Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Drozdov, Andrei' 'Marchetti, Fabio' 'Pettinari, Claudio' 'Pettinari, Riccardo' 'Shavaleev, Nail M.' 'Troyanov, Sergei' 'Voloshin, Alexander I.' _publ_contact_author_name 'Prof Claudio Pettinari' _publ_contact_author_address ; Dipartimento di Scienze Chimiche Universita degli Studi di Camerino via S. Agostino 1 60232 Camerino MC ITALY ; _publ_contact_author_email 'PETTINAR@CAMSERV.UNICAM.IT' _publ_section_title ; Synthesis, structure & luminescence properties of new rare earth metal complexes with 1-phenyl-3-methyl-4-acyl-pyrazol-5-ones ; data_euqsnum _database_code_CSD 170585 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C47 H40 Eu N6 O8 S3' _chemical_formula_weight 1066.00 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.853(2) _cell_length_b 34.270(6) _cell_length_c 15.100(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.34(3) _cell_angle_gamma 90.00 _cell_volume 4581.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method ? _exptl_crystal_F_000 2156 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6300 _exptl_absorpt_correction_T_max 0.8430 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22331 _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_sigmaI/netI 0.0994 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.87 _reflns_number_total 9698 _reflns_number_observed 5698 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2913 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+462.8609P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6785 _refine_ls_number_parameters 551 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1607 _refine_ls_R_factor_obs 0.1244 _refine_ls_wR_factor_all 0.3343 _refine_ls_wR_factor_obs 0.2846 _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.244 _refine_ls_restrained_S_all 1.180 _refine_ls_restrained_S_obs 1.274 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Eu Eu 0.73269(13) 0.09076(3) 0.13672(7) 0.0176(3) Uani 1 d . . S1 S 0.7980(10) -0.0229(2) 0.3437(5) 0.050(2) Uani 1 d . . S2 S 1.0065(9) 0.2166(2) 0.0226(5) 0.046(2) Uani 1 d . . S3 S 0.3627(8) 0.0238(2) 0.3707(5) 0.042(2) Uani 1 d . . O1 O 0.8139(19) 0.0295(5) 0.1968(11) 0.032(4) Uani 1 d . . O2 O 0.9231(19) 0.0647(5) 0.0457(11) 0.035(4) Uani 1 d . . O3 O 0.9119(21) 0.1435(5) 0.1249(14) 0.043(5) Uani 1 d . . O4 O 0.8297(23) 0.1056(5) 0.2781(11) 0.038(4) Uani 1 d . . O5 O 0.5240(20) 0.0738(5) 0.2288(12) 0.040(4) Uani 1 d . . O6 O 0.5945(19) 0.1495(5) 0.1598(13) 0.038(4) Uani 1 d . . O7 O 0.6474(25) 0.1175(5) -0.0103(13) 0.050(5) Uani 1 d . . O8 O 0.5841(19) 0.0414(5) 0.0513(10) 0.031(4) Uani 1 d . . N1 N 1.1663(26) 0.0466(5) 0.0256(13) 0.034(5) Uani 1 d . . N2 N 1.2584(24) 0.0182(5) 0.0587(12) 0.030(5) Uani 1 d U . N3 N 0.8456(26) 0.1509(7) 0.3924(15) 0.046(6) Uani 1 d . . N4 N 0.8928(30) 0.1890(7) 0.4061(15) 0.046(6) Uani 1 d . . N5 N 0.5224(24) 0.1948(6) 0.2693(14) 0.035(5) Uani 1 d . . N6 N 0.4465(25) 0.1954(6) 0.3506(14) 0.034(5) Uani 1 d . . C1 C 0.9233(29) 0.0068(7) 0.1922(16) 0.031(5) Uani 1 d . . C2 C 1.0496(24) 0.0126(6) 0.1331(13) 0.018(4) Uani 1 d . . C3 C 1.0319(27) 0.0449(6) 0.0651(13) 0.023(5) Uani 1 d . . C4 C 1.2037(30) -0.0003(6) 0.1240(15) 0.031(6) Uani 1 d . . C5 C 1.2796(34) -0.0306(8) 0.1688(18) 0.045(7) Uani 1 d . . H5A H 1.2602(181) -0.0554(12) 0.1385(78) 0.068 Uiso 1 calc R . H5B H 1.2430(164) -0.0322(39) 0.2298(43) 0.068 Uiso 1 calc R . H5C H 1.3883(42) -0.0253(29) 0.1693(114) 0.068 Uiso 1 calc R . C6 C 1.2208(26) 0.0741(7) -0.0399(15) 0.025(5) Uani 1 d . . C7 C 1.3127(27) 0.0611(7) -0.1072(15) 0.029(5) Uani 1 d . . H7 H 1.3402(27) 0.0344(7) -0.1113(15) 0.035 Uiso 1 calc R . C8 C 1.3650(28) 0.0886(8) -0.1698(16) 0.037(6) Uani 1 d . . H8 H 1.4264(28) 0.0805(8) -0.2179(16) 0.045 Uiso 1 calc R . C9 C 1.3245(29) 0.1283(9) -0.1598(19) 0.046(8) Uani 1 d . . H9 H 1.3586(29) 0.1472(9) -0.2012(19) 0.055 Uiso 1 calc R . C10 C 1.2368(34) 0.1392(8) -0.0908(17) 0.041(7) Uani 1 d . . H10 H 1.2112(34) 0.1660(8) -0.0842(17) 0.050 Uiso 1 calc R . C11 C 1.1839(35) 0.1127(7) -0.0300(18) 0.043(7) Uani 1 d . . H11 H 1.1227(35) 0.1210(7) 0.0179(18) 0.052 Uiso 1 calc R . C12 C 0.9197(27) -0.0273(7) 0.2544(16) 0.031(5) Uani 1 d . . C13 C 0.9892(31) -0.0637(8) 0.2500(21) 0.046(7) Uani 1 d . . H13 H 1.0549(31) -0.0718(8) 0.2041(21) 0.055 Uiso 1 calc R . C14 C 0.9465(42) -0.0877(11) 0.3265(27) 0.076(13) Uani 1 d . . H14 H 0.9861(42) -0.1129(11) 0.3386(27) 0.092 Uiso 1 calc R . C15 C 0.8403(51) -0.0686(10) 0.3792(23) 0.072(12) Uani 1 d . . H15 H 0.7960(51) -0.0802(10) 0.4300(23) 0.087 Uiso 1 calc R . C16 C 0.9652(32) 0.1692(7) 0.1680(17) 0.036(6) Uani 1 d . . C17 C 0.9381(31) 0.1706(9) 0.2611(19) 0.046(7) Uani 1 d . . C18 C 0.8634(26) 0.1390(6) 0.3063(14) 0.024(5) Uani 1 d . . C19 C 0.9504(37) 0.2005(8) 0.3319(20) 0.050(8) Uani 1 d . . C20 C 0.9943(48) 0.2417(9) 0.3216(25) 0.076(12) Uani 1 d . . H20A H 0.9539(268) 0.2518(25) 0.2655(93) 0.114 Uiso 1 calc R . H20B H 1.1047(49) 0.2438(13) 0.3216(186) 0.114 Uiso 1 calc R . H20C H 0.9534(275) 0.2570(17) 0.3708(105) 0.114 Uiso 1 calc R . C21 C 0.7700(10) 0.1314(3) 0.4614(5) 0.036(6) Uani 1 d G . C22 C 0.7670(13) 0.1494(3) 0.5439(5) 0.052(8) Uani 1 d G . H22 H 0.8037(14) 0.1753(4) 0.5506(5) 0.062 Uiso 1 calc R . C23 C 0.7102(14) 0.1294(4) 0.6167(5) 0.082(11) Uani 1 d GU . H23 H 0.7082(16) 0.1417(4) 0.6731(5) 0.098 Uiso 1 calc R . C24 C 0.6565(14) 0.0916(4) 0.6069(5) 0.046(6) Uani 1 d GU . H24 H 0.6177(15) 0.0780(4) 0.6567(6) 0.055 Uiso 1 calc R . C25 C 0.6595(12) 0.0736(3) 0.5244(6) 0.056(8) Uani 1 d GU . H25 H 0.6228(13) 0.0477(3) 0.5178(7) 0.067 Uiso 1 calc R . C26 C 0.7163(11) 0.0935(2) 0.4517(6) 0.053(8) Uani 1 d G . H26 H 0.7184(11) 0.0812(2) 0.3953(6) 0.064 Uiso 1 calc R . C27 C 1.0611(10) 0.2000(3) 0.1259(6) 0.030(5) Uani 1 d G . C28 C 1.2004(11) 0.2144(4) 0.1502(7) 0.054(9) Uani 1 d G . H28 H 1.2550(10) 0.2069(4) 0.2018(8) 0.065 Uiso 1 calc R . C29 C 1.2483(12) 0.2407(4) 0.0903(8) 0.043(7) Uani 1 d GU . H29 H 1.3386(13) 0.2553(4) 0.0983(9) 0.052 Uiso 1 calc R . C30 C 1.1581(14) 0.2449(4) 0.0175(8) 0.062(9) Uani 1 d G . H30 H 1.1795(15) 0.2620(4) -0.0303(8) 0.075 Uiso 1 calc R . C31 C 0.4410(11) 0.0927(3) 0.2826(6) 0.032(5) Uani 1 d G . C32 C 0.4474(9) 0.1339(3) 0.2943(5) 0.037(6) Uani 1 d G . C33 C 0.5281(9) 0.1594(3) 0.2354(5) 0.027(5) Uani 1 d G . C34 C 0.3937(9) 0.1592(3) 0.3642(6) 0.030(5) Uani 1 d G . C35 C 0.3231(10) 0.1506(3) 0.4512(7) 0.045(7) Uani 1 d G . H35A H 0.3398(197) 0.1231(15) 0.4664(63) 0.068 Uiso 1 calc R . H35B H 0.2144(38) 0.1558(56) 0.4477(39) 0.068 Uiso 1 calc R . H35C H 0.3687(159) 0.1672(42) 0.4969(25) 0.068 Uiso 1 calc R . C36 C 0.5683(25) 0.2318(7) 0.2335(17) 0.029(5) Uani 1 d . . C37 C 0.5257(35) 0.2649(8) 0.2716(19) 0.046(7) Uani 1 d . . H37 H 0.4834(35) 0.2653(8) 0.3292(19) 0.055 Uiso 1 calc R . C38 C 0.5451(48) 0.2974(11) 0.2252(25) 0.090(16) Uani 1 d . . H38 H 0.4887(48) 0.3195(11) 0.2436(25) 0.108 Uiso 1 calc R . C39 C 0.6405(39) 0.3028(8) 0.1514(27) 0.066(11) Uani 1 d . . H39 H 0.6639(39) 0.3275(8) 0.1269(27) 0.079 Uiso 1 calc R . C40 C 0.6941(35) 0.2691(8) 0.1198(19) 0.045(7) Uani 1 d . . H40 H 0.7658(35) 0.2701(8) 0.0733(19) 0.054 Uiso 1 calc R . C41 C 0.6504(33) 0.2324(8) 0.1513(19) 0.044(7) Uani 1 d . . H41 H 0.6736(33) 0.2091(8) 0.1202(19) 0.053 Uiso 1 calc R . C42 C 0.3257(27) 0.0710(7) 0.3332(15) 0.029(5) Uani 1 d . . C43 C 0.1758(28) 0.0783(7) 0.3403(18) 0.037(6) Uani 1 d . . H43 H 0.1319(28) 0.1021(7) 0.3204(18) 0.045 Uiso 1 calc R . C44 C 0.0894(34) 0.0485(11) 0.3790(23) 0.060(9) Uani 1 d . . H44 H -0.0164(34) 0.0491(11) 0.3890(23) 0.072 Uiso 1 calc R . C45 C 0.1847(41) 0.0182(9) 0.3997(21) 0.060(10) Uani 1 d . . H45 H 0.1502(41) -0.0046(9) 0.4290(21) 0.071 Uiso 1 calc R . C46 C 0.6579(39) 0.1552(8) -0.0442(21) 0.054(8) Uani 1 d . . H46A H 0.7166(39) 0.1717(8) -0.0025(21) 0.065 Uiso 1 calc R . H46B H 0.5554(39) 0.1665(8) -0.0497(21) 0.065 Uiso 1 calc R . C47 C 0.7322(32) 0.1556(10) -0.1325(19) 0.057(10) Uani 1 d . . H47A H 0.8417(40) 0.1530(69) -0.1248(21) 0.086 Uiso 1 calc R . H47B H 0.7097(220) 0.1803(30) -0.1626(67) 0.086 Uiso 1 calc R . H47C H 0.6939(199) 0.1339(42) -0.1683(60) 0.086 Uiso 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 Eu 0.0276(6) 0.0104(5) 0.0148(5) -0.0004(4) 0.0016(4) 0.0006(5) S1 0.078(6) 0.035(4) 0.037(4) 0.002(3) 0.021(4) -0.015(4) S2 0.041(4) 0.056(5) 0.042(4) 0.002(3) 0.001(3) -0.011(3) S3 0.035(4) 0.029(3) 0.063(5) 0.007(3) 0.002(3) -0.002(3) O1 0.028(9) 0.029(9) 0.039(10) -0.006(7) 0.002(7) 0.005(8) O2 0.022(9) 0.051(11) 0.032(9) 0.001(8) -0.003(7) 0.008(8) O3 0.032(10) 0.020(9) 0.078(14) 0.021(9) 0.015(10) 0.004(8) O4 0.061(13) 0.023(9) 0.030(9) 0.006(7) -0.007(8) 0.002(8) O5 0.031(10) 0.037(10) 0.052(11) -0.003(8) 0.014(9) 0.016(8) O6 0.023(9) 0.029(9) 0.063(12) 0.007(8) 0.007(8) 0.000(7) O7 0.069(15) 0.034(10) 0.047(11) 0.012(9) -0.011(10) 0.002(10) O8 0.030(9) 0.036(10) 0.026(8) -0.012(7) -0.013(7) -0.005(8) N1 0.046(14) 0.019(10) 0.036(11) 0.006(9) 0.004(10) 0.012(9) N2 0.041(11) 0.023(9) 0.025(9) 0.000(8) -0.022(8) -0.017(8) N3 0.029(13) 0.061(16) 0.047(14) -0.017(12) -0.004(10) 0.000(11) N4 0.062(17) 0.035(13) 0.040(13) -0.005(10) -0.007(12) 0.013(12) N5 0.034(12) 0.023(11) 0.047(13) 0.003(9) 0.012(10) 0.015(9) N6 0.036(12) 0.022(10) 0.043(12) 0.002(9) -0.011(10) 0.008(9) C1 0.033(14) 0.020(11) 0.040(14) -0.001(10) -0.004(11) 0.000(11) C2 0.023(12) 0.019(10) 0.013(10) -0.002(8) -0.005(8) 0.008(9) C3 0.033(14) 0.023(11) 0.012(10) 0.000(9) 0.008(9) 0.006(10) C4 0.045(16) 0.019(11) 0.028(13) 0.000(10) 0.003(11) -0.004(11) C5 0.048(18) 0.045(16) 0.043(16) 0.008(13) 0.000(13) 0.026(14) C6 0.020(12) 0.027(12) 0.028(12) -0.003(10) 0.006(10) -0.011(10) C7 0.028(13) 0.025(12) 0.035(13) -0.004(10) -0.006(10) 0.004(10) C8 0.027(13) 0.057(17) 0.028(12) 0.022(13) 0.008(10) 0.010(13) C9 0.018(13) 0.063(19) 0.055(18) 0.029(15) 0.001(12) 0.013(13) C10 0.053(18) 0.032(14) 0.040(15) 0.003(12) -0.001(13) -0.014(13) C11 0.059(19) 0.026(14) 0.045(16) 0.003(12) 0.021(14) -0.001(13) C12 0.025(13) 0.029(13) 0.037(14) 0.011(11) -0.005(10) 0.000(10) C13 0.032(15) 0.034(15) 0.070(20) 0.002(14) -0.028(14) -0.009(12) C14 0.060(22) 0.066(23) 0.102(29) 0.054(23) -0.047(21) -0.037(20) C15 0.106(32) 0.060(22) 0.051(20) 0.000(17) 0.024(21) -0.040(22) C16 0.051(17) 0.015(12) 0.041(15) 0.012(11) -0.008(12) -0.008(11) C17 0.026(14) 0.070(20) 0.043(16) 0.000(14) 0.000(12) 0.009(14) C18 0.028(13) 0.021(12) 0.023(11) -0.007(9) -0.005(9) 0.000(10) C19 0.060(20) 0.039(16) 0.050(17) -0.014(13) 0.026(15) -0.012(14) C20 0.098(31) 0.046(19) 0.084(26) -0.052(19) -0.004(22) -0.009(19) C21 0.062(18) 0.033(14) 0.012(11) 0.000(9) -0.009(11) 0.012(13) C22 0.096(26) 0.040(16) 0.020(13) 0.003(11) 0.002(14) 