# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Shu-Yan Yu' _publ_contact_author_email YUSY@RUC.EDU.CN _publ_section_title ; Self-Assembly of Hat-Shaped Trinuclear Metallo-macrocycles ; loop_ _publ_author_name 'Shu-Yan Yu.' 'Yi-Zhi Li.' 'Guo-Hong Ning.' 'Yuan-Jiang Pan.' ; Ting-Zheng Xie ; # Attachment '1564Revised.cif' data_1564 _database_code_depnum_ccdc_archive 'CCDC 757500' #TrackingRef '1564Revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C51 H39 N12 Pd3, 2(C H4 O), 3(N O3), H0.82 O0.41, 1.59(H2 O) ; _chemical_formula_sum 'C53 H51 N15 O13 Pd3' _chemical_formula_weight 1425.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.483(8) _cell_length_b 26.681(9) _cell_length_c 16.150(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.81(3) _cell_angle_gamma 90.00 _cell_volume 11887(5) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4175 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 23.22 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5728 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7592 _exptl_absorpt_correction_T_max 0.8003 _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 20893 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11517 _reflns_number_gt 8276 _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^)+(0.08P)^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 11517 _refine_ls_number_parameters 787 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.4583(3) 0.1553(3) 1.0585(6) 0.061(2) Uani 1 1 d . . . H1 H 0.4447 0.1867 1.0362 0.073 Uiso 1 1 calc R . . C2 C 0.5032(3) 0.1530(3) 1.1367(6) 0.070(3) Uani 1 1 d . . . H2 H 0.5195 0.1817 1.1693 0.085 Uiso 1 1 calc R . . C3 C 0.5234(3) 0.1043(3) 1.1653(6) 0.069(2) Uani 1 1 d . . . H3 H 0.5548 0.1010 1.2148 0.083 Uiso 1 1 calc R . . C4 C 0.4980(3) 0.0635(3) 1.1223(6) 0.062(2) Uani 1 1 d . . . H4 H 0.5105 0.0320 1.1463 0.075 Uiso 1 1 calc R . . C5 C 0.4532(3) 0.0674(3) 1.0424(5) 0.0523(17) Uani 1 1 d . . . C6 C 0.4223(3) 0.0259(3) 0.9879(6) 0.059(2) Uani 1 1 d . . . C7 C 0.4365(3) -0.0234(3) 1.0059(5) 0.060(2) Uani 1 1 d . . . H7 H 0.4677 -0.0311 1.0531 0.072 Uiso 1 1 calc R . . C8 C 0.4050(3) -0.0618(3) 0.9543(5) 0.061(2) Uani 1 1 d . . . H8 H 0.4133 -0.0952 0.9696 0.073 Uiso 1 1 calc R . . C9 C 0.3609(3) -0.0485(3) 0.8798(5) 0.0578(19) Uani 1 1 d . . . H9 H 0.3396 -0.0727 0.8401 0.069 Uiso 1 1 calc R . . C10 C 0.3490(3) 0.0019(3) 0.8653(6) 0.062(2) Uani 1 1 d . . . H10 H 0.3183 0.0105 0.8175 0.074 Uiso 1 1 calc R . . C11 C 0.1735(3) 0.0275(3) 0.5264(5) 0.0562(19) Uani 1 1 d . . . H11 H 0.2004 0.0277 0.5864 0.067 Uiso 1 1 calc R . . C12 C 0.1506(3) -0.0175(3) 0.4849(5) 0.0593(19) Uani 1 1 d . . . H12 H 0.1623 -0.0475 0.5173 0.071 Uiso 1 1 calc R . . C13 C 0.1115(3) -0.0176(3) 0.3981(6) 0.066(2) Uani 1 1 d . . . H13 H 0.0962 -0.0476 0.3704 0.079 Uiso 1 1 calc R . . C14 C 0.0940(3) 0.0280(3) 0.3497(6) 0.063(2) Uani 1 1 d . . . H14 H 0.0671 0.0287 0.2898 0.075 Uiso 1 1 calc R . . C15 C 0.1173(3) 0.0709(3) 0.3919(5) 0.0584(19) Uani 1 1 d . . . C16 C 0.1021(2) 0.1213(3) 0.3498(5) 0.0474(16) Uani 1 1 d . . . C17 C 0.0639(2) 0.1300(3) 0.2633(5) 0.0520(17) Uani 1 1 d . . . H17 H 0.0452 0.1032 0.2276 0.062 Uiso 1 1 calc R . . C18 C 0.0524(3) 0.1763(3) 0.2280(6) 0.070(2) Uani 1 1 d . . . H18 H 0.0256 0.1822 0.1692 0.084 Uiso 1 1 calc R . . C19 C 0.0815(3) 0.2150(3) 0.2810(5) 0.061(2) Uani 1 1 d . . . H19 H 0.0742 0.2478 0.2588 0.074 Uiso 1 1 calc R . . C20 C 0.1211(3) 0.2055(3) 0.3667(5) 0.0505(16) Uani 1 1 d . . . H20 H 0.1415 0.2317 0.4010 0.061 Uiso 1 1 calc R . . C21 C 0.2396(3) 0.3798(3) 0.5726(5) 0.0512(17) Uani 1 1 d . . . H21 H 0.2234 0.3501 0.5460 0.061 Uiso 1 1 calc R . . C22 C 0.2231(3) 0.4233(3) 0.5228(6) 0.065(2) Uani 1 1 d . . . H22 H 0.1963 0.4228 0.4627 0.077 Uiso 1 1 calc R . . C23 C 0.2461(3) 0.4674(3) 0.5612(6) 0.062(2) Uani 1 1 d . . . H23 H 0.2346 0.4975 0.5287 0.074 Uiso 1 1 calc R . . C24 C 0.2867(3) 0.4666(2) 0.6495(5) 0.0501(16) Uani 1 1 d . . . H24 H 0.3028 0.4963 0.6769 0.060 Uiso 1 1 calc R . . C25 C 0.3035(3) 0.4217(2) 0.6970(6) 0.0540(18) Uani 1 1 d . . . C26 C 0.3462(3) 0.4162(3) 0.7898(5) 0.0528(17) Uani 1 1 d . . . C27 C 0.3779(3) 0.4544(3) 0.8374(5) 0.0551(18) Uani 1 1 d . . . H27 H 0.3726 0.4865 0.8118 0.066 Uiso 1 1 calc R . . C28 C 0.4176(3) 0.4445(3) 0.9234(5) 0.0574(19) Uani 1 1 d . . . H28 H 0.4388 0.4702 0.9579 0.069 Uiso 1 1 calc R . . C29 C 0.4258(2) 0.3968(3) 0.9578(5) 0.0535(18) Uani 1 1 d . . . H29 H 0.4530 0.3902 1.0156 0.064 Uiso 1 1 calc R . . C30 C 0.3941(2) 0.3573(3) 0.9078(5) 0.0545(18) Uani 1 1 d . . . H30 H 0.3997 0.3247 0.9315 0.065 Uiso 1 1 calc R . . C31 C 0.2578(3) 0.1037(3) 0.8179(5) 0.0551(18) Uani 1 1 d . . . C32 C 0.2555(3) 0.0990(3) 0.9003(5) 0.0558(19) Uani 1 1 d . . . H32 H 0.2833 0.0964 0.9587 0.067 Uiso 1 1 calc R . . C33 C 0.2108(3) 0.0984(3) 0.8921(5) 0.0553(18) Uani 1 1 d . . . H33 H 0.2079 0.0951 0.9464 0.066 Uiso 1 1 calc R . . C34 C 0.1690(3) 0.1024(3) 0.8053(5) 0.0596(19) Uani 1 1 d . . . H34 H 0.1392 0.1017 0.8042 0.072 Uiso 1 1 calc R . . C35 C 0.1694(3) 0.1072(2) 0.7212(5) 0.0495(17) Uani 1 1 d . . . H35 H 0.1413 0.1096 0.6632 0.059 Uiso 1 1 calc R . . C36 C 0.2157(2) 0.1084(2) 0.7306(5) 0.0464(16) Uani 1 1 d . . . C37 C 0.2769(3) 0.1141(3) 0.7074(5) 0.0526(17) Uani 1 1 d . . . H37 H 0.2955 0.1180 0.6775 0.063 Uiso 1 1 calc R . . C38 C 0.1727(3) 0.2387(3) 0.6065(6) 0.0525(17) Uani 1 1 d . . . C39 C 0.1270(3) 0.2342(3) 0.5885(5) 0.0531(18) Uani 1 1 d . . . H39 H 0.1079 0.2075 0.5532 0.064 Uiso 1 1 calc R . . C40 C 0.1088(3) 0.2701(3) 0.6233(6) 0.0581(19) Uani 1 1 d . . . H40 H 0.0771 0.2671 0.6130 0.070 Uiso 1 1 calc R . . C41 C 0.1367(3) 0.3111(3) 0.6740(6) 0.064(2) Uani 1 1 d . . . H41 H 0.1233 0.3356 0.6952 0.076 Uiso 1 1 calc R . . C42 C 0.1847(3) 0.3152(3) 0.6929(5) 0.0579(19) Uani 1 1 d . . . H42 H 0.2037 0.3421 0.7276 0.070 Uiso 1 1 calc R . . C43 C 0.2034(3) 0.2788(3) 0.6593(5) 0.0482(16) Uani 1 1 d . . . C44 C 0.2448(3) 0.2315(3) 0.6163(5) 0.0500(17) Uani 1 1 d . . . H44 H 0.2708 0.2184 0.6113 0.060 Uiso 1 1 calc R . . C45 C 0.3240(2) 0.2596(2) 0.9179(5) 0.0446(15) Uani 1 1 d . . . C46 C 0.3069(3) 0.2936(3) 0.9591(5) 0.0540(18) Uani 1 1 d . . . H46 H 0.2970 0.3255 0.9344 0.065 Uiso 1 1 calc R . . C47 C 0.3053(3) 0.2775(3) 1.0402(5) 0.0580(19) Uani 1 1 d . . . H47 H 0.2925 0.2989 1.0680 0.070 Uiso 1 1 calc R . . C48 C 0.3218(3) 0.2320(3) 1.0793(7) 0.070(2) Uani 1 1 d . . . H48 H 0.3216 0.2237 1.1350 0.084 Uiso 1 1 calc R . . C49 C 0.3390(3) 0.1974(3) 1.0383(5) 0.0560(19) Uani 1 1 d . . . H49 H 0.3495 0.1658 1.0648 0.067 Uiso 1 1 calc R . . C50 C 0.3400(3) 0.2114(2) 0.9565(5) 0.0516(17) Uani 1 1 d . . . C51 C 0.3457(2) 0.2179(2) 0.8302(5) 0.0477(16) Uani 1 1 d . . . H51 H 0.3514 0.2095 0.7804 0.057 Uiso 1 1 calc R . . C52 C 0.3866(3) 0.0115(3) 0.1653(6) 0.061(2) Uani 1 1 d . . . H52A H 0.4196 0.0050 0.1803 0.092 Uiso 1 1 calc R . . H52B H 0.3653 -0.0102 0.1149 0.092 Uiso 1 1 calc R . . H52C H 0.3829 0.0055 0.2200 0.092 Uiso 1 1 calc R . . C53 C 0.4934(3) 0.8072(3) 0.0987(7) 0.070(2) Uani 1 1 d . . . H53A H 0.5265 0.7992 0.1428 0.105 Uiso 1 1 calc R . . H53B H 0.4878 0.8015 0.0355 0.105 Uiso 1 1 calc R . . H53C H 0.4722 0.7863 0.1108 0.105 Uiso 1 1 calc R . . N1 N 0.4327(2) 0.1143(2) 1.0120(4) 0.0601(17) Uani 1 1 d . . . N2 N 0.3785(2) 0.0383(2) 0.9150(4) 0.0486(13) Uani 1 1 d . . . N3 N 0.1566(2) 0.0703(2) 0.4793(4) 0.0499(14) Uani 1 1 d . . . N4 N 0.13066(17) 0.1599(2) 0.4007(4) 0.0413(12) Uani 1 1 d . . . N5 N 0.2779(2) 0.37882(19) 0.6574(4) 0.0419(12) Uani 1 1 d . . . N6 N 0.3543(2) 0.3688(2) 0.8225(4) 0.0537(15) Uani 1 1 d . . . N7 N 0.2966(2) 0.1068(2) 0.8016(4) 0.0481(14) Uani 1 1 d . . . N8 N 0.2294(2) 0.1153(2) 0.6616(4) 0.0492(13) Uani 1 1 d . . . N9 N 0.2015(2) 0.2097(2) 0.5795(4) 0.0439(13) Uani 1 1 d . . . N10 N 0.2468(2) 0.2741(2) 0.6611(4) 0.0474(13) Uani 1 1 d . . . N11 N 0.3286(2) 0.2622(2) 0.8367(4) 0.0487(13) Uani 1 1 d . . . N12 N 0.3543(2) 0.1863(2) 0.8997(4) 0.0492(14) Uani 1 1 d . . . N13 N 0.2699(2) 0.0663(3) 0.1490(5) 0.0614(17) Uani 1 1 d . . . N14 N 0.3750(3) 0.8522(3) 0.1504(5) 0.0622(17) Uani 1 1 d . . . N15 N 0.0373(2) 0.9158(2) 0.9726(5) 0.0584(16) Uani 1 1 d . . . O1 O 0.2368(2) 0.0798(2) 0.1654(4) 0.0647(15) Uani 1 1 d . . . O2 O 0.27690(19) 0.0223(2) 0.1393(4) 0.0619(14) Uani 1 1 d . . . O3 O 0.2971(2) 0.0985(2) 0.1444(4) 0.0638(14) Uani 1 1 d . . . O4 O 0.3935(2) 0.8658(2) 0.2340(4) 0.0664(15) Uani 1 1 d . . . O5 O 0.34141(19) 0.82204(19) 0.1169(4) 0.0561(12) Uani 1 1 d . . . O6 O 0.3977(2) 0.8627(2) 0.1060(4) 0.0646(15) Uani 1 1 d . . . O7 O 0.0533(2) 0.9353(2) 1.0517(4) 0.0646(14) Uani 1 1 d . . . O8 O 0.0444(2) 0.8715(2) 0.9646(4) 0.0650(15) Uani 1 1 d . . . O9 O 0.0160(2) 0.9437(2) 0.9010(4) 0.0770(19) Uani 1 1 d . . . O10 O 0.37522(18) 0.0609(2) 0.1372(4) 0.0601(13) Uani 1 1 d . . . H10A H 0.3711 0.0761 0.1769 0.090 Uiso 1 1 d R . . O11 O 0.4849(2) 0.8552(2) 0.1085(4) 0.0760(19) Uani 1 1 d . . . H11A H 0.4789 0.8551 0.1545 0.091 Uiso 1 1 d R . . O12 O 0.4848(5) 0.2745(6) 0.0143(10) 0.071(6) Uani 0.390(15) 1 d P . . H12D H 0.5128 0.2763 0.0190 0.085 Uiso 0.390(15) 1 d PR . . H12B H 0.4859 0.2857 0.0647 0.085 Uiso 0.390(15) 1 d PR . . O13 O 0.5370(5) 0.9238(6) 0.1908(11) 0.088(7) Uani 0.394(15) 1 d P . . H13A H 0.5114 0.9353 0.1893 0.106 Uiso 0.394(15) 1 d PR . . H13B H 0.5614 0.9304 0.2439 0.106 Uiso 0.394(15) 1 d PR . . O14 O 0.5000 0.5939(4) 0.7500 0.072(4) Uani 0.82(2) 2 d SP . . H14A H 0.5009 0.6214 0.7776 0.086 Uiso 0.41(1) 1 d PR . . H14C H 0.4759 0.5942 0.6945 0.086 Uiso 0.41(1) 1 d PR . . O15 O 0.0614(5) 0.8048(5) 0.3109(8) 0.066(5) Uani 0.407(15) 1 d P . . H15A H 0.0339 0.8009 0.3078 0.080 Uiso 0.407(15) 1 d PR . . H15B H 0.0749 0.7765 0.3173 0.080 Uiso 0.407(15) 1 d PR . . O16 O 0.4894(5) 0.5101(5) 0.8576(9) 0.069(5) Uani 0.397(15) 1 d P . . H16D H 0.4717 0.4938 0.8746 0.083 Uiso 0.397(15) 1 d PR . . H16C H 0.4796 0.5402 0.8452 0.083 Uiso 0.397(15) 1 d PR . . Pd1 Pd 0.365172(18) 0.112236(18) 0.90326(3) 0.04041(13) Uani 1 1 d . . . Pd2 Pd 0.182741(17) 0.139050(18) 0.53083(3) 0.03803(13) Uani 1 1 d . . . Pd3 Pd 0.303103(17) 0.318371(17) 0.74301(3) 0.03638(13) 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 0.050(4) 0.051(4) 0.058(4) 0.017(4) 0.008(3) -0.017(4) C2 0.053(4) 0.061(5) 0.066(5) 0.022(4) 0.004(4) -0.024(4) C3 0.039(4) 0.075(6) 0.070(5) 0.016(4) 0.008(4) -0.006(4) C4 0.036(4) 0.062(5) 0.070(5) 0.013(4) 0.011(3) 0.011(3) C5 0.047(4) 0.051(4) 0.046(4) 0.013(3) 0.013(3) 0.007(3) C6 0.037(4) 0.048(4) 0.077(5) 0.008(4) 0.016(4) 0.012(3) C7 0.062(5) 0.051(4) 0.045(4) 0.010(3) 0.008(4) 0.016(4) C8 0.069(5) 0.047(4) 0.051(4) 0.001(3) 0.017(4) 0.017(4) C9 0.062(5) 0.039(4) 0.056(4) -0.006(3) 0.016(4) 0.009(3) C10 0.068(5) 0.038(4) 0.054(4) 0.002(3) 0.008(4) 0.004(3) C11 0.072(5) 0.042(4) 0.043(4) -0.006(3) 0.019(4) -0.009(3) C12 0.065(5) 0.046(4) 0.055(4) -0.014(3) 0.019(4) -0.008(3) C13 0.064(5) 0.054(5) 0.062(5) -0.013(4) 0.015(4) -0.011(4) C14 0.066(5) 0.053(5) 0.049(4) -0.018(4) 0.013(4) -0.009(4) C15 0.050(4) 0.053(4) 0.052(4) -0.008(3) 0.008(3) -0.015(3) C16 0.028(3) 0.053(4) 0.051(4) -0.008(3) 0.010(3) -0.011(3) C17 0.034(3) 0.056(4) 0.051(4) -0.010(3) 0.008(3) -0.008(3) C18 0.062(5) 0.062(5) 0.063(5) 0.003(4) 0.012(4) -0.007(4) C19 0.068(5) 0.048(4) 0.052(4) 0.005(3) 0.016(4) 0.006(4) C20 0.062(4) 0.046(4) 0.040(3) 0.001(3) 0.022(3) 0.001(3) C21 0.055(4) 0.042(4) 0.042(4) 0.003(3) 0.012(3) 0.008(3) C22 0.066(5) 0.058(5) 0.047(4) 0.015(4) 0.009(4) -0.004(4) C23 0.069(5) 0.045(4) 0.061(5) 0.014(4) 0.023(4) 0.008(4) C24 0.062(4) 0.030(3) 0.057(4) 0.003(3) 0.028(4) -0.005(3) C25 0.051(4) 0.033(3) 0.062(4) 0.005(3) 0.014(3) -0.004(3) C26 0.059(4) 0.038(4) 0.049(4) -0.003(3) 0.016(3) -0.011(3) C27 0.061(5) 0.040(4) 0.052(4) -0.003(3) 0.017(4) -0.009(3) C28 0.053(4) 0.043(4) 0.058(4) -0.016(3) 0.013(4) -0.001(3) C29 0.038(4) 0.049(4) 0.056(4) -0.010(3) 0.009(3) 0.008(3) C30 0.037(3) 0.052(4) 0.057(4) 0.005(3) 0.010(3) -0.005(3) C31 0.044(4) 0.059(5) 0.045(4) -0.001(3) 0.007(3) -0.009(3) C32 0.053(4) 0.051(4) 0.049(4) 0.011(3) 0.012(3) -0.011(3) C33 0.052(4) 0.048(4) 0.051(4) 0.000(3) 0.013(3) -0.013(3) C34 0.053(4) 0.062(5) 0.052(4) 0.006(4) 0.016(3) 0.002(4) C35 0.045(4) 0.041(4) 0.047(4) -0.012(3) 0.010(3) -0.003(3) C36 0.046(4) 0.036(3) 0.041(3) -0.006(3) 0.007(3) -0.009(3) C37 0.048(4) 0.049(4) 0.045(4) 0.002(3) 0.010(3) -0.001(3) C38 0.050(4) 0.033(3) 0.065(5) -0.004(3) 0.020(4) -0.008(3) C39 0.047(4) 0.041(4) 0.058(4) 0.009(3) 0.014(3) -0.005(3) C40 0.050(4) 0.052(4) 0.064(5) 0.017(4) 0.021(4) 0.006(3) C41 0.052(4) 0.063(5) 0.061(5) -0.002(4) 0.015(4) 0.012(4) C42 0.056(4) 0.055(4) 0.053(4) -0.011(3) 0.017(3) 0.001(3) C43 0.048(4) 0.040(4) 0.047(4) -0.002(3) 0.016(3) -0.006(3) C44 0.045(4) 0.045(4) 0.043(4) -0.009(3) 0.008(3) -0.007(3) C45 0.044(4) 0.034(3) 0.041(4) 0.002(3) 0.009(3) -0.005(3) C46 0.065(5) 0.033(3) 0.054(4) -0.010(3) 0.021(4) -0.010(3) C47 0.056(4) 0.055(4) 0.054(4) 0.006(3) 0.019(4) 0.010(4) C48 0.074(6) 0.066(5) 0.067(5) 0.018(4) 0.032(5) 0.025(4) C49 0.056(4) 0.050(4) 0.052(4) 0.015(3) 0.018(4) 0.010(3) C50 0.067(5) 0.028(3) 0.045(4) 0.000(3) 0.016(3) -0.006(3) C51 0.045(4) 0.038(3) 0.049(4) 0.008(3) 0.015(3) 0.003(3) C52 0.060(5) 0.056(5) 0.054(4) -0.017(4) 0.016(4) -0.013(4) C53 0.068(5) 0.053(5) 0.072(6) -0.018(4) 0.020(4) -0.017(4) N1 0.050(3) 0.048(3) 0.052(4) 0.007(3) 0.001(3) 0.001(3) N2 0.050(3) 0.034(3) 0.051(3) 0.006(2) 0.016(3) 0.008(2) N3 0.061(4) 0.044(3) 0.036(3) -0.011(2) 0.016(3) -0.009(3) N4 0.029(2) 0.048(3) 0.040(3) -0.002(2) 0.011(2) -0.011(2) N5 0.054(3) 0.031(3) 0.034(3) -0.001(2) 0.017(2) -0.004(2) N6 0.057(4) 0.040(3) 0.045(3) -0.003(2) 0.009(3) -0.008(3) N7 0.043(3) 0.040(3) 0.045(3) 0.001(2) 0.009(3) 0.001(2) N8 0.046(3) 0.044(3) 0.041(3) -0.004(2) 0.008(2) -0.004(3) N9 0.054(3) 0.042(3) 0.031(3) -0.003(2) 0.017(2) -0.015(3) N10 0.044(3) 0.032(3) 0.051(3) 0.000(2) 0.011(3) -0.001(2) N11 0.051(3) 0.039(3) 0.044(3) 0.007(2) 0.013(3) 0.003(3) N12 0.053(3) 0.032(3) 0.049(3) 0.005(2) 0.014(3) 0.000(2) N13 0.049(4) 0.060(4) 0.053(4) -0.013(3) 0.007(3) -0.008(3) N14 0.062(4) 0.057(4) 0.054(4) 0.009(3) 0.017(3) 0.002(3) N15 0.056(4) 0.051(4) 0.055(4) -0.012(3) 0.016(3) -0.013(3) O1 0.052(3) 0.063(4) 0.060(3) -0.018(3) 0.012(3) -0.014(3) O2 0.054(3) 0.060(3) 0.056(3) -0.015(3) 0.014(2) -0.013(3) O3 0.058(3) 0.060(3) 0.060(3) -0.006(3) 0.018(3) -0.006(3) O4 0.064(3) 0.062(3) 0.065(4) -0.009(3) 0.026(3) -0.010(3) O5 0.051(3) 0.048(3) 0.059(3) 0.008(2) 0.018(2) 0.010(2) O6 0.062(3) 0.060(3) 0.052(3) 0.013(3) 0.011(3) -0.012(3) O7 0.063(3) 0.053(3) 0.056(3) -0.016(3) 0.011(3) -0.008(3) O8 0.067(3) 0.047(3) 0.060(3) -0.014(2) 0.014(3) -0.015(3) O9 0.057(3) 0.063(4) 0.056(3) -0.016(3) -0.016(3) 0.019(3) O10 0.048(3) 0.055(3) 0.065(3) -0.013(3) 0.018(2) -0.015(2) O11 0.059(3) 0.050(3) 0.058(3) -0.016(3) -0.020(3) -0.017(3) O12 0.058(9) 0.081(11) 0.060(9) 0.032(8) 0.017(7) 0.013(7) O13 0.057(9) 0.079(12) 0.061(10) 0.005(8) -0.026(7) 0.027(8) O14 0.062(6) 0.062(6) 0.047(5) 0.000 -0.009(4) 0.000 O15 0.054(8) 0.048(8) 0.046(7) -0.014(5) -0.017(6) 0.009(6) O16 0.078(10) 0.063(9) 0.057(9) -0.029(7) 0.025(8) -0.039(8) Pd1 0.0393(3) 0.0331(2) 0.0418(3) 0.00493(19) 0.0139(2) 0.00410(19) Pd2 0.0377(2) 0.0370(3) 0.0353(3) -0.00471(18) 0.0143(2) -0.00406(19) Pd3 0.0403(2) 0.0273(2) 0.0401(3) 0.00121(18) 0.0182(2) -0.00167(19) _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(10) . ? C1 C2 1.370(10) . ? C1 H1 0.9300 . ? C2 C3 1.422(12) . ? C2 H2 0.9300 . ? C3 C4 1.332(12) . ? C3 H3 0.9300 . ? C4 C5 1.381(10) . ? C4 H4 0.9300 . ? C5 N1 1.385(9) . ? C5 C6 1.457(11) . ? C6 N2 1.354(9) . ? C6 C7 1.374(10) . ? C7 C8 1.391(11) . ? C7 H7 0.9300 . ? C8 C9 1.375(10) . ? C8 H8 0.9300 . ? C9 C10 1.384(10) . ? C9 H9 0.9300 . ? C10 N2 1.317(9) . ? C10 H10 0.9300 . ? C11 N3 1.333(9) . ? C11 C12 1.395(10) . ? C11 H11 0.9300 . ? C12 C13 1.349(11) . ? C12 H12 0.9300 . ? C13 C14 1.408(12) . ? C13 H13 0.9300 . ? C14 C15 1.351(10) . ? C14 H14 0.9300 . ? C15 N3 1.357(9) . ? C15 C16 1.478(11) . ? C16 C17 1.355(10) . ? C16 N4 1.355(8) . ? C17 C18 1.336(11) . ? C17 H17 0.9300 . ? C18 C19 1.371(11) . ? C18 H18 0.9300 . ? C19 C20 1.368(10) . ? C19 H19 0.9300 . ? C20 N4 1.308(9) . ? C20 H20 0.9300 . ? C21 N5 1.318(8) . ? C21 C22 1.362(10) . ? C21 H21 0.9300 . ? C22 C23 1.366(11) . ? C22 H22 0.9300 . ? C23 C24 1.382(11) . ? C23 H23 0.9300 . ? C24 C25 1.383(9) . ? C24 H24 0.9300 . ? C25 N5 1.368(8) . ? C25 C26 1.461(10) . ? C26 N6 1.347(9) . ? C26 C27 1.373(10) . ? C27 C28 1.374(10) . ? C27 H27 0.9300 . ? C28 C29 1.362(10) . ? C28 H28 0.9300 . ? C29 C30 1.410(10) . ? C29 H29 0.9300 . ? C30 N6 1.378(9) . ? C30 H30 0.9300 . ? C31 N7 1.371(10) . ? C31 C32 1.372(11) . ? C31 C36 1.401(9) . ? C32 C33 1.348(11) . ? C32 H32 0.9300 . ? C33 C34 1.390(10) . ? C33 H33 0.9300 . ? C34 C35 1.370(11) . ? C34 H34 0.9300 . ? C35 C36 1.390(10) . ? C35 H35 0.9300 . ? C36 N8 1.388(10) . ? C37 N8 1.309(9) . ? C37 N7 1.351(9) . ? C37 H37 0.9300 . ? C38 C39 1.331(10) . ? C38 N9 1.412(9) . ? C38 C43 1.418(9) . ? C39 C40 1.369(11) . ? C39 H39 0.9300 . ? C40 C41 1.394(12) . ? C40 H40 0.9300 . ? C41 C42 1.394(12) . ? C41 H41 0.9300 . ? C42 C43 1.378(11) . ? C42 H42 0.9300 . ? C43 N10 1.359(9) . ? C44 N9 1.328(8) . ? C44 N10 1.332(9) . ? C44 H44 0.9300 . ? C45 C46 1.377(10) . ? C45 N11 1.388(9) . ? C45 C50 1.411(9) . ? C46 C47 1.402(11) . ? C46 H46 0.9300 . ? C47 C48 1.351(11) . ? C47 H47 0.9300 . ? C48 C49 1.389(12) . ? C48 H48 0.9300 . ? C49 C50 1.389(10) . ? C49 H49 0.9300 . ? C50 N12 1.374(10) . ? C51 N12 1.322(9) . ? C51 N11 1.326(9) . ? C51 H51 0.9300 . ? C52 O10 1.383(10) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 O11 1.334(10) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? N1 Pd1 2.002(6) . ? N2 Pd1 2.006(6) . ? N3 Pd2 2.018(6) . ? N4 Pd2 2.024(5) . ? N5 Pd3 2.021(5) . ? N6 Pd3 2.016(6) . ? N7 Pd1 1.990(6) . ? N8 Pd2 2.007(6) . ? N9 Pd2 2.017(5) . ? N10 Pd3 2.007(5) . ? N11 Pd3 2.002(5) . ? N12 Pd1 2.003(6) . ? N13 O2 1.219(9) . ? N13 O3 1.241(9) . ? N13 O1 1.246(9) . ? N14 O5 1.229(8) . ? N14 O4 1.239(9) . ? N14 O6 1.263(9) . ? N15 O8 1.219(8) . ? N15 O7 1.240(8) . ? N15 O9 1.264(9) . ? O10 H10A 0.8201 . ? O11 H11A 0.8499 . ? O12 H12D 0.8499 . ? O12 H12B 0.8500 . ? O13 H13A 0.8501 . ? O13 H13B 0.8501 . ? O14 H14A 0.8500 . ? O14 H14C 0.8500 . ? O15 H15A 0.8499 . ? O15 H15B 0.8498 . ? O16 H16D 0.8501 . ? O16 H16C 0.8499 . ? 