# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Jones' _publ_contact_author_email RAJONES@MAIL.UTEXAS.EDU _publ_section_title ; Syntheses, Structures, and Photoluminescence of 1-D Lanthanide Coordination Polymers ; loop_ _publ_author_name 'Richard Jones' 'Joseph H. Rivers' 'Wai-Kwok Wong.' 'Xiaoping Yang.' # Attachment 'Complex-1.CIF' data_Complex-1 _database_code_depnum_ccdc_archive 'CCDC 733181' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H96 Eu2 F3 N12 O16 S, C F3 O3 S' _chemical_formula_sum 'C99 H96 Eu2 F6 N12 O19 S2' _chemical_formula_weight 2239.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5068(19) _cell_length_b 14.029(3) _cell_length_c 17.803(4) _cell_angle_alpha 83.56(3) _cell_angle_beta 89.28(4) _cell_angle_gamma 84.18(3) _cell_volume 2347.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7606 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8002 _exptl_absorpt_correction_T_max 0.8923 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13282 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13282 _reflns_number_gt 9428 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR was applied to all non-hydrogen atoms to allow their Uij components approximate to isotropic behavior (restraints: 843). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+3.6253P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(3) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.496(17) _refine_ls_number_reflns 13282 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 843 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2242 _refine_ls_wR_factor_gt 0.1848 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.53546(4) 0.62073(3) 0.73483(2) 0.02636(17) Uani 1 1 d U . . Eu2 Eu 1.13966(4) 0.46530(3) 0.28040(2) 0.02575(18) Uani 1 1 d U . . S1 S 0.3738(4) 0.4918(2) 0.57963(15) 0.0626(10) Uani 1 1 d DU . . S2 S 0.9290(4) 0.0343(3) -0.02157(19) 0.0438(7) Uani 1 1 d U . . F1 F 0.5059(6) 0.3269(5) 0.6150(5) 0.112(5) Uani 1 1 d DU . . F2 F 0.2941(8) 0.3216(5) 0.5756(4) 0.1125(3) Uani 1 1 d DU . . F3 F 0.3255(9) 0.3594(5) 0.6859(3) 0.101(6) Uani 1 1 d DU . . F4 F 0.7913(10) 0.0886(7) 0.1033(5) 0.071(3) Uani 1 1 d U . . F5 F 0.6628(9) 0.1204(6) -0.0093(5) 0.064(3) Uani 1 1 d U . . F6 F 0.7153(11) -0.0317(8) 0.0505(5) 0.086(3) Uani 1 1 d U . . O1 O 0.5109(8) 0.7814(5) 0.7750(4) 0.024(2) Uani 1 1 d U . . H1A H 0.4751 0.8067 0.7350 0.029 Uiso 1 1 calc R . . O2 O 1.2222(9) 1.0104(6) 0.5963(4) 0.037(2) Uani 1 1 d U . . H2D H 1.1448 0.9996 0.6142 0.045 Uiso 1 1 calc R . . O3 O 0.4423(6) 0.5284(4) 0.6388(3) 0.0503(11) Uani 1 1 d DU . . O4 O 0.4258(8) 0.4946(6) 0.5074(3) 0.087(4) Uani 1 1 d DU . . O5 O 0.2190(5) 0.5356(4) 0.5790(4) 0.0503(11) Uani 1 1 d DU . . O6 O 0.9746(11) 0.1213(7) -0.0446(5) 0.050(2) Uani 1 1 d U . . O7 O 0.8664(12) -0.0121(7) -0.0775(5) 0.056(3) Uani 1 1 d U . . O8 O 1.0059(11) -0.0259(7) 0.0260(5) 0.050(2) Uani 1 1 d U . . O9 O 1.2426(10) 0.5582(6) 0.3795(5) 0.0503(11) Uani 1 1 d U . . H9C H 1.3231 0.5310 0.3832 0.060 Uiso 1 1 calc R . . O1B O 0.4369(7) 0.5109(5) 0.8257(3) 0.0203(16) Uani 1 1 d U . . O2B O 0.7076(8) 0.6832(5) 0.6556(4) 0.026(2) Uani 1 1 d U . . O1C O 0.7075(8) 0.4831(5) 0.7200(4) 0.0237(17) Uani 1 1 d U . . H1CA H 0.7713 0.5142 0.7311 0.028 Uiso 1 1 calc R . . O2C O 0.9726(8) 0.6002(5) 0.2919(4) 0.0212(18) Uani 1 1 d U . . H2CA H 0.9838 0.5877 0.3377 0.025 Uiso 1 1 calc R . . O1D O 0.9496(8) 0.4136(5) 0.3588(4) 0.020(2) Uani 1 1 d U . . O2D O 1.2493(9) 0.5651(6) 0.1884(5) 0.034(2) Uani 1 1 d U . . O1E O 1.0185(8) 0.4748(5) 0.1664(4) 0.029(2) Uani 1 1 d U . . H1EA H 1.0956 0.4788 0.1457 0.035 Uiso 1 1 calc R . . O2E O 1.6649(9) 0.6117(6) -0.1488(4) 0.025(2) Uani 1 1 d U . . H2EA H 1.5995 0.5935 -0.1223 0.037 Uiso 1 1 calc R . . O1F O 0.4602(10) 0.0847(6) 0.4209(5) 0.032(2) Uani 1 1 d U . . H1FA H 0.5277 0.1054 0.3975 0.048 Uiso 1 1 calc R . . O2F O 1.1670(10) 0.3064(6) 0.2388(5) 0.033(2) Uani 1 1 d U . . H2FA H 1.0824 0.3008 0.2449 0.040 Uiso 1 1 calc R . . N1 N 0.6665(11) 0.9212(7) 0.7436(5) 0.035(3) Uani 1 1 d U . . N2 N 1.0386(10) 0.9753(7) 0.7063(5) 0.026(3) Uani 1 1 d U . . N1B N 0.2625(10) 0.6560(6) 0.7361(5) 0.022(2) Uani 1 1 d U . . N2B N 0.4273(9) 0.7507(6) 0.6212(5) 0.020(5) Uani 1 1 d U . . N1C N 0.8535(10) 0.4772(6) 0.6059(5) 0.025(3) Uani 1 1 d U . . N2C N 0.8189(10) 0.6127(6) 0.4148(5) 0.014(2) Uani 1 1 d U . . N1D N 1.2394(11) 0.3449(7) 0.3910(6) 0.029(3) Uani 1 1 d U . . N2D N 1.4096(12) 0.4231(8) 0.2741(6) 0.033(3) Uani 1 1 d U . . N1E N 1.1522(9) 0.5299(7) 0.0367(5) 0.029(2) Uani 1 1 d DU . . N2E N 1.5193(10) 0.5629(7) -0.0280(5) 0.021(2) Uani 1 1 d U . . N1F N 0.6250(12) 0.1133(7) 0.3076(6) 0.030(3) Uani 1 1 d U . . N2F N 0.9924(10) 0.1714(6) 0.2629(5) 0.0165(19) Uani 1 1 d U . . C1 C 0.3519(7) 0.7914(4) 0.8779(4) 0.038(3) Uani 1 1 d GU . . H1B H 0.3175 0.7342 0.8686 0.046 Uiso 1 1 calc R . . C2 C 0.2982(8) 0.8398(5) 0.9377(4) 0.043(3) Uani 1 1 d GU . . H2A H 0.2278 0.8149 0.9684 0.052 Uiso 1 1 calc R . . C3 C 0.3497(10) 0.9254(5) 0.9515(4) 0.040(3) Uani 1 1 d GU . . H3A H 0.3138 0.9578 0.9915 0.047 Uiso 1 1 calc R . . C4 C 0.4550(10) 0.9627(5) 0.9056(5) 0.061(4) Uani 1 1 d GU . . H4A H 0.4895 1.0200 0.9149 0.074 Uiso 1 1 calc R . . C5 C 0.5087(8) 0.9143(5) 0.8459(5) 0.033(3) Uani 1 1 d GU . . C6 C 0.4572(8) 0.8287(5) 0.8320(4) 0.033(3) Uani 1 1 d GU . . C7 C 0.6169(14) 0.9511(9) 0.8088(7) 0.037(3) Uani 1 1 d U . . H7B H 0.6597 0.9993 0.8289 0.044 Uiso 1 1 calc R . . C8 C 0.7888(13) 0.9564(9) 0.7085(7) 0.039(3) Uani 1 1 d DU . . H8B H 0.7752 1.0263 0.7037 0.047 Uiso 1 1 calc R . . H8A H 0.7946 0.9374 0.6577 0.047 Uiso 1 1 calc R . . C9 C 0.9282(11) 0.9249(9) 0.7464(6) 0.029(3) Uani 1 1 d DU . . H9A H 0.9235 0.9393 0.7985 0.034 Uiso 1 1 calc R . . H9B H 0.9501 0.8559 0.7464 0.034 Uiso 1 1 calc R . . C10 C 1.1195(14) 1.0099(8) 0.7453(7) 0.034(3) Uani 1 1 d U . . H10A H 1.1050 1.0034 0.7973 0.040 Uiso 1 1 calc R . . C11 C 1.2446(7) 1.0638(5) 0.7141(4) 0.044(4) Uani 1 1 d GU . . C12 C 1.3238(8) 1.1148(6) 0.7578(4) 0.041(3) Uani 1 1 d GU . . H12A H 1.2953 1.1242 0.8068 0.049 Uiso 1 1 calc R . . C13 C 1.4456(8) 1.1518(6) 0.7282(5) 0.061(4) Uani 1 1 d GU . . H13A H 1.4986 1.1859 0.7574 0.074 Uiso 1 1 calc R . . C14 C 1.4882(8) 1.1377(7) 0.6549(5) 0.042(3) Uani 1 1 d GU . . H14A H 1.5697 1.1624 0.6352 0.050 Uiso 1 1 calc R . . C15 C 1.4090(9) 1.0867(7) 0.6113(4) 0.057(4) Uani 1 1 d GU . . H15A H 1.4375 1.0773 0.5622 0.068 Uiso 1 1 calc R . . C16 C 1.2872(8) 1.0498(5) 0.6408(4) 0.021(3) Uani 1 1 d GU . . C1B C 0.3258(5) 0.3790(4) 0.8684(3) 0.026(3) Uani 1 1 d GU . . H1BA H 0.4105 0.3523 0.8911 0.031 Uiso 1 1 calc R . . C2B C 0.2095(6) 0.3261(4) 0.8720(3) 0.024(2) Uani 1 1 d GU . . H2BA H 0.2164 0.2640 0.8971 0.029 Uiso 1 1 calc R . . C3B C 0.0829(6) 0.3660(5) 0.8381(4) 0.039(3) Uani 1 1 d GU . . H3BA H 0.0051 0.3306 0.8406 0.047 Uiso 1 1 calc R . . C4B C 0.0726(6) 0.4588(5) 0.8006(4) 0.035(3) Uani 1 1 d GU . . H4BA H -0.0121 0.4855 0.7779 0.043 Uiso 1 1 calc R . . C5B C 0.1890(7) 0.5117(4) 0.7969(4) 0.023(3) Uani 1 1 d GDU . . C6B C 0.3156(6) 0.4718(4) 0.8308(3) 0.018(2) Uani 1 1 d GU . . C7B C 0.1744(14) 0.6075(8) 0.7555(6) 0.031(3) Uani 1 1 d DU . . H7BA H 0.0825 0.6331 0.7431 0.037 Uiso 1 1 calc R . . C8B C 0.2112(14) 0.7548(9) 0.6895(7) 0.037(3) Uani 1 1 d U . . H8BA H 0.1090 0.7618 0.6850 0.045 Uiso 1 1 calc R . . H8BB H 0.2391 0.8077 0.7147 0.045 Uiso 1 1 calc R . . C9B C 0.2757(13) 0.7561(9) 0.6150(7) 0.033(3) Uani 1 1 d U . . H9BA H 0.2497 0.7019 0.5907 0.039 Uiso 1 1 calc R . . H9BB H 0.2412 0.8149 0.5840 0.039 Uiso 1 1 calc R . . C10B C 0.4836(12) 0.8035(8) 0.5843(6) 0.022(3) Uani 1 1 d U . . H10B H 0.4239 0.8485 0.5542 0.027 Uiso 1 1 calc R . . C11B C 0.6448(5) 0.8168(4) 0.5730(3) 0.021(3) Uani 1 1 d GU . . C12B C 0.6796(6) 0.8917(4) 0.5205(4) 0.024(3) Uani 1 1 d GU . . H12E H 0.6090 0.9368 0.4988 0.029 Uiso 1 1 calc R . . C13B C 0.8201(7) 0.8995(5) 0.5004(4) 0.043(4) Uani 1 1 d GU . . H13E H 0.8434 0.9496 0.4653 0.052 Uiso 1 1 calc R . . C14B C 0.9258(6) 0.8322(5) 0.5328(4) 0.025(3) Uani 1 1 d GU . . H14E H 1.0198 0.8374 0.5194 0.030 Uiso 1 1 calc R . . C15B C 0.8909(5) 0.7572(5) 0.5853(4) 0.018(3) Uani 1 1 d GU . . H15F H 0.9616 0.7122 0.6070 0.021 Uiso 1 1 calc R . . C16B C 0.7504(6) 0.7495(4) 0.6054(3) 0.017(2) Uani 1 1 d GU . . C1C C 0.7014(5) 0.3414(4) 0.8125(3) 0.0201(17) Uani 1 1 d GU . . H1CB H 0.6431 0.3748 0.8451 0.024 Uiso 1 1 calc R . . C2C C 0.7479(7) 0.2448(4) 0.8325(3) 0.043(3) Uani 1 1 d GU . . H2CB H 0.7207 0.2136 0.8784 0.052 Uiso 1 1 calc R . . C3C C 0.8350(8) 0.1947(4) 0.7837(4) 0.029(3) Uani 1 1 d GU . . H3CA H 0.8661 0.1301 0.7971 0.034 Uiso 1 1 calc R . . C4C C 0.8757(8) 0.2413(5) 0.7150(4) 0.022(3) Uani 1 1 d GU . . H4CA H 0.9340 0.2078 0.6824 0.026 Uiso 1 1 calc R . . C5C C 0.8292(8) 0.3379(5) 0.6951(3) 0.023(3) Uani 1 1 d GU . . C6C C 0.7420(7) 0.3879(4) 0.7438(3) 0.019(2) Uani 1 1 d GU . . C7C C 0.8714(11) 0.3792(7) 0.6239(6) 0.0177(13) Uani 1 1 d U . . H7CA H 0.9116 0.3400 0.5890 0.021 Uiso 1 1 calc R . . C8C C 0.9022(13) 0.5208(8) 0.5291(6) 0.025(3) Uani 1 1 d U . . H8CA H 0.9627 0.5711 0.5351 0.030 Uiso 1 1 calc R . . H8CB H 0.9552 0.4717 0.5029 0.030 Uiso 1 1 calc R . . C9C C 0.7722(13) 0.5622(8) 0.4846(6) 0.018(3) Uani 1 1 d U . . H9CA H 0.7166 0.5110 0.4739 0.022 Uiso 1 1 calc R . . H9CB H 0.7141 0.6064 0.5131 0.022 Uiso 1 1 calc R . . C10C C 0.7854(12) 0.6968(8) 0.3919(6) 0.0177(13) Uani 1 1 d U . . H10F H 0.7187 0.7323 0.4190 0.021 Uiso 1 1 calc R . . C11C C 0.8461(6) 0.7445(4) 0.3233(3) 0.014(3) Uani 1 1 d GU . . C12C C 0.8074(7) 0.8418(4) 0.3013(3) 0.028(3) Uani 1 1 d GU . . H12F H 0.7508 0.8782 0.3327 0.034 Uiso 1 1 calc R . . C13C C 0.8535(9) 0.8845(4) 0.2324(4) 0.023(3) Uani 1 1 d GU . . H13F H 0.8276 0.9496 0.2177 0.028 Uiso 1 1 calc R . . C14C C 0.9382(8) 0.8301(5) 0.1855(3) 0.021(3) Uani 1 1 d GU . . H14F H 0.9690 0.8587 0.1393 0.026 Uiso 1 1 calc R . . C15C C 0.9769(7) 0.7328(5) 0.2075(3) 0.032(2) Uani 1 1 d GU . . H15E H 1.0336 0.6964 0.1761 0.038 Uiso 1 1 calc R . . C16C C 0.9309(7) 0.6900(4) 0.2764(3) 0.015(2) Uani 1 1 d GU . . C1D C 0.7895(7) 0.3261(5) 0.4273(4) 0.036(4) Uani 1 1 d GU . . H1DA H 0.7195 0.3704 0.4041 0.044 Uiso 1 1 calc R . . C2D C 0.7527(7) 0.2498(5) 0.4780(4) 0.031(3) Uani 1 1 d GU . . H2DA H 0.6580 0.2430 0.4887 0.037 Uiso 1 1 calc R . . C3D C 0.8574(9) 0.1837(5) 0.5126(4) 0.026(3) Uani 1 1 d GU . . H3DA H 0.8328 0.1327 0.5465 0.031 Uiso 1 1 calc R . . C4D C 0.9990(8) 0.1939(5) 0.4966(5) 0.039(4) Uani 1 1 d GU . . H4DA H 1.0690 0.1496 0.5198 0.047 Uiso 1 1 calc R . . C5D C 1.0358(6) 0.2702(6) 0.4460(4) 0.024(3) Uani 1 1 d GU . . C6D C 0.9311(7) 0.3363(5) 0.4113(4) 0.023(3) Uani 1 1 d GU . . C7D C 1.1782(13) 0.2673(8) 0.4411(6) 0.023(3) Uani 1 1 d U . . H7DA H 1.2362 0.2183 0.4683 0.028 Uiso 1 1 calc R . . C8D C 1.3967(15) 0.3276(10) 0.3940(7) 0.041(4) Uani 1 1 d DU . . H8DA H 1.4249 0.2638 0.4194 0.049 Uiso 1 1 calc R . . H8DB H 1.4342 0.3746 0.4223 0.049 Uiso 1 1 calc R . . C9D C 1.4559(13) 0.3361(8) 0.3135(6) 0.026(3) Uani 1 1 d DU . . H9DA H 1.5584 0.3293 0.3154 0.031 Uiso 1 1 calc R . . H9DB H 1.4266 0.2843 0.2874 0.031 Uiso 1 1 calc R . . C10D C 1.5079(14) 0.4899(9) 0.2556(7) 0.033(3) Uani 1 1 d U . . H10C H 1.6015 0.4692 0.2684 0.040 Uiso 1 1 calc R . . C11D C 1.4811(7) 0.5871(4) 0.2190(3) 0.030(3) Uani 1 1 d GU . . C12D C 1.6002(7) 0.6374(5) 0.2130(4) 0.031(3) Uani 1 1 d GU . . H12B H 1.6841 0.6104 0.2364 0.037 Uiso 1 1 calc R . . C13D C 1.5938(9) 0.7281(6) 0.1720(5) 0.042(3) Uani 1 1 d GDU . . H13B H 1.6735 0.7618 0.1680 0.050 Uiso 1 1 calc R . . C14D C 1.4685(11) 0.7685(5) 0.1371(5) 0.053(4) Uani 1 1 d GDU . . H14B H 1.4642 0.8292 0.1097 0.064 Uiso 1 1 calc R . . C15D C 1.3494(9) 0.7183(5) 0.1431(5) 0.040(3) Uani 1 1 d GU . . H15C H 1.2655 0.7453 0.1197 0.048 Uiso 1 1 calc R . . C16D C 1.3557(7) 0.6276(5) 0.1841(4) 0.031(3) Uani 1 1 d GU . . C1E C 0.8255(6) 0.3881(4) 0.1562(3) 0.020(3) Uani 1 1 d GU . . H1EB H 0.8151 0.3856 0.2083 0.024 Uiso 1 1 calc R . . C2E C 0.7370(7) 0.3408(5) 0.1146(3) 0.027(3) Uani 1 1 d GU . . H2EB H 0.6674 0.3068 0.1390 0.032 Uiso 1 1 calc R . . C3E C 0.7525(8) 0.3445(6) 0.0367(3) 0.036(3) Uani 1 1 d GU . . H3EA H 0.6933 0.3129 0.0089 0.043 Uiso 1 1 calc R . . C4E C 0.8565(8) 0.3954(6) 0.0002(3) 0.023(2) Uani 1 1 d GU . . H4EA H 0.8669 0.3978 -0.0520 0.027 Uiso 1 1 calc R . . C5E C 0.9450(8) 0.4426(6) 0.0417(3) 0.027(3) Uani 1 1 d GU . . C6E C 0.9295(7) 0.4390(5) 0.1197(3) 0.020(3) Uani 1 1 d GU . . C7E C 1.0603(12) 0.4908(7) 0.0052(6) 0.018(3) Uani 1 1 d U . . H7EA H 1.0660 0.4928 -0.0471 0.022 Uiso 1 1 calc R . . C8E C 1.2602(11) 0.5746(8) -0.0010(6) 0.024(3) Uani 1 1 d DU . . H8EA H 1.2630 0.6384 0.0147 0.028 Uiso 1 1 calc R . . H8EB H 1.2431 0.5815 -0.0550 0.028 Uiso 1 1 calc R . . C9E C 1.4002(13) 0.5151(10) 0.0167(7) 0.034(3) Uani 1 1 d U . . H9EA H 1.3962 0.4504 0.0030 0.041 Uiso 1 1 calc R . . H9EB H 1.4193 0.5104 0.0705 0.041 Uiso 1 1 calc R . . C10E C 1.6133(13) 0.6111(9) 0.0061(7) 0.029(3) Uani 1 1 d U . . H10D H 1.6037 0.6176 0.0574 0.035 Uiso 1 1 calc R . . C11E C 1.7196(6) 0.6495(5) -0.0330(3) 0.016(3) Uani 1 1 d GU . . C12E C 1.8123(8) 0.6861(6) 0.0136(3) 0.045(4) Uani 1 1 d GU . . H12H H 1.7960 0.6826 0.0654 0.054 Uiso 1 1 calc R . . C13E C 1.9295(8) 0.7279(6) -0.0173(4) 0.032(3) Uani 1 1 d GU . . H13H H 1.9916 0.7524 0.0138 0.038 Uiso 1 1 calc R . . C14E C 1.9540(8) 0.7331(6) -0.0948(4) 0.036(3) Uani 1 1 d GU . . H14H H 2.0324 0.7611 -0.1154 0.043 Uiso 1 1 calc R . . C15E C 1.8613(8) 0.6965(6) -0.1413(3) 0.028(3) Uani 1 1 d GU . . H15H H 1.8776 0.7000 -0.1931 0.033 Uiso 1 1 calc R . . C16E C 1.7441(7) 0.6547(5) -0.1104(3) 0.023(3) Uani 1 1 d GU . . C1F C 0.2631(8) -0.0080(6) 0.3995(4) 0.037(3) Uani 1 1 d GU . . H1FB H 0.2308 -0.0019 0.4484 0.044 Uiso 1 1 calc R . . C2F C 0.1906(9) -0.0588(7) 0.3524(5) 0.060(5) Uani 1 1 d GU . . H2FB H 0.1099 -0.0866 0.3698 0.072 Uiso 1 1 calc R . . C3F C 0.2389(11) -0.0679(7) 0.2792(5) 0.052(4) Uani 1 1 d GU . . H3FA H 0.1904 -0.1019 0.2477 0.062 Uiso 1 1 calc R . . C4F C 0.3595(11) -0.0263(7) 0.2532(4) 0.061(4) Uani 1 1 d GU . . H4FA H 0.3918 -0.0325 0.2043 0.074 Uiso 1 1 calc R . . C5F C 0.4319(9) 0.0244(7) 0.3003(5) 0.027(3) Uani 1 1 d GU . . C6F C 0.3837(8) 0.0336(6) 0.3735(4) 0.044(4) Uani 1 1 d GU . . C7F C 0.5514(14) 0.0614(9) 0.2679(7) 0.028(3) Uani 1 1 d U . . H7FA H 0.5792 0.0499 0.2192 0.033 Uiso 1 1 calc R . . C8F C 0.7423(14) 0.1584(9) 0.2715(7) 0.030(3) Uani 1 1 d U . . H8FA H 0.7269 0.2275 0.2734 0.036 Uiso 1 1 calc R . . H8FB H 0.7468 0.1468 0.2188 0.036 Uiso 1 1 calc R . . C9F C 0.8863(12) 0.1186(8) 0.3108(6) 0.021(3) Uani 1 1 d U . . H9FA H 0.8877 0.1335 0.3627 0.025 Uiso 1 1 calc R . . H9FB H 0.9045 0.0494 0.3100 0.025 Uiso 1 1 calc R . . C10F C 1.0534(14) 0.1393(9) 0.2055(7) 0.028(3) Uani 1 1 d U . . H10E H 1.0281 0.0808 0.1927 0.034 Uiso 1 1 calc R . . C11F C 1.1555(6) 0.1836(4) 0.1590(3) 0.018(2) Uani 1 1 d GU . . C12F C 1.2118(8) 0.1375(5) 0.0985(4) 0.019(2) Uani 1 1 d GU . . H12C H 1.1735 0.0833 0.0853 0.022 Uiso 1 1 calc R . . C13F C 1.3251(9) 0.1725(6) 0.0580(4) 0.043(4) Uani 1 1 d GU . . H13C H 1.3627 0.1417 0.0175 0.052 Uiso 1 1 calc R . . C14F C 1.3823(8) 0.2535(6) 0.0778(5) 0.039(3) Uani 1 1 d GU . . H14C H 1.4581 0.2769 0.0507 0.046 Uiso 1 1 calc R . . C15F C 1.3260(8) 0.2996(5) 0.1382(5) 0.033(3) Uani 1 1 d GU . . H15B H 1.3643 0.3538 0.1515 0.040 Uiso 1 1 calc R . . C16F C 1.2127(8) 0.2646(5) 0.1788(4) 0.028(3) Uani 1 1 d GU . . C17 C 0.3450(9) 0.3724(3) 0.6165(4) 0.0626(10) Uani 1 1 d DU . . C18 C 0.7436(18) 0.0488(11) 0.0376(8) 0.0438(7) Uani 1 1 d U . . C19 C 1.2478(13) 0.6660(8) 0.3773(7) 0.045(3) Uani 1 1 d U . . H19A H 1.2875 0.6801 0.4236 0.067 Uiso 1 1 calc R . . H19B H 1.1538 0.6980 0.3713 0.067 Uiso 1 1 calc R . . H19C H 1.3054 0.6881 0.3356 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0225(3) 0.0332(3) 0.0249(3) -0.0121(2) -0.0009(3) -0.0003(3) Eu2 0.0204(4) 0.0329(4) 0.0264(3) -0.0139(3) 0.0021(3) -0.0032(3) S1 0.098(2) 0.0687(19) 0.0298(15) -0.0049(14) -0.0148(17) -0.0486(18) S2 0.0549(17) 0.0430(14) 0.0332(12) -0.0067(11) -0.0051(12) 0.0000(13) F1 0.120(7) 0.100(7) 0.122(7) -0.028(6) -0.019(6) -0.033(6) F2 0.120(7) 0.100(7) 0.122(7) -0.028(6) -0.019(6) -0.033(6) F3 0.127(10) 0.088(8) 0.113(9) -0.056(7) 0.047(8) -0.049(7) F4 0.084(5) 0.080(5) 0.049(4) -0.009(4) 0.006(4) -0.001(4) F5 0.061(5) 0.066(4) 0.061(4) -0.007(4) 0.006(4) 0.014(4) F6 0.081(5) 0.106(6) 0.066(5) 0.010(4) -0.010(4) -0.001(5) O1 0.025(4) 0.020(3) 0.029(4) -0.011(3) 0.003(3) -0.002(3) O2 0.040(4) 0.036(4) 0.035(4) 0.000(3) 0.018(4) -0.009(3) O3 0.042(2) 0.047(2) 0.063(2) -0.0176(18) -0.0182(19) 0.0035(18) O4 0.103(7) 0.108(7) 0.068(6) -0.042(5) 0.012(6) -0.065(5) O5 0.042(2) 0.047(2) 0.063(2) -0.0176(18) -0.0182(19) 0.0035(18) O6 0.050(4) 0.051(3) 0.041(3) 0.027(3) 0.005(3) 0.002(3) O7 0.072(6) 0.069(5) 0.028(4) -0.025(4) -0.005(4) 0.014(4) O8 0.050(4) 0.051(3) 0.041(3) 0.027(3) 0.005(3) 0.002(3) O9 0.042(2) 0.047(2) 0.063(2) -0.0176(18) -0.0182(19) 0.0035(18) O1B 0.017(3) 0.029(3) 0.015(2) -0.007(2) -0.002(2) -0.001(2) O2B 0.019(4) 0.036(4) 0.025(3) -0.010(3) -0.007(3) 0.000(3) O1C 0.024(3) 0.026(3) 0.020(3) -0.003(2) 0.003(2) 0.004(2) O2C 0.024(3) 0.023(3) 0.015(3) 0.001(2) 0.001(2) 0.001(2) O1D 0.013(4) 0.015(3) 0.027(4) 0.001(3) 0.001(3) 0.011(3) O2D 0.020(4) 0.047(4) 0.038(4) -0.014(3) 0.011(3) -0.013(3) O1E 0.019(4) 0.042(4) 0.032(4) -0.019(3) 0.003(3) -0.019(3) O2E 0.023(4) 0.036(4) 0.015(3) -0.005(3) 0.001(3) -0.005(3) O1F 0.038(5) 0.031(4) 0.030(4) -0.009(3) 0.009(4) -0.010(3) O2F 0.029(4) 0.041(4) 0.033(4) -0.018(4) 0.001(4) -0.008(4) N1 0.033(5) 0.050(5) 0.024(4) -0.008(4) 0.001(4) -0.003(4) N2 0.022(4) 0.025(4) 0.029(4) 0.003(4) 0.011(4) 0.004(4) N1B 0.017(4) 0.027(4) 0.028(4) -0.018(3) 0.000(4) -0.009(3) N2B 0.018(8) 0.014(7) 0.025(7) -0.004(6) -0.005(6) 0.013(6) N1C 0.029(5) 0.023(4) 0.020(4) 0.003(3) 0.004(4) 0.003(4) N2C 0.015(4) 0.018(4) 0.007(4) 0.000(3) -0.003(3) 0.001(3) N1D 0.015(5) 0.029(5) 0.048(5) -0.023(4) -0.003(4) -0.002(4) N2D 0.029(5) 0.040(5) 0.036(5) -0.030(4) 0.002(4) -0.003(4) N1E 0.022(4) 0.039(4) 0.031(4) -0.012(4) 0.007(4) -0.019(4) N2E 0.021(3) 0.025(3) 0.020(3) -0.006(3) 0.000(3) -0.007(3) N1F 0.026(5) 0.030(5) 0.034(5) -0.010(4) 0.000(4) 0.006(4) N2F 0.018(3) 0.019(3) 0.014(3) -0.009(2) -0.004(3) -0.005(2) C1 0.034(5) 0.036(5) 0.050(5) -0.017(4) 0.002(5) -0.023(4) C2 0.041(6) 0.046(6) 0.046(6) -0.014(5) 0.011(5) -0.011(5) C3 0.047(6) 0.042(5) 0.036(5) -0.025(4) 0.006(5) -0.011(5) C4 0.058(7) 0.053(6) 0.079(7) -0.025(5) 0.005(6) -0.013(5) C5 0.035(5) 0.031(5) 0.037(5) -0.018(4) 0.003(4) -0.006(4) C6 0.026(5) 0.041(5) 0.034(5) -0.010(4) -0.003(4) -0.006(4) C7 0.033(6) 0.034(5) 0.048(6) -0.018(4) 0.001(5) -0.011(4) C8 0.046(6) 0.040(6) 0.031(5) -0.003(4) 0.009(5) -0.007(5) C9 0.020(5) 0.036(5) 0.030(5) -0.004(4) 0.010(4) -0.002(4) C10 0.038(6) 0.031(5) 0.030(5) -0.003(4) 0.011(5) 0.005(5) C11 0.040(6) 0.045(6) 0.046(6) -0.005(5) 0.007(5) 0.006(5) C12 0.028(5) 0.057(6) 0.038(5) -0.006(5) -0.011(5) -0.006(5) C13 0.052(7) 0.064(7) 0.070(7) -0.012(5) -0.011(6) -0.007(5) C14 0.027(5) 0.046(6) 0.051(6) -0.003(5) 0.006(5) -0.002(5) C15 0.048(7) 0.060(6) 0.057(6) 0.001(5) 0.001(5) 0.009(5) C16 0.015(5) 0.024(5) 0.026(5) -0.006(4) -0.008(4) -0.002(4) C1B 0.021(5) 0.039(5) 0.019(4) -0.004(4) 0.009(4) -0.010(4) C2B 0.029(3) 0.024(3) 0.022(3) -0.011(3) 0.002(3) -0.007(3) C3B 0.034(5) 0.049(5) 0.045(5) -0.036(4) 0.009(4) -0.021(4) C4B 0.029(5) 0.047(5) 0.035(5) -0.024(4) -0.006(5) -0.007(4) C5B 0.018(5) 0.031(5) 0.023(4) -0.016(4) 0.007(4) -0.008(4) C6B 0.016(3) 0.019(3) 0.020(3) -0.007(3) 0.003(3) -0.011(3) C7B 0.033(6) 0.033(5) 0.027(5) -0.016(4) 0.000(4) 0.009(4) C8B 0.025(5) 0.035(5) 0.052(6) -0.012(5) -0.006(5) 0.005(4) C9B 0.030(5) 0.026(5) 0.042(5) -0.010(4) -0.009(5) 0.000(4) C10B 0.025(5) 0.019(5) 0.020(4) -0.008(4) -0.016(4) 0.017(4) C11B 0.020(5) 0.020(5) 0.026(5) -0.010(4) 0.000(4) -0.006(4) C12B 0.031(5) 0.016(5) 0.023(5) -0.007(4) -0.015(4) 0.008(4) C13B 0.053(6) 0.035(6) 0.041(6) 0.007(5) -0.003(5) -0.012(5) C14B 0.024(5) 0.033(5) 0.018(4) -0.002(4) 0.002(4) -0.006(4) C15B 0.028(5) 0.013(4) 0.012(4) 0.000(3) -0.004(4) -0.004(4) C16B 0.020(3) 0.016(3) 0.015(3) -0.001(3) -0.007(3) 0.001(3) C1C 0.021(3) 0.024(3) 0.017(2) -0.004(2) 0.004(2) -0.011(2) C2C 0.042(4) 0.048(4) 0.041(4) -0.004(3) -0.004(3) -0.009(3) C3C 0.035(5) 0.019(5) 0.029(5) 0.000(4) -0.006(4) 0.009(4) C4C 0.028(5) 0.016(5) 0.020(4) 0.007(4) -0.001(4) -0.005(4) C5C 0.023(5) 0.019(5) 0.025(5) -0.002(4) -0.008(4) 0.006(4) C6C 0.018(3) 0.024(3) 0.016(3) -0.003(3) -0.005(3) -0.003(3) C7C 0.016(2) 0.019(2) 0.020(2) -0.0050(18) 0.0004(19) -0.0034(19) C8C 0.029(5) 0.025(5) 0.020(5) 0.000(4) 0.007(4) 0.001(4) C9C 0.021(5) 0.018(5) 0.015(5) -0.005(4) -0.004(4) 0.001(4) C10C 0.016(2) 0.019(2) 0.020(2) -0.0050(18) 0.0004(19) -0.0034(19) C11C 0.014(5) 0.015(5) 0.010(4) 