# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Wei-Yin Sun.' 'Man-Sheng Chen.' 'Shui-Sheng Chen.' 'Yi-Zhi Li.' 'Chen Min.' 'Zhi Su.' _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email SUNWY@NJU.EDU.CN _publ_section_title ; Three-dimensional lanthanide-silver heterometallic coordination polymers: syntheses, structures and properties ; # Attachment 'sunwy.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 760885' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag N4 Nd O13' _chemical_formula_weight 874.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.6611(18) _cell_length_b 10.8856(7) _cell_length_c 20.7761(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.6930(10) _cell_angle_gamma 90.00 _cell_volume 5852.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3794 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 24.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 2.501 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5625 _exptl_absorpt_correction_T_max 0.7880 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14387 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5286 _reflns_number_gt 4922 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0594P)^2^+31.2827P] 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 5286 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.017660(19) 0.54996(7) 0.66383(3) 0.0631(2) Uani 1 1 d . . . Nd1 Nd 0.448678(9) 0.62610(2) 0.531083(12) 0.01660(11) Uani 1 1 d . . . C1 C 0.4085(2) 0.8712(4) 0.5083(3) 0.0239(11) Uani 1 1 d . . . C2 C 0.39127(19) 1.0018(5) 0.4920(3) 0.0237(11) Uani 1 1 d . . . C3 C 0.3396(2) 1.0331(5) 0.4648(3) 0.0240(11) Uani 1 1 d . . . H3 H 0.3144 0.9720 0.4528 0.029 Uiso 1 1 calc R . . C4 C 0.32531(19) 1.1562(5) 0.4553(3) 0.0255(11) Uani 1 1 d . . . C5 C 0.3630(2) 1.2473(5) 0.4754(3) 0.0269(11) Uani 1 1 d . . . H5 H 0.3536 1.3297 0.4715 0.032 Uiso 1 1 calc R . . C6 C 0.41482(19) 1.2147(4) 0.5012(3) 0.0224(10) Uani 1 1 d . . . C7 C 0.42924(19) 1.0925(5) 0.5083(3) 0.0220(10) Uani 1 1 d . . . H7 H 0.4640 1.0709 0.5238 0.026 Uiso 1 1 calc R . . C8 C 0.45557(19) 1.3121(5) 0.5276(3) 0.0267(11) Uani 1 1 d . . . C9 C 0.2523(2) 1.2884(6) 0.3915(3) 0.0348(13) Uani 1 1 d . . . C10 C 0.1960(2) 1.3168(5) 0.3747(3) 0.0296(12) Uani 1 1 d . . . C11 C 0.1573(2) 1.2310(6) 0.3649(3) 0.0422(15) Uani 1 1 d . . . H11 H 0.1651 1.1476 0.3694 0.051 Uiso 1 1 calc R . . C12 C 0.1071(2) 1.2703(7) 0.3484(3) 0.0457(16) Uani 1 1 d . . . H12 H 0.0813 1.2114 0.3407 0.055 Uiso 1 1 calc R . . C13 C 0.1308(2) 1.4704(6) 0.3522(3) 0.0384(14) Uani 1 1 d . . . H13 H 0.1220 1.5532 0.3484 0.046 Uiso 1 1 calc R . . C14 C 0.1814(2) 1.4395(6) 0.3671(3) 0.0371(13) Uani 1 1 d . . . H14 H 0.2060 1.5005 0.3721 0.045 Uiso 1 1 calc R . . C15 C 0.4038(2) 0.6155(5) 0.6387(3) 0.0262(11) Uani 1 1 d . . . C16 C 0.38049(19) 0.5964(5) 0.6930(3) 0.0226(10) Uani 1 1 d . . . C17 C 0.41216(19) 0.5744(5) 0.7611(3) 0.0248(11) Uani 1 1 d . . . H17 H 0.4479 0.5815 0.7743 0.030 Uiso 1 1 calc R . . C18 C 0.38987(18) 0.5419(5) 0.8090(2) 0.0217(10) Uani 1 1 d . . . C19 C 0.33674(19) 0.5308(5) 0.7899(2) 0.0241(11) Uani 1 1 d . . . H19 H 0.3222 0.5060 0.8219 0.029 Uiso 1 1 calc R . . C20 C 0.30541(18) 0.5572(5) 0.7228(3) 0.0250(11) Uani 1 1 d . . . C21 C 0.3274(2) 0.5906(5) 0.6747(3) 0.0282(11) Uani 1 1 d . . . H21 H 0.3063 0.6091 0.6299 0.034 Uiso 1 1 calc R . . C22 C 0.42201(18) 0.5191(5) 0.8830(3) 0.0232(11) Uani 1 1 d . . . C23 C 0.2239(2) 0.4729(6) 0.7244(3) 0.0308(12) Uani 1 1 d . . . C24 C 0.1664(2) 0.4955(5) 0.7010(3) 0.0286(12) Uani 1 1 d . . . C25 C 0.1338(2) 0.3953(6) 0.6915(3) 0.0383(14) Uani 1 1 d . . . H25 H 0.1471 0.3160 0.6963 0.046 Uiso 1 1 calc R . . C26 C 0.0816(2) 0.4140(7) 0.6751(3) 0.0427(15) Uani 1 1 d . . . H26 H 0.0600 0.3461 0.6680 0.051 Uiso 1 1 calc R . . C27 C 0.0924(2) 0.6229(6) 0.6765(3) 0.0431(16) Uani 1 1 d . . . H27 H 0.0782 0.7013 0.6708 0.052 Uiso 1 1 calc R . . C28 C 0.1452(2) 0.6112(6) 0.6924(3) 0.0377(14) Uani 1 1 d . . . H28 H 0.1659 0.6803 0.6973 0.045 Uiso 1 1 calc R . . N1 N 0.06089(18) 0.5262(6) 0.6689(3) 0.0434(13) Uani 1 1 d . . . N2 N 0.25068(16) 0.5564(5) 0.7022(2) 0.0302(11) Uani 1 1 d . . . H2 H 0.2336 0.6122 0.6741 0.036 Uiso 1 1 calc R . . N3 N 0.09348(19) 1.3882(5) 0.3428(3) 0.0390(12) Uani 1 1 d . . . N4 N 0.27171(16) 1.1874(4) 0.4298(2) 0.0291(10) Uani 1 1 d . . . H4 H 0.2505 1.1392 0.4394 0.035 Uiso 1 1 calc R . . O1 O 0.44799(15) 0.8502(3) 0.5601(2) 0.0337(9) Uani 1 1 d . . . O2 O 0.38385(14) 0.7860(3) 0.46982(19) 0.0300(8) Uani 1 1 d . . . O3 O 0.50092(14) 1.2870(4) 0.5311(2) 0.0331(9) Uani 1 1 d . . . O4 O 0.44171(15) 1.4107(4) 0.5463(2) 0.0357(9) Uani 1 1 d . . . O5 O 0.27778(18) 1.3584(6) 0.3710(3) 0.0728(19) Uani 1 1 d . . . O6 O 0.45172(15) 0.6323(4) 0.6555(2) 0.0363(10) Uani 1 1 d . . . O7 O 0.37510(14) 0.6114(4) 0.57634(19) 0.0327(9) Uani 1 1 d . . . O8 O 0.46549(14) 0.5712(4) 0.90600(19) 0.0344(9) Uani 1 1 d . . . O9 O 0.40379(14) 0.4517(4) 0.91726(19) 0.0335(9) Uani 1 1 d . . . O10 O 0.24301(16) 0.3850(4) 0.7611(2) 0.0453(11) Uani 1 1 d . . . O1W O 0.78126(18) 1.0133(5) 0.0131(2) 0.0558(13) Uani 1 1 d . . . H1WA H 0.8108 0.9812 0.0332 0.067 Uiso 1 1 d R . . H1WB H 0.7597 0.9558 -0.0037 0.067 Uiso 1 1 d R . . O2W O 0.78258(17) 0.7653(5) 0.8893(2) 0.0525(12) Uani 1 1 d . . . H2WB H 0.7798 0.8030 0.8523 0.063 Uiso 1 1 d R . . H2WA H 0.8137 0.7513 0.9148 0.063 Uiso 1 1 d R . . O3W O 0.5000 0.8277(6) 0.7500 0.061(2) Uani 1 2 d S . . H3WB H 0.5204 0.7695 0.7496 0.073 Uiso 0.50 1 d PR . . H3WA H 0.4970 0.8134 0.7886 0.073 Uiso 0.50 1 d PR . . O4W O 0.2193(6) 0.6833(10) 0.4646(8) 0.095(5) Uani 0.50 1 d P . . H4WA H 0.2253 0.7579 0.4580 0.114 Uiso 0.50 1 d PR . . H4WB H 0.1886 0.6640 0.4400 0.114 Uiso 0.50 1 d PR . . 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 Ag1 0.0240(3) 0.1031(5) 0.0658(4) 0.0140(3) 0.0202(2) 0.0182(3) Nd1 0.01552(16) 0.01439(16) 0.02002(16) -0.00017(9) 0.00643(11) 0.00085(9) C1 0.024(3) 0.021(3) 0.027(3) -0.002(2) 0.010(2) 0.001(2) C2 0.027(3) 0.019(3) 0.026(3) -0.002(2) 0.010(2) 0.005(2) C3 0.025(3) 0.020(3) 0.027(3) 0.001(2) 0.009(2) -0.001(2) C4 0.020(2) 0.029(3) 0.029(3) -0.001(2) 0.010(2) 0.004(2) C5 0.028(3) 0.018(3) 0.037(3) 0.000(2) 0.015(2) 0.004(2) C6 0.024(2) 0.015(2) 0.032(3) 0.004(2) 0.014(2) 0.004(2) C7 0.019(2) 0.019(2) 0.030(3) -0.001(2) 0.011(2) 0.000(2) C8 0.028(3) 0.023(3) 0.032(3) 0.007(2) 0.014(2) -0.001(2) C9 0.024(3) 0.042(3) 0.042(3) 0.009(3) 0.016(2) 0.006(2) C10 0.026(3) 0.034(3) 0.030(3) 0.006(2) 0.012(2) 0.006(2) C11 0.035(3) 0.035(3) 0.060(4) 0.011(3) 0.021(3) 0.005(3) C12 0.027(3) 0.053(4) 0.056(4) 0.004(3) 0.013(3) -0.006(3) C13 0.036(3) 0.039(3) 0.040(3) 0.006(3) 0.012(3) 0.016(3) C14 0.035(3) 0.035(3) 0.043(3) 0.007(3) 0.016(3) 0.002(3) C15 0.025(3) 0.029(3) 0.027(3) 0.003(2) 0.012(2) 0.004(2) C16 0.021(2) 0.024(3) 0.024(2) 0.001(2) 0.010(2) -0.001(2) C17 0.017(2) 0.028(3) 0.030(3) 0.005(2) 0.008(2) 0.001(2) C18 0.019(2) 0.022(3) 0.023(2) -0.001(2) 0.006(2) -0.0019(19) C19 0.022(3) 0.030(3) 0.021(2) -0.001(2) 0.010(2) -0.002(2) C20 0.017(2) 0.031(3) 0.026(3) 0.001(2) 0.006(2) 0.001(2) C21 0.025(3) 0.038(3) 0.020(2) 0.002(2) 0.005(2) 0.003(2) C22 0.020(2) 0.024(3) 0.025(3) -0.004(2) 0.008(2) 0.005(2) C23 0.024(3) 0.043(3) 0.024(3) -0.002(2) 0.007(2) -0.002(2) C24 0.021(3) 0.042(3) 0.024(3) 0.005(2) 0.008(2) 0.002(2) C25 0.026(3) 0.047(4) 0.045(3) -0.001(3) 0.015(3) -0.001(3) C26 0.025(3) 0.050(4) 0.056(4) -0.002(3) 0.018(3) -0.005(3) C27 0.031(3) 0.053(4) 0.050(4) 0.010(3) 0.019(3) 0.012(3) C28 0.027(3) 0.050(4) 0.039(3) 0.006(3) 0.016(3) 0.000(3) N1 0.020(2) 0.067(4) 0.043(3) 0.006(3) 0.010(2) -0.001(2) N2 0.015(2) 0.050(3) 0.024(2) 0.008(2) 0.0050(17) 0.003(2) N3 0.027(3) 0.051(3) 0.041(3) 0.007(2) 0.015(2) 0.012(2) N4 0.020(2) 0.026(2) 0.042(3) 0.006(2) 0.0113(19) 0.0031(18) O1 0.036(2) 0.0200(19) 0.033(2) -0.0027(16) -0.0029(17) 0.0036(16) O2 0.0298(19) 0.0159(18) 0.035(2) -0.0017(15) 0.0003(16) 0.0019(15) O3 0.0254(19) 0.030(2) 0.045(2) 0.0083(17) 0.0140(17) -0.0028(16) O4 0.040(2) 0.0170(19) 0.053(2) -0.0029(18) 0.021(2) -0.0067(17) O5 0.029(2) 0.090(4) 0.103(4) 0.065(4) 0.027(3) 0.015(2) O6 0.023(2) 0.061(3) 0.029(2) 0.0045(18) 0.0135(16) -0.0008(18) O7 0.0245(19) 0.049(3) 0.025(2) 0.0029(17) 0.0097(16) -0.0016(17) O8 0.0215(19) 0.047(2) 0.029(2) -0.0036(18) 0.0021(15) -0.0021(18) O9 0.030(2) 0.039(2) 0.030(2) 0.0116(17) 0.0094(16) 0.0007(17) O10 0.027(2) 0.047(3) 0.056(3) 0.015(2) 0.008(2) 0.0028(19) O1W 0.041(3) 0.066(3) 0.055(3) -0.001(3) 0.010(2) 0.009(2) O2W 0.037(2) 0.069(3) 0.045(3) 0.006(2) 0.006(2) 0.002(2) O3W 0.079(5) 0.034(4) 0.087(5) 0.000 0.052(4) 0.000 O4W 0.143(12) 0.029(6) 0.168(13) 0.015(7) 0.123(11) 0.016(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 Ag1 N1 2.154(5) . ? Ag1 N3 