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 123.3(8) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 116.2(8) . . ? C1 C2 H2 121.9 . . ? C3 C2 H2 121.9 . . ? C4 C3 C2 121.0(7) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 N1 119.3(7) . . ? C4 C5 C6 126.3(7) . . ? N1 C5 C6 114.3(6) . . ? N2 C6 C7 120.7(7) . . ? N2 C6 C5 116.2(6) . . ? C7 C6 C5 123.0(7) . . ? C6 C7 C8 120.8(7) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 117.5(7) . . ? C9 C8 H8 121.2 . . ? C7 C8 H8 121.2 . . ? C8 C9 C10 118.4(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 124.1(7) . . ? N2 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N3 C11 C12 119.4(7) . . ? N3 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.2(8) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.5(7) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 N3 121.1(8) . . ? C14 C15 C16 124.1(7) . . ? N3 C15 C16 114.8(6) . . ? C17 C16 N4 119.6(7) . . ? C17 C16 C15 124.1(6) . . ? N4 C16 C15 116.1(6) . . ? C18 C17 C16 121.5(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 118.0(8) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C20 C19 C18 120.0(8) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? N4 C20 C19 120.7(7) . . ? N4 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? N5 C21 C22 121.9(7) . . ? N5 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C21 C22 C23 119.9(7) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 118.6(7) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C23 C24 C25 120.1(7) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N5 C25 C24 118.9(6) . . ? N5 C25 C26 116.1(6) . . ? C24 C25 C26 124.9(6) . . ? N6 C26 C27 121.9(7) . . ? N6 C26 C25 113.7(6) . . ? C27 C26 C25 124.2(7) . . ? C26 C27 C28 119.0(7) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 119.6(7) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 121.5(7) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? N6 C30 C29 117.2(7) . . ? N6 C30 H30 121.4 . . ? C29 C30 H30 121.4 . . ? N7 C31 C32 131.3(7) . . ? N7 C31 C36 107.5(7) . . ? C32 C31 C36 121.2(7) . . ? C33 C32 C31 116.4(7) . . ? C33 C32 H32 121.8 . . ? C31 C32 H32 121.8 . . ? C32 C33 C34 122.4(8) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 123.3(8) . . ? C35 C34 H34 118.3 . . ? C33 C34 H34 118.3 . . ? C34 C35 C36 113.9(6) . . ? C34 C35 H35 123.1 . . ? C36 C35 H35 123.1 . . ? N8 C36 C35 129.2(6) . . ? N8 C36 C31 108.0(6) . . ? C35 C36 C31 122.8(7) . . ? N8 C37 N7 114.9(7) . . ? N8 C37 H37 122.5 . . ? N7 C37 H37 122.5 . . ? C39 C38 N9 132.2(7) . . ? C39 C38 C43 123.5(7) . . ? N9 C38 C43 104.3(6) . . ? C38 C39 C40 118.1(7) . . ? C38 C39 H39 120.9 . . ? C40 C39 H39 120.9 . . ? C39 C40 C41 121.3(8) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C40 120.1(8) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 118.8(7) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? N10 C43 C42 132.4(7) . . ? N10 C43 C38 109.3(6) . . ? C42 C43 C38 118.2(7) . . ? N9 C44 N10 112.9(7) . . ? N9 C44 H44 123.6 . . ? N10 C44 H44 123.6 . . ? C46 C45 N11 131.7(6) . . ? C46 C45 C50 121.7(7) . . ? N11 C45 C50 106.6(6) . . ? C45 C46 C47 116.6(7) . . ? C45 C46 H46 121.7 . . ? C47 C46 H46 121.7 . . ? C48 C47 C46 122.2(8) . . ? C48 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C47 C48 C49 121.7(8) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C48 C49 C50 117.8(7) . . ? C48 C49 H49 121.1 . . ? C50 C49 H49 121.1 . . ? N12 C50 C49 131.9(6) . . ? N12 C50 C45 108.1(6) . . ? C49 C50 C45 119.9(7) . . ? N12 C51 N11 115.1(7) . . ? N12 C51 H51 122.5 . . ? N11 C51 H51 122.5 . . ? O10 C52 H52A 109.5 . . ? O10 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O10 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O11 C53 H53A 109.5 . . ? O11 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O11 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C1 N1 C5 119.0(6) . . ? C1 N1 Pd1 127.2(5) . . ? C5 N1 Pd1 113.8(5) . . ? C10 N2 C6 118.2(6) . . ? C10 N2 Pd1 127.9(5) . . ? C6 N2 Pd1 113.8(5) . . ? C11 N3 C15 121.1(6) . . ? C11 N3 Pd2 124.9(5) . . ? C15 N3 Pd2 113.9(5) . . ? C20 N4 C16 120.1(6) . . ? C20 N4 Pd2 126.8(5) . . ? C16 N4 Pd2 112.9(5) . . ? C21 N5 C25 120.4(6) . . ? C21 N5 Pd3 126.0(5) . . ? C25 N5 Pd3 113.5(4) . . ? C26 N6 C30 120.7(6) . . ? C26 N6 Pd3 115.8(5) . . ? C30 N6 Pd3 123.4(5) . . ? C37 N7 C31 104.8(6) . . ? C37 N7 Pd1 130.3(5) . . ? C31 N7 Pd1 123.9(5) . . ? C37 N8 C36 104.8(6) . . ? C37 N8 Pd2 131.3(5) . . ? C36 N8 Pd2 122.2(5) . . ? C44 N9 C38 107.1(6) . . ? C44 N9 Pd2 128.9(5) . . ? C38 N9 Pd2 121.4(4) . . ? C44 N10 C43 106.4(6) . . ? C44 N10 Pd3 131.1(5) . . ? C43 N10 Pd3 121.2(5) . . ? C51 N11 C45 105.2(6) . . ? C51 N11 Pd3 129.6(5) . . ? C45 N11 Pd3 124.5(5) . . ? C51 N12 C50 105.0(6) . . ? C51 N12 Pd1 127.9(5) . . ? C50 N12 Pd1 124.7(5) . . ? O2 N13 O3 119.1(7) . . ? O2 N13 O1 121.9(7) . . ? O3 N13 O1 119.1(7) . . ? O5 N14 O4 121.6(7) . . ? O5 N14 O6 119.8(7) . . ? O4 N14 O6 117.2(7) . . ? O8 N15 O7 120.8(7) . . ? O8 N15 O9 121.2(6) . . ? O7 N15 O9 117.8(7) . . ? C52 O10 H10A 109.2 . . ? C53 O11 H11A 104.0 . . ? H12D O12 H12B 109.5 . . ? H13A O13 H13B 109.8 . . ? H14A O14 H14C 109.5 . . ? H15A O15 H15B 109.5 . . ? H16D O16 H16C 109.8 . . ? N7 Pd1 N1 175.4(3) . . ? N7 Pd1 N12 86.9(2) . . ? N1 Pd1 N12 95.4(2) . . ? N7 Pd1 N2 95.8(2) . . ? N1 Pd1 N2 81.8(2) . . ? N12 Pd1 N2 176.7(2) . . ? N8 Pd2 N9 87.5(2) . . ? N8 Pd2 N3 95.4(2) . . ? N9 Pd2 N3 173.8(3) . . ? N8 Pd2 N4 174.6(2) . . ? N9 Pd2 N4 94.9(2) . . ? N3 Pd2 N4 81.7(2) . . ? N11 Pd3 N10 87.8(2) . . ? N11 Pd3 N6 96.4(2) . . ? N10 Pd3 N6 173.8(2) . . ? N11 Pd3 N5 175.1(2) . . ? N10 Pd3 N5 95.1(2) . . ? N6 Pd3 N5 80.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 2.9(14) . . . . ? C1 C2 C3 C4 -5.2(14) . . . . ? C2 C3 C4 C5 6.8(15) . . . . ? C3 C4 C5 N1 -5.9(13) . . . . ? C3 C4 C5 C6 178.8(9) . . . . ? C4 C5 C6 N2 176.3(8) . . . . ? N1 C5 C6 N2 0.8(11) . . . . ? C4 C5 C6 C7 -5.9(14) . . . . ? N1 C5 C6 C7 178.5(8) . . . . ? N2 C6 C7 C8 -5.0(13) . . . . ? C5 C6 C7 C8 177.4(8) . . . . ? C6 C7 C8 C9 5.6(13) . . . . ? C7 C8 C9 C10 -5.2(13) . . . . ? C8 C9 C10 N2 4.4(14) . . . . ? N3 C11 C12 C13 -0.4(13) . . . . ? C11 C12 C13 C14 0.1(14) . . . . ? C12 C13 C14 C15 0.2(14) . . . . ? C13 C14 C15 N3 -0.1(13) . . . . ? C13 C14 C15 C16 -178.5(8) . . . . ? C14 C15 C16 C17 -1.7(13) . . . . ? N3 C15 C16 C17 179.8(7) . . . . ? C14 C15 C16 N4 -177.7(8) . . . . ? N3 C15 C16 N4 3.8(10) . . . . ? N4 C16 C17 C18 -2.7(12) . . . . ? C15 C16 C17 C18 -178.5(8) . . . . ? C16 C17 C18 C19 1.8(14) . . . . ? C17 C18 C19 C20 0.9(14) . . . . ? C18 C19 C20 N4 -2.9(13) . . . . ? N5 C21 C22 C23 -0.9(13) . . . . ? C21 C22 C23 C24 2.0(14) . . . . ? C22 C23 C24 C25 0.1(13) . . . . ? C23 C24 C25 N5 -3.2(12) . . . . ? C23 C24 C25 C26 179.3(8) . . . . ? N5 C25 C26 N6 0.6(11) . . . . ? C24 C25 C26 N6 178.2(8) . . . . ? N5 C25 C26 C27 175.6(8) . . . . ? C24 C25 C26 C27 -6.8(14) . . . . ? N6 C26 C27 C28 -3.8(13) . . . . ? C25 C26 C27 C28 -178.3(8) . . . . ? C26 C27 C28 C29 2.7(12) . . . . ? C27 C28 C29 C30 -0.9(12) . . . . ? C28 C29 C30 N6 0.1(12) . . . . ? N7 C31 C32 C33 178.2(8) . . . . ? C36 C31 C32 C33 1.0(11) . . . . ? C31 C32 C33 C34 -0.2(12) . . . . ? C32 C33 C34 C35 0.0(13) . . . . ? C33 C34 C35 C36 -0.7(11) . . . . ? C34 C35 C36 N8 -176.5(7) . . . . ? C34 C35 C36 C31 1.5(10) . . . . ? N7 C31 C36 N8 -1.2(8) . . . . ? C32 C31 C36 N8 176.6(7) . . . . ? N7 C31 C36 C35 -179.6(6) . . . . ? C32 C31 C36 C35 -1.8(11) . . . . ? N9 C38 C39 C40 -178.0(7) . . . . ? C43 C38 C39 C40 -0.4(12) . . . . ? C38 C39 C40 C41 1.8(12) . . . . ? C39 C40 C41 C42 -2.2(12) . . . . ? C40 C41 C42 C43 1.1(13) . . . . ? C41 C42 C43 N10 175.4(8) . . . . ? C41 C42 C43 C38 0.2(11) . . . . ? C39 C38 C43 N10 -176.8(7) . . . . ? N9 C38 C43 N10 1.3(8) . . . . ? C39 C38 C43 C42 -0.6(12) . . . . ? N9 C38 C43 C42 177.5(7) . . . . ? N11 C45 C46 C47 177.1(7) . . . . ? C50 C45 C46 C47 -1.3(11) . . . . ? C45 C46 C47 C48 3.1(12) . . . . ? C46 C47 C48 C49 -3.4(14) . . . . ? C47 C48 C49 C50 1.7(13) . . . . ? C48 C49 C50 N12 -179.4(8) . . . . ? C48 C49 C50 C45 0.1(11) . . . . ? C46 C45 C50 N12 179.4(6) . . . . ? N11 C45 C50 N12 0.6(8) . . . . ? C46 C45 C50 C49 -0.3(11) . . . . ? N11 C45 C50 C49 -179.0(7) . . . . ? C2 C1 N1 C5 -2.1(13) . . . . ? C2 C1 N1 Pd1 175.1(7) . . . . ? C4 C5 N1 C1 3.4(12) . . . . ? C6 C5 N1 C1 179.3(8) . . . . ? C4 C5 N1 Pd1 -174.2(6) . . . . ? C6 C5 N1 Pd1 1.7(9) . . . . ? C9 C10 N2 C6 -3.5(13) . . . . ? C9 C10 N2 Pd1 -178.4(7) . . . . ? C7 C6 N2 C10 3.8(12) . . . . ? C5 C6 N2 C10 -178.4(8) . . . . ? C7 C6 N2 Pd1 179.3(7) . . . . ? C5 C6 N2 Pd1 -2.9(9) . . . . ? C12 C11 N3 C15 0.4(12) . . . . ? C12 C11 N3 Pd2 176.5(6) . . . . ? C14 C15 N3 C11 -0.1(12) . . . . ? C16 C15 N3 C11 178.4(7) . . . . ? C14 C15 N3 Pd2 -176.6(7) . . . . ? C16 C15 N3 Pd2 1.9(9) . . . . ? C19 C20 N4 C16 2.1(11) . . . . ? C19 C20 N4 Pd2 -172.9(6) . . . . ? C17 C16 N4 C20 0.7(10) . . . . ? C15 C16 N4 C20 176.8(7) . . . . ? C17 C16 N4 Pd2 176.3(6) . . . . ? C15 C16 N4 Pd2 -7.6(8) . . . . ? C22 C21 N5 C25 -2.3(12) . . . . ? C22 C21 N5 Pd3 175.0(6) . . . . ? C24 C25 N5 C21 4.3(11) . . . . ? C26 C25 N5 C21 -178.0(7) . . . . ? C24 C25 N5 Pd3 -173.3(6) . . . . ? C26 C25 N5 Pd3 4.4(9) . . . . ? C27 C26 N6 C30 3.0(12) . . . . ? C25 C26 N6 C30 178.1(7) . . . . ? C27 C26 N6 Pd3 179.4(6) . . . . ? C25 C26 N6 Pd3 -5.5(9) . . . . ? C29 C30 N6 C26 -1.1(11) . . . . ? C29 C30 N6 Pd3 -177.2(6) . . . . ? N8 C37 N7 C31 -1.0(8) . . . . ? N8 C37 N7 Pd1 -169.5(5) . . . . ? C32 C31 N7 C37 -176.2(8) . . . . ? C36 C31 N7 C37 1.3(8) . . . . ? C32 C31 N7 Pd1 -6.7(12) . . . . ? C36 C31 N7 Pd1 170.8(5) . . . . ? N7 C37 N8 C36 0.2(8) . . . . ? N7 C37 N8 Pd2 165.1(5) . . . . ? C35 C36 N8 C37 178.8(7) . . . . ? C31 C36 N8 C37 0.6(8) . . . . ? C35 C36 N8 Pd2 12.2(10) . . . . ? C31 C36 N8 Pd2 -166.0(5) . . . . ? N10 C44 N9 C38 -3.6(8) . . . . ? N10 C44 N9 Pd2 -165.1(4) . . . . ? C39 C38 N9 C44 179.2(8) . . . . ? C43 C38 N9 C44 1.3(8) . . . . ? C39 C38 N9 Pd2 -17.6(11) . . . . ? C43 C38 N9 Pd2 164.5(4) . . . . ? N9 C44 N10 C43 4.4(8) . . . . ? N9 C44 N10 Pd3 171.3(5) . . . . ? C42 C43 N10 C44 -178.8(8) . . . . ? C38 C43 N10 C44 -3.4(8) . . . . ? C42 C43 N10 Pd3 12.7(11) . . . . ? C38 C43 N10 Pd3 -171.8(5) . . . . ? N12 C51 N11 C45 -1.6(8) . . . . ? N12 C51 N11 Pd3 -171.9(5) . . . . ? C46 C45 N11 C51 -178.0(7) . . . . ? C50 C45 N11 C51 0.5(7) . . . . ? C46 C45 N11 Pd3 -7.1(11) . . . . ? C50 C45 N11 Pd3 171.5(5) . . . . ? N11 C51 N12 C50 2.0(8) . . . . ? N11 C51 N12 Pd1 164.6(5) . . . . ? C49 C50 N12 C51 178.1(8) . . . . ? C45 C50 N12 C51 -1.5(8) . . . . ? C49 C50 N12 Pd1 14.7(12) . . . . ? C45 C50 N12 Pd1 -164.9(4) . . . . ? C37 N7 Pd1 N12 80.9(6) . . . . ? C31 N7 Pd1 N12 -85.7(6) . . . . ? C37 N7 Pd1 N2 -101.1(6) . . . . ? C31 N7 Pd1 N2 92.2(6) . . . . ? C1 N1 Pd1 N12 -1.7(8) . . . . ? C5 N1 Pd1 N12 175.6(6) . . . . ? C1 N1 Pd1 N2 -179.9(8) . . . . ? C5 N1 Pd1 N2 -2.5(6) . . . . ? C51 N12 Pd1 N7 -66.3(6) . . . . ? C50 N12 Pd1 N7 93.1(6) . . . . ? C51 N12 Pd1 N1 117.6(6) . . . . ? C50 N12 Pd1 N1 -82.9(6) . . . . ? C10 N2 Pd1 N7 1.9(7) . . . . ? C6 N2 Pd1 N7 -173.1(6) . . . . ? C10 N2 Pd1 N1 178.0(8) . . . . ? C6 N2 Pd1 N1 3.0(6) . . . . ? C37 N8 Pd2 N9 -73.9(7) . . . . ? C36 N8 Pd2 N9 88.8(5) . . . . ? C37 N8 Pd2 N3 111.7(7) . . . . ? C36 N8 Pd2 N3 -85.6(5) . . . . ? C44 N9 Pd2 N8 60.9(6) . . . . ? C38 N9 Pd2 N8 -98.3(5) . . . . ? C44 N9 Pd2 N4 -124.0(6) . . . . ? C38 N9 Pd2 N4 76.8(5) . . . . ? C11 N3 Pd2 N8 -5.6(7) . . . . ? C15 N3 Pd2 N8 170.8(6) . . . . ? C11 N3 Pd2 N4 179.1(7) . . . . ? C15 N3 Pd2 N4 -4.6(5) . . . . ? C20 N4 Pd2 N9 7.2(6) . . . . ? C16 N4 Pd2 N9 -168.0(5) . . . . ? C20 N4 Pd2 N3 -178.1(6) . . . . ? C16 N4 Pd2 N3 6.6(5) . . . . ? C51 N11 Pd3 N10 67.9(6) . . . . ? C45 N11 Pd3 N10 -100.8(6) . . . . ? C51 N11 Pd3 N6 -116.6(6) . . . . ? C45 N11 Pd3 N6 74.7(6) . . . . ? C44 N10 Pd3 N11 -66.0(7) . . . . ? C43 N10 Pd3 N11 99.2(5) . . . . ? C44 N10 Pd3 N5 117.9(7) . . . . ? C43 N10 Pd3 N5 -76.9(5) . . . . ? C26 N6 Pd3 N11 -170.1(6) . . . . ? C30 N6 Pd3 N11 6.3(7) . . . . ? C26 N6 Pd3 N5 6.2(6) . . . . ? C30 N6 Pd3 N5 -177.5(7) . . . . ? C21 N5 Pd3 N10 -7.3(6) . . . . ? C25 N5 Pd3 N10 170.1(5) . . . . ? C21 N5 Pd3 N6 176.9(6) . . . . ? C25 N5 Pd3 N6 -5.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.483 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.101 # Attachment '1870Revised.cif' data_1870 _database_code_depnum_ccdc_archive 'CCDC 757501' #TrackingRef '1870Revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C81 H81 N12 O15 Pd3, 3(N O3), 4.0(H2 O)' _chemical_formula_sum 'C81 H89 N15 O28 Pd3' _chemical_formula_weight 2039.87 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 12.5206(6) _cell_length_b 20.1546(12) _cell_length_c 20.5334(10) _cell_angle_alpha 97.11(3) _cell_angle_beta 105.17(3) _cell_angle_gamma 96.58(2) _cell_volume 4903.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6936 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.18 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7977 _exptl_absorpt_correction_T_max 0.8751 _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 35288 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 19265 _reflns_number_gt 13343 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.06P)^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 19265 _refine_ls_number_parameters 1208 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.3688(4) 0.5424(3) 0.7825(3) 0.0594(12) Uani 1 1 d . . . H1 H 0.3447 0.5812 0.7673 0.071 Uiso 1 1 calc R . . C2 C 0.3367(5) 0.5180(3) 0.8373(3) 0.0621(13) Uani 1 1 d . . . H2 H 0.2939 0.5421 0.8595 0.075 Uiso 1 1 calc R . . C3 C 0.3670(5) 0.4607(3) 0.8579(3) 0.0670(14) Uani 1 1 d . . . H3 H 0.3427 0.4452 0.8932 0.080 Uiso 1 1 calc R . . C4 C 0.4348(5) 0.4232(3) 0.8274(3) 0.0605(13) Uani 1 1 d . . . C5 C 0.4728(4) 0.3636(3) 0.8447(3) 0.0583(12) Uani 1 1 d . . . C6 C 0.5314(4) 0.3271(3) 0.8093(3) 0.0587(12) Uani 1 1 d . . . C7 C 0.5533(4) 0.3515(3) 0.7522(3) 0.0572(12) Uani 1 1 d . . . C8 C 0.6098(4) 0.3175(3) 0.7075(3) 0.0626(13) Uani 1 1 d . . . H8 H 0.6311 0.2759 0.7153 0.075 Uiso 1 1 calc R . . C9 C 0.6316(5) 0.3445(3) 0.6558(3) 0.0644(13) Uani 1 1 d . . . H9 H 0.6689 0.3220 0.6283 0.077 Uiso 1 1 calc R . . C10 C 0.5986(5) 0.4070(3) 0.6426(3) 0.0663(14) Uani 1 1 d . . . H10 H 0.6133 0.4254 0.6059 0.080 Uiso 1 1 calc R . . C11 C 0.5234(4) 0.4135(2) 0.7337(3) 0.0583(12) Uani 1 1 d . . . C12 C 0.4634(4) 0.4499(2) 0.7724(3) 0.0570(12) Uani 1 1 d . . . C13 C 0.7653(4) 0.5339(2) 0.4236(3) 0.0567(12) Uani 1 1 d . . . H13 H 0.7413 0.5152 0.4574 0.068 Uiso 1 1 calc R . . C14 C 0.8267(4) 0.4978(3) 0.3890(3) 0.0567(12) Uani 1 1 d . . . H14 H 0.8416 0.4554 0.3989 0.068 Uiso 1 1 calc R . . C15 C 0.8662(5) 0.5256(3) 0.3390(3) 0.0593(12) Uani 1 1 d . . . H15 H 0.9106 0.5031 0.3166 0.071 Uiso 1 1 calc R . . C16 C 0.8378(4) 0.5882(2) 0.3232(3) 0.0568(12) Uani 1 1 d . . . C17 C 0.8717(5) 0.6207(3) 0.2728(3) 0.0649(13) Uani 1 1 d . . . C18 C 0.8401(5) 0.6834(3) 0.2605(3) 0.0654(14) Uani 1 1 d . . . C19 C 0.7771(5) 0.7148(3) 0.2997(3) 0.0606(13) Uani 1 1 d . . . C20 C 0.7398(5) 0.7777(3) 0.2858(3) 0.0634(13) Uani 1 1 d . . . H20 H 0.7560 0.7993 0.2512 0.076 Uiso 1 1 calc R . . C21 C 0.6783(5) 0.8043(3) 0.3270(3) 0.0641(13) Uani 1 1 d . . . H21 H 0.6531 0.8453 0.3204 0.077 Uiso 1 1 calc R . . C22 C 0.6531(5) 0.7711(3) 0.3786(3) 0.0630(13) Uani 1 1 d . . . H22 H 0.6134 0.7910 0.4062 0.076 Uiso 1 1 calc R . . C23 C 0.7458(4) 0.6841(2) 0.3492(2) 0.0525(11) Uani 1 1 d . . . C24 C 0.7758(4) 0.6208(2) 0.3616(3) 0.0551(11) Uani 1 1 d . . . C25 C 0.3844(4) 0.9147(3) 0.5243(3) 0.0582(12) Uani 1 1 d . . . H25 H 0.4365 0.8956 0.5060 0.070 Uiso 1 1 calc R . . C26 C 0.3461(4) 0.9735(3) 0.5037(3) 0.0594(12) Uani 1 1 d . . . H26 H 0.3725 0.9920 0.4705 0.071 Uiso 1 1 calc R . . C27 C 0.2735(4) 1.0046(3) 0.5292(3) 0.0572(12) Uani 1 1 d . . . H27 H 0.2519 1.0444 0.5151 0.069 Uiso 1 1 calc R . . C28 C 0.2314(4) 0.9761(2) 0.5772(3) 0.0538(11) Uani 1 1 d . . . C29 C 0.1552(4) 1.0033(2) 0.6115(3) 0.0553(12) Uani 1 1 d . . . C30 C 0.1185(4) 0.9716(3) 0.6584(3) 0.0595(12) Uani 1 1 d . . . C31 C 0.1533(4) 0.9103(3) 0.6745(3) 0.0606(13) Uani 1 1 d . . . C32 C 0.1116(5) 0.8727(3) 0.7190(3) 0.0664(14) Uani 1 1 d . . . H32 H 0.0547 0.8863 0.7365 0.080 Uiso 1 1 calc R . . C33 C 0.1572(4) 0.8149(3) 0.7361(3) 0.0594(12) Uani 1 1 d . . . H33 H 0.1353 0.7914 0.7679 0.071 Uiso 1 1 calc R . . C34 C 0.2362(5) 0.7930(3) 0.7048(3) 0.0657(14) Uani 1 1 d . . . H34 H 0.2641 0.7536 0.7149 0.079 Uiso 1 1 calc R . . C35 C 0.2713(4) 0.9171(2) 0.5984(3) 0.0552(12) Uani 1 1 d . . . C36 C 0.2320(4) 0.8851(3) 0.6468(3) 0.0571(12) Uani 1 1 d . . . C37 C 0.7144(5) 0.5728(3) 0.6395(3) 0.0610(13) Uani 1 1 d . . . C38 C 0.7865(5) 0.5624(3) 0.6984(3) 0.0616(13) Uani 1 1 d . . . H38 H 0.7613 0.5445 0.7323 0.074 Uiso 1 1 calc R . . C39 C 0.9025(5) 0.5805(3) 0.7050(3) 0.0665(14) Uani 1 1 d . . . H39 H 0.9550 0.5740 0.7442 0.080 Uiso 1 1 calc R . . C40 C 0.9382(5) 0.6071(3) 0.6551(3) 0.0704(15) Uani 1 1 d . . . H40 H 1.0148 0.6184 0.6614 0.084 Uiso 1 1 calc R . . C41 C 0.8653(5) 0.6180(3) 0.5957(3) 0.0625(13) Uani 1 1 d . . . H41 H 0.8907 0.6375 0.5627 0.075 Uiso 1 1 calc R . . C42 C 0.7503(5) 0.5981(3) 0.5874(3) 0.0609(13) Uani 1 1 d . . . C43 C 0.5695(5) 0.5787(2) 0.5555(3) 0.0595(12) Uani 1 1 d . . . H43 H 0.4957 0.5760 0.5294 0.071 Uiso 1 1 calc R . . C44 C 0.6727(4) 0.7910(2) 0.5466(3) 0.0546(11) Uani 1 1 d . . . C45 C 0.7820(4) 0.8157(3) 0.5516(3) 0.0624(13) Uani 1 1 d . . . H45 H 0.8238 0.7918 0.5284 0.075 Uiso 1 1 calc R . . C46 C 0.8272(5) 0.8777(3) 0.5925(3) 0.0620(13) Uani 1 1 d . . . H46 H 0.9019 0.8947 0.5983 0.074 Uiso 1 1 calc R . . C47 C 0.7656(5) 0.9148(3) 0.6249(3) 0.0606(12) Uani 1 1 d . . . H47 H 0.7984 0.9571 0.6503 0.073 Uiso 1 1 calc R . . C48 C 0.6559(4) 0.8909(3) 0.6208(3) 0.0587(12) Uani 1 1 d . . . H48 H 0.6144 0.9161 0.6431 0.070 Uiso 1 1 calc R . . C49 C 0.6089(4) 0.8267(2) 0.5814(3) 0.0525(11) Uani 1 1 d . . . C50 C 0.5070(4) 0.7332(2) 0.5236(3) 0.0567(12) Uani 1 1 d . . . H50 H 0.4459 0.6989 0.5062 0.068 Uiso 1 1 calc R . . C51 C 0.5004(4) 0.7417(2) 0.7320(3) 0.0546(11) Uani 1 1 d . . . C52 C 0.5382(5) 0.8001(3) 0.7757(3) 0.0676(14) Uani 1 1 d . . . H52 H 0.5191 0.8413 0.7644 0.081 Uiso 1 1 calc R . . C53 C 0.6078(5) 0.7945(3) 0.8392(3) 0.0726(15) Uani 1 1 d . . . H53 H 0.6364 0.8339 0.8708 0.087 Uiso 1 1 calc R . . C54 C 0.6368(5) 0.7355(3) 0.8580(3) 0.0679(14) Uani 1 1 d . . . H54 H 0.6822 0.7351 0.9017 0.081 Uiso 1 1 calc R . . C55 C 0.5982(4) 0.6745(3) 0.8111(3) 0.0579(12) Uani 1 1 d . . . H55 H 0.6193 0.6336 0.8220 0.070 Uiso 1 1 calc R . . C56 C 0.5261(5) 0.6792(3) 0.7473(3) 0.0609(13) Uani 1 1 d . . . C57 C 0.4191(4) 0.6639(2) 0.6432(3) 0.0574(12) Uani 1 1 d . . . H57 H 0.3777 0.6428 0.5995 0.069 Uiso 1 1 calc R . . C58 C 0.5208(5) 0.3706(3) 0.9661(3) 0.0672(14) Uani 1 1 d . . . H58A H 0.5239 0.4194 0.9724 0.081 Uiso 1 1 calc R . . H58B H 0.5958 0.3604 0.9701 0.081 Uiso 1 1 calc R . . C59 C 0.4736(5) 0.3410(3) 1.0189(3) 0.0650(13) Uani 1 1 d . . . H59A H 0.5078 0.3681 1.0636 0.078 Uiso 1 1 calc R . . H59B H 0.3935 0.3414 1.0075 0.078 Uiso 1 1 calc R . . C60 C 0.5965(5) 0.2658(3) 1.0674(3) 0.0746(16) Uani 1 1 d . . . H60A H 0.5972 0.2857 1.1131 0.090 Uiso 1 1 calc R . . H60B H 0.6595 0.2896 1.0562 0.090 Uiso 1 1 calc R . . C61 C 0.6096(5) 0.1915(3) 1.0666(3) 0.0646(13) Uani 1 1 d . . . H61A H 0.6763 0.1877 1.1019 0.078 Uiso 1 1 calc R . . H61B H 0.5457 0.1674 1.0766 0.078 Uiso 1 1 calc R . . C62 C 0.7301(5) 0.1727(3) 1.0008(3) 0.0625(13) Uani 1 1 d . . . H62A H 0.7788 0.1556 1.0378 0.075 Uiso 1 1 calc R . . H62B H 0.7560 0.2204 1.0034 0.075 Uiso 1 1 calc R . . C63 C 0.7248(5) 0.1322(3) 0.9304(3) 0.0620(13) Uani 1 1 d . . . H63A H 0.7978 0.1198 0.9317 0.074 Uiso 1 1 calc R . . H63B H 0.6720 0.0908 0.9218 0.074 Uiso 1 1 calc R . . C64 C 0.5740(5) 0.1580(3) 0.8445(3) 0.0627(13) Uani 1 1 d . . . H64A H 0.5386 0.1233 0.8642 0.075 