# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cheng-Yong Su' _publ_contact_author_email CESSCY@MAIL.SYSU.EDU.CN _publ_section_title ; Structural and photoluminescent studies of lanthanide complexes with tripodal triRNTB (N-substituted tris(benzimidazol-2-ylmethyl)amine): ligand substituent, anionic and secondary ligand effects ; loop_ _publ_author_name 'Cheng-Yong Su.' 'Yu Liu.' 'Wei-Sheng Liu.' 'Mei Pan.' 'Xiang-Li Zheng.' # Attachment 'Compds.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 698711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H78 Cl3 Eu N16 O13' _chemical_formula_weight 1633.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.31530(10) _cell_length_b 23.3369(2) _cell_length_c 23.6480(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.8520(10) _cell_angle_gamma 90.00 _cell_volume 7344.49(13) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 27129 _cell_measurement_theta_min 2.6063 _cell_measurement_theta_max 29.2623 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6817 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Oxford Germini S Ultra' _diffrn_measurement_method '\w and \p scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56405 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.00 _reflns_number_total 15983 _reflns_number_gt 11879 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15983 _refine_ls_number_parameters 946 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.002 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 Eu1 Eu 0.146898(13) 0.748108(6) 0.500943(7) 0.02714(7) Uani 1 1 d . . . N1 N 0.1468(2) 0.86449(12) 0.49458(12) 0.0320(7) Uani 1 1 d . . . N2 N 0.3115(2) 0.79744(12) 0.52032(12) 0.0339(6) Uani 1 1 d . . . N3 N 0.4222(2) 0.86720(13) 0.50445(13) 0.0395(7) Uani 1 1 d . . . N4 N 0.0927(2) 0.79140(12) 0.40733(12) 0.0346(7) Uani 1 1 d . . . N5 N 0.0084(2) 0.85764(12) 0.35725(12) 0.0370(7) Uani 1 1 d . . . N6 N 0.0351(2) 0.80096(11) 0.56628(12) 0.0314(6) Uani 1 1 d . . . N7 N 0.0007(2) 0.87376(12) 0.62370(12) 0.0378(7) Uani 1 1 d . . . N8 N 0.1443(2) 0.63259(12) 0.50788(11) 0.0277(6) Uani 1 1 d . . . N9 N 0.2692(2) 0.69436(12) 0.44216(12) 0.0324(6) Uani 1 1 d . . . N10 N 0.3786(2) 0.62307(13) 0.43057(13) 0.0364(7) Uani 1 1 d . . . N11 N 0.1804(2) 0.70459(11) 0.59646(12) 0.0314(6) Uani 1 1 d . . . N12 N 0.1423(2) 0.64126(12) 0.66289(12) 0.0351(7) Uani 1 1 d . . . N13 N -0.0132(2) 0.69978(11) 0.47238(12) 0.0314(6) Uani 1 1 d . . . N14 N -0.0973(2) 0.63039(12) 0.42601(11) 0.0322(6) Uani 1 1 d . . . N15 N 0.3679(5) 0.9185(3) 0.6288(3) 0.1044(19) Uani 1 1 d . . . N16 N 0.2286(4) 0.8883(3) 0.3113(3) 0.1011(19) Uani 1 1 d . . . C1 C 0.2437(3) 0.88422(15) 0.47280(17) 0.0394(9) Uani 1 1 d . . . H1A H 0.2539 0.9253 0.4818 0.047 Uiso 1 1 calc R . . H1B H 0.2438 0.8796 0.4312 0.047 Uiso 1 1 calc R . . C2 C 0.3258(3) 0.84954(15) 0.49963(15) 0.0336(8) Uani 1 1 d . . . C3 C 0.4064(3) 0.77920(16) 0.54002(15) 0.0364(8) Uani 1 1 d . . . C4 C 0.4372(3) 0.72821(19) 0.56669(17) 0.0428(9) Uani 1 1 d . . . H4A H 0.3905 0.6987 0.5743 0.051 Uiso 1 1 calc R . . C5 C 0.5365(3) 0.7225(2) 0.58136(19) 0.0536(11) Uani 1 1 d . . . H5A H 0.5592 0.6882 0.5992 0.064 Uiso 1 1 calc R . . C6 C 0.6068(3) 0.7665(2) 0.5707(2) 0.0575(12) Uani 1 1 d . . . H6A H 0.6755 0.7609 0.5814 0.069 Uiso 1 1 calc R . . C7 C 0.5782(3) 0.8171(2) 0.54539(19) 0.0533(11) Uani 1 1 d . . . H7A H 0.6250 0.8468 0.5385 0.064 Uiso 1 1 calc R . . C8 C 0.4763(3) 0.82227(16) 0.53034(16) 0.0395(8) Uani 1 1 d . . . C9 C 0.4667(3) 0.92119(18) 0.48611(19) 0.0496(11) Uani 1 1 d . . . H9A H 0.4132 0.9506 0.4825 0.060 Uiso 1 1 calc R . . H9B H 0.5160 0.9343 0.5155 0.060 Uiso 1 1 calc R . . C10 C 0.5167(5) 0.9167(2) 0.4325(3) 0.0853(18) Uani 1 1 d . . . H10A H 0.5421 0.9513 0.4175 0.102 Uiso 1 1 calc R . . C11 C 0.5301(5) 0.8720(3) 0.4035(3) 0.098(2) Uani 1 1 d U . . H11A H 0.5063 0.8361 0.4163 0.118 Uiso 1 1 calc R . . H11B H 0.5641 0.8744 0.3689 0.118 Uiso 1 1 calc R . . C12 C 0.0635(3) 0.88332(15) 0.45616(16) 0.0367(8) Uani 1 1 d . . . H12A H 0.0760 0.9229 0.4431 0.044 Uiso 1 1 calc R . . H12B H -0.0003 0.8831 0.4765 0.044 Uiso 1 1 calc R . . C13 C 0.0557(3) 0.84401(14) 0.40664(15) 0.0345(8) Uani 1 1 d . . . C14 C 0.0687(3) 0.76931(17) 0.35387(16) 0.0356(8) Uani 1 1 d . . . C15 C 0.0907(3) 0.71634(16) 0.32966(16) 0.0414(9) Uani 1 1 d . . . H15A H 0.1248 0.6873 0.3509 0.050 Uiso 1 1 calc R . . C16 C 0.0617(3) 0.70764(18) 0.27460(17) 0.0504(10) Uani 1 1 d . . . H16A H 0.0773 0.6722 0.2572 0.060 Uiso 1 1 calc R . . C17 C 0.0094(4) 0.74960(16) 0.24258(19) 0.0495(11) Uani 1 1 d . . . H17A H -0.0094 0.7419 0.2042 0.059 Uiso 1 1 calc R . . C18 C -0.0152(3) 0.80174(18) 0.26613(16) 0.0459(10) Uani 1 1 d . . . H18A H -0.0512 0.8302 0.2451 0.055 Uiso 1 1 calc R . . C19 C 0.0154(3) 0.81054(15) 0.32214(16) 0.0369(8) Uani 1 1 d . . . C20 C -0.0357(3) 0.91379(16) 0.34231(18) 0.0457(10) Uani 1 1 d . . . H20A H -0.0474 0.9155 0.3008 0.055 Uiso 1 1 calc R . . H20B H 0.0132 0.9442 0.3529 0.055 Uiso 1 1 calc R . . C21 C -0.1330(4) 0.9260(2) 0.3705(2) 0.0598(13) Uani 1 1 d . . . H21A H -0.1369 0.9170 0.4095 0.072 Uiso 1 1 calc R . . C22 C -0.2114(4) 0.9477(2) 0.3455(3) 0.0783(16) Uani 1 1 d . . . H22A H -0.2103 0.9572 0.3065 0.094 Uiso 1 1 calc R . . H22B H -0.2704 0.9542 0.3661 0.094 Uiso 1 1 calc R . . C23 C 0.1317(3) 0.89012(14) 0.55107(16) 0.0353(8) Uani 1 1 d . . . H23A H 0.1079 0.9301 0.5469 0.042 Uiso 1 1 calc R . . H23B H 0.1958 0.8903 0.5735 0.042 Uiso 1 1 calc R . . C24 C 0.0552(3) 0.85493(14) 0.58029(15) 0.0334(8) Uani 1 1 d . . . C25 C -0.0374(3) 0.78293(15) 0.60348(14) 0.0317(7) Uani 1 1 d . . . C26 C -0.0874(3) 0.73065(17) 0.60898(17) 0.0394(9) Uani 1 1 d . . . H26A H -0.0736 0.6993 0.5848 0.047 Uiso 1 1 calc R . . C27 C -0.1570(3) 0.72583(18) 0.65038(17) 0.0423(9) Uani 1 1 d . . . H27A H -0.1911 0.6905 0.6549 0.051 Uiso 1 1 calc R . . C28 C -0.1791(3) 0.7720(2) 0.68623(18) 0.0476(10) Uani 1 1 d . . . H28A H -0.2281 0.7673 0.7142 0.057 Uiso 1 1 calc R . . C29 C -0.1306(3) 0.82385(17) 0.68133(17) 0.0470(10) Uani 1 1 d . . . H29A H -0.1453 0.8552 0.7053 0.056 Uiso 1 1 calc R . . C30 C -0.0599(3) 0.82849(15) 0.64024(15) 0.0378(8) Uani 1 1 d . . . C31 C 0.0014(4) 0.93115(16) 0.64978(16) 0.0493(10) Uani 1 1 d . . . H31A H -0.0689 0.9441 0.6536 0.059 Uiso 1 1 calc R . . H31B H 0.0346 0.9583 0.6241 0.059 Uiso 1 1 calc R . . C32 C 0.0531(5) 0.9336(2) 0.7059(2) 0.0704(16) Uani 1 1 d . . . H32A H 0.0531 0.9698 0.7241 0.085 Uiso 1 1 calc R . . C33 C 0.0958(4) 0.8951(3) 0.7317(3) 0.0879(18) Uani 1 1 d U . . H33A H 0.0985 0.8578 0.7158 0.105 Uiso 1 1 calc R . . H33B H 0.1264 0.9024 0.7678 0.105 Uiso 1 1 calc R . . C34 C 0.2472(3) 0.61040(14) 0.50325(15) 0.0339(8) Uani 1 1 d . . . H34A H 0.2452 0.5691 0.4939 0.041 Uiso 1 1 calc R . . H34B H 0.2848 0.6152 0.5397 0.041 Uiso 1 1 calc R . . C35 C 0.2976(3) 0.64259(14) 0.45809(14) 0.0299(7) Uani 1 1 d . . . C36 C 0.3359(3) 0.71045(15) 0.39981(15) 0.0363(8) Uani 1 1 d . . . C37 C 0.3384(3) 0.75941(18) 0.36605(18) 0.0446(10) Uani 1 1 d . . . H37A H 0.2925 0.7901 0.3705 0.053 Uiso 1 1 calc R . . C38 C 0.4117(4) 0.7609(2) 0.3255(2) 0.0524(11) Uani 1 1 d . . . H38A H 0.4159 0.7936 0.3019 0.063 Uiso 1 1 calc R . . C39 C 0.4790(3) 0.7161(2) 0.31821(19) 0.0558(12) Uani 1 1 d . . . H39A H 0.5275 0.7190 0.2897 0.067 Uiso 1 1 calc R . . C40 C 0.4767(3) 0.66688(19) 0.35203(18) 0.0501(10) Uani 1 1 d . . . H40A H 0.5228 0.6363 0.3475 0.060 Uiso 1 1 calc R . . C41 C 0.4038(3) 0.66514(16) 0.39236(15) 0.0375(8) Uani 1 1 d . . . C42 C 0.4336(3) 0.56931(17) 0.4409(2) 0.0516(11) Uani 1 1 d . . . H42A H 0.4568 0.5537 0.4047 0.062 Uiso 1 1 calc R . . H42B H 0.3885 0.5407 0.4579 0.062 Uiso 1 1 calc R . . C43 C 0.5226(4) 0.5802(3) 0.4804(3) 0.086(2) Uani 1 1 d D . . H43A H 0.5069 0.5978 0.5152 0.103 Uiso 1 1 calc R . . C44 C 0.6083(6) 0.5703(3) 0.4750(3) 0.119(3) Uani 1 1 d DU . . H44A H 0.6301 0.5526 0.4413 0.143 Uiso 1 1 calc R . . H44B H 0.6558 0.5799 0.5043 0.143 Uiso 1 1 calc R . . C45 C 0.1037(3) 0.61405(14) 0.56171(14) 0.0342(8) Uani 1 1 d . . . H45A H 0.1244 0.5741 0.5700 0.041 Uiso 1 1 calc R . . H45B H 0.0294 0.6156 0.5596 0.041 Uiso 1 1 calc R . . C46 C 0.1433(3) 0.65323(14) 0.60762(14) 0.0312(7) Uani 1 1 d . . . C47 C 0.2063(3) 0.72772(16) 0.64961(15) 0.0346(8) Uani 1 1 d . . . C48 C 0.2514(3) 0.78033(17) 0.66376(17) 0.0434(9) Uani 1 1 d . . . H48A H 0.2683 0.8075 0.6357 0.052 Uiso 1 1 calc R . . C49 C 0.2698(4) 0.79050(19) 0.72082(18) 0.0534(11) Uani 1 1 d . . . H49A H 0.3000 0.8257 0.7323 0.064 Uiso 1 1 calc R . . C50 C 0.2451(4) 0.75027(19) 0.7622(2) 0.0567(13) Uani 1 1 d . . . H50A H 0.2587 0.7591 0.8009 0.068 Uiso 1 1 calc R . . C51 C 0.2026(3) 0.69919(19) 0.74855(16) 0.0480(10) Uani 1 1 d . . . H51A H 0.1868 0.6719 0.7768 0.058 Uiso 1 1 calc R . . C52 C 0.1830(3) 0.68841(16) 0.69130(15) 0.0381(8) Uani 1 1 d . . . C53 C 0.1076(3) 0.58864(17) 0.68963(17) 0.0449(10) Uani 1 1 d . . . H53A H 0.1612 0.5743 0.7160 0.054 Uiso 1 1 calc R . . H53B H 0.0958 0.5591 0.6601 0.054 Uiso 1 1 calc R . . C54 C 0.0129(4) 0.5966(2) 0.72167(19) 0.0562(11) Uani 1 1 d . . . H54A H -0.0365 0.6214 0.7050 0.067 Uiso 1 1 calc R . . C55 C -0.0084(5) 0.5738(3) 0.7687(3) 0.0917(19) Uani 1 1 d . . . H55A H 0.0383 0.5487 0.7872 0.110 Uiso 1 1 calc R . . H55B H -0.0708 0.5818 0.7853 0.110 Uiso 1 1 calc R . . C56 C 0.0791(3) 0.60888(14) 0.46103(14) 0.0313(7) Uani 1 1 d . . . H56A H 0.1168 0.6077 0.4256 0.038 Uiso 1 1 calc R . . H56B H 0.0584 0.5693 0.4703 0.038 Uiso 1 1 calc R . . C57 C -0.0113(3) 0.64614(13) 0.45324(14) 0.0302(7) Uani 1 1 d . . . C58 C -0.1084(3) 0.72020(14) 0.45558(14) 0.0310(7) Uani 1 1 d . . . C59 C -0.1527(3) 0.77400(16) 0.46353(16) 0.0380(8) Uani 1 1 d . . . H59A H -0.1175 0.8039 0.4829 0.046 Uiso 1 1 calc R . . C60 C -0.2485(3) 0.78183(18) 0.44244(16) 0.0434(9) Uani 1 1 d . . . H60A H -0.2798 0.8180 0.4469 0.052 Uiso 1 1 calc R . . C61 C -0.3016(3) 0.73801(18) 0.41441(19) 0.0449(10) Uani 1 1 d . . . H61A H -0.3685 0.7450 0.4010 0.054 Uiso 1 1 calc R . . C62 C -0.2592(3) 0.68485(16) 0.40579(16) 0.0403(9) Uani 1 1 d . . . H62A H -0.2949 0.6551 0.3865 0.048 Uiso 1 1 calc R . . C63 C -0.1614(3) 0.67723(14) 0.42682(14) 0.0339(8) Uani 1 1 d . . . C64 C -0.1185(3) 0.57567(15) 0.39675(16) 0.0400(9) Uani 1 1 d . . . H64A H -0.1879 0.5634 0.4044 0.048 Uiso 1 1 calc R . . H64B H -0.0719 0.5459 0.4118 0.048 Uiso 1 1 calc R . . C65 C -0.1069(4) 0.58113(17) 0.33432(18) 0.0502(11) Uani 1 1 d . . . H65A H -0.0499 0.6013 0.3215 0.060 Uiso 1 1 calc R . . C66 C -0.1692(4) 0.56026(18) 0.29652(18) 0.0593(13) Uani 1 1 d . . . H66A H -0.2269 0.5399 0.3079 0.071 Uiso 1 1 calc R . . H66B H -0.1571 0.5653 0.2575 0.071 Uiso 1 1 calc R . . Cl1 Cl -0.14959(8) 0.54175(4) 0.57706(4) 0.0449(2) Uani 1 1 d . . . Cl2 Cl 0.20301(8) 1.04984(4) 0.46194(6) 0.0550(3) Uani 1 1 d . . . Cl3 Cl 0.11391(8) 0.05723(5) 0.84655(4) 0.0499(3) Uani 1 1 d . . . C67 C -0.2844(9) 0.4606(3) 0.7318(5) 0.198(6) Uani 1 1 d . . . H67A H -0.3568 0.4536 0.7332 0.298 Uiso 1 1 calc R . . H67B H -0.2729 0.4992 0.7168 0.298 Uiso 1 1 calc R . . H67C H -0.2540 0.4576 0.7699 0.298 Uiso 1 1 calc R . . C68 C -0.2414(5) 0.4206(3) 0.6970(3) 0.087(2) Uani 1 1 d U . . H68A H -0.2558 0.3820 0.7120 0.105 Uiso 1 1 calc R . . H68B H -0.2747 0.4234 0.6590 0.105 Uiso 1 1 calc R . . C69 C 0.5550(5) 0.9252(3) 0.6602(3) 0.105(2) Uani 1 1 d U . . H69A H 0.5886 0.9515 0.6346 0.158 Uiso 1 1 calc R . . H69B H 0.5864 0.8873 0.6584 0.158 Uiso 1 1 calc R . . H69C H 0.5613 0.9400 0.6990 0.158 Uiso 1 1 calc R . . C70 C 0.4483(6) 0.9207(3) 0.6433(3) 0.0813(18) Uani 1 1 d . . . C71 C 0.1659(5) 0.8903(3) 0.2079(3) 0.0938(19) Uani 1 1 d U . . H71A H 0.2148 0.9101 0.1848 0.141 Uiso 1 1 calc R . . H71B H 0.1010 0.9101 0.2047 0.141 Uiso 1 1 calc R . . H71C H 0.1579 0.8507 0.1946 0.141 Uiso 1 1 calc R . . C72 C 0.2015(4) 0.8901(3) 0.2672(3) 0.0790(17) Uani 1 1 d . . . O1 O -0.1223(4) 0.53227(15) 0.52123(16) 0.0851(13) Uani 1 1 d . . . O2 O -0.2377(3) 0.51188(19) 0.58829(19) 0.0888(13) Uani 1 1 d . . . O3 O -0.1577(3) 0.60096(14) 0.5863(2) 0.0963(14) Uani 1 1 d . . . O4 O -0.0690(3) 0.51727(15) 0.61248(16) 0.0777(10) Uani 1 1 d . . . O5 O 0.1893(3) 1.10834(14) 0.4693(3) 0.1148(18) Uani 1 1 d . . . O6 O 0.2801(3) 1.02991(17) 0.4988(2) 0.1175(18) Uani 1 1 d . . . O7 O 0.2256(5) 1.0357(4) 0.4082(2) 0.174(3) Uani 1 1 d . . . O8 O 0.1114(3) 1.02313(17) 0.4730(2) 0.0995(15) Uani 1 1 d . . . O9 O 0.0406(4) 0.0173(3) 0.8444(2) 0.164(3) Uani 1 1 d . . . O10 O 0.0844(5) 0.1095(3) 0.8710(3) 0.162(3) Uani 1 1 d . . . O11 O 0.1412(3) 0.06918(18) 0.79026(14) 0.0855(12) Uani 1 1 d . . . O12 O 0.1994(3) 0.03805(16) 0.87862(14) 0.0717(10) Uani 1 1 d . . . O13 O -0.1400(4) 0.4254(2) 0.6910(3) 0.152(2) Uani 1 1 d . . . H13A H -0.1282 0.4521 0.6683 0.228 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 Eu1 0.02984(11) 0.01970(10) 0.03175(11) -0.00016(6) -0.00111(7) 0.00032(6) N1 0.0357(17) 0.0197(13) 0.0405(16) 0.0002(11) -0.0024(14) -0.0008(11) N2 0.0348(16) 0.0275(14) 0.0391(16) -0.0004(12) -0.0021(13) -0.0005(12) N3 0.0338(17) 0.0352(16) 0.0499(18) -0.0034(14) 0.0069(15) -0.0041(13) N4 0.0390(17) 0.0243(14) 0.0402(16) 0.0014(12) -0.0030(14) -0.0006(12) N5 0.0385(17) 0.0323(15) 0.0398(16) 0.0102(13) -0.0050(14) 0.0051(13) N6 0.0303(15) 0.0213(13) 0.0425(16) -0.0022(12) -0.0004(13) -0.0024(11) N7 0.0451(18) 0.0277(15) 0.0405(16) -0.0080(13) -0.0013(14) 0.0003(13) N8 0.0310(15) 0.0227(14) 0.0291(14) -0.0004(11) -0.0037(12) 0.0013(11) N9 0.0354(16) 0.0297(14) 0.0319(15) -0.0004(11) 0.0005(13) 0.0035(12) N10 0.0298(16) 0.0350(16) 0.0442(17) -0.0053(13) -0.0022(14) 0.0024(13) N11 0.0358(16) 0.0269(14) 0.0314(14) -0.0006(11) 0.0011(13) 0.0023(12) N12 0.0403(17) 0.0327(15) 0.0323(15) 0.0002(12) 0.0027(13) 0.0025(13) N13 0.0329(16) 0.0241(13) 0.0371(15) -0.0019(12) -0.0013(13) 0.0028(12) N14 0.0394(17) 0.0261(14) 0.0309(15) -0.0013(11) -0.0022(13) -0.0047(12) N15 0.101(5) 0.116(5) 0.096(4) -0.024(4) 0.014(4) -0.016(4) N16 0.079(4) 0.104(4) 0.120(5) 0.039(4) -0.009(4) -0.022(3) C1 0.039(2) 0.0297(18) 0.049(2) 0.0055(16) -0.0026(18) -0.0083(16) C2 0.0282(17) 0.0369(19) 0.0358(19) -0.0054(15) 0.0011(15) -0.0045(15) C3 0.034(2) 0.038(2) 0.0372(19) -0.0070(16) 0.0046(16) 0.0025(16) C4 0.039(2) 0.045(2) 0.044(2) -0.0001(18) -0.0023(18) 0.0021(18) C5 0.046(3) 0.060(3) 0.054(3) 0.007(2) -0.004(2) 0.009(2) C6 0.029(2) 0.079(3) 0.065(3) -0.001(3) -0.005(2) 0.011(2) C7 0.034(2) 0.067(3) 0.058(3) -0.009(2) 0.003(2) -0.006(2) C8 0.033(2) 0.045(2) 0.041(2) -0.0055(17) 0.0015(17) -0.0007(17) C9 0.047(2) 0.042(2) 0.061(3) -0.0024(19) 0.014(2) -0.0179(19) C10 0.120(5) 0.048(3) 0.091(4) 0.006(3) 0.045(4) 0.001(3) C11 0.092(5) 0.132(6) 0.071(4) 0.003(4) 0.012(3) 0.009(4) C12 0.034(2) 0.0301(18) 0.046(2) 0.0058(15) -0.0042(17) 0.0033(15) C13 0.0313(18) 0.0294(17) 0.042(2) 0.0058(15) -0.0019(16) 0.0008(14) C14 0.0324(19) 0.0345(18) 0.040(2) 0.0058(16) -0.0043(16) -0.0034(16) C15 0.051(2) 0.035(2) 0.038(2) -0.0012(16) -0.0009(18) -0.0004(18) C16 0.060(3) 0.047(2) 0.044(2) -0.0046(19) 0.002(2) -0.003(2) C17 0.054(3) 0.060(3) 0.034(2) 0.0022(17) -0.009(2) -0.008(2) C18 0.046(2) 0.053(2) 0.039(2) 0.0094(18) -0.0071(19) 0.0003(19) C19 0.0309(19) 0.0368(19) 0.043(2) 0.0070(16) -0.0028(16) -0.0022(15) C20 0.053(3) 0.0346(19) 0.049(2) 0.0147(17) -0.001(2) 0.0085(18) C21 0.062(3) 0.060(3) 0.057(3) 0.013(2) 0.005(2) 0.020(2) C22 0.058(3) 0.087(4) 0.089(4) 0.010(3) 0.005(3) 0.021(3) C23 0.041(2) 0.0232(16) 0.042(2) -0.0067(14) -0.0015(17) -0.0033(15) C24 0.0313(18) 0.0288(17) 0.0395(19) -0.0043(14) -0.0082(16) 0.0019(14) C25 0.0324(19) 0.0310(17) 0.0315(17) -0.0021(14) -0.0018(15) 0.0027(15) C26 0.040(2) 0.0303(17) 0.048(2) -0.0043(17) 0.0006(18) -0.0036(17) C27 0.040(2) 0.040(2) 0.047(2) -0.0003(18) 0.0046(18) -0.0005(18) C28 0.046(2) 0.051(2) 0.046(2) 0.000(2) 0.006(2) -0.002(2) C29 0.054(3) 0.044(2) 0.043(2) -0.0140(18) 0.008(2) 0.0010(19) C30 0.044(2) 0.0323(18) 0.0369(19) -0.0048(15) -0.0032(17) -0.0016(16) C31 0.072(3) 0.0331(19) 0.043(2) -0.0133(17) 0.004(2) -0.004(2) C32 0.099(4) 0.045(3) 0.066(3) -0.003(2) -0.008(3) -0.029(3) C33 0.075(4) 0.113(5) 0.076(4) -0.009(4) 0.001(3) -0.016(4) C34 0.040(2) 0.0225(16) 0.0387(19) 0.0001(14) -0.0026(16) 0.0048(14) C35 0.0282(17) 0.0274(16) 0.0336(18) -0.0064(13) -0.0048(15) 0.0025(14) C36 0.035(2) 0.0364(19) 0.0369(19) -0.0012(15) -0.0052(16) -0.0023(16) C37 0.044(2) 0.047(2) 0.043(2) 0.0036(17) 0.0008(19) -0.0054(18) C38 0.047(3) 0.062(3) 0.047(2) 0.010(2) -0.002(2) -0.012(2) C39 0.040(2) 0.074(3) 0.053(3) -0.006(2) 0.013(2) -0.015(2) C40 0.034(2) 0.057(3) 0.059(3) -0.012(2) 0.0047(19) -0.0053(19) C41 0.0287(18) 0.045(2) 0.039(2) -0.0091(16) -0.0040(16) -0.0012(16) C42 0.034(2) 0.034(2) 0.086(3) -0.003(2) 0.005(2) 0.0091(17) C43 0.047(3) 0.091(4) 0.118(5) 0.043(4) -0.017(3) 0.028(3) C44 0.102(6) 0.136(6) 0.117(6) 0.028(5) -0.024(5) -0.011(5) C45 0.040(2) 0.0254(16) 0.0367(19) 0.0029(14) 0.0010(16) 0.0018(15) C46 0.0320(18) 0.0291(17) 0.0323(18) -0.0002(13) -0.0005(15) 0.0028(14) C47 0.040(2) 0.0307(17) 0.0334(18) -0.0055(15) 0.0013(16) 0.0084(16) C48 0.047(2) 0.036(2) 0.047(2) -0.0102(17) -0.0003(19) 0.0024(18) C49 0.062(3) 0.046(2) 0.052(3) -0.023(2) -0.005(2) 0.002(2) C50 0.061(3) 0.071(3) 0.038(2) -0.016(2) 0.003(2) 0.002(2) C51 0.055(3) 0.055(3) 0.034(2) -0.0052(18) 0.0068(19) 0.008(2) C52 0.037(2) 0.046(2) 0.0317(18) -0.0043(16) 0.0048(16) 0.0098(17) C53 0.057(3) 0.041(2) 0.037(2) 0.0086(16) 0.0076(19) 0.0007(19) C54 0.054(3) 0.069(3) 0.046(2) 0.013(2) 0.006(2) -0.004(2) C55 0.090(4) 0.097(4) 0.091(4) 0.006(3) 0.046(4) 0.001(4) C56 0.039(2) 0.0234(15) 0.0310(17) -0.0026(13) -0.0044(15) -0.0016(14) C57 0.0378(19) 0.0226(15) 0.0302(17) 0.0002(13) -0.0012(15) -0.0027(14) C58 0.0347(19) 0.0254(17) 0.0325(17) 0.0005(14) -0.0046(15) -0.0010(14) C59 0.039(2) 0.0316(18) 0.043(2) -0.0058(16) -0.0019(17) 0.0029(16) C60 0.039(2) 0.045(2) 0.046(2) -0.0014(18) -0.0036(18) 0.0086(18) C61 0.029(2) 0.055(2) 0.051(2) 0.0004(19) -0.0078(18) -0.0014(18) C62 0.040(2) 0.041(2) 0.039(2) -0.0022(16) -0.0064(17) -0.0061(17) C63 0.041(2) 0.0304(17) 0.0307(17) 0.0075(14) 0.0010(16) -0.0019(15) C64 0.045(2) 0.0288(18) 0.045(2) -0.0021(16) -0.0088(18) -0.0087(16) C65 0.063(3) 0.040(2) 0.049(2) -0.0103(18) 0.001(2) -0.011(2) C66 0.089(4) 0.048(2) 0.041(2) 0.0011(19) -0.006(2) 0.002(2) Cl1 0.0507(6) 0.0326(5) 0.0519(6) -0.0079(4) 0.0090(5) -0.0115(4) Cl2 0.0452(6) 0.0350(5) 0.0844(8) -0.0086(5) -0.0031(6) 0.0012(4) Cl3 0.0486(6) 0.0557(6) 0.0452(5) 0.0002(5) -0.0007(5) -0.0023(5) C67 0.257(13) 0.081(5) 0.268(13) 0.017(7) 0.182(11) 0.014(7) C68 0.089(4) 0.103(5) 0.070(4) 0.011(3) 0.004(3) -0.044(4) C69 0.094(5) 0.129(6) 0.092(5) -0.015(4) -0.003(4) 0.002(4) C70 0.102(5) 0.080(4) 0.063(4) -0.003(3) 0.007(4) -0.009(4) C71 0.078(4) 0.102(5) 0.103(5) -0.007(4) 0.026(4) -0.003(4) C72 0.053(3) 0.070(4) 0.114(5) 0.026(4) 0.006(4) 0.000(3) O1 0.147(4) 0.052(2) 0.057(2) 0.0081(17) 0.024(2) 0.013(2) O2 0.052(2) 0.094(3) 0.121(3) 0.014(2) 0.010(2) -0.032(2) O3 0.087(3) 0.0411(19) 0.161(4) -0.035(2) 0.009(3) 0.0006(19) O4 0.067(2) 0.079(2) 0.085(2) -0.006(2) -0.022(2) 0.001(2) O5 0.092(3) 0.0345(18) 0.216(5) -0.008(3) -0.019(3) 0.0011(19) O6 0.095(3) 0.076(3) 0.176(5) -0.026(3) -0.073(3) 0.023(2) O7 0.135(5) 0.301(9) 0.089(4) -0.052(5) 0.018(3) 0.067(5) O8 0.076(3) 0.062(2) 0.159(4) 0.023(3) -0.018(3) -0.023(2) O9 0.139(5) 0.214(6) 0.137(4) 0.068(4) -0.042(4) -0.134(5) O10 0.183(6) 0.150(5) 0.149(5) -0.072(4) -0.037(4) 0.100(5) O11 0.089(3) 0.112(3) 0.056(2) 0.026(2) -0.005(2) -0.010(2) O12 0.071(2) 0.088(2) 0.0553(19) 0.0066(18) -0.0117(17) 0.008(2) O13 0.135(5) 0.108(4) 0.217(6) 0.068(4) 0.090(4) 0.026(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 Eu1 N13 2.486(3) . ? Eu1 N11 2.504(3) . ? Eu1 N6 2.505(3) . ? Eu1 N2 2.505(3) . ? Eu1 N9 2.511(3) . ? Eu1 N4 2.518(3) . ? Eu1 N8 2.701(3) . ? Eu1 N1 2.720(3) . ? N1 C12 1.477(4) . ? N1 C1 1.479(5) . ? N1 C23 1.483(4) . ? N2 C2 1.326(4) . ? N2 C3 1.398(5) . ? N3 C2 1.349(4) . ? N3 C8 1.402(5) . ? N3 C9 1.464(5) . ? N4 C13 1.323(4) . ? N4 C14 1.393(5) . ? N5 C13 1.347(4) . ? N5 C19 1.383(5) . ? N5 C20 1.474(4) . ? N6 C24 1.328(4) . ? N6 C25 1.392(5) . ? N7 C24 1.350(5) . ? N7 C30 1.393(5) . ? N7 C31 1.474(4) . ? N8 C45 1.464(4) . ? N8 C34 1.471(4) . ? N8 C56 1.492(4) . ? N9 C35 1.317(4) . ? N9 C36 1.410(5) . ? N10 C35 1.356(4) . ? N10 C41 1.383(5) . ? N10 C42 1.469(5) . ? N11 C46 1.326(4) . ? N11 C47 1.401(4) . ? N12 C46 1.337(4) . ? N12 C52 1.390(5) . ? N12 C53 1.463(5) . ? N13 C57 1.332(4) . ? N13 C58 1.400(4) . ? N14 C57 1.347(4) . ? N14 C63 1.387(4) . ? N14 C64 1.475(4) . ? N15 C70 1.115(8) . ? N16 C72 1.094(8) . ? C1 C2 1.486(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.394(5) . ? C3 C4 1.402(6) . ? C4 C5 1.362(6) . ? C4 H4A 0.9500 . ? C5 C6 1.418(7) . ? C5 H5A 0.9500 . ? C6 C7 1.371(7) . ? C6 H6A 0.9500 . ? C7 C8 1.397(5) . ? C7 H7A 0.9500 . ? C9 C10 1.454(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.264(8) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C11 H11B 0.9500 . ? C12 C13 1.489(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.397(5) . ? C14 C19 1.399(5) . ? C15 C16 1.361(5) . ? C15 H15A 0.9500 . ? C16 C17 1.409(6) . ? C16 H16A 0.9500 . ? C17 C18 1.382(6) . ? C17 H17A 0.9500 . ? C18 C19 1.389(5) . ? C18 H18A 0.9500 . ? C20 C21 1.503(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.287(6) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C22 H22B 0.9500 . ? C23 C24 1.495(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.398(5) . ? C25 C30 1.412(5) . ? C26 C27 1.375(5) . ? C26 H26A 0.9500 . ? C27 C28 1.408(6) . ? C27 H27A 0.9500 . ? C28 C29 1.378(6) . ? C28 H28A 0.9500 . ? C29 C30 1.378(5) . ? C29 H29A 0.9500 . ? C31 C32 1.476(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.217(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C33 H33B 0.9500 . ? C34 C35 1.484(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C36 C37 1.395(5) . ? C36 C41 1.406(5) . ? C37 C38 1.390(6) . ? C37 H37A 0.9500 . ? C38 C39 1.391(7) . ? C38 H38A 0.9500 . ? C39 C40 1.401(6) . ? C39 H39A 0.9500 . ? C40 C41 1.383(5) . ? C40 H40A 0.9500 . ? C42 C43 1.506(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.176(8) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C44 H44B 0.9500 . ? C45 C46 1.502(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C47 C52 1.389(5) . ? C47 C48 1.402(6) . ? C48 C49 1.384(6) . ? C48 H48A 0.9500 . ? C49 C50 1.402(7) . ? C49 H49A 0.9500 . ? C50 C51 1.354(6) . ? C50 H50A 0.9500 . ? C51 C52 1.393(5) . ? C51 H51A 0.9500 . ? C53 C54 1.504(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.273(7) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C55 H55B 0.9500 . ? C56 C57 1.492(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C58 C63 1.391(5) . ? C58 C59 1.402(5) . ? C59 C60 1.366(5) . ? C59 H59A 0.9500 . ? C60 C61 1.398(6) . ? C60 H60A 0.9500 . ? C61 C62 1.381(6) . ? C61 H61A 0.9500 . ? C62 C63 1.390(5) . ? C62 H62A 0.9500 . ? C64 C65 1.495(6) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.295(6) . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C66 H66B 0.9500 . ? Cl1 O2 1.398(3) . ? Cl1 O1 1.398(4) . ? Cl1 O3 1.404(3) . ? Cl1 O4 1.457(4) . ? Cl2 O7 1.355(5) . ? Cl2 O5 1.389(3) . ? Cl2 O8 1.402(4) . ? Cl2 O6 1.404(4) . ? Cl3 O9 1.350(4) . ? Cl3 O10 1.411(5) . ? Cl3 O11 1.419(4) . ? Cl3 O12 1.420(3) . ? C67 C68 1.381(10) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 O13 1.367(8) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.468(10) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C71 C72 1.465(9) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? O13 H13A 0.8400 . ? 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 N13 Eu1 N11 100.80(9) . . ? N13 Eu1 N6 82.50(9) . . ? N11 Eu1 N6 74.65(9) . . ? N13 Eu1 N2 174.76(9) . . ? N11 Eu1 N2 83.80(9) . . ? N6 Eu1 N2 101.24(9) . . ? N13 Eu1 N9 100.88(9) . . ? N11 Eu1 N9 101.36(9) . . ? N6 Eu1 N9 175.28(9) . . ? N2 Eu1 N9 75.60(9) . . ? N13 Eu1 N4 73.98(9) . . ? N11 Eu1 N4 173.59(10) . . ? N6 Eu1 N4 100.69(9) . . ? N2 Eu1 N4 101.58(9) . . ? N9 Eu1 N4 83.48(9) . . ? N13 Eu1 N8 63.34(8) . . ? N11 Eu1 N8 62.78(8) . . ? N6 Eu1 N8 116.43(8) . . ? N2 Eu1 N8 117.40(8) . . ? N9 Eu1 N8 62.92(9) . . ? N4 Eu1 N8 116.75(8) . . ? N13 Eu1 N1 116.03(8) . . ? N11 Eu1 N1 117.05(8) . . ? N6 Eu1 N1 62.81(9) . . ? N2 Eu1 N1 63.28(9) . . ? N9 Eu1 N1 117.87(9) . . ? N4 Eu1 N1 63.32(9) . . ? N8 Eu1 N1 179.17(9) . . ? C12 N1 C1 109.8(3) . . ? C12 N1 C23 108.2(3) . . ? C1 N1 C23 109.5(3) . . ? C12 N1 Eu1 109.3(2) . . ? C1 N1 Eu1 109.3(2) . . ? C23 N1 Eu1 110.7(2) . . ? C2 N2 C3 105.3(3) . . ? C2 N2 Eu1 119.2(2) . . ? C3 N2 Eu1 134.1(2) . . ? C2 N3 C8 106.4(3) . . ? C2 N3 C9 129.1(3) . . ? C8 N3 C9 124.5(3) . . ? C13 N4 C14 105.0(3) . . ? C13 N4 Eu1 118.6(2) . . ? C14 N4 Eu1 134.4(2) . . ? C13 N5 C19 107.1(3) . . ? C13 N5 C20 126.1(3) . . ? C19 N5 C20 126.6(3) . . ? C24 N6 C25 105.5(3) . . ? C24 N6 Eu1 120.1(2) . . ? C25 N6 Eu1 132.8(2) . . ? C24 N7 C30 107.3(3) . . ? C24 N7 C31 128.1(3) . . ? C30 N7 C31 124.6(3) . . ? C45 N8 C34 109.4(3) . . ? C45 N8 C56 108.3(3) . . ? C34 N8 C56 109.6(3) . . ? C45 N8 Eu1 110.69(19) . . ? C34 N8 Eu1 109.46(19) . . ? C56 N8 Eu1 109.46(18) . . ? C35 N9 C36 105.4(3) . . ? C35 N9 Eu1 119.0(2) . . ? C36 N9 Eu1 134.0(2) . . ? C35 N10 C41 106.8(3) . . ? C35 N10 C42 127.3(3) . . ? C41 N10 C42 125.8(3) . . ? C46 N11 C47 104.6(3) . . ? C46 N11 Eu1 119.3(2) . . ? C47 N11 Eu1 133.2(2) . . ? C46 N12 C52 106.9(3) . . ? C46 N12 C53 127.7(3) . . ? C52 N12 C53 125.4(3) . . ? C57 N13 C58 104.5(3) . . ? C57 N13 Eu1 119.6(2) . . ? C58 N13 Eu1 133.1(2) . . ? C57 N14 C63 107.0(3) . . ? C57 N14 C64 127.4(3) . . ? C63 N14 C64 125.5(3) . . ? N1 C1 C2 108.7(3) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 113.3(3) . . ? N2 C2 C1 123.0(3) . . ? N3 C2 C1 123.7(3) . . ? C8 C3 N2 109.0(3) . . ? C8 C3 C4 119.9(4) . . ? N2 C3 C4 131.0(4) . . ? C5 C4 C3 117.7(4) . . ? C5 C4 H4A 121.2 . . ? C3 C4 H4A 121.2 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 121.7(4) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 116.1(4) . . ? C6 C7 H7A 122.0 . . ? C8 C7 H7A 122.0 . . ? C3 C8 C7 123.0(4) . . ? C3 C8 N3 105.9(3) . . ? C7 C8 N3 131.1(4) . . ? C10 C9 N3 113.4(4) . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? N3 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 127.6(6) . . ? C11 C10 H10A 116.2 . . ? C9 C10 H10A 116.2 . . ? C10 C11 H11A 120.0 . . ? C10 C11 H11B 120.0 . . ? H11A C11 H11B 120.0 . . ? N1 C12 C13 109.4(3) . . ? N1 C12 H12A 109.8 . . ? C13 C12 H12A 109.8 . . ? N1 C12 H12B 109.8 . . ? C13 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? N4 C13 N5 113.2(3) . . ? N4 C13 C12 123.1(3) . . ? N5 C13 C12 123.7(3) . . ? N4 C14 C15 130.9(3) . . ? N4 C14 C19 109.2(3) . . ? C15 C14 C19 119.9(3) . . ? C16 C15 C14 117.8(4) . . ? C16 C15 H15A 121.1 . . ? C14 C15 H15A 121.1 . . ? C15 C16 C17 122.0(4) . . ? C15 C16 H16A 119.0 . . ? C17 C16 H16A 119.0 . . ? C18 C17 C16 121.0(4) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 116.6(4) . . ? C17 C18 H18A 121.7 . . ? C19 C18 H18A 121.7 . . ? N5 C19 C18 131.8(3) . . ? N5 C19 C14 105.5(3) . . ? C18 C19 C14 122.6(4) . . ? N5 C20 C21 113.9(3) . . ? N5 C20 H20A 108.8 . . ? C21 C20 H20A 108.8 . . ? N5 C20 H20B 108.8 . . ? C21 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 124.7(5) . . ? C22 C21 H21A 117.6 . . ? C20 C21 H21A 117.6 . . ? C21 C22 H22A 120.0 . . ? C21 C22 H22B 120.0 . . ? H22A C22 H22B 120.0 . . ? N1 C23 C24 108.0(3) . . ? N1 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? N1 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N6 C24 N7 112.9(3) . . ? N6 C24 C23 122.7(3) . . ? N7 C24 C23 124.3(3) . . ? N6 C25 C26 131.7(3) . . ? N6 C25 C30 109.1(3) . . ? C26 C25 C30 119.2(3) . . ? C27 C26 C25 118.2(4) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C26 C27 C28 121.7(4) . . ? C26 C27 H27A 119.2 . . ? C28 C27 H27A 119.2 . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C28 C29 C30 117.4(4) . . ? C28 C29 H29A 121.3 . . ? C30 C29 H29A 121.3 . . ? C29 C30 N7 132.2(3) . . ? C29 C30 C25 122.6(3) . . ? N7 C30 C25 105.2(3) . . ? N7 C31 C32 114.0(4) . . ? N7 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N7 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 128.3(5) . . ? C33 C32 H32A 115.8 . . ? C31 C32 H32A 115.8 . . ? C32 C33 H33A 120.0 . . ? C32 C33 H33B 120.0 . . ? H33A C33 H33B 120.0 . . ? N8 C34 C35 108.6(3) . . ? N8 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? N8 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.3 . . ? N9 C35 N10 113.3(3) . . ? N9 C35 C34 122.5(3) . . ? N10 C35 C34 124.1(3) . . ? C37 C36 C41 121.1(4) . . ? C37 C36 N9 130.7(4) . . ? C41 C36 N9 108.1(3) . . ? C38 C37 C36 116.4(4) . . ? C38 C37 H37A 121.8 . . ? C36 C37 H37A 121.8 . . ? C39 C38 C37 122.4(4) . . ? C39 C38 H38A 118.8 . . ? C37 C38 H38A 118.8 . . ? C38 C39 C40 121.3(4) . . ? C38 C39 H39A 119.4 . . ? C40 C39 H39A 119.4 . . ? C41 C40 C39 116.5(4) . . ? C41 C40 H40A 121.7 . . ? C39 C40 H40A 121.7 . . ? N10 C41 C40 131.4(4) . . ? N10 C41 C36 106.4(3) . . ? C40 C41 C36 122.2(4) . . ? N10 C42 C43 109.7(4) . . ? N10 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? N10 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 130.3(8) . . ? C44 C43 H43A 114.9 . . ? C42 C43 H43A 114.8 . . ? C43 C44 H44A 120.0 . . ? C43 C44 H44B 120.0 . . ? H44A C44 H44B 120.0 . . ? N8 C45 C46 108.5(3) . . ? N8 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? N8 C45 H45B 110.0 . . ? C46 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? N11 C46 N12 113.5(3) . . ? N11 C46 C45 122.1(3) . . ? N12 C46 C45 124.4(3) . . ? C52 C47 N11 109.2(3) . . ? C52 C47 C48 120.8(3) . . ? N11 C47 C48 130.0(3) . . ? C49 C48 C47 116.3(4) . . ? C49 C48 H48A 121.8 . . ? C47 C48 H48A 121.8 . . ? C48 C49 C50 121.8(4) . . ? C48 C49 H49A 119.1 . . ? C50 C49 H49A 119.1 . . ? C51 C50 C49 121.9(4) . . ? C51 C50 H50A 119.0 . . ? C49 C50 H50A 119.0 . . ? C50 C51 C52 117.0(4) . . ? C50 C51 H51A 121.5 . . ? C52 C51 H51A 121.5 . . ? C47 C52 N12 105.8(3) . . ? C47 C52 C51 122.1(4) . . ? N12 C52 C51 132.1(4) . . ? N12 C53 C54 113.3(3) . . ? N12 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? N12 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C53 127.0(5) . . ? C55 C54 H54A 116.5 . . ? C53 C54 H54A 116.5 . . ? C54 C55 H55A 120.0 . . ? C54 C55 H55B 120.0 . . ? H55A C55 H55B 120.0 . . ? C57 C56 N8 108.9(3) . . ? C57 C56 H56A 109.9 . . ? N8 C56 H56A 109.9 . . ? C57 C56 H56B 109.9 . . ? N8 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? N13 C57 N14 113.2(3) . . ? N13 C57 C56 122.0(3) . . ? N14 C57 C56 124.8(3) . . ? C63 C58 N13 109.5(3) . . ? C63 C58 C59 120.2(3) . . ? N13 C58 C59 130.4(3) . . ? C60 C59 C58 117.5(4) . . ? C60 C59 H59A 121.2 . . ? C58 C59 H59A 121.2 . . ? C59 C60 C61 121.8(4) . . ? C59 C60 H60A 119.1 . . ? C61 C60 H60A 119.1 . . ? C62 C61 C60 121.6(4) . . ? C62 C61 H61A 119.2 . . ? C60 C61 H61A 119.2 . . ? C61 C62 C63 116.4(3) . . ? C61 C62 H62A 121.8 . . ? C63 C62 H62A 121.8 . . ? N14 C63 C58 105.8(3) . . ? N14 C63 C62 131.7(3) . . ? C58 C63 C62 122.5(3) . . ? N14 C64 C65 111.4(3) . . ? N14 C64 H64A 109.3 . . ? C65 C64 H64A 109.3 . . ? N14 C64 H64B 109.3 . . ? C65 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C66 C65 C64 124.4(4) . . ? C66 C65 H65A 117.8 . . ? C64 C65 H65A 117.8 . . ? C65 C66 H66A 120.0 . . ? C65 C66 H66B 120.0 . . ? H66A C66 H66B 120.0 . . ? O2 Cl1 O1 110.2(3) . . ? O2 Cl1 O3 113.1(3) . . ? O1 Cl1 O3 109.1(3) . . ? O2 Cl1 O4 107.6(2) . . ? O1 Cl1 O4 105.8(3) . . ? O3 Cl1 O4 110.8(2) . . ? O7 Cl2 O5 113.0(5) . . ? O7 Cl2 O8 106.7(4) . . ? O5 Cl2 O8 107.1(3) . . ? O7 Cl2 O6 108.8(4) . . ? O5 Cl2 O6 110.1(3) . . ? O8 Cl2 O6 111.1(3) . . ? O9 Cl3 O10 113.7(5) . . ? O9 Cl3 O11 107.9(3) . . ? O10 Cl3 O11 107.3(4) . . ? O9 Cl3 O12 111.6(3) . . ? O10 Cl3 O12 106.4(3) . . ? O11 Cl3 O12 109.7(2) . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O13 C68 C67 115.9(7) . . ? O13 C68 H68A 108.3 . . ? C67 C68 H68A 108.3 . . ? O13 C68 H68B 108.3 . . ? C67 C68 H68B 108.3 . . ? H68A C68 H68B 107.4 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N15 C70 C69 177.5(8) . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N16 C72 C71 178.0(8) . . ? C68 O13 H13A 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 N13 Eu1 N1 C12 -20.0(2) . . . . ? N11 Eu1 N1 C12 -138.9(2) . . . . ? N6 Eu1 N1 C12 -85.5(2) . . . . ? N2 Eu1 N1 C12 154.2(2) . . . . ? N9 Eu1 N1 C12 99.7(2) . . . . ? N4 Eu1 N1 C12 33.9(2) . . . . ? N8 Eu1 N1 C12 -61(6) . . . . ? N13 Eu1 N1 C1 -140.2(2) . . . . ? N11 Eu1 N1 C1 100.8(2) . . . . ? N6 Eu1 N1 C1 154.2(2) . . . . ? N2 Eu1 N1 C1 34.0(2) . . . . ? N9 Eu1 N1 C1 -20.5(2) . . . . ? N4 Eu1 N1 C1 -86.3(2) . . . . ? N8 Eu1 N1 C1 178(100) . . . . ? N13 Eu1 N1 C23 99.1(2) . . . . ? N11 Eu1 N1 C23 -19.8(2) . . . . ? N6 Eu1 N1 C23 33.6(2) . . . . ? N2 Eu1 N1 C23 -86.7(2) . . . . ? N9 Eu1 N1 C23 -141.2(2) . . . . ? N4 Eu1 N1 C23 153.0(2) . . . . ? N8 Eu1 N1 C23 58(6) . . . . ? N13 Eu1 N2 C2 60.5(10) . . . . ? N11 Eu1 N2 C2 -147.8(3) . . . . ? N6 Eu1 N2 C2 -74.8(3) . . . . ? N9 Eu1 N2 C2 108.8(3) . . . . ? N4 Eu1 N2 C2 28.7(3) . . . . ? N8 Eu1 N2 C2 157.3(2) . . . . ? N1 Eu1 N2 C2 -23.3(2) . . . . ? N13 Eu1 N2 C3 -104.2(9) . . . . ? N11 Eu1 N2 C3 47.5(3) . . . . ? N6 Eu1 N2 C3 120.5(3) . . . . ? N9 Eu1 N2 C3 -55.9(3) . . . . ? N4 Eu1 N2 C3 -136.0(3) . . . . ? N8 Eu1 N2 C3 -7.4(3) . . . . ? N1 Eu1 N2 C3 172.0(3) . . . . ? N13 Eu1 N4 C13 106.1(3) . . . . ? N11 Eu1 N4 C13 70.1(8) . . . . ? N6 Eu1 N4 C13 27.2(3) . . . . ? N2 Eu1 N4 C13 -76.7(3) . . . . ? N9 Eu1 N4 C13 -150.5(3) . . . . ? N8 Eu1 N4 C13 154.3(2) . . . . ? N1 Eu1 N4 C13 -24.8(2) . . . . ? N13 Eu1 N4 C14 -55.3(3) . . . . ? N11 Eu1 N4 C14 -91.4(8) . . . . ? N6 Eu1 N4 C14 -134.2(3) . . . . ? N2 Eu1 N4 C14 121.8(3) . . . . ? N9 Eu1 N4 C14 48.0(3) . . . . ? N8 Eu1 N4 C14 -7.2(4) . . . . ? N1 Eu1 N4 C14 173.7(4) . . . . ? N13 Eu1 N6 C24 -148.1(3) . . . . ? N11 Eu1 N6 C24 108.5(3) . . . . ? N2 Eu1 N6 C24 28.2(3) . . . . ? N9 Eu1 N6 C24 75.8(11) . . . . ? N4 Eu1 N6 C24 -76.1(3) . . . . ? N8 Eu1 N6 C24 156.7(2) . . . . ? N1 Eu1 N6 C24 -23.7(2) . . . . ? N13 Eu1 N6 C25 48.4(3) . . . . ? N11 Eu1 N6 C25 -55.0(3) . . . . ? N2 Eu1 N6 C25 -135.3(3) . . . . ? N9 Eu1 N6 C25 -87.6(11) . . . . ? N4 Eu1 N6 C25 120.5(3) . . . . ? N8 Eu1 N6 C25 -6.7(3) . . . . ? N1 Eu1 N6 C25 172.9(3) . . . . ? N13 Eu1 N8 C45 -84.7(2) . . . . ? N11 Eu1 N8 C45 34.9(2) . . . . ? N6 Eu1 N8 C45 -19.1(2) . . . . ? N2 Eu1 N8 C45 101.1(2) . . . . ? N9 Eu1 N8 C45 155.7(2) . . . . ? N4 Eu1 N8 C45 -137.9(2) . . . . ? N1 Eu1 N8 C45 -43(6) . . . . ? N13 Eu1 N8 C34 154.6(2) . . . . ? N11 Eu1 N8 C34 -85.7(2) . . . . ? N6 Eu1 N8 C34 -139.7(2) . . . . ? N2 Eu1 N8 C34 -19.5(2) . . . . ? N9 Eu1 N8 C34 35.0(2) . . . . ? N4 Eu1 N8 C34 101.4(2) . . . . ? N1 Eu1 N8 C34 -164(11) . . . . ? N13 Eu1 N8 C56 34.5(2) . . . . ? N11 Eu1 N8 C56 154.2(2) . . . . ? N6 Eu1 N8 C56 100.2(2) . . . . ? N2 Eu1 N8 C56 -139.6(2) . . . . ? N9 Eu1 N8 C56 -85.1(2) . . . . ? N4 Eu1 N8 C56 -18.7(2) . . . . ? N1 Eu1 N8 C56 76(6) . . . . ? N13 Eu1 N9 C35 -76.9(3) . . . . ? N11 Eu1 N9 C35 26.6(3) . . . . ? N6 Eu1 N9 C35 58.6(11) . . . . ? N2 Eu1 N9 C35 107.0(3) . . . . ? N4 Eu1 N9 C35 -149.2(3) . . . . ? N8 Eu1 N9 C35 -24.6(2) . . . . ? N1 Eu1 N9 C35 155.7(2) . . . . ? N13 Eu1 N9 C36 119.7(3) . . . . ? N11 Eu1 N9 C36 -136.8(3) . . . . ? N6 Eu1 N9 C36 -104.7(10) . . . . ? N2 Eu1 N9 C36 -56.3(3) . . . . ? N4 Eu1 N9 C36 47.5(3) . . . . ? N8 Eu1 N9 C36 172.0(3) . . . . ? N1 Eu1 N9 C36 -7.7(3) . . . . ? N13 Eu1 N11 C46 26.1(3) . . . . ? N6 Eu1 N11 C46 105.1(3) . . . . ? N2 Eu1 N11 C46 -151.4(3) . . . . ? N9 Eu1 N11 C46 -77.5(3) . . . . ? N4 Eu1 N11 C46 61.2(8) . . . . ? N8 Eu1 N11 C46 -26.2(2) . . . . ? N1 Eu1 N11 C46 152.9(2) . . . . ? N13 Eu1 N11 C47 -131.5(3) . . . . ? N6 Eu1 N11 C47 -52.5(3) . . . . ? N2 Eu1 N11 C47 51.0(3) . . . . ? N9 Eu1 N11 C47 124.9(3) . . . . ? N4 Eu1 N11 C47 -96.4(8) . . . . ? N8 Eu1 N11 C47 176.2(3) . . . . ? N1 Eu1 N11 C47 -4.7(3) . . . . ? N11 Eu1 N13 C57 -78.4(3) . . . . ? N6 Eu1 N13 C57 -151.1(3) . . . . ? N2 Eu1 N13 C57 73.0(10) . . . . ? N9 Eu1 N13 C57 25.5(3) . . . . ? N4 Eu1 N13 C57 105.4(3) . . . . ? N8 Eu1 N13 C57 -26.5(2) . . . . ? N1 Eu1 N13 C57 154.1(2) . . . . ? N11 Eu1 N13 C58 123.8(3) . . . . ? N6 Eu1 N13 C58 51.1(3) . . . . ? N2 Eu1 N13 C58 -84.8(10) . . . . ? N9 Eu1 N13 C58 -132.2(3) . . . . ? N4 Eu1 N13 C58 -52.3(3) . . . . ? N8 Eu1 N13 C58 175.7(3) . . . . ? N1 Eu1 N13 C58 -3.6(3) . . . . ? C12 N1 C1 C2 -161.1(3) . . . . ? C23 N1 C1 C2 80.2(3) . . . . ? Eu1 N1 C1 C2 -41.2(3) . . . . ? C3 N2 C2 N3 -0.4(4) . . . . ? Eu1 N2 C2 N3 -169.1(2) . . . . ? C3 N2 C2 C1 178.4(3) . . . . ? Eu1 N2 C2 C1 9.7(5) . . . . ? C8 N3 C2 N2 0.5(4) . . . . ? C9 N3 C2 N2 179.2(3) . . . . ? C8 N3 C2 C1 -178.3(3) . . . . ? C9 N3 C2 C1 0.4(6) . . . . ? N1 C1 C2 N2 24.1(5) . . . . ? N1 C1 C2 N3 -157.2(3) . . . . ? C2 N2 C3 C8 0.2(4) . . . . ? Eu1 N2 C3 C8 166.4(2) . . . . ? C2 N2 C3 C4 179.0(4) . . . . ? Eu1 N2 C3 C4 -14.8(6) . . . . ? C8 C3 C4 C5 -1.2(6) . . . . ? N2 C3 C4 C5 -179.9(4) . . . . ? C3 C4 C5 C6 0.6(7) . . . . ? C4 C5 C6 C7 0.3(7) . . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? N2 C3 C8 C7 180.0(3) . . . . ? C4 C3 C8 C7 0.9(6) . . . . ? N2 C3 C8 N3 0.1(4) . . . . ? C4 C3 C8 N3 -178.9(3) . . . . ? C6 C7 C8 C3 -0.1(6) . . . . ? C6 C7 C8 N3 179.7(4) . . . . ? C2 N3 C8 C3 -0.3(4) . . . . ? C9 N3 C8 C3 -179.1(3) . . . . ? C2 N3 C8 C7 179.8(4) . . . . ? C9 N3 C8 C7 1.0(6) . . . . ? C2 N3 C9 C10 -99.3(5) . . . . ? C8 N3 C9 C10 79.3(5) . . . . ? N3 C9 C10 C11 -4.7(10) . . . . ? C1 N1 C12 C13 79.9(4) . . . . ? C23 N1 C12 C13 -160.6(3) . . . . ? Eu1 N1 C12 C13 -40.0(3) . . . . ? C14 N4 C13 N5 0.8(4) . . . . ? Eu1 N4 C13 N5 -165.6(2) . . . . ? C14 N4 C13 C12 179.3(3) . . . . ? Eu1 N4 C13 C12 12.9(5) . . . . ? C19 N5 C13 N4 -0.6(4) . . . . ? C20 N5 C13 N4 -176.5(3) . . . . ? C19 N5 C13 C12 -179.1(3) . . . . ? C20 N5 C13 C12 5.0(6) . . . . ? N1 C12 C13 N4 21.2(5) . . . . ? N1 C12 C13 N5 -160.5(3) . . . . ? C13 N4 C14 C15 178.1(4) . . . . ? Eu1 N4 C14 C15 -18.7(6) . . . . ? C13 N4 C14 C19 -0.7(4) . . . . ? Eu1 N4 C14 C19 162.5(3) . . . . ? N4 C14 C15 C16 -176.5(4) . . . . ? C19 C14 C15 C16 2.2(6) . . . . ? C14 C15 C16 C17 -1.3(7) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C19 0.8(7) . . . . ? C13 N5 C19 C18 -176.4(4) . . . . ? C20 N5 C19 C18 -0.5(7) . . . . ? C13 N5 C19 C14 0.1(4) . . . . ? C20 N5 C19 C14 176.0(4) . . . . ? C17 C18 C19 N5 176.2(4) . . . . ? C17 C18 C19 C14 0.1(6) . . . . ? N4 C14 C19 N5 0.4(4) . . . . ? C15 C14 C19 N5 -178.6(4) . . . . ? N4 C14 C19 C18 177.3(4) . . . . ? C15 C14 C19 C18 -1.6(6) . . . . ? C13 N5 C20 C21 -74.9(5) . . . . ? C19 N5 C20 C21 110.0(4) . . . . ? N5 C20 C21 C22 -136.0(5) . . . . ? C12 N1 C23 C24 80.0(3) . . . . ? C1 N1 C23 C24 -160.4(3) . . . . ? Eu1 N1 C23 C24 -39.8(3) . . . . ? C25 N6 C24 N7 -0.4(4) . . . . ? Eu1 N6 C24 N7 -167.9(2) . . . . ? C25 N6 C24 C23 178.7(3) . . . . ? Eu1 N6 C24 C23 11.2(4) . . . . ? C30 N7 C24 N6 0.6(4) . . . . ? C31 N7 C24 N6 -178.7(3) . . . . ? C30 N7 C24 C23 -178.5(3) . . . . ? C31 N7 C24 C23 2.2(6) . . . . ? N1 C23 C24 N6 21.9(5) . . . . ? N1 C23 C24 N7 -159.1(3) . . . . ? C24 N6 C25 C26 179.7(4) . . . . ? Eu1 N6 C25 C26 -15.1(6) . . . . ? C24 N6 C25 C30 0.2(4) . . . . ? Eu1 N6 C25 C30 165.3(2) . . . . ? N6 C25 C26 C27 -179.5(4) . . . . ? C30 C25 C26 C27 0.0(5) . . . . ? C25 C26 C27 C28 0.7(6) . . . . ? C26 C27 C28 C29 -0.6(6) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C28 C29 C30 N7 179.1(4) . . . . ? C28 C29 C30 C25 0.8(6) . . . . ? C24 N7 C30 C29 -179.0(4) . . . . ? C31 N7 C30 C29 0.3(6) . . . . ? C24 N7 C30 C25 -0.4(4) . . . . ? C31 N7 C30 C25 178.9(3) . . . . ? N6 C25 C30 C29 178.9(3) . . . . ? C26 C25 C30 C29 -0.7(6) . . . . ? N6 C25 C30 N7 0.2(4) . . . . ? C26 C25 C30 N7 -179.4(3) . . . . ? C24 N7 C31 C32 -106.0(5) . . . . ? C30 N7 C31 C32 74.9(5) . . . . ? N7 C31 C32 C33 1.7(9) . . . . ? C45 N8 C34 C35 -163.6(3) . . . . ? C56 N8 C34 C35 77.9(3) . . . . ? Eu1 N8 C34 C35 -42.2(3) . . . . ? C36 N9 C35 N10 0.9(4) . . . . ? Eu1 N9 C35 N10 -166.7(2) . . . . ? C36 N9 C35 C34 178.9(3) . . . . ? Eu1 N9 C35 C34 11.3(4) . . . . ? C41 N10 C35 N9 -1.6(4) . . . . ? C42 N10 C35 N9 175.2(3) . . . . ? C41 N10 C35 C34 -179.5(3) . . . . ? C42 N10 C35 C34 -2.7(5) . . . . ? N8 C34 C35 N9 23.5(4) . . . . ? N8 C34 C35 N10 -158.7(3) . . . . ? C35 N9 C36 C37 176.4(4) . . . . ? Eu1 N9 C36 C37 -18.6(6) . . . . ? C35 N9 C36 C41 0.1(4) . . . . ? Eu1 N9 C36 C41 165.0(2) . . . . ? C41 C36 C37 C38 -0.5(6) . . . . ? N9 C36 C37 C38 -176.5(4) . . . . ? C36 C37 C38 C39 0.4(7) . . . . ? C37 C38 C39 C40 -0.4(7) . . . . ? C38 C39 C40 C41 0.5(6) . . . . ? C35 N10 C41 C40 -176.8(4) . . . . ? C42 N10 C41 C40 6.4(6) . . . . ? C35 N10 C41 C36 1.5(4) . . . . ? C42 N10 C41 C36 -175.4(3) . . . . ? C39 C40 C41 N10 177.3(4) . . . . ? C39 C40 C41 C36 -0.7(6) . . . . ? C37 C36 C41 N10 -177.8(3) . . . . ? N9 C36 C41 N10 -1.0(4) . . . . ? C37 C36 C41 C40 0.7(6) . . . . ? N9 C36 C41 C40 177.5(3) . . . . ? C35 N10 C42 C43 -94.8(5) . . . . ? C41 N10 C42 C43 81.4(5) . . . . ? N10 C42 C43 C44 -125.0(8) . . . . ? C34 N8 C45 C46 80.8(3) . . . . ? C56 N8 C45 C46 -159.9(3) . . . . ? Eu1 N8 C45 C46 -39.9(3) . . . . ? C47 N11 C46 N12 0.4(4) . . . . ? Eu1 N11 C46 N12 -162.9(2) . . . . ? C47 N11 C46 C45 178.5(3) . . . . ? Eu1 N11 C46 C45 15.2(4) . . . . ? C52 N12 C46 N11 -0.6(4) . . . . ? C53 N12 C46 N11 -179.3(3) . . . . ? C52 N12 C46 C45 -178.6(3) . . . . ? C53 N12 C46 C45 2.6(6) . . . . ? N8 C45 C46 N11 19.2(5) . . . . ? N8 C45 C46 N12 -162.9(3) . . . . ? C46 N11 C47 C52 -0.1(4) . . . . ? Eu1 N11 C47 C52 159.8(2) . . . . ? C46 N11 C47 C48 178.0(4) . . . . ? Eu1 N11 C47 C48 -22.1(6) . . . . ? C52 C47 C48 C49 -0.6(6) . . . . ? N11 C47 C48 C49 -178.5(4) . . . . ? C47 C48 C49 C50 0.3(7) . . . . ? C48 C49 C50 C51 0.4(8) . . . . ? C49 C50 C51 C52 -0.8(7) . . . . ? N11 C47 C52 N12 -0.2(4) . . . . ? C48 C47 C52 N12 -178.5(3) . . . . ? N11 C47 C52 C51 178.6(3) . . . . ? C48 C47 C52 C51 0.2(6) . . . . ? C46 N12 C52 C47 0.5(4) . . . . ? C53 N12 C52 C47 179.2(3) . . . . ? C46 N12 C52 C51 -178.2(4) . . . . ? C53 N12 C52 C51 0.6(7) . . . . ? C50 C51 C52 C47 0.4(6) . . . . ? C50 C51 C52 N12 178.9(4) . . . . ? C46 N12 C53 C54 -111.0(4) . . . . ? C52 N12 C53 C54 70.5(5) . . . . ? N12 C53 C54 C55 -141.4(5) . . . . ? C45 N8 C56 C57 81.0(3) . . . . ? C34 N8 C56 C57 -159.8(3) . . . . ? Eu1 N8 C56 C57 -39.8(3) . . . . ? C58 N13 C57 N14 -0.4(4) . . . . ? Eu1 N13 C57 N14 -163.9(2) . . . . ? C58 N13 C57 C56 178.5(3) . . . . ? Eu1 N13 C57 C56 15.1(4) . . . . ? C63 N14 C57 N13 0.3(4) . . . . ? C64 N14 C57 N13 176.0(3) . . . . ? C63 N14 C57 C56 -178.6(3) . . . . ? C64 N14 C57 C56 -2.9(5) . . . . ? N8 C56 C57 N13 19.6(4) . . . . ? N8 C56 C57 N14 -161.6(3) . . . . ? C57 N13 C58 C63 0.4(4) . . . . ? Eu1 N13 C58 C63 160.5(2) . . . . ? C57 N13 C58 C59 -179.5(4) . . . . ? Eu1 N13 C58 C59 -19.4(6) . . . . ? C63 C58 C59 C60 0.4(5) . . . . ? N13 C58 C59 C60 -179.7(4) . . . . ? C58 C59 C60 C61 0.7(6) . . . . ? C59 C60 C61 C62 -1.1(7) . . . . ? C60 C61 C62 C63 0.5(6) . . . . ? C57 N14 C63 C58 0.0(4) . . . . ? C64 N14 C63 C58 -175.8(3) . . . . ? C57 N14 C63 C62 -179.2(4) . . . . ? C64 N14 C63 C62 5.1(6) . . . . ? N13 C58 C63 N14 -0.2(4) . . . . ? C59 C58 C63 N14 179.7(3) . . . . ? N13 C58 C63 C62 179.0(3) . . . . ? C59 C58 C63 C62 -1.1(5) . . . . ? C61 C62 C63 N14 179.6(4) . . . . ? C61 C62 C63 C58 0.6(6) . . . . ? C57 N14 C64 C65 -98.8(4) . . . . ? C63 N14 C64 C65 76.1(5) . . . . ? N14 C64 C65 C66 -135.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.140 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.075 #=========================================# data_7 _database_code_depnum_ccdc_archive 'CCDC 698712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C118 H122 Eu2 F18 N28 O22 S6' _chemical_formula_weight 3122.72 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 '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 11.14290(10) _cell_length_b 25.0896(3) _cell_length_c 24.2409(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.0310(10) _cell_angle_gamma 90.00 _cell_volume 6739.54(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8392 _cell_measurement_theta_min 2.5391 _cell_measurement_theta_max 61.8105 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3172 _exptl_absorpt_coefficient_mu 8.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1887 _exptl_absorpt_correction_T_max 0.6805 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type 'Oxford Geimini S' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24199 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 61.85 _reflns_number_total 10002 _reflns_number_gt 6336 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10002 _refine_ls_number_parameters 991 _refine_ls_number_restraints 504 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.031 _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 Eu1 Eu 0.43716(3) 0.278560(13) 0.791077(13) 0.02397(10) Uani 1 1 d . . . N1 N 0.1992(4) 0.27620(19) 0.79481(17) 0.0293(10) Uani 1 1 d . . . N2 N 0.3169(4) 0.34306(17) 0.73006(17) 0.0284(11) Uani 1 1 d . . . N3 N 0.1708(4) 0.34628(19) 0.65931(18) 0.0377(12) Uani 1 1 d . . . N4 N 0.3352(4) 0.19306(17) 0.76625(17) 0.0266(11) Uani 1 1 d . . . N5 N 0.2223(4) 0.12911(19) 0.79968(18) 0.0332(11) Uani 1 1 d . . . N6 N 0.3643(4) 0.29968(18) 0.88227(17) 0.0275(11) Uani 1 1 d . . . N7 N 0.2443(4) 0.35314(19) 0.92571(19) 0.0370(12) Uani 1 1 d . . . N8 N 0.6740(3) 0.27966(19) 0.78557(16) 0.0274(10) Uani 1 1 d . . . N9 N 0.5056(4) 0.26346(17) 0.69844(17) 0.0296(11) Uani 1 1 d . . . N10 N 0.6050(4) 0.30442(18) 0.63494(18) 0.0310(11) Uani 1 1 d . . . N11 N 0.5569(4) 0.20977(17) 0.84680(17) 0.0282(11) Uani 1 1 d . . . N12 N 0.6820(4) 0.14083(19) 0.84010(19) 0.0354(12) Uani 1 1 d . . . N13 N 0.5456(4) 0.36155(17) 0.82320(18) 0.0273(11) Uani 1 1 d . . . N14 N 0.6913(4) 0.39130(19) 0.88707(19) 0.0358(12) Uani 1 1 d . . . C1 C 0.1396(4) 0.2848(2) 0.7377(2) 0.0303(13) Uani 1 1 d . . . H1A H 0.1372 0.2509 0.7167 0.036 Uiso 1 1 calc R . . H1B H 0.0556 0.2971 0.7394 0.036 Uiso 1 1 calc R . . C2 C 0.2079(5) 0.3254(2) 0.7094(2) 0.0334(14) Uani 1 1 d . . . C3 C 0.3523(5) 0.3775(2) 0.6894(2) 0.0330(14) Uani 1 1 d . . . C4 C 0.4578(5) 0.4067(2) 0.6874(2) 0.0379(15) Uani 1 1 d . . . H4A H 0.5191 0.4068 0.7178 0.045 Uiso 1 1 calc R . . C5 C 0.4706(6) 0.4354(2) 0.6400(3) 0.0469(17) Uani 1 1 d . . . H5A H 0.5420 0.4556 0.6378 0.056 Uiso 1 1 calc R . . C6 C 0.3827(6) 0.4355(3) 0.5959(3) 0.0535(18) Uani 1 1 d . . . H6A H 0.3956 0.4551 0.5636 0.064 Uiso 1 1 calc R . . C7 C 0.2746(6) 0.4074(2) 0.5974(3) 0.0465(17) Uani 1 1 d . . . H7A H 0.2129 0.4078 0.5672 0.056 Uiso 1 1 calc R . . C8 C 0.2629(5) 0.3791(2) 0.6453(2) 0.0352(14) Uani 1 1 d . . . C9 C 0.0589(5) 0.3349(3) 0.6250(3) 0.0537(18) Uani 1 1 d . . . H9A H 0.0100 0.3103 0.6446 0.081 Uiso 1 1 calc R . . H9B H 0.0772 0.3186 0.5901 0.081 Uiso 1 1 calc R . . H9C H 0.0142 0.3682 0.6171 0.081 Uiso 1 1 calc R . . C10 C 0.1654(4) 0.2233(2) 0.8161(2) 0.0323(13) Uani 1 1 d . . . H10A H 0.1781 0.2231 0.8571 0.039 Uiso 1 1 calc R . . H10B H 0.0791 0.2161 0.8046 0.039 Uiso 1 1 calc R . . C11 C 0.2407(5) 0.1815(2) 0.7936(2) 0.0308(14) Uani 1 1 d . . . C12 C 0.3824(5) 0.1426(2) 0.7540(2) 0.0345(14) Uani 1 1 d . . . C13 C 0.4782(5) 0.1296(2) 0.7243(2) 0.0357(15) Uani 1 1 d . . . H13A H 0.5246 0.1563 0.7086 0.043 Uiso 1 1 calc R . . C14 C 0.5030(6) 0.0761(3) 0.7185(3) 0.0481(17) Uani 1 1 d . . . H14A H 0.5686 0.0658 0.6989 0.058 Uiso 1 1 calc R . . C15 C 0.4345(6) 0.0371(3) 0.7408(3) 0.0525(18) Uani 1 1 d . . . H15A H 0.4554 0.0007 0.7364 0.063 Uiso 1 1 calc R . . C16 C 0.3370(6) 0.0491(2) 0.7692(3) 0.0480(17) Uani 1 1 d . . . H16A H 0.2897 0.0222 0.7840 0.058 Uiso 1 1 calc R . . C17 C 0.3120(5) 0.1029(2) 0.7748(2) 0.0340(14) Uani 1 1 d . . . C18 C 0.1292(5) 0.1042(3) 0.8298(3) 0.0490(17) Uani 1 1 d . . . H18A H 0.0769 0.1319 0.8428 0.073 Uiso 1 1 calc R . . H18B H 0.1678 0.0843 0.8616 0.073 Uiso 1 1 calc R . . H18C H 0.0808 0.0798 0.8050 0.073 Uiso 1 1 calc R . . C19 C 0.1633(5) 0.3193(2) 0.8323(2) 0.0345(15) Uani 1 1 d . . . H19A H 0.1562 0.3537 0.8122 0.041 Uiso 1 1 calc R . . H19B H 0.0841 0.3108 0.8453 0.041 Uiso 1 1 calc R . . C20 C 0.2574(5) 0.3231(2) 0.8806(2) 0.0342(15) Uani 1 1 d . . . C21 C 0.4253(5) 0.3153(2) 0.9332(2) 0.0307(14) Uani 1 1 d . . . C22 C 0.5401(5) 0.3020(2) 0.9577(2) 0.0365(15) Uani 1 1 d . . . H22A H 0.5911 0.2790 0.9396 0.044 Uiso 1 1 calc R . . C23 C 0.5773(6) 0.3233(3) 1.0087(2) 0.0471(17) Uani 1 1 d . . . H23A H 0.6550 0.3146 1.0263 0.056 Uiso 1 1 calc R . . C24 C 0.5021(6) 0.3580(3) 1.0354(3) 0.0497(18) Uani 1 1 d . . . H24A H 0.5309 0.3725 1.0706 0.060 Uiso 1 1 calc R . . C25 C 0.3890(6) 0.3712(3) 1.0121(2) 0.0467(17) Uani 1 1 d . . . H25A H 0.3382 0.3945 1.0301 0.056 Uiso 1 1 calc R . . C26 C 0.3525(5) 0.3489(2) 0.9608(2) 0.0337(14) Uani 1 1 d . . . C27 C 0.1393(5) 0.3853(3) 0.9362(3) 0.0570(19) Uani 1 1 d . . . H27A H 0.0754 0.3806 0.9055 0.086 Uiso 1 1 calc R . . H27B H 0.1625 0.4229 0.9390 0.086 Uiso 1 1 calc R . . H27C H 0.1097 0.3737 0.9709 0.086 Uiso 1 1 calc R . . C28 C 0.6990(5) 0.3062(2) 0.7330(2) 0.0320(14) Uani 1 1 d . . . H28A H 0.6987 0.3454 0.7378 0.038 Uiso 1 1 calc R . . H28B H 0.7793 0.2954 0.7230 0.038 Uiso 1 1 calc R . . C29 C 0.6043(5) 0.2904(2) 0.6885(2) 0.0276(13) Uani 1 1 d . . . C30 C 0.4364(5) 0.2598(2) 0.6461(2) 0.0309(14) Uani 1 1 d . . . C31 C 0.3239(5) 0.2363(2) 0.6312(2) 0.0374(15) Uani 1 1 d . . . H31A H 0.2827 0.2172 0.6573 0.045 Uiso 1 1 calc R . . C32 C 0.2756(5) 0.2422(2) 0.5771(2) 0.0399(15) Uani 1 1 d . . . H32A H 0.1990 0.2270 0.5655 0.048 Uiso 1 1 calc R . . C33 C 0.3368(5) 0.2700(3) 0.5386(2) 0.0472(17) Uani 1 1 d . . . H33A H 0.2995 0.2743 0.5018 0.057 Uiso 1 1 calc R . . C34 C 0.4486(5) 0.2913(2) 0.5525(2) 0.0414(16) Uani 1 1 d . . . H34A H 0.4905 0.3092 0.5258 0.050 Uiso 1 1 calc R . . C35 C 0.4981(5) 0.2860(2) 0.6064(2) 0.0345(14) Uani 1 1 d . . . C36 C 0.6997(5) 0.3338(3) 0.6113(2) 0.0472(16) Uani 1 1 d . . . H36A H 0.7655 0.3414 0.6404 0.071 Uiso 1 1 calc R . . H36B H 0.6670 0.3674 0.5956 0.071 Uiso 1 1 calc R . . H36C H 0.7307 0.3125 0.5820 0.071 Uiso 1 1 calc R . . C37 C 0.7193(4) 0.2234(2) 0.7861(2) 0.0307(13) Uani 1 1 d . . . H37A H 0.7054 0.2080 0.7484 0.037 Uiso 1 1 calc R . . H37B H 0.8071 0.2227 0.7979 0.037 Uiso 1 1 calc R . . C38 C 0.6538(5) 0.1918(2) 0.8253(2) 0.0297(14) Uani 1 1 d . . . C39 C 0.5190(5) 0.1682(2) 0.8786(2) 0.0310(14) Uani 1 1 d . . . C40 C 0.4225(5) 0.1635(2) 0.9104(2) 0.0347(14) Uani 1 1 d . . . H40A H 0.3693 0.1926 0.9141 0.042 Uiso 1 1 calc R . . C41 C 0.4060(5) 0.1160(2) 0.9361(2) 0.0424(16) Uani 1 1 d . . . H41A H 0.3396 0.1120 0.9574 0.051 Uiso 1 1 calc R . . C42 C 0.4842(6) 0.0732(3) 0.9320(3) 0.0545(18) Uani 1 1 d . . . H42A H 0.4703 0.0409 0.9508 0.065 Uiso 1 1 calc R . . C43 C 0.5818(6) 0.0765(3) 0.9012(3) 0.0501(17) Uani 1 1 d . . . H43A H 0.6354 0.0474 0.8984 0.060 Uiso 1 1 calc R . . C44 C 0.5968(5) 0.1247(2) 0.8746(2) 0.0355(15) Uani 1 1 d . . . C45 C 0.7775(5) 0.1079(2) 0.8214(3) 0.0502(17) Uani 1 1 d . . . H45A H 0.8260 0.1292 0.7981 0.075 Uiso 1 1 calc R . . H45B H 0.7417 0.0777 0.7998 0.075 Uiso 1 1 calc R . . H45C H 0.8292 0.0945 0.8536 0.075 Uiso 1 1 calc R . . C46 C 0.7360(5) 0.3091(2) 0.8337(2) 0.0346(14) Uani 1 1 d . . . H46A H 0.8152 0.3223 0.8245 0.042 Uiso 1 1 calc R . . H46B H 0.7500 0.2850 0.8661 0.042 Uiso 1 1 calc R . . C47 C 0.6573(5) 0.3553(2) 0.8472(2) 0.0329(14) Uani 1 1 d . . . C48 C 0.5029(5) 0.4070(2) 0.8489(2) 0.0319(14) Uani 1 1 d . . . C49 C 0.3925(5) 0.4327(2) 0.8405(2) 0.0345(14) Uani 1 1 d . . . H49A H 0.3316 0.4214 0.8126 0.041 Uiso 1 1 calc R . . C50 C 0.3748(6) 0.4757(2) 0.8746(3) 0.0460(17) Uani 1 1 d . . . H50A H 0.2993 0.4936 0.8704 0.055 Uiso 1 1 calc R . . C51 C 0.4651(6) 0.4935(2) 0.9151(3) 0.0469(17) Uani 1 1 d . . . H51A H 0.4492 0.5230 0.9377 0.056 Uiso 1 1 calc R . . C52 C 0.5762(6) 0.4690(2) 0.9227(3) 0.0447(16) Uani 1 1 d . . . H52A H 0.6381 0.4814 0.9496 0.054 Uiso 1 1 calc R . . C53 C 0.5932(5) 0.4256(2) 0.8893(2) 0.0340(14) Uani 1 1 d . . . C54 C 0.8054(5) 0.3938(3) 0.9214(3) 0.0557(19) Uani 1 1 d . . . H54A H 0.8580 0.3650 0.9110 0.084 Uiso 1 1 calc R . . H54B H 0.7916 0.3898 0.9604 0.084 Uiso 1 1 calc R . . H54C H 0.8440 0.4282 0.9160 0.084 Uiso 1 1 calc R . . C56 C 0.8435(6) 0.1330(3) 0.6384(3) 0.063(2) Uani 1 1 d . . . S2 S 0.93351(14) 0.18382(7) 0.67445(6) 0.0440(4) Uani 1 1 d . . . O4 O 0.8654(4) 0.23140(18) 0.66327(19) 0.0654(14) Uani 1 1 d U . . O5 O 1.0460(4) 0.18156(19) 0.6487(2) 0.0667(14) Uani 1 1 d U . . O6 O 0.9445(4) 0.1671(2) 0.73109(17) 0.0628(13) Uani 1 1 d U . . F4 F 0.7319(4) 0.1342(2) 0.6545(2) 0.1032(17) Uani 1 1 d U . . F5 F 0.8896(4) 0.08450(16) 0.6482(2) 0.0887(15) Uani 1 1 d U . . F6 F 0.8330(4) 0.13975(19) 0.58384(17) 0.0870(14) Uani 1 1 d U . . S1 S 0.98510(14) 0.21928(9) 0.93404(6) 0.0555(5) Uani 1 1 d DU A 1 C55 C 0.8877(8) 0.2218(5) 0.9856(3) 0.088(2) Uani 1 1 d U A 1 O1 O 1.0979(8) 0.2025(5) 0.9522(4) 0.058(3) Uani 0.50 1 d PU A 1 O2 O 0.917(2) 0.1918(7) 0.8916(7) 0.064(5) Uani 0.50 1 d PU A 1 O3 O 0.9840(9) 0.2796(4) 0.9224(4) 0.074(3) Uani 0.50 1 d PU A 1 F1 F 0.9427(17) 0.2514(6) 1.0315(8) 0.098(5) Uani 0.50 1 d PU A 1 F2 F 0.8810(8) 0.1678(4) 1.0050(4) 0.090(3) Uani 0.50 1 d PU A 1 F3 F 0.7762(11) 0.2334(6) 0.9701(5) 0.092(4) Uani 0.50 1 d PU A 1 O1' O 1.0370(14) 0.1678(6) 0.9567(6) 0.133(5) Uani 0.50 1 d PDU B 2 O2' O 0.927(2) 0.2109(8) 0.8809(6) 0.069(5) Uani 0.50 1 d PDU C 2 O3' O 1.0838(11) 0.2510(6) 0.9483(5) 0.099(4) Uani 0.50 1 d PDU D 2 F1' F 0.9123(14) 0.2272(7) 1.0327(7) 0.085(4) Uani 0.50 1 d PU E 2 F2' F 0.7846(15) 0.1964(7) 0.9755(7) 0.125(4) Uani 0.50 1 d PU F 2 F3' F 0.8350(12) 0.2760(5) 0.9715(5) 0.121(4) Uani 0.50 1 d PU G 2 S3 S 0.90227(16) 0.42293(7) 0.75067(9) 0.0557(5) Uani 1 1 d U H 1 C57 C 1.0189(10) 0.4702(4) 0.7610(5) 0.101(3) Uani 1 1 d U H 1 O7 O 0.8113(8) 0.4380(4) 0.7857(5) 0.065(3) Uani 0.50 1 d PU H 1 O8 O 0.8615(10) 0.4419(4) 0.6903(4) 0.067(3) Uani 0.50 1 d PU H 1 O9 O 0.9476(13) 0.3741(7) 0.7603(5) 0.055(3) Uani 0.50 1 d PU H 1 F7 F 1.0603(11) 0.4610(4) 0.8229(4) 0.093(3) Uani 0.50 1 d PU H 1 F8 F 1.1200(8) 0.4571(5) 0.7392(5) 0.079(3) Uani 0.50 1 d PU H 1 F9 F 1.002(2) 0.5185(11) 0.7573(9) 0.077(5) Uani 0.50 1 d PU H 1 O7' O 0.9180(15) 0.4175(7) 0.8141(6) 0.145(5) Uani 0.50 1 d PU I 2 O8' O 0.8048(13) 0.4361(5) 0.7273(8) 0.113(4) Uani 0.50 1 d PU J 2 O9' O 0.9558(16) 0.3747(8) 0.7315(6) 0.076(4) Uani 0.50 1 d PU K 2 F7' F 1.1161(13) 0.4611(6) 0.7847(8) 0.132(4) Uani 0.50 1 d PU L 2 F8' F 1.0435(14) 0.4768(6) 0.7011(6) 0.166(5) Uani 0.50 1 d PU M 2 F9' F 0.974(2) 0.5196(13) 0.7728(10) 0.103(6) Uani 0.50 1 d PU N 2 O1W O 0.1277(8) 0.4738(3) 1.0414(4) 0.209(4) Uani 1 1 d DU . . H1WA H 0.0639 0.4684 1.0205 0.313 Uiso 1 1 calc RD . . C59 C 0.1948(9) 0.4333(5) 1.1335(4) 0.134(4) Uani 1 1 d DU . . H59A H 0.1505 0.4072 1.1537 0.201 Uiso 1 1 calc R . . H59B H 0.2203 0.4630 1.1582 0.201 Uiso 1 1 calc R . . H59C H 0.2659 0.4162 1.1207 0.201 Uiso 1 1 calc R . . C58 C 0.1195(13) 0.4525(6) 1.0876(5) 0.175(5) Uani 1 1 d DU . . H58A H 0.0674 0.4213 1.0774 0.210 Uiso 1 1 calc R . . H58B H 0.0668 0.4778 1.1051 0.210 Uiso 1 1 calc R . . O2W O 1.143(2) -0.0344(12) 0.9470(13) 0.254(10) Uani 0.50 1 d PU . . O2W' O 1.224(2) -0.0193(10) 0.9618(12) 0.220(9) Uani 0.50 1 d PU . . 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 Eu1 0.02236(16) 0.02179(17) 0.02780(16) -0.0024(2) 0.00273(11) -0.00017(19) N1 0.032(2) 0.022(3) 0.034(2) -0.005(3) 0.005(2) 0.002(2) N2 0.029(3) 0.024(3) 0.031(2) 0.000(2) 0.000(2) 0.001(2) N3 0.037(3) 0.038(3) 0.036(3) 0.004(3) -0.009(2) 0.002(3) N4 0.026(2) 0.022(3) 0.033(2) 0.001(2) 0.008(2) 0.001(2) N5 0.032(3) 0.028(3) 0.040(3) -0.003(3) 0.005(2) -0.010(2) N6 0.023(2) 0.029(3) 0.031(2) -0.001(2) 0.005(2) 0.003(2) N7 0.031(3) 0.036(3) 0.045(3) -0.010(3) 0.010(2) -0.002(2) N8 0.028(2) 0.025(3) 0.029(2) -0.004(3) 0.0006(19) -0.001(2) N9 0.026(2) 0.029(3) 0.034(3) -0.001(2) 0.004(2) 0.001(2) N10 0.028(3) 0.032(3) 0.034(3) 0.004(2) 0.010(2) 0.003(2) N11 0.027(2) 0.025(3) 0.033(2) 0.000(2) 0.003(2) 0.004(2) N12 0.030(3) 0.031(3) 0.045(3) 0.001(3) 0.004(2) 0.005(2) N13 0.027(3) 0.018(3) 0.037(3) -0.001(2) 0.005(2) 0.000(2) N14 0.031(3) 0.031(3) 0.045(3) -0.011(3) 0.001(2) -0.011(2) C1 0.021(3) 0.032(3) 0.036(3) -0.002(3) -0.002(2) -0.002(3) C2 0.028(3) 0.031(4) 0.042(3) -0.004(3) 0.002(3) 0.008(3) C3 0.034(3) 0.024(3) 0.041(3) -0.008(3) 0.006(3) 0.009(3) C4 0.043(4) 0.026(3) 0.044(4) -0.001(3) 0.004(3) -0.003(3) C5 0.059(4) 0.034(4) 0.049(4) 0.002(4) 0.010(4) -0.010(3) C6 0.083(5) 0.036(4) 0.044(4) 0.011(4) 0.015(4) 0.006(4) C7 0.054(4) 0.037(4) 0.047(4) 0.004(4) -0.005(3) 0.005(4) C8 0.047(4) 0.022(3) 0.037(3) 0.003(3) 0.006(3) 0.005(3) C9 0.044(4) 0.061(5) 0.050(4) 0.007(4) -0.022(3) -0.003(4) C10 0.027(3) 0.035(3) 0.035(3) 0.005(3) 0.005(2) -0.003(3) C11 0.029(3) 0.024(3) 0.037(3) -0.006(3) -0.009(3) 0.005(3) C12 0.037(3) 0.026(3) 0.039(3) -0.006(3) -0.001(3) -0.004(3) C13 0.035(3) 0.025(3) 0.049(4) -0.008(3) 0.010(3) -0.005(3) C14 0.048(4) 0.040(4) 0.057(4) -0.019(4) 0.011(3) 0.002(4) C15 0.060(4) 0.023(4) 0.074(5) -0.011(4) 0.008(4) 0.001(4) C16 0.058(4) 0.023(4) 0.064(4) -0.012(4) 0.011(4) -0.010(3) C17 0.034(3) 0.027(3) 0.040(3) -0.006(3) -0.001(3) -0.002(3) C18 0.048(4) 0.039(4) 0.062(4) 0.007(4) 0.014(3) -0.014(3) C19 0.027(3) 0.035(4) 0.042(3) -0.010(3) 0.004(3) 0.008(3) C20 0.036(4) 0.034(4) 0.035(3) -0.012(3) 0.013(3) -0.006(3) C21 0.035(3) 0.028(3) 0.029(3) 0.000(3) 0.005(3) -0.007(3) C22 0.040(4) 0.035(4) 0.035(3) -0.003(3) 0.006(3) -0.005(3) C23 0.049(4) 0.050(4) 0.040(4) 0.001(4) -0.001(3) -0.011(4) C24 0.067(5) 0.045(4) 0.037(3) -0.010(4) -0.001(3) -0.009(4) C25 0.059(4) 0.039(4) 0.044(4) -0.016(4) 0.012(3) -0.009(4) C26 0.045(4) 0.020(3) 0.038(3) -0.005(3) 0.015(3) -0.006(3) C27 0.042(4) 0.063(5) 0.068(4) -0.029(4) 0.013(3) 0.012(4) C28 0.027(3) 0.030(3) 0.039(3) -0.003(3) 0.006(3) -0.003(3) C29 0.029(3) 0.020(3) 0.034(3) -0.004(3) 0.006(2) 0.007(3) C30 0.035(3) 0.031(3) 0.027(3) -0.002(3) 0.006(3) 0.005(3) C31 0.038(3) 0.043(4) 0.032(3) 0.001(3) 0.006(3) -0.006(3) C32 0.036(3) 0.048(4) 0.035(3) -0.007(3) -0.003(3) -0.001(3) C33 0.047(4) 0.060(5) 0.034(3) -0.009(4) 0.000(3) 0.008(4) C34 0.049(4) 0.044(4) 0.031(3) 0.008(3) 0.005(3) 0.010(3) C35 0.042(3) 0.030(4) 0.032(3) -0.008(3) 0.005(3) 0.011(3) C36 0.048(4) 0.047(4) 0.049(4) 0.011(4) 0.012(3) 0.001(4) C37 0.025(3) 0.028(3) 0.038(3) -0.001(3) 0.001(2) -0.001(3) C38 0.027(3) 0.026(3) 0.035(3) -0.003(3) -0.004(3) 0.000(3) C39 0.032(3) 0.030(3) 0.030(3) -0.004(3) 0.001(3) -0.002(3) C40 0.042(4) 0.029(4) 0.032(3) -0.007(3) 0.000(3) 0.004(3) C41 0.049(4) 0.035(4) 0.045(4) 0.007(3) 0.011(3) 0.000(3) C42 0.070(5) 0.038(4) 0.056(4) 0.007(4) 0.009(4) -0.003(4) C43 0.048(4) 0.035(4) 0.069(4) 0.009(4) 0.011(3) 0.007(3) C44 0.040(4) 0.029(4) 0.038(3) 0.000(3) 0.006(3) 0.002(3) C45 0.043(4) 0.037(4) 0.071(5) 0.004(4) 0.011(3) 0.014(3) C46 0.028(3) 0.037(4) 0.039(3) -0.007(3) 0.004(3) -0.002(3) C47 0.033(3) 0.025(3) 0.041(3) 0.001(3) 0.005(3) -0.006(3) C48 0.036(3) 0.025(3) 0.036(3) 0.001(3) 0.011(3) -0.010(3) C49 0.036(3) 0.021(3) 0.046(3) 0.000(3) 0.003(3) -0.004(3) C50 0.055(4) 0.025(4) 0.061(4) 0.004(4) 0.025(4) 0.004(3) C51 0.060(5) 0.030(4) 0.053(4) -0.017(3) 0.020(4) -0.002(4) C52 0.057(4) 0.032(4) 0.046(4) -0.013(3) 0.011(3) -0.010(4) C53 0.033(3) 0.031(4) 0.039(3) -0.001(3) 0.010(3) -0.007(3) C54 0.040(4) 0.058(5) 0.067(4) -0.033(4) -0.006(3) -0.005(4) C56 0.053(5) 0.061(6) 0.073(5) 0.008(5) -0.003(4) -0.002(4) S2 0.0472(9) 0.0406(10) 0.0449(9) -0.0057(9) 0.0086(7) -0.0031(8) O4 0.082(3) 0.049(3) 0.067(3) 0.002(3) 0.014(3) 0.015(3) O5 0.052(3) 0.068(3) 0.085(3) -0.010(3) 0.030(2) -0.012(3) O6 0.061(3) 0.082(4) 0.044(3) -0.005(3) 0.002(2) 0.001(3) F4 0.050(3) 0.128(4) 0.132(4) -0.025(4) 0.010(3) -0.026(3) F5 0.102(3) 0.043(3) 0.115(4) 0.003(3) -0.022(3) -0.009(3) F6 0.104(3) 0.091(4) 0.058(3) -0.012(3) -0.028(2) 0.009(3) S1 0.0404(9) 0.0837(14) 0.0429(9) -0.0059(12) 0.0063(7) -0.0120(11) C55 0.064(5) 0.136(7) 0.064(5) 0.019(6) 0.011(4) 0.020(5) O1 0.028(5) 0.089(7) 0.054(5) -0.008(6) -0.004(4) -0.015(5) O2 0.068(7) 0.073(9) 0.050(8) 0.004(7) 0.007(7) -0.009(7) O3 0.078(6) 0.054(6) 0.092(7) 0.012(6) 0.014(5) -0.006(6) F1 0.114(10) 0.125(11) 0.057(6) -0.021(8) 0.012(7) 0.027(8) F2 0.072(5) 0.107(7) 0.095(6) 0.058(6) 0.032(5) 0.009(5) F3 0.053(5) 0.135(9) 0.094(6) 0.047(8) 0.031(5) 0.035(7) O1' 0.135(9) 0.156(10) 0.114(8) -0.012(9) 0.040(8) 0.024(9) O2' 0.049(6) 0.123(12) 0.035(6) 0.010(8) 0.002(5) 0.000(9) O3' 0.086(7) 0.125(8) 0.087(7) -0.019(8) 0.017(6) -0.037(8) F1' 0.076(7) 0.145(10) 0.036(5) 0.025(8) 0.012(5) 0.013(8) F2' 0.096(7) 0.157(10) 0.127(8) 0.010(9) 0.036(6) -0.029(8) F3' 0.125(8) 0.129(8) 0.109(7) 0.013(8) 0.015(6) 0.064(7) S3 0.0409(10) 0.0388(11) 0.0873(14) -0.0076(11) 0.0072(9) -0.0012(9) C57 0.098(6) 0.072(5) 0.126(7) 0.009(6) -0.023(6) -0.014(5) O7 0.051(5) 0.051(5) 0.102(7) 0.017(6) 0.047(5) 0.030(5) O8 0.089(7) 0.068(6) 0.040(5) 0.000(5) -0.010(5) -0.008(6) O9 0.037(5) 0.038(6) 0.091(8) 0.003(8) 0.002(7) 0.000(5) F7 0.121(8) 0.072(6) 0.076(6) 0.014(6) -0.039(5) -0.017(6) F8 0.037(5) 0.100(7) 0.102(7) -0.004(7) 0.018(5) -0.019(5) F9 0.105(10) 0.025(6) 0.096(9) 0.002(7) -0.009(7) -0.006(7) O7' 0.150(10) 0.153(10) 0.136(9) 0.009(9) 0.037(8) -0.020(9) O8' 0.098(8) 0.067(7) 0.166(9) -0.016(8) -0.027(8) 0.009(7) O9' 0.064(7) 0.053(7) 0.112(10) -0.020(9) 0.017(8) 0.020(6) F7' 0.102(8) 0.097(7) 0.185(10) 0.015(10) -0.044(8) -0.018(7) F8' 0.179(10) 0.156(10) 0.171(10) 0.025(9) 0.055(9) -0.026(8) F9' 0.118(12) 0.052(7) 0.131(12) -0.018(9) -0.024(9) -0.006(8) O1W 0.259(9) 0.177(8) 0.193(8) -0.099(8) 0.030(8) -0.035(7) C59 0.109(8) 0.175(10) 0.116(8) 0.017(8) 0.001(6) -0.038(7) C58 0.205(10) 0.209(11) 0.127(8) -0.027(9) 0.091(8) -0.061(9) O2W 0.249(18) 0.234(15) 0.278(16) -0.025(13) 0.029(15) -0.010(15) O2W' 0.188(16) 0.192(14) 0.272(15) 0.017(13) -0.008(14) -0.010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N4 2.472(4) . ? Eu1 N9 2.476(4) . ? Eu1 N2 2.487(4) . ? Eu1 N13 2.491(4) . ? Eu1 N6 2.491(4) . ? Eu1 N11 2.491(4) . ? Eu1 N8 2.657(4) . ? Eu1 N1 2.663(4) . ? N1 C10 1.486(7) . ? N1 C1 1.486(6) . ? N1 C19 1.494(6) . ? N2 C2 1.339(6) . ? N2 C3 1.400(7) . ? N3 C2 1.348(7) . ? N3 C8 1.386(7) . ? N3 C9 1.452(7) . ? N4 C11 1.334(7) . ? N4 C12 1.414(7) . ? N5 C11 1.341(7) . ? N5 C17 1.387(7) . ? N5 C18 1.469(7) . ? N6 C20 1.325(6) . ? N6 C21 1.402(7) . ? N7 C20 1.349(6) . ? N7 C26 1.405(7) . ? N7 C27 1.464(7) . ? N8 C46 1.488(7) . ? N8 C28 1.490(6) . ? N8 C37 1.498(7) . ? N9 C29 1.333(6) . ? N9 C30 1.416(7) . ? N10 C29 1.347(7) . ? N10 C35 1.393(7) . ? N10 C36 1.454(7) . ? N11 C38 1.327(6) . ? N11 C39 1.388(6) . ? N12 C38 1.357(7) . ? N12 C44 1.390(7) . ? N12 C45 1.457(7) . ? N13 C47 1.327(7) . ? N13 C48 1.407(7) . ? N14 C47 1.347(7) . ? N14 C53 1.396(7) . ? N14 C54 1.446(7) . ? C1 C2 1.483(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.382(8) . ? C3 C4 1.390(7) . ? C4 C5 1.376(8) . ? C4 H4A 0.9500 . ? C5 C6 1.372(9) . ? C5 H5A 0.9500 . ? C6 C7 1.399(8) . ? C6 H6A 0.9500 . ? C7 C8 1.379(8) . ? C7 H7A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.482(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C13 1.389(7) . ? C12 C17 1.395(7) . ? C13 C14 1.379(8) . ? C13 H13A 0.9500 . ? C14 C15 1.387(8) . ? C14 H14A 0.9500 . ? C15 C16 1.378(8) . ? C15 H15A 0.9500 . ? C16 C17 1.386(8) . ? C16 H16A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.490(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 C26 1.390(7) . ? C21 C22 1.392(7) . ? C22 C23 1.370(8) . ? C22 H22A 0.9500 . ? C23 C24 1.411(8) . ? C23 H23A 0.9500 . ? C24 C25 1.367(8) . ? C24 H24A 0.9500 . ? C25 C26 1.385(8) . ? C25 H25A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.482(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C30 C31 1.398(7) . ? C30 C35 1.403(7) . ? C31 C32 1.372(8) . ? C31 H31A 0.9500 . ? C32 C33 1.398(8) . ? C32 H32A 0.9500 . ? C33 C34 1.365(8) . ? C33 H33A 0.9500 . ? C34 C35 1.370(8) . ? C34 H34A 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.486(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C39 C40 1.393(7) . ? C39 C44 1.404(8) . ? C40 C41 1.367(8) . ? C40 H40A 0.9500 . ? C41 C42 1.393(8) . ? C41 H41A 0.9500 . ? C42 C43 1.385(8) . ? C42 H42A 0.9500 . ? C43 C44 1.389(8) . ? C43 H43A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.511(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C48 C49 1.385(7) . ? C48 C53 1.406(8) . ? C49 C50 1.385(8) . ? C49 H49A 0.9500 . ? C50 C51 1.403(8) . ? C50 H50A 0.9500 . ? C51 C52 1.377(8) . ? C51 H51A 0.9500 . ? C52 C53 1.383(7) . ? C52 H52A 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C56 F6 1.327(8) . ? C56 F5 1.332(8) . ? C56 F4 1.341(8) . ? C56 S2 1.793(8) . ? S2 O4 1.425(5) . ? S2 O6 1.429(4) . ? S2 O5 1.459(4) . ? S1 O1 1.355(10) . ? S1 O2 1.395(19) . ? S1 O3 1.540(10) . ? S1 C55 1.740(8) . ? C55 F3 1.293(14) . ? C55 F1 1.424(19) . ? C55 F2 1.439(14) . ? S3 O9 1.337(18) . ? S3 O7 1.440(8) . ? S3 O8 1.560(9) . ? S3 C57 1.758(10) . ? C57 F9 1.23(3) . ? C57 F8 1.336(14) . ? C57 F7 1.541(15) . ? O1W C58 1.253(11) . ? O1W H1WA 0.8400 . ? C59 C58 1.408(13) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O2W O2W' 1.02(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Eu1 N9 79.85(14) . . ? N4 Eu1 N2 102.40(14) . . ? N9 Eu1 N2 76.02(14) . . ? N4 Eu1 N13 175.53(14) . . ? N9 Eu1 N13 103.06(14) . . ? N2 Eu1 N13 81.69(14) . . ? N4 Eu1 N6 102.50(14) . . ? N9 Eu1 N6 176.29(15) . . ? N2 Eu1 N6 100.59(14) . . ? N13 Eu1 N6 74.77(14) . . ? N4 Eu1 N11 74.75(14) . . ? N9 Eu1 N11 100.80(14) . . ? N2 Eu1 N11 176.16(14) . . ? N13 Eu1 N11 101.25(14) . . ? N6 Eu1 N11 82.65(14) . . ? N4 Eu1 N8 115.48(14) . . ? N9 Eu1 N8 63.49(13) . . ? N2 Eu1 N8 116.07(14) . . ? N13 Eu1 N8 63.59(14) . . ? N6 Eu1 N8 117.42(13) . . ? N11 Eu1 N8 63.65(14) . . ? N4 Eu1 N1 63.60(14) . . ? N9 Eu1 N1 115.48(13) . . ? N2 Eu1 N1 63.80(14) . . ? N13 Eu1 N1 117.38(14) . . ? N6 Eu1 N1 63.64(13) . . ? N11 Eu1 N1 116.39(14) . . ? N8 Eu1 N1 178.85(14) . . ? C10 N1 C1 110.4(4) . . ? C10 N1 C19 109.9(4) . . ? C1 N1 C19 109.8(4) . . ? C10 N1 Eu1 108.7(3) . . ? C1 N1 Eu1 108.3(3) . . ? C19 N1 Eu1 109.6(3) . . ? C2 N2 C3 104.7(4) . . ? C2 N2 Eu1 114.7(4) . . ? C3 N2 Eu1 130.3(3) . . ? C2 N3 C8 106.7(5) . . ? C2 N3 C9 127.2(5) . . ? C8 N3 C9 126.1(5) . . ? C11 N4 C12 103.9(4) . . ? C11 N4 Eu1 115.7(3) . . ? C12 N4 Eu1 131.1(3) . . ? C11 N5 C17 107.0(5) . . ? C11 N5 C18 126.5(5) . . ? C17 N5 C18 126.4(5) . . ? C20 N6 C21 104.8(4) . . ? C20 N6 Eu1 116.3(3) . . ? C21 N6 Eu1 131.9(3) . . ? C20 N7 C26 106.9(4) . . ? C20 N7 C27 127.2(5) . . ? C26 N7 C27 125.9(5) . . ? C46 N8 C28 109.6(4) . . ? C46 N8 C37 109.4(4) . . ? C28 N8 C37 109.6(4) . . ? C46 N8 Eu1 110.4(3) . . ? C28 N8 Eu1 108.9(3) . . ? C37 N8 Eu1 109.0(3) . . ? C29 N9 C30 104.6(4) . . ? C29 N9 Eu1 115.1(3) . . ? C30 N9 Eu1 129.1(3) . . ? C29 N10 C35 107.5(4) . . ? C29 N10 C36 126.2(5) . . ? C35 N10 C36 126.3(5) . . ? C38 N11 C39 105.7(4) . . ? C38 N11 Eu1 115.7(3) . . ? C39 N11 Eu1 130.1(3) . . ? C38 N12 C44 106.2(5) . . ? C38 N12 C45 127.5(5) . . ? C44 N12 C45 126.1(5) . . ? C47 N13 C48 104.2(4) . . ? C47 N13 Eu1 116.1(4) . . ? C48 N13 Eu1 129.9(3) . . ? C47 N14 C53 106.2(5) . . ? C47 N14 C54 127.2(5) . . ? C53 N14 C54 126.6(5) . . ? C2 C1 N1 109.2(4) . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 112.9(5) . . ? N2 C2 C1 123.0(5) . . ? N3 C2 C1 124.1(5) . . ? C8 C3 C4 120.2(6) . . ? C8 C3 N2 109.2(5) . . ? C4 C3 N2 130.6(5) . . ? C5 C4 C3 117.8(6) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? C6 C5 C4 121.6(6) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C7 121.7(6) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C8 C7 C6 116.0(6) . . ? C8 C7 H7A 122.0 . . ? C6 C7 H7A 122.0 . . ? C7 C8 C3 122.8(6) . . ? C7 C8 N3 130.6(6) . . ? C3 C8 N3 106.6(5) . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N1 109.3(4) . . ? C11 C10 H10A 109.8 . . ? N1 C10 H10A 109.8 . . ? C11 C10 H10B 109.8 . . ? N1 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? N4 C11 N5 113.9(5) . . ? N4 C11 C10 122.4(5) . . ? N5 C11 C10 123.7(5) . . ? C13 C12 C17 120.7(5) . . ? C13 C12 N4 130.0(5) . . ? C17 C12 N4 109.2(5) . . ? C14 C13 C12 117.0(6) . . ? C14 C13 H13A 121.5 . . ? C12 C13 H13A 121.5 . . ? C13 C14 C15 121.6(6) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C16 C15 C14 122.2(6) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C15 C16 C17 116.1(6) . . ? C15 C16 H16A 122.0 . . ? C17 C16 H16A 122.0 . . ? C16 C17 N5 131.7(6) . . ? C16 C17 C12 122.3(5) . . ? N5 C17 C12 106.0(5) . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N1 108.2(4) . . ? C20 C19 H19A 110.0 . . ? N1 C19 H19A 110.0 . . ? C20 C19 H19B 110.0 . . ? N1 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? N6 C20 N7 113.4(5) . . ? N6 C20 C19 123.5(5) . . ? N7 C20 C19 123.1(5) . . ? C26 C21 C22 119.8(5) . . ? C26 C21 N6 109.9(5) . . ? C22 C21 N6 130.3(5) . . ? C23 C22 C21 117.9(6) . . ? C23 C22 H22A 121.0 . . ? C21 C22 H22A 121.0 . . ? C22 C23 C24 121.1(6) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C25 C24 C23 121.7(6) . . ? C25 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? C24 C25 C26 116.4(6) . . ? C24 C25 H25A 121.8 . . ? C26 C25 H25A 121.8 . . ? C25 C26 C21 123.1(6) . . ? C25 C26 N7 131.7(5) . . ? C21 C26 N7 105.2(5) . . ? N7 C27 H27A 109.5 . . ? N7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N8 108.7(4) . . ? C29 C28 H28A 110.0 . . ? N8 C28 H28A 110.0 . . ? C29 C28 H28B 110.0 . . ? N8 C28 H28B 110.0 . . ? H28A C28 H28B 108.3 . . ? N9 C29 N10 113.3(5) . . ? N9 C29 C28 122.8(5) . . ? N10 C29 C28 123.7(5) . . ? C31 C30 C35 120.6(5) . . ? C31 C30 N9 130.4(5) . . ? C35 C30 N9 108.9(5) . . ? C32 C31 C30 117.0(5) . . ? C32 C31 H31A 121.5 . . ? C30 C31 H31A 121.5 . . ? C31 C32 C33 121.4(6) . . ? C31 C32 H32A 119.3 . . ? C33 C32 H32A 119.3 . . ? C34 C33 C32 121.8(5) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? C33 C34 C35 117.5(5) . . ? C33 C34 H34A 121.2 . . ? C35 C34 H34A 121.2 . . ? C34 C35 N10 132.7(5) . . ? C34 C35 C30 121.5(5) . . ? N10 C35 C30 105.7(4) . . ? N10 C36 H36A 109.5 . . ? N10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N8 108.7(4) . . ? C38 C37 H37A 110.0 . . ? N8 C37 H37A 110.0 . . ? C38 C37 H37B 110.0 . . ? N8 C37 H37B 110.0 . . ? H37A C37 H37B 108.3 . . ? N11 C38 N12 113.1(5) . . ? N11 C38 C37 123.0(5) . . ? N12 C38 C37 123.8(5) . . ? N11 C39 C40 132.0(5) . . ? N11 C39 C44 108.7(4) . . ? C40 C39 C44 119.3(5) . . ? C41 C40 C39 118.4(6) . . ? C41 C40 H40A 120.8 . . ? C39 C40 H40A 120.8 . . ? C40 C41 C42 121.6(6) . . ? C40 C41 H41A 119.2 . . ? C42 C41 H41A 119.2 . . ? C43 C42 C41 121.8(6) . . ? C43 C42 H42A 119.1 . . ? C41 C42 H42A 119.1 . . ? C42 C43 C44 116.2(6) . . ? C42 C43 H43A 121.9 . . ? C44 C43 H43A 121.9 . . ? N12 C44 C43 131.0(6) . . ? N12 C44 C39 106.3(5) . . ? C43 C44 C39 122.7(5) . . ? N12 C45 H45A 109.5 . . ? N12 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N12 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N8 C46 C47 108.6(4) . . ? N8 C46 H46A 110.0 . . ? C47 C46 H46A 110.0 . . ? N8 C46 H46B 110.0 . . ? C47 C46 H46B 110.0 . . ? H46A C46 H46B 108.4 . . ? N13 C47 N14 114.5(5) . . ? N13 C47 C46 122.3(5) . . ? N14 C47 C46 123.0(5) . . ? C49 C48 C53 120.6(5) . . ? C49 C48 N13 130.4(5) . . ? C53 C48 N13 109.0(5) . . ? C48 C49 C50 117.0(5) . . ? C48 C49 H49A 121.5 . . ? C50 C49 H49A 121.5 . . ? C49 C50 C51 121.9(6) . . ? C49 C50 H50A 119.1 . . ? C51 C50 H50A 119.1 . . ? C52 C51 C50 121.4(6) . . ? C52 C51 H51A 119.3 . . ? C50 C51 H51A 119.3 . . ? C51 C52 C53 116.7(6) . . ? C51 C52 H52A 121.7 . . ? C53 C52 H52A 121.7 . . ? C52 C53 N14 131.6(5) . . ? C52 C53 C48 122.4(6) . . ? N14 C53 C48 106.0(5) . . ? N14 C54 H54A 109.5 . . ? N14 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N14 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? F6 C56 F5 106.6(7) . . ? F6 C56 F4 107.4(6) . . ? F5 C56 F4 108.8(6) . . ? F6 C56 S2 112.4(5) . . ? F5 C56 S2 112.2(5) . . ? F4 C56 S2 109.3(5) . . ? O4 S2 O6 114.8(3) . . ? O4 S2 O5 114.5(3) . . ? O6 S2 O5 114.1(3) . . ? O4 S2 C56 104.1(3) . . ? O6 S2 C56 104.2(3) . . ? O5 S2 C56 103.1(3) . . ? O1 S1 O2 120.0(11) . . ? O1 S1 O3 110.8(6) . . ? O2 S1 O3 110.9(8) . . ? O1 S1 C55 113.9(5) . . ? O2 S1 C55 102.4(10) . . ? O3 S1 C55 95.9(6) . . ? F3 C55 F1 115.6(13) . . ? F3 C55 F2 103.1(12) . . ? F1 C55 F2 105.6(10) . . ? F3 C55 S1 116.9(8) . . ? F1 C55 S1 109.3(10) . . ? F2 C55 S1 105.0(8) . . ? O9 S3 O7 114.5(7) . . ? O9 S3 O8 120.8(7) . . ? O7 S3 O8 108.6(6) . . ? O9 S3 C57 109.5(8) . . ? O7 S3 C57 107.1(6) . . ? O8 S3 C57 93.8(5) . . ? F9 C57 F8 109.9(15) . . ? F9 C57 F7 104.4(14) . . ? F8 C57 F7 99.8(10) . . ? F9 C57 S3 123.5(14) . . ? F8 C57 S3 114.8(9) . . ? F7 C57 S3 100.3(8) . . ? C58 O1W H1WA 109.