0.001(16) C23 0.112(20) 0.088(18) 0.045(15) -0.004(14) 0.010(15) 0.013(16) C24 0.074(11) 0.035(9) 0.029(9) 0.006(8) -0.028(8) -0.005(8) C25 0.067(16) 0.063(15) 0.037(13) -0.005(12) -0.028(12) -0.030(13) C26 0.070(22) 0.044(17) 0.047(16) 0.009(14) 0.016(15) 0.013(16) C27 0.018(12) 0.020(11) 0.051(15) 0.014(11) -0.003(11) 0.006(9) C28 0.051(20) 0.055(18) 0.055(18) -0.008(15) -0.017(15) -0.038(16) C29 0.030(12) 0.056(14) 0.043(12) 0.018(11) -0.031(10) -0.012(11) C30 0.063(22) 0.047(18) 0.077(23) 0.031(17) -0.003(18) -0.008(16) C31 0.029(13) 0.034(13) 0.034(13) -0.002(11) 0.001(10) 0.009(11) C32 0.048(17) 0.028(13) 0.037(14) 0.000(11) 0.015(12) 0.013(12) C33 0.013(11) 0.028(12) 0.040(13) 0.007(10) 0.007(10) 0.002(9) C34 0.028(13) 0.026(12) 0.035(13) -0.007(10) -0.002(10) 0.011(10) C35 0.074(22) 0.026(13) 0.037(15) 0.002(11) 0.027(14) 0.005(13) C36 0.014(11) 0.024(12) 0.051(15) 0.008(11) 0.005(10) 0.012(9) C37 0.058(20) 0.034(15) 0.047(16) -0.004(12) 0.022(14) -0.011(14) C38 0.108(32) 0.081(26) 0.081(25) 0.058(22) 0.068(25) 0.070(25) C39 0.060(22) 0.015(13) 0.123(31) 0.010(16) 0.035(21) 0.002(13) C40 0.054(19) 0.029(14) 0.051(17) -0.003(12) 0.008(14) -0.008(13) C41 0.048(18) 0.026(13) 0.058(18) 0.006(12) 0.027(14) 0.007(12) C42 0.024(13) 0.033(13) 0.028(12) 0.007(10) -0.005(10) 0.013(10) C43 0.025(14) 0.029(13) 0.058(17) 0.016(12) -0.011(12) 0.002(11) C44 0.023(15) 0.081(25) 0.077(23) -0.003(19) 0.012(15) -0.016(16) C45 0.083(25) 0.037(16) 0.059(19) -0.009(14) 0.058(19) -0.016(16) C46 0.058(20) 0.034(16) 0.069(21) 0.015(14) 0.003(16) -0.020(14) C47 0.044(19) 0.071(21) 0.057(19) 0.033(16) -0.044(16) -0.030(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 Eu O4 2.35(2) . ? Eu O2 2.36(2) . ? Eu O6 2.38(2) . ? Eu O5 2.39(2) . ? Eu O1 2.40(2) . ? Eu O3 2.41(2) . ? Eu O8 2.496(15) . ? Eu O7 2.51(2) . ? Eu C18 3.25(2) . ? S1 C15 1.70(4) . ? S1 C12 1.74(3) . ? S2 C30 1.657(13) . ? S2 C27 1.728(12) . ? S3 C45 1.65(3) . ? S3 C42 1.74(2) . ? O1 C1 1.24(3) . ? O2 C3 1.21(3) . ? O3 C16 1.19(3) . ? O4 C18 1.25(3) . ? O5 C31 1.28(2) . ? O6 C33 1.33(2) . ? O7 C46 1.40(3) . ? N1 C3 1.34(3) . ? N1 N2 1.36(3) . ? N1 C6 1.45(3) . ? N2 C4 1.27(3) . ? N3 C18 1.37(3) . ? N3 N4 1.38(3) . ? N3 C21 1.41(3) . ? N4 C19 1.30(4) . ? N5 C33 1.32(2) . ? N5 N6 1.40(3) . ? N5 C36 1.44(3) . ? N6 C34 1.34(2) . ? C1 C2 1.45(3) . ? C1 C12 1.50(3) . ? C2 C4 1.44(3) . ? C2 C3 1.52(3) . ? C4 C5 1.41(3) . ? C6 C11 1.37(3) . ? C6 C7 1.38(3) . ? C7 C8 1.42(3) . ? C8 C9 1.42(4) . ? C9 C10 1.36(4) . ? C10 C11 1.38(4) . ? C12 C13 1.39(4) . ? C13 C14 1.47(4) . ? C14 C15 1.40(6) . ? C16 C17 1.43(4) . ? C16 C27 1.50(3) . ? C17 C18 1.44(4) . ? C17 C19 1.48(4) . ? C19 C20 1.47(4) . ? C21 C22 1.39 . ? C21 C26 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C27 C28 1.38 . ? C28 C29 1.35 . ? C29 C30 1.36 . ? C31 C32 1.42 . ? C31 C42 1.48(3) . ? C32 C33 1.44 . ? C32 C34 1.45 . ? C34 C35 1.49 . ? C36 C37 1.33(4) . ? C36 C41 1.44(3) . ? C37 C38 1.33(4) . ? C38 C39 1.41(4) . ? C39 C40 1.34(4) . ? C40 C41 1.40(4) . ? C42 C43 1.36(3) . ? C43 C44 1.41(4) . ? C44 C45 1.37(5) . ? C46 C47 1.49(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu O2 110.7(6) . . ? O4 Eu O6 82.5(6) . . ? O2 Eu O6 140.8(6) . . ? O4 Eu O5 78.7(7) . . ? O2 Eu O5 143.6(6) . . ? O6 Eu O5 73.8(6) . . ? O4 Eu O1 74.9(6) . . ? O2 Eu O1 71.0(6) . . ? O6 Eu O1 147.0(6) . . ? O5 Eu O1 78.4(6) . . ? O4 Eu O3 70.6(7) . . ? O2 Eu O3 76.6(6) . . ? O6 Eu O3 73.5(6) . . ? O5 Eu O3 137.4(6) . . ? O1 Eu O3 119.3(6) . . ? O4 Eu O8 143.5(6) . . ? O2 Eu O8 79.5(6) . . ? O6 Eu O8 112.2(6) . . ? O5 Eu O8 74.3(6) . . ? O1 Eu O8 76.0(6) . . ? O3 Eu O8 144.5(6) . . ? O4 Eu O7 146.0(6) . . ? O2 Eu O7 80.5(6) . . ? O6 Eu O7 70.7(7) . . ? O5 Eu O7 111.9(7) . . ? O1 Eu O7 137.8(6) . . ? O3 Eu O7 81.7(7) . . ? O8 Eu O7 68.6(6) . . ? O4 Eu C18 18.1(6) . . ? O2 Eu C18 113.5(6) . . ? O6 Eu C18 68.7(6) . . ? O5 Eu C18 86.4(6) . . ? O1 Eu C18 92.4(6) . . ? O3 Eu C18 56.4(6) . . ? O8 Eu C18 159.1(6) . . ? O7 Eu C18 127.9(6) . . ? C15 S1 C12 91.6(15) . . ? C30 S2 C27 90.7(7) . . ? C45 S3 C42 90.9(14) . . ? C1 O1 Eu 139.3(16) . . ? C3 O2 Eu 129.9(14) . . ? C16 O3 Eu 140.5(18) . . ? C18 O4 Eu 126.2(14) . . ? C31 O5 Eu 134.3(12) . . ? C33 O6 Eu 124.7(11) . . ? C46 O7 Eu 129.9(18) . . ? C3 N1 N2 109.7(19) . . ? C3 N1 C6 129.3(20) . . ? N2 N1 C6 120.9(20) . . ? C4 N2 N1 114.3(22) . . ? C18 N3 N4 112.7(23) . . ? C18 N3 C21 128.0(21) . . ? N4 N3 C21 118.7(19) . . ? C19 N4 N3 106.1(22) . . ? C33 N5 N6 111.9(17) . . ? C33 N5 C36 130.9(19) . . ? N6 N5 C36 116.9(18) . . ? C34 N6 N5 106.8(16) . . ? O1 C1 C2 123.5(21) . . ? O1 C1 C12 115.6(22) . . ? C2 C1 C12 120.8(21) . . ? C4 C2 C1 138.6(20) . . ? C4 C2 C3 104.7(18) . . ? C1 C2 C3 116.2(19) . . ? O2 C3 N1 125.1(20) . . ? O2 C3 C2 130.6(21) . . ? N1 C3 C2 104.2(19) . . ? N2 C4 C5 123.9(26) . . ? N2 C4 C2 106.6(21) . . ? C5 C4 C2 129.1(23) . . ? C11 C6 C7 122.4(22) . . ? C11 C6 N1 118.2(21) . . ? C7 C6 N1 119.4(21) . . ? C6 C7 C8 118.2(22) . . ? C9 C8 C7 119.0(23) . . ? C10 C9 C8 119.6(25) . . ? C9 C10 C11 121.9(27) . . ? C6 C11 C10 118.8(25) . . ? C13 C12 C1 131.1(25) . . ? C13 C12 S1 113.0(20) . . ? C1 C12 S1 115.7(18) . . ? C12 C13 C14 110.4(31) . . ? C15 C14 C13 111.2(31) . . ? C14 C15 S1 113.6(24) . . ? O3 C16 C17 119.8(24) . . ? O3 C16 C27 120.8(22) . . ? C17 C16 C27 119.5(22) . . ? C16 C17 C18 121.3(25) . . ? C16 C17 C19 136.1(28) . . ? C18 C17 C19 102.1(22) . . ? O4 C18 N3 124.4(22) . . ? O4 C18 C17 129.1(22) . . ? N3 C18 C17 106.3(21) . . ? O4 C18 Eu 35.7(10) . . ? N3 C18 Eu 148.7(17) . . ? C17 C18 Eu 99.8(15) . . ? N4 C19 C20 119.3(26) . . ? N4 C19 C17 112.6(25) . . ? C20 C19 C17 127.2(28) . . ? C22 C21 C26 120.0 . . ? C22 C21 N3 117.6(10) . . ? C26 C21 N3 121.9(10) . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C28 C27 C16 130.5(11) . . ? C28 C27 S2 111.6(4) . . ? C16 C27 S2 117.4(12) . . ? C29 C28 C27 110.3 . . ? C28 C29 C30 115.3 . . ? C29 C30 S2 111.9(4) . . ? O5 C31 C32 124.0(9) . . ? O5 C31 C42 118.4(14) . . ? C32 C31 C42 117.5(10) . . ? C31 C32 C33 122.9 . . ? C31 C32 C34 132.1 . . ? C33 C32 C34 104.8 . . ? N5 C33 O6 125.8(13) . . ? N5 C33 C32 107.3(10) . . ? O6 C33 C32 126.9(8) . . ? N6 C34 C32 109.0(10) . . ? N6 C34 C35 117.8(10) . . ? C32 C34 C35 131.8 . . ? C37 C36 N5 120.6(22) . . ? C37 C36 C41 120.5(23) . . ? N5 C36 C41 118.7(21) . . ? C36 C37 C38 116.8(28) . . ? C37 C38 C39 127.1(30) . . ? C40 C39 C38 112.6(28) . . ? C39 C40 C41 123.7(28) . . ? C40 C41 C36 116.6(24) . . ? C43 C42 C31 128.8(20) . . ? C43 C42 S3 109.2(19) . . ? C31 C42 S3 120.4(15) . . ? C42 C43 C44 115.7(25) . . ? C45 C44 C43 108.0(25) . . ? C44 C45 S3 116.0(22) . . ? O7 C46 C47 111.6(27) . . ? _refine_diff_density_max 2.698 _refine_diff_density_min -2.131 _refine_diff_density_rms 0.200 data_(NBu4)[EuQF)4 _database_code_CSD 170586 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H66 Eu F12 N9 O8' _chemical_formula_weight 1469.22 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 25.759(3) _cell_length_b 21.455(3) _cell_length_c 26.353(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.54(1) _cell_angle_gamma 90.00 _cell_volume 13451.7(29) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 4935 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 21.5 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method ? _exptl_crystal_F_000 5984 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35698 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1085 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.09 _reflns_number_total 13097 _reflns_number_observed 6684 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2561 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0234P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10536 _refine_ls_number_parameters 877 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_obs 0.0351 _refine_ls_wR_factor_all 0.0758 _refine_ls_wR_factor_obs 0.0624 _refine_ls_goodness_of_fit_all 0.818 _refine_ls_goodness_of_fit_obs 0.972 _refine_ls_restrained_S_all 0.820 _refine_ls_restrained_S_obs 0.972 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Eu1 Eu 0.5000 0.57154(2) 0.2500 0.02406(10) Uani 1 d S . Eu2 Eu 0.5000 1.07785(2) 0.2500 0.02598(10) Uani 1 d S . O1 O 0.42942(12) 0.63333(14) 0.18552(14) 0.0310(8) Uani 1 d . . O2 O 0.54026(11) 0.62838(13) 0.19355(14) 0.0330(7) Uani 1 d . . O3 O 0.47887(11) 0.50416(13) 0.17538(12) 0.0318(7) Uani 1 d . . O4 O 0.58747(11) 0.52092(14) 0.25465(14) 0.0328(7) Uani 1 d . . O5 O 0.44364(12) 1.13930(14) 0.17437(13) 0.0308(8) Uani 1 d . . O6 O 0.42828(11) 1.13025(13) 0.27345(12) 0.0324(7) Uani 1 d . . O7 O 0.42651(11) 1.00788(14) 0.21432(14) 0.0377(8) Uani 1 d . . O8 O 0.48628(12) 1.0263(2) 0.32791(13) 0.0408(8) Uani 1 d . . N1 N 0.37315(15) 0.6620(2) 0.0962(2) 0.0327(10) Uani 1 d . . N2 N 0.3781(2) 0.6760(2) 0.0466(2) 0.0389(10) Uani 1 d . . N3 N 0.4866(2) 0.4654(2) 0.0963(2) 0.0420(10) Uani 1 d . . N4 N 0.5277(2) 0.4498(2) 0.0757(2) 0.0508(12) Uani 1 d . . N5 N 0.3561(2) 1.1581(2) 0.1036(2) 0.0368(11) Uani 1 d . . N6 N 0.3001(2) 1.1654(2) 0.0981(2) 0.0492(13) Uani 1 d . . N7 N 0.34013(15) 0.9631(2) 0.2009(2) 0.0488(12) Uani 1 d . . N8 N 0.3111(2) 0.9423(2) 0.2327(2) 0.0588(14) Uani 1 d . . C1 C 0.4235(2) 0.6466(2) 0.1366(2) 0.0273(9) Uani 1 d . . C2 C 0.4634(2) 0.6510(2) 0.1112(2) 0.0315(10) Uani 1 d . . C3 C 0.5214(2) 0.6429(2) 0.1434(2) 0.0308(10) Uani 1 d . . C4 C 0.4317(2) 0.6690(2) 0.0545(2) 0.0371(10) Uani 1 d . . C5 C 0.4482(2) 0.6787(3) 0.0076(2) 0.0550(13) Uani 1 d . . H5A H 0.4627(13) 0.6404(5) -0.0007(9) 0.082 Uiso 1 calc R . H5B H 0.4768(10) 0.7103(12) 0.0166(5) 0.082 Uiso 1 calc R . H5C H 0.4161(4) 0.6917(16) -0.0238(4) 0.082 Uiso 1 calc R . C6 C 0.5646(2) 0.6529(3) 0.1187(3) 0.054(2) Uani 1 d . . C7 C 0.3183(2) 0.6642(2) 0.0983(2) 0.0306(12) Uani 1 d . . C8 C 0.2814(2) 0.7101(2) 0.0688(2) 0.0385(11) Uani 1 d . . H8 H 0.2926(2) 0.7393(2) 0.0489(2) 0.046 Uiso 1 calc R . C9 C 0.2276(2) 0.7122(3) 0.0690(2) 0.0491(13) Uani 1 d . . H9 H 0.2022(2) 0.7425(3) 0.0489(2) 0.059 Uiso 1 calc R . C10 C 0.2123(2) 0.6692(3) 0.0993(2) 0.0570(15) Uani 1 d . . H10 H 0.1763(2) 0.6704(3) 0.0995(2) 0.068 Uiso 1 calc R . C11 C 0.2494(2) 0.6243(3) 0.1293(2) 0.0557(15) Uani 1 d . . H11 H 0.2387(2) 0.5958(3) 0.1500(2) 0.067 Uiso 1 calc R . C12 C 0.3031(2) 0.6215(2) 0.1288(2) 0.0408(12) Uani 1 d . . H12 H 0.3284(2) 0.5911(2) 0.1488(2) 0.049 Uiso 1 calc R . C13 C 0.5077(2) 0.4880(2) 0.1479(2) 0.0314(10) Uani 1 d . . C14 C 0.5682(2) 0.4868(2) 0.1638(3) 0.0405(14) Uani 1 d . . C15 C 0.6030(2) 0.5020(2) 0.2186(2) 0.0336(13) Uani 1 d . . C16 C 0.5760(2) 0.4630(3) 0.1157(3) 0.0530(15) Uani 1 d . . C17 C 0.6284(2) 0.4540(3) 0.1044(3) 0.089(2) Uani 1 d . . H17A H 0.6520(10) 0.4235(17) 0.1293(14) 0.134 Uiso 