# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email JIHONG@PLAZA.SNU.AC.KR _publ_contact_author_name 'Prof Jong-In Hong' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.-I.Hong Y.K.Chung S.J.Park S.Sakamoto D.M.Shin K.Yamaguchi data_go _database_code_CSD 196032 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H90 N12 O30 Pd2' _chemical_formula_weight 1780.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5964(2) _cell_length_b 16.1544(3) _cell_length_c 22.5305(5) _cell_angle_alpha 91.0518(8) _cell_angle_beta 94.1617(7) _cell_angle_gamma 91.6743(13) _cell_volume 4206.89(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 23729 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.2256 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.37 _reflns_number_total 15047 _reflns_number_gt 5984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material WinGX _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^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15047 _refine_ls_number_parameters 1076 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.17862(4) 0.81983(3) 0.09599(2) 0.0539(2) Uani 1 1 d . . . Pd2 Pd 0.40000(4) 0.81962(3) 0.39833(2) 0.0564(2) Uani 1 1 d . . . O1 O -0.0609(3) 0.5577(3) 0.1499(2) 0.0592(13) Uani 1 1 d . . . O2 O 0.4199(3) 0.4599(3) 0.05809(18) 0.0464(11) Uani 1 1 d . . . O3 O 0.1090(4) 0.5606(3) 0.4222(2) 0.0578(13) Uani 1 1 d . . . O4 O 0.6155(3) 0.4718(3) 0.3521(2) 0.0634(14) Uani 1 1 d . . . O5 O -0.1425(3) 0.5052(3) 0.2534(2) 0.0503(12) Uani 1 1 d . . . O6 O 0.0074(3) 0.4466(3) 0.06790(18) 0.0505(12) Uani 1 1 d . . . O7 O 0.1921(3) 0.4167(3) 0.03814(17) 0.0497(11) Uani 1 1 d . . . O8 O 0.5577(3) 0.3823(3) 0.14278(19) 0.0496(12) Uani 1 1 d . . . O9 O -0.0783(3) 0.5042(3) 0.3551(2) 0.0513(12) Uani 1 1 d . . . O10 O 0.2815(4) 0.4544(3) 0.46107(18) 0.0561(12) Uani 1 1 d . . . O11 O 0.4650(3) 0.4242(3) 0.43114(19) 0.0577(13) Uani 1 1 d . . . O12 O 0.6258(3) 0.3851(3) 0.2449(2) 0.0532(12) Uani 1 1 d . . . N1 N 0.0121(4) 0.7778(3) 0.0835(2) 0.0498(14) Uani 1 1 d . . . N2 N 0.2354(4) 0.7205(3) 0.0526(3) 0.0497(14) Uani 1 1 d . . . N3 N 0.3363(4) 0.7530(3) 0.4654(2) 0.0480(14) Uani 1 1 d . . . N4 N 0.5331(4) 0.7423(3) 0.3955(2) 0.0500(14) Uani 1 1 d . . . N5 N 0.1379(5) 0.9266(4) 0.1362(3) 0.0777(19) Uani 1 1 d . . . H5A H 0.0778 0.9490 0.1154 0.093 Uiso 1 1 calc R . . H5B H 0.1168 0.9162 0.1730 0.093 Uiso 1 1 calc R . . N6 N 0.3417(4) 0.8665(4) 0.1097(3) 0.0727(18) Uani 1 1 d . . . H6C H 0.3873 0.8292 0.1279 0.087 Uiso 1 1 calc R . . H6D H 0.3702 0.8787 0.0746 0.087 Uiso 1 1 calc R . . N7 N 0.2786(6) 0.9054(4) 0.4011(3) 0.098(2) Uani 1 1 d . . . H7A H 0.2084 0.8800 0.4008 0.118 Uiso 1 1 calc R . . H7B H 0.2904 0.9353 0.4352 0.118 Uiso 1 1 calc R . . N8 N 0.4515(6) 0.8872(4) 0.3306(3) 0.094(2) Uani 1 1 d . . . H8A H 0.5288 0.8952 0.3344 0.113 Uiso 1 1 calc R . . H8B H 0.4325 0.8601 0.2959 0.113 Uiso 1 1 calc R . . C1 C -0.0203(6) 0.7039(4) 0.1033(3) 0.0501(18) Uani 1 1 d . . . H1 H 0.0362 0.6721 0.1224 0.060 Uiso 1 1 calc R . . C2 C -0.1310(6) 0.6718(4) 0.0975(3) 0.0496(18) Uani 1 1 d . . . C3 C -0.2143(6) 0.7195(5) 0.0709(4) 0.077(2) Uani 1 1 d . . . H3 H -0.2912 0.7009 0.0674 0.092 Uiso 1 1 calc R . . C4 C -0.1836(7) 0.7948(5) 0.0494(4) 0.090(3) Uani 1 1 d . . . H4 H -0.2390 0.8274 0.0302 0.107 Uiso 1 1 calc R . . C5 C -0.0722(7) 0.8211(5) 0.0562(3) 0.071(2) Uani 1 1 d . . . H5 H -0.0527 0.8724 0.0411 0.085 Uiso 1 1 calc R . . C6 C -0.1617(5) 0.5870(4) 