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O1W C58 C59 139.4(14) . . ? O1W C58 H58A 102.2 . . ? C59 C58 H58A 102.2 . . ? O1W C58 H58B 102.2 . . ? C59 C58 H58B 102.2 . . ? H58A C58 H58B 104.8 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 61.85 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.364 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.085 #===================================# data_9 _database_code_depnum_ccdc_archive 'CCDC 698713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H51 Eu N18 O21' _chemical_formula_weight 1452.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 14.0075(2) _cell_length_b 21.1128(3) _cell_length_c 21.0118(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.525(2) _cell_angle_gamma 90.00 _cell_volume 5957.31(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18471 _cell_measurement_theta_min 2.7843 _cell_measurement_theta_max 29.6794 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5975 _exptl_absorpt_correction_T_max 0.6894 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type Gemini _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40752 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14242 _reflns_number_gt 9845 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14242 _refine_ls_number_parameters 807 _refine_ls_number_restraints 922 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 Eu1 Eu 0.306435(9) 0.323427(6) 0.088249(6) 0.02079(3) Uani 1 1 d . . . N1 N 0.25395(15) 0.39612(10) 0.18124(10) 0.0239(5) Uani 1 1 d U C . N2 N 0.44448(15) 0.38293(10) 0.17533(10) 0.0266(5) Uani 1 1 d U C . N3 N 0.51495(18) 0.41383(13) 0.27905(11) 0.0386(7) Uani 1 1 d U . . N4 N 0.18284(16) 0.41728(10) 0.04982(10) 0.0266(5) Uani 1 1 d U . . N5 N 0.15973(16) 0.52139(10) 0.05679(11) 0.0287(5) Uani 1 1 d U C . N6 N 0.20773(15) 0.26998(10) 0.16037(10) 0.0254(5) Uani 1 1 d U . . N7 N 0.08527(15) 0.27154(10) 0.20941(11) 0.0279(5) Uani 1 1 d U . . N8 N 0.05918(19) 0.24667(13) 0.00079(13) 0.0465(7) Uani 1 1 d U . . N9 N 0.0313(2) 0.07260(13) -0.15357(14) 0.0554(8) Uani 1 1 d U . . N10 N 0.35656(19) 0.11980(13) -0.00103(15) 0.0509(7) Uani 1 1 d U . . N11 N 0.49475(17) 0.23663(12) 0.20949(12) 0.0380(6) Uani 1 1 d U B . N14 N 0.24830(17) 0.26570(11) -0.14404(10) 0.0311(6) Uani 1 1 d U . . N15 N 0.38492(16) 0.45118(11) -0.00544(11) 0.0296(6) Uani 1 1 d U . . N16 N 0.46091(16) 0.41723(11) -0.21357(11) 0.0307(6) Uani 1 1 d U . . C1 C 0.33174(19) 0.38740(14) 0.24546(13) 0.0299(6) Uani 1 1 d U . . H1A H 0.3237 0.4196 0.2778 0.036 Uiso 1 1 calc R C . H1B H 0.3255 0.3449 0.2637 0.036 Uiso 1 1 calc R . . C2 C 0.43094(19) 0.39417(13) 0.23384(12) 0.0270(6) Uani 1 1 d U C . C3 C 0.54449(19) 0.39722(12) 0.18283(12) 0.0251(6) Uani 1 1 d U . . C4 C 0.59980(19) 0.39665(13) 0.13629(14) 0.0310(7) Uani 1 1 d U C . H4A H 0.5717 0.3819 0.0922 0.037 Uiso 1 1 calc R . . C5 C 0.6965(2) 0.41842(14) 0.15762(15) 0.0363(7) Uani 1 1 d U . . H5A H 0.7353 0.4194 0.1272 0.044 Uiso 1 1 calc R C . C6 C 0.7385(2) 0.43875(16) 0.22196(16) 0.0428(8) Uani 1 1 d U C . H6A H 0.8054 0.4535 0.2347 0.051 Uiso 1 1 calc R . . C7 C 0.6859(2) 0.43823(18) 0.26811(16) 0.0480(9) Uani 1 1 d U . . H7A H 0.7152 0.4517 0.3125 0.058 Uiso 1 1 calc R C . C8 C 0.5880(2) 0.41724(15) 0.24694(14) 0.0360(7) Uani 1 1 d U C . C12 C 0.2488(2) 0.46347(12) 0.16104(13) 0.0281(6) Uani 1 1 d U . . H12A H 0.3168 0.4811 0.1699 0.034 Uiso 1 1 calc R C . H12B H 0.2124 0.4883 0.1867 0.034 Uiso 1 1 calc R . . C13 C 0.19616(19) 0.46726(12) 0.08889(13) 0.0266(6) Uani 1 1 d U C . C14 C 0.13320(19) 0.44050(13) -0.01390(13) 0.0280(6) Uani 1 1 d U . . C15 C 0.09975(19) 0.40923(14) -0.07420(14) 0.0320(7) Uani 1 1 d U . . H15A H 0.1073 0.3647 -0.0774 0.038 Uiso 1 1 calc R . . C16 C 0.0551(2) 0.44525(14) -0.12949(15) 0.0372(7) Uani 1 1 d U . . H16A H 0.0309 0.4253 -0.1715 0.045 Uiso 1 1 calc R . . C17 C 0.0450(2) 0.51105(16) -0.12431(15) 0.0433(8) Uani 1 1 d U . . H17A H 0.0161 0.5348 -0.1635 0.052 Uiso 1 1 calc R . . C18 C 0.0752(2) 0.54213(14) -0.06520(14) 0.0388(7) Uani 1 1 d U . . H18A H 0.0654 0.5864 -0.0621 0.047 Uiso 1 1 calc R . . C19 C 0.12092(19) 0.50603(13) -0.00951(14) 0.0308(6) Uani 1 1 d U . . C20 C 0.1654(2) 0.58523(14) 0.08489(17) 0.0470(8) Uani 1 1 d U . . H20A H 0.1501 0.5834 0.1280 0.056 Uiso 1 1 calc R A 1 H20B H 0.1150 0.6126 0.0547 0.056 Uiso 1 1 calc R A 1 C23 C 0.15667(18) 0.37501(13) 0.18730(13) 0.0270(6) Uani 1 1 d U . . H23A H 0.1028 0.3927 0.1502 0.032 Uiso 1 1 calc R C . H23B H 0.1474 0.3910 0.2294 0.032 Uiso 1 1 calc R . . C24 C 0.15032(18) 0.30493(13) 0.18604(12) 0.0248(6) Uani 1 1 d U C . C25 C 0.17906(19) 0.20723(13) 0.16861(13) 0.0277(6) Uani 1 1 d U . . C26 C 0.2175(2) 0.14980(14) 0.15466(14) 0.0362(7) Uani 1 1 d U . . H26A H 0.2701 0.1482 0.1345 0.043 Uiso 1 1 calc R . . C27 C 0.1760(3) 0.09524(14) 0.17131(17) 0.0477(9) Uani 1 1 d U . . H27A H 0.2008 0.0554 0.1622 0.057 Uiso 1 1 calc R . . C28 C 0.0978(3) 0.09690(15) 0.20147(17) 0.0506(9) Uani 1 1 d U . . H28A H 0.0701 0.0584 0.2114 0.061 Uiso 1 1 calc R . . C29 C 0.0608(2) 0.15469(16) 0.21682(16) 0.0453(8) Uani 1 1 d U . . H29A H 0.0095 0.1569 0.2381 0.054 Uiso 1 1 calc R . . C30 C 0.1028(2) 0.20742(13) 0.19936(13) 0.0307(7) Uani 1 1 d U . . C31 C 0.0111(2) 0.29547(16) 0.24005(14) 0.0381(7) Uani 1 1 d U . . H31A H 0.0400 0.3319 0.2688 0.046 Uiso 1 1 calc R . . H31B H -0.0036 0.2619 0.2688 0.046 Uiso 1 1 calc R . . C32 C -0.0827(3) 0.3157(2) 0.1926(2) 0.0723(12) Uani 1 1 d U . . H32A H -0.1294 0.3271 0.2185 0.087 Uiso 1 1 calc R . . H32B H -0.0690 0.3550 0.1710 0.087 Uiso 1 1 calc R . . C33 C -0.1334(4) 0.2731(3) 0.1415(3) 0.0991(15) Uiso 1 1 d U . . H33A H -0.1924 0.2940 0.1126 0.149 Uiso 1 1 calc R . . H33B H -0.1540 0.2354 0.1614 0.149 Uiso 1 1 calc R . . H33C H -0.0888 0.2606 0.1153 0.149 Uiso 1 1 calc R . . C34 C 0.2150(2) 0.18756(12) 0.00247(13) 0.0288(6) Uani 1 1 d U . . C35 C 0.1088(2) 0.19522(14) -0.02307(14) 0.0336(7) Uani 1 1 d U . . C36 C 0.0493(2) 0.15671(15) -0.07158(15) 0.0412(8) Uani 1 1 d U . . H36A H -0.0209 0.1623 -0.0855 0.049 Uiso 1 1 calc R . . C37 C 0.0927(2) 0.11053(14) -0.09921(14) 0.0389(8) Uani 1 1 d U . . C38 C 0.1937(2) 0.09930(14) -0.07742(13) 0.0369(8) Uani 1 1 d U . . H38A H 0.2229 0.0670 -0.0973 0.044 Uiso 1 1 calc R . . C39 C 0.2509(2) 0.13510(13) -0.02702(13) 0.0324(7) Uani 1 1 d U . . C46 C 0.32053(17) 0.35375(12) -0.06809(12) 0.0217(6) Uani 1 1 d U . . C47 C 0.37616(18) 0.41155(12) -0.06230(12) 0.0232(6) Uani 1 1 d U . . C48 C 0.42016(19) 0.43258(13) -0.10910(13) 0.0273(6) Uani 1 1 d U . . H48A H 0.4563 0.4713 -0.1029 0.033 Uiso 1 1 calc R . . C49 C 0.41086(19) 0.39651(12) -0.16532(12) 0.0270(6) Uani 1 1 d U . . C50 C 0.35494(19) 0.34123(13) -0.17699(13) 0.0265(6) Uani 1 1 d U . . H50A H 0.3485 0.3169 -0.2160 0.032 Uiso 1 1 calc R . . C51 C 0.30972(18) 0.32303(11) -0.13080(12) 0.0223(6) Uani 1 1 d U . . O1 O 0.27117(14) 0.22152(9) 0.04642(9) 0.0311(5) Uani 1 1 d U . . O2 O 0.10521(16) 0.29318(10) 0.02636(10) 0.0422(6) Uani 1 1 d U . . O3 O -0.03085(19) 0.24092(14) -0.00596(16) 0.0831(10) Uani 1 1 d U . . O4 O -0.0585(2) 0.07724(14) -0.16512(15) 0.0839(10) Uani 1 1 d U . . O5 O 0.0732(2) 0.03872(12) -0.18452(12) 0.0679(8) Uani 1 1 d U . . O6 O 0.4013(2) 0.10426(16) -0.04109(16) 0.0897(10) Uani 1 1 d U . . O7 O 0.39438(17) 0.11907(12) 0.05829(14) 0.0654(8) Uani 1 1 d U . . O8 O 0.45804(13) 0.28527(8) 0.07776(9) 0.0278(5) Uani 1 1 d U . . O9 O 0.40700(13) 0.25230(9) 0.18868(9) 0.0302(5) Uani 1 1 d U . . O10 O 0.53717(18) 0.23614(14) 0.26927(11) 0.0616(8) Uani 1 1 d U . . O15 O 0.28298(12) 0.33142(8) -0.02514(8) 0.0225(4) Uani 1 1 d U . . O16 O 0.38400(14) 0.42752(9) 0.04833(9) 0.0332(5) Uani 1 1 d U . . O17 O 0.39554(17) 0.50864(10) -0.01110(10) 0.0453(6) Uani 1 1 d U . . O18 O 0.52083(15) 0.46064(10) -0.19780(10) 0.0417(5) Uani 1 1 d U . . O19 O 0.44032(17) 0.39088(10) -0.26719(10) 0.0488(6) Uani 1 1 d DU . . O20 O 0.27946(17) 0.22010(9) -0.16692(11) 0.0461(6) Uani 1 1 d U . . O21 O 0.16718(15) 0.26692(10) -0.13299(10) 0.0432(6) Uani 1 1 d U . . C40 C 0.52153(19) 0.24249(14) 0.09783(14) 0.0314(7) Uani 1 1 d U B . C41 C 0.5462(2) 0.21599(15) 0.16335(15) 0.0394(8) Uani 1 1 d U . . C45 C 0.5795(2) 0.21606(17) 0.05848(16) 0.0495(8) Uani 1 1 d U . . N13 N 0.5641(2) 0.23634(15) -0.01011(14) 0.0611(8) Uani 1 1 d U B . C42 C 0.6279(4) 0.1815(2) 0.1955(3) 0.0295(12) Uiso 0.50 1 d P B 1 H42A H 0.6450 0.1731 0.2418 0.035 Uiso 0.50 1 calc PR B 1 C43 C 0.6848(5) 0.1595(3) 0.1550(3) 0.0407(15) Uiso 0.50 1 d P B 1 C44 C 0.6680(5) 0.1814(3) 0.0917(3) 0.0373(14) Uiso 0.50 1 d P B 1 H44A H 0.7163 0.1736 0.0688 0.045 Uiso 0.50 1 calc PR B 1 N12 N 0.7650(4) 0.1145(3) 0.1828(3) 0.0538(15) Uiso 0.50 1 d P B 1 O11 O 0.7710(4) 0.0921(2) 0.2367(3) 0.0623(14) Uiso 0.50 1 d P B 1 O12 O 0.8120(5) 0.0966(3) 0.1449(3) 0.0864(19) Uiso 0.50 1 d P B 1 O13 O 0.6357(3) 0.2266(2) -0.0326(2) 0.0628(12) Uiso 0.60 1 d P B 1 O14 O 0.4840(3) 0.2534(2) -0.0415(2) 0.0607(11) Uiso 0.60 1 d P B 1 C42' C 0.6048(4) 0.1565(3) 0.1754(3) 0.0375(14) Uiso 0.50 1 d P B 2 H42' H 0.6154 0.1363 0.2172 0.045 Uiso 0.50 1 calc PR B 2 C43' C 0.6438(4) 0.1298(3) 0.1304(3) 0.0366(13) Uiso 0.50 1 d P B 2 C44' C 0.6309(4) 0.1565(3) 0.0682(3) 0.0395(14) Uiso 0.50 1 d P B 2 H44B H 0.6542 0.1369 0.0348 0.047 Uiso 0.50 1 calc PR B 2 N12' N 0.7003(5) 0.0717(3) 0.1473(3) 0.0678(18) Uiso 0.50 1 d P B 2 O11' O 0.7147(4) 0.0477(3) 0.2027(3) 0.0709(15) Uiso 0.50 1 d P B 2 O12' O 0.7372(5) 0.0495(3) 0.1068(3) 0.093(2) Uiso 0.50 1 d P B 2 O13' O 0.5988(5) 0.2118(3) -0.0500(3) 0.0569(17) Uiso 0.40 1 d P B 2 O14' O 0.5344(6) 0.2940(5) -0.0219(4) 0.096(3) Uiso 0.40 1 d P B 2 N17 N 0.8699(5) 0.2946(3) -0.1845(3) 0.162(2) Uiso 1 1 d . . . C52 C 0.8226(4) 0.2553(3) -0.1681(3) 0.1024(18) Uiso 1 1 d . . . C53 C 0.7619(4) 0.2101(3) -0.1449(3) 0.0931(16) Uiso 1 1 d . . . H53A H 0.7473 0.1737 -0.1750 0.140 Uiso 1 1 calc R . . H53B H 0.6994 0.2304 -0.1439 0.140 Uiso 1 1 calc R . . H53C H 0.7979 0.1959 -0.1001 0.140 Uiso 1 1 calc R . . N18 N 0.8146(6) 0.0607(7) -0.0362(6) 0.346 Uiso 1 1 d D . . C54 C 0.8874(8) 0.0463(6) -0.0141(6) 0.274(6) Uiso 1 1 d D . . C55 C 0.9357(6) 0.0768(4) 0.0431(4) 0.189(4) Uiso 1 1 d D . . H55A H 0.9873 0.0490 0.0704 0.283 Uiso 1 1 calc R . . H55B H 0.8881 0.0878 0.0675 0.283 Uiso 1 1 calc R . . H55C H 0.9667 0.1154 0.0324 0.283 Uiso 1 1 calc R . . C9 C 0.5280(4) 0.4122(2) 0.3532(3) 0.0262(11) Uiso 0.50 1 d P C 1 H9A H 0.5896 0.3888 0.3759 0.031 Uiso 0.50 1 calc PR C 1 H9B H 0.4709 0.3901 0.3622 0.031 Uiso 0.50 1 calc PR C 1 C10 C 0.5344(4) 0.4803(3) 0.3794(3) 0.0349(13) Uiso 0.50 1 d P C 1 H10A H 0.5562 0.4791 0.4285 0.042 Uiso 0.50 1 calc PR C 1 H10B H 0.5861 0.5031 0.3647 0.042 Uiso 0.50 1 calc PR C 1 C11 C 0.4429(4) 0.5156(3) 0.3583(3) 0.0367(14) Uiso 0.50 1 d P C 1 H11A H 0.4540 0.5587 0.3760 0.055 Uiso 0.50 1 calc PR C 1 H11B H 0.3921 0.4949 0.3748 0.055 Uiso 0.50 1 calc PR C 1 H11C H 0.4203 0.5171 0.3097 0.055 Uiso 0.50 1 calc PR C 1 C9' C 0.5256(5) 0.4540(3) 0.3452(3) 0.0450(16) Uiso 0.50 1 d P C 2 H9'A H 0.5606 0.4944 0.3434 0.054 Uiso 0.50 1 calc PR C 2 H9'B H 0.4592 0.4636 0.3506 0.054 Uiso 0.50 1 calc PR C 2 C10' C 0.5830(6) 0.4149(4) 0.3999(4) 0.064(2) Uiso 0.50 1 d P C 2 H10C H 0.6464 0.4019 0.3918 0.077 Uiso 0.50 1 calc PR C 2 H10D H 0.5450 0.3762 0.4037 0.077 Uiso 0.50 1 calc PR C 2 C11' C 0.6038(6) 0.4531(4) 0.4632(4) 0.075(2) Uiso 0.50 1 d P C 2 H11D H 0.6440 0.4278 0.5003 0.112 Uiso 0.50 1 calc PR C 2 H11E H 0.5407 0.4645 0.4717 0.112 Uiso 0.50 1 calc PR C 2 H11F H 0.6401 0.4917 0.4587 0.112 Uiso 0.50 1 calc PR C 2 C21 C 0.2713(4) 0.6146(3) 0.0952(3) 0.0424(12) Uiso 0.60 1 d P D 1 H21A H 0.2786 0.6521 0.1246 0.051 Uiso 0.60 1 calc PR D 1 H21B H 0.3224 0.5832 0.1175 0.051 Uiso 0.60 1 calc PR D 1 C22 C 0.2894(5) 0.6347(4) 0.0289(4) 0.075(2) Uiso 0.60 1 d P D 1 H22A H 0.3569 0.6519 0.0374 0.112 Uiso 0.60 1 calc PR D 1 H22B H 0.2408 0.6672 0.0075 0.112 Uiso 0.60 1 calc PR D 1 H22C H 0.2820 0.5978 -0.0004 0.112 Uiso 0.60 1 calc PR D 1 C21' C 0.2319(7) 0.6286(5) 0.0599(5) 0.058(2) Uiso 0.40 1 d P D 2 H21C H 0.2220 0.6210 0.0119 0.069 Uiso 0.40 1 calc PR D 2 H21D H 0.2146 0.6732 0.0658 0.069 Uiso 0.40 1 calc PR D 2 C22' C 0.3267(9) 0.6180(7) 0.0931(6) 0.089(4) Uiso 0.40 1 d P D 2 H22D H 0.3697 0.6462 0.0765 0.134 Uiso 0.40 1 calc PR D 2 H22E H 0.3437 0.5738 0.0869 0.134 Uiso 0.40 1 calc PR D 2 H22F H 0.3364 0.6261 0.1405 0.134 Uiso 0.40 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02519(6) 0.01896(6) 0.01822(5) -0.00064(5) 0.00619(4) -0.00033(5) N1 0.0304(10) 0.0231(10) 0.0184(9) -0.0004(8) 0.0070(8) -0.0018(8) N2 0.0318(10) 0.0248(11) 0.0222(10) -0.0022(9) 0.0060(8) -0.0044(9) N3 0.0366(12) 0.0552(15) 0.0201(11) -0.0041(11) 0.0017(9) -0.0029(11) N4 0.0337(10) 0.0204(10) 0.0251(10) -0.0013(9) 0.0073(9) 0.0030(9) N5 0.0370(10) 0.0198(10) 0.0326(11) -0.0024(9) 0.0150(9) 0.0008(9) N6 0.0288(10) 0.0218(10) 0.0256(10) 0.0024(9) 0.0079(8) -0.0004(8) N7 0.0277(10) 0.0294(11) 0.0283(10) 0.0051(9) 0.0108(8) 0.0028(9) N8 0.0427(13) 0.0453(14) 0.0453(14) -0.0051(13) 0.0024(11) 0.0034(12) N9 0.0745(17) 0.0336(13) 0.0436(15) -0.0033(12) -0.0066(14) -0.0131(13) N10 0.0428(13) 0.0477(15) 0.0669(16) -0.0171(13) 0.0231(12) -0.0079(12) N11 0.0323(11) 0.0451(13) 0.0336(12) 0.0106(11) 0.0045(10) 0.0031(10) N14 0.0456(12) 0.0297(11) 0.0208(10) -0.0050(9) 0.0138(9) -0.0139(10) N15 0.0367(11) 0.0267(11) 0.0248(10) -0.0030(9) 0.0080(9) -0.0047(9) N16 0.0394(11) 0.0284(11) 0.0285(10) 0.0004(9) 0.0164(9) -0.0031(9) C1 0.0332(12) 0.0346(14) 0.0232(12) -0.0007(11) 0.0100(10) 0.0003(11) C2 0.0326(12) 0.0283(13) 0.0186(11) 0.0013(10) 0.0048(10) 0.0009(10) C3 0.0281(11) 0.0214(12) 0.0249(11) -0.0002(10) 0.0060(10) -0.0058(10) C4 0.0328(12) 0.0306(14) 0.0306(13) -0.0026(11) 0.0106(11) -0.0063(11) C5 0.0295(12) 0.0386(15) 0.0418(15) 0.0052(13) 0.0117(11) -0.0012(12) C6 0.0276(13) 0.0511(17) 0.0476(16) -0.0036(15) 0.0073(12) -0.0051(13) C7 0.0336(14) 0.068(2) 0.0381(15) -0.0118(15) 0.0027(13) -0.0098(14) C8 0.0351(13) 0.0458(16) 0.0271(13) 0.0002(12) 0.0091(11) 0.0007(12) C12 0.0378(13) 0.0195(12) 0.0278(12) -0.0065(10) 0.0107(10) -0.0004(10) C13 0.0324(11) 0.0214(12) 0.0289(12) 0.0001(10) 0.0133(10) 0.0034(10) C14 0.0297(11) 0.0235(12) 0.0326(12) 0.0043(11) 0.0119(10) 0.0047(10) C15 0.0327(12) 0.0316(14) 0.0316(13) -0.0022(12) 0.0088(11) 0.0113(11) C16 0.0375(13) 0.0417(15) 0.0308(13) 0.0015(13) 0.0071(11) 0.0154(12) C17 0.0461(15) 0.0524(18) 0.0336(14) 0.0145(13) 0.0148(12) 0.0168(14) C18 0.0456(14) 0.0340(15) 0.0397(14) 0.0123(12) 0.0168(12) 0.0190(12) C19 0.0299(12) 0.0303(13) 0.0348(13) 0.0011(11) 0.0134(10) 0.0034(11) C20 0.0678(17) 0.0275(15) 0.0568(17) -0.0041(14) 0.0358(14) 0.0010(14) C23 0.0301(11) 0.0313(13) 0.0215(11) -0.0016(10) 0.0107(9) -0.0020(10) C24 0.0266(11) 0.0288(12) 0.0199(11) 0.0063(10) 0.0082(9) 0.0023(10) C25 0.0320(12) 0.0268(13) 0.0244(12) 0.0066(11) 0.0082(10) 0.0030(11) C26 0.0506(15) 0.0287(14) 0.0314(13) 0.0032(12) 0.0153(12) 0.0011(13) C27 0.0712(18) 0.0221(14) 0.0540(17) 0.0078(14) 0.0244(15) 0.0038(14) C28 0.0705(18) 0.0294(15) 0.0576(17) 0.0086(14) 0.0275(15) -0.0073(14) C29 0.0447(14) 0.0462(16) 0.0529(16) 0.0246(14) 0.0267(12) 0.0085(13) C30 0.0339(12) 0.0299(13) 0.0272(12) 0.0063(11) 0.0071(10) 0.0006(11) C31 0.0374(13) 0.0454(16) 0.0382(14) 0.0017(13) 0.0217(11) 0.0042(13) C32 0.0586(19) 0.096(3) 0.067(2) 0.007(2) 0.0252(17) 0.0236(19) C34 0.0393(13) 0.0237(13) 0.0228(12) 0.0045(10) 0.0082(10) -0.0064(11) C35 0.0451(14) 0.0240(12) 0.0284(13) -0.0013(11) 0.0048(12) 0.0027(12) C36 0.0450(15) 0.0322(14) 0.0363(15) 0.0018(13) -0.0047(13) -0.0044(13) C37 0.0552(16) 0.0266(14) 0.0279(13) -0.0012(12) 0.0004(12) -0.0085(13) C38 0.0570(16) 0.0248(13) 0.0305(14) -0.0019(11) 0.0150(12) -0.0080(12) C39 0.0418(13) 0.0258(13) 0.0322(13) -0.0036(11) 0.0150(11) -0.0103(11) C46 0.0245(10) 0.0208(12) 0.0200(11) 0.0013(10) 0.0065(9) 0.0004(9) C47 0.0290(11) 0.0213(12) 0.0181(11) -0.0016(10) 0.0049(9) -0.0016(10) C48 0.0315(12) 0.0239(12) 0.0274(12) -0.0011(11) 0.0099(10) -0.0062(10) C49 0.0331(12) 0.0275(13) 0.0228(11) 0.0031(10) 0.0117(10) 0.0014(11) C50 0.0326(12) 0.0270(13) 0.0195(11) -0.0040(10) 0.0066(10) -0.0018(10) C51 0.0268(11) 0.0186(11) 0.0223(11) -0.0021(10) 0.0084(9) -0.0016(9) O1 0.0422(10) 0.0253(9) 0.0233(9) -0.0004(8) 0.0054(8) -0.0090(8) O2 0.0591(12) 0.0250(10) 0.0387(11) -0.0014(9) 0.0077(10) 0.0008(10) O3 0.0473(14) 0.0830(18) 0.111(2) -0.0318(17) 0.0097(15) 0.0100(14) O4 0.0701(16) 0.0733(17) 0.0814(19) -0.0242(16) -0.0220(15) -0.0120(15) O5 0.1031(19) 0.0476(14) 0.0427(13) -0.0164(12) 0.0042(13) -0.0104(14) O6 0.0746(16) 0.100(2) 0.110(2) -0.0246(18) 0.0528(15) 0.0020(16) O7 0.0465(13) 0.0626(15) 0.0742(16) -0.0272(14) -0.0036(12) 0.0116(12) O8 0.0297(8) 0.0264(9) 0.0261(9) -0.0024(8) 0.0061(7) -0.0014(8) O9 0.0319(9) 0.0298(10) 0.0289(9) 0.0036(8) 0.0086(7) 0.0040(8) O10 0.0520(13) 0.0945(18) 0.0281(11) 0.0111(12) -0.0051(10) -0.0040(13) O15 0.0253(8) 0.0228(9) 0.0203(8) -0.0001(7) 0.0079(7) -0.0005(7) O16 0.0430(10) 0.0338(10) 0.0233(9) -0.0029(8) 0.0104(8) -0.0070(8) O17 0.0763(13) 0.0312(11) 0.0334(10) -0.0081(9) 0.0236(10) -0.0109(10) O18 0.0498(11) 0.0412(12) 0.0383(10) -0.0011(9) 0.0191(9) -0.0181(9) O19 0.0760(13) 0.0479(13) 0.0343(10) -0.0133(10) 0.0349(9) -0.0208(11) O20 0.0681(13) 0.0260(10) 0.0505(11) -0.0140(9) 0.0272(10) -0.0072(10) O21 0.0489(11) 0.0465(12) 0.0376(10) -0.0120(10) 0.0176(9) -0.0224(10) C40 0.0268(11) 0.0348(14) 0.0323(13) 0.0074(12) 0.0080(10) 0.0027(11) C41 0.0289(12) 0.0499(17) 0.0420(14) 0.0183(13) 0.0145(11) 0.0110(12) C45 0.0499(15) 0.0554(18) 0.0533(16) 0.0183(15) 0.0313(13) 0.0229(14) N13 0.0627(14) 0.0743(19) 0.0639(15) 0.0243(14) 0.0466(12) 0.0350(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O15 2.3167(17) . ? Eu1 O1 2.3235(18) . ? Eu1 O8 2.3395(18) . ? Eu1 N2 2.579(2) . ? Eu1 N6 2.583(2) . ? Eu1 N4 2.604(2) . ? Eu1 O9 2.6461(17) . ? Eu1 O16 2.689(2) . ? Eu1 N1 2.744(2) . ? Eu1 O2 2.821(2) . ? N1 C23 1.473(3) . ? N1 C12 1.480(3) . ? N1 C1 1.485(3) . ? N2 C2 1.318(3) . ? N2 C3 1.397(3) . ? N3 C2 1.350(3) . ? N3 C8 1.379(4) . ? N3 C9 1.517(6) . ? N3 C9' 1.598(7) . ? N4 C13 1.317(3) . ? N4 C14 1.409(3) . ? N5 C13 1.351(3) . ? N5 C19 1.382(3) . ? N5 C20 1.464(4) . ? N6 C24 1.315(3) . ? N6 C25 1.409(3) . ? N7 C24 1.350(3) . ? N7 C30 1.403(4) . ? N7 C31 1.459(4) . ? N8 O2 1.213(3) . ? N8 O3 1.234(4) . ? N8 C35 1.453(4) . ? N9 O4 1.216(4) . ? N9 O5 1.223(4) . ? N9 C37 1.459(4) . ? N10 O7 1.208(4) . ? N10 O6 1.229(4) . ? N10 C39 1.461(4) . ? N11 O9 1.227(3) . ? N11 O10 1.227(3) . ? N11 C41 1.431(4) . ? N14 O20 1.212(3) . ? N14 O21 1.223(3) . ? N14 C51 1.465(3) . ? N15 O17 1.232(3) . ? N15 O16 1.239(3) . ? N15 C47 1.435(3) . ? N16 O19 1.215(3) . ? N16 O18 1.223(3) . ? N16 C49 1.454(4) . ? C1 C2 1.485(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C8 1.378(4) . ? C3 C4 1.410(4) . ? C4 C5 1.379(4) . ? C4 H4A 0.9500 . ? C5 C6 1.380(4) . ? C5 H5A 0.9500 . ? C6 C7 1.375(5) . ? C6 H6A 0.9500 . ? C7 C8 1.388(4) . ? C7 H7A 0.9500 . ? C12 C13 1.488(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.387(4) . ? C14 C19 1.400(4) . ? C15 C16 1.380(4) . ? C15 H15A 0.9500 . ? C16 C17 1.404(4) . ? C16 H16A 0.9500 . ? C17 C18 1.361(4) . ? C17 H17A 0.9500 . ? C18 C19 1.391(4) . ? C18 H18A 0.9500 . ? C20 C21' 1.503(10) . ? C20 C21 1.566(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C23 C24 1.482(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.391(4) . ? C25 C30 1.396(4) . ? C26 C27 1.379(4) . ? C26 H26A 0.9500 . ? C27 C28 1.414(5) . ? C27 H27A 0.9500 . ? C28 C29 1.399(5) . ? C28 H28A 0.9500 . ? C29 C30 1.358(4) . ? C29 H29A 0.9500 . ? C31 C32 1.469(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.426(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O1 1.254(3) . ? C34 C39 1.428(4) . ? C34 C35 1.440(4) . ? C35 C36 1.383(4) . ? C36 C37 1.363(5) . ? C36 H36A 0.9500 . ? C37 C38 1.377(4) . ? C38 C39 1.361(4) . ? C38 H38A 0.9500 . ? C46 O15 1.258(3) . ? C46 C47 1.434(3) . ? C46 C51 1.437(3) . ? C47 C48 1.374(4) . ? C48 C49 1.380(4) . ? C48 H48A 0.9500 . ? C49 C50 1.388(4) . ? C50 C51 1.357(4) . ? C50 H50A 0.9500 . ? O8 C40 1.254(3) . ? C40 C45 1.427(4) . ? C40 C41 1.434(4) . ? C41 C42 1.363(6) . ? C41 C42' 1.481(7) . ? C45 C44' 1.434(7) . ? C45 C44 1.437(6) . ? C45 N13 1.459(4) . ? N13 O14 1.184(5) . ? N13 O13' 1.200(7) . ? N13 O13 1.242(6) . ? N13 O14' 1.287(10) . ? C42 C43 1.401(9) . ? C42 H42A 0.9500 . ? C43 C44 1.363(9) . ? C43 N12 1.462(8) . ? C44 H44A 0.9500 . ? N12 O11 1.208(8) . ? N12 O12 1.229(9) . ? C42' C43' 1.344(9) . ? C42' H42' 0.9500 . ? C43' C44' 1.386(9) . ? C43' N12' 1.449(9) . ? C44' H44B 0.9500 . ? N12' O12' 1.210(10) . ? N12' O11' 1.232(9) . ? N17 C52 1.174(9) . ? C52 C53 1.451(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? N18 C54 1.038(12) . ? C54 C55 1.360(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C9 C10 1.533(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.438(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9' C10' 1.458(10) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10' C11' 1.511(11) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' H11D 0.9800 . ? C11' H11E 0.9800 . ? C11' H11F 0.9800 . ? C21 C22 1.546(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C21' C22' 1.332(14) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 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 O15 Eu1 O1 74.09(6) . . ? O15 Eu1 O8 78.18(6) . . ? O1 Eu1 O8 75.32(6) . . ? O15 Eu1 N2 123.54(6) . . ? O1 Eu1 N2 139.04(6) . . ? O8 Eu1 N2 73.57(6) . . ? O15 Eu1 N6 133.80(6) . . ? O1 Eu1 N6 74.08(7) . . ? O8 Eu1 N6 123.81(6) . . ? N2 Eu1 N6 102.41(7) . . ? O15 Eu1 N4 74.83(6) . . ? O1 Eu1 N4 122.43(6) . . ? O8 Eu1 N4 140.72(7) . . ? N2 Eu1 N4 98.48(6) . . ? N6 Eu1 N4 95.44(7) . . ? O15 Eu1 O9 138.51(6) . . ? O1 Eu1 O9 77.51(6) . . ? O8 Eu1 O9 65.68(6) . . ? N2 Eu1 O9 65.73(6) . . ? N6 Eu1 O9 62.39(6) . . ? N4 Eu1 O9 146.65(6) . . ? O15 Eu1 O16 64.62(6) . . ? O1 Eu1 O16 134.43(6) . . ? O8 Eu1 O16 78.11(6) . . ? N2 Eu1 O16 62.31(6) . . ? N6 Eu1 O16 150.58(6) . . ? N4 Eu1 O16 64.74(6) . . ? O9 Eu1 O16 122.81(5) . . ? O15 Eu1 N1 134.68(6) . . ? O1 Eu1 N1 135.72(7) . . ? O8 Eu1 N1 133.93(6) . . ? N2 Eu1 N1 61.39(7) . . ? N6 Eu1 N1 61.97(7) . . ? N4 Eu1 N1 60.40(6) . . ? O9 Eu1 N1 86.51(6) . . ? O16 Eu1 N1 88.79(6) . . ? O15 Eu1 O2 73.24(6) . . ? O1 Eu1 O2 62.54(6) . . ? O8 Eu1 O2 133.89(6) . . ? N2 Eu1 O2 152.43(7) . . ? N6 Eu1 O2 62.63(6) . . ? N4 Eu1 O2 62.64(6) . . ? O9 Eu1 O2 118.33(6) . . ? O16 Eu1 O2 118.72(6) . . ? N1 Eu1 O2 91.14(6) . . ? C23 N1 C12 110.2(2) . . ? C23 N1 C1 110.0(2) . . ? C12 N1 C1 110.0(2) . . ? C23 N1 Eu1 109.52(14) . . ? C12 N1 Eu1 109.53(15) . . ? C1 N1 Eu1 107.56(15) . . ? C2 N2 C3 105.2(2) . . ? C2 N2 Eu1 118.15(17) . . ? C3 N2 Eu1 135.26(17) . . ? C2 N3 C8 106.9(2) . . ? C2 N3 C9 122.8(3) . . ? C8 N3 C9 127.9(3) . . ? C2 N3 C9' 128.5(3) . . ? C8 N3 C9' 119.9(3) . . ? C9 N3 C9' 33.4(3) . . ? C13 N4 C14 104.9(2) . . ? C13 N4 Eu1 116.90(15) . . ? C14 N4 Eu1 131.61(17) . . ? C13 N5 C19 106.8(2) . . ? C13 N5 C20 127.4(2) . . ? C19 N5 C20 125.6(2) . . ? C24 N6 C25 104.4(2) . . ? C24 N6 Eu1 119.16(17) . . ? C25 N6 Eu1 134.54(18) . . ? C24 N7 C30 106.5(2) . . ? C24 N7 C31 128.2(2) . . ? C30 N7 C31 125.3(2) . . ? O2 N8 O3 121.8(3) . . ? O2 N8 C35 120.8(3) . . ? O3 N8 C35 117.4(3) . . ? O4 N9 O5 124.5(3) . . ? O4 N9 C37 117.3(3) . . ? O5 N9 C37 118.2(3) . . ? O7 N10 O6 123.0(3) . . ? O7 N10 C39 119.3(3) . . ? O6 N10 C39 117.6(3) . . ? O9 N11 O10 120.7(3) . . ? O9 N11 C41 119.2(2) . . ? O10 N11 C41 120.0(2) . . ? O20 N14 O21 123.4(2) . . ? O20 N14 C51 118.3(2) . . ? O21 N14 C51 118.3(2) . . ? O17 N15 O16 121.2(2) . . ? O17 N15 C47 118.5(2) . . ? O16 N15 C47 120.3(2) . . ? O19 N16 O18 123.9(2) . . ? O19 N16 C49 118.3(2) . . ? O18 N16 C49 117.8(2) . . ? C2 C1 N1 108.5(2) . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? N1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 112.6(2) . . ? N2 C2 C1 121.7(2) . . ? N3 C2 C1 125.7(2) . . ? C8 C3 N2 109.1(2) . . ? C8 C3 C4 120.2(2) . . ? N2 C3 C4 130.6(2) . . ? C5 C4 C3 117.0(3) . . ? C5 C4 H4A 121.5 . . ? C3 C4 H4A 121.5 . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 121.6(3) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 117.1(3) . . ? C6 C7 H7A 121.5 . . ? C8 C7 H7A 121.5 . . ? C3 C8 N3 106.2(2) . . ? C3 C8 C7 122.2(3) . . ? N3 C8 C7 131.5(3) . . ? N1 C12 C13 108.3(2) . . ? N1 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N1 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N4 C13 N5 113.6(2) . . ? N4 C13 C12 122.2(2) . . ? N5 C13 C12 124.2(2) . . ? C15 C14 C19 121.0(2) . . ? C15 C14 N4 130.5(2) . . ? C19 C14 N4 108.5(2) . . ? C16 C15 C14 117.5(3) . . ? C16 C15 H15A 121.3 . . ? C14 C15 H15A 121.3 . . ? C15 C16 C17 120.8(3) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 122.4(3) . . ? C18 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? C17 C18 C19 116.9(3) . . ? C17 C18 H18A 121.5 . . ? C19 C18 H18A 121.5 . . ? N5 C19 C18 132.4(3) . . ? N5 C19 C14 106.1(2) . . ? C18 C19 C14 121.5(3) . . ? N5 C20 C21' 112.8(5) . . ? N5 C20 C21 111.2(3) . . ? C21' C20 C21 31.8(4) . . ? N5 C20 H20A 109.4 . . ? C21' C20 H20A 131.4 . . ? C21 C20 H20A 109.4 . . ? N5 C20 H20B 109.4 . . ? C21' C20 H20B 79.6 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N1 C23 C24 110.6(2) . . ? N1 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N6 C24 N7 114.3(2) . . ? N6 C24 C23 121.8(2) . . ? N7 C24 C23 123.9(2) . . ? C26 C25 C30 119.5(3) . . ? C26 C25 N6 130.7(3) . . ? C30 C25 N6 109.6(2) . . ? C27 C26 C25 117.3(3) . . ? C27 C26 H26A 121.3 . . ? C25 C26 H26A 121.3 . . ? C26 C27 C28 121.9(3) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C29 C28 C27 120.7(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C28 115.8(3) . . ? C30 C29 H29A 122.1 . . ? C28 C29 H29A 122.1 . . ? C29 C30 C25 124.7(3) . . ? C29 C30 N7 130.0(3) . . ? C25 C30 N7 105.2(2) . . ? N7 C31 C32 114.4(3) . . ? N7 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N7 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 119.0(4) . . ? C33 C32 H32A 107.6 . . ? C31 C32 H32A 107.6 . . ? C33 C32 H32B 107.6 . . ? C31 C32 H32B 107.6 . . ? H32A C32 H32B 107.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O1 C34 C39 122.6(3) . . ? O1 C34 C35 125.1(3) . . ? C39 C34 C35 112.3(2) . . ? C36 C35 C34 123.4(3) . . ? C36 C35 N8 116.5(3) . . ? C34 C35 N8 120.0(2) . . ? C37 C36 C35 119.1(3) . . ? C37 C36 H36A 120.5 . . ? C35 C36 H36A 120.5 . . ? C36 C37 C38 121.5(3) . . ? C36 C37 N9 119.4(3) . . ? C38 C37 N9 119.1(3) . . ? C39 C38 C37 119.0(3) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? C38 C39 C34 124.5(3) . . ? C38 C39 N10 118.5(3) . . ? C34 C39 N10 116.9(2) . . ? O15 C46 C47 125.9(2) . . ? O15 C46 C51 122.1(2) . . ? C47 C46 C51 112.0(2) . . ? C48 C47 C46 123.9(2) . . ? C48 C47 N15 117.3(2) . . ? C46 C47 N15 118.8(2) . . ? C47 C48 C49 118.8(2) . . ? C47 C48 H48A 120.6 . . ? C49 C48 H48A 120.6 . . ? C48 C49 C50 121.8(3) . . ? C48 C49 N16 118.9(2) . . ? C50 C49 N16 119.3(2) . . ? C51 C50 C49 117.8(2) . . ? C51 C50 H50A 121.1 . . ? C49 C50 H50A 121.1 . . ? C50 C51 C46 125.4(2) . . ? C50 C51 N14 117.8(2) . . ? C46 C51 N14 116.7(2) . . ? C34 O1 Eu1 146.04(17) . . ? N8 O2 Eu1 136.30(18) . . ? C40 O8 Eu1 142.42(19) . . ? N11 O9 Eu1 133.57(17) . . ? C46 O15 Eu1 143.03(15) . . ? N15 O16 Eu1 136.38(15) . . ? O8 C40 C45 123.6(3) . . ? O8 C40 C41 123.9(3) . . ? C45 C40 C41 112.5(3) . . ? C42 C41 N11 109.9(3) . . ? C42 C41 C40 128.6(4) . . ? N11 C41 C40 120.1(2) . . ? C42 C41 C42' 27.9(3) . . ? N11 C41 C42' 120.2(3) . . ? C40 C41 C42' 117.8(4) . . ? C40 C45 C44' 127.2(4) . . ? C40 C45 C44 118.2(4) . . ? C44' C45 C44 32.5(3) . . ? C40 C45 N13 120.6(3) . . ? C44' C45 N13 109.0(4) . . ? C44 C45 N13 119.6(4) . . ? O14 N13 O13' 104.5(4) . . ? O14 N13 O13 125.3(4) . . ? O13' N13 O13 29.6(3) . . ? O14 N13 O14' 53.3(4) . . ? O13' N13 O14' 116.5(6) . . ? O13 N13 O14' 109.5(5) . . ? O14 N13 C45 119.3(3) . . ? O13' N13 C45 126.0(4) . . ? O13 N13 C45 114.7(3) . . ? O14' N13 C45 114.6(5) . . ? C41 C42 C43 114.7(5) . . ? C41 C42 H42A 122.6 . . ? C43 C42 H42A 122.6 . . ? C44 C43 C42 120.7(6) . . ? C44 C43 N12 120.8(6) . . ? C42 C43 N12 118.5(6) . . ? C43 C44 C45 122.2(6) . . ? C43 C44 H44A 118.9 . . ? C45 C44 H44A 118.9 . . ? O11 N12 O12 125.6(6) . . ? O11 N12 C43 118.1(6) . . ? O12 N12 C43 115.6(6) . . ? C43' C42' C41 123.4(5) . . ? C43' C42' H42' 118.3 . . ? C41 C42' H42' 118.3 . . ? C42' C43' C44' 121.5(6) . . ? C42' C43' N12' 119.1(6) . . ? C44' C43' N12' 119.5(6) . . ? C43' C44' C45 114.7(6) . . ? C43' C44' H44B 122.7 . . ? C45 C44' H44B 122.7 . . ? O12' N12' O11' 121.2(7) . . ? O12' N12' C43' 117.9(7) . . ? O11' N12' C43' 120.8(7) . . ? N17 C52 C53 175.8(7) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N18 C54 C55 115.8(14) . . ? C54 C55 H55A 109.4 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C9 C10 108.9(4) . . ? N3 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N3 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C9 114.8(5) . . ? C11 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10' C9' N3 106.2(5) . . ? C10' C9' H9'A 110.5 . . ? N3 C9' H9'A 110.5 . . ? C10' C9' H9'B 110.5 . . ? N3 C9' H9'B 110.5 . . ? H9'A C9' H9'B 108.7 . . ? C9' C10' C11' 108.5(7) . . ? C9' C10' H10C 110.0 . . ? C11' C10' H10C 110.0 . . ? C9' C10' H10D 110.0 . . ? C11' C10' H10D 110.0 . . ? H10C C10' H10D 108.4 . . ? C10' C11' H11D 109.5 . . ? C10' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C10' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C22 C21 C20 112.1(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C22' C21' C20 109.8(9) . . ? C22' C21' H21C 109.7 . . ? C20 C21' H21C 109.7 . . ? C22' C21' H21D 109.7 . . ? C20 C21' H21D 109.7 . . ? H21C C21' H21D 108.2 . . ? C21' C22' H22D 109.5 . . ? C21' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 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 O15 Eu1 N1 C23 91.02(16) . . . . ? O1 Eu1 N1 C23 -26.47(18) . . . . ? O8 Eu1 N1 C23 -145.42(14) . . . . ? N2 Eu1 N1 C23 -158.76(17) . . . . ? N6 Eu1 N1 C23 -34.16(14) . . . . ? N4 Eu1 N1 C23 81.04(15) . . . . ? O9 Eu1 N1 C23 -94.59(15) . . . . ? O16 Eu1 N1 C23 142.43(15) . . . . ? O2 Eu1 N1 C23 23.72(15) . . . . ? O15 Eu1 N1 C12 -29.90(18) . . . . ? O1 Eu1 N1 C12 -147.39(14) . . . . ? O8 Eu1 N1 C12 93.66(16) . . . . ? N2 Eu1 N1 C12 80.32(15) . . . . ? N6 Eu1 N1 C12 -155.08(16) . . . . ? N4 Eu1 N1 C12 -39.88(14) . . . . ? O9 Eu1 N1 C12 144.49(15) . . . . ? O16 Eu1 N1 C12 21.51(15) . . . . ? O2 Eu1 N1 C12 -97.19(15) . . . . ? O15 Eu1 N1 C1 -149.48(15) . . . . ? O1 Eu1 N1 C1 93.02(17) . . . . ? O8 Eu1 N1 C1 -25.93(19) . . . . ? N2 Eu1 N1 C1 -39.26(15) . . . . ? N6 Eu1 N1 C1 85.33(16) . . . . ? N4 Eu1 N1 C1 -159.47(18) . . . . ? O9 Eu1 N1 C1 24.90(16) . . . . ? O16 Eu1 N1 C1 -98.08(16) . . . . ? O2 Eu1 N1 C1 143.22(16) . . . . ? O15 Eu1 N2 C2 155.68(17) . . . . ? O1 Eu1 N2 C2 -99.1(2) . . . . ? O8 Eu1 N2 C2 -141.2(2) . . . . ? N6 Eu1 N2 C2 -19.2(2) . . . . ? N4 Eu1 N2 C2 78.30(19) . . . . ? O9 Eu1 N2 C2 -70.92(19) . . . . ? O16 Eu1 N2 C2 133.9(2) . . . . ? N1 Eu1 N2 C2 28.86(18) . . . . ? O2 Eu1 N2 C2 34.2(3) . . . . ? O15 Eu1 N2 C3 -40.2(2) . . . . ? O1 Eu1 N2 C3 64.9(3) . . . . ? O8 Eu1 N2 C3 22.9(2) . . . . ? N6 Eu1 N2 C3 144.9(2) . . . . ? N4 Eu1 N2 C3 -117.6(2) . . . . ? O9 Eu1 N2 C3 93.2(2) . . . . ? O16 Eu1 N2 C3 -62.0(2) . . . . ? N1 Eu1 N2 C3 -167.1(2) . . . . ? O2 Eu1 N2 C3 -161.69(19) . . . . ? O15 Eu1 N4 C13 -139.5(2) . . . . ? O1 Eu1 N4 C13 161.09(18) . . . . ? O8 Eu1 N4 C13 -91.3(2) . . . . ? N2 Eu1 N4 C13 -16.9(2) . . . . ? N6 Eu1 N4 C13 86.5(2) . . . . ? O9 Eu1 N4 C13 41.1(3) . . . . ? O16 Eu1 N4 C13 -70.79(19) . . . . ? N1 Eu1 N4 C13 33.16(18) . . . . ? O2 Eu1 N4 C13 141.8(2) . . . . ? O15 Eu1 N4 C14 7.3(2) . . . . ? O1 Eu1 N4 C14 -52.1(2) . . . . ? O8 Eu1 N4 C14 55.5(2) . . . . ? N2 Eu1 N4 C14 129.9(2) . . . . ? N6 Eu1 N4 C14 -126.7(2) . . . . ? O9 Eu1 N4 C14 -172.05(18) . . . . ? O16 Eu1 N4 C14 76.0(2) . . . . ? N1 Eu1 N4 C14 180.0(2) . . . . ? O2 Eu1 N4 C14 -71.4(2) . . . . ? O15 Eu1 N6 C24 -100.91(18) . . . . ? O1 Eu1 N6 C24 -148.96(18) . . . . ? O8 Eu1 N6 C24 151.59(16) . . . . ? N2 Eu1 N6 C24 73.20(18) . . . . ? N4 Eu1 N6 C24 -26.75(18) . . . . ? O9 Eu1 N6 C24 127.04(19) . . . . ? O16 Eu1 N6 C24 18.5(2) . . . . ? N1 Eu1 N6 C24 25.47(16) . . . . ? O2 Eu1 N6 C24 -82.05(17) . . . . ? O15 Eu1 N6 C25 60.6(2) . . . . ? O1 Eu1 N6 C25 12.5(2) . . . . ? O8 Eu1 N6 C25 -46.9(2) . . . . ? N2 Eu1 N6 C25 -125.3(2) . . . . ? N4 Eu1 N6 C25 134.7(2) . . . . ? O9 Eu1 N6 C25 -71.5(2) . . . . ? O16 Eu1 N6 C25 -179.98(18) . . . . ? N1 Eu1 N6 C25 -173.0(2) . . . . ? O2 Eu1 N6 C25 79.4(2) . . . . ? C23 N1 C1 C2 166.6(2) . . . . ? C12 N1 C1 C2 -71.9(3) . . . . ? Eu1 N1 C1 C2 47.4(2) . . . . ? C3 N2 C2 N3 -0.9(3) . . . . ? Eu1 N2 C2 N3 167.59(18) . . . . ? C3 N2 C2 C1 177.1(2) . . . . ? Eu1 N2 C2 C1 -14.4(3) . . . . ? C8 N3 C2 N2 1.7(3) . . . . ? C9 N3 C2 N2 -162.2(3) . . . . ? C9' N3 C2 N2 156.9(4) . . . . ? C8 N3 C2 C1 -176.2(3) . . . . ? C9 N3 C2 C1 19.9(5) . . . . ? C9' N3 C2 C1 -21.0(5) . . . . ? N1 C1 C2 N2 -25.2(4) . . . . ? N1 C1 C2 N3 152.5(3) . . . . ? C2 N2 C3 C8 -0.3(3) . . . . ? Eu1 N2 C3 C8 -165.78(19) . . . . ? C2 N2 C3 C4 -177.1(3) . . . . ? Eu1 N2 C3 C4 17.5(4) . . . . ? C8 C3 C4 C5 -1.7(4) . . . . ? N2 C3 C4 C5 174.7(3) . . . . ? C3 C4 C5 C6 1.3(4) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? N2 C3 C8 N3 1.3(3) . . . . ? C4 C3 C8 N3 178.4(2) . . . . ? N2 C3 C8 C7 -176.2(3) . . . . ? C4 C3 C8 C7 0.9(4) . . . . ? C2 N3 C8 C3 -1.8(3) . . . . ? C9 N3 C8 C3 161.1(3) . . . . ? C9' N3 C8 C3 -159.5(3) . . . . ? C2 N3 C8 C7 175.4(3) . . . . ? C9 N3 C8 C7 -21.7(6) . . . . ? C9' N3 C8 C7 17.7(6) . . . . ? C6 C7 C8 C3 0.4(5) . . . . ? C6 C7 C8 N3 -176.4(3) . . . . ? C23 N1 C12 C13 -76.6(3) . . . . ? C1 N1 C12 C13 162.0(2) . . . . ? Eu1 N1 C12 C13 43.9(2) . . . . ? C14 N4 C13 N5 0.1(3) . . . . ? Eu1 N4 C13 N5 155.02(18) . . . . ? C14 N4 C13 C12 -178.5(2) . . . . ? Eu1 N4 C13 C12 -23.5(3) . . . . ? C19 N5 C13 N4 -1.4(3) . . . . ? C20 N5 C13 N4 -177.6(3) . . . . ? C19 N5 C13 C12 177.1(3) . . . . ? C20 N5 C13 C12 0.9(4) . . . . ? N1 C12 C13 N4 -16.1(4) . . . . ? N1 C12 C13 N5 165.4(2) . . . . ? C13 N4 C14 C15 -179.5(3) . . . . ? Eu1 N4 C14 C15 30.8(4) . . . . ? C13 N4 C14 C19 1.3(3) . . . . ? Eu1 N4 C14 C19 -148.38(19) . . . . ? C19 C14 C15 C16 0.7(4) . . . . ? N4 C14 C15 C16 -178.4(3) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C15 C16 C17 C18 -2.3(5) . . . . ? C16 C17 C18 C19 2.7(5) . . . . ? C13 N5 C19 C18 -179.3(3) . . . . ? C20 N5 C19 C18 -3.0(5) . . . . ? C13 N5 C19 C14 2.1(3) . . . . ? C20 N5 C19 C14 178.4(3) . . . . ? C17 C18 C19 N5 -179.9(3) . . . . ? C17 C18 C19 C14 -1.5(4) . . . . ? C15 C14 C19 N5 178.6(2) . . . . ? N4 C14 C19 N5 -2.1(3) . . . . ? C15 C14 C19 C18 -0.2(4) . . . . ? N4 C14 C19 C18 179.1(3) . . . . ? C13 N5 C20 C21' 111.7(5) . . . . ? C19 N5 C20 C21' -63.9(5) . . . . ? C13 N5 C20 C21 77.4(4) . . . . ? C19 N5 C20 C21 -98.2(4) . . . . ? C12 N1 C23 C24 161.9(2) . . . . ? C1 N1 C23 C24 -76.6(3) . . . . ? Eu1 N1 C23 C24 41.4(2) . . . . ? C25 N6 C24 N7 -1.1(3) . . . . ? Eu1 N6 C24 N7 165.39(15) . . . . ? C25 N6 C24 C23 -179.9(2) . . . . ? Eu1 N6 C24 C23 -13.4(3) . . . . ? C30 N7 C24 N6 1.3(3) . . . . ? C31 N7 C24 N6 -179.4(2) . . . . ? C30 N7 C24 C23 -179.9(2) . . . . ? C31 N7 C24 C23 -0.6(4) . . . . ? N1 C23 C24 N6 -21.4(3) . . . . ? N1 C23 C24 N7 159.9(2) . . . . ? C24 N6 