# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xigeng Zhou' _publ_contact_author_email xgzhou@fudan.edu.cn loop_ _publ_author_name 'Xigeng Zhou' 'Ruiting Liu' 'Xiaoqing Li' 'Houcai Zhang' 'Linhong Weng' data_f81201c _database_code_depnum_ccdc_archive 'CCDC 762741' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H31 Er N2 O2 S' _chemical_formula_weight 590.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.636(4) _cell_length_b 22.035(8) _cell_length_c 10.014(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.064(5) _cell_angle_gamma 90.00 _cell_volume 2454.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 916 _cell_measurement_theta_min 2.602 _cell_measurement_theta_max 25.208 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 3.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4726 _exptl_absorpt_correction_T_max 0.6769 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10067 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4305 _reflns_number_gt 3356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU and ISOR were used to restrain some abnormal ADPs. ; _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^)+(0.0269P)^2^+0.4583P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4305 _refine_ls_number_parameters 329 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.801855(17) 0.060955(9) 0.14840(2) 0.03613(8) Uani 1 1 d . . . S1 S 0.57309(10) 0.11858(6) 0.06620(14) 0.0544(3) Uani 1 1 d . . . N1 N 0.7460(3) 0.12706(15) 0.3050(4) 0.0370(8) Uani 1 1 d . . . N2 N 0.5823(3) 0.17784(18) 0.3125(4) 0.0505(10) Uani 1 1 d D . . H2N H 0.515(2) 0.1947(19) 0.284(5) 0.061 Uiso 1 1 d D . . C1 C 0.7039(5) -0.0444(2) 0.1840(5) 0.0529(13) Uani 1 1 d . . . H1A H 0.6308 -0.0542 0.1195 0.064 Uiso 1 1 calc R . . C2 C 0.7189(5) -0.0134(2) 0.3066(5) 0.0558(13) Uani 1 1 d . . . H2A H 0.6576 0.0014 0.3398 0.067 Uiso 1 1 calc R . . C3 C 0.8414(5) -0.0078(2) 0.3728(5) 0.0618(15) Uani 1 1 d . . . H3A H 0.8767 0.0114 0.4577 0.074 Uiso 1 1 calc R . . C4 C 0.9016(4) -0.0361(2) 0.2889(6) 0.0565(13) Uani 1 1 d . . . H4A H 0.9845 -0.0393 0.3080 0.068 Uiso 1 1 calc R . . C5 C 0.8175(5) -0.0586(2) 0.1729(5) 0.0535(13) Uani 1 1 d . . . H5A H 0.8335 -0.0796 0.0999 0.064 Uiso 1 1 calc R . . C6 C 0.9549(4) 0.0998(2) 0.0156(6) 0.0551(13) Uani 1 1 d . . . H6A H 0.9380 0.0895 -0.0783 0.066 Uiso 1 1 calc R . . C7 C 0.9168(4) 0.1526(2) 0.0682(5) 0.0508(12) Uani 1 1 d . . . H7A H 0.8696 0.1833 0.0160 0.061 Uiso 1 1 calc R . . C8 C 0.9631(4) 0.1504(2) 0.2138(5) 0.0498(12) Uani 1 1 d . . . H8A H 0.9525 0.1799 0.2756 0.060 Uiso 1 1 calc R . . C9 C 1.0274(4) 0.0968(2) 0.2505(6) 0.0529(13) Uani 1 1 d . . . H9A H 1.0669 0.0840 0.3408 0.063 Uiso 1 1 calc R . . C10 C 1.0219(4) 0.0654(2) 0.1271(6) 0.0580(14) Uani 1 1 d . . . H10A H 1.0572 0.0280 0.1212 0.070 Uiso 1 1 calc R . . C11 C 0.6336(4) 0.14211(19) 0.2348(5) 0.0410(11) Uani 1 1 d . . . C12 C 0.6666(4) 0.1863(2) 0.4427(5) 0.0448(11) Uani 1 1 d . . . C13 C 0.6628(5) 0.2178(2) 0.5595(6) 0.0582(14) Uani 1 1 d . . . H13A H 0.5942 0.2388 0.5624 0.070 Uiso 1 1 calc R . . C14 C 0.7645(5) 0.2172(2) 0.6716(6) 0.0633(15) Uani 1 1 d . . . H14A H 0.7645 0.2378 0.7527 0.076 Uiso 1 1 calc R . . C15 C 0.8670(5) 0.1867(2) 0.6669(5) 0.0582(13) Uani 1 1 d . . . H15A H 0.9347 0.1876 0.7444 0.070 Uiso 1 1 calc R . . C16 C 0.8709(4) 0.15473(19) 0.5494(5) 0.0451(11) Uani 1 1 d . . . H16A H 0.9400 0.1341 0.5467 0.054 Uiso 1 1 calc R . . C17 C 0.7690(4) 0.15449(18) 0.4363(5) 0.0380(10) Uani 1 1 d . . . O1 O 0.7147(3) 0.03224(15) -0.0983(3) 0.0562(9) Uani 1 1 d . . . C18 C 0.6622(5) -0.0234(2) -0.1604(5) 0.0644(15) Uani 1 1 d . . . H18A H 0.5897 -0.0320 -0.1349 0.077 Uiso 1 1 calc R . . H18B H 0.7181 -0.0567 -0.1288 0.077 Uiso 1 1 calc R . . C19 C 0.6336(6) -0.0157(3) -0.3147(5) 0.0844(18) Uani 1 1 d U . . H19A H 0.6935 -0.0355 -0.3496 0.101 Uiso 1 1 calc R . . H19B H 0.5552 -0.0325 -0.3622 0.101 Uiso 1 1 calc R . . C20 C 0.6351(8) 0.0506(3) -0.3346(7) 0.122(3) Uani 1 1 d U . . H20A H 0.6864 0.0606 -0.3923 0.146 Uiso 1 1 calc R . . H20B H 0.5545 0.0649 -0.3814 0.146 Uiso 1 1 calc R . . C21 C 0.6778(7) 0.0780(3) -0.2061(6) 0.104(3) Uani 1 1 d . . . H21A H 0.6154 0.1032 -0.1885 0.124 Uiso 1 1 calc R . . H21B H 0.7456 0.1038 -0.2050 0.124 Uiso 1 1 calc R . . O2 O 0.3630(15) 0.2314(7) 0.2022(18) 0.088(6) Uani 0.562(17) 1 d PDU A 1 C22 C 0.3432(14) 0.2968(7) 0.2259(16) 0.090(6) Uani 0.562(17) 1 d PDU A 1 H22C H 0.4176 0.3196 0.2571 0.108 Uiso 0.562(17) 1 calc PR A 1 H22D H 0.2953 0.3030 0.2894 0.108 Uiso 0.562(17) 1 calc PR A 1 C23 C 0.2702(14) 0.3103(7) 0.0668(16) 0.124(7) Uani 0.562(17) 1 d PDU A 1 H23C H 0.2358 0.3507 0.0534 0.149 Uiso 0.562(17) 1 calc PR A 1 H23D H 0.3177 0.3033 0.0033 0.149 Uiso 0.562(17) 1 calc PR A 1 C24 C 0.1762(12) 0.2609(7) 0.058(2) 0.102(6) Uani 0.562(17) 1 d PDU A 1 H24C H 0.1221 0.2563 -0.0356 0.122 Uiso 0.562(17) 1 calc PR A 1 H24D H 0.1304 0.2675 0.1237 0.122 Uiso 0.562(17) 1 calc PR A 1 C25 C 0.264(2) 0.2077(6) 0.101(3) 0.107(11) Uani 0.562(17) 1 d PD A 1 H25A H 0.2286 0.1746 0.1386 0.128 Uiso 0.562(17) 1 calc PR A 1 H25B H 0.2879 0.1929 0.0214 0.128 Uiso 0.562(17) 1 calc PR A 1 O2' O 0.3475(19) 0.2377(9) 0.2396(19) 0.071(5) Uani 0.438(17) 1 d PD A 2 C22' C 0.3637(14) 0.2979(9) 0.176(2) 0.091(8) Uani 0.438(17) 1 d PDU A 2 H22A H 0.4033 0.2943 0.1034 0.109 Uiso 0.438(17) 1 calc PR A 2 H22B H 0.4046 0.3277 0.2449 0.109 Uiso 0.438(17) 1 calc PR A 2 C23' C 0.2235(15) 0.3101(8) 0.116(2) 0.108(8) Uani 0.438(17) 1 d PDU A 2 H23A H 0.1814 0.3071 0.1859 0.129 Uiso 0.438(17) 1 calc PR A 2 H23B H 0.2047 0.3482 0.0654 0.129 Uiso 0.438(17) 1 calc PR A 2 C24' C 0.205(2) 0.2538(11) 0.018(2) 0.135(12) Uani 0.438(17) 1 d PDU A 2 H24A H 0.1211 0.2466 -0.0326 0.162 Uiso 0.438(17) 1 calc PR A 2 H24B H 0.2529 0.2553 -0.0467 0.162 Uiso 0.438(17) 1 calc PR A 2 C25' C 0.254(4) 0.2087(10) 0.139(4) 0.102(13) Uani 0.438(17) 1 d PDU A 2 H25C H 0.1912 0.1969 0.1791 0.122 Uiso 0.438(17) 1 calc PR A 2 H25D H 0.2842 0.1725 0.1053 0.122 Uiso 0.438(17) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03672(12) 0.03548(12) 0.03260(12) -0.00195(10) 0.00457(8) -0.00426(10) S1 0.0403(7) 0.0574(8) 0.0533(8) -0.0014(6) -0.0054(6) -0.0043(6) N1 0.030(2) 0.043(2) 0.036(2) -0.0007(17) 0.0066(16) 0.0000(16) N2 0.039(2) 0.049(2) 0.065(3) 0.005(2) 0.018(2) 0.009(2) C1 0.053(3) 0.049(3) 0.048(3) 0.008(2) 0.001(2) -0.017(2) C2 0.065(4) 0.051(3) 0.055(3) 0.008(3) 0.024(3) 0.000(3) C3 0.087(4) 0.049(3) 0.036(3) 0.010(2) -0.003(3) -0.005(3) C4 0.045(3) 0.053(3) 0.059(4) 0.019(3) -0.003(3) 0.007(2) C5 0.073(4) 0.037(3) 0.049(3) 0.000(2) 0.016(3) 0.002(3) C6 0.057(3) 0.062(3) 0.053(3) -0.010(3) 0.027(3) -0.016(3) C7 0.052(3) 0.043(3) 0.061(4) 0.003(2) 0.022(3) -0.005(2) C8 0.046(3) 0.048(3) 0.055(3) -0.017(2) 0.015(2) -0.017(2) C9 0.036(3) 0.059(3) 0.060(3) -0.002(3) 0.009(2) -0.009(2) C10 0.047(3) 0.051(3) 0.083(4) -0.007(3) 0.030(3) 0.000(3) C11 0.035(3) 0.038(3) 0.049(3) 0.005(2) 0.011(2) -0.003(2) C12 0.048(3) 0.037(3) 0.051(3) 0.004(2) 0.017(2) 0.003(2) C13 0.069(4) 0.042(3) 0.073(4) 0.000(3) 0.036(3) 0.012(3) C14 0.101(5) 0.043(3) 0.053(4) -0.009(3) 0.034(3) 0.003(3) C15 0.085(4) 0.043(3) 0.043(3) 0.000(2) 0.012(3) -0.008(3) C16 0.057(3) 0.038(3) 0.039(3) -0.002(2) 0.012(2) 0.001(2) C17 0.042(3) 0.033(2) 0.039(3) 0.004(2) 0.012(2) 0.001(2) O1 0.073(2) 0.055(2) 0.0311(18) -0.0005(16) 0.0010(16) -0.0116(18) C18 0.071(4) 0.061(4) 0.050(3) -0.004(3) 0.001(3) -0.028(3) C19 0.106(5) 0.094(4) 0.040(3) -0.014(3) 0.001(3) -0.013(4) C20 0.173(6) 0.115(5) 0.050(4) 0.003(4) -0.009(4) -0.048(5) C21 0.182(8) 0.073(4) 0.039(3) 0.012(3) 0.006(4) -0.001(4) O2 0.059(7) 0.074(7) 0.115(9) -0.032(6) 0.000(6) 0.029(5) C22 0.085(8) 0.079(9) 0.103(9) -0.020(7) 0.023(7) 0.011(6) C23 0.143(11) 0.101(9) 0.131(10) 0.020(8) 0.045(8) 0.012(8) C24 0.076(8) 0.100(9) 0.108(9) 0.000(8) -0.004(7) 0.024(7) C25 0.089(13) 0.058(10) 0.14(2) -0.027(11) -0.009(16) 0.001(8) O2' 0.052(8) 0.067(10) 0.089(10) -0.020(7) 0.012(7) 0.029(6) C22' 0.085(10) 0.086(10) 0.100(11) -0.015(8) 0.026(8) 0.000(7) C23' 0.104(10) 0.088(10) 0.121(11) -0.009(8) 0.017(8) 0.029(8) C24' 0.130(15) 0.140(15) 0.125(14) -0.025(9) 0.023(9) 0.011(9) C25' 0.098(15) 0.094(16) 0.114(15) 0.003(9) 0.031(10) -0.014(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 Er1 N1 2.367(3) . ? Er1 O1 2.462(3) . ? Er1 C10 2.633(5) . ? Er1 C4 2.635(5) . ? Er1 C3 2.636(5) . ? Er1 C9 2.642(4) . ? Er1 C5 2.647(4) . ? Er1 C2 2.650(5) . ? Er1 C1 2.655(4) . ? Er1 C6 2.657(4) . ? Er1 C8 2.667(4) . ? Er1 C7 2.672(4) . ? Er1 S1 2.8443(15) . ? Er1 C11 2.962(4) . ? S1 C11 1.708(5) . ? N1 C11 1.333(5) . ? N1 C17 1.400(5) . ? N2 C11 1.362(6) . ? N2 C12 1.395(6) . ? N2 H2N 0.840(19) . ? C1 C2 1.371(7) . ? C1 C5 1.394(6) . ? C1 H1A 0.9300 . ? C2 C3 1.391(6) . ? C2 H2A 0.9300 . ? C3 C4 1.389(7) . ? C3 H3A 0.9300 . ? C4 C5 1.373(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C10 1.384(7) . ? C6 C7 1.401(6) . ? C6 H6A 0.9300 . ? C7 C8 1.400(6) . ? C7 H7A 0.9300 . ? C8 C9 1.389(6) . ? C8 H8A 0.9300 . ? C9 C10 1.401(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C12 C13 1.373(6) . ? C12 C17 1.399(6) . ? C13 C14 1.372(7) . ? C13 H13A 0.9300 . ? C14 C15 1.382(7) . ? C14 H14A 0.9300 . ? C15 C16 1.384(6) . ? C15 H15A 0.9300 . ? C16 C17 1.379(6) . ? C16 H16A 0.9300 . ? O1 C18 1.428(5) . ? O1 C21 1.447(7) . ? C18 C19 1.492(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.475(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.376(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O2 C25 1.391(12) . ? O2 C22 1.489(8) . ? C22 C23 1.598(15) . ? C22 H22C 0.9700 . ? C22 H22D 0.9700 . ? C23 C24 1.527(9) . ? C23 H23C 0.9700 . ? C23 H23D 0.9700 . ? C24 C25 1.534(19) . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? O2' C25' 1.400(15) . ? O2' C22' 1.507(16) . ? C22' C23' 1.588(17) . ? C22' H22A 0.9700 . ? C22' H22B 0.9700 . ? C23' C24' 1.558(17) . ? C23' H23A 0.9700 . ? C23' H23B 0.9700 . ? C24' C25' 1.54(2) . ? C24' H24A 0.9700 . ? C24' H24B 0.9700 . ? C25' H25C 0.9700 . ? C25' H25D 0.9700 . ? 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 N1 Er1 O1 135.29(11) . . ? N1 Er1 C10 119.55(14) . . ? O1 Er1 C10 93.01(15) . . ? N1 Er1 C4 108.03(15) . . ? O1 Er1 C4 108.32(15) . . ? C10 Er1 C4 77.71(17) . . ? N1 Er1 C3 78.60(15) . . ? O1 Er1 C3 128.69(14) . . ? C10 Er1 C3 99.19(18) . . ? C4 Er1 C3 30.57(15) . . ? N1 Er1 C9 89.67(14) . . ? O1 Er1 C9 122.35(14) . . ? C10 Er1 C9 30.80(14) . . ? C4 Er1 C9 78.71(16) . . ? C3 Er1 C9 86.37(17) . . ? N1 Er1 C5 125.16(13) . . ? O1 Er1 C5 80.46(13) . . ? C10 Er1 C5 90.16(16) . . ? C4 Er1 C5 30.12(14) . . ? C3 Er1 C5 50.12(16) . . ? C9 Er1 C5 103.19(16) . . ? N1 Er1 C2 76.42(15) . . ? O1 Er1 C2 109.03(14) . . ? C10 Er1 C2 127.25(17) . . ? C4 Er1 C2 50.20(16) . . ? C3 Er1 C2 30.50(14) . . ? C9 Er1 C2 116.63(16) . . ? C5 Er1 C2 49.96(15) . . ? N1 Er1 C1 103.70(14) . . ? O1 Er1 C1 81.00(13) . . ? C10 Er1 C1 120.63(16) . . ? C4 Er1 C1 50.05(15) . . ? C3 Er1 C1 50.04(16) . . ? C9 Er1 C1 128.75(16) . . ? C5 Er1 C1 30.48(13) . . ? C2 Er1 C1 29.95(14) . . ? N1 Er1 C6 119.22(13) . . ? O1 Er1 C6 73.72(13) . . ? C10 Er1 C6 30.34(14) . . ? C4 Er1 C6 105.88(17) . . ? C3 Er1 C6 129.53(18) . . ? C9 Er1 C6 50.37(16) . . ? C5 Er1 C6 109.20(16) . . ? C2 Er1 C6 155.98(17) . . ? C1 Er1 C6 136.51(16) . . ? N1 Er1 C8 72.08(13) . . ? O1 Er1 C8 119.30(13) . . ? C10 Er1 C8 50.33(15) . . ? C4 Er1 C8 107.52(16) . . ? C3 Er1 C8 106.32(16) . . ? C9 Er1 C8 30.33(14) . . ? C5 Er1 C8 133.52(15) . . ? C2 Er1 C8 131.55(16) . . ? C1 Er1 C8 155.74(15) . . ? C6 Er1 C8 50.12(15) . . ? N1 Er1 C7 89.61(13) . . ? O1 Er1 C7 89.29(13) . . ? C10 Er1 C7 50.42(15) . . ? C4 Er1 C7 126.36(15) . . ? C3 Er1 C7 135.46(16) . . ? C9 Er1 C7 50.40(16) . . ? C5 Er1 C7 138.84(15) . . ? C2 Er1 C7 161.62(16) . . ? C1 Er1 C7 166.68(16) . . ? C6 Er1 C7 30.50(14) . . ? C8 Er1 C7 30.39(13) . . ? N1 Er1 S1 60.09(8) . . ? O1 Er1 S1 75.49(9) . . ? C10 Er1 S1 144.07(12) . . ? C4 Er1 S1 138.17(12) . . ? C3 Er1 S1 114.70(14) . . ? C9 Er1 S1 135.84(12) . . ? C5 Er1 S1 120.28(11) . . ? C2 Er1 S1 88.54(12) . . ? C1 Er1 S1 91.55(12) . . ? C6 Er1 S1 114.79(13) . . ? C8 Er1 S1 105.79(11) . . ? C7 Er1 S1 94.83(11) . . ? N1 Er1 C11 26.02(11) . . ? O1 Er1 C11 109.59(12) . . ? C10 Er1 C11 137.99(14) . . ? C4 Er1 C11 124.02(15) . . ? C3 Er1 C11 93.62(16) . . ? C9 Er1 C11 111.91(14) . . ? C5 Er1 C11 127.37(13) . . ? C2 Er1 C11 79.06(15) . . ? C1 Er1 C11 98.16(14) . . ? C6 Er1 C11 123.33(14) . . ? C8 Er1 C11 87.68(13) . . ? C7 Er1 C11 93.66(13) . . ? S1 Er1 C11 34.13(9) . . ? C11 S1 Er1 76.72(15) . . ? C11 N1 C17 106.0(3) . . ? C11 N1 Er1 102.8(3) . . ? C17 N1 Er1 151.0(3) . . ? C11 N2 C12 107.7(4) . . ? C11 N2 H2N 126(3) . . ? C12 N2 H2N 126(3) . . ? C2 C1 C5 108.0(5) . . ? C2 C1 Er1 74.8(3) . . ? C5 C1 Er1 74.4(3) . . ? C2 C1 H1A 126.0 . . ? C5 C1 H1A 126.0 . . ? Er1 C1 H1A 116.8 . . ? C1 C2 C3 108.3(5) . . ? C1 C2 Er1 75.2(3) . . ? C3 C2 Er1 74.2(3) . . ? C1 C2 H2A 125.9 . . ? C3 C2 H2A 125.9 . . ? Er1 C2 H2A 116.7 . . ? C4 C3 C2 107.5(5) . . ? C4 C3 Er1 74.7(3) . . ? C2 C3 Er1 75.3(3) . . ? C4 C3 H3A 126.3 . . ? C2 C3 H3A 126.3 . . ? Er1 C3 H3A 116.0 . . ? C5 C4 C3 108.2(5) . . ? C5 C4 Er1 75.4(3) . . ? C3 C4 Er1 74.8(3) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Er1 C4 H4A 116.0 . . ? C4 C5 C1 108.0(5) . . ? C4 C5 Er1 74.5(3) . . ? C1 C5 Er1 75.1(3) . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? Er1 C5 H5A 116.5 . . ? C10 C6 C7 108.4(5) . . ? C10 C6 Er1 73.9(3) . . ? C7 C6 Er1 75.3(3) . . ? C10 C6 H6A 125.8 . . ? C7 C6 H6A 125.8 . . ? Er1 C6 H6A 117.0 . . ? C8 C7 C6 107.2(5) . . ? C8 C7 Er1 74.6(3) . . ? C6 C7 Er1 74.2(3) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? Er1 C7 H7A 117.0 . . ? C9 C8 C7 108.5(4) . . ? C9 C8 Er1 73.8(3) . . ? C7 C8 Er1 75.0(2) . . ? C9 C8 H8A 125.8 . . ? C7 C8 H8A 125.8 . . ? Er1 C8 H8A 117.4 . . ? C8 C9 C10 107.8(5) . . ? C8 C9 Er1 75.8(2) . . ? C10 C9 Er1 74.2(3) . . ? C8 C9 H9A 126.1 . . ? C10 C9 H9A 126.1 . . ? Er1 C9 H9A 116.0 . . ? C6 C10 C9 108.1(4) . . ? C6 C10 Er1 75.8(3) . . ? C9 C10 Er1 75.0(3) . . ? C6 C10 H10A 125.9 . . ? C9 C10 H10A 125.9 . . ? Er1 C10 H10A 115.5 . . ? N1 C11 N2 111.7(4) . . ? N1 C11 S1 120.1(3) . . ? N2 C11 S1 128.2(3) . . ? N1 C11 Er1 51.2(2) . . ? N2 C11 Er1 162.6(3) . . ? S1 C11 Er1 69.15(15) . . ? C13 C12 N2 132.4(4) . . ? C13 C12 C17 122.2(5) . . ? N2 C12 C17 105.4(4) . . ? C14 C13 C12 117.2(5) . . ? C14 C13 H13A 121.4 . . ? C12 C13 H13A 121.4 . . ? C13 C14 C15 121.5(5) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C14 C15 C16 121.4(5) . . ? C14 C15 H15A 119.3 . . ? C16 C15 H15A 119.3 . . ? C17 C16 C15 117.7(5) . . ? C17 C16 H16A 121.1 . . ? C15 C16 H16A 121.1 . . ? C16 C17 C12 120.0(4) . . ? C16 C17 N1 130.8(4) . . ? C12 C17 N1 109.2(4) . . ? C18 O1 C21 106.1(4) . . ? C18 O1 Er1 130.9(3) . . ? C21 O1 Er1 120.9(3) . . ? O1 C18 C19 106.9(4) . . ? O1 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O1 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C18 104.1(5) . . ? C20 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? C20 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C21 C20 C19 108.9(6) . . ? C21 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? C21 C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C20 C21 O1 109.8(6) . . ? C20 C21 H21A 109.7 . . ? O1 C21 H21A 109.7 . . ? C20 C21 H21B 109.7 . . ? O1 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C25 O2 C22 110.2(11) . . ? O2 C22 C23 94.8(11) . . ? O2 C22 H22C 112.8 . . ? C23 C22 H22C 112.8 . . ? O2 C22 H22D 112.8 . . ? C23 C22 H22D 112.8 . . ? H22C C22 H22D 110.2 . . ? C24 C23 C22 95.0(11) . . ? C24 C23 H23C 112.7 . . ? C22 C23 H23C 112.7 . . ? C24 C23 H23D 112.7 . . ? C22 C23 H23D 112.7 . . ? H23C C23 H23D 110.2 . . ? C23 C24 C25 96.8(13) . . ? C23 C24 H24C 112.4 . . ? C25 C24 H24C 112.4 . . ? C23 C24 H24D 112.4 . . ? C25 C24 H24D 112.4 . . ? H24C C24 H24D 110.0 . . ? O2 C25 C24 105.0(12) . . ? O2 C25 H25A 110.8 . . ? C24 C25 H25A 110.8 . . ? O2 C25 H25B 110.8 . . ? C24 C25 H25B 110.8 . . ? H25A C25 H25B 108.8 . . ? C25' O2' C22' 105.4(15) . . ? O2' C22' C23' 93.9(13) . . ? O2' C22' H22A 112.9 . . ? C23' C22' H22A 112.9 . . ? O2' C22' H22B 112.9 . . ? C23' C22' H22B 112.9 . . ? H22A C22' H22B 110.4 . . ? C24' C23' C22' 92.4(14) . . ? C24' C23' H23A 113.2 . . ? C22' C23' H23A 113.2 . . ? C24' C23' H23B 113.2 . . ? C22' C23' H23B 113.2 . . ? H23A C23' H23B 110.6 . . ? C25' C24' C23' 93.8(17) . . ? C25' C24' H24A 113.0 . . ? C23' C24' H24A 113.0 . . ? C25' C24' H24B 113.0 . . ? C23' C24' H24B 113.0 . . ? H24A C24' H24B 110.4 . . ? O2' C25' C24' 107.6(15) . . ? O2' C25' H25C 110.2 . . ? C24' C25' H25C 110.2 . . ? O2' C25' H25D 110.2 . . ? C24' C25' H25D 110.2 . . ? H25C C25' H25D 108.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N O2 0.840(19) 1.90(2) 2.733(14) 174(5) . N2 H2N O2' 0.840(19) 2.09(3) 2.926(18) 173(4) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.823 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.090 # Attachment '2.cif' data_f70416b _database_code_depnum_ccdc_archive 'CCDC 762742' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H31 N4 O2 S2 Yb' _chemical_formula_weight 680.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.022(7) _cell_length_b 8.927(3) _cell_length_c 18.578(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.271(4) _cell_angle_gamma 90.00 _cell_volume 2804.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 957 _cell_measurement_theta_min 3.132 _cell_measurement_theta_max 24.435 _exptl_crystal_description cubiod _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 3.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4186 _exptl_absorpt_correction_T_max 0.5400 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12307 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5461 _reflns_number_gt 4160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU and ISOR were used to restrain some abnormal ADPs. The THF molecule (O2, etc. and O2', etc.) is modeled isotropically due to severe disorder. ; _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^)+(0.0689P)^2^+0.5000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5461 _refine_ls_number_parameters 364 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.145838(15) 1.03972(3) 0.731825(17) 0.04432(12) Uani 1 1 d . A . S1 S 0.27324(11) 1.24164(18) 0.80652(11) 0.0538(4) Uani 1 1 d . A . S2 S 0.11195(10) 0.7470(2) 0.68359(13) 0.0625(5) Uani 1 1 d . A . N1 N 0.2223(3) 1.0974(6) 0.6670(3) 0.0447(12) Uani 1 1 d . A . N2 N 0.3311(3) 1.2247(6) 0.6957(4) 0.0557(14) Uani 1 1 d D . . H2N H 0.346(4) 1.309(4) 0.720(4) 0.067 Uiso 1 1 d D . . N3 N 0.2484(3) 0.8593(5) 0.7920(3) 0.0460(13) Uani 1 1 d . A . N4 N 0.2571(3) 0.6156(6) 0.7805(4) 0.0495(13) Uani 1 1 d D A . H4N H 0.251(4) 0.521(3) 0.779(5) 0.059 Uiso 1 1 d D . . C1 C 0.0027(5) 1.1227(13) 0.6945(7) 0.089(3) Uani 1 1 d . A . H1A H -0.0181 1.0854 0.7275 0.107 Uiso 1 1 calc R . . C2 C 0.0447(6) 1.2555(13) 0.7075(7) 0.097(3) Uani 1 1 d . A . H2A H 0.0565 1.3231 0.7496 0.117 Uiso 1 1 calc R . . C3 C 0.0660(5) 1.2679(10) 0.6438(6) 0.082(3) Uani 1 1 d . A . H3A H 0.0951 1.3447 0.6364 0.098 Uiso 1 1 calc R . . C4 C 0.0353(5) 1.1439(12) 0.5954(5) 0.085(3) Uani 1 1 d . A . H4A H 0.0396 1.1221 0.5486 0.102 Uiso 1 1 calc R . . C5 C -0.0030(5) 1.0576(11) 0.6282(8) 0.091(3) Uani 1 1 d . A . H5A H -0.0288 0.9676 0.6070 0.109 Uiso 1 1 calc R . . C6 C 0.2770(4) 1.1865(7) 0.7207(4) 0.0455(14) Uani 1 1 d . A . C7 C 0.3098(4) 1.1552(8) 0.6215(4) 0.0537(17) Uani 1 1 d . A . C8 C 0.3432(5) 1.1593(11) 0.5696(5) 0.079(2) Uani 1 1 d . . . H8A H 0.3885 1.2147 0.5810 0.095 Uiso 1 1 calc R A . C9 C 0.3048(6) 1.0750(12) 0.4989(5) 0.090(3) Uani 1 1 d . A . H9A H 0.3260 1.0725 0.4627 0.108 Uiso 1 1 calc R . . C10 C 0.2379(6) 0.9969(11) 0.4811(5) 0.076(2) Uani 1 1 d . . . H10A H 0.2142 0.9436 0.4328 0.092 Uiso 1 1 calc R A . C11 C 0.2037(5) 0.9942(9) 0.5329(5) 0.064(2) Uani 1 1 d . A . H11A H 0.1582 0.9390 0.5210 0.077 Uiso 1 1 calc R . . C12 C 0.2407(4) 1.0775(7) 0.6034(4) 0.0486(16) Uani 1 1 d . . . C13 C 0.2097(4) 0.7370(7) 0.7544(4) 0.0458(15) Uani 1 1 d . . . C14 C 0.3308(4) 0.6623(7) 0.8366(4) 0.0452(14) Uani 1 1 d . . . C15 C 0.4005(4) 0.5844(8) 0.8800(5) 0.0561(18) Uani 1 1 d . A . H15A H 0.4036 0.4814 0.8743 0.067 Uiso 1 1 calc R . . C16 C 0.4646(4) 0.6661(8) 0.9317(5) 0.0595(19) Uani 1 1 d . . . H16A H 0.5122 0.6173 0.9631 0.071 Uiso 1 1 calc R A . C17 C 0.4604(4) 0.8209(9) 0.9383(5) 0.0635(19) Uani 1 1 d . A . H17A H 0.5057 0.8736 0.9724 0.076 Uiso 1 1 calc R . . C18 C 0.3901(4) 0.8984(8) 0.8951(4) 0.0545(17) Uani 1 1 d . . . H18A H 0.3872 1.0014 0.9009 0.065 Uiso 1 1 calc R A . C19 C 0.3243(4) 0.8162(7) 0.8427(4) 0.0442(14) Uani 1 1 d . A . O1 O 0.1498(3) 1.0205(6) 0.8600(3) 0.0650(13) Uani 0.49(2) 1 d PD A 1 C20 C 0.1602(14) 0.8916(15) 0.9059(9) 0.060(5) Uani 0.49(2) 1 d PD A 1 H20A H 0.2142 0.8563 0.9260 0.071 Uiso 0.49(2) 1 calc PR A 1 H20B H 0.1251 0.8137 0.8720 0.071 Uiso 0.49(2) 1 calc PR A 1 C21 C 0.1440(13) 0.919(2) 0.9737(10) 0.064(6) Uani 0.49(2) 1 d PD A 1 H21A H 0.0995 0.8596 0.9691 0.077 Uiso 0.49(2) 1 calc PR A 1 H21B H 0.1898 0.8950 1.0245 0.077 Uiso 0.49(2) 1 calc PR A 1 C22 C 0.1261(19) 1.077(2) 0.9696(13) 0.093(9) Uani 0.49(2) 1 d PD A 1 H22A H 0.0799 1.0947 0.9777 0.112 Uiso 0.49(2) 1 calc PR A 1 H22B H 0.1704 1.1329 1.0100 0.112 Uiso 0.49(2) 1 calc PR A 1 C23 C 0.1114(17) 1.118(2) 0.8903(13) 0.101(9) Uani 0.49(2) 1 d PD A 1 H23A H 0.0549 1.1153 0.8548 0.121 Uiso 0.49(2) 1 calc PR A 1 H23B H 0.1297 1.2194 0.8908 0.121 Uiso 0.49(2) 1 calc PR A 1 O1' O 0.1498(3) 1.0205(6) 0.8600(3) 0.0650(13) Uani 0.51(2) 1 d PDU A 2 C20' C 0.188(2) 0.902(2) 0.9129(14) 0.149(16) Uani 0.51(2) 1 d PDU A 2 H20C H 0.2431 0.9001 0.9260 0.179 Uiso 0.51(2) 1 calc PR A 2 H20D H 0.1640 0.8077 0.8873 0.179 Uiso 0.51(2) 1 calc PR A 2 C21' C 0.179(3) 0.921(3) 0.9865(17) 0.20(3) Uani 0.51(2) 1 d PD A 2 H21C H 0.1321 0.8719 0.9819 0.236 Uiso 0.51(2) 1 calc PR A 2 H21D H 0.2250 0.8813 1.0331 0.236 Uiso 0.51(2) 1 calc PR A 2 C22' C 0.174(3) 1.079(3) 0.9933(13) 0.135(14) Uani 0.51(2) 1 d PDU A 2 H22C H 0.1294 1.1050 1.0027 0.162 Uiso 0.51(2) 1 calc PR A 2 H22D H 0.2220 1.1186 1.0373 0.162 Uiso 0.51(2) 1 calc PR A 2 C23' C 0.1636(15) 1.1352(17) 0.9177(10) 0.082(3) Uani 0.51(2) 1 d PDU A 2 H23C H 0.1192 1.2041 0.8965 0.099 Uiso 0.51(2) 1 calc PR A 2 H23D H 0.2105 1.1909 0.9258 0.099 Uiso 0.51(2) 1 calc PR A 2 O2 O 0.4949(8) 0.226(2) 0.2889(9) 0.058(4) Uiso 0.45(3) 1 d P B 1 C24 C 0.5526(15) 0.246(4) 0.2651(16) 0.095(8) Uiso 0.45(3) 1 d P B 1 H24C H 0.5302 0.2896 0.2112 0.114 Uiso 0.45(3) 1 calc PR B 1 H24D H 0.5767 0.1511 0.2641 0.114 Uiso 0.45(3) 1 calc PR B 1 C25 C 0.6112(17) 0.347(4) 0.3235(16) 0.105(9) Uiso 0.45(3) 1 d P B 1 H25C H 0.6011 0.4505 0.3059 0.126 Uiso 0.45(3) 1 calc PR B 1 H25D H 0.6645 0.3199 0.3343 0.126 Uiso 0.45(3) 1 calc PR B 1 C26 C 0.5967(13) 0.318(3) 0.3965(14) 0.080(7) Uiso 0.45(3) 1 d P B 1 H26A H 0.6413 0.2637 0.4375 0.096 Uiso 0.45(3) 1 calc PR B 1 H26B H 0.5924 0.4129 0.4197 0.096 Uiso 0.45(3) 1 calc PR B 1 C27 C 0.5249(11) 0.232(2) 0.3734(12) 0.063(6) Uiso 0.45(3) 1 d P B 1 H27A H 0.5363 0.1328 0.3972 0.075 Uiso 0.45(3) 1 calc PR B 1 H27B H 0.4887 0.2828 0.3888 0.075 Uiso 0.45(3) 1 calc PR B 1 O2' O 0.4908(8) 0.177(2) 0.2942(8) 0.074(4) Uiso 0.55(3) 1 d P B 2 C24' C 0.5541(14) 0.167(4) 0.2789(15) 0.110(8) Uiso 0.55(3) 1 d P B 2 H24A H 0.5382 0.1960 0.2232 0.133 Uiso 0.55(3) 1 calc PR B 2 H24B H 0.5726 0.0644 0.2859 0.133 Uiso 0.55(3) 1 calc PR B 2 C25' C 0.6203(12) 0.267(3) 0.3348(14) 0.096(7) Uiso 0.55(3) 1 d PD B 2 H25A H 0.6439 0.3178 0.3049 0.115 Uiso 0.55(3) 1 calc PR B 2 H25B H 0.6610 0.2082 0.3773 0.115 Uiso 0.55(3) 1 calc PR B 2 C26' C 0.5876(17) 0.382(3) 0.372(2) 0.148(11) Uiso 0.55(3) 1 d PD B 2 H26C H 0.5779 0.4782 0.3447 0.177 Uiso 0.55(3) 1 calc PR B 2 H26D H 0.6207 0.3943 0.4294 0.177 Uiso 0.55(3) 1 calc PR B 2 C27' C 0.512(2) 0.297(5) 0.352(2) 0.167(13) Uiso 0.55(3) 1 d P B 2 H27C H 0.5161 0.2554 0.4022 0.200 Uiso 0.55(3) 1 calc PR B 2 H27D H 0.4686 0.3679 0.3322 0.200 Uiso 0.55(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.04306(17) 0.04060(17) 0.0544(2) 0.00178(13) 0.02669(14) 0.00259(11) S1 0.0696(11) 0.0410(8) 0.0583(11) -0.0084(8) 0.0358(9) -0.0068(8) S2 0.0432(9) 0.0514(9) 0.0791(14) -0.0097(9) 0.0162(9) -0.0077(7) N1 0.045(3) 0.043(3) 0.050(3) -0.002(2) 0.026(2) 0.000(2) N2 0.054(3) 0.060(3) 0.058(4) -0.003(3) 0.030(3) -0.014(3) N3 0.038(3) 0.039(3) 0.059(3) -0.007(2) 0.020(2) -0.002(2) N4 0.046(3) 0.034(2) 0.073(4) -0.008(3) 0.031(3) 0.000(2) C1 0.060(5) 0.100(7) 0.126(9) 0.039(7) 0.059(6) 0.030(5) C2 0.089(7) 0.100(8) 0.094(7) -0.005(6) 0.034(6) 0.050(6) C3 0.064(5) 0.075(6) 0.102(7) 0.038(6) 0.034(5) 0.019(4) C4 0.070(5) 0.111(8) 0.066(6) 0.015(6) 0.025(5) 0.031(5) C5 0.042(4) 0.078(6) 0.123(9) 0.008(6) 0.013(5) 0.011(4) C6 0.047(3) 0.040(3) 0.050(4) 0.000(3) 0.023(3) 0.001(3) C7 0.048(4) 0.071(4) 0.050(4) 0.005(4) 0.029(3) 0.002(3) C8 0.067(5) 0.115(7) 0.071(6) 0.008(5) 0.046(4) -0.002(5) C9 0.091(7) 0.138(9) 0.057(5) 0.003(6) 0.047(5) 0.007(6) C10 0.076(6) 0.102(6) 0.052(5) -0.009(4) 0.030(4) 0.009(5) C11 0.065(5) 0.070(5) 0.053(5) -0.005(4) 0.023(4) 0.000(4) C12 0.045(3) 0.053(4) 0.052(4) 0.004(3) 0.025(3) 0.006(3) C13 0.047(3) 0.039(3) 0.059(4) -0.001(3) 0.031(3) -0.005(3) C14 0.046(3) 0.044(3) 0.052(4) 0.002(3) 0.028(3) -0.001(3) C15 0.053(4) 0.052(4) 0.070(5) 0.015(4) 0.034(4) 0.013(3) C16 0.042(3) 0.066(4) 0.064(5) 0.013(4) 0.018(3) 0.011(3) C17 0.052(4) 0.068(4) 0.061(5) -0.005(4) 0.017(3) -0.007(3) C18 0.053(4) 0.048(3) 0.057(4) -0.005(3) 0.021(3) -0.003(3) C19 0.050(3) 0.038(3) 0.048(4) -0.004(3) 0.026(3) -0.006(3) O1 0.081(3) 0.063(3) 0.067(3) 0.004(3) 0.048(3) 0.001(3) C20 0.075(12) 0.064(10) 0.039(9) -0.005(8) 0.026(8) -0.015(8) C21 0.073(12) 0.082(15) 0.049(10) -0.002(9) 0.038(9) -0.022(11) C22 0.12(2) 0.12(2) 0.063(14) -0.028(13) 0.063(15) -0.017(16) C23 0.106(19) 0.126(18) 0.066(14) -0.016(13) 0.035(13) 0.041(15) O1' 0.081(3) 0.063(3) 0.067(3) 0.004(3) 0.048(3) 0.001(3) C20' 0.15(2) 0.19(2) 0.13(2) 0.045(16) 0.080(16) 0.064(15) C21' 0.22(5) 0.25(5) 0.19(4) 0.08(4) 0.15(4) 0.13(4) C22' 0.16(3) 0.17(3) 0.082(15) -0.014(17) 0.06(2) -0.04(3) C23' 0.097(6) 0.074(5) 0.078(5) -0.001(5) 0.042(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 Yb1 N1 2.332(5) . ? Yb1 O1 2.354(5) . ? Yb1 N3 2.377(5) . ? Yb1 C1 2.591(8) . ? Yb1 C5 2.599(8) . ? Yb1 C2 2.612(8) . ? Yb1 C4 2.613(8) . ? Yb1 C3 2.618(8) . ? Yb1 S2 2.742(2) . ? Yb1 S1 2.8224(19) . ? Yb1 C6 2.908(6) . ? S1 C6 1.702(7) . ? S2 C13 1.719(6) . ? N1 C6 1.326(8) . ? N1 C12 1.389(8) . ? N2 C6 1.352(8) . ? N2 C7 1.392(9) . ? N2 H2N 0.85(2) . ? N3 C13 1.323(7) . ? N3 C19 1.369(8) . ? N4 C13 1.350(8) . ? N4 C14 1.374(8) . ? N4 H4N 0.85(2) . ? C1 C5 1.322(14) . ? C1 C2 1.387(14) . ? C1 H1A 0.9300 . ? C2 C3 1.420(14) . ? C2 H2A 0.9300 . ? C3 C4 1.377(13) . ? C3 H3A 0.9300 . ? C4 C5 1.380(13) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 C8 1.375(10) . ? C7 C12 1.386(9) . ? C8 C9 1.396(12) . ? C8 H8A 0.9300 . ? C9 C10 1.353(13) . ? C9 H9A 0.9300 . ? C10 C11 1.388(12) . ? C10 H10A 0.9300 . ? C11 C12 1.384(10) . ? C11 H11A 0.9300 . ? C14 C15 1.382(9) . ? C14 C19 1.389(8) . ? C15 C16 1.367(10) . ? C15 H15A 0.9300 . ? C16 C17 1.393(10) . ? C16 H16A 0.9300 . ? C17 C18 1.388(10) . ? C17 H17A 0.9300 . ? C18 C19 1.392(8) . ? C18 H18A 0.9300 . ? O1 C20 1.392(13) . ? O1 C23 1.408(13) . ? C20 C21 1.448(17) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.444(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.416(17) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C20' C21' 1.455(18) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.421(13) . ? C21' H21C 0.9700 . ? C21' H21D 0.9700 . ? C22' C23' 1.418(17) . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C23' H23C 0.9700 . ? C23' H23D 0.9700 . ? O2 C24 1.37(3) . ? O2 C27 1.40(3) . ? C24 C25 1.46(3) . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C25 C26 1.52(3) . ? C25 H25C 0.9700 . ? C25 H25D 0.9700 . ? C26 C27 1.45(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? O2' C24' 1.36(2) . ? O2' C27' 1.44(4) . ? C24' C25' 1.51(3) . ? C24' H24A 0.9700 . ? C24' H24B 0.9700 . ? C25' C26' 1.513(10) . ? C25' H25A 0.9700 . ? C25' H25B 0.9700 . ? C26' C27' 1.52(4) . ? C26' H26C 0.9700 . ? C26' H26D 0.9700 . ? C27' H27C 0.9700 . ? C27' H27D 0.9700 . ? 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 N1 Yb1 O1 143.12(19) . . ? N1 Yb1 N3 79.66(18) . . ? O1 Yb1 N3 80.56(19) . . ? N1 Yb1 C1 128.8(3) . . ? O1 Yb1 C1 80.5(3) . . ? N3 Yb1 C1 148.8(3) . . ? N1 Yb1 C5 109.3(3) . . ? O1 Yb1 C5 105.9(4) . . ? N3 Yb1 C5 140.4(3) . . ? C1 Yb1 C5 29.5(3) . . ? N1 Yb1 C2 109.4(3) . . ? O1 Yb1 C2 84.8(3) . . ? N3 Yb1 C2 164.2(3) . . ? C1 Yb1 C2 30.9(3) . . ? C5 Yb1 C2 50.2(3) . . ? N1 Yb1 C4 80.5(3) . . ? O1 Yb1 C4 130.3(3) . . ? N3 Yb1 C4 145.0(3) . . ? C1 Yb1 C4 50.1(3) . . ? C5 Yb1 C4 30.7(3) . . ? C2 Yb1 C4 50.8(3) . . ? N1 Yb1 C3 80.0(3) . . ? O1 Yb1 C3 115.4(3) . . ? N3 Yb1 C3 159.5(3) . . ? C1 Yb1 C3 51.2(3) . . ? C5 Yb1 C3 50.7(3) . . ? C2 Yb1 C3 31.5(3) . . ? C4 Yb1 C3 30.5(3) . . ? N1 Yb1 S2 98.66(13) . . ? O1 Yb1 S2 98.92(13) . . ? N3 Yb1 S2 61.78(12) . . ? C1 Yb1 S2 97.1(3) . . ? C5 Yb1 S2 78.6(2) . . ? C2 Yb1 S2 127.0(3) . . ? C4 Yb1 S2 93.3(3) . . ? C3 Yb1 S2 123.7(2) . . ? N1 Yb1 S1 60.95(13) . . ? O1 Yb1 S1 85.79(14) . . ? N3 Yb1 S1 82.35(13) . . ? C1 Yb1 S1 120.6(3) . . ? C5 Yb1 S1 136.4(2) . . ? C2 Yb1 S1 90.7(3) . . ? C4 Yb1 S1 112.2(3) . . ? C3 Yb1 S1 86.1(2) . . ? S2 Yb1 S1 142.16(5) . . ? N1 Yb1 C6 26.50(17) . . ? O1 Yb1 C6 118.28(19) . . ? N3 Yb1 C6 78.04(17) . . ? C1 Yb1 C6 133.1(3) . . ? C5 Yb1 C6 126.8(3) . . ? C2 Yb1 C6 104.1(3) . . ? C4 Yb1 C6 96.1(3) . . ? C3 Yb1 C6 82.9(2) . . ? S2 Yb1 C6 119.14(13) . . ? S1 Yb1 C6 34.51(13) . . ? C6 S1 Yb1 75.5(2) . . ? C13 S2 Yb1 77.9(2) . . ? C6 N1 C12 107.5(5) . . ? C6 N1 Yb1 101.8(4) . . ? C12 N1 Yb1 150.5(4) . . ? C6 N2 C7 107.8(5) . . ? C6 N2 H2N 99(5) . . ? C7 N2 H2N 142(5) . . ? C13 N3 C19 106.7(5) . . ? C13 N3 Yb1 100.0(4) . . ? C19 N3 Yb1 153.3(4) . . ? C13 N4 C14 108.1(5) . . ? C13 N4 H4N 137(5) . . ? C14 N4 H4N 113(5) . . ? C5 C1 C2 109.4(10) . . ? C5 C1 Yb1 75.6(5) . . ? C2 C1 Yb1 75.4(5) . . ? C5 C1 H1A 125.3 . . ? C2 C1 H1A 125.3 . . ? Yb1 C1 H1A 115.7 . . ? C1 C2 C3 106.5(9) . . ? C1 C2 Yb1 73.7(5) . . ? C3 C2 Yb1 74.5(5) . . ? C1 C2 H2A 126.7 . . ? C3 C2 H2A 126.7 . . ? Yb1 C2 H2A 117.3 . . ? C4 C3 C2 106.5(9) . . ? C4 C3 Yb1 74.5(5) . . ? C2 C3 Yb1 74.0(5) . . ? C4 C3 H3A 126.8 . . ? C2 C3 H3A 126.8 . . ? Yb1 C3 H3A 116.9 . . ? C3 C4 C5 108.2(9) . . ? C3 C4 Yb1 74.9(5) . . ? C5 C4 Yb1 74.1(5) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Yb1 C4 H4A 117.1 . . ? C1 C5 C4 109.4(10) . . ? C1 C5 Yb1 74.9(5) . . ? C4 C5 Yb1 75.2(5) . . ? C1 C5 H5A 125.3 . . ? C4 C5 H5A 125.3 . . ? Yb1 C5 H5A 116.5 . . ? N1 C6 N2 110.6(6) . . ? N1 C6 S1 121.5(5) . . ? N2 C6 S1 127.9(5) . . ? N1 C6 Yb1 51.7(3) . . ? N2 C6 Yb1 161.9(5) . . ? S1 C6 Yb1 70.0(2) . . ? C8 C7 C12 122.4(7) . . ? C8 C7 N2 131.6(7) . . ? C12 C7 N2 106.0(6) . . ? C7 C8 C9 115.8(8) . . ? C7 C8 H8A 122.1 . . ? C9 C8 H8A 122.1 . . ? C10 C9 C8 122.4(8) . . ? C10 C9 H9A 118.8 . . ? C8 C9 H9A 118.8 . . ? C9 C10 C11 121.8(9) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C12 C11 C10 116.8(8) . . ? C12 C11 H11A 121.6 . . ? C10 C11 H11A 121.6 . . ? C11 C12 C7 120.8(7) . . ? C11 C12 N1 131.1(7) . . ? C7 C12 N1 108.1(6) . . ? N3 C13 N4 110.8(5) . . ? N3 C13 S2 120.4(5) . . ? N4 C13 S2 128.9(5) . . ? N3 C13 Yb1 53.5(3) . . ? N4 C13 Yb1 164.2(4) . . ? S2 C13 Yb1 66.9(2) . . ? N4 C14 C15 131.5(6) . . ? N4 C14 C19 105.3(5) . . ? C15 C14 C19 123.2(6) . . ? C16 C15 C14 116.7(7) . . ? C16 C15 H15A 121.6 . . ? C14 C15 H15A 121.6 . . ? C15 C16 C17 121.5(6) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C18 C17 C16 121.5(7) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 117.4(6) . . ? C17 C18 H18A 121.3 . . ? C19 C18 H18A 121.3 . . ? N3 C19 C14 109.1(5) . . ? N3 C19 C18 131.3(6) . . ? C14 C19 C18 119.6(6) . . ? C20 O1 C23 102.6(10) . . ? C20 O1 Yb1 127.6(7) . . ? C23 O1 Yb1 125.3(9) . . ? O1 C20 C21 111.4(11) . . ? O1 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? O1 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 105.1(12) . . ? C22 C21 H21A 110.7 . . ? C20 C21 H21A 110.7 . . ? C22 C21 H21B 110.7 . . ? C20 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 103.5(12) . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22B 111.1 . . ? C21 C22 H22B 111.1 . . ? H22A C22 H22B 109.0 . . ? O1 C23 C22 111.5(12) . . ? O1 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? O1 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C21' C20' H20C 109.8 . . ? C21' C20' H20D 109.8 . . ? H20C C20' H20D 108.3 . . ? C22' C21' C20' 104.2(14) . . ? C22' C21' H21C 110.9 . . ? C20' C21' H21C 110.9 . . ? C22' C21' H21D 110.9 . . ? C20' C21' H21D 110.9 . . ? H21C C21' H21D 108.9 . . ? C23' C22' C21' 104.2(13) . . ? C23' C22' H22C 110.9 . . ? C21' C22' H22C 110.9 . . ? C23' C22' H22D 110.9 . . ? C21' C22' H22D 110.9 . . ? H22C C22' H22D 108.9 . . ? C22' C23' H23C 109.0 . . ? C22' C23' H23D 109.0 . . ? H23C C23' H23D 107.8 . . ? C24 O2 C27 112.3(16) . . ? O2 C24 C25 107(2) . . ? O2 C24 H24C 110.3 . . ? C25 C24 H24C 110.3 . . ? O2 C24 H24D 110.3 . . ? C25 C24 H24D 110.3 . . ? H24C C24 H24D 108.6 . . ? C24 C25 C26 100(2) . . ? C24 C25 H25C 111.8 . . ? C26 C25 H25C 111.8 . . ? C24 C25 H25D 111.8 . . ? C26 C25 H25D 111.8 . . ? H25C C25 H25D 109.5 . . ? C27 C26 C25 110.8(19) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? O2 C27 C26 101.4(17) . . ? O2 C27 H27A 111.5 . . ? C26 C27 H27A 111.5 . . ? O2 C27 H27B 111.5 . . ? C26 C27 H27B 111.5 . . ? H27A C27 H27B 109.3 . . ? C24' O2' C27' 103.4(19) . . ? O2' C24' C25' 111.1(19) . . ? O2' C24' H24A 109.4 . . ? C25' C24' H24A 109.4 . . ? O2' C24' H24B 109.4 . . ? C25' C24' H24B 109.4 . . ? H24A C24' H24B 108.0 . . ? C24' C25' C26' 109.0(19) . . ? C24' C25' H25A 109.9 . . ? C26' C25' H25A 109.9 . . ? C24' C25' H25B 109.9 . . ? C26' C25' H25B 109.9 . . ? H25A C25' H25B 108.3 . . ? C25' C26' C27' 95(2) . . ? C25' C26' H26C 112.7 . . ? C27' C26' H26C 112.7 . . ? C25' C26' H26D 112.7 . . ? C27' C26' H26D 112.7 . . ? H26C C26' H26D 110.1 . . ? O2' C27' C26' 118(2) . . ? O2' C27' H27C 107.9 . . ? C26' C27' H27C 107.9 . . ? O2' C27' H27D 107.9 . . ? C26' C27' H27D 107.9 . . ? H27C C27' H27D 107.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4N S1 0.85(2) 2.54(3) 3.367(5) 164(7) 1_545 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.015 _refine_diff_density_min -1.812 _refine_diff_density_rms 0.140 # Attachment '3.cif' data_f80114b _database_code_depnum_ccdc_archive 'CCDC 762743' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H47 Er N6 O4 S3' _chemical_formula_weight 903.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.288(5) _cell_length_b 17.476(7) _cell_length_c 17.081(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.642(5) _cell_angle_gamma 90.00 _cell_volume 3962(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6635 _cell_measurement_theta_min 2.229 _cell_measurement_theta_max 25.366 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 2.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6539 _exptl_absorpt_correction_T_max 0.7370 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18911 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6970 _reflns_number_gt 5577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX was used to restrain bond lengths to more standard values. SIMU was used to restrain some abnormal ADPs. ; _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^)+(0.0520P)^2^+5.1503P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6970 _refine_ls_number_parameters 469 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.069782(15) 0.104569(11) 0.801422(11) 0.03690(9) Uani 1 1 d . . . S1 S -0.00880(10) 0.16718(8) 0.95000(7) 0.0513(3) Uani 1 1 d . . . S2 S 0.17344(10) 0.00388(9) 0.90646(8) 0.0561(3) Uani 1 1 d . . . S3 S 0.10840(10) 0.19630(8) 0.66451(7) 0.0523(3) Uani 1 1 d . . . N1 N 0.1438(3) 0.2106(2) 0.8649(2) 0.0432(9) Uani 1 1 d . . . N2 N 0.1357(3) 0.2788(3) 0.9739(2) 0.0513(10) Uani 1 1 d D . . H2 H 0.115(4) 0.292(3) 1.0181(18) 0.062 Uiso 1 1 d D . . N3 N 0.2433(3) 0.0728(2) 0.7812(2) 0.0472(10) Uani 1 1 d . . . N4 N 0.3569(3) -0.0028(3) 0.8393(3) 0.0594(12) Uani 1 1 d D . . H4 H 0.378(4) -0.033(3) 0.875(3) 0.071 Uiso 1 1 d D . . N5 N -0.0588(3) 0.1837(2) 0.7417(2) 0.0482(10) Uani 1 1 d . . . N6 N -0.0769(3) 0.2666(2) 0.6440(2) 0.0502(10) Uani 1 1 d D . . H6 H -0.058(4) 0.287(3) 0.602(2) 0.060 Uiso 1 1 d D . . C1 C 0.0933(4) 0.2215(3) 0.9299(3) 0.0432(11) Uani 1 1 d . . . C2 C 0.2173(4) 0.3069(3) 0.9360(3) 0.0512(12) Uani 1 1 d . . . C3 C 0.2221(4) 0.2640(3) 0.8677(3) 0.0448(11) Uani 1 1 d . . . C4 C 0.2969(4) 0.2775(3) 0.8156(3) 0.0571(13) Uani 1 1 d . . . H4B H 0.3006 0.2493 0.7696 0.068 Uiso 1 1 calc R . . C5 C 0.3659(4) 0.3348(4) 0.8346(4) 0.0680(16) Uani 1 1 d . . . H5A H 0.4175 0.3450 0.8012 0.082 Uiso 1 1 calc R . . C6 C 0.3591(5) 0.3771(4) 0.9025(4) 0.0755(19) Uani 1 1 d . . . H6B H 0.4064 0.4152 0.9137 0.091 Uiso 1 1 calc R . . C7 C 0.2850(5) 0.3645(4) 0.9534(4) 0.0696(16) Uani 1 1 d . . . H7A H 0.2804 0.3939 0.9985 0.083 Uiso 1 1 calc R . . C8 C 0.2615(4) 0.0252(3) 0.8406(3) 0.0468(12) Uani 1 1 d . . . C9 C 0.4034(4) 0.0292(3) 0.7765(3) 0.0555(13) Uani 1 1 d . . . C10 C 0.3313(4) 0.0767(3) 0.7401(3) 0.0491(12) Uani 1 1 d . . . C11 C 0.3549(4) 0.1181(3) 0.6744(3) 0.0596(14) Uani 1 1 d . . . H11A H 0.3071 0.1492 0.6488 0.072 Uiso 1 1 calc R . . C12 C 0.4506(5) 0.1122(4) 0.6480(4) 0.0754(18) Uani 1 1 d . . . H12A H 0.4684 0.1406 0.6047 0.091 Uiso 1 1 calc R . . C13 C 0.5215(5) 0.0639(5) 0.6856(4) 0.085(2) Uani 1 1 d . . . H13A H 0.5856 0.0602 0.6663 0.102 Uiso 1 1 calc R . . C14 C 0.4987(5) 0.0222(4) 0.7501(5) 0.082(2) Uani 1 1 d . . . H14A H 0.5461 -0.0098 0.7750 0.099 Uiso 1 1 calc R . . C15 C -0.0136(4) 0.2175(3) 0.6823(3) 0.0437(11) Uani 1 1 d . . . C16 C -0.1673(4) 0.2661(3) 0.6791(3) 0.0516(13) Uani 1 1 d . . . C17 C -0.1552(4) 0.2155(3) 0.7418(3) 0.0512(12) Uani 1 1 d . . . C18 C -0.2334(4) 0.2020(4) 0.7899(4) 0.0716(17) Uani 1 1 d . . . H18A H -0.2262 0.1686 0.8323 0.086 Uiso 1 1 calc R . . C19 C -0.3228(5) 0.2396(4) 0.7731(5) 0.087(2) Uani 1 1 d . . . H19A H -0.3771 0.2308 0.8043 0.105 Uiso 1 1 calc R . . C20 C -0.3341(5) 0.2899(4) 0.7114(5) 0.086(2) Uani 1 1 d . . . H20A H -0.3957 0.3143 0.7019 0.103 Uiso 1 1 calc R . . C21 C -0.2568(5) 0.3047(3) 0.6640(4) 0.0716(17) Uani 1 1 d . . . H21A H -0.2639 0.3395 0.6229 0.086 Uiso 1 1 calc R . . O1 O 0.0548(3) 0.00732(19) 0.70148(18) 0.0521(9) Uani 1 1 d D . . C22 C 0.0850(5) -0.0707(3) 0.7154(4) 0.0768(19) Uani 1 1 d D . . H22A H 0.0681 -0.0864 0.7676 0.092 Uiso 1 1 calc R . . H22B H 0.1572 -0.0759 0.7109 0.092 Uiso 1 1 calc R . . C23 C 0.0319(7) -0.1172(3) 0.6572(4) 0.088(2) Uani 1 1 d D . . H23A H -0.0251 -0.1425 0.6795 0.106 Uiso 1 1 calc R . . H23B H 0.0762 -0.1559 0.6369 0.106 Uiso 1 1 calc R . . C24 C -0.0026(6) -0.0635(4) 0.5941(4) 0.092(2) Uani 1 1 d D . . H24A H 0.0252 -0.0778 0.5446 0.111 Uiso 1 1 calc R . . H24B H -0.0755 -0.0636 0.5878 0.111 Uiso 1 1 calc R . . C25 C 0.0344(6) 0.0122(4) 0.6195(3) 0.0776(19) Uani 1 1 d D . . H25A H 0.0951 0.0253 0.5931 0.093 Uiso 1 1 calc R . . H25B H -0.0162 0.0510 0.6076 0.093 Uiso 1 1 calc R . . O2 O -0.0724(3) 0.0233(2) 0.82710(19) 0.0531(9) Uani 1 1 d . . . C26 C -0.0872(5) -0.0183(4) 0.8993(4) 0.088(2) Uani 1 1 d . . . H26A H -0.1034 0.0168 0.9409 0.105 Uiso 1 1 calc R . . H26B H -0.0265 -0.0460 0.9154 0.105 Uiso 1 1 calc R . . C27 C -0.1704(6) -0.0715(5) 0.8835(5) 0.100(2) Uani 1 1 d U . . H27A H -0.1455 -0.1222 0.8715 0.120 Uiso 1 1 calc R . . H27B H -0.2129 -0.0750 0.9280 0.120 Uiso 1 1 calc R . . C28 C -0.2247(6) -0.0387(5) 0.8166(5) 0.112(2) Uani 1 1 d U . . H28A H -0.2779 -0.0055 0.8338 0.135 Uiso 1 1 calc R . . H28B H -0.2549 -0.0788 0.7841 0.135 Uiso 1 1 calc R . . C29 C -0.1540(4) 0.0048(4) 0.7725(4) 0.0680(16) Uani 1 1 d U . . H29A H -0.1301 -0.0254 0.7294 0.082 Uiso 1 1 calc R . . H29B H -0.1854 0.0510 0.7514 0.082 Uiso 1 1 calc R . . O3 O 0.5386(4) 0.1023(3) 1.0523(4) 0.115(2) Uani 1 1 d . . . C30 C 0.5606(8) 0.1184(7) 0.9768(7) 0.138(4) Uani 1 1 d . . . H30A H 0.5643 0.0717 0.9465 0.166 Uiso 1 1 calc R . . H30B H 0.6247 0.1448 0.9753 0.166 Uiso 1 1 calc R . . C31 C 0.4792(10) 0.1672(7) 0.9452(7) 0.156(5) Uani 1 1 d . . . H31A H 0.5021 0.2197 0.9408 0.187 Uiso 1 1 calc R . . H31B H 0.4556 0.1494 0.8938 0.187 Uiso 1 1 calc R . . C32 C 0.4006(8) 0.1620(8) 0.9995(7) 0.164(5) Uani 1 1 d . . . H32A H 0.3761 0.2125 1.0125 0.197 Uiso 1 1 calc R . . H32B H 0.3448 0.1319 0.9777 0.197 Uiso 1 1 calc R . . C33 C 0.4432(8) 0.1275(9) 1.0638(8) 0.188(6) Uani 1 1 d . . . H33A H 0.4017 0.0844 1.0779 0.226 Uiso 1 1 calc R . . H33B H 0.4450 0.1633 1.1072 0.226 Uiso 1 1 calc R . . O4 O 0.2428(9) 0.5564(5) -0.0069(9) 0.283(7) Uani 1 1 d D . . C34 C 0.3353(11) 0.5607(7) 0.0390(10) 0.214(8) Uani 1 1 d D . . H34A H 0.3307 0.5306 0.0864 0.257 Uiso 1 1 calc R . . H34B H 0.3901 0.5407 0.0095 0.257 Uiso 1 1 calc R . . C35 C 0.3523(12) 0.6358(8) 0.0574(10) 0.226(8) Uani 1 1 d D . . H35A H 0.4213 0.6497 0.0478 0.271 Uiso 1 1 calc R . . H35B H 0.3404 0.6451 0.1122 0.271 Uiso 1 1 calc R . . C36 C 0.2817(13) 0.6803(6) 0.0069(9) 0.217(8) Uani 1 1 d D . . H36A H 0.2372 0.7103 0.0383 0.260 Uiso 1 1 calc R . . H36B H 0.3181 0.7149 -0.0261 0.260 Uiso 1 1 calc R . . C37 C 0.2254(11) 0.6264(7) -0.0398(8) 0.182(6) Uani 1 1 d D . . H37A H 0.1542 0.6386 -0.0405 0.219 Uiso 1 1 calc R . . H37B H 0.2471 0.6271 -0.0933 0.219 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03943(13) 0.03988(13) 0.03128(12) 0.00240(9) 0.00057(8) 0.00062(9) S1 0.0565(8) 0.0545(8) 0.0434(7) -0.0020(6) 0.0078(6) -0.0057(6) S2 0.0554(8) 0.0681(9) 0.0449(7) 0.0148(6) 0.0023(6) 0.0094(7) S3 0.0497(7) 0.0660(8) 0.0412(7) 0.0156(6) 0.0041(5) 0.0029(6) N1 0.048(2) 0.043(2) 0.038(2) -0.0029(17) 0.0062(17) -0.0042(18) N2 0.065(3) 0.052(3) 0.037(2) -0.0071(19) 0.004(2) -0.005(2) N3 0.048(2) 0.052(2) 0.041(2) 0.0019(19) 0.0004(18) 0.002(2) N4 0.047(3) 0.066(3) 0.064(3) 0.013(2) -0.004(2) 0.008(2) N5 0.048(2) 0.049(2) 0.047(2) 0.0069(19) 0.0006(18) 0.006(2) N6 0.057(3) 0.044(2) 0.048(3) 0.0111(19) -0.008(2) 0.000(2) C1 0.051(3) 0.041(3) 0.037(3) 0.000(2) 0.001(2) 0.005(2) C2 0.055(3) 0.049(3) 0.049(3) 0.000(2) -0.007(2) -0.003(2) C3 0.049(3) 0.044(3) 0.041(3) 0.004(2) -0.006(2) -0.002(2) C4 0.053(3) 0.063(3) 0.056(3) 0.004(3) 0.003(3) -0.005(3) C5 0.051(3) 0.075(4) 0.078(4) 0.017(3) 0.007(3) -0.013(3) C6 0.077(5) 0.063(4) 0.085(5) 0.000(3) -0.011(4) -0.024(3) C7 0.083(4) 0.062(4) 0.063(4) -0.010(3) -0.003(3) -0.017(3) C8 0.044(3) 0.053(3) 0.044(3) 0.000(2) -0.005(2) 0.005(2) C9 0.045(3) 0.060(3) 0.062(3) -0.003(3) 0.002(2) 0.006(3) C10 0.045(3) 0.051(3) 0.051(3) -0.009(2) 0.004(2) 0.002(2) C11 0.052(3) 0.075(4) 0.052(3) 0.008(3) 0.008(3) 0.007(3) C12 0.066(4) 0.080(5) 0.082(5) 0.007(3) 0.025(3) 0.001(3) C13 0.050(4) 0.106(6) 0.099(5) -0.001(4) 0.024(4) 0.003(4) C14 0.052(4) 0.096(5) 0.101(5) 0.017(4) 0.010(3) 0.019(4) C15 0.048(3) 0.042(3) 0.040(3) 0.001(2) -0.004(2) 0.002(2) C16 0.049(3) 0.047(3) 0.058(3) 0.000(2) -0.005(2) 0.004(2) C17 0.049(3) 0.050(3) 0.054(3) -0.005(2) 0.002(2) 0.004(2) C18 0.061(4) 0.082(4) 0.073(4) 0.010(3) 0.013(3) 0.009(3) C19 0.058(4) 0.097(5) 0.109(6) 0.002(5) 0.026(4) 0.006(4) C20 0.057(4) 0.087(5) 0.113(6) 0.006(4) 0.005(4) 0.022(4) C21 0.065(4) 0.059(4) 0.090(5) 0.001(3) -0.013(3) 0.013(3) O1 0.067(2) 0.049(2) 0.0400(19) -0.0018(15) -0.0032(16) 0.0011(17) C22 0.102(5) 0.056(4) 0.070(4) -0.012(3) -0.015(4) 0.020(4) C23 0.133(7) 0.058(4) 0.073(5) -0.012(3) -0.012(4) 0.002(4) C24 0.128(6) 0.079(5) 0.066(4) -0.012(4) -0.025(4) -0.009(5) C25 0.114(5) 0.080(4) 0.038(3) -0.003(3) -0.009(3) -0.011(4) O2 0.054(2) 0.063(2) 0.0423(19) 0.0030(16) -0.0012(16) -0.0177(18) C26 0.092(5) 0.115(6) 0.056(4) 0.028(4) -0.005(3) -0.053(4) C27 0.088(4) 0.114(5) 0.096(5) 0.031(4) -0.012(4) -0.048(4) C28 0.091(5) 0.133(5) 0.111(5) 0.031(4) -0.017(4) -0.048(4) C29 0.054(3) 0.082(4) 0.067(4) 0.002(3) -0.011(3) -0.011(3) O3 0.087(4) 0.149(5) 0.107(4) 0.058(4) -0.008(3) 0.036(3) C30 0.117(8) 0.179(11) 0.118(9) 0.032(7) 0.000(7) 0.011(7) C31 0.172(11) 0.156(10) 0.135(9) 0.065(8) -0.039(9) -0.037(9) C32 0.113(8) 0.201(13) 0.175(12) 0.080(10) -0.028(8) 0.021(8) C33 0.104(8) 0.293(17) 0.166(11) 0.098(11) 0.003(7) 0.087(9) O4 0.240(12) 0.128(8) 0.47(2) -0.021(11) -0.120(13) -0.030(8) C34 0.191(14) 0.122(11) 0.32(2) 0.007(12) -0.116(14) 0.034(10) C35 0.257(18) 0.145(12) 0.262(19) -0.030(13) -0.140(15) 0.002(12) C36 0.287(19) 0.121(10) 0.231(16) 0.026(11) -0.109(14) -0.018(12) C37 0.252(17) 0.119(9) 0.167(12) 0.044(9) -0.082(12) -0.020(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.341(4) . ? Er1 N5 2.390(4) . ? Er1 O1 2.410(3) . ? Er1 N3 2.412(4) . ? Er1 O2 2.420(3) . ? Er1 S2 2.8258(15) . ? Er1 S3 2.9006(15) . ? Er1 C8 2.950(5) . ? Er1 S1 2.9954(15) . ? S1 C1 1.703(5) . ? S2 C8 1.702(5) . ? S3 C15 1.704(5) . ? N1 C1 1.336(6) . ? N1 C3 1.398(6) . ? N2 C1 1.359(6) . ? N2 C2 1.379(7) . ? N2 H2 0.84(2) . ? N3 C8 1.326(6) . ? N3 C10 1.393(6) . ? N4 C8 1.360(6) . ? N4 C9 1.380(7) . ? N4 H4 0.84(2) . ? N5 C15 1.339(6) . ? N5 C17 1.396(6) . ? N6 C15 1.350(6) . ? N6 C16 1.368(7) . ? N6 H6 0.85(2) . ? C2 C7 1.374(8) . ? C2 C3 1.391(7) . ? C3 C4 1.385(7) . ? C4 C5 1.387(8) . ? C4 H4B 0.9300 . ? C5 C6 1.381(9) . ? C5 H5A 0.9300 . ? C6 C7 1.361(9) . ? C6 H6B 0.9300 . ? C7 H7A 0.9300 . ? C9 C14 1.371(8) . ? C9 C10 1.391(7) . ? C10 C11 1.384(8) . ? C11 C12 1.372(8) . ? C11 H11A 0.9300 . ? C12 C13 1.398(9) . ? C12 H12A 0.9300 . ? C13 C14 1.366(10) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C16 C21 1.380(7) . ? C16 C17 1.393(7) . ? C17 C18 1.376(8) . ? C18 C19 1.377(9) . ? C18 H18A 0.9300 . ? C19 C20 1.375(10) . ? C19 H19A 0.9300 . ? C20 C21 1.362(9) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? O1 C25 1.416(6) . ? O1 C22 1.437(6) . ? C22 C23 1.444(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.485(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.470(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? O2 C29 1.434(6) . ? O2 C26 1.454(6) . ? C26 C27 1.460(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.442(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.447(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? O3 C33 1.365(11) . ? O3 C30 1.365(11) . ? C30 C31 1.461(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.431(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.353(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? O4 C37 1.362(9) . ? O4 C34 1.429(9) . ? C34 C35 1.366(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.469(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.425(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 N1 Er1 N5 90.93(14) . . ? N1 Er1 O1 154.90(13) . . ? N5 Er1 O1 94.12(13) . . ? N1 Er1 N3 82.23(14) . . ? N5 Er1 N3 137.83(14) . . ? O1 Er1 N3 77.55(13) . . ? N1 Er1 O2 134.04(12) . . ? N5 Er1 O2 82.42(13) . . ? O1 Er1 O2 71.04(12) . . ? N3 Er1 O2 130.59(13) . . ? N1 Er1 S2 90.95(10) . . ? N5 Er1 S2 161.69(10) . . ? O1 Er1 S2 91.86(9) . . ? N3 Er1 S2 60.43(10) . . ? O2 Er1 S2 83.19(9) . . ? N1 Er1 S3 81.38(10) . . ? N5 Er1 S3 59.03(10) . . ? O1 Er1 S3 80.25(9) . . ? N3 Er1 S3 78.80(10) . . ? O2 Er1 S3 129.72(8) . . ? S2 Er1 S3 139.20(4) . . ? N1 Er1 C8 85.83(14) . . ? N5 Er1 C8 164.08(14) . . ? O1 Er1 C8 82.60(13) . . ? N3 Er1 C8 26.25(13) . . ? O2 Er1 C8 110.88(13) . . ? S2 Er1 C8 34.18(10) . . ? S3 Er1 C8 105.05(10) . . ? N1 Er1 S1 58.23(10) . . ? N5 Er1 S1 83.11(10) . . ? O1 Er1 S1 146.82(9) . . ? N3 Er1 S1 125.34(10) . . ? O2 Er1 S1 75.82(9) . . ? S2 Er1 S1 82.43(5) . . ? S3 Er1 S1 124.25(5) . . ? C8 Er1 S1 108.10(10) . . ? C1 S1 Er1 73.78(16) . . ? C8 S2 Er1 76.91(17) . . ? C15 S3 Er1 76.77(16) . . ? C1 N1 C3 106.2(4) . . ? C1 N1 Er1 106.3(3) . . ? C3 N1 Er1 147.2(3) . . ? C1 N2 C2 108.6(4) . . ? C1 N2 H2 123(4) . . ? C2 N2 H2 128(4) . . ? C8 N3 C10 106.8(4) . . ? C8 N3 Er1 100.2(3) . . ? C10 N3 Er1 153.1(3) . . ? C8 N4 C9 108.5(4) . . ? C8 N4 H4 119(4) . . ? C9 N4 H4 132(4) . . ? C15 N5 C17 105.6(4) . . ? C15 N5 Er1 104.0(3) . . ? C17 N5 Er1 150.2(3) . . ? C15 N6 C16 108.9(4) . . ? C15 N6 H6 118(4) . . ? C16 N6 H6 133(4) . . ? N1 C1 N2 110.7(4) . . ? N1 C1 S1 121.5(4) . . ? N2 C1 S1 127.8(4) . . ? C7 C2 N2 133.0(5) . . ? C7 C2 C3 121.4(5) . . ? N2 C2 C3 105.6(4) . . ? C4 C3 C2 120.7(5) . . ? C4 C3 N1 130.3(5) . . ? C2 C3 N1 109.0(4) . . ? C3 C4 C5 117.3(5) . . ? C3 C4 H4B 121.4 . . ? C5 C4 H4B 121.4 . . ? C6 C5 C4 121.0(6) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C7 C6 C5 121.8(6) . . ? C7 C6 H6B 119.1 . . ? C5 C6 H6B 119.1 . . ? C6 C7 C2 117.8(6) . . ? C6 C7 H7A 121.1 . . ? C2 C7 H7A 121.1 . . ? N3 C8 N4 110.5(5) . . ? N3 C8 S2 122.5(4) . . ? N4 C8 S2 127.0(4) . . ? N3 C8 Er1 53.6(2) . . ? N4 C8 Er1 164.0(4) . . ? S2 C8 Er1 68.91(16) . . ? C14 C9 N4 132.3(6) . . ? C14 C9 C10 122.3(6) . . ? N4 C9 C10 105.4(4) . . ? C11 C10 C9 119.8(5) . . ? C11 C10 N3 131.4(5) . . ? C9 C10 N3 108.8(5) . . ? C12 C11 C10 118.4(6) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 121.6(6) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C9 117.4(6) . . ? C13 C14 H14A 121.3 . . ? C9 C14 H14A 121.3 . . ? N5 C15 N6 110.9(4) . . ? N5 C15 S3 120.2(4) . . ? N6 C15 S3 128.9(4) . . ? N6 C16 C21 132.9(5) . . ? N6 C16 C17 105.6(4) . . ? C21 C16 C17 121.5(6) . . ? C18 C17 C16 120.3(5) . . ? C18 C17 N5 130.6(5) . . ? C16 C17 N5 109.0(5) . . ? C17 C18 C19 117.5(6) . . ? C17 C18 H18A 121.3 . . ? C19 C18 H18A 121.3 . . ? C20 C19 C18 121.9(6) . . ? C20 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? C21 C20 C19 121.2(6) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C16 117.5(6) . . ? C20 C21 H21A 121.2 . . ? C16 C21 H21A 121.2 . . ? C25 O1 C22 105.0(4) . . ? C25 O1 Er1 131.6(3) . . ? C22 O1 Er1 122.6(3) . . ? O1 C22 C23 107.3(5) . . ? O1 C22 H22A 110.3 . . ? C23 C22 H22A 110.3 . . ? O1 C22 H22B 110.3 . . ? C23 C22 H22B 110.3 . . ? H22A C22 H22B 108.5 . . ? C22 C23 C24 105.6(5) . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? C22 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.8 . . ? C25 C24 C23 105.4(5) . . ? C25 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? C25 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? O1 C25 C24 106.5(5) . . ? O1 C25 H25A 110.4 . . ? C24 C25 H25A 110.4 . . ? O1 C25 H25B 110.4 . . ? C24 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C29 O2 C26 108.1(4) . . ? C29 O2 Er1 126.0(3) . . ? C26 O2 Er1 125.8(3) . . ? O2 C26 C27 107.0(5) . . ? O2 C26 H26A 110.3 . . ? C27 C26 H26A 110.3 . . ? O2 C26 H26B 110.3 . . ? C27 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? C28 C27 C26 103.8(6) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? C27 C28 C29 108.0(6) . . ? C27 C28 H28A 110.1 . . ? C29 C28 H28A 110.1 . . ? C27 C28 H28B 110.1 . . ? C29 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? O2 C29 C28 105.6(5) . . ? O2 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O2 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? C33 O3 C30 108.1(7) . . ? O3 C30 C31 106.4(9) . . ? O3 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O3 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.6 . . ? C32 C31 C30 105.9(9) . . ? C32 C31 H31A 110.6 . . ? C30 C31 H31A 110.6 . . ? C32 C31 H31B 110.6 . . ? C30 C31 H31B 110.6 . . ? H31A C31 H31B 108.7 . . ? C33 C32 C31 105.3(10) . . ? C33 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? C33 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C32 C33 O3 112.5(11) . . ? C32 C33 H33A 109.1 . . ? O3 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? O3 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C37 O4 C34 107.7(8) . . ? C35 C34 O4 107.8(8) . . ? C35 C34 H34A 110.2 . . ? O4 C34 H34A 110.2 . . ? C35 C34 H34B 110.2 . . ? O4 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C34 C35 C36 106.2(8) . . ? C34 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? C34 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C37 C36 C35 106.5(8) . . ? C37 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? C37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? O4 C37 C36 106.7(8) . . ? O4 C37 H37A 110.4 . . ? C36 C37 H37A 110.4 . . ? O4 C37 H37B 110.4 . . ? C36 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6 S1 0.85(2) 2.82(2) 3.662(5) 170(5) 4_565 N4 H4 O3 0.84(2) 2.03(3) 2.854(6) 166(6) 3_657 N2 H2 S3 0.84(2) 2.52(3) 3.321(4) 160(5) 4_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.415 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.085 # Attachment '4.cif' data_f80122b _database_code_depnum_ccdc_archive 'CCDC 762744' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H47 N6 O4 S3 Y' _chemical_formula_weight 824.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.31(4) _cell_length_b 17.55(5) _cell_length_c 17.04(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.43(4) _cell_angle_gamma 90.00 _cell_volume 3978(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 929 _cell_measurement_theta_min 2.611 _cell_measurement_theta_max 20.792 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6344 _exptl_absorpt_correction_T_max 0.8248 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17499 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7769 _reflns_number_gt 4669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU was used to restrain some abnormal ADPs. ; _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^)+(0.0693P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7769 _refine_ls_number_parameters 479 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.06946(3) 0.10408(2) 0.80174(2) 0.03886(14) Uani 1 1 d . . . S1 S -0.00876(9) 0.16761(7) 0.95053(7) 0.0528(3) Uani 1 1 d . . . S2 S 0.17444(9) 0.00296(7) 0.90682(7) 0.0588(3) Uani 1 1 d . . . S3 S 0.10744(8) 0.19611(7) 0.66426(7) 0.0544(3) Uani 1 1 d . . . N1 N 0.1441(2) 0.21085(19) 0.86506(19) 0.0435(8) Uani 1 1 d . . . N2 N 0.1357(3) 0.2779(2) 0.9743(2) 0.0512(9) Uani 1 1 d D . . H2 H 0.115(3) 0.288(3) 1.0200(16) 0.062(15) Uiso 1 1 d D . . N3 N 0.2433(3) 0.0722(2) 0.7812(2) 0.0470(9) Uani 1 1 d . . . N4 N 0.3574(3) -0.0032(2) 0.8394(3) 0.0602(11) Uani 1 1 d D . . H4 H 0.387(3) -0.035(2) 0.871(2) 0.062(15) Uiso 1 1 d D . . N5 N -0.0595(2) 0.1838(2) 0.7415(2) 0.0461(9) Uani 1 1 d . . . N6 N -0.0762(3) 0.2663(2) 0.6434(2) 0.0509(9) Uani 1 1 d D . . H6 H -0.058(3) 0.291(2) 0.6040(18) 0.051(13) Uiso 1 1 d D . . O1 O 0.0546(2) 0.00686(16) 0.70152(16) 0.0545(8) Uani 1 1 d . . . O2 O -0.0726(2) 0.02299(17) 0.82760(17) 0.0551(8) Uani 1 1 d . . . C1 C 0.0938(3) 0.2212(2) 0.9301(2) 0.0431(10) Uani 1 1 d . . . C2 C 0.2172(3) 0.3065(3) 0.9359(3) 0.0511(11) Uani 1 1 d . . . C3 C 0.2218(3) 0.2636(2) 0.8675(2) 0.0464(11) Uani 1 1 d . . . C4 C 0.2966(3) 0.2775(3) 0.8154(3) 0.0592(13) Uani 1 1 d . . . H4B H 0.3010 0.2494 0.7694 0.071 Uiso 1 1 calc R . . C5 C 0.3649(4) 0.3351(3) 0.8345(3) 0.0709(15) Uani 1 1 d . . . H5A H 0.4163 0.3453 0.8008 0.085 Uiso 1 1 calc R . . C6 C 0.3585(4) 0.3774(3) 0.9021(4) 0.0795(17) Uani 1 1 d . . . H6B H 0.4055 0.4156 0.9128 0.095 Uiso 1 1 calc R . . C7 C 0.2847(4) 0.3646(3) 0.9538(3) 0.0715(15) Uani 1 1 d . . . H7A H 0.2800 0.3937 0.9991 0.086 Uiso 1 1 calc R . . C8 C 0.2628(3) 0.0246(2) 0.8398(3) 0.0507(11) Uani 1 1 d . . . C9 C 0.4035(3) 0.0291(3) 0.7765(3) 0.0580(12) Uani 1 1 d . . . C10 C 0.3312(3) 0.0765(3) 0.7401(3) 0.0477(11) Uani 1 1 d . . . C11 C 0.3554(4) 0.1179(3) 0.6750(3) 0.0634(14) Uani 1 1 d . . . H11A H 0.3080 0.1494 0.6499 0.076 Uiso 1 1 calc R . . C12 C 0.4507(4) 0.1120(3) 0.6478(3) 0.0797(17) Uani 1 1 d . . . H12A H 0.4684 0.1400 0.6041 0.096 Uiso 1 1 calc R . . C13 C 0.5207(4) 0.0645(4) 0.6851(4) 0.0914(19) Uani 1 1 d . . . H13A H 0.5849 0.0614 0.6659 0.110 Uiso 1 1 calc R . . C14 C 0.4983(4) 0.0221(4) 0.7492(4) 0.0826(17) Uani 1 1 d . . . H14A H 0.5456 -0.0102 0.7733 0.099 Uiso 1 1 calc R . . C15 C -0.0141(3) 0.2160(2) 0.6825(2) 0.0452(10) Uani 1 1 d . . . C16 C -0.1674(3) 0.2655(2) 0.6789(3) 0.0518(11) Uani 1 1 d . . . C17 C -0.1568(3) 0.2142(3) 0.7409(3) 0.0533(12) Uani 1 1 d . . . C18 C -0.2347(4) 0.2015(3) 0.7895(3) 0.0733(15) Uani 1 1 d . . . H18A H -0.2275 0.1687 0.8323 0.088 Uiso 1 1 calc R . . C19 C -0.3238(4) 0.2390(4) 0.7726(4) 0.0886(18) Uani 1 1 d . . . H19A H -0.3784 0.2299 0.8036 0.106 Uiso 1 1 calc R . . C20 C -0.3342(4) 0.2899(4) 0.7108(4) 0.0899(19) Uani 1 1 d . . . H20A H -0.3954 0.3145 0.7014 0.108 Uiso 1 1 calc R . . C21 C -0.2573(4) 0.3046(3) 0.6638(3) 0.0735(15) Uani 1 1 d . . . H21A H -0.2641 0.3395 0.6229 0.088 Uiso 1 1 calc R . . C22 C 0.0862(4) -0.0706(3) 0.7166(3) 0.0816(17) Uani 1 1 d . . . H22A H 0.0706 -0.0857 0.7694 0.098 Uiso 1 1 calc R . . H22B H 0.1580 -0.0757 0.7108 0.098 Uiso 1 1 calc R . . C23 C 0.0293(5) -0.1189(3) 0.6571(4) 0.0897(19) Uani 1 1 d . . . H23A H -0.0281 -0.1428 0.6802 0.108 Uiso 1 1 calc R . . H23B H 0.0723 -0.1582 0.6368 0.108 Uiso 1 1 calc R . . C24 C -0.0045(5) -0.0640(3) 0.5925(3) 0.0945(19) Uani 1 1 d . . . H24A H 0.0237 -0.0783 0.5430 0.113 Uiso 1 1 calc R . . H24B H -0.0772 -0.0636 0.5859 0.113 Uiso 1 1 calc R . . C25 C 0.0340(5) 0.0131(3) 0.6190(3) 0.0841(18) Uani 1 1 d . . . H25A H 0.0946 0.0261 0.5923 0.101 Uiso 1 1 calc R . . H25B H -0.0162 0.0520 0.6078 0.101 Uiso 1 1 calc R . . C26 C -0.0867(5) -0.0192(4) 0.8998(3) 0.094(2) Uani 1 1 d . . . H26A H -0.1027 0.0154 0.9419 0.112 Uiso 1 1 calc R . . H26B H -0.0258 -0.0467 0.9152 0.112 Uiso 1 1 calc R . . C27 C -0.1695(5) -0.0725(4) 0.8845(4) 0.0946(19) Uani 1 1 d . . . H27A H -0.1444 -0.1228 0.8724 0.114 Uiso 1 1 calc R . . H27B H -0.2116 -0.0760 0.9294 0.114 Uiso 1 1 calc R . . C28 C -0.2245(5) -0.0402(4) 0.8175(4) 0.122(2) Uani 1 1 d U . . H28A H -0.2537 -0.0804 0.7849 0.147 Uiso 1 1 calc R . . H28B H -0.2784 -0.0080 0.8350 0.147 Uiso 1 1 calc R . . C29 C -0.1556(4) 0.0040(3) 0.7733(3) 0.0719(14) Uani 1 1 d U . . H29A H -0.1880 0.0500 0.7531 0.086 Uiso 1 1 calc R . . H29B H -0.1321 -0.0253 0.7294 0.086 Uiso 1 1 calc R . . O3 O 0.5385(3) 0.1023(3) 1.0533(3) 0.1171(16) Uani 1 1 d D . . C30 C 0.5632(6) 0.1186(5) 0.9757(5) 0.141(3) Uani 1 1 d D . . H30A H 0.5660 0.0722 0.9450 0.169 Uiso 1 1 calc R . . H30B H 0.6279 0.1439 0.9747 0.169 Uiso 1 1 calc R . . C31 C 0.4817(7) 0.1696(6) 0.9439(6) 0.169(4) Uani 1 1 d D . . H31A H 0.5056 0.2217 0.9410 0.203 Uiso 1 1 calc R . . H31B H 0.4592 0.1534 0.8916 0.203 Uiso 1 1 calc R . . C32 C 0.3996(6) 0.1644(6) 0.9975(6) 0.168(4) Uani 1 1 d D . . H32A H 0.3751 0.2147 1.0105 0.202 Uiso 1 1 calc R . . H32B H 0.3444 0.1348 0.9744 0.202 Uiso 1 1 calc R . . C33 C 0.4423(5) 0.1272(6) 1.0661(5) 0.184(5) Uani 1 1 d D . . H33A H 0.4440 0.1624 1.1101 0.221 Uiso 1 1 calc R . . H33B H 0.4006 0.0842 1.0794 0.221 Uiso 1 1 calc R . . O4 O 0.2421(7) 0.5556(4) -0.0062(8) 0.275(5) Uani 1 1 d D A . C34 C 0.3322(10) 0.5584(6) 0.0397(9) 0.233(6) Uani 1 1 d D . . H34A H 0.3897 0.5505 0.0076 0.280 Uiso 0.535(15) 1 calc PR A 1 H34B H 0.3327 0.5200 0.0807 0.280 Uiso 0.535(15) 1 calc PR A 1 H34C H 0.3734 0.5137 0.0309 0.280 Uiso 0.465(15) 1 d PR A 2 H34D H 0.3149 0.5582 0.0943 0.280 Uiso 0.465(15) 1 d PR A 2 C35 C 0.3338(14) 0.6350(10) 0.0735(12) 0.140(5) Uani 0.535(15) 1 d PD A 1 H35A H 0.4000 0.6576 0.0702 0.168 Uiso 0.535(15) 1 calc PR A 1 H35B H 0.3166 0.6334 0.1283 0.168 Uiso 0.535(15) 1 calc PR A 1 C36 C 0.2571(18) 0.6803(9) 0.0261(10) 0.154(7) Uani 0.535(15) 1 d PD A 1 H36A H 0.2012 0.6947 0.0577 0.184 Uiso 0.535(15) 1 calc PR A 1 H36B H 0.2868 0.7259 0.0048 0.184 Uiso 0.535(15) 1 calc PR A 1 C35' C 0.3754(14) 0.6341(9) 0.0366(14) 0.140(5) Uani 0.465(15) 1 d PD A 2 H35C H 0.4406 0.6324 0.0134 0.168 Uiso 0.465(15) 1 calc PR A 2 H35D H 0.3834 0.6555 0.0890 0.168 Uiso 0.465(15) 1 calc PR A 2 C36' C 0.3040(17) 0.6800(10) -0.0124(16) 0.154(7) Uani 0.465(15) 1 d PD A 2 H36C H 0.2767 0.7214 0.0178 0.184 Uiso 0.465(15) 1 calc PR A 2 H36D H 0.3368 0.7012 -0.0572 0.184 Uiso 0.465(15) 1 calc PR A 2 C37 C 0.2237(9) 0.6264(6) -0.0384(6) 0.196(5) Uani 1 1 d D . . H37A H 0.1529 0.6329 -0.0523 0.235 Uiso 0.535(15) 1 calc PR A 1 H37B H 0.2622 0.6340 -0.0848 0.235 Uiso 0.535(15) 1 calc PR A 1 H37C H 0.1614 0.6475 -0.0202 0.235 Uiso 0.465(15) 1 d PR A 2 H37D H 0.2179 0.6225 -0.0950 0.235 Uiso 0.465(15) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0411(2) 0.0438(2) 0.0314(2) 0.00257(19) -0.00168(16) 0.00077(19) S1 0.0574(7) 0.0585(7) 0.0428(7) -0.0021(5) 0.0062(5) -0.0058(6) S2 0.0577(8) 0.0734(8) 0.0451(7) 0.0147(6) 0.0009(6) 0.0100(6) S3 0.0517(7) 0.0711(8) 0.0406(7) 0.0160(6) 0.0031(5) 0.0036(6) N1 0.050(2) 0.045(2) 0.036(2) -0.0030(16) 0.0038(16) -0.0025(17) N2 0.065(3) 0.053(2) 0.035(2) -0.0097(19) 0.004(2) -0.0074(19) N3 0.049(2) 0.055(2) 0.038(2) 0.0034(18) -0.0009(17) 0.0067(18) N4 0.044(2) 0.068(3) 0.068(3) 0.011(2) -0.007(2) 0.013(2) N5 0.045(2) 0.052(2) 0.042(2) 0.0074(17) 0.0042(16) 0.0053(17) N6 0.054(2) 0.052(2) 0.047(3) 0.0141(19) -0.005(2) 0.0001(19) O1 0.073(2) 0.0515(19) 0.0382(18) -0.0033(14) -0.0038(15) 0.0026(16) O2 0.0590(19) 0.062(2) 0.0435(18) 0.0067(15) -0.0028(15) -0.0176(15) C1 0.051(3) 0.042(2) 0.035(2) 0.0026(19) -0.003(2) 0.006(2) C2 0.059(3) 0.050(3) 0.044(3) 0.002(2) -0.010(2) 0.000(2) C3 0.050(3) 0.047(3) 0.042(3) 0.005(2) -0.005(2) -0.001(2) C4 0.060(3) 0.066(3) 0.052(3) 0.002(2) 0.008(2) -0.009(3) C5 0.061(3) 0.080(4) 0.072(4) 0.015(3) 0.003(3) -0.017(3) C6 0.079(4) 0.078(4) 0.081(4) 0.005(3) -0.010(3) -0.029(3) C7 0.083(4) 0.073(3) 0.058(3) -0.009(3) -0.012(3) -0.019(3) C8 0.047(3) 0.052(3) 0.053(3) -0.001(2) -0.006(2) 0.004(2) C9 0.045(3) 0.064(3) 0.065(3) 0.000(3) 0.001(2) 0.002(2) C10 0.039(2) 0.053(3) 0.051(3) -0.005(2) 0.003(2) 0.002(2) C11 0.055(3) 0.081(4) 0.055(3) 0.002(3) 0.013(2) 0.008(3) C12 0.071(4) 0.091(4) 0.078(4) 0.012(3) 0.025(3) 0.011(3) C13 0.054(4) 0.113(5) 0.110(5) -0.002(4) 0.030(4) -0.001(3) C14 0.049(3) 0.099(5) 0.099(5) 0.008(4) 0.006(3) 0.013(3) C15 0.056(3) 0.042(2) 0.037(3) 0.0014(19) -0.010(2) 0.003(2) C16 0.053(3) 0.044(3) 0.057(3) -0.002(2) -0.009(2) 0.004(2) C17 0.052(3) 0.050(3) 0.058(3) -0.002(2) 0.000(2) 0.004(2) C18 0.064(3) 0.083(4) 0.074(4) 0.012(3) 0.018(3) 0.009(3) C19 0.060(4) 0.107(5) 0.101(5) 0.004(4) 0.020(3) 0.015(3) C20 0.056(4) 0.097(5) 0.116(6) 0.003(4) -0.001(4) 0.022(3) C21 0.068(4) 0.066(3) 0.086(4) 0.007(3) -0.012(3) 0.014(3) C22 0.108(5) 0.061(3) 0.073(4) -0.009(3) -0.030(3) 0.020(3) C23 0.119(5) 0.068(4) 0.080(4) -0.019(3) -0.014(4) 0.000(3) C24 0.133(6) 0.080(4) 0.067(4) -0.015(3) -0.029(4) -0.011(4) C25 0.135(5) 0.074(4) 0.042(3) -0.010(3) -0.008(3) -0.012(4) C26 0.093(4) 0.119(5) 0.068(4) 0.030(4) -0.003(3) -0.055(4) C27 0.100(5) 0.093(4) 0.090(5) 0.021(4) -0.012(4) -0.039(4) C28 0.083(4) 0.155(6) 0.125(5) 0.030(5) -0.026(4) -0.060(4) C29 0.058(3) 0.089(4) 0.066(3) 0.009(3) -0.016(3) -0.015(3) O3 0.094(3) 0.146(4) 0.110(4) 0.056(3) -0.013(3) 0.027(3) C30 0.131(7) 0.163(8) 0.129(8) 0.027(6) -0.001(6) 0.004(6) C31 0.160(9) 0.177(9) 0.167(10) 0.083(8) -0.045(8) -0.029(8) C32 0.116(7) 0.179(9) 0.206(11) 0.076(8) -0.049(7) 0.023(7) C33 0.096(6) 0.296(13) 0.162(9) 0.088(8) 0.012(6) 0.086(7) O4 0.242(10) 0.141(7) 0.431(16) -0.013(9) -0.121(10) -0.026(7) C34 0.234(14) 0.139(10) 0.315(17) -0.002(11) -0.138(13) 0.029(9) C35 0.106(13) 0.184(11) 0.129(16) -0.063(11) 0.001(9) 0.006(10) C36 0.166(18) 0.149(10) 0.144(17) 0.034(12) -0.015(12) -0.047(12) C35' 0.106(13) 0.184(11) 0.129(16) -0.063(11) 0.001(9) 0.006(10) C36' 0.166(18) 0.149(10) 0.144(17) 0.034(12) -0.015(12) -0.047(12) C37 0.279(15) 0.126(8) 0.174(10) 0.046(8) -0.097(9) 0.000(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 Y1 N1 2.361(6) . ? Y1 N5 2.410(5) . ? Y1 O1 2.416(6) . ? Y1 N3 2.421(7) . ? Y1 O2 2.423(6) . ? Y1 S2 2.846(5) . ? Y1 S3 2.907(6) . ? Y1 C8 2.975(8) . ? Y1 S1 2.996(6) . ? Y1 C15 3.006(7) . ? Y1 C1 3.008(7) . ? S1 C1 1.706(5) . ? S2 C8 1.716(6) . ? S3 C15 1.697(6) . ? N1 C1 1.331(6) . ? N1 C3 1.389(6) . ? N2 C1 1.355(6) . ? N2 C2 1.384(6) . ? N2 H2 0.854(19) . ? N3 C8 1.319(6) . ? N3 C10 1.392(6) . ? N4 C8 1.352(6) . ? N4 C9 1.379(6) . ? N4 H4 0.867(19) . ? N5 C15 1.322(6) . ? N5 C17 1.401(6) . ? N6 C15 1.364(6) . ? N6 C16 1.379(6) . ? N6 H6 0.846(19) . ? O1 C25 1.425(7) . ? O1 C22 1.442(7) . ? O2 C29 1.450(6) . ? O2 C26 1.455(6) . ? C2 C7 1.385(7) . ? C2 C3 1.390(7) . ? C3 C4 1.383(6) . ? C4 C5 1.389(7) . ? C4 H4B 0.9300 . ? C5 C6 1.375(8) . ? C5 H5A 0.9300 . ? C6 C7 1.365(8) . ? C6 H6B 0.9300 . ? C7 H7A 0.9300 . ? C9 C14 1.369(8) . ? C9 C10 1.398(7) . ? C10 C11 1.375(7) . ? C11 C12 1.374(7) . ? C11 H11A 0.9300 . ? C12 C13 1.384(8) . ? C12 H12A 0.9300 . ? C13 C14 1.364(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C16 C17 1.390(7) . ? C16 C21 1.395(7) . ? C17 C18 1.373(7) . ? C18 C19 1.377(8) . ? C18 H18A 0.9300 . ? C19 C20 1.384(8) . ? C19 H19A 0.9300 . ? C20 C21 1.350(8) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.501(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.516(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.509(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.460(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.446(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.438(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? O3 C33 1.380(7) . ? O3 C30 1.405(8) . ? C30 C31 1.492(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.456(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.435(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? O4 C37 1.375(8) . ? O4 C34 1.405(8) . ? C34 C35' 1.448(10) . ? C34 C35 1.462(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9730 . ? C34 H34D 0.9670 . ? C35 C36 1.503(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.502(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C35' C36' 1.479(10) . ? C35' H35C 0.9700 . ? C35' H35D 0.9700 . ? C36' C37 1.477(10) . ? C36' H36C 0.9700 . ? C36' H36D 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9707 . ? C37 H37D 0.9679 . ? 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 N1 Y1 N5 90.7(2) . . ? N1 Y1 O1 154.67(12) . . ? N5 Y1 O1 94.2(2) . . ? N1 Y1 N3 82.11(18) . . ? N5 Y1 N3 137.79(15) . . ? O1 Y1 N3 77.58(13) . . ? N1 Y1 O2 134.43(15) . . ? N5 Y1 O2 82.6(2) . . ? O1 Y1 O2 70.89(16) . . ? N3 Y1 O2 130.49(19) . . ? N1 Y1 S2 91.2(2) . . ? N5 Y1 S2 162.20(9) . . ? O1 Y1 S2 91.6(2) . . ? N3 Y1 S2 59.97(13) . . ? O2 Y1 S2 83.43(19) . . ? N1 Y1 S3 81.0(2) . . ? N5 Y1 S3 58.62(15) . . ? O1 Y1 S3 80.5(2) . . ? N3 Y1 S3 79.17(11) . . ? O2 Y1 S3 129.55(10) . . ? S2 Y1 S3 139.10(12) . . ? N1 Y1 C8 85.9(2) . . ? N5 Y1 C8 163.55(12) . . ? O1 Y1 C8 82.34(16) . . ? N3 Y1 C8 25.76(13) . . ? O2 Y1 C8 111.1(2) . . ? S2 Y1 C8 34.21(10) . . ? S3 Y1 C8 104.93(15) . . ? N1 Y1 S1 58.16(14) . . ? N5 Y1 S1 82.98(18) . . ? O1 Y1 S1 147.12(10) . . ? N3 Y1 S1 125.22(10) . . ? O2 Y1 S1 76.28(14) . . ? S2 Y1 S1 83.05(19) . . ? S3 Y1 S1 123.60(18) . . ? C8 Y1 S1 108.59(15) . . ? N1 Y1 C15 85.8(2) . . ? N5 Y1 C15 25.32(11) . . ? O1 Y1 C15 88.1(2) . . ? N3 Y1 C15 112.47(15) . . ? O2 Y1 C15 103.72(19) . . ? S2 Y1 C15 172.26(9) . . ? S3 Y1 C15 33.30(13) . . ? C8 Y1 C15 138.23(13) . . ? S1 Y1 C15 101.4(2) . . ? N1 Y1 C1 25.19(11) . . ? N5 Y1 C1 88.1(2) . . ? O1 Y1 C1 177.72(10) . . ? N3 Y1 C1 100.85(14) . . ? O2 Y1 C1 109.28(16) . . ? S2 Y1 C1 86.2(2) . . ? S3 Y1 C1 100.9(2) . . ? C8 Y1 C1 95.53(16) . . ? S1 Y1 C1 33.01(11) . . ? C15 Y1 C1 94.1(2) . . ? C1 S1 Y1 73.88(18) . . ? C8 S2 Y1 77.0(2) . . ? C15 S3 Y1 76.53(16) . . ? C1 N1 C3 106.5(4) . . ? C1 N1 Y1 105.8(3) . . ? C3 N1 Y1 147.4(3) . . ? C1 N2 C2 108.4(4) . . ? C1 N2 H2 121(3) . . ? C2 N2 H2 130(3) . . ? C8 N3 C10 105.8(4) . . ? C8 N3 Y1 101.3(3) . . ? C10 N3 Y1 152.9(3) . . ? C8 N4 C9 107.6(4) . . ? C8 N4 H4 130(3) . . ? C9 N4 H4 123(3) . . ? C15 N5 C17 106.5(4) . . ? C15 N5 Y1 103.4(3) . . ? C17 N5 Y1 150.0(3) . . ? C15 N6 C16 107.8(4) . . ? C15 N6 H6 122(3) . . ? C16 N6 H6 130(3) . . ? C25 O1 C22 106.8(4) . . ? C25 O1 Y1 130.5(3) . . ? C22 O1 Y1 121.7(3) . . ? C29 O2 C26 107.5(4) . . ? C29 O2 Y1 126.8(3) . . ? C26 O2 Y1 125.7(3) . . ? N1 C1 N2 110.7(4) . . ? N1 C1 S1 122.0(3) . . ? N2 C1 S1 127.3(3) . . ? N1 C1 Y1 49.0(2) . . ? N2 C1 Y1 159.3(3) . . ? S1 C1 Y1 73.11(19) . . ? N2 C2 C7 132.6(5) . . ? N2 C2 C3 105.3(4) . . ? C7 C2 C3 122.1(5) . . ? C4 C3 N1 130.8(4) . . ? C4 C3 C2 120.1(4) . . ? N1 C3 C2 109.1(4) . . ? C3 C4 C5 117.3(5) . . ? C3 C4 H4B 121.3 . . ? C5 C4 H4B 121.3 . . ? C6 C5 C4 121.7(5) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C7 C6 C5 121.5(5) . . ? C7 C6 H6B 119.2 . . ? C5 C6 H6B 119.2 . . ? C6 C7 C2 117.2(5) . . ? C6 C7 H7A 121.4 . . ? C2 C7 H7A 121.4 . . ? N3 C8 N4 112.2(4) . . ? N3 C8 S2 121.7(4) . . ? N4 C8 S2 126.1(4) . . ? N3 C8 Y1 52.9(2) . . ? N4 C8 Y1 165.1(3) . . ? S2 C8 Y1 68.8(2) . . ? C14 C9 N4 132.4(5) . . ? C14 C9 C10 122.0(5) . . ? N4 C9 C10 105.6(4) . . ? C11 C10 N3 131.7(4) . . ? C11 C10 C9 119.5(4) . . ? N3 C10 C9 108.8(4) . . ? C12 C11 C10 118.9(5) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 120.3(5) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 122.0(5) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C9 117.3(5) . . ? C13 C14 H14A 121.3 . . ? C9 C14 H14A 121.3 . . ? N5 C15 N6 111.2(4) . . ? N5 C15 S3 121.4(3) . . ? N6 C15 S3 127.4(4) . . ? N5 C15 Y1 51.2(2) . . ? N6 C15 Y1 162.3(3) . . ? S3 C15 Y1 70.17(17) . . ? N6 C16 C17 106.1(4) . . ? N6 C16 C21 132.8(5) . . ? C17 C16 C21 121.1(5) . . ? C18 C17 C16 120.6(5) . . ? C18 C17 N5 130.9(5) . . ? C16 C17 N5 108.4(4) . . ? C17 C18 C19 117.5(5) . . ? C17 C18 H18A 121.2 . . ? C19 C18 H18A 121.2 . . ? C18 C19 C20 121.7(5) . . ? C18 C19 H19A 119.2 . . ? C20 C19 H19A 119.2 . . ? C21 C20 C19 121.3(6) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C16 117.6(6) . . ? C20 C21 H21A 121.2 . . ? C16 C21 H21A 121.2 . . ? O1 C22 C23 106.1(4) . . ? O1 C22 H22A 110.5 . . ? C23 C22 H22A 110.5 . . ? O1 C22 H22B 110.5 . . ? C23 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C22 C23 C24 104.9(5) . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.8 . . ? C25 C24 C23 105.4(5) . . ? C25 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? C25 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? O1 C25 C24 106.0(4) . . ? O1 C25 H25A 110.5 . . ? C24 C25 H25A 110.5 . . ? O1 C25 H25B 110.5 . . ? C24 C25 H25B 110.5 . . ? H25A C25 H25B 108.7 . . ? O2 C26 C27 107.4(5) . . ? O2 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? O2 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C28 C27 C26 104.1(5) . . ? C28 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? C28 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 109.0 . . ? C29 C28 C27 108.2(5) . . ? C29 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? C29 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C28 C29 O2 106.0(5) . . ? C28 C29 H29A 110.5 . . ? O2 C29 H29A 110.5 . . ? C28 C29 H29B 110.5 . . ? O2 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C33 O3 C30 109.9(5) . . ? O3 C30 C31 105.6(6) . . ? O3 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.8 . . ? C32 C31 C30 106.8(7) . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C33 C32 C31 104.9(7) . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? C33 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? H32A C32 H32B 108.8 . . ? O3 C33 C32 110.7(7) . . ? O3 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? O3 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C37 O4 C34 108.9(7) . . ? O4 C34 C35' 110.0(10) . . ? O4 C34 C35 104.5(9) . . ? C35' C34 C35 34.1(9) . . ? O4 C34 H34A 110.9 . . ? C35' C34 H34A 77.8 . . ? C35 C34 H34A 110.9 . . ? O4 C34 H34B 110.9 . . ? C35' C34 H34B 132.2 . . ? C35 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? O4 C34 H34C 111.0 . . ? C35' C34 H34C 120.5 . . ? C35 C34 H34C 143.5 . . ? H34A C34 H34C 48.2 . . ? H34B C34 H34C 64.1 . . ? O4 C34 H34D 107.6 . . ? C35' C34 H34D 98.6 . . ? C35 C34 H34D 68.0 . . ? H34A C34 H34D 140.2 . . ? H34B C34 H34D 45.6 . . ? H34C C34 H34D 107.7 . . ? C34 C35 C36 106.0(11) . . ? C34 C35 H34D 39.2 . . ? C36 C35 H34D 120.8 . . ? C34 C35 H35A 110.5 . . ? C36 C35 H35A 110.5 . . ? H34D C35 H35A 125.1 . . ? C34 C35 H35B 110.5 . . ? C36 C35 H35B 110.5 . . ? H34D C35 H35B 71.3 . . ? H35A C35 H35B 108.7 . . ? C37 C36 C35 103.5(11) . . ? C37 C36 H36A 111.1 . . ? C35 C36 H36A 111.1 . . ? C37 C36 H36B 111.1 . . ? C35 C36 H36B 111.1 . . ? H36A C36 H36B 109.0 . . ? C37 C36 H37C 36.6 . . ? C35 C36 H37C 126.3 . . ? H36A C36 H37C 75.6 . . ? H36B C36 H37C 116.5 . . ? C34 C35' C36' 105.9(12) . . ? C34 C35' H35C 110.6 . . ? C36' C35' H35C 110.6 . . ? C34 C35' H35D 110.6 . . ? C36' C35' H35D 110.6 . . ? H35C C35' H35D 108.7 . . ? C37 C36' C35' 105.1(12) . . ? C37 C36' H36C 110.7 . . ? C35' C36' H36C 110.7 . . ? C37 C36' H36D 110.7 . . ? C35' C36' H36D 110.7 . . ? H36C C36' H36D 108.8 . . ? O4 C37 C36' 110.0(10) . . ? O4 C37 C36 103.6(9) . . ? C36' C37 C36 36.1(11) . . ? O4 C37 H37A 111.0 . . ? C36' C37 H37A 133.0 . . ? C36 C37 H37A 111.0 . . ? O4 C37 H37B 111.0 . . ? C36' C37 H37B 75.8 . . ? C36 C37 H37B 111.0 . . ? H37A C37 H37B 109.0 . . ? O4 C37 H37C 111.0 . . ? C36' C37 H37C 106.2 . . ? C36 C37 H37C 76.0 . . ? H37A C37 H37C 36.6 . . ? H37B C37 H37C 134.0 . . ? O4 C37 H37D 109.8 . . ? C36' C37 H37D 111.8 . . ? C36 C37 H37D 141.5 . . ? H37A C37 H37D 74.2 . . ? H37B C37 H37D 38.7 . . ? H37C C37 H37D 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S3 0.854(19) 2.48(2) 3.305(10) 163(4) 4_566 N4 H4 O3 0.867(19) 1.98(2) 2.842(7) 176(4) 3_657 N6 H6 S1 0.846(19) 2.82(2) 3.633(9) 163(4) 4_565 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.459 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.073 # Attachment '7.cif' data_f50531d _database_code_depnum_ccdc_archive 'CCDC 762745' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40 Dy2 N2 O2 S' _chemical_formula_weight 877.