0.1194(3) 0.0537(19) Uani 1 1 d . . . H6A H -0.2237 0.5902 0.1459 0.064 Uiso 1 1 calc R . . H6B H -0.1867 0.5502 0.0861 0.064 Uiso 1 1 calc R . . C7 C 0.3013(5) 0.6641(4) 0.0805(3) 0.0450(17) Uani 1 1 d . . . H7 H 0.3131 0.6673 0.1218 0.054 Uiso 1 1 calc R . . C8 C 0.3525(5) 0.6011(4) 0.0499(3) 0.0448(17) Uani 1 1 d . . . C9 C 0.3322(5) 0.5958(4) -0.0111(3) 0.0526(18) Uani 1 1 d . . . H9 H 0.3662 0.5544 -0.0325 0.063 Uiso 1 1 calc R . . C10 C 0.2625(5) 0.6508(5) -0.0405(3) 0.058(2) Uani 1 1 d . . . H10 H 0.2472 0.6471 -0.0815 0.069 Uiso 1 1 calc R . . C11 C 0.2152(5) 0.7126(4) -0.0068(3) 0.0531(19) Uani 1 1 d . . . H11 H 0.1674 0.7502 -0.0263 0.064 Uiso 1 1 calc R . . C12 C 0.4300(5) 0.5408(4) 0.0839(3) 0.0555(19) Uani 1 1 d . . . H12A H 0.5098 0.5607 0.0842 0.067 Uiso 1 1 calc R . . H12B H 0.4093 0.5387 0.1248 0.067 Uiso 1 1 calc R . . C13 C 0.2563(6) 0.6925(4) 0.4534(3) 0.0523(18) Uani 1 1 d . . . H13 H 0.2304 0.6810 0.4140 0.063 Uiso 1 1 calc R . . C14 C 0.2105(5) 0.6461(4) 0.4986(3) 0.0481(18) Uani 1 1 d . . . C15 C 0.2501(6) 0.6643(5) 0.5574(3) 0.0546(19) Uani 1 1 d . . . H15 H 0.2224 0.6342 0.5884 0.066 Uiso 1 1 calc R . . C16 C 0.3308(6) 0.7274(5) 0.5684(3) 0.060(2) Uani 1 1 d . . . H16 H 0.3575 0.7409 0.6074 0.072 Uiso 1 1 calc R . . C17 C 0.3728(5) 0.7713(5) 0.5217(4) 0.057(2) Uani 1 1 d . . . H17 H 0.4272 0.8142 0.5298 0.069 Uiso 1 1 calc R . . C18 C 0.1166(6) 0.5794(5) 0.4848(3) 0.062(2) Uani 1 1 d . . . H18A H 0.1352 0.5300 0.5069 0.075 Uiso 1 1 calc R . . H18B H 0.0430 0.5987 0.4964 0.075 Uiso 1 1 calc R . . C19 C 0.5268(6) 0.6752(5) 0.3598(3) 0.0556(19) Uani 1 1 d . . . H19 H 0.4609 0.6662 0.3341 0.067 Uiso 1 1 calc R . . C20 C 0.6155(5) 0.6171(4) 0.3591(3) 0.0450(17) Uani 1 1 d . . . C21 C 0.7113(6) 0.6318(5) 0.3974(3) 0.060(2) Uani 1 1 d . . . H21 H 0.7705 0.5942 0.3997 0.072 Uiso 1 1 calc R . . C22 C 0.7196(6) 0.7034(5) 0.4327(3) 0.073(2) Uani 1 1 d . . . H22 H 0.7859 0.7152 0.4575 0.088 Uiso 1 1 calc R . . C23 C 0.6285(6) 0.7569(5) 0.4308(3) 0.059(2) Uani 1 1 d . . . H23 H 0.6342 0.8044 0.4550 0.071 Uiso 1 1 calc R . . C24 C 0.6029(5) 0.5453(4) 0.3178(3) 0.0545(19) Uani 1 1 d . . . H24A H 0.5275 0.5446 0.2961 0.065 Uiso 1 1 calc R . . H24B H 0.6616 0.5484 0.2893 0.065 Uiso 1 1 calc R . . C25 C -0.0582(5) 0.4746(4) 0.1644(3) 0.0430(17) Uani 1 1 d . . . C26 C -0.0103(5) 0.4209(4) 0.1252(3) 0.0396(16) Uani 1 1 d . . . C27 C 0.0146(5) 0.3395(4) 0.1424(3) 0.0426(17) Uani 1 1 d . . . C28 C -0.0142(4) 0.3152(4) 0.1979(3) 0.0383(16) Uani 1 1 d . . . H28 H 0.0021 0.2618 0.2100 0.046 Uiso 1 1 calc R . . C29 C -0.0676(4) 0.3687(4) 0.2370(3) 0.0395(16) Uani 1 1 d . . . C30 C -0.0880(5) 0.4491(4) 0.2195(3) 0.0414(16) Uani 1 1 d . . . C31 C 0.3730(5) 0.3983(4) 0.0915(3) 0.0421(16) Uani 1 1 d . . . C32 C 0.4416(5) 0.3559(4) 0.1340(3) 0.0415(16) Uani 1 1 d . . . C33 C 0.3981(5) 0.2898(4) 0.1643(3) 0.0403(16) Uani 1 1 d . . . C34 C 0.2808(5) 0.2677(4) 0.1521(3) 0.0399(16) Uani 1 1 d . . . H34 H 0.2495 0.2242 0.1728 0.048 Uiso 1 1 calc R . . C35 C 0.2096(5) 0.3078(4) 0.1107(3) 0.0412(16) Uani 1 1 d . . . C36 C 0.2565(5) 0.3727(4) 0.0817(3) 0.0422(17) Uani 1 1 d . . . C37 C 0.1028(5) 0.4779(4) 0.4054(3) 0.0471(17) Uani 1 1 d . . . C38 C 0.0113(5) 0.4502(4) 0.3667(3) 0.0444(17) Uani 1 1 d . . . C39 C 0.0039(5) 0.3703(4) 0.3436(3) 0.0431(16) Uani 1 1 d . . . C40 C 0.0969(5) 0.3180(4) 0.3587(3) 0.0414(16) Uani 1 1 d . . . H40 H 0.0949 0.2645 0.3425 0.050 Uiso 1 1 calc R . . C41 C 0.1910(5) 0.3440(4) 