Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'I. Goldberg' _publ_contact_author_address ; School of Chemistry Tel Aviv University Ramat Aviv Tel Aviv 69978 ISRAEL ; _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL _publ_section_title ; Framework coordination polymers of tetra(4-carboxyphenyl)- porphyrin and lanthanide ions in crystalline solids ; loop_ _publ_author_name 'I. Goldberg' 'Sumod George' 'Sophia Lipstman' 'Sankar Muniappan' data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 627696' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H31 Dy N4 O10' _chemical_formula_sum 'C48 H31 Dy N4 O10' _chemical_formula_weight 986.27 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.8851(5) _cell_length_b 26.4514(7) _cell_length_c 9.39160(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.6484(14) _cell_angle_gamma 90.00 _cell_volume 5114.91(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6039 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5824 _exptl_absorpt_correction_T_max 0.8632 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25563 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.17 _reflns_number_total 6176 _reflns_number_gt 5624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.065. The residual electron-density maps contained however several peaks at ~3 e/\%A^3^. This disordered solvent species could not be modeled by discrete atoms. ; _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^)+(0.0524P)^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 6176 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy Dy 0.5000 0.506357(6) 0.7500 0.01092(6) Uani 1 2 d S . . C1 C 0.5000 0.18236(12) 0.7500 0.0138(6) Uani 1 2 d S . . C2 C 0.44734(12) 0.15818(9) 0.7953(3) 0.0157(5) Uani 1 1 d . . . C3 C 0.39121(12) 0.18345(9) 0.8334(3) 0.0186(5) Uani 1 1 d . . . H3 H 0.3828 0.2188 0.8286 0.022 Uiso 1 1 calc R . . C4 C 0.35300(12) 0.14738(10) 0.8771(3) 0.0179(5) Uani 1 1 d . . . H4 H 0.3125 0.1526 0.9081 0.022 Uiso 1 1 calc R . . C5 C 0.38517(11) 0.09949(9) 0.8678(2) 0.0138(4) Uani 1 1 d . . . C6 C 0.36544(11) 0.05317(9) 0.9178(2) 0.0135(5) Uani 1 1 d . . . C7 C 0.39875(12) 0.00685(9) 0.9124(3) 0.0121(5) Uani 1 1 d . . . C8 C 0.38356(12) -0.04028(9) 0.9755(3) 0.0167(5) Uani 1 1 d . . . H8 H 0.3524 -0.0453 1.0372 0.020 Uiso 1 1 calc R . . C9 C 0.42188(12) -0.07635(9) 0.9304(2) 0.0168(5) Uani 1 1 d . . . H9 H 0.4232 -0.1111 0.9566 0.020 Uiso 1 1 calc R . . C10 C 0.46036(11) -0.05227(9) 0.8354(2) 0.0138(4) Uani 1 1 d . . . C11 C 0.5000 -0.07744(12) 0.7500 0.0143(6) Uani 1 2 d S . . N12 N 0.44153(9) 0.10727(7) 0.8146(2) 0.0141(4) Uani 1 1 d . . . H12 H 0.4689 0.0838 0.7961 0.017 Uiso 0.50 1 calc PR . . N13 N 0.44704(11) -0.00134(7) 0.8325(2) 0.0127(4) Uani 1 1 d . . . H13 H 0.4661 0.0219 0.7872 0.015 Uiso 0.50 1 calc PR . . C14 C 0.5000 0.23856(13) 0.7500 0.0141(6) Uani 1 2 d S . . C15 C 0.51593(17) 0.26511(11) 0.8769(3) 0.0361(8) Uani 1 1 d . . . H15 H 0.5267 0.2473 0.9656 0.043 Uiso 1 1 calc R . . C16 C 0.51643(17) 0.31739(11) 0.8770(3) 0.0366(8) Uani 1 1 d . . . H16 H 0.5282 0.3352 0.9654 0.044 Uiso 1 1 calc R . . C17 C 0.5000 0.34383(13) 0.7500 0.0162(7) Uani 1 2 d S . . C18 C 0.5000 0.40023(13) 0.7500 0.0147(7) Uani 1 2 d S . . O19 O 0.52158(8) 0.42385(6) 0.86508(16) 0.0150(3) Uani 1 1 d . . . C20 C 0.30074(11) 0.05249(9) 0.9671(2) 0.0143(5) Uani 1 1 d . . . C21 C 0.24569(11) 0.06300(9) 0.8652(2) 0.0148(5) Uani 1 1 d . . . H21 H 0.2506 0.0737 0.7711 0.018 Uiso 1 1 calc R . . C22 C 0.18389(11) 0.05804(9) 0.8990(2) 0.0152(5) Uani 1 1 d . . . H22 H 0.1469 0.0650 0.8281 0.018 Uiso 1 1 calc R . . C23 C 0.17609(11) 0.04282(9) 1.0372(2) 0.0126(4) Uani 1 1 d . . . C24 C 0.23096(11) 0.03605(10) 1.1427(2) 0.0165(5) Uani 1 1 d . . . H24 H 0.2261 0.0285 1.2392 0.020 Uiso 1 1 calc R . . C25 C 0.29300(11) 0.04027(10) 1.1072(2) 0.0169(5) Uani 1 1 d . . . H25 H 0.3301 0.0348 1.1791 0.020 Uiso 1 1 calc R . . C26 C 0.10945(11) 0.02984(9) 1.0668(2) 0.0124(4) Uani 1 1 d . . . O27 O 0.10185(8) 0.02256(7) 1.19595(17) 0.0152(3) Uani 1 1 d . . . O28 O 0.06441(8) 0.02527(7) 0.96071(17) 0.0163(3) Uani 1 1 d . . . C29 C 0.5000 -0.13349(12) 0.7500 0.0162(7) Uani 1 2 d S . . C30 C 0.55767(12) -0.16095(10) 0.7864(3) 0.0197(5) Uani 1 1 d . . . H30 H 0.5976 -0.1434 0.8123 0.024 Uiso 1 1 calc R . . C31 C 0.55763(13) -0.21362(10) 0.7853(3) 0.0227(5) Uani 1 1 d . . . H31 H 0.5976 -0.2313 0.8090 0.027 Uiso 1 1 calc R . . C32 C 0.5000 -0.24078(14) 0.7500 0.0204(7) Uani 1 2 d S . . C33 C 0.5000 -0.29814(14) 0.7500 0.0253(8) Uani 1 2 d S . . O34 O 0.55367(11) -0.32054(7) 0.7571(2) 0.0348(5) Uani 1 1 d . . . H34 H 0.5480 -0.3484 0.7210 0.052 Uiso 0.50 1 d P . . O35 O 0.54910(8) 0.58088(6) 0.65790(17) 0.0158(3) Uani 1 1 d . . . H35A H 0.5366 0.5824 0.5548 0.024 Uiso 1 1 d R . . H35B H 0.5656 0.5517 0.6752 0.024 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy 0.01057(9) 0.01133(10) 0.01140(9) 0.000 0.00343(6) 0.000 C1 0.0167(16) 0.0078(16) 0.0174(15) 0.000 0.0045(12) 0.000 C2 0.0197(12) 0.0096(12) 0.0191(11) 0.0007(9) 0.0068(9) 0.0007(9) C3 0.0216(13) 0.0098(12) 0.0267(13) 0.0005(9) 0.0106(10) 0.0030(9) C4 0.0156(12) 0.0153(13) 0.0246(12) 0.0007(9) 0.0085(9) 0.0016(9) C5 0.0119(11) 0.0122(12) 0.0184(11) -0.0010(8) 0.0056(8) -0.0003(8) C6 0.0126(11) 0.0139(12) 0.0149(11) -0.0014(8) 0.0045(8) -0.0024(9) C7 0.0106(11) 0.0132(12) 0.0126(11) -0.0003(8) 0.0016(8) -0.0016(8) C8 0.0170(12) 0.0148(12) 0.0192(12) 0.0018(9) 0.0055(9) -0.0025(9) C9 0.0198(12) 0.0127(12) 0.0181(12) 0.0031(9) 0.0033(9) -0.0029(9) C10 0.0149(11) 0.0098(11) 0.0161(11) 0.0001(8) 0.0008(8) -0.0011(9) C11 0.0157(16) 0.0094(17) 0.0166(15) 0.000 -0.0004(12) 0.000 N12 0.0161(10) 0.0085(10) 0.0195(10) -0.0001(7) 0.0083(7) -0.0011(7) N13 0.0113(10) 0.0099(10) 0.0173(11) 0.0002(7) 0.0033(8) -0.0007(7) C14 0.0119(16) 0.0132(17) 0.0199(16) 0.000 0.0106(12) 0.000 C15 0.078(2) 0.0114(14) 0.0168(13) 0.0027(10) 0.0026(13) -0.0013(14) C16 0.077(2) 0.0122(14) 0.0180(14) -0.0028(10) 0.0017(13) -0.0009(14) C17 0.0230(18) 0.0069(16) 0.0209(16) 0.000 0.0098(13) 0.000 C18 0.0205(17) 0.0105(17) 0.0164(16) 0.000 0.0118(12) 0.000 O19 0.0243(9) 0.0079(8) 0.0138(8) 0.0007(6) 0.0064(6) 0.0006(6) C20 0.0139(11) 0.0113(12) 0.0189(11) 0.0003(8) 0.0058(8) -0.0014(8) C21 0.0144(11) 0.0162(12) 0.0148(11) 0.0021(9) 0.0054(8) -0.0014(9) C22 0.0135(11) 0.0164(12) 0.0153(11) -0.0006(9) 0.0015(8) -0.0016(9) C23 0.0125(11) 0.0090(11) 0.0173(11) 0.0011(8) 0.0057(8) -0.0012(8) C24 0.0157(11) 0.0195(13) 0.0152(11) 0.0023(9) 0.0051(8) -0.0017(9) C25 0.0126(11) 0.0205(13) 0.0173(11) 0.0023(9) 0.0014(8) -0.0003(9) C26 0.0134(11) 0.0067(11) 0.0178(11) -0.0004(8) 0.0042(8) 0.0019(8) O27 0.0136(8) 0.0171(9) 0.0164(8) 0.0044(7) 0.0068(6) -0.0005(7) O28 0.0117(8) 0.0179(9) 0.0195(8) -0.0046(7) 0.0031(6) -0.0023(7) C29 0.0273(19) 0.0066(16) 0.0157(16) 0.000 0.0067(13) 0.000 C30 0.0216(13) 0.0138(13) 0.0240(13) 0.0000(9) 0.0049(10) 0.0004(10) C31 0.0261(14) 0.0142(13) 0.0280(13) 0.0017(10) 0.0050(10) 0.0057(10) C32 0.035(2) 0.0123(18) 0.0145(16) 0.000 0.0065(14) 0.000 C33 0.049(3) 0.0111(18) 0.0161(17) 0.000 0.0058(15) 0.000 O34 0.0519(14) 0.0133(10) 0.0385(11) -0.0046(8) 0.0057(10) 0.0060(9) O35 0.0213(9) 0.0107(8) 0.0153(8) 0.0016(6) 0.0023(6) -0.0004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy O28 2.2546(15) 4_556 ? Dy O28 2.2547(16) 3 ? Dy O27 2.3935(16) 7_557 ? Dy O27 2.3936(16) 8 ? Dy O35 2.4459(16) 2_656 ? Dy O35 2.4460(16) . ? Dy O19 2.4434(16) . ? Dy O19 2.4434(16) 2_656 ? Dy C18 2.807(3) . ? Dy H35B 2.0321 . ? C1 C2 1.399(3) . ? C1 C2 1.399(3) 2_656 ? C1 C14 1.487(5) . ? C2 N12 1.367(3) . ? C2 C3 1.446(3) . ? C3 C4 1.351(3) . ? C3 H3 0.9500 . ? C4 C5 1.443(3) . ? C4 H4 0.9500 . ? C5 N12 1.370(3) . ? C5 C6 1.399(3) . ? C6 C7 1.414(3) . ? C6 C20 1.500(3) . ? C7 N13 1.372(3) . ? C7 C8 1.438(3) . ? C8 C9 1.358(3) . ? C8 H8 0.9500 . ? C9 C10 1.445(3) . ? C9 H9 0.9500 . ? C10 N13 1.375(3) . ? C10 C11 1.413(3) . ? C11 C10 1.413(3) 2_656 ? C11 C29 1.482(5) . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? C14 C15 1.375(3) 2_656 ? C14 C15 1.375(3) . ? C15 C16 1.383(4) . ? C15 H15 0.9500 . ? C16 C17 1.376(3) . ? C16 H16 0.9500 . ? C17 C16 1.376(3) 2_656 ? C17 C18 1.492(5) . ? C18 O19 1.264(2) 2_656 ? C18 O19 1.264(2) . ? C20 C25 1.390(3) . ? C20 C21 1.395(3) . ? C21 C22 1.386(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 C24 1.395(3) . ? C23 C26 1.504(3) . ? C24 C25 1.395(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O28 1.256(3) . ? C26 O27 1.265(3) . ? O27 Dy 2.3936(16) 7_557 ? O28 Dy 2.2547(15) 3_445 ? C29 C30 1.399(3) . ? C29 C30 1.399(3) 2_656 ? C30 C31 1.393(4) . ? C30 H30 0.9500 . ? C31 C32 1.393(3) . ? C31 H31 0.9500 . ? C32 C31 1.393(3) 2_656 ? C32 C33 1.517(5) . ? C33 O34 1.260(3) 2_656 ? C33 O34 1.260(3) . ? O34 H34 0.8117 . ? O35 H35A 0.9602 . ? O35 H35B 0.8500 . ? 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 O28 Dy O28 154.36(9) 4_556 3 ? O28 Dy O27 80.59(6) 4_556 7_557 ? O28 Dy O27 107.79(6) 3 7_557 ? O28 Dy O27 107.79(6) 4_556 8 ? O28 Dy O27 80.58(6) 3 8 ? O27 Dy O27 142.72(9) 7_557 8 ? O28 Dy O35 84.71(6) 4_556 2_656 ? O28 Dy O35 74.61(6) 3 2_656 ? O27 Dy O35 75.08(6) 7_557 2_656 ? O27 Dy O35 140.59(6) 8 2_656 ? O28 Dy O35 74.61(6) 4_556 . ? O28 Dy O35 84.71(6) 3 . ? O27 Dy O35 140.60(6) 7_557 . ? O27 Dy O35 75.08(6) 8 . ? O35 Dy O35 72.60(8) 2_656 . ? O28 Dy O19 128.69(6) 4_556 . ? O28 Dy O19 76.78(6) 3 . ? O27 Dy O19 74.05(6) 7_557 . ? O27 Dy O19 72.77(6) 8 . ? O35 Dy O19 128.36(5) 2_656 . ? O35 Dy O19 144.99(6) . . ? O28 Dy O19 76.78(6) 4_556 2_656 ? O28 Dy O19 128.69(6) 3 2_656 ? O27 Dy O19 72.77(6) 7_557 2_656 ? O27 Dy O19 74.05(6) 8 2_656 ? O35 Dy O19 144.99(6) 2_656 2_656 ? O35 Dy O19 128.36(5) . 2_656 ? O19 Dy O19 53.46(7) . 2_656 ? O28 Dy C18 102.82(5) 4_556 . ? O28 Dy C18 102.82(5) 3 . ? O27 Dy C18 71.36(4) 7_557 . ? O27 Dy C18 71.36(4) 8 . ? O35 Dy C18 143.70(4) 2_656 . ? O35 Dy C18 143.70(4) . . ? O19 Dy C18 26.73(4) . . ? O19 Dy C18 26.73(4) 2_656 . ? O28 Dy H35B 84.4 4_556 . ? O28 Dy H35B 80.5 3 . ? O27 Dy H35B 159.4 7_557 . ? O27 Dy H35B 56.0 8 . ? O35 Dy H35B 89.6 2_656 . ? O35 Dy H35B 19.2 . . ? O19 Dy H35B 126.5 . . ? O19 Dy H35B 117.3 2_656 . ? C18 Dy H35B 126.2 . . ? C2 C1 C2 125.6(3) . 2_656 ? C2 C1 C14 117.21(15) . . ? C2 C1 C14 117.21(15) 2_656 . ? N12 C2 C1 125.6(2) . . ? N12 C2 C3 109.2(2) . . ? C1 C2 C3 125.1(2) . . ? C4 C3 C2 107.1(2) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? C3 C4 C5 107.3(2) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? N12 C5 C6 125.0(2) . . ? N12 C5 C4 109.1(2) . . ? C6 C5 C4 125.6(2) . . ? C5 C6 C7 124.9(2) . . ? C5 C6 C20 116.4(2) . . ? C7 C6 C20 118.3(2) . . ? N13 C7 C6 124.6(2) . . ? N13 C7 C8 108.8(2) . . ? C6 C7 C8 126.3(2) . . ? C9 C8 C7 107.4(2) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? C8 C9 C10 107.5(2) . . ? C8 C9 H9 126.3 . . ? C10 C9 H9 126.3 . . ? N13 C10 C11 125.9(2) . . ? N13 C10 C9 108.2(2) . . ? C11 C10 C9 125.6(2) . . ? C10 C11 C10 123.7(3) . 2_656 ? C10 C11 C29 118.13(15) . . ? C10 C11 C29 118.13(15) 2_656 . ? C2 N12 C5 107.28(19) . . ? C2 N12 H12 126.4 . . ? C5 N12 H12 126.4 . . ? C7 N13 C10 107.97(19) . . ? C7 N13 H13 126.0 . . ? C10 N13 H13 126.0 . . ? C15 C14 C15 118.6(3) 2_656 . ? C15 C14 C1 120.69(17) 2_656 . ? C15 C14 C1 120.69(17) . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C16 118.9(3) . 2_656 ? C16 C17 C18 120.56(17) . . ? C16 C17 C18 120.56(17) 2_656 . ? O19 C18 O19 120.8(3) 2_656 . ? O19 C18 C17 119.62(15) 2_656 . ? O19 C18 C17 119.62(15) . . ? O19 C18 Dy 60.38(15) 2_656 . ? O19 C18 Dy 60.38(15) . . ? C17 C18 Dy 180.000(1) . . ? C18 O19 Dy 92.89(15) . . ? C25 C20 C21 118.9(2) . . ? C25 C20 C6 123.3(2) . . ? C21 C20 C6 117.8(2) . . ? C22 C21 C20 121.0(2) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.2(2) . . ? C24 C23 C26 121.0(2) . . ? C22 C23 C26 119.6(2) . . ? C25 C24 C23 120.4(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 120.3(2) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? O28 C26 O27 123.3(2) . . ? O28 C26 C23 117.97(19) . . ? O27 C26 C23 118.7(2) . . ? C26 O27 Dy 120.74(14) . 7_557 ? C26 O28 Dy 167.09(15) . 3_445 ? C30 C29 C30 117.4(3) . 2_656 ? C30 C29 C11 121.29(16) . . ? C30 C29 C11 121.29(16) 2_656 . ? C31 C30 C29 121.2(2) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 121.1(3) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C31 117.9(3) 2_656 . ? C31 C32 C33 121.04(17) 2_656 . ? C31 C32 C33 121.04(17) . . ? O34 C33 O34 123.9(4) 2_656 . ? O34 C33 C32 118.06(18) 2_656 . ? O34 C33 C32 118.06(18) . . ? C33 O34 H34 109.8 . . ? Dy O35 H35A 109.4 . . ? Dy O35 H35B 51.7 . . ? H35A O35 H35B 105.3 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.839 _refine_diff_density_min -1.900 _refine_diff_density_rms 0.110 #===============END================================= data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 627697' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H31 N4 O10 Sm' _chemical_formula_sum 'C48 H31 N4 O10 Sm' _chemical_formula_weight 974.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3217(3) _cell_length_b 26.5463(5) _cell_length_c 9.63690(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.8907(9) _cell_angle_gamma 90.00 _cell_volume 5246.16(13) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6127 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 1.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7200 _exptl_absorpt_correction_T_max 0.8918 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25368 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.18 _reflns_number_total 6316 _reflns_number_gt 5840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.048. Two of the carboxylic/carboxylate functions are partly disordered. ; _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^)+(0.0480P)^2^+5.1306P] 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 6316 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.5000 0.509876(5) 0.7500 0.01002(6) Uani 1 2 d S . . C1 C 0.5000 0.18259(11) 0.7500 0.0149(5) Uani 1 2 d S . . C2 C 0.55369(10) 0.15804(8) 0.8417(2) 0.0157(4) Uani 1 1 d . . . C3 C 0.61249(11) 0.18192(8) 0.9269(3) 0.0229(5) Uani 1 1 d . . . H3 H 0.6230 0.2167 0.9267 0.027 Uiso 1 1 calc R . . C4 C 0.64992(10) 0.14540(9) 1.0072(3) 0.0217(5) Uani 1 1 d . . . H4 H 0.6914 0.1500 1.0744 0.026 Uiso 1 1 calc R . . C5 C 0.61555(9) 0.09852(8) 0.9724(2) 0.0136(4) Uani 1 1 d . . . C6 C 0.63469(9) 0.05257(8) 1.0417(2) 0.0123(4) Uani 1 1 d . . . C7 C 0.60128(10) 0.00663(7) 1.0050(2) 0.0114(4) Uani 1 1 d . . . C8 C 0.61753(10) -0.04049(8) 1.0811(2) 0.0157(4) Uani 1 1 d . . . H8 H 0.6491 -0.0453 1.1711 0.019 Uiso 1 1 calc R . . C9 C 0.57943(10) -0.07670(8) 1.0005(2) 0.0156(4) Uani 1 1 d . . . H9 H 0.5787 -0.1114 1.0245 0.019 Uiso 1 1 calc R . . C10 C 0.54011(9) -0.05269(7) 0.8713(2) 0.0128(4) Uani 1 1 d . . . C11 C 0.5000 -0.07742(11) 0.7500 0.0150(5) Uani 1 2 d S . . N12 N 0.55780(8) 0.10712(6) 0.86891(18) 0.0133(3) Uani 1 1 d . . . H12 H 0.5288 0.0842 0.8276 0.016 Uiso 0.50 1 calc PR . . N13 N 0.55259(8) -0.00184(7) 0.8814(2) 0.0124(3) Uani 1 1 d . . . H13 H 0.5327 0.0212 0.8192 0.015 Uiso 0.50 1 calc PR . . C14 C 0.5000 0.23859(11) 0.7500 0.0161(6) Uani 1 2 d S . . C15 C 0.50851(14) 0.26530(9) 0.8767(3) 0.0286(5) Uani 1 1 d . . . H15 H 0.5136 0.2476 0.9648 0.034 Uiso 1 1 calc R . . C16 C 0.50982(14) 0.31793(9) 0.8774(3) 0.0292(6) Uani 1 1 d . . . H16 H 0.5175 0.3356 0.9662 0.035 Uiso 1 1 calc R . . C17 C 0.5000 0.34436(11) 0.7500 0.0154(6) Uani 1 2 d S . . C18 C 0.5000 0.40047(10) 0.7500 0.0128(5) Uani 1 2 d S . . O19 O 0.53709(7) 0.42386(5) 0.85600(15) 0.0137(3) Uani 1 1 d . . . C20 C 0.69896(9) 0.05142(7) 1.1540(2) 0.0128(4) Uani 1 1 d . . . C21 C 0.70490(10) 0.04289(8) 1.2996(2) 0.0164(4) Uani 1 1 d . . . H21 H 0.6669 0.0403 1.3326 0.020 Uiso 1 1 calc R . . C22 C 0.76656(10) 0.03816(8) 1.3973(2) 0.0157(4) Uani 1 1 d . . . H22 H 0.7702 0.0330 1.4968 0.019 Uiso 1 1 calc R . . C23 C 0.82260(9) 0.04091(7) 1.3506(2) 0.0124(4) Uani 1 1 d . . . C24 C 0.81699(9) 0.05200(8) 1.2061(2) 0.0151(4) Uani 1 1 d . . . H24 H 0.8550 0.0555 1.1737 0.018 Uiso 1 1 calc R . . C25 C 0.75581(10) 0.05786(8) 1.1100(2) 0.0157(4) Uani 1 1 d . . . H25 H 0.7524 0.0664 1.0125 0.019 Uiso 1 1 calc R . . C26 C 0.88857(9) 0.02923(7) 1.4509(2) 0.0118(4) Uani 1 1 d . . . O27 O 0.93401(7) 0.01739(6) 1.39646(17) 0.0158(3) Uani 1 1 d . . . O28 O 0.89525(7) 0.03076(6) 1.58509(15) 0.0169(3) Uani 1 1 d . . . C29 C 0.5000 -0.13368(11) 0.7500 0.0161(6) Uani 1 2 d S . . C30 C 0.44317(11) -0.16065(9) 0.7427(3) 0.0216(4) Uani 1 1 d . . . H30 H 0.4038 -0.1430 0.7371 0.026 Uiso 1 1 calc R . . C31 C 0.44330(12) -0.21315(9) 0.7435(3) 0.0242(5) Uani 1 1 d . . . H31 H 0.4041 -0.2309 0.7396 0.029 Uiso 1 1 calc R . . C32 C 0.5000 -0.23981(12) 0.7500 0.0210(6) Uani 1 2 d S . . C33 C 0.5000 -0.29688(12) 0.7500 0.0239(7) Uani 1 2 d S . . O34 O 0.45064(10) -0.31913(6) 0.7683(2) 0.0317(4) Uani 1 1 d . . . H34 H 0.4607 -0.3487 0.7964 0.048 Uiso 0.50 1 calc PR . . O35 O 0.46964(8) 0.58449(6) 0.86070(16) 0.0216(3) Uani 1 1 d . . . H35A H 0.4745 0.5784 0.9647 0.032 Uiso 1 1 d R . . H35B H 0.4452 0.5643 0.8006 0.032 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.01028(8) 0.00660(9) 0.01043(8) 0.000 -0.00178(5) 0.000 C1 0.0153(13) 0.0079(13) 0.0172(13) 0.000 -0.0029(11) 0.000 C2 0.0173(9) 0.0089(9) 0.0167(10) 0.0014(7) -0.0024(8) -0.0019(7) C3 0.0203(10) 0.0105(10) 0.0301(12) 0.0010(9) -0.0062(9) -0.0044(8) C4 0.0151(9) 0.0152(10) 0.0273(11) -0.0002(9) -0.0069(9) -0.0030(8) C5 0.0098(8) 0.0113(9) 0.0163(9) -0.0002(7) -0.0022(7) -0.0008(7) C6 0.0092(8) 0.0122(9) 0.0127(9) 0.0010(7) -0.0017(7) 0.0008(7) C7 0.0091(9) 0.0118(10) 0.0117(9) 0.0018(7) 0.0002(8) 0.0012(7) C8 0.0158(9) 0.0137(10) 0.0148(9) 0.0032(8) -0.0006(8) 0.0026(7) C9 0.0169(9) 0.0111(9) 0.0177(10) 0.0040(8) 0.0026(8) 0.0025(7) C10 0.0131(8) 0.0068(9) 0.0178(9) 0.0010(7) 0.0031(8) 0.0012(7) C11 0.0164(13) 0.0093(13) 0.0194(14) 0.000 0.0051(11) 0.000 N12 0.0141(8) 0.0060(8) 0.0154(8) 0.0013(6) -0.0031(6) 0.0003(6) N13 0.0104(8) 0.0099(8) 0.0149(9) 0.0011(6) 0.0001(7) 0.0012(6) C14 0.0178(13) 0.0097(14) 0.0159(13) 0.000 -0.0037(11) 0.000 C15 0.0550(16) 0.0099(11) 0.0174(11) 0.0023(8) 0.0041(11) -0.0022(10) C16 0.0567(16) 0.0100(11) 0.0174(11) -0.0016(8) 0.0044(11) -0.0026(10) C17 0.0198(13) 0.0056(13) 0.0171(14) 0.000 -0.0012(11) 0.000 C18 0.0154(12) 0.0068(13) 0.0157(13) 0.000 0.0032(11) 0.000 O19 0.0158(6) 0.0100(7) 0.0128(6) -0.0003(5) -0.0003(6) -0.0002(5) C20 0.0105(8) 0.0104(9) 0.0144(9) -0.0002(7) -0.0017(7) 0.0005(7) C21 0.0108(8) 0.0212(11) 0.0157(9) 0.0038(8) 0.0010(8) 0.0017(7) C22 0.0140(9) 0.0208(11) 0.0103(9) 0.0030(8) -0.0001(7) 0.0030(8) C23 0.0108(8) 0.0118(9) 0.0116(9) 0.0002(7) -0.0023(7) 0.0025(7) C24 0.0118(8) 0.0188(10) 0.0137(9) 0.0021(8) 0.0017(7) 0.0019(7) C25 0.0149(9) 0.0197(10) 0.0099(8) 0.0030(8) -0.0007(7) 0.0045(8) C26 0.0110(8) 0.0083(9) 0.0131(9) 0.0007(7) -0.0021(7) -0.0012(7) O27 0.0098(6) 0.0187(8) 0.0170(7) -0.0002(6) 0.0005(6) 0.0031(5) O28 0.0147(6) 0.0228(8) 0.0098(6) 0.0011(6) -0.0024(5) 0.0027(6) C29 0.0241(14) 0.0083(13) 0.0142(13) 0.000 0.0025(11) 0.000 C30 0.0230(11) 0.0140(11) 0.0274(11) -0.0002(9) 0.0064(9) -0.0021(8) C31 0.0310(12) 0.0137(11) 0.0282(12) 0.0001(9) 0.0085(10) -0.0058(9) C32 0.0379(18) 0.0115(15) 0.0124(13) 0.000 0.0050(13) 0.000 C33 0.0442(19) 0.0117(14) 0.0148(14) 0.000 0.0065(14) 0.000 O34 0.0484(11) 0.0118(8) 0.0372(10) 0.0030(7) 0.0155(9) -0.0020(7) O35 0.0410(9) 0.0114(7) 0.0115(7) -0.0027(6) 0.0058(7) 0.0020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm O27 2.3629(15) 7_657 ? Sm O27 2.3631(15) 8_455 ? Sm O35 2.4203(15) 2_656 ? Sm O35 2.4204(15) . ? Sm O28 2.4243(14) 4_657 ? Sm O28 2.4244(14) 3_454 ? Sm O19 2.5377(14) . ? Sm O19 2.5377(14) 2_656 ? Sm C18 2.904(3) . ? Sm H35B 2.0011 . ? C1 C2 1.401(2) . ? C1 C2 1.401(2) 2_656 ? C1 C14 1.487(4) . ? C2 N12 1.375(3) . ? C2 C3 1.444(3) . ? C3 C4 1.356(3) . ? C3 H3 0.9500 . ? C4 C5 1.437(3) . ? C4 H4 0.9500 . ? C5 N12 1.375(2) . ? C5 C6 1.397(3) . ? C6 C7 1.408(3) . ? C6 C20 1.496(3) . ? C7 N13 1.367(3) . ? C7 C8 1.443(3) . ? C8 C9 1.357(3) . ? C8 H8 0.9500 . ? C9 C10 1.445(3) . ? C9 H9 0.9500 . ? C10 N13 1.374(3) . ? C10 C11 1.407(2) . ? C11 C10 1.407(2) 2_656 ? C11 C29 1.494(4) . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? C14 C15 1.381(3) 2_656 ? C14 C15 1.381(3) . ? C15 C16 1.397(3) . ? C15 H15 0.9500 . ? C16 C17 1.380(3) . ? C16 H16 0.9500 . ? C17 C16 1.380(3) 2_656 ? C17 C18 1.489(4) . ? C18 O19 1.270(2) . ? C18 O19 1.270(2) 2_656 ? C20 C21 1.392(3) . ? C20 C25 1.400(3) . ? C21 C22 1.398(3) . ? C21 H21 0.9500 . ? C22 C23 1.390(3) . ? C22 H22 0.9500 . ? C23 C24 1.396(3) . ? C23 C26 1.505(3) . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O27 1.261(2) . ? C26 O28 1.263(2) . ? O27 Sm 2.3629(15) 7_657 ? O28 Sm 2.4243(14) 3_546 ? C29 C30 1.392(3) 2_656 ? C29 C30 1.392(3) . ? C30 C31 1.394(3) . ? C30 H30 0.9500 . ? C31 C32 1.387(3) . ? C31 H31 0.9500 . ? C32 C31 1.387(3) 2_656 ? C32 C33 1.515(4) . ? C33 O34 1.260(2) 2_656 ? C33 O34 1.260(2) . ? O34 H34 0.8400 . ? O35 H35A 0.9920 . ? O35 H35B 0.8532 . ? 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 O27 Sm O27 144.32(8) 7_657 8_455 ? O27 Sm O35 73.30(5) 7_657 2_656 ? O27 Sm O35 142.07(5) 8_455 2_656 ? O27 Sm O35 142.07(5) 7_657 . ? O27 Sm O35 73.30(5) 8_455 . ? O35 Sm O35 70.16(7) 2_656 . ? O27 Sm O28 82.49(5) 7_657 4_657 ? O27 Sm O28 105.72(5) 8_455 4_657 ? O35 Sm O28 78.01(5) 2_656 4_657 ? O35 Sm O28 80.42(6) . 4_657 ? O27 Sm O28 105.72(5) 7_657 3_454 ? O27 Sm O28 82.48(5) 8_455 3_454 ? O35 Sm O28 80.42(6) 2_656 3_454 ? O35 Sm O28 78.01(5) . 3_454 ? O28 Sm O28 153.57(8) 4_657 3_454 ? O27 Sm O19 78.10(5) 7_657 . ? O27 Sm O19 69.81(5) 8_455 . ? O35 Sm O19 145.31(5) 2_656 . ? O35 Sm O19 130.57(5) . . ? O28 Sm O19 79.18(5) 4_657 . ? O28 Sm O19 126.81(5) 3_454 . ? O27 Sm O19 69.81(5) 7_657 2_656 ? O27 Sm O19 78.10(5) 8_455 2_656 ? O35 Sm O19 130.57(5) 2_656 2_656 ? O35 Sm O19 145.31(5) . 2_656 ? O28 Sm O19 126.82(5) 4_657 2_656 ? O28 Sm O19 79.17(5) 3_454 2_656 ? O19 Sm O19 51.75(6) . 2_656 ? O27 Sm C18 72.16(4) 7_657 . ? O27 Sm C18 72.16(4) 8_455 . ? O35 Sm C18 144.92(4) 2_656 . ? O35 Sm C18 144.92(4) . . ? O28 Sm C18 103.22(4) 4_657 . ? O28 Sm C18 103.22(4) 3_454 . ? O19 Sm C18 25.88(3) . . ? O19 Sm C18 25.88(3) 2_656 . ? O27 Sm H35B 148.2 7_657 . ? O27 Sm H35B 66.0 8_455 . ? O35 Sm H35B 76.2 2_656 . ? O35 Sm H35B 19.4 . . ? O28 Sm H35B 99.8 4_657 . ? O28 Sm H35B 60.0 3_454 . ? O19 Sm H35B 133.7 . . ? O19 Sm H35B 127.6 2_656 . ? C18 Sm H35B 136.3 . . ? C2 C1 C2 124.6(3) . 2_656 ? C2 C1 C14 117.72(14) . . ? C2 C1 C14 117.73(13) 2_656 . ? N12 C2 C1 125.17(19) . . ? N12 C2 C3 108.86(17) . . ? C1 C2 C3 125.9(2) . . ? C4 C3 C2 107.13(19) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? C3 C4 C5 107.65(18) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? N12 C5 C6 125.33(18) . . ? N12 C5 C4 108.89(18) . . ? C6 C5 C4 125.54(18) . . ? C5 C6 C7 125.07(18) . . ? C5 C6 C20 116.97(17) . . ? C7 C6 C20 117.68(17) . . ? N13 C7 C6 124.94(18) . . ? N13 C7 C8 108.63(18) . . ? C6 C7 C8 126.04(19) . . ? C9 C8 C7 107.46(18) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? C8 C9 C10 107.22(18) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? N13 C10 C11 125.4(2) . . ? N13 C10 C9 108.47(18) . . ? C11 C10 C9 125.9(2) . . ? C10 C11 C10 124.4(3) 2_656 . ? C10 C11 C29 117.80(13) 2_656 . ? C10 C11 C29 117.81(13) . . ? C2 N12 C5 107.40(16) . . ? C2 N12 H12 126.3 . . ? C5 N12 H12 126.3 . . ? C7 N13 C10 108.02(17) . . ? C7 N13 H13 126.0 . . ? C10 N13 H13 126.0 . . ? C15 C14 C15 118.2(3) 2_656 . ? C15 C14 C1 120.90(14) 2_656 . ? C15 C14 C1 120.90(14) . . ? C14 C15 C16 121.0(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C16 118.8(3) . 2_656 ? C16 C17 C18 120.58(14) . . ? C16 C17 C18 120.58(14) 2_656 . ? O19 C18 O19 121.4(3) . 2_656 ? O19 C18 C17 119.28(13) . . ? O19 C18 C17 119.28(13) 2_656 . ? O19 C18 Sm 60.72(13) . . ? O19 C18 Sm 60.72(13) 2_656 . ? C17 C18 Sm 180.000(1) . . ? C18 O19 Sm 93.40(13) . . ? C21 C20 C25 118.52(18) . . ? C21 C20 C6 123.01(17) . . ? C25 C20 C6 118.44(17) . . ? C20 C21 C22 120.21(18) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.68(18) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.23(18) . . ? C22 C23 C26 121.09(17) . . ? C24 C23 C26 119.59(17) . . ? C25 C24 C23 119.86(18) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 121.24(18) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? O27 C26 O28 123.36(18) . . ? O27 C26 C23 118.28(17) . . ? O28 C26 C23 118.35(17) . . ? C26 O27 Sm 167.30(14) . 7_657 ? C26 O28 Sm 119.31(12) . 3_546 ? C30 C29 C30 118.1(3) 2_656 . ? C30 C29 C11 120.95(14) 2_656 . ? C30 C29 C11 120.94(14) . . ? C29 C30 C31 120.9(2) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 120.7(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C31 118.6(3) 2_656 . ? C31 C32 C33 120.68(15) 2_656 . ? C31 C32 C33 120.67(15) . . ? O34 C33 O34 124.1(3) 2_656 . ? O34 C33 C32 117.95(16) 2_656 . ? O34 C33 C32 117.95(16) . . ? C33 O34 H34 109.5 . . ? Sm O35 H35A 110.2 . . ? Sm O35 H35B 51.3 . . ? H35A O35 H35B 117.3 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.724 _refine_diff_density_min -1.276 _refine_diff_density_rms 0.092 #====================END============================= data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 627698' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H31 N4 O10 Pr' _chemical_formula_sum 'C48 H31 N4 O10 Pr' _chemical_formula_weight 964.68 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2748(6) _cell_length_b 26.6527(10) _cell_length_c 9.6303(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.503(2) _cell_angle_gamma 90.00 _cell_volume 5262.