Uiso 1 1 calc R . . H64B H 0.5587 0.1422 0.7959 0.075 Uiso 1 1 calc R . . C65 C 0.5264(5) 0.2226(3) 0.8555(3) 0.0591(12) Uani 1 1 d . . . H65A H 0.4456 0.2140 0.8373 0.071 Uiso 1 1 calc R . . H65B H 0.5448 0.2398 0.9040 0.071 Uiso 1 1 calc R . . C66 C 1.0503(4) 0.5990(3) 0.2667(3) 0.0639(13) Uani 1 1 d . . . H66A H 1.0683 0.5728 0.3036 0.077 Uiso 1 1 calc R . . H66B H 1.0771 0.6464 0.2853 0.077 Uiso 1 1 calc R . . C67 C 1.1055(5) 0.5765(3) 0.2121(3) 0.0626(13) Uani 1 1 d . . . H67A H 1.1814 0.5696 0.2332 0.075 Uiso 1 1 calc R . . H67B H 1.0643 0.5341 0.1849 0.075 Uiso 1 1 calc R . . C68 C 1.1479(5) 0.6055(3) 0.1143(3) 0.0625(13) Uani 1 1 d . . . H68A H 1.1015 0.5643 0.0874 0.075 Uiso 1 1 calc R . . H68B H 1.2236 0.5960 0.1309 0.075 Uiso 1 1 calc R . . C69 C 1.1471(5) 0.6606(3) 0.0697(3) 0.0652(14) Uani 1 1 d . . . H69A H 1.1830 0.7039 0.0975 0.078 Uiso 1 1 calc R . . H69B H 1.1870 0.6499 0.0360 0.078 Uiso 1 1 calc R . . C70 C 1.0240(5) 0.7309(3) 0.0277(3) 0.0625(13) Uani 1 1 d . . . H70A H 1.0677 0.7455 -0.0020 0.075 Uiso 1 1 calc R . . H70B H 1.0492 0.7610 0.0713 0.075 Uiso 1 1 calc R . . C71 C 0.8993(4) 0.7293(3) -0.0050(3) 0.0633(13) Uani 1 1 d . . . H71A H 0.8856 0.7750 -0.0102 0.076 Uiso 1 1 calc R . . H71B H 0.8786 0.7026 -0.0503 0.076 Uiso 1 1 calc R . . C72 C 0.8419(5) 0.7378(3) 0.0990(3) 0.0649(13) Uani 1 1 d . . . H72A H 0.7755 0.7577 0.1005 0.078 Uiso 1 1 calc R . . H72B H 0.9059 0.7736 0.1114 0.078 Uiso 1 1 calc R . . C73 C 0.8601(5) 0.6854(3) 0.1471(3) 0.0623(13) Uani 1 1 d . . . H73A H 0.7962 0.6496 0.1337 0.075 Uiso 1 1 calc R . . H73B H 0.9262 0.6655 0.1446 0.075 Uiso 1 1 calc R . . C74 C 0.0128(4) 1.0746(3) 0.5858(3) 0.0612(13) Uani 1 1 d . . . H74A H 0.0004 1.0823 0.6306 0.073 Uiso 1 1 calc R . . H74B H -0.0404 1.0361 0.5583 0.073 Uiso 1 1 calc R . . C75 C -0.0005(5) 1.1367(3) 0.5519(3) 0.0656(14) Uani 1 1 d . . . H75A H 0.0582 1.1738 0.5767 0.079 Uiso 1 1 calc R . . H75B H 0.0040 1.1274 0.5053 0.079 Uiso 1 1 calc R . . C76 C -0.0877(5) 1.2069(3) 0.6071(3) 0.0632(13) Uani 1 1 d . . . H76A H -0.0601 1.2489 0.5943 0.076 Uiso 1 1 calc R . . H76B H -0.0321 1.1984 0.6467 0.076 Uiso 1 1 calc R . . C77 C -0.1962(5) 1.2129(3) 0.6244(3) 0.0626(13) Uani 1 1 d . . . H77A H -0.1892 1.2574 0.6505 0.075 Uiso 1 1 calc R . . H77B H -0.2546 1.2103 0.5820 0.075 Uiso 1 1 calc R . . C78 C -0.1851(5) 1.1799(3) 0.7341(3) 0.0643(13) Uani 1 1 d . . . H78A H -0.2409 1.1960 0.7546 0.077 Uiso 1 1 calc R . . H78B H -0.1222 1.2162 0.7445 0.077 Uiso 1 1 calc R . . C79 C -0.1461(5) 1.1199(3) 0.7652(3) 0.0631(13) Uani 1 1 d . . . H79A H -0.1257 1.1307 0.8146 0.076 Uiso 1 1 calc R . . H79B H -0.2062 1.0817 0.7508 0.076 Uiso 1 1 calc R . . C80 C 0.0012(5) 1.0567(3) 0.7841(3) 0.0620(13) Uani 1 1 d . . . H80A H -0.0513 1.0168 0.7826 0.074 Uiso 1 1 calc R . . H80B H 0.0336 1.0780 0.8314 0.074 Uiso 1 1 calc R . . C81 C 0.0916(5) 1.0382(3) 0.7518(3) 0.0648(13) Uani 1 1 d . . . H81A H 0.1339 1.0790 0.7451 0.078 Uiso 1 1 calc R . . H81B H 0.1427 1.0151 0.7818 0.078 Uiso 1 1 calc R . . N1 N 0.4339(4) 0.5090(2) 0.7532(2) 0.0630(11) Uani 1 1 d . . . N2 N 0.5464(4) 0.4402(2) 0.6820(2) 0.0607(11) Uani 1 1 d . . . N3 N 0.7392(4) 0.5929(2) 0.4113(2) 0.0579(10) Uani 1 1 d . . . N4 N 0.6846(4) 0.7124(2) 0.3886(2) 0.0558(10) Uani 1 1 d . . . N5 N 0.3455(3) 0.88660(19) 0.5702(2) 0.0506(9) Uani 1 1 d . . . N6 N 0.2725(4) 0.8259(2) 0.6617(2) 0.0607(11) Uani 1 1 d . . . N7 N 0.5985(4) 0.5605(2) 0.6181(2) 0.0621(11) Uani 1 1 d . . . N8 N 0.6561(4) 0.6006(2) 0.5353(2) 0.0607(11) Uani 1 1 d . . . N9 N 0.6051(3) 0.7307(2) 0.5090(2) 0.0539(9) Uani 1 1 d . . . N10 N 0.5051(3) 0.78925(18) 0.5652(2) 0.0486(9) Uani 1 1 d . . . N11 N 0.4314(3) 0.7301(2) 0.6652(2) 0.0545(10) Uani 1 1 d . . . N12 N 0.4749(4) 0.6308(2) 0.6924(2) 0.0599(11) Uani 1 1 d . . . N13 N 0.7822(4) 0.3930(3) 0.5285(3) 0.0706(12) Uani 1 1 d . . . N14 N 0.8432(4) 0.3441(2) 0.1770(2) 0.0634(11) Uani 1 1 d . . . N15 N 0.4851(4) 0.0113(2) 0.7114(2) 0.0653(12) Uani 1 1 d . . . O1 O 0.4471(3) 0.34041(18) 0.90056(18) 0.0616(9) Uani 1 1 d . . . O2 O 0.4956(3) 0.27388(19) 1.0202(2) 0.0679(10) Uani 1 1 d . . . O3 O 0.6177(3) 0.16135(18) 1.00238(18) 0.0594(8) Uani 1 1 d . . . O4 O 0.6918(3) 0.16950(19) 0.87575(19) 0.0633(9) Uani 1 1 d . . . O5 O 0.5725(3) 0.27086(18) 0.82183(19) 0.0671(10) Uani 1 1 d . . . O6 O 0.9317(3) 0.58872(19) 0.23600(18) 0.0644(9) Uani 1 1 d . . . O7 O 1.1072(3) 0.62601(18) 0.17022(19) 0.0633(9) Uani 1 1 d . . . O8 O 1.0326(3) 0.6633(2) 0.03660(19) 0.0668(9) Uani 1 1 d . . . O9 O 0.8289(3) 0.70166(18) 0.03337(18) 0.0621(9) Uani 1 1 d . . . O10 O 0.8743(3) 0.71875(18) 0.21602(18) 0.0629(9) Uani 1 1 d . . . O11 O 0.1261(3) 1.06245(16) 0.59158(18) 0.0572(8) Uani 1 1 d . . . O12 O -0.1056(3) 1.15355(18) 0.55261(18) 0.0626(9) Uani 1 1 d . . . O13 O -0.2320(3) 1.16391(19) 0.66184(19) 0.0650(9) Uani 1 1 d . . . O14 O -0.0535(3) 1.10294(19) 0.74418(19) 0.0670(10) Uani 1 1 d . . . O15 O 0.0438(3) 0.99679(18) 0.68965(19) 0.0633(9) Uani 1 1 d . . . O16 O 0.6968(3) 0.41789(18) 0.51462(19) 0.0654(9) Uani 1 1 d . . . O17 O 0.7770(3) 0.33733(19) 0.55054(18) 0.0638(9) Uani 1 1 d . . . O18 O 0.8715(3) 0.41737(19) 0.5218(2) 0.0672(9) Uani 1 1 d . . . O19 O 0.7936(3) 0.34273(18) 0.2217(2) 0.0642(9) Uani 1 1 d . . . O20 O 0.8836(3) 0.29477(19) 0.15743(19) 0.0647(9) Uani 1 1 d . . . O21 O 0.8654(3) 0.3990(2) 0.15736(19) 0.0690(10) Uani 1 1 d . . . O22 O 0.4090(3) 0.04489(19) 0.71897(19) 0.0686(10) Uani 1 1 d . . . O23 O 0.5012(3) -0.0344(2) 0.7479(2) 0.0686(10) Uani 1 1 d . . . O24 O 0.5362(3) 0.02060(19) 0.66984(19) 0.0653(9) Uani 1 1 d . . . O25 O 0.7178(8) 0.5337(5) 0.8573(5) 0.068(4) Uani 0.392(11) 1 d P . . H25A H 0.7588 0.5429 0.8983 0.082 Uiso 0.392(11) 1 d PR . . H25B H 0.6660 0.5011 0.8537 0.082 Uiso 0.392(11) 1 d PR . . O26 O 0.8852(8) 0.7655(5) 0.7902(5) 0.073(4) Uani 0.410(11) 1 d P . . H26A H 0.9563 0.7702 0.8025 0.088 Uiso 0.410(11) 1 d PR . . H26B H 0.8637 0.7986 0.8104 0.088 Uiso 0.410(11) 1 d PR . . O27 O 0.9928(8) 0.8851(5) 0.9172(5) 0.069(3) Uani 0.402(11) 1 d P . . H27A H 0.9642 0.8534 0.8836 0.083 Uiso 0.402(11) 1 d PR . . H27B H 0.9431 0.8946 0.9367 0.083 Uiso 0.402(11) 1 d PR . . O28 O 0.6925(8) 0.8645(5) 0.0873(5) 0.072(4) Uani 0.412(11) 1 d P . . H28A H 0.7105 0.9038 0.0787 0.086 Uiso 0.412(11) 1 d PR . . H28B H 0.6227 0.8516 0.0694 0.086 Uiso 0.412(11) 1 d PR . . O29 O 0.8231(7) 0.9143(5) 0.0339(5) 0.061(3) Uani 0.390(10) 1 d P . . H29A H 0.7929 0.9081 -0.0090 0.073 Uiso 0.390(10) 1 d PR . . H29B H 0.8821 0.8961 0.0423 0.073 Uiso 0.390(10) 1 d PR . . O30 O 0.8411(7) 0.9831(5) 0.9130(5) 0.063(3) Uani 0.398(10) 1 d P . . H30B H 0.7835 0.9990 0.9184 0.076 Uiso 0.398(10) 1 d PR . . H30A H 0.8411 0.9442 0.9250 0.076 Uiso 0.398(10) 1 d PR . . O31 O 0.3707(8) 0.9905(5) 0.8533(5) 0.075(4) Uani 0.409(11) 1 d P . . H31A H 0.4407 0.9894 0.8625 0.090 Uiso 0.409(11) 1 d PR . . H31B H 0.3556 1.0243 0.8336 0.090 Uiso 0.409(11) 1 d PR . . O32 O 0.8534(7) 0.5697(5) 0.9838(5) 0.075(4) Uani 0.412(11) 1 d P . . H32A H 0.8167 0.6017 0.9737 0.091 Uiso 0.412(11) 1 d PR . . H32B H 0.8997 0.5815 1.0232 0.091 Uiso 0.412(11) 1 d PR . . O33 O 0.5789(8) 0.9415(5) 0.8886(5) 0.071(4) Uani 0.389(10) 1 d P . . H33A H 0.6322 0.9727 0.8910 0.085 Uiso 0.389(10) 1 d PR . . H33C H 0.5438 0.9538 0.9172 0.085 Uiso 0.389(10) 1 d PR . . O34 O 0.9347(7) 0.2888(5) 0.4709(5) 0.062(3) Uani 0.388(10) 1 d P . . H34A H 0.9164 0.3225 0.4924 0.074 Uiso 0.388(10) 1 d PR . . H34B H 0.8958 0.2526 0.4742 0.074 Uiso 0.388(10) 1 d PR . . Pd1 Pd 0.50730(3) 0.535741(18) 0.680932(19) 0.05236(10) Uani 1 1 d . . . Pd2 Pd 0.66413(3) 0.657471(18) 0.461326(18) 0.04963(10) Uani 1 1 d . . . Pd3 Pd 0.38771(3) 0.805023(17) 0.613109(18) 0.04585(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 0.061(3) 0.053(3) 0.063(3) 0.006(2) 0.016(2) 0.007(2) C2 0.064(3) 0.057(3) 0.059(3) 0.007(2) 0.010(2) 0.004(2) C3 0.070(3) 0.058(3) 0.070(3) 0.011(3) 0.019(3) 0.002(3) C4 0.064(3) 0.051(3) 0.062(3) 0.011(2) 0.012(2) 0.002(2) C5 0.057(3) 0.050(3) 0.064(3) 0.013(2) 0.014(2) -0.005(2) C6 0.055(3) 0.056(3) 0.063(3) 0.019(2) 0.009(2) 0.007(2) C7 0.055(3) 0.052(3) 0.064(3) 0.014(2) 0.012(2) 0.013(2) C8 0.053(3) 0.061(3) 0.073(3) 0.011(3) 0.013(3) 0.019(2) C9 0.064(3) 0.060(3) 0.067(3) 0.005(3) 0.015(3) 0.014(3) C10 0.072(3) 0.056(3) 0.066(3) 0.003(2) 0.013(3) 0.014(3) C11 0.061(3) 0.045(3) 0.068(3) 0.015(2) 0.013(2) 0.010(2) C12 0.062(3) 0.044(2) 0.062(3) 0.013(2) 0.012(2) 0.005(2) C13 0.060(3) 0.049(3) 0.064(3) 0.012(2) 0.018(2) 0.013(2) C14 0.060(3) 0.054(3) 0.056(3) 0.009(2) 0.015(2) 0.012(2) C15 0.064(3) 0.058(3) 0.060(3) 0.011(2) 0.020(2) 0.020(2) C16 0.060(3) 0.048(3) 0.061(3) 0.008(2) 0.014(2) 0.008(2) C17 0.064(3) 0.064(3) 0.070(3) 0.014(3) 0.023(3) 0.010(3) C18 0.067(3) 0.069(3) 0.066(3) 0.021(3) 0.023(3) 0.014(3) C19 0.069(3) 0.055(3) 0.055(3) 0.010(2) 0.015(2) 0.005(2) C20 0.072(3) 0.058(3) 0.055(3) 0.014(2) 0.010(3) 0.007(3) C21 0.065(3) 0.053(3) 0.075(4) 0.019(3) 0.018(3) 0.006(2) C22 0.075(4) 0.047(3) 0.069(3) 0.017(2) 0.018(3) 0.014(2) C23 0.054(3) 0.048(2) 0.052(3) 0.007(2) 0.012(2) 0.004(2) C24 0.057(3) 0.050(3) 0.059(3) 0.009(2) 0.015(2) 0.011(2) C25 0.053(3) 0.056(3) 0.067(3) 0.020(2) 0.014(2) 0.010(2) C26 0.055(3) 0.065(3) 0.059(3) 0.020(2) 0.012(2) 0.016(2) C27 0.055(3) 0.054(3) 0.060(3) 0.011(2) 0.009(2) 0.013(2) C28 0.042(2) 0.048(3) 0.070(3) 0.011(2) 0.011(2) 0.013(2) C29 0.060(3) 0.039(2) 0.066(3) 0.002(2) 0.015(2) 0.015(2) C30 0.051(3) 0.060(3) 0.069(3) 0.016(3) 0.013(2) 0.019(2) C31 0.055(3) 0.061(3) 0.069(3) 0.015(3) 0.016(2) 0.018(2) C32 0.066(3) 0.070(3) 0.066(3) 0.017(3) 0.018(3) 0.013(3) C33 0.054(3) 0.058(3) 0.063(3) 0.010(2) 0.014(2) 0.002(2) C34 0.070(3) 0.067(3) 0.065(3) 0.014(3) 0.024(3) 0.012(3) C35 0.046(3) 0.051(3) 0.070(3) 0.013(2) 0.013(2) 0.018(2) C36 0.046(3) 0.061(3) 0.066(3) 0.013(2) 0.013(2) 0.017(2) C37 0.063(3) 0.059(3) 0.066(3) 0.019(2) 0.018(3) 0.021(3) C38 0.068(3) 0.059(3) 0.059(3) 0.013(2) 0.015(3) 0.018(3) C39 0.068(3) 0.068(3) 0.062(3) 0.017(3) 0.011(3) 0.015(3) C40 0.069(4) 0.077(4) 0.064(3) 0.018(3) 0.013(3) 0.012(3) C41 0.067(3) 0.057(3) 0.064(3) 0.013(2) 0.016(3) 0.014(3) C42 0.067(3) 0.055(3) 0.063(3) 0.019(2) 0.014(3) 0.016(2) C43 0.068(3) 0.052(3) 0.061(3) 0.015(2) 0.019(3) 0.013(2) C44 0.059(3) 0.048(3) 0.061(3) 0.014(2) 0.021(2) 0.012(2) C45 0.055(3) 0.060(3) 0.071(3) 0.008(3) 0.016(3) 0.011(2) C46 0.056(3) 0.055(3) 0.073(3) 0.014(3) 0.010(3) 0.014(2) C47 0.064(3) 0.057(3) 0.057(3) 0.008(2) 0.013(2) 0.004(2) C48 0.062(3) 0.057(3) 0.055(3) 0.004(2) 0.014(2) 0.009(2) C49 0.053(3) 0.044(2) 0.063(3) 0.015(2) 0.014(2) 0.014(2) C50 0.059(3) 0.047(3) 0.065(3) 0.009(2) 0.018(2) 0.015(2) C51 0.057(3) 0.052(3) 0.056(3) 0.014(2) 0.013(2) 0.015(2) C52 0.067(3) 0.054(3) 0.074(4) 0.007(3) 0.013(3) 0.000(3) C53 0.075(4) 0.058(3) 0.073(4) 0.003(3) 0.008(3) 0.005(3) C54 0.070(4) 0.058(3) 0.070(3) 0.010(3) 0.016(3) -0.003(3) C55 0.061(3) 0.056(3) 0.057(3) 0.015(2) 0.013(2) 0.013(2) C56 0.075(3) 0.054(3) 0.056(3) 0.014(2) 0.015(3) 0.023(3) C57 0.069(3) 0.044(2) 0.060(3) 0.016(2) 0.013(2) 0.013(2) C58 0.063(3) 0.067(3) 0.065(3) 0.011(3) 0.015(3) -0.007(3) C59 0.066(3) 0.065(3) 0.066(3) 0.012(3) 0.021(3) 0.010(3) C60 0.068(4) 0.061(3) 0.078(4) -0.008(3) -0.002(3) 0.011(3) C61 0.071(3) 0.066(3) 0.059(3) 0.012(3) 0.018(3) 0.018(3) C62 0.064(3) 0.061(3) 0.064(3) 0.016(2) 0.017(3) 0.013(3) C63 0.060(3) 0.065(3) 0.065(3) 0.017(3) 0.019(3) 0.011(3) C64 0.065(3) 0.054(3) 0.068(3) 0.013(2) 0.015(3) 0.011(2) C65 0.064(3) 0.056(3) 0.057(3) 0.015(2) 0.013(2) 0.014(2) C66 0.060(3) 0.067(3) 0.060(3) 0.001(3) 0.013(2) 0.011(3) C67 0.056(3) 0.065(3) 0.065(3) 0.011(3) 0.014(2) 0.008(2) C68 0.062(3) 0.060(3) 0.067(3) 0.013(3) 0.019(3) 0.014(2) C69 0.067(3) 0.062(3) 0.063(3) 0.013(3) 0.010(3) 0.013(3) C70 0.067(3) 0.070(3) 0.054(3) 0.012(2) 0.018(2) 0.020(3) C71 0.060(3) 0.065(3) 0.065(3) 0.012(3) 0.017(3) 0.012(3) C72 0.067(3) 0.068(3) 0.062(3) 0.017(3) 0.015(3) 0.019(3) C73 0.065(3) 0.061(3) 0.060(3) 0.013(2) 0.018(3) 0.000(3) C74 0.057(3) 0.063(3) 0.063(3) 0.013(2) 0.009(2) 0.018(2) C75 0.068(3) 0.060(3) 0.071(3) 0.016(3) 0.015(3) 0.022(3) C76 0.058(3) 0.064(3) 0.065(3) 0.008(3) 0.014(3) 0.010(3) C77 0.062(3) 0.061(3) 0.065(3) 0.010(3) 0.015(3) 0.015(3) C78 0.066(3) 0.059(3) 0.067(3) 0.012(3) 0.014(3) 0.014(3) C79 0.064(3) 0.059(3) 0.066(3) 0.013(2) 0.015(3) 0.013(3) C80 0.064(3) 0.062(3) 0.060(3) 0.011(2) 0.015(3) 0.016(3) C81 0.056(3) 0.069(3) 0.066(3) 0.008(3) 0.012(3) 0.011(3) N1 0.073(3) 0.047(2) 0.073(3) 0.016(2) 0.022(2) 0.012(2) N2 0.073(3) 0.048(2) 0.059(2) 0.0107(19) 0.012(2) 0.013(2) N3 0.068(3) 0.048(2) 0.059(2) 0.0119(18) 0.016(2) 0.014(2) N4 0.063(3) 0.050(2) 0.057(2) 0.0141(18) 0.014(2) 0.0167(19) N5 0.047(2) 0.048(2) 0.059(2) 0.0121(18) 0.0124(17) 0.0147(17) N6 0.054(2) 0.057(2) 0.075(3) 0.015(2) 0.022(2) 0.014(2) N7 0.065(3) 0.059(2) 0.063(3) 0.017(2) 0.015(2) 0.013(2) N8 0.067(3) 0.054(2) 0.062(3) 0.020(2) 0.014(2) 0.013(2) N9 0.053(2) 0.054(2) 0.054(2) 0.0094(18) 0.0087(18) 0.0172(18) N10 0.050(2) 0.045(2) 0.055(2) 0.0160(17) 0.0143(17) 0.0154(17) N11 0.059(2) 0.048(2) 0.058(2) 0.0155(18) 0.0136(19) 0.0147(19) N12 0.070(3) 0.048(2) 0.061(2) 0.0171(19) 0.011(2) 0.015(2) N13 0.070(3) 0.075(3) 0.072(3) 0.023(3) 0.021(3) 0.018(3) N14 0.063(3) 0.063(3) 0.062(3) 0.012(2) 0.012(2) 0.013(2) N15 0.062(3) 0.062(3) 0.059(3) -0.004(2) 0.000(2) 0.015(2) O1 0.060(2) 0.060(2) 0.065(2) 0.0153(17) 0.0155(17) 0.0067(17) O2 0.065(2) 0.067(2) 0.070(2) 0.0150(18) 0.0121(18) 0.0116(18) O3 0.064(2) 0.059(2) 0.059(2) 0.0181(16) 0.0165(17) 0.0178(17) O4 0.062(2) 0.068(2) 0.064(2) 0.0166(18) 0.0188(17) 0.0165(18) O5 0.072(2) 0.059(2) 0.069(2) 0.0182(18) 0.0130(19) 0.0126(18) O6 0.062(2) 0.068(2) 0.060(2) 0.0045(17) 0.0148(17) 0.0110(18) O7 0.064(2) 0.062(2) 0.065(2) 0.0117(17) 0.0164(18) 0.0149(17) O8 0.062(2) 0.071(2) 0.071(2) 0.0187(19) 0.0194(19) 0.0145(18) O9 0.063(2) 0.065(2) 0.059(2) 0.0167(17) 0.0134(17) 0.0145(17) O10 0.066(2) 0.063(2) 0.061(2) 0.0128(17) 0.0195(17) 0.0090(18) O11 0.059(2) 0.0497(18) 0.064(2) 0.0125(15) 0.0134(16) 0.0183(16) O12 0.061(2) 0.062(2) 0.061(2) 0.0067(17) 0.0103(17) 0.0172(17) O13 0.062(2) 0.068(2) 0.066(2) 0.0136(18) 0.0168(18) 0.0139(18) O14 0.071(2) 0.068(2) 0.066(2) 0.0156(18) 0.0200(19) 0.0206(19) O15 0.060(2) 0.063(2) 0.066(2) 0.0058(18) 0.0156(17) 0.0152(17) O16 0.064(2) 0.060(2) 0.070(2) 0.0142(18) 0.0123(18) 0.0110(18) O17 0.060(2) 0.071(2) 0.061(2) 0.0194(18) 0.0119(17) 0.0157(18) O18 0.066(2) 0.067(2) 0.068(2) 0.0140(19) 0.0170(19) 0.0113(19) O19 0.060(2) 0.060(2) 0.074(2) 0.0140(18) 0.0175(19) 0.0165(17) O20 0.064(2) 0.067(2) 0.067(2) 0.0191(18) 0.0176(18) 0.0200(18) O21 0.074(3) 0.067(2) 0.066(2) 0.0157(19) 0.0147(19) 0.0142(19) O22 0.067(2) 0.062(2) 0.066(2) -0.0143(18) 0.0079(18) 0.0147(18) O23 0.062(2) 0.067(2) 0.075(2) 0.011(2) 0.0155(19) 0.0091(19) O24 0.072(2) 0.061(2) 0.054(2) -0.0118(17) 0.0084(18) 0.0167(18) O25 0.067(6) 0.064(6) 0.068(6) 0.008(5) 0.011(5) 0.011(5) O26 0.067(6) 0.083(7) 0.063(6) 0.000(5) 0.009(5) 0.019(5) O27 0.079(7) 0.063(6) 0.071(6) 0.022(5) 0.020(5) 0.016(5) O28 0.070(6) 0.080(7) 0.074(7) 0.029(5) 0.019(5) 0.025(5) O29 0.058(6) 0.066(6) 0.057(5) 0.020(4) 0.010(4) 0.011(4) O30 0.057(6) 0.065(6) 0.065(6) 0.013(4) 0.015(4) 0.001(4) O31 0.076(7) 0.074(7) 0.060(6) -0.017(5) 0.016(5) -0.005(5) O32 0.055(6) 0.076(7) 0.071(6) -0.015(5) -0.015(4) 0.014(5) O33 0.070(7) 0.074(7) 0.056(6) -0.014(5) 0.020(5) -0.022(5) O34 0.058(6) 0.064(6) 0.062(6) 0.016(4) 0.009(4) 0.015(4) Pd1 0.0619(2) 0.04585(19) 0.0519(2) 0.01656(15) 0.01293(17) 0.01618(16) Pd2 0.0567(2) 0.04752(19) 0.04706(19) 0.01272(15) 0.01317(16) 0.01512(16) Pd3 0.04820(19) 0.04312(18) 0.04863(19) 0.01236(14) 0.01197(15) 0.01513(15) _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 1.329(5) . ? C1 C2 1.413(7) . ? C1 H1 0.9300 . ? C2 C3 1.339(8) . ? C2 H2 0.9300 . ? C3 C4 1.412(8) . ? C3 H3 0.9300 . ? C4 C5 1.395(7) . ? C4 C12 1.418(7) . ? C5 C6 1.371(8) . ? C5 O1 1.388(5) . ? C6 O5 1.323(5) . ? C6 C7 1.405(7) . ? C7 C11 1.412(7) . ? C7 C8 1.452(7) . ? C8 C9 1.324(8) . ? C8 H8 0.9300 . ? C9 C10 1.408(7) . ? C9 H9 0.9300 . ? C10 N2 1.331(6) . ? C10 H10 0.9300 . ? C11 N2 1.330(5) . ? C11 C12 1.425(7) . ? C12 N1 1.360(5) . ? C13 N3 1.304(5) . ? C13 C14 1.383(7) . ? C13 H13 0.9300 . ? C14 C15 1.400(7) . ? C14 H14 0.9300 . ? C15 C16 1.402(7) . ? C15 H15 0.9300 . ? C16 C24 1.402(7) . ? C16 C17 1.419(7) . ? C17 O6 1.357(6) . ? C17 C18 1.399(8) . ? C18 O10 1.350(5) . ? C18 C19 1.411(8) . ? C19 C23 1.371(7) . ? C19 C20 1.435(7) . ? C20 C21 1.386(8) . ? C20 H20 0.9300 . ? C21 C22 1.405(7) . ? C21 H21 0.9300 . ? C22 N4 1.311(5) . ? C22 H22 0.9300 . ? C23 N4 1.371(5) . ? C23 C24 1.405(7) . ? C24 N3 1.377(5) . ? C25 N5 1.324(5) . ? C25 C26 1.402(7) . ? C25 H25 0.9300 . ? C26 C27 1.339(7) . ? C26 H26 0.9300 . ? C27 C28 1.386(7) . ? C27 H27 0.9300 . ? C28 C35 1.414(6) . ? C28 C29 1.443(7) . ? C29 O11 1.365(5) . ? C29 C30 1.366(7) . ? C30 O15 1.374(5) . ? C30 C31 1.405(7) . ? C31 C36 1.375(7) . ? C31 C32 1.418(8) . ? C32 C33 1.400(7) . ? C32 H32 0.9300 . ? C33 C34 1.396(7) . ? C33 H33 0.9300 . ? C34 N6 1.310(5) . ? C34 H34 0.9300 . ? C35 N5 1.380(5) . ? C35 C36 1.410(7) . ? C36 N6 1.386(5) . ? C37 C38 1.364(7) . ? C37 N7 1.384(5) . ? C37 C42 1.391(7) . ? C38 C39 1.422(8) . ? C38 H38 0.9300 . ? C39 C40 1.364(8) . ? C39 H39 0.9300 . ? C40 C41 1.378(7) . ? C40 H40 0.9300 . ? C41 C42 1.410(8) . ? C41 H41 0.9300 . ? C42 N8 1.380(5) . ? C43 N8 1.309(5) . ? C43 N7 1.349(5) . ? C43 H43 0.9300 . ? C44 C45 1.375(7) . ? C44 C49 1.403(7) . ? C44 N9 1.407(5) . ? C45 C46 1.385(7) . ? C45 H45 0.9300 . ? C46 C47 1.370(7) . ? C46 H46 0.9300 . ? C47 C48 1.380(7) . ? C47 H47 0.9300 . ? C48 C49 1.410(7) . ? C48 H48 0.9300 . ? C49 N10 1.363(5) . ? C50 N10 1.337(5) . ? C50 N9 1.343(5) . ? C50 H50 0.9300 . ? C51 C52 1.343(7) . ? C51 C56 1.387(7) . ? C51 N11 1.392(5) . ? C52 C53 1.392(8) . ? C52 H52 0.9300 . ? C53 C54 1.354(8) . ? C53 H53 0.9300 . ? C54 C55 1.414(7) . ? C54 H54 0.9300 . ? C55 C56 1.405(7) . ? C55 H55 0.9300 . ? C56 N12 1.356(5) . ? C57 N11 1.333(5) . ? C57 N12 1.364(5) . ? C57 H57 0.9300 . ? C58 O1 1.432(5) . ? C58 C59 1.515(7) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 O2 1.414(5) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 O2 1.418(6) . ? C60 C61 1.523(6) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O3 1.415(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 O3 1.409(6) . ? C62 C63 1.551(8) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 O4 1.425(6) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 O4 1.424(6) . ? C64 C65 1.510(7) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O5 1.415(6) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 O6 1.432(6) . ? C66 C67 1.514(7) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 O7 1.396(6) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 O7 1.408(6) . ? C68 C69 1.525(7) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 O8 1.427(6) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 O8 1.409(6) . ? C70 C71 1.523(7) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 O9 1.438(6) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O9 1.410(6) . ? C72 C73 1.529(7) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 O10 1.447(6) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 O11 1.444(6) . ? C74 C75 1.511(7) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 O12 1.400(6) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 O12 1.405(6) . ? C76 C77 1.504(7) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 O13 1.427(6) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 O13 1.427(6) . ? C78 C79 1.507(7) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 O14 1.401(6) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 O14 1.432(6) . ? C80 C81 1.514(7) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 O15 1.380(6) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? N1 Pd1 2.034(5) . ? N2 Pd1 2.042(4) . ? N3 Pd2 2.022(4) . ? N4 Pd2 2.017(4) . ? N5 Pd3 2.018(4) . ? N6 Pd3 2.010(4) . ? N7 Pd1 2.005(5) . ? N8 Pd2 2.029(4) . ? N9 Pd2 1.988(4) . ? N10 Pd3 2.003(4) . ? N11 Pd3 2.001(4) . ? N12 Pd1 2.002(4) . ? N13 O16 1.215(6) . ? N13 O18 1.218(6) . ? N13 O17 1.261(6) . ? N14 O20 1.237(6) . ? N14 O19 1.238(6) . ? N14 O21 1.249(6) . ? N15 O24 1.214(6) . ? N15 O23 1.257(6) . ? N15 O22 1.261(6) . ? O25 H25A 0.8501 . ? O25 H25B 0.8500 . ? O26 H26A 0.8500 . ? O26 H26B 0.8500 . ? O27 H27A 0.8501 . ? O27 H27B 0.8500 . ? O28 H28A 0.8500 . ? O28 H28B 0.8500 . ? O29 H29A 0.8500 . ? O29 H29B 0.8501 . ? O30 H30B 0.8501 . ? O30 H30A 0.8500 . ? O31 H31A 0.8500 . ? O31 H31B 0.8500 . ? O32 H32A 0.8499 . ? O32 H32B 0.8501 . ? O33 H33A 0.8500 . ? O33 H33C 0.8500 . ? O34 H34A 0.8499 . ? O34 H34B 0.8501 . ? 