Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jie Zhang' _publ_contact_author_address ; Department of Chemistry Fudan University Handan Road No220 Shanghai 200433 CHINA ; _publ_contact_author_email ZHANGJIE@FUDAN.EDU.CN _publ_section_title ; Facile Construction of Novel Organolanthanide Square-Planar Metallomacrocycles via Ligand-Based Modification ; loop_ _publ_author_name 'Jie Zhang' 'Ruifang Cai' 'Zhen-Xia Chen' 'Liping Ma' 'Xigeng Zhou' data_51020a _database_code_depnum_ccdc_archive 'CCDC 625284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H120 N12 S4 Yb4' _chemical_formula_weight 2214.40 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 15.623(2) _cell_length_b 15.623(2) _cell_length_c 21.354(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5211.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4763 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 23.14 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 3.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4598 _exptl_absorpt_correction_T_max 0.5265 _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_% 5.37 _diffrn_reflns_number 25164 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5136 _reflns_number_gt 3741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.1027P)^2^+42.1143P] 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 0.06(4) _refine_ls_number_reflns 5136 _refine_ls_number_parameters 189 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2332 _refine_ls_wR_factor_gt 0.2119 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.74327(5) 0.17837(5) -0.03070(4) 0.0719(3) Uani 1 1 d . . . S1 S 0.8486(3) 0.3091(4) -0.0665(3) 0.0860(14) Uani 1 1 d . . . C1 C 0.6584(8) 0.1711(11) 0.0745(5) 0.141(13) Uani 1 1 d G . . H1A H 0.5969 0.1599 0.0786 0.169 Uiso 1 1 calc R . . C2 C 0.7239(10) 0.1097(7) 0.0805(4) 0.104(9) Uani 1 1 d G . . H2A H 0.7156 0.0486 0.0891 0.125 Uiso 1 1 calc R . . C3 C 0.8028(8) 0.1532(8) 0.0817(4) 0.135(14) Uani 1 1 d G . . H3A H 0.8584 0.1276 0.0919 0.162 Uiso 1 1 calc R . . C4 C 0.7861(9) 0.2415(8) 0.0764(4) 0.095(7) Uani 1 1 d G . . H4A H 0.8279 0.2873 0.0830 0.114 Uiso 1 1 calc R . . C5 C 0.6968(10) 0.2525(10) 0.0720(4) 0.097(7) Uani 1 1 d G . . H5A H 0.6665 0.3073 0.0749 0.116 Uiso 1 1 calc R . . C6 C 0.8585(8) 0.0765(10) -0.0656(6) 0.124(9) Uani 1 1 d GU . . H6A H 0.9158 0.0721 -0.0472 0.149 Uiso 1 1 calc R . . C7 C 0.7945(10) 0.0290(6) -0.0515(6) 0.21(3) Uani 1 1 d G . . H7A H 0.7952 -0.0178 -0.0209 0.248 Uiso 1 1 calc R . . C8 C 0.7357(10) 0.0420(9) -0.0923(6) 0.151(15) Uani 1 1 d G . . H8A H 0.6843 0.0068 -0.0977 0.182 Uiso 1 1 calc R . . C9 C 0.7634(11) 0.0975(9) -0.1315(6) 0.20(2) Uani 1 1 d G . . H9A H 0.7363 0.1118 -0.1716 0.238 Uiso 1 1 calc R . . C10 C 0.8393(11) 0.1188(10) -0.1150(7) 0.18(2) Uani 1 1 d G . . H10A H 0.8795 0.1522 -0.1404 0.220 Uiso 1 1 calc R . . C11 C 0.8228(7) 0.4011(7) -0.0222(6) 0.080(5) Uani 1 1 d G . . C12 C 0.7396(7) 0.4328(6) -0.0217(6) 0.089(6) Uani 1 1 d G . . H12A H 0.6969 0.4051 -0.0443 0.107 Uiso 1 1 calc R . . C13 C 0.7203(7) 0.5059(7) 0.0126(7) 0.085(6) Uani 1 1 d G . . H13A H 0.6647 0.5271 0.0130 0.102 Uiso 1 1 calc R . . C14 C 0.7841(7) 0.5474(8) 0.0464(6) 0.106(9) Uani 1 1 d G . . C15 C 0.8673(7) 0.5157(9) 0.0458(6) 0.098(7) Uani 1 1 d GU . . H15A H 0.9100 0.5435 0.0684 0.118 Uiso 1 1 calc R . . C16 C 0.8867(7) 0.4426(8) 0.0115(7) 0.101(8) Uani 1 1 d G . . H16A H 0.9423 0.4214 0.0111 0.121 Uiso 1 1 calc R . . N1 N 0.7632(11) 0.6238(10) 0.0806(7) 0.080(4) Uani 1 1 d . . . H1B H 0.7776 0.6733 0.0665 0.096 Uiso 1 1 calc R . . N2 N 0.6853(13) 0.6802(12) 0.1593(8) 0.094(5) Uani 1 1 d D . . N3 N 0.698(4) 0.5365(19) 0.1588(12) 0.30(4) Uani 1 1 d D . . H3B H 0.7164 0.4953 0.1355 0.366 Uiso 1 1 calc R . . C17 C 0.7201(16) 0.6161(15) 0.1361(11) 0.096(7) Uani 1 1 d . . . C18 C 0.6688(18) 0.689(2) 0.2238(9) 0.160(12) Uiso 1 1 d D . . H18A H 0.6862 0.6367 0.2455 0.192 Uiso 1 1 calc R . . C19 C 0.709(3) 0.763(3) 0.2543(17) 0.26(3) Uiso 1 1 d D . . H19A H 0.7701 0.7592 0.2492 0.393 Uiso 1 1 calc R . . H19B H 0.6954 0.7623 0.2981 0.393 Uiso 1 1 calc R . . H19C H 0.6884 0.8146 0.2357 0.393 Uiso 1 1 calc R . . C20 C 0.581(2) 0.709(4) 0.2400(19) 0.31(3) Uiso 1 1 d D . . H20A H 0.5438 0.6656 0.2225 0.464 Uiso 1 1 calc R . . H20B H 0.5656 0.7636 0.2234 0.464 Uiso 1 1 calc R . . H20C H 0.5747 0.7091 0.2847 0.464 Uiso 1 1 calc R . . C21 C 0.653(3) 0.508(3) 0.2116(19) 0.68(10) Uiso 1 1 d D . . H21A H 0.6047 0.5470 0.2178 0.818 Uiso 1 1 calc R . . C22 C 0.620(5) 0.422(4) 0.210(3) 0.38(4) Uiso 1 1 d D . . H22A H 0.5875 0.4140 0.1721 0.565 Uiso 1 1 calc R . . H22B H 0.5837 0.4127 0.2455 0.565 Uiso 1 1 calc R . . H22C H 0.6666 0.3820 0.2107 0.565 Uiso 1 1 calc R . . C23 C 0.700(5) 0.504(6) 0.2696(16) 0.46(5) Uiso 1 1 d D . . H23A H 0.7240 0.5595 0.2788 0.689 Uiso 1 1 calc R . . H23B H 0.7457 0.4631 0.2659 0.689 Uiso 1 1 calc R . . H23C H 0.6625 0.4874 0.3029 0.689 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 0.0890(6) 0.0686(5) 0.0582(4) 0.0030(4) 0.0018(5) 0.0260(4) S1 0.071(3) 0.094(4) 0.093(4) 0.006(3) 0.004(2) 0.009(3) C1 0.12(2) 0.26(4) 0.043(11) 0.017(17) -0.001(12) 0.02(3) C2 0.077(14) 0.14(2) 0.096(15) 0.060(14) -0.015(11) -0.079(15) C3 0.23(4) 0.12(2) 0.055(12) 0.023(12) 0.018(15) 0.11(2) C4 0.085(14) 0.125(19) 0.076(12) 0.048(13) 0.001(10) -0.018(13) C5 0.14(2) 0.075(13) 0.070(12) -0.028(11) 0.010(12) -0.022(15) C6 0.056(10) 0.148(18) 0.169(19) -0.049(14) -0.021(12) 0.036(12) C7 0.41(7) 0.091(18) 0.12(2) 0.055(16) 0.10(3) 0.14(3) C8 0.066(14) 0.072(16) 0.32(5) -0.06(2) 0.00(2) 0.001(12) C9 0.41(7) 0.11(2) 0.073(15) -0.018(16) 0.00(3) 0.15(4) C10 0.24(5) 0.092(19) 0.22(4) -0.03(2) 0.18(4) -0.05(2) C11 0.068(10) 0.077(11) 0.094(14) 0.013(10) -0.010(11) -0.011(9) C12 0.093(13) 0.045(8) 0.129(16) -0.021(10) -0.012(14) 0.048(9) C13 0.041(8) 0.088(12) 0.126(18) -0.031(11) 0.012(9) -0.024(8) C14 0.16(2) 0.073(12) 0.082(15) -0.022(10) 0.015(13) -0.051(14) C15 0.071(10) 0.121(13) 0.103(13) 0.056(11) 0.020(9) 0.065(10) C16 0.040(9) 0.097(15) 0.17(2) 0.037(15) -0.009(11) 0.024(9) N1 0.092(11) 0.070(9) 0.077(10) 0.000(7) -0.012(9) 0.008(8) N2 0.123(14) 0.078(11) 0.080(11) -0.001(9) 0.018(10) 0.001(11) N3 0.67(12) 0.14(3) 0.11(2) 0.036(18) -0.01(4) 0.05(5) C17 0.127(19) 0.074(13) 0.086(14) 0.004(11) 0.017(13) -0.036(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 N1 2.336(17) 3_565 ? Yb1 C8 2.506(11) . ? Yb1 C7 2.507(9) . ? Yb1 C9 2.515(11) . ? Yb1 C6 2.516(10) . ? Yb1 C10 2.521(11) . ? Yb1 C4 2.579(10) . ? Yb1 C5 2.583(10) . ? Yb1 C3 2.604(8) . ? Yb1 C1 2.611(11) . ? Yb1 C2 2.624(9) . ? Yb1 S1 2.732(6) . ? S1 C11 1.767(12) . ? C1 C5 1.408(4) . ? C1 C2 1.408(4) . ? C1 H1A 0.9800 . ? C2 C3 1.408(4) . ? C2 H2A 0.9800 . ? C3 C4 1.408(4) . ? C3 H3A 0.9800 . ? C4 C5 1.408(4) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C10 1.281(4) . ? C6 C7 1.281(4) . ? C6 H6A 0.9800 . ? C7 C8 1.281(4) . ? C7 H7A 0.9800 . ? C8 C9 1.281(4) . ? C8 H8A 0.9800 . ? C9 C10 1.281(4) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 C12 1.391(8) . ? C11 C16 1.391(8) . ? C12 C13 1.391(8) . ? C12 H12A 0.9300 . ? C13 C14 1.390(8) . ? C13 H13A 0.9300 . ? C14 C15 1.391(8) . ? C14 N1 1.437(19) . ? C14 Yb1 3.133(13) 4_655 ? C15 C16 1.391(8) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? N1 C17 1.37(3) . ? N1 Yb1 2.336(17) 4_655 ? N1 H1B 0.8600 . ? N2 C17 1.24(3) . ? N2 C18 1.409(10) . ? N3 C17 1.38(3) . ? N3 C21 1.402(10) . ? N3 H3B 0.8600 . ? C18 C20 1.449(19) . ? C18 C19 1.462(19) . ? C18 H18A 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.44(2) . ? C21 C23 1.44(2) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Yb1 C8 93.1(5) 3_565 . ? N1 Yb1 C7 122.5(5) 3_565 . ? C8 Yb1 C7 29.62(10) . . ? N1 Yb1 C9 84.6(5) 3_565 . ? C8 Yb1 C9 29.56(9) . . ? C7 Yb1 C9 48.76(15) . . ? N1 Yb1 C6 133.2(5) 3_565 . ? C8 Yb1 C6 48.76(15) . . ? C7 Yb1 C6 29.56(10) . . ? C9 Yb1 C6 48.67(14) . . ? N1 Yb1 C10 107.1(6) 3_565 . ? C8 Yb1 C10 48.70(14) . . ? C7 Yb1 C10 48.70(15) . . ? C9 Yb1 C10 29.48(8) . . ? C6 Yb1 C10 29.47(10) . . ? N1 Yb1 C4 117.6(5) 3_565 . ? C8 Yb1 C4 143.4(4) . . ? C7 Yb1 C4 115.5(4) . . ? C9 Yb1 C4 156.7(5) . . ? C6 Yb1 C4 108.6(4) . . ? C10 Yb1 C4 128.3(5) . . ? N1 Yb1 C5 89.3(5) 3_565 . ? C8 Yb1 C5 144.4(5) . . ? C7 Yb1 C5 131.1(4) . . ? C9 Yb1 C5 170.5(6) . . ? C6 Yb1 C5 137.4(4) . . ? C10 Yb1 C5 159.8(6) . . ? C4 Yb1 C5 31.66(9) . . ? N1 Yb1 C3 139.9(4) 3_565 . ? C8 Yb1 C3 111.8(4) . . ? C7 Yb1 C3 84.8(3) . . ? C9 Yb1 C3 131.9(4) . . ? C6 Yb1 C3 85.5(3) . . ? C10 Yb1 C3 113.0(4) . . ? C4 Yb1 C3 31.52(11) . . ? C5 Yb1 C3 52.11(15) . . ? N1 Yb1 C1 90.2(5) 3_565 . ? C8 Yb1 C1 112.9(5) . . ? C7 Yb1 C1 105.9(4) . . ? C9 Yb1 C1 141.0(6) . . ? C6 Yb1 C1 126.2(4) . . ? C10 Yb1 C1 154.2(4) . . ? C4 Yb1 C1 52.08(14) . . ? C5 Yb1 C1 31.46(10) . . ? C3 Yb1 C1 51.81(16) . . ? N1 Yb1 C2 118.7(5) 3_565 . ? C8 Yb1 C2 97.0(4) . . ? C7 Yb1 C2 79.4(3) . . ? C9 Yb1 C2 125.7(4) . . ? C6 Yb1 C2 95.3(3) . . ? C10 Yb1 C2 124.3(4) . . ? C4 Yb1 C2 51.93(16) . . ? C5 Yb1 C2 51.89(15) . . ? C3 Yb1 C2 31.25(11) . . ? C1 Yb1 C2 31.21(11) . . ? N1 Yb1 S1 93.5(4) 3_565 . ? C8 Yb1 S1 121.2(4) . . ? C7 Yb1 S1 117.0(4) . . ? C9 Yb1 S1 93.5(4) . . ? C6 Yb1 S1 87.7(4) . . ? C10 Yb1 S1 73.6(4) . . ? C4 Yb1 S1 78.8(3) . . ? C5 Yb1 S1 94.1(4) . . ? C3 Yb1 S1 99.0(3) . . ? C1 Yb1 S1 125.4(4) . . ? C2 Yb1 S1 129.0(3) . . ? C11 S1 Yb1 108.7(5) . . ? C5 C1 C2 108.0 . . ? C5 C1 Yb1 73.2(2) . . ? C2 C1 Yb1 74.9(2) . . ? C5 C1 H1A 125.6 . . ? C2 C1 H1A 125.6 . . ? Yb1 C1 H1A 125.6 . . ? C3 C2 C1 108.0 . . ? C3 C2 Yb1 73.6(3) . . ? C1 C2 Yb1 73.9(2) . . ? C3 C2 H2A 125.7 . . ? C1 C2 H2A 125.7 . . ? Yb1 C2 H2A 125.7 . . ? C4 C3 C2 108.0 . . ? C4 C3 Yb1 73.2(2) . . ? C2 C3 Yb1 75.2(3) . . ? C4 C3 H3A 125.6 . . ? C2 C3 H3A 125.6 . . ? Yb1 C3 H3A 125.6 . . ? C3 C4 C5 108.0 . . ? C3 C4 Yb1 75.2(2) . . ? C5 C4 Yb1 74.3(3) . . ? C3 C4 H4A 125.5 . . ? C5 C4 H4A 125.5 . . ? Yb1 C4 H4A 125.5 . . ? C1 C5 C4 108.0 . . ? C1 C5 Yb1 75.4(3) . . ? C4 C5 Yb1 74.0(3) . . ? C1 C5 H5A 125.5 . . ? C4 C5 H5A 125.5 . . ? Yb1 C5 H5A 125.5 . . ? C10 C6 C7 108.0 . . ? C10 C6 Yb1 75.5(2) . . ? C7 C6 Yb1 74.8(3) . . ? C10 C6 H6A 125.4 . . ? C7 C6 H6A 125.4 . . ? Yb1 C6 H6A 125.4 . . ? C6 C7 C8 108.0 . . ? C6 C7 Yb1 75.6(3) . . ? C8 C7 Yb1 75.2(3) . . ? C6 C7 H7A 125.4 . . ? C8 C7 H7A 125.4 . . ? Yb1 C7 H7A 125.4 . . ? C9 C8 C7 108.0 . . ? C9 C8 Yb1 75.6(2) . . ? C7 C8 Yb1 75.2(3) . . ? C9 C8 H8A 125.4 . . ? C7 C8 H8A 125.4 . . ? Yb1 C8 H8A 125.4 . . ? C8 C9 C10 108.0 . . ? C8 C9 Yb1 74.8(3) . . ? C10 C9 Yb1 75.5(3) . . ? C8 C9 H9A 125.4 . . ? C10 C9 H9A 125.4 . . ? Yb1 C9 H9A 125.4 . . ? C6 C10 C9 108.0 . . ? C6 C10 Yb1 75.0(2) . . ? C9 C10 Yb1 75.0(3) . . ? C6 C10 H10A 125.4 . . ? C9 C10 H10A 125.4 . . ? Yb1 C10 H10A 125.4 . . ? C12 C11 C16 120.0 . . ? C12 C11 S1 120.5(7) . . ? C16 C11 S1 119.5(7) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 N1 119.2(10) . . ? C15 C14 N1 120.8(10) . . ? C13 C14 Yb1 122.3(5) . 