0.3967(3) 0.0443(17) Uani 1 1 d . . . C42 C 0.1916(5) 0.4247(5) 0.4193(3) 0.0479(18) Uani 1 1 d . . . C43 C 0.5424(5) 0.3611(4) 0.2828(3) 0.0459(17) Uani 1 1 d . . . C44 C 0.5391(5) 0.4064(4) 0.3363(3) 0.0494(18) Uani 1 1 d . . . C45 C 0.4604(6) 0.3815(4) 0.3767(3) 0.0450(17) Uani 1 1 d . . . C46 C 0.3850(5) 0.3149(4) 0.3652(3) 0.0411(16) Uani 1 1 d . . . C47 C 0.3913(5) 0.2715(4) 0.3113(3) 0.0404(16) Uani 1 1 d . . . H47 H 0.3407 0.2265 0.3026 0.049 Uiso 1 1 calc R . . C48 C 0.4709(5) 0.2931(4) 0.2698(3) 0.0412(16) Uani 1 1 d . . . C49 C -0.0757(6) 0.5460(4) 0.3004(3) 0.058(2) Uani 1 1 d . . . H49A H -0.1040 0.6014 0.3055 0.070 Uiso 1 1 calc R . . H49B H 0.0038 0.5513 0.2899 0.070 Uiso 1 1 calc R . . C50 C 0.3835(6) 0.4860(4) 0.4376(3) 0.060(2) Uani 1 1 d . . . H50A H 0.3638 0.5098 0.3991 0.072 Uiso 1 1 calc R . . H50B H 0.4177 0.5298 0.4638 0.072 Uiso 1 1 calc R . . C51 C 0.5892(5) 0.4310(4) 0.1947(3) 0.0559(19) Uani 1 1 d . . . H51A H 0.6510 0.4697 0.1862 0.067 Uiso 1 1 calc R . . H51B H 0.5234 0.4630 0.2043 0.067 Uiso 1 1 calc R . . C52 C 0.1200(5) 0.4788(4) 0.0592(3) 0.0553(19) Uani 1 1 d . . . H52A H 0.1547 0.5020 0.0965 0.066 Uiso 1 1 calc R . . H52B H 0.1144 0.5230 0.0307 0.066 Uiso 1 1 calc R . . C53 C -0.0968(5) 0.3431(4) 0.2984(3) 0.0445(17) Uani 1 1 d . . . H53 H -0.1633 0.3754 0.3082 0.053 Uiso 1 1 calc R . . C54 C 0.2957(5) 0.2910(4) 0.4087(3) 0.0453(17) Uani 1 1 d . . . H54 H 0.3295 0.3069 0.4486 0.054 Uiso 1 1 calc R . . C55 C 0.4757(5) 0.2472(4) 0.2108(3) 0.0430(17) Uani 1 1 d . . . H55 H 0.5552 0.2531 0.1990 0.052 Uiso 1 1 calc R . . C56 C 0.0806(5) 0.2849(4) 0.1014(3) 0.0475(17) Uani 1 1 d . . . H56 H 0.0557 0.2992 0.0604 0.057 Uiso 1 1 calc R . . C57 C -0.1342(5) 0.2515(4) 0.3027(3) 0.0519(18) Uani 1 1 d . . . H57A H -0.2030 0.2404 0.2771 0.062 Uiso 1 1 calc R . . H57B H -0.1495 0.2397 0.3430 0.062 Uiso 1 1 calc R . . H57C H -0.0735 0.2173 0.2906 0.062 Uiso 1 1 calc R . . C58 C 0.2672(6) 0.1988(4) 0.4098(3) 0.060(2) Uani 1 1 d . . . H58A H 0.2202 0.1874 0.4422 0.072 Uiso 1 1 calc R . . H58B H 0.3376 0.1690 0.4149 0.072 Uiso 1 1 calc R . . H58C H 0.2260 0.1817 0.3729 0.072 Uiso 1 1 calc R . . C59 C 0.4482(5) 0.1555(4) 0.2149(3) 0.0577(19) Uani 1 1 d . . . H59A H 0.3685 0.1472 0.2228 0.069 Uiso 1 1 calc R . . H59B H 0.4966 0.1327 0.2465 0.069 Uiso 1 1 calc R . . H59C H 0.4619 0.1282 0.1780 0.069 Uiso 1 1 calc R . . C60 C 0.0550(5) 0.1924(4) 0.1074(3) 0.0554(19) Uani 1 1 d . . . H60A H 0.0754 0.1764 0.1475 0.066 Uiso 1 1 calc R . . H60B H 0.0993 0.1618 0.0806 0.066 Uiso 1 1 calc R . . H60C H -0.0259 0.1807 0.0978 0.066 Uiso 1 1 calc R . . C61 C 0.2355(8) 0.9838(6) 0.1397(6) 0.144(5) Uani 1 1 d . . . H61A H 0.2348 1.0156 0.1036 0.173 Uiso 1 1 calc R . . H61B H 0.2297 1.0221 0.1729 0.173 Uiso 1 1 calc R . . C62 C 0.3393(8) 0.9422(6) 0.1472(5) 0.121(4) Uani 1 1 d . . . H62A H 0.3522 0.9274 0.1886 0.145 Uiso 1 1 calc R . . H62B H 0.4023 0.9795 0.1379 0.145 Uiso 1 1 calc R . . C63 C 0.2810(12) 0.9615(7) 0.3499(5) 0.135(4) Uani 1 1 d . . . H63A H 0.2289 0.9396 0.3174 0.162 Uiso 1 1 calc R . . H63B H 0.2545 1.0155 0.3614 0.162 Uiso 1 1 calc R . . C64 C 0.3935(10) 0.9698(6) 0.3309(5) 0.130(4) Uani 1 1 d . . . H64A H 0.4390 1.0084 0.3572 0.155 Uiso 1 1 calc R . . H64B H 0.3900 0.9920 0.2911 0.155 Uiso 1 1 calc R . . N1N N 0.2277(9) 0.7343(9) 0.2525(6) 0.139(4) Uani 1 1 d D . . O1N O 0.2482(8) 0.7044(7) 0.3021(4) 0.180(4) Uani 1 1 d D . . O2N O 0.2178(13) 0.8087(8) 0.2475(5) 0.240(6) Uani 1 1 d D . . O3N O 0.1978(7) 0.6896(7) 0.2108(4) 0.172(4) Uani 1 1 d D . . N2N N 0.5425(8) 0.7242(8) 0.1887(5) 0.114(3) Uani 1 1 d . . . O4N O 0.5356(7) 0.7401(6) 0.1382(4) 0.150(3) Uani 1 1 d . . . O5N O 0.5893(11) 0.6655(8) 0.2038(6) 0.252(7) Uani 1 1 d . . . O6N O 0.5076(11) 0.7749(9) 0.2207(5) 0.252(7) Uani 1 1 d . . . N3N N 0.0807(9) 0.0726(7) 0.2700(5) 0.103(3) Uani 1 1 d . . . O7N O 0.1465(8) 0.1233(6) 0.2577(4) 0.169(5) Uani 1 1 d . . . O8N O 0.0393(7) 0.0737(5) 0.3190(4) 0.150(3) Uani 1 1 d . . . O9N O 0.0542(8) 0.0082(8) 0.2423(4) 0.196(5) Uani 1 1 d . . . N4N N 0.5000 0.0000 0.5000 0.177(14) Uani 1 2 d SD . . O10N O 0.463(3) 0.0606(12) 0.4802(16) 0.180(11) Uani 0.50 1 d PD . . O11N O 0.6037(17) -0.007(3) 0.5041(16) 0.27(2) Uani 0.50 1 d PD . . O12N O 0.429(4) -0.046(3) 0.519(2) 0.74(4) Uani 0.50 1 d PD . . N5N N 0.906(2) 0.0217(14) 0.0218(9) 0.149(10) Uani 0.50 1 d PD A -1 O13N O 0.9326(18) 0.0119(9) 0.0755(9) 0.218(12) Uani 0.50 1 d PD A -1 O14N O 0.971(4) 0.001(4) -0.0140(11) 0.187(19) Uani 0.50 1 d PD A -1 O15N O 0.827(2) 0.0659(19) 0.0163(15) 0.41(3) Uani 0.50 1 d PD A -1 O11M O 0.3329(11) 0.5377(9) 0.2325(8) 0.111(5) Uani 0.493(4) 1 d P B 1 O12M O 0.280(2) 0.5421(15) 0.2871(14) 0.131(16) Uiso 0.25(2) 1 d PD B 2 O13M O 0.252(3) 0.534(2) 0.2172(16) 0.136(16) Uiso 0.25(2) 1 d P B 3 C1M C 0.2473(7) 0.4683(7) 0.2488(4) 0.091(3) Uani 1 1 d D . . O2M O 0.5618(16) 0.1015(8) 0.0136(6) 0.347(9) Uani 1 1 d D . . C2M C 0.4801(10) 0.1809(11) 0.0227(6) 0.172(6) Uani 1 1 d D . . O3M O 0.9865(11) 0.1437(10) 0.5636(10) 0.457(16) Uani 1 1 d D . . C3M C 0.9736(15) 0.1641(13) 0.4928(11) 0.326(15) Uani 1 1 d D . . O4M O 0.9117(11) 0.8654(13) 0.2846(10) 0.486(17) Uani 1 1 d D . . C4M C 0.853(2) 0.7749(10) 0.2654(11) 0.320(13) Uani 1 1 d D . . O5M O 0.7032(10) 0.9498(11) 0.3484(9) 0.351(10) Uani 1 1 d D . . C5M C 0.722(2) 1.0477(12) 0.3579(12) 0.319(14) Uani 1 1 d D . . O1S O 0.7521(18) 0.079(2) 0.1616(12) 0.29(2) Uani 0.49(3) 1 d P C 1 O2S O 0.677(3) 0.977(3) 0.140(2) 0.61(5) Uani 0.51(3) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0573(3) 0.0408(4) 0.0640(4) 0.0000(3) 0.0081(3) 0.0018(3) Pd2 0.0655(4) 0.0470(4) 0.0566(4) 0.0067(3) 0.0014(3) 0.0045(3) O1 0.048(3) 0.051(3) 0.078(3) 0.018(3) -0.008(2) -0.001(2) O2 0.053(3) 0.037(3) 0.051(3) 0.001(2) 0.018(2) 0.005(2) O3 0.065(3) 0.047(3) 0.059(3) -0.007(3) -0.002(2) -0.005(2) O4 0.053(3) 0.048(3) 0.084(4) 0.012(3) -0.025(2) -0.013(2) O5 0.039(2) 0.047(3) 0.064(3) 0.002(3) 0.000(2) 0.007(2) O6 0.036(2) 0.069(3) 0.045(3) 0.025(2) -0.001(2) -0.004(2) O7 0.053(3) 0.062(3) 0.035(3) 0.008(2) 0.005(2) 0.003(2) O8 0.039(3) 0.060(3) 0.050(3) 0.003(3) 0.010(2) -0.001(2) O9 0.047(3) 0.048(3) 0.060(3) -0.001(3) 0.010(2) 0.012(2) O10 0.060(3) 0.063(3) 0.043(3) -0.012(2) -0.005(2) 0.001(2) O11 0.050(3) 0.067(3) 0.054(3) -0.007(3) -0.012(2) 0.008(2) O12 0.036(2) 0.063(3) 0.060(3) 0.016(3) -0.004(2) 0.002(2) N1 0.051(3) 0.038(4) 0.061(4) 0.008(3) 0.005(3) 0.006(3) N2 0.050(3) 0.050(4) 0.049(4) 0.003(3) 0.000(3) 0.008(3) N3 0.052(3) 0.047(4) 0.044(4) -0.006(3) -0.001(3) 0.002(3) N4 0.063(4) 0.039(4) 0.048(4) 0.002(3) 0.004(3) 0.000(3) N5 0.074(4) 0.066(5) 0.095(5) -0.016(4) 0.024(4) -0.001(4) N6 0.064(4) 0.056(4) 0.098(5) -0.001(4) 0.009(3) -0.002(3) N7 0.092(5) 0.076(5) 0.124(7) -0.003(5) -0.011(5) 0.029(4) N8 0.148(6) 0.068(5) 0.065(5) 0.019(4) 0.003(4) -0.012(5) C1 0.055(5) 0.043(5) 0.054(5) 0.018(4) 0.006(3) 0.009(4) C2 0.051(4) 0.045(5) 0.053(5) 0.010(4) 0.001(3) 0.005(4) C3 