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 118.8(5) . . ? N1 C1 H1 120.6 . . ? C2 C1 H1 120.6 . . ? C3 C2 C1 121.2(6) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 121.6(6) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 127.1(5) . . ? C5 C4 C12 118.4(5) . . ? C3 C4 C12 114.5(5) . . ? C6 C5 O1 119.4(4) . . ? C6 C5 C4 123.7(5) . . ? O1 C5 C4 116.9(5) . . ? O5 C6 C5 128.6(5) . . ? O5 C6 C7 113.9(5) . . ? C5 C6 C7 117.5(5) . . ? C6 C7 C11 122.2(5) . . ? C6 C7 C8 124.5(5) . . ? C11 C7 C8 113.3(5) . . ? C9 C8 C7 121.6(5) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 120.1(6) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 120.7(5) . . ? N2 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? N2 C11 C7 124.5(5) . . ? N2 C11 C12 117.3(4) . . ? C7 C11 C12 118.2(5) . . ? N1 C12 C4 122.9(5) . . ? N1 C12 C11 117.3(4) . . ? C4 C12 C11 119.7(5) . . ? N3 C13 C14 123.7(5) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 119.2(5) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 118.8(5) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C24 C16 C15 117.2(5) . . ? C24 C16 C17 119.1(5) . . ? C15 C16 C17 123.6(5) . . ? O6 C17 C18 121.4(5) . . ? O6 C17 C16 118.6(5) . . ? C18 C17 C16 120.0(5) . . ? O10 C18 C17 123.1(5) . . ? O10 C18 C19 117.0(4) . . ? C17 C18 C19 119.7(5) . . ? C23 C19 C18 120.4(5) . . ? C23 C19 C20 119.0(5) . . ? C18 C19 C20 120.5(5) . . ? C21 C20 C19 116.0(5) . . ? C21 C20 H20 122.0 . . ? C19 C20 H20 122.0 . . ? C20 C21 C22 121.7(5) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? N4 C22 C21 121.1(5) . . ? N4 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? N4 C23 C19 122.8(4) . . ? N4 C23 C24 116.7(4) . . ? C19 C23 C24 120.5(5) . . ? N3 C24 C16 122.9(4) . . ? N3 C24 C23 116.8(4) . . ? C16 C24 C23 120.2(5) . . ? N5 C25 C26 119.2(5) . . ? N5 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 123.6(5) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C26 C27 C28 118.3(5) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C27 C28 C35 117.9(5) . . ? C27 C28 C29 126.0(4) . . ? C35 C28 C29 115.9(5) . . ? O11 C29 C30 125.5(4) . . ? O11 C29 C28 112.6(4) . . ? C30 C29 C28 121.8(4) . . ? C29 C30 O15 121.7(4) . . ? C29 C30 C31 120.7(5) . . ? O15 C30 C31 117.6(5) . . ? C36 C31 C30 119.4(5) . . ? C36 C31 C32 117.6(5) . . ? C30 C31 C32 123.0(5) . . ? C33 C32 C31 119.0(5) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C34 C33 C32 118.9(5) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? N6 C34 C33 122.6(5) . . ? N6 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? N5 C35 C36 117.2(4) . . ? N5 C35 C28 121.6(4) . . ? C36 C35 C28 121.1(5) . . ? C31 C36 N6 122.6(4) . . ? C31 C36 C35 120.7(5) . . ? N6 C36 C35 116.5(4) . . ? C38 C37 N7 129.9(5) . . ? C38 C37 C42 122.9(5) . . ? N7 C37 C42 107.2(4) . . ? C37 C38 C39 116.1(5) . . ? C37 C38 H38 122.0 . . ? C39 C38 H38 122.0 . . ? C40 C39 C38 121.3(5) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C41 122.6(6) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C40 C41 C42 116.6(5) . . ? C40 C41 H41 121.7 . . ? C42 C41 H41 121.7 . . ? N8 C42 C37 107.5(4) . . ? N8 C42 C41 132.1(5) . . ? C37 C42 C41 120.4(5) . . ? N8 C43 N7 112.9(4) . . ? N8 C43 H43 123.6 . . ? N7 C43 H43 123.6 . . ? C45 C44 C49 121.9(5) . . ? C45 C44 N9 129.8(4) . . ? C49 C44 N9 108.3(4) . . ? C44 C45 C46 117.1(5) . . ? C44 C45 H45 121.4 . . ? C46 C45 H45 121.4 . . ? C47 C46 C45 122.2(5) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C46 C47 C48 121.5(5) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C49 117.5(5) . . ? C47 C48 H48 121.2 . . ? C49 C48 H48 121.2 . . ? N10 C49 C44 107.2(4) . . ? N10 C49 C48 133.0(4) . . ? C44 C49 C48 119.7(5) . . ? N10 C50 N9 114.0(4) . . ? N10 C50 H50 123.0 . . ? N9 C50 H50 123.0 . . ? C52 C51 C56 124.1(5) . . ? C52 C51 N11 129.4(4) . . ? C56 C51 N11 106.5(4) . . ? C51 C52 C53 115.2(5) . . ? C51 C52 H52 122.4 . . ? C53 C52 H52 122.4 . . ? C54 C53 C52 124.3(6) . . ? C54 C53 H53 117.8 . . ? C52 C53 H53 117.9 . . ? C53 C54 C55 120.0(5) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 116.2(5) . . ? C56 C55 H55 121.9 . . ? C54 C55 H55 121.9 . . ? N12 C56 C51 109.3(4) . . ? N12 C56 C55 130.5(4) . . ? C51 C56 C55 120.1(5) . . ? N11 C57 N12 111.7(4) . . ? N11 C57 H57 124.1 . . ? N12 C57 H57 124.1 . . ? O1 C58 C59 106.6(4) . . ? O1 C58 H58A 110.4 . . ? C59 C58 H58A 110.4 . . ? O1 C58 H58B 110.4 . . ? C59 C58 H58B 110.4 . . ? H58A C58 H58B 108.6 . . ? O2 C59 C58 109.4(4) . . ? O2 C59 H59A 109.8 . . ? C58 C59 H59A 109.8 . . ? O2 C59 H59B 109.8 . . ? C58 C59 H59B 109.8 . . ? H59A C59 H59B 108.2 . . ? O2 C60 C61 111.7(4) . . ? O2 C60 H60A 109.3 . . ? C61 C60 H60A 109.3 . . ? O2 C60 H60B 109.3 . . ? C61 C60 H60B 109.3 . . ? H60A C60 H60B 107.9 . . ? O3 C61 C60 111.5(4) . . ? O3 C61 H61A 109.3 . . ? C60 C61 H61A 109.3 . . ? O3 C61 H61B 109.3 . . ? C60 C61 H61B 109.3 . . ? H61A C61 H61B 108.0 . . ? O3 C62 C63 102.4(4) . . ? O3 C62 H62A 111.3 . . ? C63 C62 H62A 111.3 . . ? O3 C62 H62B 111.3 . . ? C63 C62 H62B 111.3 . . ? H62A C62 H62B 109.2 . . ? O4 C63 C62 112.6(4) . . ? O4 C63 H63A 109.1 . . ? C62 C63 H63A 109.1 . . ? O4 C63 H63B 109.1 . . ? C62 C63 H63B 109.1 . . ? H63A C63 H63B 107.8 . . ? O4 C64 C65 109.9(4) . . ? O4 C64 H64A 109.7 . . ? C65 C64 H64A 109.7 . . ? O4 C64 H64B 109.7 . . ? C65 C64 H64B 109.7 . . ? H64A C64 H64B 108.2 . . ? O5 C65 C64 108.9(4) . . ? O5 C65 H65A 109.9 . . ? C64 C65 H65A 109.9 . . ? O5 C65 H65B 109.9 . . ? C64 C65 H65B 109.9 . . ? H65A C65 H65B 108.3 . . ? O6 C66 C67 108.1(4) . . ? O6 C66 H66A 110.1 . . ? C67 C66 H66A 110.1 . . ? O6 C66 H66B 110.1 . . ? C67 C66 H66B 110.1 . . ? H66A C66 H66B 108.4 . . ? O7 C67 C66 109.4(5) . . ? O7 C67 H67A 109.8 . . ? C66 C67 H67A 109.8 . . ? O7 C67 H67B 109.8 . . ? C66 C67 H67B 109.8 . . ? H67A C67 H67B 108.2 . . ? O7 C68 C69 110.5(4) . . ? O7 C68 H68A 109.5 . . ? C69 C68 H68A 109.5 . . ? O7 C68 H68B 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? O8 C69 C68 106.9(5) . . ? O8 C69 H69A 110.3 . . ? C68 C69 H69A 110.3 . . ? O8 C69 H69B 110.3 . . ? C68 C69 H69B 110.3 . . ? H69A C69 H69B 108.6 . . ? O8 C70 C71 103.7(4) . . ? O8 C70 H70A 111.0 . . ? C71 C70 H70A 111.0 . . ? O8 C70 H70B 111.0 . . ? C71 C70 H70B 111.0 . . ? H70A C70 H70B 109.0 . . ? O9 C71 C70 113.8(4) . . ? O9 C71 H71A 108.8 . . ? C70 C71 H71A 108.8 . . ? O9 C71 H71B 108.8 . . ? C70 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? O9 C72 C73 105.1(4) . . ? O9 C72 H72A 110.7 . . ? C73 C72 H72A 110.7 . . ? O9 C72 H72B 110.7 . . ? C73 C72 H72B 110.7 . . ? H72A C72 H72B 108.8 . . ? O10 C73 C72 108.6(4) . . ? O10 C73 H73A 110.0 . . ? C72 C73 H73A 110.0 . . ? O10 C73 H73B 110.0 . . ? C72 C73 H73B 110.0 . . ? H73A C73 H73B 108.3 . . ? O11 C74 C75 106.2(4) . . ? O11 C74 H74A 110.5 . . ? C75 C74 H74A 110.5 . . ? O11 C74 H74B 110.5 . . ? C75 C74 H74B 110.5 . . ? H74A C74 H74B 108.7 . . ? O12 C75 C74 106.9(5) . . ? O12 C75 H75A 110.3 . . ? C74 C75 H75A 110.3 . . ? O12 C75 H75B 110.3 . . ? C74 C75 H75B 110.3 . . ? H75A C75 H75B 108.6 . . ? O12 C76 C77 109.3(4) . . ? O12 C76 H76A 109.8 . . ? C77 C76 H76A 109.8 . . ? O12 C76 H76B 109.8 . . ? C77 C76 H76B 109.8 . . ? H76A C76 H76B 108.3 . . ? O13 C77 C76 116.7(4) . . ? O13 C77 H77A 108.1 . . ? C76 C77 H77A 108.1 . . ? O13 C77 H77B 108.1 . . ? C76 C77 H77B 108.1 . . ? H77A C77 H77B 107.3 . . ? O13 C78 C79 112.2(4) . . ? O13 C78 H78A 109.2 . . ? C79 C78 H78A 109.2 . . ? O13 C78 H78B 109.2 . . ? C79 C78 H78B 109.2 . . ? H78A C78 H78B 107.9 . . ? O14 C79 C78 109.7(5) . . ? O14 C79 H79A 109.7 . . ? C78 C79 H79A 109.7 . . ? O14 C79 H79B 109.7 . . ? C78 C79 H79B 109.7 . . ? H79A C79 H79B 108.2 . . ? O14 C80 C81 105.1(4) . . ? O14 C80 H80A 110.7 . . ? C81 C80 H80A 110.7 . . ? O14 C80 H80B 110.7 . . ? C81 C80 H80B 110.7 . . ? H80A C80 H80B 108.8 . . ? O15 C81 C80 109.9(4) . . ? O15 C81 H81A 109.7 . . ? C80 C81 H81A 109.7 . . ? O15 C81 H81B 109.7 . . ? C80 C81 H81B 109.7 . . ? H81A C81 H81B 108.2 . . ? C1 N1 C12 120.8(3) . . ? C1 N1 Pd1 128.4(3) . . ? C12 N1 Pd1 110.8(3) . . ? C11 N2 C10 119.8(3) . . ? C11 N2 Pd1 111.8(3) . . ? C10 N2 Pd1 128.2(3) . . ? C13 N3 C24 118.0(3) . . ? C13 N3 Pd2 129.8(3) . . ? C24 N3 Pd2 111.8(2) . . ? C22 N4 C23 119.3(3) . . ? C22 N4 Pd2 128.2(3) . . ? C23 N4 Pd2 112.4(2) . . ? C25 N5 C35 119.4(3) . . ? C25 N5 Pd3 129.0(2) . . ? C35 N5 Pd3 111.5(2) . . ? C34 N6 C36 119.0(3) . . ? C34 N6 Pd3 129.1(3) . . ? C36 N6 Pd3 111.8(3) . . ? C43 N7 C37 105.7(3) . . ? C43 N7 Pd1 131.6(3) . . ? C37 N7 Pd1 122.0(3) . . ? C43 N8 C42 106.8(3) . . ? C43 N8 Pd2 129.2(3) . . ? C42 N8 Pd2 121.0(3) . . ? C50 N9 C44 103.7(3) . . ? C50 N9 Pd2 132.3(3) . . ? C44 N9 Pd2 123.2(3) . . ? C50 N10 C49 106.7(3) . . ? C50 N10 Pd3 126.5(2) . . ? C49 N10 Pd3 125.2(2) . . ? C57 N11 C51 106.6(3) . . ? C57 N11 Pd3 129.7(3) . . ? C51 N11 Pd3 122.8(2) . . ? C56 N12 C57 105.8(3) . . ? C56 N12 Pd1 125.2(3) . . ? C57 N12 Pd1 127.5(3) . . ? O16 N13 O18 124.7(5) . . ? O16 N13 O17 117.3(5) . . ? O18 N13 O17 118.0(5) . . ? O20 N14 O19 121.5(5) . . ? O20 N14 O21 118.7(5) . . ? O19 N14 O21 119.2(5) . . ? O24 N15 O23 122.2(5) . . ? O24 N15 O22 122.2(5) . . ? O23 N15 O22 115.5(5) . . ? C5 O1 C58 115.7(3) . . ? C59 O2 C60 116.1(3) . . ? C62 O3 C61 109.5(4) . . ? C64 O4 C63 113.0(4) . . ? C6 O5 C65 123.7(4) . . ? C17 O6 C66 115.6(3) . . ? C67 O7 C68 112.3(4) . . ? C70 O8 C69 107.5(4) . . ? C72 O9 C71 116.2(4) . . ? C18 O10 C73 119.2(3) . . ? C29 O11 C74 118.1(3) . . ? C75 O12 C76 107.0(4) . . ? C78 O13 C77 114.7(4) . . ? C79 O14 C80 111.1(4) . . ? C30 O15 C81 115.1(3) . . ? H25A O25 H25B 109.5 . . ? H26A O26 H26B 109.5 . . ? H27A O27 H27B 109.5 . . ? H28A O28 H28B 109.5 . . ? H29A O29 H29B 109.5 . . ? H30B O30 H30A 109.5 . . ? H31A O31 H31B 109.5 . . ? H32A O32 H32B 109.5 . . ? H33A O33 H33C 109.5 . . ? H34A O34 H34B 109.5 . . ? N12 Pd1 N7 89.36(18) . . ? N12 Pd1 N1 93.59(18) . . ? N7 Pd1 N1 172.53(18) . . ? N12 Pd1 N2 172.95(17) . . ? N7 Pd1 N2 95.01(18) . . ? N1 Pd1 N2 81.42(18) . . ? N9 Pd2 N4 92.58(17) . . ? N9 Pd2 N3 172.36(18) . . ? N4 Pd2 N3 81.71(16) . . ? N9 Pd2 N8 90.44(17) . . ? N4 Pd2 N8 175.45(17) . . ? N3 Pd2 N8 94.97(17) . . ? N11 Pd3 N10 88.63(16) . . ? N11 Pd3 N6 93.47(17) . . ? N10 Pd3 N6 177.11(16) . . ? N11 Pd3 N5 173.97(17) . . ? N10 Pd3 N5 95.12(15) . . ? N6 Pd3 N5 82.63(17) . . ? 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(8) . . . . ? C1 C2 C3 C4 1.9(9) . . . . ? C2 C3 C4 C5 179.2(5) . . . . ? C2 C3 C4 C12 -2.3(8) . . . . ? C3 C4 C5 C6 174.8(5) . . . . ? C12 C4 C5 C6 -3.7(8) . . . . ? C3 C4 C5 O1 -4.1(8) . . . . ? C12 C4 C5 O1 177.4(4) . . . . ? O1 C5 C6 O5 -2.2(8) . . . . ? C4 C5 C6 O5 178.9(5) . . . . ? O1 C5 C6 C7 178.5(4) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? O5 C6 C7 C11 -175.2(4) . . . . ? C5 C6 C7 C11 4.1(8) . . . . ? O5 C6 C7 C8 3.5(7) . . . . ? C5 C6 C7 C8 -177.2(5) . . . . ? C6 C7 C8 C9 -177.5(5) . . . . ? C11 C7 C8 C9 1.3(8) . . . . ? C7 C8 C9 C10 -0.9(8) . . . . ? C8 C9 C10 N2 0.8(8) . . . . ? C6 C7 C11 N2 177.0(4) . . . . ? C8 C7 C11 N2 -1.8(7) . . . . ? C6 C7 C11 C12 -3.7(8) . . . . ? C8 C7 C11 C12 177.5(5) . . . . ? C5 C4 C12 N1 -177.6(4) . . . . ? C3 C4 C12 N1 3.8(7) . . . . ? C5 C4 C12 C11 4.0(8) . . . . ? C3 C4 C12 C11 -174.6(5) . . . . ? N2 C11 C12 N1 0.3(7) . . . . ? C7 C11 C12 N1 -179.0(4) . . . . ? N2 C11 C12 C4 178.8(4) . . . . ? C7 C11 C12 C4 -0.5(7) . . . . ? N3 C13 C14 C15 1.6(8) . . . . ? C13 C14 C15 C16 -3.0(8) . . . . ? C14 C15 C16 C24 3.4(7) . . . . ? C14 C15 C16 C17 -179.1(5) . . . . ? C24 C16 C17 O6 179.9(4) . . . . ? C15 C16 C17 O6 2.4(8) . . . . ? C24 C16 C17 C18 -2.1(8) . . . . ? C15 C16 C17 C18 -179.6(5) . . . . ? O6 C17 C18 O10 -5.6(9) . . . . ? C16 C17 C18 O10 176.4(5) . . . . ? O6 C17 C18 C19 179.6(5) . . . . ? C16 C17 C18 C19 1.7(9) . . . . ? O10 C18 C19 C23 -175.6(4) . . . . ? C17 C18 C19 C23 -0.5(8) . . . . ? O10 C18 C19 C20 7.7(8) . . . . ? C17 C18 C19 C20 -177.3(5) . . . . ? C23 C19 C20 C21 3.1(8) . . . . ? C18 C19 C20 C21 179.9(5) . . . . ? C19 C20 C21 C22 -0.8(8) . . . . ? C20 C21 C22 N4 -1.8(8) . . . . ? C18 C19 C23 N4 -180.0(4) . . . . ? C20 C19 C23 N4 -3.2(7) . . . . ? C18 C19 C23 C24 -0.2(8) . . . . ? C20 C19 C23 C24 176.7(5) . . . . ? C15 C16 C24 N3 -2.6(7) . . . . ? C17 C16 C24 N3 179.8(4) . . . . ? C15 C16 C24 C23 179.1(5) . . . . ? C17 C16 C24 C23 1.4(8) . . . . ? N4 C23 C24 N3 1.1(6) . . . . ? C19 C23 C24 N3 -178.7(4) . . . . ? N4 C23 C24 C16 179.5(4) . . . . ? C19 C23 C24 C16 -0.3(8) . . . . ? N5 C25 C26 C27 1.8(8) . . . . ? C25 C26 C27 C28 -1.9(8) . . . . ? C26 C27 C28 C35 2.5(7) . . . . ? C26 C27 C28 C29 178.2(5) . . . . ? C27 C28 C29 O11 0.2(7) . . . . ? C35 C28 C29 O11 176.0(4) . . . . ? C27 C28 C29 C30 -179.8(5) . . . . ? C35 C28 C29 C30 -4.0(7) . . . . ? O11 C29 C30 O15 1.6(8) . . . . ? C28 C29 C30 O15 -178.4(4) . . . . ? O11 C29 C30 C31 179.4(5) . . . . ? C28 C29 C30 C31 -0.6(8) . . . . ? C29 C30 C31 C36 5.2(8) . . . . ? O15 C30 C31 C36 -176.9(4) . . . . ? C29 C30 C31 C32 -175.3(5) . . . . ? O15 C30 C31 C32 2.6(8) . . . . ? C36 C31 C32 C33 4.3(8) . . . . ? C30 C31 C32 C33 -175.3(5) . . . . ? C31 C32 C33 C34 -4.9(8) . . . . ? C32 C33 C34 N6 2.5(8) . . . . ? C27 C28 C35 N5 -3.1(7) . . . . ? C29 C28 C35 N5 -179.3(4) . . . . ? C27 C28 C35 C36 -179.7(5) . . . . ? C29 C28 C35 C36 4.1(7) . . . . ? C30 C31 C36 N6 178.4(4) . . . . ? C32 C31 C36 N6 -1.2(8) . . . . ? C30 C31 C36 C35 -5.0(8) . . . . ? C32 C31 C36 C35 175.4(5) . . . . ? N5 C35 C36 C31 -176.5(4) . . . . ? C28 C35 C36 C31 0.2(8) . . . . ? N5 C35 C36 N6 0.4(6) . . . . ? C28 C35 C36 N6 177.1(4) . . . . ? N7 C37 C38 C39 180.0(5) . . . . ? C42 C37 C38 C39 1.4(8) . . . . ? C37 C38 C39 C40 0.5(8) . . . . ? C38 C39 C40 C41 -0.2(9) . . . . ? C39 C40 C41 C42 -2.0(9) . . . . ? C38 C37 C42 N8 178.6(5) . . . . ? N7 C37 C42 N8 -0.2(5) . . . . ? C38 C37 C42 C41 -3.7(8) . . . . ? N7 C37 C42 C41 177.5(4) . . . . ? C40 C41 C42 N8 -179.1(5) . . . . ? C40 C41 C42 C37 3.9(8) . . . . ? C49 C44 C45 C46 0.0(8) . . . . ? N9 C44 C45 C46 179.3(4) . . . . ? C44 C45 C46 C47 -2.6(8) . . . . ? C45 C46 C47 C48 2.9(8) . . . . ? C46 C47 C48 C49 -0.5(8) . . . . ? C45 C44 C49 N10 179.3(4) . . . . ? N9 C44 C49 N10 -0.1(5) . . . . ? C45 C44 C49 C48 2.3(7) . . . . ? N9 C44 C49 C48 -177.2(4) . . . . ? C47 C48 C49 N10 -178.2(5) . . . . ? C47 C48 C49 C44 -2.0(7) . . . . ? C56 C51 C52 C53 0.7(9) . . . . ? N11 C51 C52 C53 -179.1(5) . . . . ? C51 C52 C53 C54 -0.6(10) . . . . ? C52 C53 C54 C55 1.8(10) . . . . ? C53 C54 C55 C56 -2.8(8) . . . . ? C52 C51 C56 N12 179.9(5) . . . . ? N11 C51 C56 N12 -0.2(6) . . . . ? C52 C51 C56 C55 -1.9(9) . . . . ? N11 C51 C56 C55 178.0(5) . . . . ? C54 C55 C56 N12 -179.4(5) . . . . ? C54 C55 C56 C51 2.8(8) . . . . ? O1 C58 C59 O2 74.7(5) . . . . ? O2 C60 C61 O3 63.5(5) . . . . ? O3 C62 C63 O4 83.5(5) . . . . ? O4 C64 C65 O5 63.9(6) . . . . ? O6 C66 C67 O7 76.9(5) . . . . ? O7 C68 C69 O8 -70.0(6) . . . . ? O8 C70 C71 O9 54.9(6) . . . . ? O9 C72 C73 O10 -180.0(4) . . . . ? O11 C74 C75 O12 -173.7(4) . . . . ? O12 C76 C77 O13 76.3(6) . . . . ? O13 C78 C79 O14 68.2(6) . . . . ? O14 C80 C81 O15 -71.9(5) . . . . ? C2 C1 N1 C12 4.2(6) . . . . ? C2 C1 N1 Pd1 -173.0(3) . . . . ? C4 C12 N1 C1 -4.9(6) . . . . ? C11 C12 N1 C1 173.5(4) . . . . ? C4 C12 N1 Pd1 172.7(4) . . . . ? C11 C12 N1 Pd1 -8.8(5) . . . . ? C7 C11 N2 C10 1.8(7) . . . . ? C12 C11 N2 C10 -177.5(4) . . . . ? C7 C11 N2 Pd1 -172.3(4) . . . . ? C12 C11 N2 Pd1 8.4(5) . . . . ? C9 C10 N2 C11 -1.2(7) . . . . ? C9 C10 N2 Pd1 171.9(3) . . . . ? C14 C13 N3 C24 -0.6(6) . . . . ? C14 C13 N3 Pd2 -173.5(3) . . . . ? C16 C24 N3 C13 1.1(6) . . . . ? C23 C24 N3 C13 179.5(4) . . . . ? C16 C24 N3 Pd2 175.2(4) . . . . ? C23 C24 N3 Pd2 -6.4(5) . . . . ? C21 C22 N4 C23 1.9(7) . . . . ? C21 C22 N4 Pd2 177.1(3) . . . . ? C19 C23 N4 C22 0.6(6) . . . . ? C24 C23 N4 C22 -179.2(4) . . . . ? C19 C23 N4 Pd2 -175.4(4) . . . . ? C24 C23 N4 Pd2 4.8(5) . . . . ? C26 C25 N5 C35 -2.2(6) . . . . ? C26 C25 N5 Pd3 -177.2(3) . . . . ? C36 C35 N5 C25 179.7(4) . . . . ? C28 C35 N5 C25 3.0(6) . . . . ? C36 C35 N5 Pd3 -4.4(5) . . . . ? C28 C35 N5 Pd3 178.8(4) . . . . ? C33 C34 N6 C36 0.6(7) . . . . ? C33 C34 N6 Pd3 178.2(3) . . . . ? C31 C36 N6 C34 -1.2(7) . . . . ? C35 C36 N6 C34 -178.0(4) . . . . ? C31 C36 N6 Pd3 -179.2(4) . . . . ? C35 C36 N6 Pd3 4.0(5) . . . . ? N8 C43 N7 C37 0.6(5) . . . . ? N8 C43 N7 Pd1 170.6(3) . . . . ? C38 C37 N7 C43 -178.9(6) . . . . ? C42 C37 N7 C43 -0.2(5) . . . . ? C38 C37 N7 Pd1 9.9(7) . . . . ? C42 C37 N7 Pd1 -171.4(3) . . . . ? N7 C43 N8 C42 -0.7(5) . . . . ? N7 C43 N8 Pd2 -161.0(3) . . . . ? C37 C42 N8 C43 0.6(5) . . . . ? C41 C42 N8 C43 -176.7(6) . . . . ? C37 C42 N8 Pd2 162.8(3) . . . . ? C41 C42 N8 Pd2 -14.5(7) . . . . ? N10 C50 N9 C44 1.3(4) . . . . ? N10 C50 N9 Pd2 170.9(3) . . . . ? C45 C44 N9 C50 179.9(5) . . . . ? C49 C44 N9 C50 -0.7(4) . . . . ? C45 C44 N9 Pd2 9.1(6) . . . . ? C49 C44 N9 Pd2 -171.5(2) . . . . ? N9 C50 N10 C49 -1.4(4) . . . . ? N9 C50 N10 Pd3 -167.7(3) . . . . ? C44 C49 N10 C50 0.9(4) . . . . ? C48 C49 N10 C50 177.4(5) . . . . ? C44 C49 N10 Pd3 167.3(2) . . . . ? C48 C49 N10 Pd3 -16.2(6) . . . . ? N12 C57 N11 C51 1.1(5) . . . . ? N12 C57 N11 Pd3 170.7(3) . . . . ? C52 C51 N11 C57 179.3(6) . . . . ? C56 C51 N11 C57 -0.5(5) . . . . ? C52 C51 N11 Pd3 8.8(7) . . . . ? C56 C51 N11 Pd3 -171.0(3) . . . . ? C51 C56 N12 C57 0.9(5) . . . . ? C55 C56 N12 C57 -177.1(6) . . . . ? C51 C56 N12 Pd1 167.6(3) . . . . ? C55 C56 N12 Pd1 -10.3(7) . . . . ? N11 C57 N12 C56 -1.3(5) . . . . ? N11 C57 N12 Pd1 -167.6(3) . . . . ? C6 C5 O1 C58 97.9(5) . . . . ? C4 C5 O1 C58 -83.1(5) . . . . ? C59 C58 O1 C5 176.9(4) . . . . ? C58 C59 O2 C60 91.5(5) . . . . ? C61 C60 O2 C59 177.8(4) . . . . ? C63 C62 O3 C61 175.8(4) . . . . ? C60 C61 O3 C62 85.9(5) . . . . ? C65 C64 O4 C63 115.7(5) . . . . ? C62 C63 O4 C64 -92.1(5) . . . . ? C5 C6 O5 C65 27.7(6) . . . . ? C7 C6 O5 C65 -153.1(4) . . . . ? C64 C65 O5 C6 165.2(4) . . . . ? C18 C17 O6 C66 96.3(5) . . . . ? C16 C17 O6 C66 -85.7(5) . . . . ? C67 C66 O6 C17 -164.8(4) . . . . ? C66 C67 O7 C68 -174.3(4) . . . . ? C69 C68 O7 C67 179.4(4) . . . . ? C71 C70 O8 C69 -177.8(4) . . . . ? C68 C69 O8 C70 147.9(4) . . . . ? C73 C72 O9 C71 -128.0(5) . . . . ? C70 C71 O9 C72 63.4(6) . . . . ? C17 C18 O10 C73 51.5(6) . . . . ? C19 C18 O10 C73 -133.7(4) . . . . ? C72 C73 O10 C18 149.1(4) . . . . ? C30 C29 O11 C74 -36.6(6) . . . . ? C28 C29 O11 C74 143.4(3) . . . . ? C75 C74 O11 C29 -170.6(4) . . . . ? C74 C75 O12 C76 100.3(5) . . . . ? C77 C76 O12 C75 -162.5(4) . . . . ? C79 C78 O13 C77 -135.4(5) . . . . ? C76 C77 O13 C78 84.9(6) . . . . ? C78 C79 O14 C80 166.9(4) . . . . ? C81 C80 O14 C79 175.0(4) . . . . ? C29 C30 O15 C81 -93.6(5) . . . . ? C31 C30 O15 C81 88.5(5) . . . . ? C80 C81 O15 C30 -174.2(4) . . . . ? C56 N12 Pd1 N7 -101.7(4) . . . . ? C57 N12 Pd1 N7 62.2(4) . . . . ? C56 N12 Pd1 N1 71.5(4) . . . . ? C57 N12 Pd1 N1 -124.7(4) . . . . ? C43 N7 Pd1 N12 -66.6(4) . . . . ? C37 N7 Pd1 N12 102.0(3) . . . . ? C43 N7 Pd1 N2 119.0(4) . . . . ? C37 N7 Pd1 N2 -72.4(3) . . . . ? C1 N1 Pd1 N12 12.5(4) . . . . ? C12 N1 Pd1 N12 -164.9(3) . . . . ? C1 N1 Pd1 N2 -172.5(4) . . . . ? C12 N1 Pd1 N2 10.1(3) . . . . ? C11 N2 Pd1 N7 163.3(3) . . . . ? C10 N2 Pd1 N7 -10.3(4) . . . . ? C11 N2 Pd1 N1 -10.1(3) . . . . ? C10 N2 Pd1 N1 176.3(4) . . . . ? C50 N9 Pd2 N4 120.1(3) . . . . ? C44 N9 Pd2 N4 -72.0(3) . . . . ? C50 N9 Pd2 N8 -63.3(3) . . . . ? C44 N9 Pd2 N8 104.6(3) . . . . ? C22 N4 Pd2 N9 -7.0(4) . . . . ? C23 N4 Pd2 N9 168.5(3) . . . . ? C22 N4 Pd2 N3 178.1(4) . . . . ? C23 N4 Pd2 N3 -6.3(3) . . . . ? C13 N3 Pd2 N4 -179.9(4) . . . . ? C24 N3 Pd2 N4 6.9(3) . . . . ? C13 N3 Pd2 N8 3.2(4) . . . . ? C24 N3 Pd2 N8 -170.0(3) . . . . ? C43 N8 Pd2 N9 58.6(4) . . . . ? C42 N8 Pd2 N9 -99.2(3) . . . . ? C43 N8 Pd2 N3 -126.8(4) . . . . ? C42 N8 Pd2 N3 75.4(3) . . . . ? C57 N11 Pd3 N10 -67.8(4) . . . . ? C51 N11 Pd3 N10 100.3(3) . . . . ? C57 N11 Pd3 N6 114.2(4) . . . . ? C51 N11 Pd3 N6 -77.7(3) . . . . ? C50 N10 Pd3 N11 63.9(3) . . . . ? C49 N10 Pd3 N11 -99.9(3) . . . . ? C50 N10 Pd3 N5 -120.9(3) . . . . ? C49 N10 Pd3 N5 75.3(3) . . . . ? C34 N6 Pd3 N11 -7.3(4) . . . . ? C36 N6 Pd3 N11 170.5(3) . . . . ? C34 N6 Pd3 N5 177.3(4) . . . . ? C36 N6 Pd3 N5 -4.9(3) . . . . ? C25 N5 Pd3 N10 2.2(3) . . . . ? C35 N5 Pd3 N10 -173.1(2) . . . . ? C25 N5 Pd3 N6 -179.6(4) . . . . ? C35 N5 Pd3 N6 5.