4_655 ? C15 C14 Yb1 99.9(5) . 4_655 ? N1 C14 Yb1 44.5(8) . 4_655 ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C11 C16 C15 120.0 . . ? C11 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 N1 C14 118.7(16) . . ? C17 N1 Yb1 131.1(13) . 4_655 ? C14 N1 Yb1 110.0(10) . 4_655 ? C17 N1 H1B 120.6 . . ? C14 N1 H1B 120.6 . . ? Yb1 N1 H1B 11.3 4_655 . ? C17 N2 C18 123(2) . . ? C17 N3 C21 134(4) . . ? C17 N3 H3B 113.1 . . ? C21 N3 H3B 113.1 . . ? N2 C17 N1 119.4(19) . . ? N2 C17 N3 119(3) . . ? N1 C17 N3 120(3) . . ? N2 C18 C20 115.3(18) . . ? N2 C18 C19 115.8(18) . . ? C20 C18 C19 98.0(16) . . ? N2 C18 H18A 109.0 . . ? C20 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 117(2) . . ? N3 C21 C23 117(2) . . ? C22 C21 C23 99.6(18) . . ? N3 C21 H21A 107.6 . . ? C22 C21 H21A 107.6 . . ? C23 C21 H21A 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.119 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.193 # Attachment 'complex 1b.cif' data_51222a _database_code_depnum_ccdc_archive 'CCDC 625285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H120 Er4 N12 S4' _chemical_formula_weight 2191.28 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P-42(1)c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 15.6756(10) _cell_length_b 15.6756(10) _cell_length_c 21.494(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5281.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5969 _cell_measurement_theta_min 2.295 _cell_measurement_theta_max 19.792 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 3.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6399 _exptl_absorpt_correction_T_max 0.7358 _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_% 4.85 _diffrn_reflns_number 27489 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4665 _reflns_number_gt 3346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0576P)^2^+148.9159P] 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 0.08(7) _refine_ls_number_reflns 4665 _refine_ls_number_parameters 189 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.1026 _refine_ls_wR_factor_ref 0.2766 _refine_ls_wR_factor_gt 0.2506 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.198 _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 0.25641(8) 0.82083(8) 1.03043(6) 0.0723(4) Uani 1 1 d . . . S1 S 0.1499(4) 0.6885(6) 1.0667(4) 0.083(2) Uani 1 1 d . . . C1 C 0.3424(12) 0.8260(15) 0.9259(7) 0.15(2) Uani 1 1 d G . . H1A H 0.4041 0.8343 0.9222 0.181 Uiso 1 1 calc R . . C2 C 0.2798(14) 0.8904(10) 0.9190(6) 0.092(12) Uani 1 1 d G . . H2A H 0.2911 0.9509 0.9108 0.111 Uiso 1 1 calc R . . C3 C 0.1988(12) 0.8504(13) 0.9163(5) 0.14(2) Uani 1 1 d G . . H3A H 0.1449 0.8786 0.9059 0.167 Uiso 1 1 calc R . . C4 C 0.2114(15) 0.7613(14) 0.9215(6) 0.126(17) Uani 1 1 d G . . H4A H 0.1679 0.7175 0.9142 0.151 Uiso 1 1 calc R . . C5 C 0.3001(17) 0.7461(13) 0.9274(6) 0.123(18) Uani 1 1 d G . . H5A H 0.3279 0.6903 0.9242 0.148 Uiso 1 1 calc R . . C6 C 0.1418(12) 0.9288(13) 1.0632(9) 0.113(12) Uani 1 1 d GU . . H6A H 0.0857 0.9354 1.0438 0.135 Uiso 1 1 calc R . . C7 C 0.2085(15) 0.9735(8) 1.0505(8) 0.106(11) Uani 1 1 d GU . . H7A H 0.2109 1.0203 1.0202 0.128 Uiso 1 1 calc R . . C8 C 0.2655(14) 0.9575(12) 1.0922(9) 0.122(12) Uani 1 1 d GU . . H8A H 0.3176 0.9908 1.0990 0.147 Uiso 1 1 calc R . . C9 C 0.2340(16) 0.9029(13) 1.1308(8) 0.141(15) Uani 1 1 d GU . . H9A H 0.2586 0.8880 1.1713 0.169 Uiso 1 1 calc R . . C10 C 0.1575(15) 0.8852(13) 1.1129(9) 0.16(2) Uani 1 1 d G . . H10A H 0.1152 0.8535 1.1372 0.190 Uiso 1 1 calc R . . C11 C 0.1786(11) 0.5980(11) 1.0210(8) 0.102(12) Uani 1 1 d G . . C12 C 0.2615(11) 0.5669(9) 1.0197(8) 0.072(7) Uani 1 1 d GU . . H12A H 0.3043 0.5946 1.0418 0.086 Uiso 1 1 calc R . . C13 C 0.2805(10) 0.4943(9) 0.9853(9) 0.091(10) Uani 1 1 d G . . H13A H 0.3360 0.4735 0.9844 0.109 Uiso 1 1 calc R . . C14 C 0.2167(11) 0.4529(11) 0.9522(8) 0.086(10) Uani 1 1 d G . . C15 C 0.1338(11) 0.4840(12) 0.9535(8) 0.085(9) Uani 1 1 d GU . . H15A H 0.0911 0.4563 0.9314 0.102 Uiso 1 1 calc R . . C16 C 0.1148(10) 0.5566(13) 0.9879(9) 0.095(11) Uani 1 1 d G . . H16A H 0.0592 0.5774 0.9888 0.114 Uiso 1 1 calc R . . N1 N 0.240(2) 0.3759(13) 0.9190(10) 0.087(7) Uani 1 1 d . . . H1B H 0.2272 0.3264 0.9338 0.104 Uiso 1 1 calc R . . N2 N 0.3148(19) 0.3145(18) 0.8410(10) 0.094(8) Uani 1 1 d D . . N3 N 0.298(3) 0.467(2) 0.8430(17) 0.21(3) Uani 1 1 d D . . H3B H 0.2720 0.5065 0.8633 0.250 Uiso 1 1 calc R . . C17 C 0.282(2) 0.384(2) 0.8631(15) 0.088(10) Uani 1 1 d . . . C18 C 0.329(2) 0.312(2) 0.7766(11) 0.163(18) Uiso 1 1 d D . . H18A H 0.3168 0.3690 0.7606 0.196 Uiso 1 1 calc R . . C19 C 0.279(3) 0.253(4) 0.740(2) 0.30(4) Uiso 1 1 d D . . H19A H 0.2196 0.2623 0.7486 0.457 Uiso 1 1 calc R . . H19B H 0.2943 0.1958 0.7510 0.457 Uiso 1 1 calc R . . H19C H 0.2901 0.2627 0.6968 0.457 Uiso 1 1 calc R . . C20 C 0.414(2) 0.290(4) 0.756(2) 0.25(3) Uiso 1 1 d D . . H20A H 0.4534 0.3313 0.7725 0.375 Uiso 1 1 calc R . . H20B H 0.4158 0.2912 0.7116 0.375 Uiso 1 1 calc R . . H20C H 0.4284 0.2345 0.7710 0.375 Uiso 1 1 calc R . . C21 C 0.350(3) 0.494(4) 0.794(2) 0.43(7) Uiso 1 1 d D . . H21A H 0.3889 0.4465 0.7853 0.513 Uiso 1 1 calc R . . C22 C 0.403(5) 0.568(6) 0.803(4) 0.43(7) Uiso 1 1 d D . . H22A H 0.4305 0.5640 0.8426 0.651 Uiso 1 1 calc R . . H22B H 0.3678 0.6180 0.8016 0.651 Uiso 1 1 calc R . . H22C H 0.4447 0.5701 0.7706 0.651 Uiso 1 1 calc R . . C23 C 0.310(5) 0.515(5) 0.7360(18) 0.34(5) Uiso 1 1 d D . . H23A H 0.2820 0.4654 0.7195 0.508 Uiso 1 1 calc R . . H23B H 0.3524 0.5345 0.7071 0.508 Uiso 1 1 calc R . . H23C H 0.2686 0.5594 0.7426 0.508 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 0.0860(9) 0.0682(7) 0.0628(6) 0.0045(7) 0.0020(8) 0.0234(6) S1 0.055(4) 0.095(6) 0.099(5) 0.009(5) 0.001(4) 0.015(4) C1 0.10(3) 0.29(6) 0.06(2) 0.06(3) 0.020(18) 0.10(4) C2 0.10(3) 0.10(2) 0.08(2) 0.048(18) 0.007(17) -0.04(2) C3 0.29(7) 0.09(2) 0.040(15) 0.020(15) 0.01(2) 0.12(3) C4 0.08(2) 0.22(5) 0.071(19) 0.06(3) 0.004(17) -0.05(3) C5 0.23(5) 0.07(2) 0.072(19) -0.040(18) 0.05(2) -0.06(3) C6 0.077(16) 0.116(19) 0.14(2) -0.040(16) -0.007(15) 0.027(14) C7 0.15(2) 0.053(13) 0.111(18) 0.029(13) 0.007(15) 0.021(14) C8 0.120(19) 0.093(17) 0.15(2) -0.047(16) 0.008(17) -0.015(15) C9 0.16(2) 0.14(2) 0.12(2) 0.010(16) -0.005(18) 0.037(18) C10 0.19(5) 0.07(2) 0.22(5) -0.03(3) 0.17(4) -0.03(2) C11 0.16(3) 0.083(19) 0.068(19) 0.027(16) 0.03(2) 0.07(2) C12 0.073(13) 0.037(9) 0.105(15) -0.021(11) -0.021(13) 0.049(10) C13 0.035(13) 0.10(2) 0.14(3) -0.04(2) 0.017(15) -0.028(13) C14 0.14(3) 0.040(13) 0.077(19) -0.037(12) 0.019(16) -0.021(15) C15 0.075(14) 0.080(14) 0.099(16) 0.044(13) 0.014(12) 0.046(12) C16 0.028(13) 0.11(3) 0.14(3) 0.00(2) -0.023(16) -0.001(14) N1 0.13(2) 0.059(13) 0.070(13) -0.013(11) -0.008(16) 0.029(15) N2 0.12(2) 0.085(17) 0.080(16) -0.010(15) 0.029(16) -0.002(17) N3 0.35(8) 0.11(3) 0.17(3) 0.07(3) 0.08(4) 0.01(3) C17 0.09(2) 0.09(2) 0.09(2) -0.001(18) 0.019(17) -0.042(18) _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 2.36(3) 3_567 ? Er1 C8 2.525(15) . ? Er1 C9 2.537(15) . ? Er1 C7 2.545(12) . ? Er1 C10 2.561(15) . ? Er1 C6 2.567(14) . ? Er1 C5 2.597(13) . ? Er1 C4 2.618(13) . ? Er1 C1 2.622(15) . ? Er1 C3 2.655(11) . ? Er1 C2 2.658(11) . ? Er1 S1 2.774(9) . ? S1 C11 1.783(17) . ? C1 C5 1.416(6) . ? C1 C2 1.416(6) . ? C1 H1A 0.9800 . ? C2 C3 1.416(6) . ? C2 H2A 0.9800 . ? C3 C4 1.416(6) . ? C3 H3A 0.9800 . ? C4 C5 1.416(6) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.289(5) . ? C6 C10 1.291(5) . ? C6 H6A 0.9800 . ? C7 C8 1.291(5) . ? C7 H7A 0.9800 . ? C8 C9 1.290(5) . ? C8 H8A 0.9800 . ? C9 C10 1.289(5) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 C12 1.388(10) . ? C11 C16 1.389(10) . ? C12 C13 1.389(10) . ? C12 H12A 0.9300 . ? C13 C14 1.389(10) . ? C13 H13A 0.9300 . ? C14 C15 1.388(10) . ? C14 N1 1.45(2) . ? C15 C16 1.389(10) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? N1 C17 1.38(4) . ? N1 Er1 2.36(3) 4_657 ? N1 H1B 0.8600 . ? N2 C17 1.30(4) . ? N2 C18 1.404(10) . ? N3 C17 1.39(4) . ? N3 C21 1.400(10) . ? N3 H3B 0.8600 . ? C18 C19 1.435(19) . ? C18 C20 1.437(19) . ? C18 H18A 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.43(2) . ? C21 C23 1.44(2) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 C8 93.1(9) 3_567 . ? N1 Er1 C9 85.5(8) 3_567 . ? C8 Er1 C9 29.53(12) . . ? N1 Er1 C7 122.2(9) 3_567 . ? C8 Er1 C7 29.49(14) . . ? C9 Er1 C7 48.6(2) . . ? N1 Er1 C10 108.6(8) 3_567 . ? C8 Er1 C10 48.39(18) . . ? C9 Er1 C10 29.28(11) . . ? C7 Er1 C10 48.3(2) . . ? N1 Er1 C6 133.8(7) 3_567 . ? C8 Er1 C6 48.3(2) . . ? C9 Er1 C6 48.3(2) . . ? C7 Er1 C6 29.20(15) . . ? C10 Er1 C6 29.16(15) . . ? N1 Er1 C5 90.1(7) 3_567 . ? C8 Er1 C5 144.7(7) . . ? C9 Er1 C5 172.1(10) . . ? C7 Er1 C5 130.2(5) . . ? C10 Er1 C5 158.0(9) . . ? C6 Er1 C5 135.7(7) . . ? N1 Er1 C4 118.8(8) 3_567 . ? C8 Er1 C4 142.0(6) . . ? C9 Er1 C4 154.7(8) . . ? C7 Er1 C4 114.0(6) . . ? C10 Er1 C4 126.6(8) . . ? C6 Er1 C4 107.0(7) . . ? C5 Er1 C4 31.51(12) . . ? N1 Er1 C1 89.9(7) 3_567 . ? C8 Er1 C1 113.3(7) . . ? C9 Er1 C1 141.7(8) . . ? C7 