# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Song Dang' _publ_contact_author_email dangsong@ciac.jl.cn _publ_author_name 'Song Dang' data_LaL _database_code_depnum_ccdc_archive 'CCDC 891416' #TrackingRef '- LnL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H54 La2 N2 O21' _chemical_formula_weight 1392.85 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 33.136(6) _cell_length_b 7.3933(12) _cell_length_c 14.349(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.510(3) _cell_angle_gamma 90.00 _cell_volume 3403.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5479 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6349 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _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 9109 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.99 _reflns_number_total 6423 _reflns_number_gt 5468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0641P)^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 constr _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 -0.01(3) _refine_ls_number_reflns 6423 _refine_ls_number_parameters 375 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.002 _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 La1 La 0.749342(10) 1.25673(9) 0.03623(2) 0.02835(12) Uani 1 1 d . . . N1 N 0.4456(5) 0.046(4) 0.9015(12) 0.148(7) Uani 1 1 d . . . O1 O 0.30389(15) 0.5284(7) 0.0424(4) 0.0347(12) Uani 1 1 d . . . O2 O 0.32897(14) 0.2643(15) 0.0222(4) 0.0545(14) Uani 1 1 d . . . O3 O 0.7213(2) 1.1617(9) 0.1739(4) 0.0516(16) Uani 1 1 d . . . O4 O 0.72005(16) 0.9403(7) 0.0719(4) 0.0343(12) Uani 1 1 d . . . O5 O 0.73267(15) 0.0743(7) 0.8839(3) 0.0316(11) Uani 1 1 d . . . O6 O 0.69523(18) -0.1546(8) 0.8154(4) 0.0435(14) Uani 1 1 d . . . O7 O 0.60210(18) 0.6110(8) 0.3154(4) 0.0468(15) Uani 1 1 d . . . O8 O 0.60725(18) 0.4811(8) 0.5423(4) 0.0447(15) Uani 1 1 d . . . O9 O 0.49255(16) 0.6234(8) 0.2756(4) 0.0460(15) Uani 1 1 d . . . O10 O 0.5000 0.5775(11) 0.5000 0.0386(18) Uani 1 2 d S . . O11 O 0.4732(5) 0.0763(19) 0.7822(10) 0.148(5) Uani 1 1 d . . . C1 C 0.5520(2) 0.5728(11) 0.4105(5) 0.0297(17) Uani 1 1 d . . . C2 C 0.5294(2) 0.6843(11) 0.4709(6) 0.0376(19) Uani 1 1 d . . . H2A H 0.5494 0.7314 0.5270 0.045 Uiso 1 1 calc R . . H2B H 0.5156 0.7860 0.4334 0.045 Uiso 1 1 calc R . . C3 C 0.5744(2) 0.4139(11) 0.4661(5) 0.0356(18) Uani 1 1 d . . . H3A H 0.5552 0.3428 0.4921 0.043 Uiso 1 1 calc R . . H3B H 0.5857 0.3371 0.4240 0.043 Uiso 1 1 calc R . . C4 C 0.5812(2) 0.7025(10) 0.3776(5) 0.035(2) Uani 1 1 d . . . H4A H 0.5653 0.8035 0.3437 0.042 Uiso 1 1 calc R . . H4B H 0.6015 0.7497 0.4331 0.042 Uiso 1 1 calc R . . C5 C 0.5200(2) 0.4882(11) 0.3247(6) 0.0351(18) Uani 1 1 d . . . H5A H 0.5344 0.4324 0.2810 0.042 Uiso 1 1 calc R . . H5B H 0.5042 0.3952 0.3477 0.042 Uiso 1 1 calc R . . C6 C 0.6278(3) 0.7145(12) 0.2755(7) 0.042(3) Uani 1 1 d . . . C7 C 0.6363(3) 0.8918(15) 0.2981(7) 0.053(3) Uani 1 1 d . . . H7A H 0.6242 0.9499 0.3419 0.063 Uiso 1 1 calc R . . C8 C 0.6635(3) 0.9854(14) 0.2544(7) 0.051(2) Uani 1 1 d . . . H8A H 0.6691 1.1069 0.2688 0.061 Uiso 1 1 calc R . . C9 C 0.6820(3) 0.9011(13) 0.1911(6) 0.0376(19) Uani 1 1 d . . . C10 C 0.6735(3) 0.7183(14) 0.1700(7) 0.050(3) Uani 1 1 d . . . H10A H 0.6858 0.6584 0.1273 0.060 Uiso 1 1 calc R . . C11 C 0.6467(3) 0.6280(14) 0.2129(7) 0.057(3) Uani 1 1 d . . . H11A H 0.6412 0.5061 0.1994 0.068 Uiso 1 1 calc R . . C12 C 0.4544(2) 0.5673(12) 0.2187(5) 0.0371(19) Uani 1 1 d . . . C13 C 0.4251(2) 0.7012(11) 0.1922(6) 0.047(2) Uani 1 1 d . . . H13A H 0.4314 0.8206 0.2106 0.057 Uiso 1 1 calc R . . C14 C 0.3856(2) 0.6538(11) 0.1371(6) 0.042(2) Uani 1 1 d . . . H14A H 0.3653 0.7427 0.1189 0.050 Uiso 1 1 calc R . . C15 C 0.3762(2) 0.4761(10) 0.1089(5) 0.0311(16) Uani 1 1 d . . . C16 C 0.4071(2) 0.3479(12) 0.1366(6) 0.046(2) Uani 1 1 d . . . H16A H 0.4012 0.2279 0.1188 0.055 Uiso 1 1 calc R . . C17 C 0.4465(2) 0.3928(12) 0.1902(6) 0.045(2) Uani 1 1 d . . . H17A H 0.4673 0.3053 0.2064 0.054 Uiso 1 1 calc R . . C18 C 0.3344(2) 0.4202(11) 0.0538(5) 0.0316(17) Uani 1 1 d . . . C19 C 0.6290(3) 0.3577(16) 0.6051(7) 0.036(3) Uani 1 1 d . . . C20 C 0.6208(4) 0.1752(17) 0.6037(9) 0.052(3) Uani 1 1 d . . . H20A H 0.5992 0.1267 0.5560 0.062 Uiso 1 1 calc R . . C21 C 0.6445(3) 0.0657(16) 0.6723(8) 0.051(3) Uani 1 1 d . . . H21A H 0.6380 -0.0566 0.6722 0.062 Uiso 1 1 calc R . . C22 C 0.6785(3) 0.1317(12) 0.7428(7) 0.030(2) Uani 1 1 d . . . C23 C 0.6867(3) 0.3146(11) 0.7436(7) 0.037(3) Uani 1 1 d . . . H23A H 0.7088 0.3622 0.7904 0.045 Uiso 1 1 calc R . . C24 C 0.6621(3) 0.4295(12) 0.6748(7) 0.037(2) Uani 1 1 d . . . H24A H 0.6678 0.5527 0.6756 0.044 Uiso 1 1 calc R . . C25 C 0.7031(2) 0.0093(11) 0.8175(5) 0.0337(17) Uani 1 1 d . . . C26 C 0.4384(11) 0.268(7) 0.8961(19) 0.282(19) Uani 1 1 d . . . H26A H 0.4491 0.3170 0.8451 0.424 Uiso 1 1 calc R . . H26B H 0.4529 0.3217 0.9562 0.424 Uiso 1 1 calc R . . H26C H 0.4092 0.2942 0.8840 0.424 Uiso 1 1 calc R . . C27 C 0.4354(8) -0.069(5) 0.9623(14) 0.245(18) Uani 1 1 d . . . H27A H 0.4434 -0.1893 0.9487 0.367 Uiso 