Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ana de Bettencourt-Dias' _publ_contact_author_address ; Department of Chemistry Syracuse University Syracuse NY 13244-4100 UNITED STATES OF AMERICA ; _publ_contact_author_email DEBETTEN@SYR.EDU _publ_section_title ; Nitro-functionalization and quantum yield of Eu(III) and Tb(III) benzoic acid complexes ; loop_ _publ_author_name 'A.de Bettencourt-Dias' 'Subha Viswanathan' data_pbar111102005a _database_code_depnum_ccdc_archive 'CCDC 603285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Europium 3-Nitrobenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H23 Eu N3 O15' _chemical_formula_weight 745.41 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7100(19) _cell_length_b 10.579(2) _cell_length_c 13.361(3) _cell_angle_alpha 77.41(3) _cell_angle_beta 88.78(3) _cell_angle_gamma 88.16(3) _cell_volume 1338.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 99(2) _cell_measurement_reflns_used 7177 _cell_measurement_theta_min 2.598 _cell_measurement_theta_max 28.2415 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 2.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4437 _exptl_absorpt_correction_T_max 0.8296 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 99(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 CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 14194 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6584 _reflns_number_gt 6137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0407P)^2^+1.7318P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6584 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 C1 C -0.0051(3) 1.3196(3) 0.5978(2) 0.0130(5) Uani 1 1 d . . . C2 C -0.1278(3) 1.3451(3) 0.6468(2) 0.0146(6) Uani 1 1 d . . . H2A H -0.2029 1.2884 0.6533 0.018 Uiso 1 1 calc R . . C3 C -0.1361(3) 1.4565(3) 0.6857(2) 0.0161(6) Uani 1 1 d . . . C4 C -0.0299(3) 1.5431(3) 0.6772(2) 0.0180(6) Uani 1 1 d . . . H4 H -0.0401 1.6193 0.7038 0.022 Uiso 1 1 calc R . . C5 C 0.0909(3) 1.5153(3) 0.6290(3) 0.0186(6) Uani 1 1 d . . . H5 H 0.1652 1.5730 0.6219 0.022 Uiso 1 1 calc R . . C6 C 0.1043(3) 1.4028(3) 0.5906(2) 0.0164(6) Uani 1 1 d . . . H6 H 0.1887 1.3830 0.5594 0.020 Uiso 1 1 calc R . . C7 C 0.0081(3) 1.2024(3) 0.5512(2) 0.0135(5) Uani 1 1 d . . . C8 C 0.5703(3) 0.8742(3) 0.2544(2) 0.0140(6) Uani 1 1 d . . . C9 C 0.4893(3) 0.8660(3) 0.1719(2) 0.0156(6) Uani 1 1 d . . . H9 H 0.3924 0.8812 0.1739 0.019 Uiso 1 1 calc R . . C10 C 0.5534(3) 0.8352(3) 0.0864(2) 0.0176(6) Uani 1 1 d . . . C11 C 0.6939(4) 0.8104(3) 0.0803(3) 0.0223(7) Uani 1 1 d . . . H11A H 0.7345 0.7884 0.0208 0.027 Uiso 1 1 calc R . . C12 C 0.7735(3) 0.8184(4) 0.1629(3) 0.0238(7) Uani 1 1 d . . . H12 H 0.8700 0.8010 0.1609 0.029 Uiso 1 1 calc R . . C13 C 0.7127(3) 0.8518(3) 0.2492(3) 0.0196(6) Uani 1 1 d . . . H13 H 0.7684 0.8595 0.3050 0.024 Uiso 1 1 calc R . . C14 C 0.5040(3) 0.9058(3) 0.3484(2) 0.0136(6) Uani 1 1 d . . . C15 C 0.2662(3) 0.7160(3) 0.7642(2) 0.0139(6) Uani 1 1 d . . . C16 C 0.3649(3) 0.6146(3) 0.7773(2) 0.0170(6) Uani 1 1 d . . . H16 H 0.4268 0.6074 0.7227 0.020 Uiso 1 1 calc R . . C17 C 0.3724(4) 0.5244(3) 0.8699(3) 0.0228(7) Uani 1 1 d . . . H17 H 0.4415 0.4574 0.8791 0.027 Uiso 1 1 calc R . . C18 C 0.2796(3) 0.5317(3) 0.9492(3) 0.0226(7) Uani 1 1 d . . . H18 H 0.2825 0.4694 1.0122 0.027 Uiso 1 1 calc R . . C19 C 0.1826(3) 0.6328(4) 0.9334(2) 0.0212(7) Uani 1 1 d . . . C20 C 0.1751(3) 0.7260(3) 0.8439(2) 0.0181(6) Uani 1 1 d . . . H20 H 0.1092 0.7956 0.8368 0.022 Uiso 1 1 calc R . . C21 C 0.2576(3) 0.8148(3) 0.6647(2) 0.0141(6) Uani 1 1 d . . . C22 C 0.1653(3) 1.1092(3) 0.2135(2) 0.0195(6) Uani 1 1 d . . . H22A H 0.2671 1.1046 0.2076 0.023 Uiso 1 1 calc R . . H22B H 0.1329 1.1921 0.1694 0.023 Uiso 1 1 calc R . . C23 C 0.1066(4) 0.9989(3) 0.1755(3) 0.0249(7) Uani 1 1 d . . . H23A H 0.1391 0.9165 0.2185 0.037 Uiso 1 1 calc R . . H23B H 0.1367 1.0036 0.1044 0.037 Uiso 1 1 calc R . . H23C H 0.0058 1.0047 0.1790 0.037 Uiso 1 1 calc R . . C24 C 0.4035(5) 0.3921(6) 0.4643(4) 0.0530(13) Uani 1 1 d . . . H24A H 0.3114 0.4115 0.4893 0.080 Uiso 1 1 calc R . . H24B H 0.4140 0.2989 0.4675 0.080 Uiso 1 1 calc R . . H24C H 0.4156 0.4396 0.3931 0.080 Uiso 1 1 calc R . . Eu1 Eu 0.258433(13) 1.006394(13) 0.476627(11) 0.01061(5) Uani 1 1 d . . . N1 N -0.2624(3) 1.4821(3) 0.7407(2) 0.0211(6) Uani 1 1 d . . . N2 N 0.4670(3) 0.8267(3) -0.0012(2) 0.0253(6) Uani 1 1 d . . . N3 N 0.0819(3) 0.6414(4) 1.0151(2) 0.0309(7) Uani 1 1 d . . . O1 O 0.1251(2) 1.1741(2) 0.51992(18) 0.0188(5) Uani 1 1 d . . . O2 O -0.2805(3) 1.5899(2) 0.76102(19) 0.0238(5) Uani 1 1 d . . . O3 O -0.3441(3) 1.3960(3) 0.7655(3) 0.0429(8) Uani 1 1 d . . . O4 O 0.3744(2) 0.9088(2) 0.35351(17) 0.0178(4) Uani 1 1 d . . . O6 O 0.3453(3) 0.8578(3) 0.0019(2) 0.0349(6) Uani 1 1 d . . . O7 O 0.5223(3) 0.7877(3) -0.0728(2) 0.0413(7) Uani 1 1 d . . . O8 O 0.3445(2) 0.8077(2) 0.59420(16) 0.0147(4) Uani 1 1 d . . . O9 O 0.1635(2) 0.9019(2) 0.65292(16) 0.0151(4) Uani 1 1 d . . . O10 O 0.0085(3) 0.7400(4) 1.0048(2) 0.0476(9) Uani 1 1 d . . . O11 O 0.0747(3) 0.5483(3) 1.0888(2) 0.0409(8) Uani 1 1 d . . . O12 O 0.3836(2) 1.1825(2) 0.3728(2) 0.0247(5) Uani 1 1 d . . . O13 O 0.0979(2) 0.8599(2) 0.45267(18) 0.0193(5) Uani 1 1 d . . . O14 O 0.4214(2) 1.0708(2) 0.58229(18) 0.0194(5) Uani 1 1 d . . . O15 O 0.1264(2) 1.1077(2) 0.31850(17) 0.0183(5) Uani 1 1 d . . . O17 O 0.4988(6) 0.4282(5) 0.5229(4) 0.0835(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0120(13) 0.0126(13) 0.0144(13) -0.0030(11) -0.0008(11) 0.0004(10) C2 0.0140(14) 0.0129(14) 0.0163(14) -0.0023(11) 0.0003(11) 0.0015(11) C3 0.0173(15) 0.0155(14) 0.0147(14) -0.0027(11) 0.0029(11) 0.0037(11) C4 0.0269(17) 0.0128(14) 0.0145(14) -0.0035(11) -0.0010(12) -0.0016(12) C5 0.0193(15) 0.0176(15) 0.0212(15) -0.0081(13) 0.0006(12) -0.0062(12) C6 0.0137(14) 0.0189(15) 0.0175(14) -0.0060(12) -0.0008(11) 0.0001(11) C7 0.0149(14) 0.0120(13) 0.0131(13) -0.0016(11) -0.0017(11) 0.0000(11) C8 0.0138(14) 0.0123(13) 0.0169(14) -0.0054(11) 0.0025(11) 0.0004(10) C9 0.0152(14) 0.0141(14) 0.0177(14) -0.0039(11) 0.0011(11) -0.0012(11) C10 0.0219(16) 0.0169(15) 0.0151(14) -0.0059(12) 0.0009(12) -0.0019(12) C11 0.0239(17) 0.0243(17) 0.0211(16) -0.0106(14) 0.0088(13) -0.0030(13) C12 0.0142(15) 0.0304(19) 0.0303(18) -0.0149(15) 0.0071(13) 0.0006(13) C13 0.0141(14) 0.0252(17) 0.0223(16) -0.0119(13) 0.0011(12) 0.0016(12) C14 0.0134(13) 0.0124(13) 0.0157(14) -0.0048(11) 0.0024(11) -0.0003(10) C15 0.0111(13) 0.0171(14) 0.0143(13) -0.0048(11) 0.0003(11) -0.0010(11) C16 0.0145(14) 0.0162(15) 0.0206(15) -0.0050(12) 0.0029(12) -0.0006(11) C17 0.0216(16) 0.0187(16) 0.0255(17) 0.0000(13) 0.0020(13) 0.0041(13) C18 0.0199(16) 0.0253(17) 0.0182(15) 0.0045(13) -0.0002(13) 0.0005(13) C19 0.0146(15) 0.0337(19) 0.0146(14) -0.0041(13) 0.0016(12) 0.0020(13) C20 0.0136(14) 0.0253(16) 0.0153(14) -0.0047(13) 0.0002(11) 0.0038(12) C21 0.0111(13) 0.0162(14) 0.0167(14) -0.0071(12) 0.0004(11) -0.0017(11) C22 0.0159(15) 0.0255(17) 0.0155(14) -0.0019(13) 0.0016(12) 0.0023(12) C23 0.0254(17) 0.0246(18) 0.0245(17) -0.0057(14) -0.0001(14) 0.0049(14) C24 0.048(3) 0.054(3) 0.060(3) -0.017(3) 0.004(2) -0.010(2) Eu1 0.00770(8) 0.01121(8) 0.01335(8) -0.00378(5) 0.00177(5) -0.00016(5) N1 0.0224(14) 0.0210(14) 0.0202(13) -0.0064(11) 0.0048(11) 0.0053(11) N2 0.0323(17) 0.0283(16) 0.0178(14) -0.0100(12) -0.0028(12) -0.0010(13) N3 0.0205(15) 0.055(2) 0.0135(13) 0.0008(14) 0.0015(11) 0.0067(14) O1 0.0139(10) 0.0179(11) 0.0262(12) -0.0090(9) 0.0028(9) 0.0025(8) O2 0.0323(13) 0.0173(11) 0.0216(12) -0.0054(9) 0.0009(10) 0.0113(10) O3 0.0335(15) 0.0349(16) 0.066(2) -0.0260(15) 0.0309(15) -0.0102(13) O4 0.0106(10) 0.0246(12) 0.0189(11) -0.0070(9) 0.0022(8) 0.0024(8) O6 0.0309(15) 0.0479(18) 0.0298(14) -0.0173(13) -0.0108(12) 0.0077(13) O7 0.0441(17) 0.062(2) 0.0261(14) -0.0274(15) 0.0012(13) -0.0029(15) O8 0.0122(10) 0.0168(10) 0.0150(10) -0.0036(8) 0.0036(8) 0.0015(8) O9 0.0119(10) 0.0179(11) 0.0152(10) -0.0034(8) 0.0024(8) 0.0023(8) O10 0.0382(17) 0.073(2) 0.0248(14) -0.0017(15) 0.0098(12) 0.0298(16) O11 0.0300(15) 0.068(2) 0.0165(13) 0.0084(13) 0.0033(11) 0.0055(14) O12 0.0118(11) 0.0222(12) 0.0338(14) 0.0078(10) -0.0017(10) -0.0025(9) O13 0.0152(11) 0.0199(11) 0.0251(12) -0.0097(10) 0.0006(9) -0.0051(9) O14 0.0149(10) 0.0280(13) 0.0188(11) -0.0123(10) 0.0019(9) -0.0029(9) O15 0.0117(10) 0.0267(12) 0.0157(11) -0.0036(9) 0.0004(8) 0.0022(9) O17 0.098(4) 0.071(3) 0.089(4) -0.033(3) -0.006(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.390(4) . ? C1 C2 1.394(4) . ? C1 C7 1.504(4) . ? C2 C3 1.387(4) . ? C2 H2A 0.9500 . ? C3 C4 1.388(4) . ? C3 N1 1.465(4) . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O13 1.249(4) 2_576 ? C7 O1 1.252(4) . ? C8 C9 1.388(4) . ? C8 C13 1.397(4) . ? C8 C14 1.496(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 N2 1.475(4) . ? C11 C12 1.379(5) . ? C11 H11A 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O4 1.258(4) . ? C14 O14 1.259(4) 2_676 ? C15 C20 1.390(4) . ? C15 C16 1.399(4) . ? C15 C21 1.504(4) . ? C16 C17 1.390(5) . ? C16 H16 0.9500 . ? C17 C18 1.390(5) . ? C17 H17 0.9500 . ? C18 C19 1.386(5) . ? C18 H18 0.9500 . ? C19 C20 1.375(5) . ? C19 N3 1.466(4) . ? C20 H20 0.9500 . ? C21 O9 1.264(4) . ? C21 O8 1.264(4) . ? C22 O15 1.442(4) . ? C22 C23 1.502(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O17 1.341(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Eu1 O13 2.307(2) . ? Eu1 O1 2.329(2) . ? Eu1 O14 2.355(2) . ? Eu1 O4 2.372(2) . ? Eu1 O12 2.412(2) . ? Eu1 O8 2.468(2) . ? Eu1 O15 2.509(2) . ? Eu1 O9 2.541(2) . ? N1 O3 1.213(4) . ? N1 O2 1.235(4) . ? N2 O6 1.218(4) . ? N2 O7 1.228(4) . ? N3 O10 1.228(5) . ? N3 O11 1.234(4) . ? O13 C7 1.249(4) 2_576 ? O14 C14 1.259(4) 2_676 ? O17 O17 1.509(10) 2_666 ? 