Er1 C1 105.5(5) . . ? C10 Er1 C1 153.1(6) . . ? C6 Er1 C1 125.1(6) . . ? C5 Er1 C1 31.49(13) . . ? C4 Er1 C1 51.87(19) . . ? N1 Er1 C3 139.8(6) 3_567 . ? C8 Er1 C3 110.9(5) . . ? C9 Er1 C3 130.5(6) . . ? C7 Er1 C3 83.8(4) . . ? C10 Er1 C3 111.4(7) . . ? C6 Er1 C3 84.3(5) . . ? C5 Er1 C3 51.7(2) . . ? C4 Er1 C3 31.14(15) . . ? C1 Er1 C3 51.5(2) . . ? N1 Er1 C2 118.0(7) 3_567 . ? C8 Er1 C2 96.8(5) . . ? C9 Er1 C2 125.3(6) . . ? C7 Er1 C2 78.9(4) . . ? C10 Er1 C2 123.1(6) . . ? C6 Er1 C2 94.2(5) . . ? C5 Er1 C2 51.7(2) . . ? C4 Er1 C2 51.5(2) . . ? C1 Er1 C2 31.11(15) . . ? C3 Er1 C2 30.92(14) . . ? N1 Er1 S1 92.8(7) 3_567 . ? C8 Er1 S1 121.4(5) . . ? C9 Er1 S1 93.3(6) . . ? C7 Er1 S1 118.6(5) . . ? C10 Er1 S1 74.7(5) . . ? C6 Er1 S1 89.7(6) . . ? C5 Er1 S1 93.5(6) . . ? C4 Er1 S1 79.8(5) . . ? C1 Er1 S1 125.0(5) . . ? C3 Er1 S1 100.7(5) . . ? C2 Er1 S1 130.0(5) . . ? C11 S1 Er1 106.7(7) . . ? C5 C1 C2 108.0 . . ? C5 C1 Er1 73.3(4) . . ? C2 C1 Er1 75.9(3) . . ? C5 C1 H1A 125.5 . . ? C2 C1 H1A 125.5 . . ? Er1 C1 H1A 125.5 . . ? C3 C2 C1 108.0 . . ? C3 C2 Er1 74.5(5) . . ? C1 C2 Er1 73.0(3) . . ? C3 C2 H2A 125.7 . . ? C1 C2 H2A 125.7 . . ? Er1 C2 H2A 125.7 . . ? C4 C3 C2 108.0 . . ? C4 C3 Er1 73.0(3) . . ? C2 C3 Er1 74.6(4) . . ? C4 C3 H3A 125.7 . . ? C2 C3 H3A 125.7 . . ? Er1 C3 H3A 125.7 . . ? C3 C4 C5 108.0 . . ? C3 C4 Er1 75.9(3) . . ? C5 C4 Er1 73.4(4) . . ? C3 C4 H4A 125.5 . . ? C5 C4 H4A 125.5 . . ? Er1 C4 H4A 125.5 . . ? C1 C5 C4 108.0 . . ? C1 C5 Er1 75.2(4) . . ? C4 C5 Er1 75.1(4) . . ? C1 C5 H5A 125.4 . . ? C4 C5 H5A 125.4 . . ? Er1 C5 H5A 125.4 . . ? C7 C6 C10 108.0 . . ? C7 C6 Er1 74.5(4) . . ? C10 C6 Er1 75.2(3) . . ? C7 C6 H6A 125.5 . . ? C10 C6 H6A 125.5 . . ? Er1 C6 H6A 125.5 . . ? C6 C7 C8 107.9 . . ? C6 C7 Er1 76.3(5) . . ? C8 C7 Er1 74.4(4) . . ? C6 C7 H7A 125.4 . . ? C8 C7 H7A 125.4 . . ? Er1 C7 H7A 125.4 . . ? C9 C8 C7 108.1 . . ? C9 C8 Er1 75.7(3) . . ? C7 C8 Er1 76.1(4) . . ? C9 C8 H8A 125.2 . . ? C7 C8 H8A 125.2 . . ? Er1 C8 H8A 125.2 . . ? C10 C9 C8 107.9 . . ? C10 C9 Er1 76.4(5) . . ? C8 C9 Er1 74.7(4) . . ? C10 C9 H9A 125.4 . . ? C8 C9 H9A 125.4 . . ? Er1 C9 H9A 125.4 . . ? C9 C10 C6 108.0 . . ? C9 C10 Er1 74.3(4) . . ? C6 C10 Er1 75.6(3) . . ? C9 C10 H10A 125.4 . . ? C6 C10 H10A 125.4 . . ? Er1 C10 H10A 125.4 . . ? C12 C11 C16 120.0 . . ? C12 C11 S1 121.8(11) . . ? C16 C11 S1 118.2(11) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.1 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 N1 122.3(17) . . ? C13 C14 N1 117.7(16) . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C11 C16 C15 120.0 . . ? C11 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 N1 C14 118(2) . . ? C17 N1 Er1 131.8(19) . 4_657 ? C14 N1 Er1 109.6(16) . 4_657 ? C17 N1 H1B 120.9 . . ? C14 N1 H1B 120.9 . . ? Er1 N1 H1B 12.9 4_657 . ? C17 N2 C18 117(3) . . ? C17 N3 C21 128(4) . . ? C17 N3 H3B 115.8 . . ? C21 N3 H3B 115.8 . . ? N2 C17 N1 116(3) . . ? N2 C17 N3 127(3) . . ? N1 C17 N3 116(3) . . ? N2 C18 C19 118(2) . . ? N2 C18 C20 117(2) . . ? C19 C18 C20 100.9(17) . . ? N2 C18 H18A 106.7 . . ? C19 C18 H18A 106.7 . . ? C20 C18 H18A 106.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 119(2) . . ? N3 C21 C23 118(2) . . ? C22 C21 C23 100.4(19) . . ? N3 C21 H21A 106.2 . . ? C22 C21 H21A 106.2 . . ? C23 C21 H21A 106.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.763 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.207 # Attachment 'complex 2a.cif' data_51117a _database_code_depnum_ccdc_archive 'CCDC 625286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H152 N12 S4 Yb4' _chemical_formula_weight 2534.90 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' 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' _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 29.400(8) _cell_length_b 16.934(4) _cell_length_c 30.963(12) _cell_angle_alpha 90.00 _cell_angle_beta 112.029(3) _cell_angle_gamma 90.00 _cell_volume 14291(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5335 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 19.94 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5104 _exptl_absorpt_coefficient_mu 2.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6882 _exptl_absorpt_correction_T_max 0.7745 _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_% 6.62 _diffrn_reflns_number 31371 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12565 _reflns_number_gt 7201 _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. ; _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^)+(0.1735P)^2^+165.6492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12565 _refine_ls_number_parameters 583 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.3094 _refine_ls_wR_factor_gt 0.2587 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.58362(2) 0.12751(4) 0.58756(2) 0.0588(2) Uani 1 1 d . . . Yb2 Yb 0.72053(2) 0.13197(4) 0.90580(2) 0.0613(3) Uani 1 1 d . . . S1 S 0.32179(14) 0.0748(3) 0.53823(13) 0.0691(10) Uani 1 1 d . . . S2 S 0.66111(13) 0.1844(2) 0.65582(13) 0.0645(9) Uani 1 1 d . . . N1 N 0.5260(4) 0.2102(8) 0.6025(4) 0.062(3) Uani 1 1 d . . . N2 N 0.5712(4) 0.3224(8) 0.6242(4) 0.071(3) Uani 1 1 d . . . H2B H 0.5923 0.3048 0.6134 0.085 Uiso 1 1 calc R . . N3 N 0.4868(4) 0.3304(8) 0.6066(5) 0.075(3) Uani 1 1 d . . . H3B H 0.4662 0.3091 0.6168 0.090 Uiso 1 1 calc R . . N4 N 0.6761(4) 0.0516(7) 0.8410(4) 0.059(3) Uani 1 1 d . . . N5 N 0.6684(10) -0.0588(11) 0.8805(6) 0.172(11) Uani 1 1 d . . . H5B H 0.6730 -0.0297 0.9045 0.207 Uiso 1 1 calc R . . N6 N 0.6482(11) -0.0651(11) 0.7969(6) 0.178(12) Uani 1 1 d . . . H6B H 0.6204 -0.0538 0.7754 0.214 Uiso 1 1 calc R . . C1 C 0.6151(8) 0.2392(12) 0.5482(6) 0.089(5) Uani 1 1 d . . . H1A H 0.6312 0.2880 0.5633 0.107 Uiso 1 1 calc R . . C2 C 0.5687(8) 0.2320(12) 0.5217(7) 0.090(6) Uani 1 1 d . . . H2A H 0.5446 0.2747 0.5147 0.108 Uiso 1 1 calc R . . C3 C 0.5591(7) 0.1555(14) 0.5013(6) 0.094(6) Uani 1 1 d . . . H3A H 0.5289 0.1383 0.4762 0.112 Uiso 1 1 calc R . . C4 C 0.6067(10) 0.1177(13) 0.5156(8) 0.106(7) Uani 1 1 d . . . H4A H 0.6150 0.0697 0.5025 0.127 Uiso 1 1 calc R . . C5 C 0.6385(8) 0.1706(17) 0.5444(8) 0.106(7) Uani 1 1 d . . . H5A H 0.6742 0.1641 0.5568 0.128 Uiso 1 1 calc R . . C6 C 0.5276(7) 0.0038(10) 0.5841(6) 0.076(4) Uani 1 1 d . . . H6A H 0.4917 0.0033 0.5718 0.091 Uiso 1 1 calc R . . C7 C 0.5555(7) -0.0187(9) 0.5616(6) 0.081(5) Uani 1 1 d . . . H7A H 0.5431 -0.0373 0.5292 0.098 Uiso 1 1 calc R . . C8 C 0.6072(7) -0.0203(10) 0.5929(7) 0.091(5) Uani 1 1 d . . . H8A H 0.6345 -0.0437 0.5866 0.109 Uiso 1 1 calc R . . C9 C 0.6064(8) -0.0002(10) 0.6377(6) 0.093(6) Uani 1 1 d . . . H9A H 0.6337 -0.0062 0.6678 0.112 Uiso 1 1 calc R . . C10 C 0.5587(7) 0.0169(9) 0.6311(6) 0.077(5) Uani 1 1 d . . . H10A H 0.5470 0.0259 0.6565 0.092 Uiso 1 1 calc R . . C11 C 0.3826(5) 0.1121(9) 0.5571(5) 0.063(4) Uani 1 1 d . . . C12 C 0.4001(6) 0.1423(9) 0.5258(5) 0.067(4) Uani 1 1 d . . . H12A H 0.3803 0.1411 0.4943 0.080 Uiso 1 1 calc R . . C13 C 0.4489(5) 0.1765(9) 0.5401(5) 0.066(4) Uani 1 1 d . . . H13A H 0.4604 0.1981 0.5185 0.080 Uiso 1 1 calc R . . C14 C 0.4774(5) 0.1757(9) 0.5866(5) 0.061(4) Uani 1 1 d . . . C15 C 0.4602(5) 0.1405(9) 0.6180(5) 0.068(4) Uani 1 1 d . . . H15A H 0.4805 0.1385 0.6493 0.082 Uiso 1 1 calc R . . C16 C 0.4152(5) 0.1094(10) 0.6043(5) 0.072(4) Uani 1 1 d . . . H16A H 0.4050 0.0856 0.6263 0.087 Uiso 1 1 calc R . . C17 C 0.5290(5) 0.2872(9) 0.6110(5) 0.063(4) Uani 1 1 d . . . C18 C 0.5864(6) 0.3926(9) 0.6575(6) 0.073(4) Uani 1 1 d . . . H18A H 0.5574 0.4189 0.6589 0.087 Uiso 1 1 calc R . . C19 C 0.6184(11) 0.3641(12) 0.7043(7) 0.136(10) Uani 1 1 d . . . H19A H 0.6498 0.3460 0.7046 0.163 Uiso 1 1 calc R . . H19B H 0.6028 0.3217 0.7148 0.163 Uiso 1 1 calc R . . C20 C 0.6246(14) 0.4426(17) 0.7360(10) 0.183(15) Uani 1 1 d . . . H20A H 0.5930 0.4664 0.7311 0.219 Uiso 1 1 calc R . . H20B H 0.6411 0.4307 0.7689 0.219 Uiso 1 1 calc R . . C21 C 0.6567(11) 0.4984(16) 0.7182(14) 0.175(13) Uani 1 1 d . . . H21A H 0.6672 0.5447 0.7380 0.210 Uiso 1 1 calc R . . H21B H 0.6856 0.4708 0.7180 0.210 Uiso 1 1 calc R . . C22 C 0.6272(10) 0.5194(15) 0.6743(9) 0.121(8) Uani 1 1 d . . . H22A H 0.6433 0.5596 0.6628 0.145 Uiso 1 1 calc R . . H22B H 0.5969 0.5414 0.6747 0.145 Uiso 1 1 calc R . . C23 C 0.6158(9) 0.4487(14) 0.6423(8) 0.123(8) Uani 1 1 d . . . H23A H 0.5976 0.4652 0.6105 0.148 Uiso 1 1 calc R . . H23B H 0.6460 0.4238 0.6437 0.148 Uiso 1 1 calc R . . C24 C 0.4754(6) 0.4097(10) 0.5858(6) 0.077(4) Uani 1 1 d . . . H24A H 0.5062 0.4391 0.5936 0.092 Uiso 1 1 calc R . . C25 C 0.4521(16) 0.4056(17) 0.5358(9) 0.23(2) Uani 1 1 d . . . H25A H 0.4224 0.3743 0.5271 0.279 Uiso 1 1 calc R . . H25B H 0.4739 0.3805 0.5230 0.279 Uiso 1 1 calc R . . C26 C 0.4397(18) 0.4883(18) 0.5162(10) 0.23(2) Uani 1 1 d . . . H26A H 0.4215 0.4859 0.4828 0.278 Uiso 1 1 calc R . . H26B H 0.4696 0.5180 0.5219 0.278 Uiso 1 1 calc R . . C27 C 0.4084(8) 0.5289(15) 0.5403(15) 0.174(16) Uani 1 1 d . . . H27A H 0.3959 0.5788 0.5250 0.209 Uiso 1 1 calc R . . H27B H 0.3806 0.4957 0.5377 0.209 Uiso 1 1 calc R . . C28 C 0.4366(13) 0.5422(19) 0.5869(12) 0.180(14) Uani 1 1 d . . . H28A H 0.4191 0.5726 0.6023 0.217 Uiso 1 1 calc R . . H28B H 0.4675 0.5677 0.5912 0.217 Uiso 1 1 calc R . . C29 C 0.4437(11) 0.4530(14) 0.6036(11) 0.159(11) Uani 1 1 d . . . H29A H 0.4576 0.4515 0.6374 0.190 Uiso 1 1 calc R . . H29B H 0.4119 0.4273 0.5933 0.190 Uiso 1 1 calc R . . C30 C 0.6978(9) 0.2544(11) 0.8479(7) 0.095(6) Uani 1 1 d . . . H30A H 0.6941 0.2560 0.8152 0.114 Uiso 1 1 calc R . . C31 C 0.7389(7) 0.2761(11) 0.8879(8) 0.093(6) Uani 1 1 d . . . H31A H 0.7704 0.2928 0.8868 0.112 Uiso 1 1 calc R . . C32 C 0.7279(7) 0.2811(9) 0.9275(6) 0.087(5) Uani 1 1 d . . . H32A H 0.7497 0.3029 0.9574 0.104 Uiso 1 1 calc R . . C33 C 0.6799(7) 0.2603(10) 0.9170(7) 0.081(5) Uani 1 1 d . . . H33A H 0.6609 0.2677 0.9368 0.097 Uiso 1 1 calc R . . C34 C 0.6603(7) 0.2445(9) 0.8668(8) 0.102(7) Uani 1 1 d . . . H34A H 0.6254 0.2368 0.8480 0.123 Uiso 1 1 calc R . . C35 C 0.8100(7) 