2.160(5) 5_576 ? Ag1 Ag1 3.3619(12) 2_556 ? Nd1 O8 2.347(4) 2_656 ? Nd1 O4 2.383(4) 1_545 ? Nd1 O9 2.403(4) 6_565 ? Nd1 O3 2.404(4) 5_676 ? Nd1 O2 2.501(3) . ? Nd1 O1 2.514(4) . ? Nd1 O7 2.531(4) . ? Nd1 O6 2.558(4) . ? C1 O1 1.254(6) . ? C1 O2 1.256(6) . ? C1 C2 1.499(7) . ? C2 C3 1.381(7) . ? C2 C7 1.393(7) . ? C3 C4 1.391(7) . ? C3 H3 0.9300 . ? C4 C5 1.393(7) . ? C4 N4 1.428(6) . ? C5 C6 1.386(7) . ? C5 H5 0.9300 . ? C6 C7 1.381(7) . ? C6 C8 1.503(7) . ? C7 H7 0.9300 . ? C8 O4 1.247(7) . ? C8 O3 1.260(6) . ? C9 O5 1.212(7) . ? C9 N4 1.353(7) . ? C9 C10 1.502(7) . ? C10 C11 1.380(8) . ? C10 C14 1.389(8) . ? C11 C12 1.378(9) . ? C11 H11 0.9300 . ? C12 N3 1.330(8) . ? C12 H12 0.9300 . ? C13 N3 1.327(8) . ? C13 C14 1.364(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.258(6) . ? C15 O7 1.259(6) . ? C15 C16 1.498(7) . ? C16 C21 1.381(7) . ? C16 C17 1.398(7) . ? C17 C18 1.388(7) . ? C17 H17 0.9300 . ? C18 C19 1.386(7) . ? C18 C22 1.499(7) . ? C19 C20 1.388(7) . ? C19 H19 0.9300 . ? C20 C21 1.390(7) . ? C20 N2 1.420(6) . ? C21 H21 0.9300 . ? C22 O9 1.246(6) . ? C22 O8 1.261(6) . ? C23 O10 1.221(7) . ? C23 N2 1.352(7) . ? C23 C24 1.511(7) . ? C24 C28 1.374(8) . ? C24 C25 1.384(8) . ? C25 C26 1.376(8) . ? C25 H25 0.9300 . ? C26 N1 1.336(9) . ? C26 H26 0.9300 . ? C27 N1 1.340(9) . ? C27 C28 1.383(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N2 H2 0.8600 . ? N3 Ag1 2.160(5) 5_576 ? N4 H4 0.8600 . ? O3 Nd1 2.404(4) 5_676 ? O4 Nd1 2.383(4) 1_565 ? O8 Nd1 2.347(4) 2_656 ? O9 Nd1 2.403(4) 6_566 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O2W H2WB 0.8502 . ? O2W H2WA 0.8501 . ? O3W H3WB 0.8500 . ? O3W H3WA 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 168.7(2) . 5_576 ? N1 Ag1 Ag1 92.28(14) . 2_556 ? N3 Ag1 Ag1 88.74(14) 5_576 2_556 ? O8 Nd1 O4 77.80(14) 2_656 1_545 ? O8 Nd1 O9 121.83(13) 2_656 6_565 ? O4 Nd1 O9 75.28(14) 1_545 6_565 ? O8 Nd1 O3 74.62(13) 2_656 5_676 ? O4 Nd1 O3 123.23(14) 1_545 5_676 ? O9 Nd1 O3 78.82(13) 6_565 5_676 ? O8 Nd1 O2 149.66(14) 2_656 . ? O4 Nd1 O2 132.49(13) 1_545 . ? O9 Nd1 O2 73.52(12) 6_565 . ? O3 Nd1 O2 84.29(13) 5_676 . ? O8 Nd1 O1 101.86(14) 2_656 . ? O4 Nd1 O1 156.20(15) 1_545 . ? O9 Nd1 O1 122.19(13) 6_565 . ? O3 Nd1 O1 78.58(14) 5_676 . ? O2 Nd1 O1 51.81(12) . . ? O8 Nd1 O7 124.40(13) 2_656 . ? O4 Nd1 O7 77.00(14) 1_545 . ? O9 Nd1 O7 98.02(13) 6_565 . ? O3 Nd1 O7 156.89(13) 5_676 . ? O2 Nd1 O7 72.96(13) . . ? O1 Nd1 O7 84.10(14) . . ? O8 Nd1 O6 77.19(13) 2_656 . ? O4 Nd1 O6 82.36(14) 1_545 . ? O9 Nd1 O6 145.58(13) 6_565 . ? O3 Nd1 O6 135.60(13) 5_676 . ? O2 Nd1 O6 104.92(13) . . ? O1 Nd1 O6 74.48(14) . . ? O7 Nd1 O6 50.92(12) . . ? O1 C1 O2 121.5(5) . . ? O1 C1 C2 118.5(4) . . ? O2 C1 C2 119.9(5) . . ? C3 C2 C7 120.5(5) . . ? C3 C2 C1 121.8(5) . . ? C7 C2 C1 117.7(4) . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 N4 119.2(5) . . ? C5 C4 N4 120.8(5) . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.5(5) . . ? C7 C6 C8 119.3(4) . . ? C5 C6 C8 120.0(4) . . ? C6 C7 C2 119.4(5) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? O4 C8 O3 125.3(5) . . ? O4 C8 C6 116.6(4) . . ? O3 C8 C6 118.1(5) . . ? O5 C9 N4 124.0(5) . . ? O5 C9 C10 118.2(5) . . ? N4 C9 C10 117.8(5) . . ? C11 C10 C14 117.0(5) . . ? C11 C10 C9 125.6(5) . . ? C14 C10 C9 117.5(5) . . ? C12 C11 C10 119.3(6) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N3 C12 C11 123.4(6) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? N3 C13 C14 123.3(6) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.9(6) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? O6 C15 O7 120.7(5) . . ? O6 C15 C16 120.2(5) . . ? O7 C15 C16 119.1(5) . . ? C21 C16 C17 119.7(4) . . ? C21 C16 C15 119.9(4) . . ? C17 C16 C15 120.2(4) . . ? C18 C17 C16 119.5(4) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 120.8(4) . . ? C19 C18 C22 117.6(4) . . ? C17 C18 C22 121.6(4) . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 N2 121.4(4) . . ? C21 C20 N2 118.5(4) . . ? C16 C21 C20 120.5(5) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? O9 C22 O8 124.9(5) . . ? O9 C22 C18 118.1(4) . . ? O8 C22 C18 117.1(5) . . ? O10 C23 N2 124.9(5) . . ? O10 C23 C24 120.2(5) . . ? N2 C23 C24 115.0(5) . . ? C28 C24 C25 118.5(5) . . ? C28 C24 C23 123.0(5) . . ? C25 C24 C23 118.5(5) . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N1 C26 C25 122.4(6) . . ? N1 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N1 C27 C28 122.9(6) . . ? N1 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C24 C28 C27 118.8(6) . . ? C24 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C26 N1 C27 117.8(5) . . ? C26 N1 Ag1 120.4(4) . . ? C27 N1 Ag1 121.0(4) . . ? C23 N2 C20 123.7(5) . . ? C23 N2 H2 118.1 . . ? C20 N2 H2 118.1 . . ? C13 N3 C12 117.2(5) . . ? C13 N3 Ag1 119.1(4) . 5_576 ? C12 N3 Ag1 122.9(4) . 5_576 ? C9 N4 C4 123.7(5) . . ? C9 N4 H4 118.1 . . ? C4 N4 H4 118.1 . . ? C1 O1 Nd1 92.9(3) . . ? C1 O2 Nd1 93.4(3) . . ? C8 O3 Nd1 129.6(3) . 5_676 ? C8 O4 Nd1 139.2(4) . 1_565 ? C15 O6 Nd1 93.5(3) . . ? C15 O7 Nd1 94.7(3) . . ? C22 O8 Nd1 165.3(4) . 2_656 ? C22 O9 Nd1 126.7(3) . 6_566 ? H1WA O1W H1WB 108.2 . . ? H2WB O2W H2WA 113.6 . . ? H3WB O3W H3WA 99.1 . . ? H4WA O4W H4WB 110.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -144.2(5) . . . . ? O2 C1 C2 C3 36.6(7) . . . . ? O1 C1 C2 C7 32.8(7) . . . . ? O2 C1 C2 C7 -146.4(5) . . . . ? C7 C2 C3 C4 -1.8(7) . . . . ? C1 C2 C3 C4 175.2(5) . . . . ? C2 C3 C4 C5 -2.1(8) . . . . ? C2 C3 C4 N4 -177.4(5) . . . . ? C3 C4 C5 C6 3.5(8) . . . . ? N4 C4 C5 C6 178.8(5) . . . . ? C4 C5 C6 C7 -1.1(8) . . . . ? C4 C5 C6 C8 -175.7(5) . . . . ? C5 C6 C7 C2 -2.7(7) . . . . ? C8 C6 C7 C2 171.9(4) . . . . ? C3 C2 C7 C6 4.1(7) . . . . ? C1 C2 C7 C6 -172.9(5) . . . . ? C7 C6 C8 O4 -151.4(5) . . . . ? C5 C6 C8 O4 23.2(7) . . . . ? C7 C6 C8 O3 26.4(7) . . . . ? C5 C6 C8 O3 -159.0(5) . . . . ? O5 C9 C10 C11 149.1(7) . . . . ? N4 C9 C10 C11 -32.2(9) . . . . ? O5 C9 C10 C14 -29.6(9) . . . . ? N4 C9 C10 C14 149.1(6) . . . . ? C14 C10 C11 C12 0.0(9) . . . . ? C9 C10 C11 C12 -178.7(6) . . . . ? C10 C11 C12 N3 -1.7(10) . . . . ? N3 C13 C14 C10 -1.5(9) . . . . ? C11 C10 C14 C13 1.6(8) . . . . ? C9 C10 C14 C13 -179.7(5) . . . . ? O6 C15 C16 C21 173.4(5) . . . . ? O7 C15 C16 C21 -8.3(8) . . . . ? O6 C15 C16 C17 -11.9(8) . . . . ? O7 C15 C16 C17 166.4(5) . . . . ? C21 C16 C17 C18 2.7(8) . . . . ? C15 C16 C17 C18 -172.0(5) . . . . ? C16 C17 C18 C19 0.1(8) . . . . ? C16 C17 C18 C22 -179.1(5) . . . . ? C17 C18 C19 C20 -2.5(8) . . . . ? C22 C18 C19 C20 176.8(5) . . . . ? C18 C19 C20 C21 2.0(8) . . . . ? C18 C19 C20 N2 -175.0(5) . . . . ? C17 C16 C21 C20 -3.1(8) . . . . ? C15 C16 C21 C20 171.6(5) . . . . ? C19 C20 C21 C16 0.8(8) . . . . ? N2 C20 C21 C16 177.9(5) . . . . ? C19 C18 C22 O9 25.1(7) . . . . ? C17 C18 C22 O9 -155.7(5) . . . . ? C19 C18 C22 O8 -154.1(5) . . . . ? C17 C18 C22 O8 25.2(7) . . . . ? O10 C23 C24 C28 145.3(6) . . . . ? N2 C23 C24 C28 -34.2(7) . . . . ? O10 C23 C24 C25 -30.9(8) . . . . ? N2 C23 C24 C25 149.6(5) . . . . ? C28 C24 C25 C26 -1.1(9) . . . . ? C23 C24 C25 C26 175.3(5) . . . . ? C24 C25 C26 N1 -1.2(10) . . . . ? C25 C24 C28 C27 1.6(8) . . . . ? C23 C24 C28 C27 -174.6(5) . . . . ? N1 C27 C28 C24 -0.1(10) . . . . ? C25 C26 N1 C27 2.7(10) . . . . ? C25 C26 N1 Ag1 -167.3(5) . . . . ? C28 C27 N1 C26 -2.1(10) . . . . ? C28 C27 N1 Ag1 167.9(5) . . . . ? Ag1 Ag1 N1 C26 84.9(5) 2_556 . . . ? N3 Ag1 N1 C27 10.2(13) 5_576 . . . ? Ag1 Ag1 N1 C27 -84.8(5) 2_556 . . . ? O10 C23 N2 C20 -4.5(9) . . . . ? C24 C23 N2 C20 175.0(5) . . . . ? C19 C20 N2 C23 -39.3(8) . . . . ? C21 C20 N2 C23 143.6(5) . . . . ? C14 C13 N3 C12 -0.1(9) . . . . ? C14 C13 N3 Ag1 170.0(5) . . . 5_576 ? C11 C12 N3 C13 1.8(10) . . . . ? C11 C12 N3 Ag1 -167.9(5) . . . 5_576 ? O5 C9 N4 C4 5.1(10) . . . . ? C10 C9 N4 C4 -173.5(5) . . . . ? C3 C4 N4 C9 -150.1(5) . . . . ? C5 C4 N4 C9 34.6(8) . . . . ? O2 C1 O1 Nd1 6.2(5) . . . . ? C2 C1 O1 Nd1 -172.9(4) . . . . ? O8 Nd1 O1 C1 159.7(3) 2_656 . . . ? O4 Nd1 O1 C1 -113.6(4) 1_545 . . . ? O9 Nd1 O1 C1 19.5(4) 6_565 . . . ? O3 Nd1 O1 C1 88.3(3) 5_676 . . . ? O2 Nd1 O1 C1 -3.4(3) . . . . ? O7 Nd1 O1 C1 -76.3(3) . . . . ? O6 Nd1 O1 C1 -127.3(3) . . . . ? O1 C1 O2 Nd1 -6.3(5) . . . . ? C2 C1 O2 Nd1 172.9(4) . . . . ? O8 Nd1 O2 C1 -30.9(5) 2_656 . . . ? O4 Nd1 O2 C1 152.5(3) 1_545 . . . ? O9 Nd1 O2 C1 -156.6(3) 6_565 . . . ? O3 Nd1 O2 C1 -76.6(3) 5_676 . . . ? O1 Nd1 O2 C1 3.4(3) . . . . ? O7 Nd1 O2 C1 99.4(3) . . . . ? O6 Nd1 O2 C1 59.2(3) . . . . ? O4 C8 O3 Nd1 -67.7(7) . . . 5_676 ? C6 C8 O3 Nd1 114.7(5) . . . 5_676 ? O3 C8 O4 Nd1 50.1(8) . . . 1_565 ? C6 C8 O4 Nd1 -132.2(4) . . . 