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 C6 C1 C2 120.3(3) . . ? C6 C1 C7 119.9(3) . . ? C2 C1 C7 119.8(3) . . ? C3 C2 C1 117.5(3) . . ? C3 C2 H2A 121.2 . . ? C1 C2 H2A 121.2 . . ? C2 C3 C4 123.4(3) . . ? C2 C3 N1 118.1(3) . . ? C4 C3 N1 118.4(3) . . ? C5 C4 C3 118.0(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O13 C7 O1 124.8(3) 2_576 . ? O13 C7 C1 117.7(3) 2_576 . ? O1 C7 C1 117.5(3) . . ? C9 C8 C13 119.7(3) . . ? C9 C8 C14 119.5(3) . . ? C13 C8 C14 120.8(3) . . ? C10 C9 C8 118.2(3) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 123.0(3) . . ? C9 C10 N2 118.1(3) . . ? C11 C10 N2 118.9(3) . . ? C12 C11 C10 118.3(3) . . ? C12 C11 H11A 120.9 . . ? C10 C11 H11A 120.9 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.6(3) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? O4 C14 O14 123.0(3) . 2_676 ? O4 C14 C8 117.6(3) . . ? O14 C14 C8 119.4(3) 2_676 . ? C20 C15 C16 119.8(3) . . ? C20 C15 C21 119.4(3) . . ? C16 C15 C21 120.8(3) . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 117.9(3) . . ? C19 C18 H18 121.1 . . ? C17 C18 H18 121.1 . . ? C20 C19 C18 123.2(3) . . ? C20 C19 N3 117.8(3) . . ? C18 C19 N3 119.0(3) . . ? C19 C20 C15 118.4(3) . . ? C19 C20 H20 120.8 . . ? C15 C20 H20 120.8 . . ? O9 C21 O8 121.6(3) . . ? O9 C21 C15 119.6(3) . . ? O8 C21 C15 118.8(3) . . ? O15 C22 C23 112.6(3) . . ? O15 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? O15 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O17 C24 H24A 109.5 . . ? O17 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O17 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O13 Eu1 O1 103.67(8) . . ? O13 Eu1 O14 149.22(9) . . ? O1 Eu1 O14 83.20(8) . . ? O13 Eu1 O4 79.05(8) . . ? O1 Eu1 O4 151.18(8) . . ? O14 Eu1 O4 109.37(8) . . ? O13 Eu1 O12 137.65(9) . . ? O1 Eu1 O12 83.13(9) . . ? O14 Eu1 O12 72.47(9) . . ? O4 Eu1 O12 76.62(9) . . ? O13 Eu1 O8 79.11(8) . . ? O1 Eu1 O8 126.99(8) . . ? O14 Eu1 O8 73.16(8) . . ? O4 Eu1 O8 81.82(8) . . ? O12 Eu1 O8 129.97(8) . . ? O13 Eu1 O15 72.50(8) . . ? O1 Eu1 O15 74.30(8) . . ? O14 Eu1 O15 137.39(8) . . ? O4 Eu1 O15 79.43(8) . . ? O12 Eu1 O15 69.32(8) . . ? O8 Eu1 O15 148.39(8) . . ? O13 Eu1 O9 73.09(8) . . ? O1 Eu1 O9 77.47(8) . . ? O14 Eu1 O9 79.42(8) . . ? O4 Eu1 O9 129.41(8) . . ? O12 Eu1 O9 147.44(9) . . ? O8 Eu1 O9 52.24(7) . . ? O15 Eu1 O9 128.05(7) . . ? O3 N1 O2 122.8(3) . . ? O3 N1 C3 118.6(3) . . ? O2 N1 C3 118.6(3) . . ? O6 N2 O7 124.0(3) . . ? O6 N2 C10 118.3(3) . . ? O7 N2 C10 117.7(3) . . ? O10 N3 O11 124.3(3) . . ? O10 N3 C19 117.7(3) . . ? O11 N3 C19 117.9(3) . . ? C7 O1 Eu1 143.4(2) . . ? C14 O4 Eu1 120.2(2) . . ? C21 O8 Eu1 94.74(18) . . ? C21 O9 Eu1 91.32(18) . . ? C7 O13 Eu1 166.4(2) 2_576 . ? C14 O14 Eu1 169.9(2) 2_676 . ? C22 O15 Eu1 127.37(18) . . ? C24 O17 O17 100.4(6) . 2_666 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.130 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.138 # Attachment 'CCDC603286.cif' data_pbar1-dec192005a _database_code_depnum_ccdc_archive 'CCDC 603286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Europium 4-Nitrobenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Eu2 N6 O29' _chemical_formula_weight 1390.67 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2242(18) _cell_length_b 15.102(3) _cell_length_c 18.587(4) _cell_angle_alpha 75.93(3) _cell_angle_beta 82.88(3) _cell_angle_gamma 79.00(3) _cell_volume 2457.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 97(2) _cell_measurement_reflns_used 9793 _cell_measurement_theta_min 2.4835 _cell_measurement_theta_max 28.3140 _exptl_crystal_description needles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 2.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4188 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 97(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 CCD detector' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 25551 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11169 _reflns_number_gt 9434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0350P)^2^+3.9202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11169 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 C1 C -0.5702(4) 0.9572(3) 0.6899(2) 0.0113(8) Uani 1 1 d . . . C2 C -0.6368(4) 1.0454(3) 0.7136(2) 0.0113(8) Uani 1 1 d . . . C3 C -0.7591(5) 1.1023(3) 0.6813(3) 0.0171(9) Uani 1 1 d . . . H3 H -0.8001 1.0863 0.6427 0.021 Uiso 1 1 calc R . . C4 C -0.8224(5) 1.1829(3) 0.7052(3) 0.0204(10) Uani 1 1 d . . . H4 H -0.9036 1.2237 0.6818 0.024 Uiso 1 1 calc R . . C5 C -0.7638(5) 1.2017(3) 0.7636(3) 0.0202(10) Uani 1 1 d . . . C6 C -0.6439(5) 1.1458(3) 0.7983(3) 0.0191(10) Uani 1 1 d . . . H6 H -0.6071 1.1605 0.8387 0.023 Uiso 1 1 calc R . . C7 C -0.5790(5) 1.0677(3) 0.7723(2) 0.0146(9) Uani 1 1 d . . . H7 H -0.4948 1.0289 0.7943 0.018 Uiso 1 1 calc R . . C8 C -0.0417(4) 0.9612(3) 0.6206(2) 0.0106(8) Uani 1 1 d . . . C9 C -0.1222(4) 1.0585(3) 0.6178(2) 0.0128(8) Uani 1 1 d . . . C10 C -0.2273(5) 1.0746(3) 0.6753(3) 0.0217(10) Uani 1 1 d . . . H10 H -0.2533 1.0241 0.7133 0.026 Uiso 1 1 calc R . . C11 C -0.2943(5) 1.1643(3) 0.6775(3) 0.0231(10) Uani 1 1 d . . . H11 H -0.3654 1.1761 0.7171 0.028 Uiso 1 1 calc R . . C12 C -0.2559(5) 1.2359(3) 0.6212(3) 0.0184(9) Uani 1 1 d . . . C13 C -0.1528(5) 1.2217(3) 0.5629(3) 0.0198(10) Uani 1 1 d . . . H13 H -0.1293 1.2722 0.5243 0.024 Uiso 1 1 calc R . . C14 C -0.0849(5) 1.1321(3) 0.5622(3) 0.0189(9) Uani 1 1 d . . . H14 H -0.0118 1.1208 0.5232 0.023 Uiso 1 1 calc R . . C15 C 0.1653(5) 0.8954(3) 0.8142(2) 0.0136(9) Uani 1 1 d . . . C16 C 0.1662(4) 0.9479(3) 0.8727(2) 0.0131(8) Uani 1 1 d . . . C17 C 0.0616(5) 1.0277(3) 0.8745(2) 0.0144(9) Uani 1 1 d . . . H17 H -0.0149 1.0451 0.8415 0.017 Uiso 1 1 calc R . . C18 C 0.0687(5) 1.0816(3) 0.9240(2) 0.0164(9) Uani 1 1 d . . . H18 H -0.0031 1.1352 0.9265 0.020 Uiso 1 1 calc R . . C19 C 0.1841(5) 1.0547(3) 0.9698(2) 0.0145(9) Uani 1 1 d . . . C20 C 0.2880(5) 0.9754(3) 0.9711(3) 0.0185(9) Uani 1 1 d . . . H20 H 0.3640 0.9585 1.0044 0.022 Uiso 1 1 calc R . . C21 C 0.2775(5) 0.9211(3) 0.9222(2) 0.0163(9) Uani 1 1 d . . . H21 H 0.3462 0.8656 0.9222 0.020 Uiso 1 1 calc R . . C22 C 0.4739(5) 0.6445(3) 0.7318(2) 0.0127(8) Uani 1 1 d . . . C23 C 0.5292(5) 0.5439(3) 0.7637(2) 0.0135(8) Uani 1 1 d . . . C24 C 0.6811(5) 0.5103(3) 0.7578(3) 0.0188(10) Uani 1 1 d . . . H24 H 0.7483 0.5508 0.7335 0.023 Uiso 1 1 calc R . . C25 C 0.7338(5) 0.4176(3) 0.7874(3) 0.0253(11) Uani 1 1 d . . . H25 H 0.8368 0.3936 0.7834 0.030 Uiso 1 1 calc R . . C26 C 0.6323(5) 0.3613(3) 0.8229(3) 0.0230(10) Uani 1 1 d . . . C27 C 0.4816(5) 0.3923(3) 0.8303(3) 0.0208(10) Uani 1 1 d . . . H27 H 0.4152 0.3519 0.8559 0.025 Uiso 1 1 calc R . . C28 C 0.4306(5) 0.4846(3) 0.7990(2) 0.0165(9) Uani 1 1 d . . . H28 H 0.3272 0.5076 0.8017 0.020 Uiso 1 1 calc R . . C29 C -0.0400(4) 0.6677(3) 0.8180(2) 0.0119(8) Uani 1 1 d . . . C30 C 0.0580(4) 0.6036(3) 0.8736(2) 0.0125(8) Uani 1 1 d . . . C31 C 0.1585(5) 0.6376(3) 0.9057(3) 0.0191(10) Uani 1 1 d . . . H31 H 0.1659 0.7015 0.8913 0.023 Uiso 1 1 calc R . . C32 C 0.2469(5) 0.5793(4) 0.9582(3) 0.0214(10) Uani 1 1 d . . . H32 H 0.3117 0.6024 0.9823 0.026 Uiso 1 1 calc R . . C33 C 0.2383(5) 0.4861(3) 0.9745(2) 0.0177(9) Uani 1 1 d . . . C34 C 0.1432(5) 0.4488(3) 0.9429(2) 0.0170(9) Uani 1 1 d . . . H34 H 0.1420 0.3841 0.9549 0.020 Uiso 1 1 calc R . . C35 C 0.0488(5) 0.5098(3) 0.8927(2) 0.0153(9) Uani 1 1 d . . . H35 H -0.0216 0.4872 0.8717 0.018 Uiso 1 1 calc R . . C36 C 0.0208(4) 0.6626(3) 0.6319(2) 0.0124(8) Uani 1 1 d . . . C37 C 0.0874(5) 0.5720(3) 0.6112(2) 0.0147(9) Uani 1 1 d . . . C38 C 0.2426(5) 0.5496(4) 0.6000(3) 0.0221(10) Uani 1 1 d . . . H38 H 0.3039 0.5892 0.6086 0.027 Uiso 1 1 calc R . . C39 C 0.3049(6) 0.4703(4) 0.5767(3) 0.0304(12) Uani 1 1 d . . . H39 H 0.4095 0.4547 0.5687 0.037 Uiso 1 1 calc R . . C40 C 0.2148(6) 0.4140(4) 0.5652(3) 0.0287(12) Uani 1 1 d . . . C41 C 0.0614(6) 0.4315(3) 0.5781(3) 0.0233(10) Uani 1 1 d . . . H41 H 0.0014 0.3903 0.5709 0.028 Uiso 1 1 calc R . . C42 C -0.0006(5) 0.5122(3) 0.6021(3) 0.0184(9) Uani 1 1 d . . . H42 H -0.1049 0.5260 0.6123 0.022 Uiso 1 1 calc R . . Eu1 Eu -0.26226(2) 0.786975(14) 0.720218(11) 0.00918(6) Uani 1 1 d . . . Eu2 Eu 0.18520(2) 0.812826(14) 0.686429(11) 0.00979(6) Uani 1 1 d . . . N1 N -0.8346(4) 1.2840(3) 0.7921(3) 0.0271(10) Uani 1 1 d . . . N2 N -0.3297(5) 1.3314(3) 0.6245(2) 0.0231(9) Uani 1 1 d . . . N3 N 0.1979(4) 1.1153(3) 1.0193(2) 0.0213(9) Uani 1 1 d . . . N4 N 0.6877(5) 0.2622(3) 0.8521(3) 0.0365(12) Uani 1 1 d . . . N5 N 0.3384(4) 0.4232(3) 1.0278(2) 0.0244(10) Uani 1 1 d . . . N6 N 0.2802(6) 0.3321(4) 0.5346(3) 0.0401(13) Uani 1 1 d . . . O1 O -0.6512(3) 0.9215(2) 0.65942(18) 0.0173(7) Uani 1 1 d . . . O2 O -0.4393(3) 0.9233(2) 0.70344(17) 0.0148(6) Uani 1 1 d . . . O3 O -0.9072(5) 1.3470(3) 0.7502(2) 0.0433(11) Uani 1 1 d . . . O4 O -0.8174(4) 1.2834(3) 0.8562(2) 0.0341(9) Uani 1 1 d . . . O5 O -0.0984(3) 0.8934(2) 0.65919(16) 0.0144(6) Uani 1 1 d . . . O6 O 0.0876(3) 0.9502(2) 0.58973(17) 0.0153(6) Uani 1 1 d . . . O7 O -0.4340(4) 1.3406(3) 0.6707(2) 0.0323(9) Uani 1 1 d . . . O8 O -0.2823(5) 1.3954(3) 0.5807(2) 0.0393(10) Uani 1 1 d . . . O9 O 0.0650(3) 0.9215(2) 0.76957(16) 0.0122(6) Uani 1 1 d . . . O10 O 0.2671(3) 0.8277(2) 0.80835(17) 0.0134(6) Uani 1 1 d . . . O11 O 0.0925(4) 1.1732(3) 1.0316(2) 0.0296(8) Uani 1 1 d . . . O12 O 0.3168(4) 1.1027(3) 1.0472(2) 0.0292(8) Uani 1 1 d . . . O13 O 0.3356(3) 0.6697(2) 0.73118(17) 0.0149(6) Uani 1 1 d . . . O14 O 0.5667(3) 0.6977(2) 0.70780(18) 0.0172(7) Uani 1 1 d . . . O15 O 0.6010(5) 0.2132(3) 0.8876(3) 0.0475(12) Uani 1 1 d . . . O16 O 0.8191(5) 0.2329(3) 0.8369(3) 0.0601(15) Uani 1 1 d . . . O17 O -0.1707(3) 0.6554(2) 0.81921(17) 0.0145(6) Uani 1 1 d . . . O18 O 0.0102(3) 0.7344(2) 0.77203(16) 0.0131(6) Uani 1 1 d . . . O19 O 0.3587(4) 0.3399(3) 1.0283(2) 0.0363(10) Uani 1 1 d . . . O20 O 0.3983(4) 0.4558(3) 1.0678(2) 0.0330(9) Uani 1 1 d . . . O21 O -0.1123(3) 0.6730(2) 0.65760(17) 0.0152(6) Uani 1 1 d . . . O22 O 0.1044(3) 0.7229(2) 0.61975(17) 0.0154(6) Uani 1 1 d . . . O23 O 0.1959(5) 0.2866(3) 0.5190(2) 0.0425(11) Uani 1 1 d . . . O24 O 0.4162(5) 0.3149(4) 0.5250(3) 0.0671(17) Uani 1 1 d . . . O25 O -0.3222(3) 0.8258(2) 