# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Niu, Shuyun' _publ_contact_author_email syniu@sohu.com _publ_section_title ; Synthesis, structure of a series of new luminescent Ag-Ln coordination polymers and the influence of introduction of Ag(I) ion on the NIR luminescence from Ln(III) centre ; loop_ _publ_author_name 'Shuyun Niu' 'Jin Jing' 'Qian Han' 'Yuxian Chi' # Attachment '- 743494-complex 2.CIF' data_bb _database_code_depnum_ccdc_archive 'CCDC 743494' #TrackingRef '- 743494-complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Ag5 O16 Yb' _chemical_formula_weight 1368.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.816(5) _cell_length_b 14.875(13) _cell_length_c 15.196(11) _cell_angle_alpha 63.78(3) _cell_angle_beta 81.62(3) _cell_angle_gamma 81.61(3) _cell_volume 1561(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11114 _cell_measurement_theta_min 6.13 _cell_measurement_theta_max 55.79 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 6.123 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2185 _exptl_absorpt_correction_T_max 0.4876 _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12659 _diffrn_reflns_av_R_equivalents 0.1077 _diffrn_reflns_av_sigmaI/netI 0.1414 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5793 _reflns_number_gt 4419 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1028P)^2^+82.0680P] 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 5793 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.2639 _refine_ls_wR_factor_gt 0.2492 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.35291(9) 0.25083(5) 0.25100(5) 0.0152(2) Uani 1 1 d . . . Ag1 Ag 0.1312(2) 0.09114(10) 0.49240(11) 0.0275(4) Uani 1 1 d . . . Ag2 Ag 0.1805(2) 0.40837(10) 0.00676(11) 0.0283(4) Uani 1 1 d . . . Ag3 Ag -0.2132(2) 0.33026(12) 0.01868(14) 0.0394(5) Uani 1 1 d . . . Ag4 Ag -0.3033(2) 0.17140(12) 0.48470(14) 0.0387(5) Uani 1 1 d . . . Ag5 Ag -0.1477(2) 0.25114(12) 0.25187(14) 0.0363(4) Uani 1 1 d . . . O1 O 0.1017(18) 0.2539(10) 0.0329(11) 0.033(3) Uani 1 1 d . . . O2 O 0.3145(17) 0.2159(10) 0.1253(10) 0.024(3) Uani 1 1 d . . . O3 O 0.1445(17) -0.0139(9) 0.4050(9) 0.025(3) Uani 1 1 d . . . O4 O 0.1183(15) 0.1456(9) 0.2989(9) 0.020(3) Uani 1 1 d . . . O5 O -0.0266(18) 0.2443(10) 0.4660(11) 0.035(4) Uani 1 1 d . . . O6 O 0.2205(17) 0.2877(9) 0.3735(10) 0.024(3) Uani 1 1 d . . . O7 O 0.0850(17) 0.5139(9) 0.0947(9) 0.026(3) Uani 1 1 d . . . O8 O 0.0868(15) 0.3549(8) 0.2022(9) 0.018(3) Uani 1 1 d . . . O9 O 0.558(2) 0.3383(11) 0.4368(12) 0.037(4) Uani 1 1 d . . . O10 O 0.5699(15) 0.3044(9) 0.3078(10) 0.021(3) Uani 1 1 d . . . O11 O 0.7069(18) 0.4407(10) 0.0953(11) 0.032(3) Uani 1 1 d . . . O12 O 0.4383(18) 0.3955(9) 0.1275(11) 0.031(3) Uani 1 1 d . . . O13 O 0.7255(17) 0.0623(9) 0.4075(10) 0.027(3) Uani 1 1 d . . . O14 O 0.4487(15) 0.1066(9) 0.3752(9) 0.022(3) Uani 1 1 d . . . O15 O 0.6344(16) 0.1985(9) 0.1939(10) 0.021(3) Uani 1 1 d . . . O16 O 0.7184(18) 0.1669(11) 0.0649(10) 0.029(3) Uani 1 1 d . . . C1 C 0.192(2) 0.1908(13) 0.0983(13) 0.021(4) Uani 1 1 d . . . C2 C 0.161(3) 0.0816(13) 0.1378(15) 0.025(4) Uani 1 1 d . . . C3 C 0.155(3) 0.0463(16) 0.0679(16) 0.040(5) Uani 1 1 d . . . H3A H 0.1664 0.0895 0.0011 0.047 Uiso 1 1 calc R . . C4 C 0.130(3) -0.053(2) 0.098(2) 0.050(7) Uani 1 1 d . . . H4A H 0.1338 -0.0782 0.0512 0.060 Uiso 1 1 calc R . . C5 C 0.100(3) -0.1188(16) 0.1992(17) 0.036(5) Uani 1 1 d . . . H5A H 0.0784 -0.1853 0.2193 0.044 Uiso 1 1 calc R . . C6 C 0.102(3) -0.0807(15) 0.2670(17) 0.031(5) Uani 1 1 d . . . H6A H 0.0857 -0.1231 0.3338 0.037 Uiso 1 1 calc R . . C7 C 0.130(2) 0.0190(12) 0.2383(15) 0.026(4) Uani 1 1 d . . . C8 C 0.132(2) 0.0513(12) 0.3164(13) 0.018(4) Uani 1 1 d . . . C9 C 0.067(3) 0.3088(15) 0.3975(15) 0.029(5) Uani 1 1 d . . . C10 C -0.010(3) 0.4153(15) 0.3624(15) 0.027(4) Uani 1 1 d . . . C11 C -0.091(3) 0.4525(16) 0.4297(17) 0.038(5) Uani 1 1 d . . . H11A H -0.1084 0.4086 0.4960 0.046 Uiso 1 1 calc R . . C12 C -0.143(4) 0.553(2) 0.399(2) 0.055(7) Uani 1 1 d . . . H12A H -0.1883 0.5768 0.4456 0.066 Uiso 1 1 calc R . . C13 C -0.131(3) 0.6178(16) 0.3014(18) 0.043(6) Uani 1 1 d . . . H13A H -0.1654 0.6860 0.2816 0.052 Uiso 1 1 calc R . . C14 C -0.069(3) 0.5821(14) 0.2328(15) 0.028(4) Uani 1 1 d . . . H14A H -0.0726 0.6254 0.1663 0.034 Uiso 1 1 calc R . . C15 C 0.000(2) 0.4823(13) 0.2598(13) 0.019(4) Uani 1 1 d . . . C16 C 0.057(2) 0.4478(13) 0.1814(12) 0.021(4) Uani 1 1 d . . . C17 C 0.538(2) 0.3633(14) 0.3514(14) 0.025(4) Uani 1 1 d . . . C18 C 0.486(3) 0.4723(15) 0.2899(15) 0.029(4) Uani 1 1 d . . . C19 C 0.427(3) 0.5395(18) 0.331(2) 0.043(6) Uani 1 1 d . . . H19A H 0.4146 0.5144 0.3995 0.052 Uiso 1 1 calc R . . C20 C 0.386(3) 0.6387(18) 0.278(2) 0.047(6) Uani 1 1 d . . . H20A H 0.3461 0.6809 0.3086 0.056 Uiso 1 1 calc R . . C21 C 0.405(3) 0.6762(15) 0.1748(19) 0.040(5) Uani 1 1 d . . . H21A H 0.3752 0.7441 0.1362 0.048 Uiso 1 1 calc R . . C22 C 0.467(3) 0.6130(15) 0.1297(18) 0.037(5) Uani 1 1 d . . . H22A H 0.4852 0.6394 0.0614 0.044 Uiso 1 1 calc R . . C23 C 0.502(2) 0.5121(13) 0.1852(13) 0.019(4) Uani 1 1 d . . . C24 C 0.555(2) 0.4422(13) 0.1345(13) 0.019(3) Uiso 1 1 d . . . C25 C 0.659(2) 0.1403(13) 0.1536(14) 0.018(4) Uani 1 1 d . . . C26 C 0.624(2) 0.0316(13) 0.2139(15) 0.025(4) Uani 1 1 d . . . C27 C 0.625(3) -0.0314(16) 0.1669(17) 0.037(5) Uani 1 1 d . . . H27A H 0.6423 -0.0067 0.0987 0.044 Uiso 1 1 calc R . . C28 C 0.597(4) -0.1329(18) 0.2267(19) 0.046(6) Uani 1 1 d . . . H28A H 0.5806 -0.1738 0.1975 0.056 Uiso 1 1 calc R . . C29 C 0.595(3) -0.1713(18) 0.3234(19) 0.042(6) Uani 1 1 d . . . H29A H 0.5901 -0.2402 0.3604 0.051 Uiso 1 1 calc R . . C30 C 0.600(3) -0.1095(15) 0.3722(17) 0.030(4) Uani 1 1 d . . . H30A H 0.5975 -0.1374 0.4404 0.036 Uiso 1 1 calc R . . C31 C 0.609(2) -0.0059(13) 0.3159(14) 0.022(4) Uani 1 1 d . . . C32 C 0.597(3) 0.0593(13) 0.3695(14) 0.028(4) 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 Yb1 0.0135(4) 0.0121(4) 0.0145(4) 0.0004(3) -0.0019(3) -0.0040(3) Ag1 0.0292(8) 0.0189(7) 0.0231(7) 0.0009(6) -0.0035(6) 0.0004(6) Ag2 0.0340(8) 0.0178(7) 0.0239(7) 0.0022(6) -0.0041(6) -0.0105(6) Ag3 0.0393(9) 0.0240(8) 0.0453(10) -0.0068(7) 0.0058(8) -0.0102(7) Ag4 0.0393(10) 0.0255(8) 0.0464(10) -0.0083(7) -0.0179(8) 0.0021(7) Ag5 0.0244(8) 0.0287(8) 0.0582(12) -0.0203(8) -0.0038(8) -0.0044(6) O1 0.026(7) 0.030(7) 0.035(8) 0.001(6) -0.021(7) -0.008(6) O2 0.024(7) 0.027(7) 0.028(7) -0.015(6) -0.009(6) -0.004(5) O3 0.027(7) 0.015(6) 0.017(6) 0.006(5) -0.002(5) -0.005(5) O4 0.007(5) 0.023(6) 0.025(6) -0.005(5) -0.001(5) -0.004(4) O5 0.027(7) 0.024(7) 0.036(8) 0.006(6) -0.003(6) -0.009(6) O6 0.022(7) 0.021(6) 0.030(7) -0.011(6) -0.010(6) 0.004(5) O7 0.025(7) 0.022(6) 0.016(6) 0.007(5) -0.008(5) -0.002(5) O8 0.012(6) 0.010(5) 0.028(7) -0.003(5) -0.006(5) 0.000(4) O9 0.036(9) 0.033(8) 0.044(9) -0.017(7) -0.014(7) 0.002(6) O10 0.011(6) 0.020(6) 0.031(7) -0.011(5) -0.002(5) -0.004(5) O11 0.030(7) 0.019(6) 0.039(8) -0.006(6) 0.009(6) -0.011(5) O12 0.028(7) 0.012(6) 0.043(8) 0.005(6) -0.023(7) -0.006(5) O13 0.026(7) 0.018(6) 0.031(7) 0.002(5) -0.023(6) -0.005(5) O14 0.013(6) 0.014(6) 0.026(7) 0.004(5) -0.003(5) -0.003(5) O15 0.017(6) 0.017(6) 0.031(7) -0.010(5) -0.003(6) -0.005(5) O16 0.025(7) 0.038(8) 0.023(7) -0.018(6) 0.004(6) 0.007(6) C1 0.017(9) 0.019(9) 0.022(9) -0.005(7) 0.001(7) -0.008(7) C2 0.029(10) 0.018(9) 0.040(11) -0.020(8) -0.009(9) -0.005(7) C3 0.057(15) 0.031(11) 0.028(11) -0.008(9) -0.018(11) 0.004(10) C4 0.050(15) 0.050(15) 0.08(2) -0.052(15) -0.025(14) 0.005(12) C5 0.046(13) 0.026(10) 0.039(12) -0.010(9) -0.026(11) 0.001(9) C6 0.037(12) 0.023(10) 0.042(12) -0.017(9) -0.017(10) -0.002(8) C7 0.025(10) 0.005(7) 0.033(11) 0.006(7) 0.001(8) -0.003(6) C8 0.015(8) 0.008(7) 0.019(8) 0.006(6) -0.007(7) 0.003(6) C9 0.022(10) 0.029(10) 0.028(10) 0.002(8) -0.021(9) -0.008(8) C10 0.021(9) 0.030(10) 0.031(10) -0.014(9) -0.004(8) -0.002(8) C11 0.046(13) 0.027(11) 0.031(11) -0.007(9) 0.004(10) 0.003(9) C12 0.070(19) 0.059(17) 0.047(15) -0.040(14) 0.008(14) 0.000(14) C13 0.056(15) 0.020(10) 0.042(13) -0.011(9) -0.002(11) 0.019(10) C14 0.027(10) 0.014(8) 0.031(10) 0.001(8) 0.000(9) -0.004(7) C15 0.012(8) 0.017(8) 0.023(9) -0.008(7) 0.007(7) 0.001(6) C16 0.015(8) 0.026(9) 0.010(8) 0.005(7) -0.004(7) -0.004(7) C17 0.015(9) 0.026(10) 0.027(10) 0.001(8) -0.014(8) -0.006(7) C18 0.035(11) 0.027(10) 0.029(10) -0.014(8) -0.013(9) -0.002(8) C19 0.042(13) 0.039(13) 0.063(16) -0.039(12) -0.004(12) 0.009(10) C20 0.046(14) 0.031(12) 0.063(17) -0.028(12) 0.021(12) -0.002(10) C21 0.040(13) 0.015(9) 0.058(15) -0.010(10) -0.008(11) -0.002(8) C22 0.031(11) 0.028(10) 0.047(13) -0.005(10) -0.010(10) -0.016(9) C23 0.010(8) 0.028(9) 0.022(9) -0.010(7) -0.009(7) -0.004(6) C25 0.006(7) 0.022(9) 0.029(10) -0.015(8) 0.002(7) -0.003(6) C26 0.019(9) 0.015(8) 0.036(11) -0.006(8) -0.007(8) 0.001(7) C27 0.054(14) 0.027(10) 0.030(11) -0.013(9) 0.000(10) -0.010(9) C28 0.063(17) 0.036(13) 