15 C62 C63 111.1(3) . . ? N15 C62 C61 117.4(3) . . ? C63 C62 C61 131.2(3) . . ? C62 C63 C64 106.2(3) . . ? C62 C63 C68 127.3(3) . . ? C64 C63 C68 126.5(3) . . ? N16 C64 C63 105.6(3) . . ? N16 C64 C65 122.0(3) . . ? C63 C64 C65 132.3(3) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N17 C66 C67 119.8(4) . . ? N17 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C66 C67 C68 122.1(4) . . ? C66 C67 H67 118.9 . . ? C68 C67 H67 118.9 . . ? C67 C68 C69 114.5(3) . . ? C67 C68 C63 123.9(3) . . ? C69 C68 C63 121.5(3) . . ? C70 C69 C68 120.9(4) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 N17 122.9(4) . . ? C69 C70 H70 118.6 . . ? N17 C70 H70 118.6 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N18 C72 C73 107.2(3) . . ? N18 C72 C71 123.0(3) . . ? C73 C72 C71 129.4(3) . . ? C78 C73 C74 129.6(3) . . ? C78 C73 C72 126.3(3) . . ? C74 C73 C72 104.1(3) . . ? N19 C74 C73 107.8(3) . . ? N19 C74 C75 123.5(3) . . ? C73 C74 C75 128.5(3) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N20 C76 C77 119.3(4) . . ? N20 C76 H76 120.4 . . ? C77 C76 H76 120.4 . . ? C76 C77 C78 122.5(4) . . ? C76 C77 H77 118.8 . . ? C78 C77 H77 118.8 . . ? C73 C78 C77 121.8(3) . . ? C73 C78 C79 122.6(3) . . ? C77 C78 C79 115.5(3) . . ? C80 C79 C78 120.3(4) . . ? C80 C79 H79 119.8 . . ? C78 C79 H79 119.8 . . ? C79 C80 N20 121.0(4) . . ? C79 C80 H80 119.5 . . ? N20 C80 H80 119.5 . . ? C1 N1 C5 116.6(3) . . ? C1 N1 Pd1 126.3(3) . . ? C5 N1 Pd1 116.6(3) . . ? C6 N2 C10 116.5(3) . . ? C6 N2 Pd1 116.0(3) . . ? C10 N2 Pd1 127.6(3) . . ? C11 N3 C15 119.3(3) . . ? C11 N3 Pd2 125.7(3) . . ? C15 N3 Pd2 114.6(2) . . ? C20 N4 C16 119.8(4) . . ? C20 N4 Pd2 125.7(3) . . ? C16 N4 Pd2 114.5(3) . . ? C22 N5 N6 107.0(3) . . ? C22 N5 Pd1 136.9(3) . . ? N6 N5 Pd1 115.9(2) . . ? C24 N6 N5 107.0(3) . . ? C24 N6 Pd2 138.9(3) . . ? N5 N6 Pd2 113.95(19) . . ? C30 N7 C26 123.1(3) . . ? C32 N8 N9 108.4(3) . . ? C32 N8 Pd1 136.0(2) . . ? N9 N8 Pd1 115.4(2) . . ? N8 N9 C34 107.9(3) . . ? N8 N9 Pd2 114.5(2) . . ? C34 N9 Pd2 137.5(3) . . ? C36 N10 C40 125.3(4) . . ? C45 N11 C41 120.0(3) . . ? C45 N11 Pd3 113.7(2) . . ? C41 