0.003(4) -0.006(4) 0.001(4) C12C 0.033(6) 0.030(5) 0.025(5) -0.022(4) -0.004(5) 0.001(4) C13C 0.025(5) 0.019(5) 0.025(5) 0.013(4) -0.012(4) -0.015(4) C14C 0.017(4) 0.028(5) 0.017(4) 0.012(4) -0.006(4) -0.008(4) C15C 0.031(4) 0.036(4) 0.031(4) -0.008(3) 0.006(3) -0.013(3) C16C 0.014(3) 0.017(3) 0.013(3) 0.000(3) -0.006(3) -0.003(3) C1D 0.038(6) 0.039(6) 0.033(6) -0.009(5) -0.008(5) 0.000(5) C2D 0.036(6) 0.028(5) 0.031(5) -0.010(4) -0.008(5) 0.000(5) C3D 0.040(6) 0.023(5) 0.017(5) -0.010(4) -0.004(4) -0.007(4) C4D 0.046(6) 0.030(6) 0.041(6) -0.009(5) -0.008(5) 0.001(5) C5D 0.025(5) 0.020(5) 0.026(5) -0.001(4) 0.001(4) 0.003(4) C6D 0.025(5) 0.027(5) 0.019(5) -0.011(4) 0.002(4) -0.004(4) C7D 0.029(5) 0.015(5) 0.024(5) 0.002(4) -0.007(4) -0.005(4) C8D 0.040(6) 0.034(6) 0.050(6) -0.008(5) -0.011(5) 0.000(5) C9D 0.015(5) 0.025(5) 0.040(5) -0.014(4) -0.009(4) 0.009(4) C10D 0.021(5) 0.047(6) 0.038(5) -0.025(5) 0.002(5) -0.009(5) C11D 0.029(6) 0.040(5) 0.026(5) -0.018(4) 0.005(5) -0.015(4) C12D 0.021(5) 0.041(5) 0.034(5) -0.023(4) 0.006(5) -0.003(4) C13D 0.042(4) 0.044(4) 0.042(4) -0.011(3) 0.000(3) -0.011(3) C14D 0.053(6) 0.054(6) 0.057(6) -0.012(5) 0.016(5) -0.019(5) C15D 0.040(6) 0.045(6) 0.044(6) -0.026(5) -0.001(5) -0.020(5) C16D 0.014(5) 0.054(6) 0.031(5) -0.025(4) 0.012(4) -0.011(4) C1E 0.016(5) 0.021(5) 0.023(5) -0.004(4) 0.006(4) -0.006(4) C2E 0.019(5) 0.028(5) 0.033(5) 0.005(4) 0.002(4) -0.010(4) C3E 0.034(6) 0.044(5) 0.034(5) -0.012(4) -0.004(5) -0.011(5) C4E 0.023(3) 0.027(3) 0.020(3) -0.004(3) 0.001(3) -0.011(3) C5E 0.024(5) 0.033(5) 0.029(5) -0.009(4) -0.006(4) -0.017(4) C6E 0.017(5) 0.022(5) 0.022(5) -0.005(4) 0.005(4) -0.004(4) C7E 0.029(5) 0.010(4) 0.017(4) -0.009(3) 0.006(4) 0.000(4) C8E 0.017(5) 0.034(5) 0.021(5) -0.011(4) 0.005(4) -0.002(4) C9E 0.031(6) 0.043(6) 0.034(5) -0.015(5) 0.014(5) -0.019(5) C10E 0.024(5) 0.040(6) 0.021(5) 0.003(4) 0.002(4) -0.006(5) C11E 0.015(5) 0.018(5) 0.013(4) -0.001(4) 0.001(4) 0.000(4) C12E 0.049(6) 0.062(6) 0.028(5) -0.024(5) -0.007(5) -0.003(5) C13E 0.029(5) 0.044(5) 0.028(5) -0.010(4) -0.012(4) -0.024(4) C14E 0.036(4) 0.037(4) 0.036(4) -0.004(3) 0.001(3) -0.007(3) C15E 0.015(5) 0.042(6) 0.025(5) 0.002(4) -0.001(4) -0.005(4) C16E 0.021(5) 0.028(5) 0.018(5) 0.000(4) -0.006(4) 0.003(4) C1F 0.032(6) 0.035(5) 0.044(6) -0.003(5) 0.012(5) -0.004(5) C2F 0.050(7) 0.052(7) 0.078(8) -0.010(6) -0.011(6) -0.012(6) C3F 0.045(6) 0.060(6) 0.055(6) -0.016(5) -0.016(5) -0.018(5) C4F 0.056(7) 0.075(7) 0.051(6) -0.008(5) -0.011(6) 0.005(6) C5F 0.022(5) 0.029(5) 0.029(5) 0.003(4) -0.008(4) 0.001(4) C6F 0.033(6) 0.040(6) 0.056(6) -0.003(5) 0.000(5) 0.004(5) C7F 0.030(6) 0.030(5) 0.020(5) -0.004(4) -0.004(4) 0.007(4) C8F 0.034(6) 0.020(5) 0.034(5) -0.002(4) 0.016(5) 0.007(4) C9F 0.029(5) 0.022(5) 0.016(4) -0.013(4) 0.002(4) -0.010(4) C10F 0.025(5) 0.028(5) 0.034(5) -0.016(4) -0.001(5) -0.003(4) C11F 0.021(3) 0.020(3) 0.017(3) -0.010(3) -0.002(3) -0.006(3) C12F 0.023(3) 0.018(3) 0.018(3) -0.011(3) 0.003(3) -0.008(3) C13F 0.047(6) 0.046(6) 0.040(6) -0.021(5) 0.020(5) -0.001(5) C14F 0.039(6) 0.040(6) 0.041(6) -0.017(5) 0.004(5) -0.009(5) C15F 0.031(4) 0.035(4) 0.036(4) -0.010(3) 0.002(3) -0.007(3) C16F 0.027(6) 0.020(5) 0.039(5) -0.014(4) 0.003(5) -0.001(4) C17 0.098(2) 0.0687(19) 0.0298(15) -0.0049(14) -0.0148(17) -0.0486(18) C18 0.0549(17) 0.0430(14) 0.0332(12) -0.0067(11) -0.0051(12) 0.0000(13) C19 0.040(6) 0.043(5) 0.049(5) -0.019(5) 0.000(5) 0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2B 2.322(8) . ? Eu1 O1B 2.359(7) . ? Eu1 O2E 2.407(8) 1_456 ? Eu1 O1 2.429(7) . ? Eu1 O1C 2.436(7) . ? Eu1 O3 2.480(5) . ? Eu1 N1B 2.593(9) . ? Eu1 N2B 2.705(8) . ? Eu2 O1E 2.330(7) . ? Eu2 O2D 2.338(8) . ? Eu2 O2C 2.370(8) . ? Eu2 O1D 2.391(8) . ? Eu2 O2F 2.415(8) . ? Eu2 O9 2.567(9) . ? Eu2 N1D 2.570(10) . ? Eu2 N2D 2.578(11) . ? S1 O4 1.370(5) . ? S1 O3 1.416(5) . ? S1 O5 1.536(5) . ? S1 C17 1.777(5) . ? S2 O8 1.302(10) . ? S2 O6 1.355(10) . ? S2 O7 1.418(11) . ? S2 C18 2.046(15) . ? F1 C17 1.598(10) . ? F2 C17 1.210(9) . ? F3 C17 1.242(9) . ? F4 C18 1.448(18) . ? F5 C18 1.402(16) . ? F6 C18 1.185(18) . ? O1 C6 1.342(10) . ? O1 H1A 0.8200 . ? O2 C16 1.223(11) . ? O2 H2D 0.8200 . ? O9 C19 1.514(14) . ? O9 H9C 0.8200 . ? O1B C6B 1.325(9) . ? O2B C16B 1.307(9) . ? O1C C6C 1.363(8) . ? O1C H1CA 0.8200 . ? O2C C16C 1.283(9) . ? O2C H2CA 0.8200 . ? O1D C6D 1.374(9) . ? O2D C16D 1.400(11) . ? O1E C6E 1.363(9) . ? O1E H1EA 0.8200 . ? O2E C16E 1.264(10) . ? O2E Eu1 2.407(8) 1_654 ? O2E H2EA 0.8200 . ? O1F C6F 1.419(11) . ? O1F H1FA 0.8200 . ? O2F C16F 1.323(10) . ? O2F H2FA 0.8200 . ? N1 C7 1.343(16) . ? N1 C8 1.419(16) . ? N2 C10 1.214(16) . ? N2 C9 1.459(14) . ? N1B C7B 1.157(15) . ? N1B C8B 1.569(14) . ? N2B C10B 1.109(14) . ? N2B C9B 1.441(15) . ? N1C C7C 1.369(13) . ? N1C C8C 1.522(13) . ? N2C C10C 1.217(13) . ? N2C C9C 1.447(14) . ? N1D C8D 1.491(17) . ? N1D C7D 1.489(15) . ? N2D C9D 1.372(15) . ? N2D C10D 1.401(17) . ? N1E C7E 1.247(14) . ? N1E C8E 1.385(13) . ? N2E C10E 1.361(16) . ? N2E C9E 1.542(15) . ? N1F C7F 1.322(17) . ? N1F C8F 1.446(17) . ? N2F C10F 1.273(15) . ? N2F C9F 1.509(14) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1B 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C7 1.332(15) . ? C5 C6 1.3900 . ? C7 H7B 0.9300 . ? C8 C9 1.499(15) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.538(14) . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B H1BA 0.9300 . ? C2B C3B 1.3900 . ? C2B H2BA 0.9300 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B C7B 1.453(11) . ? C7B H7BA 0.9300 . ? C8B C9B 1.453(17) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C10B C11B 1.570(13) . ? C10B H10B 0.9300 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C12B H12E 0.9300 . ? C13B C14B 1.3900 . ? C13B H13E 0.9300 . ? C14B C15B 1.3900 . ? C14B H14E 0.9300 . ? C15B C16B 1.3900 . ? C15B H15F 0.9300 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C1C H1CB 0.9300 . ? C2C C3C 1.3900 . ? C2C H2CB 0.9300 . ? C3C C4C 1.3900 . ? C3C H3CA 0.9300 . ? C4C C5C 1.3900 . ? C4C H4CA 0.9300 . ? C5C C6C 1.3900 . ? C5C C7C 1.404(11) . ? C7C H7CA 0.9300 . ? C8C C9C 1.507(12) . ? C8C H8CA 0.9700 . ? C8C H8CB 0.9700 . ? C9C H9CA 0.9700 . ? C9C H9CB 0.9700 . ? C10C C11C 1.466(12) . ? C10C H10F 0.9300 . ? C11C C12C 1.3900 . ? C11C C16C 1.3900 . ? C12C C13C 1.3900 . ? C12C H12F 0.9300 . ? C13C C14C 1.3900 . ? C13C H13F 0.9300 . ? C14C C15C 1.3900 . ? C14C H14F 0.9300 . ? C15C C16C 1.3900 . ? C15C H15E 0.9300 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D H1DA 0.9300 . ? C2D C3D 1.3900 . ? C2D H2DA 0.9300 . ? C3D C4D 1.3900 . ? C3D H3DA 0.9300 . ? C4D C5D 1.3900 . ? C4D H4DA 0.9300 . ? C5D C7D 1.353(14) . ? C5D C6D 1.3900 . ? C7D H7DA 0.9300 . ? C8D C9D 1.530(15) . ? C8D H8DA 0.9700 . ? C8D H8DB 0.9700 . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C10D C11D 1.443(14) . ? C10D H10C 0.9300 . ? C11D C12D 1.3900 . ? C11D C16D 1.3900 . ? C12D C13D 1.3900 . ? C12D H12B 0.9300 . ? C13D C14D 1.3900 . ? C13D H13B 0.9300 . ? C14D C15D 1.3900 . ? C14D H14B 0.9300 . ? C15D C16D 1.3900 . ? C15D H15C 0.9300 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C1E H1EB 0.9300 . ? C2E C3E 1.3900 . ? C2E H2EB 0.9300 . ? C3E C4E 1.3900 . ? C3E H3EA 0.9300 . ? C4E C5E 1.3900 . ? C4E H4EA 0.9300 . ? C5E C6E 1.3900 . ? C5E C7E 1.454(12) . ? C7E H7EA 0.9300 . ? C8E C9E 1.515(13) . ? C8E H8EA 0.9700 . ? C8E H8EB 0.9700 . ? C9E H9EA 0.9700 . ? C9E H9EB 0.9700 . ? C10E C11E 1.343(14) . ? C10E H10D 0.9300 . ? C11E C12E 1.3900 . ? C11E C16E 1.3900 . ? C12E C13E 1.3900 . ? C12E H12H 0.9300 . ? C13E C14E 1.3900 . ? C13E H13H 0.9300 . ? C14E C15E 1.3900 . ? C14E H14H 0.9300 . ? C15E C16E 1.3900 . ? C15E H15H 0.9300 . ? C1F C2F 1.3900 . ? C1F C6F 1.3900 . ? C1F H1FB 0.9300 . ? C2F C3F 1.3900 . ? C2F H2FB 0.9300 . ? C3F C4F 1.3900 . ? C3F H3FA 0.9300 . ? C4F C5F 1.3900 . ? C4F H4FA 0.9300 . ? C5F C6F 1.3900 . ? C5F C7F 1.389(15) . ? C7F H7FA 0.9300 . ? C8F C9F 1.567(17) . ? C8F H8FA 0.9700 . ? C8F H8FB 0.9700 . ? C9F H9FA 0.9700 . ? C9F H9FB 0.9700 . ? C10F C11F 1.415(14) . ? C10F H10E 0.9300 . ? C11F C12F 1.3900 . ? C11F C16F 1.3900 . ? C12F C13F 1.3900 . ? C12F H12C 0.9300 . ? C13F C14F 1.3900 . ? C13F H13C 0.9300 . ? C14F C15F 1.3900 . ? C14F H14C 0.9300 . ? C15F C16F 1.3900 . ? C15F H15B 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Eu1 O1B 157.3(2) . . ? O2B Eu1 O2E 97.1(3) . 1_456 ? O1B Eu1 O2E 71.2(3) . 1_456 ? O2B Eu1 O1 83.1(3) . . ? O1B Eu1 O1 110.5(2) . . ? O2E Eu1 O1 73.0(3) 1_456 . ? O2B Eu1 O1C 75.4(3) . . ? O1B Eu1 O1C 83.3(2) . . ? O2E Eu1 O1C 79.7(3) 1_456 . ? O1 Eu1 O1C 142.7(3) . . ? O2B Eu1 O3 94.5(2) . . ? O1B Eu1 O3 86.2(2) . . ? O2E Eu1 O3 145.9(2) 1_456 . ? O1 Eu1 O3 140.5(2) . . ? O1C Eu1 O3 72.3(2) . . ? O2B Eu1 N1B 131.9(3) . . ? O1B Eu1 N1B 70.0(3) . . ? O2E Eu1 N1B 119.5(3) 1_456 . ? O1 Eu1 N1B 79.4(3) . . ? O1C Eu1 N1B 137.1(3) . . ? O3 Eu1 N1B 73.1(2) . . ? O2B Eu1 N2B 66.8(3) . . ? O1B Eu1 N2B 134.2(3) . . ? O2E Eu1 N2B 140.9(3) 1_456 . ? O1 Eu1 N2B 69.9(3) . . ? O1C Eu1 N2B 125.4(2) . . ? O3 Eu1 N2B 72.9(2) . . ? N1B Eu1 N2B 65.1(3) . . ? O1E Eu2 O2D 70.6(3) . . ? O1E Eu2 O2C 79.2(3) . . ? O2D Eu2 O2C 86.4(3) . . ? O1E Eu2 O1D 95.9(3) . . ? O2D Eu2 O1D 156.1(3) . . ? O2C Eu2 O1D 71.5(3) . . ? O1E Eu2 O2F 72.7(3) . . ? O2D Eu2 O2F 106.0(3) . . ? O2C Eu2 O2F 142.9(3) . . ? O1D Eu2 O2F 87.7(3) . . ? O1E Eu2 O9 146.6(3) . . ? O2D Eu2 O9 87.4(3) . . ? O2C Eu2 O9 74.5(3) . . ? O1D Eu2 O9 94.9(3) . . ? O2F Eu2 O9 139.3(3) . . ? O1E Eu2 N1D 142.4(3) . . ? O2D Eu2 N1D 132.0(3) . . ? O2C Eu2 N1D 125.1(3) . . ? O1D Eu2 N1D 70.5(3) . . ? O2F Eu2 N1D 71.8(3) . . ? O9 Eu2 N1D 70.9(3) . . ? O1E Eu2 N2D 116.0(3) . . ? O2D Eu2 N2D 66.9(3) . . ? O2C Eu2 N2D 139.7(3) . . ? O1D Eu2 N2D 136.6(3) . . ? O2F Eu2 N2D 75.8(3) . . ? O9 Eu2 N2D 74.7(3) . . ? N1D Eu2 N2D 66.2(3) . . ? O4 S1 O3 123.1(5) . . ? O4 S1 O5 110.3(4) . . ? O3 S1 O5 107.1(4) . . ? O4 S1 C17 111.1(4) . . ? O3 S1 C17 104.5(4) . . ? O5 S1 C17 97.7(4) . . ? O8 S2 O6 118.8(7) . . ? O8 S2 O7 112.7(7) . . ? O6 S2 O7 116.5(6) . . ? O8 S2 C18 100.6(6) . . ? O6 S2 C18 111.2(6) . . ? O7 S2 C18 92.3(6) . . ? C6 O1 Eu1 140.3(5) . . ? C6 O1 H1A 109.5 . . ? Eu1 O1 H1A 93.8 . . ? C16 O2 H2D 109.5 . . ? S1 O3 Eu1 169.4(4) . . ? C19 O9 Eu2 128.1(7) . . ? C19 O9 H9C 109.5 . . ? Eu2 O9 H9C 100.4 . . ? C6B O1B Eu1 133.9(5) . . ? C16B O2B Eu1 151.7(5) . . ? C6C O1C Eu1 143.6(5) . . ? C6C O1C H1CA 109.5 . . ? Eu1 O1C H1CA 89.9 . . ? C16C O2C Eu2 150.8(6) . . ? C16C O2C H2CA 109.5 . . ? Eu2 O2C H2CA 86.2 . . ? C6D O1D Eu2 135.7(5) . . ? C16D O2D Eu2 138.5(6) . . ? C6E O1E Eu2 151.0(5) . . ? C6E O1E H1EA 109.5 . . ? Eu2 O1E H1EA 86.5 . . ? C16E O2E Eu1 145.0(6) . 1_654 ? C16E O2E H2EA 109.5 . . ? Eu1 O2E H2EA 94.2 1_654 . ? C6F O1F H1FA 109.5 . . ? C16F O2F Eu2 138.8(6) . . ? C16F O2F H2FA 109.5 . . ? Eu2 O2F H2FA 91.5 . . ? C7 N1 C8 121.1(11) . . ? C10 N2 C9 116.1(10) . . ? C7B N1B C8B 115.5(10) . . ? C7B N1B Eu1 131.5(8) . . ? C8B N1B Eu1 112.0(7) . . ? C10B N2B C9B 118.0(10) . . ? C10B N2B Eu1 128.0(8) . . ? C9B N2B Eu1 113.7(6) . . ? C7C N1C C8C 119.4(9) . . ? C10C N2C C9C 126.0(10) . . ? C8D N1D C7D 109.0(9) . . ? C8D N1D Eu2 115.1(7) . . ? C7D N1D Eu2 133.3(8) . . ? C9D N2D C10D 118.3(11) . . ? C9D N2D Eu2 113.7(8) . . ? C10D N2D Eu2 124.9(8) . . ? C7E N1E C8E 124.4(10) . . ? C10E N2E C9E 121.8(10) . . ? C7F N1F C8F 118.6(11) . . ? C10F N2F C9F 123.5(10) . . ? C2 C1 C6 120.0 . . ? C2 C1 H1B 120.0 . . ? C6 C1 H1B 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C7 C5 C6 124.1(8) . . ? C7 C5 C4 115.7(8) . . ? C6 C5 C4 120.0 . . ? O1 C6 C5 119.8(5) . . ? O1 C6 C1 120.2(5) . . ? C5 C6 C1 120.0 . . ? C5 C7 N1 122.4(12) . . ? C5 C7 H7B 118.8 . . ? N1 C7 H7B 118.8 . . ? N1 C8 C9 117.5(10) . . ? N1 C8 H8B 107.9 . . ? C9 C8 H8B 107.9 . . ? N1 C8 H8A 107.9 . . ? C9 C8 H8A 107.9 . . ? H8B C8 H8A 107.2 . . ? N2 C9 C8 109.5(9) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N2 C10 C11 124.2(10) . . ? N2 C10 H10A 117.9 . . ? C11 C10 H10A 117.9 . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 123.4(6) . . ? C16 C11 C10 116.2(6) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? O2 C16 C15 114.4(6) . . ? O2 C16 C11 125.5(6) . . ? C15 C16 C11 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B H1BA 120.0 . . ? C6B C1B H1BA 120.0 . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2BA 120.0 . . ? C3B C2B H2BA 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3BA 120.0 . . ? C4B C3B H3BA 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4BA 120.0 . . ? C3B C4B H4BA 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B C7B 121.9(7) . . ? C4B C5B C7B 118.1(7) . . ? O1B C6B C5B 125.9(4) . . ? O1B C6B C1B 113.9(4) . . ? C5B C6B C1B 120.0 . . ? N1B C7B C5B 128.3(11) . . ? N1B C7B H7BA 115.8 . . ? C5B C7B H7BA 115.8 . . ? C9B C8B N1B 108.0(9) . . ? C9B C8B H8BA 110.1 . . ? N1B C8B H8BA 110.1 . . ? C9B C8B H8BB 110.1 . . ? N1B C8B H8BB 110.1 . . ? H8BA C8B H8BB 108.4 . . ? N2B C9B C8B 110.2(10) . . ? N2B C9B H9BA 109.6 . . ? C8B C9B H9BA 109.6 . . ? N2B C9B H9BB 109.6 . . ? C8B C9B H9BB 109.6 . . ? H9BA C9B H9BB 108.1 . . ? N2B C10B C11B 132.2(10) . . ? N2B C10B H10B 113.9 . . ? C11B C10B H10B 113.9 . . ? C12B C11B C16B 120.0 . . ? C12B C11B C10B 117.2(5) . . ? C16B C11B C10B 122.2(5) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12E 120.0 . . ? C13B C12B H12E 120.0 . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13E 120.0 . . ? C12B C13B H13E 120.0 . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14E 120.0 . . ? C15B C14B H14E 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15F 120.0 . . ? C14B C15B H15F 120.0 . . ? O2B C16B C15B 124.5(5) . . ? O2B C16B C11B 115.4(5) . . ? C15B C16B C11B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C H1CB 120.0 . . ? C6C C1C H1CB 120.0 . . ? C3C C2C C1C 120.0 . . ? C3C C2C H2CB 120.0 . . ? C1C C2C H2CB 120.0 . . ? C2C C3C C4C 120.0 . . ? C2C C3C H3CA 120.0 . . ? C4C C3C H3CA 120.0 . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4CA 120.0 . . ? C3C C4C H4CA 120.0 . . ? C6C C5C C4C 120.0 . . ? C6C C5C C7C 123.2(6) . . ? C4C C5C C7C 116.7(6) . . ? O1C C6C C5C 115.1(4) . . ? O1C C6C C1C 124.8(4) . . ? C5C C6C C1C 120.0 . . ? N1C C7C C5C 120.2(9) . . ? N1C C7C H7CA 119.9 . . ? C5C C7C H7CA 119.9 . . ? C9C C8C N1C 107.5(8) . . ? C9C C8C H8CA 110.2 . . ? N1C C8C H8CA 110.2 . . ? C9C C8C H8CB 110.2 . . ? N1C C8C H8CB 110.2 . . ? H8CA C8C H8CB 108.5 . . ? N2C C9C C8C 107.5(8) . . ? N2C C9C H9CA 110.2 . . ? C8C C9C H9CA 110.2 . . ? N2C C9C H9CB 110.2 . . ? C8C C9C H9CB 110.2 . . ? H9CA C9C H9CB 108.5 . . ? N2C C10C C11C 122.6(10) . . ? N2C C10C H10F 118.7 . . ? C11C C10C H10F 118.7 . . ? C12C C11C C16C 120.0 . . ? C12C C11C C10C 120.0(5) . . ? C16C C11C C10C 119.6(5) . . ? C13C C12C C11C 120.0 . . ? C13C C12C H12F 120.0 . . ? C11C C12C H12F 120.0 . . ? C12C C13C C14C 120.0 . . ? C12C C13C H13F 120.0 . . ? C14C C13C H13F 120.0 . . ? C13C C14C C15C 120.0 . . ? C13C C14C H14F 120.0 . . ? C15C C14C H14F 120.0 . . ? C16C C15C C14C 120.0 . . ? C16C C15C H15E 120.0 . . ? C14C C15C H15E 120.0 . . ? O2C C16C C15C 115.4(5) . . ? O2C C16C C11C 124.6(5) . . ? C15C C16C C11C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D H1DA 120.0 . . ? C6D C1D H1DA 120.0 . . ? C1D C2D C3D 120.0 . . ? C1D C2D H2DA 120.0 . . ? C3D C2D H2DA 120.0 . . ? C2D C3D C4D 120.0 . . ? C2D C3D H3DA 120.0 . . ? C4D C3D H3DA 120.0 . . ? C3D C4D C5D 120.0 . . ? C3D C4D H4DA 120.0 . . ? C5D C4D H4DA 120.0 . . ? C7D C5D C4D 109.6(7) . . ? C7D C5D C6D 130.3(6) . . ? C4D C5D C6D 120.0 . . ? O1D C6D C5D 127.1(5) . . ? O1D C6D C1D 112.9(5) . . ? C5D C6D C1D 120.0 . . ? C5D C7D N1D 118.0(9) . . ? C5D C7D H7DA 121.0 . . ? N1D C7D H7DA 121.0 . . ? N1D C8D C9D 109.3(10) . . ? N1D C8D H8DA 109.8 . . ? C9D C8D H8DA 109.8 . . ? N1D C8D H8DB 109.8 . . ? C9D C8D H8DB 109.8 . . ? H8DA C8D H8DB 108.3 . . ? N2D C9D C8D 111.4(10) . . ? N2D C9D H9DA 109.4 . . ? C8D C9D H9DA 109.4 . . ? N2D C9D H9DB 109.4 . . ? C8D C9D H9DB 109.3 . . ? H9DA C9D H9DB 108.0 . . ? N2D C10D C11D 127.6(11) . . ? N2D C10D H10C 116.2 . . ? C11D C10D H10C 116.2 . . ? C12D C11D C16D 120.0 . . ? C12D C11D C10D 113.7(7) . . ? C16D C11D C10D 126.0(7) . . ? C11D C12D C13D 120.0 . . ? C11D C12D H12B 120.0 . . ? C13D C12D H12B 120.0 . . ? C14D C13D C12D 120.0 . . ? C14D C13D H13B 120.0 . . ? C12D C13D H13B 120.0 . . ? C13D C14D C15D 120.0 . . ? C13D C14D H14B 120.0 . . ? C15D C14D H14B 120.0 . . ? C16D C15D C14D 120.0 . . ? C16D C15D H15C 120.0 . . ? C14D C15D H15C 120.0 . . ? C15D C16D C11D 120.0 . . ? C15D C16D O2D 126.0(6) . . ? C11D C16D O2D 113.7(6) . . ? C2E C1E C6E 120.0 . . ? C2E C1E H1EB 120.0 . . ? C6E C1E H1EB 120.0 . . ? C1E C2E C3E 120.0 . . ? C1E C2E H2EB 120.0 . . ? C3E C2E H2EB 120.0 . . ? C4E C3E C2E 120.0 . . ? C4E C3E H3EA 120.0 . . ? C2E C3E H3EA 120.0 . . ? C5E C4E C3E 120.0 . . ? C5E C4E H4EA 120.0 . . ? C3E C4E H4EA 120.0 . . ? C4E C5E C6E 120.0 . . ? C4E C5E C7E 120.7(6) . . ? C6E C5E C7E 119.2(6) . . ? O1E C6E C5E 124.7(4) . . ? O1E C6E C1E 115.0(4) . . ? C5E C6E C1E 120.0 . . ? N1E C7E C5E 126.8(9) . . ? N1E C7E H7EA 116.6 . . ? C5E C7E H7EA 116.6 . . ? N1E C8E C9E 109.7(8) . . ? N1E C8E H8EA 109.7 . . ? C9E C8E H8EA 109.7 . . ? N1E C8E H8EB 109.7 . . ? C9E C8E H8EB 109.7 . . ? H8EA C8E H8EB 108.2 . . ? C8E C9E N2E 109.5(8) . . ? C8E C9E H9EA 109.8 . . ? N2E C9E H9EA 109.8 . . ? C8E C9E H9EB 109.8 . . ? N2E C9E H9EB 109.8 . . ? H9EA C9E H9EB 108.2 . . ? C11E C10E N2E 121.2(10) . . ? C11E C10E H10D 119.4 . . ? N2E C10E H10D 119.4 . . ? C10E C11E C12E 112.2(7) . . ? C10E C11E C16E 127.8(7) . . ? C12E C11E C16E 120.0 . . ? C13E C12E C11E 120.0 . . ? C13E C12E H12H 120.0 . . ? C11E C12E H12H 120.0 . . ? C12E C13E C14E 120.0 . . ? C12E C13E H13H 120.0 . . ? C14E C13E H13H 120.0 . . ? C15E C14E C13E 120.0 . . ? C15E C14E H14H 120.0 . . ? C13E C14E H14H 120.0 . . ? C16E C15E C14E 120.0 . . ? C16E C15E H15H 120.0 . . ? C14E C15E H15H 120.0 . . ? O2E C16E C15E 122.4(5) . . ? O2E C16E C11E 117.2(5) . . ? C15E C16E C11E 120.0 . . ? C2F C1F C6F 120.0 . . ? C2F C1F H1FB 120.0 . . ? C6F C1F H1FB 120.0 . . ? C1F C2F C3F 120.0 . . ? C1F C2F H2FB 120.0 . . ? C3F C2F H2FB 120.0 . . ? C4F C3F C2F 120.0 . . ? C4F C3F H3FA 120.0 . . ? C2F C3F H3FA 120.0 . . ? C5F C4F C3F 120.0 . . ? C5F C4F H4FA 120.0 . . ? C3F C4F H4FA 120.0 . . ? C4F C5F C6F 120.0 . . ? C4F C5F C7F 114.3(8) . . ? C6F C5F C7F 125.7(8) . . ? C5F C6F C1F 120.0 . . ? C5F C6F O1F 119.1(6) . . ? C1F C6F O1F 120.9(6) . . ? N1F C7F C5F 118.8(11) . . ? N1F C7F H7FA 120.6 . . ? C5F C7F H7FA 120.6 . . ? N1F C8F C9F 111.8(10) . . ? N1F C8F H8FA 109.3 . . ? C9F C8F H8FA 109.3 . . ? N1F C8F H8FB 109.3 . . ? C9F C8F H8FB 109.3 . . ? H8FA C8F H8FB 107.9 . . ? N2F C9F C8F 102.8(9) . . ? N2F C9F H9FA 111.2 . . ? C8F C9F H9FA 111.2 . . ? N2F C9F H9FB 111.2 . . ? C8F C9F H9FB 111.2 . . ? H9FA C9F H9FB 109.1 . . ? N2F C10F C11F 126.6(11) . . ? N2F C10F H10E 116.7 . . ? C11F C10F H10E 116.7 . . ? C12F C11F C16F 120.0 . . ? C12F C11F C10F 118.7(6) . . ? C16F C11F C10F 120.8(6) . . ? C13F C12F C11F 120.0 . . ? C13F C12F H12C 120.0 . . ? C11F C12F H12C 120.0 . . ? C12F C13F C14F 120.0 . . ? C12F C13F H13C 120.0 . . ? C14F C13F H13C 120.0 . . ? C15F C14F C13F 120.0 . . ? C15F C14F H14C 120.0 . . ? C13F C14F H14C 120.0 . . ? C14F C15F C16F 120.0 . . ? C14F C15F H15B 120.0 . . ? C16F C15F H15B 120.0 . . ? O2F C16F C15F 118.6(6) . . ? O2F C16F C11F 121.3(6) . . ? C15F C16F C11F 120.0 . . ? F2 C17 F3 119.8(7) . . ? F2 C17 F1 99.1(6) . . ? F3 C17 F1 98.1(7) . . ? F2 C17 S1 118.8(6) . . ? F3 C17 S1 115.5(6) . . ? F1 C17 S1 97.3(5) . . ? F6 C18 F5 123.9(15) . . ? F6 C18 F4 113.6(12) . . ? F5 C18 F4 110.1(11) . . ? F6 C18 S2 103.0(11) . . ? F5 C18 S2 102.0(9) . . ? F4 C18 S2 100.3(10) . . ? O9 C19 H19A 109.5 . . ? O9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.090 _refine_diff_density_min -2.840 _refine_diff_density_rms 0.225 # Attachment 'Complex-2.CIF' data_Complex-2 _database_code_depnum_ccdc_archive 'CCDC 733182' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H96 F3 N12 Nd2 O16 S, C F3 O3 S' _chemical_formula_sum 'C99 H96 F6 N12 Nd2 O19 S2' _chemical_formula_weight 2224.48 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' S S 0.1246 0.1234 '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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5105(19) _cell_length_b 14.286(3) _cell_length_c 17.870(4) _cell_angle_alpha 82.99(3) _cell_angle_beta 89.68(4) _cell_angle_gamma 83.67(3) _cell_volume 2395.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8928 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8308 _exptl_absorpt_correction_T_max 0.8592 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15839 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15839 _reflns_number_gt 11065 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR was applied to all non-hydrogen atoms to allow their Uij components approximate to isotropic behavior (restraints: 843). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+4.5502P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.505(19) _refine_ls_number_reflns 15839 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 843 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.54193(3) 0.61835(3) 0.73635(2) 0.02825(16) Uani 1 1 d U . . Nd2 Nd 1.13316(3) 0.46747(3) 0.27875(2) 0.02905(17) Uani 1 1 d U . . S1 S 0.3685(3) 0.49404(18) 0.58042(14) 0.0617(8) Uani 1 1 d DU . . S2 S 0.9294(3) 0.0335(2) -0.02137(17) 0.0473(6) Uani 1 1 d U . . F1 F 0.5065(5) 0.3322(5) 0.6102(5) 0.137(4) Uani 1 1 d DU . . F2 F 0.2895(6) 0.3254(4) 0.5790(3) 0.098(3) Uani 1 1 d DU . . F3 F 0.3365(8) 0.3600(5) 0.6879(3) 0.119(3) Uani 1 1 d DU . . F4 F 0.7862(8) 0.0889(5) 0.1000(4) 0.0636(17) Uani 1 1 d U . . F5 F 0.6616(7) 0.1145(6) -0.0117(4) 0.0625(18) Uani 1 1 d U . . F6 F 0.7101(9) -0.0262(7) 0.0550(5) 0.082(3) Uani 1 1 d U . . O1 O 0.5168(7) 0.7799(5) 0.7799(4) 0.038(2) Uani 1 1 d U . . H1A H 0.4826 0.8043 0.7392 0.046 Uiso 1 1 calc R . . O2 O 1.2249(8) 1.0060(5) 0.5962(4) 0.042(2) Uani 1 1 d DU . . H2A H 1.1483 0.9944 0.6141 0.051 Uiso 1 1 calc R . . O3 O 0.4459(5) 0.5297(4) 0.6366(3) 0.0493(10) Uani 1 1 d DU . . O4 O 0.4100(7) 0.5033(5) 0.5058(2) 0.096(3) Uani 1 1 d DU . . O5 O 0.2133(4) 0.5294(4) 0.5884(3) 0.0493(10) Uani 1 1 d DU . . O6 O 0.9717(11) 0.1251(8) -0.0388(6) 0.071(3) Uani 1 1 d U . . O7 O 0.8653(9) -0.0113(7) -0.0779(5) 0.0625(18) Uani 1 1 d U . . O8 O 1.0100(11) -0.0325(7) 0.0237(5) 0.0636(17) Uani 1 1 d U . . O9 O 1.2394(8) 0.5618(6) 0.3793(4) 0.0493(10) Uani 1 1 d U . . H9C H 1.3200 0.5346 0.3832 0.059 Uiso 1 1 calc R . . O1B O 0.4322(6) 0.5138(5) 0.8312(3) 0.0265(18) Uani 1 1 d U . . O2B O 0.7192(7) 0.6772(5) 0.6537(4) 0.033(2) Uani 1 1 d U . . O1C O 0.7123(6) 0.4811(5) 0.7202(3) 0.0236(17) Uani 1 1 d U . . H1CA H 0.7777 0.5108 0.7297 0.028 Uiso 1 1 calc R . . O2C O 0.9565(7) 0.6068(5) 0.2907(4) 0.026(2) Uani 1 1 d U . . H2CA H 0.9580 0.5952 0.3368 0.032 Uiso 1 1 calc R . . O1D O 0.9506(7) 0.4080(5) 0.3642(4) 0.0236(19) Uani 1 1 d U . . O2D O 1.2406(8) 0.5748(5) 0.1862(4) 0.033(2) Uani 1 1 d U . . O1E O 1.0058(6) 0.4774(5) 0.1602(3) 0.0261(18) Uani 1 1 d U . . H1EA H 1.0788 0.4879 0.1376 0.031 Uiso 1 1 calc R . . O2E O 1.6720(8) 0.6059(6) -0.1451(4) 0.034(2) Uani 1 1 d U . . H2EA H 1.6101 0.5834 -0.1189 0.052 Uiso 1 1 calc R . . O1F O 0.4586(8) 0.0869(5) 0.4184(4) 0.038(2) Uani 1 1 d U . . H1FA H 0.5251 0.1068 0.3943 0.056 Uiso 1 1 calc R . . O2F O 1.1663(7) 0.3063(5) 0.2391(4) 0.0242(18) Uani 1 1 d U . . H2FA H 1.0827 0.2990 0.2459 0.029 Uiso 1 1 calc R . . N1 N 0.6768(8) 0.9213(6) 0.7445(4) 0.029(2) Uani 1 1 d U . . N2 N 1.0475(9) 0.9722(7) 0.7097(5) 0.038(3) Uani 1 1 d U . . N1B N 0.2601(7) 0.6523(5) 0.7394(4) 0.029(5) Uani 1 1 d DU . . N2B N 0.4322(7) 0.7456(6) 0.6216(4) 0.025(2) Uani 1 1 d DU . . N1C N 0.8579(8) 0.4757(5) 0.6033(4) 0.0223(9) Uani 1 1 d U . . N2C N 0.8101(9) 0.6151(6) 0.4150(4) 0.0223(9) Uani 1 1 d U . . N1D N 1.2508(10) 0.3386(7) 0.3922(6) 0.037(3) Uani 1 1 d U . . N2D N 1.4099(9) 0.4260(7) 0.2761(5) 0.032(2) Uani 1 1 d U . . N1E N 1.1468(9) 0.5267(6) 0.0384(5) 0.036(2) Uani 1 1 d U . . N2E N 1.5191(8) 0.5590(6) -0.0219(4) 0.022(2) Uani 1 1 d U . . N1F N 0.6255(9) 0.1167(6) 0.3072(5) 0.029(2) Uani 1 1 d U . . N2F N 0.9940(9) 0.1781(7) 0.2609(5) 0.033(2) Uani 1 1 d U . . C1 C 0.3548(6) 0.7914(4) 0.8796(3) 0.040(3) Uani 1 1 d GU . . H1B H 0.3206 0.7357 0.8695 0.048 Uiso 1 1 calc R . . C2 C 0.2999(7) 0.8377(4) 0.9391(3) 0.043(3) Uani 1 1 d GU . . H2B H 0.2289 0.8130 0.9688 0.051 Uiso 1 1 calc R . . C3 C 0.3510(8) 0.9210(5) 0.9542(4) 0.044(3) Uani 1 1 d GU . . H3A H 0.3142 0.9520 0.9941 0.052 Uiso 1 1 calc R . . C4 C 0.4571(8) 0.9579(4) 0.9099(5) 0.054(4) Uani 1 1 d GU . . H4A H 0.4913 1.0136 0.9200 0.065 Uiso 1 1 calc R . . C5 C 0.5121(7) 0.9116(5) 0.8503(4) 0.036(3) Uani 1 1 d GU . . C6 C 0.4609(6) 0.8283(4) 0.8352(3) 0.039(3) Uani 1 1 d GU . . C7 C 0.6115(12) 0.9492(8) 0.8096(6) 0.041(3) Uani 1 1 d U . . H7B H 0.6430 1.0023 0.8266 0.049 Uiso 1 1 calc R . . C8 C 0.7974(10) 0.9547(8) 0.7062(6) 0.038(3) Uani 1 1 d DU . . H8B H 0.7827 1.0235 0.6973 0.046 Uiso 1 1 calc R . . H8A H 0.8041 0.9313 0.6574 0.046 Uiso 1 1 calc R . . C9 C 0.9348(10) 0.9259(8) 0.7473(6) 0.040(3) Uani 1 1 d DU . . H9A H 0.9259 0.9424 0.7983 0.048 Uiso 1 1 calc R . . H9B H 0.9574 0.8577 0.7502 0.048 Uiso 1 1 calc R . . C10 C 1.1225(10) 1.0105(7) 0.7475(6) 0.029(3) Uani 1 1 d U . . H10A H 1.1027 1.0127 0.7983 0.035 Uiso 1 1 calc R . . C11 C 1.2465(6) 1.0544(4) 0.7139(3) 0.044(3) Uani 1 1 d GU . . C12 C 1.3249(7) 1.1020(6) 0.7594(4) 0.056(3) Uani 1 1 d GDU . . H12A H 1.2967 1.1082 0.8086 0.068 Uiso 1 1 calc R . . C13 C 1.4456(8) 1.1401(6) 0.7313(5) 0.057(4) Uani 1 1 d GDU . . H13A H 1.4981 1.1720 0.7617 0.069 Uiso 1 1 calc R . . C14 C 1.4879(7) 1.1308(6) 0.6578(5) 0.054(4) Uani 1 1 d GU . . H14A H 1.5687 1.1563 0.6390 0.065 Uiso 1 1 calc R . . C15 C 1.4094(8) 1.0832(6) 0.6123(4) 0.047(7) Uani 1 1 d GU . . H15A H 1.4377 1.0769 0.5631 0.057 Uiso 1 1 calc R . . C16 C 1.2887(7) 1.0450(5) 0.6404(3) 0.031(3) Uani 1 1 d GDU . . C1B C 0.3304(5) 0.3744(4) 0.8696(3) 0.033(3) Uani 1 1 d GU . . H1BA H 0.4157 0.3484 0.8927 0.039 Uiso 1 1 calc R . . C2B C 0.2162(5) 0.3212(4) 0.8722(3) 0.036(3) Uani 1 1 d GU . . H2BA H 0.2250 0.2597 0.8970 0.043 Uiso 1 1 calc R . . C3B C 0.0888(5) 0.3600(5) 0.8376(4) 0.036(3) Uani 1 1 d GU . . H3BA H 0.0124 0.3244 0.8394 0.043 Uiso 1 1 calc R . . C4B C 0.0757(5) 0.4520(5) 0.8006(4) 0.024(2) Uani 1 1 d GU . . H4BA H -0.0096 0.4779 0.7775 0.029 Uiso 1 1 calc R . . C5B C 0.1899(6) 0.5051(4) 0.7980(3) 0.023(2) Uani 1 1 d GU . . C6B C 0.3173(5) 0.4663(4) 0.8325(3) 0.029(2) Uani 1 1 d GU . . C7B C 0.1669(9) 0.6039(7) 0.7536(5) 0.025(2) Uani 1 1 d DU . . H7BA H 0.0759 0.6274 0.7369 0.030 Uiso 1 1 calc R . . C8B C 0.2088(9) 0.7458(7) 0.6938(6) 0.029(3) Uani 1 1 d U . . H8BA H 0.1068 0.7500 0.6880 0.034 Uiso 1 1 calc R . . H8BB H 0.2296 0.7971 0.7215 0.034 Uiso 1 1 calc R . . C9B C 0.2744(10) 0.7591(8) 0.6171(6) 0.036(3) Uani 1 1 d U . . H9BA H 0.2422 0.7139 0.5865 0.044 Uiso 1 1 calc R . . H9BB H 0.2435 0.8224 0.5927 0.044 Uiso 1 1 calc R . . C10B C 0.4903(9) 0.8059(6) 0.5837(5) 0.0179(19) Uani 1 1 d DU . . H10B H 0.4288 0.8530 0.5566 0.021 Uiso 1 1 calc R . . C11B C 0.6447(4) 0.8181(4) 0.5728(3) 0.039(3) Uani 1 1 d GU . . C12B C 0.6756(5) 0.8941(4) 0.5214(3) 0.030(3) Uani 1 1 d GU . . H12B H 0.6033 0.9393 0.5016 0.036 Uiso 1 1 calc R . . C13B C 0.8146(6) 0.9024(5) 0.4995(4) 0.034(3) Uani 1 1 d GU . . H13B H 0.8353 0.9532 0.4651 0.041 Uiso 1 1 calc R . . C14B C 0.9227(5) 0.8347(5) 0.5291(4) 0.032(3) Uani 1 1 d GU . . H14B H 1.0157 0.8403 0.5145 0.038 Uiso 1 1 calc R . . C15B C 0.8918(5) 0.7588(5) 0.5806(4) 0.028(3) Uani 1 1 d GU . . H15D H 0.9641 0.7135 0.6003 0.033 Uiso 1 1 calc R . . C16B C 0.7528(5) 0.7505(4) 0.6024(3) 0.022(2) Uani 1 1 d GU . . C1C C 0.7083(5) 0.3450(4) 0.8057(2) 0.039(2) Uani 1 1 d GDU . . H1CB H 0.6501 0.3798 0.8368 0.047 Uiso 1 1 calc R . . C2C C 0.7521(6) 0.2497(4) 0.8281(3) 0.038(3) Uani 1 1 d GDU . . H2CB H 0.7232 0.2206 0.8742 0.045 Uiso 1 1 calc R . . C3C C 0.8390(7) 0.1977(4) 0.7816(3) 0.049(3) Uani 1 1 d GU . . H3CA H 0.8683 0.1339 0.7966 0.059 Uiso 1 1 calc R . . C4C C 0.8822(6) 0.2410(4) 0.7127(3) 0.0200(19) Uani 1 1 d GU . . H4CA H 0.9404 0.2063 0.6816 0.024 Uiso 1 1 calc R . . C5C C 0.8384(6) 0.3364(4) 0.6903(3) 0.014(2) Uani 1 1 d GU . . C6C C 0.7515(5) 0.3884(4) 0.7368(3) 0.025(2) Uani 1 1 d GDU . . C7C C 0.8756(10) 0.3840(8) 0.6217(6) 0.036(3) Uani 1 1 d U . . H7CA H 0.9164 0.3474 0.5860 0.043 Uiso 1 1 calc R . . C8C C 0.9072(9) 0.5182(7) 0.5291(5) 0.0224(11) Uani 1 1 d U . . H8CA H 0.9591 0.4699 0.5028 0.027 Uiso 1 1 calc R . . H8CB H 0.9688 0.5664 0.5357 0.027 Uiso 1 1 calc R . . C9C C 0.7753(10) 0.5619(8) 0.4846(5) 0.0224(11) Uani 1 1 d U . . H9CA H 0.7197 0.5120 0.4741 0.027 Uiso 1 1 calc R . . H9CB H 0.7180 0.6034 0.5147 0.027 Uiso 1 1 calc R . . C10C C 0.7798(9) 0.7030(7) 0.3915(5) 0.018(2) Uani 1 1 d U . . H10F H 0.7187 0.7402 0.4196 0.022 Uiso 1 1 calc R . . C11C C 0.8389(5) 0.7473(4) 0.3211(2) 0.030(3) Uani 1 1 d GU . . C12C C 0.7989(6) 0.8442(4) 0.3046(3) 0.038(3) Uani 1 1 d GU . . H12C H 0.7420 0.8763 0.3379 0.046 Uiso 1 1 calc R . . C13C C 0.8437(7) 0.8931(3) 0.2383(3) 0.0180(18) Uani 1 1 d GU . . H13C H 0.8169 0.9579 0.2273 0.022 Uiso 1 1 calc R . . C14C C 0.9287(6) 0.8451(4) 0.1885(3) 0.025(3) Uani 1 1 d GU . . H14C H 0.9587 0.8779 0.1442 0.030 Uiso 1 1 calc R . . C15C C 0.9687(5) 0.7483(4) 0.2050(3) 0.020(5) Uani 1 1 d GU . . H15F H 1.0256 0.7162 0.1717 0.024 Uiso 1 1 calc R . . C16C C 0.9239(5) 0.6994(3) 0.2713(3) 0.017(2) Uani 1 1 d GU . . C1D C 0.7925(5) 0.3216(4) 0.4317(3) 0.034(3) Uani 1 1 d GU . . H1DA H 0.7207 0.3656 0.4096 0.041 Uiso 1 1 calc R . . C2D C 0.7595(6) 0.2446(5) 0.4814(4) 0.032(3) Uani 1 1 d GU . . H2DA H 0.6655 0.2371 0.4926 0.038 Uiso 1 1 calc R . . C3D C 0.8669(7) 0.1789(5) 0.5143(4) 0.043(3) Uani 1 1 d GDU . . H3DA H 0.8448 0.1274 0.5476 0.052 Uiso 1 1 calc R . . C4D C 1.0074(6) 0.1902(5) 0.4976(4) 0.043(3) Uani 1 1 d GDU . . H4DA H 1.0793 0.1462 0.5196 0.052 Uiso 1 1 calc R . . C5D C 1.0405(5) 0.2672(5) 0.4479(4) 0.013(2) Uani 1 1 d GU . . C6D C 0.9330(5) 0.3329(4) 0.4149(3) 0.028(3) Uani 1 1 d GU . . C7D C 1.1891(12) 0.2679(8) 0.4432(6) 0.032(3) Uani 1 1 d U . . H7DA H 1.2479 0.2222 0.4733 0.038 Uiso 1 1 calc R . . C8D C 1.4043(12) 0.3319(9) 0.3953(6) 0.038(3) Uani 1 1 d DU . . H8DA H 1.4421 0.2732 0.4250 0.045 Uiso 1 1 calc R . . H8DB H 1.4342 0.3846 0.4182 0.045 Uiso 1 1 calc R . . C9D C 1.4565(12) 0.3343(9) 0.3153(6) 0.038(3) Uani 1 1 d DU . . H9DA H 1.5590 0.3232 0.3150 0.045 Uiso 1 1 calc R . . H9DB H 1.4189 0.2852 0.2910 0.045 Uiso 1 1 calc R . . C10D C 1.5028(11) 0.4958(8) 0.2537(6) 0.035(3) Uani 1 1 d U . . H10C H 1.5977 0.4755 0.2642 0.042 Uiso 1 1 calc R . . C11D C 1.4780(6) 0.5875(4) 0.2195(3) 0.036(3) Uani 1 1 d GU . . C12D C 1.5948(6) 0.6383(5) 0.2169(4) 0.045(3) Uani 1 1 d GU . . H12D H 1.6778 0.6120 0.2420 0.054 Uiso 1 1 calc R . . C13D C 1.5874(7) 0.7284(5) 0.1767(4) 0.048(3) Uani 1 1 d GU . . H13D H 1.6655 0.7624 0.1750 0.057 Uiso 1 1 calc R . . C14D C 1.4632(8) 0.7677(4) 0.1391(4) 0.044(3) Uani 1 1 d GU . . H14D H 1.4582 0.8280 0.1122 0.053 Uiso 1 1 calc R . . C15D C 1.3464(7) 0.7169(5) 0.1417(4) 0.030(3) Uani 1 1 d GU . . H15G H 1.2633 0.7432 0.1165 0.036 Uiso 1 1 calc R . . C16D C 1.3538(6) 0.6268(5) 0.1819(4) 0.033(3) Uani 1 1 d GU . . C1E C 0.8126(5) 0.3896(3) 0.1492(2) 0.0169(18) Uani 1 1 d GU . . H1EB H 0.7970 0.3884 0.2007 0.020 Uiso 1 1 calc R . . C2E C 0.7276(6) 0.3437(5) 0.1059(3) 0.039(3) Uani 1 1 d GU . . H2EB H 0.6551 0.3118 0.1284 0.047 Uiso 1 1 calc R . . C3E C 0.7508(7) 0.3454(5) 0.0289(3) 0.046(3) Uani 1 1 d GU . . H3EA H 0.6939 0.3147 -0.0001 0.056 Uiso 1 1 calc R . . C4E C 0.8591(7) 0.3931(5) -0.0048(2) 0.024(2) Uani 1 1 d GU . . H4EA H 0.8746 0.3942 -0.0563 0.029 Uiso 1 1 calc R . . C5E C 0.9441(6) 0.4390(5) 0.0386(3) 0.019(2) Uani 1 1 d GU . . C6E C 0.9208(5) 0.4372(4) 0.1156(3) 0.029(3) Uani 1 1 d GU . . C7E C 1.0564(10) 0.4888(7) 0.0049(5) 0.026(2) Uani 1 1 d U . . H7EA H 1.0629 0.4934 -0.0474 0.031 Uiso 1 1 calc R . . C8E C 1.2600(10) 0.5752(8) -0.0018(6) 0.030(3) Uani 1 1 d U . . H8EA H 1.2594 0.6387 0.0123 0.036 Uiso 1 1 calc R . . H8EB H 1.2447 0.5803 -0.0559 0.036 Uiso 1 1 calc R . . C9E C 1.4013(10) 0.5177(8) 0.0193(6) 0.026(3) Uani 1 1 d U . . H9EA H 1.4174 0.5154 0.0731 0.031 Uiso 1 1 calc R . . H9EB H 1.3985 0.4532 0.0081 0.031 Uiso 1 1 calc R . . C10E C 1.6079(11) 0.6107(8) 0.0127(7) 0.034(3) Uani 1 1 d U . . H10D H 1.5937 0.6204 0.0628 0.040 Uiso 1 1 calc R . . C11E C 1.7213(5) 0.6492(4) -0.0282(3) 0.032(3) Uani 1 1 d GU . . C12E C 1.8096(7) 0.6904(5) 0.0169(3) 0.055(4) Uani 1 1 d GU . . H12F H 1.7927 0.6887 0.0683 0.066 Uiso 1 1 calc R . . C13E C 1.9231(7) 0.7340(6) -0.0149(4) 0.039(3) Uani 1 1 d GU . . H13E H 1.9822 0.7615 0.0153 0.046 Uiso 1 1 calc R . . C14E C 1.9484(7) 0.7365(6) -0.0918(4) 0.033(3) Uani 1 1 d GU . . H14F H 2.0243 0.7657 -0.1130 0.039 Uiso 1 1 calc R . . C15E C 1.8601(7) 0.6954(6) -0.1369(3) 0.047(3) Uani 1 1 d GU . . H15H H 1.8769 0.6971 -0.1883 0.056 Uiso 1 1 calc R . . C16E C 1.7465(6) 0.6517(5) -0.1051(3) 0.021(2) Uani 1 1 d GU . . C1F C 0.2598(6) -0.0062(5) 0.3994(3) 0.048(3) Uani 1 1 d GU . . H1FC H 0.2279 0.0027 0.4476 0.057 Uiso 1 1 calc R . . C2F C 0.1881(7) -0.0595(6) 0.3554(4) 0.051(3) Uani 1 1 d GU . . H2FB H 0.1082 -0.0863 0.3741 0.062 Uiso 1 1 calc R . . C3F C 0.2358(9) -0.0729(6) 0.2834(4) 0.055(3) Uani 1 1 d GDU . . H3FA H 0.1879 -0.1086 0.2539 0.066 Uiso 1 1 calc R . . C4F C 0.3552(8) -0.0329(6) 0.2554(4) 0.048(3) Uani 1 1 d GDU . . H4FA H 0.3871 -0.0418 0.2072 0.057 Uiso 1 1 calc R . . C5F C 0.4269(7) 0.0204(6) 0.2995(4) 0.033(3) Uani 1 1 d GU . . C6F C 0.3792(7) 0.0338(5) 0.3715(4) 0.045(3) Uani 1 1 d GU . . C7F C 0.5457(13) 0.0666(9) 0.2688(7) 0.040(3) Uani 1 1 d U . . H7FA H 0.5688 0.0614 0.2187 0.048 Uiso 1 1 calc R . . C8F C 0.7419(11) 0.1634(9) 0.2700(7) 0.038(3) Uani 1 1 d DU . . H8FA H 0.7247 0.2312 0.2724 0.046 Uiso 1 1 calc R . . H8FB H 0.7441 0.1533 0.2173 0.046 Uiso 1 1 calc R . . C9F C 0.8880(10) 0.1249(8) 0.3072(6) 0.031(3) Uani 1 1 d DU . . H9FA H 0.8902 0.1373 0.3593 0.037 Uiso 1 1 calc R . . H9FB H 0.9077 0.0571 0.3055 0.037 Uiso 1 1 calc R . . C10F C 1.0432(12) 0.1409(8) 0.2060(7) 0.036(3) Uani 1 1 d U . . H10E H 1.0098 0.0863 0.1930 0.043 Uiso 1 1 calc R . . C11F C 1.1555(5) 0.1844(4) 0.1614(3) 0.032(3) Uani 1 1 d GU . . C12F C 1.2115(7) 0.1378(4) 0.1022(4) 0.031(3) Uani 1 1 d GU . . H12G H 1.1728 0.0848 0.0896 0.038 Uiso 1 1 calc R . . C13F C 1.3255(7) 0.1705(6) 0.0619(4) 0.049(3) Uani 1 1 d GU . . H13F H 1.3629 0.1394 0.0223 0.059 Uiso 1 1 calc R . . C14F C 1.3834(7) 0.2498(6) 0.0808(4) 0.040(3) Uani 1 1 d GU . . H14G H 1.4596 0.2717 0.0538 0.048 Uiso 1 1 calc R . . C15F C 1.3274(7) 0.2963(5) 0.1400(4) 0.034(3) Uani 1 1 d GU . . H15I H 1.3661 0.3493 0.1526 0.041 Uiso 1 1 calc R . . C16F C 1.2135(6) 0.2636(4) 0.1803(3) 0.028(6) Uani 1 1 d GU . . C17 C 0.3666(6) 0.3730(3) 0.6151(3) 0.0567(8) Uani 1 1 d DU . . C18 C 0.7460(15) 0.0487(10) 0.0360(8) 0.0473(6) Uani 1 1 d U . . C19 C 1.2449(12) 0.6680(8) 0.3749(6) 0.052(3) Uani 1 1 d U . . H19A H 1.2843 0.6826 0.4209 0.078 Uiso 1 1 calc R . . H19B H 1.1509 0.7001 0.3678 0.078 Uiso 1 1 calc R . . H19C H 1.3029 0.6885 0.3333 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0254(3) 0.0334(3) 0.0277(3) -0.0110(2) 0.0025(2) -0.0028(2) Nd2 0.0237(3) 0.0404(4) 0.0257(3) -0.0132(3) 0.0019(2) -0.0049(3) S1 0.0960(19) 0.0645(17) 0.0323(14) -0.0086(12) -0.0146(13) -0.0387(15) S2 0.0584(13) 0.0466(14) 0.0360(12) -0.0052(10) -0.0063(10) -0.0015(11) F1 0.134(6) 0.135(7) 0.140(7) -0.028(6) -0.005(6) 0.009(5) F2 0.128(5) 0.089(5) 0.088(5) -0.013(4) -0.016(4) -0.054(4) F3 0.172(6) 0.074(5) 0.123(5) -0.035(4) 0.056(5) -0.045(4) F4 0.072(3) 0.066(3) 0.049(3) 0.005(2) 0.007(2) -0.003(3) F5 0.055(3) 0.082(4) 0.051(3) -0.019(3) -0.001(2) 0.003(3) F6 0.072(4) 0.093(5) 0.073(4) 0.013(4) 0.002(4) 0.005(4) O1 0.031(3) 0.038(4) 0.047(4) -0.005(3) -0.002(3) -0.015(3) O2 0.044(4) 0.043(4) 0.040(4) -0.007(3) 0.015(3) -0.004(3) O3 0.0456(17) 0.0481(19) 0.0552(19) -0.0172(16) -0.0171(15) 0.0034(15) O4 0.111(6) 0.115(6) 0.073(5) -0.037(4) -0.002(4) -0.031(5) O5 0.0456(17) 0.0481(19) 0.0552(19) -0.0172(16) -0.0171(15) 0.0034(15) O6 0.071(5) 0.065(5) 0.068(5) 0.028(4) -0.005(4) -0.009(4) O7 0.055(3) 0.082(4) 0.051(3) -0.019(3) -0.001(2) 0.003(3) O8 0.072(3) 0.066(3) 0.049(3) 0.005(2) 0.007(2) -0.003(3) O9 0.0456(17) 0.0481(19) 0.0552(19) -0.0172(16) -0.0171(15) 0.0034(15) O1B 0.017(3) 0.049(4) 0.018(3) -0.008(3) 0.003(2) -0.020(3) O2B 0.024(3) 0.048(4) 0.028(3) -0.003(3) 0.004(3) -0.007(3) O1C 0.027(3) 0.027(3) 0.016(3) -0.003(3) 0.000(2) 0.005(3) O2C 0.024(3) 0.040(4) 0.014(3) 0.002(3) 0.004(3) -0.004(3) O1D 0.021(3) 0.025(4) 0.024(3) -0.006(3) -0.003(3) 0.005(3) O2D 0.029(4) 0.038(4) 0.031(4) -0.008(3) 0.001(3) 0.002(3) O1E 0.022(3) 0.040(4) 0.019(3) -0.009(3) 0.002(2) -0.010(3) O2E 0.031(4) 0.051(4) 0.023(4) -0.006(3) 0.008(3) -0.012(3) O1F 0.047(4) 0.033(4) 0.032(4) -0.002(3) 0.019(3) -0.006(3) O2F 0.027(3) 0.028(4) 0.021(3) -0.017(3) 0.005(3) -0.004(3) N1 0.039(4) 0.028(4) 0.023(4) -0.005(3) -0.006(3) -0.016(3) N2 0.039(4) 0.034(4) 0.036(4) 0.003(4) 0.014(4) 0.005(4) N1B 0.026(8) 0.027(8) 0.037(8) -0.025(6) 0.003(6) 0.006(6) N2B 0.015(3) 0.033(4) 0.028(4) -0.012(3) 0.002(3) 0.005(3) N1C 0.0251(16) 0.0229(18) 0.0174(16) 0.0015(14) 0.0034(13) -0.0001(14) N2C 0.0251(16) 0.0229(18) 0.0174(16) 0.0015(14) 0.0034(13) -0.0001(14) N1D 0.034(4) 0.030(4) 0.050(5) -0.020(4) -0.018(4) -0.002(4) N2D 0.018(4) 0.049(5) 0.035(4) -0.021(4) 0.004(3) -0.013(3) N1E 0.029(4) 0.039(4) 0.042(4) -0.003(4) 0.006(3) -0.017(3) N2E 0.018(4) 0.040(4) 0.013(4) -0.010(3) 0.007(3) -0.017(3) N1F 0.031(4) 0.021(4) 0.032(4) -0.002(4) 0.006(3) 0.010(3) N2F 0.033(4) 0.039(5) 0.030(4) -0.012(4) 0.018(3) -0.005(3) C1 0.038(5) 0.043(5) 0.040(5) -0.011(4) 0.010(4) -0.005(4) C2 0.038(5) 0.045(5) 0.049(5) -0.018(4) 0.017(4) -0.008(4) C3 0.048(5) 0.050(5) 0.041(5) -0.028(4) 0.006(4) -0.013(4) C4 0.053(6) 0.050(6) 0.063(6) -0.027(5) 0.013(5) -0.007(5) C5 0.036(5) 0.039(5) 0.038(5) -0.024(4) 0.004(4) -0.008(4) C6 0.041(5) 0.044(5) 0.033(5) -0.002(4) -0.004(4) -0.002(4) C7 0.044(5) 0.034(5) 0.046(5) -0.015(4) 0.009(4) 0.000(4) C8 0.042(5) 0.037(5) 0.038(5) -0.002(4) 0.010(4) -0.018(4) C9 0.041(5) 0.040(5) 0.036(5) -0.003(4) 0.014(4) 0.005(4) C10 0.030(4) 0.033(5) 0.023(4) 0.002(4) 0.010(4) 0.001(4) C11 0.039(5) 0.038(5) 0.054(6) -0.004(4) 0.002(4) 0.001(4) C12 0.050(5) 0.069(6) 0.053(6) -0.014(5) -0.010(5) -0.008(5) C13 0.049(6) 0.064(6) 0.062(6) -0.015(5) -0.013(5) -0.013(5) C14 0.048(6) 0.049(6) 0.062(6) -0.003(5) 0.005(5) -0.002(5) C15 0.041(5) 0.047(6) 0.050(5) 0.006(5) -0.003(4) 0.018(4) C16 0.028(4) 0.026(5) 0.035(5) 0.003(4) 0.001(4) 0.005(4) C1B 0.018(4) 0.050(5) 0.030(5) -0.005(4) -0.004(4) -0.001(4) C2B 0.044(5) 0.039(5) 0.031(5) -0.016(4) 0.004(4) -0.017(4) C3B 0.028(4) 0.060(5) 0.028(4) -0.030(4) 0.013(4) -0.013(4) C4B 0.021(3) 0.032(3) 0.022(3) -0.011(3) 0.000(2) -0.005(3) C5B 0.015(4) 0.029(4) 0.027(4) -0.014(4) 0.000(3) -0.006(3) C6B 0.027(4) 0.036(4) 0.030(4) -0.020(4) 0.004(3) -0.017(4) C7B 0.014(4) 0.037(5) 0.022(4) -0.008(4) 0.010(3) 0.007(4) C8B 0.012(4) 0.032(5) 0.045(5) -0.016(4) -0.001(3) -0.003(3) C9B 0.026(4) 0.038(5) 0.043(5) -0.006(4) -0.009(4) 0.007(4) C10B 0.022(3) 0.015(3) 0.015(3) -0.005(2) -0.012(2) 0.003(2) C11B 0.042(5) 0.036(5) 0.038(5) -0.013(4) 0.001(4) 0.005(4) C12B 0.032(4) 0.030(5) 0.026(4) -0.003(4) -0.006(4) 0.009(4) C13B 0.046(5) 0.025(5) 0.031(5) 0.005(4) -0.003(4) -0.011(4) C14B 0.038(5) 0.034(5) 0.024(4) -0.001(4) 0.010(4) -0.008(4) C15B 0.028(4) 0.031(5) 0.022(4) 0.002(4) 0.006(4) 0.002(4) C16B 0.022(4) 0.023(4) 0.020(4) -0.001(4) -0.017(3) 0.008(3) C1C 0.037(3) 0.043(3) 0.038(3) -0.010(3) 0.007(3) -0.008(3) C2C 0.037(5) 0.062(6) 0.016(4) -0.004(4) 0.004(4) -0.018(4) C3C 0.059(5) 0.040(5) 0.050(5) -0.003(4) -0.012(4) -0.012(4) C4C 0.024(3) 0.019(3) 0.016(3) 0.000(2) 0.000(2) -0.002(2) C5C 0.012(4) 0.016(4) 0.013(3) -0.002(3) 0.001(3) -0.001(3) C6C 0.024(4) 0.035(5) 0.012(4) 0.007(4) -0.011(3) -0.001(4) C7C 0.022(4) 0.046(5) 0.037(5) -0.009(4) -0.006(4) 0.008(4) C8C 0.025(2) 0.025(2) 0.017(2) -0.0025(18) 0.0033(17) 0.0002(18) C9C 0.025(2) 0.025(2) 0.017(2) -0.0025(18) 0.0033(17) 0.0002(18) C10C 0.013(4) 0.025(4) 0.019(4) -0.007(3) -0.003(3) -0.004(3) C11C 0.028(5) 0.031(5) 0.032(5) -0.004(4) -0.015(4) -0.005(4) C12C 0.048(5) 0.034(5) 0.035(5) -0.014(4) -0.009(4) -0.005(4) C13C 0.020(3) 0.016(3) 0.017(3) 0.002(2) -0.007(2) -0.006(2) C14C 0.024(4) 0.018(4) 0.032(5) 0.009(4) -0.009(4) -0.012(3) C15C 0.015(6) 0.026(6) 0.021(6) -0.007(4) 0.007(4) -0.009(4) C16C 0.017(3) 0.019(3) 0.016(3) -0.008(2) -0.004(2) -0.001(2) C1D 0.034(5) 0.042(5) 0.027(5) -0.007(4) -0.004(4) 0.000(4) C2D 0.029(5) 0.036(5) 0.033(5) -0.011(4) 0.000(4) -0.009(4) C3D 0.059(6) 0.036(6) 0.034(5) -0.007(4) 0.003(5) 0.000(5) C4D 0.051(6) 0.039(5) 0.042(5) -0.017(4) -0.006(4) -0.006(4) C5D 0.023(4) 0.007(4) 0.009(4) 0.001(3) -0.010(3) -0.001(3) C6D 0.028(5) 0.030(5) 0.029(5) -0.013(4) 0.015(4) -0.007(4) C7D 0.040(5) 0.027(5) 0.028(5) -0.006(4) -0.011(4) 0.006(4) C8D 0.034(5) 0.028(5) 0.051(6) -0.003(4) -0.006(4) -0.005(4) C9D 0.031(5) 0.035(5) 0.049(5) -0.020(4) 0.001(4) 0.001(4) C10D 0.020(5) 0.053(5) 0.038(5) -0.026(4) 0.000(4) -0.006(4) C11D 0.032(5) 0.051(6) 0.029(5) -0.020(4) 0.009(4) -0.008(4) C12D 0.031(5) 0.060(6) 0.048(5) -0.019(5) 0.003(4) -0.012(4) C13D 0.045(5) 0.064(6) 0.042(5) -0.019(5) 0.000(4) -0.029(5) C14D 0.039(5) 0.055(6) 0.040(5) -0.007(5) 0.015(4) -0.007(5) C15D 0.033(5) 0.037(5) 0.025(5) -0.012(4) 0.000(4) -0.019(4) C16D 0.024(5) 0.047(5) 0.031(5) -0.020(4) 0.005(4) 