Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Xigeng Zhou' _publ_contact_author_address ; Department of Chemistry Fudan University Shanghai 200433 CHINA ; _publ_contact_author_email XGZHOU@FUDAN.EDU.CN _publ_section_title ; Unusual modification methods for the ureido ligand of lanthanocene derivatives ; loop_ _publ_author_name 'Xigeng Zhou' 'Ruifang Cai' 'Linhong Weng' 'Jie Zhang' data_f30814a _database_code_depnum_ccdc_archive 'CCDC 247293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Dy N3 O2' _chemical_formula_weight 579.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 17.841(2) _cell_length_b 7.9480(10) _cell_length_c 19.008(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.590(2) _cell_angle_gamma 90.00 _cell_volume 2450.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 3.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 9952 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4314 _reflns_number_gt 3744 _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. ; _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^)+(0.0308P)^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 4314 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.276110(11) 1.04713(3) 0.207541(11) 0.03684(8) Uani 1 1 d . . . O1 O 0.17739(17) 0.8361(4) 0.12803(16) 0.0501(8) Uani 1 1 d . . . O2 O 0.24163(18) 0.8983(4) 0.28950(15) 0.0526(8) Uani 1 1 d . . . N1 N 0.3435(2) 1.1437(5) 0.3460(2) 0.0457(9) Uani 1 1 d . . . N2 N 0.3336(2) 1.0307(5) 0.39627(19) 0.0438(9) Uani 1 1 d . . . N3 N 0.2659(2) 0.7981(5) 0.4112(2) 0.0570(11) Uani 1 1 d . . . C1 C 0.4169(3) 0.8760(8) 0.2576(3) 0.0719(15) Uani 1 1 d . . . H1A H 0.4410 0.8120 0.3059 0.086 Uiso 1 1 calc R . . C2 C 0.4392(3) 1.0351(8) 0.2465(4) 0.0687(16) Uani 1 1 d . . . H2A H 0.4808 1.1046 0.2863 0.082 Uiso 1 1 calc R . . C3 C 0.4033(3) 1.0712(7) 0.1695(4) 0.0711(16) Uani 1 1 d . . . H3A H 0.4161 1.1691 0.1451 0.085 Uiso 1 1 calc R . . C4 C 0.3588(3) 0.9293(9) 0.1303(3) 0.0745(18) Uani 1 1 d . . . H4A H 0.3365 0.9094 0.0744 0.089 Uiso 1 1 calc R . . C5 C 0.3683(3) 0.8108(7) 0.1861(4) 0.0713(16) Uani 1 1 d . . . H5A H 0.3526 0.6922 0.1758 0.086 Uiso 1 1 calc R . . C6 C 0.2600(4) 1.3600(7) 0.1578(3) 0.0693(15) Uani 1 1 d . . . H6A H 0.3055 1.4352 0.1628 0.083 Uiso 1 1 calc R . . C7 C 0.2202(4) 1.3583(7) 0.2059(3) 0.0690(15) Uani 1 1 d . . . H7A H 0.2339 1.4301 0.2515 0.083 Uiso 1 1 calc R . . C8 C 0.1513(4) 1.2629(9) 0.1732(5) 0.0862(19) Uani 1 1 d . . . H8A H 0.1073 1.2549 0.1912 0.103 Uiso 1 1 calc R . . C9 C 0.1462(4) 1.2080(8) 0.1021(4) 0.099(3) Uani 1 1 d . . . H9A H 0.0981 1.1549 0.0614 0.118 Uiso 1 1 calc R . . C10 C 0.2139(5) 1.2695(8) 0.0938(3) 0.084(2) Uani 1 1 d . . . H10A H 0.2218 1.2676 0.0458 0.101 Uiso 1 1 calc R . . C11 C 0.1628(3) 0.7844(8) 0.0507(3) 0.0774(17) Uani 1 1 d . . . H11A H 0.1632 0.8813 0.0198 0.093 Uiso 1 1 calc R . . H11B H 0.2053 0.7068 0.0521 0.093 Uiso 1 1 calc R . . C12 C 0.0834(4) 0.7035(11) 0.0180(4) 0.121(3) Uani 1 1 d . . . H12A H 0.0451 0.7704 -0.0244 0.145 Uiso 1 1 calc R . . H12B H 0.0882 0.5937 -0.0020 0.145 Uiso 1 1 calc R . . C13 C 0.0537(4) 0.6861(9) 0.0759(3) 0.098(2) Uani 1 1 d . . . H13A H 0.0504 0.5680 0.0872 0.117 Uiso 1 1 calc R . . H13B H -0.0009 0.7348 0.0585 0.117 Uiso 1 1 calc R . . C14 C 0.1110(3) 0.7735(8) 0.1452(3) 0.0706(16) Uani 1 1 d . . . H14A H 0.0834 0.8658 0.1580 0.085 Uiso 1 1 calc R . . H14B H 0.1321 0.6967 0.1888 0.085 Uiso 1 1 calc R . . C15 C 0.4244(3) 1.4010(7) 0.3577(3) 0.0721(16) Uani 1 1 d . . . H15A H 0.4145 1.3768 0.3051 0.108 Uiso 1 1 calc R . . H15B H 0.4822 1.4199 0.3876 0.108 Uiso 1 1 calc R . . H15C H 0.3941 1.4998 0.3592 0.108 Uiso 1 1 calc R . . C16 C 0.3969(3) 1.2561(6) 0.3907(3) 0.0502(11) Uani 1 1 d . . . C17 C 0.4213(3) 1.2150(7) 0.4682(3) 0.0588(13) Uani 1 1 d . . . H17 H 0.4589 1.2738 0.5105 0.071 Uiso 1 1 calc R . . C18 C 0.3804(3) 1.0746(6) 0.4708(3) 0.0512(12) Uani 1 1 d . . . C19 C 0.3843(4) 0.9780(7) 0.5395(3) 0.0733(16) Uani 1 1 d . . . H19A H 0.3302 0.9705 0.5385 0.110 Uiso 1 1 calc R . . H19B H 0.4205 1.0345 0.5859 0.110 Uiso 1 1 calc R . . H19C H 0.4049 0.8669 0.5384 0.110 Uiso 1 1 calc R . . C20 C 0.2745(3) 0.8971(6) 0.3628(2) 0.0429(10) Uani 1 1 d . . . C21 C 0.2072(3) 0.6677(7) 0.3835(2) 0.0522(12) Uani 1 1 d . . . C22 C 0.2320(4) 0.5041(7) 0.4051(3) 0.0613(14) Uani 1 1 d . . . H22 H 0.2875 0.4810 0.4343 0.074 Uiso 1 1 calc R . . C23 C 0.1754(4) 0.3743(8) 0.3837(3) 0.0751(16) Uani 1 1 d . . . H23 H 0.1933 0.2648 0.3985 0.090 Uiso 1 1 calc R . . C24 C 0.0947(4) 0.4045(9) 0.3417(4) 0.086(2) Uani 1 1 d . . . H24 H 0.0571 0.3162 0.3274 0.103 Uiso 1 1 calc R . . C25 C 0.0683(4) 0.5658(9) 0.3202(4) 0.0839(19) Uani 1 1 d . . . H25 H 0.0125 0.5871 0.2919 0.101 Uiso 1 1 calc R . . C26 C 0.1240(3) 0.6970(7) 0.3401(3) 0.0725(16) Uani 1 1 d . . . H26 H 0.1055 0.8059 0.3243 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.04062(12) 0.03775(13) 0.03307(12) 0.00147(9) 0.01625(9) -0.00168(9) O1 0.0509(18) 0.059(2) 0.0391(17) -0.0104(15) 0.0174(14) -0.0136(16) O2 0.062(2) 0.059(2) 0.0327(18) 0.0017(14) 0.0151(15) -0.0220(16) N1 0.052(2) 0.043(2) 0.044(2) -0.0027(18) 0.0220(18) -0.0084(19) N2 0.050(2) 0.046(2) 0.036(2) -0.0013(17) 0.0178(17) -0.0064(18) N3 0.069(3) 0.064(3) 0.039(2) 0.0061(19) 0.023(2) -0.015(2) C1 0.057(3) 0.078(4) 0.079(4) 0.016(3) 0.026(3) 0.022(3) C2 0.041(3) 0.079(4) 0.088(4) -0.018(3) 0.028(3) -0.005(3) C3 0.065(3) 0.066(4) 0.105(5) 0.014(4) 0.058(4) 0.004(3) C4 0.056(3) 0.122(6) 0.054(3) -0.016(4) 0.032(3) 0.013(3) C5 0.058(3) 0.045(4) 0.115(5) -0.021(3) 0.040(4) 0.000(3) C6 0.100(4) 0.038(3) 0.075(4) 0.016(3) 0.042(4) 0.002(3) C7 0.099(4) 0.052(4) 0.058(3) 0.002(3) 0.035(3) 0.031(3) C8 0.068(4) 0.083(5) 0.117(6) 0.025(4) 0.048(4) 0.029(4) C9 0.080(5) 0.053(4) 0.092(5) 0.006(4) -0.034(4) 0.016(3) C10 0.143(6) 0.059(4) 0.039(3) 0.017(3) 