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6020 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.19 _exptl_crystal_description needles _exptl_crystal_colour purple _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5474 _exptl_absorpt_correction_T_max 0.9085 _exptl_absorpt_process_details 'Blessing 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23020 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.19 _reflns_number_total 6334 _reflns_number_gt 5053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.074. ; _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^)+(0.0798P)^2^+0.9255P] 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 6333 _refine_ls_number_parameters 291 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.055 _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 Pr Pr 0.5000 0.510444(11) 0.7500 0.01962(10) Uani 1 2 d S . . C1 C 0.5000 0.1820(2) 0.7500 0.0228(10) Uani 1 2 d S . . C2 C 0.55407(17) 0.15748(14) 0.8407(4) 0.0255(8) Uani 1 1 d . . . C3 C 0.61251(19) 0.18122(15) 0.9239(4) 0.0314(9) Uani 1 1 d . . . H3 H 0.6230 0.2159 0.9234 0.038 Uiso 1 1 calc R . . C4 C 0.64996(19) 0.14484(15) 1.0034(4) 0.0326(9) Uani 1 1 d . . . H4 H 0.6915 0.1495 1.0696 0.039 Uiso 1 1 calc R . . C5 C 0.61589(17) 0.09809(14) 0.9703(4) 0.0236(7) Uani 1 1 d . . . C6 C 0.63490(16) 0.05244(14) 1.0390(3) 0.0209(7) Uani 1 1 d . . . C7 C 0.60165(17) 0.00667(13) 1.0041(4) 0.0191(7) Uani 1 1 d . . . C8 C 0.61766(17) -0.04029(15) 1.0795(4) 0.0253(8) Uani 1 1 d . . . H8 H 0.6493 -0.0451 1.1691 0.030 Uiso 1 1 calc R . . C9 C 0.57954(17) -0.07642(14) 1.0000(4) 0.0229(7) Uani 1 1 d . . . H9 H 0.5788 -0.1109 1.0243 0.028 Uiso 1 1 calc R . . C10 C 0.53990(16) -0.05230(14) 0.8703(4) 0.0206(7) Uani 1 1 d . . . C11 C 0.5000 -0.07693(19) 0.7500 0.0204(10) Uani 1 2 d S . . N12 N 0.55806(14) 0.10692(11) 0.8683(3) 0.0213(6) Uani 1 1 d . . . H12 H 0.5288 0.0842 0.8279 0.026 Uiso 0.50 1 calc PR . . N13 N 0.55261(14) -0.00181(11) 0.8809(3) 0.0219(7) Uani 1 1 d . . . H13 H 0.5327 0.0212 0.8192 0.026 Uiso 0.50 1 calc PR . . C14 C 0.5000 0.2383(2) 0.7500 0.0245(11) Uani 1 2 d S . . C15 C 0.4918(2) 0.26488(16) 0.6246(4) 0.0391(10) Uani 1 1 d . . . H15 H 0.4870 0.2473 0.5366 0.047 Uiso 1 1 calc R . . C16 C 0.4905(2) 0.31660(15) 0.6233(4) 0.0382(10) Uani 1 1 d . . . H16 H 0.4829 0.3340 0.5342 0.046 Uiso 1 1 calc R . . C17 C 0.5000 0.3435(2) 0.7500 0.0256(11) Uani 1 2 d S . . C18 C 0.5000 0.3992(2) 0.7500 0.0202(10) Uani 1 2 d S . . O19 O 0.53698(12) 0.42275(10) 0.8554(2) 0.0233(5) Uani 1 1 d . . . C20 C 0.69932(16) 0.05146(14) 1.1530(4) 0.0219(7) Uani 1 1 d . . . C21 C 0.70376(17) 0.04266(15) 1.2973(4) 0.0255(8) Uani 1 1 d . . . H21 H 0.6651 0.0394 1.3282 0.031 Uiso 1 1 calc R . . C22 C 0.76456(16) 0.03850(15) 1.3972(4) 0.0244(8) Uani 1 1 d . . . H22 H 0.7672 0.0336 1.4963 0.029 Uiso 1 1 calc R . . C23 C 0.82125(16) 0.04153(14) 1.3518(3) 0.0217(7) Uani 1 1 d . . . C24 C 0.81714(17) 0.05248(15) 1.2085(4) 0.0244(8) Uani 1 1 d . . . H24 H 0.8558 0.0561 1.1778 0.029 Uiso 1 1 calc R . . C25 C 0.75661(17) 0.05814(15) 1.1105(4) 0.0235(7) Uani 1 1 d . . . H25 H 0.7541 0.0667 1.0133 0.028 Uiso 1 1 calc R . . C26 C 0.88658(17) 0.02999(15) 1.4546(4) 0.0248(7) Uani 1 1 d . . . O27 O 0.93339(12) 0.01770(10) 1.4046(3) 0.0261(6) Uani 1 1 d . . . O28 O 0.89197(12) 0.03231(11) 1.5888(2) 0.0279(6) Uani 1 1 d . . . C29 C 0.5000 -0.1331(2) 0.7500 0.0230(10) Uani 1 2 d S . . C30 C 0.5573(2) -0.16014(15) 0.7585(4) 0.0309(8) Uani 1 1 d . . . H30 H 0.5969 -0.1426 0.7661 0.037 Uiso 1 1 calc R . . C31 C 0.5569(2) -0.21231(15) 0.7562(4) 0.0323(9) Uani 1 1 d . . . H31 H 0.5964 -0.2295 0.7588 0.039 Uiso 1 1 calc R . . C32 C 0.5000 -0.24101(18) 0.7500 0.0312(12) Uani 1 2 d SD . . C33 C 0.5000 -0.29409(18) 0.7500 0.0353(14) Uani 1 2 d SD . . O34 O 0.54989(16) -0.31806(12) 0.7326(3) 0.0427(7) Uani 1 1 d . . . H34 H 0.5387 -0.3472 0.7033 0.064 Uiso 0.50 1 calc PR . . O35 O 0.53061(15) 0.58671(10) 0.6378(3) 0.0341(7) Uani 1 1 d . . . H35A H 0.5329 0.5839 0.5389 0.051 Uiso 1 1 d R . . H35B H 0.5527 0.5619 0.6875 0.051 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr 0.01938(15) 0.01589(16) 0.01999(15) 0.000 -0.00097(9) 0.000 C1 0.026(3) 0.017(3) 0.019(2) 0.000 -0.0030(18) 0.000 C2 0.0260(19) 0.019(2) 0.0263(18) 0.0027(14) -0.0012(14) 0.0003(14) C3 0.032(2) 0.016(2) 0.038(2) -0.0010(16) -0.0047(16) -0.0048(15) C4 0.0246(19) 0.027(2) 0.037(2) -0.0002(16) -0.0089(15) -0.0065(16) C5 0.0220(17) 0.021(2) 0.0237(17) -0.0013(14) -0.0010(13) 0.0021(14) C6 0.0177(16) 0.0213(19) 0.0201(16) 0.0005(13) -0.0011(12) 0.0020(13) C7 0.0182(16) 0.0182(17) 0.0179(15) 0.0016(13) -0.0005(12) 0.0015(13) C8 0.0226(17) 0.025(2) 0.0242(17) 0.0019(15) -0.0007(13) 0.0024(15) C9 0.0234(17) 0.0199(19) 0.0225(16) 0.0063(14) 0.0007(13) 0.0029(14) C10 0.0191(16) 0.0162(18) 0.0243(17) 0.0026(13) 0.0022(13) 0.0002(13) C11 0.022(2) 0.016(3) 0.023(2) 0.000 0.0060(18) 0.000 N12 0.0224(15) 0.0160(16) 0.0207(14) 0.0015(11) -0.0026(11) 0.0003(12) N13 0.0172(14) 0.0222(18) 0.0237(14) 0.0007(12) 0.0008(11) 0.0004(11) C14 0.024(2) 0.021(3) 0.025(2) 0.000 0.0006(19) 0.000 C15 0.073(3) 0.018(2) 0.0218(18) -0.0019(15) 0.0048(18) 0.003(2) C16 0.074(3) 0.016(2) 0.0225(19) 0.0048(15) 0.0096(19) 0.000(2) C17 0.033(3) 0.017(3) 0.024(2) 0.000 0.002(2) 0.000 C18 0.022(2) 0.022(3) 0.018(2) 0.000 0.0076(17) 0.000 O19 0.0255(13) 0.0189(14) 0.0225(12) 0.0007(10) 0.0011(9) -0.0011(10) C20 0.0197(17) 0.0188(19) 0.0219(16) -0.0016(13) -0.0039(13) 0.0023(13) C21 0.0206(17) 0.029(2) 0.0241(17) 0.0012(15) 0.0010(13) 0.0015(14) C22 0.0202(17) 0.031(2) 0.0190(16) 0.0036(14) -0.0007(12) 0.0036(15) C23 0.0204(16) 0.0209(19) 0.0196(16) 0.0002(13) -0.0018(12) 0.0019(13) C24 0.0199(17) 0.029(2) 0.0219(16) -0.0013(14) 0.0008(13) 0.0020(14) C25 0.0227(17) 0.026(2) 0.0195(16) 0.0018(14) 0.0010(13) 0.0031(14) C26 0.0215(17) 0.0174(18) 0.0309(18) 0.0015(15) -0.0014(13) -0.0004(14) O27 0.0181(12) 0.0274(17) 0.0301(13) -0.0007(10) 0.0019(10) 0.0012(10) O28 0.0238(13) 0.0385(17) 0.0168(11) 0.0040(11) -0.0026(9) 0.0022(12) C29 0.029(3) 0.019(3) 0.017(2) 0.000 -0.0003(18) 0.000 C30 0.033(2) 0.022(2) 0.035(2) -0.0012(16) 0.0045(16) 0.0005(16) C31 0.037(2) 0.021(2) 0.039(2) -0.0023(16) 0.0096(17) 0.0044(17) C32 0.044(3) 0.030(3) 0.019(2) 0.000 0.007(2) 0.000 C33 0.055(4) 0.028(3) 0.021(3) 0.000 0.006(2) 0.000 O34 0.060(2) 0.0229(17) 0.0440(18) -0.0017(13) 0.0111(15) 0.0036(14) O35 0.0584(19) 0.0204(15) 0.0209(12) 0.0036(11) 0.0060(12) -0.0040(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr O27 2.432(3) 7_657 ? Pr O27 2.432(3) 8_455 ? Pr O35 2.470(3) . ? Pr O35 2.470(3) 2_656 ? Pr O28 2.475(2) 3_454 ? Pr O28 2.475(2) 4_657 ? Pr O19 2.586(3) 2_656 ? Pr O19 2.586(3) . ? Pr C18 2.965(5) . ? Pr H35B 1.9651 . ? C1 C2 1.405(4) . ? C1 C2 1.405(4) 2_656 ? C1 C14 1.501(8) . ? C2 N12 1.372(5) . ? C2 C3 1.434(5) . ? C3 C4 1.355(5) . ? C3 H3 0.9500 . ? C4 C5 1.434(5) . ? C4 H4 0.9500 . ? C5 N12 1.374(4) . ? C5 C6 1.392(5) . ? C6 C7 1.405(5) . ? C6 C20 1.510(4) . ? C7 N13 1.373(4) . ? C7 C8 1.442(5) . ? C8 C9 1.356(5) . ? C8 H8 0.9500 . ? C9 C10 1.457(4) . ? C9 H9 0.9500 . ? C10 N13 1.371(4) . ? C10 C11 1.403(4) . ? C11 C10 1.403(4) 2_656 ? C11 C29 1.497(7) . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? C14 C15 1.370(5) . ? C14 C15 1.370(5) 2_656 ? C15 C16 1.379(6) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C16 1.383(5) 2_656 ? C17 C18 1.483(7) . ? C18 O19 1.271(4) . ? C18 O19 1.271(3) 2_656 ? C20 C21 1.387(5) . ? C20 C25 1.397(5) . ? C21 C22 1.395(4) . ? C21 H21 0.9500 . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 C24 1.389(5) . ? C23 C26 1.507(4) . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O27 1.260(5) . ? C26 O28 1.268(4) . ? O27 Pr 2.432(3) 7_657 ? O28 Pr 2.475(2) 3_546 ? C29 C30 1.399(5) . ? C29 C30 1.399(5) 2_656 ? C30 C31 1.391(6) . ? C30 H30 0.9500 . ? C31 C32 1.420(5) . ? C31 H31 0.9500 . ? C32 C31 1.420(5) 2_656 ? C32 C33 1.415(7) . ? C33 O34 1.287(4) 2_656 ? C33 O34 1.287(4) . ? O34 H34 0.8400 . ? O35 H35A 0.9695 . ? O35 H35B 0.8766 . ? 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 O27 Pr O27 144.07(12) 7_657 8_455 ? O27 Pr O35 73.80(9) 7_657 . ? O27 Pr O35 141.87(9) 8_455 . ? O27 Pr O35 141.87(9) 7_657 2_656 ? O27 Pr O35 73.80(9) 8_455 2_656 ? O35 Pr O35 69.23(13) . 2_656 ? O27 Pr O28 106.49(8) 7_657 3_454 ? O27 Pr O28 82.03(8) 8_455 3_454 ? O35 Pr O28 80.85(10) . 3_454 ? O35 Pr O28 76.79(9) 2_656 3_454 ? O27 Pr O28 82.03(8) 7_657 4_657 ? O27 Pr O28 106.49(8) 8_455 4_657 ? O35 Pr O28 76.79(9) . 4_657 ? O35 Pr O28 80.85(10) 2_656 4_657 ? O28 Pr O28 152.76(14) 3_454 4_657 ? O27 Pr O19 69.32(8) 7_657 2_656 ? O27 Pr O19 78.20(8) 8_455 2_656 ? O35 Pr O19 131.34(8) . 2_656 ? O35 Pr O19 145.85(9) 2_656 2_656 ? O28 Pr O19 80.36(9) 3_454 2_656 ? O28 Pr O19 126.39(9) 4_657 2_656 ? O27 Pr O19 78.20(8) 7_657 . ? O27 Pr O19 69.32(8) 8_455 . ? O35 Pr O19 145.85(9) . . ? O35 Pr O19 131.34(8) 2_656 . ? O28 Pr O19 126.39(9) 3_454 . ? O28 Pr O19 80.36(9) 4_657 . ? O19 Pr O19 50.62(10) 2_656 . ? O27 Pr C18 72.04(6) 7_657 . ? O27 Pr C18 72.04(6) 8_455 . ? O35 Pr C18 145.39(7) . . ? O35 Pr C18 145.39(7) 2_656 . ? O28 Pr C18 103.62(7) 3_454 . ? O28 Pr C18 103.62(7) 4_657 . ? O19 Pr C18 25.31(5) 2_656 . ? O19 Pr C18 25.31(5) . . ? O27 Pr H35B 63.5 7_657 . ? O27 Pr H35B 151.2 8_455 . ? O35 Pr H35B 18.7 . . ? O35 Pr H35B 78.4 2_656 . ? O28 Pr H35B 98.9 3_454 . ? O28 Pr H35B 61.1 4_657 . ? O19 Pr H35B 130.5 2_656 . ? O19 Pr H35B 127.7 . . ? C18 Pr H35B 134.2 . . ? C2 C1 C2 124.7(5) . 2_656 ? C2 C1 C14 117.7(2) . . ? C2 C1 C14 117.7(2) 2_656 . ? N12 C2 C1 125.1(3) . . ? N12 C2 C3 109.0(3) . . ? C1 C2 C3 125.9(4) . . ? C4 C3 C2 106.9(3) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? C3 C4 C5 108.1(3) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? N12 C5 C6 125.5(3) . . ? N12 C5 C4 108.2(3) . . ? C6 C5 C4 126.0(3) . . ? C5 C6 C7 125.5(3) . . ? C5 C6 C20 116.9(3) . . ? C7 C6 C20 117.4(3) . . ? N13 C7 C6 124.6(3) . . ? N13 C7 C8 108.4(3) . . ? C6 C7 C8 126.7(3) . . ? C9 C8 C7 107.8(3) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? C8 C9 C10 107.0(3) . . ? C8 C9 H9 126.5 . . ? C10 C9 H9 126.5 . . ? N13 C10 C11 125.8(3) . . ? N13 C10 C9 108.2(3) . . ? C11 C10 C9 125.8(4) . . ? C10 C11 C10 124.2(5) . 2_656 ? C10 C11 C29 117.9(2) . . ? C10 C11 C29 117.9(2) 2_656 . ? C2 N12 C5 107.7(3) . . ? C2 N12 H12 126.2 . . ? C5 N12 H12 126.2 . . ? C10 N13 C7 108.4(3) . . ? C10 N13 H13 125.8 . . ? C7 N13 H13 125.8 . . ? C15 C14 C15 117.7(5) . 2_656 ? C15 C14 C1 121.2(3) . . ? C15 C14 C1 121.2(3) 2_656 . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C16 117.5(5) 2_656 . ? C16 C17 C18 121.3(3) 2_656 . ? C16 C17 C18 121.3(3) . . ? O19 C18 O19 120.8(5) . 2_656 ? O19 C18 C17 119.6(2) . . ? O19 C18 C17 119.6(2) 2_656 . ? O19 C18 Pr 60.4(2) . . ? O19 C18 Pr 60.4(2) 2_656 . ? C17 C18 Pr 180.0 . . ? C18 O19 Pr 94.3(2) . . ? C21 C20 C25 118.9(3) . . ? C21 C20 C6 122.5(3) . . ? C25 C20 C6 118.6(3) . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 C26 119.9(3) . . ? C22 C23 C26 120.4(3) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.7(3) . . ? C24 C25 H25 119.6 . . ? C20 C25 H25 119.6 . . ? O27 C26 O28 122.5(3) . . ? O27 C26 C23 119.1(3) . . ? O28 C26 C23 118.4(3) . . ? C26 O27 Pr 164.5(2) . 7_657 ? C26 O28 Pr 116.3(2) . 3_546 ? C30 C29 C30 117.9(5) . 2_656 ? C30 C29 C11 121.0(3) . . ? C30 C29 C11 121.0(3) 2_656 . ? C31 C30 C29 120.9(4) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C32 C31 C30 122.7(4) . . ? C32 C31 H31 118.7 . . ? C30 C31 H31 118.7 . . ? C31 C32 C31 114.8(5) . 2_656 ? C31 C32 C33 122.6(2) . . ? C31 C32 C33 122.6(2) 2_656 . ? O34 C33 O34 120.5(5) 2_656 . ? O34 C33 C32 119.7(2) 2_656 . ? O34 C33 C32 119.7(2) . . ? C33 O34 H34 109.5 . . ? Pr O35 H35A 117.0 . . ? Pr O35 H35B 46.0 . . ? H35A O35 H35B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.564 _refine_diff_density_min -1.764 _refine_diff_density_rms 0.130 #==========================END========================== data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 627699' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H31 Gd N4 O10' _chemical_formula_sum 'C48 H31 Gd N4 O10' _chemical_formula_weight 981.02 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3667(4) _cell_length_b 26.5131(6) _cell_length_c 9.6096(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.1315(16) _cell_angle_gamma 90.00 _cell_volume 5229.47(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6060 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.26 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6200 _exptl_absorpt_correction_T_max 0.8792 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24189 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.26 _reflns_number_total 6269 _reflns_number_gt 5154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.064. ; _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^)+(0.0541P)^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 6269 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Gd Gd 0.5000 0.510150(9) 0.7500 0.01537(8) Uani 1 2 d S . . C1 C 0.5000 -0.07742(17) 0.7500 0.0172(9) Uani 1 2 d S . . C2 C 0.54040(15) -0.05269(13) 0.8722(3) 0.0194(7) Uani 1 1 d . . . C3 C 0.57982(15) -0.07648(13) 1.0013(3) 0.0201(7) Uani 1 1 d . . . H3 H 0.5792 -0.1112 1.0254 0.024 Uiso 1 1 calc R . . C4 C 0.61809(15) -0.04032(13) 1.0825(3) 0.0203(7) Uani 1 1 d . . . H4 H 0.6498 -0.0451 1.1728 0.024 Uiso 1 1 calc R . . C5 C 0.60147(15) 0.00650(12) 1.0061(3) 0.0160(6) Uani 1 1 d . . . C6 C 0.63441(14) 0.05292(13) 1.0431(3) 0.0175(7) Uani 1 1 d . . . C7 C 0.61521(15) 0.09883(13) 0.9747(3) 0.0192(7) Uani 1 1 d . . . C8 C 0.64995(16) 0.14598(14) 1.0088(4) 0.0256(8) Uani 1 1 d . . . H8 H 0.6917 0.1506 1.0752 0.031 Uiso 1 1 calc R . . C9 C 0.61222(17) 0.18237(14) 0.9291(4) 0.0271(8) Uani 1 1 d . . . H9 H 0.6226 0.2172 0.9297 0.033 Uiso 1 1 calc R . . C10 C 0.55316(15) 0.15866(12) 0.8425(3) 0.0186(7) Uani 1 1 d . . . C11 C 0.5000 0.18362(18) 0.7500 0.0203(10) Uani 1 2 d S . . N12 N 0.55297(13) -0.00169(10) 0.8819(3) 0.0183(6) Uani 1 1 d . . . H12 H 0.5333 0.0214 0.8193 0.022 Uiso 0.50 1 calc PR . . N13 N 0.55811(13) 0.10787(10) 0.8700(3) 0.0191(6) Uani 1 1 d . . . H13 H 0.5294 0.0849 0.8274 0.023 Uiso 0.50 1 calc PR . . C14 C 0.5000 -0.13412(18) 0.7500 0.0214(10) Uani 1 2 d S . . C15 C 0.55717(18) -0.16093(14) 0.7596(4) 0.0263(8) Uani 1 1 d . . . H15 H 0.5965 -0.1431 0.7664 0.032 Uiso 1 1 calc R . . C16 C 0.55759(19) -0.21314(14) 0.7596(4) 0.0286(8) Uani 1 1 d . . . H16 H 0.5969 -0.2308 0.7660 0.034 Uiso 1 1 calc R . . C17 C 0.5000 -0.2398(2) 0.7500 0.0285(12) Uani 1 2 d S . . C18 C 0.5000 -0.2969(2) 0.7500 0.0355(14) Uani 1 2 d S . . O19 O 0.44952(15) -0.31945(10) 0.7630(3) 0.0376(7) Uani 1 1 d . . . H19 H 0.4589 -0.3486 0.7869 0.052 Uiso 0.50 1 d P . . C20 C 0.69921(14) 0.05135(12) 1.1546(3) 0.0177(7) Uani 1 1 d . . . C21 C 0.75594(15) 0.05740(14) 1.1091(3) 0.0213(7) Uani 1 1 d . . . H21 H 0.7521 0.0659 1.0111 0.026 Uiso 1 1 calc R . . C22 C 0.81700(15) 0.05125(13) 1.2040(3) 0.0202(7) Uani 1 1 d . . . H22 H 0.8546 0.0540 1.1702 0.024 Uiso 1 1 calc R . . C23 C 0.82353(15) 0.04098(12) 1.3490(3) 0.0174(6) Uani 1 1 d . . . C24 C 0.76828(15) 0.03904(13) 1.3976(3) 0.0195(7) Uani 1 1 d . . . H24 H 0.7726 0.0342 1.4978 0.023 Uiso 1 1 calc R . . C25 C 0.70656(15) 0.04404(13) 1.3015(3) 0.0216(7) Uani 1 1 d . . . H25 H 0.6692 0.0425 1.3365 0.026 Uiso 1 1 calc R . . C26 C 0.88963(15) 0.02923(13) 1.4488(3) 0.0175(6) Uani 1 1 d . . . O27 O 0.89720(11) 0.03094(10) 1.5834(2) 0.0225(5) Uani 1 1 d . . . O28 O 0.93461(10) 0.01691(8) 1.3933(2) 0.0193(5) Uani 1 1 d . . . C29 C 0.5000 0.23923(19) 0.7500 0.0210(10) Uani 1 2 d S . . C30 C 0.4924(2) 0.26618(15) 0.6242(4) 0.0365(10) Uani 1 1 d . . . H30 H 0.4878 0.2486 0.5357 0.044 Uiso 1 1 calc R . . C31 C 0.4912(2) 0.31861(15) 0.6238(4) 0.0391(10) Uani 1 1 d . . . H31 H 0.4843 0.3363 0.5348 0.047 Uiso 1 1 calc R . . C32 C 0.5000 0.34514(19) 0.7500 0.0217(10) Uani 1 2 d S . . C33 C 0.5000 0.40130(18) 0.7500 0.0176(9) Uani 1 2 d S . . O34 O 0.46290(10) 0.42489(8) 0.6441(2) 0.0182(5) Uani 1 1 d . . . O35 O 0.53080(13) 0.58433(9) 0.6395(2) 0.0270(6) Uani 1 1 d . . . H35A H 0.5415 0.5795 0.5493 0.040 Uiso 1 1 d R . . H35B H 0.5523 0.5634 0.7058 0.040 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.01469(12) 0.01308(13) 0.01435(12) 0.000 -0.00259(8) 0.000 C1 0.018(2) 0.012(2) 0.021(2) 0.000 0.0037(19) 0.000 C2 0.0180(16) 0.0159(18) 0.0222(16) 0.0014(13) 0.0021(13) 0.0004(13) C3 0.0208(16) 0.0152(18) 0.0214(16) 0.0009(13) 0.0012(14) 0.0009(13) C4 0.0189(16) 0.0194(19) 0.0202(16) -0.0003(13) 0.0016(13) 0.0045(13) C5 0.0127(14) 0.0172(17) 0.0161(14) 0.0001(12) 0.0005(12) 0.0008(12) C6 0.0137(15) 0.0188(18) 0.0172(15) 0.0008(12) -0.0005(13) 0.0004(12) C7 0.0129(15) 0.0176(18) 0.0230(16) -0.0014(13) -0.0016(13) -0.0012(13) C8 0.0182(17) 0.023(2) 0.0266(17) -0.0025(14) -0.0086(14) -0.0034(14) C9 0.0248(18) 0.0146(19) 0.0333(19) -0.0004(14) -0.0063(15) -0.0049(14) C10 0.0210(16) 0.0124(17) 0.0189(15) -0.0014(12) -0.0004(14) -0.0018(13) C11 0.021(2) 0.015(3) 0.020(2) 0.000 -0.0021(19) 0.000 N12 0.0141(13) 0.0171(18) 0.0202(13) 0.0000(10) -0.0011(11) 0.0011(10) N13 0.0164(13) 0.0142(15) 0.0213(14) 0.0011(11) -0.0039(11) -0.0015(11) C14 0.029(3) 0.016(3) 0.017(2) 0.000 0.004(2) 0.000 C15 0.0286(19) 0.020(2) 0.0304(19) -0.0011(15) 0.0080(16) -0.0009(15) C16 0.039(2) 0.017(2) 0.0287(19) 0.0010(14) 0.0086(17) 0.0035(16) C17 0.045(3) 0.023(3) 0.014(2) 0.000 0.002(2) 0.000 C18 0.066(4) 0.025(3) 0.014(2) 0.000 0.008(3) 0.000 O19 0.0615(19) 0.0125(14) 0.0384(15) 0.0039(11) 0.0130(14) -0.0028(13) C20 0.0157(15) 0.0140(17) 0.0191(15) -0.0015(12) -0.0026(13) -0.0003(12) C21 0.0178(16) 0.029(2) 0.0137(14) 0.0011(13) -0.0017(13) 0.0024(14) C22 0.0158(15) 0.0235(19) 0.0191(15) 0.0029(13) 0.0014(13) 0.0025(13) C23 0.0153(15) 0.0159(18) 0.0169(14) -0.0010(12) -0.0024(13) 0.0006(12) C24 0.0206(16) 0.0219(19) 0.0141(14) 0.0024(13) 0.0015(13) 0.0011(13) C25 0.0160(15) 0.028(2) 0.0204(16) 0.0037(13) 0.0040(13) 0.0012(13) C26 0.0196(16) 0.0140(16) 0.0136(14) 0.0016(12) -0.0044(13) -0.0020(13) O27 0.0187(11) 0.0282(14) 0.0165(11) 0.0029(10) -0.0018(9) 0.0032(10) O28 0.0133(11) 0.0221(15) 0.0203(11) -0.0011(9) 0.0009(9) 0.0019(9) C29 0.016(2) 0.018(3) 0.022(2) 0.000 -0.0060(19) 0.000 C30 0.067(3) 0.023(2) 0.0183(17) -0.0031(15) 0.0096(19) 0.0041(19) C31 0.077(3) 0.019(2) 0.0194(18) 0.0003(15) 0.010(2) 0.000(2) C32 0.022(2) 0.016(3) 0.023(2) 0.000 -0.001(2) 0.000 C33 0.018(2) 0.017(2) 0.019(2) 0.000 0.0075(19) 0.000 O34 0.0202(11) 0.0150(12) 0.0158(10) 0.0013(9) -0.0009(9) -0.0004(9) O35 0.0463(15) 0.0184(14) 0.0151(11) 0.0034(9) 0.0067(11) -0.0018(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O28 2.331(2) 7_657 ? Gd O28 2.331(2) 8_455 ? Gd O27 2.395(2) 4_657 ? Gd O27 2.395(2) 3_454 ? Gd O35 2.412(2) 2_656 ? Gd O35 2.412(2) . ? Gd O34 2.515(2) 2_656 ? Gd O34 2.515(2) . ? Gd C33 2.886(5) . ? Gd H35B 1.9197 . ? C1 C2 1.411(4) 2_656 ? C1 C2 1.411(4) . ? C1 C14 1.503(7) . ? C2 N12 1.377(4) . ? C2 C3 1.437(4) . ? C3 C4 1.357(5) . ? C3 H3 0.9500 . ? C4 C5 1.436(5) . ? C4 H4 0.9500 . ? C5 N12 1.363(4) . ? C5 C6 1.413(5) . ? C6 C7 1.390(5) . ? C6 C20 1.497(4) . ? C7 N13 1.370(4) . ? C7 C8 1.444(5) . ? C8 C9 1.351(5) . ? C8 H8 0.9500 . ? C9 C10 1.448(5) . ? C9 H9 0.9500 . ? C10 N13 1.371(4) . ? C10 C11 1.399(4) . ? C11 C10 1.399(4) 2_656 ? C11 C29 1.475(7) . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? C14 C15 1.394(4) . ? C14 C15 1.394(4) 2_656 ? C15 C16 1.384(5) . ? C15 H15 0.9500 . ? C16 C17 1.400(5) . ? C16 H16 0.9500 . ? C17 C16 1.400(5) 2_656 ? C17 C18 1.512(8) . ? C18 O19 1.270(4) 2_656 ? C18 O19 1.270(4) . ? O19 H19 0.8147 . ? C20 C25 1.390(4) . ? C20 C21 1.407(4) . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 C26 1.503(4) . ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O27 1.258(4) . ? C26 O28 1.265(4) . ? O27 Gd 2.395(2) 3_546 ? O28 Gd 2.331(2) 7_657 ? C29 C30 1.375(5) 2_656 ? C29 C30 1.375(5) . ? C30 C31 1.390(6) . ? C30 H30 0.9500 . ? C31 C32 1.369(4) . ? C31 H31 0.9500 . ? C32 C31 1.369(4) 2_656 ? C32 C33 1.489(7) . ? C33 O34 1.268(3) 2_656 ? C33 O34 1.268(3) . ? O35 H35A 0.9647 . ? O35 H35B 0.8735 . ? 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 O28 Gd O28 144.14(11) 7_657 8_455 ? O28 Gd O27 82.93(8) 7_657 4_657 ? O28 Gd O27 105.35(8) 8_455 4_657 ? O28 Gd O27 105.35(8) 7_657 3_454 ? O28 Gd O27 82.92(8) 8_455 3_454 ? O27 Gd O27 153.40(12) 4_657 3_454 ? O28 Gd O35 142.45(8) 7_657 2_656 ? O28 Gd O35 73.09(8) 8_455 2_656 ? O27 Gd O35 80.20(8) 4_657 2_656 ? O27 Gd O35 78.17(8) 3_454 2_656 ? O28 Gd O35 73.09(8) 7_657 . ? O28 Gd O35 142.45(8) 8_455 . ? O27 Gd O35 78.17(8) 4_657 . ? O27 Gd O35 80.20(8) 3_454 . ? O35 Gd O35 70.74(11) 2_656 . ? O28 Gd O34 77.84(7) 7_657 2_656 ? O28 Gd O34 69.97(7) 8_455 2_656 ? O27 Gd O34 78.98(8) 4_657 2_656 ? O27 Gd O34 127.20(8) 3_454 2_656 ? O35 Gd O34 130.43(7) 2_656 2_656 ? O35 Gd O34 144.81(8) . 2_656 ? O28 Gd O34 69.97(7) 7_657 . ? O28 Gd O34 77.83(7) 8_455 . ? O27 Gd O34 127.20(8) 4_657 . ? O27 Gd O34 78.98(8) 3_454 . ? O35 Gd O34 144.81(8) 2_656 . ? O35 Gd O34 130.43(7) . . ? O34 Gd O34 52.01(10) 2_656 . ? O28 Gd C33 72.07(6) 7_657 . ? O28 Gd C33 72.07(6) 8_455 . ? O27 Gd C33 103.30(6) 4_657 . ? O27 Gd C33 103.30(6) 3_454 . ? O35 Gd C33 144.63(6) 2_656 . ? O35 Gd C33 144.63(6) . . ? O34 Gd C33 26.01(5) 2_656 . ? O34 Gd C33 26.01(5) . . ? O28 Gd H35B 67.3 7_657 . ? O28 Gd H35B 147.0 8_455 . ? O27 Gd H35B 59.8 4_657 . ? O27 Gd H35B 99.5 3_454 . ? O35 Gd H35B 75.2 2_656 . ? O35 Gd H35B 19.3 . . ? O34 Gd H35B 127.8 2_656 . ? O34 Gd H35B 135.1 . . ? C33 Gd H35B 137.3 . . ? C2 C1 C2 124.6(4) 2_656 . ? C2 C1 C14 117.7(2) 2_656 . ? C2 C1 C14 117.7(2) . . ? N12 C2 C1 125.1(3) . . ? N12 C2 C3 108.4(3) . . ? C1 C2 C3 126.2(3) . . ? C4 C3 C2 107.5(3) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? C3 C4 C5 107.0(3) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N12 C5 C6 124.3(3) . . ? N12 C5 C4 109.3(3) . . ? C6 C5 C4 126.1(3) . . ? C7 C6 C5 125.6(3) . . ? C7 C6 C20 117.1(3) . . ? C5 C6 C20 116.9(3) . . ? N13 C7 C6 125.9(3) . . ? N13 C7 C8 108.2(3) . . ? C6 C7 C8 125.8(3) . . ? C9 C8 C7 107.5(3) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 C10 107.7(3) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? N13 C10 C11 126.3(3) . . ? N13 C10 C9 107.9(3) . . ? C11 C10 C9 125.7(3) . . ? C10 C11 C10 123.5(4) 2_656 . ? C10 C11 C29 118.2(2) 2_656 . ? C10 C11 C29 118.2(2) . . ? C5 N12 C2 107.6(3) . . ? C5 N12 H12 126.2 . . ? C2 N12 H12 126.2 . . ? C7 N13 C10 108.6(3) . . ? C7 N13 H13 125.7 . . ? C10 N13 H13 125.7 . . ? C15 C14 C15 118.7(5) . 2_656 ? C15 C14 C1 120.7(2) . . ? C15 C14 C1 120.7(2) 2_656 . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C16 119.3(5) . 2_656 ? C16 C17 C18 120.4(2) . . ? C16 C17 C18 120.4(2) 2_656 . ? O19 C18 O19 123.8(5) 2_656 . ? O19 C18 C17 118.1(3) 2_656 . ? O19 C18 C17 118.1(3) . . ? C18 O19 H19 109.0 . . ? C25 C20 C21 117.9(3) . . ? C25 C20 C6 123.5(3) . . ? C21 C20 C6 118.6(3) . . ? C22 C21 C20 121.3(3) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.2(3) . . ? C24 C23 C26 121.0(3) . . ? C22 C23 C26 119.7(3) . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C20 C25 C24 120.5(3) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? O27 C26 O28 123.2(3) . . ? O27 C26 C23 118.6(3) . . ? O28 C26 C23 118.3(3) . . ? C26 O27 Gd 120.7(2) . 3_546 ? C26 O28 Gd 168.3(2) . 7_657 ? C30 C29 C30 117.4(5) 2_656 . ? C30 C29 C11 121.3(2) 2_656 . ? C30 C29 C11 121.3(2) . . ? C29 C30 C31 121.3(3) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 120.9(4) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C31 118.2(5) 2_656 . ? C31 C32 C33 120.9(2) 2_656 . ? C31 C32 C33 120.9(2) . . ? O34 C33 O34 120.9(4) 2_656 . ? O34 C33 C32 119.6(2) 2_656 . ? O34 C33 C32 119.6(2) . . ? O34 C33 Gd 60.4(2) 2_656 . ? O34 C33 Gd 60.4(2) . . ? C32 C33 Gd 180.000(1) . . ? C33 O34 Gd 93.6(2) . . ? Gd O35 H35A 116.6 . . ? Gd O35 H35B 46.6 . . ? H35A O35 H35B 111.2 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.833 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.115 #==================END============================== ata_Compound-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H26 Ca0.19 Er N4 O10' _chemical_formula_sum 'C48 H26 Ca0.19 Er N4 O10' _chemical_formula_weight 993.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P nna' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4217(8) _cell_length_b 22.1411(19) _cell_length_c 26.340(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5494.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7235 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.23 _exptl_crystal_description 'needles' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1975 _exptl_absorpt_coefficient_mu 1.595 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.5348 _exptl_absorpt_correction_T_max 0.9247 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.7 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42881 _diffrn_reflns_av_R_equivalents 0.0950 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.23 _reflns_number_total 6725 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^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 6725 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _refine_ls_shift/su_max 0.000 _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 Er Er 0.2500 0.5000 -0.013806(8) 0.02232(9) Uani 1 2 d S . . Ca Ca 0.2500 0.0000 0.0550(2) 0.038(3) Uani 0.187(5) 2 d SP . . C1 C 0.2500 0.0000 -0.0762(2) 0.0489(18) Uani 1 2 d S . . C2 C 0.2051(6) 0.0529(2) -0.05128(17) 0.0545(15) Uani 1 1 d . . . C3 C 0.1482(7) 0.1050(3) -0.07586(19) 0.075(2) Uani 1 1 d . . . H3 H 0.1313 0.1095 -0.1112 0.090 Uiso 1 1 calc R . . C4 C 0.1228(7) 0.1469(2) -0.03948(19) 0.0701(19) Uani 1 1 d . . . H4 H 0.0888 0.1869 -0.0446 0.084 Uiso 1 1 calc R . . C5 C 0.1572(7) 0.1193(2) 0.00833(18) 0.0583(17) Uani 1 1 d . . . C6 C 0.1494(6) 0.14934(19) 0.05552(17) 0.0468(13) Uani 1 1 d . . . C7 C 0.1763(6) 0.1223(2) 0.10278(17) 0.0488(13) Uani 1 1 d . . . C8 C 0.1625(6) 0.1522(2) 0.15145(16) 0.0485(13) Uani 1 1 d . . . H8 H 0.1393 0.1935 0.1568 0.058 Uiso 1 1 calc R . . C9 C 0.1882(6) 0.1112(2) 0.18749(17) 0.0492(13) Uani 1 1 d . . . H9 H 0.1848 0.1180 0.2231 0.059 Uiso 1 1 calc R . . C10 C 0.2223(5) 0.0546(2) 0.16269(16) 0.0408(12) Uani 1 1 d . . . C11 C 0.2500 0.0000 0.1873(2) 0.0386(15) Uani 1 2 d S . . N12 N 0.2087(5) 0.06225(18) 0.00018(16) 0.0540(13) Uani 1 1 d . . . N13 N 0.2131(4) 0.06329(17) 0.11119(13) 0.0456(11) Uani 1 1 d . . . C14 C 0.2500 0.0000 -0.1325(2) 0.0465(18) Uani 1 2 d S . . C15 C 0.3473(6) 0.0343(3) -0.1596(2) 0.0646(16) Uani 1 1 d . . . H15 H 0.4144 0.0586 -0.1421 0.077 Uiso 1 1 calc R . . C16 C 0.3467(7) 0.0332(3) -0.2119(2) 0.0774(19) Uani 1 1 d . . . H16 H 0.4155 0.0561 -0.2299 0.093 Uiso 1 1 calc R . . C17 C 0.2500 0.0000 -0.2386(3) 0.069(3) Uani 1 2 d S . . C18 C 0.2500 0.0000 -0.2974(3) 0.075(3) Uani 1 2 d S . . O19 O 0.1575(5) -0.0296(3) -0.31921(18) 0.120(2) Uani 1 1 d . . . C20 C 0.1115(6) 0.2136(2) 0.05410(16) 0.0424(12) Uani 1 1 d . . . C21 C 0.2059(7) 0.2571(3) 0.0375(3) 0.089(2) Uani 1 1 d . . . H21 H 0.3008 0.2452 0.0305 0.107 Uiso 1 1 calc R . . C22 C 0.1698(6) 0.3168(2) 0.0304(3) 0.0743(19) Uani 1 1 d . . . H22 H 0.2378 0.3447 0.0178 0.089 Uiso 1 1 calc R . . C23 C 0.0351(4) 0.33550(18) 0.04164(15) 0.0268(9) Uani 1 1 d . . . C24 C -0.0599(5) 0.2944(2) 0.0609(2) 0.0483(13) Uani 1 1 d . . . H24 H -0.1533 0.3072 0.0692 0.058 Uiso 1 1 calc R . . C25 C -0.0221(5) 0.2342(2) 0.0686(2) 0.0533(14) Uani 1 1 d . . . H25 H -0.0878 0.2071 0.0837 0.064 Uiso 1 1 calc R . . C26 C -0.0111(4) 0.3982(2) 0.02950(14) 0.0253(10) Uani 1 1 d . . . O27 O 0.0782(3) 0.43393(12) 0.01085(10) 0.0294(7) Uani 1 1 d . . . O28 O -0.1371(3) 0.41226(13) 0.03765(11) 0.0349(7) Uani 1 1 d . . . C29 C 0.2500 0.0000 0.2441(2) 0.0352(14) Uani 1 2 d S . . C30 C 0.1567(5) -0.0352(2) 0.27093(17) 0.0392(11) Uani 1 1 d . . . H30 H 0.0908 -0.0599 0.2532 0.047 Uiso 1 1 calc R . . C31 C 0.1572(5) -0.0355(2) 0.32345(16) 0.0342(10) Uani 1 1 d . . . H31 H 0.0923 -0.0605 0.3413 0.041 Uiso 1 1 calc R . . C32 C 0.2500 0.0000 0.3500(2) 0.0269(12) Uani 1 2 d S . . C33 C 0.2500 0.0000 0.40709(18) 0.0234(11) Uani 1 2 d S . . O34 O 0.1661(3) -0.03485(12) 0.43084(10) 0.0253(6) Uani 1 1 d . . . O35 O 0.3822(3) 0.52934(14) -0.08702(10) 0.0353(7) Uani 1 1 d . . . H35A H 0.4773 0.5311 -0.0812 0.016 Uiso 0.50 1 d P . . H35B H 0.3695 0.5111 -0.1173 0.016 Uiso 0.50 1 d P . . 