0.004(4) C1E 0.019(3) 0.019(3) 0.013(3) -0.003(2) 0.002(2) -0.004(2) C2E 0.031(5) 0.049(5) 0.037(5) -0.003(4) 0.013(4) -0.005(4) C3E 0.050(5) 0.058(5) 0.038(5) -0.020(4) -0.008(4) -0.019(4) C4E 0.032(4) 0.034(4) 0.014(4) -0.011(3) 0.009(3) -0.027(3) C5E 0.020(4) 0.020(4) 0.017(4) -0.001(3) -0.005(3) -0.010(3) C6E 0.025(4) 0.035(5) 0.027(4) -0.013(4) 0.003(4) 0.003(4) C7E 0.026(4) 0.031(5) 0.020(4) -0.010(4) 0.005(3) 0.003(4) C8E 0.027(4) 0.043(5) 0.025(4) -0.013(4) 0.013(3) -0.012(4) C9E 0.025(4) 0.040(5) 0.017(4) -0.009(4) 0.005(4) -0.013(4) C10E 0.026(5) 0.042(5) 0.035(5) -0.009(4) 0.002(4) -0.004(4) C11E 0.026(5) 0.036(5) 0.037(5) -0.014(4) -0.001(4) -0.005(4) C12E 0.052(6) 0.075(7) 0.041(6) -0.025(5) 0.004(5) -0.001(5) C13E 0.032(5) 0.058(6) 0.033(5) -0.013(4) 0.002(4) -0.026(4) C14E 0.026(5) 0.046(5) 0.030(5) -0.002(4) -0.006(4) -0.021(4) C15E 0.042(5) 0.059(6) 0.041(5) -0.007(5) 0.005(4) -0.010(5) C16E 0.016(4) 0.024(5) 0.022(4) 0.003(4) -0.004(4) -0.010(4) C1F 0.040(5) 0.044(6) 0.056(6) 0.005(5) 0.014(5) -0.001(4) C2F 0.025(5) 0.055(6) 0.073(6) -0.003(5) -0.003(4) -0.005(4) C3F 0.049(5) 0.056(6) 0.061(6) -0.007(5) -0.022(5) -0.010(5) C4F 0.046(5) 0.050(6) 0.046(5) -0.008(5) -0.003(4) 0.002(4) C5F 0.022(5) 0.041(5) 0.034(5) -0.003(4) -0.004(4) 0.008(4) C6F 0.034(5) 0.044(6) 0.054(6) -0.010(5) 0.001(5) 0.011(4) C7F 0.040(5) 0.043(6) 0.034(5) -0.010(4) -0.005(4) 0.010(4) C8F 0.042(5) 0.031(5) 0.039(5) 0.001(4) 0.013(4) 0.003(4) C9F 0.038(5) 0.031(5) 0.027(5) -0.019(4) -0.002(4) -0.007(4) C10F 0.031(5) 0.038(5) 0.043(5) -0.016(4) -0.005(4) -0.018(4) C11F 0.041(5) 0.027(5) 0.029(5) -0.012(4) 0.002(4) -0.005(4) C12F 0.037(5) 0.025(4) 0.039(5) -0.020(4) 0.001(4) -0.017(4) C13F 0.057(6) 0.057(6) 0.034(5) -0.018(5) 0.020(4) 0.000(5) C14F 0.036(5) 0.043(5) 0.044(5) -0.009(4) 0.000(4) -0.020(4) C15F 0.031(5) 0.036(5) 0.042(5) -0.020(4) 0.002(4) -0.022(4) C16F 0.027(8) 0.031(9) 0.027(8) -0.015(7) 0.000(6) -0.003(6) C17 0.0860(19) 0.0595(17) 0.0323(14) -0.0086(12) -0.0146(13) -0.0387(15) C18 0.0584(13) 0.0466(14) 0.0360(12) -0.0052(10) -0.0063(10) -0.0015(11) C19 0.049(5) 0.052(5) 0.056(5) -0.029(4) 0.001(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O2B 2.390(7) . ? Nd1 O2E 2.437(7) 1_456 ? Nd1 O1B 2.429(6) . ? Nd1 O1C 2.447(6) . ? Nd1 O1 2.510(7) . ? Nd1 O3 2.538(5) . ? Nd1 N1B 2.672(7) . ? Nd1 N2B 2.701(7) . ? Nd2 O2D 2.417(8) . ? Nd2 O1E 2.428(6) . ? Nd2 O1D 2.460(7) . ? Nd2 O2F 2.477(7) . ? Nd2 O2C 2.489(7) . ? Nd2 O9 2.642(8) . ? Nd2 N2D 2.635(8) . ? Nd2 N1D 2.722(9) . ? S1 O4 1.383(5) . ? S1 O3 1.423(5) . ? S1 O5 1.518(5) . ? S1 C17 1.766(5) . ? S2 O8 1.338(10) . ? S2 O6 1.410(11) . ? S2 O7 1.433(10) . ? S2 C18 2.023(13) . ? F1 C17 1.399(6) . ? F2 C17 1.282(6) . ? F3 C17 1.325(6) . ? F4 C18 1.413(16) . ? F5 C18 1.379(15) . ? F6 C18 1.169(16) . ? O1 C6 1.348(9) . ? O1 H1A 0.8200 . ? O2 C16 1.221(10) . ? O2 H2A 0.8200 . ? O9 C19 1.516(13) . ? O9 H9C 0.8200 . ? O1B C6B 1.347(8) . ? O2B C16B 1.369(8) . ? O1C C6C 1.333(8) . ? O1C H1CA 0.8200 . ? O2C C16C 1.328(9) . ? O2C H2CA 0.8200 . ? O1D C6D 1.342(9) . ? O2D C16D 1.370(10) . ? O1E C6E 1.356(8) . ? O1E H1EA 0.8200 . ? O2E C16E 1.290(9) . ? O2E Nd1 2.437(7) 1_654 ? O2E H2EA 0.8200 . ? O1F C6F 1.462(10) . ? O1F H1FA 0.8200 . ? O2F C16F 1.330(8) . ? O2F H2FA 0.8200 . ? N1 C7 1.395(13) . ? N1 C8 1.430(13) . ? N2 C10 1.203(14) . ? N2 C9 1.441(14) . ? N1B C7B 1.191(11) . ? N1B C8B 1.510(12) . ? N2B C10B 1.210(11) . ? N2B C9B 1.494(12) . ? N1C C7C 1.304(13) . ? N1C C8C 1.485(11) . ? N2C C10C 1.277(12) . ? N2C C9C 1.432(12) . ? N1D C7D 1.448(14) . ? N1D C8D 1.454(14) . ? N2D C10D 1.424(14) . ? N2D C9D 1.434(14) . ? N1E C7E 1.257(13) . ? N1E C8E 1.481(13) . ? N2E C10E 1.377(14) . ? N2E C9E 1.476(13) . ? N1F C7F 1.344(16) . ? N1F C8F 1.469(14) . ? N2F C10F 1.237(14) . ? N2F C9F 1.511(14) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1B 0.9300 . ? C2 C3 1.3900 . ? C2 H2B 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C7 1.312(13) . ? C5 C6 1.3900 . ? C7 H7B 0.9300 . ? C8 C9 1.494(13) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.485(11) . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B H1BA 0.9300 . ? C2B C3B 1.3900 . ? C2B H2BA 0.9300 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B C7B 1.526(10) . ? C7B H7BA 0.9300 . ? C8B C9B 1.503(14) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C10B C11B 1.506(10) . ? C10B H10B 0.9300 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C12B H12B 0.9300 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15D 0.9300 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C1C H1CB 0.9300 . ? C2C C3C 1.3900 . ? C2C H2CB 0.9300 . ? C3C C4C 1.3900 . ? C3C H3CA 0.9300 . ? C4C C5C 1.3900 . ? C4C H4CA 0.9300 . ? C5C C7C 1.391(12) . ? C5C C6C 1.3900 . ? C7C H7CA 0.9300 . ? C8C C9C 1.521(10) . ? C8C H8CA 0.9700 . ? C8C H8CB 0.9700 . ? C9C H9CA 0.9700 . ? C9C H9CB 0.9700 . ? C10C C11C 1.475(10) . ? C10C H10F 0.9300 . ? C11C C12C 1.3900 . ? C11C C16C 1.3900 . ? C12C C13C 1.3900 . ? C12C H12C 0.9300 . ? C13C C14C 1.3900 . ? C13C H13C 0.9300 . ? C14C C15C 1.3900 . ? C14C H14C 0.9300 . ? C15C C16C 1.3900 . ? C15C H15F 0.9300 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D H1DA 0.9300 . ? C2D C3D 1.3900 . ? C2D H2DA 0.9300 . ? C3D C4D 1.3900 . ? C3D H3DA 0.9300 . ? C4D C5D 1.3900 . ? C4D H4DA 0.9300 . ? C5D C6D 1.3900 . ? C5D C7D 1.416(12) . ? C7D H7DA 0.9300 . ? C8D C9D 1.507(14) . ? C8D H8DA 0.9700 . ? C8D H8DB 0.9700 . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C10D C11D 1.373(13) . ? C10D H10C 0.9300 . ? C11D C12D 1.3900 . ? C11D C16D 1.3900 . ? C12D C13D 1.3900 . ? C12D H12D 0.9300 . ? C13D C14D 1.3900 . ? C13D H13D 0.9300 . ? C14D C15D 1.3900 . ? C14D H14D 0.9300 . ? C15D C16D 1.3900 . ? C15D H15G 0.9300 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C1E H1EB 0.9300 . ? C2E C3E 1.3900 . ? C2E H2EB 0.9300 . ? C3E C4E 1.3900 . ? C3E H3EA 0.9300 . ? C4E C5E 1.3900 . ? C4E H4EA 0.9300 . ? C5E C6E 1.3900 . ? C5E C7E 1.437(11) . ? C7E H7EA 0.9300 . ? C8E C9E 1.519(11) . ? C8E H8EA 0.9700 . ? C8E H8EB 0.9700 . ? C9E H9EA 0.9700 . ? C9E H9EB 0.9700 . ? C10E C11E 1.423(12) . ? C10E H10D 0.9300 . ? C11E C12E 1.3900 . ? C11E C16E 1.3900 . ? C12E C13E 1.3900 . ? C12E H12F 0.9300 . ? C13E C14E 1.3900 . ? C13E H13E 0.9300 . ? C14E C15E 1.3900 . ? C14E H14F 0.9300 . ? C15E C16E 1.3900 . ? C15E H15H 0.9300 . ? C1F C2F 1.3900 . ? C1F C6F 1.3900 . ? C1F H1FC 0.9300 . ? C2F C3F 1.3900 . ? C2F H2FB 0.9300 . ? C3F C4F 1.3900 . ? C3F H3FA 0.9300 . ? C4F C5F 1.3900 . ? C4F H4FA 0.9300 . ? C5F C6F 1.3900 . ? C5F C7F 1.443(14) . ? C7F H7FA 0.9300 . ? C8F C9F 1.559(13) . ? C8F H8FA 0.9700 . ? C8F H8FB 0.9700 . ? C9F H9FA 0.9700 . ? C9F H9FB 0.9700 . ? C10F C11F 1.476(12) . ? C10F H10E 0.9300 . ? C11F C12F 1.3900 . ? C11F C16F 1.3900 . ? C12F C13F 1.3900 . ? C12F H12G 0.9300 . ? C13F C14F 1.3900 . ? C13F H13F 0.9300 . ? C14F C15F 1.3900 . ? C14F H14G 0.9300 . ? C15F C16F 1.3900 . ? C15F H15I 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Nd1 O2E 98.4(2) . 1_456 ? O2B Nd1 O1B 159.1(2) . . ? O2E Nd1 O1B 70.7(2) 1_456 . ? O2B Nd1 O1C 74.1(2) . . ? O2E Nd1 O1C 80.7(2) 1_456 . ? O1B Nd1 O1C 86.4(2) . . ? O2B Nd1 O1 85.5(2) . . ? O2E Nd1 O1 72.4(2) 1_456 . ? O1B Nd1 O1 106.9(2) . . ? O1C Nd1 O1 143.4(2) . . ? O2B Nd1 O3 92.4(2) . . ? O2E Nd1 O3 146.4(2) 1_456 . ? O1B Nd1 O3 88.3(2) . . ? O1C Nd1 O3 71.74(19) . . ? O1 Nd1 O3 140.5(2) . . ? O2B Nd1 N1B 133.7(2) . . ? O2E Nd1 N1B 118.2(2) 1_456 . ? O1B Nd1 N1B 66.2(2) . . ? O1C Nd1 N1B 135.6(2) . . ? O1 Nd1 N1B 80.1(2) . . ? O3 Nd1 N1B 73.1(2) . . ? O2B Nd1 N2B 67.3(2) . . ? O2E Nd1 N2B 142.2(3) 1_456 . ? O1B Nd1 N2B 132.0(2) . . ? O1C Nd1 N2B 124.1(2) . . ? O1 Nd1 N2B 71.7(2) . . ? O3 Nd1 N2B 71.2(2) . . ? N1B Nd1 N2B 66.4(2) . . ? O2D Nd2 O1E 71.4(2) . . ? O2D Nd2 O1D 158.0(2) . . ? O1E Nd2 O1D 98.8(2) . . ? O2D Nd2 O2F 108.7(2) . . ? O1E Nd2 O2F 73.7(2) . . ? O1D Nd2 O2F 86.3(2) . . ? O2D Nd2 O2C 84.5(2) . . ? O1E Nd2 O2C 79.7(2) . . ? O1D Nd2 O2C 74.2(2) . . ? O2F Nd2 O2C 144.1(2) . . ? O2D Nd2 O9 85.4(3) . . ? O1E Nd2 O9 146.5(2) . . ? O1D Nd2 O9 94.0(2) . . ? O2F Nd2 O9 138.3(2) . . ? O2C Nd2 O9 74.1(2) . . ? O2D Nd2 N2D 68.6(3) . . ? O1E Nd2 N2D 117.3(2) . . ? O1D Nd2 N2D 132.2(2) . . ? O2F Nd2 N2D 75.9(3) . . ? O2C Nd2 N2D 139.0(3) . . ? O9 Nd2 N2D 73.4(3) . . ? O2D Nd2 N1D 130.8(3) . . ? O1E Nd2 N1D 141.4(3) . . ? O1D Nd2 N1D 69.0(3) . . ? O2F Nd2 N1D 69.2(3) . . ? O2C Nd2 N1D 127.2(3) . . ? O9 Nd2 N1D 72.2(3) . . ? N2D Nd2 N1D 63.3(3) . . ? O4 S1 O3 121.2(4) . . ? O4 S1 O5 111.6(4) . . ? O3 S1 O5 107.9(3) . . ? O4 S1 C17 110.2(4) . . ? O3 S1 C17 103.4(3) . . ? O5 S1 C17 100.2(3) . . ? O8 S2 O6 120.1(7) . . ? O8 S2 O7 108.9(6) . . ? O6 S2 O7 120.4(6) . . ? O8 S2 C18 103.1(6) . . ? O6 S2 C18 106.7(6) . . ? O7 S2 C18 92.1(5) . . ? C6 O1 Nd1 142.4(5) . . ? C6 O1 H1A 109.5 . . ? Nd1 O1 H1A 91.5 . . ? C16 O2 H2A 109.5 . . ? S1 O3 Nd1 168.6(4) . . ? C19 O9 Nd2 127.8(6) . . ? C19 O9 H9C 109.5 . . ? Nd2 O9 H9C 100.1 . . ? C6B O1B Nd1 134.5(4) . . ? C16B O2B Nd1 145.6(5) . . ? C6C O1C Nd1 148.3(4) . . ? C6C O1C H1CA 109.4 . . ? Nd1 O1C H1CA 90.4 . . ? C16C O2C Nd2 145.4(5) . . ? C16C O2C H2CA 109.5 . . ? Nd2 O2C H2CA 91.2 . . ? C6D O1D Nd2 139.3(5) . . ? C16D O2D Nd2 137.9(5) . . ? C6E O1E Nd2 148.3(5) . . ? C6E O1E H1EA 109.5 . . ? Nd2 O1E H1EA 89.3 . . ? C16E O2E Nd1 143.2(6) . 1_654 ? C16E O2E H2EA 109.4 . . ? Nd1 O2E H2EA 95.5 1_654 . ? C6F O1F H1FA 109.4 . . ? C16F O2F Nd2 139.4(5) . . ? C16F O2F H2FA 109.5 . . ? Nd2 O2F H2FA 92.2 . . ? C7 N1 C8 129.1(9) . . ? C10 N2 C9 117.5(9) . . ? C7B N1B C8B 112.1(7) . . ? C7B N1B Nd1 134.2(6) . . ? C8B N1B Nd1 111.3(5) . . ? C10B N2B C9B 114.8(8) . . ? C10B N2B Nd1 128.2(6) . . ? C9B N2B Nd1 115.1(6) . . ? C7C N1C C8C 120.2(8) . . ? C10C N2C C9C 129.9(9) . . ? C7D N1D C8D 114.6(9) . . ? C7D N1D Nd2 131.1(7) . . ? C8D N1D Nd2 113.8(7) . . ? C10D N2D C9D 123.3(9) . . ? C10D N2D Nd2 122.3(7) . . ? C9D N2D Nd2 112.9(7) . . ? C7E N1E C8E 122.6(9) . . ? C10E N2E C9E 121.1(8) . . ? C7F N1F C8F 120.5(10) . . ? C10F N2F C9F 115.8(10) . . ? C2 C1 C6 120.0 . . ? C2 C1 H1B 120.0 . . ? C6 C1 H1B 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2B 120.0 . . ? C1 C2 H2B 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C7 C5 C6 122.0(7) . . ? C7 C5 C4 118.0(7) . . ? C6 C5 C4 120.0 . . ? O1 C6 C5 121.1(5) . . ? O1 C6 C1 118.8(5) . . ? C5 C6 C1 120.0 . . ? C5 C7 N1 129.6(10) . . ? C5 C7 H7B 115.2 . . ? N1 C7 H7B 115.3 . . ? N1 C8 C9 114.7(8) . . ? N1 C8 H8B 108.5 . . ? C9 C8 H8B 108.7 . . ? N1 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? H8B C8 H8A 107.6 . . ? N2 C9 C8 111.1(9) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 120.7(9) . . ? N2 C10 H10A 119.7 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 118.1(5) . . ? C16 C11 C10 121.8(6) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? O2 C16 C15 115.6(5) . . ? O2 C16 C11 124.4(5) . . ? C15 C16 C11 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B H1BA 120.0 . . ? C6B C1B H1BA 120.0 . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2BA 120.0 . . ? C3B C2B H2BA 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3BA 120.0 . . ? C2B C3B H3BA 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4BA 120.0 . . ? C3B C4B H4BA 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B C7B 123.8(5) . . ? C4B C5B C7B 116.2(5) . . ? O1B C6B C5B 122.8(4) . . ? O1B C6B C1B 117.2(4) . . ? C5B C6B C1B 120.0 . . ? N1B C7B C5B 123.0(8) . . ? N1B C7B H7BA 118.5 . . ? C5B C7B H7BA 118.5 . . ? C9B C8B N1B 113.5(8) . . ? C9B C8B H8BA 108.8 . . ? N1B C8B H8BA 108.9 . . ? C9B C8B H8BB 108.9 . . ? N1B C8B H8BB 108.8 . . ? H8BA C8B H8BB 107.7 . . ? N2B C9B C8B 111.7(8) . . ? N2B C9B H9BA 109.3 . . ? C8B C9B H9BA 109.3 . . ? N2B C9B H9BB 109.2 . . ? C8B C9B H9BB 109.3 . . ? H9BA C9B H9BB 107.9 . . ? N2B C10B C11B 131.2(7) . . ? N2B C10B H10B 114.4 . . ? C11B C10B H10B 114.4 . . ? C12B C11B C16B 120.0 . . ? C12B C11B C10B 116.3(4) . . ? C16B C11B C10B 123.0(4) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B H13B 120.0 . . ? C14B C13B H13B 120.0 . . ? C15B C14B C13B 120.0 . . ? C15B C14B H14B 120.0 . . ? C13B C14B H14B 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15D 120.0 . . ? C14B C15B H15D 120.0 . . ? O2B C16B C15B 121.3(4) . . ? O2B C16B C11B 118.7(4) . . ? C15B C16B C11B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C H1CB 119.9 . . ? C6C C1C H1CB 120.1 . . ? C3C C2C C1C 120.0 . . ? C3C C2C H2CB 120.0 . . ? C1C C2C H2CB 120.0 . . ? C2C C3C C4C 120.0 . . ? C2C C3C H3CA 120.0 . . ? C4C C3C H3CA 120.0 . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4CA 120.0 . . ? C3C C4C H4CA 120.0 . . ? C7C C5C C6C 116.8(6) . . ? C7C C5C C4C 123.1(6) . . ? C6C C5C C4C 120.0 . . ? O1C C6C C5C 122.7(4) . . ? O1C C6C C1C 117.2(4) . . ? C5C C6C C1C 120.0 . . ? N1C C7C C5C 125.4(9) . . ? N1C C7C H7CA 117.3 . . ? C5C C7C H7CA 117.3 . . ? N1C C8C C9C 106.4(6) . . ? N1C C8C H8CA 110.4 . . ? C9C C8C H8CA 110.4 . . ? N1C C8C H8CB 110.5 . . ? C9C C8C H8CB 110.4 . . ? H8CA C8C H8CB 108.6 . . ? N2C C9C C8C 111.6(7) . . ? N2C C9C H9CA 109.3 . . ? C8C C9C H9CA 109.3 . . ? N2C C9C H9CB 109.3 . . ? C8C C9C H9CB 109.3 . . ? H9CA C9C H9CB 108.0 . . ? N2C C10C C11C 121.9(8) . . ? N2C C10C H10F 119.0 . . ? C11C C10C H10F 119.1 . . ? C12C C11C C16C 120.0 . . ? C12C C11C C10C 114.8(5) . . ? C16C C11C C10C 125.2(5) . . ? C11C C12C C13C 120.0 . . ? C11C C12C H12C 120.0 . . ? C13C C12C H12C 120.0 . . ? C14C C13C C12C 120.0 . . ? C14C C13C H13C 120.0 . . ? C12C C13C H13C 120.0 . . ? C15C C14C C13C 120.0 . . ? C15C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C14C C15C C16C 120.0 . . ? C14C C15C H15F 120.0 . . ? C16C C15C H15F 120.0 . . ? O2C C16C C15C 123.6(4) . . ? O2C C16C C11C 116.4(4) . . ? C15C C16C C11C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D H1DA 120.0 . . ? C6D C1D H1DA 120.0 . . ? C1D C2D C3D 120.0 . . ? C1D C2D H2DA 120.0 . . ? C3D C2D H2DA 120.0 . . ? C4D C3D C2D 120.0 . . ? C4D C3D H3DA 120.0 . . ? C2D C3D H3DA 120.0 . . ? C3D C4D C5D 120.0 . . ? C3D C4D H4DA 120.0 . . ? C5D C4D H4DA 120.0 . . ? C4D C5D C6D 120.0 . . ? C4D C5D C7D 110.3(6) . . ? C6D C5D C7D 129.6(6) . . ? O1D C6D C5D 125.8(4) . . ? O1D C6D C1D 114.2(4) . . ? C5D C6D C1D 120.0 . . ? N1D C7D C5D 120.9(9) . . ? N1D C7D H7DA 119.5 . . ? C5D C7D H7DA 119.5 . . ? N1D C8D C9D 107.2(9) . . ? N1D C8D H8DA 110.3 . . ? C9D C8D H8DA 110.3 . . ? N1D C8D H8DB 110.2 . . ? C9D C8D H8DB 110.2 . . ? H8DA C8D H8DB 108.5 . . ? N2D C9D C8D 107.9(9) . . ? N2D C9D H9DA 110.1 . . ? C8D C9D H9DA 110.2 . . ? N2D C9D H9DB 110.1 . . ? C8D C9D H9DB 110.1 . . ? H9DA C9D H9DB 108.4 . . ? C11D C10D N2D 131.8(9) . . ? C11D C10D H10C 114.1 . . ? N2D C10D H10C 114.1 . . ? C10D C11D C12D 114.6(6) . . ? C10D C11D C16D 125.0(6) . . ? C12D C11D C16D 120.0 . . ? C13D C12D C11D 120.0 . . ? C13D C12D H12D 120.0 . . ? C11D C12D H12D 120.0 . . ? C12D C13D C14D 120.0 . . ? C12D C13D H13D 120.0 . . ? C14D C13D H13D 120.0 . . ? C13D C14D C15D 120.0 . . ? C13D C14D H14D 120.0 . . ? C15D C14D H14D 120.0 . . ? C16D C15D C14D 120.0 . . ? C16D C15D H15G 120.0 . . ? C14D C15D H15G 120.0 . . ? O2D C16D C15D 121.7(5) . . ? O2D C16D C11D 118.3(5) . . ? C15D C16D C11D 120.0 . . ? C2E C1E C6E 120.0 . . ? C2E C1E H1EB 120.0 . . ? C6E C1E H1EB 120.0 . . ? C3E C2E C1E 120.0 . . ? C3E C2E H2EB 120.0 . . ? C1E C2E H2EB 120.0 . . ? C2E C3E C4E 120.0 . . ? C2E C3E H3EA 120.0 . . ? C4E C3E H3EA 120.0 . . ? C5E C4E C3E 120.0 . . ? C5E C4E H4EA 120.0 . . ? C3E C4E H4EA 120.0 . . ? C4E C5E C6E 120.0 . . ? C4E C5E C7E 120.8(5) . . ? C6E C5E C7E 119.2(5) . . ? O1E C6E C5E 121.6(4) . . ? O1E C6E C1E 118.4(4) . . ? C5E C6E C1E 120.0 . . ? N1E C7E C5E 126.9(9) . . ? N1E C7E H7EA 116.5 . . ? C5E C7E H7EA 116.6 . . ? N1E C8E C9E 108.4(7) . . ? N1E C8E H8EA 110.0 . . ? C9E C8E H8EA 110.0 . . ? N1E C8E H8EB 110.0 . . ? C9E C8E H8EB 110.0 . . ? H8EA C8E H8EB 108.4 . . ? N2E C9E C8E 111.6(7) . . ? N2E C9E H9EA 109.3 . . ? C8E C9E H9EA 109.3 . . ? N2E C9E H9EB 109.3 . . ? C8E C9E H9EB 109.3 . . ? H9EA C9E H9EB 108.0 . . ? N2E C10E C11E 120.0(10) . . ? N2E C10E H10D 120.0 . . ? C11E C10E H10D 120.0 . . ? C12E C11E C16E 120.0 . . ? C12E C11E C10E 112.7(6) . . ? C16E C11E C10E 127.2(6) . . ? C11E C12E C13E 120.0 . . ? C11E C12E H12F 120.0 . . ? C13E C12E H12F 120.0 . . ? C14E C13E C12E 120.0 . . ? C14E C13E H13E 120.0 . . ? C12E C13E H13E 120.0 . . ? C13E C14E C15E 120.0 . . ? C13E C14E H14F 120.0 . . ? C15E C14E H14F 120.0 . . ? C16E C15E C14E 120.0 . . ? C16E C15E H15H 120.0 . . ? C14E C15E H15H 120.0 . . ? O2E C16E C15E 120.3(5) . . ? O2E C16E C11E 119.4(5) . . ? C15E C16E C11E 120.0 . . ? C2F C1F C6F 120.0 . . ? C2F C1F H1FC 120.0 . . ? C6F C1F H1FC 120.0 . . ? C1F C2F C3F 120.0 . . ? C1F C2F H2FB 120.0 . . ? C3F C2F H2FB 120.0 . . ? C2F C3F C4F 120.0 . . ? C2F C3F H3FA 120.0 . . ? C4F C3F H3FA 120.0 . . ? C3F C4F C5F 120.0 . . ? C3F C4F H4FA 120.0 . . ? C5F C4F H4FA 120.0 . . ? C6F C5F C4F 120.0 . . ? C6F C5F C7F 120.0(7) . . ? C4F C5F C7F 119.9(7) . . ? C5F C6F C1F 120.0 . . ? C5F C6F O1F 119.5(5) . . ? C1F C6F O1F 120.5(5) . . ? N1F C7F C5F 124.8(10) . . ? N1F C7F H7FA 117.5 . . ? C5F C7F H7FA 117.7 . . ? N1F C8F C9F 112.1(9) . . ? N1F C8F H8FA 109.2 . . ? C9F C8F H8FA 109.2 . . ? N1F C8F H8FB 109.2 . . ? C9F C8F H8FB 109.2 . . ? H8FA C8F H8FB 107.9 . . ? N2F C9F C8F 104.8(8) . . ? N2F C9F H9FA 110.8 . . ? C8F C9F H9FA 110.7 . . ? N2F C9F H9FB 110.8 . . ? C8F C9F H9FB 110.7 . . ? H9FA C9F H9FB 108.9 . . ? N2F C10F C11F 119.3(10) . . ? N2F C10F H10E 120.3 . . ? C11F C10F H10E 120.4 . . ? C12F C11F C16F 120.0 . . ? C12F C11F C10F 117.1(6) . . ? C16F C11F C10F 122.7(6) . . ? C13F C12F C11F 120.0 . . ? C13F C12F H12G 120.0 . . ? C11F C12F H12G 120.0 . . ? C12F C13F C14F 120.0 . . ? C12F C13F H13F 120.0 . . ? C14F C13F H13F 120.0 . . ? C15F C14F C13F 120.0 . . ? C15F C14F H14G 120.0 . . ? C13F C14F H14G 120.0 . . ? C14F C15F C16F 120.0 . . ? C14F C15F H15I 120.0 . . ? C16F C15F H15I 120.0 . . ? O2F C16F C15F 118.9(5) . . ? O2F C16F C11F 121.0(5) . . ? C15F C16F C11F 120.0 . . ? F2 C17 F3 109.4(5) . . ? F2 C17 F1 107.1(5) . . ? F3 C17 F1 104.9(5) . . ? F2 C17 S1 116.6(4) . . ? F3 C17 S1 112.6(4) . . ? F1 C17 S1 105.4(4) . . ? F6 C18 F5 120.2(13) . . ? F6 C18 F4 109.5(11) . . ? F5 C18 F4 110.7(11) . . ? F6 C18 S2 109.2(10) . . ? F5 C18 S2 103.0(8) . . ? F4 C18 S2 102.6(8) . . ? O9 C19 H19A 109.5 . . ? O9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.150 _refine_diff_density_min -1.934 _refine_diff_density_rms 0.166 # Attachment 'Complex-3.CIF' data_Complex-3 _database_code_depnum_ccdc_archive 'CCDC 733183' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H96 Er2 F3 N12 O16 S, C F3 O3 S' _chemical_formula_sum 'C99 H96 Er2 F6 N12 O19 S2' _chemical_formula_weight 2270.52 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.3209(19) _cell_length_b 14.000(3) _cell_length_c 17.577(4) _cell_angle_alpha 84.07(3) _cell_angle_beta 89.09(4) _cell_angle_gamma 84.48(3) _cell_volume 2270.8(8) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 8588 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 1.974 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.7177 _exptl_absorpt_correction_T_max 0.8270 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14053 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14053 _reflns_number_gt 9733 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ISOR was applied to all non-hydrogen atoms to allow their Uij components approximate to isotropic behavior (restraints: 843). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+3.9789P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(3) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.511(15) _refine_ls_number_reflns 14053 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 843 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1853 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.52794(3) 0.62376(3) 0.73322(2) 0.03110(16) Uani 1 1 d U . . Er2 Er 1.14506(3) 0.46363(3) 0.28180(2) 0.03067(17) Uani 1 1 d U . . S1 S 0.3921(3) 0.4856(2) 0.57873(15) 0.0589(9) Uani 1 1 d DU . . S2 S 0.9315(4) 0.0346(3) -0.02281(19) 0.0504(8) Uani 1 1 d DU . . F1 F 0.3694(8) 0.3505(5) 0.6872(3) 0.106(4) Uani 1 1 d DU . . F2 F 0.2913(8) 0.3214(4) 0.5785(3) 0.102(3) Uani 1 1 d DU . . F3 F 0.1711(6) 0.4230(6) 0.6464(5) 0.129(5) Uani 1 1 d DU . . F4 F 0.8039(9) 0.0903(6) 0.0999(4) 0.0644(18) Uani 1 1 d U . . F5 F 0.6601(8) 0.1120(5) -0.0118(4) 0.0582(17) Uani 1 1 d U . . F6 F 0.7149(11) -0.0228(7) 0.0566(5) 0.088(2) Uani 1 1 d U . . O1 O 0.5094(7) 0.7805(5) 0.7739(4) 0.028(2) Uani 1 1 d U . . H1A H 0.4753 0.8047 0.7328 0.033 Uiso 1 1 calc R . . O2 O 1.2173(8) 1.0092(5) 0.5939(4) 0.034(2) Uani 1 1 d U . . H2D H 1.1402 0.9952 0.6129 0.041 Uiso 1 1 calc R . . O3 O 0.4323(6) 0.5350(4) 0.6406(3) 0.0272(19) Uani 1 1 d DU . . O4 O 0.5156(6) 0.4362(6) 0.5419(5) 0.100(6) Uani 1 1 d DU . . O5 O 0.2939(7) 0.5388(5) 0.5246(4) 0.096(4) Uani 1 1 d DU . . O6 O 0.9697(10) 0.1299(7) -0.0384(6) 0.0582(17) Uani 1 1 d U . . O7 O 0.8797(14) -0.0137(10) -0.0808(7) 0.088(2) Uani 1 1 d U . . O8 O 1.0022(12) -0.0341(8) 0.0237(6) 0.0644(18) Uani 1 1 d U . . O9 O 1.2441(8) 0.5596(5) 0.3792(4) 0.032(2) Uani 1 1 d U . . H9C H 1.3254 0.5316 0.3833 0.038 Uiso 1 1 calc R . . O1B O 0.4325(7) 0.5113(5) 0.8241(4) 0.0246(17) Uani 1 1 d U . . O2B O 0.7069(8) 0.6810(5) 0.6596(4) 0.030(2) Uani 1 1 d U . . O1C O 0.6950(7) 0.4887(5) 0.7176(3) 0.0268(18) Uani 1 1 d U . . H1CA H 0.7592 0.5219 0.7269 0.020 Uiso 1 1 calc R . . O2C O 0.9836(8) 0.5974(6) 0.2895(4) 0.023(2) Uani 1 1 d U . . H2CA H 0.9870 0.5834 0.3359 0.027 Uiso 1 1 calc R . . O1D O 0.9572(7) 0.4111(5) 0.3590(4) 0.0274(17) Uani 1 1 d U . . O2D O 1.2510(8) 0.5633(6) 0.1935(4) 0.026(2) Uani 1 1 d U . . O1E O 1.0205(7) 0.4697(5) 0.1727(4) 0.029(2) Uani 1 1 d U . . H1EA H 1.0950 0.4805 0.1493 0.035 Uiso 1 1 calc R . . O2E O 1.6524(8) 0.6106(6) -0.1509(4) 0.026(2) Uani 1 1 d U . . H2EA H 1.5903 0.5881 -0.1228 0.038 Uiso 1 1 calc R . . O1F O 0.4636(10) 0.0811(6) 0.4198(5) 0.038(2) Uani 1 1 d U . . H1FA H 0.5323 0.1025 0.3964 0.057 Uiso 1 1 calc R . . O2F O 1.1688(8) 0.3062(6) 0.2404(4) 0.028(2) Uani 1 1 d U . . H2FA H 1.0833 0.2991 0.2481 0.033 Uiso 1 1 calc R . . N1 N 0.6655(9) 0.9235(7) 0.7464(5) 0.028(2) Uani 1 1 d U . . N2 N 1.0368(10) 0.9770(6) 0.7065(5) 0.029(3) Uani 1 1 d U . . N1B N 0.2609(10) 0.6590(7) 0.7387(5) 0.035(3) Uani 1 1 d U . . N2B N 0.4254(9) 0.7465(6) 0.6225(5) 0.0257(19) Uani 1 1 d U . . N1C N 0.8463(9) 0.4818(6) 0.6029(5) 0.027(2) Uani 1 1 d U . . N2C N 0.8241(10) 0.6116(6) 0.4108(5) 0.017(2) Uani 1 1 d U . . N1D N 1.2388(10) 0.3399(7) 0.3968(5) 0.025(2) Uani 1 1 d U . . N2D N 1.4099(10) 0.4205(5) 0.2780(5) 0.028(3) Uani 1 1 d DU . . N1E N 1.1559(7) 0.5304(6) 0.0455(5) 0.029(2) Uani 1 1 d DU . . N2E N 1.5181(9) 0.5632(7) -0.0262(5) 0.019(2) Uani 1 1 d U . . N1F N 0.6303(10) 0.1083(7) 0.3109(6) 0.028(3) Uani 1 1 d U . . N2F N 0.9940(11) 0.1686(7) 0.2671(5) 0.029(3) Uani 1 1 d U . . C1 C 0.3450(6) 0.7929(4) 0.8746(3) 0.039(3) Uani 1 1 d GU . . H1B H 0.3077 0.7371 0.8624 0.047 Uiso 1 1 calc R . . C2 C 0.2913(7) 0.8381(5) 0.9373(4) 0.047(4) Uani 1 1 d GU . . H2B H 0.2180 0.8126 0.9671 0.057 Uiso 1 1 calc R . . C3 C 0.3470(9) 0.9214(5) 0.9555(4) 0.035(2) Uani 1 1 d GU . . H3A H 0.3111 0.9516 0.9974 0.042 Uiso 1 1 calc R . . C4 C 0.4566(9) 0.9595(5) 0.9110(5) 0.055(4) Uani 1 1 d GU . . H4A H 0.4939 1.0152 0.9231 0.066 Uiso 1 1 calc R . . C5 C 0.5103(7) 0.9143(5) 0.8483(4) 0.019(2) Uani 1 1 d GU . . C6 C 0.4546(7) 0.8310(4) 0.8301(3) 0.026(3) Uani 1 1 d GU . . C7 C 0.6104(12) 0.9474(8) 0.8129(6) 0.033(3) Uani 1 1 d U . . H7B H 0.6536 0.9950 0.8349 0.039 Uiso 1 1 calc R . . C8 C 0.7851(8) 0.9661(8) 0.7040(6) 0.026(3) Uani 1 1 d DU . . H8B H 0.7736 1.0357 0.7037 0.032 Uiso 1 1 calc R . . H8A H 0.7864 0.9504 0.6515 0.032 Uiso 1 1 calc R . . C9 C 0.9259(9) 0.9244(9) 0.7441(6) 0.042(3) Uani 1 1 d DU . . H9A H 0.9210 0.9334 0.7981 0.050 Uiso 1 1 calc R . . H9B H 0.9445 0.8560 0.7388 0.050 Uiso 1 1 calc R . . C10 C 1.1211(15) 1.0160(10) 0.7476(8) 0.052(4) Uani 1 1 d U . . H10A H 1.1072 1.0126 0.8002 0.062 Uiso 1 1 calc R . . C11 C 1.2361(7) 1.0645(5) 0.7134(4) 0.042(3) Uani 1 1 d GU . . C12 C 1.3144(9) 1.1153(7) 0.7596(4) 0.063(4) Uani 1 1 d GDU . . H12A H 1.2846 1.1222 0.8096 0.075 Uiso 1 1 calc R . . C13 C 1.4373(10) 1.1557(8) 0.7309(6) 0.051(5) Uani 1 1 d GDU . . H13A H 1.4896 1.1896 0.7618 0.061 Uiso 1 1 calc R . . C14 C 1.4818(9) 1.1453(8) 0.6561(6) 0.054(4) Uani 1 1 d GDU . . H14A H 1.5640 1.1724 0.6370 0.065 Uiso 1 1 calc R . . C15 C 1.4036(9) 1.0946(8) 0.6100(5) 0.052(4) Uani 1 1 d GU . . H15A H 1.4334 1.0877 0.5599 0.063 Uiso 1 1 calc R . . C16 C 1.2807(8) 1.0542(6) 0.6386(4) 0.031(3) Uani 1 1 d GU . . C1B C 0.3209(6) 0.3780(4) 0.8672(3) 0.032(3) Uani 1 1 d GU . . H1BA H 0.4072 0.3502 0.8890 0.039 Uiso 1 1 calc R . . C2B C 0.1995(7) 0.3272(4) 0.8727(4) 0.036(3) Uani 1 1 d GDU . . H2BA H 0.2046 0.2654 0.8982 0.043 Uiso 1 1 calc R . . C3B C 0.0705(6) 0.3687(5) 0.8400(4) 0.044(3) Uani 1 1 d GDU . . H3BA H -0.0107 0.3347 0.8437 0.053 Uiso 1 1 calc R . . C4B C 0.0628(6) 0.4611(6) 0.8018(4) 0.040(3) Uani 1 1 d GU . . H4BA H -0.0235 0.4889 0.7800 0.048 Uiso 1 1 calc R . . C5B C 0.1842(7) 0.5119(5) 0.7963(4) 0.029(3) Uani 1 1 d GU . . C6B C 0.3132(6) 0.4703(4) 0.8290(3) 0.027(3) Uani 1 1 d GU . . C7B C 0.1693(12) 0.6028(7) 0.7586(6) 0.026(2) Uani 1 1 d U . . H7BA H 0.0750 0.6262 0.7459 0.031 Uiso 1 1 calc R . . C8B C 0.2146(10) 0.7544(8) 0.6954(4) 0.033(3) Uani 1 1 d DU . . H8BA H 0.2484 0.8059 0.7212 0.040 Uiso 1 1 calc R . . H8BB H 0.1102 0.7639 0.6933 0.040 Uiso 1 1 calc R . . C9B C 0.2769(11) 0.7575(9) 0.6137(4) 0.033(3) Uani 1 1 d DU . . H9BA H 0.2453 0.7057 0.5875 0.040 Uiso 1 1 calc R . . H9BB H 0.2465 0.8186 0.5846 0.040 Uiso 1 1 calc R . . C10B C 0.4945(12) 0.8052(7) 0.5810(6) 0.026(3) Uani 1 1 d U . . H10B H 0.4354 0.8514 0.5514 0.031 Uiso 1 1 calc R . . C11B C 0.6399(5) 0.8154(4) 0.5702(3) 0.027(2) Uani 1 1 d GU . . C12B C 0.6835(6) 0.8881(4) 0.5175(4) 0.027(3) Uani 1 1 d GU . . H12B H 0.6152 0.9326 0.4924 0.033 Uiso 1 1 calc R . . C13B C 0.8294(7) 0.8941(5) 0.5023(4) 0.044(3) Uani 1 1 d GU . . H13B H 0.8586 0.9427 0.4670 0.053 Uiso 1 1 calc R . . C14B C 0.9315(6) 0.8275(6) 0.5397(4) 0.036(3) Uani 1 1 d GU . . H14B H 1.0291 0.8316 0.5295 0.043 Uiso 1 1 calc R . . C15B C 0.8879(6) 0.7549(5) 0.5925(4) 0.026(3) Uani 1 1 d GU . . H15D H 0.9562 0.7103 0.6175 0.031 Uiso 1 1 calc R . . C16B C 0.7420(6) 0.7488(4) 0.6077(3) 0.020(3) Uani 1 1 d GU . . C1C C 0.6884(5) 0.3485(4) 0.8133(2) 0.0253(19) Uani 1 1 d GU . . H1CB H 0.6282 0.3827 0.8457 0.030 Uiso 1 1 calc R . . C2C C 0.7329(6) 0.2517(4) 0.8336(3) 0.0358(18) Uani 1 1 d GU . . H2CB H 0.7023 0.2212 0.8797 0.043 Uiso 1 1 calc R . . C3C C 0.8229(7) 0.2006(4) 0.7851(4) 0.024(3) Uani 1 1 d GU . . H3CA H 0.8527 0.1359 0.7988 0.029 Uiso 1 1 calc R . . C4C C 0.8686(7) 0.2463(5) 0.7162(3) 0.028(3) Uani 1 1 d GU . . H4CA H 0.9289 0.2121 0.6838 0.033 Uiso 1 1 calc R . . C5C C 0.8242(7) 0.3430(5) 0.6958(3) 0.020(2) Uani 1 1 d GU . . C6C C 0.7341(6) 0.3942(4) 0.7444(3) 0.025(3) Uani 1 1 d GU . . C7C C 0.8672(11) 0.3810(8) 0.6297(6) 0.029(3) Uani 1 1 d U . . H7CA H 0.9152 0.3398 0.5974 0.035 Uiso 1 1 calc R . . C8C C 0.8980(12) 0.5210(8) 0.5299(6) 0.026(3) Uani 1 1 d U . . H8CA H 0.9518 0.4703 0.5046 0.032 Uiso 1 1 calc R . . H8CB H 0.9621 0.5700 0.5370 0.032 Uiso 1 1 calc R . . C9C C 0.7736(12) 0.5642(9) 0.4815(6) 0.021(3) Uani 1 1 d U . . H9CA H 0.7144 0.5140 0.4707 0.025 Uiso 1 1 calc R . . H9CB H 0.7148 0.6105 0.5090 0.025 Uiso 1 1 calc R . . C10C C 0.7948(10) 0.6928(7) 0.3934(4) 0.014(2) Uani 1 1 d DU . . H10F H 0.7309 0.7276 0.4238 0.017 Uiso 1 1 calc R . . C11C C 0.8577(6) 0.7442(4) 0.3223(3) 0.028(3) Uani 1 1 d GDU . . C12C C 0.8167(7) 0.8403(4) 0.2976(3) 0.024(3) Uani 1 1 d GU . . H12C H 0.7614 0.8788 0.3292 0.029 Uiso 1 1 calc R . . C13C C 0.8583(9) 0.8789(4) 0.2255(4) 0.031(2) Uani 1 1 d GDU . . H13C H 0.8309 0.9432 0.2089 0.037 Uiso 1 1 calc R . . C14C C 0.9409(8) 0.8214(6) 0.1781(3) 0.0272(17) Uani 1 1 d GDU . . H14C H 0.9688 0.8472 0.1299 0.033 Uiso 1 1 calc R . . C15C C 0.9819(7) 0.7253(5) 0.2029(3) 0.044(2) Uani 1 1 d GDU . . H15F H 1.0372 0.6868 0.1712 0.053 Uiso 1 1 calc R . . C16C C 0.9403(7) 0.6866(4) 0.2750(3) 0.016(3) Uani 1 1 d GU . . C1D C 0.7840(6) 0.3280(4) 0.4271(3) 0.024(3) Uani 1 1 d GU . . H1DA H 0.7126 0.3728 0.4050 0.029 Uiso 1 1 calc R . . C2D C 0.7466(6) 0.2517(5) 0.4782(4) 0.022(3) Uani 1 1 d GU . . H2DA H 0.6503 0.2455 0.4903 0.026 Uiso 1 1 calc R . . C3D C 0.8533(8) 0.1847(5) 0.5113(4) 0.024(3) Uani 1 1 d GU . . H3DA H 0.8283 0.1337 0.5455 0.029 Uiso 1 1 calc R . . C4D C 0.9974(7) 0.1940(5) 0.4932(4) 0.036(3) Uani 1 1 d GU . . H4DA H 1.0688 0.1491 0.5153 0.043 Uiso 1 1 calc R . . C5D C 1.0347(5) 0.2702(5) 0.4420(4) 0.017(2) Uani 1 1 d GU . . C6D C 0.9280(6) 0.3372(4) 0.4090(3) 0.020(3) Uani 1 1 d GU . . C7D C 1.1844(13) 0.2710(9) 0.4388(7) 0.030(3) Uani 1 1 d U . . H7DA H 1.2437 0.2229 0.4665 0.036 Uiso 1 1 calc R . . C8D C 1.3949(11) 0.3268(9) 0.3957(6) 0.029(3) Uani 1 1 d U . . H8DA H 1.4262 0.2654 0.4240 0.034 Uiso 1 1 calc R . . H8DB H 1.4314 0.3771 0.4219 0.034 Uiso 1 1 calc R . . C9D C 1.4581(13) 0.3291(7) 0.3201(6) 0.040(3) Uani 1 1 d DU . . H9DA H 1.5624 0.3220 0.3236 0.048 Uiso 1 1 calc R . . H9DB H 1.4285 0.2765 0.2941 0.048 Uiso 1 1 calc R . . C10D C 1.5062(14) 0.4752(5) 0.2593(6) 0.034(3) Uani 1 1 d DU . . H10C H 1.6004 0.4508 0.2711 0.041 Uiso 1 1 calc R . . C11D C 1.4856(7) 0.5779(4) 0.2189(3) 0.036(3) Uani 1 1 d GDU . . C12D C 1.6072(7) 0.6284(5) 0.2135(4) 0.035(3) Uani 1 1 d GU . . H12D H 1.6930 0.6007 0.2361 0.042 Uiso 1 1 calc R . . C13D C 1.6007(8) 0.7203(5) 0.1745(5) 0.036(3) Uani 1 1 d GU . . H13D H 1.6821 0.7541 0.1710 0.043 Uiso 1 1 calc R . . C14D C 1.4725(9) 0.7616(4) 0.1409(4) 0.041(3) Uani 1 1 d GU . . H14D H 1.4681 0.8231 0.1148 0.050 Uiso 1 1 calc R . . C15D C 1.3508(8) 0.7111(5) 0.1462(4) 0.035(3) Uani 1 1 d GU . . H15G H 1.2650 0.7388 0.1237 0.042 Uiso 1 1 calc R . . C16D C 1.3574(6) 0.6192(5) 0.1852(4) 0.029(3) Uani 1 1 d GU . . C1E C 0.8204(6) 0.3905(4) 0.1649(3) 0.024(3) Uani 1 1 d GU . . H1EB H 0.8100 0.3886 0.2177 0.029 Uiso 1 1 calc R . . C2E C 0.7226(7) 0.3493(5) 0.1224(3) 0.045(3) Uani 1 1 d GU . . H2EB H 0.6467 0.3198 0.1469 0.054 Uiso 1 1 calc R . . C3E C 0.7382(8) 0.3521(6) 0.0435(3) 0.049(4) Uani 1 1 d GU . . H3EA H 0.6728 0.3245 0.0151 0.059 Uiso 1 1 calc R . . C4E C 0.8517(8) 0.3961(6) 0.0070(3) 0.030(2) Uani 1 1 d GU . . H4EA H 0.8621 0.3980 -0.0459 0.036 Uiso 1 1 calc R . . C5E C 0.9495(7) 0.4373(6) 0.0494(3) 0.017(2) Uani 1 1 d GU . . C6E C 0.9338(6) 0.4345(5) 0.1284(3) 0.025(3) Uani 1 1 d GU . . C7E C 1.0546(11) 0.4875(8) 0.0118(6) 0.024(3) Uani 1 1 d U . . H7EA H 1.0554 0.4919 -0.0414 0.029 Uiso 1 1 calc R . . C8E C 1.2659(8) 0.5728(7) -0.0005(5) 0.024(3) Uani 1 1 d DU . . H8EA H 1.2741 0.6378 0.0125 0.028 Uiso 1 1 calc R . . H8EB H 1.2408 0.5765 -0.0541 0.028 Uiso 1 1 calc R . . C9E C 1.4039(12) 0.5141(10) 0.0130(7) 0.039(3) Uani 1 1 d U . . H9EA H 1.4233 0.5037 0.0675 0.046 Uiso 1 1 calc R . . H9EB H 1.3994 0.4517 -0.0058 0.046 Uiso 1 1 calc R . . C10E C 1.6082(13) 0.6040(9) 0.0050(7) 0.027(3) Uani 1 1 d U . . H10D H 1.6010 0.6074 0.0575 0.032 Uiso 1 1 calc R . . C11E C 1.7174(6) 0.6443(5) -0.0336(3) 0.034(3) Uani 1 1 d GU . . C12E C 1.8126(7) 0.6839(5) 0.0116(3) 0.035(3) Uani 1 1 d GU . . H12F H 1.8018 0.6777 0.0645 0.042 Uiso 1 1 calc R . . C13E C 1.9239(7) 0.7327(6) -0.0223(4) 0.024(3) Uani 1 1 d GU . . H13E H 1.9876 0.7592 0.0079 0.029 Uiso 1 1 calc R . . C14E C 1.9401(7) 0.7420(6) -0.1014(4) 0.019(3) Uani 1 1 d GU . . H14F H 2.0146 0.7746 -0.1241 0.023 Uiso 1 1 calc R . . C15E C 1.8450(7) 0.7024(6) -0.1466(3) 0.029(3) Uani 1 1 d GU . . H15H H 1.8558 0.7086 -0.1995 0.035 Uiso 1 1 calc R . . C16E C 1.7336(7) 0.6536(5) -0.1127(3) 0.027(2) Uani 1 1 d GU . . C1F C 0.2646(7) -0.0046(5) 0.4010(3) 0.044(4) Uani 1 1 d GU . . H1FC H 0.2325 0.0038 0.4504 0.053 Uiso 1 1 calc R . . C2F C 0.1886(7) -0.0569(6) 0.3550(4) 0.0358(18) Uani 1 1 d GU . . H2FB H 0.1057 -0.0834 0.3736 0.043 Uiso 1 1 calc R . . C3F C 0.2366(8) -0.0695(6) 0.2811(4) 0.0272(17) Uani 1 1 d GU . . H3FA H 0.1858 -0.1045 0.2503 0.033 Uiso 1 1 calc R . . C4F C 0.3606(8) -0.0299(6) 0.2532(3) 0.044(2) Uani 1 1 d GU . . H4FA H 0.3927 -0.0384 0.2038 0.053 Uiso 1 1 calc R . . C5F C 0.4365(7) 0.0224(6) 0.2992(4) 0.028(3) Uani 1 1 d GU . . C6F C 0.3885(7) 0.0350(6) 0.3731(4) 0.040(4) Uani 1 1 d GU . . C7F C 0.5592(12) 0.0640(8) 0.2708(6) 0.018(3) Uani 1 1 d U . . H7FA H 0.5877 0.0580 0.2205 0.022 Uiso 1 1 calc R . . C8F C 0.7505(11) 0.1536(8) 0.2709(6) 0.024(3) Uani 1 1 d U . . H8FA H 0.7334 0.2232 0.2702 0.029 Uiso 1 1 calc R . . H8FB H 0.7547 0.1381 0.2183 0.029 Uiso 1 1 calc R . . C9F C 0.8869(12) 0.1210(10) 0.3076(7) 0.035(3) Uani 1 1 d U . . H9FA H 0.8839 0.1358 0.3603 0.042 Uiso 1 1 calc R . . H9FB H 0.9069 0.0518 0.3071 0.042 Uiso 1 1 calc R . . C10F C 1.0515(13) 0.1297(10) 0.2133(7) 0.038(3) Uani 1 1 d U . . H10E H 1.0292 0.0689 0.2034 0.046 Uiso 1 1 calc R . . C11F C 1.1578(7) 0.1814(5) 0.1641(4) 0.044(3) Uani 1 1 d GDU . . C12F C 1.2148(8) 0.1328(5) 0.1037(4) 0.036(3) Uani 1 1 d GU . . H12G H 1.1785 0.0761 0.0930 0.043 Uiso 1 1 calc R . . C13F C 1.3258(9) 0.1691(6) 0.0593(4) 0.057(4) Uani 1 1 d GU . . H13F H 1.3639 0.1366 0.0189 0.069 Uiso 1 1 calc R . . C14F C 1.3800(8) 0.2539(6) 0.0753(5) 0.037(3) Uani 1 1 d GU . . H14G H 1.4543 0.2782 0.0456 0.044 Uiso 1 1 calc R . . C15F C 1.3230(8) 0.3024(5) 0.1357(5) 0.032(3) Uani 1 1 d GU . . H15I H 1.3592 0.3592 0.1464 0.038 Uiso 1 1 calc R . . C16F C 1.2119(8) 0.2662(5) 0.1801(4) 0.028(3) Uani 1 1 d GDU . . C17 C 0.2995(6) 0.3895(3) 0.6236(3) 0.0689(9) Uani 1 1 d DU . . C18 C 0.7599(9) 0.0480(11) 0.0299(7) 0.0504(8) Uani 1 1 d DU . . C19 C 1.2532(12) 0.6691(8) 0.3742(6) 0.041(3) Uani 1 1 d U . . H19A H 1.2929 0.6853 0.4208 0.062 Uiso 1 1 calc R . . H19B H 1.1584 0.7020 0.3669 0.062 Uiso 1 1 calc R . . H19C H 1.3139 0.6885 0.3319 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0246(3) 0.0408(3) 0.0303(3) -0.0144(2) -0.0005(2) -0.0038(2) Er2 0.0243(3) 0.0406(3) 0.0291(3) -0.0130(3) -0.0003(2) -0.0031(3) S1 0.0848(19) 0.0673(18) 0.0342(15) -0.0161(14) -0.0063(15) -0.0430(16) S2 0.0595(16) 0.0465(14) 0.0454(14) -0.0057(12) -0.0055(13) -0.0046(13) F1 0.127(8) 0.108(6) 0.093(6) -0.037(5) 0.009(6) -0.038(6) F2 0.148(6) 0.087(5) 0.081(5) -0.022(4) -0.005(4) -0.049(4) F3 0.147(8) 0.141(8) 0.118(8) -0.067(6) -0.024(6) -0.080(6) F4 0.080(3) 0.064(3) 0.046(3) -0.013(3) -0.002(3) 0.017(3) F5 0.055(3) 0.054(3) 0.060(3) 0.024(3) -0.001(3) -0.008(3) F6 0.099(4) 0.102(4) 0.061(3) -0.011(3) -0.005(3) 0.009(3) O1 0.024(3) 0.025(3) 0.036(4) -0.016(3) -0.002(3) -0.002(3) O2 0.034(4) 0.037(4) 0.030(4) -0.002(3) 0.010(3) -0.006(3) O3 0.029(3) 0.030(4) 0.027(3) -0.018(3) -0.011(3) -0.006(3) O4 0.109(8) 0.096(8) 0.107(8) -0.082(6) 0.019(7) -0.027(7) O5 0.106(7) 0.107(7) 0.086(6) -0.047(5) -0.057(5) -0.030(6) O6 0.055(3) 0.054(3) 0.060(3) 0.024(3) -0.001(3) -0.008(3) O7 0.099(4) 0.102(4) 0.061(3) -0.011(3) -0.005(3) 0.009(3) O8 0.080(3) 0.064(3) 0.046(3) -0.013(3) -0.002(3) 0.017(3) O9 0.024(4) 0.035(4) 0.038(4) -0.013(3) -0.005(3) 0.001(3) O1B 0.017(3) 0.034(3) 0.024(3) -0.007(2) -0.003(2) -0.008(2) O2B 0.021(3) 0.040(4) 0.028(3) -0.010(3) 0.001(3) 0.002(3) O1C 0.025(3) 0.031(3) 0.024(3) -0.005(3) 0.006(3) 0.004(3) O2C 0.023(4) 0.030(4) 0.013(3) 0.000(3) 0.002(3) -0.001(3) O1D 0.024(3) 0.030(3) 0.027(3) -0.002(2) -0.005(2) 0.006(2) O2D 0.016(3) 0.036(4) 0.028(4) -0.008(3) 0.002(3) -0.003(3) O1E 0.020(3) 0.044(4) 0.026(3) -0.019(3) -0.009(3) -0.007(3) O2E 0.016(3) 0.040(4) 0.023(4) -0.006(3) 0.013(3) -0.014(3) O1F 0.040(4) 0.038(4) 0.037(4) -0.008(4) 0.005(4) -0.007(4) O2F 0.022(4) 0.037(4) 0.027(4) -0.014(3) 0.005(3) -0.006(3) N1 0.022(4) 0.035(4) 0.027(4) -0.001(4) 0.006(3) -0.005(4) N2 0.026(4) 0.026(4) 0.035(4) -0.002(4) 0.001(4) 0.001(4) N1B 0.031(4) 0.036(4) 0.040(4) -0.018(4) -0.001(4) -0.003(4) N2B 0.023(3) 0.025(3) 0.029(3) -0.010(2) -0.001(2) 0.003(2) N1C 0.025(4) 0.030(4) 0.025(4) 0.004(4) -0.002(4) -0.006(4) N2C 0.025(4) 0.015(4) 0.010(4) 0.000(3) 0.004(3) 0.008(4) N1D 0.018(3) 0.026(3) 0.032(3) -0.008(3) -0.008(3) 0.002(3) N2D 0.019(4) 0.036(5) 0.033(4) -0.029(4) 0.001(4) 0.002(4) N1E 0.028(3) 0.026(4) 0.036(4) -0.008(4) 0.006(3) -0.018(3) N2E 0.016(3) 0.028(3) 0.015(3) -0.006(3) -0.001(2) -0.006(3) N1F 0.019(4) 0.031(5) 0.033(5) 0.002(4) 0.003(4) 0.002(4) N2F 0.029(5) 0.036(5) 0.024(4) -0.020(4) 0.001(4) -0.005(4) C1 0.037(5) 0.040(5) 0.046(5) -0.020(4) -0.002(4) -0.011(4) C2 0.045(6) 0.049(6) 0.050(6) -0.014(5) 0.016(5) -0.008(5) C3 0.036(3) 0.037(4) 0.035(3) -0.010(3) 0.006(3) -0.005(3) C4 0.058(6) 0.048(6) 0.065(6) -0.034(5) 0.012(5) -0.010(5) C5 0.020(3) 0.019(3) 0.018(3) -0.006(3) 0.004(3) -0.002(3) C6 0.023(5) 0.036(5) 0.022(4) -0.011(4) 0.003(4) -0.001(4) C7 0.032(5) 0.030(5) 0.042(5) -0.023(4) -0.005(4) -0.014(4) C8 0.023(5) 0.027(5) 0.028(5) 0.001(4) 0.004(4) -0.002(4) C9 0.040(5) 0.047(6) 0.038(5) -0.004(5) 0.013(5) -0.002(5) C10 0.054(6) 0.055(6) 0.045(6) 0.000(5) -0.001(5) 0.004(5) C11 0.035(5) 0.043(6) 0.049(6) -0.003(5) -0.004(5) -0.001(5) C12 0.053(6) 0.075(7) 0.062(6) -0.018(5) -0.011(5) -0.006(5) C13 0.042(7) 0.050(8) 0.064(8) -0.012(6) -0.010(6) -0.022(6) C14 0.039(6) 0.057(7) 0.067(7) -0.007(6) 0.003(6) -0.010(5) C15 0.045(6) 0.053(6) 0.056(6) -0.001(5) 0.004(5) 0.005(5) C16 0.022(5) 0.027(5) 0.042(5) -0.003(4) -0.004(4) 0.002(4) C1B 0.023(5) 0.044(5) 0.032(5) -0.013(4) 0.005(4) -0.006(4) C2B 0.044(6) 0.042(5) 0.024(5) -0.015(4) 0.011(4) -0.005(5) C3B 0.034(5) 0.065(6) 0.041(5) -0.033(5) 0.006(4) -0.010(5) C4B 0.033(5) 0.059(6) 0.033(5) -0.018(5) 0.007(4) -0.011(5) C5B 0.018(4) 0.046(5) 0.026(5) -0.017(4) 0.007(4) -0.012(4) C6B 0.024(5) 0.036(5) 0.026(5) -0.015(4) 0.005(4) -0.014(4) C7B 0.022(3) 0.032(3) 0.026(3) -0.010(3) -0.002(3) -0.004(3) C8B 0.013(4) 0.036(5) 0.052(5) -0.018(4) -0.010(4) 0.004(4) C9B 0.019(5) 0.033(5) 0.047(5) -0.008(4) -0.010(4) 0.003(4) C10B 0.035(5) 0.017(5) 0.025(4) -0.012(4) -0.014(4) 0.017(4) C11B 0.028(3) 0.026(3) 0.027(3) -0.010(3) -0.003(3) 0.000(3) C12B 0.033(5) 0.023(5) 0.024(4) -0.008(4) -0.012(4) 0.018(4) C13B 0.054(6) 0.043(5) 0.039(5) -0.004(5) 0.001(5) -0.022(5) C14B 0.041(5) 0.031(5) 0.035(5) -0.003(4) 0.002(4) -0.008(4) C15B 0.028(5) 0.026(5) 0.023(5) 0.003(4) 0.001(4) -0.005(4) C16B 0.026(5) 0.016(4) 0.019(4) -0.004(4) -0.003(4) -0.003(4) C1C 0.027(3) 0.029(3) 0.022(3) -0.005(2) 0.008(2) -0.013(2) C2C 0.027(3) 0.047(3) 0.031(3) -0.003(2) -0.003(2) 0.006(2) C3C 0.026(4) 0.021(4) 0.027(4) -0.003(4) -0.015(4) -0.005(4) C4C 0.032(5) 0.025(5) 0.026(5) 0.003(4) -0.007(4) -0.011(4) C5C 0.017(4) 0.027(4) 0.018(4) -0.004(3) -0.005(3) -0.003(3) C6C 0.016(4) 0.036(5) 0.023(4) -0.008(4) -0.002(4) -0.003(4) C7C 0.030(5) 0.030(5) 0.026(5) 0.003(4) -0.007(4) -0.006(4) C8C 0.028(5) 0.028(5) 0.023(5) -0.006(4) 0.003(4) 0.003(4) C9C 0.022(5) 0.027(5) 0.012(4) 0.002(4) -0.001(4) 0.002(4) C10C 0.013(3) 0.017(3) 0.013(3) -0.004(3) 0.002(3) -0.004(3) C11C 0.029(5) 0.029(5) 0.027(5) -0.004(4) -0.002(4) -0.003(4) C12C 0.028(5) 0.026(5) 0.022(5) -0.012(4) 0.002(4) -0.013(4) C13C 0.030(4) 0.029(4) 0.032(4) 0.005(3) -0.009(3) -0.008(3) C14C 0.020(3) 0.039(3) 0.021(3) -0.005(2) -0.005(2) 0.010(2) C15C 0.036(4) 0.059(4) 0.041(4) -0.013(3) 0.003(3) -0.014(3) C16C 0.010(4) 0.023(5) 0.015(4) 0.001(4) -0.010(4) -0.002(4) C1D 0.024(5) 0.029(5) 0.021(5) -0.010(4) -0.011(4) -0.001(4) C2D 0.021(5) 0.026(5) 0.017(5) -0.004(4) -0.006(4) 0.002(4) C3D 0.037(5) 0.014(5) 0.021(5) 0.001(4) -0.002(4) 0.000(4) C4D 0.038(6) 0.036(6) 0.037(5) -0.013(5) -0.009(5) -0.003(5) C5D 0.022(5) 0.008(4) 0.020(4) -0.001(4) -0.007(4) 0.008(4) C6D 0.015(5) 0.025(5) 0.020(5) -0.003(4) 0.001(4) -0.003(4) C7D 0.022(5) 0.029(5) 0.036(5) 0.002(4) -0.008(4) 0.000(4) C8D 0.020(5) 0.029(5) 0.037(5) -0.009(4) -0.021(4) 0.005(4) C9D 0.028(6) 0.045(6) 0.052(6) -0.023(5) -0.002(5) -0.003(5) C10D 0.023(5) 0.050(6) 0.032(5) -0.024(4) -0.002(4) 0.003(4) C11D 0.028(5) 0.056(6) 0.027(5) -0.019(5) 0.002(4) -0.006(5) C12D 0.023(5) 0.057(6) 0.031(5) -0.019(5) 0.000(4) -0.020(5) C13D 0.020(5) 0.058(6) 0.037(5) -0.027(5) 0.005(4) -0.020(4) C14D 0.043(6) 0.046(6) 0.042(6) -0.016(5) 0.010(5) -0.025(5) C15D 0.030(5) 0.043(6) 0.037(5) -0.021(5) 0.007(4) -0.015(5) C16D 0.018(5) 0.049(6) 0.019(5) -0.013(4) 0.004(4) 0.001(5) C1E 0.019(4) 0.031(5) 0.024(4) -0.005(4) -0.005(4) -0.005(4) C2E 0.038(5) 0.051(6) 0.046(6) -0.011(5) -0.002(5) -0.007(5) C3E 0.051(6) 0.058(6) 0.042(6) -0.014(5) 0.007(5) -0.011(5) C4E 0.028(3) 0.035(3) 0.030(3) -0.004(3) 0.003(3) -0.013(3) C5E 0.012(4) 0.027(5) 0.015(4) -0.014(4) -0.002(3) 0.000(4) C6E 0.017(4) 0.026(5) 0.032(5) -0.008(4) 0.001(4) -0.002(4) C7E 0.025(5) 0.037(5) 0.009(4) -0.002(4) 0.001(4) 0.000(4) C8E 0.024(4) 0.029(5) 0.021(4) -0.011(4) -0.005(4) -0.007(4) C9E 0.039(6) 0.051(6) 0.029(5) -0.009(5) 0.007(5) -0.016(5) C10E 0.027(5) 0.036(5) 0.018(5) -0.009(4) 0.007(4) -0.003(4) C11E 0.029(5) 0.042(6) 0.034(5) -0.005(5) -0.001(5) -0.014(5) C12E 0.032(5) 0.038(5) 0.037(4) -0.009(4) -0.010(4) 0.000(4) C13E 0.028(4) 0.022(5) 0.027(4) -0.012(4) -0.008(4) -0.014(4) C14E 0.018(4) 0.022(5) 0.019(4) 0.000(4) 0.005(4) -0.013(4) C15E 0.029(5) 0.040(6) 0.018(5) -0.008(4) 0.013(4) 0.000(5) C16E 0.024(3) 0.027(3) 0.030(3) -0.004(3) -0.001(3) -0.002(3) C1F 0.035(6) 0.042(6) 0.051(6) 0.001(5) 0.007(5) 0.005(5) C2F 0.027(3) 0.047(3) 0.031(3) -0.003(2) -0.003(2) 0.006(2) C3F 0.020(3) 0.039(3) 0.021(3) -0.005(2) -0.005(2) 0.010(2) C4F 0.036(4) 0.059(4) 0.041(4) -0.013(3) 0.003(3) -0.014(3) C5F 0.022(5) 0.028(5) 0.032(5) 0.000(4) -0.003(4) 0.006(4) C6F 0.024(5) 0.041(6) 0.051(6) -0.002(5) -0.008(5) 0.009(5) C7F 0.021(5) 0.022(5) 0.011(4) -0.006(4) 0.004(4) 0.007(4) C8F 0.032(5) 0.015(5) 0.022(5) -0.001(4) 0.008(4) 0.008(4) C9F 0.034(6) 0.038(6) 0.035(5) -0.008(5) 0.001(5) -0.007(5) C10F 0.024(5) 0.050(6) 0.040(6) 0.008(5) 0.004(4) -0.018(5) C11F 0.043(6) 0.047(6) 0.048(6) -0.026(5) 0.004(5) -0.011(5) C12F 0.041(6) 0.032(5) 0.039(5) -0.025(4) 0.008(5) -0.014(4) C13F 0.061(6) 0.062(6) 0.054(6) -0.035(5) 0.022(5) -0.005(5) C14F 0.031(5) 0.041(6) 0.044(5) -0.023(5) 0.008(4) -0.011(4) C15F 0.023(5) 0.034(5) 0.040(5) -0.011(5) -0.002(4) -0.006(4) C16F 0.029(5) 0.021(5) 0.038(5) -0.018(4) -0.003(4) -0.004(4) C17 0.0748(19) 0.0773(18) 0.0642(15) -0.0161(14) -0.0063(15) -0.0430(16) C18 0.0595(16) 0.0465(14) 0.0454(14) -0.0057(12) -0.0055(13) -0.0046(13) C19 0.038(5) 0.041(5) 0.037(5) 0.011(4) 0.006(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O2B 2.253(7) . ? Er1 O2E 2.342(8) 1_456 ? Er1 O1C 2.367(6) . ? Er1 O1 2.367(7) . ? Er1 O1B 2.350(7) . ? Er1 O3 2.381(5) . ? Er1 N1B 2.493(9) . ? Er1 N2B 2.590(8) . ? Er2 O2D 2.259(8) . ? Er2 O1E 2.247(7) . ? Er2 O1D 2.327(7) . ? Er2 O2C 2.301(8) . ? Er2 O2F 2.381(8) . ? Er2 N2D 2.486(9) . ? Er2 O9 2.519(8) . ? Er2 N1D 2.625(9) . ? S1 O3 1.420(5) . ? S1 O5 1.431(5) . ? S1 O4 1.462(6) . ? S1 C17 1.777(5) . ? S2 O8 1.326(11) . ? S2 O7 1.397(13) . ? S2 O6 1.412(10) . ? S2 C18 1.839(8) . ? F1 C17 1.342(6) . ? F2 C17 1.310(6) . ? F3 C17 1.314(6) . ? F4 C18 1.499(16) . ? F5 C18 1.389(14) . ? F6 C18 1.165(17) . ? O1 C6 1.340(9) . ? O1 H1A 0.8200 . ? O2 C16 1.246(11) . ? O2 H2D 0.8200 . ? O9 C19 1.538(13) . ? O9 H9C 0.8200 . ? O1B C6B 1.297(9) . ? O2B C16B 1.308(9) . ? O1C C6C 1.374(8) . ? O1C H1CA 0.8200 . ? O2C C16C 1.277(9) . ? O2C H2CA 0.8200 . ? O1D C6D 1.332(9) . ? O2D C16D 1.319(10) . ? O1E C6E 1.296(9) . ? O1E H1EA 0.8200 . ? O2E C16E 1.255(9) . ? O2E Er1 2.342(8) 1_654 ? O2E H2EA 0.8200 . ? O1F C6F 1.339(11) . ? O1F H1FA 0.8200 . ? O2F C16F 1.290(10) . ? O2F H2FA 0.8200 . ? N1 C7 1.332(14) . ? N1 C8 1.470(12) . ? N2 C10 1.272(17) . ? N2 C9 1.439(14) . ? N1B C7B 1.238(14) . ? N1B C8B 1.496(13) . ? N2B C10B 1.258(14) . ? N2B C9B 1.386(13) . ? N1C C7C 1.438(14) . ? N1C C8C 1.437(13) . ? N2C C10C 1.154(12) . ? N2C C9C 1.442(13) . ? N1D C7D 1.292(15) . ? N1D C8D 1.449(14) . ? N2D C10D 1.253(14) . ? N2D C9D 1.445(8) . ? N1E C7E 1.344(13) . ? N1E C8E 1.431(8) . ? N2E C10E 1.226(15) . ? N2E C9E 1.449(14) . ? N1F C7F 1.227(15) . ? N1F C8F 1.474(14) . ? N2F C10F 1.230(16) . ? N2F C9F 1.398(15) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1B 0.9300 . ? C2 C3 1.3900 . ? C2 H2B 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C7 1.215(12) . ? C5 C6 1.3900 . ? C7 H7B 0.9300 . ? C8 C9 1.535(8) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.416(15) . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B H1BA 0.9300 . ? C2B C3B 1.3900 . ? C2B H2BA 0.9300 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B C7B 1.369(11) . ? C7B H7BA 0.9300 . ? C8B C9B 1.537(8) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C10B C11B 1.385(12) . ? C10B H10B 0.9300 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C12B H12B 0.9300 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15D 0.9300 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C1C H1CB 0.9300 . ? C2C C3C 1.3900 . ? C2C H2CB 0.9300 . ? C3C C4C 1.3900 . ? C3C H3CA 0.9300 . ? C4C C5C 1.3900 . ? C4C H4CA 0.9300 . ? C5C C7C 1.301(11) . ? C5C C6C 1.3900 . ? C7C H7CA 0.9300 . ? C8C C9C 1.491(11) . ? C8C H8CA 0.9700 . ? C8C H8CB 0.9700 . ? C9C H9CA 0.9700 . ? C9C H9CB 0.9700 . ? C10C C11C 1.515(7) . ? C10C H10F 0.9300 . ? C11C C12C 1.3900 . ? C11C C16C 1.3900 . ? C12C C13C 1.3900 . ? C12C H12C 0.9300 . ? C13C C14C 1.3900 . ? C13C H13C 0.9300 . ? C14C C15C 1.3900 . ? C14C H14C 0.9300 . ? C15C C16C 1.3900 . ? C15C H15F 0.9300 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D H1DA 0.9300 . ? C2D C3D 1.3900 . ? C2D H2DA 0.9300 . ? C3D C4D 1.3900 . ? C3D H3DA 0.9300 . ? C4D C5D 1.3900 . ? C4D H4DA 0.9300 . ? C5D C6D 1.3900 . ? C5D C7D 1.396(13) . ? C7D H7DA 0.9300 . ? C8D C9D 1.443(15) . ? C8D H8DA 0.9700 . ? C8D H8DB 0.9700 . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C10D C11D 1.533(7) . ? C10D H10C 0.9300 . ? C11D C12D 1.3900 . ? C11D C16D 1.3900 . ? C12D C13D 1.3900 . ? C12D H12D 0.9300 . ? C13D C14D 1.3900 . ? C13D H13D 0.9300 . ? C14D C15D 1.3900 . ? C14D H14D 0.9300 . ? C15D C16D 1.3900 . ? C15D H15G 0.9300 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C1E H1EB 0.9300 . ? C2E C3E 1.3900 . ? C2E H2EB 0.9300 . ? C3E C4E 1.3900 . ? C3E H3EA 0.9300 . ? C4E C5E 1.3900 . ? C4E H4EA 0.9300 . ? C5E C7E 1.381(12) . ? C5E C6E 1.3900 . ? C7E H7EA 0.9300 . ? C8E C9E 1.467(12) . ? C8E H8EA 0.9700 . ? C8E H8EB 0.9700 . ? C9E H9EA 0.9700 . ? C9E H9EB 0.9700 . ? C10E C11E 1.351(13) . ? C10E H10D 0.9300 . ? C11E C12E 1.3900 . ? C11E C16E 1.3900 . ? C12E C13E 1.3900 . ? C12E H12F 0.9300 . ? C13E C14E 1.3900 . ? C13E H13E 0.9300 . ? C14E C15E 1.3900 . ? C14E H14F 0.9300 . ? C15E C16E 1.3900 . ? C15E H15H 0.9300 . ? C1F C2F 1.3900 . ? C1F C6F 1.3900 . ? C1F H1FC 0.9300 . ? C2F C3F 1.3900 . ? C2F H2FB 0.9300 . ? C3F C4F 1.3900 . ? C3F H3FA 0.9300 . ? C4F C5F 1.3900 . ? C4F H4FA 0.9300 . ? C5F C6F 1.3900 . ? C5F C7F 1.395(13) . ? C7F H7FA 0.9300 . ? C8F C9F 1.447(15) . ? C8F H8FA 0.9700 . ? C8F H8FB 0.9700 . ? C9F H9FA 0.9700 . ? C9F H9FB 0.9700 . ? C10F C11F 1.495(13) . ? C10F H10E 0.9300 . ? C11F C12F 1.3900 . ? C11F C16F 1.3900 . ? C12F C13F 1.3900 . ? C12F H12G 0.9300 . ? C13F C14F 1.3900 . ? C13F H13F 0.9300 . ? C14F C15F 1.3900 . ? C14F H14G 0.9300 . ? C15F C16F 1.3900 . ? C15F H15I 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B Er1 O2E 96.2(3) . 1_456 ? O2B Er1 O1C 74.3(2) . . ? O2E Er1 O1C 79.5(2) 1_456 . ? O2B Er1 O1 82.8(3) . . ? O2E Er1 O1 73.7(3) 1_456 . ? O1C Er1 O1 142.4(2) . . ? O2B Er1 O1B 153.3(2) . . ? O2E Er1 O1B 68.8(2) 1_456 . ? O1C Er1 O1B 81.2(2) . . ? O1 Er1 O1B 112.1(2) . . ? O2B Er1 O3 96.8(2) . . ? O2E Er1 O3 144.4(2) 1_456 . ? O1C Er1 O3 72.4(2) . . ? O1 Er1 O3 140.9(2) . . ? O1B Er1 O3 85.4(2) . . ? O2B Er1 N1B 135.4(3) . . ? O2E Er1 N1B 117.1(3) 1_456 . ? O1C Er1 N1B 137.2(3) . . ? O1 Er1 N1B 79.5(3) . . ? O1B Er1 N1B 70.8(3) . . ? O3 Er1 N1B 73.6(3) . . ? O2B Er1 N2B 69.1(3) . . ? O2E Er1 N2B 143.1(3) 1_456 . ? O1C Er1 N2B 124.7(2) . . ? O1 Er1 N2B 71.0(3) . . ? O1B Er1 N2B 135.8(3) . . ? O3 Er1 N2B 72.4(2) . . ? N1B Er1 N2B 66.5(3) . . ? O2D Er2 O1E 72.7(3) . . ? O2D Er2 O1D 155.7(2) . . ? O1E Er2 O1D 94.1(3) . . ? O2D Er2 O2C 82.8(3) . . ? O1E Er2 O2C 77.7(3) . . ? O1D Er2 O2C 74.3(3) . . ? O2D Er2 O2F 108.2(3) . . ? O1E Er2 O2F 72.2(3) . . ? O1D Er2 O2F 86.1(3) . . ? O2C Er2 O2F 142.6(3) . . ? O2D Er2 N2D 69.2(3) . . ? O1E Er2 N2D 118.4(3) . . ? O1D Er2 N2D 134.7(2) . . ? O2C Er2 N2D 139.3(3) . . ? O2F Er2 N2D 76.1(3) . . ? O2D Er2 O9 85.8(3) . . ? O1E Er2 O9 146.0(2) . . ? O1D Er2 O9 95.3(2) . . ? O2C Er2 O9 73.6(3) . . ? O2F Er2 O9 141.0(2) . . ? N2D Er2 O9 75.5(3) . . ? O2D Er2 N1D 134.6(3) . . ? O1E Er2 N1D 140.3(3) . . ? O1D Er2 N1D 68.1(3) . . ? O2C Er2 N1D 126.1(3) . . ? O2F Er2 N1D 71.5(3) . . ? N2D Er2 N1D 66.8(3) . . ? O9 Er2 N1D 73.1(3) . . ? O3 S1 O5 116.3(4) . . ? O3 S1 O4 112.9(4) . . ? O5 S1 O4 112.4(4) . . ? O3 S1 C17 103.9(3) . . ? O5 S1 C17 106.3(4) . . ? O4 S1 C17 103.6(4) . . ? O8 S2 O7 104.7(7) . . ? O8 S2 O6 125.1(7) . . ? O7 S2 O6 120.7(7) . . ? O8 S2 C18 99.6(6) . . ? O7 S2 C18 96.0(7) . . ? O6 S2 C18 104.2(6) . . ? C6 O1 Er1 141.8(5) . . ? C6 O1 H1A 109.5 . . ? Er1 O1 H1A 92.1 . . ? C16 O2 H2D 109.4 . . ? S1 O3 Er1 171.9(4) . . ? C19 O9 Er2 128.2(6) . . ? C19 O9 H9C 109.4 . . ? Er2 O9 H9C 99.0 . . ? C6B O1B Er1 133.8(5) . . ? C16B O2B Er1 145.6(5) . . ? C6C O1C Er1 144.0(4) . . ? C6C O1C H1CA 109.4 . . ? Er1 O1C H1CA 87.8 . . ? C16C O2C Er2 153.7(6) . . ? C16C O2C H2CA 109.5 . . ? Er2 O2C H2CA 85.9 . . ? C6D O1D Er2 140.2(5) . . ? C16D O2D Er2 141.5(6) . . ? C6E O1E Er2 152.0(6) . . ? C6E O1E H1EA 109.5 . . ? Er2 O1E H1EA 88.0 . . ? C16E O2E Er1 142.8(6) . 1_654 ? C16E O2E H2EA 109.5 . . ? Er1 O2E H2EA 98.5 1_654 . ? C6F O1F H1FA 109.5 . . ? C16F O2F Er2 137.7(6) . . ? C16F O2F H2FA 109.4 . . ? Er2 O2F H2FA 92.8 . . ? C7 N1 C8 126.5(10) . . ? C10 N2 C9 118.3(10) . . ? C7B N1B C8B 119.4(9) . . ? C7B N1B Er1 128.3(7) . . ? C8B N1B Er1 110.8(6) . . ? C10B N2B C9B 115.9(9) . . ? C10B N2B Er1 126.6(7) . . ? C9B N2B Er1 117.0(6) . . ? C7C N1C C8C 123.1(9) . . ? C10C N2C C9C 121.7(9) . . ? C7D N1D C8D 111.9(10) . . ? C7D N1D Er2 134.7(8) . . ? C8D N1D Er2 110.0(7) . . ? C10D N2D C9D 115.8(9) . . ? C10D N2D Er2 127.7(6) . . ? C9D N2D Er2 114.6(7) . . ? C7E N1E C8E 119.4(8) . . ? C10E N2E C9E 125.1(10) . . ? C7F N1F C8F 114.6(10) . . ? C10F N2F C9F 117.0(11) . . ? C2 C1 C6 120.0 . . ? C2 C1 H1B 120.1 . . ? C6 C1 H1B 119.9 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2B 120.0 . . ? C3 C2 H2B 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C7 C5 C6 122.0(7) . . ? C7 C5 C4 117.9(7) . . ? C6 C5 C4 120.0 . . ? O1 C6 C5 122.5(5) . . ? O1 C6 C1 117.3(5) . . ? C5 C6 C1 120.0 . . ? C5 C7 N1 127.6(10) . . ? C5 C7 H7B 116.2 . . ? N1 C7 H7B 116.3 . . ? N1 C8 C9 107.8(8) . . ? N1 C8 H8B 110.2 . . ? C9 C8 H8B 110.1 . . ? N1 C8 H8A 110.1 . . ? C9 C8 H8A 110.2 . . ? H8B C8 H8A 108.5 . . ? N2 C9 C8 105.4(8) . . ? N2 C9 H9A 110.7 . . ? C8 C9 H9A 110.7 . . ? N2 C9 H9B 110.6 . . ? C8 C9 H9B 110.6 . . ? H9A C9 H9B 108.8 . . ? N2 C10 C11 120.3(12) . . ? N2 C10 H10A 120.0 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C12 117.8(7) . . ? C10 C11 C16 121.8(7) . . ? C12 C11 C16 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? O2 C16 C15 116.1(6) . . ? O2 C16 C11 123.9(6) . . ? C15 C16 C11 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B H1BA 120.0 . . ? C6B C1B H1BA 120.0 . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2BA 120.0 . . ? C3B C2B H2BA 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3BA 120.0 . . ? C2B C3B H3BA 120.0 . . ? C3B C4B C5B 120.0 . . ? C3B C4B H4BA 120.0 . . ? C5B C4B H4BA 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B C7B 122.8(6) . . ? C4B C5B C7B 117.2(6) . . ? O1B C6B C5B 123.9(5) . . ? O1B C6B C1B 116.0(5) . . ? C5B C6B C1B 120.0 . . ? N1B C7B C5B 130.5(10) . . ? N1B C7B H7BA 114.7 . . ? C5B C7B H7BA 114.8 . . ? N1B C8B C9B 109.7(8) . . ? N1B C8B H8BA 109.6 . . ? C9B C8B H8BA 109.7 . . ? N1B C8B H8BB 109.9 . . ? C9B C8B H8BB 109.8 . . ? H8BA C8B H8BB 108.2 . . ? N2B C9B C8B 105.4(8) . . ? N2B C9B H9BA 110.6 . . ? C8B C9B H9BA 110.6 . . ? N2B C9B H9BB 110.8 . . ? C8B C9B H9BB 110.7 . . ? H9BA C9B H9BB 108.8 . . ? N2B C10B C11B 133.6(9) . . ? N2B C10B H10B 113.3 . . ? C11B C10B H10B 113.2 . . ? C10B C11B C12B 119.8(5) . . ? C10B C11B C16B 120.0(5) . . ? C12B C11B C16B 120.0 . . ? C13B C12B C11B 120.0 . . ? C13B C12B H12B 120.0 . . ? C11B C12B H12B 120.0 . . ? C14B C13B C12B 120.0 . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B C15B 120.0 . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15D 120.0 . . ? C14B C15B H15D 120.0 . . ? O2B C16B C15B 117.6(4) . . ? O2B C16B C11B 122.4(4) . . ? C15B C16B C11B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C H1CB 120.0 . . ? C6C C1C H1CB 120.0 . . ? C3C C2C C1C 120.0 . . ? C3C C2C H2CB 120.0 . . ? C1C C2C H2CB 120.0 . . ? C4C C3C C2C 120.0 . . ? C4C C3C H3CA 120.0 . . ? C2C C3C H3CA 120.0 . . ? C3C C4C C5C 120.0 . . ? C3C C4C H4CA 120.0 . . ? C5C C4C H4CA 120.0 . . ? C7C C5C C6C 122.9(6) . . ? C7C C5C C4C 117.1(6) . . ? C6C C5C C4C 120.0 . . ? C5C C6C C1C 120.0 . . ? C5C C6C O1C 114.9(4) . . ? C1C C6C O1C 125.1(4) . . ? C5C C7C N1C 124.9(10) . . ? C5C C7C H7CA 117.6 . . ? N1C C7C H7CA 117.5 . . ? N1C C8C C9C 109.6(7) . . ? N1C C8C H8CA 109.6 . . ? C9C C8C H8CA 109.7 . . ? N1C C8C H8CB 110.0 . . ? C9C C8C H8CB 109.7 . . ? H8CA C8C H8CB 108.2 . . ? N2C C9C C8C 110.3(8) . . ? N2C C9C H9CA 109.4 . . ? C8C C9C H9CA 109.6 . . ? N2C C9C H9CB 109.7 . . ? C8C C9C H9CB 109.6 . . ? H9CA C9C H9CB 108.1 . . ? N2C C10C C11C 121.6(8) . . ? N2C C10C H10F 119.3 . . ? C11C C10C H10F 119.1 . . ? C12C C11C C16C 120.0 . . ? C12C C11C C10C 122.6(5) . . ? C16C C11C C10C 116.5(5) . . ? C13C C12C C11C 120.0 . . ? C13C C12C H12C 120.0 . . ? C11C C12C H12C 120.0 . . ? C12C C13C C14C 120.0 . . ? C12C C13C H13C 120.0 . . ? C14C C13C H13C 120.0 . . ? C15C C14C C13C 120.0 . . ? C15C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C14C C15C C16C 120.0 . . ? C14C C15C H15F 120.0 . . ? C16C C15C H15F 120.0 . . ? O2C C16C C15C 113.1(5) . . ? O2C C16C C11C 126.9(5) . . ? C15C C16C C11C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D H1DA 120.0 . . ? C6D C1D H1DA 120.0 . . ? C1D C2D C3D 120.0 . . ? C1D C2D H2DA 120.0 . . ? C3D C2D H2DA 120.0 . . ? C4D C3D C2D 120.0 . . ? C4D C3D H3DA 120.0 . . ? C2D C3D H3DA 120.0 . . ? C3D C4D C5D 120.0 . . ? C3D C4D H4DA 120.0 . . ? C5D C4D H4DA 120.0 . . ? C6D C5D C4D 120.0 . . ? C6D C5D C7D 129.6(6) . . ? C4D C5D C7D 110.0(6) . . ? O1D C6D C5D 122.7(5) . . ? O1D C6D C1D 117.3(5) . . ? C5D C6D C1D 120.0 . . ? N1D C7D C5D 118.7(10) . . ? N1D C7D H7DA 120.6 . . ? C5D C7D H7DA 120.7 . . ? N1D C8D C9D 114.5(9) . . ? N1D C8D H8DA 108.5 . . ? C9D C8D H8DA 108.7 . . ? N1D C8D H8DB 108.7 . . ? C9D C8D H8DB 108.7 . . ? H8DA C8D H8DB 107.6 . . ? N2D C9D C8D 108.3(9) . . ? N2D C9D H9DA 109.9 . . ? C8D C9D H9DA 110.0 . . ? N2D C9D H9DB 110.2 . . ? C8D C9D H9DB 110.1 . . ? H9DA C9D H9DB 108.4 . . ? N2D C10D C11D 127.1(10) . . ? N2D C10D H10C 116.4 . . ? C11D C10D H10C 116.4 . . ? C12D C11D C16D 120.0 . . ? C12D C11D C10D 115.9(6) . . ? C16D C11D C10D 124.0(6) . . ? C13D C12D C11D 120.0 . . ? C13D C12D H12D 120.0 . . ? C11D C12D H12D 120.0 . . ? C12D C13D C14D 120.0 . . ? C12D C13D H13D 120.0 . . ? C14D C13D H13D 120.0 . . ? C15D C14D C13D 120.0 . . ? C15D C14D H14D 120.0 . . ? C13D C14D H14D 120.0 . . ? C14D C15D C16D 120.0 . . ? C14D C15D H15G 120.0 . . ? C16D C15D H15G 120.0 . . ? O2D C16D C15D 126.0(5) . . ? O2D C16D C11D 113.9(5) . . ? C15D C16D C11D 120.0 . . ? C2E C1E C6E 120.0 . . ? C2E C1E H1EB 120.0 . . ? C6E C1E H1EB 120.0 . . ? C3E C2E C1E 120.0 . . ? C3E C2E H2EB 120.0 . . ? C1E C2E H2EB 120.0 . . ? C2E C3E C4E 120.0 . . ? C2E C3E H3EA 120.0 . . ? C4E C3E H3EA 120.0 . . ? C5E C4E C3E 120.0 . . ? C5E C4E H4EA 120.0 . . ? C3E C4E H4EA 120.0 . . ? C7E C5E C4E 119.2(6) . . ? C7E C5E C6E 120.6(6) . . ? C4E C5E C6E 120.0 . . ? O1E C6E C5E 124.4(4) . . ? O1E C6E C1E 115.6(4) . . ? C5E C6E C1E 120.0 . . ? N1E C7E C5E 125.5(8) . . ? N1E C7E H7EA 117.3 . . ? C5E C7E H7EA 117.2 . . ? N1E C8E C9E 109.5(7) . . ? N1E C8E H8EA 109.8 . . ? C9E C8E H8EA 109.8 . . ? N1E C8E H8EB 109.8 . . ? C9E C8E H8EB 109.8 . . ? H8EA C8E H8EB 108.2 . . ? N2E C9E C8E 109.4(8) . . ? N2E C9E H9EA 109.7 . . ? C8E C9E H9EA 109.8 . . ? N2E C9E H9EB 109.8 . . ? C8E C9E H9EB 109.8 . . ? H9EA C9E H9EB 108.3 . . ? N2E C10E C11E 122.9(10) . . ? N2E C10E H10D 118.5 . . ? C11E C10E H10D 118.6 . . ? C10E C11E C12E 114.9(6) . . ? C10E C11E C16E 125.0(6) . . ? C12E C11E C16E 120.0 . . ? C13E C12E C11E 120.0 . . ? C13E C12E H12F 120.0 . . ? C11E C12E H12F 120.0 . . ? C12E C13E C14E 120.0 . . ? C12E C13E H13E 120.0 . . ? C14E C13E H13E 120.0 . . ? C13E C14E C15E 120.0 . . ? C13E C14E H14F 120.0 . . ? C15E C14E H14F 120.0 . . ? C16E C15E C14E 120.0 . . ? C16E C15E H15H 120.0 . . ? C14E C15E H15H 120.0 . . ? O2E C16E C15E 121.8(5) . . ? O2E C16E C11E 117.9(5) . . ? C15E C16E C11E 120.0 . . ? C2F C1F C6F 120.0 . . ? C2F C1F H1FC 120.0 . . ? C6F C1F H1FC 120.0 . . ? C1F C2F C3F 120.0 . . ? C1F C2F H2FB 120.0 . . ? C3F C2F H2FB 120.0 . . ? C4F C3F C2F 120.0 . . ? C4F C3F H3FA 120.0 . . ? C2F C3F H3FA 120.0 . . ? C3F C4F C5F 120.0 . . ? C3F C4F H4FA 120.0 . . ? C5F C4F H4FA 120.0 . . ? C6F C5F C4F 120.0 . . ? C6F C5F C7F 119.9(6) . . ? C4F C5F C7F 120.1(6) . . ? O1F C6F C5F 121.1(6) . . ? O1F C6F C1F 118.8(6) . . ? C5F C6F C1F 120.0 . . ? N1F C7F C5F 121.4(10) . . ? N1F C7F H7FA 119.2 . . ? C5F C7F H7FA 119.5 . . ? N1F C8F C9F 111.5(9) . . ? N1F C8F H8FA 109.4 . . ? C9F C8F H8FA 109.4 . . ? N1F C8F H8FB 109.2 . . ? C9F C8F H8FB 109.3 . . ? H8FA C8F H8FB 108.0 . . ? N2F C9F C8F 107.8(10) . . ? N2F C9F H9FA 110.1 . . ? C8F C9F H9FA 110.1 . . ? N2F C9F H9FB 110.1 . . ? C8F C9F H9FB 110.3 . . ? H9FA C9F H9FB 108.5 . . ? N2F C10F C11F 119.2(12) . . ? N2F C10F H10E 120.4 . . ? C11F C10F H10E 120.5 . . ? C12F C11F C16F 120.0 . . ? C12F C11F C10F 115.1(7) . . ? C16F C11F C10F 124.5(7) . . ? C11F C12F C13F 120.0 . . ? C11F C12F H12G 120.0 . . ? C13F C12F H12G 120.0 . . ? C14F C13F C12F 120.0 . . ? C14F C13F H13F 120.0 . . ? C12F C13F H13F 120.0 . . ? C13F C14F C15F 120.0 . . ? C13F C14F H14G 120.0 . . ? C15F C14F H14G 120.0 . . ? C16F C15F C14F 120.0 . . ? C16F C15F H15I 120.0 . . ? C14F C15F H15I 120.0 . . ? O2F C16F C15F 119.7(6) . . ? O2F C16F C11F 119.9(6) . . ? C15F C16F C11F 120.0 . . ? F2 C17 F3 111.5(6) . . ? F2 C17 F1 108.1(5) . . ? F3 C17 F1 105.8(6) . . ? F2 C17 S1 111.5(4) . . ? F3 C17 S1 109.9(5) . . ? F1 C17 S1 109.8(4) . . ? F6 C18 F5 114.6(10) . . ? F6 C18 F4 101.4(10) . . ? F5 C18 F4 110.4(11) . . ? F6 C18 S2 116.7(10) . . ? F5 C18 S2 110.6(8) . . ? F4 C18 S2 101.9(6) . . ? O9 C19 H19A 109.5 . . ? O9 C19 H19B 109.4 . . ? H19A C19 H19B 109.5 . . ? O9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.890 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.179 # Attachment 'Complex-4.CIF' data_Complex-4 _database_code_depnum_ccdc_archive 'CCDC 733184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H42 N4 O10 Yb2' _chemical_formula_sum 'C38 H42 N4 O10 Yb2' _chemical_formula_weight 1060.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.117(3) _cell_length_b 20.590(4) _cell_length_c 22.583(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7959(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9602 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 4.731 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.4668 _exptl_absorpt_correction_T_max 0.6755 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13346 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7006 _reflns_number_gt 5575 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+4.0196P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7006 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.12001(2) 0.689214(16) 0.588598(15) 0.01908(14) Uani 1 1 d U . . Yb2 Yb 0.33504(2) 0.654373(16) 0.533881(15) 0.01938(14) Uani 1 1 d U . . N1 N 0.0262(4) 0.7368(3) 0.6644(3) 0.0182(14) Uani 1 1 d U . . N2 N 0.1403(4) 0.8107(3) 0.6048(3) 0.0187(14) Uani 1 1 d U . . N1B N 0.4291(4) 0.5912(3) 0.4688(3) 0.0179(14) Uani 1 1 d U . . N2B N 0.4672(4) 0.6444(3) 0.5798(3) 0.0172(14) Uani 1 1 d U . . O1 O 0.0572(3) 0.6080(2) 0.6312(2) 0.0186(12) Uani 1 1 d U . . O2 O 0.2194(3) 0.7246(2) 0.5251(2) 0.0137(11) Uani 1 1 d U . . O3 O 0.0191(3) 0.7329(2) 0.5345(2) 0.0202(12) Uani 1 1 d U . . O4 O -0.0988(3) 0.7631(3) 0.5074(2) 0.0217(12) Uani 1 1 d U . . O5 O 0.2270(3) 0.6106(2) 0.5912(2) 0.0139(11) Uani 1 1 d U . . O6 O 0.3269(3) 0.5444(2) 0.5791(2) 0.0188(12) Uani 1 1 d U . . O7 O 0.2040(3) 0.7090(3) 0.6738(2) 0.0188(12) Uani 1 1 d U . . H7B H 0.2474 0.7102 0.6585 0.023 Uiso 1 1 calc R . . O8 O 0.1162(3) 0.6175(2) 0.4994(2) 0.0176(11) Uani 1 1 d U . . H8C H 0.1602 0.6220 0.4857 0.021 Uiso 1 1 calc R . . O1B O 0.2650(3) 0.6115(3) 0.4573(2) 0.0184(12) Uani 1 1 d U . . O2B O 0.3391(3) 0.7140(2) 0.6220(2) 0.0169(11) Uani 1 1 d U . . C1 C 0.0161(4) 0.5926(4) 0.6787(3) 0.0165(16) Uani 1 1 d U . . C2 C 0.0078(5) 0.5273(4) 0.6953(4) 0.0233(18) Uani 1 1 d U . . H2A H 0.0289 0.4952 0.6712 0.028 Uiso 1 1 calc R . . C3 C -0.0309(4) 0.5092(4) 0.7464(4) 0.0219(18) Uani 1 1 d U . . H3A H -0.0324 0.4657 0.7573 0.026 Uiso 1 1 calc R . . C4 C -0.0676(5) 0.5554(4) 0.7817(4) 0.0248(19) Uani 1 1 d U . . H4A H -0.0946 0.5434 0.8157 0.030 Uiso 1 1 calc R . . C5 C -0.0629(5) 0.6200(4) 0.7646(4) 0.0273(19) Uani 1 1 d U . . H5A H -0.0889 0.6511 0.7870 0.033 Uiso 1 1 calc R . . C6 C -0.0206(5) 0.6398(4) 0.7154(3) 0.0195(17) Uani 1 1 d U . . C7 C -0.0161(5) 0.7091(4) 0.7038(4) 0.0225(18) Uani 1 1 d U . . H7A H -0.0469 0.7360 0.7273 0.027 Uiso 1 1 calc R . . C8 C 0.0221(5) 0.8085(4) 0.6621(4) 0.0240(19) Uani 1 1 d U . . H8A H -0.0039 0.8248 0.6973 0.029 Uiso 1 1 calc R . . H8B H -0.0079 0.8220 0.6278 0.029 Uiso 1 1 calc R . . C9 C 0.1036(5) 0.8359(4) 0.6585(4) 0.0214(18) Uani 1 1 d U . . H9A H 0.1016 0.8830 0.6572 0.026 Uiso 1 1 calc R . . H9B H 0.1335 0.8231 0.6931 0.026 Uiso 1 1 calc R . . C10 C 0.1724(4) 0.8527(4) 0.5702(4) 0.0195(17) Uani 1 1 d U . . H10A H 0.1741 0.8955 0.5835 0.023 Uiso 1 1 calc R . . C11 C 0.2060(4) 0.8398(4) 0.5128(4) 0.0170(16) Uani 1 1 d U . . C12 C 0.2174(5) 0.8953(4) 0.4756(4) 0.0245(19) Uani 1 1 d U . . H12A H 0.2074 0.9367 0.4903 0.029 Uiso 1 1 calc R . . C13 C 0.2432(5) 0.8877(5) 0.4182(4) 0.031(2) Uani 1 1 d U . . H13A H 0.2506 0.9240 0.3943 0.037 Uiso 1 1 calc R . . C14 C 0.2580(5) 0.8261(5) 0.3958(4) 0.031(2) Uani 1 1 d U . . H14A H 0.2746 0.8212 0.3568 0.038 Uiso 1 1 calc R . . C15 C 0.2480(5) 0.7725(4) 0.4313(4) 0.0237(18) Uani 1 1 d U . . H15A H 0.2580 0.7316 0.4156 0.028 Uiso 1 1 calc R . . C16 C 0.2232(4) 0.7773(4) 0.4907(3) 0.0166(16) Uani 1 1 d U . . C17 C -0.0487(5) 0.7203(4) 0.5164(3) 0.0172(16) Uani 1 1 d U . . C18 C -0.0704(5) 0.6514(4) 0.5036(4) 0.030(2) Uani 1 1 d U . . H18A H -0.1237 0.6496 0.4903 0.045 Uiso 1 1 calc R . . H18B H -0.0648 0.6259 0.5389 0.045 Uiso 1 1 calc R . . H18C H -0.0368 0.6345 0.4733 0.045 Uiso 1 1 calc R . . C19 C 0.2584(4) 0.5544(4) 0.5981(3) 0.0154(16) Uani 1 1 d U . . C20 C 0.2142(5) 0.5011(4) 0.6278(4) 0.030(2) Uani 1 1 d U . . H20A H 0.2350 0.4941 0.6668 0.045 Uiso 1 1 calc R . . H20B H 0.2191 0.4619 0.6050 0.045 Uiso 1 1 calc R . . H20C H 0.1601 0.5129 0.6307 0.045 Uiso 1 1 calc R . . C21 C 0.2071(6) 0.6703(5) 0.7269(4) 0.040(2) Uani 1 1 d U . . H21A H 0.2453 0.6883 0.7534 0.059 Uiso 1 1 calc R . . H21B H 0.2213 0.6266 0.7170 0.059 Uiso 1 1 calc R . . H21C H 0.1568 0.6705 0.7457 0.059 Uiso 1 1 calc R . . C22 C 0.0946(5) 0.5503(4) 0.4974(4) 0.029(2) Uani 1 1 d U . . H22A H 0.0986 0.5348 0.4575 0.044 Uiso 1 1 calc R . . H22B H 0.0417 0.5455 0.5110 0.044 Uiso 1 1 calc R . . H22C H 0.1289 0.5257 0.5225 0.044 Uiso 1 1 calc R . . C1B C 0.2724(5) 0.5821(4) 0.4061(3) 0.0178(17) Uani 1 1 d U . . C2B C 0.2087(5) 0.5729(4) 0.3680(4) 0.029(2) Uani 1 1 d U . . H2BA H 0.1602 0.5891 0.3792 0.034 Uiso 1 1 calc R . . C3B C 0.2146(6) 0.5414(5) 0.3153(4) 0.035(2) Uani 1 1 d U . . H3BA H 0.1706 0.5368 0.2914 0.042 Uiso 1 1 calc R . . C4B C 0.2859(6) 0.5158(5) 0.2965(4) 0.035(2) Uani 1 1 d U . . H4BA H 0.2898 0.4930 0.2611 0.042 Uiso 1 1 calc R . . C5B C 0.3497(6) 0.5252(4) 0.3314(4) 0.029(2) Uani 1 1 d U . . H5BA H 0.3977 0.5093 0.3187 0.035 Uiso 1 1 calc R . . C6B C 0.3459(5) 0.5577(4) 0.3852(3) 0.0185(17) Uani 1 1 d U . . C7B C 0.4187(4) 0.5649(3) 0.4185(3) 0.0161(16) Uani 1 1 d U . . H7BA H 0.4631 0.5480 0.4006 0.019 Uiso 1 1 calc R . . C8B C 0.5091(5) 0.5924(4) 0.4906(4) 0.0234(18) Uani 1 1 d U . . H8BA H 0.5344 0.6322 0.4777 0.028 Uiso 1 1 calc R . . H8BB H 0.5378 0.5561 0.4741 0.028 Uiso 1 1 calc R . . C9B C 0.5110(5) 0.5887(4) 0.5580(4) 0.0217(18) Uani 1 1 d U . . H9BA H 0.4872 0.5486 0.5715 0.026 Uiso 1 1 calc R . . H9BB H 0.5644 0.5902 0.5722 0.026 Uiso 1 1 calc R . . C10B C 0.5057(5) 0.6886(4) 0.6064(4) 0.0202(17) Uani 1 1 d U . . H10B H 0.5592 0.6824 0.6105 0.024 Uiso 1 1 calc R . . C11B C 0.4729(4) 0.7475(4) 0.6309(3) 0.0178(16) Uani 1 1 d U . . C12B C 0.5252(5) 0.7956(4) 0.6499(4) 0.0271(19) Uani 1 1 d U . . H12B H 0.5786 0.7888 0.6452 0.033 Uiso 1 1 calc R . . C13B C 0.4999(5) 0.8522(4) 0.6750(4) 0.029(2) Uani 1 1 d U . . H13B H 0.5354 0.8846 0.6851 0.034 Uiso 1 1 calc R . . C14B C 0.4198(5) 0.8608(4) 0.6855(4) 0.028(2) Uani 1 1 d U . . H14B H 0.4024 0.8982 0.7044 0.034 Uiso 1 1 calc R . . C15B C 0.3663(5) 0.8141(4) 0.6677(4) 0.0210(18) Uani 1 1 d U . . H15B H 0.3134 0.8205 0.6751 0.025 Uiso 1 1 calc R . . C16B C 0.3911(5) 0.7573(4) 0.6388(3) 0.0179(17) Uani 1 1 d U . . 