0.58710(17) 0.0159(6) Uani 1 1 d . . . O26 O -0.4399(3) 0.7764(2) 0.83314(17) 0.0163(7) Uani 1 1 d . . . O27 O -0.2165(3) 0.8777(2) 0.80634(16) 0.0150(6) Uani 1 1 d . . . O28 O 0.3722(3) 0.7937(2) 0.57883(17) 0.0166(7) Uani 1 1 d . . . O29 O 0.6542(5) 0.9991(3) 0.5086(2) 0.0360(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0114(18) 0.010(2) 0.012(2) -0.0018(16) 0.0016(15) -0.0020(16) C2 0.0090(18) 0.013(2) 0.012(2) -0.0055(17) 0.0032(15) -0.0010(16) C3 0.0118(19) 0.020(2) 0.018(2) -0.0044(19) -0.0027(17) 0.0003(18) C4 0.014(2) 0.015(2) 0.027(3) -0.003(2) 0.0003(18) 0.0052(18) C5 0.016(2) 0.018(2) 0.026(3) -0.011(2) 0.0113(18) -0.0028(19) C6 0.016(2) 0.021(2) 0.023(2) -0.010(2) 0.0040(18) -0.0070(19) C7 0.0096(19) 0.017(2) 0.018(2) -0.0057(18) 0.0012(16) -0.0034(17) C8 0.0123(19) 0.012(2) 0.0086(19) -0.0030(16) -0.0033(15) -0.0010(16) C9 0.0102(18) 0.013(2) 0.016(2) -0.0066(17) -0.0029(16) 0.0005(16) C10 0.019(2) 0.015(2) 0.029(3) -0.005(2) 0.008(2) -0.0052(19) C11 0.014(2) 0.020(3) 0.034(3) -0.011(2) 0.0069(19) -0.0004(19) C12 0.019(2) 0.013(2) 0.024(2) -0.0060(19) -0.0065(19) 0.0008(18) C13 0.032(3) 0.012(2) 0.014(2) -0.0027(18) -0.0009(19) -0.0016(19) C14 0.022(2) 0.019(2) 0.017(2) -0.0068(19) 0.0002(18) -0.0046(19) C15 0.0116(19) 0.013(2) 0.017(2) -0.0054(17) 0.0014(16) -0.0040(16) C16 0.0106(19) 0.013(2) 0.015(2) -0.0046(17) 0.0017(16) -0.0023(16) C17 0.0132(19) 0.017(2) 0.015(2) -0.0056(18) -0.0008(16) -0.0043(17) C18 0.015(2) 0.016(2) 0.019(2) -0.0088(18) 0.0019(17) 0.0012(17) C19 0.017(2) 0.019(2) 0.011(2) -0.0097(18) 0.0016(16) -0.0056(18) C20 0.016(2) 0.024(3) 0.015(2) -0.0060(19) -0.0010(17) -0.0013(19) C21 0.014(2) 0.017(2) 0.018(2) -0.0066(18) -0.0022(17) 0.0039(17) C22 0.0134(19) 0.014(2) 0.012(2) -0.0065(17) -0.0012(16) -0.0005(17) C23 0.014(2) 0.013(2) 0.014(2) -0.0049(17) -0.0027(16) 0.0009(17) C24 0.015(2) 0.014(2) 0.029(3) -0.010(2) 0.0001(18) -0.0013(18) C25 0.016(2) 0.019(2) 0.044(3) -0.014(2) -0.013(2) 0.0056(19) C26 0.027(2) 0.012(2) 0.031(3) -0.007(2) -0.013(2) 0.0070(19) C27 0.021(2) 0.016(2) 0.024(2) -0.005(2) -0.0018(19) -0.0013(19) C28 0.0112(19) 0.017(2) 0.020(2) -0.0040(19) -0.0002(17) -0.0025(17) C29 0.0069(17) 0.014(2) 0.015(2) -0.0082(17) 0.0002(15) 0.0043(16) C30 0.0073(18) 0.018(2) 0.010(2) -0.0048(17) 0.0034(15) 0.0015(16) C31 0.016(2) 0.018(2) 0.020(2) -0.0002(19) 0.0008(18) -0.0026(18) C32 0.011(2) 0.034(3) 0.020(2) -0.003(2) -0.0028(18) -0.0059(19) C33 0.0098(19) 0.022(2) 0.016(2) 0.0005(19) 0.0008(17) 0.0048(18) C34 0.018(2) 0.016(2) 0.013(2) -0.0041(18) 0.0032(17) 0.0038(18) C35 0.0129(19) 0.018(2) 0.015(2) -0.0045(18) -0.0003(16) -0.0026(17) C36 0.0135(19) 0.013(2) 0.012(2) -0.0070(17) -0.0035(16) 0.0016(16) C37 0.014(2) 0.014(2) 0.014(2) -0.0063(17) -0.0002(16) 0.0033(17) C38 0.015(2) 0.026(3) 0.026(3) -0.012(2) -0.0019(19) 0.0043(19) C39 0.021(2) 0.039(3) 0.030(3) -0.018(3) -0.004(2) 0.013(2) C40 0.040(3) 0.024(3) 0.020(3) -0.013(2) -0.005(2) 0.013(2) C41 0.035(3) 0.015(2) 0.022(2) -0.009(2) -0.003(2) -0.002(2) C42 0.021(2) 0.017(2) 0.019(2) -0.0094(19) 0.0009(18) -0.0001(18) Eu1 0.00568(9) 0.00963(11) 0.01232(11) -0.00422(8) -0.00085(7) 0.00083(7) Eu2 0.00633(9) 0.01033(11) 0.01321(11) -0.00513(8) -0.00064(7) 0.00051(8) N1 0.019(2) 0.019(2) 0.042(3) -0.013(2) 0.0120(19) -0.0043(18) N2 0.029(2) 0.015(2) 0.026(2) -0.0083(18) -0.0097(18) 0.0023(17) N3 0.022(2) 0.028(2) 0.0147(19) -0.0095(17) 0.0049(16) -0.0051(18) N4 0.036(3) 0.015(2) 0.059(3) -0.005(2) -0.026(2) 0.004(2) N5 0.0128(18) 0.034(3) 0.017(2) 0.0025(18) 0.0029(16) 0.0058(18) N6 0.054(3) 0.031(3) 0.029(3) -0.018(2) -0.010(2) 0.025(2) O1 0.0146(15) 0.0183(17) 0.0227(17) -0.0114(14) 0.0002(13) -0.0041(13) O2 0.0099(13) 0.0133(15) 0.0198(16) -0.0058(13) -0.0026(12) 0.0047(12) O3 0.045(2) 0.023(2) 0.051(3) -0.009(2) 0.010(2) 0.0138(19) O4 0.032(2) 0.030(2) 0.046(2) -0.0277(19) 0.0077(18) -0.0032(17) O5 0.0137(14) 0.0160(16) 0.0142(15) -0.0052(13) 0.0000(12) -0.0025(12) O6 0.0110(14) 0.0172(16) 0.0163(15) -0.0038(13) -0.0014(12) 0.0012(12) O7 0.032(2) 0.024(2) 0.038(2) -0.0143(17) 0.0000(17) 0.0094(16) O8 0.058(3) 0.0137(19) 0.041(2) -0.0046(17) 0.003(2) -0.0003(18) O9 0.0080(13) 0.0146(15) 0.0158(15) -0.0078(12) -0.0031(11) 0.0010(11) O10 0.0096(13) 0.0129(15) 0.0197(16) -0.0101(13) -0.0011(12) 0.0015(12) O11 0.0283(19) 0.031(2) 0.033(2) -0.0209(17) -0.0022(16) 0.0034(16) O12 0.0226(18) 0.043(2) 0.030(2) -0.0238(18) -0.0020(15) -0.0062(17) O13 0.0088(13) 0.0123(15) 0.0215(16) -0.0044(13) 0.0017(12) 0.0023(12) O14 0.0130(14) 0.0141(16) 0.0236(17) -0.0017(13) -0.0022(13) -0.0031(12) O15 0.051(3) 0.017(2) 0.070(3) 0.007(2) -0.025(2) -0.0048(19) O16 0.039(2) 0.023(2) 0.112(4) -0.005(3) -0.026(3) 0.012(2) O17 0.0096(13) 0.0146(16) 0.0180(16) -0.0020(13) -0.0018(12) -0.0007(12) O18 0.0122(14) 0.0108(15) 0.0148(15) -0.0019(12) -0.0006(12) 0.0004(12) O19 0.037(2) 0.032(2) 0.028(2) -0.0026(17) -0.0049(17) 0.0198(18) O20 0.0197(18) 0.050(3) 0.0245(19) 0.0052(18) -0.0085(15) -0.0069(17) O21 0.0102(14) 0.0173(16) 0.0203(16) -0.0107(13) -0.0011(12) 0.0001(12) O22 0.0153(14) 0.0178(16) 0.0156(15) -0.0095(13) 0.0019(12) -0.0035(13) O23 0.073(3) 0.023(2) 0.032(2) -0.0175(18) -0.002(2) 0.007(2) O24 0.053(3) 0.071(4) 0.084(4) -0.059(3) -0.022(3) 0.039(3) O25 0.0157(14) 0.0177(16) 0.0145(15) -0.0061(13) 0.0009(12) -0.0014(13) O26 0.0081(13) 0.0211(17) 0.0163(16) -0.0023(13) 0.0004(12) 0.0023(12) O27 0.0083(13) 0.0240(17) 0.0149(15) -0.0107(13) 0.0006(11) -0.0010(12) O28 0.0091(14) 0.0205(17) 0.0194(16) -0.0063(13) 0.0009(12) 0.0002(12) O29 0.056(3) 0.026(2) 0.026(2) 0.0000(16) -0.0032(19) -0.0141(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.250(5) . ? C1 O1 1.255(5) . ? C1 C2 1.501(6) . ? C2 C3 1.385(6) . ? C2 C7 1.406(6) . ? C3 C4 1.395(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(7) . ? C4 H4 0.9500 . ? C5 C6 1.380(7) . ? C5 N1 1.475(6) . ? C6 C7 1.386(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O6 1.257(5) . ? C8 O5 1.261(5) . ? C8 C9 1.506(6) . ? C9 C14 1.386(6) . ? C9 C10 1.387(6) . ? C10 C11 1.385(7) . ? C10 H10 0.9500 . ? C11 C12 1.377(7) . ? C11 H11 0.9500 . ? C12 C13 1.380(6) . ? C12 N2 1.484(6) . ? C13 C14 1.381(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O9 1.262(5) . ? C15 O10 1.266(5) . ? C15 C16 1.495(6) . ? C16 C17 1.397(6) . ? C16 C21 1.399(6) . ? C17 C18 1.383(6) . ? C17 H17 0.9500 . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 C20 1.381(7) . ? C19 N3 1.477(6) . ? C20 C21 1.386(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O14 1.253(5) . ? C22 O13 1.260(5) . ? C22 C23 1.503(6) . ? C23 C28 1.392(6) . ? C23 C24 1.397(6) . ? C24 C25 1.390(7) . ? C24 H24 0.9500 . ? C25 C26 1.383(7) . ? C25 H25 0.9500 . ? C26 C27 1.381(7) . ? C26 N4 1.476(6) . ? C27 C28 1.389(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 O17 1.251(5) . ? C29 O18 1.273(5) . ? C29 C30 1.495(6) . ? C30 C35 1.391(6) . ? C30 C31 1.395(6) . ? C31 C32 1.378(6) . ? C31 H31 0.9500 . ? C32 C33 1.381(7) . ? C32 H32 0.9500 . ? C33 C34 1.382(7) . ? C33 N5 1.473(6) . ? C34 C35 1.399(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 O21 1.255(5) . ? C36 O22 1.265(5) . ? C36 C37 1.508(6) . ? C37 C42 1.375(6) . ? C37 C38 1.408(6) . ? C38 C39 1.371(7) . ? C38 H38 0.9500 . ? C39 C40 1.364(8) . ? C39 H39 0.9500 . ? C40 C41 1.391(7) . ? C40 N6 1.479(6) . ? C41 C42 1.396(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? Eu1 O14 2.327(3) 1_455 ? Eu1 O2 2.353(3) . ? Eu1 O5 2.402(3) . ? Eu1 O21 2.428(3) . ? Eu1 O17 2.452(3) . ? Eu1 O27 2.465(3) . ? Eu1 O26 2.490(3) . ? Eu1 O25 2.506(3) . ? Eu1 O18 2.709(3) . ? Eu2 O22 2.317(3) . ? Eu2 O13 2.357(3) . ? Eu2 O1 2.362(3) 1_655 ? Eu2 O18 2.391(3) . ? Eu2 O6 2.494(3) . ? Eu2 O28 2.509(3) . ? Eu2 O9 2.535(3) . ? Eu2 O10 2.548(3) . ? Eu2 O5 2.719(3) . ? N1 O3 1.219(6) . ? N1 O4 1.220(6) . ? N2 O8 1.216(6) . ? N2 O7 1.218(5) . ? N3 O11 1.217(5) . ? N3 O12 1.233(5) . ? N4 O15 1.215(6) . ? N4 O16 1.232(6) . ? N5 O20 1.218(6) . ? N5 O19 1.235(6) . ? N6 O24 1.231(7) . ? N6 O23 1.232(7) . ? O1 Eu2 2.362(3) 1_455 ? O14 Eu1 2.327(3) 1_655 ? 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 O2 C1 O1 124.7(4) . . ? O2 C1 C2 117.7(4) . . ? O1 C1 C2 117.7(4) . . ? C3 C2 C7 119.7(4) . . ? C3 C2 C1 120.9(4) . . ? C7 C2 C1 119.3(4) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 118.1(4) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C6 C5 C4 123.3(4) . . ? C6 C5 N1 117.9(5) . . ? C4 C5 N1 118.8(4) . . ? C5 C6 C7 117.9(4) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C6 C7 C2 120.5(4) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O6 C8 O5 121.4(4) . . ? O6 C8 C9 118.3(4) . . ? O5 C8 C9 120.0(4) . . ? C14 C9 C10 120.0(4) . . ? C14 C9 C8 121.2(4) . . ? C10 C9 C8 118.6(4) . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 122.4(4) . . ? C11 C12 N2 117.8(4) . . ? C13 C12 N2 119.8(4) . . ? C12 C13 C14 118.3(4) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C13 C14 C9 120.6(4) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O9 C15 O10 120.8(4) . . ? O9 C15 C16 119.1(4) . . ? O10 C15 C16 120.0(4) . . ? C17 C16 C21 120.0(4) . . ? C17 C16 C15 119.7(4) . . ? C21 C16 C15 120.2(4) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 117.7(4) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C20 C19 C18 123.8(4) . . ? C20 C19 N3 118.3(4) . . ? C18 C19 N3 117.9(4) . . ? C19 C20 C21 117.8(4) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C20 C21 C16 120.2(4) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? O14 C22 O13 124.2(4) . . ? O14 C22 C23 118.7(4) . . ? O13 C22 C23 117.1(4) . . ? C28 C23 C24 120.0(4) . . ? C28 C23 C22 120.6(4) . . ? C24 C23 C22 119.3(4) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 118.1(4) . . ? C26 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? C27 C26 C25 123.5(4) . . ? C27 C26 N4 118.3(5) . . ? C25 C26 N4 118.2(4) . . ? C26 C27 C28 117.5(4) . . ? C26 C27 H27 121.2 . . ? C28 C27 H27 121.2 . