# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'David A. Leigh' _publ_contact_author_email David.Leigh@ed.ac.uk loop_ _publ_author_name D.A.Leigh P.Lusby B.Walker A.Slawin data_3H4 _database_code_depnum_ccdc_archive 'CCDC 874997' #TrackingRef '- 3H4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C93 H113 N7 O12' _chemical_formula_sum 'C93 H113 N7 O12' _chemical_formula_weight 1520.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.663(11) _cell_length_b 11.665(4) _cell_length_c 28.056(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.997(9) _cell_angle_gamma 90.00 _cell_volume 8432(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6175 _cell_measurement_theta_min 21.0 _cell_measurement_theta_max 69.0 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8464 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112492 _diffrn_reflns_av_R_equivalents 0.1994 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 67.20 _reflns_number_total 14994 _reflns_number_gt 8642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. The NH hydrogen atoms were located from a difference map and refined isotropically subject to a distance restraint. ; _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^)+(0.2000P)^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 14994 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.1259 _refine_ls_wR_factor_ref 0.4100 _refine_ls_wR_factor_gt 0.3598 _refine_ls_goodness_of_fit_ref 1.288 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.006 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 0.8116(3) 1.7766(5) 0.5035(2) 0.0992(17) Uani 1 1 d . . . H1A H 0.7977 1.7134 0.4775 0.119 Uiso 1 1 calc R . . H1B H 0.8499 1.7746 0.5182 0.119 Uiso 1 1 calc R . . N2 N 0.79676(19) 1.7570(4) 0.54663(18) 0.0905(12) Uani 1 1 d D . . H2N H 0.7637(12) 1.716(5) 0.531(2) 0.13(2) Uiso 1 1 d D . . C3 C 0.8292(2) 1.7792(5) 0.5974(2) 0.0904(14) Uani 1 1 d . . . O3 O 0.87303(16) 1.8198(4) 0.61246(18) 0.1178(13) Uani 1 1 d . . . C4 C 0.8085(2) 1.7498(4) 0.6368(2) 0.0820(13) Uani 1 1 d . . . N5 N 0.76298(15) 1.6937(3) 0.61744(14) 0.0719(9) Uani 1 1 d . . . C6 C 0.74377(18) 1.6695(4) 0.65189(18) 0.0746(12) Uani 1 1 d . . . C7 C 0.7674(2) 1.7030(5) 0.70454(19) 0.0876(14) Uani 1 1 d . . . H7A H 0.7512 1.6875 0.7270 0.105 Uiso 1 1 calc R . . C8 C 0.8144(2) 1.7589(5) 0.7243(2) 0.1048(18) Uani 1 1 d . . . H8A H 0.8315 1.7812 0.7605 0.126 Uiso 1 1 calc R . . C9 C 0.8357(2) 1.7813(5) 0.6898(2) 0.0969(16) Uani 1 1 d . . . H9A H 0.8685 1.8179 0.7020 0.116 Uiso 1 1 calc R . . C10 C 0.69436(18) 1.5989(4) 0.63123(17) 0.0716(11) Uani 1 1 d . . . O10 O 0.67255(13) 1.5792(3) 0.65995(12) 0.0825(9) Uani 1 1 d . . . N11 N 0.67854(15) 1.5574(3) 0.58243(14) 0.0744(10) Uani 1 1 d D . . H11N H 0.6963(15) 1.574(4) 0.5603(15) 0.084(14) Uiso 1 1 d D . . C12 C 0.63388(19) 1.4801(4) 0.55712(18) 0.0788(13) Uani 1 1 d . . . H12A H 0.6270 1.4425 0.5850 0.095 Uiso 1 1 calc R . . H12B H 0.6428 1.4194 0.5378 0.095 Uiso 1 1 calc R . . C13 C 0.58508(18) 1.5403(4) 0.51883(16) 0.0707(11) Uani 1 1 d . . . C14 C 0.55581(19) 1.6065(4) 0.53663(18) 0.0772(12) Uani 1 1 d . . . H14A H 0.5659 1.6119 0.5736 0.093 Uiso 1 1 calc R . . C15 C 0.51204(18) 1.6653(4) 0.50150(17) 0.0728(12) Uani 1 1 d . . . H15A H 0.4925 1.7103 0.5145 0.087 Uiso 1 1 calc R . . C16 C 0.49707(18) 1.6578(4) 0.44742(17) 0.0695(11) Uani 1 1 d . . . C17 C 0.52568(19) 1.5910(4) 0.42892(17) 0.0730(12) Uani 1 1 d . . . H17A H 0.5150 1.5848 0.3918 0.088 Uiso 1 1 calc R . . C18 C 0.56959(19) 1.5331(4) 0.46383(16) 0.0730(12) Uani 1 1 d . . . H18A H 0.5892 1.4887 0.4507 0.088 Uiso 1 1 calc R . . O19 O 0.45376(12) 1.7081(3) 0.40898(11) 0.0800(9) Uani 1 1 d . . . C20 C 0.4294(2) 1.8009(4) 0.4235(2) 0.0861(14) Uani 1 1 d . . . H20A H 0.4226 1.7759 0.4536 0.103 Uiso 1 1 calc R . . H20B H 0.3955 1.8177 0.3933 0.103 Uiso 1 1 calc R . . C21 C 0.4607(2) 1.9084(4) 0.43876(18) 0.0822(13) Uani 1 1 d . . . H21A H 0.4932 1.8935 0.4710 0.099 Uiso 1 1 calc R . . H21B H 0.4410 1.9676 0.4477 0.099 Uiso 1 1 calc R . . C22 C 0.4745(2) 1.9558(4) 0.39526(18) 0.0836(13) Uani 1 1 d . . . H22A H 0.4975 1.9009 0.3890 0.100 Uiso 1 1 calc R . . H22B H 0.4424 1.9640 0.3618 0.100 Uiso 1 1 calc R . . C23 C 0.5014(2) 2.0711(4) 0.41099(19) 0.0886(14) Uani 1 1 d . . . H23A H 0.4756 2.1279 0.4109 0.106 Uiso 1 1 calc R . . H23B H 0.5287 2.0652 0.4479 0.106 Uiso 1 1 calc R . . C24 C 0.5257(2) 2.1170(5) 0.3774(2) 0.0907(14) Uani 1 1 d . . . H24A H 0.4989 2.1217 0.3402 0.109 Uiso 1 1 calc R . . H24B H 0.5527 2.0627 0.3786 0.109 Uiso 1 1 calc R . . C25 C 0.5500(2) 2.2340(4) 0.3947(2) 0.0903(15) Uani 1 1 d . . . H25A H 0.5744 2.2303 0.4328 0.108 Uiso 1 1 calc R . . H25B H 0.5222 2.2890 0.3908 0.108 Uiso 1 1 calc R . . C26 C 0.5792(2) 2.2812(4) 0.3645(2) 0.0950(16) Uani 1 1 d . . . H26A H 0.5548 2.2841 0.3263 0.114 Uiso 1 1 calc R . . H26B H 0.5897 2.3610 0.3764 0.114 Uiso 1 1 calc R . . C27 C 0.6272(2) 2.2145(5) 0.3707(2) 0.0999(16) Uani 1 1 d . . . H27A H 0.6497 2.2017 0.4089 0.120 Uiso 1 1 calc R . . H27B H 0.6164 2.1385 0.3536 0.120 Uiso 1 1 calc R . . C28 C 0.6581(3) 2.2770(5) 0.3461(2) 0.1004(17) Uani 1 1 d . . . H28A H 0.6340 2.2985 0.3094 0.120 Uiso 1 1 calc R . . H28B H 0.6718 2.3489 0.3661 0.120 Uiso 1 1 calc R . . C29 C 0.7022(3) 2.2131(5) 0.3446(2) 0.1037(18) Uani 1 1 d . . . H29A H 0.6902 2.1362 0.3291 0.124 Uiso 1 1 calc R . . H29B H 0.7148 2.2543 0.3217 0.124 Uiso 1 1 calc R . . O30 O 0.74400(16) 2.2010(3) 0.39702(15) 0.1011(11) Uani 1 1 d . . . C31 C 0.7569(2) 2.0956(5) 0.4207(2) 0.0858(14) Uani 1 1 d . . . C32 C 0.8055(2) 2.0905(5) 0.4635(2) 0.0976(16) Uani 1 1 d . . . H32A H 0.8269 2.1567 0.4740 0.117 Uiso 1 1 calc R . . C33 C 0.8226(2) 1.9886(5) 0.4908(2) 0.0966(16) Uani 1 1 d . . . H33A H 0.8555 1.9864 0.5208 0.116 Uiso 1 1 calc R . . C34 C 0.7925(2) 1.8880(5) 0.4753(2) 0.0921(16) Uani 1 1 d . . . C35 C 0.7438(2) 1.8981(5) 0.4328(2) 0.0907(15) Uani 1 1 d . . . H35A H 0.7217 1.8330 0.4222 0.109 Uiso 1 1 calc R . . C36 C 0.7267(2) 1.9985(5) 0.4059(2) 0.0901(15) Uani 1 1 d . . . H36A H 0.6935 2.0014 0.3765 0.108 Uiso 1 1 calc R . . C37 C 0.6532(2) 2.0224(5) 0.5111(2) 0.0916(15) Uani 1 1 d . . . H37A H 0.6341 2.0959 0.5046 0.110 Uiso 1 1 calc R . . H37B H 0.6624 2.0102 0.4814 0.110 Uiso 1 1 calc R . . O38 O 0.62008(15) 1.9343(3) 0.51062(16) 0.1046(11) Uani 1 1 d . . . C39 C 0.6422(2) 1.8211(4) 0.5178(2) 0.0913(15) Uani 1 1 d . . . H39A H 0.6219 1.7696 0.5298 0.110 Uiso 1 1 calc R . . H39B H 0.6780 1.8242 0.5465 0.110 Uiso 1 1 calc R . . C40 C 0.6437(2) 1.7698(5) 0.46974(19) 0.0844(14) Uani 1 1 d . . . N41 N 0.67773(17) 1.6822(4) 0.48006(15) 0.0822(11) Uani 1 1 d . . . C42 C 0.6773(2) 1.6219(5) 0.4389(2) 0.0946(16) Uani 1 1 d . . . C43 C 0.6452(3) 1.6522(7) 0.3860(2) 0.117(2) Uani 1 1 d . . . H43A H 0.6457 1.6093 0.3574 0.141 Uiso 1 1 calc R . . C44 C 0.6128(3) 1.7463(7) 0.3766(2) 0.121(2) Uani 1 1 d . . . H44A H 0.5914 1.7704 0.3413 0.145 Uiso 1 1 calc R . . C45 C 0.6118(3) 1.8036(5) 0.4181(2) 0.1098(19) Uani 1 1 d . . . H45A H 0.5893 1.8673 0.4119 0.132 Uiso 1 1 calc R . . C46 C 0.7155(3) 1.5283(5) 0.4547(3) 0.114(2) Uani 1 1 d . . . H46A H 0.7194 1.5004 0.4233 0.137 Uiso 1 1 calc R . . H46B H 0.7496 1.5570 0.4810 0.137 Uiso 1 1 calc R . . O47 O 0.69912(18) 1.4371(4) 0.47707(17) 0.1117(12) Uani 1 1 d . . . C48 C 0.7357(3) 1.3489(6) 0.4993(3) 0.125(2) Uani 1 1 d . . . H48A H 0.7511 1.3299 0.4749 0.150 Uiso 1 1 calc R . . H48B H 0.7179 1.2795 0.5034 0.150 Uiso 1 1 calc R . . C49 C 0.7781(3) 1.3819(6) 0.5523(3) 0.1082(18) Uani 1 1 d . . . C50 C 0.8230(4) 1.4375(8) 0.5592(3) 0.147(3) Uani 1 1 d . . . H50A H 0.8278 1.4530 0.5283 0.176 Uiso 1 1 calc R . . C51 C 0.8612(3) 1.4720(8) 0.6064(3) 0.140(3) Uani 1 1 d . . . H51A H 0.8907 1.5118 0.6081 0.168 Uiso 1 1 calc R . . C52 C 0.8559(3) 1.4477(6) 0.6525(3) 0.118(2) Uani 1 1 d . . . C53 C 0.8097(3) 1.3948(5) 0.6470(3) 0.1085(19) Uani 1 1 d . . . H53A H 0.8043 1.3803 0.6775 0.130 Uiso 1 1 calc R . . C54 C 0.7717(3) 1.3635(5) 0.5970(3) 0.1141(19) Uani 1 1 d . . . H54A H 0.7406 1.3284 0.5940 0.137 Uiso 1 1 calc R . . O55 O 0.8951(2) 1.4824(4) 0.69893(19) 0.1264(14) Uani 1 1 d . . . C56 C 0.8917(3) 1.4491(8) 0.7445(3) 0.142(3) Uani 1 1 d . . . H56A H 0.8842 1.3659 0.7430 0.171 Uiso 1 1 calc R . . H56B H 0.8630 1.4908 0.7475 0.171 Uiso 1 1 calc R . . C57 C 0.9408(4) 1.4741(8) 0.7907(3) 0.146(3) Uani 1 1 d . . . H57A H 0.9692 1.4417 0.7838 0.175 Uiso 1 1 calc R . . H57B H 0.9408 1.4322 0.8214 0.175 Uiso 1 1 calc R . . C58 C 0.9536(3) 1.5940(7) 0.8064(2) 0.126(2) Uani 1 1 d . . . H58A H 0.9227 1.6313 0.8068 0.151 Uiso 1 1 calc R . . H58B H 0.9609 1.6330 0.7791 0.151 Uiso 1 1 calc R . . C59 C 0.9993(3) 1.6121(6) 0.8599(3) 0.123(2) Uani 1 1 d . . . H59A H 1.0313 1.5922 0.8566 0.148 Uiso 1 1 calc R . . H59B H 0.9961 1.5570 0.8852 0.148 Uiso 1 1 calc R . . C60 C 1.0064(3) 1.7299(6) 0.8840(3) 0.116(2) Uani 1 1 d . . . H60A H 1.0128 1.7845 0.8605 0.139 Uiso 1 1 calc R . . H60B H 0.9736 1.7528 0.8850 0.139 Uiso 1 1 calc R . . C61 C 1.0504(3) 1.7410(6) 0.9397(3) 0.120(2) Uani 1 1 d . . . H61A H 1.0453 1.6819 0.9623 0.144 Uiso 1 1 calc R . . H61B H 1.0834 1.7230 0.9380 0.144 Uiso 1 1 calc R . . C62 C 1.0564(3) 1.8533(6) 0.9664(3) 0.117(2) Uani 1 1 d . . . H62A H 1.0236 1.8721 0.9683 0.140 Uiso 1 1 calc R . . H62B H 1.0623 1.9128 0.9444 0.140 Uiso 1 1 calc R . . C63 C 1.1012(3) 1.8581(6) 1.0226(3) 0.121(2) Uani 1 1 d . . . H63A H 1.0919 1.8105 1.0463 0.146 Uiso 1 1 calc R . . H63B H 1.1325 1.8241 1.0219 0.146 Uiso 1 1 calc R . . C64 C 1.1139(2) 1.9745(5) 1.0448(2) 0.1076(18) Uani 1 1 d . . . H64A H 1.0845 2.0050 1.0506 0.129 Uiso 1 1 calc R . . H64B H 1.1190 2.0253 1.0193 0.129 Uiso 1 1 calc R . . C65 C 1.1626(3) 1.9746(6) 1.0970(2) 0.1098(18) Uani 1 1 d . . . H65A H 1.1547 1.9439 1.1255 0.132 Uiso 1 1 calc R . . H65B H 1.1893 1.9250 1.0941 0.132 Uiso 1 1 calc R . . O66 O 1.18111(15) 2.0852(3) 1.10899(15) 0.1047(11) Uani 1 1 d . . . C67 C 1.2274(2) 2.1028(4) 1.15408(19) 0.0835(13) Uani 1 1 d . . . C68 C 1.2549(2) 2.0178(4) 1.1895(2) 0.0911(15) Uani 1 1 d . . . H68A H 1.2427 1.9409 1.1839 0.109 Uiso 1 1 calc R . . C69 C 1.3003(2) 2.0458(4) 1.2332(2) 0.0870(14) Uani 1 1 d . . . H69A H 1.3191 1.9873 1.2576 0.104 Uiso 1 1 calc R . . C70 C 1.31907(19) 2.1555(4) 1.24236(18) 0.0770(12) Uani 1 1 d . . . C71 C 1.2913(2) 2.2401(4) 1.20624(19) 0.0840(14) Uani 1 1 d . . . H71A H 1.3035 2.3170 1.2118 0.101 Uiso 1 1 calc R . . C72 C 1.2457(2) 2.2125(4) 1.1620(2) 0.0835(13) Uani 1 1 d . . . H72A H 1.2271 2.2704 1.1371 0.100 Uiso 1 1 calc R . . C73 C 1.3686(2) 2.1809(4) 1.2921(2) 0.0895(15) Uani 1 1 d . . . H73A H 1.3624 2.1655 1.3235 0.107 Uiso 1 1 calc R . . H73B H 1.3961 2.1277 1.2935 0.107 Uiso 1 1 calc R . . N74 N 1.38728(17) 2.2973(3) 1.29536(16) 0.0825(11) Uani 1 1 d D . . H74N H 1.3774(19) 2.359(3) 1.3128(19) 0.104(17) Uiso 1 1 d D . . C75 C 1.4209(2) 2.3259(5) 1.27614(18) 0.0811(13) Uani 1 1 d . . . O75 O 1.43994(16) 2.2566(3) 1.25636(14) 0.1026(11) Uani 1 1 d . . . C76 C 1.43354(18) 2.4501(4) 1.27892(16) 0.0731(12) Uani 1 1 d . . . N77 N 1.40227(14) 2.5221(3) 1.28848(13) 0.0681(9) Uani 1 1 d . . . C78 C 1.41129(18) 2.6341(4) 1.28903(15) 0.0706(11) Uani 1 1 d . . . C79 C 1.4518(2) 2.6782(5) 1.28190(18) 0.0865(14) Uani 1 1 d . . . H79A H 1.4576 2.7586 1.2836 0.104 Uiso 1 1 calc R . . C80 C 1.4843(2) 2.6040(6) 1.27213(19) 0.0903(15) Uani 1 1 d . . . H80A H 1.5130 2.6327 1.2673 0.108 Uiso 1 1 calc R . . C81 C 1.4747(2) 2.4890(5) 1.26961(18) 0.0869(14) Uani 1 1 d . . . H81A H 1.4956 2.4366 1.2616 0.104 Uiso 1 1 calc R . . C82 C 1.3716(2) 2.7124(4) 1.29421(16) 0.0764(13) Uani 1 1 d . . . O82 O 1.37085(14) 2.8148(3) 1.28534(12) 0.0907(10) Uani 1 1 d . . . N83 N 1.33776(15) 2.6573(3) 1.30724(14) 0.0756(10) Uani 1 1 d D . . H83N H 1.3400(19) 2.5734(6) 1.3072(19) 0.096(15) Uiso 1 1 d D . . C84 C 1.2887(2) 2.7084(5) 1.2999(2) 0.0870(14) Uani 1 1 d . . . H84A H 1.2911 2.7928 1.2981 0.104 Uiso 1 1 calc R . . H84B H 1.2823 2.6899 1.3310 0.104 Uiso 1 1 calc R . . C85 C 1.24373(19) 2.6660(4) 1.25025(18) 0.0754(12) Uani 1 1 d . . . C86 C 1.2006(2) 2.7328(4) 1.2239(2) 0.0858(14) Uani 1 1 d . . . H86A H 1.1986 2.8065 1.2372 0.103 Uiso 1 1 calc R . . C87 C 1.1596(2) 2.6934(5) 1.1778(2) 0.0923(15) Uani 1 1 d . . . H87A H 1.1311 2.7431 1.1591 0.111 Uiso 1 1 calc R . . C88 C 1.15895(19) 2.5868(4) 1.15863(19) 0.0764(12) Uani 1 1 d . . . C89 C 1.2013(2) 2.5163(4) 1.1855(2) 0.0898(14) Uani 1 1 d . . . H89A H 1.2019 2.4406 1.1732 0.108 Uiso 1 1 calc R . . C90 C 1.2432(2) 2.5575(4) 1.23079(19) 0.0864(14) Uani 1 1 d . . . H90A H 1.2723 2.5090 1.2488 0.104 Uiso 1 1 calc R . . O91 O 1.11626(13) 2.5546(3) 1.11367(13) 0.0897(10) Uani 1 1 d . . . C92 C 1.11547(19) 2.4424(4) 1.09397(18) 0.0804(13) Uani 1 1 d . . . H92A H 1.1131 2.3853 1.1189 0.096 Uiso 1 1 calc R . . H92B H 1.1478 2.4281 1.0904 0.096 Uiso 1 1 calc R . . C93 C 1.0692(2) 2.4311(5) 1.0407(2) 0.0921(15) Uani 1 1 d . . . H93A H 1.0722 2.4880 1.0159 0.110 Uiso 1 1 calc R . . H93B H 1.0372 2.4483 1.0445 0.110 Uiso 1 1 calc R . . C94 C 1.0650(2) 2.3109(5) 1.0173(2) 0.0975(16) Uani 1 1 d . . . H94A H 1.0997 2.2863 1.0216 0.117 Uiso 1 1 calc R . . H94B H 1.0537 2.2567 1.0373 0.117 Uiso 1 1 calc R . . C95 C 1.0271(3) 2.3051(6) 0.9589(2) 0.120(2) Uani 1 1 d . . . H95A H 0.9919 2.3236 0.9552 0.144 Uiso 1 1 calc R . . H95B H 1.0367 2.3644 0.9396 0.144 Uiso 1 1 calc R . . C96 C 1.0252(3) 2.1910(6) 0.9336(2) 0.126(2) Uani 1 1 d . . . H96A H 1.0144 2.1320 0.9521 0.152 Uiso 1 1 calc R . . H96B H 1.0605 2.1712 0.9383 0.152 Uiso 1 1 calc R . . C97 C 0.9883(4) 2.1877(9) 0.8748(4) 0.178(4) Uani 1 1 d DU . . H97A H 0.9992 2.2476 0.8567 0.214 Uiso 1 1 calc R . . H97B H 0.9532 2.2082 0.8705 0.214 Uiso 1 1 calc R . . C98 C 0.9845(4) 2.0711(9) 0.8456(4) 0.186(4) Uani 1 1 d DU . . H98A H 0.9932 2.0111 0.8732 0.223 Uiso 1 1 calc R . . H98B H 1.0134 2.0717 0.8353 0.223 Uiso 1 1 calc R . . C99 C 0.9343(5) 2.0229(13) 0.7941(5) 0.245(6) Uani 1 1 d DU . . H99A H 0.9414 1.9506 0.7800 0.294 Uiso 1 1 calc R . . H99B H 0.9031 2.0147 0.8004 0.294 Uiso 1 1 calc R . . C100 C 0.9322(5) 2.1241(11) 0.7615(4) 0.208(4) Uani 1 1 d DU . . H10E H 0.9667 2.1412 0.7630 0.250 Uiso 1 1 calc R . . H10F H 0.9194 2.1926 0.7729 0.250 Uiso 1 1 calc R . . C101 C 0.8897(4) 2.0812(9) 0.7002(4) 0.168(3) Uani 1 1 d DU . . H10G H 0.8871 2.1397 0.6735 0.202 Uiso 1 1 calc R . . H10H H 0.9013 2.0081 0.6909 0.202 Uiso 1 1 calc R . . O102 O 0.8385(2) 2.0658(4) 0.70117(15) 0.1293(15) Uani 1 1 d . . . C103 C 0.7943(3) 2.0523(5) 0.6530(2) 0.0989(17) Uani 1 1 d . . . C104 C 0.7490(3) 2.0307(5) 0.6565(2) 0.1016(17) Uani 1 1 d . . . H10A H 0.7492 2.0220 0.6902 0.122 Uiso 1 1 calc R . . C105 C 0.7028(2) 2.0214(5) 0.6109(2) 0.0955(15) Uani 1 1 d . . . H10B H 0.6714 2.0070 0.6135 0.115 Uiso 1 1 calc R . . C106 C 0.7023(2) 2.0331(4) 0.56134(19) 0.0797(13) Uani 1 1 d . . . C107 C 0.7481(2) 2.0510(4) 0.5594(2) 0.0885(14) Uani 1 1 d . . . H10C H 0.7487 2.0551 0.5258 0.106 Uiso 1 1 calc R . . C108 C 0.7941(2) 2.0635(4) 0.60483(19) 0.0905(15) Uani 1 1 d . . . H10D H 0.8254 2.0798 0.6023 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.123(4) 0.101(4) 0.101(4) -0.004(3) 0.075(4) -0.008(3) N2 0.106(3) 0.100(3) 0.084(3) -0.007(2) 0.058(3) -0.012(3) C3 0.093(4) 0.090(3) 0.095(4) -0.001(3) 0.049(3) -0.003(3) O3 0.095(3) 0.139(3) 0.126(3) -0.010(3) 0.054(2) -0.021(2) C4 0.089(3) 0.083(3) 0.072(3) 0.004(2) 0.033(3) -0.001(3) N5 0.082(3) 0.070(2) 0.066(2) 0.0010(17) 0.034(2) 0.0012(19) C6 0.084(3) 0.074(3) 0.062(3) -0.001(2) 0.028(2) -0.002(2) C7 0.098(4) 0.101(4) 0.059(3) -0.008(2) 0.031(3) -0.005(3) C8 0.116(5) 0.117(4) 0.068(3) -0.012(3) 0.028(3) -0.022(4) C9 0.090(4) 0.104(4) 0.081(3) -0.003(3) 0.024(3) -0.013(3) C10 0.084(3) 0.071(3) 0.058(2) 0.003(2) 0.030(2) 0.004(2) O10 0.104(2) 0.086(2) 0.0673(18) -0.0025(15) 0.0459(18) -0.0080(17) N11 0.082(2) 0.080(2) 0.055(2) -0.0043(17) 0.0245(19) -0.0085(19) C12 0.101(3) 0.065(3) 0.073(3) 0.003(2) 0.041(3) -0.003(2) C13 0.089(3) 0.068(3) 0.056(2) -0.004(2) 0.032(2) -0.011(2) C14 0.091(3) 0.088(3) 0.058(2) -0.010(2) 0.037(3) -0.013(3) C15 0.082(3) 0.079(3) 0.059(2) -0.009(2) 0.032(2) -0.010(2) C16 0.079(3) 0.066(3) 0.061(2) -0.008(2) 0.029(2) -0.010(2) C17 0.091(3) 0.072(3) 0.057(2) -0.005(2) 0.033(2) -0.006(2) C18 0.094(3) 0.075(3) 0.059(2) -0.010(2) 0.041(2) -0.010(2) O19 0.087(2) 0.086(2) 0.0618(18) -0.0141(15) 0.0274(16) 0.0016(17) C20 0.093(3) 0.086(3) 0.081(3) -0.005(2) 0.039(3) 0.006(3) C21 0.102(3) 0.075(3) 0.063(3) -0.011(2) 0.030(3) -0.013(3) C22 0.099(3) 0.085(3) 0.061(3) -0.001(2) 0.030(2) 0.002(3) C23 0.104(4) 0.090(3) 0.068(3) -0.002(2) 0.035(3) 0.002(3) C24 0.105(4) 0.094(4) 0.073(3) 0.003(3) 0.039(3) 0.000(3) C25 0.111(4) 0.090(3) 0.070(3) 0.000(2) 0.039(3) -0.006(3) C26 0.134(5) 0.079(3) 0.068(3) -0.001(2) 0.040(3) -0.001(3) C27 0.120(4) 0.096(4) 0.086(4) 0.002(3) 0.047(3) -0.002(3) C28 0.129(5) 0.101(4) 0.078(3) -0.012(3) 0.051(3) -0.025(4) C29 0.136(5) 0.110(4) 0.073(3) -0.004(3) 0.053(4) -0.015(4) O30 0.129(3) 0.089(2) 0.086(2) -0.0120(19) 0.048(2) -0.020(2) C31 0.118(4) 0.080(3) 0.076(3) -0.010(3) 0.058(3) -0.016(3) C32 0.114(4) 0.091(4) 0.101(4) -0.012(3) 0.060(4) -0.018(3) C33 0.105(4) 0.110(4) 0.085(3) -0.014(3) 0.051(3) -0.020(3) C34 0.123(5) 0.089(4) 0.090(4) -0.016(3) 0.071(4) -0.026(3) C35 0.120(4) 0.085(4) 0.086(4) -0.015(3) 0.063(4) -0.025(3) C36 0.123(4) 0.088(4) 0.072(3) -0.018(3) 0.054(3) -0.027(3) C37 0.100(4) 0.076(3) 0.090(4) 0.014(3) 0.033(3) 0.003(3) O38 0.103(3) 0.091(3) 0.113(3) 0.007(2) 0.041(2) 0.002(2) C39 0.107(4) 0.072(3) 0.096(4) 0.012(3) 0.045(3) 0.009(3) C40 0.096(3) 0.082(3) 0.069(3) 0.011(2) 0.031(3) -0.017(3) N41 0.107(3) 0.079(3) 0.064(2) -0.0088(19) 0.041(2) -0.016(2) C42 0.131(5) 0.091(4) 0.080(3) -0.015(3) 0.063(3) -0.026(3) C43 0.155(6) 0.138(6) 0.056(3) -0.011(3) 0.043(4) -0.058(5) C44 0.136(6) 0.140(6) 0.065(4) 0.015(4) 0.023(4) -0.045(5) C45 0.125(5) 0.103(4) 0.077(4) 0.022(3) 0.022(3) -0.025(3) C46 0.171(6) 0.096(4) 0.121(5) -0.037(4) 0.107(5) -0.046(4) O47 0.140(3) 0.096(3) 0.114(3) -0.010(2) 0.069(3) -0.004(3) C48 0.143(6) 0.111(5) 0.121(5) -0.023(4) 0.058(5) 0.014(4) C49 0.116(5) 0.117(5) 0.114(5) -0.014(4) 0.072(4) 0.007(4) C50 0.164(8) 0.191(8) 0.109(6) -0.010(5) 0.080(6) 0.030(7) C51 0.131(6) 0.209(8) 0.101(5) -0.025(5) 0.069(5) -0.023(5) C52 0.128(5) 0.133(5) 0.086(4) -0.007(4) 0.042(4) 0.017(4) C53 0.132(5) 0.090(4) 0.136(6) 0.015(4) 0.088(5) 0.007(4) C54 0.140(6) 0.090(4) 0.113(5) -0.009(3) 0.055(5) -0.013(4) O55 0.152(4) 0.143(4) 0.098(3) 0.003(3) 0.068(3) 0.000(3) C56 0.147(7) 0.154(7) 0.130(6) 0.028(5) 0.064(6) 0.012(5) C57 0.170(7) 0.159(7) 0.103(5) -0.022(5) 0.055(5) -0.016(6) C58 0.142(6) 0.148(6) 0.086(4) -0.022(4) 0.048(4) -0.023(5) C59 0.133(5) 0.136(6) 0.098(4) -0.012(4) 0.047(4) -0.009(4) C60 0.124(5) 0.104(4) 0.109(5) -0.012(4) 0.040(4) -0.012(4) C61 0.121(5) 0.137(6) 0.101(4) -0.012(4) 0.047(4) -0.007(4) C62 0.115(4) 0.108(4) 0.105(4) -0.016(4) 0.028(4) -0.017(4) C63 0.128(5) 0.112(5) 0.097(4) -0.004(3) 0.024(4) -0.006(4) C64 0.107(4) 0.114(5) 0.090(4) -0.014(3) 0.032(3) -0.008(3) C65 0.117(5) 0.104(4) 0.100(4) -0.011(3) 0.041(4) -0.005(4) O66 0.113(3) 0.089(3) 0.089(2) -0.0057(19) 0.023(2) -0.011(2) C67 0.095(3) 0.083(3) 0.072(3) -0.002(2) 0.036(3) 0.001(3) C68 0.106(4) 0.071(3) 0.081(3) 0.004(2) 0.027(3) -0.003(3) C69 0.115(4) 0.063(3) 0.083(3) 0.009(2) 0.043(3) 0.005(3) C70 0.094(3) 0.060(3) 0.074(3) 0.003(2) 0.034(3) 0.003(2) C71 0.109(4) 0.062(3) 0.073(3) 0.005(2) 0.033(3) 0.003(2) C72 0.099(4) 0.072(3) 0.080(3) 0.011(2) 0.039(3) 0.011(3) C73 0.101(4) 0.064(3) 0.086(3) 0.001(2) 0.025(3) -0.002(2) N74 0.097(3) 0.071(3) 0.080(3) -0.0040(19) 0.039(2) -0.004(2) C75 0.087(3) 0.088(3) 0.064(3) 0.002(2) 0.028(3) 0.016(3) O75 0.119(3) 0.100(3) 0.087(2) -0.0101(19) 0.044(2) 0.025(2) C76 0.072(3) 0.088(3) 0.052(2) 0.003(2) 0.021(2) 0.000(2) N77 0.074(2) 0.072(2) 0.0517(18) -0.0004(15) 0.0215(17) 0.0012(18) C78 0.084(3) 0.075(3) 0.049(2) 0.0049(19) 0.026(2) -0.004(2) C79 0.093(4) 0.093(3) 0.062(3) 0.012(2) 0.023(3) -0.009(3) C80 0.081(3) 0.120(5) 0.067(3) 0.018(3) 0.030(3) -0.008(3) C81 0.082(3) 0.115(4) 0.063(3) 0.007(3) 0.032(2) 0.011(3) C82 0.095(3) 0.068(3) 0.055(2) -0.005(2) 0.023(2) -0.004(3) O82 0.121(3) 0.064(2) 0.074(2) 0.0055(15) 0.0295(19) 0.0011(17) N83 0.082(3) 0.068(2) 0.073(2) -0.0019(18) 0.030(2) -0.004(2) C84 0.087(3) 0.086(3) 0.082(3) -0.008(2) 0.033(3) 0.006(3) C85 0.087(3) 0.073(3) 0.068(3) -0.002(2) 0.037(2) 0.003(2) C86 0.090(3) 0.075(3) 0.087(3) -0.008(2) 0.034(3) 0.006(3) C87 0.096(4) 0.084(3) 0.093(4) 0.003(3) 0.038(3) 0.018(3) C88 0.075(3) 0.077(3) 0.071(3) -0.003(2) 0.027(2) 0.004(2) C89 0.102(4) 0.078(3) 0.078(3) -0.010(2) 0.029(3) 0.005(3) C90 0.095(3) 0.075(3) 0.073(3) -0.012(2) 0.021(3) 0.009(3) O91 0.085(2) 0.094(2) 0.080(2) -0.0093(17) 0.0271(18) 0.0064(17) C92 0.084(3) 0.087(3) 0.065(3) -0.006(2) 0.028(2) 0.001(3) C93 0.087(3) 0.103(4) 0.085(3) -0.012(3) 0.036(3) 0.005(3) C94 0.086(3) 0.121(4) 0.078(3) -0.016(3) 0.028(3) 0.003(3) C95 0.128(5) 0.132(5) 0.082(4) -0.022(3) 0.030(4) 0.019(4) C96 0.104(4) 0.152(6) 0.083(4) -0.029(4) 0.004(3) 0.029(4) C97 0.178(4) 0.178(4) 0.178(4) -0.0021(10) 0.0769(18) 0.0026(10) C98 0.186(4) 0.185(4) 0.185(4) -0.0020(10) 0.0801(19) 0.0012(10) C99 0.245(6) 0.245(6) 0.245(6) -0.0004(10) 0.107(3) -0.0001(10) C100 0.209(4) 0.208(4) 0.208(4) -0.0003(10) 0.091(2) 0.0002(10) C101 0.168(3) 0.169(3) 0.168(3) 0.0002(10) 0.0730(17) -0.0009(10) O102 0.155(4) 0.140(3) 0.070(2) -0.011(2) 0.028(2) 0.008(3) C103 0.122(5) 0.093(4) 0.064(3) -0.010(3) 0.025(3) 0.011(3) C104 0.132(5) 0.105(4) 0.079(4) -0.007(3) 0.057(4) 0.017(4) C105 0.112(4) 0.087(3) 0.093(4) -0.005(3) 0.050(4) 0.005(3) C106 0.098(4) 0.069(3) 0.071(3) -0.001(2) 0.036(3) 0.006(2) C107 0.112(4) 0.081(3) 0.074(3) -0.006(2) 0.042(3) -0.002(3) C108 0.104(4) 0.090(3) 0.067(3) -0.009(2) 0.028(3) -0.003(3) _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 N2 1.464(6) . ? C1 C34 1.495(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C3 1.342(7) . ? N2 H2N 0.979(5) . ? C3 O3 1.230(6) . ? C3 C4 1.506(8) . ? C4 N5 1.343(6) . ? C4 C9 1.392(7) . ? N5 C6 1.336(6) . ? C6 C7 1.385(6) . ? C6 C10 1.516(7) . ? C7 C8 1.374(8) . ? C7 H7A 0.9500 . ? C8 C9 1.379(8) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 O10 1.239(5) . ? C10 N11 1.331(5) . ? N11 C12 1.469(6) . ? N11 H11N 0.979(5) . ? C12 C13 1.512(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.384(6) . ? C13 C18 1.409(6) . ? C14 C15 1.390(7) . ? C14 H14A 0.9500 . ? C15 C16 1.387(6) . ? C15 H15A 0.9500 . ? C16 O19 1.369(5) . ? C16 C17 1.386(6) . ? C17 C18 1.385(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O19 C20 1.441(6) . ? C20 C21 