0.055(16) -0.034(12) 0.014(13) -0.022(11) C29 0.048(14) 0.031(12) 0.049(14) -0.018(11) -0.007(12) -0.001(10) C30 0.021(10) 0.026(10) 0.038(11) -0.011(9) -0.003(9) 0.001(7) C31 0.014(8) 0.016(8) 0.027(10) 0.003(7) -0.009(7) -0.010(6) C32 0.031(11) 0.011(8) 0.022(9) 0.012(7) -0.011(9) 0.000(7) _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 O6 2.238(14) . ? Yb1 O12 2.255(13) . ? Yb1 O14 2.256(12) . ? Yb1 O2 2.258(12) . ? Yb1 O10 2.384(12) . ? Yb1 O15 2.396(13) . ? Yb1 O8 2.401(11) . ? Yb1 O4 2.405(11) . ? Yb1 C24 3.127(17) . ? Yb1 C32 3.141(17) . ? Yb1 Ag1 3.708(3) . ? Yb1 Ag2 3.733(3) . ? Ag1 O5 2.322(15) . ? Ag1 O13 2.337(12) 2_656 ? Ag1 O3 2.442(14) . ? Ag1 O3 2.561(13) 2_556 ? Ag2 O11 2.307(13) 2_665 ? Ag2 O1 2.313(14) . ? Ag2 O7 2.456(15) . ? Ag2 O7 2.584(12) 2_565 ? Ag3 O16 2.334(15) 1_455 ? Ag3 O11 2.371(15) 1_455 ? Ag3 O7 2.448(13) 2_565 ? Ag3 O1 2.553(14) . ? Ag3 Ag5 3.297(4) . ? Ag4 O13 2.358(14) 1_455 ? Ag4 O9 2.392(15) 1_455 ? Ag4 O3 2.475(12) 2_556 ? Ag4 O5 2.483(14) . ? Ag4 Ag5 3.296(4) . ? Ag5 O8 2.388(11) . ? Ag5 O15 2.392(12) 1_455 ? Ag5 O10 2.399(12) 1_455 ? Ag5 O4 2.406(12) . ? O1 C1 1.25(2) . ? O2 C1 1.25(2) . ? O3 C8 1.27(2) . ? O3 Ag4 2.475(12) 2_556 ? O3 Ag1 2.561(13) 2_556 ? O4 C8 1.30(2) . ? O5 C9 1.28(2) . ? O6 C9 1.24(2) . ? O7 C16 1.26(2) . ? O7 Ag3 2.448(13) 2_565 ? O7 Ag2 2.584(12) 2_565 ? O8 C16 1.27(2) . ? O9 C17 1.21(2) . ? O9 Ag4 2.392(15) 1_655 ? O10 C17 1.29(2) . ? O10 Ag5 2.399(12) 1_655 ? O11 C24 1.25(2) . ? O11 Ag2 2.307(13) 2_665 ? O11 Ag3 2.371(15) 1_655 ? O12 C24 1.27(2) . ? O13 C32 1.25(2) . ? O13 Ag1 2.337(12) 2_656 ? O13 Ag4 2.358(14) 1_655 ? O14 C32 1.27(2) . ? O15 C25 1.24(2) . ? O15 Ag5 2.392(12) 1_655 ? O16 C25 1.26(2) . ? O16 Ag3 2.334(15) 1_655 ? C1 C2 1.51(2) . ? C2 C3 1.39(3) . ? C2 C7 1.40(3) . ? C3 C4 1.38(3) . ? C3 H3A 0.9300 . ? C4 C5 1.42(4) . ? C4 H4A 0.9300 . ? C5 C6 1.38(3) . ? C5 H5A 0.9300 . ? C6 C7 1.39(2) . ? C6 H6A 0.9300 . ? C7 C8 1.47(3) . ? C9 C10 1.49(3) . ? C10 C11 1.40(3) . ? C10 C15 1.43(3) . ? C11 C12 1.37(3) . ? C11 H11A 0.9300 . ? C12 C13 1.37(4) . ? C12 H12A 0.9300 . ? C13 C14 1.37(3) . ? C13 H13A 0.9300 . ? C14 C15 1.40(2) . ? C14 H14A 0.9300 . ? C15 C16 1.48(3) . ? C17 C18 1.50(3) . ? C18 C19 1.39(3) . ? C18 C23 1.42(3) . ? C19 C20 1.35(3) . ? C19 H19A 0.9300 . ? C20 C21 1.41(4) . ? C20 H20A 0.9300 . ? C21 C22 1.39(3) . ? C21 H21A 0.9300 . ? C22 C23 1.37(3) . ? C22 H22A 0.9300 . ? C23 C24 1.53(2) . ? C25 C26 1.51(2) . ? C26 C31 1.39(3) . ? C26 C27 1.41(3) . ? C27 C28 1.41(3) . ? C27 H27A 0.9300 . ? C28 C29 1.32(3) . ? C28 H28A 0.9300 . ? C29 C30 1.42(3) . ? C29 H29A 0.9300 . ? C30 C31 1.40(3) . ? C30 H30A 0.9300 . ? C31 C32 1.50(3) . ? 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 O6 Yb1 O12 107.3(5) . . ? O6 Yb1 O14 83.7(5) . . ? O12 Yb1 O14 143.3(4) . . ? O6 Yb1 O2 145.4(5) . . ? O12 Yb1 O2 82.9(5) . . ? O14 Yb1 O2 108.2(5) . . ? O6 Yb1 O10 73.7(5) . . ? O12 Yb1 O10 72.5(5) . . ? O14 Yb1 O10 77.6(4) . . ? O2 Yb1 O10 139.8(5) . . ? O6 Yb1 O15 140.7(4) . . ? O12 Yb1 O15 77.5(5) . . ? O14 Yb1 O15 72.9(4) . . ? O2 Yb1 O15 73.4(5) . . ? O10 Yb1 O15 70.7(4) . . ? O6 Yb1 O8 69.7(4) . . ? O12 Yb1 O8 75.7(4) . . ? O14 Yb1 O8 139.4(4) . . ? O2 Yb1 O8 81.5(5) . . ? O10 Yb1 O8 120.5(4) . . ? O15 Yb1 O8 145.1(4) . . ? O6 Yb1 O4 81.8(5) . . ? O12 Yb1 O4 139.5(4) . . ? O14 Yb1 O4 75.7(4) . . ? O2 Yb1 O4 70.5(5) . . ? O10 Yb1 O4 145.4(4) . . ? O15 Yb1 O4 120.5(4) . . ? O8 Yb1 O4 70.8(4) . . ? O6 Yb1 C24 98.8(5) . . ? O12 Yb1 C24 20.0(4) . . ? O14 Yb1 C24 126.1(4) . . ? O2 Yb1 C24 99.6(5) . . ? O10 Yb1 C24 52.6(4) . . ? O15 Yb1 C24 72.3(4) . . ? O8 Yb1 C24 88.9(4) . . ? O4 Yb1 C24 158.2(4) . . ? O6 Yb1 C32 100.3(5) . . ? O12 Yb1 C32 126.3(5) . . ? O14 Yb1 C32 19.8(5) . . ? O2 Yb1 C32 99.5(5) . . ? O10 Yb1 C32 72.4(5) . . ? O15 Yb1 C32 53.1(5) . . ? O8 Yb1 C32 158.0(5) . . ? O4 Yb1 C32 88.7(5) . . ? C24 Yb1 C32 112.4(5) . . ? O6 Yb1 Ag1 48.9(3) . . ? O12 Yb1 Ag1 156.0(4) . . ? O14 Yb1 Ag1 49.2(3) . . ? O2 Yb1 Ag1 114.9(3) . . ? O10 Yb1 Ag1 99.0(3) . . ? O15 Yb1 Ag1 121.7(3) . . ? O8 Yb1 Ag1 90.6(3) . . ? O4 Yb1 Ag1 46.6(3) . . ? C24 Yb1 Ag1 145.0(3) . . ? C32 Yb1 Ag1 68.9(4) . . ? O6 Yb1 Ag2 114.5(3) . . ? O12 Yb1 Ag2 49.6(3) . . ? O14 Yb1 Ag2 155.6(3) . . ? O2 Yb1 Ag2 47.6(3) . . ? O10 Yb1 Ag2 121.9(3) . . ? O15 Yb1 Ag2 98.4(3) . . ? O8 Yb1 Ag2 46.9(3) . . ? O4 Yb1 Ag2 90.3(3) . . ? C24 Yb1 Ag2 69.5(3) . . ? C32 Yb1 Ag2 144.6(4) . . ? Ag1 Yb1 Ag2 130.90(6) . . ? O5 Ag1 O13 152.5(5) . 2_656 ? O5 Ag1 O3 130.3(5) . . ? O13 Ag1 O3 75.1(4) 2_656 . ? O5 Ag1 O3 85.0(4) . 2_556 ? O13 Ag1 O3 84.8(4) 2_656 2_556 ? O3 Ag1 O3 89.9(4) . 2_556 ? O5 Ag1 Yb1 81.0(4) . . ? O13 Ag1 Yb1 118.8(4) 2_656 . ? O3 Ag1 Yb1 79.0(3) . . ? O3 Ag1 Yb1 149.5(3) 2_556 . ? O11 Ag2 O1 150.7(5) 2_665 . ? O11 Ag2 O7 76.3(5) 2_665 . ? O1 Ag2 O7 131.3(5) . . ? O11 Ag2 O7 84.4(5) 2_665 2_565 ? O1 Ag2 O7 86.3(4) . 2_565 ? O7 Ag2 O7 89.3(4) . 2_565 ? O11 Ag2 Yb1 119.4(4) 2_665 . ? O1 Ag2 Yb1 81.0(3) . . ? O7 Ag2 Yb1 78.1(3) . . ? O7 Ag2 Yb1 148.5(3) 2_565 . ? O16 Ag3 O11 131.2(5) 1_455 1_455 ? O16 Ag3 O7 153.4(5) 1_455 2_565 ? O11 Ag3 O7 75.3(5) 1_455 2_565 ? O16 Ag3 O1 85.6(5) 1_455 . ? O11 Ag3 O1 114.2(5) 1_455 . ? O7 Ag3 O1 84.2(4) 2_565 . ? O16 Ag3 Ag5 85.6(3) 1_455 . ? O11 Ag3 Ag5 60.7(4) 1_455 . ? O7 Ag3 Ag5 115.0(3) 2_565 . ? O1 Ag3 Ag5 74.5(3) . . ? O13 Ag4 O9 130.8(5) 1_455 1_455 ? O13 Ag4 O3 74.1(4) 1_455 2_556 ? O9 Ag4 O3 155.1(5) 1_455 2_556 ? O13 Ag4 O5 111.6(5) 1_455 . ? O9 Ag4 O5 87.0(5) 1_455 . ? O3 Ag4 O5 83.5(4) 2_556 . ? O13 Ag4 Ag5 60.3(3) 1_455 . ? O9 Ag4 Ag5 85.5(4) 1_455 . ? O3 Ag4 Ag5 113.1(3) 2_556 . ? O5 Ag4 Ag5 72.4(4) . . ? O8 Ag5 O15 144.4(4) . 1_455 ? O8 Ag5 O10 121.2(4) . 1_455 ? O15 Ag5 O10 70.5(4) 1_455 1_455 ? O8 Ag5 O4 71.0(4) . . ? O15 Ag5 O4 119.9(4) 1_455 . ? O10 Ag5 O4 146.1(4) 1_455 . ? O8 Ag5 Ag4 115.9(3) . . ? O15 Ag5 Ag4 98.5(3) 1_455 . ? O10 Ag5 Ag4 55.4(3) 1_455 . ? O4 Ag5 Ag4 90.7(3) . . ? O8 Ag5 Ag3 89.6(3) . . ? O15 Ag5 Ag3 54.8(3) 1_455 . ? O10 Ag5 Ag3 98.0(3) 1_455 . ? O4 Ag5 Ag3 114.3(3) . . ? Ag4 Ag5 Ag3 149.58(7) . . ? C1 O1 Ag2 104.9(11) . . ? C1 O1 Ag3 137.8(13) . . ? Ag2 O1 Ag3 88.5(5) . . ? C1 O2 Yb1 136.2(12) . . ? C8 O3 Ag1 102.3(11) . . ? C8 O3 Ag4 145.4(12) . 2_556 ? Ag1 O3 Ag4 101.9(5) . 2_556 ? C8 O3 Ag1 118.3(11) . 2_556 ? Ag1 O3 Ag1 90.1(4) . 2_556 ? Ag4 O3 Ag1 85.9(4) 2_556 2_556 ? C8 O4 Yb1 126.2(10) . . ? C8 O4 Ag5 121.6(10) . . ? Yb1 O4 Ag5 108.7(5) . . ? C9 O5 Ag1 103.7(13) . . ? C9 O5 Ag4 137.7(12) . . ? Ag1 O5 Ag4 91.1(5) . . ? C9 O6 Yb1 133.6(12) . . ? C16 O7 Ag3 148.9(13) . 2_565 ? C16 O7 Ag2 100.9(12) . . ? Ag3 O7 Ag2 100.7(5) 2_565 . ? C16 O7 Ag2 116.8(11) . 2_565 ? Ag3 O7 Ag2 84.9(4) 2_565 2_565 ? Ag2 O7 Ag2 90.7(4) . 2_565 ? C16 O8 Ag5 120.4(10) . . ? C16 O8 Yb1 127.1(10) . . ? Ag5 O8 Yb1 109.5(4) . . ? C17 O9 Ag4 102.0(13) . 1_655 ? C17 O10 Yb1 124.2(11) . . ? C17 O10 Ag5 125.8(11) . 1_655 ? Yb1 O10 Ag5 109.5(5) . 1_655 ? C24 O11 Ag2 118.7(12) . 2_665 ? C24 O11 Ag3 117.6(11) . 1_655 ? Ag2 O11 Ag3 107.7(6) 2_665 1_655 ? C24 O12 Yb1 122.7(11) . . ? C32 O13 Ag1 117.4(11) . 2_656 ? C32 O13 Ag4 117.3(13) . 1_655 ? Ag1 O13 Ag4 108.9(5) 2_656 1_655 ? C32 O14 Yb1 123.2(11) . . ? C25 O15 Ag5 126.3(11) . 1_655 ? C25 O15 Yb1 123.5(10) . . ? Ag5 O15 Yb1 109.3(5) 1_655 . ? C25 O16 Ag3 102.4(11) . 1_655 ? O1 C1 O2 121.4(16) . . ? O1 C1 C2 117.9(15) . . ? O2 C1 C2 120.4(16) . . ? C3 C2 C7 120.4(17) . . ? C3 C2 C1 116.0(18) . . ? C7 C2 C1 123.4(16) . . ? C4 C3 C2 120(2) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 121(2) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C6 C5 C4 118(2) . . ? C6 C5 H5A 121.1 . . ? C4 C5 H5A 121.1 . . ? C5 C6 C7 122(2) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C6 C7 C2 118.8(19) . . ? C6 C7 C8 117.5(17) . . ? C2 C7 C8 123.6(15) . . ? O3 C8 O4 117.8(17) . . ? O3 C8 C7 120.1(15) . . ? O4 C8 C7 122.1(14) . . ? O6 C9 O5 122.7(18) . . ? O6 C9 C10 121.3(17) . . ? O5 C9 C10 114.9(19) . . ? C11 C10 C15 118.4(18) . . ? C11 C10 C9 120.5(19) . . ? C15 C10 C9 121.0(18) . . ? C12 C11 C10 121(2) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 121(2) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C12 C13 C14 120(2) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 121.9(19) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C14 C15 C10 117.8(17) . . ? C14 C15 C16 118.8(17) . . ? C10 C15 C16 122.9(15) . . ? O7 C16 O8 121.4(18) . . ? O7 C16 C15 117.6(16) . . ? O8 C16 C15 120.9(15) . . ? O9 C17 O10 124.7(17) . . ? O9 C17 C18 117.5(19) . . ? O10 C17 C18 117.6(17) . . ? C19 C18 C23 117.2(19) . . ? C19 C18 C17 122(2) . . ? C23 C18 C17 120.4(18) . . ? C20 C19 C18 124(2) . . ? C20 C19 H19A 118.1 . . ? C18 C19 H19A 118.1 . . ? C19 C20 C21 118(2) . . ? C19 C20 H20A 121.1 . . ? C21 C20 H20A 121.1 . . ? C22 C21 C20 120.6(19) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C21 120(2) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C18 119.9(19) . . ? C22 C23 C24 119.7(18) . . ? C18 C23 C24 120.4(16) . . ? O11 C24 O12 123.5(17) . . ? O11 C24 C23 118.2(15) . . ? O12 C24 C23 118.0(16) . . ? O11 C24 Yb1 123.9(12) . . ? O12 C24 Yb1 37.4(8) . . ? C23 C24 Yb1 107.7(11) . . ? O15 C25 O16 122.9(16) . . ? O15 C25 C26 119.1(17) . . ? O16 C25 C26 117.9(16) . . ? C31 C26 C27 121.5(17) . . ? C31 C26 C25 118.4(17) . . ? C27 C26 C25 119.8(18) . . ? C26 C27 C28 118(2) . . ? C26 C27 H27A 121.2 . . ? C28 C27 H27A 121.2 . . ? C29 C28 C27 121(2) . . ? C29 C28 H28A 119.3 . . ? C27 C28 H28A 119.3 . . ? C28 C29 C30 121(2) . . ? C28 C29 H29A 119.3 . . ? C30 C29 H29A 119.3 . . ? C31 C30 C29 119(2) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? C26 C31 C30 118.6(18) . . ? C26 C31 C32 123.4(15) . . ? C30 C31 C32 118.0(17) . . ? O13 C32 O14 124(2) . . ? O13 C32 C31 119.8(18) . . ? O14 C32 C31 116.1(17) . . ? O13 C32 Yb1 123.4(12) . . ? O14 C32 Yb1 36.9(7) . . ? C31 C32 Yb1 105.1(11) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 5.944 _refine_diff_density_min -3.352 _refine_diff_density_rms 0.454 # Attachment '743495-complex_1.CIF.txt' data_aa _database_code_depnum_ccdc_archive 'CCDC 743495' #TrackingRef '743495-complex_1.