C25 C26 -175.7(3) . . . . ? Eu1 N6 C25 C26 20.9(4) . . . . ? C24 N6 C25 C30 0.5(3) . . . . ? Eu1 N6 C25 C30 -162.92(17) . . . . ? C30 C25 C26 C27 1.1(4) . . . . ? N6 C25 C26 C27 177.0(3) . . . . ? C25 C26 C27 C28 -0.1(4) . . . . ? C26 C27 C28 C29 -1.3(5) . . . . ? C27 C28 C29 C30 1.7(5) . . . . ? C28 C29 C30 C25 -0.7(4) . . . . ? C28 C29 C30 N7 -177.8(3) . . . . ? C26 C25 C30 C29 -0.7(4) . . . . ? N6 C25 C30 C29 -177.4(3) . . . . ? C26 C25 C30 N7 176.9(2) . . . . ? N6 C25 C30 N7 0.3(3) . . . . ? C24 N7 C30 C29 176.6(3) . . . . ? C31 N7 C30 C29 -2.8(4) . . . . ? C24 N7 C30 C25 -0.9(3) . . . . ? C31 N7 C30 C25 179.7(2) . . . . ? C24 N7 C31 C32 83.0(4) . . . . ? C30 N7 C31 C32 -97.8(4) . . . . ? N7 C31 C32 C33 52.2(5) . . . . ? O1 C34 C35 C36 -179.9(3) . . . . ? C39 C34 C35 C36 -1.2(4) . . . . ? O1 C34 C35 N8 1.9(4) . . . . ? C39 C34 C35 N8 -179.4(3) . . . . ? O2 N8 C35 C36 -156.9(3) . . . . ? O3 N8 C35 C36 23.2(4) . . . . ? O2 N8 C35 C34 21.4(4) . . . . ? O3 N8 C35 C34 -158.5(3) . . . . ? C34 C35 C36 C37 -2.9(5) . . . . ? N8 C35 C36 C37 175.4(3) . . . . ? C35 C36 C37 C38 3.5(5) . . . . ? C35 C36 C37 N9 -175.8(3) . . . . ? O4 N9 C37 C36 -11.2(5) . . . . ? O5 N9 C37 C36 168.5(3) . . . . ? O4 N9 C37 C38 169.6(3) . . . . ? O5 N9 C37 C38 -10.8(4) . . . . ? C36 C37 C38 C39 0.2(5) . . . . ? N9 C37 C38 C39 179.5(3) . . . . ? C37 C38 C39 C34 -4.9(5) . . . . ? C37 C38 C39 N10 175.6(3) . . . . ? O1 C34 C39 C38 -176.1(3) . . . . ? C35 C34 C39 C38 5.2(4) . . . . ? O1 C34 C39 N10 3.4(4) . . . . ? C35 C34 C39 N10 -175.3(3) . . . . ? O7 N10 C39 C38 -135.9(3) . . . . ? O6 N10 C39 C38 39.5(4) . . . . ? O7 N10 C39 C34 44.5(4) . . . . ? O6 N10 C39 C34 -140.0(3) . . . . ? O15 C46 C47 C48 176.6(2) . . . . ? C51 C46 C47 C48 -4.5(3) . . . . ? O15 C46 C47 N15 -5.1(4) . . . . ? C51 C46 C47 N15 173.7(2) . . . . ? O17 N15 C47 C48 26.8(3) . . . . ? O16 N15 C47 C48 -151.6(2) . . . . ? O17 N15 C47 C46 -151.6(2) . . . . ? O16 N15 C47 C46 30.0(3) . . . . ? C46 C47 C48 C49 0.1(4) . . . . ? N15 C47 C48 C49 -178.2(2) . . . . ? C47 C48 C49 C50 2.8(4) . . . . ? C47 C48 C49 N16 -177.4(2) . . . . ? O19 N16 C49 C48 -169.0(2) . . . . ? O18 N16 C49 C48 10.5(4) . . . . ? O19 N16 C49 C50 10.9(4) . . . . ? O18 N16 C49 C50 -169.7(2) . . . . ? C48 C49 C50 C51 -0.6(4) . . . . ? N16 C49 C50 C51 179.6(2) . . . . ? C49 C50 C51 C46 -4.8(4) . . . . ? C49 C50 C51 N14 178.2(2) . . . . ? O15 C46 C51 C50 -174.0(2) . . . . ? C47 C46 C51 C50 7.0(4) . . . . ? O15 C46 C51 N14 3.0(3) . . . . ? C47 C46 C51 N14 -176.0(2) . . . . ? O20 N14 C51 C50 42.5(3) . . . . ? O21 N14 C51 C50 -135.6(2) . . . . ? O20 N14 C51 C46 -134.7(2) . . . . ? O21 N14 C51 C46 47.1(3) . . . . ? C39 C34 O1 Eu1 142.3(3) . . . . ? C35 C34 O1 Eu1 -39.2(5) . . . . ? O15 Eu1 O1 C34 -47.3(3) . . . . ? O8 Eu1 O1 C34 -129.0(4) . . . . ? N2 Eu1 O1 C34 -170.6(3) . . . . ? N6 Eu1 O1 C34 98.7(3) . . . . ? N4 Eu1 O1 C34 12.4(4) . . . . ? O9 Eu1 O1 C34 163.2(4) . . . . ? O16 Eu1 O1 C34 -72.7(4) . . . . ? N1 Eu1 O1 C34 91.7(3) . . . . ? O2 Eu1 O1 C34 31.7(3) . . . . ? O3 N8 O2 Eu1 159.0(2) . . . . ? C35 N8 O2 Eu1 -20.9(4) . . . . ? O15 Eu1 O2 N8 82.2(3) . . . . ? O1 Eu1 O2 N8 1.8(3) . . . . ? O8 Eu1 O2 N8 28.1(3) . . . . ? N2 Eu1 O2 N8 -145.8(3) . . . . ? N6 Eu1 O2 N8 -83.7(3) . . . . ? N4 Eu1 O2 N8 163.5(3) . . . . ? O9 Eu1 O2 N8 -54.4(3) . . . . ? O16 Eu1 O2 N8 129.7(3) . . . . ? N1 Eu1 O2 N8 -141.1(3) . . . . ? O15 Eu1 O8 C40 -137.5(3) . . . . ? O1 Eu1 O8 C40 -61.1(3) . . . . ? N2 Eu1 O8 C40 91.9(3) . . . . ? N6 Eu1 O8 C40 -2.2(3) . . . . ? N4 Eu1 O8 C40 175.2(3) . . . . ? O9 Eu1 O8 C40 21.6(3) . . . . ? O16 Eu1 O8 C40 156.3(3) . . . . ? N1 Eu1 O8 C40 79.7(3) . . . . ? O2 Eu1 O8 C40 -85.1(3) . . . . ? O10 N11 O9 Eu1 137.8(2) . . . . ? C41 N11 O9 Eu1 -45.0(4) . . . . ? O15 Eu1 O9 N11 52.0(3) . . . . ? O1 Eu1 O9 N11 99.6(2) . . . . ? O8 Eu1 O9 N11 20.2(2) . . . . ? N2 Eu1 O9 N11 -61.9(2) . . . . ? N6 Eu1 O9 N11 178.0(2) . . . . ? N4 Eu1 O9 N11 -128.9(2) . . . . ? O16 Eu1 O9 N11 -35.7(2) . . . . ? N1 Eu1 O9 N11 -122.0(2) . . . . ? O2 Eu1 O9 N11 148.6(2) . . . . ? C47 C46 O15 Eu1 -33.2(4) . . . . ? C51 C46 O15 Eu1 148.02(19) . . . . ? O1 Eu1 O15 C46 -131.3(3) . . . . ? O8 Eu1 O15 C46 -53.4(3) . . . . ? N2 Eu1 O15 C46 7.5(3) . . . . ? N6 Eu1 O15 C46 -179.4(2) . . . . ? N4 Eu1 O15 C46 97.8(3) . . . . ? O9 Eu1 O15 C46 -82.8(3) . . . . ? O16 Eu1 O15 C46 28.9(3) . . . . ? N1 Eu1 O15 C46 88.8(3) . . . . ? O2 Eu1 O15 C46 163.2(3) . . . . ? O17 N15 O16 Eu1 153.99(19) . . . . ? C47 N15 O16 Eu1 -27.7(4) . . . . ? O15 Eu1 O16 N15 3.9(2) . . . . ? O1 Eu1 O16 N15 31.0(3) . . . . ? O8 Eu1 O16 N15 86.3(2) . . . . ? N2 Eu1 O16 N15 163.9(3) . . . . ? N6 Eu1 O16 N15 -132.0(2) . . . . ? N4 Eu1 O16 N15 -80.6(2) . . . . ? O9 Eu1 O16 N15 136.8(2) . . . . ? N1 Eu1 O16 N15 -138.1(2) . . . . ? O2 Eu1 O16 N15 -47.5(3) . . . . ? Eu1 O8 C40 C45 148.3(2) . . . . ? Eu1 O8 C40 C41 -33.7(4) . . . . ? O9 N11 C41 C42 -159.7(3) . . . . ? O10 N11 C41 C42 17.5(5) . . . . ? O9 N11 C41 C40 32.8(4) . . . . ? O10 N11 C41 C40 -150.1(3) . . . . ? O9 N11 C41 C42' -130.9(4) . . . . ? O10 N11 C41 C42' 46.2(5) . . . . ? O8 C40 C41 C42 -162.7(4) . . . . ? C45 C40 C41 C42 15.6(5) . . . . ? O8 C40 C41 N11 2.3(4) . . . . ? C45 C40 C41 N11 -179.5(3) . . . . ? O8 C40 C41 C42' 166.4(4) . . . . ? C45 C40 C41 C42' -15.4(5) . . . . ? O8 C40 C45 C44' -160.3(4) . . . . ? C41 C40 C45 C44' 21.5(5) . . . . ? O8 C40 C45 C44 162.4(4) . . . . ? C41 C40 C45 C44 -15.8(5) . . . . ? O8 C40 C45 N13 -2.7(5) . . . . ? C41 C40 C45 N13 179.0(3) . . . . ? C40 C45 N13 O14 -29.9(5) . . . . ? C44' C45 N13 O14 131.3(4) . . . . ? C44 C45 N13 O14 165.2(4) . . . . ? C40 C45 N13 O13' -169.7(5) . . . . ? C44' C45 N13 O13' -8.5(6) . . . . ? C44 C45 N13 O13' 25.4(7) . . . . ? C40 C45 N13 O13 158.3(4) . . . . ? C44' C45 N13 O13 -40.5(5) . . . . ? C44 C45 N13 O13 -6.6(6) . . . . ? C40 C45 N13 O14' 30.3(6) . . . . ? C44' C45 N13 O14' -168.5(5) . . . . ? C44 C45 N13 O14' -134.6(6) . . . . ? N11 C41 C42 C43 -179.2(4) . . . . ? C40 C41 C42 C43 -13.1(7) . . . . ? C42' C41 C42 C43 63.4(8) . . . . ? C41 C42 C43 C44 11.4(8) . . . . ? C41 C42 C43 N12 -171.0(5) . . . . ? C42 C43 C44 C45 -14.3(9) . . . . ? N12 C43 C44 C45 168.1(5) . . . . ? C40 C45 C44 C43 16.9(7) . . . . ? C44' C45 C44 C43 -99.0(9) . . . . ? N13 C45 C44 C43 -177.8(5) . . . . ? C44 C43 N12 O11 -173.3(6) . . . . ? C42 C43 N12 O11 9.1(9) . . . . ? C44 C43 N12 O12 -2.7(9) . . . . ? C42 C43 N12 O12 179.7(6) . . . . ? C42 C41 C42' C43' -114.2(11) . . . . ? N11 C41 C42' C43' 170.7(5) . . . . ? C40 C41 C42' C43' 6.6(7) . . . . ? C41 C42' C43' C44' -0.4(9) . . . . ? C41 C42' C43' N12' 179.7(5) . . . . ? C42' C43' C44' C45 4.1(8) . . . . ? N12' C43' C44' C45 -176.0(5) . . . . ? C40 C45 C44' C43' -16.0(7) . . . . ? C44 C45 C44' C43' 68.9(8) . . . . ? N13 C45 C44' C43' -175.6(4) . . . . ? C42' C43' N12' O12' -177.8(7) . . . . ? C44' C43' N12' O12' 2.3(10) . . . . ? C42' C43' N12' O11' -1.7(10) . . . . ? C44' C43' N12' O11' 178.5(6) . . . . ? C2 N3 C9 C10 -113.3(4) . . . . ? C8 N3 C9 C10 86.3(5) . . . . ? C9' N3 C9 C10 -1.8(5) . . . . ? N3 C9 C10 C11 69.5(6) . . . . ? C2 N3 C9' C10' 120.5(5) . . . . ? C8 N3 C9' C10' -87.0(6) . . . . ? C9 N3 C9' C10' 27.5(5) . . . . ? N3 C9' C10' C11' 174.7(6) . . . . ? N5 C20 C21 C22 73.7(5) . . . . ? C21' C20 C21 C22 -25.7(8) . . . . ? N5 C20 C21' C22' -80.5(9) . . . . ? C21 C20 C21' C22' 13.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.277 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.111 #=====================================# data_12 _database_code_depnum_ccdc_archive 'CCDC 698714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H37 Cl3 Eu N7 O' _chemical_formula_weight 781.99 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 12.5760(4) _cell_length_b 16.8021(3) _cell_length_c 16.3175(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.530(4) _cell_angle_gamma 90.00 _cell_volume 3184.79(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8141 _cell_measurement_theta_min 2.5897 _cell_measurement_theta_max 30.2425 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 2.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6608 _exptl_absorpt_correction_T_max 0.8954 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0855 _diffrn_measurement_device_type Germini _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17110 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5788 _reflns_number_gt 4236 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5788 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.19414(2) 0.737335(11) -0.043235(13) 0.01937(7) Uani 1 1 d . . . N1 N 0.3873(3) 0.76863(18) 0.0771(2) 0.0225(8) Uani 1 1 d . . . N2 N 0.5189(3) 0.75786(17) 0.2148(2) 0.0214(8) Uani 1 1 d . . . N3 N 0.1702(3) 0.60303(17) 0.0210(2) 0.0200(9) Uani 1 1 d . . . N4 N 0.1238(3) 0.52853(17) 0.1154(2) 0.0199(9) Uani 1 1 d . . . N5 N 0.0389(3) 0.81634(17) -0.0138(2) 0.0199(8) Uani 1 1 d . . . N6 N -0.0065(3) 0.90180(17) 0.0728(2) 0.0204(9) Uani 1 1 d . . . N7 N 0.2033(3) 0.73715(17) 0.1258(2) 0.0178(8) Uani 1 1 d . . . C1 C 0.4086(4) 0.7496(2) 0.1612(3) 0.0199(10) Uani 1 1 d . . . C2 C 0.4951(4) 0.7889(2) 0.0776(3) 0.0234(11) Uani 1 1 d . . . C3 C 0.5265(4) 0.8134(2) 0.0074(3) 0.0301(12) Uani 1 1 d . . . H3A H 0.4707 0.8198 -0.0511 0.036 Uiso 1 1 calc R . . C4 C 0.6415(4) 0.8278(2) 0.0274(3) 0.0302(12) Uani 1 1 d . . . H4A H 0.6652 0.8440 -0.0188 0.036 Uiso 1 1 calc R . . C5 C 0.7246(4) 0.8194(2) 0.1132(3) 0.0300(12) Uani 1 1 d . . . H5A H 0.8031 0.8294 0.1238 0.036 Uiso 1 1 calc R . . C6 C 0.6948(4) 0.7966(2) 0.1832(3) 0.0269(11) Uani 1 1 d . . . H6A H 0.7506 0.7913 0.2419 0.032 Uiso 1 1 calc R . . C7 C 0.5793(4) 0.7822(2) 0.1628(3) 0.0201(10) Uani 1 1 d . . . C8 C 0.5704(4) 0.7426(2) 0.3111(3) 0.0324(12) Uani 1 1 d . . . H8A H 0.5100 0.7270 0.3319 0.049 Uiso 1 1 calc R . . H8B H 0.6084 0.7911 0.3420 0.049 Uiso 1 1 calc R . . H8C H 0.6272 0.6997 0.3233 0.049 Uiso 1 1 calc R . . C9 C 0.3182(4) 0.7177(2) 0.1902(2) 0.0199(10) Uani 1 1 d . . . H9A H 0.3264 0.6592 0.1970 0.024 Uiso 1 1 calc R . . H9B H 0.3285 0.7407 0.2486 0.024 Uiso 1 1 calc R . . C10 C 0.1384(4) 0.6021(2) 0.0893(2) 0.0197(10) Uani 1 1 d . . . C11 C 0.1771(4) 0.5226(2) 0.0009(3) 0.0213(10) Uani 1 1 d . . . C12 C 0.2085(4) 0.4866(2) -0.0631(3) 0.0264(11) Uani 1 1 d . . . H12A H 0.2287 0.5173 -0.1038 0.032 Uiso 1 1 calc R . . C13 C 0.2092(4) 0.4045(2) -0.0653(3) 0.0308(12) Uani 1 1 d . . . H13A H 0.2301 0.3785 -0.1086 0.037 Uiso 1 1 calc R . . C14 C 0.1800(4) 0.3584(2) -0.0056(3) 0.0307(12) Uani 1 1 d . . . H14A H 0.1823 0.3020 -0.0089 0.037 Uiso 1 1 calc R . . C15 C 0.1479(4) 0.3933(2) 0.0580(3) 0.0251(11) Uani 1 1 d . . . H15A H 0.1269 0.3625 0.0983 0.030 Uiso 1 1 calc R . . C16 C 0.1480(4) 0.4759(2) 0.0599(3) 0.0204(10) Uani 1 1 d . . . C17 C 0.0943(4) 0.5061(2) 0.1912(3) 0.0284(12) Uani 1 1 d . . . H17A H 0.0816 0.5543 0.2201 0.043 Uiso 1 1 calc R . . H17B H 0.1576 0.4753 0.2338 0.043 Uiso 1 1 calc R . . H17C H 0.0241 0.4738 0.1703 0.043 Uiso 1 1 calc R . . C18 C 0.1216(4) 0.6772(2) 0.1324(3) 0.0226(11) Uani 1 1 d . . . H18A H 0.0416 0.6967 0.1021 0.027 Uiso 1 1 calc R . . H18B H 0.1355 0.6672 0.1954 0.027 Uiso 1 1 calc R . . C19 C 0.0667(4) 0.8448(2) 0.0680(3) 0.0206(11) Uani 1 1 d . . . C20 C -0.0596(4) 0.8588(2) -0.0659(3) 0.0232(11) Uani 1 1 d . . . C21 C -0.1273(4) 0.8558(2) -0.1569(3) 0.0297(12) Uani 1 1 d . . . H21A H -0.1090 0.8205 -0.1950 0.036 Uiso 1 1 calc R . . C22 C -0.2207(5) 0.9055(3) -0.1890(3) 0.0348(12) Uani 1 1 d . . . H22A H -0.2680 0.9037 -0.2505 0.042 Uiso 1 1 calc R . . C23 C -0.2485(4) 0.9586(2) -0.1349(3) 0.0330(12) Uani 1 1 d . . . H23A H -0.3137 0.9922 -0.1600 0.040 Uiso 1 1 calc R . . C24 C -0.1830(4) 0.9631(2) -0.0458(3) 0.0284(12) Uani 1 1 d . . . H24A H -0.2016 0.9993 -0.0085 0.034 Uiso 1 1 calc R . . C25 C -0.0883(4) 0.9126(2) -0.0119(3) 0.0219(11) Uani 1 1 d . . . C26 C 0.0004(4) 0.9488(2) 0.1495(3) 0.0259(11) Uani 1 1 d . . . H26A H 0.0652 0.9300 0.2019 0.039 Uiso 1 1 calc R . . H26B H -0.0712 0.9430 0.1595 0.039 Uiso 1 1 calc R . . H26C H 0.0120 1.0049 0.1388 0.039 Uiso 1 1 calc R . . C27 C 0.1692(4) 0.8168(2) 0.1449(3) 0.0206(10) Uani 1 1 d . . . H27A H 0.2337 0.8546 0.1562 0.025 Uiso 1 1 calc R . . H27B H 0.1509 0.8146 0.1987 0.025 Uiso 1 1 calc R . . C28 C 0.4385(5) 0.5058(3) 0.3528(4) 0.0543(17) Uani 1 1 d . . . H28A H 0.4255 0.4631 0.3888 0.081 Uiso 1 1 calc R . . H28B H 0.3754 0.5443 0.3374 0.081 Uiso 1 1 calc R . . H28C H 0.5115 0.5325 0.3866 0.081 Uiso 1 1 calc R . . C29 C 0.4433(5) 0.4713(3) 0.2699(3) 0.0476(15) Uani 1 1 d . . . H29A H 0.5062 0.4317 0.2851 0.057 Uiso 1 1 calc R . . H29B H 0.3699 0.4441 0.2355 0.057 Uiso 1 1 calc R . . C30 C 0.4903(5) 0.5025(3) 0.1477(3) 0.0504(16) Uani 1 1 d . . . H30A H 0.4288 0.4660 0.1108 0.060 Uiso 1 1 calc R . . H30B H 0.5634 0.4723 0.1718 0.060 Uiso 1 1 calc R . . C31 C 0.5018(5) 0.5705(3) 0.0929(3) 0.0503(15) Uani 1 1 d . . . H31A H 0.5227 0.5502 0.0447 0.075 Uiso 1 1 calc R . . H31B H 0.5619 0.6067 0.1302 0.075 Uiso 1 1 calc R . . H31C H 0.4284 0.5990 0.0679 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.32548(11) 0.66637(6) -0.11628(7) 0.0310(3) Uani 1 1 d . . . Cl2 Cl 0.01701(11) 0.69245(6) -0.18929(7) 0.0303(3) Uani 1 1 d . . . Cl1 Cl 0.21361(12) 0.87570(6) -0.11213(8) 0.0414(3) Uani 1 1 d . . . O1 O 0.4628(3) 0.53335(18) 0.2184(2) 0.0454(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02094(16) 0.02315(11) 0.01449(10) 0.00002(9) 0.00731(10) -0.00087(11) N1 0.021(3) 0.0313(18) 0.0137(17) -0.0012(14) 0.0044(19) -0.0092(17) N2 0.023(3) 0.0260(18) 0.0142(17) 0.0020(13) 0.006(2) 0.0008(16) N3 0.020(3) 0.0250(18) 0.0176(18) 0.0006(13) 0.010(2) 0.0000(16) N4 0.023(3) 0.0229(18) 0.0151(17) 0.0014(13) 0.009(2) -0.0022(16) N5 0.016(3) 0.0234(18) 0.0185(18) -0.0016(14) 0.004(2) -0.0033(16) N6 0.023(3) 0.0200(18) 0.0208(19) 0.0002(14) 0.012(2) -0.0005(16) N7 0.018(3) 0.0202(16) 0.0163(16) -0.0010(13) 0.0086(18) -0.0026(16) C1 0.016(3) 0.020(2) 0.017(2) 0.0032(15) 0.000(2) -0.0009(18) C2 0.019(3) 0.031(2) 0.021(2) -0.0005(17) 0.008(3) -0.005(2) C3 0.031(4) 0.039(3) 0.020(2) -0.0010(18) 0.009(3) -0.006(2) C4 0.024(4) 0.044(3) 0.024(3) -0.0029(19) 0.011(3) -0.010(2) C5 0.020(4) 0.032(2) 0.040(3) -0.007(2) 0.014(3) -0.008(2) C6 0.026(4) 0.028(2) 0.024(2) -0.0004(18) 0.006(3) 0.000(2) C7 0.018(3) 0.023(2) 0.017(2) -0.0031(16) 0.005(2) -0.0013(18) C8 0.032(4) 0.048(3) 0.017(2) 0.0049(19) 0.009(3) 0.002(2) C9 0.024(3) 0.024(2) 0.013(2) 0.0014(15) 0.008(2) -0.0011(19) C10 0.014(3) 0.025(2) 0.018(2) -0.0005(16) 0.003(2) -0.0052(19) C11 0.021(3) 0.020(2) 0.022(2) -0.0001(17) 0.007(2) -0.0008(19) C12 0.021(4) 0.036(3) 0.024(2) -0.0019(18) 0.011(3) -0.004(2) C13 0.034(4) 0.030(3) 0.034(3) -0.0106(19) 0.019(3) -0.001(2) C14 0.031(4) 0.024(2) 0.034(3) -0.0043(19) 0.008(3) -0.002(2) C15 0.026(3) 0.021(2) 0.028(2) 0.0038(17) 0.009(3) -0.0028(19) C16 0.020(3) 0.021(2) 0.020(2) -0.0019(16) 0.007(2) -0.0016(19) C17 0.037(4) 0.032(2) 0.022(2) -0.0014(17) 0.017(3) -0.011(2) C18 0.022(3) 0.028(2) 0.022(2) -0.0001(17) 0.014(3) -0.001(2) C19 0.024(3) 0.021(2) 0.020(2) -0.0009(16) 0.012(2) -0.005(2) C20 0.024(4) 0.026(2) 0.020(2) 0.0001(17) 0.008(3) -0.003(2) C21 0.027(4) 0.030(2) 0.028(3) -0.0012(19) 0.006(3) -0.004(2) C22 0.024(4) 0.042(3) 0.030(3) 0.001(2) 0.000(3) -0.002(2) C23 0.018(4) 0.036(3) 0.039(3) 0.012(2) 0.003(3) 0.008(2) C24 0.022(4) 0.028(2) 0.038(3) 0.0028(19) 0.014(3) 0.000(2) C25 0.019(3) 0.022(2) 0.028(2) 0.0031(17) 0.013(3) -0.0017(19) C26 0.028(4) 0.026(2) 0.026(2) -0.0025(17) 0.012(3) 0.002(2) C27 0.021(3) 0.024(2) 0.018(2) -0.0005(16) 0.009(2) 0.0004(19) C28 0.056(5) 0.047(3) 0.075(4) -0.006(3) 0.042(4) 0.000(3) C29 0.042(5) 0.039(3) 0.063(4) 0.005(2) 0.020(4) -0.004(3) C30 0.052(5) 0.056(3) 0.037(3) -0.013(2) 0.010(3) 0.009(3) C31 0.047(5) 0.053(3) 0.047(3) -0.007(3) 0.014(4) -0.001(3) Cl3 0.0331(9) 0.0354(6) 0.0282(6) 0.0002(4) 0.0158(7) 0.0021(5) Cl2 0.0300(9) 0.0347(6) 0.0231(6) -0.0078(4) 0.0067(6) -0.0046(5) Cl1 0.0432(10) 0.0375(6) 0.0485(8) 0.0150(5) 0.0231(8) 0.0043(6) O1 0.054(3) 0.0389(18) 0.044(2) 0.0000(15) 0.021(2) 0.0012(17) _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 Eu1 N1 2.525(4) . ? Eu1 N3 2.554(3) . ? Eu1 N5 2.554(3) . ? Eu1 Cl1 2.6343(10) . ? Eu1 Cl3 2.6606(10) . ? Eu1 Cl2 2.6726(12) . ? Eu1 N7 2.716(3) . ? N1 C1 1.332(5) . ? N1 C2 1.396(5) . ? N2 C1 1.333(5) . ? N2 C7 1.400(5) . ? N2 C8 1.475(5) . ? N3 C10 1.322(4) . ? N3 C11 1.401(5) . ? N4 C10 1.342(4) . ? N4 C16 1.380(4) . ? N4 C17 1.470(4) . ? N5 C19 1.332(5) . ? N5 C20 1.399(5) . ? N6 C19 1.351(5) . ? N6 C25 1.382(5) . ? N6 C26 1.454(4) . ? N7 C9 1.462(5) . ? N7 C18 1.471(5) . ? N7 C27 1.475(4) . ? C1 C9 1.488(5) . ? C2 C7 1.393(6) . ? C2 C3 1.407(5) . ? C3 C4 1.377(6) . ? C3 H3A 0.9500 . ? C4 C5 1.397(6) . ? C4 H4A 0.9500 . ? C5 C6 1.385(5) . ? C5 H5A 0.9500 . ? C6 C7 1.381(6) . ? C6 H6A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C18 1.498(5) . ? C11 C12 1.388(5) . ? C11 C16 1.395(5) . ? C12 C13 1.380(6) . ? C12 H12A 0.9500 . ? C13 C14 1.399(5) . ? C13 H13A 0.9500 . ? C14 C15 1.381(5) . ? C14 H14A 0.9500 . ? C15 C16 1.389(5) . ? C15 H15A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C27 1.489(6) . ? C20 C21 1.401(6) . ? C20 C25 1.402(5) . ? C21 C22 1.371(6) . ? C21 H21A 0.9500 . ? C22 C23 1.392(6) . ? C22 H22A 0.9500 . ? C23 C24 1.371(6) . ? C23 H23A 0.9500 . ? C24 C25 1.393(6) . ? C24 H24A 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.493(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O1 1.418(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O1 1.423(5) . ? C30 C31 1.491(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 N1 Eu1 N3 95.42(11) . . ? N1 Eu1 N5 108.81(10) . . ? N3 Eu1 N5 99.39(10) . . ? N1 Eu1 Cl1 85.93(8) . . ? N3 Eu1 Cl1 178.62(9) . . ? N5 Eu1 Cl1 79.88(7) . . ? N1 Eu1 Cl3 82.21(8) . . ? N3 Eu1 Cl3 88.79(7) . . ? N5 Eu1 Cl3 165.38(8) . . ? Cl1 Eu1 Cl3 91.67(3) . . ? N1 Eu1 Cl2 167.66(7) . . ? N3 Eu1 Cl2 85.84(8) . . ? N5 Eu1 Cl2 83.01(8) . . ? Cl1 Eu1 Cl2 92.89(4) . . ? Cl3 Eu1 Cl2 85.55(4) . . ? N1 Eu1 N7 63.69(10) . . ? N3 Eu1 N7 63.14(9) . . ? N5 Eu1 N7 63.10(10) . . ? Cl1 Eu1 N7 117.37(7) . . ? Cl3 Eu1 N7 131.48(8) . . ? Cl2 Eu1 N7 126.99(8) . . ? C1 N1 C2 104.0(4) . . ? C1 N1 Eu1 120.3(3) . . ? C2 N1 Eu1 134.3(2) . . ? C1 N2 C7 107.6(3) . . ? C1 N2 C8 127.1(3) . . ? C7 N2 C8 125.3(4) . . ? C10 N3 C11 104.6(3) . . ? C10 N3 Eu1 118.6(2) . . ? C11 N3 Eu1 136.8(2) . . ? C10 N4 C16 106.9(3) . . ? C10 N4 C17 127.7(3) . . ? C16 N4 C17 125.3(3) . . ? C19 N5 C20 104.9(3) . . ? C19 N5 Eu1 116.7(3) . . ? C20 N5 Eu1 135.5(2) . . ? C19 N6 C25 107.3(3) . . ? C19 N6 C26 128.1(4) . . ? C25 N6 C26 124.5(3) . . ? C9 N7 C18 108.7(3) . . ? C9 N7 C27 109.7(3) . . ? C18 N7 C27 109.8(3) . . ? C9 N7 Eu1 112.1(2) . . ? C18 N7 Eu1 108.4(2) . . ? C27 N7 Eu1 108.1(2) . . ? N1 C1 N2 113.5(4) . . ? N1 C1 C9 122.5(4) . . ? N2 C1 C9 123.9(3) . . ? C7 C2 N1 110.5(3) . . ? C7 C2 C3 119.6(4) . . ? N1 C2 C3 129.9(4) . . ? C4 C3 C2 117.1(4) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? C3 C4 C5 122.3(4) . . ? C3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C7 C6 C5 116.2(4) . . ? C7 C6 H6A 121.9 . . ? C5 C6 H6A 121.9 . . ? C6 C7 C2 123.6(4) . . ? C6 C7 N2 132.1(4) . . ? C2 C7 N2 104.3(4) . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N7 C9 C1 110.9(3) . . ? N7 C9 H9A 109.5 . . ? C1 C9 H9A 109.5 . . ? N7 C9 H9B 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N3 C10 N4 113.6(3) . . ? N3 C10 C18 121.9(3) . . ? N4 C10 C18 124.5(3) . . ? C12 C11 C16 120.0(3) . . ? C12 C11 N3 131.1(3) . . ? C16 C11 N3 108.9(3) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 H12A 121.2 . . ? C11 C12 H12A 121.2 . . ? C12 C13 C14 122.0(4) . . ? C12 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C14 C15 C16 116.3(3) . . ? C14 C15 H15A 121.9 . . ? C16 C15 H15A 121.9 . . ? N4 C16 C15 131.0(3) . . ? N4 C16 C11 106.0(3) . . ? C15 C16 C11 123.1(3) . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C10 108.3(3) . . ? N7 C18 H18A 110.0 . . ? C10 C18 H18A 110.0 . . ? N7 C18 H18B 110.0 . . ? C10 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? N5 C19 N6 112.9(4) . . ? N5 C19 C27 122.8(4) . . ? N6 C19 C27 124.3(3) . . ? N5 C20 C21 131.5(4) . . ? N5 C20 C25 109.1(4) . . ? C21 C20 C25 119.4(4) . . ? C22 C21 C20 117.9(4) . . ? C22 C21 H21A 121.0 . . ? C20 C21 H21A 121.1 . . ? C21 C22 C23 122.3(4) . . ? C21 C22 H22A 118.9 . . ? C23 C22 H22A 118.9 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 117.5(4) . . ? C23 C24 H24A 121.2 . . ? C25 C24 H24A 121.2 . . ? N6 C25 C24 132.2(4) . . ? N6 C25 C20 105.8(4) . . ? C24 C25 C20 122.0(4) . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C19 109.6(3) . . ? N7 C27 H27A 109.7 . . ? C19 C27 H27A 109.7 . . ? N7 C27 H27B 109.7 . . ? C19 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 C28 109.1(4) . . ? O1 C29 H29A 109.9 . . ? C28 C29 H29A 109.9 . . ? O1 C29 H29B 109.9 . . ? C28 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O1 C30 C31 108.5(4) . . ? O1 C30 H30A 110.0 . . ? C31 C30 H30A 110.0 . . ? O1 C30 H30B 110.0 . . ? C31 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 O1 C30 111.3(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.685 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.099 #==================================# data_13 _database_code_depnum_ccdc_archive 'CCDC 698715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H59 Cl3 N15 O13 Tb' _chemical_formula_weight 1415.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.809(5) _cell_length_b 21.053(4) _cell_length_c 22.626(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6102(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 5 _cell_measurement_theta_max 12.5 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6249 _exptl_absorpt_correction_T_max 0.6391 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemense P4' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7940 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7677 _reflns_number_gt 5964 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+2.0984P] 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 geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00058(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(18) _refine_ls_number_reflns 7677 _refine_ls_number_parameters 785 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.011 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 Tb1 Tb 0.37290(3) 0.801710(14) 0.283440(14) 0.02779(6) Uani 1 1 d . . . N1 N 0.5504(4) 0.8500(3) 0.3293(3) 0.0322(15) Uani 1 1 d . . . N2 N 0.1983(5) 0.7555(3) 0.2374(2) 0.0354(16) Uani 1 1 d . . . N11 N 0.4943(4) 0.7257(3) 0.3272(2) 0.0300(15) Uani 1 1 d . . . N12 N 0.5722(4) 0.6989(3) 0.4115(2) 0.0349(14) Uani 1 1 d . . . C11 C 0.5789(6) 0.8134(3) 0.3823(3) 0.0384(19) Uani 1 1 d . . . H11A H 0.5408 0.8297 0.4155 0.080 Uiso 1 1 d R . . H11B H 0.6522 0.8177 0.3901 0.080 Uiso 1 1 d R . . C12 C 0.5499(6) 0.7447(3) 0.3735(3) 0.0314(18) Uani 1 1 d . . . C13 C 0.5304(6) 0.6434(3) 0.3892(4) 0.038(2) Uani 1 1 d . . . C14 C 0.5276(7) 0.5807(3) 0.4110(4) 0.051(2) Uani 1 1 d . . . H14A H 0.5593 0.5695 0.4480 0.080 Uiso 1 1 d R . . C15 C 0.4792(7) 0.5375(4) 0.3782(4) 0.053(3) Uani 1 1 d . . . H15A H 0.4779 0.4944 0.3920 0.080 Uiso 1 1 d R . . C16 C 0.4280(7) 0.5522(4) 0.3230(4) 0.057(3) Uani 1 1 d . . . H16A H 0.3914 0.5196 0.3017 0.080 Uiso 1 1 d R . . C17 C 0.4325(6) 0.6146(3) 0.3022(3) 0.039(2) Uani 1 1 d . . . H17A H 0.4025 0.6258 0.2647 0.080 Uiso 1 1 d R . . C18 C 0.4822(5) 0.6591(3) 0.3356(3) 0.0319(18) Uani 1 1 d . . . C19 C 0.6270(7) 0.7057(4) 0.4673(3) 0.053(2) Uani 1 1 d . . . H19A H 0.6472 0.7492 0.4726 0.080 Uiso 1 1 d R . . H19B H 0.5827 0.6928 0.4993 0.080 Uiso 1 1 d R . . H19C H 0.6883 0.6794 0.4666 0.080 Uiso 1 1 d R . . N21 N 0.3522(5) 0.8793(2) 0.3641(2) 0.0338(16) Uani 1 1 d . . . N22 N 0.3909(6) 0.9789(3) 0.3927(3) 0.048(2) Uani 1 1 d . . . C21 C 0.5326(6) 0.9173(3) 0.3447(4) 0.041(2) Uani 1 1 d . . . H21A H 0.5423 0.9440 0.3108 0.080 Uiso 1 1 d R . . H21B H 0.5814 0.9299 0.3747 0.080 Uiso 1 1 d R . . C22 C 0.4243(7) 0.9236(3) 0.3677(3) 0.042(2) Uani 1 1 d . . . C23 C 0.2846(8) 0.9685(4) 0.4050(3) 0.049(2) Uani 1 1 d . . . C24 C 0.2096(9) 1.0084(5) 0.4289(4) 0.072(3) Uani 1 1 d . . . H24A H 0.2273 1.0505 0.4418 0.080 Uiso 1 1 d R . . C25 C 0.1111(9) 0.9837(5) 0.4347(4) 0.076(3) Uani 1 1 d . . . H25A H 0.0561 1.0100 0.4499 0.080 Uiso 1 1 d R . . C26 C 0.0893(7) 0.9205(4) 0.4172(4) 0.059(3) Uani 1 1 d . . . H26A H 0.0192 0.9048 0.4212 0.080 Uiso 1 1 d R . . C27 C 0.1624(6) 0.8828(4) 0.3951(3) 0.051(2) Uani 1 1 d . . . H27A H 0.1468 0.8397 0.3845 0.080 Uiso 1 1 d R . . C28 C 0.2635(7) 0.9061(4) 0.3884(3) 0.043(2) Uani 1 1 d . . . C29 C 0.4502(9) 1.0363(4) 0.4028(5) 0.085(4) Uani 1 1 d . . . H29A H 0.5213 1.0299 0.3909 0.080 Uiso 1 1 d R . . H29B H 0.4200 1.0699 0.3799 0.080 Uiso 1 1 d R . . H29C H 0.4482 1.0474 0.4440 0.080 Uiso 1 1 d R . . N31 N 0.4891(4) 0.8605(2) 0.2146(3) 0.0356(15) Uani 1 1 d . . . N32 N 0.6478(5) 0.8641(3) 0.1761(3) 0.0438(18) Uani 1 1 d . . . C31 C 0.6347(5) 0.8447(3) 0.2857(3) 0.0436(18) Uani 1 1 d . . . H31A H 0.6642 0.8028 0.2866 0.080 Uiso 1 1 d R . . H31B H 0.6887 0.8748 0.2947 0.080 Uiso 1 1 d R . . C32 C 0.5916(5) 0.8581(3) 0.2252(3) 0.0366(19) Uani 1 1 d . . . C33 C 0.5815(7) 0.8705(3) 0.1299(3) 0.043(2) Uani 1 1 d . . . C34 C 0.5972(7) 0.8766(4) 0.0696(4) 0.053(3) Uani 1 1 d . . . H34A H 0.6663 0.8756 0.0531 0.080 Uiso 1 1 d R . . C35 C 0.5106(8) 0.8824(4) 0.0351(4) 0.058(3) Uani 1 1 d . . . H35A H 0.5211 0.8856 -0.0068 0.080 Uiso 1 1 d R . . C36 C 0.4100(8) 0.8826(4) 0.0576(4) 0.067(3) Uani 1 1 d . . . H36A H 0.3524 0.8893 0.0311 0.080 Uiso 1 1 d R . . C37 C 0.3921(7) 0.8759(3) 0.1186(3) 0.050(2) Uani 1 1 d . . . H37A H 0.3233 0.8749 0.1353 0.080 Uiso 1 1 d R . . C38 C 0.4783(6) 0.8697(3) 0.1533(3) 0.0355(19) Uani 1 1 d . . . C39 C 0.7611(7) 0.8657(5) 0.1713(5) 0.091(4) Uani 1 1 d . . . H39A H 0.7916 0.8606 0.2097 0.080 Uiso 1 1 d R . . H39B H 0.7824 0.8311 0.1463 0.080 Uiso 1 1 d R . . H39C H 0.7840 0.9051 0.1543 0.080 Uiso 1 1 d R . . N41 N 0.2470(5) 0.8803(3) 0.2450(3) 0.0341(16) Uani 1 1 d . . . N42 N 0.0856(5) 0.9152(3) 0.2593(3) 0.0400(17) Uani 1 1 d . . . C41 C 0.1106(5) 0.7981(3) 0.2530(3) 0.0365(17) Uani 1 1 d . . . H41A H 0.0851 0.7880 0.2918 0.080 Uiso 1 1 d R . . H41B H 0.0548 0.7922 0.2252 0.080 Uiso 1 1 d R . . C42 C 0.1470(6) 0.8643(3) 0.2516(3) 0.037(2) Uani 1 1 d . . . C43 C 0.1481(6) 0.9681(4) 0.2569(3) 0.043(2) Uani 1 1 d . . . C44 C 0.1246(8) 1.0320(4) 0.2613(4) 0.053(2) Uani 1 1 d . . . H44A H 0.0549 1.0468 0.2685 0.080 Uiso 1 1 d R . . C45 C 0.2082(7) 1.0740(4) 0.2543(5) 0.062(3) Uani 1 1 d . . . H45A H 0.1960 1.1189 0.2561 0.080 Uiso 1 1 d R . . C46 C 0.3090(8) 1.0525(4) 0.2455(4) 0.061(3) Uani 1 1 d . . . H46A H 0.3639 1.0833 0.2418 0.080 Uiso 1 1 d R . . C47 C 0.3327(7) 0.9895(4) 0.2408(4) 0.047(2) Uani 1 1 d . . . H47A H 0.4026 0.9749 0.2336 0.080 Uiso 1 1 d R . . C48 C 0.2483(6) 0.9468(3) 0.2478(3) 0.038(2) Uani 1 1 d . . . C49 C -0.0293(6) 0.9169(4) 0.2679(4) 0.057(3) Uani 1 1 d . . . H49A H -0.0558 0.8742 0.2680 0.080 Uiso 1 1 d R . . H49B H -0.0453 0.9369 0.3049 0.080 Uiso 1 1 d R . . H49C H -0.0611 0.9404 0.2363 0.080 Uiso 1 1 d R . . N51 N 0.3931(5) 0.7322(3) 0.1977(2) 0.0375(16) Uani 1 1 d . . . N52 N 0.3521(5) 0.7194(3) 0.1025(2) 0.0413(18) Uani 1 1 d . . . C51 C 0.2088(6) 0.7512(4) 0.1713(3) 0.041(2) Uani 1 1 d . . . H51A H 0.1915 0.7911 0.1533 0.080 Uiso 1 1 d R . . H51B H 0.1623 0.7192 0.1564 0.080 Uiso 1 1 d R . . C52 C 0.3196(7) 0.7338(3) 0.1574(3) 0.039(2) Uani 1 1 d . . . C53 C 0.4588(7) 0.7108(3) 0.1071(3) 0.044(2) Uani 1 1 d . . . C54 C 0.5334(7) 0.7008(4) 0.0636(3) 0.053(2) Uani 1 1 d . . . H54A H 0.5145 0.6982 0.0226 0.080 Uiso 1 1 d R . . C55 C 0.6352(8) 0.6946(4) 0.0817(4) 0.064(3) Uani 1 1 d . . . H55A H 0.6892 0.6878 0.0530 0.080 Uiso 1 1 d R . . C56 C 0.6622(7) 0.6992(4) 0.1410(4) 0.061(3) Uani 1 1 d . . . H56A H 0.7339 0.6933 0.1521 0.080 Uiso 1 1 d R . . C57 C 0.5884(6) 0.7099(3) 0.1847(4) 0.046(2) Uani 1 1 d . . . H57A H 0.6071 0.7131 0.2256 0.080 Uiso 1 1 d R . . C58 C 0.4859(7) 0.7165(3) 0.1665(3) 0.037(2) Uani 1 1 d . . . C59 C 0.2888(8) 0.7193(5) 0.0502(4) 0.072(3) Uani 1 1 d . . . H59A H 0.2170 0.7262 0.0605 0.080 Uiso 1 1 d R . . H59B H 0.3118 0.7525 0.0242 0.080 Uiso 1 1 d R . . H59C H 0.2955 0.6790 0.0306 0.080 Uiso 1 1 d R . . N61 N 0.2649(5) 0.7351(3) 0.3504(3) 0.0348(16) Uani 1 1 d . . . N62 N 0.1907(5) 0.6402(3) 0.3615(3) 0.0439(18) Uani 1 1 d . . . C61 C 0.1786(6) 0.6909(3) 0.2622(3) 0.040(2) Uani 1 1 d . . . H61A H 0.2180 0.6601 0.2403 0.080 Uiso 1 1 d R . . H61B H 0.1058 0.6809 0.2586 0.080 Uiso 1 1 d R . . C62 C 0.2093(5) 0.6894(4) 0.3261(3) 0.0386(19) Uani 1 1 d . . . C63 C 0.2369(6) 0.6546(4) 0.4144(4) 0.043(2) Uani 1 1 d . . . C64 C 0.2464(8) 0.6196(4) 0.4665(4) 0.065(3) Uani 1 1 d . . . H64A H 0.2137 0.5788 0.4706 0.080 Uiso 1 1 d R . . C65 C 0.3081(8) 0.6484(5) 0.5117(4) 0.069(3) Uani 1 1 d . . . H65A H 0.3203 0.6254 0.5476 0.080 Uiso 1 1 d R . . C66 C 0.3494(6) 0.7067(4) 0.5048(4) 0.057(3) Uani 1 1 d . . . H66A H 0.3854 0.7255 0.5377 0.080 Uiso 1 1 d R . . C67 C 0.3398(6) 0.7417(4) 0.4527(3) 0.043(2) Uani 1 1 d . . . H67A H 0.3710 0.7829 0.4484 0.080 Uiso 1 1 d R . . C68 C 0.2842(5) 0.7134(3) 0.4073(3) 0.034(2) Uani 1 1 d . . . C69 C 0.1338(9) 0.5830(4) 0.3451(5) 0.073(3) Uani 1 1 d . . . H69A H 0.1099 0.5862 0.3050 0.080 Uiso 1 1 d R . . H69B H 0.1788 0.5467 0.3489 0.080 Uiso 1 1 d R . . H69C H 0.0749 0.5782 0.3710 0.080 Uiso 1 1 d R . . Cl1 Cl -0.1320(2) 0.73492(10) 0.32238(10) 0.0575(6) Uani 1 1 d . . . O11 O -0.2251(5) 0.7102(3) 0.3456(4) 0.105(3) Uani 1 1 d . . . O12 O -0.0528(6) 0.6939(5) 0.3326(4) 0.128(3) Uani 1 1 d . . . O13 O -0.1132(8) 0.7941(4) 0.3475(3) 0.125(3) Uani 1 1 d . . . O14 O -0.1403(7) 0.7441(4) 0.2611(3) 0.104(3) Uani 1 1 d . . . Cl2 Cl 0.2294(2) 0.53277(13) 0.16354(17) 0.0913(10) Uani 1 1 d . . . O21 O 0.3036(8) 0.5769(5) 0.1583(6) 0.168(5) Uani 1 1 d . . . O22 O 0.1342(8) 0.5567(4) 0.1787(5) 0.158(5) Uani 1 1 d D . . O23 O 0.2594(9) 0.4965(7) 0.2225(6) 0.194(5) Uani 1 1 d . . . O24 O 0.2279(9) 0.4886(5) 0.1228(5) 0.169(5) Uani 1 1 d . . . Cl3 Cl 0.03004(17) 0.89218(11) 0.08854(10) 0.0951(11) Uani 1 1 d D A 1 O31 O 0.0196(9) 0.9188(4) 0.03131(18) 0.174(12) Uiso 0.40 1 d PD A 1 O32 O -0.0379(4) 0.8404(2) 0.0968(5) 0.177(10) Uiso 0.50 1 d PD A 1 O33 O 0.1348(3) 0.8732(4) 0.0980(5) 0.28(3) Uiso 0.30 1 d PD A 1 O31' O -0.0547(4) 0.8893(5) 0.0481(3) 0.185(9) Uiso 0.60 1 d PD B 2 O32' O 0.0330(9) 0.8350(2) 0.1217(3) 0.200(11) Uiso 0.50 1 d PD C 2 O33' O 0.1245(3) 0.9027(5) 0.0588(3) 0.182(7) Uiso 0.70 1 d PD D 2 O34 O 0.0064(6) 0.9424(3) 0.1302(3) 0.221(7) Uiso 1 1 d D . . N1W N 0.4533(12) 0.8863(6) 0.5081(5) 0.135(5) Uani 1 1 d . . . C1W C 0.4059(9) 0.9086(6) 0.5414(5) 0.079(4) Uani 1 1 d . . . C2W C 0.3350(9) 0.9329(6) 0.5852(6) 0.103(5) Uani 1 1 d . . . H2WA H 0.3590 0.9742 0.5968 0.080 Uiso 1 1 d R . . H2WB H 0.2653 0.9360 0.5699 0.080 Uiso 1 1 d R . . H2WC H 0.3355 0.9051 0.6188 0.080 Uiso 1 1 d R . . O1W O -0.0607(17) 0.6714(10) 0.1185(9) 0.140(7) Uiso 0.50 1 d P E 1 O1W' O 0.031(2) 0.6570(10) 0.1068(12) 0.244(14) Uiso 0.50 1 d PD F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02664(12) 0.02567(11) 0.03108(12) -0.00055(16) 0.00071(17) -0.00040(17) N1 0.024(3) 0.033(3) 0.039(3) -0.001(3) 0.002(3) -0.004(3) N2 0.038(3) 0.033(3) 0.035(3) 0.000(3) -0.004(3) 0.002(3) N11 0.030(3) 0.027(3) 0.033(3) 0.007(3) -0.005(3) 0.001(3) N12 0.030(3) 0.039(3) 0.036(3) 0.016(3) -0.001(3) -0.002(3) C11 0.032(3) 0.046(4) 0.038(4) 0.013(4) -0.009(3) -0.006(4) C12 0.029(3) 0.037(4) 0.029(3) -0.008(3) 0.008(3) 0.001(3) C13 0.031(4) 0.029(4) 0.054(5) -0.003(4) 0.007(4) -0.002(3) C14 0.057(5) 0.033(4) 0.063(5) 0.022(4) -0.002(5) 0.007(4) C15 0.062(6) 0.033(4) 0.065(6) 0.007(4) 0.005(5) 0.008(4) C16 0.045(5) 0.037(4) 0.089(7) 0.002(5) 0.023(5) 0.000(4) C17 0.039(4) 0.036(4) 0.043(4) -0.012(3) -0.006(4) 0.002(4) C18 0.026(3) 0.027(3) 0.043(4) 0.007(3) 0.007(3) 0.008(3) C19 0.065(5) 0.056(4) 0.039(4) 0.008(4) -0.012(5) -0.021(6) N21 0.037(4) 0.026(3) 0.038(3) -0.002(3) 0.007(3) 0.007(3) N22 0.063(5) 0.036(3) 0.047(3) -0.009(3) 0.003(4) 0.003(4) C21 0.040(4) 0.030(4) 0.052(5) -0.007(4) 0.015(4) -0.003(4) C22 0.058(5) 0.032(4) 0.036(4) -0.005(3) 0.003(4) 0.009(4) C23 0.074(6) 0.042(4) 0.032(4) -0.004(4) 0.006(5) 0.017(5) C24 0.093(8) 0.054(5) 0.070(6) -0.012(5) 0.018(6) 0.026(6) C25 0.076(7) 0.083(6) 0.068(6) 0.009(5) 0.019(6) 0.043(6) C26 0.054(5) 0.073(6) 0.049(5) 0.013(5) 0.010(4) 0.023(5) C27 0.051(5) 0.061(5) 0.041(4) 0.006(4) 0.021(4) 0.013(4) C28 0.055(5) 0.053(5) 0.020(3) 0.006(4) 0.006(4) 0.013(4) C29 0.103(8) 0.044(5) 0.108(8) -0.040(5) 0.028(8) -0.011(6) N31 0.034(3) 0.030(3) 0.044(3) -0.002(3) 0.000(4) -0.001(3) N32 0.035(4) 0.041(3) 0.055(4) 0.005(3) 0.012(3) 0.005(3) C31 0.028(3) 0.048(4) 0.055(4) 0.002(4) 0.018(5) 0.000(4) C32 0.026(3) 0.039(4) 0.045(4) -0.003(4) 0.008(3) -0.003(3) C33 0.053(5) 0.032(4) 0.043(4) 0.010(4) 0.006(4) 0.007(4) C34 0.058(6) 0.043(4) 0.059(5) 0.008(4) 0.018(5) -0.006(4) C35 0.090(7) 0.049(5) 0.035(4) 0.006(4) 0.006(5) 0.001(6) C36 0.082(7) 0.071(6) 0.047(5) 0.015(5) -0.014(5) 0.000(6) C37 0.065(6) 0.036(4) 0.048(4) 0.013(4) -0.006(5) 0.002(4) C38 0.042(4) 0.027(3) 0.037(4) 0.001(3) 0.004(4) 0.002(3) C39 0.034(5) 0.104(8) 0.135(10) 0.046(8) 0.035(6) 0.005(6) N41 0.030(3) 0.029(3) 0.043(3) -0.001(3) -0.002(3) -0.001(3) N42 0.038(3) 0.036(3) 0.046(3) 0.005(3) -0.001(3) 0.004(3) C41 0.028(3) 0.035(3) 0.047(4) -0.001(4) 0.001(3) -0.007(4) C42 0.033(4) 0.044(4) 0.033(4) 0.010(3) -0.011(3) -0.002(3) C43 0.041(5) 0.043(4) 0.044(4) 0.007(4) -0.001(4) 0.012(4) C44 0.048(4) 0.051(4) 0.061(5) -0.005(4) 0.004(5) 0.019(5) C45 0.064(6) 0.025(4) 0.098(7) 0.007(5) -0.002(6) 0.001(4) C46 0.068(6) 0.036(4) 0.080(6) 0.004(5) -0.008(6) -0.006(5) C47 0.049(5) 0.035(4) 0.056(5) 0.004(4) -0.008(4) -0.009(4) C48 0.051(5) 0.028(4) 0.034(4) 0.010(3) 0.002(4) 0.000(4) C49 0.030(4) 0.061(5) 0.079(7) 0.000(5) 0.000(4) 0.002(4) N51 0.036(3) 0.040(3) 0.036(3) 0.006(3) 0.002(3) 0.000(3) N52 0.058(4) 0.040(3) 0.025(3) -0.003(3) 0.000(3) 0.002(3) C51 0.037(4) 0.047(4) 0.038(4) -0.008(4) -0.012(4) -0.006(4) C52 0.055(5) 0.025(3) 0.038(4) 0.002(3) 0.003(4) -0.008(4) C53 0.073(5) 0.021(4) 0.039(4) -0.002(3) -0.004(4) -0.013(4) C54 0.092(6) 0.033(4) 0.035(4) 0.012(4) 0.009(4) 0.013(6) C55 0.092(6) 0.044(4) 0.056(4) 0.011(4) 0.030(5) 0.030(6) C56 0.057(5) 0.045(4) 0.080(6) 0.000(6) 0.026(5) 0.006(5) C57 0.049(4) 0.036(4) 0.053(5) -0.005(4) 0.001(4) -0.003(4) C58 0.053(5) 0.034(4) 0.025(3) 0.003(3) 0.001(4) 0.006(4) C59 0.091(7) 0.084(7) 0.042(5) -0.011(5) -0.004(6) -0.009(7) N61 0.034(3) 0.032(3) 0.038(3) 0.008(3) 0.007(3) 0.004(3) N62 0.031(3) 0.033(3) 0.068(4) 0.003(3) 0.003(4) -0.002(3) C61 0.032(4) 0.037(4) 0.052(4) 0.001(4) -0.003(3) 0.000(4) C62 0.030(3) 0.035(4) 0.051(4) 0.008(4) 0.007(3) -0.005(4) C63 0.033(4) 0.041(4) 0.057(5) 0.006(4) 0.014(4) 0.005(4) C64 0.066(6) 0.056(5) 0.072(6) 0.017(5) 0.025(5) 0.006(5) C65 0.069(6) 0.097(7) 0.040(5) 0.017(5) 0.006(5) 0.035(6) C66 0.047(5) 0.074(6) 0.050(4) -0.007(5) 0.006(4) 0.016(5) C67 0.038(4) 0.056(5) 0.036(4) 0.005(4) 0.011(3) 0.012(4) C68 0.022(3) 0.044(4) 0.035(4) 0.005(3) 0.004(3) 0.012(3) C69 0.079(6) 0.039(4) 0.101(7) 0.014(5) 0.011(8) -0.008(6) Cl1 0.0520(11) 0.0514(11) 0.0691(13) 0.0071(11) 0.0139(14) 0.0017(13) O11 0.068(4) 0.083(5) 0.163(7) 0.030(5) 0.064(5) 0.004(4) O12 0.060(4) 0.141(6) 0.184(8) 0.076(7) 0.018(5) 0.045(5) O13 0.196(9) 0.088(5) 0.089(5) -0.022(5) 0.048(6) -0.049(7) O14 0.099(6) 0.141(7) 0.074(4) 0.018(5) -0.004(5) -0.016(6) Cl2 0.0613(16) 0.0675(15) 0.145(3) -0.0381(18) 0.0174(19) -0.0083(14) O21 0.128(8) 0.113(7) 0.263(13) -0.046(9) 0.067(9) -0.051(7) O22 0.095(6) 0.124(7) 0.256(12) -0.057(8) 0.007(9) 0.037(7) O23 0.164(9) 0.235(11) 0.184(11) -0.062(11) -0.041(11) 0.091(9) O24 0.146(9) 0.171(8) 0.191(9) -0.123(7) -0.025(9) 0.020(8) Cl3 0.131(3) 0.0910(19) 0.0631(16) 0.0097(16) -0.0129(19) -0.010(2) N1W 0.200(14) 0.115(9) 0.088(7) -0.017(7) -0.032(9) 0.011(10) C1W 0.087(8) 0.083(7) 0.068(6) 0.002(6) -0.019(6) -0.006(7) C2W 0.082(9) 0.093(8) 0.134(11) 0.030(8) -0.014(8) 0.008(7) _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 Tb1 N11 2.442(6) . ? Tb1 N51 2.443(6) . ? Tb1 N21 2.464(5) . ? Tb1 N41 2.469(6) . ? Tb1 N31 2.484(6) . ? Tb1 N61 2.485(6) . ? Tb1 N2 2.652(6) . ? Tb1 N1 2.697(6) . ? N1 C31 1.467(9) . ? N1 C11 1.471(9) . ? N1 C21 1.477(9) . ? N2 C41 1.480(9) . ? N2 C61 1.491(9) . ? N2 C51 1.505(9) . ? N11 C12 1.328(9) . ? N11 C18 1.422(8) . ? N12 C12 1.323(9) . ? N12 C13 1.382(9) . ? N12 C19 1.452(9) . ? C11 C12 1.506(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9601 . ? C13 C18 1.400(11) . ? C13 C14 1.409(10) . ? C14 C15 1.327(12) . ? C14 H14A 0.9600 . ? C15 C16 1.445(13) . ? C15 H15A 0.9600 . ? C16 C17 1.397(11) . ? C16 H16A 0.9599 . ? C17 C18 1.363(10) . ? C17 H17A 0.9599 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9599 . ? N21 C22 1.315(9) . ? N21 C28 1.383(10) . ? N22 C22 1.363(9) . ? N22 C23 1.407(12) . ? N22 C29 1.444(11) . ? C21 C22 1.487(11) . ? C21 H21A 0.9600 . ? C21 H21B 0.9599 . ? C23 C24 1.386(13) . ? C23 C28 1.393(11) . ? C24 C25 1.371(15) . ? C24 H24A 0.9601 . ? C25 C26 1.416(13) . ? C25 H25A 0.9599 . ? C26 C27 1.325(12) . ? C26 H26A 0.9600 . ? C27 C28 1.392(12) . ? C27 H27A 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9599 . ? C29 H29C 0.9600 . ? N31 C32 1.336(9) . ? N31 C38 1.408(10) . ? N32 C32 1.331(9) . ? N32 C33 1.353(10) . ? N32 C39 1.456(10) . ? C31 C32 1.501(10) . ? C31 H31A 0.9599 . ? C31 H31B 0.9600 . ? C33 C34 1.385(11) . ? C33 C38 1.424(11) . ? C34 C35 1.362(13) . ? C34 H34A 0.9600 . ? C35 C36 1.385(14) . ? C35 H35A 0.9599 . ? C36 C37 1.407(12) . ? C36 H36A 0.9600 . ? C37 C38 1.360(11) . ? C37 H37A 0.9600 . ? C39 H39A 0.9599 . ? C39 H39B 0.9600 . ? C39 H39C 0.9601 . ? N41 C42 1.333(9) . ? N41 C48 1.403(8) . ? N42 C42 1.340(9) . ? N42 C43 1.373(10) . ? N42 C49 1.485(9) . ? C41 C42 1.470(10) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C43 C48 1.375(11) . ? C43 C44 1.382(10) . ? C44 C45 1.397(12) . ? C44 H44A 0.9600 . ? C45 C46 1.383(13) . ? C45 H45A 0.9600 . ? C46 C47 1.364(11) . ? C46 H46A 0.9600 . ? C47 C48 1.415(11) . ? C47 H47A 0.9600 . ? C49 H49A 0.9601 . ? C49 H49B 0.9599 . ? C49 H49C 0.9601 . ? N51 C52 1.311(9) . ? N51 C58 1.422(10) . ? N52 C52 1.345(9) . ? N52 C53 1.382(11) . ? N52 C59 1.435(10) . ? C51 C52 1.499(11) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C53 C54 1.388(11) . ? C53 C58 1.394(10) . ? C54 C55 1.373(13) . ? C54 H54A 0.9601 . ? C55 C56 1.388(12) . ? C55 H55A 0.9599 . ? C56 C57 1.386(11) . ? C56 H56A 0.9600 . ? C57 C58 1.383(11) . ? C57 H57A 0.9601 . ? C59 H59A 0.9599 . ? C59 H59B 0.9599 . ? C59 H59C 0.9600 . ? N61 C62 1.317(9) . ? N61 C68 1.389(9) . ? N62 C62 1.331(9) . ? N62 C63 1.369(10) . ? N62 C69 1.456(10) . ? C61 C62 1.498(10) . ? C61 H61A 0.9599 . ? C61 H61B 0.9600 . ? C63 C68 1.388(10) . ? C63 C64 1.397(12) . ? C64 C65 1.426(13) . ? C64 H64A 0.9599 . ? C65 C66 1.345(13) . ? C65 H65A 0.9601 . ? C66 C67 1.396(11) . ? C66 H66A 0.9600 . ? C67 C68 1.385(10) . ? C67 H67A 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9601 . ? C69 H69C 0.9600 . ? Cl1 O12 1.353(8) . ? Cl1 O13 1.390(8) . ? Cl1 O11 1.403(7) . ? Cl1 O14 1.405(7) . ? Cl2 O24 1.310(10) . ? Cl2 O21 1.335(10) . ? Cl2 O22 1.363(10) . ? Cl2 O23 1.584(14) . ? Cl3 O32 1.407(4) . ? Cl3 O33 1.417(4) . ? Cl3 O31 1.417(4) . ? Cl3 O34 1.450(5) . ? N1W C1W 1.075(16) . ? C1W C2W 1.438(16) . ? C2W H2WA 0.9601 . ? C2W H2WB 0.9600 . ? C2W H2WC 0.9600 . ? 