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.334(4) _cell_length_b 17.848(7) _cell_length_c 19.865(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3309(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 3.068 _cell_measurement_theta_max 26.538 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6575 _exptl_absorpt_correction_T_max 0.8035 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.63 _diffrn_reflns_number 15060 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6382 _reflns_number_gt 5863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU was used to restrain some abnormal ADPs. CONN was used to tune the generation of the connectivity table. ; _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^)+(0.0631P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_number_reflns 6382 _refine_ls_number_parameters 379 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 1.07616(4) 0.84508(2) 0.183792(17) 0.03863(11) Uani 1 1 d . . . Dy2 Dy 0.95523(4) 1.075433(18) 0.011620(16) 0.03377(10) Uani 1 1 d . . . S1 S 0.9982(2) 0.92112(12) 0.06049(10) 0.0470(5) Uani 1 1 d . . . N1 N 1.2143(8) 0.9487(4) 0.1462(3) 0.0458(17) Uani 1 1 d . . . N2 N 1.1616(8) 1.0449(4) 0.0756(3) 0.0462(17) Uani 1 1 d . . . C1 C 1.315(2) 0.7837(11) 0.1362(11) 0.121(7) Uani 1 1 d . . . H1A H 1.3735 0.8041 0.0995 0.145 Uiso 1 1 calc R . . C2 C 1.3378(15) 0.7961(9) 0.2036(12) 0.108(6) Uani 1 1 d . . . H2A H 1.4168 0.8253 0.2228 0.129 Uiso 1 1 calc R . . C3 C 1.2548(19) 0.7465(10) 0.2378(7) 0.097(5) Uani 1 1 d . . . H3A H 1.2628 0.7365 0.2862 0.116 Uiso 1 1 calc R . . C4 C 1.1767(16) 0.7093(8) 0.1976(11) 0.104(6) Uani 1 1 d . . . H4A H 1.1192 0.6655 0.2102 0.125 Uiso 1 1 calc R . . C5 C 1.214(2) 0.7291(10) 0.1295(9) 0.110(6) Uani 1 1 d . . . H5A H 1.1888 0.7020 0.0883 0.132 Uiso 1 1 calc R . . C6 C 0.9092(12) 0.8439(7) 0.2912(5) 0.071(3) Uani 1 1 d . . . H6A H 0.8548 0.8007 0.3075 0.085 Uiso 1 1 calc R . . C7 C 1.0428(14) 0.8658(7) 0.3142(4) 0.070(3) Uani 1 1 d . . . H7A H 1.0978 0.8406 0.3496 0.084 Uiso 1 1 calc R . . C8 C 1.0730(14) 0.9333(8) 0.2882(5) 0.077(3) Uani 1 1 d . . . H8A H 1.1542 0.9644 0.3023 0.093 Uiso 1 1 calc R . . C9 C 0.958(2) 0.9594(7) 0.2490(6) 0.092(5) Uani 1 1 d . . . H9A H 0.9445 1.0104 0.2319 0.111 Uiso 1 1 calc R . . C10 C 0.8546(14) 0.9014(9) 0.2490(6) 0.090(5) Uani 1 1 d . . . H10A H 0.7563 0.9050 0.2319 0.108 Uiso 1 1 calc R . . C11 C 0.7759(16) 0.7252(8) 0.1833(6) 0.103(4) Uani 1 1 d DU . . H11A H 0.7144 0.7581 0.2093 0.124 Uiso 1 1 calc R . . H11B H 0.8313 0.6947 0.2142 0.124 Uiso 1 1 calc R . . C12 C 0.6878(18) 0.6764(9) 0.1381(7) 0.122(6) Uani 1 1 d D . . H12A H 0.5877 0.6778 0.1513 0.146 Uiso 1 1 calc R . . H12B H 0.7210 0.6249 0.1399 0.146 Uiso 1 1 calc R . . C13 C 0.7072(18) 0.7082(11) 0.0687(7) 0.141(8) Uani 1 1 d D . . H13A H 0.6245 0.7379 0.0560 0.169 Uiso 1 1 calc R . . H13B H 0.7192 0.6682 0.0361 0.169 Uiso 1 1 calc R . . C14 C 0.8396(17) 0.7564(9) 0.0716(5) 0.110(6) Uani 1 1 d D . . H14A H 0.9193 0.7313 0.0499 0.133 Uiso 1 1 calc R . . H14B H 0.8230 0.8037 0.0489 0.133 Uiso 1 1 calc R . . C15 C 1.1347(9) 0.9738(5) 0.0953(4) 0.0417(18) Uani 1 1 d . . . C16 C 1.3040(9) 1.0074(5) 0.1623(4) 0.048(2) Uani 1 1 d . . . C17 C 1.4074(11) 1.0166(7) 0.2124(5) 0.065(3) Uani 1 1 d . . . H17A H 1.4283 0.9779 0.2421 0.078 Uiso 1 1 calc R . . C18 C 1.4781(11) 1.0843(7) 0.2170(5) 0.069(3) Uani 1 1 d . . . H18A H 1.5498 1.0903 0.2491 0.083 Uiso 1 1 calc R . . C19 C 1.4450(12) 1.1422(7) 0.1754(5) 0.075(3) Uani 1 1 d . . . H19A H 1.4924 1.1877 0.1805 0.090 Uiso 1 1 calc R . . C20 C 1.3405(11) 1.1347(6) 0.1251(5) 0.062(3) Uani 1 1 d . . . H20A H 1.3199 1.1743 0.0962 0.075 Uiso 1 1 calc R . . C21 C 1.2694(9) 1.0675(5) 0.1196(4) 0.0452(19) Uani 1 1 d . . . C22 C 0.8175(14) 1.1333(6) 0.1180(6) 0.073(3) Uani 1 1 d . . . H22A H 0.7670 1.1043 0.1526 0.088 Uiso 1 1 calc R . . C23 C 0.9571(13) 1.1599(7) 0.1232(6) 0.080(3) Uani 1 1 d . . . H23A H 1.0211 1.1540 0.1619 0.096 Uiso 1 1 calc R . . C24 C 0.9776(18) 1.2092(7) 0.0674(9) 0.105(6) Uani 1 1 d . . . H24A H 1.0586 1.2436 0.0617 0.126 Uiso 1 1 calc R . . C25 C 0.8528(19) 1.2103(7) 0.0298(9) 0.104(5) Uani 1 1 d . . . H25A H 0.8300 1.2463 -0.0058 0.124 Uiso 1 1 calc R . . C26 C 0.7557(14) 1.1641(8) 0.0620(8) 0.088(4) Uani 1 1 d . . . H26A H 0.6535 1.1611 0.0510 0.106 Uiso 1 1 calc R . . C27 C 1.1652(13) 1.1018(7) -0.0743(5) 0.067(3) Uani 1 1 d . . . H27A H 1.2626 1.1172 -0.0621 0.081 Uiso 1 1 calc R . . C28 C 1.0558(15) 1.1498(7) -0.0937(6) 0.081(3) Uani 1 1 d . . . H28A H 1.0629 1.2044 -0.0978 0.097 Uiso 1 1 calc R . . C29 C 0.9404(17) 1.1043(10) -0.1176(5) 0.100(5) Uani 1 1 d . . . H29A H 0.8553 1.1230 -0.1411 0.120 Uiso 1 1 calc R . . C30 C 0.9809(14) 1.0298(9) -0.1135(5) 0.082(4) Uani 1 1 d . . . H30A H 0.9295 0.9875 -0.1337 0.098 Uiso 1 1 calc R . . C31 C 1.1201(12) 1.0270(7) -0.0862(5) 0.064(3) Uani 1 1 d . . . H31A H 1.1815 0.9825 -0.0844 0.077 Uiso 1 1 calc R . . C32 C 0.6415(11) 0.9814(8) 0.0478(5) 0.083(4) Uani 1 1 d D . . H32A H 0.6027 1.0208 0.0761 0.100 Uiso 1 1 calc R . . H32B H 0.6994 0.9483 0.0753 0.100 Uiso 1 1 calc R . . C33 C 0.5217(12) 0.9382(7) 0.0134(6) 0.094(4) Uani 1 1 d D . . H33A H 0.5485 0.8862 0.0072 0.113 Uiso 1 1 calc R . . H33B H 0.4345 0.9403 0.0399 0.113 Uiso 1 1 calc R . . C34 C 0.5008(13) 0.9764(11) -0.0537(8) 0.133(7) Uani 1 1 d D . . H34A H 0.4897 0.9398 -0.0894 0.160 Uiso 1 1 calc R . . H34B H 0.4168 1.0084 -0.0528 0.160 Uiso 1 1 calc R . . C35 C 0.6339(14) 1.0219(11) -0.0639(6) 0.128(7) Uani 1 1 d D . . H35A H 0.6834 1.0052 -0.1042 0.153 Uiso 1 1 calc R . . H35B H 0.6092 1.0743 -0.0695 0.153 Uiso 1 1 calc R . . O1 O 0.8703(8) 0.7687(4) 0.1411(3) 0.071(2) Uani 1 1 d DU . . O2 O 0.7250(6) 1.0126(4) -0.0061(3) 0.0584(17) Uani 1 1 d 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 Dy1 0.0437(2) 0.03999(19) 0.03222(17) 0.00625(14) 0.00186(15) 0.00589(16) Dy2 0.03513(18) 0.03451(17) 0.03167(16) 0.00422(13) 0.00338(13) 0.00364(14) S1 0.0557(12) 0.0401(10) 0.0451(10) 0.0040(9) -0.0137(9) -0.0048(9) N1 0.047(4) 0.052(4) 0.039(4) 0.009(3) -0.012(3) -0.004(3) N2 0.054(4) 0.049(4) 0.037(4) 0.006(3) -0.009(3) -0.009(3) C1 0.128(15) 0.099(13) 0.136(15) 0.056(11) 0.072(13) 0.062(11) C2 0.058(8) 0.081(10) 0.184(18) -0.002(12) -0.022(10) 0.021(7) C3 0.106(12) 0.105(12) 0.080(9) 0.030(9) -0.005(8) 0.060(10) C4 0.075(9) 0.068(9) 0.169(17) 0.051(10) 0.018(11) 0.022(7) C5 0.138(16) 0.093(11) 0.099(11) -0.028(10) -0.015(11) 0.057(11) C6 0.076(7) 0.083(7) 0.053(5) -0.005(5) 0.024(5) -0.003(7) C7 0.077(7) 0.101(8) 0.031(4) -0.008(5) 0.001(5) 0.004(6) C8 0.079(8) 0.097(9) 0.056(6) -0.019(6) -0.001(6) -0.019(8) C9 0.155(14) 0.056(7) 0.065(7) -0.002(5) 0.031(9) 0.039(9) C10 0.068(7) 0.141(13) 0.060(7) -0.037(8) -0.003(6) 0.046(8) C11 0.112(8) 0.103(8) 0.094(7) 0.013(7) 0.005(7) -0.048(7) C12 0.135(15) 0.113(13) 0.118(12) -0.002(10) -0.007(11) -0.054(12) C13 0.149(17) 0.162(17) 0.113(13) -0.003(12) -0.024(12) -0.101(15) C14 0.140(14) 0.113(12) 0.078(9) -0.004(8) -0.021(9) -0.065(11) C15 0.045(5) 0.042(5) 0.038(4) -0.003(3) -0.003(3) -0.003(4) C16 0.034(4) 0.068(6) 0.043(4) 0.011(4) -0.005(3) -0.008(4) C17 0.054(6) 0.096(8) 0.045(5) 0.006(5) -0.014(4) -0.005(6) C18 0.055(6) 0.106(9) 0.047(5) -0.001(6) -0.011(4) -0.034(6) C19 0.068(6) 0.098(8) 0.058(6) -0.010(6) -0.003(5) -0.041(7) C20 0.068(6) 0.062(6) 0.056(5) 0.004(5) -0.008(5) -0.021(5) C21 0.046(4) 0.053(5) 0.036(4) 0.003(4) -0.001(3) -0.005(4) C22 0.078(8) 0.065(7) 0.077(7) -0.024(6) 0.030(6) 0.008(6) C23 0.069(7) 0.091(8) 0.079(7) -0.047(7) 0.009(6) 0.013(7) C24 0.099(11) 0.046(7) 0.171(15) -0.047(8) 0.051(11) -0.008(6) C25 0.096(11) 0.059(8) 0.156(15) 0.014(8) 0.032(11) 0.031(7) C26 0.069(8) 0.088(9) 0.108(10) -0.033(8) 0.011(7) 0.038(7) C27 0.060(6) 0.091(8) 0.050(5) 0.009(5) 0.016(5) -0.019(6) C28 0.092(9) 0.082(8) 0.069(7) 0.033(6) 0.016(7) -0.006(8) C29 0.079(8) 0.176(15) 0.046(6) 0.050(8) -0.003(6) 0.018(10) C30 0.079(9) 0.124(11) 0.042(5) -0.016(6) 0.016(5) -0.029(8) C31 0.063(7) 0.085(8) 0.044(5) -0.012(5) 0.021(5) 0.003(6) C32 0.046(6) 0.120(11) 0.082(8) 0.021(7) 0.000(6) -0.021(7) C33 0.075(8) 0.112(10) 0.095(9) -0.007(8) 0.022(7) -0.031(7) C34 0.066(9) 0.174(17) 0.160(16) 0.077(14) -0.042(9) -0.042(10) C35 0.081(10) 0.213(19) 0.089(10) 0.061(11) -0.050(8) -0.063(12) O1 0.082(5) 0.069(4) 0.062(4) 0.002(3) 0.005(4) -0.026(4) O2 0.032(3) 0.082(5) 0.061(4) 0.013(3) -0.013(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N1 2.375(7) . ? Dy1 O1 2.504(7) . ? Dy1 C8 2.604(10) . ? Dy1 C4 2.613(12) . ? Dy1 C2 2.624(13) . ? Dy1 C7 2.635(9) . ? Dy1 C10 2.639(11) . ? Dy1 C6 2.642(9) . ? Dy1 C3 2.651(11) . ? Dy1 C1 2.658(15) . ? Dy1 C9 2.658(10) . ? Dy1 C5 2.666(14) . ? Dy1 S1 2.893(2) . ? Dy1 C15 2.944(8) . ? Dy2 N2 2.371(7) . ? Dy2 O2 2.449(5) . ? Dy2 C25 2.615(12) . ? Dy2 C29 2.622(10) . ? Dy2 C31 2.625(9) . ? Dy2 C30 2.627(10) . ? Dy2 C24 2.640(11) . ? Dy2 C27 2.641(10) . ? Dy2 C26 2.641(10) . ? Dy2 C28 2.650(10) . ? Dy2 C23 2.680(10) . ? Dy2 C22 2.681(10) . ? Dy2 S1 2.948(2) . ? Dy2 C15 2.977(8) . ? S1 C15 1.728(8) . ? N1 C15 1.332(10) . ? N1 C16 1.380(11) . ? N2 C15 1.351(11) . ? N2 C21 1.392(11) . ? C1 C5 1.36(3) . ? C1 C2 1.37(3) . ? C2 C3 1.36(2) . ? C3 C4 1.27(2) . ? C4 C5 1.44(2) . ? C6 C7 1.384(16) . ? C6 C10 1.418(17) . ? C7 C8 1.341(16) . ? C8 C9 1.408(18) . ? C9 C10 1.41(2) . ? C11 O1 1.443(8) . ? C11 C12 1.497(9) . ? C12 C13 1.502(9) . ? C13 C14 1.508(9) . ? C14 O1 1.426(8) . ? C16 C17 1.395(12) . ? C16 C21 1.406(12) . ? C17 C18 1.379(14) . ? C18 C19 1.359(16) . ? C19 C20 1.403(14) . ? C20 C21 1.376(12) . ? C22 C26 1.370(18) . ? C22 C23 1.391(17) . ? C23 C24 1.43(2) . ? C24 C25 1.38(2) . ? C25 C26 1.38(2) . ? C27 C28 1.387(17) . ? C27 C31 1.421(16) . ? C28 C29 1.430(19) . ? C29 C30 1.386(19) . ? C30 C31 1.409(16) . ? C32 O2 1.436(8) . ? C32 C33 1.521(9) . ? C33 C34 1.509(9) . ? C34 C35 1.497(9) . ? C35 O2 1.440(8) . ? 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 N1 Dy1 O1 137.2(2) . . ? N1 Dy1 C8 77.6(3) . . ? O1 Dy1 C8 126.2(3) . . ? N1 Dy1 C4 124.0(4) . . ? O1 Dy1 C4 78.8(5) . . ? C8 Dy1 C4 118.8(6) . . ? N1 Dy1 C2 78.5(5) . . ? O1 Dy1 C2 125.7(4) . . ? C8 Dy1 C2 95.3(5) . . ? C4 Dy1 C2 48.8(5) . . ? N1 Dy1 C7 105.3(3) . . ? O1 Dy1 C7 108.6(3) . . ? C8 Dy1 C7 29.7(3) . . ? C4 Dy1 C7 94.0(6) . . ? C2 Dy1 C7 90.5(6) . . ? N1 Dy1 C10 106.5(4) . . ? O1 Dy1 C10 76.8(4) . . ? C8 Dy1 C10 51.0(4) . . ? C4 Dy1 C10 125.7(5) . . ? C2 Dy1 C10 141.5(5) . . ? C7 Dy1 C10 51.1(4) . . ? N1 Dy1 C6 125.5(3) . . ? O1 Dy1 C6 79.4(3) . . ? C8 Dy1 C6 49.8(4) . . ? C4 Dy1 C6 96.9(5) . . ? C2 Dy1 C6 115.2(6) . . ? C7 Dy1 C6 30.4(3) . . ? C10 Dy1 C6 31.2(4) . . ? N1 Dy1 C3 107.6(5) . . ? O1 Dy1 C3 105.0(5) . . ? C8 Dy1 C3 94.9(5) . . ? C4 Dy1 C3 27.9(5) . . ? C2 Dy1 C3 29.9(5) . . ? C7 Dy1 C3 76.7(4) . . ? C10 Dy1 C3 123.1(5) . . ? C6 Dy1 C3 92.2(4) . . ? N1 Dy1 C1 75.7(5) . . ? O1 Dy1 C1 107.4(6) . . ? C8 Dy1 C1 122.8(7) . . ? C4 Dy1 C1 49.8(5) . . ? C2 Dy1 C1 30.1(6) . . ? C7 Dy1 C1 120.4(6) . . ? C10 Dy1 C1 171.4(6) . . ? C6 Dy1 C1 141.2(5) . . ? C3 Dy1 C1 48.9(5) . . ? N1 Dy1 C9 77.4(4) . . ? O1 Dy1 C9 105.3(5) . . ? C8 Dy1 C9 31.0(4) . . ? C4 Dy1 C9 144.1(5) . . ? C2 Dy1 C9 124.7(6) . . ? C7 Dy1 C9 50.5(4) . . ? C10 Dy1 C9 31.0(4) . . ? C6 Dy1 C9 50.7(4) . . ? C3 Dy1 C9 125.0(5) . . ? C1 Dy1 C9 147.0(7) . . ? N1 Dy1 C5 102.4(5) . . ? O1 Dy1 C5 79.2(5) . . ? C8 Dy1 C5 142.8(5) . . ? C4 Dy1 C5 31.7(5) . . ? C2 Dy1 C5 49.6(5) . . ? C7 Dy1 C5 124.3(5) . . ? C10 Dy1 C5 150.8(7) . . ? C6 Dy1 C5 127.3(6) . . ? C3 Dy1 C5 49.0(5) . . ? C1 Dy1 C5 29.6(6) . . ? C9 Dy1 C5 173.8(5) . . ? N1 Dy1 S1 60.34(16) . . ? O1 Dy1 S1 77.00(17) . . ? C8 Dy1 S1 112.8(3) . . ? C4 Dy1 S1 127.9(5) . . ? C2 Dy1 S1 121.2(5) . . ? C7 Dy1 S1 137.5(3) . . ? C10 Dy1 S1 92.3(3) . . ? C6 Dy1 S1 122.6(3) . . ? C3 Dy1 S1 144.3(3) . . ? C1 Dy1 S1 95.9(4) . . ? C9 Dy1 S1 87.0(3) . . ? C5 Dy1 S1 98.2(4) . . ? N1 Dy1 C15 26.3(2) . . ? O1 Dy1 C15 111.4(2) . . ? C8 Dy1 C15 90.3(3) . . ? C4 Dy1 C15 136.0(4) . . ? C2 Dy1 C15 100.2(5) . . ? C7 Dy1 C15 120.0(3) . . ? C10 Dy1 C15 98.1(4) . . ? C6 Dy1 C15 126.7(3) . . ? C3 Dy1 C15 130.0(5) . . ? C1 Dy1 C15 87.3(4) . . ? C9 Dy1 C15 76.7(3) . . ? C5 Dy1 C15 105.9(5) . . ? S1 Dy1 C15 34.42(16) . . ? N2 Dy2 O2 133.2(2) . . ? N2 Dy2 C25 115.7(5) . . ? O2 Dy2 C25 96.9(4) . . ? N2 Dy2 C29 127.8(4) . . ? O2 Dy2 C29 84.4(4) . . ? C25 Dy2 C29 86.3(6) . . ? N2 Dy2 C31 81.1(3) . . ? O2 Dy2 C31 104.9(3) . . ? C25 Dy2 C31 128.3(5) . . ? C29 Dy2 C31 51.0(4) . . ? N2 Dy2 C30 111.2(4) . . ? O2 Dy2 C30 78.6(3) . . ? C25 Dy2 C30 116.7(6) . . ? C29 Dy2 C30 30.6(4) . . ? C31 Dy2 C30 31.1(4) . . ? N2 Dy2 C24 85.3(5) . . ? O2 Dy2 C24 122.9(4) . . ? C25 Dy2 C24 30.5(5) . . ? C29 Dy2 C24 103.7(6) . . ? C31 Dy2 C24 124.2(4) . . ? C30 Dy2 C24 132.1(5) . . ? N2 Dy2 C27 77.6(3) . . ? O2 Dy2 C27 129.8(3) . . ? C25 Dy2 C27 101.3(5) . . ? C29 Dy2 C27 51.1(4) . . ? C31 Dy2 C27 31.3(4) . . ? C30 Dy2 C27 51.4(4) . . ? C24 Dy2 C27 92.9(4) . . ? N2 Dy2 C26 120.5(4) . . ? O2 Dy2 C26 73.1(4) . . ? C25 Dy2 C26 30.5(4) . . ? C29 Dy2 C26 102.5(5) . . ? C31 Dy2 C26 153.0(5) . . ? C30 Dy2 C26 127.5(5) . . ? C24 Dy2 C26 49.8(5) . . ? C27 Dy2 C26 131.4(4) . . ? N2 Dy2 C28 104.5(4) . . ? O2 Dy2 C28 115.3(3) . . ? C25 Dy2 C28 77.2(5) . . ? C29 Dy2 C28 31.5(4) . . ? C31 Dy2 C28 51.2(4) . . ? C30 Dy2 C28 51.4(4) . . ? C24 Dy2 C28 81.4(5) . . ? C27 Dy2 C28 30.4(4) . . ? C26 Dy2 C28 104.4(5) . . ? N2 Dy2 C23 71.4(3) . . ? O2 Dy2 C23 112.4(3) . . ? C25 Dy2 C23 51.0(5) . . ? C29 Dy2 C23 134.4(5) . . ? C31 Dy2 C23 142.5(4) . . ? C30 Dy2 C23 163.0(5) . . ? C24 Dy2 C23 31.1(4) . . ? C27 Dy2 C23 115.4(4) . . ? C26 Dy2 C23 49.8(4) . . ? C28 Dy2 C23 111.7(5) . . ? N2 Dy2 C22 93.2(4) . . ? O2 Dy2 C22 82.4(3) . . ? C25 Dy2 C22 50.3(5) . . ? C29 Dy2 C22 132.1(5) . . ? C31 Dy2 C22 172.6(4) . . ? C30 Dy2 C22 155.4(4) . . ? C24 Dy2 C22 50.1(4) . . ? C27 Dy2 C22 142.8(4) . . ? C26 Dy2 C22 29.8(4) . . ? C28 Dy2 C22 126.9(4) . . ? C23 Dy2 C22 30.1(4) . . ? N2 Dy2 S1 59.88(18) . . ? O2 Dy2 S1 74.86(16) . . ? C25 Dy2 S1 149.8(4) . . ? C29 Dy2 S1 120.9(4) . . ? C31 Dy2 S1 81.7(3) . . ? C30 Dy2 S1 90.5(4) . . ? C24 Dy2 S1 134.1(4) . . ? C27 Dy2 S1 106.2(3) . . ? C26 Dy2 S1 122.1(4) . . ? C28 Dy2 S1 132.8(3) . . ? C23 Dy2 S1 104.6(3) . . ? C22 Dy2 S1 99.5(3) . . ? N2 Dy2 C15 26.3(2) . . ? O2 Dy2 C15 107.1(2) . . ? C25 Dy2 C15 133.6(5) . . ? C29 Dy2 C15 134.1(4) . . ? C31 Dy2 C15 83.3(3) . . ? C30 Dy2 C15 106.7(4) . . ? C24 Dy2 C15 105.8(5) . . ? C27 Dy2 C15 93.0(3) . . ? C26 Dy2 C15 123.4(4) . . ? C28 Dy2 C15 123.1(4) . . ? C23 Dy2 C15 83.0(3) . . ? C22 Dy2 C15 93.7(3) . . ? S1 Dy2 C15 33.91(16) . . ? C15 S1 Dy1 74.4(3) . . ? C15 S1 Dy2 74.0(3) . . ? Dy1 S1 Dy2 138.70(8) . . ? C15 N1 C16 105.0(7) . . ? C15 N1 Dy1 101.4(5) . . ? C16 N1 Dy1 148.0(6) . . ? C15 N2 C21 103.0(7) . . ? C15 N2 Dy2 102.7(5) . . ? C21 N2 Dy2 148.9(6) . . ? C5 C1 C2 108.5(16) . . ? C5 C1 Dy1 75.5(10) . . ? C2 C1 Dy1 73.5(8) . . ? C3 C2 C1 107.2(16) . . ? C3 C2 Dy1 76.2(8) . . ? C1 C2 Dy1 76.3(9) . . ? C4 C3 C2 110.7(15) . . ? C4 C3 Dy1 74.4(8) . . ? C2 C3 Dy1 73.9(7) . . ? C3 C4 C5 108.8(15) . . ? C3 C4 Dy1 77.7(9) . . ? C5 C4 Dy1 76.2(8) . . ? C1 C5 C4 104.7(16) . . ? C1 C5 Dy1 74.9(9) . . ? C4 C5 Dy1 72.1(8) . . ? C7 C6 C10 108.4(12) . . ? C7 C6 Dy1 74.5(5) . . ? C10 C6 Dy1 74.3(6) . . ? C8 C7 C6 108.4(12) . . ? C8 C7 Dy1 73.9(6) . . ? C6 C7 Dy1 75.1(5) . . ? C7 C8 C9 110.5(12) . . ? C7 C8 Dy1 76.5(6) . . ? C9 C8 Dy1 76.6(6) . . ? C8 C9 C10 106.1(10) . . ? C8 C9 Dy1 72.4(6) . . ? C10 C9 Dy1 73.8(6) . . ? C9 C10 C6 106.6(11) . . ? C9 C10 Dy1 75.3(7) . . ? C6 C10 Dy1 74.5(6) . . ? O1 C11 C12 107.5(9) . . ? C11 C12 C13 105.3(9) . . ? C12 C13 C14 106.2(9) . . ? O1 C14 C13 106.8(9) . . ? N1 C15 N2 115.6(7) . . ? N1 C15 S1 122.1(6) . . ? N2 C15 S1 122.2(6) . . ? N1 C15 Dy1 52.3(4) . . ? N2 C15 Dy1 160.0(6) . . ? S1 C15 Dy1 71.2(3) . . ? N1 C15 Dy2 160.5(6) . . ? N2 C15 Dy2 51.0(4) . . ? S1 C15 Dy2 72.1(3) . . ? Dy1 C15 Dy2 134.8(3) . . ? N1 C16 C17 132.5(9) . . ? N1 C16 C21 107.4(7) . . ? C17 C16 C21 120.0(9) . . ? C18 C17 C16 118.8(9) . . ? C19 C18 C17 121.1(9) . . ? C18 C19 C20 121.2(10) . . ? C21 C20 C19 118.4(10) . . ? C20 C21 N2 130.7(8) . . ? C20 C21 C16 120.4(8) . . ? N2 C21 C16 108.9(7) . . ? C26 C22 C23 108.5(12) . . ? C26 C22 Dy2 73.5(6) . . ? C23 C22 Dy2 74.9(6) . . ? C22 C23 C24 106.2(13) . . ? C22 C23 Dy2 75.0(6) . . ? C24 C23 Dy2 72.9(6) . . ? C25 C24 C23 108.3(13) . . ? C25 C24 Dy2 73.7(8) . . ? C23 C24 Dy2 76.0(6) . . ? C26 C25 C24 107.1(14) . . ? C26 C25 Dy2 75.8(7) . . ? C24 C25 Dy2 75.8(7) . . ? C22 C26 C25 109.8(14) . . ? C22 C26 Dy2 76.7(6) . . ? C25 C26 Dy2 73.7(7) . . ? C28 C27 C31 108.4(11) . . ? C28 C27 Dy2 75.2(6) . . ? C31 C27 Dy2 73.7(6) . . ? C27 C28 C29 107.3(12) . . ? C27 C28 Dy2 74.5(6) . . ? C29 C28 Dy2 73.2(6) . . ? C30 C29 C28 108.6(13) . . ? C30 C29 Dy2 74.9(6) . . ? C28 C29 Dy2 75.3(6) . . ? C29 C30 C31 108.0(13) . . ? C29 C30 Dy2 74.5(7) . . ? C31 C30 Dy2 74.4(6) . . ? C30 C31 C27 107.7(12) . . ? C30 C31 Dy2 74.5(6) . . ? C27 C31 Dy2 75.0(6) . . ? O2 C32 C33 105.1(7) . . ? C34 C33 C32 105.2(9) . . ? C35 C34 C33 104.9(8) . . ? O2 C35 C34 108.6(8) . . ? C14 O1 C11 110.9(8) . . ? C14 O1 Dy1 124.5(6) . . ? C11 O1 Dy1 124.3(6) . . ? C32 O2 C35 108.6(7) . . ? C32 O2 Dy2 123.2(5) . . ? C35 O2 Dy2 125.5(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.243 _refine_diff_density_min -1.906 _refine_diff_density_rms 0.148 # Attachment '6.cif' data_f70513a _database_code_depnum_ccdc_archive 'CCDC 762746' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40 Er2 N2 O2 S' _chemical_formula_weight 887.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.290(3) _cell_length_b 17.813(6) _cell_length_c 19.826(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3281(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 902 _cell_measurement_theta_min 2.507 _cell_measurement_theta_max 24.964 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 5.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4241 _exptl_absorpt_correction_T_max 0.6255 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16360 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7075 _reflns_number_gt 6144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU and SADI were used to restrain some abnormal ADPs. CONN was used to tune the generation of the connectivity table. ; _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^)+(0.0335P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(15) _refine_ls_number_reflns 7075 _refine_ls_number_parameters 379 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 1.07565(3) 0.845262(18) 0.183875(14) 0.04048(9) Uani 1 1 d D . . Er2 Er 0.95528(3) 1.075228(16) 0.011653(13) 0.03559(8) Uani 1 1 d D . . S1 S 0.99842(19) 0.92132(10) 0.06090(9) 0.0451(4) Uani 1 1 d . . . N1 N 1.2149(6) 0.9485(3) 0.1467(3) 0.0457(14) Uani 1 1 d D . . N2 N 1.1606(6) 1.0443(3) 0.0768(3) 0.0411(13) Uani 1 1 d D . . C1 C 1.3075(17) 0.7798(9) 0.1332(8) 0.107(5) Uani 1 1 d . . . H1A H 1.3631 0.7975 0.0943 0.128 Uiso 1 1 calc R . . C2 C 1.3378(12) 0.7962(7) 0.2024(11) 0.119(5) Uani 1 1 d . . . H2A H 1.4200 0.8242 0.2206 0.143 Uiso 1 1 calc R . . C3 C 1.2492(16) 0.7456(9) 0.2368(6) 0.098(4) Uani 1 1 d . . . H3A H 1.2560 0.7346 0.2851 0.118 Uiso 1 1 calc R . . C4 C 1.1752(13) 0.7080(6) 0.1952(10) 0.100(4) Uani 1 1 d . . . H4A H 1.1160 0.6646 0.2076 0.120 Uiso 1 1 calc R . . C5 C 1.2055(17) 0.7271(9) 0.1320(7) 0.101(4) Uani 1 1 d . . . H5A H 1.1738 0.6998 0.0917 0.121 Uiso 1 1 calc R . . C6 C 0.9100(10) 0.8440(6) 0.2908(4) 0.069(2) Uani 1 1 d . . . H6A H 0.8554 0.8007 0.3075 0.083 Uiso 1 1 calc R . . C7 C 1.0419(11) 0.8663(5) 0.3135(4) 0.067(2) Uani 1 1 d . . . H7A H 1.0973 0.8408 0.3487 0.080 Uiso 1 1 calc R . . C8 C 1.0720(13) 0.9346(6) 0.2886(4) 0.078(3) Uani 1 1 d . . . H8A H 1.1521 0.9666 0.3032 0.094 Uiso 1 1 calc R . . C9 C 0.9551(17) 0.9584(6) 0.2497(5) 0.091(4) Uani 1 1 d . . . H9A H 0.9400 1.0092 0.2321 0.109 Uiso 1 1 calc R . . C10 C 0.8554(11) 0.9017(9) 0.2506(5) 0.091(4) Uani 1 1 d . . . H10A H 0.7565 0.9053 0.2338 0.109 Uiso 1 1 calc R . . C11 C 0.7785(16) 0.7245(9) 0.1836(5) 0.135(6) Uani 1 1 d DU . . H11A H 0.7176 0.7568 0.2108 0.162 Uiso 1 1 calc R . . H11B H 0.8359 0.6936 0.2136 0.162 Uiso 1 1 calc R . . C12 C 0.6882(15) 0.6760(7) 0.1394(5) 0.117(5) Uani 1 1 d D . . H12A H 0.7218 0.6245 0.1405 0.140 Uiso 1 1 calc R . . H12B H 0.5884 0.6773 0.1536 0.140 Uiso 1 1 calc R . . C13 C 0.7041(14) 0.7081(7) 0.0706(5) 0.117(5) Uani 1 1 d D . . H13A H 0.6200 0.7376 0.0588 0.140 Uiso 1 1 calc R . . H13B H 0.7155 0.6684 0.0376 0.140 Uiso 1 1 calc R . . C14 C 0.8355(14) 0.7567(7) 0.0726(4) 0.113(5) Uani 1 1 d D . . H14A H 0.9148 0.7320 0.0497 0.136 Uiso 1 1 calc R . . H14B H 0.8168 0.8041 0.0501 0.136 Uiso 1 1 calc R . . C15 C 1.1355(8) 0.9736(4) 0.0958(3) 0.0412(16) Uani 1 1 d . . . C16 C 1.3030(8) 1.0082(4) 0.1626(3) 0.0460(17) Uani 1 1 d . . . C17 C 1.4073(9) 1.0159(6) 0.2128(4) 0.063(2) Uani 1 1 d . . . H17A H 1.4287 0.9769 0.2423 0.076 Uiso 1 1 calc R . . C18 C 1.4774(9) 1.0841(6) 0.2166(4) 0.066(2) Uani 1 1 d . . . H18A H 1.5491 1.0904 0.2488 0.080 Uiso 1 1 calc R . . C19 C 1.4449(10) 1.1428(5) 0.1746(4) 0.071(2) Uani 1 1 d . . . H19A H 1.4934 1.1882 0.1795 0.085 Uiso 1 1 calc R . . C20 C 1.3412(9) 1.1356(5) 0.1249(4) 0.063(2) Uani 1 1 d . . . H20A H 1.3207 1.1752 0.0959 0.076 Uiso 1 1 calc R . . C21 C 1.2685(7) 1.0677(4) 0.1196(3) 0.0446(17) Uani 1 1 d . . . C22 C 0.8192(11) 1.1323(6) 0.1175(5) 0.072(3) Uani 1 1 d . . . H22A H 0.7715 1.1032 0.1530 0.087 Uiso 1 1 calc R . . C23 C 0.9570(11) 1.1620(6) 0.1211(6) 0.083(3) Uani 1 1 d . . . H23A H 1.0228 1.1567 0.1594 0.100 Uiso 1 1 calc R . . C24 C 0.9782(16) 1.2075(6) 0.0668(7) 0.101(4) Uani 1 1 d . . . H24A H 1.0604 1.2414 0.0611 0.121 Uiso 1 1 calc R . . C25 C 0.8521(18) 1.2104(6) 0.0293(7) 0.109(5) Uani 1 1 d . . . H25A H 0.8289 1.2469 -0.0061 0.131 Uiso 1 1 calc R . . C26 C 0.7537(11) 1.1629(6) 0.0633(7) 0.085(3) Uani 1 1 d . . . H26A H 0.6506 1.1592 0.0533 0.102 Uiso 1 1 calc R . . C27 C 1.1614(9) 1.1016(5) -0.0742(4) 0.058(2) Uani 1 1 d . . . H27A H 1.2591 1.1176 -0.0622 0.070 Uiso 1 1 calc R . . C28 C 1.0535(11) 1.1482(6) -0.0940(4) 0.078(3) Uani 1 1 d . . . H28A H 1.0606 1.2029 -0.0982 0.093 Uiso 1 1 calc R . . C29 C 0.9435(13) 1.1051(8) -0.1175(4) 0.092(4) Uani 1 1 d . . . H29A H 0.8585 1.1241 -0.1414 0.110 Uiso 1 1 calc R . . C30 C 0.9827(12) 1.0305(8) -0.1129(4) 0.086(4) Uani 1 1 d . . . H30A H 0.9312 0.9883 -0.1334 0.103 Uiso 1 1 calc R . . C31 C 1.1191(10) 1.0275(6) -0.0858(4) 0.064(2) Uani 1 1 d . . . H31A H 1.1817 0.9832 -0.0844 0.076 Uiso 1 1 calc R . . C32 C 0.6428(9) 0.9811(6) 0.0475(4) 0.079(3) Uani 1 1 d D . . H32A H 0.6047 1.0203 0.0764 0.095 Uiso 1 1 calc R . . H32B H 0.7015 0.9477 0.0747 0.095 Uiso 1 1 calc R . . C33 C 0.5225(10) 0.9384(6) 0.0146(5) 0.092(3) Uani 1 1 d D . . H33A H 0.5487 0.8862 0.0083 0.110 Uiso 1 1 calc R . . H33B H 0.4357 0.9409 0.0417 0.110 Uiso 1 1 calc R . . C34 C 0.5010(11) 0.9765(8) -0.0518(6) 0.122(5) Uani 1 1 d D . . H34A H 0.4847 0.9398 -0.0872 0.147 Uiso 1 1 calc R . . H34B H 0.4191 1.0102 -0.0499 0.147 Uiso 1 1 calc R . . C35 C 0.6360(12) 1.0191(9) -0.0645(5) 0.137(7) Uani 1 1 d D . . H35A H 0.6850 0.9988 -0.1037 0.165 Uiso 1 1 calc R . . H35B H 0.6138 1.0714 -0.0733 0.165 Uiso 1 1 calc R . . O1 O 0.8708(6) 0.7693(3) 0.1415(3) 0.0654(16) Uani 1 1 d DU . . O2 O 0.7264(5) 1.0130(3) -0.0063(3) 0.0580(14) Uani 1 1 d 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 Er1 0.04307(17) 0.04430(17) 0.03407(14) 0.00595(13) 0.00202(13) 0.00577(14) Er2 0.03402(15) 0.03872(15) 0.03404(13) 0.00449(12) 0.00342(12) 0.00364(12) S1 0.0514(10) 0.0402(9) 0.0437(9) 0.0042(8) -0.0145(7) -0.0045(8) N1 0.042(3) 0.053(4) 0.042(3) 0.011(3) -0.006(3) 0.001(3) N2 0.043(3) 0.044(3) 0.036(3) 0.005(3) -0.007(2) -0.003(3) C1 0.102(10) 0.109(11) 0.110(10) 0.054(9) 0.050(9) 0.060(9) C2 0.043(6) 0.085(8) 0.230(18) -0.001(11) -0.025(9) 0.033(6) C3 0.099(10) 0.115(11) 0.080(7) 0.038(8) 0.002(7) 0.062(8) C4 0.082(8) 0.056(7) 0.162(14) 0.028(8) -0.004(9) 0.009(5) C5 0.122(12) 0.099(10) 0.081(8) -0.033(8) -0.018(8) 0.053(9) C6 0.072(6) 0.079(6) 0.057(5) -0.015(5) 0.025(5) -0.006(5) C7 0.068(6) 0.100(7) 0.032(3) -0.003(4) 0.002(4) 0.008(5) C8 0.097(8) 0.084(7) 0.053(5) -0.016(5) 0.011(5) -0.011(7) C9 0.146(11) 0.061(6) 0.065(6) 0.003(5) 0.041(8) 0.038(8) C10 0.049(6) 0.162(12) 0.061(6) -0.035(7) 0.004(5) 0.031(7) C11 0.144(12) 0.165(13) 0.097(8) 0.034(9) -0.004(9) -0.095(10) C12 0.147(13) 0.107(10) 0.097(8) -0.017(8) 0.016(9) -0.058(9) C13 0.128(12) 0.111(10) 0.111(9) 0.007(8) -0.026(9) -0.063(9) C14 0.139(12) 0.119(10) 0.081(7) -0.007(7) -0.012(8) -0.065(9) C15 0.045(4) 0.043(4) 0.035(3) -0.001(3) -0.006(3) 0.001(3) C16 0.036(4) 0.063(5) 0.039(3) 0.008(3) -0.003(3) -0.004(3) C17 0.047(5) 0.094(7) 0.049(4) 0.008(4) -0.007(4) -0.008(4) C18 0.046(5) 0.103(7) 0.051(4) -0.006(5) -0.002(4) -0.022(5) C19 0.056(5) 0.091(7) 0.066(5) -0.014(5) 0.003(5) -0.038(5) C20 0.065(5) 0.069(6) 0.055(5) 0.007(4) -0.010(4) -0.019(4) C21 0.037(4) 0.061(5) 0.036(3) -0.003(4) 0.000(3) -0.010(3) C22 0.065(6) 0.078(7) 0.073(6) -0.023(5) 0.026(5) 0.012(5) C23 0.066(6) 0.090(7) 0.094(7) -0.059(6) 0.016(6) -0.001(6) C24 0.112(11) 0.051(6) 0.139(11) -0.038(7) 0.039(9) -0.019(6) C25 0.140(12) 0.055(7) 0.131(11) 0.005(7) 0.019(10) 0.051(7) C26 0.055(6) 0.064(6) 0.136(10) -0.021(7) 0.020(6) 0.024(5) C27 0.048(5) 0.082(6) 0.046(4) 0.014(4) 0.011(4) -0.015(4) C28 0.076(7) 0.092(7) 0.065(5) 0.051(5) 0.022(5) 0.006(6) C29 0.069(7) 0.164(11) 0.042(4) 0.044(6) -0.001(5) 0.004(8) C30 0.092(8) 0.134(10) 0.031(4) -0.021(5) 0.020(5) -0.041(7) C31 0.056(5) 0.094(7) 0.042(4) -0.018(4) 0.013(4) -0.001(5) C32 0.048(5) 0.100(8) 0.090(7) 0.022(6) 0.011(5) -0.007(5) C33 0.065(6) 0.104(8) 0.107(8) 0.002(7) 0.015(6) -0.030(6) C34 0.070(8) 0.150(12) 0.148(12) 0.047(10) -0.036(7) -0.029(8) C35 0.075(8) 0.237(17) 0.100(8) 0.079(10) -0.055(7) -0.067(10) O1 0.072(4) 0.068(4) 0.056(3) -0.001(3) 0.002(3) -0.026(3) O2 0.033(2) 0.081(4) 0.061(3) 0.015(3) -0.007(2) -0.008(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 Er1 N1 2.366(6) . ? Er1 O1 2.482(5) . ? Er1 C2 2.613(9) . ? Er1 C7 2.615(7) . ? Er1 C8 2.617(9) . ? Er1 C3 2.618(9) . ? Er1 C6 2.620(8) . ? Er1 C4 2.624(10) . ? Er1 C5 2.634(11) . ? Er1 C10 2.636(9) . ? Er1 C1 2.647(11) . ? Er1 C9 2.649(9) . ? Er1 S1 2.8799(18) . ? Er1 C15 2.930(7) . ? Er2 N2 2.369(6) . ? Er2 O2 2.424(5) . ? Er2 C31 2.602(8) . ? Er2 C27 2.605(7) . ? Er2 C30 2.606(8) . ? Er2 C24 2.607(9) . ? Er2 C25 2.616(9) . ? Er2 C29 2.618(8) . ? Er2 C28 2.629(7) . ? Er2 C26 2.644(8) . ? Er2 C22 2.652(8) . ? Er2 C23 2.663(8) . ? Er2 S1 2.938(2) . ? Er2 C15 2.977(7) . ? S1 C15 1.722(7) . ? N1 C15 1.329(8) . ? N1 C16 1.379(9) . ? N2 C15 1.335(9) . ? N2 C21 1.378(9) . ? C1 C5 1.33(2) . ? C1 C2 1.43(2) . ? C2 C3 1.398(18) . ? C3 C4 1.266(16) . ? C4 C5 1.328(19) . ? C6 C7 1.363(12) . ? C6 C10 1.397(15) . ? C7 C8 1.343(13) . ? C8 C9 1.397(16) . ? C9 C10 1.370(16) . ? C11 O1 1.439(8) . ? C11 C12 1.489(9) . ? C12 C13 1.486(8) . ? C13 C14 1.497(9) . ? C14 O1 1.422(8) . ? C16 C17 1.396(10) . ? C16 C21 1.398(10) . ? C17 C18 1.380(12) . ? C18 C19 1.371(12) . ? C19 C20 1.383(11) . ? C20 C21 1.390(10) . ? C22 C26 1.350(14) . ? C22 C23 1.387(14) . ? C23 C24 1.362(15) . ? C24 C25 1.388(18) . ? C25 C26 1.417(17) . ? C27 C28 1.359(12) . ? C27 C31 1.397(13) . ? C28 C29 1.361(15) . ? C29 C30 1.381(16) . ? C30 C31 1.377(14) . ? C32 O2 1.436(7) . ? C32 C33 1.500(8) . ? C33 C34 1.494(9) . ? C34 C35 1.487(8) . ? C35 O2 1.433(7) . ? 