1 calc R . H17B H 0.6483(11) 0.4929(6) 0.1094(20) 0.134 Uiso 1 calc R . H17C H 0.6185(3) 0.4400(23) 0.0673(7) 0.134 Uiso 1 calc R . C18 C 0.6674(2) 0.4916(3) 0.2372(3) 0.054(2) Uani 1 d . . C19 C 0.4292(2) 0.4521(2) 0.0629(2) 0.0439(12) Uani 1 d . . C20 C 0.4165(2) 0.3994(3) 0.0301(2) 0.064(2) Uani 1 d . . H20 H 0.4449(2) 0.3735(3) 0.0285(2) 0.077 Uiso 1 calc R . C21 C 0.3606(3) 0.3863(3) -0.0004(3) 0.082(2) Uani 1 d . . H21 H 0.3514(3) 0.3502(3) -0.0214(3) 0.099 Uiso 1 calc R . C22 C 0.3190(2) 0.4243(4) -0.0004(3) 0.083(2) Uani 1 d . . H22 H 0.2820(2) 0.4163(4) -0.0235(3) 0.099 Uiso 1 calc R . C23 C 0.3315(3) 0.4747(4) 0.0337(3) 0.101(3) Uani 1 d . . H23 H 0.3027(3) 0.4991(4) 0.0362(3) 0.121 Uiso 1 calc R . C24 C 0.3876(2) 0.4898(3) 0.0651(3) 0.072(2) Uani 1 d . . H24 H 0.3963(2) 0.5251(3) 0.0871(3) 0.087 Uiso 1 calc R . C25 C 0.3906(2) 1.1464(2) 0.1581(2) 0.0319(10) Uani 1 d . . C26 C 0.3547(2) 1.1470(2) 0.1878(2) 0.0313(10) Uani 1 d . . C27 C 0.3768(2) 1.1396(2) 0.2449(2) 0.0327(11) Uani 1 d . . C28 C 0.2988(2) 1.1582(2) 0.1464(2) 0.0417(13) Uani 1 d . . C29 C 0.2428(2) 1.1615(3) 0.1520(3) 0.075(2) Uani 1 d . . H29A H 0.2441(6) 1.1931(15) 0.1783(14) 0.112 Uiso 1 calc R . H29B H 0.2346(9) 1.1219(7) 0.1642(18) 0.112 Uiso 1 calc R . H29C H 0.2140(3) 1.1717(21) 0.1171(5) 0.112 Uiso 1 calc R . C30 C 0.3397(2) 1.1436(3) 0.2778(2) 0.0499(14) Uani 1 d . . C31 C 0.3702(2) 1.1623(2) 0.0573(2) 0.044(2) Uani 1 d . . C32 C 0.4131(2) 1.1279(3) 0.0533(2) 0.058(2) Uani 1 d . . H32 H 0.4336(2) 1.1012(3) 0.0817(2) 0.070 Uiso 1 calc R . C33 C 0.4261(3) 1.1324(3) 0.0071(3) 0.080(2) Uani 1 d . . H33 H 0.4552(3) 1.1085(3) 0.0048(3) 0.095 Uiso 1 calc R . C34 C 0.3967(3) 1.1719(3) -0.0353(2) 0.079(2) Uani 1 d . . H34 H 0.4064(3) 1.1758(3) -0.0657(2) 0.095 Uiso 1 calc R . C35 C 0.3530(3) 1.2052(3) -0.0320(3) 0.086(2) Uani 1 d . . H35 H 0.3321(3) 1.2309(3) -0.0612(3) 0.103 Uiso 1 calc R . C36 C 0.3389(3) 1.2017(3) 0.0142(2) 0.066(2) Uani 1 d . . H36 H 0.3095(3) 1.2252(3) 0.0163(2) 0.079 Uiso 1 calc R . C37 C 0.3916(2) 0.9877(2) 0.2337(2) 0.0405(13) Uani 1 d . . C38 C 0.3948(2) 0.9830(2) 0.2883(3) 0.0439(15) Uani 1 d . . C39 C 0.4449(2) 1.0021(2) 0.3333(2) 0.0405(13) Uani 1 d . . C40 C 0.3424(2) 0.9536(3) 0.2847(3) 0.057(2) Uani 1 d . . C41 C 0.3207(2) 0.9370(3) 0.3269(3) 0.083(2) Uani 1 d . . H41A H 0.3200(18) 0.9734(6) 0.3478(12) 0.125 Uiso 1 calc R . H41B H 0.3446(12) 0.9060(16) 0.3509(12) 0.125 Uiso 1 calc R . H41C H 0.2833(8) 0.9207(20) 0.3096(3) 0.125 Uiso 1 calc R . C42 C 0.4496(3) 0.9918(3) 0.3922(3) 0.065(2) Uani 1 d . . C43 C 0.3180(2) 0.9525(2) 0.1428(2) 0.0485(14) Uani 1 d . . C44 C 0.3336(2) 0.9890(2) 0.1083(3) 0.059(2) Uani 1 d . . H44 H 0.3574(2) 1.0228(2) 0.1225(3) 0.071 Uiso 1 calc R . C45 C 0.3142(3) 0.9757(3) 0.0520(3) 0.073(2) Uani 1 d . . H45 H 0.3251(3) 1.0006(3) 0.0289(3) 0.087 Uiso 1 calc R . C46 C 0.2789(3) 0.9258(3) 0.0311(3) 0.084(2) Uani 1 d . . H46 H 0.2669(3) 0.9158(3) -0.0060(3) 0.101 Uiso 1 calc R . C47 C 0.2615(2) 0.8906(3) 0.0655(4) 0.096(3) Uani 1 d . . H47 H 0.2364(2) 0.8580(3) 0.0508(4) 0.115 Uiso 1 calc R . C48 C 0.2806(2) 0.9023(3) 0.1216(3) 0.075(2) Uani 1 d . . H48 H 0.2690(2) 0.8778(3) 0.1445(3) 0.090 Uiso 1 calc R . N9 N 0.5000 0.3212(3) 0.2500 0.059(2) Uani 1 d S . C49 C 0.4503(2) 0.3635(2) 0.2196(2) 0.0548(15) Uani 1 d . . H49A H 0.4594(2) 0.3886(2) 0.1935(2) 0.066 Uiso 1 calc R . H49B H 0.4447(2) 0.3916(2) 0.2458(2) 0.066 Uiso 1 calc R . C50 C 0.6050(2) 0.3280(3) 0.3113(3) 0.089(2) Uani 1 d . . C51 C 0.6485(3) 0.3724(3) 0.3469(3) 0.097(2) Uani 1 d . . H51A H 0.6360(3) 0.3888(3) 0.3747(3) 0.117 Uiso 1 calc R . H51B H 0.6511(3) 0.4072(3) 0.3245(3) 0.117 Uiso 1 calc R . C52 C 0.2061(3) 1.1552(4) -0.1249(4) 0.114(3) Uani 1 d . . H52A H 0.2038(5) 1.1910(19) -0.1040(22) 0.171 Uiso 1 calc R . H52B H 0.2206(12) 1.1675(28) -0.1520(4) 0.171 Uiso 1 calc R . H52C H 0.2306(8) 1.1248(11) -0.1008(21) 0.171 Uiso 1 calc R . C53 C 0.5129(3) 1.2796(2) 0.2094(3) 0.071(2) Uani 1 d . . H53A H 0.4815(3) 1.2515(2) 0.1922(3) 0.085 Uiso 1 calc R . H53B H 0.5457(3) 1.2544(2) 0.2294(3) 0.085 Uiso 1 calc R . C54 C 0.5240(4) 0.3168(4) 0.1641(4) 0.120(3) Uani 1 d . . H54A H 0.5468(4) 0.3529(4) 0.1806(4) 0.143 Uiso 1 calc R . H54B H 0.4885(4) 0.3315(4) 0.1373(4) 0.143 Uiso 1 calc R . C55 C 0.4457(6) 1.2773(4) 0.3659(4) 0.173(6) Uani 1 d . . H55A H 0.4337(6) 1.3050(4) 0.3885(4) 0.207 Uiso 1 calc R . H55B H 0.4122(6) 1.2591(4) 0.3385(4) 0.207 Uiso 1 calc R . C56 C 0.4764(5) 1.2321(5) 0.3974(5) 0.177(5) Uani 1 d . . H56A H 0.4840(36) 1.2011(24) 0.3748(6) 0.265 Uiso 1 calc R . H56B H 0.4563(19) 1.2133(32) 0.4175(31) 0.265 Uiso 1 calc R . H56C H 0.5113(19) 1.2489(10) 0.4226(29) 0.265 Uiso 1 calc R . N10 N 0.5000 0.8176(3) 0.2500 0.055(2) Uani 0.70(2) d SP 1 C57 C 0.4800(2) 0.8604(2) 0.1999(2) 0.053(2) Uani 1 d . 1 H57A H 0.4485(2) 0.8848(2) 0.2006(2) 0.064 Uiso 1 calc R 1 H57B H 0.5101(2) 0.8892(2) 0.2030(2) 0.064 Uiso 1 calc R 1 C58 C 0.4620(2) 0.8277(3) 0.1448(3) 0.083(2) Uani 1 d . 1 H58A H 0.4948(2) 0.8109(3) 0.1401(3) 0.100 Uiso 1 calc R 1 H58B H 0.4373(2) 0.7932(3) 0.1440(3) 0.100 Uiso 1 calc R 1 C59 C 0.5682(3) 0.8720(3) 0.4017(3) 0.077(2) Uani 1 d . 1 H59A H 0.5461(3) 0.9099(3) 0.3960(3) 0.093 Uiso 1 calc R 1 H59B H 0.6039(3) 0.8831(3) 0.3997(3) 0.093 Uiso 1 calc R 1 C60 C 0.5795(3) 0.8482(3) 0.4593(3) 0.093(2) Uani 1 d . 1 H60A H 0.5970(19) 0.8805(8) 0.4855(3) 0.140 Uiso 1 calc R 1 H60B H 0.6040(17) 0.8127(14) 0.4668(8) 0.140 Uiso 1 calc R 1 H60C H 0.5447(4) 0.8364(22) 0.4618(7) 0.140 Uiso 1 calc R 1 C61 C 0.5475(2) 0.7756(2) 0.2500(3) 0.083(2) Uani 0.70(2) d P 1 H61A H 0.5590(2) 0.7498(2) 0.2827(3) 0.099 Uiso 0.70(2) calc PR 1 H61B H 0.5328(2) 0.7481(2) 0.2185(3) 0.099 Uiso 0.70(2) calc PR 1 C62 C 0.5987(2) 0.8076(3) 0.2483(3) 0.069(2) Uani 0.70(2) d P 1 H62A H 0.6111(2) 0.8410(3) 0.2751(3) 0.083 Uiso 0.70(2) calc PR 1 H62B H 0.5917(2) 0.8244(3) 0.2121(3) 0.083 Uiso 0.70(2) calc PR 1 C63 C 0.6419(4) 0.7544(5) 0.2628(6) 0.076(4) Uani 0.70(2) d P 1 H63A H 0.6531(4) 0.7435(5) 0.3013(6) 0.092 Uiso 0.70(2) calc PR 1 H63B H 0.6251(4) 0.7179(5) 0.2409(6) 0.092 Uiso 0.70(2) calc PR 1 C64 C 0.6910(5) 0.7734(6) 0.2523(6) 0.107(6) Uani 0.70(2) d P 1 H64A H 0.7188(16) 0.7410(19) 0.2639(34) 0.160 Uiso 0.70(2) calc PR 1 H64B H 0.7063(22) 0.8109(24) 0.2723(29) 0.160 Uiso 0.70(2) calc PR 1 H64C H 0.6804(9) 0.7808(39) 0.2137(7) 0.160 Uiso 0.70(2) calc PR 1 N10A N 0.5000 0.8176(3) 0.2500 0.055(2) Uani 0.30(2) d SP 2 C61A C 0.5475(2) 0.7756(2) 0.2500(3) 0.083(2) Uani 0.30(2) d P 2 H61C H 0.5590(7) 0.7498(8) 0.2827(9) 0.099 Uiso 0.30(2) calc PR 2 H61D H 0.5328(7) 0.7481(8) 0.2185(9) 0.099 Uiso 0.30(2) calc PR 2 C62A C 0.5987(2) 0.8076(3) 0.2483(3) 0.069(2) Uani 0.30(2) d P 2 H62C H 0.6186(7) 0.8234(8) 0.2852(9) 0.083 Uiso 0.30(2) calc PR 2 H62D H 0.5846(7) 0.8440(8) 0.2253(9) 0.083 Uiso 0.30(2) calc PR 2 C63A C 0.6470(7) 0.7792(8) 0.2298(9) 0.042(6) Uani 0.30(2) d P 2 H63C H 0.6314(7) 0.7680(8) 0.1912(9) 0.051 Uiso 0.30(2) calc PR 2 H63D H 0.6769(7) 0.8093(8) 0.2359(9) 0.051 Uiso 0.30(2) calc PR 2 C64A C 0.6691(8) 0.7215(11) 0.2656(8) 0.049(7) Uani 0.30(2) d P 2 H64D H 0.6935(40) 0.6986(31) 0.2526(30) 0.073 Uiso 0.30(2) calc PR 2 H64E H 0.6380(8) 0.6956(29) 0.2638(40) 0.073 Uiso 0.30(2) calc PR 2 H64F H 0.6895(43) 0.7341(11) 0.3030(11) 0.073 Uiso 0.30(2) calc PR 2 F1 F 0.56473(14) 0.7120(2) 0.1018(2) 0.0848(13) Uani 1 d . . F2 F 0.61640(12) 0.6414(2) 0.1547(2) 0.0710(11) Uani 1 d . . F3 F 0.55582(13) 0.6154(2) 0.07550(14) 0.0759(11) Uani 1 d . . F4 F 0.67849(12) 0.43176(15) 0.2311(2) 0.0642(10) Uani 1 d . . F5 F 0.68926(11) 0.5266(2) 0.2090(2) 0.0744(11) Uani 1 d . . F6 F 0.69360(10) 0.50503(15) 0.28992(15) 0.0686(10) Uani 1 d . . F7 F 0.31570(12) 1.1997(2) 0.27315(14) 0.0649(10) Uani 1 d . . F8 F 0.29852(11) 1.1012(2) 0.26135(14) 0.0675(9) Uani 1 d . . F9 F 0.36893(13) 1.1337(2) 0.33157(14) 0.0650(10) Uani 1 d . . F10 F 0.44581(13) 0.9320(2) 0.4029(2) 0.0850(13) Uani 1 d . . F11 F 0.4107(2) 1.0233(2) 0.4035(2) 0.1042(14) Uani 1 d . . F12 F 0.49998(14) 1.0112(2) 0.42810(14) 0.0879(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0188(2) 0.0245(2) 0.0248(2) 0.000 0.0039(2) 0.000 Eu2 0.0190(2) 0.0298(2) 0.0248(2) 0.000 0.0036(2) 0.000 O1 0.025(2) 0.034(2) 0.033(2) 0.0038(15) 0.0098(15) 0.0045(13) O2 0.0256(15) 0.030(2) 0.040(2) 0.0023(15) 0.0085(15) -0.0009(13) O3 0.0247(14) 0.035(2) 0.033(2) -0.0049(14) 0.0078(14) -0.0013(13) O4 0.024(2) 0.031(2) 0.038(2) -0.003(2) 0.0058(15) 0.0016(13) O5 0.025(2) 0.037(2) 0.028(2) 0.0029(15) 0.0070(14) -0.0012(13) O6 0.0239(15) 0.040(2) 0.028(2) 0.0017(14) 0.0044(14) 0.0000(13) O7 0.029(2) 0.037(2) 0.043(2) -0.002(2) 0.0097(15) -0.0046(14) O8 0.031(2) 0.047(2) 0.039(2) 0.012(2) 0.0076(15) 0.001(2) N1 0.027(2) 0.037(2) 0.030(3) 0.007(2) 0.008(2) 0.003(2) N2 0.043(2) 0.053(2) 0.022(2) 0.006(2) 0.013(2) 0.003(2) N3 0.043(2) 0.047(2) 0.035(2) -0.010(2) 0.013(2) -0.006(2) N4 0.053(3) 0.064(3) 0.042(3) -0.012(2) 0.026(2) -0.003(2) N5 0.035(2) 0.042(2) 0.023(2) 0.004(2) -0.001(2) -0.002(2) N6 0.029(2) 0.051(3) 0.051(3) 0.004(2) -0.003(2) 0.002(2) N7 0.026(2) 0.040(2) 0.073(3) 0.007(2) 0.011(2) -0.004(2) N8 0.031(2) 0.051(3) 0.085(4) 0.019(3) 0.012(2) -0.001(2) C1 0.029(2) 0.025(2) 0.023(2) 0.003(2) 0.004(2) 0.003(2) C2 0.029(2) 0.033(2) 0.028(2) -0.001(2) 0.007(2) 0.002(2) C3 0.034(2) 0.026(2) 0.034(3) 0.003(2) 0.014(2) 0.000(2) C4 0.036(2) 0.043(3) 0.031(2) 0.002(2) 0.012(2) 0.003(2) C5 0.051(3) 0.083(4) 0.031(3) 0.005(3) 0.016(2) 0.003(3) C6 0.043(3) 0.072(4) 0.052(4) 0.020(3) 0.023(3) 0.006(3) C7 0.033(3) 0.038(3) 0.019(2) 0.000(2) 0.008(2) 0.003(2) C8 0.035(2) 0.047(3) 0.032(3) 0.009(2) 0.011(2) 0.006(2) C9 0.036(3) 0.065(3) 0.043(3) 0.014(3) 0.011(2) 0.018(2) C10 0.030(2) 0.086(4) 0.056(3) 0.021(3) 0.017(2) 0.014(3) C11 0.047(3) 0.068(4) 0.054(4) 0.026(3) 0.022(3) 0.005(3) C12 0.034(2) 0.053(3) 0.031(3) 0.008(2) 0.008(2) 0.002(2) C13 0.034(2) 0.026(2) 0.031(3) -0.002(2) 0.009(2) -0.002(2) C14 0.033(3) 0.034(3) 0.060(4) -0.009(3) 0.024(3) -0.008(2) C15 0.022(2) 0.026(2) 0.054(4) -0.005(2) 0.015(2) -0.001(2) C16 0.055(3) 0.060(4) 0.057(4) -0.025(3) 0.036(3) -0.011(3) C17 0.070(4) 0.119(6) 0.105(6) -0.052(5) 0.063(4) -0.019(4) C18 0.034(3) 0.050(3) 0.077(5) -0.019(3) 0.020(3) -0.001(2) C19 0.046(3) 0.047(3) 0.030(3) -0.006(2) 0.005(2) -0.001(2) C20 0.059(3) 0.080(4) 0.051(4) -0.034(3) 0.018(3) -0.010(3) C21 0.078(4) 0.093(5) 0.058(4) -0.039(4) 0.006(3) -0.016(4) C22 0.052(3) 0.114(6) 0.054(4) -0.032(4) -0.012(3) -0.004(4) C23 0.057(4) 0.108(6) 0.089(6) -0.036(5) -0.027(4) 0.029(4) C24 0.055(3) 0.062(4) 0.066(4) -0.027(3) -0.015(3) 0.008(3) C25 0.034(2) 0.026(2) 0.028(2) 0.003(2) 0.002(2) -0.003(2) C26 0.023(2) 0.036(2) 0.028(3) 0.002(2) 0.003(2) -0.004(2) C27 0.024(2) 0.030(2) 