# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dangsong@ciac.jl.cn _publ_contact_author_name 'Song Dang' loop_ _publ_author_name 'Zhongming Sun' 'Song Dang' data_C29H28NO10Er _database_code_depnum_ccdc_archive 'CCDC 852924' #TrackingRef 'CIAC-D1Er.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Er N O10' _chemical_formula_weight 718.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 18.037(2) _cell_length_b 24.308(3) _cell_length_c 6.9817(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3061.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 2.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6349 _exptl_absorpt_correction_T_max 0.7453 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2980 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.18 _reflns_number_total 2980 _reflns_number_gt 2796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(18) _refine_ls_number_reflns 2980 _refine_ls_number_parameters 203 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 1.0000 -0.016345(8) -0.02958(8) 0.02720(9) Uani 1 2 d S . . O1 O 1.0000 0.06107(17) -0.2214(7) 0.0363(11) Uani 1 2 d S . . O2 O 1.07083(18) -0.03789(14) -0.3207(5) 0.0355(8) Uani 1 1 d . . . O3 O 1.12848(18) -0.04591(16) -0.0529(12) 0.0513(13) Uani 1 1 d . . . O4 O 1.4095(4) -0.0750(3) -0.5585(19) 0.065(2) Uani 0.50 1 d PU . . O4' O 1.3741(6) -0.1053(4) -0.6946(16) 0.064(2) Uani 0.50 1 d PU . . O5 O 1.0000 0.3006(2) 0.1439(9) 0.0602(16) Uani 1 2 d S . . O6 O 1.0000 0.1124(2) -0.4839(6) 0.0483(16) Uani 1 2 d S . . C1 C 1.0000 0.3973(3) 0.2075(10) 0.0360(16) Uani 1 2 d S . . C2 C 1.0522(7) 0.3923(5) 0.3790(19) 0.046(3) Uani 0.50 1 d P . . C2' C 1.0830(9) 0.3917(6) 0.276(2) 0.054(3) Uani 0.50 1 d P . . C3 C 1.0000 0.3543(3) 0.0555(12) 0.060(2) Uani 1 2 d S . . H3A H 0.9569 0.3586 -0.0236 0.072 Uiso 0.50 1 d PR . . C4 C 1.0000 0.4535(3) 0.1096(17) 0.074(3) Uani 1 2 d S . . H4A H 1.0000 0.4819 0.2055 0.111 Uiso 1 2 d SR . . H4B H 1.0435 0.4571 0.0312 0.111 Uiso 0.50 1 d PR . . C5 C 1.0000 0.2558(5) 0.0263(14) 0.057(4) Uani 1 2 d S . . C6 C 1.0000 0.2063(4) 0.1121(15) 0.058(3) Uani 1 2 d S . . H6A H 1.0000 0.2049 0.2452 0.069 Uiso 1 2 calc SR . . C7 C 1.0000 0.1582(3) 0.0123(12) 0.048(3) Uani 1 2 d S . . H7A H 1.0000 0.1245 0.0759 0.058 Uiso 1 2 calc SR . . C8 C 1.0000 0.1603(3) -0.1857(13) 0.0407(19) Uani 1 2 d S . . C9 C 1.0000 0.2081(4) -0.2687(15) 0.073(4) Uani 1 2 d S . . H9A H 1.0000 0.2094 -0.4018 0.088 Uiso 1 2 calc SR . . C10 C 1.0000 0.2596(5) -0.1628(17) 0.083(5) Uani 1 2 d S . . H10A H 1.0000 0.2934 -0.2248 0.099 Uiso 1 2 calc SR . . C11 C 1.0000 0.1094(3) -0.3012(10) 0.0356(16) Uani 1 2 d S . . C12 C 1.1299(3) -0.04783(19) -0.2290(8) 0.0353(11) Uani 1 1 d . . . C13 C 