N11 Pd3 126.1(3) . . ? C50 N12 C46 118.4(3) . . ? C50 N12 Pd3 127.9(3) . . ? C46 N12 Pd3 113.4(2) . . ? C55 N13 C51 115.6(3) . . ? C55 N13 Pd4 117.9(3) . . ? C51 N13 Pd4 126.6(3) . . ? C56 N14 C60 123.4(3) . . ? C56 N14 Pd4 114.6(3) . . ? C60 N14 Pd4 122.0(3) . . ? C62 N15 N16 107.8(3) . . ? C62 N15 Pd3 138.6(2) . . ? N16 N15 Pd3 113.4(2) . . ? C64 N16 N15 109.2(3) . . ? C64 N16 Pd4 133.9(2) . . ? N15 N16 Pd4 116.7(2) . . ? C66 N17 C70 119.8(3) . . ? N19 N18 C72 108.3(3) . . ? N19 N18 Pd3 117.0(2) . . ? C72 N18 Pd3 134.3(2) . . ? C74 N19 N18 112.4(3) . . ? C74 N19 Pd4 133.6(3) . . ? N18 N19 Pd4 113.8(2) . . ? C76 N20 C80 121.3(3) . . ? O2 N21 O3 127.8(4) . . ? O2 N21 O1 114.8(3) . . ? O3 N21 O1 117.3(4) . . ? O4 N22 O5 125.4(3) . . ? O4 N22 O6 119.3(3) . . ? O5 N22 O6 115.0(3) . . ? O9 N23 O7 126.8(4) . . ? O9 N23 O8 118.8(3) . . ? O7 N23 O8 114.2(3) . . ? O12 N24 O11 125.7(3) . . ? O12 N24 O10 116.3(3) . . ? O11 N24 O10 117.7(3) . . ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 109.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 109.5 . . ? H5X O5W H5Y 109.5 . . ? H6X O6W H6Y 109.5 . . ? H7X O7W H7Y 109.5 . . ? H8X O8W H8Y 109.5 . . ? H9X O9W H9Y 109.5 . . ? H10X O10W H10Y 109.5 . . ? H11X O11W H11Y 109.5 . . ? H12X O12W H12Y 109.5 . . ? H13X O13W H13Y 109.5 . . ? N2 Pd1 N1 80.53(14) . . ? N2 Pd1 N5 175.79(14) . . ? N1 Pd1 N5 96.22(13) . . ? N2 Pd1 N8 96.32(13) . . ? N1 Pd1 N8 174.46(13) . . ? N5 Pd1 N8 86.70(12) . . ? N2 Pd1 Pd2 113.82(10) . . ? N1 Pd1 Pd2 112.74(10) . . ? N5 Pd1 Pd2 64.89(9) . . ? N8 Pd1 Pd2 64.27(9) . . ? N3 Pd2 N9 174.07(12) . . ? N3 Pd2 N6 97.46(13) . . ? N9 Pd2 N6 84.94(13) . . ? N3 Pd2 N4 81.37(13) . . ? N9 Pd2 N4 95.91(13) . . ? N6 Pd2 N4 176.40(11) . . ? N3 Pd2 Pd1 110.42(9) . . ? N9 Pd2 Pd1 65.63(9) . . ? N6 Pd2 Pd1 65.21(8) . . ? N4 Pd2 Pd1 111.95(9) . . ? N18 Pd3 N15 87.48(12) . . ? N18 Pd3 N12 95.08(12) . . ? N15 Pd3 N12 176.71(12) . . ? N18 Pd3 N11 175.97(12) . . ? N15 Pd3 N11 95.28(12) . . ? N12 Pd3 N11 82.06(12) . . ? N18 Pd3 Pd4 64.17(8) . . ? N15 Pd3 Pd4 65.16(8) . . ? N12 Pd3 Pd4 114.15(10) . . ? N11 Pd3 Pd4 114.38(9) . . ? N13 Pd4 N16 97.20(13) . . ? N13 Pd4 N19 175.66(13) . . ? N16 Pd4 N19 85.27(13) . . ? N13 Pd4 N14 79.60(14) . . ? N16 Pd4 N14 173.67(12) . . ? N19 Pd4 N14 97.59(14) . . ? N13 Pd4 Pd3 112.91(9) . . ? N16 Pd4 Pd3 64.58(8) . . ? N19 Pd4 Pd3 64.91(8) . . ? N14 Pd4 Pd3 111.49(10) . . ? 