0.027(4) 0.032(4) C11 0.087(4) 0.095(5) 0.049(3) -0.025(3) 0.027(3) -0.021(3) C12 0.078(4) 0.194(9) 0.081(5) -0.064(5) 0.022(4) -0.053(5) C13 0.075(4) 0.132(7) 0.067(4) -0.011(4) 0.011(3) -0.048(4) C14 0.056(3) 0.087(4) 0.071(4) -0.016(3) 0.028(3) -0.024(3) C15 0.084(4) 0.064(4) 0.068(4) -0.008(3) 0.032(3) -0.026(3) C16 0.049(3) 0.051(3) 0.050(3) -0.009(2) 0.020(2) -0.009(2) C17 0.055(3) 0.067(4) 0.046(3) -0.014(2) 0.011(2) -0.007(3) C18 0.053(3) 0.061(4) 0.034(3) -0.003(2) 0.013(2) 0.001(2) C19 0.085(4) 0.089(5) 0.033(3) 0.000(3) 0.012(3) -0.007(3) C20 0.041(2) 0.051(3) 0.037(3) -0.001(2) 0.016(2) -0.001(2) C21 0.066(3) 0.064(4) 0.037(3) 0.004(2) 0.032(2) -0.009(3) C22 0.080(4) 0.063(4) 0.050(3) -0.003(3) 0.035(3) -0.002(3) C23 0.115(5) 0.056(4) 0.076(4) -0.010(3) 0.061(4) -0.018(4) C24 0.101(5) 0.089(5) 0.089(5) -0.016(4) 0.060(4) -0.040(4) C25 0.063(4) 0.102(6) 0.089(5) 0.005(4) 0.034(3) -0.020(4) C26 0.069(4) 0.078(4) 0.073(4) 0.017(3) 0.032(3) -0.010(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 O2 2.236(3) . ? Dy1 O1 2.446(3) . ? Dy1 N1 2.516(3) . ? Dy1 C6 2.633(5) . ? Dy1 C5 2.638(5) . ? Dy1 C4 2.647(5) . ? Dy1 C10 2.651(5) . ? Dy1 C1 2.660(5) . ? Dy1 C3 2.660(5) . ? Dy1 C7 2.662(5) . ? Dy1 C8 2.667(5) . ? Dy1 C9 2.676(5) . ? O1 C11 1.441(5) . ? O1 C14 1.442(5) . ? O2 C20 1.267(5) . ? N1 C16 1.323(5) . ? N1 N2 1.376(5) . ? N2 C18 1.357(5) . ? N2 C20 1.444(5) . ? N3 C20 1.267(5) . ? N3 C21 1.411(6) . ? C1 C2 1.368(8) . ? C1 C5 1.373(7) . ? C2 C3 1.362(8) . ? C3 C4 1.402(8) . ? C4 C5 1.375(7) . ? C6 C10 1.357(8) . ? C6 C7 1.370(7) . ? C7 C8 1.356(8) . ? C8 C9 1.387(8) . ? C9 C10 1.372(9) . ? C11 C12 1.440(7) . ? C12 C13 1.412(7) . ? C13 C14 1.464(7) . ? C15 C16 1.488(6) . ? C16 C17 1.392(6) . ? C17 C18 1.346(6) . ? C18 C19 1.490(7) . ? C21 C22 1.379(7) . ? C21 C26 1.386(6) . ? C22 C23 1.381(8) . ? C23 C24 1.346(8) . ? C24 C25 1.368(9) . ? C25 C26 1.380(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 O2 Dy1 O1 74.44(10) . . ? O2 Dy1 N1 65.36(11) . . ? O1 Dy1 N1 139.79(10) . . ? O2 Dy1 C6 136.78(15) . . ? O1 Dy1 C6 118.87(15) . . ? N1 Dy1 C6 91.16(16) . . ? O2 Dy1 C5 95.79(17) . . ? O1 Dy1 C5 75.61(14) . . ? N1 Dy1 C5 108.74(16) . . ? C6 Dy1 C5 126.81(18) . . ? O2 Dy1 C4 125.26(19) . . ? O1 Dy1 C4 80.72(15) . . ? N1 Dy1 C4 123.64(15) . . ? C6 Dy1 C4 97.9(2) . . ? C5 Dy1 C4 30.17(16) . . ? O2 Dy1 C10 141.01(19) . . ? O1 Dy1 C10 90.22(18) . . ? N1 Dy1 C10 120.33(16) . . ? C6 Dy1 C10 29.75(17) . . ? C5 Dy1 C10 115.2(2) . . ? C4 Dy1 C10 85.7(2) . . ? O2 Dy1 C1 88.46(15) . . ? O1 Dy1 C1 101.56(17) . . ? N1 Dy1 C1 79.20(16) . . ? C6 Dy1 C1 123.85(19) . . ? C5 Dy1 C1 30.03(16) . . ? C4 Dy1 C1 49.94(18) . . ? C10 Dy1 C1 130.2(2) . . ? O2 Dy1 C3 137.78(15) . . ? O1 Dy1 C3 110.97(16) . . ? N1 Dy1 C3 99.88(17) . . ? C6 Dy1 C3 79.20(17) . . ? C5 Dy1 C3 49.60(17) . . ? C4 Dy1 C3 30.64(17) . . ? C10 Dy1 C3 81.1(2) . . ? C1 Dy1 C3 49.34(18) . . ? O2 Dy1 C7 106.81(15) . . ? O1 Dy1 C7 117.38(16) . . ? N1 Dy1 C7 75.07(14) . . ? C6 Dy1 C7 29.99(15) . . ? C5 Dy1 C7 156.12(19) . . ? C4 Dy1 C7 127.9(2) . . ? C10 Dy1 C7 48.97(17) . . ? C1 Dy1 C7 140.6(2) . . ? C3 Dy1 C7 106.72(19) . . ? O2 Dy1 C8 93.82(16) . . ? O1 Dy1 C8 88.65(19) . . ? N1 Dy1 C8 92.7(2) . . ? C6 Dy1 C8 49.44(18) . . ? C5 Dy1 C8 158.6(2) . . ? C4 Dy1 C8 133.8(2) . . ? C10 Dy1 C8 49.36(19) . . ? C1 Dy1 C8 169.8(2) . . ? C3 Dy1 C8 127.38(18) . . ? C7 Dy1 C8 29.47(18) . . ? O2 Dy1 C9 111.8(2) . . ? O1 Dy1 C9 71.83(16) . . ? N1 Dy1 C9 121.72(19) . . ? C6 Dy1 C9 49.36(19) . . ? C5 Dy1 C9 128.8(2) . . ? C4 Dy1 C9 105.2(2) . . ? C10 Dy1 C9 29.85(19) . . ? C1 Dy1 C9 155.1(2) . . ? C3 Dy1 C9 109.5(3) . . ? C7 Dy1 C9 48.98(18) . . ? C8 Dy1 C9 30.09(18) . . ? C11 O1 C14 108.4(4) . . ? C11 O1 Dy1 127.1(3) . . ? C14 O1 Dy1 123.0(3) . . ? C20 O2 Dy1 129.4(3) . . ? C16 N1 N2 105.2(3) . . ? C16 N1 Dy1 141.3(3) . . ? N2 N1 Dy1 112.5(2) . . ? C18 N2 N1 110.8(4) . . ? C18 N2 C20 131.9(4) . . ? N1 N2 C20 117.1(3) . . ? C20 N3 C21 118.8(4) . . ? C2 C1 C5 107.5(5) . . ? C2 C1 Dy1 76.4(3) . . ? C5 C1 Dy1 74.1(3) . . ? C3 C2 C1 108.9(5) . . ? C3 C2 Dy1 74.1(3) . . ? C1 C2 Dy1 74.0(3) . . ? C2 C3 C4 108.1(5) . . ? C2 C3 Dy1 76.4(3) . . ? C4 C3 Dy1 74.2(3) . . ? C5 C4 C3 106.3(5) . . ? C5 C4 Dy1 74.5(3) . . ? C3 C4 Dy1 75.2(3) . . ? C4 C5 C1 109.2(5) . . ? C4 C5 Dy1 75.3(3) . . ? C1 C5 Dy1 75.9(3) . . ? C10 C6 C7 107.7(6) . . ? C10 C6 Dy1 75.9(3) . . ? C7 C6 Dy1 76.2(3) . . ? C8 C7 C6 108.8(5) . . ? C8 C7 Dy1 75.5(3) . . ? C6 C7 Dy1 73.8(3) . . ? C7 C8 C9 107.6(6) . . ? C7 C8 Dy1 75.0(3) . . ? C9 C8 Dy1 75.3(3) . . ? C10 C9 C8 107.2(6) . . ? C10 C9 Dy1 74.1(3) . . ? C8 C9 Dy1 74.6(3) . . ? C6 C10 C9 108.7(6) . . ? C6 C10 Dy1 74.4(3) . . ? C9 C10 Dy1 76.1(3) . . ? C12 C11 O1 107.2(4) . . ? C13 C12 C11 109.1(5) . . ? C12 C13 C14 107.9(5) . . ? O1 C14 C13 107.0(4) . . ? N1 C16 C17 110.2(4) . . ? N1 C16 C15 121.8(4) . . ? C17 C16 C15 127.9(4) . . ? C18 C17 C16 107.3(4) . . ? C17 C18 N2 106.4(4) . . ? C17 C18 C19 129.0(5) . . ? N2 C18 C19 124.5(4) . . ? N3 C20 O2 131.5(4) . . ? N3 C20 N2 115.1(4) . . ? O2 C20 N2 113.4(4) . . ? C22 C21 C26 117.9(5) . . ? C22 C21 N3 119.0(5) . . ? C26 C21 N3 122.9(5) . . ? C21 C22 C23 120.8(6) . . ? C24 C23 C22 120.8(6) . . ? C23 C24 C25 119.6(6) . . ? C24 C25 C26 120.5(6) . . ? C25 C26 C21 120.4(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.837 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.079 data_f40618a _database_code_depnum_ccdc_archive 'CCDC 247295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 Dy2 N4 O4 S2' _chemical_formula_weight 1216.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.181(4) _cell_length_b 11.410(4) _cell_length_c 12.070(4) _cell_angle_alpha 115.574(4) _cell_angle_beta 101.615(4) _cell_angle_gamma 100.959(5) _cell_volume 1292.