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 N1 Er1 O1 137.54(19) . . ? N1 Er1 C2 78.1(4) . . ? O1 Er1 C2 125.4(3) . . ? N1 Er1 C7 105.1(3) . . ? O1 Er1 C7 108.6(3) . . ? C2 Er1 C7 91.2(5) . . ? N1 Er1 C8 77.4(3) . . ? O1 Er1 C8 126.2(3) . . ? C2 Er1 C8 96.0(5) . . ? C7 Er1 C8 29.7(3) . . ? N1 Er1 C3 108.4(4) . . ? O1 Er1 C3 103.8(4) . . ? C2 Er1 C3 31.0(4) . . ? C7 Er1 C3 77.1(4) . . ? C8 Er1 C3 95.9(4) . . ? N1 Er1 C6 125.4(3) . . ? O1 Er1 C6 79.6(3) . . ? C2 Er1 C6 115.5(5) . . ? C7 Er1 C6 30.2(3) . . ? C8 Er1 C6 49.9(3) . . ? C3 Er1 C6 91.8(4) . . ? N1 Er1 C4 123.9(3) . . ? O1 Er1 C4 77.9(4) . . ? C2 Er1 C4 49.3(4) . . ? C7 Er1 C4 95.3(5) . . ? C8 Er1 C4 120.3(5) . . ? C3 Er1 C4 27.9(4) . . ? C6 Er1 C4 97.5(4) . . ? N1 Er1 C5 104.4(5) . . ? O1 Er1 C5 77.5(4) . . ? C2 Er1 C5 50.3(4) . . ? C7 Er1 C5 123.6(4) . . ? C8 Er1 C5 143.3(4) . . ? C3 Er1 C5 48.2(4) . . ? C6 Er1 C5 125.3(5) . . ? C4 Er1 C5 29.3(4) . . ? N1 Er1 C10 106.5(4) . . ? O1 Er1 C10 77.5(3) . . ? C2 Er1 C10 141.3(5) . . ? C7 Er1 C10 50.1(3) . . ? C8 Er1 C10 50.2(4) . . ? C3 Er1 C10 122.4(4) . . ? C6 Er1 C10 30.8(3) . . ? C4 Er1 C10 125.9(5) . . ? C5 Er1 C10 148.9(6) . . ? N1 Er1 C1 77.2(4) . . ? O1 Er1 C1 104.8(5) . . ? C2 Er1 C1 31.6(5) . . ? C7 Er1 C1 122.3(4) . . ? C8 Er1 C1 125.4(6) . . ? C3 Er1 C1 49.7(4) . . ? C6 Er1 C1 141.4(4) . . ? C4 Er1 C1 48.3(4) . . ? C5 Er1 C1 29.3(4) . . ? C10 Er1 C1 171.9(4) . . ? N1 Er1 C9 78.1(3) . . ? O1 Er1 C9 104.9(4) . . ? C2 Er1 C9 125.4(5) . . ? C7 Er1 C9 49.9(3) . . ? C8 Er1 C9 30.8(3) . . ? C3 Er1 C9 125.3(4) . . ? C6 Er1 C9 50.2(3) . . ? C4 Er1 C9 144.7(5) . . ? C5 Er1 C9 173.4(4) . . ? C10 Er1 C9 30.0(4) . . ? C1 Er1 C9 150.0(6) . . ? N1 Er1 S1 60.48(14) . . ? O1 Er1 S1 77.21(14) . . ? C2 Er1 S1 120.6(5) . . ? C7 Er1 S1 137.3(2) . . ? C8 Er1 S1 112.5(3) . . ? C3 Er1 S1 144.3(3) . . ? C6 Er1 S1 122.9(2) . . ? C4 Er1 S1 126.8(4) . . ? C5 Er1 S1 99.2(3) . . ? C10 Er1 S1 93.0(3) . . ? C1 Er1 S1 95.1(3) . . ? C9 Er1 S1 87.4(2) . . ? N1 Er1 C15 26.42(19) . . ? O1 Er1 C15 111.64(19) . . ? C2 Er1 C15 99.7(4) . . ? C7 Er1 C15 119.8(3) . . ? C8 Er1 C15 90.1(3) . . ? C3 Er1 C15 130.6(4) . . ? C6 Er1 C15 126.9(3) . . ? C4 Er1 C15 135.3(4) . . ? C5 Er1 C15 107.7(4) . . ? C10 Er1 C15 98.6(4) . . ? C1 Er1 C15 87.9(3) . . ? C9 Er1 C15 77.3(3) . . ? S1 Er1 C15 34.47(14) . . ? N2 Er2 O2 132.81(19) . . ? N2 Er2 C31 81.8(3) . . ? O2 Er2 C31 104.8(2) . . ? N2 Er2 C27 78.8(2) . . ? O2 Er2 C27 129.2(2) . . ? C31 Er2 C27 31.1(3) . . ? N2 Er2 C30 111.5(3) . . ? O2 Er2 C30 78.9(3) . . ? C31 Er2 C30 30.7(3) . . ? C27 Er2 C30 50.5(3) . . ? N2 Er2 C24 85.2(4) . . ? O2 Er2 C24 123.1(4) . . ? C31 Er2 C24 124.0(4) . . ? C27 Er2 C24 92.9(4) . . ? C30 Er2 C24 131.7(4) . . ? N2 Er2 C25 115.9(4) . . ? O2 Er2 C25 96.9(4) . . ? C31 Er2 C25 127.9(4) . . ? C27 Er2 C25 101.0(4) . . ? C30 Er2 C25 116.3(5) . . ? C24 Er2 C25 30.8(4) . . ? N2 Er2 C29 127.9(3) . . ? O2 Er2 C29 85.0(3) . . ? C31 Er2 C29 50.6(4) . . ? C27 Er2 C29 49.8(3) . . ? C30 Er2 C29 30.6(3) . . ? C24 Er2 C29 103.3(5) . . ? C25 Er2 C29 85.9(5) . . ? N2 Er2 C28 105.7(3) . . ? O2 Er2 C28 114.5(3) . . ? C31 Er2 C28 50.7(3) . . ? C27 Er2 C28 30.1(3) . . ? C30 Er2 C28 50.4(4) . . ? C24 Er2 C28 81.9(4) . . ? C25 Er2 C28 77.2(4) . . ? C29 Er2 C28 30.1(3) . . ? N2 Er2 C26 119.8(3) . . ? O2 Er2 C26 72.9(3) . . ? C31 Er2 C26 153.4(4) . . ? C27 Er2 C26 131.8(3) . . ? C30 Er2 C26 128.0(4) . . ? C24 Er2 C26 50.3(4) . . ? C25 Er2 C26 31.3(4) . . ? C29 Er2 C26 103.2(4) . . ? C28 Er2 C26 105.2(4) . . ? N2 Er2 C22 92.4(3) . . ? O2 Er2 C22 82.7(3) . . ? C31 Er2 C22 172.5(3) . . ? C27 Er2 C22 143.0(3) . . ? C30 Er2 C22 155.9(4) . . ? C24 Er2 C22 50.3(4) . . ? C25 Er2 C22 50.7(4) . . ? C29 Er2 C22 132.5(4) . . ? C28 Er2 C22 127.3(3) . . ? C26 Er2 C22 29.5(3) . . ? N2 Er2 C23 71.7(3) . . ? O2 Er2 C23 112.9(3) . . ? C31 Er2 C23 142.3(3) . . ? C27 Er2 C23 115.0(3) . . ? C30 Er2 C23 161.5(4) . . ? C24 Er2 C23 29.9(3) . . ? C25 Er2 C23 50.1(4) . . ? C29 Er2 C23 132.8(4) . . ? C28 Er2 C23 111.1(4) . . ? C26 Er2 C23 49.2(4) . . ? C22 Er2 C23 30.3(3) . . ? N2 Er2 S1 59.44(14) . . ? O2 Er2 S1 75.01(13) . . ? C31 Er2 S1 82.1(2) . . ? C27 Er2 S1 106.6(2) . . ? C30 Er2 S1 90.9(3) . . ? C24 Er2 S1 133.9(4) . . ? C25 Er2 S1 149.9(3) . . ? C29 Er2 S1 121.4(3) . . ? C28 Er2 S1 132.8(2) . . ? C26 Er2 S1 121.3(3) . . ? C22 Er2 S1 99.2(2) . . ? C23 Er2 S1 105.6(3) . . ? N2 Er2 C15 25.85(19) . . ? O2 Er2 C15 107.27(18) . . ? C31 Er2 C15 83.6(3) . . ? C27 Er2 C15 93.6(2) . . ? C30 Er2 C15 106.9(3) . . ? C24 Er2 C15 105.6(4) . . ? C25 Er2 C15 133.7(4) . . ? C29 Er2 C15 134.0(3) . . ? C28 Er2 C15 123.5(3) . . ? C26 Er2 C15 122.7(3) . . ? C22 Er2 C15 93.3(3) . . ? C23 Er2 C15 83.9(3) . . ? S1 Er2 C15 33.85(14) . . ? C15 S1 Er1 74.4(2) . . ? C15 S1 Er2 74.3(2) . . ? Er1 S1 Er2 138.97(7) . . ? C15 N1 C16 104.1(6) . . ? C15 N1 Er1 101.2(5) . . ? C16 N1 Er1 148.6(5) . . ? C15 N2 C21 103.9(6) . . ? C15 N2 Er2 103.4(4) . . ? C21 N2 Er2 148.3(5) . . ? C5 C1 C2 107.4(12) . . ? C5 C1 Er1 74.8(7) . . ? C2 C1 Er1 72.9(6) . . ? C3 C2 C1 102.7(12) . . ? C3 C2 Er1 74.7(6) . . ? C1 C2 Er1 75.5(6) . . ? C4 C3 C2 110.0(12) . . ? C4 C3 Er1 76.3(7) . . ? C2 C3 Er1 74.3(6) . . ? C3 C4 C5 111.4(13) . . ? C3 C4 Er1 75.8(7) . . ? C5 C4 Er1 75.8(7) . . ? C4 C5 C1 108.3(13) . . ? C4 C5 Er1 74.9(7) . . ? C1 C5 Er1 75.9(8) . . ? C7 C6 C10 107.4(10) . . ? C7 C6 Er1 74.7(5) . . ? C10 C6 Er1 75.2(5) . . ? C8 C7 C6 109.3(10) . . ? C8 C7 Er1 75.2(5) . . ? C6 C7 Er1 75.1(4) . . ? C7 C8 C9 108.4(10) . . ? C7 C8 Er1 75.0(5) . . ? C9 C8 Er1 75.9(5) . . ? C10 C9 C8 107.2(9) . . ? C10 C9 Er1 74.5(5) . . ? C8 C9 Er1 73.4(5) . . ? C9 C10 C6 107.7(9) . . ? C9 C10 Er1 75.5(5) . . ? C6 C10 Er1 74.0(5) . . ? O1 C11 C12 108.4(8) . . ? C13 C12 C11 105.1(8) . . ? C12 C13 C14 106.2(8) . . ? O1 C14 C13 107.7(8) . . ? N1 C15 N2 115.8(6) . . ? N1 C15 S1 122.3(6) . . ? N2 C15 S1 121.7(5) . . ? N1 C15 Er1 52.4(4) . . ? N2 C15 Er1 159.6(5) . . ? S1 C15 Er1 71.2(2) . . ? N1 C15 Er2 160.6(5) . . ? N2 C15 Er2 50.7(3) . . ? S1 C15 Er2 71.8(2) . . ? Er1 C15 Er2 134.6(3) . . ? N1 C16 C17 130.6(7) . . ? N1 C16 C21 108.1(6) . . ? C17 C16 C21 121.3(7) . . ? C18 C17 C16 116.9(8) . . ? C19 C18 C17 122.4(8) . . ? C18 C19 C20 121.0(8) . . ? C19 C20 C21 118.3(8) . . ? N2 C21 C20 131.7(7) . . ? N2 C21 C16 108.2(6) . . ? C20 C21 C16 120.1(7) . . ? C26 C22 C23 107.6(10) . . ? C26 C22 Er2 74.9(5) . . ? C23 C22 Er2 75.3(5) . . ? C24 C23 C22 108.7(11) . . ? C24 C23 Er2 72.7(5) . . ? C22 C23 Er2 74.4(5) . . ? C23 C24 C25 108.9(11) . . ? C23 C24 Er2 77.3(5) . . ? C25 C24 Er2 74.9(6) . . ? C24 C25 C26 105.5(11) . . ? C24 C25 Er2 74.2(6) . . ? C26 C25 Er2 75.5(5) . . ? C22 C26 C25 109.2(11) . . ? C22 C26 Er2 75.6(5) . . ? C25 C26 Er2 73.3(5) . . ? C28 C27 C31 108.8(9) . . ? C28 C27 Er2 75.9(5) . . ? C31 C27 Er2 74.3(5) . . ? C27 C28 C29 108.0(10) . . ? C27 C28 Er2 74.0(4) . . ? C29 C28 Er2 74.5(5) . . ? C28 C29 C30 108.8(11) . . ? C28 C29 Er2 75.4(5) . . ? C30 C29 Er2 74.2(5) . . ? C31 C30 C29 107.9(11) . . ? C31 C30 Er2 74.5(4) . . ? C29 C30 Er2 75.2(5) . . ? C30 C31 C27 106.6(10) . . ? C30 C31 Er2 74.8(5) . . ? C27 C31 Er2 74.6(5) . . ? O2 C32 C33 106.3(7) . . ? C34 C33 C32 104.6(7) . . ? C35 C34 C33 105.6(7) . . ? O2 C35 C34 108.6(7) . . ? C14 O1 C11 109.4(7) . . ? C14 O1 Er1 126.0(5) . . ? C11 O1 Er1 124.2(5) . . ? C35 O2 C32 108.1(6) . . ? C35 O2 Er2 126.7(5) . . ? C32 O2 Er2 123.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.605 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.128 # Attachment '8.cif' data_f70511b _database_code_depnum_ccdc_archive 'CCDC 762747' #TrackingRef '8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40 N2 O2 S Y2' _chemical_formula_weight 730.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.356(3) _cell_length_b 17.880(6) _cell_length_c 19.923(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3333(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 872 _cell_measurement_theta_min 2.661 _cell_measurement_theta_max 21.505 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 3.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4147 _exptl_absorpt_correction_T_max 0.7638 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15358 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6504 _reflns_number_gt 4681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU was used to restrain some abnormal ADPs. CONN was used to tune the generation of the connectivity table. ; _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^)+(0.0200P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.023(8) _refine_ls_number_reflns 6504 _refine_ls_number_parameters 379 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 1.07649(6) 0.84469(3) 0.18348(2) 0.04323(15) Uani 1 1 d . . . Y2 Y 0.95460(5) 1.07516(3) 0.01113(2) 0.03851(14) Uani 1 1 d . . . S1 S 0.99979(15) 0.92098(8) 0.06002(7) 0.0475(4) Uani 1 1 d . . . N1 N 1.2157(5) 0.9489(3) 0.1459(2) 0.0488(12) Uani 1 1 d . . . N2 N 1.1623(5) 1.0444(3) 0.0757(2) 0.0471(12) Uani 1 1 d . . . C1 C 1.3143(14) 0.7831(7) 0.1357(7) 0.113(4) Uani 1 1 d . . . H1A H 1.3727 0.8029 0.0990 0.136 Uiso 1 1 calc R . . C2 C 1.3377(10) 0.7948(6) 0.2027(9) 0.118(4) Uani 1 1 d . . . H2A H 1.4173 0.8229 0.2223 0.141 Uiso 1 1 calc R . . C3 C 1.2495(14) 0.7441(7) 0.2364(5) 0.106(4) Uani 1 1 d . . . H3A H 1.2558 0.7329 0.2845 0.127 Uiso 1 1 calc R . . C4 C 1.1735(11) 0.7053(5) 0.1931(9) 0.111(4) Uani 1 1 d . . . H4A H 1.1160 0.6609 0.2033 0.133 Uiso 1 1 calc R . . C5 C 1.2137(15) 0.7287(7) 0.1301(5) 0.111(4) Uani 1 1 d . . . H5A H 1.1869 0.7039 0.0881 0.133 Uiso 1 1 calc R . . C6 C 0.9120(8) 0.8443(4) 0.2911(3) 0.0729(19) Uani 1 1 d . . . H6A H 0.8584 0.8010 0.3077 0.088 Uiso 1 1 calc R . . C7 C 1.0417(8) 0.8661(4) 0.3136(3) 0.0688(18) Uani 1 1 d . . . H7A H 1.0964 0.8411 0.3491 0.083 Uiso 1 1 calc R . . C8 C 1.0709(9) 0.9345(4) 0.2882(3) 0.0746(19) Uani 1 1 d . . . H8A H 1.1507 0.9662 0.3025 0.090 Uiso 1 1 calc R . . C9 C 0.9580(12) 0.9585(4) 0.2500(4) 0.092(3) Uani 1 1 d . . . H9A H 0.9439 1.0093 0.2327 0.110 Uiso 1 1 calc R . . C10 C 0.8554(8) 0.9014(6) 0.2509(4) 0.091(3) Uani 1 1 d . . . H10A H 0.7566 0.9051 0.2348 0.110 Uiso 1 1 calc R . . C11 C 0.7798(10) 0.7242(5) 0.1820(4) 0.125(3) Uani 1 1 d DU . . H11A H 0.7200 0.7563 0.2094 0.150 Uiso 1 1 calc R . . H11B H 0.8366 0.6931 0.2116 0.150 Uiso 1 1 calc R . . C12 C 0.6892(11) 0.6766(5) 0.1388(4) 0.125(4) Uani 1 1 d D . . H12A H 0.7209 0.6250 0.1404 0.149 Uiso 1 1 calc R . . H12B H 0.5901 0.6789 0.1530 0.149 Uiso 1 1 calc R . . C13 C 0.7061(11) 0.7075(6) 0.0707(5) 0.133(4) Uani 1 1 d D . . H13A H 0.6221 0.7359 0.0580 0.160 Uiso 1 1 calc R . . H13B H 0.7201 0.6676 0.0384 0.160 Uiso 1 1 calc R . . C14 C 0.8329(10) 0.7564(5) 0.0733(4) 0.114(3) Uani 1 1 d D . . H14A H 0.9115 0.7330 0.0495 0.136 Uiso 1 1 calc R . . H14B H 0.8118 0.8036 0.0516 0.136 Uiso 1 1 calc R . . C15 C 1.1364(6) 0.9734(3) 0.0952(3) 0.0428(13) Uani 1 1 d . . . C16 C 1.3023(6) 1.0084(3) 0.1621(3) 0.0488(14) Uani 1 1 d . . . C17 C 1.4071(7) 1.0164(4) 0.2117(3) 0.0630(17) Uani 1 1 d . . . H17A H 1.4299 0.9771 0.2404 0.076 Uiso 1 1 calc R . . C18 C 1.4756(7) 1.0845(4) 0.2165(3) 0.0698(18) Uani 1 1 d . . . H18A H 1.5460 1.0911 0.2489 0.084 Uiso 1 1 calc R . . C19 C 1.4424(7) 1.1419(4) 0.1751(3) 0.0736(19) Uani 1 1 d . . . H19A H 1.4894 1.1873 0.1803 0.088 Uiso 1 1 calc R . . C20 C 1.3399(7) 1.1347(4) 0.1249(3) 0.0658(19) Uani 1 1 d . . . H20A H 1.3201 1.1741 0.0958 0.079 Uiso 1 1 calc R . . C21 C 1.2694(6) 1.0681(3) 0.1195(2) 0.0474(14) Uani 1 1 d . . . C22 C 0.8169(9) 1.1331(4) 0.1176(4) 0.075(2) Uani 1 1 d . . . H22A H 0.7690 1.1039 0.1526 0.090 Uiso 1 1 calc R . . C23 C 0.9544(10) 1.1605(5) 0.1215(4) 0.087(2) Uani 1 1 d . . . H23A H 1.0189 1.1549 0.1599 0.104 Uiso 1 1 calc R . . C24 C 0.9759(13) 1.2069(5) 0.0678(6) 0.107(3) Uani 1 1 d . . . H24A H 1.0573 1.2409 0.0627 0.129 Uiso 1 1 calc R . . C25 C 0.8516(14) 1.2108(5) 0.0313(5) 0.110(3) Uani 1 1 d . . . H25A H 0.8296 1.2477 -0.0035 0.132 Uiso 1 1 calc R . . C26 C 0.7521(9) 1.1623(5) 0.0627(5) 0.090(3) Uani 1 1 d . . . H26A H 0.6498 1.1593 0.0525 0.108 Uiso 1 1 calc R . . C27 C 1.1592(7) 1.1021(4) -0.0756(3) 0.0656(19) Uani 1 1 d . . . H27A H 1.2559 1.1183 -0.0637 0.079 Uiso 1 1 calc R . . C28 C 1.0529(10) 1.1484(5) -0.0943(3) 0.082(2) Uani 1 1 d . . . H28A H 1.0604 1.2029 -0.0980 0.098 Uiso 1 1 calc R . . C29 C 0.9408(10) 1.1056(7) -0.1185(3) 0.101(3) Uani 1 1 d . . . H29A H 0.8567 1.1247 -0.1423 0.121 Uiso 1 1 calc R . . C30 C 0.9819(9) 1.0293(6) -0.1138(3) 0.084(3) Uani 1 1 d . . . H30A H 0.9324 0.9868 -0.1344 0.101 Uiso 1 1 calc R . . C31 C 1.1194(7) 1.0287(5) -0.0869(3) 0.070(2) Uani 1 1 d . . . H31A H 1.1832 0.9853 -0.0851 0.083 Uiso 1 1 calc R . . C32 C 0.6423(7) 0.9805(4) 0.0470(3) 0.082(2) Uani 1 1 d D . . H32A H 0.6049 1.0193 0.0761 0.099 Uiso 1 1 calc R . . H32B H 0.7011 0.9471 0.0737 0.099 Uiso 1 1 calc R . . C33 C 0.5228(8) 0.9382(4) 0.0150(4) 0.094(2) Uani 1 1 d D . . H33A H 0.5490 0.8863 0.0077 0.113 Uiso 1 1 calc R . . H33B H 0.4373 0.9401 0.0425 0.113 Uiso 1 1 calc R . . C34 C 0.5010(9) 0.9774(6) -0.0491(5) 0.134(4) Uani 1 1 d D . . H34A H 0.4200 1.0110 -0.0460 0.161 Uiso 1 1 calc R . . H34B H 0.4831 0.9417 -0.0848 0.161 Uiso 1 1 calc R . . C35 C 0.6341(8) 1.0201(6) -0.0627(4) 0.123(4) Uani 1 1 d D . . H35A H 0.6811 1.0005 -0.1024 0.148 Uiso 1 1 calc R . . H35B H 0.6118 1.0723 -0.0705 0.148 Uiso 1 1 calc R . . O1 O 0.8722(5) 0.7690(2) 0.1408(2) 0.0736(13) Uani 1 1 d DU . . O2 O 0.7252(4) 1.0129(2) -0.0060(2) 0.0619(11) Uani 1 1 d 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 Y1 0.0478(3) 0.0446(3) 0.0373(3) 0.0057(3) 0.0022(3) 0.0057(3) Y2 0.0386(3) 0.0397(3) 0.0372(3) 0.0040(2) 0.0035(2) 0.0039(3) S1 0.0539(9) 0.0432(7) 0.0455(8) 0.0033(7) -0.0137(6) -0.0035(7) N1 0.049(3) 0.055(3) 0.043(3) 0.014(2) -0.007(2) -0.005(2) N2 0.048(3) 0.049(3) 0.045(3) 0.008(2) -0.011(2) -0.006(2) C1 0.099(8) 0.110(9) 0.131(10) 0.051(8) 0.056(8) 0.045(7) C2 0.059(6) 0.089(7) 0.205(13) -0.011(9) -0.031(7) 0.034(5) C3 0.119(9) 0.116(8) 0.083(6) 0.050(7) 0.016(6) 0.069(7) C4 0.090(7) 0.056(5) 0.186(13) 0.026(7) 0.014(8) 0.014(5) C5 0.134(10) 0.118(9) 0.081(7) -0.013(7) 0.004(7) 0.081(8) C6 0.076(5) 0.088(5) 0.055(4) 0.000(4) 0.020(4) -0.009(5) C7 0.074(5) 0.095(5) 0.037(3) 0.001(4) -0.007(4) 0.007(4) C8 0.083(5) 0.081(5) 0.059(4) -0.019(4) 0.010(4) -0.003(5) C9 0.144(9) 0.063(4) 0.069(5) -0.002(4) 0.038(6) 0.039(6) C10 0.056(5) 0.155(8) 0.064(5) -0.039(6) 0.005(4) 0.028(6) C11 0.137(7) 0.135(6) 0.102(6) 0.009(6) 0.007(6) -0.064(6) C12 0.156(10) 0.110(7) 0.108(7) -0.017(6) 0.023(7) -0.066(7) C13 0.155(10) 0.131(8) 0.114(8) 0.003(7) -0.034(7) -0.076(8) C14 0.141(9) 0.096(6) 0.104(7) 0.004(6) -0.018(6) -0.051(6) C15 0.045(3) 0.048(3) 0.036(3) 0.004(3) -0.001(2) 0.005(3) C16 0.039(3) 0.066(4) 0.041(3) 0.003(3) -0.004(3) -0.008(3) C17 0.051(4) 0.089(5) 0.049(3) 0.013(3) -0.003(3) -0.013(4) C18 0.047(4) 0.107(5) 0.055(4) -0.006(4) -0.004(3) -0.019(4) C19 0.060(4) 0.093(5) 0.068(4) -0.012(4) 0.001(4) -0.034(4) C20 0.070(4) 0.063(4) 0.065(4) 0.016(4) -0.004(3) -0.022(4) C21 0.046(3) 0.062(4) 0.034(3) -0.001(3) -0.001(2) -0.006(3) C22 0.072(5) 0.076(5) 0.077(5) -0.022(4) 0.027(4) 0.008(5) C23 0.087(6) 0.091(5) 0.081(5) -0.047(5) 0.012(5) 0.001(6) C24 0.115(9) 0.058(5) 0.148(9) -0.043(6) 0.040(8) -0.006(5) C25 0.136(10) 0.053(5) 0.141(9) 0.006(5) 0.018(8) 0.049(6) C26 0.063(5) 0.071(5) 0.136(8) -0.031(6) 0.015(5) 0.024(5) C27 0.052(4) 0.092(5) 0.053(4) 0.011(4) 0.012(3) -0.011(4) C28 0.086(6) 0.094(5) 0.065(4) 0.039(4) 0.012(4) 0.007(6) C29 0.078(6) 0.184(10) 0.041(4) 0.041(5) -0.005(4) 0.006(7) C30 0.086(6) 0.133(7) 0.035(4) -0.022(4) 0.017(4) -0.033(6) C31 0.056(5) 0.096(6) 0.056(4) -0.015(4) 0.020(3) 0.002(4) C32 0.060(5) 0.098(6) 0.088(5) 0.023(5) 0.008(4) -0.019(4) C33 0.081(5) 0.103(6) 0.098(6) -0.009(5) 0.018(5) -0.038(5) C34 0.079(7) 0.166(9) 0.157(9) 0.065(8) -0.050(6) -0.037(6) C35 0.075(6) 0.198(10) 0.096(6) 0.060(7) -0.044(5) -0.052(7) O1 0.088(3) 0.069(3) 0.064(3) 0.002(2) 0.009(3) -0.029(3) O2 0.038(2) 0.082(3) 0.065(3) 0.020(2) -0.009(2) -0.005(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 Y1 N1 2.394(4) . ? Y1 O1 2.492(4) . ? Y1 C2 2.630(8) . ? Y1 C8 2.634(6) . ? Y1 C6 2.638(6) . ? Y1 C3 2.640(7) . ? Y1 C7 2.641(6) . ? Y1 C1 2.659(9) . ? Y1 C4 2.659(7) . ? Y1 C5 2.660(8) . ? Y1 C10 2.667(7) . ? Y1 C9 2.669(6) . ? Y1 S1 2.9028(16) . ? Y1 C15 2.949(5) . ? Y2 N2 2.394(4) . ? Y2 O2 2.442(4) . ? Y2 C24 2.620(7) . ? Y2 C31 2.622(6) . ? Y2 C27 2.623(6) . ? Y2 C30 2.633(6) . ? Y2 C28 2.640(6) . ? Y2 C25 2.641(7) . ? Y2 C29 2.643(6) . ? Y2 C26 2.660(7) . ? Y2 C23 2.676(6) . ? Y2 C22 2.689(6) . ? Y2 S1 2.9542(17) . ? Y2 C15 3.002(5) . ? S1 C15 1.733(6) . ? N1 C15 1.327(6) . ? N1 C16 1.375(7) . ? N2 C15 1.351(7) . ? N2 C21 1.395(7) . ? C1 C5 1.357(15) . ? C1 C2 1.368(14) . ? C2 C3 1.398(13) . ? C3 C4 1.316(12) . ? C4 C5 1.375(13) . ? C6 C7 1.351(9) . ? C6 C10 1.401(10) . ? C7 C8 1.353(9) . ? C8 C9 1.371(11) . ? C9 C10 1.402(11) . ? C11 O1 1.436(7) . ? C11 C12 1.477(8) . ? C12 C13 1.473(8) . ? C13 C14 1.474(8) . ? C14 O1 1.413(7) . ? C16 C21 1.398(7) . ? C16 C17 1.400(8) . ? C17 C18 1.378(8) . ? C18 C19 1.353(9) . ? C19 C20 1.391(9) . ? C20 C21 1.366(8) . ? C22 C26 1.355(10) . ? C22 C23 1.379(11) . ? C23 C24 1.369(11) . ? C24 C25 1.373(14) . ? C25 C26 1.417(12) . ? C27 C28 1.346(9) . ? C27 C31 1.382(10) . ? C28 C29 1.385(11) . ? C29 C30 1.420(11) . ? C30 C31 1.394(10) . ? C32 O2 1.432(6) . ? C32 C33 1.493(7) . ? C33 C34 1.472(7) . ? C34 C35 1.485(8) . ? C35 O2 1.421(6) . ? 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 N1 Y1 O1 137.18(16) . . ? N1 Y1 C2 78.7(3) . . ? O1 Y1 C2 125.3(2) . . ? N1 Y1 C8 77.5(2) . . ? O1 Y1 C8 125.9(2) . . ? C2 Y1 C8 96.3(4) . . ? N1 Y1 C6 125.0(2) . . ? O1 Y1 C6 80.1(2) . . ? C2 Y1 C6 115.0(4) . . ? C8 Y1 C6 49.2(2) . . ? N1 Y1 C3 108.8(4) . . ? O1 Y1 C3 103.7(4) . . ? C2 Y1 C3 30.8(3) . . ? C8 Y1 C3 96.4(3) . . ? C6 Y1 C3 91.8(3) . . ? N1 Y1 C7 105.2(2) . . ? O1 Y1 C7 108.6(2) . . ? C2 Y1 C7 91.2(4) . . ? C8 Y1 C7 29.72(19) . . ? C6 Y1 C7 29.7(2) . . ? C3 Y1 C7 77.4(3) . . ? N1 Y1 C1 75.8(3) . . ? O1 Y1 C1 107.1(4) . . ? C2 Y1 C1 30.0(3) . . ? C8 Y1 C1 123.6(4) . . ? C6 Y1 C1 141.0(3) . . ? C3 Y1 C1 49.3(3) . . ? C7 Y1 C1 121.0(4) . . ? N1 Y1 C4 124.5(2) . . ? O1 Y1 C4 77.1(3) . . ? C2 Y1 C4 49.8(3) . . ? C8 Y1 C4 121.4(4) . . ? C6 Y1 C4 97.9(3) . . ? C3 Y1 C4 28.8(3) . . ? C7 Y1 C4 96.1(4) . . ? C1 Y1 C4 49.6(3) . . ? N1 Y1 C5 102.7(4) . . ? O1 Y1 C5 79.1(4) . . ? C2 Y1 C5 49.1(3) . . ? C8 Y1 C5 143.3(3) . . ? C6 Y1 C5 127.2(4) . . ? C3 Y1 C5 48.1(3) . . ? C7 Y1 C5 124.4(3) . . ? C1 Y1 C5 29.6(3) . . ? C4 Y1 C5 30.0(3) . . ? N1 Y1 C10 106.5(3) . . ? O1 Y1 C10 77.5(2) . . ? C2 Y1 C10 141.0(4) . . ? C8 Y1 C10 49.7(2) . . ? C6 Y1 C10 30.6(2) . . ? C3 Y1 C10 122.2(3) . . ? C7 Y1 C10 49.8(2) . . ? C1 Y1 C10 170.7(4) . . ? C4 Y1 C10 125.8(3) . . ? C5 Y1 C10 150.7(5) . . ? N1 Y1 C9 77.7(2) . . ? O1 Y1 C9 105.3(3) . . ? C2 Y1 C9 124.9(4) . . ? C8 Y1 C9 30.0(2) . . ? C6 Y1 C9 50.0(2) . . ? C3 Y1 C9 125.2(3) . . ? C7 Y1 C9 49.6(2) . . ? C1 Y1 C9 147.3(5) . . ? C4 Y1 C9 145.1(4) . . ? C5 Y1 C9 173.2(3) . . ? C10 Y1 C9 30.5(2) . . ? N1 Y1 S1 60.23(11) . . ? O1 Y1 S1 77.08(11) . . ? C2 Y1 S1 120.8(4) . . ? C8 Y1 S1 112.32(19) . . ? C6 Y1 S1 123.05(19) . . ? C3 Y1 S1 144.1(2) . . ? C7 Y1 S1 137.18(16) . . ? C1 Y1 S1 95.7(3) . . ? C4 Y1 S1 125.9(4) . . ? C5 Y1 S1 98.4(2) . . ? C10 Y1 S1 93.2(2) . . ? C9 Y1 S1 87.68(18) . . ? N1 Y1 C15 26.21(15) . . ? O1 Y1 C15 111.47(15) . . ? C2 Y1 C15 100.1(4) . . ? C8 Y1 C15 90.0(2) . . ? C6 Y1 C15 126.7(2) . . ? C3 Y1 C15 130.8(3) . . ? C7 Y1 C15 119.73(19) . . ? C1 Y1 C15 87.2(2) . . ? C4 Y1 C15 135.2(3) . . ? C5 Y1 C15 106.1(4) . . ? C10 Y1 C15 98.7(3) . . ? C9 Y1 C15 77.30(19) . . ? S1 Y1 C15 34.43(11) . . ? N2 Y2 O2 133.13(14) . . ? N2 Y2 C24 85.0(3) . . ? O2 Y2 C24 122.5(3) . . ? N2 Y2 C31 81.4(2) . . ? O2 Y2 C31 105.6(2) . . ? C24 Y2 C31 124.1(3) . . ? N2 Y2 C27 78.7(2) . . ? O2 Y2 C27 129.28(19) . . ? C24 Y2 C27 93.6(3) . . ? C31 Y2 C27 30.6(2) . . ? N2 Y2 C30 111.0(2) . . ? O2 Y2 C30 79.1(2) . . ? C24 Y2 C30 132.8(4) . . ? C31 Y2 C30 30.8(2) . . ? C27 Y2 C30 50.5(2) . . ? N2 Y2 C28 105.0(2) . . ? O2 Y2 C28 114.9(2) . . ? C24 Y2 C28 82.6(3) . . ? C31 Y2 C28 50.2(3) . . ? C27 Y2 C28 29.6(2) . . ? C30 Y2 C28 50.8(3) . . ? N2 Y2 C25 115.2(3) . . ? O2 Y2 C25 96.9(3) . . ? C24 Y2 C25 30.3(3) . . ? C31 Y2 C25 128.2(3) . . ? C27 Y2 C25 101.4(3) . . ? C30 Y2 C25 117.7(3) . . ? C28 Y2 C25 78.1(3) . . ? N2 Y2 C29 127.7(2) . . ? O2 Y2 C29 85.1(2) . . ? C24 Y2 C29 103.9(4) . . ? C31 Y2 C29 50.7(3) . . ? C27 Y2 C29 49.8(3) . . ? C30 Y2 C29 31.2(2) . . ? C28 Y2 C29 30.4(2) . . ? C25 Y2 C29 86.7(3) . . ? N2 Y2 C26 120.3(3) . . ? O2 Y2 C26 72.3(2) . . ? C24 Y2 C26 50.3(3) . . ? C31 Y2 C26 153.1(3) . . ? C27 Y2 C26 131.8(3) . . ? C30 Y2 C26 128.1(3) . . ? C28 Y2 C26 105.4(3) . . ? C25 Y2 C26 31.0(3) . . ? C29 Y2 C26 102.8(3) . . ? N2 Y2 C23 72.0(2) . . ? O2 Y2 C23 112.0(2) . . ? C24 Y2 C23 29.9(2) . . ? C31 Y2 C23 142.4(3) . . ? C27 Y2 C23 115.9(3) . . ? C30 Y2 C23 162.6(3) . . ? C28 Y2 C23 111.8(3) . . ? C25 Y2 C23 49.5(3) . . ? C29 Y2 C23 133.3(3) . . ? C26 Y2 C23 49.3(3) . . ? N2 Y2 C22 93.1(2) . . ? O2 Y2 C22 82.2(2) . . ? C24 Y2 C22 49.5(3) . . ? C31 Y2 C22 172.2(2) . . ? C27 Y2 C22 143.0(2) . . ? C30 Y2 C22 155.8(3) . . ? C28 Y2 C22 127.1(3) . . ? C25 Y2 C22 49.6(3) . . ? C29 Y2 C22 131.9(3) . . ? C26 Y2 C22 29.3(2) . . ? C23 Y2 C22 29.8(2) . . ? N2 Y2 S1 59.50(11) . . ? O2 Y2 S1 75.29(10) . . ? C24 Y2 S1 133.3(3) . . ? C31 Y2 S1 82.30(18) . . ? C27 Y2 S1 106.52(17) . . ? C30 Y2 S1 90.4(2) . . ? C28 Y2 S1 132.47(18) . . ? C25 Y2 S1 149.2(2) . . ? C29 Y2 S1 121.4(3) . . ? C26 Y2 S1 121.4(2) . . ? C23 Y2 S1 105.1(2) . . ? C22 Y2 S1 99.66(18) . . ? N2 Y2 C15 26.00(14) . . ? O2 Y2 C15 107.42(14) . . ? C24 Y2 C15 105.2(3) . . ? C31 Y2 C15 83.7(2) . . ? C27 Y2 C15 93.8(2) . . ? C30 Y2 C15 106.5(2) . . ? C28 Y2 C15 123.2(2) . . ? C25 Y2 C15 132.7(3) . . ? C29 Y2 C15 134.3(2) . . ? C26 Y2 C15 122.9(3) . . ? C23 Y2 C15 83.6(2) . . ? C22 Y2 C15 93.7(2) . . ? S1 Y2 C15 33.81(11) . . ? C15 S1 Y1 74.26(18) . . ? C15 S1 Y2 74.61(18) . . ? Y1 S1 Y2 138.87(5) . . ? C15 N1 C16 104.7(4) . . ? C15 N1 Y1 101.0(4) . . ? C16 N1 Y1 148.1(4) . . ? C15 N2 C21 103.5(5) . . ? C15 N2 Y2 103.0(3) . . ? C21 N2 Y2 148.2(4) . . ? C5 C1 C2 107.5(10) . . ? C5 C1 Y1 75.3(6) . . ? C2 C1 Y1 73.8(5) . . ? C1 C2 C3 106.0(10) . . ? C1 C2 Y1 76.2(6) . . ? C3 C2 Y1 75.0(5) . . ? C4 C3 C2 110.2(9) . . ? C4 C3 Y1 76.5(5) . . ? C2 C3 Y1 74.2(4) . . ? C3 C4 C5 106.9(10) . . ? C3 C4 Y1 74.8(5) . . ? C5 C4 Y1 75.0(5) . . ? C1 C5 C4 109.4(11) . . ? C1 C5 Y1 75.2(6) . . ? C4 C5 Y1 75.0(5) . . ? C7 C6 C10 108.7(7) . . ? C7 C6 Y1 75.3(4) . . ? C10 C6 Y1 75.8(4) . . ? C6 C7 C8 108.5(7) . . ? C6 C7 Y1 75.0(3) . . ? C8 C7 Y1 74.8(4) . . ? C7 C8 C9 109.6(8) . . ? C7 C8 Y1 75.5(4) . . ? C9 C8 Y1 76.5(4) . . ? C8 C9 C10 107.0(7) . . ? C8 C9 Y1 73.6(4) . . ? C10 C9 Y1 74.7(4) . . ? C6 C10 C9 106.2(7) . . ? C6 C10 Y1 73.6(4) . . ? C9 C10 Y1 74.9(4) . . ? O1 C11 C12 109.5(6) . . ? C13 C12 C11 105.0(6) . . ? C12 C13 C14 106.1(7) . . ? O1 C14 C13 109.7(7) . . ? N1 C15 N2 115.4(5) . . ? N1 C15 S1 122.9(4) . . ? N2 C15 S1 121.6(4) . . ? N1 C15 Y1 52.8(3) . . ? N2 C15 Y1 160.0(4) . . ? S1 C15 Y1 71.31(19) . . ? N1 C15 Y2 160.2(4) . . ? N2 C15 Y2 51.0(3) . . ? S1 C15 Y2 71.58(18) . . ? Y1 C15 Y2 134.3(2) . . ? N1 C16 C21 108.6(5) . . ? N1 C16 C17 131.1(6) . . ? C21 C16 C17 120.3(5) . . ? C18 C17 C16 117.7(6) . . ? C19 C18 C17 121.4(6) . . ? C18 C19 C20 121.8(6) . . ? C21 C20 C19 118.0(6) . . ? C20 C21 N2 131.3(6) . . ? C20 C21 C16 120.8(5) . . ? N2 C21 C16 107.9(5) . . ? C26 C22 C23 109.0(8) . . ? C26 C22 Y2 74.1(4) . . ? C23 C22 Y2 74.6(4) . . ? C24 C23 C22 108.0(9) . . ? C24 C23 Y2 72.8(4) . . ? C22 C23 Y2 75.6(4) . . ? C23 C24 C25 108.6(9) . . ? C23 C24 Y2 77.3(4) . . ? C25 C24 Y2 75.7(5) . . ? C24 C25 C26 107.0(9) . . ? C24 C25 Y2 74.0(4) . . ? C26 C25 Y2 75.2(4) . . ? C22 C26 C25 107.4(9) . . ? C22 C26 Y2 76.5(4) . . ? C25 C26 Y2 73.8(4) . . ? C28 C27 C31 109.8(7) . . ? C28 C27 Y2 75.9(4) . . ? C31 C27 Y2 74.7(4) . . ? C27 C28 C29 108.5(7) . . ? C27 C28 Y2 74.5(4) . . ? C29 C28 Y2 74.9(4) . . ? C28 C29 C30 107.6(8) . . ? C28 C29 Y2 74.7(4) . . ? C30 C29 Y2 74.0(4) . . ? C31 C30 C29 106.4(8) . . ? C31 C30 Y2 74.2(4) . . ? C29 C30 Y2 74.8(4) . . ? C27 C31 C30 107.7(8) . . ? C27 C31 Y2 74.8(4) . . ? C30 C31 Y2 75.1(4) . . ? O2 C32 C33 107.2(5) . . ? C34 C33 C32 103.5(6) . . ? C33 C34 C35 106.7(6) . . ? O2 C35 C34 108.1(6) . . ? C14 O1 C11 107.3(6) . . ? C14 O1 Y1 127.7(4) . . ? C11 O1 Y1 124.7(4) . . ? C35 O2 C32 107.4(5) . . ? C35 O2 Y2 126.6(4) . . ? C32 O2 Y2 123.