1.1981(3) -0.0617(2) -0.3350(10) 0.0494(14) Uani 1 1 d . . . C14 C 1.1972(3) -0.0757(2) -0.523(2) 0.0644(16) Uani 1 1 d . . . H14 H 1.1521 -0.0777 -0.5877 0.077 Uiso 1 1 calc R . . C15 C 1.2611(5) -0.0867(4) -0.6198(13) 0.096(2) Uani 1 1 d U . . H15 H 1.2591 -0.0966 -0.7484 0.115 Uiso 1 1 calc R . . C16 C 1.3275(4) -0.0835(3) -0.530(2) 0.112(2) Uani 1 1 d DU . . C17 C 1.3310(4) -0.0676(5) -0.3400(16) 0.116(3) Uani 1 1 d DU . . H17 H 1.3765 -0.0632 -0.2795 0.139 Uiso 1 1 calc R . . C18 C 1.2660(4) -0.0585(4) -0.2420(13) 0.087(3) Uani 1 1 d . . . H18 H 1.2675 -0.0501 -0.1121 0.105 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 0.03067(14) 0.03195(13) 0.01898(12) -0.0001(2) 0.000 0.000 O1 0.056(3) 0.027(2) 0.026(2) -0.0005(19) 0.000 0.000 O2 0.0283(19) 0.0410(17) 0.0374(19) 0.0079(16) 0.0027(14) 0.0062(15) O3 0.0398(16) 0.077(2) 0.037(4) -0.015(3) -0.006(2) 0.0112(16) O4 0.035(3) 0.081(4) 0.080(7) -0.032(5) 0.014(5) 0.000(3) O4' 0.032(4) 0.082(5) 0.079(5) -0.027(4) -0.003(4) 0.001(5) O5 0.107(5) 0.035(3) 0.039(3) -0.009(3) 0.000 0.000 O6 0.079(4) 0.038(2) 0.028(4) 0.000(2) 0.000 0.000 C1 0.027(3) 0.040(4) 0.040(4) -0.014(3) 0.000 0.000 C2 0.023(6) 0.065(7) 0.049(6) -0.019(6) -0.002(5) -0.004(5) C2' 0.035(7) 0.070(8) 0.057(8) -0.028(7) 0.006(7) 0.013(7) C3 0.096(7) 0.040(4) 0.044(4) -0.013(4) 0.000 0.000 C4 0.100(8) 0.039(5) 0.082(8) -0.003(5) 0.000 0.000 C5 0.082(7) 0.040(5) 0.049(9) -0.016(4) 0.000 0.000 C6 0.093(7) 0.052(6) 0.029(5) 0.002(5) 0.000 0.000 C7 0.079(6) 0.031(3) 0.035(8) -0.006(4) 0.000 0.000 C8 0.058(5) 0.032(4) 0.032(5) 0.001(4) 0.000 0.000 C9 0.160(12) 0.027(4) 0.034(5) -0.012(4) 0.000 0.000 C10 0.169(14) 0.031(6) 0.049(8) -0.004(5) 0.000 0.000 C11 0.042(4) 0.032(3) 0.033(4) 0.002(3) 0.000 0.000 C12 0.028(3) 0.031(2) 0.047(3) -0.001(2) 0.001(2) 0.003(2) C13 0.033(3) 0.053(3) 0.062(4) 0.009(3) 0.008(3) 0.018(2) C14 0.066(3) 0.064(3) 0.064(4) 0.001(7) 0.021(8) 0.019(3) C15 0.085(5) 0.096(5) 0.107(5) 0.010(4) 0.052(4) 0.035(5) C16 0.065(3) 0.124(4) 0.148(5) 0.009(5) 0.037(5) 0.051(3) C17 0.044(4) 0.166(7) 0.138(5) 0.064(6) 0.010(4) 0.039(5) C18 0.032(3) 0.137(7) 0.094(6) 0.054(6) 0.004(3) 0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.310(5) . ? Er1 O2 2.345(3) 3 ? Er1 O2 2.345(3) 2_755 ? Er1 O6 2.356(5) 2_755 ? Er1 O1 2.411(5) 2_755 ? Er1 O3 2.432(3) 4_755 ? Er1 O3 2.432(3) . ? Er1 O2 2.457(4) 4_755 ? Er1 O2 2.457(4) . ? Er1 C11 2.767(7) 2_755 ? Er1 C12 2.831(5) 4_755 ? Er1 C12 2.831(5) . ? O1 C11 1.300(8) . ? O1 Er1 2.411(5) 2_754 ? O2 C12 1.266(6) . ? O2 Er1 2.345(3) 2_754 ? O3 C12 1.230(11) . ? O4 C2 1.139(13) 8_744 ? O4 C2' 1.418(18) 8_744 ? O4 C16 1.506(10) . ? O4' C2' 0.804(14) 8_744 ? O4' C2 1.426(15) 8_744 ? O4' C16 1.519(15) . ? O5 