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Ag5 Eu O16' _chemical_formula_weight 1347.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9028(11) _cell_length_b 14.954(2) _cell_length_c 15.182(2) _cell_angle_alpha 63.4592(17) _cell_angle_beta 81.4312(19) _cell_angle_gamma 81.2837(17) _cell_volume 1579.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2859 _cell_measurement_theta_min 2.565 _cell_measurement_theta_max 27.737 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 5.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6308 _exptl_absorpt_correction_T_max 0.6308 _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 'Bruker Apex2 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8595 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6078 _reflns_number_gt 4714 _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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6078 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Eu1 Eu 0.35555(3) 0.25131(2) 0.25159(2) 0.01550(8) Uani 1 1 d . . . Ag1 Ag 0.12553(6) 0.08966(3) 0.49158(3) 0.02978(12) Uani 1 1 d . . . Ag2 Ag 0.17520(7) 0.40995(3) 0.00756(3) 0.03120(13) Uani 1 1 d . . . Ag3 Ag -0.21533(7) 0.33114(4) 0.01772(4) 0.04199(15) Uani 1 1 d . . . Ag4 Ag -0.30890(7) 0.17086(4) 0.48669(4) 0.04071(15) Uani 1 1 d . . . Ag5 Ag -0.14562(6) 0.25177(4) 0.25233(4) 0.04038(15) Uani 1 1 d . . . O1 O 0.0989(6) 0.2568(3) 0.0346(3) 0.0361(11) Uani 1 1 d . . . O2 O 0.3228(5) 0.2148(3) 0.1212(3) 0.0253(9) Uani 1 1 d . . . O3 O 0.1446(5) -0.0151(3) 0.4030(3) 0.0273(10) Uani 1 1 d . . . O4 O 0.1203(5) 0.1448(3) 0.2950(3) 0.0203(9) Uani 1 1 d . . . O5 O -0.0316(5) 0.2412(3) 0.4643(3) 0.0381(11) Uani 1 1 d . . . O6 O 0.2174(5) 0.2884(3) 0.3798(3) 0.0241(9) Uani 1 1 d . . . O7 O 0.0841(5) 0.5166(3) 0.0955(3) 0.0274(10) Uani 1 1 d . . . O8 O 0.0863(5) 0.3562(3) 0.2031(3) 0.0203(9) Uani 1 1 d . . . O9 O 0.5575(6) 0.3374(3) 0.4415(3) 0.0332(11) Uani 1 1 d . . . O10 O 0.5726(5) 0.3061(3) 0.3105(3) 0.0211(9) Uani 1 1 d . . . O11 O 0.7127(5) 0.4398(3) 0.0983(3) 0.0311(10) Uani 1 1 d . . . O12 O 0.4431(5) 0.4013(3) 0.1236(3) 0.0241(9) Uani 1 1 d . . . O13 O 0.7337(5) 0.0629(3) 0.4052(3) 0.0297(10) Uani 1 1 d . . . O14 O 0.4559(5) 0.1025(3) 0.3811(3) 0.0232(9) Uani 1 1 d . . . O15 O 0.6396(5) 0.1977(3) 0.1956(3) 0.0193(8) Uani 1 1 d . . . O16 O 0.7251(6) 0.1662(3) 0.0648(3) 0.0335(11) Uani 1 1 d . . . C1 C 0.1962(8) 0.1927(4) 0.0955(4) 0.0227(13) Uani 1 1 d . . . C2 C 0.1630(7) 0.0845(4) 0.1342(4) 0.0215(13) Uani 1 1 d . . . C3 C 0.1633(8) 0.0480(5) 0.0650(5) 0.0324(15) Uani 1 1 d . . . H3A H 0.1804 0.0908 -0.0020 0.039 Uiso 1 1 calc R . . C4 C 0.1385(9) -0.0511(5) 0.0941(5) 0.0383(17) Uani 1 1 d . . . H4A H 0.1410 -0.0749 0.0468 0.046 Uiso 1 1 calc R . . C5 C 0.1102(9) -0.1147(5) 0.1926(5) 0.0354(16) Uani 1 1 d . . . H5A H 0.0921 -0.1813 0.2123 0.042 Uiso 1 1 calc R . . C6 C 0.1090(8) -0.0787(4) 0.2619(5) 0.0306(15) Uani 1 1 d . . . H6A H 0.0886 -0.1218 0.3286 0.037 Uiso 1 1 calc R . . C7 C 0.1372(7) 0.0198(4) 0.2352(4) 0.0254(14) Uani 1 1 d . . . C8 C 0.1345(7) 0.0509(4) 0.3162(4) 0.0217(13) Uani 1 1 d . . . C9 C 0.0608(8) 0.3072(4) 0.4036(4) 0.0224(13) Uani 1 1 d . . . C10 C -0.0160(7) 0.4147(4) 0.3631(4) 0.0230(13) Uani 1 1 d . . . C11 C -0.0965(8) 0.4488(5) 0.4320(5) 0.0348(16) Uani 1 1 d . . . H11A H -0.1103 0.4039 0.4985 0.042 Uiso 1 1 calc R . . C12 C -0.1558(10) 0.5487(5) 0.4025(5) 0.0442(19) Uani 1 1 d . . . H12A H -0.2065 0.5714 0.4492 0.053 Uiso 1 1 calc R . . C13 C -0.1397(9) 0.6150(5) 0.3036(5) 0.0414(18) Uani 1 1 d . . . H13A H -0.1787 0.6824 0.2840 0.050 Uiso 1 1 calc R . . C14 C -0.0674(9) 0.5827(4) 0.2342(5) 0.0351(16) Uani 1 1 d . . . H14A H -0.0596 0.6279 0.1677 0.042 Uiso 1 1 calc R . . C15 C -0.0050(7) 0.4820(4) 0.2626(4) 0.0244(13) Uani 1 1 d . . . C16 C 0.0598(7) 0.4501(4) 0.1822(4) 0.0213(13) Uani 1 1 d . . . C17 C 0.5412(7) 0.3652(4) 0.3532(5) 0.0242(14) Uani 1 1 d . . . C18 C 0.4911(8) 0.4745(4) 0.2887(4) 0.0242(13) Uani 1 1 d . . . C19 C 0.4338(8) 0.5401(5) 0.3307(5) 0.0337(16) Uani 1 1 d . . . H19A H 0.4255 0.5158 0.3991 0.040 Uiso 1 1 calc R . . C20 C 0.3887(9) 0.6410(5) 0.2737(5) 0.0417(18) Uani 1 1 d . . . H20A H 0.3446 0.6835 0.3032 0.050 Uiso 1 1 calc R . . C21 C 0.4109(9) 0.6774(5) 0.1714(5) 0.0427(18) Uani 1 1 d . . . H21A H 0.3851 0.7455 0.1321 0.051 Uiso 1 1 calc R . . C22 C 0.4697(8) 0.6148(5) 0.1276(5) 0.0330(16) Uani 1 1 d . . . H22A H 0.4861 0.6410 0.0590 0.040 Uiso 1 1 calc R . . C23 C 0.5059(7) 0.5111(4) 0.1853(4) 0.0208(13) Uani 1 1 d . . . C24 C 0.5592(7) 0.4449(4) 0.1330(4) 0.0198(13) Uani 1 1 d . . . C25 C 0.6686(7) 0.1392(4) 0.1515(4) 0.0224(13) Uani 1 1 d . . . C26 C 0.6320(7) 0.0314(4) 0.2147(4) 0.0235(13) Uani 1 1 d . . . C27 C 0.6233(8) -0.0306(5) 0.1708(5) 0.0324(15) Uani 1 1 d . . . H27A H 0.6316 -0.0043 0.1022 0.039 Uiso 1 1 calc R . . C28 C 0.6026(9) -0.1314(5) 0.2273(5) 0.0401(18) Uani 1 1 d . . . H28A H 0.5941 -0.1721 0.1967 0.048 Uiso 1 1 calc R . . C29 C 0.5944(9) -0.1715(5) 0.3291(5) 0.0407(18) Uani 1 1 d . . . H29A H 0.5831 -0.2395 0.3671 0.049 Uiso 1 1 calc R . . C30 C 0.6032(8) -0.1106(4) 0.3741(5) 0.0283(14) Uani 1 1 d . . . H30A H 0.6014 -0.1387 0.4425 0.034 Uiso 1 1 calc R . . C31 C 0.6147(7) -0.0073(4) 0.3191(4) 0.0219(13) Uani 1 1 d . . . C32 C 0.6028(7) 0.0586(4) 0.3707(4) 0.0204(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01206(15) 0.01361(14) 0.01813(15) -0.00440(11) -0.00282(11) -0.00011(11) Ag1 0.0318(3) 0.0216(2) 0.0282(3) -0.0056(2) -0.0041(2) 0.0041(2) Ag2 0.0372(3) 0.0211(2) 0.0297(3) -0.0046(2) -0.0042(2) -0.0064(2) Ag3 0.0435(4) 0.0259(3) 0.0502(3) -0.0126(3) 0.0086(3) -0.0102(2) Ag4 0.0421(3) 0.0277(3) 0.0505(3) -0.0141(2) -0.0184(3) 0.0064(2) Ag5 0.0179(3) 0.0352(3) 0.0717(4) -0.0257(3) -0.0083(3) -0.0008(2) O1 0.041(3) 0.021(2) 0.041(3) -0.004(2) -0.025(2) 0.000(2) O2 0.024(2) 0.028(2) 0.027(2) -0.0128(19) -0.0021(18) -0.0057(18) O3 0.028(2) 0.023(2) 0.022(2) 0.0002(18) -0.0077(18) -0.0027(18) O4 0.015(2) 0.017(2) 0.027(2) -0.0080(17) -0.0041(17) 0.0003(16) O5 0.028(3) 0.028(3) 0.045(3) -0.006(2) 0.011(2) -0.006(2) O6 0.018(2) 0.026(2) 0.025(2) -0.0093(18) -0.0015(18) 0.0024(18) O7 0.024(2) 0.021(2) 0.024(2) -0.0011(19) 0.0015(18) 0.0021(18) O8 0.017(2) 0.015(2) 0.024(2) -0.0058(17) -0.0017(17) 0.0010(16) O9 0.043(3) 0.029(2) 0.027(2) -0.011(2) -0.008(2) 0.001(2) O10 0.015(2) 0.019(2) 0.032(2) -0.0126(18) -0.0081(18) 0.0012(16) O11 0.023(2) 0.028(2) 0.038(3) -0.011(2) 0.006(2) -0.0090(19) O12 0.021(2) 0.018(2) 0.028(2) -0.0034(18) -0.0078(18) -0.0041(17) O13 0.028(2) 0.028(2) 0.030(2) -0.0070(19) -0.016(2) 0.0015(19) O14 0.017(2) 0.018(2) 0.026(2) -0.0040(17) -0.0005(17) 0.0044(17) O15 0.015(2) 0.017(2) 0.024(2) -0.0083(17) -0.0001(17) 0.0013(16) O16 0.041(3) 0.027(2) 0.024(2) -0.004(2) 0.002(2) -0.004(2) C1 0.028(4) 0.024(3) 0.015(3) -0.009(3) -0.001(3) 0.000(3) C2 0.020(3) 0.018(3) 0.023(3) -0.004(2) -0.006(3) -0.002(2) C3 0.037(4) 0.036(4) 0.023(3) -0.011(3) -0.005(3) -0.006(3) C4 0.052(5) 0.034(4) 0.039(4) -0.024(3) -0.007(3) -0.005(3) C5 0.048(5) 0.018(3) 0.042(4) -0.013(3) -0.006(3) -0.005(3) C6 0.038(4) 0.021(3) 0.031(4) -0.007(3) -0.010(3) -0.005(3) C7 0.020(3) 0.020(3) 0.035(4) -0.010(3) -0.007(3) 0.001(3) C8 0.016(3) 0.022(3) 0.022(3) -0.004(3) -0.002(2) -0.006(2) C9 0.024(4) 0.023(3) 0.018(3) -0.008(3) -0.003(3) 0.001(3) C10 0.018(3) 0.025(3) 0.027(3) -0.014(3) 0.002(3) -0.001(3) C11 0.041(4) 0.028(4) 0.029(4) -0.010(3) -0.003(3) 0.006(3) C12 0.060(5) 0.032(4) 0.039(4) -0.019(3) 0.003(4) 0.003(4) C13 0.054(5) 0.018(3) 0.050(5) -0.017(3) 0.000(4) 0.009(3) C14 0.044(4) 0.018(3) 0.034(4) -0.006(3) -0.002(3) 0.007(3) C15 0.022(3) 0.019(3) 0.027(3) -0.009(3) -0.001(3) 0.004(3) C16 0.015(3) 0.017(3) 0.028(3) -0.005(3) -0.008(3) -0.001(2) C17 0.013(3) 0.019(3) 0.036(4) -0.009(3) 0.001(3) -0.003(2) C18 0.025(3) 0.015(3) 