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.329 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.076 # Attachment '2051h4.cif' data_2051h4 _database_code_depnum_ccdc_archive 'CCDC 757502' #TrackingRef '2051h4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H51 N12 Pd3, 3(F6 P), 3(C2 H3 N)' _chemical_formula_sum 'C63 H60 F18 N15 P3 Pd3' _chemical_formula_weight 1781.37 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pmna ' _symmetry_space_group_name_Hall '-P 2ac 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x, -y, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x-1/2, -y, z-1/2' '-x, y, z' _cell_length_a 31.371(6) _cell_length_b 18.990(4) _cell_length_c 12.262(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7305(3) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.8144 _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 area detector' _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 18722 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7331 _reflns_number_gt 5475 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^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 7331 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.16769(16) 0.2649(3) 0.1538(4) 0.0486(11) Uani 1 1 d . . . H1 H 0.1496 0.2271 0.1676 0.058 Uiso 1 1 calc R . . C2 C 0.20813(15) 0.2517(3) 0.1180(4) 0.0507(12) Uani 1 1 d . . . H2 H 0.2171 0.2056 0.1076 0.061 Uiso 1 1 calc R . . C3 C 0.23586(15) 0.3070(3) 0.0971(5) 0.0543(12) Uani 1 1 d . . . C4 C 0.27951(16) 0.2891(3) 0.0556(5) 0.0594(13) Uani 1 1 d . . . H4A H 0.2825 0.3056 -0.0180 0.089 Uiso 1 1 calc R . . H4B H 0.2834 0.2390 0.0575 0.089 Uiso 1 1 calc R . . H4C H 0.3006 0.3114 0.1008 0.089 Uiso 1 1 calc R . . C5 C 0.22125(15) 0.3732(3) 0.1107(4) 0.0506(12) Uani 1 1 d . . . H5 H 0.2392 0.4109 0.0959 0.061 Uiso 1 1 calc R . . C6 C 0.17951(14) 0.3864(2) 0.1466(4) 0.0405(9) Uani 1 1 d . . . C7 C 0.16041(13) 0.4554(2) 0.1612(3) 0.0380(9) Uani 1 1 d . . . C8 C 0.18190(14) 0.5187(2) 0.1551(4) 0.0455(11) Uani 1 1 d . . . H8 H 0.2108 0.5185 0.1385 0.055 Uiso 1 1 calc R . . C9 C 0.16174(17) 0.5822(3) 0.1728(4) 0.0538(12) Uani 1 1 d . . . C10 C 0.18564(18) 0.6518(3) 0.1724(4) 0.0536(12) Uani 1 1 d . . . H10A H 0.1716 0.6842 0.1241 0.080 Uiso 1 1 calc R . . H10B H 0.2144 0.6442 0.1480 0.080 Uiso 1 1 calc R . . H10C H 0.1860 0.6710 0.2448 0.080 Uiso 1 1 calc R . . C11 C 0.11762(19) 0.5790(3) 0.1877(5) 0.0630(14) Uani 1 1 d . . . H11 H 0.1021 0.6206 0.1927 0.076 Uiso 1 1 calc R . . C12 C 0.09706(15) 0.5161(2) 0.1952(5) 0.0509(12) Uani 1 1 d . . . H12 H 0.0679 0.5157 0.2083 0.061 Uiso 1 1 calc R . . C13 C 0.0000 0.3849(3) 0.2041(5) 0.0393(13) Uani 1 2 d S . . H13 H 0.0000 0.3792 0.1287 0.047 Uiso 1 2 calc SR . . C14 C 0.02209(13) 0.3952(2) 0.3710(4) 0.0407(9) Uani 1 1 d . . . C15 C 0.04599(16) 0.4007(3) 0.4660(4) 0.0540(12) Uani 1 1 d . . . H15 H 0.0756 0.4016 0.4653 0.065 Uiso 1 1 calc R . . C16 C 0.02304(17) 0.4047(3) 0.5604(4) 0.0542(12) Uani 1 1 d . . . H16 H 0.0375 0.4074 0.6266 0.065 Uiso 1 1 calc R . . C17 C 0.05157(14) 0.2180(3) 0.1926(4) 0.0479(11) Uani 1 1 d . . . H17 H 0.0401 0.2324 0.1263 0.057 Uiso 1 1 calc R . . C18 C 0.08694(13) 0.2191(3) 0.3416(4) 0.0463(10) Uani 1 1 d . . . C19 C 0.11237(16) 0.2348(3) 0.4323(4) 0.0532(12) Uani 1 1 d . . . H19 H 0.1251 0.2787 0.4407 0.064 Uiso 1 1 calc R . . C20 C 0.1175(2) 0.1826(3) 0.5082(5) 0.0708(16) Uani 1 1 d . . . H20 H 0.1346 0.1907 0.5689 0.085 Uiso 1 1 calc R . . C21 C 0.09729(19) 0.1164(3) 0.4957(6) 0.0689(16) Uani 1 1 d . . . H21 H 0.1011 0.0824 0.5494 0.083 Uiso 1 1 calc R . . C22 C 0.07270(18) 0.1008(3) 0.4091(5) 0.0627(14) Uani 1 1 d . . . H22 H 0.0598 0.0570 0.4015 0.075 Uiso 1 1 calc R . . C23 C 0.06752(13) 0.1540(3) 0.3309(5) 0.0495(11) Uani 1 1 d . . . C24 C 0.08490(16) 0.0111(3) 0.1539(5) 0.0566(13) Uani 1 1 d . . . H24 H 0.0975 0.0543 0.1693 0.068 Uiso 1 1 calc R . . C25 C 0.11032(18) -0.0460(3) 0.1351(4) 0.0577(13) Uani 1 1 d . . . H25 H 0.1398 -0.0416 0.1374 0.069 Uiso 1 1 calc R . . C26 C 0.09194(19) -0.1101(3) 0.1128(5) 0.0659(15) Uani 1 1 d . . . C27 C 0.11921(17) -0.1761(3) 0.0933(5) 0.0601(14) Uani 1 1 d . . . H27A H 0.1009 -0.2160 0.0826 0.090 Uiso 1 1 calc R . . H27B H 0.1372 -0.1841 0.1554 0.090 Uiso 1 1 calc R . . H27C H 0.1366 -0.1693 0.0297 0.090 Uiso 1 1 calc R . . C28 C 0.04857(17) -0.1150(3) 0.1069(4) 0.0541(12) Uani 1 1 d . . . H28 H 0.0359 -0.1578 0.0894 0.065 Uiso 1 1 calc R . . C29 C 0.02344(16) -0.0566(3) 0.1270(4) 0.0512(12) Uani 1 1 d . . . C30 C 0.18874(19) 0.0837(3) 0.2946(5) 0.0649(15) Uani 1 1 d . . . C31 C 0.20987(18) 0.0613(3) 0.3940(5) 0.0602(14) Uani 1 1 d . . . H31B H 0.2258 0.0191 0.3800 0.072 Uiso 1 1 calc R . . H31C H 0.1889 0.0522 0.4493 0.072 Uiso 1 1 calc R . . H31A H 0.2289 0.0977 0.4183 0.072 Uiso 1 1 calc R . . C32 C 1.0000 0.1321(5) 0.6098(8) 0.072(2) Uani 1 2 d S . . H33A H 0.9756 0.2287 0.6117 0.108 Uiso 1 1 d R . . H33C H 1.0000 0.2132 0.5070 0.108 Uiso 1 2 d SR . . C33 C 1.0000 0.2058(4) 0.5837(7) 0.0601(19) Uani 1 2 d S . . F1 F 0.03549(10) 0.36424(15) 0.9654(3) 0.0619(8) Uani 1 1 d . . . F2 F 0.03553(10) 0.29850(17) 0.8153(3) 0.0669(8) Uani 1 1 d . . . F3 F 0.0000 0.4016(2) 0.8192(3) 0.0569(10) Uani 1 2 d S . . F4 F 0.0000 0.2634(2) 0.9672(4) 0.0636(11) Uani 1 2 d S . . F5 F 0.21238(10) 0.45801(15) 0.5616(2) 0.0602(8) Uani 1 1 d . . . F6 F 0.17748(10) 0.44492(16) 0.4039(3) 0.0602(8) Uani 1 1 d . . . F7 F 0.14166(10) 0.45962(15) 0.5634(3) 0.0595(7) Uani 1 1 d . . . F8 F 0.23071(10) 0.07833(17) 0.8235(3) 0.0646(8) Uani 1 1 d . . . F9 F 0.20685(10) 0.13811(16) 0.6838(2) 0.0596(8) Uani 1 1 d . . . F10 F 0.23146(10) 0.19538(18) 0.8303(3) 0.0661(8) Uani 1 1 d . . . N1 N 0.15317(11) 0.3306(2) 0.1697(3) 0.0446(9) Uani 1 1 d . . . N2 N 0.11766(11) 0.4546(2) 0.1842(3) 0.0403(8) Uani 1 1 d . . . N3 N 0.03555(12) 0.3892(2) 0.2622(3) 0.0440(8) Uani 1 1 d . . . N4 N 0.07640(12) 0.2585(2) 0.2507(3) 0.0455(9) Uani 1 1 d . . . N5 N 0.04370(12) 0.1542(2) 0.2354(4) 0.0491(9) Uani 1 1 d . . . N6 N 0.04160(11) 0.0063(2) 0.1507(3) 0.0465(9) Uani 1 1 d . . . N7 N 0.17355(14) 0.0969(3) 0.2111(4) 0.0615(11) Uani 1 1 d . . . N8 N 1.0000 0.0728(4) 0.6288(6) 0.0685(18) Uani 1 2 d S . . P1 P 0.0000 0.33226(10) 0.88876(15) 0.0507(4) Uani 1 2 d S . . P2 P 0.17618(6) 0.5000 0.5000 0.0505(4) Uani 1 2 d S . . P3 P 0.2500 0.13970(11) 0.7500 0.0602(5) Uani 1 2 d S . 1 Pd1 Pd 0.094184(11) 0.358279(19) 0.21642(3) 0.04361(11) Uani 1 1 d . . . Pd2 Pd 0.0000 0.08321(3) 0.18970(5) 0.04423(14) Uani 1 2 d S . . 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 0.044(2) 0.045(3) 0.057(3) 0.009(2) 0.005(2) -0.001(2) C2 0.046(3) 0.048(3) 0.059(3) 0.001(2) 0.018(2) 0.013(2) C3 0.033(2) 0.055(3) 0.075(3) 0.007(2) 0.012(2) 0.011(2) C4 0.046(3) 0.069(3) 0.062(3) 0.003(3) 0.003(2) 0.015(3) C5 0.033(2) 0.052(3) 0.067(3) 0.006(2) 0.014(2) -0.002(2) C6 0.041(2) 0.043(2) 0.037(2) 0.0037(18) 0.0136(18) -0.0040(18) C7 0.035(2) 0.037(2) 0.042(2) 0.0068(18) 0.0088(18) 0.0024(17) C8 0.034(2) 0.037(2) 0.065(3) 0.000(2) 0.013(2) -0.0050(17) C9 0.052(3) 0.053(3) 0.057(3) -0.003(2) 0.004(2) -0.004(2) C10 0.063(3) 0.036(2) 0.061(3) -0.004(2) 0.018(3) -0.006(2) C11 0.062(3) 0.050(3) 0.077(4) -0.004(3) 0.012(3) 0.012(2) C12 0.039(2) 0.040(2) 0.073(3) -0.001(2) 0.005(2) 0.0088(18) C13 0.037(3) 0.053(4) 0.028(3) 0.002(2) 0.000 0.000 C14 0.031(2) 0.043(2) 0.049(2) -0.0096(19) 0.0030(18) 0.0017(18) C15 0.043(3) 0.072(3) 0.046(3) -0.002(2) -0.007(2) -0.001(2) C16 0.057(3) 0.055(3) 0.051(3) -0.017(2) -0.006(2) 0.002(2) C17 0.039(2) 0.049(3) 0.055(3) 0.003(2) 0.001(2) 0.000(2) C18 0.0296(19) 0.056(3) 0.053(3) 0.006(2) 0.0031(19) -0.007(2) C19 0.040(2) 0.060(3) 0.060(3) 0.012(2) -0.001(2) -0.004(2) C20 0.070(4) 0.071(4) 0.071(4) 0.014(3) -0.025(3) 0.001(3) C21 0.068(4) 0.056(3) 0.083(4) 0.018(3) -0.005(3) 0.006(3) C22 0.048(3) 0.066(3) 0.074(4) 0.009(3) 0.005(3) 0.005(3) C23 0.0261(19) 0.055(3) 0.068(3) 0.010(2) 0.004(2) 0.0043(19) C24 0.047(3) 0.049(3) 0.074(3) -0.003(3) 0.015(3) 0.000(2) C25 0.048(3) 0.069(3) 0.056(3) -0.007(3) 0.000(2) 0.013(3) C26 0.059(3) 0.077(4) 0.061(3) -0.014(3) 0.013(3) 0.018(3) C27 0.051(3) 0.066(3) 0.062(3) -0.019(3) -0.005(3) 0.024(3) C28 0.051(3) 0.045(3) 0.066(3) -0.012(2) -0.001(2) 0.009(2) C29 0.044(3) 0.049(3) 0.061(3) -0.006(2) 0.002(2) -0.002(2) C30 0.059(3) 0.066(4) 0.069(3) 0.018(3) 0.006(3) -0.009(3) C31 0.051(3) 0.068(3) 0.062(3) 0.002(3) 0.003(3) 0.021(3) C32 0.082(6) 0.066(5) 0.068(5) -0.007(4) 0.000 0.000 C33 0.066(5) 0.049(4) 0.066(5) -0.003(3) 0.000 0.000 F1 0.0670(19) 0.0516(16) 0.0672(19) -0.0160(14) 0.0030(15) -0.0179(14) F2 0.0666(19) 0.0591(18) 0.075(2) -0.0188(16) 0.0115(16) 0.0066(15) F3 0.065(3) 0.049(2) 0.056(2) 0.0118(18) 0.000 0.000 F4 0.063(3) 0.072(3) 0.055(2) 0.016(2) 0.000 0.000 F5 0.0654(19) 0.0554(16) 0.0596(17) -0.0165(14) -0.0322(15) 0.0115(14) F6 0.0575(17) 0.0627(18) 0.0605(18) -0.0182(14) -0.0153(14) -0.0094(14) F7 0.0597(18) 0.0548(16) 0.0640(17) 0.0117(14) 0.0021(14) -0.0156(14) F8 0.0615(18) 0.067(2) 0.0656(19) 0.0113(15) 0.0025(15) -0.0063(15) F9 0.0677(19) 0.0537(17) 0.0575(17) 0.0138(13) -0.0138(15) -0.0052(14) F10 0.0631(18) 0.071(2) 0.0646(19) -0.0142(16) -0.0027(15) 0.0062(16) N1 0.0313(17) 0.046(2) 0.056(2) -0.0030(17) 0.0028(17) -0.0044(15) N2 0.0271(16) 0.050(2) 0.043(2) 0.0044(16) -0.0001(15) 0.0045(15) N3 0.0393(19) 0.057(2) 0.0361(18) -0.0042(17) 0.0062(15) -0.0042(17) N4 0.0358(19) 0.048(2) 0.052(2) 0.0049(18) 0.0060(17) -0.0095(16) N5 0.0362(18) 0.043(2) 0.068(3) -0.0030(18) 0.0045(18) -0.0007(16) N6 0.0350(18) 0.048(2) 0.057(2) 0.0084(18) 0.0052(17) 0.0007(16) N7 0.043(2) 0.068(3) 0.073(3) 0.009(2) -0.005(2) -0.006(2) N8 0.071(4) 0.070(4) 0.065(4) 0.015(3) 0.000 0.000 P1 0.0641(11) 0.0479(10) 0.0400(9) -0.0013(7) 0.000 0.000 P2 0.0410(9) 0.0536(10) 0.0571(11) -0.0023(8) 0.000 0.000 P3 0.0595(11) 0.0604(12) 0.0607(11) 0.000 0.0018(10) 0.000 Pd1 0.04202(19) 0.0434(2) 0.0454(2) -0.00055(14) 0.00434(15) -0.00397(14) Pd2 0.0356(2) 0.0365(2) 0.0606(3) 0.0039(2) 0.000 0.000 _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 1.343(5) . ? C1 C2 1.365(6) . ? C1 H1 0.9300 . ? C2 C3 1.387(7) . ? C2 H2 0.9300 . ? C3 C5 1.348(7) . ? C3 C4 1.500(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.404(6) . ? C5 H5 0.9300 . ? C6 N1 1.374(4) . ? C6 C7 1.452(6) . ? C7 N2 1.371(4) . ? C7 C8 1.379(6) . ? C8 C9 1.379(7) . ? C8 H8 0.9300 . ? C9 C11 1.397(8) . ? C9 C10 1.520(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.361(8) . ? C11 H11 0.9300 . ? C12 N2 1.341(5) . ? C12 H12 0.9300 . ? C13 N3 1.326(4) . ? C13 N3 1.326(4) 8 ? C13 H13 0.9300 . ? C14 C14 1.386(8) 8 ? C14 C15 1.389(7) . ? C14 N3 1.404(4) . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 C16 1.446(11) 8 ? C16 H16 0.9300 . ? C17 N4 1.306(5) . ? C17 N5 1.344(5) . ? C17 H17 0.9300 . ? C18 N4 1.382(5) . ? C18 C23 1.384(7) . ? C18 C19 1.401(7) . ? C19 C20 1.369(7) . ? C19 H19 0.9300 . ? C20 C21 1.417(9) . ? C20 H20 0.9300 . ? C21 C22 1.345(9) . ? C21 H21 0.9300 . ? C22 C23 1.402(7) . ? C22 H22 0.9300 . ? C23 N5 1.390(5) . ? C24 N6 1.362(5) . ? C24 C25 1.366(7) . ? C24 H24 0.9300 . ? C25 C26 1.373(9) . ? C25 H25 0.9300 . ? C26 C28 1.365(8) . ? C26 C27 1.536(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.383(7) . ? C28 H28 0.9300 . ? C29 N6 1.355(5) . ? C29 C29 1.471(10) 8 ? C30 N7 1.157(6) . ? C30 C31 1.451(8) . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C31 H31A 0.9600 . ? C32 N8 1.151(9) . ? C32 C33 1.436(12) . ? C33 H33A 0.9438 . ? C33 H33C 0.9506 . ? F1 P1 1.579(3) . ? F2 P1 1.570(3) . ? F3 P1 1.569(4) . ? F4 P1 1.623(5) . ? F5 P2 1.580(3) . ? F6 P2 1.576(3) . ? F7 P2 1.538(3) . ? F8 P3 1.592(3) . ? F9 P3 1.579(3) . ? F10 P3 1.558(3) . ? N1 Pd1 2.007(4) . ? N2 Pd1 2.012(4) . ? N3 Pd1 2.011(4) . ? N4 Pd1 2.019(4) . ? N5 Pd2 2.002(4) . ? N6 Pd2 2.016(4) . ? P1 F2 1.570(3) 8 ? P1 F1 1.579(3) 8 ? P2 F7 1.538(3) 4_566 ? P2 F6 1.576(3) 4_566 ? P2 F5 1.580(3) 4_566 ? P3 F10 1.558(3) 3_556 ? P3 F9 1.579(3) 3_556 ? P3 F8 1.592(3) 3_556 ? Pd2 N5 2.002(4) 8 ? Pd2 N6 2.016(4) 8 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.1(4) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 120.3(5) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C5 C3 C2 118.0(4) . . ? C5 C3 C4 124.3(5) . . ? C2 C3 C4 117.7(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 C6 121.5(5) . . ? C3 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? N1 C6 C5 119.1(4) . . ? N1 C6 C7 115.0(3) . . ? C5 C6 C7 125.8(4) . . ? N2 C7 C8 120.0(4) . . ? N2 C7 C6 114.8(3) . . ? C8 C7 C6 125.3(4) . . ? C9 C8 C7 121.9(4) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C11 115.9(5) . . ? C8 C9 C10 122.3(5) . . ? C11 C9 C10 121.8(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 121.1(5) . . ? C12 C11 H11 119.5 . . ? C9 C11 H11 119.5 . . ? N2 C12 C11 122.0(4) . . ? N2 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N3 C13 N3 114.5(4) . 8 ? N3 C13 H13 122.7 . . ? N3 C13 H13 122.7 8 . ? C14 C14 C15 122.7(3) 8 . ? C14 C14 N3 107.49(17) 8 . ? C15 C14 N3 129.8(4) . . ? C16 C15 C14 115.5(5) . . ? C16 C15 H15 122.2 . . ? C14 C15 H15 122.2 . . ? C15 C16 C16 121.8(3) . 8 ? C15 C16 H16 119.1 . . ? C16 C16 H16 119.1 8 . ? N4 C17 N5 115.4(4) . . ? N4 C17 H17 122.3 . . ? N5 C17 H17 122.3 . . ? N4 C18 C23 107.6(4) . . ? N4 C18 C19 131.4(4) . . ? C23 C18 C19 121.0(5) . . ? C20 C19 C18 116.9(5) . . ? C20 C19 H19 121.5 . . ? C18 C19 H19 121.5 . . ? C19 C20 C21 121.1(6) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 122.5(6) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C23 116.6(6) . . ? C21 C22 H22 121.7 . . ? C23 C22 H22 121.7 . . ? C18 C23 N5 108.3(4) . . ? C18 C23 C22 121.9(5) . . ? N5 C23 C22 129.8(5) . . ? N6 C24 C25 121.6(5) . . ? N6 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 119.4(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C28 C26 C25 119.3(5) . . ? C28 C26 C27 119.4(6) . . ? C25 C26 C27 121.3(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 C29 120.3(5) . . ? C26 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? N6 C29 C28 120.4(4) . . ? N6 C29 C29 114.9(2) . 8 ? C28 C29 C29 124.8(3) . 8 ? N7 C30 C31 174.3(6) . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? H31C C31 H31A 109.5 . . ? N8 C32 C33 178.8(9) . . ? C32 C33 H33A 111.5 . . ? C32 C33 H33C 111.4 . . ? H33A C33 H33C 107.0 . . ? C1 N1 C6 118.9(3) . . ? C1 N1 Pd1 126.7(2) . . ? C6 N1 Pd1 114.3(2) . . ? C12 N2 C7 118.8(3) . . ? C12 N2 Pd1 126.6(2) . . ? C7 N2 Pd1 114.1(2) . . ? C13 N3 C14 105.2(3) . . ? C13 N3 Pd1 127.0(2) . . ? C14 N3 Pd1 124.3(2) . . ? C17 N4 C18 105.3(3) . . ? C17 N4 Pd1 127.1(3) . . ? C18 N4 Pd1 127.6(2) . . ? C17 N5 C23 103.4(3) . . ? C17 N5 Pd2 128.6(3) . . ? C23 N5 Pd2 127.1(3) . . ? C29 N6 C24 119.0(3) . . ? C29 N6 Pd2 114.7(2) . . ? C24 N6 Pd2 126.1(3) . . ? F3 P1 F2 91.79(19) . 8 ? F3 P1 F2 91.79(19) . . ? F2 P1 F2 90.5(3) 8 . ? F3 P1 F1 90.04(18) . . ? F2 P1 F1 178.1(2) 8 . ? F2 P1 F1 89.89(17) . . ? F3 P1 F1 90.04(18) . 8 ? F2 P1 F1 89.89(17) 8 8 ? F2 P1 F1 178.1(2) . 8 ? F1 P1 F1 89.7(2) . 8 ? F3 P1 F4 176.6(3) . . ? F2 P1 F4 90.61(19) 8 . ? F2 P1 F4 90.61(19) . . ? F1 P1 F4 87.55(19) . . ? F1 P1 F4 87.55(19) 8 . ? F7 P2 F7 90.5(3) . 4_566 ? F7 P2 F6 93.75(18) . . ? F7 P2 F6 88.33(17) 4_566 . ? F7 P2 F6 88.33(17) . 4_566 ? F7 P2 F6 93.75(17) 4_566 4_566 ? F6 P2 F6 177.0(3) . 4_566 ? F7 P2 F5 90.74(17) . . ? F7 P2 F5 178.17(18) 4_566 . ? F6 P2 F5 90.23(16) . . ? F6 P2 F5 87.64(16) 4_566 . ? F7 P2 F5 178.17(18) . 4_566 ? F7 P2 F5 90.74(17) 4_566 4_566 ? F6 P2 F5 87.65(16) . 4_566 ? F6 P2 F5 90.23(16) 4_566 4_566 ? F5 P2 F5 88.1(3) . 4_566 ? F10 P3 F10 94.5(3) . 3_556 ? F10 P3 F9 90.45(17) . 3_556 ? F10 P3 F9 91.03(18) 3_556 3_556 ? F10 P3 F9 91.03(18) . . ? F10 P3 F9 90.45(17) 3_556 . ? F9 P3 F9 177.8(3) 3_556 . ? F10 P3 F8 175.1(2) . 3_556 ? F10 P3 F8 89.84(18) 3_556 3_556 ? F9 P3 F8 87.21(17) 3_556 3_556 ? F9 P3 F8 91.19(18) . 3_556 ? F10 P3 F8 89.84(18) . . ? F10 P3 F8 175.1(2) 3_556 . ? F9 P3 F8 91.19(18) 3_556 . ? F9 P3 F8 87.21(17) . . ? F8 P3 F8 85.9(3) 3_556 . ? N1 Pd1 N3 178.19(16) . . ? N1 Pd1 N2 81.07(15) . . ? N3 Pd1 N2 97.12(15) . . ? N1 Pd1 N4 93.92(16) . . ? N3 Pd1 N4 87.89(15) . . ? N2 Pd1 N4 174.55(15) . . ? N5 Pd2 N5 86.4(2) . 8 ? N5 Pd2 N6 175.62(16) . 