C5 1.365(11) . ? O5 C3 1.442(10) . ? O6 C11 1.278(8) . ? O6 Er1 2.356(5) 2_754 ? C1 C3 1.491(10) . ? C1 C4 1.527(12) . ? C1 C2 1.529(13) 4_755 ? C1 C2 1.529(13) . ? C1 C2' 1.578(16) . ? C1 C2' 1.578(16) 4_755 ? C2 C2' 0.910(16) . ? C2 O4 1.139(13) 8_756 ? C2 O4' 1.426(15) 8_756 ? C2 C2 1.88(2) 4_755 ? C2' O4' 0.804(14) 8_756 ? C2' O4 1.418(18) 8_756 ? C3 H3A 0.9599 . ? C4 H4A 0.9602 . ? C4 H4B 0.9601 . ? C5 C10 1.324(16) . ? C5 C6 1.343(16) . ? C6 C7 1.362(13) . ? C6 H6A 0.9300 . ? C7 C8 1.383(14) . ? C7 H7A 0.9300 . ? C8 C9 1.297(13) . ? C8 C11 1.478(10) . ? C9 C10 1.454(16) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 Er1 2.767(7) 2_754 ? C12 C13 1.475(7) . ? C13 C14 1.359(16) . ? C13 C18 1.387(10) . ? C14 C15 1.361(10) . ? C14 H14 0.9300 . ? C15 C16 1.355(14) . ? C15 H15 0.9300 . ? C16 C17 1.382(10) . ? C17 C18 1.376(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O2 84.41(14) . 3 ? O1 Er1 O2 84.41(14) . 2_755 ? O2 Er1 O2 66.04(16) 3 2_755 ? O1 Er1 O6 152.34(16) . 2_755 ? O2 Er1 O6 118.22(12) 3 2_755 ? O2 Er1 O6 118.22(12) 2_755 2_755 ? O1 Er1 O1 152.24(16) . 2_755 ? O2 Er1 O1 72.45(13) 3 2_755 ? O2 Er1 O1 72.45(13) 2_755 2_755 ? O6 Er1 O1 55.42(15) 2_755 2_755 ? O1 Er1 O3 101.65(14) . 4_755 ? O2 Er1 O3 136.65(19) 3 4_755 ? O2 Er1 O3 71.85(17) 2_755 4_755 ? O6 Er1 O3 73.51(10) 2_755 4_755 ? O1 Er1 O3 85.79(19) 2_755 4_755 ? O1 Er1 O3 101.65(14) . . ? O2 Er1 O3 71.85(17) 3 . ? O2 Er1 O3 136.65(19) 2_755 . ? O6 Er1 O3 73.51(10) 2_755 . ? O1 Er1 O3 85.79(19) 2_755 . ? O3 Er1 O3 144.7(2) 4_755 . ? O1 Er1 O2 72.19(13) . 4_755 ? O2 Er1 O2 156.59(9) 3 4_755 ? O2 Er1 O2 110.55(13) 2_755 4_755 ? O6 Er1 O2 84.31(12) 2_755 4_755 ? O1 Er1 O2 129.95(11) 2_755 4_755 ? O3 Er1 O2 52.1(2) 4_755 4_755 ? O3 Er1 O2 112.2(2) . 4_755 ? O1 Er1 O2 72.19(13) . . ? O2 Er1 O2 110.55(13) 3 . ? O2 Er1 O2 156.59(9) 2_755 . ? O6 Er1 O2 84.31(12) 2_755 . ? O1 Er1 O2 129.95(11) 2_755 . ? O3 Er1 O2 112.2(2) 4_755 . ? O3 Er1 O2 52.1(2) . . ? O2 Er1 O2 62.66(16) 4_755 . ? O1 Er1 C11 179.76(18) . 2_755 ? O2 Er1 C11 95.80(15) 3 2_755 ? O2 Er1 C11 95.80(15) 2_755 2_755 ? O6 Er1 C11 27.41(17) 2_755 2_755 ? O1 Er1 C11 28.00(17) 2_755 2_755 ? O3 Er1 C11 78.29(15) 4_755 2_755 ? O3 Er1 C11 78.29(15) . 2_755 ? O2 Er1 C11 107.61(14) 4_755 2_755 ? O2 Er1 C11 107.61(14) . 2_755 ? O1 Er1 C12 86.28(12) . 4_755 ? O2 Er1 C12 155.36(13) 3 4_755 ? O2 Er1 C12 90.39(13) 2_755 4_755 ? O6 Er1 C12 78.39(11) 2_755 4_755 ? O1 Er1 C12 108.48(12) 2_755 4_755 ? O3 Er1 C12 25.6(2) 4_755 4_755 ? O3 Er1 C12 132.53(18) . 4_755 ? O2 Er1 C12 26.52(13) 4_755 4_755 ? O2 Er1 C12 88.05(14) . 