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.370 _cell_measurement_theta_max 26.959 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 2.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3802 _exptl_absorpt_correction_T_max 0.5211 _exptl_absorpt_process_details ? _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_% 12.62 _diffrn_reflns_number 5404 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4472 _reflns_number_gt 3854 _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. ; _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^)+(0.0858P)^2^+0.1121P] 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 4472 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Dy1 Dy 0.51488(3) -0.07258(3) 0.62268(3) 0.03580(16) Uani 1 1 d . . . S1 S 0.2233(2) 0.0966(3) 0.6327(3) 0.0566(6) Uani 1 1 d . . . N1 N 0.3094(6) 0.1446(6) 0.4528(6) 0.0404(15) Uani 1 1 d . . . N2 N 0.1706(11) 0.6526(10) 0.8695(9) 0.098(4) Uani 1 1 d . . . H2B H 0.0965 0.6639 0.8529 0.117 Uiso 1 1 calc R . . H2C H 0.2376 0.7220 0.9218 0.117 Uiso 1 1 calc R . . O1 O 0.4012(5) 0.0318(5) 0.5323(5) 0.0415(12) Uani 1 1 d . . . C1 C 0.4367(12) -0.3157(11) 0.5994(15) 0.088(4) Uani 1 1 d . . . H1A H 0.4886 -0.3548 0.6409 0.106 Uiso 1 1 calc R . . C2 C 0.4153(10) -0.3416(10) 0.4739(15) 0.079(4) Uani 1 1 d . . . H2A H 0.4514 -0.4002 0.4120 0.095 Uiso 1 1 calc R . . C3 C 0.3206(11) -0.2910(10) 0.4443(11) 0.072(3) Uani 1 1 d . . . H3A H 0.2784 -0.3071 0.3573 0.086 Uiso 1 1 calc R . . C4 C 0.2779(10) -0.2369(10) 0.5471(14) 0.073(3) Uani 1 1 d . . . H4A H 0.2003 -0.2089 0.5460 0.087 Uiso 1 1 calc R . . C5 C 0.3504(15) -0.2501(13) 0.6468(14) 0.100(5) Uani 1 1 d . . . H5A H 0.3311 -0.2357 0.7265 0.120 Uiso 1 1 calc R . . C6 C 0.5970(13) 0.0215(11) 0.8750(9) 0.073(3) Uani 1 1 d . . . H6A H 0.5778 -0.0312 0.9190 0.088 Uiso 1 1 calc R . . C7 C 0.5286(12) 0.1088(13) 0.8565(9) 0.077(3) Uani 1 1 d . . . H7A H 0.4559 0.1281 0.8867 0.092 Uiso 1 1 calc R . . C8 C 0.6042(12) 0.1840(10) 0.8148(10) 0.072(3) Uani 1 1 d . . . H8A H 0.5897 0.2627 0.8074 0.086 Uiso 1 1 calc R . . C9 C 0.7121(10) 0.1457(10) 0.8075(9) 0.062(3) Uani 1 1 d . . . H9A H 0.7867 0.1918 0.7942 0.074 Uiso 1 1 calc R . . C10 C 0.7059(10) 0.0445(11) 0.8440(9) 0.065(3) Uani 1 1 d . . . H10A H 0.7766 0.0086 0.8604 0.078 Uiso 1 1 calc R . . C11 C 0.3171(7) 0.0941(7) 0.5283(8) 0.0372(17) Uani 1 1 d . . . C12 C 0.2086(7) 0.1950(8) 0.4237(8) 0.0415(18) Uani 1 1 d . . . C13 C 0.0870(8) 0.1098(9) 0.3498(9) 0.051(2) Uani 1 1 d . . . H13A H 0.0681 0.0163 0.3202 0.061 Uiso 1 1 calc R . . C14 C -0.0092(9) 0.1626(11) 0.3185(9) 0.062(2) Uani 1 1 d . . . H14A H -0.0919 0.1034 0.2675 0.074 Uiso 1 1 calc R . . C15 C 0.0150(10) 0.2986(12) 0.3608(12) 0.068(3) Uani 1 1 d . . . H15A H -0.0503 0.3326 0.3400 0.082 Uiso 1 1 calc R . . C16 C 0.1352(11) 0.3833(12) 0.4332(13) 0.078(3) Uani 1 1 d . . . H16A H 0.1516 0.4767 0.4636 0.093 Uiso 1 1 calc R . . C17 C 0.2359(9) 0.3355(8) 0.4641(10) 0.057(2) Uani 1 1 d . . . H17A H 0.3192 0.3952 0.5104 0.068 Uiso 1 1 calc R . . C18 C 0.2091(9) 0.2621(9) 0.6948(9) 0.050(2) Uani 1 1 d . . . C19 C 0.0888(10) 0.2806(10) 0.6724(9) 0.060(2) Uani 1 1 d . . . H19A H 0.0154 0.2055 0.6195 0.072 Uiso 1 1 calc R . . C20 C 0.0788(11) 0.4125(11) 0.7300(10) 0.070(3) Uani 1 1 d . . . H20A H -0.0013 0.4246 0.7111 0.084 Uiso 1 1 calc R . . C21 C 0.1821(12) 0.5222(12) 0.8118(9) 0.069(3) Uani 1 1 d . . . C22 C 0.3011(12) 0.5029(12) 0.8337(10) 0.076(3) Uani 1 1 d . . . H22A H 0.3742 0.5779 0.8884 0.092 Uiso 1 1 calc R . . C23 C 0.3128(10) 0.3731(10) 0.7752(9) 0.064(3) Uani 1 1 d . . . H23A H 0.3937 0.3622 0.7917 0.076 Uiso 1 1 calc R . . O2 O 0.9310(19) 0.694(2) 0.9397(17) 0.201(7) Uiso 1 1 d . . . C24 C 0.869(4) 0.816(4) 0.966(3) 0.274(16) Uiso 1 1 d . . . H24A H 0.9076 0.8898 1.0552 0.328 Uiso 1 1 calc R . . H24B H 0.8791 0.8532 0.9083 0.328 Uiso 1 1 calc R . . C25 C 0.733(3) 0.747(4) 0.939(3) 0.230(13) Uiso 1 1 d . . . H25A H 0.7079 0.7964 1.0142 0.276 Uiso 1 1 calc R . . H25B H 0.6814 0.7527 0.8674 0.276 Uiso 1 1 calc R . . C26 C 0.704(3) 0.614(4) 0.909(3) 0.251(15) Uiso 1 1 d . . . H26A H 0.6450 0.5545 0.8212 0.301 Uiso 1 1 calc R . . H26B H 0.6650 0.5982 0.9686 0.301 Uiso 1 1 calc R . . C27 C 0.835(3) 0.588(3) 0.922(3) 0.197(10) Uiso 1 1 d . . . H27A H 0.8572 0.5719 0.9954 0.237 Uiso 1 1 calc R . . H27B H 0.8273 0.5056 0.8449 0.237 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0359(2) 0.0225(2) 0.0458(3) 0.01412(17) 0.01369(17) 0.00808(15) S1 0.0633(15) 0.0528(14) 0.0811(16) 0.0422(13) 0.0435(13) 0.0308(12) N1 0.034(4) 0.031(3) 0.052(4) 0.020(3) 0.009(3) 0.005(3) N2 0.111(9) 0.061(6) 0.072(6) -0.004(5) -0.007(6) 0.051(6) O1 0.040(3) 0.036(3) 0.053(3) 0.021(3) 0.019(3) 0.020(2) C1 0.078(9) 0.044(6) 0.132(12) 0.060(8) -0.007(8) -0.003(6) C2 0.042(6) 0.032(5) 0.139(12) 0.027(6) 0.028(7) -0.001(4) C3 0.065(7) 0.042(5) 0.075(7) 0.021(5) 0.006(6) -0.014(5) C4 0.042(6) 0.046(6) 0.126(10) 0.040(7) 0.031(6) 0.007(4) C5 0.115(12) 0.070(8) 0.103(10) 0.038(8) 0.063(9) -0.015(8) C6 0.107(10) 0.066(7) 0.042(5) 0.022(5) 0.022(6) 0.030(7) C7 0.076(8) 0.080(8) 0.049(6) 0.005(6) 0.022(6) 0.034(6) C8 0.098(9) 0.038(5) 0.053(6) 0.005(5) 0.009(6) 0.021(5) C9 0.062(7) 0.048(5) 0.048(5) 0.011(5) 0.000(5) 0.008(5) C10 0.060(7) 0.066(7) 0.054(6) 0.017(5) 0.010(5) 0.027(5) C11 0.030(4) 0.025(4) 0.051(5) 0.014(4) 0.014(3) 0.007(3) C12 0.033(4) 0.036(4) 0.066(5) 0.029(4) 0.021(4) 0.018(3) C13 0.038(5) 0.036(4) 0.067(6) 0.019(4) 0.014(4) 0.005(4) C14 0.038(5) 0.068(7) 0.069(6) 0.030(6) 0.008(5) 0.014(5) C15 0.046(6) 0.078(7) 0.113(9) 0.068(7) 0.031(6) 0.029(5) C16 0.072(8) 0.066(7) 0.136(10) 0.071(8) 0.046(7) 0.040(6) C17 0.044(5) 0.030(4) 0.093(7) 0.029(5) 0.020(5) 0.008(4) C18 0.055(6) 0.048(5) 0.051(5) 0.020(4) 0.025(4) 0.026(4) C19 0.050(6) 0.061(6) 0.061(6) 0.019(5) 0.017(5) 0.025(5) C20 0.071(7) 0.070(7) 0.060(6) 0.015(6) 0.020(6) 0.048(6) C21 0.085(8) 0.071(7) 