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 N11 Tb1 N51 82.09(19) . . ? N11 Tb1 N21 101.67(18) . . ? N51 Tb1 N21 175.24(18) . . ? N11 Tb1 N41 176.7(2) . . ? N51 Tb1 N41 101.01(19) . . ? N21 Tb1 N41 75.31(19) . . ? N11 Tb1 N31 101.50(19) . . ? N51 Tb1 N31 74.74(19) . . ? N21 Tb1 N31 101.49(19) . . ? N41 Tb1 N31 80.62(19) . . ? N11 Tb1 N61 74.78(19) . . ? N51 Tb1 N61 101.82(19) . . ? N21 Tb1 N61 82.11(19) . . ? N41 Tb1 N61 103.2(2) . . ? N31 Tb1 N61 175.38(18) . . ? N11 Tb1 N2 117.12(18) . . ? N51 Tb1 N2 63.76(19) . . ? N21 Tb1 N2 116.33(19) . . ? N41 Tb1 N2 63.69(18) . . ? N31 Tb1 N2 116.21(19) . . ? N61 Tb1 N2 64.05(19) . . ? N11 Tb1 N1 63.52(18) . . ? N51 Tb1 N1 116.21(18) . . ? N21 Tb1 N1 63.63(18) . . ? N41 Tb1 N1 115.69(18) . . ? N31 Tb1 N1 63.19(19) . . ? N61 Tb1 N1 116.59(19) . . ? N2 Tb1 N1 179.28(18) . . ? C31 N1 C11 109.0(5) . . ? C31 N1 C21 110.2(5) . . ? C11 N1 C21 110.3(6) . . ? C31 N1 Tb1 109.4(4) . . ? C11 N1 Tb1 109.0(4) . . ? C21 N1 Tb1 108.8(4) . . ? C41 N2 C61 109.5(5) . . ? C41 N2 C51 109.9(6) . . ? C61 N2 C51 109.5(6) . . ? C41 N2 Tb1 108.9(4) . . ? C61 N2 Tb1 109.3(4) . . ? C51 N2 Tb1 109.7(4) . . ? C12 N11 C18 104.5(6) . . ? C12 N11 Tb1 117.6(4) . . ? C18 N11 Tb1 129.0(5) . . ? C12 N12 C13 107.2(6) . . ? C12 N12 C19 126.7(6) . . ? C13 N12 C19 126.0(6) . . ? N1 C11 C12 109.5(6) . . ? N1 C11 H11A 109.0 . . ? C12 C11 H11A 108.7 . . ? N1 C11 H11B 110.2 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.6 . . ? N12 C12 N11 114.0(6) . . ? N12 C12 C11 124.2(6) . . ? N11 C12 C11 121.7(6) . . ? N12 C13 C18 106.6(6) . . ? N12 C13 C14 132.4(7) . . ? C18 C13 C14 121.0(7) . . ? C15 C14 C13 117.3(8) . . ? C15 C14 H14A 121.2 . . ? C13 C14 H14A 121.6 . . ? C14 C15 C16 123.2(8) . . ? C14 C15 H15A 118.3 . . ? C16 C15 H15A 118.5 . . ? C17 C16 C15 118.3(8) . . ? C17 C16 H16A 121.6 . . ? C15 C16 H16A 120.1 . . ? C18 C17 C16 118.6(7) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.7 . . ? C17 C18 C13 121.6(6) . . ? C17 C18 N11 130.9(7) . . ? C13 C18 N11 107.5(6) . . ? N12 C19 H19A 109.4 . . ? N12 C19 H19B 110.0 . . ? H19A C19 H19B 109.5 . . ? N12 C19 H19C 108.9 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 N21 C28 105.2(6) . . ? C22 N21 Tb1 116.2(5) . . ? C28 N21 Tb1 130.8(5) . . ? C22 N22 C23 104.6(6) . . ? C22 N22 C29 128.0(8) . . ? C23 N22 C29 127.4(7) . . ? N1 C21 C22 108.2(6) . . ? N1 C21 H21A 110.6 . . ? C22 C21 H21A 110.4 . . ? N1 C21 H21B 109.4 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.6 . . ? N21 C22 N22 114.3(7) . . ? N21 C22 C21 124.7(6) . . ? N22 C22 C21 120.9(7) . . ? C24 C23 C28 122.8(9) . . ? C24 C23 N22 130.8(8) . . ? C28 C23 N22 106.4(7) . . ? C25 C24 C23 116.5(9) . . ? C25 C24 H24A 122.5 . . ? C23 C24 H24A 120.9 . . ? C24 C25 C26 120.7(9) . . ? C24 C25 H25A 119.4 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 121.9(9) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 118.8 . . ? C26 C27 C28 119.2(8) . . ? C26 C27 H27A 120.8 . . ? C28 C27 H27A 119.9 . . ? N21 C28 C27 131.6(8) . . ? N21 C28 C23 109.4(7) . . ? C27 C28 C23 118.9(8) . . ? N22 C29 H29A 109.7 . . ? N22 C29 H29B 108.6 . . ? H29A C29 H29B 109.5 . . ? N22 C29 H29C 110.1 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 N31 C38 106.2(6) . . ? C32 N31 Tb1 117.2(5) . . ? C38 N31 Tb1 128.9(5) . . ? C32 N32 C33 108.4(6) . . ? C32 N32 C39 127.1(8) . . ? C33 N32 C39 124.5(8) . . ? N1 C31 C32 109.1(6) . . ? N1 C31 H31A 110.2 . . ? C32 C31 H31A 109.7 . . ? N1 C31 H31B 109.7 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.4 . . ? N32 C32 N31 112.1(7) . . ? N32 C32 C31 125.5(6) . . ? N31 C32 C31 122.2(7) . . ? N32 C33 C34 132.7(8) . . ? N32 C33 C38 107.1(6) . . ? C34 C33 C38 120.1(8) . . ? C35 C34 C33 117.0(8) . . ? C35 C34 H34A 122.1 . . ? C33 C34 H34A 120.9 . . ? C34 C35 C36 123.3(8) . . ? C34 C35 H35A 117.2 . . ? C36 C35 H35A 119.5 . . ? C35 C36 C37 120.7(9) . . ? C35 C36 H36A 119.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 116.3(9) . . ? C38 C37 H37A 121.1 . . ? C36 C37 H37A 122.6 . . ? C37 C38 N31 131.4(7) . . ? C37 C38 C33 122.6(7) . . ? N31 C38 C33 106.1(6) . . ? N32 C39 H39A 109.6 . . ? N32 C39 H39B 108.0 . . ? H39A C39 H39B 109.5 . . ? N32 C39 H39C 110.8 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 N41 C48 105.1(6) . . ? C42 N41 Tb1 114.8(4) . . ? C48 N41 Tb1 130.2(5) . . ? C42 N42 C43 107.5(6) . . ? C42 N42 C49 128.2(7) . . ? C43 N42 C49 124.3(6) . . ? C42 C41 N2 109.2(6) . . ? C42 C41 H41A 109.7 . . ? N2 C41 H41A 110.0 . . ? C42 C41 H41B 110.0 . . ? N2 C41 H41B 109.4 . . ? H41A C41 H41B 108.5 . . ? N41 C42 N42 112.1(6) . . ? N41 C42 C41 123.2(6) . . ? N42 C42 C41 124.7(6) . . ? N42 C43 C48 106.7(6) . . ? N42 C43 C44 131.3(8) . . ? C48 C43 C44 122.0(8) . . ? C43 C44 C45 116.2(8) . . ? C43 C44 H44A 122.1 . . ? C45 C44 H44A 121.7 . . ? C46 C45 C44 121.6(7) . . ? C46 C45 H45A 118.7 . . ? C44 C45 H45A 119.6 . . ? C47 C46 C45 122.5(8) . . ? C47 C46 H46A 119.1 . . ? C45 C46 H46A 118.4 . . ? C46 C47 C48 116.0(8) . . ? C46 C47 H47A 122.1 . . ? C48 C47 H47A 121.9 . . ? C43 C48 N41 108.7(7) . . ? C43 C48 C47 121.6(7) . . ? N41 C48 C47 129.7(7) . . ? N42 C49 H49A 109.2 . . ? N42 C49 H49B 109.7 . . ? H49A C49 H49B 109.5 . . ? N42 C49 H49C 109.6 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 N51 C58 105.1(6) . . ? C52 N51 Tb1 117.5(5) . . ? C58 N51 Tb1 128.5(4) . . ? C52 N52 C53 105.4(6) . . ? C52 N52 C59 126.0(7) . . ? C53 N52 C59 128.4(7) . . ? C52 C51 N2 107.9(6) . . ? C52 C51 H51A 110.1 . . ? N2 C51 H51A 110.4 . . ? C52 C51 H51B 110.0 . . ? N2 C51 H51B 109.6 . . ? H51A C51 H51B 108.7 . . ? N51 C52 N52 114.5(7) . . ? N51 C52 C51 122.7(7) . . ? N52 C52 C51 122.8(7) . . ? N52 C53 C54 130.4(7) . . ? N52 C53 C58 107.9(7) . . ? C54 C53 C58 121.7(8) . . ? C55 C54 C53 117.2(7) . . ? C55 C54 H54A 121.5 . . ? C53 C54 H54A 121.3 . . ? C54 C55 C56 121.2(8) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.0 . . ? C57 C56 C55 122.0(9) . . ? C57 C56 H56A 119.1 . . ? C55 C56 H56A 118.8 . . ? C58 C57 C56 116.9(8) . . ? C58 C57 H57A 121.1 . . ? C56 C57 H57A 122.0 . . ? C57 C58 C53 121.0(8) . . ? C57 C58 N51 132.0(7) . . ? C53 C58 N51 106.9(7) . . ? N52 C59 H59A 109.8 . . ? N52 C59 H59B 109.2 . . ? H59A C59 H59B 109.5 . . ? N52 C59 H59C 109.4 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 N61 C68 104.1(6) . . ? C62 N61 Tb1 117.3(5) . . ? C68 N61 Tb1 130.6(5) . . ? C62 N62 C63 106.1(6) . . ? C62 N62 C69 125.5(7) . . ? C63 N62 C69 128.4(7) . . ? N2 C61 C62 109.7(6) . . ? N2 C61 H61A 109.4 . . ? C62 C61 H61A 110.2 . . ? N2 C61 H61B 109.5 . . ? C62 C61 H61B 109.4 . . ? H61A C61 H61B 108.6 . . ? N61 C62 N62 114.4(7) . . ? N61 C62 C61 122.0(7) . . ? N62 C62 C61 123.4(7) . . ? N62 C63 C68 106.5(7) . . ? N62 C63 C64 131.3(8) . . ? C68 C63 C64 122.0(8) . . ? C63 C64 C65 115.3(9) . . ? C63 C64 H64A 120.9 . . ? C65 C64 H64A 123.7 . . ? C66 C65 C64 121.7(9) . . ? C66 C65 H65A 119.6 . . ? C64 C65 H65A 118.8 . . ? C65 C66 C67 122.9(8) . . ? C65 C66 H66A 118.5 . . ? C67 C66 H66A 118.6 . . ? C68 C67 C66 116.4(8) . . ? C68 C67 H67A 121.7 . . ? C66 C67 H67A 121.8 . . ? C67 C68 C63 121.5(7) . . ? C67 C68 N61 129.7(7) . . ? C63 C68 N61 108.8(6) . . ? N62 C69 H69A 110.0 . . ? N62 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N62 C69 H69C 108.9 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O12 Cl1 O13 111.8(6) . . ? O12 Cl1 O11 109.7(5) . . ? O13 Cl1 O11 109.0(5) . . ? O12 Cl1 O14 108.2(6) . . ? O13 Cl1 O14 107.1(5) . . ? O11 Cl1 O14 110.9(6) . . ? O24 Cl2 O21 116.2(8) . . ? O24 Cl2 O22 115.3(7) . . ? O21 Cl2 O22 113.7(6) . . ? O24 Cl2 O23 104.7(7) . . ? O21 Cl2 O23 103.7(8) . . ? O22 Cl2 O23 100.6(7) . . ? O32 Cl3 O33 110.3(4) . . ? O32 Cl3 O31 111.6(5) . . ? O33 Cl3 O31 109.8(5) . . ? O32 Cl3 O34 110.5(5) . . ? O33 Cl3 O34 107.8(5) . . ? O31 Cl3 O34 106.7(4) . . ? N1W C1W C2W 173.9(15) . . ? C1W C2W H2WA 108.0 . . ? C1W C2W H2WB 111.4 . . ? H2WA C2W H2WB 109.5 . . ? C1W C2W H2WC 109.0 . . ? H2WA C2W H2WC 109.5 . . ? H2WB C2W H2WC 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 N11 Tb1 N1 C31 83.4(4) . . . . ? N51 Tb1 N1 C31 18.0(5) . . . . ? N21 Tb1 N1 C31 -156.7(5) . . . . ? N41 Tb1 N1 C31 -100.2(4) . . . . ? N31 Tb1 N1 C31 -36.7(4) . . . . ? N61 Tb1 N1 C31 138.1(4) . . . . ? N2 Tb1 N1 C31 -70(15) . . . . ? N11 Tb1 N1 C11 -35.8(4) . . . . ? N51 Tb1 N1 C11 -101.1(4) . . . . ? N21 Tb1 N1 C11 84.2(4) . . . . ? N41 Tb1 N1 C11 140.6(4) . . . . ? N31 Tb1 N1 C11 -155.8(5) . . . . ? N61 Tb1 N1 C11 19.0(5) . . . . ? N2 Tb1 N1 C11 171(33) . . . . ? N11 Tb1 N1 C21 -156.1(5) . . . . ? N51 Tb1 N1 C21 138.5(4) . . . . ? N21 Tb1 N1 C21 -36.2(4) . . . . ? N41 Tb1 N1 C21 20.3(5) . . . . ? N31 Tb1 N1 C21 83.8(5) . . . . ? N61 Tb1 N1 C21 -101.4(5) . . . . ? N2 Tb1 N1 C21 51(15) . . . . ? N11 Tb1 N2 C41 139.1(4) . . . . ? N51 Tb1 N2 C41 -156.1(5) . . . . ? N21 Tb1 N2 C41 18.6(5) . . . . ? N41 Tb1 N2 C41 -37.3(4) . . . . ? N31 Tb1 N2 C41 -100.8(4) . . . . ? N61 Tb1 N2 C41 84.3(4) . . . . ? N1 Tb1 N2 C41 -68(15) . . . . ? N11 Tb1 N2 C61 19.5(5) . . . . ? N51 Tb1 N2 C61 84.3(4) . . . . ? N21 Tb1 N2 C61 -101.0(4) . . . . ? N41 Tb1 N2 C61 -156.9(5) . . . . ? N31 Tb1 N2 C61 139.6(4) . . . . ? N61 Tb1 N2 C61 -35.3(4) . . . . ? N1 Tb1 N2 C61 172(25) . . . . ? N11 Tb1 N2 C51 -100.6(5) . . . . ? N51 Tb1 N2 C51 -35.7(4) . . . . ? N21 Tb1 N2 C51 139.0(4) . . . . ? N41 Tb1 N2 C51 83.0(5) . . . . ? N31 Tb1 N2 C51 19.5(5) . . . . ? N61 Tb1 N2 C51 -155.3(5) . . . . ? N1 Tb1 N2 C51 52(16) . . . . ? N51 Tb1 N11 C12 158.0(5) . . . . ? N21 Tb1 N11 C12 -19.0(5) . . . . ? N41 Tb1 N11 C12 -44(3) . . . . ? N31 Tb1 N11 C12 85.4(5) . . . . ? N61 Tb1 N11 C12 -97.4(5) . . . . ? N2 Tb1 N11 C12 -146.9(5) . . . . ? N1 Tb1 N11 C12 33.4(5) . . . . ? N51 Tb1 N11 C18 -59.9(6) . . . . ? N21 Tb1 N11 C18 123.1(6) . . . . ? N41 Tb1 N11 C18 98(3) . . . . ? N31 Tb1 N11 C18 -132.5(6) . . . . ? N61 Tb1 N11 C18 44.7(6) . . . . ? N2 Tb1 N11 C18 -4.9(6) . . . . ? N1 Tb1 N11 C18 175.5(6) . . . . ? C31 N1 C11 C12 -84.2(7) . . . . ? C21 N1 C11 C12 154.6(6) . . . . ? Tb1 N1 C11 C12 35.2(6) . . . . ? C13 N12 C12 N11 1.2(8) . . . . ? C19 N12 C12 N11 -176.8(7) . . . . ? C13 N12 C12 C11 178.1(7) . . . . ? C19 N12 C12 C11 0.1(11) . . . . ? C18 N11 C12 N12 -1.9(8) . . . . ? Tb1 N11 C12 N12 148.5(5) . . . . ? C18 N11 C12 C11 -178.9(6) . . . . ? Tb1 N11 C12 C11 -28.4(8) . . . . ? N1 C11 C12 N12 175.0(6) . . . . ? N1 C11 C12 N11 -8.3(9) . . . . ? C12 N12 C13 C18 0.1(8) . . . . ? C19 N12 C13 C18 178.1(7) . . . . ? C12 N12 C13 C14 -178.2(9) . . . . ? C19 N12 C13 C14 -0.2(13) . . . . ? N12 C13 C14 C15 179.3(8) . . . . ? C18 C13 C14 C15 1.1(12) . . . . ? C13 C14 C15 C16 -1.7(14) . . . . ? C14 C15 C16 C17 2.1(13) . . . . ? C15 C16 C17 C18 -1.9(12) . . . . ? C16 C17 C18 C13 1.5(11) . . . . ? C16 C17 C18 N11 -176.5(8) . . . . ? N12 C13 C18 C17 -179.7(7) . . . . ? C14 C13 C18 C17 -1.1(12) . . . . ? N12 C13 C18 N11 -1.3(8) . . . . ? C14 C13 C18 N11 177.3(7) . . . . ? C12 N11 C18 C17 -179.9(8) . . . . ? Tb1 N11 C18 C17 34.4(11) . . . . ? C12 N11 C18 C13 1.9(8) . . . . ? Tb1 N11 C18 C13 -143.9(5) . . . . ? N11 Tb1 N21 C22 83.7(5) . . . . ? N51 Tb1 N21 C22 -58(3) . . . . ? N41 Tb1 N21 C22 -97.8(5) . . . . ? N31 Tb1 N21 C22 -20.8(5) . . . . ? N61 Tb1 N21 C22 156.3(5) . . . . ? N2 Tb1 N21 C22 -147.9(5) . . . . ? N1 Tb1 N21 C22 31.3(5) . . . . ? N11 Tb1 N21 C28 -132.1(6) . . . . ? N51 Tb1 N21 C28 86(2) . . . . ? N41 Tb1 N21 C28 46.4(6) . . . . ? N31 Tb1 N21 C28 123.4(6) . . . . ? N61 Tb1 N21 C28 -59.5(6) . . . . ? N2 Tb1 N21 C28 -3.7(6) . . . . ? N1 Tb1 N21 C28 175.5(6) . . . . ? C31 N1 C21 C22 157.0(6) . . . . ? C11 N1 C21 C22 -82.5(7) . . . . ? Tb1 N1 C21 C22 37.0(7) . . . . ? C28 N21 C22 N22 -0.2(9) . . . . ? Tb1 N21 C22 N22 152.5(5) . . . . ? C28 N21 C22 C21 -177.4(7) . . . . ? Tb1 N21 C22 C21 -24.8(9) . . . . ? C23 N22 C22 N21 -1.5(9) . . . . ? C29 N22 C22 N21 -179.8(8) . . . . ? C23 N22 C22 C21 175.9(7) . . . . ? C29 N22 C22 C21 -2.4(13) . . . . ? N1 C21 C22 N21 -11.7(10) . . . . ? N1 C21 C22 N22 171.2(7) . . . . ? C22 N22 C23 C24 -178.1(9) . . . . ? C29 N22 C23 C24 0.2(15) . . . . ? C22 N22 C23 C28 2.4(8) . . . . ? C29 N22 C23 C28 -179.2(8) . . . . ? C28 C23 C24 C25 -1.3(14) . . . . ? N22 C23 C24 C25 179.3(9) . . . . ? C23 C24 C25 C26 0.6(14) . . . . ? C24 C25 C26 C27 0.3(14) . . . . ? C25 C26 C27 C28 -0.5(13) . . . . ? C22 N21 C28 C27 177.8(8) . . . . ? Tb1 N21 C28 C27 30.8(12) . . . . ? C22 N21 C28 C23 1.8(8) . . . . ? Tb1 N21 C28 C23 -145.2(5) . . . . ? C26 C27 C28 N21 -176.0(8) . . . . ? C26 C27 C28 C23 -0.2(12) . . . . ? C24 C23 C28 N21 177.8(8) . . . . ? N22 C23 C28 N21 -2.7(8) . . . . ? C24 C23 C28 C27 1.2(12) . . . . ? N22 C23 C28 C27 -179.3(7) . . . . ? N11 Tb1 N31 C32 -20.8(5) . . . . ? N51 Tb1 N31 C32 -99.2(5) . . . . ? N21 Tb1 N31 C32 83.8(5) . . . . ? N41 Tb1 N31 C32 156.6(5) . . . . ? N61 Tb1 N31 C32 -57(3) . . . . ? N2 Tb1 N31 C32 -149.0(5) . . . . ? N1 Tb1 N31 C32 31.4(5) . . . . ? N11 Tb1 N31 C38 124.1(5) . . . . ? N51 Tb1 N31 C38 45.7(5) . . . . ? N21 Tb1 N31 C38 -131.3(5) . . . . ? N41 Tb1 N31 C38 -58.5(6) . . . . ? N61 Tb1 N31 C38 88(3) . . . . ? N2 Tb1 N31 C38 -4.1(6) . . . . ? N1 Tb1 N31 C38 176.3(6) . . . . ? C11 N1 C31 C32 157.5(6) . . . . ? C21 N1 C31 C32 -81.3(7) . . . . ? Tb1 N1 C31 C32 38.4(6) . . . . ? C33 N32 C32 N31 -0.4(8) . . . . ? C39 N32 C32 N31 178.0(8) . . . . ? C33 N32 C32 C31 174.8(7) . . . . ? C39 N32 C32 C31 -6.8(13) . . . . ? C38 N31 C32 N32 -0.8(8) . . . . ? Tb1 N31 C32 N32 151.4(5) . . . . ? C38 N31 C32 C31 -176.2(6) . . . . ? Tb1 N31 C32 C31 -24.0(9) . . . . ? N1 C31 C32 N32 172.4(7) . . . . ? N1 C31 C32 N31 -12.8(9) . . . . ? C32 N32 C33 C34 -178.1(8) . . . . ? C39 N32 C33 C34 3.5(14) . . . . ? C32 N32 C33 C38 1.4(8) . . . . ? C39 N32 C33 C38 -177.0(8) . . . . ? N32 C33 C34 C35 -179.7(8) . . . . ? C38 C33 C34 C35 0.8(11) . . . . ? C33 C34 C35 C36 0.1(13) . . . . ? C34 C35 C36 C37 -0.6(14) . . . . ? C35 C36 C37 C38 0.2(13) . . . . ? C36 C37 C38 N31 -178.0(7) . . . . ? C36 C37 C38 C33 0.8(11) . . . . ? C32 N31 C38 C37 -179.5(8) . . . . ? Tb1 N31 C38 C37 32.7(11) . . . . ? C32 N31 C38 C33 1.6(8) . . . . ? Tb1 N31 C38 C33 -146.2(5) . . . . ? N32 C33 C38 C37 179.1(7) . . . . ? C34 C33 C38 C37 -1.3(11) . . . . ? N32 C33 C38 N31 -1.9(8) . . . . ? C34 C33 C38 N31 177.7(7) . . . . ? N11 Tb1 N41 C42 -71(3) . . . . ? N51 Tb1 N41 C42 87.3(5) . . . . ? N21 Tb1 N41 C42 -95.8(5) . . . . ? N31 Tb1 N41 C42 159.6(5) . . . . ? N61 Tb1 N41 C42 -17.7(5) . . . . ? N2 Tb1 N41 C42 34.1(5) . . . . ? N1 Tb1 N41 C42 -146.3(5) . . . . ? N11 Tb1 N41 C48 69(3) . . . . ? N51 Tb1 N41 C48 -132.7(6) . . . . ? N21 Tb1 N41 C48 44.2(6) . . . . ? N31 Tb1 N41 C48 -60.4(6) . . . . ? N61 Tb1 N41 C48 122.2(6) . . . . ? N2 Tb1 N41 C48 174.0(7) . . . . ? N1 Tb1 N41 C48 -6.4(7) . . . . ? C61 N2 C41 C42 156.5(6) . . . . ? C51 N2 C41 C42 -83.2(7) . . . . ? Tb1 N2 C41 C42 37.0(6) . . . . ? C48 N41 C42 N42 -1.1(8) . . . . ? Tb1 N41 C42 N42 148.3(5) . . . . ? C48 N41 C42 C41 -178.3(7) . . . . ? Tb1 N41 C42 C41 -28.9(9) . . . . ? C43 N42 C42 N41 0.9(8) . . . . ? C49 N42 C42 N41 179.8(7) . . . . ? C43 N42 C42 C41 178.0(7) . . . . ? C49 N42 C42 C41 -3.0(12) . . . . ? N2 C41 C42 N41 -8.3(10) . . . . ? N2 C41 C42 N42 174.9(6) . . . . ? C42 N42 C43 C48 -0.2(8) . . . . ? C49 N42 C43 C48 -179.2(7) . . . . ? C42 N42 C43 C44 178.9(9) . . . . ? C49 N42 C43 C44 -0.1(14) . . . . ? N42 C43 C44 C45 -177.4(8) . . . . ? C48 C43 C44 C45 1.7(12) . . . . ? C43 C44 C45 C46 -2.0(14) . . . . ? C44 C45 C46 C47 2.4(16) . . . . ? C45 C46 C47 C48 -2.3(14) . . . . ? N42 C43 C48 N41 -0.5(9) . . . . ? C44 C43 C48 N41 -179.7(7) . . . . ? N42 C43 C48 C47 177.5(7) . . . . ? C44 C43 C48 C47 -1.7(12) . . . . ? C42 N41 C48 C43 0.9(8) . . . . ? Tb1 N41 C48 C43 -141.8(6) . . . . ? C42 N41 C48 C47 -176.8(8) . . . . ? Tb1 N41 C48 C47 40.4(11) . . . . ? C46 C47 C48 C43 1.9(12) . . . . ? C46 C47 C48 N41 179.4(8) . . . . ? N11 Tb1 N51 C52 158.8(5) . . . . ? N21 Tb1 N51 C52 -59(3) . . . . ? N41 Tb1 N51 C52 -19.9(5) . . . . ? N31 Tb1 N51 C52 -96.9(5) . . . . ? N61 Tb1 N51 C52 86.3(5) . . . . ? N2 Tb1 N51 C52 33.3(5) . . . . ? N1 Tb1 N51 C52 -145.9(5) . . . . ? N11 Tb1 N51 C58 -59.1(5) . . . . ? N21 Tb1 N51 C58 83(2) . . . . ? N41 Tb1 N51 C58 122.1(5) . . . . ? N31 Tb1 N51 C58 45.2(5) . . . . ? N61 Tb1 N51 C58 -131.7(5) . . . . ? N2 Tb1 N51 C58 175.3(6) . . . . ? N1 Tb1 N51 C58 -3.9(6) . . . . ? C41 N2 C51 C52 155.2(6) . . . . ? C61 N2 C51 C52 -84.4(7) . . . . ? Tb1 N2 C51 C52 35.4(7) . . . . ? C58 N51 C52 N52 1.4(8) . . . . ? Tb1 N51 C52 N52 151.5(5) . . . . ? C58 N51 C52 C51 -177.6(7) . . . . ? Tb1 N51 C52 C51 -27.5(9) . . . . ? C53 N52 C52 N51 -3.3(8) . . . . ? C59 N52 C52 N51 -178.2(7) . . . . ? C53 N52 C52 C51 175.7(7) . . . . ? C59 N52 C52 C51 0.9(11) . . . . ? N2 C51 C52 N51 -8.5(10) . . . . ? N2 C51 C52 N52 172.5(6) . . . . ? C52 N52 C53 C54 -173.6(8) . . . . ? C59 N52 C53 C54 1.1(13) . . . . ? C52 N52 C53 C58 3.8(8) . . . . ? C59 N52 C53 C58 178.5(7) . . . . ? N52 C53 C54 C55 179.2(8) . . . . ? C58 C53 C54 C55 2.1(11) . . . . ? C53 C54 C55 C56 -1.0(13) . . . . ? C54 C55 C56 C57 0.3(14) . . . . ? C55 C56 C57 C58 -0.6(12) . . . . ? C56 C57 C58 C53 1.7(11) . . . . ? C56 C57 C58 N51 -174.6(8) . . . . ? N52 C53 C58 C57 179.8(7) . . . . ? C54 C53 C58 C57 -2.5(11) . . . . ? N52 C53 C58 N51 -3.1(8) . . . . ? C54 C53 C58 N51 174.6(7) . . . . ? C52 N51 C58 C57 177.8(8) . . . . ? Tb1 N51 C58 C57 32.2(11) . . . . ? C52 N51 C58 C53 1.1(8) . . . . ? Tb1 N51 C58 C53 -144.5(5) . . . . ? N11 Tb1 N61 C62 -100.5(5) . . . . ? N51 Tb1 N61 C62 -22.2(5) . . . . ? N21 Tb1 N61 C62 155.1(5) . . . . ? N41 Tb1 N61 C62 82.3(5) . . . . ? N31 Tb1 N61 C62 -64(3) . . . . ? N2 Tb1 N61 C62 30.7(5) . . . . ? N1 Tb1 N61 C62 -149.7(5) . . . . ? N11 Tb1 N61 C68 43.1(6) . . . . ? N51 Tb1 N61 C68 121.4(6) . . . . ? N21 Tb1 N61 C68 -61.3(6) . . . . ? N41 Tb1 N61 C68 -134.1(6) . . . . ? N31 Tb1 N61 C68 80(3) . . . . ? N2 Tb1 N61 C68 174.3(6) . . . . ? N1 Tb1 N61 C68 -6.1(6) . . . . ? C41 N2 C61 C62 -81.5(7) . . . . ? C51 N2 C61 C62 157.8(6) . . . . ? Tb1 N2 C61 C62 37.7(6) . . . . ? C68 N61 C62 N62 -0.1(8) . . . . ? Tb1 N61 C62 N62 152.2(5) . . . . ? C68 N61 C62 C61 -174.8(6) . . . . ? Tb1 N61 C62 C61 -22.5(9) . . . . ? C63 N62 C62 N61 0.7(9) . . . . ? C69 N62 C62 N61 -178.3(7) . . . . ? C63 N62 C62 C61 175.4(7) . . . . ? C69 N62 C62 C61 -3.6(12) . . . . ? N2 C61 C62 N61 -12.9(9) . . . . ? N2 C61 C62 N62 172.8(6) . . . . ? C62 N62 C63 C68 -1.1(8) . . . . ? C69 N62 C63 C68 177.9(8) . . . . ? C62 N62 C63 C64 -176.9(9) . . . . ? C69 N62 C63 C64 2.1(14) . . . . ? N62 C63 C64 C65 175.1(8) . . . . ? C68 C63 C64 C65 -0.1(12) . . . . ? C63 C64 C65 C66 3.0(14) . . . . ? C64 C65 C66 C67 -3.2(14) . . . . ? C65 C66 C67 C68 0.2(12) . . . . ? C66 C67 C68 C63 2.7(11) . . . . ? C66 C67 C68 N61 -177.4(7) . . . . ? N62 C63 C68 C67 -179.0(7) . . . . ? C64 C63 C68 C67 -2.8(12) . . . . ? N62 C63 C68 N61 1.0(8) . . . . ? C64 C63 C68 N61 177.3(7) . . . . ? C62 N61 C68 C67 179.5(7) . . . . ? Tb1 N61 C68 C67 32.4(11) . . . . ? C62 N61 C68 C63 -0.6(8) . . . . ? Tb1 N61 C68 C63 -147.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.909 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.118 #=====================# data_18 _database_code_depnum_ccdc_archive 'CCDC 698716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H78 Cl3 N14 O12 Tb' _chemical_formula_weight 1812.93 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 47.992(10) _cell_length_b 57.798(12) _cell_length_c 12.112(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 33597(12) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14848 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7517 _exptl_absorpt_correction_T_max 0.8885 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku IP' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18802 _diffrn_reflns_av_R_equivalents 0.1228 _diffrn_reflns_av_sigmaI/netI 0.1375 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -67 _diffrn_reflns_limit_k_max 67 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.50 _reflns_number_total 10602 _reflns_number_gt 8576 _reflns_threshold_expression >2sigma(I) _computing_data_collection BIOTEX _computing_cell_refinement BIOTEX _computing_data_reduction BIOTEX _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+20.0000P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.465(14) _refine_ls_number_reflns 10602 _refine_ls_number_parameters 872 _refine_ls_number_restraints 826 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.1926 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.008 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 Tb1 Tb 0.933337(8) 0.144441(7) 0.39228(5) 0.05852(9) Uani 1 1 d . . . N1 N 0.93567(13) 0.14627(12) 0.6108(7) 0.065(2) Uani 1 1 d . . . N2 N 0.91494(14) 0.08423(12) 0.6270(6) 0.067(2) Uani 1 1 d . . . N3 N 0.91279(13) 0.11065(12) 0.4909(5) 0.0563(19) Uani 1 1 d . . . N4 N 0.88972(17) 0.19669(15) 0.6136(6) 0.085(3) Uani 1 1 d . . . N5 N 0.91464(15) 0.17970(13) 0.4802(5) 0.063(2) Uani 1 1 d . . . N6 N 1.01181(13) 0.15716(14) 0.5995(5) 0.066(2) Uani 1 1 d . . . N7 N 0.98023(15) 0.14362(13) 0.4776(6) 0.070(2) Uani 1 1 d . . . N8 N 0.92686(14) 0.14485(13) 0.1742(5) 0.058(2) Uani 1 1 d . . . N9 N 0.88435(14) 0.14603(13) 0.3207(5) 0.063(2) Uani 1 1 d . . . N10 N 0.85367(15) 0.16254(17) 0.2070(6) 0.083(3) Uani 1 1 d . . . N11 N 0.96088(14) 0.17303(14) 0.2893(5) 0.067(2) Uani 1 1 d . . . N12 N 0.98965(13) 0.18121(15) 0.1543(6) 0.080(2) Uani 1 1 d . . . N13 N 0.94924(15) 0.10949(14) 0.2895(6) 0.073(2) Uani 1 1 d . . . N14 N 0.94291(16) 0.08104(16) 0.1662(7) 0.089(3) Uani 1 1 d . . . C1 C 0.90436(18) 0.16161(19) 0.1550(7) 0.086(3) Uani 1 1 d . . . H1A H 0.9111 0.1772 0.1693 0.103 Uiso 1 1 calc R . . H1B H 0.8983 0.1608 0.0787 0.103 Uiso 1 1 calc R . . C2 C 0.88092(17) 0.15630(18) 0.2286(7) 0.067(3) Uani 1 1 d . . . C3 C 0.85791(16) 0.14516(19) 0.3720(6) 0.075(3) Uani 1 1 d . . . C4 C 0.84789(18) 0.13654(19) 0.4687(8) 0.075(3) Uani 1 1 d . . . H4 H 0.8601 0.1296 0.5185 0.089 Uiso 1 1 calc R . . C5 C 0.8209(2) 0.1378(3) 0.4930(13) 0.118(5) Uani 1 1 d . . . H5 H 0.8144 0.1326 0.5610 0.142 Uiso 1 1 calc R . . C6 C 0.8025(2) 0.1469(2) 0.4167(8) 0.096(4) Uani 1 1 d . . . H6 H 0.7836 0.1471 0.4342 0.115 Uiso 1 1 calc R . . C7 C 0.8105(2) 0.1555(3) 0.3186(9) 0.105(5) Uani 1 1 d . . . H7 H 0.7978 0.1611 0.2672 0.126 Uiso 1 1 calc R . . C8 C 0.8383(2) 0.1554(2) 0.2997(9) 0.092(4) Uani 1 1 d . . . C16 C 0.92009(19) 0.12082(18) 0.1385(8) 0.079(3) Uani 1 1 d . . . H16A H 0.9007 0.1175 0.1543 0.095 Uiso 1 1 calc R . . H16B H 0.9229 0.1194 0.0595 0.095 Uiso 1 1 calc R . . C17 C 0.93788(19) 0.10409(18) 0.1962(7) 0.069(3) Uani 1 1 d . . . C18 C 0.96352(18) 0.0890(2) 0.3231(8) 0.079(3) Uani 1 1 d . . . C19 C 0.97944(17) 0.0848(2) 0.4149(7) 0.082(3) Uani 1 1 d . . . H19 H 0.9822 0.0963 0.4674 0.099 Uiso 1 1 calc R . . C20 C 0.9915(2) 0.0628(2) 0.4283(11) 0.112(5) Uani 1 1 d . . . H20 H 1.0022 0.0596 0.4903 0.135 Uiso 1 1 calc R . . C21 C 0.9872(3) 0.0450(3) 0.3464(12) 0.145(6) Uani 1 1 d . . . H21 H 0.9945 0.0302 0.3565 0.174 Uiso 1 1 calc R . . C22 C 0.9720(3) 0.0502(2) 0.2531(12) 0.116(5) Uani 1 1 d . . . H22 H 0.9700 0.0394 0.1970 0.139 Uiso 1 1 calc R . . C23 C 0.9594(2) 0.0726(2) 0.2435(9) 0.083(3) Uani 1 1 d . . . C24 C 0.9340(2) 0.0702(2) 0.0639(9) 0.093(3) Uani 1 1 d U . . H24A H 0.9479 0.0590 0.0416 0.111 Uiso 1 1 calc R . . H24B H 0.9329 0.0819 0.0067 0.111 Uiso 1 1 calc R . . C25 C 0.90562(10) 0.05798(10) 0.0740(5) 0.092(3) Uani 1 1 d GU . . C26 C 0.88124(10) 0.06762(10) 0.0325(4) 0.122(4) Uani 1 1 d GU . . H26 H 0.8814 0.0825 0.0036 0.146 Uiso 1 1 calc R . . C27 C 0.85660(11) 0.05500(11) 0.0344(6) 0.133(4) Uani 1 1 d GU . . H27 H 0.8403 0.0615 0.0066 0.160 Uiso 1 1 calc R . . C28 C 0.85633(11) 0.03272(11) 0.0776(7) 0.134(4) Uani 1 1 d GU . . H28 H 0.8398 0.0243 0.0788 0.160 Uiso 1 1 calc R . . C29 C 0.88072(12) 0.02307(10) 0.1190(6) 0.132(4) Uani 1 1 d GU . . H29 H 0.8805 0.0082 0.1480 0.159 Uiso 1 1 calc R . . C30 C 0.90536(11) 0.03570(10) 0.1172(5) 0.121(4) Uani 1 1 d GU . . H30 H 0.9217 0.0292 0.1449 0.145 Uiso 1 1 calc R . . C9 C 0.84181(15) 0.17384(11) 0.1091(9) 0.111(4) Uani 1 1 d GDU . . H9A H 0.8559 0.1743 0.0515 0.133 Uiso 1 1 calc R . . H9B H 0.8264 0.1646 0.0820 0.133 Uiso 1 1 calc R . . C10 C 0.83212(11) 0.19705(14) 0.1303(6) 0.125(3) Uani 1 1 d GDU . . C11 C 0.81780(11) 0.20767(18) 0.0444(7) 0.173(5) Uani 1 1 d GDU . . H11 H 0.8148 0.1998 -0.0214 0.208 Uiso 1 1 calc R . . C12 C 0.80791(14) 0.23012(18) 0.0569(10) 0.195(5) Uani 1 1 d GDU . . H12 H 0.7983 0.2372 -0.0006 0.234 Uiso 1 1 calc R . . C13 C 0.81235(15) 0.24196(15) 0.1552(13) 0.193(5) Uani 1 1 d GDU . . H13 H 0.8057 0.2570 0.1635 0.231 Uiso 1 1 calc R . . C14 C 0.82667(14) 0.23134(19) 0.2411(11) 0.213(5) Uani 1 1 d GDU . . H14 H 0.8296 0.2393 0.3069 0.255 Uiso 1 1 calc R . . C15 C 0.83655(12) 0.20888(18) 0.2287(7) 0.187(5) Uani 1 1 d GDU . . H15 H 0.8461 0.2018 0.2862 0.224 Uiso 1 1 calc R . . C39 C 0.99756(12) 0.1858(3) 0.0474(9) 0.132(4) Uani 1 1 d GDU . . H39A H 0.9898 0.2008 0.0280 0.158 Uiso 1 1 calc R . . H39B H 0.9885 0.1745 0.0006 0.158 Uiso 1 1 calc R . . C40 C 1.02798(15) 0.18620(15) 0.0164(4) 0.133(4) Uani 1 1 d GDU . . C41 C 1.04852(16) 0.20169(16) -0.0164(5) 0.197(5) Uani 1 1 d GDU . . H41 H 1.0448 0.2175 -0.0177 0.236 Uiso 1 1 calc R . . C42 C 1.07465(15) 0.19359(17) -0.0474(5) 0.192(5) Uani 1 1 d GDU . . H42 H 1.0884 0.2040 -0.0693 0.230 Uiso 1 1 calc R . . C43 C 1.08023(15) 0.16999(18) -0.0455(5) 0.196(5) Uani 1 1 d GDU . . H43 H 1.0977 0.1646 -0.0662 0.235 Uiso 1 1 calc R . . C44 C 1.05968(15) 0.15450(16) -0.0127(5) 0.211(5) Uani 1 1 d GDU . . H44 H 1.0634 0.1387 -0.0115 0.253 Uiso 1 1 calc R . . C45 C 1.03356(14) 0.16260(15) 0.0182(4) 0.183(5) Uani 1 1 d GDU . . H45 H 1.0198 0.1522 0.0402 0.220 Uiso 1 1 calc R . . C9' C 0.9180(2) 0.07497(19) 0.7363(7) 0.082(3) Uani 1 1 d GDU . . H9'1 H 0.8996 0.0722 0.7673 0.098 Uiso 1 1 calc R . . H9'2 H 0.9272 0.0863 0.7824 0.098 Uiso 1 1 calc R . . C10' C 0.93406(5) 0.05307(4) 0.73903(17) 0.094(3) Uani 1 1 d GDU . . C11' C 0.95831(5) 0.04995(4) 0.67808(17) 0.129(4) Uani 1 1 d GDU . . H11' H 0.9649 0.0618 0.6331 0.155 Uiso 1 1 calc R . . C12' C 0.97274(5) 0.02914(4) 0.68439(19) 0.165(5) Uani 1 1 d GDU . . H12' H 0.9890 0.0271 0.6436 0.198 Uiso 1 1 calc R . . C13' C 0.96291(6) 0.01145(4) 0.7516(2) 0.161(5) Uani 1 1 d GDU . . H13' H 0.9726 -0.0025 0.7559 0.194 Uiso 1 1 calc R . . C14' C 0.93865(6) 0.01456(4) 0.8126(2) 0.142(4) Uani 1 1 d GDU . . H14' H 0.9321 0.0027 0.8576 0.171 Uiso 1 1 calc R . . C15' C 0.92423(5) 0.03538(4) 0.80628(18) 0.111(3) Uani 1 1 d GDU . . H15' H 0.9080 0.0375 0.8471 0.134 Uiso 1 1 calc R . . C31 C 0.95271(6) 0.15122(5) 0.11877(18) 0.082(3) Uani 1 1 d G . . H31A H 0.9487 0.1572 0.0456 0.099 Uiso 1 1 calc R . . H31B H 0.9646 0.1377 0.1110 0.099 Uiso 1 1 calc R . . C32 C 0.96713(6) 0.16917(5) 0.1854(2) 0.060(2) Uani 1 1 d G . . C33 C 0.97998(6) 0.19014(4) 0.3257(2) 0.071(3) Uani 1 1 d G . . C34 C 0.98080(6) 0.20131(4) 0.4271(2) 0.090(4) Uani 1 1 d G . . H34 H 0.9674 0.1988 0.4814 0.108 Uiso 1 1 calc R . . C35 C 1.00323(6) 0.21674(4) 0.4427(3) 0.092(3) Uani 1 1 d G . . H35 H 1.0045 0.2247 0.5094 0.110 Uiso 1 1 calc R . . C36 C 1.02379(7) 0.22068(5) 0.3625(3) 0.113(5) Uani 1 1 d G . . H36 H 1.0390 0.2301 0.3778 0.136 Uiso 1 1 calc R . . C37 C 1.02107(7) 0.21020(5) 0.2597(3) 0.102(4) Uani 1 1 d G . . H37 H 1.0332 0.2138 0.2024 0.122 Uiso 1 1 calc R . . C38 C 0.99953(6) 0.19412(5) 0.2445(2) 0.077(3) Uani 1 1 d G . . C1' C 0.93728(4) 0.12278(4) 0.66285(17) 0.068(3) Uani 1 1 d G . . H1'1 H 0.9566 0.1180 0.6683 0.081 Uiso 1 1 calc R . . H1'2 H 0.9296 0.1234 0.7368 0.081 Uiso 1 1 calc R . . C2' C 0.92140(4) 0.10563(4) 0.59526(17) 0.070(3) Uani 1 1 d G . . C3' C 0.89921(4) 0.09046(4) 0.46152(18) 0.062(3) Uani 1 1 d G . . C4' C 0.88561(5) 0.08631(5) 0.35648(19) 0.074(3) Uani 1 1 d G . . H4' H 0.8847 0.0975 0.3014 0.088 Uiso 1 1 calc R . . C5' C 0.87390(5) 0.06418(5) 0.3438(2) 0.091(4) Uani 1 1 d G . . H5' H 0.8650 0.0604 0.2782 0.109 Uiso 1 1 calc R . . C6' C 0.87545(5) 0.04857(5) 0.4248(2) 0.088(3) Uani 1 1 d G . . H6' H 0.8669 0.0343 0.4126 0.105 Uiso 1 1 calc R . . C7' C 0.88888(5) 0.05175(4) 0.52768(19) 0.105(4) Uani 1 1 d G . . H7' H 0.8899 0.0404 0.5821 0.126 Uiso 1 1 calc R . . C8' C 0.90065(4) 0.07442(4) 0.53839(18) 0.066(3) Uani 1 1 d G . . C16' C 0.96082(5) 0.15849(4) 0.65390(19) 0.058(2) Uani 1 1 d G . . H16C H 0.9652 0.1532 0.7278 0.069 Uiso 1 1 calc R . . H16D H 0.9576 0.1750 0.6564 0.069 Uiso 1 1 calc R . . C17' C 0.98445(5) 0.15294(4) 0.57555(19) 0.064(3) Uani 1 1 d G . . C18' C 1.00780(5) 0.14325(4) 0.4318(2) 0.065(3) Uani 1 1 d G . . C19' C 1.01575(5) 0.13305(5) 0.3257(2) 0.074(3) Uani 1 1 d G . . H19' H 1.0033 0.1268 0.2750 0.088 Uiso 1 1 calc R . . C20' C 1.04612(5) 0.13410(5) 0.3105(2) 0.090(3) Uani 1 1 d G . . H20' H 1.0532 0.1278 0.2455 0.108 Uiso 1 1 calc R . . C21' C 1.06458(5) 0.14316(5) 0.3808(3) 0.097(3) Uani 1 1 d G . . H21' H 1.0833 0.1436 0.3609 0.116 Uiso 1 1 calc R . . C22' C 1.05585(5) 0.15264(5) 0.4917(2) 0.092(4) Uani 1 1 d G . . H22' H 1.0679 0.1589 0.5438 0.111 Uiso 1 1 calc R . . C23' C 1.02617(5) 0.15068(4) 0.5052(2) 0.065(3) Uani 1 1 d G . . C24' C 1.02275(5) 0.16623(4) 0.7053(2) 0.080(3) Uani 1 1 d GU . . H24C H 1.0410 0.1596 0.7195 0.096 Uiso 1 1 calc R . . H24D H 1.0104 0.1617 0.7650 0.096 Uiso 1 1 calc R . . C25' C 1.02511(6) 0.19276(7) 0.7022(3) 0.088(3) Uani 1 1 d GU . . C26' C 1.04846(6) 0.20403(8) 0.6607(3) 0.104(3) Uani 1 1 d GU . . H26' H 1.0633 0.1955 0.6329 0.125 Uiso 1 1 calc R . . C27' C 1.04961(7) 0.22806(8) 0.6608(4) 0.113(3) Uani 1 1 d GU . . H27' H 1.0652 0.2356 0.6330 0.136 Uiso 1 1 calc R . . C28' C 1.02741(8) 0.24082(8) 0.7023(4) 0.123(4) Uani 1 1 d GU . . H28' H 1.0282 0.2569 0.7024 0.147 Uiso 1 1 calc R . . C29' C 1.00406(7) 0.22956(7) 0.7438(3) 0.111(3) Uani 1 1 d GU . . H29' H 0.9892 0.2381 0.7716 0.133 Uiso 1 1 calc R . . C30' C 1.00291(7) 0.20553(7) 0.7437(3) 0.099(3) Uani 1 1 d GU . . H30' H 0.9873 0.1980 0.7715 0.118 Uiso 1 1 calc R . . C31' C 0.91024(7) 0.15798(8) 0.6537(4) 0.062(2) Uani 1 1 d G . . H31C H 0.9131 0.1629 0.7295 0.074 Uiso 1 1 calc R . . H31D H 0.8945 0.1475 0.6517 0.074 Uiso 1 1 calc R . . C32' C 0.90470(7) 0.17899(8) 0.5799(3) 0.066(3) Uani 1 1 d G . . C33' C 0.90665(7) 0.20187(9) 0.4404(3) 0.074(3) Uani 1 1 d G . . C34' C 0.91053(8) 0.21187(11) 0.3389(3) 0.101(4) Uani 1 1 d G . . H34' H 0.9198 0.2043 0.2819 0.121 Uiso 1 1 calc R . . C35' C 0.89911(9) 0.23511(11) 0.3263(4) 0.165(6) Uani 1 1 d G . . H35' H 0.9032 0.2438 0.2637 0.198 Uiso 1 1 calc R . . C36' C 0.88194(8) 0.24434(10) 0.4086(5) 0.174(5) Uani 1 1 d GU . . H36' H 0.8729 0.2583 0.3944 0.208 Uiso 1 1 calc R . . C37' C 0.87767(7) 0.23366(9) 0.5118(4) 0.167(5) Uani 1 1 d GU . . H37' H 0.8675 0.2405 0.5685 0.201 Uiso 1 1 calc R . . C38' C 0.89011(7) 0.21160(9) 0.5218(4) 0.094(4) Uani 1 1 d G . . C39' C 0.87631(6) 0.20184(10) 0.7171(4) 0.103(4) Uani 1 1 d GDU . . H39C H 0.8830 0.2165 0.7452 0.123 Uiso 1 1 calc R . . H39D H 0.8808 0.1899 0.7707 0.123 Uiso 1 1 calc R . . C40' C 0.84435(4) 0.20302(4) 0.70036(17) 0.110(3) Uani 1 1 d GDU . . C41' C 0.82922(4) 0.19054(4) 0.62270(18) 0.157(4) Uani 1 1 d GDU . . H41' H 0.8384 0.1812 0.5721 0.188 Uiso 1 1 calc R . . C42' C 0.80032(4) 0.19211(5) 0.6206(2) 0.179(5) Uani 1 1 d GDU . . H42' H 0.7902 0.1838 0.5686 0.214 Uiso 1 1 calc R . . C43' C 0.78656(4) 0.20614(5) 0.6962(2) 0.171(5) Uani 1 1 d GDU . . H43' H 0.7672 0.2072 0.6948 0.205 Uiso 1 1 calc R . . C44' C 0.80169(4) 0.21862(5) 0.7738(2) 0.144(4) Uani 1 1 d GDU . . H44' H 0.7925 0.2280 0.8244 0.173 Uiso 1 1 calc R . . C45' C 0.83059(4) 0.21705(4) 0.77592(19) 0.131(4) Uani 1 1 d GDU . . H45' H 0.8407 0.2254 0.8279 0.157 Uiso 1 1 calc R . . Cl1 Cl 0.98658(4) 0.11079(5) 0.9034(2) 0.1007(9) Uani 1 1 d GDU . . O11 O 0.99360(5) 0.10805(5) 1.0151(3) 0.169(4) Uani 1 1 d GDU . . O12 O 1.00577(4) 0.12289(5) 0.8674(3) 0.220(5) Uani 1 1 d GU . . O13 O 0.98689(5) 0.09511(5) 0.8182(3) 0.204(5) Uani 1 1 d GU . . O14 O 0.95803(4) 0.11621(4) 0.9117(2) 0.181(4) Uani 1 1 d GU . . Cl2 Cl 0.87150(4) 0.13098(4) 0.87020(19) 0.1243(11) Uani 1 1 d GDU . . O21 O 0.85805(4) 0.12257(4) 0.9546(2) 0.202(4) Uani 1 1 d GDU A . O22 O 0.85756(4) 0.14999(4) 0.82883(17) 0.150(4) Uani 0.60 1 d PGDU A 1 O23 O 0.87375(4) 0.11505(4) 0.7861(2) 0.137(4) Uani 0.50 1 d PGDU A 1 O24 O 0.89824(4) 0.13796(4) 0.89416(17) 0.129(4) Uani 0.50 1 d PGDU A 1 O22' O 0.86167(4) 0.13198(4) 0.77015(19) 0.144(4) Uani 0.40 1 d PGDU A 2 O23' O 0.89571(4) 0.11631(4) 0.8643(2) 0.139(4) Uani 0.50 1 d PGDU A 2 O24' O 0.88362(4) 0.15210(4) 0.89846(16) 0.152(4) Uani 0.50 1 d PGDU A 2 Cl3 Cl 0.92706(4) 0.21199(4) 0.95859(19) 0.1237(12) Uani 1 1 d GDU . . O31 O 0.93713(5) 0.21055(5) 1.0722(2) 0.155(4) Uani 1 1 d GU . . O32 O 0.93071(4) 0.23145(4) 0.8943(2) 0.206(4) Uani 1 1 d GDU . . O33 O 0.93485(4) 0.19264(4) 0.89796(18) 0.158(3) Uani 1 1 d GU . . O34 O 0.89701(4) 0.21096(4) 0.97785(18) 0.176(4) Uani 1 1 d GU . . 