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? O17 C29 O18 121.8(4) . . ? O17 C29 C30 118.8(4) . . ? O18 C29 C30 119.4(3) . . ? C35 C30 C31 120.3(4) . . ? C35 C30 C29 119.4(4) . . ? C31 C30 C29 120.2(4) . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 117.8(4) . . ? C31 C32 H32 121.1 . . ? C33 C32 H32 121.1 . . ? C32 C33 C34 123.7(4) . . ? C32 C33 N5 117.7(4) . . ? C34 C33 N5 118.5(4) . . ? C33 C34 C35 117.5(4) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C30 C35 C34 119.9(4) . . ? C30 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? O21 C36 O22 125.6(4) . . ? O21 C36 C37 118.2(4) . . ? O22 C36 C37 116.2(4) . . ? C42 C37 C38 119.9(4) . . ? C42 C37 C36 121.2(4) . . ? C38 C37 C36 118.9(4) . . ? C39 C38 C37 119.7(5) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.2(5) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 123.1(5) . . ? C39 C40 N6 119.5(5) . . ? C41 C40 N6 117.3(5) . . ? C40 C41 C42 117.1(5) . . ? C40 C41 H41 121.4 . . ? C42 C41 H41 121.4 . . ? C37 C42 C41 120.8(4) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? O14 Eu1 O2 92.45(11) 1_455 . ? O14 Eu1 O5 147.29(11) 1_455 . ? O2 Eu1 O5 82.16(11) . . ? O14 Eu1 O21 77.38(10) 1_455 . ? O2 Eu1 O21 144.15(10) . . ? O5 Eu1 O21 88.23(10) . . ? O14 Eu1 O17 85.70(11) 1_455 . ? O2 Eu1 O17 140.11(11) . . ? O5 Eu1 O17 118.67(10) . . ? O21 Eu1 O17 74.11(11) . . ? O14 Eu1 O27 139.06(11) 1_455 . ? O2 Eu1 O27 72.63(10) . . ? O5 Eu1 O27 69.86(10) . . ? O21 Eu1 O27 135.37(10) . . ? O17 Eu1 O27 82.94(10) . . ? O14 Eu1 O26 72.49(11) 1_455 . ? O2 Eu1 O26 72.12(11) . . ? O5 Eu1 O26 134.27(10) . . ? O21 Eu1 O26 133.67(11) . . ? O17 Eu1 O26 69.36(10) . . ? O27 Eu1 O26 66.68(10) . . ? O14 Eu1 O25 71.03(11) 1_455 . ? O2 Eu1 O25 73.02(11) . . ? O5 Eu1 O25 76.56(10) . . ? O21 Eu1 O25 71.15(10) . . ? O17 Eu1 O25 141.48(10) . . ? O27 Eu1 O25 134.40(10) . . ? O26 Eu1 O25 127.44(10) . . ? O14 Eu1 O18 130.05(10) 1_455 . ? O2 Eu1 O18 135.58(10) . . ? O5 Eu1 O18 68.41(10) . . ? O21 Eu1 O18 69.44(10) . . ? O17 Eu1 O18 50.30(9) . . ? O27 Eu1 O18 66.44(10) . . ? O26 Eu1 O18 105.32(9) . . ? O25 Eu1 O18 127.09(10) . . ? O22 Eu2 O13 80.47(11) . . ? O22 Eu2 O1 135.00(11) . 1_655 ? O13 Eu2 O1 104.49(11) . 1_655 ? O22 Eu2 O18 75.80(11) . . ? O13 Eu2 O18 79.52(10) . . ? O1 Eu2 O18 149.13(11) 1_655 . ? O22 Eu2 O6 87.11(11) . . ? O13 Eu2 O6 155.42(10) . . ? O1 Eu2 O6 70.00(11) 1_655 . ? O18 Eu2 O6 117.96(10) . . ? O22 Eu2 O28 71.47(10) . . ? O13 Eu2 O28 76.38(11) . . ? O1 Eu2 O28 66.69(11) 1_655 . ? O18 Eu2 O28 141.91(10) . . ? O6 Eu2 O28 79.59(10) . . ? O22 Eu2 O9 136.23(10) . . ? O13 Eu2 O9 122.81(10) . . ? O1 Eu2 O9 78.97(10) 1_655 . ? O18 Eu2 O9 73.59(10) . . ? O6 Eu2 O9 80.50(10) . . ? O28 Eu2 O9 144.50(10) . . ? O22 Eu2 O10 148.69(10) . . ? O13 Eu2 O10 75.35(10) . . ? O1 Eu2 O10 71.35(11) 1_655 . ? O18 Eu2 O10 80.44(10) . . ? O6 Eu2 O10 122.38(10) . . ? O28 Eu2 O10 120.39(9) . . ? O9 Eu2 O10 51.24(9) . . ? O22 Eu2 O5 74.55(10) . . ? O13 Eu2 O5 143.09(10) . . ? O1 Eu2 O5 112.40(10) 1_655 . ? O18 Eu2 O5 68.38(10) . . ? O6 Eu2 O5 49.58(9) . . ? O28 Eu2 O5 119.14(10) . . ? O9 Eu2 O5 65.47(9) . . ? O10 Eu2 O5 114.98(9) . . ? O3 N1 O4 124.8(4) . . ? O3 N1 C5 117.8(5) . . ? O4 N1 C5 117.4(4) . . ? O8 N2 O7 124.2(4) . . ? O8 N2 C12 117.8(4) . . ? O7 N2 C12 118.0(4) . . ? O11 N3 O12 123.5(4) . . ? O11 N3 C19 119.2(4) . . ? O12 N3 C19 117.3(4) . . ? O15 N4 O16 123.5(5) . . ? O15 N4 C26 118.7(5) . . ? O16 N4 C26 117.7(5) . . ? O20 N5 O19 123.6(4) . . ? O20 N5 C33 118.8(4) . . ? O19 N5 C33 117.5(4) . . ? O24 N6 O23 124.1(5) . . ? O24 N6 C40 117.5(5) . . ? O23 N6 C40 118.4(5) . . ? C1 O1 Eu2 142.0(3) . 1_455 ? C1 O2 Eu1 144.8(3) . . ? C8 O5 Eu1 165.7(3) . . ? C8 O5 Eu2 85.2(2) . . ? Eu1 O5 Eu2 109.08(11) . . ? C8 O6 Eu2 95.5(3) . . ? C15 O9 Eu2 94.1(2) . . ? C15 O10 Eu2 93.4(3) . . ? C22 O13 Eu2 133.0(3) . . ? C22 O14 Eu1 154.3(3) . 1_655 ? C29 O17 Eu1 100.3(3) . . ? C29 O18 Eu2 157.7(3) . . ? C29 O18 Eu1 87.6(2) . . ? Eu2 O18 Eu1 109.77(11) . . ? C36 O21 Eu1 132.6(3) . . ? C36 O22 Eu2 137.4(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.597 _refine_diff_density_min -1.675 _refine_diff_density_rms 0.143 # Attachment 'CCDC603287.cif' data_pbar1-jan0806a _database_code_depnum_ccdc_archive 'CCDC 603287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Terbium 4-Nitrobenzoate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 N6 O29 Tb2' _chemical_formula_weight 1404.59 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2692(19) _cell_length_b 15.369(3) _cell_length_c 18.353(4) _cell_angle_alpha 75.37(3) _cell_angle_beta 81.32(3) _cell_angle_gamma 78.15(3) _cell_volume 2462.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 96(2) _cell_measurement_reflns_used 6330 _cell_measurement_theta_min 2.446 _cell_measurement_theta_max 28.2815 _exptl_crystal_description needles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 2.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4711 _exptl_absorpt_correction_T_max 0.8910 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 96(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 CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 25707 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.00 _reflns_number_total 11802 _reflns_number_gt 10487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0334P)^2^+3.7647P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11802 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.8316(3) 0.6066(2) 0.18398(18) 0.0139(6) Uani 1 1 d . . . C2 C 0.8334(4) 0.5527(2) 0.12596(19) 0.0147(6) Uani 1 1 d . . . C3 C 0.7267(4) 0.5799(2) 0.07489(19) 0.0185(7) Uani 1 1 d . . . H3 H 0.6601 0.6361 0.0730 0.022 Uiso 1 1 calc R . . C4 C 0.7171(4) 0.5252(2) 0.0268(2) 0.0205(7) Uani 1 1 d . . . H4 H 0.6433 0.5422 -0.0074 0.025 Uiso 1 1 calc R . . C5 C 0.8191(4) 0.4446(2) 0.03028(19) 0.0183(7) Uani 1 1 d . . . C6 C 0.9300(4) 0.4177(2) 0.0778(2) 0.0185(7) Uani 1 1 d . . . H6 H 1.0003 0.3632 0.0773 0.022 Uiso 1 1 calc R . . C7 C 0.9356(4) 0.4726(2) 0.12629(19) 0.0169(6) Uani 1 1 d . . . H7 H 1.0101 0.4554 0.1601 0.020 Uiso 1 1 calc R . . C8 C 1.0307(4) 0.5427(2) 0.38063(18) 0.0134(6) Uani 1 1 d . . . C9 C 1.1059(4) 0.4450(2) 0.3862(2) 0.0157(6) Uani 1 1 d . . . C10 C 1.0502(4) 0.3742(2) 0.4381(2) 0.0218(7) Uani 1 1 d . . . H10 H 0.9691 0.3873 0.4743 0.026 Uiso 1 1 calc R . . C11 C 1.1124(5) 0.2840(2) 0.4373(2) 0.0265(8) Uani 1 1 d . . . H11 H 1.0751 0.2350 0.4728 0.032 Uiso 1 1 calc R . . C12 C 1.2298(4) 0.2677(2) 0.3836(2) 0.0224(7) Uani 1 1 d . . . C13 C 1.2872(4) 0.3364(3) 0.3323(3) 0.0359(11) Uani 1 1 d . . . H13 H 1.3684 0.3231 0.2962 0.043 Uiso 1 1 calc R . . C14 C 1.2246(4) 0.4264(3) 0.3338(3) 0.0327(10) Uani 1 1 d . . . H14 H 1.2637 0.4752 0.2988 0.039 Uiso 1 1 calc R . . C15 C 1.5604(4) 0.5464(2) 0.30902(18) 0.0131(6) Uani 1 1 d . . . C16 C 1.6254(3) 0.4583(2) 0.28590(19) 0.0139(6) Uani 1 1 d . . . C17 C 1.5685(4) 0.4364(2) 0.22759(19) 0.0164(6) Uani 1 1 d . . . H17 H 1.4855 0.4754 0.2052 0.020 Uiso 1 1 calc R . . C18 C 1.6323(4) 0.3583(2) 0.2024(2) 0.0215(7) Uani 1 1 d . . . H18 H 1.5964 0.3439 0.1618 0.026 Uiso 1 1 calc R . . C19 C 1.7500(4) 0.3020(2) 0.2381(2) 0.0240(8) Uani 1 1 d . . . C20 C 1.8082(4) 0.3207(2) 0.2963(2) 0.0238(8) Uani 1 1 d . . . H20 H 1.8885 0.2798 0.3198 0.029 Uiso 1 1 calc R . . C21 C 1.7463(4) 0.4009(2) 0.3196(2) 0.0202(7) Uani 1 1 d . . . H21 H 1.7863 0.4166 0.3583 0.024 Uiso 1 1 calc R . . C22 C 0.9586(4) 0.8332(2) 0.36769(18) 0.0141(6) Uani 1 1 d . . . C23 C 0.8901(4) 0.9227(2) 0.38827(19) 0.0162(6) Uani 1 1 d . . . C24 C 0.9779(4) 0.9800(2) 0.3996(2) 0.0218(7) Uani 1 1 d . . . H24 H 1.0827 0.9652 0.3905 0.026 Uiso 1 1 calc R . . C25 C 0.9137(5) 1.0585(2) 0.4242(2) 0.0265(8) Uani 1 1 d . . . H25 H 0.9729 1.0980 0.4326 0.032 Uiso 1 1 calc R . . C26 C 0.7598(5) 1.0780(3) 0.4361(2) 0.0284(9) Uani 1 1 d . . . C27 C 0.6693(5) 1.0239(3) 0.4223(2) 0.0305(9) Uani 1 1 d . . . H27 H 0.5644 1.0400 0.4293 0.037 Uiso 1 1 calc R . . C28 C 0.7363(4) 0.9461(3) 0.3980(2) 0.0233(8) Uani 1 1 d . . . H28 H 0.6769 0.9078 0.3878 0.028 Uiso 1 1 calc R . . C29 C 1.0297(3) 0.8285(2) 0.18170(18) 0.0141(6) Uani 1 1 d . . . C30 C 0.9355(3) 0.8964(2) 0.12651(18) 0.0138(6) Uani 1 1 d . . . C31 C 0.9494(4) 0.9880(2) 0.10937(19) 0.0185(7) Uani 1 1 d . . . H31 H 1.0203 1.0069 0.1317 0.022 Uiso 1 1 calc R . . C32 C 0.8595(4) 1.0519(2) 0.0596(2) 0.0225(8) Uani 1 1 d . . . H32 H 0.8649 1.1150 0.0489 0.027 Uiso 1 1 calc R . . C33 C 0.7619(4) 1.0207(3) 0.0262(2) 0.0253(8) Uani 1 1 d . . . C34 C 0.7499(4) 0.9298(3) 0.0403(2) 0.0268(8) Uani 1 1 d . . . H34 H 0.6847 0.9105 0.0148 0.032 Uiso 1 1 calc R . . C35 C 0.8350(4) 0.8672(3) 0.0925(2) 0.0211(7) Uani 1 1 d . . . H35 H 0.8251 0.8047 0.1050 0.025 Uiso 1 1 calc R . . C36 C 0.5080(4) 0.8537(2) 0.26666(18) 0.0135(6) Uani 1 1 d . . . C37 C 0.4543(4) 0.9541(2) 0.23695(18) 0.0146(6) Uani 1 1 d . . . C38 C 0.5555(4) 1.0119(2) 0.2045(2) 0.0189(7) Uani 1 1 d . . . H38 H 0.6587 0.9882 0.2021 0.023 Uiso 1 1 calc R . . C39 C 0.5066(4) 1.1037(2) 0.1756(2) 0.0234(8) Uani 1 1 d . . . H39 H 0.5745 1.1435 0.1518 0.028 Uiso 1 1 calc R . . C40 C 0.3552(4) 1.1358(2) 0.1826(2) 0.0268(8) Uani 1 1 d . . . C41 C 0.2514(4) 1.0804(3) 0.2149(3) 0.0287(9) Uani 1 1 d . . . H41 H 0.1484 1.1048 0.2187 0.034 Uiso 1 1 calc R . . C42 C 0.3029(4) 0.9880(2) 0.2415(2) 0.0213(7) Uani 1 1 d . . . H42 H 0.2346 0.9478 0.2630 0.026 Uiso 1 1 calc R . . N1 N 0.8064(4) 0.3848(2) -0.01871(17) 0.0241(7) Uani 1 1 d . . . N2 N 1.2945(4) 0.1722(2) 0.38061(19) 0.0274(7) Uani 1 1 d . . . N3 N 1.8196(4) 0.2193(2) 0.2098(2) 0.0312(8) Uani 1 1 d . . . N4 N 0.6905(5) 1.1577(3) 0.4678(2) 0.0418(10) Uani 1 1 d . . . N5 N 0.6644(4) 1.0869(3) -0.0262(2) 0.0361(9) Uani 1 1 d . . . N6 N 0.3022(4) 1.2347(2) 0.1558(3) 0.0403(10) Uani 1 1 d . . . O1 O 0.7301(2) 0.67491(16) 0.18731(14) 0.0165(5) Uani 1 1 d . . . O2 O 0.9280(2) 0.58088(15) 0.23046(13) 0.0149(5) Uani 1 1 d . . . O3 O 0.6889(3) 0.3969(2) -0.04635(17) 0.0343(7) Uani 1 1 d . . . O4 O 0.9130(3) 0.32621(19) -0.03051(17) 0.0311(6) Uani 1 1 d . . . O5 O 0.8969(3) 0.55779(15) 0.40677(13) 