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 Yb1 0.0148(2) 0.0206(2) 0.0218(2) 0.00006(15) 0.00114(14) 0.00144(14) Yb2 0.0129(2) 0.0209(2) 0.0243(2) -0.00126(15) -0.00018(14) -0.00087(14) N1 0.015(3) 0.018(3) 0.021(3) -0.001(3) 0.003(3) 0.002(3) N2 0.017(3) 0.015(3) 0.023(3) -0.002(3) -0.003(3) 0.004(3) N1B 0.013(3) 0.015(3) 0.026(3) 0.001(3) 0.003(3) -0.001(3) N2B 0.016(3) 0.015(3) 0.021(3) 0.000(3) -0.001(3) 0.002(3) O1 0.018(3) 0.017(3) 0.022(3) 0.000(2) 0.011(2) 0.001(2) O2 0.010(3) 0.016(2) 0.016(2) 0.002(2) -0.001(2) -0.001(2) O3 0.013(3) 0.021(3) 0.027(3) -0.004(2) -0.004(2) 0.002(2) O4 0.011(3) 0.022(3) 0.031(3) 0.004(3) 0.001(2) 0.004(2) O5 0.010(3) 0.013(2) 0.018(3) 0.001(2) 0.003(2) 0.001(2) O6 0.011(3) 0.017(3) 0.028(3) 0.003(2) 0.003(2) 0.001(2) O7 0.010(3) 0.029(3) 0.018(3) -0.002(2) 0.000(2) 0.004(2) O8 0.004(2) 0.022(3) 0.027(3) -0.007(2) 0.002(2) -0.001(2) O1B 0.014(3) 0.022(3) 0.019(3) -0.006(2) -0.001(2) -0.001(2) O2B 0.009(3) 0.018(3) 0.024(3) -0.005(2) -0.005(2) 0.000(2) C1 0.009(4) 0.022(4) 0.019(4) 0.001(3) -0.001(3) 0.003(3) C2 0.023(4) 0.023(4) 0.024(4) -0.002(3) 0.003(3) -0.001(3) C3 0.016(4) 0.026(4) 0.024(4) 0.000(4) 0.000(3) -0.006(3) C4 0.024(4) 0.027(4) 0.023(4) -0.002(4) 0.007(3) -0.008(3) C5 0.025(4) 0.028(4) 0.029(4) -0.013(4) 0.006(3) -0.003(4) C6 0.017(4) 0.022(4) 0.020(4) 0.001(3) 0.006(3) 0.001(3) C7 0.016(4) 0.025(4) 0.027(4) -0.006(4) 0.000(3) 0.005(3) C8 0.033(5) 0.017(4) 0.022(4) 0.001(3) 0.006(3) 0.009(3) C9 0.026(4) 0.017(4) 0.021(4) -0.003(3) 0.003(3) 0.003(3) C10 0.013(4) 0.019(4) 0.026(4) -0.002(3) -0.006(3) 0.000(3) C11 0.008(4) 0.019(4) 0.024(4) 0.002(3) 0.001(3) -0.003(3) C12 0.014(4) 0.018(4) 0.041(5) 0.009(4) -0.008(3) 0.000(3) C13 0.023(4) 0.036(5) 0.035(4) 0.016(4) 0.003(4) 0.001(4) C14 0.029(5) 0.042(5) 0.023(4) 0.011(4) 0.003(4) 0.005(4) C15 0.018(4) 0.028(4) 0.026(4) 0.004(4) 0.000(3) 0.000(3) C16 0.009(4) 0.023(4) 0.018(4) 0.004(3) -0.004(3) 0.000(3) C17 0.018(4) 0.020(4) 0.014(3) 0.001(3) 0.004(3) 0.002(3) C18 0.018(4) 0.025(4) 0.047(5) 0.001(4) -0.008(4) 0.000(3) C19 0.014(4) 0.018(4) 0.014(3) 0.000(3) -0.003(3) 0.001(3) C20 0.025(4) 0.029(4) 0.036(4) 0.005(4) 0.008(4) 0.008(4) C21 0.029(5) 0.060(6) 0.030(4) 0.014(4) -0.003(4) 0.005(4) C22 0.024(4) 0.028(4) 0.036(5) -0.008(4) 0.000(4) -0.005(4) C1B 0.018(4) 0.017(4) 0.019(4) 0.001(3) -0.003(3) -0.006(3) C2B 0.024(4) 0.040(5) 0.022(4) -0.002(4) -0.007(3) 0.005(4) C3B 0.032(5) 0.041(5) 0.030(4) -0.006(4) -0.010(4) -0.005(4) C4B 0.041(5) 0.040(5) 0.024(4) -0.012(4) -0.002(4) -0.001(4) C5B 0.032(5) 0.035(4) 0.021(4) 0.001(4) 0.008(4) -0.004(4) C6B 0.019(4) 0.016(4) 0.020(4) 0.004(3) 0.005(3) -0.001(3) C7B 0.012(4) 0.012(3) 0.024(4) 0.004(3) 0.006(3) -0.005(3) C8B 0.011(4) 0.021(4) 0.039(4) -0.010(4) 0.002(3) 0.003(3) C9B 0.013(4) 0.017(4) 0.035(4) -0.001(3) -0.001(3) 0.005(3) C10B 0.012(4) 0.026(4) 0.023(4) 0.000(3) -0.005(3) 0.006(3) C11B 0.015(4) 0.017(3) 0.021(4) 0.000(3) -0.004(3) -0.004(3) C12B 0.017(4) 0.032(4) 0.032(4) -0.001(4) -0.002(3) -0.001(3) C13B 0.031(5) 0.024(4) 0.031(4) -0.004(4) 0.003(4) -0.010(4) C14B 0.035(5) 0.020(4) 0.030(4) -0.003(4) -0.003(4) -0.005(4) C15B 0.017(4) 0.022(4) 0.024(4) 0.002(3) 0.000(3) 0.002(3) C16B 0.022(4) 0.019(4) 0.012(3) 0.002(3) -0.001(3) -0.003(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 Yb1 O1 2.208(5) . ? Yb1 O3 2.299(5) . ? Yb1 O2 2.341(5) . ? Yb1 O7 2.435(5) . ? Yb1 O5 2.445(5) . ? Yb1 O8 2.497(5) . ? Yb1 N1 2.543(6) . ? Yb1 N2 2.552(6) . ? Yb1 Yb2 3.9483(8) . ? Yb2 O4 2.245(5) 4_566 ? Yb2 O1B 2.282(5) . ? Yb2 O2B 2.340(5) . ? Yb2 O5 2.431(5) . ? Yb2 O2 2.459(5) . ? Yb2 O6 2.489(5) . ? Yb2 N2B 2.497(6) . ? Yb2 N1B 2.539(6) . ? Yb2 C19 2.839(7) . ? N1 C7 1.282(10) . ? N1 C8 1.479(10) . ? N2 C10 1.289(10) . ? N2 C9 1.463(10) . ? N1B C7B 1.270(10) . ? N1B C8B 1.455(10) . ? N2B C10B 1.273(10) . ? N2B C9B 1.457(10) . ? O1 C1 1.322(9) . ? O2 C16 1.335(9) . ? O3 C17 1.257(9) . ? O4 C17 1.247(9) . ? O4 Yb2 2.245(5) 4_466 ? O5 C19 1.285(9) . ? O6 C19 1.266(9) . ? O7 C21 1.440(10) . ? O7 H7B 0.8200 . ? O8 C22 1.433(10) . ? O8 H8C 0.8200 . ? O1B C1B 1.311(9) . ? O2B C16B 1.314(9) . ? C1 C2 1.403(11) . ? C1 C6 1.424(11) . ? C2 C3 1.381(11) . ? C2 H2A 0.9300 . ? C3 C4 1.391(12) . ? C3 H3A 0.9300 . ? C4 C5 1.386(12) . ? C4 H4A 0.9300 . ? C5 C6 1.387(11) . ? C5 H5A 0.9300 . ? C6 C7 1.453(11) . ? C7 H7A 0.9300 . ? C8 C9 1.507(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.443(11) . ? C10 H10A 0.9300 . ? C11 C16 1.411(11) . ? C11 C12 1.432(11) . ? C12 C13 1.380(12) . ? C12 H12A 0.9300 . ? C13 C14 1.388(13) . ? C13 H13A 0.9300 . ? C14 C15 1.376(12) . ? C14 H14A 0.9300 . ? C15 C16 1.411(11) . ? C15 H15A 0.9300 . ? C17 C18 1.495(11) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.493(11) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C1B C2B 1.404(11) . ? C1B C6B 1.434(11) . ? C2B C3B 1.359(12) . ? C2B H2BA 0.9300 . ? C3B C4B 1.396(13) . ? C3B H3BA 0.9300 . ? C4B C5B 1.359(13) . ? C4B H4BA 0.9300 . ? C5B C6B 1.388(12) . ? C5B H5BA 0.9300 . ? C6B C7B 1.463(11) . ? C7B H7BA 0.9300 . ? C8B C9B 1.524(12) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C10B C11B 1.446(11) . ? C10B H10B 0.9300 . ? C11B C12B 1.403(11) . ? C11B C16B 1.426(11) . ? C12B C13B 1.366(12) . ? C12B H12B 0.9300 . ? C13B C14B 1.402(13) . ? C13B H13B 0.9300 . ? C14B C15B 1.386(12) . ? C14B H14B 0.9300 . ? C15B C16B 1.406(11) . ? C15B H15B 0.9300 . ? 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 Yb1 O3 99.28(19) . . ? O1 Yb1 O2 148.91(17) . . ? O3 Yb1 O2 95.69(18) . . ? O1 Yb1 O7 94.01(19) . . ? O3 Yb1 O7 142.90(18) . . ? O2 Yb1 O7 90.17(17) . . ? O1 Yb1 O5 81.55(17) . . ? O3 Yb1 O5 146.61(17) . . ? O2 Yb1 O5 71.14(16) . . ? O7 Yb1 O5 69.48(17) . . ? O1 Yb1 O8 83.73(18) . . ? O3 Yb1 O8 77.51(17) . . ? O2 Yb1 O8 73.09(16) . . ? O7 Yb1 O8 138.67(17) . . ? O5 Yb1 O8 69.37(16) . . ? O1 Yb1 N1 71.98(19) . . ? O3 Yb1 N1 74.44(19) . . ? O2 Yb1 N1 138.70(19) . . ? O7 Yb1 N1 77.11(19) . . ? O5 Yb1 N1 135.38(18) . . ? O8 Yb1 N1 138.90(18) . . ? O1 Yb1 N2 138.2(2) . . ? O3 Yb1 N2 78.2(2) . . ? O2 Yb1 N2 71.56(19) . . ? O7 Yb1 N2 69.07(19) . . ? O5 Yb1 N2 122.93(19) . . ? O8 Yb1 N2 134.31(19) . . ? N1 Yb1 N2 67.2(2) . . ? O1 Yb1 Yb2 116.93(13) . . ? O3 Yb1 Yb2 127.27(13) . . ? O2 Yb1 Yb2 35.66(12) . . ? O7 Yb1 Yb2 74.18(12) . . ? O5 Yb1 Yb2 35.82(11) . . ? O8 Yb1 Yb2 70.41(11) . . ? N1 Yb1 Yb2 150.38(15) . . ? N2 Yb1 Yb2 95.50(15) . . ? O4 Yb2 O1B 104.04(19) 4_566 . ? O4 Yb2 O2B 86.62(19) 4_566 . ? O1B Yb2 O2B 149.70(18) . . ? O4 Yb2 O5 152.36(18) 4_566 . ? O1B Yb2 O5 81.98(17) . . ? O2B Yb2 O5 76.39(17) . . ? O4 Yb2 O2 85.83(17) 4_566 . ? O1B Yb2 O2 75.12(17) . . ? O2B Yb2 O2 77.54(16) . . ? O5 Yb2 O2 69.45(16) . . ? O4 Yb2 O6 152.58(18) 4_566 . ? O1B Yb2 O6 85.98(18) . . ? O2B Yb2 O6 97.49(18) . . ? O5 Yb2 O6 53.22(16) . . ? O2 Yb2 O6 121.56(16) . . ? O4 Yb2 N2B 77.2(2) 4_566 . ? O1B Yb2 N2B 139.38(19) . . ? O2B Yb2 N2B 70.28(19) . . ? O5 Yb2 N2B 115.95(18) . . ? O2 Yb2 N2B 144.19(18) . . ? O6 Yb2 N2B 78.78(18) . . ? O4 Yb2 N1B 80.1(2) 4_566 . ? O1B Yb2 N1B 72.3(2) . . ? O2B Yb2 N1B 137.93(19) . . ? O5 Yb2 N1B 126.91(18) . . ? O2 Yb2 N1B 139.92(19) . . ? O6 Yb2 N1B 78.83(18) . . ? N2B Yb2 N1B 67.9(2) . . ? O4 Yb2 C19 173.7(2) 4_566 . ? O1B Yb2 C19 82.2(2) . . ? O2B Yb2 C19 87.70(19) . . ? O5 Yb2 C19 26.82(19) . . ? O2 Yb2 C19 95.50(19) . . ? O6 Yb2 C19 26.45(19) . . ? N2B Yb2 C19 98.4(2) . . ? N1B Yb2 C19 102.5(2) . . ? O4 Yb2 Yb1 117.56(14) 4_566 . ? O1B Yb2 Yb1 79.49(13) . . ? O2B Yb2 Yb1 70.51(12) . . ? O5 Yb2 Yb1 36.06(11) . . ? O2 Yb2 Yb1 33.71(11) . . ? O6 Yb2 Yb1 89.14(12) . . ? N2B Yb2 Yb1 136.85(15) . . ? N1B Yb2 Yb1 149.95(14) . . ? C19 Yb2 Yb1 62.70(15) . . ? C7 N1 C8 116.2(7) . . ? C7 N1 Yb1 130.8(5) . . ? C8 N1 Yb1 113.0(5) . . ? C10 N2 C9 116.6(6) . . ? C10 N2 Yb1 129.0(5) . . ? C9 N2 Yb1 114.1(5) . . ? C7B N1B C8B 116.3(7) . . ? C7B N1B Yb2 130.2(5) . . ? C8B N1B Yb2 113.1(5) . . ? C10B N2B C9B 117.2(7) . . ? C10B N2B Yb2 127.3(5) . . ? C9B N2B Yb2 113.0(5) . . ? C1 O1 Yb1 142.6(5) . . ? C16 O2 Yb1 130.1(4) . . ? C16 O2 Yb2 119.0(4) . . ? Yb1 O2 Yb2 110.63(19) . . ? C17 O3 Yb1 141.8(5) . . ? C17 O4 Yb2 161.7(5) . 4_466 ? C19 O5 Yb2 94.6(4) . . ? C19 O5 Yb1 155.9(5) . . ? Yb2 O5 Yb1 108.12(18) . . ? C19 O6 Yb2 92.4(4) . . ? C21 O7 Yb1 126.0(5) . . ? C21 O7 H7B 109.5 . . ? Yb1 O7 H7B 102.1 . . ? C22 O8 Yb1 127.1(5) . . ? C22 O8 H8C 109.5 . . ? Yb1 O8 H8C 102.4 . . ? C1B O1B Yb2 142.7(5) . . ? C16B O2B Yb2 128.4(5) . . ? O1 C1 C2 120.1(7) . . ? O1 C1 C6 122.9(7) . . ? C2 C1 C6 116.9(7) . . ? C3 C2 C1 122.1(8) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? C2 C3 C4 120.6(8) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 118.0(7) . . ? C5 C4 H4A 121.0 . . ? C3 C4 H4A 121.0 . . ? C4 C5 C6 122.4(8) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 119.7(7) . . ? C5 C6 C7 117.5(7) . . ? C1 C6 C7 122.8(7) . . ? N1 C7 C6 126.3(7) . . ? N1 C7 H7A 116.8 . . ? C6 C7 H7A 116.8 . . ? N1 C8 C9 109.4(7) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? N2 C9 C8 108.0(6) . . ? N2 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N2 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N2 C10 C11 126.2(7) . . ? N2 C10 H10A 116.9 . . ? C11 C10 H10A 116.9 . . ? C16 C11 C12 119.6(7) . . ? C16 C11 C10 124.7(7) . . ? C12 C11 C10 115.6(7) . . ? C13 C12 C11 120.2(8) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 120.4(8) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 119.9(8) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 122.4(8) . . ? C14 C15 H15A 118.8 . . ? C16 C15 H15A 118.8 . . ? O2 C16 C15 120.7(7) . . ? O2 C16 C11 121.7(7) . . ? C15 C16 C11 117.5(7) . . ? O4 C17 O3 122.8(7) . . ? O4 C17 C18 117.9(7) . . ? O3 C17 C18 119.3(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C19 O5 119.6(7) . . ? O6 C19 C20 120.1(7) . . ? O5 C19 C20 120.3(7) . . ? O6 C19 Yb2 61.1(4) . . ? O5 C19 Yb2 58.6(4) . . ? C20 C19 Yb2 175.6(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O7 C21 H21A 109.5 . . ? O7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1B C1B C2B 121.9(7) . . ? O1B C1B C6B 122.5(7) . . ? C2B C1B C6B 115.6(7) . . ? C3B C2B C1B 123.0(9) . . ? C3B C2B H2BA 118.5 . . ? C1B C2B H2BA 118.5 . . ? C2B C3B C4B 120.7(9) . . ? C2B C3B H3BA 119.7 . . ? C4B C3B H3BA 119.7 . . ? C5B C4B C3B 118.2(8) . . ? C5B C4B H4BA 120.9 . . ? C3B C4B H4BA 120.9 . . ? C4B C5B C6B 122.6(9) . . ? C4B C5B H5BA 118.7 . . ? C6B C5B H5BA 118.7 . . ? C5B C6B C1B 119.8(8) . . ? C5B C6B C7B 117.4(7) . . ? C1B C6B C7B 122.8(7) . . ? N1B C7B C6B 128.6(7) . . ? N1B C7B H7BA 115.7 . . ? C6B C7B H7BA 115.7 . . ? N1B C8B C9B 110.9(7) . . ? N1B C8B H8BA 109.5 . . ? C9B C8B H8BA 109.5 . . ? N1B C8B H8BB 109.5 . . ? C9B C8B H8BB 109.5 . . ? H8BA C8B H8BB 108.1 . . ? N2B C9B C8B 106.7(6) . . ? N2B C9B H9BA 110.4 . . ? C8B C9B H9BA 110.4 . . ? N2B C9B H9BB 110.4 . . ? C8B C9B H9BB 110.4 . . ? H9BA C9B H9BB 108.6 . . ? N2B C10B C11B 125.3(7) . . ? N2B C10B H10B 117.3 . . ? C11B C10B H10B 117.3 . . ? C12B C11B C16B 119.2(7) . . ? C12B C11B C10B 117.5(7) . . ? C16B C11B C10B 123.2(7) . . ? C13B C12B C11B 121.8(8) . . ? C13B C12B H12B 119.1 . . ? C11B C12B H12B 119.1 . . ? C12B C13B C14B 119.2(8) . . ? C12B C13B H13B 120.4 . . ? C14B C13B H13B 120.4 . . ? C15B C14B C13B 120.6(8) . . ? C15B C14B H14B 119.7 . . ? C13B C14B H14B 119.7 . . ? C14B C15B C16B 120.8(8) . . ? C14B C15B H15B 119.6 . . ? C16B C15B H15B 119.6 . . ? O2B C16B C15B 119.7(7) . . ? O2B C16B C11B 122.1(7) . . ? C15B C16B C11B 118.2(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.703 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.283 # Attachment 'Complex-5.CIF' data_Complex-5 _database_code_depnum_ccdc_archive 'CCDC 733185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H48 N4 O18 Tb3, C4 H10 O, C0.5 H2 O0.5' _chemical_formula_sum 'C50.50 H60 N4 O19.50 Tb3' _chemical_formula_weight 1511.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.194(3) _cell_length_b 20.024(4) _cell_length_c 20.223(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.40(3) _cell_angle_gamma 90.00 _cell_volume 5729(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12019 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 3.738 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.6040 _exptl_absorpt_correction_T_max 0.7296 _exptl_absorpt_process_details ; Absorption correction given as Gaussian ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15917 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10058 _reflns_number_gt 8585 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XL SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+5.5780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00041(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10058 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.27113(2) 0.332886(17) 0.387693(17) 0.02103(11) Uani 1 1 d U . . Tb2 Tb 0.13999(2) 0.478147(17) 0.284344(17) 0.02098(11) Uani 1 1 d U . . Tb3 Tb 0.09967(3) 0.642984(19) 0.193441(19) 0.02764(12) Uani 1 1 d U . . N1 N 0.3832(4) 0.2506(3) 0.4690(3) 0.0278(14) Uani 1 1 d U . . N2 N 0.2631(4) 0.3341(3) 0.5099(3) 0.0267(14) Uani 1 1 d U . . N3 N -0.0016(5) 0.6359(4) 0.0652(4) 0.0435(18) Uani 1 1 d U . . N4 N 0.1313(6) 0.7396(4) 0.1259(4) 0.0452(18) Uani 1 1 d U . . O1 O 0.4296(4) 0.2892(3) 0.2217(3) 0.0410(14) Uani 1 1 d U . . O2 O 0.3587(4) 0.2914(3) 0.3299(3) 0.0297(12) Uani 1 1 d U . . O3 O 0.1496(3) 0.4090(2) 0.3843(3) 0.0237(10) Uani 1 1 d U . . O4 O 0.0005(3) 0.4814(2) 0.3260(3) 0.0247(11) Uani 1 1 d U . . O5 O -0.0060(3) 0.4138(3) 0.2077(3) 0.0294(12) Uani 1 1 d U . . O6 O 0.0386(3) 0.5314(3) 0.1756(2) 0.0280(12) Uani 1 1 d U . . O7 O 0.2013(4) 0.7123(3) 0.2704(3) 0.0324(12) Uani 1 1 d U . . O8 O 0.3215(5) 0.7554(3) 0.4039(3) 0.0468(15) Uani 1 1 d U . . O9 O 0.1611(4) 0.2504(3) 0.3764(3) 0.0352(13) Uani 1 1 d U . . O10 O 0.0325(5) 0.1977(4) 0.3113(4) 0.064(2) Uani 1 1 d U . . O11 O 0.1702(4) 0.3514(3) 0.2677(3) 0.0281(11) Uani 1 1 d U . . O12 O 0.1780(4) 0.4243(3) 0.1884(3) 0.0323(12) Uani 1 1 d U . . O13 O 0.3980(4) 0.4124(3) 0.4498(3) 0.0307(12) Uani 1 1 d U . . O14 O 0.2985(3) 0.4423(2) 0.3452(2) 0.0242(11) Uani 1 1 d U . . O15 O 0.1949(4) 0.5515(3) 0.3920(3) 0.0279(11) Uani 1 1 d U . . O16 O 0.0889(3) 0.5977(3) 0.2988(3) 0.0265(11) Uani 1 1 d U . . O17 O 0.2285(3) 0.5603(3) 0.2502(3) 0.0259(11) Uani 1 1 d U . . O18 O 0.2148(4) 0.6012(3) 0.1463(3) 0.0312(12) Uani 1 1 d U . . C1 C 0.4305(8) 0.3601(5) 0.2217(6) 0.054(3) Uani 1 1 d U . . H1A H 0.3949 0.3762 0.1748 0.081 Uiso 1 1 calc R . . H1B H 0.4945 0.3756 0.2360 0.081 Uiso 1 1 calc R . . H1C H 0.4028 0.3764 0.2543 0.081 Uiso 1 1 calc R . . C2 C 0.4794(6) 0.2612(4) 0.2878(4) 0.0338(18) Uani 1 1 d U . . C3 C 0.5652(6) 0.2313(5) 0.2991(5) 0.045(2) Uani 1 1 d U . . H3A H 0.5898 0.2319 0.2631 0.054 Uiso 1 1 calc R . . C4 C 0.6151(7) 0.2009(5) 0.3622(6) 0.052(2) Uani 1 1 d U . . H4A H 0.6730 0.1809 0.3691 0.063 Uiso 1 1 calc R . . C5 C 0.5790(6) 0.1999(5) 0.4159(5) 0.045(2) Uani 1 1 d U . . H5A H 0.6127 0.1792 0.4589 0.054 Uiso 1 1 calc R . . C6 C 0.4912(6) 0.2301(4) 0.4054(4) 0.0344(18) Uani 1 1 d U . . C7 C 0.4396(5) 0.2628(4) 0.3413(4) 0.0299(17) Uani 1 1 d U . . C8 C 0.4581(6) 0.2249(4) 0.4640(5) 0.0357(19) Uani 1 1 d U . . H8A H 0.4957 0.1999 0.5028 0.043 Uiso 1 1 calc R . . C9 C 0.3673(6) 0.2370(4) 0.5342(4) 0.0373(19) Uani 1 1 d U . . H9A H 0.4233 0.2168 0.5687 0.045 Uiso 1 1 calc R . . H9B H 0.3151 0.2061 0.5249 0.045 Uiso 1 1 calc R . . C10 C 0.3450(6) 0.3018(4) 0.5632(4) 0.0329(18) Uani 1 1 d U . . H10A H 0.3316 0.2929 0.6057 0.040 Uiso 1 1 calc R . . H10B H 0.3993 0.3314 0.5758 0.040 Uiso 1 1 calc R . . C11 C 0.1938(6) 0.3500(4) 0.5278(4) 0.0294(17) Uani 1 1 d U . . H11A H 0.1997 0.3389 0.5739 0.035 Uiso 1 1 calc R . . C12 C 0.1068(5) 0.3833(4) 0.4855(4) 0.0267(16) Uani 1 1 d U . . C13 C 0.0357(6) 0.3893(4) 0.5156(4) 0.0317(18) Uani 1 1 d U . . H13A H 0.0460 0.3701 0.5597 0.038 Uiso 1 1 calc R . . C14 C -0.0462(6) 0.4222(4) 0.4820(4) 0.0344(18) Uani 1 1 d U . . H14A H -0.0921 0.4242 0.5023 0.041 Uiso 1 1 calc R . . C15 C -0.0618(5) 0.4528(4) 0.4174(4) 0.0308(17) Uani 1 1 d U . . H15A H -0.1180 0.4757 0.3943 0.037 Uiso 1 1 calc R . . C16 C 0.0063(5) 0.4493(3) 0.3877(4) 0.0225(15) Uani 1 1 d U . . C17 C 0.0907(5) 0.4124(3) 0.4188(4) 0.0210(14) Uani 1 1 d U . . C18 C -0.0864(5) 0.5156(4) 0.2876(4) 0.0315(17) Uani 1 1 d U . . H18A H -0.0970 0.5498 0.3172 0.047 Uiso 1 1 calc R . . H18B H -0.1378 0.4843 0.2745 0.047 Uiso 1 1 calc R . . H18C H -0.0825 0.5355 0.2456 0.047 Uiso 1 1 calc R . . C19 C -0.0383(6) 0.3538(4) 0.2307(4) 0.0352(19) Uani 1 1 d U . . H19A H -0.1061 0.3537 0.2135 0.053 Uiso 1 1 calc R . . H19B H -0.0138 0.3520 0.2816 0.053 Uiso 1 1 calc R . . H19C H -0.0166 0.3156 0.2122 0.053 Uiso 1 1 calc R . . C20 C -0.0547(5) 0.4357(4) 0.1388(4) 0.0314(18) Uani 1 1 d U . . C21 C -0.1252(6) 0.3987(5) 0.0894(5) 0.042(2) Uani 1 1 d U . . H21A H -0.1441 0.3577 0.1013 0.050 Uiso 1 1 calc R . . C22 C -0.1676(7) 0.4251(5) 0.0204(5) 0.048(2) Uani 1 1 d U . . H22A H -0.2163 0.4019 -0.0136 0.058 Uiso 1 1 calc R . . C23 C -0.1378(7) 0.4844(5) 0.0032(5) 0.047(2) Uani 1 1 d U . . H23A H -0.1635 0.4993 -0.0435 0.057 Uiso 1 1 calc R . . C24 C -0.0702(6) 0.5234(4) 0.0531(4) 0.0359(19) Uani 1 1 d U . . C25 C -0.0261(5) 0.4983(4) 0.1235(4) 0.0292(17) Uani 1 1 d U . . C26 C -0.0501(6) 0.5880(5) 0.0292(4) 0.041(2) Uani 1 1 d U . . H26A H -0.0766 0.5953 -0.0195 0.049 Uiso 1 1 calc R . . C27 C -0.0024(7) 0.7015(6) 0.0286(5) 0.055(3) Uani 1 1 d U . . H27A H -0.0291 0.6953 -0.0225 0.066 Uiso 1 1 calc R . . H27B H -0.0417 0.7333 0.0414 0.066 Uiso 1 1 calc R . . C28 C 0.0932(8) 0.7275(5) 0.0492(5) 0.053(3) Uani 1 1 d U . . H28A H 0.0928 0.7688 0.0240 0.064 Uiso 1 1 calc R . . H28B H 0.1328 0.6956 0.0369 0.064 Uiso 1 1 calc R . . C29 C 0.1784(7) 0.7934(5) 0.1474(5) 0.044(2) Uani 1 1 d U . . H29A H 0.1782 0.8235 