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 -2.8(6) . . . . ? C1 C2 C3 C4 7.4(6) . . . . ? C2 C3 C4 C5 -15.5(7) . . . . ? C3 C4 C5 N1 18.4(8) . . . . ? C3 C4 C5 C6 173.4(4) . . . . ? C4 C5 C6 C7 14.2(7) . . . . ? N1 C5 C6 C7 172.1(4) . . . . ? C4 C5 C6 N2 -169.7(5) . . . . ? N1 C5 C6 N2 -11.8(5) . . . . ? N2 C6 C7 C8 7.1(6) . . . . ? C5 C6 C7 C8 -177.1(4) . . . . ? C6 C7 C8 C9 -7.0(6) . . . . ? C7 C8 C9 C10 2.8(7) . . . . ? C8 C9 C10 N2 1.7(8) . . . . ? N3 C11 C12 C13 -3.0(6) . . . . ? C11 C12 C13 C14 3.0(6) . . . . ? C12 C13 C14 C15 -4.0(5) . . . . ? C13 C14 C15 N3 5.1(5) . . . . ? C13 C14 C15 C16 -174.3(4) . . . . ? C14 C15 C16 C17 4.1(7) . . . . ? N3 C15 C16 C17 -175.4(4) . . . . ? C14 C15 C16 N4 176.6(3) . . . . ? N3 C15 C16 N4 -2.8(5) . . . . ? N4 C16 C17 C18 5.6(7) . . . . ? C15 C16 C17 C18 177.8(4) . . . . ? C16 C17 C18 C19 -5.0(6) . . . . ? C17 C18 C19 C20 2.1(6) . . . . ? C18 C19 C20 N4 0.1(6) . . . . ? N5 C22 C23 C24 -0.2(5) . . . . ? C21 C22 C23 C24 172.6(4) . . . . ? N5 C22 C23 C28 -177.6(4) . . . . ? C21 C22 C23 C28 -4.8(7) . . . . ? C22 C23 C24 N6 2.7(5) . . . . ? C28 C23 C24 N6 -180.0(4) . . . . ? C22 C23 C24 C25 174.2(5) . . . . ? C28 C23 C24 C25 -8.5(9) . . . . ? N7 C26 C27 C28 -3.8(6) . . . . ? C26 C27 C28 C29 2.6(6) . . . . ? C26 C27 C28 C23 -173.8(4) . . . . ? C24 C23 C28 C27 -52.6(7) . . . . ? C22 C23 C28 C27 124.3(4) . . . . ? C24 C23 C28 C29 131.0(5) . . . . ? C22 C23 C28 C29 -52.1(6) . . . . ? C27 C28 C29 C30 0.6(6) . . . . ? C23 C28 C29 C30 177.1(4) . . . . ? C28 C29 C30 N7 -2.6(6) . . . . ? N8 C32 C33 C34 1.2(5) . . . . ? C31 C32 C33 C34 -178.7(4) . . . . ? N8 C32 C33 C38 176.4(4) . . . . ? C31 C32 C33 C38 -3.5(7) . . . . ? C32 C33 C34 N9 -2.3(4) . . . . ? C38 C33 C34 N9 -177.6(4) . . . . ? C32 C33 C34 C35 -176.2(4) . . . . ? C38 C33 