0.039(5) 0.010(5) 0.015(5) 0.047(6) C22 0.069(7) 0.063(7) 0.056(6) 0.004(5) -0.003(5) 0.022(6) C23 0.061(6) 0.061(6) 0.064(6) 0.020(5) 0.017(5) 0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.315(5) . ? Dy1 O1 2.427(5) 2_656 ? Dy1 N1 2.461(6) 2_656 ? Dy1 C1 2.617(9) . ? Dy1 C5 2.623(10) . ? Dy1 C7 2.633(9) . ? Dy1 C6 2.636(9) . ? Dy1 C3 2.644(10) . ? Dy1 C10 2.650(10) . ? Dy1 C2 2.650(10) . ? Dy1 C4 2.651(10) . ? Dy1 C8 2.653(10) . ? S1 C18 1.758(9) . ? S1 C11 1.789(8) . ? N1 C11 1.269(10) . ? N1 C12 1.409(9) . ? N1 Dy1 2.461(6) 2_656 ? N2 C21 1.389(13) . ? N2 H2B 0.8600 . ? N2 H2C 0.8600 . ? O1 C11 1.287(8) . ? O1 Dy1 2.427(5) 2_656 ? C1 C2 1.372(17) . ? C1 C5 1.395(18) . ? C1 H1A 0.9800 . ? C2 C3 1.357(16) . ? C2 H2A 0.9800 . ? C3 C4 1.355(16) . ? C3 H3A 0.9800 . ? C4 C5 1.392(19) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C10 1.356(15) . ? C6 C7 1.429(15) . ? C6 H6A 0.9800 . ? C7 C8 1.404(17) . ? C7 H7A 0.9800 . ? C8 C9 1.364(15) . ? C8 H8A 0.9800 . ? C9 C10 1.397(14) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 Dy1 2.841(7) 2_656 ? C12 C13 1.360(11) . ? C12 C17 1.407(11) . ? C13 C14 1.394(12) . ? C13 H13A 0.9300 . ? C14 C15 1.357(14) . ? C14 H14A 0.9300 . ? C15 C16 1.344(15) . ? C15 H15A 0.9300 . ? C16 C17 1.395(13) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C23 1.348(14) . ? C18 C19 1.392(13) . ? C19 C20 1.398(13) . ? C19 H19A 0.9300 . ? C20 C21 1.341(16) . ? C20 H20A 0.9300 . ? C21 C22 1.381(15) . ? C22 C23 1.385(14) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? O2 C27 1.37(3) . ? O2 C24 1.61(3) . ? C24 C25 1.47(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.36(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.54(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 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 Dy1 O1 66.84(19) . 2_656 ? O1 Dy1 N1 119.97(19) . 2_656 ? O1 Dy1 N1 53.28(18) 2_656 2_656 ? O1 Dy1 C1 128.7(3) . . ? O1 Dy1 C1 123.2(4) 2_656 . ? N1 Dy1 C1 85.8(4) 2_656 . ? O1 Dy1 C5 108.2(5) . . ? O1 Dy1 C5 143.7(3) 2_656 . ? N1 Dy1 C5 116.6(4) 2_656 . ? C1 Dy1 C5 30.9(4) . . ? O1 Dy1 C7 90.6(3) . . ? O1 Dy1 C7 127.9(3) 2_656 . ? N1 Dy1 C7 128.0(3) 2_656 . ? C1 Dy1 C7 107.8(5) . . ? C5 Dy1 C7 86.9(4) . . ? O1 Dy1 C6 122.0(3) . . ? O1 Dy1 C6 135.8(3) 2_656 . ? N1 Dy1 C6 104.7(3) 2_656 . ? C1 Dy1 C6 86.7(4) . . ? C5 Dy1 C6 78.7(4) . . ? C7 Dy1 C6 31.5(3) . . ? O1 Dy1 C3 81.2(3) . . ? O1 Dy1 C3 94.7(3) 2_656 . ? N1 Dy1 C3 98.5(3) 2_656 . ? C1 Dy1 C3 49.7(4) . . ? C5 Dy1 C3 49.9(4) . . ? C7 Dy1 C3 129.0(4) . . ? C6 Dy1 C3 128.5(4) . . ? O1 Dy1 C10 128.2(3) . . ? O1 Dy1 C10 107.7(3) 2_656 . ? N1 Dy1 C10 78.4(3) 2_656 . ? C1 Dy1 C10 98.5(4) . . ? C5 Dy1 C10 102.8(5) . . ? C7 Dy1 C10 50.4(3) . . ? C6 Dy1 C10 29.7(3) . . ? C3 Dy1 C10 148.1(4) . . ? O1 Dy1 C2 109.0(3) . . ? O1 Dy1 C2 95.9(3) 2_656 . ? N1 Dy1 C2 75.7(3) 2_656 . ? C1 Dy1 C2 30.2(4) . . ? C5 Dy1 C2 50.1(4) . . ? C7 Dy1 C2 136.1(5) . . ? C6 Dy1 C2 116.7(4) . . ? C3 Dy1 C2 29.7(4) . . ? C10 Dy1 C2 122.8(4) . . ? O1 Dy1 C4 80.2(3) . . ? O1 Dy1 C4 120.2(3) 2_656 . ? N1 Dy1 C4 124.9(3) 2_656 . ? C1 Dy1 C4 50.3(4) . . ? C5 Dy1 C4 30.6(4) . . ? C7 Dy1 C4 99.3(4) . . ? C6 Dy1 C4 103.9(4) . . ? C3 Dy1 C4 29.7(3) . . ? C10 Dy1 C4 131.6(4) . . ? C2 Dy1 C4 49.4(3) . . ? O1 Dy1 C8 79.0(3) . . ? O1 Dy1 C8 97.3(3) 2_656 . ? N1 Dy1 C8 110.2(3) 2_656 . ? C1 Dy1 C8 136.5(5) . . ? C5 Dy1 C8 117.6(4) . . ? C7 Dy1 C8 30.8(4) . . ? C6 Dy1 C8 50.6(3) . . ? C3 Dy1 C8 150.6(4) . . ? C10 Dy1 C8 49.7(3) . . ? C2 Dy1 C8 166.5(4) . . ? C4 Dy1 C8 124.4(4) . . ? C18 S1 C11 103.0(4) . . ? C11 N1 C12 123.4(7) . . ? C11 N1 Dy1 93.7(5) . 2_656 ? C12 N1 Dy1 141.7(5) . 2_656 ? C21 N2 H2B 120.0 . . ? C21 N2 H2C 120.0 . . ? H2B N2 H2C 120.0 . . ? C11 O1 Dy1 151.5(5) . . ? C11 O1 Dy1 94.8(4) . 2_656 ? Dy1 O1 Dy1 113.16(19) . 2_656 ? C2 C1 C5 107.7(11) . . ? C2 C1 Dy1 76.3(6) . . ? C5 C1 Dy1 74.8(6) . . ? C2 C1 H1A 125.5 . . ? C5 C1 H1A 125.5 . . ? Dy1 C1 H1A 125.5 . . ? C3 C2 C1 108.2(11) . . ? C3 C2 Dy1 74.9(6) . . ? C1 C2 Dy1 73.6(6) . . ? C3 C2 H2A 125.5 . . ? C1 C2 H2A 125.5 . . ? Dy1 C2 H2A 125.5 . . ? C4 C3 C2 109.4(12) . . ? C4 C3 Dy1 75.4(6) . . ? C2 C3 Dy1 75.4(6) . . ? C4 C3 H3A 124.8 . . ? C2 C3 H3A 124.8 . . ? Dy1 C3 H3A 124.8 . . ? C3 C4 C5 107.8(11) . . ? C3 C4 Dy1 74.9(6) . . ? C5 C4 Dy1 73.6(6) . . ? C3 C4 H4A 125.7 . . ? C5 C4 H4A 125.7 . . ? Dy1 C4 H4A 125.7 . . ? C4 C5 C1 106.8(11) . . ? C4 C5 Dy1 75.8(6) . . ? C1 C5 Dy1 74.3(6) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? Dy1 C5 H5A 125.9 . . ? C10 C6 C7 107.9(10) . . ? C10 C6 Dy1 75.7(6) . . ? C7 C6 Dy1 74.2(5) . . ? C10 C6 H6A 125.5 . . ? C7 C6 H6A 125.5 . . ? Dy1 C6 H6A 125.5 . . ? C8 C7 C6 105.8(10) . . ? C8 C7 Dy1 75.4(5) . . ? C6 C7 Dy1 74.4(5) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? Dy1 C7 H7A 126.4 . . ? C9 C8 C7 109.4(10) . . ? C9 C8 Dy1 76.2(6) . . ? C7 C8 Dy1 73.8(6) . . ? C9 C8 H8A 124.9 . . ? C7 C8 H8A 124.9 . . ? Dy1 C8 H8A 124.9 . . ? C8 C9 C10 107.5(10) . . ? C8 C9 Dy1 74.1(6) . . ? C10 C9 Dy1 73.6(6) . . ? C8 C9 H9A 125.9 . . ? C10 C9 H9A 125.9 . . ? Dy1 C9 H9A 125.9 . . ? C6 C10 C9 109.5(10) . . ? C6 C10 Dy1 74.6(6) . . ? C9 C10 Dy1 75.9(5) . . ? C6 C10 H10A 124.8 . . ? C9 C10 H10A 124.8 . . ? Dy1 C10 H10A 124.8 . . ? N1 C11 O1 118.1(7) . . ? N1 C11 S1 127.9(6) . . ? O1 C11 S1 113.9(6) . . ? N1 C11 Dy1 59.8(4) . 2_656 ? O1 C11 Dy1 58.3(4) . 2_656 ? S1 C11 Dy1 172.2(4) . 