4_755 ? C11 Er1 C12 93.58(13) 2_755 4_755 ? O1 Er1 C12 86.28(12) . . ? O2 Er1 C12 90.39(13) 3 . ? O2 Er1 C12 155.36(13) 2_755 . ? O6 Er1 C12 78.39(11) 2_755 . ? O1 Er1 C12 108.48(12) 2_755 . ? O3 Er1 C12 132.53(18) 4_755 . ? O3 Er1 C12 25.6(2) . . ? O2 Er1 C12 88.05(14) 4_755 . ? O2 Er1 C12 26.52(13) . . ? C11 Er1 C12 93.58(13) 2_755 . ? C12 Er1 C12 111.7(2) 4_755 . ? C11 O1 Er1 169.9(5) . . ? C11 O1 Er1 91.4(4) . 2_754 ? Er1 O1 Er1 98.63(16) . 2_754 ? C12 O2 Er1 151.7(3) . 2_754 ? C12 O2 Er1 93.4(3) . . ? Er1 O2 Er1 96.39(11) 2_754 . ? C12 O3 Er1 95.6(3) . . ? C2 O4 C2' 39.8(8) 8_744 8_744 ? C2 O4 C16 123.4(10) 8_744 . ? C2' O4 C16 97.1(10) 8_744 . ? C2' O4' C2 36.1(13) 8_744 8_744 ? C2' O4' C16 139.3(16) 8_744 . ? C2 O4' C16 104.9(9) 8_744 . ? C5 O5 C3 117.7(7) . . ? C11 O6 Er1 94.5(4) . 2_754 ? C3 C1 C4 108.1(7) . . ? C3 C1 C2 120.1(6) . 4_755 ? C4 C1 C2 114.9(6) . 4_755 ? C3 C1 C2 120.1(6) . . ? C4 C1 C2 114.9(6) . . ? C2 C1 C2 76.1(11) 4_755 . ? C3 C1 C2' 98.9(5) . . ? C4 C1 C2' 102.3(7) . . ? C2 C1 C2' 110.0(10) 4_755 . ? C2 C1 C2' 34.0(6) . . ? C3 C1 C2' 98.9(5) . 4_755 ? C4 C1 C2' 102.3(7) . 4_755 ? C2 C1 C2' 34.0(6) 4_755 4_755 ? C2 C1 C2' 110.0(10) . 4_755 ? C2' C1 C2' 143.3(14) . 4_755 ? C2' C2 O4 86.9(15) . 8_756 ? C2' C2 O4' 31.4(11) . 8_756 ? O4 C2 O4' 62.9(9) 8_756 8_756 ? C2' C2 C1 75.9(15) . . ? O4 C2 C1 128.2(12) 8_756 . ? O4' C2 C1 106.8(10) 8_756 . ? C2' C2 C2 127.6(13) . 4_755 ? O4 C2 C2 127.3(8) 8_756 4_755 ? O4' C2 C2 158.7(7) 8_756 4_755 ? C1 C2 C2 51.9(5) . 4_755 ? O4' C2' C2 112(2) 8_756 . ? O4' C2' O4 69.3(13) 8_756 8_756 ? C2 C2' O4 53.3(11) . 8_756 ? O4' C2' C1 169(2) 8_756 . ? C2 C2' C1 70.0(13) . . ? O4 C2' C1 106.7(10) 8_756 . ? O5 C3 C1 109.3(6) . . ? O5 C3 H3A 110.2 . . ? C1 C3 H3A 109.4 . . ? C1 C4 H4A 109.3 . . ? C1 C4 H4B 109.6 . . ? H4A C4 H4B 109.5 . . ? C10 C5 C6 120.5(12) . . ? C10 C5 O5 123.0(13) . . ? C6 C5 O5 116.5(8) . . ? C5 C6 C7 122.7(9) . . ? C5 C6 H6A 118.6 . . ? C7 C6 H6A 118.6 . . ? C6 C7 C8 118.6(9) . . ? C6 C7 H7A 120.7 . . ? C8 C7 H7A 120.7 . . ? C9 C8 C7 118.7(9) . . ? C9 C8 C11 120.4(8) . . ? C7 C8 C11 120.9(8) . . ? C8 C9 C10 122.9(9) . . ? C8 C9 H9A 118.5 . . ? C10 C9 H9A 118.5 . . ? C5 C10 C9 116.5(12) . . ? C5 C10 H10A 121.7 . . ? C9 C10 H10A 121.7 . . ? O6 C11 O1 118.6(6) . . ? O6 C11 C8 119.8(6) . . ? O1 C11 C8 121.6(6) . . ? O6 C11 Er1 58.1(4) . 2_754 ? O1 C11 Er1 60.6(3) . 2_754 ? C8 C11 Er1 177.9(5) . 2_754 ? O3 C12 O2 118.7(4) . . ? O3 C12 C13 121.8(5) . . ? O2 C12 C13 119.5(5) . . ? O3 C12 Er1 58.7(2) . . ? O2 C12 Er1 60.0(2) . . ? C13 C12 Er1 177.5(4) . . ? C14 C13 C18 118.6(6) . . ? C14 C13 C12 122.1(6) . . ? C18 C13 C12 119.2(6) . . ? C13 C14 C15 121.1(10) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 120.6(11) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.0(8) . . ? C15 C16 O4 144.6(13) . . ? C17 C16 O4 