0.055(5) 0.058(6) 0.115(7) 0.015(5) -0.005(5) 0.009(4) C4 0.053(5) 0.059(6) 0.155(9) 0.037(6) -0.018(5) 0.012(4) C5 0.072(5) 0.050(5) 0.089(6) 0.025(5) 0.002(4) 0.007(4) C6 0.040(4) 0.056(5) 0.065(5) 0.008(4) -0.003(3) 0.004(3) C7 0.050(4) 0.051(5) 0.034(4) 0.003(4) 0.005(3) 0.002(4) C8 0.034(4) 0.039(4) 0.062(5) 0.010(4) 0.002(3) -0.002(3) C9 0.050(4) 0.052(5) 0.057(5) -0.002(4) 0.009(4) 0.001(4) C10 0.054(4) 0.063(5) 0.054(5) 0.003(4) -0.006(4) 0.005(4) C11 0.049(4) 0.042(5) 0.067(6) 0.004(4) -0.003(4) 0.003(3) C12 0.038(4) 0.055(5) 0.073(5) 0.007(4) -0.003(3) 0.005(3) C13 0.057(4) 0.051(5) 0.049(5) -0.011(4) 0.005(4) 0.002(4) C14 0.052(4) 0.041(5) 0.053(5) -0.007(4) 0.014(4) 0.012(3) C15 0.056(4) 0.062(5) 0.049(5) 0.002(4) 0.016(4) 0.013(4) C16 0.054(4) 0.067(6) 0.056(5) -0.010(5) -0.011(4) 0.012(4) C17 0.047(4) 0.057(5) 0.068(6) -0.004(5) -0.001(4) -0.002(4) C18 0.070(5) 0.063(5) 0.054(5) -0.013(4) 0.018(4) -0.001(4) C19 0.058(4) 0.052(5) 0.056(5) 0.001(4) 0.004(4) -0.010(4) C20 0.051(4) 0.045(5) 0.040(4) 0.007(4) 0.007(3) -0.004(4) C21 0.060(5) 0.067(6) 0.051(5) -0.001(4) -0.002(4) 0.010(4) C22 0.057(5) 0.103(7) 0.057(5) -0.023(5) -0.011(4) 0.010(5) C23 0.062(5) 0.071(6) 0.043(4) -0.004(4) -0.005(4) -0.002(4) C24 0.053(4) 0.052(5) 0.060(5) 0.006(4) 0.012(3) -0.005(4) C25 0.036(4) 0.034(5) 0.058(5) 0.009(4) -0.006(3) 0.003(3) C26 0.035(3) 0.040(5) 0.043(4) 0.014(4) -0.007(3) -0.005(3) C27 0.031(3) 0.055(5) 0.040(4) -0.001(4) -0.003(3) -0.011(3) C28 0.034(3) 0.038(4) 0.043(4) 0.002(4) 0.002(3) 0.001(3) C29 0.030(3) 0.045(5) 0.043(4) 0.014(4) -0.003(3) -0.009(3) C30 0.033(3) 0.040(5) 0.051(5) 0.001(4) 0.001(3) -0.001(3) C31 0.047(4) 0.044(5) 0.037(4) 0.001(4) 0.013(3) 0.006(3) C32 0.035(4) 0.042(4) 0.049(4) -0.005(4) 0.005(3) 0.003(3) C33 0.048(4) 0.033(4) 0.040(4) -0.006(3) 0.007(3) 0.003(3) C34 0.045(4) 0.038(4) 0.038(4) -0.001(3) 0.009(3) -0.002(3) C35 0.040(4) 0.041(4) 0.043(4) 0.002(4) 0.007(3) -0.001(3) C36 0.039(4) 0.049(5) 0.039(4) 0.002(4) 0.003(3) 0.010(3) C37 0.050(4) 0.045(5) 0.047(4) -0.002(4) 0.012(3) -0.001(4) C38 0.041(4) 0.045(5) 0.049(4) 0.008(4) 0.005(3) 0.005(3) C39 0.050(4) 0.042(5) 0.039(4) -0.001(3) 0.013(3) -0.002(3) C40 0.048(4) 0.039(4) 0.038(4) 0.002(3) 0.005(3) -0.002(3) C41 0.052(4) 0.050(5) 0.031(4) 0.001(3) 0.001(3) 0.002(3) C42 0.046(4) 0.058(5) 0.039(4) -0.006(4) 0.003(3) -0.006(4) C43 0.034(4) 0.051(5) 0.052(5) 0.019(4) -0.003(3) 0.003(3) C44 0.044(4) 0.044(5) 0.059(5) 0.011(4) -0.012(4) -0.001(3) C45 0.057(4) 0.044(5) 0.032(4) -0.003(4) -0.009(3) 0.008(4) C46 0.041(4) 0.044(5) 0.038(4) 0.006(3) -0.004(3) 0.005(3) C47 0.035(3) 0.040(4) 0.044(4) 0.005(3) -0.012(3) 0.003(3) C48 0.040(4) 0.044(5) 0.039(4) 0.006(3) -0.006(3) 0.003(3) C49 0.062(5) 0.036(5) 0.079(6) 0.001(4) 0.013(4) 0.011(4) C50 0.054(5) 0.056(5) 0.067(5) -0.008(4) -0.011(4) -0.006(4) C51 0.040(4) 0.056(5) 0.071(5) 0.010(4) 0.005(4) -0.009(3) C52 0.046(4) 0.071(6) 0.050(5) 0.020(4) -0.001(3) 0.003(4) C53 0.031(3) 0.052(5) 0.051(4) 0.008(4) 0.004(3) 0.001(3) C54 0.056(4) 0.047(5) 0.032(4) 0.005(3) -0.007(3) 0.002(3) C55 0.033(3) 0.044(5) 0.053(4) 0.011(4) 0.006(3) 0.007(3) C56 0.054(4) 0.044(5) 0.042(4) 0.003(4) -0.004(3) -0.007(3) C57 0.054(4) 0.047(5) 0.056(5) 0.008(4) 0.015(3) -0.009(3) C58 0.066(5) 0.059(6) 0.056(5) 0.020(4) 0.005(4) 0.002(4) C59 0.067(4) 0.044(5) 0.063(5) 0.004(4) 0.004(4) 0.007(4) C60 0.052(4) 0.047(5) 0.066(5) -0.003(4) -0.007(3) 0.000(3) C61 0.082(7) 0.060(7) 0.289(16) -0.061(9) 