0.0166(5) Uani 1 1 d . . . O6 O 1.0978(3) 0.60646(15) 0.34519(14) 0.0177(5) Uani 1 1 d . . . O7 O 1.2359(4) 0.11112(19) 0.42117(19) 0.0436(8) Uani 1 1 d . . . O8 O 1.4058(3) 0.1602(2) 0.3361(2) 0.0385(7) Uani 1 1 d . . . O9 O 1.4283(3) 0.57888(16) 0.29793(14) 0.0177(5) Uani 1 1 d . . . O10 O 1.6414(3) 0.58221(17) 0.33750(15) 0.0205(5) Uani 1 1 d . . . O11 O 1.8028(4) 0.2189(2) 0.1455(2) 0.0413(8) Uani 1 1 d . . . O12 O 1.8907(4) 0.1571(2) 0.2525(2) 0.0508(10) Uani 1 1 d . . . O13 O 0.8732(3) 0.77636(16) 0.37720(13) 0.0165(5) Uani 1 1 d . . . O14 O 1.0933(2) 0.82067(16) 0.34382(14) 0.0169(5) Uani 1 1 d . . . O15 O 0.5543(4) 1.1726(3) 0.4807(2) 0.0608(11) Uani 1 1 d . . . O16 O 0.7725(5) 1.2042(2) 0.48019(19) 0.0483(9) Uani 1 1 d . . . O17 O 0.9758(2) 0.76319(15) 0.22678(13) 0.0137(4) Uani 1 1 d . . . O18 O 1.1614(2) 0.83738(16) 0.18174(13) 0.0170(5) Uani 1 1 d . . . O19 O 0.6011(3) 1.0587(3) -0.06712(18) 0.0487(10) Uani 1 1 d . . . O20 O 0.6520(4) 1.1678(2) -0.02536(18) 0.0524(10) Uani 1 1 d . . . O21 O 0.4132(3) 0.80249(16) 0.29055(14) 0.0182(5) Uani 1 1 d . . . O22 O 0.6460(2) 0.82628(15) 0.26712(14) 0.0161(5) Uani 1 1 d . . . O23 O 0.1705(4) 1.2640(2) 0.1724(3) 0.0697(14) Uani 1 1 d . . . O24 O 0.3905(4) 1.2827(2) 0.1210(2) 0.0524(10) Uani 1 1 d . . . O25 O 0.6144(2) 0.70198(16) 0.42176(14) 0.0170(5) Uani 1 1 d . . . O26 O 1.2108(3) 0.62252(17) 0.19596(14) 0.0190(5) Uani 1 1 d . . . O27 O 1.3121(3) 0.67640(16) 0.41368(13) 0.0174(5) Uani 1 1 d . . . O28 O 1.4336(2) 0.71951(17) 0.16692(14) 0.0187(5) Uani 1 1 d . . . O30 O 0.3465(3) 0.50446(19) 0.48947(17) 0.0329(7) Uani 1 1 d . . . Tb1 Tb 0.798368(16) 0.688702(10) 0.311421(8) 0.01142(4) Uani 1 1 d . . . Tb2 Tb 1.252188(15) 0.711356(9) 0.280926(8) 0.01086(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0109(14) 0.0139(15) 0.0162(15) -0.0005(12) -0.0017(12) -0.0042(12) C2 0.0143(15) 0.0148(15) 0.0154(15) -0.0035(12) -0.0006(12) -0.0043(12) C3 0.0182(16) 0.0191(16) 0.0179(16) -0.0049(13) -0.0028(13) -0.0008(13) C4 0.0199(17) 0.0243(18) 0.0190(17) -0.0052(14) -0.0041(13) -0.0057(14) C5 0.0227(17) 0.0206(17) 0.0133(16) -0.0064(13) 0.0015(13) -0.0070(14) C6 0.0183(16) 0.0161(16) 0.0198(17) -0.0037(13) 0.0017(13) -0.0032(13) C7 0.0126(15) 0.0183(16) 0.0194(16) -0.0038(13) -0.0009(12) -0.0028(12) C8 0.0139(15) 0.0134(15) 0.0132(15) -0.0037(12) -0.0047(12) 0.0003(12) C9 0.0123(15) 0.0131(15) 0.0223(17) -0.0042(13) -0.0061(12) -0.0002(12) C10 0.033(2) 0.0162(16) 0.0151(16) -0.0033(13) 0.0007(14) -0.0038(14) C11 0.047(2) 0.0136(17) 0.0165(17) 0.0002(13) -0.0049(16) -0.0029(16) C12 0.0252(18) 0.0136(16) 0.029(2) -0.0069(14) -0.0114(15) 0.0033(14) C13 0.0185(19) 0.0201(19) 0.066(3) -0.016(2) 0.0140(19) -0.0025(15) C14 0.0220(19) 0.0156(17) 0.057(3) -0.0117(18) 0.0154(18) -0.0057(15) C15 0.0153(15) 0.0094(14) 0.0125(15) -0.0004(11) 0.0027(12) -0.0032(11) C16 0.0110(14) 0.0116(14) 0.0173(16) -0.0025(12) 0.0014(12) -0.0011(11) C17 0.0129(15) 0.0153(15) 0.0209(17) -0.0035(13) -0.0003(12) -0.0040(12) C18 0.0193(17) 0.0216(17) 0.0253(19) -0.0096(15) 0.0040(14) -0.0067(14) C19 0.0247(19) 0.0134(16) 0.029(2) -0.0067(14) 0.0127(15) -0.0017(14) C20 0.0206(17) 0.0171(17) 0.0260(19) 0.0005(14) 0.0008(14) 0.0050(14) C21 0.0174(16) 0.0203(17) 0.0199(17) -0.0027(14) -0.0038(13) 0.0021(13) C22 0.0136(15) 0.0152(15) 0.0138(15) -0.0049(12) -0.0041(12) 0.0004(12) C23 0.0168(16) 0.0143(15) 0.0159(16) -0.0049(12) -0.0029(12) 0.0037(12) C24 0.0247(18) 0.0197(17) 0.0223(18) -0.0075(14) -0.0037(14) -0.0030(14) C25 0.043(2) 0.0157(17) 0.0224(19) -0.0077(14) -0.0042(16) -0.0030(16) C26 0.044(2) 0.0175(17) 0.0195(18) -0.0089(14) -0.0031(16) 0.0097(16) C27 0.028(2) 0.029(2) 0.029(2) -0.0113(17) -0.0039(16) 0.0126(16) C28 0.0198(18) 0.0206(17) 0.0284(19) -0.0086(15) -0.0049(14) 0.0046(14) C29 0.0116(14) 0.0156(15) 0.0137(15) -0.0036(12) -0.0015(12) 0.0010(12) C30 0.0087(14) 0.0192(16) 0.0108(14) -0.0018(12) -0.0001(11) 0.0009(12) C31 0.0180(16) 0.0175(16) 0.0166(16) -0.0030(13) -0.0006(13) 0.0024(13) C32 0.0286(19) 0.0168(16) 0.0145(16) -0.0004(13) 0.0021(14) 0.0063(14) C33 0.0141(16) 0.035(2) 0.0142(16) 0.0058(15) 0.0003(13) 0.0073(15) C34 0.0162(17) 0.041(2) 0.0198(18) 0.0037(16) -0.0068(14) -0.0080(16) C35 0.0176(17) 0.0222(18) 0.0208(18) 0.0012(14) -0.0042(13) -0.0035(14) C36 0.0144(15) 0.0125(15) 0.0143(15) -0.0042(12) -0.0040(12) -0.0009(12) C37 0.0162(15) 0.0116(14) 0.0158(15) -0.0037(12) -0.0042(12) 0.0008(12) C38 0.0173(16) 0.0162(16) 0.0214(17) -0.0038(13) -0.0003(13) -0.0006(13) C39 0.0270(19) 0.0142(16) 0.0276(19) -0.0001(14) -0.0047(15) -0.0050(14) C40 0.031(2) 0.0115(16) 0.038(2) -0.0020(15) -0.0198(17) 0.0038(14) C41 0.0174(18) 0.0188(18) 0.049(3) -0.0058(17) -0.0143(17) 0.0041(14) C42 0.0151(16) 0.0147(16) 0.034(2) -0.0044(14) -0.0071(14) 0.0008(13) N1 0.0318(18) 0.0273(17) 0.0168(15) -0.0095(13) 0.0028(13) -0.0114(14) N2 0.0366(19) 0.0172(15) 0.0299(18) -0.0095(14) -0.0164(15) 0.0065(14) N3 0.0300(18) 0.0184(16) 0.041(2) -0.0115(15) 0.0140(15) -0.0032(14) N4 0.070(3) 0.0232(18) 0.0266(19) -0.0133(15) -0.0049(18) 0.0131(19) N5 0.0193(16) 0.049(2) 0.0206(17) 0.0126(16) 0.0022(13) 0.0096(15) N6 0.043(2) 0.0149(16) 0.064(3) 0.0004(17) -0.032(2) 0.0005(15) O1 0.0142(11) 0.0152(11) 0.0217(12) -0.0074(9) -0.0062(9) 0.0011(9) O2 0.0095(10) 0.0167(11) 0.0192(12) -0.0065(9) -0.0028(9) 0.0003(9) O3 0.0292(15) 0.0508(19) 0.0324(16) -0.0245(15) -0.0034(12) -0.0096(14) O4 0.0344(16) 0.0306(15) 0.0332(16) -0.0198(13) -0.0004(12) -0.0036(12) O5 0.0137(11) 0.0146(11) 0.0193(12) -0.0019(9) -0.0026(9) 0.0005(9) O6 0.0193(12) 0.0113(11) 0.0221(13) -0.0051(9) 0.0034(10) -0.0041(9) O7 0.074(2) 0.0120(13) 0.0397(18) -0.0022(13) -0.0063(17) -0.0011(14) O8 0.0368(17) 0.0239(15) 0.054(2) -0.0175(14) -0.0074(15) 0.0085(13) O9 0.0156(11) 0.0142(11) 0.0225(12) -0.0055(10) -0.0064(9) 0.0041(9) O10 0.0191(12) 0.0200(12) 0.0265(13) -0.0113(10) -0.0011(10) -0.0063(10) O11 0.0443(19) 0.0338(17) 0.052(2) -0.0296(16) 0.0091(15) -0.0058(14) O12 0.058(2) 0.0219(15) 0.056(2) -0.0067(15) 0.0122(18) 0.0136(15) O13 0.0159(11) 0.0174(11) 0.0176(12) -0.0063(9) 0.0001(9) -0.0046(9) O14 0.0112(11) 0.0159(11) 0.0247(13) -0.0092(10) -0.0030(9) 0.0019(9) O15 0.059(2) 0.055(2) 0.068(3) -0.043(2) -0.009(2) 0.0294(19) O16 0.086(3) 0.0219(15) 0.0348(18) -0.0156(14) 0.0017(17) 0.0000(17) O17 0.0136(11) 0.0125(10) 0.0137(11) -0.0015(9) -0.0022(8) -0.0009(8) O18 0.0119(11) 0.0177(11) 0.0200(12) -0.0012(9) -0.0055(9) -0.0002(9) O19 0.0255(16) 0.074(2) 0.0322(17) 0.0225(17) -0.0146(14) -0.0109(16) O20 0.061(2) 0.044(2) 0.0277(17) 0.0040(15) -0.0056(15) 0.0312(17) O21 0.0145(11) 0.0140(11) 0.0258(13) -0.0017(10) -0.0052(10) -0.0035(9) O22 0.0120(11) 0.0127(11) 0.0212(12) -0.0018(9) -0.0022(9) 0.0011(9) O23 0.042(2) 0.0231(17) 0.136(4) -0.005(2) -0.033(2) 0.0131(15) O24 0.061(2) 0.0163(15) 0.074(3) 0.0106(16) -0.028(2) -0.0046(15) O25 0.0117(11) 0.0189(12) 0.0204(12) -0.0077(10) 0.0017(9) -0.0012(9) O26 0.0121(11) 0.0240(13) 0.0229(13) -0.0094(10) -0.0034(9) -0.0019(9) O27 0.0183(12) 0.0154(11) 0.0164(12) -0.0027(9) -0.0007(9) -0.0005(9) O28 0.0108(11) 0.0226(12) 0.0187(12) 0.0004(10) -0.0014(9) -0.0002(9) O30 0.0360(16) 0.0217(14) 0.0343(16) 0.0084(12) -0.0037(13) -0.0083(12) Tb1 0.01007(7) 0.00910(7) 0.01483(8) -0.00315(6) -0.00252(5) 0.00031(5) Tb2 0.00867(7) 0.00889(7) 0.01429(8) -0.00227(6) -0.00219(5) 0.00036(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 C1 O2 1.264(4) . ? C1 O1 1.264(4) . ? C1 C2 1.501(5) . ? C2 C7 1.390(5) . ? C2 C3 1.394(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.380(5) . ? C5 N1 1.470(4) . ? C6 C7 1.386(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O6 1.256(4) . ? C8 O5 1.257(4) . ? C8 C9 1.505(4) . ? C9 C14 1.380(5) . ? C9 C10 1.385(5) . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 C13 1.365(6) . ? C12 N2 1.479(4) . ? C13 C14 1.391(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 O9 1.251(4) . ? C15 O10 1.254(4) . ? C15 C16 1.502(4) . ? C16 C21 1.394(5) . ? C16 C17 1.401(5) . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.382(5) . ? C18 H18 0.9500 . ? C19 C20 1.381(6) . ? C19 N3 1.482(5) . ? C20 C21 1.390(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O14 1.251(4) . ? C22 O13 1.259(4) . ? C22 C23 1.507(4) . ? C23 C24 1.385(5) . ? C23 C28 1.392(5) . ? C24 C25 1.383(5) . ? C24 H24 0.9500 . ? C25 C26 1.391(6) . ? C25 H25 0.9500 . ? C26 C27 1.385(6) . ? C26 N4 1.475(5) . ? C27 C28 1.377(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 O18 1.256(4) . ? C29 O17 1.266(4) . ? C29 C30 1.496(4) . ? C30 C31 1.392(5) . ? C30 C35 1.395(5) . ? C31 C32 1.390(5) . ? C31 H31 0.9500 . ? C32 C33 1.386(6) . ? C32 H32 0.9500 . ? C33 C34 1.381(6) . ? C33 N5 1.471(5) . ? C34 C35 1.383(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 O21 1.256(4) . ? C36 O22 1.263(4) . ? C36 C37 1.506(4) . ? C37 C38 1.389(5) . ? C37 C42 1.390(5) . ? C38 C39 1.381(5) . ? C38 H38 0.9500 . ? C39 C40 1.387(5) . ? C39 H39 0.9500 . ? C40 C41 1.382(6) . ? C40 N6 1.477(5) . ? C41 C42 1.388(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? N1 O4 1.226(4) . ? N1 O3 1.231(4) . ? N2 O7 1.210(5) . ? N2 O8 1.229(5) . ? N3 O11 1.215(5) . ? N3 O12 1.217(5) . ? N4 O16 1.224(5) . ? N4 O15 1.234(6) . ? N5 O19 1.224(5) . ? N5 O20 1.229(5) . ? N6 O24 1.214(5) . ? N6 O23 1.232(5) . ? O1 Tb1 2.523(2) . ? O2 Tb1 2.507(2) . ? O5 Tb1 2.428(2) . ? O6 Tb2 2.349(2) . ? O6 Tb1 2.893(3) . ? O9 Tb2 2.318(2) . ? O10 Tb1 2.323(2) 1_655 ? O13 Tb1 2.283(2) . ? O14 Tb2 2.403(2) . ? O17 Tb1 2.352(2) . ? O17 Tb2 2.778(2) . ? O18 Tb2 2.405(2) . ? O21 Tb2 2.299(2) 1_455 ? O22 Tb1 2.319(2) . ? O25 Tb1 2.464(2) . ? O26 Tb2 2.432(2) . ? O27 Tb2 2.482(2) . ? O28 Tb2 2.472(2) . ? Tb1 O10 2.323(2) 1_455 ? Tb2 O21 2.299(2) 1_655 ? 