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 Er 0.02534(14) 0.01871(14) 0.02292(13) 0.000 0.000 0.00475(13) Ca 0.069(5) 0.023(4) 0.023(3) 0.000 0.000 0.019(4) C1 0.087(5) 0.031(4) 0.029(3) 0.000 0.000 0.011(4) C2 0.103(4) 0.037(3) 0.024(2) 0.006(2) 0.000(2) 0.022(3) C3 0.143(6) 0.055(4) 0.025(3) 0.005(3) -0.002(3) 0.045(4) C4 0.135(6) 0.037(3) 0.037(3) 0.011(3) 0.006(3) 0.038(3) C5 0.116(5) 0.027(3) 0.031(3) 0.006(2) 0.000(3) 0.032(3) C6 0.093(4) 0.015(2) 0.033(3) 0.007(2) 0.002(3) 0.020(3) C7 0.087(4) 0.026(3) 0.034(3) -0.001(2) 0.009(3) 0.021(3) C8 0.085(4) 0.028(3) 0.033(3) 0.000(2) 0.002(3) 0.020(3) C9 0.092(4) 0.028(3) 0.027(2) -0.003(2) 0.004(3) 0.020(3) C10 0.072(4) 0.026(3) 0.024(2) -0.0018(19) 0.007(2) 0.010(2) C11 0.065(4) 0.022(3) 0.029(3) 0.000 0.000 0.015(4) N12 0.109(4) 0.024(2) 0.0282(18) 0.0037(18) 0.004(2) 0.026(2) N13 0.088(3) 0.023(2) 0.0263(18) 0.0008(17) 0.0028(19) 0.023(2) C14 0.066(5) 0.042(4) 0.032(3) 0.000 0.000 0.025(4) C15 0.081(4) 0.062(4) 0.051(3) 0.004(3) 0.002(3) -0.008(3) C16 0.079(5) 0.109(6) 0.045(3) 0.012(4) 0.015(3) 0.002(4) C17 0.046(4) 0.127(9) 0.033(4) 0.000 0.000 0.046(6) C18 0.035(4) 0.133(9) 0.057(5) 0.000 0.000 -0.020(6) O19 0.088(4) 0.211(6) 0.060(3) -0.003(4) -0.005(3) 0.020(4) C20 0.070(3) 0.029(3) 0.029(2) 0.005(2) 0.005(2) 0.019(2) C21 0.081(4) 0.041(4) 0.145(6) 0.035(4) 0.063(5) 0.040(3) C22 0.053(3) 0.038(3) 0.132(5) 0.037(4) 0.033(4) 0.015(3) C23 0.033(2) 0.016(2) 0.031(2) 0.0061(18) 0.003(2) 0.0046(18) C24 0.037(3) 0.033(3) 0.075(4) 0.012(3) 0.004(2) 0.013(2) C25 0.058(3) 0.035(3) 0.067(3) 0.024(3) -0.004(3) -0.001(3) C26 0.030(2) 0.025(3) 0.021(2) -0.0020(18) -0.0003(18) 0.0058(18) O27 0.0342(16) 0.0162(16) 0.0376(18) 0.0009(13) -0.0075(14) 0.0030(13) O28 0.0320(16) 0.0304(18) 0.0423(17) 0.0073(15) 0.0069(15) 0.0078(13) C29 0.055(4) 0.024(3) 0.026(3) 0.000 0.000 0.015(4) C30 0.050(3) 0.028(3) 0.039(3) -0.007(2) -0.005(2) 0.006(2) C31 0.042(3) 0.030(3) 0.031(2) -0.004(2) 0.001(2) 0.001(2) C32 0.037(3) 0.019(3) 0.025(3) 0.000 0.000 0.002(3) C33 0.028(3) 0.025(3) 0.017(2) 0.000 0.000 0.008(3) O34 0.0289(15) 0.0193(16) 0.0279(15) 0.0018(12) -0.0025(13) -0.0098(13) O35 0.0290(15) 0.052(2) 0.0247(15) 0.0018(14) 0.0004(13) 0.0031(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er O27 2.276(3) . ? Er O27 2.276(3) 2_565 ? Er O28 2.302(3) 5_565 ? Er O28 2.302(3) 6_655 ? Er O35 2.386(3) . ? Er O35 2.386(3) 2_565 ? Er O34 2.449(2) 3 ? Er O34 2.449(2) 4 ? Er C33 2.811(5) 3 ? Ca N12 2.034(6) . ? Ca N12 2.034(6) 2 ? Ca N13 2.068(6) . ? Ca N13 2.068(6) 2 ? Ca C5 3.042(5) . ? Ca C5 3.043(5) 2 ? Ca C2 3.064(7) 2 ? Ca C2 3.064(7) . ? Ca C7 3.066(5) 2 ? Ca C7 3.066(5) . ? Ca C10 3.094(7) 2 ? Ca C10 3.094(7) . ? C1 C2 1.407(6) . ? C1 C2 1.408(6) 2 ? C1 C14 1.483(9) . ? C2 N12 1.372(6) . ? C2 C3 1.429(6) . ? C3 C4 1.355(7) . ? C3 H3 0.9500 . ? C4 C5 1.437(7) . ? C4 H4 0.9500 . ? C5 N12 1.371(6) . ? C5 C6 1.411(6) . ? C6 C7 1.404(6) . ? C6 C20 1.468(6) . ? C7 N13 1.370(6) . ? C7 C8 1.449(6) . ? C8 C9 1.335(6) . ? C8 H8 0.9500 . ? C9 C10 1.451(6) . ? C9 H9 0.9500 . ? C10 N13 1.373(5) . ? C10 C11 1.396(5) . ? C11 C10 1.396(5) 2 ? C11 C29 1.495(8) . ? C14 C15 1.388(6) . ? C14 C15 1.388(6) 2 ? C15 C16 1.377(7) . ? C15 H15 0.9500 . ? C16 C17 1.366(8) . ? C16 H16 0.9500 . ? C17 C16 1.366(8) 2 ? C17 C18 1.547(11) . ? C18 O19 1.233(6) 2 ? C18 O19 1.233(6) . ? C20 C21 1.383(7) . ? C20 C25 1.392(6) . ? C21 C22 1.377(7) . ? C21 H21 0.9500 . ? C22 C23 1.367(6) . ? C22 H22 0.9500 . ? C23 C24 1.374(6) . ? C23 C26 1.489(6) . ? C24 C25 1.394(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O28 1.246(4) . ? C26 O27 1.255(5) . ? O28 Er 2.302(3) 5_565 ? C29 C30 1.372(6) . ? C29 C30 1.372(6) 2 ? C30 C31 1.383(6) . ? C30 H30 0.9500 . ? C31 C32 1.367(5) . ? C31 H31 0.9500 . ? C32 C31 1.367(5) 2 ? C32 C33 1.505(7) . ? C33 O34 1.270(3) 2 ? C33 O34 1.270(3) . ? C33 Er 2.811(5) 3 ? O34 Er 2.449(2) 3 ? O35 H35A 0.9094 . ? O35 H35B 0.9014 . ? 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 O27 Er O27 146.85(13) . 2_565 ? O27 Er O28 106.95(9) . 5_565 ? O27 Er O28 82.19(9) 2_565 5_565 ? O27 Er O28 82.18(9) . 6_655 ? O27 Er O28 106.96(9) 2_565 6_655 ? O28 Er O28 148.34(15) 5_565 6_655 ? O27 Er O35 140.97(10) . . ? O27 Er O35 71.60(9) 2_565 . ? O28 Er O35 77.94(10) 5_565 . ? O28 Er O35 76.59(10) 6_655 . ? O27 Er O35 71.60(9) . 2_565 ? O27 Er O35 140.97(10) 2_565 2_565 ? O28 Er O35 76.59(10) 5_565 2_565 ? O28 Er O35 77.94(10) 6_655 2_565 ? O35 Er O35 72.15(13) . 2_565 ? O27 Er O34 73.64(9) . 3 ? O27 Er O34 76.85(9) 2_565 3 ? O28 Er O34 80.11(9) 5_565 3 ? O28 Er O34 131.19(10) 6_655 3 ? O35 Er O34 143.52(10) . 3 ? O35 Er O34 129.68(9) 2_565 3 ? O27 Er O34 76.85(9) . 4 ? O27 Er O34 73.64(9) 2_565 4 ? O28 Er O34 131.19(10) 5_565 4 ? O28 Er O34 80.11(9) 6_655 4 ? O35 Er O34 129.68(9) . 4 ? O35 Er O34 143.52(10) 2_565 4 ? O34 Er O34 53.65(12) 3 4 ? O27 Er C33 73.42(7) . 3 ? O27 Er C33 73.42(7) 2_565 3 ? O28 Er C33 105.83(7) 5_565 3 ? O28 Er C33 105.83(7) 6_655 3 ? O35 Er C33 143.93(7) . 3 ? O35 Er C33 143.93(7) 2_565 3 ? O34 Er C33 26.82(6) 3 3 ? O34 Er C33 26.82(6) 4 3 ? N12 Ca N12 89.5(3) . 2 ? N12 Ca N13 90.96(15) . . ? N12 Ca N13 178.6(2) 2 . ? N12 Ca N13 178.6(2) . 2 ? N12 Ca N13 90.95(15) 2 2 ? N13 Ca N13 88.6(3) . 2 ? N12 Ca C5 21.50(14) . . ? N12 Ca C5 110.9(3) 2 . ? N13 Ca C5 69.65(13) . . ? N13 Ca C5 157.8(3) 2 . ? N12 Ca C5 110.9(3) . 2 ? N12 Ca C5 21.50(14) 2 2 ? N13 Ca C5 157.8(3) . 2 ? N13 Ca C5 69.65(13) 2 2 ? C5 Ca C5 132.3(3) . 2 ? N12 Ca C2 68.7(2) . 2 ? N12 Ca C2 20.91(16) 2 2 ? N13 Ca C2 159.4(2) . 2 ? N13 Ca C2 111.82(16) 2 2 ? C5 Ca C2 90.1(2) . 2 ? C5 Ca C2 42.20(14) 2 2 ? N12 Ca C2 20.91(16) . . ? N12 Ca C2 68.7(2) 2 . ? N13 Ca C2 111.83(16) . . ? N13 Ca C2 159.4(2) 2 . ? C5 Ca C2 42.21(14) . . ? C5 Ca C2 90.1(2) 2 . ? C2 Ca C2 47.9(2) 2 . ? N12 Ca C7 159.0(3) . 2 ? N12 Ca C7 69.48(15) 2 2 ? N13 Ca C7 110.1(3) . 2 ? N13 Ca C7 21.47(13) 2 2 ? C5 Ca C7 176.39(18) . 2 ? C5 Ca C7 48.22(12) 2 2 ? C2 Ca C7 90.36(14) 2 2 ? C2 Ca C7 138.1(2) . 2 ? N12 Ca C7 69.48(15) . . ? N12 Ca C7 159.0(3) 2 . ? N13 Ca C7 21.47(13) . . ? N13 Ca C7 110.1(3) 2 . ? C5 Ca C7 48.22(12) . . ? C5 Ca C7 176.39(18) 2 . ? C2 Ca C7 138.1(2) 2 . ? C2 Ca C7 90.36(14) . . ? C7 Ca C7 131.5(3) 2 . ? N12 Ca C10 158.7(2) . 2 ? N12 Ca C10 111.72(16) 2 2 ? N13 Ca C10 67.8(2) . 2 ? N13 Ca C10 20.77(15) 2 2 ? C5 Ca C10 137.20(19) . 2 ? C5 Ca C10 90.40(14) 2 2 ? C2 Ca C10 132.59(12) 2 2 ? C2 Ca C10 176.88(14) . 2 ? C7 Ca C10 42.24(13) 2 2 ? C7 Ca C10 89.29(19) . 2 ? N12 Ca C10 111.72(16) . . ? N12 Ca C10 158.7(2) 2 . ? N13 Ca C10 20.77(15) . . ? N13 Ca C10 67.8(2) 2 . ? C5 Ca C10 90.41(14) . . ? C5 Ca C10 137.20(19) 2 . ? C2 Ca C10 176.88(14) 2 . ? C2 Ca C10 132.59(12) . . ? C7 Ca C10 89.29(19) 2 . ? C7 Ca C10 42.24(13) . . ? C10 Ca C10 47.09(19) 2 . ? C2 C1 C2 124.4(6) . 2 ? C2 C1 C14 117.8(3) . . ? C2 C1 C14 117.8(3) 2 . ? N12 C2 C1 125.4(4) . . ? N12 C2 C3 109.6(4) . . ? C1 C2 C3 125.0(4) . . ? N12 C2 Ca 32.0(2) . . ? C1 C2 Ca 93.8(3) . . ? C3 C2 Ca 140.8(3) . . ? C4 C3 C2 107.4(4) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? C3 C4 C5 106.8(4) . . ? C3 C4 H4 126.6 . . ? C5 C4 H4 126.6 . . ? N12 C5 C6 126.2(4) . . ? N12 C5 C4 109.5(4) . . ? C6 C5 C4 124.1(4) . . ? N12 C5 Ca 32.9(2) . . ? C6 C5 Ca 93.9(3) . . ? C4 C5 Ca 142.0(4) . . ? C7 C6 C5 124.8(4) . . ? C7 C6 C20 118.7(4) . . ? C5 C6 C20 116.5(4) . . ? N13 C7 C6 126.5(4) . . ? N13 C7 C8 108.4(4) . . ? C6 C7 C8 125.0(4) . . ? N13 C7 Ca 33.5(2) . . ? C6 C7 Ca 93.1(3) . . ? C8 C7 Ca 141.9(3) . . ? C9 C8 C7 107.6(4) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? C8 C9 C10 107.9(4) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? N13 C10 C11 126.3(4) . . ? N13 C10 C9 108.0(4) . . ? C11 C10 C9 125.5(4) . . ? N13 C10 Ca 32.3(2) . . ? C11 C10 Ca 94.1(3) . . ? C9 C10 Ca 140.3(3) . . ? C10 C11 C10 124.7(5) . 2 ? C10 C11 C29 117.7(3) . . ? C10 C11 C29 117.7(3) 2 . ? C5 N12 C2 106.6(4) . . ? C5 N12 Ca 125.5(4) . . ? C2 N12 Ca 127.1(3) . . ? C7 N13 C10 108.0(4) . . ? C7 N13 Ca 125.0(3) . . ? C10 N13 Ca 127.0(3) . . ? C15 C14 C15 118.1(7) . 2 ? C15 C14 C1 121.0(3) . . ? C15 C14 C1 121.0(3) 2 . ? C16 C15 C14 120.2(6) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 121.9(6) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C16 117.9(7) . 2 ? C16 C17 C18 121.1(4) . . ? C16 C17 C18 121.1(4) 2 . ? O19 C18 O19 124.4(9) 2 . ? O19 C18 C17 117.8(4) 2 . ? O19 C18 C17 117.8(4) . . ? C21 C20 C25 116.1(4) . . ? C21 C20 C6 121.8(5) . . ? C25 C20 C6 122.1(5) . . ? C22 C21 C20 123.6(5) . . ? C22 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C23 C22 C21 119.3(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.0(4) . . ? C22 C23 C26 120.4(4) . . ? C24 C23 C26 120.4(4) . . ? C23 C24 C25 121.3(4) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C20 C25 C24 120.3(5) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? O28 C26 O27 123.2(4) . . ? O28 C26 C23 118.3(4) . . ? O27 C26 C23 118.4(3) . . ? C26 O27 Er 173.5(3) . . ? C26 O28 Er 127.2(3) . 5_565 ? C30 C29 C30 117.9(6) . 2 ? C30 C29 C11 121.1(3) . . ? C30 C29 C11 121.1(3) 2 . ? C29 C30 C31 121.1(4) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.7(4) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C31 118.5(5) 2 . ? C31 C32 C33 120.7(3) 2 . ? C31 C32 C33 120.7(3) . . ? O34 C33 O34 121.0(4) 2 . ? O34 C33 C32 119.5(2) 2 . ? O34 C33 C32 119.5(2) . . ? O34 C33 Er 60.5(2) 2 3 ? O34 C33 Er 60.5(2) . 3 ? C32 C33 Er 180.0 . 3 ? C33 O34 Er 92.7(2) . 3 ? Er O35 H35A 112.9 . . ? Er O35 H35B 121.5 . . ? H35A O35 H35B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.889 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.114 #===========================END================================= data_Compound-6 _database_code_depnum_ccdc_archive 'CCDC 627701' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H50 N7 O15 Sm2' _chemical_formula_sum 'C75 H50 N7 O15 Sm2' _chemical_formula_weight 1589.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5598(3) _cell_length_b 24.0771(3) _cell_length_c 31.2327(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.0195(5) _cell_angle_gamma 90.00 _cell_volume 15658.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 15051 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.90 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6344 _exptl_absorpt_coefficient_mu 1.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6537 _exptl_absorpt_correction_T_max 0.8605 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50061 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.90 _reflns_number_total 18264 _reflns_number_gt 11990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.095. Two of the carboxylic/carboxylate functions are partly disordered. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18264 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.914384(14) 0.229593(11) 0.199273(9) 0.02170(10) Uani 1 1 d . . . Sm2 Sm 0.827364(17) 0.690081(12) 0.586873(10) 0.03062(11) Uani 1 1 d . . . C1 C 0.8373(3) 0.2452(2) 0.4833(2) 0.0283(14) Uani 1 1 d . . . C2 C 0.8264(3) 0.2975(2) 0.4609(2) 0.0348(16) Uani 1 1 d . . . H2 H 0.8251 0.3041 0.4306 0.042 Uiso 1 1 calc R . . C3 C 0.8184(3) 0.3353(3) 0.4900(2) 0.0386(16) Uani 1 1 d . . . H3 H 0.8092 0.3736 0.4842 0.046 Uiso 1 1 calc R . . C4 C 0.8262(3) 0.3076(2) 0.5321(2) 0.0335(15) Uani 1 1 d . . . C5 C 0.8315(3) 0.3331(2) 0.5730(2) 0.0273(14) Uani 1 1 d . . . C6 C 0.8367(3) 0.3044(2) 0.6131(2) 0.0305(14) Uani 1 1 d . . . C7 C 0.8452(3) 0.3292(3) 0.6565(2) 0.0361(15) Uani 1 1 d . . . H7 H 0.8536 0.3673 0.6635 0.043 Uiso 1 1 calc R . . C8 C 0.8390(3) 0.2894(2) 0.6850(2) 0.0317(14) Uani 1 1 d . . . H8 H 0.8420 0.2941 0.7157 0.038 Uiso 1 1 calc R . . C9 C 0.8270(3) 0.2382(2) 0.6604(2) 0.0266(13) Uani 1 1 d . . . C10 C 0.8097(3) 0.1879(2) 0.67519(18) 0.0240(12) Uani 1 1 d . . . C11 C 0.8056(3) 0.1369(2) 0.65230(19) 0.0242(13) Uani 1 1 d . . . C12 C 0.7918(3) 0.0834(2) 0.66807(19) 0.0273(13) Uani 1 1 d . . . H12 H 0.7784 0.0764 0.6942 0.033 Uiso 1 1 calc R . . C13 C 0.8013(3) 0.0450(2) 0.63895(18) 0.0273(13) Uani 1 1 d . . . H13 H 0.7965 0.0060 0.6409 0.033 Uiso 1 1 calc R . . C14 C 0.8201(3) 0.0749(2) 0.60411(19) 0.0254(13) Uani 1 1 d . . . C15 C 0.8376(3) 0.0498(2) 0.5685(2) 0.0310(14) Uani 1 1 d . . . C16 C 0.8527(3) 0.0773(2) 0.5331(2) 0.0345(15) Uani 1 1 d . . . C17 C 0.8727(4) 0.0519(2) 0.4972(2) 0.0420(18) Uani 1 1 d . . . H17 H 0.8813 0.0136 0.4946 0.050 Uiso 1 1 calc R . . C18 C 0.8770(4) 0.0917(2) 0.4681(2) 0.0404(17) Uani 1 1 d . . . H18 H 0.8880 0.0868 0.4408 0.048 Uiso 1 1 calc R . . C19 C 0.8615(3) 0.1439(2) 0.48657(19) 0.0270(13) Uani 1 1 d . . . C20 C 0.8557(3) 0.1954(2) 0.46558(19) 0.0261(13) Uani 1 1 d . . . N21 N 0.8339(2) 0.25214(17) 0.52596(16) 0.0236(11) Uani 1 1 d . . . H21 H 0.8362 0.2258 0.5458 0.028 Uiso 1 1 calc R . . N22 N 0.8307(2) 0.24857(19) 0.61770(16) 0.0254(11) Uani 1 1 d . . . N23 N 0.8207(2) 0.13072(18) 0.61206(16) 0.0247(11) Uani 1 1 d . . . H23 H 0.8290 0.1573 0.5951 0.030 Uiso 1 1 calc R . . N24 N 0.8484(3) 0.13325(18) 0.52649(16) 0.0312(12) Uani 1 1 d . . . C25 C 0.8307(3) 0.3951(2) 0.5751(2) 0.0368(16) Uani 1 1 d . . . C26 C 0.8760(4) 0.4253(3) 0.5594(3) 0.054(2) Uani 1 1 d . . . H26 H 0.9061 0.4063 0.5473 0.065 Uiso 1 1 calc R . . C27 C 0.8769(5) 0.4837(3) 0.5618(3) 0.069(3) Uani 1 1 d . . . H27 H 0.9077 0.5042 0.5513 0.083 Uiso 1 1 calc R . . C28 C 0.8314(4) 0.5119(3) 0.5799(3) 0.051(2) Uani 1 1 d . A . C29 C 0.7875(4) 0.4811(3) 0.5948(3) 0.066(3) Uani 1 1 d . . . H29 H 0.7573 0.4994 0.6073 0.079 Uiso 1 1 calc R . . C30 C 0.7869(4) 0.4230(3) 0.5916(3) 0.051(2) Uani 1 1 d . . . H30 H 0.7554 0.4026 0.6013 0.061 Uiso 1 1 calc R . . C31 C 0.8305(5) 0.5746(3) 0.5830(3) 0.066(3) Uani 1 1 d . . . O32A O 0.8695(7) 0.6014(4) 0.5638(4) 0.052(3) Uiso 0.58(2) 1 d P A 1 O33A O 0.7971(6) 0.5968(3) 0.6051(4) 0.037(3) Uiso 0.58(2) 1 d P A 1 O32B O 0.8401(8) 0.6029(5) 0.5487(5) 0.042(4) Uiso 0.42(2) 1 d P A 2 O33B O 0.8259(8) 0.5958(4) 0.6184(5) 0.036(4) Uiso 0.42(2) 1 d P A 2 C34 C 0.7914(3) 0.1859(2) 0.71861(19) 0.0236(12) Uani 1 1 d . . . C35 C 0.7279(3) 0.1742(2) 0.7186(2) 0.0300(14) Uani 1 1 d . . . H35 H 0.6981 0.1650 0.6913 0.036 Uiso 1 1 calc R . . C36 C 0.7073(3) 0.1755(2) 0.75670(19) 0.0276(13) Uani 1 1 d . . . H36 H 0.6640 0.1670 0.7560 0.033 Uiso 1 1 calc R . . C37 C 0.7520(3) 0.1896(2) 0.79699(19) 0.0247(13) Uani 1 1 d . . . C38 C 0.8156(3) 0.1989(3) 0.7974(2) 0.0337(15) Uani 1 1 d . . . H38 H 0.8461 0.2060 0.8248 0.040 Uiso 1 1 calc R . . C39 C 0.8356(3) 0.1978(2) 0.7586(2) 0.0313(14) Uani 1 1 d . . . H39 H 0.8791 0.2053 0.7594 0.038 Uiso 1 1 calc R . . C40 C 0.7295(3) 0.1965(2) 0.83786(19) 0.0244(13) Uani 1 1 d . . . O41 O 0.66876(19) 0.20489(15) 0.83351(13) 0.0240(9) Uani 1 1 d . . . O42 O 0.7675(2) 0.19501(17) 0.87532(13) 0.0323(10) Uani 1 1 d . . . C43 C 0.8415(3) -0.0127(2) 0.57041(19) 0.0282(14) Uani 1 1 d . . . C44 C 0.8959(3) -0.0381(3) 0.5967(2) 0.0380(16) Uani 1 1 d . . . H44 H 0.9331 -0.0170 0.6098 0.046 Uiso 1 1 calc R . . C45 C 0.8948(3) -0.0953(2) 0.6037(2) 0.0338(15) Uani 1 1 d . . . H45 H 0.9316 -0.1129 0.6221 0.041 Uiso 1 1 calc R . . C46 C 0.8419(3) -0.1268(2) 0.58454(18) 0.0278(14) Uani 1 1 d . . . C47 C 0.7888(3) -0.1009(2) 0.5565(2) 0.0353(15) Uani 1 1 d . . . H47 H 0.7522 -0.1224 0.5424 0.042 Uiso 1 1 calc R . . C48 C 0.7890(3) -0.0448(2) 0.5490(2) 0.0374(16) Uani 1 1 d . . . H48 H 0.7532 -0.0277 0.5290 0.045 Uiso 1 1 calc R . . C49 C 0.8392(3) -0.1875(2) 0.5940(2) 0.0279(14) Uani 1 1 d . . . O50 O 0.7910(3) -0.21366(17) 0.57385(17) 0.0466(13) Uani 1 1 d . . . O51 O 0.8861(2) -0.21014(16) 0.62149(14) 0.0312(10) Uani 1 1 d . . . C52 C 0.8715(3) 0.1991(2) 0.42177(19) 0.0257(13) Uani 1 1 d . . . C53 C 0.9364(4) 0.1988(3) 0.4204(2) 0.0443(18) Uani 1 1 d . . . H53 H 0.9694 0.1940 0.4469 0.053 Uiso 1 1 calc R . . C54 C 0.9520(3) 0.2055(3) 0.3806(2) 0.0334(15) Uani 1 1 d . . . H54 H 0.9957 0.2053 0.3799 0.040 Uiso 1 1 calc R . . C55 C 0.9037(3) 0.2125(2) 0.34131(18) 0.0236(13) Uani 1 1 d . . . C56 C 0.8395(3) 0.2109(3) 0.3427(2) 0.0312(14) Uani 1 1 d . . . H56 H 0.8062 0.2145 0.3162 0.037 Uiso 1 1 calc R . . C57 C 0.8245(3) 0.2042(3) 0.3828(2) 0.0341(15) Uani 1 1 d . . . H57 H 0.7807 0.2030 0.3834 0.041 Uiso 1 1 calc R . . C58 C 0.9206(3) 0.2211(2) 0.2992(2) 0.0271(14) Uani 1 1 d . . . O59 O 0.9785(2) 0.22719(16) 0.29873(14) 0.0318(10) Uani 1 1 d . . . O60 O 0.8753(2) 0.22367(16) 0.26413(14) 0.0352(10) Uani 1 1 d . . . C61 C 1.0009(3) -0.1532(2) 0.21048(18) 0.0216(12) Uani 1 1 d . . . C62 C 1.0074(3) -0.1268(2) 0.1706(2) 0.0310(14) Uani 1 1 d . . . H62 H 1.0068 -0.0879 0.1654 0.037 Uiso 1 1 calc R . . C63 C 1.0144(3) -0.1668(2) 0.1418(2) 0.0291(14) Uani 1 1 d . . . H63 H 1.0203 -0.1612 0.1130 0.035 Uiso 1 1 calc R . . C64 C 1.0112(3) -0.2200(2) 0.16302(19) 0.0224(12) Uani 1 1 d . . . C65 C 1.0196(3) -0.2718(2) 0.14509(19) 0.0234(12) Uani 1 1 d . . . C66 C 1.0159(3) -0.3232(2) 0.16399(19) 0.0247(13) Uani 1 1 d . . . C67 C 1.0196(3) -0.3762(2) 0.1423(2) 0.0353(15) Uani 1 1 d . . . H67 H 1.0265 -0.3821 0.1139 0.042 Uiso 1 1 calc R . . C68 C 1.0109(3) -0.4160(2) 0.1719(2) 0.0381(16) Uani 1 1 d . . . H68 H 1.0091 -0.4549 0.1669 0.046 Uiso 1 1 calc R . . C69 C 1.0051(3) -0.3893(2) 0.2113(2) 0.0263(13) Uani 1 1 d . . . C70 C 1.0000 -0.4159(3) 0.2500 0.0232(17) Uani 1 2 d S . . C71 C 1.0000 -0.1262(3) 0.2500 0.0246(18) Uani 1 2 d S . . N72 N 1.0024(2) -0.21068(19) 0.20433(16) 0.0246(11) Uani 1 1 d . . . H72 H 0.9983 -0.2363 0.2235 0.030 Uiso 0.50 1 calc PR . . N73 N 1.0079(2) -0.33317(18) 0.20565(16) 0.0252(11) Uani 1 1 d . . . H73 H 1.0052 -0.3077 0.2253 0.030 Uiso 0.50 1 calc PR . . C74 C 1.0000 -0.0643(3) 0.2500 0.032(2) Uani 1 2 d S . . C75 C 0.9514(3) -0.0342(2) 0.2209(2) 0.0312(14) Uani 1 1 d . . . H75 H 0.9183 -0.0538 0.2004 0.037 Uiso 1 1 calc R . . C76 C 0.9500(3) 0.0231(2) 0.2210(2) 0.0317(15) Uani 1 1 d . . . H76 H 0.9156 0.0426 0.2017 0.038 Uiso 1 1 calc R . . C77 C 1.0000 0.0525(3) 0.2500 0.030(2) Uani 1 2 d S . . C78 C 1.0000 0.1148(4) 0.2500 0.034(2) Uani 1 2 d S . . O79 O 0.9521(2) 0.13892(15) 0.22534(14) 0.0320(10) Uani 1 1 d . . . C80 C 1.0370(3) -0.2731(2) 0.1012(2) 0.0314(14) Uani 1 1 d . B . C81 C 1.1012(4) -0.2795(3) 0.1012(3) 0.052(2) Uani 1 1 d . . . H81 H 1.1333 -0.2813 0.1285 0.062 Uiso 1 1 calc R . . C82 C 1.1185(5) -0.2833(3) 0.0615(3) 0.066(3) Uani 1 1 d . B . H82 H 1.1625 -0.2864 0.0618 0.079 Uiso 1 1 calc R . . C83 C 1.0716(5) -0.2826(3) 0.0214(3) 0.061(3) Uani 1 1 d . . . C84 C 1.0107(5) -0.2763(4) 0.0227(3) 0.081(3) Uani 1 1 d . B . H84 H 0.9784 -0.2750 -0.0045 0.097 Uiso 1 1 calc R . . C85 C 0.9924(4) -0.2714(4) 0.0619(2) 0.058(2) Uani 1 1 d . . . H85 H 0.9484 -0.2670 0.0612 0.070 Uiso 1 1 calc R B . C86A C 1.0772(9) -0.2888(6) -0.0247(6) 0.047(4) Uiso 0.592(17) 1 d P B 1 O87A O 1.0337(8) -0.2981(5) -0.0577(5) 0.096(5) Uiso 0.592(17) 1 d P B 1 O88A O 1.1290(5) -0.2797(4) -0.0320(4) 0.048(3) Uiso 0.592(17) 1 d P . 1 C86B C 1.1118(9) -0.2906(6) -0.0123(6) 0.026(4) Uiso 0.408(17) 1 d P . 2 O87B O 1.0792(8) -0.2854(6) -0.0489(6) 0.059(5) Uiso 0.408(17) 1 d P . 2 O88B O 1.1682(8) -0.2914(6) -0.0096(6) 0.066(6) Uiso 0.408(17) 1 d P . 2 C89 C 1.0000 -0.4787(3) 0.2500 0.0266(19) Uani 1 2 d S . . C90 C 0.9457(3) -0.5071(2) 0.2256(2) 0.0340(15) Uani 1 1 d . . . H90 H 0.9090 -0.4874 0.2092 0.041 Uiso 1 1 calc R . . C91 C 0.9468(3) -0.5664(2) 0.2261(2) 0.0305(14) Uani 1 1 d . . . H91 H 0.9103 -0.5864 0.2096 0.037 Uiso 1 1 calc R . . C92 C 1.0000 -0.5953(3) 0.2500 0.0249(19) Uani 1 2 d S . . C93 C 1.0000 -0.6568(3) 0.2500 0.0239(18) Uani 1 2 d S . . O94 O 0.94955(19) -0.68136(16) 0.22840(15) 0.0318(10) Uani 1 1 d . . . O95 O 0.81422(19) 0.17508(16) 0.18074(13) 0.0282(9) Uani 1 1 d . . . C96 C 0.7754(3) 0.1636(3) 0.2028(2) 0.0374(16) Uani 1 1 d . . . H96 H 0.7830 0.1792 0.2316 0.045 Uiso 1 1 calc R . . N97 N 0.7251(3) 0.1318(2) 0.18929(19) 0.0396(14) Uani 1 1 d . . . C98 C 0.7089(4) 0.1059(4) 0.1455(3) 0.069(3) Uani 1 1 d . . . H98A H 0.7232 0.1299 0.1246 0.103 Uiso 1 1 calc R . . H98B H 0.6623 0.1007 0.1354 0.103 Uiso 1 1 calc R . . H98C H 0.7304 0.0698 0.1472 0.103 Uiso 1 1 calc R . . C99 C 0.6820(4) 0.1204(4) 0.2182(3) 0.062(2) Uani 1 1 d . . . H99A H 0.7022 0.1333 0.2484 0.093 Uiso 1 1 calc R . . H99B H 0.6740 0.0803 0.2188 0.093 Uiso 1 1 calc R . . H99C H 0.6411 0.1399 0.2067 0.093 Uiso 1 1 calc R . . O100 O 0.7271(4) 0.6877(3) 0.5279(3) 0.113(3) Uiso 1 1 d . A . H10A H 0.7183 0.6504 0.5185 0.170 Uiso 1 1 d R . . H10B H 0.6929 0.7085 0.5389 0.170 Uiso 1 1 d R . . O101 O 0.9365(3) 0.6825(3) 0.6356(2) 0.093(2) Uani 1 1 d . A . H10C H 0.9381 0.6518 0.6550 0.140 Uiso 1 1 d R . . H10D H 0.9660 0.6767 0.6181 0.140 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.03164(19) 0.01403(14) 0.01947(16) -0.00164(11) 0.00669(12) 0.00284(12) Sm2 0.0561(2) 0.01681(16) 0.01764(16) -0.00050(12) 0.00727(15) -0.00330(14) C1 0.041(4) 0.026(3) 0.023(3) 0.002(2) 0.019(3) -0.003(3) C2 0.057(4) 0.018(3) 0.036(4) 0.010(3) 0.024(3) 0.010(3) C3 0.059(5) 0.021(3) 0.042(4) 0.009(3) 0.024(4) 0.011(3) C4 0.040(4) 0.020(3) 0.043(4) 0.005(3) 0.016(3) 0.008(3) C5 0.029(3) 0.013(3) 0.044(4) -0.004(2) 0.016(3) 0.003(2) C6 0.029(3) 0.023(3) 0.046(4) -0.002(3) 0.022(3) 0.007(3) C7 0.038(4) 0.030(3) 0.040(4) -0.014(3) 0.009(3) -0.003(3) C8 0.045(4) 0.024(3) 0.030(3) -0.009(3) 0.015(3) 0.001(3) C9 0.030(3) 0.025(3) 0.030(3) -0.006(2) 0.018(3) -0.002(3) C10 0.021(3) 0.034(3) 0.018(3) -0.003(2) 0.007(2) 0.008(3) C11 0.031(3) 0.023(3) 0.021(3) -0.004(2) 0.011(3) -0.006(3) C12 0.036(4) 0.026(3) 0.024(3) 0.002(2) 0.013(3) 0.001(3) C13 0.043(4) 0.021(3) 0.020(3) 0.002(2) 0.011(3) 0.003(3) C14 0.039(4) 0.018(3) 0.023(3) 0.000(2) 0.014(3) -0.001(3) C15 0.047(4) 0.023(3) 0.026(3) 0.004(2) 0.014(3) 0.001(3) C16 0.065(5) 0.020(3) 0.025(3) 0.003(2) 0.023(3) 0.001(3) C17 0.090(6) 0.017(3) 0.030(3) -0.003(3) 0.036(4) 0.009(3) C18 0.076(5) 0.024(3) 0.033(4) -0.001(3) 0.036(4) 0.006(3) C19 0.039(4) 0.023(3) 0.025(3) -0.004(2) 0.019(3) 0.000(3) C20 0.042(4) 0.017(3) 0.024(3) 0.000(2) 0.018(3) 0.003(3) N21 0.036(3) 0.011(2) 0.031(3) 0.0040(19) 0.021(2) 0.003(2) N22 0.031(3) 0.022(2) 0.028(3) -0.004(2) 0.015(2) 0.003(2) N23 0.035(3) 0.018(2) 0.026(3) 0.0008(19) 0.015(2) 0.002(2) N24 0.058(4) 0.017(2) 0.025(3) 0.005(2) 0.023(3) 0.004(2) C25 0.050(4) 0.022(3) 0.045(4) -0.002(3) 0.024(3) 0.001(3) C26 0.071(5) 0.032(4) 0.078(6) 0.002(4) 0.053(5) 0.004(4) C27 0.113(7) 0.024(4) 0.096(7) -0.021(4) 0.073(6) -0.017(4) C28 0.066(5) 0.034(4) 0.062(5) -0.001(3) 0.036(4) -0.002(4) C29 0.087(7) 0.028(4) 0.100(7) 0.000(4) 0.055(6) 0.002(4) C30 0.067(5) 0.025(3) 0.073(6) -0.005(3) 0.043(5) 0.002(3) C31 0.125(8) 0.020(3) 0.078(6) -0.012(4) 0.072(6) -0.011(4) C34 0.023(3) 0.027(3) 0.025(3) 0.001(2) 0.014(3) 0.008(2) C35 0.038(4) 0.031(3) 0.024(3) -0.004(3) 0.012(3) 0.002(3) C36 0.034(3) 0.026(3) 0.027(3) -0.003(2) 0.015(3) -0.001(3) C37 0.038(4) 0.017(3) 0.022(3) -0.001(2) 0.015(3) 0.010(3) C38 0.038(4) 0.037(4) 0.029(3) -0.008(3) 0.013(3) 0.013(3) C39 0.027(3) 0.035(3) 0.032(3) -0.006(3) 0.008(3) 0.000(3) C40 0.035(4) 0.014(3) 0.021(3) 0.000(2) 0.001(3) 0.005(2) O41 0.031(2) 0.0193(19) 0.024(2) 0.0008(16) 0.0124(18) -0.0039(18) O42 0.040(3) 0.037(2) 0.021(2) 0.0016(18) 0.010(2) 0.010(2) C43 0.053(4) 0.020(3) 0.018(3) 0.001(2) 0.020(3) 0.006(3) C44 0.048(4) 0.030(3) 0.036(4) -0.004(3) 0.010(3) -0.002(3) C45 0.052(4) 0.024(3) 0.026(3) 0.010(3) 0.011(3) 0.006(3) C46 0.046(4) 0.021(3) 0.019(3) 0.001(2) 0.012(3) -0.010(3) C47 0.053(4) 0.027(3) 0.023(3) -0.007(3) 0.003(3) -0.006(3) C48 0.055(4) 0.026(3) 0.025(3) 0.003(3) 0.000(3) 0.003(3) C49 0.046(4) 0.017(3) 0.024(3) -0.002(2) 0.016(3) -0.002(3) O50 0.070(4) 0.016(2) 0.050(3) 0.006(2) 0.010(3) -0.001(2) O51 0.045(3) 0.024(2) 0.031(2) 0.0065(18) 0.021(2) 0.013(2) C52 0.040(4) 0.019(3) 0.025(3) 0.001(2) 0.022(3) -0.004(3) C53 0.047(4) 0.062(5) 0.026(4) 0.009(3) 0.013(3) 0.011(4) C54 0.037(4) 0.043(4) 0.027(3) 0.001(3) 0.020(3) 0.004(3) C55 0.044(4) 0.013(2) 0.019(3) -0.001(2) 0.019(3) 0.000(2) C56 0.035(4) 0.036(3) 0.026(3) 0.007(3) 0.015(3) -0.004(3) C57 0.041(4) 0.039(3) 0.034(4) 0.006(3) 0.030(3) 0.003(3) C58 0.052(4) 0.008(2) 0.025(3) -0.003(2) 0.017(3) 0.002(3) O59 0.039(3) 0.026(2) 0.038(3) -0.0085(18) 0.025(2) -0.0076(19) O60 0.051(3) 0.031(2) 0.025(2) 0.0032(19) 0.013(2) -0.003(2) C61 0.023(3) 0.017(3) 0.025(3) 0.000(2) 0.007(2) -0.006(2) C62 0.046(4) 0.016(3) 0.031(3) 0.004(2) 0.009(3) 0.000(3) C63 0.041(4) 0.019(3) 0.028(3) 0.010(2) 0.010(3) 0.001(3) C64 0.022(3) 0.022(3) 0.023(3) 0.003(2) 0.005(2) 0.000(2) C65 0.027(3) 0.019(3) 0.026(3) 0.003(2) 0.009(3) 0.003(2) C66 0.031(3) 0.020(3) 0.025(3) 0.004(2) 0.011(3) 0.004(3) C67 0.058(4) 0.025(3) 0.029(3) -0.003(3) 0.022(3) -0.007(3) C68 0.068(5) 0.016(3) 0.036(4) -0.010(3) 0.023(4) -0.004(3) C69 0.036(3) 0.014(3) 0.031(3) -0.002(2) 0.013(3) 0.001(3) C70 0.031(5) 0.015(4) 0.026(4) 0.000 0.013(4) 0.000 C71 0.030(5) 0.011(3) 0.031(5) 0.000 0.005(4) 0.000 N72 0.031(3) 0.016(2) 0.026(3) -0.0028(19) 0.006(2) -0.003(2) N73 0.037(3) 0.017(2) 0.026(3) 0.0011(19) 0.017(2) 0.002(2) C74 0.049(6) 0.017(4) 0.028(5) 0.000 0.004(4) 0.000 C75 0.039(4) 0.015(3) 0.034(4) 0.002(2) 0.000(3) -0.002(3) C76 0.036(4) 0.013(3) 0.040(4) -0.002(3) 0.001(3) 0.003(3) C77 0.033(5) 0.020(4) 0.030(5) 0.000 -0.002(4) 0.000 C78 0.041(6) 0.029(5) 0.027(5) 0.000 -0.001(4) 0.000 O79 0.043(3) 0.0134(19) 0.036(3) 0.0043(17) 0.004(2) -0.0004(19) C80 0.049(4) 0.023(3) 0.030(3) 0.002(3) 0.024(3) 0.004(3) C81 0.053(5) 0.052(5) 0.058(5) -0.023(4) 0.030(4) -0.008(4) C82 0.089(7) 0.048(5) 0.084(7) -0.025(5) 0.067(6) -0.018(5) C83 0.118(8) 0.027(4) 0.061(6) 0.004(4) 0.068(6) -0.003(4) C84 0.108(8) 0.118(9) 0.024(4) 0.021(5) 0.031(5) 0.025(7) C85 0.048(5) 0.099(7) 0.027(4) 0.012(4) 0.010(4) 0.017(4) C89 0.042(5) 0.006(3) 0.034(5) 0.000 0.014(4) 0.000 C90 0.044(4) 0.022(3) 0.039(4) 0.007(3) 0.017(3) 0.003(3) C91 0.033(4) 0.020(3) 0.036(4) 0.002(3) 0.005(3) 0.005(3) C92 0.041(5) 0.012(4) 0.028(4) 0.000 0.020(4) 0.000 C93 0.027(5) 0.021(4) 0.027(4) 0.000 0.014(4) 0.000 O94 0.026(2) 0.021(2) 0.046(3) 0.0040(19) 0.006(2) 0.0005(18) O95 0.034(2) 0.024(2) 0.027(2) 0.0066(17) 0.0097(19) -0.0081(18) C96 0.047(4) 0.033(4) 0.036(4) -0.003(3) 0.020(3) -0.007(3) N97 0.048(4) 0.038(3) 0.041(3) -0.008(3) 0.028(3) -0.016(3) C98 0.064(6) 0.090(7) 0.063(6) -0.036(5) 0.036(5) -0.031(5) C99 0.067(6) 0.068(5) 0.064(6) -0.004(4) 0.039(5) -0.013(4) O101 0.068(4) 0.154(7) 0.064(4) 0.037(4) 0.028(4) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O59 2.296(4) 2_755 ? Sm1 O94 2.375(4) 1_565 ? Sm1 O60 2.391(4) . ? Sm1 O51 2.393(4) 6 ? Sm1 O79 2.398(4) . ? Sm1 O41 2.408(4) 7_656 ? Sm1 O95 2.465(4) . ? Sm1 Sm2 4.0214(4) 6_565 ? Sm2 O88A 2.276(10) 2_765 ? Sm2 O100 2.451(8) . ? Sm2 O33A 2.446(8) . ? Sm2 O32B 2.465(11) . ? Sm2 O50 2.447(4) 1_565 ? Sm2 O101 2.455(6) . ? Sm2 O33B 2.479(11) . ? Sm2 O88B 2.480(16) 2_765 ? Sm2 O32A 2.497(10) . ? Sm2 O41 2.492(4) 4_656 ? Sm2 O42 2.617(4) 4_656 ? Sm2 O87B 2.655(17) 2_765 ? C1 N21 1.363(7) . ? C1 C20 1.420(8) . ? C1 C2 1.431(8) . ? C2 C3 1.330(9) . ? C2 H2 0.9500 . ? C3 C4 1.444(9) . ? C3 H3 0.9500 . ? C4 N21 1.366(7) . ? C4 C5 1.397(9) . ? C5 C6 1.408(9) . ? C5 C25 1.493(8) . ? C6 N22 1.362(7) . ? C6 C7 1.449(9) . ? C7 C8 1.337(9) . ? C7 H7 0.9500 . ? C8 C9 1.440(8) . ? C8 H8 0.9500 . ? C9 N22 1.380(7) . ? C9 C10 1.380(8) . ? C10 C11 1.412(8) . ? C10 C34 1.508(8) . ? C11 N23 1.386(7) . ? C11 C12 1.438(8) . ? C12 C13 1.349(7) . ? C12 H12 0.9500 . ? C13 C14 1.447(7) . ? C13 H13 0.9500 . ? C14 N23 1.367(7) . ? C14 C15 1.402(8) . ? C15 C16 1.395(8) . ? C15 C43 1.508(8) . ? C16 N24 1.362(7) . ? C16 C17 1.438(8) . ? C17 C18 1.341(8) . ? C17 H17 0.9500 . ? C18 C19 1.459(8) . ? C18 H18 0.9500 . ? C19 C20 1.392(8) . ? C19 N24 1.372(7) . ? C20 C52 1.497(8) . ? N21 H21 0.8800 . ? N23 H23 0.8800 . ? C25 C30 1.365(9) . ? C25 C26 1.403(9) . ? C26 C27 1.408(9) . ? C26 H26 0.9500 . ? C27 C28 1.426(10) . ? C27 H27 0.9500 . ? C28 C29 1.375(10) . ? C28 C31 1.512(10) . ? C29 C30 1.402(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O33A 1.241(11) . ? C31 O33B 1.246(13) . ? C31 O32A 1.320(12) . ? C31 O32B 1.330(14) . ? C34 C35 1.396(8) . ? C34 C39 1.392(8) . ? C35 C36 1.376(8) . ? C35 H35 0.9500 . ? C36 C37 1.413(8) . ? C36 H36 0.9500 . ? C37 C38 1.387(9) . ? C37 C40 1.487(8) . ? C38 C39 1.387(8) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O42 1.243(7) . ? C40 O41 1.297(7) . ? C40 Sm2 2.923(6) 4_646 ? O41 Sm1 2.408(4) 7_656 ? O41 Sm2 2.492(4) 4_646 ? O42 Sm2 2.617(4) 4_646 ? C43 C44 1.386(9) . ? C43 C48 1.390(9) . ? C44 C45 1.395(8) . ? C44 H44 0.9500 . ? C45 C46 1.370(9) . ? C45 H45 0.9500 . ? C46 C47 1.395(9) . ? C46 C49 1.495(8) . ? C47 C48 1.373(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O50 1.239(8) . ? C49 O51 1.267(7) . ? C49 Sm2 2.962(5) 1_545 ? O50 Sm2 2.447(4) 1_545 ? O51 Sm1 2.393(4) 6_556 ? O51 Sm2 2.799(4) 1_545 ? C52 C57 1.372(9) . ? C52 C53 1.411(9) . ? C53 C54 1.377(9) . ? C53 H53 0.9500 . ? C54 C55 1.399(9) . ? C54 H54 0.9500 . ? C55 C56 1.396(8) . ? C55 C58 1.469(8) . ? C56 C57 1.380(8) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O60 1.266(7) . ? C58 O59 1.259(7) . ? O59 Sm1 2.296(4) 2_755 ? C61 N72 1.398(7) . ? C61 C71 1.400(6) . ? C61 C62 1.436(8) . ? C62 C63 1.354(8) . ? C62 H62 0.9500 . ? C63 C64 1.450(7) . ? C63 H63 0.9500 . ? C64 N72 1.370(7) . ? C64 C65 1.399(7) . ? C65 C66 1.382(7) . ? C65 C80 1.512(8) . ? C66 N73 1.377(7) . ? C66 C67 1.456(8) . ? C67 C68 1.378(8) . ? C67 H67 0.9500 . ? C68 C69 1.422(8) . ? C68 H68 0.9500 . ? C69 N73 1.367(7) . ? C69 C70 1.395(6) . ? C70 C69 1.395(6) 2_755 ? C70 C89 1.513(10) . ? C71 C61 1.400(6) 2_755 ? C71 C74 1.491(11) . ? N72 H72 0.8800 . ? N73 H73 0.8800 . ? C74 C75 1.399(7) 2_755 ? C74 C75 1.399(7) . ? C75 C76 1.381(8) . ? C75 H75 0.9500 . ? C76 C77 1.406(7) . ? C76 H76 0.9500 . ? C77 C76 1.406(7) 2_755 ? C77 C78 1.500(12) . ? C78 O79 1.258(6) 2_755 ? C78 O79 1.258(6) . ? C80 C85 1.349(10) . ? C80 C81 1.392(10) . ? C81 C82 1.385(11) . ? C81 H81 0.9500 . ? C82 C83 1.392(13) . ? C82 H82 0.9500 . ? C83 C84 1.332(13) . ? C83 C86A 1.484(17) . ? C83 C86B 1.541(18) . ? C84 C85 1.387(11) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86A O87A 1.22(2) . ? C86A O88A 1.22(2) . ? O88A Sm2 2.276(10) 2_745 ? C86B O87B 1.18(3) . ? C86B O88B 1.20(2) . ? C86B Sm2 2.989(17) 2_745 ? O87B Sm2 2.655(17) 2_745 ? O88B Sm2 2.480(16) 2_745 ? C89 C90 1.399(7) . ? C89 C90 1.399(7) 2_755 ? C90 C91 1.428(8) . ? C90 H90 0.9500 . ? C91 C92 1.384(7) . ? C91 H91 0.9500 . ? C92 C91 1.384(7) 2_755 ? C92 C93 1.480(11) . ? C93 O94 1.268(5) . ? C93 O94 1.268(5) 2_755 ? O94 Sm1 2.375(4) 1_545 ? O95 C96 1.244(7) . ? C96 N97 1.306(8) . ? C96 H96 0.9500 . ? N97 C98 1.460(9) . ? N97 C99 1.482(9) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? O100 H10A 0.9488 . ? O100 H10B 1.0210 . ? O101 H10C 0.9519 . ? O101 H10D 0.9495 . ? 