0.034(4) -0.012(3) -0.004(3) 0.001(2) C19 0.038(4) 0.030(4) 0.032(4) -0.016(3) 0.000(3) 0.001(3) C20 0.056(5) 0.025(4) 0.053(5) -0.026(4) -0.008(4) 0.007(3) C21 0.048(5) 0.023(4) 0.054(5) -0.014(3) -0.008(4) 0.003(3) C22 0.034(4) 0.025(3) 0.033(4) -0.005(3) -0.009(3) -0.002(3) C23 0.011(3) 0.019(3) 0.032(3) -0.010(3) -0.002(2) -0.002(2) C24 0.019(3) 0.014(3) 0.017(3) 0.002(2) -0.007(2) 0.000(2) C25 0.016(3) 0.025(3) 0.024(3) -0.009(3) -0.002(3) -0.004(3) C26 0.014(3) 0.019(3) 0.034(3) -0.010(3) -0.001(3) 0.002(2) C27 0.039(4) 0.027(3) 0.036(4) -0.021(3) 0.005(3) -0.004(3) C28 0.052(5) 0.029(4) 0.045(4) -0.024(3) 0.010(4) -0.010(3) C29 0.047(5) 0.021(3) 0.048(5) -0.012(3) 0.001(4) 0.000(3) C30 0.031(4) 0.017(3) 0.030(4) -0.007(3) 0.003(3) 0.002(3) C31 0.019(3) 0.021(3) 0.024(3) -0.008(3) -0.004(3) -0.001(2) C32 0.022(3) 0.014(3) 0.017(3) 0.001(2) -0.004(2) -0.002(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 Eu1 O6 2.331(4) . ? Eu1 O2 2.334(4) . ? Eu1 O12 2.337(4) . ? Eu1 O14 2.338(4) . ? Eu1 O15 2.429(4) . ? Eu1 O10 2.439(4) . ? Eu1 O8 2.440(4) . ? Eu1 O4 2.455(4) . ? Eu1 C32 3.176(5) . ? Eu1 C24 3.179(5) . ? Eu1 Ag1 3.7295(6) . ? Eu1 Ag2 3.7522(7) . ? Ag1 O5 2.304(4) . ? Ag1 O13 2.335(4) 2_656 ? Ag1 O3 2.456(4) . ? Ag1 O3 2.544(4) 2_556 ? Ag2 O1 2.299(4) . ? Ag2 O11 2.317(4) 2_665 ? Ag2 O7 2.472(4) . ? Ag2 O7 2.567(4) 2_565 ? Ag3 O16 2.343(4) 1_455 ? Ag3 O11 2.398(4) 1_455 ? Ag3 O7 2.429(4) 2_565 ? Ag3 O1 2.563(4) . ? Ag3 Ag5 3.3177(10) . ? Ag4 O9 2.384(4) 1_455 ? Ag4 O13 2.397(4) 1_455 ? Ag4 O3 2.482(4) 2_556 ? Ag4 O5 2.486(4) . ? Ag4 Ag5 3.3235(9) . ? Ag5 O15 2.397(4) 1_455 ? Ag5 O8 2.403(4) . ? Ag5 O4 2.420(4) . ? Ag5 O10 2.430(4) 1_455 ? O1 C1 1.249(7) . ? O2 C1 1.262(7) . ? O3 C8 1.251(6) . ? O3 Ag4 2.482(4) 2_556 ? O3 Ag1 2.544(4) 2_556 ? O4 C8 1.282(6) . ? O5 C9 1.250(7) . ? O6 C9 1.262(7) . ? O7 C16 1.254(6) . ? O7 Ag3 2.429(4) 2_565 ? O7 Ag2 2.567(4) 2_565 ? O8 C16 1.284(6) . ? O9 C17 1.234(7) . ? O9 Ag4 2.384(4) 1_655 ? O10 C17 1.289(7) . ? O10 Ag5 2.430(4) 1_655 ? O11 C24 1.254(7) . ? O11 Ag2 2.317(4) 2_665 ? O11 Ag3 2.398(4) 1_655 ? O12 C24 1.262(6) . ? O13 C32 1.249(6) . ? O13 Ag1 2.335(4) 2_656 ? O13 Ag4 2.397(4) 1_655 ? O14 C32 1.269(7) . ? O15 C25 1.298(7) . ? O15 Ag5 2.397(4) 1_655 ? O16 C25 1.224(6) . ? O16 Ag3 2.343(4) 1_655 ? C1 C2 1.505(8) . ? C2 C3 1.382(8) . ? C2 C7 1.403(8) . ? C3 C4 1.382(9) . ? C3 H3A 0.9300 . ? C4 C5 1.373(9) . ? C4 H4A 0.9300 . ? C5 C6 1.377(8) . ? C5 H5A 0.9300 . ? C6 C7 1.388(8) . ? C6 H6A 0.9300 . ? C7 C8 1.493(8) . ? C9 C10 1.503(8) . ? C10 C11 1.393(8) . ? C10 C15 1.401(8) . ? C11 C12 1.381(9) . ? C11 H11A 0.9300 . ? C12 C13 1.380(9) . ? C12 H12A 0.9300 . ? C13 C14 1.364(9) . ? C13 H13A 0.9300 . ? C14 C15 1.398(8) . ? C14 H14A 0.9300 . ? C15 C16 1.497(8) . ? C17 C18 1.509(8) . ? C18 C19 1.383(8) . ? C18 C23 1.404(8) . ? C19 C20 1.383(9) . ? C19 H19A 0.9300 . ? C20 C21 1.390(9) . ? C20 H20A 0.9300 . ? C21 C22 1.366(9) . ? C21 H21A 0.9300 . ? C22 C23 1.407(8) . ? C22 H22A 0.9300 . ? C23 C24 1.506(8) . ? C25 C26 1.510(8) . ? C26 C27 1.375(8) . ? C26 C31 1.416(8) . ? C27 C28 1.383(8) . ? C27 H27A 0.9300 . ? C28 C29 1.380(9) . ? C28 H28A 0.9300 . ? C29 C30 1.373(9) . ? C29 H29A 0.9300 . ? C30 C31 1.400(7) . ? C30 H30A 0.9300 . ? C31 C32 1.494(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O2 146.24(13) . . ? O6 Eu1 O12 107.32(14) . . ? O2 Eu1 O12 83.05(13) . . ? O6 Eu1 O14 83.43(13) . . ? O2 Eu1 O14 107.95(14) . . ? O12 Eu1 O14 142.80(14) . . ? O6 Eu1 O15 140.13(13) . . ? O2 Eu1 O15 72.85(13) . . ? O12 Eu1 O15 77.87(13) . . ? O14 Eu1 O15 72.18(13) . . ? O6 Eu1 O10 73.48(13) . . ? O2 Eu1 O10 139.36(13) . . ? O12 Eu1 O10 72.27(13) . . ? O14 Eu1 O10 77.31(13) . . ? O15 Eu1 O10 70.74(12) . . ? O6 Eu1 O8 69.35(13) . . ? O2 Eu1 O8 82.81(13) . . ? O12 Eu1 O8 76.20(13) . . ? O14 Eu1 O8 139.23(12) . . ? O15 Eu1 O8 146.21(12) . . ? O10 Eu1 O8 120.17(12) . . ? O6 Eu1 O4 83.31(13) . . ? O2 Eu1 O4 69.17(13) . . ? O12 Eu1 O4 138.38(12) . . ? O14 Eu1 O4 77.12(13) . . ? O15 Eu1 O4 119.64(12) . . ? O10 Eu1 O4 147.08(13) . . ? O8 Eu1 O4 70.25(12) . . ? O6 Eu1 C32 100.55(14) . . ? O2 Eu1 C32 98.52(14) . . ? O12 Eu1 C32 125.70(14) . . ? O14 Eu1 C32 20.15(13) . . ? O15 Eu1 C32 52.03(13) . . ? O10 Eu1 C32 72.48(13) . . ? O8 Eu1 C32 158.10(13) . . ? O4 Eu1 C32 89.67(13) . . ? O6 Eu1 C24 99.08(14) . . ? O2 Eu1 C24 99.36(14) . . ? O12 Eu1 C24 19.86(13) . . ? O14 Eu1 C24 125.43(14) . . ? O15 Eu1 C24 72.25(13) . . ? O10 Eu1 C24 52.43(13) . . ? O8 Eu1 C24 89.47(13) . . ? O4 Eu1 C24 157.43(13) . . ? C32 Eu1 C24 111.70(14) . . ? O6 Eu1 Ag1 49.35(9) . . ? O2 Eu1 Ag1 113.94(9) . . ? O12 Eu1 Ag1 156.28(10) . . ? O14 Eu1 Ag1 50.26(9) . . ? O15 Eu1 Ag1 121.85(8) . . ? O10 Eu1 Ag1 100.38(9) . . ? O8 Eu1 Ag1 89.16(8) . . ? O4 Eu1 Ag1 46.88(9) . . ? C32 Eu1 Ag1 70.22(10) . . ? C24 Eu1 Ag1 146.21(10) . . ? O6 Eu1 Ag2 113.72(9) . . ? O2 Eu1 Ag2 48.50(10) . . ? O12 Eu1 Ag2 50.66(9) . . ? O14 Eu1 Ag2 156.01(10) . . ? O15 Eu1 Ag2 100.14(9) . . ? O10 Eu1 Ag2 122.50(9) . . ? O8 Eu1 Ag2 46.25(9) . . ? O4 Eu1 Ag2 87.95(9) . . ? C32 Eu1 Ag2 145.09(10) . . ? C24 Eu1 Ag2 70.45(10) . . ? Ag1 Eu1 Ag2 128.333(15) . . ? O5 Ag1 O13 151.70(15) . 2_656 ? O5 Ag1 O3 130.38(15) . . ? O13 Ag1 O3 75.82(13) 2_656 . ? O5 Ag1 O3 84.12(14) . 2_556 ? O13 Ag1 O3 84.39(13) 2_656 2_556 ? O3 Ag1 O3 92.12(13) . 2_556 ? O5 Ag1 Eu1 81.14(10) . . ? O13 Ag1 Eu1 118.80(10) 2_656 . ? O3 Ag1 Eu1 79.55(9) . . ? O3 Ag1 Eu1 151.77(9) 2_556 . ? O1 Ag2 O11 149.67(15) . 2_665 ? O1 Ag2 O7 132.05(14) . . ? O11 Ag2 O7 76.75(14) 2_665 . ? O1 Ag2 O7 85.08(13) . 2_565 ? O11 Ag2 O7 84.77(13) 2_665 2_565 ? O7 Ag2 O7 91.58(13) . 2_565 ? O1 Ag2 Eu1 81.04(10) . . ? O11 Ag2 Eu1 119.53(10) 2_665 . ? O7 Ag2 Eu1 78.49(9) . . ? O7 Ag2 Eu1 149.91(9) 2_565 . ? O16 Ag3 O11 131.76(14) 1_455 1_455 ? O16 Ag3 O7 152.10(14) 1_455 2_565 ? O11 Ag3 O7 76.11(13) 1_455 2_565 ? O16 Ag3 O1 85.06(14) 1_455 . ? O11 Ag3 O1 110.88(14) 1_455 . ? O7 Ag3 O1 82.59(13) 2_565 . ? O16 Ag3 Ag5 85.58(10) 1_455 . ? O11 Ag3 Ag5 59.05(10) 1_455 . ? O7 Ag3 Ag5 114.20(10) 2_565 . ? O1 Ag3 Ag5 72.95(10) . . ? O9 Ag4 O13 132.57(13) 1_455 1_455 ? O9 Ag4 O3 153.13(14) 1_455 2_556 ? O13 Ag4 O3 74.25(13) 1_455 2_556 ? O9 Ag4 O5 86.84(14) 1_455 . ? O13 Ag4 O5 107.38(15) 1_455 . ? O3 Ag4 O5 81.79(13) 2_556 . ? O9 Ag4 Ag5 86.51(10) 1_455 . ? O13 Ag4 Ag5 58.94(10) 1_455 . ? O3 Ag4 Ag5 111.89(10) 2_556 . ? O5 Ag4 Ag5 69.95(11) . . ? O15 Ag5 O8 145.24(13) 1_455 . ? O15 Ag5 O4 118.04(12) 1_455 . ? O8 Ag5 O4 71.45(12) . . ? O15 Ag5 O10 71.41(12) 1_455 1_455 ? O8 Ag5 O10 120.22(12) . 1_455 ? O4 Ag5 O10 147.23(13) . 1_455 ? O15 Ag5 Ag3 54.61(9) 1_455 . ? O8 Ag5 Ag3 90.64(9) . . ? O4 Ag5 Ag3 112.93(9) . . ? O10 Ag5 Ag3 98.11(9) 1_455 . ? O15 Ag5 Ag4 97.07(9) 1_455 . ? O8 Ag5 Ag4 116.41(9) . . ? O4 Ag5 Ag4 93.21(9) . . ? O10 Ag5 Ag4 54.02(9) 1_455 . ? Ag3 Ag5 Ag4 147.73(2) . . ? C1 O1 Ag2 105.6(4) . . ? C1 O1 Ag3 142.0(4) . . ? Ag2 O1 Ag3 89.42(14) . . ? C1 O2 Eu1 132.9(4) . . ? C8 O3 Ag1 100.7(4) . . ? C8 O3 Ag4 145.3(4) . 2_556 ? Ag1 O3 Ag4 101.73(14) . 2_556 ? C8 O3 Ag1 119.8(4) . 2_556 ? Ag1 O3 Ag1 87.88(13) . 2_556 ? Ag4 O3 Ag1 87.13(12) 2_556 2_556 ? C8 O4 Ag5 123.0(3) . . ? C8 O4 Eu1 126.8(3) . . ? Ag5 O4 Eu1 108.58(14) . . ? C9 O5 Ag1 105.9(4) . . ? C9 O5 Ag4 142.8(4) . . ? Ag1 O5 Ag4 92.54(15) . . ? C9 O6 Eu1 132.2(4) . . ? C16 O7 Ag3 148.4(4) . 2_565 ? C16 O7 Ag2 100.0(4) . . ? Ag3 O7 Ag2 100.72(14) 2_565 . ? C16 O7 Ag2 117.7(3) . 2_565 ? Ag3 O7 Ag2 86.53(12) 2_565 2_565 ? Ag2 O7 Ag2 88.42(13) . 2_565 ? C16 O8 Ag5 121.9(3) . . ? C16 O8 Eu1 125.5(3) . . ? Ag5 O8 Eu1 109.61(14) . . ? C17 O9 Ag4 101.4(4) . 1_655 ? C17 O10 Ag5 126.2(3) . 1_655 ? C17 O10 Eu1 125.0(3) . . ? Ag5 O10 Eu1 108.21(14) 1_655 . ? C24 O11 Ag2 117.0(4) . 2_665 ? C24 O11 Ag3 115.8(4) . 1_655 ? Ag2 O11 Ag3 106.35(16) 2_665 1_655 ? C24 O12 Eu1 121.1(3) . . ? C32 O13 Ag1 116.8(4) . 2_656 ? C32 O13 Ag4 114.3(4) . 1_655 ? Ag1 O13 Ag4 108.05(15) 2_656 1_655 ? C32 O14 Eu1 120.5(3) . . ? C25 O15 Ag5 125.6(3) . 1_655 ? C25 O15 Eu1 124.3(3) . . ? Ag5 O15 Eu1 109.64(14) 1_655 . ? C25 O16 Ag3 102.6(4) . 