2_656 ? C13 C12 C17 119.0(7) . . ? C13 C12 N1 121.5(7) . . ? C17 C12 N1 119.3(7) . . ? C12 C13 C14 120.0(8) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 121.5(9) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C16 C15 C14 118.8(9) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 122.0(10) . . ? C15 C16 H16A 119.0 . . ? C17 C16 H16A 119.0 . . ? C16 C17 C12 118.5(9) . . ? C16 C17 H17A 120.7 . . ? C12 C17 H17A 120.7 . . ? C23 C18 C19 118.4(8) . . ? C23 C18 S1 120.7(7) . . ? C19 C18 S1 120.6(8) . . ? C18 C19 C20 119.7(10) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C21 C20 C19 121.5(9) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 118.3(9) . . ? C20 C21 N2 120.9(10) . . ? C22 C21 N2 120.7(11) . . ? C21 C22 C23 120.7(11) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C18 C23 C22 121.2(9) . . ? C18 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C27 O2 C24 105(2) . . ? C25 C24 O2 102(3) . . ? C25 C24 H24A 111.3 . . ? O2 C24 H24A 111.3 . . ? C25 C24 H24B 111.3 . . ? O2 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? C26 C25 C24 115(3) . . ? C26 C25 H25A 108.4 . . ? C24 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? C24 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C25 C26 C27 104(3) . . ? C25 C26 H26A 111.0 . . ? C27 C26 H26A 111.0 . . ? C25 C26 H26B 111.0 . . ? C27 C26 H26B 111.0 . . ? H26A C26 H26B 109.0 . . ? O2 C27 C26 113(3) . . ? O2 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? O2 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? 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 O2 0.86 2.31 3.03(2) 140.8 1_455 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.668 _refine_diff_density_min -2.420 _refine_diff_density_rms 0.173 data_f50621a _database_code_depnum_ccdc_archive 'CCDC 282114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 Er N3 O2' _chemical_formula_weight 583.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 17.842(7) _cell_length_b 7.947(3) _cell_length_c 18.988(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.686(4) _cell_angle_gamma 90.00 _cell_volume 2446.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 946 _cell_measurement_theta_min 2.513 _cell_measurement_theta_max 24.964 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 3.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4236 _exptl_absorpt_correction_T_max 0.6251 _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_% 6.29 _diffrn_reflns_number 9780 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4319 _reflns_number_gt 3471 _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. ; _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^)+(0.0473P)^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 4319 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 0.223540(13) 0.45423(3) 0.292487(12) 0.03592(10) Uani 1 1 d . . . N1 N 0.2338(3) 0.7033(7) 0.0893(3) 0.0569(14) Uani 1 1 d . . . N2 N 0.1664(3) 0.4686(6) 0.1043(2) 0.0421(11) Uani 1 1 d . . . N3 N 0.1565(3) 0.3569(6) 0.1553(2) 0.0442(11) Uani 1 1 d . . . O1 O 0.2581(2) 0.6026(6) 0.21141(19) 0.0511(10) Uani 1 1 d . . . C1 C 0.1317(4) 0.6906(9) 0.3126(5) 0.071(2) Uani 1 1 d . . . H1A H 0.1471 0.8095 0.3224 0.086 Uiso 1 1 calc R . . C2 C 0.1421(4) 0.5703(11) 0.3699(4) 0.071(2) Uani 1 1 d . . . H2A H 0.1644 0.5901 0.4259 0.086 Uiso 1 1 calc R . . C3 C 0.0965(4) 0.4302(9) 0.3301(5) 0.0660(19) Uani 1 1 d . . . H3A H 0.0839 0.3320 0.3544 0.079 Uiso 1 1 calc R . . C4 C 0.0615(4) 0.4641(10) 0.2530(4) 0.0644(19) Uani 1 1 d . . . H4A H 0.0202 0.3937 0.2133 0.077 Uiso 1 1 calc R . . C5 C 0.0833(4) 0.6232(11) 0.2415(4) 0.0676(18) Uani 1 1 d . . . H5A H 0.0591 0.6859 0.1927 0.081 Uiso 1 1 calc R . . C6 C 0.2800(5) 0.1443(9) 0.2940(4) 0.0677(19) Uani 1 1 d . . . H6A H 0.2669 0.0721 0.2485 0.081 Uiso 1 1 calc R . . C7 C 0.3489(5) 0.2429(11) 0.3275(6) 0.087(3) Uani 1 1 d . . . H7A H 0.3931 0.2526 0.3099 0.104 Uiso 1 1 calc R . . C8 C 0.3534(6) 0.2964(10) 0.3978(6) 0.099(3) Uani 1 1 d . . . H8A H 0.4012 0.3511 0.4383 0.119 Uiso 1 1 calc R . . C9 C 0.2857(6) 0.2355(10) 0.4067(4) 0.081(2) Uani 1 1 d . . . H9A H 0.2780 0.2375 0.4548 0.097 Uiso 1 1 calc R . . C10 C 0.2410(4) 0.1418(8) 0.3426(4) 0.0659(18) Uani 1 1 d . . . H10A H 0.1956 0.0662 0.3375 0.079 Uiso 1 1 calc R . . C11 C 0.0752(4) 0.0972(9) 0.1430(4) 0.071(2) Uani 1 1 d . . . H11A H 0.1062 -0.0009 0.1422 0.107 Uiso 1 1 calc R . . H11B H 0.0176 0.0772 0.1123 0.107 Uiso 1 1 calc R . . H11C H 0.0840 0.1212 0.1955 0.107 Uiso 1 1 calc R . . C12 C 0.1031(3) 0.2444(8) 0.1105(3) 0.0487(14) Uani 1 1 d . . . C13 C 0.0787(4) 0.2845(8) 0.0330(3) 0.0555(16) Uani 1 1 d . . . H13 H 0.0412 0.2249 -0.0091 0.067 Uiso 1 1 calc R . . C14 C 0.1191(3) 0.4254(8) 0.0298(3) 0.0494(15) Uani 1 1 d . . . C15 C 0.1161(5) 0.5198(9) -0.0393(4) 0.071(2) Uani 1 1 d . . . H15A H 0.1012 0.6348 -0.0361 0.106 Uiso 1 1 calc R . . H15B H 0.0759 0.4694 -0.0855 0.106 Uiso 1 1 calc R . . H15C H 0.1693 0.5161 -0.0405 0.106 Uiso 1 1 calc R . . C16 C 0.2247(3) 0.6023(7) 0.1378(3) 0.0410(13) Uani 1 1 d . . . C17 C 0.2925(4) 0.8322(8) 0.1171(3) 0.0505(15) Uani 1 1 d . . . C18 C 0.2677(5) 0.9954(8) 0.0953(4) 0.0585(17) Uani 1 1 d . . . H18 H 0.2122 1.0182 0.0659 0.070 Uiso 1 1 calc R . . C19 C 0.3242(5) 1.1265(10) 0.1165(4) 0.074(2) Uani 1 1 d . . . H19 H 0.3060 1.2360 0.1021 0.088 Uiso 1 1 calc R . . C20 C 0.4053(5) 1.0965(11) 0.1579(5) 0.082(2) Uani 1 1 d . . . H20 H 0.4430 1.1848 0.1713 0.099 Uiso 1 1 calc R . . C21 C 0.4319(5) 0.9353(11) 0.1801(5) 0.084(2) Uani 1 1 d . . . H21 H 0.4878 0.9147 0.2091 0.100 Uiso 1 1 calc R . . C22 C 0.3768(4) 0.8037(9) 0.1600(4) 0.0700(19) Uani 1 1 d . . . H22 H 0.3959 0.6948 0.1751 0.084 Uiso 1 1 calc R . . O2 O 0.3216(2) 0.6645(5) 0.37130(19) 0.0487(10) Uani 1 1 d . . . C23 C 0.3876(4) 0.7294(10) 0.3539(4) 0.0677(19) Uani 1 1 d . . . H23A H 0.3660 0.8075 0.3108 0.081 Uiso 1 1 calc R . . H23B H 0.4151 0.6383 0.3401 0.081 Uiso 1 1 calc R . . C24 C 0.4461(5) 0.8161(12) 0.4242(4) 0.097(3) Uani 1 1 d . . . H24A H 0.5006 0.7668 0.4414 0.117 Uiso 1 1 calc R . . H24B H 0.4497 0.9344 0.4135 0.117 Uiso 1 1 calc R . . C25 C 0.4163(5) 0.7974(15) 0.4824(5) 0.121(4) Uani 1 1 d . . . H25A H 0.4116 0.9068 0.5028 0.145 Uiso 1 1 calc R . . H25B H 0.4546 0.7300 0.5247 0.145 Uiso 1 1 calc R . . C26 C 0.3357(4) 0.7155(10) 0.4488(3) 0.072(2) Uani 1 1 d . . . H26A H 0.3352 0.6183 0.4795 0.086 Uiso 1 1 calc R . . H26B H 0.2931 0.7929 0.4473 0.086 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 0.03867(15) 0.03735(16) 0.03512(15) 0.00111(11) 0.01876(11) -0.00176(12) N1 0.067(3) 0.063(4) 0.042(3) 0.006(2) 0.024(2) -0.017(3) N2 0.044(3) 0.047(3) 0.037(2) 0.000(2) 0.018(2) -0.006(2) N3 0.045(2) 0.049(3) 0.043(2) 0.001(2) 0.022(2) -0.008(2) O1 0.058(2) 0.061(3) 0.034(2) -0.0003(18) 0.0186(18) -0.022(2) C1 0.051(4) 0.052(4) 0.121(6) -0.030(4) 0.046(4) -0.003(3) C2 0.052(4) 0.115(7) 0.054(4) -0.014(4) 0.030(3) 0.013(4) C3 0.059(4) 0.063(5) 0.099(6) 0.011(4) 0.056(4) 0.002(4) C4 0.040(3) 0.078(5) 0.080(5) -0.022(4) 0.029(3) -0.006(4) C5 0.048(4) 0.073(5) 0.079(5) 0.011(4) 0.024(3) 0.016(4) C6 0.099(6) 0.048(4) 0.058(4) 0.001(3) 0.035(4) 0.031(4) C7 0.060(5) 0.086(6) 0.124(7) 0.032(6) 0.048(5) 0.027(5) C8 0.083(6) 0.057(5) 0.092(6) 0.005(5) -0.029(5) 0.020(5) C9 0.129(7) 0.061(5) 0.046(4) 0.018(4) 0.030(4) 0.029(5) C10 0.086(5) 0.036(4) 0.081(5) 0.015(4) 0.041(4) 0.006(4) C11 0.081(5) 0.060(5) 0.073(4) -0.008(4) 0.033(4) -0.026(4) C12 0.050(3) 0.049(4) 0.049(3) -0.011(3) 0.023(3) -0.011(3) C13 0.053(4) 0.059(4) 0.046(3) -0.013(3) 0.013(3) -0.007(3) C14 0.046(3) 0.063(4) 0.037(3) -0.006(3) 0.015(3) 0.001(3) C15 0.085(5) 0.083(5) 0.037(3) 0.004(3) 0.017(3) -0.004(4) C16 0.038(3) 0.046(3) 0.042(3) 0.000(3) 0.020(2) -0.001(3) C17 0.060(4) 0.065(4) 0.035(3) 0.001(3) 0.028(3) -0.013(3) C18 0.075(4) 0.061(5) 0.051(4) 0.000(3) 0.038(3) -0.002(4) C19 0.110(6) 0.052(4) 0.080(5) -0.010(4) 0.062(5) -0.014(5) C20 0.091(6) 0.087(6) 0.087(6) -0.014(5) 0.055(5) -0.037(5) C21 0.061(5) 0.103(7) 0.092(6) 0.007(5) 0.037(4) -0.016(5) C22 0.068(4) 0.067(5) 0.080(5) 0.014(4) 0.036(4) -0.008(4) O2 0.047(2) 0.059(3) 0.042(2) -0.0100(19) 0.0203(17) -0.014(2) C23 0.053(4) 0.084(5) 0.070(4) -0.016(4) 0.029(3) -0.026(4) C24 0.068(5) 0.134(8) 0.071(5) -0.006(5) 0.010(4) -0.047(5) C25 0.081(6) 0.199(12) 0.081(6) -0.068(7) 0.033(5) -0.056(7) C26 0.075(5) 0.089(6) 0.052(4) -0.019(4) 0.025(3) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.221(4) . ? Er1 O2 2.430(4) . ? Er1 N3 2.492(4) . ? Er1 C1 2.624(6) . ? Er1 C2 2.628(6) . ? Er1 C10 2.631(6) . ? Er1 C9 2.635(6) . ? Er1 C5 2.642(6) . ? Er1 C7 2.649(7) . ? Er1 C3 2.652(6) . ? Er1 C6 2.657(7) . ? Er1 C8 2.659(7) . ? N1 C16 1.281(6) . ? N1 C17 1.401(7) . ? N2 C14 1.353(7) . ? N2 N3 1.379(6) . ? N2 C16 1.437(7) . ? N3 C12 1.325(7) . ? O1 C16 1.270(6) . ? C1 C5 1.373(9) . ? C1 C2 1.401(9) . ? C2 C3 1.400(10) . ? C3 C4 1.356(10) . ? C4 C5 1.367(10) . ? C6 C10 1.370(9) . ? C6 C7 1.370(11) . ? C7 C8 1.370(11) . ? C8 C9 1.375(12) . ? C9 C10 1.364(10) . ? C11 C12 1.501(8) . ? C12 C13 1.386(7) . ? C13 C14 1.347(8) . ? C14 C15 1.492(8) . ? C17 C18 1.376(9) . ? C17 C22 1.399(8) . ? C18 C19 1.387(10) . ? C19 C20 1.349(11) . ? C20 C21 1.370(11) . ? C21 C22 1.376(9) . ? O2 C26 1.444(6) . ? O2 C23 1.446(7) . ? C23 C24 1.477(9) . ? C24 C25 1.419(10) . ? C25 C26 1.460(9) . ? 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 74.04(13) . . ? O1 Er1 N3 65.87(14) . . ? O2 Er1 N3 139.89(13) . . ? O1 Er1 C1 95.3(2) . . ? O2 Er1 C1 75.56(17) . . ? N3 Er1 C1 108.6(2) . . ? O1 Er1 C2 125.4(2) . . ? O2 Er1 C2 80.68(19) . . ? N3 Er1 C2 123.88(18) . . ? C1 Er1 C2 30.9(2) . . ? O1 Er1 C10 136.60(19) . . ? O2 Er1 C10 118.70(19) . . ? N3 Er1 C10 91.0(2) . . ? C1 Er1 C10 127.6(2) . . ? C2 Er1 C10 98.0(2) . . ? O1 Er1 C9 141.0(2) . . ? O2 Er1 C9 90.0(2) . . ? N3 Er1 C9 120.6(2) . . ? C1 Er1 C9 115.2(3) . . ? C2 Er1 C9 85.0(3) . . ? C10 Er1 C9 30.0(2) . . ? O1 Er1 C5 88.3(2) . . ? O2 Er1 C5 101.8(2) . . ? N3 Er1 C5 78.9(2) . . ? C1 Er1 C5 30.2(2) . . ? C2 Er1 C5 50.7(2) . . ? C10 Er1 C5 124.3(2) . . ? C9 Er1 C5 130.2(3) . . ? O1 Er1 C7 93.5(2) . . ? O2 Er1 C7 88.1(3) . . ? N3 Er1 C7 93.0(3) . . ? C1 Er1 C7 158.4(3) . . ? C2 Er1 C7 133.4(3) . . ? C10 Er1 C7 49.5(2) . . ? C9 Er1 C7 49.8(2) . . ? C5 Er1 C7 170.1(3) . . ? O1 Er1 C3 137.78(19) . . ? O2 Er1 C3 111.11(19) . . ? N3 Er1 C3 99.7(2) . . ? C1 Er1 C3 49.9(2) . . ? C2 Er1 C3 30.8(2) . . ? C10 Er1 C3 79.6(2) . . ? C9 Er1 C3 81.1(3) . . ? C5 Er1 C3 49.5(2) . . ? C7 Er1 C3 127.8(2) . . ? O1 Er1 C6 106.6(2) . . ? O2 Er1 C6 117.3(2) . . ? N3 Er1 C6 74.79(18) . . ? C1 Er1 C6 156.8(2) . . ? C2 Er1 C6 128.0(3) . . ? C10 Er1 C6 30.0(2) . . ? C9 Er1 C6 49.6(2) . . ? C5 Er1 C6 140.5(3) . . ? C7 Er1 C6 29.9(2) . . ? C3 Er1 C6 107.1(2) . . ? O1 Er1 C8 111.4(3) . . ? O2 Er1 C8 71.6(2) . . ? N3 Er1 C8 121.8(2) . . ? C1 Er1 C8 129.0(3) . . ? C2 Er1 C8 104.9(3) . . ? C10 Er1 C8 49.3(2) . . ? C9 Er1 C8 30.1(3) . . ? C5 Er1 C8 155.5(3) . . ? C7 Er1 C8 29.9(2) . . ? C3 Er1 C8 109.7(3) . . ? C6 Er1 C8 49.3(2) . . ? C16 N1 C17 119.1(5) . . ? C14 N2 N3 111.4(5) . . ? C14 N2 C16 132.1(5) . . ? N3 N2 C16 116.5(4) . . ? C12 N3 N2 104.6(4) . . ? C12 N3 Er1 141.5(4) . . ? N2 N3 Er1 112.9(3) . . ? C16 O1 Er1 128.6(3) . . ? C5 C1 C2 108.8(7) . . ? C5 C1 Er1 75.6(4) . . ? C2 C1 Er1 74.7(4) . . ? C3 C2 C1 105.4(6) . . ? C3 C2 Er1 75.6(4) . . ? C1 C2 Er1 74.4(3) . . ? C4 C3 C2 109.0(7) . . ? C4 C3 Er1 75.9(4) . . ? C2 C3 Er1 73.7(3) . . ? C3 C4 C5 108.9(7) . . ? C3 C4 Er1 74.6(4) . . ? C5 C4 Er1 74.0(4) . . ? C4 C5 C1 107.9(7) . . ? C4 C5 Er1 76.1(4) . . ? C1 C5 Er1 74.2(4) . . ? C10 C6 C7 107.7(7) . . ? C10 C6 Er1 74.0(4) . . ? C7 C6 Er1 74.8(4) . . ? C6 C7 C8 107.9(7) . . ? C6 C7 Er1 75.3(4) . . ? C8 C7 Er1 75.4(4) . . ? C7 C8 C9 108.2(7) . . ? C7 C8 Er1 74.7(4) . . ? C9 C8 Er1 74.0(4) . . ? C10 C9 C8 107.5(7) . . ? C10 C9 Er1 74.8(4) . . ? C8 C9 Er1 75.9(4) . . ? C9 C10 C6 108.7(7) . . ? C9 C10 Er1 75.1(4) . . ? C6 C10 Er1 76.0(4) . . ? N3 C12 C13 110.4(5) . . ? N3 C12 C11 122.4(5) . . ? C13 C12 C11 127.2(6) . . ? C14 C13 C12 107.6(5) . . ? C13 C14 N2 106.0(5) . . ? C13 C14 C15 129.4(6) . . ? N2 C14 C15 124.6(6) . . ? O1 C16 N1 130.4(5) . . ? O1 C16 N2 114.1(5) . . ? N1 C16 N2 115.5(5) . . ? C18 C17 C22 117.3(6) . . ? C18 C17 N1 118.7(6) . . ? C22 C17 N1 123.6(6) . . ? C17 C18 C19 121.2(7) . . ? C20 C19 C18 120.6(8) . . ? C19 C20 C21 119.6(8) . . ? C20 C21 C22 120.7(8) . . ? C21 C22 C17 120.6(7) . . ? C26 O2 C23 108.7(4) . . ? C26 O2 Er1 126.5(4) . . ? C23 O2 Er1 123.4(3) . . ? O2 C23 C24 107.1(5) . . ? C25 C24 C23 107.6(6) . . ? C24 C25 C26 109.1(6) . . ? O2 C26 C25 106.9(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.305 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.105 data_f50628a _database_code_depnum_ccdc_archive 'CCDC 282115' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58 N4 O4 S2 Y2' _chemical_formula_weight 1068.