0.045(3) 0.001(2) 0.014(2) 0.001(2) C28 0.030(2) 0.046(3) 0.036(3) 0.001(2) -0.002(2) 0.004(2) C29 0.017(2) 0.116(6) 0.075(4) 0.000(4) -0.002(2) 0.004(3) C30 0.032(3) 0.064(3) 0.057(4) 0.000(3) 0.020(3) 0.012(3) C31 0.053(3) 0.037(3) 0.028(3) 0.006(2) 0.000(3) -0.006(2) C32 0.083(4) 0.059(4) 0.030(3) 0.001(3) 0.018(3) 0.018(3) C33 0.122(6) 0.078(5) 0.047(4) 0.002(4) 0.041(4) 0.019(4) C34 0.141(6) 0.060(4) 0.041(3) 0.003(4) 0.039(4) 0.004(5) C35 0.127(6) 0.065(4) 0.037(4) 0.021(3) 0.000(4) 0.000(4) C36 0.076(4) 0.069(4) 0.037(3) 0.018(3) 0.003(3) 0.004(3) C37 0.023(2) 0.032(3) 0.055(4) 0.008(2) 0.002(2) -0.004(2) C38 0.032(3) 0.035(3) 0.061(4) 0.013(3) 0.014(3) 0.000(2) C39 0.039(3) 0.047(3) 0.037(3) 0.016(2) 0.017(2) 0.003(2) C40 0.038(3) 0.056(4) 0.079(5) 0.023(3) 0.026(3) 0.003(3) C41 0.038(3) 0.100(5) 0.111(6) 0.051(5) 0.027(3) 0.002(3) C42 0.054(4) 0.082(5) 0.062(4) 0.025(4) 0.024(3) -0.010(3) C43 0.025(2) 0.038(3) 0.063(4) -0.006(3) -0.005(2) 0.000(2) C44 0.048(3) 0.041(3) 0.064(4) -0.006(3) -0.006(3) -0.003(2) C45 0.068(4) 0.053(3) 0.062(5) -0.013(3) -0.014(3) 0.002(3) C46 0.074(4) 0.052(4) 0.078(5) -0.012(4) -0.025(4) 0.009(4) C47 0.056(4) 0.055(4) 0.112(7) -0.017(4) -0.041(4) -0.017(3) C48 0.044(3) 0.049(3) 0.099(6) 0.007(3) -0.011(3) -0.007(3) N9 0.082(5) 0.026(3) 0.073(6) 0.000 0.035(5) 0.000 C49 0.079(4) 0.029(3) 0.062(4) 0.004(3) 0.033(3) 0.006(3) C50 0.060(3) 0.063(4) 0.121(6) -0.012(5) 0.008(4) 0.005(4) C51 0.096(5) 0.078(5) 0.095(6) 0.017(4) 0.012(5) 0.008(4) C52 0.072(4) 0.112(7) 0.136(8) -0.029(6) 0.015(5) -0.005(4) C53 0.090(4) 0.031(3) 0.093(5) -0.011(3) 0.036(4) 0.005(3) C54 0.194(9) 0.100(6) 0.103(6) -0.022(6) 0.100(7) 0.016(7) C55 0.363(18) 0.080(6) 0.087(7) 0.014(5) 0.100(10) -0.039(9) C56 0.234(14) 0.141(10) 0.136(11) 0.020(9) 0.048(10) 0.009(10) N10 0.033(3) 0.016(3) 0.096(6) 0.000 0.002(4) 0.000 C57 0.041(3) 0.020(2) 0.085(4) 0.002(3) 0.008(3) 0.002(2) C58 0.067(3) 0.052(3) 0.097(5) -0.009(4) -0.006(3) 0.014(3) C59 0.068(4) 0.058(4) 0.084(5) 0.002(4) 0.006(4) -0.001(3) C60 0.083(5) 0.087(5) 0.082(5) 0.020(4) 0.002(4) -0.008(4) C61 0.053(3) 0.026(3) 0.127(6) -0.016(3) -0.013(4) 0.016(2) C62 0.049(3) 0.071(4) 0.076(4) -0.017(3) 0.011(3) 0.027(3) C63 0.057(6) 0.049(6) 0.108(10) -0.010(6) 0.014(6) 0.014(5) C64 0.058(7) 0.092(9) 0.158(12) -0.045(9) 0.027(7) 0.025(6) N10A 0.033(3) 0.016(3) 0.096(6) 0.000 0.002(4) 0.000 C61A 0.053(3) 0.026(3) 0.127(6) -0.016(3) -0.013(4) 0.016(2) C62A 0.049(3) 0.071(4) 0.076(4) -0.017(3) 0.011(3) 0.027(3) C63A 0.026(10) 0.039(10) 0.064(13) 0.031(10) 0.020(9) 0.006(7) C64A 0.032(10) 0.057(15) 0.052(12) 0.012(10) 0.012(8) 0.015(10) F1 0.062(2) 0.092(3) 0.106(3) 0.052(2) 0.038(2) -0.005(2) F2 0.031(2) 0.113(3) 0.073(3) 0.025(2) 0.025(2) 0.005(2) F3 0.062(2) 0.126(3) 0.053(2) 0.009(2) 0.037(2) 0.027(2) F4 0.040(2) 0.052(2) 0.093(3) -0.021(2) 0.017(2) 0.0098(15) F5 0.039(2) 0.077(2) 0.117(3) -0.010(2) 0.041(2) -0.017(2) F6 0.0279(13) 0.080(2) 0.082(3) -0.033(2) 0.0030(15) 0.0042(14) F7 0.051(2) 0.079(2) 0.067(2) -0.008(2) 0.025(2) 0.025(2) F8 0.036(2) 0.094(2) 0.082(2) 0.000(2) 0.032(2) -0.013(2) F9 0.048(2) 0.109(3) 0.045(2) 0.008(2) 0.026(2) 0.015(2) F10 0.057(2) 0.110(3) 0.076(3) 0.062(3) 0.013(2) -0.011(2) F11 0.100(3) 0.156(4) 0.078(3) 0.030(3) 0.058(2) 0.023(3) F12 0.081(2) 0.135(3) 0.043(2) 0.018(2) 0.019(2) -0.032(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.331(3) . ? Eu1 O3 2.331(3) 2_655 ? Eu1 O1 2.363(3) 2_655 ? Eu1 O1 2.363(3) . ? Eu1 O2 2.441(3) . ? Eu1 O2 2.441(3) 2_655 ? Eu1 O4 2.462(3) . ? Eu1 O4 2.462(3) 2_655 ? Eu2 O7 2.315(3) . ? Eu2 O7 2.315(3) 2_655 ? Eu2 O5 2.366(3) . ? Eu2 O5 2.366(3) 2_655 ? Eu2 O6 2.436(3) 2_655 ? Eu2 O6 2.436(3) . ? Eu2 O8 2.474(3) 2_655 ? Eu2 O8 2.474(3) . ? O1 C1 1.270(5) . ? O2 C3 1.260(5) . ? O3 C13 1.269(5) . ? O4 C15 1.232(6) . ? O5 C25 1.276(5) . ? O6 C27 1.265(5) . ? O7 C37 1.268(6) . ? O8 C39 1.243(6) . ? N1 C1 1.366(5) . ? N1 N2 1.395(6) . ? N1 C7 1.435(6) . ? N2 C4 1.325(5) . ? N3 C13 1.346(6) . ? N3 N4 1.402(6) . ? N3 C19 1.431(6) . ? N4 C16 1.318(7) . ? N5 C25 1.391(6) . ? N5 N6 1.401(5) . ? N5 C31 1.404(7) . ? N6 C28 1.295(7) . ? N7 C37 1.380(6) . ? N7 N8 1.394(6) . ? N7 C43 1.433(7) . ? N8 C40 1.318(8) . ? C1 C2 1.429(6) . ? C2 C3 1.418(6) . ? C2 C4 1.452(6) . ? C3 C6 1.506(7) . ? C4 C5 1.469(6) . ? C6 F2 1.330(6) . ? C6 F3 1.340(7) . ? C6 F1 1.344(6) . ? C7 C12 1.371(7) . ? C7 C8 1.381(6) . ? C8 C9 1.389(6) . ? C9 C10 1.375(7) . ? C10 C11 1.373(7) . ? C11 C12 1.389(7) . ? C13 C14 1.451(6) . ? C14 C15 1.416(8) . ? C14 C16 1.451(8) . ? C15 C18 1.554(6) . ? C16 C17 1.502(7) . ? C18 F6 1.322(7) . ? C18 F5 1.326(7) . ? C18 F4 1.338(6) . ? C19 C24 1.361(7) . ? C19 C20 1.385(7) . ? C20 C21 1.384(8) . ? C21 C22 1.346(9) . ? C22 C23 1.362(9) . ? C23 C24 1.400(8) . ? C25 C26 1.422(6) . ? C26 C27 1.399(6) . ? C26 C28 1.455(6) . ? C27 C30 1.518(7) . ? C28 C29 1.508(7) . ? C30 F7 1.337(6) . ? C30 F8 1.338(6) . ? C30 F9 1.343(6) . ? C31 C32 1.366(7) . ? C31 C36 1.397(7) . ? C32 C33 1.384(8) . ? C33 C34 1.375(8) . ? C34 C35 1.364(9) . ? C35 C36 1.400(9) . ? C37 C38 1.413(8) . ? C38 C39 1.436(7) . ? C38 C40 1.460(7) . ? C39 C42 1.525(8) . ? C40 C41 1.468(9) . ? C42 F10 1.326(7) . ? C42 F11 1.334(7) . ? C42 F12 1.346(7) . ? C43 C44 1.370(8) . ? C43 C48 1.411(7) . ? C44 C45 1.401(9) . ? C45 C46 1.378(8) . ? C46 C47 1.381(11) . ? C47 C48 1.391(11) . ? N9 C49 1.522(6) 2_655 ? N9 C49 1.522(6) . ? N9 C53 1.525(7) 1_545 ? N9 C53 1.525(7) 2_645 ? C49 C50 1.544(7) 2_655 ? C50 C51 1.496(9) . ? C50 C49 1.544(7) 2_655 ? C51 C52 1.504(9) 8_566 ? C52 C51 1.504(9) 8_465 ? C53 N9 1.525(7) 1_565 ? C53 C54 1.552(10) 1_565 ? C54 C53 1.552(10) 1_545 ? C54 C55 1.556(11) 2_645 ? C55 C56 1.325(13) . ? C55 C54 1.556(11) 2_665 ? N10 C61 1.519(6) . ? N10 C61 1.519(6) 2_655 ? N10 C57 1.527(6) . ? N10 C57 1.527(6) 2_655 ? C57 C58 1.516(8) . ? C58 C59 1.511(8) 2_655 ? C59 C58 1.511(8) 2_655 ? C59 C60 1.519(9) . ? C61 C62 1.504(8) . ? C62 C63 1.536(11) . ? C63 C64 1.45(2) . ? N10A C61A 1.519(6) . ? N10A C61A 1.519(6) 2_655 ? C61A C62A 1.504(8) . ? C62A C63A 1.62(2) . ? C63A C64A 1.53(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O3 103.33(15) . 2_655 ? O3 Eu1 O1 145.21(10) . 2_655 ? O3 Eu1 O1 82.81(10) 2_655 2_655 ? O3 Eu1 O1 82.81(10) . . ? O3 Eu1 O1 145.21(10) 2_655 . ? O1 Eu1 O1 111.73(15) 2_655 . ? O3 Eu1 O2 79.17(10) . . ? O3 Eu1 O2 143.87(9) 2_655 . ? O1 Eu1 O2 76.61(11) 2_655 . ? O1 Eu1 O2 70.79(10) . . ? O3 Eu1 O2 143.87(9) . 2_655 ? O3 Eu1 O2 79.17(10) 2_655 2_655 ? O1 Eu1 O2 70.79(10) 2_655 2_655 ? O1 Eu1 O2 76.61(11) . 2_655 ? O2 Eu1 O2 120.05(14) . 2_655 ? O3 Eu1 O4 71.44(10) . . ? O3 Eu1 O4 76.77(11) 2_655 . ? O1 Eu1 O4 76.96(10) 2_655 . ? O1 Eu1 O4 136.11(11) . . ? O2 Eu1 O4 69.89(10) . . ? O2 Eu1 O4 141.69(10) 2_655 . ? O3 Eu1 O4 76.77(11) . 2_655 ? O3 Eu1 O4 71.44(10) 2_655 2_655 ? O1 Eu1 O4 136.11(11) 2_655 2_655 ? O1 Eu1 O4 76.96(10) . 2_655 ? O2 Eu1 O4 141.69(10) . 2_655 ? O2 Eu1 O4 69.89(10) 2_655 2_655 ? O4 Eu1 O4 127.64(13) . 2_655 ? O7 Eu2 O7 99.12(14) . 2_655 ? O7 Eu2 O5 82.94(10) . . ? O7 Eu2 O5 147.75(12) 2_655 . ? O7 Eu2 O5 147.75(12) . 2_655 ? O7 Eu2 O5 82.94(10) 2_655 2_655 ? O5 Eu2 O5 112.28(15) . 2_655 ? O7 Eu2 O6 141.08(11) . 2_655 ? O7 Eu2 O6 79.67(10) 2_655 2_655 ? O5 Eu2 O6 79.00(10) . 2_655 ? O5 Eu2 O6 71.12(11) 2_655 2_655 ? O7 Eu2 O6 79.67(10) . . ? O7 Eu2 O6 141.08(11) 2_655 . ? O5 Eu2 O6 71.12(11) . . ? O5 Eu2 O6 79.00(10) 2_655 . ? O6 Eu2 O6 125.03(13) 2_655 . ? O7 Eu2 O8 74.21(11) . 2_655 ? O7 Eu2 O8 72.09(11) 2_655 2_655 ? O5 Eu2 O8 77.67(11) . 2_655 ? O5 Eu2 O8 135.34(10) 2_655 2_655 ? O6 Eu2 O8 68.41(10) 2_655 2_655 ? O6 Eu2 O8 141.30(9) . 2_655 ? O7 Eu2 O8 72.09(11) . . ? O7 Eu2 O8 74.21(11) 2_655 . ? O5 Eu2 O8 135.34(10) . . ? O5 Eu2 O8 77.67(11) 2_655 . ? O6 Eu2 O8 141.30(10) 2_655 . ? O6 Eu2 O8 68.41(10) . . ? O8 Eu2 O8 126.9(2) 2_655 . ? C1 O1 Eu1 128.0(3) . . ? C3 O2 Eu1 132.8(3) . . ? C13 O3 Eu1 130.8(3) . . ? C15 O4 Eu1 132.0(3) . . ? C25 O5 Eu2 125.7(3) . . ? C27 O6 Eu2 130.3(3) . . ? C37 O7 Eu2 130.8(3) . . ? C39 O8 Eu2 133.2(3) . . ? C1 N1 N2 112.5(4) . . ? C1 N1 C7 129.2(4) . . ? N2 N1 C7 118.2(4) . . ? C4 N2 N1 106.9(4) . . ? C13 N3 N4 113.9(4) . . ? C13 N3 C19 127.9(4) . . ? N4 N3 C19 118.1(4) . . ? C16 N4 N3 105.1(4) . . ? C25 N5 N6 110.6(4) . . ? C25 N5 C31 129.2(4) . . ? N6 N5 C31 120.2(4) . . ? C28 N6 N5 107.4(4) . . ? C37 N7 N8 110.7(5) . . ? C37 N7 C43 128.5(5) . . ? N8 N7 C43 120.5(4) . . ? C40 N8 N7 108.0(4) . . ? O1 C1 N1 123.7(4) . . ? O1 C1 C2 131.5(4) . . ? N1 C1 C2 104.8(4) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C4 134.1(4) . . ? C1 C2 C4 106.2(3) . . ? O2 C3 C2 123.6(4) . . ? O2 C3 C6 115.8(4) . . ? C2 C3 C6 120.5(4) . . ? N2 C4 C2 109.5(4) . . ? N2 C4 C5 118.2(4) . . ? C2 C4 C5 132.3(4) . . ? F2 C6 F3 107.0(5) . . ? F2 C6 F1 106.4(5) . . ? F3 C6 F1 107.8(5) . . ? F2 C6 C3 111.8(5) . . ? F3 C6 C3 111.7(5) . . ? F1 C6 C3 111.9(5) . . ? C12 C7 C8 121.1(5) . . ? C12 C7 N1 120.4(4) . . ? C8 C7 N1 118.4(4) . . ? C7 C8 C9 119.5(5) . . ? C10 C9 C8 119.3(4) . . ? C11 C10 C9 120.9(4) . . ? C10 C11 C12 120.1(5) . . ? C7 C12 C11 119.0(5) . . ? O3 C13 N3 125.3(4) . . ? O3 C13 C14 129.7(4) . . ? N3 C13 C14 105.0(4) . . ? C15 C14 C16 136.6(5) . . ? C15 C14 C13 118.8(5) . . ? C16 C14 C13 104.3(5) . . ? O4 C15 C14 126.6(4) . . ? O4 C15 C18 115.3(5) . . ? C14 C15 C18 118.1(5) . . ? N4 C16 C14 111.7(5) . . ? N4 C16 C17 117.4(5) . . ? C14 C16 C17 130.9(5) . . ? F6 C18 F5 108.1(4) . . ? F6 C18 F4 106.8(5) . . ? F5 C18 F4 108.6(5) . . ? F6 C18 C15 110.7(5) . . ? F5 C18 C15 111.9(5) . . ? F4 C18 C15 110.5(4) . . ? C24 C19 C20 120.7(5) . . ? C24 C19 N3 120.1(4) . . ? C20 C19 N3 119.1(5) . . ? C21 C20 C19 118.1(6) . . ? C22 C21 C20 122.0(6) . . ? C21 C22 C23 119.5(5) . . ? C22 C23 C24 120.2(6) . . ? C19 C24 C23 119.3(6) . . ? O5 C25 N5 123.2(4) . . ? O5 C25 C26 130.8(4) . . ? N5 C25 C26 105.9(4) . . ? C27 C26 C25 120.7(4) . . ? C27 C26 C28 134.6(4) . . ? C25 C26 C28 104.7(4) . . ? O6 C27 C26 124.0(4) . . ? O6 C27 C30 114.6(4) . . ? C26 C27 C30 121.5(4) . . ? N6 C28 C26 111.5(4) . . ? N6 C28 C29 118.4(4) . . ? C26 C28 C29 130.1(5) . . ? F7 C30 F8 107.6(4) . . ? F7 C30 F9 107.0(5) . . ? F8 C30 F9 106.7(5) . . ? F7 C30 C27 111.7(5) . . ? F8 C30 C27 111.8(4) . . ? F9 C30 C27 111.9(4) . . ? C32 C31 C36 119.8(6) . . ? C32 C31 N5 121.3(5) . . ? C36 C31 N5 118.9(5) . . ? C31 C32 C33 120.4(6) . . ? C34 C33 C32 120.9(7) . . ? C35 C34 C33 118.9(6) . . ? C34 C35 C36 121.5(6) . . ? C31 C36 C35 118.6(6) . . ? O7 C37 N7 122.5(5) . . ? O7 C37 C38 131.3(4) . . ? N7 C37 C38 106.1(4) . . ? C37 C38 C39 120.3(5) . . ? C37 C38 C40 105.8(5) . . ? C39 C38 C40 133.8(6) . . ? O8 C39 C38 124.2(5) . . ? O8 C39 C42 116.1(5) . . ? C38 C39 C42 119.7(5) . . ? N8 C40 C38 109.3(5) . . ? N8 C40 C41 118.8(5) . . ? C38 C40 C41 131.8(6) . . ? F10 C42 F11 108.7(5) . . ? F10 C42 F12 106.2(5) . . ? F11 C42 F12 106.9(6) . . ? F10 C42 C39 111.9(6) . . ? F11 C42 C39 112.4(5) . . ? F12 C42 C39 110.4(5) . . ? C44 C43 C48 120.3(6) . . ? C44 C43 N7 121.4(4) . . ? C48 C43 N7 118.3(6) . . ? C43 C44 C45 120.6(5) . . ? C46 C45 C44 119.7(7) . . ? C45 C46 C47 119.5(7) . . ? C46 C47 C48 121.9(6) . . ? C47 C48 C43 117.8(7) . . ? C49 N9 C49 106.8(6) 2_655 . ? C49 N9 C53 110.7(3) 2_655 1_545 ? C49 N9 C53 110.2(3) . 