1_565 ? O7 C15 O6 Nd1 -4.7(5) . . . . ? C16 C15 O6 Nd1 173.6(4) . . . . ? O8 Nd1 O6 C15 -156.0(3) 2_656 . . . ? O4 Nd1 O6 C15 -76.8(3) 1_545 . . . ? O9 Nd1 O6 C15 -27.3(4) 6_565 . . . ? O3 Nd1 O6 C15 152.4(3) 5_676 . . . ? O2 Nd1 O6 C15 55.2(3) . . . . ? O1 Nd1 O6 C15 97.6(3) . . . . ? O7 Nd1 O6 C15 2.6(3) . . . . ? O6 C15 O7 Nd1 4.7(5) . . . . ? C16 C15 O7 Nd1 -173.5(4) . . . . ? O8 Nd1 O7 C15 23.0(4) 2_656 . . . ? O4 Nd1 O7 C15 88.1(3) 1_545 . . . ? O9 Nd1 O7 C15 160.9(3) 6_565 . . . ? O3 Nd1 O7 C15 -118.8(4) 5_676 . . . ? O2 Nd1 O7 C15 -129.2(3) . . . . ? O1 Nd1 O7 C15 -77.4(3) . . . . ? O6 Nd1 O7 C15 -2.6(3) . . . . ? O9 C22 O8 Nd1 25.8(17) . . . 2_656 ? C18 C22 O8 Nd1 -155.1(12) . . . 2_656 ? O8 C22 O9 Nd1 -10.0(7) . . . 6_566 ? C18 C22 O9 Nd1 171.0(3) . . . 6_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.776 _refine_diff_density_min -2.404 _refine_diff_density_rms 0.144 data_2 _database_code_depnum_ccdc_archive 'CCDC 760886' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag N4 O13 Sm' _chemical_formula_weight 880.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.543(3) _cell_length_b 10.8090(11) _cell_length_c 20.637(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.706(2) _cell_angle_gamma 90.00 _cell_volume 5747.1(11) _cell_formula_units_Z 8 _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 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 2.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5795 _exptl_absorpt_correction_T_max 0.7682 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13921 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5064 _reflns_number_gt 4344 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0737P)^2^+12.3585P] 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 5064 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Ag1 Ag 0.51774(2) 0.94937(8) 0.33570(3) 0.0623(2) Uani 1 1 d . . . Sm1 Sm 0.051271(10) 0.87494(3) 0.468847(13) 0.01556(12) Uani 1 1 d . . . C1 C 0.0955(2) 0.8869(5) 0.3627(3) 0.0233(13) Uani 1 1 d . . . C2 C 0.1191(2) 0.9045(5) 0.3074(3) 0.0220(13) Uani 1 1 d . . . C3 C 0.1725(2) 0.9088(6) 0.3254(3) 0.0257(13) Uani 1 1 d . . . H3 H 0.1938 0.8896 0.3704 0.031 Uiso 1 1 calc R . . C4 C 0.1943(2) 0.9411(6) 0.2774(3) 0.0238(13) Uani 1 1 d . . . C5 C 0.1627(2) 0.9692(5) 0.2107(3) 0.0233(13) Uani 1 1 d . . . H5 H 0.1773 0.9965 0.1790 0.028 Uiso 1 1 calc R . . C6 C 0.1096(2) 0.9571(5) 0.1907(3) 0.0204(12) Uani 1 1 d . . . C7 C 0.0775(2) 0.9792(5) 0.1171(3) 0.0222(13) Uani 1 1 d . . . C8 C 0.0872(2) 0.9243(6) 0.2390(3) 0.0237(13) Uani 1 1 d . . . H8 H 0.0514 0.9157 0.2257 0.028 Uiso 1 1 calc R . . C9 C 0.2758(2) 1.0271(7) 0.2760(3) 0.0318(15) Uani 1 1 d . . . C10 C 0.3336(2) 1.0043(6) 0.2993(3) 0.0273(14) Uani 1 1 d . . . C11 C 0.3550(3) 0.8875(7) 0.3075(3) 0.0364(16) Uani 1 1 d . . . H11 H 0.3342 0.8176 0.3020 0.044 Uiso 1 1 calc R . . C12 C 0.4079(3) 0.8764(7) 0.3240(4) 0.0406(18) Uani 1 1 d . . . H12 H 0.4223 0.7975 0.3301 0.049 Uiso 1 1 calc R . . C13 C 0.4182(3) 1.0858(7) 0.3252(4) 0.0403(17) Uani 1 1 d . . . H13 H 0.4399 1.1544 0.3324 0.048 Uiso 1 1 calc R . . C14 C 0.3660(3) 1.1040(7) 0.3085(4) 0.0367(16) Uani 1 1 d . . . H14 H 0.3526 1.1838 0.3034 0.044 Uiso 1 1 calc R . . C15 C 0.0904(2) 0.6303(5) 0.4914(3) 0.0220(13) Uani 1 1 d . . . C16 C 0.1075(2) 0.5002(5) 0.5069(3) 0.0224(12) Uani 1 1 d . . . C17 C 0.1594(2) 0.4679(5) 0.5338(3) 0.0224(12) Uani 1 1 d . . . H17 H 0.1847 0.5292 0.5456 0.027 Uiso 1 1 calc R . . C18 C 0.1739(2) 0.3447(6) 0.5432(3) 0.0240(13) Uani 1 1 d . . . C19 C 0.1362(2) 0.2513(6) 0.5238(3) 0.0264(13) Uani 1 1 d . . . H19 H 0.1459 0.1684 0.5284 0.032 Uiso 1 1 calc R . . C20 C 0.0832(2) 0.2850(5) 0.4973(3) 0.0222(12) Uani 1 1 d . . . C21 C 0.0429(2) 0.1883(6) 0.4718(3) 0.0250(13) Uani 1 1 d . . . C22 C 0.0696(2) 0.4083(5) 0.4912(3) 0.0212(12) Uani 1 1 d . . . H22 H 0.0347 0.4304 0.4764 0.025 Uiso 1 1 calc R . . C23 C 0.2467(2) 0.2115(6) 0.6080(3) 0.0322(15) Uani 1 1 d . . . C24 C 0.3035(2) 0.1831(6) 0.6250(3) 0.0290(14) Uani 1 1 d . . . C25 C 0.3419(2) 0.2709(7) 0.6349(4) 0.0381(16) Uani 1 1 d . . . H25 H 0.3340 0.3548 0.6300 0.046 Uiso 1 1 calc R . . C26 C 0.3925(3) 0.2302(8) 0.6522(4) 0.0465(19) Uani 1 1 d . . . H26 H 0.4186 0.2892 0.6608 0.056 Uiso 1 1 calc R . . C27 C 0.3692(3) 0.0296(7) 0.6483(3) 0.0378(17) Uani 1 1 d . . . H27 H 0.3782 -0.0537 0.6525 0.045 Uiso 1 1 calc R . . C28 C 0.3180(2) 0.0599(6) 0.6330(3) 0.0337(15) Uani 1 1 d . . . H28 H 0.2933 -0.0016 0.6280 0.040 Uiso 1 1 calc R . . N1 N 0.4390(2) 0.9725(6) 0.3315(3) 0.0420(15) Uani 1 1 d . . . N2 N 0.24891(18) 0.9427(5) 0.2978(2) 0.0281(12) Uani 1 1 d . . . H2 H 0.2661 0.8863 0.3260 0.034 Uiso 1 1 calc R . . N3 N 0.4060(2) 0.1113(6) 0.6573(3) 0.0377(14) Uani 1 1 d . . . N4 N 0.22714(17) 0.3124(5) 0.5695(3) 0.0272(11) Uani 1 1 d . . . H4 H 0.2485 0.3608 0.5602 0.033 Uiso 1 1 calc R . . O1 O 0.04790(16) 0.8700(4) 0.3455(2) 0.0350(11) Uani 1 1 d . . . O2 O 0.12447(16) 0.8908(4) 0.4249(2) 0.0322(11) Uani 1 1 d . . . O3 O 0.03420(15) 0.9262(4) 0.0938(2) 0.0309(10) Uani 1 1 d . . . O4 O 0.09514(16) 1.0468(4) 0.0816(2) 0.0301(10) Uani 1 1 d . . . O5 O 0.25678(18) 1.1161(4) 0.2394(3) 0.0433(13) Uani 1 1 d . . . O6 O 0.05101(17) 0.6525(4) 0.4385(2) 0.0323(11) Uani 1 1 d . . . O7 O 0.11509(15) 0.7158(4) 0.5304(2) 0.0276(9) Uani 1 1 d . . . O8 O -0.00214(15) 0.2120(4) 0.4687(2) 0.0297(10) Uani 1 1 d . . . O9 O 0.05731(17) 0.0875(4) 0.4528(2) 0.0339(10) Uani 1 1 d . . . O10 O 0.2214(2) 0.1408(6) 0.6285(4) 0.072(2) Uani 1 1 d . . . O1W O 0.2194(2) 0.0090(5) 0.4873(3) 0.0555(15) Uani 1 1 d . . . H1WC H 0.1903 -0.0270 0.4686 0.067 Uiso 1 1 d R . . H1WD H 0.2196 0.0433 0.5245 0.067 Uiso 1 1 d R . . O3W O 0.5000 0.1720(7) 0.2500 0.058(2) Uani 1 2 d S . . H3WD H 0.4806 0.2308 0.2534 0.069 Uiso 0.50 1 d PR . . H3WB H 0.5287 0.1746 0.2839 0.069 Uiso 0.50 1 d PR . . O4W O -0.0080(6) 0.1563(15) 0.3054(9) 0.113(6) Uani 0.50 1 d P . . H4WB H -0.0163 0.1112 0.2694 0.135 Uiso 0.50 1 d PR . . H4WC H 0.0007 0.1106 0.3413 0.135 Uiso 0.50 1 d PR . . O2W O 0.21660(18) 0.7670(5) 0.6101(3) 0.0518(14) Uani 1 1 d . . . H2WA H 0.2231 0.8035 0.6488 0.062 Uiso 1 1 d R . . H2WB H 0.1840 0.7573 0.5914 0.062 Uiso 1 1 d 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 Ag1 0.0225(3) 0.1078(6) 0.0596(4) 0.0134(4) 0.0180(3) 0.0180(3) Sm1 0.01367(18) 0.01707(18) 0.01558(18) -0.00003(11) 0.00474(12) 0.00083(10) C1 0.020(3) 0.029(3) 0.023(3) 0.004(2) 0.010(3) 0.005(2) C2 0.022(3) 0.028(3) 0.018(3) 0.004(2) 0.010(2) 0.001(2) C3 0.021(3) 0.037(4) 0.018(3) 0.004(3) 0.006(2) -0.001(3) C4 0.015(3) 0.037(4) 0.019(3) -0.001(3) 0.006(2) 0.000(2) C5 0.021(3) 0.035(3) 0.016(3) -0.001(2) 0.010(2) -0.002(3) C6 0.019(3) 0.024(3) 0.018(3) 0.000(2) 0.007(2) 0.000(2) C7 0.017(3) 0.027(3) 0.020(3) -0.004(2) 0.002(2) 0.004(2) C8 0.016(3) 0.031(3) 0.023(3) 0.004(3) 0.006(2) -0.001(2) C9 0.020(3) 0.050(4) 0.027(3) -0.008(3) 0.010(3) -0.001(3) C10 0.016(3) 0.044(4) 0.022(3) 0.003(3) 0.006(2) 0.001(3) C11 0.027(4) 0.051(5) 0.033(4) 0.004(3) 0.015(3) -0.004(3) C12 0.029(4) 0.050(5) 0.043(4) 0.007(3) 0.014(3) 0.010(3) C13 0.024(3) 0.052(5) 0.045(4) -0.006(4) 0.012(3) -0.006(3) C14 0.026(4) 0.048(4) 0.040(4) -0.001(3) 0.015(3) 0.001(3) C15 0.022(3) 0.023(3) 0.025(3) 0.004(2) 0.013(3) 0.005(2) C16 0.027(3) 0.020(3) 0.020(3) 0.002(2) 0.009(2) 0.003(2) C17 0.022(3) 0.023(3) 0.024(3) 0.000(2) 0.009(2) 0.002(2) C18 0.018(3) 0.031(3) 0.025(3) -0.005(3) 0.010(2) -0.001(2) C19 0.026(3) 0.020(3) 0.036(3) 0.001(3) 0.014(3) 0.007(2) C20 0.020(3) 0.021(3) 0.026(3) 0.002(2) 0.010(2) 0.000(2) C21 0.027(3) 0.027(4) 0.022(3) 0.009(3) 0.011(3) 0.000(3) C22 0.016(3) 0.023(3) 0.026(3) 0.004(2) 0.007(2) 0.005(2) C23 0.022(3) 0.040(4) 0.036(4) 0.009(3) 0.012(3) 0.007(3) C24 0.023(3) 0.038(4) 0.026(3) 0.005(3) 0.009(3) 0.007(3) C25 0.027(3) 0.039(4) 0.050(4) 0.010(3) 0.016(3) 0.009(3) C26 0.026(4) 0.061(5) 0.051(5) 0.006(4) 0.012(3) -0.008(3) C27 0.037(4) 0.042(4) 0.036(4) 0.002(3) 0.015(3) 0.016(3) C28 0.026(3) 0.038(4) 0.034(4) 0.006(3) 0.006(3) 0.004(3) N1 0.022(3) 0.071(5) 0.035(3) 0.004(3) 0.012(2) 0.001(3) N2 0.013(2) 0.049(3) 0.020(3) 0.007(2) 0.004(2) 0.002(2) N3 0.022(3) 0.055(4) 0.037(3) 0.008(3) 0.012(3) 0.012(3) N4 0.017(2) 0.028(3) 0.038(3) 0.006(2) 0.010(2) 0.003(2) O1 0.019(2) 0.063(3) 0.024(2) 0.006(2) 0.0097(18) 0.000(2) O2 0.024(2) 0.056(3) 0.018(2) 0.0008(19) 0.0090(19) -0.002(2) O3 0.017(2) 0.047(3) 0.026(2) -0.006(2) 0.0039(17) -0.002(2) O4 0.026(2) 0.041(3) 0.022(2) 0.0091(19) 0.0056(18) 0.0000(19) O5 0.022(2) 0.050(3) 0.053(3) 0.014(3) 0.008(2) 0.004(2) O6 0.034(3) 0.021(2) 0.029(2) 0.0008(18) -0.005(2) 0.0042(18) O7 0.029(2) 0.017(2) 0.028(2) -0.0041(18) 0.0003(18) 0.0012(17) O8 0.024(2) 0.029(2) 0.038(2) 0.0093(19) 0.0133(19) 0.0002(18) O9 0.037(3) 0.021(2) 0.045(3) -0.002(2) 0.017(2) -0.0046(19) O10 0.026(3) 0.093(5) 0.101(5) 0.068(4) 0.026(3) 0.017(3) O1W 0.042(3) 0.076(4) 0.045(3) -0.004(3) 0.011(2) -0.021(3) O3W 