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 O2 C1 O1 121.2(3) . . ? O2 C1 C2 119.4(3) . . ? O1 C1 C2 119.4(3) . . ? C7 C2 C3 120.0(3) . . ? C7 C2 C1 119.9(3) . . ? C3 C2 C1 120.0(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 117.7(3) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C6 C5 C4 123.4(3) . . ? C6 C5 N1 118.6(3) . . ? C4 C5 N1 118.0(3) . . ? C5 C6 C7 117.8(3) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C2 120.7(3) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O6 C8 O5 121.6(3) . . ? O6 C8 C9 119.9(3) . . ? O5 C8 C9 118.2(3) . . ? C14 C9 C10 120.2(3) . . ? C14 C9 C8 118.5(3) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.2(3) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 C12 C11 122.5(3) . . ? C13 C12 N2 118.6(3) . . ? C11 C12 N2 118.9(3) . . ? C12 C13 C14 118.8(4) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C9 C14 C13 120.0(4) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O9 C15 O10 124.8(3) . . ? O9 C15 C16 116.9(3) . . ? O10 C15 C16 118.3(3) . . ? C21 C16 C17 120.2(3) . . ? C21 C16 C15 120.2(3) . . ? C17 C16 C15 119.5(3) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 117.8(3) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C20 C19 C18 123.5(3) . . ? C20 C19 N3 119.0(4) . . ? C18 C19 N3 117.5(4) . . ? C19 C20 C21 118.2(3) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C16 119.8(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? O14 C22 O13 125.5(3) . . ? O14 C22 C23 118.6(3) . . ? O13 C22 C23 115.8(3) . . ? C24 C23 C28 120.1(3) . . ? C24 C23 C22 120.9(3) . . ? C28 C23 C22 119.0(3) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 118.0(4) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C27 C26 C25 122.9(3) . . ? C27 C26 N4 118.6(4) . . ? C25 C26 N4 118.5(4) . . ? C28 C27 C26 117.8(4) . . ? C28 C27 H27 121.1 . . ? C26 C27 H27 121.1 . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? O18 C29 O17 121.5(3) . . ? O18 C29 C30 118.9(3) . . ? O17 C29 C30 119.5(3) . . ? C31 C30 C35 120.7(3) . . ? C31 C30 C29 119.6(3) . . ? C35 C30 C29 119.7(3) . . ? C32 C31 C30 120.0(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 118.0(3) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C34 C33 C32 123.0(3) . . ? C34 C33 N5 117.8(4) . . ? C32 C33 N5 119.2(4) . . ? C33 C34 C35 118.6(4) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? C34 C35 C30 119.7(3) . . ? C34 C35 H35 120.2 . . ? C30 C35 H35 120.2 . . ? O21 C36 O22 123.9(3) . . ? O21 C36 C37 118.3(3) . . ? O22 C36 C37 117.8(3) . . ? C38 C37 C42 120.5(3) . . ? C38 C37 C36 120.1(3) . . ? C42 C37 C36 119.4(3) . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 117.9(3) . . ? C38 C39 H39 121.1 . . ? C40 C39 H39 121.1 . . ? C41 C40 C39 123.4(3) . . ? C41 C40 N6 118.3(4) . . ? C39 C40 N6 118.3(4) . . ? C40 C41 C42 117.7(3) . . ? C40 C41 H41 121.2 . . ? C42 C41 H41 121.2 . . ? C41 C42 C37 120.2(3) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? O4 N1 O3 123.4(3) . . ? O4 N1 C5 118.7(3) . . ? O3 N1 C5 117.9(3) . . ? O7 N2 O8 124.1(3) . . ? O7 N2 C12 119.0(3) . . ? O8 N2 C12 116.9(3) . . ? O11 N3 O12 124.8(4) . . ? O11 N3 C19 117.7(4) . . ? O12 N3 C19 117.5(4) . . ? O16 N4 O15 124.4(4) . . ? O16 N4 C26 117.6(4) . . ? O15 N4 C26 118.0(4) . . ? O19 N5 O20 124.3(4) . . ? O19 N5 C33 118.9(4) . . ? O20 N5 C33 116.8(4) . . ? O24 N6 O23 123.8(4) . . ? O24 N6 C40 118.8(4) . . ? O23 N6 C40 117.4(4) . . ? C1 O1 Tb1 92.74(19) . . ? C1 O2 Tb1 93.51(19) . . ? C8 O5 Tb1 101.5(2) . . ? C8 O6 Tb2 172.4(2) . . ? C8 O6 Tb1 80.07(18) . . ? Tb2 O6 Tb1 107.29(9) . . ? C15 O9 Tb2 144.6(2) . . ? C15 O10 Tb1 144.4(2) . 1_655 ? C22 O13 Tb1 139.7(2) . . ? C22 O14 Tb2 134.5(2) . . ? C29 O17 Tb1 157.8(2) . . ? C29 O17 Tb2 85.45(18) . . ? Tb1 O17 Tb2 110.96(9) . . ? C29 O18 Tb2 103.4(2) . . ? C36 O21 Tb2 155.9(2) . 1_455 ? C36 O22 Tb1 135.7(2) . . ? O13 Tb1 O22 81.05(9) . . ? O13 Tb1 O10 136.13(9) . 1_455 ? O22 Tb1 O10 103.78(9) . 1_455 ? O13 Tb1 O17 75.07(8) . . ? O22 Tb1 O17 81.49(8) . . ? O10 Tb1 O17 148.61(8) 1_455 . ? O13 Tb1 O5 86.56(8) . . ? O22 Tb1 O5 155.53(8) . . ? O10 Tb1 O5 71.28(9) 1_455 . ? O17 Tb1 O5 115.62(8) . . ? O13 Tb1 O25 71.91(8) . . ? O22 Tb1 O25 77.77(9) . . ? O10 Tb1 O25 66.88(8) 1_455 . ? O17 Tb1 O25 143.18(8) . . ? O5 Tb1 O25 78.35(8) . . ? O13 Tb1 O2 134.96(8) . . ? O22 Tb1 O2 124.28(8) . . ? O10 Tb1 O2 78.40(8) 1_455 . ? O17 Tb1 O2 73.45(8) . . ? O5 Tb1 O2 79.02(8) . . ? O25 Tb1 O2 143.09(8) . . ? O13 Tb1 O1 147.76(8) . . ? O22 Tb1 O1 75.41(8) . . ? O10 Tb1 O1 71.88(9) 1_455 . ? O17 Tb1 O1 79.88(8) . . ? O5 Tb1 O1 122.96(8) . . ? O25 Tb1 O1 122.73(8) . . ? O2 Tb1 O1 51.93(8) . . ? O13 Tb1 O6 72.79(8) . . ? O22 Tb1 O6 143.71(7) . . ? O10 Tb1 O6 112.51(8) 1_455 . ? O17 Tb1 O6 67.91(7) . . ? O5 Tb1 O6 47.73(7) . . ? O25 Tb1 O6 115.80(8) . . ? O2 Tb1 O6 65.94(7) . . ? O1 Tb1 O6 115.78(8) . . ? O21 Tb2 O9 94.11(8) 1_655 . ? O21 Tb2 O6 146.83(9) 1_655 . ? O9 Tb2 O6 80.89(9) . . ? O21 Tb2 O14 77.95(8) 1_655 . ? O9 Tb2 O14 144.44(8) . . ? O6 Tb2 O14 87.22(8) . . ? O21 Tb2 O18 84.84(8) 1_655 . ? O9 Tb2 O18 140.18(9) . . ? O6 Tb2 O18 119.65(8) . . ? O14 Tb2 O18 74.28(9) . . ? O21 Tb2 O26 139.70(9) 1_655 . ? O9 Tb2 O26 72.85(8) . . ? O6 Tb2 O26 70.19(8) . . ? O14 Tb2 O26 133.57(8) . . ? O18 Tb2 O26 82.45(8) . . ? O21 Tb2 O28 72.85(9) 1_655 . ? O9 Tb2 O28 71.44(9) . . ? O6 Tb2 O28 133.93(8) . . ? O14 Tb2 O28 135.43(8) . . ? O18 Tb2 O28 70.28(8) . . ? O26 Tb2 O28 66.85(8) . . ? O21 Tb2 O27 70.50(9) 1_655 . ? O9 Tb2 O27 73.02(9) . . ? O6 Tb2 O27 76.72(9) . . ? O14 Tb2 O27 71.65(8) . . ? O18 Tb2 O27 141.22(8) . . ? O26 Tb2 O27 135.34(8) . . ? O28 Tb2 O27 125.91(8) . . ? O21 Tb2 O17 128.61(8) 1_655 . ? O9 Tb2 O17 135.17(8) . . ? O6 Tb2 O17 70.06(8) . . ? O14 Tb2 O17 68.69(8) . . ? O18 Tb2 O17 49.62(7) . . ? O26 Tb2 O17 65.61(8) . . ? O28 Tb2 O17 105.32(7) . . ? O27 Tb2 O17 128.59(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.785 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.128 # Attachment 'CCDC606245.cif' data_pbar1-apr162006-trial1 _database_code_depnum_ccdc_archive 'CCDC 606245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 Eu2 N6 O28' _chemical_formula_weight 1424.73 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.385(3) _cell_length_b 12.912(3) _cell_length_c 17.889(4) _cell_angle_alpha 97.49(3) _cell_angle_beta 109.64(3) _cell_angle_gamma 101.99(3) _cell_volume 2572.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 2812 _cell_measurement_theta_min 2.4615 _cell_measurement_theta_max 22.2645 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7869 _exptl_absorpt_correction_T_max 0.9514 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(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 CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 27369 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11779 _reflns_number_gt 8478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0619P)^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_number_reflns 11779 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 C1 C 0.8711(6) 0.6414(5) 0.4696(4) 0.0113(13) Uani 1 1 d . . . C2 C 0.8092(6) 0.7306(6) 0.4567(4) 0.0150(14) Uani 1 1 d . . . C3 C 0.6897(6) 0.7170(6) 0.4430(4) 0.0190(16) Uani 1 1 d . . . C4 C 0.6375(7) 0.8022(7) 0.4378(4) 0.0227(17) Uani 1 1 d . . . H4 H 0.5555 0.7903 0.4292 0.027 Uiso 1 1 calc R . . C5 C 0.7059(8) 0.9036(7) 0.4452(5) 0.0285(19) Uani 1 1 d . . . H5 H 0.6709 0.9625 0.4411 0.034 Uiso 1 1 calc R . . C6 C 0.8267(7) 0.9212(6) 0.4589(5) 0.0231(17) Uani 1 1 d . . . H6 H 0.8739 0.9918 0.4637 0.028 Uiso 1 1 calc R . . C7 C 0.8774(7) 0.8341(6) 0.4652(4) 0.0172(15) Uani 1 1 d . . . H7 H 0.9600 0.8461 0.4756 0.021 Uiso 1 1 calc R . . C8 C 1.1505(6) 0.7771(5) 0.3945(4) 0.0125(14) Uani 1 1 d . . . C9 C 1.1494(6) 0.8817(5) 0.3654(4) 0.0128(14) Uani 1 1 d . . . C10 C 1.0408(6) 0.9064(6) 0.3389(4) 0.0168(15) Uani 1 1 d . . . H10 H 0.9710 0.8551 0.3352 0.020 Uiso 1 1 calc R . . C11 C 1.0327(7) 1.0056(6) 0.3176(5) 0.0229(17) Uani 1 1 d . . . H11 H 0.9579 1.0217 0.3002 0.027 Uiso 1 1 calc R . . C12 C 1.1324(7) 1.0796(6) 0.3218(5) 0.0244(18) Uani 1 1 d . . . H12 H 1.1266 1.1470 0.3073 0.029 Uiso 1 1 calc R . . C13 C 1.2430(7) 1.0561(6) 0.3475(5) 0.0237(17) Uani 1 1 d . . . H13 H 1.3126 1.1063 0.3499 0.028 Uiso 1 1 calc R . . C14 C 1.2479(6) 0.9584(6) 0.3692(4) 0.0166(15) Uani 1 1 d . . . C15 C 0.8671(6) 0.3871(6) 0.3567(4) 0.0141(14) Uani 1 1 d . . . C16 C 0.7511(6) 0.3187(6) 0.2931(4) 0.0164(15) Uani 1 1 d . . . C17 C 0.7097(7) 0.2069(6) 0.2764(4) 0.0181(15) Uani 1 1 d . . . C18 C 0.5983(7) 0.1511(6) 0.2213(5) 0.0246(17) Uani 1 1 d . . . H18 H 0.5736 0.0741 0.2108 0.030 Uiso 1 1 calc R . . C19 C 0.5227(7) 0.2080(7) 0.1816(5) 0.0267(18) Uani 1 1 d . . . H19 H 0.4450 0.1700 0.1438 0.032 Uiso 1 1 calc R . . C20 C 0.5590(7) 0.3204(7) 0.1962(5) 0.0221(17) Uani 1 1 d . . . H20 H 0.5064 0.3596 0.1693 0.026 Uiso 1 1 calc R . . C21 C 0.6738(7) 0.3752(6) 0.2511(4) 0.0211(16) Uani 1 1 d . . . H21 H 0.6998 0.4519 0.2601 0.025 Uiso 1 1 calc R . . C22 C 1.4144(7) 0.7151(7) 0.5663(5) 0.0258(18) Uani 1 1 d . . . H22A H 1.3736 0.7578 0.5911 0.039 Uiso 1 1 calc R . . H22B H 1.4620 0.7615 0.5431 0.039 Uiso 1 1 calc R . . H22C H 1.4667 0.6861 0.6078 0.039 Uiso 1 1 calc R . . C23 C 1.2383(8) 0.4115(7) 0.3315(5) 0.030(2) Uani 1 1 d . . . H23A H 1.2349 0.3715 0.3740 0.045 Uiso 1 1 calc R . . H23B H 1.3206 0.4336 0.3346 0.045 Uiso 1 1 calc R . . H23C H 1.1876 0.3648 0.2780 0.045 Uiso 1 1 calc R . . C24 C 0.6924(6) 0.3471(5) 0.0308(4) 0.0134(14) Uani 1 1 d . . . C25 C 0.5625(6) 0.2923(6) -0.0008(4) 0.0122(13) Uani 1 1 d . . . C26 C 0.4826(7) 0.3544(6) -0.0026(4) 0.0184(15) Uani 1 1 d . . . H26 H 0.5122 0.4289 0.0237 0.022 Uiso 1 1 calc R . . C27 C 0.3608(7) 0.3098(6) -0.0421(5) 0.0211(16) Uani 1 1 d . . . H27 H 0.3075 0.3534 -0.0427 0.025 Uiso 1 1 calc R . . C28 C 0.3177(7) 0.2017(6) -0.0805(5) 0.0217(17) Uani 1 1 d . . . H28 H 0.2346 0.1716 -0.1096 0.026 Uiso 1 1 calc R . . C29 C 0.3933(6) 0.1368(6) -0.0771(5) 0.0203(16) Uani 1 1 d . . . H29 H 0.3633 0.0620 -0.1026 0.024 Uiso 1 1 calc R . . C30 C 0.5126(6) 0.1823(6) -0.0364(4) 0.0143(14) Uani 1 1 d . . . C31 C 1.0678(6) 0.3074(6) 0.0003(4) 0.0127(14) Uani 1 1 d . . . C32 C 1.0938(6) 0.1973(5) -0.0075(4) 0.0131(14) Uani 1 1 d . . . C33 C 1.0393(6) 