1_655 ? O1 C1 O2 123.0(5) . . ? O1 C1 C2 116.9(5) . . ? O2 C1 C2 120.0(5) . . ? C3 C2 C7 119.5(5) . . ? C3 C2 C1 117.0(5) . . ? C7 C2 C1 123.5(5) . . ? C4 C3 C2 120.8(6) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C5 C4 C3 120.3(6) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.2(6) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C7 121.9(6) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C6 C7 C2 118.3(6) . . ? C6 C7 C8 117.6(5) . . ? C2 C7 C8 124.1(5) . . ? O3 C8 O4 121.7(5) . . ? O3 C8 C7 119.2(5) . . ? O4 C8 C7 119.1(5) . . ? O5 C9 O6 123.0(5) . . ? O5 C9 C10 117.9(5) . . ? O6 C9 C10 118.9(5) . . ? C11 C10 C15 119.0(6) . . ? C11 C10 C9 116.5(5) . . ? C15 C10 C9 124.4(5) . . ? C12 C11 C10 120.6(6) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C13 C12 C11 119.8(6) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 120.8(6) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C10 119.4(6) . . ? C14 C15 C16 117.5(5) . . ? C10 C15 C16 123.0(5) . . ? O7 C16 O8 121.8(5) . . ? O7 C16 C15 118.6(5) . . ? O8 C16 C15 119.6(5) . . ? O9 C17 O10 123.4(5) . . ? O9 C17 C18 119.7(5) . . ? O10 C17 C18 116.8(5) . . ? C19 C18 C23 119.3(5) . . ? C19 C18 C17 120.3(6) . . ? C23 C18 C17 120.4(5) . . ? C18 C19 C20 121.8(6) . . ? C18 C19 H19A 119.1 . . ? C20 C19 H19A 119.1 . . ? C19 C20 C21 118.4(6) . . ? C19 C20 H20A 120.8 . . ? C21 C20 H20A 120.8 . . ? C22 C21 C20 121.1(6) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C23 120.6(6) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C18 C23 C22 118.5(5) . . ? C18 C23 C24 123.3(5) . . ? C22 C23 C24 118.2(5) . . ? O11 C24 O12 124.4(6) . . ? O11 C24 C23 118.5(5) . . ? O12 C24 C23 117.0(5) . . ? O11 C24 Eu1 122.2(4) . . ? O12 C24 Eu1 39.0(2) . . ? C23 C24 Eu1 106.4(3) . . ? O16 C25 O15 124.0(5) . . ? O16 C25 C26 120.2(5) . . ? O15 C25 C26 115.8(5) . . ? C27 C26 C31 119.9(5) . . ? C27 C26 C25 119.8(5) . . ? C31 C26 C25 120.2(5) . . ? C26 C27 C28 120.9(6) . . ? C26 C27 H27A 119.6 . . ? C28 C27 H27A 119.6 . . ? C29 C28 C27 119.9(6) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C30 C29 C28 119.9(6) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 121.5(6) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C30 C31 C26 117.7(5) . . ? C30 C31 C32 120.1(5) . . ? C26 C31 C32 122.3(5) . . ? O13 C32 O14 124.2(6) . . ? O13 C32 C31 118.7(5) . . ? O14 C32 C31 116.9(5) . . ? O13 C32 Eu1 122.9(4) . . ? O14 C32 Eu1 39.4(2) . . ? C31 C32 Eu1 105.7(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.907 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.156 # Attachment '743496-complex_3.CIF.txt' data_h07327 _database_code_depnum_ccdc_archive 'CCDC 743496' #TrackingRef '743496-complex_3.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Ag5 Er O16' _chemical_formula_weight 1363.06 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' Ag Ag -0.8971 1.1015 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8516(16) _cell_length_b 14.938(3) _cell_length_c 15.208(3) _cell_angle_alpha 63.69(3) _cell_angle_beta 81.53(3) _cell_angle_gamma 81.41(3) _cell_volume 1574.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10667 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 54.98 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1278 _exptl_absorpt_coefficient_mu 5.767 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5695 _exptl_absorpt_correction_T_max 0.7733 _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12942 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0834 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5829 _reflns_number_gt 4336 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1084P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5829 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.010 _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 Er1 Er 0.35371(6) 0.25125(4) 0.25139(3) 0.02264(18) Uani 1 1 d . . . Ag1 Ag 0.12902(13) 0.09026(7) 0.49223(6) 0.0353(3) Uani 1 1 d . . . Ag2 Ag 0.17915(13) 0.40899(7) 0.00682(7) 0.0366(3) Uani 1 1 d . . . Ag3 Ag -0.21374(15) 0.33131(8) 0.01806(8) 0.0475(3) Uani 1 1 d . . . Ag4 Ag -0.30624(15) 0.17051(8) 0.48638(8) 0.0466(3) Uani 1 1 d . . . Ag5 Ag -0.14703(12) 0.25167(8) 0.25238(8) 0.0436(3) Uani 1 1 d . . . O1 O 0.1021(12) 0.2551(7) 0.0335(6) 0.041(2) Uani 1 1 d . . . O2 O 0.3192(10) 0.2144(6) 0.1244(5) 0.0287(18) Uani 1 1 d . . . O3 O 0.1430(11) -0.0133(7) 0.4035(5) 0.035(2) Uani 1 1 d . . . O4 O 0.1200(10) 0.1453(6) 0.2962(5) 0.0274(17) Uani 1 1 d . . . O5 O -0.0281(12) 0.2420(7) 0.4679(6) 0.043(2) Uani 1 1 d . . . O6 O 0.2170(10) 0.2874(6) 0.3768(5) 0.0308(18) Uani 1 1 d . . . O7 O 0.0843(11) 0.5147(6) 0.0941(5) 0.0335(19) Uani 1 1 d . . . O8 O 0.0860(10) 0.3561(6) 0.2019(5) 0.0250(17) Uani 1 1 d . . . O9 O 0.5572(13) 0.3354(7) 0.4410(6) 0.042(2) Uani 1 1 d . . . O10 O 0.5715(9) 0.3047(6) 0.3098(5) 0.0249(16) Uani 1 1 d . . . O11 O 0.7090(10) 0.4408(6) 0.0974(6) 0.035(2) Uani 1 1 d . . . O12 O 0.4399(10) 0.3976(6) 0.1268(6) 0.0313(18) Uani 1 1 d . . . O13 O 0.7297(11) 0.0624(7) 0.4065(6) 0.037(2) Uani 1 1 d . . . O14 O 0.4519(10) 0.1050(6) 0.3773(6) 0.0308(18) Uani 1 1 d . . . O15 O 0.6359(9) 0.1999(6) 0.1950(5) 0.0226(16) Uani 1 1 d . . . O16 O 0.7205(12) 0.1686(7) 0.0647(6) 0.041(2) Uani 1 1 d . . . C1 C 0.1945(16) 0.1926(9) 0.0960(8) 0.030(3) Uani 1 1 d . . . C2 C 0.1620(15) 0.0843(9) 0.1365(7) 0.029(3) Uani 1 1 d . . . C3 C 0.1587(17) 0.0457(10) 0.0683(9) 0.037(3) Uani 1 1 d . . . H3A H 0.1749 0.0881 0.0015 0.044 Uiso 1 1 calc R . . C4 C 0.1325(19) -0.0520(10) 0.0960(9) 0.039(3) Uani 1 1 d . . . H4A H 0.1332 -0.0754 0.0486 0.047 Uiso 1 1 calc R . . C5 C 0.105(2) -0.1151(11) 0.1940(10) 0.046(4) Uani 1 1 d . . . H5A H 0.0872 -0.1817 0.2135 0.055 Uiso 1 1 calc R . . C6 C 0.1042(18) -0.0792(10) 0.2638(9) 0.042(3) Uani 1 1 d . . . H6A H 0.0827 -0.1214 0.3303 0.050 Uiso 1 1 calc R . . C7 C 0.1349(16) 0.0186(8) 0.2354(8) 0.029(3) Uani 1 1 d . . . C8 C 0.1338(15) 0.0518(9) 0.3161(8) 0.029(3) Uani 1 1 d . . . C9 C 0.0612(14) 0.3072(9) 0.4037(7) 0.024(2) Uani 1 1 d . . . C10 C -0.0136(15) 0.4144(9) 0.3617(8) 0.030(3) Uani 1 1 d . . . C11 C -0.0972(17) 0.4487(11) 0.4316(9) 0.039(3) Uani 1 1 d . . . H11A H -0.1146 0.4039 0.4976 0.047 Uiso 1 1 calc R . . C12 C -0.153(2) 0.5505(11) 0.4008(9) 0.046(4) Uani 1 1 d . . . H12A H -0.2022 0.5736 0.4474 0.055 Uiso 1 1 calc R . . C13 C -0.138(2) 0.6167(11) 0.3036(11) 0.051(4) Uani 1 1 d . . . H13A H -0.1753 0.6843 0.2844 0.062 Uiso 1 1 calc R . . C14 C -0.0650(19) 0.5815(10) 0.2318(9) 0.041(3) Uani 1 1 d . . . H14A H -0.0575 0.6260 0.1653 0.049 Uiso 1 1 calc R . . C15 C -0.0047(14) 0.4811(9) 0.2607(8) 0.026(2) Uani 1 1 d . . . C16 C 0.0599(15) 0.4483(9) 0.1818(8) 0.030(3) Uani 1 1 d . . . C17 C 0.5426(15) 0.3638(9) 0.3554(9) 0.033(3) Uani 1 1 d . . . C18 C 0.4869(16) 0.4717(9) 0.2897(8) 0.030(3) Uani 1 1 d . . . C19 C 0.4277(18) 0.5376(11) 0.3333(12) 0.049(4) Uani 1 1 d . . . H19A H 0.4152 0.5128 0.4016 0.059 Uiso 1 1 calc R . . C20 C 0.388(2) 0.6386(10) 0.2761(11) 0.047(3) Uani 1 1 d . . . H20A H 0.3479 0.6809 0.3064 0.057 Uiso 1 1 calc R . . C21 C 0.4071(18) 0.6786(10) 0.1726(10) 0.044(3) Uani 1 1 d . . . H21A H 0.3800 0.7466 0.1341 0.053 Uiso 1 1 calc R . . C22 C 0.4681(16) 0.6131(9) 0.1290(10) 0.036(3) Uani 1 1 d . . . H22A H 0.4859 0.6385 0.0608 0.044 Uiso 1 1 calc R . . C23 C 0.5027(15) 0.5104(9) 0.1867(9) 0.031(3) Uani 1 1 d . . . C24 C 0.5549(16) 0.4440(8) 0.1350(8) 0.030(3) Uani 1 1 d . . . C25 C 0.6625(14) 0.1406(8) 0.1527(8) 0.027(2) Uani 1 1 d . . . C26 C 0.6278(15) 0.0326(9) 0.2118(8) 0.029(3) Uani 1 1 d . . . C27 C 0.6231(18) -0.0306(10) 0.1694(9) 0.038(3) Uani 1 1 d . . . H27A H 0.6342 -0.0045 0.1010 0.045 Uiso 1 1 calc R . . C28 C 0.603(2) -0.1304(11) 0.2227(11) 0.049(4) Uani 1 1 d . . . H28A H 0.5943 -0.1707 0.1916 0.059 Uiso 1 1 calc R . . C29 C 0.5948(17) -0.1708(10) 0.3263(11) 0.046(3) Uani 1 1 d . . . H29A H 0.5857 -0.2391 0.3641 0.055 Uiso 1 1 calc R . . C30 C 0.6006(16) -0.1098(9) 0.3718(9) 0.036(3) Uani 1 1 d . . . H30A H 0.5973 -0.1373 0.4401 0.043 Uiso 1 1 calc R . . C31 C 0.6113(15) -0.0065(9) 0.3162(9) 0.031(3) Uani 1 1 d . . . C32 C 0.6005(14) 0.0594(9) 0.3711(8) 0.028(3) 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 Er1 0.0188(3) 0.0213(3) 0.0241(3) -0.0060(2) -0.0029(2) -0.00247(19) Ag1 0.0366(6) 0.0294(5) 0.0319(5) -0.0073(4) -0.0035(4) 0.0019(4) Ag2 0.0411(6) 0.0290(5) 0.0337(5) -0.0066(4) -0.0025(4) -0.0097(4) Ag3 0.0480(7) 0.0335(6) 0.0537(6) -0.0138(5) 0.0090(5) -0.0118(5) Ag4 0.0473(7) 0.0357(6) 0.0551(6) -0.0162(5) -0.0183(5) 0.0039(5) Ag5 0.0247(5) 0.0393(6) 0.0692(7) -0.0242(5) -0.0084(5) -0.0029(4) O1 0.044(6) 0.036(5) 0.040(5) -0.011(4) -0.019(4) -0.001(4) O2 0.026(4) 0.039(5) 0.025(4) -0.015(4) -0.008(3) -0.006(3) O3 0.034(5) 0.036(5) 0.027(4) -0.005(4) -0.002(4) -0.006(4) O4 0.033(5) 0.023(4) 0.021(4) -0.005(3) 0.003(3) -0.006(3) O5 0.041(5) 0.032(5) 0.045(5) -0.007(4) 0.000(4) -0.001(4) O6 0.025(4) 0.036(5) 0.025(4) -0.006(3) -0.008(3) -0.002(3) O7 0.036(5) 0.029(5) 0.024(4) 0.000(3) -0.002(4) -0.005(4) O8 0.022(4) 0.026(4) 0.024(4) -0.008(3) -0.008(3) 0.000(3) O9 0.053(6) 0.045(6) 0.034(5) -0.018(4) -0.021(4) -0.002(4) O10 0.015(4) 0.027(4) 0.028(4) -0.006(3) -0.005(3) 0.000(3) O11 0.019(4) 0.037(5) 0.045(5) -0.015(4) 0.012(4) -0.014(3) O12 0.027(4) 0.021(4) 0.037(4) -0.002(3) -0.007(4) -0.005(3) O13 0.034(5) 0.035(5) 0.039(4) -0.010(4) -0.020(4) 0.001(4) O14 0.017(4) 0.030(5) 0.040(4) -0.011(4) 0.004(3) -0.002(3) O15 0.013(4) 0.027(4) 0.033(4) -0.018(3) -0.002(3) -0.003(3) O16 0.045(5) 0.039(5) 0.038(5) -0.020(4) 0.006(4) -0.001(4) C1 0.035(7) 0.023(6) 0.026(6) -0.006(5) 0.002(5) -0.005(5) C2 0.032(7) 0.033(7) 0.019(5) -0.008(5) -0.002(5) -0.009(5) C3 0.037(7) 0.040(8) 0.037(7) -0.020(6) 0.000(6) -0.006(6) C4 0.061(9) 0.030(7) 0.031(6) -0.016(5) 0.001(6) -0.012(6) C5 0.057(9) 0.034(8) 0.051(8) -0.023(6) 0.012(7) -0.017(6) C6 