1 1 calc R . . H27B H 0.4059 -0.0652 0.9554 0.367 Uiso 1 1 calc R . . H27C H 0.4497 -0.0369 1.0270 0.367 Uiso 1 1 calc R . . C28 C 0.4642(7) -0.015(3) 0.8385(14) 0.137(8) Uani 1 1 d . . . H28A H 0.4706 -0.1375 0.8389 0.164 Uiso 1 1 calc R . . C29 C 0.7093(2) 1.0070(12) 0.1437(6) 0.0367(18) 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 La1 0.02424(18) 0.02574(19) 0.0330(2) 0.0003(3) 0.00326(13) -0.0011(3) N1 0.125(13) 0.23(2) 0.088(11) 0.015(12) 0.017(9) -0.063(14) O1 0.021(3) 0.035(3) 0.043(3) -0.003(2) -0.001(2) 0.008(2) O2 0.026(2) 0.039(3) 0.089(4) -0.011(6) -0.003(2) 0.002(5) O3 0.070(4) 0.051(4) 0.043(3) -0.010(3) 0.032(3) -0.017(3) O4 0.037(3) 0.030(3) 0.044(3) 0.007(2) 0.026(2) 0.010(2) O5 0.029(3) 0.033(3) 0.026(3) 0.002(2) -0.006(2) -0.002(2) O6 0.043(3) 0.034(3) 0.042(3) 0.004(3) -0.012(3) -0.005(3) O7 0.044(3) 0.049(4) 0.059(4) 0.004(3) 0.035(3) -0.009(3) O8 0.043(3) 0.041(3) 0.037(3) 0.012(3) -0.016(3) 0.002(3) O9 0.027(3) 0.041(3) 0.057(4) 0.009(3) -0.014(3) -0.008(3) O10 0.041(4) 0.041(4) 0.043(5) 0.000 0.027(4) 0.000 O11 0.175(13) 0.129(11) 0.158(12) -0.041(10) 0.076(10) -0.067(10) C1 0.017(3) 0.047(5) 0.023(4) 0.009(3) 0.000(3) -0.002(3) C2 0.031(4) 0.044(4) 0.040(4) 0.004(3) 0.012(3) -0.001(3) C3 0.033(4) 0.043(5) 0.029(4) 0.000(3) 0.004(3) 0.001(4) C4 0.022(3) 0.049(6) 0.036(4) 0.009(3) 0.012(3) 0.000(3) C5 0.019(3) 0.043(5) 0.039(4) 0.005(4) -0.001(3) 0.000(3) C6 0.038(4) 0.045(8) 0.050(5) 0.011(4) 0.025(4) -0.002(4) C7 0.060(6) 0.056(6) 0.055(6) -0.009(5) 0.039(5) -0.010(5) C8 0.060(6) 0.046(5) 0.058(6) -0.005(5) 0.037(5) -0.013(5) C9 0.042(5) 0.042(5) 0.031(4) 0.003(4) 0.015(4) -0.011(4) C10 0.052(5) 0.051(10) 0.059(5) -0.004(5) 0.038(4) -0.004(5) C11 0.074(7) 0.038(5) 0.073(7) -0.005(5) 0.045(6) -0.015(5) C12 0.020(4) 0.050(5) 0.036(4) 0.006(4) -0.003(3) -0.004(3) C13 0.033(4) 0.037(5) 0.059(6) 0.001(4) -0.010(4) -0.002(3) C14 0.028(4) 0.036(5) 0.054(5) 0.006(4) -0.005(4) 0.002(3) C15 0.021(3) 0.035(4) 0.035(4) 0.000(3) 0.001(3) 0.002(3) C16 0.035(4) 0.036(4) 0.056(6) -0.006(4) -0.006(4) 0.005(4) C17 0.030(4) 0.042(5) 0.054(5) -0.001(4) -0.007(4) 0.011(4) C18 0.024(4) 0.034(5) 0.035(4) 0.002(3) 0.004(3) -0.003(3) C19 0.031(5) 0.043(6) 0.027(5) 0.009(5) -0.004(4) 0.003(4) C20 0.048(6) 0.038(6) 0.049(7) 0.001(5) -0.026(5) -0.007(5) C21 0.049(6) 0.044(6) 0.050(6) -0.011(5) -0.008(5) -0.010(5) C22 0.029(4) 0.031(5) 0.029(5) -0.002(4) 0.003(3) 0.002(4) C23 0.039(5) 0.034(6) 0.029(4) 0.008(3) -0.010(4) -0.005(4) C24 0.040(5) 0.023(5) 0.038(5) 0.004(4) -0.006(4) -0.009(4) C25 0.037(4) 0.036(5) 0.026(4) 0.002(3) 0.006(3) 0.001(3) C26 0.36(5) 0.25(4) 0.23(3) -0.04(4) 0.08(3) 0.15(4) C27 0.19(2) 0.40(5) 0.098(14) 0.06(2) -0.052(14) -0.17(3) C28 0.147(17) 0.17(2) 0.092(13) -0.028(14) 0.033(12) -0.087(15) C29 0.032(4) 0.047(5) 0.032(4) 0.005(4) 0.008(3) 0.000(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 La1 O1 2.459(5) 3 ? La1 O4 2.463(5) 4_655 ? La1 O3 2.485(6) . ? La1 O5 2.509(5) 1_564 ? La1 O2 2.520(5) 2_665 ? La1 O6 2.525(5) 4_666 ? La1 O5 2.615(5) 4_666 ? La1 O4 2.631(5) . ? La1 O1 2.724(5) 2_665 ? La1 C29 2.928(8) . ? La1 C25 2.952(8) 4_666 ? La1 C18 3.006(7) 2_665 ? N1 C28 1.30(2) . ? N1 C27 1.32(3) . ? N1 C26 1.66(5) . ? O1 C18 1.268(9) . ? O1 La1 2.459(5) 3_445 ? O1 La1 2.724(5) 2_645 ? O2 C18 1.236(13) . ? O2 La1 2.520(5) 2_645 ? O3 C29 1.251(10) . ? O4 C29 1.271(9) . ? O4 La1 2.463(5) 4_645 ? O5 C25 1.276(9) . ? O5 La1 2.509(5) 1_546 ? O5 La1 2.615(5) 4_636 ? O6 C25 1.239(10) . ? O6 La1 2.525(5) 4_636 ? O7 C6 1.372(10) . ? O7 C4 1.431(9) . ? O8 C19 1.355(12) . ? O8 C3 1.425(9) . ? O9 C12 1.384(8) . ? O9 C5 1.415(9) . ? O10 C2 1.397(8) . ? O10 C2 1.397(8) 2_656 ? O11 C28 1.15(2) . ? C1 C3 1.507(11) . ? C1 C4 1.517(9) . ? C1 C2 1.522(11) . ? C1 C5 1.543(10) . ? C6 C7 1.363(15) . ? C6 C11 1.375(13) . ? C7 C8 1.403(12) . ? C8 C9 1.368(12) . ? C9 C10 1.399(15) . ? C9 C29 1.483(11) . ? C10 C11 1.374(12) . ? C12 C17 1.359(12) . ? C12 C13 1.373(11) . ? C13 C14 1.393(11) . ? C14 C15 1.387(11) . ? C15 C16 1.379(11) . ? C15 C18 1.471(10) . ? C16 C17 1.380(11) . ? C18 La1 3.006(7) 2_645 ? C19 C20 1.375(11) . ? C19 C24 1.392(13) . ? C20 C21 1.361(15) . ? C21 C22 1.400(13) . ? C22 C23 1.379(13) . ? C22 C25 1.482(11) . ? C23 C24 1.400(12) . ? C25 La1 2.952(8) 4_636 ? 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 La1 O4 89.20(18) 3 4_655 ? O1 La1 O3 101.3(2) 3 . ? O4 La1 O3 162.03(18) 4_655 . ? O1 La1 O5 70.22(16) 3 1_564 ? O4 La1 O5 77.48(16) 4_655 1_564 ? O3 La1 O5 119.71(19) . 1_564 ? O1 La1 O2 135.5(3) 3 2_665 ? O4 La1 O2 109.3(2) 4_655 2_665 ? O3 La1 O2 73.2(2) . 2_665 ? O5 La1 O2 74.8(2) 1_564 2_665 ? O1 La1 O6 77.00(18) 3 4_666 ? O4 La1 O6 93.48(19) 4_655 4_666 ? O3 La1 O6 75.0(2) . 4_666 ? O5 La1 O6 145.98(18) 1_564 4_666 ? O2 La1 O6 138.2(2) 2_665 4_666 ? O1 La1 O5 121.06(16) 3 4_666 ? O4 La1 O5 72.33(16) 4_655 4_666 ? O3 La1 O5 89.73(18) . 