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 O59 Sm1 O94 78.07(14) 2_755 1_565 ? O59 Sm1 O60 123.26(16) 2_755 . ? O94 Sm1 O60 82.93(14) 1_565 . ? O59 Sm1 O51 90.69(15) 2_755 6 ? O94 Sm1 O51 122.51(14) 1_565 6 ? O60 Sm1 O51 142.72(15) . 6 ? O59 Sm1 O79 73.56(14) 2_755 . ? O94 Sm1 O79 130.18(14) 1_565 . ? O60 Sm1 O79 79.70(14) . . ? O51 Sm1 O79 98.12(14) 6 . ? O59 Sm1 O41 131.38(13) 2_755 7_656 ? O94 Sm1 O41 72.55(13) 1_565 7_656 ? O60 Sm1 O41 90.72(14) . 7_656 ? O51 Sm1 O41 74.39(14) 6 7_656 ? O79 Sm1 O41 152.97(14) . 7_656 ? O59 Sm1 O95 143.84(14) 2_755 . ? O94 Sm1 O95 138.08(14) 1_565 . ? O60 Sm1 O95 71.80(14) . . ? O51 Sm1 O95 71.36(13) 6 . ? O79 Sm1 O95 78.15(14) . . ? O41 Sm1 O95 74.84(13) 7_656 . ? O59 Sm1 Sm2 105.92(10) 2_755 6_565 ? O94 Sm1 Sm2 86.02(10) 1_565 6_565 ? O60 Sm1 Sm2 125.54(11) . 6_565 ? O51 Sm1 Sm2 43.06(10) 6 6_565 ? O79 Sm1 Sm2 140.80(10) . 6_565 ? O41 Sm1 Sm2 35.54(9) 7_656 6_565 ? O95 Sm1 Sm2 82.47(9) . 6_565 ? O88A Sm2 O100 84.1(3) 2_765 . ? O88A Sm2 O33A 130.9(3) 2_765 . ? O100 Sm2 O33A 85.2(4) . . ? O88A Sm2 O32B 77.8(4) 2_765 . ? O100 Sm2 O32B 78.7(5) . . ? O33A Sm2 O32B 53.2(3) . . ? O88A Sm2 O50 75.5(3) 2_765 1_565 ? O100 Sm2 O50 73.4(2) . 1_565 ? O33A Sm2 O50 144.6(3) . 1_565 ? O32B Sm2 O50 142.9(4) . 1_565 ? O88A Sm2 O101 88.5(3) 2_765 . ? O100 Sm2 O101 168.8(3) . . ? O33A Sm2 O101 93.3(4) . . ? O32B Sm2 O101 91.6(5) . . ? O50 Sm2 O101 112.8(2) 1_565 . ? O88A Sm2 O33B 129.9(3) 2_765 . ? O100 Sm2 O33B 100.2(5) . . ? O33A Sm2 O33B 15.2(3) . . ? O32B Sm2 O33B 55.0(4) . . ? O50 Sm2 O33B 153.8(3) 1_565 . ? O101 Sm2 O33B 78.1(5) . . ? O88A Sm2 O88B 23.5(4) 2_765 2_765 ? O100 Sm2 O88B 61.4(4) . 2_765 ? O33A Sm2 O88B 118.1(4) . 2_765 ? O32B Sm2 O88B 69.2(5) . 2_765 ? O50 Sm2 O88B 76.1(4) 1_565 2_765 ? O101 Sm2 O88B 110.1(4) . 2_765 ? O33B Sm2 O88B 124.0(5) . 2_765 ? O88A Sm2 O32A 78.7(3) 2_765 . ? O100 Sm2 O32A 94.5(4) . . ? O33A Sm2 O32A 54.7(3) . . ? O32B Sm2 O32A 15.8(3) . . ? O50 Sm2 O32A 152.4(3) 1_565 . ? O101 Sm2 O32A 75.7(4) . . ? O33B Sm2 O32A 51.3(3) . . ? O88B Sm2 O32A 76.3(4) 2_765 . ? O88A Sm2 O41 142.3(3) 2_765 4_656 ? O100 Sm2 O41 123.3(2) . 4_656 ? O33A Sm2 O41 80.9(2) . 4_656 ? O32B Sm2 O41 128.7(3) . 4_656 ? O50 Sm2 O41 87.52(15) 1_565 4_656 ? O101 Sm2 O41 67.25(18) . 4_656 ? O33B Sm2 O41 74.6(3) . 4_656 ? O88B Sm2 O41 161.0(4) 2_765 4_656 ? O32A Sm2 O41 119.3(3) . 4_656 ? O88A Sm2 O42 148.1(3) 2_765 4_656 ? O100 Sm2 O42 72.5(2) . 4_656 ? O33A Sm2 O42 69.5(2) . 4_656 ? O32B Sm2 O42 117.1(3) . 4_656 ? O50 Sm2 O42 77.15(15) 1_565 4_656 ? O101 Sm2 O42 117.36(18) . 4_656 ? O33B Sm2 O42 76.7(3) . 4_656 ? O88B Sm2 O42 131.5(4) 2_765 4_656 ? O32A Sm2 O42 123.7(3) . 4_656 ? O41 Sm2 O42 51.04(13) 4_656 4_656 ? O88A Sm2 O87B 23.6(4) 2_765 2_765 ? O100 Sm2 O87B 107.0(4) . 2_765 ? O33A Sm2 O87B 125.9(4) . 2_765 ? O32B Sm2 O87B 77.3(5) . 2_765 ? O50 Sm2 O87B 87.9(4) 1_565 2_765 ? O101 Sm2 O87B 65.0(4) . 2_765 ? O33B Sm2 O87B 118.1(5) . 2_765 ? O88B Sm2 O87B 45.6(5) 2_765 2_765 ? O32A Sm2 O87B 71.7(4) . 2_765 ? O41 Sm2 O87B 125.5(4) 4_656 2_765 ? O42 Sm2 O87B 164.6(3) 4_656 2_765 ? N21 C1 C20 125.1(5) . . ? N21 C1 C2 109.2(5) . . ? C20 C1 C2 125.4(5) . . ? C3 C2 C1 107.5(6) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.5(5) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? N21 C4 C5 125.0(6) . . ? N21 C4 C3 108.4(5) . . ? C5 C4 C3 126.4(5) . . ? C4 C5 C6 124.5(5) . . ? C4 C5 C25 118.6(6) . . ? C6 C5 C25 116.9(5) . . ? N22 C6 C5 126.2(6) . . ? N22 C6 C7 107.5(5) . . ? C5 C6 C7 126.2(5) . . ? C8 C7 C6 108.5(6) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 C9 107.1(6) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N22 C9 C10 124.8(5) . . ? N22 C9 C8 108.2(5) . . ? C10 C9 C8 126.9(6) . . ? C9 C10 C11 125.5(5) . . ? C9 C10 C34 119.1(5) . . ? C11 C10 C34 115.5(5) . . ? N23 C11 C10 123.7(5) . . ? N23 C11 C12 109.4(5) . . ? C10 C11 C12 126.6(5) . . ? C13 C12 C11 107.6(5) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 106.7(5) . . ? C12 C13 H13 126.6 . . ? C14 C13 H13 126.6 . . ? N23 C14 C15 125.1(5) . . ? N23 C14 C13 110.1(5) . . ? C15 C14 C13 124.8(5) . . ? C16 C15 C14 126.1(5) . . ? C16 C15 C43 118.9(5) . . ? C14 C15 C43 114.9(5) . . ? N24 C16 C15 124.7(5) . . ? N24 C16 C17 108.9(5) . . ? C15 C16 C17 126.4(5) . . ? C18 C17 C16 108.3(5) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? C17 C18 C19 106.5(5) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? C20 C19 N24 125.5(5) . . ? C20 C19 C18 125.7(5) . . ? N24 C19 C18 108.7(5) . . ? C19 C20 C1 124.6(5) . . ? C19 C20 C52 118.0(5) . . ? C1 C20 C52 117.3(5) . . ? C4 N21 C1 107.1(5) . . ? C4 N21 H21 126.4 . . ? C1 N21 H21 126.4 . . ? C6 N22 C9 108.1(5) . . ? C14 N23 C11 106.1(5) . . ? C14 N23 H23 126.9 . . ? C11 N23 H23 126.9 . . ? C16 N24 C19 107.6(5) . . ? C30 C25 C26 119.2(6) . . ? C30 C25 C5 121.7(6) . . ? C26 C25 C5 119.1(6) . . ? C25 C26 C27 120.1(7) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 119.7(7) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 118.8(7) . . ? C29 C28 C31 119.7(7) . . ? C27 C28 C31 121.5(7) . . ? C28 C29 C30 120.6(7) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 121.6(7) . . ? C25 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? O33A C31 O33B 30.4(6) . . ? O33A C31 O32A 124.8(8) . . ? O33B C31 O32A 114.2(9) . . ? O33A C31 O32B 117.5(9) . . ? O33B C31 O32B 124.8(9) . . ? O32A C31 O32B 29.9(6) . . ? O33A C31 C28 118.9(7) . . ? O33B C31 C28 118.0(8) . . ? O32A C31 C28 116.1(7) . . ? O32B C31 C28 117.0(8) . . ? O33A C31 Sm2 61.4(5) . . ? O33B C31 Sm2 62.9(6) . . ? O32A C31 Sm2 63.7(5) . . ? O32B C31 Sm2 62.3(6) . . ? C28 C31 Sm2 178.9(8) . . ? C31 O32A Sm2 88.1(6) . . ? C31 O33A Sm2 92.2(6) . . ? C31 O32B Sm2 89.2(6) . . ? C31 O33B Sm2 90.5(7) . . ? C35 C34 C39 119.0(5) . . ? C35 C34 C10 119.4(5) . . ? C39 C34 C10 121.5(5) . . ? C36 C35 C34 122.1(6) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C37 118.6(6) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C38 C37 C36 119.4(5) . . ? C38 C37 C40 121.0(5) . . ? C36 C37 C40 119.5(5) . . ? C37 C38 C39 121.3(6) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C34 119.5(6) . . ? C38 C39 H39 120.2 . . ? C34 C39 H39 120.2 . . ? O42 C40 O41 120.3(5) . . ? O42 C40 C37 121.5(6) . . ? O41 C40 C37 118.2(5) . . ? O42 C40 Sm2 63.5(3) . 4_646 ? O41 C40 Sm2 58.0(3) . 4_646 ? C37 C40 Sm2 169.1(4) . 4_646 ? C40 O41 Sm1 140.1(3) . 7_656 ? C40 O41 Sm2 95.8(3) . 4_646 ? Sm1 O41 Sm2 110.30(15) 7_656 4_646 ? C40 O42 Sm2 91.4(4) . 4_646 ? C44 C43 C48 119.9(5) . . ? C44 C43 C15 119.6(6) . . ? C48 C43 C15 120.3(6) . . ? C43 C44 C45 118.8(6) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C46 C45 C44 121.6(6) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 118.8(5) . . ? C45 C46 C49 121.7(6) . . ? C47 C46 C49 119.5(6) . . ? C48 C47 C46 120.6(6) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 120.1(6) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? O50 C49 O51 122.9(5) . . ? O50 C49 C46 117.8(6) . . ? O51 C49 C46 119.3(6) . . ? O50 C49 Sm2 53.9(3) . 1_545 ? O51 C49 Sm2 70.2(3) . 1_545 ? C46 C49 Sm2 164.7(4) . 1_545 ? C49 O50 Sm2 101.9(4) . 1_545 ? C49 O51 Sm1 136.0(4) . 6_556 ? C49 O51 Sm2 84.6(3) . 1_545 ? Sm1 O51 Sm2 101.23(14) 6_556 1_545 ? C57 C52 C53 118.8(5) . . ? C57 C52 C20 121.7(5) . . ? C53 C52 C20 119.4(6) . . ? C54 C53 C52 120.2(6) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 120.3(6) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C56 C55 C54 119.2(5) . . ? C56 C55 C58 120.7(6) . . ? C54 C55 C58 120.1(6) . . ? C55 C56 C57 119.9(6) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C52 C57 C56 121.5(6) . . ? C52 C57 H57 119.3 . . ? C56 C57 H57 119.3 . . ? O60 C58 O59 121.9(5) . . ? O60 C58 C55 117.8(6) . . ? O59 C58 C55 120.3(6) . . ? C58 O59 Sm1 174.4(4) . 2_755 ? C58 O60 Sm1 111.9(4) . . ? N72 C61 C71 125.9(5) . . ? N72 C61 C62 108.0(5) . . ? C71 C61 C62 125.8(5) . . ? C63 C62 C61 108.3(5) . . ? C63 C62 H62 125.9 . . ? C61 C62 H62 125.9 . . ? C62 C63 C64 107.3(5) . . ? C62 C63 H63 126.4 . . ? C64 C63 H63 126.4 . . ? N72 C64 C65 125.9(5) . . ? N72 C64 C63 108.7(5) . . ? C65 C64 C63 125.3(5) . . ? C66 C65 C64 126.8(5) . . ? C66 C65 C80 115.1(5) . . ? C64 C65 C80 118.0(5) . . ? C65 C66 N73 126.5(5) . . ? C65 C66 C67 124.7(5) . . ? N73 C66 C67 108.8(5) . . ? C68 C67 C66 105.3(5) . . ? C68 C67 H67 127.3 . . ? C66 C67 H67 127.3 . . ? C67 C68 C69 108.9(5) . . ? C67 C68 H68 125.5 . . ? C69 C68 H68 125.5 . . ? N73 C69 C70 125.6(5) . . ? N73 C69 C68 108.5(5) . . ? C70 C69 C68 125.9(5) . . ? C69 C70 C69 125.5(7) 2_755 . ? C69 C70 C89 117.2(3) 2_755 . ? C69 C70 C89 117.3(3) . . ? C61 C71 C61 124.7(7) . 2_755 ? C61 C71 C74 117.7(3) . . ? C61 C71 C74 117.7(3) 2_755 . ? C64 N72 C61 107.7(5) . . ? C64 N72 H72 126.1 . . ? C61 N72 H72 126.1 . . ? C69 N73 C66 108.4(5) . . ? C69 N73 H73 125.8 . . ? C66 N73 H73 125.8 . . ? C75 C74 C75 117.6(7) 2_755 . ? C75 C74 C71 121.2(4) 2_755 . ? C75 C74 C71 121.2(4) . . ? C76 C75 C74 122.0(6) . . ? C76 C75 H75 119.0 . . ? C74 C75 H75 119.0 . . ? C75 C76 C77 119.4(6) . . ? C75 C76 H76 120.3 . . ? C77 C76 H76 120.3 . . ? C76 C77 C76 119.6(7) . 2_755 ? C76 C77 C78 120.2(4) . . ? C76 C77 C78 120.2(4) 2_755 . ? O79 C78 O79 125.0(8) 2_755 . ? O79 C78 C77 117.5(4) 2_755 . ? O79 C78 C77 117.5(4) . . ? C78 O79 Sm1 141.4(4) . . ? C85 C80 C81 118.4(7) . . ? C85 C80 C65 122.5(6) . . ? C81 C80 C65 118.9(6) . . ? C82 C81 C80 120.4(8) . . ? C82 C81 H81 119.8 . . ? C80 C81 H81 119.8 . . ? C81 C82 C83 120.2(8) . . ? C81 C82 H82 119.9 . . ? C83 C82 H82 119.9 . . ? C84 C83 C82 117.7(7) . . ? C84 C83 C86A 111.7(11) . . ? C82 C83 C86A 130.6(11) . . ? C84 C83 C86B 140.2(12) . . ? C82 C83 C86B 102.1(10) . . ? C86A C83 C86B 28.5(7) . . ? C83 C84 C85 123.0(9) . . ? C83 C84 H84 118.5 . . ? C85 C84 H84 118.5 . . ? C80 C85 C84 120.2(8) . . ? C80 C85 H85 119.9 . . ? C84 C85 H85 119.9 . . ? O87A C86A O88A 114.6(16) . . ? O87A C86A C83 126.9(16) . . ? O88A C86A C83 118.3(15) . . ? C86A O88A Sm2 131.5(10) . 2_745 ? O87B C86B O88B 114.1(19) . . ? O87B C86B C83 110.4(17) . . ? O88B C86B C83 134.0(17) . . ? O87B C86B Sm2 62.3(12) . 2_745 ? O88B C86B Sm2 53.9(10) . 2_745 ? C83 C86B Sm2 172.1(12) . 2_745 ? C86B O87B Sm2 94.5(14) . 2_745 ? C86B O88B Sm2 103.2(12) . 2_745 ? C90 C89 C90 121.5(7) . 2_755 ? C90 C89 C70 119.2(4) . . ? C90 C89 C70 119.2(4) 2_755 . ? C89 C90 C91 118.3(6) . . ? C89 C90 H90 120.9 . . ? C91 C90 H90 120.9 . . ? C92 C91 C90 121.1(6) . . ? C92 C91 H91 119.4 . . ? C90 C91 H91 119.4 . . ? C91 C92 C91 119.6(7) 2_755 . ? C91 C92 C93 120.2(4) 2_755 . ? C91 C92 C93 120.2(4) . . ? O94 C93 O94 124.3(7) . 2_755 ? O94 C93 C92 117.8(4) . . ? O94 C93 C92 117.8(4) 2_755 . ? C93 O94 Sm1 140.3(4) . 1_545 ? C96 O95 Sm1 131.4(4) . . ? O95 C96 N97 124.9(6) . . ? O95 C96 H96 117.6 . . ? N97 C96 H96 117.6 . . ? C96 N97 C98 122.0(6) . . ? C96 N97 C99 120.8(6) . . ? C98 N97 C99 117.1(6) . . ? N97 C98 H98A 109.5 . . ? N97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? N97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N97 C99 H99A 109.5 . . ? N97 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N97 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? Sm2 O100 H10A 108.7 . . ? Sm2 O100 H10B 108.0 . . ? H10A O100 H10B 117.7 . . ? Sm2 O101 H10C 108.9 . . ? Sm2 O101 H10D 109.4 . . ? H10C O101 H10D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.851 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.153 #=================END============================ data_Compound-7 _database_code_depnum_ccdc_archive 'CCDC 627702' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C150 H94 Cu3 Dy4 N14 O30' _chemical_formula_sum 'C150 H94 Cu3 Dy4 N14 O30' _chemical_formula_weight 3413.01 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' O O 0.0106 0.0060 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6137(8) _cell_length_b 23.9695(7) _cell_length_c 30.9377(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.1922(17) _cell_angle_gamma 90.00 _cell_volume 15392.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 13327 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6732 _exptl_absorpt_coefficient_mu 2.395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4475 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.8 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42682 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.1244 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.87 _reflns_number_total 17634 _reflns_number_gt 9406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.080. ; _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^)+(0.0578P)^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 17634 _refine_ls_number_parameters 913 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.913583(16) 0.224987(13) 0.199438(11) 0.02976(11) Uani 1 1 d . . . Dy2 Dy 0.824580(18) 0.691223(13) 0.587260(12) 0.03362(11) Uani 1 1 d . . . C1 C 0.8238(3) 0.3069(3) 0.5328(2) 0.0282(16) Uani 1 1 d . . . C2 C 0.8144(3) 0.3354(3) 0.4908(2) 0.0307(17) Uani 1 1 d . . . H2 H 0.8038 0.3736 0.4850 0.037 Uiso 1 1 calc R . . C3 C 0.8237(3) 0.2969(3) 0.4608(2) 0.0313(17) Uani 1 1 d . . . H3 H 0.8222 0.3034 0.4302 0.038 Uiso 1 1 calc R . . C4 C 0.8363(3) 0.2445(3) 0.4843(2) 0.0274(16) Uani 1 1 d . . . C5 C 0.8574(3) 0.1964(3) 0.4670(2) 0.0278(16) Uani 1 1 d . . . C6 C 0.8671(3) 0.1467(3) 0.4914(2) 0.0325(17) Uani 1 1 d . . . C7 C 0.8857(4) 0.0956(3) 0.4739(3) 0.042(2) Uani 1 1 d . . . H7 H 0.8989 0.0917 0.4472 0.050 Uiso 1 1 calc R . . C8 C 0.8807(4) 0.0543(3) 0.5023(3) 0.044(2) Uani 1 1 d . . . H8 H 0.8907 0.0160 0.5000 0.053 Uiso 1 1 calc R . . C9 C 0.8573(3) 0.0800(3) 0.5371(2) 0.0340(18) Uani 1 1 d . . . C10 C 0.8384(3) 0.0516(3) 0.5705(2) 0.0296(17) Uani 1 1 d . . . C11 C 0.8168(3) 0.0780(3) 0.6034(2) 0.0271(16) Uani 1 1 d . . . C12 C 0.7940(3) 0.0483(3) 0.6367(2) 0.0292(16) Uani 1 1 d . . . H12 H 0.7878 0.0092 0.6384 0.035 Uiso 1 1 calc R . . C13 C 0.7838(3) 0.0872(3) 0.6645(2) 0.0329(17) Uani 1 1 d . . . H13 H 0.7680 0.0809 0.6898 0.040 Uiso 1 1 calc R . . C14 C 0.8004(3) 0.1400(3) 0.6500(2) 0.0249(15) Uani 1 1 d . . . C15 C 0.8065(3) 0.1890(3) 0.6749(2) 0.0285(16) Uani 1 1 d . . . C16 C 0.8276(3) 0.2390(3) 0.6598(2) 0.0282(16) Uani 1 1 d . . . C17 C 0.8403(3) 0.2890(3) 0.6853(2) 0.0327(17) Uani 1 1 d . . . H17 H 0.8420 0.2930 0.7161 0.039 Uiso 1 1 calc R . . C18 C 0.8497(3) 0.3298(3) 0.6578(2) 0.0335(18) Uani 1 1 d . . . H18 H 0.8611 0.3674 0.6657 0.040 Uiso 1 1 calc R . . C19 C 0.8391(3) 0.3049(3) 0.6142(2) 0.0288(16) Uani 1 1 d . . . C20 C 0.8310(3) 0.3331(3) 0.5740(3) 0.0308(17) Uani 1 1 d . . . N21 N 0.8328(2) 0.2502(2) 0.52807(18) 0.0244(13) Uani 1 1 d . . . N22 N 0.8511(3) 0.1377(2) 0.53050(18) 0.0267(13) Uani 1 1 d . . . N23 N 0.8183(3) 0.1339(2) 0.61071(19) 0.0287(14) Uani 1 1 d . . . N24 N 0.8310(2) 0.2475(2) 0.61724(18) 0.0240(13) Uani 1 1 d . . . C25 C 0.8731(4) 0.1999(3) 0.4235(2) 0.0314(17) Uani 1 1 d . . . C26 C 0.8263(3) 0.2031(3) 0.3838(3) 0.0328(18) Uani 1 1 d . . . H26 H 0.7824 0.2018 0.3836 0.039 Uiso 1 1 calc R . . C27 C 0.8420(3) 0.2082(3) 0.3436(2) 0.0301(17) Uani 1 1 d . . . H27 H 0.8088 0.2098 0.3160 0.036 Uiso 1 1 calc R . . C28 C 0.9065(3) 0.2109(2) 0.3434(2) 0.0255(16) Uani 1 1 d . . . C29 C 0.9539(4) 0.2064(3) 0.3841(3) 0.0401(19) Uani 1 1 d . . . H29 H 0.9980 0.2071 0.3844 0.048 Uiso 1 1 calc R . . C30 C 0.9383(3) 0.2008(3) 0.4238(3) 0.042(2) Uani 1 1 d . . . H30 H 0.9712 0.1975 0.4514 0.050 Uiso 1 1 calc R . . C31 C 0.9234(4) 0.2186(3) 0.3003(2) 0.0293(17) Uani 1 1 d . . . O32 O 0.8787(2) 0.22042(18) 0.26423(16) 0.0323(11) Uani 1 1 d . . . O33 O 0.9825(2) 0.22300(18) 0.30117(16) 0.0341(12) Uani 1 1 d . . . C34 C 0.8409(4) -0.0106(3) 0.5713(2) 0.0306(17) Uani 1 1 d . . . C35 C 0.8971(4) -0.0372(3) 0.5981(3) 0.044(2) Uani 1 1 d . . . H35 H 0.9351 -0.0163 0.6113 0.053 Uiso 1 1 calc R . . C36 C 0.8954(4) -0.0956(3) 0.6047(3) 0.043(2) Uani 1 1 d . . . H36 H 0.9323 -0.1139 0.6232 0.052 Uiso 1 1 calc R . . C37 C 0.8397(3) -0.1268(3) 0.5843(2) 0.0271(16) Uani 1 1 d . . . C38 C 0.7881(4) -0.0993(3) 0.5574(2) 0.041(2) Uani 1 1 d . . . H38 H 0.7510 -0.1203 0.5424 0.049 Uiso 1 1 calc R . . C39 C 0.7871(4) -0.0421(3) 0.5509(2) 0.0382(19) Uani 1 1 d . . . H39 H 0.7495 -0.0246 0.5325 0.046 Uiso 1 1 calc R . . C40 C 0.8376(4) -0.1872(3) 0.5926(3) 0.039(2) Uani 1 1 d . . . O41 O 0.7893(3) -0.21449(19) 0.57239(18) 0.0411(13) Uani 1 1 d . . . O42 O 0.8853(2) -0.20993(18) 0.62082(17) 0.0370(12) Uani 1 1 d . . . C43 C 0.7888(3) 0.1872(3) 0.7183(2) 0.0270(16) Uani 1 1 d . . . C44 C 0.7246(3) 0.1780(3) 0.7174(2) 0.0289(16) Uani 1 1 d . . . H44 H 0.6933 0.1705 0.6896 0.035 Uiso 1 1 calc R . . C45 C 0.7067(3) 0.1800(2) 0.7566(2) 0.0282(17) Uani 1 1 d . . . H45 H 0.6629 0.1733 0.7554 0.034 Uiso 1 1 calc R . . C46 C 0.7501(3) 0.1913(3) 0.7974(2) 0.0255(15) Uani 1 1 d . . . C47 C 0.8150(3) 0.1973(3) 0.7989(2) 0.0362(18) Uani 1 1 d . . . H47 H 0.8465 0.2020 0.8270 0.043 Uiso 1 1 calc R . . C48 C 0.8335(3) 0.1962(3) 0.7592(2) 0.0336(18) Uani 1 1 d . . . H48 H 0.8775 0.2018 0.7604 0.040 Uiso 1 1 calc R . . C49 C 0.7300(4) 0.1985(3) 0.8384(3) 0.0296(17) Uani 1 1 d . . . O50 O 0.6688(2) 0.20828(17) 0.83337(14) 0.0251(10) Uani 1 1 d . . . O51 O 0.7676(2) 0.19606(18) 0.87664(15) 0.0307(11) Uani 1 1 d . . . C52 C 0.8308(3) 0.3964(3) 0.5758(3) 0.0377(19) Uani 1 1 d . . . C53 C 0.8760(4) 0.4272(3) 0.5620(3) 0.045(2) Uani 1 1 d . . . H53 H 0.9076 0.4089 0.5510 0.054 Uiso 1 1 calc R . . C54 C 0.8749(5) 0.4858(3) 0.5642(3) 0.062(3) Uani 1 1 d . . . H54 H 0.9059 0.5071 0.5549 0.075 Uiso 1 1 calc R . . C55 C 0.8291(5) 0.5122(3) 0.5797(3) 0.061(3) Uani 1 1 d . . . C56 C 0.7835(4) 0.4821(3) 0.5934(3) 0.060(3) Uani 1 1 d . . . H56 H 0.7522 0.5005 0.6046 0.072 Uiso 1 1 calc R . . C57 C 0.7845(4) 0.4248(3) 0.5908(3) 0.050(2) Uani 1 1 d . . . H57 H 0.7525 0.4040 0.5995 0.060 Uiso 1 1 calc R . . C58 C 0.8278(5) 0.5748(3) 0.5819(4) 0.075(3) Uani 1 1 d . . . O59 O 0.8053(3) 0.5987(2) 0.6102(2) 0.077(2) Uani 1 1 d . . . O60 O 0.8502(4) 0.6031(2) 0.5544(2) 0.084(2) Uani 1 1 d . . . Cu1 Cu 0.83309(4) 0.19250(3) 0.57157(3) 0.0328(2) Uani 1 1 d . . . C61 C 1.0000 0.8673(4) 0.2500 0.035(3) Uani 1 2 d S . . C62 C 0.9984(3) 0.8394(3) 0.2101(2) 0.0283(16) Uani 1 1 d . . . C63 C 1.0000(4) 0.8666(3) 0.1688(3) 0.0410(19) Uani 1 1 d . . . H63 H 0.9957 0.9055 0.1626 0.049 Uiso 1 1 calc R . . C64 C 1.0088(3) 0.8269(3) 0.1409(2) 0.0340(18) Uani 1 1 d . . . H64 H 1.0136 0.8324 0.1116 0.041 Uiso 1 1 calc R . . C65 C 1.0098(3) 0.7742(3) 0.1631(2) 0.0310(17) Uani 1 1 d . . . C66 C 1.0214(3) 0.7236(3) 0.1446(3) 0.0348(18) Uani 1 1 d . . . C67 C 1.0186(3) 0.6729(3) 0.1657(2) 0.0295(16) Uani 1 1 d . . . C68 C 1.0232(3) 0.6202(3) 0.1450(3) 0.0401(19) Uani 1 1 d . . . H68 H 1.0302 0.6144 0.1163 0.048 Uiso 1 1 calc R . . C69 C 1.0156(4) 0.5803(3) 0.1737(3) 0.044(2) Uani 1 1 d . . . H69 H 1.0164 0.5411 0.1693 0.053 Uiso 1 1 calc R . . C70 C 1.0062(3) 0.6082(3) 0.2118(2) 0.0292(17) Uani 1 1 d . . . C71 C 1.0000 0.5792(4) 0.2500 0.027(2) Uani 1 2 d S . . N72 N 1.0030(3) 0.7819(2) 0.20572(18) 0.0266(13) Uani 1 1 d . . . N73 N 1.0091(3) 0.6657(2) 0.20701(19) 0.0304(14) Uani 1 1 d . . . C74 C 1.0000 0.9303(4) 0.2500 0.030(2) Uani 1 2 d S . . C75 C 0.9476(4) 0.9611(3) 0.2249(3) 0.044(2) Uani 1 1 d . . . H75 H 0.9105 0.9418 0.2076 0.053 Uiso 1 1 calc R . . C76 C 0.9477(4) 1.0178(3) 0.2245(3) 0.0383(19) Uani 1 1 d . . . H76 H 0.9110 1.0366 0.2062 0.046 Uiso 1 1 calc R . . C77 C 1.0000 1.0501(3) 0.2500 0.029(2) Uani 1 2 d SD . . C78 C 1.0000 1.1089(3) 0.2500 0.030(2) Uani 1 2 d SD . . O79 O 1.0490(2) 1.13563(17) 0.27398(17) 0.0370(12) Uani 1 1 d . . . C80 C 1.0362(4) 0.7230(3) 0.1007(3) 0.0318(17) Uani 1 1 d . . . C81 C 1.0998(4) 0.7220(3) 0.0984(3) 0.063(3) Uani 1 1 d . . . H81 H 1.1348 0.7242 0.1250 0.075 Uiso 1 1 calc R . . C82 C 1.1113(5) 0.7176(3) 0.0554(4) 0.074(3) Uani 1 1 d . . . H82 H 1.1547 0.7187 0.0543 0.089 Uiso 1 1 calc R . . C83 C 1.0641(5) 0.7117(3) 0.0155(3) 0.053(2) Uani 1 1 d D . . C84 C 1.0036(5) 0.7133(4) 0.0207(3) 0.076(3) Uani 1 1 d . . . H84 H 0.9684 0.7105 -0.0057 0.091 Uiso 1 1 calc R . . C85 C 0.9898(4) 0.7186(4) 0.0614(3) 0.064(3) Uani 1 1 d . . . H85 H 0.9460 0.7191 0.0618 0.077 Uiso 1 1 calc R . . C86 C 1.0777(6) 0.7062(4) -0.0262(3) 0.068(3) Uani 1 1 d D . . O87 O 1.0335(5) 0.6873(5) -0.0595(3) 0.114(5) Uani 1 1 d . . . O88 O 1.1305(4) 0.7171(2) -0.0313(3) 0.095(3) Uani 1 1 d . . . C89 C 1.0000 0.5176(4) 0.2500 0.027(2) Uani 1 2 d S . . C90 C 0.9477(3) 0.4883(3) 0.2251(3) 0.0353(18) Uani 1 1 d . . . H90 H 0.9111 0.5081 0.2077 0.042 Uiso 1 1 calc R . . C91 C 0.9468(3) 0.4306(3) 0.2247(2) 0.0351(18) Uani 1 1 d . . . H91 H 0.9100 0.4113 0.2072 0.042 Uiso 1 1 calc R . . C92 C 1.0000 0.4008(4) 0.2500 0.026(2) Uani 1 2 d S . . C93 C 1.0000 0.3383(4) 0.2500 0.033(3) Uani 1 2 d S . . O94 O 0.9508(2) 0.31367(17) 0.22724(18) 0.0386(13) Uani 1 1 d . . . Cu2 Cu 1.0000 0.72357(5) 0.2500 0.0354(3) Uani 1 2 d S . . O95 O 0.8153(2) 0.17105(18) 0.18042(16) 0.0330(12) Uani 1 1 d . . . C96 C 0.7771(4) 0.1579(4) 0.2028(3) 0.060(3) Uani 1 1 d . . . H96 H 0.7868 0.1719 0.2326 0.072 Uiso 1 1 calc R . . N97 N 0.7266(3) 0.1278(3) 0.1897(3) 0.067(2) Uani 1 1 d . . . C98 C 0.7059(4) 0.1028(4) 0.1454(3) 0.079(3) Uani 1 1 d . . . H98A H 0.7032 0.1315 0.1225 0.118 Uiso 1 1 calc R . . H98B H 0.6635 0.0856 0.1411 0.118 Uiso 1 1 calc R . . H98C H 0.7370 0.0741 0.1427 0.118 Uiso 1 1 calc R . . C99 C 0.6872(5) 0.1144(5) 0.2204(3) 0.096(4) Uani 1 1 d . . . H99A H 0.6858 0.0738 0.2241 0.143 Uiso 1 1 calc R . . H99B H 0.6434 0.1286 0.2077 0.143 Uiso 1 1 calc R . . H99C H 0.7063 0.1318 0.2498 0.143 Uiso 1 1 calc R . . O100 O 0.7294(3) 0.6826(4) 0.5264(2) 0.116(3) Uani 1 1 d . . . HOA H 0.7108 0.7197 0.5181 0.139 Uiso 1 1 d R . . HOB H 0.6982 0.6592 0.5357 0.139 Uiso 1 1 d R . . O101 O 0.9321(3) 0.6748(3) 0.6339(2) 0.097(3) Uani 1 1 d . . . H10A H 0.9614 0.6722 0.6148 0.146 Uiso 1 1 d R . . H10B H 0.9330 0.6396 0.6501 0.146 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0322(2) 0.02937(18) 0.0287(2) -0.00421(15) 0.01022(16) 0.00148(16) Dy2 0.0492(2) 0.02618(18) 0.0270(2) -0.00121(15) 0.01321(18) -0.00207(16) C1 0.031(4) 0.025(3) 0.034(4) -0.002(3) 0.017(4) -0.005(3) C2 0.028(4) 0.030(4) 0.036(5) 0.002(3) 0.012(4) -0.003(3) C3 0.031(4) 0.028(4) 0.039(5) 0.005(3) 0.017(4) 0.000(3) C4 0.025(4) 0.029(4) 0.032(4) 0.005(3) 0.016(3) -0.002(3) C5 0.030(4) 0.033(4) 0.024(4) 0.007(3) 0.014(3) 0.003(3) C6 0.033(4) 0.035(4) 0.036(5) 0.003(3) 0.020(4) 0.003(3) C7 0.055(5) 0.041(4) 0.040(5) 0.002(4) 0.031(4) 0.011(4) C8 0.067(6) 0.034(4) 0.035(5) 0.005(4) 0.021(4) 0.013(4) C9 0.043(5) 0.028(4) 0.038(5) 0.003(3) 0.021(4) 0.011(3) C10 0.037(4) 0.027(4) 0.022(4) -0.002(3) 0.003(3) 0.001(3) C11 0.028(4) 0.028(4) 0.026(4) 0.001(3) 0.009(3) 0.004(3) C12 0.035(4) 0.033(4) 0.023(4) 0.006(3) 0.012(3) 0.008(3) C13 0.034(4) 0.046(4) 0.025(4) 0.008(3) 0.018(4) 0.003(3) C14 0.031(4) 0.027(4) 0.019(4) 0.000(3) 0.012(3) -0.001(3) C15 0.028(4) 0.033(4) 0.027(4) -0.004(3) 0.013(3) 0.002(3) C16 0.029(4) 0.032(4) 0.029(4) 0.001(3) 0.016(3) 0.000(3) C17 0.031(4) 0.039(4) 0.033(4) -0.009(4) 0.016(4) -0.006(3) C18 0.028(4) 0.031(4) 0.041(5) -0.004(4) 0.008(4) 0.000(3) C19 0.026(4) 0.032(4) 0.035(5) -0.002(3) 0.020(3) -0.005(3) C20 0.028(4) 0.025(4) 0.045(5) -0.004(3) 0.019(4) -0.003(3) N21 0.025(3) 0.023(3) 0.030(3) 0.004(3) 0.015(3) 0.002(2) N22 0.038(3) 0.022(3) 0.026(3) 0.004(2) 0.019(3) 0.005(3) N23 0.033(3) 0.024(3) 0.034(4) 0.004(3) 0.017(3) -0.002(3) N24 0.028(3) 0.025(3) 0.022(3) 0.007(3) 0.011(3) 0.006(2) C25 0.038(5) 0.036(4) 0.025(4) 0.004(3) 0.017(4) 0.003(3) C26 0.029(4) 0.031(4) 0.046(5) 0.001(4) 0.024(4) 0.000(3) C27 0.025(4) 0.045(4) 0.018(4) 0.010(3) 0.002(3) -0.001(3) C28 0.034(4) 0.020(3) 0.027(4) 0.003(3) 0.017(4) 0.003(3) C29 0.031(4) 0.058(5) 0.037(5) 0.007(4) 0.020(4) 0.009(4) C30 0.029(4) 0.071(5) 0.029(5) 0.004(4) 0.012(4) 0.009(4) C31 0.041(5) 0.021(3) 0.031(5) 0.003(3) 0.018(4) 0.001(3) O32 0.042(3) 0.034(3) 0.022(3) 0.002(2) 0.010(3) -0.004(2) O33 0.042(3) 0.031(3) 0.041(3) 0.001(2) 0.030(3) -0.004(2) C34 0.046(5) 0.029(4) 0.018(4) -0.003(3) 0.011(4) 0.009(4) C35 0.061(6) 0.032(4) 0.043(5) 0.002(4) 0.018(5) 0.001(4) C36 0.052(5) 0.042(4) 0.038(5) 0.016(4) 0.017(4) 0.013(4) C37 0.030(4) 0.039(4) 0.011(4) -0.005(3) 0.005(3) 0.014(3) C38 0.051(5) 0.039(4) 0.033(5) -0.002(4) 0.014(4) -0.007(4) C39 0.051(5) 0.036(4) 0.028(5) 0.001(4) 0.011(4) 0.010(4) C40 0.056(6) 0.033(4) 0.039(5) 0.017(4) 0.034(5) 0.019(4) O41 0.049(3) 0.032(3) 0.047(4) 0.001(3) 0.020(3) 0.000(3) O42 0.049(3) 0.034(3) 0.038(3) 0.008(2) 0.028(3) 0.012(3) C43 0.036(4) 0.026(4) 0.021(4) -0.004(3) 0.010(4) 0.004(3) C44 0.033(4) 0.031(4) 0.026(4) 0.002(3) 0.013(3) 0.005(3) C45 0.022(4) 0.032(4) 0.037(5) -0.002(3) 0.019(4) 0.000(3) C46 0.025(4) 0.029(4) 0.022(4) 0.005(3) 0.007(3) 0.004(3) C47 0.032(4) 0.049(5) 0.024(4) 0.001(4) 0.003(4) 0.004(4) C48 0.031(4) 0.045(4) 0.031(5) 0.002(4) 0.019(4) 0.010(3) C49 0.036(5) 0.020(3) 0.031(5) 0.003(3) 0.008(4) -0.002(3) O50 0.028(3) 0.029(2) 0.019(3) 0.005(2) 0.008(2) 0.005(2) O51 0.027(3) 0.046(3) 0.019(3) 0.002(2) 0.006(2) 0.004(2) C52 0.036(5) 0.039(4) 0.042(5) -0.004(4) 0.017(4) -0.003(4) C53 0.060(5) 0.036(4) 0.052(6) -0.003(4) 0.037(5) -0.008(4) C54 0.096(7) 0.042(5) 0.063(7) -0.005(4) 0.047(6) -0.020(5) C55 0.109(8) 0.036(5) 0.055(6) -0.019(4) 0.049(6) -0.019(5) C56 0.078(7) 0.033(4) 0.084(7) -0.008(5) 0.049(6) -0.003(4) C57 0.056(5) 0.030(4) 0.075(7) -0.002(4) 0.036(5) -0.003(4) C58 0.125(9) 0.029(5) 0.096(9) -0.006(5) 0.072(8) -0.017(5) O59 0.142(6) 0.031(3) 0.093(5) -0.007(3) 0.089(5) -0.009(3) O60 0.169(7) 0.029(3) 0.087(5) -0.007(3) 0.089(5) -0.014(4) Cu1 0.0400(5) 0.0311(5) 0.0336(5) 0.0010(4) 0.0205(5) 0.0008(4) C61 0.028(6) 0.040(6) 0.040(7) 0.000 0.015(5) 0.000 C62 0.026(4) 0.026(4) 0.036(5) 0.000(3) 0.013(4) -0.002(3) C63 0.052(5) 0.032(4) 0.043(5) 0.006(4) 0.020(4) 0.008(4) C64 0.041(5) 0.032(4) 0.031(5) 0.006(3) 0.013(4) 0.000(3) C65 0.029(4) 0.033(4) 0.031(4) 0.008(3) 0.009(3) 0.000(3) C66 0.038(4) 0.028(4) 0.045(5) -0.002(3) 0.024(4) -0.001(3) C67 0.026(4) 0.035(4) 0.029(4) -0.006(3) 0.010(4) -0.002(3) C68 0.047(5) 0.033(4) 0.045(5) -0.002(4) 0.020(4) -0.004(4) C69 0.058(5) 0.029(4) 0.051(6) -0.006(4) 0.023(5) -0.009(4) C70 0.027(4) 0.027(4) 0.033(5) -0.002(3) 0.007(4) 0.003(3) C71 0.022(5) 0.023(5) 0.033(6) 0.000 0.005(5) 0.000 N72 0.031(3) 0.024(3) 0.029(3) 0.003(3) 0.016(3) 0.001(2) N73 0.031(3) 0.025(3) 0.037(4) 0.001(3) 0.013(3) 0.001(3) C74 0.021(6) 0.033(5) 0.034(6) 0.000 0.007(5) 0.000 C75 0.037(5) 0.024(4) 0.063(6) -0.005(4) 0.000(4) -0.006(4) C76 0.042(5) 0.026(4) 0.042(5) 0.000(4) 0.003(4) 0.009(4) C77 0.034(6) 0.022(5) 0.030(6) 0.000 0.006(5) 0.000 C78 0.028(6) 0.022(5) 0.035(7) 0.000 -0.002(5) 