92.5(9) . . ? C15 C16 O4' 96.8(10) . . ? C17 C16 O4' 143.0(9) . . ? O4 C16 O4' 53.5(7) . . ? C18 C17 C16 118.9(8) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C13 120.7(9) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.18 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.846 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.088 #===END # Attachment 'CIAC-D1Y.cif' data_C29 _database_code_depnum_ccdc_archive 'CCDC 852925' #TrackingRef 'CIAC-D1Y.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 N O10 Y' _chemical_formula_weight 639.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 18.0366(10) _cell_length_b 24.1755(13) _cell_length_c 6.9866(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3046.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 1.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5950 _exptl_absorpt_correction_T_max 0.7453 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3018 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.09 _reflns_number_total 3018 _reflns_number_gt 2660 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+1.5208P] 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 0.030(13) _refine_ls_number_reflns 3018 _refine_ls_number_parameters 205 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.5000 0.51617(2) 1.51261(13) 0.02517(18) Uani 1 2 d S . . O1 O 0.5000 0.8020(2) 0.8372(9) 0.0539(15) Uani 1 2 d S . . O2 O 0.5894(5) 0.9257(4) 0.5437(15) 0.066(3) Uani 0.50 1 d PU . . O2' O 0.6257(4) 0.8923(4) 0.6793(14) 0.051(2) Uani 0.50 1 d PU . . O3 O 0.5000 0.6134(2) 1.4666(6) 0.0428(14) Uani 1 2 d S . . O4 O 0.5000 0.56170(18) 1.2051(7) 0.0311(11) Uani 1 2 d S . . O5 O 0.92958(17) 0.96208(15) 0.3026(5) 0.0308(7) Uani 1 1 d . . . O6 O 0.87112(17) 0.95424(16) 0.0332(8) 0.0458(9) Uani 1 1 d . . . C1 C 0.5000 0.8982(3) 0.7760(11) 0.0325(16) Uani 1 2 d S . . C2 C 0.5000 0.8557(4) 0.9298(14) 0.061(3) Uani 1 2 d S . . H2B H 0.5435 0.8597 1.0076 0.074 Uiso 0.50 1 d PR . . C3 C 0.5000 0.9562(4) 0.8727(17) 0.075(3) Uani 1 2 d S . . H3A H 0.5000 0.9849 0.7776 0.113 Uiso 1 2 d SR . . H3B H 0.5435 0.9596 0.9512 0.113 Uiso 0.50 1 d PR . . C4' C 0.5520(6) 0.8927(5) 0.6037(18) 0.036(2) Uani 0.50 1 d P . . C4 C 0.5806(9) 0.8944(5) 0.711(2) 0.047(3) Uani 0.50 1 d PU . . C5 C 0.5000 0.7575(3) 0.9553(10) 0.053(2) Uani 1 2 d SDU . . C6 C 0.5000 0.7068(3) 0.8647(13) 0.053(2) Uani 1 2 d SD . . H6 H 0.5000 0.7048 0.7318 0.064 Uiso 1 2 calc SR . . C7 C 0.5000 0.6594(3) 0.9720(9) 0.047(2) Uani 1 2 d SD . . H7 H 0.5000 0.6254 0.9099 0.056 Uiso 1 2 calc SR . . C8 C 0.5000 0.6606(3) 1.1683(10) 0.0391(18) Uani 1 2 d SD . . C9 C 0.5000 0.7114(3) 1.2567(14) 0.086(4) Uani 1 2 d SDU . . H9 H 0.5000 0.7133 1.3896 0.103 Uiso 1 2 