4_666 ? O5 La1 O5 147.19(15) 1_564 4_666 ? O2 La1 O5 103.2(3) 2_665 4_666 ? O6 La1 O5 50.20(16) 4_666 4_666 ? O1 La1 O4 71.71(16) 3 . ? O4 La1 O4 147.41(14) 4_655 . ? O3 La1 O4 50.56(17) . . ? O5 La1 O4 71.34(16) 1_564 . ? O2 La1 O4 71.6(3) 2_665 . ? O6 La1 O4 107.01(18) 4_666 . ? O5 La1 O4 140.15(16) 4_666 . ? O1 La1 O1 156.21(4) 3 2_665 ? O4 La1 O1 70.06(17) 4_655 2_665 ? O3 La1 O1 101.8(2) . 2_665 ? O5 La1 O1 93.28(16) 1_564 2_665 ? O2 La1 O1 48.7(3) 2_665 2_665 ? O6 La1 O1 114.62(17) 4_666 2_665 ? O5 La1 O1 64.68(14) 4_666 2_665 ? O4 La1 O1 120.25(15) . 2_665 ? O1 La1 C29 88.5(2) 3 . ? O4 La1 C29 172.6(2) 4_655 . ? O3 La1 C29 25.1(2) . . ? O5 La1 C29 95.2(2) 1_564 . ? O2 La1 C29 67.9(2) 2_665 . ? O6 La1 C29 92.8(2) 4_666 . ? O5 La1 C29 114.8(2) 4_666 . ? O4 La1 C29 25.7(2) . . ? O1 La1 C29 110.57(19) 2_665 . ? O1 La1 C25 98.8(2) 3 4_666 ? O4 La1 C25 82.44(19) 4_655 4_666 ? O3 La1 C25 81.5(2) . 4_666 ? O5 La1 C25 157.1(2) 1_564 4_666 ? O2 La1 C25 123.0(3) 2_665 4_666 ? O6 La1 C25 24.6(2) 4_666 4_666 ? O5 La1 C25 25.60(18) 4_666 4_666 ? O4 La1 C25 125.54(19) . 4_666 ? O1 La1 C25 90.15(19) 2_665 4_666 ? C29 La1 C25 104.8(2) . 4_666 ? O1 La1 C18 151.98(19) 3 2_665 ? O4 La1 C18 89.4(2) 4_655 2_665 ? O3 La1 C18 88.1(2) . 2_665 ? O5 La1 C18 82.16(18) 1_564 2_665 ? O2 La1 C18 23.8(3) 2_665 2_665 ? O6 La1 C18 131.0(2) 4_666 2_665 ? O5 La1 C18 84.94(18) 4_666 2_665 ? O4 La1 C18 95.46(19) . 2_665 ? O1 La1 C18 24.94(18) 2_665 2_665 ? C29 La1 C18 89.4(2) . 2_665 ? C25 La1 C18 108.8(2) 4_666 2_665 ? C28 N1 C27 119(3) . . ? C28 N1 C26 114(2) . . ? C27 N1 C26 128(3) . . ? C18 O1 La1 173.5(5) . 3_445 ? C18 O1 La1 90.1(4) . 2_645 ? La1 O1 La1 95.60(16) 3_445 2_645 ? C18 O2 La1 100.7(5) . 2_645 ? C29 O3 La1 97.6(5) . . ? C29 O4 La1 165.3(5) . 4_645 ? C29 O4 La1 90.3(5) . . ? La1 O4 La1 97.90(16) 4_645 . ? C25 O5 La1 144.4(5) . 1_546 ? C25 O5 La1 92.1(4) . 4_636 ? La1 O5 La1 97.17(15) 1_546 4_636 ? C25 O6 La1 97.4(5) . 4_636 ? C6 O7 C4 116.4(6) . . ? C19 O8 C3 116.9(7) . . ? C12 O9 C5 117.4(6) . . ? C2 O10 C2 111.2(8) . 2_656 ? C3 C1 C4 113.0(6) . . ? C3 C1 C2 111.6(6) . . ? C4 C1 C2 106.1(6) . . ? C3 C1 C5 104.8(6) . . ? C4 C1 C5 111.9(6) . . ? C2 C1 C5 109.6(6) . . ? O10 C2 C1 110.1(6) . . ? O8 C3 C1 108.3(6) . . ? O7 C4 C1 109.9(6) . . ? O9 C5 C1 109.8(6) . . ? C7 C6 O7 123.4(9) . . ? C7 C6 C11 120.1(8) . . ? O7 C6 C11 116.4(8) . . ? C6 C7 C8 119.1(9) . . ? C9 C8 C7 121.2(9) . . ? C8 C9 C10 118.9(8) . . ? C8 C9 C29 119.4(8) . . ? C10 C9 C29 121.7(8) . . ? C11 C10 C9 119.5(9) . . ? C10 C11 C6 121.2(9) . . ? C17 C12 C13 122.1(7) . . ? C17 C12 O9 122.7(7) . . ? C13 C12 O9 115.2(7) . . ? C12 C13 C14 118.4(8) . . ? C15 C14 C13 120.9(7) . . ? C16 C15 C14 118.1(7) . . ? C16 C15 C18 119.6(7) . . ? C14 C15 C18 122.4(7) . . ? C15 C16 C17 121.8(8) . . ? C12 C17 C16 118.7(8) . . ? O2 C18 O1 120.2(6) . . ? O2 C18 C15 119.4(7) . . ? O1 C18 C15 120.4(7) . . ? O2 C18 La1 55.4(4) . 2_645 ? O1 C18 La1 65.0(4) . 2_645 ? C15 C18 La1 170.8(5) . 2_645 ? O8 C19 C20 125.6(11) . . ? O8 C19 C24 114.3(10) . . ? C20 C19 C24 120.1(11) . . ? C21 C20 C19 119.8(12) . . ? C20 C21 C22 122.0(11) . . ? C23 C22 C21 118.0(10) . . ? C23 C22 C25 121.4(8) . . ? C21 C22 C25 120.5(9) . . ? C22 C23 C24 120.7(10) . . ? C19 C24 C23 119.4(9) . . ? O6 C25 O5 120.3(7) . . ? O6 C25 C22 120.3(7) . . ? O5 C25 C22 119.4(7) . . ? O6 C25 La1 58.0(4) . 4_636 ? O5 C25 La1 62.3(4) . 4_636 ? C22 C25 La1 178.3(6) . 4_636 ? O11 C28 N1 123(3) . . ? O3 C29 O4 120.4(7) . . ? O3 C29 C9 120.0(8) . . ? O4 C29 C9 119.6(8) . . ? O3 C29 La1 57.3(4) . . ? O4 C29 La1 64.0(4) . . ? C9 C29 La1 169.4(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.990 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.158 data_EuL _database_code_depnum_ccdc_archive 'CCDC 891417' #TrackingRef '- LnL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H54 Eu2 N2 O21' _chemical_formula_weight 1418.95 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 32.789(3) _cell_length_b 7.1091(7) _cell_length_c 14.5399(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.454(2) _cell_angle_gamma 90.00 _cell_volume 3281.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6196 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _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 9102 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.08 _reflns_number_total 4624 _reflns_number_gt 4081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0641P)^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 constr _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 0.59(3) _refine_ls_number_reflns 4624 _refine_ls_number_parameters 375 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.218 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.003 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 0.748719(11) 1.25779(13) 0.03118(2) 0.02592(14) Uani 1 1 d . . . N1 N 0.4465(7) 0.031(5) 0.9060(14) 0.147(10) Uani 1 1 d . . . O1 O 0.3024(2) 0.5287(12) 0.0405(5) 0.0407(19) Uani 1 1 d . . . O2 O 0.32742(18) 0.253(2) 0.0333(5) 0.0531(18) Uani 1 1 d . . . O3 O 0.7176(3) 1.1829(12) 0.1593(6) 0.056(2) Uani 1 1 d . . . O4 O 0.7202(2) 0.9392(11) 0.0664(5) 0.0376(17) Uani 1 1 d . . . O5 O 0.7356(2) 0.0665(11) 0.8889(4) 0.0317(16) Uani 1 1 d . . . O6 O 0.6981(3) -0.1742(11) 