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 Tb1 0.06813(16) 0.0582(2) 0.04921(14) 0.0038(2) 0.00426(19) -0.0038(2) N1 0.067(4) 0.048(5) 0.079(5) 0.003(3) 0.010(3) -0.006(3) N2 0.098(4) 0.049(4) 0.054(4) 0.003(4) -0.011(4) 0.002(4) N3 0.069(4) 0.054(5) 0.046(3) 0.004(3) -0.008(3) 0.000(3) N4 0.118(5) 0.069(5) 0.068(5) 0.009(4) 0.012(4) 0.023(5) N5 0.084(4) 0.055(5) 0.050(3) 0.006(3) 0.010(3) 0.000(4) N6 0.065(4) 0.060(5) 0.074(4) -0.008(4) -0.005(3) -0.007(4) N7 0.078(4) 0.052(5) 0.079(4) 0.003(4) 0.024(4) -0.001(4) N8 0.065(3) 0.077(6) 0.033(3) 0.003(3) 0.010(3) -0.005(4) N9 0.080(4) 0.061(5) 0.048(3) 0.009(3) 0.007(3) -0.006(4) N10 0.074(4) 0.102(7) 0.073(5) 0.012(5) 0.008(4) -0.006(5) N11 0.078(4) 0.061(5) 0.062(4) 0.002(4) 0.007(3) -0.012(4) N12 0.075(4) 0.109(6) 0.055(4) -0.009(5) 0.027(4) -0.023(4) N13 0.081(4) 0.060(5) 0.079(5) -0.009(4) 0.008(4) -0.003(4) N14 0.094(5) 0.086(6) 0.088(6) -0.031(5) 0.020(4) -0.016(5) C1 0.114(6) 0.099(8) 0.045(4) 0.016(5) -0.001(5) 0.040(6) C2 0.071(5) 0.068(6) 0.060(5) -0.011(5) 0.000(4) 0.002(5) C3 0.062(4) 0.119(8) 0.043(5) 0.012(5) -0.009(4) -0.010(5) C4 0.069(5) 0.087(7) 0.068(5) -0.016(5) 0.007(4) 0.012(5) C5 0.083(6) 0.130(12) 0.142(11) -0.006(10) 0.036(7) 0.001(7) C6 0.084(5) 0.111(9) 0.092(8) -0.033(7) 0.007(5) 0.005(6) C7 0.068(5) 0.167(13) 0.081(6) 0.014(8) -0.005(5) 0.006(7) C8 0.069(5) 0.108(9) 0.099(7) -0.014(7) -0.003(6) 0.017(6) C16 0.091(5) 0.097(7) 0.051(4) -0.017(6) 0.014(5) -0.004(5) C17 0.093(6) 0.071(7) 0.044(4) -0.009(4) 0.009(4) -0.018(5) C18 0.066(5) 0.088(8) 0.083(6) 0.019(6) 0.004(5) 0.011(5) C19 0.074(5) 0.107(9) 0.066(6) 0.004(6) -0.012(4) -0.017(5) C20 0.107(7) 0.107(11) 0.123(10) 0.014(8) -0.027(7) 0.013(7) C21 0.187(12) 0.102(11) 0.145(12) -0.007(9) -0.036(10) 0.051(10) C22 0.138(9) 0.073(9) 0.138(10) -0.004(8) 0.040(8) 0.022(7) C23 0.079(6) 0.075(8) 0.094(7) -0.025(6) 0.000(5) 0.003(5) C24 0.110(6) 0.083(7) 0.084(5) -0.025(5) 0.013(5) -0.007(5) C25 0.098(5) 0.088(6) 0.089(5) -0.004(5) 0.008(5) -0.015(5) C26 0.133(7) 0.106(7) 0.127(7) -0.005(6) 0.002(6) -0.021(6) C27 0.134(7) 0.123(8) 0.142(7) -0.024(7) 0.006(6) -0.027(6) C28 0.129(7) 0.125(8) 0.147(7) -0.032(7) 0.003(6) -0.019(7) C29 0.138(7) 0.110(7) 0.149(8) -0.014(7) 0.009(7) -0.025(6) C30 0.120(6) 0.108(7) 0.134(7) -0.014(6) 0.012(6) -0.042(6) C9 0.102(6) 0.126(8) 0.106(7) 0.015(6) -0.018(5) 0.030(6) C10 0.130(6) 0.122(7) 0.124(6) 0.017(6) -0.023(6) 0.020(6) C11 0.188(8) 0.150(8) 0.182(8) 0.020(8) 0.012(7) 0.028(7) C12 0.203(8) 0.175(9) 0.207(9) 0.012(8) 0.005(8) 0.046(8) C13 0.208(8) 0.168(8) 0.203(9) -0.005(8) -0.009(8) 0.043(8) C14 0.240(9) 0.184(9) 0.214(9) -0.014(8) -0.009(8) 0.045(8) C15 0.213(8) 0.158(9) 0.190(8) 0.003(8) -0.008(8) 0.043(8) C39 0.115(7) 0.178(9) 0.102(7) 0.007(7) 0.026(6) -0.037(7) C40 0.095(5) 0.175(7) 0.128(6) -0.006(6) 0.013(5) -0.019(6) C41 0.178(8) 0.225(9) 0.188(8) 0.005(8) 0.027(8) -0.004(8) C42 0.164(8) 0.217(9) 0.195(8) 0.018(8) 0.041(7) -0.005(8) C43 0.173(8) 0.221(9) 0.193(8) 0.022(8) 0.030(7) -0.013(8) C44 0.197(9) 0.229(9) 0.207(9) 0.008(8) 0.013(8) -0.015(8) C45 0.163(8) 0.208(9) 0.178(8) 0.003(8) 0.013(7) -0.004(8) C9' 0.096(5) 0.071(6) 0.078(5) 0.009(5) 0.019(5) -0.006(5) C10' 0.099(5) 0.085(6) 0.098(5) 0.027(5) 0.002(5) 0.009(5) C11' 0.123(6) 0.117(7) 0.148(7) 0.044(6) 0.017(6) 0.024(6) C12' 0.159(7) 0.148(8) 0.186(8) 0.044(7) 0.018(7) 0.037(7) C13' 0.169(8) 0.130(8) 0.185(8) 0.032(7) 0.006(7) 0.019(7) C14' 0.160(7) 0.114(7) 0.154(7) 0.034(7) 0.001(7) 0.013(7) C15' 0.133(6) 0.087(7) 0.114(6) 0.035(6) 0.008(6) 0.008(6) C31 0.088(5) 0.070(6) 0.089(6) 0.034(5) 0.006(5) -0.017(5) C32 0.068(4) 0.054(5) 0.057(4) 0.018(4) -0.003(4) -0.002(4) C33 0.082(5) 0.064(6) 0.067(5) 0.018(5) -0.005(5) -0.015(5) C34 0.122(7) 0.073(7) 0.074(6) 0.002(5) -0.007(5) -0.022(6) C35 0.138(8) 0.055(7) 0.081(6) 0.001(6) 0.005(6) -0.008(6) C36 0.091(6) 0.146(12) 0.102(9) -0.013(8) -0.019(6) -0.018(7) C37 0.101(6) 0.114(9) 0.092(7) -0.018(7) 0.035(6) -0.049(6) C38 0.089(6) 0.075(7) 0.068(5) -0.010(5) 0.013(5) -0.023(5) C1' 0.077(5) 0.077(7) 0.049(5) 0.007(4) 0.016(4) -0.006(5) C2' 0.058(4) 0.076(7) 0.075(5) 0.017(5) -0.001(4) -0.011(5) C3' 0.061(4) 0.059(6) 0.067(5) 0.005(5) 0.012(4) -0.008(4) C4' 0.091(6) 0.065(7) 0.064(5) 0.012(4) -0.010(4) -0.017(5) C5' 0.097(6) 0.085(8) 0.091(7) -0.010(6) -0.001(6) -0.010(6) C6' 0.102(6) 0.075(7) 0.086(7) -0.003(6) 0.011(5) -0.031(6) C7' 0.109(7) 0.076(9) 0.130(9) 0.008(7) 0.038(7) -0.020(7) C8' 0.065(5) 0.047(6) 0.086(6) 0.011(5) 0.006(4) 0.002(4) C16' 0.079(4) 0.060(5) 0.035(3) -0.003(4) 0.007(4) 0.013(4) C17' 0.069(5) 0.053(6) 0.071(5) -0.004(5) 0.012(4) 0.007(4) C18' 0.065(4) 0.056(6) 0.073(5) 0.011(5) -0.003(4) -0.007(4) C19' 0.070(5) 0.092(8) 0.059(5) 0.010(5) 0.007(4) 0.002(5) C20' 0.103(6) 0.079(7) 0.089(6) 0.003(6) 0.056(5) 0.016(6) C21' 0.076(5) 0.115(8) 0.098(7) 0.002(8) -0.023(7) -0.016(6) C22' 0.074(5) 0.088(8) 0.114(8) 0.014(7) 0.005(6) 0.018(6) C23' 0.068(5) 0.060(6) 0.066(5) 0.018(4) 0.018(4) -0.006(4) C24' 0.086(5) 0.088(7) 0.067(5) -0.004(5) -0.021(4) 0.004(5) C25' 0.090(5) 0.097(6) 0.078(5) -0.011(5) -0.015(4) -0.013(5) C26' 0.117(6) 0.093(6) 0.102(6) -0.007(6) -0.007(5) -0.013(5) C27' 0.127(6) 0.105(7) 0.107(6) -0.014(6) -0.012(6) -0.012(6) C28' 0.139(7) 0.108(7) 0.122(6) -0.031(6) -0.033(6) -0.004(6) C29' 0.122(6) 0.109(7) 0.102(6) -0.027(6) -0.010(6) -0.009(6) C30' 0.103(6) 0.098(7) 0.095(6) -0.022(5) -0.005(5) 0.000(6) C31' 0.071(4) 0.067(6) 0.047(4) 0.008(5) 0.004(4) -0.006(4) C32' 0.091(6) 0.035(5) 0.073(5) 0.008(4) 0.001(5) 0.003(4) C33' 0.091(6) 0.053(6) 0.079(5) 0.008(5) -0.010(5) 0.003(5) C34' 0.147(9) 0.075(8) 0.081(6) 0.024(6) 0.004(6) 0.032(7) C35' 0.230(13) 0.067(9) 0.198(12) 0.036(9) 0.117(11) 0.034(10) C36' 0.214(9) 0.149(9) 0.158(9) 0.034(8) 0.042(8) 0.053(8) C37' 0.213(9) 0.139(9) 0.149(8) 0.033(8) 0.051(8) 0.047(8) C38' 0.112(7) 0.077(7) 0.093(7) 0.014(6) 0.016(6) 0.046(6) C39' 0.121(7) 0.094(7) 0.093(6) 0.010(6) 0.011(6) 0.011(6) C40' 0.124(6) 0.101(6) 0.104(6) -0.015(5) 0.015(5) 0.016(5) C41' 0.145(7) 0.156(8) 0.168(8) -0.019(8) -0.007(7) 0.005(7) C42' 0.158(7) 0.172(9) 0.206(9) -0.022(8) 0.014(8) 0.001(7) C43' 0.152(7) 0.169(9) 0.191(8) -0.023(8) 0.019(7) 0.008(7) C44' 0.135(7) 0.139(8) 0.158(8) -0.030(7) 0.023(7) 0.025(7) C45' 0.136(7) 0.124(8) 0.132(7) -0.030(7) -0.004(6) 0.016(7) Cl1 0.0846(13) 0.133(2) 0.0846(15) 0.0024(18) 0.0168(14) -0.0007(15) O11 0.183(7) 0.186(9) 0.137(7) 0.027(6) -0.029(6) 0.018(7) O12 0.233(8) 0.216(9) 0.210(9) 0.017(8) 0.041(8) -0.050(8) O13 0.205(8) 0.219(9) 0.187(8) -0.026(8) 0.007(7) 0.018(8) O14 0.164(6) 0.245(9) 0.135(7) -0.004(7) -0.004(6) 0.043(7) Cl2 0.1220(18) 0.161(3) 0.0896(17) 0.0371(19) 0.0382(16) 0.023(2) O21 0.196(7) 0.220(9) 0.190(7) 0.057(7) 0.083(6) -0.009(7) O22 0.154(7) 0.156(7) 0.140(7) 0.014(7) 0.006(6) 0.038(6) O23 0.140(7) 0.139(7) 0.132(7) -0.006(7) 0.026(6) 0.001(7) O24 0.119(6) 0.166(7) 0.102(6) 0.017(7) 0.023(7) 0.021(6) O22' 0.140(7) 0.161(8) 0.133(7) 0.013(7) 0.002(7) 0.003(7) O23' 0.137(7) 0.154(8) 0.125(7) 0.016(7) 0.026(6) 0.022(7) O24' 0.160(7) 0.162(8) 0.132(7) 0.014(7) 0.011(7) 0.019(7) Cl3 0.136(2) 0.119(3) 0.116(2) 0.032(2) -0.0124(19) -0.006(2) O31 0.168(6) 0.154(8) 0.143(6) 0.026(6) -0.018(6) 0.004(6) O32 0.244(8) 0.189(8) 0.185(7) 0.040(9) -0.027(7) -0.012(8) O33 0.174(6) 0.153(7) 0.147(6) 0.002(8) -0.012(6) 0.023(6) O34 0.171(7) 0.190(9) 0.167(7) -0.004(7) 0.000(6) 0.012(7) _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 Tb1 N11 2.456(7) . ? Tb1 N5 2.468(7) . ? Tb1 N7 2.477(7) . ? Tb1 N13 2.493(8) . ? Tb1 N3 2.493(7) . ? Tb1 N9 2.508(7) . ? Tb1 N1 2.651(8) . ? Tb1 N8 2.660(6) . ? N1 C31' 1.489(8) . ? N1 C16' 1.493(7) . ? N1 C1' 1.499(8) . ? N2 C2' 1.332(7) . ? N2 C8' 1.394(7) . ? N2 C9' 1.436(10) . ? N3 C2' 1.361(6) . ? N3 C3' 1.384(7) . ? N4 C32' 1.315(9) . ? N4 C38' 1.407(9) . ? N4 C39' 1.441(8) . ? N5 C32' 1.300(8) . ? N5 C33' 1.422(9) . ? N6 C17' 1.367(7) . ? N6 C23' 1.386(7) . ? N6 C24' 1.481(7) . ? N7 C17' 1.319(8) . ? N7 C18' 1.434(7) . ? N8 C31 1.458(7) . ? N8 C1 1.469(11) . ? N8 C16 1.491(12) . ? N9 C2 1.274(11) . ? N9 C3 1.414(10) . ? N10 C2 1.382(11) . ? N10 C8 1.407(13) . ? N10 C9 1.469(13) . ? N11 C32 1.313(7) . ? N11 C33 1.419(8) . ? N12 C32 1.339(7) . ? N12 C39 1.375(13) . ? N12 C38 1.405(8) . ? N13 C17 1.292(11) . ? N13 C18 1.429(13) . ? N14 C23 1.320(13) . ? N14 C17 1.402(13) . ? N14 C24 1.453(13) . ? C1 C2 1.468(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.361(12) . ? C3 C8 1.414(14) . ? C4 C5 1.331(13) . ? C4 H4 0.9300 . ? C5 C6 1.382(17) . ? C5 H5 0.9300 . ? C6 C7 1.343(16) . ? C6 H6 0.9300 . ? C7 C8 1.355(13) . ? C7 H7 0.9300 . ? C16 C17 1.467(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 C23 1.364(15) . ? C18 C19 1.370(13) . ? C19 C20 1.407(17) . ? C19 H19 0.9300 . ? C20 C21 1.443(19) . ? C20 H20 0.9300 . ? C21 C22 1.377(19) . ? C21 H21 0.9300 . ? C22 C23 1.432(17) . ? C22 H22 0.9300 . ? C24 C25 1.540(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C9 C10 1.443(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C39 C40 1.508(9) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C9' C10' 1.483(13) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C10' C11' 1.3900 . ? C10' C15' 1.3900 . ? C11' C12' 1.3900 . ? C11' H11' 0.9300 . ? C12' C13' 1.3900 . ? C12' H12' 0.9300 . ? C13' C14' 1.3900 . ? C13' H13' 0.9300 . ? C14' C15' 1.3900 . ? C14' H14' 0.9300 . ? C15' H15' 0.9300 . ? C31 C32 1.4856 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C33 C38 1.3786 . ? C33 C34 1.3888 . ? C34 C35 1.4104 . ? C34 H34 0.9300 . ? C35 C36 1.4040 . ? C35 H35 0.9300 . ? C36 C37 1.3909 . ? C36 H36 0.9300 . ? C37 C38 1.4019 . ? C37 H37 0.9300 . ? C1' C2' 1.4945 . ? C1' H1'1 0.9700 . ? C1' H1'2 0.9700 . ? C3' C8' 1.3159 . ? C3' C4' 1.4498 . ? C4' C5' 1.4056 . ? C4' H4' 0.9300 . ? C5' C6' 1.3351 . ? C5' H5' 0.9300 . ? C6' C7' 1.4144 . ? C6' H6' 0.9300 . ? C7' C8' 1.4326 . ? C7' H7' 0.9300 . ? C16' C17' 1.5131 . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C18' C23' 1.3231 . ? C18' C19' 1.4641 . ? C19' C20' 1.4706 . ? C19' H19' 0.9300 . ? C20' C21' 1.3356 . ? C20' H20' 0.9300 . ? C21' C22' 1.5102 . ? C21' H21' 0.9300 . ? C22' C23' 1.4380 . ? C22' H22' 0.9300 . ? C24' C25' 1.538(5) . ? C24' H24C 0.9700 . ? C24' H24D 0.9700 . ? C25' C26' 1.3900 . ? C25' C30' 1.3900 . ? C26' C27' 1.3900 . ? C26' H26' 0.9300 . ? C27' C28' 1.3900 . ? C27' H27' 0.9300 . ? C28' C29' 1.3900 . ? C28' H28' 0.9300 . ? C29' C30' 1.3900 . ? C29' H29' 0.9300 . ? C30' H30' 0.9300 . ? C31' C32' 1.5310 . ? C31' H31C 0.9700 . ? C31' H31D 0.9700 . ? C33' C34' 1.3716 . ? C33' C38' 1.3850 . ? C34' C35' 1.4591 . ? C34' H34' 0.9300 . ? C35' C36' 1.3991 . ? C35' H35' 0.9300 . ? C36' C37' 1.4101 . ? C36' H36' 0.9300 . ? C37' C38' 1.4130 . ? C37' H37' 0.9300 . ? C39' C40' 1.549(4) . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? C40' C41' 1.3900 . ? C40' C45' 1.3900 . ? C41' C42' 1.3900 . ? C41' H41' 0.9300 . ? C42' C43' 1.3900 . ? C42' H42' 0.9300 . ? C43' C44' 1.3900 . ? C43' H43' 0.9300 . ? C44' C45' 1.3900 . ? C44' H44' 0.9300 . ? C45' H45' 0.9300 . ? Cl1 O12 1.2358 . ? Cl1 O13 1.3736 . ? Cl1 O11 1.4031 . ? Cl1 O14 1.4089 . ? Cl2 O22' 1.3018 . ? Cl2 O21 1.3026 . ? Cl2 O24 1.3762 . ? Cl2 O23 1.3774 . ? Cl2 O22 1.3805 . ? Cl2 O24' 1.3945 . ? Cl2 O23' 1.4402 . ? Cl3 O32 1.3788 . ? Cl3 O33 1.3892 . ? Cl3 O31 1.4612 . ? Cl3 O34 1.4619 . ? 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 N11 Tb1 N5 81.9(2) . . ? N11 Tb1 N7 74.7(2) . . ? N5 Tb1 N7 99.6(2) . . ? N11 Tb1 N13 97.3(3) . . ? N5 Tb1 N13 174.8(2) . . ? N7 Tb1 N13 85.1(2) . . ? N11 Tb1 N3 169.5(2) . . ? N5 Tb1 N3 107.2(2) . . ? N7 Tb1 N3 98.3(2) . . ? N13 Tb1 N3 74.1(2) . . ? N11 Tb1 N9 107.7(2) . . ? N5 Tb1 N9 77.2(2) . . ? N7 Tb1 N9 175.5(2) . . ? N13 Tb1 N9 98.3(2) . . ? N3 Tb1 N9 79.8(2) . . ? N11 Tb1 N1 117.2(2) . . ? N5 Tb1 N1 63.4(2) . . ? N7 Tb1 N1 63.0(2) . . ? N13 Tb1 N1 121.2(2) . . ? N3 Tb1 N1 64.5(2) . . ? N9 Tb1 N1 112.5(2) . . ? N11 Tb1 N8 63.4(2) . . ? N5 Tb1 N8 112.2(2) . . ? N7 Tb1 N8 121.4(2) . . ? N13 Tb1 N8 63.1(2) . . ? N3 Tb1 N8 115.9(2) . . ? N9 Tb1 N8 63.0(2) . . ? N1 Tb1 N8 174.9(2) . . ? C31' N1 C16' 109.0(5) . . ? C31' N1 C1' 107.9(5) . . ? C16' N1 C1' 103.8(5) . . ? C31' N1 Tb1 109.4(4) . . ? C16' N1 Tb1 113.7(4) . . ? C1' N1 Tb1 112.7(4) . . ? C2' N2 C8' 105.7(5) . . ? C2' N2 C9' 126.1(7) . . ? C8' N2 C9' 127.5(7) . . ? C2' N3 C3' 101.7(5) . . ? C2' N3 Tb1 119.5(4) . . ? C3' N3 Tb1 136.4(4) . . ? C32' N4 C38' 103.0(5) . . ? C32' N4 C39' 132.4(7) . . ? C38' N4 C39' 124.5(7) . . ? C32' N5 C33' 104.1(6) . . ? C32' N5 Tb1 120.6(5) . . ? C33' N5 Tb1 134.1(4) . . ? C17' N6 C23' 104.7(5) . . ? C17' N6 C24' 126.0(5) . . ? C23' N6 C24' 129.3(5) . . ? C17' N7 C18' 102.2(5) . . ? C17' N7 Tb1 120.5(4) . . ? C18' N7 Tb1 132.6(5) . . ? C31 N8 C1 112.7(6) . . ? C31 N8 C16 106.7(6) . . ? C1 N8 C16 114.1(7) . . ? C31 N8 Tb1 111.1(4) . . ? C1 N8 Tb1 104.4(5) . . ? C16 N8 Tb1 107.8(5) . . ? C2 N9 C3 106.6(7) . . ? C2 N9 Tb1 116.2(6) . . ? C3 N9 Tb1 133.5(5) . . ? C2 N10 C8 105.6(8) . . ? C2 N10 C9 129.5(7) . . ? C8 N10 C9 124.9(7) . . ? C32 N11 C33 105.5(5) . . ? C32 N11 Tb1 119.7(5) . . ? C33 N11 Tb1 131.3(4) . . ? C32 N12 C39 126.0(7) . . ? C32 N12 C38 109.3(5) . . ? C39 N12 C38 122.4(8) . . ? C17 N13 C18 104.5(8) . . ? C17 N13 Tb1 120.2(7) . . ? C18 N13 Tb1 132.6(6) . . ? C23 N14 C17 105.7(8) . . ? C23 N14 C24 128.4(10) . . ? C17 N14 C24 125.5(9) . . ? C2 C1 N8 109.2(8) . . ? C2 C1 H1A 109.8 . . ? N8 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? N8 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N9 C2 N10 114.2(8) . . ? N9 C2 C1 122.0(8) . . ? N10 C2 C1 123.8(8) . . ? C4 C3 N9 135.1(8) . . ? C4 C3 C8 116.7(8) . . ? N9 C3 C8 108.1(7) . . ? C5 C4 C3 120.9(10) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.7(12) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 123.4(10) . . ? C7 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? C6 C7 C8 115.3(11) . . ? C6 C7 H7 122.3 . . ? C8 C7 H7 122.4 . . ? C7 C8 N10 130.6(10) . . ? C7 C8 C3 123.7(11) . . ? N10 C8 C3 105.5(8) . . ? C17 C16 N8 110.4(8) . . ? C17 C16 H16A 109.6 . . ? N8 C16 H16A 109.6 . . ? C17 C16 H16B 109.6 . . ? N8 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N13 C17 N14 112.6(9) . . ? N13 C17 C16 120.2(9) . . ? N14 C17 C16 127.1(8) . . ? C23 C18 C19 122.1(11) . . ? C23 C18 N13 107.7(8) . . ? C19 C18 N13 130.2(10) . . ? C18 C19 C20 118.8(11) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C21 120.4(11) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 118.9(14) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 119.2(13) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? N14 C23 C18 109.4(10) . . ? N14 C23 C22 130.1(11) . . ? C18 C23 C22 120.5(11) . . ? N14 C24 C25 113.0(8) . . ? N14 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? N14 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 120.0 . . ? C26 C25 C24 122.2(5) . . ? C30 C25 C24 117.5(5) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C10 C9 N10 113.2(8) . . ? C10 C9 H9A 108.9 . . ? N10 C9 H9A 108.9 . . ? C10 C9 H9B 109.0 . . ? N10 C9 H9B 108.9 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C15 120.0 . . ? C11 C10 C9 115.9(6) . . ? C15 C10 C9 124.1(6) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? N12 C39 C40 120.3(7) . . ? N12 C39 H39A 107.2 . . ? C40 C39 H39A 107.3 . . ? N12 C39 H39B 107.2 . . ? C40 C39 H39B 107.2 . . ? H39A C39 H39B 106.9 . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 140.1(7) . . ? C45 C40 C39 99.7(7) . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? N2 C9' C10' 113.0(7) . . ? N2 C9' H9'1 109.0 . . ? C10' C9' H9'1 108.9 . . ? N2 C9' H9'2 108.9 . . ? C10' C9' H9'2 109.1 . . ? H9'1 C9' H9'2 107.8 . . ? C11' C10' C15' 120.0 . . ? C11' C10' C9' 122.4(3) . . ? C15' C10' C9' 117.6(3) . . ? C10' C11' C12' 120.0 . . ? C10' C11' H11' 120.0 . . ? C12' C11' H11' 120.0 . . ? C13' C12' C11' 120.0 . . ? C13' C12' H12' 120.0 . . ? C11' C12' H12' 120.0 . . ? C12' C13' C14' 120.0 . . ? C12' C13' H13' 120.0 . . ? C14' C13' H13' 120.0 . . ? C15' C14' C13' 120.0 . . ? C15' C14' H14' 120.0 . . ? C13' C14' H14' 120.0 . . ? C14' C15' C10' 120.0 . . ? C14' C15' H15' 120.0 . . ? C10' C15' H15' 120.0 . . ? N8 C31 C32 108.8(3) . . ? N8 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? N8 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N11 C32 N12 111.5(5) . . ? N11 C32 C31 122.2(3) . . ? N12 C32 C31 125.9(3) . . ? C38 C33 C34 122.3 . . ? C38 C33 N11 109.6(3) . . ? C34 C33 N11 128.1(3) . . ? C33 C34 C35 115.7 . . ? C33 C34 H34 122.1 . . ? C35 C34 H34 122.1 . . ? C36 C35 C34 123.1 . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.4 . . ? C37 C36 C35 118.9 . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 118.4 . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? C33 C38 C37 121.3 . . ? C33 C38 N12 103.7(3) . . ? C37 C38 N12 134.7(3) . . ? C2' C1' N1 110.1(3) . . ? C2' C1' H1'1 109.6 . . ? N1 C1' H1'1 109.6 . . ? C2' C1' H1'2 109.6 . . ? N1 C1' H1'2 109.6 . . ? H1'1 C1' H1'2 108.2 . . ? N2 C2' N3 113.3(4) . . ? N2 C2' C1' 125.2(3) . . ? N3 C2' C1' 121.5(3) . . ? C8' C3' N3 112.8(3) . . ? C8' C3' C4' 121.9 . . ? N3 C3' C4' 125.3(3) . . ? C5' C4' C3' 115.2 . . ? C5' C4' H4' 122.4 . . ? C3' C4' H4' 122.4 . . ? C6' C5' C4' 120.8 . . ? C6' C5' H5' 119.6 . . ? C4' C5' H5' 119.6 . . ? C5' C6' C7' 125.8 . . ? C5' C6' H6' 117.1 . . ? C7' C6' H6' 117.1 . . ? C6' C7' C8' 112.2 . . ? C6' C7' H7' 123.9 . . ? C8' C7' H7' 123.9 . . ? C3' C8' N2 106.5(3) . . ? C3' C8' C7' 124.0 . . ? N2 C8' C7' 129.5(3) . . ? N1 C16' C17' 106.6(3) . . ? N1 C16' H16C 110.4 . . ? C17' C16' H16C 110.4 . . ? N1 C16' H16D 110.4 . . ? C17' C16' H16D 110.4 . . ? H16C C16' H16D 108.6 . . ? N7 C17' N6 114.3(5) . . ? N7 C17' C16' 122.4(3) . . ? N6 C17' C16' 123.3(3) . . ? C23' C18' N7 110.5(3) . . ? C23' C18' C19' 123.1 . . ? N7 C18' C19' 125.8(3) . . ? C18' C19' C20' 110.6 . . ? C18' C19' H19' 124.7 . . ? C20' C19' H19' 124.7 . . ? C21' C20' C19' 126.4 . . ? C21' C20' H20' 116.8 . . ? C19' C20' H20' 116.8 . . ? C20' C21' C22' 121.7 . . ? C20' C21' H21' 119.2 . . ? C22' C21' H21' 119.2 . . ? C23' C22' C21' 110.3 . . ? C23' C22' H22' 124.8 . . ? C21' C22' H22' 124.8 . . ? C18' C23' N6 108.0(3) . . ? C18' C23' C22' 127.5 . . ? N6 C23' C22' 124.4(3) . . ? N6 C24' C25' 111.0(4) . . ? N6 C24' H24C 109.4 . . ? C25' C24' H24C 109.4 . . ? N6 C24' H24D 109.4 . . ? C25' C24' H24D 109.4 . . ? H24C C24' H24D 108.0 . . ? C26' C25' C30' 120.0 . . ? C26' C25' C24' 122.37(17) . . ? C30' C25' C24' 117.63(17) . . ? C27' C26' C25' 120.0 . . ? C27' C26' H26' 120.0 . . ? C25' C26' H26' 120.0 . . ? C26' C27' C28' 120.0 . . ? C26' C27' H27' 120.0 . . ? C28' C27' H27' 120.0 . . ? C29' C28' C27' 120.0 . . ? C29' C28' H28' 120.0 . . ? C27' C28' H28' 120.0 . . ? C30' C29' C28' 120.0 . . ? C30' C29' H29' 120.0 . . ? C28' C29' H29' 120.0 . . ? C29' C30' C25' 120.0 . . ? C29' C30' H30' 120.0 . . ? C25' C30' H30' 120.0 . . ? N1 C31' C32' 107.4(4) . . ? N1 C31' H31C 110.2 . . ? C32' C31' H31C 110.2 . . ? N1 C31' H31D 110.2 . . ? C32' C31' H31D 110.2 . . ? H31C C31' H31D 108.5 . . ? N5 C32' N4 117.7(6) . . ? N5 C32' C31' 120.3(4) . . ? N4 C32' C31' 122.1(4) . . ? C34' C33' C38' 123.0 . . ? C34' C33' N5 130.3(3) . . ? C38' C33' N5 106.2(3) . . ? C33' C34' C35' 115.5 . . ? C33' C34' H34' 122.2 . . ? C35' C34' H34' 122.2 . . ? C36' C35' C34' 119.9 . . ? C36' C35' H35' 120.1 . . ? C34' C35' H35' 120.1 . . ? C35' C36' C37' 123.4 . . ? C35' C36' H36' 118.3 . . ? C37' C36' H36' 118.3 . . ? C36' C37' C38' 114.2 . . ? C36' C37' H37' 122.9 . . ? C38' C37' H37' 122.9 . . ? C33' C38' N4 108.7(4) . . ? C33' C38' C37' 123.2 . . ? N4 C38' C37' 127.9(4) . . ? N4 C39' C40' 109.7(4) . . ? N4 C39' H39C 109.7 . . ? C40' C39' H39C 109.7 . . ? N4 C39' H39D 109.7 . . ? C40' C39' H39D 109.7 . . ? H39C C39' H39D 108.2 . . ? C41' C40' C45' 120.0 . . ? C41' C40' C39' 125.7(2) . . ? C45' C40' C39' 114.2(2) . . ? C40' C41' C42' 120.0 . . ? C40' C41' H41' 120.0 . . ? C42' C41' H41' 120.0 . . ? C43' C42' C41' 120.0 . . ? C43' C42' H42' 120.0 . . ? C41' C42' H42' 120.0 . . ? C44' C43' C42' 120.0 . . ? C44' C43' H43' 120.0 . . ? C42' C43' H43' 120.0 . . ? C45' C44' C43' 120.0 . . ? C45' C44' H44' 120.0 . . ? C43' C44' H44' 120.0 . . ? C44' C45' C40' 120.0 . . ? C44' C45' H45' 120.0 . . ? C40' C45' H45' 120.0 . . ? O12 Cl1 O13 95.7 . . ? O12 Cl1 O11 103.0 . . ? O13 Cl1 O11 130.3 . . ? O12 Cl1 O14 128.6 . . ? O13 Cl1 O14 102.2 . . ? O11 Cl1 O14 101.0 . . ? O22' Cl2 O21 124.5 . . ? O22' Cl2 O24 121.4 . . ? O21 Cl2 O24 114.0 . . ? O22' Cl2 O23 50.9 . . ? O21 Cl2 O23 111.7 . . ? O24 Cl2 O23 106.2 . . ? O22' Cl2 O22 56.7 . . ? O21 Cl2 O22 110.0 . . ? O24 Cl2 O22 107.2 . . ? O23 Cl2 O22 107.6 . . ? O22' Cl2 O24' 109.9 . . ? O21 Cl2 O24' 109.9 . . ? O24 Cl2 O24' 45.8 . . ? O23 Cl2 O24' 137.2 . . ? O22 Cl2 O24' 66.1 . . ? O22' Cl2 O23' 105.8 . . ? O21 Cl2 O23' 102.6 . . ? O24 Cl2 O23' 55.3 . . ? O23 Cl2 O23' 60.4 . . ? O22 Cl2 O23' 147.3 . . ? O24' Cl2 O23' 101.0 . . ? O32 Cl3 O33 108.9 . . ? O32 Cl3 O31 122.4 . . ? O33 Cl3 O31 111.3 . . ? O32 Cl3 O34 104.4 . . ? O33 Cl3 O34 108.5 . . ? O31 Cl3 O34 100.0 . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.885 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.094 #====================================# data_22 _database_code_depnum_ccdc_archive 'CCDC 698717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H75 Cl3 N13 O15 Tb' _chemical_formula_weight 1555.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 13.730(2) _cell_length_b 13.730(2) _cell_length_c 32.236(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5262.7(15) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 257 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2394 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.8135 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku RAXIS II IP' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6155 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.57 _reflns_number_total 3248 _reflns_number_gt 3222 _reflns_threshold_expression >2sigma(I) _computing_data_collection BIOTEX _computing_cell_refinement BIOTEX _computing_data_reduction BIOTEX _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^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 geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00154(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.495(10) _refine_ls_number_reflns 3248 _refine_ls_number_parameters 297 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.005 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 Tb1 Tb 0.6667 1.3333 0.1284 0.04859(6) Uani 1 3 d S . . N1 N 0.6667 1.3333 0.0426(2) 0.0568(14) Uani 1 3 d S . . N2 N 0.7002(3) 1.5091(3) 0.09515(12) 0.0559(9) Uani 1 1 d . . . N3 N 0.7330(3) 1.6264(3) 0.04148(13) 0.0635(9) Uani 1 1 d . . . C1 C 0.6382(4) 1.4179(4) 0.02726(14) 0.0638(11) Uani 1 1 d . . . H1B H 0.5581 1.3866 0.0270 0.080 Uiso 1 1 d R . . H1C H 0.6657 1.4393 -0.0005 0.080 Uiso 1 1 d R . . C2 C 0.6906(3) 1.5161(3) 0.05418(13) 0.0570(10) Uani 1 1 d . . . C3 C 0.7645(4) 1.6901(4) 0.07731(15) 0.0614(11) Uani 1 1 d . . . C4 C 0.8179(4) 1.8071(4) 0.08428(18) 0.0755(14) Uani 1 1 d . . . H4A H 0.8364 1.8591 0.0617 0.080 Uiso 1 1 d R . . C5 C 0.8392(4) 1.8426(4) 0.12430(19) 0.0767(15) Uani 1 1 d . . . H5A H 0.8716 1.9215 0.1299 0.080 Uiso 1 1 d R . . C6 C 0.8191(4) 1.7714(4) 0.15629(19) 0.0773(15) Uani 1 1 d . . . H6A H 0.8387 1.8017 0.1838 0.080 Uiso 1 1 d R . . C7 C 0.7707(4) 1.6570(4) 0.15072(16) 0.0676(12) Uani 1 1 d . . . H7A H 0.7547 1.6063 0.1735 0.080 Uiso 1 1 d R . . C8 C 0.7454(3) 1.6177(3) 0.11043(14) 0.0586(11) Uani 1 1 d . . . C9 C 0.7455(4) 1.6670(4) -0.00063(16) 0.0732(14) Uani 1 1 d . . . H9A H 0.7540 1.6164 -0.0188 0.080 Uiso 1 1 d R . . H9B H 0.8125 1.7392 -0.0025 0.080 Uiso 1 1 d R . . C10 C 0.6463(5) 1.6795(6) -0.01591(19) 0.093(2) Uani 1 1 d . . . H10A H 0.6386 1.7328 0.0010 0.080 Uiso 1 1 d R . . H10B H 0.5782 1.6081 -0.0143 0.080 Uiso 1 1 d R . . C11 C 0.6705(6) 1.7214(6) -0.0606(2) 0.114(3) Uani 1 1 d . . . H11A H 0.6100 1.7298 -0.0715 0.080 Uiso 1 1 d R . . H11B H 0.7391 1.7924 -0.0617 0.080 Uiso 1 1 d R . . H11C H 0.6785 1.6673 -0.0770 0.080 Uiso 1 1 d R . . O1 O 0.6230(3) 1.1819(2) 0.16558(11) 0.0644(9) Uani 1 1 d . . . N4 N 0.6165(3) 0.9457(3) 0.20343(14) 0.0739(11) Uani 1 1 d . . . N5 N 0.6127(3) 1.0097(3) 0.17099(12) 0.0630(10) Uani 1 1 d . . . C12 C 0.6268(3) 1.1086(4) 0.18762(16) 0.0602(12) Uani 1 1 d . . . C13 C 0.6424(4) 1.1038(4) 0.23005(17) 0.0729(14) Uani 1 1 d . . . H13A H 0.6552 1.1611 0.2499 0.080 Uiso 1 1 d R . . C14 C 0.6379(4) 1.0034(4) 0.23874(16) 0.0711(13) Uani 1 1 d . . . C15 C 0.6253(5) 0.8467(5) 0.1955(2) 0.1009(17) Uani 1 1 d . . . H15A H 0.6266 0.8131 0.2215 0.080 Uiso 1 1 d R . . H15B H 0.5622 0.7936 0.1794 0.080 Uiso 1 1 d R . . H15C H 0.6936 0.8682 0.1806 0.080 Uiso 1 1 d R . . C16 C 0.6525(5) 0.9621(6) 0.2790(2) 0.0965(18) Uani 1 1 d . . . H16A H 0.6433 0.8885 0.2755 0.080 Uiso 1 1 d R . . H16B H 0.7269 1.0127 0.2891 0.080 Uiso 1 1 d R . . H16C H 0.5982 0.9585 0.2986 0.080 Uiso 1 1 d R . . C17 C 0.5755(4) 0.9669(4) 0.13067(16) 0.0684(13) Uani 1 1 d . . . C18 C 0.4632(6) 0.9134(6) 0.1204(3) 0.109(2) Uani 1 1 d . . . H18A H 0.4076 0.9034 0.1407 0.080 Uiso 1 1 d R . . C19 C 0.4337(8) 0.8733(7) 0.0803(3) 0.132(3) Uani 1 1 d . . . H19A H 0.3562 0.8392 0.0722 0.158 Uiso 1 1 d R . . C20 C 0.5055(7) 0.8822(6) 0.0519(2) 0.124(3) Uani 1 1 d . . . H20A H 0.4805 0.8503 0.0248 0.080 Uiso 1 1 d R . . C21 C 0.6166(8) 0.9362(6) 0.0616(2) 0.114(3) Uani 1 1 d . . . H21A H 0.6703 0.9444 0.0408 0.080 Uiso 1 1 d R . . C22 C 0.6525(6) 0.9776(5) 0.1012(2) 0.0887(18) Uani 1 1 d . . . H22A H 0.7310 1.0141 0.1081 0.080 Uiso 1 1 d R . . Cl1 Cl 0.6667 1.3333 0.31931(6) 0.0632(4) Uani 1 3 d SD . . O11 O 0.6667 1.3333 0.27548(19) 0.095(2) Uani 1 3 d SD . . O12 O 0.6802(3) 1.2414(3) 0.33384(14) 0.0915(12) Uani 1 1 d D . . Cl2 Cl 0.3333 0.6667 -0.06827(12) 0.1030(9) Uani 1 3 d SD . 1 O21 O 0.3333 0.6667 -0.0250(4) 0.38(2) Uiso 0.67 3 d SPD A 1 O22 O 0.2303(7) 0.6397(9) -0.0876(3) 0.154(3) Uiso 0.67 1 d PD B 1 O21' O 0.3333 0.6667 -0.1101(9) 0.32(4) Uiso 0.33 3 d SPD C 2 O22' O 0.2378(15) 0.6356(18) -0.0463(5) 0.142(6) Uiso 0.33 1 d PD D 2 Cl3 Cl 0.6667 1.3333 -0.09082(8) 0.0941(8) Uani 1 3 d S . . O31 O 0.6667 1.3333 -0.1350(2) 0.136(4) Uani 1 3 d S . . O32 O 0.6938(6) 1.4372(5) -0.07557(19) 0.142(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.05035(7) 0.05035(7) 0.04507(12) 0.000 0.000 0.02518(4) N1 0.0571(19) 0.0571(19) 0.056(3) 0.000 0.000 0.0286(9) N2 0.0782(16) 0.0436(12) 0.0534(18) 0.0025(13) -0.0003(16) 0.0362(11) N3 0.0727(16) 0.0620(15) 0.062(2) 0.0112(16) 0.0027(17) 0.0382(13) C1 0.0725(19) 0.0672(19) 0.056(2) -0.0018(19) -0.003(2) 0.0380(16) C2 0.0690(18) 0.0582(17) 0.048(2) 0.0063(16) 0.0057(18) 0.0352(14) C3 0.0704(19) 0.0617(18) 0.057(2) 0.0115(18) 0.010(2) 0.0368(15) C4 0.087(2) 0.0561(19) 0.080(3) 0.015(2) 0.016(3) 0.0336(18) C5 0.082(2) 0.056(2) 0.088(3) -0.001(2) -0.001(3) 0.0315(18) C6 0.075(2) 0.070(2) 0.085(3) -0.010(2) 0.005(3) 0.0342(19) C7 0.083(2) 0.0638(19) 0.064(3) -0.0044(19) -0.005(2) 0.0420(16) C8 0.0605(16) 0.0609(18) 0.057(2) -0.0010(18) -0.0016(18) 0.0326(14) C9 0.087(3) 0.069(2) 0.064(3) 0.005(2) -0.002(2) 0.0386(19) C10 0.085(3) 0.107(4) 0.070(3) 0.005(3) -0.005(3) 0.036(3) C11 0.128(4) 0.123(4) 0.078(4) 0.025(3) -0.021(4) 0.055(4) O1 0.0781(16) 0.0514(13) 0.0662(19) 0.0110(13) 0.0027(16) 0.0343(12) N4 0.099(2) 0.0720(16) 0.067(2) 0.0134(17) 0.006(2) 0.0554(14) N5 0.0783(18) 0.0657(17) 0.052(2) 0.0120(16) 0.0101(17) 0.0409(14) C12 0.0529(17) 0.0525(18) 0.071(3) 0.001(2) 0.001(2) 0.0230(14) C13 0.081(2) 0.070(2) 0.064(3) -0.008(2) -0.004(2) 0.035(2) C14 0.082(2) 0.085(2) 0.061(3) 0.010(2) 0.006(2) 0.0528(18) C15 0.149(3) 0.095(2) 0.092(4) 0.023(3) 0.023(4) 0.085(2) C16 0.111(3) 0.134(3) 0.079(4) 0.026(3) 0.007(3) 0.087(2) C17 0.079(2) 0.0572(19) 0.066(3) -0.001(2) -0.005(2) 0.0316(17) C18 0.095(3) 0.110(4) 0.121(5) -0.023(4) -0.028(4) 0.050(3) C19 0.138(5) 0.100(4) 0.133(6) -0.029(4) -0.058(5) 0.041(4) C20 0.195(6) 0.111(4) 0.080(4) -0.022(3) -0.047(4) 0.087(4) C21 0.183(6) 0.106(4) 0.056(3) -0.010(3) -0.004(4) 0.076(4) C22 0.116(4) 0.082(3) 0.066(3) -0.003(3) 0.007(3) 0.047(3) Cl1 0.0656(6) 0.0656(6) 0.0586(10) 0.000 0.000 0.0328(3) O11 0.116(3) 0.116(3) 0.054(3) 0.000 0.000 0.0581(16) O12 0.1037(19) 0.0813(17) 0.102(3) 0.000(2) -0.019(2) 0.0555(15) Cl2 0.0931(10) 0.0931(10) 0.123(2) 0.000 0.000 0.0465(5) Cl3 0.1130(12) 0.1130(12) 0.0565(12) 0.000 0.000 0.0565(6) O31 0.179(5) 0.179(5) 0.050(4) 0.000 0.000 0.089(3) O32 0.207(5) 0.132(4) 0.092(3) -0.015(3) 0.003(4) 0.088(4) _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 Tb1 O1 2.206(3) . ? Tb1 O1 2.206(3) 2_775 ? Tb1 O1 2.206(3) 3_575 ? Tb1 N2 2.465(3) 3_575 ? Tb1 N2 2.465(3) 2_775 ? Tb1 N2 2.465(3) . ? Tb1 N1 2.765(7) . ? N1 C1 1.483(5) 3_575 ? N1 C1 1.483(5) 2_775 ? N1 C1 1.483(5) . ? N2 C2 1.335(6) . ? N2 C8 1.388(5) . ? N3 C3 1.381(6) . ? N3 C2 1.385(5) . ? N3 C9 1.444(6) . ? C1 C2 1.456(6) . ? C1 H1B 0.9600 . ? C1 H1C 0.9599 . ? C3 C8 1.392(6) . ? C3 C4 1.411(6) . ? C4 C5 1.358(8) . ? C4 H4A 0.9600 . ? C5 C6 1.351(8) . ? C5 H5A 0.9600 . ? C6 C7 1.377(7) . ? C6 H6A 0.9599 . ? C7 C8 1.383(7) . ? C7 H7A 0.9599 . ? C9 C10 1.536(9) . ? C9 H9A 0.9599 . ? C9 H9B 0.9600 . ? C10 C11 1.526(9) . ? C10 H10A 0.9599 . ? C10 H10B 0.9600 . ? C11 H11A 0.9599 . ? C11 H11B 0.9601 . ? C11 H11C 0.9600 . ? O1 C12 1.254(6) . ? N4 C14 1.333(7) . ? N4 N5 1.383(6) . ? N4 C15 1.446(7) . ? N5 C12 1.381(6) . ? N5 C17 1.413(6) . ? C12 C13 1.391(7) . ? C13 C14 1.379(8) . ? C13 H13A 0.9599 . ? C14 C16 1.469(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9599 . ? C16 H16A 0.9599 . ? C16 H16B 0.9601 . ? C16 H16C 0.9600 . ? C17 C18 1.376(8) . ? C17 C22 1.375(9) . ? C18 C19 1.384(11) . ? C18 H18A 0.9599 . ? C19 C20 1.307(13) . ? C19 H19A 0.9601 . ? C20 C21 1.358(12) . ? C20 H20A 0.9601 . ? C21 C22 1.384(9) . ? C21 H21A 0.9599 . ? C22 H22A 0.9600 . ? Cl1 O11 1.413(6) . ? Cl1 O12 1.443(4) . ? Cl1 O12 1.443(4) 2_775 ? Cl1 O12 1.443(4) 3_575 ? Cl2 O21 1.396(14) . ? Cl2 O22 1.414(9) . ? Cl2 O22 1.414(9) 3_565 ? Cl2 O22 1.414(9) 2_665 ? Cl3 O32 1.373(7) 3_575 ? Cl3 O32 1.373(7) 2_775 ? Cl3 O32 1.373(7) . ? Cl3 O31 1.425(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O1 93.33(13) . 2_775 ? O1 Tb1 O1 93.33(13) . 3_575 ? O1 Tb1 O1 93.33(13) 2_775 3_575 ? O1 Tb1 N2 85.85(13) . 3_575 ? O1 Tb1 N2 78.03(13) 2_775 3_575 ? O1 Tb1 N2 171.25(14) 3_575 3_575 ? O1 Tb1 N2 78.03(13) . 2_775 ? O1 Tb1 N2 171.25(13) 2_775 2_775 ? O1 Tb1 N2 85.85(13) 3_575 2_775 ? N2 Tb1 N2 102.46(10) 3_575 2_775 ? O1 Tb1 N2 171.25(14) . . ? O1 Tb1 N2 85.85(13) 2_775 . ? O1 Tb1 N2 78.03(13) 3_575 . ? N2 Tb1 N2 102.46(10) 3_575 . ? N2 Tb1 N2 102.46(10) 2_775 . ? O1 Tb1 N1 122.87(9) . . ? O1 Tb1 N1 122.87(9) 2_775 . ? O1 Tb1 N1 122.87(9) 3_575 . ? N2 Tb1 N1 64.20(9) 3_575 . ? N2 Tb1 N1 64.20(9) 2_775 . ? N2 Tb1 N1 64.20(9) . . ? C1 N1 C1 109.4(3) 3_575 2_775 ? C1 N1 C1 109.4(3) 3_575 . ? C1 N1 C1 109.4(3) 2_775 . ? C1 N1 Tb1 109.5(3) 3_575 . ? C1 N1 Tb1 109.5(3) 2_775 . ? C1 N1 Tb1 109.5(3) . . ? C2 N2 C8 106.3(4) . . ? C2 N2 Tb1 121.6(3) . . ? C8 N2 Tb1 131.4(3) . . ? C3 N3 C2 105.8(4) . . ? C3 N3 C9 127.0(4) . . ? C2 N3 C9 127.1(4) . . ? C2 C1 N1 108.9(4) . . ? C2 C1 H1B 110.2 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1C 109.6 . . ? N1 C1 H1C 109.6 . . ? H1B C1 H1C 108.4 . . ? N2 C2 N3 111.6(4) . . ? N2 C2 C1 122.9(4) . . ? N3 C2 C1 125.4(4) . . ? N3 C3 C8 107.6(4) . . ? N3 C3 C4 132.4(4) . . ? C8 C3 C4 119.7(4) . . ? C5 C4 C3 117.1(5) . . ? C5 C4 H4A 121.6 . . ? C3 C4 H4A 121.3 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 118.6 . . ? C5 C6 C7 122.2(5) . . ? C5 C6 H6A 118.7 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C8 116.9(5) . . ? C6 C7 H7A 122.1 . . ? C8 C7 H7A 121.0 . . ? C7 C8 N2 130.1(4) . . ? C7 C8 C3 121.4(4) . . ? N2 C8 C3 108.6(4) . . ? N3 C9 C10 113.8(5) . . ? N3 C9 H9A 109.3 . . ? C10 C9 H9A 108.7 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 107.9(6) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 110.2 . . ? C11 C10 H10B 110.8 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.8 . . ? C10 C11 H11A 110.6 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 108.4 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 O1 Tb1 164.3(3) . . ? C14 N4 N5 109.6(4) . . ? C14 N4 C15 127.7(5) . . ? N5 N4 C15 120.8(5) . . ? C12 N5 N4 107.4(4) . . ? C12 N5 C17 127.6(4) . . ? N4 N5 C17 123.5(4) . . ? O1 C12 N5 121.8(5) . . ? O1 C12 C13 131.6(5) . . ? N5 C12 C13 106.5(4) . . ? C14 C13 C12 108.4(5) . . ? C14 C13 H13A 125.6 . . ? C12 C13 H13A 126.0 . . ? N4 C14 C13 107.9(5) . . ? N4 C14 C16 123.9(5) . . ? C13 C14 C16 128.2(5) . . ? N4 C15 H15A 109.3 . . ? N4 C15 H15B 110.0 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.1 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.2 . . ? C14 C16 H16B 108.7 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 110.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.2(6) . . ? C18 C17 N5 121.2(6) . . ? C22 C17 N5 119.6(5) . . ? C17 C18 C19 117.6(8) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 121.6 . . ? C20 C19 C18 124.2(8) . . ? C20 C19 H19A 117.0 . . ? C18 C19 H19A 118.8 . . ? C19 C20 C21 118.6(7) . . ? C19 C20 H20A 120.9 . . ? C21 C20 H20A 120.5 . . ? C20 C21 C22 120.6(8) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 120.0 . . ? C17 C22 C21 119.8(7) . . ? C17 C22 H22A 119.8 . . ? C21 C22 H22A 120.4 . . ? O11 Cl1 O12 108.9(2) . . ? O11 Cl1 O12 108.9(2) . 2_775 ? O12 Cl1 O12 110.0(2) . 2_775 ? O11 Cl1 O12 108.9(2) . 3_575 ? O12 Cl1 O12 110.0(2) . 3_575 ? O12 Cl1 O12 110.0(2) 2_775 3_575 ? O21 Cl2 O22 116.1(4) . . ? O21 Cl2 O22 116.1(4) . 3_565 ? O22 Cl2 O22 102.1(5) . 3_565 ? O21 Cl2 O22 116.1(4) . 2_665 ? O22 Cl2 O22 102.1(5) . 2_665 ? O22 Cl2 O22 102.1(5) 3_565 2_665 ? O32 Cl3 O32 107.9(3) 3_575 2_775 ? O32 Cl3 O32 107.9(3) 3_575 . ? O32 Cl3 O32 107.9(3) 2_775 . ? O32 Cl3 O31 111.0(3) 3_575 . ? O32 Cl3 O31 111.0(3) 2_775 . ? O32 Cl3 O31 111.0(3) . . ? 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 O1 Tb1 N1 C1 -90.3(2) . . . 3_575 ? O1 Tb1 N1 C1 29.7(2) 2_775 . . 3_575 ? O1 Tb1 N1 C1 149.7(2) 3_575 . . 3_575 ? N2 Tb1 N1 C1 -24.36(19) 3_575 . . 3_575 ? N2 Tb1 N1 C1 -144.36(19) 2_775 . . 3_575 ? N2 Tb1 N1 C1 95.64(19) . . . 3_575 ? O1 Tb1 N1 C1 29.7(2) . . . 2_775 ? O1 Tb1 N1 C1 149.7(2) 2_775 . . 2_775 ? O1 Tb1 N1 C1 -90.3(2) 3_575 . . 2_775 ? N2 Tb1 N1 C1 95.64(19) 3_575 . . 2_775 ? N2 Tb1 N1 C1 -24.36(19) 2_775 . . 2_775 ? N2 Tb1 N1 C1 -144.36(19) . . . 