0.1233(5) -0.0815(4) 0.0148(14) Uani 1 1 d . . . H33 H 0.9895 0.1433 -0.1274 0.018 Uiso 1 1 calc R . . C34 C 1.0569(6) 0.0194(6) -0.0893(4) 0.0160(15) Uani 1 1 d . . . H34 H 1.0195 -0.0299 -0.1407 0.019 Uiso 1 1 calc R . . C35 C 1.1280(7) -0.0126(6) -0.0234(5) 0.0191(16) Uani 1 1 d . . . H35 H 1.1396 -0.0832 -0.0297 0.023 Uiso 1 1 calc R . . C36 C 1.1820(6) 0.0582(6) 0.0514(5) 0.0151(15) Uani 1 1 d . . . H36 H 1.2305 0.0377 0.0976 0.018 Uiso 1 1 calc R . . C37 C 1.1627(6) 0.1607(5) 0.0568(4) 0.0141(14) Uani 1 1 d . . . C38 C 1.1837(6) 0.5810(6) 0.1382(4) 0.0145(14) Uani 1 1 d . . . C39 C 1.3132(6) 0.6398(6) 0.1678(4) 0.0136(14) Uani 1 1 d . . . C40 C 1.3939(7) 0.5792(7) 0.1678(5) 0.0254(18) Uani 1 1 d . . . H40 H 1.3665 0.5032 0.1464 0.030 Uiso 1 1 calc R . . C41 C 1.5150(7) 0.6311(7) 0.1993(5) 0.0266(18) Uani 1 1 d . . . H41 H 1.5693 0.5890 0.1990 0.032 Uiso 1 1 calc R . . C42 C 1.5591(7) 0.7399(7) 0.2307(5) 0.0277(19) Uani 1 1 d . . . H42 H 1.6425 0.7727 0.2526 0.033 Uiso 1 1 calc R . . C43 C 1.4796(7) 0.8020(7) 0.2301(5) 0.0260(18) Uani 1 1 d . . . H43 H 1.5075 0.8782 0.2509 0.031 Uiso 1 1 calc R . . C44 C 1.3604(7) 0.7510(6) 0.1987(4) 0.0190(16) Uani 1 1 d . . . C45 C 0.8476(7) 0.6325(6) 0.2134(5) 0.0208(16) Uani 1 1 d . . . H45A H 0.8604 0.7045 0.2006 0.031 Uiso 1 1 calc R . . H45B H 0.8544 0.6397 0.2701 0.031 Uiso 1 1 calc R . . H45C H 0.7680 0.5876 0.1775 0.031 Uiso 1 1 calc R . . C46 C 0.9310(7) 0.2512(5) 0.1838(5) 0.0192(16) Uani 1 1 d . . . H46A H 0.8472 0.2095 0.1579 0.029 Uiso 1 1 calc R . . H46B H 0.9639 0.2403 0.2393 0.029 Uiso 1 1 calc R . . H46C H 0.9759 0.2265 0.1525 0.029 Uiso 1 1 calc R . . Eu1 Eu 1.11215(3) 0.57421(3) 0.43974(2) 0.01035(9) Uani 1 1 d . . . Eu2 Eu 0.93106(3) 0.46475(3) 0.08113(2) 0.00967(9) Uani 1 1 d . . . N1 N 0.6108(6) 0.6069(6) 0.4252(4) 0.0259(15) Uani 1 1 d . . . N2 N 1.3651(6) 0.9346(5) 0.3935(4) 0.0226(14) Uani 1 1 d . . . N3 N 0.7896(6) 0.1433(5) 0.3168(4) 0.0252(15) Uani 1 1 d . . . N4 N 0.5892(6) 0.1077(5) -0.0266(4) 0.0209(14) Uani 1 1 d . . . N5 N 1.2247(5) 0.2358(5) 0.1373(4) 0.0185(13) Uani 1 1 d . . . N6 N 1.2766(7) 0.8204(5) 0.1969(4) 0.0260(15) Uani 1 1 d . . . O1 O 0.9401(4) 0.6340(4) 0.4322(3) 0.0160(10) Uani 1 1 d . . . O2 O 0.5330(6) 0.5949(6) 0.4533(5) 0.058(2) Uani 1 1 d . . . O3 O 0.6236(5) 0.5343(4) 0.3805(3) 0.0251(12) Uani 1 1 d . . . O4 O 1.1111(4) 0.6880(4) 0.3414(3) 0.0160(10) Uani 1 1 d . . . O5 O 1.1806(4) 0.7786(4) 0.4688(3) 0.0157(10) Uani 1 1 d . . . O6 O 1.3653(5) 0.8393(4) 0.3948(3) 0.0257(12) Uani 1 1 d . . . O7 O 1.4532(5) 1.0093(5) 0.4112(4) 0.0377(16) Uani 1 1 d . . . O8 O 0.9465(4) 0.4369(4) 0.3342(3) 0.0160(10) Uani 1 1 d . . . O9 O 0.7479(6) 0.0451(5) 0.3065(5) 0.0490(19) Uani 1 1 d . . . O10 O 0.8942(5) 0.1903(4) 0.3559(3) 0.0234(12) Uani 1 1 d . . . O11 O 1.1219(5) 0.6041(4) 0.5707(3) 0.0198(11) Uani 1 1 d . . . O12 O 1.3292(5) 0.6283(5) 0.5040(4) 0.0387(16) Uani 1 1 d . . . O13 O 1.1966(4) 0.5065(4) 0.3430(3) 0.0157(10) Uani 1 1 d . . . O14 O 1.1500(4) 0.4159(4) 0.4823(3) 0.0174(11) Uani 1 1 d . . . O15 O 0.7266(4) 0.4467(4) 0.0651(3) 0.0158(10) Uani 1 1 d . . . O16 O 0.7638(4) 0.2959(4) 0.0191(3) 0.0151(10) Uani 1 1 d . . . O17 O 0.6413(5) 0.0992(4) 0.0434(3) 0.0259(12) Uani 1 1 d . . . O18 O 0.5927(5) 0.0560(5) -0.0876(3) 0.0321(14) Uani 1 1 d . . . O19 O 1.0230(4) 0.3292(4) 0.0509(3) 0.0143(10) Uani 1 1 d . . . O20 O 1.2687(5) 0.3309(4) 0.1410(3) 0.0226(12) Uani 1 1 d . . . O21 O 1.2332(5) 0.1973(4) 0.1978(3) 0.0271(13) Uani 1 1 d . . . O22 O 1.1219(4) 0.5590(4) 0.0625(3) 0.0133(10) Uani 1 1 d . . . O23 O 1.1405(4) 0.5455(4) 0.1870(3) 0.0175(11) Uani 1 1 d . . . O24 O 1.1716(5) 0.7737(5) 0.1732(4) 0.0324(14) Uani 1 1 d . . . O25 O 1.3190(6) 0.9168(5) 0.2196(4) 0.0380(16) Uani 1 1 d . . . O26 O 0.9095(4) 0.6360(4) 0.0475(3) 0.0175(11) Uani 1 1 d . . . O27 O 0.9348(4) 0.5827(4) 0.2017(3) 0.0158(10) Uani 1 1 d . . . O28 O 0.9397(4) 0.3635(4) 0.1861(3) 0.0151(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 C1 0.008(3) 0.011(3) 0.008(3) -0.002(3) -0.004(3) 0.001(3) C2 0.017(4) 0.018(4) 0.010(3) 0.002(3) 0.005(3) 0.005(3) C3 0.018(4) 0.029(4) 0.012(3) 0.003(3) 0.005(3) 0.011(3) C4 0.025(4) 0.036(5) 0.016(4) 0.007(3) 0.011(3) 0.020(4) C5 0.039(5) 0.028(5) 0.024(4) 0.006(4) 0.010(4) 0.024(4) C6 0.037(5) 0.010(4) 0.022(4) 0.002(3) 0.009(4) 0.009(3) C7 0.022(4) 0.013(4) 0.016(4) 0.005(3) 0.003(3) 0.009(3) C8 0.011(3) 0.011(3) 0.016(4) 0.003(3) 0.005(3) 0.003(3) C9 0.026(4) 0.009(3) 0.010(3) 0.006(3) 0.010(3) 0.010(3) C10 0.019(4) 0.017(4) 0.018(4) 0.006(3) 0.008(3) 0.009(3) C11 0.029(4) 0.018(4) 0.028(4) 0.006(3) 0.011(4) 0.018(3) C12 0.042(5) 0.018(4) 0.022(4) 0.015(3) 0.013(4) 0.020(4) C13 0.031(4) 0.018(4) 0.025(4) 0.006(3) 0.015(4) 0.004(3) C14 0.017(4) 0.016(4) 0.016(4) 0.002(3) 0.006(3) 0.003(3) C15 0.020(4) 0.013(3) 0.011(3) 0.002(3) 0.006(3) 0.007(3) C16 0.019(4) 0.018(4) 0.016(4) 0.000(3) 0.012(3) 0.005(3) C17 0.019(4) 0.015(4) 0.020(4) 0.001(3) 0.009(3) 0.002(3) C18 0.028(4) 0.015(4) 0.029(5) -0.002(3) 0.012(4) 0.004(3) C19 0.014(4) 0.029(5) 0.030(5) 0.000(4) 0.004(4) 0.004(3) C20 0.019(4) 0.030(4) 0.018(4) 0.006(3) 0.004(3) 0.013(3) C21 0.025(4) 0.020(4) 0.018(4) 0.008(3) 0.004(3) 0.010(3) C22 0.019(4) 0.032(5) 0.022(4) 0.000(4) 0.007(3) 0.003(3) C23 0.052(6) 0.026(4) 0.029(5) 0.012(4) 0.025(4) 0.027(4) C24 0.019(4) 0.012(3) 0.009(3) 0.006(3) 0.004(3) 0.005(3) C25 0.011(3) 0.015(3) 0.011(3) 0.004(3) 0.004(3) 0.003(3) C26 0.025(4) 0.014(4) 0.022(4) 0.004(3) 0.013(3) 0.008(3) C27 0.022(4) 0.021(4) 0.022(4) 0.008(3) 0.005(3) 0.012(3) C28 0.013(4) 0.029(4) 0.025(4) 0.010(3) 0.006(3) 0.009(3) C29 0.014(4) 0.012(4) 0.027(4) 0.005(3) 0.005(3) -0.008(3) C30 0.014(3) 0.015(3) 0.017(4) 0.008(3) 0.006(3) 0.007(3) C31 0.011(3) 0.017(4) 0.012(3) -0.001(3) 0.007(3) 0.007(3) C32 0.017(4) 0.008(3) 0.019(4) 0.006(3) 0.010(3) 0.007(3) C33 0.016(4) 0.015(3) 0.015(4) 0.003(3) 0.008(3) 0.004(3) C34 0.016(4) 0.014(4) 0.019(4) -0.001(3) 0.008(3) 0.005(3) C35 0.026(4) 0.012(3) 0.031(4) 0.007(3) 0.020(4) 0.011(3) C36 0.012(3) 0.016(4) 0.025(4) 0.010(3) 0.012(3) 0.008(3) C37 0.023(4) 0.009(3) 0.020(4) 0.006(3) 0.015(3) 0.011(3) C38 0.018(4) 0.013(3) 0.013(3) 0.002(3) 0.003(3) 0.012(3) C39 0.012(3) 0.021(4) 0.010(3) 0.008(3) 0.004(3) 0.007(3) C40 0.021(4) 0.023(4) 0.035(5) 0.011(4) 0.011(4) 0.008(3) C41 0.016(4) 0.027(4) 0.037(5) 0.011(4) 0.008(4) 0.006(3) C42 0.013(4) 0.042(5) 0.021(4) 0.013(4) 0.002(3) -0.003(4) C43 0.028(4) 0.025(4) 0.020(4) 0.005(3) 0.008(4) -0.002(4) C44 0.030(4) 0.016(4) 0.011(3) 0.002(3) 0.009(3) 0.007(3) C45 0.023(4) 0.020(4) 0.023(4) 0.004(3) 0.008(3) 0.013(3) C46 0.032(4) 0.007(3) 0.029(4) 0.007(3) 0.019(4) 0.012(3) Eu1 0.01348(19) 0.00967(18) 0.00919(18) 0.00237(13) 0.00444(14) 0.00530(14) Eu2 0.01265(18) 0.00896(17) 0.00930(18) 0.00217(13) 0.00476(14) 0.00567(14) N1 0.018(3) 0.031(4) 0.029(4) 0.009(3) 0.009(3) 0.006(3) N2 0.022(3) 0.026(4) 0.023(4) 0.008(3) 0.010(3) 0.010(3) N3 0.033(4) 0.015(3) 0.034(4) 0.006(3) 0.018(3) 0.010(3) N4 0.018(3) 0.017(3) 0.031(4) 0.010(3) 0.010(3) 0.008(3) N5 0.021(3) 0.020(3) 0.019(3) 0.005(3) 0.011(3) 0.009(3) N6 0.042(4) 0.015(3) 0.028(4) 0.006(3) 0.019(4) 0.010(3) O1 0.019(3) 0.018(3) 0.017(3) 0.007(2) 0.009(2) 0.008(2) O2 0.047(4) 0.058(5) 0.088(6) 0.014(4) 0.053(5) 0.006(4) O3 0.029(3) 0.017(3) 0.024(3) 0.000(2) 0.005(3) 0.006(2) O4 0.022(3) 0.012(2) 0.013(2) 0.003(2) 0.004(2) 0.006(2) O5 0.023(3) 0.009(2) 0.013(2) 0.003(2) 0.005(2) 0.005(2) O6 0.019(3) 0.023(3) 0.039(3) 0.012(3) 0.011(3) 0.010(2) O7 0.019(3) 0.032(4) 0.055(4) 0.013(3) 0.010(3) -0.004(3) O8 0.019(3) 0.017(3) 0.012(2) 0.000(2) 0.006(2) 0.008(2) O9 0.043(4) 0.020(3) 0.076(5) 0.017(3) 0.010(4) 0.007(3) O10 0.025(3) 0.022(3) 0.027(3) 0.006(2) 0.009(3) 0.013(2) O11 0.032(3) 0.020(3) 0.011(3) 0.007(2) 0.008(2) 0.014(2) O12 0.018(3) 0.025(3) 0.055(4) -0.011(3) -0.002(3) 0.006(3) O13 0.021(3) 0.019(3) 0.011(2) 0.003(2) 0.007(2) 0.013(2) O14 0.022(3) 0.015(3) 0.018(3) 0.004(2) 0.011(2) 0.004(2) O15 0.011(2) 0.010(2) 0.022(3) -0.003(2) 0.005(2) 0.002(2) O16 0.018(3) 0.011(2) 0.017(3) 0.002(2) 0.007(2) 0.006(2) O17 0.030(3) 0.025(3) 0.029(3) 0.013(3) 0.012(3) 0.014(3) O18 0.036(3) 0.028(3) 0.030(3) -0.009(3) 0.010(3) 0.016(3) O19 0.018(3) 0.012(2) 0.019(3) 0.007(2) 0.008(2) 0.012(2) O20 0.027(3) 0.013(3) 0.025(3) 0.004(2) 0.007(3) 0.003(2) O21 0.044(4) 0.023(3) 0.016(3) 0.004(2) 0.010(3) 0.016(3) O22 0.017(3) 0.013(2) 0.009(2) 0.0031(19) 0.003(2) 0.006(2) O23 0.021(3) 0.021(3) 0.015(3) 0.008(2) 0.008(2) 0.009(2) O24 0.028(3) 0.026(3) 0.038(4) -0.001(3) 0.003(3) 0.016(3) O25 0.058(4) 0.015(3) 0.055(4) 0.005(3) 0.038(4) 0.013(3) O26 0.023(3) 0.018(3) 0.016(3) 0.004(2) 0.010(2) 0.009(2) O27 0.021(3) 0.015(3) 0.017(3) 0.003(2) 0.010(2) 0.010(2) O28 0.024(3) 0.011(2) 0.014(3) 0.007(2) 0.009(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.261(8) . ? C1 O14 1.261(8) 2_766 ? C1 C2 1.511(9) . ? C2 C7 1.383(10) . ? C2 C3 1.386(10) . ? C3 C4 1.385(10) . ? C3 N1 1.474(10) . ? C4 C5 1.366(12) . ? C4 H4 0.9500 . ? C5 C6 1.395(11) . ? C5 H5 0.9500 . ? C6 C7 1.398(10) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 O5 1.249(8) . ? C8 O4 1.279(8) . ? C8 C9 1.512(9) . ? C8 Eu1 2.834(7) . ? C9 C14 1.377(10) . ? C9 C10 1.387(9) . ? C10 C11 1.396(10) . ? C10 H10 0.9500 . ? C11 C12 1.368(11) . ? C11 H11 0.9500 . ? C12 C13 1.402(11) . ? C12 H12 0.9500 . ? C13 C14 1.375(10) . ? C13 H13 0.9500 . ? C14 N2 1.478(9) . ? C15 O11 1.248(8) 2_766 ? C15 O8 1.268(8) . ? C15 C16 1.500(10) . ? C15 Eu1 3.200(7) . ? C16 C17 1.383(10) . ? C16 C21 1.401(10) . ? C17 C18 1.372(11) . ? C17 N3 1.479(10) . ? C18 C19 1.377(11) . ? C18 H18 0.9500 . ? C19 C20 1.389(11) . ? C19 H19 0.9500 . ? C20 C21 1.395(11) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O12 1.416(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O13 1.444(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O16 1.261(8) . ? C24 O15 1.266(8) . ? C24 C25 1.490(9) . ? C24 Eu2 2.800(7) . ? C25 C26 1.392(9) . ? C25 C30 1.392(10) . ? C26 C27 1.387(10) . ? C26 