C34 C35 8.5(8) . . . . ? N10 C36 C37 C38 -1.9(6) . . . . ? C36 C37 C38 C39 1.3(6) . . . . ? C36 C37 C38 C33 178.1(4) . . . . ? C34 C33 C38 C39 26.9(6) . . . . ? C32 C33 C38 C39 -147.6(4) . . . . ? C34 C33 C38 C37 -149.9(4) . . . . ? C32 C33 C38 C37 35.6(6) . . . . ? C37 C38 C39 C40 -1.6(6) . . . . ? C33 C38 C39 C40 -178.3(4) . . . . ? C38 C39 C40 N10 2.5(6) . . . . ? N11 C41 C42 C43 5.9(6) . . . . ? C41 C42 C43 C44 -5.5(6) . . . . ? C42 C43 C44 C45 3.5(5) . . . . ? C43 C44 C45 N11 -1.7(5) . . . . ? C43 C44 C45 C46 173.6(3) . . . . ? N11 C45 C46 N12 0.8(5) . . . . ? C44 C45 C46 N12 -174.8(3) . . . . ? N11 C45 C46 C47 -179.9(4) . . . . ? C44 C45 C46 C47 4.5(6) . . . . ? N12 C46 C47 C48 5.1(7) . . . . ? C45 C46 C47 C48 -174.1(4) . . . . ? C46 C47 C48 C49 -1.9(7) . . . . ? C47 C48 C49 C50 0.6(6) . . . . ? C48 C49 C50 N12 -2.8(6) . . . . ? N13 C51 C52 C53 4.6(5) . . . . ? C51 C52 C53 C54 -5.0(6) . . . . ? C52 C53 C54 C55 3.7(6) . . . . ? C53 C54 C55 N13 -1.6(6) . . . . ? C53 C54 C55 C56 -177.9(4) . . . . ? C54 C55 C56 N14 176.1(3) . . . . ? N13 C55 C56 N14 -0.6(5) . . . . ? C54 C55 C56 C57 0.9(6) . . . . ? N13 C55 C56 C57 -175.8(3) . . . . ? N14 C56 C57 C58 4.9(6) . . . . ? C55 C56 C57 C58 -179.9(4) . . . . ? C56 C57 C58 C59 -9.3(6) . . . . ? C57 C58 C59 C60 9.5(6) . . . . ? C58 C59 C60 N14 -5.4(5) . . . . ? N15 C62 C63 C64 1.4(4) . . . . ? C61 C62 C63 C64 175.9(4) . . . . ? N15 C62 C63 C68 -175.0(4) . . . . ? C61 C62 C63 C68 -0.5(7) . . . . ? C62 C63 C64 N16 0.5(4) . . . . ? C68 C63 C64 N16 177.0(4) . . . . ? C62 C63 C64 C65 176.2(4) . . . . ? C68 C63 C64 C65 -7.4(7) . . . . ? N17 C66 C67 C68 0.0(7) . . . . ? C66 C67 C68 C69 1.6(6) . . . . ? C66 C67 C68 C63 178.7(4) . . . . ? C62 C63 C68 C67 -33.0(6) . . . . ? C64 C63 C68 C67 151.2(4) . . . . ? C62 C63 C68 C69 143.8(4) . . . . ? C64 C63 C68 C69 -31.9(6) . . . . ? C67 C68 C69 C70 -2.7(6) . . . . ? C63 C68 C69 C70 -179.8(4) . . . . ? C68 C69 C70 N17 2.1(6) . . . . ? N18 C72 C73 C78 177.1(4) . . . . ? C71 C72 C73 C78 4.2(6) . . . . ? N18 C72 C73 C74 -4.0(4) . . . . ? C71 C72 C73 C74 -176.9(4) . . . . ? C78 C73 C74 N19 -176.7(4) . . . . ? C72 C73 C74 N19 4.5(4) . . . . ? C78 C73 C74 C75 -1.4(7) . . . . ? C72 C73 C74 C75 179.7(4) . . . . ? N20 C76 C77 C78 2.8(6) . . . . ? C74 C73 C78 C77 -128.4(4) . . . . ? C72 C73 C78 C77 50.2(6) . . . . ? C74 C73 C78 C79 54.1(6) . . . . ? C72 C73 C78 C79 -127.2(4) . . . . ? C76 C77 C78 C73 -178.6(4) . . . . ? C76 C77 C78 C79 -1.0(6) . . . . ? C73 C78 C79 C80 177.0(4) . . . . ? C77 C78 C79 C80 -0.6(6) . . . . ? C78 C79 C80 N20 0.5(6) . . . . ? C2 C1 N1 C5 4.6(6) . . . . ? C2 C1 N1 Pd1 176.4(3) . . . . ? C4 C5 N1 C1 -12.7(7) . . . . ? C6 C5 N1 C1 -171.4(3) . . . . ? C4 C5 N1 Pd1 174.7(4) . . . . ? C6 C5 N1 Pd1 15.9(5) . . . . ? C7 C6 N2 C10 -2.4(6) . . . . ? C5 C6 N2 C10 -178.4(4) . . . . ? C7 C6 N2 Pd1 178.6(3) . . . . ? C5 C6 N2 Pd1 2.6(5) . . . . ? C9 C10 N2 C6 -2.2(7) . . . . ? C9 C10 N2 Pd1 176.8(3) . . . . ? C12 C11 N3 C15 3.8(5) . . . . ? C12 C11 N3 Pd2 176.8(3) . . . . ? C14 C15 N3 C11 -5.0(5) . . . . ? C16 C15 N3 C11 174.4(3) . . . . ? C14 C15 N3 Pd2 -178.8(3) . . . . ? C16 C15 N3 Pd2 0.7(4) . . . . ? C19 C20 N4 C16 0.5(6) . . . . ? C19 C20 N4 Pd2 -179.3(3) . . . . ? C17 C16 N4 C20 -3.3(6) . . . . ? C15 C16 N4 C20 -176.2(3) . . . . ? C17 C16 N4 Pd2 176.5(3) . . . . ? C15 C16 N4 Pd2 3.6(5) . . . . ? C23 C22 N5 N6 -2.3(4) . . . . ? C21 C22 N5 N6 -175.6(4) . . . . ? C23 C22 N5 Pd1 -176.7(3) . . . . ? C21 C22 N5 Pd1 10.0(7) . . . . ? C23 C24 N6 N5 -4.2(5) . . . . ? C25 C24 N6 N5 -177.5(3) . . . . ? C23 C24 N6 Pd2 179.4(3) . . . . ? C25 C24 N6 Pd2 6.0(6) . . . . ? C22 N5 N6 C24 3.9(4) . . . . ? Pd1 N5 N6 C24 179.6(3) . . . . ? C22 N5 N6 Pd2 -178.7(3) . . . . ? Pd1 N5 N6 Pd2 -2.9(3) . . . . ? C29 C30 N7 C26 1.4(6) . . . . ? C27 C26 N7 C30 1.8(6) . . . . ? C33 C32 N8 N9 0.5(4) . . . . ? C31 C32 N8 N9 -179.6(3) . . . . ? C33 C32 N8 Pd1 175.0(3) . . . . ? C31 C32 N8 Pd1 -5.1(6) . . . . ? C32 N8 N9 C34 -1.9(4) . . . . ? Pd1 N8 N9 C34 -177.7(2) . . . . ? C32 N8 N9 Pd2 179.6(2) . . . . ? Pd1 N8 N9 Pd2 3.9(3) . . . . ? C33 C34 N9 N8 2.6(4) . . . . ? C35 C34 N9 N8 178.0(3) . . . . ? C33 C34 N9 Pd2 -179.5(3) . . . . ? C35 C34 N9 Pd2 -4.1(6) . . . . ? C37 