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.612 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.068 # Attachment '9.cif' data_f70511c _database_code_depnum_ccdc_archive 'CCDC 762748' #TrackingRef '9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H104 N8 O8 S4 Yb4' _chemical_formula_weight 2078.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.814(8) _cell_length_b 10.924(3) _cell_length_c 26.601(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.674(4) _cell_angle_gamma 90.00 _cell_volume 8066(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 962 _cell_measurement_theta_min 2.555 _cell_measurement_theta_max 23.901 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 4.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4498 _exptl_absorpt_correction_T_max 0.6478 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16656 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7070 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU and EADP was used to restrain some abnormal ADPs. ; _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^)+(0.0446P)^2^+13.7430P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7070 _refine_ls_number_parameters 451 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.061774(12) 0.54059(3) 0.289192(12) 0.03780(11) Uani 1 1 d D . . Yb2 Yb 0.033744(12) 0.74921(3) 0.187904(12) 0.03762(11) Uani 1 1 d D . . N1 N 0.1154(2) 0.6537(6) 0.3484(2) 0.0455(16) Uani 1 1 d . . . N2 N 0.1151(2) 0.7155(6) 0.4281(2) 0.0522(18) Uani 1 1 d . . . H2B H 0.1045 0.7338 0.4568 0.063 Uiso 1 1 calc R . . N3 N 0.0861(2) 0.6355(6) 0.1350(2) 0.0449(16) Uani 1 1 d . . . N4 N 0.1649(3) 0.5869(6) 0.1401(2) 0.0531(18) Uani 1 1 d . . . H4B H 0.1937 0.5732 0.1527 0.064 Uiso 1 1 calc R . . S1 S 0.03012(7) 0.6229(2) 0.38766(7) 0.0485(5) Uani 1 1 d . . . S2 S 0.13001(7) 0.6698(2) 0.22718(7) 0.0491(5) Uani 1 1 d D . . O1 O 0.02273(18) 0.5467(4) 0.21040(16) 0.0377(11) Uani 1 1 d D . . H1O H 0.0357(6) 0.5011(15) 0.1904(6) 0.057 Uiso 1 1 d D . . O2 O -0.03875(18) 0.7436(5) 0.22263(19) 0.0412(12) Uani 1 1 d D . . H2O H -0.0626(17) 0.784(7) 0.214(2) 0.062 Uiso 1 1 d D . . C1 C 0.0575(4) 0.3084(9) 0.3131(5) 0.074(3) Uani 1 1 d . . . H1A H 0.0297 0.2685 0.3269 0.089 Uiso 1 1 calc R . . C2 C 0.0672(4) 0.3078(8) 0.2638(4) 0.065(3) Uani 1 1 d . . . H2A H 0.0478 0.2676 0.2366 0.078 Uiso 1 1 calc R . . C3 C 0.1123(5) 0.3537(9) 0.2602(4) 0.081(3) Uani 1 1 d . . . H3A H 0.1301 0.3520 0.2296 0.097 Uiso 1 1 calc R . . C4 C 0.1316(4) 0.3831(9) 0.3064(5) 0.083(3) Uani 1 1 d . . . H4A H 0.1655 0.4028 0.3151 0.100 Uiso 1 1 calc R . . C5 C 0.0958(5) 0.3547(10) 0.3412(4) 0.082(3) Uani 1 1 d . . . H5A H 0.1009 0.3506 0.3780 0.098 Uiso 1 1 calc R . . C6 C 0.0896(3) 0.6702(8) 0.3880(3) 0.0435(19) Uani 1 1 d . . . C7 C 0.1627(3) 0.6885(7) 0.3643(3) 0.0438(19) Uani 1 1 d . . . C8 C 0.2057(3) 0.6893(9) 0.3389(3) 0.063(2) Uani 1 1 d . . . H8A H 0.2066 0.6647 0.3055 0.076 Uiso 1 1 calc R . . C9 C 0.2457(3) 0.7284(10) 0.3662(4) 0.075(3) Uani 1 1 d . . . H9A H 0.2747 0.7308 0.3507 0.090 Uiso 1 1 calc R . . C10 C 0.2455(3) 0.7647(10) 0.4158(4) 0.074(3) Uani 1 1 d . . . H10A H 0.2744 0.7875 0.4328 0.089 Uiso 1 1 calc R . . C11 C 0.2035(4) 0.7679(9) 0.4408(4) 0.073(3) Uani 1 1 d . . . H11A H 0.2028 0.7958 0.4738 0.088 Uiso 1 1 calc R . . C12 C 0.1634(3) 0.7275(8) 0.4140(3) 0.049(2) Uani 1 1 d . . . C13 C 0.0581(4) 0.9813(8) 0.1957(4) 0.062(2) Uani 1 1 d . . . H13A H 0.0733 1.0210 0.2257 0.075 Uiso 1 1 calc R . . C14 C 0.0075(4) 0.9824(8) 0.1807(4) 0.065(3) Uani 1 1 d . . . H14A H -0.0180 1.0221 0.1986 0.077 Uiso 1 1 calc R . . C15 C 0.0034(4) 0.9358(9) 0.1322(4) 0.079(3) Uani 1 1 d . . . H15A H -0.0261 0.9366 0.1100 0.094 Uiso 1 1 calc R . . C16 C 0.0498(4) 0.9058(9) 0.1170(4) 0.067(3) Uani 1 1 d . . . H16A H 0.0582 0.8863 0.0826 0.081 Uiso 1 1 calc R . . C17 C 0.0812(4) 0.9355(9) 0.1568(4) 0.068(3) Uani 1 1 d . . . H17A H 0.1163 0.9368 0.1550 0.082 Uiso 1 1 calc R . . C18 C 0.1280(3) 0.6261(8) 0.1651(3) 0.047(2) Uani 1 1 d . . . C19 C 0.1009(3) 0.6024(7) 0.0869(3) 0.0434(19) Uani 1 1 d . . . C20 C 0.0731(3) 0.5954(8) 0.0415(3) 0.056(2) Uani 1 1 d . . . H20A H 0.0403 0.6126 0.0391 0.067 Uiso 1 1 calc R . . C21 C 0.0977(4) 0.5609(9) -0.0003(3) 0.063(3) Uani 1 1 d . . . H21A H 0.0809 0.5564 -0.0316 0.076 Uiso 1 1 calc R . . C22 C 0.1463(5) 0.5333(9) 0.0032(4) 0.078(3) Uani 1 1 d . . . H22A H 0.1608 0.5097 -0.0258 0.094 Uiso 1 1 calc R . . C23 C 0.1742(3) 0.5392(9) 0.0477(4) 0.067(3) Uani 1 1 d . . . H23A H 0.2071 0.5230 0.0499 0.080 Uiso 1 1 calc R . . C24 C 0.1484(3) 0.5722(8) 0.0899(3) 0.054(2) Uani 1 1 d . . . C25 C 0.3032(5) 0.5571(15) 0.1575(5) 0.149(6) Uani 1 1 d D . . H25A H 0.3083 0.6375 0.1433 0.179 Uiso 1 1 calc R . . H25B H 0.3038 0.4966 0.1309 0.179 Uiso 1 1 calc R . . C26 C 0.3415(4) 0.5296(15) 0.1988(6) 0.131(6) Uani 1 1 d D . . H26A H 0.3549 0.4487 0.1944 0.158 Uiso 1 1 calc R . . H26B H 0.3673 0.5892 0.1987 0.158 Uiso 1 1 calc R . . C27 C 0.3166(6) 0.536(2) 0.2473(6) 0.207(10) Uani 1 1 d D . . H27A H 0.3292 0.4757 0.2712 0.248 Uiso 1 1 calc R . . H27B H 0.3200 0.6170 0.2624 0.248 Uiso 1 1 calc R . . C28 C 0.2652(5) 0.5101(18) 0.2307(5) 0.180(6) Uani 1 1 d DU . . H28A H 0.2589 0.4229 0.2321 0.215 Uiso 1 1 calc R . . H28B H 0.2437 0.5521 0.2522 0.215 Uiso 1 1 calc R . . C29 C 0.1044(4) 0.7622(11) 0.5726(4) 0.096(4) Uani 1 1 d D . . H29A H 0.1216 0.8331 0.5863 0.115 Uiso 1 1 calc R . . H29B H 0.1262 0.6930 0.5732 0.115 Uiso 1 1 calc R . . C30 C 0.0607(5) 0.7340(11) 0.6028(4) 0.099(4) Uani 1 1 d D . . H30A H 0.0639 0.6538 0.6183 0.119 Uiso 1 1 calc R . . H30B H 0.0577 0.7946 0.6291 0.119 Uiso 1 1 calc R . . C31 C 0.0177(5) 0.7375(14) 0.5664(5) 0.138(6) Uani 1 1 d D . . H31A H -0.0093 0.7778 0.5809 0.165 Uiso 1 1 calc R . . H31B H 0.0080 0.6557 0.5558 0.165 Uiso 1 1 calc R . . C32 C 0.0353(4) 0.8098(14) 0.5235(5) 0.120(5) Uani 1 1 d D . . H32A H 0.0186 0.7848 0.4920 0.143 Uiso 1 1 calc R . . H32B H 0.0297 0.8965 0.5284 0.143 Uiso 1 1 calc R . . O3 O 0.2587(3) 0.5529(12) 0.1808(4) 0.157(4) Uani 1 1 d DU . . O4 O 0.0853(3) 0.7858(8) 0.5225(2) 0.095(2) Uani 1 1 d D . . C35 C 0.2071(8) 0.906(5) 0.0358(9) 0.39(3) Uani 1 1 d D . . H35A H 0.2235 0.9791 0.0258 0.462 Uiso 1 1 calc R . . H35B H 0.2236 0.8350 0.0229 0.462 Uiso 1 1 calc R . . C36 C 0.1548(8) 0.907(4) 0.0157(9) 0.34(3) Uani 1 1 d D . . H36A H 0.1377 0.8388 0.0294 0.413 Uiso 1 1 calc R . . H36B H 0.1395 0.9824 0.0257 0.413 Uiso 1 1 calc R . . C33 C 0.2570(7) 0.870(3) 0.1142(12) 0.49(3) Uani 1 1 d D . . H33A H 0.2579 0.8711 0.1503 0.735 Uiso 1 1 calc R . . H33B H 0.2789 0.9304 0.1028 0.735 Uiso 1 1 calc R . . H33C H 0.2663 0.7906 0.1029 0.735 Uiso 1 1 calc R . . C38 C 0.1012(7) 0.915(3) -0.0623(12) 0.49(3) Uani 1 1 d D . . H38A H 0.1000 0.9084 -0.0983 0.735 Uiso 1 1 calc R . . H38B H 0.0899 0.9950 -0.0532 0.735 Uiso 1 1 calc R . . H38C H 0.0811 0.8537 -0.0488 0.735 Uiso 1 1 calc R . . C34 C 0.2065(7) 0.899(2) 0.0930(9) 0.40(3) Uani 1 1 d D . . H34A H 0.1959 0.9763 0.1062 0.482 Uiso 1 1 calc R . . H34B H 0.1844 0.8354 0.1026 0.482 Uiso 1 1 calc R . . C37 C 0.1525(8) 0.898(3) -0.0410(8) 0.36(3) Uani 1 1 d D . . H37A H 0.1644 0.8191 -0.0510 0.429 Uiso 1 1 calc R . . H37B H 0.1729 0.9610 -0.0545 0.429 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 Yb1 0.03627(19) 0.0453(2) 0.03133(17) 0.00047(15) -0.00164(13) 0.00400(15) Yb2 0.03698(19) 0.0439(2) 0.03196(18) 0.00318(15) 0.00237(14) -0.00158(15) N1 0.044(4) 0.058(4) 0.034(3) -0.008(3) -0.001(3) -0.001(3) N2 0.051(4) 0.072(5) 0.033(4) -0.004(3) -0.004(3) -0.001(4) N3 0.055(4) 0.050(4) 0.030(3) 0.002(3) 0.005(3) 0.001(3) N4 0.050(4) 0.063(5) 0.046(4) -0.001(3) 0.002(3) 0.006(3) S1 0.0381(11) 0.0724(15) 0.0348(10) 0.0050(10) -0.0004(9) -0.0015(10) S2 0.0388(11) 0.0694(14) 0.0387(11) -0.0023(10) 0.0009(9) -0.0061(10) O1 0.047(3) 0.041(3) 0.025(2) -0.001(2) 0.001(2) 0.002(2) O2 0.048(3) 0.042(3) 0.033(3) 0.002(2) 0.003(2) 0.008(2) C1 0.089(8) 0.052(6) 0.084(8) 0.015(6) 0.022(7) -0.002(5) C2 0.055(6) 0.051(6) 0.086(8) -0.008(5) -0.020(6) 0.009(5) C3 0.115(10) 0.056(6) 0.076(7) 0.006(6) 0.028(7) 0.033(6) C4 0.059(7) 0.063(7) 0.123(10) 0.004(7) -0.026(7) 0.028(5) C5 0.119(10) 0.076(8) 0.048(6) 0.006(5) -0.002(7) 0.034(7) C6 0.028(4) 0.066(5) 0.035(4) -0.003(4) -0.006(3) 0.003(4) C7 0.035(4) 0.052(5) 0.043(4) -0.002(4) -0.004(4) 0.001(4) C8 0.049(6) 0.086(7) 0.053(5) -0.008(5) -0.006(4) 0.002(5) C9 0.041(5) 0.126(10) 0.058(6) -0.002(6) 0.001(5) -0.005(6) C10 0.036(5) 0.105(9) 0.081(7) 0.002(6) -0.007(5) -0.012(5) C11 0.101(9) 0.073(7) 0.043(5) -0.008(5) -0.016(6) -0.017(6) C12 0.035(5) 0.066(6) 0.045(5) 0.005(4) -0.005(4) -0.002(4) C13 0.065(6) 0.053(6) 0.069(6) 0.000(5) 0.005(5) -0.013(5) C14 0.072(7) 0.043(5) 0.082(7) 0.016(5) 0.024(6) 0.009(4) C15 0.097(9) 0.051(6) 0.082(8) 0.029(6) -0.029(7) -0.009(6) C16 0.078(7) 0.065(6) 0.061(6) 0.006(5) 0.024(6) 0.001(5) C17 0.059(6) 0.064(6) 0.083(7) 0.025(6) 0.015(6) -0.004(5) C18 0.029(4) 0.071(6) 0.041(4) 0.003(4) 0.010(4) 0.000(4) C19 0.051(5) 0.045(5) 0.035(4) -0.002(4) 0.010(4) 0.001(4) C20 0.063(6) 0.064(6) 0.039(5) -0.007(4) -0.001(4) 0.000(5) C21 0.067(6) 0.089(7) 0.034(5) -0.003(5) 0.007(4) 0.006(5) C22 0.123(10) 0.067(7) 0.048(6) -0.012(5) 0.027(6) -0.005(7) C23 0.050(6) 0.089(7) 0.063(6) -0.014(6) 0.022(5) 0.001(5) C24 0.064(6) 0.056(6) 0.042(5) 0.002(4) 0.013(4) -0.004(4) C25 0.168(18) 0.143(15) 0.133(14) -0.016(11) -0.020(14) -0.010(13) C26 0.067(9) 0.133(13) 0.187(17) -0.010(12) -0.043(11) -0.001(8) C27 0.22(3) 0.25(3) 0.132(17) -0.011(17) -0.073(17) 0.00(2) C28 0.113(9) 0.323(15) 0.102(8) -0.014(11) 0.002(8) 0.068(10) C29 0.103(10) 0.096(9) 0.088(9) -0.011(7) 0.003(8) 0.011(7) C30 0.136(13) 0.101(10) 0.065(7) -0.004(7) 0.035(8) -0.004(8) C31 0.161(17) 0.128(14) 0.127(13) -0.003(10) 0.036(13) -0.029(11) C32 0.068(8) 0.192(16) 0.099(10) -0.017(10) 0.010(8) -0.006(9) O3 0.076(6) 0.298(14) 0.095(6) -0.006(8) -0.009(5) 0.073(7) O4 0.100(6) 0.127(7) 0.058(5) -0.012(4) 0.013(4) -0.014(5) C35 0.52(8) 0.25(4) 0.42(6) -0.07(5) 0.33(6) -0.04(6) C36 0.48(8) 0.19(3) 0.37(6) -0.09(4) 0.14(5) -0.12(5) C33 0.075(10) 0.33(3) 1.08(9) -0.12(4) 0.16(2) -0.006(15) C38 0.075(10) 0.33(3) 1.08(9) -0.12(4) 0.16(2) -0.006(15) C34 0.28(4) 0.15(2) 0.81(9) -0.14(4) 0.33(5) -0.08(2) C37 0.63(8) 0.16(2) 0.31(4) -0.01(3) 0.28(5) 0.00(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.299(4) . ? Yb1 O2 2.324(5) 2 ? Yb1 O1 2.352(5) 2 ? Yb1 N1 2.436(6) . ? Yb1 C5 2.601(10) . ? Yb1 C4 2.613(9) . ? Yb1 C1 2.620(10) . ? Yb1 C3 2.622(10) . ? Yb1 C2 2.639(9) . ? Yb1 S2 2.952(2) . ? Yb1 S1 2.956(2) . ? Yb1 C6 3.042(7) . ? Yb2 O2 2.272(5) . ? Yb2 O1 2.317(5) . ? Yb2 O2 2.376(5) 2 ? Yb2 N3 2.430(6) . ? Yb2 C17 2.591(9) . ? Yb2 C16 2.607(9) . ? Yb2 C15 2.627(9) . ? Yb2 C13 2.630(9) . ? Yb2 C14 2.653(9) . ? Yb2 S1 2.939(2) 2 ? Yb2 S2 2.942(2) . ? Yb2 C18 3.042(8) . ? N1 C6 1.326(9) . ? N1 C7 1.408(9) . ? N2 C6 1.337(9) . ? N2 C12 1.422(10) . ? N3 C18 1.376(9) . ? N3 C19 1.415(9) . ? N4 C18 1.329(9) . ? N4 C24 1.393(10) . ? S1 C6 1.732(8) . ? S1 Yb2 2.939(2) 2 ? S2 C18 1.716(8) . ? O1 Yb1 2.352(5) 2 ? O2 Yb1 2.324(5) 2 ? O2 Yb2 2.376(5) 2 ? C1 C2 1.357(14) . ? C1 C5 1.358(14) . ? C2 C3 1.359(14) . ? C3 C4 1.347(14) . ? C4 C5 1.438(15) . ? C7 C12 1.386(11) . ? C7 C8 1.411(11) . ? C8 C9 1.358(12) . ? C9 C10 1.377(14) . ? C10 C11 1.382(14) . ? C11 C12 1.361(12) . ? C13 C17 1.351(13) . ? C13 C14 1.437(13) . ? C14 C15 1.386(14) . ? C15 C16 1.414(14) . ? C16 C17 1.368(13) . ? C19 C24 1.361(11) . ? C19 C20 1.395(11) . ? C20 C21 1.393(11) . ? C21 C22 1.382(14) . ? C22 C23 1.374(13) . ? C23 C24 1.416(11) . ? C25 O3 1.421(9) . ? C25 C26 1.509(9) . ? C26 C27 1.504(9) . ? C27 C28 1.495(9) . ? C28 O3 1.407(9) . ? C29 O4 1.425(8) . ? C29 C30 1.531(9) . ? C30 C31 1.490(9) . ? C31 C32 1.497(9) . ? C32 O4 1.418(8) . ? C35 C36 1.519(7) . ? C35 C34 1.526(7) . ? C36 C37 1.508(7) . ? C33 C34 1.513(7) . ? C38 C37 1.513(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O2 74.86(17) . 2 ? O1 Yb1 O1 65.77(19) . 2 ? O2 Yb1 O1 72.94(17) 2 2 ? O1 Yb1 N1 144.0(2) . . ? O2 Yb1 N1 75.8(2) 2 . ? O1 Yb1 N1 123.63(19) 2 . ? O1 Yb1 C5 130.0(3) . . ? O2 Yb1 C5 154.8(3) 2 . ? O1 Yb1 C5 110.4(3) 2 . ? N1 Yb1 C5 82.3(3) . . ? O1 Yb1 C4 118.8(3) . . ? O2 Yb1 C4 147.9(3) 2 . ? O1 Yb1 C4 138.6(3) 2 . ? N1 Yb1 C4 78.6(3) . . ? C5 Yb1 C4 32.0(3) . . ? O1 Yb1 C1 102.9(3) . . ? O2 Yb1 C1 160.1(3) 2 . ? O1 Yb1 C1 88.0(3) 2 . ? N1 Yb1 C1 111.7(3) . . ? C5 Yb1 C1 30.2(3) . . ? C4 Yb1 C1 50.6(4) . . ? O1 Yb1 C3 89.2(3) . . ? O2 Yb1 C3 148.4(3) 2 . ? O1 Yb1 C3 125.3(3) 2 . ? N1 Yb1 C3 105.5(3) . . ? C5 Yb1 C3 50.6(3) . . ? C4 Yb1 C3 29.8(3) . . ? C1 Yb1 C3 49.5(3) . . ? O1 Yb1 C2 80.0(2) . . ? O2 Yb1 C2 154.8(2) 2 . ? O1 Yb1 C2 95.9(3) 2 . ? N1 Yb1 C2 127.7(3) . . ? C5 Yb1 C2 50.1(3) . . ? C4 Yb1 C2 49.9(3) . . ? C1 Yb1 C2 29.9(3) . . ? C3 Yb1 C2 29.9(3) . . ? O1 Yb1 S2 76.10(13) . . ? O2 Yb1 S2 69.49(13) 2 . ? O1 Yb1 S2 131.86(12) 2 . ? N1 Yb1 S2 74.29(16) . . ? C5 Yb1 S2 116.5(3) . . ? C4 Yb1 S2 85.1(3) . . ? C1 Yb1 S2 129.7(2) . . ? C3 Yb1 S2 80.3(3) . . ? C2 Yb1 S2 105.6(3) . . ? O1 Yb1 S1 130.45(13) . . ? O2 Yb1 S1 74.60(13) 2 . ? O1 Yb1 S1 68.46(11) 2 . ? N1 Yb1 S1 58.53(16) . . ? C5 Yb1 S1 83.4(2) . . ? C4 Yb1 S1 107.8(3) . . ? C1 Yb1 S1 93.4(3) . . ? C3 Yb1 S1 133.9(2) . . ? C2 Yb1 S1 123.1(3) . . ? S2 Yb1 S1 126.02(6) . . ? O1 Yb1 C6 148.60(19) . . ? O2 Yb1 C6 74.1(2) 2 . ? O1 Yb1 C6 100.47(18) 2 . ? N1 Yb1 C6 25.0(2) . . ? C5 Yb1 C6 80.8(3) . . ? C4 Yb1 C6 90.6(3) . . ? C1 Yb1 C6 104.7(3) . . ? C3 Yb1 C6 120.3(3) . . ? C2 Yb1 C6 130.9(3) . . ? S2 Yb1 C6 97.08(16) . . ? S1 Yb1 C6 33.54(14) . . ? O2 Yb2 O1 74.56(17) . . ? O2 Yb2 O2 65.7(2) . 2 ? O1 Yb2 O2 73.55(16) . 2 ? O2 Yb2 N3 143.3(2) . . ? O1 Yb2 N3 75.84(19) . . ? O2 Yb2 N3 124.6(2) 2 . ? O2 Yb2 C17 129.4(3) . . ? O1 Yb2 C17 155.7(3) . . ? O2 Yb2 C17 110.0(3) 2 . ? N3 Yb2 C17 83.1(3) . . ? O2 Yb2 C16 120.6(3) . . ? O1 Yb2 C16 147.7(3) . . ? O2 Yb2 C16 137.8(3) 2 . ? N3 Yb2 C16 77.3(3) . . ? C17 Yb2 C16 30.5(3) . . ? O2 Yb2 C15 89.4(3) . . ? O1 Yb2 C15 147.5(3) . . ? O2 Yb2 C15 125.5(3) 2 . ? N3 Yb2 C15 104.6(3) . . ? C17 Yb2 C15 50.3(3) . . ? C16 Yb2 C15 31.3(3) . . ? O2 Yb2 C13 103.0(3) . . ? O1 Yb2 C13 159.7(3) . . ? O2 Yb2 C13 87.0(3) 2 . ? N3 Yb2 C13 112.2(3) . . ? C17 Yb2 C13 30.0(3) . . ? C16 Yb2 C13 50.9(3) . . ? C15 Yb2 C13 50.8(3) . . ? O2 Yb2 C14 78.9(2) . . ? O1 Yb2 C14 153.5(2) . . ? O2 Yb2 C14 95.5(3) 2 . ? N3 Yb2 C14 128.4(3) . . ? C17 Yb2 C14 50.7(3) . . ? C16 Yb2 C14 51.4(3) . . ? C15 Yb2 C14 30.4(3) . . ? C13 Yb2 C14 31.6(3) . . ? O2 Yb2 S1 75.65(14) . 2 ? O1 Yb2 S1 69.18(12) . 2 ? O2 Yb2 S1 131.83(12) 2 2 ? N3 Yb2 S1 73.87(16) . 2 ? C17 Yb2 S1 116.6(3) . 2 ? C16 Yb2 S1 86.4(3) . 2 ? C15 Yb2 S1 79.6(2) . 2 ? C13 Yb2 S1 130.4(2) . 2 ? C14 Yb2 S1 104.5(2) . 2 ? O2 Yb2 S2 131.22(13) . . ? O1 Yb2 S2 76.07(13) . . ? O2 Yb2 S2 69.09(13) 2 . ? N3 Yb2 S2 59.31(15) . . ? C17 Yb2 S2 82.8(2) . . ? C16 Yb2 S2 104.9(3) . . ? C15 Yb2 S2 132.9(3) . . ? C13 Yb2 S2 91.9(2) . . ? C14 Yb2 S2 123.3(2) . . ? S1 Yb2 S2 126.94(6) 2 . ? O2 Yb2 C18 150.2(2) . . ? O1 Yb2 C18 76.1(2) . . ? O2 Yb2 C18 101.1(2) 2 . ? N3 Yb2 C18 26.20(19) . . ? C17 Yb2 C18 79.6(3) . . ? C16 Yb2 C18 87.5(3) . . ? C15 Yb2 C18 118.7(3) . . ? C13 Yb2 C18 102.8(3) . . ? C14 Yb2 C18 130.3(3) . . ? S1 Yb2 C18 98.46(16) 2 . ? S2 Yb2 C18 33.28(15) . . ? C6 N1 C7 105.5(6) . . ? C6 N1 Yb1 104.0(5) . . ? C7 N1 Yb1 148.6(5) . . ? C6 N2 C12 106.6(6) . . ? C18 N3 C19 102.9(6) . . ? C18 N3 Yb2 102.6(4) . . ? C19 N3 Yb2 150.9(5) . . ? C18 N4 C24 107.4(7) . . ? C6 S1 Yb2 113.5(3) . 2 ? C6 S1 Yb1 75.9(3) . . ? Yb2 S1 Yb1 74.82(5) 2 . ? C18 S2 Yb2 76.6(3) . . ? C18 S2 Yb1 115.0(3) . . ? Yb2 S2 Yb1 74.72(5) . . ? Yb1 O1 Yb2 101.58(18) . . ? Yb1 O1 Yb1 114.12(19) . 2 ? Yb2 O1 Yb1 100.20(18) . 2 ? Yb2 O2 Yb1 102.41(19) . 2 ? Yb2 O2 Yb2 114.2(2) . 2 ? Yb1 O2 Yb2 99.10(19) 2 2 ? C2 C1 C5 109.7(10) . . ? C2 C1 Yb1 75.8(6) . . ? C5 C1 Yb1 74.2(6) . . ? C1 C2 C3 107.9(10) . . ? C1 C2 Yb1 74.3(6) . . ? C3 C2 Yb1 74.4(6) . . ? C4 C3 C2 109.9(10) . . ? C4 C3 Yb1 74.7(6) . . ? C2 C3 Yb1 75.7(6) . . ? C3 C4 C5 106.4(10) . . ? C3 C4 Yb1 75.4(6) . . ? C5 C4 Yb1 73.5(6) . . ? C1 C5 C4 106.1(10) . . ? C1 C5 Yb1 75.7(6) . . ? C4 C5 Yb1 74.5(5) . . ? N1 C6 N2 113.4(7) . . ? N1 C6 S1 121.4(6) . . ? N2 C6 S1 124.9(6) . . ? N1 C6 Yb1 51.0(4) . . ? N2 C6 Yb1 162.5(6) . . ? S1 C6 Yb1 70.5(2) . . ? C12 C7 N1 108.9(7) . . ? C12 C7 C8 119.7(7) . . ? N1 C7 C8 131.4(7) . . ? C9 C8 C7 115.8(8) . . ? C8 C9 C10 123.4(10) . . ? C9 C10 C11 121.6(9) . . ? C12 C11 C10 115.4(9) . . ? C11 C12 C7 124.0(9) . . ? C11 C12 N2 130.4(8) . . ? C7 C12 N2 105.6(7) . . ? C17 C13 C14 107.1(9) . . ? C17 C13 Yb2 73.4(5) . . ? C14 C13 Yb2 75.1(5) . . ? C15 C14 C13 106.1(9) . . ? C15 C14 Yb2 73.8(5) . . ? C13 C14 Yb2 73.3(5) . . ? C14 C15 C16 109.2(10) . . ? C14 C15 Yb2 75.8(5) . . ? C16 C15 Yb2 73.5(5) . . ? C17 C16 C15 105.8(9) . . ? C17 C16 Yb2 74.1(5) . . ? C15 C16 Yb2 75.1(5) . . ? C13 C17 C16 111.7(9) . . ? C13 C17 Yb2 76.6(5) . . ? C16 C17 Yb2 75.4(6) . . ? N4 C18 N3 112.7(7) . . ? N4 C18 S2 126.3(6) . . ? N3 C18 S2 120.9(6) . . ? N4 C18 Yb2 161.0(6) . . ? N3 C18 Yb2 51.2(4) . . ? S2 C18 Yb2 70.2(3) . . ? C24 C19 C20 121.3(8) . . ? C24 C19 N3 110.3(7) . . ? C20 C19 N3 128.4(8) . . ? C21 C20 C19 115.7(8) . . ? C22 C21 C20 122.2(9) . . ? C23 C22 C21 122.9(9) . . ? C22 C23 C24 114.2(9) . . ? C19 C24 N4 106.7(7) . . ? C19 C24 C23 123.6(8) . . ? N4 C24 C23 129.6(9) . . ? O3 C25 C26 105.6(9) . . ? C27 C26 C25 105.8(10) . . ? C28 C27 C26 102.8(11) . . ? O3 C28 C27 106.1(11) . . ? O4 C29 C30 105.5(8) . . ? C31 C30 C29 106.5(8) . . ? C30 C31 C32 102.8(9) . . ? O4 C32 C31 106.6(9) . . ? C28 O3 C25 111.0(9) . . ? C32 O4 C29 108.9(8) . . ? C36 C35 C34 106.3(10) . . ? C37 C36 C35 109.2(10) . . ? C33 C34 C35 108.2(10) . . ? C36 C37 C38 110.0(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B O4 0.86 1.95 2.804(10) 174.7 . N4 H4B O3 0.86 1.93 2.785(11) 176.6 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.965 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.135 # Attachment '10.cif' data_f61106a _database_code_depnum_ccdc_archive 'CCDC 762749' #TrackingRef '10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H76 Er4 N8 O8 S4' _chemical_formula_weight 1882.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.815(9) _cell_length_b 10.978(3) _cell_length_c 26.611(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.602(4) _cell_angle_gamma 90.00 _cell_volume 8110(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1012 _cell_measurement_theta_min 3.015 _cell_measurement_theta_max 26.941 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 4.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6296 _exptl_absorpt_correction_T_max 0.6760 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16547 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7126 _reflns_number_gt 5512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. Data were SQEEZEd due to presence of a disordered THF. The THF molecule (O4, etc) is modeled isotropically due to severe disorder. ; _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^)+(0.0426P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7126 _refine_ls_number_parameters 378 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.561969(9) 0.53909(3) 0.289392(9) 0.03679(9) Uani 1 1 d D . . Er2 Er 0.466022(9) 0.74993(2) 0.312337(9) 0.03689(9) Uani 1 1 d D . . S1 S 0.53087(5) 0.62399(16) 0.38780(5) 0.0471(4) Uani 1 1 d . . . S2 S 0.37000(5) 0.66840(17) 0.27346(5) 0.0489(4) Uani 1 1 d . . . O1 O 0.52320(12) 0.5451(4) 0.21065(12) 0.0351(8) Uani 1 1 d D . . H1O H 0.5363(14) 0.510(5) 0.1877(8) 0.053 Uiso 1 1 d D . . O2 O 0.53944(13) 0.7433(3) 0.27704(13) 0.0371(9) Uani 1 1 d D . . H2O H 0.5602(6) 0.7912(17) 0.2885(12) 0.056 Uiso 1 1 d D . . N1 N 0.61646(16) 0.6542(5) 0.34855(17) 0.0450(12) Uani 1 1 d . . . N2 N 0.61647(18) 0.7168(5) 0.42803(17) 0.0495(13) Uani 1 1 d . . . H2B H 0.6060 0.7345 0.4569 0.059 Uiso 1 1 calc R . . N3 N 0.41286(16) 0.6351(5) 0.36549(17) 0.0444(12) Uani 1 1 d . . . N4 N 0.33477(17) 0.5862(5) 0.36104(19) 0.0519(14) Uani 1 1 d . . . H4B H 0.3060 0.5730 0.3486 0.062 Uiso 1 1 calc R . . C1 C 0.5578(3) 0.3064(7) 0.3136(4) 0.073(2) Uani 1 1 d . . . H1A H 0.5300 0.2659 0.3273 0.087 Uiso 1 1 calc R . . C2 C 0.5685(3) 0.3063(7) 0.2637(3) 0.066(2) Uani 1 1 d . . . H2A H 0.5490 0.2669 0.2363 0.080 Uiso 1 1 calc R . . C3 C 0.6120(3) 0.3512(7) 0.2597(3) 0.077(2) Uani 1 1 d . . . H3A H 0.6304 0.3483 0.2295 0.092 Uiso 1 1 calc R . . C4 C 0.6305(3) 0.3793(8) 0.3081(4) 0.091(3) Uani 1 1 d . . . H4A H 0.6643 0.3990 0.3174 0.110 Uiso 1 1 calc R . . C5 C 0.5964(4) 0.3514(8) 0.3415(3) 0.086(3) Uani 1 1 d . . . H5A H 0.6017 0.3471 0.3782 0.103 Uiso 1 1 calc R . . C6 C 0.5900(2) 0.6715(6) 0.3879(2) 0.0431(14) Uani 1 1 d . . . C7 C 0.6633(2) 0.6902(6) 0.3647(2) 0.0486(16) Uani 1 1 d . . . C8 C 0.6631(2) 0.7293(6) 0.4143(2) 0.0498(16) Uani 1 1 d . . . C9 C 0.7050(3) 0.7676(7) 0.4410(3) 0.069(2) Uani 1 1 d . . . H9A H 0.7049 0.7929 0.4743 0.083 Uiso 1 1 calc R . . C10 C 0.7465(3) 0.7663(8) 0.4158(3) 0.078(2) Uani 1 1 d . . . H10A H 0.7752 0.7915 0.4325 0.093 Uiso 1 1 calc R . . C11 C 0.7468(3) 0.7291(8) 0.3670(3) 0.078(2) Uani 1 1 d . . . H11A H 0.7758 0.7298 0.3514 0.094 Uiso 1 1 calc R . . C12 C 0.7053(2) 0.6900(7) 0.3392(3) 0.0641(19) Uani 1 1 d . . . H12A H 0.7058 0.6655 0.3058 0.077 Uiso 1 1 calc R . . C13 C 0.4423(3) 0.9845(7) 0.3051(3) 0.065(2) Uani 1 1 d . . . H13A H 0.4279 1.0252 0.2750 0.078 Uiso 1 1 calc R . . C14 C 0.4915(3) 0.9838(7) 0.3207(3) 0.072(2) Uani 1 1 d . . . H14A H 0.5171 1.0231 0.3030 0.087 Uiso 1 1 calc R . . C15 C 0.4963(3) 0.9360(7) 0.3684(3) 0.072(2) Uani 1 1 d . . . H15A H 0.5258 0.9375 0.3905 0.087 Uiso 1 1 calc R . . C16 C 0.4509(4) 0.9083(7) 0.3831(3) 0.075(2) Uani 1 1 d . . . H16A H 0.4431 0.8878 0.4176 0.090 Uiso 1 1 calc R . . C17 C 0.4175(3) 0.9378(7) 0.3444(3) 0.069(2) Uani 1 1 d . . . H17A H 0.3826 0.9411 0.3469 0.082 Uiso 1 1 calc R . . C18 C 0.3726(2) 0.6247(6) 0.3351(2) 0.0459(15) Uani 1 1 d . . . C19 C 0.3993(2) 0.6012(6) 0.4136(2) 0.0426(14) Uani 1 1 d . . . C20 C 0.4257(2) 0.5939(7) 0.4589(2) 0.0580(18) Uani 1 1 d . . . H20A H 0.4585 0.6118 0.4614 0.070 Uiso 1 1 calc R . . C21 C 0.4020(3) 0.5592(7) 0.5006(2) 0.066(2) Uani 1 1 d . . . H21A H 0.4193 0.5531 0.5316 0.079 Uiso 1 1 calc R . . C22 C 0.3537(3) 0.5335(7) 0.4976(3) 0.066(2) Uani 1 1 d . . . H22A H 0.3389 0.5118 0.5267 0.080 Uiso 1 1 calc R . . C23 C 0.3268(2) 0.5387(7) 0.4532(3) 0.0635(19) Uani 1 1 d . . . H23A H 0.2941 0.5209 0.4510 0.076 Uiso 1 1 calc R . . C24 C 0.3508(2) 0.5720(6) 0.4111(2) 0.0484(16) Uani 1 1 d . . . O3 O 0.5840(2) 0.7854(6) 0.5222(2) 0.0930(19) Uani 1 1 d . . . C25 C 0.6025(3) 0.7600(8) 0.5713(3) 0.092(3) Uani 1 1 d . . . H25A H 0.6200 0.8301 0.5852 0.110 Uiso 1 1 calc R . . H25B H 0.6245 0.6915 0.5711 0.110 Uiso 1 1 calc R . . C26 C 0.5614(5) 0.7305(9) 0.6025(4) 0.114(4) Uani 1 1 d . . . H26A H 0.5649 0.6498 0.6171 0.137 Uiso 1 1 calc R . . H26B H 0.5588 0.7895 0.6293 0.137 Uiso 1 1 calc R . . C27 C 0.5196(5) 0.7363(12) 0.5668(6) 0.144(5) Uani 1 1 d . . . H27A H 0.5092 0.6551 0.5568 0.173 Uiso 1 1 calc R . . H27B H 0.4931 0.7776 0.5816 0.173 Uiso 1 1 calc R . . C28 C 0.5345(4) 0.8021(13) 0.5248(4) 0.125(4) Uani 1 1 d . . . H28A H 0.5176 0.7729 0.4942 0.150 Uiso 1 1 calc R . . H28B H 0.5273 0.8880 0.5286 0.150 Uiso 1 1 calc R . . O4 O 0.2426(3) 0.5504(7) 0.3185(3) 0.133(3) Uiso 1 1 d D . . C29 C 0.1979(4) 0.5561(12) 0.3414(4) 0.153(5) Uiso 1 1 d D . . H29A H 0.1926 0.6373 0.3544 0.183 Uiso 1 1 calc R . . H29B H 0.1974 0.4985 0.3690 0.183 Uiso 1 1 calc R . . C30 C 0.1595(4) 0.5244(12) 0.3007(4) 0.135(4) Uiso 1 1 d D . . H30A H 0.1485 0.4411 0.3040 0.162 Uiso 1 1 calc R . . H30B H 0.1321 0.5790 0.3014 0.162 Uiso 1 1 calc R . . C31 C 0.1850(4) 0.5407(13) 0.2548(5) 0.177(6) Uiso 1 1 d D . . H31A H 0.1816 0.6238 0.2427 0.213 Uiso 1 1 calc R . . H31B H 0.1723 0.4859 0.2286 0.213 Uiso 1 1 calc R . . C32 C 0.2376(5) 0.5117(14) 0.2693(5) 0.205(7) Uiso 1 1 d D . . H32A H 0.2439 0.4252 0.2666 0.246 Uiso 1 1 calc R . . H32B H 0.2589 0.5560 0.2483 0.246 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03746(15) 0.04270(17) 0.02945(14) 0.00036(12) -0.00375(10) 0.00378(12) Er2 0.03793(15) 0.04252(17) 0.02999(14) -0.00295(12) 0.00024(11) 0.00175(11) S1 0.0424(8) 0.0665(11) 0.0317(7) 0.0049(7) -0.0028(6) 0.0012(8) S2 0.0418(8) 0.0686(12) 0.0358(8) 0.0017(8) -0.0011(6) 0.0045(8) O1 0.037(2) 0.041(2) 0.0281(19) 0.0016(18) 0.0011(16) -0.0011(17) O2 0.037(2) 0.039(2) 0.035(2) -0.0055(18) -0.0018(17) -0.0055(17) N1 0.042(3) 0.055(4) 0.038(3) -0.004(2) -0.004(2) -0.001(2) N2 0.059(3) 0.063(4) 0.025(2) -0.008(2) -0.004(2) -0.001(3) N3 0.040(3) 0.058(4) 0.034(3) 0.002(2) -0.003(2) 0.002(2) N4 0.038(3) 0.065(4) 0.053(3) -0.003(3) 0.006(2) -0.006(2) C1 0.078(6) 0.048(5) 0.094(6) 0.016(5) 0.015(5) 0.009(4) C2 0.076(5) 0.049(5) 0.071(5) -0.012(4) -0.023(4) 0.017(4) C3 0.086(6) 0.062(6) 0.085(6) 0.008(4) 0.031(5) 0.029(5) C4 0.063(5) 0.062(6) 0.143(9) -0.007(6) -0.039(6) 0.024(4) C5 0.138(9) 0.065(6) 0.053(5) 0.011(4) -0.015(5) 0.038(6) C6 0.048(3) 0.054(4) 0.026(3) 0.000(3) -0.006(3) 0.004(3) C7 0.044(4) 0.054(4) 0.046(4) 0.003(3) -0.008(3) 0.000(3) C8 0.057(4) 0.054(4) 0.037(3) -0.001(3) -0.006(3) -0.008(3) C9 0.076(5) 0.076(6) 0.052(4) -0.009(4) -0.015(4) -0.014(4) C10 0.054(5) 0.097(7) 0.079(6) -0.003(5) -0.018(4) -0.022(4) C11 0.043(4) 0.113(7) 0.077(6) -0.003(5) -0.007(4) -0.012(4) C12 0.042(4) 0.087(6) 0.063(4) -0.005(4) 0.000(3) -0.003(4) C13 0.086(6) 0.049(5) 0.060(5) -0.006(4) 0.001(4) 0.014(4) C14 0.078(6) 0.049(5) 0.093(6) -0.014(4) 0.028(5) -0.005(4) C15 0.080(6) 0.060(5) 0.073(5) -0.028(4) -0.023(4) -0.001(4) C16 0.123(7) 0.055(5) 0.049(4) -0.019(4) 0.015(5) 0.003(5) C17 0.069(5) 0.053(5) 0.085(6) -0.024(4) 0.017(4) 0.005(4) C18 0.044(3) 0.054(4) 0.041(3) 0.000(3) 0.008(3) 0.001(3) C19 0.045(3) 0.052(4) 0.032(3) 0.000(3) 0.005(3) 0.005(3) C20 0.059(4) 0.072(5) 0.043(4) 0.003(3) 0.002(3) -0.003(4) C21 0.081(5) 0.078(6) 0.039(4) 0.007(4) 0.003(4) -0.004(4) C22 0.083(5) 0.071(5) 0.048(4) 0.011(4) 0.022(4) 0.001(4) C23 0.054(4) 0.083(6) 0.055(4) 0.007(4) 0.015(3) -0.008(4) C24 0.046(4) 0.055(4) 0.045(4) 0.004(3) 0.013(3) 0.002(3) O3 0.083(4) 0.139(6) 0.059(3) -0.024(3) 0.019(3) -0.011(4) C25 0.110(7) 0.091(7) 0.074(6) -0.018(5) 0.002(5) 0.009(5) C26 0.184(12) 0.093(8) 0.070(6) -0.003(5) 0.043(8) 0.005(8) C27 0.129(11) 0.140(12) 0.167(14) 0.013(10) 0.046(10) -0.017(8) C28 0.114(9) 0.170(12) 0.091(8) -0.023(8) 0.006(7) 0.001(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.297(3) . ? Er1 O2 2.345(4) . ? Er1 O1 2.370(3) 2_655 ? Er1 N1 2.464(5) . ? Er1 C4 2.616(7) . ? Er1 C5 2.631(7) . ? Er1 C3 2.637(7) . ? Er1 C1 2.639(8) . ? Er1 C2 2.655(7) . ? Er1 S1 2.9597(17) . ? Er1 S2 2.9650(17) 2_655 ? Er1 Er2 3.6093(8) 2_655 ? Er2 O2 2.302(4) . ? Er2 O1 2.354(4) 2_655 ? Er2 O2 2.375(4) 2_655 ? Er2 N3 2.458(5) . ? Er2 C16 2.617(7) . ? Er2 C17 2.635(7) . ? Er2 C15 2.636(7) . ? Er2 C13 2.663(7) . ? Er2 C14 2.669(7) . ? Er2 S2 2.9424(17) . ? Er2 S1 2.9568(16) . ? Er2 Er1 3.6093(8) 2_655 ? S1 C6 1.727(6) . ? S2 C18 1.705(6) . ? S2 Er1 2.9650(17) 2_655 ? O1 Er2 2.354(4) 2_655 ? O1 Er1 2.370(3) 2_655 ? O2 Er2 2.375(4) 2_655 ? N1 C6 1.330(7) . ? N1 C7 1.403(7) . ? N2 C6 1.352(7) . ? N2 C8 1.377(8) . ? N3 C18 1.344(7) . ? N3 C19 1.406(7) . ? N4 C18 1.363(7) . ? N4 C24 1.388(8) . ? C1 C5 1.360(11) . ? C1 C2 1.381(11) . ? C2 C3 1.318(10) . ? C3 C4 1.392(11) . ? C4 C5 1.374(12) . ? C7 C12 1.388(8) . ? C7 C8 1.388(8) . ? C8 C9 1.390(9) . ? C9 C10 1.371(10) . ? C10 C11 1.363(11) . ? C11 C12 1.399(9) . ? C13 C17 1.386(10) . ? C13 C14 1.403(10) . ? C14 C15 1.372(10) . ? C15 C16 1.381(11) . ? C16 C17 1.382(11) . ? C19 C20 1.374(8) . ? C19 C24 1.384(8) . ? C20 C21 1.381(9) . ? C21 C22 1.371(10) . ? C22 C23 1.361(9) . ? C23 C24 1.387(8) . ? O3 C28 1.396(11) . ? O3 C25 1.401(10) . ? C25 C26 1.491(13) . ? C26 C27 1.456(15) . ? C27 C28 1.413(14) . ? O4 C32 1.375(12) . ? O4 C29 1.421(11) . ? C29 C30 1.515(12) . ? C30 C31 1.460(12) . ? C31 C32 1.523(13) . ? 