1.491(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.541(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.517(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.497(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.512(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.529(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.523(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.527(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.483(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O30 1.440(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C31 1.368(6) . ? C31 C36 1.375(7) . ? C31 C32 1.385(8) . ? C32 C33 1.383(8) . ? C32 H32A 0.9500 . ? C33 C34 1.407(7) . ? C33 H33A 0.9500 . ? C34 C35 1.386(8) . ? C35 C36 1.363(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 O38 1.395(6) . ? C37 C106 1.498(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O38 C39 1.440(6) . ? C39 C40 1.495(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N41 1.352(7) . ? C40 C45 1.390(7) . ? N41 C42 1.347(6) . ? C42 C43 1.407(9) . ? C42 C46 1.469(9) . ? C43 C44 1.388(10) . ? C43 H43A 0.9500 . ? C44 C45 1.351(10) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 O47 1.415(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O47 C48 1.404(8) . ? C48 C49 1.501(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.362(9) . ? C49 C50 1.379(10) . ? C50 C51 1.358(10) . ? C50 H50A 0.9500 . ? C51 C52 1.394(10) . ? C51 H51A 0.9500 . ? C52 O55 1.357(8) . ? C52 C53 1.409(9) . ? C53 C54 1.396(9) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? O55 C56 1.381(8) . ? C56 C57 1.464(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.464(10) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.515(9) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.505(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.525(9) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.480(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.537(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.472(8) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.516(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O66 1.379(7) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O66 C67 1.390(6) . ? C67 C72 1.363(7) . ? C67 C68 1.380(7) . ? C68 C69 1.380(7) . ? C68 H68A 0.9500 . ? C69 C70 1.368(6) . ? C69 H69A 0.9500 . ? C70 C71 1.388(6) . ? C70 C73 1.522(7) . ? C71 C72 1.390(7) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 N74 1.447(6) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? N74 C75 1.337(7) . ? N74 H74N 0.979(5) . ? C75 O75 1.234(6) . ? C75 C76 1.488(7) . ? C76 N77 1.338(6) . ? C76 C81 1.391(7) . ? N77 C78 1.331(6) . ? C78 C79 1.363(7) . ? C78 C82 1.515(7) . ? C79 C80 1.385(8) . ? C79 H79A 0.9500 . ? C80 C81 1.365(8) . ? C80 H80A 0.9500 . ? C81 H81A 0.9500 . ? C82 O82 1.219(5) . ? C82 N83 1.340(6) . ? N83 C84 1.456(6) . ? N83 H83N 0.980(5) . ? C84 C85 1.508(7) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C90 1.375(6) . ? C85 C86 1.372(7) . ? C86 C87 1.389(7) . ? C86 H86A 0.9500 . ? C87 C88 1.352(7) . ? C87 H87A 0.9500 . ? C88 O91 1.370(5) . ? C88 C89 1.384(7) . ? C89 C90 1.396(7) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? O91 C92 1.416(6) . ? C92 C93 1.507(7) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.531(8) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.518(8) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.499(9) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.520(11) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.566(11) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.628(12) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.480(12) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.690(11) . ? C100 H10E 0.9900 . ? C100 H10F 0.9900 . ? C101 O102 1.490(10) . ? C101 H10G 0.9900 . ? C101 H10H 0.9900 . ? O102 C103 1.400(7) . ? C103 C108 1.354(8) . ? C103 C104 1.368(8) . ? C104 C105 1.382(8) . ? C104 H10A 0.9500 . ? C105 C106 1.392(7) . ? C105 H10B 0.9500 . ? C106 C107 1.353(7) . ? C107 C108 1.382(7) . ? C107 H10C 0.9500 . ? C108 H10D 0.9500 . ? 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 C1 C34 113.6(4) . . ? N2 C1 H1A 108.8 . . ? C34 C1 H1A 108.8 . . ? N2 C1 H1B 108.8 . . ? C34 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 N2 C1 121.9(5) . . ? C3 N2 H2N 131(4) . . ? C1 N2 H2N 106(4) . . ? O3 C3 N2 124.6(5) . . ? O3 C3 C4 120.5(5) . . ? N2 C3 C4 114.9(5) . . ? N5 C4 C9 123.4(5) . . ? N5 C4 C3 116.1(5) . . ? C9 C4 C3 120.5(5) . . ? C6 N5 C4 116.5(4) . . ? N5 C6 C7 123.2(5) . . ? N5 C6 C10 116.8(4) . . ? C7 C6 C10 120.0(5) . . ? C8 C7 C6 120.0(5) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 117.6(5) . . ? C7 C8 H8A 121.2 . . ? C9 C8 H8A 121.2 . . ? C8 C9 C4 119.2(5) . . ? C8 C9 H9A 120.4 . . ? C4 C9 H9A 120.4 . . ? O10 C10 N11 124.1(4) . . ? O10 C10 C6 120.4(4) . . ? N11 C10 C6 115.5(4) . . ? C10 N11 C12 123.5(4) . . ? C10 N11 H11N 123(3) . . ? C12 N11 H11N 113(3) . . ? N11 C12 C13 113.4(4) . . ? N11 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C18 118.6(4) . . ? C14 C13 C12 121.4(4) . . ? C18 C13 C12 120.0(4) . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? O19 C16 C17 115.3(4) . . ? O19 C16 C15 125.0(4) . . ? C17 C16 C15 119.7(4) . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C13 119.9(4) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? C16 O19 C20 118.9(3) . . ? O19 C20 C21 114.0(4) . . ? O19 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? O19 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 113.9(4) . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 111.2(4) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 116.8(4) . . ? C24 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? C22 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C23 C24 C25 113.4(4) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 C26 115.7(4) . . ? C24 C25 H25A 108.3 . . ? C26 C25 H25A 108.3 . . ? C24 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C25 116.0(4) . . ? C27 C26 H26A 108.3 . . ? C25 C26 H26A 108.3 . . ? C27 C26 H26B 108.3 . . ? C25 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C28 C27 C26 112.3(5) . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 116.3(5) . . ? C29 C28 H28A 108.2 . . ? C27 C28 H28A 108.2 . . ? C29 C28 H28B 108.2 . . ? C27 C28 H28B 108.2 . . ? H28A C28 H28B 107.4 . . ? O30 C29 C28 111.0(4) . . ? O30 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? O30 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 O30 C29 120.7(4) . . ? O30 C31 C36 126.4(5) . . ? O30 C31 C32 114.5(5) . . ? C36 C31 C32 119.1(5) . . ? C31 C32 C33 119.7(5) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C32 C33 C34 121.7(6) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 116.4(6) . . ? C35 C34 C1 121.7(5) . . ? C33 C34 C1 121.9(6) . . ? C36 C35 C34 122.1(5) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C35 C36 C31 121.0(6) . . ? C35 C36 H36A 119.5 . . ? C31 C36 H36A 119.5 . . ? O38 C37 C106 115.2(4) . . ? O38 C37 H37A 108.5 . . ? C106 C37 H37A 108.5 . . ? O38 C37 H37B 108.5 . . ? C106 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C37 O38 C39 114.8(4) . . ? O38 C39 C40 115.2(4) . . ? O38 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? O38 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? N41 C40 C45 121.4(5) . . ? N41 C40 C39 114.4(4) . . ? C45 C40 C39 124.1(6) . . ? C42 N41 C40 118.4(5) . . ? N41 C42 C43 122.0(6) . . ? N41 C42 C46 113.8(5) . . ? C43 C42 C46 124.1(6) . . ? C44 C43 C42 118.2(6) . . ? C44 C43 H43A 120.9 . . ? C42 C43 H43A 120.9 . . ? C45 C44 C43 119.5(6) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? C44 C45 C40 120.3(7) . . ? C44 C45 H45A 119.8 . . ? C40 C45 H45A 119.8 . . ? O47 C46 C42 110.2(5) . . ? O47 C46 H46A 109.6 . . ? C42 C46 H46A 109.6 . . ? O47 C46 H46B 109.6 . . ? C42 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C48 O47 C46 114.9(6) . . ? O47 C48 C49 112.0(5) . . ? O47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? O47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C54 C49 C50 116.1(7) . . ? C54 C49 C48 119.6(7) . . ? C50 C49 C48 124.2(7) . . ? C51 C50 C49 125.3(7) . . ? C51 C50 H50A 117.3 . . ? C49 C50 H50A 117.3 . . ? C50 C51 C52 118.5(8) . . ? C50 C51 H51A 120.7 . . ? C52 C51 H51A 120.7 . . ? O55 C52 C51 116.7(7) . . ? O55 C52 C53 125.5(7) . . ? C51 C52 C53 117.8(7) . . ? C54 C53 C52 120.4(6) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C49 C54 C53 121.6(7) . . ? C49 C54 H54A 119.2 . . ? C53 C54 H54A 119.2 . . ? C56 O55 C52 116.1(6) . . ? O55 C56 C57 109.4(7) . . ? O55 C56 H56A 109.8 . . ? C57 C56 H56A 109.8 . . ? O55 C56 H56B 109.8 . . ? C57 C56 H56B 109.8 . . ? H56A C56 H56B 108.2 . . ? C56 C57 C58 118.3(8) . . ? C56 C57 H57A 107.7 . . ? C58 C57 H57A 107.7 . . ? C56 C57 H57B 107.7 . . ? C58 C57 H57B 107.7 . . ? H57A C57 H57B 107.1 . . ? C57 C58 C59 115.2(7) . . ? C57 C58 H58A 108.5 . . ? C59 C58 H58A 108.5 . . ? C57 C58 H58B 108.5 . . ? C59 C58 H58B 108.5 . . ? H58A C58 H58B 107.5 . . ? C58 C59 C60 117.4(6) . . ? C58 C59 H59A 108.0 . . ? C60 C59 H59A 108.0 . . ? C58 C59 H59B 108.0 . . ? C60 C59 H59B 108.0 . . ? H59A C59 H59B 107.2 . . ? C61 C60 C59 115.2(6) . . ? C61 C60 H60A 108.5 . . ? C59 C60 H60A 108.5 . . ? C61 C60 H60B 108.5 . . ? C59 C60 H60B 108.5 . . ? H60A C60 H60B 107.5 . . ? C62 C61 C60 117.0(6) . . ? C62 C61 H61A 108.1 . . ? C60 C61 H61A 108.0 . . ? C62 C61 H61B 108.0 . . ? C60 C61 H61B 108.0 . . ? H61A C61 H61B 107.3 . . ? C61 C62 C63 114.2(6) . . ? C61 C62 H62A 108.7 . . ? C63 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C63 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? C64 C63 C62 114.2(5) . . ? C64 C63 H63A 108.7 . . ? C62 C63 H63A 108.7 . . ? C64 C63 H63B 108.7 . . ? C62 C63 H63B 108.7 . . ? H63A C63 H63B 107.6 . . ? C63 C64 C65 111.2(5) . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64B 109.4 . . ? C65 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? O66 C65 C64 109.3(5) . . ? O66 C65 H65A 109.8 . . ? C64 C65 H65A 109.8 . . ? O66 C65 H65B 109.8 . . ? C64 C65 H65B 109.8 . . ? H65A C65 H65B 108.3 . . ? C65 O66 C67 118.2(4) . . ? C72 C67 C68 120.0(5) . . ? C72 C67 O66 115.6(4) . . ? C68 C67 O66 124.4(5) . . ? C67 C68 C69 119.2(5) . . ? C67 C68 H68A 120.4 . . ? C69 C68 H68A 120.4 . . ? C70 C69 C68 121.9(5) . . ? C70 C69 H69A 119.0 . . ? C68 C69 H69A 119.0 . . ? C69 C70 C71 118.4(5) . . ? C69 C70 C73 119.1(4) . . ? C71 C70 C73 122.5(4) . . ? C70 C71 C72 120.1(5) . . ? C70 C71 H71A 120.0 . . ? C72 C71 H71A 120.0 . . ? C67 C72 C71 120.4(5) . . ? C67 C72 H72A 119.8 . . ? C71 C72 H72A 119.8 . . ? N74 C73 C70 114.3(4) . . ? N74 C73 H73A 108.7 . . ? C70 C73 H73A 108.7 . . ? N74 C73 H73B 108.7 . . ? C70 C73 H73B 108.7 . . ? H73A C73 H73B 107.6 . . ? C75 N74 C73 121.3(5) . . ? C75 N74 H74N 116(3) . . ? C73 N74 H74N 123(3) . . ? O75 C75 N74 123.9(5) . . ? O75 C75 C76 121.0(5) . . ? N74 C75 C76 115.1(4) . . ? N77 C76 C81 122.1(5) . . ? N77 C76 C75 116.9(4) . . ? C81 C76 C75 121.0(5) . . ? C78 N77 C76 118.3(4) . . ? N77 C78 C79 122.9(5) . . ? N77 C78 C82 116.2(4) . . ? C79 C78 C82 120.8(5) . . ? C78 C79 C80 118.9(5) . . ? C78 C79 H79A 120.5 . . ? C80 C79 H79A 120.5 . . ? C81 C80 C79 119.0(5) . . ? C81 C80 H80A 120.5 . . ? C79 C80 H80A 120.5 . . ? C80 C81 C76 118.7(5) . . ? C80 C81 H81A 120.7 . . ? C76 C81 H81A 120.7 . . ? O82 C82 N83 125.2(5) . . ? O82 C82 C78 121.1(5) . . ? N83 C82 C78 113.6(4) . . ? C82 N83 C84 122.3(4) . . ? C82 N83 H83N 115(3) . . ? C84 N83 H83N 118(3) . . ? N83 C84 C85 112.2(4) . . ? N83 C84 H84A 109.2 . . ? C85 C84 H84A 109.2 . . ? N83 C84 H84B 109.2 . . ? C85 C84 H84B 109.2 . . ? H84A C84 H84B 107.9 . . ? C90 C85 C86 117.2(5) . . ? C90 C85 C84 121.7(4) . . ? C86 C85 C84 121.1(4) . . ? C85 C86 C87 120.6(5) . . ? C85 C86 H86A 119.7 . . ? C87 C86 H86A 119.7 . . ? C88 C87 C86 122.2(5) . . ? C88 C87 H87A 118.9 . . ? C86 C87 H87A 118.9 . . ? C87 C88 O91 118.0(4) . . ? C87 C88 C89 118.3(5) . . ? O91 C88 C89 123.7(4) . . ? C88 C89 C90 119.3(5) . . ? C88 C89 H89A 120.3 . . ? C90 C89 H89A 120.3 . . ? C85 C90 C89 122.3(5) . . ? C85 C90 H90A 118.8 . . ? C89 C90 H90A 118.9 . . ? C88 O91 C92 117.9(4) . . ? O91 C92 C93 108.9(4) . . ? O91 C92 H92A 109.9 . . ? C93 C92 H92A 109.9 . . ? O91 C92 H92B 109.9 . . ? C93 C92 H92B 109.9 . . ? H92A C92 H92B 108.3 . . ? C92 C93 C94 112.1(4) . . ? C92 C93 H93A 109.2 . . ? C94 C93 H93A 109.2 . . ? C92 C93 H93B 109.2 . . ? C94 C93 H93B 109.2 . . ? H93A C93 H93B 107.9 . . ? C95 C94 C93 112.8(5) . . ? C95 C94 H94A 109.0 . . ? C93 C94 H94A 109.0 . . ? C95 C94 H94B 109.0 . . ? C93 C94 H94B 109.0 . . ? H94A C94 H94B 107.8 . . ? C96 C95 C94 114.3(5) . . ? C96 C95 H95A 108.7 . . ? C94 C95 H95A 108.7 . . ? C96 C95 H95B 108.7 . . ? C94 C95 H95B 108.7 . . ? H95A C95 H95B 107.6 . . ? C95 C96 C97 113.7(6) . . ? C95 C96 H96A 108.8 . . ? C97 C96 H96A 108.8 . . ? C95 C96 H96B 108.8 . . ? C97 C96 H96B 108.8 . . ? H96A C96 H96B 107.7 . . ? C96 C97 C98 116.4(8) . . ? C96 C97 H97A 108.2 . . ? C98 C97 H97A 108.2 . . ? C96 C97 H97B 108.2 . . ? C98 C97 H97B 108.2 . . ? H97A C97 H97B 107.3 . . ? C97 C98 C99 126.5(9) . . ? C97 C98 H98A 105.7 . . ? C99 C98 H98A 105.7 . . ? C97 C98 H98B 105.7 . . ? C99 C98 H98B 105.7 . . ? H98A C98 H98B 106.1 . . ? C100 C99 C98 93.1(10) . . ? C100 C99 H99A 113.1 . . ? C98 C99 H99A 113.1 . . ? C100 C99 H99B 113.1 . . ? C98 C99 H99B 113.1 . . ? H99A C99 H99B 110.5 . . ? C99 C100 C101 102.1(10) . . ? C99 C100 H10E 111.4 . . ? C101 C100 H10E 111.4 . . ? C99 C100 H10F 111.4 . . ? C101 C100 H10F 111.4 . . ? H10E C100 H10F 109.2 . . ? O102 C101 C100 107.0(7) . . ? O102 C101 H10G 110.3 . . ? C100 C101 H10G 110.3 . . ? O102 C101 H10H 110.3 . . ? C100 C101 H10H 110.3 . . ? H10G C101 H10H 108.6 . . ? C103 O102 C101 118.6(5) . . ? C108 C103 C104 120.0(5) . . ? C108 C103 O102 124.0(6) . . ? C104 C103 O102 116.0(5) . . ? C103 C104 C105 120.1(5) . . ? C103 C104 H10A 120.0 . . ? C105 C104 H10A 120.0 . . ? C104 C105 C106 120.2(6) . . ? C104 C105 H10B 119.9 . . ? C106 C105 H10B 119.9 . . ? C107 C106 C105 118.0(5) . . ? C107 C106 C37 120.2(5) . . ? C105 C106 C37 121.7(5) . . ? C106 C107 C108 121.9(5) . . ? C106 C107 H10C 119.1 . . ? C108 C107 H10C 119.1 . . ? C103 C108 C107 119.7(6) . . ? C103 C108 H10D 120.1 . . ? C107 C108 H10D 120.1 . . ? 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 C34 C1 N2 C3 -97.7(6) . . . . ? C1 N2 C3 O3 1.9(9) . . . . ? C1 N2 C3 C4 -177.7(5) . . . . ? O3 C3 C4 N5 -172.5(5) . . . . ? N2 C3 C4 N5 7.1(7) . . . . ? O3 C3 C4 C9 8.2(8) . . . . ? N2 C3 C4 C9 -172.2(5) . . . . ? C9 C4 N5 C6 0.7(7) . . . . ? C3 C4 N5 C6 -178.6(4) . . . . ? C4 N5 C6 C7 2.5(7) . . . . ? C4 N5 C6 C10 -175.8(4) . . . . ? N5 C6 C7 C8 -3.6(8) . . . . ? C10 C6 C7 C8 174.7(5) . . . . ? C6 C7 C8 C9 1.3(8) . . . . ? C7 C8 C9 C4 1.7(9) . . . . ? N5 C4 C9 C8 -2.8(8) . . . . ? C3 C4 C9 C8 176.4(5) . . . . ? N5 C6 C10 O10 -175.5(4) . . . . ? C7 C6 C10 O10 6.1(7) . . . . ? N5 C6 C10 N11 7.4(6) . . . . ? C7 C6 C10 N11 -171.0(4) . . . . ? O10 C10 N11 C12 -1.7(7) . . . . ? C6 C10 N11 C12 175.2(4) . . . . ? C10 N11 C12 C13 100.1(5) . . . . ? N11 C12 C13 C14 -76.3(5) . . . . ? N11 C12 C13 C18 101.4(5) . . . . ? C18 C13 C14 C15 -0.1(7) . . . . ? C12 C13 C14 C15 177.6(4) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C14 C15 C16 O19 177.5(4) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? O19 C16 C17 C18 -178.3(4) . . . . ? C15 C16 C17 C18 -1.1(7) . . . . ? C16 C17 C18 C13 1.1(7) . . . . ? C14 C13 C18 C17 -0.5(6) . . . . ? C12 C13 C18 C17 -178.2(4) . . . . ? C17 C16 O19 C20 -164.2(4) . . . . ? C15 C16 O19 C20 18.8(6) . . . . ? C16 O19 C20 C21 69.0(5) . . . . ? O19 C20 C21 C22 57.8(6) . . . . ? C20 C21 C22 C23 174.1(5) . . . . ? C21 C22 C23 C24 169.0(5) . . . . ? C22 C23 C24 C25 178.0(5) . . . . ? C23 C24 C25 C26 175.4(5) . . . . ? C24 C25 C26 C27 -64.4(6) . . . . ? C25 C26 C27 C28 -171.6(5) . . . . ? C26 C27 C28 C29 -173.2(5) . . . . ? C27 C28 C29 O30 -70.6(6) . . . . ? C28 C29 O30 C31 112.5(5) . . . . ? C29 O30 C31 C36 -17.0(7) . . . . ? C29 O30 C31 C32 163.1(5) . . . . ? O30 C31 C32 C33 179.5(5) . . . . ? C36 C31 C32 C33 -0.5(8) . . . . ? C31 C32 C33 C34 1.9(8) . . . . ? C32 C33 C34 C35 -2.9(7) . . . . ? C32 C33 C34 C1 177.8(5) . . . . ? N2 C1 C34 C35 -87.5(6) . . . . ? N2 C1 C34 C33 91.8(6) . . . . ? C33 C34 C35 C36 2.7(7) . . . . ? C1 C34 C35 C36 -178.0(5) . . . . ? C34 C35 C36 C31 -1.4(8) . . . . ? O30 C31 C36 C35 -179.7(5) . . . . ? C32 C31 C36 C35 0.2(7) . . . . ? C106 C37 O38 C39 -60.2(6) . . . . ? C37 O38 C39 C40 -78.5(6) . . . . ? O38 C39 C40 N41 160.8(4) . . . . ? O38 C39 C40 C45 -22.1(8) . . . . ? C45 C40 N41 C42 -5.1(7) . . . . ? C39 C40 N41 C42 172.1(4) . . . . ? C40 N41 C42 C43 4.3(7) . . . . ? C40 N41 C42 C46 -179.5(4) . . . . ? N41 C42 C43 C44 -0.8(9) . . . . ? C46 C42 C43 C44 -176.7(6) . . . . ? C42 C43 C44 C45 -1.9(9) . . . . ? C43 C44 C45 C40 1.1(9) . . . . ? N41 C40 C45 C44 2.5(8) . . . . ? C39 C40 C45 C44 -174.5(5) . . . . ? N41 C42 C46 O47 73.3(6) . . . . ? C43 C42 C46 O47 -110.5(6) . . . . ? C42 C46 O47 C48 -172.8(5) . . . . ? C46 O47 C48 C49 76.7(7) . . . . ? O47 C48 C49 C54 87.5(8) . . . . ? O47 C48 C49 C50 -88.2(8) . . . . ? C54 C49 C50 C51 1.7(12) . . . . ? C48 C49 C50 C51 177.5(8) . . . . ? C49 C50 C51 C52 1.7(14) . . . . ? C50 C51 C52 O55 179.2(7) . . . . ? C50 C51 C52 C53 -3.8(11) . . . . ? O55 C52 C53 C54 179.5(6) . . . . ? C51 C52 C53 C54 2.8(10) . . . . ? C50 C49 C54 C53 -2.7(10) . . . . ? C48 C49 C54 C53 -178.8(6) . . . . ? C52 C53 C54 C49 0.5(10) . . . . ? C51 C52 O55 C56 -174.5(7) . . . . ? C53 C52 O55 C56 8.8(10) . . . . ? C52 O55 C56 C57 169.6(6) . . . . ? O55 C56 C57 C58 71.9(9) . . . . ? C56 C57 C58 C59 168.9(7) . . . . ? C57 C58 C59 C60 -165.7(7) . . . . ? C58 C59 C60 C61 175.4(6) . . . . ? C59 C60 C61 C62 -175.8(7) . . . . ? C60 C61 C62 C63 179.4(6) . . . . ? C61 C62 C63 C64 168.4(6) . . . . ? C62 C63 C64 C65 -172.4(6) . . . . ? C63 C64 C65 O66 163.6(6) . . . . ? C64 C65 O66 C67 -176.6(5) . . . . ? C65 O66 C67 C72 175.5(5) . . . . ? C65 O66 C67 C68 -3.8(8) . . . . ? C72 C67 C68 C69 1.1(8) . . . . ? O66 C67 C68 C69 -179.5(5) . . . . ? C67 C68 C69 C70 -0.3(8) . . . . ? C68 C69 C70 C71 -0.2(8) . . . . ? C68 C69 C70 C73 178.4(5) . . . . ? C69 C70 C71 C72 -0.1(8) . . . . ? C73 C70 C71 C72 -178.7(5) . . . . ? C68 C67 C72 C71 -1.5(8) . . . . ? O66 C67 C72 C71 179.1(5) . . . . ? C70 C71 C72 C67 1.0(8) . . . . ? C69 C70 C73 N74 174.9(5) . . . . ? C71 C70 C73 N74 -6.5(8) . . . . ? C70 C73 N74 C75 -91.0(6) . . . . ? C73 N74 C75 O75 -2.8(7) . . . . ? C73 N74 C75 C76 175.8(4) . . . . ? O75 C75 C76 N77 163.9(4) . . . . ? N74 C75 C76 N77 -14.7(6) . . . . ? O75 C75 C76 C81 -13.3(7) . . . . ? N74 C75 C76 C81 168.0(4) . . . . ? C81 C76 N77 C78 -0.1(6) . . . . ? C75 C76 N77 C78 -177.3(4) . . . . ? C76 N77 C78 C79 -2.1(6) . . . . ? C76 N77 C78 C82 173.7(3) . . . . ? N77 C78 C79 C80 1.9(7) . . . . ? C82 C78 C79 C80 -173.7(4) . . . . ? C78 C79 C80 C81 0.4(7) . . . . ? C79 C80 C81 C76 -2.4(7) . . . . ? N77 C76 C81 C80 2.3(7) . . . . ? C75 C76 C81 C80 179.4(4) . . . . ? N77 C78 C82 O82 -166.3(4) . . . . ? C79 C78 C82 O82 9.6(6) . . . . ? N77 C78 C82 N83 11.6(5) . . . . ? C79 C78 C82 N83 -172.5(4) . . . . ? O82 C82 N83 C84 15.3(7) . . . . ? C78 C82 N83 C84 -162.5(4) . . . . ? C82 N83 C84 C85 99.6(5) . . . . ? N83 C84 C85 C90 30.9(7) . . . . ? N83 C84 C85 C86 -151.9(5) . . . . ? C90 C85 C86 C87 -3.6(8) . . . . ? C84 C85 C86 C87 179.2(5) . . . . ? C85 C86 C87 C88 3.8(9) . . . . ? C86 C87 C88 O91 178.3(5) . . . . ? C86 C87 C88 C89 -1.7(8) . . . . ? C87 C88 C89 C90 -0.6(8) . . . . ? O91 C88 C89 C90 179.5(5) . . . . ? C86 C85 C90 C89 1.4(8) . . . . ? C84 C85 C90 C89 178.6(5) . . . . ? C88 C89 C90 C85 0.7(8) . . . . ? C87 C88 O91 C92 -179.5(5) . . . . ? C89 C88 O91 C92 0.5(7) . . . . ? C88 O91 C92 C93 -171.9(4) . . . . ? O91 C92 C93 C94 -178.7(5) . . . . ? C92 C93 C94 C95 -166.4(5) . . . . ? C93 C94 C95 C96 175.2(6) . . . . ? C94 C95 C96 C97 -178.2(7) . . . . ? C95 C96 C97 C98 179.9(8) . . . . ? C96 C97 C98 C99 151.2(11) . . . . ? C97 C98 C99 C100 57.7(15) . . . . ? C98 C99 C100 C101 168.4(8) . . . . ? C99 C100 C101 O102 65.0(11) . . . . ? C100 C101 O102 C103 167.6(6) . . . . ? C101 O102 C103 C108 -6.7(9) . . . . ? C101 O102 C103 C104 175.7(6) . . . . ? C108 C103 C104 C105 -0.7(9) . . . . ? O102 C103 C104 C105 177.0(5) . . . . ? C103 C104 C105 C106 0.5(8) . . . . ? C104 C105 C106 C107 1.5(7) . . . . ? C104 C105 C106 C37 179.4(5) . . . . ? O38 C37 C106 C107 136.4(5) . . . . ? O38 C37 C106 C105 -41.4(7) . . . . ? C105 C106 C107 C108 -3.4(7) . . . . ? C37 C106 C107 C108 178.8(5) . . . . ? C104 C103 C108 C107 -1.1(8) . . . . ? O102 C103 C108 C107 -178.6(5) . . . . ? C106 C107 C108 C103 3.2(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N N41 0.979(5) 2.28(2) 3.210(7) 159(5) . N11 H11N N5 0.979(5) 2.34(5) 2.696(5) 100(3) . N11 H11N N41 0.979(5) 2.43(3) 3.211(5) 136(3) . N74 H74N O10 0.979(5) 2.03(3) 2.911(6) 149(4) 3_797 N83 H83N O10 0.980(5) 2.11(3) 2.964(5) 145(4) 3_797 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.939 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.142 # Attachment '- Pd3H2.cif' data_Pd3H2 _database_code_depnum_ccdc_archive 'CCDC 874998' #TrackingRef '- Pd3H2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C93 H111 N7 O12 Pd,2(C2 H2 N)' _chemical_formula_sum 'C97 H117 N9 O12 Pd' _chemical_formula_weight 1707.40 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 13.579(2) _cell_length_b 17.669(3) _cell_length_c 19.456(3) _cell_angle_alpha 77.683(8) _cell_angle_beta 74.610(8) _cell_angle_gamma 81.063(8) _cell_volume 4373.