C36 N10 C40 3.0(6) . . . . ? C39 C40 N10 C36 -3.3(6) . . . . ? C44 C45 N11 C41 1.9(6) . . . . ? C46 C45 N11 C41 -173.6(3) . . . . ? C44 C45 N11 Pd3 176.7(3) . . . . ? C46 C45 N11 Pd3 1.2(4) . . . . ? C42 C41 N11 C45 -4.0(6) . . . . ? C42 C41 N11 Pd3 -178.0(3) . . . . ? C49 C50 N12 C46 6.0(6) . . . . ? C49 C50 N12 Pd3 179.7(3) . . . . ? C47 C46 N12 C50 -7.1(6) . . . . ? C45 C46 N12 C50 172.2(3) . . . . ? C47 C46 N12 Pd3 178.3(3) . . . . ? C45 C46 N12 Pd3 -2.4(4) . . . . ? C54 C55 N13 C51 0.9(5) . . . . ? C56 C55 N13 C51 177.7(3) . . . . ? C54 C55 N13 Pd4 -179.3(3) . . . . ? C56 C55 N13 Pd4 -2.5(4) . . . . ? C52 C51 N13 C55 -2.5(5) . . . . ? C52 C51 N13 Pd4 177.8(3) . . . . ? C57 C56 N14 C60 -0.8(5) . . . . ? C55 C56 N14 C60 -176.3(3) . . . . ? C57 C56 N14 Pd4 178.8(3) . . . . ? C55 C56 N14 Pd4 3.3(4) . . . . ? C59 C60 N14 C56 1.4(5) . . . . ? C59 C60 N14 Pd4 -178.2(3) . . . . ? C63 C62 N15 N16 -2.8(4) . . . . ? C61 C62 N15 N16 -178.1(3) . . . . ? C63 C62 N15 Pd3 -177.7(3) . . . . ? C61 C62 N15 Pd3 7.0(6) . . . . ? C63 C64 N16 N15 -2.2(4) . . . . ? C65 C64 N16 N15 -178.4(3) . . . . ? C63 C64 N16 Pd4 -177.8(3) . . . . ? C65 C64 N16 Pd4 6.0(5) . . . . ? C62 N15 N16 C64 3.1(4) . . . . ? Pd3 N15 N16 C64 179.5(2) . . . . ? C62 N15 N16 Pd4 179.6(2) . . . . ? Pd3 N15 N16 Pd4 -4.0(3) . . . . ? C67 C66 N17 C70 -0.8(6) . . . . ? C69 C70 N17 C66 -0.3(7) . . . . ? C73 C72 N18 N19 2.2(4) . . . . ? C71 C72 N18 N19 175.6(3) . . . . ? C73 C72 N18 Pd3 175.2(3) . . . . ? C71 C72 N18 Pd3 -11.4(5) . . . . ? C73 C74 N19 N18 -3.4(5) . . . . ? C75 C74 N19 N18 -178.9(4) . . . . ? C73 C74 N19 Pd4 -178.2(3) . . . . ? C75 C74 N19 Pd4 6.2(7) . . . . ? C72 N18 N19 C74 0.7(4) . . . . ? Pd3 N18 N19 C74 -173.7(3) . . . . ? C72 N18 N19 Pd4 176.7(2) . . . . ? Pd3 N18 N19 Pd4 2.3(3) . . . . ? C77 C76 N20 C80 -2.9(6) . . . . ? C79 C80 N20 C76 1.3(6) . . . . ? C6 N2 Pd1 N1 5.0(3) . . . . ? C10 N2 Pd1 N1 -173.9(4) . . . . ? C6 N2 Pd1 N8 -179.6(3) . . . . ? C10 N2 Pd1 N8 1.5(4) . . . . ? C6 N2 Pd1 Pd2 115.8(3) . . . . ? C10 N2 Pd1 Pd2 -63.2(4) . . . . ? C1 N1 Pd1 N2 176.0(4) . . . . ? C5 N1 Pd1 N2 -12.2(3) . . . . ? C1 N1 Pd1 N5 -1.3(4) . . . . ? C5 N1 Pd1 N5 170.5(3) . . . . ? C1 N1 Pd1 Pd2 64.0(4) . . . . ? C5 N1 Pd1 Pd2 -124.2(3) . . . . ? C22 N5 Pd1 N1 -71.8(4) . . . . ? N6 N5 Pd1 N1 114.2(3) . . . . ? C22 N5 Pd1 N8 112.9(4) . . . . ? N6 N5 Pd1 N8 -61.1(3) . . . . ? C22 N5 Pd1 Pd2 176.0(4) . . . . ? N6 N5 Pd1 Pd2 1.9(2) . . . . ? C32 N8 Pd1 N2 69.9(4) . . . . ? N9 N8 Pd1 N2 -116.0(2) . . . . ? C32 N8 Pd1 N5 -113.1(4) . . . . ? N9 N8 Pd1 N5 61.1(2) . . . . ? C32 N8 Pd1 Pd2 -176.7(4) . . . . ? N9 N8 Pd1 Pd2 -2.52(19) . . . . ? C11 N3 Pd2 N6 4.2(3) . . . . ? C15 N3 Pd2 N6 177.5(2) . . . . ? C11 N3 Pd2 N4 -172.3(3) . . . . ? C15 N3 Pd2 N4 0.9(2) . . . . ? C11 N3 Pd2 Pd1 -62.0(3) . . . . ? C15 N3 Pd2 Pd1 111.2(2) . . . . ? N8 N9 Pd2 N6 -67.5(2) . . . . ? C34 N9 Pd2 N6 114.6(4) . . . . ? N8 N9 Pd2 N4 108.9(2) . . . . ? C34 N9 Pd2 N4 -68.9(4) . . . . ? N8 N9 Pd2 Pd1 -2.51(19) . . . . ? C34 N9 Pd2 Pd1 179.7(4) . . . . ? C24 N6 Pd2 N3 69.1(4) . . . . ? N5 N6 Pd2 N3 -107.2(3) . . . . ? C24 N6 Pd2 N9 -116.4(4) . . . . ? N5 N6 Pd2 N9 67.3(3) . . . . ? C24 N6 Pd2 Pd1 178.1(5) . . . . ? N5 N6 Pd2 Pd1 1.9(2) . . . . ? C20 N4 Pd2 N3 177.3(3) . . . . ? C16 N4 Pd2 N3 -2.5(3) . . . . ? C20 N4 Pd2 N9 2.6(3) . . . . ? C16 N4 Pd2 N9 -177.2(3) . . . . ? C20 N4 Pd2 Pd1 68.6(3) . . . . ? C16 N4 Pd2 Pd1 -111.2(3) . . . . ? N2 Pd1 Pd2 N3 -88.03(15) . . . . ? N1 Pd1 Pd2 N3 1.40(14) . . . . ? N5 Pd1 Pd2 N3 87.58(15) . . . . ? N8 Pd1 Pd2 N3 -173.49(13) . . . . ? N2 Pd1 Pd2 N9 87.19(15) . . . . ? N1 Pd1 Pd2 N9 176.62(14) . . . . ? N5 Pd1 Pd2 N9 -97.20(15) . . . . ? N8 Pd1 Pd2 N9 1.73(13) . . . . ? N2 Pd1 Pd2 N6 -176.92(15) . . . . ? N1 Pd1 Pd2 N6 -87.49(14) . . . . ? N5 Pd1 Pd2 N6 -1.31(14) . . . . ? N8 Pd1 Pd2 N6 97.62(13) . . . . ? N2 Pd1 Pd2 N4 0.68(15) . . . . ? N1 Pd1 Pd2 N4 90.10(14) . . . . ? N5 Pd1 Pd2 N4 176.28(14) . . . . ? N8 Pd1 Pd2 N4 -84.79(13) . . . . ? N19 N18 Pd3 N15 62.0(3) . . . . ? C72 N18 Pd3 N15 -110.5(3) . . . . ? N19 N18 Pd3 N12 -115.9(3) . . . . ? C72 N18 Pd3 N12 71.6(3) . . . . ? N19 N18 Pd3 Pd4 -1.5(2) . . . . ? C72 N18 Pd3 Pd4 -174.0(4) . . . . ? C62 N15 Pd3 