# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bin Zhao' _publ_contact_author_email zhaobin@nankai.edu.cn _publ_author_name 'Bin Zhao' data_1 _database_code_depnum_ccdc_archive 'CCDC 905407' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 O27 Pr2 S3' _chemical_formula_weight 1386.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3379(6) _cell_length_b 15.7099(14) _cell_length_c 22.4311(12) _cell_angle_alpha 102.474(6) _cell_angle_beta 101.713(5) _cell_angle_gamma 104.905(7) _cell_volume 2986.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5270 _cell_measurement_theta_min 2.4149 _cell_measurement_theta_max 29.1515 _exptl_crystal_description needle _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7153 _exptl_absorpt_correction_T_max 0.7153 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20345 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10511 _reflns_number_gt 7301 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10511 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.031 _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 Pr1 Pr -0.02254(4) 0.63810(2) 0.698100(16) 0.02359(11) Uani 1 1 d . . . Pr2 Pr 0.46403(4) 0.58747(2) 0.642491(16) 0.02222(11) Uani 1 1 d . . . S1 S 0.2776(3) 0.65044(17) 1.03212(9) 0.0522(6) Uani 1 1 d . . . S2 S 0.4258(2) 1.12782(14) 0.59534(10) 0.0455(5) Uani 1 1 d . . . S3 S 1.0215(2) 1.15632(14) 0.77185(10) 0.0464(5) Uani 1 1 d . . . C1 C 0.3261(8) 0.6244(4) 0.7780(3) 0.0263(16) Uani 1 1 d . . . C2 C 0.4079(7) 0.6237(4) 0.8422(3) 0.0258(16) Uani 1 1 d . . . C3 C 0.3277(7) 0.6021(5) 0.8851(3) 0.0308(17) Uani 1 1 d . . . H3 H 0.2212 0.5887 0.8744 0.037 Uiso 1 1 calc R . . C4 C 0.4060(9) 0.6005(5) 0.9443(3) 0.0384(19) Uani 1 1 d . . . C5 C 0.5666(9) 0.6253(5) 0.9636(3) 0.045(2) Uani 1 1 d . . . C6 C 0.6458(8) 0.6486(5) 0.9202(3) 0.042(2) Uani 1 1 d . . . H6 H 0.7527 0.6649 0.9315 0.051 Uiso 1 1 calc R . . C7 C 0.5688(8) 0.6479(5) 0.8611(3) 0.0379(19) Uani 1 1 d . . . H7 H 0.6246 0.6639 0.8330 0.045 Uiso 1 1 calc R . . C8 C 0.7910(10) 0.6483(7) 1.0449(4) 0.088(3) Uani 1 1 d . . . H8A H 0.8289 0.6139 1.0144 0.132 Uiso 1 1 calc R . . H8B H 0.8195 0.6356 1.0848 0.132 Uiso 1 1 calc R . . H8C H 0.8349 0.7127 1.0502 0.132 Uiso 1 1 calc R . . C9 C 0.2923(9) 0.6059(5) 1.0982(3) 0.0382(19) Uani 1 1 d . . . C10 C 0.1565(9) 0.5573(6) 1.1083(3) 0.051(2) Uani 1 1 d . . . H10 H 0.0606 0.5469 1.0808 0.061 Uiso 1 1 calc R . . C11 C 0.1718(8) 0.5248(5) 1.1619(3) 0.0384(19) Uani 1 1 d . . . H11 H 0.0833 0.4931 1.1705 0.046 Uiso 1 1 calc R . . C12 C 0.3117(7) 0.5378(5) 1.2018(3) 0.0268(16) Uani 1 1 d . . . C13 C 0.4436(8) 0.5858(5) 1.1902(3) 0.039(2) Uani 1 1 d . . . H13 H 0.5395 0.5955 1.2173 0.047 Uiso 1 1 calc R . . C14 C 0.4334(8) 0.6199(6) 1.1377(3) 0.048(2) Uani 1 1 d . . . H14 H 0.5225 0.6520 1.1296 0.057 Uiso 1 1 calc R . . C15 C 0.3252(7) 0.5013(4) 1.2584(3) 0.0231(15) Uani 1 1 d . . . C16 C 0.2873(7) 0.7585(5) 0.6457(3) 0.0267(16) Uani 1 1 d . . . C17 C 0.3189(7) 0.8500(5) 0.6323(3) 0.0274(16) Uani 1 1 d . . . C18 C 0.4352(8) 0.8775(5) 0.6041(3) 0.0385(19) Uani 1 1 d . . . H18 H 0.4909 0.8384 0.5925 0.046 Uiso 1 1 calc R . . C19 C 0.4682(8) 0.9618(5) 0.5932(3) 0.0362(18) Uani 1 1 d . . . H19 H 0.5463 0.9798 0.5742 0.043 Uiso 1 1 calc R . . C20 C 0.3857(8) 1.0208(5) 0.6102(3) 0.0358(18) Uani 1 1 d . . . C21 C 0.2707(9) 0.9941(5) 0.6387(4) 0.051(2) Uani 1 1 d . . . H21 H 0.2158 1.0335 0.6508 0.061 Uiso 1 1 calc R . . C22 C 0.2372(8) 0.9087(5) 0.6493(3) 0.042(2) Uani 1 1 d . . . H22 H 0.1588 0.8906 0.6681 0.050 Uiso 1 1 calc R . . C23 C 0.2151(9) 1.1628(5) 0.5180(3) 0.0393(19) Uani 1 1 d . . . C24 C 0.2722(8) 1.2218(5) 0.4861(3) 0.0369(19) Uani 1 1 d . . . H24 H 0.3655 1.2243 0.4768 0.044 Uiso 1 1 calc R . . C25 C 0.1908(7) 1.2782(5) 0.4676(3) 0.0260(16) Uani 1 1 d . . . C26 C 0.0522(7) 1.2740(5) 0.4826(3) 0.0368(19) Uani 1 1 d . . . H26 H -0.0032 1.3117 0.4703 0.044 Uiso 1 1 calc R . . C27 C -0.0038(8) 1.2144(6) 0.5156(3) 0.045(2) Uani 1 1 d . . . H27 H -0.0960 1.2125 0.5258 0.054 Uiso 1 1 calc R . . C28 C 0.0773(9) 1.1574(5) 0.5336(3) 0.044(2) Uani 1 1 d . . . C29 C -0.1198(10) 1.0840(7) 0.5774(4) 0.100(4) Uani 1 1 d . . . H29A H -0.1974 1.0716 0.5385 0.149 Uiso 1 1 calc R . . H29B H -0.1169 1.1393 0.6067 0.149 Uiso 1 1 calc R . . H29C H -0.1437 1.0337 0.5954 0.149 Uiso 1 1 calc R . . C30 C 0.2523(9) 1.3404(5) 0.4305(3) 0.0327(17) Uani 1 1 d . . . C31 C 0.7987(8) 0.7753(4) 0.7118(3) 0.0290(17) Uani 1 1 d . . . C32 C 0.7452(7) 0.8572(5) 0.7281(3) 0.0294(16) Uani 1 1 d . . . C33 C 0.6259(8) 0.8568(5) 0.7567(3) 0.0365(18) Uani 1 1 d . . . H33 H 0.5724 0.8030 0.7640 0.044 Uiso 1 1 calc R . . C34 C 0.5865(8) 0.9350(5) 0.7741(3) 0.0394(19) Uani 1 1 d . . . H34 H 0.5078 0.9342 0.7938 0.047 Uiso 1 1 calc R . . C35 C 0.6635(8) 1.0150(5) 0.7626(3) 0.0359(18) Uani 1 1 d . . . C36 C 0.7817(7) 1.0146(4) 0.7347(3) 0.0297(16) Uani 1 1 d . . . C37 C 0.8245(7) 0.9378(4) 0.7174(3) 0.0313(17) Uani 1 1 d . . . H37 H 0.9053 0.9396 0.6988 0.038 Uiso 1 1 calc R . . C38 C 0.5169(10) 1.1035(6) 0.8068(4) 0.077(3) Uani 1 1 d . . . H38A H 0.4183 1.0637 0.7796 0.115 Uiso 1 1 calc R . . H38B H 0.5159 1.1659 0.8163 0.115 Uiso 1 1 calc R . . H38C H 0.5382 1.0865 0.8455 0.115 Uiso 1 1 calc R . . C39 C 1.0522(8) 1.2476(5) 0.7387(3) 0.0356(18) Uani 1 1 d . . . C40 C 1.1676(8) 1.2634(5) 0.7088(3) 0.0399(19) Uani 1 1 d . . . H40 H 1.2340 1.2282 0.7092 0.048 Uiso 1 1 calc R . . C41 C 1.1840(7) 1.3305(5) 0.6787(3) 0.0303(17) Uani 1 1 d . . . H41 H 1.2607 1.3407 0.6579 0.036 Uiso 1 1 calc R . . C42 C 1.0855(7) 1.3837(4) 0.6792(3) 0.0258(16) Uani 1 1 d . . . C43 C 0.9711(8) 1.3682(5) 0.7109(3) 0.043(2) Uani 1 1 d . . . H43 H 0.9053 1.4037 0.7116 0.052 Uiso 1 1 calc R . . C44 C 0.9566(9) 1.3004(5) 0.7408(4) 0.050(2) Uani 1 1 d . . . H44 H 0.8817 1.2903 0.7625 0.060 Uiso 1 1 calc R . . C45 C 1.0988(7) 1.4589(5) 0.6449(3) 0.0281(17) Uani 1 1 d . . . O1 O 0.0499(7) 0.7371(4) 0.8111(2) 0.0721(19) Uani 1 1 d . . . H1A H 0.1296 0.7924 0.8193 0.108 Uiso 1 1 d R . . H1B H -0.0319 0.7549 0.8225 0.108 Uiso 1 1 d R . . O2 O 0.1826(5) 0.6091(3) 0.7657(2) 0.0402(13) Uani 1 1 d . . . O3 O 0.4049(5) 0.6404(3) 0.7392(2) 0.0358(12) Uani 1 1 d . . . O4 O 0.1903(5) 0.7395(3) 0.6764(2) 0.0453(14) Uani 1 1 d . . . O5 O 0.6276(6) 0.6227(4) 1.0230(2) 0.0597(17) Uani 1 1 d . . . O6 O 0.3229(6) 0.5745(4) 0.9863(2) 0.0524(15) Uani 1 1 d . . . O7 O 0.3937(7) 0.7369(4) 1.0473(2) 0.0657(18) Uani 1 1 d . . . O8 O 0.1206(7) 0.6418(5) 1.0052(3) 0.087(2) Uani 1 1 d . . . O9 O 0.4519(5) 0.5038(3) 1.2887(2) 0.0372(12) Uani 1 1 d . . . O10 O 0.2003(5) 0.4690(3) 1.2721(2) 0.0374(12) Uani 1 1 d . . . O11 O 0.5014(6) 0.4490(3) 0.5746(2) 0.0526(15) Uani 1 1 d . . . H11A H 0.5692 0.4324 0.5969 0.079 Uiso 1 1 d R . . H11B H 0.4164 0.4048 0.5607 0.079 Uiso 1 1 d R . . O12 O 0.3096(6) 0.5519(3) 0.5243(2) 0.0495(14) Uani 1 1 d . . . H12A H 0.2108 0.5457 0.5206 0.074 Uiso 1 1 d R . . H12B H 0.3470 0.5969 0.5084 0.074 Uiso 1 1 d R . . O13 O 0.7179(5) 0.6954(3) 0.7110(2) 0.0345(12) Uani 1 1 d . . . O14 O 0.3595(5) 0.7082(3) 0.6258(2) 0.0357(12) Uani 1 1 d . . . O15 O 0.5659(7) 1.1494(4) 0.5788(3) 0.080(2) Uani 1 1 d . . . O16 O 0.4031(6) 1.1949(3) 0.6428(2) 0.0490(14) Uani 1 1 d . . . O17 O 0.2891(7) 1.1001(4) 0.5322(2) 0.0644(17) Uani 1 1 d . . . O18 O 0.0295(7) 1.0953(4) 0.5645(2) 0.0700(19) Uani 1 1 d . . . O19 O 0.3833(6) 1.3455(4) 0.4237(2) 0.0595(17) Uani 1 1 d . . . O20 O 0.1689(5) 1.3849(3) 0.4076(2) 0.0400(13) Uani 1 1 d . . . O21 O 0.9270(5) 0.7867(3) 0.6995(2) 0.0482(14) Uani 1 1 d . . . O22 O 0.6319(6) 1.0952(4) 0.7759(3) 0.0580(16) Uani 1 1 d . . . O23 O 0.8612(5) 1.0950(3) 0.7221(2) 0.0363(12) Uani 1 1 d . . . O24 O 0.9959(7) 1.1823(4) 0.8320(2) 0.0694(18) Uani 1 1 d . . . O25 O 1.1330(6) 1.1107(4) 0.7645(3) 0.0735(19) Uani 1 1 d . . . O26 O 1.2177(5) 1.4802(3) 0.6263(2) 0.0347(12) Uani 1 1 d . . . O27 O 0.9923(5) 1.4925(3) 0.6363(2) 0.0311(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0243(2) 0.0227(2) 0.0295(2) 0.01317(18) 0.00989(17) 0.01025(16) Pr2 0.0235(2) 0.0213(2) 0.0273(2) 0.01275(17) 0.01096(16) 0.00818(16) S1 0.0698(16) 0.0711(18) 0.0377(12) 0.0341(12) 0.0240(11) 0.0365(13) S2 0.0622(15) 0.0323(12) 0.0649(14) 0.0328(11) 0.0341(12) 0.0245(10) S3 0.0501(13) 0.0291(12) 0.0556(14) 0.0238(11) 0.0022(10) 0.0051(9) C1 0.036(4) 0.022(4) 0.025(4) 0.010(3) 0.008(3) 0.015(3) C2 0.030(4) 0.024(4) 0.027(4) 0.009(3) 0.012(3) 0.011(3) C3 0.025(4) 0.041(5) 0.031(4) 0.013(4) 0.010(3) 0.012(3) C4 0.052(5) 0.037(5) 0.030(4) 0.014(4) 0.016(4) 0.014(4) C5 0.048(5) 0.049(6) 0.038(5) 0.009(4) -0.001(4) 0.026(4) C6 0.034(5) 0.050(5) 0.035(4) 0.006(4) 0.004(4) 0.008(4) C7 0.038(5) 0.042(5) 0.038(4) 0.014(4) 0.017(4) 0.013(4) C8 0.086(8) 0.099(9) 0.050(6) 0.009(6) -0.032(5) 0.029(6) C9 0.053(5) 0.052(5) 0.027(4) 0.026(4) 0.022(4) 0.025(4) C10 0.041(5) 0.090(7) 0.030(4) 0.024(5) 0.009(4) 0.031(5) C11 0.034(5) 0.051(5) 0.040(4) 0.024(4) 0.017(4) 0.016(4) C12 0.030(4) 0.032(4) 0.022(4) 0.006(3) 0.010(3) 0.014(3) C13 0.028(4) 0.055(5) 0.030(4) 0.025(4) 0.002(3) 0.002(3) C14 0.033(5) 0.068(6) 0.045(5) 0.033(5) 0.012(4) 0.006(4) C15 0.027(4) 0.019(4) 0.027(4) 0.008(3) 0.009(3) 0.010(3) C16 0.029(4) 0.031(4) 0.024(4) 0.016(3) 0.003(3) 0.014(3) C17 0.030(4) 0.026(4) 0.033(4) 0.015(3) 0.015(3) 0.011(3) C18 0.038(5) 0.035(5) 0.060(5) 0.025(4) 0.021(4) 0.024(3) C19 0.031(4) 0.035(5) 0.057(5) 0.026(4) 0.024(4) 0.014(3) C20 0.047(5) 0.028(4) 0.045(5) 0.021(4) 0.024(4) 0.016(3) C21 0.062(6) 0.041(5) 0.079(6) 0.034(5) 0.043(5) 0.035(4) C22 0.053(5) 0.038(5) 0.058(5) 0.029(4) 0.035(4) 0.025(4) C23 0.062(6) 0.033(5) 0.037(4) 0.021(4) 0.022(4) 0.024(4) C24 0.041(5) 0.044(5) 0.049(5) 0.027(4) 0.029(4) 0.028(4) C25 0.031(4) 0.027(4) 0.026(4) 0.013(3) 0.011(3) 0.013(3) C26 0.023(4) 0.051(5) 0.034(4) 0.015(4) 0.002(3) 0.011(3) C27 0.026(4) 0.067(6) 0.046(5) 0.025(5) 0.019(4) 0.008(4) C28 0.062(6) 0.037(5) 0.022(4) 0.016(4) 0.007(4) -0.004(4) C29 0.085(8) 0.119(10) 0.058(6) 0.035(6) 0.027(6) -0.044(7) C30 0.044(5) 0.026(4) 0.026(4) 0.014(3) 0.004(3) 0.006(3) C31 0.034(4) 0.017(4) 0.035(4) 0.007(3) 0.009(3) 0.008(3) C32 0.025(4) 0.023(4) 0.040(4) 0.010(3) 0.008(3) 0.007(3) C33 0.037(4) 0.030(5) 0.039(4) 0.010(4) 0.007(3) 0.008(3) C34 0.030(4) 0.029(5) 0.060(5) 0.008(4) 0.016(4) 0.011(3) C35 0.029(4) 0.027(4) 0.051(5) 0.009(4) 0.005(4) 0.013(3) C36 0.035(4) 0.018(4) 0.035(4) 0.012(3) 0.008(3) 0.007(3) C37 0.035(4) 0.022(4) 0.039(4) 0.011(3) 0.017(3) 0.007(3) C38 0.085(8) 0.047(6) 0.101(8) 0.006(6) 0.029(6) 0.036(5) C39 0.045(5) 0.018(4) 0.041(4) 0.011(3) 0.008(4) 0.008(3) C40 0.039(5) 0.027(4) 0.065(5) 0.023(4) 0.011(4) 0.021(3) C41 0.022(4) 0.028(4) 0.048(4) 0.013(4) 0.015(3) 0.014(3) C42 0.022(4) 0.020(4) 0.035(4) 0.009(3) 0.010(3) 0.004(3) C43 0.050(5) 0.032(5) 0.071(6) 0.027(4) 0.037(4) 0.026(4) C44 0.060(6) 0.045(5) 0.075(6) 0.041(5) 0.042(5) 0.030(4) C45 0.026(4) 0.024(4) 0.026(4) 0.000(3) 0.003(3) 0.003(3) O1 0.074(4) 0.080(5) 0.058(4) -0.008(3) 0.005(3) 0.049(4) O2 0.030(3) 0.054(4) 0.041(3) 0.023(3) 0.007(2) 0.015(2) O3 0.042(3) 0.045(3) 0.027(3) 0.012(2) 0.015(2) 0.018(2) O4 0.037(3) 0.045(3) 0.084(4) 0.048(3) 0.038(3) 0.022(2) O5 0.069(4) 0.078(5) 0.030(3) 0.014(3) -0.005(3) 0.036(3) O6 0.080(4) 0.048(4) 0.033(3) 0.018(3) 0.023(3) 0.015(3) O7 0.119(5) 0.053(4) 0.044(3) 0.026(3) 0.040(3) 0.035(4) O8 0.077(5) 0.148(7) 0.078(4) 0.073(5) 0.026(4) 0.068(5) O9 0.036(3) 0.043(3) 0.042(3) 0.024(3) 0.008(2) 0.019(2) O10 0.037(3) 0.043(3) 0.053(3) 0.033(3) 0.025(2) 0.022(2) O11 0.060(4) 0.045(4) 0.055(4) 0.010(3) 0.013(3) 0.027(3) O12 0.061(4) 0.046(4) 0.039(3) 0.015(3) 0.011(3) 0.012(3) O13 0.041(3) 0.024(3) 0.039(3) 0.011(2) 0.012(2) 0.008(2) O14 0.048(3) 0.031(3) 0.043(3) 0.018(2) 0.021(2) 0.024(2) O15 0.084(5) 0.059(4) 0.145(6) 0.066(4) 0.074(5) 0.038(4) O16 0.060(4) 0.035(3) 0.055(3) 0.014(3) 0.013(3) 0.020(3) O17 0.118(5) 0.047(4) 0.046(4) 0.026(3) 0.020(3) 0.048(4) O18 0.089(5) 0.063(5) 0.050(4) 0.035(3) 0.022(3) -0.006(3) O19 0.037(3) 0.093(5) 0.070(4) 0.060(4) 0.026(3) 0.017(3) O20 0.048(3) 0.037(3) 0.039(3) 0.023(3) 0.003(2) 0.015(2) O21 0.027(3) 0.039(3) 0.085(4) 0.020(3) 0.024(3) 0.011(2) O22 0.056(4) 0.032(3) 0.094(5) 0.014(3) 0.027(3) 0.027(3) O23 0.046(3) 0.022(3) 0.043(3) 0.019(2) 0.007(2) 0.009(2) O24 0.097(5) 0.041(4) 0.046(4) 0.015(3) -0.002(3) -0.005(3) O25 0.055(4) 0.058(4) 0.128(5) 0.062(4) 0.018(4) 0.030(3) O26 0.023(3) 0.033(3) 0.048(3) 0.015(2) 0.015(2) 0.001(2) O27 0.036(3) 0.025(3) 0.043(3) 0.016(2) 0.014(2) 0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O10 2.352(4) 2_567 ? Pr1 O20 2.383(5) 2_576 ? Pr1 O2 2.397(5) . ? Pr1 O4 2.414(4) . ? Pr1 O27 2.458(4) 1_445 ? Pr1 O21 2.492(5) 1_455 ? Pr1 O1 2.523(5) . ? Pr1 O13 2.840(4) 1_455 ? Pr1 C31 3.049(7) 1_455 ? Pr2 O3 2.376(4) . ? Pr2 O26 2.381(4) 1_445 ? Pr2 O14 2.409(5) . ? Pr2 O9 2.469(5) 2_667 ? Pr2 O19 2.472(5) 2_676 ? Pr2 O13 2.487(4) . ? Pr2 O11 2.519(4) . ? Pr2 O12 2.609(5) . ? S1 O7 1.424(6) . ? S1 O8 1.427(6) . ? S1 O6 1.601(5) . ? S1 C9 1.767(7) . ? S2 O15 1.410(5) . ? S2 O16 1.418(5) . ? S2 O17 1.593(6) . ? S2 C20 1.745(7) . ? S3 O24 1.410(5) . ? S3 O25 1.424(6) . ? S3 O23 1.591(5) . ? S3 C39 1.740(7) . ? C1 O2 1.260(7) . ? C1 O3 1.273(7) . ? C1 C2 1.490(9) . ? C2 C3 1.381(8) . ? C2 C7 1.400(9) . ? C3 C4 1.389(9) . ? C4 C5 1.397(9) . ? C4 O6 1.398(7) . ? C5 O5 1.353(8) . ? C5 C6 1.391(9) . ? C6 C7 1.370(9) . ? C8 O5 1.424(9) . ? C9 C14 1.365(9) . ? C9 C10 1.391(9) . ? C10 C11 1.400(10) . ? C11 C12 1.364(9) . ? C12 C13 1.375(8) . ? C12 C15 1.498(9) . ? C13 C14 1.389(9) . ? C15 O9 1.225(7) . ? C15 O10 1.273(7) . ? C16 O14 1.233(7) . ? C16 O4 1.260(7) . ? C16 C17 1.498(9) . ? C17 C22 1.381(9) . ? C17 C18 1.386(8) . ? C18 C19 1.368(9) . ? C19 C20 1.390(9) . ? C20 C21 1.379(9) . ? C21 C22 1.380(10) . ? C23 C24 1.357(9) . ? C23 C28 1.387(10) . ? C23 O17 1.396(9) . ? C24 C25 1.382(9) . ? C25 C26 1.391(8) . ? C25 C30 1.495(9) . ? C26 C27 1.379(9) . ? C27 C28 1.385(11) . ? C28 O18 1.351(8) . ? C29 O18 1.454(9) . ? C30 O19 1.247(8) . ? C30 O20 1.279(8) . ? C31 O21 1.260(7) . ? C31 O13 1.281(7) . ? C31 C32 1.496(9) . ? C31 Pr1 3.049(7) 1_655 ? C32 C37 1.390(9) . ? C32 C33 1.393(8) . ? C33 C34 1.371(9) . ? C34 C35 1.383(10) . ? C35 O22 1.353(8) . ? C35 C36 1.376(9) . ? C36 C37 1.370(9) . ? C36 O23 1.408(7) . ? C38 O22 1.409(8) . ? C39 C44 1.367(10) . ? C39 C40 1.378(9) . ? C40 C41 1.363(9) . ? C41 C42 1.394(9) . ? C42 C43 1.398(8) . ? C42 C45 1.536(9) . ? C43 C44 1.369(10) . ? C45 O27 1.242(8) . ? C45 O26 1.255(7) . ? O9 Pr2 2.469(5) 2_667 ? O10 Pr1 2.352(4) 2_567 ? O13 Pr1 2.840(4) 1_655 ? O19 Pr2 2.472(4) 2_676 ? O20 Pr1 2.383(5) 2_576 ? O21 Pr1 2.492(5) 1_655 ? O26 Pr2 2.381(4) 1_665 ? O27 Pr1 2.458(4) 1_665 ? 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 O10 Pr1 O20 99.00(16) 2_567 2_576 ? O10 Pr1 O2 88.92(16) 2_567 . ? O20 Pr1 O2 147.24(16) 2_576 . ? O10 Pr1 O4 170.91(16) 2_567 . ? O20 Pr1 O4 87.95(17) 2_576 . ? O2 Pr1 O4 82.10(16) . . ? O10 Pr1 O27 78.85(15) 2_567 1_445 ? O20 Pr1 O27 74.80(16) 2_576 1_445 ? O2 Pr1 O27 75.68(15) . 1_445 ? O4 Pr1 O27 97.50(15) . 1_445 ? O10 Pr1 O21 116.14(15) 2_567 1_455 ? O20 Pr1 O21 75.57(17) 2_576 1_455 ? O2 Pr1 O21 128.91(17) . 1_455 ? O4 Pr1 O21 71.16(15) . 1_455 ? O27 Pr1 O21 148.58(16) 1_445 1_455 ? O10 Pr1 O1 86.43(18) 2_567 . ? O20 Pr1 O1 144.01(18) 2_576 . ? O2 Pr1 O1 67.73(17) . . ? O4 Pr1 O1 91.39(19) . . ? O27 Pr1 O1 140.70(17) 1_445 . ? O21 Pr1 O1 70.23(18) 1_455 . ? O10 Pr1 O13 68.61(14) 2_567 1_455 ? O20 Pr1 O13 74.67(14) 2_576 1_455 ? O2 Pr1 O13 136.95(14) . 1_455 ? O4 Pr1 O13 119.26(15) . 1_455 ? O27 Pr1 O13 130.48(14) 1_445 1_455 ? O21 Pr1 O13 48.28(13) 1_455 1_455 ? O1 Pr1 O13 74.41(15) . 1_455 ? O10 Pr1 C31 92.57(17) 2_567 1_455 ? O20 Pr1 C31 75.80(17) 2_576 1_455 ? O2 Pr1 C31 135.92(17) . 1_455 ? O4 Pr1 C31 94.82(17) . 1_455 ? O27 Pr1 C31 147.57(16) 1_445 1_455 ? O21 Pr1 C31 23.66(14) 1_455 1_455 ? O1 Pr1 C31 68.41(18) . 1_455 ? O13 Pr1 C31 24.79(14) 1_455 1_455 ? O3 Pr2 O26 78.14(15) . 1_445 ? O3 Pr2 O14 76.40(16) . . ? O26 Pr2 O14 93.53(16) 1_445 . ? O3 Pr2 O9 74.42(15) . 2_667 ? O26 Pr2 O9 82.44(16) 1_445 2_667 ? O14 Pr2 O9 150.76(15) . 2_667 ? O3 Pr2 O19 137.23(18) . 2_676 ? O26 Pr2 O19 137.26(17) 1_445 2_676 ? O14 Pr2 O19 78.00(17) . 