0.065(5) 0.037(4) 0.083(6) 0.000 0.041(5) 0.000 O4W 0.068(10) 0.104(12) 0.129(14) 0.030(10) -0.011(9) -0.034(9) O2W 0.034(3) 0.070(4) 0.044(3) -0.006(3) 0.004(2) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.155(5) 5_666 ? Ag1 N1 2.155(5) . ? Ag1 Ag1 3.3201(14) 2_655 ? Sm1 O3 2.317(4) 2 ? Sm1 O9 2.335(4) 1_565 ? Sm1 O4 2.367(4) 6_576 ? Sm1 O8 2.369(4) 5_566 ? Sm1 O7 2.467(4) . ? Sm1 O6 2.484(4) . ? Sm1 O2 2.493(4) . ? Sm1 O1 2.515(4) . ? C1 O1 1.245(7) . ? C1 O2 1.249(7) . ? C1 C2 1.512(8) . ? C2 C3 1.385(8) . ? C2 C8 1.392(8) . ? C3 C4 1.371(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(8) . ? C4 N2 1.412(7) . ? C5 C6 1.377(8) . ? C5 H5 0.9300 . ? C6 C8 1.392(8) . ? C6 C7 1.482(8) . ? C7 O4 1.249(7) . ? C7 O3 1.254(7) . ? C8 H8 0.9300 . ? C9 O5 1.222(8) . ? C9 N2 1.350(8) . ? C9 C10 1.512(8) . ? C10 C14 1.368(9) . ? C10 C11 1.378(9) . ? C11 C12 1.379(9) . ? C11 H11 0.9300 . ? C12 N1 1.320(9) . ? C12 H12 0.9300 . ? C13 N1 1.339(9) . ? C13 C14 1.368(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.256(7) . ? C15 O6 1.261(7) . ? C15 C16 1.481(8) . ? C16 C17 1.384(8) . ? C16 C22 1.393(8) . ? C17 C18 1.383(8) . ? C17 H17 0.9300 . ? C18 C19 1.401(8) . ? C18 N4 1.417(7) . ? C19 C20 1.413(8) . ? C19 H19 0.9300 . ? C20 C22 1.379(8) . ? C20 C21 1.480(8) . ? C21 O8 1.247(7) . ? C21 O9 1.267(8) . ? C22 H22 0.9300 . ? C23 O10 1.208(8) . ? C23 N4 1.345(8) . ? C23 C24 1.508(8) . ? C24 C25 1.381(9) . ? C24 C28 1.383(10) . ? C25 C26 1.383(9) . ? C25 H25 0.9300 . ? C26 N3 1.331(9) . ? C26 H26 0.9300 . ? C27 N3 1.309(9) . ? C27 C28 1.371(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N2 H2 0.8600 . ? N3 Ag1 2.155(5) 5_666 ? N4 H4 0.8600 . ? O3 Sm1 2.317(4) 2 ? O4 Sm1 2.367(4) 6_575 ? O8 Sm1 2.369(4) 5_566 ? O9 Sm1 2.335(4) 1_545 ? O1W H1WC 0.8501 . ? O1W H1WD 0.8500 . ? O3W H3WD 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WB 0.8499 . ? O4W H4WC 0.8501 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8499 . ? 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 N3 Ag1 N1 168.8(2) 5_666 . ? N3 Ag1 Ag1 89.09(15) 5_666 2_655 ? N1 Ag1 Ag1 92.51(15) . 2_655 ? O3 Sm1 O9 78.17(16) 2 1_565 ? O3 Sm1 O4 121.87(15) 2 6_576 ? O9 Sm1 O4 75.55(16) 1_565 6_576 ? O3 Sm1 O8 74.66(14) 2 5_566 ? O9 Sm1 O8 123.39(15) 1_565 5_566 ? O4 Sm1 O8 78.35(15) 6_576 5_566 ? O3 Sm1 O7 148.49(15) 2 . ? O9 Sm1 O7 133.28(14) 1_565 . ? O4 Sm1 O7 73.73(14) 6_576 . ? O8 Sm1 O7 83.29(14) 5_566 . ? O3 Sm1 O6 100.31(15) 2 . ? O9 Sm1 O6 155.59(17) 1_565 . ? O4 Sm1 O6 123.27(14) 6_576 . ? O8 Sm1 O6 78.56(16) 5_566 . ? O7 Sm1 O6 52.60(13) . . ? O3 Sm1 O2 124.99(14) 2 . ? O9 Sm1 O2 76.92(16) 1_565 . ? O4 Sm1 O2 97.82(14) 6_576 . ? O8 Sm1 O2 156.47(14) 5_566 . ? O7 Sm1 O2 73.42(14) . . ? O6 Sm1 O2 84.57(15) . . ? O3 Sm1 O1 76.91(14) 2 . ? O9 Sm1 O1 81.76(16) 1_565 . ? O4 Sm1 O1 145.70(14) 6_576 . ? O8 Sm1 O1 135.95(14) 5_566 . ? O7 Sm1 O1 105.72(14) . . ? O6 Sm1 O1 74.25(15) . . ? O2 Sm1 O1 51.53(14) . . ? O1 C1 O2 121.6(5) . . ? O1 C1 C2 119.6(5) . . ? O2 C1 C2 118.8(5) . . ? C3 C2 C8 119.8(5) . . ? C3 C2 C1 120.1(5) . . ? C8 C2 C1 119.9(5) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 N2 118.7(5) . . ? C5 C4 N2 121.6(5) . . ? C6 C5 C4 120.5(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C8 120.1(5) . . ? C5 C6 C7 118.6(5) . . ? C8 C6 C7 121.2(5) . . ? O4 C7 O3 123.8(5) . . ? O4 C7 C6 118.6(5) . . ? O3 C7 C6 117.5(5) . . ? C6 C8 C2 119.0(5) . . ? C6 C8 H8 120.5 . . ? C2 C8 H8 120.5 . . ? O5 C9 N2 124.9(6) . . ? O5 C9 C10 119.9(6) . . ? N2 C9 C10 115.2(6) . . ? C14 C10 C11 118.4(6) . . ? C14 C10 C9 118.5(6) . . ? C11 C10 C9 122.9(6) . . ? C12 C11 C10 118.5(6) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N1 C12 C11 123.0(7) . . ? N1 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N1 C13 C14 122.0(7) . . ? N1 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C10 C14 C13 119.8(7) . . ? C10 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? O7 C15 O6 121.3(5) . . ? O7 C15 C16 120.1(5) . . ? O6 C15 C16 118.6(5) . . ? C17 C16 C22 119.8(5) . . ? C17 C16 C15 122.0(5) . . ? C22 C16 C15 118.2(5) . . ? C16 C17 C18 120.3(5) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 N4 119.9(5) . . ? C19 C18 N4 119.6(5) . . ? C18 C19 C20 118.9(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C22 C20 C19 119.7(5) . . ? C22 C20 C21 120.3(5) . . ? C19 C20 C21 119.9(5) . . ? O8 C21 O9 125.1(6) . . ? O8 C21 C20 118.8(6) . . ? O9 C21 C20 116.1(5) . . ? C20 C22 C16 120.7(5) . . ? C20 C22 H22 119.6 . . ? C16 C22 H22 119.6 . . ? O10 C23 N4 124.0(6) . . ? O10 C23 C24 118.0(6) . . ? N4 C23 C24 117.9(5) . . ? C25 C24 C28 118.0(6) . . ? C25 C24 C23 124.9(6) . . ? C28 C24 C23 117.1(6) . . ? C24 C25 C26 118.0(7) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? N3 C26 C25 123.8(7) . . ? N3 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? N3 C27 C28 123.7(7) . . ? N3 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? C27 C28 C24 119.2(6) . . ? C27 C28 H28 120.4 . . ? C24 C28 H28 120.4 . . ? C12 N1 C13 118.1(6) . . ? C12 N1 Ag1 121.0(5) . . ? C13 N1 Ag1 120.0(5) . . ? C9 N2 C4 124.2(5) . . ? C9 N2 H2 117.9 . . ? C4 N2 H2 117.9 . . ? C27 N3 C26 117.3(6) . . ? C27 N3 Ag1 119.5(5) . 5_666 ? C26 N3 Ag1 122.5(5) . 5_666 ? C23 N4 C18 124.8(5) . . ? C23 N4 H4 117.6 . . ? C18 N4 H4 117.6 . . ? C1 O1 Sm1 92.8(3) . . ? C1 O2 Sm1 93.8(4) . . ? C7 O3 Sm1 164.3(4) . 2 ? C7 O4 Sm1 128.0(4) . 6_575 ? C15 O6 Sm1 92.4(3) . . ? C15 O7 Sm1 93.3(3) . . ? C21 O8 Sm1 129.8(4) . 5_566 ? C21 O9 Sm1 139.1(4) . 1_545 ? H1WC O1W H1WD 108.4 . . ? H3WD O3W H3WB 109.6 . . ? H4WB O4W H4WC 109.5 . . ? H2WA O2W H2WB 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -172.4(6) . . . . ? O2 C1 C2 C3 8.3(9) . . . . ? O1 C1 C2 C8 11.6(9) . . . . ? O2 C1 C2 C8 -167.7(6) . . . . ? C8 C2 C3 C4 4.7(10) . . . . ? C1 C2 C3 C4 -171.3(6) . . . . ? C2 C3 C4 C5 -0.2(10) . . . . ? C2 C3 C4 N2 -179.2(6) . . . . ? C3 C4 C5 C6 -4.4(9) . . . . ? N2 C4 C5 C6 174.6(6) . . . . ? C4 C5 C6 C8 4.3(9) . . . . ? C4 C5 C6 C7 -175.4(5) . . . . ? C5 C6 C7 O4 -24.4(8) . . . . ? C8 C6 C7 O4 155.8(6) . . . . ? C5 C6 C7 O3 154.1(6) . . . . ? C8 C6 C7 O3 -25.7(8) . . . . ? C5 C6 C8 C2 0.2(9) . . . . ? C7 C6 C8 C2 -180.0(5) . . . . ? C3 C2 C8 C6 -4.7(9) . . . . ? C1 C2 C8 C6 171.3(5) . . . . ? O5 C9 C10 C14 30.5(9) . . . . ? N2 C9 C10 C14 -150.3(6) . . . . ? O5 C9 C10 C11 -145.3(7) . . . . ? N2 C9 C10 C11 33.9(8) . . . . ? C14 C10 C11 C12 -0.5(9) . . . . ? C9 C10 C11 C12 175.3(6) . . . . ? C10 C11 C12 N1 -0.8(11) . . . . ? C11 C10 C14 C13 0.2(10) . . . . ? C9 C10 C14 C13 -175.8(6) . . . . ? N1 C13 C14 C10 1.5(11) . . . . ? O7 C15 C16 C17 -37.0(8) . . . . ? O6 C15 C16 C17 142.9(6) . . . . ? O7 C15 C16 C22 145.4(6) . . . . ? O6 C15 C16 C22 -34.8(8) . . . . ? C22 C16 C17 C18 1.9(8) . . . . ? C15 C16 C17 C18 -175.7(5) . . . . ? C16 C17 C18 C19 1.9(9) . . . . ? C16 C17 C18 N4 178.7(5) . . . . ? C17 C18 C19 C20 -2.7(9) . . . . ? N4 C18 C19 C20 -179.6(5) . . . . ? C18 C19 C20 C22 -0.2(8) . . . . ? C18 C19 C20 C21 175.6(5) . . . . ? C22 C20 C21 O8 -25.9(8) . . . . ? C19 C20 C21 O8 158.3(5) . . . . ? C22 C20 C21 O9 152.2(6) . . . . ? C19 C20 C21 O9 -23.6(8) . . . . ? C19 C20 C22 C16 4.0(8) . . . . ? C21 C20 C22 C16 -171.8(5) . . . . ? C17 C16 C22 C20 -4.9(8) . . . . ? C15 C16 C22 C20 172.8(5) . . . . ? O10 C23 C24 C25 -149.1(8) . . . . ? N4 C23 C24 C25 32.5(10) . . . . ? O10 C23 C24 C28 29.1(10) . . . . ? N4 C23 C24 C28 -149.3(6) . . . . ? C28 C24 C25 C26 -0.1(9) . . . . ? C23 C24 C25 C26 178.1(6) . . . . ? C24 C25 C26 N3 2.6(11) . . . . ? N3 C27 C28 C24 1.4(10) . . . . ? C25 C24 C28 C27 -1.8(9) . . . . ? C23 C24 C28 C27 179.9(6) . . . . ? C11 C12 N1 C13 2.5(11) . . . . ? C11 C12 N1 Ag1 -166.9(5) . . . . ? C14 C13 N1 C12 -2.8(10) . . . . ? C14 C13 N1 Ag1 166.7(5) . . . . ? N3 Ag1 N1 C12 -13.6(14) 5_666 . . . ? Ag1 Ag1 N1 C12 84.5(5) 2_655 . . . ? N3 Ag1 N1 C13 177.2(10) 5_666 . . . ? Ag1 Ag1 N1 C13 -84.7(5) 2_655 . . . ? O5 C9 N2 C4 4.5(10) . . . . ? C10 C9 N2 C4 -174.7(5) . . . . ? C3 C4 N2 C9 -142.5(6) . . . . ? C5 C4 N2 C9 38.5(9) . . . . ? C28 C27 N3 C26 1.1(10) . . . . ? C28 C27 N3 Ag1 -169.9(5) . . . 5_666 ? C25 C26 N3 C27 -3.1(11) . . . . ? C25 C26 N3 Ag1 167.6(5) . . . 5_666 ? O10 C23 N4 C18 -5.0(11) . . . . ? C24 C23 N4 C18 173.2(5) . . . . ? C17 C18 N4 C23 149.7(6) . . . . ? C19 C18 N4 C23 -33.4(9) . . . . ? O2 C1 O1 Sm1 4.6(6) . . . . ? C2 C1 O1 Sm1 -174.7(5) . . . . ? O3 Sm1 O1 C1 157.0(4) 2 . . . ? O9 Sm1 O1 C1 77.3(4) 1_565 . . . ? O4 Sm1 O1 C1 28.6(5) 6_576 . . . ? O8 Sm1 O1 C1 -152.2(3) 5_566 . . . ? O7 Sm1 O1 C1 -55.5(4) . . . . ? O6 Sm1 O1 C1 -98.2(4) . . . . ? O2 Sm1 O1 C1 -2.5(3) . . . . ? O1 C1 O2 Sm1 -4.7(6) . . . . ? C2 C1 O2 Sm1 174.7(5) . . . . ? O3 Sm1 O2 C1 -22.1(4) 2 . . . ? O9 Sm1 O2 C1 -87.3(4) 1_565 . . . ? O4 Sm1 O2 C1 -160.4(4) 6_576 . . . ? O8 Sm1 O2 C1 120.9(4) 5_566 . . . ? O7 Sm1 O2 C1 129.2(4) . . . . ? O6 Sm1 O2 C1 76.7(4) . . . . ? O1 Sm1 O2 C1 2.5(3) . . . . ? O4 C7 O3 Sm1 -30.2(18) . . . 