N18 114.7(4) . . . . ? N16 N15 Pd3 N18 -60.0(2) . . . . ? C62 N15 Pd3 N11 -68.3(4) . . . . ? N16 N15 Pd3 N11 117.0(2) . . . . ? C62 N15 Pd3 Pd4 177.3(4) . . . . ? N16 N15 Pd3 Pd4 2.58(19) . . . . ? C50 N12 Pd3 N18 5.5(4) . . . . ? C46 N12 Pd3 N18 179.5(3) . . . . ? C50 N12 Pd3 N11 -171.6(4) . . . . ? C46 N12 Pd3 N11 2.3(3) . . . . ? C50 N12 Pd3 Pd4 -58.4(4) . . . . ? C46 N12 Pd3 Pd4 115.6(2) . . . . ? C45 N11 Pd3 N15 -179.9(3) . . . . ? C41 N11 Pd3 N15 -5.6(3) . . . . ? C45 N11 Pd3 N12 -1.9(3) . . . . ? C41 N11 Pd3 N12 172.5(3) . . . . ? C45 N11 Pd3 Pd4 -114.9(2) . . . . ? C41 N11 Pd3 Pd4 59.5(3) . . . . ? C55 N13 Pd4 N16 177.8(3) . . . . ? C51 N13 Pd4 N16 -2.5(3) . . . . ? C55 N13 Pd4 N14 3.3(3) . . . . ? C51 N13 Pd4 N14 -176.9(3) . . . . ? C55 N13 Pd4 Pd3 112.4(2) . . . . ? C51 N13 Pd4 Pd3 -67.9(3) . . . . ? C64 N16 Pd4 N13 66.1(3) . . . . ? N15 N16 Pd4 N13 -109.3(2) . . . . ? C64 N16 Pd4 N19 -117.5(3) . . . . ? N15 N16 Pd4 N19 67.1(2) . . . . ? C64 N16 Pd4 Pd3 178.1(4) . . . . ? N15 N16 Pd4 Pd3 2.7(2) . . . . ? C74 N19 Pd4 N16 109.3(4) . . . . ? N18 N19 Pd4 N16 -65.6(2) . . . . ? C74 N19 Pd4 N14 -76.4(4) . . . . ? N18 N19 Pd4 N14 108.8(3) . . . . ? C74 N19 Pd4 Pd3 173.4(4) . . . . ? N18 N19 Pd4 Pd3 -1.5(2) . . . . ? C56 N14 Pd4 N13 -3.5(3) . . . . ? C56 N14 Pd4 N19 179.8(3) . . . . ? C60 N14 Pd4 N19 -0.6(3) . . . . ? C56 N14 Pd4 Pd3 -114.2(3) . . . . ? C60 N14 Pd4 Pd3 65.4(3) . . . . ? N18 Pd3 Pd4 N13 -174.88(14) . . . . ? N15 Pd3 Pd4 N13 85.32(14) . . . . ? N12 Pd3 Pd4 N13 -91.15(14) . . . . ? N11 Pd3 Pd4 N13 0.97(14) . . . . ? N18 Pd3 Pd4 N16 97.99(14) . . . . ? N15 Pd3 Pd4 N16 -1.81(13) . . . . ? N12 Pd3 Pd4 N16 -178.28(14) . . . . ? N11 Pd3 Pd4 N16 -86.16(14) . . . . ? N18 Pd3 Pd4 N19 1.01(14) . . . . ? N15 Pd3 Pd4 N19 -98.80(14) . . . . ? N12 Pd3 Pd4 N19 84.73(14) . . . . ? N11 Pd3 Pd4 N19 176.86(14) . . . . ? N18 Pd3 Pd4 N14 -87.42(14) . . . . ? N15 Pd3 Pd4 N14 172.78(14) . . . . ? N12 Pd3 Pd4 N14 -3.69(14) . . . . ? N11 Pd3 Pd4 N14 88.43(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.719 _refine_diff_density_min -1.524 _refine_diff_density_rms 0.094