0.1123 0.053 Uiso 1 1 calc R . . C30 C 0.2316(6) 0.8128(4) 0.2191(5) 0.0335(18) Uani 1 1 d U . . C31 C 0.2746(6) 0.8772(4) 0.2297(5) 0.041(2) Uani 1 1 d U . . H31A H 0.2673 0.9041 0.1906 0.049 Uiso 1 1 calc R . . C32 C 0.3264(7) 0.9001(5) 0.2961(5) 0.048(2) Uani 1 1 d U . . H32A H 0.3507 0.9433 0.3028 0.058 Uiso 1 1 calc R . . C33 C 0.3421(6) 0.8572(4) 0.3537(5) 0.044(2) Uani 1 1 d U . . H33A H 0.3788 0.8717 0.3990 0.053 Uiso 1 1 calc R . . C34 C 0.3043(6) 0.7939(4) 0.3447(5) 0.0376(19) Uani 1 1 d U . . C35 C 0.2443(6) 0.7706(4) 0.2772(5) 0.0332(18) Uani 1 1 d U . . C36 C 0.3695(7) 0.6938(5) 0.4038(6) 0.055(3) Uani 1 1 d U . . H36A H 0.3790 0.6700 0.4471 0.083 Uiso 1 1 calc R . . H36B H 0.4296 0.7030 0.4003 0.083 Uiso 1 1 calc R . . H36C H 0.3320 0.6671 0.3641 0.083 Uiso 1 1 calc R . . C37 C 0.1200(8) 0.2076(5) 0.3318(6) 0.055(3) Uani 1 1 d U . . C38 C 0.1724(14) 0.1728(10) 0.2940(11) 0.124(6) Uani 1 1 d U . . H38A H 0.2381 0.1846 0.3146 0.186 Uiso 1 1 calc R . . H38B H 0.1479 0.1856 0.2448 0.186 Uiso 1 1 calc R . . H38C H 0.1656 0.1254 0.2977 0.186 Uiso 1 1 calc R . . C39 C 0.1807(5) 0.3656(4) 0.2098(4) 0.0308(18) Uani 1 1 d U . . C40 C 0.1949(7) 0.3080(5) 0.1661(5) 0.049(2) Uani 1 1 d U . . H40A H 0.2519 0.2846 0.1929 0.073 Uiso 1 1 calc R . . H40B H 0.1997 0.3250 0.1231 0.073 Uiso 1 1 calc R . . H40C H 0.1421 0.2780 0.1545 0.073 Uiso 1 1 calc R . . C41 C 0.3711(5) 0.4544(4) 0.4019(4) 0.0248(15) Uani 1 1 d U . . C42 C 0.4205(6) 0.5199(4) 0.4073(5) 0.039(2) Uani 1 1 d U . . H42A H 0.4856 0.5152 0.4377 0.058 Uiso 1 1 calc R . . H42B H 0.3908 0.5528 0.4266 0.058 Uiso 1 1 calc R . . H42C H 0.4169 0.5337 0.3609 0.058 Uiso 1 1 calc R . . C43 C 0.1435(5) 0.6006(4) 0.3643(4) 0.0251(16) Uani 1 1 d U . . C44 C 0.1428(6) 0.6637(4) 0.4042(5) 0.0359(19) Uani 1 1 d U . . C45 C 0.2581(5) 0.5656(4) 0.1988(4) 0.0246(15) Uani 1 1 d U . . C46 C 0.3480(6) 0.5305(5) 0.2037(5) 0.041(2) Uani 1 1 d U . . H46A H 0.3354 0.4839 0.1937 0.061 Uiso 1 1 calc R . . H46B H 0.3944 0.5358 0.2506 0.061 Uiso 1 1 calc R . . H46C H 0.3715 0.5495 0.1698 0.061 Uiso 1 1 calc R . . O19 O 0.2906(5) 0.4749(4) 0.6331(4) 0.070(2) Uani 1 1 d U . . C50 C 0.3538(10) 0.4148(7) 0.7389(7) 0.085(4) Uani 1 1 d DU . . H50A H 0.4115 0.4003 0.7752 0.127 Uiso 1 1 calc R . . H50B H 0.3170 0.3765 0.7164 0.127 Uiso 1 1 calc R . . H50C H 0.3185 0.4416 0.7598 0.127 Uiso 1 1 calc R . . C49 C 0.3757(7) 0.4540(6) 0.6865(5) 0.056(3) Uani 1 1 d DU . . H49B H 0.4131 0.4926 0.7091 0.067 Uiso 1 1 calc R . . H49A H 0.4121 0.4273 0.6656 0.067 Uiso 1 1 calc R . . C48 C 0.3079(11) 0.5080(8) 0.5674(8) 0.090(4) Uani 1 1 d U . . H48B H 0.3451 0.4771 0.5515 0.108 Uiso 1 1 calc R . . H48A H 0.2470 0.5124 0.5290 0.108 Uiso 1 1 calc R . . C47 C 0.3562(11) 0.5753(8) 0.5780(8) 0.095(4) Uani 1 1 d U . . H47A H 0.3623 0.5893 0.5345 0.142 Uiso 1 1 calc R . . H47B H 0.4177 0.5720 0.6146 0.142 Uiso 1 1 calc R . . H47C H 0.3191 0.6075 0.5917 0.142 Uiso 1 1 calc R . . O20 O 0.4609(18) 1.0125(15) 0.4731(13) 0.125(8) Uani 0.50 1 d PU . . H20A H 0.5028 0.9970 0.5105 0.187 Uiso 0.50 1 d PR . . C51 C 0.388(2) 1.0388(18) 0.4967(18) 0.105(10) Uani 0.50 1 d PU . . H51C H 0.3379 1.0575 0.4569 0.126 Uiso 0.50 1 calc PR . . H51A H 0.4148 1.0730 0.5316 0.126 Uiso 0.50 1 calc PR . . H51B H 0.3638 1.0035 0.5171 0.126 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02003(19) 0.01803(19) 0.02376(19) 0.00045(13) 0.00650(14) 0.00034(13) Tb2 0.02003(19) 0.0222(2) 0.01975(19) 0.00282(13) 0.00616(14) 0.00057(13) Tb3 0.0293(2) 0.0278(2) 0.0261(2) 0.01005(15) 0.01055(16) 0.00543(15) N1 0.029(3) 0.024(3) 0.029(3) 0.006(3) 0.008(3) 0.005(3) N2 0.030(3) 0.023(3) 0.024(3) 0.002(2) 0.007(3) 0.004(3) N3 0.040(4) 0.048(4) 0.036(4) 0.018(3) 0.005(3) -0.004(3) N4 0.063(5) 0.042(4) 0.031(3) 0.006(3) 0.017(3) -0.001(4) O1 0.045(3) 0.044(3) 0.036(3) -0.005(3) 0.018(3) 0.010(3) O2 0.026(3) 0.034(3) 0.030(3) -0.001(2) 0.011(2) 0.004(2) O3 0.024(2) 0.022(3) 0.026(2) 0.004(2) 0.010(2) 0.005(2) O4 0.024(2) 0.025(3) 0.026(2) 0.004(2) 0.009(2) 0.004(2) O5 0.026(3) 0.033(3) 0.027(3) 0.002(2) 0.006(2) -0.004(2) O6 0.023(3) 0.039(3) 0.017(2) 0.003(2) 0.001(2) 0.002(2) O7 0.041(3) 0.023(3) 0.033(3) 0.001(2) 0.013(2) -0.005(2) O8 0.054(4) 0.028(3) 0.050(3) 0.006(3) 0.009(3) -0.008(3) O9 0.032(3) 0.034(3) 0.035(3) 0.001(2) 0.006(2) -0.012(2) O10 0.053(4) 0.081(5) 0.058(4) -0.014(4) 0.018(3) -0.035(4) O11 0.024(3) 0.030(3) 0.026(3) -0.004(2) 0.004(2) -0.003(2) O12 0.033(3) 0.037(3) 0.029(3) 0.002(2) 0.013(2) 0.001(2) O13 0.032(3) 0.025(3) 0.028(3) 0.003(2) 0.002(2) -0.009(2) O14 0.025(2) 0.025(3) 0.024(2) 0.000(2) 0.009(2) -0.002(2) O15 0.031(3) 0.024(3) 0.027(3) 0.002(2) 0.009(2) 0.002(2) O16 0.028(3) 0.026(3) 0.028(3) 0.008(2) 0.013(2) 0.004(2) O17 0.027(3) 0.026(3) 0.025(2) 0.009(2) 0.011(2) 0.003(2) O18 0.031(3) 0.037(3) 0.028(3) 0.010(2) 0.014(2) 0.003(2) C1 0.061(6) 0.051(5) 0.053(5) 0.011(4) 0.025(4) 0.005(4) C2 0.029(4) 0.036(4) 0.037(4) -0.010(3) 0.013(3) 0.000(3) C3 0.039(4) 0.050(5) 0.052(5) -0.006(4) 0.024(4) 0.004(4) C4 0.043(5) 0.048(5) 0.066(6) -0.001(4) 0.021(4) 0.016(4) C5 0.034(4) 0.050(5) 0.051(5) 0.005(4) 0.013(4) 0.016(4) C6 0.032(4) 0.029(4) 0.040(4) -0.002(3) 0.010(3) 0.003(3) C7 0.028(4) 0.022(4) 0.040(4) -0.003(3) 0.012(3) 0.001(3) C8 0.032(4) 0.028(4) 0.043(4) 0.006(3) 0.008(3) 0.007(3) C9 0.040(4) 0.031(4) 0.040(4) 0.010(3) 0.013(4) 0.005(3) C10 0.037(4) 0.032(4) 0.030(4) 0.006(3) 0.011(3) 0.005(3) C11 0.034(4) 0.030(4) 0.025(4) 0.003(3) 0.011(3) -0.003(3) C12 0.029(4) 0.026(4) 0.028(4) -0.002(3) 0.013(3) -0.002(3) C13 0.036(4) 0.038(4) 0.027(4) 0.003(3) 0.019(3) 0.001(3) C14 0.034(4) 0.040(4) 0.036(4) 0.002(3) 0.022(3) 0.002(3) C15 0.023(4) 0.034(4) 0.034(4) 0.002(3) 0.010(3) 0.005(3) C16 0.029(4) 0.015(3) 0.025(3) -0.002(3) 0.012(3) -0.003(3) C17 0.022(3) 0.020(3) 0.022(3) 0.002(3) 0.009(3) 0.000(3) C18 0.022(4) 0.031(4) 0.036(4) 0.009(3) 0.006(3) 0.008(3) C19 0.033(4) 0.033(4) 0.035(4) 0.000(3) 0.007(3) -0.007(3) C20 0.022(4) 0.039(4) 0.030(4) -0.008(3) 0.005(3) 0.006(3) C21 0.040(4) 0.036(4) 0.044(4) -0.005(4) 0.009(4) -0.004(4) C22 0.047(5) 0.051(5) 0.034(4) -0.009(4) -0.001(4) -0.010(4) C23 0.051(5) 0.050(5) 0.029(4) 0.003(4) 0.001(4) 0.002(4) C24 0.034(4) 0.040(4) 0.028(4) -0.007(3) 0.004(3) 0.004(3) C25 0.026(4) 0.031(4) 0.029(4) 0.000(3) 0.008(3) 0.004(3) C26 0.042(4) 0.050(5) 0.025(4) 0.009(4) 0.006(3) 0.004(4) C27 0.057(5) 0.058(6) 0.036(4) 0.020(4) 0.000(4) -0.010(4) C28 0.068(6) 0.047(5) 0.041(5) 0.013(4) 0.017(4) -0.001(4) C29 0.060(5) 0.033(5) 0.047(5) 0.011(4) 0.028(4) 0.004(4) C30 0.031(4) 0.027(4) 0.048(4) 0.004(3) 0.021(4) 0.004(3) C31 0.048(5) 0.027(4) 0.057(5) 0.010(4) 0.029(4) 0.001(3) C32 0.047(5) 0.035(5) 0.063(5) 0.005(4) 0.020(4) -0.007(4) C33 0.037(4) 0.026(4) 0.060(5) 0.005(4) 0.006(4) -0.004(3) C34 0.035(4) 0.032(4) 0.043(4) 0.001(4) 0.011(4) 0.003(3) C35 0.034(4) 0.022(4) 0.048(4) 0.012(3) 0.020(4) 0.002(3) C36 0.049(5) 0.036(5) 0.061(5) 0.007(4) -0.003(4) -0.004(4) C37 0.061(6) 0.049(5) 0.066(6) -0.021(5) 0.035(5) -0.021(4) C38 0.125(9) 0.114(9) 0.145(10) -0.043(8) 0.063(8) -0.031(7) C39 0.023(4) 0.037(4) 0.029(4) -0.006(3) 0.006(3) 0.000(3) C40 0.052(5) 0.057(5) 0.035(4) -0.009(4) 0.012(4) 0.014(4) C41 0.020(3) 0.029(4) 0.026(3) 0.003(3) 0.009(3) 0.002(3) C42 0.033(4) 0.032(4) 0.040(4) 0.008(3) 0.001(3) -0.002(3) C43 0.026(4) 0.024(4) 0.027(4) 0.004(3) 0.013(3) -0.003(3) C44 0.045(4) 0.030(4) 0.037(4) -0.004(3) 0.020(4) 0.000(3) C45 0.026(3) 0.024(4) 0.025(3) 0.001(3) 0.010(3) -0.003(3) C46 0.034(4) 0.044(5) 0.051(5) 0.011(4) 0.025(4) 0.010(4) O19 0.055(4) 0.076(5) 0.072(5) -0.015(4) 0.014(4) 0.010(4) C50 0.092(7) 0.076(7) 0.088(7) -0.007(6) 0.035(6) -0.001(6) C49 0.048(5) 0.064(6) 0.050(5) -0.003(5) 0.013(4) 0.006(4) C48 0.087(7) 0.116(9) 0.081(7) -0.019(6) 0.046(6) -0.008(7) C47 0.113(8) 0.099(8) 0.091(7) -0.004(6) 0.061(7) 0.023(7) O20 0.127(12) 0.132(12) 0.120(11) -0.006(9) 0.052(9) -0.006(9) C51 0.097(13) 0.100(13) 0.117(13) 0.000(9) 0.039(9) -0.008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O2 2.227(5) . ? Tb1 O9 2.300(5) . ? Tb1 O3 2.376(5) . ? Tb1 O11 2.380(5) . ? Tb1 O14 2.444(5) . ? Tb1 O13 2.462(5) . ? Tb1 N1 2.506(6) . ? Tb1 N2 2.518(6) . ? Tb1 C41 2.826(8) . ? Tb1 Tb2 3.7094(9) . ? Tb2 O14 2.381(5) . ? Tb2 O17 2.380(5) . ? Tb2 O3 2.411(5) . ? Tb2 O6 2.424(5) . ? Tb2 O12 2.465(5) . ? Tb2 O15 2.503(5) . ? Tb2 O5 2.544(5) . ? Tb2 O4 2.552(5) . ? Tb2 O16 2.566(5) . ? Tb2 O11 2.622(5) . ? Tb2 C39 2.901(8) . ? Tb2 C43 2.927(8) . ? Tb3 O7 2.232(5) . ? Tb3 O10 2.259(7) 2 ? Tb3 O16 2.375(5) . ? Tb3 O6 2.395(5) . ? Tb3 O18 2.425(5) . ? Tb3 N3 2.491(7) . ? Tb3 O17 2.500(5) . ? Tb3 N4 2.514(7) . ? Tb3 C45 2.831(7) . ? N1 C8 1.285(10) . ? N1 C9 1.450(10) . ? N2 C11 1.273(10) . ? N2 C10 1.467(10) . ? N3 C26 1.264(12) . ? N3 C27 1.507(12) . ? N4 C29 1.277(12) . ? N4 C28 1.466(12) . ? O1 C2 1.391(10) . ? O1 C1 1.421(12) . ? O2 C7 1.298(9) . ? O3 C17 1.322(8) . ? O4 C16 1.377(8) . ? O4 C18 1.437(9) . ? O5 C20 1.390(9) . ? O5 C19 1.439(10) . ? O6 C25 1.327(9) . ? O7 C35 1.320(9) . ? O8 C34 1.367(11) . ? O8 C36 1.432(12) . ? O9 C37 1.236(11) . ? O10 C37 1.256(12) . ? O10 Tb3 2.259(7) 2_545 ? O11 C39 1.269(10) . ? O12 C39 1.249(10) . ? O13 C41 1.235(9) . ? O14 C41 1.290(9) . ? O15 C43 1.254(9) . ? O16 C43 1.283(9) . ? O17 C45 1.278(9) . ? O18 C45 1.249(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.376(12) . ? C2 C7 1.419(11) . ? C3 C4 1.368(14) . ? C3 H3A 0.9300 . ? C4 C5 1.382(14) . ? C4 H4A 0.9300 . ? C5 C6 1.409(12) . ? C5 H5A 0.9300 . ? C6 C7 1.408(11) . ? C6 C8 1.451(12) . ? C8 H8A 0.9300 . ? C9 C10 1.512(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.448(11) . ? C11 H11A 0.9300 . ? C12 C17 1.407(10) . ? C12 C13 1.425(10) . ? C13 C14 1.352(11) . ? C13 H13A 0.9300 . ? C14 C15 1.382(11) . ? C14 H14A 0.9300 . ? C15 C16 1.376(10) . ? C15 H15A 0.9300 . ? C16 C17 1.414(10) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.383(12) . ? C20 C25 1.398(12) . ? C21 C22 1.410(13) . ? C21 H21A 0.9300 . ? C22 C23 1.360(14) . ? C22 H22A 0.9300 . ? C23 C24 1.387(12) . ? C23 H23A 0.9300 . ? C24 C25 1.425(11) . ? C24 C26 1.453(13) . ? C26 H26A 0.9300 . ? C27 C28 1.454(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.432(13) . ? C29 H29A 0.9300 . ? C30 C35 1.402(11) . ? C30 C31 1.425(12) . ? C31 C32 1.364(14) . ? C31 H31A 0.9300 . ? C32 C33 1.396(13) . ? C32 H32A 0.9300 . ? C33 C34 1.376(12) . ? C33 H33A 0.9300 . ? C34 C35 1.416(12) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.47(2) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.515(12) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.495(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.501(11) . ? C45 C46 1.507(11) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? O19 C49 1.413(12) . ? O19 C48 1.591(16) . ? C50 C49 1.450(15) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C49 H49B 0.9700 . ? C49 H49A 0.9700 . ? C48 C47 1.51(2) . ? C48 H48B 0.9700 . ? C48 H48A 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? O20 O20 1.38(5) 3_676 ? O20 C51 1.45(4) . ? O20 H20A 0.8499 . ? C51 H51C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O9 103.4(2) . . ? O2 Tb1 O3 146.21(18) . . ? O9 Tb1 O3 85.89(19) . . ? O2 Tb1 O11 79.00(18) . . ? O9 Tb1 O11 80.56(19) . . ? O3 Tb1 O11 70.48(17) . . ? O2 Tb1 O14 86.52(18) . . ? O9 Tb1 O14 144.99(18) . . ? O3 Tb1 O14 69.21(16) . . ? O11 Tb1 O14 68.34(17) . . ? O2 Tb1 O13 90.14(19) . . ? O9 Tb1 O13 156.91(18) . . ? O3 Tb1 O13 93.20(18) . . ? O11 Tb1 O13 120.85(17) . . ? O14 Tb1 O13 52.96(16) . . ? O2 Tb1 N1 72.9(2) . . ? O9 Tb1 N1 83.6(2) . . ? O3 Tb1 N1 140.88(18) . . ? O11 Tb1 N1 143.38(19) . . ? O14 Tb1 N1 131.18(19) . . ? O13 Tb1 N1 82.66(19) . . ? O2 Tb1 N2 140.41(19) . . ? O9 Tb1 N2 79.1(2) . . ? O3 Tb1 N2 72.92(18) . . ? O11 Tb1 N2 139.04(19) . . ? O14 Tb1 N2 114.28(18) . . ? O13 Tb1 N2 78.59(19) . . ? N1 Tb1 N2 68.1(2) . . ? O2 Tb1 C41 88.4(2) . . ? O9 Tb1 C41 166.3(2) . . ? O3 Tb1 C41 80.46(19) . . ? O11 Tb1 C41 95.27(19) . . ? O14 Tb1 C41 27.12(18) . . ? O13 Tb1 C41 25.84(19) . . ? N1 Tb1 C41 106.7(2) . . ? N2 Tb1 C41 96.2(2) . . ? O2 Tb1 Tb2 107.33(14) . . ? O9 Tb1 Tb2 106.57(14) . . ? O3 Tb1 Tb2 39.54(11) . . ? O11 Tb1 Tb2 44.72(13) . . ? O14 Tb1 Tb2 39.12(11) . . ? O13 Tb1 Tb2 86.57(12) . . ? N1 Tb1 Tb2 169.23(15) . . ? N2 Tb1 Tb2 109.67(14) . . ? C41 Tb1 Tb2 62.65(14) . . ? O14 Tb2 O17 77.66(17) . . ? O14 Tb2 O3 69.69(16) . . ? O17 Tb2 O3 140.58(17) . . ? O14 Tb2 O6 142.17(17) . . ? O17 Tb2 O6 70.83(17) . . ? O3 Tb2 O6 146.91(17) . . ? O14 Tb2 O12 78.02(17) . . ? O17 Tb2 O12 75.78(18) . . ? O3 Tb2 O12 116.68(17) . . ? O6 Tb2 O12 74.44(18) . . ? O14 Tb2 O15 76.90(17) . . ? O17 Tb2 O15 78.63(17) . . ? O3 Tb2 O15 73.07(17) . . ? O6 Tb2 O15 115.52(17) . . ? O12 Tb2 O15 147.30(17) . . ? O14 Tb2 O5 130.94(17) . . ? O17 Tb2 O5 129.21(16) . . ? O3 Tb2 O5 89.56(17) . . ? O6 Tb2 O5 63.00(17) . . ? O12 Tb2 O5 72.64(17) . . ? O15 Tb2 O5 140.06(17) . . ? O14 Tb2 O4 129.97(16) . . ? O17 Tb2 O4 134.69(16) . . ? O3 Tb2 O4 62.69(15) . . ? O6 Tb2 O4 87.65(16) . . ? O12 Tb2 O4 137.08(17) . . ? O15 Tb2 O4 75.60(16) . . ? O5 Tb2 O4 64.49(16) . . ? O14 Tb2 O16 120.87(17) . . ? O17 Tb2 O16 67.34(16) . . ? O3 Tb2 O16 111.65(16) . . ? O6 Tb2 O16 64.80(17) . . ? O12 Tb2 O16 131.67(17) . . ? O15 Tb2 O16 51.13(16) . . ? O5 Tb2 O16 108.00(17) . . ? O4 Tb2 O16 67.44(16) . . ? O14 Tb2 O11 65.38(16) . . ? O17 Tb2 O11 119.16(17) . . ? O3 Tb2 O11 65.91(16) . . ? O6 Tb2 O11 113.11(17) . . ? O12 Tb2 O11 51.21(17) . . ? O15 Tb2 O11 131.36(16) . . ? O5 Tb2 O11 65.58(16) . . ? O4 Tb2 O11 105.83(16) . . ? O16 Tb2 O11 172.69(16) . . ? O14 Tb2 C39 70.58(19) . . ? O17 Tb2 C39 97.8(2) . . ? O3 Tb2 C39 91.7(2) . . ? O6 Tb2 C39 93.2(2) . . ? O12 Tb2 C39 25.3(2) . . ? O15 Tb2 C39 147.25(19) . . ? O5 Tb2 C39 66.03(19) . . ? O4 Tb2 C39 123.5(2) . . ? O16 Tb2 C39 156.2(2) . . ? O11 Tb2 C39 25.9(2) . . ? O14 Tb2 C43 98.94(19) . . ? O17 Tb2 C43 71.53(18) . . ? O3 Tb2 C43 91.99(18) . . ? O6 Tb2 C43 90.58(19) . . ? O12 Tb2 C43 147.01(19) . . ? O15 Tb2 C43 25.18(18) . . ? O5 Tb2 C43 126.65(19) . . ? O4 Tb2 C43 69.28(18) . . ? O16 Tb2 C43 25.95(18) . . ? O11 Tb2 C43 155.90(18) . . ? C39 Tb2 C43 166.8(2) . . ? O7 Tb3 O10 96.1(3) . 2 ? O7 Tb3 O16 82.47(19) . . ? O10 Tb3 O16 82.7(2) 2 . ? O7 Tb3 O6 144.79(18) . . ? O10 Tb3 O6 99.0(3) 2 . ? O16 Tb3 O6 68.27(17) . . ? O7 Tb3 O18 94.2(2) . . ? O10 Tb3 O18 155.2(2) 2 . ? O16 Tb3 O18 121.07(17) . . ? O6 Tb3 O18 85.07(18) . . ? O7 Tb3 N3 140.3(2) . . ? O10 Tb3 N3 77.4(3) 2 . ? O16 Tb3 N3 133.9(2) . . ? O6 Tb3 N3 74.4(2) . . ? O18 Tb3 N3 80.3(2) . . ? O7 Tb3 O17 82.28(19) . . ? O10 Tb3 O17 151.1(2) 2 . ? O16 Tb3 O17 68.52(16) . . ? O6 Tb3 O17 69.30(16) . . ? O18 Tb3 O17 52.84(16) . . ? N3 Tb3 O17 121.5(2) . . ? O7 Tb3 N4 71.3(2) . . ? O10 Tb3 N4 86.9(3) 2 . ? O16 Tb3 N4 150.5(2) . . ? O6 Tb3 N4 140.9(2) . . ? O18 Tb3 N4 75.2(2) . . ? N3 Tb3 N4 69.3(2) . . ? O17 Tb3 N4 119.1(2) . . ? O7 Tb3 C45 87.2(2) . . ? O10 Tb3 C45 175.8(3) 2 . ? O16 Tb3 C45 95.29(19) . . ? O6 Tb3 C45 76.83(19) . . ? O18 Tb3 C45 26.04(18) . . ? N3 Tb3 C45 101.7(2) . . ? O17 Tb3 C45 26.83(18) . . ? N4 Tb3 C45 96.5(2) . . ? O7 Tb3 Tb2 105.10(14) . . ? O10 Tb3 Tb2 115.8(2) 2 . ? O16 Tb3 Tb2 43.16(12) . . ? O6 Tb3 Tb2 39.79(11) . . ? O18 Tb3 Tb2 82.86(12) . . ? N3 Tb3 Tb2 113.08(18) . . ? O17 Tb3 Tb2 39.19(11) . . ? N4 Tb3 Tb2 157.24(19) . . ? C45 Tb3 Tb2 60.70(14) . . ? C8 N1 C9 116.3(7) . . ? C8 N1 Tb1 128.4(5) . . ? C9 N1 Tb1 114.9(5) . . ? C11 N2 C10 118.0(6) . . ? C11 N2 Tb1 128.6(5) . . ? C10 N2 Tb1 112.6(5) . . ? C26 N3 C27 118.7(7) . . ? C26 N3 Tb3 130.6(6) . . ? C27 N3 Tb3 110.7(6) . . ? C29 N4 C28 117.1(8) . . ? C29 N4 Tb3 131.2(6) . . ? C28 N4 Tb3 111.6(6) . . ? C2 O1 C1 113.7(7) . . ? C7 O2 Tb1 141.3(5) . . ? C17 O3 Tb1 133.4(4) . . ? C17 O3 Tb2 124.5(4) . . ? Tb1 O3 Tb2 101.60(18) . . ? C16 O4 C18 117.0(6) . . ? C16 O4 Tb2 120.0(4) . . ? C18 O4 Tb2 123.0(4) . . ? C20 O5 C19 117.9(6) . . ? C20 O5 Tb2 118.6(5) . . ? C19 O5 Tb2 123.4(4) . . ? C25 O6 Tb3 136.0(5) . . ? C25 O6 Tb2 122.8(5) . . ? Tb3 O6 Tb2 101.00(18) . . ? C35 O7 Tb3 144.4(5) . . ? C34 O8 C36 114.8(8) . . ? C37 O9 Tb1 136.5(6) . . ? C37 O10 Tb3 155.3(8) . 2_545 ? C39 O11 Tb1 136.4(5) . . ? C39 O11 Tb2 89.4(5) . . ? Tb1 O11 Tb2 95.61(17) . . ? C39 O12 Tb2 97.3(5) . . ? C41 O13 Tb1 93.8(4) . . ? C41 O14 Tb2 141.1(5) . . ? C41 O14 Tb1 93.2(4) . . ? Tb2 O14 Tb1 100.50(17) . . ? C43 O15 Tb2 96.7(4) . . ? C43 O16 Tb3 132.8(4) . . ? C43 O16 Tb2 92.9(4) . . ? Tb3 O16 Tb2 97.56(18) . . ? C45 O17 Tb2 134.2(5) . . ? C45 O17 Tb3 91.2(4) . . ? Tb2 O17 Tb3 99.23(17) . . ? C45 O18 Tb3 95.5(4) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 119.0(7) . . ? C3 C2 C7 121.7(8) . . ? O1 C2 C7 119.3(7) . . ? C4 C3 C2 121.1(9) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 119.8(9) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 120.0(9) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 121.1(8) . . ? C7 C6 C8 122.9(7) . . ? C5 C6 C8 116.0(8) . . ? O2 C7 C6 122.8(7) . . ? O2 C7 C2 121.0(7) . . ? C6 C7 C2 116.2(7) . . ? N1 C8 C6 128.0(8) . . ? N1 C8 H8A 116.0 . . ? C6 C8 H8A 116.0 . . ? N1 C9 C10 109.1(7) . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C9 110.1(7) . . ? N2 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? N2 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 128.2(7) . . ? N2 C11 H11A 115.9 . . ? C12 C11 H11A 115.9 . . ? C17 C12 C13 118.7(7) . . ? C17 C12 C11 124.0(7) . . ? C13 C12 C11 117.2(7) . . ? C14 C13 C12 121.9(7) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 120.1(7) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 119.5(7) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? O4 C16 C15 124.2(7) . . ? O4 C16 C17 113.3(6) . . ? C15 C16 C17 122.5(7) . . ? O3 C17 C12 124.7(6) . . ? O3 C17 C16 118.1(6) . . ? C12 C17 C16 117.1(6) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O5 123.0(8) . . ? C21 C20 C25 122.8(8) . . ? O5 C20 C25 114.2(7) . . ? C20 C21 C22 117.8(9) . . ? C20 C21 H21A 121.1 . . ? C22 C21 H21A 121.1 . . ? C23 C22 C21 120.5(8) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 122.1(8) . . ? C22 C23 H23A 118.9 . . ? C24 C23 H23A 118.9 . . ? C23 C24 C25 118.8(8) . . ? C23 C24 C26 116.7(8) . . ? C25 C24 C26 124.5(7) . . ? O6 C25 C20 118.2(7) . . ? O6 C25 C24 124.0(7) . . ? C20 C25 C24 117.7(7) . . ? N3 C26 C24 129.3(8) . . ? N3 C26 H26A 115.3 . . ? C24 C26 H26A 115.3 . . ? C28 C27 N3 110.0(8) . . ? C28 C27 H27A 109.7 . . ? N3 C27 H27A 109.7 . . ? C28 C27 H27B 109.7 . . ? N3 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 N4 109.3(8) . . ? C27 C28 H28A 109.8 . . ? N4 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? N4 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? N4 C29 C30 127.7(8) . . ? N4 C29 H29A 116.1 . . ? C30 C29 H29A 116.1 . . ? C35 C30 C31 120.2(8) . . ? C35 C30 C29 122.6(8) . . ? C31 C30 C29 117.2(8) . . ? C32 C31 C30 121.4(8) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? C31 C32 C33 118.3(9) . . ? C31 C32 H32A 120.8 . . ? C33 C32 H32A 120.8 . . ? C34 C33 C32 121.4(9) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? O8 C34 C33 117.9(8) . . ? O8 C34 C35 120.7(7) . . ? C33 C34 C35 121.4(8) . . ? O7 C35 C30 122.2(8) . . ? O7 C35 C34 120.8(7) . . ? C30 C35 C34 117.0(7) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O9 C37 O10 122.8(10) . . ? O9 C37 C38 119.0(11) . . ? O10 C37 C38 117.7(11) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O12 C39 O11 122.0(7) . . ? O12 C39 C40 120.5(8) . . ? O11 C39 C40 117.5(8) . . ? O12 C39 Tb2 57.4(4) . . ? O11 C39 Tb2 64.7(4) . . ? C40 C39 Tb2 175.5(6) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O13 C41 O14 120.1(7) . . ? O13 C41 C42 121.7(7) . . ? O14 C41 C42 118.2(6) . . ? O13 C41 Tb1 60.4(4) . . ? O14 C41 Tb1 59.7(4) . . ? C42 C41 Tb1 177.7(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O15 C43 O16 119.3(7) . . ? O15 C43 C44 123.1(7) . . ? O16 C43 C44 117.7(7) . . ? O15 C43 Tb2 58.2(4) . . ? O16 C43 Tb2 61.1(4) . . ? C44 C43 Tb2 178.6(6) . . ? O18 C45 O17 120.4(7) . . ? O18 C45 C46 120.4(7) . . ? O17 C45 C46 119.2(7) . . ? O18 C45 Tb3 58.5(4) . . ? O17 C45 Tb3 62.0(4) . . ? C46 C45 Tb3 174.4(6) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 O19 C48 112.3(9) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O19 C49 C50 109.3(10) . . ? O19 C49 H49B 109.8 . . ? C50 C49 H49B 109.8 . . ? O19 C49 H49A 109.8 . . ? C50 C49 H49A 109.8 . . ? H49B C49 H49A 108.3 . . ? C47 C48 O19 118.2(11) . . ? C47 C48 H48B 107.8 . . ? O19 C48 H48B 107.8 . . ? C47 C48 H48A 107.8 . . ? O19 C48 H48A 107.8 . . ? H48B C48 H48A 107.1 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O20 O20 C51 114(3) 3_676 . ? O20 O20 H20A 10.1 3_676 . ? C51 O20 H20A 104.5 . . ? O20 C51 H51C 109.5 . . ? O20 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? O20 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.066 _refine_diff_density_min -3.993 _refine_diff_density_rms 0.193