0.1004(16) 0.9109(8) 0.112(7) Uani 1 1 d . . . H35A H 0.8239 0.1147 0.8877 0.135 Uiso 1 1 calc R . . C36 C 0.7891(7) 0.0278(14) 0.9143(7) 0.096(6) Uani 1 1 d . . . H36A H 0.7856 -0.0166 0.8929 0.116 Uiso 1 1 calc R . . C37 C 0.7819(6) 0.0232(11) 0.9539(7) 0.087(5) Uani 1 1 d . . . H37A H 0.7732 -0.0246 0.9668 0.104 Uiso 1 1 calc R . . C38 C 0.7973(6) 0.0927(14) 0.9771(7) 0.096(6) Uani 1 1 d . . . H38A H 0.8013 0.1020 1.0096 0.115 Uiso 1 1 calc R . . C39 C 0.8136(7) 0.1450(12) 0.9502(8) 0.099(6) Uani 1 1 d . . . H39A H 0.8321 0.1940 0.9609 0.119 Uiso 1 1 calc R . . C40 C 0.6637(5) 0.1485(8) 0.7099(5) 0.058(3) Uani 1 1 d . . . C41 C 0.7073(5) 0.1142(10) 0.7404(6) 0.074(4) Uani 1 1 d . . . H41A H 0.7342 0.1117 0.7316 0.088 Uiso 1 1 calc R . . C42 C 0.7115(5) 0.0840(9) 0.7834(5) 0.069(4) Uani 1 1 d . . . H42A H 0.7412 0.0632 0.8032 0.083 Uiso 1 1 calc R . . C43 C 0.6703(5) 0.0848(8) 0.7973(4) 0.056(3) Uani 1 1 d . . . C44 C 0.6288(5) 0.1209(9) 0.7683(5) 0.063(4) Uani 1 1 d . . . H44A H 0.6025 0.1261 0.7779 0.076 Uiso 1 1 calc R . . C45 C 0.6238(5) 0.1514(8) 0.7236(5) 0.062(4) Uani 1 1 d . . . H45A H 0.5941 0.1729 0.7039 0.074 Uiso 1 1 calc R . . C46 C 0.6694(11) -0.0202(13) 0.8392(6) 0.143(11) Uani 1 1 d . . . C47 C 0.6603(11) -0.1426(11) 0.8849(7) 0.116(8) Uani 1 1 d . . . H47A H 0.6502 -0.1704 0.8551 0.139 Uiso 1 1 calc R . . C48 C 0.6236(12) -0.1527(16) 0.9088(9) 0.149(11) Uani 1 1 d . . . H48A H 0.5919 -0.1322 0.8887 0.178 Uiso 1 1 calc R . . H48B H 0.6345 -0.1227 0.9376 0.178 Uiso 1 1 calc R . . C49 C 0.6178(10) -0.247(2) 0.9204(10) 0.148(11) Uani 1 1 d . . . H49A H 0.5979 -0.2518 0.9391 0.177 Uiso 1 1 calc R . . H49B H 0.6024 -0.2763 0.8918 0.177 Uiso 1 1 calc R . . C50 C 0.6696(14) -0.2772(14) 0.9471(9) 0.146(11) Uani 1 1 d . . . H50A H 0.6807 -0.2541 0.9780 0.176 Uiso 1 1 calc R . . H50B H 0.6672 -0.3337 0.9509 0.176 Uiso 1 1 calc R . . C51 C 0.7061(13) -0.2653(17) 0.9301(11) 0.157(11) Uani 1 1 d . . . H51A H 0.6993 -0.2953 0.9017 0.188 Uiso 1 1 calc R . . H51B H 0.7375 -0.2821 0.9528 0.188 Uiso 1 1 calc R . . C52 C 0.7072(10) -0.1744(15) 0.9201(10) 0.139(9) Uani 1 1 d . . . H52A H 0.7147 -0.1458 0.9491 0.167 Uiso 1 1 calc R . . H52B H 0.7335 -0.1643 0.9091 0.167 Uiso 1 1 calc R . . C53 C 0.6833(11) -0.1425(17) 0.7933(11) 0.139(9) Uiso 1 1 d D . . H53A H 0.6960 -0.1666 0.8243 0.167 Uiso 1 1 calc R . . C54 C 0.726(3) -0.126(4) 0.782(3) 0.59(8) Uiso 1 1 d D . . H54A H 0.7552 -0.1303 0.8096 0.705 Uiso 1 1 calc R . . H54B H 0.7237 -0.0728 0.7701 0.705 Uiso 1 1 calc R . . C55 C 0.7301(14) -0.181(2) 0.7467(15) 0.223(17) Uiso 1 1 d D . . H55A H 0.7560 -0.2172 0.7638 0.268 Uiso 1 1 calc R . . H55B H 0.7431 -0.1490 0.7277 0.268 Uiso 1 1 calc R . . C56 C 0.6912(14) -0.229(2) 0.7136(13) 0.209(15) Uiso 1 1 d D . . H56A H 0.7049 -0.2733 0.7025 0.251 Uiso 1 1 calc R . . H56B H 0.6705 -0.1983 0.6872 0.251 Uiso 1 1 calc R . . C57 C 0.6633(16) -0.257(3) 0.7419(16) 0.26(2) Uiso 1 1 d D . . H57A H 0.6359 -0.2888 0.7221 0.316 Uiso 1 1 calc R . . H57B H 0.6844 -0.2916 0.7663 0.316 Uiso 1 1 calc R . . C58 C 0.6440(15) -0.195(3) 0.7640(17) 0.29(2) Uiso 1 1 d D . . H58A H 0.6198 -0.1638 0.7399 0.347 Uiso 1 1 calc R . . H58B H 0.6280 -0.2191 0.7829 0.347 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 0.0628(4) 0.0659(4) 0.0496(4) -0.0036(3) 0.0233(3) 0.0028(3) Yb2 0.0508(4) 0.0667(4) 0.0594(4) -0.0157(3) 0.0125(3) 0.0006(3) S1 0.059(2) 0.084(3) 0.057(2) -0.0029(19) 0.0133(17) -0.0121(19) S2 0.053(2) 0.083(3) 0.056(2) 0.0031(18) 0.0182(17) -0.0008(18) N1 0.058(7) 0.081(9) 0.046(7) -0.001(6) 0.019(5) 0.000(6) N2 0.039(6) 0.084(9) 0.086(9) -0.020(7) 0.020(6) 0.000(6) N3 0.058(7) 0.081(9) 0.086(10) -0.002(7) 0.029(7) -0.001(7) N4 0.078(8) 0.055(7) 0.037(6) -0.005(5) 0.013(5) -0.012(6) N5 0.34(3) 0.083(13) 0.056(10) -0.015(9) 0.030(15) -0.051(16) N6 0.32(3) 0.092(13) 0.059(10) -0.010(9) 0.002(14) -0.047(17) C1 0.095(14) 0.092(14) 0.083(13) 0.000(10) 0.036(12) -0.016(11) C2 0.097(14) 0.107(15) 0.081(13) 0.038(11) 0.050(11) 0.042(12) C3 0.091(14) 0.132(17) 0.046(10) -0.010(10) 0.013(9) -0.015(12) C4 0.17(2) 0.106(15) 0.086(14) 0.009(12) 0.094(16) 0.017(15) C5 0.087(14) 0.15(2) 0.096(16) -0.007(15) 0.047(12) -0.008(14) C6 0.084(11) 0.069(10) 0.083(12) -0.007(8) 0.040(10) -0.003(8) C7 0.095(13) 0.066(10) 0.070(11) -0.019(8) 0.016(10) 0.001(9) C8 0.092(13) 0.068(11) 0.107(15) -0.001(10) 0.031(11) 0.018(9) C9 0.117(16) 0.067(11) 0.065(12) 0.012(8) 0.000(10) 0.001(10) C10 0.109(14) 0.056(9) 0.083(13) 0.006(8) 0.057(11) 0.008(9) C11 0.063(9) 0.073(10) 0.053(8) -0.006(7) 0.023(7) -0.008(7) C12 0.069(9) 0.074(10) 0.052(9) -0.013(7) 0.017(7) -0.001(7) C13 0.066(9) 0.067(10) 0.059(9) 0.001(7) 0.016(8) 0.001(7) C14 0.041(7) 0.078(10) 0.063(9) -0.019(7) 0.019(7) -0.005(6) C15 0.055(9) 0.097(12) 0.051(9) -0.003(8) 0.019(7) 0.003(8) C16 0.054(8) 0.107(12) 0.054(9) -0.009(8) 0.018(7) -0.008(8) C17 0.055(8) 0.060(9) 0.077(10) -0.017(7) 0.029(7) -0.013(7) C18 0.062(9) 0.066(9) 0.078(11) -0.007(8) 0.012(8) 0.001(7) C19 0.21(3) 0.083(14) 0.071(13) -0.018(10) 0.001(15) -0.040(14) C20 0.29(4) 0.13(2) 0.16(2) -0.09(2) 0.13(3) -0.11(3) C21 0.16(3) 0.098(19) 0.26(4) -0.09(2) 0.06(3) -0.061(18) C22 0.120(19) 0.12(2) 0.106(18) 0.008(15) 0.029(15) -0.025(15) C23 0.142(19) 0.120(18) 0.120(18) 0.000(14) 0.063(15) -0.055(15) C24 0.066(10) 0.067(11) 0.083(12) -0.003(8) 0.012(8) 0.000(8) C25 0.45(6) 0.12(2) 0.084(18) -0.001(15) 0.05(3) 0.14(3) C26 0.47(7) 0.11(2) 0.11(2) 0.011(17) 0.10(3) 0.05(3) C27 0.063(13) 0.093(18) 0.32(5) -0.03(2) 0.02(2) 0.020(12) C28 0.16(3) 0.12(2) 0.21(4) -0.02(2) 0.02(3) 0.05(2) C29 0.20(3) 0.090(17) 0.23(3) 0.043(18) 0.14(2) 0.067(18) C30 0.121(16) 0.077(13) 0.088(14) -0.006(10) 0.041(13) -0.012(11) C31 0.090(13) 0.073(12) 0.129(18) -0.005(11) 0.055(13) -0.023(10) C32 0.113(15) 0.056(10) 0.078(12) -0.023(8) 0.021(11) -0.016(9) C33 0.080(11) 0.072(11) 0.104(14) -0.013(9) 0.049(11) 0.019(9) C34 0.086(13) 0.037(8) 0.136(18) -0.004(9) -0.015(12) 0.022(8) C35 0.077(12) 0.16(2) 0.127(19) -0.031(16) 0.064(13) 0.007(14) C36 0.072(12) 0.120(17) 0.084(14) -0.043(12) 0.013(10) 0.020(11) C37 0.062(10) 0.088(13) 0.085(13) -0.007(10) -0.002(9) 0.014(9) C38 0.043(8) 0.140(18) 0.076(12) -0.030(12) -0.011(8) 0.006(10) C39 0.080(12) 0.086(13) 0.124(17) -0.041(12) 0.029(12) -0.016(10) C40 0.048(7) 0.066(9) 0.050(8) -0.015(6) 0.008(6) -0.002(6) C41 0.045(8) 0.097(12) 0.068(10) -0.003(8) 0.009(7) 0.008(7) C42 0.055(8) 0.089(11) 0.063(10) 0.015(8) 0.022(7) 0.031(8) C43 0.062(8) 0.061(8) 0.034(7) -0.009(6) 0.005(6) 0.007(6) C44 0.053(8) 0.088(11) 0.052(8) -0.003(7) 0.024(7) -0.009(7) C45 0.055(8) 0.065(9) 0.058(9) -0.010(7) 0.012(7) 0.002(7) C46 0.28(3) 0.088(15) 0.043(11) -0.011(10) 0.041(15) -0.049(17) C47 0.20(3) 0.066(12) 0.059(12) 0.003(9) 0.021(15) -0.018(13) C48 0.23(3) 0.11(2) 0.11(2) 0.003(15) 0.06(2) 0.02(2) C49 0.14(2) 0.20(3) 0.12(2) -0.07(2) 0.067(18) -0.02(2) C50 0.25(4) 0.079(15) 0.13(2) 0.008(14) 0.10(3) 0.012(19) C51 0.22(3) 0.13(2) 0.18(3) -0.002(19) 0.13(3) 0.02(2) C52 0.16(2) 0.11(2) 0.14(2) -0.002(17) 0.05(2) -0.041(17) _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 2.372(12) . ? Yb1 C3 2.537(17) . ? Yb1 C5 2.558(19) . ? Yb1 C4 2.567(16) . ? Yb1 C10 2.570(15) . ? Yb1 C8 2.585(17) . ? Yb1 C9 2.599(17) . ? Yb1 C1 2.600(18) . ? Yb1 C2 2.611(16) . ? Yb1 C7 2.639(16) . ? Yb1 S2 2.641(4) . ? Yb1 C6 2.642(17) . ? Yb2 N4 2.370(10) . ? Yb2 C33 2.565(15) . ? Yb2 C39 2.569(19) . ? Yb2 C34 2.573(15) . ? Yb2 C38 2.583(16) . ? Yb2 C32 2.602(15) . ? Yb2 C31 2.604(17) . ? Yb2 C37 2.616(17) . ? Yb2 C36 2.618(17) . ? Yb2 C35 2.630(17) . ? Yb2 C30 2.656(19) . ? Yb2 S1 2.666(4) 2_656 ? S1 C11 1.775(15) . ? S1 Yb2 2.666(4) 2_656 ? S2 C40 1.756(15) . ? N1 C17 1.326(18) . ? N1 C14 1.450(17) . ? N2 C17 1.296(17) . ? N2 C18 1.526(19) . ? N2 H2B 0.8600 . ? N3 C17 1.402(18) . ? N3 C24 1.47(2) . ? N3 H3B 0.8600 . ? N4 C46 1.23(2) . ? N4 C43 1.415(16) . ? N5 C46 1.44(3) . ? N5 C47 1.45(2) . ? N5 H5B 0.8600 . ? N6 C46 1.44(2) . ? N6 C53 1.69(3) . ? N6 H6B 0.8600 . ? C1 C2 1.31(2) . ? C1 C5 1.38(3) . ? C1 H1A 0.9800 . ? C2 C3 1.42(3) . ? C2 H2A 0.9800 . ? C3 C4 1.45(3) . ? C3 H3A 0.9800 . ? C4 C5 1.36(3) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.32(2) . ? C6 C10 1.42(2) . ? C6 H6A 0.9800 . ? C7 C8 1.46(2) . ? C7 H7A 0.9800 . ? C8 C9 1.44(3) . ? C8 H8A 0.9800 . ? C9 C10 1.37(2) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 C12 1.36(2) . ? C11 C16 1.42(2) . ? C12 C13 1.46(2) . ? C12 H12A 0.9300 . ? C13 C14 1.367(19) . ? C13 H13A 0.9300 . ? C14 C15 1.39(2) . ? C15 C16 1.34(2) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C23 1.48(2) . ? C18 C19 1.48(3) . ? C18 H18A 0.9800 . ? C19 C20 1.62(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.58(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.36(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.51(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.44(3) . ? C24 C29 1.45(3) . ? C24 H24A 0.9800 . ? C25 C26 1.51(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.55(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.39(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.58(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.42(3) . ? C30 C34 1.44(3) . ? C30 H30A 0.9800 . ? C31 C32 1.38(2) . ? C31 H31A 0.9800 . ? C32 C33 1.37(2) . ? C32 H32A 0.9800 . ? C33 C34 1.47(3) . ? C33 H33A 0.9800 . ? C34 H34A 0.9800 . ? C35 C36 1.40(3) . ? C35 C39 1.40(3) . ? C35 H35A 0.9800 . ? C36 C37 1.32(3) . ? C36 H36A 0.9800 . ? C37 C38 1.37(3) . ? C37 H37A 0.9800 . ? C38 C39 1.41(3) . ? C38 H38A 0.9800 . ? C39 H39A 0.9800 . ? C40 C45 1.389(19) . ? C40 C41 1.40(2) . ? C41 C42 1.39(2) . ? C41 H41A 0.9300 . ? C42 C43 1.431(19) . ? C42 H42A 0.9300 . ? C43 C44 1.359(19) . ? C44 C45 1.43(2) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C47 C52 1.50(3) . ? C47 C48 1.53(4) . ? C47 H47A 0.9800 . ? C48 C49 1.65(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.53(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.38(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.57(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.45(2) . ? C53 