0.000 O79 0.036(3) 0.022(2) 0.047(3) 0.001(2) 0.004(3) -0.001(2) C80 0.040(4) 0.026(4) 0.039(5) -0.004(3) 0.026(4) -0.005(3) C81 0.060(6) 0.073(6) 0.064(6) -0.047(5) 0.032(5) -0.028(5) C82 0.083(7) 0.060(6) 0.115(10) -0.040(6) 0.087(8) -0.032(5) C83 0.074(7) 0.049(5) 0.049(6) 0.010(5) 0.039(6) 0.008(5) C84 0.059(6) 0.142(9) 0.030(5) 0.018(6) 0.018(5) 0.034(6) C85 0.029(5) 0.131(9) 0.037(5) 0.011(6) 0.018(4) 0.019(5) C86 0.095(9) 0.063(6) 0.060(7) 0.018(6) 0.044(7) 0.035(6) O87 0.126(9) 0.175(14) 0.043(5) 0.028(7) 0.039(6) 0.057(9) O88 0.176(8) 0.035(3) 0.122(7) 0.006(4) 0.122(6) 0.008(4) C89 0.024(6) 0.030(5) 0.022(6) 0.000 -0.003(5) 0.000 C90 0.037(5) 0.027(4) 0.040(5) 0.004(3) 0.008(4) 0.008(3) C91 0.033(4) 0.034(4) 0.034(5) -0.004(4) 0.004(4) -0.002(3) C92 0.024(6) 0.028(5) 0.026(6) 0.000 0.005(5) 0.000 C93 0.033(6) 0.029(5) 0.044(7) 0.000 0.023(6) 0.000 O94 0.033(3) 0.022(3) 0.056(4) 0.001(2) 0.006(3) -0.001(2) Cu2 0.0372(7) 0.0319(7) 0.0407(8) 0.000 0.0171(7) 0.000 O95 0.031(3) 0.038(3) 0.031(3) 0.002(2) 0.009(2) -0.002(2) C96 0.073(7) 0.069(6) 0.041(6) -0.003(5) 0.022(5) -0.021(5) N97 0.056(5) 0.075(5) 0.080(6) -0.016(5) 0.038(5) -0.038(4) C98 0.068(7) 0.115(9) 0.065(7) -0.036(6) 0.038(6) -0.020(6) C99 0.083(8) 0.146(11) 0.074(8) -0.028(7) 0.049(7) -0.046(7) O100 0.089(5) 0.207(9) 0.056(5) -0.083(5) 0.028(4) 0.007(5) O101 0.063(4) 0.169(7) 0.071(5) 0.054(5) 0.037(4) 0.059(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 Dy1 O33 2.251(4) 2_755 ? Dy1 O32 2.332(4) . ? Dy1 O79 2.355(4) 2_745 ? Dy1 O94 2.349(4) . ? Dy1 O42 2.364(5) 6 ? Dy1 O50 2.399(4) 7_656 ? Dy1 O95 2.414(5) . ? Dy2 O88 2.293(6) 2_755 ? Dy2 O100 2.379(7) . ? Dy2 O41 2.388(5) 1_565 ? Dy2 O101 2.402(6) . ? Dy2 O59 2.401(5) . ? Dy2 O50 2.454(4) 4_656 ? Dy2 O60 2.472(5) . ? Dy2 O51 2.544(4) 4_656 ? Dy2 O42 2.766(5) 1_565 ? Dy2 C58 2.797(8) . ? Dy2 C49 2.867(7) 4_656 ? Dy2 C40 2.928(7) 1_565 ? C1 N21 1.386(8) . ? C1 C20 1.388(9) . ? C1 C2 1.433(9) . ? C2 C3 1.361(9) . ? C2 H2 0.9500 . ? C3 C4 1.439(9) . ? C3 H3 0.9500 . ? C4 N21 1.383(8) . ? C4 C5 1.402(9) . ? C5 C6 1.394(9) . ? C5 C25 1.479(9) . ? C6 N22 1.364(8) . ? C6 C7 1.443(9) . ? C7 C8 1.346(9) . ? C7 H7 0.9500 . ? C8 C9 1.450(9) . ? C8 H8 0.9500 . ? C9 C10 1.391(9) . ? C9 N22 1.397(8) . ? C10 C11 1.385(9) . ? C10 C34 1.493(9) . ? C11 N23 1.358(8) . ? C11 C12 1.448(9) . ? C12 C13 1.329(9) . ? C12 H12 0.9500 . ? C13 C14 1.421(9) . ? C13 H13 0.9500 . ? C14 N23 1.383(8) . ? C14 C15 1.390(9) . ? C15 C16 1.407(9) . ? C15 C43 1.495(9) . ? C16 N24 1.355(8) . ? C16 C17 1.417(9) . ? C17 C18 1.347(9) . ? C17 H17 0.9500 . ? C18 C19 1.433(9) . ? C18 H18 0.9500 . ? C19 C20 1.383(10) . ? C19 N24 1.394(8) . ? C20 C52 1.519(9) . ? N21 Cu1 1.928(5) . ? N22 Cu1 1.942(5) . ? N23 Cu1 1.939(5) . ? N24 Cu1 1.942(5) . ? C25 C26 1.359(10) . ? C25 C30 1.405(10) . ? C26 C27 1.382(9) . ? C26 H26 0.9500 . ? C27 C28 1.398(9) . ? C27 H27 0.9500 . ? C28 C29 1.389(9) . ? C28 C31 1.489(9) . ? C29 C30 1.369(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O32 1.256(8) . ? C31 O33 1.275(8) . ? O33 Dy1 2.251(4) 2_755 ? C34 C39 1.383(10) . ? C34 C35 1.417(10) . ? C35 C36 1.416(9) . ? C35 H35 0.9500 . ? C36 C37 1.410(10) . ? C36 H36 0.9500 . ? C37 C38 1.362(9) . ? C37 C40 1.472(10) . ? C38 C39 1.384(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O41 1.242(9) . ? C40 O42 1.273(9) . ? C40 Dy2 2.928(7) 1_545 ? O41 Dy2 2.388(5) 1_545 ? O42 Dy1 2.364(5) 6_556 ? O42 Dy2 2.766(5) 1_545 ? C43 C48 1.378(9) . ? C43 C44 1.399(9) . ? C44 C45 1.372(9) . ? C44 H44 0.9500 . ? C45 C46 1.375(9) . ? C45 H45 0.9500 . ? C46 C47 1.398(9) . ? C46 C49 1.461(9) . ? C47 C48 1.394(9) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O51 1.236(8) . ? C49 O50 1.308(8) . ? C49 Dy2 2.867(7) 4_646 ? O50 Dy1 2.399(4) 7_656 ? O50 Dy2 2.454(4) 4_646 ? O51 Dy2 2.544(4) 4_646 ? C52 C53 1.384(9) . ? C52 C57 1.394(9) . ? C53 C54 1.407(10) . ? C53 H53 0.9500 . ? C54 C55 1.369(11) . ? C54 H54 0.9500 . ? C55 C56 1.381(11) . ? C55 C58 1.502(11) . ? C56 C57 1.375(10) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O59 1.251(10) . ? C58 O60 1.285(9) . ? C61 C62 1.397(8) 2_755 ? C61 C62 1.397(8) . ? C61 C74 1.509(13) . ? C62 N72 1.392(8) . ? C62 C63 1.444(9) . ? C63 C64 1.333(9) . ? C63 H63 0.9500 . ? C64 C65 1.433(9) . ? C64 H64 0.9500 . ? C65 N72 1.380(8) . ? C65 C66 1.394(9) . ? C66 C67 1.388(9) . ? C66 C80 1.479(9) . ? C67 N73 1.362(8) . ? C67 C68 1.432(9) . ? C68 C69 1.346(9) . ? C68 H68 0.9500 . ? C69 C70 1.419(9) . ? C69 H69 0.9500 . ? C70 N73 1.390(8) . ? C70 C71 1.408(8) . ? C71 C70 1.408(8) 2_755 ? C71 C89 1.478(12) . ? N72 Cu2 1.971(5) . ? N73 Cu2 1.969(5) . ? C74 C75 1.393(9) . ? C74 C75 1.393(9) 2_755 ? C75 C76 1.360(9) . ? C75 H75 0.9500 . ? C76 C77 1.415(8) . ? C76 H76 0.9500 . ? C77 C76 1.415(8) 2_755 ? C77 C78 1.410(10) . ? C78 O79 1.283(5) . ? C78 O79 1.283(5) 2_755 ? O79 Dy1 2.355(4) 2_765 ? C80 C85 1.347(11) . ? C80 C81 1.397(10) . ? C81 C82 1.421(12) . ? C81 H81 0.9500 . ? C82 C83 1.371(13) . ? C82 H82 0.9500 . ? C83 C84 1.361(12) . ? C83 C86 1.409(14) . ? C84 C85 1.380(11) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 O88 1.224(12) . ? C86 O87 1.277(13) . ? O88 Dy2 2.293(6) 2_755 ? C89 C90 1.371(8) 2_755 ? C89 C90 1.371(8) . ? C90 C91 1.383(9) . ? C90 H90 0.9500 . ? C91 C92 1.393(8) . ? C91 H91 0.9500 . ? C92 C91 1.393(8) 2_755 ? C92 C93 1.498(13) . ? C93 O94 1.248(6) 2_755 ? C93 O94 1.249(6) . ? Cu2 N73 1.969(5) 2_755 ? Cu2 N72 1.971(5) 2_755 ? O95 C96 1.257(9) . ? C96 N97 1.275(10) . ? C96 H96 0.9500 . ? N97 C98 1.447(10) . ? N97 C99 1.478(10) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? O100 HOA 0.9800 . ? O100 HOB 0.9800 . ? O101 H10A 0.9800 . ? O101 H10B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O33 Dy1 O32 124.63(17) 2_755 . ? O33 Dy1 O79 74.80(16) 2_755 2_745 ? O32 Dy1 O79 79.56(16) . 2_745 ? O33 Dy1 O94 77.41(16) 2_755 . ? O32 Dy1 O94 83.53(16) . . ? O79 Dy1 O94 130.24(17) 2_745 . ? O33 Dy1 O42 87.75(17) 2_755 6 ? O32 Dy1 O42 145.49(17) . 6 ? O79 Dy1 O42 100.70(16) 2_745 6 ? O94 Dy1 O42 118.60(17) . 6 ? O33 Dy1 O50 129.44(15) 2_755 7_656 ? O32 Dy1 O50 90.87(15) . 7_656 ? O79 Dy1 O50 153.67(15) 2_745 7_656 ? O94 Dy1 O50 71.91(15) . 7_656 ? O42 Dy1 O50 73.61(15) 6 7_656 ? O33 Dy1 O95 142.95(15) 2_755 . ? O32 Dy1 O95 73.22(16) . . ? O79 Dy1 O95 77.93(15) 2_745 . ? O94 Dy1 O95 139.60(16) . . ? O42 Dy1 O95 73.14(16) 6 . ? O50 Dy1 O95 75.82(15) 7_656 . ? O88 Dy2 O100 83.2(3) 2_755 . ? O88 Dy2 O41 77.2(2) 2_755 1_565 ? O100 Dy2 O41 76.7(2) . 1_565 ? O88 Dy2 O101 87.4(3) 2_755 . ? O100 Dy2 O101 160.0(2) . . ? O41 Dy2 O101 118.3(2) 1_565 . ? O88 Dy2 O59 128.18(19) 2_755 . ? O100 Dy2 O59 88.3(3) . . ? O41 Dy2 O59 149.2(2) 1_565 . ? O101 Dy2 O59 83.6(3) . . ? O88 Dy2 O50 142.3(2) 2_755 4_656 ? O100 Dy2 O50 127.02(18) . 4_656 ? O41 Dy2 O50 87.79(16) 1_565 4_656 ? O101 Dy2 O50 69.55(19) . 4_656 ? O59 Dy2 O50 79.88(17) . 4_656 ? O88 Dy2 O60 74.36(19) 2_755 . ? O100 Dy2 O60 81.1(2) . . ? O41 Dy2 O60 145.60(19) 1_565 . ? O101 Dy2 O60 79.4(3) . . ? O59 Dy2 O60 53.81(18) . . ? O50 Dy2 O60 126.61(18) 4_656 . ? O88 Dy2 O51 150.1(2) 2_755 4_656 ? O100 Dy2 O51 74.98(19) . 4_656 ? O41 Dy2 O51 78.15(16) 1_565 4_656 ? O101 Dy2 O51 119.30(18) . 4_656 ? O59 Dy2 O51 71.98(18) . 4_656 ? O50 Dy2 O51 52.20(14) 4_656 4_656 ? O60 Dy2 O51 120.81(18) . 4_656 ? O88 Dy2 O42 78.19(19) 2_755 1_565 ? O100 Dy2 O42 125.9(2) . 1_565 ? O41 Dy2 O42 49.78(17) 1_565 1_565 ? O101 Dy2 O42 68.7(2) . 1_565 ? O59 Dy2 O42 141.6(2) . 1_565 ? O50 Dy2 O42 65.96(13) 4_656 1_565 ? O60 Dy2 O42 138.46(19) . 1_565 ? O51 Dy2 O42 98.26(13) 4_656 1_565 ? O88 Dy2 C58 101.7(2) 2_755 . ? O100 Dy2 C58 84.1(3) . . ? O41 Dy2 C58 160.8(3) 1_565 . ? O101 Dy2 C58 80.5(3) . . ? O59 Dy2 C58 26.5(2) . . ? O50 Dy2 C58 103.3(2) 4_656 . ? O60 Dy2 C58 27.3(2) . . ? O51 Dy2 C58 96.1(2) 4_656 . ? O42 Dy2 C58 149.3(3) 1_565 . ? O88 Dy2 C49 160.72(19) 2_755 4_656 ? O100 Dy2 C49 100.5(2) . 4_656 ? O41 Dy2 C49 85.19(17) 1_565 4_656 ? O101 Dy2 C49 94.3(2) . 4_656 ? O59 Dy2 C49 71.05(18) . 4_656 ? O50 Dy2 C49 27.05(17) 4_656 4_656 ? O60 Dy2 C49 124.84(18) . 4_656 ? O51 Dy2 C49 25.51(16) 4_656 4_656 ? O42 Dy2 C49 84.52(16) 1_565 4_656 ? C58 Dy2 C49 97.5(2) . 4_656 ? O88 Dy2 C40 73.70(19) 2_755 1_565 ? O100 Dy2 C40 100.3(3) . 1_565 ? O41 Dy2 C40 24.41(19) 1_565 1_565 ? O101 Dy2 C40 93.9(3) . 1_565 ? O59 Dy2 C40 157.63(19) . 1_565 ? O50 Dy2 C40 78.45(17) 4_656 1_565 ? O60 Dy2 C40 147.61(19) . 1_565 ? O51 Dy2 C40 90.24(17) 4_656 1_565 ? O42 Dy2 C40 25.64(18) 1_565 1_565 ? C58 Dy2 C40 173.0(3) . 1_565 ? C49 Dy2 C40 87.02(18) 4_656 1_565 ? N21 C1 C20 123.9(6) . . ? N21 C1 C2 111.1(6) . . ? C20 C1 C2 124.6(6) . . ? C3 C2 C1 106.6(6) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C2 C3 C4 106.8(6) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? N21 C4 C5 124.6(6) . . ? N21 C4 C3 110.8(6) . . ? C5 C4 C3 124.1(6) . . ? C6 C5 C4 120.8(6) . . ? C6 C5 C25 120.3(6) . . ? C4 C5 C25 118.9(6) . . ? N22 C6 C5 125.4(6) . . ? N22 C6 C7 111.3(6) . . ? C5 C6 C7 122.5(6) . . ? C8 C7 C6 107.3(6) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.3(6) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? C10 C9 N22 123.8(6) . . ? C10 C9 C8 125.4(6) . . ? N22 C9 C8 110.5(6) . . ? C11 C10 C9 123.5(6) . . ? C11 C10 C34 117.6(6) . . ? C9 C10 C34 119.0(6) . . ? N23 C11 C10 125.2(6) . . ? N23 C11 C12 111.3(6) . . ? C10 C11 C12 123.4(6) . . ? C13 C12 C11 105.5(6) . . ? C13 C12 H12 127.3 . . ? C11 C12 H12 127.3 . . ? C12 C13 C14 108.6(6) . . ? C12 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? N23 C14 C15 124.7(6) . . ? N23 C14 C13 109.9(6) . . ? C15 C14 C13 124.8(6) . . ? C14 C15 C16 121.7(6) . . ? C14 C15 C43 117.6(6) . . ? C16 C15 C43 120.6(6) . . ? N24 C16 C15 124.1(6) . . ? N24 C16 C17 111.0(6) . . ? C15 C16 C17 124.5(6) . . ? C18 C17 C16 107.6(6) . . ? C18 C17 H17 126.2 . . ? C16 C17 H17 126.2 . . ? C17 C18 C19 106.2(6) . . ? C17 C18 H18 126.9 . . ? C19 C18 H18 126.9 . . ? C20 C19 N24 123.8(6) . . ? C20 C19 C18 126.2(6) . . ? N24 C19 C18 109.7(6) . . ? C19 C20 C1 123.9(6) . . ? C19 C20 C52 117.0(6) . . ? C1 C20 C52 119.1(6) . . ? C4 N21 C1 104.3(5) . . ? C4 N21 Cu1 128.5(4) . . ? C1 N21 Cu1 127.0(4) . . ? C6 N22 C9 104.5(5) . . ? C6 N22 Cu1 128.2(4) . . ? C9 N22 Cu1 127.0(4) . . ? C11 N23 C14 104.6(5) . . ? C11 N23 Cu1 127.7(4) . . ? C14 N23 Cu1 127.5(4) . . ? C16 N24 C19 104.8(5) . . ? C16 N24 Cu1 128.6(4) . . ? C19 N24 Cu1 126.3(4) . . ? C26 C25 C30 119.8(6) . . ? C26 C25 C5 121.6(6) . . ? C30 C25 C5 118.6(7) . . ? C25 C26 C27 120.7(6) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 120.2(6) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 118.5(6) . . ? C29 C28 C31 121.3(6) . . ? C27 C28 C31 120.3(6) . . ? C30 C29 C28 121.1(7) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C25 119.6(7) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? O32 C31 O33 122.3(6) . . ? O32 C31 C28 118.7(6) . . ? O33 C31 C28 119.0(7) . . ? C31 O32 Dy1 114.3(4) . . ? C31 O33 Dy1 176.1(4) . 2_755 ? C39 C34 C35 119.7(6) . . ? C39 C34 C10 121.1(6) . . ? C35 C34 C10 118.6(7) . . ? C36 C35 C34 118.4(7) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C37 C36 C35 121.0(7) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C36 117.9(7) . . ? C38 C37 C40 121.5(7) . . ? C36 C37 C40 120.6(7) . . ? C37 C38 C39 123.0(7) . . ? C37 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C34 C39 C38 119.9(7) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? O41 C40 O42 121.7(7) . . ? O41 C40 C37 119.5(7) . . ? O42 C40 C37 118.8(8) . . ? O41 C40 Dy2 52.7(4) . 1_545 ? O42 C40 Dy2 70.1(4) . 1_545 ? C37 C40 Dy2 167.2(5) . 1_545 ? C40 O41 Dy2 102.9(4) . 1_545 ? C40 O42 Dy1 134.3(4) . 6_556 ? C40 O42 Dy2 84.3(4) . 1_545 ? Dy1 O42 Dy2 102.42(16) 6_556 1_545 ? C48 C43 C44 118.7(6) . . ? C48 C43 C15 122.1(6) . . ? C44 C43 C15 119.2(6) . . ? C45 C44 C43 120.0(7) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 122.1(6) . . ? C46 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? C45 C46 C47 118.1(6) . . ? C45 C46 C49 122.0(6) . . ? C47 C46 C49 119.9(6) . . ? C48 C47 C46 120.2(7) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C43 C48 C47 120.8(7) . . ? C43 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? O51 C49 O50 119.7(6) . . ? O51 C49 C46 123.3(6) . . ? O50 C49 C46 116.9(6) . . ? O51 C49 Dy2 62.4(4) . 4_646 ? O50 C49 Dy2 58.6(3) . 4_646 ? C46 C49 Dy2 167.8(5) . 4_646 ? C49 O50 Dy1 140.9(4) . 7_656 ? C49 O50 Dy2 94.4(4) . 4_646 ? Dy1 O50 Dy2 111.32(16) 7_656 4_646 ? C49 O51 Dy2 92.1(4) . 4_646 ? C53 C52 C57 118.4(7) . . ? C53 C52 C20 120.9(6) . . ? C57 C52 C20 120.7(6) . . ? C52 C53 C54 119.7(7) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C55 C54 C53 120.1(8) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 120.9(7) . . ? C54 C55 C58 120.1(8) . . ? C56 C55 C58 119.0(8) . . ? C57 C56 C55 118.7(8) . . ? C57 C56 H56 120.6 . . ? C55 C56 H56 120.6 . . ? C56 C57 C52 122.1(7) . . ? C56 C57 H57 118.9 . . ? C52 C57 H57 118.9 . . ? O59 C58 O60 120.9(7) . . ? O59 C58 C55 120.3(8) . . ? O60 C58 C55 118.8(8) . . ? O59 C58 Dy2 58.8(4) . . ? O60 C58 Dy2 62.1(4) . . ? C55 C58 Dy2 179.1(7) . . ? C58 O59 Dy2 94.7(5) . . ? C58 O60 Dy2 90.6(5) . . ? N21 Cu1 N23 170.6(2) . . ? N21 Cu1 N22 89.5(2) . . ? N23 Cu1 N22 91.0(2) . . ? N21 Cu1 N24 91.4(2) . . ? N23 Cu1 N24 89.8(2) . . ? N22 Cu1 N24 170.1(2) . . ? C62 C61 C62 122.8(9) 2_755 . ? C62 C61 C74 118.6(5) 2_755 . ? C62 C61 C74 118.6(5) . . ? C61 C62 N72 125.1(7) . . ? C61 C62 C63 124.4(6) . . ? N72 C62 C63 110.0(6) . . ? C64 C63 C62 106.9(6) . . ? C64 C63 H63 126.5 . . ? C62 C63 H63 126.5 . . ? C63 C64 C65 107.9(7) . . ? C63 C64 H64 126.1 . . ? C65 C64 H64 126.1 . . ? N72 C65 C66 125.9(6) . . ? N72 C65 C64 110.4(6) . . ? C66 C65 C64 123.4(7) . . ? C67 C66 C65 122.3(7) . . ? C67 C66 C80 118.1(6) . . ? C65 C66 C80 119.6(6) . . ? N73 C67 C66 126.1(6) . . ? N73 C67 C68 110.8(6) . . ? C66 C67 C68 123.1(7) . . ? C69 C68 C67 107.2(7) . . ? C69 C68 H68 126.4 . . ? C67 C68 H68 126.4 . . ? C68 C69 C70 106.7(6) . . ? C68 C69 H69 126.7 . . ? C70 C69 H69 126.7 . . ? N73 C70 C71 126.6(6) . . ? N73 C70 C69 110.9(6) . . ? C71 C70 C69 122.3(6) . . ? C70 C71 C70 120.9(8) 2_755 . ? C70 C71 C89 119.6(4) 2_755 . ? C70 C71 C89 119.5(4) . . ? C65 N72 C62 104.7(5) . . ? C65 N72 Cu2 127.1(4) . . ? C62 N72 Cu2 128.2(4) . . ? C67 N73 C70 104.4(5) . . ? C67 N73 Cu2 128.0(4) . . ? C70 N73 Cu2 127.6(5) . . ? C75 C74 C75 116.0(9) . 2_755 ? C75 C74 C61 122.0(4) . . ? C75 C74 C61 122.0(4) 2_755 . ? C76 C75 C74 122.1(7) . . ? C76 C75 H75 118.9 . . ? C74 C75 H75 118.9 . . ? C75 C76 C77 123.0(7) . . ? C75 C76 H76 118.5 . . ? C77 C76 H76 118.5 . . ? C76 C77 C76 113.7(7) 2_755 . ? C76 C77 C78 123.1(4) 2_755 . ? C76 C77 C78 123.1(4) . . ? O79 C78 O79 120.1(6) . 2_755 ? O79 C78 C77 119.9(3) . . ? O79 C78 C77 119.9(3) 2_755 . ? C78 O79 Dy1 143.5(4) . 2_765 ? C85 C80 C81 116.6(7) . . ? C85 C80 C66 122.1(7) . . ? C81 C80 C66 121.1(7) . . ? C80 C81 C82 118.6(9) . . ? C80 C81 H81 120.7 . . ? C82 C81 H81 120.7 . . ? C83 C82 C81 124.7(8) . . ? C83 C82 H82 117.6 . . ? C81 C82 H82 117.6 . . ? C84 C83 C82 112.9(7) . . ? C84 C83 C86 124.2(10) . . ? C82 C83 C86 122.8(10) . . ? C83 C84 C85 124.6(9) . . ? C83 C84 H84 117.7 . . ? C85 C84 H84 117.7 . . ? C80 C85 C84 122.4(8) . . ? C80 C85 H85 118.8 . . ? C84 C85 H85 118.8 . . ? O88 C86 O87 119.1(8) . . ? O88 C86 C83 122.7(11) . . ? O87 C86 C83 118.1(11) . . ? C86 O88 Dy2 130.3(7) . 2_755 ? C90 C89 C90 118.4(9) 2_755 . ? C90 C89 C71 120.8(4) 2_755 . ? C90 C89 C71 120.8(4) . . ? C89 C90 C91 121.6(7) . . ? C89 C90 H90 119.2 . . ? C91 C90 H90 119.2 . . ? C90 C91 C92 120.1(7) . . ? C90 C91 H91 120.0 . . ? C92 C91 H91 120.0 . . ? C91 C92 C91 118.3(9) 2_755 . ? C91 C92 C93 120.8(4) 2_755 . ? C91 C92 C93 120.8(4) . . ? O94 C93 O94 123.5(9) 2_755 . ? O94 C93 C92 118.2(4) 2_755 . ? O94 C93 C92 118.2(4) . . ? C93 O94 Dy1 141.7(5) . . ? N73 Cu2 N73 90.5(3) 2_755 . ? N73 Cu2 N72 90.0(2) 2_755 2_755 ? N73 Cu2 N72 176.3(2) . 2_755 ? N73 Cu2 N72 176.3(2) 2_755 . ? N73 Cu2 N72 90.0(2) . . ? N72 Cu2 N72 89.7(3) 2_755 . ? C96 O95 Dy1 132.0(5) . . ? O95 C96 N97 127.1(9) . . ? O95 C96 H96 116.5 . . ? N97 C96 H96 116.5 . . ? C96 N97 C98 123.1(8) . . ? C96 N97 C99 121.0(8) . . ? C98 N97 C99 115.8(7) . . ? N97 C98 H98A 109.5 . . ? N97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? N97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N97 C99 H99A 109.5 . . ? N97 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N97 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? Dy2 O100 HOA 109.2 . . ? Dy2 O100 HOB 109.3 . . ? HOA O100 HOB 109.5 . . ? Dy2 O101 H10A 109.2 . . ? Dy2 O101 H10B 109.0 . . ? H10A O101 H10B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.726 _refine_diff_density_min -1.332 _refine_diff_density_rms 0.171 #===========================END======================= data_Compound-8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H45 Cu0.26 Eu2 N7 O15' _chemical_formula_sum 'C75 H45 Cu0.26 Eu2 N7 O15' _chemical_formula_weight 1604.62 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5909(3) _cell_length_b 24.0263(4) _cell_length_c 31.1146(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.7945(8) _cell_angle_gamma 90.00 _cell_volume 15531.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 14712 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 27.28 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6380 _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6243 _exptl_absorpt_correction_T_max 0.8457 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52947 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.87 _reflns_number_total 18311 _reflns_number_gt 12582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^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 18311 _refine_ls_number_parameters 907 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.913776(10) 0.229188(8) 0.198660(6) 0.02304(6) Uani 1 1 d . . . Eu2 Eu 0.824788(11) 0.309566(8) 0.087268(6) 0.02735(7) Uani 1 1 d . . . C1 C 0.8243(2) 0.30742(16) 0.53066(13) 0.0281(9) Uani 1 1 d . . . C2 C 0.8167(2) 0.33557(17) 0.48909(14) 0.0341(10) Uani 1 1 d . . . H2 H 0.8077 0.3740 0.4835 0.041 Uiso 1 1 calc R . . C3 C 0.8247(2) 0.29720(17) 0.45935(14) 0.0341(10) Uani 1 1 d . . . H3 H 0.8232 0.3037 0.4290 0.041 Uiso 1 1 calc R . . C4 C 0.8359(2) 0.24463(16) 0.48235(13) 0.0263(9) Uani 1 1 d . . . C5 C 0.8540(2) 0.19467(16) 0.46511(13) 0.0273(9) Uani 1 1 d . . . C6 C 0.8605(2) 0.14305(17) 0.48629(13) 0.0297(9) Uani 1 1 d . . . C7 C 0.8764(2) 0.09158(18) 0.46904(14) 0.0379(11) Uani 1 1 d . . . H7 H 0.8888 0.0868 0.4422 0.046 Uiso 1 1 calc R . . C8 C 0.8707(3) 0.05100(18) 0.49745(14) 0.0433(12) Uani 1 1 d . . . H8 H 0.8784 0.0125 0.4944 0.052 Uiso 1 1 calc R . . C9 C 0.8510(2) 0.07676(17) 0.53335(14) 0.0341(10) Uani 1 1 d . . . C10 C 0.8357(2) 0.04920(16) 0.56858(13) 0.0310(10) Uani 1 1 d . . . C11 C 0.8174(2) 0.07494(15) 0.60352(13) 0.0270(9) Uani 1 1 d . . . C12 C 0.7980(2) 0.04562(18) 0.63812(13) 0.0304(9) Uani 1 1 d . . . H12 H 0.7926 0.0065 0.6400 0.037 Uiso 1 1 calc R . . C13 C 0.7889(2) 0.08416(16) 0.66740(13) 0.0302(9) Uani 1 1 d . . . H13 H 0.7757 0.0773 0.6937 0.036 Uiso 1 1 calc R . . C14 C 0.80293(19) 0.13783(16) 0.65126(12) 0.0263(9) Uani 1 1 d . . . C15 C 0.80862(19) 0.18802(16) 0.67522(13) 0.0266(9) Uani 1 1 d . . . C16 C 0.82617(19) 0.23876(16) 0.65964(13) 0.0257(9) Uani 1 1 d . . . C17 C 0.8390(2) 0.28915(17) 0.68435(14) 0.0326(10) Uani 1 1 d . . . H17 H 0.8411 0.2936 0.7151 0.039 Uiso 1 1 calc R . . C18 C 0.8477(2) 0.32974(18) 0.65630(14) 0.0332(10) Uani 1 1 d . . . H18 H 0.8585 0.3675 0.6638 0.040 Uiso 1 1 calc R . . C19 C 0.8376(2) 0.30486(16) 0.61312(14) 0.0285(9) Uani 1 1 d . . . C20 C 0.8308(2) 0.33331(16) 0.57280(14) 0.0286(9) Uani 1 1 d . . . N21 N 0.83239(16) 0.25076(13) 0.52513(11) 0.0264(8) Uani 1 1 d . . . N22 N 0.84687(17) 0.13319(13) 0.52627(11) 0.0302(8) Uani 1 1 d . . . N23 N 0.81866(16) 0.13067(13) 0.61138(10) 0.0270(8) Uani 1 1 d . . . N24 N 0.82911(16) 0.24850(13) 0.61722(11) 0.0273(8) Uani 1 1 d . . . C25 C 0.8711(2) 0.19846(16) 0.42151(12) 0.0257(9) Uani 1 1 d . . . C26 C 0.8235(2) 0.20171(16) 0.38138(13) 0.0297(9) Uani 1 1 d . . . H26 H 0.7794 0.1993 0.3810 0.036 Uiso 1 1 calc R . . C27 C 0.8404(2) 0.20847(17) 0.34187(13) 0.0307(9) Uani 1 1 d . . . H27 H 0.8077 0.2112 0.3145 0.037 Uiso 1 1 calc R . . C28 C 0.9044(2) 0.21134(15) 0.34179(12) 0.0238(8) Uani 1 1 d . . . C29 C 0.9514(2) 0.2053(2) 0.38118(14) 0.0395(11) Uani 1 1 d . . . H29 H 0.9954 0.2054 0.3814 0.047 Uiso 1 1 calc R . . C30 C 0.9340(2) 0.1991(2) 0.42118(14) 0.0462(13) Uani 1 1 d . . . H30 H 0.9667 0.1953 0.4485 0.055 Uiso 1 1 calc R . . C31 C 0.9216(2) 0.22126(15) 0.29960(13) 0.0270(9) Uani 1 1 d . . . O32 O 0.87734(15) 0.22344(11) 0.26352(9) 0.0319(7) Uani 1 1 d . . . O33 O 0.98061(15) 0.22695(11) 0.30058(9) 0.0327(7) Uani 1 1 d . . . C34 C 0.8385(2) -0.01303(16) 0.57052(13) 0.0319(10) Uani 1 1 d . . . C35 C 0.8932(2) -0.03965(17) 0.59662(15) 0.0396(11) Uani 1 1 d . . . H35 H 0.9312 -0.0189 0.6093 0.048 Uiso 1 1 calc R . . C36 C 0.8920(2) -0.09618(16) 0.60401(14) 0.0340(10) Uani 1 1 d . . . H36 H 0.9290 -0.1139 0.6226 0.041 Uiso 1 1 calc R . . C37 C 0.8376(2) -0.12744(17) 0.58469(12) 0.0285(10) Uani 1 1 d . . . C38 C 0.7835(2) -0.10111(16) 0.55687(13) 0.0336(10) Uani 1 1 d . . . H38 H 0.7464 -0.1223 0.5428 0.040 Uiso 1 1 calc R . . C39 C 0.7842(2) -0.04469(17) 0.54988(13) 0.0373(11) Uani 1 1 d . . . H39 H 0.7474 -0.0270 0.5309 0.045 Uiso 1 1 calc R . . C40 C 0.8347(2) -0.18791(17) 0.59256(13) 0.0319(10) Uani 1 1 d . . . O41 O 0.78593(16) -0.21484(12) 0.57285(10) 0.0379(7) Uani 1 1 d . . . O42 O 0.88297(15) -0.21147(11) 0.61986(9) 0.0320(7) Uani 1 1 d . . . C43 C 0.7897(2) 0.18675(15) 0.71798(13) 0.0256(9) Uani 1 1 d . . . C44 C 0.7263(2) 0.17523(16) 0.71755(13) 0.0264(9) Uani 1 1 d . . . H44 H 0.6959 0.1661 0.6901 0.032 Uiso 1 1 calc R . . C45 C 0.7069(2) 0.17694(16) 0.75646(12) 0.0256(9) Uani 1 1 d . . . H45 H 0.6635 0.1692 0.7557 0.031 Uiso 1 1 calc R . . C46 C 0.7512(2) 0.19002(16) 0.79656(12) 0.0258(9) Uani 1 1 d . . . C47 C 0.8150(2) 0.19834(18) 0.79797(14) 0.0324(10) Uani 1 1 d . . . H47 H 0.8457 0.2048 0.8258 0.039 Uiso 1 1 calc R . . C48 C 0.8351(2) 0.19726(17) 0.75854(14) 0.0336(10) Uani 1 1 d . . . H48 H 0.8789 0.2036 0.7596 0.040 Uiso 1 1 calc R . . C49 C 0.7295(2) 0.19682(15) 0.83813(13) 0.0247(9) Uani 1 1 d . . . O50 O 0.66933(13) 0.20530(10) 0.83369(8) 0.0229(6) Uani 1 1 d . . . O51 O 0.76844(14) 0.19433(11) 0.87614(9) 0.0301(6) Uani 1 1 d . . . C52 C 0.8310(2) 0.39537(17) 0.57436(14) 0.0334(10) Uani 1 1 d . . . C53 C 0.8768(2) 0.42612(18) 0.55984(15) 0.0413(11) Uani 1 1 d . . . H53 H 0.9075 0.4073 0.5483 0.050 Uiso 1 1 calc R . . C54 C 0.8776(3) 0.48342(19) 0.56227(17) 0.0515(14) Uani 1 1 d . . . H54 H 0.9086 0.5040 0.5523 0.062 Uiso 1 1 calc R . . C55 C 0.8326(3) 0.51134(19) 0.57935(16) 0.0472(13) Uani 1 1 d . . . C56 C 0.7872(3) 0.48084(18) 0.59355(18) 0.0511(14) Uani 1 1 d . . . H56 H 0.7565 0.4995 0.6051 0.061 Uiso 1 1 calc R . . C57 C 0.7866(2) 0.42312(17) 0.59086(16) 0.0417(12) Uani 1 1 d . . . H57 H 0.7552 0.4026 0.6005 0.050 Uiso 1 1 calc R . . C58 C 0.8319(3) 0.57345(19) 0.58190(18) 0.0566(16) Uani 1 1 d . . . O59 O 0.8067(2) 0.59678(13) 0.60965(13) 0.0727(13) Uani 1 1 d . . . O60 O 0.8555(2) 0.60282(13) 0.55580(13) 0.0722(13) Uani 1 1 d . . . Cu1 Cu 0.8317(2) 0.19023(16) 0.56940(14) 0.0374(10) Uani 0.13 1 d P . . C61 C 1.0000 0.8733(2) 0.2500 0.0264(13) Uani 1 2 d S . . C62 C 1.00199(19) 0.84578(15) 0.21024(13) 0.0253(9) Uani 1 1 d . . . C63 C 1.0081(2) 0.87259(17) 0.17059(15) 0.0362(11) Uani 1 1 d . . . H63 H 1.0075 0.9116 0.1654 0.043 Uiso 1 1 calc R . . C64 C 1.0150(2) 0.83232(17) 0.14176(14) 0.0341(10) Uani 1 1 d . . . H64 H 1.0205 0.8379 0.1128 0.041 Uiso 1 1 calc R . . C65 C 1.0125(2) 0.77982(16) 0.16287(13) 0.0280(9) Uani 1 1 d . . . C66 C 1.02096(19) 0.72818(16) 0.14455(13) 0.0266(9) Uani 1 1 d . . . C67 C 1.0165(2) 0.67601(16) 0.16418(12) 0.0259(9) Uani 1 1 d . . . C68 C 1.0195(2) 0.62308(16) 0.14278(13) 0.0293(9) Uani 1 1 d . . . H68 H 1.0251 0.6173 0.1139 0.035 Uiso 1 1 calc R . . C69 C 1.0126(2) 0.58314(16) 0.17208(13) 0.0317(10) Uani 1 1 d . . . H69 H 1.0121 0.5441 0.1671 0.038 Uiso 1 1 calc R . . C70 C 1.00614(19) 0.60993(15) 0.21147(13) 0.0255(9) Uani 1 1 d . . . C71 C 1.0000 0.5834(2) 0.2500 0.0261(12) Uani 1 2 d S . . N72 N 1.00355(16) 0.78881(13) 0.20461(11) 0.0251(7) Uani 1 1 d . . . N73 N 1.00862(15) 0.66706(13) 0.20602(10) 0.0239(7) Uani 1 1 d . . . C74 C 1.0000 0.9350(2) 0.2500 0.0260(12) Uani 1 2 d S . . C75 C 0.9497(2) 0.96544(17) 0.22201(15) 0.0347(10) Uani 1 1 d . . . H75 H 0.9147 0.9462 0.2026 0.042 Uiso 1 1 calc R . . C76 C 0.9500(2) 1.02291(16) 0.22198(14) 0.0330(10) Uani 1 1 d . . . H76 H 0.9154 1.0425 0.2024 0.040 Uiso 1 1 calc R . . C77 C 1.0000 1.0522(2) 0.2500 0.0284(13) Uani 1 2 d S . . C78 C 1.0000 1.1153(2) 0.2500 0.0308(13) Uani 1 2 d S . . O79 O 1.04841(14) 1.13924(11) 0.27498(9) 0.0334(7) Uani 1 1 d . . . C80 C 1.0366(2) 0.72670(15) 0.10056(13) 0.0275(9) Uani 1 1 d . . . C81 C 1.0988(2) 0.7236(2) 0.09793(17) 0.0495(13) Uani 1 1 d . . . H81 H 1.1326 0.7249 0.1249 0.059 Uiso 1 1 calc R . . C82 C 1.1145(3) 0.7189(2) 0.05848(19) 0.0523(15) Uani 1 1 d . . . H82 H 1.1583 0.7171 0.0581 0.063 Uiso 1 1 calc R . . C83 C 1.0660(3) 0.7167(2) 0.01915(17) 0.0495(14) Uani 1 1 d . . . C84 C 1.0044(3) 0.7197(3) 0.02129(17) 0.088(2) Uani 1 1 d . . . H84 H 0.9704 0.7176 -0.0055 0.106 Uiso 1 1 calc R . . C85 C 0.9902(3) 0.7257(3) 0.06140(17) 0.077(2) Uani 1 1 d . . . H85 H 0.9465 0.7293 0.0616 0.093 Uiso 1 1 calc R . . C86 C 1.0796(4) 0.7103(2) -0.0271(2) 0.073(2) Uani 1 1 d . . . O87 O 1.0334(3) 0.6959(3) -0.05900(16) 0.149(3) Uani 1 1 d . . . O88 O 1.1329(3) 0.71874(14) -0.02955(15) 0.0798(16) Uani 1 1 d . . . C89 C 1.0000 0.5211(2) 0.2500 0.0252(12) Uani 1 2 d S . . C90 C 0.9472(2) 0.49174(16) 0.22455(13) 0.0305(9) Uani 1 1 d . . . H90 H 0.9109 0.5114 0.2070 0.037 Uiso 1 1 calc R . . C91 C 0.9472(2) 0.43344(16) 0.22463(14) 0.0301(9) Uani 1 1 d . . . H91 H 0.9108 0.4138 0.2072 0.036 Uiso 1 1 calc R . . C92 C 1.0000 0.4042(2) 0.2500 0.0220(12) Uani 1 2 d S . . C93 C 1.0000 0.3421(2) 0.2500 0.0234(12) Uani 1 2 d S . . O94 O 0.95009(14) 0.31737(11) 0.22745(9) 0.0300(6) Uiso 1 1 d . . . Cu2 Cu 0.5000 0.2268(3) 0.2500 0.141(3) Uani 0.26 2 d SP . . O95 O 0.81429(14) 0.17436(11) 0.18012(9) 0.0296(6) Uani 1 1 d . . . C96 C 0.7777(3) 0.1604(2) 0.20284(16) 0.0568(15) Uani 1 1 d . . . H96 H 0.7885 0.1728 0.2330 0.068 Uiso 1 1 calc R . . N97 N 0.7260(2) 0.13061(18) 0.18934(14) 0.0576(12) Uani 1 1 d . . . C98 C 0.7057(3) 0.1092(3) 0.14534(18) 0.0739(19) Uani 1 1 d . . . H98A H 0.7191 0.1345 0.1249 0.111 Uiso 1 1 calc R . . H98B H 0.6587 0.1057 0.1363 0.111 Uiso 1 1 calc R . . H98C H 0.7252 0.0725 0.1444 0.111 Uiso 1 1 calc R . . C99 C 0.6836(3) 0.1184(3) 0.2187(2) 0.088(2) Uani 1 1 d . . . H99A H 0.6775 0.0780 0.2199 0.132 Uiso 1 1 calc R . . H99B H 0.6418 0.1364 0.2065 0.132 Uiso 1 1 calc R . . H99C H 0.7036 0.1325 0.2488 0.132 Uiso 1 1 calc R . . O100A O 0.7310(3) 0.3372(4) 0.0361(3) 0.040(3) Uiso 0.438(13) 1 d P . . O100B O 0.7292(3) 0.3051(3) 0.0221(2) 0.047(2) Uiso 0.562(13) 1 d P . . O101 O 0.93397(19) 0.3212(2) 0.13332(12) 0.0948(17) Uani 1 1 d . . . H10A H 0.9424 0.3585 0.1473 0.114 Uiso 1 1 calc R . . H10B H 0.9669 0.3115 0.1178 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02717(12) 0.02001(11) 0.02018(11) -0.00373(8) 0.00344(8) 0.00229(8) Eu2 0.04282(14) 0.02044(12) 0.01760(11) 0.00127(8) 0.00622(9) 0.00152(9) C1 0.028(2) 0.025(2) 0.036(2) 0.0017(18) 0.0167(18) 0.0001(17) C2 0.046(3) 0.024(2) 0.037(2) 0.005(2) 0.022(2) 0.0049(19) C3 0.046(3) 0.032(2) 0.028(2) 0.003(2) 0.018(2) 0.002(2) C4 0.031(2) 0.026(2) 0.027(2) 0.0023(18) 0.0166(18) 0.0017(17) C5 0.037(3) 0.028(2) 0.022(2) 0.0021(17) 0.0171(18) 0.0028(18) C6 0.038(3) 0.029(2) 0.027(2) 0.0012(18) 0.0180(18) 0.0056(19) C7 0.060(3) 0.035(2) 0.027(2) 0.003(2) 0.025(2) 0.010(2) C8 