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9061 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.8 _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44474 _diffrn_reflns_av_R_equivalents 0.0905 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.39 _reflns_number_total 15933 _reflns_number_gt 10647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. The NH hydrogen atoms were located from a difference map and refined isotropically subject to a distance restraint. ; _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^)+(0.1653P)^2^+23.0733P] 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 15933 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1641 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3327 _refine_ls_wR_factor_gt 0.2963 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 0.13888(5) 0.20208(4) 0.15740(4) 0.0489(2) Uani 1 1 d . . . C1 C 0.0083(6) 0.1679(5) 0.0564(5) 0.055(2) Uani 1 1 d . . . H1A H 0.0035 0.1832 0.0053 0.066 Uiso 1 1 calc R . . H1B H -0.0521 0.1946 0.0865 0.066 Uiso 1 1 calc R . . N2 N 0.1015(5) 0.1934(3) 0.0635(4) 0.0463(16) Uani 1 1 d . . . C3 C 0.1695(6) 0.2215(4) 0.0028(5) 0.0465(19) Uani 1 1 d . . . O3 O 0.1663(4) 0.2219(3) -0.0608(3) 0.0498(13) Uani 1 1 d . . . C4 C 0.2549(6) 0.2552(4) 0.0176(5) 0.0447(19) Uani 1 1 d . . . N5 N 0.2470(5) 0.2549(3) 0.0874(4) 0.0468(16) Uani 1 1 d . . . C6 C 0.3152(7) 0.2823(5) 0.1116(5) 0.053(2) Uani 1 1 d . . . C7 C 0.3993(6) 0.3124(4) 0.0623(5) 0.051(2) Uani 1 1 d . . . H7A H 0.4490 0.3322 0.0782 0.061 Uiso 1 1 calc R . . C8 C 0.4104(7) 0.3134(4) -0.0102(5) 0.053(2) Uani 1 1 d . . . H8A H 0.4683 0.3337 -0.0448 0.064 Uiso 1 1 calc R . . C9 C 0.3375(6) 0.2849(4) -0.0328(5) 0.049(2) Uani 1 1 d . . . H9A H 0.3447 0.2859 -0.0829 0.058 Uiso 1 1 calc R . . C10 C 0.2905(8) 0.2730(5) 0.1935(5) 0.056(2) Uani 1 1 d . . . O10 O 0.3460(5) 0.2997(4) 0.2215(4) 0.0641(17) Uani 1 1 d . . . N11 N 0.2080(6) 0.2343(4) 0.2262(4) 0.0500(16) Uani 1 1 d . . . C12 C 0.1724(8) 0.2269(5) 0.3039(5) 0.060(2) Uani 1 1 d . . . H12A H 0.0977 0.2434 0.3159 0.071 Uiso 1 1 calc R . . H12B H 0.2065 0.2632 0.3200 0.071 Uiso 1 1 calc R . . C13 C 0.1914(7) 0.1464(5) 0.3461(5) 0.055(2) Uani 1 1 d . . . C14 C 0.2832(7) 0.1001(5) 0.3273(5) 0.057(2) Uani 1 1 d . . . H14A H 0.3337 0.1190 0.2854 0.069 Uiso 1 1 calc R . . C15 C 0.3036(7) 0.0274(5) 0.3674(5) 0.062(2) Uani 1 1 d . . . H15A H 0.3665 -0.0036 0.3528 0.074 Uiso 1 1 calc R . . C16 C 0.2321(7) 0.0008(5) 0.4284(5) 0.060(2) Uani 1 1 d . . . C17 C 0.1380(8) 0.0441(6) 0.4483(5) 0.067(3) Uani 1 1 d . . . H17A H 0.0873 0.0246 0.4897 0.080 Uiso 1 1 calc R . . C18 C 0.1197(7) 0.1164(6) 0.4065(5) 0.064(2) Uani 1 1 d . . . H18A H 0.0555 0.1462 0.4199 0.076 Uiso 1 1 calc R . . O19 O 0.2441(5) -0.0697(4) 0.4745(3) 0.0719(19) Uani 1 1 d . . . C20 C 0.3289(10) -0.1230(6) 0.4497(6) 0.091(4) Uani 1 1 d . . . H20A H 0.3939 -0.1050 0.4508 0.110 Uiso 1 1 calc R . . H20B H 0.3325 -0.1281 0.3994 0.110 Uiso 1 1 calc R . . C21 C 0.3115(10) -0.2025(6) 0.5020(7) 0.092(4) Uani 1 1 d . . . H21A H 0.3647 -0.2431 0.4833 0.110 Uiso 1 1 calc R . . H21B H 0.3192 -0.1984 0.5502 0.110 Uiso 1 1 calc R . . C22 C 0.2038(12) -0.2276(7) 0.5104(7) 0.099(4) Uani 1 1 d . . . H22A H 0.1969 -0.2781 0.5442 0.119 Uiso 1 1 calc R . . H22B H 0.1508 -0.1886 0.5321 0.119 Uiso 1 1 calc R . . C23 C 0.1855(12) -0.2354(8) 0.4431(8) 0.107(4) Uani 1 1 d . . . H23A H 0.2339 -0.2783 0.4240 0.128 Uiso 1 1 calc R . . H23B H 0.1997 -0.1868 0.4076 0.128 Uiso 1 1 calc R . . C24 C 0.0737(11) -0.2522(8) 0.4505(7) 0.096(4) Uani 1 1 d . . . H24A H 0.0590 -0.2994 0.4879 0.116 Uiso 1 1 calc R . . H24B H 0.0260 -0.2081 0.4680 0.116 Uiso 1 1 calc R . . C25 C 0.0516(12) -0.2642(8) 0.3808(8) 0.109(5) Uani 1 1 d . . . H25A H 0.0778 -0.2213 0.3415 0.131 Uiso 1 1 calc R . . H25B H 0.0912 -0.3133 0.3681 0.131 Uiso 1 1 calc R . . C26 C -0.0521(14) -0.2674(10) 0.3827(8) 0.125(5) Uani 1 1 d . . . H26A H -0.0938 -0.2191 0.3957 0.150 Uiso 1 1 calc R . . H26B H -0.0792 -0.3121 0.4195 0.150 Uiso 1 1 calc R . . C27 C -0.0596(17) -0.2785(10) 0.293(2) 0.29(2) Uani 1 1 d D . . H27A H -0.0047 -0.3169 0.2722 0.349 Uiso 1 1 calc R . . H27B H -0.1275 -0.2926 0.2932 0.349 Uiso 1 1 calc R . . C28 C -0.0443(18) -0.2012(13) 0.2567(10) 0.173(8) Uani 1 1 d DU . . H28A H -0.0949 -0.1633 0.2819 0.208 Uiso 1 1 calc R . . H28B H 0.0258 -0.1895 0.2540 0.208 Uiso 1 1 calc R . . C29 C -0.0579(13) -0.1986(10) 0.1875(10) 0.137(6) Uani 1 1 d D . . H29A H -0.1268 -0.1721 0.1845 0.164 Uiso 1 1 calc R . . H29B H -0.0547 -0.2524 0.1793 0.164 Uiso 1 1 calc R . . O30 O 0.0149(6) -0.1603(4) 0.1341(5) 0.097(3) Uani 1 1 d . . . C31 C 0.0058(8) -0.0798(6) 0.1180(7) 0.071(3) Uani 1 1 d . . . C32 C -0.0731(9) -0.0324(7) 0.1534(6) 0.081(3) Uani 1 1 d . . . H32A H -0.1272 -0.0541 0.1909 0.097 Uiso 1 1 calc R . . C33 C -0.0718(7) 0.0483(6) 0.1328(5) 0.063(2) Uani 1 1 d . . . H33A H -0.1265 0.0813 0.1566 0.075 Uiso 1 1 calc R . . C34 C 0.0058(6) 0.0813(5) 0.0794(5) 0.0494(19) Uani 1 1 d . . . C35 C 0.0824(7) 0.0299(5) 0.0433(5) 0.057(2) Uani 1 1 d . . . H35A H 0.1346 0.0510 0.0038 0.068 Uiso 1 1 calc R . . C36 C 0.0837(8) -0.0496(5) 0.0635(6) 0.064(3) Uani 1 1 d . . . H36A H 0.1380 -0.0831 0.0400 0.077 Uiso 1 1 calc R . . C37 C -0.2176(8) 0.3554(5) 0.2667(5) 0.068(3) Uani 1 1 d . . . H37A H -0.2145 0.3684 0.2141 0.082 Uiso 1 1 calc R . . H37B H -0.1770 0.3907 0.2785 0.082 Uiso 1 1 calc R . . O38 O -0.1795(5) 0.2749(3) 0.2873(4) 0.0711(18) Uani 1 1 d . . . C39 C -0.0829(7) 0.2547(5) 0.2445(5) 0.063(2) Uani 1 1 d . . . H39A H -0.0314 0.2856 0.2499 0.076 Uiso 1 1 calc R . . H39B H -0.0845 0.2640 0.1928 0.076 Uiso 1 1 calc R . . C40 C -0.0570(7) 0.1686(5) 0.2718(5) 0.055(2) Uani 1 1 d . . . N41 N 0.0347(5) 0.1354(4) 0.2360(3) 0.0442(15) Uani 1 1 d . . . C42 C 0.0608(6) 0.0592(5) 0.2558(4) 0.0482(19) Uani 1 1 d . . . C43 C -0.0029(7) 0.0137(5) 0.3110(5) 0.056(2) Uani 1 1 d . . . H43A H 0.0164 -0.0405 0.3237 0.068 Uiso 1 1 calc R . . C44 C -0.0951(8) 0.0478(5) 0.3478(5) 0.065(3) Uani 1 1 d . . . H44A H -0.1390 0.0177 0.3869 0.078 Uiso 1 1 calc R . . C45 C -0.1221(7) 0.1256(5) 0.3269(5) 0.066(3) Uani 1 1 d . . . H45A H -0.1860 0.1496 0.3506 0.079 Uiso 1 1 calc R . . C46 C 0.1605(6) 0.0261(4) 0.2133(5) 0.050(2) Uani 1 1 d . . . H46A H 0.1609 0.0375 0.1612 0.060 Uiso 1 1 calc R . . H46B H 0.2175 0.0507 0.2196 0.060 Uiso 1 1 calc R . . O47 O 0.1756(4) -0.0563(3) 0.2370(3) 0.0493(13) Uani 1 1 d . . . C48 C 0.2684(7) -0.0866(5) 0.1927(5) 0.062(2) Uani 1 1 d . . . H48A H 0.3264 -0.0616 0.1968 0.074 Uiso 1 1 calc R . . H48B H 0.2640 -0.0736 0.1414 0.074 Uiso 1 1 calc R . . C49 C 0.2887(6) -0.1728(5) 0.2136(5) 0.053(2) Uani 1 1 d . . . C50 C 0.3617(7) -0.2028(5) 0.2519(5) 0.057(2) Uani 1 1 d . . . H50A H 0.3936 -0.1686 0.2689 0.068 Uiso 1 1 calc R . . C51 C 0.3900(7) -0.2835(5) 0.2662(5) 0.060(2) Uani 1 1 d . . . H51A H 0.4419 -0.3037 0.2918 0.071 Uiso 1 1 calc R . . C52 C 0.3421(8) -0.3336(5) 0.2432(5) 0.058(2) Uani 1 1 d . . . C53 C 0.2694(8) -0.3028(6) 0.2051(5) 0.064(2) Uani 1 1 d . . . H53A H 0.2366 -0.3366 0.1884 0.077 Uiso 1 1 calc R . . C54 C 0.2428(7) -0.2234(5) 0.1903(5) 0.062(2) Uani 1 1 d . . . H54A H 0.1922 -0.2034 0.1636 0.075 Uiso 1 1 calc R . . O55 O 0.3646(6) -0.4128(3) 0.2538(4) 0.0689(18) Uani 1 1 d . . . C56 C 0.4337(8) -0.4484(6) 0.3002(5) 0.069(3) Uani 1 1 d . . . H56A H 0.4974 -0.4221 0.2836 0.082 Uiso 1 1 calc R . . H56B H 0.4527 -0.5038 0.2956 0.082 Uiso 1 1 calc R . . C57 C 0.3859(8) -0.4432(6) 0.3793(5) 0.070(3) Uani 1 1 d . . . H57A H 0.4301 -0.4769 0.4092 0.084 Uiso 1 1 calc R . . H57B H 0.3847 -0.3889 0.3857 0.084 Uiso 1 1 calc R . . C58 C 0.2788(9) -0.4667(6) 0.4070(5) 0.073(3) Uani 1 1 d . . . H58A H 0.2777 -0.5189 0.3963 0.087 Uiso 1 1 calc R . . H58B H 0.2321 -0.4293 0.3816 0.087 Uiso 1 1 calc R . . C59 C 0.2410(9) -0.4689(7) 0.4878(5) 0.083(3) Uani 1 1 d . . . H59A H 0.2520 -0.4189 0.4984 0.099 Uiso 1 1 calc R . . H59B H 0.2837 -0.5107 0.5127 0.099 Uiso 1 1 calc R . . C60 C 0.1273(9) -0.4825(7) 0.5203(5) 0.074(3) Uani 1 1 d . . . H60A H 0.0841 -0.4420 0.4945 0.089 Uiso 1 1 calc R . . H60B H 0.1164 -0.5337 0.5121 0.089 Uiso 1 1 calc R . . C61 C 0.0932(9) -0.4808(9) 0.5989(6) 0.094(4) Uani 1 1 d . . . H61A H 0.1157 -0.4337 0.6075 0.113 Uiso 1 1 calc R . . H61B H 0.1291 -0.5266 0.6248 0.113 Uiso 1 1 calc R . . C62 C -0.0192(9) -0.4809(7) 0.6316(5) 0.082(3) Uani 1 1 d . . . H62A H -0.0429 -0.5266 0.6212 0.098 Uiso 1 1 calc R . . H62B H -0.0554 -0.4336 0.6080 0.098 Uiso 1 1 calc R . . C63 C -0.0496(9) -0.4835(7) 0.7133(6) 0.082(3) Uani 1 1 d . . . H63A H -0.0252 -0.5357 0.7372 0.099 Uiso 1 1 calc R . . H63B H -0.0128 -0.4450 0.7243 0.099 Uiso 1 1 calc R . . C64 C -0.1601(8) -0.4676(6) 0.7460(6) 0.069(3) Uani 1 1 d . . . H64A H -0.1981 -0.5048 0.7344 0.083 Uiso 1 1 calc R . . H64B H -0.1847 -0.4144 0.7244 0.083 Uiso 1 1 calc R . . C65 C -0.1836(8) -0.4746(5) 0.8294(5) 0.064(2) Uani 1 1 d . . . H65A H -0.2572 -0.4584 0.8489 0.076 Uiso 1 1 calc R . . H65B H -0.1676 -0.5291 0.8524 0.076 Uiso 1 1 calc R . . O66 O -0.1231(5) -0.4264(4) 0.8436(3) 0.0640(16) Uani 1 1 d . . . C67 C -0.1210(7) -0.4310(5) 0.9140(5) 0.053(2) Uani 1 1 d . . . C68 C -0.0441(7) -0.3957(5) 0.9243(6) 0.059(2) Uani 1 1 d . . . H68A H 0.0039 -0.3719 0.8833 0.071 Uiso 1 1 calc R . . C69 C -0.0353(7) -0.3943(5) 0.9923(6) 0.061(2) Uani 1 1 d . . . H69A H 0.0187 -0.3694 0.9978 0.073 Uiso 1 1 calc R . . C70 C -0.1033(7) -0.4282(5) 1.0533(5) 0.056(2) Uani 1 1 d . . . C71 C -0.1800(7) -0.4639(5) 1.0428(5) 0.052(2) Uani 1 1 d . . . H71A H -0.2276 -0.4874 1.0842 0.062 Uiso 1 1 calc R . . C72 C -0.1913(7) -0.4675(5) 0.9743(4) 0.049(2) Uani 1 1 d . . . H72A H -0.2441 -0.4934 0.9687 0.059 Uiso 1 1 calc R . . C73 C -0.0920(8) -0.4272(5) 1.1273(6) 0.069(3) Uani 1 1 d . . . H73A H -0.0933 -0.4808 1.1557 0.083 Uiso 1 1 calc R . . H73B H -0.0244 -0.4099 1.1232 0.083 Uiso 1 1 calc R . . N74 N -0.1725(6) -0.3762(4) 1.1660(4) 0.0552(18) Uani 1 1 d D . . H74N H -0.185(7) -0.327(3) 1.134(4) 0.08(3) Uiso 1 1 d D . . C75 C -0.2267(8) -0.4002(5) 1.2322(6) 0.065(3) Uani 1 1 d . . . O75 O -0.2180(6) -0.4681(4) 1.2666(4) 0.090(2) Uani 1 1 d . . . C76 C -0.2983(7) -0.3390(5) 1.2688(5) 0.058(2) Uani 1 1 d . . . N77 N -0.3111(5) -0.2687(4) 1.2293(4) 0.0509(17) Uani 1 1 d . . . C78 C -0.3726(6) -0.2142(5) 1.2609(5) 0.055(2) Uani 1 1 d . . . C79 C -0.4229(8) -0.2276(7) 1.3360(5) 0.073(3) Uani 1 1 d . . . H79A H -0.4657 -0.1872 1.3581 0.088 Uiso 1 1 calc R . . C80 C -0.4075(8) -0.3003(8) 1.3751(5) 0.083(4) Uani 1 1 d . . . H80A H -0.4394 -0.3109 1.4254 0.100 Uiso 1 1 calc R . . C81 C -0.3479(8) -0.3567(7) 1.3432(5) 0.076(3) Uani 1 1 d . . . H81A H -0.3389 -0.4079 1.3700 0.091 Uiso 1 1 calc R . . C82 C -0.3917(7) -0.1357(5) 1.2140(5) 0.058(2) Uani 1 1 d . . . O82 O -0.4590(5) -0.0856(4) 1.2399(3) 0.0671(17) Uani 1 1 d . . . N83 N -0.3334(5) -0.1266(4) 1.1470(4) 0.0512(17) Uani 1 1 d D . . H83N H -0.289(6) -0.175(3) 1.142(5) 0.08(3) Uiso 1 1 d D . . C84 C -0.3548(7) -0.0609(5) 1.0919(5) 0.057(2) Uani 1 1 d . . . H84A H -0.2894 -0.0401 1.0638 0.069 Uiso 1 1 calc R . . H84B H -0.3989 -0.0192 1.1158 0.069 Uiso 1 1 calc R . . C85 C -0.4070(6) -0.0826(4) 1.0410(4) 0.0464(19) Uani 1 1 d . . . C86 C -0.5000(7) -0.1163(5) 1.0699(4) 0.051(2) Uani 1 1 d . . . H86A H -0.5273 -0.1253 1.1208 0.062 Uiso 1 1 calc R . . C87 C -0.5513(6) -0.1363(5) 1.0268(4) 0.050(2) Uani 1 1 d . . . H87A H -0.6146 -0.1580 1.0479 0.060 Uiso 1 1 calc R . . C88 C -0.5133(6) -0.1256(4) 0.9524(5) 0.049(2) Uani 1 1 d . . . C89 C -0.4205(7) -0.0935(5) 0.9223(4) 0.050(2) Uani 1 1 d . . . H89A H -0.3925 -0.0856 0.8714 0.060 Uiso 1 1 calc R . . C90 C -0.3694(7) -0.0732(4) 0.9677(5) 0.051(2) Uani 1 1 d . . . H90A H -0.3058 -0.0519 0.9469 0.061 Uiso 1 1 calc R . . O91 O -0.5696(5) -0.1476(3) 0.9126(3) 0.0564(15) Uani 1 1 d . . . C92 C -0.5360(7) -0.1346(5) 0.8367(5) 0.060(2) Uani 1 1 d . . . H92A H -0.4687 -0.1651 0.8219 0.072 Uiso 1 1 calc R . . H92B H -0.5278 -0.0787 0.8178 0.072 Uiso 1 1 calc R . . C93 C -0.6154(9) -0.1597(9) 0.8060(6) 0.094(4) Uani 1 1 d . . . H93A H -0.6128 -0.2172 0.8176 0.113 Uiso 1 1 calc R . . H93B H -0.6845 -0.1383 0.8306 0.113 Uiso 1 1 calc R . . C94 C -0.6015(11) -0.1341(8) 0.7253(7) 0.105(4) Uani 1 1 d . . . H94A H -0.5280 -0.1442 0.7013 0.126 Uiso 1 1 calc R . . H94B H -0.6406 -0.1658 0.7079 0.126 Uiso 1 1 calc R . . C95 C -0.6337(11) -0.0553(7) 0.7049(7) 0.097(4) Uani 1 1 d . . . H95A H -0.5939 -0.0240 0.7222 0.117 Uiso 1 1 calc R . . H95B H -0.7068 -0.0454 0.7301 0.117 Uiso 1 1 calc