2_676 ? O9 Pr2 O19 123.74(16) 2_667 2_676 ? O3 Pr2 O13 78.02(14) . . ? O26 Pr2 O13 152.54(15) 1_445 . ? O14 Pr2 O13 93.93(16) . . ? O9 Pr2 O13 78.20(16) 2_667 . ? O19 Pr2 O13 70.19(16) 2_676 . ? O3 Pr2 O11 142.03(17) . . ? O26 Pr2 O11 81.65(16) 1_445 . ? O14 Pr2 O11 137.02(16) . . ? O9 Pr2 O11 71.28(16) 2_667 . ? O19 Pr2 O11 77.31(18) 2_676 . ? O13 Pr2 O11 109.81(16) . . ? O3 Pr2 O12 131.57(16) . . ? O26 Pr2 O12 72.08(16) 1_445 . ? O14 Pr2 O12 68.45(16) . . ? O9 Pr2 O12 135.56(16) 2_667 . ? O19 Pr2 O12 65.82(17) 2_676 . ? O13 Pr2 O12 134.99(15) . . ? O11 Pr2 O12 69.48(17) . . ? O7 S1 O8 119.7(4) . . ? O7 S1 O6 109.0(3) . . ? O8 S1 O6 108.2(4) . . ? O7 S1 C9 110.2(4) . . ? O8 S1 C9 109.7(4) . . ? O6 S1 C9 97.8(3) . . ? O15 S2 O16 118.1(4) . . ? O15 S2 O17 107.8(4) . . ? O16 S2 O17 109.1(3) . . ? O15 S2 C20 110.4(3) . . ? O16 S2 C20 111.9(3) . . ? O17 S2 C20 97.4(3) . . ? O24 S3 O25 119.4(4) . . ? O24 S3 O23 108.4(3) . . ? O25 S3 O23 108.6(3) . . ? O24 S3 C39 111.4(3) . . ? O25 S3 C39 109.7(4) . . ? O23 S3 C39 96.8(3) . . ? O2 C1 O3 124.2(6) . . ? O2 C1 C2 117.4(5) . . ? O3 C1 C2 118.4(6) . . ? C3 C2 C7 118.4(6) . . ? C3 C2 C1 121.0(6) . . ? C7 C2 C1 120.5(6) . . ? C2 C3 C4 120.0(6) . . ? C3 C4 C5 121.7(6) . . ? C3 C4 O6 119.5(6) . . ? C5 C4 O6 118.8(7) . . ? O5 C5 C6 127.3(7) . . ? O5 C5 C4 115.3(7) . . ? C6 C5 C4 117.4(7) . . ? C7 C6 C5 121.1(7) . . ? C6 C7 C2 121.2(6) . . ? C14 C9 C10 122.0(7) . . ? C14 C9 S1 120.2(5) . . ? C10 C9 S1 117.8(6) . . ? C9 C10 C11 116.5(7) . . ? C12 C11 C10 122.5(6) . . ? C11 C12 C13 119.4(7) . . ? C11 C12 C15 121.5(6) . . ? C13 C12 C15 119.1(6) . . ? C12 C13 C14 120.0(7) . . ? C9 C14 C13 119.7(6) . . ? O9 C15 O10 123.8(6) . . ? O9 C15 C12 119.8(6) . . ? O10 C15 C12 116.4(6) . . ? O14 C16 O4 125.5(7) . . ? O14 C16 C17 116.9(6) . . ? O4 C16 C17 117.6(6) . . ? C22 C17 C18 119.2(7) . . ? C22 C17 C16 121.2(6) . . ? C18 C17 C16 119.6(6) . . ? C19 C18 C17 120.2(6) . . ? C18 C19 C20 120.5(6) . . ? C21 C20 C19 119.5(7) . . ? C21 C20 S2 119.9(6) . . ? C19 C20 S2 120.6(5) . . ? C20 C21 C22 119.8(7) . . ? C21 C22 C17 120.7(6) . . ? C24 C23 C28 122.3(7) . . ? C24 C23 O17 120.2(7) . . ? C28 C23 O17 117.4(7) . . ? C23 C24 C25 119.6(7) . . ? C24 C25 C26 119.3(6) . . ? C24 C25 C30 119.0(6) . . ? C26 C25 C30 121.7(7) . . ? C27 C26 C25 120.5(7) . . ? C26 C27 C28 120.1(7) . . ? O18 C28 C27 124.2(8) . . ? O18 C28 C23 117.5(8) . . ? C27 C28 C23 118.3(7) . . ? O19 C30 O20 123.7(7) . . ? O19 C30 C25 117.5(7) . . ? O20 C30 C25 118.8(7) . . ? O21 C31 O13 120.3(6) . . ? O21 C31 C32 118.4(6) . . ? O13 C31 C32 121.3(6) . . ? O21 C31 Pr1 52.5(3) . 1_655 ? O13 C31 Pr1 68.4(4) . 1_655 ? C32 C31 Pr1 167.1(5) . 1_655 ? C37 C32 C33 119.3(6) . . ? C37 C32 C31 118.0(6) . . ? C33 C32 C31 122.5(6) . . ? C34 C33 C32 120.6(7) . . ? C33 C34 C35 120.3(7) . . ? O22 C35 C36 115.8(7) . . ? O22 C35 C34 125.6(6) . . ? C36 C35 C34 118.6(7) . . ? C37 C36 C35 122.3(6) . . ? C37 C36 O23 117.9(6) . . ? C35 C36 O23 119.7(6) . . ? C36 C37 C32 118.9(6) . . ? C44 C39 C40 121.1(7) . . ? C44 C39 S3 118.9(6) . . ? C40 C39 S3 119.9(6) . . ? C41 C40 C39 119.8(6) . . ? C40 C41 C42 119.8(6) . . ? C41 C42 C43 119.8(7) . . ? C41 C42 C45 121.2(5) . . ? C43 C42 C45 119.0(6) . . ? C44 C43 C42 119.5(7) . . ? C39 C44 C43 120.0(7) . . ? O27 C45 O26 124.9(7) . . ? O27 C45 C42 118.8(6) . . ? O26 C45 C42 116.2(6) . . ? C1 O2 Pr1 140.9(4) . . ? C1 O3 Pr2 148.9(4) . . ? C16 O4 Pr1 153.6(5) . . ? C5 O5 C8 117.3(6) . . ? C4 O6 S1 119.3(5) . . ? C15 O9 Pr2 133.1(4) . 2_667 ? C15 O10 Pr1 155.2(4) . 2_567 ? C31 O13 Pr2 133.3(5) . . ? C31 O13 Pr1 86.8(4) . 1_655 ? Pr2 O13 Pr1 115.62(16) . 1_655 ? C16 O14 Pr2 145.0(4) . . ? C23 O17 S2 120.8(5) . . ? C28 O18 C29 118.4(8) . . ? C30 O19 Pr2 134.7(5) . 2_676 ? C30 O20 Pr1 131.1(4) . 2_576 ? C31 O21 Pr1 103.8(4) . 1_655 ? C35 O22 C38 120.0(6) . . ? C36 O23 S3 116.9(4) . . ? C45 O26 Pr2 147.7(4) . 1_665 ? C45 O27 Pr1 128.4(4) . 1_665 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.020 0.000 0.000 526.8 5.1 2 0.000 0.500 0.500 16.3 5.5 3 0.295 0.683 0.440 30.9 6.5 4 0.705 0.317 0.560 30.9 6.7 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.834 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.127 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 905408' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 Eu2 O27 S3' _chemical_formula_weight 1408.84 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2706(3) _cell_length_b 15.6634(7) _cell_length_c 22.3100(8) _cell_angle_alpha 102.250(3) _cell_angle_beta 101.468(3) _cell_angle_gamma 104.507(3) _cell_volume 2954.21(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7045 _cell_measurement_theta_min 2.4357 _cell_measurement_theta_max 29.1738 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6574 _exptl_absorpt_correction_T_max 0.6574 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19427 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0937 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10382 _reflns_number_gt 7563 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10382 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.51437(4) 0.36033(2) 0.802130(15) 0.02194(10) Uani 1 1 d . . . Eu2 Eu 0.02952(3) 0.41202(2) 0.856588(15) 0.01951(10) Uani 1 1 d . . . C1 C 0.2065(7) 0.2422(5) 0.8548(3) 0.0220(15) Uani 1 1 d . . . C2 C 0.1745(7) 0.1491(5) 0.8677(3) 0.0261(17) Uani 1 1 d . . . C3 C 0.2574(8) 0.0910(5) 0.8504(3) 0.039(2) Uani 1 1 d . . . H3 H 0.3378 0.1096 0.8322 0.046 Uiso 1 1 calc R . . C4 C 0.2205(9) 0.0045(6) 0.8601(4) 0.047(2) Uani 1 1 d . . . H4 H 0.2740 -0.0359 0.8474 0.056 Uiso 1 1 calc R . . C5 C 0.1037(8) -0.0215(5) 0.8890(3) 0.0353(19) Uani 1 1 d . . . C6 C 0.0214(8) 0.0368(5) 0.9070(3) 0.0353(19) Uani 1 1 d . . . H6 H -0.0575 0.0190 0.9261 0.042 Uiso 1 1 calc R . . C7 C 0.0586(8) 0.1221(5) 0.8962(3) 0.0341(19) Uani 1 1 d . . . H7 H 0.0042 0.1622 0.9084 0.041 Uiso 1 1 calc R . . C8 C 0.2718(8) -0.1672(5) 0.9806(3) 0.0360(19) Uani 1 1 d . . . C9 C 0.4121(9) -0.1566(6) 0.9654(3) 0.044(2) Uani 1 1 d . . . C10 C 0.5000(8) -0.2114(6) 0.9844(3) 0.041(2) Uani 1 1 d . . . H10 H 0.5940 -0.2067 0.9746 0.049 Uiso 1 1 calc R . . C11 C 0.4484(7) -0.2730(5) 1.0181(3) 0.0337(19) Uani 1 1 d . . . H11 H 0.5092 -0.3082 1.0311 0.040 Uiso 1 1 calc R . . C12 C 0.3084(7) -0.2822(5) 1.0321(3) 0.0228(15) Uani 1 1 d . . . C13 C 0.2219(7) -0.2277(5) 1.0126(3) 0.0306(18) Uani 1 1 d . . . H13 H 0.1270 -0.2330 1.0218 0.037 Uiso 1 1 calc R . . C14 C 0.6049(10) -0.0763(8) 0.9236(4) 0.089(4) Uani 1 1 d . . . H14A H 0.6135 -0.1319 0.8986 0.134 Uiso 1 1 calc R . . H14B H 0.6822 -0.0555 0.9637 0.134 Uiso 1 1 calc R . . H14C H 0.6199 -0.0301 0.9013 0.134 Uiso 1 1 calc R . . C15 C 0.2513(7) -0.3458(5) 1.0694(3) 0.0261(16) Uani 1 1 d . . . C16 C -0.2992(8) 0.2269(5) 0.7884(3) 0.0293(17) Uani 1 1 d . . . C17 C -0.2495(7) 0.1431(5) 0.7708(3) 0.0254(16) Uani 1 1 d . . . C18 C -0.1297(7) 0.1411(5) 0.7416(3) 0.0297(17) Uani 1 1 d . . . H18 H -0.0768 0.1939 0.7330 0.036 Uiso 1 1 calc R . . C19 C -0.0888(8) 0.0635(5) 0.7257(3) 0.0369(19) Uani 1 1 d . . . H19 H -0.0078 0.0640 0.7068 0.044 Uiso 1 1 calc R . . C20 C -0.1677(8) -0.0165(5) 0.7373(3) 0.0349(18) Uani 1 1 d . . . C21 C -0.2868(7) -0.0143(5) 0.7659(3) 0.0295(17) Uani 1 1 d . . . C22 C -0.3283(7) 0.0633(5) 0.7826(3) 0.0281(17) Uani 1 1 d . . . H22 H -0.4088 0.0626 0.8017 0.034 Uiso 1 1 calc R . . C23 C -0.0188(10) -0.1051(6) 0.6928(5) 0.073(3) Uani 1 1 d . . . H23A H -0.0662 -0.1424 0.6498 0.109 Uiso 1 1 calc R . . H23B H 0.0488 -0.1329 0.7145 0.109 Uiso 1 1 calc R . . H23C H 0.0396 -0.0452 0.6927 0.109 Uiso 1 1 calc R . . C24 C -0.5530(8) -0.2479(5) 0.7626(3) 0.0340(18) Uani 1 1 d . . . C25 C -0.4549(8) -0.3005(6) 0.7606(4) 0.049(2) Uani 1 1 d . . . H25 H -0.3770 -0.2900 0.7400 0.059 Uiso 1 1 calc R . . C26 C -0.4765(8) -0.3699(5) 0.7907(4) 0.039(2) Uani 1 1 d . . . H26 H -0.4109 -0.4062 0.7904 0.047 Uiso 1 1 calc R . . C27 C -0.5924(7) -0.3866(5) 0.8209(3) 0.0240(15) Uani 1 1 d . . . C28 C -0.6900(7) -0.3326(5) 0.8212(3) 0.0326(18) Uani 1 1 d . . . H28 H -0.7678 -0.3431 0.8419 0.039 Uiso 1 1 calc R . . C29 C -0.6735(7) -0.2637(5) 0.7914(4) 0.0368(19) Uani 1 1 d . . . H29 H -0.7408 -0.2285 0.7906 0.044 Uiso 1 1 calc R . . C30 C -0.6112(7) -0.4617(5) 0.8538(3) 0.0257(16) Uani 1 1 d . . . C31 C 0.1697(7) 0.3764(5) 0.7229(3) 0.0225(15) Uani 1 1 d . . . C32 C 0.0903(7) 0.3764(5) 0.6585(3) 0.0243(16) Uani 1 1 d . . . C33 C -0.0724(7) 0.3514(5) 0.6377(3) 0.0368(19) Uani 1 1 d . . . H33 H -0.1306 0.3350 0.6653 0.044 Uiso 1 1 calc R . . C34 C -0.1458(8) 0.3510(6) 0.5788(3) 0.042(2) Uani 1 1 d . . . H34 H -0.2531 0.3347 0.5668 0.050 Uiso 1 1 calc R . . C35 C -0.0640(8) 0.3742(5) 0.5361(3) 0.039(2) Uani 1 1 d . . . C36 C 0.0939(8) 0.3981(5) 0.5560(3) 0.0342(18) Uani 1 1 d . . . C37 C 0.1736(7) 0.3991(5) 0.6157(3) 0.0297(17) Uani 1 1 d . . . H37 H 0.2809 0.4146 0.6270 0.036 Uiso 1 1 calc R . . C38 C -0.2901(10) 0.3498(7) 0.4528(4) 0.081(3) Uani 1 1 d . . . H38A H -0.3178 0.3572 0.4109 0.121 Uiso 1 1 calc R . . H38B H -0.3318 0.3866 0.4806 0.121 Uiso 1 1 calc R . . H38C H -0.3314 0.2865 0.4513 0.121 Uiso 1 1 calc R . . C39 C 0.2150(8) 0.3929(6) 0.4013(3) 0.0347(19) Uani 1 1 d . . . C40 C 0.3473(8) 0.4429(6) 0.3919(3) 0.048(2) Uani 1 1 d . . . H40 H 0.4423 0.4532 0.4202 0.057 Uiso 1 1 calc R . . C41 C 0.3395(8) 0.4790(6) 0.3391(3) 0.038(2) Uani 1 1 d . . . H41 H 0.4297 0.5127 0.3323 0.046 Uiso 1 1 calc R . . C42 C 0.1992(7) 0.4645(5) 0.2979(3) 0.0225(15) Uani 1 1 d . . . C43 C 0.0666(8) 0.4152(6) 0.3093(3) 0.041(2) Uani 1 1 d . . . H43 H -0.0290 0.4050 0.2814 0.049 Uiso 1 1 calc R . . C44 C 0.0742(8) 0.3806(6) 0.3620(3) 0.045(2) Uani 1 1 d . . . H44 H -0.0158 0.3495 0.3703 0.054 Uiso 1 1 calc R . . C45 C 0.1899(8) 0.5048(5) 0.2418(3) 0.0274(16) Uani 1 1 d . . . O1 O 0.3085(5) 0.2629(4) 0.8251(2) 0.0395(13) Uani 1 1 d . . . O2 O 0.1300(5) 0.2925(3) 0.8732(2) 0.0345(12) Uani 1 1 d . . . O3 O 0.0865(6) -0.1965(4) 0.8557(2) 0.0477(14) Uani 1 1 d . . . O4 O -0.0868(6) -0.1514(4) 0.9171(3) 0.0700(19) Uani 1 1 d . . . O5 O 0.1915(7) -0.1051(4) 0.9683(2) 0.0587(17) Uani 1 1 d . . . O6 O 0.4544(7) -0.0934(4) 0.9347(3) 0.0624(17) Uani 1 1 d . . . O7 O 0.3411(5) -0.3854(3) 1.0940(2) 0.0338(12) Uani 1 1 d . . . O8 O 0.1203(5) -0.3541(4) 1.0757(2) 0.0451(15) Uani 1 1 d . . . O9 O -0.2142(5) 0.3052(3) 0.7896(2) 0.0346(12) Uani 1 1 d . . . O10 O -0.4283(5) 0.2169(3) 0.8011(2) 0.0413(13) Uani 1 1 d . . . O11 O -0.1361(6) -0.0973(4) 0.7249(3) 0.0552(16) Uani 1 1 d . . . O12 O -0.3646(5) -0.0949(3) 0.7788(2) 0.0365(12) Uani 1 1 d . . . O13 O -0.4990(7) -0.1805(4) 0.6680(3) 0.0696(19) Uani 1 1 d . . . O14 O -0.6360(6) -0.1089(4) 0.7362(3) 0.076(2) Uani 1 1 d . . . O15 O -0.5030(5) -0.4984(3) 0.8622(2) 0.0273(11) Uani 1 1 d . . . O16 O -0.7301(5) -0.4824(3) 0.8722(2) 0.0338(12) Uani 1 1 d . . . O17 O 0.3121(5) 0.3895(4) 0.7355(2) 0.0374(13) Uani 1 1 d . . . O18 O 0.0897(5) 0.3611(4) 0.7615(2) 0.0359(13) Uani 1 1 d . . . O19 O -0.1242(6) 0.3784(4) 0.4764(2) 0.0541(16) Uani 1 1 d . . . O21 O 0.1824(6) 0.4254(4) 0.5139(2) 0.0479(14) Uani 1 1 d . . . O22 O 0.3835(7) 0.3566(5) 0.4947(3) 0.081(2) Uani 1 1 d . . . O23 O 0.1095(7) 0.2637(4) 0.4526(2) 0.0607(17) Uani 1 1 d . . . O24 O 0.0597(5) 0.5009(3) 0.2107(2) 0.0313(12) Uani 1 1 d . . . O25 O 0.3158(5) 0.5366(3) 0.2293(2) 0.0355(13) Uani 1 1 d . . . O26 O 0.1845(6) 0.4490(4) 0.9722(2) 0.0553(16) Uani 1 1 d . . . H26A H 0.1587 0.4020 0.9857 0.083 Uiso 1 1 d R . . H26B H 0.2806 0.4630 0.9743 0.083 Uiso 1 1 d R . . O27 O 0.0013(6) 0.5504(4) 0.9235(2) 0.0511(15) Uani 1 1 d . . . H27A H -0.0210 0.5849 0.9001 0.077 Uiso 1 1 d R . . H27B H -0.0719 0.5352 0.9412 0.077 Uiso 1 1 d R . . O28 O 0.4486(7) 0.2619(5) 0.6913(2) 0.070(2) Uani 1 1 d . . . H28A H 0.3651 0.2134 0.6830 0.105 Uiso 1 1 d R . . H28B H 0.4284 0.2933 0.6632 0.105 Uiso 1 1 d R . . S1 S -0.5254(2) -0.15584(15) 0.72837(11) 0.0461(6) Uani 1 1 d . . . S2 S 0.0599(2) -0.13065(15) 0.90260(10) 0.0420(5) Uani 1 1 d . . . S3 S 0.2259(3) 0.34882(18) 0.46750(9) 0.0478(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02446(19) 0.0215(2) 0.0244(2) 0.01108(16) 0.00878(15) 0.00910(16) Eu2 0.02113(18) 0.0196(2) 0.0223(2) 0.01074(16) 0.00894(14) 0.00743(15) C1 0.021(3) 0.018(4) 0.027(4) 0.013(3) 0.003(3) 0.002(3) C2 0.032(4) 0.030(5) 0.028(4) 0.019(3) 0.009(3) 0.021(4) C3 0.042(4) 0.043(6) 0.054(5) 0.030(4) 0.029(4) 0.026(4) C4 0.065(5) 0.045(6) 0.066(6) 0.039(5) 0.039(5) 0.043(5) C5 0.044(4) 0.037(5) 0.036(5) 0.021(4) 0.014(4) 0.019(4) C6 0.036(4) 0.040(5) 0.047(5) 0.025(4) 0.026(4) 0.020(4) C7 0.040(4) 0.037(5) 0.044(5) 0.022(4) 0.021(4) 0.027(4) C8 0.046(5) 0.038(5) 0.035(5) 0.024(4) 0.014(4) 0.018(4) C9 0.049(5) 0.050(6) 0.031(5) 0.024(4) 0.012(4) 0.001(4) C10 0.028(4) 0.048(6) 0.046(5) 0.014(4) 0.019(4) 0.002(4) C11 0.029(4) 0.046(5) 0.033(4) 0.018(4) 0.007(3) 0.019(4) C12 0.025(4) 0.022(4) 0.023(4) 0.009(3) 0.004(3) 0.009(3) C13 0.028(4) 0.039(5) 0.037(4) 0.019(4) 0.017(3) 0.018(4) C14 0.087(7) 0.109(10) 0.056(7) 0.049(7) 0.021(5) -0.022(7) C15 0.027(4) 0.029(5) 0.022(4) 0.012(3) 0.002(3) 0.006(3) C16 0.037(4) 0.012(4) 0.031(4) 0.001(3) 0.004(3) 0.003(3) C17 0.022(3) 0.021(4) 0.033(4) 0.007(3) 0.004(3) 0.010(3) C18 0.023(4) 0.023(4) 0.038(4) 0.010(4) 0.004(3) -0.001(3) C19 0.031(4) 0.030(5) 0.054(5) 0.010(4) 0.018(4) 0.011(4) C20 0.032(4) 0.028(5) 0.042(5) 0.006(4) 0.001(3) 0.013(4) C21 0.027(4) 0.026(5) 0.033(4) 0.015(4) 0.001(3) 0.003(3) C22 0.026(4) 0.032(5) 0.027(4) 0.009(3) 0.005(3) 0.011(3) C23 0.077(6) 0.046(7) 0.104(8) 0.002(6) 0.040(6) 0.039(6) C24 0.037(4) 0.017(4) 0.043(5) 0.010(4) 0.006(4) 0.001(3) C25 0.048(5) 0.049(6) 0.078(6) 0.039(5) 0.038(5) 0.027(5) C26 0.039(4) 0.034(5) 0.063(6) 0.026(4) 0.027(4) 0.021(4) C27 0.024(3) 0.018(4) 0.030(4) 0.004(3) 0.008(3) 0.007(3) C28 0.031(4) 0.032(5) 0.042(5) 0.017(4) 0.017(3) 0.012(4) C29 0.028(4) 0.028(5) 0.061(5) 0.019(4) 0.011(4) 0.016(4) C30 0.026(4) 0.017(4) 0.025(4) 0.001(3) 0.003(3) -0.002(3) C31 0.020(4) 0.019(4) 0.026(4) 0.007(3) 0.000(3) 0.006(3) C32 0.028(4) 0.026(4) 0.021(4) 0.009(3) 0.007(3) 0.011(3) C33 0.035(4) 0.040(5) 0.040(5) 0.014(4) 0.015(4) 0.012(4) C34 0.033(4) 0.055(6) 0.033(5) 0.008(4) 0.001(4) 0.015(4) C35 0.039(4) 0.043(6) 0.028(4) 0.005(4) -0.005(4) 0.015(4) C36 0.048(5) 0.033(5) 0.025(4) 0.008(4) 0.018(4) 0.014(4) C37 0.030(4) 0.033(5) 0.029(4) 0.012(4) 0.007(3) 0.012(3) C38 0.073(7) 0.093(9) 0.056(6) 0.022(6) -0.029(5) 0.024(6) C39 0.034(4) 0.060(6) 0.021(4) 0.028(4) 0.010(3) 0.018(4) C40 0.034(4) 0.089(8) 0.035(5) 0.038(5) 0.011(4) 0.026(5) C41 0.027(4) 0.060(6) 0.039(5) 0.030(4) 0.012(3) 0.017(4) C42 0.026(4) 0.028(4) 0.018(4) 0.011(3) 0.007(3) 0.010(3) C43 0.029(4) 0.063(6) 0.036(5) 0.032(4) 0.002(3) 0.013(4) C44 0.039(4) 0.061(6) 0.040(5) 0.034(5) 0.018(4) 0.001(4) C45 0.039(4) 0.026(5) 0.027(4) 0.011(3) 0.015(3) 0.019(4) O1 0.038(3) 0.038(4) 0.062(4) 0.035(3) 0.027(3) 0.019(3) O2 0.053(3) 0.031(3) 0.037(3) 0.021(3) 0.021(2) 0.026(3) O3 0.063(3) 0.032(4) 0.054(4) 0.013(3) 0.013(3) 0.026(3) O4 0.062(4) 0.050(4) 0.130(6) 0.051(4) 0.057(4) 0.026(3) O5 0.106(5) 0.044(4) 0.042(3) 0.023(3) 0.013(3) 0.046(4) O6 0.077(4) 0.049(4) 0.061(4) 0.034(4) 0.027(3) -0.005(3) O7 0.049(3) 0.025(3) 0.029(3) 0.014(2) 0.002(2) 0.016(3) O8 0.028(3) 0.069(4) 0.048(3) 0.037(3) 0.012(2) 0.012(3) O9 0.045(3) 0.018(3) 0.037(3) 0.008(2) 0.008(2) 0.003(2) O10 0.028(3) 0.031(3) 0.064(4) 0.008(3) 0.012(3) 0.012(2) O11 0.054(3) 0.034(4) 0.088(5) 0.014(3) 0.029(3) 0.026(3) O12 0.042(3) 0.021(3) 0.044(3) 0.013(3) 0.009(2) 0.004(2) O13 0.101(5) 0.046(4) 0.042(4) 0.019(3) 0.003(3) -0.005(4) O14 0.042(3) 0.054(5) 0.148(6) 0.067(5) 0.015(4) 0.020(3) O15 0.028(2) 0.023(3) 0.035(3) 0.012(2) 0.006(2) 0.013(2) O16 0.026(2) 0.028(3) 0.052(3) 0.021(3) 0.017(2) 0.003(2) O17 0.032(3) 0.055(4) 0.034(3) 0.025(3) 0.007(2) 0.018(3) O18 0.043(3) 0.047(4) 0.024(3) 0.010(3) 0.015(2) 0.020(3) O19 0.066(4) 0.071(5) 0.027(3) 0.016(3) -0.002(3) 0.032(3) O21 0.074(4) 0.044(4) 0.025(3) 0.013(3) 0.019(3) 0.011(3) O22 0.080(4) 0.141(7) 0.068(4) 0.069(5) 0.032(4) 0.071(5) O23 0.102(5) 0.051(4) 0.041(4) 0.029(3) 0.032(3) 0.022(4) O24 0.031(3) 0.040(3) 0.029(3) 0.023(3) 0.004(2) 0.011(2) O25 0.036(3) 0.044(4) 0.048(3) 0.033(3) 0.026(2) 0.019(3) O26 0.057(3) 0.057(5) 0.050(4) 0.018(3) 0.012(3) 0.014(3) O27 0.074(4) 0.045(4) 0.046(4) 0.015(3) 0.026(3) 0.031(3) O28 0.089(4) 0.096(6) 0.040(4) 0.009(4) 0.020(3) 0.059(4) S1 0.0479(12) 0.0290(13) 0.0569(15) 0.0250(11) 0.0024(11) 0.0022(10) S2 0.0558(13) 0.0302(13) 0.0565(14) 0.0259(11) 0.0266(11) 0.0206(11) S3 0.0660(15) 0.0672(18) 0.0299(12) 0.0312(12) 0.0212(10) 0.0330(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O25 2.286(4) 2_666 ? Eu1 O7 2.332(4) 2_657 ? Eu1 O1 2.345(5) . ? Eu1 O17 2.354(4) . ? Eu1 O15 2.393(5) 1_665 ? Eu1 O10 2.432(5) 1_655 ? Eu1 O28 2.485(5) . ? Eu1 O9 2.902(4) 1_655 ? Eu1 C16 3.033(7) 1_655 ? Eu2 O16 2.329(4) 1_665 ? Eu2 O18 2.329(4) . ? Eu2 O2 2.354(4) . ? Eu2 O24 2.395(4) 2_566 ? Eu2 O8 2.411(5) 2_557 ? Eu2 O9 2.417(5) . ? Eu2 O27 2.461(5) . ? Eu2 O26 2.555(5) . ? C1 O2 1.246(7) . ? C1 O1 1.274(7) . ? C1 C2 1.516(9) . ? C2 C3 1.373(9) . ? C2 C7 1.377(8) . ? C3 C4 1.387(10) . ? C3 H3 0.9300 . ? C4 C5 1.385(9) . ? C4 H4 0.9300 . ? C5 C6 1.375(9) . ? C5 S2 1.762(7) . ? C6 C7 1.378(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.350(9) . ? C8 C9 1.387(9) . ? C8 O5 1.405(8) . ? C9 O6 1.344(8) . ? C9 C10 1.395(10) . ? C10 C11 1.393(9) . ? C10 H10 0.9300 . ? C11 C12 1.375(8) . ? C11 H11 0.9300 . ? C12 C13 1.386(8) . ? C12 C15 1.492(9) . ? C13 H13 0.9300 . ? C14 O6 1.435(9) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O8 1.229(7) . ? C15 O7 1.265(7) . ? C16 O10 1.264(7) . ? C16 O9 1.271(8) . ? C16 C17 1.499(9) . ? C16 Eu1 3.033(7) 1_455 ? C17 C22 1.387(9) . ? C17 C18 1.398(8) . ? C18 C19 1.360(9) . ? C18 H18 0.9300 . ? C19 C20 1.388(10) . ? C19 H19 0.9300 . ? C20 O11 1.354(8) . ? C20 C21 1.383(9) . ? C21 C22 1.365(9) . ? C21 O12 1.406(8) . ? C22 H22 0.9300 . ? C23 O11 1.431(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.372(9) . ? C24 C29 1.393(9) . ? C24 S1 1.757(7) . ? C25 C26 1.387(9) . ? C25 H25 0.9300 . ? C26 C27 1.378(8) . ? C26 H26 0.9300 . ? C27 C28 1.384(8) . ? C27 C30 1.507(9) . ? C28 C29 1.376(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O16 1.244(7) . ? C30 O15 1.276(7) . ? C31 O17 1.247(7) . ? C31 O18 1.266(7) . ? C31 C32 1.479(8) . ? C32 C37 1.390(8) . ? C32 C33 1.412(8) . ? C33 C34 1.353(9) . ? C33 H33 0.9300 . ? C34 C35 1.381(10) . ? C34 H34 0.9300 . ? C35 O19 1.360(8) . ? C35 C36 1.370(9) . ? C36 C37 1.384(8) . ? C36 O21 1.427(8) . ? C37 H37 0.9300 . ? C38 O19 1.440(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.361(9) . ? C39 C44 1.362(9) . ? C39 S3 1.755(6) . ? C40 C41 1.406(9) . ? C40 H40 0.9300 . ? C41 C42 1.370(8) . ? C41 H41 0.9300 . ? C42 C43 1.380(9) . ? C42 C45 1.513(8) . ? C43 C44 1.392(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 O24 1.247(7) . ? C45 O25 1.259(7) . ? O3 S2 1.410(5) . ? O4 S2 1.434(5) . ? O5 S2 1.610(5) . ? O7 Eu1 2.332(4) 2_657 ? O8 Eu2 2.411(5) 2_557 ? O9 Eu1 2.902(4) 1_455 ? O10 Eu1 2.432(5) 1_455 ? O12 S1 1.601(5) . ? O13 S1 1.407(6) . ? O14 S1 1.420(6) . ? O15 Eu1 2.393(4) 1_445 ? O16 Eu2 2.329(4) 1_445 ? O21 S3 1.598(6) . ? O22 S3 1.430(5) . ? O23 S3 1.415(6) . ? O24 Eu2 2.395(4) 2_566 ? O25 Eu1 2.286(4) 2_666 ? O26 H26A 0.8514 . ? O26 H26B 0.8515 . ? O27 H27A 0.8599 . ? O27 H27B 0.8598 . ? O28 H28A 0.8938 . ? O28 H28B 0.8934 . ? 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 O25 Eu1 O7 99.23(16) 2_666 2_657 ? O25 Eu1 O1 170.47(14) 2_666 . ? O7 Eu1 O1 88.08(17) 2_657 . ? O25 Eu1 O17 88.01(15) 2_666 . ? O7 Eu1 O17 146.69(17) 2_657 . ? O1 Eu1 O17 82.54(15) . . ? O25 Eu1 O15 79.50(16) 2_666 1_665 ? O7 Eu1 O15 73.88(15) 2_657 1_665 ? O1 Eu1 O15 96.84(16) . 1_665 ? O17 Eu1 O15 75.61(16) . 1_665 ? O25 Eu1 O10 114.99(16) 2_666 1_655 ? O7 Eu1 O10 76.24(16) 2_657 1_655 ? O1 Eu1 O10 72.56(16) . 1_655 ? O17 Eu1 O10 129.80(17) . 1_655 ? O15 Eu1 O10 148.59(15) 1_665 1_655 ? O25 Eu1 O28 85.5(2) 2_666 . ? O7 Eu1 O28 143.72(17) 2_657 . ? O1 Eu1 O28 92.3(2) . . ? O17 Eu1 O28 68.86(17) . . ? O15 Eu1 O28 141.76(17) 1_665 . ? O10 Eu1 O28 69.35(19) 1_655 . ? O25 Eu1 O9 67.93(14) 2_666 1_655 ? O7 Eu1 O9 74.64(14) 2_657 1_655 ? O1 Eu1 O9 120.33(14) . 1_655 ? O17 Eu1 O9 137.02(14) . 1_655 ? O15 Eu1 O9 129.58(14) 1_665 1_655 ? O10 Eu1 O9 48.03(14) 1_655 1_655 ? O28 Eu1 O9 74.01(15) . 1_655 ? O25 Eu1 C16 91.47(18) 2_666 1_655 ? O7 Eu1 C16 76.46(17) 2_657 1_655 ? O1 Eu1 C16 96.21(18) . 1_655 ? O17 Eu1 C16 136.19(18) . 1_655 ? O15 Eu1 C16 147.05(16) 1_665 1_655 ? O10 Eu1 C16 23.64(16) 1_655 1_655 ? O28 Eu1 C16 67.43(17) . 1_655 ? O9 Eu1 C16 24.62(15) 1_655 1_655 ? O16 Eu2 O18 78.28(17) 1_665 . ? O16 Eu2 O2 94.76(16) 1_665 . ? O18 Eu2 O2 76.89(16) . . ? O16 Eu2 O24 83.62(15) 1_665 2_566 ? O18 Eu2 O24 74.85(16) . 2_566 ? O2 Eu2 O24 151.43(16) . 2_566 ? O16 Eu2 O8 135.75(17) 1_665 2_557 ? O18 Eu2 O8 140.13(19) . 2_557 ? O2 Eu2 O8 79.63(16) . 2_557 ? O24 Eu2 O8 120.84(15) 2_566 2_557 ? O16 Eu2 O9 152.41(16) 1_665 . ? O18 Eu2 O9 77.35(16) . . ? O2 Eu2 O9 92.14(16) . . ? O24 Eu2 O9 77.70(15) 2_566 . ? O8 Eu2 O9 71.80(16) 2_557 . ? O16 Eu2 O27 78.99(18) 1_665 . ? O18 Eu2 O27 140.80(18) . . ? O2 Eu2 O27 136.61(16) . . ? O24 Eu2 O27 71.23(16) 2_566 . ? O8 Eu2 O27 76.10(19) 2_557 . ? O9 Eu2 O27 113.15(16) . . ? O16 Eu2 O26 70.87(18) 1_665 . ? O18 Eu2 O26 131.07(16) . . ? O2 Eu2 O26 69.10(17) . . ? O24 Eu2 O26 135.30(17) 2_566 . ? O8 Eu2 O26 66.13(17) 2_557 . ? O9 Eu2 O26 136.16(17) . . ? O27 Eu2 O26 68.32(17) . . ? O2 C1 O1 124.8(6) . . ? O2 C1 C2 117.6(6) . . ? O1 C1 C2 117.5(6) . . ? C3 C2 C7 119.9(6) . . ? C3 C2 C1 120.9(6) . . ? C7 C2 C1 119.2(6) . . ? C2 C3 C4 119.6(7) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.9(7) . . ? C6 C5 S2 119.6(6) . . ? C4 C5 S2 119.5(6) . . ? C5 C6 C7 118.5(6) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 121.4(6) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C13 C8 C9 121.6(6) . . ? C13 C8 O5 120.4(6) . . ? C9 C8 O5 117.5(6) . . ? O6 C9 C8 117.7(7) . . ? O6 C9 C10 125.0(7) . . ? C8 C9 C10 117.3(7) . . ? C11 C10 C9 120.7(6) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.6(6) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 118.1(6) . . ? C11 C12 C15 122.0(6) . . ? C13 C12 C15 119.9(6) . . ? C8 C13 C12 121.7(6) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.1 . . ? O6 C14 H14A 109.5 . . ? O6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O8 C15 O7 124.1(6) . . ? O8 C15 C12 117.2(6) . . ? O7 C15 C12 118.6(6) . . ? O10 C16 O9 121.5(6) . . ? O10 C16 C17 117.8(6) . . ? O9 C16 C17 120.6(6) . . ? O10 C16 Eu1 50.5(3) . 1_455 ? O9 C16 Eu1 71.9(4) . 1_455 ? C17 C16 Eu1 164.2(5) . 1_455 ? C22 C17 C18 118.5(6) . . ? C22 C17 C16 118.6(6) . . ? C18 C17 C16 122.9(6) . . ? C19 C18 C17 121.4(7) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 120.2(7) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? O11 C20 C21 116.0(7) . . ? O11 C20 C19 125.8(7) . . ? C21 C20 C19 118.2(7) . . ? C22 C21 C20 122.2(7) . . ? C22 C21 O12 119.6(6) . . ? C20 C21 O12 118.1(6) . . ? C21 C22 C17 119.5(6) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? O11 C23 H23A 109.5 . . ? O11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 122.6(7) . . ? C25 C24 S1 119.3(6) . . ? C29 C24 S1 118.1(5) . . ? C24 C25 C26 117.4(7) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? C27 C26 C25 121.8(6) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 119.1(6) . . ? C26 C27 C30 120.4(6) . . ? C28 C27 C30 120.5(6) . . ? C29 C28 C27 121.0(6) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C24 118.1(6) . . ? C28 C29 H29 120.9 . . ? C24 C29 H29 120.9 . . ? O16 C30 O15 124.5(6) . . ? O16 C30 C27 117.4(6) . . ? O15 C30 C27 118.1(6) . . ? O17 C31 O18 123.7(6) . . ? O17 C31 C32 117.7(6) . . ? O18 C31 C32 118.5(5) . . ? C37 C32 C33 117.7(6) . . ? C37 C32 C31 121.0(5) . . ? C33 C32 C31 121.3(6) . . ? C34 C33 C32 121.6(6) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 121.1(6) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? O19 C35 C36 116.0(7) . . ? O19 C35 C34 126.5(6) . . ? C36 C35 C34 117.4(6) . . ? C35 C36 C37 123.4(6) . . ? C35 C36 O21 119.0(6) . . ? C37 C36 O21 117.6(6) . . ? C36 C37 C32 118.8(6) . . ? C36 C37 H37 120.6 . . ? C32 C37 H37 120.6 . . ? O19 C38 H38A 109.5 . . ? O19 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O19 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 121.0(6) . . ? C40 C39 S3 119.2(5) . . ? C44 C39 S3 119.6(5) . . ? C39 C40 C41 119.6(6) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 120.0(7) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 119.1(6) . . ? C41 C42 C45 120.3(6) . . ? C43 C42 C45 120.6(6) . . ? C42 C43 C44 120.8(6) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C39 C44 C43 119.3(7) . . ? C39 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? O24 C45 O25 125.5(6) . . ? O24 C45 C42 118.1(6) . . ? O25 C45 C42 116.3(6) . . ? C1 O1 Eu1 155.5(5) . . ? C1 O2 Eu2 145.6(4) . . ? C8 O5 S2 120.2(5) . . ? C9 O6 C14 118.1(7) . . ? C15 O7 Eu1 132.7(4) . 2_657 ? C15 O8 Eu2 137.1(4) . 2_557 ? C16 O9 Eu2 135.9(4) . . ? C16 O9 Eu1 83.5(4) . 1_455 ? Eu2 O9 Eu1 115.40(18) . 1_455 ? C16 O10 Eu1 105.9(4) . 1_455 ? C20 O11 C23 118.6(6) . . ? C21 O12 S1 116.2(4) . . ? C30 O15 Eu1 129.6(4) . 1_445 ? C30 O16 Eu2 147.3(5) . 1_445 ? C31 O17 Eu1 142.2(4) . . ? C31 O18 Eu2 149.3(5) . . ? C35 O19 C38 117.6(6) . . ? C36 O21 S3 118.6(5) . . ? C45 O24 Eu2 133.7(4) . 2_566 ? C45 O25 Eu1 154.1(4) . 2_666 ? Eu2 O26 H26A 109.0 . . ? Eu2 O26 H26B 109.4 . . ? H26A O26 H26B 109.5 . . ? Eu2 O27 H27A 109.3 . . ? Eu2 O27 H27B 109.9 . . ? H27A O27 H27B 109.0 . . ? Eu1 O28 H28A 111.8 . . ? Eu1 O28 H28B 110.9 . . ? H28A O28 H28B 107.3 . . ? O13 S1 O14 119.1(4) . . ? O13 S1 O12 108.7(3) . . ? O14 S1 O12 107.7(4) . . ? O13 S1 C24 111.9(4) . . ? O14 S1 C24 110.9(4) . . ? O12 S1 C24 95.7(3) . . ? O3 S2 O4 118.6(4) . . ? O3 S2 O5 109.7(3) . . ? O4 S2 O5 107.3(4) . . ? O3 S2 C5 112.1(3) . . ? O4 S2 C5 109.3(3) . . ? O5 S2 C5 97.7(3) . . ? O23 S3 O22 120.0(4) . . ? O23 S3 O21 109.3(3) . . ? O22 S3 O21 107.2(4) . . ? O23 S3 C39 110.3(4) . . ? O22 S3 C39 109.0(3) . . ? O21 S3 C39 98.9(3) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.020 0.000 0.500 514 52 ' ' 2 0.214 0.320 0.058 33 1 ' ' 3 0.500 0.500 0.000 18 8 ' ' 4 0.786 0.680 0.941 33 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.971 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.132 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 905409' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 Gd2 O27 S3' _chemical_formula_weight 1419.42 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2654(3) _cell_length_b 15.6423(7) _cell_length_c 22.2867(10) _cell_angle_alpha 102.154(4) _cell_angle_beta 101.481(3) _cell_angle_gamma 104.445(3) _cell_volume 2947.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8197 _cell_measurement_theta_min 2.4378 _cell_measurement_theta_max 29.2228 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 2.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6436 _exptl_absorpt_correction_T_max 0.6436 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18350 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10290 _reflns_number_gt 8034 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+32.9038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10290 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1444 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.96946(5) 0.58785(3) 0.14350(2) 0.02024(13) Uani 1 1 d . . . Gd2 Gd 0.48586(5) 0.63989(3) 0.19773(2) 0.02233(14) Uani 1 1 d . . . C1 C 0.6115(10) 0.4624(6) 0.1463(4) 0.022(2) Uani 1 1 d . . . C2 C 0.5919(10) 0.3867(6) 0.1792(5) 0.027(2) Uani 1 1 d . . . C3 C 0.6922(11) 0.3345(7) 0.1797(5) 0.036(3) Uani 1 1 d . . . H3 H 0.7726 0.3467 0.1605 0.043 Uiso 1 1 calc R . . C4 C 0.6729(12) 0.2641(7) 0.2087(6) 0.038(3) Uani 1 1 d . . . H4 H 0.7391 0.2281 0.2085 0.046 Uiso 1 1 calc R . . C5 C 0.5541(12) 0.2475(7) 0.2381(5) 0.036(3) Uani 1 1 d . . . C6 C 0.4558(14) 0.3007(8) 0.2393(7) 0.051(3) Uani 1 1 d . . . H6 H 0.3776 0.2902 0.2598 0.062 Uiso 1 1 calc R . . C7 C 0.4764(13) 0.3702(8) 0.2092(6) 0.043(3) Uani 1 1 d . . . H7 H 0.4105 0.4064 0.2093 0.052 Uiso 1 1 calc R . . C8 C 0.2865(12) 0.0152(6) 0.2341(5) 0.031(2) Uani 1 1 d . . . C9 C 0.3262(11) -0.0628(6) 0.2171(5) 0.030(2) Uani 1 1 d . . . H9 H 0.4065 -0.0623 0.1978 0.036 Uiso 1 1 calc R . . C10 C 0.2463(10) -0.1438(6) 0.2285(5) 0.026(2) Uani 1 1 d . . . C11 C 0.1276(11) -0.1429(7) 0.2578(5) 0.034(2) Uani 1 1 d . . . H11 H 0.0748 -0.1960 0.2662 0.041 Uiso 1 1 calc R . . C12 C 0.0868(11) -0.0627(7) 0.2746(5) 0.038(3) Uani 1 1 d . . . H12 H 0.0061 -0.0628 0.2936 0.046 Uiso 1 1 calc R . . C13 C 0.1656(12) 0.0163(7) 0.2631(5) 0.034(2) Uani 1 1 d . . . C14 C 0.0180(16) 0.1074(10) 0.3076(8) 0.076(5) Uani 1 1 d . . . H14A H -0.0822 0.0736 0.2792 0.114 Uiso 1 1 calc R . . H14B H 0.0243 0.1709 0.3218 0.114 Uiso 1 1 calc R . . H14C H 0.0336 0.0831 0.3437 0.114 Uiso 1 1 calc R . . C15 C 0.2943(11) -0.2269(7) 0.2111(5) 0.029(2) Uani 1 1 d . . . C16 C 0.8292(12) 0.6236(7) 0.2764(4) 0.028(2) Uani 1 1 d . . . C17 C 0.9113(11) 0.6245(7) 0.3417(4) 0.027(2) Uani 1 1 d . . . C18 C 1.0714(11) 0.6492(7) 0.3613(5) 0.038(3) Uani 1 1 d . . . H18 H 1.1290 0.6659 0.3336 0.046 Uiso 1 1 calc R . . C19 C 1.1459(12) 0.6493(9) 0.4212(5) 0.046(3) Uani 1 1 d . . . H19 H 1.2533 0.6669 0.4335 0.055 Uiso 1 1 calc R . . C20 C 1.0639(13) 0.6238(8) 0.4638(5) 0.041(3) Uani 1 1 d . . . C21 C 0.9040(12) 0.6013(7) 0.4442(5) 0.033(2) Uani 1 1 d . . . C22 C 0.8261(11) 0.6013(7) 0.3848(5) 0.032(2) Uani 1 1 d . . . H22 H 0.7189 0.5862 0.3733 0.038 Uiso 1 1 calc R . . C23 C 1.2886(16) 0.6487(12) 0.5471(7) 0.085(5) Uani 1 1 d . . . H23A H 1.3269 0.6053 0.5229 0.127 Uiso 1 1 calc R . . H23B H 1.3166 0.6498 0.5912 0.127 Uiso 1 1 calc R . . H23C H 1.3329 0.7087 0.5426 0.127 Uiso 1 1 calc R . . C24 C 0.7849(12) 0.6049(8) 0.5990(5) 0.035(3) Uani 1 1 d . . . C25 C 0.9252(13) 0.6198(8) 0.6389(5) 0.044(3) Uani 1 1 d . . . H25 H 1.0144 0.6541 0.6317 0.052 Uiso 1 1 calc R . . C26 C 0.9342(12) 0.5830(8) 0.6906(5) 0.040(3) Uani 1 1 d . . . H26 H 1.0299 0.5913 0.7178 0.047 Uiso 1 1 calc R . . C27 C 0.8000(10) 0.5341(7) 0.7014(4) 0.025(2) Uani 1 1 d . . . C28 C 0.6598(12) 0.5204(8) 0.6609(5) 0.041(3) Uani 1 1 d . . . H28 H 0.5698 0.4873 0.6683 0.049 Uiso 1 1 calc R . . C29 C 0.6515(13) 0.5554(9) 0.6094(5) 0.050(3) Uani 1 1 d . . . H29 H 0.5561 0.5457 0.5815 0.060 Uiso 1 1 calc R . . C30 C 0.8110(11) 0.4958(6) 0.7589(5) 0.025(2) Uani 1 1 d . . . C31 C 0.2504(11) 0.6546(7) 0.0700(4) 0.027(2) Uani 1 1 d . . . C32 C 0.3080(10) 0.7176(6) 0.0325(5) 0.025(2) Uani 1 1 d . . . C33 C 0.4484(11) 0.7264(8) 0.0188(5) 0.035(3) Uani 1 1 d . . . H33 H 0.5089 0.6912 0.0323 0.043 Uiso 1 1 calc R . . C34 C 0.5009(12) 0.7874(9) -0.0153(5) 0.043(3) Uani 1 1 d . . . H34 H 0.5945 0.7916 -0.0256 0.051 Uiso 1 1 calc R . . C35 C 0.4139(14) 0.8410(8) -0.0334(5) 0.046(3) Uani 1 1 d . . . C36 C 0.6035(17) 0.9221(12) -0.0762(7) 0.092(6) Uani 1 1 d . . . H36A H 0.6102 0.8665 -0.1020 0.138 Uiso 1 1 calc R . . H36B H 0.6810 0.9412 -0.0363 0.138 Uiso 1 1 calc R . . H36C H 0.6201 0.9692 -0.0978 0.138 Uiso 1 1 calc R . . C37 C 0.2714(13) 0.8318(7) -0.0186(5) 0.040(3) Uani 1 1 d . . . C38 C 0.2186(12) 0.7704(7) 0.0127(5) 0.034(2) Uani 1 1 d . . . H38 H 0.1224 0.7638 0.0209 0.040 Uiso 1 1 calc R . . C39 C 0.1038(13) 0.9793(7) -0.1105(5) 0.036(3) Uani 1 1 d . . . C40 C 0.2210(14) 1.0040(8) -0.1395(6) 0.046(3) Uani 1 1 d . . . H40 H 0.2743 0.9634 -0.1523 0.055 Uiso 1 1 calc R . . C41 C 0.2567(12) 1.0911(8) -0.1488(6) 0.040(3) Uani 1 1 d . . . H41 H 0.3380 1.1097 -0.1664 0.048 Uiso 1 1 calc R . . C42 C 0.1762(10) 1.1495(6) -0.1328(5) 0.024(2) Uani 1 1 d . . . C43 C 0.0578(12) 1.1241(7) -0.1028(5) 0.036(3) Uani 1 1 d . . . H43 H 0.0037 1.1645 -0.0906 0.043 Uiso 1 1 calc R . . C44 C 0.0230(12) 1.0385(7) -0.0919(5) 0.037(3) Uani 1 1 d . . . H44 H -0.0545 1.0209 -0.0721 0.044 Uiso 1 1 calc R . . C45 C 0.2086(10) 1.2434(7) -0.1445(4) 0.026(2) Uani 1 1 d . . . O1 O 0.7296(7) 0.4829(5) 0.1276(4) 0.0373(18) Uani 1 1 d . . . O2 O 0.5057(7) 0.4997(4) 0.1387(3) 0.0269(15) Uani 1 1 d . . . O3 O 0.6369(10) 0.1085(6) 0.2632(6) 0.075(3) Uani 1 1 d . . . O4 O 0.4978(12) 0.1818(6) 0.3316(4) 0.071(3) Uani 1 1 d . . . O5 O 0.3643(8) 0.0954(5) 0.2208(4) 0.0411(19) Uani 1 1 d . . . O6 O 0.1348(10) 0.0990(5) 0.2750(5) 0.059(2) Uani 1 1 d . . . O7 O 0.2091(8) -0.3054(4) 0.2099(4) 0.0390(18) Uani 1 1 d . . . O8 O 0.4237(8) -0.2189(5) 0.1991(4) 0.0423(19) Uani 1 1 d . . . O9 O 0.9104(8) 0.6393(5) 0.2384(3) 0.0354(17) Uani 1 1 d . . . O10 O 0.6850(8) 0.6102(5) 0.2648(3) 0.0387(18) Uani 1 1 d . . . O11 O 1.1243(10) 0.6226(7) 0.5243(4) 0.059(2) Uani 1 1 d . . . O12 O 0.8917(11) 0.7366(6) 0.5481(4) 0.059(2) Uani 1 1 d . . . O13 O 0.8181(10) 0.5732(6) 0.4862(4) 0.050(2) Uani 1 1 d . . . O14 O 0.6177(12) 0.6445(9) 0.5053(5) 0.089(4) Uani 1 1 d . . . O15 O 0.6853(8) 0.4627(5) 0.7708(4) 0.0377(18) Uani 1 1 d . . . O16 O 0.9396(8) 0.4987(5) 0.7899(3) 0.0335(17) Uani 1 1 d . . . O17 O 0.3424(9) 0.6148(5) 0.0954(3) 0.0386(18) Uani 1 1 d . . . O18 O 0.1181(8) 0.6458(6) 0.0766(4) 0.048(2) Uani 1 1 d . . . O19 O 0.4536(11) 0.9062(6) -0.0649(4) 0.070(3) Uani 1 1 d . . . O20 O 0.0880(10) 0.8036(5) -0.1441(4) 