0.073(4) 0.028(2) 0.036(3) 0.000(2) 0.028(2) 0.016(2) C9 0.054(3) 0.025(2) 0.031(2) -0.0027(19) 0.024(2) 0.007(2) C10 0.046(3) 0.021(2) 0.027(2) 0.0029(18) 0.0122(19) 0.0036(19) C11 0.041(3) 0.017(2) 0.024(2) 0.0012(17) 0.0114(18) 0.0046(17) C12 0.037(3) 0.030(2) 0.026(2) 0.0054(18) 0.0109(18) 0.0009(19) C13 0.039(3) 0.030(2) 0.026(2) 0.0044(18) 0.0155(19) -0.0010(19) C14 0.029(2) 0.029(2) 0.024(2) -0.0007(17) 0.0119(17) 0.0018(17) C15 0.025(2) 0.030(2) 0.027(2) 0.0004(18) 0.0111(17) 0.0019(17) C16 0.025(2) 0.030(2) 0.028(2) -0.0083(18) 0.0153(17) -0.0033(17) C17 0.034(3) 0.033(2) 0.034(2) -0.006(2) 0.0155(19) -0.0052(19) C18 0.031(3) 0.035(2) 0.037(2) -0.011(2) 0.0145(19) -0.0026(19) C19 0.027(2) 0.025(2) 0.037(2) -0.0103(19) 0.0159(18) -0.0030(17) C20 0.032(2) 0.025(2) 0.035(2) -0.0010(19) 0.0178(18) 0.0007(17) N21 0.031(2) 0.0202(17) 0.0340(19) -0.0047(15) 0.0195(16) 0.0002(14) N22 0.041(2) 0.0273(19) 0.0285(19) 0.0066(15) 0.0194(16) 0.0020(16) N23 0.034(2) 0.0250(18) 0.0258(18) -0.0001(14) 0.0141(15) 0.0030(15) N24 0.032(2) 0.0253(18) 0.0298(18) 0.0012(15) 0.0171(15) 0.0000(14) C25 0.034(2) 0.025(2) 0.022(2) 0.0014(17) 0.0133(17) 0.0038(17) C26 0.028(2) 0.033(2) 0.034(2) 0.0091(19) 0.0182(19) -0.0001(18) C27 0.030(2) 0.034(2) 0.027(2) 0.0042(19) 0.0070(18) -0.0035(19) C28 0.034(2) 0.0193(19) 0.021(2) 0.0019(16) 0.0119(17) 0.0017(16) C29 0.024(2) 0.067(3) 0.029(2) 0.009(2) 0.0100(18) 0.009(2) C30 0.039(3) 0.084(4) 0.020(2) 0.003(2) 0.0137(19) 0.010(3) C31 0.041(3) 0.016(2) 0.029(2) -0.0040(17) 0.019(2) -0.0012(17) O32 0.0444(19) 0.0311(16) 0.0192(15) 0.0026(12) 0.0069(13) -0.0043(13) O33 0.0426(19) 0.0315(16) 0.0327(16) -0.0036(13) 0.0250(14) -0.0054(13) C34 0.052(3) 0.023(2) 0.024(2) 0.0007(18) 0.016(2) 0.003(2) C35 0.043(3) 0.029(2) 0.047(3) -0.001(2) 0.013(2) -0.001(2) C36 0.041(3) 0.026(2) 0.033(2) 0.0067(19) 0.008(2) 0.008(2) C37 0.044(3) 0.030(2) 0.0150(19) -0.0010(17) 0.0138(18) 0.0096(19) C38 0.046(3) 0.025(2) 0.029(2) -0.0035(19) 0.009(2) -0.003(2) C39 0.051(3) 0.033(2) 0.025(2) 0.000(2) 0.005(2) 0.009(2) C40 0.052(3) 0.026(2) 0.025(2) 0.0007(19) 0.023(2) 0.006(2) O41 0.053(2) 0.0228(15) 0.0374(17) -0.0004(13) 0.0123(15) -0.0010(15) O42 0.048(2) 0.0250(15) 0.0299(15) 0.0034(13) 0.0228(14) 0.0066(14) C43 0.033(2) 0.023(2) 0.024(2) -0.0029(17) 0.0125(17) 0.0031(17) C44 0.031(2) 0.024(2) 0.025(2) -0.0011(17) 0.0081(17) 0.0022(17) C45 0.028(2) 0.027(2) 0.024(2) -0.0008(17) 0.0105(17) 0.0011(17) C46 0.031(2) 0.027(2) 0.020(2) -0.0013(17) 0.0087(17) 0.0052(17) C47 0.028(2) 0.045(3) 0.025(2) -0.0039(19) 0.0079(17) 0.0042(19) C48 0.027(2) 0.043(3) 0.033(2) -0.004(2) 0.0116(18) 0.0029(19) C49 0.036(3) 0.017(2) 0.023(2) 0.0006(16) 0.0100(18) 0.0021(17) O50 0.0265(16) 0.0229(13) 0.0212(14) -0.0006(11) 0.0099(11) 0.0008(11) O51 0.0333(17) 0.0366(17) 0.0209(14) 0.0018(12) 0.0080(12) 0.0037(13) C52 0.042(3) 0.027(2) 0.038(2) -0.0009(19) 0.023(2) -0.0040(19) C53 0.050(3) 0.032(2) 0.050(3) -0.010(2) 0.028(2) -0.008(2) C54 0.074(4) 0.031(3) 0.065(3) -0.003(2) 0.045(3) -0.014(2) C55 0.073(4) 0.026(2) 0.055(3) -0.002(2) 0.039(3) -0.004(2) C56 0.070(4) 0.025(2) 0.072(4) -0.004(2) 0.043(3) 0.005(2) C57 0.045(3) 0.028(2) 0.061(3) -0.001(2) 0.032(3) -0.006(2) C58 0.098(5) 0.018(2) 0.072(4) -0.009(2) 0.055(4) -0.009(3) O59 0.136(4) 0.0218(17) 0.090(3) -0.0076(18) 0.083(3) -0.006(2) O60 0.131(4) 0.0258(18) 0.088(3) 0.0012(19) 0.079(3) -0.008(2) Cu1 0.047(3) 0.031(2) 0.038(2) 0.0014(19) 0.018(2) -0.0010(19) C61 0.023(3) 0.014(3) 0.041(3) 0.000 0.008(3) 0.000 C62 0.027(2) 0.019(2) 0.030(2) 0.0030(17) 0.0078(17) -0.0001(16) C63 0.044(3) 0.021(2) 0.045(3) 0.007(2) 0.015(2) 0.0031(19) C64 0.049(3) 0.028(2) 0.030(2) 0.0071(19) 0.019(2) 0.001(2) C65 0.031(2) 0.023(2) 0.031(2) 0.0026(18) 0.0112(18) 0.0021(17) C66 0.027(2) 0.030(2) 0.026(2) 0.0040(18) 0.0130(17) 0.0011(17) C67 0.033(2) 0.026(2) 0.023(2) 0.0011(17) 0.0153(17) 0.0000(17) C68 0.038(3) 0.026(2) 0.027(2) -0.0047(18) 0.0146(18) -0.0040(18) C69 0.049(3) 0.018(2) 0.034(2) -0.0056(18) 0.019(2) -0.0004(18) C70 0.032(2) 0.0165(19) 0.030(2) 0.0012(17) 0.0120(17) 0.0024(16) C71 0.034(3) 0.019(3) 0.027(3) 0.000 0.010(2) 0.000 N72 0.0251(19) 0.0200(16) 0.0324(19) -0.0029(14) 0.0117(15) -0.0021(14) N73 0.0277(19) 0.0241(17) 0.0242(17) 0.0013(14) 0.0141(14) 0.0007(14) C74 0.025(3) 0.022(3) 0.031(3) 0.000 0.007(2) 0.000 C75 0.030(3) 0.023(2) 0.045(3) 0.0004(19) 0.001(2) -0.0043(18) C76 0.031(3) 0.021(2) 0.041(3) 0.0013(19) 0.0001(19) 0.0059(18) C77 0.029(3) 0.021(3) 0.030(3) 0.000 0.001(2) 0.000 C78 0.031(4) 0.027(3) 0.033(3) 0.000 0.007(3) 0.000 O79 0.0323(17) 0.0183(14) 0.0426(17) -0.0022(13) -0.0019(13) -0.0026(12) C80 0.036(2) 0.021(2) 0.031(2) 0.0046(17) 0.0176(19) -0.0021(17) C81 0.037(3) 0.068(3) 0.047(3) -0.030(3) 0.018(2) -0.021(2) C82 0.058(4) 0.048(3) 0.068(4) -0.026(3) 0.047(3) -0.020(3) C83 0.077(4) 0.040(3) 0.046(3) 0.013(2) 0.042(3) 0.013(3) C84 0.065(4) 0.181(8) 0.020(3) 0.017(3) 0.015(3) 0.037(5) C85 0.040(3) 0.164(7) 0.031(3) 0.018(3) 0.013(2) 0.031(4) C86 0.130(7) 0.042(3) 0.072(5) 0.024(3) 0.070(5) 0.032(4) O87 0.146(6) 0.272(9) 0.033(3) 0.012(4) 0.033(3) 0.076(6) O88 0.145(5) 0.038(2) 0.097(3) 0.005(2) 0.102(3) 0.008(2) C89 0.032(3) 0.017(3) 0.027(3) 0.000 0.010(2) 0.000 C90 0.033(3) 0.023(2) 0.034(2) 0.0059(18) 0.0068(19) 0.0060(18) C91 0.031(2) 0.022(2) 0.036(2) 0.0006(18) 0.0079(19) -0.0038(17) C92 0.023(3) 0.019(3) 0.028(3) 0.000 0.012(2) 0.000 C93 0.025(3) 0.020(3) 0.030(3) 0.000 0.016(2) 0.000 Cu2 0.143(7) 0.116(5) 0.166(7) 0.000 0.049(5) 0.000 O95 0.0366(18) 0.0280(15) 0.0250(15) 0.0035(12) 0.0096(13) -0.0020(13) C96 0.056(4) 0.076(4) 0.036(3) -0.002(3) 0.008(2) -0.030(3) N97 0.064(3) 0.065(3) 0.051(3) -0.012(2) 0.029(2) -0.032(2) C98 0.058(4) 0.109(5) 0.063(4) -0.028(4) 0.030(3) -0.035(4) C99 0.079(5) 0.115(6) 0.082(5) -0.014(4) 0.044(4) -0.043(4) O101 0.053(3) 0.191(5) 0.043(2) -0.037(3) 0.0185(19) -0.043(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O33 2.275(3) 2_755 ? Eu1 O94 2.350(3) . ? Eu1 O32 2.361(3) . ? Eu1 O79 2.376(3) 2_745 ? Eu1 O50 2.393(3) 7_656 ? Eu1 O42 2.397(3) 6 ? Eu1 O95 2.451(3) . ? Eu1 O33 3.107(3) . ? Eu1 C31 3.105(4) . ? Eu1 O101 3.114(5) . ? Eu1 Eu2 3.9760(3) . ? Eu1 Eu1 4.1945(4) 2_755 ? Eu2 O100A 2.306(7) . ? Eu2 O88 2.328(3) 5_765 ? Eu2 O59 2.418(3) 6_565 ? Eu2 O101 2.419(4) . ? Eu2 O41 2.425(3) 6 ? Eu2 O50 2.454(2) 7_656 ? Eu2 O100B 2.471(6) . ? Eu2 O60 2.487(3) 6_565 ? Eu2 O51 2.570(3) 7_656 ? Eu2 O42 2.733(3) 6 ? Eu2 C58 2.822(4) 6_565 ? Eu2 C49 2.874(4) 7_656 ? C1 N21 1.389(5) . ? C1 C20 1.424(6) . ? C1 C2 1.429(6) . ? C2 C3 1.350(6) . ? C2 H2 0.9500 . ? C3 C4 1.440(6) . ? C3 H3 0.9500 . ? C4 N21 1.361(5) . ? C4 C5 1.413(5) . ? C5 C6 1.393(5) . ? C5 C25 1.503(5) . ? C6 N22 1.375(5) . ? C6 C7 1.427(6) . ? C7 C8 1.344(6) . ? C7 H7 0.9500 . ? C8 C9 1.440(5) . ? C8 H8 0.9500 . ? C9 N22 1.373(5) . ? C9 C10 1.395(5) . ? C10 C11 1.397(5) . ? C10 C34 1.497(6) . ? C11 N23 1.360(5) . ? C11 C12 1.442(5) . ? C12 C13 1.350(5) . ? C12 H12 0.9500 . ? C13 C14 1.446(5) . ? C13 H13 0.9500 . ? C14 N23 1.383(5) . ? C14 C15 1.405(5) . ? C15 C16 1.402(5) . ? C15 C43 1.495(5) . ? C16 N24 1.359(5) . ? C16 C17 1.420(6) . ? C17 C18 1.356(6) . ? C17 H17 0.9500 . ? C18 C19 1.432(6) . ? C18 H18 0.9500 . ? C19 N24 1.377(5) . ? C19 C20 1.401(6) . ? C20 C52 1.492(6) . ? N21 Cu1 2.006(5) . ? N22 Cu1 2.006(5) . ? N23 Cu1 2.009(5) . ? N24 Cu1 2.055(5) . ? C25 C30 1.361(6) . ? C25 C26 1.387(6) . ? C26 C27 1.384(5) . ? C26 H26 0.9500 . ? C27 C28 1.384(6) . ? C27 H27 0.9500 . ? C28 C29 1.369(6) . ? C28 C31 1.477(5) . ? C29 C30 1.402(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O32 1.261(5) . ? C31 O33 1.275(5) . ? O33 Eu1 2.275(3) 2_755 ? C34 C39 1.399(6) . ? C34 C35 1.393(6) . ? C35 C36 1.379(6) . ? C35 H35 0.9500 . ? C36 C37 1.386(6) . ? C36 H36 0.9500 . ? C37 C38 1.400(6) . ? C37 C40 1.477(6) . ? C38 C39 1.374(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O41 1.246(5) . ? C40 O42 1.283(5) . ? C40 Eu2 2.932(4) 6_556 ? O41 Eu2 2.425(3) 6_556 ? O42 Eu1 2.397(3) 6_556 ? O42 Eu2 2.733(3) 6_556 ? C43 C44 1.393(6) . ? C43 C48 1.394(6) . ? C44 C45 1.385(5) . ? C44 H44 0.9500 . ? C45 C46 1.386(5) . ? C45 H45 0.9500 . ? C46 C47 1.381(6) . ? C46 C49 1.500(5) . ? C47 C48 1.408(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O51 1.252(5) . ? C49 O50 1.284(5) . ? C49 Eu2 2.875(4) 7_656 ? O50 Eu1 2.393(3) 7_656 ? O50 Eu2 2.454(2) 7_656 ? O51 Eu2 2.570(3) 7_656 ? C52 C57 1.377(6) . ? C52 C53 1.404(6) . ? C53 C54 1.379(6) . ? C53 H53 0.9500 . ? C54 C55 1.398(6) . ? C54 H54 0.9500 . ? C55 C56 1.389(6) . ? C55 C58 1.495(6) . ? C56 C57 1.389(6) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O59 1.269(5) . ? C58 O60 1.281(5) . ? C58 Eu2 2.822(4) 6_566 ? O59 Eu2 2.419(3) 6_566 ? O60 Eu2 2.487(3) 6_566 ? C61 C62 1.414(4) 2_755 ? C61 C62 1.414(4) . ? C61 C74 1.483(7) . ? C62 N72 1.382(5) . ? C62 C63 1.429(5) . ? C63 C64 1.355(6) . ? C63 H63 0.9500 . ? C64 C65 1.430(6) . ? C64 H64 0.9500 . ? C65 N72 1.381(5) . ? C65 C66 1.398(5) . ? C66 C67 1.409(5) . ? C66 C80 1.497(5) . ? C67 N73 1.375(4) . ? C67 C68 1.445(5) . ? C68 C69 1.360(5) . ? C68 H68 0.9500 . ? C69 C70 1.424(5) . ? C69 H69 0.9500 . ? C70 N73 1.386(5) . ? C70 C71 1.395(4) . ? C71 C70 1.395(4) 2_755 ? C71 C89 1.498(7) . ? N72 Cu2 2.068(6) 3 ? N73 Cu2 2.027(6) 3 ? C74 C75 1.398(5) 2_755 ? C74 C75 1.398(5) . ? C75 C76 1.381(6) . ? C75 H75 0.9500 . ? C76 C77 1.381(5) . ? C76 H76 0.9500 . ? C77 C76 1.381(5) 2_755 ? C77 C78 1.516(8) . ? C78 O79 1.259(4) . ? C78 O79 1.259(4) 2_755 ? O79 Eu1 2.376(3) 2_765 ? C80 C85 1.350(7) . ? C80 C81 1.369(6) . ? C81 C82 1.364(6) . ? C81 H81 0.9500 . ? C82 C83 1.378(8) . ? C82 H82 0.9500 . ? C83 C84 1.352(8) . ? C83 C86 1.552(7) . ? C84 C85 1.372(7) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C86 O88 1.190(8) . ? C86 O87 1.251(10) . ? C86 Eu2 3.178(6) 5_765 ? O88 Eu2 2.328(3) 5_765 ? C89 C90 1.390(5) 2_755 ? C89 C90 1.390(5) . ? C90 C91 1.401(5) . ? C90 H90 0.9500 . ? C91 C92 1.389(5) . ? C91 H91 0.9500 . ? C92 C91 1.389(5) 2_755 ? C92 C93 1.491(7) . ? C93 O94 1.263(4) 2_755 ? C93 O94 1.263(4) . ? Cu2 N73 2.027(6) 4_645 ? Cu2 N73 2.027(6) 3_445 ? Cu2 N72 2.068(6) 4_645 ? Cu2 N72 2.068(6) 3_445 ? O95 C96 1.242(5) . ? C96 N97 1.295(6) . ? C96 H96 0.9500 . ? N97 C98 1.416(6) . ? N97 C99 1.488(6) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? O101 H10A 0.9900 . ? O101 H10B 0.9900 . ? 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 O33 Eu1 O94 77.76(10) 2_755 . ? O33 Eu1 O32 123.78(10) 2_755 . ? O94 Eu1 O32 83.17(9) . . ? O33 Eu1 O79 74.07(10) 2_755 2_745 ? O94 Eu1 O79 129.85(10) . 2_745 ? O32 Eu1 O79 79.33(10) . 2_745 ? O33 Eu1 O50 130.89(9) 2_755 7_656 ? O94 Eu1 O50 72.64(9) . 7_656 ? O32 Eu1 O50 90.69(9) . 7_656 ? O79 Eu1 O50 153.04(9) 2_745 7_656 ? O33 Eu1 O42 90.27(10) 2_755 6 ? O94 Eu1 O42 121.39(9) . 6 ? O32 Eu1 O42 143.09(10) . 6 ? O79 Eu1 O42 99.50(9) 2_745 6 ? O50 Eu1 O42 73.68(9) 7_656 6 ? O33 Eu1 O95 143.28(9) 2_755 . ? O94 Eu1 O95 138.96(9) . . ? O32 Eu1 O95 72.26(9) . . ? O79 Eu1 O95 77.83(9) 2_745 . ? O50 Eu1 O95 75.28(9) 7_656 . ? O42 Eu1 O95 71.49(9) 6 . ? O33 Eu1 O33 78.65(8) 2_755 . ? O94 Eu1 O33 67.20(8) . . ? O32 Eu1 O33 45.31(9) . . ? O79 Eu1 O33 67.13(8) 2_745 . ? O50 Eu1 O33 121.84(8) 7_656 . ? O42 Eu1 O33 164.45(9) 6 . ? O95 Eu1 O33 111.40(8) . . ? O33 Eu1 C31 102.12(11) 2_755 . ? O94 Eu1 C31 75.47(9) . . ? O32 Eu1 C31 21.68(11) . . ? O79 Eu1 C31 71.10(10) 2_745 . ? O50 Eu1 C31 107.09(9) 7_656 . ? O42 Eu1 C31 161.29(10) 6 . ? O95 Eu1 C31 90.45(10) . . ? O33 Eu1 C31 23.68(9) . . ? O33 Eu1 O101 72.87(10) 2_755 . ? O94 Eu1 O101 61.13(10) . . ? O32 Eu1 O101 137.57(11) . . ? O79 Eu1 O101 140.83(11) 2_745 . ? O50 Eu1 O101 58.70(10) 7_656 . ? O42 Eu1 O101 60.49(10) 6 . ? O95 Eu1 O101 119.83(9) . . ? O33 Eu1 O101 124.76(9) . . ? C31 Eu1 O101 136.50(10) . . ? O33 Eu1 Eu2 105.41(7) 2_755 . ? O94 Eu1 Eu2 85.77(7) . . ? O32 Eu1 Eu2 125.39(7) . . ? O79 Eu1 Eu2 141.43(7) 2_745 . ? O50 Eu1 Eu2 35.39(6) 7_656 . ? O42 Eu1 Eu2 42.36(7) 6 . ? O95 Eu1 Eu2 82.60(6) . . ? O33 Eu1 Eu2 151.43(5) . . ? C31 Eu1 Eu2 142.35(7) . . ? O101 Eu1 Eu2 37.46(7) . . ? O33 Eu1 Eu1 46.57(7) 2_755 2_755 ? O94 Eu1 Eu1 64.84(7) . 2_755 ? O32 Eu1 Eu1 77.42(7) . 2_755 ? O79 Eu1 Eu1 65.59(7) 2_745 2_755 ? O50 Eu1 Eu1 136.79(6) 7_656 2_755 ? O42 Eu1 Eu1 136.10(7) 6 2_755 ? O95 Eu1 Eu1 135.94(6) . 2_755 ? O33 Eu1 Eu1 32.12(5) . 2_755 ? C31 Eu1 Eu1 55.75(8) . 2_755 ? O101 Eu1 Eu1 104.14(7) . 2_755 ? Eu2 Eu1 Eu1 141.452(6) . 2_755 ? O100A Eu2 O88 90.4(2) . 5_765 ? O100A Eu2 O59 75.5(3) . 6_565 ? O88 Eu2 O59 128.47(11) 5_765 6_565 ? O100A Eu2 O101 155.0(2) . . ? O88 Eu2 O101 88.09(17) 5_765 . ? O59 Eu2 O101 85.96(17) 6_565 . ? O100A Eu2 O41 87.0(2) . 6 ? O88 Eu2 O41 76.81(12) 5_765 6 ? O59 Eu2 O41 148.39(12) 6_565 6 ? O101 Eu2 O41 116.79(16) . 6 ? O100A Eu2 O50 121.97(19) . 7_656 ? O88 Eu2 O50 143.77(13) 5_765 7_656 ? O59 Eu2 O50 79.36(10) 6_565 7_656 ? O101 Eu2 O50 69.32(11) . 7_656 ? O41 Eu2 O50 88.27(9) 6 7_656 ? O88 Eu2 O100B 76.7(2) 5_765 . ? O59 Eu2 O100B 96.5(2) 6_565 . ? O101 Eu2 O100B 162.35(16) . . ? O41 Eu2 O100B 68.74(19) 6 . ? O50 Eu2 O100B 128.32(15) 7_656 . ? O100A Eu2 O60 76.2(2) . 6_565 ? O88 Eu2 O60 74.98(11) 5_765 6_565 ? O59 Eu2 O60 53.62(10) 6_565 6_565 ? O101 Eu2 O60 79.28(17) . 6_565 ? O41 Eu2 O60 146.89(11) 6 6_565 ? O50 Eu2 O60 124.84(11) 7_656 6_565 ? O100B Eu2 O60 88.08(19) . 6_565 ? O100A Eu2 O51 70.71(18) . 7_656 ? O88 Eu2 O51 148.29(15) 5_765 7_656 ? O59 Eu2 O51 72.48(10) 6_565 7_656 ? O101 Eu2 O51 119.76(10) . 7_656 ? O41 Eu2 O51 76.97(9) 6 7_656 ? O50 Eu2 O51 51.97(9) 7_656 7_656 ? O100B Eu2 O51 77.41(15) . 7_656 ? O60 Eu2 O51 122.01(10) 6_565 7_656 ? O100A Eu2 O42 137.2(2) . 6 ? O88 Eu2 O42 78.27(11) 5_765 6 ? O59 Eu2 O42 142.15(12) 6_565 6 ? O101 Eu2 O42 66.71(15) . 6 ? O41 Eu2 O42 50.22(10) 6 6 ? O50 Eu2 O42 67.01(8) 7_656 6 ? O100B Eu2 O42 117.63(19) . 6 ? O60 Eu2 O42 137.00(11) 6_565 6 ? O51 Eu2 O42 98.09(8) 7_656 6 ? O100A Eu2 C58 74.0(3) . 6_565 ? O88 Eu2 C58 101.90(13) 5_765 6_565 ? O59 Eu2 C58 26.63(11) 6_565 6_565 ? O101 Eu2 C58 81.94(19) . 6_565 ? O41 Eu2 C58 160.98(15) 6 6_565 ? O50 Eu2 C58 102.44(12) 7_656 6_565 ? O100B Eu2 C58 92.4(2) . 6_565 ? O60 Eu2 C58 26.99(11) 6_565 6_565 ? O51 Eu2 C58 97.14(12) 7_656 6_565 ? O42 Eu2 C58 148.64(15) 6 6_565 ? O100A Eu2 C49 95.6(2) . 7_656 ? O88 Eu2 C49 159.95(11) 5_765 7_656 ? O59 Eu2 C49 71.58(10) 6_565 7_656 ? O101 Eu2 C49 94.22(12) . 7_656 ? O41 Eu2 C49 84.42(10) 6 7_656 ? O50 Eu2 C49 26.41(10) 7_656 7_656 ? O100B Eu2 C49 103.15(16) . 7_656 ? O60 Eu2 C49 125.03(10) 6_565 7_656 ? O51 Eu2 C49 25.83(10) 7_656 7_656 ? O42 Eu2 C49 84.35(9) 6 7_656 ? C58 Eu2 C49 98.15(12) 6_565 7_656 ? N21 C1 C20 123.9(4) . . ? N21 C1 C2 109.8(3) . . ? C20 C1 C2 125.8(4) . . ? C3 C2 C1 107.0(4) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.1(4) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N21 C4 C5 123.9(3) . . ? N21 C4 C3 110.2(3) . . ? C5 C4 C3 125.7(3) . . ? C6 C5 C4 125.4(3) . . ? C6 C5 C25 117.6(3) . . ? C4 C5 C25 116.9(3) . . ? N22 C6 C5 124.2(3) . . ? N22 C6 C7 108.9(3) . . ? C5 C6 C7 126.7(3) . . ? C8 C7 C6 107.9(3) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 107.3(4) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N22 C9 C10 125.2(3) . . ? N22 C9 C8 108.7(3) . . ? C10 C9 C8 126.1(4) . . ? C11 C10 C9 125.3(4) . . ? C11 C10 C34 115.3(3) . . ? C9 C10 C34 119.3(3) . . ? N23 C11 C10 125.5(4) . . ? N23 C11 C12 110.0(3) . . ? C10 C11 C12 124.5(4) . . ? C13 C12 C11 107.1(4) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? C12 C13 C14 107.1(3) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N23 C14 C15 125.1(3) . . ? N23 C14 C13 109.1(3) . . ? C15 C14 C13 125.3(3) . . ? C16 C15 C14 123.8(3) . . ? C16 C15 C43 119.4(3) . . ? C14 C15 C43 116.7(3) . . ? N24 C16 C15 125.0(3) . . ? N24 C16 C17 109.0(3) . . ? C15 C16 C17 125.8(3) . . ? C18 C17 C16 107.8(4) . . ? C18 C17 H17 126.1 . . ? C16 C17 H17 126.1 . . ? C17 C18 C19 106.9(4) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? N24 C19 C20 125.4(4) . . ? N24 C19 C18 108.3(3) . . ? C20 C19 C18 126.0(4) . . ? C19 C20 C1 124.9(4) . . ? C19 C20 C52 117.4(3) . . ? C1 C20 C52 117.7(3) . . ? C4 N21 C1 105.6(3) . . ? C4 N21 Cu1 127.3(3) . . ? C1 N21 Cu1 126.9(3) . . ? C9 N22 C6 107.2(3) . . ? C9 N22 Cu1 125.6(3) . . ? C6 N22 Cu1 127.0(3) . . ? C11 N23 C14 106.6(3) . . ? C11 N23 Cu1 125.7(3) . . ? C14 N23 Cu1 127.4(3) . . ? C16 N24 C19 107.6(3) . . ? C16 N24 Cu1 127.1(3) . . ? C19 N24 Cu1 124.9(3) . . ? C30 C25 C26 119.3(4) . . ? C30 C25 C5 119.9(4) . . ? C26 C25 C5 120.8(4) . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.8(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.3(4) . . ? C29 C28 C31 120.6(4) . . ? C27 C28 C31 120.1(4) . . ? C28 C29 C30 119.6(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 121.1(4) . . ? C25 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? O32 C31 O33 121.8(3) . . ? O32 C31 C28 119.0(4) . . ? O33 C31 C28 119.2(4) . . ? O32 C31 Eu1 43.76(18) . . ? O33 C31 Eu1 78.2(2) . . ? C28 C31 Eu1 162.0(3) . . ? C31 O32 Eu1 114.6(3) . . ? C31 O33 Eu1 175.1(2) . 2_755 ? C31 O33 Eu1 78.1(2) . . ? Eu1 O33 Eu1 101.30(8) 2_755 . ? C39 C34 C35 119.3(4) . . ? C39 C34 C10 120.3(4) . . ? C35 C34 C10 120.0(4) . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.9(4) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 119.2(4) . . ? C36 C37 C40 122.0(4) . . ? C38 C37 C40 118.7(4) . . ? C39 C38 C37 120.1(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.5(4) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? O41 C40 O42 121.5(4) . . ? O41 C40 C37 119.8(4) . . ? O42 C40 C37 118.7(4) . . ? O41 C40 Eu2 54.2(2) . 6_556 ? O42 C40 Eu2 68.3(2) . 6_556 ? C37 C40 Eu2 167.6(3) . 6_556 ? C40 O41 Eu2 101.1(3) . 6_556 ? C40 O42 Eu1 134.8(2) . 6_556 ? C40 O42 Eu2 85.8(2) . 6_556 ? Eu1 O42 Eu2 101.42(9) 6_556 6_556 ? C44 C43 C48 119.4(3) . . ? C44 C43 C15 120.1(4) . . ? C48 C43 C15 120.5(4) . . ? C45 C44 C43 121.0(4) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 119.7(4) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 119.9(3) . . ? C47 C46 C49 120.0(4) . . ? C45 C46 C49 120.0(4) . . ? C46 C47 C48 120.7(4) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C43 C48 C47 119.0(4) . . ? C43 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? O51 C49 O50 120.6(3) . . ? O51 C49 C46 121.5(4) . . ? O50 C49 C46 117.9(3) . . ? O51 C49 Eu2 63.4(2) . 7_656 ? O50 C49 Eu2 58.19(18) . 7_656 ? C46 C49 Eu2 169.2(3) . 7_656 ? C49 O50 Eu1 140.4(2) . 7_656 ? C49 O50 Eu2 95.4(2) . 7_656 ? Eu1 O50 Eu2 110.22(9) 7_656 7_656 ? C49 O51 Eu2 90.8(2) . 7_656 ? C57 C52 C53 119.3(4) . . ? C57 C52 C20 120.0(4) . . ? C53 C52 C20 120.8(4) . . ? C54 C53 C52 120.4(4) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 120.1(4) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 119.4(4) . . ? C56 C55 C58 119.4(4) . . ? C54 C55 C58 121.2(4) . . ? C57 C56 C55 120.3(4) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C52 C57 C56 120.6(4) . . ? C52 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? O59 C58 O60 120.4(4) . . ? O59 C58 C55 119.3(4) . . ? O60 C58 C55 120.3(4) . . ? O59 C58 Eu2 58.7(2) . 6_566 ? O60 C58 Eu2 61.7(2) . 6_566 ? C55 C58 Eu2 177.4(4) . 6_566 ? C58 O59 Eu2 94.7(3) . 6_566 ? C58 O60 Eu2 91.3(3) . 6_566 ? N21 Cu1 N22 90.2(2) . . ? N21 Cu1 N23 172.6(3) . . ? N22 Cu1 N23 91.5(2) . . ? N21 Cu1 N24 90.6(2) . . ? N22 Cu1 N24 172.4(3) . . ? N23 Cu1 N24 88.7(2) . . ? C62 C61 C62 124.2(5) 2_755 . ? C62 C61 C74 117.9(2) 2_755 . ? C62 C61 C74 117.9(2) . . ? N72 C62 C61 125.6(4) . . ? N72 C62 C63 109.0(3) . . ? C61 C62 C63 125.2(4) . . ? C64 C63 C62 107.6(4) . . ? C64 C63 H63 126.2 . . ? C62 C63 H63 126.2 . . ? C63 C64 C65 107.5(4) . . ? C63 C64 H64 126.2 . . ? C65 C64 H64 126.2 . . ? N72 C65 C66 126.1(3) . . ? N72 C65 C64 109.1(3) . . ? C66 C65 C64 124.8(4) . . ? C65 C66 C67 125.5(3) . . ? C65 C66 C80 118.7(3) . . ? C67 C66 C80 115.7(3) . . ? N73 C67 C66 126.2(3) . . ? N73 C67 C68 109.3(3) . . ? C66 C67 C68 124.5(3) . . ? C69 C68 C67 106.6(3) . . ? C69 C68 H68 126.7 . . ? C67 C68 H68 126.7 . . ? C68 C69 C70 108.2(3) . . ? C68 C69 H69 125.9 . . ? C70 C69 H69 125.9 . . ? N73 C70 C71 124.9(4) . . ? N73 C70 C69 109.1(3) . . ? C71 C70 C69 126.0(4) . . ? C70 C71 C70 125.7(5) . 2_755 ? C70 C71 C89 117.1(2) . . ? C70 C71 C89 117.1(2) 2_755 . ? C65 N72 C62 106.8(3) . . ? C65 N72 Cu2 124.8(3) . 3 ? C62 N72 Cu2 128.3(3) . 3 ? C67 N73 C70 106.8(3) . . ? C67 N73 Cu2 125.9(3) . 3 ? C70 N73 Cu2 127.3(3) . 3 ? C75 C74 C75 117.0(5) 2_755 . ? C75 C74 C61 121.5(3) 2_755 . ? C75 C74 C61 121.5(3) . . ? C76 C75 C74 121.3(4) . . ? C76 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C77 C76 C75 120.8(4) . . ? C77 C76 H76 119.6 . . ? C75 C76 H76 119.6 . . ? C76 C77 C76 118.7(5) . 2_755 ? C76 C77 C78 120.7(3) . . ? C76 C77 C78 120.7(3) 2_755 . ? O79 C78 O79 125.7(5) . 2_755 ? O79 C78 C77 117.2(3) . . ? O79 C78 C77 117.2(3) 2_755 . ? C78 O79 Eu1 141.1(3) . 2_765 ? C85 C80 C81 116.3(4) . . ? C85 C80 C66 121.9(4) . . ? C81 C80 C66 121.7(4) . . ? C80 C81 C82 123.1(5) . . ? C80 C81 H81 118.4 . . ? C82 C81 H81 118.4 . . ? C81 C82 C83 119.2(5) . . ? C81 C82 H82 120.4 . . ? C83 C82 H82 120.4 . . ? C84 C83 C82 118.3(4) . . ? C84 C83 C86 119.2(6) . . ? C82 C83 C86 122.5(6) . . ? C83 C84 C85 121.1(6) . . ? C83 C84 H84 119.4 . . ? C85 C84 H84 119.4 . . ? C80 C85 C84 121.9(5) . . ? C80 C85 H85 119.0 . . ? C84 C85 H85 119.0 . . ? O88 C86 O87 124.9(6) . . ? O88 C86 C83 118.2(8) . . ? O87 C86 C83 116.9(7) . . ? O88 C86 Eu2 36.3(3) . 5_765 ? O87 C86 Eu2 89.8(4) . 5_765 ? C83 C86 Eu2 151.4(5) . 5_765 ? C86 O88 Eu2 126.1(5) . 5_765 ? C90 C89 C90 119.0(5) 2_755 . ? C90 C89 C71 120.5(2) 2_755 . ? C90 C89 C71 120.5(2) . . ? C89 C90 C91 120.5(4) . . ? C89 C90 H90 119.8 . . ? C91 C90 H90 119.8 . . ? C92 C91 C90 120.4(4) . . ? C92 C91 H91 119.8 . . ? C90 C91 H91 119.8 . . ? C91 C92 C91 119.2(5) 2_755 . ? C91 C92 C93 120.4(2) 2_755 . ? C91 C92 C93 120.4(2) . . ? O94 C93 O94 123.9(5) 2_755 . ? O94 C93 C92 118.1(2) 2_755 . ? O94 C93 C92 118.1(2) . . ? C93 O94 Eu1 141.4(3) . . ? N73 Cu2 N73 89.8(3) 4_645 3_445 ? N73 Cu2 N72 91.25(12) 4_645 4_645 ? N73 Cu2 N72 176.88(16) 3_445 4_645 ? N73 Cu2 N72 176.88(16) 4_645 3_445 ? N73 Cu2 N72 91.25(12) 3_445 3_445 ? N72 Cu2 N72 87.9(3) 4_645 3_445 ? C96 O95 Eu1 131.6(3) . . ? O95 C96 N97 126.1(5) . . ? O95 C96 H96 116.9 . . ? N97 C96 H96 116.9 . . ? C96 N97 C98 121.9(4) . . ? C96 N97 C99 122.0(5) . . ? C98 N97 C99 116.1(4) . . ? N97 C98 H98A 109.5 . . ? N97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? N97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N97 C99 H99A 109.5 . . ? N97 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N97 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? Eu2 O101 Eu1 91.00(13) . . ? Eu2 O101 H10A 113.5 . . ? Eu1 O101 H10A 113.5 . . ? Eu2 O101 H10B 113.5 . . ? Eu1 O101 H10B 113.5 . . ? H10A O101 H10B 110.8 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.918 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.122 #======================END=========================== data_Compound-9 _database_code_depnum_ccdc_archive 'CCDC 627704' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H33 N5 O10 Yb' _chemical_formula_sum 'C51 H33 N5 O10 Yb' _chemical_formula_weight 1048.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 8.7631(2) _cell_length_b 15.9735(4) _cell_length_c 19.0533(6) _cell_angle_alpha 100.1278(9) _cell_angle_beta 95.4584(8) _cell_angle_gamma 102.206(2) _cell_volume 2541.75(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7710 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.25 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5541 _exptl_absorpt_correction_T_max 0.7623 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.7 deg \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22843 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.25 _reflns_number_total 11868 _reflns_number_gt 9223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.061. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^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 11868 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.099 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.169527(19) -0.056160(12) -0.030078(10) 0.01459(7) Uani 1 1 d . . . C1 C 1.0074(5) 0.7388(3) 0.5112(2) 0.0222(10) Uani 1 1 d . . . C2 C 1.0665(6) 0.8244(3) 0.4969(3) 0.0296(11) Uani 1 1 d . . . H2 H 1.1223 0.8749 0.5311 0.036 Uiso 1 1 calc R . . C3 C 1.0276(6) 0.8194(3) 0.4252(3) 0.0289(11) Uani 1 1 d . . . H3 H 1.0529 0.8657 0.4000 0.035 Uiso 1 1 calc R . . C4 C 0.9419(5) 0.7320(3) 0.3946(3) 0.0229(10) Uani 1 1 d . . . C5 C 0.8873(5) 0.6987(3) 0.3216(2) 0.0196(9) Uani 1 1 d . . . C6 C 0.8016(5) 0.6132(3) 0.2919(2) 0.0193(9) Uani 1 1 d . . . C7 C 0.7446(5) 0.5793(3) 0.2170(2) 0.0235(10) Uani 1 1 d . . . H7 H 0.7653 0.6091 0.1788 0.028 Uiso 1 1 calc R . . C8 C 0.6565(6) 0.4975(3) 0.2106(3) 0.0249(10) Uani 1 1 d . . . H8 H 0.6038 0.4591 0.1672 0.030 Uiso 1 1 calc R . . C9 C 0.6573(5) 0.4794(3) 0.2826(2) 0.0183(9) Uani 1 1 d . . . C10 C 0.5647(5) 0.4048(3) 0.3000(2) 0.0183(9) Uani 1 1 d . . . C11 C 0.5514(5) 0.3896(3) 0.3692(2) 0.0203(9) Uani 1 1 d . . . C12 C 0.4488(6) 0.3165(3) 0.3880(3) 0.0274(11) Uani 1 1 d . . . H12 H 0.3735 0.2713 0.3555 0.033 Uiso 1 1 calc R . . C13 C 0.4786(6) 0.3233(3) 0.4604(3) 0.0268(11) Uani 1 1 d . . . H13 H 0.4251 0.2854 0.4881 0.032 Uiso 1 1 calc R . . C14 C 0.6065(5) 0.3987(3) 0.4872(3) 0.0219(10) Uani 1 1 d . . . C15 C 0.6886(5) 0.4241(3) 0.5572(2) 0.0199(9) Uani 1 1 d . . . C16 C 0.8080(5) 0.4988(3) 0.5822(2) 0.0202(9) Uani 1 1 d . . . C17 C 0.9094(5) 0.5211(3) 0.6512(3) 0.0245(10) Uani 1 1 d . . . H17 H 0.9103 0.4854 0.6861 0.029 Uiso 1 1 calc R . . C18 C 1.0007(5) 0.6010(3) 0.6564(2) 0.0237(10) Uani 1 1 d . . . H18 H 1.0771 0.6325 0.6962 0.028 Uiso 1 1 calc R . . C19 C 0.9629(5) 0.6309(3) 0.5909(2) 0.0207(10) Uani 1 1 d . . . C20 C 1.0280(5) 0.7140(3) 0.5779(2) 0.0194(9) Uani 1 1 d . . . N21 N 0.9287(4) 0.6851(3) 0.44827(19) 0.0203(8) Uani 1 1 d . . . H21 H 0.8785 0.6300 0.4432 0.024 Uiso 1 1 calc R . . N22 N 0.7478(4) 0.5509(2) 0.3311(2) 0.0174(8) Uani 1 1 d . . . N23 N 0.6430(4) 0.4391(3) 0.4312(2) 0.0200(8) Uani 1 1 d . . . H23 H 0.7133 0.4884 0.4344 0.024 Uiso 1 1 calc R . . N24 N 0.8496(4) 0.5666(3) 0.5459(2) 0.0213(8) Uani 1 1 d . . . C25 C 0.9217(5) 0.7597(3) 0.2699(2) 0.0192(9) Uani 1 1 d . . . C26 C 0.8385(5) 0.8245(3) 0.2671(3) 0.0229(10) Uani 1 1 d . . . H26 H 0.7645 0.8322 0.2996 0.028 Uiso 1 1 calc R . . C27 C 0.8631(5) 0.8781(3) 0.2169(3) 0.0260(11) Uani 1 1 d . . . H27 H 0.8053 0.9219 0.2149 0.031 Uiso 1 1 calc R . . C28 C 0.9726(5) 0.8673(3) 0.1697(2) 0.0182(9) Uani 1 1 d . . . C29 C 1.0587(5) 0.8041(3) 0.1746(2) 0.0219(10) Uani 1 1 d . . . H29 H 1.1364 0.7977 0.1437 0.026 Uiso 1 1 calc R . . C30 C 1.0323(5) 0.7510(3) 0.2235(3) 0.0236(10) Uani 1 1 d . . . H30 H 1.0907 0.7075 0.2255 0.028 Uiso 1 1 calc R . . C31 C 0.9909(5) 0.9202(3) 0.1119(2) 0.0156(9) Uani 1 1 d . . . O32 O 1.1020(3) 0.9135(2) 0.07479(16) 0.0183(7) Uani 1 1 d . . . O33 O 0.8928(3) 0.9658(2) 0.10291(16) 0.0194(7) Uani 1 1 d . . . C34 C 0.4774(5) 0.3336(3) 0.2383(2) 0.0202(9) Uani 1 1 d . . . C35 C 0.5624(5) 0.2862(3) 0.1952(3) 0.0216(10) Uani 1 1 d . . . H35 H 0.6743 0.3009 0.2041 0.026 Uiso 1 1 calc R . . C36 C 0.4854(5) 0.2184(3) 0.1399(2) 0.0181(9) Uani 1 1 d . . . H36 H 0.5451 0.1863 0.1113 0.022 Uiso 1 1 d R . . C37 C 0.3230(5) 0.1959(3) 0.1254(2) 0.0161(9) Uani 1 1 d . . . C38 C 0.2380(5) 0.2451(3) 0.1667(2) 0.0210(10) Uani 1 1 d . . . H38 H 0.1262 0.2316 0.1566 0.025 Uiso 1 1 calc R . . C39 C 0.3141(5) 0.3131(3) 0.2221(3) 0.0240(10) Uani 1 1 d . . . H39 H 0.2544 0.3464 0.2496 0.029 Uiso 1 1 calc R . . C40 C 0.2434(4) 0.1181(3) 0.0680(2) 0.0153(9) Uani 1 1 d . . . O41 O 0.0935(3) 0.0953(2) 0.05761(17) 0.0201(7) Uani 1 1 d . . . O42 O 0.3242(3) 0.0760(2) 0.03201(16) 0.0185(7) Uani 1 1 d . . . C43 C 0.6491(5) 0.3636(3) 0.6084(3) 0.0214(10) Uani 1 1 d . . . C44 C 0.6113(5) 0.3951(3) 0.6758(3) 0.0247(10) Uani 1 1 d . . . H44 H 0.6054 0.4544 0.6890 0.030 Uiso 1 1 calc R . . C45 C 0.5819(5) 0.3385(4) 0.7243(3) 0.0293(11) Uani 1 1 d . . . H45 H 0.5567 0.3599 0.7705 0.035 Uiso 1 1 calc R . . C46 C 0.5893(5) 0.2513(3) 0.7052(3) 0.0249(10) Uani 1 1 d . . . C47 C 0.6243(6) 0.2203(3) 0.6382(3) 0.0306(11) Uani 1 1 d . . . H47 H 0.6282 0.1607 0.6248 0.037 Uiso 1 1 calc R . . C48 C 0.6541(6) 0.2757(3) 0.5899(3) 0.0305(11) Uani 1 1 d . . . H48 H 0.6783 0.2534 0.5438 0.037 Uiso 1 1 calc R . . C49 C 0.5632(5) 0.1951(4) 0.7597(3) 0.0275(11) Uani 1 1 d . . . O50 O 0.5667(4) 0.2244(3) 0.82314(19) 0.0355(9) Uani 1 1 d . . . O51 O 0.5406(4) 0.1105(2) 0.73265(19) 0.0335(9) Uani 1 1 d . . . C52 C 1.1204(5) 0.7810(3) 0.6407(2) 0.0188(9) Uani 1 1 d . . . C53 C 1.2786(5) 0.8210(3) 0.6426(2) 0.0245(10) Uani 1 1 d . . . H53 H 1.3300 0.8079 0.6017 0.029 Uiso 1 1 calc R . . C54 C 1.3623(5) 0.8799(3) 0.7036(3) 0.0250(11) Uani 1 1 d . . . H54 H 1.4702 0.9066 0.7040 0.030 Uiso 1 1 calc R . . C55 C 1.2892(5) 0.8998(3) 0.7636(2) 0.0196(9) Uani 1 1 d . . . C56 C 1.1295(5) 0.8622(3) 0.7609(2) 0.0260(11) Uani 1 1 d . . . H56 H 1.0775 0.8766 0.8013 0.031 Uiso 1 1 calc R . . C57 C 1.0465(5) 0.8044(4) 0.7003(3) 0.0284(11) Uani 1 1 d . . . H57 H 0.9373 0.7801 0.6992 0.034 Uiso 1 1 calc R . . C58 C 1.3810(5) 0.9566(3) 0.8318(2) 0.0153(9) Uani 1 1 d . . . O59 O 1.5019(3) 1.0145(2) 0.83001(17) 0.0231(7) Uani 1 1 d . . . O60 O 1.3335(3) 0.9423(2) 0.89010(15) 0.0157(6) Uani 1 1 d . . . O61 O 0.3873(3) -0.0917(2) 0.02818(16) 0.0177(6) Uani 1 1 d . . . O62 O 0.1231(4) -0.2070(2) -0.06814(19) 0.0253(7) Uani 1 1 d . B . C63 C 0.1590(8) -0.2568(5) -0.0295(5) 0.072(3) Uani 1 1 d . . . H63 H 0.2413 -0.2293 0.0090 0.087 Uiso 1 1 calc R A 1 N64A N 0.1063(15) -0.3370(9) -0.0319(7) 0.068(3) Uiso 0.50 1 d P B 1 C65A C 0.0273(17) -0.3870(10) -0.1018(8) 0.061(4) Uiso 0.50 1 d P B 1 H65A H -0.0871 -0.3981 -0.1019 0.091 Uiso 0.50 1 calc PR B 1 H65B H 0.0589 -0.4427 -0.1117 0.091 Uiso 0.50 1 calc PR B 1 H65C H 0.0568 -0.3537 -0.1390 0.091 Uiso 0.50 1 calc PR B 1 C66A C 0.123(2) -0.3842(16) 0.0296(12) 0.105(7) Uiso 0.50 1 d P B 1 H66A H 0.2055 -0.3476 0.0675 0.158 Uiso 0.50 1 calc PR B 1 H66B H 0.1516 -0.4395 0.0120 0.158 Uiso 0.50 1 calc PR B 1 H66C H 0.0228 -0.3961 0.0489 0.158 Uiso 0.50 1 calc PR B 1 N64B N 0.1362(13) -0.3464(8) -0.0683(6) 0.056(3) Uiso 0.50 1 d P B 2 C65B C 0.0389(13) -0.3820(8) -0.1428(6) 0.037(3) Uiso 0.50 1 d P B 2 H65D H -0.0689 -0.4101 -0.1374 0.056 Uiso 0.50 1 calc PR B 2 H65E H 0.0867 -0.4248 -0.1706 0.056 Uiso 0.50 1 calc PR B 2 H65F H 0.0367 -0.3337 -0.1680 0.056 Uiso 0.50 1 calc PR B 2 C66B C 0.211(2) -0.4027(14) -0.0242(11) 0.093(6) Uiso 0.50 1 d P B 2 H66D H 0.3069 -0.4128 -0.0429 0.140 Uiso 0.50 1 calc PR B 2 H66E H 0.1359 -0.4588 -0.0277 0.140 Uiso 0.50 1 calc PR B 2 H66F H 0.2365 -0.3723 0.0263 0.140 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.01237(10) 0.01641(11) 0.01416(11) 0.00378(7) 0.00122(6) 0.00122(7) C1 0.028(2) 0.023(3) 0.013(2) 0.0004(19) 0.0017(17) 0.0034(19) C2 0.043(3) 0.019(3) 0.021(3) 0.002(2) -0.002(2) -0.001(2) C3 0.037(3) 0.021(3) 0.023(3) 0.006(2) -0.004(2) -0.002(2) C4 0.029(2) 0.019(3) 0.018(2) 0.005(2) -0.0004(18) 0.0021(19) C5 0.019(2) 0.025(3) 0.016(2) 0.0092(19) 0.0010(16) 0.0036(18) C6 0.021(2) 0.020(2) 0.017(2) 0.0062(19) 0.0002(16) 0.0046(18) C7 0.032(3) 0.024(3) 0.014(2) 0.008(2) 0.0018(18) 0.003(2) C8 0.034(3) 0.021(3) 0.015(2) 0.002(2) -0.0018(18) 0.000(2) C9 0.019(2) 0.016(2) 0.018(2) 0.0036(18) -0.0031(16) 0.0029(17) C10 0.018(2) 0.013(2) 0.021(2) 0.0009(18) -0.0012(16) 0.0024(16) C11 0.021(2) 0.019(2) 0.020(2) 0.0041(19) 0.0032(17) 0.0023(18) C12 0.031(3) 0.018(3) 0.030(3) 0.004(2) 0.002(2) -0.0009(19) C13 0.030(3) 0.024(3) 0.025(3) 0.009(2) 0.0075(19) -0.002(2) C14 0.024(2) 0.018(2) 0.023(2) 0.005(2) 0.0054(18) 0.0023(18) C15 0.027(2) 0.019(2) 0.017(2) 0.0055(19) 0.0073(17) 0.0070(18) C16 0.027(2) 0.016(2) 0.019(2) 0.0040(19) 0.0052(17) 0.0065(18) C17 0.026(2) 0.028(3) 0.020(2) 0.009(2) 0.0004(18) 0.005(2) C18 0.024(2) 0.029(3) 0.015(2) 0.004(2) -0.0034(17) 0.0025(19) C19 0.022(2) 0.025(3) 0.014(2) 0.006(2) 0.0036(17) 0.0012(18) C20 0.025(2) 0.020(2) 0.011(2) -0.0003(18) -0.0016(16) 0.0036(18) N21 0.031(2) 0.014(2) 0.0119(19) 0.0006(15) 0.0006(15) 0.0007(15) N22 0.0222(19) 0.0131(19) 0.0157(19) 0.0026(15) -0.0005(14) 0.0033(14) N23 0.0228(19) 0.017(2) 0.020(2) 0.0077(16) 0.0044(15) 0.0011(15) N24 0.026(2) 0.017(2) 0.020(2) 0.0074(17) 0.0030(15) 0.0023(16) C25 0.024(2) 0.016(2) 0.016(2) 0.0039(18) 0.0007(17) 0.0002(17) C26 0.025(2) 0.030(3) 0.021(2) 0.014(2) 0.0099(18) 0.0114(19) C27 0.029(3) 0.032(3) 0.023(3) 0.013(2) 0.0064(19) 0.014(2) C28 0.020(2) 0.021(2) 0.015(2) 0.0062(19) 0.0004(16) 0.0036(17) C29 0.024(2) 0.027(3) 0.020(2) 0.009(2) 0.0094(17) 0.0105(19) C30 0.023(2) 0.023(3) 0.029(3) 0.010(2) 0.0023(18) 0.0092(19) C31 0.014(2) 0.017(2) 0.014(2) 0.0051(18) 0.0013(15) 0.0004(16) O32 0.0179(15) 0.0249(18) 0.0154(16) 0.0093(13) 0.0051(11) 0.0065(12) O33 0.0165(15) 0.0250(18) 0.0221(17) 0.0132(14) 0.0070(12) 0.0081(13) C34 0.023(2) 0.017(2) 0.019(2) 0.0045(19) -0.0023(17) 0.0027(18) C35 0.014(2) 0.021(3) 0.027(3) 0.001(2) -0.0037(17) 0.0031(17) C36 0.019(2) 0.016(2) 0.015(2) -0.0067(18) 0.0017(16) 0.0031(17) C37 0.017(2) 0.017(2) 0.012(2) 0.0028(18) -0.0026(15) 0.0021(16) C38 0.009(2) 0.026(3) 0.023(2) -0.001(2) -0.0012(16) -0.0005(17) C39 0.022(2) 0.025(3) 0.022(3) -0.001(2) 0.0035(18) 0.0033(19) C40 0.0090(19) 0.013(2) 0.020(2) 0.0052(18) -0.0021(15) -0.0052(16) O41 0.0167(15) 0.0208(18) 0.0218(17) 0.0062(14) 0.0014(12) 0.0013(12) O42 0.0153(15) 0.0160(17) 0.0188(16) -0.0034(13) -0.0012(12) -0.0006(12) C43 0.023(2) 0.019(3) 0.021(2) 0.005(2) 0.0007(17) 0.0027(18) C44 0.026(2) 0.027(3) 0.022(3) 0.003(2) 0.0070(18) 0.0063(19) C45 0.028(3) 0.040(3) 0.023(3) 0.010(2) 0.0099(19) 0.010(2) C46 0.022(2) 0.027(3) 0.024(3) 0.010(2) 0.0032(18) -0.0004(19) C47 0.044(3) 0.019(3) 0.028(3) 0.006(2) 0.008(2) 0.003(2) C48 0.043(3) 0.024(3) 0.027(3) 0.007(2) 0.013(2) 0.008(2) C49 0.024(2) 0.034(3) 0.026(3) 0.009(2) 0.0051(19) 0.007(2) O50 0.044(2) 0.043(2) 0.024(2) 0.0162(18) 0.0101(15) 0.0080(17) O51 0.045(2) 0.026(2) 0.028(2) 0.0124(17) 0.0056(16) -0.0013(16) C52 0.024(2) 0.019(2) 0.010(2) 0.0023(18) -0.0035(16) 0.0012(18) C53 0.028(2) 0.028(3) 0.014(2) 0.001(2) 0.0042(18) 0.003(2) C54 0.020(2) 0.030(3) 0.020(2) 0.004(2) 0.0062(17) -0.0047(19) C55 0.022(2) 0.019(2) 0.016(2) 0.0038(19) -0.0012(17) 0.0018(17) C56 0.020(2) 0.037(3) 0.014(2) -0.004(2) 0.0036(17) -0.002(2) C57 0.018(2) 0.041(3) 0.019(2) 0.002(2) -0.0007(17) -0.003(2) C58 0.014(2) 0.015(2) 0.016(2) 0.0039(18) 0.0012(15) 0.0030(16) O59 0.0227(16) 0.0272(19) 0.0145(16) 0.0057(14) -0.0018(12) -0.0045(13) O60 0.0173(15) 0.0216(17) 0.0105(15) 0.0054(13) 0.0057(11) 0.0061(12) O61 0.0142(14) 0.0236(18) 0.0153(16) 0.0062(13) -0.0006(11) 0.0035(12) O62 0.0217(16) 0.0182(18) 0.034(2) 0.0020(15) 0.0045(13) 0.0034(13) C63 0.059(4) 0.027(4) 0.122(8) 0.030(4) -0.005(4) -0.013(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 Yb O60 2.190(3) 1_444 ? Yb O32 2.241(3) 1_445 ? Yb O41 2.242(3) 2 ? Yb O33 2.280(3) 2_665 ? Yb O42 2.302(3) . ? Yb O62 2.327(3) . ? Yb O61 2.340(3) . ? Yb O41 2.926(3) . ? Yb C40 2.973(4) . ? Yb C63 3.189(7) . ? Yb Yb 3.9420(4) 2 ? C1 N21 1.371(6) . ? C1 C20 1.402(6) . ? C1 C2 1.438(7) . ? C2 C3 1.360(7) . ? C2 H2 0.9500 . ? C3 C4 1.428(7) . ? C3 H3 0.9500 . ? C4 N21 1.369(6) . ? C4 C5 1.398(7) . ? C5 C6 1.401(7) . ? C5 C25 1.509(6) . ? C6 N22 1.378(6) . ? C6 C7 1.434(6) . ? C7 C8 1.347(7) . ? C7 H7 0.9500 . ? C8 C9 1.451(7) . ? C8 H8 0.9500 . ? C9 N22 1.376(6) . ? C9 C10 1.403(6) . ? C10 C11 1.394(7) . ? C10 C34 1.500(6) . ? C11 N23 1.374(6) . ? C11 C12 1.436(6) . ? C12 C13 1.360(7) . ? C12 H12 0.9500 . ? C13 C14 1.440(7) . ? C13 H13 0.9500 . ? C14 N23 1.370(6) . ? C14 C15 1.401(7) . ? C15 C16 1.386(7) . ? C15 C43 1.503(6) . ? C16 N24 1.388(6) . ? C16 C17 1.458(7) . ? C17 C18 1.336(7) . ? C17 H17 0.9500 . ? C18 C19 1.447(7) . ? C18 H18 0.9500 . ? C19 N24 1.369(6) . ? C19 C20 1.404(7) . ? C20 C52 1.494(6) . ? N21 H21 0.8800 . ? N23 H23 0.8800 . ? C25 C30 1.385(7) . ? C25 C26 1.392(7) . ? C26 C27 1.394(7) . ? C26 H26 0.9500 . ? C27 C28 1.392(6) . ? C27 H27 0.9500 . ? C28 C29 1.394(7) . ? C28 C31 1.503(6) . ? C29 C30 1.369(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O33 1.257(5) . ? C31 O32 1.267(5) . ? O32 Yb 2.241(3) 1_665 ? O33 Yb 2.280(3) 2_665 ? C34 C39 1.390(6) . ? C34 C35 1.392(7) . ? C35 C36 1.377(6) . ? C35 H35 0.9500 . ? C36 C37 1.381(6) . ? C36 H36 0.9500 . ? C37 C38 1.391(6) . ? C37 C40 1.495(6) . ? C38 C39 1.377(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O42 1.247(5) . ? C40 O41 1.273(5) . ? O41 Yb 2.242(3) 2 ? C43 C44 1.393(7) . ? C43 C48 1.398(7) . ? C44 C45 1.406(7) . ? C44 H44 0.9500 . ? C45 C46 1.393(8) . ? C45 H45 0.9500 . ? C46 C47 1.374(7) . ? C46 C49 1.492(7) . ? C47 C48 1.388(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O50 1.211(6) . ? C49 O51 1.325(7) . ? C52 C53 1.393(6) . ? C52 C57 1.394(7) . ? C53 C54 1.391(7) . ? C53 H53 0.9500 . ? C54 C55 1.383(7) . ? C54 H54 0.9500 . ? C55 C56 1.394(6) . ? C55 C58 1.497(6) . ? C56 C57 1.377(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O59 1.257(5) . ? C58 O60 1.263(5) . ? O60 Yb 2.190(3) 1_666 ? O62 C63 1.242(8) . ? C63 N64A 1.257(15) . ? C63 N64B 1.455(15) . ? C63 H63 0.9500 . ? N64A C65A 1.453(19) . ? N64A C66A 1.51(2) . ? C65A H65A 0.9800 . ? C65A H65B 0.9800 . ? C65A H65C 0.9800 . ? C66A H66A 0.9800 . ? C66A H66B 0.9800 . ? C66A H66C 0.9800 . ? N64B C66B 1.53(2) . ? N64B C65B 1.531(16) . ? C65B H65D 0.9800 . ? C65B H65E 0.9800 . ? C65B H65F 0.9800 . ? C66B H66D 0.9800 . ? C66B H66E 0.9800 . ? C66B H66F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O60 Yb O32 149.16(11) 1_444 1_445 ? O60 Yb O41 124.10(11) 1_444 2 ? O32 Yb O41 79.81(11) 1_445 2 ? O60 Yb O33 74.43(11) 1_444 2_665 ? O32 Yb O33 135.16(11) 1_445 2_665 ? O41 Yb O33 74.52(11) 2 2_665 ? O60 Yb O42 89.24(11) 1_444 . ? O32 Yb O42 88.78(11) 1_445 . ? O41 Yb O42 128.41(11) 2 . ? O33 Yb O42 79.58(11) 2_665 . ? O60 Yb O62 82.11(12) 1_444 . ? O32 Yb O62 85.19(12) 1_445 . ? O41 Yb O62 77.64(12) 2 . ? O33 Yb O62 123.12(12) 2_665 . ? O42 Yb O62 151.66(11) . . ? O60 Yb O61 76.14(10) 1_444 . ? O32 Yb O61 73.59(10) 1_445 . ? O41 Yb O61 144.00(11) 2 . ? O33 Yb O61 141.24(10) 2_665 . ? O42 Yb O61 75.35(11) . . ? O62 Yb O61 76.38(11) . . ? O60 Yb O41 128.24(10) 1_444 . ? O32 Yb O41 69.39(10) 1_445 . ? O41 Yb O41 81.44(11) 2 . ? O33 Yb O41 70.88(10) 2_665 . ? O42 Yb O41 47.84(9) . . ? O62 Yb O41 149.53(10) . . ? O61 Yb O41 110.39(10) . . ? O60 Yb C40 110.05(11) 1_444 . ? O32 Yb C40 76.27(12) 1_445 . ? O41 Yb C40 106.27(11) 2 . ? O33 Yb C40 76.52(12) 2_665 . ? O42 Yb C40 23.19(10) . . ? O62 Yb C40 159.83(12) . . ? O61 Yb C40 90.65(11) . . ? O41 Yb C40 24.91(10) . . ? O60 Yb C63 89.77(18) 1_444 . ? O32 Yb C63 70.67(19) 1_445 . ? O41 Yb C63 87.27(15) 2 . ? O33 Yb C63 141.99(19) 2_665 . ? O42 Yb C63 135.61(17) . . ? O62 Yb C63 18.88(19) . . ? O61 Yb C63 61.40(16) . . ? O41 Yb C63 139.79(18) . . ? C40 Yb C63 141.33(19) . . ? O60 Yb Yb 141.10(8) 1_444 2 ? O32 Yb Yb 68.78(8) 1_445 2 ? O41 Yb Yb 47.22(9) 2 2 ? O33 Yb Yb 66.74(7) 2_665 2 ? O42 Yb Yb 81.67(7) . 2 ? O62 Yb Yb 121.20(8) . 2 ? O61 Yb Yb 135.94(8) . 2 ? O41 Yb Yb 34.22(6) . 2 ? C40 Yb Yb 59.08(8) . 2 ? C63 Yb Yb 122.66(14) . 2 ? N21 C1 C20 125.6(4) . . ? N21 C1 C2 108.4(4) . . ? C20 C1 C2 126.0(4) . . ? C3 C2 C1 107.1(5) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 107.7(4) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? N21 C4 C5 125.6(4) . . ? N21 C4 C3 108.6(4) . . ? C5 C4 C3 125.7(4) . . ? C6 C5 C4 125.5(4) . . ? C6 C5 C25 116.7(4) . . ? C4 C5 C25 117.7(4) . . ? N22 C6 C5 124.9(4) . . ? N22 C6 C7 109.4(4) . . ? C5 C6 C7 125.5(4) . . ? C8 C7 C6 107.8(4) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 106.9(4) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N22 C9 C10 125.8(4) . . ? N22 C9 C8 109.2(4) . . ? C10 C9 C8 124.6(4) . . ? C11 C10 C9 125.8(4) . . ? C11 C10 C34 117.2(4) . . ? C9 C10 C34 116.9(4) . . ? N23 C11 C10 125.5(4) . . ? N23 C11 C12 107.9(4) . . ? C10 C11 C12 126.4(4) . . ? C13 C12 C11 108.0(4) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? C12 C13 C14 107.0(4) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N23 C14 C15 124.9(4) . . ? N23 C14 C13 108.4(4) . . ? C15 C14 C13 126.6(4) . . ? C16 C15 C14 125.3(4) . . ? C16 C15 C43 117.3(4) . . ? C14 C15 C43 117.4(4) . . ? C15 C16 N24 125.6(4) . . ? C15 C16 C17 126.4(4) . . ? N24 C16 C17 107.9(4) . . ? C18 C17 C16 107.5(4) . . ? C18 C17 H17 126.2 . . ? C16 C17 H17 126.2 . . ? C17 C18 C19 108.0(4) . . ? C17 C18 H18 126.0 . . ? C19 C18 H18 126.0 . . ? N24 C19 C20 126.2(4) . . ? N24 C19 C18 108.8(4) . . ? C20 C19 C18 124.9(4) . . ? C19 C20 C1 124.7(4) . . ? C19 C20 C52 116.9(4) . . ? C1 C20 C52 118.4(4) . . ? C1 N21 C4 108.1(4) . . ? C1 N21 H21 126.0 . . ? C4 N21 H21 126.0 . . ? C9 N22 C6 106.6(4) . . ? C14 N23 C11 108.5(4) . . ? C14 N23 H23 125.8 . . ? C11 N23 H23 125.8 . . ? C19 N24 C16 107.6(4) . . ? C30 C25 C26 118.9(4) . . ? C30 C25 C5 121.2(4) . . ? C26 C25 C5 119.9(4) . . ? C27 C26 C25 120.5(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 119.8(4) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 119.2(4) . . ? C27 C28 C31 120.1(4) . . ? C29 C28 C31 120.6(4) . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 121.1(4) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.4 . . ? O33 C31 O32 125.2(4) . . ? O33 C31 C28 117.5(4) . . ? O32 C31 C28 117.2(4) . . ? C31 O32 Yb 137.6(3) . 1_665 ? C31 O33 Yb 140.2(3) . 2_665 ? C39 C34 C35 118.4(4) . . ? C39 C34 C10 122.5(4) . . ? C35 C34 C10 119.0(4) . . ? C36 C35 C34 120.5(4) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 121.2(4) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 118.5(4) . . ? C36 C37 C40 119.5(4) . . ? C38 C37 C40 121.9(4) . . ? C39 C38 C37 120.7(4) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C34 120.7(5) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? O42 C40 O41 121.2(4) . . ? O42 C40 C37 119.8(3) . . ? O41 C40 C37 119.0(4) . . ? O42 C40 Yb 46.6(2) . . ? O41 C40 Yb 75.5(2) . . ? C37 C40 Yb 162.5(3) . . ? C40 O41 Yb 175.4(3) . 2 ? C40 O41 Yb 79.6(3) . . ? Yb O41 Yb 98.56(11) 2 . ? C40 O42 Yb 110.2(2) . . ? C44 C43 C48 119.0(4) . . ? C44 C43 C15 120.3(4) . . ? C48 C43 C15 120.7(4) . . ? C43 C44 C45 119.5(5) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 120.6(5) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C47 C46 C45 119.6(5) . . ? C47 C46 C49 122.1(5) . . ? C45 C46 C49 118.3(5) . . ? C46 C47 C48 120.3(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 120.9(5) . . ? C47 C48 H48 119.5 . . ? C43 C48 H48 119.5 . . ? O50 C49 O51 123.2(5) . . ? O50 C49 C46 123.1(5) . . ? O51 C49 C46 113.7(4) . . ? C53 C52 C57 118.2(4) . . ? C53 C52 C20 122.7(4) . . ? C57 C52 C20 119.0(4) . . ? C52 C53 C54 120.8(4) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 119.0(4) . . ? C54 C55 C58 120.9(4) . . ? C56 C55 C58 120.0(4) . . ? C57 C56 C55 120.6(4) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C52 120.9(4) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.5 . . ? O59 C58 O60 122.5(4) . . ? O59 C58 C55 120.4(4) . . ? O60 C58 C55 117.1(4) . . ? C58 O60 Yb 153.8(3) . 1_666 ? C63 O62 Yb 123.8(5) . . ? O62 C63 N64A 131.8(10) . . ? O62 C63 N64B 113.1(9) . . ? N64A C63 N64B 31.8(7) . . ? O62 C63 Yb 37.3(3) . . ? N64A C63 Yb 160.8(8) . . ? N64B C63 Yb 149.9(7) . . ? O62 C63 H63 114.1 . . ? N64A C63 H63 114.1 . . ? N64B C63 H63 124.0 . . ? Yb C63 H63 79.5 . . ? C63 N64A C65A 114.9(13) . . ? C63 N64A C66A 126.2(15) . . ? C65A N64A C66A 118.9(15) . . ? C63 N64B C66B 112.4(11) . . ? C63 N64B C65B 123.6(10) . . ? C66B N64B C65B 123.9(13) . . ? N64B C65B H65D 109.5 . . ? N64B C65B H65E 109.5 . . ? H65D C65B H65E 109.5 . . ? N64B C65B H65F 109.5 . . ? H65D C65B H65F 109.5 . . ? H65E C65B H65F 109.5 . . ? N64B C66B H66D 109.4 . . ? N64B C66B H66E 109.4 . . ? H66D C66B H66E 109.5 . . ? N64B C66B H66F 109.5 . . ? H66D C66B H66F 109.5 . . ? H66E C66B H66F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 2.318 _refine_diff_density_min -2.252 _refine_diff_density_rms 0.163 #======================END========================== data_Compound-10 _database_code_depnum_ccdc_archive 'CCDC 627705' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H31 Er N4 O10' _chemical_formula_sum 'C48 H31 Er N4 O10' _chemical_formula_weight 991.03 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' Er Er -0.2586 4.9576 '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 8.8318(2) _cell_length_b 15.8540(3) _cell_length_c 19.1824(5) _cell_angle_alpha 99.6993(9) _cell_angle_beta 96.4107(9) _cell_angle_gamma 101.9196(16) _cell_volume 2560.39(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9456 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.26 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 1.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4848 _exptl_absorpt_correction_T_max 0.8489 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28212 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.26 _reflns_number_total 12209 _reflns_number_gt 9248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The results below reflect crystallographic refinement after applying the Squeeze procedure (Spek, 2003), to subtract the contribution of the severely disordered solvent which could not be modeled by discrete atoms from the diffraction data. Conventional refinement of the same structural model based on the original diffraction data converged at R1=0.075. ; _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^)+(0.0768P)^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 12209 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.022 _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 Er Er 0.16778(2) -0.056046(13) -0.028978(11) 0.02215(8) Uani 1 1 d . . . C1 C -0.3965(6) -0.6036(3) 0.4846(3) 0.0281(10) Uani 1 1 d . . . C2 C -0.5238(6) -0.6787(3) 0.4570(3) 0.0332(11) Uani 1 1 d . . . H2 H -0.5776 -0.7171 0.4839 0.040 Uiso 1 1 calc R . . C3 C -0.5528(6) -0.6844(3) 0.3846(3) 0.0314(11) Uani 1 1 d . . . H3 H -0.6282 -0.7290 0.3518 0.038 Uiso 1 1 calc R . . C4 C -0.4502(5) -0.6116(3) 0.3668(3) 0.0255(10) Uani 1 1 d . . . C5 C -0.4353(5) -0.5961(3) 0.2986(3) 0.0263(10) Uani 1 1 d . . . C6 C -0.3418(5) -0.5199(3) 0.2818(3) 0.0271(10) Uani 1 1 d . . . C7 C -0.3412(6) -0.5013(3) 0.2113(3) 0.0327(11) Uani 1 1 d . . . H7 H -0.3941 -0.5394 0.1679 0.039 Uiso 1 1 calc R . . C8 C -0.2510(6) -0.4193(3) 0.2181(3) 0.0306(11) Uani 1 1 d . . . H8 H -0.2296 -0.3888 0.1805 0.037 Uiso 1 1 calc R . . C9 C -0.1936(5) -0.3870(3) 0.2931(2) 0.0243(9) Uani 1 1 d . . . C10 C -0.1051(5) -0.3015(3) 0.3232(2) 0.0247(9) Uani 1 1 d . . . C11 C -0.0522(6) -0.2693(3) 0.3959(3) 0.0273(10) Uani 1 1 d . . . C12 C 0.0338(6) -0.1813(3) 0.4274(3) 0.0315(11) Uani 1 1 d . . . H12 H 0.0605 -0.1344 0.4027 0.038 Uiso 1 1 calc R . . C13 C 0.0700(6) -0.1773(3) 0.4987(3) 0.0348(11) Uani 1 1 d . . . H13 H 0.1256 -0.1270 0.5332 0.042 Uiso 1 1 calc R . . C14 C 0.0088(6) -0.2632(3) 0.5123(2) 0.0284(10) Uani 1 1 d . . . C15 C 0.0264(5) -0.2887(3) 0.5786(2) 0.0260(10) Uani 1 1 d . . . C16 C -0.0420(6) -0.3724(3) 0.5910(3) 0.0269(10) Uani 1 1 d . . . C17 C -0.0055(6) -0.4031(3) 0.6560(3) 0.0313(11) Uani 1 1 d . . . H17 H 0.0707 -0.3720 0.6959 0.038 Uiso 1 1 calc R . . C18 C -0.0978(6) -0.4834(3) 0.6504(3) 0.0327(11) Uani 1 1 d . . . H18 H -0.0988 -0.5198 0.6850 0.039 Uiso 1 1 calc R . . C19 C -0.1965(6) -0.5037(3) 0.5806(2) 0.0269(10) Uani 1 1 d . . . C20 C -0.3165(6) -0.5797(3) 0.5547(3) 0.0284(10) Uani 1 1 d . . . N21 N -0.3585(5) -0.5626(2) 0.4292(2) 0.0268(8) Uani 1 1 d . . . H21 H -0.2875 -0.5135 0.4329 0.032 Uiso 0.50 1 calc PR . . N22 N -0.2499(4) -0.4499(2) 0.3307(2) 0.0246(8) Uani 1 1 d . . . H22 H -0.2307 -0.4461 0.3772 0.030 Uiso 0.50 1 calc PR . . N23 N -0.0671(4) -0.3175(2) 0.4489(2) 0.0256(8) Uani 1 1 d . . . H23 H -0.1163 -0.3730 0.4433 0.031 Uiso 0.50 1 calc PR . . N24 N -0.1537(4) -0.4358(2) 0.5456(2) 0.0258(8) Uani 1 1 d . . . H24 H -0.1918 -0.4337 0.5017 0.031 Uiso 0.50 1 calc PR . . C25 C -0.5216(5) -0.6654(3) 0.2362(3) 0.0268(10) Uani 1 1 d . . . C26 C -0.6857(6) -0.6870(3) 0.2194(3) 0.0316(11) Uani 1 1 d . . . H26 H -0.7451 -0.6542 0.2468 0.038 Uiso 1 1 calc R . . C27 C -0.7616(5) -0.7548(3) 0.1640(3) 0.0267(10) Uani 1 1 d . . . H27 H -0.8727 -0.7689 0.1536 0.032 Uiso 1 1 calc R . . C28 C -0.6754(5) -0.8027(3) 0.1230(2) 0.0239(9) Uani 1 1 d . . . C29 C -0.5124(5) -0.7805(3) 0.1378(2) 0.0256(10) Uani 1 1 d . . . H29 H -0.4533 -0.8120 0.1092 0.031 Uiso 1 1 calc R . . C30 C -0.4366(5) -0.7131(3) 0.1936(3) 0.0292(10) Uani 1 1 d . . . H30 H -0.3255 -0.6988 0.2034 0.035 Uiso 1 1 calc R . . C31 C -0.7546(5) -0.8808(3) 0.0659(3) 0.0248(9) Uani 1 1 d . . . O32 O -0.9006(3) -0.9056(2) 0.05449(17) 0.0274(7) Uani 1 1 d . . . O33 O -0.6714(3) -0.9221(2) 0.03051(17) 0.0264(7) Uani 1 1 d . . . C34 C -0.0706(5) -0.2403(3) 0.2722(2) 0.0252(10) Uani 1 1 d . . . C35 C 0.0396(6) -0.2494(3) 0.2270(3) 0.0290(10) Uani 1 1 d . . . H35 H 0.0975 -0.2932 0.2299 0.035 Uiso 1 1 calc R . . C36 C 0.0664(5) -0.1956(3) 0.1778(3) 0.0282(10) Uani 1 1 d . . . H36 H 0.1442 -0.2016 0.1480 0.034 Uiso 1 1 calc R . . C37 C -0.0211(5) -0.1322(3) 0.1718(2) 0.0245(9) Uani 1 1 d . . . C38 C -0.1298(6) -0.1217(3) 0.2177(3) 0.0336(11) Uani 1 1 d . . . H38 H -0.1888 -0.0784 0.2143 0.040 Uiso 1 1 calc R . . C39 C -0.1527(6) -0.1743(3) 0.2685(3) 0.0333(11) Uani 1 1 d . . . H39 H -0.2244 -0.1652 0.3009 0.040 Uiso 1 1 calc R . . C40 C -0.0036(5) -0.0797(3) 0.1142(2) 0.0243(9) Uani 1 1 d . . . O41 O -0.0996(4) -0.0325(2) 0.10494(17) 0.0277(7) Uani 1 1 d . . . O42 O 0.1058(3) -0.0863(2) 0.07769(17) 0.0269(7) Uani 1 1 d . . . C43 C 0.1168(6) -0.2226(3) 0.6417(2) 0.0271(10) Uani 1 1 d . . . C44 C 0.2748(6) -0.1819(3) 0.6451(3) 0.0321(11) Uani 1 1 d . . . H44 H 0.3266 -0.1953 0.6052 0.039 Uiso 1 1 calc R . . C45 C 0.3568(6) -0.1225(3) 0.7054(3) 0.0312(11) Uani 1 1 d . . . H45 H 0.4631 -0.0945 0.7060 0.037 Uiso 1 1 calc R . . C46 C 0.2853(5) -0.1034(3) 0.7648(2) 0.0244(9) Uani 1 1 d . . . C47 C 0.1281(5) -0.1431(3) 0.7617(3) 0.0331(11) Uani 1 1 d . . . H47 H 0.0772 -0.1306 0.8021 0.040 Uiso 1 1 calc R . . C48 C 0.0454(6) -0.2004(4) 0.7008(3) 0.0371(12) Uani 1 1 d . . . H48 H -0.0628 -0.2251 0.6993 0.045 Uiso 1 1 calc R . . C49 C 0.3750(5) -0.0455(3) 0.8321(2) 0.0241(9) Uani 1 1 d . . . O50 O 0.3295(3) -0.0595(2) 0.89080(16) 0.0242(7) Uani 1 1 d . . . O51 O 0.4944(4) 0.0130(2) 0.83080(17) 0.0309(7) Uani 1 1 d . . . C52 C -0.3577(6) -0.6402(3) 0.6052(3) 0.0287(10) Uani 1 1 d . . . C53 C -0.3972(6) -0.6086(3) 0.6726(3) 0.0334(11) Uani 1 1 d . . . H53 H -0.4037 -0.5490 0.6850 0.040 Uiso 1 1 calc R . . C54 C -0.4260(6) -0.6631(3) 0.7200(3) 0.0362(12) Uani 1 1 d . . . H54 H -0.4500 -0.6406 0.7656 0.043 Uiso 1 1 calc R . . C55 C -0.4206(6) -0.7512(3) 0.7026(3) 0.0319(11) Uani 1 1 d . . . C56 C -0.3855(6) -0.7832(3) 0.6358(3) 0.0348(11) Uani 1 1 d . . . H56 H -0.3833 -0.8434 0.6228 0.042 Uiso 1 1 calc R . . C57 C -0.3541(6) -0.7280(3) 0.5883(3) 0.0353(12) Uani 1 1 d . . . H57 H -0.3294 -0.7508 0.5430 0.042 Uiso 1 1 calc R . . C58 C -0.4440(6) -0.8063(3) 0.7582(3) 0.0317(11) Uani 1 1 d . . . O59 O -0.4389(5) -0.7765(2) 0.8205(2) 0.0422(9) Uani 1 1 d . . . O60 O -0.4699(5) -0.8922(2) 0.73210(19) 0.0393(9) Uani 1 1 d . . . H60 H -0.4893 -0.9201 0.7648 0.059 Uiso 1 1 calc R . . O61 O 0.3885(3) -0.0927(2) 0.02939(17) 0.0255(7) Uani 1 1 d . . . H61A H 0.4185 -0.0568 0.0779 0.038 Uiso 1 1 d R . . H61B H 0.4763 -0.0814 0.0024 0.038 Uiso 1 1 d R . . O62 O 0.1212(4) -0.2093(2) -0.0659(2) 0.0339(8) Uani 1 1 d . . . H62A H 0.1704 -0.2226 -0.1075 0.051 Uiso 1 1 d R . . H62B H 0.1647 -0.2340 -0.0273 0.051 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er 0.01849(11) 0.02765(12) 0.01951(12) 0.00492(8) 0.00277(7) 0.00336(8) C1 0.034(3) 0.024(2) 0.027(3) 0.005(2) 0.006(2) 0.007(2) C2 0.039(3) 0.032(3) 0.028(3) 0.011(2) 0.008(2) 0.000(2) C3 0.033(3) 0.024(2) 0.033(3) 0.004(2) 0.001(2) 0.000(2) C4 0.023(2) 0.022(2) 0.028(3) 0.0010(19) -0.0011(19) 0.0039(19) C5 0.029(2) 0.023(2) 0.026(3) 0.0044(19) 0.0035(19) 0.0054(19) C6 0.026(2) 0.025(2) 0.027(3) 0.0001(19) -0.0008(19) 0.006(2) C7 0.038(3) 0.031(3) 0.024(3) 0.001(2) -0.002(2) 0.002(2) C8 0.034(3) 0.032(3) 0.023(3) 0.006(2) -0.001(2) 0.002(2) C9 0.027(2) 0.028(2) 0.019(2) 0.0038(18) 0.0025(18) 0.0095(19) C10 0.029(2) 0.025(2) 0.023(2) 0.0081(19) 0.0089(19) 0.0063(19) C11 0.032(2) 0.027(2) 0.022(2) 0.0065(19) 0.003(2) 0.004(2) C12 0.045(3) 0.021(2) 0.029(3) 0.008(2) 0.007(2) 0.004(2) C13 0.048(3) 0.026(2) 0.028(3) 0.005(2) 0.005(2) 0.004(2) C14 0.035(3) 0.027(2) 0.020(2) 0.0014(19) 0.002(2) 0.003(2) C15 0.028(2) 0.025(2) 0.021(2) 0.0015(19) -0.0013(19) 0.0024(19) C16 0.030(2) 0.024(2) 0.026(3) 0.004(2) 0.004(2) 0.006(2) C17 0.034(3) 0.032(3) 0.024(3) 0.004(2) -0.002(2) 0.003(2) C18 0.033(3) 0.039(3) 0.028(3) 0.014(2) 0.003(2) 0.006(2) C19 0.034(3) 0.026(2) 0.022(2) 0.0063(19) 0.009(2) 0.007(2) C20 0.034(3) 0.026(2) 0.029(3) 0.007(2) 0.013(2) 0.009(2) N21 0.030(2) 0.025(2) 0.023(2) 0.0024(16) 0.0031(17) 0.0028(17) N22 0.027(2) 0.0215(19) 0.022(2) 0.0030(16) -0.0016(16) 0.0033(16) N23 0.031(2) 0.0241(19) 0.019(2) 0.0038(16) 0.0004(16) 0.0019(17) N24 0.031(2) 0.0215(19) 0.027(2) 0.0070(17) 0.0080(17) 0.0060(17) C25 0.027(2) 0.021(2) 0.029(3) 0.0064(19) 0.002(2) -0.0021(19) C26 0.033(3) 0.029(2) 0.033(3) 0.003(2) 0.007(2) 0.007(2) C27 0.020(2) 0.029(2) 0.028(3) 0.002(2) 0.0036(19) 0.0005(19) C28 0.026(2) 0.022(2) 0.022(2) 0.0049(18) 0.0019(18) 0.0014(18) C29 0.025(2) 0.025(2) 0.025(2) -0.0019(19) 0.0016(19) 0.0068(19) C30 0.022(2) 0.030(2) 0.035(3) 0.007(2) 0.004(2) 0.004(2) C31 0.021(2) 0.026(2) 0.027(2) 0.0065(19) 0.0055(18) 0.0016(19) O32 0.0190(16) 0.0311(17) 0.0280(18) 0.0033(14) 0.0009(13) 0.0000(13) O33 0.0182(15) 0.0298(17) 0.0260(18) 0.0019(14) 0.0011(13) -0.0020(13) C34 0.029(2) 0.025(2) 0.023(2) 0.0092(19) 0.0060(19) 0.0054(19) C35 0.030(2) 0.029(2) 0.030(3) 0.008(2) 0.004(2) 0.010(2) C36 0.026(2) 0.034(3) 0.027(3) 0.006(2) 0.0083(19) 0.010(2) C37 0.024(2) 0.028(2) 0.022(2) 0.0082(19) 0.0017(18) 0.0045(19) C38 0.044(3) 0.036(3) 0.032(3) 0.015(2) 0.014(2) 0.024(2) C39 0.037(3) 0.042(3) 0.027(3) 0.010(2) 0.013(2) 0.016(2) C40 0.022(2) 0.033(2) 0.018(2) 0.0054(19) 0.0025(18) 0.007(2) O41 0.0263(16) 0.0318(17) 0.0274(18) 0.0102(14) 0.0057(14) 0.0075(14) O42 0.0209(15) 0.0391(18) 0.0235(17) 0.0114(14) 0.0043(13) 0.0084(14) C43 0.032(2) 0.029(2) 0.017(2) 0.0055(19) -0.0010(19) 0.001(2) C44 0.030(3) 0.040(3) 0.024(3) 0.003(2) 0.008(2) 0.004(2) C45 0.028(2) 0.040(3) 0.023(3) 0.007(2) 0.005(2) -0.001(2) C46 0.026(2) 0.028(2) 0.019(2) 0.0051(19) 0.0014(18) 0.0072(19) C47 0.024(2) 0.048(3) 0.022(3) 0.000(2) 0.0045(19) -0.001(2) C48 0.026(2) 0.050(3) 0.028(3) 0.000(2) 0.005(2) -0.002(2) C49 0.024(2) 0.026(2) 0.025(2) 0.0055(19) 0.0057(18) 0.011(2) O50 0.0220(15) 0.0300(17) 0.0226(17) 0.0080(13) 0.0057(13) 0.0071(13) O51 0.0274(17) 0.0405(19) 0.0198(17) 0.0077(15) 0.0010(13) -0.0036(15) C52 0.035(3) 0.027(2) 0.025(3) 0.005(2) 0.004(2) 0.008(2) C53 0.036(3) 0.030(3) 0.036(3) 0.003(2) 0.013(2) 0.010(2) C54 0.042(3) 0.039(3) 0.030(3) 0.008(2) 0.019(2) 0.008(2) C55 0.034(3) 0.032(3) 0.029(3) 0.006(2) 0.009(2) 0.004(2) C56 0.046(3) 0.026(2) 0.034(3) 0.005(2) 0.011(2) 0.010(2) C57 0.048(3) 0.029(3) 0.031(3) 0.005(2) 0.014(2) 0.009(2) C58 0.032(3) 0.032(3) 0.031(3) 0.009(2) 0.011(2) 0.003(2) O59 0.053(2) 0.043(2) 0.032(2) 0.0100(17) 0.0143(18) 0.0085(19) O60 0.054(2) 0.0343(19) 0.029(2) 0.0133(16) 0.0118(18) 0.0017(18) O61 0.0209(15) 0.0323(17) 0.0232(17) 0.0070(14) 0.0038(13) 0.0043(13) O62 0.0299(18) 0.0297(18) 0.042(2) 0.0071(16) 0.0086(16) 0.0059(15) _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 Er O50 2.215(3) 1_554 ? Er O42 2.278(3) . ? Er O32 2.286(3) 2_445 ? Er O41 2.302(3) 2 ? Er O33 2.324(3) 1_665 ? Er O62 2.349(3) . ? Er O61 2.365(3) . ? Er O32 2.854(3) 1_665 ? Er C31 2.955(5) 1_665 ? Er Er 3.9271(4) 2 ? C1 N21 1.374(6) . ? C1 C20 1.398(7) . ? C1 C2 1.437(7) . ? C2 C3 1.369(7) . ? C2 H2 0.9500 . ? C3 C4 1.428(7) . ? C3 H3 0.9500 . ? C4 N21 1.380(6) . ? C4 C5 1.386(7) . ? C5 C6 1.423(7) . ? C5 C25 1.493(6) . ? C6 N22 1.369(6) . ? C6 C7 1.433(7) . ? C7 C8 1.355(7) . ? C7 H7 0.9500 . ? C8 C9 1.438(6) . ? C8 H8 0.9500 . ? C9 N22 1.371(6) . ? C9 C10 1.407(6) . ? C10 C11 1.393(7) . ? C10 C34 1.503(6) . ? C11 N23 1.372(6) . ? C11 C12 1.436(7) . ? C12 C13 1.357(7) . ? C12 H12 0.9500 . ? C13 C14 1.436(7) . ? C13 H13 0.9500 . ? C14 N23 1.379(6) . ? C14 C15 1.400(6) . ? C15 C16 1.412(6) . ? C15 C43 1.487(6) . ? C16 N24 1.359(6) . ? C16 C17 1.439(7) . ? C17 C18 1.343(7) . ? C17 H17 0.9500 . ? C18 C19 1.461(7) . ? C18 H18 0.9500 . ? C19 N24 1.373(6) . ? C19 C20 1.404(7) . ? C20 C52 1.497(7) . ? N21 H21 0.8800 . ? N22 H22 0.8800 . ? N23 H23 0.8800 . ? N24 H24 0.8800 . ? C25 C30 1.402(7) . ? C25 C26 1.405(7) . ? C26 C27 1.376(7) . ? C26 H26 0.9500 . ? C27 C28 1.396(6) . ? C27 H27 0.9500 . ? C28 C29 1.394(6) . ? C28 C31 1.495(6) . ? C29 C30 1.377(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O33 1.261(5) . ? C31 O32 1.251(5) . ? C31 Er 2.954(5) 1_445 ? O32 Er 2.286(3) 2_445 ? O32 Er 2.853(3) 1_445 ? O33 Er 2.324(3) 1_445 ? C34 C35 1.386(7) . ? C34 C39 1.397(6) . ? C35 C36 1.384(7) . ? C35 H35 0.9500 . ? C36 C37 1.400(6) . ? C36 H36 0.9500 . ? C37 C38 1.389(6) . ? C37 C40 1.493(6) . ? C38 C39 1.391(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O41 1.258(5) . ? C40 O42 1.266(5) . ? O41 Er 2.302(3) 2 ? C43 C48 1.387(7) . ? C43 C44 1.401(7) . ? C44 C45 1.383(7) . ? C44 H44 0.9500 . ? C45 C46 1.382(6) . ? C45 H45 0.9500 . ? C46 C47 1.391(7) . ? C46 C49 1.486(6) . ? C47 C48 1.379(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O51 1.258(6) . ? C49 O50 1.276(5) . ? O50 Er 2.215(3) 1_556 ? C52 C57 1.383(7) . ? C52 C53 1.414(7) . ? C53 C54 1.366(7) . ? C53 H53 0.9500 . ? C54 C55 1.391(7) . ? C54 H54 0.9500 . ? C55 C56 1.390(7) . ? C55 C58 1.494(7) . ? C56 C57 1.378(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O59 1.202(6) . ? C58 O60 1.331(6) . ? O60 H60 0.8400 . ? O61 H61A 0.9827 . ? O61 H61B 0.9827 . ? O62 H62A 0.9635 . ? O62 H62B 0.9718 . ? 