R . . C96 C -0.6227(12) -0.0256(9) 0.6218(8) 0.121(5) Uani 1 1 d . . . H96A H -0.5510 -0.0383 0.5954 0.145 Uiso 1 1 calc R . . H96B H -0.6678 -0.0525 0.6046 0.145 Uiso 1 1 calc R . . C97 C -0.6510(10) 0.0603(7) 0.6058(6) 0.093(4) Uani 1 1 d . . . H97A H -0.7218 0.0715 0.6346 0.111 Uiso 1 1 calc R . . H97B H -0.6052 0.0856 0.6239 0.111 Uiso 1 1 calc R . . C98 C -0.6471(10) 0.0978(8) 0.5320(7) 0.098(4) Uani 1 1 d . . . H98A H -0.7010 0.0787 0.5164 0.117 Uiso 1 1 calc R . . H98B H -0.5801 0.0797 0.5018 0.117 Uiso 1 1 calc R . . C99 C -0.6597(10) 0.1846(7) 0.5144(6) 0.091(4) Uani 1 1 d . . . H99A H -0.7198 0.2025 0.5510 0.109 Uiso 1 1 calc R . . H99B H -0.5988 0.2027 0.5223 0.109 Uiso 1 1 calc R . . C100 C -0.6731(11) 0.2261(7) 0.4439(8) 0.104(5) Uani 1 1 d . . . H10A H -0.7306 0.2054 0.4339 0.125 Uiso 1 1 calc R . . H10B H -0.6104 0.2124 0.4072 0.125 Uiso 1 1 calc R . . C101 C -0.6932(9) 0.3111(7) 0.4316(6) 0.077(3) Uani 1 1 d . . . H10C H -0.6967 0.3304 0.3805 0.093 Uiso 1 1 calc R . . H10D H -0.7606 0.3263 0.4630 0.093 Uiso 1 1 calc R . . O102 O -0.6157(5) 0.3471(4) 0.4465(3) 0.0729(19) Uani 1 1 d . . . C103 C -0.5244(8) 0.3507(5) 0.3983(5) 0.061(2) Uani 1 1 d . . . C104 C -0.5002(8) 0.3318(5) 0.3284(5) 0.066(3) Uani 1 1 d . . . H10E H -0.5509 0.3152 0.3111 0.079 Uiso 1 1 calc R . . C105 C -0.4027(8) 0.3378(5) 0.2859(5) 0.062(2) Uani 1 1 d . . . H10F H -0.3868 0.3253 0.2388 0.074 Uiso 1 1 calc R . . C106 C -0.3251(7) 0.3621(5) 0.3097(6) 0.063(2) Uani 1 1 d . . . C107 C -0.3540(8) 0.3856(5) 0.3761(5) 0.065(3) Uani 1 1 d . . . H10G H -0.3048 0.4059 0.3921 0.078 Uiso 1 1 calc R . . C108 C -0.4511(8) 0.3807(6) 0.4199(5) 0.063(2) Uani 1 1 d . . . H10H H -0.4683 0.3979 0.4651 0.075 Uiso 1 1 calc R . . N111 N -0.2356(9) 0.3320(7) 0.0950(6) 0.101(3) Uani 1 1 d . . . C111 C -0.2400(9) 0.3060(6) 0.0455(6) 0.077(3) Uani 1 1 d . . . C112 C -0.2365(9) 0.2719(7) -0.0123(7) 0.088(3) Uani 1 1 d . . . H11A H -0.1676 0.2455 -0.0280 0.132 Uiso 1 1 calc R . . H11B H -0.2524 0.3120 -0.0523 0.132 Uiso 1 1 calc R . . H11C H -0.2870 0.2339 0.0022 0.132 Uiso 1 1 calc R . . N113 N 0.5974(8) 0.4371(6) -0.0536(6) 0.089(3) Uani 1 1 d . . . C113 C 0.5512(9) 0.4825(7) -0.0897(6) 0.074(3) Uani 1 1 d . . . C114 C 0.4929(9) 0.5372(6) -0.1331(7) 0.085(3) Uani 1 1 d . . . H11D H 0.4847 0.5137 -0.1723 0.127 Uiso 1 1 calc R . . H11E H 0.5288 0.5839 -0.1539 0.127 Uiso 1 1 calc R . . H11F H 0.4251 0.5516 -0.1030 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0516(4) 0.0404(4) 0.0492(4) -0.0072(3) -0.0087(3) 0.0049(3) C1 0.043(5) 0.051(5) 0.062(5) -0.009(4) -0.007(4) 0.008(4) N2 0.050(4) 0.032(3) 0.051(4) -0.003(3) -0.011(3) 0.007(3) C3 0.051(5) 0.032(4) 0.054(5) -0.005(3) -0.019(4) 0.011(3) O3 0.055(3) 0.042(3) 0.050(3) -0.009(2) -0.013(3) 0.005(3) C4 0.041(4) 0.025(3) 0.064(5) -0.006(3) -0.013(4) 0.008(3) N5 0.057(4) 0.032(3) 0.049(4) -0.003(3) -0.019(3) 0.007(3) C6 0.055(5) 0.036(4) 0.070(6) -0.009(4) -0.025(5) 0.006(4) C7 0.049(5) 0.031(4) 0.073(6) -0.007(4) -0.021(4) 0.001(4) C8 0.049(5) 0.031(4) 0.067(6) 0.006(4) -0.003(4) -0.005(4) C9 0.055(5) 0.031(4) 0.055(5) -0.001(3) -0.016(4) 0.004(4) C10 0.072(6) 0.036(4) 0.062(5) -0.016(4) -0.027(5) 0.020(4) O10 0.071(4) 0.053(4) 0.079(4) -0.025(3) -0.032(4) 0.003(3) N11 0.060(4) 0.042(4) 0.050(4) -0.012(3) -0.017(3) -0.001(3) C12 0.066(6) 0.050(5) 0.066(6) -0.020(4) -0.020(5) 0.005(4) C13 0.061(6) 0.053(5) 0.050(5) -0.009(4) -0.017(4) 0.002(4) C14 0.054(5) 0.058(5) 0.053(5) -0.005(4) -0.005(4) -0.004(4) C15 0.051(5) 0.061(6) 0.061(6) -0.003(4) -0.006(4) 0.003(4) C16 0.068(6) 0.047(5) 0.056(5) -0.004(4) -0.009(5) 0.000(4) C17 0.070(6) 0.066(6) 0.051(5) -0.004(4) -0.001(5) -0.001(5) C18 0.056(6) 0.072(6) 0.061(6) -0.020(5) -0.013(5) 0.008(5) O19 0.076(4) 0.050(4) 0.062(4) 0.002(3) 0.013(3) 0.009(3) C20 0.100(9) 0.056(6) 0.079(7) 0.000(5) 0.024(6) 0.013(6) C21 0.093(9) 0.061(7) 0.089(8) 0.002(6) 0.010(7) 0.013(6) C22 0.150(13) 0.058(7) 0.072(8) -0.011(6) -0.008(8) 0.007(7) C23 0.120(12) 0.076(8) 0.097(10) -0.003(7) 0.005(8) -0.002(8) C24 0.110(10) 0.089(9) 0.080(8) -0.033(7) 0.002(7) 0.000(7) C25 0.105(11) 0.069(8) 0.128(12) 0.010(8) -0.016(9) 0.004(7) C26 0.142(15) 0.120(13) 0.107(11) 0.012(9) -0.031(11) -0.039(11) C27 0.20(2) 0.079(12) 0.69(7) -0.07(2) -0.30(3) 0.035(13) C28 0.173(8) 0.173(8) 0.173(8) -0.0314(17) -0.042(2) -0.0183(13) C29 0.118(12) 0.121(12) 0.161(16) 0.048(11) -0.064(12) -0.032(10) O30 0.091(6) 0.056(4) 0.149(8) 0.018(5) -0.055(6) -0.027(4) C31 0.058(6) 0.057(6) 0.103(8) 0.001(6) -0.037(6) -0.009(5) C32 0.072(7) 0.082(8) 0.079(7) 0.017(6) -0.014(6) -0.030(6) C33 0.053(5) 0.066(6) 0.060(5) 0.002(5) -0.008(4) -0.005(5) C34 0.043(5) 0.052(5) 0.057(5) -0.010(4) -0.020(4) -0.004(4) C35 0.055(5) 0.046(5) 0.068(6) -0.013(4) -0.015(4) -0.004(4) C36 0.060(6) 0.047(5) 0.093(7) -0.019(5) -0.033(6) 0.005(4) C37 0.088(7) 0.040(5) 0.063(6) -0.002(4) -0.011(5) 0.012(5) O38 0.073(4) 0.048(3) 0.070(4) -0.003(3) 0.006(3) 0.010(3) C39 0.056(5) 0.050(5) 0.067(6) -0.007(4) 0.004(5) 0.008(4) C40 0.056(5) 0.053(5) 0.051(5) -0.010(4) -0.012(4) 0.011(4) N41 0.044(4) 0.042(4) 0.040(3) -0.003(3) -0.006(3) 0.003(3) C42 0.047(5) 0.050(5) 0.043(4) -0.006(4) -0.007(4) -0.002(4) C43 0.056(5) 0.045(5) 0.059(5) -0.005(4) -0.007(4) 0.002(4) C44 0.073(6) 0.050(5) 0.056(5) -0.003(4) 0.006(5) -0.008(5) C45 0.062(6) 0.054(5) 0.059(6) -0.002(4) 0.011(5) -0.001(5) C46 0.048(5) 0.038(4) 0.056(5) -0.004(4) -0.002(4) -0.002(4) O47 0.049(3) 0.039(3) 0.047(3) 0.001(2) -0.001(3) 0.002(2) C48 0.052(5) 0.050(5) 0.066(6) -0.005(4) 0.002(4) 0.009(4) C49 0.044(5) 0.046(5) 0.055(5) -0.003(4) -0.001(4) 0.008(4) C50 0.067(6) 0.040(4) 0.057(5) -0.013(4) -0.005(5) 0.002(4) C51 0.059(5) 0.061(6) 0.053(5) -0.004(4) -0.016(4) 0.007(4) C52 0.074(6) 0.038(4) 0.061(5) -0.011(4) -0.016(5) -0.002(4) C53 0.077(7) 0.056(5) 0.063(6) -0.007(4) -0.030(5) 0.003(5) C54 0.062(6) 0.047(5) 0.068(6) 0.007(4) -0.018(5) 0.003(4) O55 0.096(5) 0.039(3) 0.071(4) -0.008(3) -0.027(4) 0.007(3) C56 0.085(7) 0.053(5) 0.061(6) -0.001(4) -0.027(5) 0.017(5) C57 0.081(7) 0.051(5) 0.072(6) 0.002(5) -0.025(6) 0.006(5) C58 0.088(8) 0.067(6) 0.062(6) 0.001(5) -0.031(6) 0.001(6) C59 0.097(9) 0.090(8) 0.059(6) -0.002(6) -0.026(6) -0.004(7) C60 0.088(8) 0.082(7) 0.058(6) -0.007(5) -0.032(6) -0.012(6) C61 0.078(8) 0.139(12) 0.072(7) -0.028(7) -0.020(6) -0.017(8) C62 0.102(9) 0.090(8) 0.057(6) -0.014(6) -0.022(6) -0.016(7) C63 0.089(8) 0.090(8) 0.074(7) -0.025(6) -0.023(6) -0.009(6) C64 0.074(7) 0.062(6) 0.076(7) -0.015(5) -0.024(5) -0.007(5) C65 0.073(6) 0.046(5) 0.070(6) -0.008(4) -0.014(5) -0.008(5) O66 0.074(4) 0.056(4) 0.061(4) -0.013(3) -0.014(3) -0.005(3) C67 0.061(5) 0.038(4) 0.055(5) -0.006(4) -0.017(4) 0.011(4) C68 0.051(5) 0.039(5) 0.078(7) -0.003(4) -0.009(5) 0.000(4) C69 0.060(6) 0.035(4) 0.095(8) -0.010(5) -0.040(6) 0.008(4) C70 0.056(5) 0.039(4) 0.072(6) -0.012(4) -0.029(5) 0.019(4) C71 0.049(5) 0.046(5) 0.053(5) -0.005(4) -0.006(4) 0.003(4) C72 0.055(5) 0.041(4) 0.053(5) -0.011(4) -0.021(4) 0.008(4) C73 0.082(7) 0.051(5) 0.088(7) -0.022(5) -0.051(6) 0.021(5) N74 0.070(5) 0.039(4) 0.053(4) -0.005(3) -0.021(4) 0.012(3) C75 0.066(6) 0.051(5) 0.081(7) 0.001(5) -0.037(6) -0.001(5) O75 0.109(6) 0.055(4) 0.100(6) 0.021(4) -0.044(5) -0.004(4) C76 0.058(5) 0.056(5) 0.056(5) 0.006(4) -0.021(4) -0.005(4) N77 0.049(4) 0.047(4) 0.055(4) -0.002(3) -0.017(3) -0.001(3) C78 0.045(5) 0.066(6) 0.052(5) -0.005(4) -0.015(4) -0.005(4) C79 0.059(6) 0.099(8) 0.047(5) -0.005(5) -0.003(5) 0.001(6) C80 0.067(7) 0.128(10) 0.037(5) 0.015(6) -0.008(5) -0.008(7) C81 0.065(6) 0.091(8) 0.057(6) 0.019(6) -0.022(5) 0.000(6) C82 0.057(5) 0.053(5) 0.071(6) -0.018(4) -0.027(5) 0.008(4) O82 0.066(4) 0.072(4) 0.065(4) -0.032(3) -0.016(3) 0.014(3) N83 0.053(4) 0.041(4) 0.051(4) -0.010(3) -0.004(3) 0.008(3) C84 0.063(6) 0.037(4) 0.062(5) -0.006(4) -0.006(5) 0.003(4) C85 0.051(5) 0.031(4) 0.050(5) -0.003(3) -0.008(4) 0.003(3) C86 0.059(5) 0.046(5) 0.042(4) -0.009(4) -0.009(4) 0.009(4) C87 0.048(5) 0.049(5) 0.043(4) -0.004(4) 0.001(4) 0.001(4) C88 0.052(5) 0.033(4) 0.059(5) -0.007(4) -0.014(4) 0.010(4) C89 0.061(5) 0.043(4) 0.039(4) -0.005(3) -0.010(4) 0.006(4) C90 0.055(5) 0.032(4) 0.054(5) 0.001(3) -0.002(4) 0.001(4) O91 0.061(4) 0.047(3) 0.054(3) -0.007(3) -0.008(3) 0.006(3) C92 0.073(6) 0.041(5) 0.059(5) -0.001(4) -0.015(5) 0.002(4) C93 0.084(8) 0.142(12) 0.061(7) -0.033(7) -0.007(6) -0.028(8) C94 0.099(9) 0.120(11) 0.091(9) -0.020(8) -0.036(8) 0.031(8) C95 0.109(10) 0.077(8) 0.097(9) 0.012(7) -0.025(8) -0.020(7) C96 0.099(10) 0.122(12) 0.118(12) 0.017(10) -0.020(9) -0.007(9) C97 0.095(9) 0.100(9) 0.077(8) 0.024(7) -0.032(7) -0.029(7) C98 0.092(9) 0.107(10) 0.096(9) -0.003(8) -0.035(8) -0.016(8) C99 0.110(10) 0.086(8) 0.074(7) 0.022(6) -0.035(7) -0.025(7) C100 0.123(11) 0.081(8) 0.126(11) 0.018(7) -0.071(9) -0.044(8) C101 0.081(7) 0.085(8) 0.068(6) 0.006(6) -0.029(6) -0.024(6) O102 0.074(5) 0.083(5) 0.056(4) 0.004(3) -0.018(4) -0.011(4) C103 0.064(6) 0.059(6) 0.060(6) -0.005(4) -0.025(5) 0.001(5) C104 0.072(7) 0.058(6) 0.065(6) -0.001(5) -0.025(5) -0.003(5) C105 0.082(7) 0.041(5) 0.067(6) -0.004(4) -0.034(6) 0.001(5) C106 0.058(6) 0.037(4) 0.081(7) -0.002(4) -0.011(5) 0.009(4) C107 0.073(7) 0.056(6) 0.073(6) -0.018(5) -0.033(6) 0.007(5) C108 0.067(6) 0.063(6) 0.056(5) -0.002(4) -0.017(5) -0.003(5) N111 0.113(9) 0.099(8) 0.094(8) -0.021(6) -0.013(7) -0.035(7) C111 0.089(8) 0.069(7) 0.071(7) -0.018(6) -0.008(6) -0.016(6) C112 0.087(8) 0.093(8) 0.090(8) -0.028(7) -0.030(7) 0.004(7) N113 0.083(7) 0.091(7) 0.087(7) 0.000(6) -0.015(6) -0.024(6) C113 0.087(8) 0.069(7) 0.070(7) -0.010(5) -0.022(6) -0.018(6) C114 0.095(8) 0.068(7) 0.091(8) -0.009(6) -0.028(7) -0.010(6) _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 N5 1.925(7) . ? Pd1 N11 2.037(7) . ? Pd1 N2 2.062(7) . ? Pd1 N41 2.081(6) . ? C1 N2 1.456(11) . ? C1 C34 1.504(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C3 1.345(10) . ? C3 O3 1.249(9) . ? C3 C4 1.499(12) . ? C4 N5 1.332(10) . ? C4 C9 1.370(11) . ? N5 C6 1.337(11) . ? C6 C7 1.377(12) . ? C6 C10 1.516(12) . ? C7 C8 1.376(12) . ? C7 H7A 0.9500 . ? C8 C9 1.381(12) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 O10 1.235(11) . ? C10 N11 1.342(12) . ? N11 C12 1.444(11) . ? C12 C13 1.506(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.377(13) . ? C13 C14 1.388(12) . ? C14 C15 1.383(12) . ? C14 H14A 0.9500 . ? C15 C16 1.366(12) . ? C15 H15A 0.9500 . ? C16 O19 1.384(10) . ? C16 C17 1.389(13) . ? C17 C18 1.385(13) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O19 C20 1.418(11) . ? C20 C21 1.559(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.550(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.433(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.556(19) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.527(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.410(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.83(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.42(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.397(19) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O30 1.371(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C31 1.382(12) . ? C31 C36 1.366(14) . ? C31 C32 1.378(16) . ? C32 C33 1.397(14) . ? C32 H32A 0.9500 . ? C33 C34 1.372(12) . ? C33 H33A 0.9500 . ? C34 C35 1.411(12) . ? C35 C36 