H26 0.9500 . ? C27 C28 1.379(11) . ? C27 H27 0.9500 . ? C28 C29 1.372(10) . ? C28 H28 0.9500 . ? C29 C30 1.365(10) . ? C29 H29 0.9500 . ? C30 N4 1.473(9) . ? C31 O19 1.241(7) . ? C31 O26 1.258(8) 2_765 ? C31 C32 1.521(9) . ? C32 C33 1.386(10) . ? C32 C37 1.387(10) . ? C33 C34 1.400(9) . ? C33 H33 0.9500 . ? C34 C35 1.385(10) . ? C34 H34 0.9500 . ? C35 C36 1.378(10) . ? C35 H35 0.9500 . ? C36 C37 1.390(9) . ? C36 H36 0.9500 . ? C37 N5 1.479(9) . ? C38 O23 1.255(8) . ? C38 O22 1.271(8) . ? C38 C39 1.499(10) . ? C38 Eu2 2.930(7) . ? C39 C44 1.391(10) . ? C39 C40 1.391(10) . ? C40 C41 1.390(11) . ? C40 H40 0.9500 . ? C41 C42 1.362(12) . ? C41 H41 0.9500 . ? C42 C43 1.391(12) . ? C42 H42 0.9500 . ? C43 C44 1.367(11) . ? C43 H43 0.9500 . ? C44 N6 1.501(10) . ? C45 O27 1.425(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O28 1.426(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? Eu1 O11 2.282(5) . ? Eu1 O14 2.354(5) . ? Eu1 O1 2.382(5) . ? Eu1 O4 2.433(5) . ? Eu1 O8 2.435(5) . ? Eu1 O12 2.443(6) . ? Eu1 O13 2.461(4) . ? Eu1 O5 2.524(5) . ? Eu1 Eu1 4.3507(13) 2_766 ? Eu2 O19 2.377(4) . ? Eu2 O22 2.388(4) 2_765 ? Eu2 O15 2.408(5) . ? Eu2 O26 2.410(5) . ? Eu2 O28 2.410(5) . ? Eu2 O27 2.453(5) . ? Eu2 O16 2.494(5) . ? Eu2 O23 2.542(5) . ? Eu2 O22 2.573(5) . ? Eu2 Eu2 3.9428(11) 2_765 ? N1 O2 1.220(8) . ? N1 O3 1.222(8) . ? N2 O7 1.213(8) . ? N2 O6 1.235(8) . ? N3 O10 1.220(8) . ? N3 O9 1.230(8) . ? N4 O18 1.223(8) . ? N4 O17 1.231(8) . ? N5 O20 1.220(8) . ? N5 O21 1.230(8) . ? N6 O25 1.201(8) . ? N6 O24 1.214(9) . ? O11 C15 1.248(8) 2_766 ? O14 C1 1.261(8) 2_766 ? O22 Eu2 2.388(4) 2_765 ? O26 C31 1.258(8) 2_765 ? 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 C1 O14 127.2(6) . 2_766 ? O1 C1 C2 116.1(6) . . ? O14 C1 C2 116.7(6) 2_766 . ? C7 C2 C3 117.6(7) . . ? C7 C2 C1 118.3(6) . . ? C3 C2 C1 123.9(6) . . ? C2 C3 C4 122.6(7) . . ? C2 C3 N1 119.7(7) . . ? C4 C3 N1 117.5(7) . . ? C5 C4 C3 118.9(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 120.6(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.3(7) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C2 C7 C6 121.0(7) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O5 C8 O4 121.6(6) . . ? O5 C8 C9 119.8(6) . . ? O4 C8 C9 118.4(6) . . ? O5 C8 Eu1 62.9(3) . . ? O4 C8 Eu1 58.9(3) . . ? C9 C8 Eu1 170.8(5) . . ? C14 C9 C10 117.4(6) . . ? C14 C9 C8 125.7(6) . . ? C10 C9 C8 116.6(6) . . ? C9 C10 C11 120.9(7) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.1(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 118.2(7) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C13 C14 C9 123.3(7) . . ? C13 C14 N2 116.8(6) . . ? C9 C14 N2 119.8(6) . . ? O11 C15 O8 123.4(7) 2_766 . ? O11 C15 C16 117.6(6) 2_766 . ? O8 C15 C16 118.9(6) . . ? O11 C15 Eu1 80.6(4) 2_766 . ? O8 C15 Eu1 43.2(3) . . ? C16 C15 Eu1 159.6(5) . . ? C17 C16 C21 117.2(7) . . ? C17 C16 C15 126.7(7) . . ? C21 C16 C15 116.0(6) . . ? C18 C17 C16 122.9(7) . . ? C18 C17 N3 117.9(7) . . ? C16 C17 N3 119.2(7) . . ? C17 C18 C19 119.2(7) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 120.5(7) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 119.2(7) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C16 121.0(7) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? O12 C22 H22A 109.5 . . ? O12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O13 C23 H23A 109.5 . . ? O13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O16 C24 O15 122.0(6) . . ? O16 C24 C25 120.0(6) . . ? O15 C24 C25 117.9(6) . . ? O16 C24 Eu2 63.0(4) . . ? O15 C24 Eu2 59.0(3) . . ? C25 C24 Eu2 174.5(5) . . ? C26 C25 C30 116.1(6) . . ? C26 C25 C24 119.3(6) . . ? C30 C25 C24 124.3(6) . . ? C27 C26 C25 121.5(7) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 119.3(7) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 120.9(7) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C28 118.5(7) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C29 C30 C25 123.5(7) . . ? C29 C30 N4 116.7(6) . . ? C25 C30 N4 119.7(6) . . ? O19 C31 O26 127.7(6) . 2_765 ? O19 C31 C32 116.4(6) . . ? O26 C31 C32 115.8(6) 2_765 . ? C33 C32 C37 116.0(6) . . ? C33 C32 C31 119.6(6) . . ? C37 C32 C31 124.2(6) . . ? C32 C33 C34 120.8(7) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 121.0(7) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 119.8(6) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 117.5(7) . . ? C35 C36 H36 121.3 . . ? C37 C36 H36 121.3 . . ? C32 C37 C36 124.9(7) . . ? C32 C37 N5 119.0(6) . . ? C36 C37 N5 116.1(6) . . ? O23 C38 O22 120.7(7) . . ? O23 C38 C39 119.9(6) . . ? O22 C38 C39 119.1(6) . . ? O23 C38 Eu2 59.8(4) . . ? O22 C38 Eu2 61.2(4) . . ? C39 C38 Eu2 179.5(5) . . ? C44 C39 C40 116.7(7) . . ? C44 C39 C38 124.9(6) . . ? C40 C39 C38 118.3(7) . . ? C41 C40 C39 119.3(8) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C42 C41 C40 122.8(8) . . ? C42 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C41 C42 C43 118.6(7) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 118.6(8) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C39 123.9(7) . . ? C43 C44 N6 117.4(7) . . ? C39 C44 N6 118.7(7) . . ? O27 C45 H45A 109.5 . . ? O27 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O27 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O28 C46 H46A 109.5 . . ? O28 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O28 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O11 Eu1 O14 76.52(17) . . ? O11 Eu1 O1 75.83(17) . . ? O14 Eu1 O1 124.85(16) . . ? O11 Eu1 O4 134.21(17) . . ? O14 Eu1 O4 147.51(16) . . ? O1 Eu1 O4 80.14(16) . . ? O11 Eu1 O8 120.45(18) . . ? O14 Eu1 O8 79.72(17) . . ? O1 Eu1 O8 74.84(16) . . ? O4 Eu1 O8 89.07(16) . . ? O11 Eu1 O12 83.6(2) . . ? O14 Eu1 O12 78.47(19) . . ? O1 Eu1 O12 142.64(18) . . ? O4 Eu1 O12 93.0(2) . . ? O8 Eu1 O12 142.19(18) . . ? O11 Eu1 O13 147.34(17) . . ? O14 Eu1 O13 78.89(16) . . ? O1 Eu1 O13 136.59(16) . . ? O4 Eu1 O13 68.75(16) . . ? O8 Eu1 O13 75.14(16) . . ? O12 Eu1 O13 70.60(19) . . ? O11 Eu1 O5 83.18(17) . . ? O14 Eu1 O5 145.92(17) . . ? O1 Eu1 O5 74.59(16) . . ? O4 Eu1 O5 52.84(15) . . ? O8 Eu1 O5 134.36(16) . . ? O12 Eu1 O5 72.23(18) . . ? O13 Eu1 O5 106.58(16) . . ? O11 Eu1 C8 108.29(19) . . ? O14 Eu1 C8 160.02(18) . . ? O1 Eu1 C8 74.79(17) . . ? O4 Eu1 C8 26.74(17) . . ? O8 Eu1 C8 112.14(18) . . ? O12 Eu1 C8 82.8(2) . . ? O13 Eu1 C8 88.49(17) . . ? O5 Eu1 C8 26.15(17) . . ? O11 Eu1 C15 99.58(19) . . ? O14 Eu1 C15 73.12(17) . . ? O1 Eu1 C15 65.80(17) . . ? O4 Eu1 C15 105.24(17) . . ? O8 Eu1 C15 20.88(16) . . ? O12 Eu1 C15 149.70(19) . . ? O13 Eu1 C15 93.45(17) . . ? O5 Eu1 C15 138.02(17) . . ? C8 Eu1 C15 123.56(18) . . ? O11 Eu1 Eu1 46.59(14) . 2_766 ? O14 Eu1 Eu1 64.54(12) . 2_766 ? O1 Eu1 Eu1 61.69(11) . 2_766 ? O4 Eu1 Eu1 140.92(12) . 2_766 ? O8 Eu1 Eu1 73.88(11) . 2_766 ? O12 Eu1 Eu1 122.03(17) . 2_766 ? O13 Eu1 Eu1 135.31(12) . 2_766 ? O5 Eu1 Eu1 118.11(11) . 2_766 ? C8 Eu1 Eu1 133.06(13) . 2_766 ? C15 Eu1 Eu1 53.04(12) . 2_766 ? O19 Eu2 O22 77.05(16) . 2_765 ? O19 Eu2 O15 129.21(16) . . ? O22 Eu2 O15 90.65(17) 2_765 . ? O19 Eu2 O26 138.18(16) . . ? O22 Eu2 O26 73.02(16) 2_765 . ? O15 Eu2 O26 79.99(16) . . ? O19 Eu2 O28 76.08(16) . . ? O22 Eu2 O28 141.78(16) 2_765 . ? O15 Eu2 O28 85.74(17) . . ? O26 Eu2 O28 142.76(16) . . ? O19 Eu2 O27 138.11(16) . . ? O22 Eu2 O27 143.61(15) 2_765 . ? O15 Eu2 O27 73.54(16) . . ? O26 Eu2 O27 72.06(16) . . ? O28 Eu2 O27 70.93(16) . . ? O19 Eu2 O16 75.74(16) . . ? O22 Eu2 O16 74.01(16) 2_765 . ? O15 Eu2 O16 53.57(15) . . ? O26 Eu2 O16 121.46(16) . . ? O28 Eu2 O16 73.37(16) . . ? O27 Eu2 O16 117.02(16) . . ? O19 Eu2 O23 79.96(16) . . ? O22 Eu2 O23 125.18(16) 2_765 . ? O15 Eu2 O23 140.48(16) . . ? O26 Eu2 O23 94.04(17) . . ? O28 Eu2 O23 75.67(16) . . ? O27 Eu2 O23 67.53(16) . . ? O16 Eu2 O23 144.30(16) . . ? O19 Eu2 O22 72.10(15) . . ? O22 Eu2 O22 74.78(17) 2_765 . ? O15 Eu2 O22 151.40(15) . . ? O26 Eu2 O22 72.32(15) . . ? O28 Eu2 O22 120.90(16) . . ? O27 Eu2 O22 103.74(16) . . ? O16 Eu2 O22 139.15(15) . . ? O23 Eu2 O22 50.84(15) . . ? O19 Eu2 C24 102.49(18) . . ? O22 Eu2 C24 81.17(18) 2_765 . ? O15 Eu2 C24 26.80(18) . . ? O26 Eu2 C24 101.04(18) . . ? O28 Eu2 C24 78.68(18) . . ? O27 Eu2 C24 95.70(18) . . ? O16 Eu2 C24 26.77(17) . . ? O23 Eu2 C24 152.82(17) . . ? O22 Eu2 C24 155.95(17) . . ? O19 Eu2 C38 76.03(17) . . ? O22 Eu2 C38 100.38(18) 2_765 . ? O15 Eu2 C38 154.46(17) . . ? O26 Eu2 C38 81.33(18) . . ? O28 Eu2 C38 98.95(18) . . ? O27 Eu2 C38 84.24(18) . . ? O16 Eu2 C38 151.76(16) . . ? O23 Eu2 C38 25.27(17) . . ? O22 Eu2 C38 25.66(16) . . ? C24 Eu2 C38 177.49(18) . . ? O19 Eu2 Eu2 70.35(11) . 2_765 ? O22 Eu2 Eu2 39.02(11) 2_765 2_765 ? O15 Eu2 Eu2 125.43(12) . 2_765 ? O26 Eu2 Eu2 67.97(11) . 2_765 ? O28 Eu2 Eu2 144.18(11) . 2_765 ? O27 Eu2 Eu2 129.98(11) . 2_765 ? O16 Eu2 Eu2 109.07(11) . 2_765 ? O23 Eu2 Eu2 86.38(11) . 2_765 ? O22 Eu2 Eu2 35.76(10) . 2_765 ? C24 Eu2 Eu2 120.19(14) . 2_765 ? C38 Eu2 Eu2 61.38(14) . 2_765 ? O2 N1 O3 123.9(7) . . ? O2 N1 C3 117.6(7) . . ? O3 N1 C3 118.4(6) . . ? O7 N2 O6 125.0(6) . . ? O7 N2 C14 118.3(6) . . ? O6 N2 C14 116.7(6) . . ? O10 N3 O9 123.6(7) . . ? O10 N3 C17 118.3(6) . . ? O9 N3 C17 118.0(7) . . ? O18 N4 O17 125.0(6) . . ? O18 N4 C30 118.3(6) . . ? O17 N4 C30 116.6(6) . . ? O20 N5 O21 123.2(6) . . ? O20 N5 C37 119.1(6) . . ? O21 N5 C37 117.6(6) . . ? O25 N6 O24 125.7(7) . . ? O25 N6 C44 117.5(7) . . ? O24 N6 C44 116.8(6) . . ? C1 O1 Eu1 141.8(4) . . ? C8 O4 Eu1 94.4(4) . . ? C8 O5 Eu1 90.9(4) . . ? C15 O8 Eu1 115.9(4) . . ? C15 O11 Eu1 174.0(5) 2_766 . ? C22 O12 Eu1 134.8(5) . . ? C23 O13 Eu1 132.5(4) . . ? C1 O14 Eu1 139.0(4) 2_766 . ? C24 O15 Eu2 94.2(4) . . ? C24 O16 Eu2 90.3(4) . . ? C31 O19 Eu2 135.5(4) . . ? C38 O22 Eu2 161.3(4) . 2_765 ? C38 O22 Eu2 93.1(4) . . ? Eu2 O22 Eu2 105.22(17) 2_765 . ? C38 O23 Eu2 94.9(4) . . ? C31 O26 Eu2 137.9(4) 2_765 . ? C45 O27 Eu2 130.6(4) . . ? C46 O28 Eu2 130.4(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.003 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.226