0.051(2) Uani 1 1 d . . . O21 O 0.1902(11) 0.8945(6) -0.0317(4) 0.057(2) Uani 1 1 d . . . O22 O -0.0862(11) 0.8495(6) -0.0827(5) 0.072(3) Uani 1 1 d . . . O23 O 0.3091(8) 1.2629(5) -0.1745(4) 0.041(2) Uani 1 1 d . . . O24 O 0.1322(8) 1.2934(5) -0.1268(3) 0.0363(17) Uani 1 1 d . . . O25 O 0.5497(11) 0.7327(8) 0.3063(5) 0.075(3) Uani 1 1 d . . . H25A H 0.6386 0.7919 0.3190 0.113 Uiso 1 1 d R . . H25B H 0.4655 0.7567 0.3211 0.113 Uiso 1 1 d R . . O26 O 1.0008(9) 0.4506(5) 0.0770(4) 0.051(2) Uani 1 1 d . . . H26A H 0.9467 0.4026 0.0839 0.077 Uiso 1 1 d R . . H26B H 0.9701 0.4486 0.0378 0.077 Uiso 1 1 d R . . O27 O 0.8163(11) 0.5516(6) 0.0291(4) 0.061(2) Uani 1 1 d . . . H27A H 0.7159 0.5323 0.0252 0.091 Uiso 1 1 d R . . H27B H 0.8354 0.6011 0.0154 0.091 Uiso 1 1 d R . . S1 S 0.7745(4) 0.6507(2) 0.53249(14) 0.0493(8) Uani 1 1 d . . . S2 S 0.5246(3) 0.15572(19) 0.27132(15) 0.0457(8) Uani 1 1 d . . . S3 S 0.0601(4) 0.8697(2) -0.09722(16) 0.0433(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0227(2) 0.0193(2) 0.0242(3) 0.0117(2) 0.01024(19) 0.00791(18) Gd2 0.0259(3) 0.0212(3) 0.0247(3) 0.0116(2) 0.0090(2) 0.00932(19) C1 0.025(5) 0.009(4) 0.026(5) 0.002(4) 0.007(4) -0.003(4) C2 0.026(5) 0.018(5) 0.037(6) 0.006(4) 0.010(4) 0.007(4) C3 0.022(5) 0.034(6) 0.059(7) 0.025(6) 0.018(5) 0.006(4) C4 0.036(6) 0.022(6) 0.065(8) 0.021(5) 0.014(6) 0.014(5) C5 0.040(6) 0.028(6) 0.044(6) 0.021(5) 0.009(5) 0.012(5) C6 0.055(8) 0.035(7) 0.085(10) 0.035(7) 0.039(7) 0.018(6) C7 0.044(7) 0.043(7) 0.069(8) 0.035(6) 0.036(6) 0.026(5) C8 0.051(6) 0.007(4) 0.036(6) 0.009(4) 0.009(5) 0.012(4) C9 0.034(6) 0.019(5) 0.041(6) 0.012(5) 0.011(5) 0.011(4) C10 0.021(5) 0.020(5) 0.043(6) 0.016(5) 0.008(4) 0.008(4) C11 0.022(5) 0.039(6) 0.032(6) 0.001(5) 0.002(4) 0.005(4) C12 0.025(5) 0.039(7) 0.051(7) 0.011(6) 0.013(5) 0.008(5) C13 0.037(6) 0.019(5) 0.044(6) 0.000(5) 0.012(5) 0.009(4) C14 0.072(10) 0.048(9) 0.116(14) 0.007(9) 0.038(10) 0.033(8) C15 0.029(5) 0.021(5) 0.031(5) 0.005(4) 0.004(4) 0.002(4) C16 0.042(6) 0.027(5) 0.021(5) 0.007(4) 0.011(5) 0.017(5) C17 0.037(6) 0.032(6) 0.018(5) 0.012(4) 0.011(4) 0.014(4) C18 0.026(6) 0.039(6) 0.043(6) 0.006(5) 0.003(5) 0.007(5) C19 0.027(6) 0.063(8) 0.041(7) 0.011(6) -0.003(5) 0.013(5) C20 0.049(7) 0.043(7) 0.024(5) 0.004(5) -0.005(5) 0.019(5) C21 0.050(7) 0.030(6) 0.023(5) 0.008(4) 0.012(5) 0.015(5) C22 0.028(5) 0.039(6) 0.031(6) 0.011(5) 0.011(5) 0.012(5) C23 0.070(10) 0.096(13) 0.060(9) 0.029(9) -0.027(8) 0.007(9) C24 0.046(7) 0.052(7) 0.017(5) 0.019(5) 0.014(5) 0.021(5) C25 0.045(7) 0.055(8) 0.044(7) 0.039(6) 0.021(6) 0.010(6) C26 0.026(5) 0.059(8) 0.041(6) 0.032(6) 0.009(5) 0.009(5) C27 0.030(5) 0.029(5) 0.020(5) 0.009(4) 0.006(4) 0.015(4) C28 0.031(6) 0.067(8) 0.039(6) 0.033(6) 0.015(5) 0.019(5) C29 0.035(6) 0.083(10) 0.034(6) 0.028(7) 0.004(5) 0.017(6) C30 0.035(6) 0.023(5) 0.029(5) 0.012(4) 0.021(5) 0.015(4) C31 0.031(5) 0.032(6) 0.020(5) 0.017(4) 0.000(4) 0.009(4) C32 0.022(5) 0.027(5) 0.030(5) 0.014(4) 0.010(4) 0.007(4) C33 0.020(5) 0.060(7) 0.041(6) 0.032(6) 0.009(5) 0.022(5) C34 0.027(6) 0.072(9) 0.036(6) 0.029(6) 0.015(5) 0.010(6) C35 0.049(7) 0.050(8) 0.035(6) 0.019(6) 0.013(6) 0.000(6) C36 0.088(11) 0.109(14) 0.052(9) 0.037(9) 0.024(8) -0.037(10) C37 0.061(7) 0.031(6) 0.041(6) 0.021(5) 0.020(6) 0.024(5) C38 0.039(6) 0.038(6) 0.034(6) 0.020(5) 0.012(5) 0.019(5) C39 0.054(7) 0.028(6) 0.044(6) 0.023(5) 0.021(6) 0.025(5) C40 0.069(8) 0.039(7) 0.062(8) 0.029(6) 0.043(7) 0.040(6) C41 0.042(6) 0.051(7) 0.052(7) 0.030(6) 0.027(6) 0.032(6) C42 0.019(5) 0.028(5) 0.031(5) 0.017(4) 0.005(4) 0.012(4) C43 0.041(6) 0.036(6) 0.045(7) 0.020(5) 0.026(5) 0.020(5) C44 0.036(6) 0.040(6) 0.048(7) 0.026(6) 0.025(5) 0.013(5) C45 0.025(5) 0.025(5) 0.026(5) 0.010(4) 0.005(4) 0.006(4) O1 0.027(4) 0.030(4) 0.060(5) 0.019(4) 0.022(4) 0.004(3) O2 0.029(4) 0.025(4) 0.034(4) 0.010(3) 0.013(3) 0.017(3) O3 0.044(5) 0.055(6) 0.140(10) 0.060(6) 0.018(6) 0.021(4) O4 0.110(8) 0.044(5) 0.048(5) 0.025(5) 0.013(5) 0.000(5) O5 0.048(5) 0.027(4) 0.045(5) 0.019(4) 0.006(4) 0.003(3) O6 0.058(5) 0.031(5) 0.095(7) 0.012(5) 0.021(5) 0.027(4) O7 0.049(5) 0.015(4) 0.047(5) 0.011(3) 0.005(4) 0.006(3) O8 0.034(4) 0.027(4) 0.071(6) 0.014(4) 0.016(4) 0.015(3) O9 0.048(4) 0.044(5) 0.022(4) 0.013(3) 0.016(3) 0.019(4) O10 0.036(4) 0.055(5) 0.039(4) 0.028(4) 0.013(3) 0.024(4) O11 0.066(6) 0.080(7) 0.030(4) 0.018(4) -0.005(4) 0.030(5) O12 0.105(7) 0.049(5) 0.037(5) 0.019(4) 0.035(5) 0.034(5) O13 0.072(6) 0.053(5) 0.031(4) 0.019(4) 0.028(4) 0.014(4) O14 0.081(7) 0.158(12) 0.068(7) 0.072(8) 0.030(6) 0.066(8) O15 0.044(4) 0.043(5) 0.047(5) 0.031(4) 0.031(4) 0.021(4) O16 0.032(4) 0.034(4) 0.039(4) 0.021(3) 0.005(3) 0.012(3) O17 0.063(5) 0.029(4) 0.021(4) 0.005(3) 0.008(4) 0.011(4) O18 0.035(4) 0.077(6) 0.047(5) 0.037(5) 0.021(4) 0.017(4) O19 0.074(6) 0.071(7) 0.057(6) 0.044(5) 0.016(5) -0.012(5) O20 0.069(6) 0.031(4) 0.051(5) 0.014(4) 0.010(4) 0.016(4) O21 0.106(7) 0.039(5) 0.043(5) 0.022(4) 0.019(5) 0.043(5) O22 0.073(6) 0.056(6) 0.121(9) 0.054(6) 0.059(6) 0.027(5) O23 0.034(4) 0.040(4) 0.073(6) 0.038(4) 0.029(4) 0.018(3) O24 0.051(4) 0.035(4) 0.041(4) 0.024(4) 0.020(4) 0.026(4) O25 0.058(6) 0.101(8) 0.071(7) 0.014(6) 0.009(5) 0.045(6) O26 0.067(6) 0.041(5) 0.050(5) 0.006(4) 0.024(5) 0.024(4) O27 0.083(6) 0.050(6) 0.043(5) 0.009(4) 0.021(5) 0.008(5) S1 0.067(2) 0.068(2) 0.0346(16) 0.0338(16) 0.0210(15) 0.0354(18) S2 0.0487(17) 0.0272(15) 0.0554(19) 0.0227(14) 0.0018(15) 0.0013(13) S3 0.0567(18) 0.0312(15) 0.0588(19) 0.0280(15) 0.0249(16) 0.0217(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.320(6) . ? Gd1 O9 2.320(7) . ? Gd1 O24 2.345(7) 2_675 ? Gd1 O16 2.380(7) 2_766 ? Gd1 O18 2.388(7) 1_655 ? Gd1 O7 2.390(7) 1_665 ? Gd1 O26 2.455(7) . ? Gd1 O27 2.526(8) . ? Gd2 O15 2.287(6) 2_666 ? Gd2 O17 2.297(7) . ? Gd2 O23 2.339(6) 2_675 ? Gd2 O10 2.340(7) . ? Gd2 O2 2.378(6) . ? Gd2 O8 2.414(7) 1_565 ? Gd2 O25 2.415(10) . ? Gd2 O7 2.942(8) 1_565 ? C1 O1 1.240(11) . ? C1 O2 1.261(11) . ? C1 C2 1.511(13) . ? C2 C7 1.370(13) . ? C2 C3 1.381(14) . ? C3 C4 1.382(14) . ? C3 H3 0.9300 . ? C4 C5 1.387(15) . ? C4 H4 0.9300 . ? C5 C6 1.379(15) . ? C5 S2 1.737(10) . ? C6 C7 1.388(15) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.360(13) . ? C8 C13 1.402(14) . ? C8 O5 1.405(11) . ? C9 C10 1.400(13) . ? C9 H9 0.9300 . ? C10 C11 1.388(13) . ? C10 C15 1.478(13) . ? C11 C12 1.397(15) . ? C11 H11 0.9300 . ? C12 C13 1.372(14) . ? C12 H12 0.9300 . ? C13 O6 1.376(12) . ? C14 O6 1.436(15) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O8 1.263(11) . ? C15 O7 1.274(11) . ? C16 O9 1.262(11) . ? C16 O10 1.263(12) . ? C16 C17 1.499(13) . ? C17 C18 1.387(14) . ? C17 C22 1.407(13) . ? C18 C19 1.374(15) . ? C18 H18 0.9300 . ? C19 C20 1.391(16) . ? C19 H19 0.9300 . ? C20 O11 1.360(12) . ? C20 C21 1.388(15) . ? C21 C22 1.376(14) . ? C21 O13 1.413(12) . ? C22 H22 0.9300 . ? C23 O11 1.428(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.355(15) . ? C24 C29 1.376(15) . ? C24 S1 1.773(10) . ? C25 C26 1.389(14) . ? C25 H25 0.9300 . ? C26 C27 1.384(13) . ? C26 H26 0.9300 . ? C27 C28 1.365(13) . ? C27 C30 1.519(13) . ? C28 C29 1.370(15) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O16 1.238(11) . ? C30 O15 1.255(11) . ? C31 O18 1.241(12) . ? C31 O17 1.287(12) . ? C31 C32 1.488(12) . ? C32 C33 1.376(13) . ? C32 C38 1.383(13) . ? C33 C34 1.395(14) . ? C33 H33 0.9300 . ? C34 C35 1.367(17) . ? C34 H34 0.9300 . ? C35 O19 1.371(13) . ? C35 C37 1.405(16) . ? C36 O19 1.431(17) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.354(14) . ? C37 O21 1.418(13) . ? C38 H38 0.9300 . ? C39 C44 1.377(14) . ? C39 C40 1.385(15) . ? C39 S3 1.764(10) . ? C40 C41 1.390(15) . ? C40 H40 0.9300 . ? C41 C42 1.351(14) . ? C41 H41 0.9300 . ? C42 C43 1.412(13) . ? C42 C45 1.514(13) . ? C43 C44 1.382(14) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 O24 1.235(12) . ? C45 O23 1.264(11) . ? O3 S2 1.436(9) . ? O4 S2 1.409(10) . ? O5 S2 1.597(8) . ? O7 Gd1 2.390(7) 1_445 ? O7 Gd2 2.942(8) 1_545 ? O8 Gd2 2.414(7) 1_545 ? O12 S1 1.425(9) . ? O13 S1 1.606(9) . ? O14 S1 1.429(10) . ? O15 Gd2 2.287(6) 2_666 ? O16 Gd1 2.380(7) 2_766 ? O18 Gd1 2.388(7) 1_455 ? O20 S3 1.419(9) . ? O21 S3 1.601(9) . ? O22 S3 1.431(9) . ? O23 Gd2 2.339(6) 2_675 ? O24 Gd1 2.345(7) 2_675 ? O25 H25A 1.0153 . ? O25 H25B 1.0270 . ? O26 H26A 0.8545 . ? O26 H26B 0.8551 . ? O27 H27A 0.8830 . ? O27 H27B 0.8817 . ? 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 Gd1 O9 78.7(3) . . ? O1 Gd1 O24 94.2(3) . 2_675 ? O9 Gd1 O24 76.7(2) . 2_675 ? O1 Gd1 O16 84.3(2) . 2_766 ? O9 Gd1 O16 75.4(3) . 2_766 ? O24 Gd1 O16 151.8(3) 2_675 2_766 ? O1 Gd1 O18 135.7(3) . 1_655 ? O9 Gd1 O18 139.6(3) . 1_655 ? O24 Gd1 O18 79.8(3) 2_675 1_655 ? O16 Gd1 O18 120.3(3) 2_766 1_655 ? O1 Gd1 O7 152.5(3) . 1_665 ? O9 Gd1 O7 76.7(3) . 1_665 ? O24 Gd1 O7 91.9(2) 2_675 1_665 ? O16 Gd1 O7 77.8(2) 2_766 1_665 ? O18 Gd1 O7 71.8(3) 1_655 1_665 ? O1 Gd1 O26 79.6(3) . . ? O9 Gd1 O26 141.3(3) . . ? O24 Gd1 O26 136.7(3) 2_675 . ? O16 Gd1 O26 70.9(3) 2_766 . ? O18 Gd1 O26 75.8(3) 1_655 . ? O7 Gd1 O26 113.1(3) 1_665 . ? O1 Gd1 O27 70.6(3) . . ? O9 Gd1 O27 131.2(3) . . ? O24 Gd1 O27 68.9(3) 2_675 . ? O16 Gd1 O27 135.3(3) 2_766 . ? O18 Gd1 O27 66.2(3) 1_655 . ? O7 Gd1 O27 136.1(3) 1_665 . ? O26 Gd1 O27 68.6(3) . . ? O15 Gd2 O17 98.7(3) 2_666 . ? O15 Gd2 O23 170.9(2) 2_666 2_675 ? O17 Gd2 O23 88.3(3) . 2_675 ? O15 Gd2 O10 87.7(3) 2_666 . ? O17 Gd2 O10 147.2(3) . . ? O23 Gd2 O10 83.3(3) 2_675 . ? O15 Gd2 O2 80.0(2) 2_666 . ? O17 Gd2 O2 74.3(2) . . ? O23 Gd2 O2 96.6(2) 2_675 . ? O10 Gd2 O2 75.3(2) . . ? O15 Gd2 O8 113.4(2) 2_666 1_565 ? O17 Gd2 O8 76.3(3) . 1_565 ? O23 Gd2 O8 73.7(2) 2_675 1_565 ? O10 Gd2 O8 130.4(3) . 1_565 ? O2 Gd2 O8 149.2(3) . 1_565 ? O15 Gd2 O25 84.5(3) 2_666 . ? O17 Gd2 O25 144.7(3) . . ? O23 Gd2 O25 93.1(3) 2_675 . ? O10 Gd2 O25 67.7(3) . . ? O2 Gd2 O25 140.3(3) . . ? O8 Gd2 O25 70.3(3) 1_565 . ? O15 Gd2 O7 67.2(2) 2_666 1_565 ? O17 Gd2 O7 74.3(2) . 1_565 ? O23 Gd2 O7 120.6(2) 2_675 1_565 ? O10 Gd2 O7 136.5(2) . 1_565 ? O2 Gd2 O7 129.7(2) . 1_565 ? O8 Gd2 O7 47.2(2) 1_565 1_565 ? O25 Gd2 O7 74.7(3) . 1_565 ? O1 C1 O2 124.1(9) . . ? O1 C1 C2 117.9(9) . . ? O2 C1 C2 118.1(8) . . ? C7 C2 C3 119.8(9) . . ? C7 C2 C1 120.4(9) . . ? C3 C2 C1 119.8(9) . . ? C2 C3 C4 119.9(9) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.5(10) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 121.0(10) . . ? C6 C5 S2 119.5(8) . . ? C4 C5 S2 119.4(8) . . ? C5 C6 C7 118.3(11) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 121.3(10) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C13 121.2(9) . . ? C9 C8 O5 119.8(9) . . ? C13 C8 O5 119.0(9) . . ? C8 C9 C10 120.1(10) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.0(9) . . ? C11 C10 C15 121.8(9) . . ? C9 C10 C15 119.1(9) . . ? C10 C11 C12 120.4(10) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.2(10) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 O6 126.5(10) . . ? C12 C13 C8 119.1(9) . . ? O6 C13 C8 114.4(9) . . ? O6 C14 H14A 109.5 . . ? O6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O8 C15 O7 120.1(9) . . ? O8 C15 C10 118.9(8) . . ? O7 C15 C10 121.0(9) . . ? O9 C16 O10 125.6(9) . . ? O9 C16 C17 117.3(9) . . ? O10 C16 C17 117.0(9) . . ? C18 C17 C22 118.8(9) . . ? C18 C17 C16 121.1(9) . . ? C22 C17 C16 120.0(9) . . ? C19 C18 C17 120.8(11) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 121.4(10) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? O11 C20 C21 115.9(10) . . ? O11 C20 C19 126.7(10) . . ? C21 C20 C19 117.3(9) . . ? C22 C21 C20 122.7(10) . . ? C22 C21 O13 119.0(9) . . ? C20 C21 O13 118.2(9) . . ? C21 C22 C17 119.0(9) . . ? C21 C22 H22 120.5 . . ? C17 C22 H22 120.5 . . ? O11 C23 H23A 109.5 . . ? O11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 121.2(9) . . ? C25 C24 S1 119.0(8) . . ? C29 C24 S1 119.8(8) . . ? C24 C25 C26 119.2(10) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 119.5(10) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 120.2(9) . . ? C28 C27 C30 120.6(9) . . ? C26 C27 C30 119.1(8) . . ? C27 C28 C29 120.0(10) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 119.7(10) . . ? C28 C29 H29 120.2 . . ? C24 C29 H29 120.2 . . ? O16 C30 O15 124.9(9) . . ? O16 C30 C27 119.1(8) . . ? O15 C30 C27 116.0(9) . . ? O18 C31 O17 123.7(9) . . ? O18 C31 C32 118.1(9) . . ? O17 C31 C32 118.2(9) . . ? C33 C32 C38 119.6(9) . . ? C33 C32 C31 121.9(9) . . ? C38 C32 C31 118.4(9) . . ? C32 C33 C34 120.7(10) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 119.5(10) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.3 . . ? C34 C35 O19 125.8(11) . . ? C34 C35 C37 119.1(10) . . ? O19 C35 C37 115.1(12) . . ? O19 C36 H36A 109.5 . . ? O19 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O19 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C35 121.2(11) . . ? C38 C37 O21 120.2(10) . . ? C35 C37 O21 118.4(10) . . ? C37 C38 C32 119.8(10) . . ? C37 C38 H38 120.1 . . ? C32 C38 H38 120.1 . . ? C44 C39 C40 121.5(9) . . ? C44 C39 S3 120.1(8) . . ? C40 C39 S3 118.4(8) . . ? C39 C40 C41 118.1(10) . . ? C39 C40 H40 121.0 . . ? C41 C40 H40 121.0 . . ? C42 C41 C40 121.7(10) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C43 119.8(9) . . ? C41 C42 C45 122.8(9) . . ? C43 C42 C45 117.3(9) . . ? C44 C43 C42 119.3(10) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C39 C44 C43 119.6(9) . . ? C39 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? O24 C45 O23 125.0(9) . . ? O24 C45 C42 118.6(8) . . ? O23 C45 C42 116.3(9) . . ? C1 O1 Gd1 147.0(7) . . ? C1 O2 Gd2 131.0(6) . . ? C8 O5 S2 115.7(6) . . ? C13 O6 C14 117.8(10) . . ? C15 O7 Gd1 136.2(7) . 1_445 ? C15 O7 Gd2 83.1(6) . 1_545 ? Gd1 O7 Gd2 115.2(3) 1_445 1_545 ? C15 O8 Gd2 108.7(6) . 1_545 ? C16 O9 Gd1 148.5(7) . . ? C16 O10 Gd2 140.5(6) . . ? C20 O11 C23 117.6(10) . . ? C21 O13 S1 117.4(7) . . ? C30 O15 Gd2 155.2(7) . 2_666 ? C30 O16 Gd1 134.8(6) . 2_766 ? C31 O17 Gd2 133.1(6) . . ? C31 O18 Gd1 137.5(7) . 1_455 ? C35 O19 C36 116.3(12) . . ? C37 O21 S3 120.8(7) . . ? C45 O23 Gd2 154.8(7) . 2_675 ? C45 O24 Gd1 146.3(6) . 2_675 ? Gd2 O25 H25A 116.5 . . ? Gd2 O25 H25B 117.7 . . ? H25A O25 H25B 100.8 . . ? Gd1 O26 H26A 109.6 . . ? Gd1 O26 H26B 109.2 . . ? H26A O26 H26B 109.3 . . ? Gd1 O27 H27A 111.2 . . ? Gd1 O27 H27B 110.2 . . ? H27A O27 H27B 107.8 . . ? O12 S1 O14 119.3(7) . . ? O12 S1 O13 110.0(5) . . ? O14 S1 O13 107.7(6) . . ? O12 S1 C24 110.2(5) . . ? O14 S1 C24 109.5(6) . . ? O13 S1 C24 98.0(5) . . ? O4 S2 O3 120.1(7) . . ? O4 S2 O5 109.0(5) . . ? O3 S2 O5 107.9(5) . . ? O4 S2 C5 110.8(6) . . ? O3 S2 C5 110.2(5) . . ? O5 S2 C5 96.1(4) . . ? O20 S3 O22 119.1(6) . . ? O20 S3 O21 109.3(5) . . ? O22 S3 O21 107.0(6) . . ? O20 S3 C39 112.4(5) . . ? O22 S3 C39 108.9(5) . . ? O21 S3 C39 97.8(5) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.024 0.000 0.500 518 127 ' ' 2 0.214 0.321 0.059 34 11 ' ' 3 0.500 0.500 0.000 18 7 ' ' 4 0.786 0.679 0.941 34 11 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.184 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.177 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 905410' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 O27 S3 Tb2' _chemical_formula_weight 1422.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2574(19) _cell_length_b 15.601(3) _cell_length_c 22.274(4) _cell_angle_alpha 102.19(3) _cell_angle_beta 101.58(3) _cell_angle_gamma 104.32(3) _cell_volume 2936.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6026 _cell_measurement_theta_min 2.3514 _cell_measurement_theta_max 29.2334 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 2.