0.026(8) -0.004(6) C62 0.091(7) 0.091(8) 0.175(11) -0.055(8) 0.001(7) -0.036(6) C63 0.178(12) 0.094(9) 0.131(10) 0.024(8) -0.028(9) 0.043(9) C64 0.153(10) 0.084(9) 0.153(11) 0.073(7) 0.003(9) 0.018(8) N1N 0.141(8) 0.150(12) 0.119(11) -0.007(10) -0.039(8) 0.010(8) O1N 0.194(8) 0.253(12) 0.087(6) 0.006(7) -0.030(6) -0.007(8) O2N 0.352(16) 0.173(11) 0.186(11) -0.011(10) -0.046(10) 0.034(12) O3N 0.174(8) 0.244(12) 0.089(6) -0.013(7) -0.026(5) -0.017(7) N2N 0.116(7) 0.146(10) 0.081(7) 0.021(8) 0.004(6) 0.007(6) O4N 0.124(6) 0.201(9) 0.127(7) 0.044(7) 0.011(6) 0.005(5) O5N 0.270(13) 0.232(13) 0.262(14) 0.124(11) 0.006(10) 0.094(11) O6N 0.336(15) 0.270(15) 0.165(10) -0.055(10) 0.110(10) 0.060(12) N3N 0.110(8) 0.115(9) 0.084(7) -0.024(7) -0.004(6) 0.036(7) O7N 0.151(7) 0.180(9) 0.170(9) 0.043(7) -0.001(6) -0.079(7) O8N 0.160(7) 0.153(8) 0.140(7) -0.005(7) 0.035(6) 0.017(5) O9N 0.203(9) 0.226(11) 0.158(9) -0.083(9) 0.043(7) -0.027(8) N4N 0.19(2) 0.21(4) 0.117(15) 0.035(15) -0.059(16) -0.08(2) O10N 0.22(2) 0.067(13) 0.24(3) 0.100(15) -0.062(18) 0.005(15) O11N 0.50(6) 0.16(3) 0.14(2) -0.09(2) -0.11(4) 0.07(4) O12N 0.89(8) 0.49(4) 0.74(10) 0.45(6) -0.46(8) -0.562 N5N 0.25(3) 0.12(2) 0.081(16) 0.011(16) 0.016(18) -0.05(2) O13N 0.31(3) 0.055(10) 0.26(2) -0.018(15) -0.13(2) -0.030(13) O14N 0.42(5) 0.058(10) 0.10(2) 0.04(2) 0.11(3) -0.01(3) O15N 0.20(3) 0.28(4) 0.71(8) 0.13(4) -0.22(4) 0.02(2) O11M 0.054(8) 0.144(13) 0.140(13) 0.003(10) 0.033(8) 0.027(8) C1M 0.068(6) 0.119(8) 0.089(7) 0.017(7) 0.017(5) 0.006(6) O2M 0.56(3) 0.241(15) 0.232(14) 0.128(12) -0.050(16) -0.020(16) C2M 0.109(9) 0.245(18) 0.167(13) -0.037(13) 0.042(8) 0.035(10) O3M 0.228(13) 0.37(2) 0.74(4) 0.27(2) -0.269(19) -0.074(13) C3M 0.174(15) 0.32(3) 0.52(4) 0.26(3) 0.14(2) 0.134(16) O4M 0.174(11) 0.53(3) 0.79(4) 0.43(3) 0.147(17) 0.037(15) C4M 0.48(4) 0.092(12) 0.39(3) 0.001(17) 0.09(3) -0.013(17) O5M 0.169(11) 0.35(2) 0.55(3) 0.09(2) 0.133(13) 0.011(12) C5M 0.33(3) 0.178(18) 0.46(3) -0.11(2) 0.20(2) -0.110(19) O1S 0.151(19) 0.43(5) 0.29(3) -0.11(3) 0.016(17) 0.01(2) O2S 0.35(4) 0.47(6) 0.94(10) -0.44(7) -0.40(6) 0.33(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.015(5) . ? Pd1 N6 2.016(5) . ? Pd1 N5 2.017(6) . ? Pd1 N1 2.027(5) . ? Pd2 N7 2.007(6) . ? Pd2 N8 2.008(6) . ? Pd2 N4 2.017(5) . ? Pd2 N3 2.041(6) . ? O1 C25 1.388(7) . ? O1 C6 1.411(6) . ? O2 C31 1.383(7) . ? O2 C12 1.418(7) . ? O3 C37 1.381(7) . ? O3 C18 1.432(7) . ? O4 C44 1.383(7) . ? O4 C24 1.435(8) . ? O5 C30 1.371(7) . ? O5 C49 1.409(7) . ? O6 C26 1.391(7) . ? O6 C52 1.419(7) . ? O7 C36 1.405(7) . ? O7 C52 1.421(7) . ? O8 C32 1.399(7) . ? O8 C51 1.417(7) . ? O9 C38 1.390(7) . ? O9 C49 1.419(7) . ? O10 C50 1.416(7) . ? O10 C42 1.419(7) . ? O11 C45 1.393(7) . ? O11 C50 1.408(7) . ? O12 C43 1.387(7) . ? O12 C51 1.409(7) . ? N1 C1 1.336(8) . ? N1 C5 1.339(8) . ? N2 C7 1.342(7) . ? N2 C11 1.345(8) . ? N3 C17 1.332(8) . ? N3 C13 1.337(8) . ? N4 C23 1.329(7) . ? N4 C19 1.336(8) . ? N5 C61 1.437(10) . ? N6 C62 1.476(9) . ? N7 C63 1.480(12) . ? N8 C64 1.511(11) . ? C1 C2 1.366(8) . ? C2 C3 1.365(9) . ? C2 C6 1.506(9) . ? C3 C4 1.364(10) . ? C4 C5 1.345(9) . ? C7 C8 1.391(8) . ? C8 C9 1.379(9) . ? C8 C12 1.523(8) . ? C9 C10 1.366(9) . ? C10 C11 1.392(9) . ? C13 C14 1.401(9) . ? C14 C15 1.394(9) . ? C14 C18 1.522(9) . ? C15 C16 1.370(9) . ? C16 C17 1.390(9) . ? C19 C20 1.413(8) . ? C20 C21 1.368(8) . ? C20 C24 1.471(8) . ? C21 C22 1.389(9) . ? C22 C23 1.384(9) . ? C25 C30 1.381(8) . ? C25 