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.192(3) _cell_length_b 11.414(4) _cell_length_c 12.089(4) _cell_angle_alpha 115.648(4) _cell_angle_beta 101.544(4) _cell_angle_gamma 100.942(4) _cell_volume 1295.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 2.850 _cell_measurement_theta_max 22.489 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6500 _exptl_absorpt_correction_T_max 0.7188 _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_% 3.63 _diffrn_reflns_number 5455 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4500 _reflns_number_gt 3014 _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. ; _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^)+(0.0547P)^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 4500 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 0.51474(4) -0.07236(4) 0.62169(4) 0.04411(16) Uani 1 1 d . . . S1 S 0.22381(12) 0.09711(13) 0.63256(13) 0.0657(4) Uani 1 1 d . . . N1 N 0.3101(3) 0.1450(3) 0.4529(3) 0.0445(8) Uani 1 1 d . . . N2 N 0.1730(5) 0.6545(5) 0.8701(4) 0.1039(16) Uani 1 1 d . . . H2B H 0.0987 0.6656 0.8558 0.125 Uiso 1 1 calc R . . H2C H 0.2403 0.7242 0.9202 0.125 Uiso 1 1 calc R . . O1 O 0.4028(2) 0.0323(3) 0.5325(2) 0.0465(7) Uani 1 1 d . . . C1 C 0.4377(6) -0.3182(6) 0.5951(8) 0.092(2) Uani 1 1 d . . . H1A H 0.4897 -0.3592 0.6338 0.111 Uiso 1 1 calc R . . C2 C 0.4134(5) -0.3408(5) 0.4736(7) 0.0815(17) Uani 1 1 d . . . H2A H 0.4488 -0.3985 0.4103 0.098 Uiso 1 1 calc R . . C3 C 0.3188(5) -0.2904(5) 0.4449(6) 0.0770(15) Uani 1 1 d . . . H3A H 0.2749 -0.3070 0.3583 0.092 Uiso 1 1 calc R . . C4 C 0.2801(5) -0.2354(5) 0.5493(7) 0.0805(17) Uani 1 1 d . . . H4A H 0.2032 -0.2062 0.5499 0.097 Uiso 1 1 calc R . . C5 C 0.3498(7) -0.2514(7) 0.6458(6) 0.104(2) Uani 1 1 d . . . H5A H 0.3307 -0.2382 0.7252 0.125 Uiso 1 1 calc R . . C6 C 0.5968(6) 0.0234(6) 0.8740(4) 0.0810(16) Uani 1 1 d . . . H6A H 0.5769 -0.0281 0.9187 0.097 Uiso 1 1 calc R . . C7 C 0.5310(5) 0.1113(6) 0.8552(5) 0.0831(16) Uani 1 1 d . . . H7A H 0.4581 0.1307 0.8850 0.100 Uiso 1 1 calc R . . C8 C 0.6031(6) 0.1847(5) 0.8125(5) 0.0748(15) Uani 1 1 d . . . H8A H 0.5894 0.2639 0.8058 0.090 Uiso 1 1 calc R . . C9 C 0.7098(5) 0.1435(5) 0.8048(4) 0.0684(14) Uani 1 1 d . . . H9A H 0.7840 0.1883 0.7901 0.082 Uiso 1 1 calc R . . C10 C 0.7062(5) 0.0451(5) 0.8427(4) 0.0708(14) Uani 1 1 d . . . H10A H 0.7772 0.0101 0.8598 0.085 Uiso 1 1 calc R . . C11 C 0.3166(4) 0.0946(4) 0.5285(4) 0.0440(10) Uani 1 1 d . . . C12 C 0.2087(4) 0.1963(4) 0.4226(4) 0.0469(10) Uani 1 1 d . . . C13 C 0.0866(4) 0.1111(5) 0.3503(4) 0.0573(12) Uani 1 1 d . . . H13A H 0.0681 0.0178 0.3216 0.069 Uiso 1 1 calc R . . C14 C -0.0097(4) 0.1615(5) 0.3193(5) 0.0675(13) Uani 1 1 d . . . H14A H -0.0925 0.1024 0.2694 0.081 Uiso 1 1 calc R . . C15 C 0.0169(5) 0.2989(6) 0.3621(5) 0.0769(15) Uani 1 1 d . . . H15A H -0.0485 0.3335 0.3431 0.092 Uiso 1 1 calc R . . C16 C 0.1384(5) 0.3846(5) 0.4321(5) 0.0754(15) Uani 1 1 d . . . H16A H 0.1565 0.4778 0.4601 0.090 Uiso 1 1 calc R . . C17 C 0.2350(4) 0.3338(4) 0.4617(5) 0.0626(13) Uani 1 1 d . . . H17A H 0.3185 0.3925 0.5083 0.075 Uiso 1 1 calc R . . C18 C 0.2088(4) 0.2635(5) 0.6960(4) 0.0575(12) Uani 1 1 d . . . C19 C 0.0896(5) 0.2822(5) 0.6729(4) 0.0651(13) Uani 1 1 d . . . H19A H 0.0166 0.2075 0.6175 0.078 Uiso 1 1 calc R . . C20 C 0.0794(5) 0.4123(6) 0.7324(5) 0.0741(15) Uani 1 1 d . . . H20A H -0.0014 0.4233 0.7175 0.089 Uiso 1 1 calc R . . C21 C 0.1843(5) 0.5253(6) 0.8127(4) 0.0710(14) Uani 1 1 d . . . C22 C 0.3030(5) 0.5043(6) 0.8325(5) 0.0806(15) Uani 1 1 d . . . H22A H 0.3765 0.5792 0.8851 0.097 Uiso 1 1 calc R . . C23 C 0.3142(5) 0.3763(5) 0.7766(5) 0.0705(14) Uani 1 1 d . . . H23A H 0.3949 0.3653 0.7935 0.085 Uiso 1 1 calc R . . O2 O 0.9335(8) 0.6970(10) 0.9485(8) 0.230(3) Uiso 1 1 d . . . C24 C 0.8829(14) 0.8012(15) 0.9608(13) 0.257(6) Uiso 1 1 d . . . H24A H 0.8939 0.8241 0.8942 0.308 Uiso 1 1 calc R . . H24B H 0.9317 0.8814 1.0440 0.308 Uiso 1 1 calc R . . C25 C 0.7506(13) 0.7714(15) 0.9513(13) 0.247(6) Uiso 1 1 d . . . H25A H 0.7394 0.8193 1.0352 0.296 Uiso 1 1 calc R . . H25B H 0.7030 0.7949 0.8919 0.296 Uiso 1 1 calc R . . C26 C 0.7140(12) 0.6332(14) 0.9047(12) 0.237(5) Uiso 1 1 d . . . H26A H 0.6674 0.5857 0.8127 0.284 Uiso 1 1 calc R . . H26B H 0.6585 0.6086 0.9485 0.284 Uiso 1 1 calc R . . C27 C 0.8311(11) 0.5945(12) 0.9280(11) 0.215(5) Uiso 1 1 d . . . H27A H 0.8429 0.5813 1.0030 0.258 Uiso 1 1 calc R . . H27B H 0.8238 0.5095 0.8537 0.258 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 0.0450(2) 0.0402(2) 0.0538(3) 0.0247(2) 0.02119(19) 0.01734(17) S1 0.0736(8) 0.0721(8) 0.0924(9) 0.0547(8) 0.0550(7) 0.0425(7) N1 0.0414(19) 0.0403(19) 0.060(2) 0.0271(18) 0.0208(17) 0.0175(16) N2 0.115(4) 0.084(3) 0.075(3) 0.007(3) 0.003(3) 0.060(3) O1 0.0485(16) 0.0460(16) 0.0600(18) 0.0298(14) 0.0272(14) 0.0266(13) C1 0.081(4) 0.063(4) 0.133(6) 0.068(4) 0.003(4) 0.007(3) C2 0.053(3) 0.040(3) 0.123(5) 0.017(3) 0.033(4) 0.006(2) C3 0.060(4) 0.058(3) 0.084(4) 0.030(3) 0.002(3) -0.011(3) C4 0.054(3) 0.061(3) 