C58 1.468(19) . ? C53 H53A 0.9800 . ? C54 C55 1.46(2) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.470(19) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.484(19) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.481(19) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 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 C3 98.8(6) . . ? N1 Yb1 C5 124.7(7) . . ? C3 Yb1 C5 51.8(7) . . ? N1 Yb1 C4 130.4(6) . . ? C3 Yb1 C4 33.0(7) . . ? C5 Yb1 C4 30.7(7) . . ? N1 Yb1 C10 87.9(5) . . ? C3 Yb1 C10 131.6(7) . . ? C5 Yb1 C10 147.3(7) . . ? C4 Yb1 C10 129.0(6) . . ? N1 Yb1 C8 138.8(5) . . ? C3 Yb1 C8 102.2(7) . . ? C5 Yb1 C8 95.9(8) . . ? C4 Yb1 C8 80.9(7) . . ? C10 Yb1 C8 51.9(6) . . ? N1 Yb1 C9 114.7(6) . . ? C3 Yb1 C9 133.8(7) . . ? C5 Yb1 C9 118.5(8) . . ? C4 Yb1 C9 111.9(7) . . ? C10 Yb1 C9 30.7(6) . . ? C8 Yb1 C9 32.2(6) . . ? N1 Yb1 C1 93.8(6) . . ? C3 Yb1 C1 51.8(6) . . ? C5 Yb1 C1 31.0(6) . . ? C4 Yb1 C1 52.0(6) . . ? C10 Yb1 C1 175.9(7) . . ? C8 Yb1 C1 126.9(7) . . ? C9 Yb1 C1 145.9(7) . . ? N1 Yb1 C2 80.2(5) . . ? C3 Yb1 C2 32.0(6) . . ? C5 Yb1 C2 49.6(7) . . ? C4 Yb1 C2 52.2(6) . . ? C10 Yb1 C2 155.1(7) . . ? C8 Yb1 C2 131.9(6) . . ? C9 Yb1 C2 163.9(7) . . ? C1 Yb1 C2 29.0(5) . . ? N1 Yb1 C7 116.7(5) . . ? C3 Yb1 C7 85.5(7) . . ? C5 Yb1 C7 107.1(7) . . ? C4 Yb1 C7 80.2(7) . . ? C10 Yb1 C7 50.1(5) . . ? C8 Yb1 C7 32.5(5) . . ? C9 Yb1 C7 51.9(5) . . ? C1 Yb1 C7 131.7(6) . . ? C2 Yb1 C7 117.1(7) . . ? N1 Yb1 S2 95.3(3) . . ? C3 Yb1 S2 126.4(5) . . ? C5 Yb1 S2 77.9(5) . . ? C4 Yb1 S2 106.8(7) . . ? C10 Yb1 S2 100.1(5) . . ? C8 Yb1 S2 99.9(4) . . ? C9 Yb1 S2 82.7(4) . . ? C1 Yb1 S2 76.0(4) . . ? C2 Yb1 S2 102.7(6) . . ? C7 Yb1 S2 131.6(4) . . ? N1 Yb1 C6 89.8(5) . . ? C3 Yb1 C6 100.3(6) . . ? C5 Yb1 C6 135.3(7) . . ? C4 Yb1 C6 106.1(7) . . ? C10 Yb1 C6 31.5(5) . . ? C8 Yb1 C6 51.9(6) . . ? C9 Yb1 C6 51.8(6) . . ? C1 Yb1 C6 152.1(6) . . ? C2 Yb1 C6 125.9(7) . . ? C7 Yb1 C6 28.9(5) . . ? S2 Yb1 C6 131.3(4) . . ? N4 Yb2 C33 117.7(5) . . ? N4 Yb2 C39 129.8(5) . . ? C33 Yb2 C39 108.1(6) . . ? N4 Yb2 C34 88.0(5) . . ? C33 Yb2 C34 33.2(6) . . ? C39 Yb2 C34 126.5(7) . . ? N4 Yb2 C38 127.1(6) . . ? C33 Yb2 C38 113.8(6) . . ? C39 Yb2 C38 31.9(6) . . ? C34 Yb2 C38 144.9(6) . . ? N4 Yb2 C32 137.9(5) . . ? C33 Yb2 C32 30.7(5) . . ? C39 Yb2 C32 79.0(6) . . ? C34 Yb2 C32 51.6(6) . . ? C38 Yb2 C32 93.9(7) . . ? N4 Yb2 C31 116.8(6) . . ? C33 Yb2 C31 51.6(6) . . ? C39 Yb2 C31 76.7(7) . . ? C34 Yb2 C31 50.8(6) . . ? C38 Yb2 C31 103.8(7) . . ? C32 Yb2 C31 30.9(6) . . ? N4 Yb2 C37 96.9(5) . . ? C33 Yb2 C37 140.9(6) . . ? C39 Yb2 C37 52.2(6) . . ? C34 Yb2 C37 173.9(7) . . ? C38 Yb2 C37 30.4(6) . . ? C32 Yb2 C37 124.3(6) . . ? C31 Yb2 C37 128.8(6) . . ? N4 Yb2 C36 81.8(5) . . ? C33 Yb2 C36 159.7(6) . . ? C39 Yb2 C36 51.6(6) . . ? C34 Yb2 C36 156.2(8) . . ? C38 Yb2 C36 49.3(6) . . ? C32 Yb2 C36 130.0(7) . . ? C31 Yb2 C36 116.0(7) . . ? C37 Yb2 C36 29.3(6) . . ? N4 Yb2 C35 98.9(6) . . ? C33 Yb2 C35 132.1(7) . . ? C39 Yb2 C35 31.3(6) . . ? C34 Yb2 C35 132.5(8) . . ? C38 Yb2 C35 50.4(7) . . ? C32 Yb2 C35 101.4(8) . . ? C31 Yb2 C35 85.4(8) . . ? C37 Yb2 C35 50.4(7) . . ? C36 Yb2 C35 30.8(6) . . ? N4 Yb2 C30 87.6(5) . . ? C33 Yb2 C30 54.4(6) . . ? C39 Yb2 C30 104.1(7) . . ? C34 Yb2 C30 31.9(6) . . ? C38 Yb2 C30 134.1(7) . . ? C32 Yb2 C30 52.6(6) . . ? C31 Yb2 C30 31.3(6) . . ? C37 Yb2 C30 151.5(7) . . ? C36 Yb2 C30 125.7(8) . . ? C35 Yb2 C30 101.1(8) . . ? N4 Yb2 S1 95.6(3) . 2_656 ? C33 Yb2 S1 82.2(4) . 2_656 ? C39 Yb2 S1 110.2(6) . 2_656 ? C34 Yb2 S1 99.6(6) . 2_656 ? C38 Yb2 S1 79.8(5) . 2_656 ? C32 Yb2 S1 101.4(5) . 2_656 ? C31 Yb2 S1 131.6(5) . 2_656 ? C37 Yb2 S1 76.4(5) . 2_656 ? C36 Yb2 S1 102.7(6) . 2_656 ? C35 Yb2 S1 126.0(6) . 2_656 ? C30 Yb2 S1 131.4(5) . 2_656 ? C11 S1 Yb2 108.3(5) . 2_656 ? C40 S2 Yb1 110.6(5) . . ? C17 N1 C14 116.6(12) . . ? C17 N1 Yb1 128.3(9) . . ? C14 N1 Yb1 112.4(9) . . ? C17 N2 C18 125.1(12) . . ? C17 N2 H2B 117.4 . . ? C18 N2 H2B 117.4 . . ? C17 N3 C24 124.5(13) . . ? C17 N3 H3B 117.7 . . ? C24 N3 H3B 117.7 . . ? C46 N4 C43 113.0(13) . . ? C46 N4 Yb2 129.4(12) . . ? C43 N4 Yb2 114.3(8) . . ? C46 N5 C47 125.8(17) . . ? C46 N5 H5B 117.1 . . ? C47 N5 H5B 117.1 . . ? C46 N6 C53 114(2) . . ? C46 N6 H6B 123.1 . . ? C53 N6 H6B 123.1 . . ? C2 C1 C5 107.7(19) . . ? C2 C1 Yb1 75.9(11) . . ? C5 C1 Yb1 72.8(12) . . ? C2 C1 H1A 125.7 . . ? C5 C1 H1A 125.7 . . ? Yb1 C1 H1A 125.7 . . ? C1 C2 C3 110.6(17) . . ? C1 C2 Yb1 75.0(11) . . ? C3 C2 Yb1 71.1(10) . . ? C1 C2 H2A 124.6 . . ? C3 C2 H2A 124.6 . . ? Yb1 C2 H2A 124.6 . . ? C2 C3 C4 104.9(17) . . ? C2 C3 Yb1 76.8(10) . . ? C4 C3 Yb1 74.6(10) . . ? C2 C3 H3A 126.5 . . ? C4 C3 H3A 126.5 . . ? Yb1 C3 H3A 126.5 . . ? C5 C4 C3 105.0(19) . . ? C5 C4 Yb1 74.3(11) . . ? C3 C4 Yb1 72.4(9) . . ? C5 C4 H4A 127.0 . . ? C3 C4 H4A 127.0 . . ? Yb1 C4 H4A 127.0 . . ? C4 C5 C1 112(2) . . ? C4 C5 Yb1 75.0(11) . . ? C1 C5 Yb1 76.2(11) . . ? C4 C5 H5A 123.8 . . ? C1 C5 H5A 123.8 . . ? Yb1 C5 H5A 123.8 . . ? C7 C6 C10 107.5(16) . . ? C7 C6 Yb1 75.4(10) . . ? C10 C6 Yb1 71.4(9) . . ? C7 C6 H6A 125.9 . . ? C10 C6 H6A 125.9 . . ? Yb1 C6 H6A 125.9 . . ? C6 C7 C8 110.6(16) . . ? C6 C7 Yb1 75.7(10) . . ? C8 C7 Yb1 71.7(9) . . ? C6 C7 H7A 124.6 . . ? C8 C7 H7A 124.6 . . ? Yb1 C7 H7A 124.6 . . ? C9 C8 C7 104.4(17) . . ? C9 C8 Yb1 74.4(10) . . ? C7 C8 Yb1 75.7(9) . . ? C9 C8 H8A 126.8 . . ? C7 C8 H8A 126.8 . . ? Yb1 C8 H8A 126.8 . . ? C10 C9 C8 106.9(16) . . ? C10 C9 Yb1 73.4(10) . . ? C8 C9 Yb1 73.4(10) . . ? C10 C9 H9A 126.2 . . ? C8 C9 H9A 126.2 . . ? Yb1 C9 H9A 126.2 . . ? C9 C10 C6 110.5(15) . . ? C9 C10 Yb1 75.8(10) . . ? C6 C10 Yb1 77.0(9) . . ? C9 C10 H10A 124.2 . . ? C6 C10 H10A 124.2 . . ? Yb1 C10 H10A 124.2 . . ? C12 C11 C16 117.3(14) . . ? C12 C11 S1 120.3(12) . . ? C16 C11 S1 122.4(11) . . ? C11 C12 C13 121.9(14) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C14 C13 C12 117.4(14) . . ? C14 C13 H13A 121.3 . . ? C12 C13 H13A 121.3 . . ? C13 C14 C15 120.2(13) . . ? C13 C14 N1 119.3(13) . . ? C15 C14 N1 120.6(13) . . ? C16 C15 C14 121.7(14) . . ? C16 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? C15 C16 C11 121.2(14) . . ? C15 C16 H16A 119.4 . . ? C11 C16 H16A 119.4 . . ? N2 C17 N1 119.9(13) . . ? N2 C17 N3 119.8(13) . . ? N1 C17 N3 120.2(12) . . ? C23 C18 C19 106.8(17) . . ? C23 C18 N2 110.3(15) . . ? C19 C18 N2 109.0(14) . . ? C23 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? N2 C18 H18A 110.3 . . ? C18 C19 C20 102(2) . . ? C18 C19 H19A 111.3 . . ? C20 C19 H19A 111.3 . . ? C18 C19 H19B 111.3 . . ? C20 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? C21 C20 C19 103(2) . . ? C21 C20 H20A 111.2 . . ? C19 C20 H20A 111.2 . . ? C21 C20 H20B 111.2 . . ? C19 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? C22 C21 C20 105(2) . . ? 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 . . ? C21 C22 C23 111(2) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C18 C23 C22 108.3(18) . . ? C18 C23 H23A 110.0 . . ? C22 C23 H23A 110.0 . . ? C18 C23 H23B 110.0 . . ? C22 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C25 C24 C29 109(2) . . ? C25 C24 N3 111.4(16) . . ? C29 C24 N3 111.7(16) . . ? C25 C24 H24A 108.3 . . ? C29 C24 H24A 108.3 . . ? N3 C24 H24A 108.3 . . ? C24 C25 C26 109(2) . . ? C24 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? C24 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? C25 C26 C27 108(3) . . ? C25 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? C25 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C28 C27 C26 110(2) . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27B 109.6 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 C29 98(3) . . ? C27 C28 H28A 112.2 . . ? C29 C28 H28A 112.2 . . ? C27 C28 H28B 112.2 . . ? C29 C28 H28B 112.2 . . ? H28A C28 H28B 109.8 . . ? C24 C29 C28 113(2) . . ? C24 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C24 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C34 102.1(17) . . ? C31 C30 Yb2 72.3(11) . . ? C34 C30 Yb2 70.9(10) . . ? C31 C30 H30A 128.5 . . ? C34 C30 H30A 128.5 . . ? Yb2 C30 H30A 128.5 . . ? C32 C31 C30 112.5(17) . . ? C32 C31 Yb2 74.5(10) . . ? C30 C31 Yb2 76.4(10) . . ? C32 C31 H31A 123.5 . . ? C30 C31 H31A 123.5 . . ? Yb2 C31 H31A 123.5 . . ? C33 C32 C31 109.7(16) . . ? C33 C32 Yb2 73.2(9) . . ? C31 C32 Yb2 74.7(10) . . ? C33 C32 H32A 124.9 . . ? C31 C32 H32A 124.9 . . ? Yb2 C32 H32A 124.9 . . ? C32 C33 C34 105.0(16) . . ? C32 C33 Yb2 76.1(9) . . ? C34 C33 Yb2 73.7(8) . . ? C32 C33 H33A 126.6 . . ? C34 C33 H33A 126.6 . . ? Yb2 C33 H33A 126.6 . . ? C30 C34 C33 110.7(16) . . ? C30 C34 Yb2 77.2(11) . . ? C33 C34 Yb2 73.1(8) . . ? C30 C34 H34A 124.3 . . ? C33 C34 H34A 124.3 . . ? Yb2 C34 H34A 124.3 . . ? C36 C35 C39 108(2) . . ? C36 C35 Yb2 74.1(10) . . ? C39 C35 Yb2 72.0(10) . . ? C36 C35 H35A 126.0 . . ? C39 C35 H35A 126.0 . . ? Yb2 C35 H35A 126.0 . . ? C37 C36 C35 110.4(18) . . ? C37 C36 Yb2 75.3(10) . . ? C35 C36 Yb2 75.1(11) . . ? C37 C36 H36A 124.4 . . ? C35 C36 H36A 124.4 . . ? Yb2 C36 H36A 124.4 . . ? C36 C37 C38 108(2) . . ? C36 C37 Yb2 75.4(11) . . ? C38 C37 Yb2 73.4(11) . . ? C36 C37 H37A 125.8 . . ? C38 C37 H37A 125.8 . . ? Yb2 C37 H37A 125.8 . . ? C37 C38 C39 110.4(19) . . ? C37 C38 Yb2 76.1(9) . . ? C39 C38 Yb2 73.5(11) . . ? C37 C38 H38A 124.5 . . ? C39 C38 H38A 124.5 . . ? Yb2 C38 H38A 124.5 . . ? C35 C39 C38 104.0(19) . . ? C35 C39 Yb2 76.8(11) . . ? C38 C39 Yb2 74.6(10) . . ? C35 C39 H39A 126.8 . . ? C38 C39 H39A 126.8 . . ? Yb2 C39 H39A 126.8 . . ? C45 C40 C41 118.2(14) . . ? C45 C40 S2 122.6(11) . . ? C41 C40 S2 119.2(11) . . ? C42 C41 C40 121.9(14) . . ? C42 C41 H41A 119.0 . . ? C40 C41 H41A 119.0 . . ? C41 C42 C43 120.4(13) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C44 C43 N4 124.6(13) . . ? C44 C43 C42 117.1(13) . . ? N4 C43 C42 118.2(12) . . ? C43 C44 C45 122.9(13) . . ? C43 C44 H44A 118.5 . . ? C45 C44 H44A 118.5 . . ? C40 C45 C44 119.3(13) . . ? C40 