C26 1.383(8) . ? C26 C27 1.410(8) . ? C27 C28 1.379(8) . ? C27 C56 1.526(8) . ? C28 C29 1.411(8) . ? C29 C30 1.387(8) . ? C29 C53 1.510(8) . ? C31 C32 1.401(8) . ? C31 C36 1.402(8) . ? C32 C33 1.380(8) . ? C33 C34 1.402(7) . ? C33 C55 1.519(8) . ? C34 C35 1.383(8) . ? C35 C36 1.366(8) . ? C35 C56 1.529(8) . ? C37 C38 1.381(8) . ? C37 C42 1.383(8) . ? C38 C39 1.381(8) . ? C39 C40 1.415(8) . ? C39 C53 1.541(8) . ? C40 C41 1.388(8) . ? C41 C42 1.390(8) . ? C41 C54 1.517(8) . ? C43 C48 1.371(8) . ? C43 C44 1.403(9) . ? C44 C45 1.392(9) . ? C45 C46 1.376(9) . ? C46 C47 1.400(8) . ? C46 C54 1.523(8) . ? C47 C48 1.403(8) . ? C48 C55 1.516(8) . ? C53 C57 1.536(8) . ? C54 C58 1.517(9) . ? C55 C59 1.512(8) . ? C56 C60 1.526(8) . ? C61 C62 1.397(11) . ? C63 C64 1.407(13) . ? N1N O3N 1.198(11) . ? N1N O2N 1.217(12) . ? N1N O1N 1.234(11) . ? N2N O5N 1.150(12) . ? N2N O4N 1.169(10) . ? N2N O6N 1.182(12) . ? N3N O7N 1.155(12) . ? N3N O9N 1.223(11) . ? N3N O8N 1.235(10) . ? N4N O10N 1.164(14) . ? N4N O10N 1.164(14) 2_656 ? N4N O12N 1.194(18) 2_656 ? N4N O12N 1.194(18) . ? N4N O11N 1.208(18) 2_656 ? N4N O11N 1.208(18) . ? O10N O11N 1.22(4) 2_656 ? O10N O12N 1.28(5) 2_656 ? O11N O12N 1.06(5) 2_656 ? O11N O10N 1.22(4) 2_656 ? O12N O11N 1.06(5) 2_656 ? O12N O10N 1.28(5) 2_656 ? N5N O15N 1.183(13) . ? N5N O14N 1.193(14) . ? N5N O13N 1.241(13) . ? O11M C1M 1.543(17) . ? O12M C1M 1.484(18) . ? O13M C1M 1.29(4) . ? O2M C2M 1.635(14) . ? O3M C3M 1.632(17) . ? O4M C4M 1.631(17) . ? O5M C5M 1.599(14) . ? 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 N2 Pd1 N6 90.7(2) . . ? N2 Pd1 N5 173.3(2) . . ? N6 Pd1 N5 83.4(2) . . ? N2 Pd1 N1 91.8(2) . . ? N6 Pd1 N1 177.5(2) . . ? N5 Pd1 N1 94.1(2) . . ? N7 Pd2 N8 83.2(3) . . ? N7 Pd2 N4 174.6(3) . . ? N8 Pd2 N4 93.3(3) . . ? N7 Pd2 N3 93.5(3) . . ? N8 Pd2 N3 176.1(3) . . ? N4 Pd2 N3 90.1(2) . . ? C25 O1 C6 118.4(5) . . ? C31 O2 C12 117.1(5) . . ? C37 O3 C18 117.0(5) . . ? C44 O4 C24 116.5(5) . . ? C30 O5 C49 117.3(4) . . ? C26 O6 C52 115.8(4) . . ? C36 O7 C52 116.4(4) . . ? C32 O8 C51 116.7(4) . . ? C38 O9 C49 114.9(4) . . ? C50 O10 C42 116.7(5) . . ? C45 O11 C50 117.1(5) . . ? C43 O12 C51 117.4(4) . . ? C1 N1 C5 115.6(6) . . ? C1 N1 Pd1 120.9(4) . . ? C5 N1 Pd1 123.4(5) . . ? C7 N2 C11 117.8(5) . . ? C7 N2 Pd1 121.9(4) . . ? C11 N2 Pd1 120.0(4) . . ? C17 N3 C13 119.8(6) . . ? C17 N3 Pd2 119.6(5) . . ? C13 N3 Pd2 120.5(5) . . ? C23 N4 C19 118.8(6) . . ? C23 N4 Pd2 119.6(5) . . ? C19 N4 Pd2 121.6(4) . . ? C61 N5 Pd1 110.2(5) . . ? C62 N6 Pd1 108.2(5) . . ? C63 N7 Pd2 111.6(6) . . ? C64 N8 Pd2 109.4(6) . . ? N1 C1 C2 124.4(6) . . ? C3 C2 C1 117.6(7) . . ? C3 C2 C6 120.4(6) . . ? C1 C2 C6 121.9(6) . . ? C4 C3 C2 119.3(7) . . ? C5 C4 C3 119.2(7) . . ? N1 C5 C4 123.8(7) . . ? O1 C6 C2 106.7(5) . . ? N2 C7 C8 122.3(6) . . ? C9 C8 C7 118.4(6) . . ? C9 C8 C12 121.8(6) . . ? C7 C8 C12 119.9(6) . . ? C10 C9 C8 120.5(6) . . ? C9 C10 C11 117.7(7) . . ? N2 C11 C10 123.2(6) . . ? O2 C12 C8 111.9(5) . . ? N3 C13 C14 121.8(6) . . ? C15 C14 C13 118.4(7) . . ? C15 C14 C18 120.0(7) . . ? C13 C14 C18 121.5(6) . . ? C16 C15 C14 118.5(7) . . ? C15 C16 C17 120.3(7) . . ? N3 C17 C16 121.1(7) . . ? O3 C18 C14 108.9(6) . . ? N4 C19 C20 123.2(6) . . ? C21 C20 C19 117.1(6) . . ? C21 C20 C24 123.0(6) . . ? C19 C20 C24 119.9(6) . . ? C20 C21 C22 119.6(6) . . ? C23 C22 C21 119.5(6) . . ? N4 C23 C22 121.7(7) . . ? O4 C24 C20 107.9(5) . . ? C30 C25 C26 121.3(6) . . ? C30 C25 O1 120.5(6) . . ? C26 C25 O1 