0.8234(5) 0.047(2) Uani 1 1 d . . . O7 O 0.6037(3) 0.6076(13) 0.3180(6) 0.049(2) Uani 1 1 d . . . O8 O 0.6092(2) 0.4796(12) 0.5445(5) 0.046(2) Uani 1 1 d . . . O9 O 0.4936(2) 0.6210(12) 0.2793(6) 0.051(2) Uani 1 1 d . . . O10 O 0.5000 0.5774(17) 0.5000 0.044(3) Uani 1 2 d S . . O11 O 0.4735(6) 0.071(3) 0.7840(13) 0.148(7) Uani 1 1 d . . . C1 C 0.5532(3) 0.5688(16) 0.4131(7) 0.031(2) Uani 1 1 d . . . C2 C 0.5302(3) 0.6878(16) 0.4715(8) 0.040(3) Uani 1 1 d . . . H2A H 0.5502 0.7372 0.5270 0.047 Uiso 1 1 calc R . . H2B H 0.5165 0.7932 0.4338 0.047 Uiso 1 1 calc R . . C3 C 0.5762(3) 0.4072(16) 0.4691(7) 0.035(2) Uani 1 1 d . . . H3A H 0.5569 0.3329 0.4950 0.042 Uiso 1 1 calc R . . H3B H 0.5879 0.3270 0.4282 0.042 Uiso 1 1 calc R . . C4 C 0.5824(3) 0.7063(16) 0.3797(7) 0.038(3) Uani 1 1 d . . . H4A H 0.5661 0.8099 0.3456 0.045 Uiso 1 1 calc R . . H4B H 0.6029 0.7571 0.4340 0.045 Uiso 1 1 calc R . . C5 C 0.5209(3) 0.4793(17) 0.3299(7) 0.038(3) Uani 1 1 d . . . H5A H 0.5353 0.4172 0.2876 0.046 Uiso 1 1 calc R . . H5B H 0.5046 0.3857 0.3536 0.046 Uiso 1 1 calc R . . C6 C 0.6291(4) 0.7123(16) 0.2777(9) 0.042(4) Uani 1 1 d . . . C7 C 0.6373(5) 0.899(2) 0.2966(10) 0.057(4) Uani 1 1 d . . . H7A H 0.6257 0.9615 0.3402 0.069 Uiso 1 1 calc R . . C8 C 0.6634(4) 0.993(2) 0.2493(10) 0.055(3) Uani 1 1 d . . . H8A H 0.6690 1.1200 0.2623 0.066 Uiso 1 1 calc R . . C9 C 0.6811(4) 0.907(2) 0.1846(9) 0.043(3) Uani 1 1 d . . . C10 C 0.6738(5) 0.715(3) 0.1684(10) 0.066(6) Uani 1 1 d . . . H10A H 0.6864 0.6510 0.1272 0.079 Uiso 1 1 calc R . . C11 C 0.6472(4) 0.621(2) 0.2150(10) 0.057(3) Uani 1 1 d . . . H11A H 0.6417 0.4937 0.2030 0.068 Uiso 1 1 calc R . . C12 C 0.4558(3) 0.5662(18) 0.2228(8) 0.040(3) Uani 1 1 d . . . C13 C 0.4261(3) 0.7035(16) 0.1932(8) 0.045(3) Uani 1 1 d . . . H13A H 0.4328 0.8282 0.2098 0.054 Uiso 1 1 calc R . . C14 C 0.3862(3) 0.6586(17) 0.1386(8) 0.045(3) Uani 1 1 d . . . H14A H 0.3660 0.7523 0.1195 0.055 Uiso 1 1 calc R . . C15 C 0.3765(3) 0.4727(17) 0.1129(7) 0.038(3) Uani 1 1 d . . . C16 C 0.4061(3) 0.3370(18) 0.1429(8) 0.045(3) Uani 1 1 d . . . H16A H 0.3994 0.2120 0.1273 0.054 Uiso 1 1 calc R . . C17 C 0.4466(3) 0.3831(19) 0.1971(9) 0.052(3) Uani 1 1 d . . . H17A H 0.4670 0.2901 0.2154 0.062 Uiso 1 1 calc R . . C18 C 0.3334(3) 0.4143(16) 0.0588(7) 0.032(2) Uani 1 1 d . . . C19 C 0.6308(5) 0.349(3) 0.6084(12) 0.042(4) Uani 1 1 d . . . C20 C 0.6230(6) 0.160(3) 0.6091(12) 0.050(5) Uani 1 1 d . . . H20A H 0.6016 0.1069 0.5621 0.060 Uiso 1 1 calc R . . C21 C 0.6472(4) 0.048(2) 0.6800(9) 0.046(4) Uani 1 1 d . . . H21A H 0.6403 -0.0784 0.6835 0.055 Uiso 1 1 calc R . . C22 C 0.6812(4) 0.1217(18) 0.7454(9) 0.033(3) Uani 1 1 d . . . C23 C 0.6898(4) 0.3097(17) 0.7442(9) 0.039(4) Uani 1 1 d . . . H23A H 0.7120 0.3612 0.7900 0.047 Uiso 1 1 calc R . . C24 C 0.6652(4) 0.4237(18) 0.6743(9) 0.041(3) Uani 1 1 d . . . H24A H 0.6717 0.5505 0.6717 0.049 Uiso 1 1 calc R . . C25 C 0.7060(3) -0.0040(15) 0.8229(7) 0.032(2) Uani 1 1 d . . . C26 C 0.4426(16) 0.268(9) 0.907(3) 0.30(3) Uani 1 1 d . . . H26A H 0.4531 0.3192 0.8559 0.451 Uiso 1 1 calc R . . H26B H 0.4588 0.3159 0.9662 0.451 Uiso 1 1 calc R . . H26C H 0.4136 0.3030 0.8978 0.451 Uiso 1 1 calc R . . C27 C 0.4360(11) -0.092(7) 0.9688(18) 0.28(3) Uani 1 1 d . . . H27A H 0.4441 -0.2170 0.9557 0.420 Uiso 1 1 calc R . . H27B H 0.4062 -0.0877 0.9622 0.420 Uiso 1 1 calc R . . H27C H 0.4505 -0.0575 1.0324 0.420 Uiso 1 1 calc R . . C28 C 0.4636(8) -0.030(4) 0.8392(16) 0.120(9) Uani 1 1 d . . . H28A H 0.4681 -0.1584 0.8351 0.144 Uiso 1 1 calc R . . C29 C 0.7080(3) 1.0139(17) 0.1352(8) 0.039(3) 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 0.0218(2) 0.0289(2) 0.0251(2) -0.0003(4) 0.00226(13) -0.0015(4) N1 0.118(16) 0.23(3) 0.086(13) -0.004(15) 0.017(12) -0.062(18) O1 0.030(4) 0.049(5) 0.039(4) -0.006(4) 0.001(3) 0.003(3) O2 0.027(3) 0.050(5) 0.076(5) -0.007(9) 0.002(3) 0.007(8) O3 0.076(6) 0.053(6) 0.048(5) -0.016(4) 0.035(4) -0.025(4) O4 0.042(4) 0.038(4) 0.040(4) 0.003(3) 0.024(3) 0.006(3) O5 0.026(3) 0.039(4) 0.025(3) -0.001(3) -0.003(3) -0.004(3) O6 0.048(5) 0.037(5) 0.043(4) 0.003(3) -0.011(4) -0.002(3) O7 0.047(5) 0.056(6) 0.057(5) 0.006(4) 0.035(4) -0.005(4) O8 0.044(5) 0.047(5) 0.035(4) 0.002(4) -0.013(3) 0.002(4) O9 0.027(4) 0.054(6) 0.060(5) 0.016(4) -0.011(4) -0.010(4) O10 0.041(6) 0.045(7) 0.055(7) 0.000 0.030(5) 0.000 O11 0.166(17) 0.136(15) 0.158(15) -0.008(13) 0.069(13) -0.057(13) C1 0.020(5) 0.045(6) 0.027(5) 0.007(4) 0.005(4) 0.004(4) C2 0.031(5) 0.049(7) 0.041(6) 0.000(4) 0.013(4) -0.009(4) C3 0.028(5) 0.041(6) 0.034(5) 0.007(5) 0.002(4) 0.001(5) C4 0.029(5) 0.052(10) 0.036(5) 0.009(5) 0.016(4) 0.004(4) C5 0.026(5) 0.050(7) 0.037(6) 0.012(5) 0.005(4) 0.004(5) C6 0.049(6) 0.036(11) 0.051(7) 0.005(5) 0.030(5) -0.003(5) C7 0.070(9) 0.061(10) 0.056(8) 0.003(8) 0.045(7) 0.006(8) C8 0.061(8) 0.048(8) 0.073(9) -0.009(7) 0.048(7) -0.006(7) C9 0.041(6) 0.049(8) 0.045(7) -0.007(6) 0.023(5) -0.009(6) C10 0.063(8) 0.09(2) 0.054(7) -0.009(9) 0.038(6) -0.018(10) C11 0.059(8) 0.037(7) 0.079(10) -0.003(7) 0.024(7) -0.011(6) C12 