0.139(6) 0.050(4) 0.049(4) 0.022(3) C5 0.119(6) 0.085(5) 0.097(5) 0.047(4) 0.055(5) -0.017(4) C6 0.105(4) 0.093(4) 0.051(3) 0.039(3) 0.025(3) 0.033(4) C7 0.078(4) 0.099(4) 0.053(3) 0.013(3) 0.024(3) 0.044(4) C8 0.095(4) 0.049(3) 0.060(3) 0.012(3) 0.013(3) 0.030(3) C9 0.064(3) 0.061(3) 0.052(3) 0.015(3) 0.005(3) 0.005(3) C10 0.066(3) 0.082(4) 0.053(3) 0.022(3) 0.010(3) 0.034(3) C11 0.040(2) 0.034(2) 0.054(3) 0.017(2) 0.018(2) 0.0108(19) C12 0.043(3) 0.046(3) 0.065(3) 0.031(2) 0.026(2) 0.020(2) C13 0.047(3) 0.053(3) 0.075(3) 0.033(3) 0.023(2) 0.015(2) C14 0.043(3) 0.082(4) 0.084(4) 0.045(3) 0.020(3) 0.023(3) C15 0.060(3) 0.101(4) 0.116(4) 0.080(4) 0.039(3) 0.048(3) C16 0.067(4) 0.064(3) 0.129(5) 0.065(3) 0.045(3) 0.033(3) C17 0.047(3) 0.049(3) 0.101(4) 0.043(3) 0.026(3) 0.017(2) C18 0.062(3) 0.067(3) 0.061(3) 0.034(3) 0.033(3) 0.036(3) C19 0.059(3) 0.076(4) 0.065(3) 0.030(3) 0.029(2) 0.032(3) C20 0.070(4) 0.091(4) 0.065(3) 0.029(3) 0.026(3) 0.053(3) C21 0.087(4) 0.073(4) 0.046(3) 0.018(3) 0.016(3) 0.043(3) C22 0.074(4) 0.076(4) 0.064(3) 0.016(3) 0.007(3) 0.030(3) C23 0.058(3) 0.077(4) 0.074(3) 0.027(3) 0.021(3) 0.038(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 2.303(3) . ? Y1 O1 2.408(2) 2_656 ? Y1 N1 2.454(3) 2_656 ? Y1 C1 2.629(5) . ? Y1 C7 2.631(5) . ? Y1 C4 2.634(5) . ? Y1 C6 2.637(5) . ? Y1 C5 2.640(5) . ? Y1 C2 2.645(5) . ? Y1 C3 2.649(5) . ? Y1 C8 2.652(5) . ? Y1 C9 2.653(4) . ? S1 C18 1.771(5) . ? S1 C11 1.779(4) . ? N1 C11 1.270(5) . ? N1 C12 1.428(5) . ? N1 Y1 2.454(3) 2_656 ? N2 C21 1.376(6) . ? O1 C11 1.308(4) . ? O1 Y1 2.408(2) 2_656 ? C1 C2 1.335(8) . ? C1 C5 1.430(8) . ? C2 C3 1.352(7) . ? C3 C4 1.345(7) . ? C4 C5 1.371(8) . ? C6 C10 1.362(7) . ? C6 C7 1.418(7) . ? C7 C8 1.380(7) . ? C8 C9 1.369(7) . ? C9 C10 1.382(7) . ? C11 Y1 2.842(4) 2_656 ? C12 C13 1.364(5) . ? C12 C17 1.377(5) . ? C13 C14 1.375(6) . ? C14 C15 1.369(7) . ? C15 C16 1.357(7) . ? C16 C17 1.377(6) . ? C18 C23 1.370(6) . ? C18 C19 1.383(6) . ? C19 C20 1.381(7) . ? C20 C21 1.368(7) . ? C21 C22 1.386(7) . ? C22 C23 1.362(7) . ? O2 C27 1.367(11) . ? O2 C24 1.376(14) . ? C24 C25 1.424(14) . ? C25 C26 1.366(14) . ? C26 C27 1.474(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 Y1 O1 66.54(10) . 2_656 ? O1 Y1 N1 120.16(10) . 2_656 ? O1 Y1 N1 53.75(10) 2_656 2_656 ? O1 Y1 C1 128.96(15) . . ? O1 Y1 C1 122.2(2) 2_656 . ? N1 Y1 C1 84.72(19) 2_656 . ? O1 Y1 C7 90.42(15) . . ? O1 Y1 C7 127.29(17) 2_656 . ? N1 Y1 C7 127.42(14) 2_656 . ? C1 Y1 C7 109.3(3) . . ? O1 Y1 C4 80.86(15) . . ? O1 Y1 C4 120.65(18) 2_656 . ? N1 Y1 C4 125.01(15) 2_656 . ? C1 Y1 C4 50.32(17) . . ? C7 Y1 C4 99.6(2) . . ? O1 Y1 C6 121.66(15) . . ? O1 Y1 C6 135.78(15) 2_656 . ? N1 Y1 C6 104.58(16) 2_656 . ? C1 Y1 C6 87.8(2) . . ? C7 Y1 C6 31.24(16) . . ? C4 Y1 C6 103.4(2) . . ? O1 Y1 C5 108.6(2) . . ? O1 Y1 C5 143.52(16) 2_656 . ? N1 Y1 C5 116.2(2) 2_656 . ? C1 Y1 C5 31.50(19) . . ? C7 Y1 C5 87.7(2) . . ? C4 Y1 C5 30.13(17) . . ? C6 Y1 C5 79.0(2) . . ? O1 Y1 C2 108.94(18) . . ? O1 Y1 C2 96.17(16) 2_656 . ? N1 Y1 C2 76.16(13) 2_656 . ? C1 Y1 C2 29.33(17) . . ? C7 Y1 C2 136.5(2) . . ? C4 Y1 C2 48.96(16) . . ? C6 Y1 C2 117.0(2) . . ? C5 Y1 C2 49.58(19) . . ? O1 Y1 C3 81.34(15) . . ? O1 Y1 C3 95.05(15) 2_656 . ? N1 Y1 C3 99.05(17) 2_656 . ? C1 Y1 C3 49.35(18) . . ? C7 Y1 C3 129.1(2) . . ? C4 Y1 C3 29.50(15) . . ? C6 Y1 C3 128.35(18) . . ? C5 Y1 C3 49.39(18) . . ? C2 Y1 C3 29.59(15) . . ? O1 Y1 C8 78.48(13) . . ? O1 Y1 C8 97.11(15) 2_656 . ? N1 Y1 C8 110.34(16) 2_656 . ? C1 Y1 C8 137.6(2) . . ? C7 Y1 C8 30.29(16) . . ? C4 Y1 C8 124.0(2) . . ? C6 Y1 C8 50.57(17) . . ? C5 Y1 C8 117.9(2) . . ? C2 Y1 C8 166.5(2) . . ? C3 Y1 C8 149.9(2) . . ? O1 Y1 C9 99.97(14) . . ? O1 Y1 C9 86.86(13) 2_656 . ? N1 Y1 C9 81.61(14) 2_656 . ? C1 Y1 C9 128.99(19) . . ? C7 Y1 C9 49.62(16) . . ? C4 Y1 C9 149.1(2) . . ? C6 Y1 C9 49.67(16) . . ? C5 Y1 C9 128.63(19) . . ? C2 Y1 C9 149.7(2) . . ? C3 Y1 C9 178.00(17) . . ? C8 Y1 C9 29.92(14) . . ? C18 S1 C11 103.3(2) . . ? C11 N1 C12 123.3(3) . . ? C11 N1 Y1 94.1(2) . 2_656 ? C12 N1 Y1 141.5(3) . 2_656 ? C11 O1 Y1 151.0(2) . . ? C11 O1 Y1 95.2(2) . 2_656 ? Y1 O1 Y1 113.46(10) . 2_656 ? C2 C1 C5 106.5(6) . . ? C2 C1 Y1 76.0(3) . . ? C5 C1 Y1 74.7(3) . . ? C1 C2 C3 110.2(6) . . ? C1 C2 Y1 74.7(3) . . ? C3 C2 Y1 75.4(3) . . ? C4 C3 C2 108.4(5) . . ? C4 C3 Y1 74.6(3) . . ? C2 C3 Y1 75.0(3) . . ? C3 C4 C5 108.9(5) . . ? C3 C4 Y1 75.9(3) . . ? C5 C4 Y1 75.2(3) . . ? C4 C5 C1 106.0(5) . . ? C4 C5 Y1 74.7(3) . . ? C1 C5 Y1 73.8(3) . . ? C10 C6 C7 107.4(5) . . ? C10 C6 Y1 75.8(3) . . ? C7 C6 Y1 74.2(3) . . ? C8 C7 C6 107.6(5) . . ? C8 C7 Y1 75.7(3) . . ? C6 C7 Y1 74.6(3) . . ? C9 C8 C7 107.5(5) . . ? C9 C8 Y1 75.1(3) . . ? C7 C8 Y1 74.0(3) . . ? C8 C9 C10 109.3(5) . . ? C8 C9 Y1 75.0(3) . . ? C10 C9 Y1 74.9(3) . . ? C6 C10 C9 108.2(5) . . ? C6 C10 Y1 74.4(3) . . ? C9 C10 Y1 74.9(3) . . ? N1 C11 O1 117.0(4) . . ? N1 C11 S1 128.8(3) . . ? O1 C11 S1 114.2(3) . . ? N1 C11 Y1 59.4(2) . 2_656 ? O1 C11 Y1 57.56(18) . 2_656 ? S1 C11 Y1 171.7(2) . 2_656 ? C13 C12 C17 118.9(4) . . ? C13 C12 N1 121.4(4) . . ? C17 C12 N1 119.7(4) . . ? C12 C13 C14 120.8(4) . . ? C15 C14 C13 119.8(4) . . ? C16 C15 C14 120.1(5) . . ? C15 C16 C17 120.0(5) . . ? C16 C17 C12 120.4(4) . . ? C23 C18 C19 118.4(4) . . ? C23 C18 S1 120.5(4) . . ? C19 C18 S1 120.9(4) . . ? C20 C19 C18 119.7(5) . . ? C21 C20 C19 122.1(5) . . ? C20 C21 N2 121.6(5) . . ? C20 C21 C22 117.1(5) . . ? N2 C21 C22 121.4(5) . . ? C23 C22 C21 121.4(5) . . ? C22 C23 C18 121.2(5) . . ? C27 O2 C24 103.5(10) . . ? O2 C24 C25 114.9(13) . . ? C26 C25 C24 101.9(13) . . ? C25 C26 C27 107.8(12) . . ? O2 C27 C26 108.4(10) . . ? 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 O2 0.86 2.35 3.072(10) 141.3 1_455 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.506 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.064