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 Er1 O2 74.85(13) . . ? O1 Er1 O1 65.59(14) . 2_655 ? O2 Er1 O1 73.44(13) . 2_655 ? O1 Er1 N1 143.40(15) . . ? O2 Er1 N1 75.37(14) . . ? O1 Er1 N1 124.10(14) 2_655 . ? O1 Er1 C4 119.2(3) . . ? O2 Er1 C4 148.5(2) . . ? O1 Er1 C4 137.4(2) 2_655 . ? N1 Er1 C4 79.1(2) . . ? O1 Er1 C5 129.7(2) . . ? O2 Er1 C5 155.2(2) . . ? O1 Er1 C5 110.7(3) 2_655 . ? N1 Er1 C5 82.9(2) . . ? C4 Er1 C5 30.4(3) . . ? O1 Er1 C3 88.6(2) . . ? O2 Er1 C3 147.9(2) . . ? O1 Er1 C3 124.6(2) 2_655 . ? N1 Er1 C3 106.1(2) . . ? C4 Er1 C3 30.7(2) . . ? C5 Er1 C3 50.5(2) . . ? O1 Er1 C1 103.0(2) . . ? O2 Er1 C1 160.73(19) . . ? O1 Er1 C1 88.1(2) 2_655 . ? N1 Er1 C1 112.0(2) . . ? C4 Er1 C1 49.2(3) . . ? C5 Er1 C1 29.9(2) . . ? C3 Er1 C1 49.3(2) . . ? O1 Er1 C2 80.10(18) . . ? O2 Er1 C2 154.95(18) . . ? O1 Er1 C2 96.4(2) 2_655 . ? N1 Er1 C2 127.54(19) . . ? C4 Er1 C2 48.9(2) . . ? C5 Er1 C2 49.7(2) . . ? C3 Er1 C2 28.8(2) . . ? C1 Er1 C2 30.2(2) . . ? O1 Er1 S1 130.67(9) . . ? O2 Er1 S1 74.49(9) . . ? O1 Er1 S1 69.14(9) 2_655 . ? N1 Er1 S1 58.36(11) . . ? C4 Er1 S1 107.0(3) . . ? C5 Er1 S1 84.11(19) . . ? C3 Er1 S1 134.46(19) . . ? C1 Er1 S1 93.9(2) . . ? C2 Er1 S1 124.03(19) . . ? O1 Er1 S2 75.60(10) . 2_655 ? O2 Er1 S2 68.76(10) . 2_655 ? O1 Er1 S2 131.28(9) 2_655 2_655 ? N1 Er1 S2 74.10(12) . 2_655 ? C4 Er1 S2 86.9(3) . 2_655 ? C5 Er1 S2 116.6(3) . 2_655 ? C3 Er1 S2 80.68(19) . 2_655 ? C1 Er1 S2 129.86(18) . 2_655 ? C2 Er1 S2 105.0(2) . 2_655 ? S1 Er1 S2 125.50(5) . 2_655 ? O1 Er1 Er2 39.68(10) . 2_655 ? O2 Er1 Er2 40.43(9) . 2_655 ? O1 Er1 Er2 79.24(9) 2_655 2_655 ? N1 Er1 Er2 104.20(12) . 2_655 ? C4 Er1 Er2 133.9(3) . 2_655 ? C5 Er1 Er2 162.2(2) . 2_655 ? C3 Er1 Er2 111.72(18) . 2_655 ? C1 Er1 Er2 142.5(2) . 2_655 ? C2 Er1 Er2 116.03(17) . 2_655 ? S1 Er1 Er2 113.61(4) . 2_655 ? S2 Er1 Er2 52.06(3) 2_655 2_655 ? O2 Er2 O1 74.52(12) . 2_655 ? O2 Er2 O2 65.98(14) . 2_655 ? O1 Er2 O2 73.25(12) 2_655 2_655 ? O2 Er2 N3 143.12(15) . . ? O1 Er2 N3 75.56(14) 2_655 . ? O2 Er2 N3 123.90(14) 2_655 . ? O2 Er2 C16 120.1(2) . . ? O1 Er2 C16 148.3(2) 2_655 . ? O2 Er2 C16 137.6(2) 2_655 . ? N3 Er2 C16 78.3(2) . . ? O2 Er2 C17 129.9(2) . . ? O1 Er2 C17 155.19(19) 2_655 . ? O2 Er2 C17 110.3(2) 2_655 . ? N3 Er2 C17 82.9(2) . . ? C16 Er2 C17 30.5(2) . . ? O2 Er2 C15 89.7(2) . . ? O1 Er2 C15 147.74(19) 2_655 . ? O2 Er2 C15 126.0(2) 2_655 . ? N3 Er2 C15 104.7(2) . . ? C16 Er2 C15 30.5(2) . . ? C17 Er2 C15 50.4(2) . . ? O2 Er2 C13 102.9(2) . . ? O1 Er2 C13 160.06(18) 2_655 . ? O2 Er2 C13 87.55(18) 2_655 . ? N3 Er2 C13 112.5(2) . . ? C16 Er2 C13 50.1(2) . . ? C17 Er2 C13 30.3(2) . . ? C15 Er2 C13 50.2(2) . . ? O2 Er2 C14 80.03(19) . . ? O1 Er2 C14 154.55(19) 2_655 . ? O2 Er2 C14 96.5(2) 2_655 . ? N3 Er2 C14 127.7(2) . . ? C16 Er2 C14 49.8(3) . . ? C17 Er2 C14 50.1(2) . . ? C15 Er2 C14 30.0(2) . . ? C13 Er2 C14 30.5(2) . . ? O2 Er2 S2 130.99(9) . . ? O1 Er2 S2 75.27(9) 2_655 . ? O2 Er2 S2 68.84(9) 2_655 . ? N3 Er2 S2 58.71(11) . . ? C16 Er2 S2 105.8(2) . . ? C17 Er2 S2 83.12(18) . . ? C15 Er2 S2 133.28(18) . . ? C13 Er2 S2 93.08(18) . . ? C14 Er2 S2 123.51(19) . . ? O2 Er2 S1 75.13(10) . . ? O1 Er2 S1 69.37(9) 2_655 . ? O2 Er2 S1 131.59(9) 2_655 . ? N3 Er2 S1 74.49(11) . . ? C16 Er2 S1 86.6(2) . . ? C17 Er2 S1 116.68(19) . . ? C15 Er2 S1 79.53(18) . . ? C13 Er2 S1 129.73(17) . . ? C14 Er2 S1 104.2(2) . . ? S2 Er2 S1 126.73(5) . . ? O2 Er2 Er1 80.15(9) . 2_655 ? O1 Er2 Er1 38.53(8) 2_655 2_655 ? O2 Er2 Er1 39.83(9) 2_655 2_655 ? N3 Er2 Er1 89.62(11) . 2_655 ? C16 Er2 Er1 158.3(2) . 2_655 ? C17 Er2 Er1 130.84(18) . 2_655 ? C15 Er2 Er1 165.3(2) . 2_655 ? C13 Er2 Er1 121.69(16) . 2_655 ? C14 Er2 Er1 136.30(19) . 2_655 ? S2 Er2 Er1 52.62(3) . 2_655 ? S1 Er2 Er1 107.65(4) . 2_655 ? C6 S1 Er2 113.6(2) . . ? C6 S1 Er1 76.41(19) . . ? Er2 S1 Er1 75.29(4) . . ? C18 S2 Er2 76.4(2) . . ? C18 S2 Er1 114.6(2) . 2_655 ? Er2 S2 Er1 75.32(4) . 2_655 ? Er1 O1 Er2 101.79(14) . 2_655 ? Er1 O1 Er1 114.31(14) . 2_655 ? Er2 O1 Er1 99.80(13) 2_655 2_655 ? Er2 O2 Er1 102.07(14) . . ? Er2 O2 Er2 113.89(14) . 2_655 ? Er1 O2 Er2 99.74(13) . 2_655 ? C6 N1 C7 105.5(5) . . ? C6 N1 Er1 103.2(4) . . ? C7 N1 Er1 149.6(4) . . ? C6 N2 C8 107.6(5) . . ? C18 N3 C19 105.4(5) . . ? C18 N3 Er2 101.8(4) . . ? C19 N3 Er2 149.8(4) . . ? C18 N4 C24 108.0(5) . . ? C5 C1 C2 108.4(8) . . ? C5 C1 Er1 74.7(5) . . ? C2 C1 Er1 75.5(4) . . ? C3 C2 C1 109.3(7) . . ? C3 C2 Er1 74.8(5) . . ? C1 C2 Er1 74.2(4) . . ? C2 C3 C4 107.3(8) . . ? C2 C3 Er1 76.3(4) . . ? C4 C3 Er1 73.8(4) . . ? C5 C4 C3 108.6(8) . . ? C5 C4 Er1 75.5(4) . . ? C3 C4 Er1 75.5(4) . . ? C1 C5 C4 106.4(8) . . ? C1 C5 Er1 75.4(5) . . ? C4 C5 Er1 74.2(5) . . ? N1 C6 N2 112.0(5) . . ? N1 C6 S1 121.9(4) . . ? N2 C6 S1 125.7(4) . . ? C12 C7 C8 121.3(6) . . ? C12 C7 N1 130.0(6) . . ? C8 C7 N1 108.7(5) . . ? N2 C8 C7 106.3(5) . . ? N2 C8 C9 132.0(6) . . ? C7 C8 C9 121.7(6) . . ? C10 C9 C8 116.9(7) . . ? C11 C10 C9 121.6(7) . . ? C10 C11 C12 122.8(7) . . ? C7 C12 C11 115.6(7) . . ? C17 C13 C14 107.2(7) . . ? C17 C13 Er2 73.7(4) . . ? C14 C13 Er2 75.0(4) . . ? C15 C14 C13 108.2(7) . . ? C15 C14 Er2 73.7(4) . . ? C13 C14 Er2 74.5(4) . . ? C14 C15 C16 108.0(7) . . ? C14 C15 Er2 76.3(4) . . ? C16 C15 Er2 74.0(4) . . ? C15 C16 C17 108.6(7) . . ? C15 C16 Er2 75.5(4) . . ? C17 C16 Er2 75.5(4) . . ? C16 C17 C13 107.9(7) . . ? C16 C17 Er2 74.0(4) . . ? C13 C17 Er2 75.9(4) . . ? N3 C18 N4 111.2(5) . . ? N3 C18 S2 122.6(4) . . ? N4 C18 S2 125.9(5) . . ? C20 C19 C24 119.5(6) . . ? C20 C19 N3 130.9(6) . . ? C24 C19 N3 109.5(5) . . ? C19 C20 C21 117.8(6) . . ? C22 C21 C20 121.8(7) . . ? C23 C22 C21 121.6(6) . . ? C22 C23 C24 116.5(6) . . ? C19 C24 C23 122.7(6) . . ? C19 C24 N4 105.8(5) . . ? C23 C24 N4 131.4(6) . . ? C28 O3 C25 106.6(7) . . ? O3 C25 C26 108.2(8) . . ? C27 C26 C25 103.7(9) . . ? C28 C27 C26 106.0(10) . . ? O3 C28 C27 108.2(11) . . ? C32 O4 C29 112.5(9) . . ? O4 C29 C30 106.3(9) . . ? C31 C30 C29 102.2(9) . . ? C30 C31 C32 105.9(11) . . ? O4 C32 C31 102.5(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B O4 0.86 1.90 2.764(9) 177.0 . N2 H2B O3 0.86 1.96 2.820(7) 176.3 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.880 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.122 # Attachment '11.cif' data_f70416c _database_code_depnum_ccdc_archive 'CCDC 762750' #TrackingRef '11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H104 N8 O8 S4 Y4' _chemical_formula_weight 1741.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.862(10) _cell_length_b 11.001(3) _cell_length_c 26.692(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.336(8) _cell_angle_gamma 90.00 _cell_volume 8167(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 917 _cell_measurement_theta_min 2.538 _cell_measurement_theta_max 20.753 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 2.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5237 _exptl_absorpt_correction_T_max 0.6168 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18244 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8029 _reflns_number_gt 4508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. DFIX was used to restrain bond lengths to more standard values. SIMU and SADI were used to restrain some abnormal ADPs. ; _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^)+(0.0536P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8029 _refine_ls_number_parameters 457 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.062160(18) 0.53864(5) 0.289312(18) 0.03502(15) Uani 1 1 d D . . Y2 Y 0.034171(18) 0.75068(5) 0.187479(18) 0.03494(15) Uani 1 1 d D . . N1 N 0.11686(15) 0.6534(4) 0.34891(15) 0.0410(11) Uani 1 1 d . . . N2 N 0.11639(17) 0.7150(4) 0.42807(16) 0.0463(12) Uani 1 1 d . . . H2B H 0.1058 0.7328 0.4568 0.056 Uiso 1 1 calc R . . N3 N 0.08784(15) 0.6351(4) 0.13403(15) 0.0419(11) Uani 1 1 d . . . N4 N 0.16576(16) 0.5858(4) 0.13880(17) 0.0485(12) Uani 1 1 d . . . H4B H 0.1943 0.5722 0.1515 0.058 Uiso 1 1 calc R . . S1 S 0.03107(5) 0.62354(14) 0.38826(5) 0.0450(4) Uani 1 1 d . . . S2 S 0.13081(5) 0.66882(15) 0.22601(5) 0.0465(4) Uani 1 1 d . . . O1 O 0.02347(12) 0.5453(3) 0.21031(11) 0.0341(8) Uani 1 1 d D . . H1O H 0.0320(18) 0.501(2) 0.1900(7) 0.051 Uiso 1 1 d D . . O2 O -0.03949(12) 0.7441(3) 0.22290(12) 0.0343(8) Uani 1 1 d D . . H2O H -0.0605(14) 0.785(4) 0.2090(18) 0.051 Uiso 1 1 d D . . C1 C 0.0582(3) 0.3039(6) 0.3142(3) 0.069(2) Uani 1 1 d . . . H1A H 0.0310 0.2626 0.3285 0.083 Uiso 1 1 calc R . . C2 C 0.0686(3) 0.3044(6) 0.2646(3) 0.070(2) Uani 1 1 d . . . H2A H 0.0492 0.2647 0.2376 0.085 Uiso 1 1 calc R . . C3 C 0.1127(3) 0.3518(6) 0.2597(3) 0.073(2) Uani 1 1 d . . . H3A H 0.1306 0.3491 0.2292 0.087 Uiso 1 1 calc R . . C4 C 0.1317(3) 0.3793(6) 0.3064(4) 0.084(3) Uani 1 1 d . . . H4A H 0.1655 0.3990 0.3149 0.100 Uiso 1 1 calc R . . C5 C 0.0979(4) 0.3503(7) 0.3405(3) 0.082(3) Uani 1 1 d . . . H5A H 0.1039 0.3470 0.3770 0.099 Uiso 1 1 calc R . . C6 C 0.0900(2) 0.6694(5) 0.38812(19) 0.0416(14) Uani 1 1 d . . . C7 C 0.1632(2) 0.6896(5) 0.3646(2) 0.0418(14) Uani 1 1 d . . . C8 C 0.2054(2) 0.6898(6) 0.3400(2) 0.0573(17) Uani 1 1 d . . . H8A H 0.2059 0.6656 0.3067 0.069 Uiso 1 1 calc R . . C9 C 0.2472(2) 0.7274(6) 0.3665(3) 0.070(2) Uani 1 1 d . . . H9A H 0.2762 0.7262 0.3509 0.084 Uiso 1 1 calc R . . C10 C 0.2464(2) 0.7661(6) 0.4152(3) 0.074(2) Uani 1 1 d . . . H10A H 0.2749 0.7929 0.4315 0.089 Uiso 1 1 calc R . . C11 C 0.2050(2) 0.7668(6) 0.4408(2) 0.0622(18) Uani 1 1 d . . . H11A H 0.2049 0.7921 0.4740 0.075 Uiso 1 1 calc R . . C12 C 0.1632(2) 0.7280(5) 0.4145(2) 0.0443(14) Uani 1 1 d . . . C13 C 0.0567(3) 0.9858(6) 0.1941(3) 0.0654(19) Uani 1 1 d . . . H13A H 0.0702 1.0264 0.2244 0.078 Uiso 1 1 calc R . . C14 C 0.0088(3) 0.9839(6) 0.1786(3) 0.071(2) Uani 1 1 d . . . H14A H -0.0171 1.0232 0.1960 0.085 Uiso 1 1 calc R . . C15 C 0.0047(3) 0.9373(6) 0.1306(3) 0.074(2) Uani 1 1 d . . . H15A H -0.0243 0.9392 0.1080 0.088 Uiso 1 1 calc R . . C16 C 0.0504(3) 0.9100(6) 0.1170(2) 0.072(2) Uani 1 1 d . . . H16A H 0.0589 0.8895 0.0829 0.086 Uiso 1 1 calc R . . C17 C 0.0832(3) 0.9399(6) 0.1562(3) 0.069(2) Uani 1 1 d . . . H17A H 0.1182 0.9448 0.1544 0.083 Uiso 1 1 calc R . . C18 C 0.12779(19) 0.6251(5) 0.16396(19) 0.0387(13) Uani 1 1 d . . . C19 C 0.1012(2) 0.6021(5) 0.08599(19) 0.0412(14) Uani 1 1 d . . . C20 C 0.0748(2) 0.5965(6) 0.0410(2) 0.0559(17) Uani 1 1 d . . . H20A H 0.0422 0.6159 0.0385 0.067 Uiso 1 1 calc R . . C21 C 0.0990(3) 0.5603(6) -0.0007(2) 0.0643(19) Uani 1 1 d . . . H21A H 0.0820 0.5550 -0.0317 0.077 Uiso 1 1 calc R . . C22 C 0.1466(3) 0.5325(6) 0.0021(2) 0.0641(19) Uani 1 1 d . . . H22A H 0.1612 0.5093 -0.0268 0.077 Uiso 1 1 calc R . . C23 C 0.1737(2) 0.5378(6) 0.0471(2) 0.0604(17) Uani 1 1 d . . . H23A H 0.2063 0.5195 0.0491 0.072 Uiso 1 1 calc R . . C24 C 0.1502(2) 0.5714(5) 0.0887(2) 0.0457(15) Uani 1 1 d . . . C25 C 0.3027(4) 0.5517(11) 0.1601(4) 0.142(4) Uani 1 1 d . . . H25A H 0.3080 0.6318 0.1463 0.171 Uiso 1 1 calc R . . H25B H 0.3042 0.4923 0.1334 0.171 Uiso 1 1 calc R . . C26 C 0.3392(3) 0.5247(10) 0.2006(5) 0.152(5) Uani 1 1 d . . . H26A H 0.3531 0.4448 0.1963 0.183 Uiso 1 1 calc R . . H26B H 0.3648 0.5848 0.2017 0.183 Uiso 1 1 calc R . . C27 C 0.3127(4) 0.5297(14) 0.2458(4) 0.190(7) Uani 1 1 d . . . H27A H 0.3224 0.4643 0.2686 0.228 Uiso 1 1 calc R . . H27B H 0.3179 0.6067 0.2629 0.228 Uiso 1 1 calc R . . C28 C 0.2643(4) 0.5167(12) 0.2285(4) 0.168(3) Uani 1 1 d U . . H28A H 0.2543 0.4330 0.2328 0.202 Uiso 1 1 calc R . . H28B H 0.2443 0.5679 0.2483 0.202 Uiso 1 1 calc R . . C29 C 0.1034(3) 0.7630(7) 0.5705(3) 0.093(3) Uani 1 1 d . . . H29A H 0.1199 0.8351 0.5833 0.112 Uiso 1 1 calc R . . H29B H 0.1263 0.6967 0.5704 0.112 Uiso 1 1 calc R . . C30 C 0.0621(4) 0.7307(8) 0.6035(3) 0.110(3) Uani 1 1 d . . . H30A H 0.0665 0.6504 0.6181 0.132 Uiso 1 1 calc R . . H30B H 0.0594 0.7896 0.6302 0.132 Uiso 1 1 calc R . . C31 C 0.0203(4) 0.7341(10) 0.5688(4) 0.136(4) Uani 1 1 d . . . H31A H -0.0064 0.7731 0.5842 0.163 Uiso 1 1 calc R . . H31B H 0.0107 0.6523 0.5590 0.163 Uiso 1 1 calc R . . C32 C 0.0338(4) 0.8031(10) 0.5252(3) 0.126(4) Uani 1 1 d . . . H32A H 0.0165 0.7741 0.4950 0.151 Uiso 1 1 calc R . . H32B H 0.0269 0.8888 0.5294 0.151 Uiso 1 1 calc R . . O3 O 0.2583(2) 0.5469(8) 0.1810(2) 0.151(3) Uani 1 1 d U . . O4 O 0.0839(2) 0.7838(5) 0.52265(18) 0.0906(17) Uani 1 1 d . . . C35 C 0.2114(6) 0.902(2) 0.0339(6) 0.352(18) Uani 1 1 d D . . H35A H 0.2259 0.8264 0.0234 0.422 Uiso 1 1 calc R . . H35B H 0.2293 0.9703 0.0218 0.422 Uiso 1 1 calc R . . C36 C 0.1581(6) 0.9085(18) 0.0177(6) 0.336(18) Uani 1 1 d D . . H36A H 0.1407 0.8457 0.0345 0.403 Uiso 1 1 calc R . . H36B H 0.1453 0.9868 0.0269 0.403 Uiso 1 1 calc R . . C33 C 0.2506(6) 0.8609(17) 0.1156(8) 0.322(14) Uani 1 1 d D . . H33A H 0.2474 0.8648 0.1512 0.482 Uiso 1 1 calc R . . H33B H 0.2775 0.9095 0.1069 0.482 Uiso 1 1 calc R . . H33C H 0.2557 0.7780 0.1059 0.482 Uiso 1 1 calc R . . C38 C 0.1027(6) 0.9253(16) -0.0573(8) 0.349(16) Uani 1 1 d D . . H38A H 0.1010 0.9186 -0.0932 0.524 Uiso 1 1 calc R . . H38B H 0.0958 1.0075 -0.0480 0.524 Uiso 1 1 calc R . . H38C H 0.0797 0.8715 -0.0438 0.524 Uiso 1 1 calc R . . C34 C 0.2071(5) 0.9065(17) 0.0897(7) 0.316(14) Uani 1 1 d D . . H34A H 0.2016 0.9897 0.0999 0.379 Uiso 1 1 calc R . . H34B H 0.1799 0.8579 0.0987 0.379 Uiso 1 1 calc R . . C37 C 0.1520(6) 0.8919(17) -0.0371(6) 0.345(18) Uani 1 1 d D . . H37A H 0.1583 0.8076 -0.0452 0.414 Uiso 1 1 calc R . . H37B H 0.1754 0.9417 -0.0532 0.414 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 Y1 0.0355(3) 0.0398(3) 0.0292(3) 0.0008(2) -0.0026(2) 0.0036(3) Y2 0.0364(3) 0.0391(3) 0.0293(3) 0.0032(2) 0.0008(2) -0.0012(3) N1 0.034(3) 0.055(3) 0.033(3) -0.002(2) -0.005(2) -0.003(2) N2 0.053(3) 0.057(3) 0.028(3) -0.007(2) -0.002(2) -0.003(2) N3 0.042(3) 0.053(3) 0.031(3) 0.004(2) 0.000(2) -0.002(2) N4 0.030(3) 0.066(3) 0.049(3) 0.002(2) 0.003(2) 0.006(2) S1 0.0400(8) 0.0640(10) 0.0306(8) 0.0043(7) -0.0015(6) 0.0002(7) S2 0.0395(9) 0.0659(11) 0.0337(8) -0.0016(7) -0.0007(6) -0.0043(8) O1 0.038(2) 0.036(2) 0.0279(19) -0.0048(16) 0.0014(16) 0.0006(17) O2 0.036(2) 0.039(2) 0.0270(19) 0.0012(17) -0.0035(15) 0.0065(18) C1 0.079(6) 0.045(4) 0.086(6) 0.018(4) 0.023(5) 0.006(4) C2 0.087(6) 0.032(4) 0.088(6) -0.008(4) -0.033(5) 0.016(4) C3 0.085(6) 0.055(5) 0.080(6) 0.006(4) 0.025(5) 0.023(4) C4 0.058(5) 0.051(5) 0.137(8) 0.001(5) -0.035(5) 0.025(4) C5 0.133(8) 0.070(6) 0.042(4) 0.003(4) -0.020(5) 0.036(5) C6 0.047(4) 0.049(4) 0.028(3) 0.001(3) -0.004(3) 0.003(3) C7 0.046(4) 0.044(4) 0.035(3) -0.001(3) -0.004(3) 0.002(3) C8 0.044(4) 0.075(5) 0.053(4) -0.004(3) 0.003(3) -0.001(3) C9 0.040(4) 0.098(6) 0.072(5) -0.007(4) -0.005(3) -0.006(4) C10 0.049(4) 0.091(6) 0.079(5) -0.002(4) -0.027(4) -0.022(4) C11 0.063(5) 0.076(5) 0.046(4) -0.007(3) -0.014(3) -0.012(4) C12 0.044(4) 0.044(4) 0.043(3) 0.002(3) -0.009(3) 0.001(3) C13 0.092(6) 0.043(4) 0.060(5) 0.004(3) -0.009(4) -0.015(4) C14 0.086(6) 0.034(4) 0.095(6) 0.020(4) 0.028(5) 0.011(4) C15 0.094(6) 0.048(5) 0.075(5) 0.025(4) -0.027(5) -0.002(4) C16 0.117(7) 0.055(5) 0.046(4) 0.022(3) 0.029(5) -0.004(5) C17 0.055(5) 0.062(5) 0.092(6) 0.020(4) 0.015(4) -0.014(4) C18 0.037(3) 0.041(3) 0.038(3) 0.004(3) 0.001(3) -0.004(3) C19 0.048(4) 0.047(4) 0.030(3) 0.003(3) 0.007(3) -0.002(3) C20 0.056(4) 0.073(5) 0.038(4) -0.001(3) 0.001(3) 0.005(3) C21 0.078(5) 0.080(5) 0.036(4) -0.004(3) 0.006(3) -0.008(4) C22 0.080(5) 0.069(5) 0.045(4) -0.014(3) 0.025(4) -0.001(4) C23 0.054(4) 0.074(5) 0.054(4) -0.009(4) 0.014(3) 0.008(4) C24 0.049(4) 0.046(4) 0.043(4) -0.005(3) 0.011(3) -0.009(3) C25 0.089(8) 0.183(12) 0.153(10) 0.003(8) 0.001(7) -0.001(8) C26 0.069(7) 0.130(9) 0.251(15) -0.008(10) -0.058(9) 0.006(6) C27 0.122(11) 0.33(2) 0.111(10) 0.011(11) -0.036(8) 0.006(12) C28 0.084(5) 0.311(9) 0.108(5) -0.012(7) -0.007(5) 0.057(6) C29 0.100(7) 0.091(7) 0.089(6) -0.019(5) 0.004(5) 0.012(5) C30 0.176(11) 0.096(7) 0.062(6) -0.008(5) 0.028(6) 0.013(7) C31 0.138(11) 0.127(9) 0.149(11) 0.018(8) 0.061(9) -0.017(7) C32 0.103(8) 0.178(11) 0.097(8) -0.033(7) 0.005(6) -0.001(8) O3 0.066(4) 0.293(8) 0.091(4) -0.003(5) -0.017(4) 0.052(5) O4 0.090(4) 0.133(5) 0.050(3) -0.016(3) 0.015(3) -0.006(3) C35 0.41(4) 0.24(2) 0.44(3) -0.03(2) 0.34(3) 0.01(2) C36 0.37(3) 0.210(19) 0.46(4) -0.13(2) 0.31(3) -0.12(2) C33 0.21(2) 0.21(2) 0.53(4) 0.02(2) -0.13(2) 0.013(16) C38 0.176(17) 0.183(18) 0.68(5) -0.13(2) -0.06(2) 0.058(14) C34 0.25(3) 0.174(19) 0.53(5) -0.11(3) 0.13(3) -0.039(18) C37 0.55(5) 0.178(18) 0.33(3) 0.04(2) 0.24(3) 0.10(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O1 2.313(3) . ? Y1 O2 2.365(4) 2 ? Y1 O1 2.388(3) 2 ? Y1 N1 2.483(4) . ? Y1 C4 2.633(6) . ? Y1 C3 2.639(6) . ? Y1 C5 2.644(7) . ? Y1 C2 2.669(6) . ? Y1 C1 2.670(6) . ? Y1 S1 2.9773(16) . ? Y1 S2 2.9900(16) . ? Y1 Y2 3.6319(10) . ? Y2 O2 2.310(3) . ? Y2 O1 2.364(3) . ? Y2 O2 2.389(3) 2 ? Y2 N3 2.477(4) . ? Y2 C16 2.630(6) . ? Y2 C17 2.651(6) . ? Y2 C15 2.655(6) . ? Y2 C13 2.665(6) . ? Y2 C14 2.669(6) . ? Y2 S2 2.9658(17) . ? Y2 S1 2.9866(16) 2 ? Y2 C18 3.049(5) . ? N1 C6 1.333(6) . ? N1 C7 1.391(6) . ? N2 C6 1.355(6) . ? N2 C12 1.380(7) . ? N2 H2B 0.8600 . ? N3 C18 1.337(6) . ? N3 C19 1.404(6) . ? N4 C18 1.357(6) . ? N4 C24 1.392(6) . ? N4 H4B 0.8600 . ? S1 C6 1.719(6) . ? S1 Y2 2.9867(16) 2 ? S2 C18 1.722(5) . ? O1 Y1 2.388(3) 2 ? O1 H1O 0.780(19) . ? O2 Y1 2.365(4) 2 ? O2 Y2 2.389(3) 2 ? O2 H2O 0.810(19) . ? C1 C2 1.371(9) . ? C1 C5 1.373(10) . ? C1 H1A 0.9800 . ? C2 C3 1.348(9) . ? C2 H2A 0.9800 . ? C3 C4 1.359(9) . ? C3 H3A 0.9800 . ? C4 C5 1.384(10) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C7 C8 1.380(7) . ? C7 C12 1.398(7) . ? C8 C9 1.390(8) . ? C8 H8A 0.9300 . ? C9 C10 1.369(9) . ? C9 H9A 0.9300 . ? C10 C11 1.375(9) . ? C10 H10A 0.9300 . ? C11 C12 1.391(8) . ? C11 H11A 0.9300 . ? C13 C14 1.374(9) . ? C13 C17 1.382(9) . ? C13 H13A 0.9800 . ? C14 C15 1.379(9) . ? C14 H14A 0.9800 . ? C15 C16 1.376(9) . ? C15 H15A 0.9800 . ? C16 C17 1.387(9) . ? C16 H16A 0.9800 . ? C17 H17A 0.9800 . ? C19 C20 1.374(7) . ? C19 C24 1.402(7) . ? C20 C21 1.393(8) . ? C20 H20A 0.9300 . ? C21 C22 1.358(9) . ? C21 H21A 0.9300 . ? C22 C23 1.383(8) . ? C22 H22A 0.9300 . ? C23 C24 1.371(7) . ? C23 H23A 0.9300 . ? C25 O3 1.386(10) . ? C25 C26 1.473(12) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.451(13) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.408(13) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O3 1.314(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 O4 1.378(8) . ? C29 C30 1.531(11) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.446(12) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.457(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O4 1.416(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C35 C34 1.502(9) . ? C35 C36 1.524(9) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.473(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C33 C34 1.448(9) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C38 C37 1.492(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 Y1 O2 74.78(11) . 2 ? O1 Y1 O1 65.80(12) . 2 ? O2 Y1 O1 73.29(11) 2 2 ? O1 Y1 N1 143.54(13) . . ? O2 Y1 N1 75.61(13) 2 . ? O1 Y1 N1 123.92(13) 2 . ? O1 Y1 C4 118.6(2) . . ? O2 Y1 C4 148.0(2) 2 . ? O1 Y1 C4 138.2(2) 2 . ? N1 Y1 C4 79.0(2) . . ? O1 Y1 C3 88.9(2) . . ? O2 Y1 C3 147.80(18) 2 . ? O1 Y1 C3 125.2(2) 2 . ? N1 Y1 C3 105.6(2) . . ? C4 Y1 C3 29.9(2) . . ? O1 Y1 C5 129.58(19) . . ? O2 Y1 C5 155.49(18) 2 . ? O1 Y1 C5 111.6(2) 2 . ? N1 Y1 C5 82.5(2) . . ? C4 Y1 C5 30.4(2) . . ? C3 Y1 C5 49.7(2) . . ? O1 Y1 C2 80.78(17) . . ? O2 Y1 C2 155.56(17) 2 . ? O1 Y1 C2 96.5(2) 2 . ? N1 Y1 C2 126.97(18) . . ? C4 Y1 C2 48.7(2) . . ? C3 Y1 C2 29.4(2) . . ? C5 Y1 C2 48.9(2) . . ? O1 Y1 C1 103.5(2) . . ? O2 Y1 C1 160.78(18) 2 . ? O1 Y1 C1 88.44(18) 2 . ? N1 Y1 C1 111.4(2) . . ? C4 Y1 C1 49.7(2) . . ? C3 Y1 C1 49.6(2) . . ? C5 Y1 C1 29.9(2) . . ? C2 Y1 C1 29.8(2) . . ? O1 Y1 S1 130.89(9) . . ? O2 Y1 S1 74.53(8) 2 . ? O1 Y1 S1 69.16(8) 2 . ? N1 Y1 S1 58.10(10) . . ? C4 Y1 S1 107.7(2) . . ? C3 Y1 S1 134.27(17) . . ? C5 Y1 S1 84.72(17) . . ? C2 Y1 S1 123.3(2) . . ? C1 Y1 S1 93.70(18) . . ? O1 Y1 S2 75.48(9) . . ? O2 Y1 S2 68.82(9) 2 . ? O1 Y1 S2 131.30(8) 2 . ? N1 Y1 S2 74.31(10) . . ? C4 Y1 S2 85.9(2) . . ? C3 Y1 S2 80.42(17) . . ? C5 Y1 S2 115.7(2) . . ? C2 Y1 S2 105.5(2) . . ? C1 Y1 S2 129.85(16) . . ? S1 Y1 S2 125.43(5) . . ? O1 Y1 Y2 39.56(8) . . ? O2 Y1 Y2 40.43(8) 2 . ? O1 Y1 Y2 79.19(8) 2 . ? N1 Y1 Y2 104.48(10) . . ? C4 Y1 Y2 132.9(2) . . ? C3 Y1 Y2 111.79(17) . . ? C5 Y1 Y2 161.41(17) . . ? C2 Y1 Y2 116.73(17) . . ? C1 Y1 Y2 142.8(2) . . ? S1 Y1 Y2 113.67(4) . . ? S2 Y1 Y2 52.12(3) . . ? O2 Y2 O1 74.71(12) . . ? O2 Y2 O2 66.06(13) . 2 ? O1 Y2 O2 73.41(11) . 2 ? O2 Y2 N3 143.14(14) . . ? O1 Y2 N3 75.36(13) . . ? O2 Y2 N3 123.84(13) 2 . ? O2 Y2 C16 120.5(2) . . ? O1 Y2 C16 148.34(18) . . ? O2 Y2 C16 137.14(19) 2 . ? N3 Y2 C16 78.2(2) . . ? O2 Y2 C17 129.74(18) . . ? O1 Y2 C17 155.09(18) . . ? O2 Y2 C17 109.6(2) 2 . ? N3 Y2 C17 83.3(2) . . ? C16 Y2 C17 30.5(2) . . ? O2 Y2 C15 90.3(2) . . ? O1 Y2 C15 147.93(18) . . ? O2 Y2 C15 126.5(2) 2 . ? N3 Y2 C15 104.1(2) . . ? C16 Y2 C15 30.2(2) . . ? C17 Y2 C15 50.2(2) . . ? O2 Y2 C13 102.4(2) . . ? O1 Y2 C13 160.64(16) . . ? O2 Y2 C13 87.83(17) 2 . ? N3 Y2 C13 112.9(2) . . ? C16 Y2 C13 49.5(2) . . ? C17 Y2 C13 30.13(19) . . ? C15 Y2 C13 49.5(2) . . ? O2 Y2 C14 80.16(18) . . ? O1 Y2 C14 154.87(18) . . ? O2 Y2 C14 96.8(2) 2 . ? N3 Y2 C14 127.47(19) . . ? C16 Y2 C14 49.6(2) . . ? C17 Y2 C14 49.9(2) . . ? C15 Y2 C14 30.0(2) . . ? C13 Y2 C14 29.9(2) . . ? O2 Y2 S2 131.21(8) . . ? O1 Y2 S2 75.28(9) . . ? O2 Y2 S2 68.99(9) 2 . ? N3 Y2 S2 58.51(10) . . ? C16 Y2 S2 105.1(2) . . ? C17 Y2 S2 82.76(16) . . ? C15 Y2 S2 132.61(18) . . ? C13 Y2 S2 93.80(18) . . ? C14 Y2 S2 123.59(19) . . ? O2 Y2 S1 75.06(9) . 2 ? O1 Y2 S1 69.27(8) . 2 ? O2 Y2 S1 131.57(9) 2 2 ? N3 Y2 S1 74.56(10) . 2 ? C16 Y2 S1 87.20(19) . 2 ? C17 Y2 S1 117.31(18) . 2 ? C15 Y2 S1 79.61(16) . 2 ? C13 Y2 S1 129.12(15) . 2 ? C14 Y2 S1 104.0(2) . 2 ? S2 Y2 S1 126.66(5) . 2 ? O2 Y2 C18 149.45(13) . . ? O1 Y2 C18 75.07(13) . . ? O2 Y2 C18 100.86(13) 2 . ? N3 Y2 C18 25.39(13) . . ? C16 Y2 C18 88.3(2) . . ? C17 Y2 C18 80.12(18) . . ? C15 Y2 C18 118.2(2) . . ? C13 Y2 C18 104.6(2) . . ? C14 Y2 C18 130.00(19) . . ? S2 Y2 C18 33.23(10) . . ? S1 Y2 C18 98.22(10) 2 . ? C6 N1 C7 106.1(4) . . ? C6 N1 Y1 102.7(3) . . ? C7 N1 Y1 149.6(4) . . ? C6 N2 C12 108.0(5) . . ? C6 N2 H2B 126.0 . . ? C12 N2 H2B 126.0 . . ? C18 N3 C19 105.6(4) . . ? C18 N3 Y2 102.0(3) . . ? C19 N3 Y2 149.3(4) . . ? C18 N4 C24 107.7(4) . . ? C18 N4 H4B 126.2 . . ? C24 N4 H4B 126.2 . . ? C6 S1 Y1 76.28(18) . . ? C6 S1 Y2 113.91(19) . 