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_T_max 0.6268 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19413 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10278 _reflns_number_gt 7845 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10278 _refine_ls_number_parameters 700 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _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 0.51526(3) 0.860583(19) 0.802175(13) 0.02307(9) Uani 1 1 d . . . Tb2 Tb 0.03181(3) 0.911887(18) 0.855819(13) 0.02160(9) Uani 1 1 d . . . C1 C 0.1739(7) 0.8770(4) 0.7232(3) 0.0251(13) Uani 1 1 d . . . C2 C 0.0911(7) 0.8760(4) 0.6575(3) 0.0250(13) Uani 1 1 d . . . C3 C -0.0698(7) 0.8504(4) 0.6387(3) 0.0368(16) Uani 1 1 d . . . H3 H -0.1260 0.8330 0.6667 0.044 Uiso 1 1 calc R . . C4 C -0.1455(7) 0.8505(5) 0.5796(3) 0.0406(17) Uani 1 1 d . . . H4 H -0.2529 0.8341 0.5680 0.049 Uiso 1 1 calc R . . C5 C -0.0648(8) 0.8746(4) 0.5362(3) 0.0365(16) Uani 1 1 d . . . C6 C 0.0961(8) 0.8977(4) 0.5560(3) 0.0355(16) Uani 1 1 d . . . C7 C 0.1734(7) 0.9000(4) 0.6158(3) 0.0301(15) Uani 1 1 d . . . H7 H 0.2809 0.9177 0.6280 0.036 Uiso 1 1 calc R . . C8 C -0.2899(9) 0.8470(6) 0.4526(4) 0.084(3) Uani 1 1 d . . . H8A H -0.3281 0.7831 0.4507 0.126 Uiso 1 1 calc R . . H8B H -0.3185 0.8548 0.4107 0.126 Uiso 1 1 calc R . . H8C H -0.3338 0.8823 0.4804 0.126 Uiso 1 1 calc R . . C9 C 0.2176(7) 0.8953(5) 0.4015(3) 0.0360(17) Uani 1 1 d . . . C10 C 0.0743(8) 0.8816(5) 0.3617(3) 0.0456(19) Uani 1 1 d . . . H10 H -0.0151 0.8493 0.3699 0.055 Uiso 1 1 calc R . . C11 C 0.0653(7) 0.9171(4) 0.3086(3) 0.0415(18) Uani 1 1 d . . . H11 H -0.0306 0.9082 0.2813 0.050 Uiso 1 1 calc R . . C12 C 0.1973(7) 0.9646(4) 0.2970(3) 0.0256(14) Uani 1 1 d . . . C13 C 0.3397(7) 0.9789(5) 0.3391(3) 0.0429(18) Uani 1 1 d . . . H13 H 0.4296 1.0116 0.3315 0.051 Uiso 1 1 calc R . . C14 C 0.3500(7) 0.9461(5) 0.3908(3) 0.0467(19) Uani 1 1 d . . . H14 H 0.4459 0.9577 0.4190 0.056 Uiso 1 1 calc R . . C15 C 0.1898(7) 1.0054(4) 0.2413(3) 0.0233(13) Uani 1 1 d . . . C16 C 0.2123(7) 0.7454(4) 0.8554(3) 0.0286(15) Uani 1 1 d . . . C17 C 0.1782(7) 0.6509(4) 0.8690(3) 0.0258(14) Uani 1 1 d . . . C18 C 0.0609(7) 0.6246(4) 0.8963(3) 0.0369(17) Uani 1 1 d . . . H18 H 0.0048 0.6646 0.9073 0.044 Uiso 1 1 calc R . . C19 C 0.0253(7) 0.5401(4) 0.9077(3) 0.0380(17) Uani 1 1 d . . . H19 H -0.0527 0.5229 0.9273 0.046 Uiso 1 1 calc R . . C20 C 0.1064(7) 0.4808(4) 0.8896(3) 0.0340(16) Uani 1 1 d . . . C21 C 0.2255(8) 0.5061(4) 0.8622(3) 0.0426(19) Uani 1 1 d . . . H21 H 0.2809 0.4659 0.8510 0.051 Uiso 1 1 calc R . . C22 C 0.2612(7) 0.5916(4) 0.8516(3) 0.0402(18) Uani 1 1 d . . . H22 H 0.3406 0.6096 0.8328 0.048 Uiso 1 1 calc R . . C23 C 0.2716(8) 0.3321(4) 0.9816(3) 0.0368(16) Uani 1 1 d . . . C24 C 0.2179(7) 0.2706(4) 1.0136(3) 0.0314(15) Uani 1 1 d . . . H24 H 0.1222 0.2651 1.0222 0.038 Uiso 1 1 calc R . . C25 C 0.3055(6) 0.2165(4) 1.0334(3) 0.0259(14) Uani 1 1 d . . . C26 C 0.4425(7) 0.2239(5) 1.0180(3) 0.0388(17) Uani 1 1 d . . . H26 H 0.5013 0.1870 1.0303 0.047 Uiso 1 1 calc R . . C27 C 0.4962(7) 0.2837(5) 0.9850(3) 0.0414(18) Uani 1 1 d . . . H27 H 0.5891 0.2858 0.9746 0.050 Uiso 1 1 calc R . . C28 C 0.4140(8) 0.3413(5) 0.9670(3) 0.0402(17) Uani 1 1 d . . . C29 C 0.2477(7) 0.1536(4) 1.0711(3) 0.0295(15) Uani 1 1 d . . . C30 C 0.6058(9) 0.4204(6) 0.9236(4) 0.090(3) Uani 1 1 d . . . H30A H 0.6839 0.4554 0.9624 0.135 Uiso 1 1 calc R . . H30B H 0.6110 0.4538 0.8921 0.135 Uiso 1 1 calc R . . H30C H 0.6226 0.3623 0.9084 0.135 Uiso 1 1 calc R . . C31 C 0.7060(7) 0.7270(4) 0.7872(3) 0.0295(14) Uani 1 1 d . . . C32 C 0.7554(6) 0.6435(4) 0.7711(3) 0.0258(14) Uani 1 1 d . . . C33 C 0.6754(7) 0.5633(4) 0.7824(3) 0.0304(15) Uani 1 1 d . . . H33 H 0.5942 0.5630 0.8012 0.036 Uiso 1 1 calc R . . C34 C 0.7155(7) 0.4855(4) 0.7660(3) 0.0293(14) Uani 1 1 d . . . C35 C 0.8350(7) 0.4814(4) 0.7383(3) 0.0377(16) Uani 1 1 d . . . C36 C 0.9135(7) 0.5617(4) 0.7261(3) 0.0371(16) Uani 1 1 d . . . H36 H 0.9934 0.5611 0.7066 0.045 Uiso 1 1 calc R . . C37 C 0.8759(7) 0.6412(4) 0.7420(3) 0.0334(15) Uani 1 1 d . . . H37 H 0.9302 0.6939 0.7335 0.040 Uiso 1 1 calc R . . C38 C 0.9834(10) 0.3910(5) 0.6947(4) 0.076(3) Uani 1 1 d . . . H38A H 0.9500 0.3932 0.6515 0.114 Uiso 1 1 calc R . . H38B H 1.0016 0.3330 0.6948 0.114 Uiso 1 1 calc R . . H38C H 1.0773 0.4401 0.7164 0.114 Uiso 1 1 calc R . . C39 C 0.4451(7) 0.2518(4) 0.7627(3) 0.0351(16) Uani 1 1 d . . . C40 C 0.3276(7) 0.2363(4) 0.7922(3) 0.0360(16) Uani 1 1 d . . . H40 H 0.2620 0.2728 0.7926 0.043 Uiso 1 1 calc R . . C41 C 0.3089(6) 0.1663(4) 0.8208(3) 0.0318(15) Uani 1 1 d . . . H41 H 0.2284 0.1544 0.8400 0.038 Uiso 1 1 calc R . . C42 C 0.4085(6) 0.1130(4) 0.8215(3) 0.0249(13) Uani 1 1 d . . . C43 C 0.5252(8) 0.1300(4) 0.7919(3) 0.047(2) Uani 1 1 d . . . H43 H 0.5913 0.0938 0.7918 0.056 Uiso 1 1 calc R . . C44 C 0.5459(8) 0.1998(5) 0.7624(4) 0.052(2) Uani 1 1 d . . . H44 H 0.6256 0.2114 0.7428 0.063 Uiso 1 1 calc R . . C45 C 0.3896(7) 0.0359(4) 0.8544(3) 0.0273(14) Uani 1 1 d . . . O1 O 0.0938(5) 0.8631(3) 0.76197(19) 0.0395(12) Uani 1 1 d . . . O2 O 0.3163(4) 0.8909(3) 0.7351(2) 0.0373(11) Uani 1 1 d . . . O3 O -0.1259(6) 0.8777(4) 0.4762(2) 0.0570(14) Uani 1 1 d . . . O4 O 0.1828(5) 0.9262(3) 0.5135(2) 0.0473(13) Uani 1 1 d . . . O5 O 0.1100(6) 0.7638(3) 0.4523(2) 0.0595(15) Uani 1 1 d . . . O6 O 0.3827(6) 0.8564(4) 0.4952(3) 0.078(2) Uani 1 1 d . . . O7 O 0.0605(4) 1.0019(3) 0.21015(19) 0.0326(10) Uani 1 1 d . . . O8 O 0.3152(5) 1.0380(3) 0.2286(2) 0.0365(11) Uani 1 1 d . . . O9 O 0.1365(5) 0.7952(3) 0.87350(19) 0.0348(11) Uani 1 1 d . . . O10 O 0.3126(5) 0.7637(3) 0.8251(2) 0.0401(12) Uani 1 1 d . . . O11 O -0.0851(6) 0.3508(4) 0.9179(3) 0.0758(19) Uani 1 1 d . . . O12 O 0.0889(5) 0.3056(3) 0.8579(2) 0.0494(13) Uani 1 1 d . . . O13 O 0.1901(6) 0.3944(3) 0.9682(2) 0.0538(14) Uani 1 1 d . . . O14 O 0.4960(4) -0.0004(3) 0.86226(19) 0.0299(10) Uani 1 1 d . . . O15 O 0.2696(4) 0.0164(3) 0.8729(2) 0.0377(11) Uani 1 1 d . . . O16 O 0.1138(5) 0.1467(3) 1.0779(2) 0.0449(13) Uani 1 1 d . . . O17 O 0.3368(5) 0.1138(3) 1.09625(19) 0.0370(11) Uani 1 1 d . . . O18 O 0.3639(6) 0.3915(4) 0.7371(3) 0.0775(19) Uani 1 1 d . . . O19 O 0.6353(5) 0.4043(3) 0.7794(2) 0.0371(11) Uani 1 1 d . . . O20 O 0.4496(6) 0.7636(4) 0.6923(2) 0.0766(18) Uani 1 1 d . . . H20A H 0.3727 0.7123 0.6853 0.115 Uiso 1 1 d R . . H20B H 0.4193 0.7934 0.6645 0.115 Uiso 1 1 d R . . O21 O 0.0080(6) 1.0491(3) 0.9234(2) 0.0559(14) Uani 1 1 d . . . H21A H -0.0867 1.0485 0.9148 0.084 Uiso 1 1 d R . . H21B H 0.0381 1.0499 0.9625 0.084 Uiso 1 1 d R . . O22 O 0.5779(5) 0.7196(3) 0.7998(2) 0.0418(12) Uani 1 1 d . . . O23 O 0.1865(6) 0.9498(4) 0.9713(2) 0.0697(16) Uani 1 1 d . . . H23A H 0.1547 0.9051 0.9863 0.105 Uiso 1 1 d R . . H23B H 0.2816 0.9584 0.9728 0.105 Uiso 1 1 d R . . O24 O 0.4547(6) 0.4049(3) 0.9356(2) 0.0613(15) Uani 1 1 d . . . O25 O 0.7950(5) 0.8058(3) 0.7896(2) 0.0396(11) Uani 1 1 d . . . O26 O 0.8663(5) 0.4008(3) 0.7264(3) 0.0562(14) Uani 1 1 d . . . O27 O 0.5032(7) 0.3189(3) 0.6687(2) 0.0714(16) Uani 1 1 d . . . S1 S 0.2266(2) 0.84955(14) 0.46758(8) 0.0476(5) Uani 1 1 d . . . S2 S 0.0608(2) 0.37061(12) 0.90340(9) 0.0433(5) Uani 1 1 d . . . S3 S 0.4759(2) 0.34457(12) 0.72949(10) 0.0461(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02808(17) 0.02087(17) 0.02421(18) 0.01020(14) 0.00911(14) 0.00925(13) Tb2 0.02417(16) 0.01996(17) 0.02620(18) 0.01202(14) 0.01079(14) 0.00833(13) C1 0.038(4) 0.019(3) 0.021(3) 0.005(3) 0.009(3) 0.014(3) C2 0.031(3) 0.023(3) 0.017(3) 0.003(3) 0.002(3) 0.007(3) C3 0.035(4) 0.039(4) 0.032(4) 0.009(4) 0.006(3) 0.008(3) C4 0.025(3) 0.052(5) 0.036(4) 0.005(4) -0.001(3) 0.011(3) C5 0.046(4) 0.035(4) 0.021(4) 0.000(3) -0.008(3) 0.018(3) C6 0.049(4) 0.037(4) 0.027(4) 0.012(3) 0.014(3) 0.019(4) C7 0.026(3) 0.039(4) 0.023(4) 0.010(3) 0.005(3) 0.007(3) C8 0.068(6) 0.092(8) 0.061(6) 0.021(6) -0.040(5) 0.014(6) C9 0.042(4) 0.058(5) 0.017(3) 0.015(4) 0.010(3) 0.025(4) C10 0.057(5) 0.050(5) 0.040(4) 0.029(4) 0.026(4) 0.009(4) C11 0.035(4) 0.048(5) 0.038(4) 0.024(4) 0.005(3) 0.000(3) C12 0.037(3) 0.027(3) 0.024(3) 0.014(3) 0.016(3) 0.016(3) C13 0.035(4) 0.063(5) 0.042(4) 0.032(4) 0.018(4) 0.015(4) C14 0.035(4) 0.082(6) 0.033(4) 0.028(4) 0.008(3) 0.024(4) C15 0.029(3) 0.018(3) 0.030(4) 0.007(3) 0.013(3) 0.014(3) C16 0.037(4) 0.029(4) 0.029(4) 0.015(3) 0.013(3) 0.018(3) C17 0.035(3) 0.024(3) 0.027(4) 0.013(3) 0.008(3) 0.018(3) C18 0.045(4) 0.033(4) 0.051(5) 0.024(4) 0.023(4) 0.025(3) C19 0.040(4) 0.050(4) 0.045(4) 0.031(4) 0.028(4) 0.022(4) C20 0.043(4) 0.033(4) 0.040(4) 0.021(4) 0.017(3) 0.023(3) C21 0.054(4) 0.039(4) 0.063(5) 0.031(4) 0.036(4) 0.033(4) C22 0.047(4) 0.043(4) 0.056(5) 0.030(4) 0.032(4) 0.030(4) C23 0.056(4) 0.027(4) 0.034(4) 0.015(3) 0.014(4) 0.016(3) C24 0.036(4) 0.041(4) 0.030(4) 0.017(3) 0.021(3) 0.021(3) C25 0.029(3) 0.025(3) 0.022(3) 0.007(3) 0.004(3) 0.005(3) C26 0.032(4) 0.058(5) 0.034(4) 0.016(4) 0.009(3) 0.023(4) C27 0.026(3) 0.066(5) 0.035(4) 0.020(4) 0.013(3) 0.009(4) C28 0.045(4) 0.043(4) 0.029(4) 0.017(4) 0.010(3) 0.001(4) C29 0.040(4) 0.032(4) 0.018(3) 0.009(3) 0.008(3) 0.011(3) C30 0.074(6) 0.108(8) 0.060(6) 0.038(6) 0.021(5) -0.036(5) C31 0.036(4) 0.022(4) 0.026(4) 0.004(3) -0.001(3) 0.010(3) C32 0.026(3) 0.026(3) 0.025(3) 0.009(3) 0.002(3) 0.010(3) C33 0.036(4) 0.024(4) 0.030(4) 0.004(3) 0.011(3) 0.008(3) C34 0.037(4) 0.015(3) 0.031(4) 0.008(3) 0.003(3) 0.003(3) C35 0.036(4) 0.025(4) 0.052(5) 0.007(4) 0.007(4) 0.016(3) C36 0.031(4) 0.035(4) 0.045(4) 0.004(4) 0.015(3) 0.011(3) C37 0.034(4) 0.031(4) 0.031(4) 0.010(3) 0.006(3) 0.005(3) C38 0.094(7) 0.056(6) 0.104(8) 0.022(6) 0.045(6) 0.053(6) C39 0.044(4) 0.020(4) 0.037(4) 0.009(3) 0.005(3) 0.005(3) C40 0.026(3) 0.026(4) 0.060(5) 0.018(4) 0.011(3) 0.012(3) C41 0.024(3) 0.029(4) 0.042(4) 0.008(3) 0.010(3) 0.006(3) C42 0.030(3) 0.013(3) 0.031(4) 0.007(3) 0.008(3) 0.004(3) C43 0.055(4) 0.033(4) 0.085(6) 0.034(4) 0.048(5) 0.032(4) C44 0.067(5) 0.043(5) 0.080(6) 0.039(5) 0.053(5) 0.030(4) C45 0.032(3) 0.018(3) 0.023(4) 0.000(3) 0.006(3) -0.001(3) O1 0.056(3) 0.049(3) 0.025(3) 0.015(2) 0.018(2) 0.028(3) O2 0.029(2) 0.049(3) 0.038(3) 0.023(3) 0.002(2) 0.015(2) O3 0.071(3) 0.073(4) 0.026(3) 0.015(3) -0.007(3) 0.034(3) O4 0.074(3) 0.050(3) 0.025(3) 0.018(3) 0.024(3) 0.017(3) O5 0.107(4) 0.042(3) 0.041(3) 0.022(3) 0.032(3) 0.023(3) O6 0.074(4) 0.134(6) 0.068(4) 0.070(4) 0.030(3) 0.065(4) O7 0.031(2) 0.034(3) 0.038(3) 0.022(2) 0.007(2) 0.013(2) O8 0.036(2) 0.044(3) 0.048(3) 0.029(3) 0.023(2) 0.021(2) O9 0.053(3) 0.031(3) 0.036(3) 0.022(2) 0.021(2) 0.024(2) O10 0.038(3) 0.039(3) 0.060(3) 0.031(3) 0.026(3) 0.014(2) O11 0.076(4) 0.056(4) 0.135(6) 0.057(4) 0.069(4) 0.031(3) O12 0.068(3) 0.034(3) 0.051(3) 0.014(3) 0.015(3) 0.022(3) O13 0.095(4) 0.040(3) 0.042(3) 0.020(3) 0.018(3) 0.042(3) O14 0.032(2) 0.026(2) 0.038(3) 0.012(2) 0.008(2) 0.017(2) O15 0.029(2) 0.034(3) 0.052(3) 0.014(2) 0.018(2) 0.004(2) O16 0.035(3) 0.064(3) 0.045(3) 0.038(3) 0.011(2) 0.012(2) O17 0.054(3) 0.032(3) 0.031(3) 0.017(2) 0.005(2) 0.023(2) O18 0.056(3) 0.058(4) 0.140(6) 0.064(4) 0.023(4) 0.027(3) O19 0.044(3) 0.023(2) 0.042(3) 0.016(2) 0.005(2) 0.005(2) O20 0.096(4) 0.100(5) 0.045(3) 0.011(4) 0.010(3) 0.062(4) O21 0.075(4) 0.055(3) 0.038(3) 0.000(3) 0.019(3) 0.027(3) O22 0.030(2) 0.027(3) 0.063(3) 0.006(3) 0.006(2) 0.010(2) O23 0.078(4) 0.072(4) 0.058(4) 0.020(3) 0.012(3) 0.023(3) O24 0.073(4) 0.055(4) 0.051(3) 0.032(3) 0.019(3) -0.005(3) O25 0.049(3) 0.015(2) 0.046(3) 0.006(2) 0.003(2) 0.002(2) O26 0.053(3) 0.031(3) 0.096(4) 0.017(3) 0.027(3) 0.026(3) O27 0.104(4) 0.042(3) 0.045(4) 0.015(3) 0.006(3) -0.010(3) S1 0.0707(13) 0.0629(14) 0.0302(11) 0.0289(11) 0.0233(10) 0.0353(12) S2 0.0562(12) 0.0347(11) 0.0579(13) 0.0295(10) 0.0272(11) 0.0231(9) S3 0.0500(11) 0.0288(10) 0.0549(13) 0.0233(10) 0.0037(10) 0.0020(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 O8 2.259(4) 2_676 ? Tb1 O17 2.293(4) 2_667 ? Tb1 O10 2.318(4) . ? Tb1 O2 2.339(4) . ? Tb1 O14 2.364(4) 1_565 ? Tb1 O22 2.401(4) . ? Tb1 O20 2.457(5) . ? Tb2 O15 2.297(4) 1_565 ? Tb2 O1 2.303(4) . ? Tb2 O9 2.331(4) . ? Tb2 O7 2.365(4) 2_576 ? Tb2 O16 2.366(4) 2_567 ? Tb2 O25 2.366(5) 1_455 ? Tb2 O21 2.429(4) . ? Tb2 O23 2.545(5) . ? C1 O2 1.244(6) . ? C1 O1 1.265(6) . ? C1 C2 1.504(7) . ? C2 C7 1.369(7) . ? C2 C3 1.392(8) . ? C3 C4 1.362(8) . ? C3 H3 0.9300 . ? C4 C5 1.392(8) . ? C4 H4 0.9300 . ? C5 O3 1.358(7) . ? C5 C6 1.395(8) . ? C6 C7 1.367(8) . ? C6 O4 1.430(6) . ? C7 H7 0.9300 . ? C8 O3 1.423(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.377(9) . ? C9 C14 1.380(8) . ? C9 S1 1.763(6) . ? C10 C11 1.405(7) . ? C10 H10 0.9300 . ? C11 C12 1.368(7) . ? C11 H11 0.9300 . ? C12 C13 1.392(8) . ? C12 C15 1.507(7) . ? C13 C14 1.350(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.239(6) . ? C15 O8 1.258(6) . ? C16 O9 1.228(6) . ? C16 O10 1.265(6) . ? C16 C17 1.538(7) . ? C17 C18 1.367(7) . ? C17 C22 1.383(7) . ? C18 C19 1.368(8) . ? C18 H18 0.9300 . ? C19 C20 1.375(7) . ? C19 H19 0.9300 . ? C20 C21 1.378(7) . ? C20 S2 1.773(6) . ? C21 C22 1.376(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.370(7) . ? C23 C28 1.400(8) . ? C23 O13 1.412(7) . ? C24 C25 1.385(7) . ? C24 H24 0.9300 . ? C25 C26 1.364(7) . ? C25 C29 1.491(7) . ? C26 C27 1.365(8) . ? C26 H26 0.9300 . ? C27 C28 1.384(8) . ? C27 H27 0.9300 . ? C28 O24 1.352(7) . ? C29 O16 1.259(6) . ? C29 O17 1.263(6) . ? C30 O24 1.447(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 O22 1.255(6) . ? C31 O25 1.283(7) . ? C31 C32 1.484(7) . ? C32 C33 1.387(7) . ? C32 C37 1.402(7) . ? C33 C34 1.355(7) . ? C33 H33 0.9300 . ? C34 C35 1.379(7) . ? C34 O19 1.425(6) . ? C35 O26 1.343(7) . ? C35 C36 1.395(8) . ? C36 C37 1.364(8) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O26 1.429(7) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.377(7) . ? C39 C44 1.379(8) . ? C39 S3 1.749(6) . ? C40 C41 1.369(7) . ? C40 H40 0.9300 . ? C41 C42 1.386(7) . ? C41 H41 0.9300 . ? C42 C43 1.375(7) . ? C42 C45 1.527(7) . ? C43 C44 1.381(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 O15 1.251(6) . ? C45 O14 1.254(6) . ? O4 S1 1.592(5) . ? O5 S1 1.420(5) . ? O6 S1 1.420(5) . ? O7 Tb2 2.365(4) 2_576 ? O8 Tb1 2.259(4) 2_676 ? O11 S2 1.426(4) . ? O12 S2 1.388(5) . ? O13 S2 1.585(5) . ? O14 Tb1 2.364(4) 1_545 ? O15 Tb2 2.297(4) 1_545 ? O16 Tb2 2.366(4) 2_567 ? O17 Tb1 2.293(4) 2_667 ? O18 S3 1.427(5) . ? O19 S3 1.582(5) . ? O20 H20A 0.8910 . ? O20 H20B 0.8899 . ? O21 H21A 0.8561 . ? O21 H21B 0.8554 . ? O23 H23A 0.8504 . ? O23 H23B 0.8500 . ? O25 Tb2 2.366(5) 1_655 ? O27 S3 1.419(5) . ? 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 O8 Tb1 O17 97.59(15) 2_676 2_667 ? O8 Tb1 O10 171.28(13) 2_676 . ? O17 Tb1 O10 89.25(15) 2_667 . ? O8 Tb1 O2 87.79(14) 2_676 . ? O17 Tb1 O2 147.89(14) 2_667 . ? O10 Tb1 O2 83.55(14) . . ? O8 Tb1 O14 80.49(14) 2_676 1_565 ? O17 Tb1 O14 73.95(14) 2_667 1_565 ? O10 Tb1 O14 96.33(14) . 1_565 ? O2 Tb1 O14 75.82(15) . 1_565 ? O8 Tb1 O22 112.89(13) 2_676 . ? O17 Tb1 O22 76.49(15) 2_667 . ? O10 Tb1 O22 73.90(13) . . ? O2 Tb1 O22 130.26(16) . . ? O14 Tb1 O22 148.96(14) 1_565 . ? O8 Tb1 O20 85.40(19) 2_676 . ? O17 Tb1 O20 143.47(15) 2_667 . ? O10 Tb1 O20 92.32(19) . . ? O2 Tb1 O20 68.30(16) . . ? O14 Tb1 O20 141.82(15) 1_565 . ? O22 Tb1 O20 68.99(17) . . ? O15 Tb2 O1 78.33(16) 1_565 . ? O15 Tb2 O9 93.45(14) 1_565 . ? O1 Tb2 O9 77.28(13) . . ? O15 Tb2 O7 84.96(14) 1_565 2_576 ? O1 Tb2 O7 75.40(14) . 2_576 ? O9 Tb2 O7 152.38(14) . 2_576 ? O15 Tb2 O16 134.96(16) 1_565 2_567 ? O1 Tb2 O16 140.29(17) . 2_567 ? O9 Tb2 O16 79.40(14) . 2_567 ? O7 Tb2 O16 120.50(13) 2_576 2_567 ? O15 Tb2 O25 152.98(15) 1_565 1_455 ? O1 Tb2 O25 77.38(16) . 1_455 ? O9 Tb2 O25 92.61(15) . 1_455 ? O7 Tb2 O25 77.63(14) 2_576 1_455 ? O16 Tb2 O25 72.05(15) 2_567 1_455 ? O15 Tb2 O21 77.98(16) 1_565 . ? O1 Tb2 O21 140.67(15) . . ? O9 Tb2 O21 135.03(16) . . ? O7 Tb2 O21 71.64(16) 2_576 . ? O16 Tb2 O21 76.68(16) 2_567 . ? O25 Tb2 O21 114.89(16) 1_455 . ? O15 Tb2 O23 69.81(17) 1_565 . ? O1 Tb2 O23 130.94(16) . . ? O9 Tb2 O23 68.72(16) . . ? O7 Tb2 O23 134.81(16) 2_576 . ? O16 Tb2 O23 66.17(17) 2_567 . ? O25 Tb2 O23 136.48(16) 1_455 . ? O21 Tb2 O23 66.89(17) . . ? O2 C1 O1 124.9(5) . . ? O2 C1 C2 117.4(5) . . ? O1 C1 C2 117.7(5) . . ? C7 C2 C3 119.5(5) . . ? C7 C2 C1 120.3(5) . . ? C3 C2 C1 120.2(5) . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 121.2(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? O3 C5 C4 127.0(6) . . ? O3 C5 C6 116.2(6) . . ? C4 C5 C6 116.8(6) . . ? C7 C6 C5 122.5(5) . . ? C7 C6 O4 119.1(6) . . ? C5 C6 O4 118.2(5) . . ? C6 C7 C2 119.5(6) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 120.6(5) . . ? C10 C9 S1 118.3(5) . . ? C14 C9 S1 121.0(5) . . ? C9 C10 C11 118.9(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.1(5) . . ? C11 C12 C15 120.9(5) . . ? C13 C12 C15 119.9(5) . . ? C14 C13 C12 121.4(6) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C9 119.7(6) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? O7 C15 O8 124.8(5) . . ? O7 C15 C12 117.7(5) . . ? O8 C15 C12 117.5(5) . . ? O9 C16 O10 126.1(5) . . ? O9 C16 C17 116.8(5) . . ? O10 C16 C17 117.1(5) . . ? C18 C17 C22 120.4(5) . . ? C18 C17 C16 119.1(5) . . ? C22 C17 C16 120.4(5) . . ? C17 C18 C19 120.6(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 119.0(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 121.2(5) . . ? C19 C20 S2 119.6(4) . . ? C21 C20 S2 119.1(4) . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C17 119.6(5) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? C24 C23 C28 121.6(5) . . ? C24 C23 O13 119.7(5) . . ? C28 C23 O13 118.5(5) . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 118.2(5) . . ? C26 C25 C29 122.8(5) . . ? C24 C25 C29 119.0(5) . . ? C25 C26 C27 122.2(5) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C28 120.8(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? O24 C28 C27 127.1(6) . . ? O24 C28 C23 115.9(6) . . ? C27 C28 C23 117.0(5) . . ? O16 C29 O17 124.2(5) . . ? O16 C29 C25 117.1(5) . . ? O17 C29 C25 118.6(5) . . ? O24 C30 H30A 109.5 . . ? O24 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O24 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O22 C31 O25 120.8(5) . . ? O22 C31 C32 119.1(5) . . ? O25 C31 C32 120.1(5) . . ? C33 C32 C37 118.5(5) . . ? C33 C32 C31 119.1(5) . . ? C37 C32 C31 122.3(5) . . ? C34 C33 C32 119.9(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 123.0(5) . . ? C33 C34 O19 119.4(5) . . ? C35 C34 O19 117.6(5) . . ? O26 C35 C34 117.0(5) . . ? O26 C35 C36 126.1(5) . . ? C34 C35 C36 116.9(5) . . ? C37 C36 C35 121.5(5) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C32 120.1(5) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? O26 C38 H38A 109.5 . . ? O26 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O26 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 121.8(5) . . ? C40 C39 S3 119.2(5) . . ? C44 C39 S3 118.9(5) . . ? C41 C40 C39 119.0(5) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C40 C41 C42 120.7(5) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C43 C42 C41 119.2(5) . . ? C43 C42 C45 119.9(5) . . ? C41 C42 C45 120.9(5) . . ? C42 C43 C44 121.2(5) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C39 C44 C43 118.2(5) . . ? C39 C44 H44 120.9 . . ? C43 C44 H44 120.9 . . ? O15 C45 O14 125.6(5) . . ? O15 C45 C42 116.3(5) . . ? O14 C45 C42 118.0(5) . . ? C1 O1 Tb2 150.8(4) . . ? C1 O2 Tb1 140.4(3) . . ? C5 O3 C8 117.5(6) . . ? C6 O4 S1 117.6(4) . . ? C15 O7 Tb2 134.7(3) . 2_576 ? C15 O8 Tb1 155.4(3) . 2_676 ? C16 O9 Tb2 145.8(3) . . ? C16 O10 Tb1 153.9(4) . . ? C23 O13 S2 121.7(4) . . ? C45 O14 Tb1 129.9(4) . 1_545 ? C45 O15 Tb2 146.1(4) . 1_545 ? C29 O16 Tb2 136.1(4) . 2_567 ? C29 O17 Tb1 133.6(4) . 2_667 ? C34 O19 S3 116.2(4) . . ? Tb1 O20 H20A 111.5 . . ? Tb1 O20 H20B 110.8 . . ? H20A O20 H20B 107.4 . . ? Tb2 O21 H21A 109.6 . . ? Tb2 O21 H21B 109.3 . . ? H21A O21 H21B 109.2 . . ? C31 O22 Tb1 109.3(3) . . ? Tb2 O23 H23A 109.2 . . ? Tb2 O23 H23B 109.1 . . ? H23A O23 H23B 109.5 . . ? C28 O24 C30 117.3(6) . . ? C31 O25 Tb2 137.8(4) . 1_655 ? C35 O26 C38 119.5(5) . . ? O5 S1 O6 119.5(3) . . ? O5 S1 O4 109.6(3) . . ? O6 S1 O4 107.3(3) . . ? O5 S1 C9 110.8(3) . . ? O6 S1 C9 109.2(3) . . ? O4 S1 C9 98.4(3) . . ? O12 S2 O11 119.4(3) . . ? O12 S2 O13 108.3(3) . . ? O11 S2 O13 107.2(3) . . ? O12 S2 C20 112.0(3) . . ? O11 S2 C20 109.4(3) . . ? O13 S2 C20 98.1(3) . . ? O27 S3 O18 119.6(4) . . ? O27 S3 O19 108.5(3) . . ? O18 S3 O19 108.4(3) . . ? O27 S3 C39 111.2(3) . . ? O18 S3 C39 110.2(3) . . ? O19 S3 C39 96.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -7.2(8) . . . . ? O1 C1 C2 C7 173.2(5) . . . . ? O2 C1 C2 C3 172.5(5) . . . . ? O1 C1 C2 C3 -7.0(8) . . . . ? C7 C2 C3 C4 -1.1(9) . . . . ? C1 C2 C3 C4 179.1(6) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C3 C4 C5 O3 -179.9(6) . . . . ? C3 C4 C5 C6 0.6(10) . . . . ? O3 C5 C6 C7 178.2(6) . . . . ? C4 C5 C6 C7 -2.2(10) . . . . ? O3 C5 C6 O4 2.7(9) . . . . ? C4 C5 C6 O4 -177.7(5) . . . . ? C5 C6 C7 C2 2.2(10) . . . . ? O4 C6 C7 C2 177.6(5) . . . . ? C3 C2 C7 C6 -0.5(9) . . . . ? C1 C2 C7 C6 179.2(5) . . . . ? C14 C9 C10 C11 2.4(10) . . . . ? S1 C9 C10 C11 -179.6(5) . . . . ? C9 C10 C11 C12 -0.2(10) . . . . ? C10 C11 C12 C13 -1.3(10) . . . . ? C10 C11 C12 C15 -178.4(6) . . . . ? C11 C12 C13 C14 0.6(10) . . . . ? C15 C12 C13 C14 177.6(6) . . . . ? C12 C13 C14 C9 1.7(11) . . . . ? C10 C9 C14 C13 -3.2(11) . . . . ? S1 C9 C14 C13 178.8(5) . . . . ? C11 C12 C15 O7 6.7(8) . . . . ? C13 C12 C15 O7 -170.3(6) . . . . ? C11 C12 C15 O8 -171.2(6) . . . . ? C13 C12 C15 O8 11.7(8) . . . . ? O9 C16 C17 C18 4.2(9) . . . . ? O10 C16 C17 C18 -174.0(6) . . . . ? O9 C16 C17 C22 -178.4(6) . . . . ? O10 C16 C17 C22 3.4(9) . . . . ? C22 C17 C18 C19 0.9(10) . . . . ? C16 C17 C18 C19 178.4(6) . . . . ? C17 C18 C19 C20 -1.7(11) . . . . ? C18 C19 C20 C21 2.0(11) . . . . ? C18 C19 C20 S2 -179.5(5) . . . . ? C19 C20 C21 C22 -1.4(11) . . . . ? S2 C20 C21 C22 -179.9(6) . . . . ? C20 C21 C22 C17 0.5(11) . . . . ? C18 C17 C22 C21 -0.3(10) . . . . ? C16 C17 C22 C21 -177.7(6) . . . . ? C28 C23 C24 C25 1.0(10) . . . . ? O13 C23 C24 C25 -172.7(6) . . . . ? C23 C24 C25 C26 -2.4(10) . . . . ? C23 C24 C25 C29 176.9(6) . . . . ? C24 C25 C26 C27 1.3(10) . . . . ? C29 C25 C26 C27 -178.0(6) . . . . ? C25 C26 C27 C28 1.4(11) . . . . ? C26 C27 C28 O24 178.5(7) . . . . ? C26 C27 C28 C23 -2.8(11) . . . . ? C24 C23 C28 O24 -179.5(6) . . . . ? O13 C23 C28 O24 -5.8(9) . . . . ? C24 C23 C28 C27 1.6(10) . . . . ? O13 C23 C28 C27 175.3(6) . . . . ? C26 C25 C29 O16 -174.1(6) . . . . ? C24 C25 C29 O16 6.6(9) . . . . ? C26 C25 C29 O17 8.6(9) . . . . ? C24 C25 C29 O17 -170.6(6) . . . . ? O22 C31 C32 C33 -12.6(8) . . . . ? O25 C31 C32 C33 165.8(6) . . . . ? O22 C31 C32 C37 164.2(6) . . . . ? O25 C31 C32 C37 -17.3(9) . . . . ? C37 C32 C33 C34 0.7(9) . . . . ? C31 C32 C33 C34 177.7(6) . . . . ? C32 C33 C34 C35 0.4(10) . . . . ? C32 C33 C34 O19 178.3(5) . . . . ? C33 C34 C35 O26 177.7(6) . . . . ? O19 C34 C35 O26 -0.2(9) . . . . ? C33 C34 C35 C36 -1.4(10) . . . . ? O19 C34 C35 C36 -179.3(6) . . . . ? O26 C35 C36 C37 -177.7(6) . . . . ? C34 C35 C36 C37 1.3(10) . . . . ? C35 C36 C37 C32 -0.2(10) . . . . ? C33 C32 C37 C36 -0.8(9) . . . . ? C31 C32 C37 C36 -177.7(6) . . . . ? C44 C39 C40 C41 -1.2(11) . . . . ? S3 C39 C40 C41 -176.8(5) . . . . ? C39 C40 C41 C42 1.5(10) . . . . ? C40 C41 C42 C43 -1.3(10) . . . . ? C40 C41 C42 C45 179.0(6) . . . . ? C41 C42 C43 C44 0.9(11) . . . . ? C45 C42 C43 C44 -179.4(7) . . . . ? C40 C39 C44 C43 0.8(12) . . . . ? S3 C39 C44 C43 176.4(6) . . . . ? C42 C43 C44 C39 -0.7(12) . . . . ? C43 C42 C45 O15 -170.9(6) . . . . ? C41 C42 C45 O15 8.8(9) . . . . ? C43 C42 C45 O14 11.2(9) . . . . ? C41 C42 C45 O14 -169.1(6) . . . . ? O2 C1 O1 Tb2 63.2(10) . . . . ? C2 C1 O1 Tb2 -117.3(7) . . . . ? O15 Tb2 O1 C1 -16.4(7) 1_565 . . . ? O9 Tb2 O1 C1 -112.7(8) . . . . ? O7 Tb2 O1 C1 71.4(7) 2_576 . . . ? O16 Tb2 O1 C1 -168.1(7) 2_567 . . . ? O25 Tb2 O1 C1 151.7(8) 1_455 . . . ? O21 Tb2 O1 C1 37.6(9) . . . . ? O23 Tb2 O1 C1 -66.2(8) . . . . ? O1 C1 O2 Tb1 25.1(10) . . . . ? C2 C1 O2 Tb1 -154.4(4) . . . . ? O8 Tb1 O2 C1 -168.3(6) 2_676 . . . ? O17 Tb1 O2 C1 -67.5(7) 2_667 . . . ? O10 Tb1 O2 C1 10.7(6) . . . . ? O14 Tb1 O2 C1 -87.5(6) 1_565 . . . ? O22 Tb1 O2 C1 73.2(6) . . . . ? O20 Tb1 O2 C1 105.8(6) . . . . ? C4 C5 O3 C8 -4.8(10) . . . . ? C6 C5 O3 C8 174.7(6) . . . . ? C7 C6 O4 S1 91.1(7) . . . . ? C5 C6 O4 S1 -93.3(6) . . . . ? O8 C15 O7 Tb2 -26.3(9) . . . 2_576 ? C12 C15 O7 Tb2 155.9(4) . . . 2_576 ? O7 C15 O8 Tb1 40.2(14) . . . 2_676 ? C12 C15 O8 Tb1 -142.0(8) . . . 2_676 ? O10 C16 O9 Tb2 26.5(12) . . . . ? C17 C16 O9 Tb2 -151.5(5) . . . . ? O15 Tb2 O9 C16 -62.4(8) 1_565 . . . ? O1 Tb2 O9 C16 14.8(8) . . . . ? O7 Tb2 O9 C16 23.3(9) 2_576 . . . ? O16 Tb2 O9 C16 162.4(8) 2_567 . . . ? O25 Tb2 O9 C16 91.2(8) 1_455 . . . ? O21 Tb2 O9 C16 -138.9(7) . . . . ? O23 Tb2 O9 C16 -129.2(8) . . . . ? O9 C16 O10 Tb1 38.7(13) . . . . ? C17 C16 O10 Tb1 -143.3(7) . . . . ? O8 Tb1 O10 C16 -80.5(14) 2_676 . . . ? O17 Tb1 O10 C16 61.4(9) 2_667 . . . ? O2 Tb1 O10 C16 -87.2(9) . . . . ? O14 Tb1 O10 C16 -12.4(9) 1_565 . . . ? O22 Tb1 O10 C16 137.6(9) . . . . ? O20 Tb1 O10 C16 -155.1(9) . . . . ? C24 C23 O13 S2 -91.9(7) . . . . ? C28 C23 O13 S2 94.3(7) . . . . ? O15 C45 O14 Tb1 83.1(7) . . . 1_545 ? C42 C45 O14 Tb1 -99.2(6) . . . 1_545 ? O14 C45 O15 Tb2 -75.1(10) . . . 1_545 ? C42 C45 O15 Tb2 107.1(7) . . . 1_545 ? O17 C29 O16 Tb2 11.6(10) . . . 2_567 ? C25 C29 O16 Tb2 -165.4(4) . . . 2_567 ? O16 C29 O17 Tb1 -75.3(8) . . . 2_667 ? C25 C29 O17 Tb1 101.7(6) . . . 2_667 ? C33 C34 O19 S3 82.7(6) . . . . ? C35 C34 O19 S3 -99.3(6) . . . . ? O25 C31 O22 Tb1 13.0(7) . . . . ? C32 C31 O22 Tb1 -168.5(4) . . . . ? O8 Tb1 O22 C31 6.3(4) 2_676 . . . ? O17 Tb1 O22 C31 -86.4(4) 2_667 . . . ? O10 Tb1 O22 C31 -179.6(4) . . . . ? O2 Tb1 O22 C31 113.9(4) . . . . ? O14 Tb1 O22 C31 -104.5(4) 1_565 . . . ? O20 Tb1 O22 C31 81.5(4) . . . . ? C27 C28 O24 C30 -5.3(11) . . . . ? C23 C28 O24 C30 176.0(6) . . . . ? O22 C31 O25 Tb2 108.2(6) . . . 1_655 ? C32 C31 O25 Tb2 -70.2(8) . . . 1_655 ? C34 C35 O26 C38 176.7(7) . . . . ? C36 C35 O26 C38 -4.3(11) . . . . ? C6 O4 S1 O5 30.9(5) . . . . ? C6 O4 S1 O6 -100.2(5) . . . . ? C6 O4 S1 C9 146.5(5) . . . . ? C10 C9 S1 O5 35.8(6) . . . . ? C14 C9 S1 O5 -146.2(6) . . . . ? C10 C9 S1 O6 169.4(6) . . . . ? C14 C9 S1 O6 -12.5(7) . . . . ? C10 C9 S1 O4 -78.9(6) . . . . ? C14 C9 S1 O4 99.1(6) . . . . ? C23 O13 S2 O12 -23.9(5) . . . . ? C23 O13 S2 O11 106.3(5) . . . . ? C23 O13 S2 C20 -140.4(4) . . . . ? C19 C20 S2 O12 149.6(6) . . . . ? C21 C20 S2 O12 -31.9(7) . . . . ? C19 C20 S2 O11 14.7(7) . . . . ? C21 C20 S2 O11 -166.7(6) . . . . ? C19 C20 S2 O13 -96.8(6) . . . . ? C21 C20 S2 O13 81.7(6) . . . . ? C34 O19 S3 O27 57.8(5) . . . . ? C34 O19 S3 O18 -73.4(4) . . . . ? C34 O19 S3 C39 172.8(4) . . . . ? C40 C39 S3 O27 -136.6(6) . . . . ? C44 C39 S3 O27 47.6(7) . . . . ? C40 C39 S3 O18 -1.7(7) . . . . ? C44 C39 S3 O18 -177.5(6) . . . . ? C40 C39 S3 O19 110.6(6) . . . . ? C44 C39 S3 O19 -65.1(6) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.081 0.500 0.500 481 104 ' ' 2 0.251 0.823 0.069 16 8 ' ' 3 0.749 0.176 0.931 16 8 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.788 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.125 #===end data_5 _database_code_depnum_ccdc_archive 'CCDC 905411' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H0.50 Dy2 O27 S3' _chemical_formula_weight 1394.13 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1999(6) _cell_length_b 15.578(3) _cell_length_c 22.142(5) _cell_angle_alpha 102.856(17) _cell_angle_beta 101.552(12) _cell_angle_gamma 104.517(12) _cell_volume 2882.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1747 _cell_measurement_theta_min 2.3711 _cell_measurement_theta_max 28.8218 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1333 _exptl_absorpt_coefficient_mu 2.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6082 _exptl_absorpt_correction_T_max 0.6082 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19158 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10062 _reflns_number_gt 6402 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10062 _refine_ls_number_parameters 700 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.011 _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 Dy1 Dy 0.52922(5) 0.41287(3) 0.35775(2) 0.01652(14) Uani 1 1 d . . . Dy2 Dy 0.01408(5) 0.36223(3) 0.30430(2) 0.01633(14) Uani 1 1 d . . . S1 S -0.0252(3) -0.15626(19) 0.22927(14) 0.0270(7) Uani 1 1 d . . . S2 S 0.5496(3) -0.1323(2) 0.40031(14) 0.0276(7) Uani 1 1 d . . . S3 S 0.7291(3) 0.3511(2) -0.03211(13) 0.0266(7) Uani 1 1 d . . . O1 O 0.5069(8) 0.5488(5) 0.4248(3) 0.0295(19) Uani 1 1 d . . . H1A H 0.4179 0.5543 0.4103 0.044 Uiso 1 1 d R . . H1B H 0.5163 0.5440 0.4628 0.044 Uiso 1 1 d R . . O2 O 0.4406(7) 0.4984(4) 0.2909(3) 0.0185(16) Uani 1 1 d . . . O3 O -0.2327(7) -0.4830(4) 0.3731(3) 0.0228(17) Uani 1 1 d . . . O4 O 0.5890(8) 0.3602(5) 0.2627(3) 0.0260(18) Uani 1 1 d . . . O5 O 0.2885(8) 0.3073(5) 0.2916(3) 0.0263(18) Uani 1 1 d . . . O7 O 0.6294(8) 0.2949(4) 0.3752(3) 0.0263(19) Uani 1 1 d . . . O8 O 0.6848(10) 0.4499(6) 0.4729(4) 0.057(3) Uani 1 1 d . . . H8A H 0.6651 0.4011 0.4851 0.085 Uiso 1 1 d R . . H8B H 0.7817 0.4687 0.4753 0.085 Uiso 1 1 d R . . O9 O 0.8092(7) 0.2655(5) 0.3264(3) 0.0240(18) Uani 1 1 d . . . O10 O -0.0005(7) -0.4968(4) 0.3655(3) 0.0144(15) Uani 1 1 d . . . O11 O 0.8160(7) 0.3937(4) 0.2385(3) 0.0208(17) Uani 1 1 d . . . O12 O -0.0471(8) 0.2683(6) 0.1939(3) 0.044(2) Uani 1 1 d . . . H12A H -0.1078 0.2134 0.1888 0.066 Uiso 1 1 d R . . H12B H -0.0941 0.2935 0.1682 0.066 Uiso 1 1 d R . . O13 O 0.3769(8) 0.3798(5) -0.0241(3) 0.0308(19) Uani 1 1 d . . . O14 O 0.6856(7) 0.4286(5) 0.0150(3) 0.0248(18) Uani 1 1 d . . . O15 O 0.6082(8) 0.2646(5) -0.0476(3) 0.0293(19) Uani 1 1 d . . . O16 O 0.8870(8) 0.3566(6) -0.0046(3) 0.039(2) Uani 1 1 d . . . O17 O 0.1841(7) 0.4643(5) 0.2735(3) 0.0238(18) Uani 1 1 d . . . O18 O 0.0714(7) 0.2189(5) 0.3018(3) 0.030(2) Uani 1 1 d . . . O19 O 0.3694(8) -0.0981(5) 0.2254(4) 0.0304(19) Uani 1 1 d . . . O20 O 0.1379(7) -0.0941(5) 0.2804(3) 0.0215(17) Uani 1 1 d . . . O21 O 0.0007(9) -0.1831(5) 0.1679(3) 0.042(2) Uani 1 1 d . . . O22 O -0.1400(8) -0.1093(5) 0.2363(4) 0.039(2) Uani 1 1 d . . . O23 O 0.4006(8) -0.1526(5) 0.4135(4) 0.037(2) Uani 1 1 d . . . O24 O 0.5805(8) -0.1981(5) 0.3534(3) 0.0279(18) Uani 1 1 d . . . O25 O 0.6781(9) -0.1081(5) 0.4671(3) 0.036(2) Uani 1 1 d . . . O26 O 0.9462(8) -0.0912(5) 0.4342(3) 0.038(2) Uani 1 1 d . . . O27 O 0.1542(7) 0.3862(5) 0.4068(3) 0.0271(18) Uani 1 1 d U . . O28 O 0.3826(7) 0.3578(5) 0.4255(3) 0.0293(19) Uani 1 1 d . . . C1 C 0.6683(10) 0.3769(6) 0.2242(4) 0.011(2) Uani 1 1 d U . . C2 C 0.5914(11) 0.3780(6) 0.1589(4) 0.014(2) Uani 1 1 d . . . C3 C 0.4248(10) 0.3515(6) 0.1387(4) 0.014(2) Uani 1 1 d . . . H3 H 0.3671 0.3345 0.1665 0.017 Uiso 1 1 calc R . . C4 C 0.3508(12) 0.3510(7) 0.0792(5) 0.027(3) Uani 1 1 d . . . H4 H 0.2424 0.3338 0.0665 0.032 Uiso 1 1 calc R . . C5 C 0.4360(12) 0.3761(7) 0.0366(5) 0.022(3) Uani 1 1 d . . . C6 C 0.6003(11) 0.4021(7) 0.0567(5) 0.019(2) Uani 1 1 d . . . C7 C 0.6742(10) 0.4023(7) 0.1182(4) 0.017(2) Uani 1 1 d . . . H7 H 0.7825 0.4195 0.1314 0.020 Uiso 1 1 calc R . . C8 C 0.2108(12) 0.3531(9) -0.0467(5) 0.048(4) Uani 1 1 d . . . H8C H 0.1818 0.3584 -0.0895 0.072 Uiso 1 1 calc R . . H8D H 0.1721 0.3928 -0.0188 0.072 Uiso 1 1 calc R . . H8E H 0.1670 0.2902 -0.0471 0.072 Uiso 1 1 calc R . . C9 C 0.7181(10) 0.3956(7) -0.0977(5) 0.017(2) Uani 1 1 d U . . C10 C 0.8541(11) 0.4451(7) -0.1088(5) 0.025(3) Uani 1 1 d . . . H10 H 0.9509 0.4556 -0.0808 0.030 Uiso 1 1 calc R . . C11 C 0.8432(12) 0.4784(7) -0.1618(5) 0.026(3) Uani 1 1 d . . . H11 H 0.9341 0.5103 -0.1697 0.032 Uiso 1 1 calc R . . C12 C 0.5641(11) 0.4175(7) -0.1923(5) 0.024(3) Uani 1 1 d . . . H12 H 0.4674 0.4092 -0.2196 0.029 Uiso 1 1 calc R . . C13 C 0.5734(11) 0.3816(7) -0.1396(5) 0.023(3) Uani 1 1 d . . . H13 H 0.4826 0.3483 -0.1324 0.028 Uiso 1 1 calc R . . C14 C 0.3096(11) 0.4960(7) 0.2601(5) 0.016(2) Uani 1 1 d . . . C15 C 0.6997(10) 0.4655(7) -0.2038(5) 0.015(2) Uani 1 1 d . . . C16 C -0.1111(10) -0.4616(6) 0.3559(4) 0.013(2) Uani 1 1 d . . . C17 C 0.2045(12) 0.2301(8) 0.2897(5) 0.028(3) Uani 1 1 d . . . C18 C 0.2528(10) 0.1446(7) 0.2713(5) 0.015(2) Uani 1 1 d . . . C19 C 0.3738(10) 0.1452(7) 0.2419(4) 0.021(2) Uani 1 1 d . . . H19 H 0.4280 0.1985 0.2338 0.025 Uiso 1 1 calc R . . C20 C 0.4100(11) 0.0639(7) 0.2253(5) 0.020(2) Uani 1 1 d . . . H20 H 0.4896 0.0633 0.2052 0.024 Uiso 1 1 calc R . . C21 C 0.3344(11) -0.0161(7) 0.2369(5) 0.022(2) Uani 1 1 d U . . C22 C 0.2157(10) -0.0146(7) 0.2672(4) 0.015(2) Uani 1 1 d . . . C23 C 0.1735(10) 0.0644(7) 0.2840(4) 0.017(2) Uani 1 1 d . . . H23 H 0.0931 0.0644 0.3037 0.021 Uiso 1 1 calc R . . C24 C 0.4850(12) -0.1062(8) 0.1923(6) 0.047(4) Uani 1 1 d . . . H24A H 0.4510 -0.1008 0.1498 0.070 Uiso 1 1 calc R . . H24B H 0.5012 -0.1653 0.1895 0.070 Uiso 1 1 calc R . . H24C H 0.5810 -0.0579 0.2154 0.070 Uiso 1 1 calc R . . C25 C -0.0544(11) -0.2485(7) 0.2630(5) 0.022(3) Uani 1 1 d . . . C26 C 0.0441(12) -0.3009(8) 0.2621(5) 0.034(3) Uani 1 1 d . . . H26 H 0.1214 -0.2912 0.2407 0.040 Uiso 1 1 calc R . . C27 C 0.0268(11) -0.3682(7) 0.2932(5) 0.022(2) Uani 1 1 d U . . H27 H 0.0971 -0.4020 0.2948 0.026 Uiso 1 1 calc R . . C28 C -0.0933(10) -0.3873(7) 0.3226(4) 0.014(2) Uani 1 1 d . . . C29 C -0.1945(10) -0.3319(6) 0.3222(4) 0.013(2) Uani 1 1 d U . . H29 H -0.2738 -0.3419 0.3426 0.016 Uiso 1 1 calc R . . C30 C -0.1755(10) -0.2644(6) 0.2922(4) 0.014(2) Uani 1 1 d . . . H30 H -0.2431 -0.2289 0.2911 0.017 Uiso 1 1 calc R . . C31 C 0.7054(11) 0.2459(7) 0.3557(5) 0.020(2) Uani 1 1 d . . . C32 C 0.6725(11) 0.1511(8) 0.3694(5) 0.023(3) Uani 1 1 d . . . C33 C 0.7550(13) 0.0906(7) 0.3506(5) 0.032(3) Uani 1 1 d . . . H33 H 