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? N4 C46 N6 124.8(17) . . ? N4 C46 N5 117.7(17) . . ? N6 C46 N5 114.9(18) . . ? N5 C47 C52 106(2) . . ? N5 C47 C48 109(2) . . ? C52 C47 C48 103.4(19) . . ? N5 C47 H47A 112.5 . . ? C52 C47 H47A 112.5 . . ? C48 C47 H47A 112.5 . . ? C47 C48 C49 111(2) . . ? C47 C48 H48A 109.4 . . ? C49 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C49 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C48 106(2) . . ? C50 C49 H49A 110.5 . . ? C48 C49 H49A 110.5 . . ? C50 C49 H49B 110.5 . . ? C48 C49 H49B 110.5 . . ? H49A C49 H49B 108.7 . . ? C51 C50 C49 120(3) . . ? C51 C50 H50A 107.2 . . ? C49 C50 H50A 107.2 . . ? C51 C50 H50B 107.2 . . ? C49 C50 H50B 107.2 . . ? H50A C50 H50B 106.8 . . ? C50 C51 C52 107(2) . . ? C50 C51 H51A 110.3 . . ? C52 C51 H51A 110.3 . . ? C50 C51 H51B 110.3 . . ? C52 C51 H51B 110.3 . . ? H51A C51 H51B 108.5 . . ? C47 C52 C51 114(2) . . ? C47 C52 H52A 108.7 . . ? C51 C52 H52A 108.7 . . ? C47 C52 H52B 108.7 . . ? C51 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C54 C53 C58 121(4) . . ? C54 C53 N6 118(4) . . ? C58 C53 N6 99(3) . . ? C54 C53 H53A 106.0 . . ? C58 C53 H53A 106.0 . . ? N6 C53 H53A 106.0 . . ? C53 C54 C55 113(4) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 127(4) . . ? C54 C55 H55A 105.4 . . ? C56 C55 H55A 105.4 . . ? C54 C55 H55B 105.4 . . ? C56 C55 H55B 105.4 . . ? H55A C55 H55B 106.0 . . ? C55 C56 C57 103(3) . . ? C55 C56 H56A 111.2 . . ? C57 C56 H56A 111.1 . . ? C55 C56 H56B 111.2 . . ? C57 C56 H56B 111.2 . . ? H56A C56 H56B 109.1 . . ? C58 C57 C56 116(4) . . ? C58 C57 H57A 108.3 . . ? C56 C57 H57A 108.3 . . ? C58 C57 H57B 108.3 . . ? C56 C57 H57B 108.3 . . ? H57A C57 H57B 107.4 . . ? C53 C58 C57 112(4) . . ? C53 C58 H58A 109.3 . . ? C57 C58 H58A 109.3 . . ? C53 C58 H58B 109.3 . . ? C57 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.510 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.257 # Attachment 'complex 2b.cif' data_60106b _database_code_depnum_ccdc_archive 'CCDC 625287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H152 Er4 N12 S4' _chemical_formula_weight 2511.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 29.382(3) _cell_length_b 16.9543(19) _cell_length_c 30.951(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.8000(10) _cell_angle_gamma 90.00 _cell_volume 14315(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 794 _cell_measurement_theta_min 2.190 _cell_measurement_theta_max 23.906 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 2.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4847 _exptl_absorpt_correction_T_max 0.7939 _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_% 5.81 _diffrn_reflns_number 38109 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12608 _reflns_number_gt 7431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.1697P)^2^+186.7915P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12608 _refine_ls_number_parameters 583 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.3088 _refine_ls_wR_factor_gt 0.2444 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.080 _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 0.58403(2) 0.12695(4) 0.58786(2) 0.0558(2) Uani 1 1 d . . . Er2 Er 0.72012(2) 0.13066(4) 0.90582(2) 0.0582(2) Uani 1 1 d . . . S1 S 0.32216(13) 0.0728(2) 0.53781(12) 0.0662(9) Uani 1 1 d . . . S2 S 0.66170(12) 0.1843(2) 0.65592(12) 0.0637(9) Uani 1 1 d . . . N1 N 0.5252(4) 0.2106(7) 0.6030(4) 0.058(3) Uani 1 1 d . . . N2 N 0.5712(4) 0.3226(7) 0.6251(4) 0.070(3) Uani 1 1 d . . . H2B H 0.5923 0.3042 0.6145 0.084 Uiso 1 1 calc R . . N3 N 0.4868(4) 0.3295(7) 0.6070(4) 0.071(3) Uani 1 1 d . . . H3B H 0.4658 0.3086 0.6169 0.085 Uiso 1 1 calc R . . N4 N 0.6760(4) 0.0502(7) 0.8407(4) 0.060(3) Uani 1 1 d . . . N5 N 0.6667(10) -0.0602(10) 0.8789(5) 0.174(10) Uani 1 1 d U . . H5B H 0.6704 -0.0299 0.9023 0.209 Uiso 1 1 calc R . . N6 N 0.6517(10) -0.0668(10) 0.7970(5) 0.163(10) Uani 1 1 d . . . H6B H 0.6248 -0.0532 0.7750 0.196 Uiso 1 1 calc R . . C1 C 0.6156(8) 0.2395(12) 0.5468(6) 0.089(5) Uani 1 1 d . . . H1A H 0.6316 0.2887 0.5613 0.106 Uiso 1 1 calc R . . C2 C 0.5683(7) 0.2306(11) 0.5207(6) 0.083(5) Uani 1 1 d . . . H2A H 0.5439 0.2729 0.5137 0.099 Uiso 1 1 calc R . . C3 C 0.5594(7) 0.1581(15) 0.5016(6) 0.097(6) Uani 1 1 d . . . H3A H 0.5291 0.1411 0.4766 0.116 Uiso 1 1 calc R . . C4 C 0.6071(11) 0.1201(11) 0.5145(8) 0.106(7) Uani 1 1 d . . . H4A H 0.6149 0.0726 0.5006 0.128 Uiso 1 1 calc R . . C5 C 0.6390(7) 0.1711(16) 0.5432(7) 0.103(6) Uani 1 1 d . . . H5A H 0.6747 0.1646 0.5549 0.123 Uiso 1 1 calc R . . C6 C 0.5290(6) 0.0019(9) 0.5861(6) 0.080(4) Uani 1 1 d . . . H6A H 0.4931 0.0021 0.5746 0.095 Uiso 1 1 calc R . . C7 C 0.5559(7) -0.0199(9) 0.5606(6) 0.085(5) Uani 1 1 d . . . H7A H 0.5431 -0.0394 0.5285 0.102 Uiso 1 1 calc R . . C8 C 0.6063(8) -0.0226(10) 0.5925(8) 0.102(6) Uani 1 1 d . . . H8A H 0.6337 -0.0456 0.5860 0.123 Uiso 1 1 calc R . . C9 C 0.6069(8) -0.0024(10) 0.6374(6) 0.089(5) Uani 1 1 d . . . H9A H 0.6346 -0.0091 0.6670 0.106 Uiso 1 1 calc R . . C10 C 0.5596(8) 0.0141(9) 0.6322(6) 0.082(5) Uani 1 1 d . . . H10A H 0.5482 0.0221 0.6580 0.099 Uiso 1 1 calc R . . C11 C 0.3828(5) 0.1109(8) 0.5568(5) 0.060(3) Uani 1 1 d . . . C12 C 0.4006(5) 0.1423(9) 0.5257(5) 0.066(4) Uani 1 1 d . . . H12A H 0.3809 0.1424 0.4942 0.079 Uiso 1 1 calc R . . C13 C 0.4482(5) 0.1747(8) 0.5400(5) 0.061(3) Uani 1 1 d . . . H13A H 0.4602 0.1949 0.5184 0.074 Uiso 1 1 calc R . . C14 C 0.4768(5) 0.1756(8) 0.5875(5) 0.062(3) Uani 1 1 d . . . C15 C 0.4598(5) 0.1410(9) 0.6182(4) 0.065(4) Uani 1 1 d . . . H15A H 0.4798 0.1392 0.6495 0.078 Uiso 1 1 calc R . . C16 C 0.4145(5) 0.1090(10) 0.6040(5) 0.070(4) Uani 1 1 d . . . H16A H 0.4040 0.0854 0.6258 0.084 Uiso 1 1 calc R . . C17 C 0.5277(5) 0.2867(8) 0.6116(5) 0.057(3) Uani 1 1 d . . . C18 C 0.5864(5) 0.3914(9) 0.6567(5) 0.070(4) Uani 1 1 d . . . H18A H 0.5570 0.4161 0.6585 0.084 Uiso 1 1 calc R . . C19 C 0.6185(9) 0.3642(10) 0.7048(6) 0.106(7) Uani 1 1 d . . . H19A H 0.6485 0.3415 0.7040 0.127 Uiso 1 1 calc R . . H19B H 0.6017 0.3240 0.7154 0.127 Uiso 1 1 calc R . . C20 C 0.6311(11) 0.4368(13) 0.7392(8) 0.143(9) Uani 1 1 d . . . H20A H 0.6013 0.4594 0.7405 0.171 Uiso 1 1 calc R . . H20B H 0.6519 0.4202 0.7703 0.171 Uiso 1 1 calc R . . C21 C 0.6575(9) 0.4968(16) 0.7209(11) 0.157(11) Uani 1 1 d . . . H21A H 0.6655 0.5427 0.7410 0.189 Uiso 1 1 calc R . . H21B H 0.6880 0.4743 0.7210 0.189 Uiso 1 1 calc R . . C22 C 0.6261(10) 0.5213(13) 0.6721(9) 0.130(8) Uani 1 1 d . . . H22A H 0.5964 0.5463 0.6720 0.156 Uiso 1 1 calc R . . H22B H 0.6437 0.5590 0.6605 0.156 Uiso 1 1 calc R . . C23 C 0.6136(8) 0.4510(12) 0.6418(7) 0.111(7) Uani 1 1 d . . . H23A H 0.5940 0.4673 0.6103 0.133 Uiso 1 1 calc R . . H23B H 0.6435 0.4276 0.6414 0.133 Uiso 1 1 calc R . . C24 C 0.4759(6) 0.4092(9) 0.5862(6) 0.078(4) Uani 1 1 d U . . H24A H 0.5068 0.4380 0.5941 0.093 Uiso 1 1 calc R . . C25 C 0.4524(13) 0.4061(15) 0.5363(9) 0.175(12) Uani 1 1 d U . . H25A H 0.4226 0.3750 0.5281 0.210 Uiso 1 1 calc R . . H25B H 0.4740 0.3799 0.5236 0.210 Uiso 1 1 calc R . . C26 C 0.4397(16) 0.4863(18) 0.5148(9) 0.23(2) Uani 1 1 d . . . H26A H 0.4213 0.4817 0.4816 0.278 Uiso 1 1 calc R . . H26B H 0.4694 0.5160 0.5195 0.278 Uiso 1 1 calc R . . C27 C 0.4092(8) 0.5279(13) 0.5380(14) 0.185(16) Uani 1 1 d . . . H27A H 0.4001 0.5798 0.5243 0.222 Uiso 1 1 calc R . . H27B H 0.3794 0.4982 0.5325 0.222 Uiso 1 1 calc R . . C28 C 0.4359(11) 0.5363(16) 0.5883(9) 0.147(10) Uani 1 1 d . . . H28A H 0.4166 0.5649 0.6027 0.176 Uiso 1 1 calc R . . H28B H 0.4668 0.5636 0.5950 0.176 Uiso 1 1 calc R . . C29 C 0.4440(11) 0.4533(14) 0.6050(11) 0.153(10) Uani 1 1 d . . . H29A H 0.4588 0.4530 0.6387 0.184 Uiso 1 1 calc R . . H29B H 0.4126 0.4267 0.5959 0.184 Uiso 1 1 calc R . . C30 C 0.6966(8) 0.2535(10) 0.8496(7) 0.090(5) Uani 1 1 d . . . H30A H 0.6930 0.2542 0.8169 0.108 Uiso 1 1 calc R . . C31 C 0.7373(7) 0.2774(10) 0.8872(7) 0.093(5) Uani 1 1 d . . . H31A H 0.7681 0.2944 0.8846 0.111 Uiso 1 1 calc R . . C32 C 0.7284(7) 0.2822(9) 0.9273(6) 0.084(5) Uani 1 1 d . . . H32A H 0.7504 0.3051 0.9567 0.101 Uiso 1 1 calc R . . C33 C 0.6797(7) 0.2626(10) 0.9164(7) 0.093(5) Uani 1 1 d . . . H33A H 0.6609 0.2706 0.9365 0.112 Uiso 1 1 calc R . . C34 C 0.6592(7) 0.2457(10) 0.8665(8) 0.100(6) Uani 1 1 d . . . H34A H 0.6243 0.2397 0.8475 0.120 Uiso 1 1 calc R . . C35 C 0.8095(7) 0.0985(16) 0.9110(8) 0.105(6) Uani 1 1 d . . . H35A H 0.8222 0.1137 0.8871 0.127 Uiso 1 1 calc R . . C36 C 0.7904(7) 0.0295(14) 0.9126(7) 0.100(7) Uani 1 1 d . . . H36A H 0.7875 -0.0136 0.8907 0.120 Uiso 1 1 calc R . . C37 C 0.7828(6) 0.0216(11) 0.9543(7) 0.093(6) Uani 1 1 d . . . H37A H 0.7750 -0.0271 0.9672 0.112 Uiso 1 1 calc R . . C38 C 0.7983(6) 0.0935(12) 0.9778(6) 0.087(5) Uani 1 1 d . . . H38A H 0.8028 0.1034 1.0104 0.105 Uiso 1 1 calc R . . C39 C 0.8147(7) 0.1443(12) 0.9495(8) 0.103(6) Uani 1 1 d . . . H39A H 0.8335 0.1933 0.9590 0.123 Uiso 1 1 calc R . . C40 C 0.6640(5) 0.1479(8) 0.7097(5) 0.059(3) Uani 1 1 d . . . C41 C 0.7077(5) 0.1151(9) 0.7410(5) 0.072(4) Uani 1 1 d . . . H41A H 0.7355 0.1160 0.7334 0.087 Uiso 1 1 calc R . . C42 C 0.7110(5) 0.0820(9) 0.7822(5) 0.068(4) Uani 1 1 d . . . H42A H 0.7401 0.0581 0.8010 0.082 Uiso 1 1 calc R . . C43 C 0.6707(5) 0.0836(8) 0.7967(4) 0.056(3) Uani 1 1 d . . . C44 C 0.6285(5) 0.1186(8) 0.7674(5) 0.065(4) Uani 1 1 d . . . H44A H 0.6017 0.1220 0.7764 0.079 Uiso 1 1 calc R . . C45 C 0.6246(5) 0.1492(9) 0.7248(5) 0.063(3) Uani 1 1 d . . . H45A H 0.5950 0.1712 0.7056 0.076 Uiso 1 1 calc R . . C46 C 0.6668(10) -0.0232(13) 0.8388(6) 0.137(10) Uani 1 1 d . . . C47 C 0.6612(11) -0.1447(11) 0.8862(7) 0.116(8) Uani 1 1 d . . . H47A H 0.6516 -0.1737 0.8568 0.139 Uiso 1 1 calc R . . C48 C 0.6235(12) -0.1513(17) 0.9065(9) 0.148(10) Uani 1 1 d . . . H48A H 0.5920 -0.1344 0.8842 0.178 Uiso 1 1 calc R . . H48B H 0.6319 -0.1186 0.9341 0.178 Uiso 1 1 calc R . . C49 C 0.6213(11) -0.2468(17) 0.9203(10) 0.143(9) Uani 1 1 d . . . H49A H 0.6009 -0.2523 0.9386 0.172 Uiso 1 