0.022(5) 0.051(7) 0.040(6) 0.009(5) -0.006(4) -0.007(5) C13 0.034(5) 0.034(8) 0.058(7) 0.001(5) -0.006(5) -0.002(4) C14 0.030(6) 0.043(7) 0.057(7) 0.010(6) -0.002(5) 0.005(5) C15 0.026(5) 0.046(7) 0.040(6) 0.007(5) 0.004(4) -0.002(5) C16 0.028(5) 0.040(6) 0.060(7) -0.005(5) -0.003(5) -0.001(5) C17 0.025(6) 0.051(8) 0.069(8) -0.003(6) -0.009(5) 0.014(5) C18 0.024(5) 0.034(6) 0.036(6) 0.002(5) 0.005(4) 0.006(4) C19 0.032(7) 0.051(10) 0.034(8) 0.014(7) -0.008(6) -0.004(6) C20 0.059(10) 0.046(10) 0.031(8) 0.009(7) -0.016(7) -0.012(8) C21 0.055(8) 0.035(7) 0.036(7) 0.007(5) -0.009(6) -0.017(6) C22 0.029(6) 0.035(7) 0.031(6) -0.007(5) -0.003(5) 0.006(5) C23 0.041(7) 0.037(10) 0.029(6) 0.008(5) -0.010(5) -0.003(5) C24 0.043(7) 0.027(7) 0.047(8) -0.001(5) 0.001(6) -0.005(6) C25 0.031(5) 0.035(6) 0.028(5) 0.000(4) 0.002(4) 0.000(5) C26 0.39(7) 0.27(6) 0.23(4) 0.00(6) 0.06(4) 0.22(6) C27 0.20(3) 0.51(9) 0.096(17) 0.10(3) -0.022(19) -0.19(4) C28 0.125(19) 0.16(2) 0.091(15) -0.018(16) 0.053(14) -0.058(17) C29 0.031(6) 0.049(7) 0.040(6) 0.007(5) 0.016(5) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.332(7) 4_655 ? Eu1 O1 2.377(8) 3 ? Eu1 O3 2.397(8) . ? Eu1 O5 2.423(7) 1_564 ? Eu1 O2 2.438(6) 2_665 ? Eu1 O6 2.430(7) 4_666 ? Eu1 O5 2.476(7) 4_666 ? Eu1 O4 2.551(8) . ? Eu1 O1 2.595(8) 2_665 ? Eu1 C25 2.828(10) 4_666 ? Eu1 C29 2.844(11) . ? Eu1 C18 2.907(10) 2_665 ? N1 C28 1.31(3) . ? N1 C27 1.37(3) . ? N1 C26 1.69(7) . ? O1 C18 1.278(12) . ? O1 Eu1 2.377(8) 3_445 ? O1 Eu1 2.595(8) 2_645 ? O2 C18 1.204(19) . ? O2 Eu1 2.438(6) 2_645 ? O3 C29 1.269(14) . ? O4 C29 1.282(13) . ? O4 Eu1 2.332(7) 4_645 ? O5 C25 1.283(11) . ? O5 Eu1 2.423(7) 1_546 ? O5 Eu1 2.476(7) 4_636 ? O6 C25 1.238(13) . ? O6 Eu1 2.430(7) 4_636 ? O7 C6 1.354(13) . ? O7 C4 1.449(13) . ? O8 C19 1.378(18) . ? O8 C3 1.430(11) . ? O9 C12 1.362(12) . ? O9 C5 1.424(13) . ? O10 C2 1.404(12) 2_656 ? O10 C2 1.404(12) . ? O11 C28 1.18(3) . ? C1 C3 1.498(14) . ? C1 C2 1.525(14) . ? C1 C4 1.529(14) . ? C1 C5 1.534(14) . ? C6 C11 1.369(18) . ? C6 C7 1.37(2) . ? C7 C8 1.398(18) . ? C8 C9 1.367(17) . ? C9 C10 1.39(3) . ? C9 C29 1.478(16) . ? C10 C11 1.403(19) . ? C12 C17 1.367(18) . ? C12 C13 1.369(15) . ? C13 C14 1.389(14) . ? C14 C15 1.388(17) . ? C15 C16 1.361(16) . ? C15 C18 1.494(14) . ? C16 C17 1.403(15) . ? C18 Eu1 2.907(10) 2_645 ? C19 C20 1.368(15) . ? C19 C24 1.390(19) . ? C20 C21 1.38(2) . ? C21 C22 1.378(16) . ? C22 C23 1.367(19) . ? C22 C25 1.507(16) . ? C23 C24 1.390(17) . ? C25 Eu1 2.828(10) 4_636 ? 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 O4 Eu1 O1 89.0(3) 4_655 3 ? O4 Eu1 O3 158.6(3) 4_655 . ? O1 Eu1 O3 104.9(3) 3 . ? O4 Eu1 O5 78.6(2) 4_655 1_564 ? O1 Eu1 O5 68.6(2) 3 1_564 ? O3 Eu1 O5 121.3(3) . 1_564 ? O4 Eu1 O2 109.5(3) 4_655 2_665 ? O1 Eu1 O2 133.3(4) 3 2_665 ? O3 Eu1 O2 72.7(3) . 2_665 ? O5 Eu1 O2 73.6(3) 1_564 2_665 ? O4 Eu1 O6 95.2(3) 4_655 4_666 ? O1 Eu1 O6 74.1(3) 3 4_666 ? O3 Eu1 O6 73.8(3) . 4_666 ? O5 Eu1 O6 142.2(3) 1_564 4_666 ? O2 Eu1 O6 141.4(3) 2_665 4_666 ? O4 Eu1 O5 74.0(3) 4_655 4_666 ? O1 Eu1 O5 121.1(2) 3 4_666 ? O3 Eu1 O5 84.9(3) . 4_666 ? O5 Eu1 O5 150.4(2) 1_564 4_666 ? O2 Eu1 O5 105.4(4) 2_665 4_666 ? O6 Eu1 O5 52.8(2) 4_666 4_666 ? O4 Eu1 O4 148.4(2) 4_655 . ? O1 Eu1 O4 71.6(2) 3 . ? O3 Eu1 O4 53.0(2) . . ? O5 Eu1 O4 71.2(2) 1_564 . ? O2 Eu1 O4 71.0(4) 2_665 . ? O6 Eu1 O4 102.8(3) 4_666 . ? O5 Eu1 O4 137.4(2) 4_666 . ? O4 Eu1 O1 71.5(3) 4_655 2_665 ? O1 Eu1 O1 157.88(7) 3 2_665 ? O3 Eu1 O1 96.8(3) . 2_665 ? O5 Eu1 O1 96.6(2) 1_564 2_665 ? O2 Eu1 O1 50.1(4) 2_665 2_665 ? O6 Eu1 O1 116.9(3) 4_666 2_665 ? O5 Eu1 O1 64.4(2) 4_666 2_665 ? O4 Eu1 O1 120.4(2) . 2_665 ? O4 Eu1 C25 84.1(3) 4_655 4_666 ? O1 Eu1 C25 97.2(3) 3 4_666 ? O3 Eu1 C25 78.2(3) . 4_666 ? O5 Eu1 C25 157.6(3) 1_564 4_666 ? O2 Eu1 C25 126.3(4) 2_665 4_666 ? O6 Eu1 C25 25.8(3) 4_666 4_666 ? O5 Eu1 C25 27.0(2) 4_666 4_666 ? O4 Eu1 C25 122.1(3) . 4_666 ? O1 Eu1 C25 91.3(3) 2_665 4_666 ? O4 Eu1 C29 174.6(3) 4_655 . ? O1 Eu1 C29 89.5(3) 3 . ? O3 Eu1 C29 26.3(3) . . ? O5 Eu1 C29 96.0(3) 1_564 . ? O2 Eu1 C29 68.0(4) 2_665 . ? O6 Eu1 C29 89.4(3) 4_666 . ? O5 Eu1 C29 111.2(3) 4_666 . ? O4 Eu1 C29 26.8(3) . . ? O1 Eu1 C29 108.9(3) 2_665 . ? C25 Eu1 C29 101.2(3) 4_666 . ? O4 Eu1 C18 90.7(3) 4_655 2_665 ? O1 Eu1 C18 151.4(3) 3 2_665 ? O3 Eu1 C18 84.7(3) . 2_665 ? O5 Eu1 C18 83.3(3) 1_564 2_665 ? O2 Eu1 C18 24.0(4) 2_665 2_665 ? O6 Eu1 C18 134.3(3) 4_666 2_665 ? O5 Eu1 C18 86.1(3) 4_666 2_665 ? O4 Eu1 C18 94.9(3) . 2_665 ? O1 Eu1 C18 26.1(3) 2_665 2_665 ? C25 Eu1 C18 111.2(3) 4_666 2_665 ? C29 Eu1 C18 88.1(3) . 2_665 ? C28 N1 C27 120(4) . . ? C28 N1 C26 112(3) . . ? C27 N1 C26 127(3) . . ? C18 O1 Eu1 171.1(7) . 3_445 ? C18 O1 Eu1 90.7(6) . 2_645 ? Eu1 O1 Eu1 95.2(2) 3_445 2_645 ? C18 O2 Eu1 100.4(8) . 2_645 ? C29 O3 Eu1 96.9(6) . . ? C29 O4 Eu1 166.6(7) . 4_645 ? C29 O4 Eu1 89.5(7) . . ? Eu1 O4 Eu1 97.5(2) 4_645 . ? C25 O5 Eu1 142.9(7) . 1_546 ? C25 O5 Eu1 92.0(6) . 4_636 ? Eu1 O5 Eu1 97.2(2) 1_546 4_636 ? C25 O6 Eu1 95.3(6) . 