2 ? C6 C7 O3 Sm1 151.4(12) . . . 2 ? O3 C7 O4 Sm1 11.0(8) . . . 6_575 ? C6 C7 O4 Sm1 -170.6(4) . . . 6_575 ? O7 C15 O6 Sm1 -6.4(6) . . . . ? C16 C15 O6 Sm1 173.7(5) . . . . ? O3 Sm1 O6 C15 -158.6(4) 2 . . . ? O9 Sm1 O6 C15 117.3(4) 1_565 . . . ? O4 Sm1 O6 C15 -19.0(4) 6_576 . . . ? O8 Sm1 O6 C15 -86.8(4) 5_566 . . . ? O7 Sm1 O6 C15 3.5(3) . . . . ? O2 Sm1 O6 C15 76.8(4) . . . . ? O1 Sm1 O6 C15 128.3(4) . . . . ? O6 C15 O7 Sm1 6.5(6) . . . . ? C16 C15 O7 Sm1 -173.7(5) . . . . ? O3 Sm1 O7 C15 31.8(5) 2 . . . ? O9 Sm1 O7 C15 -152.2(3) 1_565 . . . ? O4 Sm1 O7 C15 157.0(4) 6_576 . . . ? O8 Sm1 O7 C15 77.2(4) 5_566 . . . ? O6 Sm1 O7 C15 -3.5(3) . . . . ? O2 Sm1 O7 C15 -99.5(4) . . . . ? O1 Sm1 O7 C15 -58.8(4) . . . . ? O9 C21 O8 Sm1 67.5(8) . . . 5_566 ? C20 C21 O8 Sm1 -114.6(5) . . . 5_566 ? O8 C21 O9 Sm1 -49.9(9) . . . 1_545 ? C20 C21 O9 Sm1 132.1(5) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.268 _refine_diff_density_min -1.932 _refine_diff_density_rms 0.157 data_3 _database_code_depnum_ccdc_archive 'CCDC 760887' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag Eu N4 O13' _chemical_formula_weight 882.33 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' 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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.647(3) _cell_length_b 10.9007(10) _cell_length_c 20.8067(19) _cell_angle_alpha 90.00 _cell_angle_beta 110.5710(10) _cell_angle_gamma 90.00 _cell_volume 5870.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 28.20 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 2.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5717 _exptl_absorpt_correction_T_max 0.7629 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14725 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5445 _reflns_number_gt 4902 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0849P)^2^+45.7812P] 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 5445 _refine_ls_number_parameters 429 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.027 _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 Ag1 Ag 0.48236(2) 1.44818(9) 1.16413(4) 0.0674(3) Uani 1 1 d . . . Eu1 Eu 0.051519(10) 0.62607(2) 0.969070(13) 0.01964(13) Uani 1 1 d . . . C1 C 0.0959(2) 0.6155(5) 0.8613(3) 0.0254(12) Uani 1 1 d . . . C2 C 0.1194(2) 0.5966(6) 0.8067(3) 0.0252(12) Uani 1 1 d . . . C3 C 0.1725(2) 0.5908(7) 0.8251(3) 0.0286(13) Uani 1 1 d . . . H3 H 0.1936 0.6089 0.8698 0.034 Uiso 1 1 calc R . . C4 C 0.1945(2) 0.5579(6) 0.7767(3) 0.0258(12) Uani 1 1 d . . . C5 C 0.1632(2) 0.5308(6) 0.7101(3) 0.0235(12) Uani 1 1 d . . . H5 H 0.1779 0.5045 0.6785 0.028 Uiso 1 1 calc R . . C6 C 0.1101(2) 0.5428(5) 0.6906(3) 0.0214(11) Uani 1 1 d . . . C7 C 0.0876(2) 0.5771(6) 0.7386(3) 0.0252(12) Uani 1 1 d . . . H7 H 0.0520 0.5868 0.7254 0.030 Uiso 1 1 calc R . . C8 C 0.2759(2) 0.4727(7) 0.7752(3) 0.0315(14) Uani 1 1 d . . . C9 C 0.3337(2) 0.4951(6) 0.7984(3) 0.0290(13) Uani 1 1 d . . . C10 C 0.3547(3) 0.6114(7) 0.8070(4) 0.0390(16) Uani 1 1 d . . . H10 H 0.3338 0.6803 0.8018 0.047 Uiso 1 1 calc R . . C11 C 0.4076(3) 0.6232(7) 0.8235(4) 0.0449(19) Uani 1 1 d . . . H11 H 0.4219 0.7015 0.8296 0.054 Uiso 1 1 calc R . . C12 C 0.4181(3) 0.4157(8) 0.8247(4) 0.0445(17) Uani 1 1 d . . . H12 H 0.4399 0.3480 0.8318 0.053 Uiso 1 1 calc R . . C13 C 0.3659(3) 0.3964(7) 0.8079(4) 0.0388(16) Uani 1 1 d . . . H13 H 0.3527 0.3170 0.8031 0.047 Uiso 1 1 calc R . . C14 C 0.0780(2) 0.5203(5) 0.6172(3) 0.0230(11) Uani 1 1 d . . . C15 C 0.0911(2) 0.8717(5) 0.9918(3) 0.0223(12) Uani 1 1 d . . . C16 C 0.1081(2) 1.0017(5) 1.0076(3) 0.0224(11) Uani 1 1 d . . . C17 C 0.0700(2) 1.0923(6) 0.9909(3) 0.0235(11) Uani 1 1 d . . . H17 H 0.0353 1.0707 0.9749 0.028 Uiso 1 1 calc R . . C18 C 0.0845(2) 1.2151(5) 0.9982(3) 0.0225(11) Uani 1 1 d . . . C19 C 0.1369(2) 1.2480(5) 1.0244(3) 0.0265(12) Uani 1 1 d . . . H19 H 0.1465 1.3302 1.0285 0.032 Uiso 1 1 calc R . . C20 C 0.1745(2) 1.1565(6) 1.0443(3) 0.0248(12) Uani 1 1 d . . . C21 C 0.1602(2) 1.0330(5) 1.0348(3) 0.0244(12) Uani 1 1 d . . . H21 H 0.1853 0.9721 1.0467 0.029 Uiso 1 1 calc R . . C22 C 0.2471(2) 1.2884(7) 1.1079(3) 0.0360(15) Uani 1 1 d . . . C23 C 0.3038(2) 1.3165(6) 1.1248(3) 0.0304(13) Uani 1 1 d . . . C24 C 0.3181(3) 1.4381(7) 1.1321(3) 0.0373(15) Uani 1 1 d . . . H24 H 0.2933 1.4988 1.1267 0.045 Uiso 1 1 calc R . . C25 C 0.3692(3) 1.4695(7) 1.1476(4) 0.0415(16) Uani 1 1 d . . . H25 H 0.3780 1.5521 1.1514 0.050 Uiso 1 1 calc R . . C26 C 0.3928(3) 1.2688(8) 1.1521(4) 0.0489(19) Uani 1 1 d . . . H26 H 0.4187 1.2101 1.1604 0.059 Uiso 1 1 calc R . . C27 C 0.3421(3) 1.2291(7) 1.1350(4) 0.0426(17) Uani 1 1 d . . . H27 H 0.3341 1.1459 1.1304 0.051 Uiso 1 1 calc R . . C28 C 0.0440(2) 1.3121(6) 0.9724(3) 0.0261(12) Uani 1 1 d . . . N1 N 0.4387(2) 0.5274(7) 0.8311(3) 0.0470(16) Uani 1 1 d . . . N2 N 0.24913(17) 0.5564(5) 0.7970(2) 0.0304(12) Uani 1 1 d . . . H2 H 0.2663 0.6123 0.8249 0.036 Uiso 1 1 calc R . . N3 N 0.4062(2) 1.3871(6) 1.1573(3) 0.0415(15) Uani 1 1 d . . . N4 N 0.22790(18) 1.1873(5) 1.0702(3) 0.0298(11) Uani 1 1 d . . . H4 H 0.2492 1.1386 1.0613 0.036 Uiso 1 1 calc R . . O1 O 0.12479(17) 0.6120(4) 0.9235(2) 0.0333(10) Uani 1 1 d . . . O2 O 0.04825(17) 0.6309(5) 0.8446(2) 0.0373(12) Uani 1 1 d . . . O3 O 0.03435(16) 0.5717(5) 0.5939(2) 0.0348(10) Uani 1 1 d . . . O4 O 0.09627(16) 0.4512(4) 0.5830(2) 0.0339(10) Uani 1 1 d . . . O5 O 0.25705(18) 0.3848(5) 0.7388(3) 0.0453(13) Uani 1 1 d . . . O6 O 0.11617(16) 0.7867(4) 1.0302(2) 0.0294(9) Uani 1 1 d . . . O7 O 0.05187(17) 0.8496(4) 0.9401(2) 0.0335(10) Uani 1 1 d . . . O8 O -0.00099(15) 1.2879(4) 0.9682(2) 0.0325(10) Uani 1 1 d . . . O9 O 0.05839(18) 1.4116(4) 0.9534(3) 0.0363(10) Uani 1 1 d . . . O10 O 0.2217(2) 1.3590(7) 1.1283(4) 0.080(3) Uani 1 1 d . . . O1W O 0.21743(19) 0.7359(6) 0.1112(3) 0.0539(14) Uani 1 1 d . . . H1WA H 0.2236 0.6982 0.1490 0.065 Uiso 1 1 d R . . H1WB H 0.1850 0.7448 0.0921 0.065 Uiso 1 1 d R . . O2W O 0.2193(2) 0.4901(6) 0.9866(3) 0.0572(15) Uani 1 1 d . . . H2WC H 0.2166 0.4575 1.0223 0.069 Uiso 1 1 d R . . H2WD H 0.1905 0.5199 0.9609 0.069 Uiso 1 1 d R . . O3W O 0.5079(5) 0.1543(15) 0.1932(8) 0.082(5) Uani 0.50 1 d PD . . H3WA H 0.4938 0.0925 0.1690 0.098 Uiso 0.50 1 d PRD . . H3WB H 0.5037 0.2171 0.1676 0.098 Uiso 0.50 1 d PRD . . O4W O 1.0000 0.8275(8) 0.7500 0.063(2) Uani 1 2 d S . . H4WB H 0.9799 0.8016 0.7113 0.076 Uiso 0.50 1 d PR . . H4WA H 0.9912 0.7967 0.7818 0.076 Uiso 0.50 1 d PR . . 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 Ag1 0.0242(3) 0.1196(7) 0.0627(4) -0.0164(4) 0.0208(3) -0.0207(3) Eu1 0.01888(19) 0.0210(2) 0.02021(18) 0.00009(9) 0.00831(13) -0.00088(9) C1 0.022(3) 0.033(3) 0.024(3) -0.006(2) 0.011(2) -0.004(2) C2 0.022(3) 0.037(3) 0.021(3) -0.004(2) 0.012(2) -0.002(2) C3 0.022(3) 0.046(4) 0.017(3) -0.005(3) 0.007(2) -0.003(3) C4 0.014(2) 0.042(4) 0.022(3) 0.000(2) 0.008(2) -0.001(2) C5 0.017(3) 0.038(3) 0.017(2) 0.000(2) 0.008(2) 0.003(2) C6 0.019(3) 0.027(3) 0.018(3) -0.002(2) 0.006(2) 0.001(2) C7 0.016(2) 0.035(3) 0.024(3) -0.002(2) 0.007(2) 0.003(2) C8 0.022(3) 0.051(4) 0.025(3) 0.005(3) 0.011(2) 0.003(3) C9 0.018(3) 0.050(4) 0.020(3) -0.003(3) 0.008(2) -0.004(3) C10 0.026(3) 0.061(5) 0.036(4) -0.008(3) 0.018(3) -0.001(3) C11 0.028(4) 0.065(6) 0.046(4) -0.014(3) 0.019(3) -0.014(3) C12 0.029(3) 0.056(5) 0.051(4) 0.004(4) 0.017(3) 0.006(3) C13 0.025(3) 0.054(4) 0.041(4) 0.002(3) 0.016(3) 0.001(3) C14 0.017(3) 0.031(3) 0.020(3) 0.004(2) 0.006(2) -0.001(2) C15 0.021(3) 0.024(3) 0.025(3) 0.001(2) 0.012(2) -0.001(2) C16 0.027(3) 0.020(3) 0.024(3) -0.001(2) 0.013(2) -0.005(2) C17 0.022(3) 0.024(3) 0.029(3) -0.004(2) 0.014(2) -0.008(2) C18 0.020(3) 0.021(3) 0.029(3) -0.002(2) 0.012(2) 0.002(2) C19 0.027(3) 0.022(3) 0.034(3) -0.001(2) 0.016(2) -0.008(2) C20 0.021(3) 0.029(3) 0.027(3) -0.003(2) 0.012(2) -0.004(2) C21 0.024(3) 0.025(3) 0.025(3) -0.001(2) 0.010(2) 0.000(2) C22 0.026(3) 0.048(4) 0.040(3) -0.014(3) 0.018(3) -0.009(3) C23 0.025(3) 0.041(4) 0.029(3) -0.009(3) 0.014(2) -0.008(3) C24 0.031(3) 0.040(4) 0.039(4) -0.005(3) 0.009(3) -0.002(3) C25 0.037(4) 0.047(4) 0.042(4) -0.002(3) 0.016(3) -0.016(3) C26 0.027(3) 0.063(5) 0.057(5) -0.010(4) 0.015(3) 0.006(3) C27 0.034(3) 0.038(4) 0.058(4) -0.011(3) 0.018(3) -0.008(3) C28 0.029(3) 0.024(3) 0.029(3) -0.009(2) 0.015(2) 0.003(2) N1 0.021(3) 0.084(5) 0.037(3) -0.006(3) 0.013(2) -0.005(3) N2 0.014(2) 0.056(4) 0.022(2) -0.007(2) 0.0067(19) -0.005(2) N3 0.024(3) 0.067(4) 0.036(3) -0.012(3) 0.014(2) -0.016(3) N4 0.019(2) 0.032(3) 0.039(3) -0.008(2) 0.011(2) -0.005(2) O1 0.026(2) 0.055(3) 