8 ? N5 Pd2 N6 96.37(16) 8 8 ? N5 Pd2 N6 96.37(16) . . ? N5 Pd2 N6 175.62(16) 8 . ? N6 Pd2 N6 80.6(2) 8 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.475 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.093 # Attachment '1993cRevised.cif' data_1993c _database_code_depnum_ccdc_archive 'CCDC 758057' #TrackingRef '1993cRevised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C93 H87 N12 O15 Pd3, C4 H10 O, 3(F6 P), 3(C2 H3 N)' _chemical_formula_sum 'C103 H106 F18 N15 O16 P3 Pd3' _chemical_formula_weight 2564.14 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 14.013(3) _cell_length_b 18.506(4) _cell_length_c 22.193(4) _cell_angle_alpha 97.49(2) _cell_angle_beta 100.866(8) _cell_angle_gamma 97.15(2) _cell_volume 5537.8(19) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3716 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 23.42 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2604 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8251 _exptl_absorpt_correction_T_max 0.8645 _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 32622 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 25.10 _reflns_number_total 19302 _reflns_number_gt 13416 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+0.55P] 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 19302 _refine_ls_number_parameters 1427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.8285(3) 0.3130(2) 0.91940(18) 0.0556(9) Uani 1 1 d . . . H1 H 0.8514 0.3508 0.8995 0.067 Uiso 1 1 calc R . . C2 C 0.7642(3) 0.3270(2) 0.9588(2) 0.0602(10) Uani 1 1 d . . . H2 H 0.7457 0.3734 0.9658 0.072 Uiso 1 1 calc R . . C3 C 0.7298(3) 0.2725(2) 0.98630(18) 0.0539(9) Uani 1 1 d . . . H3 H 0.6849 0.2811 1.0114 0.065 Uiso 1 1 calc R . . C4 C 0.7587(3) 0.2024(2) 0.97894(18) 0.0517(9) Uani 1 1 d . . . C5 C 0.7278(3) 0.1438(2) 1.00765(17) 0.0500(8) Uani 1 1 d . . . C6 C 0.7624(2) 0.07679(19) 0.99653(17) 0.0436(8) Uani 1 1 d . . . C7 C 0.8270(3) 0.0684(2) 0.95623(17) 0.0498(8) Uani 1 1 d . . . C8 C 0.8659(3) 0.0012(2) 0.94239(19) 0.0564(9) Uani 1 1 d . . . H8 H 0.8512 -0.0387 0.9623 0.068 Uiso 1 1 calc R . . C9 C 0.9246(3) -0.0036(2) 0.89953(19) 0.0572(10) Uani 1 1 d . . . H9 H 0.9466 -0.0477 0.8880 0.069 Uiso 1 1 calc R . . C10 C 0.9512(3) 0.0595(2) 0.87313(17) 0.0513(9) Uani 1 1 d . . . H10 H 0.9937 0.0565 0.8457 0.062 Uiso 1 1 calc R . . C11 C 0.8572(3) 0.1271(2) 0.9275(2) 0.0584(10) Uani 1 1 d . . . C12 C 0.8231(3) 0.1941(2) 0.93866(18) 0.0542(9) Uani 1 1 d . . . C13 C 1.1102(3) -0.0007(2) 0.6478(2) 0.0604(10) Uani 1 1 d . . . H13 H 1.0978 0.0170 0.6863 0.072 Uiso 1 1 calc R . . C14 C 1.1295(3) -0.0717(2) 0.6381(2) 0.0567(10) Uani 1 1 d . . . H14 H 1.1338 -0.1009 0.6693 0.068 Uiso 1 1 calc R . . C15 C 1.1423(2) -0.0975(2) 0.57839(19) 0.0533(9) Uani 1 1 d . . . H15 H 1.1520 -0.1462 0.5691 0.064 Uiso 1 1 calc R . . C16 C 1.1410(3) -0.05225(19) 0.53207(18) 0.0505(9) Uani 1 1 d . . . C17 C 1.1532(3) -0.0743(2) 0.47021(18) 0.0520(9) Uani 1 1 d . . . C18 C 1.1519(3) -0.0246(2) 0.42828(19) 0.0535(9) Uani 1 1 d . . . C19 C 1.1309(3) 0.0466(2) 0.44515(19) 0.0566(9) Uani 1 1 d . . . C20 C 1.1238(3) 0.0997(2) 0.4046(2) 0.0558(9) Uani 1 1 d . . . H20 H 1.1308 0.0876 0.3638 0.067 Uiso 1 1 calc R . . C21 C 1.1070(3) 0.1679(2) 0.4252(2) 0.0662(11) Uani 1 1 d . . . H21 H 1.1030 0.2025 0.3983 0.079 Uiso 1 1 calc R . . C22 C 1.0955(2) 0.1881(2) 0.48705(17) 0.0513(9) Uani 1 1 d . . . H22 H 1.0839 0.2354 0.5004 0.062 Uiso 1 1 calc R . . C23 C 1.1193(3) 0.06940(19) 0.50684(17) 0.0472(8) Uani 1 1 d . . . C24 C 1.1213(3) 0.01889(19) 0.54820(18) 0.0494(8) Uani 1 1 d . . . C25 C 0.8965(3) 0.4583(2) 0.54344(17) 0.0490(8) Uani 1 1 d . . . H25 H 0.9323 0.4206 0.5348 0.059 Uiso 1 1 calc R . . C26 C 0.8599(3) 0.4975(2) 0.49569(18) 0.0532(9) Uani 1 1 d . . . H26 H 0.8717 0.4851 0.4561 0.064 Uiso 1 1 calc R . . C27 C 0.8070(3) 0.5536(2) 0.50724(18) 0.0509(9) Uani 1 1 d . . . H27 H 0.7817 0.5796 0.4764 0.061 Uiso 1 1 calc R . . C28 C 0.7931(3) 0.5698(2) 0.57021(18) 0.0562(10) Uani 1 1 d . . . C29 C 0.7424(3) 0.6317(2) 0.58923(18) 0.0517(9) Uani 1 1 d . . . C30 C 0.7249(3) 0.6415(2) 0.64839(19) 0.0523(9) Uani 1 1 d . . . C31 C 0.7592(3) 0.5984(2) 0.69301(18) 0.0575(10) Uani 1 1 d . . . C32 C 0.7425(3) 0.6048(2) 0.75270(18) 0.0568(9) Uani 1 1 d . . . H32 H 0.7069 0.6405 0.7664 0.068 Uiso 1 1 calc R . . C33 C 0.7781(3) 0.5587(2) 0.7914(2) 0.0617(10) Uani 1 1 d . . . H33 H 0.7645 0.5609 0.8310 0.074 Uiso 1 1 calc R . . C34 C 0.8350(3) 0.5085(2) 0.77079(19) 0.0554(9) Uani 1 1 d . . . H34 H 0.8615 0.4788 0.7983 0.066 Uiso 1 1 calc R . . C35 C 0.8146(3) 0.5425(2) 0.6742(2) 0.0613(10) Uani 1 1 d . . . C36 C 0.8288(3) 0.5299(2) 0.6133(2) 0.0601(10) Uani 1 1 d . . . C37 C 1.1348(3) 0.1902(2) 0.8118(2) 0.0667(12) Uani 1 1 d . . . C38 C 1.1962(3) 0.2113(2) 0.8660(2) 0.0559(9) Uani 1 1 d . . . H38 H 1.1734 0.2190 0.9026 0.067 Uiso 1 1 calc R . . C39 C 1.2978(3) 0.2218(2) 0.86620(19) 0.0574(10) Uani 1 1 d . . . C40 C 1.3686(3) 0.2455(2) 0.9229(2) 0.0614(10) Uani 1 1 d . . . H40 H 1.3490 0.2501 0.9608 0.074 Uiso 1 1 calc R . . C41 C 1.4692(3) 0.2619(2) 0.9204(2) 0.0658(11) Uani 1 1 d . . . H41 H 1.5149 0.2835 0.9563 0.079 Uiso 1 1 calc R . . C42 C 1.4986(3) 0.2468(2) 0.86757(19) 0.0575(10) Uani 1 1 d . . . H42 H 1.5654 0.2543 0.8676 0.069 Uiso 1 1 calc R . . C43 C 1.4325(3) 0.2202(2) 0.81251(18) 0.0567(10) Uani 1 1 d . . . H43 H 1.4554 0.2084 0.7763 0.068 Uiso 1 1 calc R . . C44 C 1.3322(3) 0.2108(2) 0.8104(2) 0.0640(11) Uani 1 1 d . . . C45 C 1.2639(3) 0.1862(2) 0.7525(2) 0.0569(10) Uani 1 1 d . . . H45 H 1.2855 0.1761 0.7156 0.068 Uiso 1 1 calc R . . C46 C 1.1633(3) 0.1776(2) 0.75326(19) 0.0552(9) Uani 1 1 d . . . C47 C 1.0067(3) 0.1623(2) 0.7325(2) 0.0602(10) Uani 1 1 d . . . H47 H 0.9423 0.1547 0.7100 0.072 Uiso 1 1 calc R . . C48 C 1.1570(3) 0.31400(19) 0.63215(16) 0.0463(8) Uani 1 1 d . . . C49 C 1.2523(3) 0.3147(2) 0.6342(2) 0.0603(10) Uani 1 1 d . . . H49 H 1.2761 0.2704 0.6267 0.072 Uiso 1 1 calc R . . C50 C 1.3181(3) 0.3817(2) 0.6477(2) 0.0628(11) Uani 1 1 d . . . C51 C 1.4210(3) 0.3837(2) 0.65046(18) 0.0528(9) Uani 1 1 d . . . H51 H 1.4456 0.3401 0.6414 0.063 Uiso 1 1 calc R . . C52 C 1.4813(3) 0.4462(2) 0.66550(17) 0.0546(9) Uani 1 1 d . . . H52 H 1.5480 0.4461 0.6669 0.065 Uiso 1 1 calc R . . C53 C 1.4475(3) 0.5136(2) 0.6797(2) 0.0592(10) Uani 1 1 d . . . H53 H 1.4916 0.5574 0.6904 0.071 Uiso 1 1 calc R . . C54 C 1.3521(3) 0.5144(2) 0.6776(2) 0.0674(11) Uani 1 1 d . . . H54 H 1.3304 0.5589 0.6880 0.081 Uiso 1 1 calc R . . C55 C 1.2830(3) 0.4487(2) 0.66005(19) 0.0591(10) Uani 1 1 d . . . C56 C 1.1772(3) 0.4490(2) 0.65691(18) 0.0542(9) Uani 1 1 d . . . H56 H 1.1518 0.4926 0.6640 0.065 Uiso 1 1 calc R . . C57 C 1.1193(3) 0.3831(2) 0.64331(17) 0.0501(9) Uani 1 1 d . . . C58 C 0.9978(3) 0.2926(2) 0.6249(2) 0.0608(10) Uani 1 1 d . . . H58 H 0.9345 0.2671 0.6196 0.073 Uiso 1 1 calc R . . C59 C 1.0573(3) 0.4175(2) 0.80589(19) 0.0582(10) Uani 1 1 d . . . C60 C 1.1305(3) 0.4815(2) 0.8175(2) 0.0602(10) Uani 1 1 d . . . H60 H 1.1312 0.5150 0.7897 0.072 Uiso 1 1 calc R . . C61 C 1.2012(3) 0.4912(2) 0.87282(17) 0.0504(9) Uani 1 1 d . . . C62 C 1.2779(3) 0.5495(2) 0.88440(19) 0.0580(10) Uani 1 1 d . . . H62 H 1.2798 0.5826 0.8564 0.070 Uiso 1 1 calc R . . C63 C 1.3516(3) 0.5590(2) 0.9370(2) 0.0594(11) Uani 1 1 d . . . H63 H 1.4031 0.5980 0.9440 0.071 Uiso 1 1 calc R . . C64 C 1.3483(3) 0.5102(2) 0.9793(2) 0.0696(12) Uani 1 1 d . . . H64 H 1.3972 0.5169 1.0151 0.084 Uiso 1 1 calc R . . C65 C 1.2731(3) 0.4519(2) 0.9685(2) 0.0604(10) Uani 1 1 d . . . H65 H 1.2715 0.4192 0.9969 0.072 Uiso 1 1 calc R . . C66 C 1.1991(3) 0.4415(2) 0.91508(19) 0.0545(9) Uani 1 1 d . . . C67 C 1.1232(3) 0.3788(2) 0.90279(18) 0.0584(10) Uani 1 1 d . . . H67 H 1.1204 0.3456 0.9307 0.070 Uiso 1 1 calc R . . C68 C 1.0549(3) 0.3696(2) 0.84854(19) 0.0597(10) Uani 1 1 d . . . C69 C 0.9337(3) 0.3283(2) 0.7718(2) 0.0597(10) Uani 1 1 d . . . H69 H 0.8786 0.2988 0.7462 0.072 Uiso 1 1 calc R . . C70 C 0.5610(3) 0.1126(2) 1.00937(19) 0.0579(10) Uani 1 1 d . . . H70A H 0.5629 0.0602 1.0074 0.070 Uiso 1 1 calc R . . H70B H 0.5459 0.1230 0.9672 0.070 Uiso 1 1 calc R . . C71 C 0.4832(3) 0.1333(2) 1.04260(19) 0.0587(10) Uani 1 1 d . . . H71A H 0.4998 0.1836 1.0644 0.070 Uiso 1 1 calc R . . H71B H 0.4199 0.1276 1.0143 0.070 Uiso 1 1 calc R . . C72 C 0.4148(3) 0.0941(2) 1.12250(16) 0.0516(9) Uani 1 1 d . . . H72A H 0.3477 0.0838 1.0986 0.062 Uiso 1 1 calc R . . H72B H 0.4275 0.1441 1.1450 0.062 Uiso 1 1 calc R . . C73 C 0.4347(3) 0.0389(2) 1.16528(19) 0.0548(9) Uani 1 1 d . . . H73A H 0.3946 0.0433 1.1963 0.066 Uiso 1 1 calc R . . H73B H 0.4172 -0.0105 1.1418 0.066 Uiso 1 1 calc R . . C74 C 0.5963(3) 0.0146(3) 1.1540(2) 0.0692(11) Uani 1 1 d . . . H74A H 0.5581 -0.0294 1.1276 0.083 Uiso 1 1 calc R . . H74B H 0.6212 0.0480 1.1284 0.083 Uiso 1 1 calc R . . C75 C 0.6773(3) -0.0040(2) 1.2005(2) 0.0589(10) Uani 1 1 d . . . H75A H 0.6740 0.0158 1.2426 0.071 Uiso 1 1 calc R . . H75B H 0.6769 -0.0568 1.1970 0.071 Uiso 1 1 calc R . . C76 C 0.7906(3) -0.0159(2) 1.1356(2) 0.0662(11) Uani 1 1 d . . . H76A H 0.7384 -0.0567 1.1173 0.079 Uiso 1 1 calc R . . H76B H 0.8497 -0.0352 1.1522 0.079 Uiso 1 1 calc R . . C77 C 0.8086(4) 0.0332(3) 1.0897(2) 0.0734(13) Uani 1 1 d . . . H77A H 0.8113 0.0836 1.1094 0.088 Uiso 1 1 calc R . . H77B H 0.8732 0.0287 1.0812 0.088 Uiso 1 1 calc R . . C78 C 1.2675(3) -0.1585(2) 0.4653(2) 0.0683(12) Uani 1 1 d . . . H78A H 1.3002 -0.1320 0.5060 0.082 Uiso 1 1 calc R . . H78B H 1.3016 -0.1397 0.4350 0.082 Uiso 1 1 calc R . . C79 C 1.2739(3) -0.2392(2) 0.4635(2) 0.0594(10) Uani 1 1 d . . . H79A H 1.3416 -0.2454 0.4786 0.071 Uiso 1 1 calc R . . H79B H 1.2345 -0.2593 0.4907 0.071 Uiso 1 1 calc R . . C80 C 1.3065(3) -0.3141(2) 0.37575(19) 0.0566(9) Uani 1 1 d . . . H80A H 1.2741 -0.3635 0.3571 0.068 Uiso 1 1 calc R . . H80B H 1.3614 -0.3187 0.4081 0.068 Uiso 1 1 calc R . . C81 C 1.3468(3) -0.2768(2) 0.32588(19) 0.0562(9) Uani 1 1 d . . . H81A H 1.3955 -0.2345 0.3463 0.067 Uiso 1 1 calc R . . H81B H 1.3800 -0.3112 0.3037 0.067 Uiso 1 1 calc R . . C82 C 1.3148(3) -0.2133(2) 0.24170(17) 0.0540(9) Uani 1 1 d . . . H82A H 1.2729 -0.2282 0.2007 0.065 Uiso 1 1 calc R . . H82B H 1.3794 -0.2256 0.2393 0.065 Uiso 1 1 calc R . . C83 C 1.3237(3) -0.12951(19) 0.25929(18) 0.0482(8) Uani 1 1 d . . . H83A H 1.3666 -0.1138 0.2999 0.058 Uiso 1 1 calc R . . H83B H 1.3530 -0.1054 0.2294 0.058 Uiso 1 1 calc R . . C84 C 1.2410(3) -0.0329(2) 0.28677(19) 0.0584(10) Uani 1 1 d . . . H84A H 1.1820 -0.0138 0.2699 0.070 Uiso 1 1 calc R . . H84B H 1.2958 -0.0055 0.2744 0.070 Uiso 1 1 calc R . . C85 C 1.2571(3) -0.0199(2) 0.3556(2) 0.0593(10) Uani 1 1 d . . . H85A H 1.3073 -0.0471 0.3737 0.071 Uiso 1 1 calc R . . H85B H 1.2771 0.0321 0.3719 0.071 Uiso 1 1 calc R . . C86 C 0.6129(3) 0.6837(2) 0.5247(2) 0.0562(10) Uani 1 1 d . . . H86A H 0.6049 0.6991 0.4842 0.067 Uiso 1 1 calc R . . H86B H 0.6005 0.7237 0.5536 0.067 Uiso 1 1 calc R . . C87 C 0.5382(3) 0.6196(2) 0.5212(2) 0.0624(11) Uani 1 1 d . . . H87A H 0.5513 0.5785 0.4937 0.075 Uiso 1 1 calc R . . H87B H 0.5424 0.6056 0.5621 0.075 Uiso 1 1 calc R . . C88 C 0.3793(3) 0.6211(2) 0.5430(2) 0.0677(12) Uani 1 1 d . . . H88A H 0.3872 0.5741 0.5566 0.081 Uiso 1 1 calc R . . H88B H 0.3106 0.6199 0.5244 0.081 Uiso 1 1 calc R . . C89 C 0.4124(3) 0.6845(2) 0.59926(19) 0.0586(10) Uani 1 1 d . . . H89A H 0.3661 0.6789 0.6264 0.070 Uiso 1 1 calc R . . H89B H 0.4756 0.6772 0.6221 0.070 Uiso 1 1 calc R . . C90 C 0.4324(3) 0.8210(2) 0.6338(2) 0.0674(11) Uani 1 1 d . . . H90A H 0.4268 0.8060 0.6734 0.081 Uiso 1 1 calc R . . H90B H 0.3801 0.8494 0.6220 0.081 Uiso 1 1 calc R . . C91 C 0.5305(3) 0.8688(2) 0.64077(19) 0.0558(10) Uani 1 1 d . . . H91A H 0.5306 0.8877 0.6020 0.067 Uiso 1 1 calc R . . H91B H 0.5331 0.9109 0.6724 0.067 Uiso 1 1 calc R . . C92 C 0.6631(3) 0.8192(2) 0.71269(18) 0.0554(9) Uani 1 1 d . . . H92A H 0.6131 0.7964 0.7321 0.066 Uiso 1 1 calc R . . H92B H 0.7014 0.8615 0.7412 0.066 Uiso 1 1 calc R . . C93 C 0.7290(3) 0.7640(2) 0.69366(18) 0.0570(10) Uani 1 1 d . . . H93A H 0.7640 0.7821 0.6635 0.068 Uiso 1 1 calc R . . H93B H 0.7770 0.7584 0.7297 0.068 Uiso 1 1 calc R . . C94 C 0.9475(3) 0.53500(19) 0.9274(2) 0.0561(9) Uani 1 1 d . . . C95 C 1.0228(3) 0.5968(2) 0.9316(2) 0.0599(10) Uani 1 1 d . . . H95A H 1.0632 0.5852 0.9023 0.090 Uiso 1 1 calc R . . H95B H 1.0625 0.6074 0.9728 0.090 Uiso 1 1 calc R . . H95C H 0.9928 0.6390 0.9223 0.090 Uiso 1 1 calc R . . C96 C 0.5373(3) 0.4136(2) 0.8290(2) 0.0598(10) Uani 1 1 d . . . C97 C 0.4296(3) 0.4133(2) 0.8254(2) 0.0616(10) Uani 1 1 d . . . H97A H 0.3968 0.4098 0.7828 0.092 Uiso 1 1 calc R . . H97B H 0.4196 0.4582 0.8488 0.092 Uiso 1 1 calc R . . H97C H 0.4033 0.3719 0.8424 0.092 Uiso 1 1 calc R . . C98 C 1.0029(3) 0.1327(2) 0.2287(2) 0.0604(10) Uani 1 1 d . . . C99 C 0.9804(3) 0.2020(2) 0.20593(18) 0.0595(10) Uani 1 1 d . . . H99A H 1.0300 0.2196 0.1846 0.089 Uiso 1 1 calc R . . H99B H 0.9791 0.2386 0.2405 0.089 Uiso 1 1 calc R . . H99C H 0.9174 0.1927 0.1779 0.089 Uiso 1 1 calc R . . C100 C 0.4096(3) 0.3477(2) 0.1412(2) 0.0704(12) Uani 1 1 d . . . H10A H 0.4350 0.3533 0.1045 0.106 Uiso 1 1 calc R . . H10B H 0.3972 0.3946 0.1595 0.106 Uiso 1 1 calc R . . H10C H 0.3494 0.3135 0.1303 0.106 Uiso 1 1 calc R . . C101 C 0.4861(3) 0.3181(2) 0.18855(19) 0.0598(11) Uani 1 1 d . . . H10D H 0.5054 0.3550 0.2257 0.072 Uiso 1 1 calc R . . H10E H 0.4527 0.2745 0.2001 0.072 Uiso 1 1 calc R . . C102 C 0.6402(3) 0.2616(2) 0.20984(18) 0.0530(9) Uani 1 1 d . . . H10F H 0.6062 0.2138 0.2134 0.064 Uiso 1 1 calc R . . H10G H 0.6613 0.2902 0.2511 0.064 Uiso 1 1 calc R . . C103 C 0.7296(3) 0.2515(2) 0.18110(19) 0.0528(9) Uani 1 1 d . . . H10H H 0.7734 0.2266 0.2068 0.079 Uiso 1 1 calc R . . H10I H 0.7633 0.2989 0.1780 0.079 Uiso 1 1 calc R . . H10J H 0.7084 0.2228 0.1404 0.079 Uiso 1 1 calc R . . F1 F 0.95983(15) 0.39040(11) 0.41908(10) 0.0550(5) Uani 1 1 d . . . F2 F 1.02009(15) 0.30955(11) 0.35681(10) 0.0514(5) Uani 1 1 d . . . F3 F 0.91742(15) 0.26831(12) 0.41680(10) 0.0557(5) Uani 1 1 d . . . F4 F 0.80764(15) 0.33846(11) 0.37520(10) 0.0538(5) Uani 1 1 d . . . F5 F 0.90982(15) 0.37453(11) 0.31411(10) 0.0525(5) Uani 1 1 d . . . F6 F 0.86769(15) 0.25411(11) 0.31329(10) 0.0530(5) Uani 1 1 d . . . F7 F 0.88167(15) 0.71325(11) 0.89205(10) 0.0552(5) Uani 1 1 d . . . F8 F 0.93931(15) 0.74419(12) 0.99756(10) 0.0572(5) Uani 1 1 d . . . F9 F 0.77781(16) 0.73292(12) 0.95520(10) 0.0575(5) Uani 1 1 d . . . F10 F 0.81655(15) 0.81814(11) 0.89196(9) 0.0499(5) Uani 1 1 d . . . F11 F 0.97463(15) 0.82667(11) 0.93574(9) 0.0512(5) Uani 1 1 d . . . F12 F 0.86651(16) 0.84447(11) 0.99611(10) 0.0534(5) Uani 1 1 d . . . F13 F 0.36148(15) 0.04462(11) 0.53380(10) 0.0550(5) Uani 1 1 d . . . F14 F 0.49573(15) 0.05228(11) 0.60983(10) 0.0514(5) Uani 1 1 d . . . F15 F 0.31355(15) 0.13710(12) 0.59072(10) 0.0557(5) Uani 1 1 d . . . F16 F 0.34131(15) 0.03779(12) 0.63062(10) 0.0541(5) Uani 1 1 d . . . F17 F 0.46643(15) 0.15595(11) 0.56872(10) 0.0525(5) Uani 1 1 d . . . F18 F 0.44748(15) 0.14331(11) 0.66639(10) 0.0529(5) Uani 1 1 d . . . N1 N 0.8584(3) 0.2486(2) 0.90912(18) 0.0715(10) Uani 1 1 d . . . N2 N 0.9196(3) 0.1203(2) 0.88522(16) 0.0633(9) Uani 1 1 d . . . N3 N 1.1082(2) 0.04368(16) 0.60625(16) 0.0577(8) Uani 1 1 d . . . N4 N 1.1013(2) 0.13910(17) 0.52547(16) 0.0559(8) Uani 1 1 d . . . N5 N 0.8806(3) 0.47457(17) 0.59983(16) 0.0588(8) Uani 1 1 d . . . N6 N 0.8533(2) 0.50048(18) 0.71517(17) 0.0601(8) Uani 1 1 d . . . N7 N 0.9761(3) 0.31346(19) 0.82492(16) 0.0604(8) Uani 1 1 d . . . N8 N 1.0306(2) 0.17683(19) 0.79640(17) 0.0618(9) Uani 1 1 d . . . N9 N 1.0831(2) 0.16002(17) 0.70633(16) 0.0565(8) Uani 1 1 d . . . N10 N 1.0752(2) 0.25938(17) 0.62048(15) 0.0554(8) Uani 1 1 d . . . N11 N 1.0185(3) 0.36483(18) 0.63744(17) 0.0630(9) Uani 1 1 d . . . N12 N 0.9781(3) 0.3914(2) 0.75749(17) 0.0674(9) Uani 1 1 d . . . N13 N 0.8850(3) 0.48460(19) 0.92129(17) 0.0626(9) Uani 1 1 d . . . N14 N 0.6130(2) 0.41133(17) 0.82559(16) 0.0588(8) Uani 1 1 d . . . N15 N 1.0131(2) 0.07783(17) 0.24200(14) 0.0504(7) Uani 1 1 d . . . O1 O 0.65490(18) 0.15306(13) 1.04079(12) 0.0521(6) Uani 1 1 d . . . O2 O 0.48365(19) 0.08228(14) 1.08412(12) 0.0524(6) Uani 1 1 d . . . O3 O 0.53745(19) 0.05098(14) 1.19557(12) 0.0546(6) Uani 1 1 d . . . O4 O 0.76251(19) 0.03251(14) 1.18201(13) 0.0561(6) Uani 1 1 d . . . O5 O 0.74204(19) 0.02263(14) 1.03260(12) 0.0556(6) Uani 1 1 d . . . O6 O 1.16710(19) -0.14508(14) 0.45207(13) 0.0589(7) Uani 1 1 d . . . O7 O 1.2405(2) -0.27752(17) 0.40305(13) 0.0701(8) Uani 1 1 d . . . O8 O 1.2765(2) -0.25364(14) 0.28326(12) 0.0570(6) Uani 1 1 d . . . O9 O 1.23135(19) -0.10824(14) 0.26050(12) 0.0550(6) Uani 1 1 d . . . O10 O 1.1622(2) -0.04660(15) 0.36867(13) 0.0635(7) Uani 1 1 d . . . O11 O 0.71278(18) 0.67308(14) 0.54359(12) 0.0527(6) Uani 1 1 d . . . O12 O 0.43927(18) 0.63434(13) 0.49850(11) 0.0494(6) Uani 1 1 d . . . O13 O 0.42129(19) 0.75772(14) 0.58848(13) 0.0580(7) Uani 1 1 d . . . O14 O 0.62101(18) 0.83940(13) 0.65629(11) 0.0496(6) Uani 1 1 d . . . O15 O 0.67059(18) 0.69496(15) 0.66750(13) 0.0579(7) Uani 1 1 d . . . O16 O 0.57478(18) 0.29923(14) 0.17080(13) 0.0558(6) Uani 1 1 d . . . P1 P 0.91214(7) 0.32216(6) 0.36627(5) 0.0540(2) Uani 1 1 d . . . P2 P 0.87574(7) 0.77885(5) 0.94349(5) 0.0497(2) Uani 1 1 d . . . P3 P 0.40537(8) 0.09517(6) 0.59867(5) 0.0540(2) Uani 1 1 d . . . Pd1 Pd 0.94738(3) 0.21573(2) 0.852994(16) 0.06387(9) Uani 1 1 d . . . Pd2 Pd 1.08775(2) 0.151453(15) 0.615579(14) 0.04952(8) Uani 1 1 d . . . Pd3 Pd 0.93428(2) 0.431116(17) 0.677266(15) 0.05735(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 0.054(2) 0.062(2) 0.055(2) 0.0214(18) 0.0057(18) 0.0195(18) C2 0.068(3) 0.049(2) 0.064(3) 0.0135(19) 0.018(2) 0.0017(19) C3 0.054(2) 0.067(2) 0.054(2) 0.0291(19) 0.0203(18) 0.0237(19) C4 0.0371(18) 0.058(2) 0.058(2) 0.0052(17) 0.0057(16) 0.0067(16) C5 0.0451(19) 0.054(2) 0.048(2) 0.0058(16) 0.0016(16) 0.0122(16) C6 0.0333(16) 0.0479(19) 0.054(2) 0.0171(16) 0.0117(15) 0.0080(14) C7 0.050(2) 0.059(2) 0.045(2) 0.0136(17) 0.0139(16) 0.0143(17) C8 0.062(2) 0.050(2) 0.062(2) 0.0116(18) 0.025(2) 0.0040(18) C9 0.053(2) 0.064(2) 0.063(2) 0.017(2) 0.0254(19) 0.0132(18) C10 0.0450(19) 0.070(2) 0.047(2) 0.0286(18) 0.0106(16) 0.0163(17) C11 0.046(2) 0.068(3) 0.066(3) 0.021(2) 0.0135(18) 0.0151(18) C12 0.052(2) 0.061(2) 0.048(2) 0.0059(17) 0.0074(17) 0.0094(18) C13 0.053(2) 0.048(2) 0.082(3) 0.0100(19) 0.006(2) 0.0242(17) C14 0.052(2) 0.0434(19) 0.078(3) 0.0073(18) 0.0184(19) 0.0136(16) C15 0.0328(17) 0.052(2) 0.071(3) 0.0034(19) 0.0041(17) 0.0081(15) C16 0.048(2) 0.0393(18) 0.062(2) 0.0035(16) 0.0053(17) 0.0123(15) C17 0.0421(19) 0.0450(19) 0.062(2) -0.0166(17) 0.0062(17) 0.0122(15) C18 0.055(2) 0.047(2) 0.060(2) -0.0083(17) 0.0240(18) 0.0112(16) C19 0.052(2) 0.058(2) 0.058(2) -0.0053(18) 0.0129(18) 0.0125(18) C20 0.052(2) 0.054(2) 0.067(3) 0.0069(19) 0.0170(19) 0.0240(17) C21 0.077(3) 0.057(2) 0.063(3) 0.007(2) 0.006(2) 0.017(2) C22 0.0384(18) 0.049(2) 0.055(2) -0.0020(16) -0.0083(16) 0.0003(15) C23 0.0454(19) 0.0441(18) 0.054(2) 0.0030(16) 0.0177(16) 0.0069(15) C24 0.0425(19) 0.0481(19) 0.059(2) 0.0064(17) 0.0071(16) 0.0198(15) C25 0.0393(18) 0.053(2) 0.053(2) 0.0085(17) 0.0024(16) 0.0097(15) C26 0.0433(19) 0.066(2) 0.051(2) 0.0071(18) 0.0092(16) 0.0124(17) C27 0.0405(18) 0.058(2) 0.059(2) 0.0093(17) 0.0159(16) 0.0166(16) C28 0.051(2) 0.076(3) 0.054(2) 0.024(2) 