4_636 ? C6 O7 C4 116.5(9) . . ? C19 O8 C3 116.0(11) . . ? C12 O9 C5 118.0(9) . . ? C2 O10 C2 112.1(12) 2_656 . ? C3 C1 C2 112.0(8) . . ? C3 C1 C4 113.2(8) . . ? C2 C1 C4 105.0(9) . . ? C3 C1 C5 105.4(9) . . ? C2 C1 C5 109.2(8) . . ? C4 C1 C5 112.2(8) . . ? O10 C2 C1 109.7(9) . . ? O8 C3 C1 108.8(9) . . ? O7 C4 C1 108.9(9) . . ? O9 C5 C1 109.6(9) . . ? C11 C6 C7 119.9(12) . . ? C11 C6 O7 116.2(11) . . ? C7 C6 O7 123.8(12) . . ? C6 C7 C8 118.7(13) . . ? C9 C8 C7 122.7(14) . . ? C8 C9 C10 118.0(13) . . ? C8 C9 C29 120.6(13) . . ? C10 C9 C29 121.3(13) . . ? C9 C10 C11 119.3(15) . . ? C6 C11 C10 121.2(14) . . ? O9 C12 C17 122.8(10) . . ? O9 C12 C13 117.0(11) . . ? C17 C12 C13 120.2(9) . . ? C12 C13 C14 120.7(10) . . ? C15 C14 C13 119.5(10) . . ? C16 C15 C14 119.5(10) . . ? C16 C15 C18 118.5(10) . . ? C14 C15 C18 121.9(10) . . ? C15 C16 C17 120.9(11) . . ? C12 C17 C16 119.3(11) . . ? O2 C18 O1 118.7(9) . . ? O2 C18 C15 119.2(9) . . ? O1 C18 C15 122.1(10) . . ? O2 C18 Eu1 55.6(5) . 2_645 ? O1 C18 Eu1 63.2(5) . 2_645 ? C15 C18 Eu1 172.7(8) . 2_645 ? C20 C19 O8 127.0(17) . . ? C20 C19 C24 119.4(16) . . ? O8 C19 C24 113.6(15) . . ? C19 C20 C21 119.9(17) . . ? C22 C21 C20 120.7(14) . . ? C23 C22 C21 119.8(14) . . ? C23 C22 C25 121.0(12) . . ? C21 C22 C25 118.9(11) . . ? C22 C23 C24 119.8(14) . . ? C19 C24 C23 120.3(13) . . ? O6 C25 O5 119.9(9) . . ? O6 C25 C22 120.6(9) . . ? O5 C25 C22 119.6(10) . . ? O6 C25 Eu1 58.8(5) . 4_636 ? O5 C25 Eu1 61.1(5) . 4_636 ? C22 C25 Eu1 179.1(8) . 4_636 ? O11 C28 N1 123(3) . . ? O3 C29 O4 120.2(10) . . ? O3 C29 C9 119.4(10) . . ? O4 C29 C9 120.4(11) . . ? O3 C29 Eu1 56.8(5) . . ? O4 C29 Eu1 63.7(6) . . ? C9 C29 Eu1 171.1(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.290 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.229 data_TbL _database_code_depnum_ccdc_archive 'CCDC 891418' #TrackingRef '- LnL.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H54 N2 O21 Tb2' _chemical_formula_weight 1432.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 32.6663(15) _cell_length_b 7.0665(3) _cell_length_c 14.5262(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.3980(10) _cell_angle_gamma 90.00 _cell_volume 3247.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6393 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _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 9070 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.08 _reflns_number_total 6276 _reflns_number_gt 5696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0641P)^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 constr _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 0.021(17) _refine_ls_number_reflns 6276 _refine_ls_number_parameters 375 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.004 _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 Tb1 Tb 0.748658(7) 1.25638(8) 0.030483(15) 0.02523(9) Uani 1 1 d . . . N1 N 0.4472(4) 0.040(3) 0.9079(10) 0.139(6) Uani 1 1 d . . . O1 O 0.30311(15) 0.5355(8) 0.0409(3) 0.0380(11) Uani 1 1 d . . . O2 O 0.32670(13) 0.2526(15) 0.0345(3) 0.0511(11) Uani 1 1 d . . . O3 O 0.71679(19) 1.1905(7) 0.1567(4) 0.0509(15) Uani 1 1 d . . . O4 O 0.72078(15) 0.9446(7) 0.0665(3) 0.0345(11) Uani 1 1 d . . . O5 O 0.73613(14) 0.0703(7) 0.8894(3) 0.0301(10) Uani 1 1 d . . . O6 O 0.69865(17) -0.1713(7) 0.8247(4) 0.0435(13) Uani 1 1 d . . . O7 O 0.60379(17) 0.6124(8) 0.3179(4) 0.0446(13) Uani 1 1 d . . . O8 O 0.60913(17) 0.4810(7) 0.5445(3) 0.0446(12) Uani 1 1 d . . . O9 O 0.49384(16) 0.6265(8) 0.2800(4) 0.0492(14) Uani 1 1 d . . . O10 O 0.5000 0.5801(10) 0.5000 0.0418(17) Uani 1 2 d S . . O11 O 0.4728(4) 0.0752(18) 0.7836(9) 0.139(4) Uani 1 1 d . . . C1 C 0.55337(19) 0.5742(10) 0.4130(4) 0.0274(13) Uani 1 1 d . . . C2 C 0.5304(2) 0.6922(10) 0.4714(5) 0.0373(17) Uani 1 1 d . . . H2A H 0.5505 0.7416 0.5270 0.045 Uiso 1 1 calc R . . H2B H 0.5166 0.7985 0.4339 0.045 Uiso 1 1 calc R . . C3 C 0.5762(2) 0.4083(11) 0.4698(5) 0.0350(15) Uani 1 1 d . . . H3A H 0.5566 0.3348 0.4957 0.042 Uiso 1 1 calc R . . H3B H 0.5879 0.3266 0.4290 0.042 Uiso 1 1 calc R . . C4 C 0.5828(2) 0.7092(10) 0.3795(5) 0.0348(19) Uani 1 1 d . . . H4A H 0.5668 0.8147 0.3460 0.042 Uiso 1 1 calc R . . H4B H 0.6036 0.7589 0.4339 0.042 Uiso 1 1 calc R . . C5 C 0.5211(2) 0.4847(11) 0.3293(5) 0.0348(15) Uani 1 1 d . . . H5A H 0.5357 0.4239 0.2867 0.042 Uiso 1 1 calc R . . H5B H 0.5048 0.3892 0.3525 0.042 Uiso 1 1 calc R . . C6 C 0.6291(2) 0.7167(11) 0.2768(6) 0.042(2) Uani 1 1 d . . . C7 C 0.6376(3) 0.9060(14) 0.2970(7) 0.057(2) Uani 1 1 d . . . H7A H 0.6263 0.9689 0.3412 0.068 Uiso 1 1 calc R . . C8 C 0.6638(3) 1.0002(13) 0.2485(6) 0.052(2) Uani 1 1 d . . . H8A H 0.6696 1.1278 0.2611 0.063 Uiso 1 1 calc R . . C9 C 0.6812(2) 0.9116(12) 0.1836(5) 0.0388(17) Uani 1 1 d . . . C10 C 0.6734(3) 0.7165(14) 0.1678(6) 0.051(3) Uani 1 1 d . . . H10A H 0.6854 0.6516 0.1254 0.061 Uiso 1 1 calc R . . C11 C 0.6477(3) 0.6222(12) 0.2155(6) 0.051(2) Uani 1 1 d . . . H11A H 0.6431 0.4930 0.2058 0.061 Uiso 1 1 calc R . . C12 C 0.4557(2) 0.5691(11) 0.2238(5) 0.0361(16) Uani 1 1 d . . . C13 C 0.4264(2) 0.7107(10) 0.1928(5) 0.047(2) Uani 1 1 d . . . H13A H 0.4333 