0.022(2) -0.0010(19) 0.0125(18) 0.0002(19) O2 0.024(2) 0.066(4) 0.024(2) -0.0055(19) 0.0115(18) -0.001(2) O3 0.024(2) 0.050(3) 0.029(2) 0.007(2) 0.0064(17) 0.001(2) O4 0.031(2) 0.046(3) 0.023(2) -0.0096(19) 0.0078(17) 0.0011(19) O5 0.025(2) 0.051(3) 0.055(3) -0.013(2) 0.008(2) -0.002(2) O6 0.031(2) 0.019(2) 0.032(2) 0.0014(17) 0.0025(17) -0.0029(17) O7 0.036(2) 0.020(2) 0.032(2) 0.0008(18) -0.0027(19) -0.0043(18) O8 0.025(2) 0.035(2) 0.041(2) -0.0111(19) 0.0154(18) 0.0014(18) O9 0.043(3) 0.019(2) 0.052(3) 0.000(2) 0.023(2) 0.0052(19) O10 0.027(3) 0.103(5) 0.115(6) -0.080(5) 0.032(3) -0.019(3) O1W 0.035(3) 0.076(4) 0.044(3) 0.004(3) 0.006(2) 0.002(3) O2W 0.047(3) 0.074(4) 0.047(3) -0.001(3) 0.012(2) 0.015(3) O3W 0.055(8) 0.093(10) 0.079(10) -0.020(8) 0.002(7) 0.029(7) O4W 0.079(6) 0.047(5) 0.080(6) 0.000 0.049(5) 0.000 _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 Ag1 N3 2.165(5) . ? Ag1 N1 2.166(5) 5_677 ? Ag1 Ag1 3.3573(14) 2_657 ? Eu1 O3 2.349(4) 2_556 ? Eu1 O9 2.377(5) 1_545 ? Eu1 O4 2.408(4) 6_566 ? Eu1 O8 2.411(4) 5_577 ? Eu1 O6 2.506(4) . ? Eu1 O7 2.511(4) . ? Eu1 O1 2.524(4) . ? Eu1 O2 2.560(4) . ? C1 O2 1.251(7) . ? C1 O1 1.260(7) . ? C1 C2 1.508(8) . ? C2 C3 1.383(8) . ? C2 C7 1.396(8) . ? C3 C4 1.392(8) . ? C3 H3 0.9300 . ? C4 C5 1.383(8) . ? C4 N2 1.418(7) . ? C5 C6 1.387(7) . ? C5 H5 0.9300 . ? C6 C7 1.401(8) . ? C6 C14 1.492(7) . ? C7 H7 0.9300 . ? C8 O5 1.219(8) . ? C8 N2 1.349(8) . ? C8 C9 1.518(8) . ? C9 C13 1.365(10) . ? C9 C10 1.380(10) . ? C10 C11 1.386(9) . ? C10 H10 0.9300 . ? C11 N1 1.327(10) . ? C11 H11 0.9300 . ? C12 N1 1.330(11) . ? C12 C13 1.378(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4 1.257(7) . ? C14 O3 1.263(7) . ? C15 O7 1.253(7) . ? C15 O6 1.261(7) . ? C15 C16 1.494(8) . ? C16 C17 1.394(8) . ? C16 C21 1.393(8) . ? C17 C18 1.390(8) . ? C17 H17 0.9300 . ? C18 C19 1.404(8) . ? C18 C28 1.496(8) . ? C19 C20 1.394(9) . ? C19 H19 0.9300 . ? C20 C21 1.398(8) . ? C20 N4 1.423(7) . ? C21 H21 0.9300 . ? C22 O10 1.215(8) . ? C22 N4 1.349(8) . ? C22 C23 1.512(8) . ? C23 C24 1.376(10) . ? C23 C27 1.386(10) . ? C24 C25 1.378(9) . ? C24 H24 0.9300 . ? C25 N3 1.322(10) . ? C25 H25 0.9300 . ? C26 N3 1.336(11) . ? C26 C27 1.387(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O8 1.245(7) . ? C28 O9 1.266(9) . ? N1 Ag1 2.166(5) 5_677 ? N2 H2 0.8600 . ? N4 H4 0.8600 . ? O3 Eu1 2.349(4) 2_556 ? O4 Eu1 2.408(4) 6_565 ? O8 Eu1 2.411(4) 5_577 ? O9 Eu1 2.377(5) 1_565 ? O1W H1WA 0.8498 . ? O1W H1WB 0.8497 . ? O2W H2WC 0.8501 . ? O2W H2WD 0.8501 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WB 0.8500 . ? O4W H4WA 0.8500 . ? 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 N3 Ag1 N1 169.1(3) . 5_677 ? N3 Ag1 Ag1 88.97(16) . 2_657 ? N1 Ag1 Ag1 92.28(16) 5_677 2_657 ? O3 Eu1 O9 77.83(17) 2_556 1_545 ? O3 Eu1 O4 121.97(16) 2_556 6_566 ? O9 Eu1 O4 75.70(16) 1_545 6_566 ? O3 Eu1 O8 74.67(15) 2_556 5_577 ? O9 Eu1 O8 123.12(16) 1_545 5_577 ? O4 Eu1 O8 78.38(15) 6_566 5_577 ? O3 Eu1 O6 149.34(15) 2_556 . ? O9 Eu1 O6 132.80(15) 1_545 . ? O4 Eu1 O6 73.53(14) 6_566 . ? O8 Eu1 O6 84.20(15) 5_577 . ? O3 Eu1 O7 101.51(16) 2_556 . ? O9 Eu1 O7 156.05(17) 1_545 . ? O4 Eu1 O7 122.15(15) 6_566 . ? O8 Eu1 O7 78.73(16) 5_577 . ? O6 Eu1 O7 51.82(13) . . ? O3 Eu1 O1 124.23(14) 2_556 . ? O9 Eu1 O1 77.01(16) 1_545 . ? O4 Eu1 O1 98.38(15) 6_566 . ? O8 Eu1 O1 157.00(15) 5_577 . ? O6 Eu1 O1 73.13(15) . . ? O7 Eu1 O1 84.10(16) . . ? O3 Eu1 O2 76.80(15) 2_556 . ? O9 Eu1 O2 81.80(16) 1_545 . ? O4 Eu1 O2 145.73(15) 6_566 . ? O8 Eu1 O2 135.89(15) 5_577 . ? O6 Eu1 O2 105.35(14) . . ? O7 Eu1 O2 74.85(15) . . ? O1 Eu1 O2 50.90(14) . . ? O3 Eu1 Eu1 51.87(12) 2_556 5_567 ? O9 Eu1 Eu1 61.56(12) 1_545 5_567 ? O4 Eu1 Eu1 70.11(10) 6_566 5_567 ? O8 Eu1 Eu1 62.19(11) 5_577 5_567 ? O6 Eu1 Eu1 134.24(10) . 5_567 ? O7 Eu1 Eu1 136.38(11) . 5_567 ? O1 Eu1 Eu1 138.49(11) . 5_567 ? O2 Eu1 Eu1 120.36(11) . 5_567 ? O2 C1 O1 121.0(5) . . ? O2 C1 C2 120.0(5) . . ? O1 C1 C2 119.1(5) . . ? C3 C2 C7 120.2(5) . . ? C3 C2 C1 119.6(5) . . ? C7 C2 C1 120.0(5) . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 N2 121.3(5) . . ? C3 C4 N2 118.6(5) . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.4(5) . . ? C5 C6 C14 118.2(5) . . ? C7 C6 C14 121.5(5) . . ? C2 C7 C6 119.0(5) . . ? C2 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? O5 C8 N2 125.1(6) . . ? O5 C8 C9 119.8(6) . . ? N2 C8 C9 115.1(6) . . ? C13 C9 C10 118.9(6) . . ? C13 C9 C8 118.6(6) . . ? C10 C9 C8 122.4(6) . . ? C9 C10 C11 118.4(7) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? N1 C11 C10 122.7(7) . . ? N1 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? N1 C12 C13 122.6(7) . . ? N1 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C9 C13 C12 119.2(7) . . ? C9 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? O4 C14 O3 124.6(5) . . ? O4 C14 C6 117.8(5) . . ? O3 C14 C6 117.6(5) . . ? O7 C15 O6 121.4(5) . . ? O7 C15 C16 118.8(5) . . ? O6 C15 C16 119.8(5) . . ? C17 C16 C21 120.7(5) . . ? C17 C16 C15 117.8(5) . . ? C21 C16 C15 121.5(5) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 C28 119.4(5) . . ? C19 C18 C28 120.0(5) . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.1(5) . . ? C19 C20 N4 120.7(5) . . ? C21 C20 N4 119.1(5) . . ? C16 C21 C20 119.7(5) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? O10 C22 N4 124.3(6) . . ? O10 C22 C23 118.0(6) . . ? N4 C22 C23 117.6(5) . . ? C24 C23 C27 118.1(6) . . ? C24 C23 C22 117.0(6) . . ? C27 C23 C22 124.8(6) . . ? C23 C24 C25 119.7(7) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N3 C25 C24 122.9(7) . . ? N3 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N3 C26 C27 123.3(7) . . ? N3 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C23 118.3(7) . . ? C26 C27 H27 120.9 . . ? C23 C27 H27 120.9 . . ? O8 C28 O9 125.2(6) . . ? O8 C28 C18 118.6(6) . . ? O9 C28 C18 116.1(5) . . ? C11 N1 C12 118.2(6) . . ? C11 N1 Ag1 120.6(5) . 5_677 ? C12 N1 Ag1 120.4(5) . 5_677 ? C8 N2 C4 124.1(5) . . ? C8 N2 H2 118.0 . . ? C4 N2 H2 118.0 . . ? C25 N3 C26 117.7(6) . . ? C25 N3 Ag1 119.0(5) . . ? C26 N3 Ag1 122.6(5) . . ? C22 N4 C20 123.8(5) . . ? C22 N4 H4 118.1 . . ? C20 N4 H4 118.1 . . ? C1 O1 Eu1 94.7(3) . . ? C1 O2 Eu1 93.2(4) . . ? C14 O3 Eu1 165.6(4) . 2_556 ? C14 O4 Eu1 126.7(4) . 6_565 ? C15 O6 Eu1 93.2(3) . . ? C15 O7 Eu1 93.1(3) . . ? C28 O8 Eu1 129.4(4) . 5_577 ? C28 O9 Eu1 138.7(4) . 1_565 ? H1WA O1W H1WB 108.8 . . ? H2WC O2W H2WD 111.1 . . ? H3WA O3W H3WB 109.5 . . ? H4WB O4W H4WA 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 174.1(6) . . . . ? O1 C1 C2 C3 -7.8(9) . . . . ? O2 C1 C2 C7 -10.0(9) . . . . ? O1 C1 C2 C7 168.0(6) . . . . ? C7 C2 C3 C4 -4.0(10) . . . . ? C1 C2 C3 C4 171.8(6) . . . . ? C2 C3 C4 C5 -0.1(10) . . . . ? C2 C3 C4 N2 178.2(6) . . . . ? C3 C4 C5 C6 3.5(9) . . . . ? N2 C4 C5 C6 -174.8(6) . . . . ? C4 C5 C6 C7 -2.8(9) . . . . ? C4 C5 C6 C14 176.2(5) . . . . ? C3 C2 C7 C6 4.7(10) . . . . ? C1 C2 C7 C6 -171.1(6) . . . . ? C5 C6 C7 C2 -1.3(9) . . . . ? C14 C6 C7 C2 179.8(6) . . . . ? O5 C8 C9 C13 -31.0(9) . . . . ? N2 C8 C9 C13 149.8(6) . . . . ? O5 C8 C9 C10 145.7(7) . . . . ? N2 C8 C9 C10 -33.4(8) . . . . ? C13 C9 C10 C11 1.3(10) . . . . ? C8 C9 C10 C11 -175.4(6) . . . . ? C9 C10 C11 N1 0.3(11) . . . . ? C10 C9 C13 C12 -1.0(10) . . . . ? C8 C9 C13 C12 175.9(6) . . . . ? N1 C12 C13 C9 -1.1(11) . . . . ? C5 C6 C14 O4 25.4(8) . . . . ? C7 C6 C14 O4 -155.7(6) . . . . ? C5 C6 C14 O3 -154.9(6) . . . . ? C7 C6 C14 O3 24.1(8) . . . . ? O7 C15 C16 C17 32.8(8) . . . . ? O6 C15 C16 C17 -147.3(5) . . . . ? O7 C15 C16 C21 -143.9(6) . . . . ? O6 C15 C16 C21 36.0(8) . . . . ? C21 C16 C17 C18 3.3(8) . . . . ? C15 C16 C17 C18 -173.4(5) . . . . ? C16 C17 C18 C19 -2.1(8) . . . . ? C16 C17 C18 C28 172.7(5) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C28 C18 C19 C20 -176.0(5) . . . . ? C18 C19 C20 C21 3.3(9) . . . . ? C18 C19 C20 N4 179.2(5) . . . . ? C17 C16 C21 C20 -1.2(8) . . . . ? C15 C16 C21 C20 175.4(5) . . . . ? C19 C20 C21 C16 -2.1(8) . . . . ? N4 C20 C21 C16 -178.1(5) . . . . ? O10 C22 C23 C24 -29.5(10) . . . . ? N4 C22 C23 C24 149.4(6) . . . . ? O10 C22 C23 C27 148.7(8) . . . . ? N4 C22 C23 C27 -32.3(10) . . . . ? C27 C23 C24 C25 1.5(10) . . . . ? C22 C23 C24 C25 179.9(6) . . . . ? C23 C24 C25 N3 -1.4(11) . . . . ? N3 C26 C27 C23 -2.0(12) . . . . ? C24 C23 C27 C26 0.1(10) . . . . ? C22 C23 C27 C26 -178.1(7) . . . . ? C17 C18 C28 O8 25.7(8) . . . . ? C19 C18 C28 O8 -159.4(5) . . . . ? C17 C18 C28 O9 -151.1(5) . . . . ? C19 C18 C28 O9 23.7(8) . . . . ? C10 C11 N1 C12 -2.3(11) . . . . ? C10 C11 N1 Ag1 167.2(6) . . . 5_677 ? C13 C12 N1 C11 2.7(11) . . . . ? C13 C12 N1 Ag1 -166.9(6) . . . 