1 calc R . . H49B H 0.6066 -0.2775 0.8920 0.172 Uiso 1 1 calc R . . C50 C 0.6728(13) -0.2785(14) 0.9481(10) 0.147(10) Uani 1 1 d . . . H50A H 0.6841 -0.2554 0.9790 0.176 Uiso 1 1 calc R . . H50B H 0.6706 -0.3350 0.9517 0.176 Uiso 1 1 calc R . . C51 C 0.7071(11) -0.2637(15) 0.9286(9) 0.137(9) Uani 1 1 d . . . H51A H 0.6990 -0.2925 0.8996 0.164 Uiso 1 1 calc R . . H51B H 0.7393 -0.2805 0.9496 0.164 Uiso 1 1 calc R . . C52 C 0.7071(11) -0.1746(15) 0.9196(11) 0.150(10) Uani 1 1 d . . . H52A H 0.7144 -0.1470 0.9489 0.179 Uiso 1 1 calc R . . H52B H 0.7331 -0.1628 0.9084 0.179 Uiso 1 1 calc R . . C53 C 0.6819(9) -0.1410(15) 0.7876(9) 0.132(8) Uiso 1 1 d D . . H53A H 0.6998 -0.1674 0.8173 0.159 Uiso 1 1 calc R . . C54 C 0.7172(13) -0.1172(18) 0.7659(14) 0.208(16) Uiso 1 1 d D . . H54A H 0.7017 -0.0791 0.7414 0.250 Uiso 1 1 calc R . . H54B H 0.7454 -0.0921 0.7891 0.250 Uiso 1 1 calc R . . C55 C 0.7335(12) -0.1841(18) 0.7464(13) 0.200(14) Uiso 1 1 d D . . H55A H 0.7552 -0.2161 0.7716 0.240 Uiso 1 1 calc R . . H55B H 0.7522 -0.1651 0.7284 0.240 Uiso 1 1 calc R . . C56 C 0.6931(12) -0.2333(19) 0.7166(11) 0.182(12) Uiso 1 1 d D . . H56A H 0.7059 -0.2785 0.7055 0.219 Uiso 1 1 calc R . . H56B H 0.6724 -0.2033 0.6898 0.219 Uiso 1 1 calc R . . C57 C 0.6643(14) -0.260(2) 0.7447(13) 0.229(17) Uiso 1 1 d D . . H57A H 0.6393 -0.2968 0.7266 0.274 Uiso 1 1 calc R . . H57B H 0.6859 -0.2871 0.7722 0.274 Uiso 1 1 calc R . . C58 C 0.6407(11) -0.1927(18) 0.7588(12) 0.194(13) Uiso 1 1 d D . . H58A H 0.6219 -0.2111 0.7769 0.233 Uiso 1 1 calc R . . H58B H 0.6190 -0.1645 0.7318 0.233 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 0.0585(4) 0.0640(4) 0.0462(4) -0.0039(3) 0.0209(3) 0.0022(3) Er2 0.0500(4) 0.0649(4) 0.0553(4) -0.0142(3) 0.0144(3) -0.0001(3) S1 0.0580(19) 0.080(3) 0.054(2) -0.0027(17) 0.0136(16) -0.0123(17) S2 0.0546(19) 0.081(2) 0.055(2) 0.0004(17) 0.0188(16) -0.0005(17) N1 0.049(6) 0.071(8) 0.053(6) -0.002(5) 0.019(5) 0.000(5) N2 0.045(6) 0.077(8) 0.086(9) -0.024(7) 0.023(6) 0.002(6) N3 0.061(7) 0.065(8) 0.088(9) -0.007(6) 0.029(6) -0.002(6) N4 0.073(7) 0.058(7) 0.045(6) -0.005(5) 0.017(5) -0.005(5) N5 0.36(3) 0.078(11) 0.057(9) -0.013(8) 0.043(14) -0.061(15) N6 0.30(3) 0.080(11) 0.058(9) -0.013(8) 0.011(13) -0.038(14) C1 0.105(14) 0.103(14) 0.062(10) -0.001(9) 0.036(10) -0.018(11) C2 0.088(12) 0.087(12) 0.073(11) 0.023(9) 0.029(10) 0.020(10) C3 0.093(13) 0.139(18) 0.052(10) 0.012(11) 0.019(9) -0.008(13) C4 0.19(2) 0.083(13) 0.088(14) 0.004(10) 0.101(16) 0.012(14) C5 0.079(12) 0.16(2) 0.080(13) 0.005(14) 0.047(10) 0.007(14) C6 0.084(11) 0.068(10) 0.093(13) -0.011(9) 0.040(10) -0.019(8) C7 0.105(13) 0.063(10) 0.078(11) -0.017(8) 0.024(10) -0.005(9) C8 0.105(15) 0.071(12) 0.140(18) -0.012(11) 0.056(14) 0.016(10) C9 0.118(15) 0.065(10) 0.065(10) 0.013(8) 0.014(10) 0.000(10) C10 0.125(15) 0.061(10) 0.083(12) 0.002(8) 0.063(11) 0.005(9) C11 0.057(8) 0.067(9) 0.053(8) -0.008(6) 0.016(6) -0.004(6) C12 0.062(8) 0.085(10) 0.052(8) -0.011(7) 0.021(7) -0.009(7) C13 0.062(8) 0.068(9) 0.052(8) -0.006(6) 0.018(6) -0.005(7) C14 0.054(8) 0.068(9) 0.062(9) -0.016(7) 0.021(7) 0.006(6) C15 0.054(8) 0.105(12) 0.034(7) -0.004(7) 0.015(6) 0.000(7) C16 0.051(8) 0.111(12) 0.042(7) -0.003(7) 0.009(6) -0.003(8) C17 0.052(8) 0.062(9) 0.056(8) -0.012(6) 0.018(6) -0.004(6) C18 0.059(8) 0.070(9) 0.078(10) -0.005(8) 0.022(7) 0.002(7) C19 0.145(18) 0.067(11) 0.080(12) -0.009(9) 0.012(12) -0.004(10) C20 0.23(3) 0.102(17) 0.102(16) -0.047(13) 0.067(17) -0.054(18) C21 0.13(2) 0.12(2) 0.21(3) -0.08(2) 0.04(2) -0.066(16) C22 0.15(2) 0.103(17) 0.13(2) 0.010(15) 0.041(17) -0.037(15) C23 0.142(18) 0.113(16) 0.091(14) -0.019(12) 0.058(13) -0.046(14) C24 0.060(9) 0.069(10) 0.091(12) -0.009(8) 0.014(8) -0.004(7) C25 0.29(3) 0.105(17) 0.104(17) -0.003(14) 0.045(19) 0.079(19) C26 0.45(6) 0.15(3) 0.090(18) 0.028(17) 0.10(3) 0.12(3) C27 0.072(13) 0.073(14) 0.33(5) 0.00(2) -0.02(2) 0.013(11) C28 0.17(3) 0.12(2) 0.13(2) -0.006(16) 0.03(2) 0.038(17) C29 0.18(2) 0.102(18) 0.21(3) 0.014(18) 0.11(2) 0.060(17) C30 0.124(15) 0.074(11) 0.080(12) -0.009(9) 0.048(12) -0.008(10) C31 0.102(14) 0.080(12) 0.102(14) -0.007(10) 0.046(12) -0.021(10) C32 0.095(13) 0.070(10) 0.076(11) -0.025(8) 0.018(9) -0.014(9) C33 0.109(15) 0.071(11) 0.115(16) -0.002(10) 0.060(13) 0.029(10) C34 0.094(13) 0.061(11) 0.112(16) -0.002(10) 0.000(12) 0.018(9) C35 0.077(12) 0.148(19) 0.105(15) -0.028(15) 0.049(11) 0.006(13) C36 0.072(11) 0.124(17) 0.096(15) -0.049(13) 0.020(10) 0.023(11) C37 0.062(10) 0.079(12) 0.109(15) -0.018(10) -0.002(10) 0.021(8) C38 0.057(9) 0.112(14) 0.072(11) -0.016(10) -0.001(8) 0.004(9) C39 0.070(11) 0.103(14) 0.129(17) -0.033(13) 0.029(11) -0.018(10) C40 0.046(7) 0.075(9) 0.052(8) -0.012(6) 0.014(6) -0.006(6) C41 0.048(8) 0.091(11) 0.074(10) 0.000(8) 0.018(7) 0.002(7) C42 0.064(8) 0.089(11) 0.051(8) 0.003(7) 0.020(7) 0.014(7) C43 0.067(8) 0.053(8) 0.048(7) -0.005(6) 0.020(6) 0.003(6) C44 0.052(8) 0.084(10) 0.063(9) -0.003(7) 0.025(7) 0.003(7) C45 0.053(8) 0.079(9) 0.057(8) 0.004(7) 0.020(6) 0.006(7) C46 0.23(3) 0.095(15) 0.052(11) 0.003(10) 0.013(13) -0.037(16) C47 0.20(3) 0.071(12) 0.068(12) -0.012(9) 0.045(15) -0.035(14) C48 0.21(3) 0.15(2) 0.094(17) -0.013(15) 0.069(19) 0.03(2) C49 0.17(3) 0.15(2) 0.13(2) -0.040(18) 0.08(2) -0.03(2) C50 0.21(3) 0.083(15) 0.14(2) 0.009(14) 0.06(2) -0.017(18) C51 0.18(2) 0.14(2) 0.13(2) 0.009(16) 0.10(2) 0.007(18) C52 0.17(3) 0.11(2) 0.16(3) 0.014(18) 0.06(2) -0.047(18) _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 2.413(11) . ? Er1 C3 2.550(16) . ? Er1 C5 2.597(17) . ? Er1 C4 2.601(16) . ? Er1 C10 2.607(16) . ? Er1 C8 2.609(17) . ? Er1 C9 2.617(16) . ? Er1 C2 2.628(16) . ? Er1 C1 2.644(17) . ? Er1 S2 2.649(4) . ? Er1 C6 2.654(15) . ? Er1 C7 2.660(16) . ? Er2 N4 2.379(10) . ? Er2 C39 2.609(18) . ? Er2 C33 2.611(15) . ? Er2 C38 2.615(15) . ? Er2 C34 2.622(16) . ? Er2 C35 2.628(17) . ? Er2 C36 2.632(17) . ? Er2 C30 2.636(18) . ? Er2 C32 2.643(16) . ? Er2 C31 2.644(18) . ? Er2 C37 2.649(16) . ? Er2 S1 2.675(4) 2_656 ? S1 C11 1.777(14) . ? S1 Er2 2.675(4) 2_656 ? S2 C40 1.751(14) . ? N1 C17 1.314(17) . ? N1 C14 1.446(17) . ? N2 C17 1.335(16) . ? N2 C18 1.480(18) . ? N2 H2B 0.8600 . ? N3 C17 1.367(17) . ? N3 C24 1.48(2) . ? N3 H3B 0.8600 . ? N4 C46 1.27(2) . ? N4 C43 1.429(16) . ? N5 C46 1.39(2) . ? N5 C47 1.47(2) . ? N5 H5B 0.8600 . ? N6 C46 1.41(2) . ? N6 C53 1.63(3) . ? N6 H6B 0.8600 . ? C1 C2 1.33(2) . ? C1 C5 1.37(3) . ? C1 H1A 0.9800 . ? C2 C3 1.35(3) . ? C2 H2A 0.9800 . ? C3 C4 1.46(3) . ? C3 H3A 0.9800 . ? C4 C5 1.34(3) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.36(2) . ? C6 C10 1.39(2) . ? C6 H6A 0.9800 . ? C7 C8 1.44(3) . ? C7 H7A 0.9800 . ? C8 C9 1.42(3) . ? C8 H8A 0.9800 . ? C9 C10 1.37(2) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C11 C12 1.36(2) . ? C11 C16 1.413(18) . ? C12 C13 1.413(19) . ? C12 H12A 0.9300 . ? C13 C14 1.397(18) . ? C13 H13A 0.9300 . ? C14 C15 1.360(19) . ? C15 C16 1.351(19) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C23 1.47(2) . ? C18 C19 1.51(2) . ? C18 H18A 0.9800 . ? C19 C20 1.58(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.51(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.51(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.48(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.44(3) . ? C24 C29 1.47(2) . ? C24 H24A 0.9800 . ? C25 C26 1.50(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.52(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.47(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.49(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.38(2) . ? C30 C34 1.39(3) . ? C30 H30A 0.9800 . ? C31 C32 1.36(2) . ? C31 H31A 0.9800 . ? C32 C33 1.38(2) . ? C32 H32A 0.9800 . ? C33 C34 1.46(3) . ? C33 H33A 0.9800 . ? C34 H34A 0.9800 . ? C35 C36 1.31(3) . ? C35 C39 1.38(3) . ? C35 H35A 0.9800 . ? C36 C37 1.40(3) . ? C36 H36A 0.9800 . ? C37 C38 1.41(2) . ? C37 H37A 0.9800 . ? C38 C39 1.43(3) . ? C38 H38A 0.9800 . ? C39 H39A 0.9800 . ? C40 C45 1.400(18) . ? C40 C41 1.405(19) . ? C41 C42 1.36(2) . ? C41 H41A 0.9300 . ? C42 C43 1.413(18) . ? C42 H42A 0.9300 . ? C43 C44 1.371(18) . ? C44 C45 1.38(2) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C47 C52 1.45(3) . ? C47 C48 1.47(3) . ? C47 H47A 0.9800 . ? C48 C49 1.68(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.53(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.38(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.54(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.486(18) . ? C53 C58 1.493(18) . ? C53 H53A 0.9800 . ? C54 C55 1.445(18) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.464(18) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.491(19) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.481(19) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 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 C3 97.8(6) . . ? N1 Er1 C5 124.5(6) . . ? C3 Er1 C5 51.2(6) . . ? N1 Er1 C4 129.3(6) . . ? C3 Er1 C4 32.8(7) . . ? C5 Er1 C4 29.9(6) . . ? N1 Er1 C10 88.4(5) . . ? C3 Er1 C10 132.6(7) . . ? C5 Er1 C10 147.1(7) . . ? C4 Er1 C10 129.7(6) . . ? N1 Er1 C8 138.0(5) . . ? C3 Er1 C8 103.1(8) . . ? C5 Er1 C8 96.7(8) . . ? C4 Er1 C8 82.2(6) . . ? C10 Er1 C8 51.0(6) . . ? N1 Er1 C9 115.2(6) . . ? C3 Er1 C9 134.3(7) . . ? C5 Er1 C9 118.6(7) . . ? C4 Er1 C9 112.4(6) . . ? C10 Er1 C9 30.4(5) . . ? C8 Er1 C9 31.6(6) . . ? N1 Er1 C2 80.3(5) . . ? C3 Er1 C2 30.1(6) . . ? C5 Er1 C2 49.3(6) . . ? C4 Er1 C2 50.7(6) . . ? C10 Er1 C2 154.9(6) . . ? C8 Er1 C2 131.3(7) . . ? C9 Er1 C2 162.8(6) . . ? N1 Er1 C1 94.2(5) . . ? C3 Er1 C1 50.3(6) . . ? C5 Er1 C1 30.4(6) . . ? C4 Er1 C1 50.3(6) . . ? C10 Er1 C1 175.8(6) . . ? C8 Er1 C1 127.0(7) . . ? C9 Er1 C1 145.8(7) . . ? C2 Er1 C1 29.3(5) . . ? N1 Er1 S2 95.6(3) . . ? C3 Er1 S2 125.6(5) . . ? C5 Er1 S2 78.2(5) . . ? C4 Er1 S2 106.5(7) . . ? C10 Er1 S2 100.1(5) . . ? C8 Er1 S2 100.8(5) . . ? C9 Er1 S2 83.3(4) . . ? C2 Er1 S2 103.3(5) . . ? C1 Er1 S2 76.4(4) . . ? N1 Er1 C6 89.9(5) . . ? C3 Er1 C6 