0.044(8) 0.043(8) 0.039(7) -0.012(6) -0.018(6) -0.013(6) C7 0.044(7) 0.011(5) 0.028(6) -0.002(4) -0.019(5) 0.001(5) C8 0.025(6) 0.031(7) 0.024(5) -0.001(5) -0.010(5) -0.009(5) C9 0.016(5) 0.033(6) 0.020(5) -0.009(5) -0.001(4) -0.002(4) C10 0.031(6) 0.027(6) 0.030(6) -0.014(5) 0.006(5) 0.000(5) C11 0.041(8) 0.050(9) 0.024(6) -0.015(6) 0.002(6) -0.005(6) C12 0.058(9) 0.051(9) 0.032(7) -0.027(6) 0.004(6) 0.003(7) C13 0.063(10) 0.030(8) 0.055(8) -0.020(7) 0.005(8) 0.007(7) C14 0.054(9) 0.027(7) 0.032(6) -0.005(5) -0.003(6) 0.003(6) C15 0.013(5) 0.035(7) 0.028(5) -0.016(5) 0.004(4) -0.002(4) C16 0.025(6) 0.026(7) 0.029(6) -0.001(5) -0.003(5) -0.002(5) C17 0.026(6) 0.025(6) 0.051(8) -0.021(6) 0.003(6) -0.006(5) C18 0.034(7) 0.028(6) 0.032(6) -0.015(5) 0.001(5) -0.014(5) C19 0.039(8) 0.042(9) 0.066(9) -0.022(7) 0.000(7) -0.005(6) C20 0.052(9) 0.030(7) 0.065(9) -0.029(7) -0.002(7) 0.003(6) C21 0.046(8) 0.025(7) 0.060(8) -0.015(6) -0.017(7) -0.002(6) C22 0.031(7) 0.026(7) 0.048(7) -0.012(6) -0.012(6) 0.002(5) C23 0.020(6) 0.026(6) 0.040(6) -0.012(5) 0.008(5) -0.001(4) C24 0.036(7) 0.014(5) 0.028(6) 0.002(4) 0.005(5) -0.008(5) C25 0.019(6) 0.021(6) 0.032(6) -0.006(5) -0.003(5) 0.007(4) C26 0.023(6) 0.039(7) 0.024(5) -0.011(5) -0.006(5) -0.003(5) C27 0.049(8) 0.035(7) 0.032(6) -0.017(6) -0.004(6) -0.005(6) C28 0.063(10) 0.031(8) 0.059(9) -0.025(7) 0.000(8) -0.004(7) C29 0.035(8) 0.029(7) 0.064(9) -0.011(6) -0.002(7) -0.007(6) C30 0.032(7) 0.033(7) 0.040(7) -0.014(6) 0.002(6) -0.005(5) C31 0.021(6) 0.031(7) 0.042(7) -0.018(5) 0.001(5) -0.006(5) C32 0.021(6) 0.029(6) 0.022(5) -0.001(5) -0.005(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O6 2.284(8) . ? Er1 O12 2.285(7) . ? Er1 O2 2.290(7) . ? Er1 O14 2.293(8) . ? Er1 O15 2.398(7) . ? Er1 O10 2.416(8) . ? Er1 O8 2.424(7) . ? Er1 O4 2.424(8) . ? Ag1 O5 2.314(9) . ? Ag1 O13 2.332(8) 2_656 ? Ag1 O3 2.445(9) . ? Ag1 O3 2.553(8) 2_556 ? Ag2 O1 2.309(9) . ? Ag2 O11 2.311(8) 2_665 ? Ag2 O7 2.454(9) . ? Ag2 O7 2.572(8) 2_565 ? Ag3 O16 2.328(9) 1_455 ? Ag3 O11 2.395(9) 1_455 ? Ag3 O7 2.438(8) 2_565 ? Ag3 O1 2.567(9) . ? Ag3 Ag5 3.3157(19) . ? Ag4 O9 2.370(10) 1_455 ? Ag4 O13 2.380(9) 1_455 ? Ag4 O3 2.492(9) 2_556 ? Ag4 O5 2.497(10) . ? Ag4 Ag5 3.319(2) . ? Ag5 O15 2.386(7) 1_455 ? Ag5 O8 2.397(8) . ? Ag5 O10 2.407(7) 1_455 ? Ag5 O4 2.417(8) . ? O1 C1 1.230(14) . ? O2 C1 1.265(14) . ? O3 C8 1.257(13) . ? O3 Ag4 2.492(9) 2_556 ? O3 Ag1 2.553(8) 2_556 ? O4 C8 1.282(14) . ? O5 C9 1.246(13) . ? O6 C9 1.267(13) . ? O7 C16 1.269(13) . ? O7 Ag3 2.438(8) 2_565 ? O7 Ag2 2.572(8) 2_565 ? O8 C16 1.262(14) . ? O9 C17 1.195(14) . ? O9 Ag4 2.370(10) 1_655 ? O10 C17 1.322(14) . ? O10 Ag5 2.407(7) 1_655 ? O11 C24 1.263(14) . ? O11 Ag2 2.311(8) 2_665 ? O11 Ag3 2.395(9) 1_655 ? O12 C24 1.267(14) . ? O13 C32 1.232(14) . ? O13 Ag1 2.332(8) 2_656 ? O13 Ag4 2.380(9) 1_655 ? O14 C32 1.274(13) . ? O15 C25 1.285(14) . ? O15 Ag5 2.386(7) 1_655 ? O16 C25 1.247(13) . ? O16 Ag3 2.328(9) 1_655 ? C1 C2 1.501(16) . ? C2 C7 1.389(14) . ? C2 C3 1.397(17) . ? C3 C4 1.367(18) . ? C3 H3A 0.9300 . ? C4 C5 1.370(17) . ? C4 H4A 0.9300 . ? C5 C6 1.385(18) . ? C5 H5A 0.9300 . ? C6 C7 1.376(17) . ? C6 H6A 0.9300 . ? C7 C8 1.513(16) . ? C9 C10 1.496(16) . ? C10 C11 1.414(16) . ? C10 C15 1.411(15) . ? C11 C12 1.40(2) . ? C11 H11A 0.9300 . ? C12 C13 1.365(19) . ? C12 H12A 0.9300 . ? C13 C14 1.427(18) . ? C13 H13A 0.9300 . ? C14 C15 1.390(17) . ? C14 H14A 0.9300 . ? C15 C16 1.484(16) . ? C17 C18 1.509(17) . ? C18 C23 1.402(16) . ? C18 C19 1.406(18) . ? C19 C20 1.38(2) . ? C19 H19A 0.9300 . ? C20 C21 1.408(19) . ? C20 H20A 0.9300 . ? C21 C22 1.402(19) . ? C21 H21A 0.9300 . ? C22 C23 1.396(16) . ? C22 H22A 0.9300 . ? C23 C24 1.499(17) . ? C25 C26 1.503(16) . ? C26 C27 1.366(17) . ? C26 C31 1.420(15) . ? C27 C28 1.367(18) . ? C27 H27A 0.9300 . ? C28 C29 1.410(19) . ? C28 H28A 0.9300 . ? C29 C30 1.376(19) . ? C29 H29A 0.9300 . ? C30 C31 1.401(17) . ? C30 H30A 0.9300 . ? C31 C32 1.534(17) . ? 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 O6 Er1 O12 107.5(3) . . ? O6 Er1 O2 145.7(3) . . ? O12 Er1 O2 83.4(3) . . ? O6 Er1 O14 83.6(3) . . ? O12 Er1 O14 143.0(3) . . ? O2 Er1 O14 107.4(3) . . ? O6 Er1 O15 140.4(3) . . ? O12 Er1 O15 77.3(3) . . ? O2 Er1 O15 73.1(3) . . ? O14 Er1 O15 72.7(3) . . ? O6 Er1 O10 73.9(3) . . ? O12 Er1 O10 72.5(3) . . ? O2 Er1 O10 139.6(3) . . ? O14 Er1 O10 77.4(3) . . ? O15 Er1 O10 70.3(2) . . ? O6 Er1 O8 69.7(3) . . ? O12 Er1 O8 75.7(3) . . ? O2 Er1 O8 82.3(3) . . ? O14 Er1 O8 139.7(2) . . ? O15 Er1 O8 145.3(2) . . ? O10 Er1 O8 120.6(3) . . ? O6 Er1 O4 82.5(3) . . ? O12 Er1 O4 139.0(3) . . ? O2 Er1 O4 69.5(3) . . ? O14 Er1 O4 76.3(3) . . ? O15 Er1 O4 120.2(3) . . ? O10 Er1 O4 146.2(2) . . ? O8 Er1 O4 70.9(3) . . ? O5 Ag1 O13 151.3(3) . 2_656 ? O5 Ag1 O3 130.6(3) . . ? O13 Ag1 O3 75.9(3) 2_656 . ? O5 Ag1 O3 84.7(3) . 2_556 ? O13 Ag1 O3 84.0(3) 2_656 2_556 ? O3 Ag1 O3 90.6(3) . 2_556 ? O1 Ag2 O11 150.1(3) . 2_665 ? O1 Ag2 O7 131.5(3) . . ? O11 Ag2 O7 76.8(3) 2_665 . ? O1 Ag2 O7 86.2(3) . 2_565 ? O11 Ag2 O7 84.3(3) 2_665 2_565 ? O7 Ag2 O7 89.5(3) . 2_565 ? O16 Ag3 O11 131.0(3) 1_455 1_455 ? O16 Ag3 O7 153.5(3) 1_455 2_565 ? O11 Ag3 O7 75.6(3) 1_455 2_565 ? O16 Ag3 O1 85.5(3) 1_455 . ? O11 Ag3 O1 112.9(3) 1_455 . ? O7 Ag3 O1 83.7(3) 2_565 . ? O16 Ag3 Ag5 85.4(2) 1_455 . ? O11 Ag3 Ag5 59.8(2) 1_455 . ? O7 Ag3 Ag5 114.5(2) 2_565 . ? O1 Ag3 Ag5 73.91(19) . . ? O9 Ag4 O13 131.6(3) 1_455 1_455 ? O9 Ag4 O3 154.2(3) 1_455 2_556 ? O13 Ag4 O3 74.2(3) 1_455 2_556 ? O9 Ag4 O5 87.0(3) 1_455 . ? O13 Ag4 O5 109.9(3) 1_455 . ? O3 Ag4 O5 82.4(3) 2_556 . ? O9 Ag4 Ag5 86.0(2) 1_455 . ? O13 Ag4 Ag5 59.6(2) 1_455 . ? O3 Ag4 Ag5 112.53(19) 2_556 . ? O5 Ag4 Ag5 71.8(2) . . ? O15 Ag5 O8 144.3(2) 1_455 . ? O15 Ag5 O10 70.6(3) 1_455 1_455 ? O8 Ag5 O10 120.8(3) . 1_455 ? O15 Ag5 O4 119.2(3) 1_455 . ? O8 Ag5 O4 71.4(3) . . ? O10 Ag5 O4 146.7(2) 1_455 . ? O15 Ag5 Ag3 54.79(18) 1_455 . ? O8 Ag5 Ag3 89.54(17) . . ? O10 Ag5 Ag3 98.40(17) 1_455 . ? O4 Ag5 Ag3 113.21(18) . . ? O15 Ag5 Ag4 97.74(17) 1_455 . ? O8 Ag5 Ag4 116.55(18) . . ? O10 Ag5 Ag4 54.64(17) 1_455 . ? O4 Ag5 Ag4 92.10(17) . . ? Ag3 Ag5 Ag4 148.91(4) . . ? C1 O1 Ag2 105.3(8) . . ? C1 O1 Ag3 139.8(8) . . ? Ag2 O1 Ag3 88.6(3) . . ? C1 O2 Er1 135.2(7) . . ? C8 O3 Ag1 102.0(8) . . ? C8 O3 Ag4 144.6(8) . 2_556 ? Ag1 O3 Ag4 101.5(3) . 2_556 ? C8 O3 Ag1 120.0(7) . 2_556 ? Ag1 O3 Ag1 89.4(3) . 2_556 ? Ag4 O3 Ag1 86.3(2) 2_556 2_556 ? C8 O4 Ag5 122.5(7) . . ? C8 O4 Er1 127.0(7) . . ? Ag5 O4 Er1 108.5(3) . . ? C9 O5 Ag1 105.3(7) . . ? C9 O5 Ag4 139.0(8) . . ? Ag1 O5 Ag4 91.5(3) . . ? C9 O6 Er1 135.1(7) . . ? C16 O7 Ag3 147.6(8) . 2_565 ? C16 O7 Ag2 100.7(8) . . ? Ag3 O7 Ag2 101.0(3) 2_565 . ? C16 O7 Ag2 117.8(7) . 2_565 ? Ag3 O7 Ag2 85.8(2) 2_565 2_565 ? Ag2 O7 Ag2 90.5(3) . 2_565 ? C16 O8 Ag5 121.9(7) . . ? C16 O8 Er1 125.7(7) . . ? Ag5 O8 Er1 109.2(3) . . ? C17 O9 Ag4 102.7(8) . 1_655 ? C17 O10 Ag5 124.8(7) . 1_655 ? C17 O10 Er1 125.8(7) . . ? Ag5 O10 Er1 108.9(3) 1_655 . ? C24 O11 Ag2 118.0(7) . 2_665 ? C24 O11 Ag3 117.0(8) . 1_655 ? Ag2 O11 Ag3 106.6(3) 2_665 1_655 ? C24 O12 Er1 122.5(7) . . ? C32 O13 Ag1 117.3(8) . 2_656 ? C32 O13 Ag4 115.3(8) . 1_655 ? Ag1 O13 Ag4 108.4(3) 2_656 1_655 ? C32 O14 Er1 122.7(7) . . ? C25 O15 Ag5 125.7(6) . 1_655 ? C25 O15 Er1 123.4(6) . . ? Ag5 O15 Er1 110.2(3) 1_655 . ? C25 O16 Ag3 103.4(7) . 1_655 ? O1 C1 O2 123.4(11) . . ? O1 C1 C2 117.9(11) . . ? O2 C1 C2 118.6(10) . . ? C7 C2 C3 116.7(11) . . ? C7 C2 C1 126.4(10) . . ? C3 C2 C1 116.9(10) . . ? C4 C3 C2 122.5(11) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 119.6(12) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 119.6(13) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C7 C6 C5 120.4(12) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 121.2(11) . . ? C6 C7 C8 117.2(10) . . ? C2 C7 C8 121.6(10) . . ? O3 C8 O4 120.1(11) . . ? O3 C8 C7 119.3(11) . . ? O4 C8 C7 120.6(9) . . ? O5 C9 O6 122.6(11) . . ? O5 C9 C10 119.0(10) . . ? O6 C9 C10 118.3(10) . . ? C11 C10 C15 119.4(11) . . ? C11 C10 C9 115.3(10) . . ? C15 C10 C9 125.3(10) . . ? C12 C11 C10 119.5(11) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C13 C12 C11 121.3(12) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 119.5(13) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 120.3(11) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C10 119.6(10) . . ? C14 C15 C16 117.5(10) . . ? C10 C15 C16 122.8(10) . . ? O8 C16 O7 121.1(11) . . ? O8 C16 C15 120.3(10) . . ? O7 C16 C15 118.6(11) . . ? O9 C17 O10 123.8(11) . . ? O9 C17 C18 122.2(11) . . ? O10 C17 C18 114.0(10) . . ? C23 C18 C19 118.6(12) . . ? C23 C18 C17 122.7(11) . . ? C19 C18 C17 118.6(11) . . ? C20 C19 C18 120.9(13) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C19 C20 C21 121.0(13) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C22 C21 C20 118.2(12) . . ? C22 C21 H21A 120.9 . . ? C20 C21 H21A 120.9 . . ? C23 C22 C21 120.9(12) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C18 120.4(11) . . ? C22 C23 C24 117.9(10) . . ? C18 C23 C24 121.7(10) . . ? O11 C24 O12 123.1(11) . . ? O11 C24 C23 118.5(10) . . ? O12 C24 C23 118.3(10) . . ? O16 C25 O15 122.5(10) . . ? O16 C25 C26 118.3(11) . . ? O15 C25 C26 119.1(9) . . ? C27 C26 C31 119.0(11) . . ? C27 C26 C25 122.6(10) . . ? C31 C26 C25 118.2(11) . . ? C26 C27 C28 123.0(12) . . ? C26 C27 H27A 118.5 . . ? C28 C27 H27A 118.5 . . ? C27 C28 C29 118.3(13) . . ? C27 C28 H28A 120.8 . . ? C29 C28 H28A 120.8 . . ? C30 C29 C28 120.3(13) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 120.6(12) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C30 C31 C26 118.6(11) . . ? C30 C31 C32 118.3(10) . . ? C26 C31 C32 123.1(11) . . ? O13 C32 O14 125.9(12) . . ? O13 C32 C31 119.4(10) . . ? O14 C32 C31 114.7(10) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 3.841 _refine_diff_density_min -1.765 _refine_diff_density_rms 0.345 # Attachment '743497-complex_4.CIF.txt' data_h07338 _database_code_depnum_ccdc_archive 'CCDC 743497' #TrackingRef '743497-complex_4.