1_545 ? C49 N9 C53 110.2(3) 2_655 2_645 ? C49 N9 C53 110.7(3) . 2_645 ? C53 N9 C53 108.2(6) 1_545 2_645 ? N9 C49 C50 113.8(4) . 2_655 ? C51 C50 C49 109.5(5) . 2_655 ? C50 C51 C52 114.8(6) . 8_566 ? N9 C53 C54 113.1(5) 1_565 1_565 ? C53 C54 C55 112.8(7) 1_545 2_645 ? C56 C55 C54 114.9(13) . 2_665 ? C61 N10 C61 107.3(6) . 2_655 ? C61 N10 C57 111.2(4) . . ? C61 N10 C57 110.6(3) 2_655 . ? C61 N10 C57 110.6(3) . 2_655 ? C61 N10 C57 111.2(4) 2_655 2_655 ? C57 N10 C57 106.0(5) . 2_655 ? C58 C57 N10 115.3(4) . . ? C59 C58 C57 111.0(5) 2_655 . ? C58 C59 C60 116.2(6) 2_655 . ? C62 C61 N10 116.4(4) . . ? C61 C62 C63 102.3(6) . . ? C64 C63 C62 110.2(10) . . ? C61A N10A C61A 107.3(6) . 2_655 ? C62A C61A N10A 116.4(4) . . ? C61A C62A C63A 128.4(8) . . ? C64A C63A C62A 105.4(15) . . ? _refine_diff_density_max 0.516 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.060 data_Nd(Q')3.H2O.EtOH _database_code_CSD 170587 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H53 N6 Nd O8' _chemical_formula_weight 1082.28 _chemical_melting_point ? _chemical_compound_source ? 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1864(8) _cell_length_b 14.9116(9) _cell_length_c 15.1994(9) _cell_angle_alpha 87.835(8) _cell_angle_beta 66.550(10) _cell_angle_gamma 64.160(10) _cell_volume 2434.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _exptl_crystal_description ? _exptl_crystal_colour pale-violet _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method ? _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 1.130 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART(Bruker) _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21126 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.92 _reflns_number_total 11366 _reflns_number_observed 7327 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2630 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0571P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8736 _refine_ls_number_parameters 653 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_obs 0.0442 _refine_ls_wR_factor_all 0.1145 _refine_ls_wR_factor_obs 0.1018 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd Nd 0.20780(2) 0.31771(2) 0.187012(15) 0.02208(9) Uani 1 d . . O1 O 0.0961(2) 0.3351(2) 0.3585(2) 0.0216(6) Uani 1 d . . O2 O 0.2880(2) 0.3958(2) 0.2638(2) 0.0235(6) Uani 1 d . . O3 O 0.2705(2) 0.1641(2) 0.0912(2) 0.0243(6) Uani 1 d . . O4 O 0.3378(2) 0.1743(2) 0.2424(2) 0.0252(6) Uani 1 d . . O5 O 0.1847(2) 0.3724(2) 0.0407(2) 0.0223(6) Uani 1 d . . O6 O 0.0160(2) 0.3253(2) 0.1981(2) 0.0248(6) Uani 1 d . . O7 O 0.4193(2) 0.2867(2) 0.0675(2) 0.0248(6) Uani 1 d D . H1 H 0.4722(34) 0.2355(24) 0.0398(30) 0.030 Uiso 1 d D . O8 O 0.0744(3) 0.5026(2) 0.2194(2) 0.0244(6) Uani 1 d D . H2 H 0.0312(38) 0.5415(32) 0.1829(31) 0.029 Uiso 1 d . . H3 H 0.0347(37) 0.5329(30) 0.2712(21) 0.029 Uiso 1 d D . N1 N 0.0430(3) 0.3584(2) 0.5251(2) 0.0207(7) Uani 1 d . . N2 N 0.0693(3) 0.4022(2) 0.5879(2) 0.0230(7) Uani 1 d . . N3 N 0.1279(3) 0.3837(2) -0.0866(2) 0.0214(7) Uani 1 d . . N4 N 0.0427(3) 0.3683(2) -0.1091(2) 0.0239(7) Uani 1 d . . N5 N 0.3517(3) -0.0054(2) 0.0306(2) 0.0222(7) Uani 1 d . . N6 N 0.4161(3) -0.0999(2) 0.0521(2) 0.0246(8) Uani 1 d . . C1 C 0.1093(3) 0.3630(3) 0.4290(3) 0.0208(8) Uani 1 d . . C2 C 0.1852(3) 0.4071(3) 0.4323(3) 0.0209(8) Uani 1 d . . C3 C 0.2752(3) 0.4175(3) 0.3482(3) 0.0207(8) Uani 1 d . . C4 C 0.3657(4) 0.4505(3) 0.3549(3) 0.0236(9) Uani 1 d . . H4A H 0.3188(4) 0.5111(3) 0.4057(3) 0.028 Uiso 1 calc R . H4B H 0.4053(4) 0.4699(3) 0.2922(3) 0.028 Uiso 1 calc R . C5 C 0.4668(3) 0.3698(3) 0.3787(3) 0.0222(9) Uani 1 d . . C6 C 0.5397(4) 0.3956(3) 0.4076(3) 0.0263(9) Uani 1 d . . H6 H 0.5244(4) 0.4640(3) 0.4134(3) 0.032 Uiso 1 calc R . C7 C 0.6341(4) 0.3235(3) 0.4282(3) 0.0281(9) Uani 1 d . . H7 H 0.6842(4) 0.3424(3) 0.4462(3) 0.034 Uiso 1 calc R . C8 C 0.6554(4) 0.2237(3) 0.4225(3) 0.0293(10) Uani 1 d . . H8 H 0.7190(4) 0.1742(3) 0.4377(3) 0.035 Uiso 1 calc R . C9 C 0.5832(4) 0.1971(3) 0.3944(3) 0.0308(10) Uani 1 d . . H9 H 0.5975(4) 0.1288(3) 0.3901(3) 0.037 Uiso 1 calc R . C10 C 0.4898(4) 0.2693(3) 0.3726(3) 0.0276(9) Uani 1 d . . H10 H 0.4410(4) 0.2499(3) 0.3533(3) 0.033 Uiso 1 calc R . C11 C 0.1527(3) 0.4304(3) 0.5330(3) 0.0216(8) Uani 1 d . . C12 C 0.1915(4) 0.4863(3) 0.5812(3) 0.0242(9) Uani 1 d . . H12A H 0.1674(21) 0.5544(7) 0.5646(15) 0.036 Uiso 1 calc R . H12B H 0.2819(4) 0.4503(10) 0.5591(14) 0.036 Uiso 1 calc R . H12C H 0.1506(18) 0.4909(17) 0.6519(3) 0.036 Uiso 1 calc R . C13 C -0.0427(4) 0.3195(3) 0.5625(3) 0.0237(9) Uani 1 d . . C14 C -0.1193(4) 0.3406(3) 0.6620(3) 0.0295(10) Uani 1 d . . H14 H -0.1136(4) 0.3815(3) 0.7045(3) 0.035 Uiso 1 calc R . C15 C -0.2030(4) 0.3023(3) 0.6987(3) 0.0324(10) Uani 1 d . . H15 H -0.2550(4) 0.3174(3) 0.7664(3) 0.039 Uiso 1 calc R . C16 C -0.2128(4) 0.2422(3) 0.6388(3) 0.0325(10) Uani 1 d . . H16 H -0.2717(4) 0.2169(3) 0.6648(3) 0.039 Uiso 1 calc R . C17 C -0.1359(4) 0.2195(3) 0.5407(3) 0.0314(10) Uani 1 d . . H17 H -0.1408(4) 0.1773(3) 0.4989(3) 0.038 Uiso 1 calc R . C18 C -0.0517(4) 0.2579(3) 0.5029(3) 0.0274(9) Uani 1 d . . H18 H 0.0006(4) 0.2419(3) 0.4352(3) 0.033 Uiso 1 calc R . C19 C 0.3292(4) 0.0717(3) 0.0937(3) 0.0226(9) Uani 1 d . . C20 C 0.3830(3) 0.0246(3) 0.1588(3) 0.0222(9) Uani 1 d . . C21 C 0.3845(3) 0.0810(3) 0.2309(3) 0.0223(9) Uani 1 d . . C22 C 0.4430(4) 0.0295(3) 0.2992(3) 0.0263(9) Uani 1 d . . H22A H 0.4987(4) 0.0566(3) 0.3012(3) 0.032 Uiso 1 calc R . H22B H 0.4937(4) -0.0440(3) 0.2745(3) 0.032 Uiso 1 calc R . C23 C 0.3420(4) 0.0473(3) 0.4020(3) 0.0303(10) Uani 1 d . . C24 C 0.3339(5) 0.0973(5) 0.4746(4) 0.064(2) Uani 1 d . . H24 H 0.3943(5) 0.1200(5) 0.4636(4) 0.077 Uiso 1 calc R . C25 C 0.2362(5) 0.1198(4) 0.5718(3) 0.0509(14) Uani 1 d . . H25 H 0.2288(5) 0.1604(4) 0.6230(3) 0.061 Uiso 1 calc R . C26 C 0.1554(4) 0.0807(4) 0.5873(3) 0.0362(11) Uani 1 d . . H26 H 0.0917(4) 0.0922(4) 0.6505(3) 0.043 Uiso 1 calc R . C27 C 0.1665(4) 0.0247(4) 0.5116(4) 0.0387(11) Uani 1 d . . H27 H 0.1108(4) -0.0031(4) 0.5226(4) 0.046 Uiso 1 calc R . C28 C 0.2584(4) 0.0085(3) 0.4193(4) 0.0350(11) Uani 1 d . . H28 H 0.2645(4) -0.0296(3) 0.3671(4) 0.042 Uiso 1 calc R . C29 C 0.4344(4) -0.0812(3) 0.1275(3) 0.0245(9) Uani 1 d . . C30 C 0.5025(4) -0.1705(3) 0.1661(3) 0.0321(10) Uani 1 d . . H30A H 0.4529(13) -0.1633(11) 0.2359(5) 0.048 Uiso 1 calc R . H30B H 0.5827(12) -0.1742(13) 0.1554(19) 0.048 Uiso 1 calc R . H30C H 0.5166(24) -0.2324(4) 0.1323(15) 0.048 Uiso 1 calc R . C31 C 0.3119(3) -0.0009(3) -0.0443(3) 0.0214(8) Uani 1 d . . C32 C 0.2550(4) 0.0911(3) -0.0733(3) 0.0277(9) Uani 1 d . . H32 H 0.2456(4) 0.1516(3) -0.0451(3) 0.033 Uiso 1 calc R . C33 C 0.2122(4) 0.0929(3) -0.1447(3) 0.0279(9) Uani 1 d . . H33 H 0.1735(4) 0.1552(3) -0.1646(3) 0.034 Uiso 1 calc R . C34 C 0.2256(4) 0.0062(3) -0.1859(3) 0.0308(10) Uani 1 d . . H34 H 0.1959(4) 0.0084(3) -0.2340(3) 0.037 Uiso 1 calc R . C35 C 0.2824(4) -0.0849(3) -0.1575(3) 0.0299(10) Uani 1 d . . H35 H 0.2913(4) -0.1450(3) -0.1859(3) 0.036 Uiso 1 calc R . C36 C 0.3264(4) -0.0883(3) -0.0876(3) 0.0276(9) Uani 1 d . . H36 H 0.3669(4) -0.1512(3) -0.0693(3) 0.033 Uiso 1 calc R . C37 C 0.1139(4) 0.3680(3) 0.0060(3) 0.0211(8) Uani 1 d . . C38 C 0.0145(3) 0.3410(3) 0.0457(3) 0.0214(8) Uani 1 d . . C39 C -0.0251(3) 0.3148(3) 0.1396(3) 0.0230(9) Uani 1 d . . C40 C -0.1121(4) 0.2676(3) 0.1742(3) 0.0290(10) Uani 1 d . . H40A H -0.1450(4) 0.2678(3) 0.1259(3) 0.035 Uiso 1 calc R . H40B H -0.1832(4) 0.3073(3) 0.2366(3) 0.035 Uiso 1 calc R . C41 C -0.0424(4) 0.1602(3) 0.1876(3) 0.0256(9) Uani 1 d . . C42 C -0.0157(4) 0.1425(4) 0.2684(3) 0.0336(10) Uani 1 d . . H42 H -0.0455(4) 0.1978(4) 0.3165(3) 0.040 Uiso 1 calc R . C43 C 0.0541(5) 0.0449(4) 0.2793(4) 0.0474(14) Uani 1 d . . H43 H 0.0726(5) 0.0339(4) 0.3343(4) 0.057 Uiso 1 calc R . C44 C 0.0968(4) -0.0364(4) 0.2103(4) 0.0489(14) Uani 1 d . . H44 H 0.1441(4) -0.1032(4) 0.2180(4) 0.059 Uiso 1 calc R . C45 C 0.0703(5) -0.0197(4) 0.1302(4) 0.0465(13) Uani 1 d . . H45 H 0.0990(5) -0.0752(4) 0.0828(4) 0.056 Uiso 1 calc R . C46 C 0.0015(4) 0.0785(4) 0.1187(3) 0.0357(11) Uani 1 d . . H46 H -0.0153(4) 0.0894(4) 0.0629(3) 0.043 Uiso 1 calc R . C47 C -0.0236(4) 0.3432(3) -0.0317(3) 0.0231(9) Uani 1 d . . C48 C -0.1214(4) 0.3213(3) -0.0380(3) 0.0306(10) Uani 1 d . . H48A H -0.2004(7) 0.3589(17) 0.0191(10) 0.046 Uiso 1 calc R . H48B H -0.0958(13) 0.2488(4) -0.0403(21) 0.046 Uiso 1 calc R . H48C H -0.1320(19) 0.3419(20) -0.0971(11) 0.046 Uiso 1 calc R . C49 C 0.2325(4) 0.3851(3) -0.1630(3) 0.0231(9) Uani 1 d . . C50 C 0.2889(4) 0.4373(3) -0.1438(3) 0.0281(9) Uani 1 d . . H50 H 0.2538(4) 0.4766(3) -0.0818(3) 0.034 Uiso 1 calc R . C51 C 0.3985(4) 0.4306(3) -0.2180(3) 0.0334(10) Uani 1 d . . H51 H 0.4388(4) 0.4650(3) -0.2058(3) 0.040 Uiso 1 calc R . C52 C 0.4494(4) 0.3748(3) -0.3088(3) 0.0352(11) Uani 1 d . . H52 H 0.5245(4) 0.3703(3) -0.3582(3) 0.042 Uiso 1 calc R . C53 C 0.3910(4) 0.3258(3) -0.3273(3) 0.0358(11) Uani 1 d . . H53 H 0.4251(4) 0.2888(3) -0.3902(3) 0.043 Uiso 1 calc R . C54 C 0.2821(4) 0.3299(3) -0.2547(3) 0.0293(10) Uani 1 d . . H54 H 0.2423(4) 0.2954(3) -0.2677(3) 0.035 Uiso 1 calc R . C55 C 0.4475(4) 0.3664(3) 0.0307(3) 0.0318(10) Uani 1 d . . H55A H 0.3779(4) 0.4317(3) 0.0704(3) 0.038 Uiso 1 calc R . H55B H 0.4553(4) 0.3672(3) -0.0368(3) 0.038 Uiso 1 calc R . C56 C 0.5653(5) 0.3555(4) 0.0317(5) 0.057(2) Uani 1 d . . H56A H 0.5748(19) 0.4163(13) 0.0144(27) 0.085 Uiso 1 calc R . H56B H 0.6362(5) 0.2965(17) -0.0155(20) 0.085 Uiso 1 calc R . H56C H 0.5620(15) 0.3466(28) 0.0968(8) 0.085 Uiso 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 Nd 0.02288(13) 0.02256(13) 0.02033(12) 0.00267(9) -0.01034(9) -0.00892(10) O1 0.0235(14) 0.0233(15) 0.0220(14) 0.0027(12) -0.0137(12) -0.0103(12) O2 0.0244(14) 0.025(2) 0.0223(14) 0.0048(12) -0.0120(12) -0.0108(13) O3 0.0276(15) 0.0193(15) 0.0272(15) 0.0044(12) -0.0155(13) -0.0083(13) O4 0.029(2) 0.021(2) 0.0264(15) 0.0032(12) -0.0149(13) -0.0089(13) O5 0.0196(14) 0.0226(15) 0.0224(14) 0.0020(12) -0.0094(12) -0.0072(12) O6 0.0215(14) 0.031(2) 0.0205(14) 0.0037(12) -0.0088(12) -0.0107(13) O7 0.0200(15) 0.020(2) 0.030(2) 0.0003(13) -0.0086(13) -0.0072(12) O8 0.028(2) 0.022(2) 