102.2(6) . . ? C5 Er1 C6 135.6(7) . . ? C4 Er1 C6 107.5(6) . . ? C10 Er1 C6 30.6(5) . . ? C8 Er1 C6 50.5(6) . . ? C9 Er1 C6 50.5(6) . . ? C2 Er1 C6 126.2(6) . . ? C1 Er1 C6 152.4(6) . . ? S2 Er1 C6 130.4(4) . . ? N1 Er1 C7 116.8(5) . . ? C3 Er1 C7 85.9(7) . . ? C5 Er1 C7 106.4(7) . . ? C4 Er1 C7 80.4(6) . . ? C10 Er1 C7 50.6(5) . . ? C8 Er1 C7 31.8(6) . . ? C9 Er1 C7 51.9(5) . . ? C2 Er1 C7 115.6(6) . . ? C1 Er1 C7 130.3(6) . . ? S2 Er1 C7 132.1(4) . . ? C6 Er1 C7 29.6(5) . . ? N4 Er2 C39 129.1(5) . . ? N4 Er2 C33 117.9(5) . . ? C39 Er2 C33 107.8(7) . . ? N4 Er2 C38 127.9(5) . . ? C39 Er2 C38 31.9(6) . . ? C33 Er2 C38 113.3(6) . . ? N4 Er2 C34 88.3(5) . . ? C39 Er2 C34 125.9(7) . . ? C33 Er2 C34 32.5(6) . . ? C38 Er2 C34 143.8(6) . . ? N4 Er2 C35 98.7(6) . . ? C39 Er2 C35 30.6(6) . . ? C33 Er2 C35 131.4(8) . . ? C38 Er2 C35 50.0(6) . . ? C34 Er2 C35 132.6(8) . . ? N4 Er2 C36 81.9(5) . . ? C39 Er2 C36 50.5(6) . . ? C33 Er2 C36 158.2(7) . . ? C38 Er2 C36 50.2(6) . . ? C34 Er2 C36 154.5(8) . . ? C35 Er2 C36 28.8(6) . . ? N4 Er2 C30 88.1(5) . . ? C39 Er2 C30 103.8(7) . . ? C33 Er2 C30 52.1(6) . . ? C38 Er2 C30 133.2(7) . . ? C34 Er2 C30 30.6(6) . . ? C35 Er2 C30 102.4(8) . . ? C36 Er2 C30 125.0(7) . . ? N4 Er2 C32 137.8(5) . . ? C39 Er2 C32 78.6(6) . . ? C33 Er2 C32 30.6(5) . . ? C38 Er2 C32 92.9(6) . . ? C34 Er2 C32 51.5(6) . . ? C35 Er2 C32 100.9(7) . . ? C36 Er2 C32 128.1(7) . . ? C30 Er2 C32 51.3(5) . . ? N4 Er2 C31 116.3(5) . . ? C39 Er2 C31 77.1(7) . . ? C33 Er2 C31 49.8(6) . . ? C38 Er2 C31 103.5(6) . . ? C34 Er2 C31 49.6(6) . . ? C35 Er2 C31 86.6(8) . . ? C36 Er2 C31 115.0(7) . . ? C30 Er2 C31 30.4(5) . . ? C32 Er2 C31 29.9(5) . . ? N4 Er2 C37 97.2(5) . . ? C39 Er2 C37 52.1(6) . . ? C33 Er2 C37 141.3(6) . . ? C38 Er2 C37 31.0(5) . . ? C34 Er2 C37 173.8(7) . . ? C35 Er2 C37 49.6(7) . . ? C36 Er2 C37 30.6(6) . . ? C30 Er2 C37 151.9(7) . . ? C32 Er2 C37 123.8(5) . . ? C31 Er2 C37 129.1(6) . . ? N4 Er2 S1 95.9(3) . 2_656 ? C39 Er2 S1 110.9(6) . 2_656 ? C33 Er2 S1 83.6(4) . 2_656 ? C38 Er2 S1 80.2(5) . 2_656 ? C34 Er2 S1 100.0(6) . 2_656 ? C35 Er2 S1 125.4(6) . 2_656 ? C36 Er2 S1 104.4(6) . 2_656 ? C30 Er2 S1 130.4(5) . 2_656 ? C32 Er2 S1 102.3(4) . 2_656 ? C31 Er2 S1 131.2(4) . 2_656 ? C37 Er2 S1 76.6(5) . 2_656 ? C11 S1 Er2 107.6(5) . 2_656 ? C40 S2 Er1 110.1(4) . . ? C17 N1 C14 116.5(11) . . ? C17 N1 Er1 128.6(9) . . ? C14 N1 Er1 112.4(8) . . ? C17 N2 C18 125.8(11) . . ? C17 N2 H2B 117.1 . . ? C18 N2 H2B 117.1 . . ? C17 N3 C24 124.7(12) . . ? C17 N3 H3B 117.6 . . ? C24 N3 H3B 117.6 . . ? C46 N4 C43 113.4(13) . . ? C46 N4 Er2 129.8(11) . . ? C43 N4 Er2 114.3(8) . . ? C46 N5 C47 127.8(17) . . ? C46 N5 H5B 116.1 . . ? C47 N5 H5B 116.1 . . ? C46 N6 C53 124(2) . . ? C46 N6 H6B 117.9 . . ? C53 N6 H6B 117.9 . . ? C2 C1 C5 107.3(18) . . ? C2 C1 Er1 74.7(10) . . ? C5 C1 Er1 72.9(11) . . ? C2 C1 H1A 126.0 . . ? C5 C1 H1A 126.0 . . ? Er1 C1 H1A 126.0 . . ? C1 C2 C3 110.9(17) . . ? C1 C2 Er1 76.0(10) . . ? C3 C2 Er1 71.7(10) . . ? C1 C2 H2A 124.4 . . ? C3 C2 H2A 124.4 . . ? Er1 C2 H2A 124.4 . . ? C2 C3 C4 105.9(18) . . ? C2 C3 Er1 78.1(10) . . ? C4 C3 Er1 75.5(9) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? Er1 C3 H3A 125.9 . . ? C5 C4 C3 105.2(18) . . ? C5 C4 Er1 74.9(10) . . ? C3 C4 Er1 71.7(9) . . ? C5 C4 H4A 126.9 . . ? C3 C4 H4A 126.9 . . ? Er1 C4 H4A 126.9 . . ? C4 C5 C1 110.5(19) . . ? C4 C5 Er1 75.2(11) . . ? C1 C5 Er1 76.7(10) . . ? C4 C5 H5A 124.3 . . ? C1 C5 H5A 124.3 . . ? Er1 C5 H5A 124.3 . . ? C7 C6 C10 110.1(16) . . ? C7 C6 Er1 75.4(9) . . ? C10 C6 Er1 72.8(9) . . ? C7 C6 H6A 124.7 . . ? C10 C6 H6A 124.7 . . ? Er1 C6 H6A 124.7 . . ? C6 C7 C8 106.4(16) . . ? C6 C7 Er1 74.9(9) . . ? C8 C7 Er1 72.1(9) . . ? C6 C7 H7A 126.4 . . ? C8 C7 H7A 126.4 . . ? Er1 C7 H7A 126.4 . . ? C9 C8 C7 107.3(17) . . ? C9 C8 Er1 74.5(9) . . ? C7 C8 Er1 76.1(9) . . ? C9 C8 H8A 125.7 . . ? C7 C8 H8A 125.7 . . ? Er1 C8 H8A 125.7 . . ? C10 C9 C8 106.9(16) . . ? C10 C9 Er1 74.4(10) . . ? C8 C9 Er1 73.9(10) . . ? C10 C9 H9A 126.0 . . ? C8 C9 H9A 126.0 . . ? Er1 C9 H9A 126.0 . . ? C9 C10 C6 109.3(15) . . ? C9 C10 Er1 75.2(10) . . ? C6 C10 Er1 76.6(9) . . ? C9 C10 H10A 124.7 . . ? C6 C10 H10A 124.7 . . ? Er1 C10 H10A 124.7 . . ? C12 C11 C16 117.5(13) . . ? C12 C11 S1 120.7(11) . . ? C16 C11 S1 121.9(11) . . ? C11 C12 C13 121.8(13) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C14 C13 C12 118.2(13) . . ? C14 C13 H13A 120.9 . . ? C12 C13 H13A 120.9 . . ? C15 C14 C13 119.7(13) . . ? C15 C14 N1 121.1(12) . . ? C13 C14 N1 119.1(13) . . ? C16 C15 C14 121.5(13) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C11 121.2(13) . . ? C15 C16 H16A 119.4 . . ? C11 C16 H16A 119.4 . . ? N1 C17 N2 119.2(12) . . ? N1 C17 N3 121.2(12) . . ? N2 C17 N3 119.6(12) . . ? C23 C18 N2 113.5(14) . . ? C23 C18 C19 107.9(15) . . ? N2 C18 C19 109.6(13) . . ? C23 C18 H18A 108.6 . . ? N2 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? C18 C19 C20 109.3(16) . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? C21 C20 C19 107.2(19) . . ? C21 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? C21 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.5 . . ? C22 C21 C20 110.7(19) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 109(2) . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? C18 C23 C22 113.1(17) . . ? C18 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C18 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C29 108.7(19) . . ? C25 C24 N3 111.9(15) . . ? C29 C24 N3 111.0(16) . . ? C25 C24 H24A 108.4 . . ? C29 C24 H24A 108.4 . . ? N3 C24 H24A 108.4 . . ? C24 C25 C26 113(2) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 C27 108(3) . . ? C25 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? C25 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C28 C27 C26 112(2) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 103(2) . . ? C27 C28 H28A 111.1 . . ? C29 C28 H28A 111.1 . . ? C27 C28 H28B 111.1 . . ? C29 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? C24 C29 C28 113(2) . . ? C24 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C24 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C34 105.7(16) . . ? C31 C30 Er2 75.1(11) . . ? C34 C30 Er2 74.2(10) . . ? C31 C30 H30A 126.5 . . ? C34 C30 H30A 126.5 . . ? Er2 C30 H30A 126.5 . . ? C32 C31 C30 112.7(17) . . ? C32 C31 Er2 75.0(10) . . ? C30 C31 Er2 74.5(10) . . ? C32 C31 H31A 123.5 . . ? C30 C31 H31A 123.5 . . ? Er2 C31 H31A 123.5 . . ? C31 C32 C33 107.2(16) . . ? C31 C32 Er2 75.1(10) . . ? C33 C32 Er2 73.5(9) . . ? C31 C32 H32A 125.9 . . ? C33 C32 H32A 125.9 . . ? Er2 C32 H32A 125.9 . . ? C32 C33 C34 106.7(17) . . ? C32 C33 Er2 76.0(9) . . ? C34 C33 Er2 74.2(9) . . ? C32 C33 H33A 126.0 . . ? C34 C33 H33A 126.0 . . ? Er2 C33 H33A 126.0 . . ? C30 C34 C33 107.8(17) . . ? C30 C34 Er2 75.2(11) . . ? C33 C34 Er2 73.3(9) . . ? C30 C34 H34A 125.7 . . ? C33 C34 H34A 125.7 . . ? Er2 C34 H34A 125.7 . . ? C36 C35 C39 112(2) . . ? C36 C35 Er2 75.8(11) . . ? C39 C35 Er2 74.0(10) . . ? C36 C35 H35A 123.6 . . ? C39 C35 H35A 123.6 . . ? Er2 C35 H35A 123.6 . . ? C35 C36 C37 109.8(18) . . ? C35 C36 Er2 75.4(12) . . ? C37 C36 Er2 75.3(9) . . ? C35 C36 H36A 124.6 . . ? C37 C36 H36A 124.6 . . ? Er2 C36 H36A 124.6 . . ? C36 C37 C38 105.3(19) . . ? C36 C37 Er2 74.0(11) . . ? C38 C37 Er2 73.2(9) . . ? C36 C37 H37A 126.8 . . ? C38 C37 H37A 126.8 . . ? Er2 C37 H37A 126.8 . . ? C37 C38 C39 108.8(18) . . ? C37 C38 Er2 75.8(9) . . ? C39 C38 Er2 73.8(10) . . ? C37 C38 H38A 125.2 . . ? C39 C38 H38A 125.2 . . ? Er2 C38 H38A 125.2 . . ? C35 C39 C38 103.6(19) . . ? C35 C39 Er2 75.4(11) . . ? C38 C39 Er2 74.3(9) . . ? C35 C39 H39A 127.2 . . ? C38 C39 H39A 127.2 . . ? Er2 C39 H39A 127.2 . . ? C45 C40 C41 115.5(13) . . ? C45 C40 S2 124.5(11) . . ? C41 C40 S2 120.0(11) . . ? C42 C41 C40 122.6(14) . . ? C42 C41 H41A 118.7 . . ? C40 C41 H41A 118.7 . . ? C41 C42 C43 120.9(13) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C42 117.1(13) . . ? C44 C43 N4 123.7(12) . . ? C42 C43 N4 119.3(12) . . ? C43 C44 C45 122.0(13) . . ? C43 C44 H44A 119.0 . . ? C45 C44 H44A 119.0 . . ? C44 C45 C40 121.9(13) . . ? C44 C45 H45A 119.1 . . ? C40 C45 H45A 119.1 . . ? N4 C46 N5 118.1(17) . . ? N4 C46 N6 123.0(17) . . ? N5 C46 N6 118.6(18) . . ? C52 C47 C48 109(2) . . ? C52 C47 N5 109(2) . . ? C48 C47 N5 107(2) . . ? C52 C47 H47A 110.9 . . ? C48 C47 H47A 110.9 . . ? N5 C47 H47A 110.9 . . ? C47 C48 C49 107(2) . . ? C47 C48 H48A 110.3 . . ? C49 C48 H48A 110.3 . . ? C47 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.6 . . ? C50 C49 C48 111(2) . . ? C50 C49 H49A 109.5 . . ? C48 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? C51 C50 C49 115(2) . . ? C51 C50 H50A 108.5 . . ? C49 C50 H50A 108.5 . . ? C51 C50 H50B 108.5 . . ? C49 C50 H50B 108.5 . . ? H50A C50 H50B 107.5 . . ? C50 C51 C52 108(2) . . ? C50 C51 H51A 110.1 . . ? C52 C51 H51A 110.1 . . ? C50 C51 H51B 110.1 . . ? C52 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? C47 C52 C51 114(2) . . ? C47 C52 H52A 108.7 . . ? C51 C52 H52A 108.7 . . ? C47 C52 H52B 108.7 . . ? C51 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C54 C53 C58 116(3) . . ? C54 C53 N6 113(2) . . ? C58 C53 N6 101(2) . . ? C54 C53 H53A 109.0 . . ? C58 C53 H53A 109.0 . . ? N6 C53 H53A 109.0 . . ? C55 C54 C53 112(3) . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54B 109.3 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C54 C55 C56 113(3) . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 C57 108(3) . . ? C55 C56 H56A 110.1 . . ? C57 C56 H56A 110.1 . . ? C55 C56 H56B 110.1 . . ? C57 C56 H56B 110.1 . . ? H56A C56 H56B 108.5 . . ? C58 C57 C56 112(3) . . ? C58 C57 H57A 109.3 . . ? C56 C57 H57A 109.3 . . ? C58 C57 H57B 109.3 . . ? C56 C57 H57B 109.3 . . ? H57A C57 H57B 107.9 . . ? C57 C58 C53 105(3) . . ? C57 C58 H58A 110.7 . . ? C53 C58 H58A 110.7 . . ? C57 C58 H58B 110.7 . . ? C53 C58 H58B 110.7 . . ? H58A C58 H58B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.136 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.262