2_775 ? O1 Tb1 N1 C1 149.7(2) . . . . ? O1 Tb1 N1 C1 -90.3(2) 2_775 . . . ? O1 Tb1 N1 C1 29.7(2) 3_575 . . . ? N2 Tb1 N1 C1 -144.36(19) 3_575 . . . ? N2 Tb1 N1 C1 95.64(19) 2_775 . . . ? N2 Tb1 N1 C1 -24.36(19) . . . . ? O1 Tb1 N2 C2 -138.1(8) . . . . ? O1 Tb1 N2 C2 136.9(4) 2_775 . . . ? O1 Tb1 N2 C2 -128.8(4) 3_575 . . . ? N2 Tb1 N2 C2 60.1(3) 3_575 . . . ? N2 Tb1 N2 C2 -45.9(3) 2_775 . . . ? N1 Tb1 N2 C2 7.1(3) . . . . ? O1 Tb1 N2 C8 52.5(10) . . . . ? O1 Tb1 N2 C8 -32.5(4) 2_775 . . . ? O1 Tb1 N2 C8 61.8(4) 3_575 . . . ? N2 Tb1 N2 C8 -109.3(4) 3_575 . . . ? N2 Tb1 N2 C8 144.8(4) 2_775 . . . ? N1 Tb1 N2 C8 -162.3(4) . . . . ? C1 N1 C1 C2 -82.3(6) 3_575 . . . ? C1 N1 C1 C2 157.9(4) 2_775 . . . ? Tb1 N1 C1 C2 37.8(3) . . . . ? C8 N2 C2 N3 2.9(5) . . . . ? Tb1 N2 C2 N3 -168.8(3) . . . . ? C8 N2 C2 C1 -175.2(4) . . . . ? Tb1 N2 C2 C1 13.1(6) . . . . ? C3 N3 C2 N2 -3.6(5) . . . . ? C9 N3 C2 N2 174.3(4) . . . . ? C3 N3 C2 C1 174.5(4) . . . . ? C9 N3 C2 C1 -7.6(8) . . . . ? N1 C1 C2 N2 -36.6(6) . . . . ? N1 C1 C2 N3 145.5(4) . . . . ? C2 N3 C3 C8 2.7(5) . . . . ? C9 N3 C3 C8 -175.2(5) . . . . ? C2 N3 C3 C4 176.1(5) . . . . ? C9 N3 C3 C4 -1.8(9) . . . . ? N3 C3 C4 C5 -178.6(5) . . . . ? C8 C3 C4 C5 -5.8(8) . . . . ? C3 C4 C5 C6 5.2(9) . . . . ? C4 C5 C6 C7 -3.0(9) . . . . ? C5 C6 C7 C8 1.3(8) . . . . ? C6 C7 C8 N2 177.8(5) . . . . ? C6 C7 C8 C3 -2.2(7) . . . . ? C2 N2 C8 C7 178.9(5) . . . . ? Tb1 N2 C8 C7 -10.5(7) . . . . ? C2 N2 C8 C3 -1.1(5) . . . . ? Tb1 N2 C8 C3 169.5(3) . . . . ? N3 C3 C8 C7 178.9(4) . . . . ? C4 C3 C8 C7 4.5(7) . . . . ? N3 C3 C8 N2 -1.1(5) . . . . ? C4 C3 C8 N2 -175.5(4) . . . . ? C3 N3 C9 C10 -87.6(6) . . . . ? C2 N3 C9 C10 94.9(6) . . . . ? N3 C9 C10 C11 -179.4(5) . . . . ? O1 Tb1 O1 C12 -32.0(13) 2_775 . . . ? O1 Tb1 O1 C12 -125.6(12) 3_575 . . . ? N2 Tb1 O1 C12 45.7(13) 3_575 . . . ? N2 Tb1 O1 C12 149.4(13) 2_775 . . . ? N2 Tb1 O1 C12 -116.4(14) . . . . ? N1 Tb1 O1 C12 101.2(13) . . . . ? C14 N4 N5 C12 -3.1(5) . . . . ? C15 N4 N5 C12 -168.4(4) . . . . ? C14 N4 N5 C17 -170.3(5) . . . . ? C15 N4 N5 C17 24.5(7) . . . . ? Tb1 O1 C12 N5 -101.7(12) . . . . ? Tb1 O1 C12 C13 79.4(15) . . . . ? N4 N5 C12 O1 -177.4(4) . . . . ? C17 N5 C12 O1 -10.9(7) . . . . ? N4 N5 C12 C13 1.8(5) . . . . ? C17 N5 C12 C13 168.3(4) . . . . ? O1 C12 C13 C14 179.2(5) . . . . ? N5 C12 C13 C14 0.2(5) . . . . ? N5 N4 C14 C13 3.2(6) . . . . ? C15 N4 C14 C13 167.1(5) . . . . ? N5 N4 C14 C16 -177.3(5) . . . . ? C15 N4 C14 C16 -13.3(8) . . . . ? C12 C13 C14 N4 -2.1(6) . . . . ? C12 C13 C14 C16 178.4(5) . . . . ? C12 N5 C17 C18 -79.0(7) . . . . ? N4 N5 C17 C18 85.5(7) . . . . ? C12 N5 C17 C22 101.8(6) . . . . ? N4 N5 C17 C22 -93.7(6) . . . . ? C22 C17 C18 C19 -0.4(10) . . . . ? N5 C17 C18 C19 -179.6(6) . . . . ? C17 C18 C19 C20 0.7(14) . . . . ? C18 C19 C20 C21 -1.6(14) . . . . ? C19 C20 C21 C22 2.2(13) . . . . ? C18 C17 C22 C21 1.0(10) . . . . ? N5 C17 C22 C21 -179.7(6) . . . . ? C20 C21 C22 C17 -1.9(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.400 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.072 #=======================================# data_27 _database_code_depnum_ccdc_archive 'CCDC 698718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H42.50 N16 O23 Sm' _chemical_formula_weight 1397.86 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' Sm Sm -0.1638 3.4418 '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 14.1569(11) _cell_length_b 21.2008(16) _cell_length_c 21.2720(16) _cell_angle_alpha 90.00 _cell_angle_beta 107.7700(10) _cell_angle_gamma 90.00 _cell_volume 6079.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2826 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7421 _exptl_absorpt_correction_T_max 0.8163 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37860 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12909 _reflns_number_gt 10036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+7.0000P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12909 _refine_ls_number_parameters 885 _refine_ls_number_restraints 867 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.018 _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 Sm1 Sm 0.803009(13) 0.823966(8) 0.085025(8) 0.03854(5) Uani 1 1 d . A . N1 N 0.7467(2) 0.89631(14) 0.17595(13) 0.0451(7) Uani 1 1 d . A . N2 N 0.7047(2) 0.76976(14) 0.15640(14) 0.0478(8) Uani 1 1 d . . . N3 N 0.5794(2) 0.77123(17) 0.19929(16) 0.0590(9) Uani 1 1 d . . . N4 N 0.6782(2) 0.91858(14) 0.04419(14) 0.0486(8) Uani 1 1 d . . . N5 N 0.6532(2) 1.02178(14) 0.05130(16) 0.0528(8) Uani 1 1 d . . . N6 N 0.9381(2) 0.88546(15) 0.17546(14) 0.0488(8) Uani 1 1 d . A . N7 N 1.0042(3) 0.9172(2) 0.27808(19) 0.0826(13) Uani 1 1 d U . . N8 N 0.8832(3) 0.95001(15) -0.00656(15) 0.0537(9) Uani 1 1 d . . . N9 N 0.9679(3) 0.91532(16) -0.20728(16) 0.0598(9) Uani 1 1 d . . . N10 N 0.7499(3) 0.76500(17) -0.14658(15) 0.0656(10) Uani 1 1 d . . . N11 N 0.9928(3) 0.73936(19) 0.21172(17) 0.0668(11) Uani 1 1 d U . . N13 N 1.0717(4) 0.7463(3) -0.0001(2) 0.1099(15) Uani 1 1 d U . . N14 N 0.5651(3) 0.7477(2) -0.0113(2) 0.0865(14) Uani 1 1 d U B . N15 N 0.5482(4) 0.5722(2) -0.1635(2) 0.1014(17) Uani 1 1 d U . . N16 N 0.8637(4) 0.6207(3) 0.0060(3) 0.1198(19) Uani 1 1 d U . . C1 C 0.6495(3) 0.87447(19) 0.17955(19) 0.0523(9) Uani 1 1 d U . . H1A H 0.5972 0.8909 0.1422 0.063 Uiso 1 1 calc R . . H1B H 0.6388 0.8903 0.2196 0.063 Uiso 1 1 calc R . . C2 C 0.6451(3) 0.80453(19) 0.17914(17) 0.0469(9) Uani 1 1 d U . . C3 C 0.6779(3) 0.70729(19) 0.16477(19) 0.0565(10) Uani 1 1 d U . . C4 C 0.7190(4) 0.6511(2) 0.1532(2) 0.0725(12) Uani 1 1 d U . . H4 H 0.7729 0.6495 0.1370 0.087 Uiso 1 1 calc R . . C5 C 0.6735(5) 0.5965(3) 0.1678(3) 0.0933(16) Uani 1 1 d U . . H5A H 0.6982 0.5574 0.1606 0.112 Uiso 1 1 calc R . . C6 C 0.5928(5) 0.5982(3) 0.1925(3) 0.1015(16) Uani 1 1 d U . . H6A H 0.5651 0.5605 0.2006 0.122 Uiso 1 1 calc R . . C7 C 0.5534(4) 0.6542(3) 0.2051(3) 0.0899(14) Uani 1 1 d U . . H7A H 0.5003 0.6558 0.2222 0.108 Uiso 1 1 calc R . . C8 C 0.5983(4) 0.7082(2) 0.1907(2) 0.0675(12) Uani 1 1 d U . . C9 C 0.5011(3) 0.7943(3) 0.2248(2) 0.0821(14) Uani 1 1 d DU . . H9A H 0.4946 0.7655 0.2586 0.099 Uiso 1 1 calc R . . H9B H 0.5211 0.8349 0.2456 0.099 Uiso 1 1 calc R . . C10 C 0.4051(5) 0.8012(3) 0.1757(3) 0.1047(15) Uani 1 1 d DU . . H10A H 0.3540 0.8173 0.1899 0.126 Uiso 1 1 calc R . . C11 C 0.3836(5) 0.7869(3) 0.1132(3) 0.1152(17) Uani 1 1 d DU . . H11A H 0.4323 0.7706 0.0967 0.138 Uiso 1 1 calc R . . H11B H 0.3195 0.7929 0.0852 0.138 Uiso 1 1 calc R . . C12 C 0.7390(3) 0.96296(17) 0.15611(18) 0.0516(10) Uani 1 1 d U . . H12A H 0.8046 0.9815 0.1668 0.062 Uiso 1 1 calc R . . H12B H 0.7014 0.9860 0.1798 0.062 Uiso 1 1 calc R . . C13 C 0.6878(3) 0.96734(17) 0.08283(18) 0.0474(9) Uani 1 1 d U . . C14 C 0.6336(3) 0.94242(19) -0.01891(18) 0.0510(9) Uani 1 1 d U . . C15 C 0.6037(3) 0.9132(2) -0.0802(2) 0.0643(11) Uani 1 1 d U . . H15A H 0.6096 0.8698 -0.0840 0.077 Uiso 1 1 calc R . . C16 C 0.5648(4) 0.9507(3) -0.1356(2) 0.0746(13) Uani 1 1 d U . . H16A H 0.5454 0.9320 -0.1771 0.090 Uiso 1 1 calc R . . C17 C 0.5541(4) 1.0153(3) -0.1304(2) 0.0791(13) Uani 1 1 d U . . H17A H 0.5283 1.0390 -0.1686 0.095 Uiso 1 1 calc R . . C18 C 0.5810(3) 1.0452(2) -0.0699(2) 0.0698(12) Uani 1 1 d U . . H18A H 0.5738 1.0886 -0.0663 0.084 Uiso 1 1 calc R . . C19 C 0.6194(3) 1.00710(19) -0.01457(19) 0.0535(10) Uani 1 1 d U . . C20 C 0.6545(4) 1.0841(2) 0.0799(3) 0.0786(14) Uani 1 1 d DU . . H20A H 0.5944 1.1058 0.0551 0.094 Uiso 1 1 calc R . . H20B H 0.6513 1.0787 0.1245 0.094 Uiso 1 1 calc R . . C21 C 0.7361(4) 1.1243(4) 0.0830(4) 0.1274(18) Uani 1 1 d DU . . H21A H 0.7331 1.1645 0.0997 0.153 Uiso 1 1 calc R . . C22 C 0.8093(5) 1.1127(4) 0.0664(4) 0.152(2) Uani 1 1 d DU . . H22A H 0.8166 1.0732 0.0494 0.183 Uiso 1 1 calc R . . H22B H 0.8581 1.1432 0.0709 0.183 Uiso 1 1 calc R . . C23 C 0.8243(3) 0.8890(2) 0.24063(18) 0.0567(10) Uani 1 1 d U . . H23A H 0.8153 0.9204 0.2714 0.068 Uiso 1 1 calc R A . H23B H 0.8194 0.8475 0.2588 0.068 Uiso 1 1 calc R . . C24 C 0.9209(3) 0.89659(19) 0.23094(18) 0.0547(10) Uani 1 1 d U A . C25 C 1.0379(3) 0.89948(19) 0.1849(2) 0.0556(10) Uani 1 1 d U . . C26 C 1.0947(3) 0.8998(2) 0.1422(2) 0.0645(12) Uani 1 1 d U A . H26A H 1.0682 0.8864 0.0987 0.077 Uiso 1 1 calc R . . C27 C 1.1914(4) 0.9204(3) 0.1659(3) 0.0810(14) Uani 1 1 d U . . H27A H 1.2300 0.9209 0.1375 0.097 Uiso 1 1 calc R A . C28 C 1.2310(4) 0.9393(3) 0.2272(3) 0.1043(18) Uani 1 1 d U A . H28A H 1.2973 0.9514 0.2410 0.125 Uiso 1 1 calc R . . C29 C 1.1770(4) 0.9418(3) 0.2722(3) 0.1078(19) Uani 1 1 d U . . H29A H 1.2045 0.9569 0.3149 0.129 Uiso 1 1 calc R A . C30 C 1.0785(4) 0.9200(3) 0.2491(2) 0.0772(14) Uani 1 1 d U A . C34 C 0.8219(3) 0.85214(17) -0.06953(16) 0.0426(8) Uani 1 1 d U . . C35 C 0.8765(3) 0.90947(17) -0.06287(16) 0.0451(9) Uani 1 1 d U . . C36 C 0.9224(3) 0.93066(18) -0.10689(17) 0.0479(9) Uani 1 1 d U . . H36A H 0.9571 0.9686 -0.0998 0.057 Uiso 1 1 calc R . . C37 C 0.9161(3) 0.89462(18) -0.16197(17) 0.0508(9) Uani 1 1 d U . . C38 C 0.8598(3) 0.83969(19) -0.17482(18) 0.0541(10) Uani 1 1 d U . . H38A H 0.8543 0.8162 -0.2127 0.065 Uiso 1 1 calc R . . C39 C 0.8132(3) 0.82115(16) -0.13078(18) 0.0476(9) Uani 1 1 d U . . C46 C 0.7188(3) 0.68778(18) 0.00015(19) 0.0539(10) Uani 1 1 d U B . C47 C 0.6155(4) 0.6960(2) -0.0311(2) 0.0630(12) Uani 1 1 d U . . C48 C 0.5590(4) 0.6584(2) -0.0822(2) 0.0763(14) Uani 1 1 d U . . H48A H 0.4912 0.6652 -0.1004 0.092 Uiso 1 1 calc R . . C49 C 0.6055(4) 0.6108(2) -0.1053(2) 0.0757(14) Uani 1 1 d U . . C50 C 0.7048(4) 0.5988(2) -0.0782(2) 0.0739(13) Uani 1 1 d U . . H50A H 0.7360 0.5670 -0.0946 0.089 Uiso 1 1 calc R . . C51 C 0.7563(4) 0.6356(2) -0.0262(2) 0.0678(12) Uani 1 1 d U . . O1 O 0.78236(19) 0.82989(11) -0.02815(12) 0.0473(6) Uani 1 1 d U . . O2 O 0.8789(2) 0.92766(13) 0.04528(12) 0.0582(7) Uani 1 1 d U . . O3 O 0.8935(3) 1.00703(15) -0.01333(16) 0.0817(10) Uani 1 1 d U . . O4 O 1.0287(2) 0.95731(17) -0.19048(16) 0.0777(9) Uani 1 1 d U . . O5 O 0.9470(3) 0.88960(17) -0.26162(16) 0.0892(10) Uani 1 1 d U . . O6 O 0.7803(3) 0.71998(17) -0.16776(19) 0.0971(11) Uani 1 1 d U . . O7 O 0.6678(3) 0.76781(18) -0.14078(17) 0.0876(10) Uani 1 1 d U . . O8 O 0.95669(18) 0.78729(12) 0.08092(12) 0.0519(7) Uani 1 1 d U . . O9 O 0.9057(2) 0.75403(14) 0.18921(13) 0.0609(8) Uani 1 1 d U A . O10 O 1.0367(3) 0.7399(2) 0.27055(18) 0.1019(13) Uani 1 1 d U . . O13 O 1.1130(5) 0.7236(3) -0.0337(3) 0.164(2) Uani 1 1 d U . . O14 O 1.0401(4) 0.7982(3) -0.0147(3) 0.1562(18) Uani 1 1 d U . . O15 O 0.7724(2) 0.72121(12) 0.04563(13) 0.0566(7) Uani 1 1 d U . . O16 O 0.6086(3) 0.79185(15) 0.01967(15) 0.0725(9) Uani 1 1 d U . . O17 O 0.4735(4) 0.7437(3) -0.0257(3) 0.1502(19) Uani 1 1 d U . . O18 O 0.5954(4) 0.5386(2) -0.1880(2) 0.1278(16) Uani 1 1 d U . . O19 O 0.4584(5) 0.5804(3) -0.1796(3) 0.1483(19) Uani 1 1 d U . . O20 O 0.9100(6) 0.6070(4) -0.0285(4) 0.202(2) Uani 1 1 d U . . O21 O 0.8949(4) 0.6189(3) 0.0631(3) 0.151(2) Uani 1 1 d U . . C31 C 1.0134(13) 0.9476(8) 0.3395(7) 0.1526(19) Uani 0.50 1 d PDU A 1 H31A H 1.0389 0.9899 0.3383 0.183 Uiso 0.50 1 calc PR A 1 H31B H 0.9482 0.9513 0.3451 0.183 Uiso 0.50 1 calc PR A 1 C32 C 1.0769(10) 0.9150(8) 0.3945(7) 0.156(2) Uani 0.40 1 d PDU A 1 H32A H 1.0682 0.8718 0.3979 0.187 Uiso 0.40 1 calc PR A 1 C33 C 1.1481(13) 0.9434(10) 0.4411(9) 0.158(2) Uani 0.40 1 d PDU A 1 H33A H 1.1582 0.9866 0.4386 0.190 Uiso 0.40 1 calc PR A 1 H33B H 1.1881 0.9202 0.4763 0.190 Uiso 0.40 1 calc PR A 1 C31' C 1.0139(13) 0.9018(4) 0.3529(8) 0.149(3) Uani 0.50 1 d PDU A 2 H31C H 0.9626 0.8726 0.3557 0.179 Uiso 0.50 1 calc PR A 2 H31D H 1.0783 0.8836 0.3754 0.179 Uiso 0.50 1 calc PR A 2 C32' C 1.0027(12) 0.9598(4) 0.3799(6) 0.1624(19) Uani 0.60 1 d PDU A 2 H32B H 1.0116 0.9599 0.4251 0.195 Uiso 0.60 1 calc PR A 2 C33' C 0.9815(7) 1.0141(4) 0.3506(7) 0.1617(18) Uani 0.60 1 d PDU A 2 H33C H 0.9717 1.0173 0.3054 0.194 Uiso 0.60 1 calc PR A 2 H33D H 0.9761 1.0497 0.3748 0.194 Uiso 0.60 1 calc PR A 2 C40 C 1.0227(3) 0.7465(2) 0.1032(2) 0.0569(10) Uani 1 1 d U B 1 C41 C 1.0508(4) 0.7232(3) 0.1703(3) 0.0601(16) Uani 0.70 1 d PDU B 1 C42 C 1.1282(5) 0.6833(3) 0.1979(4) 0.0828(19) Uani 0.70 1 d PDU B 1 H42A H 1.1424 0.6698 0.2414 0.099 Uiso 0.70 1 calc PR B 1 C43 C 1.1833(6) 0.6641(4) 0.1593(4) 0.0970(19) Uani 0.70 1 d PDU B 1 C44 C 1.1658(6) 0.6843(3) 0.0957(4) 0.0828(19) Uani 0.70 1 d PDU B 1 H44A H 1.2030 0.6692 0.0697 0.099 Uiso 0.70 1 calc PR B 1 C45 C 1.0913(5) 0.7280(3) 0.0714(3) 0.0682(17) Uani 0.70 1 d PDU B 1 N12 N 1.2672(6) 0.6186(5) 0.1883(4) 0.1432(16) Uani 0.70 1 d PDU B 1 O11 O 1.2706(6) 0.5935(4) 0.2405(4) 0.1545(19) Uani 0.70 1 d PDU B 1 O12 O 1.3134(6) 0.6022(4) 0.1507(4) 0.1513(18) Uani 0.70 1 d PDU B 1 C41' C 1.0387(10) 0.7094(6) 0.1575(7) 0.054(4) Uiso 0.30 1 d PD B 2 C42' C 1.1005(8) 0.6594(6) 0.1774(6) 0.056(3) Uiso 0.30 1 d PD B 2 H42' H 1.1101 0.6408 0.2185 0.067 Uiso 0.30 1 calc PR B 2 C43' C 1.1477(9) 0.6377(5) 0.1349(5) 0.061(4) Uiso 0.30 1 d PD B 2 C44' C 1.1327(10) 0.6624(6) 0.0734(6) 0.061(4) Uiso 0.30 1 d PD B 2 H44' H 1.1613 0.6441 0.0438 0.073 Uiso 0.30 1 calc PR B 2 C45' C 1.0736(9) 0.7153(5) 0.0565(6) 0.046(3) Uiso 0.30 1 d PD B 2 N12' N 1.2096(7) 0.5787(5) 0.1548(5) 0.075(4) Uiso 0.30 1 d PD B 2 O11' O 1.2206(7) 0.5554(6) 0.2083(5) 0.085(3) Uiso 0.30 1 d PD B 2 O12' O 1.2499(9) 0.5601(6) 0.1144(6) 0.100(4) Uiso 0.30 1 d PD B 2 O2W' O 0.3365(10) 0.7618(6) 0.8105(6) 0.158(4) Uiso 0.50 1 d P C 1 O1W' O 0.405(2) 0.5641(14) 0.0100(14) 0.177(10) Uiso 0.25 1 d P D 1 O3W' O 0.2558(15) 0.6999(10) 0.8653(10) 0.118(6) Uiso 0.25 1 d P E 1 O1W O 0.4687(19) 0.5195(13) 0.0060(14) 0.171(10) Uiso 0.25 1 d P . 2 O2W O 0.2875(11) 0.7195(7) 0.8282(7) 0.175(5) Uiso 0.50 1 d P F 2 O3W O 0.3759(16) 0.7994(12) 0.8065(10) 0.127(7) Uiso 0.25 1 d P G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.04177(9) 0.03736(9) 0.03621(8) 0.00037(7) 0.01147(7) 0.00146(7) N1 0.0510(16) 0.0433(15) 0.0417(13) -0.0001(12) 0.0152(12) 0.0009(14) N2 0.0527(16) 0.0420(15) 0.0486(15) 0.0073(12) 0.0154(13) 0.0020(14) N3 0.0595(17) 0.060(2) 0.0643(17) 0.0040(15) 0.0292(14) -0.0019(16) N4 0.0560(17) 0.0431(16) 0.0437(14) 0.0008(12) 0.0109(13) 0.0084(14) N5 0.0579(17) 0.0404(16) 0.0638(17) 0.0055(14) 0.0238(14) 0.0032(14) N6 0.0500(16) 0.0490(17) 0.0448(15) 0.0007(13) 0.0104(13) -0.0063(14) N7 0.070(2) 0.116(3) 0.0509(18) -0.017(2) 0.0017(17) -0.005(2) N8 0.0679(19) 0.0465(16) 0.0484(15) -0.0085(13) 0.0203(14) -0.0092(15) N9 0.081(2) 0.0524(18) 0.0551(16) -0.0017(14) 0.0343(15) -0.0023(17) N10 0.101(2) 0.0587(19) 0.0459(15) -0.0158(14) 0.0352(15) -0.0207(19) N11 0.066(2) 0.075(2) 0.0576(18) 0.0130(17) 0.0152(16) 0.0076(19) N13 0.137(3) 0.102(3) 0.125(3) 0.018(2) 0.092(2) 0.041(3) N14 0.061(2) 0.091(3) 0.096(3) -0.010(2) 0.006(2) 0.002(2) N15 0.120(4) 0.068(3) 0.100(3) 0.008(2) 0.009(3) -0.011(3) N16 0.120(3) 0.137(4) 0.113(3) -0.034(3) 0.050(3) 0.019(3) C1 0.0544(18) 0.053(2) 0.0552(17) 0.0018(16) 0.0259(15) 0.0073(17) C2 0.0461(17) 0.0524(18) 0.0433(16) 0.0082(15) 0.0154(14) 0.0028(16) C3 0.072(2) 0.0488(19) 0.0507(17) 0.0096(15) 0.0218(16) 0.0023(18) C4 0.099(3) 0.053(2) 0.070(2) 0.0137(19) 0.033(2) 0.007(2) C5 0.130(3) 0.055(2) 0.100(3) 0.011(2) 0.042(3) 0.003(3) C6 0.134(3) 0.073(3) 0.110(3) 0.015(2) 0.054(3) -0.018(3) C7 0.107(3) 0.081(3) 0.096(3) 0.018(2) 0.050(2) -0.014(3) C8 0.079(2) 0.067(2) 0.0609(19) 0.0101(18) 0.0278(18) -0.010(2) C9 0.077(2) 0.093(3) 0.092(3) 0.008(2) 0.050(2) -0.001(2) C10 0.091(2) 0.107(3) 0.124(3) 0.020(2) 0.045(2) 0.010(2) C11 0.101(3) 0.114(3) 0.127(3) 0.017(2) 0.029(2) 0.005(2) C12 0.058(2) 0.0428(18) 0.0537(18) -0.0087(15) 0.0165(15) 0.0011(17) C13 0.0506(17) 0.0413(17) 0.0528(17) 0.0026(15) 0.0194(14) 0.0042(16) C14 0.0482(17) 0.0545(19) 0.0497(17) 0.0071(15) 0.0142(14) 0.0118(16) C15 0.062(2) 0.073(2) 0.0544(19) 0.0032(18) 0.0127(17) 0.021(2) C16 0.076(2) 0.092(3) 0.053(2) 0.007(2) 0.0167(18) 0.027(2) C17 0.078(2) 0.094(3) 0.066(2) 0.028(2) 0.0229(19) 0.031(2) C18 0.067(2) 0.068(2) 0.077(2) 0.0238(19) 0.0257(18) 0.021(2) C19 0.0508(18) 0.0531(19) 0.0596(18) 0.0125(16) 0.0216(15) 0.0093(16) C20 0.091(3) 0.047(2) 0.104(3) 0.002(2) 0.040(2) 0.003(2) C21 0.134(3) 0.099(3) 0.154(3) 0.005(3) 0.052(3) -0.004(3) C22 0.155(3) 0.130(3) 0.167(3) 0.005(3) 0.041(2) -0.007(3) C23 0.066(2) 0.064(2) 0.0407(16) -0.0037(16) 0.0165(15) -0.0014(19) C24 0.058(2) 0.056(2) 0.0413(17) -0.0049(16) 0.0017(16) -0.0002(18) C25 0.0510(19) 0.0508(19) 0.0583(19) 0.0011(16) 0.0067(16) -0.0044(17) C26 0.055(2) 0.058(2) 0.077(2) 0.0043(19) 0.0163(18) -0.0074(18) C27 0.059(2) 0.079(3) 0.102(3) 0.005(2) 0.022(2) -0.006(2) C28 0.063(3) 0.118(3) 0.118(3) -0.010(3) 0.007(3) -0.009(3) C29 0.075(3) 0.126(3) 0.103(3) -0.021(3) -0.001(3) -0.016(3) C30 0.057(2) 0.090(3) 0.075(2) -0.010(2) 0.004(2) -0.004(2) C34 0.0480(16) 0.0426(16) 0.0368(14) 0.0008(13) 0.0122(12) 0.0050(15) C35 0.0504(17) 0.0443(17) 0.0399(15) -0.0048(13) 0.0127(13) 0.0009(15) C36 0.0533(18) 0.0430(17) 0.0471(16) -0.0022(14) 0.0151(14) -0.0015(16) C37 0.0616(19) 0.0504(19) 0.0446(15) 0.0005(14) 0.0225(14) -0.0023(17) C38 0.072(2) 0.0497(18) 0.0445(16) -0.0079(14) 0.0242(15) -0.0024(17) C39 0.0600(19) 0.0419(17) 0.0421(15) -0.0035(13) 0.0171(14) -0.0046(15) C46 0.065(2) 0.0442(17) 0.0531(17) 0.0006(15) 0.0195(15) -0.0119(16) C47 0.071(2) 0.0483(19) 0.064(2) -0.0029(18) 0.0125(19) -0.0046(19) C48 0.081(3) 0.059(2) 0.072(2) 0.001(2) 0.000(2) -0.011(2) C49 0.098(3) 0.056(2) 0.060(2) -0.0023(19) 0.004(2) -0.017(2) C50 0.097(3) 0.059(2) 0.069(2) -0.0136(18) 0.029(2) -0.011(2) C51 0.073(2) 0.060(2) 0.070(2) -0.0063(19) 0.0215(19) -0.007(2) O1 0.0531(13) 0.0491(13) 0.0385(11) 0.0003(10) 0.0123(10) -0.0022(11) O2 0.0712(16) 0.0619(16) 0.0423(12) -0.0087(11) 0.0188(11) -0.0087(14) O3 0.119(2) 0.0596(16) 0.0732(16) -0.0152(14) 0.0400(15) -0.0179(17) O4 0.0819(17) 0.0819(19) 0.0770(16) -0.0007(15) 0.0358(14) -0.0210(16) O5 0.122(2) 0.090(2) 0.0724(15) -0.0150(15) 0.0548(15) -0.0261(18) O6 0.129(2) 0.0694(19) 0.104(2) -0.0256(16) 0.0521(18) -0.0189(19) O7 0.096(2) 0.090(2) 0.0821(18) -0.0168(16) 0.0351(16) -0.0330(18) O8 0.0457(13) 0.0496(14) 0.0591(13) 0.0032(11) 0.0142(11) 0.0066(12) O9 0.0543(15) 0.0661(17) 0.0622(15) 0.0119(13) 0.0175(12) 0.0112(14) O10 0.098(2) 0.127(3) 0.0725(19) 0.0101(19) 0.0135(17) 0.014(2) O13 0.188(3) 0.174(4) 0.157(3) 0.003(3) 0.090(2) 0.025(3) O14 0.165(3) 0.177(3) 0.147(3) 0.029(3) 0.079(2) 0.043(3) O15 0.0677(16) 0.0454(13) 0.0539(13) -0.0046(11) 0.0144(12) -0.0091(13) O16 0.085(2) 0.0553(17) 0.0728(18) -0.0021(14) 0.0174(16) 0.0034(16) O17 0.122(3) 0.143(3) 0.174(3) -0.036(3) 0.028(2) 0.008(3) O18 0.159(3) 0.107(3) 0.105(2) -0.022(2) 0.024(2) -0.003(2) O19 0.143(3) 0.125(3) 0.146(3) -0.018(3) -0.001(3) -0.017(3) O20 0.182(4) 0.229(4) 0.212(4) -0.015(3) 0.085(3) 0.016(3) O21 0.136(3) 0.153(3) 0.154(3) -0.011(3) 0.028(3) 0.022(3) C31 0.152(3) 0.160(3) 0.146(3) -0.010(3) 0.045(3) -0.002(3) C32 0.156(3) 0.158(3) 0.152(3) -0.005(3) 0.043(3) -0.002(3) C33 0.158(3) 0.159(3) 0.155(3) -0.003(3) 0.044(3) -0.002(3) C31' 0.149(4) 0.155(4) 0.141(4) -0.009(4) 0.042(4) -0.002(4) C32' 0.160(3) 0.164(3) 0.157(3) -0.005(3) 0.040(3) -0.005(3) C33' 0.162(3) 0.163(3) 0.156(3) -0.007(2) 0.042(2) -0.003(2) C40 0.0502(18) 0.056(2) 0.0656(19) 0.0051(17) 0.0197(15) 0.0043(17) C41 0.052(3) 0.061(3) 0.066(3) 0.008(2) 0.016(2) 0.014(2) C42 0.077(3) 0.085(3) 0.084(3) 0.015(3) 0.022(3) 0.025(3) C43 0.089(3) 0.099(3) 0.105(3) 0.013(3) 0.033(3) 0.034(3) C44 0.074(3) 0.085(3) 0.095(3) 0.006(3) 0.034(3) 0.019(3) C45 0.063(3) 0.069(3) 0.075(3) 0.004(3) 0.026(2) 0.007(3) N12 0.140(2) 0.151(3) 0.147(2) 0.016(2) 0.056(2) 0.040(2) O11 0.151(3) 0.157(3) 0.155(3) 0.014(3) 0.046(2) 0.035(3) O12 0.144(3) 0.158(3) 0.159(3) 0.016(3) 0.057(2) 0.034(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 Sm1 O15 2.327(3) . ? Sm1 O8 2.337(3) . ? Sm1 O1 2.338(2) . ? Sm1 N6 2.610(3) . ? Sm1 N2 2.617(3) . ? Sm1 N4 2.639(3) . ? Sm1 O9 2.694(3) . ? Sm1 O2 2.694(3) . ? Sm1 O16 2.763(3) . ? Sm1 N1 2.770(3) . ? N1 C12 1.469(5) . ? N1 C1 1.476(5) . ? N1 C23 1.484(4) . ? N2 C2 1.318(5) . ? N2 C3 1.404(5) . ? N3 C2 1.338(5) . ? N3 C8 1.386(6) . ? N3 C9 1.459(6) . ? N4 C13 1.302(5) . ? N4 C14 1.392(4) . ? N5 C13 1.350(5) . ? N5 C19 1.371(5) . ? N5 C20 1.452(6) . ? N6 C24 1.297(5) . ? N6 C25 1.397(5) . ? N7 C24 1.366(5) . ? N7 C30 1.373(7) . ? N7 C31 1.426(17) . ? N7 C31' 1.589(17) . ? N8 O2 1.219(4) . ? N8 O3 1.231(4) . ? N8 C35 1.454(5) . ? N9 O4 1.214(5) . ? N9 O5 1.230(4) . ? N9 C37 1.447(5) . ? N10 O6 1.190(5) . ? N10 O7 1.207(5) . ? N10 C39 1.466(5) . ? N11 O10 1.216(5) . ? N11 O9 1.219(4) . ? N11 C41 1.417(8) . ? N11 C41' 1.617(15) . ? N13 O13 1.158(7) . ? N13 O14 1.192(8) . ? N13 C45' 1.366(13) . ? N13 C45 1.511(8) . ? N14 O16 1.201(5) . ? N14 O17 1.241(7) . ? N14 C47 1.439(7) . ? N15 O18 1.199(7) . ? N15 O19 1.224(8) . ? N15 C49 1.498(6) . ? N16 O21 1.160(8) . ? N16 O20 1.160(9) . ? N16 C51 1.498(7) . ? C1 C2 1.484(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.381(7) . ? C3 C8 1.397(7) . ? C4 C5 1.404(8) . ? C4 H4 0.9300 . ? C5 C6 1.396(9) . ? C5 H5A 0.9300 . ? C6 C7 1.372(9) . ? C6 H6A 0.9300 . ? C7 C8 1.389(7) . ? C7 H7A 0.9300 . ? C9 C10 1.446(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.306(7) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C11 H11B 0.9300 . ? C12 C13 1.508(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.387(6) . ? C14 C19 1.393(6) . ? C15 C16 1.388(6) . ? C15 H15A 0.9300 . ? C16 C17 1.387(7) . ? C16 H16A 0.9300 . ? C17 C18 1.379(7) . ? C17 H17A 0.9300 . ? C18 C19 1.395(6) . ? C18 H18A 0.9300 . ? C20 C21 1.421(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.218(8) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C22 H22B 0.9300 . ? C23 C24 1.454(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C30 1.380(6) . ? C25 C26 1.383(7) . ? C26 C27 1.378(6) . ? C26 H26A 0.9300 . ? C27 C28 1.314(8) . ? C27 H27A 0.9300 . ? C28 C29 1.397(10) . ? C28 H28A 0.9300 . ? C29 C30 1.407(8) . ? C29 H29A 0.9300 . ? C34 O1 1.270(4) . ? C34 C35 1.424(5) . ? C34 C39 1.431(5) . ? C35 C36 1.368(5) . ? C36 C37 1.379(5) . ? C36 H36A 0.9300 . ? C37 C38 1.390(6) . ? C38 C39 1.358(6) . ? C38 H38A 0.9300 . ? C46 O15 1.251(4) . ? C46 C51 1.414(6) . ? C46 C47 1.421(6) . ? C47 C48 1.388(6) . ? C48 C49 1.375(8) . ? C48 H48A 0.9300 . ? C49 C50 1.371(7) . ? C50 C51 1.368(6) . ? C50 H50A 0.9300 . ? O8 C40 1.256(5) . ? C31 C32 1.419(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.323(10) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C33 H33B 0.9300 . ? C31' C32' 1.387(12) . ? C31' H31C 0.9700 . ? C31' H31D 0.9700 . ? C32' C33' 1.299(9) . ? C32' H32B 0.9300 . ? C33' H33C 0.9300 . ? C33' H33D 0.9300 . ? C40 C45 1.399(8) . ? C40 C41 1.447(7) . ? C41 C42 1.367(8) . ? C42 C43 1.356(11) . ? C42 H42A 0.9300 . ? C43 C44 1.367(10) . ? C43 N12 1.508(10) . ? C44 C45 1.380(9) . ? C44 H44A 0.9300 . ? N12 O11 1.220(10) . ? N12 O12 1.227(11) . ? C41' C42' 1.358(14) . ? C42' C43' 1.359(14) . ? C42' H42' 0.9300 . ? C43' C44' 1.365(14) . ? C43' N12' 1.510(13) . ? C44' C45' 1.380(14) . ? C44' H44' 0.9300 . ? N12' O11' 1.206(13) . ? N12' O12' 1.233(14) . ? O1W O1W 1.29(5) 3_665 ? 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 O15 Sm1 O8 75.42(10) . . ? O15 Sm1 O1 74.25(9) . . ? O8 Sm1 O1 78.74(9) . . ? O15 Sm1 N6 138.34(9) . . ? O8 Sm1 N6 73.29(10) . . ? O1 Sm1 N6 124.41(9) . . ? O15 Sm1 N2 73.99(10) . . ? O8 Sm1 N2 122.77(9) . . ? O1 Sm1 N2 134.37(9) . . ? N6 Sm1 N2 101.04(9) . . ? O15 Sm1 N4 124.11(9) . . ? O8 Sm1 N4 141.08(10) . . ? O1 Sm1 N4 76.08(9) . . ? N6 Sm1 N4 97.44(9) . . ? N2 Sm1 N4 95.95(10) . . ? O15 Sm1 O9 77.02(9) . . ? O8 Sm1 O9 64.72(9) . . ? O1 Sm1 O9 138.00(9) . . ? N6 Sm1 O9 65.07(9) . . ? N2 Sm1 O9 61.96(9) . . ? N4 Sm1 O9 145.91(9) . . ? O15 Sm1 O2 134.37(9) . . ? O8 Sm1 O2 78.16(9) . . ? O1 Sm1 O2 64.50(8) . . ? N6 Sm1 O2 63.32(8) . . ? N2 Sm1 O2 150.91(9) . . ? N4 Sm1 O2 64.37(10) . . ? O9 Sm1 O2 122.73(8) . . ? O15 Sm1 O16 62.65(10) . . ? O8 Sm1 O16 134.01(9) . . ? O1 Sm1 O16 72.71(10) . . ? N6 Sm1 O16 152.53(10) . . ? N2 Sm1 O16 63.87(9) . . ? N4 Sm1 O16 63.75(9) . . ? O9 Sm1 O16 118.87(9) . . ? O2 Sm1 O16 118.33(9) . . ? O15 Sm1 N1 135.10(10) . . ? O8 Sm1 N1 132.85(9) . . ? O1 Sm1 N1 135.81(8) . . ? N6 Sm1 N1 60.74(10) . . ? N2 Sm1 N1 61.36(9) . . ? N4 Sm1 N1 60.15(9) . . ? O9 Sm1 N1 85.89(9) . . ? O2 Sm1 N1 89.69(9) . . ? O16 Sm1 N1 91.89(9) . . ? C12 N1 C1 109.1(3) . . ? C12 N1 C23 109.7(3) . . ? C1 N1 C23 110.9(3) . . ? C12 N1 Sm1 110.1(2) . . ? C1 N1 Sm1 109.5(2) . . ? C23 N1 Sm1 107.5(2) . . ? C2 N2 C3 104.6(3) . . ? C2 N2 Sm1 118.7(2) . . ? C3 N2 Sm1 134.4(3) . . ? C2 N3 C8 106.6(4) . . ? C2 N3 C9 128.6(4) . . ? C8 N3 C9 124.8(4) . . ? C13 N4 C14 104.5(3) . . ? C13 N4 Sm1 117.7(2) . . ? C14 N4 Sm1 130.9(2) . . ? C13 N5 C19 105.9(3) . . ? C13 N5 C20 127.8(3) . . ? C19 N5 C20 126.2(3) . . ? C24 N6 C25 107.0(3) . . ? C24 N6 Sm1 117.6(3) . . ? C25 N6 Sm1 133.9(3) . . ? C24 N7 C30 107.0(4) . . ? C24 N7 C31 129.3(9) . . ? C30 N7 C31 121.6(9) . . ? C24 N7 C31' 117.4(7) . . ? C30 N7 C31' 127.9(7) . . ? C31 N7 C31' 38.8(7) . . ? O2 N8 O3 121.9(3) . . ? O2 N8 C35 120.5(3) . . ? O3 N8 C35 117.7(3) . . ? O4 N9 O5 123.2(4) . . ? O4 N9 C37 119.0(3) . . ? O5 N9 C37 117.8(3) . . ? O6 N10 O7 123.3(4) . . ? O6 N10 C39 118.1(4) . . ? O7 N10 C39 118.5(4) . . ? O10 N11 O9 122.7(4) . . ? O10 N11 C41 115.5(4) . . ? O9 N11 C41 121.8(4) . . ? O10 N11 C41' 123.2(6) . . ? O9 N11 C41' 113.5(5) . . ? C41 N11 C41' 13.2(6) . . ? O13 N13 O14 116.3(6) . . ? O13 N13 C45' 117.7(7) . . ? O14 N13 C45' 125.5(7) . . ? O13 N13 C45 122.8(6) . . ? O14 N13 C45 116.1(5) . . ? C45' N13 C45 16.3(6) . . ? O16 N14 O17 120.8(5) . . ? O16 N14 C47 122.5(4) . . ? O17 N14 C47 116.7(5) . . ? O18 N15 O19 129.1(6) . . ? O18 N15 C49 116.8(5) . . ? O19 N15 C49 114.1(6) . . ? O21 N16 O20 123.2(7) . . ? O21 N16 C51 119.6(6) . . ? O20 N16 C51 117.0(6) . . ? N1 C1 C2 110.5(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N2 C2 N3 114.1(4) . . ? N2 C2 C1 122.1(3) . . ? N3 C2 C1 123.8(4) . . ? C4 C3 C8 121.1(4) . . ? C4 C3 N2 130.3(4) . . ? C8 C3 N2 108.6(4) . . ? C3 C4 C5 115.1(5) . . ? C3 C4 H4 122.4 . . ? C5 C4 H4 122.4 . . ? C6 C5 C4 123.1(5) . . ? C6 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? C7 C6 C5 121.5(5) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 115.4(6) . . ? C6 C7 H7A 122.3 . . ? C8 C7 H7A 122.3 . . ? N3 C8 C7 130.3(5) . . ? N3 C8 C3 106.0(4) . . ? C7 C8 C3 123.7(5) . . ? C10 C9 N3 114.8(5) . . ? C10 C9 H9A 108.6 . . ? N3 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? N3 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 126.0(6) . . ? C11 C10 H10A 117.0 . . ? C9 C10 H10A 117.0 . . ? C10 C11 H11A 120.0 . . ? C10 C11 H11B 120.0 . . ? H11A C11 H11B 120.0 . . ? N1 C12 C13 109.0(3) . . ? N1 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N1 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 N5 114.4(3) . . ? N4 C13 C12 121.9(3) . . ? N5 C13 C12 123.6(3) . . ? C15 C14 N4 131.5(4) . . ? C15 C14 C19 119.5(4) . . ? N4 C14 C19 109.0(3) . . ? C14 C15 C16 118.1(4) . . ? C14 C15 H15A 121.0 . . ? C16 C15 H15A 121.0 . . ? C17 C16 C15 121.5(4) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 116.5(4) . . ? C17 C18 H18A 121.8 . . ? C19 C18 H18A 121.8 . . ? N5 C19 C14 106.2(3) . . ? N5 C19 C18 131.0(4) . . ? C14 C19 C18 122.8(4) . . ? C21 C20 N5 118.1(5) . . ? C21 C20 H20A 107.8 . . ? N5 C20 H20A 107.8 . . ? C21 C20 H20B 107.8 . . ? N5 C20 H20B 107.8 . . ? H20A C20 H20B 107.1 . . ? C22 C21 C20 128.1(8) . . ? C22 C21 H21A 115.9 . . ? C20 C21 H21A 115.9 . . ? C21 C22 H22A 120.0 . . ? C21 C22 H22B 120.0 . . ? H22A C22 H22B 120.0 . . ? C24 C23 N1 108.6(3) . . ? C24 C23 H23A 110.0 . . ? N1 C23 H23A 110.0 . . ? C24 C23 H23B 110.0 . . ? N1 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? N6 C24 N7 111.5(4) . . ? N6 C24 C23 123.7(3) . . ? N7 C24 C23 124.8(4) . . ? C30 C25 C26 119.9(4) . . ? C30 C25 N6 107.8(4) . . ? C26 C25 N6 132.1(4) . . ? C27 C26 C25 118.2(5) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C28 C27 C26 122.3(6) . . ? C28 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C27 C28 C29 122.3(6) . . ? C27 C28 H28A 118.8 . . ? C29 C28 H28A 118.8 . . ? C28 C29 C30 116.1(6) . . ? C28 C29 H29A 122.0 . . ? C30 C29 H29A 122.0 . . ? N7 C30 C25 106.6(4) . . ? N7 C30 C29 132.1(5) . . ? C25 C30 C29 121.2(5) . . ? O1 C34 C35 126.1(3) . . ? O1 C34 C39 121.8(3) . . ? C35 C34 C39 112.1(3) . . ? C36 C35 C34 124.7(3) . . ? C36 C35 N8 116.4(3) . . ? C34 C35 N8 118.9(3) . . ? C35 C36 C37 118.6(3) . . ? C35 C36 H36A 120.7 . . ? C37 C36 H36A 120.7 . . ? C36 C37 C38 121.1(4) . . ? C36 C37 N9 118.9(3) . . ? C38 C37 N9 120.0(3) . . ? C39 C38 C37 118.5(3) . . ? C39 C38 H38A 120.8 . . ? C37 C38 H38A 120.8 . . ? C38 C39 C34 124.8(3) . . ? C38 C39 N10 117.9(3) . . ? C34 C39 N10 117.3(3) . . ? O15 C46 C51 122.5(4) . . ? O15 C46 C47 125.9(4) . . ? C51 C46 C47 111.6(4) . . ? C48 C47 C46 124.1(5) . . ? C48 C47 N14 116.6(4) . . ? C46 C47 N14 119.2(4) . . ? C49 C48 C47 118.5(5) . . ? C49 C48 H48A 120.7 . . ? C47 C48 H48A 120.7 . . ? C50 C49 C48 121.8(4) . . ? C50 C49 N15 118.2(5) . . ? C48 C49 N15 119.9(5) . . ? C51 C50 C49 117.4(5) . . ? C51 C50 H50A 121.3 . . ? C49 C50 H50A 121.3 . . ? C50 C51 C46 126.5(4) . . ? C50 C51 N16 117.7(5) . . ? C46 C51 N16 115.8(4) . . ? C34 O1 Sm1 142.3(2) . . ? N8 O2 Sm1 137.4(2) . . ? C40 O8 Sm1 144.0(3) . . ? N11 O9 Sm1 133.7(3) . . ? C46 O15 Sm1 144.2(3) . . ? N14 O16 Sm1 137.2(3) . . ? C32 C31 N7 113.1(14) . . ? C32 C31 H31A 109.0 . . ? N7 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? N7 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 122.8(17) . . ? C33 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? C32 C33 H33A 120.0 . . ? C32 C33 H33B 120.0 . . ? H33A C33 H33B 120.0 . . ? C32' C31' N7 104.3(8) . . ? C32' C31' H31C 110.9 . . ? N7 C31' H31C 110.9 . . ? C32' C31' H31D 110.9 . . ? N7 C31' H31D 110.9 . . ? H31C C31' H31D 108.9 . . ? C33' C32' C31' 128.7(13) . . ? C33' C32' H32B 115.7 . . ? C31' C32' H32B 115.7 . . ? C32' C33' H33C 120.0 . . ? C32' C33' H33D 120.0 . . ? H33C C33' H33D 120.0 . . ? O8 C40 C45 123.8(4) . . ? O8 C40 C41 123.8(4) . . ? C45 C40 C41 111.1(4) . . ? C42 C41 N11 115.1(6) . . ? C42 C41 C40 125.3(6) . . ? N11 C41 C40 119.6(4) . . ? C43 C42 C41 117.3(7) . . ? C43 C42 H42A 121.3 . . ? C41 C42 H42A 121.3 . . ? C42 C43 C44 122.8(7) . . ? C42 C43 N12 118.1(7) . . ? C44 C43 N12 119.1(7) . . ? C43 C44 C45 117.9(7) . . ? C43 C44 H44A 121.0 . . ? C45 C44 H44A 121.0 . . ? C44 C45 C40 124.8(6) . . ? C44 C45 N13 115.8(6) . . ? C40 C45 N13 118.3(5) . . ? O11 N12 O12 126.1(9) . . ? O11 N12 C43 117.3(8) . . ? O12 N12 C43 115.2(8) . . ? C42' C41' N11 116.4(10) . . ? C41' C42' C43' 117.2(11) . . ? C41' C42' H42' 121.4 . . ? C43' C42' H42' 121.4 . . ? C42' C43' C44' 122.9(10) . . ? C42' C43' N12' 117.1(10) . . ? C44' C43' N12' 119.6(10) . . ? C43' C44' C45' 117.8(12) . . ? C43' C44' H44' 121.1 . . ? C45' C44' H44' 121.1 . . ? N13 C45' C44' 117.9(11) . . ? O11' N12' O12' 124.9(12) . . ? O11' N12' C43' 120.0(11) . . ? O12' N12' C43' 115.0(10) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.308 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.124 #=====================================# data_29 _database_code_depnum_ccdc_archive 'CCDC 698719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H88 N20 O19 Sm2' _chemical_formula_weight 2102.54 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' Sm Sm -0.1638 3.4418 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8614(10) _cell_length_b 22.5574(10) _cell_length_c 24.3685(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.169(10) _cell_angle_gamma 90.00 _cell_volume 9244.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 12 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6895 _exptl_absorpt_correction_T_max 0.7571 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 800 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19665 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.97 _reflns_number_total 18047 _reflns_number_gt 11554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+180.4462P] 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 geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18047 _refine_ls_number_parameters 1210 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.1543 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.2458 _refine_ls_wR_factor_gt 0.2099 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.002 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 Sm1 Sm 0.86446(2) 0.984061(19) 0.73528(2) 0.04098(11) Uani 1 1 d . . . Sm2 Sm 0.13024(2) 0.497179(19) 0.734490(18) 0.03681(10) Uani 1 1 d . . . C1 C 1.0506(5) 1.0424(4) 0.7111(4) 0.047(2) Uani 1 1 d . . . H1A H 1.1069 1.0401 0.7057 0.056 Uiso 1 1 calc R . . H1B H 1.0408 1.0791 0.7302 0.056 Uiso 1 1 calc R . . C2 C 1.0034(5) 1.0415(4) 0.6564(4) 0.042(2) Uani 1 1 d . . . C3 C 0.9106(5) 1.0236(4) 0.5935(4) 0.051(3) Uani 1 1 d . . . C4 C 0.8427(6) 1.0047(5) 0.5620(4) 0.066(3) Uani 1 1 d . . . H4A H 0.8040 0.9824 0.5778 0.079 Uiso 1 1 calc R . . C5 C 0.8342(6) 1.0199(6) 0.5062(5) 0.080(4) Uani 1 1 d . . . H5A H 0.7882 1.0101 0.4848 0.096 Uiso 1 1 calc R . . C6 C 0.8944(7) 1.0494(5) 0.4838(5) 0.078(4) Uani 1 1 d . . . H6A H 0.8894 1.0576 0.4464 0.093 Uiso 1 1 calc R . . C7 C 0.9624(7) 1.0675(4) 0.5138(4) 0.063(3) Uani 1 1 d . . . H7A H 1.0023 1.0880 0.4973 0.075 Uiso 1 1 calc R . . C8 C 0.9691(5) 1.0542(4) 0.5691(4) 0.045(2) Uani 1 1 d . . . C9 C 1.1033(6) 1.0964(4) 0.6026(4) 0.057(3) Uani 1 1 d . . . H9A H 1.1183 1.0916 0.5651 0.068 Uiso 1 1 calc R . . H9B H 1.1451 1.0790 0.6269 0.068 Uiso 1 1 calc R . . C10 C 1.0981(5) 1.1613(4) 0.6150(4) 0.046(2) Uani 1 1 d D . . C11 C 1.0641(6) 1.2004(5) 0.5769(5) 0.083(4) Uani 1 1 d D . . H11A H 1.0430 1.1871 0.5428 0.100 Uiso 1 1 calc R . . C12 C 1.0619(7) 1.2598(6) 0.5902(6) 0.101(5) Uani 1 1 d D . . H12A H 1.0373 1.2863 0.5651 0.121 Uiso 1 1 calc R . . C13 C 1.0933(8) 1.2798(6) 0.6367(6) 0.100(5) Uani 1 1 d D . . H13A H 1.0924 1.3204 0.6432 0.120 Uiso 1 1 calc R . . C14 C 1.1279(7) 1.2432(6) 0.6769(6) 0.090(4) Uani 1 1 d D . . H14A H 1.1493 1.2578 0.7105 0.108 Uiso 1 1 calc R . . C15 C 1.1290(6) 1.1836(5) 0.6643(5) 0.061(3) Uani 1 1 d D . . H15A H 1.1517 1.1575 0.6904 0.074 Uiso 1 1 calc R . . C16 C 1.0613(5) 0.9382(3) 0.7224(4) 0.044(2) Uani 1 1 d . . . H16A H 1.1173 0.9359 0.7347 0.053 Uiso 1 1 calc R . . H16B H 1.0569 0.9390 0.6825 0.053 Uiso 1 1 calc R . . C17 C 1.0187(5) 0.8854(3) 0.7423(4) 0.040(2) Uani 1 1 d . . . C18 C 0.9243(5) 0.8299(4) 0.7697(4) 0.047(2) Uani 1 1 d . . . C19 C 0.8567(6) 0.8061(4) 0.7879(4) 0.055(3) Uani 1 1 d . . . H19A H 0.8136 0.8302 0.7945 0.065 Uiso 1 1 calc R . . C20 C 0.8535(6) 0.7462(4) 0.7964(5) 0.062(3) Uani 1 1 d . . . H20A H 0.8064 0.7294 0.8067 0.074 Uiso 1 1 calc R . . C21 C 0.9191(6) 0.7093(4) 0.7900(5) 0.064(3) Uani 1 1 d . . . H21A H 0.9165 0.6691 0.7982 0.077 Uiso 1 1 calc R . . C22 C 0.9871(6) 0.7329(4) 0.7717(4) 0.059(3) Uani 1 1 d . . . H22A H 1.0305 0.7089 0.7656 0.071 Uiso 1 1 calc R . . C23 C 0.9897(6) 0.7936(4) 0.7623(4) 0.051(3) Uani 1 1 d . . . C24 C 1.1271(5) 0.8099(4) 0.7288(4) 0.058(3) Uani 1 1 d . . . H24A H 1.1483 0.7801 0.7545 0.069 Uiso 1 1 calc R . . H24B H 1.1635 0.8433 0.7304 0.069 Uiso 1 1 calc R . . C25 C 1.1218(5) 0.7849(4) 0.6725(4) 0.059(3) Uani 1 1 d DU . . C26 C 1.1206(5) 0.7260(5) 0.6640(5) 0.070(3) Uani 1 1 d DU . . H26A H 1.1232 0.7001 0.6937 0.084 Uiso 1 1 calc R . . C27 C 1.1152(7) 0.7036(6) 0.6096(6) 0.094(4) Uani 1 1 d DU . . H27A H 1.1196 0.6629 0.6044 0.113 Uiso 1 1 calc R . . C28 C 1.1044(9) 0.7377(7) 0.5665(7) 0.109(4) Uani 1 1 d DU . . H28A H 1.0913 0.7220 0.5317 0.131 Uiso 1 1 calc R . . C29 C 1.1133(10) 0.7986(7) 0.5747(7) 0.123(4) Uani 1 1 d DU . . H29A H 1.1143 0.8238 0.5445 0.148 Uiso 1 1 calc R . . C30 C 1.1207(8) 0.8216(5) 0.6264(5) 0.098(4) Uani 1 1 d DU . . H30A H 1.1250 0.8624 0.6311 0.117 Uiso 1 1 calc R . . C31 C 1.0522(5) 1.0010(4) 0.8027(4) 0.048(2) Uani 1 1 d . . . H31A H 1.0465 0.9642 0.8226 0.058 Uiso 1 1 calc R . . H31B H 1.1078 1.0124 0.8063 0.058 Uiso 1 1 calc R . . C32 C 1.0040(5) 1.0474(4) 0.8264(4) 0.040(2) Uani 1 1 d . . . C33 C 0.9048(5) 1.1059(4) 0.8367(4) 0.047(2) Uani 1 1 d . . . C34 C 0.8352(5) 1.1393(4) 0.8305(4) 0.056(3) Uani 1 1 d . . . H34A H 0.7962 1.1322 0.8023 0.067 Uiso 1 1 calc R . . C35 C 0.8276(6) 1.1844(4) 0.8694(5) 0.064(3) Uani 1 1 d . . . H35A H 0.7813 1.2070 0.8679 0.077 Uiso 1 1 calc R . . C36 C 0.8861(6) 1.1959(5) 0.9094(4) 0.063(3) Uani 1 1 d . . . H36A H 0.8778 1.2263 0.9341 0.076 Uiso 1 1 calc R . . C37 C 0.9562(6) 1.1655(5) 0.9156(4) 0.059(3) Uani 1 1 d . . . H37A H 0.9956 1.1744 0.9430 0.071 Uiso 1 1 calc R . . C38 C 0.9643(6) 1.1202(4) 0.8776(4) 0.049(3) Uani 1 1 d . . . C39 C 1.1068(3) 1.0828(3) 0.8997(3) 0.052(3) Uani 1 1 d . . . H39A H 1.1149 1.1216 0.9163 0.063 Uiso 1 1 calc R . . H39B H 1.1474 1.0769 0.8740 0.063 Uiso 1 1 calc R . . C40 C 1.1165(3) 1.0360(3) 0.9444(3) 0.057(3) Uani 1 1 d RDU . . C41 C 1.0954(3) 1.0473(3) 0.9975(3) 0.083(3) Uani 1 1 d RDU . . H41A H 1.0684 1.0821 1.0045 0.100 Uiso 1 1 calc R . . C42 C 1.1134(6) 1.0084(5) 1.0395(5) 0.089(3) Uani 1 1 d DU . . H42A H 1.1036 1.0162 1.0758 0.107 Uiso 1 1 calc R . . C43 C 1.1478(8) 0.9558(6) 1.0227(6) 0.096(4) Uani 1 1 d DU . . H43A H 1.1544 