0.0174(14) -0.0012(12) -0.0104(13) -0.0052(13) N1 0.021(2) 0.021(2) 0.017(2) 0.0011(14) -0.0075(14) -0.0076(15) N2 0.026(2) 0.024(2) 0.021(2) 0.0028(15) -0.0118(15) -0.011(2) N3 0.021(2) 0.025(2) 0.020(2) 0.0049(14) -0.0103(14) -0.0103(15) N4 0.024(2) 0.026(2) 0.026(2) 0.005(2) -0.014(2) -0.011(2) N5 0.024(2) 0.018(2) 0.024(2) 0.0018(14) -0.0112(15) -0.0071(15) N6 0.022(2) 0.019(2) 0.024(2) 0.0017(15) -0.0082(15) -0.0039(15) C1 0.016(2) 0.018(2) 0.021(2) 0.002(2) -0.007(2) -0.002(2) C2 0.022(2) 0.019(2) 0.023(2) 0.003(2) -0.012(2) -0.008(2) C3 0.021(2) 0.017(2) 0.023(2) 0.003(2) -0.013(2) -0.005(2) C4 0.029(2) 0.022(2) 0.020(2) 0.005(2) -0.010(2) -0.013(2) C5 0.020(2) 0.028(2) 0.018(2) 0.003(2) -0.006(2) -0.012(2) C6 0.030(2) 0.030(2) 0.019(2) 0.004(2) -0.008(2) -0.015(2) C7 0.024(2) 0.038(3) 0.024(2) 0.002(2) -0.011(2) -0.016(2) C8 0.020(2) 0.034(3) 0.025(2) 0.001(2) -0.010(2) -0.005(2) C9 0.029(2) 0.024(2) 0.035(2) -0.001(2) -0.014(2) -0.008(2) C10 0.026(2) 0.031(2) 0.031(2) 0.000(2) -0.015(2) -0.013(2) C11 0.021(2) 0.017(2) 0.024(2) 0.001(2) -0.010(2) -0.005(2) C12 0.022(2) 0.025(2) 0.022(2) 0.003(2) -0.011(2) -0.007(2) C13 0.025(2) 0.021(2) 0.025(2) 0.005(2) -0.013(2) -0.009(2) C14 0.035(2) 0.029(2) 0.022(2) 0.002(2) -0.010(2) -0.014(2) C15 0.029(2) 0.035(3) 0.028(2) 0.007(2) -0.006(2) -0.016(2) C16 0.029(2) 0.027(2) 0.044(3) 0.012(2) -0.018(2) -0.013(2) C17 0.042(3) 0.033(3) 0.033(2) 0.011(2) -0.023(2) -0.023(2) C18 0.034(2) 0.030(2) 0.027(2) 0.009(2) -0.018(2) -0.018(2) C19 0.021(2) 0.025(2) 0.018(2) 0.002(2) -0.004(2) -0.010(2) C20 0.020(2) 0.021(2) 0.022(2) 0.003(2) -0.009(2) -0.006(2) C21 0.020(2) 0.024(2) 0.021(2) 0.006(2) -0.009(2) -0.009(2) C22 0.029(2) 0.022(2) 0.031(2) 0.005(2) -0.020(2) -0.008(2) C23 0.033(2) 0.020(2) 0.034(2) 0.009(2) -0.011(2) -0.013(2) C24 0.078(4) 0.140(6) 0.058(3) 0.078(4) -0.057(3) -0.100(4) C25 0.067(4) 0.072(4) 0.026(3) 0.003(3) -0.020(3) -0.042(3) C26 0.030(2) 0.040(3) 0.033(3) 0.014(2) -0.014(2) -0.012(2) C27 0.028(2) 0.036(3) 0.050(3) 0.014(2) -0.014(2) -0.016(2) C28 0.028(2) 0.033(3) 0.046(3) 0.005(2) -0.017(2) -0.014(2) C29 0.022(2) 0.023(2) 0.028(2) 0.006(2) -0.010(2) -0.011(2) C30 0.039(3) 0.023(2) 0.035(2) 0.009(2) -0.021(2) -0.010(2) C31 0.022(2) 0.024(2) 0.016(2) 0.002(2) -0.006(2) -0.010(2) C32 0.026(2) 0.024(2) 0.029(2) 0.003(2) -0.013(2) -0.008(2) C33 0.028(2) 0.027(2) 0.024(2) 0.006(2) -0.012(2) -0.007(2) C34 0.028(2) 0.037(3) 0.027(2) 0.005(2) -0.014(2) -0.012(2) C35 0.034(2) 0.027(2) 0.027(2) -0.001(2) -0.013(2) -0.012(2) C36 0.028(2) 0.023(2) 0.031(2) 0.005(2) -0.016(2) -0.008(2) C37 0.023(2) 0.016(2) 0.022(2) 0.002(2) -0.012(2) -0.005(2) C38 0.019(2) 0.020(2) 0.023(2) 0.002(2) -0.010(2) -0.005(2) C39 0.018(2) 0.022(2) 0.025(2) 0.003(2) -0.009(2) -0.006(2) C40 0.024(2) 0.044(3) 0.025(2) 0.007(2) -0.013(2) -0.019(2) C41 0.022(2) 0.033(2) 0.026(2) 0.008(2) -0.009(2) -0.017(2) C42 0.031(2) 0.038(3) 0.035(2) 0.006(2) -0.014(2) -0.018(2) C43 0.038(3) 0.068(4) 0.053(3) 0.037(3) -0.028(3) -0.033(3) C44 0.030(3) 0.031(3) 0.065(4) 0.021(3) -0.007(3) -0.010(2) C45 0.041(3) 0.034(3) 0.051(3) 0.002(2) -0.002(3) -0.021(2) C46 0.040(3) 0.042(3) 0.032(2) 0.009(2) -0.013(2) -0.027(2) C47 0.026(2) 0.019(2) 0.027(2) 0.003(2) -0.015(2) -0.009(2) C48 0.033(2) 0.037(3) 0.031(2) 0.008(2) -0.021(2) -0.017(2) C49 0.022(2) 0.025(2) 0.019(2) 0.007(2) -0.010(2) -0.007(2) C50 0.030(2) 0.023(2) 0.027(2) 0.007(2) -0.011(2) -0.010(2) C51 0.031(2) 0.034(3) 0.036(3) 0.015(2) -0.013(2) -0.016(2) C52 0.023(2) 0.038(3) 0.032(2) 0.016(2) -0.007(2) -0.009(2) C53 0.030(2) 0.038(3) 0.021(2) 0.009(2) -0.009(2) -0.002(2) C54 0.030(2) 0.029(2) 0.027(2) 0.008(2) -0.017(2) -0.008(2) C55 0.031(2) 0.029(2) 0.032(2) 0.005(2) -0.011(2) -0.013(2) C56 0.045(3) 0.042(3) 0.100(5) 0.028(3) -0.036(3) -0.030(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 Nd O1 2.387(3) . ? Nd O3 2.386(3) . ? Nd O6 2.419(3) . ? Nd O5 2.428(2) . ? Nd O2 2.449(3) . ? Nd O4 2.458(2) . ? Nd O8 2.475(3) . ? Nd O7 2.490(3) . ? O1 C1 1.263(4) . ? O2 C3 1.262(4) . ? O3 C19 1.261(5) . ? O4 C21 1.238(5) . ? O5 C37 1.265(4) . ? O6 C39 1.255(4) . ? O7 C55 1.426(5) . ? O7 H1 0.76(3) . ? O8 H2 0.95(4) . ? O8 H3 0.77(3) . ? N1 C1 1.390(5) . ? N1 N2 1.403(4) . ? N1 C13 1.405(5) . ? N2 C11 1.315(5) . ? N3 C37 1.370(5) . ? N3 N4 1.404(4) . ? N3 C49 1.414(5) . ? N4 C47 1.313(5) . ? N5 C19 1.374(5) . ? N5 N6 1.399(4) . ? N5 C31 1.420(5) . ? N6 C29 1.324(5) . ? C1 C2 1.432(5) . ? C2 C3 1.416(5) . ? C2 C11 1.427(5) . ? C3 C4 1.512(5) . ? C4 C5 1.520(5) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.391(6) . ? C5 C10 1.393(6) . ? C6 C7 1.386(5) . ? C6 H6 0.95 . ? C7 C8 1.388(6) . ? C7 H7 0.95 . ? C8 C9 1.383(6) . ? C8 H8 0.95 . ? C9 C10 1.388(5) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? C11 C12 1.486(5) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C18 1.386(6) . ? C13 C14 1.397(6) . ? C14 C15 1.374(6) . ? C14 H14 0.95 . ? C15 C16 1.379(6) . ? C15 H15 0.95 . ? C16 C17 1.379(6) . ? C16 H16 0.95 . ? C17 C18 1.383(6) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C20 1.432(5) . ? C20 C21 1.418(6) . ? C20 C29 1.429(6) . ? C21 C22 1.523(5) . ? C22 C23 1.533(6) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.298(7) . ? C23 C28 1.390(6) . ? C24 C25 1.449(7) . ? C24 H24 0.95 . ? C25 C26 1.365(7) . ? C25 H25 0.95 . ? C26 C27 1.368(7) . ? C26 H26 0.95 . ? C27 C28 1.383(6) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? C29 C30 1.497(5) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C36 1.384(6) . ? C31 C32 1.400(5) . ? C32 C33 1.402(6) . ? C32 H32 0.95 . ? C33 C34 1.369(6) . ? C33 H33 0.95 . ? C34 C35 1.385(6) . ? C34 H34 0.95 . ? C35 C36 1.389(6) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.434(5) . ? C38 C39 1.417(5) . ? C38 C47 1.445(5) . ? C39 C40 1.511(5) . ? C40 C41 1.514(6) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 C46 1.384(6) . ? C41 C42 1.393(6) . ? C42 C43 1.388(7) . ? C42 H42 0.95 . ? C43 C44 1.385(8) . ? C43 H43 0.95 . ? C44 C45 1.380(7) . ? C44 H44 0.95 . ? C45 C46 1.396(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C48 1.500(5) . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 C50 1.392(6) . ? C49 C54 1.394(6) . ? C50 C51 1.398(6) . ? C50 H50 0.95 . ? C51 C52 1.382(6) . ? C51 H51 0.95 . ? C52 C53 1.372(7) . ? C52 H52 0.95 . ? C53 C54 1.398(6) . ? C53 H53 0.95 . ? C54 H54 0.95 . ? C55 C56 1.496(6) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd O3 116.85(9) . . ? O1 Nd O6 78.74(8) . . ? O3 Nd O6 75.25(9) . . ? O1 Nd O5 143.40(8) . . ? O3 Nd O5 76.94(9) . . ? O6 Nd O5 72.29(9) . . ? O1 Nd O2 73.11(9) . . ? O3 Nd O2 140.71(9) . . ? O6 Nd O2 142.03(9) . . ? O5 Nd O2 119.05(9) . . ? O1 Nd O4 72.48(9) . . ? O3 Nd O4 70.72(9) . . ? O6 Nd O4 117.40(9) . . ? O5 Nd O4 141.39(9) . . ? O2 Nd O4 77.68(9) . . ? O1 Nd O8 82.39(9) . . ? O3 Nd O8 143.56(9) . . ? O6 Nd O8 79.18(9) . . ? O5 Nd O8 70.75(9) . . ? O2 Nd O8 72.36(9) . . ? O4 Nd O8 145.36(9) . . ? O1 Nd O7 138.58(9) . . ? O3 Nd O7 80.03(9) . . ? O6 Nd O7 142.25(9) . . ? O5 Nd O7 74.65(9) . . ? O2 Nd O7 71.59(9) . . ? O4 Nd O7 79.41(9) . . ? O8 Nd O7 106.49(9) . . ? C1 O1 Nd 131.6(2) . . ? C3 O2 Nd 137.9(2) . . ? C19 O3 Nd 134.6(2) . . ? C21 O4 Nd 140.0(2) . . ? C37 O5 Nd 129.6(2) . . ? C39 O6 Nd 136.5(2) . . ? C55 O7 Nd 122.6(2) . . ? C55 O7 H1 111.4(36) . . ? Nd O7 H1 125.1(36) . . ? Nd O8 H2 127.3(26) . . ? Nd O8 H3 122.3(33) . . ? H2 O8 H3 103.8(41) . . ? C1 N1 N2 110.8(3) . . ? C1 N1 C13 128.8(3) . . ? N2 N1 C13 120.4(3) . . ? C11 N2 N1 106.8(3) . . ? C37 N3 N4 111.4(3) . . ? C37 N3 C49 127.1(3) . . ? N4 N3 C49 119.1(3) . . ? C47 N4 N3 106.5(3) . . ? C19 N5 N6 111.5(3) . . ? C19 N5 C31 129.6(3) . . ? N6 N5 C31 118.8(3) . . ? C29 N6 N5 105.7(3) . . ? O1 C1 N1 123.5(3) . . ? O1 C1 C2 131.1(3) . . ? N1 C1 C2 105.3(3) . . ? C3 C2 C11 131.0(4) . . ? C3 C2 C1 123.5(3) . . ? C11 C2 C1 105.5(3) . . ? O2 C3 C2 122.1(3) . . ? O2 C3 C4 116.4(3) . . ? C2 C3 C4 121.4(3) . . ? C3 C4 C5 113.7(3) . . ? C3 C4 H4A 108.8(2) . . ? C5 C4 H4A 108.8(2) . . ? C3 C4 H4B 108.8(2) . . ? C5 C4 H4B 108.8(2) . . ? H4A C4 H4B 107.7 . . ? C6 C5 C10 118.1(4) . . ? C6 C5 C4 119.9(4) . . ? C10 C5 C4 122.0(3) . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6 119.3(3) . . ? C5 C6 H6 119.3(2) . . ? C6 C7 C8 120.0(4) . . ? C6 C7 H7 120.0(3) . . ? C8 C7 H7 120.0(2) . . ? C9 C8 C7 119.3(4) . . ? C9 C8 H8 120.4(2) . . ? C7 C8 H8 120.4(2) . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9 119.7(2) . . ? C10 C9 H9 119.7(3) . . ? C9 C10 C5 120.8(4) . . ? C9 C10 H10 119.6(3) . . ? C5 C10 H10 119.6(2) . . ? N2 C11 C2 111.6(3) . . ? N2 C11 C12 118.3(3) . . ? C2 C11 C12 129.9(4) . . ? C11 C12 H12A 109.5(2) . . ? C11 C12 H12B 109.5(2) . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5(2) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.4(4) . . ? C18 C13 N1 121.5(4) . . ? C14 C13 N1 120.1(4) . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9(3) . . ? C13 C14 H14 119.9(3) . . ? C14 C15 C16 121.2(4) . . ? C14 C15 H15 119.4(3) . . ? C16 C15 H15 119.4(3) . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16 120.5(3) . . ? C15 C16 H16 120.5(3) . . ? C16 C17 C18 120.3(4) . . ? C16 C17 H17 119.9(3) . . ? C18 C17 H17 119.9(3) . . ? C17 C18 C13 120.9(4) . . ? C17 C18 H18 119.5(3) . . ? C13 C18 H18 119.5(2) . . ? O3 C19 N5 124.1(3) . . ? O3 C19 C20 129.7(4) . . ? N5 C19 C20 106.2(3) . . ? C21 C20 C29 133.2(3) . . ? C21 C20 C19 122.2(4) . . ? C29 C20 C19 104.4(3) . . ? O4 C21 C20 122.0(3) . . ? O4 C21 C22 116.4(4) . . ? C20 C21 C22 121.5(4) . . ? C21 C22 C23 110.5(3) . . ? C21 C22 H22A 109.5(2) . . ? C23 C22 H22A 109.5(2) . . ? C21 C22 H22B 109.5(2) . . ? C23 C22 H22B 109.5(2) . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 118.6(4) . . ? C24 C23 C22 121.0(4) . . ? C28 C23 C22 120.4(4) . . ? C23 C24 C25 122.6(4) . . ? C23 C24 H24 118.7(3) . . ? C25 C24 H24 118.7(3) . . ? C26 C25 C24 117.7(5) . . ? C26 C25 H25 121.2(3) . . ? C24 C25 H25 121.2(3) . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26 120.1(3) . . ? C27 C26 H26 120.1(3) . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27 119.8(3) . . ? C28 C27 H27 119.8(3) . . ? C27 C28 C23 120.8(5) . . ? C27 C28 H28 119.6(3) . . ? C23 C28 H28 119.6(3) . . ? N6 C29 C20 112.2(3) . . ? N6 C29 C30 117.1(4) . . ? C20 C29 C30 130.7(4) . . ? C29 C30 H30A 109.5(2) . . ? C29 C30 H30B 109.5(2) . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5(2) . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.4(3) . . ? C36 C31 N5 119.5(3) . . ? C32 C31 N5 121.0(4) . . ? C31 C32 C33 119.2(4) . . ? C31 C32 H32 120.4(2) . . ? C33 C32 H32 120.4(3) . . ? C34 C33 C32 120.8(4) . . ? C34 C33 H33 119.6(2) . . ? C32 C33 H33 119.6(3) . . ? C33 C34 C35 119.9(4) . . ? C33 C34 H34 120.0(2) . . ? C35 C34 H34 120.0(3) . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 119.9(3) . . ? C36 C35 H35 119.9(3) . . ? C31 C36 C35 120.5(4) . . ? C31 C36 H36 119.7(2) . . ? C35 C36 H36 119.7(3) . . ? O5 C37 N3 122.7(3) . . ? O5 C37 C38 131.0(3) . . ? N3 C37 C38 106.1(3) . . ? C39 C38 C37 123.3(3) . . ? C39 C38 C47 132.1(4) . . ? C37 C38 C47 104.5(3) . . ? O6 C39 C38 121.1(4) . . ? O6 C39 C40 115.7(3) . . ? C38 C39 C40 123.2(3) . . ? C39 C40 C41 109.4(3) . . ? C39 C40 H40A 109.8(2) . . ? C41 C40 H40A 109.8(2) . . ? C39 C40 H40B 109.8(2) . . ? C41 C40 H40B 109.8(2) . . ? H40A C40 H40B 108.2 . . ? C46 C41 C42 118.6(4) . . ? C46 C41 C40 121.5(4) . . ? C42 C41 C40 119.8(4) . . ? C43 C42 C41 120.7(5) . . ? C43 C42 H42 119.7(3) . . ? C41 C42 H42 119.7(3) . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H43 119.9(3) . . ? C42 C43 H43 119.9(3) . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44 120.2(3) . . ? C43 C44 H44 120.2(3) . . ? C44 C45 C46 120.1(5) . . ? C44 C45 H45 119.9(3) . . ? C46 C45 H45 119.9(3) . . ? C41 C46 C45 120.8(4) . . ? C41 C46 H46 119.6(2) . . ? C45 C46 H46 119.6(3) . . ? N4 C47 C38 111.5(3) . . ? N4 C47 C48 116.8(3) . . ? C38 C47 C48 131.7(4) . . ? C47 C48 H48A 109.5(2) . . ? C47 C48 H48B 109.5(2) . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5(2) . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C54 120.8(4) . . ? C50 C49 N3 119.2(4) . . ? C54 C49 N3 119.8(4) . . ? C49 C50 C51 118.4(4) . . ? C49 C50 H50 120.8(2) . . ? C51 C50 H50 120.8(3) . . ? C52 C51 C50 121.3(4) . . ? C52 C51 H51 119.4(3) . . ? C50 C51 H51 119.4(3) . . ? C53 C52 C51 119.7(4) . . ? C53 C52 H52 120.2(3) . . ? C51 C52 H52 120.2(3) . . ? C52 C53 C54 120.8(4) . . ? C52 C53 H53 119.6(3) . . ? C54 C53 H53 119.6(3) . . ? C49 C54 C53 119.1(4) . . ? C49 C54 H54 120.5(3) . . ? C53 C54 H54 120.5(3) . . ? O7 C55 C56 112.4(4) . . ? O7 C55 H55A 109.1(2) . . ? C56 C55 H55A 109.1(3) . . ? O7 C55 H55B 109.1(2) . . ? C56 C55 H55B 109.1(3) . . ? H55A C55 H55B 107.8 . . ? C55 C56 H56A 109.5(3) . . ? C55 C56 H56B 109.5(3) . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5(3) . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _refine_diff_density_max 1.049 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.089 data_dyql3 _database_code_CSD 170588 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H59 Dy N6 O9' _chemical_formula_weight 1146.61 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.526(3) _cell_length_b 15.219(3) _cell_length_c 16.225(3) _cell_angle_alpha 63.31(3) _cell_angle_beta 85.20(3) _cell_angle_gamma 63.76(3) _cell_volume 2648.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4075 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method ? _exptl_crystal_F_000 1174 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 IPDS(Stoe) _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22019 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1188 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10572 _reflns_number_observed 4567 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3749 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0515P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6823 _refine_ls_number_parameters 684 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_obs 0.0587 _refine_ls_wR_factor_all 0.2647 _refine_ls_wR_factor_obs 0.1156 _refine_ls_goodness_of_fit_all 0.928 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 2.025 _refine_ls_restrained_S_obs 1.076 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group DY Dy 0.30502(4) 0.67544(3) 0.67378(3) 0.0366(2) Uani 1 d . . O1 O 0.1818(3) 0.8573(2) 0.6145(2) 0.0137(7) Uani 1 d U . O2 O 0.1398(3) 0.6798(3) 0.7339(2) 0.0143(7) Uani 1 d . . O3 O 0.4666(3) 0.5698(3) 0.6309(2) 0.0137(7) Uani 1 d U . O4 O 0.2530(3) 0.5757(3) 0.6248(3) 0.0141(7) Uani 1 d . . O5 O 0.3885(3) 0.5087(3) 0.8016(2) 0.0172(8) Uani 1 d . . O6 O 0.3020(3) 0.7113(3) 0.8045(2) 0.0167(8) Uani 1 d . . O7 O 0.4325(3) 0.7458(3) 0.6662(3) 0.0202(8) Uani 1 d D . H1 H 0.4375(70) 0.7566(66) 0.7065(39) 0.030 Uiso 1 d D . O8 O 0.2900(3) 0.7692(3) 0.5063(2) 0.0131(7) Uani 1 d DU . H2 H 0.2417(33) 0.8099(40) 0.4753(37) 0.020 Uiso 1 d D . H3 H 0.3219(43) 0.7366(43) 0.4833(40) 0.020 Uiso 1 d D . O9 O 0.5231(7) 0.1841(5) 1.2243(4) 0.061(2) Uani 1 d D . H4 H 0.5008(119) 0.2219(59) 1.1687(31) 0.092 Uiso 1 d D . N1 N 0.0268(3) 1.0201(3) 0.5920(3) 0.0241(9) Uani 1 d . . N2 N -0.0803(4) 1.0533(3) 0.6153(3) 0.0317(10) Uani 1 d . . N3 N 0.5967(4) 0.4074(3) 0.6285(3) 0.0136(9) Uani 1 d . . N4 N 0.5959(4) 0.3219(3) 0.6162(3) 0.0159(9) Uani 1 d . . N5 N 0.4331(4) 0.3721(3) 0.9544(3) 0.0183(9) Uani 1 d . . N6 N 0.4233(4) 0.3608(4) 1.0451(3) 0.0199(10) Uani 1 d D . C1 C 0.0836(4) 0.9073(4) 0.6299(3) 0.0114(10) Uani 1 d . . C2 C 0.0118(4) 0.8661(4) 0.6836(3) 0.0124(10) Uani 1 d . . C3 C 0.0466(4) 0.7495(4) 0.7373(3) 0.0130(10) Uani 1 d . . C4 C -0.0876(4) 0.9613(4) 0.6712(4) 0.0153(11) Uani 1 d . . C5 C -0.1945(5) 0.9703(5) 0.7082(5) 0.038(2) Uani 1 d . . H5A H -0.1799(8) 0.9265(37) 0.7762(6) 0.056 Uiso 1 calc R . H5B H -0.2291(23) 0.9426(42) 0.6813(29) 0.056 Uiso 1 calc R . H5C H -0.2449(18) 1.0478(8) 0.6913(34) 0.056 Uiso 1 calc R . C6 C -0.0289(5) 0.7087(4) 0.8008(4) 0.0231(12) Uani 1 d . . H6A H -0.0439(5) 0.7374(4) 0.8468(4) 0.035 Uiso 1 calc R . H6B H -0.1009(5) 0.7399(4) 0.7629(4) 0.035 Uiso 1 calc R . C7 C 0.0173(5) 0.5845(4) 0.8527(4) 0.0212(13) Uani 1 d . . C8 C 0.1057(5) 0.5216(5) 0.9242(5) 0.0296(14) Uani 1 d . . H8 H 0.1396(5) 0.5562(5) 0.9396(5) 0.044 Uiso 1 calc R . C9 C 0.1451(6) 0.4076(6) 0.9737(6) 0.043(2) Uani 1 d . . H9 H 0.2056(6) 0.3648(6) 1.0229(6) 0.065 Uiso 1 calc R . C10 C 0.0965(7) 0.3566(6) 0.9515(6) 0.044(2) Uani 1 d . . H10 H 0.1236(7) 0.2789(6) 0.9858(6) 0.066 Uiso 1 calc R . C11 C 0.0087(11) 0.4180(7) 0.8798(6) 0.059(3) Uani 1 d . . H11 H -0.0239(11) 0.3827(7) 0.8640(6) 0.089 Uiso 1 calc R . C12 C -0.0317(7) 0.5330(6) 0.8305(5) 0.040(2) Uani 1 d . . H12 H -0.0927(7) 0.5758(6) 0.7817(5) 0.060 Uiso 1 calc R . C13 C 0.0666(4) 1.0983(4) 0.5399(4) 0.0119(10) Uani 1 d . . C14 C 0.1810(5) 1.0668(5) 0.5404(6) 0.037(2) Uani 1 d . . H14 H 0.2336(5) 0.9919(5) 0.5766(6) 0.055 Uiso 1 calc R . C15 C 0.2165(5) 1.1435(5) 0.4890(7) 0.047(2) Uani 1 d . . H15 H 0.2942(5) 1.1210(5) 0.4914(7) 0.071 Uiso 1 calc R . C16 C 0.1439(5) 1.2526(5) 0.4335(5) 0.0329(14) Uani 1 d . . H16 H 0.1708(5) 1.3045(5) 0.3972(5) 0.049 Uiso 1 calc R . C17 C 0.0314(5) 1.2844(4) 0.4322(4) 0.0224(12) Uani 1 d . . H17 H -0.0199(5) 1.3595(4) 0.3945(4) 0.034 Uiso 1 calc R . C18 C -0.0088(4) 1.2092(4) 0.4847(4) 0.0178(11) Uani 1 d . . H18 H -0.0867(4) 1.2327(4) 0.4832(4) 0.027 Uiso 1 calc R . C19 C 0.4897(4) 0.4818(4) 0.6256(3) 0.0098(10) Uani 1 d U . C20 C 0.4191(4) 0.4393(4) 0.6151(3) 0.0109(10) Uani 1 d . . C21 C 0.3025(4) 0.4914(4) 0.6105(3) 0.0120(10) Uani 1 d . . C22 C 0.4930(4) 0.3409(4) 0.6091(4) 0.0177(11) Uani 1 d . . C23 C 0.4677(5) 0.2578(5) 0.6028(6) 0.041(2) Uani 1 d . . H23A H 0.4138(37) 0.2941(11) 0.5471(22) 0.061 Uiso 1 calc R . H23B H 0.4364(45) 0.2249(34) 0.6583(19) 0.061 Uiso 1 calc R . H23C H 0.5364(10) 0.1999(26) 0.5989(42) 0.061 Uiso 1 calc R . C24 C 0.2288(4) 0.4520(4) 0.5866(4) 0.0192(11) Uani 1 d . . H24A H 0.2539(4) 0.4368(4) 0.5333(4) 0.029 Uiso 1 calc R . H24B H 0.1515(4) 0.5122(4) 0.5666(4) 0.029 Uiso 1 calc R . C25 C 0.2288(4) 0.3489(4) 0.6667(4) 0.0193(12) Uani 1 d . . C26 C 0.1988(5) 0.2834(5) 0.6451(6) 0.034(2) Uani 1 d . . H26 H 0.1784(5) 0.3047(5) 0.5819(6) 0.051 Uiso 1 calc R . C27 C 0.1989(5) 0.1880(6) 0.7153(8) 0.048(2) Uani 1 d . . H27 H 0.1790(5) 0.1442(6) 0.6997(8) 0.072 Uiso 1 calc R . C28 C 0.2279(7) 0.1553(5) 0.8089(8) 0.055(3) Uani 1 d . . H28 H 0.2271(7) 0.0904(5) 0.8571(8) 0.066 Uiso 1 calc R . C29 C 0.2580(8) 0.2202(6) 0.8298(6) 0.053(2) Uani 1 d . . H29 H 0.2781(8) 0.1991(6) 0.8930(6) 0.080 Uiso 1 calc R . C30 C 0.2592(6) 0.3166(5) 0.7587(5) 0.0323(15) Uani 1 d . . H30 H 0.2809(6) 0.3595(5) 0.7741(5) 0.048 Uiso 1 calc R . C31 C 0.6980(4) 0.4047(4) 0.6453(4) 0.0145(11) Uani 1 d . . C32 C 0.7044(4) 0.4751(4) 0.6756(4) 0.0204(11) Uani 1 d . . H32 H 0.6381(4) 0.5263(4) 0.6852(4) 0.031 Uiso 1 calc R . C33 C 0.8047(5) 0.4718(5) 0.6917(5) 0.0277(13) Uani 1 d . . H33 H 0.8063(5) 0.5219(5) 0.7107(5) 0.041 Uiso 1 calc R . C34 C 0.9040(5) 0.3957(6) 0.6806(5) 0.0314(15) Uani 1 d . . H34 H 0.9734(5) 0.3929(6) 0.6918(5) 0.047 Uiso 1 calc R . C35 C 0.8978(5) 0.3235(6) 0.6522(5) 0.034(2) Uani 1 d . . H35 H 0.9644(5) 0.2708(6) 0.6445(5) 0.051 Uiso 1 calc R . C36 C 0.7980(5) 0.3270(5) 0.6352(4) 0.0244(12) Uani 1 d . . H36 H 0.7965(5) 0.2767(5) 0.6166(4) 0.037 Uiso 1 calc R . C37 C 0.3909(4) 0.4799(4) 0.8881(4) 0.0146(10) Uani 1 d . . C38 C 0.3557(4) 0.5422(4) 0.9386(4) 0.0142(10) Uani 1 d . . C39 C 0.3162(4) 0.6587(4) 0.8921(4) 0.0157(11) Uani 1 d . . C40 C 0.3766(4) 0.4630(4) 1.0342(4) 0.0176(11) Uani 1 d . . C41 C 0.3553(5) 0.4758(5) 1.1221(4) 0.0300(14) Uani 1 d . . H41A H 0.2818(17) 0.5376(25) 1.1116(11) 0.045 Uiso 1 calc R . H41B H 0.4125(23) 0.4903(39) 1.1388(19) 0.045 Uiso 1 calc R . H41C H 0.3578(39) 0.4078(15) 1.1730(9) 0.045 Uiso 1 calc R . C42 C 0.2961(5) 0.7254(5) 0.9461(4) 0.0226(12) Uani 1 d . . H42A H 0.3200(5) 0.6735(5) 1.0134(4) 0.034 Uiso 1 calc R . H42B H 0.3430(5) 0.7642(5) 0.9261(4) 0.034 Uiso 1 calc R . C43 C 0.1763(5) 0.8091(6) 0.9319(6) 0.037(2) Uani 1 d . . C44 C 0.1175(14) 0.7902(11) 1.0081(15) 0.127(8) Uani 1 d . . H44 H 0.1515(14) 0.7251(11) 1.0656(15) 0.190 Uiso 1 calc R . C45 C 0.0082(22) 0.8686(26) 0.9981(34) 0.215(19) Uani 1 d . . H45 H -0.0335(22) 0.8564(26) 1.0486(34) 0.323 Uiso 1 calc R . C46 C -0.0381(11) 0.9612(30) 0.9170(33) 0.179(16) Uani 1 d . . H46 H -0.1124(11) 1.0139(30) 0.9122(33) 0.268 Uiso 1 calc R . C47 C 0.0209(17) 0.9853(16) 0.8350(19) 0.156(12) Uani 1 d . . H47 H -0.0141(17) 1.0502(16) 0.7775(19) 0.233 Uiso 1 calc R . C48 C 0.1338(10) 0.9051(9) 0.8473(8) 0.080(4) Uani 1 d . . H48 H 0.1786(10) 0.9170(9) 0.7991(8) 0.119 Uiso 1 calc R . C49 C 0.4917(5) 0.2757(4) 0.9419(4) 0.0206(12) Uani 1 d . . C50 C 0.5536(6) 0.2780(5) 0.8686(4) 0.0294(14) Uani 1 d . . H50 H 0.5542(6) 0.3449(5) 0.8242(4) 0.044 Uiso 1 calc R . C51 C 0.6148(8) 0.1809(5) 0.8610(6) 0.048(2) Uani 1 d . . H51 H 0.6557(8) 0.1813(5) 0.8105(6) 0.072 Uiso 1 calc R . C52 C 0.6150(9) 0.0832(6) 0.9287(7) 0.057(2) Uani 1 d . . H52 H 0.6583(9) 0.0167(6) 0.9246(7) 0.086 Uiso 1 calc R . C53 C 0.5551(9) 0.0811(6) 1.0000(6) 0.058(2) Uani 1 d . . H53 H 0.5572(9) 0.0134(6) 1.0456(6) 0.087 Uiso 1 calc R . C54 C 0.4898(7) 0.1786(5) 1.0068(5) 0.038(2) Uani 1 d . . H54 H 0.4449(7) 0.1782(5) 1.0551(5) 0.058 Uiso 1 calc R . C55 C 0.5101(6) 0.7643(7) 0.6049(6) 0.043(2) Uani 1 d . . H55A H 0.5284(6) 0.7180(7) 0.5728(6) 0.065 Uiso 1 