1.376(12) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 O38 1.446(10) . ? C37 C106 1.478(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O38 C39 1.394(10) . ? C39 C40 1.518(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C45 1.366(12) . ? C40 N41 1.366(10) . ? N41 C42 1.338(10) . ? C42 C43 1.379(11) . ? C42 C46 1.492(11) . ? C43 C44 1.385(12) . ? C43 H43A 0.9500 . ? C44 C45 1.368(12) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 O47 1.430(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O47 C48 1.425(9) . ? C48 C49 1.492(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.374(13) . ? C49 C50 1.371(12) . ? C50 C51 1.407(12) . ? C50 H50A 0.9500 . ? C51 C52 1.382(13) . ? C51 H51A 0.9500 . ? C52 C53 1.368(13) . ? C52 O55 1.369(10) . ? C53 C54 1.382(12) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? O55 C56 1.454(11) . ? C56 C57 1.520(14) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.501(14) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.513(14) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.541(15) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.480(14) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.491(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.526(14) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.474(15) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.550(13) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O66 1.384(11) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O66 C67 1.363(10) . ? C67 C68 1.372(13) . ? C67 C72 1.406(12) . ? C68 C69 1.366(13) . ? C68 H68A 0.9500 . ? C69 C70 1.381(13) . ? C69 H69A 0.9500 . ? C70 C71 1.378(12) . ? C70 C73 1.492(13) . ? C71 C72 1.396(11) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 N74 1.457(11) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? N74 C75 1.319(12) . ? N74 H74N 0.980(5) . ? C75 O75 1.248(11) . ? C75 C76 1.502(14) . ? C76 N77 1.327(10) . ? C76 C81 1.415(13) . ? N77 C78 1.317(11) . ? C78 C79 1.426(12) . ? C78 C82 1.515(12) . ? C79 C80 1.363(15) . ? C79 H79A 0.9500 . ? C80 C81 1.334(16) . ? C80 H80A 0.9500 . ? C81 H81A 0.9500 . ? C82 O82 1.251(10) . ? C82 N83 1.325(11) . ? N83 C84 1.452(10) . ? N83 H83N 0.979(5) . ? C84 C85 1.500(12) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C90 1.364(11) . ? C85 C86 1.407(12) . ? C86 C87 1.351(12) . ? C86 H86A 0.9500 . ? C87 C88 1.384(11) . ? C87 H87A 0.9500 . ? C88 O91 1.367(10) . ? C88 C89 1.394(12) . ? C89 C90 1.389(12) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? O91 C92 1.405(10) . ? C92 C93 1.523(14) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.507(16) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.397(16) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.563(18) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.493(18) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.439(15) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.492(16) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.454(15) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 C101 1.464(16) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 O102 1.429(12) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? O102 C103 1.342(11) . ? C103 C108 1.389(13) . ? C103 C104 1.411(13) . ? C104 C105 1.369(14) . ? C104 H10E 0.9500 . ? C105 C106 1.413(14) . ? C105 H10F 0.9500 . ? C106 C107 1.380(13) . ? C107 C108 1.371(13) . ? C107 H10G 0.9500 . ? C108 H10H 0.9500 . ? N111 C111 1.172(14) . ? C111 C112 1.370(15) . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? N113 C113 1.169(13) . ? C113 C114 1.431(16) . ? C114 H11D 0.9800 . ? C114 H11E 0.9800 . ? C114 H11F 0.9800 . ? 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 N5 Pd1 N11 80.7(3) . . ? N5 Pd1 N2 80.6(3) . . ? N11 Pd1 N2 161.1(3) . . ? N5 Pd1 N41 173.6(2) . . ? N11 Pd1 N41 97.0(3) . . ? N2 Pd1 N41 101.9(3) . . ? N2 C1 C34 112.2(6) . . ? N2 C1 H1A 109.2 . . ? C34 C1 H1A 109.2 . . ? N2 C1 H1B 109.2 . . ? C34 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 N2 C1 118.3(7) . . ? C3 N2 Pd1 113.6(5) . . ? C1 N2 Pd1 127.8(5) . . ? O3 C3 N2 126.6(8) . . ? O3 C3 C4 120.4(8) . . ? N2 C3 C4 113.0(7) . . ? N5 C4 C9 118.8(8) . . ? N5 C4 C3 114.7(7) . . ? C9 C4 C3 126.5(8) . . ? C4 N5 C6 123.8(8) . . ? C4 N5 Pd1 117.7(6) . . ? C6 N5 Pd1 118.2(6) . . ? N5 C6 C7 118.8(8) . . ? N5 C6 C10 113.6(8) . . ? C7 C6 C10 127.6(8) . . ? C8 C7 C6 119.1(8) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C4 C9 C8 119.5(8) . . ? C4 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? O10 C10 N11 128.6(9) . . ? O10 C10 C6 118.9(9) . . ? N11 C10 C6 112.5(8) . . ? C10 N11 C12 117.5(7) . . ? C10 N11 Pd1 114.8(6) . . ? C12 N11 Pd1 127.4(6) . . ? N11 C12 C13 115.0(7) . . ? N11 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? N11 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C18 C13 C14 117.1(8) . . ? C18 C13 C12 121.4(8) . . ? C14 C13 C12 121.4(8) . . ? C15 C14 C13 122.1(8) . . ? C15 C14 H14A 118.9 . . ? C13 C14 H14A 118.9 . . ? C16 C15 C14 119.1(8) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 O19 125.0(8) . . ? C15 C16 C17 120.7(8) . . ? O19 C16 C17 114.3(8) . . ? C16 C17 C18 118.6(9) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? C13 C18 C17 122.3(9) . . ? C13 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C16 O19 C20 116.7(7) . . ? O19 C20 C21 106.4(8) . . ? O19 C20 H20A 110.4 . . ? C21 C20 H20A 110.4 . . ? O19 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C22 C21 C20 112.4(10) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 113.2(12) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 113.0(12) . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 114.9(11) . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C26 C25 C24 116.3(14) . . ? C26 C25 H25A 108.2 . . ? C24 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? C24 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C27 108.2(15) . . ? C25 C26 H26A 110.1 . . ? C27 C26 H26A 110.1 . . ? C25 C26 H26B 110.1 . . ? C27 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? C28 C27 C26 98.0(16) . . ? C28 C27 H27A 112.2 . . ? C26 C27 H27A 112.2 . . ? C28 C27 H27B 112.2 . . ? C26 C27 H27B 112.2 . . ? H27A C27 H27B 109.8 . . ? C29 C28 C27 104(2) . . ? C29 C28 H28A 110.9 . . ? C27 C28 H28A 110.9 . . ? C29 C28 H28B 110.8 . . ? C27 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? C28 C29 O30 112.3(16) . . ? C28 C29 H29A 109.1 . . ? O30 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? O30 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? C31 O30 C29 120.5(12) . . ? C36 C31 C32 121.5(9) . . ? C36 C31 O30 114.1(10) . . ? C32 C31 O30 124.4(10) . . ? C31 C32 C33 118.6(9) . . ? C31 C32 H32A 120.7 . . ? C33 C32 H32A 120.7 . . ? C34 C33 C32 122.0(9) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C35 116.9(8) . . ? C33 C34 C1 122.8(8) . . ? C35 C34 C1 120.2(8) . . ? C36 C35 C34 121.9(9) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C31 C36 C35 118.9(9) . . ? C31 C36 H36A 120.5 . . ? C35 C36 H36A 120.5 . . ? O38 C37 C106 104.6(7) . . ? O38 C37 H37A 110.8 . . ? C106 C37 H37A 110.8 . . ? O38 C37 H37B 110.8 . . ? C106 C37 H37B 110.8 . . ? H37A C37 H37B 108.9 . . ? C39 O38 C37 112.8(7) . . ? O38 C39 C40 105.6(7) . . ? O38 C39 H39A 110.6 . . ? C40 C39 H39A 110.6 . . ? O38 C39 H39B 110.6 . . ? C40 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? C45 C40 N41 121.4(8) . . ? C45 C40 C39 122.8(8) . . ? N41 C40 C39 115.8(7) . . ? C42 N41 C40 118.9(7) . . ? C42 N41 Pd1 119.4(5) . . ? C40 N41 Pd1 121.5(5) . . ? N41 C42 C43 121.5(7) . . ? N41 C42 C46 116.3(7) . . ? C43 C42 C46 122.2(7) . . ? C42 C43 C44 119.4(8) . . ? C42 C43 H43A 120.3 . . ? C44 C43 H43A 120.3 . . ? C45 C44 C43 119.0(8) . . ? C45 C44 H44A 120.5 . . ? C43 C44 H44A 120.5 . . ? C40 C45 C44 119.8(9) . . ? C40 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? O47 C46 C42 110.4(6) . . ? O47 C46 H46A 109.6 . . ? C42 C46 H46A 109.6 . . ? O47 C46 H46B 109.6 . . ? C42 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C48 O47 C46 108.9(6) . . ? O47 C48 C49 112.0(7) . . ? O47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? O47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C54 C49 C50 118.7(8) . . ? C54 C49 C48 121.8(8) . . ? C50 C49 C48 119.3(9) . . ? C49 C50 C51 120.6(9) . . ? C49 C50 H50A 119.7 . . ? C51 C50 H50A 119.7 . . ? C52 C51 C50 119.9(8) . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C53 C52 O55 116.8(8) . . ? C53 C52 C51 118.7(8) . . ? O55 C52 C51 124.4(8) . . ? C52 C53 C54 121.2(9) . . ? C52 C53 H53A 119.4 . . ? C54 C53 H53A 119.4 . . ? C49 C54 C53 120.9(9) . . ? C49 C54 H54A 119.6 . . ? C53 C54 H54A 119.6 . . ? C52 O55 C56 118.4(7) . . ? O55 C56 C57 112.3(8) . . ? O55 C56 H56A 109.1 . . ? C57 C56 H56A 109.1 . . ? O55 C56 H56B 109.1 . . ? C57 C56 H56B 109.1 . . ? H56A C56 H56B 107.9 . . ? C58 C57 C56 114.4(9) . . ? C58 C57 H57A 108.7 . . ? C56 C57 H57A 108.7 . . ? C58 C57 H57B 108.7 . . ? C56 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? C57 C58 C59 111.4(9) . . ? C57 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? C57 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C58 C59 C60 115.7(9) . . ? C58 C59 H59A 108.4 . . ? C60 C59 H59A 108.4 . . ? C58 C59 H59B 108.4 . . ? C60 C59 H59B 108.4 . . ? H59A C59 H59B 107.4 . . ? C61 C60 C59 113.4(9) . . ? C61 C60 H60A 108.9 . . ? C59 C60 H60A 108.9 . . ? C61 C60 H60B 108.9 . . ? C59 C60 H60B 108.9 . . ? H60A C60 H60B 107.7 . . ? C60 C61 C62 116.3(10) . . ? C60 C61 H61A 108.2 . . ? C62 C61 H61A 108.2 . . ? C60 C61 H61B 108.2 . . ? C62 C61 H61B 108.2 . . ? H61A C61 H61B 107.4 . . ? C61 C62 C63 114.1(10) . . ? C61 C62 H62A 108.7 . . ? C63 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C63 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? C64 C63 C62 116.2(10) . . ? C64 C63 H63A 108.2 . . ? C62 C63 H63A 108.2 . . ? C64 C63 H63B 108.2 . . ? C62 C63 H63B 108.2 . . ? H63A C63 H63B 107.4 . . ? C63 C64 C65 112.4(9) . . ? C63 C64 H64A 109.1 . . ? C65 C64 H64A 109.1 . . ? C63 C64 H64B 109.1 . . ? C65 C64 H64B 109.1 . . ? H64A C64 H64B 107.9 . . ? O66 C65 C64 107.4(8) . . ? O66 C65 H65A 110.2 . . ? C64 C65 H65A 110.2 . . ? O66 C65 H65B 110.2 . . ? C64 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? C67 O66 C65 117.6(7) . . ? O66 C67 C68 115.4(8) . . ? O66 C67 C72 124.8(8) . . ? C68 C67 C72 119.8(8) . . ? C69 C68 C67 121.2(9) . . ? C69 C68 H68A 119.4 . . ? C67 C68 H68A 119.4 . . ? C68 C69 C70 121.4(9) . . ? C68 C69 H69A 119.3 . . ? C70 C69 H69A 119.3 . . ? C71 C70 C69 117.3(8) . . ? C71 C70 C73 121.8(9) . . ? C69 C70 C73 120.9(9) . . ? C70 C71 C72 123.3(8) . . ? C70 C71 H71A 118.4 . . ? C72 C71 H71A 118.4 . . ? C71 C72 C67 117.1(8) . . ? C71 C72 H72A 121.5 . . ? C67 C72 H72A 121.5 . . ? N74 C73 C70 112.8(7) . . ? N74 C73 H73A 109.0 . . ? C70 C73 H73A 109.0 . . ? N74 C73 H73B 109.0 . . ? C70 C73 H73B 109.0 . . ? H73A C73 H73B 107.8 . . ? C75 N74 C73 122.1(8) . . ? C75 N74 H74N 127(6) . . ? C73 N74 H74N 110(6) . . ? O75 C75 N74 124.5(10) . . ? O75 C75 C76 119.1(10) . . ? N74 C75 C76 116.3(8) . . ? N77 C76 C81 122.2(9) . . ? N77 C76 C75 117.6(8) . . ? C81 C76 C75 120.2(9) . . ? C78 N77 C76 118.4(8) . . ? N77 C78 C79 122.2(9) . . ? N77 C78 C82 117.8(8) . . ? C79 C78 C82 120.0(9) . . ? C80 C79 C78 117.9(10) . . ? C80 C79 H79A 121.1 . . ? C78 C79 H79A 121.1 . . ? C81 C80 C79 120.4(9) . . ? C81 