0.9264 1.0494 0.115 Uiso 1 1 calc R . . C44 C 1.1716(8) 0.9426(7) 0.9754(6) 0.095(4) Uani 1 1 d DU . . H44A H 1.1980 0.9074 0.9688 0.114 Uiso 1 1 calc R . . C45 C 1.1539(7) 0.9873(6) 0.9327(5) 0.079(3) Uani 1 1 d DU . . H45A H 1.1692 0.9810 0.8972 0.095 Uiso 1 1 calc R . . C46 C -0.0534(5) 0.5020(4) 0.7907(4) 0.043(2) Uani 1 1 d . . . H46A H -0.1080 0.5157 0.7905 0.052 Uiso 1 1 calc R . . H46B H -0.0502 0.4636 0.8086 0.052 Uiso 1 1 calc R . . C47 C -0.0006(5) 0.5441(4) 0.8216(4) 0.047(2) Uani 1 1 d . . . C48 C 0.0969(5) 0.6042(4) 0.8441(4) 0.051(3) Uani 1 1 d . . . C49 C 0.1606(6) 0.6399(5) 0.8475(5) 0.067(3) Uani 1 1 d . . . H49A H 0.1894 0.6458 0.8168 0.080 Uiso 1 1 calc R . . C50 C 0.1834(7) 0.6674(6) 0.8956(6) 0.095(4) Uani 1 1 d . . . H50A H 0.2279 0.6918 0.8980 0.114 Uiso 1 1 calc R . . C51 C 0.1395(8) 0.6587(7) 0.9416(6) 0.102(5) Uani 1 1 d . . . H51A H 0.1562 0.6775 0.9745 0.123 Uiso 1 1 calc R . . C52 C 0.0737(7) 0.6240(6) 0.9402(5) 0.086(4) Uani 1 1 d . . . H52A H 0.0451 0.6184 0.9710 0.103 Uiso 1 1 calc R . . C53 C 0.0514(5) 0.5974(4) 0.8899(4) 0.055(3) Uani 1 1 d . . . C54 C -0.0642(6) 0.5297(4) 0.9109(4) 0.056(3) Uani 1 1 d . . . H54A H -0.1188 0.5343 0.8961 0.067 Uiso 1 1 calc R . . H54B H -0.0590 0.5483 0.9469 0.067 Uiso 1 1 calc R . . C55 C -0.0448(6) 0.4657(5) 0.9164(4) 0.060(3) Uani 1 1 d D . . C56 C 0.0341(7) 0.4485(5) 0.9275(4) 0.084(4) Uani 1 1 d D . . H56A H 0.0740 0.4768 0.9333 0.101 Uiso 1 1 calc R . . C57 C 0.0520(8) 0.3888(6) 0.9298(4) 0.089(4) Uani 1 1 d D . . H57A H 0.1049 0.3777 0.9369 0.107 Uiso 1 1 calc R . . C58 C -0.0031(9) 0.3458(6) 0.9223(5) 0.096(5) Uani 1 1 d D . . H58A H 0.0108 0.3059 0.9242 0.115 Uiso 1 1 calc R . . C59 C -0.0799(9) 0.3634(6) 0.9117(5) 0.089(4) Uani 1 1 d D . . H59A H -0.1190 0.3346 0.9057 0.107 Uiso 1 1 calc R . . C60 C -0.1019(8) 0.4221(5) 0.9098(5) 0.078(4) Uani 1 1 d D . . H60A H -0.1553 0.4324 0.9040 0.094 Uiso 1 1 calc R . . C61 C -0.0617(5) 0.4394(3) 0.7099(4) 0.042(2) Uani 1 1 d . . . H61A H -0.0568 0.4385 0.6705 0.050 Uiso 1 1 calc R . . H61B H -0.1174 0.4349 0.7166 0.050 Uiso 1 1 calc R . . C62 C -0.0144(5) 0.3908(3) 0.7370(3) 0.037(2) Uani 1 1 d . . . C63 C 0.0858(5) 0.3458(4) 0.7813(4) 0.040(2) Uani 1 1 d . . . C64 C 0.1565(5) 0.3281(4) 0.8074(4) 0.049(2) Uani 1 1 d . . . H64A H 0.2003 0.3532 0.8103 0.058 Uiso 1 1 calc R . . C65 C 0.1605(6) 0.2709(5) 0.8295(5) 0.069(3) Uani 1 1 d . . . H65A H 0.2078 0.2580 0.8476 0.083 Uiso 1 1 calc R . . C66 C 0.0957(6) 0.2330(5) 0.8252(5) 0.073(4) Uani 1 1 d . . . H66A H 0.1008 0.1949 0.8396 0.087 Uiso 1 1 calc R . . C67 C 0.0241(6) 0.2505(4) 0.7999(4) 0.055(3) Uani 1 1 d . . . H67A H -0.0199 0.2255 0.7981 0.066 Uiso 1 1 calc R . . C68 C 0.0197(5) 0.3068(4) 0.7773(4) 0.046(2) Uani 1 1 d . . . C69 C -0.1218(5) 0.3129(4) 0.7371(4) 0.044(2) Uani 1 1 d . . . H69A H -0.1600 0.3449 0.7383 0.053 Uiso 1 1 calc R . . H69B H -0.1332 0.2846 0.7654 0.053 Uiso 1 1 calc R . . C70 C -0.1332(5) 0.2831(4) 0.6823(4) 0.053(3) Uani 1 1 d D . . C71 C -0.1192(5) 0.2222(5) 0.6780(5) 0.066(3) Uani 1 1 d D . . H71A H -0.1033 0.1998 0.7089 0.079 Uiso 1 1 calc R . . C72 C -0.1296(6) 0.1967(5) 0.6276(6) 0.090(4) Uani 1 1 d D . . H72A H -0.1218 0.1560 0.6253 0.108 Uiso 1 1 calc R . . C73 C -0.1505(8) 0.2261(7) 0.5808(6) 0.101(5) Uani 1 1 d D . . H73A H -0.1552 0.2072 0.5468 0.121 Uiso 1 1 calc R . . C74 C -0.1648(8) 0.2870(6) 0.5860(5) 0.087(4) Uani 1 1 d D . . H74A H -0.1815 0.3090 0.5550 0.104 Uiso 1 1 calc R . . C75 C -0.1543(7) 0.3153(5) 0.6371(5) 0.076(4) Uani 1 1 d D . . H75A H -0.1619 0.3560 0.6398 0.091 Uiso 1 1 calc R . . C76 C -0.0635(5) 0.5464(3) 0.6985(3) 0.039(2) Uani 1 1 d . . . H76A H -0.1203 0.5414 0.6904 0.047 Uiso 1 1 calc R . . H76B H -0.0546 0.5836 0.7180 0.047 Uiso 1 1 calc R . . C77 C -0.0223(5) 0.5472(3) 0.6462(4) 0.040(2) Uani 1 1 d . . . C78 C 0.0724(5) 0.5413(4) 0.5910(4) 0.047(2) Uani 1 1 d . . . C79 C 0.1414(6) 0.5323(4) 0.5668(4) 0.054(3) Uani 1 1 d . . . H79A H 0.1857 0.5156 0.5859 0.065 Uiso 1 1 calc R . . C80 C 0.1426(7) 0.5498(5) 0.5103(5) 0.072(3) Uani 1 1 d . . . H80A H 0.1894 0.5460 0.4926 0.086 Uiso 1 1 calc R . . C81 C 0.0750(7) 0.5723(4) 0.4815(4) 0.066(3) Uani 1 1 d . . . H81A H 0.0773 0.5823 0.4446 0.079 Uiso 1 1 calc R . . C82 C 0.0055(7) 0.5802(4) 0.5057(4) 0.063(3) Uani 1 1 d . . . H82A H -0.0396 0.5952 0.4863 0.076 Uiso 1 1 calc R . . C83 C 0.0052(5) 0.5647(4) 0.5618(4) 0.044(2) Uani 1 1 d . . . C84 C -0.1340(6) 0.5916(4) 0.5848(4) 0.053(3) Uani 1 1 d . . . H84A H -0.1678 0.5796 0.6134 0.064 Uiso 1 1 calc R . . H84B H -0.1553 0.5740 0.5505 0.064 Uiso 1 1 calc R . . C85 C -0.1373(5) 0.6574(5) 0.5793(4) 0.054(3) Uani 1 1 d D . . C86 C -0.1722(5) 0.6844(5) 0.5330(4) 0.069(3) Uani 1 1 d D . . H86A H -0.1920 0.6614 0.5034 0.082 Uiso 1 1 calc R . . C87 C -0.1777(6) 0.7451(6) 0.5305(5) 0.089(4) Uani 1 1 d D . . H87A H -0.2014 0.7629 0.4990 0.106 Uiso 1 1 calc R . . C88 C -0.1489(8) 0.7797(6) 0.5733(6) 0.094(5) Uani 1 1 d D . . H88A H -0.1533 0.8207 0.5709 0.112 Uiso 1 1 calc R . . C89 C -0.1147(9) 0.7549(7) 0.6186(7) 0.112(5) Uani 1 1 d DU . . H89A H -0.0950 0.7780 0.6480 0.134 Uiso 1 1 calc R . . C90 C -0.1090(7) 0.6940(5) 0.6206(5) 0.077(4) Uani 1 1 d D . . H90A H -0.0844 0.6768 0.6521 0.093 Uiso 1 1 calc R . . N1 N 1.0269(4) 0.9919(3) 0.7438(3) 0.0394(18) Uani 1 1 d . . . N2 N 0.9338(4) 1.0167(3) 0.6494(3) 0.0453(19) Uani 1 1 d . . . N3 N 1.0284(4) 1.0635(3) 0.6088(3) 0.0425(19) Uani 1 1 d . . . N4 N 0.9443(4) 0.8877(3) 0.7569(3) 0.0424(19) Uani 1 1 d . . . N5 N 1.0488(4) 0.8299(3) 0.7454(3) 0.043(2) Uani 1 1 d . . . N6 N 0.9312(4) 1.0589(3) 0.8058(3) 0.045(2) Uani 1 1 d . . . N7 N 1.0266(4) 1.0812(3) 0.8689(3) 0.047(2) Uani 1 1 d . . . N8 N 0.7581(4) 1.0725(3) 0.6839(3) 0.053(2) Uani 1 1 d . . . N9 N 0.7768(5) 0.8842(3) 0.6821(4) 0.056(2) Uani 1 1 d . . . N10 N 0.7732(5) 0.9746(4) 0.8327(4) 0.059(2) Uani 1 1 d . . . N11 N -0.0309(4) 0.4959(3) 0.7332(3) 0.0355(16) Uani 1 1 d . . . N12 N 0.0609(4) 0.5683(3) 0.8019(3) 0.0414(19) Uani 1 1 d . . . N13 N -0.0108(4) 0.5590(3) 0.8744(3) 0.049(2) Uani 1 1 d . . . N14 N 0.0607(4) 0.3984(3) 0.7557(3) 0.0426(19) Uani 1 1 d . . . N15 N -0.0424(4) 0.3370(3) 0.7500(3) 0.0419(19) Uani 1 1 d . . . N16 N 0.0526(4) 0.5314(3) 0.6447(3) 0.045(2) Uani 1 1 d . . . N17 N -0.0541(4) 0.5686(3) 0.5981(3) 0.047(2) Uani 1 1 d . . . N18 N 0.2225(5) 0.4075(3) 0.6819(4) 0.056(2) Uani 1 1 d . . . N19 N 0.2324(5) 0.4887(4) 0.8371(3) 0.059(2) Uani 1 1 d . . . N20 N 0.2342(5) 0.5916(4) 0.7000(3) 0.057(2) Uani 1 1 d . . . O1 O 0.7486(4) 1.0187(3) 0.6739(3) 0.059(2) Uani 1 1 d . . . O2 O 0.8201(4) 1.0879(3) 0.7119(3) 0.0577(19) Uani 1 1 d . . . O3 O 0.7088(5) 1.1095(3) 0.6660(4) 0.093(3) Uani 1 1 d . . . O4 O 0.8336(4) 0.9079(3) 0.6597(3) 0.0566(19) Uani 1 1 d . . . O5 O 0.7598(4) 0.9080(3) 0.7262(3) 0.0549(19) Uani 1 1 d . . . O6 O 0.7408(5) 0.8426(3) 0.6613(4) 0.080(3) Uani 1 1 d . . . O7 O 0.7559(3) 1.0106(3) 0.7945(3) 0.059(2) Uani 1 1 d . . . O8 O 0.8390(4) 0.9469(3) 0.8315(3) 0.0573(19) Uani 1 1 d . . . O9 O 0.7295(4) 0.9669(4) 0.8708(3) 0.073(2) Uani 1 1 d . . . O10 O 0.1612(4) 0.4292(3) 0.6574(3) 0.0528(18) Uani 1 1 d . . . O11 O 0.2379(4) 0.4222(3) 0.7309(3) 0.059(2) Uani 1 1 d . . . O12 O 0.2662(5) 0.3749(4) 0.6574(4) 0.102(3) Uani 1 1 d . . . O13 O 0.2480(4) 0.5249(3) 0.8006(3) 0.0557(19) Uani 1 1 d . . . O14 O 0.1661(4) 0.4652(3) 0.8330(3) 0.070(2) Uani 1 1 d . . . O15 O 0.2817(5) 0.4783(4) 0.8750(4) 0.101(3) Uani 1 1 d . . . O16 O 0.2430(4) 0.5392(3) 0.6844(3) 0.0546(19) Uani 1 1 d . . . O17 O 0.1695(4) 0.6028(3) 0.7221(3) 0.0558(19) Uani 1 1 d . . . O18 O 0.2842(5) 0.6287(4) 0.6975(4) 0.101(3) Uani 1 1 d . . . O19 O 0.0589(9) 0.2028(7) 0.0334(5) 0.171(6) Uani 1 1 d . . . C91 C 0.0184(7) 0.2082(7) 0.0743(11) 0.242(9) Uani 1 1 d DU . . H91A H -0.0080 0.2463 0.0707 0.290 Uiso 1 1 calc R . . H91B H 0.0559 0.2109 0.1063 0.290 Uiso 1 1 calc R . . C92 C -0.0444(11) 0.1634(9) 0.0882(11) 0.261(10) Uani 1 1 d DU . . H92A H -0.0687 0.1761 0.1206 0.391 Uiso 1 1 calc R . . H92B H -0.0200 0.1254 0.0948 0.391 Uiso 1 1 calc R . . H92C H -0.0841 0.1605 0.0581 0.391 Uiso 1 1 calc R . . C93 C 0.1210(15) 0.2494(12) 0.0346(10) 0.203(8) Uani 1 1 d U . . H93A H 0.1560 0.2459 0.0678 0.244 Uiso 1 1 calc R . . H93B H 0.0968 0.2884 0.0338 0.244 Uiso 1 1 calc R . . C94 C 0.1672(14) 0.2404(11) -0.0158(10) 0.206(8) Uani 1 1 d U . . H94A H 0.2119 0.2669 -0.0142 0.310 Uiso 1 1 calc R . . H94B H 0.1334 0.2485 -0.0483 0.310 Uiso 1 1 calc R . . H94C H 0.1857 0.2002 -0.0168 0.310 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 Sm1 0.02806(19) 0.0392(2) 0.0560(3) 0.0024(2) 0.00518(18) -0.00007(17) Sm2 0.02858(18) 0.0376(2) 0.0441(2) 0.00024(19) 0.00186(16) 0.00068(17) C1 0.037(4) 0.048(5) 0.057(6) 0.006(4) 0.011(4) -0.009(4) C2 0.033(4) 0.043(5) 0.050(5) -0.001(4) -0.002(4) 0.002(4) C3 0.039(4) 0.060(5) 0.053(5) 0.017(4) 0.003(4) 0.005(4) C4 0.046(5) 0.076(7) 0.074(7) 0.018(6) -0.008(5) 0.018(5) C5 0.056(6) 0.107(9) 0.072(7) 0.022(6) -0.040(5) -0.007(6) C6 0.088(8) 0.076(8) 0.070(8) 0.004(6) 0.009(7) 0.007(7) C7 0.070(7) 0.053(6) 0.066(7) -0.001(5) 0.010(6) -0.007(5) C8 0.055(5) 0.031(4) 0.048(5) 0.005(4) -0.002(4) 0.006(4) C9 0.059(6) 0.048(5) 0.065(6) 0.002(5) 0.014(5) -0.003(5) C10 0.039(4) 0.049(5) 0.051(5) -0.003(4) 0.009(4) -0.008(4) C11 0.109(10) 0.057(7) 0.083(9) 0.013(6) -0.004(8) -0.013(7) C12 0.112(10) 0.060(7) 0.134(12) 0.024(8) 0.033(9) -0.008(7) C13 0.110(10) 0.073(8) 0.120(11) -0.043(8) 0.039(9) -0.006(7) C14 0.075(8) 0.098(9) 0.097(10) -0.027(8) 0.013(7) -0.025(7) C15 0.055(6) 0.059(6) 0.072(7) -0.001(5) 0.015(5) -0.013(5) C16 0.031(4) 0.032(4) 0.069(6) -0.002(4) 0.000(4) 0.005(3) C17 0.029(4) 0.034(4) 0.056(5) 0.001(4) 0.001(4) 0.003(3) C18 0.032(4) 0.039(4) 0.070(6) 0.007(4) 0.000(4) 0.006(4) C19 0.050(5) 0.045(5) 0.071(6) -0.009(5) 0.020(5) -0.001(4) C20 0.055(6) 0.051(6) 0.080(7) 0.006(5) 0.005(5) -0.018(5) C21 0.076(7) 0.042(5) 0.073(7) 0.015(5) 0.002(6) -0.010(5) C22 0.053(5) 0.047(5) 0.080(7) 0.011(5) 0.014(5) 0.008(4) C23 0.057(5) 0.034(5) 0.064(6) -0.002(4) 0.012(5) 0.002(4) C24 0.039(5) 0.050(5) 0.086(7) -0.002(5) 0.009(5) 0.011(4) C25 0.064(5) 0.042(4) 0.072(5) 0.004(4) 0.016(5) 0.014(4) C26 0.083(6) 0.051(5) 0.079(6) 0.001(5) 0.021(5) 0.001(5) C27 0.112(7) 0.069(6) 0.105(7) -0.013(6) 0.023(6) -0.004(6) C28 0.136(7) 0.092(7) 0.099(7) -0.018(6) 0.013(6) 0.007(6) C29 0.158(7) 0.102(7) 0.110(7) 0.008(6) 0.014(6) 0.017(6) C30 0.133(7) 0.070(6) 0.093(7) -0.005(5) 0.029(6) 0.016(6) C31 0.040(4) 0.046(5) 0.058(5) -0.015(4) 0.005(4) 0.005(4) C32 0.033(4) 0.042(4) 0.045(5) 0.008(4) -0.002(4) 0.000(3) C33 0.037(4) 0.052(5) 0.054(5) 0.000(4) 0.013(4) -0.006(4) C34 0.043(5) 0.056(6) 0.069(7) -0.010(5) 0.014(5) 0.005(4) C35 0.060(6) 0.050(6) 0.084(8) -0.007(5) 0.022(6) 0.008(5) C36 0.074(7) 0.059(6) 0.058(6) -0.012(5) 0.015(5) 0.004(5) C37 0.064(6) 0.067(6) 0.047(6) -0.007(5) 0.009(5) -0.017(5) C38 0.057(5) 0.035(4) 0.057(6) 0.008(4) 0.010(5) -0.004(4) C39 0.058(6) 0.054(5) 0.044(5) -0.001(4) -0.003(5) -0.001(4) C40 0.048(4) 0.066(5) 0.055(5) 0.008(4) -0.011(4) -0.011(4) C41 0.077(6) 0.106(6) 0.067(6) 0.016(5) 0.007(5) 0.017(5) C42 0.088(6) 0.106(6) 0.075(6) 0.043(5) 0.021(5) 0.016(6) C43 0.090(6) 0.106(7) 0.090(6) 0.033(6) -0.001(6) -0.009(6) C44 0.079(6) 0.110(7) 0.092(7) 0.018(6) -0.023(6) -0.008(6) C45 0.072(6) 0.092(6) 0.071(6) 0.013(5) -0.011(5) -0.012(5) C46 0.035(4) 0.039(4) 0.057(5) -0.003(4) 0.016(4) 0.005(4) C47 0.047(5) 0.039(5) 0.053(5) -0.004(4) 0.000(4) 0.008(4) C48 0.039(5) 0.052(5) 0.062(6) -0.006(5) 0.004(4) 0.003(4) C49 0.044(5) 0.083(7) 0.075(7) -0.042(6) 0.013(5) -0.016(5) C50 0.056(6) 0.115(9) 0.116(10) -0.050(8) 0.026(7) -0.032(6) C51 0.075(8) 0.142(11) 0.089(9) -0.057(8) 0.002(7) -0.027(8) C52 0.077(8) 0.114(10) 0.070(8) -0.035(7) 0.020(6) -0.016(7) C53 0.045(5) 0.060(6) 0.061(6) -0.017(5) 0.013(5) -0.015(4) C54 0.054(5) 0.061(6) 0.054(6) 0.000(5) 0.012(5) -0.009(5) C55 0.060(6) 0.071(7) 0.051(6) 0.012(5) 0.012(5) 0.001(5) C56 0.058(6) 0.089(8) 0.108(9) 0.037(7) 0.027(6) 0.026(6) C57 0.089(8) 0.096(9) 0.087(9) 0.022(7) 0.034(7) 0.024(7) C58 0.139(12) 0.082(9) 0.070(8) -0.004(7) 0.027(8) 0.026(9) C59 0.124(11) 0.065(7) 0.076(8) 0.010(6) -0.003(8) -0.013(7) C60 0.084(8) 0.073(7) 0.072(8) -0.004(6) -0.024(6) -0.015(6) C61 0.041(4) 0.034(4) 0.050(5) -0.001(4) 0.005(4) 0.000(3) C62 0.045(4) 0.030(4) 0.036(4) -0.010(3) 0.012(4) -0.008(3) C63 0.046(5) 0.032(4) 0.044(5) 0.008(4) 0.009(4) 0.004(4) C64 0.042(5) 0.053(5) 0.052(5) 0.011(4) 0.007(4) 0.000(4) C65 0.053(6) 0.066(6) 0.087(8) 0.017(6) 0.003(6) 0.025(5) C66 0.061(6) 0.045(5) 0.114(9) 0.026(6) 0.018(6) 0.014(5) C67 0.054(5) 0.040(5) 0.072(7) 0.013(5) 0.010(5) 0.002(4) C68 0.041(4) 0.039(5) 0.061(6) -0.003(4) 0.012(4) 0.006(4) C69 0.039(4) 0.039(4) 0.055(6) 0.000(4) 0.003(4) -0.004(4) C70 0.041(5) 0.052(5) 0.065(6) 0.004(5) 0.010(5) -0.010(4) C71 0.074(7) 0.055(6) 0.071(7) -0.001(5) 0.025(6) -0.015(5) C72 0.106(9) 0.063(7) 0.105(10) -0.022(7) 0.024(8) -0.029(7) C73 0.122(11) 0.113(11) 0.069(8) -0.020(8) 0.014(8) -0.040(9) C74 0.101(10) 0.094(9) 0.064(8) 0.010(7) 0.005(7) -0.009(8) C75 0.089(8) 0.049(6) 0.088(9) -0.003(6) 0.000(7) -0.015(6) C76 0.033(4) 0.035(4) 0.048(5) 0.004(4) -0.006(4) 0.007(3) C77 0.042(4) 0.032(4) 0.046(5) 0.009(4) 0.005(4) -0.002(3) C78 0.044(5) 0.057(5) 0.039(5) -0.012(4) -0.003(4) -0.012(4) C79 0.066(6) 0.055(6) 0.041(5) -0.001(4) 0.001(5) -0.002(5) C80 0.090(8) 0.068(7) 0.059(7) -0.006(5) 0.022(6) -0.019(6) C81 0.101(8) 0.053(6) 0.045(6) 0.003(5) 0.015(6) -0.005(6) C82 0.076(7) 0.054(6) 0.058(6) -0.007(5) -0.003(5) 0.010(5) C83 0.044(5) 0.033(4) 0.053(5) -0.005(4) 0.000(4) -0.002(4) C84 0.055(5) 0.047(5) 0.056(6) 0.010(4) -0.006(5) -0.006(4) C85 0.045(5) 0.066(6) 0.052(6) 0.008(5) 0.008(4) 0.016(4) C86 0.055(6) 0.074(7) 0.074(8) 0.007(6) -0.011(6) 0.013(5) C87 0.079(8) 0.098(8) 0.089(9) 0.046(7) 0.011(7) 0.034(7) C88 0.103(10) 0.066(8) 0.113(11) -0.006(8) 0.018(9) 0.001(7) C89 0.114(9) 0.089(8) 0.130(10) -0.016(8) -0.003(8) 0.028(7) C90 0.081(8) 0.059(6) 0.090(9) 0.004(6) -0.006(7) 0.023(6) N1 0.031(3) 0.039(4) 0.049(4) 0.005(3) 0.003(3) 0.003(3) N2 0.045(4) 0.037(4) 0.055(4) 0.006(3) 0.009(3) -0.008(3) N3 0.045(4) 0.041(4) 0.043(4) 0.005(3) 0.012(3) -0.004(3) N4 0.036(4) 0.035(4) 0.056(5) 0.007(3) 0.006(3) 0.002(3) N5 0.027(3) 0.041(4) 0.063(5) 0.004(3) 0.008(3) 0.006(3) N6 0.040(4) 0.048(4) 0.048(4) 0.001(3) 0.006(3) 0.004(3) N7 0.046(4) 0.060(5) 0.035(4) 0.000(3) 0.008(3) -0.005(4) N8 0.034(4) 0.056(5) 0.070(5) 0.001(4) 0.005(4) 0.016(3) N9 0.050(4) 0.040(4) 0.077(6) -0.016(4) -0.007(4) -0.001(3) N10 0.045(4) 0.070(5) 0.063(5) 0.000(4) 0.006(4) -0.016(4) N11 0.036(3) 0.035(3) 0.036(3) 0.001(3) 0.003(3) -0.003(3) N12 0.033(3) 0.045(4) 0.048(4) -0.010(3) 0.012(3) -0.005(3) N13 0.038(4) 0.061(5) 0.049(5) -0.006(4) 0.005(3) -0.007(3) N14 0.038(4) 0.036(4) 0.055(4) 0.009(3) 0.014(3) -0.002(3) N15 0.038(4) 0.039(4) 0.050(4) 0.002(3) 0.009(3) -0.002(3) N16 0.032(3) 0.052(4) 0.051(4) 0.002(3) 0.002(3) 0.003(3) N17 0.042(4) 0.042(4) 0.057(5) 0.005(4) -0.005(4) 0.004(3) N18 0.057(5) 0.046(4) 0.066(5) 0.007(4) 0.010(4) 0.009(4) N19 0.061(5) 0.052(5) 0.059(5) -0.009(4) -0.019(4) 0.007(4) N20 0.057(4) 0.055(5) 0.060(5) 0.001(4) 0.019(4) -0.022(4) O1 0.047(3) 0.045(4) 0.084(5) -0.005(3) -0.002(3) 0.008(3) O2 0.049(4) 0.058(4) 0.065(4) 0.007(3) -0.007(3) -0.008(3) O3 0.087(5) 0.065(5) 0.120(7) -0.003(5) -0.032(5) 0.023(4) O4 0.048(4) 0.051(4) 0.072(5) -0.007(3) 0.010(3) -0.007(3) O5 0.045(3) 0.045(3) 0.077(5) -0.007(3) 0.016(3) -0.004(3) O6 0.074(5) 0.065(4) 0.103(6) -0.021(4) 0.014(4) -0.028(4) O7 0.031(3) 0.057(4) 0.091(5) 0.000(4) 0.014(3) 0.005(3) O8 0.052(4) 0.064(4) 0.057(4) -0.017(3) 0.010(3) 0.017(3) O9 0.063(4) 0.093(5) 0.068(5) 0.006(4) 0.029(4) -0.005(4) O10 0.052(4) 0.047(3) 0.059(4) 0.002(3) 0.001(3) 0.000(3) O11 0.044(3) 0.065(4) 0.069(5) 0.007(4) 0.008(3) 0.010(3) O12 0.111(6) 0.094(6) 0.105(7) -0.013(5) 0.044(5) 0.047(5) O13 0.042(3) 0.058(4) 0.066(4) 0.013(3) -0.004(3) -0.009(3) O14 0.060(4) 0.094(5) 0.053(4) 0.009(4) -0.014(3) -0.031(4) O15 0.112(6) 0.104(6) 0.080(5) 0.027(5) -0.044(5) -0.034(5) O16 0.046(3) 0.042(3) 0.077(5) -0.006(3) 0.011(3) -0.004(3) O17 0.053(4) 0.046(4) 0.069(4) 0.004(3) 0.018(3) 0.003(3) O18 0.099(5) 0.076(5) 0.135(7) -0.027(5) 0.060(5) -0.050(4) O19 0.190(13) 0.198(13) 0.126(10) -0.037(10) 0.023(9) -0.039(11) C91 0.248(14) 0.242(14) 0.237(14) -0.004(12) 0.021(12) -0.009(12) C92 0.265(14) 0.266(14) 0.251(15) -0.012(12) 0.020(12) -0.042(12) C93 0.194(13) 0.221(13) 0.193(13) -0.007(11) 0.002(11) -0.006(11) C94 0.202(13) 0.211(13) 0.205(13) 0.001(11) 0.009(11) -0.001(11) _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 Sm1 O5 2.459(6) . ? Sm1 O7 2.485(6) . ? Sm1 O1 2.499(6) . ? Sm1 O2 2.511(7) . ? Sm1 O4 2.544(7) . ? Sm1 O8 2.555(7) . ? Sm1 N2 2.577(7) . ? Sm1 N4 2.590(7) . ? Sm1 N6 2.605(7) . ? Sm1 N1 2.738(6) . ? Sm1 N8 2.906(7) . ? Sm1 N10 2.929(8) . ? Sm2 O11 2.487(6) . ? Sm2 O17 2.496(6) . ? Sm2 O10 2.510(6) . ? Sm2 O16 2.518(6) . ? Sm2 O14 2.537(7) . ? Sm2 O13 2.543(6) . ? Sm2 N16 2.585(7) . ? Sm2 N14 2.588(7) . ? Sm2 N12 2.631(7) . ? Sm2 N11 2.715(6) . ? Sm2 N18 2.907(8) . ? Sm2 N20 2.921(8) . ? C1 N1 1.463(11) . ? C1 C2 1.503(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.299(10) . ? C2 N3 1.356(11) . ? C3 C8 1.374(13) . ? C3 C4 1.397(13) . ? C3 N2 1.399(11) . ? C4 C5 1.399(15) . ? C4 H4A 0.9300 . ? C5 C6 1.360(16) . ? C5 H5A 0.9300 . ? C6 C7 1.376(16) . ? C6 H6A 0.9300 . ? C7 C8 1.379(14) . ? C7 H7A 0.9300 . ? C8 N3 1.355(11) . ? C9 N3 1.482(12) . ? C9 C10 1.499(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.371(14) . ? C10 C11 1.376(14) . ? C11 C12 1.380(17) . ? C11 H11A 0.9300 . ? C12 C13 1.298(19) . ? C12 H12A 0.9300 . ? C13 C14 1.377(19) . ? C13 H13A 0.9300 . ? C14 C15 1.380(16) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 N1 1.456(10) . ? C16 C17 1.490(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N4 1.329(10) . ? C17 N5 1.351(10) . ? C18 C19 1.363(13) . ? C18 N4 1.388(11) . ? C18 C23 1.395(12) . ? C19 C20 1.370(13) . ? C19 H19A 0.9300 . ? C20 C21 1.403(15) . ? C20 H20A 0.9300 . ? C21 C22 1.368(14) . ? C21 H21A 0.9300 . ? C22 C23 1.390(13) . ? C22 H22A 0.9300 . ? C23 N5 1.374(11) . ? C24 N5 1.479(11) . ? C24 C25 1.479(14) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.344(14) . ? C25 C30 1.395(13) . ? C26 C27 1.415(18) . ? C26 H26A 0.9300 . ? C27 C28 1.30(2) . ? C27 H27A 0.9300 . ? C28 C29 1.40(2) . ? C28 H28A 0.9300 . ? C29 C30 1.36(2) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.469(12) . ? C31 N1 1.480(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N6 1.318(10) . ? C32 N7 1.319(11) . ? C33 N6 1.392(11) . ? C33 C34 1.394(12) . ? C33 C38 1.398(13) . ? C34 C35 1.402(14) . ? C34 H34A 0.9300 . ? C35 C36 1.360(15) . ? C35 H35A 0.9300 . ? C36 C37 1.366(15) . ? C36 H36A 0.9300 . ? C37 C38 1.393(13) . ? C37 H37A 0.9300 . ? C38 N7 1.398(12) . ? C39 N7 1.499(9) . ? C39 C40 1.5163 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C45 1.309(14) . ? C40 C41 1.3899 . ? C41 C42 1.365(13) . ? C41 H41A 0.9300 . ? C42 C43 1.394(18) . ? C42 H42A 0.9300 . ? C43 C44 1.284(19) . ? C43 H43A 0.9300 . ? C44 C45 1.463(18) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C47 1.472(12) . ? C46 N11 1.485(10) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 N12 1.296(11) . ? C47 N13 1.352(12) . ? C48 C49 1.340(13) . ? C48 C53 1.409(14) . ? C48 N12 1.409(11) . ? C49 C50 1.357(16) . ? C49 H49A 0.9300 . ? C50 C51 1.401(19) . ? C50 H50A 0.9300 . ? C51 C52 1.358(18) . ? C51 H51A 0.9300 . ? C52 C53 1.392(15) . ? C52 H52A 0.9300 . ? C53 N13 1.391(11) . ? C54 N13 1.467(12) . ? C54 C55 1.485(14) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C60 1.376(15) . ? C55 C56 1.394(14) . ? C56 C57 1.381(17) . ? C56 H56A 0.9300 . ? C57 C58 1.345(19) . ? C57 H57A 0.9300 . ? C58 C59 1.361(19) . ? C58 H58A 0.9300 . ? C59 C60 1.376(17) . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? C61 N11 1.474(10) . ? C61 C62 1.482(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 N14 1.325(10) . ? C62 N15 1.348(10) . ? C63 C64 1.369(12) . ? C63 N14 1.392(10) . ? C63 C68 1.417(12) . ? C64 C65 1.398(14) . ? C64 H64A 0.9300 . ? C65 C66 1.385(15) . ? C65 H65A 0.9300 . ? C66 C67 1.373(14) . ? C66 H66A 0.9300 . ? C67 C68 1.384(12) . ? C67 H67A 0.9300 . ? C68 N15 1.381(11) . ? C69 N15 1.456(10) . ? C69 C70 1.494(13) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C75 1.347(15) . ? C70 C71 1.398(14) . ? C71 C72 1.357(17) . ? C71 H71A 0.9300 . ? C72 C73 1.346(19) . ? C72 H72A 0.9300 . ? C73 C74 1.402(19) . ? C73 H73A 0.9300 . ? C74 C75 1.397(17) . ? C74 H74A 0.9300 . ? C75 H75A 0.9300 . ? C76 C77 1.494(12) . ? C76 N11 1.499(10) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 N16 1.316(10) . ? C77 N17 1.344(11) . ? C78 C79 1.358(13) . ? C78 N16 1.391(11) . ? C78 C83 1.398(12) . ? C79 C80 1.435(14) . ? C79 H79A 0.9300 . ? C80 C81 1.391(16) . ? C80 H80A 0.9300 . ? C81 C82 1.361(16) . ? C81 H81A 0.9300 . ? C82 C83 1.411(14) . ? C82 H82A 0.9300 . ? C83 N17 1.385(12) . ? C84 N17 1.458(11) . ? C84 C85 1.490(13) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C90 1.361(15) . ? C85 C86 1.375(14) . ? C86 C87 1.375(16) . ? C86 H86A 0.9300 . ? C87 C88 1.364(18) . ? C87 H87A 0.9300 . ? C88 C89 1.33(2) . ? C88 H88A 0.9300 . ? C89 C90 1.377(18) . ? C89 H89A 0.9300 . ? C90 H90A 0.9300 . ? N8 O3 1.234(10) . ? N8 O1 1.247(10) . ? N8 O2 1.256(10) . ? N9 O6 1.208(10) . ? N9 O5 1.253(10) . ? N9 O4 1.255(10) . ? N10 O9 1.239(11) . ? N10 O7 1.252(10) . ? N10 O8 1.276(10) . ? N18 O12 1.225(11) . ? N18 O11 1.248(10) . ? N18 O10 1.254(10) . ? N19 O15 1.218(11) . ? N19 O14 1.235(10) . ? N19 O13 1.250(10) . ? N20 O18 1.192(10) . ? N20 O16 1.255(10) . ? N20 O17 1.276(10) . ? O19 C91 1.25(2) . ? O19 C93 1.48(3) . ? C91 C92 1.519(10) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 C94 1.51(3) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? 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 O5 Sm1 O7 70.5(2) . . ? O5 Sm1 O1 68.8(2) . . ? O7 Sm1 O1 72.3(2) . . ? O5 Sm1 O2 115.5(2) . . ? O7 Sm1 O2 71.8(2) . . ? O1 Sm1 O2 50.6(2) . . ? O5 Sm1 O4 49.9(2) . . ? O7 Sm1 O4 117.5(2) . . ? O1 Sm1 O4 70.6(2) . . ? O2 Sm1 O4 115.1(2) . . ? O5 Sm1 O8 71.8(2) . . ? O7 Sm1 O8 50.7(2) . . ? O1 Sm1 O8 118.4(2) . . ? O2 Sm1 O8 116.5(2) . . ? O4 Sm1 O8 113.8(2) . . ? O5 Sm1 N2 119.4(2) . . ? O7 Sm1 N2 143.1(2) . . ? O1 Sm1 N2 78.8(2) . . ? O2 Sm1 N2 72.2(2) . . ? O4 Sm1 N2 71.7(2) . . ? O8 Sm1 N2 162.7(2) . . ? O5 Sm1 N4 78.0(2) . . ? O7 Sm1 N4 118.5(2) . . ? O1 Sm1 N4 139.2(2) . . ? O2 Sm1 N4 166.0(2) . . ? O4 Sm1 N4 69.9(2) . . ? O8 Sm1 N4 70.0(2) . . ? N2 Sm1 N4 98.3(2) . . ? O5 Sm1 N6 141.6(2) . . ? O7 Sm1 N6 76.2(2) . . ? O1 Sm1 N6 118.3(2) . . ? O2 Sm1 N6 69.7(2) . . ? O4 Sm1 N6 166.1(2) . . ? O8 Sm1 N6 72.6(2) . . ? N2 Sm1 N6 98.7(2) . . ? N4 Sm1 N6 102.5(2) . . ? O5 Sm1 N1 139.4(2) . . ? O7 Sm1 N1 135.7(2) . . ? O1 Sm1 N1 139.4(2) . . ? O2 Sm1 N1 103.7(2) . . ? O4 Sm1 N1 104.4(2) . . ? O8 Sm1 N1 100.7(2) . . ? N2 Sm1 N1 62.1(2) . . ? N4 Sm1 N1 62.4(2) . . ? N6 Sm1 N1 61.7(2) . . ? O5 Sm1 N8 91.3(2) . . ? O7 Sm1 N8 68.1(2) . . ? O1 Sm1 N8 25.3(2) . . ? O2 Sm1 N8 25.5(2) . . ? O4 Sm1 N8 93.7(2) . . ? O8 Sm1 N8 118.8(2) . . ? N2 Sm1 N8 75.9(2) . . ? N4 Sm1 N8 163.6(2) . . ? N6 Sm1 N8 93.6(2) . . ? N1 Sm1 N8 124.8(2) . . ? O5 Sm1 N10 66.8(2) . . ? O7 Sm1 N10 25.1(2) . . ? O1 Sm1 N10 94.2(2) . . ? O2 Sm1 N10 94.9(2) . . ? O4 Sm1 N10 116.5(2) . . ? O8 Sm1 N10 25.8(2) . . ? N2 Sm1 N10 167.1(2) . . ? N4 Sm1 N10 94.0(2) . . ? N6 Sm1 N10 74.9(2) . . ? N1 Sm1 N10 121.7(2) . . ? N8 Sm1 N10 93.1(2) . . ? O11 Sm2 O17 116.3(2) . . ? O11 Sm2 O10 50.6(2) . . ? O17 Sm2 O10 114.9(2) . . ? O11 Sm2 O16 70.1(2) . . ? O17 Sm2 O16 50.7(2) . . ? O10 Sm2 O16 70.2(2) . . ? O11 Sm2 O14 73.5(2) . . ? O17 Sm2 O14 109.8(2) . . ? O10 Sm2 O14 119.1(2) . . ? O16 Sm2 O14 115.4(2) . . ? O11 Sm2 O13 69.6(2) . . ? O17 Sm2 O13 68.9(2) . . ? O10 Sm2 O13 115.4(2) . . ? O16 Sm2 O13 68.4(2) . . ? O14 Sm2 O13 49.4(2) . . ? O11 Sm2 N16 119.9(2) . . ? O17 Sm2 N16 74.6(2) . . ? O10 Sm2 N16 70.7(2) . . ? O16 Sm2 N16 80.2(2) . . ? O14 Sm2 N16 163.2(2) . . ? O13 Sm2 N16 141.9(2) . . ? O11 Sm2 N14 76.4(2) . . ? O17 Sm2 N14 166.9(2) . . ? O10 Sm2 N14 75.2(2) . . ? O16 Sm2 N14 142.2(2) . . ? O14 Sm2 N14 69.3(2) . . ? O13 Sm2 N14 115.5(2) . . ? N16 Sm2 N14 102.5(2) . . ? O11 Sm2 N12 142.7(2) . . ? O17 Sm2 N12 68.1(2) . . ? O10 Sm2 N12 165.1(2) . . ? O16 Sm2 N12 117.3(2) . . ? O14 Sm2 N12 70.6(2) . . ? O13 Sm2 N12 79.4(2) . . ? N16 Sm2 N12 97.3(2) . . ? N14 Sm2 N12 99.9(2) . . ? O11 Sm2 N11 136.5(2) . . ? O17 Sm2 N11 106.4(2) . . ? O10 Sm2 N11 104.3(2) . . ? O16 Sm2 N11 142.0(2) . . ? O14 Sm2 N11 100.2(2) . . ? O13 Sm2 N11 138.1(2) . . ? N16 Sm2 N11 63.2(2) . . ? N14 Sm2 N11 61.7(2) . . ? N12 Sm2 N11 61.6(2) . . ? O11 Sm2 N18 25.3(2) . . ? O17 Sm2 N18 117.1(2) . . ? O10 Sm2 N18 25.5(2) . . ? O16 Sm2 N18 66.5(2) . . ? O14 Sm2 N18 97.0(2) . . ? O13 Sm2 N18 91.9(2) . . ? N16 Sm2 N18 95.1(2) . . ? N14 Sm2 N18 75.7(2) . . ? N12 Sm2 N18 167.6(2) . . ? N11 Sm2 N18 123.7(2) . . ? O11 Sm2 N20 91.8(2) . . ? O17 Sm2 N20 25.7(2) . . ? O10 Sm2 N20 93.9(2) . . ? O16 Sm2 N20 25.3(2) . . ? O14 Sm2 N20 111.9(2) . . ? O13 Sm2 N20 63.0(2) . . ? N16 Sm2 N20 79.4(2) . . ? N14 Sm2 N20 167.3(2) . . ? N12 Sm2 N20 92.2(2) . . ? N11 Sm2 N20 128.7(2) . . ? N18 Sm2 N20 91.7(2) . . ? N1 C1 C2 108.9(7) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 112.4(8) . . ? N2 C2 C1 122.5(8) . . ? N3 C2 C1 125.1(7) . . ? C8 C3 C4 120.1(9) . . ? C8 C3 N2 108.5(8) . . ? C4 C3 N2 131.4(9) . . ? C3 C4 C5 118.7(10) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 118.9(10) . . ? C6 C5 H5A 120.6 . . ? C4 C5 H5A 120.6 . . ? C5 C6 C7 123.4(11) . . ? C5 C6 H6A 118.3 . . ? C7 C6 H6A 118.3 . . ? C6 C7 C8 117.3(10) . . ? C6 C7 H7A 121.3 . . ? C8 C7 H7A 121.3 . . ? N3 C8 C3 106.6(8) . . ? N3 C8 C7 131.9(9) . . ? C3 C8 C7 121.5(9) . . ? N3 C9 C10 113.9(8) . . ? N3 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N3 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C15 C10 C11 117.9(9) . . ? C15 C10 C9 120.8(9) . . ? C11 C10 C9 121.3(9) . . ? C10 C11 C12 118.9(12) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 121.7(13) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 122.5(13) . . ? C12 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C15 116.0(12) . . ? C13 C14 H14A 122.0 . . ? C15 C14 H14A 122.0 . . ? C10 C15 C14 122.9(11) . . ? C10 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? N1 C16 C17 109.6(7) . . ? N1 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? N1 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N4 C17 N5 112.3(7) . . ? N4 C17 C16 122.8(7) . . ? N5 C17 C16 124.8(7) . . ? C19 C18 N4 131.7(8) . . ? C19 C18 C23 119.9(8) . . ? N4 C18 C23 108.4(8) . . ? C18 C19 C20 118.8(9) . . ? C18 C19 H19A 120.6 . . ? C20 C19 H19A 120.6 . . ? C19 C20 C21 121.8(9) . . ? C19 C20 H20A 119.1 . . ? C21 C20 H20A 119.1 . . ? C22 C21 C20 119.5(9) . . ? C22 C21 H21A 120.2 . . ? C20 C21 H21A 120.2 . . ? C21 C22 C23 118.3(9) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? N5 C23 C22 131.9(9) . . ? N5 C23 C18 106.6(7) . . ? C22 C23 C18 121.5(9) . . ? N5 C24 C25 112.0(8) . . ? N5 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N5 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C30 117.5(10) . . ? C26 C25 C24 121.4(9) . . ? C30 C25 C24 121.1(9) . . ? C25 C26 C27 119.9(11) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 122.6(13) . . ? C28 C27 H27A 118.7 . . ? C26 C27 H27A 118.7 . . ? C27 C28 C29 117.3(15) . . ? C27 C28 H28A 121.4 . . ? C29 C28 H28A 121.4 . . ? C30 C29 C28 120.6(15) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C25 121.0(12) . . ? C29 C30 H30A 119.5 . . ? C25 C30 H30A 119.5 . . ? C32 C31 N1 110.6(7) . . ? C32 C31 H31A 109.5 . . ? N1 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? N1 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N6 C32 N7 113.1(8) . . ? N6 C32 C31 121.1(8) . . ? N7 C32 C31 125.7(8) . . ? N6 C33 C34 130.8(9) . . ? N6 C33 C38 108.7(8) . . ? C34 C33 C38 120.5(9) . . ? C33 C34 C35 115.9(9) . . ? C33 C34 H34A 122.0 . . ? C35 C34 H34A 122.0 . . ? C36 C35 C34 121.7(10) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C35 C36 C37 124.1(10) . . ? C35 C36 H36A 118.0 . . ? C37 C36 H36A 118.0 . . ? C36 C37 C38 114.9(9) . . ? C36 C37 H37A 122.6 . . ? C38 C37 H37A 122.6 . . ? C37 C38 N7 132.3(9) . . ? C37 C38 C33 122.9(9) . . ? N7 C38 C33 104.8(8) . . ? N7 C39 C40 112.9(4) . . ? N7 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? N7 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C45 C40 C41 121.2(6) . . ? C45 C40 C39 117.1(6) . . ? C41 C40 C39 121.2 . . ? C42 C41 C40 121.4(6) . . ? C42 C41 H41A 119.3 . . ? C40 C41 H41A 119.3 . . ? C41 C42 C43 113.7(11) . . ? C41 C42 H42A 123.1 . . ? C43 C42 H42A 123.1 . . ? C44 C43 C42 128.6(14) . . ? C44 C43 H43A 115.7 . . ? C42 C43 H43A 115.7 . . ? C43 C44 C45 114.8(14) . . ? C43 C44 H44A 122.6 . . ? C45 C44 H44A 122.6 . . ? C40 C45 C44 119.9(11) . . ? C40 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C47 C46 N11 110.9(7) . . ? C47 C46 H46A 109.5 . . ? N11 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? N11 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? N12 C47 N13 114.1(8) . . ? N12 C47 C46 123.6(8) . . ? N13 C47 C46 122.2(8) . . ? C49 C48 C53 119.8(9) . . ? C49 C48 N12 133.6(9) . . ? C53 C48 N12 106.5(8) . . ? C48 C49 C50 120.1(11) . . ? C48 C49 H49A 119.9 . . ? C50 C49 H49A 119.9 . . ? C49 C50 C51 119.8(11) . . ? C49 C50 H50A 120.1 . . ? C51 C50 H50A 120.1 . . ? C52 C51 C50 122.5(12) . . ? C52 C51 H51A 118.8 . . ? C50 C51 H51A 118.8 . . ? C51 C52 C53 116.1(12) . . ? C51 C52 H52A 121.9 . . ? C53 C52 H52A 121.9 . . ? N13 C53 C52 131.1(10) . . ? N13 C53 C48 107.2(8) . . ? C52 C53 C48 121.5(9) . . ? N13 C54 C55 110.5(8) . . ? N13 C54 H54A 109.5 . . ? C55 C54 H54A 109.5 . . ? N13 C54 H54B 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? C60 C55 C56 118.3(11) . . ? C60 C55 C54 122.4(10) . . ? C56 C55 C54 119.3(10) . . ? C57 C56 C55 118.8(12) . . ? C57 C56 H56A 120.6 . . ? C55 C56 H56A 120.6 . . ? C58 C57 C56 123.4(13) . . ? C58 C57 H57A 118.3 . . ? C56 C57 H57A 118.3 . . ? C57 C58 C59 117.0(13) . . ? C57 C58 H58A 121.5 . . ? C59 C58 H58A 121.5 . . ? C58 C59 C60 122.5(13) . . ? C58 C59 H59A 118.8 . . ? C60 C59 H59A 118.8 . . ? C59 C60 C55 119.9(12) . . ? C59 C60 H60A 120.0 . . ? C55 C60 H60A 120.0 . . ? N11 C61 C62 107.8(7) . . ? N11 C61 H61A 110.1 . . ? C62 C61 H61A 110.1 . . ? N11 C61 H61B 110.1 . . ? C62 C61 H61B 110.1 . . ? H61A C61 H61B 108.5 . . ? N14 C62 N15 112.2(7) . . ? N14 C62 C61 121.8(7) . . ? N15 C62 C61 125.7(7) . . ? C64 C63 N14 133.1(8) . . ? C64 C63 C68 120.3(8) . . ? N14 C63 C68 106.6(7) . . ? C63 C64 C65 117.6(9) . . ? C63 C64 H64A 121.2 . . ? C65 C64 H64A 121.2 . . ? C66 C65 C64 121.7(9) . . ? C66 C65 H65A 119.2 . . ? C64 C65 H65A 119.2 . . ? C67 C66 C65 121.3(10) . . ? C67 C66 H66A 119.3 . . ? C65 C66 H66A 119.3 . . ? C66 C67 C68 117.5(9) . . ? C66 C67 H67A 121.3 . . ? C68 C67 H67A 121.3 . . ? N15 C68 C67 131.4(8) . . ? N15 C68 C63 107.0(7) . . ? C67 C68 C63 121.6(8) . . ? N15 C69 C70 114.6(7) . . ? N15 C69 H69A 108.6 . . ? C70 C69 H69A 108.6 . . ? N15 C69 H69B 108.6 . . ? C70 C69 H69B 108.6 . . ? H69A C69 H69B 107.6 . . ? C75 C70 C71 120.3(10) . . ? C75 C70 C69 119.8(9) . . ? C71 C70 C69 119.9(9) . . ? C72 C71 C70 118.3(11) . . ? C72 C71 H71A 120.8 . . ? C70 C71 H71A 120.9 . . ? C73 C72 C71 124.5(12) . . ? C73 C72 H72A 117.7 . . ? C71 C72 H72A 117.7 . . ? C72 C73 C74 116.2(13) . . ? C72 C73 H73A 121.9 . . ? C74 C73 H73A 121.9 . . ? C75 C74 C73 121.2(12) . . ? C75 C74 H74A 119.4 . . ? C73 C74 H74A 119.4 . . ? C70 C75 C74 119.4(11) . . ? C70 C75 H75A 120.3 . . ? C74 C75 H75A 120.3 . . ? C77 C76 N11 108.4(6) . . ? C77 C76 H76A 110.0 . . ? N11 C76 H76A 110.0 . . ? C77 C76 H76B 110.0 . . ? N11 C76 H76B 110.0 . . ? H76A C76 H76B 108.4 . . ? N16 C77 N17 113.3(8) . . ? N16 C77 C76 121.9(7) . . ? N17 C77 C76 124.5(7) . . ? C79 C78 N16 131.0(8) . . ? C79 C78 C83 121.6(9) . . ? N16 C78 C83 107.4(8) . . ? C78 C79 C80 116.6(9) . . ? C78 C79 H79A 121.7 . . ? C80 C79 H79A 121.7 . . ? C81 C80 C79 121.1(11) . . ? C81 C80 H80A 119.4 . . ? C79 C80 H80A 119.4 . . ? C82 C81 C80 121.9(10) . . ? C82 C81 H81A 119.1 . . ? C80 C81 H81A 119.1 . . ? C81 C82 C83 116.9(10) . . ? C81 C82 H82A 121.5 . . ? C83 C82 H82A 121.5 . . ? N17 C83 C78 107.2(8) . . ? N17 C83 C82 131.0(9) . . ? C78 C83 C82 121.8(9) . . ? N17 C84 C85 113.7(7) . . ? N17 C84 H84A 108.8 . . ? C85 C84 H84A 108.8 . . ? N17 C84 H84B 108.8 . . ? C85 C84 H84B 108.8 . . ? H84A C84 H84B 107.7 . . ? C90 C85 C86 116.4(10) . . ? C90 C85 C84 121.9(9) . . ? C86 C85 C84 121.6(9) . . ? C87 C86 C85 120.1(11) . . ? C87 C86 H86A 119.9 . . ? C85 C86 H86A 119.9 . . ? C88 C87 C86 121.0(12) . . ? C88 C87 H87A 119.5 . . ? C86 C87 H87A 119.5 . . ? C89 C88 C87 120.2(13) . . ? C89 C88 H88A 119.9 . . ? C87 C88 H88A 119.9 . . ? C88 C89 C90 118.3(15) . . ? C88 C89 H89A 120.8 . . ? C90 C89 H89A 120.8 . . ? C85 C90 C89 123.9(12) . . ? C85 C90 H90A 118.0 . . ? C89 C90 H90A 118.0 . . ? C16 N1 C1 108.8(7) . . ? C16 N1 C31 111.6(7) . . ? C1 N1 C31 110.4(7) . . ? C16 N1 Sm1 110.0(5) . . ? C1 N1 Sm1 108.7(5) . . ? C31 N1 Sm1 107.4(5) . . ? C2 N2 C3 105.4(7) . . ? C2 N2 Sm1 118.4(6) . . ? C3 N2 Sm1 135.3(5) . . ? C8 N3 C2 107.1(7) . . ? C8 N3 C9 126.5(8) . . ? C2 N3 C9 126.3(8) . . ? C17 N4 C18 105.8(7) . . ? C17 N4 Sm1 117.8(5) . . ? C18 N4 Sm1 134.6(5) . . ? C17 N5 C23 106.9(7) . . ? C17 N5 C24 127.3(7) . . ? C23 N5 C24 125.6(7) . . ? C32 N6 C33 105.6(7) . . ? C32 N6 Sm1 118.0(6) . . ? C33 N6 Sm1 135.3(5) . . ? C32 N7 C38 107.8(7) . . ? C32 N7 C39 127.3(7) . . ? C38 N7 C39 124.7(7) . . ? O3 N8 O1 121.1(8) . . ? O3 N8 O2 121.2(8) . . ? O1 N8 O2 117.7(7) . . ? O3 N8 Sm1 174.3(7) . . ? O1 N8 Sm1 58.8(4) . . ? O2 N8 Sm1 59.4(4) . . ? O6 N9 O5 123.5(9) . . ? O6 N9 O4 121.7(9) . . ? O5 N9 O4 114.8(7) . . ? O6 N9 Sm1 178.6(7) . . ? O5 N9 Sm1 55.4(4) . . ? O4 N9 Sm1 59.4(4) . . ? O9 N10 O7 122.0(8) . . ? O9 N10 O8 120.8(8) . . ? O7 N10 O8 117.2(8) . . ? O9 N10 Sm1 173.6(6) . . ? O7 N10 Sm1 57.2(4) . . ? O8 N10 Sm1 60.5(5) . . ? C61 N11 C46 109.6(6) . . ? C61 N11 C76 109.7(6) . . ? C46 N11 C76 110.7(6) . . ? C61 N11 Sm2 109.7(5) . . ? C46 N11 Sm2 108.2(4) . . ? C76 N11 Sm2 108.9(4) . . ? C47 N12 C48 106.6(7) . . ? C47 N12 Sm2 112.2(5) . . ? C48 N12 Sm2 128.2(5) . . ? C47 N13 C53 105.5(8) . . ? C47 N13 C54 126.2(8) . . ? C53 N13 C54 126.8(8) . . ? C62 N14 C63 107.3(7) . . ? C62 N14 Sm2 118.6(5) . . ? C63 N14 Sm2 134.1(5) . . ? C62 N15 C68 106.9(7) . . ? C62 N15 C69 128.1(7) . . ? C68 N15 C69 125.0(7) . . ? C77 N16 C78 106.2(7) . . ? C77 N16 Sm2 119.0(6) . . ? C78 N16 Sm2 134.7(5) . . ? C77 N17 C83 105.8(7) . . ? C77 N17 C84 128.8(8) . . ? C83 N17 C84 125.4(8) . . ? O12 N18 O11 122.3(9) . . ? O12 N18 O10 120.4(9) . . ? O11 N18 O10 117.3(8) . . ? O12 N18 Sm2 172.7(7) . . ? O11 N18 Sm2 58.2(4) . . ? O10 N18 Sm2 59.3(4) . . ? O15 N19 O14 122.9(9) . . ? O15 N19 O13 119.8(9) . . ? O14 N19 O13 117.3(8) . . ? O15 N19 Sm2 169.2(7) . . ? O14 N19 Sm2 59.2(5) . . ? O13 N19 Sm2 59.5(4) . . ? O18 N20 O16 123.1(8) . . ? O18 N20 O17 120.9(8) . . ? O16 N20 O17 115.9(7) . . ? O18 N20 Sm2 165.4(7) . . ? O16 N20 Sm2 59.1(4) . . ? O17 N20 Sm2 58.2(4) . . ? N8 O1 Sm1 96.0(5) . . ? N8 O2 Sm1 95.1(5) . . ? N9 O4 Sm1 95.5(5) . . ? N9 O5 Sm1 99.7(5) . . ? N10 O7 Sm1 97.7(5) . . ? N10 O8 Sm1 93.7(5) . . ? N18 O10 Sm2 95.2(5) . . ? N18 O11 Sm2 96.5(5) . . ? N19 O13 Sm2 95.5(5) . . ? N19 O14 Sm2 96.1(5) . . ? N20 O16 Sm2 95.6(5) . . ? N20 O17 Sm2 96.1(5) . . ? C91 O19 C93 109.9(16) . . ? O19 C91 C92 123(2) . . ? O19 C91 H91A 106.6 . . ? C92 C91 H91A 106.6 . . ? O19 C91 H91B 106.6 . . ? C92 C91 H91B 106.6 . . ? H91A C91 H91B 106.6 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O19 C93 C94 107(2) . . ? O19 C93 H93A 110.3 . . ? C94 C93 H93A 110.3 . . ? O19 C93 H93B 110.3 . . ? C94 C93 H93B 110.3 . . ? H93A C93 H93B 108.5 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.301 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.158 #================================END