calc SR . . C10 C 0.5000 0.7599(4) 1.1508(13) 0.098(5) Uani 1 2 d SDU . . H10 H 0.5000 0.7939 1.2126 0.118 Uiso 1 2 calc SR . . C11 C 0.5000 0.6099(3) 1.2857(10) 0.0331(16) Uani 1 2 d S . . C12 C 0.6735(4) 0.9143(4) 0.5117(18) 0.110(2) Uani 1 1 d DU . . C13 C 0.7400(4) 0.9112(4) 0.6055(13) 0.092(3) Uani 1 1 d DU . . H13 H 0.7421 0.9010 0.7337 0.110 Uiso 1 1 calc R . . C14 C 0.8029(4) 0.9235(3) 0.5067(12) 0.0688(19) Uani 1 1 d DU . . H14 H 0.8482 0.9223 0.5701 0.083 Uiso 1 1 calc R . . C15 C 0.8015(3) 0.9374(3) 0.3168(9) 0.0521(15) Uani 1 1 d DU . . C16 C 0.7338(3) 0.9408(4) 0.2250(13) 0.094(3) Uani 1 1 d DU . . H16 H 0.7317 0.9496 0.0956 0.113 Uiso 1 1 calc R . . C17 C 0.6692(5) 0.9309(4) 0.3254(16) 0.112(3) Uani 1 1 d DU . . H17 H 0.6234 0.9356 0.2667 0.135 Uiso 1 1 calc R . . C18 C 0.8700(3) 0.9521(2) 0.2099(8) 0.0325(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0240(3) 0.0361(3) 0.0154(3) -0.0014(4) 0.000 0.000 O1 0.083(4) 0.044(3) 0.035(3) 0.005(3) 0.000 0.000 O2 0.066(4) 0.092(6) 0.039(7) 0.033(6) -0.005(5) -0.014(4) O2' 0.016(3) 0.072(5) 0.064(5) 0.015(4) -0.011(3) -0.002(4) O3 0.067(3) 0.044(3) 0.017(3) 0.0055(19) 0.000 0.000 O4 0.047(3) 0.029(2) 0.017(2) -0.001(2) 0.000 0.000 O5 0.0260(16) 0.0426(18) 0.0237(18) -0.0032(16) 0.0018(13) -0.0053(15) O6 0.0338(16) 0.073(2) 0.031(2) 0.010(3) -0.008(2) -0.0103(15) C1 0.025(3) 0.040(4) 0.033(4) 0.010(3) 0.000 0.000 C2 0.100(7) 0.044(5) 0.039(5) 0.005(4) 0.000 0.000 C3 0.123(9) 0.047(5) 0.056(6) -0.003(5) 0.000 0.000 C4' 0.027(5) 0.048(6) 0.034(6) 0.023(5) 0.009(4) -0.001(5) C4 0.043(5) 0.052(5) 0.045(5) 0.014(4) -0.003(4) 0.001(4) C5 0.080(6) 0.040(5) 0.038(6) 0.011(3) 0.000 0.000 C6 0.078(6) 0.049(6) 0.031(5) 0.015(4) 0.000 0.000 C7 0.074(5) 0.041(4) 0.025(6) 0.002(3) 0.000 0.000 C8 0.049(4) 0.038(4) 0.030(4) 0.003(3) 0.000 0.000 C9 0.200(14) 0.032(5) 0.025(5) -0.006(3) 0.000 0.000 C10 0.219(15) 0.026(5) 0.051(7) -0.003(5) 0.000 0.000 C11 0.042(4) 0.032(4) 0.026(4) 0.006(3) 0.000 0.000 C12 0.074(3) 0.129(4) 0.127(5) -0.004(5) 0.035(4) -0.050(3) C13 0.068(3) 0.110(6) 0.097(6) -0.016(5) 0.056(3) -0.039(4) C14 0.075(4) 0.073(4) 0.059(4) -0.004(5) 0.035(6) -0.028(3) C15 0.036(3) 0.065(4) 0.055(4) -0.014(3) 0.007(3) -0.019(3) C16 0.023(3) 0.174(9) 0.085(6) -0.061(6) 0.010(3) -0.023(4) C17 0.073(4) 0.140(5) 0.124(5) -0.029(4) 0.003(4) -0.024(4) C18 0.026(2) 0.033(3) 0.038(3) -0.002(2) 0.000(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O4 2.314(5) 2_665 ? Y1 O5 2.340(3) 5_446 ? Y1 O5 2.340(3) 8_646 ? Y1 O3 2.373(5) . ? Y1 O4 2.414(5) . ? Y1 O6 2.436(3) 6_666 ? Y1 O6 2.436(3) 7_466 ? Y1 O5 2.449(3) 6_666 ? Y1 O5 2.449(3) 7_466 ? Y1 C11 2.765(7) . ? Y1 C18 2.826(5) 6_666 ? Y1 C18 2.826(5) 7_466 ? O1 C5 