0.8355 0.1092 0.3322 0.039 Uiso 1 1 calc R . . C34 C 0.7174(12) 0.0016(7) 0.3593(5) 0.031(3) Uani 1 1 d . . . H34 H 0.7709 -0.0397 0.3468 0.037 Uiso 1 1 calc R . . C35 C 0.5960(11) -0.0217(7) 0.3876(5) 0.020(2) Uani 1 1 d . . . C36 C 0.5163(11) 0.0399(7) 0.4063(4) 0.022(3) Uani 1 1 d . . . H36 H 0.4370 0.0229 0.4257 0.026 Uiso 1 1 calc R . . C37 C 0.5538(11) 0.1254(7) 0.3964(5) 0.023(3) Uani 1 1 d . . . H37 H 0.4984 0.1659 0.4080 0.028 Uiso 1 1 calc R . . C38 C 0.7611(11) -0.1694(7) 0.4791(5) 0.021(2) Uani 1 1 d U . . C39 C 0.9071(13) -0.1566(8) 0.4643(6) 0.033(3) Uani 1 1 d . . . C40 C 0.9490(11) -0.2727(7) 0.5165(4) 0.021(3) Uani 1 1 d . . . H40 H 1.0109 -0.3081 0.5287 0.026 Uiso 1 1 calc R . . C41 C 0.8051(11) -0.2846(7) 0.5303(4) 0.017(2) Uani 1 1 d . . . C42 C 0.7114(11) -0.2318(7) 0.5105(5) 0.020(2) Uani 1 1 d . . . H42 H 0.6146 -0.2397 0.5189 0.024 Uiso 1 1 calc R . . C43 C 0.2498(11) 0.3475(7) 0.4322(5) 0.019(2) Uani 1 1 d . . . C44 C 1.0985(14) -0.0714(10) 0.4239(6) 0.075(5) Uani 1 1 d . . . H44A H 1.1064 -0.1253 0.3953 0.112 Uiso 1 1 calc R . . H44B H 1.1757 -0.0547 0.4643 0.112 Uiso 1 1 calc R . . H44C H 1.1154 -0.0211 0.4051 0.112 Uiso 1 1 calc R . . C74 C 1.0005(11) -0.2090(7) 0.4851(5) 0.022(3) Uani 1 1 d . . . H74 H 1.0983 -0.2006 0.4776 0.027 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 Dy1 0.0192(3) 0.0134(3) 0.0220(3) 0.0087(2) 0.0108(2) 0.0064(2) Dy2 0.0187(3) 0.0145(3) 0.0183(3) 0.0068(2) 0.0063(2) 0.0066(2) S1 0.0296(16) 0.0178(16) 0.0301(18) 0.0090(14) 0.0018(14) 0.0043(14) S2 0.0335(17) 0.0223(16) 0.0315(18) 0.0106(14) 0.0121(14) 0.0113(14) S3 0.0305(16) 0.0356(19) 0.0198(17) 0.0124(14) 0.0100(13) 0.0143(15) O1 0.045(5) 0.032(5) 0.023(5) 0.010(4) 0.018(4) 0.022(4) O2 0.023(4) 0.013(4) 0.021(4) 0.002(3) 0.004(3) 0.012(3) O3 0.018(4) 0.015(4) 0.035(5) 0.003(4) 0.011(3) 0.006(3) O4 0.038(4) 0.028(5) 0.017(4) 0.005(4) 0.011(4) 0.019(4) O5 0.032(4) 0.019(4) 0.026(5) 0.004(4) 0.006(4) 0.006(4) O7 0.036(4) 0.014(4) 0.044(5) 0.014(4) 0.023(4) 0.019(4) O8 0.061(6) 0.065(7) 0.045(6) 0.007(5) 0.014(5) 0.025(5) O9 0.029(4) 0.030(5) 0.030(5) 0.023(4) 0.014(4) 0.022(4) O10 0.017(4) 0.014(4) 0.014(4) 0.005(3) 0.008(3) 0.006(3) O11 0.020(4) 0.022(4) 0.021(4) 0.014(4) 0.003(3) 0.003(3) O12 0.054(5) 0.062(6) 0.027(5) 0.008(4) 0.005(4) 0.043(5) O13 0.027(4) 0.040(5) 0.018(4) -0.001(4) -0.003(4) 0.012(4) O14 0.031(4) 0.027(4) 0.010(4) 0.000(3) 0.005(3) 0.002(4) O15 0.035(4) 0.026(5) 0.028(5) 0.008(4) 0.015(4) 0.007(4) O16 0.037(5) 0.058(6) 0.038(5) 0.030(5) 0.013(4) 0.027(5) O17 0.016(4) 0.020(4) 0.042(5) 0.016(4) 0.015(4) 0.005(3) O18 0.013(4) 0.020(4) 0.056(6) 0.006(4) 0.008(4) 0.010(3) O19 0.030(4) 0.015(4) 0.060(6) 0.019(4) 0.023(4) 0.014(4) O20 0.019(4) 0.016(4) 0.030(5) 0.014(4) 0.008(3) 0.000(3) O21 0.065(6) 0.029(5) 0.018(5) 0.008(4) 0.003(4) -0.001(4) O22 0.031(4) 0.033(5) 0.057(6) 0.023(5) 0.006(4) 0.013(4) O23 0.028(4) 0.021(4) 0.070(6) 0.020(4) 0.026(4) 0.006(4) O24 0.038(4) 0.024(4) 0.027(5) 0.010(4) 0.013(4) 0.014(4) O25 0.063(5) 0.036(5) 0.022(5) 0.013(4) 0.015(4) 0.032(5) O26 0.041(5) 0.035(5) 0.023(5) 0.011(4) 0.011(4) -0.020(4) O27 0.0280(19) 0.026(2) 0.027(2) 0.0088(11) 0.0061(11) 0.0089(11) O28 0.014(4) 0.044(5) 0.033(5) 0.024(4) 0.007(3) 0.003(4) C1 0.011(2) 0.011(2) 0.012(2) 0.0030(11) 0.0027(11) 0.0039(12) C2 0.023(5) 0.008(5) 0.013(6) 0.004(4) 0.008(5) 0.002(5) C3 0.012(5) 0.014(6) 0.011(6) 0.003(5) 0.001(4) -0.006(5) C4 0.021(6) 0.022(7) 0.035(7) 0.004(6) 0.009(5) 0.005(5) C5 0.031(6) 0.024(7) 0.007(6) -0.002(5) -0.004(5) 0.015(5) C6 0.026(6) 0.022(6) 0.016(6) 0.009(5) 0.014(5) 0.010(5) C7 0.014(5) 0.023(6) 0.015(6) 0.015(5) 0.002(4) 0.004(5) C8 0.042(8) 0.063(10) 0.024(8) 0.008(7) -0.014(6) 0.013(7) C9 0.017(2) 0.017(2) 0.016(2) 0.0042(11) 0.0049(12) 0.0051(12) C10 0.021(6) 0.027(7) 0.024(7) 0.007(5) 0.002(5) 0.009(5) C11 0.030(6) 0.025(7) 0.021(7) 0.001(5) 0.002(5) 0.010(6) C12 0.025(6) 0.028(7) 0.018(6) 0.006(5) 0.005(5) 0.006(5) C13 0.013(5) 0.029(7) 0.028(7) 0.014(6) 0.008(5) 0.002(5) C14 0.019(6) 0.013(6) 0.020(6) 0.005(5) 0.009(5) 0.008(5) C15 0.011(5) 0.018(6) 0.019(6) 0.004(5) 0.009(5) 0.009(5) C16 0.014(5) 0.012(6) 0.013(6) 0.005(5) 0.003(4) 0.004(5) C17 0.026(6) 0.026(7) 0.024(7) -0.001(6) -0.006(5) 0.010(6) C18 0.007(5) 0.015(6) 0.022(6) 0.007(5) -0.001(4) 0.003(5) C19 0.013(5) 0.022(6) 0.024(6) 0.006(5) 0.003(5) 0.001(5) C20 0.016(5) 0.016(6) 0.026(7) 0.004(5) 0.009(5) 0.000(5) C21 0.023(3) 0.022(3) 0.023(3) 0.0058(12) 0.0060(12) 0.0076(13) C22 0.015(5) 0.012(6) 0.013(6) 0.006(5) 0.000(4) -0.005(5) C23 0.017(5) 0.023(6) 0.016(6) 0.004(5) 0.003(5) 0.012(5) C24 0.040(7) 0.040(8) 0.050(9) -0.016(7) 0.008(6) 0.024(7) C25 0.020(6) 0.017(6) 0.021(6) 0.005(5) -0.003(5) 0.002(5) C26 0.030(7) 0.034(7) 0.047(8) 0.012(6) 0.031(6) 0.012(6) C27 0.022(3) 0.022(3) 0.022(3) 0.0065(12) 0.0062(12) 0.0074(12) C28 0.014(5) 0.020(6) 0.009(5) -0.001(5) 0.007(4) 0.006(5) C29 0.013(2) 0.013(2) 0.013(2) 0.0042(11) 0.0039(11) 0.0034(12) C30 0.010(5) 0.011(5) 0.016(6) 0.000(5) 0.002(4) 0.000(4) C31 0.015(5) 0.022(6) 0.017(6) 0.005(5) -0.008(5) 0.002(5) C32 0.012(5) 0.032(7) 0.016(6) 0.001(5) -0.005(5) 0.004(5) C33 0.047(7) 0.018(6) 0.048(8) 0.025(6) 0.029(7) 0.012(6) C34 0.045(7) 0.026(7) 0.051(8) 0.029(6) 0.036(6) 0.028(6) C35 0.017(5) 0.022(6) 0.025(6) 0.013(5) 0.003(5) 0.007(5) C36 0.020(6) 0.031(7) 0.011(6) 0.010(5) 0.003(5) -0.002(5) C37 0.032(6) 0.028(7) 0.021(6) 0.015(5) 0.015(5) 0.016(6) C38 0.021(3) 0.020(3) 0.021(3) 0.0063(12) 0.0055(12) 0.0063(12) C39 0.035(7) 0.023(7) 0.032(8) 0.001(6) 0.014(6) -0.005(6) C40 0.017(5) 0.029(7) 0.013(6) 0.003(5) -0.003(5) 0.007(5) C41 0.029(6) 0.013(6) 0.006(5) 0.002(4) 0.001(5) 0.007(5) C42 0.019(5) 0.021(6) 0.024(6) 0.014(5) 0.000(5) 0.010(5) C43 0.020(6) 0.022(6) 0.010(6) 0.006(5) 0.000(5) -0.001(5) C44 0.055(9) 0.086(12) 0.040(10) -0.004(9) 0.018(8) -0.040(9) C74 0.012(5) 0.031(7) 0.022(6) 0.010(5) 0.007(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O3 2.284(6) 1_665 ? Dy1 O4 2.307(6) . ? Dy1 O7 2.323(6) . ? Dy1 O5 2.358(7) . ? Dy1 O2 2.360(6) . ? Dy1 O28 2.368(6) . ? Dy1 O1 2.381(6) . ? Dy1 O8 2.520(8) . ? Dy2 O17 2.259(6) . ? Dy2 O27 2.273(7) . ? Dy2 O9 2.310(7) 1_455 ? Dy2 O11 2.321(6) 1_455 ? Dy2 O10 2.362(6) 1_565 ? Dy2 O18 2.411(7) . ? Dy2 O12 2.425(7) . ? Dy2 O5 2.906(6) . ? S1 O21 1.415(7) . ? S1 O22 1.442(7) . ? S1 O20 1.605(7) . ? S1 C25 1.749(11) . ? S2 O24 1.415(6) . ? S2 O23 1.432(6) . ? S2 O25 1.599(8) . ? S2 C35 1.766(10) . ? S3 O16 1.431(7) . ? S3 O15 1.435(7) . ? S3 O14 1.599(6) . ? S3 C9 1.739(10) . ? O2 C14 1.247(10) . ? O3 C16 1.244(10) . ? O3 Dy1 2.284(6) 1_445 ? O4 C1 1.258(10) . ? O5 C17 1.242(13) . ? O7 C31 1.225(10) . ? O9 C31 1.272(11) . ? O9 Dy2 2.310(7) 1_655 ? O10 C16 1.274(10) . ? O10 Dy2 2.362(6) 1_545 ? O11 C1 1.276(9) . ? O11 Dy2 2.321(6) 1_655 ? O13 C5 1.365(11) . ? O13 C8 1.428(11) . ? O14 C6 1.390(10) . ? O17 C14 1.258(10) . ? O18 C17 1.283(11) . ? O19 C21 1.377(11) . ? O19 C24 1.421(10) . ? O20 C22 1.390(11) . ? O25 C38 1.400(11) . ? O26 C39 1.352(13) . ? O26 C44 1.432(12) . ? O27 C43 1.293(11) . ? O28 C43 1.235(10) . ? C1 C2 1.482(12) . ? C2 C7 1.349(12) . ? C2 C3 1.430(11) . ? C3 C4 1.353(13) . ? C4 C5 1.402(13) . ? C5 C6 1.410(13) . ? C6 C7 1.394(13) . ? C9 C10 1.394(12) . ? C9 C13 1.397(13) . ? C10 C11 1.382(13) . ? C11 C15 1.392(13) . ? C12 C15 1.387(12) . ? C12 C13 1.399(13) . ? C14 C15 1.496(13) 2_665 ? C15 C14 1.496(13) 2_665 ? C16 C28 1.499(13) . ? C17 C18 1.506(13) . ? C18 C19 1.397(11) . ? C18 C23 1.398(13) . ? C19 C20 1.379(12) . ? C20 C21 1.373(14) . ? C21 C22 1.394(11) . ? C22 C23 1.377(12) . ? C25 C26 1.364(13) . ? C25 C30 1.393(12) . ? C26 C27 1.372(14) . ? C27 C28 1.393(11) . ? C28 C29 1.419(12) . ? C29 C30 1.358(12) . ? C31 C32 1.542(14) . ? C32 C37 1.363(12) . ? C32 C33 1.395(12) . ? C33 C34 1.408(14) . ? C34 C35 1.396(12) . ? C35 C36 1.388(12) . ? C36 C37 1.369(14) . ? C38 C42 1.358(13) . ? C38 C39 1.422(13) . ? C39 C74 1.406(15) . ? C40 C74 1.376(13) . ? C40 C41 1.394(12) . ? C41 C42 1.406(12) . ? C41 C43 1.478(13) 2_656 ? C43 C41 1.478(13) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Dy1 O4 78.0(2) 1_665 . ? O3 Dy1 O7 94.6(2) 1_665 . ? O4 Dy1 O7 77.1(2) . . ? O3 Dy1 O5 152.2(2) 1_665 . ? O4 Dy1 O5 77.5(2) . . ? O7 Dy1 O5 92.5(2) . . ? O3 Dy1 O2 83.5(2) 1_665 . ? O4 Dy1 O2 75.1(2) . . ? O7 Dy1 O2 151.9(2) . . ? O5 Dy1 O2 77.7(2) . . ? O3 Dy1 O28 135.6(2) 1_665 . ? O4 Dy1 O28 140.5(3) . . ? O7 Dy1 O28 79.5(2) . . ? O5 Dy1 O28 72.2(2) . . ? O2 Dy1 O28 120.9(2) . . ? O3 Dy1 O1 78.6(2) 1_665 . ? O4 Dy1 O1 141.4(2) . . ? O7 Dy1 O1 135.2(2) . . ? O5 Dy1 O1 114.0(2) . . ? O2 Dy1 O1 72.1(2) . . ? O28 Dy1 O1 75.7(2) . . ? O3 Dy1 O8 71.2(3) 1_665 . ? O4 Dy1 O8 130.5(2) . . ? O7 Dy1 O8 68.1(2) . . ? O5 Dy1 O8 135.9(3) . . ? O2 Dy1 O8 135.7(3) . . ? O28 Dy1 O8 65.7(3) . . ? O1 Dy1 O8 67.8(3) . . ? O17 Dy2 O27 99.9(2) . . ? O17 Dy2 O9 170.6(2) . 1_455 ? O27 Dy2 O9 87.5(2) . 1_455 ? O17 Dy2 O11 87.2(2) . 1_455 ? O27 Dy2 O11 146.2(2) . 1_455 ? O9 Dy2 O11 83.4(2) 1_455 1_455 ? O17 Dy2 O10 79.6(2) . 1_565 ? O27 Dy2 O10 73.6(2) . 1_565 ? O9 Dy2 O10 97.0(2) 1_455 1_565 ? O11 Dy2 O10 75.4(2) 1_455 1_565 ? O17 Dy2 O18 114.4(2) . . ? O27 Dy2 O18 76.3(2) . . ? O9 Dy2 O18 72.9(2) 1_455 . ? O11 Dy2 O18 130.6(2) 1_455 . ? O10 Dy2 O18 148.6(2) 1_565 . ? O17 Dy2 O12 83.8(3) . . ? O27 Dy2 O12 144.2(2) . . ? O9 Dy2 O12 93.7(3) 1_455 . ? O11 Dy2 O12 69.1(2) 1_455 . ? O10 Dy2 O12 141.3(3) 1_565 . ? O18 Dy2 O12 70.0(3) . . ? O17 Dy2 O5 67.5(2) . . ? O27 Dy2 O5 74.9(2) . . ? O9 Dy2 O5 120.6(2) 1_455 . ? O11 Dy2 O5 136.9(2) 1_455 . ? O10 Dy2 O5 129.0(2) 1_565 . ? O18 Dy2 O5 48.0(2) . . ? O12 Dy2 O5 73.8(2) . . ? O21 S1 O22 118.8(5) . . ? O21 S1 O20 108.9(4) . . ? O22 S1 O20 108.8(4) . . ? O21 S1 C25 111.2(5) . . ? O22 S1 C25 110.6(5) . . ? O20 S1 C25 96.2(4) . . ? O24 S2 O23 119.8(4) . . ? O24 S2 O25 108.6(4) . . ? O23 S2 O25 107.0(4) . . ? O24 S2 C35 111.7(5) . . ? O23 S2 C35 109.0(4) . . ? O25 S2 C35 98.5(5) . . ? O16 S3 O15 119.2(5) . . ? O16 S3 O14 108.1(4) . . ? O15 S3 O14 108.5(4) . . ? O16 S3 C9 110.0(4) . . ? O15 S3 C9 110.6(5) . . ? O14 S3 C9 98.4(4) . . ? C14 O2 Dy1 134.3(7) . . ? C16 O3 Dy1 148.7(6) . 1_445 ? C1 O4 Dy1 148.2(6) . . ? C17 O5 Dy1 136.1(7) . . ? C17 O5 Dy2 83.3(6) . . ? Dy1 O5 Dy2 115.7(2) . . ? C31 O7 Dy1 143.7(7) . . ? C31 O9 Dy2 155.0(7) . 1_655 ? C16 O10 Dy2 127.6(6) . 1_545 ? C1 O11 Dy2 140.8(6) . 1_655 ? C5 O13 C8 116.2(8) . . ? C6 O14 S3 118.6(6) . . ? C14 O17 Dy2 154.8(6) . . ? C17 O18 Dy2 105.8(7) . . ? C21 O19 C24 118.3(8) . . ? C22 O20 S1 116.1(6) . . ? C38 O25 S2 120.9(6) . . ? C39 O26 C44 117.2(10) . . ? C43 O27 Dy2 133.1(6) . . ? C43 O28 Dy1 138.2(6) . . ? O4 C1 O11 122.9(9) . . ? O4 C1 C2 120.3(8) . . ? O11 C1 C2 116.8(8) . . ? C7 C2 C3 119.5(9) . . ? C7 C2 C1 121.7(9) . . ? C3 C2 C1 118.8(8) . . ? C4 C3 C2 120.3(9) . . ? C3 C4 C5 120.6(9) . . ? O13 C5 C4 126.7(9) . . ? O13 C5 C6 114.3(9) . . ? C4 C5 C6 118.9(9) . . ? O14 C6 C7 121.2(9) . . ? O14 C6 C5 119.2(9) . . ? C7 C6 C5 119.6(9) . . ? C2 C7 C6 121.1(9) . . ? C10 C9 C13 119.7(10) . . ? C10 C9 S3 120.0(8) . . ? C13 C9 S3 120.3(8) . . ? C11 C10 C9 119.2(9) . . ? C10 C11 C15 121.7(10) . . ? C15 C12 C13 119.7(9) . . ? C9 C13 C12 120.4(9) . . ? O2 C14 O17 124.6(10) . . ? O2 C14 C15 118.1(8) . 2_665 ? O17 C14 C15 117.3(8) . 2_665 ? C12 C15 C11 119.2(10) . . ? C12 C15 C14 119.9(9) . 2_665 ? C11 C15 C14 120.9(9) . 2_665 ? O3 C16 O10 125.1(9) . . ? O3 C16 C28 116.9(8) . . ? O10 C16 C28 118.1(8) . . ? O5 C17 O18 121.9(9) . . ? O5 C17 C18 121.3(9) . . ? O18 C17 C18 116.7(10) . . ? C19 C18 C23 120.7(9) . . ? C19 C18 C17 120.7(9) . . ? C23 C18 C17 118.6(8) . . ? C20 C19 C18 117.6(9) . . ? C21 C20 C19 123.2(9) . . ? C20 C21 O19 126.8(8) . . ? C20 C21 C22 118.1(9) . . ? O19 C21 C22 115.0(9) . . ? C23 C22 O20 119.4(8) . . ? C23 C22 C21 121.0(9) . . ? O20 C22 C21 119.6(8) . . ? C22 C23 C18 119.3(8) . . ? C26 C25 C30 121.7(10) . . ? C26 C25 S1 119.6(8) . . ? C30 C25 S1 118.7(7) . . ? C25 C26 C27 118.7(9) . . ? C26 C27 C28 121.6(9) . . ? C27 C28 C29 118.2(9) . . ? C27 C28 C16 120.9(8) . . ? C29 C28 C16 120.9(8) . . ? C30 C29 C28 119.9(8) . . ? C29 C30 C25 119.8(8) . . ? O7 C31 O9 126.9(10) . . ? O7 C31 C32 116.0(9) . . ? O9 C31 C32 117.0(8) . . ? C37 C32 C33 120.9(11) . . ? C37 C32 C31 118.1(9) . . ? C33 C32 C31 120.8(9) . . ? C32 C33 C34 120.6(10) . . ? C35 C34 C33 116.7(9) . . ? C36 C35 C34 121.6(10) . . ? C36 C35 S2 121.0(7) . . ? C34 C35 S2 117.4(7) . . ? C37 C36 C35 120.4(9) . . ? C32 C37 C36 119.8(9) . . ? C42 C38 O25 120.4(8) . . ? C42 C38 C39 121.3(9) . . ? O25 C38 C39 117.8(10) . . ? O26 C39 C74 126.2(9) . . ? O26 C39 C38 116.2(10) . . ? C74 C39 C38 117.5(10) . . ? C74 C40 C41 120.8(9) . . ? C40 C41 C42 118.9(9) . . ? C40 C41 C43 122.5(9) . 2_656 ? C42 C41 C43 118.5(8) . 2_656 ? C38 C42 C41 120.5(9) . . ? O28 C43 O27 124.0(9) . . ? O28 C43 C41 118.0(9) . 2_656 ? O27 C43 C41 118.0(8) . 2_656 ? C40 C74 C39 120.9(9) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 0.000 0.000 501 149 ' ' 2 0.000 0.500 0.500 14 9 ' ' 3 0.282 0.678 0.440 30 13 ' ' 4 0.717 0.321 0.560 30 12 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.002 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.206 #===end data_6 _database_code_depnum_ccdc_archive 'CCDC 905412' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H38 Ho2 O27.50 S3' _chemical_formula_weight 1444.79 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1671(18) _cell_length_b 15.520(3) _cell_length_c 22.199(4) _cell_angle_alpha 102.89(3) _cell_angle_beta 101.79(3) _cell_angle_gamma 104.14(3) _cell_volume 2871.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6312 _cell_measurement_theta_min 2.3774 _cell_measurement_theta_max 29.0054 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 2.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5921 _exptl_absorpt_correction_T_max 0.5921 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2116 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17925 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10086 _reflns_number_gt 7740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10086 _refine_ls_number_parameters 706 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.2018 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.98324(6) 0.63831(3) 0.69647(2) 0.01646(18) Uani 1 1 d . . . Ho2 Ho 0.47007(6) 0.58854(3) 0.64393(2) 0.01740(18) Uani 1 1 d . . . C1 C 0.7964(12) 0.7703(8) 0.7094(5) 0.017(2) Uani 1 1 d . . . C2 C 0.7450(12) 0.8544(8) 0.7265(5) 0.015(2) Uani 1 1 d . . . C3 C 0.6251(12) 0.8564(8) 0.7576(5) 0.019(2) Uani 1 1 d . . . H3 H 0.5732 0.8036 0.7668 0.023 Uiso 1 1 calc R . . C4 C 0.5851(14) 0.9375(8) 0.7742(6) 0.026(3) Uani 1 1 d . . . H4 H 0.5051 0.9377 0.7940 0.031 Uiso 1 1 calc R . . C5 C 0.6602(14) 1.0174(8) 0.7623(5) 0.025(3) Uani 1 1 d . . . C6 C 0.7829(13) 1.0154(8) 0.7332(5) 0.024(3) Uani 1 1 d . . . C7 C 0.8247(13) 0.9352(9) 0.7150(5) 0.024(3) Uani 1 1 d . . . H7 H 0.9050 0.9354 0.6952 0.028 Uiso 1 1 calc R . . C8 C 0.5103(17) 1.1056(11) 0.8065(7) 0.046(4) Uani 1 1 d . . . H8A H 0.4104 1.0650 0.7794 0.069 Uiso 1 1 calc R . . H8B H 0.5065 1.1683 0.8169 0.069 Uiso 1 1 calc R . . H8C H 0.5351 1.0881 0.8453 0.069 Uiso 1 1 calc R . . C9 C 1.0516(14) 1.2481(8) 0.7353(5) 0.025(3) Uani 1 1 d . . . C10 C 0.9468(18) 1.2992(9) 0.7349(7) 0.040(4) Uani 1 1 d . . . H10 H 0.8653 1.2872 0.7539 0.048 Uiso 1 1 calc R . . C11 C 0.9696(15) 1.3696(10) 0.7046(6) 0.033(3) Uani 1 1 d . . . H11 H 0.9034 1.4065 0.7043 0.040 Uiso 1 1 calc R . . C14 C 1.1738(13) 1.2657(8) 0.7086(5) 0.021(2) Uani 1 1 d . . . H14 H 1.2429 1.2307 0.7101 0.025 Uiso 1 1 calc R . . C16 C 0.3291(12) 0.6243(8) 0.7753(5) 0.015(2) Uani 1 1 d U . . C17 C 0.4094(13) 0.6245(8) 0.8404(5) 0.018(2) Uani 1 1 d . . . C18 C 0.5734(12) 0.6486(8) 0.8618(5) 0.021(2) Uani 1 1 d . . . H18 H 0.6326 0.6650 0.8344 0.025 Uiso 1 1 calc R . . C19 C 0.6481(14) 0.6487(10) 0.9221(6) 0.033(3) Uani 1 1 d . . . H19 H 0.7568 0.6658 0.9350 0.040 Uiso 1 1 calc R . . C20 C 0.5632(14) 0.6236(8) 0.9642(5) 0.024(3) Uani 1 1 d . . . C21 C 0.4048(16) 0.6009(9) 0.9442(5) 0.034(3) Uani 1 1 d . . . C22 C 0.3232(13) 0.5990(9) 0.8818(5) 0.027(3) Uani 1 1 d . . . H22 H 0.2145 0.5810 0.8690 0.032 Uiso 1 1 calc R . . C23 C 0.7914(17) 0.6495(12) 1.0478(6) 0.049(4) Uani 1 1 d . . . H23A H 0.8213 0.6495 1.0918 0.073 Uiso 1 1 calc R . . H23B H 0.8317 0.7111 1.0448 0.073 Uiso 1 1 calc R . . H23C H 0.8332 0.6082 1.0224 0.073 Uiso 1 1 calc R . . C24 C 0.2813(14) 0.6028(8) 1.0989(4) 0.021(3) Uani 1 1 d . . . C25 C 0.4241(14) 