5_677 ? O5 C8 N2 C4 -4.3(10) . . . . ? C9 C8 N2 C4 174.8(5) . . . . ? C5 C4 N2 C8 -39.0(9) . . . . ? C3 C4 N2 C8 142.7(6) . . . . ? C24 C25 N3 C26 -0.5(11) . . . . ? C24 C25 N3 Ag1 169.7(5) . . . . ? C27 C26 N3 C25 2.2(12) . . . . ? C27 C26 N3 Ag1 -167.6(6) . . . . ? N1 Ag1 N3 C25 -167.3(10) 5_677 . . . ? Ag1 Ag1 N3 C25 96.0(5) 2_657 . . . ? N1 Ag1 N3 C26 2.4(16) 5_677 . . . ? Ag1 Ag1 N3 C26 -94.4(6) 2_657 . . . ? O10 C22 N4 C20 5.9(12) . . . . ? C23 C22 N4 C20 -173.0(6) . . . . ? C19 C20 N4 C22 33.5(9) . . . . ? C21 C20 N4 C22 -150.6(6) . . . . ? O2 C1 O1 Eu1 4.4(6) . . . . ? C2 C1 O1 Eu1 -173.7(5) . . . . ? O3 Eu1 O1 C1 22.3(4) 2_556 . . . ? O9 Eu1 O1 C1 87.6(4) 1_545 . . . ? O4 Eu1 O1 C1 160.7(4) 6_566 . . . ? O8 Eu1 O1 C1 -119.3(4) 5_577 . . . ? O6 Eu1 O1 C1 -129.4(4) . . . . ? O7 Eu1 O1 C1 -77.6(4) . . . . ? O2 Eu1 O1 C1 -2.3(3) . . . . ? Eu1 Eu1 O1 C1 91.3(4) 5_567 . . . ? O1 C1 O2 Eu1 -4.3(6) . . . . ? C2 C1 O2 Eu1 173.7(5) . . . . ? O3 Eu1 O2 C1 -156.9(4) 2_556 . . . ? O9 Eu1 O2 C1 -77.5(4) 1_545 . . . ? O4 Eu1 O2 C1 -28.4(5) 6_566 . . . ? O8 Eu1 O2 C1 152.3(3) 5_577 . . . ? O6 Eu1 O2 C1 54.7(4) . . . . ? O7 Eu1 O2 C1 97.1(4) . . . . ? O1 Eu1 O2 C1 2.4(3) . . . . ? Eu1 Eu1 O2 C1 -127.6(3) 5_567 . . . ? O4 C14 O3 Eu1 25(2) . . . 2_556 ? C6 C14 O3 Eu1 -155.1(13) . . . 2_556 ? O3 C14 O4 Eu1 -8.4(9) . . . 6_565 ? C6 C14 O4 Eu1 171.4(4) . . . 6_565 ? O7 C15 O6 Eu1 -6.8(6) . . . . ? C16 C15 O6 Eu1 173.3(4) . . . . ? O3 Eu1 O6 C15 -30.4(5) 2_556 . . . ? O9 Eu1 O6 C15 152.6(3) 1_545 . . . ? O4 Eu1 O6 C15 -156.1(4) 6_566 . . . ? O8 Eu1 O6 C15 -76.5(3) 5_577 . . . ? O7 Eu1 O6 C15 3.7(3) . . . . ? O1 Eu1 O6 C15 99.5(4) . . . . ? O2 Eu1 O6 C15 59.6(4) . . . . ? Eu1 Eu1 O6 C15 -117.6(3) 5_567 . . . ? O6 C15 O7 Eu1 6.8(6) . . . . ? C16 C15 O7 Eu1 -173.3(4) . . . . ? O3 Eu1 O7 C15 159.4(3) 2_556 . . . ? O9 Eu1 O7 C15 -114.7(5) 1_545 . . . ? O4 Eu1 O7 C15 19.4(4) 6_566 . . . ? O8 Eu1 O7 C15 87.8(4) 5_577 . . . ? O6 Eu1 O7 C15 -3.7(3) . . . . ? O1 Eu1 O7 C15 -76.8(4) . . . . ? O2 Eu1 O7 C15 -127.9(4) . . . . ? Eu1 Eu1 O7 C15 113.8(3) 5_567 . . . ? O9 C28 O8 Eu1 -69.1(8) . . . 5_577 ? C18 C28 O8 Eu1 114.3(5) . . . 5_577 ? O8 C28 O9 Eu1 50.8(9) . . . 1_565 ? C18 C28 O9 Eu1 -132.6(5) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.548 _refine_diff_density_min -1.877 _refine_diff_density_rms 0.199 data_4 _database_code_depnum_ccdc_archive 'CCDC 760888' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag Gd N4 O13' _chemical_formula_weight 887.62 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.607(2) _cell_length_b 10.7939(10) _cell_length_c 20.6785(19) _cell_angle_alpha 90.00 _cell_angle_beta 110.8280(10) _cell_angle_gamma 90.00 _cell_volume 5759.2(9) _cell_formula_units_Z 8 _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 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 3.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5542 _exptl_absorpt_correction_T_max 0.7117 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14750 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5352 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0979P)^2^+13.8608P] 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 5352 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.01773(2) 0.55007(7) 0.33561(3) 0.0554(2) Uani 1 1 d . . . Gd1 Gd 0.551125(9) 0.62445(2) 0.468798(12) 0.01353(14) Uani 1 1 d . . . C1 C 0.5959(2) 0.6126(5) 0.3630(3) 0.0220(12) Uani 1 1 d . . . C2 C 0.6190(2) 0.5947(6) 0.3081(3) 0.0220(11) Uani 1 1 d . . . C3 C 0.6723(2) 0.5904(6) 0.3264(3) 0.0234(11) Uani 1 1 d . . . H3 H 0.6936 0.6093 0.3715 0.028 Uiso 1 1 calc R . . C4 C 0.6943(2) 0.5582(5) 0.2778(3) 0.0221(11) Uani 1 1 d . . . C5 C 0.6626(2) 0.5312(5) 0.2104(3) 0.0190(11) Uani 1 1 d . . . H5 H 0.6771 0.5058 0.1783 0.023 Uiso 1 1 calc R . . C6 C 0.6097(2) 0.5421(5) 0.1912(3) 0.0188(11) Uani 1 1 d . . . C7 C 0.5869(2) 0.5738(5) 0.2395(3) 0.0213(11) Uani 1 1 d . . . H7 H 0.5511 0.5809 0.2263 0.026 Uiso 1 1 calc R . . C8 C 0.57653(19) 0.5219(5) 0.1161(3) 0.0188(11) Uani 1 1 d . . . C9 C 0.7758(2) 0.4737(6) 0.2763(3) 0.0277(13) Uani 1 1 d . . . C10 C 0.8332(2) 0.4956(6) 0.2992(3) 0.0258(12) Uani 1 1 d . . . C11 C 0.8547(3) 0.6129(6) 0.3074(4) 0.0325(15) Uani 1 1 d . . . H11 H 0.8339 0.6828 0.3022 0.039 Uiso 1 1 calc R . . C12 C 0.9074(3) 0.6243(6) 0.3233(4) 0.0376(18) Uani 1 1 d . . . H12 H 0.9215 0.7035 0.3286 0.045 Uiso 1 1 calc R . . C13 C 0.9184(2) 0.4135(7) 0.3258(4) 0.0372(15) Uani 1 1 d . . . H13 H 0.9402 0.3450 0.3334 0.045 Uiso 1 1 calc R . . C14 C 0.8658(2) 0.3947(6) 0.3091(4) 0.0329(14) Uani 1 1 d . . . H14 H 0.8525 0.3147 0.3046 0.039 Uiso 1 1 calc R . . C15 C 0.5898(2) 0.8677(4) 0.4913(3) 0.0198(12) Uani 1 1 d . . . C16 C 0.6070(2) 0.9991(5) 0.5069(3) 0.0206(11) Uani 1 1 d . . . C17 C 0.5684(2) 1.0914(5) 0.4906(3) 0.0208(11) Uani 1 1 d . . . H17 H 0.5335 1.0697 0.4754 0.025 Uiso 1 1 calc R . . C18 C 0.5831(2) 1.2154(5) 0.4976(3) 0.0200(11) Uani 1 1 d . . . C19 C 0.6349(2) 1.2478(5) 0.5231(3) 0.0227(11) Uani 1 1 d . . . H19 H 0.6443 1.3309 0.5270 0.027 Uiso 1 1 calc R . . C20 C 0.6733(2) 1.1560(5) 0.5431(3) 0.0218(11) Uani 1 1 d . . . C21 C 0.6590(2) 1.0310(5) 0.5336(3) 0.0207(11) Uani 1 1 d . . . H21 H 0.6844 0.9696 0.5451 0.025 Uiso 1 1 calc R . . C22 C 0.5426(2) 1.3137(5) 0.4718(3) 0.0204(11) Uani 1 1 d . . . C23 C 0.7467(2) 1.2883(6) 0.6074(3) 0.0292(13) Uani 1 1 d . . . C24 C 0.8029(2) 1.3173(6) 0.6244(3) 0.0248(12) Uani 1 1 d . . . C25 C 0.8177(2) 1.4413(6) 0.6329(3) 0.0315(14) Uani 1 1 d . . . H25 H 0.7933 1.5032 0.6284 0.038 Uiso 1 1 calc R . . C26 C 0.8688(2) 1.4707(6) 0.6482(3) 0.0327(14) Uani 1 1 d . . . H26 H 0.8780 1.5541 0.6522 0.039 Uiso 1 1 calc R . . C27 C 0.8919(2) 1.2690(7) 0.6513(4) 0.0394(16) Uani 1 1 d . . . H27 H 0.9175 1.2091 0.6587 0.047 Uiso 1 1 calc R . . C28 C 0.8416(3) 1.2304(6) 0.6344(4) 0.0372(15) Uani 1 1 d . . . H28 H 0.8336 1.1464 0.6297 0.045 Uiso 1 1 calc R . . N1 N 0.93922(19) 0.5278(6) 0.3314(3) 0.0377(13) Uani 1 1 d . . . N2 N 0.74896(17) 0.5563(5) 0.2982(2) 0.0260(11) Uani 1 1 d . . . H2 H 0.7662 0.6124 0.3267 0.031 Uiso 1 1 calc R . . N3 N 0.9060(2) 1.3880(5) 0.6576(3) 0.0336(13) Uani 1 1 d . . . N4 N 0.72720(17) 1.1879(4) 0.5690(3) 0.0260(10) Uani 1 1 d . . . H4 H 0.7484 1.1395 0.5592 0.031 Uiso 1 1 calc R . . O1 O 0.54727(17) 0.6298(4) 0.3458(2) 0.0315(11) Uani 1 1 d . . . O2 O 0.62451(16) 0.6083(4) 0.4262(2) 0.0291(10) Uani 1 1 d . . . O3 O 0.53404(14) 0.5763(4) 0.09398(19) 0.0286(9) Uani 1 1 d . . . O4 O 0.59457(16) 0.4538(4) 0.0811(2) 0.0280(9) Uani 1 1 d . . . O5 O 0.75684(19) 0.3838(4) 0.2395(3) 0.0405(12) Uani 1 1 d . . . O6 O 0.61412(15) 0.7821(3) 0.5304(2) 0.0265(9) Uani 1 1 d . . . O7 O 0.55035(16) 0.8458(4) 0.4381(2) 0.0281(9) Uani 1 1 d . . . O8 O 0.49705(14) 1.2880(4) 0.4690(2) 0.0278(9) Uani 1 1 d . . . O9 O 0.55587(16) 1.4118(4) 0.4526(2) 0.0298(9) Uani 1 1 d . . . O10 O 0.7208(2) 1.3601(6) 0.6282(4) 0.0628(19) Uani 1 1 d . . . O1W O 0.71661(19) 0.7322(5) 0.6092(3) 0.0511(13) Uani 1 1 d . . . H1WA H 0.6838 0.7363 0.5907 0.061 Uiso 1 1 d R . . H1WB H 0.7266 0.6804 0.6423 0.061 Uiso 1 1 d R . . O2W O 0.7189(2) 0.4895(6) 0.4866(3) 0.0534(14) Uani 1 1 d . . . H2WA H 0.6899 0.5258 0.4680 0.064 Uiso 1 1 d R . . H2WB H 0.7192 0.4554 0.5239 0.064 Uiso 1 1 d R . . O3W O 0.5000 0.8278(7) 0.2500 0.056(2) Uani 1 2 d S . . H3WA H 0.5167 0.7815 0.2838 0.067 Uiso 0.50 1 d PR . . H3WB H 0.4833 0.7815 0.2162 0.067 Uiso 0.50 1 d PR . . O4W O 0.7786(6) 0.6870(11) 0.5310(9) 0.090(5) Uani 0.50 1 d P . . H4WA H 0.7633 0.6209 0.5120 0.108 Uiso 0.50 1 d PR . . H4WB H 0.7634 0.7138 0.5575 0.108 Uiso 0.50 1 d PR . . 