0.8361 0.2087 0.056 Uiso 1 1 calc R . . C14 C 0.3863(2) 0.6648(11) 0.1375(5) 0.0408(17) Uani 1 1 d . . . H14A H 0.3663 0.7594 0.1167 0.049 Uiso 1 1 calc R . . C15 C 0.3762(2) 0.4768(11) 0.1137(5) 0.0347(15) Uani 1 1 d . . . C16 C 0.4064(2) 0.3407(12) 0.1444(5) 0.0434(18) Uani 1 1 d . . . H16A H 0.3999 0.2151 0.1278 0.052 Uiso 1 1 calc R . . C17 C 0.4461(2) 0.3853(12) 0.1995(6) 0.0462(19) Uani 1 1 d . . . H17A H 0.4661 0.2907 0.2198 0.055 Uiso 1 1 calc R . . C18 C 0.3332(2) 0.4178(11) 0.0595(5) 0.0349(15) Uani 1 1 d . . . C19 C 0.6313(3) 0.3548(16) 0.6086(7) 0.040(2) Uani 1 1 d . . . C20 C 0.6234(3) 0.1641(16) 0.6102(8) 0.046(3) Uani 1 1 d . . . H20A H 0.6017 0.1113 0.5633 0.055 Uiso 1 1 calc R . . C21 C 0.6475(3) 0.0486(13) 0.6811(6) 0.045(2) Uani 1 1 d . . . H21A H 0.6407 -0.0788 0.6842 0.054 Uiso 1 1 calc R . . C22 C 0.6815(2) 0.1255(12) 0.7470(5) 0.0298(17) Uani 1 1 d . . . C23 C 0.6909(3) 0.3147(11) 0.7446(6) 0.037(2) Uani 1 1 d . . . H23A H 0.7141 0.3651 0.7883 0.045 Uiso 1 1 calc R . . C24 C 0.6653(3) 0.4305(11) 0.6761(6) 0.039(2) Uani 1 1 d . . . H24A H 0.6710 0.5593 0.6755 0.047 Uiso 1 1 calc R . . C25 C 0.7061(2) 0.0021(9) 0.8236(4) 0.0294(14) Uani 1 1 d . . . C26 C 0.4422(11) 0.263(5) 0.9077(19) 0.29(2) Uani 1 1 d . . . H26A H 0.4526 0.3162 0.8571 0.436 Uiso 1 1 calc R . . H26B H 0.4580 0.3133 0.9674 0.436 Uiso 1 1 calc R . . H26C H 0.4129 0.2950 0.8985 0.436 Uiso 1 1 calc R . . C27 C 0.4363(8) -0.087(5) 0.9693(13) 0.30(2) Uani 1 1 d . . . H27A H 0.4446 -0.2124 0.9554 0.443 Uiso 1 1 calc R . . H27B H 0.4063 -0.0840 0.9618 0.443 Uiso 1 1 calc R . . H27C H 0.4504 -0.0547 1.0335 0.443 Uiso 1 1 calc R . . C28 C 0.4637(6) -0.023(3) 0.8414(11) 0.129(7) Uani 1 1 d . . . H28A H 0.4687 -0.1525 0.8390 0.155 Uiso 1 1 calc R . . C29 C 0.7080(2) 1.0205(10) 0.1342(5) 0.0354(16) 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 0.02046(13) 0.02973(14) 0.02408(13) -0.0006(2) 0.00289(9) -0.0013(2) N1 0.106(10) 0.215(19) 0.092(9) -0.003(11) 0.018(8) -0.047(11) O1 0.023(2) 0.051(3) 0.035(3) -0.004(2) -0.002(2) 0.006(2) O2 0.027(2) 0.045(3) 0.073(3) -0.005(6) -0.0044(19) 0.001(5) O3 0.067(4) 0.049(3) 0.048(3) -0.009(2) 0.036(3) -0.018(3) O4 0.035(3) 0.037(3) 0.039(3) 0.001(2) 0.025(2) 0.005(2) O5 0.022(2) 0.042(3) 0.022(2) -0.0008(19) -0.0027(17) -0.0020(19) O6 0.043(3) 0.038(3) 0.037(3) 0.006(2) -0.013(2) -0.003(2) O7 0.048(3) 0.048(3) 0.050(3) 0.003(2) 0.035(3) -0.004(2) O8 0.043(3) 0.042(3) 0.036(3) 0.006(2) -0.014(2) -0.001(2) O9 0.028(3) 0.050(3) 0.057(3) 0.014(3) -0.015(2) -0.007(2) O10 0.034(4) 0.043(4) 0.059(4) 0.000 0.034(3) 0.000 O11 0.161(11) 0.133(9) 0.132(9) -0.015(8) 0.055(8) -0.060(9) C1 0.018(3) 0.041(4) 0.022(3) 0.008(3) 0.003(2) -0.001(3) C2 0.028(3) 0.046(4) 0.040(4) -0.001(3) 0.014(3) -0.005(3) C3 0.028(4) 0.048(4) 0.026(3) 0.001(3) 0.001(3) -0.002(3) C4 0.025(3) 0.049(6) 0.031(3) 0.006(3) 0.010(2) 0.002(3) C5 0.023(3) 0.049(4) 0.029(3) 0.011(3) 0.001(3) -0.001(3) C6 0.039(4) 0.046(8) 0.049(4) 0.010(4) 0.025(3) -0.003(3) C7 0.068(6) 0.060(6) 0.056(5) -0.004(5) 0.044(5) -0.005(5) C8 0.055(5) 0.047(5) 0.068(5) -0.009(4) 0.039(5) -0.012(4) C9 0.037(4) 0.048(5) 0.035(4) -0.005(3) 0.015(3) -0.010(4) C10 0.052(5) 0.059(9) 0.053(4) -0.004(4) 0.037(4) -0.002(4) C11 0.059(6) 0.031(4) 0.072(6) -0.005(4) 0.035(5) -0.004(4) C12 0.016(3) 0.047(4) 0.040(4) 0.008(3) -0.005(3) -0.004(3) C13 0.036(4) 0.039(6) 0.056(4) 0.003(3) -0.007(3) -0.005(3) C14 0.027(4) 0.045(4) 0.044(4) 0.012(3) -0.003(3) 0.006(3) C15 0.024(3) 0.047(4) 0.032(3) 0.005(3) 0.004(3) 0.003(3) C16 0.033(4) 0.041(4) 0.049(4) -0.001(3) -0.003(3) 0.005(3) C17 0.025(4) 0.052(5) 0.051(5) 0.000(4) -0.010(3) 0.007(3) C18 0.028(4) 0.045(4) 0.032(4) 0.005(3) 0.008(3) 0.001(3) C19 0.040(5) 0.041(5) 0.031(5) 0.003(4) -0.003(4) -0.001(4) C20 0.047(6) 0.038(5) 0.039(6) -0.001(4) -0.015(4) -0.009(4) C21 0.047(5) 0.039(4) 0.037(4) 0.007(3) -0.012(4) -0.009(4) C22 0.026(4) 0.042(5) 0.019(3) -0.004(3) -0.001(3) 0.002(3) C23 0.037(4) 0.038(5) 0.029(4) 0.002(3) -0.006(3) -0.001(3) C24 0.050(5) 0.023(4) 0.038(4) 0.004(3) 0.001(4) -0.002(4) C25 0.030(4) 0.035(4) 0.022(3) 0.002(3) 0.004(3) 0.002(3) C26 0.39(5) 0.22(3) 0.23(3) -0.08(3) 0.03(3) 0.18(3) C27 0.24(3) 0.51(6) 0.090(12) 0.09(2) -0.043(13) -0.25(3) C28 0.156(16) 0.163(16) 0.074(9) -0.026(10) 0.038(10) -0.080(13) C29 0.033(4) 0.042(4) 0.033(3) 0.005(3) 0.011(3) 0.004(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 Tb1 O4 2.334(4) 4_655 ? Tb1 O1 2.343(5) 3 ? Tb1 O3 2.369(5) . ? Tb1 O5 2.383(4) 1_564 ? Tb1 O2 2.408(4) 2_665 ? Tb1 O6 2.419(5) 4_666 ? Tb1 O4 2.489(5) . ? Tb1 O5 2.497(5) 4_666 ? Tb1 O1 2.637(5) 2_665 ? Tb1 C29 2.793(7) . ? Tb1 C25 2.851(6) 4_666 ? Tb1 C18 2.901(7) 2_665 ? N1 C28 1.30(2) . ? N1 C27 1.37(2) . ? N1 C26 1.59(4) . ? O1 C18 1.263(8) . ? O1 Tb1 2.343(5) 3_445 ? O1 Tb1 2.637(5) 2_645 ? O2 C18 1.225(12) . ? O2 Tb1 2.408(4) 2_645 ? O3 C29 1.259(9) . ? O4 C29 1.277(8) . ? O4 Tb1 2.334(4) 4_645 ? O5 C25 1.280(8) . ? O5 Tb1 2.383(4) 1_546 ? O5 Tb1 2.497(5) 4_636 ? O6 C25 1.251(8) . ? O6 Tb1 2.419(5) 4_636 ? O7 C6 1.352(8) . ? O7 C4 1.430(8) . ? O8 C19 1.360(11) . ? O8 C3 1.421(8) . ? O9 C12 1.370(8) . ? O9 C5 1.412(9) . ? O10 C2 1.411(7) 2_656 ? O10 C2 1.411(7) . ? O11 C28 1.184(17) . ? C1 C2 1.515(9) . ? C1 C3 1.518(9) . ? C1 C4 1.518(9) . ? C1 C5 1.534(9) . ? C6 C11 1.371(11) . ? C6 C7 1.383(14) . ? C7 C8 1.405(11) . ? C8 C9 1.366(11) . ? C9 C10 1.410(14) . ? C9 C29 1.481(10) . ? C10 C11 1.383(11) . ? C12 C17 1.362(11) . ? C12 C13 1.381(10) . ? C13 C14 1.393(10) . ? C14 C15 1.391(11) . ? C15 C16 1.370(10) . ? C15 C18 1.489(10) . ? C16 C17 1.381(10) . ? C18 Tb1 2.901(7) 2_645 ? C19 C20 1.374(10) . ? C19 C24 1.394(13) . ? C20 C21 1.394(13) . ? C21 C22 1.385(11) . ? C22 C23 1.374(12) . ? C22 C25 1.484(10) . ? C23 C24 1.394(11) . ? C25 Tb1 2.851(6) 4_636 ? 