2 ? Y1 S1 Y2 75.13(4) . 2 ? C18 S2 Y2 76.04(19) . . ? C18 S2 Y1 114.38(18) . . ? Y2 S2 Y1 75.15(4) . . ? Y1 O1 Y2 101.90(13) . . ? Y1 O1 Y1 114.08(12) . 2 ? Y2 O1 Y1 99.87(12) . 2 ? Y1 O1 H1O 118(2) . . ? Y2 O1 H1O 112(2) . . ? Y1 O1 H1O 109(4) 2 . ? Y2 O2 Y1 102.11(13) . 2 ? Y2 O2 Y2 113.83(13) . 2 ? Y1 O2 Y2 99.63(12) 2 2 ? Y2 O2 H2O 116(4) . . ? Y1 O2 H2O 107(4) 2 . ? Y2 O2 H2O 116(4) 2 . ? C2 C1 C5 106.4(7) . . ? C2 C1 Y1 75.1(4) . . ? C5 C1 Y1 74.0(4) . . ? C2 C1 H1A 126.2 . . ? C5 C1 H1A 126.2 . . ? Y1 C1 H1A 126.2 . . ? C3 C2 C1 109.9(7) . . ? C3 C2 Y1 74.1(4) . . ? C1 C2 Y1 75.1(4) . . ? C3 C2 H2A 124.7 . . ? C1 C2 H2A 124.7 . . ? Y1 C2 H2A 124.7 . . ? C2 C3 C4 107.8(7) . . ? C2 C3 Y1 76.5(4) . . ? C4 C3 Y1 74.8(4) . . ? C2 C3 H3A 125.4 . . ? C4 C3 H3A 125.4 . . ? Y1 C3 H3A 125.4 . . ? C3 C4 C5 107.9(7) . . ? C3 C4 Y1 75.3(4) . . ? C5 C4 Y1 75.2(4) . . ? C3 C4 H4A 125.4 . . ? C5 C4 H4A 125.4 . . ? Y1 C4 H4A 125.4 . . ? C1 C5 C4 108.0(7) . . ? C1 C5 Y1 76.1(4) . . ? C4 C5 Y1 74.4(4) . . ? C1 C5 H5A 125.4 . . ? C4 C5 H5A 125.4 . . ? Y1 C5 H5A 125.4 . . ? N1 C6 N2 111.3(5) . . ? N1 C6 S1 122.9(4) . . ? N2 C6 S1 125.5(4) . . ? C8 C7 N1 131.2(5) . . ? C8 C7 C12 120.0(5) . . ? N1 C7 C12 108.8(5) . . ? C7 C8 C9 118.1(6) . . ? C7 C8 H8A 121.0 . . ? C9 C8 H8A 121.0 . . ? C10 C9 C8 121.1(6) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 122.2(6) . . ? C9 C10 H10A 118.9 . . ? C11 C10 H10A 118.9 . . ? C10 C11 C12 116.8(6) . . ? C10 C11 H11A 121.6 . . ? C12 C11 H11A 121.6 . . ? N2 C12 C11 132.5(6) . . ? N2 C12 C7 105.7(5) . . ? C11 C12 C7 121.8(6) . . ? C14 C13 C17 109.0(6) . . ? C14 C13 Y2 75.2(4) . . ? C17 C13 Y2 74.4(4) . . ? C14 C13 H13A 125.1 . . ? C17 C13 H13A 125.1 . . ? Y2 C13 H13A 125.1 . . ? C13 C14 C15 108.1(7) . . ? C13 C14 Y2 74.9(4) . . ? C15 C14 Y2 74.4(4) . . ? C13 C14 H14A 125.5 . . ? C15 C14 H14A 125.5 . . ? Y2 C14 H14A 125.5 . . ? C16 C15 C14 107.4(7) . . ? C16 C15 Y2 73.9(4) . . ? C14 C15 Y2 75.5(4) . . ? C16 C15 H15A 125.7 . . ? C14 C15 H15A 125.7 . . ? Y2 C15 H15A 125.7 . . ? C15 C16 C17 109.1(6) . . ? C15 C16 Y2 75.9(4) . . ? C17 C16 Y2 75.6(4) . . ? C15 C16 H16A 124.9 . . ? C17 C16 H16A 124.9 . . ? Y2 C16 H16A 124.9 . . ? C13 C17 C16 106.4(7) . . ? C13 C17 Y2 75.5(4) . . ? C16 C17 Y2 73.9(4) . . ? C13 C17 H17A 126.1 . . ? C16 C17 H17A 126.1 . . ? Y2 C17 H17A 126.1 . . ? N3 C18 N4 112.1(5) . . ? N3 C18 S2 123.0(4) . . ? N4 C18 S2 124.7(4) . . ? N3 C18 Y2 52.6(3) . . ? N4 C18 Y2 161.4(4) . . ? S2 C18 Y2 70.73(18) . . ? C20 C19 C24 120.3(5) . . ? C20 C19 N3 130.7(5) . . ? C24 C19 N3 109.0(5) . . ? C19 C20 C21 116.8(6) . . ? C19 C20 H20A 121.6 . . ? C21 C20 H20A 121.6 . . ? C22 C21 C20 122.5(6) . . ? C22 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? C21 C22 C23 121.4(6) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C24 C23 C22 116.9(6) . . ? C24 C23 H23A 121.6 . . ? C22 C23 H23A 121.6 . . ? C23 C24 N4 132.2(6) . . ? C23 C24 C19 122.1(6) . . ? N4 C24 C19 105.7(4) . . ? O3 C25 C26 107.0(9) . . ? O3 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? O3 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? C27 C26 C25 103.9(9) . . ? C27 C26 H26A 111.0 . . ? C25 C26 H26A 111.0 . . ? C27 C26 H26B 111.0 . . ? C25 C26 H26B 111.0 . . ? H26A C26 H26B 109.0 . . ? C28 C27 C26 104.4(9) . . ? C28 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? C28 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? O3 C28 C27 110.8(10) . . ? O3 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? O3 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? O4 C29 C30 107.6(7) . . ? O4 C29 H29A 110.2 . . ? C30 C29 H29A 110.2 . . ? O4 C29 H29B 110.2 . . ? C30 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? C31 C30 C29 103.3(7) . . ? C31 C30 H30A 111.1 . . ? C29 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? C29 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C30 C31 C32 106.8(9) . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? O4 C32 C31 105.2(8) . . ? O4 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? O4 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C28 O3 C25 109.4(7) . . ? C29 O4 C32 108.5(6) . . ? C34 C35 C36 98.5(9) . . ? C34 C35 H35A 112.1 . . ? C36 C35 H35A 112.1 . . ? C34 C35 H35B 112.1 . . ? C36 C35 H35B 112.1 . . ? H35A C35 H35B 109.7 . . ? C37 C36 C35 109.3(11) . . ? C37 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? C37 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C33 C34 C35 110.4(13) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C36 C37 C38 112.3(13) . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B O3 0.86 1.93 2.786(7) 178.1 . N2 H2B O4 0.86 1.98 2.834(6) 176.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.578 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.089 # Attachment '5.cif' data_a00630c _database_code_depnum_ccdc_archive 'CCDC 783261' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40 N2 O2 S Yb2' _chemical_formula_weight 898.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.281(2) _cell_length_b 17.876(4) _cell_length_c 19.787(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3282.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5598 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.98 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 5.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5449 _exptl_absorpt_correction_T_max 0.6558 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13557 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5750 _reflns_number_gt 5247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX was used to restrain bond lengths to more standard values. SIMU was used to restrain some abnormal ADPs. CONN was used to tune the generation of the connectivity table. ; _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^)+(0.0230P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(13) _refine_ls_number_reflns 5750 _refine_ls_number_parameters 379 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0579 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb -0.07518(3) 0.154482(15) 0.815585(13) 0.04067(8) Uani 1 1 d . . . Yb2 Yb 0.04431(3) -0.075452(14) 0.987930(12) 0.03579(7) Uani 1 1 d . . . S1 S 0.00516(18) 0.07933(9) 0.93808(8) 0.0464(4) Uani 1 1 d . . . N1 N -0.2121(6) 0.0521(3) 0.8531(3) 0.0441(13) Uani 1 1 d . . . N2 N -0.1582(6) -0.0445(3) 0.9237(3) 0.0393(12) Uani 1 1 d . . . C1 C -0.3091(14) 0.2151(7) 0.8652(7) 0.102(5) Uani 1 1 d . . . H1A H -0.3521 0.1894 0.9007 0.122 Uiso 1 1 calc R . . C2 C -0.3356(12) 0.2052(7) 0.7970(8) 0.106(4) Uani 1 1 d . . . H2A H -0.4015 0.1721 0.7780 0.127 Uiso 1 1 calc R . . C3 C -0.2468(15) 0.2530(8) 0.7626(6) 0.101(4) Uani 1 1 d . . . H3A H -0.2413 0.2574 0.7159 0.121 Uiso 1 1 calc R . . C4 C -0.1706(12) 0.2918(5) 0.8065(9) 0.103(4) Uani 1 1 d . . . H4A H -0.1024 0.3283 0.7963 0.124 Uiso 1 1 calc R . . C5 C -0.2100(17) 0.2687(8) 0.8700(6) 0.109(4) Uani 1 1 d . . . H5A H -0.1731 0.2876 0.9103 0.130 Uiso 1 1 calc R . . C6 C 0.0903(9) 0.1567(5) 0.7091(4) 0.065(2) Uani 1 1 d . . . H6A H 0.1345 0.2022 0.6995 0.078 Uiso 1 1 calc R . . C7 C -0.0406(10) 0.1335(5) 0.6862(3) 0.063(2) Uani 1 1 d . . . H7A H -0.1011 0.1607 0.6579 0.076 Uiso 1 1 calc R . . C8 C -0.0685(11) 0.0646(5) 0.7113(4) 0.076(2) Uani 1 1 d . . . H8A H -0.1513 0.0368 0.7029 0.092 Uiso 1 1 calc R . . C9 C 0.0449(15) 0.0424(5) 0.7512(4) 0.087(3) Uani 1 1 d . . . H9A H 0.0523 -0.0025 0.7747 0.104 Uiso 1 1 calc R . . C10 C 0.1465(10) 0.0995(6) 0.7500(4) 0.080(3) Uani 1 1 d . . . H10A H 0.2350 0.0998 0.7721 0.096 Uiso 1 1 calc R . . C11 C 0.2227(14) 0.2757(7) 0.8164(5) 0.139(5) Uani 1 1 d DU . . H11A H 0.1648 0.3065 0.7865 0.167 Uiso 1 1 calc R . . H11B H 0.2844 0.2442 0.7890 0.167 Uiso 1 1 calc R . . C12 C 0.3110(13) 0.3236(6) 0.8610(5) 0.120(5) Uani 1 1 d D . . H12A H 0.4109 0.3231 0.8467 0.144 Uiso 1 1 calc R . . H12B H 0.2763 0.3747 0.8602 0.144 Uiso 1 1 calc R . . C13 C 0.2969(13) 0.2918(6) 0.9291(5) 0.121(5) Uani 1 1 d D . . H13A H 0.2842 0.3313 0.9622 0.145 Uiso 1 1 calc R . . H13B H 0.3823 0.2633 0.9408 0.145 Uiso 1 1 calc R . . C14 C 0.1679(13) 0.2422(6) 0.9275(4) 0.115(4) Uani 1 1 d D . . H14A H 0.1893 0.1949 0.9493 0.138 Uiso 1 1 calc R . . H14B H 0.0883 0.2656 0.9512 0.138 Uiso 1 1 calc R . . C15 C -0.1330(7) 0.0266(4) 0.9038(3) 0.0410(15) Uani 1 1 d . . . C16 C -0.3004(8) -0.0080(4) 0.8371(3) 0.0502(17) Uani 1 1 d . . . C17 C -0.4065(8) -0.0155(5) 0.7867(3) 0.061(2) Uani 1 1 d . . . H17A H -0.4277 0.0235 0.7573 0.073 Uiso 1 1 calc R . . C18 C -0.4780(8) -0.0833(5) 0.7827(4) 0.068(2) Uani 1 1 d . . . H18A H -0.5503 -0.0897 0.7506 0.081 Uiso 1 1 calc R . . C19 C -0.4440(9) -0.1408(5) 0.8251(4) 0.067(2) Uani 1 1 d . . . H19A H -0.4930 -0.1858 0.8202 0.081 Uiso 1 1 calc R . . C20 C -0.3405(9) -0.1354(4) 0.8748(4) 0.065(2) Uani 1 1 d . . . H20A H -0.3207 -0.1751 0.9037 0.078 Uiso 1 1 calc R . . C21 C -0.2675(7) -0.0682(4) 0.8799(3) 0.0450(16) Uani 1 1 d . . . C22 C 0.1841(10) -0.1327(5) 0.8842(5) 0.073(3) Uani 1 1 d . . . H22A H 0.2276 -0.0989 0.8549 0.088 Uiso 1 1 calc R . . C23 C 0.0446(10) -0.1604(5) 0.8789(5) 0.079(2) Uani 1 1 d . . . H23A H -0.0216 -0.1493 0.8450 0.094 Uiso 1 1 calc R . . C24 C 0.0227(14) -0.2070(5) 0.9326(7) 0.099(4) Uani 1 1 d . . . H24A H -0.0625 -0.2325 0.9416 0.119 Uiso 1 1 calc R . . C25 C 0.1463(16) -0.2105(5) 0.9718(7) 0.109(4) Uani 1 1 d . . . H25A H 0.1601 -0.2381 1.0111 0.131 Uiso 1 1 calc R . . C26 C 0.2456(10) -0.1639(5) 0.9397(6) 0.079(3) Uani 1 1 d . . . H26A H 0.3395 -0.1555 0.9542 0.095 Uiso 1 1 calc R . . C27 C -0.1648(9) -0.1015(5) 1.0719(4) 0.061(2) Uani 1 1 d . . . H27A H -0.2523 -0.1168 1.0536 0.074 Uiso 1 1 calc R . . C28 C -0.0548(11) -0.1471(5) 1.0927(4) 0.076(2) Uani 1 1 d . . . H28A H -0.0541 -0.1991 1.0906 0.091 Uiso 1 1 calc R . . C29 C 0.0549(12) -0.1027(7) 1.1173(4) 0.089(3) Uani 1 1 d . . . H29A H 0.1415 -0.1199 1.1352 0.107 Uiso 1 1 calc R . . C30 C 0.0158(10) -0.0282(6) 1.1112(4) 0.075(3) Uani 1 1 d . . . H30A H 0.0708 0.0131 1.1234 0.090 Uiso 1 1 calc R . . C31 C -0.1207(9) -0.0271(5) 1.0835(4) 0.062(2) Uani 1 1 d . . . H31A H -0.1744 0.0155 1.0740 0.075 Uiso 1 1 calc R . . C32 C 0.3579(8) 0.0181(5) 0.9522(4) 0.078(3) Uani 1 1 d D . . H32A H 0.2998 0.0509 0.9243 0.094 Uiso 1 1 calc R . . H32B H 0.3978 -0.0211 0.9240 0.094 Uiso 1 1 calc R . . C33 C 0.4760(9) 0.0612(5) 0.9866(4) 0.093(3) Uani 1 1 d D . . H33A H 0.5649 0.0580 0.9610 0.112 Uiso 1 1 calc R . . H33B H 0.4496 0.1135 0.9913 0.112 Uiso 1 1 calc R . . C34 C 0.4931(10) 0.0256(7) 1.0543(5) 0.117(4) Uani 1 1 d D . . H34A H 0.5782 -0.0059 1.0552 0.140 Uiso 1 1 calc R . . H34B H 0.5022 0.0634 1.0892 0.140 Uiso 1 1 calc R . . C35 C 0.3612(10) -0.0200(7) 1.0652(5) 0.119(5) Uani 1 1 d D . . H35A H 0.3871 -0.0719 1.0727 0.143 Uiso 1 1 calc R . . H35B H 0.3096 -0.0021 1.1046 0.143 Uiso 1 1 calc R . . O1 O 0.1307(6) 0.2302(3) 0.8584(2) 0.0639(15) Uani 1 1 d DU . . O2 O 0.2723(4) -0.0136(3) 1.0063(2) 0.0546(12) Uani 1 1 d 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 Yb1 0.04684(17) 0.04370(15) 0.03146(14) 0.00620(12) 0.00201(12) 0.00662(13) Yb2 0.03652(14) 0.03859(14) 0.03225(13) 0.00437(11) 0.00378(11) 0.00340(12) S1 0.0555(11) 0.0424(8) 0.0414(9) 0.0056(8) -0.0140(7) -0.0058(8) N1 0.047(3) 0.048(3) 0.037(3) 0.007(2) -0.002(3) -0.001(3) N2 0.043(3) 0.043(3) 0.032(3) 0.005(2) -0.008(2) -0.004(2) C1 0.088(8) 0.094(9) 0.124(11) 0.055(8) 0.064(8) 0.042(7) C2 0.057(6) 0.094(8) 0.167(13) -0.013(9) -0.030(7) 0.042(6) C3 0.107(10) 0.116(10) 0.079(7) 0.043(8) 0.005(7) 0.059(8) C4 0.083(8) 0.047(5) 0.179(14) 0.033(7) 0.014(9) 0.013(5) C5 0.147(13) 0.101(9) 0.078(8) -0.010(7) 0.003(8) 0.068(9) C6 0.074(6) 0.075(5) 0.046(4) -0.008(4) 0.021(4) -0.004(5) C7 0.068(5) 0.089(6) 0.033(4) -0.007(4) 0.002(4) 0.010(5) C8 0.091(7) 0.085(6) 0.053(5) -0.029(5) 0.005(5) -0.005(6) C9 0.151(10) 0.065(5) 0.045(5) 0.001(4) 0.031(7) 0.031(7) C10 0.054(5) 0.142(9) 0.043(5) -0.023(5) -0.004(4) 0.027(6) C11 0.178(13) 0.157(11) 0.083(7) 0.016(8) 0.010(8) -0.111(10) C12 0.158(12) 0.107(9) 0.096(8) -0.006(7) 0.035(8) -0.070(8) C13 0.139(12) 0.105(9) 0.119(10) -0.008(7) -0.021(8) -0.064(8) C14 0.164(12) 0.107(8) 0.074(7) 0.010(6) -0.029(7) -0.060(8) C15 0.040(4) 0.050(4) 0.033(4) 0.000(3) -0.004(3) 0.001(3) C16 0.046(4) 0.067(5) 0.037(4) 0.000(3) -0.002(3) -0.007(4) C17 0.050(5) 0.091(6) 0.042(4) 0.011(4) -0.008(3) -0.007(4) C18 0.048(5) 0.108(7) 0.047(4) -0.004(5) -0.010(3) -0.028(5) C19 0.050(5) 0.086(6) 0.065(5) -0.014(4) -0.001(4) -0.029(5) C20 0.077(6) 0.065(5) 0.053(5) 0.007(4) 0.000(4) -0.023(4) C21 0.050(4) 0.053(4) 0.032(3) 0.008(3) 0.000(3) -0.008(3) C22 0.069(6) 0.065(6) 0.085(7) -0.029(5) 0.031(5) 0.000(5) C23 0.068(6) 0.080(6) 0.088(6) -0.040(5) 0.015(5) 0.005(6) C24 0.094(9) 0.059(6) 0.143(10) -0.029(6) 0.040(8) -0.006(6) C25 0.122(10) 0.052(6) 0.153(11) 0.015(6) 0.041(9) 0.046(6) C26 0.060(6) 0.064(6) 0.114(8) -0.021(6) 0.005(5) 0.031(5) C27 0.053(5) 0.090(6) 0.040(4) -0.003(4) 0.011(3) -0.013(4) C28 0.079(6) 0.086(6) 0.061(5) 0.035(4) 0.011(5) 0.006(6) C29 0.075(6) 0.152(9) 0.040(4) 0.031(5) -0.009(5) -0.006(7) C30 0.080(7) 0.115(8) 0.031(4) -0.019(4) 0.017(4) -0.037(6) C31 0.054(5) 0.087(6) 0.047(5) -0.017(4) 0.016(4) 0.004(4) C32 0.048(5) 0.102(7) 0.085(6) 0.015(5) 0.011(4) -0.012(5) C33 0.076(6) 0.109(7) 0.095(7) -0.006(6) 0.021(6) -0.042(6) C34 0.068(7) 0.158(11) 0.124(9) 0.055(8) -0.027(6) -0.033(7) C35 0.062(6) 0.200(13) 0.096(8) 0.043(8) -0.042(6) -0.041(8) O1 0.079(4) 0.064(3) 0.049(3) 0.003(3) 0.003(3) -0.022(3) O2 0.040(3) 0.074(3) 0.050(3) 0.012(3) -0.005(2) -0.003(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 Yb1 N1 2.349(5) . ? Yb1 O1 2.489(5) . ? Yb1 C3 2.596(9) . ? Yb1 C2 2.607(9) . ? Yb1 C7 2.607(6) . ? Yb1 C6 2.607(7) . ? Yb1 C8 2.616(7) . ? Yb1 C4 2.616(9) . ? Yb1 C1 2.617(9) . ? Yb1 C9 2.623(8) . ? Yb1 C10 2.624(8) . ? Yb1 C5 2.626(10) . ? Yb1 S1 2.8698(16) . ? Yb2 N2 2.336(5) . ? Yb2 O2 2.415(4) . ? Yb2 C31 2.582(7) . ? Yb2 C30 2.594(7) . ? Yb2 C27 2.597(7) . ? Yb2 C24 2.601(9) . ? Yb2 C28 2.605(7) . ? Yb2 C29 2.608(7) . ? Yb2 C25 2.613(8) . ? Yb2 C26 2.626(7) . ? Yb2 C22 2.635(7) . ? Yb2 C23 2.639(7) . ? Yb2 S1 2.9599(18) . ? S1 C15 1.729(7) . ? N1 C15 1.325(8) . ? N1 C16 1.387(8) . ? N2 C15 1.351(8) . ? N2 C21 1.400(8) . ? C1 C5 1.331(17) . ? C1 C2 1.382(16) . ? C1 H1A 0.9300 . ? C2 C3 1.368(15) . ? C2 H2A 0.9300 . ? C3 C4 1.318(15) . ? C3 H3A 0.9300 . ? C4 C5 1.373(15) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.361(11) . ? C6 C10 1.404(11) . ? C6 H6A 0.9300 . ? C7 C8 1.353(11) . ? C7 H7A 0.9300 . ? C8 C9 1.375(13) . ? C8 H8A 0.9300 . ? C9 C10 1.390(13) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 O1 1.443(7) . ? C11 C12 1.477(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.468(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.490(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O1 1.427(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C21 1.403(9) . ? C16 C17 1.407(9) . ? C17 C18 1.384(10) . ? C17 H17A 0.9300 . ? C18 C19 1.364(10) . ? C18 H18A 0.9300 . ? C19 C20 1.378(11) . ? C19 H19A 0.9300 . ? C20 C21 1.383(9) . ? C20 H20A 0.9300 . ? C22 C26 1.357(12) . ? C22 C23 1.390(12) . ? C22 H22A 0.9300 . ? C23 C24 1.365(13) . ? C23 H23A 0.9300 . ? C24 C25 1.386(16) . ? C24 H24A 0.9300 . ? C25 C26 1.394(14) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.370(11) . ? C27 C31 1.411(11) . ? C27 H27A 0.9300 . ? C28 C29 1.380(13) . ? C28 H28A 0.9300 . ? C29 C30 1.385(13) . ? C29 H29A 0.9300 . ? C30 C31 1.380(11) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 O2 1.448(7) . ? C32 C33 1.503(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.492(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.486(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 O2 1.433(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? 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 N1 Yb1 O1 137.01(17) . . ? N1 Yb1 C3 108.9(4) . . ? O1 Yb1 C3 103.9(4) . . ? N1 Yb1 C2 79.3(4) . . ? O1 Yb1 C2 124.8(3) . . ? C3 Yb1 C2 30.5(3) . . ? N1 Yb1 C7 105.4(2) . . ? O1 Yb1 C7 108.5(2) . . ? C3 Yb1 C7 77.1(3) . . ? C2 Yb1 C7 91.5(4) . . ? N1 Yb1 C6 125.9(2) . . ? O1 Yb1 C6 79.3(2) . . ? C3 Yb1 C6 91.4(3) . . ? C2 Yb1 C6 115.3(4) . . ? C7 Yb1 C6 30.3(2) . . ? N1 Yb1 C8 77.5(3) . . ? O1 Yb1 C8 125.7(3) . . ? C3 Yb1 C8 96.5(4) . . ? C2 Yb1 C8 97.1(4) . . ? C7 Yb1 C8 30.0(2) . . ? C6 Yb1 C8 50.1(3) . . ? N1 Yb1 C4 124.7(3) . . ? O1 Yb1 C4 76.9(3) . . ? C3 Yb1 C4 29.3(3) . . ? C2 Yb1 C4 49.5(4) . . ? C7 Yb1 C4 96.3(4) . . ? C6 Yb1 C4 97.4(4) . . ? C8 Yb1 C4 122.0(5) . . ? N1 Yb1 C1 75.9(3) . . ? O1 Yb1 C1 106.5(4) . . ? C3 Yb1 C1 50.3(3) . . ? C2 Yb1 C1 30.7(4) . . ? C7 Yb1 C1 122.0(4) . . ? C6 Yb1 C1 141.7(3) . . ? C8 Yb1 C1 124.7(5) . . ? C4 Yb1 C1 49.9(3) . . ? N1 Yb1 C9 77.8(3) . . ? O1 Yb1 C9 104.7(3) . . ? C3 Yb1 C9 125.7(4) . . ? C2 Yb1 C9 126.2(4) . . ? C7 Yb1 C9 50.3(3) . . ? C6 Yb1 C9 50.9(3) . . ? C8 Yb1 C9 30.4(3) . . ? C4 Yb1 C9 145.8(4) . . ? C1 Yb1 C9 148.3(5) . . ? N1 Yb1 C10 106.8(3) . . ? O1 Yb1 C10 76.7(3) . . ? C3 Yb1 C10 122.4(3) . . ? C2 Yb1 C10 141.9(4) . . ? C7 Yb1 C10 50.5(3) . . ? C6 Yb1 C10 31.1(3) . . ? C8 Yb1 C10 50.3(3) . . ? C4 Yb1 C10 125.7(4) . . ? C1 Yb1 C10 172.3(4) . . ? C9 Yb1 C10 30.7(3) . . ? N1 Yb1 C5 102.6(4) . . ? O1 Yb1 C5 78.7(4) . . ? C3 Yb1 C5 49.1(4) . . ? C2 Yb1 C5 49.2(4) . . ? C7 Yb1 C5 125.0(3) . . ? C6 Yb1 C5 126.9(4) . . ? C8 Yb1 C5 144.3(4) . . ? C4 Yb1 C5 30.4(3) . . ? C1 Yb1 C5 29.4(4) . . ? C9 Yb1 C5 174.7(4) . . ? C10 Yb1 C5 150.2(5) . . ? N1 Yb1 S1 60.59(13) . . ? O1 Yb1 S1 76.58(12) . . ? C3 Yb1 S1 144.9(3) . . ? C2 Yb1 S1 121.5(4) . . ? C7 Yb1 S1 136.89(19) . . ? C6 Yb1 S1 122.4(2) . . ? C8 Yb1 S1 111.9(2) . . ? C4 Yb1 S1 125.8(4) . . ? C1 Yb1 S1 95.3(3) . . ? C9 Yb1 S1 86.7(2) . . ? C10 Yb1 S1 92.2(2) . . ? C5 Yb1 S1 98.1(3) . . ? N2 Yb2 O2 132.72(17) . . ? N2 Yb2 C31 80.9(2) . . ? O2 Yb2 C31 104.8(2) . . ? N2 Yb2 C30 110.6(3) . . ? O2 Yb2 C30 78.4(2) . . ? C31 Yb2 C30 30.9(3) . . ? N2 Yb2 C27 77.9(2) . . ? O2 Yb2 C27 129.8(2) . . ? C31 Yb2 C27 31.6(2) . . ? C30 Yb2 C27 51.7(3) . . ? N2 Yb2 C24 85.6(4) . . ? O2 Yb2 C24 123.0(3) . . ? C31 Yb2 C24 124.4(3) . . ? C30 Yb2 C24 133.0(4) . . ? C27 Yb2 C24 92.8(3) . . ? N2 Yb2 C28 105.4(3) . . ? O2 Yb2 C28 114.5(2) . . ? C31 Yb2 C28 51.1(3) . . ? C30 Yb2 C28 51.4(3) . . ? C27 Yb2 C28 30.5(3) . . ? C24 Yb2 C28 82.1(3) . . ? N2 Yb2 C29 127.5(3) . . ? O2 Yb2 C29 84.5(3) . . ? C31 Yb2 C29 50.6(3) . . ? C30 Yb2 C29 30.9(3) . . ? C27 Yb2 C29 50.7(3) . . ? C24 Yb2 C29 104.3(4) . . ? C28 Yb2 C29 30.7(3) . . ? N2 Yb2 C25 116.3(4) . . ? O2 Yb2 C25 97.1(4) . . ? C31 Yb2 C25 127.9(3) . . ? C30 Yb2 C25 116.9(4) . . ? C27 Yb2 C25 100.6(3) . . ? C24 Yb2 C25 30.8(3) . . ? C28 Yb2 C25 76.8(3) . . ? C29 Yb2 C25 86.2(4) . . ? N2 Yb2 C26 121.1(3) . . ? O2 Yb2 C26 73.0(2) . . ? C31 Yb2 C26 152.8(3) . . ? C30 Yb2 C26 127.6(3) . . ? C27 Yb2 C26 131.0(3) . . ? C24 Yb2 C26 50.0(3) . . ? C28 Yb2 C26 104.1(3) . . ? C29 Yb2 C26 102.6(4) . . ? C25 Yb2 C26 30.9(3) . . ? N2 Yb2 C22 93.7(3) . . ? O2 Yb2 C22 82.2(2) . . ? C31 Yb2 C22 172.9(3) . . ? C30 Yb2 C22 155.4(3) . . ? C27 Yb2 C22 142.8(3) . . ? C24 Yb2 C22 50.1(3) . . ? C28 Yb2 C22 127.1(3) . . ? C29 Yb2 C22 132.3(4) . . ? C25 Yb2 C22 50.7(3) . . ? C26 Yb2 C22 29.9(3) . . ? N2 Yb2 C23 72.1(3) . . ? O2 Yb2 C23 112.7(2) . . ? C31 Yb2 C23 142.4(3) . . ? C30 Yb2 C23 163.0(3) . . ? C27 Yb2 C23 114.9(3) . . ? C24 Yb2 C23 30.2(3) . . ? C28 Yb2 C23 111.6(3) . . ? C29 Yb2 C23 134.1(4) . . ? C25 Yb2 C23 50.8(4) . . ? C26 Yb2 C23 49.9(3) . . ? C22 Yb2 C23 30.6(3) . . ? N2 Yb2 S1 59.89(13) . . ? O2 Yb2 S1 74.32(11) . . ? C31 Yb2 S1 81.9(2) . . ? C30 Yb2 S1 89.8(3) . . ? C27 Yb2 S1 106.8(2) . . ? C24 Yb2 S1 134.0(3) . . ? C28 Yb2 S1 133.0(2) . . ? C29 Yb2 S1 120.4(3) . . ? C25 Yb2 S1 150.2(3) . . ? C26 Yb2 S1 121.9(3) . . ? C22 Yb2 S1 99.5(2) . . ? C23 Yb2 S1 105.4(2) . . ? C15 S1 Yb1 74.4(2) . . ? C15 S1 Yb2 73.3(2) . . ? Yb1 S1 Yb2 138.67(6) . . ? C15 N1 C16 103.6(5) . . ? C15 N1 Yb1 102.0(4) . . ? C16 N1 Yb1 148.3(4) . . ? C15 N2 C21 103.3(5) . . ? C15 N2 Yb2 104.0(4) . . ? C21 N2 Yb2 148.1(4) . . ? C5 C1 C2 106.6(11) . . ? C5 C1 Yb1 75.6(6) . . ? C2 C1 Yb1 74.2(6) . . ? C5 C1 H1A 126.7 . . ? C2 C1 H1A 126.7 . . ? Yb1 C1 H1A 115.8 . . ? C3 C2 C1 107.3(11) . . ? C3 C2 Yb1 74.3(6) . . ? C1 C2 Yb1 75.1(6) . . ? C3 C2 H2A 126.4 . . ? C1 C2 H2A 126.4 . . ? Yb1 C2 H2A 116.4 . . ? C4 C3 C2 109.0(11) . . ? C4 C3 Yb1 76.2(6) . . ? C2 C3 Yb1 75.2(5) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Yb1 C3 H3A 115.1 . . ? C3 C4 C5 107.5(11) . . ? C3 C4 Yb1 74.5(6) . . ? C5 C4 Yb1 75.2(6) . . ? C3 C4 H4A 126.2 . . ? C5 C4 H4A 126.2 . . ? Yb1 C4 H4A 116.2 . . ? C1 C5 C4 109.5(12) . . ? C1 C5 Yb1 74.9(6) . . ? C4 C5 Yb1 74.4(6) . . ? C1 C5 H5A 125.2 . . ? C4 C5 H5A 125.2 . . ? Yb1 C5 H5A 117.3 . . ? C7 C6 C10 107.5(8) . . ? C7 C6 Yb1 74.8(4) . . ? C10 C6 Yb1 75.1(4) . . ? C7 C6 H6A 126.2 . . ? C10 C6 H6A 126.2 . . ? Yb1 C6 H6A 116.0 . . ? C8 C7 C6 109.1(8) . . ? C8 C7 Yb1 75.4(4) . . ? C6 C7 Yb1 74.9(4) . . ? C8 C7 H7A 125.5 . . ? C6 C7 H7A 125.5 . . ? Yb1 C7 H7A 116.3 . . ? C7 C8 C9 109.1(9) . . ? C7 C8 Yb1 74.6(4) . . ? C9 C8 Yb1 75.1(4) . . ? C7 C8 H8A 125.5 . . ? C9 C8 H8A 125.5 . . ? Yb1 C8 H8A 116.8 . . ? C8 C9 C10 107.3(8) . . ? C8 C9 Yb1 74.5(5) . . ? C10 C9 Yb1 74.7(5) . . ? C8 C9 H9A 126.4 . . ? C10 C9 H9A 126.4 . . ? Yb1 C9 H9A 116.6 . . ? C9 C10 C6 107.0(8) . . ? C9 C10 Yb1 74.6(5) . . ? C6 C10 Yb1 73.8(4) . . ? C9 C10 H10A 126.5 . . ? C6 C10 H10A 126.5 . . ? Yb1 C10 H10A 117.3 . . ? O1 C11 C12 108.2(7) . . ? O1 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O1 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C13 C12 C11 106.0(7) . . ? C13 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? C13 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C12 C13 C14 106.4(7) . . ? C12 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? C12 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? O1 C14 C13 107.7(7) . . ? O1 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? O1 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? N1 C15 N2 116.6(6) . . ? N1 C15 S1 121.4(5) . . ? N2 C15 S1 121.8(5) . . ? N1 C16 C21 109.1(6) . . ? N1 C16 C17 130.5(7) . . ? C21 C16 C17 120.4(7) . . ? C18 C17 C16 117.4(7) . . ? C18 C17 H17A 121.3 . . ? C16 C17 H17A 121.3 . . ? C19 C18 C17 120.9(7) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 123.2(7) . . ? C18 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C19 C20 C21 117.0(7) . . ? C19 C20 H20A 121.5 . . ? C21 C20 H20A 121.5 . . ? C20 C21 N2 131.5(6) . . ? C20 C21 C16 121.1(7) . . ? N2 C21 C16 107.4(6) . . ? C26 C22 C23 107.9(9) . . ? C26 C22 Yb2 74.7(5) . . ? C23 C22 Yb2 74.8(4) . . ? C26 C22 H22A 126.1 . . ? C23 C22 H22A 126.1 . . ? Yb2 C22 H22A 116.5 . . ? C24 C23 C22 107.3(10) . . ? C24 C23 Yb2 73.4(5) . . ? C22 C23 Yb2 74.6(5) . . ? C24 C23 H23A 126.4 . . ? C22 C23 H23A 126.4 . . ? Yb2 C23 H23A 117.7 . . ? C23 C24 C25 109.9(10) . . ? C23 C24 Yb2 76.4(5) . . ? C25 C24 Yb2 75.0(6) . . ? C23 C24 H24A 125.1 . . ? C25 C24 H24A 125.1 . . ? Yb2 C24 H24A 115.4 . . ? C24 C25 C26 105.4(10) . . ? C24 C25 Yb2 74.1(5) . . ? C26 C25 Yb2 75.1(5) . . ? C24 C25 H25A 127.3 . . ? C26 C25 H25A 127.3 . . ? Yb2 C25 H25A 116.0 . . ? C22 C26 C25 109.6(10) . . ? C22 C26 Yb2 75.4(4) . . ? C25 C26 Yb2 74.0(5) . . ? C22 C26 H26A 125.2 . . ? C25 C26 H26A 125.2 . . ? Yb2 C26 H26A 117.2 . . ? C28 C27 C31 107.2(8) . . ? C28 C27 Yb2 75.0(5) . . ? C31 C27 Yb2 73.6(4) . . ? C28 C27 H27A 126.4 . . ? C31 C27 H27A 126.4 . . ? Yb2 C27 H27A 117.1 . . ? C27 C28 C29 108.3(8) . . ? C27 C28 Yb2 74.4(4) . . ? C29 C28 Yb2 74.8(5) . . ? C27 C28 H28A 125.9 . . ? C29 C28 H28A 125.9 . . ? Yb2 C28 H28A 117.0 . . ? C28 C29 C30 109.2(9) . . ? C28 C29 Yb2 74.5(4) . . ? C30 C29 Yb2 74.0(4) . . ? C28 C29 H29A 125.4 . . ? C30 C29 H29A 125.4 . . ? Yb2 C29 H29A 117.9 . . ? C31 C30 C29 106.8(9) . . ? C31 C30 Yb2 74.0(4) . . ? C29 C30 Yb2 75.1(5) . . ? C31 C30 H30A 126.6 . . ? C29 C30 H30A 126.6 . . ? Yb2 C30 H30A 116.5 . . ? C30 C31 C27 108.5(9) . . ? C30 C31 Yb2 75.0(4) . . ? C27 C31 Yb2 74.8(4) . . ? C30 C31 H31A 125.8 . . ? C27 C31 H31A 125.8 . . ? Yb2 C31 H31A 116.4 . . ? O2 C32 C33 105.4(6) . . ? O2 C32 H32A 110.7 . . ? C33 C32 H32A 110.7 . . ? O2 C32 H32B 110.7 . . ? C33 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C34 C33 C32 105.4(7) . . ? C34 C33 H33A 110.7 . . ? C32 C33 H33A 110.7 . . ? C34 C33 H33B 110.7 . . ? C32 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? C35 C34 C33 106.0(7) . . ? C35 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? C35 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? O2 C35 C34 108.2(7) . . ? O2 C35 H35A 110.1 . . ? C34 C35 H35A 110.1 . . ? O2 C35 H35B 110.1 . . ? C34 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? C14 O1 C11 108.8(6) . . ? C14 O1 Yb1 126.4(5) . . ? C11 O1 Yb1 124.4(5) . . ? C35 O2 C32 108.5(6) . . ? C35 O2 Yb2 126.2(4) . . ? C32 O2 Yb2 123.3(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.888 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.088