1.356(10) . ? O1 C2 1.451(11) . ? O2 C4' 1.126(12) . ? O2 C4 1.399(16) . ? O2 O2' 1.406(13) . ? O2 C12 1.557(13) . ? O2' C4 0.844(14) . ? O2' C4' 1.431(13) . ? O2' C12 1.548(14) . ? O3 C11 1.267(8) . ? O4 C11 1.294(9) . ? O4 Y1 2.314(5) 2_664 ? O5 C18 1.278(6) . ? O5 Y1 2.340(3) 5_554 ? O5 Y1 2.449(3) 6_663 ? O6 C18 1.236(8) . ? O6 Y1 2.436(3) 6_663 ? C1 C2 1.486(11) . ? C1 C4 1.526(16) . ? C1 C4 1.526(16) 4_655 ? C1 C4' 1.531(13) . ? C1 C4' 1.531(13) 4_655 ? C1 C3 1.557(13) . ? C4' C4 0.908(15) . ? C4' C4' 1.88(2) 4_655 ? C5 C10 1.367(9) . ? C5 C6 1.380(9) . ? C6 C7 1.368(9) . ? C7 C8 1.372(9) . ? C8 C9 1.375(8) . ? C8 C11 1.476(10) . ? C9 C10 1.385(9) . ? C12 C17 1.364(10) . ? C12 C13 1.369(9) . ? C13 C14 1.361(7) . ? C14 C15 1.369(9) . ? C15 C16 1.382(8) . ? C15 C18 1.487(7) . ? C16 C17 1.379(9) . ? C18 Y1 2.826(5) 6_663 ? 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 O4 Y1 O5 84.82(14) 2_665 5_446 ? O4 Y1 O5 84.82(14) 2_665 8_646 ? O5 Y1 O5 65.75(16) 5_446 8_646 ? O4 Y1 O3 152.24(17) 2_665 . ? O5 Y1 O3 117.96(12) 5_446 . ? O5 Y1 O3 117.96(12) 8_646 . ? O4 Y1 O4 152.67(16) 2_665 . ? O5 Y1 O4 72.36(13) 5_446 . ? O5 Y1 O4 72.36(13) 8_646 . ? O3 Y1 O4 55.09(15) . . ? O4 Y1 O6 101.80(11) 2_665 6_666 ? O5 Y1 O6 135.97(14) 5_446 6_666 ? O5 Y1 O6 71.53(13) 8_646 6_666 ? O3 Y1 O6 73.57(10) . 6_666 ? O4 Y1 O6 85.33(13) . 6_666 ? O4 Y1 O6 101.80(12) 2_665 7_466 ? O5 Y1 O6 71.53(13) 5_446 7_466 ? O5 Y1 O6 135.96(14) 8_646 7_466 ? O3 Y1 O6 73.57(10) . 7_466 ? O4 Y1 O6 85.33(13) . 7_466 ? O6 Y1 O6 145.16(19) 6_666 7_466 ? O4 Y1 O5 72.16(13) 2_665 6_666 ? O5 Y1 O5 156.98(9) 5_446 6_666 ? O5 Y1 O5 110.93(12) 8_646 6_666 ? O3 Y1 O5 84.22(12) . 6_666 ? O4 Y1 O5 129.69(11) . 6_666 ? O6 Y1 O5 52.65(14) 6_666 6_666 ? O6 Y1 O5 112.52(15) 7_466 6_666 ? O4 Y1 O5 72.16(13) 2_665 7_466 ? O5 Y1 O5 110.93(12) 5_446 7_466 ? O5 Y1 O5 156.98(9) 8_646 7_466 ? O3 Y1 O5 84.22(12) . 7_466 ? O4 Y1 O5 129.69(11) . 7_466 ? O6 Y1 O5 112.52(15) 6_666 7_466 ? O6 Y1 O5 52.65(14) 7_466 7_466 ? O5 Y1 O5 62.49(15) 6_666 7_466 ? O4 Y1 C11 179.4(2) 2_665 . ? O5 Y1 C11 95.65(16) 5_446 . ? O5 Y1 C11 95.65(16) 8_646 . ? O3 Y1 C11 27.20(19) . . ? O4 Y1 C11 27.89(19) . . ? O6 Y1 C11 78.07(12) 6_666 . ? O6 Y1 C11 78.07(12) 7_466 . ? O5 Y1 C11 107.37(16) 6_666 . ? O5 Y1 C11 107.37(15) 7_466 . ? O4 Y1 C18 86.40(13) 2_665 6_666 ? O5 Y1 C18 155.20(13) 5_446 6_666 ? O5 Y1 C18 90.40(13) 8_646 6_666 ? O3 Y1 C18 78.30(12) . 6_666 ? O4 Y1 C18 108.08(12) . 6_666 ? O6 Y1 C18 25.83(18) 6_666 6_666 ? O6 Y1 C18 133.10(15) 7_466 6_666 ? O5 Y1 C18 26.84(13) 6_666 6_666 ? O5 Y1 C18 88.19(13) 7_466 6_666 ? C11 Y1 C18 93.28(14) . 6_666 ? O4 Y1 C18 86.40(13) 2_665 7_466 ? O5 Y1 C18 90.40(13) 5_446 7_466 ? O5 Y1 C18 155.20(13) 8_646 7_466 ? O3 Y1 C18 78.30(12) . 