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 O4 Tb1 O1 89.25(18) 4_655 3 ? O4 Tb1 O3 156.24(17) 4_655 . ? O1 Tb1 O3 106.96(19) 3 . ? O4 Tb1 O5 78.65(15) 4_655 1_564 ? O1 Tb1 O5 69.72(16) 3 1_564 ? O3 Tb1 O5 122.86(17) . 1_564 ? O4 Tb1 O2 108.6(2) 4_655 2_665 ? O1 Tb1 O2 134.7(3) 3 2_665 ? O3 Tb1 O2 72.42(19) . 2_665 ? O5 Tb1 O2 73.5(2) 1_564 2_665 ? O4 Tb1 O6 94.94(18) 4_655 4_666 ? O1 Tb1 O6 73.73(17) 3 4_666 ? O3 Tb1 O6 73.9(2) . 4_666 ? O5 Tb1 O6 142.90(17) 1_564 4_666 ? O2 Tb1 O6 141.3(2) 2_665 4_666 ? O4 Tb1 O4 149.87(14) 4_655 . ? O1 Tb1 O4 73.03(16) 3 . ? O3 Tb1 O4 53.78(15) . . ? O5 Tb1 O4 72.46(15) 1_564 . ? O2 Tb1 O4 71.4(3) 2_665 . ? O6 Tb1 O4 102.86(17) 4_666 . ? O4 Tb1 O5 73.11(16) 4_655 4_666 ? O1 Tb1 O5 120.12(15) 3 4_666 ? O3 Tb1 O5 83.62(16) . 4_666 ? O5 Tb1 O5 149.61(15) 1_564 4_666 ? O2 Tb1 O5 105.0(3) 2_665 4_666 ? O6 Tb1 O5 52.48(15) 4_666 4_666 ? O4 Tb1 O5 136.84(14) . 4_666 ? O4 Tb1 O1 70.44(16) 4_655 2_665 ? O1 Tb1 O1 157.83(6) 3 2_665 ? O3 Tb1 O1 95.11(18) . 2_665 ? O5 Tb1 O1 96.79(15) 1_564 2_665 ? O2 Tb1 O1 50.3(3) 2_665 2_665 ? O6 Tb1 O1 115.62(16) 4_666 2_665 ? O4 Tb1 O1 120.82(15) . 2_665 ? O5 Tb1 O1 63.42(14) 4_666 2_665 ? O4 Tb1 C29 175.71(19) 4_655 . ? O1 Tb1 C29 91.27(19) 3 . ? O3 Tb1 C29 26.65(19) . . ? O5 Tb1 C29 97.54(18) 1_564 . ? O2 Tb1 C29 68.2(2) 2_665 . ? O6 Tb1 C29 89.3(2) 4_666 . ? O4 Tb1 C29 27.20(17) . . ? O5 Tb1 C29 110.20(18) 4_666 . ? O1 Tb1 C29 108.32(18) 2_665 . ? O4 Tb1 C25 83.18(17) 4_655 4_666 ? O1 Tb1 C25 96.50(18) 3 4_666 ? O3 Tb1 C25 77.91(18) . 4_666 ? O5 Tb1 C25 157.16(17) 1_564 4_666 ? O2 Tb1 C25 126.0(2) 2_665 4_666 ? O6 Tb1 C25 25.82(18) 4_666 4_666 ? O4 Tb1 C25 122.14(17) . 4_666 ? O5 Tb1 C25 26.66(16) 4_666 4_666 ? O1 Tb1 C25 89.99(17) 2_665 4_666 ? C29 Tb1 C25 101.0(2) . 4_666 ? O4 Tb1 C18 89.33(19) 4_655 2_665 ? O1 Tb1 C18 152.95(18) 3 2_665 ? O3 Tb1 C18 83.9(2) . 2_665 ? O5 Tb1 C18 83.53(17) 1_564 2_665 ? O2 Tb1 C18 24.5(3) 2_665 2_665 ? O6 Tb1 C18 133.29(18) 4_666 2_665 ? O4 Tb1 C18 95.65(18) . 2_665 ? O5 Tb1 C18 85.12(17) 4_666 2_665 ? O1 Tb1 C18 25.81(17) 2_665 2_665 ? C29 Tb1 C18 88.3(2) . 2_665 ? C25 Tb1 C18 110.1(2) 4_666 2_665 ? C28 N1 C27 119(3) . . ? C28 N1 C26 113.8(19) . . ? C27 N1 C26 127(2) . . ? C18 O1 Tb1 171.6(4) . 3_445 ? C18 O1 Tb1 88.9(4) . 2_645 ? Tb1 O1 Tb1 94.04(16) 3_445 2_645 ? C18 O2 Tb1 100.9(5) . 2_645 ? C29 O3 Tb1 95.8(4) . . ? C29 O4 Tb1 166.9(5) . 4_645 ? C29 O4 Tb1 89.8(4) . . ? Tb1 O4 Tb1 98.26(15) 4_645 . ? C25 O5 Tb1 141.8(4) . 1_546 ? C25 O5 Tb1 92.3(4) . 4_636 ? Tb1 O5 Tb1 96.77(14) 1_546 4_636 ? C25 O6 Tb1 96.8(4) . 4_636 ? C6 O7 C4 117.2(6) . . ? C19 O8 C3 117.3(7) . . ? C12 O9 C5 117.2(6) . . ? C2 O10 C2 111.7(7) 2_656 . ? C2 C1 C3 111.4(5) . . ? C2 C1 C4 106.0(5) . . ? C3 C1 C4 113.2(5) . . ? C2 C1 C5 109.5(5) . . ? C3 C1 C5 105.1(6) . . ? C4 C1 C5 111.7(5) . . ? O10 C2 C1 109.8(6) . . ? O8 C3 C1 108.2(6) . . ? O7 C4 C1 109.9(5) . . ? O9 C5 C1 109.4(6) . . ? O7 C6 C11 116.1(7) . . ? O7 C6 C7 123.1(7) . . ? C11 C6 C7 120.7(7) . . ? C6 C7 C8 117.9(8) . . ? C9 C8 C7 122.5(8) . . ? C8 C9 C10 118.1(7) . . ? C8 C9 C29 119.6(8) . . ? C10 C9 C29 122.3(7) . . ? C11 C10 C9 119.8(8) . . ? C6 C11 C10 120.8(8) . . ? C17 C12 O9 123.6(6) . . ? C17 C12 C13 120.6(6) . . ? O9 C12 C13 115.8(7) . . ? C12 C13 C14 119.8(7) . . ? C15 C14 C13 119.7(7) . . ? C16 C15 C14 118.8(7) . . ? C16 C15 C18 118.9(7) . . ? C14 C15 C18 122.2(6) . . ? C15 C16 C17 121.7(8) . . ? C12 C17 C16 119.4(7) . . ? O2 C18 O1 119.7(6) . . ? O2 C18 C15 119.6(6) . . ? O1 C18 C15 120.7(7) . . ? O2 C18 Tb1 54.6(3) . 2_645 ? O1 C18 Tb1 65.3(4) . 2_645 ? C15 C18 Tb1 172.2(5) . 2_645 ? O8 C19 C20 125.8(11) . . ? O8 C19 C24 115.2(9) . . ? C20 C19 C24 119.0(11) . . ? C19 C20 C21 120.9(11) . . ? C22 C21 C20 119.3(9) . . ? C23 C22 C21 120.7(9) . . ? C23 C22 C25 120.6(8) . . ? C21 C22 C25 118.7(7) . . ? C22 C23 C24 119.5(9) . . ? C23 C24 C19 120.6(8) . . ? O6 C25 O5 118.4(6) . . ? O6 C25 C22 120.9(6) . . ? O5 C25 C22 120.7(6) . . ? O6 C25 Tb1 57.4(3) . 4_636 ? O5 C25 Tb1 61.1(3) . 4_636 ? C22 C25 Tb1 178.2(5) . 4_636 ? O11 C28 N1 123(2) . . ? O3 C29 O4 120.3(6) . . ? O3 C29 C9 119.5(6) . . ? O4 C29 C9 120.1(7) . . ? O3 C29 Tb1 57.5(3) . . ? O4 C29 Tb1 63.0(3) . . ? C9 C29 Tb1 172.0(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.352 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.178