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 O50 Er O42 148.35(11) 1_554 . ? O50 Er O32 125.23(11) 1_554 2_445 ? O42 Er O32 79.39(11) . 2_445 ? O50 Er O41 74.48(11) 1_554 2 ? O42 Er O41 136.12(11) . 2 ? O32 Er O41 74.14(11) 2_445 2 ? O50 Er O33 88.10(11) 1_554 1_665 ? O42 Er O33 89.72(11) . 1_665 ? O32 Er O33 128.64(11) 2_445 1_665 ? O41 Er O33 80.61(11) 2 1_665 ? O50 Er O62 81.68(12) 1_554 . ? O42 Er O62 85.10(12) . . ? O32 Er O62 78.43(11) 2_445 . ? O41 Er O62 121.91(12) 2 . ? O33 Er O62 150.94(11) 1_665 . ? O50 Er O61 75.60(11) 1_554 . ? O42 Er O61 73.34(10) . . ? O32 Er O61 143.83(11) 2_445 . ? O41 Er O61 141.74(11) 2 . ? O33 Er O61 75.10(11) 1_665 . ? O62 Er O61 76.01(11) . . ? O50 Er O32 128.01(10) 1_554 1_665 ? O42 Er O32 70.08(10) . 1_665 ? O32 Er O32 80.95(11) 2_445 1_665 ? O41 Er O32 71.66(10) 2 1_665 ? O33 Er O32 48.55(9) 1_665 1_665 ? O62 Er O32 150.21(11) . 1_665 ? O61 Er O32 110.57(10) . 1_665 ? O50 Er C31 109.81(12) 1_554 1_665 ? O42 Er C31 76.77(12) . 1_665 ? O32 Er C31 105.69(12) 2_445 1_665 ? O41 Er C31 77.54(12) 2 1_665 ? O33 Er C31 24.05(11) 1_665 1_665 ? O62 Er C31 160.13(13) . 1_665 ? O61 Er C31 90.86(11) . 1_665 ? O32 Er C31 24.79(10) 1_665 1_665 ? O50 Er Er 141.57(7) 1_554 2 ? O42 Er Er 69.22(7) . 2 ? O32 Er Er 45.85(8) 2_445 2 ? O41 Er Er 67.19(8) 2 2 ? O33 Er Er 83.26(7) 1_665 2 ? O62 Er Er 120.92(8) . 2 ? O61 Er Er 136.49(8) . 2 ? O32 Er Er 35.10(6) 1_665 2 ? C31 Er Er 59.85(8) 1_665 2 ? N21 C1 C20 125.4(4) . . ? N21 C1 C2 108.4(4) . . ? C20 C1 C2 126.1(4) . . ? C3 C2 C1 106.9(4) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 108.3(4) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? N21 C4 C5 125.4(4) . . ? N21 C4 C3 107.9(4) . . ? C5 C4 C3 126.5(4) . . ? C4 C5 C6 125.9(4) . . ? C4 C5 C25 118.2(4) . . ? C6 C5 C25 115.9(4) . . ? N22 C6 C5 125.4(4) . . ? N22 C6 C7 109.7(4) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 107.0(4) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 107.3(4) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N22 C9 C10 125.6(4) . . ? N22 C9 C8 109.2(4) . . ? C10 C9 C8 125.0(4) . . ? C11 C10 C9 125.3(4) . . ? C11 C10 C34 118.3(4) . . ? C9 C10 C34 116.4(4) . . ? N23 C11 C10 125.5(4) . . ? N23 C11 C12 108.8(4) . . ? C10 C11 C12 125.6(4) . . ? C13 C12 C11 107.6(4) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 107.3(4) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N23 C14 C15 125.3(4) . . ? N23 C14 C13 108.8(4) . . ? C15 C14 C13 125.9(4) . . ? C14 C15 C16 124.5(4) . . ? C14 C15 C43 118.6(4) . . ? C16 C15 C43 116.8(4) . . ? N24 C16 C15 126.5(4) . . ? N24 C16 C17 109.1(4) . . ? C15 C16 C17 124.5(4) . . ? C18 C17 C16 108.2(4) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? C17 C18 C19 106.4(4) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? N24 C19 C20 126.2(4) . . ? N24 C19 C18 108.6(4) . . ? C20 C19 C18 125.3(4) . . ? C1 C20 C19 124.5(4) . . ? C1 C20 C52 118.0(4) . . ? C19 C20 C52 117.5(4) . . ? C1 N21 C4 108.5(4) . . ? C1 N21 H21 125.8 . . ? C4 N21 H21 125.8 . . ? C6 N22 C9 106.9(4) . . ? C6 N22 H22 126.6 . . ? C9 N22 H22 126.6 . . ? C11 N23 C14 107.5(4) . . ? C11 N23 H23 126.2 . . ? C14 N23 H23 126.2 . . ? C16 N24 C19 107.6(4) . . ? C16 N24 H24 126.2 . . ? C19 N24 H24 126.2 . . ? C30 C25 C26 118.3(4) . . ? C30 C25 C5 119.0(4) . . ? C26 C25 C5 122.7(4) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.6(4) . . ? C29 C28 C31 119.1(4) . . ? C27 C28 C31 121.2(4) . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 120.7(4) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? O33 C31 O32 120.7(4) . . ? O33 C31 C28 118.8(4) . . ? O32 C31 C28 120.5(4) . . ? O33 C31 Er 48.7(2) . 1_445 ? O32 C31 Er 73.1(3) . 1_445 ? C28 C31 Er 162.7(3) . 1_445 ? C31 O32 Er 176.2(3) . 2_445 ? C31 O32 Er 82.1(3) . 1_445 ? Er O32 Er 99.05(11) 2_445 1_445 ? C31 O33 Er 107.2(3) . 1_445 ? C35 C34 C39 119.0(4) . . ? C35 C34 C10 121.0(4) . . ? C39 C34 C10 120.0(4) . . ? C36 C35 C34 121.0(4) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 120.0(4) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.3(4) . . ? C38 C37 C40 120.4(4) . . ? C36 C37 C40 120.3(4) . . ? C37 C38 C39 120.4(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.3(4) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? O41 C40 O42 124.5(4) . . ? O41 C40 C37 117.7(4) . . ? O42 C40 C37 117.8(4) . . ? C40 O41 Er 140.5(3) . 2 ? C40 O42 Er 137.1(3) . . ? C48 C43 C44 117.5(4) . . ? C48 C43 C15 119.9(4) . . ? C44 C43 C15 122.6(4) . . ? C45 C44 C43 121.1(5) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C46 C45 C44 120.6(5) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 118.6(4) . . ? C45 C46 C49 121.3(4) . . ? C47 C46 C49 120.0(4) . . ? C48 C47 C46 120.7(5) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C43 121.3(5) . . ? C47 C48 H48 119.3 . . ? C43 C48 H48 119.3 . . ? O51 C49 O50 121.6(4) . . ? O51 C49 C46 120.7(4) . . ? O50 C49 C46 117.6(4) . . ? C49 O50 Er 153.5(3) . 1_556 ? C57 C52 C53 118.0(5) . . ? C57 C52 C20 121.2(4) . . ? C53 C52 C20 120.8(4) . . ? C54 C53 C52 120.5(5) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 120.9(5) . . ? C53 C54 H54 119.5 . . ? C55 C54 H54 119.5 . . ? C56 C55 C54 118.9(5) . . ? C56 C55 C58 122.5(5) . . ? C54 C55 C58 118.5(4) . . ? C57 C56 C55 120.3(5) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C52 121.4(5) . . ? C56 C57 H57 119.3 . . ? C52 C57 H57 119.3 . . ? O59 C58 O60 123.0(5) . . ? O59 C58 C55 123.6(5) . . ? O60 C58 C55 113.4(4) . . ? C58 O60 H60 109.5 . . ? Er O61 H61A 109.5 . . ? Er O61 H61B 109.5 . . ? H61A O61 H61B 109.3 . . ? Er O62 H62A 109.2 . . ? Er O62 H62B 109.1 . . ? H62A O62 H62B 109.9 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.924 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.142 #========================END========================== data_Compound-11 _database_code_depnum_ccdc_archive 'CCDC 627706' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H36 Er N5 O10' _chemical_formula_sum 'C51 H36 Er N5 O10' _chemical_formula_weight 1046.11 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5175(2) _cell_length_b 28.1745(6) _cell_length_c 21.4217(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.1026(7) _cell_angle_gamma 90.00 _cell_volume 5101.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9351 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 28.22 _exptl_crystal_description needles _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4829 _exptl_absorpt_correction_T_max 0.9196 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38816 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.33 _reflns_number_total 11698 _reflns_number_gt 8274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+6.2820P] 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 11698 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.023 _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 Er Er 1.29497(3) 0.058314(8) 0.006439(10) 0.01317(8) Uani 1 1 d . . . C1 C 0.6964(6) -0.05535(19) 0.5251(2) 0.0154(10) Uani 1 1 d . . . C2 C 0.6097(6) -0.0839(2) 0.5661(2) 0.0187(11) Uani 1 1 d . . . H2 H 0.5882 -0.1170 0.5626 0.022 Uiso 1 1 calc R . . C3 C 0.5663(6) -0.05414(19) 0.6102(2) 0.0187(11) Uani 1 1 d . . . H3 H 0.5071 -0.0624 0.6434 0.022 Uiso 1 1 calc R . . C4 C 0.6252(6) -0.00772(19) 0.5980(2) 0.0170(11) Uani 1 1 d . . . C5 C 0.6146(6) 0.0328(2) 0.6366(2) 0.0165(11) Uani 1 1 d . . . C6 C 0.6562(6) 0.07873(19) 0.6201(2) 0.0153(10) Uani 1 1 d . . . C7 C 0.6592(6) 0.12053(19) 0.6589(2) 0.0187(11) Uani 1 1 d . . . H7 H 0.6453 0.1213 0.7022 0.022 Uiso 1 1 calc R . . C8 C 0.6850(6) 0.1581(2) 0.6235(2) 0.0214(12) Uani 1 1 d . . . H8 H 0.6907 0.1903 0.6367 0.026 Uiso 1 1 calc R . . C9 C 0.7028(6) 0.14016(19) 0.5607(2) 0.0159(11) Uani 1 1 d . . . C10 C 0.7191(6) 0.1686(2) 0.5078(2) 0.0190(12) Uani 1 1 d . . . C11 C 0.7521(6) 0.15069(19) 0.4493(2) 0.0162(11) Uani 1 1 d . . . C12 C 0.7699(6) 0.17965(19) 0.3947(2) 0.0191(11) Uani 1 1 d . . . H12 H 0.7523 0.2129 0.3907 0.023 Uiso 1 1 calc R . . C13 C 0.8164(6) 0.15038(19) 0.3506(2) 0.0160(11) Uani 1 1 d . . . H13 H 0.8357 0.1593 0.3095 0.019 Uiso 1 1 calc R . . C14 C 0.8315(6) 0.10328(19) 0.3768(2) 0.0157(11) Uani 1 1 d . . . C15 C 0.8859(6) 0.06300(19) 0.3477(2) 0.0152(11) Uani 1 1 d . . . C16 C 0.8894(6) 0.01669(18) 0.3730(2) 0.0148(10) Uani 1 1 d . . . C17 C 0.9598(6) -0.02460(19) 0.3477(2) 0.0159(11) Uani 1 1 d . . . H17 H 1.0172 -0.0250 0.3124 0.019 Uiso 1 1 calc R . . C18 C 0.9298(6) -0.0624(2) 0.3830(2) 0.0176(11) Uani 1 1 d . . . H18 H 0.9625 -0.0942 0.3773 0.021 Uiso 1 1 calc R . . C19 C 0.8389(6) -0.04542(19) 0.4307(2) 0.0166(11) Uani 1 1 d . . . C20 C 0.7723(6) -0.07329(18) 0.4752(2) 0.0147(11) Uani 1 1 d . . . N21 N 0.6971(5) -0.00938(16) 0.54432(19) 0.0169(9) Uani 1 1 d . . . H21 H 0.7365 0.0149 0.5256 0.020 Uiso 0.50 1 calc PR . . N22 N 0.6890(5) 0.09221(16) 0.56132(19) 0.0154(9) Uani 1 1 d . . . H22 H 0.6992 0.0730 0.5296 0.018 Uiso 0.50 1 calc PR . . N23 N 0.7878(5) 0.10481(16) 0.43632(18) 0.0153(9) Uani 1 1 d . . . H23 H 0.7835 0.0804 0.4617 0.018 Uiso 0.50 1 calc PR . . N24 N 0.8212(5) 0.00297(16) 0.42461(19) 0.0170(9) Uani 1 1 d . . . H24 H 0.7744 0.0217 0.4495 0.020 Uiso 0.50 1 calc PR . . C25 C 0.5666(6) 0.02560(18) 0.7005(2) 0.0143(10) Uani 1 1 d . . . C26 C 0.4527(6) 0.05415(19) 0.7234(2) 0.0187(11) Uani 1 1 d . . . H26 H 0.3952 0.0763 0.6961 0.022 Uiso 1 1 calc R . . C27 C 0.4221(6) 0.05078(18) 0.7851(2) 0.0171(11) Uani 1 1 d . . . H27 H 0.3473 0.0714 0.8004 0.020 Uiso 1 1 calc R . . C28 C 0.5008(6) 0.01714(19) 0.8246(2) 0.0154(11) Uani 1 1 d . . . C29 C 0.6053(6) -0.0136(2) 0.8012(2) 0.0201(12) Uani 1 1 d . . . H29 H 0.6533 -0.0383 0.8270 0.024 Uiso 1 1 calc R . . C30 C 0.6403(6) -0.0085(2) 0.7403(2) 0.0212(12) Uani 1 1 d . . . H30 H 0.7165 -0.0289 0.7254 0.025 Uiso 1 1 calc R . . C31 C 0.4761(6) 0.01510(19) 0.8928(2) 0.0160(11) Uani 1 1 d . . . O32 O 0.3960(5) 0.04689(14) 0.91406(17) 0.0245(9) Uani 1 1 d . . . O33 O 0.5380(4) -0.01923(13) 0.92567(16) 0.0193(8) Uani 1 1 d . . . C34 C 0.6959(6) 0.22037(19) 0.5138(2) 0.0201(12) Uani 1 1 d . . . C35 C 0.5551(6) 0.2411(2) 0.4813(3) 0.0225(12) Uani 1 1 d . . . H35 H 0.4807 0.2224 0.4554 0.027 Uiso 1 1 calc R . . C36 C 0.5308(6) 0.2895(2) 0.4888(3) 0.0240(12) Uani 1 1 d . . . H36 H 0.4378 0.3039 0.4680 0.029 Uiso 1 1 calc R . . C37 C 0.6390(6) 0.3171(2) 0.5260(2) 0.0208(12) Uani 1 1 d . . . C38 C 0.7741(6) 0.2972(2) 0.5558(3) 0.0255(13) Uani 1 1 d . . . H38 H 0.8504 0.3165 0.5799 0.031 Uiso 1 1 calc R . . C39 C 0.8001(7) 0.2488(2) 0.5508(3) 0.0217(12) Uani 1 1 d . . . H39 H 0.8918 0.2350 0.5735 0.026 Uiso 1 1 calc R . . C40 C 0.6081(7) 0.3700(2) 0.5301(3) 0.0252(13) Uani 1 1 d . . . O41 O 0.7227(5) 0.39603(14) 0.5498(2) 0.0335(10) Uani 1 1 d . . . O42 O 0.4690(4) 0.38404(14) 0.51210(18) 0.0256(9) Uani 1 1 d . . . C43 C 0.9378(6) 0.06925(18) 0.2842(2) 0.0166(11) Uani 1 1 d . . . C44 C 0.8745(6) 0.0411(2) 0.2344(2) 0.0173(11) Uani 1 1 d . . . H44 H 0.7938 0.0190 0.2408 0.021 Uiso 1 1 calc R . . C45 C 0.9252(6) 0.04415(19) 0.1755(2) 0.0170(11) Uani 1 1 d . . . H45 H 0.8814 0.0239 0.1425 0.020 Uiso 1 1 calc R . . C46 C 1.0414(6) 0.07729(19) 0.1651(2) 0.0149(10) Uani 1 1 d . . . C47 C 1.1038(6) 0.10708(19) 0.2137(2) 0.0156(11) Uani 1 1 d . . . H47 H 1.1801 0.1303 0.2063 0.019 Uiso 1 1 calc R . . C48 C 1.0544(6) 0.10289(18) 0.2734(2) 0.0148(10) Uani 1 1 d . . . H48 H 1.0995 0.1227 0.3067 0.018 Uiso 1 1 calc R . . C49 C 1.1124(6) 0.07665(19) 0.1044(2) 0.0126(10) Uani 1 1 d . . . O50 O 1.0849(4) 0.04123(13) 0.06764(16) 0.0173(8) Uani 1 1 d . . . O51 O 1.2125(4) 0.10733(13) 0.09229(15) 0.0177(8) Uani 1 1 d . . . C52 C 0.7845(6) -0.12610(18) 0.4703(2) 0.0140(10) Uani 1 1 d . . . C53 C 0.8534(6) -0.1527(2) 0.5222(3) 0.0231(12) Uani 1 1 d . . . H53 H 0.8933 -0.1370 0.5601 0.028 Uiso 1 1 calc R . . C54 C 0.8634(7) -0.2017(2) 0.5183(3) 0.0247(12) Uani 1 1 d . . . H54 H 0.9107 -0.2193 0.5535 0.030 Uiso 1 1 calc R . . C55 C 0.8041(6) -0.2254(2) 0.4629(2) 0.0209(12) Uani 1 1 d . . . C56 C 0.7363(6) -0.1996(2) 0.4119(2) 0.0228(12) Uani 1 1 d . . . H56 H 0.6964 -0.2154 0.3741 0.027 Uiso 1 1 calc R . . C57 C 0.7259(7) -0.1504(2) 0.4156(2) 0.0223(12) Uani 1 1 d . . . H57 H 0.6781 -0.1330 0.3802 0.027 Uiso 1 1 calc R . . C58 C 0.8212(7) -0.2781(2) 0.4612(3) 0.0232(12) Uani 1 1 d . . . O59 O 0.8703(5) -0.30159(14) 0.50684(18) 0.0275(9) Uani 1 1 d . . . O60 O 0.7728(5) -0.29680(14) 0.40494(18) 0.0299(10) Uani 1 1 d . . . H60 H 0.7874 -0.3263 0.4062 0.045 Uiso 1 1 calc R . . O61 O 1.0914(4) 0.08656(15) -0.05948(17) 0.0266(9) Uani 1 1 d . . . C62 C 0.9688(7) 0.1110(2) -0.0688(3) 0.0252(13) Uani 1 1 d . . . H62 H 0.9396 0.1293 -0.0348 0.030 Uiso 1 1 calc R . . N63 N 0.8781(5) 0.11291(18) -0.1226(2) 0.0266(11) Uani 1 1 d . . . C64 C 0.9159(9) 0.0852(3) -0.1767(3) 0.057(2) Uani 1 1 d . . . H64A H 0.9365 0.1068 -0.2106 0.085 Uiso 1 1 calc R . . H64B H 0.8264 0.0645 -0.1914 0.085 Uiso 1 1 calc R . . H64C H 1.0100 0.0658 -0.1642 0.085 Uiso 1 1 calc R . . C65 C 0.7338(8) 0.1414(3) -0.1306(4) 0.052(2) Uani 1 1 d . . . H65A H 0.6415 0.1203 -0.1364 0.078 Uiso 1 1 calc R . . H65B H 0.7338 0.1618 -0.1676 0.078 Uiso 1 1 calc R . . H65C H 0.7290 0.1610 -0.0932 0.078 Uiso 1 1 calc R . . O66 O 1.2105(4) -0.01766(14) -0.02018(16) 0.0213(9) Uani 1 1 d . . . H66A H 1.1403 -0.0287 0.0093 0.032 Uiso 1 1 d R . . H66B H 1.3028 -0.0388 -0.0188 0.032 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er 0.01696(13) 0.01353(12) 0.00903(11) 0.00009(10) 0.00173(8) -0.00111(10) C1 0.015(3) 0.017(3) 0.013(2) -0.003(2) -0.0009(18) 0.002(2) C2 0.030(3) 0.017(3) 0.009(2) -0.002(2) 0.004(2) -0.002(2) C3 0.023(3) 0.022(3) 0.012(2) 0.000(2) 0.005(2) -0.004(2) C4 0.018(3) 0.020(3) 0.013(3) 0.002(2) 0.002(2) 0.004(2) C5 0.016(3) 0.026(3) 0.007(2) 0.004(2) -0.0002(19) 0.001(2) C6 0.017(3) 0.018(3) 0.011(2) 0.002(2) 0.0022(19) 0.001(2) C7 0.027(3) 0.019(3) 0.010(3) -0.004(2) 0.003(2) -0.004(2) C8 0.027(3) 0.019(3) 0.020(3) -0.006(2) 0.010(2) 0.000(2) C9 0.012(3) 0.019(3) 0.017(3) -0.002(2) 0.0030(19) -0.001(2) C10 0.019(3) 0.021(3) 0.017(3) -0.003(2) 0.002(2) -0.002(2) C11 0.015(3) 0.015(3) 0.018(3) 0.003(2) -0.002(2) 0.000(2) C12 0.025(3) 0.014(3) 0.019(3) 0.006(2) 0.003(2) 0.007(2) C13 0.017(3) 0.023(3) 0.007(2) 0.001(2) -0.0010(19) 0.000(2) C14 0.014(3) 0.021(3) 0.011(2) 0.000(2) -0.0005(19) 0.002(2) C15 0.013(3) 0.022(3) 0.010(2) -0.004(2) 0.0006(18) -0.008(2) C16 0.015(3) 0.016(3) 0.012(2) -0.003(2) -0.0032(19) 0.000(2) C17 0.018(3) 0.017(3) 0.013(3) -0.002(2) 0.004(2) 0.001(2) C18 0.024(3) 0.020(3) 0.009(2) -0.001(2) 0.0055(19) 0.002(2) C19 0.022(3) 0.016(3) 0.012(3) 0.0001(19) 0.006(2) 0.000(2) C20 0.015(3) 0.015(3) 0.013(3) -0.002(2) -0.0012(19) 0.0032(19) N21 0.019(2) 0.019(3) 0.014(2) 0.0020(18) 0.0046(17) 0.0029(18) N22 0.018(2) 0.015(2) 0.013(2) 0.0004(17) 0.0046(17) 0.0027(17) N23 0.018(2) 0.019(2) 0.008(2) 0.0013(17) 0.0004(16) 0.0046(18) N24 0.022(2) 0.019(2) 0.010(2) 0.0033(17) 0.0039(17) 0.0048(18) C25 0.019(3) 0.015(3) 0.008(2) 0.0025(19) 0.0017(19) -0.001(2) C26 0.023(3) 0.021(3) 0.013(3) 0.002(2) 0.002(2) 0.003(2) C27 0.017(3) 0.017(3) 0.017(3) 0.001(2) 0.002(2) 0.001(2) C28 0.016(3) 0.023(3) 0.007(2) 0.002(2) 0.0013(18) 0.004(2) C29 0.026(3) 0.025(3) 0.011(3) 0.007(2) 0.007(2) 0.007(2) C30 0.022(3) 0.024(3) 0.019(3) 0.001(2) 0.005(2) 0.013(2) C31 0.021(3) 0.021(3) 0.006(2) -0.001(2) -0.0003(19) -0.005(2) O32 0.035(2) 0.025(2) 0.0149(19) -0.0004(15) 0.0103(17) 0.0062(17) O33 0.0195(19) 0.023(2) 0.0156(19) 0.0066(15) 0.0009(14) 0.0015(15) C34 0.026(3) 0.017(3) 0.020(3) 0.001(2) 0.012(2) 0.000(2) C35 0.018(3) 0.021(3) 0.030(3) -0.003(2) 0.009(2) -0.007(2) C36 0.021(3) 0.025(3) 0.027(3) 0.003(2) 0.009(2) 0.006(2) C37 0.023(3) 0.022(3) 0.019(3) 0.000(2) 0.010(2) -0.004(2) C38 0.017(3) 0.028(3) 0.032(3) -0.003(3) 0.006(2) 0.000(2) C39 0.024(3) 0.020(3) 0.021(3) -0.003(2) 0.003(2) -0.001(2) C40 0.033(4) 0.021(3) 0.023(3) 0.006(2) 0.008(2) 0.003(3) O41 0.030(2) 0.011(2) 0.059(3) -0.0034(19) -0.001(2) -0.0036(17) O42 0.027(2) 0.023(2) 0.027(2) 0.0017(17) 0.0048(17) 0.0167(17) C43 0.020(3) 0.021(3) 0.009(2) 0.0011(19) 0.0033(19) 0.005(2) C44 0.016(3) 0.022(3) 0.014(3) 0.001(2) 0.003(2) -0.004(2) C45 0.016(3) 0.022(3) 0.012(3) -0.003(2) -0.0008(19) -0.004(2) C46 0.017(3) 0.016(3) 0.010(2) 0.001(2) -0.0040(19) 0.004(2) C47 0.013(3) 0.020(3) 0.014(3) 0.001(2) 0.0000(19) 0.005(2) C48 0.017(3) 0.017(3) 0.010(2) -0.0037(19) 0.0014(19) 0.001(2) C49 0.010(3) 0.017(3) 0.011(2) 0.004(2) 0.0015(18) 0.0054(19) O50 0.0142(19) 0.023(2) 0.0151(19) -0.0052(15) 0.0052(14) -0.0039(15) O51 0.022(2) 0.019(2) 0.0125(18) 0.0002(14) 0.0058(14) -0.0060(15) C52 0.013(3) 0.018(3) 0.012(3) -0.001(2) 0.0053(19) -0.003(2) C53 0.028(3) 0.020(3) 0.020(3) -0.001(2) -0.002(2) -0.004(2) C54 0.024(3) 0.021(3) 0.028(3) 0.005(2) -0.003(2) 0.001(2) C55 0.022(3) 0.022(3) 0.018(3) 0.002(2) 0.000(2) -0.002(2) C56 0.030(3) 0.021(3) 0.015(3) -0.003(2) -0.003(2) 0.002(2) C57 0.034(3) 0.019(3) 0.014(3) 0.004(2) 0.002(2) 0.007(2) C58 0.032(3) 0.018(3) 0.020(3) 0.002(2) 0.006(2) 0.000(2) O59 0.030(2) 0.018(2) 0.032(2) 0.0049(17) -0.0050(17) -0.0029(17) O60 0.052(3) 0.013(2) 0.025(2) -0.0002(17) 0.0075(19) 0.0046(19) O61 0.022(2) 0.033(3) 0.023(2) 0.0055(18) -0.0055(16) 0.0090(18) C62 0.025(3) 0.029(3) 0.020(3) 0.002(2) -0.002(2) -0.001(2) N63 0.022(3) 0.030(3) 0.025(3) 0.003(2) -0.006(2) 0.008(2) C64 0.065(5) 0.068(6) 0.033(4) -0.024(4) -0.013(3) 0.022(4) C65 0.034(4) 0.060(5) 0.056(5) -0.005(4) -0.017(3) 0.025(4) O66 0.020(2) 0.027(2) 0.018(2) -0.0089(16) 0.0077(15) -0.0057(16) _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 Er O42 2.192(4) 4_665 ? Er O33 2.200(3) 3_756 ? Er O61 2.242(4) . ? Er O32 2.276(4) 1_654 ? Er O66 2.307(4) . ? Er O50 2.394(3) . ? Er O51 2.470(3) . ? Er C49 2.810(5) . ? C1 N21 1.359(6) . ? C1 C20 1.409(7) . ? C1 C2 1.459(7) . ? C2 C3 1.348(7) . ? C2 H2 0.9500 . ? C3 C4 1.436(7) . ? C3 H3 0.9500 . ? C4 N21 1.369(6) . ? C4 C5 1.418(7) . ? C5 C6 1.399(7) . ? C5 C25 1.490(6) . ? C6 N22 1.376(6) . ? C6 C7 1.440(7) . ? C7 C8 1.334(7) . ? C7 H7 0.9500 . ? C8 C9 1.464(7) . ? C8 H8 0.9500 . ? C9 N22 1.356(7) . ? C9 C10 1.407(7) . ? C10 C11 1.411(7) . ? C10 C34 1.481(8) . ? C11 N23 1.364(7) . ? C11 C12 1.450(7) . ? C12 C13 1.349(7) . ? C12 H12 0.9500 . ? C13 C14 1.440(7) . ? C13 H13 0.9500 . ? C14 N23 1.373(6) . ? C14 C15 1.400(7) . ? C15 C16 1.411(7) . ? C15 C43 1.494(7) . ? C16 N24 1.367(6) . ? C16 C17 1.444(7) . ? C17 C18 1.348(7) . ? C17 H17 0.9500 . ? C18 C19 1.438(7) . ? C18 H18 0.9500 . ? C19 N24 1.376(7) . ? C19 C20 1.408(7) . ? C20 C52 1.496(7) . ? N21 H21 0.8800 . ? N22 H22 0.8800 . ? N23 H23 0.8800 . ? N24 H24 0.8800 . ? C25 C30 1.383(7) . ? C25 C26 1.395(7) . ? C26 C27 1.380(7) . ? C26 H26 0.9500 . ? C27 C28 1.387(7) . ? C27 H27 0.9500 . ? C28 C29 1.380(7) . ? C28 C31 1.504(6) . ? C29 C30 1.381(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O32 1.246(6) . ? C31 O33 1.271(6) . ? O32 Er 2.276(4) 1_456 ? O33 Er 2.200(3) 3_756 ? C34 C39 1.373(8) . ? C34 C35 1.434(8) . ? C35 C36 1.391(8) . ? C35 H35 0.9500 . ? C36 C37 1.381(8) . ? C36 H36 0.9500 . ? C37 C38 1.365(8) . ? C37 C40 1.516(8) . ? C38 C39 1.389(8) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 O41 1.253(7) . ? C40 O42 1.264(7) . ? O42 Er 2.192(4) 4_466 ? C43 C44 1.384(7) . ? C43 C48 1.412(7) . ? C44 C45 1.384(7) . ? C44 H44 0.9500 . ? C45 C46 1.398(7) . ? C45 H45 0.9500 . ? C46 C47 1.390(7) . ? C46 C49 1.502(7) . ? C47 C48 1.400(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 O51 1.263(6) . ? C49 O50 1.275(6) . ? C52 C57 1.395(7) . ? C52 C53 1.407(7) . ? C53 C54 1.387(8) . ? C53 H53 0.9500 . ? C54 C55 1.399(8) . ? C54 H54 0.9500 . ? C55 C56 1.378(7) . ? C55 C58 1.493(8) . ? C56 C57 1.392(7) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 O59 1.212(6) . ? C58 O60 1.333(6) . ? O60 H60 0.8400 . ? O61 C62 1.246(7) . ? C62 N63 1.307(7) . ? C62 H62 0.9500 . ? N63 C65 1.460(7) . ? N63 C64 1.466(8) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O66 H66A 0.9740 . ? O66 H66B 0.9826 . ? 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 O42 Er O33 87.52(14) 4_665 3_756 ? O42 Er O61 103.70(15) 4_665 . ? O33 Er O61 168.64(14) 3_756 . ? O42 Er O32 80.04(14) 4_665 1_654 ? O33 Er O32 102.76(13) 3_756 1_654 ? O61 Er O32 81.30(14) . 1_654 ? O42 Er O66 152.76(14) 4_665 . ? O33 Er O66 81.68(13) 3_756 . ? O61 Er O66 88.88(14) . . ? O32 Er O66 78.10(13) 1_654 . ? O42 Er O50 131.66(13) 4_665 . ? O33 Er O50 90.20(12) 3_756 . ? O61 Er O50 81.03(13) . . ? O32 Er O50 146.73(13) 1_654 . ? O66 Er O50 73.60(12) . . ? O42 Er O51 78.29(13) 4_665 . ? O33 Er O51 90.45(12) 3_756 . ? O61 Er O51 90.09(13) . . ? O32 Er O51 154.04(13) 1_654 . ? O66 Er O51 126.45(11) . . ? O50 Er O51 53.43(11) . . ? O42 Er C49 104.79(15) 4_665 . ? O33 Er C49 88.32(13) 3_756 . ? O61 Er C49 87.07(14) . . ? O32 Er C49 168.21(14) 1_654 . ? O66 Er C49 99.84(14) . . ? O50 Er C49 26.87(13) . . ? O51 Er C49 26.71(13) . . ? N21 C1 C20 125.9(5) . . ? N21 C1 C2 109.1(4) . . ? C20 C1 C2 124.9(5) . . ? C3 C2 C1 106.3(5) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 108.0(5) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? N21 C4 C5 125.8(5) . . ? N21 C4 C3 108.9(4) . . ? C5 C4 C3 125.4(5) . . ? C6 C5 C4 124.1(4) . . ? C6 C5 C25 117.7(5) . . ? C4 C5 C25 118.1(5) . . ? N22 C6 C5 124.9(5) . . ? N22 C6 C7 108.1(4) . . ? C5 C6 C7 126.7(4) . . ? C8 C7 C6 108.3(5) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 107.0(5) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? N22 C9 C10 126.3(5) . . ? N22 C9 C8 108.3(4) . . ? C10 C9 C8 125.2(5) . . ? C11 C10 C9 124.2(5) . . ? C11 C10 C34 118.1(5) . . ? C9 C10 C34 117.6(5) . . ? N23 C11 C10 126.4(5) . . ? N23 C11 C12 108.7(4) . . ? C10 C11 C12 124.6(5) . . ? C13 C12 C11 106.9(5) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? C12 C13 C14 108.1(4) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? N23 C14 C15 125.5(5) . . ? N23 C14 C13 108.1(4) . . ? C15 C14 C13 126.4(5) . . ? C14 C15 C16 124.9(4) . . ? C14 C15 C43 117.4(5) . . ? C16 C15 C43 117.6(4) . . ? N24 C16 C15 125.5(4) . . ? N24 C16 C17 108.3(4) . . ? C15 C16 C17 126.2(5) . . ? C18 C17 C16 108.0(4) . . ? C18 C17 H17 126.0 . . ? C16 C17 H17 126.0 . . ? C17 C18 C19 107.0(5) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? N24 C19 C20 124.6(5) . . ? N24 C19 C18 108.9(4) . . ? C20 C19 C18 126.4(5) . . ? C1 C20 C19 125.1(5) . . ? C1 C20 C52 116.9(5) . . ? C19 C20 C52 118.0(4) . . ? C1 N21 C4 107.6(4) . . ? C1 N21 H21 126.2 . . ? C4 N21 H21 126.2 . . ? C9 N22 C6 108.2(4) . . ? C9 N22 H22 125.9 . . ? C6 N22 H22 125.9 . . ? C11 N23 C14 108.2(4) . . ? C11 N23 H23 125.9 . . ? C14 N23 H23 125.9 . . ? C16 N24 C19 107.7(4) . . ? C16 N24 H24 126.1 . . ? C19 N24 H24 126.1 . . ? C30 C25 C26 117.8(4) . . ? C30 C25 C5 120.3(5) . . ? C26 C25 C5 121.8(5) . . ? C25 C26 C27 121.3(5) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 119.7(5) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 C31 120.2(4) . . ? C27 C28 C31 120.3(5) . . ? C28 C29 C30 120.2(5) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 121.3(5) . . ? C25 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? O32 C31 O33 123.6(4) . . ? O32 C31 C28 118.4(5) . . ? O33 C31 C28 118.0(5) . . ? C31 O32 Er 134.6(3) . 1_456 ? C31 O33 Er 159.5(3) . 3_756 ? C39 C34 C35 119.0(5) . . ? C39 C34 C10 122.7(5) . . ? C35 C34 C10 118.3(5) . . ? C36 C35 C34 118.1(5) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C37 C36 C35 121.3(5) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 120.1(5) . . ? C36 C37 C40 118.5(5) . . ? C38 C37 C40 121.2(5) . . ? C37 C38 C39 120.1(5) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 121.3(5) . . ? C34 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? O41 C40 O42 125.5(6) . . ? O41 C40 C37 117.5(5) . . ? O42 C40 C37 117.0(5) . . ? C40 O42 Er 148.4(4) . 4_466 ? C44 C43 C48 118.2(4) . . ? C44 C43 C15 120.3(5) . . ? C48 C43 C15 121.5(4) . . ? C43 C44 C45 122.0(5) . . ? C43 C44 H44 119.0 . . ? C45 C44 H44 119.0 . . ? C44 C45 C46 119.5(5) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 119.8(5) . . ? C47 C46 C49 119.8(5) . . ? C45 C46 C49 119.9(5) . . ? C46 C47 C48 120.1(5) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 120.2(5) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? O51 C49 O50 119.1(4) . . ? O51 C49 C46 121.6(5) . . ? O50 C49 C46 118.8(4) . . ? O51 C49 Er 61.5(2) . . ? O50 C49 Er 58.1(2) . . ? C46 C49 Er 165.7(3) . . ? C49 O50 Er 95.0(3) . . ? C49 O51 Er 91.8(3) . . ? C57 C52 C53 118.3(5) . . ? C57 C52 C20 121.7(5) . . ? C53 C52 C20 120.0(5) . . ? C54 C53 C52 120.4(5) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 120.5(5) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C56 C55 C54 119.5(5) . . ? C56 C55 C58 122.5(5) . . ? C54 C55 C58 118.0(5) . . ? C55 C56 C57 120.2(5) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C56 C57 C52 121.2(5) . . ? C56 C57 H57 119.4 . . ? C52 C57 H57 119.4 . . ? O59 C58 O60 123.4(5) . . ? O59 C58 C55 123.3(5) . . ? O60 C58 C55 113.3(5) . . ? C58 O60 H60 109.5 . . ? C62 O61 Er 149.8(4) . . ? O61 C62 N63 123.8(6) . . ? O61 C62 H62 118.1 . . ? N63 C62 H62 118.1 . . ? C62 N63 C65 121.6(5) . . ? C62 N63 C64 120.8(5) . . ? C65 N63 C64 117.6(5) . . ? N63 C64 H64A 109.5 . . ? N63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N63 C65 H65A 109.5 . . ? N63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Er O66 H66A 109.5 . . ? Er O66 H66B 109.3 . . ? H66A O66 H66B 109.9 . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.702 _refine_diff_density_min -1.866 _refine_diff_density_rms 0.171 #============================END==========================