117.6(6) . . ? C25 C26 O6 119.3(6) . . ? C25 C26 C27 120.0(6) . . ? O6 C26 C27 120.6(6) . . ? C28 C27 C26 118.0(6) . . ? C28 C27 C56 122.9(6) . . ? C26 C27 C56 118.9(6) . . ? C27 C28 C29 122.2(6) . . ? C30 C29 C28 118.5(6) . . ? C30 C29 C53 119.0(6) . . ? C28 C29 C53 122.4(6) . . ? O5 C30 C25 116.9(6) . . ? O5 C30 C29 123.1(6) . . ? C25 C30 C29 119.9(6) . . ? O2 C31 C32 121.2(6) . . ? O2 C31 C36 121.1(6) . . ? C32 C31 C36 117.6(6) . . ? C33 C32 O8 121.6(5) . . ? C33 C32 C31 121.9(6) . . ? O8 C32 C31 116.5(6) . . ? C32 C33 C34 117.3(5) . . ? C32 C33 C55 119.6(5) . . ? C34 C33 C55 122.9(6) . . ? C35 C34 C33 122.9(6) . . ? C36 C35 C34 117.7(6) . . ? C36 C35 C56 121.0(6) . . ? C34 C35 C56 121.1(6) . . ? C35 C36 C31 122.5(6) . . ? C35 C36 O7 122.2(5) . . ? C31 C36 O7 115.2(6) . . ? O3 C37 C38 118.3(6) . . ? O3 C37 C42 122.5(6) . . ? C38 C37 C42 118.7(6) . . ? C39 C38 C37 122.0(6) . . ? C39 C38 O9 120.6(5) . . ? C37 C38 O9 117.2(6) . . ? C38 C39 C40 117.5(5) . . ? C38 C39 C53 120.3(5) . . ? C40 C39 C53 121.9(6) . . ? C41 C40 C39 122.1(6) . . ? C40 C41 C42 117.3(6) . . ? C40 C41 C54 122.3(6) . . ? C42 C41 C54 120.1(6) . . ? C37 C42 C41 122.4(6) . . ? C37 C42 O10 116.8(6) . . ? C41 C42 O10 120.7(6) . . ? C48 C43 O12 121.2(6) . . ? C48 C43 C44 121.7(6) . . ? O12 C43 C44 117.1(6) . . ? O4 C44 C45 118.6(6) . . ? O4 C44 C43 122.7(7) . . ? C45 C44 C43 118.7(6) . . ? C46 C45 C44 122.0(6) . . ? C46 C45 O11 120.8(6) . . ? C44 C45 O11 117.2(6) . . ? C45 C46 C47 117.4(6) . . ? C45 C46 C54 121.2(6) . . ? C47 C46 C54 121.4(6) . . ? C46 C47 C48 122.6(6) . . ? C43 C48 C47 117.6(6) . . ? C43 C48 C55 119.8(6) . . ? C47 C48 C55 122.5(6) . . ? O5 C49 O9 113.1(5) . . ? O11 C50 O10 111.9(6) . . ? O12 C51 O8 114.5(5) . . ? O6 C52 O7 111.7(5) . . ? C29 C53 C57 114.4(5) . . ? C29 C53 C39 108.9(5) . . ? C57 C53 C39 113.7(5) . . ? C58 C54 C41 114.0(5) . . ? C58 C54 C46 114.1(5) . . ? C41 C54 C46 108.2(5) . . ? C59 C55 C48 112.8(6) . . ? C59 C55 C33 113.4(5) . . ? C48 C55 C33 108.5(5) . . ? C60 C56 C27 113.8(6) . . ? C60 C56 C35 112.8(5) . . ? C27 C56 C35 108.8(5) . . ? C62 C61 N5 111.1(8) . . ? C61 C62 N6 113.5(7) . . ? C64 C63 N7 110.7(9) . . ? C63 C64 N8 111.0(9) . . ? O3N N1N O2N 118.8(13) . . ? O3N N1N O1N 119.7(13) . . ? O2N N1N O1N 120.2(14) . . ? O5N N2N O4N 119.2(14) . . ? O5N N2N O6N 125.3(14) . . ? O4N N2N O6N 115.3(14) . . ? O7N N3N O9N 127.0(13) . . ? O7N N3N O8N 120.9(12) . . ? O9N N3N O8N 111.4(13) . . ? O10N N4N O10N 180(3) . 2_656 ? O10N N4N O12N 66(3) . 2_656 ? O10N N4N O12N 114(3) 2_656 2_656 ? O10N N4N O12N 114(3) . . ? O10N N4N O12N 66(3) 2_656 . ? O12N N4N O12N 180(3) 2_656 . ? O10N N4N O11N 62(2) . 2_656 ? O10N N4N O11N 118(2) 2_656 2_656 ? O12N N4N O11N 127(3) 2_656 2_656 ? O12N N4N O11N 53(3) . 2_656 ? O10N N4N O11N 118(2) . . ? O10N N4N O11N 62(2) 2_656 . ? O12N N4N O11N 53(3) 2_656 . ? O12N N4N O11N 127(3) . . ? O11N N4N O11N 180(3) 2_656 . ? N4N O10N O11N 60.7(15) . 2_656 ? N4N O10N O12N 58.3(15) . 2_656 ? O11N O10N O12N 119(2) 2_656 2_656 ? O12N O11N N4N 63(2) 2_656 . ? O12N O11N O10N 120(3) 2_656 2_656 ? N4N O11N O10N 57.2(14) . 2_656 ? O11N O12N N4N 64.4(18) 2_656 . ? O11N O12N O10N 120(3) 2_656 2_656 ? N4N O12N O10N 56.0(16) . 2_656 ? O15N N5N O14N 130(2) . . ? O15N N5N O13N 109.4(19) . . ? O14N N5N O13N 119(2) . . ? O13M C1M O12M 69.5(19) . . ? O13M C1M O11M 39.2(15) . . ? O12M C1M O11M 55.7(13) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.742 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.080