C80 H80A 119.8 . . ? C79 C80 H80A 119.8 . . ? C80 C81 C76 118.9(10) . . ? C80 C81 H81A 120.6 . . ? C76 C81 H81A 120.6 . . ? O82 C82 N83 125.3(8) . . ? O82 C82 C78 119.6(9) . . ? N83 C82 C78 115.1(7) . . ? C82 N83 C84 121.5(7) . . ? C82 N83 H83N 107(6) . . ? C84 N83 H83N 130(6) . . ? N83 C84 C85 112.5(7) . . ? N83 C84 H84A 109.1 . . ? C85 C84 H84A 109.1 . . ? N83 C84 H84B 109.1 . . ? C85 C84 H84B 109.1 . . ? H84A C84 H84B 107.8 . . ? C90 C85 C86 116.9(8) . . ? C90 C85 C84 124.3(8) . . ? C86 C85 C84 118.8(7) . . ? C87 C86 C85 121.6(8) . . ? C87 C86 H86A 119.2 . . ? C85 C86 H86A 119.2 . . ? C86 C87 C88 121.2(8) . . ? C86 C87 H87A 119.4 . . ? C88 C87 H87A 119.4 . . ? O91 C88 C87 117.6(8) . . ? O91 C88 C89 123.8(8) . . ? C87 C88 C89 118.6(8) . . ? C90 C89 C88 119.1(8) . . ? C90 C89 H89A 120.4 . . ? C88 C89 H89A 120.4 . . ? C85 C90 C89 122.6(8) . . ? C85 C90 H90A 118.7 . . ? C89 C90 H90A 118.7 . . ? C88 O91 C92 119.3(7) . . ? O91 C92 C93 108.5(8) . . ? O91 C92 H92A 110.0 . . ? C93 C92 H92A 110.0 . . ? O91 C92 H92B 110.0 . . ? C93 C92 H92B 110.0 . . ? H92A C92 H92B 108.4 . . ? C94 C93 C92 114.5(11) . . ? C94 C93 H93A 108.6 . . ? C92 C93 H93A 108.6 . . ? C94 C93 H93B 108.6 . . ? C92 C93 H93B 108.6 . . ? H93A C93 H93B 107.6 . . ? C95 C94 C93 113.5(12) . . ? C95 C94 H94A 108.9 . . ? C93 C94 H94A 108.9 . . ? C95 C94 H94B 108.9 . . ? C93 C94 H94B 108.9 . . ? H94A C94 H94B 107.7 . . ? C94 C95 C96 115.9(12) . . ? C94 C95 H95A 108.3 . . ? C96 C95 H95A 108.3 . . ? C94 C95 H95B 108.3 . . ? C96 C95 H95B 108.3 . . ? H95A C95 H95B 107.4 . . ? C97 C96 C95 111.1(13) . . ? C97 C96 H96A 109.4 . . ? C95 C96 H96A 109.4 . . ? C97 C96 H96B 109.4 . . ? C95 C96 H96B 109.4 . . ? H96A C96 H96B 108.0 . . ? C98 C97 C96 118.9(13) . . ? C98 C97 H97A 107.6 . . ? C96 C97 H97A 107.6 . . ? C98 C97 H97B 107.6 . . ? C96 C97 H97B 107.6 . . ? H97A C97 H97B 107.0 . . ? C97 C98 C99 118.8(12) . . ? C97 C98 H98A 107.6 . . ? C99 C98 H98A 107.6 . . ? C97 C98 H98B 107.6 . . ? C99 C98 H98B 107.6 . . ? H98A C98 H98B 107.0 . . ? C100 C99 C98 121.7(12) . . ? C100 C99 H99A 106.9 . . ? C98 C99 H99A 106.9 . . ? C100 C99 H99B 106.9 . . ? C98 C99 H99B 106.9 . . ? H99A C99 H99B 106.7 . . ? C99 C100 C101 119.2(12) . . ? C99 C100 H10A 107.5 . . ? C101 C100 H10A 107.5 . . ? C99 C100 H10B 107.5 . . ? C101 C100 H10B 107.5 . . ? H10A C100 H10B 107.0 . . ? O102 C101 C100 112.1(9) . . ? O102 C101 H10C 109.2 . . ? C100 C101 H10C 109.2 . . ? O102 C101 H10D 109.2 . . ? C100 C101 H10D 109.2 . . ? H10C C101 H10D 107.9 . . ? C103 O102 C101 118.6(8) . . ? O102 C103 C108 114.6(9) . . ? O102 C103 C104 126.2(9) . . ? C108 C103 C104 119.1(9) . . ? C105 C104 C103 119.1(10) . . ? C105 C104 H10E 120.4 . . ? C103 C104 H10E 120.4 . . ? C104 C105 C106 122.1(10) . . ? C104 C105 H10F 118.9 . . ? C106 C105 H10F 118.9 . . ? C107 C106 C105 116.8(9) . . ? C107 C106 C37 123.3(10) . . ? C105 C106 C37 119.7(10) . . ? C108 C107 C106 122.4(9) . . ? C108 C107 H10G 118.8 . . ? C106 C107 H10G 118.8 . . ? C107 C108 C103 120.1(9) . . ? C107 C108 H10H 120.0 . . ? C103 C108 H10H 120.0 . . ? N111 C111 C112 174.7(14) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? N113 C113 C114 178.8(13) . . ? C113 C114 H11D 109.5 . . ? C113 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C113 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? 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 C34 C1 N2 C3 112.3(8) . . . . ? C34 C1 N2 Pd1 -74.0(8) . . . . ? N5 Pd1 N2 C3 4.3(5) . . . . ? N11 Pd1 N2 C3 13.8(11) . . . . ? N41 Pd1 N2 C3 -169.7(5) . . . . ? N5 Pd1 N2 C1 -169.6(6) . . . . ? N11 Pd1 N2 C1 -160.1(7) . . . . ? N41 Pd1 N2 C1 16.4(6) . . . . ? C1 N2 C3 O3 -7.0(11) . . . . ? Pd1 N2 C3 O3 178.4(6) . . . . ? C1 N2 C3 C4 172.5(6) . . . . ? Pd1 N2 C3 C4 -2.0(7) . . . . ? O3 C3 C4 N5 176.8(6) . . . . ? N2 C3 C4 N5 -2.8(9) . . . . ? O3 C3 C4 C9 -3.5(11) . . . . ? N2 C3 C4 C9 176.9(7) . . . . ? C9 C4 N5 C6 0.3(11) . . . . ? C3 C4 N5 C6 -180.0(6) . . . . ? C9 C4 N5 Pd1 -173.0(5) . . . . ? C3 C4 N5 Pd1 6.7(8) . . . . ? N11 Pd1 N5 C4 177.0(6) . . . . ? N2 Pd1 N5 C4 -6.1(5) . . . . ? N41 Pd1 N5 C4 107(2) . . . . ? N11 Pd1 N5 C6 3.3(6) . . . . ? N2 Pd1 N5 C6 -179.8(6) . . . . ? N41 Pd1 N5 C6 -66(3) . . . . ? C4 N5 C6 C7 -0.5(11) . . . . ? Pd1 N5 C6 C7 172.8(5) . . . . ? C4 N5 C6 C10 -178.2(6) . . . . ? Pd1 N5 C6 C10 -4.9(8) . . . . ? N5 C6 C7 C8 0.1(11) . . . . ? C10 C6 C7 C8 177.5(7) . . . . ? C6 C7 C8 C9 0.4(11) . . . . ? N5 C4 C9 C8 0.2(10) . . . . ? C3 C4 C9 C8 -179.5(7) . . . . ? C7 C8 C9 C4 -0.5(11) . . . . ? N5 C6 C10 O10 -176.7(7) . . . . ? C7 C6 C10 O10 5.8(12) . . . . ? N5 C6 C10 N11 4.0(10) . . . . ? C7 C6 C10 N11 -173.5(8) . . . . ? O10 C10 N11 C12 5.3(12) . . . . ? C6 C10 N11 C12 -175.4(6) . . . . ? O10 C10 N11 Pd1 179.3(7) . . . . ? C6 C10 N11 Pd1 -1.4(8) . . . . ? N5 Pd1 N11 C10 -0.8(5) . . . . ? N2 Pd1 N11 C10 -10.3(11) . . . . ? N41 Pd1 N11 C10 173.2(5) . . . . ? N5 Pd1 N11 C12 172.5(7) . . . . ? N2 Pd1 N11 C12 163.0(7) . . . . ? N41 Pd1 N11 C12 -13.5(7) . . . . ? C10 N11 C12 C13 -108.6(9) . . . . ? Pd1 N11 C12 C13 78.2(9) . . . . ? N11 C12 C13 C18 -140.8(9) . . . . ? N11 C12 C13 C14 41.3(12) . . . . ? C18 C13 C14 C15 -0.9(14) . . . . ? C12 C13 C14 C15 177.0(9) . . . . ? C13 C14 C15 C16 -1.3(15) . . . . ? C14 C15 C16 O19 -178.1(9) . . . . ? C14 C15 C16 C17 3.1(15) . . . . ? C15 C16 C17 C18 -2.5(15) . . . . ? O19 C16 C17 C18 178.6(9) . . . . ? C14 C13 C18 C17 1.6(14) . . . . ? C12 C13 C18 C17 -176.4(9) . . . . ? C16 C17 C18 C13 0.1(15) . . . . ? C15 C16 O19 C20 -11.1(15) . . . . ? C17 C16 O19 C20 167.9(10) . . . . ? C16 O19 C20 C21 -167.7(10) . . . . ? O19 C20 C21 C22 52.1(14) . . . . ? C20 C21 C22 C23 58.9(14) . . . . ? C21 C22 C23 C24 -174.0(10) . . . . ? C22 C23 C24 C25 -177.6(11) . . . . ? C23 C24 C25 C26 -170.5(12) . . . . ? C24 C25 C26 C27 177.9(11) . . . . ? C25 C26 C27 C28 -74.5(18) . . . . ? C26 C27 C28 C29 -174.5(16) . . . . ? C27 C28 C29 O30 -136.6(18) . . . . ? C28 C29 O30 C31 -80.3(18) . . . . ? C29 O30 C31 C36 -179.8(11) . . . . ? C29 O30 C31 C32 0.9(17) . . . . ? C36 C31 C32 C33 -0.6(16) . . . . ? O30 C31 C32 C33 178.6(9) . . . . ? C31 C32 C33 C34 -0.7(16) . . . . ? C32 C33 C34 C35 3.1(14) . . . . ? C32 C33 C34 C1 179.8(9) . . . . ? N2 C1 C34 C33 122.7(9) . . . . ? N2 C1 C34 C35 -60.7(10) . . . . ? C33 C34 C35 C36 -4.4(13) . . . . ? C1 C34 C35 C36 178.8(8) . . . . ? C32 C31 C36 C35 -0.6(15) . . . . ? O30 C31 C36 C35 -179.9(8) . . . . ? C34 C35 C36 C31 3.2(14) . . . . ? C106 C37 O38 C39 171.6(9) . . . . ? C37 O38 C39 C40 -178.2(8) . . . . ? O38 C39 C40 C45 0.8(13) . . . . ? O38 C39 C40 N41 178.5(8) . . . . ? C45 C40 N41 C42 -0.2(13) . . . . ? C39 C40 N41 C42 -177.9(8) . . . . ? C45 C40 N41 Pd1 -175.4(7) . . . . ? C39 C40 N41 Pd1 6.8(10) . . . . ? N5 Pd1 N41 C42 -22(3) . . . . ? N11 Pd1 N41 C42 -90.9(6) . . . . ? N2 Pd1 N41 C42 90.3(6) . . . . ? N5 Pd1 N41 C40 153(2) . . . . ? N11 Pd1 N41 C40 84.4(6) . . . . ? N2 Pd1 N41 C40 -94.5(6) . . . . ? C40 N41 C42 C43 0.3(12) . . . . ? Pd1 N41 C42 C43 175.6(6) . . . . ? C40 N41 C42 C46 178.4(7) . . . . ? Pd1 N41 C42 C46 -6.3(10) . . . . ? N41 C42 C43 C44 -1.2(14) . . . . ? C46 C42 C43 C44 -179.1(9) . . . . ? C42 C43 C44 C45 1.9(15) . . . . ? N41 C40 C45 C44 0.9(15) . . . . ? C39 C40 C45 C44 178.5(9) . . . . ? C43 C44 C45 C40 -1.8(15) . . . . ? N41 C42 C46 O47 -176.3(7) . . . . ? C43 C42 C46 O47 1.8(12) . . . . ? C42 C46 O47 C48 176.7(7) . . . . ? C46 O47 C48 C49 -179.3(8) . . . . ? O47 C48 C49 C54 81.9(11) . . . . ? O47 C48 C49 C50 -103.9(9) . . . . ? C54 C49 C50 C51 0.7(13) . . . . ? C48 C49 C50 C51 -173.6(8) . . . . ? C49 C50 C51 C52 -1.6(13) . . . . ? C50 C51 C52 C53 1.6(14) . . . . ? C50 C51 C52 O55 179.3(8) . . . . ? O55 C52 C53 C54 -178.7(9) . . . . ? C51 C52 C53 C54 -0.8(15) . . . . ? C50 C49 C54 C53 0.1(14) . . . . ? C48 C49 C54 C53 174.3(9) . . . . ? C52 C53 C54 C49 -0.1(15) . . . . ? C53 C52 O55 C56 -173.9(9) . . . . ? C51 C52 O55 C56 8.3(13) . . . . ? C52 O55 C56 C57 69.0(11) . . . . ? O55 C56 C57 C58 47.4(11) . . . . ? C56 C57 C58 C59 173.6(8) . . . . ? C57 C58 C59 C60 172.8(9) . . . . ? C58 C59 C60 C61 -177.6(10) . . . . ? C59 C60 C61 C62 170.6(11) . . . . ? C60 C61 C62 C63 177.0(11) . . . . ? C61 C62 C63 C64 167.9(11) . . . . ? C62 C63 C64 C65 177.8(9) . . . . ? C63 C64 C65 O66 54.1(11) . . . . ? C64 C65 O66 C67 -171.6(7) . . . . ? C65 O66 C67 C68 166.3(8) . . . . ? C65 O66 C67 C72 -14.5(12) . . . . ? O66 C67 C68 C69 178.2(7) . . . . ? C72 C67 C68 C69 -1.1(12) . . . . ? C67 C68 C69 C70 0.0(13) . . . . ? C68 C69 C70 C71 0.4(12) . . . . ? C68 C69 C70 C73 179.1(8) . . . . ? C69 C70 C71 C72 0.2(12) . . . . ? C73 C70 C71 C72 -178.4(7) . . . . ? C70 C71 C72 C67 -1.2(12) . . . . ? O66 C67 C72 C71 -177.5(7) . . . . ? C68 C67 C72 C71 1.6(11) . . . . ? C71 C70 C73 N74 -71.6(11) . . . . ? C69 C70 C73 N74 109.8(10) . . . . ? C70 C73 N74 C75 128.8(10) . . . . ? C73 N74 C75 O75 -3.2(15) . . . . ? C73 N74 C75 C76 173.0(8) . . . . ? O75 C75 C76 N77 -175.5(8) . . . . ? N74 C75 C76 N77 8.1(13) . . . . ? O75 C75 C76 C81 5.8(14) . . . . ? N74 C75 C76 C81 -170.6(9) . . . . ? C81 C76 N77 C78 -0.5(13) . . . . ? C75 C76 N77 C78 -179.1(8) . . . . ? C76 N77 C78 C79 2.1(13) . . . . ? C76 N77 C78 C82 -176.2(8) . . . . ? N77 C78 C79 C80 -1.5(15) . . . . ? C82 C78 C79 C80 176.6(9) . . . . ? C78 C79 C80 C81 -0.6(17) . . . . ? C79 C80 C81 C76 2.1(17) . . . . ? N77 C76 C81 C80 -1.6(16) . . . . ? C75 C76 C81 C80 177.0(10) . . . . ? N77 C78 C82 O82 171.4(8) . . . . ? C79 C78 C82 O82 -6.9(13) . . . . ? N77 C78 C82 N83 -8.4(12) . . . . ? C79 C78 C82 N83 173.3(9) . . . . ? O82 C82 N83 C84 -11.1(14) . . . . ? C78 C82 N83 C84 168.7(8) . . . . ? C82 N83 C84 C85 -101.7(9) . . . . ? N83 C84 C85 C90 -122.1(8) . . . . ? N83 C84 C85 C86 56.5(10) . . . . ? C90 C85 C86 C87 -2.0(11) . . . . ? C84 C85 C86 C87 179.2(7) . . . . ? C85 C86 C87 C88 1.3(12) . . . . ? C86 C87 C88 O91 179.7(7) . . . . ? C86 C87 C88 C89 -0.2(12) . . . . ? O91 C88 C89 C90 -180.0(7) . . . . ? C87 C88 C89 C90 -0.1(11) . . . . ? C86 C85 C90 C89 1.8(11) . . . . ? C84 C85 C90 C89 -179.6(7) . . . . ? C88 C89 C90 C85 -0.7(12) . . . . ? C87 C88 O91 C92 177.2(7) . . . . ? C89 C88 O91 C92 -2.9(11) . . . . ? C88 O91 C92 C93 -176.5(8) . . . . ? O91 C92 C93 C94 167.9(10) . . . . ? C92 C93 C94 C95 -76.4(15) . . . . ? C93 C94 C95 C96 -179.1(12) . . . . ? C94 C95 C96 C97 -175.2(13) . . . . ? C95 C96 C97 C98 -179.0(12) . . . . ? C96 C97 C98 C99 -170.9(12) . . . . ? C97 C98 C99 C100 -170.0(13) . . . . ? C98 C99 C100 C101 175.3(12) . . . . ? C99 C100 C101 O102 55.9(16) . . . . ? C100 C101 O102 C103 75.5(12) . . . . ? C101 O102 C103 C108 -175.0(8) . . . . ? C101 O102 C103 C104 9.2(14) . . . . ? O102 C103 C104 C105 -179.3(9) . . . . ? C108 C103 C104 C105 5.0(13) . . . . ? C103 C104 C105 C106 0.3(13) . . . . ? C104 C105 C106 C107 -5.1(13) . . . . ? C104 C105 C106 C37 170.2(8) . . . . ? O38 C37 C106 C107 93.7(10) . . . . ? O38 C37 C106 C105 -81.2(10) . . . . ? C105 C106 C107 C108 4.6(13) . . . . ? C37 C106 C107 C108 -170.4(9) . . . . ? C106 C107 C108 C103 0.5(14) . . . . ? O102 C103 C108 C107 178.4(8) . . . . ? C104 C103 C108 C107 -5.5(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N74 H74N O3 0.980(5) 2.08(3) 3.038(9) 164(8) 2_556 N83 H83N O3 0.979(5) 2.17(6) 2.966(9) 138(8) 2_556 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.776 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.090