0.0206(18) 0.0294(19) C29 0.052(2) 0.058(2) 0.048(2) 0.0094(17) 0.0076(17) 0.0227(17) C30 0.0429(19) 0.061(2) 0.066(2) 0.0256(19) 0.0211(17) 0.0281(17) C31 0.064(2) 0.072(3) 0.045(2) 0.0190(18) 0.0139(18) 0.027(2) C32 0.071(3) 0.051(2) 0.054(2) 0.0135(17) 0.0128(19) 0.0243(19) C33 0.064(2) 0.069(3) 0.060(3) 0.024(2) 0.009(2) 0.030(2) C34 0.049(2) 0.061(2) 0.061(2) 0.0130(19) 0.0097(18) 0.0258(18) C35 0.056(2) 0.061(2) 0.078(3) 0.033(2) 0.021(2) 0.0170(19) C36 0.073(3) 0.052(2) 0.061(3) 0.0164(19) 0.017(2) 0.0177(19) C37 0.046(2) 0.070(3) 0.075(3) -0.017(2) 0.013(2) 0.0031(19) C38 0.054(2) 0.054(2) 0.065(3) 0.0238(19) 0.0134(19) 0.0109(17) C39 0.046(2) 0.060(2) 0.062(2) 0.0076(19) 0.0006(18) 0.0079(17) C40 0.066(3) 0.051(2) 0.065(3) 0.0131(19) 0.007(2) 0.0105(19) C41 0.071(3) 0.060(2) 0.057(3) -0.0056(19) -0.007(2) 0.022(2) C42 0.054(2) 0.054(2) 0.062(3) 0.0034(19) 0.0058(19) 0.0121(18) C43 0.070(3) 0.054(2) 0.050(2) 0.0026(17) 0.0163(19) 0.0259(19) C44 0.068(3) 0.060(2) 0.067(3) 0.014(2) 0.009(2) 0.026(2) C45 0.056(2) 0.055(2) 0.066(3) 0.0265(19) 0.0117(19) 0.0156(18) C46 0.050(2) 0.062(2) 0.057(2) 0.0156(19) 0.0108(18) 0.0161(18) C47 0.058(2) 0.058(2) 0.067(3) 0.016(2) 0.018(2) 0.0017(18) C48 0.059(2) 0.0457(19) 0.0412(19) 0.0127(15) 0.0167(16) 0.0180(16) C49 0.054(2) 0.054(2) 0.068(3) 0.0064(19) -0.0022(19) 0.0153(18) C50 0.059(2) 0.051(2) 0.082(3) 0.013(2) 0.017(2) 0.0128(18) C51 0.051(2) 0.046(2) 0.059(2) 0.0161(17) 0.0046(17) 0.0040(16) C52 0.066(2) 0.054(2) 0.050(2) 0.0169(17) 0.0283(19) -0.0017(18) C53 0.065(3) 0.050(2) 0.071(3) 0.0173(19) 0.038(2) -0.0063(18) C54 0.068(3) 0.063(3) 0.066(3) -0.002(2) 0.009(2) 0.010(2) C55 0.065(2) 0.065(2) 0.049(2) 0.0117(19) 0.0109(19) 0.016(2) C56 0.070(2) 0.0438(19) 0.057(2) 0.0166(17) 0.0235(19) 0.0147(18) C57 0.061(2) 0.052(2) 0.0406(19) 0.0135(16) 0.0079(16) 0.0199(18) C58 0.056(2) 0.058(2) 0.075(3) 0.036(2) 0.010(2) 0.0154(18) C59 0.055(2) 0.062(2) 0.060(2) 0.015(2) 0.0139(19) 0.0141(19) C60 0.053(2) 0.064(2) 0.065(3) 0.008(2) 0.0115(19) 0.0147(19) C61 0.047(2) 0.059(2) 0.048(2) 0.0050(17) 0.0173(16) 0.0077(16) C62 0.059(2) 0.055(2) 0.055(2) -0.0168(18) 0.0218(19) 0.0061(18) C63 0.054(2) 0.050(2) 0.067(3) -0.0235(19) 0.020(2) 0.0030(17) C64 0.070(3) 0.052(2) 0.078(3) -0.011(2) 0.003(2) 0.016(2) C65 0.055(2) 0.063(2) 0.064(3) 0.009(2) 0.0105(19) 0.0180(19) C66 0.063(2) 0.0429(19) 0.058(2) -0.0013(17) 0.0177(19) 0.0122(17) C67 0.062(2) 0.065(2) 0.046(2) 0.0048(18) 0.0075(18) 0.0099(19) C68 0.047(2) 0.078(3) 0.058(2) 0.017(2) 0.0160(18) 0.0085(19) C69 0.059(2) 0.062(2) 0.069(3) 0.020(2) 0.027(2) 0.0203(19) C70 0.060(2) 0.055(2) 0.060(2) 0.0161(19) 0.0154(19) 0.0025(18) C71 0.056(2) 0.060(2) 0.061(2) 0.0195(19) 0.0075(19) 0.0096(18) C72 0.0430(19) 0.072(2) 0.0383(19) 0.0090(17) 0.0077(15) 0.0050(17) C73 0.0410(19) 0.068(2) 0.067(2) 0.025(2) 0.0235(18) 0.0179(17) C74 0.072(3) 0.074(3) 0.068(3) 0.020(2) 0.016(2) 0.022(2) C75 0.057(2) 0.064(2) 0.064(3) 0.020(2) 0.0195(19) 0.0210(19) C76 0.068(3) 0.070(3) 0.064(3) 0.018(2) 0.015(2) 0.013(2) C77 0.092(3) 0.066(3) 0.053(3) 0.017(2) -0.005(2) 0.000(2) C78 0.060(2) 0.051(2) 0.080(3) -0.009(2) -0.014(2) 0.0199(19) C79 0.059(2) 0.045(2) 0.069(3) 0.0003(18) 0.005(2) 0.0102(17) C80 0.057(2) 0.055(2) 0.060(2) 0.0140(18) 0.0083(19) 0.0164(18) C81 0.062(2) 0.0429(19) 0.068(3) 0.0211(18) 0.0127(19) 0.0160(17) C82 0.059(2) 0.054(2) 0.041(2) -0.0089(16) 0.0028(17) 0.0061(17) C83 0.0435(19) 0.0460(19) 0.061(2) 0.0170(17) 0.0212(17) 0.0066(15) C84 0.043(2) 0.062(2) 0.061(2) -0.0088(19) 0.0006(17) 0.0080(17) C85 0.065(2) 0.048(2) 0.066(3) -0.0047(18) 0.019(2) 0.0210(18) C86 0.066(2) 0.050(2) 0.066(3) 0.0300(19) 0.023(2) 0.0240(18) C87 0.062(2) 0.048(2) 0.068(3) 0.0236(19) -0.015(2) 0.0063(18) C88 0.069(3) 0.055(2) 0.070(3) 0.017(2) 0.013(2) -0.029(2) C89 0.061(2) 0.064(2) 0.055(2) 0.0175(19) 0.0256(19) -0.0056(19) C90 0.058(2) 0.058(2) 0.091(3) 0.013(2) 0.019(2) 0.020(2) C91 0.050(2) 0.0466(19) 0.061(2) -0.0219(17) -0.0012(17) 0.0227(16) C92 0.057(2) 0.063(2) 0.055(2) 0.0146(19) 0.0253(18) 0.0208(18) C93 0.059(2) 0.064(2) 0.049(2) 0.0043(18) 0.0074(18) 0.0245(19) C94 0.061(2) 0.0399(19) 0.067(3) 0.0021(17) 0.0132(19) 0.0108(17) C95 0.057(2) 0.046(2) 0.067(3) -0.0193(18) 0.0030(19) 0.0144(17) C96 0.056(2) 0.060(2) 0.065(3) 0.016(2) 0.0121(19) 0.0096(19) C97 0.069(3) 0.054(2) 0.059(2) -0.0041(19) 0.014(2) 0.0118(19) C98 0.051(2) 0.062(2) 0.070(3) 0.011(2) 0.023(2) -0.0010(18) C99 0.056(2) 0.065(2) 0.051(2) -0.0128(19) 0.0114(18) 0.0038(19) C100 0.054(2) 0.055(2) 0.085(3) 0.009(2) -0.011(2) -0.0161(19) C101 0.050(2) 0.052(2) 0.062(2) -0.0173(18) -0.0148(18) 0.0141(17) C102 0.056(2) 0.053(2) 0.054(2) 0.0127(17) 0.0145(18) 0.0192(18) C103 0.054(2) 0.0429(19) 0.062(2) -0.0062(16) 0.0153(18) 0.0158(16) F1 0.0480(12) 0.0565(12) 0.0618(13) 0.0114(10) 0.0112(10) 0.0110(9) F2 0.0525(12) 0.0452(11) 0.0555(12) -0.0045(9) 0.0140(10) 0.0122(9) F3 0.0552(12) 0.0630(13) 0.0539(12) 0.0151(10) 0.0148(10) 0.0173(10) F4 0.0528(12) 0.0530(12) 0.0542(13) -0.0065(10) 0.0164(10) 0.0106(9) F5 0.0580(12) 0.0495(11) 0.0550(12) 0.0133(9) 0.0146(10) 0.0176(9) F6 0.0554(12) 0.0513(11) 0.0564(13) 0.0095(9) 0.0162(10) 0.0166(9) F7 0.0484(11) 0.0517(12) 0.0641(14) 0.0003(10) 0.0116(10) 0.0116(9) F8 0.0529(12) 0.0588(13) 0.0581(13) 0.0186(10) -0.0002(10) 0.0097(10) F9 0.0545(12) 0.0628(13) 0.0580(13) 0.0138(10) 0.0146(10) 0.0100(10) F10 0.0536(12) 0.0517(11) 0.0479(12) 0.0138(9) 0.0139(9) 0.0101(9) F11 0.0530(12) 0.0572(12) 0.0469(11) 0.0139(9) 0.0146(9) 0.0101(9) F12 0.0607(12) 0.0493(11) 0.0515(12) 0.0121(9) 0.0114(10) 0.0096(9) F13 0.0480(11) 0.0566(12) 0.0616(13) 0.0114(10) 0.0111(10) 0.0110(9) F14 0.0525(11) 0.0453(11) 0.0555(12) -0.0045(9) 0.0141(9) 0.0123(9) F15 0.0551(12) 0.0630(13) 0.0540(13) 0.0149(10) 0.0148(10) 0.0173(10) F16 0.0505(12) 0.0594(12) 0.0538(12) 0.0115(10) 0.0112(10) 0.0110(10) F17 0.0580(12) 0.0495(11) 0.0550(13) 0.0133(9) 0.0147(10) 0.0176(9) F18 0.0554(12) 0.0513(11) 0.0562(13) 0.0094(10) 0.0162(10) 0.0166(9) N1 0.080(3) 0.066(2) 0.074(2) 0.0156(19) 0.021(2) 0.0166(19) N2 0.071(2) 0.068(2) 0.053(2) 0.0142(17) 0.0162(17) 0.0122(17) N3 0.062(2) 0.0426(17) 0.070(2) 0.0046(15) 0.0173(17) 0.0133(14) N4 0.0609(19) 0.0458(17) 0.061(2) 0.0034(15) 0.0119(16) 0.0150(15) N5 0.071(2) 0.0461(17) 0.061(2) 0.0112(15) 0.0131(17) 0.0152(15) N6 0.0510(18) 0.063(2) 0.068(2) 0.0177(17) 0.0129(16) 0.0057(15) N7 0.063(2) 0.061(2) 0.060(2) 0.0135(16) 0.0132(16) 0.0120(16) N8 0.0554(19) 0.064(2) 0.066(2) 0.0162(17) 0.0116(17) 0.0045(16) N9 0.0593(19) 0.0502(18) 0.062(2) 0.0048(15) 0.0169(16) 0.0148(15) N10 0.0603(19) 0.0523(18) 0.0557(19) 0.0027(14) 0.0169(15) 0.0149(15) N11 0.063(2) 0.0566(19) 0.071(2) 0.0155(17) 0.0124(17) 0.0144(16) N12 0.075(2) 0.064(2) 0.065(2) 0.0176(17) 0.0095(18) 0.0153(18) N13 0.064(2) 0.062(2) 0.066(2) 0.0189(17) 0.0167(17) 0.0108(16) N14 0.0508(18) 0.0530(18) 0.068(2) 0.0145(16) 0.0158(16) -0.0212(14) N15 0.0477(17) 0.0613(19) 0.0503(18) 0.0148(15) 0.0184(14) 0.0197(14) O1 0.0507(14) 0.0503(14) 0.0565(15) 0.0086(12) 0.0100(12) 0.0144(11) O2 0.0618(16) 0.0527(14) 0.0472(14) 0.0116(11) 0.0176(12) 0.0123(12) O3 0.0581(15) 0.0543(14) 0.0564(16) 0.0174(12) 0.0142(12) 0.0151(12) O4 0.0566(15) 0.0485(14) 0.0670(17) 0.0172(12) 0.0125(13) 0.0148(12) O5 0.0596(16) 0.0546(15) 0.0568(16) 0.0160(12) 0.0142(13) 0.0145(12) O6 0.0566(15) 0.0569(15) 0.0616(17) -0.0092(13) 0.0155(13) 0.0180(12) O7 0.0703(19) 0.080(2) 0.0546(17) -0.0087(14) 0.0111(14) 0.0157(15) O8 0.0679(17) 0.0488(14) 0.0550(16) 0.0114(12) 0.0096(13) 0.0126(12) O9 0.0513(14) 0.0628(16) 0.0506(15) -0.0014(12) 0.0137(12) 0.0132(12) O10 0.0659(17) 0.0554(16) 0.0632(18) -0.0109(13) 0.0129(14) 0.0087(13) O11 0.0507(14) 0.0611(15) 0.0543(16) 0.0196(12) 0.0175(12) 0.0179(12) O12 0.0532(14) 0.0488(13) 0.0527(15) 0.0169(11) 0.0156(12) 0.0153(11) O13 0.0542(15) 0.0565(15) 0.0604(16) 0.0105(13) 0.0174(13) -0.0123(12) O14 0.0499(14) 0.0546(14) 0.0507(15) 0.0159(12) 0.0155(11) 0.0174(11) O15 0.0419(13) 0.0722(17) 0.0636(17) 0.0083(14) 0.0172(12) 0.0170(12) O16 0.0493(14) 0.0551(15) 0.0607(16) -0.0132(12) 0.0212(12) 0.0071(12) P1 0.0504(5) 0.0593(6) 0.0536(6) 0.0115(5) 0.0111(4) 0.0109(4) P2 0.0537(5) 0.0518(5) 0.0476(5) 0.0138(4) 0.0145(4) 0.0101(4) P3 0.0504(5) 0.0593(6) 0.0537(6) 0.0114(5) 0.0111(4) 0.0110(4) Pd1 0.0626(2) 0.0706(2) 0.0599(2) 0.01338(16) 0.01311(15) 0.01205(16) Pd2 0.04926(16) 0.04519(15) 0.05699(18) 0.00270(12) 0.01688(13) 0.01493(12) Pd3 0.06472(19) 0.05227(17) 0.05775(19) 0.01589(14) 0.01170(15) 0.01331(14) _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 1.319(4) . ? C1 C2 1.393(6) . ? C1 H1 0.9300 . ? C2 C3 1.333(5) . ? C2 H2 0.9300 . ? C3 C4 1.404(5) . ? C3 H3 0.9300 . ? C4 C5 1.392(5) . ? C4 C12 1.393(5) . ? C5 O1 1.381(4) . ? C5 C6 1.395(5) . ? C6 C7 1.396(5) . ? C6 O5 1.397(3) . ? C7 C11 1.389(5) . ? C7 C8 1.438(5) . ? C8 C9 1.372(5) . ? C8 H8 0.9300 . ? C9 C10 1.413(5) . ? C9 H9 0.9300 . ? C10 N2 1.274(4) . ? C10 H10 0.9300 . ? C11 C12 1.393(6) . ? C11 N2 1.402(4) . ? C12 N1 1.365(4) . ? C13 N3 1.312(4) . ? C13 C14 1.371(5) . ? C13 H13 0.9300 . ? C14 C15 1.401(6) . ? C14 H14 0.9300 . ? C15 C16 1.407(5) . ? C15 H15 0.9300 . ? C16 C24 1.394(5) . ? C16 C17 1.429(5) . ? C17 O6 1.367(3) . ? C17 C18 1.391(6) . ? C18 O10 1.372(4) . ? C18 C19 1.405(5) . ? C19 C20 1.417(6) . ? C19 C23 1.425(5) . ? C20 C21 1.350(5) . ? C20 H20 0.9300 . ? C21 C22 1.419(6) . ? C21 H21 0.9300 . ? C22 N4 1.323(4) . ? C22 H22 0.9300 . ? C23 N4 1.371(3) . ? C23 C24 1.392(5) . ? C24 N3 1.364(4) . ? C25 N5 1.315(4) . ? C25 C26 1.413(5) . ? C25 H25 0.9300 . ? C26 C27 1.374(5) . ? C26 H26 0.9300 . ? C27 C28 1.445(5) . ? C27 H27 0.9300 . ? C28 C36 1.343(5) . ? C28 C29 1.479(5) . ? C29 C30 1.374(5) . ? C29 O11 1.381(4) . ? C30 O15 1.392(3) . ? C30 C31 1.403(5) . ? C31 C32 1.381(5) . ? C31 C35 1.435(6) . ? C32 C33 1.359(5) . ? C32 H32 0.9300 . ? C33 C34 1.386(5) . ? C33 H33 0.9300 . ? C34 N6 1.301(4) . ? C34 H34 0.9300 . ? C35 N6 1.352(4) . ? C35 C36 1.398(6) . ? C36 N5 1.361(4) . ? C37 C38 1.319(6) . ? C37 N8 1.418(4) . ? C37 C46 1.430(6) . ? C38 C39 1.412(5) . ? C38 H38 0.9300 . ? C39 C44 1.411(6) . ? C39 C40 1.427(6) . ? C40 C41 1.417(6) . ? C40 H40 0.9300 . ? C41 C42 1.322(6) . ? C41 H41 0.9300 . ? C42 C43 1.377(6) . ? C42 H42 0.9300 . ? C43 C44 1.386(6) . ? C43 H43 0.9300 . ? C44 C45 1.431(6) . ? C45 C46 1.401(5) . ? C45 H45 0.9300 . ? C46 N9 1.354(4) . ? C47 N9 1.314(4) . ? C47 N8 1.376(4) . ? C47 H47 0.9300 . ? C48 C49 1.326(5) . ? C48 N10 1.391(4) . ? C48 C57 1.453(4) . ? C49 C50 1.411(6) . ? C49 H49 0.9300 . ? C50 C55 1.404(4) . ? C50 C51 1.428(4) . ? C51 C52 1.308(5) . ? C51 H51 0.9300 . ? C52 C53 1.407(6) . ? C52 H52 0.9300 . ? C53 C54 1.331(6) . ? C53 H53 0.9300 . ? C54 C55 1.417(6) . ? C54 H54 0.9300 . ? C55 C56 1.471(6) . ? C56 C57 1.342(5) . ? C56 H56 0.9300 . ? C57 N11 1.387(4) . ? C58 N11 1.313(4) . ? C58 N10 1.325(4) . ? C58 H58 0.9300 . ? C59 N12 1.379(4) . ? C59 C68 1.380(6) . ? C59 C60 1.429(6) . ? C60 C61 1.400(6) . ? C60 H60 0.9300 . ? C61 C62 1.385(5) . ? C61 C66 1.399(5) . ? C62 C63 1.380(6) . ? C62 H62 0.9300 . ? C63 C64 1.389(6) . ? C63 H63 0.9300 . ? C64 C65 1.373(6) . ? C64 H64 0.9300 . ? C65 C66 1.394(6) . ? C65 H65 0.9300 . ? C66 C67 1.433(5) . ? C67 C68 1.366(6) . ? C67 H67 0.9300 . ? C68 N7 1.389(4) . ? C69 N7 1.296(4) . ? C69 N12 1.357(4) . ? C69 H69 0.9300 . ? C70 O1 1.432(4) . ? C70 C71 1.487(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 O2 1.402(4) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O2 1.421(4) . ? C72 C73 1.499(5) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 O3 1.445(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.489(6) . ? C74 O3 1.500(5) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 O4 1.451(4) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 O4 1.422(4) . ? C76 C77 1.486(6) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 O5 1.399(4) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 O6 1.442(4) . ? C78 C79 1.504(5) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 O7 1.399(4) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 O7 1.392(4) . ? C80 C81 1.536(5) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 O8 1.382(4) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 O8 1.401(4) . ? C82 C83 1.532(5) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 O9 1.403(3) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 O9 1.419(4) . ? C84 C85 1.484(6) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 O10 1.455(4) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 O11 1.428(4) . ? C86 C87 1.465(5) . ? C86 H86A 0.9700 . ? C86 H86B 0.9700 . ? C87 O12 1.454(4) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 O12 1.438(4) . ? C88 C89 1.554(6) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 O13 1.400(4) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 O13 1.413(4) . ? C90 C91 1.509(6) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 O14 1.442(3) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 O14 1.398(4) . ? C92 C93 1.531(5) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 O15 1.416(4) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 N13 1.173(4) . ? C94 C95 1.436(5) . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 N14 1.082(4) . ? C96 C97 1.496(6) . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 0.9600 . ? C98 N15 1.113(4) . ? C98 C99 1.486(6) . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? C100 C101 1.558(4) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 O16 1.442(5) . ? C101 H10D 0.9700 . ? C101 H10E 0.9700 . ? C102 O16 1.447(5) . ? C102 C103 1.529(5) . ? C102 H10F 0.9700 . ? C102 H10G 0.9700 . ? C103 H10H 0.9600 . ? C103 H10I 0.9600 . ? C103 H10J 0.9600 . ? F1 P1 1.589(2) . ? F2 P1 1.607(2) . ? F3 P1 1.592(2) . ? F4 P1 1.574(2) . ? F5 P1 1.602(2) . ? F6 P1 1.581(2) . ? F7 P2 1.576(2) . ? F8 P2 1.608(2) . ? F9 P2 1.605(2) . ? F10 P2 1.592(2) . ? F11 P2 1.599(2) . ? F12 P2 1.607(2) . ? F13 P3 1.581(2) . ? F14 P3 1.574(2) . ? F15 P3 1.577(2) . ? F16 P3 1.623(2) . ? F17 P3 1.615(2) . ? F18 P3 1.608(2) . ? N1 Pd1 2.013(4) . ? N2 Pd1 2.011(4) . ? N3 Pd2 2.040(3) . ? N4 Pd2 2.030(3) . ? N5 Pd3 2.047(3) . ? N6 Pd3 2.021(4) . ? N7 Pd1 2.007(3) . ? N8 Pd1 1.995(4) . ? N9 Pd2 2.013(3) . ? N10 Pd2 2.017(3) . ? N11 Pd3 2.038(4) . ? N12 Pd3 2.032(4) . ? 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 122.9(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 122.6(4) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C12 120.2(4) . . ? C5 C4 C3 125.5(4) . . ? C12 C4 C3 114.3(4) . . ? O1 C5 C4 116.9(3) . . ? O1 C5 C6 122.9(3) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C7 120.0(3) . . ? C5 C6 O5 118.6(3) . . ? C7 C6 O5 120.7(3) . . ? C11 C7 C6 119.8(3) . . ? C11 C7 C8 116.8(3) . . ? C6 C7 C8 123.4(3) . . ? C9 C8 C7 119.5(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.0(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 123.0(3) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C7 C11 C12 120.3(4) . . ? C7 C11 N2 121.7(3) . . ? C12 C11 N2 118.0(3) . . ? N1 C12 C4 124.4(3) . . ? N1 C12 C11 115.8(3) . . ? C4 C12 C11 119.8(4) . . ? N3 C13 C14 124.1(4) . . ? N3 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C15 116.0(4) . . ? C13 C14 H14 122.0 . . ? C15 C14 H14 122.0 . . ? C14 C15 C16 122.1(4) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C24 C16 C15 115.9(4) . . ? C24 C16 C17 118.4(4) . . ? C15 C16 C17 125.6(3) . . ? O6 C17 C18 119.5(3) . . ? O6 C17 C16 119.7(3) . . ? C18 C17 C16 120.8(3) . . ? O10 C18 C17 120.4(3) . . ? O10 C18 C19 119.5(4) . . ? C17 C18 C19 119.8(3) . . ? C18 C19 C20 123.6(4) . . ? C18 C19 C23 119.7(4) . . ? C20 C19 C23 116.7(3) . . ? C21 C20 C19 119.9(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 121.6(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? N4 C22 C21 119.4(3) . . ? N4 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? N4 C23 C24 119.2(3) . . ? N4 C23 C19 121.3(3) . . ? C24 C23 C19 119.5(3) . . ? N3 C24 C23 116.7(3) . . ? N3 C24 C16 121.7(3) . . ? C23 C24 C16 121.5(4) . . ? N5 C25 C26 120.9(3) . . ? N5 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 120.6(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 116.1(4) . . ? C26 C27 H27 122.0 . . ? C28 C27 H27 122.0 . . ? C36 C28 C27 120.3(4) . . ? C36 C28 C29 118.5(4) . . ? C27 C28 C29 121.1(3) . . ? C30 C29 O11 125.8(3) . . ? C30 C29 C28 118.7(3) . . ? O11 C29 C28 115.4(3) . . ? C29 C30 O15 121.5(3) . . ? C29 C30 C31 122.8(3) . . ? O15 C30 C31 115.8(3) . . ? C32 C31 C30 125.4(4) . . ? C32 C31 C35 117.8(3) . . ? C30 C31 C35 116.8(3) . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 118.8(4) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? N6 C34 C33 123.7(3) . . ? N6 C34 H34 118.1 . . ? C33 C34 H34 118.1 . . ? N6 C35 C36 118.8(3) . . ? N6 C35 C31 120.4(4) . . ? C36 C35 C31 120.8(4) . . ? C28 C36 N5 121.7(4) . . ? C28 C36 C35 122.1(4) . . ? N5 C36 C35 116.2(3) . . ? C38 C37 N8 130.9(4) . . ? C38 C37 C46 124.9(4) . . ? N8 C37 C46 104.1(3) . . ? C37 C38 C39 117.6(4) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? C44 C39 C38 121.0(4) . . ? C44 C39 C40 118.2(4) . . ? C38 C39 C40 120.8(4) . . ? C41 C40 C39 118.9(4) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C42 C41 C40 120.6(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 121.6(4) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C44 120.8(4) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C39 119.4(4) . . ? C43 C44 C45 120.4(4) . . ? C39 C44 C45 120.0(4) . . ? C46 C45 C44 117.9(4) . . ? C46 C45 H45 121.1 . . ? C44 C45 H45 121.1 . . ? N9 C46 C45 131.0(4) . . ? N9 C46 C37 110.6(3) . . ? C45 C46 C37 118.4(4) . . ? N9 C47 N8 113.9(3) . . ? N9 C47 H47 123.0 . . ? N8 C47 H47 123.0 . . ? C49 C48 N10 135.0(3) . . ? C49 C48 C57 119.8(3) . . ? N10 C48 C57 105.3(2) . . ? C48 C49 C50 120.9(4) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C55 C50 C49 119.9(3) . . ? C55 C50 C51 118.2(3) . . ? C49 C50 C51 121.9(3) . . ? C52 C51 C50 120.9(3) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 121.5(4) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.2 . . ? C54 C53 C52 119.6(4) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 121.4(4) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C50 C55 C54 118.3(4) . . ? C50 C55 C56 119.8(3) . . ? C54 C55 C56 121.9(4) . . ? C57 C56 C55 116.7(4) . . ? C57 C56 H56 121.6 . . ? C55 C56 H56 121.6 . . ? C56 C57 N11 130.8(3) . . ? C56 C57 C48 122.8(3) . . ? N11 C57 C48 106.4(2) . . ? N11 C58 N10 113.9(3) . . ? N11 C58 H58 123.1 . . ? N10 C58 H58 123.1 . . ? N12 C59 C68 106.8(3) . . ? N12 C59 C60 132.0(4) . . ? C68 C59 C60 121.2(4) . . ? C61 C60 C59 116.6(4) . . ? C61 C60 H60 121.7 . . ? C59 C60 H60 121.7 . . ? C62 C61 C66 119.2(4) . . ? C62 C61 C60 119.0(4) . . ? C66 C61 C60 121.7(4) . . ? C63 C62 C61 120.9(4) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C62 C63 C64 119.7(4) . . ? C62 C63 H63 120.2 . . ? C64 C63 H63 120.2 . . ? C65 C64 C63 120.2(4) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 120.3(4) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 119.7(4) . . ? C65 C66 C67 120.0(4) . . ? C61 C66 C67 120.3(4) . . ? C68 C67 C66 117.5(4) . . ? C68 C67 H67 121.2 . . ? C66 C67 H67 121.2 . . ? C67 C68 C59 122.7(4) . . ? C67 C68 N7 129.1(4) . . ? C59 C68 N7 108.1(3) . . ? N7 C69 N12 112.9(3) . . ? N7 C69 H69 123.6 . . ? N12 C69 H69 123.6 . . ? O1 C70 C71 110.4(3) . . ? O1 C70 H70A 109.6 . . ? C71 C70 H70A 109.6 . . ? O1 C70 H70B 109.6 . . ? C71 C70 H70B 109.6 . . ? H70A C70 H70B 108.1 . . ? O2 C71 C70 101.5(3) . . ? O2 C71 H71A 111.5 . . ? C70 C71 H71A 111.5 . . ? O2 C71 H71B 111.5 . . ? C70 C71 H71B 111.5 . . ? H71A C71 H71B 109.3 . . ? O2 C72 C73 100.8(3) . . ? O2 C72 H72A 111.6 . . ? C73 C72 H72A 111.6 . . ? O2 C72 H72B 111.6 . . ? C73 C72 H72B 111.6 . . ? H72A C72 H72B 109.4 . . ? O3 C73 C72 110.5(3) . . ? O3 C73 H73A 109.6 . . ? C72 C73 H73A 109.6 . . ? O3 C73 H73B 109.6 . . ? C72 C73 H73B 109.6 . . ? H73A C73 H73B 108.1 . . ? C75 C74 O3 101.2(3) . . ? C75 C74 H74A 111.5 . . ? O3 C74 H74A 111.5 . . ? C75 C74 H74B 111.5 . . ? O3 C74 H74B 111.5 . . ? H74A C74 H74B 109.3 . . ? O4 C75 C74 100.7(3) . . ? O4 C75 H75A 111.6 . . ? C74 C75 H75A 111.6 . . ? O4 C75 H75B 111.6 . . ? C74 C75 H75B 111.6 . . ? H75A C75 H75B 109.4 . . ? O4 C76 C77 102.2(3) . . ? O4 C76 H76A 111.3 . . ? C77 C76 H76A 111.3 . . ? O4 C76 H76B 111.3 . . ? C77 C76 H76B 111.3 . . ? H76A C76 H76B 109.2 . . ? O5 C77 C76 118.5(4) . . ? O5 C77 H77A 107.7 . . ? C76 C77 H77A 107.7 . . ? O5 C77 H77B 107.7 . . ? C76 C77 H77B 107.7 . . ? H77A C77 H77B 107.1 . . ? O6 C78 C79 112.0(3) . . ? O6 C78 H78A 109.2 . . ? C79 C78 H78A 109.2 . . ? O6 C78 H78B 109.2 . . ? C79 C78 H78B 109.2 . . ? H78A C78 H78B 107.9 . . ? O7 C79 C78 110.7(3) . . ? O7 C79 H79A 109.5 . . ? C78 C79 H79A 109.5 . . ? O7 C79 H79B 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 108.1 . . ? O7 C80 C81 115.2(3) . . ? O7 C80 H80A 108.5 . . ? C81 C80 H80A 108.5 . . ? O7 C80 H80B 108.5 . . ? C81 C80 H80B 108.5 . . ? H80A C80 H80B 107.5 . . ? O8 C81 C80 114.5(3) . . ? O8 C81 H81A 108.6 . . ? C80 C81 H81A 108.6 . . ? O8 C81 H81B 108.6 . . ? C80 C81 H81B 108.6 . . ? H81A C81 H81B 107.6 . . ? O8 C82 C83 114.2(3) . . ? O8 C82 H82A 108.7 . . ? C83 C82 H82A 108.7 . . ? O8 C82 H82B 108.7 . . ? C83 C82 H82B 108.7 . . ? H82A C82 H82B 107.6 . . ? O9 C83 C82 111.0(3) . . ? O9 C83 H83A 109.4 . . ? C82 C83 H83A 109.4 . . ? O9 C83 H83B 109.4 . . ? C82 C83 H83B 109.4 . . ? H83A C83 H83B 108.0 . . ? O9 C84 C85 113.9(3) . . ? O9 C84 H84A 108.8 . . ? C85 C84 H84A 108.8 . . ? O9 C84 H84B 108.8 . . ? C85 C84 H84B 108.8 . . ? H84A C84 H84B 107.7 . . ? O10 C85 C84 104.4(3) . . ? O10 C85 H85A 110.9 . . ? C84 C85 H85A 110.9 . . ? O10 C85 H85B 110.9 . . ? C84 C85 H85B 110.9 . . ? H85A C85 H85B 108.9 . . ? O11 C86 C87 116.1(3) . . ? O11 C86 H86A 108.3 . . ? C87 C86 H86A 108.3 . . ? O11 C86 H86B 108.3 . . ? C87 C86 H86B 108.3 . . ? H86A C86 H86B 107.4 . . ? O12 C87 C86 112.2(3) . . ? O12 C87 H87A 109.2 . . ? C86 C87 H87A 109.2 . . ? O12 C87 H87B 109.2 . . ? C86 C87 H87B 109.2 . . ? H87A C87 H87B 107.9 . . ? O12 C88 C89 108.1(3) . . ? O12 C88 H88A 110.1 . . ? C89 C88 H88A 110.1 . . ? O12 C88 H88B 110.1 . . ? C89 C88 H88B 110.1 . . ? H88A C88 H88B 108.4 . . ? O13 C89 C88 119.2(3) . . ? O13 C89 H89A 107.5 . . ? C88 C89 H89A 107.5 . . ? O13 C89 H89B 107.5 . . ? C88 C89 H89B 107.5 . . ? H89A C89 H89B 107.0 . . ? O13 C90 C91 111.6(3) . . ? O13 C90 H90A 109.3 . . ? C91 C90 H90A 109.3 . . ? O13 C90 H90B 109.3 . . ? C91 C90 H90B 109.3 . . ? H90A C90 H90B 108.0 . . ? O14 C91 C90 120.8(3) . . ? O14 C91 H91A 107.1 . . ? C90 C91 H91A 107.1 . . ? O14 C91 H91B 107.1 . . ? C90 C91 H91B 107.1 . . ? H91A C91 H91B 106.8 . . ? O14 C92 C93 103.3(3) . . ? O14 C92 H92A 111.1 . . ? C93 C92 H92A 111.1 . . ? O14 C92 H92B 111.1 . . ? C93 C92 H92B 111.1 . . ? H92A C92 H92B 109.1 . . ? O15 C93 C92 109.6(3) . . ? O15 C93 H93A 109.8 . . ? C92 C93 H93A 109.8 . . ? O15 C93 H93B 109.8 . . ? C92 C93 H93B 109.8 . . ? H93A C93 H93B 108.2 . . ? N13 C94 C95 177.0(4) . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? N14 C96 C97 173.1(4) . . ? C96 C97 H97A 109.5 . . ? C96 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N15 C98 C99 174.1(4) . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O16 C101 C100 119.2(3) . . ? O16 C101 H10D 107.5 . . ? C100 C101 H10D 107.5 . . ? O16 C101 H10E 107.5 . . ? C100 C101 H10E 107.5 . . ? H10D C101 H10E 107.0 . . ? O16 C102 C103 109.1(3) . . ? O16 C102 H10F 109.9 . . ? C103 C102 H10F 109.9 . . ? O16 C102 H10G 109.9 . . ? C103 C102 H10G 109.9 . . ? H10F C102 H10G 108.3 . . ? C102 C103 H10H 109.5 . . ? C102 C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C102 C103 H10J 109.5 . . ? H10H C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? C1 N1 C12 117.2(3) . . ? C1 N1 Pd1 129.5(2) . . ? C12 N1 Pd1 113.2(2) . . ? C10 N2 C11 119.9(3) . . ? C10 N2 Pd1 129.4(2) . . ? C11 N2 Pd1 110.7(2) . . ? C13 N3 C24 120.0(2) . . ? C13 N3 Pd2 128.4(2) . . ? C24 N3 Pd2 111.6(2) . . ? C22 N4 C23 121.2(2) . . ? C22 N4 Pd2 128.40(19) . . ? C23 N4 Pd2 110.36(19) . . ? C25 N5 C36 120.3(2) . . ? C25 N5 Pd3 127.8(2) . . ? C36 N5 Pd3 111.7(2) . . ? C34 N6 C35 119.2(3) . . ? C34 N6 Pd3 129.3(2) . . ? C35 N6 Pd3 111.5(2) . . ? C69 N7 C68 106.3(3) . . ? C69 N7 Pd1 123.4(2) . . ? C68 N7 Pd1 128.8(2) . . ? C47 N8 C37 105.2(3) . . ? C47 N8 Pd1 126.9(2) . . ? C37 N8 Pd1 122.8(2) . . ? C47 N9 C46 106.0(3) . . ? C47 N9 Pd2 128.9(2) . . ? C46 N9 Pd2 124.3(2) . . ? C58 N10 C48 107.3(2) . . ? C58 N10 Pd2 129.6(2) . . ? C48 N10 Pd2 122.0(2) . . ? C58 N11 C57 107.1(2) . . ? C58 N11 Pd3 124.3(2) . . ? C57 N11 Pd3 123.7(2) . . ? C69 N12 C59 105.9(3) . . ? C69 N12 Pd3 124.1(2) . . ? C59 N12 Pd3 129.9(2) . . ? C5 O1 C70 112.92(17) . . ? C71 O2 C72 110.7(2) . . ? C73 O3 C74 110.1(2) . . ? C76 O4 C75 109.6(3) . . ? C6 O5 C77 112.48(19) . . ? C17 O6 C78 115.49(19) . . ? C80 O7 C79 117.8(2) . . ? C81 O8 C82 114.2(2) . . ? C83 O9 C84 111.0(2) . . ? C18 O10 C85 114.93(18) . . ? C29 O11 C86 122.69(18) . . ? C88 O12 C87 110.0(3) . . ? C89 O13 C90 126.0(3) . . ? C92 O14 C91 128.4(2) . . ? C30 O15 C93 113.31(17) . . ? C101 O16 C102 120.5(3) . . ? F4 P1 F6 92.98(12) . . ? F4 P1 F1 88.63(12) . . ? F6 P1 F1 178.37(13) . . ? F4 P1 F3 91.89(12) . . ? F6 P1 F3 89.91(12) . . ? F1 P1 F3 90.30(13) . . ? F4 P1 F5 90.21(12) . . ? F6 P1 F5 88.96(12) . . ? F1 P1 F5 90.77(12) . . ? F3 P1 F5 177.66(13) . . ? F4 P1 F2 177.28(13) . . ? F6 P1 F2 88.69(12) . . ? F1 P1 F2 89.69(12) . . ? F3 P1 F2 90.25(12) . . ? F5 P1 F2 87.68(12) . . ? F7 P2 F10 90.29(12) . . ? F7 P2 F11 93.58(12) . . ? F10 P2 F11 88.28(11) . . ? F7 P2 F9 89.14(12) . . ? F10 P2 F9 93.30(12) . . ? F11 P2 F9 176.85(13) . . ? F7 P2 F12 178.26(13) . . ? F10 P2 F12 89.63(12) . . ? F11 P2 F12 88.15(12) . . ? F9 P2 F12 89.13(12) . . ? F7 P2 F8 92.45(13) . . ? F10 P2 F8 176.39(13) . . ? F11 P2 F8 89.20(12) . . ? F9 P2 F8 89.09(12) . . ? F12 P2 F8 87.70(12) . . ? F14 P3 F15 177.05(14) . . ? F14 P3 F13 91.21(12) . . ? F15 P3 F13 90.38(12) . . ? F14 P3 F18 88.41(11) . . ? F15 P3 F18 89.87(12) . . ? F13 P3 F18 177.02(13) . . ? F14 P3 F17 91.20(12) . . ? F15 P3 F17 91.19(12) . . ? F13 P3 F17 93.38(12) . . ? F18 P3 F17 89.58(12) . . ? F14 P3 F16 91.33(12) . . ? F15 P3 F16 86.22(12) . . ? F13 P3 F16 88.56(12) . . ? F18 P3 F16 88.49(12) . . ? F17 P3 F16 176.78(13) . . ? N8 Pd1 N7 87.24(14) . . ? N8 Pd1 N2 94.73(14) . . ? N7 Pd1 N2 177.32(14) . . ? N8 Pd1 N1 176.39(15) . . ? N7 Pd1 N1 95.86(15) . . ? N2 Pd1 N1 82.23(15) . . ? N9 Pd2 N10 88.47(13) . . ? N9 Pd2 N4 175.77(13) . . ? N10 Pd2 N4 94.29(13) . . ? N9 Pd2 N3 94.99(14) . . ? N10 Pd2 N3 175.50(14) . . ? N4 Pd2 N3 82.10(13) . . ? N6 Pd3 N12 93.89(15) . . ? N6 Pd3 N11 177.53(14) . . ? N12 Pd3 N11 87.77(15) . . ? N6 Pd3 N5 81.32(14) . . ? N12 Pd3 N5 174.99(14) . . ? N11 Pd3 N5 97.07(14) . . ? 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 -1.4(6) . . . . ? C1 C2 C3 C4 2.5(6) . . . . ? C2 C3 C4 C5 178.1(4) . . . . ? C2 C3 C4 C12 -2.4(6) . . . . ? C12 C4 C5 O1 -172.2(3) . . . . ? C3 C4 C5 O1 7.2(5) . . . . ? C12 C4 C5 C6 0.8(6) . . . . ? C3 C4 C5 C6 -179.8(4) . . . . ? O1 C5 C6 C7 171.9(3) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? O1 C5 C6 O5 -16.8(5) . . . . ? C4 C5 C6 O5 170.7(3) . . . . ? C5 C6 C7 C11 0.4(5) . . . . ? O5 C6 C7 C11 -170.8(3) . . . . ? C5 C6 C7 C8 -180.0(4) . . . . ? O5 C6 C7 C8 8.9(5) . . . . ? C11 C7 C8 C9 -4.0(6) . . . . ? C6 C7 C8 C9 176.3(4) . . . . ? C7 C8 C9 C10 4.4(6) . . . . ? C8 C9 C10 N2 -3.2(6) . . . . ? C6 C7 C11 C12 -0.2(6) . . . . ? C8 C7 C11 C12 -179.9(4) . . . . ? C6 C7 C11 N2 -177.9(3) . . . . ? C8 C7 C11 N2 2.4(6) . . . . ? C5 C4 C12 N1 -179.1(3) . . . . ? C3 C4 C12 N1 1.4(5) . . . . ? C5 C4 C12 C11 -0.6(6) . . . . ? C3 C4 C12 C11 179.9(4) . . . . ? C7 C11 C12 N1 178.9(3) . . . . ? N2 C11 C12 N1 -3.3(5) . . . . ? C7 C11 C12 C4 0.3(6) . . . . ? N2 C11 C12 C4 178.1(3) . . . . ? N3 C13 C14 C15 -3.5(6) . . . . ? C13 C14 C15 C16 3.4(5) . . . . ? C14 C15 C16 C24 -3.1(5) . . . . ? C14 C15 C16 C17 -179.9(4) . . . . ? C24 C16 C17 O6 -176.3(3) . . . . ? C15 C16 C17 O6 0.4(5) . . . . ? C24 C16 C17 C18 4.1(5) . . . . ? C15 C16 C17 C18 -179.1(4) . . . . ? O6 C17 C18 O10 1.5(5) . . . . ? C16 C17 C18 O10 -178.9(3) . . . . ? O6 C17 C18 C19 175.5(3) . . . . ? C16 C17 C18 C19 -4.9(6) . . . . ? O10 C18 C19 C20 -3.1(6) . . . . ? C17 C18 C19 C20 -177.2(4) . . . . ? O10 C18 C19 C23 179.4(3) . . . . ? C17 C18 C19 C23 5.3(6) . . . . ? C18 C19 C20 C21 -177.5(4) . . . . ? C23 C19 C20 C21 0.1(6) . . . . ? C19 C20 C21 C22 -0.4(6) . . . . ? C20 C21 C22 N4 0.0(6) . . . . ? C18 C19 C23 N4 178.2(3) . . . . ? C20 C19 C23 N4 0.5(5) . . . . ? C18 C19 C23 C24 -5.0(5) . . . . ? C20 C19 C23 C24 177.3(3) . . . . ? N4 C23 C24 N3 -2.2(5) . . . . ? C19 C23 C24 N3 -179.0(3) . . . . ? N4 C23 C24 C16 -178.8(3) . . . . ? C19 C23 C24 C16 4.4(5) . . . . ? C15 C16 C24 N3 2.6(5) . . . . ? C17 C16 C24 N3 179.7(3) . . . . ? C15 C16 C24 C23 179.1(3) . . . . ? C17 C16 C24 C23 -3.9(5) . . . . ? N5 C25 C26 C27 0.2(5) . . . . ? C25 C26 C27 C28 0.7(5) . . . . ? C26 C27 C28 C36 -1.5(6) . . . . ? C26 C27 C28 C29 176.5(4) . . . . ? C36 C28 C29 C30 -6.5(6) . . . . ? C27 C28 C29 C30 175.4(4) . . . . ? C36 C28 C29 O11 176.2(3) . . . . ? C27 C28 C29 O11 -1.8(5) . . . . ? O11 C29 C30 O15 2.2(6) . . . . ? C28 C29 C30 O15 -174.8(3) . . . . ? O11 C29 C30 C31 -178.4(3) . . . . ? C28 C29 C30 C31 4.7(6) . . . . ? C29 C30 C31 C32 -178.8(4) . . . . ? O15 C30 C31 C32 0.7(6) . . . . ? C29 C30 C31 C35 0.0(6) . . . . ? O15 C30 C31 C35 179.5(3) . . . . ? C30 C31 C32 C33 178.7(4) . . . . ? C35 C31 C32 C33 -0.1(6) . . . . ? C31 C32 C33 C34 3.2(7) . . . . ? C32 C33 C34 N6 -3.0(6) . . . . ? C32 C31 C35 N6 -3.5(6) . . . . ? C30 C31 C35 N6 177.6(3) . . . . ? C32 C31 C35 C36 175.9(4) . . . . ? C30 C31 C35 C36 -3.0(6) . . . . ? C27 C28 C36 N5 1.4(6) . . . . ? C29 C28 C36 N5 -176.6(3) . . . . ? C27 C28 C36 C35 -178.2(4) . . . . ? C29 C28 C36 C35 3.7(7) . . . . ? N6 C35 C36 C28 -179.6(4) . . . . ? C31 C35 C36 C28 1.0(7) . . . . ? N6 C35 C36 N5 0.8(6) . . . . ? C31 C35 C36 N5 -178.6(3) . . . . ? N8 C37 C38 C39 -178.5(4) . . . . ? C46 C37 C38 C39 -0.4(7) . . . . ? C37 C38 C39 C44 0.7(6) . . . . ? C37 C38 C39 C40 179.2(4) . . . . ? C44 C39 C40 C41 4.3(6) . . . . ? C38 C39 C40 C41 -174.2(4) . . . . ? C39 C40 C41 C42 -8.4(6) . . . . ? C40 C41 C42 C43 5.1(6) . . . . ? C41 C42 C43 C44 2.3(6) . . . . ? C42 C43 C44 C39 -6.3(6) . . . . ? C42 C43 C44 C45 177.4(4) . . . . ? C38 C39 C44 C43 -178.7(4) . . . . ? C40 C39 C44 C43 2.8(6) . . . . ? C38 C39 C44 C45 -2.3(6) . . . . ? C40 C39 C44 C45 179.2(4) . . . . ? C43 C44 C45 C46 179.9(4) . . . . ? C39 C44 C45 C46 3.5(6) . . . . ? C44 C45 C46 N9 175.2(3) . . . . ? C44 C45 C46 C37 -3.2(6) . . . . ? C38 C37 C46 N9 -177.0(4) . . . . ? N8 C37 C46 N9 1.5(4) . . . . ? C38 C37 C46 C45 1.7(7) . . . . ? N8 C37 C46 C45 -179.7(3) . . . . ? N10 C48 C49 C50 179.9(4) . . . . ? C57 C48 C49 C50 0.5(6) . . . . ? C48 C49 C50 C55 1.0(6) . . . . ? C48 C49 C50 C51 179.7(4) . . . . ? C55 C50 C51 C52 1.6(4) . . . . ? C49 C50 C51 C52 -177.2(3) . . . . ? C50 C51 C52 C53 0.1(6) . . . . ? C51 C52 C53 C54 -0.2(6) . . . . ? C52 C53 C54 C55 -1.5(7) . . . . ? C49 C50 C55 C54 175.7(3) . . . . ? C51 C50 C55 C54 -3.1(5) . . . . ? C49 C50 C55 C56 -2.0(5) . . . . ? C51 C50 C55 C56 179.2(3) . . . . ? C53 C54 C55 C50 3.2(6) . . . . ? C53 C54 C55 C56 -179.2(4) . . . . ? C50 C55 C56 C57 1.4(5) . . . . ? C54 C55 C56 C57 -176.2(4) . . . . ? C55 C56 C57 N11 179.5(3) . . . . ? C55 C56 C57 C48 0.1(5) . . . . ? C49 C48 C57 C56 -1.1(4) . . . . ? N10 C48 C57 C56 179.4(3) . . . . ? C49 C48 C57 N11 179.4(3) . . . . ? N10 C48 C57 N11 -0.1(2) . . . . ? N12 C59 C60 C61 179.5(4) . . . . ? C68 C59 C60 C61 2.5(6) . . . . ? C59 C60 C61 C62 175.5(3) . . . . ? C59 C60 C61 C66 -1.1(6) . . . . ? C66 C61 C62 C63 -0.2(5) . . . . ? C60 C61 C62 C63 -177.0(4) . . . . ? C61 C62 C63 C64 -0.8(6) . . . . ? C62 C63 C64 C65 1.1(6) . . . . ? C63 C64 C65 C66 -0.3(6) . . . . ? C64 C65 C66 C61 -0.7(6) . . . . ? C64 C65 C66 C67 177.4(4) . . . . ? C62 C61 C66 C65 1.0(5) . . . . ? C60 C61 C66 C65 177.7(4) . . . . ? C62 C61 C66 C67 -177.1(3) . . . . ? C60 C61 C66 C67 -0.4(6) . . . . ? C65 C66 C67 C68 -177.3(4) . . . . ? C61 C66 C67 C68 0.8(6) . . . . ? C66 C67 C68 C59 0.6(6) . . . . ? C66 C67 C68 N7 178.3(3) . . . . ? N12 C59 C68 C67 -179.9(4) . . . . ? C60 C59 C68 C67 -2.2(7) . . . . ? N12 C59 C68 N7 1.9(4) . . . . ? C60 C59 C68 N7 179.6(3) . . . . ? O1 C70 C71 O2 -89.9(3) . . . . ? O2 C72 C73 O3 55.6(3) . . . . ? O3 C74 C75 O4 -124.1(3) . . . . ? O4 C76 C77 O5 -109.1(4) . . . . ? O6 C78 C79 O7 67.6(5) . . . . ? O7 C80 C81 O8 -46.1(5) . . . . ? O8 C82 C83 O9 -61.3(4) . . . . ? O9 C84 C85 O10 -72.7(3) . . . . ? O11 C86 C87 O12 -176.9(3) . . . . ? O12 C88 C89 O13 49.9(5) . . . . ? O13 C90 C91 O14 -57.1(5) . . . . ? O14 C92 C93 O15 -77.6(3) . . . . ? C2 C1 N1 C12 0.5(5) . . . . ? C2 C1 N1 Pd1 178.3(3) . . . . ? C4 C12 N1 C1 -0.5(5) . . . . ? C11 C12 N1 C1 -179.1(3) . . . . ? C4 C12 N1 Pd1 -178.7(3) . . . . ? C11 C12 N1 Pd1 2.8(4) . . . . ? C9 C10 N2 C11 1.5(5) . . . . ? C9 C10 N2 Pd1 -179.8(3) . . . . ? C7 C11 N2 C10 -1.2(5) . . . . ? C12 C11 N2 C10 -179.0(3) . . . . ? C7 C11 N2 Pd1 179.9(3) . . . . ? C12 C11 N2 Pd1 2.1(4) . . . . ? C14 C13 N3 C24 3.1(5) . . . . ? C14 C13 N3 Pd2 -176.5(3) . . . . ? C23 C24 N3 C13 -179.3(3) . . . . ? C16 C24 N3 C13 -2.7(4) . . . . ? C23 C24 N3 Pd2 0.4(3) . . . . ? C16 C24 N3 Pd2 177.0(3) . . . . ? C21 C22 N4 C23 0.6(4) . . . . ? C21 C22 N4 Pd2 -179.9(2) . . . . ? C24 C23 N4 C22 -177.7(3) . . . . ? C19 C23 N4 C22 -0.9(4) . . . . ? C24 C23 N4 Pd2 2.7(3) . . . . ? C19 C23 N4 Pd2 179.5(3) . . . . ? C26 C25 N5 C36 -0.4(4) . . . . ? C26 C25 N5 Pd3 -175.1(2) . . . . ? C28 C36 N5 C25 -0.5(5) . . . . ? C35 C36 N5 C25 179.2(3) . . . . ? C28 C36 N5 Pd3 175.1(3) . . . . ? C35 C36 N5 Pd3 -5.3(4) . . . . ? C33 C34 N6 C35 -0.7(5) . . . . ? C33 C34 N6 Pd3 179.7(3) . . . . ? C36 C35 N6 C34 -175.5(3) . . . . ? C31 C35 N6 C34 3.9(5) . . . . ? C36 C35 N6 Pd3 4.2(4) . . . . ? C31 C35 N6 Pd3 -176.4(3) . . . . ? N12 C69 N7 C68 -0.3(3) . . . . ? N12 C69 N7 Pd1 -167.5(2) . . . . ? C67 C68 N7 C69 -179.0(4) . . . . ? C59 C68 N7 C69 -1.0(4) . . . . ? C67 C68 N7 Pd1 -12.8(5) . . . . ? C59 C68 N7 Pd1 165.3(2) . . . . ? N9 C47 N8 C37 4.4(4) . . . . ? N9 C47 N8 Pd1 159.3(2) . . . . ? C38 C37 N8 C47 175.1(5) . . . . ? C46 C37 N8 C47 -3.3(4) . . . . ? C38 C37 N8 Pd1 18.8(6) . . . . ? C46 C37 N8 Pd1 -159.6(2) . . . . ? N8 C47 N9 C46 -3.4(3) . . . . ? N8 C47 N9 Pd2 -172.9(2) . . . . ? C45 C46 N9 C47 -177.5(4) . . . . ? C37 C46 N9 C47 1.0(4) . . . . ? C45 C46 N9 Pd2 -7.4(5) . . . . ? C37 C46 N9 Pd2 171.2(2) . . . . ? N11 C58 N10 C48 1.1(3) . . . . ? N11 C58 N10 Pd2 169.3(2) . . . . ? C49 C48 N10 C58 -180.0(4) . . . . ? C57 C48 N10 C58 -0.5(2) . . . . ? C49 C48 N10 Pd2 10.7(5) . . . . ? C57 C48 N10 Pd2 -169.89(16) . . . . ? N10 C58 N11 C57 -1.1(4) . . . . ? N10 C58 N11 Pd3 -157.1(2) . . . . ? C56 C57 N11 C58 -178.7(4) . . . . ? C48 C57 N11 C58 0.7(3) . . . . ? C56 C57 N11 Pd3 -22.5(5) . . . . ? C48 C57 N11 Pd3 156.88(18) . . . . ? N7 C69 N12 C59 1.5(3) . . . . ? N7 C69 N12 Pd3 178.6(2) . . . . ? C68 C59 N12 C69 -2.0(4) . . . . ? C60 C59 N12 C69 -179.4(4) . . . . ? C68 C59 N12 Pd3 -178.9(2) . . . . ? C60 C59 N12 Pd3 3.8(6) . . . . ? C4 C5 O1 C70 105.4(3) . . . . ? C6 C5 O1 C70 -67.4(3) . . . . ? C71 C70 O1 C5 -171.7(2) . . . . ? C70 C71 O2 C72 178.3(3) . . . . ? C73 C72 O2 C71 -175.3(3) . . . . ? C72 C73 O3 C74 -83.1(4) . . . . ? C75 C74 O3 C73 -149.8(3) . . . . ? C77 C76 O4 C75 135.3(3) . . . . ? C74 C75 O4 C76 -87.7(3) . . . . ? C5 C6 O5 C77 -83.1(3) . . . . ? C7 C6 O5 C77 88.2(3) . . . . ? C76 C77 O5 C6 174.2(3) . . . . ? C18 C17 O6 C78 92.9(3) . . . . ? C16 C17 O6 C78 -86.6(3) . . . . ? C79 C78 O6 C17 161.5(3) . . . . ? C81 C80 O7 C79 -105.5(4) . . . . ? C78 C79 O7 C80 119.2(3) . . . . ? C80 C81 O8 C82 174.0(3) . . . . ? C83 C82 O8 C81 -98.6(3) . . . . ? C82 C83 O9 C84 170.1(3) . . . . ? C85 C84 O9 C83 -85.5(4) . . . . ? C17 C18 O10 C85 -106.3(3) . . . . ? C19 C18 O10 C85 79.7(4) . . . . ? C84 C85 O10 C18 -165.0(2) . . . . ? C30 C29 O11 C86 -53.9(4) . . . . ? C28 C29 O11 C86 123.1(3) . . . . ? C87 C86 O11 C29 -38.9(4) . . . . ? C89 C88 O12 C87 72.7(4) . . . . ? C86 C87 O12 C88 -123.0(4) . . . . ? C88 C89 O13 C90 167.5(3) . . . . ? C91 C90 O13 C89 115.7(4) . . . . ? C93 C92 O14 C91 156.7(3) . . . . ? C90 C91 O14 C92 -70.5(4) . . . . ? C29 C30 O15 C93 -90.1(4) . . . . ? C31 C30 O15 C93 90.4(3) . . . . ? C92 C93 O15 C30 179.5(2) . . . . ? C100 C101 O16 C102 -170.8(3) . . . . ? C103 C102 O16 C101 -177.7(3) . . . . ? C47 N8 Pd1 N7 -72.8(3) . . . . ? C37 N8 Pd1 N7 78.1(2) . . . . ? C47 N8 Pd1 N2 109.0(3) . . . . ? C37 N8 Pd1 N2 -100.1(2) . . . . ? C69 N7 Pd1 N8 77.1(3) . . . . ? C68 N7 Pd1 N8 -87.0(3) . . . . ? C69 N7 Pd1 N1 -101.1(3) . . . . ? C68 N7 Pd1 N1 94.8(3) . . . . ? C10 N2 Pd1 N8 2.7(3) . . . . ? C11 N2 Pd1 N8 -178.4(2) . . . . ? C10 N2 Pd1 N1 -179.2(3) . . . . ? C11 N2 Pd1 N1 -0.4(2) . . . . ? C1 N1 Pd1 N7 2.7(4) . . . . ? C12 N1 Pd1 N7 -179.4(2) . . . . ? C1 N1 Pd1 N2 -179.2(4) . . . . ? C12 N1 Pd1 N2 -1.3(2) . . . . ? C47 N9 Pd2 N10 77.5(3) . . . . ? C46 N9 Pd2 N10 -90.3(2) . . . . ? C47 N9 Pd2 N3 -105.4(3) . . . . ? C46 N9 Pd2 N3 86.8(2) . . . . ? C58 N10 Pd2 N9 -73.1(3) . . . . ? C48 N10 Pd2 N9 93.6(2) . . . . ? C58 N10 Pd2 N4 110.1(3) . . . . ? C48 N10 Pd2 N4 -83.2(2) . . . . ? C22 N4 Pd2 N10 -4.1(3) . . . . ? C23 N4 Pd2 N10 175.5(2) . . . . ? C22 N4 Pd2 N3 178.6(3) . . . . ? C23 N4 Pd2 N3 -1.82(19) . . . . ? C13 N3 Pd2 N9 3.6(3) . . . . ? C24 N3 Pd2 N9 -176.1(2) . . . . ? C13 N3 Pd2 N4 -179.5(3) . . . . ? C24 N3 Pd2 N4 0.8(2) . . . . ? C34 N6 Pd3 N12 -4.2(3) . . . . ? C35 N6 Pd3 N12 176.2(2) . . . . ? C34 N6 Pd3 N5 174.3(3) . . . . ? C35 N6 Pd3 N5 -5.3(2) . . . . ? C69 N12 Pd3 N6 96.2(3) . . . . ? C59 N12 Pd3 N6 -87.4(3) . . . . ? C69 N12 Pd3 N11 -85.6(3) . . . . ? C59 N12 Pd3 N11 90.8(3) . . . . ? C58 N11 Pd3 N12 70.4(3) . . . . ? C57 N11 Pd3 N12 -81.7(3) . . . . ? C58 N11 Pd3 N5 -108.3(3) . . . . ? C57 N11 Pd3 N5 99.6(3) . . . . ? C25 N5 Pd3 N6 -179.1(3) . . . . ? C36 N5 Pd3 N6 5.7(2) . . . . ? C25 N5 Pd3 N11 2.8(3) . . . . ? C36 N5 Pd3 N11 -172.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.831 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.065