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Ag5 Ho O16' _chemical_formula_weight 1360.73 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.858(5) _cell_length_b 14.940(10) _cell_length_c 15.211(11) _cell_angle_alpha 63.63(3) _cell_angle_beta 81.49(3) _cell_angle_gamma 81.38(2) _cell_volume 1575.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10151 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 54.98 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 5.612 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5773 _exptl_absorpt_correction_T_max 0.7784 _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13022 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6081 _reflns_number_gt 4369 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1358P)^2^+2.3837P] 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 6081 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2151 _refine_ls_wR_factor_gt 0.1948 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ho1 Ho 0.35415(7) 0.25110(4) 0.25135(4) 0.0201(2) Uani 1 1 d . . . Ag1 Ag 0.12829(13) 0.09028(8) 0.49206(8) 0.0333(3) Uani 1 1 d . . . Ag2 Ag 0.17800(14) 0.40920(8) 0.00700(8) 0.0338(3) Uani 1 1 d . . . Ag3 Ag -0.21414(16) 0.33116(8) 0.01814(10) 0.0445(3) Uani 1 1 d . . . Ag4 Ag -0.30631(16) 0.17101(8) 0.48613(10) 0.0441(3) Uani 1 1 d . . . Ag5 Ag -0.14679(13) 0.25155(8) 0.25213(10) 0.0420(3) Uani 1 1 d . . . O1 O 0.0996(13) 0.2554(7) 0.0336(8) 0.039(2) Uani 1 1 d . . . O2 O 0.3192(11) 0.2138(6) 0.1236(7) 0.0265(19) Uani 1 1 d . . . O3 O 0.1417(13) -0.0133(7) 0.4029(8) 0.038(2) Uani 1 1 d . . . O4 O 0.1199(10) 0.1459(6) 0.2953(6) 0.0234(18) Uani 1 1 d . . . O5 O -0.0270(13) 0.2419(7) 0.4671(8) 0.042(3) Uani 1 1 d . . . O6 O 0.2192(11) 0.2873(7) 0.3769(7) 0.030(2) Uani 1 1 d . . . O7 O 0.0841(11) 0.5144(7) 0.0955(7) 0.031(2) Uani 1 1 d . . . O8 O 0.0876(9) 0.3554(6) 0.2018(7) 0.0229(18) Uani 1 1 d . . . O9 O 0.5597(13) 0.3376(7) 0.4393(7) 0.038(2) Uani 1 1 d . . . O10 O 0.5704(11) 0.3054(7) 0.3095(7) 0.031(2) Uani 1 1 d . . . O11 O 0.7097(12) 0.4405(7) 0.0977(7) 0.032(2) Uani 1 1 d . . . O12 O 0.4404(12) 0.3972(7) 0.1271(7) 0.030(2) Uani 1 1 d . . . O13 O 0.7301(11) 0.0611(7) 0.4065(8) 0.034(2) Uani 1 1 d . . . O14 O 0.4534(11) 0.1049(6) 0.3787(7) 0.0273(19) Uani 1 1 d . . . O15 O 0.6343(10) 0.1987(7) 0.1950(7) 0.029(2) Uani 1 1 d . . . O16 O 0.7210(13) 0.1679(7) 0.0645(7) 0.037(2) Uani 1 1 d . . . C1 C 0.1934(18) 0.1922(9) 0.0966(9) 0.025(3) Uani 1 1 d . . . C2 C 0.1614(17) 0.0836(10) 0.1358(10) 0.028(3) Uani 1 1 d . . . C3 C 0.158(2) 0.0472(11) 0.0669(12) 0.041(4) Uani 1 1 d . . . H3A H 0.1729 0.0900 0.0001 0.049 Uiso 1 1 calc R . . C4 C 0.134(2) -0.0519(12) 0.0964(12) 0.042(4) Uani 1 1 d . . . H4A H 0.1379 -0.0758 0.0490 0.050 Uiso 1 1 calc R . . C5 C 0.105(2) -0.1163(11) 0.1943(12) 0.041(4) Uani 1 1 d . . . H5A H 0.0841 -0.1823 0.2134 0.049 Uiso 1 1 calc R . . C6 C 0.108(2) -0.0806(11) 0.2640(12) 0.043(4) Uani 1 1 d . . . H6A H 0.0915 -0.1240 0.3305 0.052 Uiso 1 1 calc R . . C7 C 0.1348(16) 0.0189(9) 0.2370(10) 0.025(3) Uani 1 1 d . . . C8 C 0.1355(14) 0.0511(8) 0.3175(8) 0.019(2) Uani 1 1 d . . . C9 C 0.0618(17) 0.3062(10) 0.4039(9) 0.027(3) Uani 1 1 d . . . C10 C -0.0127(17) 0.4144(9) 0.3634(9) 0.025(3) Uani 1 1 d . . . C11 C -0.094(2) 0.4494(10) 0.4310(11) 0.038(3) Uani 1 1 d . . . H11A H -0.1102 0.4048 0.4972 0.046 Uiso 1 1 calc R . . C12 C -0.153(2) 0.5507(12) 0.4009(14) 0.050(4) Uani 1 1 d . . . H12A H -0.2012 0.5732 0.4479 0.060 Uiso 1 1 calc R . . C13 C -0.140(2) 0.6160(12) 0.3056(13) 0.050(4) Uani 1 1 d . . . H13A H -0.1771 0.6835 0.2867 0.060 Uiso 1 1 calc R . . C14 C -0.069(2) 0.5814(10) 0.2343(11) 0.038(3) Uani 1 1 d . . . H14A H -0.0663 0.6260 0.1679 0.046 Uiso 1 1 calc R . . C15 C -0.0012(17) 0.4812(9) 0.2611(11) 0.028(3) Uani 1 1 d . . . C16 C 0.0606(16) 0.4480(9) 0.1831(9) 0.024(3) Uani 1 1 d . . . C17 C 0.5407(17) 0.3660(10) 0.3530(12) 0.034(3) Uani 1 1 d . . . C18 C 0.4892(18) 0.4754(9) 0.2859(11) 0.033(3) Uani 1 1 d . . . C19 C 0.4293(18) 0.5390(11) 0.3320(12) 0.036(3) Uani 1 1 d . . . H19A H 0.4184 0.5129 0.4004 0.043 Uiso 1 1 calc R . . C20 C 0.387(2) 0.6385(13) 0.2773(16) 0.058(5) Uani 1 1 d . . . H20A H 0.3451 0.6806 0.3075 0.069 Uiso 1 1 calc R . . C21 C 0.409(2) 0.6768(12) 0.1729(14) 0.052(4) Uani 1 1 d . . . H21A H 0.3810 0.7447 0.1341 0.062 Uiso 1 1 calc R . . C22 C 0.4714(17) 0.6129(10) 0.1283(11) 0.034(3) Uani 1 1 d . . . H22A H 0.4923 0.6388 0.0600 0.041 Uiso 1 1 calc R . . C23 C 0.5026(15) 0.5101(9) 0.1862(10) 0.025(3) Uani 1 1 d . . . C24 C 0.5572(14) 0.4423(8) 0.1347(9) 0.021(3) Uani 1 1 d . . . C25 C 0.6645(16) 0.1405(10) 0.1511(9) 0.025(3) Uani 1 1 d . . . C26 C 0.6281(15) 0.0308(9) 0.2157(10) 0.027(3) Uani 1 1 d . . . C27 C 0.6240(18) -0.0316(10) 0.1686(11) 0.034(3) Uani 1 1 d . . . H27A H 0.6370 -0.0057 0.1002 0.041 Uiso 1 1 calc R . . C28 C 0.601(2) -0.1308(10) 0.2250(13) 0.042(4) Uani 1 1 d . . . H28A H 0.5887 -0.1716 0.1950 0.051 Uiso 1 1 calc R . . C29 C 0.594(2) -0.1709(11) 0.3270(14) 0.047(4) Uani 1 1 d . . . H29A H 0.5850 -0.2392 0.3649 0.056 Uiso 1 1 calc R . . C30 C 0.6017(18) -0.1094(10) 0.3722(12) 0.036(3) Uani 1 1 d . . . H30A H 0.6003 -0.1372 0.4404 0.044 Uiso 1 1 calc R . . C31 C 0.6113(14) -0.0052(9) 0.3167(9) 0.019(2) Uani 1 1 d . . . C32 C 0.6005(15) 0.0586(9) 0.3698(9) 0.024(3) 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 Ho1 0.0181(3) 0.0176(3) 0.0202(3) -0.0043(2) -0.0005(2) -0.0028(2) Ag1 0.0360(6) 0.0247(5) 0.0285(6) -0.0036(5) -0.0019(4) 0.0015(4) Ag2 0.0395(6) 0.0242(5) 0.0308(6) -0.0039(5) -0.0024(5) -0.0097(4) Ag3 0.0462(7) 0.0291(6) 0.0498(8) -0.0113(6) 0.0097(6) -0.0117(5) Ag4 0.0459(7) 0.0309(6) 0.0527(8) -0.0139(6) -0.0167(6) 0.0030(5) Ag5 0.0276(6) 0.0341(6) 0.0656(9) -0.0223(6) -0.0044(5) -0.0038(4) O1 0.041(5) 0.019(5) 0.047(6) 0.003(4) -0.027(5) -0.007(4) O2 0.022(4) 0.029(5) 0.030(5) -0.012(4) -0.003(4) -0.009(4) O3 0.045(6) 0.025(5) 0.038(6) -0.001(5) -0.012(5) -0.014(4) O4 0.015(4) 0.026(5) 0.024(4) -0.005(4) 0.008(3) -0.010(3) O5 0.037(5) 0.022(5) 0.052(7) -0.003(5) 0.009(5) -0.011(4) O6 0.018(4) 0.037(5) 0.030(5) -0.014(4) -0.006(4) 0.009(4) O7 0.029(5) 0.027(5) 0.024(5) -0.001(4) -0.002(4) 0.001(4) O8 0.011(4) 0.018(4) 0.034(5) -0.005(4) -0.004(3) -0.002(3) O9 0.048(6) 0.034(6) 0.030(6) -0.011(5) -0.012(5) -0.001(4) O10 0.027(5) 0.024(5) 0.032(5) -0.003(4) 0.001(4) -0.004(4) O11 0.034(5) 0.029(5) 0.026(5) -0.007(4) 0.010(4) -0.012(4) O12 0.031(5) 0.025(5) 0.026(5) -0.002(4) -0.003(4) -0.004(4) O13 0.027(5) 0.030(5) 0.044(6) -0.011(5) -0.012(4) -0.006(4) O14 0.023(4) 0.024(5) 0.025(5) -0.003(4) 0.004(4) -0.004(4) O15 0.018(4) 0.031(5) 0.029(5) -0.007(4) 0.006(4) -0.004(3) O16 0.046(6) 0.036(6) 0.020(5) -0.008(4) 0.008(4) -0.002(4) C1 0.042(7) 0.014(6) 0.022(7) -0.010(5) -0.003(6) -0.001(5) C2 0.035(7) 0.030(7) 0.027(7) -0.015(6) 0.006(6) -0.020(6) C3 0.059(10) 0.024(7) 0.035(8) -0.004(6) -0.010(7) -0.011(6) C4 0.058(10) 0.042(9) 0.040(9) -0.030(8) -0.014(8) 0.005(7) C5 0.059(10) 0.029(8) 0.044(9) -0.024(7) -0.019(8) 0.009(7) C6 0.059(10) 0.029(8) 0.036(9) -0.009(7) -0.005(8) -0.008(7) C7 0.022(6) 0.023(6) 0.029(7) -0.009(6) 0.001(5) -0.003(5) C8 0.015(5) 0.017(6) 0.011(6) 0.005(5) 0.002(4) -0.001(4) C9 0.036(7) 0.026(7) 0.020(6) -0.010(6) -0.012(6) 0.009(6) C10 0.036(7) 0.016(6) 0.020(6) -0.003(5) 0.000(5) -0.004(5) C11 0.061(10) 0.016(6) 0.023(7) 0.004(6) -0.003(7) -0.002(6) C12 0.064(11) 0.033(9) 0.051(11) -0.019(8) 0.005(9) -0.006(8) C13 0.063(11) 0.027(8) 0.051(11) -0.012(8) 0.000(8) 0.007(7) C14 0.055(9) 0.023(7) 0.030(8) -0.004(6) -0.011(7) -0.003(6) C15 0.029(7) 0.015(6) 0.042(8) -0.014(6) 0.002(6) -0.007(5) C16 0.027(6) 0.015(6) 0.015(6) 0.008(5) -0.008(5) -0.003(5) C17 0.030(7) 0.023(7) 0.050(10) -0.014(7) -0.012(7) 0.001(5) C18 0.034(7) 0.014(6) 0.046(9) -0.005(6) -0.013(6) -0.002(5) C19 0.035(7) 0.031(8) 0.040(9) -0.015(7) -0.005(6) 0.003(6) C20 0.056(10) 0.040(10) 