calc R . H55B H 0.5796(6) 0.7421(7) 0.6412(6) 0.065 Uiso 1 calc R . C56 C 0.4648(7) 0.8828(6) 0.5339(6) 0.044(2) Uani 1 d . . H56A H 0.5165(26) 0.8916(10) 0.4883(26) 0.066 Uiso 1 calc R . H56B H 0.4560(48) 0.9277(9) 0.5649(8) 0.066 Uiso 1 calc R . H56C H 0.3923(25) 0.9068(15) 0.5020(30) 0.066 Uiso 1 calc R . C57 C 0.5556(9) 0.0757(7) 1.2450(7) 0.063(2) Uani 1 d . . H57A H 0.6112(9) 0.0274(7) 1.3021(7) 0.094 Uiso 1 calc R . H57B H 0.5939(9) 0.0632(7) 1.1937(7) 0.094 Uiso 1 calc R . C58 C 0.4731(31) 0.0414(25) 1.2585(11) 0.178(14) Uani 1 d . . H58A H 0.4762(286) -0.0036(362) 1.3253(29) 0.266 Uiso 1 calc R . H58B H 0.4850(248) -0.0025(357) 1.2259(301) 0.266 Uiso 1 calc R . H58C H 0.3999(39) 0.1061(26) 1.2339(326) 0.266 Uiso 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 DY 0.0343(3) 0.0305(2) 0.0368(3) -0.0156(2) 0.0056(2) -0.0081(2) O1 0.0083(14) 0.0077(13) 0.015(2) -0.0050(11) 0.0037(13) 0.0035(11) O2 0.008(2) 0.0110(15) 0.019(2) -0.0071(14) 0.007(2) -0.0008(14) O3 0.008(2) 0.0080(14) 0.020(2) -0.0087(14) 0.0034(15) 0.0027(13) O4 0.007(2) 0.0081(15) 0.022(2) -0.0093(15) -0.001(2) 0.0032(13) O5 0.022(2) 0.0068(14) 0.008(2) -0.0003(13) -0.004(2) 0.0037(14) O6 0.020(2) 0.014(2) 0.011(2) -0.0079(15) 0.000(2) -0.0006(15) O7 0.017(2) 0.019(2) 0.029(2) -0.013(2) 0.006(2) -0.010(2) O8 0.008(2) 0.009(2) 0.008(2) -0.0034(14) -0.0018(15) 0.0075(13) O9 0.115(5) 0.040(3) 0.029(3) 0.004(2) -0.026(3) -0.050(3) N1 0.017(2) 0.018(2) 0.027(2) -0.013(2) 0.003(2) 0.002(2) N2 0.021(2) 0.029(2) 0.039(3) -0.020(2) 0.012(2) -0.004(2) N3 0.011(2) 0.007(2) 0.021(2) -0.010(2) 0.004(2) 0.000(2) N4 0.012(2) 0.012(2) 0.026(2) -0.013(2) 0.007(2) -0.004(2) N5 0.023(2) 0.010(2) 0.009(2) 0.001(2) -0.008(2) -0.001(2) N6 0.022(2) 0.019(2) 0.009(2) -0.002(2) -0.002(2) -0.007(2) C1 0.010(2) 0.008(2) 0.012(2) -0.007(2) 0.002(2) 0.001(2) C2 0.008(2) 0.010(2) 0.013(2) -0.007(2) 0.000(2) 0.003(2) C3 0.016(3) 0.016(2) 0.008(2) -0.007(2) 0.004(2) -0.007(2) C4 0.005(2) 0.012(2) 0.017(3) -0.004(2) -0.001(2) 0.003(2) C5 0.013(3) 0.028(3) 0.051(4) -0.012(3) 0.015(3) -0.001(2) C6 0.017(3) 0.017(2) 0.028(3) -0.007(2) 0.011(3) -0.006(2) C7 0.021(3) 0.020(2) 0.020(3) -0.008(2) 0.013(3) -0.010(2) C8 0.022(3) 0.031(3) 0.033(4) -0.010(3) 0.011(3) -0.015(3) C9 0.027(3) 0.038(4) 0.041(4) -0.009(3) 0.020(3) -0.007(3) C10 0.061(5) 0.031(3) 0.044(5) -0.025(4) 0.032(5) -0.022(4) C11 0.127(9) 0.047(4) 0.027(4) -0.017(4) 0.017(6) -0.059(6) C12 0.064(5) 0.036(3) 0.025(3) -0.008(3) -0.005(4) -0.032(4) C13 0.008(2) 0.012(2) 0.015(3) -0.012(2) -0.002(2) 0.003(2) C14 0.010(3) 0.015(3) 0.060(5) 0.000(3) -0.011(3) 0.000(2) C15 0.013(3) 0.020(3) 0.074(6) 0.001(3) -0.006(4) -0.002(2) C16 0.025(3) 0.015(3) 0.046(4) -0.004(3) 0.000(3) -0.009(2) C17 0.021(3) 0.011(2) 0.025(3) -0.005(2) 0.001(3) -0.002(2) C18 0.013(3) 0.010(2) 0.019(3) -0.006(2) 0.002(2) 0.004(2) C19 0.004(2) 0.005(2) 0.012(2) -0.003(2) 0.000(2) 0.004(2) C20 0.009(2) 0.006(2) 0.014(2) -0.008(2) 0.001(2) 0.002(2) C21 0.006(2) 0.011(2) 0.014(3) -0.005(2) 0.002(2) -0.002(2) C22 0.011(3) 0.013(2) 0.028(3) -0.013(2) 0.008(2) -0.002(2) C23 0.021(3) 0.029(3) 0.091(6) -0.047(4) 0.023(4) -0.011(3) C24 0.010(2) 0.017(2) 0.025(3) -0.011(2) -0.002(2) 0.001(2) C25 0.003(2) 0.020(2) 0.041(4) -0.021(3) 0.009(2) -0.003(2) C26 0.012(3) 0.023(3) 0.068(5) -0.026(3) -0.005(3) -0.002(2) C27 0.018(3) 0.026(3) 0.098(8) -0.028(4) 0.009(4) -0.009(3) C28 0.042(4) 0.021(3) 0.088(7) -0.020(4) 0.038(5) -0.014(3) C29 0.070(5) 0.034(4) 0.051(5) -0.022(4) 0.039(5) -0.023(4) C30 0.044(4) 0.028(3) 0.029(4) -0.016(3) 0.016(3) -0.019(3) C31 0.007(2) 0.017(2) 0.018(3) -0.010(2) 0.003(2) -0.002(2) C32 0.010(2) 0.024(3) 0.028(3) -0.018(2) 0.000(2) -0.002(2) C33 0.016(3) 0.037(3) 0.039(4) -0.026(3) 0.005(3) -0.011(3) C34 0.012(3) 0.053(4) 0.045(4) -0.036(3) 0.007(3) -0.014(3) C35 0.007(3) 0.048(4) 0.051(4) -0.040(4) 0.004(3) 0.002(3) C36 0.011(3) 0.025(3) 0.038(3) -0.024(3) 0.002(3) 0.001(2) C37 0.012(2) 0.013(2) 0.011(3) -0.001(2) -0.004(2) -0.004(2) C38 0.010(2) 0.015(2) 0.014(3) -0.008(2) 0.001(2) -0.002(2) C39 0.016(3) 0.019(2) 0.020(3) -0.016(2) 0.006(2) -0.007(2) C40 0.014(3) 0.023(3) 0.011(3) -0.005(2) 0.004(2) -0.007(2) C41 0.032(3) 0.033(3) 0.014(3) -0.011(3) 0.005(3) -0.005(3) C42 0.025(3) 0.027(3) 0.024(3) -0.022(3) 0.004(3) -0.007(2) C43 0.022(3) 0.046(4) 0.071(5) -0.051(4) 0.017(4) -0.015(3) C44 0.123(11) 0.088(8) 0.241(19) -0.131(11) 0.154(14) -0.070(8) C45 0.111(14) 0.181(21) 0.537(57) -0.288(33) 0.218(27) -0.117(17) C46 0.035(6) 0.210(26) 0.411(44) -0.283(33) 0.005(15) -0.004(10) C47 0.093(11) 0.119(12) 0.223(23) -0.147(16) -0.112(16) 0.069(10) C48 0.065(6) 0.057(5) 0.080(7) -0.055(6) -0.041(6) 0.035(5) C49 0.027(3) 0.010(2) 0.017(3) -0.003(2) -0.010(3) -0.003(2) C50 0.035(3) 0.016(3) 0.023(3) -0.009(2) -0.001(3) 0.001(3) C51 0.060(5) 0.018(3) 0.034(4) -0.009(3) -0.010(4) 0.009(3) C52 0.079(6) 0.017(3) 0.053(5) -0.015(3) -0.011(5) -0.001(4) C53 0.098(7) 0.017(3) 0.046(5) -0.007(3) -0.008(5) -0.020(4) C54 0.053(4) 0.018(3) 0.037(4) -0.003(3) -0.009(4) -0.017(3) C55 0.032(4) 0.051(4) 0.043(4) -0.019(4) 0.014(4) -0.020(3) C56 0.044(4) 0.042(4) 0.048(4) -0.025(3) 0.013(4) -0.018(3) C57 0.065(6) 0.043(4) 0.044(5) -0.009(4) -0.011(5) -0.004(4) C58 0.351(37) 0.247(26) 0.069(8) -0.040(12) 0.041(14) -0.278(31) _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 O5 2.268(4) . ? DY O1 2.271(3) . ? DY O3 2.342(3) . ? DY O2 2.349(3) . ? DY O4 2.356(3) . ? DY O7 2.368(4) . ? DY O6 2.410(3) . ? DY O8 2.411(3) . ? O1 C1 1.276(6) . ? O2 C3 1.254(6) . ? O3 C19 1.276(6) . ? O4 C21 1.277(6) . ? O5 C37 1.267(7) . ? O6 C39 1.258(7) . ? O7 C55 1.417(8) . ? O9 C57 1.383(12) . ? N1 C1 1.371(6) . ? N1 N2 1.389(6) . ? N1 C13 1.417(7) . ? N2 C4 1.326(7) . ? N3 C19 1.376(7) . ? N3 C31 1.400(8) . ? N3 N4 1.406(6) . ? N4 C22 1.294(7) . ? N5 C37 1.366(7) . ? N5 N6 1.405(7) . ? N5 C49 1.425(7) . ? N6 C40 1.324(7) . ? C1 C2 1.415(7) . ? C2 C4 1.417(7) . ? C2 C3 1.439(7) . ? C3 C6 1.516(7) . ? C4 C5 1.492(8) . ? C6 C7 1.513(8) . ? C7 C8 1.384(10) . ? C7 C12 1.391(10) . ? C8 C9 1.393(10) . ? C9 C10 1.380(14) . ? C10 C11 1.38(2) . ? C11 C12 1.404(12) . ? C13 C18 1.401(7) . ? C13 C14 1.403(8) . ? C14 C15 1.356(10) . ? C15 C16 1.377(10) . ? C16 C17 1.377(9) . ? C17 C18 1.389(8) . ? C19 C20 1.424(8) . ? C20 C21 1.408(7) . ? C20 C22 1.429(7) . ? C21 C24 1.517(8) . ? C22 C23 1.494(8) . ? C24 C25 1.523(8) . ? C25 C30 1.380(10) . ? C25 C26 1.406(9) . ? C26 C27 1.386(12) . ? C27 C28 1.40(2) . ? C28 C29 1.390(15) . ? C29 C30 1.408(10) . ? C31 C32 1.399(8) . ? C31 C36 1.406(8) . ? C32 C33 1.378(9) . ? C33 C34 1.396(9) . ? C34 C35 1.404(10) . ? C35 C36 1.373(9) . ? C37 C38 1.425(7) . ? C38 C39 1.423(8) . ? C38 C40 1.426(8) . ? C39 C42 1.546(7) . ? C40 C41 1.512(8) . ? C42 C43 1.508(9) . ? C43 C48 1.39(2) . ? C43 C44 1.40(2) . ? C44 C45 1.39(3) . ? C45 C46 1.34(6) . ? C46 C47 1.48(5) . ? C47 C48 1.43(2) . ? C49 C54 1.387(9) . ? C49 C50 1.393(9) . ? C50 C51 1.395(9) . ? C51 C52 1.395(13) . ? C52 C53 1.35(2) . ? C53 C54 1.402(12) . ? C55 C56 1.493(12) . ? C57 C58 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 DY O1 147.67(12) . . ? O5 DY O3 74.04(12) . . ? O1 DY O3 135.78(12) . . ? O5 DY O2 84.35(13) . . ? O1 DY O2 74.61(12) . . ? O3 DY O2 143.71(11) . . ? O5 DY O4 82.07(13) . . ? O1 DY O4 113.94(13) . . ? O3 DY O4 74.94(12) . . ? O2 DY O4 73.45(12) . . ? O5 DY O7 100.72(14) . . ? O1 DY O7 81.55(13) . . ? O3 DY O7 73.54(12) . . ? O2 DY O7 140.29(12) . . ? O4 DY O7 146.15(12) . . ? O5 DY O6 73.33(12) . . ? O1 DY O6 77.38(13) . . ? O3 DY O6 124.51(13) . . ? O2 DY O6 74.00(13) . . ? O4 DY O6 140.67(12) . . ? O7 DY O6 70.06(13) . . ? O5 DY O8 143.72(11) . . ? O1 DY O8 68.58(12) . . ? O3 DY O8 72.41(12) . . ? O2 DY O8 116.00(13) . . ? O4 DY O8 76.29(12) . . ? O7 DY O8 82.70(14) . . ? O6 DY O8 139.01(12) . . ? C1 O1 DY 132.2(3) . . ? C3 O2 DY 138.6(3) . . ? C19 O3 DY 127.7(3) . . ? C21 O4 DY 137.0(3) . . ? C37 O5 DY 132.3(3) . . ? C39 O6 DY 137.6(3) . . ? C55 O7 DY 133.2(4) . . ? C1 N1 N2 110.9(4) . . ? C1 N1 C13 128.2(4) . . ? N2 N1 C13 120.8(4) . . ? C4 N2 N1 106.0(4) . . ? C19 N3 C31 129.7(4) . . ? C19 N3 N4 110.3(4) . . ? C31 N3 N4 120.0(4) . . ? C22 N4 N3 106.8(4) . . ? C37 N5 N6 112.5(4) . . ? C37 N5 C49 128.0(5) . . ? N6 N5 C49 119.3(4) . . ? C40 N6 N5 104.9(4) . . ? O1 C1 N1 122.6(4) . . ? O1 C1 C2 130.9(4) . . ? N1 C1 C2 106.5(4) . . ? C1 C2 C4 104.9(4) . . ? C1 C2 C3 121.7(4) . . ? C4 C2 C3 133.4(4) . . ? O2 C3 C2 121.2(4) . . ? O2 C3 C6 118.7(4) . . ? C2 C3 C6 120.0(4) . . ? N2 C4 C2 111.7(4) . . ? N2 C4 C5 118.6(5) . . ? C2 C4 C5 129.7(5) . . ? C7 C6 C3 114.7(4) . . ? C8 C7 C12 119.5(6) . . ? C8 C7 C6 120.7(5) . . ? C12 C7 C6 119.8(6) . . ? C7 C8 C9 120.2(7) . . ? C10 C9 C8 120.3(8) . . ? C9 C10 C11 120.4(6) . . ? C10 C11 C12 119.4(8) . . ? C7 C12 C11 120.3(8) . . ? C18 C13 C14 118.6(5) . . ? C18 C13 N1 120.1(4) . . ? C14 C13 N1 121.3(4) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 122.5(6) . . ? C15 C16 C17 118.1(5) . . ? C16 C17 C18 121.5(5) . . ? C17 C18 C13 119.4(5) . . ? O3 C19 N3 123.1(4) . . ? O3 C19 C20 130.8(4) . . ? N3 C19 C20 106.1(4) . . ? C21 C20 C19 123.7(4) . . ? C21 C20 C22 131.7(5) . . ? C19 C20 C22 104.6(4) . . ? O4 C21 C20 121.4(4) . . ? O4 C21 C24 116.5(4) . . ? C20 C21 C24 122.1(4) . . ? N4 C22 C20 112.2(5) . . ? N4 C22 C23 118.5(4) . . ? C20 C22 C23 129.1(5) . . ? C21 C24 C25 114.1(5) . . ? C30 C25 C26 119.2(6) . . ? C30 C25 C24 122.6(5) . . ? C26 C25 C24 118.2(6) . . ? C27 C26 C25 120.5(8) . . ? C26 C27 C28 120.7(7) . . ? C29 C28 C27 118.4(6) . . ? C28 C29 C30 121.1(9) . . ? C25 C30 C29 120.0(7) . . ? C32 C31 N3 122.0(4) . . ? C32 C31 C36 117.9(5) . . ? N3 C31 C36 120.1(5) . . ? C33 C32 C31 121.4(5) . . ? C32 C33 C34 120.8(5) . . ? C33 C34 C35 117.7(5) . . ? C36 C35 C34 121.8(5) . . ? C35 C36 C31 120.4(5) . . ? O5 C37 N5 122.8(4) . . ? O5 C37 C38 132.0(4) . . ? N5 C37 C38 105.2(4) . . ? C39 C38 C37 120.9(5) . . ? C39 C38 C40 133.5(5) . . ? C37 C38 C40 105.4(4) . . ? O6 C39 C38 121.3(4) . . ? O6 C39 C42 116.7(4) . . ? C38 C39 C42 121.9(5) . . ? N6 C40 C38 111.9(4) . . ? N6 C40 C41 116.4(5) . . ? C38 C40 C41 131.7(5) . . ? C43 C42 C39 113.7(5) . . ? C48 C43 C44 123.6(10) . . ? C48 C43 C42 118.4(7) . . ? C44 C43 C42 117.7(10) . . ? C45 C44 C43 118.9(24) . . ? C46 C45 C44 119.9(25) . . ? C45 C46 C47 123.2(11) . . ? C48 C47 C46 116.0(22) . . ? C43 C48 C47 118.2(17) . . ? C54 C49 C50 120.8(5) . . ? C54 C49 N5 118.5(6) . . ? C50 C49 N5 120.6(5) . . ? C49 C50 C51 119.3(6) . . ? C52 C51 C50 119.1(7) . . ? C53 C52 C51 121.5(7) . . ? C52 C53 C54 120.1(7) . . ? C49 C54 C53 119.1(7) . . ? O7 C55 C56 111.3(6) . . ? O9 C57 C58 117.6(18) . . ? _refine_diff_density_max 0.510 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.073