0.6164(9) 1.1379(5) 0.026(3) Uani 1 1 d . . . H25 H 0.5141 0.6496 1.1302 0.031 Uiso 1 1 calc R . . C26 C 0.4337(15) 0.5791(8) 1.1905(5) 0.029(3) Uani 1 1 d . . . H26 H 0.5311 0.5849 1.2165 0.035 Uiso 1 1 calc R . . C27 C 0.3016(13) 0.5349(7) 1.2033(5) 0.016(2) Uani 1 1 d U . . C28 C 0.1552(13) 0.5232(9) 1.1627(5) 0.024(3) Uani 1 1 d . . . H28 H 0.0641 0.4925 1.1710 0.029 Uiso 1 1 calc R . . C29 C 0.1473(14) 0.5580(10) 1.1097(6) 0.030(3) Uani 1 1 d . . . H29 H 0.0509 0.5505 1.0821 0.036 Uiso 1 1 calc R . . C30 C 0.3086(13) 0.4942(7) 1.2600(5) 0.017(2) Uani 1 1 d . . . C31 C 0.7433(14) 0.6533(8) 0.5686(5) 0.021(3) Uani 1 1 d . . . C32 C 0.8029(12) 0.7144(8) 0.5316(5) 0.020(2) Uani 1 1 d . . . C33 C 0.9432(13) 0.7232(9) 0.5166(5) 0.023(3) Uani 1 1 d U . . H33 H 1.0032 0.6863 0.5286 0.027 Uiso 1 1 calc R . . C34 C 0.9976(13) 0.7848(10) 0.4842(6) 0.031(3) Uani 1 1 d . . . H34 H 1.0925 0.7888 0.4745 0.038 Uiso 1 1 calc R . . C35 C 0.9083(14) 0.8421(10) 0.4659(5) 0.030(3) Uani 1 1 d . . . C36 C 0.7623(14) 0.8293(8) 0.4804(5) 0.023(3) Uani 1 1 d . . . C37 C 0.7117(14) 0.7680(8) 0.5118(5) 0.022(3) Uani 1 1 d . . . H37 H 0.6150 0.7616 0.5204 0.027 Uiso 1 1 calc R . . C38 C 1.0973(17) 0.9220(13) 0.4229(7) 0.062(5) Uani 1 1 d . . . H38A H 1.0891 0.9346 0.3821 0.093 Uiso 1 1 calc R . . H38B H 1.1333 0.8688 0.4222 0.093 Uiso 1 1 calc R . . H38C H 1.1701 0.9748 0.4561 0.093 Uiso 1 1 calc R . . C39 C 0.6021(15) 0.9783(9) 0.3870(6) 0.029(3) Uani 1 1 d . . . C40 C 0.7229(17) 1.0053(10) 0.3606(6) 0.035(3) Uani 1 1 d . . . H40 H 0.7790 0.9651 0.3485 0.043 Uiso 1 1 calc R . . C41 C 0.7602(14) 1.0934(10) 0.3522(6) 0.034(3) Uani 1 1 d . . . H41 H 0.8420 1.1112 0.3344 0.041 Uiso 1 1 calc R . . C42 C 0.6823(14) 1.1539(9) 0.3690(5) 0.025(3) Uani 1 1 d . . . C43 C 0.5606(14) 1.1253(9) 0.3968(5) 0.023(3) Uani 1 1 d . . . H43 H 0.5038 1.1657 0.4077 0.028 Uiso 1 1 calc R . . C44 C 0.5221(14) 1.0414(9) 0.4084(5) 0.025(3) Uani 1 1 d . . . H44 H 0.4463 1.0261 0.4297 0.030 Uiso 1 1 calc R . . C15 C 1.1083(12) 1.4610(7) 0.6445(5) 0.014(2) Uani 1 1 d U . . C13 C 1.1942(13) 1.3370(7) 0.6788(5) 0.019(2) Uani 1 1 d . . . H13 H 1.2787 1.3513 0.6618 0.022 Uiso 1 1 calc R . . C45 C 0.7130(13) 1.2462(9) 0.3558(5) 0.020(3) Uani 1 1 d . . . C12 C 1.0876(13) 1.3852(7) 0.6754(5) 0.018(2) Uani 1 1 d U . . O1 O 0.9265(9) 0.7804(5) 0.6993(4) 0.0232(18) Uani 1 1 d . . . O2 O 0.7100(8) 0.6939(5) 0.7095(3) 0.0194(17) Uani 1 1 d . . . O3 O 1.0470(11) 0.7306(6) 0.8058(4) 0.037(2) Uani 1 1 d . . . H3A H 1.1159 0.7904 0.8141 0.056 Uiso 1 1 d R . . H3B H 0.9598 0.7406 0.8193 0.056 Uiso 1 1 d R . . O4 O 0.6272(10) 1.0988(6) 0.7736(4) 0.035(2) Uani 1 1 d . . . O5 O 0.8586(9) 1.0949(5) 0.7185(3) 0.0220(18) Uani 1 1 d . . . O6 O 1.1351(10) 1.1105(7) 0.7631(5) 0.042(2) Uani 1 1 d . . . O7 O 0.9953(13) 1.1834(6) 0.8304(4) 0.046(3) Uani 1 1 d . . . O8 O 1.2305(9) 1.4839(5) 0.6271(3) 0.0234(18) Uani 1 1 d . . . O9 O 1.0014(9) 1.4993(5) 0.6355(4) 0.0234(18) Uani 1 1 d . . . O10 O 0.8327(10) 0.6119(6) 0.5940(4) 0.029(2) Uani 1 1 d . . . O11 O 0.6079(9) 0.6424(6) 0.5758(4) 0.029(2) Uani 1 1 d . . . O12 O 0.4893(10) 0.4549(6) 0.5745(4) 0.032(2) Uani 1 1 d . . . H12A H 0.5602 0.4338 0.5946 0.049 Uiso 1 1 d R . . H12B H 0.3993 0.4100 0.5607 0.049 Uiso 1 1 d R . . O13 O 0.3025(16) 0.5485(10) 0.5278(5) 0.074(4) Uani 1 1 d . . . H13A H 0.3518 0.5831 0.5040 0.112 Uiso 1 1 d R . . H13B H 0.2791 0.4860 0.5042 0.112 Uiso 1 1 d R . . O14 O 0.4108(9) 0.6426(6) 0.7376(3) 0.0211(17) Uani 1 1 d . . . O15 O 0.9486(11) 0.9043(7) 0.4351(4) 0.044(3) Uani 1 1 d . . . O16 O 0.6823(11) 0.8934(7) 0.4686(4) 0.038(2) Uani 1 1 d . . . O17 O 0.4028(11) 0.8486(7) 0.4130(5) 0.042(2) Uani 1 1 d . . . O18 O 0.5804(10) 0.8021(6) 0.3539(4) 0.034(2) Uani 1 1 d . . . O19 O 0.8151(9) 1.2656(6) 0.3271(4) 0.0274(19) Uani 1 1 d . . . O20 O 0.6385(10) 1.2997(6) 0.3769(4) 0.031(2) Uani 1 1 d . . . O21 O 0.1843(9) 0.6080(5) 0.7624(3) 0.0204(17) Uani 1 1 d . . . O22 O 0.6232(10) 0.6190(7) 1.0243(4) 0.035(2) Uani 1 1 d . . . O23 O 0.3125(10) 0.5709(6) 0.9838(4) 0.032(2) Uani 1 1 d . . . O24 O 0.3925(11) 0.7339(7) 1.0477(4) 0.040(2) Uani 1 1 d . . . O25 O 0.1132(11) 0.6447(7) 1.0056(4) 0.038(2) Uani 1 1 d . . . O26 O 0.4407(8) 0.4961(5) 1.2898(3) 0.0206(17) Uani 1 1 d . . . O27 O 0.1839(9) 0.4638(6) 1.2728(4) 0.0239(18) Uani 1 1 d . . . S1 S 1.0217(4) 1.1565(2) 0.76981(14) 0.0270(7) Uani 1 1 d . . . S2 S 0.2708(4) 0.6494(3) 1.03226(14) 0.0324(8) Uani 1 1 d . . . S3 S 0.5527(4) 0.8692(2) 0.40068(15) 0.0298(7) Uani 1 1 d . . . O28 O 0.0000 0.5000 0.5000 0.069(5) Uani 1 2 d S . . H28A H 0.0301 0.4541 0.4851 0.104 Uiso 1 1 d R . . H28B H -0.0219 0.4945 0.5346 0.104 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.0190(3) 0.0140(3) 0.0147(3) 0.0032(2) 0.0027(2) 0.0045(2) Ho2 0.0181(3) 0.0136(3) 0.0218(3) 0.0066(2) 0.0078(2) 0.0038(2) C1 0.009(6) 0.018(6) 0.018(5) 0.003(5) 0.001(4) -0.001(5) C2 0.019(6) 0.016(6) 0.008(5) 0.005(4) -0.005(4) 0.006(5) C3 0.017(6) 0.018(6) 0.018(5) 0.003(5) 0.005(4) -0.001(5) C4 0.028(7) 0.023(7) 0.033(6) 0.005(5) 0.022(6) 0.009(6) C5 0.026(7) 0.013(6) 0.025(6) -0.005(5) 0.002(5) -0.002(5) C6 0.020(6) 0.023(7) 0.025(6) 0.011(5) 0.001(5) 0.002(5) C7 0.013(6) 0.030(7) 0.020(6) 0.005(5) -0.001(5) 0.000(5) C8 0.040(9) 0.041(9) 0.050(9) 0.000(7) 0.005(7) 0.020(8) C9 0.038(7) 0.008(6) 0.020(6) 0.006(5) -0.002(5) -0.004(5) C10 0.062(10) 0.021(7) 0.061(9) 0.028(7) 0.039(8) 0.020(7) C11 0.033(8) 0.038(8) 0.047(8) 0.029(7) 0.022(6) 0.018(7) C14 0.014(6) 0.013(6) 0.021(5) -0.005(5) -0.003(5) -0.007(5) C16 0.008(5) 0.017(5) 0.013(4) -0.005(4) -0.003(4) 0.004(4) C17 0.025(6) 0.016(6) 0.011(5) -0.002(4) 0.008(4) 0.004(5) C18 0.010(6) 0.017(6) 0.028(6) -0.001(5) 0.006(5) -0.002(5) C19 0.018(7) 0.035(8) 0.031(7) -0.007(6) -0.007(5) 0.005(6) C20 0.026(7) 0.017(6) 0.017(6) -0.003(5) -0.008(5) 0.002(5) C21 0.042(8) 0.030(7) 0.019(6) -0.007(5) 0.011(6) 0.001(6) C22 0.015(6) 0.035(7) 0.021(6) 0.010(6) -0.005(5) -0.002(5) C23 0.048(10) 0.064(11) 0.031(7) 0.015(8) -0.007(7) 0.025(9) C24 0.035(7) 0.021(6) 0.002(5) 0.002(4) 0.002(5) 0.006(5) C25 0.031(7) 0.026(7) 0.023(6) 0.014(5) 0.011(5) 0.002(6) C26 0.037(8) 0.014(6) 0.024(6) -0.002(5) 0.005(5) -0.005(6) C27 0.031(6) 0.014(5) 0.006(4) 0.003(4) 0.007(4) 0.007(4) C28 0.019(6) 0.032(7) 0.027(6) 0.015(6) 0.007(5) 0.010(6) C29 0.024(7) 0.042(8) 0.022(6) 0.009(6) 0.003(5) 0.007(6) C30 0.024(7) 0.008(5) 0.020(5) -0.001(4) 0.008(5) 0.008(5) C31 0.034(7) 0.011(6) 0.008(5) -0.003(4) -0.008(5) 0.003(5) C32 0.013(6) 0.023(6) 0.014(5) -0.003(5) 0.002(4) -0.004(5) C33 0.016(5) 0.033(6) 0.011(5) -0.001(4) -0.007(4) 0.007(5) C34 0.008(6) 0.057(9) 0.026(6) 0.011(6) 0.006(5) 0.003(6) C35 0.025(7) 0.038(8) 0.014(5) 0.004(5) -0.002(5) -0.005(6) C36 0.034(7) 0.022(6) 0.012(5) 0.010(5) 0.002(5) 0.003(5) C37 0.031(7) 0.032(7) 0.006(5) 0.001(5) 0.008(5) 0.014(6) C38 0.045(10) 0.072(13) 0.034(8) 0.010(8) 0.002(7) -0.033(9) C39 0.039(8) 0.033(8) 0.024(6) 0.020(6) 0.007(6) 0.017(6) C40 0.055(9) 0.040(8) 0.032(7) 0.025(7) 0.021(7) 0.032(8) C41 0.019(7) 0.043(9) 0.049(8) 0.020(7) 0.016(6) 0.012(6) C42 0.022(7) 0.033(7) 0.022(6) 0.012(6) 0.000(5) 0.014(6) C43 0.028(7) 0.034(7) 0.019(6) 0.008(5) 0.011(5) 0.025(6) C44 0.024(7) 0.031(7) 0.019(6) 0.006(5) 0.006(5) 0.008(6) C15 0.013(4) 0.010(4) 0.013(4) -0.006(3) 0.004(3) 0.004(3) C13 0.016(6) 0.011(5) 0.020(5) 0.002(5) 0.000(4) -0.005(5) C45 0.014(6) 0.034(7) 0.008(5) 0.002(5) -0.004(4) 0.009(5) C12 0.022(5) 0.010(5) 0.010(4) -0.006(4) 0.000(4) -0.005(4) O1 0.016(4) 0.015(4) 0.041(5) 0.009(4) 0.010(4) 0.007(3) O2 0.017(4) 0.006(4) 0.024(4) -0.002(3) -0.003(3) -0.002(3) O3 0.035(5) 0.032(5) 0.028(4) -0.019(4) -0.002(4) 0.014(4) O4 0.036(5) 0.026(5) 0.048(5) 0.009(4) 0.018(4) 0.012(4) O5 0.020(4) 0.019(4) 0.022(4) 0.013(4) -0.002(3) -0.004(3) O6 0.021(5) 0.028(5) 0.069(7) 0.023(5) -0.004(4) 0.002(4) O7 0.089(8) 0.018(5) 0.009(4) -0.002(4) 0.008(4) -0.012(5) O8 0.015(4) 0.017(4) 0.024(4) -0.004(3) 0.003(3) -0.009(3) O9 0.028(5) 0.012(4) 0.024(4) 0.001(3) 0.002(3) 0.003(4) O10 0.040(5) 0.020(5) 0.023(4) 0.004(4) 0.003(4) 0.012(4) O11 0.013(4) 0.042(6) 0.032(5) 0.023(4) 0.000(3) 0.004(4) O12 0.034(5) 0.023(5) 0.026(4) -0.006(4) 0.004(4) -0.001(4) O13 0.088(10) 0.057(8) 0.058(7) -0.006(6) 0.001(7) 0.024(8) O14 0.021(4) 0.031(5) 0.007(3) 0.000(3) -0.002(3) 0.008(4) O15 0.048(6) 0.041(6) 0.031(5) 0.015(5) 0.020(4) -0.017(5) O16 0.060(6) 0.039(6) 0.024(4) 0.012(4) 0.015(4) 0.027(5) O17 0.037(6) 0.029(5) 0.067(7) 0.023(5) 0.025(5) 0.007(5) O18 0.044(6) 0.027(5) 0.021(4) -0.001(4) 0.001(4) 0.009(4) O19 0.024(5) 0.039(5) 0.024(4) 0.019(4) 0.004(4) 0.010(4) O20 0.039(5) 0.044(6) 0.036(5) 0.033(5) 0.020(4) 0.031(5) O21 0.020(4) 0.016(4) 0.021(4) 0.006(3) -0.002(3) 0.003(3) O22 0.038(5) 0.044(6) 0.012(4) -0.001(4) -0.008(4) 0.013(5) O23 0.041(5) 0.036(5) 0.019(4) 0.004(4) 0.016(4) 0.009(4) O24 0.054(6) 0.035(6) 0.040(5) 0.016(5) 0.021(5) 0.020(5) O25 0.049(6) 0.055(7) 0.023(4) 0.019(5) 0.007(4) 0.031(5) O26 0.015(4) 0.015(4) 0.027(4) 0.007(3) -0.002(3) 0.002(3) O27 0.027(5) 0.022(5) 0.031(4) 0.017(4) 0.013(4) 0.011(4) S1 0.0277(17) 0.0159(15) 0.0299(16) 0.0085(13) 0.0014(13) -0.0029(13) S2 0.043(2) 0.042(2) 0.0194(15) 0.0149(15) 0.0106(14) 0.0171(17) S3 0.0393(19) 0.0273(17) 0.0270(16) 0.0120(14) 0.0110(14) 0.0123(15) O28 0.112(15) 0.079(13) 0.034(8) 0.029(9) 0.023(9) 0.047(12) _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 Ho1 O27 2.247(8) 2_667 ? Ho1 O10 2.296(8) . ? Ho1 O19 2.305(8) 2_776 ? Ho1 O21 2.321(7) 1_655 ? Ho1 O9 2.341(8) 1_545 ? Ho1 O1 2.377(7) . ? Ho1 O3 2.397(8) . ? Ho2 O20 2.286(8) 2_676 ? Ho2 O14 2.287(7) . ? Ho2 O8 2.291(7) 1_445 ? Ho2 O11 2.326(8) . ? Ho2 O26 2.335(7) 2_667 ? Ho2 O2 2.345(7) . ? Ho2 O12 2.360(8) . ? Ho2 O13 2.567(11) . ? C1 O1 1.238(12) . ? C1 O2 1.256(13) . ? C1 C2 1.490(15) . ? C2 C7 1.395(16) . ? C2 C3 1.416(15) . ? C3 C4 1.388(16) . ? C4 C5 1.374(16) . ? C5 O4 1.350(14) . ? C5 C6 1.410(16) . ? C6 C7 1.390(17) . ? C6 O5 1.402(13) . ? C8 O4 1.427(16) . ? C9 C14 1.370(16) . ? C9 C10 1.387(18) . ? C9 S1 1.751(11) . ? C10 C11 1.403(16) . ? C11 C12 1.371(16) . ? C14 C13 1.403(15) . ? C16 O21 1.248(12) . ? C16 O14 1.265(12) . ? C16 C17 1.482(14) . ? C17 C22 1.389(15) . ? C17 C18 1.407(15) . ? C18 C19 1.373(16) . ? C19 C20 1.395(17) . ? C20 O22 1.359(13) . ? C20 C21 1.359(17) . ? C21 O23 1.413(14) . ? C21 C22 1.423(16) . ? C23 O22 1.442(16) . ? C24 C29 1.352(16) . ? C24 C25 1.352(16) . ? C24 S2 1.781(10) . ? C25 C26 1.411(16) . ? C26 C27 1.357(16) . ? C27 C28 1.400(15) . ? C27 C30 1.525(14) . ? C28 C29 1.398(16) . ? C30 O27 1.241(13) . ? C30 O26 1.245(13) . ? C31 O11 1.259(14) . ? C31 O10 1.277(13) . ? C31 C32 1.468(15) . ? C32 C33 1.376(15) . ? C32 C37 1.392(16) . ? C33 C34 1.377(17) . ? C34 C35 1.417(18) . ? C35 O15 1.325(15) . ? C35 C36 1.417(17) . ? C36 C37 1.347(15) . ? C36 O16 1.411(14) . ? C38 O15 1.417(17) . ? C39 C40 1.377(17) . ? C39 C44 1.418(17) . ? C39 S3 1.754(12) . ? C40 C41 1.389(19) . ? C41 C42 1.345(18) . ? C42 C43 1.409(16) . ? C42 C45 1.497(17) . ? C43 C44 1.360(17) . ? C15 O8 1.255(12) . ? C15 O9 1.269(12) . ? C15 C12 1.481(15) . ? C13 C12 1.369(16) . ? C45 O19 1.250(13) . ? C45 O20 1.269(14) . ? O5 S1 1.602(8) . ? O6 S1 1.412(10) . ? O7 S1 1.406(9) . ? O8 Ho2 2.291(7) 1_665 ? O9 Ho1 2.341(8) 1_565 ? O16 S3 1.620(9) . ? O17 S3 1.429(9) . ? O18 S3 1.408(9) . ? O19 Ho1 2.305(8) 2_776 ? O20 Ho2 2.286(8) 2_676 ? O21 Ho1 2.321(7) 1_455 ? O23 S2 1.613(9) . ? O24 S2 1.418(10) . ? O25 S2 1.422(9) . ? O26 Ho2 2.335(7) 2_667 ? O27 Ho1 2.247(7) 2_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O27 Ho1 O10 98.2(3) 2_667 . ? O27 Ho1 O19 170.8(3) 2_667 2_776 ? O10 Ho1 O19 88.5(3) . 2_776 ? O27 Ho1 O21 87.3(3) 2_667 1_655 ? O10 Ho1 O21 147.4(3) . 1_655 ? O19 Ho1 O21 83.7(3) 2_776 1_655 ? O27 Ho1 O9 80.1(3) 2_667 1_545 ? O10 Ho1 O9 73.8(3) . 1_545 ? O19 Ho1 O9 96.0(3) 2_776 1_545 ? O21 Ho1 O9 75.6(3) 1_655 1_545 ? O27 Ho1 O1 115.0(3) 2_667 . ? O10 Ho1 O1 76.6(3) . . ? O19 Ho1 O1 72.5(3) 2_776 . ? O21 Ho1 O1 129.9(3) 1_655 . ? O9 Ho1 O1 148.5(3) 1_545 . ? O27 Ho1 O3 83.9(3) 2_667 . ? O10 Ho1 O3 144.3(3) . . ? O19 Ho1 O3 94.2(3) 2_776 . ? O21 Ho1 O3 68.1(3) 1_655 . ? O9 Ho1 O3 140.8(3) 1_545 . ? O1 Ho1 O3 70.4(3) . . ? O20 Ho2 O14 77.6(3) 2_676 . ? O20 Ho2 O8 92.5(3) 2_676 1_445 ? O14 Ho2 O8 79.0(3) . 1_445 ? O20 Ho2 O11 78.7(3) 2_676 . ? O14 Ho2 O11 140.2(3) . . ? O8 Ho2 O11 133.6(3) 1_445 . ? O20 Ho2 O26 153.2(3) 2_676 2_667 ? O14 Ho2 O26 75.7(3) . 2_667 ? O8 Ho2 O26 84.1(3) 1_445 2_667 ? O11 Ho2 O26 122.2(3) . 2_667 ? O20 Ho2 O2 94.8(3) 2_676 . ? O14 Ho2 O2 77.4(3) . . ? O8 Ho2 O2 153.1(3) 1_445 . ? O11 Ho2 O2 73.2(3) . . ? O26 Ho2 O2 77.8(3) 2_667 . ? O20 Ho2 O12 131.2(3) 2_676 . ? O14 Ho2 O12 143.7(3) . . ? O8 Ho2 O12 78.2(3) 1_445 . ? O11 Ho2 O12 74.5(3) . . ? O26 Ho2 O12 74.1(3) 2_667 . ? O2 Ho2 O12 114.8(3) . . ? O20 Ho2 O13 65.8(4) 2_676 . ? O14 Ho2 O13 128.8(3) . . ? O8 Ho2 O13 68.6(4) 1_445 . ? O11 Ho2 O13 66.3(4) . . ? O26 Ho2 O13 135.3(4) 2_667 . ? O2 Ho2 O13 137.5(4) . . ? O12 Ho2 O13 66.2(4) . . ? O1 C1 O2 123.2(10) . . ? O1 C1 C2 118.0(10) . . ? O2 C1 C2 118.6(9) . . ? C7 C2 C3 119.1(10) . . ? C7 C2 C1 118.6(10) . . ? C3 C2 C1 122.2(10) . . ? C4 C3 C2 119.8(10) . . ? C5 C4 C3 122.0(11) . . ? O4 C5 C4 127.3(11) . . ? O4 C5 C6 115.0(10) . . ? C4 C5 C6 117.6(11) . . ? C7 C6 O5 118.8(10) . . ? C7 C6 C5 122.0(11) . . ? O5 C6 C5 119.1(10) . . ? C6 C7 C2 119.4(11) . . ? C14 C9 C10 122.4(10) . . ? C14 C9 S1 119.7(9) . . ? C10 C9 S1 117.9(9) . . ? C9 C10 C11 116.7(12) . . ? C12 C11 C10 121.3(12) . . ? C9 C14 C13 119.6(11) . . ? O21 C16 O14 124.8(9) . . ? O21 C16 C17 116.6(9) . . ? O14 C16 C17 118.5(9) . . ? C22 C17 C18 118.2(10) . . ? C22 C17 C16 120.4(10) . . ? C18 C17 C16 121.4(9) . . ? C19 C18 C17 121.5(11) . . ? C18 C19 C20 120.9(11) . . ? O22 C20 C21 115.7(11) . . ? O22 C20 C19 126.4(11) . . ? C21 C20 C19 117.9(10) . . ? C20 C21 O23 120.4(11) . . ? C20 C21 C22 122.8(11) . . ? O23 C21 C22 116.7(11) . . ? C17 C22 C21 118.6(11) . . ? C29 C24 C25 122.6(10) . . ? C29 C24 S2 119.1(9) . . ? C25 C24 S2 118.2(9) . . ? C24 C25 C26 118.7(11) . . ? C27 C26 C25 120.3(11) . . ? C26 C27 C28 119.8(10) . . ? C26 C27 C30 121.4(10) . . ? C28 C27 C30 118.8(10) . . ? C29 C28 C27 119.4(11) . . ? C24 C29 C28 119.2(11) . . ? O27 C30 O26 126.1(10) . . ? O27 C30 C27 117.5(9) . . ? O26 C30 C27 116.4(9) . . ? O11 C31 O10 120.6(10) . . ? O11 C31 C32 120.9(10) . . ? O10 C31 C32 118.4(11) . . ? C33 C32 C37 118.6(10) . . ? C33 C32 C31 124.3(11) . . ? C37 C32 C31 117.1(10) . . ? C32 C33 C34 122.2(11) . . ? C33 C34 C35 119.7(11) . . ? O15 C35 C34 125.3(12) . . ? O15 C35 C36 118.1(12) . . ? C34 C35 C36 116.5(11) . . ? C37 C36 O16 120.9(11) . . ? C37 C36 C35 122.4(11) . . ? O16 C36 C35 116.1(10) . . ? C36 C37 C32 120.5(11) . . ? C40 C39 C44 120.2(12) . . ? C40 C39 S3 121.4(10) . . ? C44 C39 S3 118.2(9) . . ? C39 C40 C41 119.3(12) . . ? C42 C41 C40 122.5(12) . . ? C41 C42 C43 117.3(12) . . ? C41 C42 C45 123.1(11) . . ? C43 C42 C45 119.5(10) . . ? C44 C43 C42 123.1(11) . . ? C43 C44 C39 117.4(11) . . ? O8 C15 O9 122.4(10) . . ? O8 C15 C12 118.5(9) . . ? O9 C15 C12 119.2(9) . . ? C12 C13 C14 118.8(10) . . ? O19 C45 O20 125.3(12) . . ? O19 C45 C42 117.0(10) . . ? O20 C45 C42 117.5(10) . . ? C13 C12 C11 121.0(10) . . ? C13 C12 C15 119.3(10) . . ? C11 C12 C15 119.4(10) . . ? C1 O1 Ho1 106.6(7) . . ? C1 O2 Ho2 135.6(6) . . ? C5 O4 C8 116.8(10) . . ? C6 O5 S1 114.4(6) . . ? C15 O8 Ho2 148.7(7) . 1_665 ? C15 O9 Ho1 129.7(7) . 1_565 ? C31 O10 Ho1 133.5(7) . . ? C31 O11 Ho2 137.4(6) . . ? C16 O14 Ho2 146.4(7) . . ? C35 O15 C38 119.4(12) . . ? C36 O16 S3 119.9(8) . . ? C45 O19 Ho1 155.6(8) . 2_776 ? C45 O20 Ho2 143.5(7) . 2_676 ? C16 O21 Ho1 140.3(7) . 1_455 ? C20 O22 C23 116.1(10) . . ? C21 O23 S2 117.1(8) . . ? C30 O26 Ho2 134.0(7) . 2_667 ? C30 O27 Ho1 153.5(7) . 2_667 ? O7 S1 O6 119.1(6) . . ? O7 S1 O5 108.8(5) . . ? O6 S1 O5 109.0(5) . . ? O7 S1 C9 111.9(6) . . ? O6 S1 C9 109.7(6) . . ? O5 S1 C9 95.8(5) . . ? O24 S2 O25 120.1(6) . . ? O24 S2 O23 107.9(5) . . ? O25 S2 O23 107.8(5) . . ? O24 S2 C24 110.6(6) . . ? O25 S2 C24 109.4(5) . . ? O23 S2 C24 98.9(5) . . ? O18 S3 O17 118.1(6) . . ? O18 S3 O16 109.6(5) . . ? O17 S3 O16 107.1(5) . . ? O18 S3 C39 111.1(6) . . ? O17 S3 C39 110.5(6) . . ? O16 S3 C39 98.6(6) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.016 0.000 0.000 464.1 -8.1 2 0.279 0.685 0.454 20.7 -2.3 3 0.721 0.315 0.546 20.7 -1.8 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.764 _refine_diff_density_min -2.195 _refine_diff_density_rms 0.292