0.088(15) -0.041(11) -0.007(10) 0.006(8) C21 0.063(11) 0.033(9) 0.057(11) -0.022(9) -0.012(9) 0.021(8) C22 0.034(7) 0.032(8) 0.032(8) -0.009(6) 0.004(6) -0.014(6) C23 0.015(5) 0.017(6) 0.041(8) -0.011(6) 0.003(5) -0.003(4) C24 0.015(5) 0.009(5) 0.031(7) -0.001(5) -0.005(5) -0.004(4) C25 0.026(6) 0.027(7) 0.020(6) -0.012(6) 0.005(5) 0.001(5) C26 0.020(6) 0.019(6) 0.031(7) -0.003(6) -0.002(5) 0.001(5) C27 0.036(7) 0.029(7) 0.033(8) -0.013(6) 0.012(6) -0.008(6) C28 0.053(9) 0.019(7) 0.055(11) -0.020(7) 0.004(8) 0.000(6) C29 0.055(10) 0.020(7) 0.065(12) -0.017(8) 0.002(9) -0.014(7) C30 0.035(7) 0.026(7) 0.038(8) -0.009(7) 0.006(6) 0.001(6) C31 0.015(5) 0.023(6) 0.021(6) -0.011(5) 0.002(5) -0.002(4) C32 0.019(6) 0.018(6) 0.021(6) 0.006(5) -0.006(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O12 2.279(9) . ? Ho1 O6 2.282(9) . ? Ho1 O14 2.304(9) . ? Ho1 O2 2.307(9) . ? Ho1 O15 2.390(8) . ? Ho1 O10 2.413(9) . ? Ho1 O8 2.415(8) . ? Ho1 O4 2.424(8) . ? Ag1 O5 2.304(10) . ? Ag1 O13 2.321(9) 2_656 ? Ag1 O3 2.453(10) . ? Ag1 O3 2.544(10) 2_556 ? Ag2 O1 2.312(9) . ? Ag2 O11 2.314(9) 2_665 ? Ag2 O7 2.463(10) . ? Ag2 O7 2.577(9) 2_565 ? Ag3 O16 2.333(10) 1_455 ? Ag3 O11 2.396(9) 1_455 ? Ag3 O7 2.449(9) 2_565 ? Ag3 O1 2.552(10) . ? Ag3 Ag5 3.312(3) . ? Ag4 O9 2.382(10) 1_455 ? Ag4 O13 2.402(10) 1_455 ? Ag4 O5 2.501(10) . ? Ag4 O3 2.505(10) 2_556 ? Ag4 Ag5 3.319(3) . ? Ag5 O8 2.402(8) . ? Ag5 O15 2.408(9) 1_455 ? Ag5 O4 2.410(8) . ? Ag5 O10 2.420(9) 1_455 ? O1 C1 1.245(16) . ? O2 C1 1.260(15) . ? O3 C8 1.229(15) . ? O3 Ag4 2.505(10) 2_556 ? O3 Ag1 2.544(10) 2_556 ? O4 C8 1.292(14) . ? O5 C9 1.231(17) . ? O6 C9 1.275(16) . ? O7 C16 1.265(15) . ? O7 Ag3 2.449(9) 2_565 ? O7 Ag2 2.577(9) 2_565 ? O8 C16 1.272(14) . ? O9 C17 1.212(18) . ? O9 Ag4 2.382(10) 1_655 ? O10 C17 1.318(16) . ? O10 Ag5 2.420(9) 1_655 ? O11 C24 1.248(15) . ? O11 Ag2 2.314(9) 2_665 ? O11 Ag3 2.396(9) 1_655 ? O12 C24 1.264(14) . ? O13 C32 1.244(15) . ? O13 Ag1 2.321(9) 2_656 ? O13 Ag4 2.402(10) 1_655 ? O14 C32 1.277(15) . ? O15 C25 1.290(15) . ? O15 Ag5 2.408(9) 1_655 ? O16 C25 1.226(15) . ? O16 Ag3 2.333(10) 1_655 ? C1 C2 1.507(16) . ? C2 C3 1.382(19) . ? C2 C7 1.411(18) . ? C3 C4 1.38(2) . ? C3 H3A 0.9300 . ? C4 C5 1.37(2) . ? C4 H4A 0.9300 . ? C5 C6 1.39(2) . ? C5 H5A 0.9300 . ? C6 C7 1.395(19) . ? C6 H6A 0.9300 . ? C7 C8 1.504(17) . ? C9 C10 1.508(17) . ? C10 C11 1.387(19) . ? C10 C15 1.425(18) . ? C11 C12 1.40(2) . ? C11 H11A 0.9300 . ? C12 C13 1.34(2) . ? C12 H12A 0.9300 . ? C13 C14 1.41(2) . ? C13 H13A 0.9300 . ? C14 C15 1.404(18) . ? C14 H14A 0.9300 . ? C15 C16 1.473(18) . ? C17 C18 1.522(18) . ? C18 C23 1.36(2) . ? C18 C19 1.41(2) . ? C19 C20 1.36(2) . ? C19 H19A 0.9300 . ? C20 C21 1.42(3) . ? C20 H20A 0.9300 . ? C21 C22 1.40(2) . ? C21 H21A 0.9300 . ? C22 C23 1.394(18) . ? C22 H22A 0.9300 . ? C23 C24 1.516(17) . ? C25 C26 1.536(17) . ? C26 C31 1.376(17) . ? C26 C27 1.412(19) . ? C27 C28 1.37(2) . ? C27 H27A 0.9300 . ? C28 C29 1.39(2) . ? C28 H28A 0.9300 . ? C29 C30 1.38(2) . ? C29 H29A 0.9300 . ? C30 C31 1.411(18) . ? C30 H30A 0.9300 . ? C31 C32 1.486(17) . ? 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 O12 Ho1 O6 107.4(3) . . ? O12 Ho1 O14 142.7(3) . . ? O6 Ho1 O14 83.1(3) . . ? O12 Ho1 O2 83.5(3) . . ? O6 Ho1 O2 146.0(3) . . ? O14 Ho1 O2 107.9(3) . . ? O12 Ho1 O15 77.6(3) . . ? O6 Ho1 O15 140.4(3) . . ? O14 Ho1 O15 72.6(3) . . ? O2 Ho1 O15 72.7(3) . . ? O12 Ho1 O10 72.2(3) . . ? O6 Ho1 O10 73.4(3) . . ? O14 Ho1 O10 77.2(3) . . ? O2 Ho1 O10 139.8(3) . . ? O15 Ho1 O10 71.1(3) . . ? O12 Ho1 O8 75.8(3) . . ? O6 Ho1 O8 70.1(3) . . ? O14 Ho1 O8 139.7(3) . . ? O2 Ho1 O8 82.2(3) . . ? O15 Ho1 O8 145.1(3) . . ? O10 Ho1 O8 120.4(3) . . ? O12 Ho1 O4 138.7(3) . . ? O6 Ho1 O4 82.9(3) . . ? O14 Ho1 O4 77.0(3) . . ? O2 Ho1 O4 69.1(3) . . ? O15 Ho1 O4 119.8(3) . . ? O10 Ho1 O4 146.6(3) . . ? O8 Ho1 O4 70.5(3) . . ? O5 Ag1 O13 151.1(4) . 2_656 ? O5 Ag1 O3 130.4(4) . . ? O13 Ag1 O3 76.5(3) 2_656 . ? O5 Ag1 O3 85.1(3) . 2_556 ? O13 Ag1 O3 84.0(3) 2_656 2_556 ? O3 Ag1 O3 90.8(4) . 2_556 ? O1 Ag2 O11 149.9(4) . 2_665 ? O1 Ag2 O7 131.3(4) . . ? O11 Ag2 O7 77.1(3) 2_665 . ? O1 Ag2 O7 85.8(3) . 2_565 ? O11 Ag2 O7 84.2(3) 2_665 2_565 ? O7 Ag2 O7 90.4(3) . 2_565 ? O16 Ag3 O11 131.2(3) 1_455 1_455 ? O16 Ag3 O7 152.9(3) 1_455 2_565 ? O11 Ag3 O7 75.9(3) 1_455 2_565 ? O16 Ag3 O1 85.3(3) 1_455 . ? O11 Ag3 O1 112.6(3) 1_455 . ? O7 Ag3 O1 83.6(3) 2_565 . ? O16 Ag3 Ag5 85.6(2) 1_455 . ? O11 Ag3 Ag5 59.7(2) 1_455 . ? O7 Ag3 Ag5 114.7(2) 2_565 . ? O1 Ag3 Ag5 73.8(2) . . ? O9 Ag4 O13 131.9(3) 1_455 1_455 ? O9 Ag4 O5 86.7(3) 1_455 . ? O13 Ag4 O5 109.6(3) 1_455 . ? O9 Ag4 O3 154.0(3) 1_455 2_556 ? O13 Ag4 O3 74.1(3) 1_455 2_556 ? O5 Ag4 O3 82.0(3) . 2_556 ? O9 Ag4 Ag5 85.7(3) 1_455 . ? O13 Ag4 Ag5 59.8(2) 1_455 . ? O5 Ag4 Ag5 71.7(3) . . ? O3 Ag4 Ag5 112.4(3) 2_556 . ? O8 Ag5 O15 144.7(3) . 1_455 ? O8 Ag5 O4 71.0(3) . . ? O15 Ag5 O4 119.2(3) 1_455 . ? O8 Ag5 O10 121.0(3) . 1_455 ? O15 Ag5 O10 70.6(3) 1_455 1_455 ? O4 Ag5 O10 147.1(3) . 1_455 ? O8 Ag5 Ag3 89.8(2) . . ? O15 Ag5 Ag3 54.9(2) 1_455 . ? O4 Ag5 Ag3 113.2(2) . . ? O10 Ag5 Ag3 98.2(2) 1_455 . ? O8 Ag5 Ag4 116.4(2) . . ? O15 Ag5 Ag4 97.6(2) 1_455 . ? O4 Ag5 Ag4 92.4(2) . . ? O10 Ag5 Ag4 54.7(2) 1_455 . ? Ag3 Ag5 Ag4 148.77(5) . . ? C1 O1 Ag2 105.1(8) . . ? C1 O1 Ag3 140.0(10) . . ? Ag2 O1 Ag3 88.9(3) . . ? C1 O2 Ho1 134.3(8) . . ? C8 O3 Ag1 101.4(8) . . ? C8 O3 Ag4 144.3(9) . 2_556 ? Ag1 O3 Ag4 101.1(4) . 2_556 ? C8 O3 Ag1 121.5(8) . 2_556 ? Ag1 O3 Ag1 89.2(4) . 2_556 ? Ag4 O3 Ag1 86.1(3) 2_556 2_556 ? C8 O4 Ag5 123.3(7) . . ? C8 O4 Ho1 126.2(7) . . ? Ag5 O4 Ho1 108.9(3) . . ? C9 O5 Ag1 105.5(8) . . ? C9 O5 Ag4 139.3(10) . . ? Ag1 O5 Ag4 91.6(3) . . ? C9 O6 Ho1 134.1(8) . . ? C16 O7 Ag3 147.8(8) . 2_565 ? C16 O7 Ag2 100.9(8) . . ? Ag3 O7 Ag2 100.5(3) 2_565 . ? C16 O7 Ag2 118.5(7) . 2_565 ? Ag3 O7 Ag2 85.4(3) 2_565 2_565 ? Ag2 O7 Ag2 89.6(3) . 2_565 ? C16 O8 Ag5 121.2(7) . . ? C16 O8 Ho1 125.5(7) . . ? Ag5 O8 Ho1 109.5(3) . . ? C17 O9 Ag4 103.3(8) . 1_655 ? C17 O10 Ho1 125.7(8) . . ? C17 O10 Ag5 125.1(8) . 1_655 ? Ho1 O10 Ag5 108.6(4) . 1_655 ? C24 O11 Ag2 118.9(8) . 2_665 ? C24 O11 Ag3 115.8(8) . 1_655 ? Ag2 O11 Ag3 106.6(4) 2_665 1_655 ? C24 O12 Ho1 122.4(8) . . ? C32 O13 Ag1 118.1(8) . 2_656 ? C32 O13 Ag4 115.3(8) . 1_655 ? Ag1 O13 Ag4 108.3(4) 2_656 1_655 ? C32 O14 Ho1 121.6(8) . . ? C25 O15 Ho1 125.2(8) . . ? C25 O15 Ag5 124.6(7) . 1_655 ? Ho1 O15 Ag5 109.7(4) . 1_655 ? C25 O16 Ag3 103.1(8) . 1_655 ? O1 C1 O2 123.4(11) . . ? O1 C1 C2 117.5(11) . . ? O2 C1 C2 119.0(11) . . ? C3 C2 C7 119.4(12) . . ? C3 C2 C1 116.7(12) . . ? C7 C2 C1 123.9(11) . . ? C4 C3 C2 120.6(14) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C5 C4 C3 121.3(13) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 118.5(14) . . ? C4 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? C5 C6 C7 121.7(15) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C2 118.5(12) . . ? C6 C7 C8 118.1(12) . . ? C2 C7 C8 123.4(11) . . ? O3 C8 O4 122.1(12) . . ? O3 C8 C7 118.9(11) . . ? O4 C8 C7 118.8(10) . . ? O5 C9 O6 123.3(12) . . ? O5 C9 C10 118.6(12) . . ? O6 C9 C10 117.8(12) . . ? C11 C10 C15 119.4(11) . . ? C11 C10 C9 117.0(11) . . ? C15 C10 C9 123.6(11) . . ? C10 C11 C12 120.8(14) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 121.2(16) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 119.4(15) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 121.6(14) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C14 C15 C10 117.5(12) . . ? C14 C15 C16 119.0(13) . . ? C10 C15 C16 123.2(11) . . ? O7 C16 O8 120.1(12) . . ? O7 C16 C15 118.1(11) . . ? O8 C16 C15 121.7(11) . . ? O9 C17 O10 122.4(12) . . ? O9 C17 C18 122.3(13) . . ? O10 C17 C18 115.2(13) . . ? C23 C18 C19 121.7(12) . . ? C23 C18 C17 121.6(12) . . ? C19 C18 C17 116.8(13) . . ? C20 C19 C18 120.4(15) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C19 C20 C21 118.5(15) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C22 C21 C20 120.3(15) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C21 119.9(14) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C18 C23 C22 118.9(12) . . ? C18 C23 C24 122.9(11) . . ? C22 C23 C24 118.2(12) . . ? O11 C24 O12 125.2(12) . . ? O11 C24 C23 117.9(10) . . ? O12 C24 C23 116.7(10) . . ? O16 C25 O15 123.9(12) . . ? O16 C25 C26 120.7(12) . . ? O15 C25 C26 115.4(11) . . ? C31 C26 C27 122.1(12) . . ? C31 C26 C25 119.7(11) . . ? C27 C26 C25 118.1(12) . . ? C28 C27 C26 119.0(14) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 120.3(13) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 120.0(14) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 121.2(14) . . ? C29 C30 H30A 119.4 . . ? C31 C30 H30A 119.4 . . ? C26 C31 C30 117.1(11) . . ? C26 C31 C32 124.2(11) . . ? C30 C31 C32 118.7(11) . . ? O13 C32 O14 123.6(13) . . ? O13 C32 C31 119.4(11) . . ? O14 C32 C31 116.9(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 6.176 _refine_diff_density_min -2.664 _refine_diff_density_rms 0.369