7_466 ? O4 Y1 C18 108.08(12) . 7_466 ? O6 Y1 C18 133.10(15) 6_666 7_466 ? O6 Y1 C18 25.83(18) 7_466 7_466 ? O5 Y1 C18 88.19(13) 6_666 7_466 ? O5 Y1 C18 26.84(13) 7_466 7_466 ? C11 Y1 C18 93.28(14) . 7_466 ? C18 Y1 C18 112.1(2) 6_666 7_466 ? C5 O1 C2 116.0(6) . . ? C4' O2 C4 40.4(8) . . ? C4' O2 O2' 67.8(8) . . ? C4 O2 O2' 35.0(6) . . ? C4' O2 C12 120.7(10) . . ? C4 O2 C12 97.7(9) . . ? O2' O2 C12 62.7(7) . . ? C4 O2' O2 72.0(11) . . ? C4 O2' C4' 36.8(11) . . ? O2 O2' C4' 46.8(6) . . ? C4 O2' C12 135.4(13) . . ? O2 O2' C12 63.4(7) . . ? C4' O2' C12 103.6(8) . . ? C11 O3 Y1 93.9(4) . . ? C11 O4 Y1 170.2(5) . 2_664 ? C11 O4 Y1 91.3(4) . . ? Y1 O4 Y1 98.42(16) 2_664 . ? C18 O5 Y1 151.6(3) . 5_554 ? C18 O5 Y1 93.3(3) . 6_663 ? Y1 O5 Y1 96.73(11) 5_554 6_663 ? C18 O6 Y1 95.0(3) . 6_663 ? C2 C1 C4 100.1(6) . . ? C2 C1 C4 100.1(6) . 4_655 ? C4 C1 C4 144.4(13) . 4_655 ? C2 C1 C4' 120.6(6) . . ? C4 C1 C4' 34.6(6) . . ? C4 C1 C4' 110.0(10) 4_655 . ? C2 C1 C4' 120.6(6) . 4_655 ? C4 C1 C4' 110.0(10) . 4_655 ? C4 C1 C4' 34.6(6) 4_655 4_655 ? C4' C1 C4' 75.5(10) . 4_655 ? C2 C1 C3 108.0(7) . . ? C4 C1 C3 100.6(6) . . ? C4 C1 C3 100.6(6) 4_655 . ? C4' C1 C3 114.8(7) . . ? C4' C1 C3 114.8(7) 4_655 . ? O1 C2 C1 107.2(7) . . ? C4 C4' O2 86.2(14) . . ? C4 C4' O2' 33.8(11) . . ? O2 C4' O2' 65.5(8) . . ? C4 C4' C1 72.4(13) . . ? O2 C4' C1 126.7(12) . . ? O2' C4' C1 106.2(9) . . ? C4 C4' C4' 124.6(13) . 4_655 ? O2 C4' C4' 126.8(7) . 4_655 ? O2' C4' C4' 158.3(6) . 4_655 ? C1 C4' C4' 52.3(5) . 4_655 ? O2' C4 C4' 109(2) . . ? O2' C4 O2 72.9(12) . . ? C4' C4 O2 53.4(10) . . ? O2' C4 C1 177.6(19) . . ? C4' C4 C1 73.0(14) . . ? O2 C4 C1 109.0(11) . . ? O1 C5 C10 125.1(8) . . ? O1 C5 C6 115.2(7) . . ? C10 C5 C6 119.7(8) . . ? C7 C6 C5 119.5(8) . . ? C6 C7 C8 122.0(8) . . ? C7 C8 C9 117.9(7) . . ? C7 C8 C11 122.6(7) . . ? C9 C8 C11 119.5(7) . . ? C8 C9 C10 121.0(8) . . ? C5 C10 C9 119.9(9) . . ? O3 C11 O4 119.7(7) . . ? O3 C11 C8 119.9(7) . . ? O4 C11 C8 120.4(6) . . ? O3 C11 Y1 58.9(4) . . ? O4 C11 Y1 60.8(4) . . ? C8 C11 Y1 178.8(5) . . ? C17 C12 C13 121.4(8) . . ? C17 C12 O2' 142.4(7) . . ? C13 C12 O2' 96.1(8) . . ? C17 C12 O2 91.8(8) . . ? C13 C12 O2 142.5(11) . . ? O2' C12 O2 53.9(5) . . ? C14 C13 C12 118.4(8) . . ? C13 C14 C15 121.9(7) . . ? C14 C15 C16 118.7(6) . . ? C14 C15 C18 122.0(5) . . ? C16 C15 C18 119.2(6) . . ? C17 C16 C15 120.0(8) . . ? C12 C17 C16 119.3(9) . . ? O6 C18 O5 119.0(4) . . ? O6 C18 C15 121.7(4) . . ? O5 C18 C15 119.3(5) . . ? O6 C18 Y1 59.2(2) . 6_663 ? O5 C18 Y1 59.9(2) . 6_663 ? C15 C18 Y1 178.0(4) . 6_663 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.105 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.084 #===END