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 Ag1 0.0199(3) 0.0933(5) 0.0549(4) -0.0116(3) 0.0158(3) -0.0156(3) Gd1 0.01202(19) 0.0139(2) 0.01412(19) 0.00023(8) 0.00399(13) -0.00072(8) C1 0.017(3) 0.028(3) 0.023(3) -0.002(2) 0.009(2) -0.002(2) C2 0.019(3) 0.029(3) 0.020(3) -0.004(2) 0.009(2) -0.004(2) C3 0.016(3) 0.039(3) 0.013(3) -0.003(3) 0.004(2) -0.001(2) C4 0.014(3) 0.031(3) 0.020(3) -0.002(2) 0.006(2) -0.003(2) C5 0.014(3) 0.029(3) 0.013(2) 0.000(2) 0.003(2) 0.003(2) C6 0.018(3) 0.021(3) 0.016(3) -0.001(2) 0.005(2) 0.001(2) C7 0.017(3) 0.021(3) 0.026(3) -0.001(2) 0.008(2) -0.001(2) C8 0.013(3) 0.027(3) 0.013(2) 0.005(2) 0.0010(19) -0.004(2) C9 0.018(3) 0.040(3) 0.021(3) 0.003(3) 0.003(2) 0.003(2) C10 0.019(3) 0.039(3) 0.020(3) 0.001(3) 0.008(2) 0.000(2) C11 0.024(3) 0.046(4) 0.030(3) -0.008(3) 0.012(3) 0.001(3) C12 0.022(4) 0.052(5) 0.041(4) -0.008(3) 0.013(3) -0.010(3) C13 0.026(3) 0.044(4) 0.044(4) 0.004(3) 0.015(3) 0.008(3) C14 0.021(3) 0.039(3) 0.040(4) 0.000(3) 0.012(3) -0.002(3) C15 0.020(3) 0.018(3) 0.022(3) -0.002(2) 0.008(2) -0.004(2) C16 0.025(3) 0.017(3) 0.020(3) -0.002(2) 0.007(2) -0.003(2) C17 0.012(3) 0.022(3) 0.026(3) 0.005(2) 0.005(2) 0.000(2) C18 0.020(3) 0.016(2) 0.026(3) -0.003(2) 0.011(2) -0.002(2) C19 0.024(3) 0.017(2) 0.027(3) 0.001(2) 0.010(2) -0.004(2) C20 0.017(3) 0.025(3) 0.022(3) -0.002(2) 0.006(2) -0.004(2) C21 0.017(3) 0.024(3) 0.022(3) 0.001(2) 0.008(2) 0.000(2) C22 0.017(3) 0.021(3) 0.022(3) -0.009(2) 0.005(2) 0.000(2) C23 0.020(3) 0.038(3) 0.029(3) -0.006(3) 0.009(2) -0.006(2) C24 0.021(3) 0.034(3) 0.020(3) -0.003(2) 0.008(2) -0.005(2) C25 0.027(3) 0.037(3) 0.028(3) -0.006(3) 0.006(2) -0.004(3) C26 0.029(3) 0.038(3) 0.031(3) -0.004(3) 0.011(3) -0.015(3) C27 0.023(3) 0.047(4) 0.048(4) -0.007(3) 0.011(3) 0.003(3) C28 0.031(3) 0.032(3) 0.047(4) -0.006(3) 0.013(3) -0.003(3) N1 0.012(2) 0.063(4) 0.037(3) -0.004(3) 0.008(2) 0.000(2) N2 0.011(2) 0.043(3) 0.020(2) -0.004(2) 0.0000(18) -0.003(2) N3 0.017(3) 0.053(4) 0.030(3) -0.005(2) 0.007(2) -0.007(2) N4 0.015(2) 0.027(2) 0.037(3) -0.003(2) 0.010(2) -0.0010(19) O1 0.019(2) 0.058(3) 0.017(2) -0.0045(18) 0.0066(17) 0.0014(17) O2 0.021(2) 0.050(3) 0.019(2) -0.0008(18) 0.0107(17) 0.0021(18) O3 0.017(2) 0.045(2) 0.0171(19) 0.0066(19) -0.0022(15) 0.0019(19) O4 0.031(2) 0.036(2) 0.0167(19) -0.0115(17) 0.0068(16) -0.0020(18) O5 0.019(2) 0.046(3) 0.050(3) -0.013(2) 0.004(2) -0.0019(19) O6 0.024(2) 0.0172(18) 0.031(2) 0.0019(17) 0.0010(16) -0.0021(16) O7 0.027(2) 0.0194(18) 0.026(2) 0.0025(18) -0.0047(17) -0.0025(17) O8 0.0147(19) 0.031(2) 0.035(2) -0.0112(18) 0.0057(16) -0.0004(16) O9 0.035(2) 0.0134(19) 0.042(2) 0.0005(19) 0.015(2) 0.0015(17) O10 0.026(3) 0.080(4) 0.085(5) -0.060(3) 0.022(3) -0.013(2) O1W 0.035(3) 0.070(3) 0.041(3) 0.005(3) 0.005(2) 0.003(3) O2W 0.040(3) 0.072(4) 0.043(3) 0.009(3) 0.009(2) 0.013(3) O3W 0.073(6) 0.029(4) 0.072(6) 0.000 0.035(5) 0.000 O4W 0.132(14) 0.038(6) 0.146(15) -0.017(8) 0.106(12) -0.019(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 Ag1 N1 2.151(5) . ? Ag1 N3 2.165(5) 5_776 ? Ag1 Ag1 3.3208(13) 2_755 ? Gd1 O3 2.305(4) 2_655 ? Gd1 O9 2.330(4) 1_545 ? Gd1 O8 2.352(4) 5_676 ? Gd1 O4 2.358(4) 6_566 ? Gd1 O6 2.443(4) . ? Gd1 O7 2.470(4) . ? Gd1 O2 2.486(4) . ? Gd1 O1 2.508(4) . ? C1 O2 1.264(7) . ? C1 O1 1.273(7) . ? C1 C2 1.501(8) . ? C2 C3 1.385(8) . ? C2 C7 1.397(8) . ? C3 C4 1.390(8) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C4 N2 1.416(7) . ? C5 C6 1.376(7) . ? C5 H5 0.9300 . ? C6 C7 1.400(8) . ? C6 C8 1.513(7) . ? C7 H7 0.9300 . ? C8 O3 1.244(6) . ? C8 O4 1.253(7) . ? C9 O5 1.229(8) . ? C9 N2 1.337(8) . ? C9 C10 1.504(8) . ? C10 C14 1.381(9) . ? C10 C11 1.382(9) . ? C11 C12 1.379(9) . ? C11 H11 0.9300 . ? C12 N1 1.334(9) . ? C12 H12 0.9300 . ? C13 N1 1.348(9) . ? C13 C14 1.383(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.254(7) . ? C15 O7 1.265(7) . ? C15 C16 1.494(7) . ? C16 C21 1.387(8) . ? C16 C17 1.410(8) . ? C17 C18 1.391(8) . ? C17 H17 0.9300 . ? C18 C19 1.380(8) . ? C18 C22 1.497(7) . ? C19 C20 1.401(8) . ? C19 H19 0.9300 . ? C20 C21 1.399(8) . ? C20 N4 1.434(7) . ? C21 H21 0.9300 . ? C22 O9 1.232(8) . ? C22 O8 1.268(7) . ? C23 O10 1.232(8) . ? C23 N4 1.339(8) . ? C23 C24 1.498(8) . ? C24 C28 1.380(9) . ? C24 C25 1.393(9) . ? C25 C26 1.370(9) . ? C25 H25 0.9300 . ? C26 N3 1.321(9) . ? C26 H26 0.9300 . ? C27 N3 1.336(9) . ? C27 C28 1.371(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N2 H2 0.8600 . ? N3 Ag1 2.165(5) 5_776 ? N4 H4 0.8600 . ? O3 Gd1 2.305(4) 2_655 ? O4 Gd1 2.358(4) 6_565 ? O8 Gd1 2.352(4) 5_676 ? O9 Gd1 2.330(4) 1_565 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8502 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 168.4(2) . 5_776 ? N1 Ag1 Ag1 92.63(15) . 2_755 ? N3 Ag1 Ag1 88.88(15) 5_776 2_755 ? O3 Gd1 O9 78.17(15) 2_655 1_545 ? O3 Gd1 O8 74.73(14) 2_655 5_676 ? O9 Gd1 O8 123.11(15) 1_545 5_676 ? O3 Gd1 O4 122.25(15) 2_655 6_566 ? O9 Gd1 O4 75.77(15) 1_545 6_566 ? O8 Gd1 O4 78.12(14) 5_676 6_566 ? O3 Gd1 O6 147.70(14) 2_655 . ? O9 Gd1 O6 134.05(14) 1_545 . ? O8 Gd1 O6 82.61(14) 5_676 . ? O4 Gd1 O6 73.61(14) 6_566 . ? O3 Gd1 O7 99.18(15) 2_655 . ? O9 Gd1 O7 155.69(17) 1_545 . ? O8 Gd1 O7 78.31(15) 5_676 . ? O4 Gd1 O7 123.67(14) 6_566 . ? O6 Gd1 O7 53.11(13) . . ? O3 Gd1 O2 125.52(14) 2_655 . ? O9 Gd1 O2 77.59(15) 1_545 . ? O8 Gd1 O2 155.86(14) 5_676 . ? O4 Gd1 O2 97.51(14) 6_566 . ? O6 Gd1 O2 73.43(14) . . ? O7 Gd1 O2 84.85(15) . . ? O3 Gd1 O1 76.53(14) 2_655 . ? O9 Gd1 O1 82.00(15) 1_545 . ? O8 Gd1 O1 135.79(14) 5_676 . ? O4 Gd1 O1 146.09(14) 6_566 . ? O6 Gd1 O1 106.15(14) . . ? O7 Gd1 O1 73.94(14) . . ? O2 Gd1 O1 52.28(14) . . ? O2 C1 O1 120.3(5) . . ? O2 C1 C2 119.9(5) . . ? O1 C1 C2 119.8(5) . . ? C3 C2 C7 120.1(5) . . ? C3 C2 C1 119.6(5) . . ? C7 C2 C1 120.1(5) . . ? C2 C3 C4 120.3(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.9(5) . . ? C5 C4 N2 121.4(5) . . ? C3 C4 N2 118.7(5) . . ? C6 C5 C4 119.8(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 C8 118.5(5) . . ? C7 C6 C8 120.4(5) . . ? C2 C7 C6 118.7(5) . . ? C2 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? O3 C8 O4 125.6(5) . . ? O3 C8 C6 117.2(5) . . ? O4 C8 C6 117.3(5) . . ? O5 C9 N2 124.9(6) . . ? O5 C9 C10 119.2(6) . . ? N2 C9 C10 115.9(5) . . ? C14 C10 C11 118.5(6) . . ? C14 C10 C9 118.7(6) . . ? C11 C10 C9 122.7(6) . . ? C12 C11 C10 118.7(6) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N1 C12 C11 123.5(6) . . ? N1 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? N1 C13 C14 122.2(6) . . ? N1 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C10 C14 C13 119.5(6) . . ? C10 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? O6 C15 O7 121.4(5) . . ? O6 C15 C16 120.2(5) . . ? O7 C15 C16 118.4(5) . . ? C21 C16 C17 120.5(5) . . ? C21 C16 C15 121.8(5) . . ? C17 C16 C15 117.6(5) . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 120.6(5) . . ? C19 C18 C22 119.8(5) . . ? C17 C18 C22 119.4(5) . . ? C18 C19 C20 120.3(5) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 119.7(5) . . ? C21 C20 N4 119.1(5) . . ? C19 C20 N4 121.1(5) . . ? C16 C21 C20 119.6(5) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? O9 C22 O8 125.3(5) . . ? O9 C22 C18 117.0(5) . . ? O8 C22 C18 117.7(5) . . ? O10 C23 N4 123.8(6) . . ? O10 C23 C24 118.0(5) . . ? N4 C23 C24 118.2(5) . . ? C28 C24 C25 117.3(5) . . ? C28 C24 C23 125.1(6) . . ? C25 C24 C23 117.6(5) . . ? C26 C25 C24 118.9(6) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N3 C26 C25 124.1(6) . . ? N3 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? N3 C27 C28 123.4(6) . . ? N3 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? C27 C28 C24 119.4(6) . . ? C27 C28 H28 120.3 . . ? C24 C28 H28 120.3 . . ? C12 N1 C13 117.5(5) . . ? C12 N1 Ag1 121.8(5) . . ? C13 N1 Ag1 119.9(4) . . ? C9 N2 C4 124.6(5) . . ? C9 N2 H2 117.7 . . ? C4 N2 H2 117.7 . . ? C26 N3 C27 116.8(5) . . ? C26 N3 Ag1 119.2(4) . 5_776 ? C27 N3 Ag1 123.1(4) . 5_776 ? C23 N4 C20 124.1(5) . . ? C23 N4 H4 117.9 . . ? C20 N4 H4 117.9 . . ? C1 O1 Gd1 93.0(3) . . ? C1 O2 Gd1 94.2(3) . . ? C8 O3 Gd1 162.3(4) . 2_655 ? C8 O4 Gd1 127.7(4) . 6_565 ? C15 O6 Gd1 93.3(3) . . ? C15 O7 Gd1 91.8(3) . . ? C22 O8 Gd1 129.1(3) . 5_676 ? C22 O9 Gd1 139.6(4) . 1_565 ? H1WA O1W H1WB 112.6 . . ? H2WA O2W H2WB 108.4 . . ? H3WA O3W H3WB 107.9 . . ? H4WA O4W H4WB 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -8.8(9) . . . . ? O1 C1 C2 C3 172.5(6) . . . . ? O2 C1 C2 C7 166.8(5) . . . . ? O1 C1 C2 C7 -11.9(8) . . . . ? C7 C2 C3 C4 -3.9(10) . . . . ? C1 C2 C3 C4 171.7(6) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C2 C3 C4 N2 179.2(6) . . . . ? C3 C4 C5 C6 3.0(8) . . . . ? N2 C4 C5 C6 -175.5(5) . . . . ? C4 C5 C6 C7 -3.4(8) . . . . ? C4 C5 C6 C8 175.2(5) . . . . ? C3 C2 C7 C6 3.5(9) . . . . ? C1 C2 C7 C6 -172.1(5) . . . . ? C5 C6 C7 C2 0.1(8) . . . . ? C8 C6 C7 C2 -178.5(5) . . . . ? C5 C6 C8 O3 -152.6(5) . . . . ? C7 C6 C8 O3 26.0(7) . . . . ? C5 C6 C8 O4 26.1(7) . . . . ? C7 C6 C8 O4 -155.3(5) . . . . ? O5 C9 C10 C14 -31.3(9) . . . . ? N2 C9 C10 C14 149.0(6) . . . . ? O5 C9 C10 C11 145.3(6) . . . . ? N2 C9 C10 C11 -34.4(8) . . . . ? C14 C10 C11 C12 1.6(9) . . . . ? C9 C10 C11 C12 -175.0(6) . . . . ? C10 C11 C12 N1 -0.1(11) . . . . ? C11 C10 C14 C13 -0.9(10) . . . . ? C9 C10 C14 C13 175.8(6) . . . . ? N1 C13 C14 C10 -1.4(11) . . . . ? O6 C15 C16 C21 37.6(8) . . . . ? O7 C15 C16 C21 -142.2(6) . . . . ? O6 C15 C16 C17 -145.1(6) . . . . ? O7 C15 C16 C17 35.0(8) . . . . ? C21 C16 C17 C18 4.0(8) . . . . ? C15 C16 C17 C18 -173.3(5) . . . . ? C16 C17 C18 C19 -2.9(8) . . . . ? C16 C17 C18 C22 172.0(5) . . . . ? C17 C18 C19 C20 -0.9(8) . . . . ? C22 C18 C19 C20 -175.8(5) . . . . ? C18 C19 C20 C21 3.5(8) . . . . ? C18 C19 C20 N4 179.4(5) . . . . ? C17 C16 C21 C20 -1.3(8) . . . . ? C15 C16 C21 C20 175.8(5) . . . . ? C19 C20 C21 C16 -2.4(8) . . . . ? N4 C20 C21 C16 -178.3(5) . . . . ? C19 C18 C22 O9 23.8(8) . . . . ? C17 C18 C22 O9 -151.1(5) . . . . ? C19 C18 C22 O8 -158.8(5) . . . . ? C17 C18 C22 O8 26.2(7) . . . . ? O10 C23 C24 C28 149.0(7) . . . . ? N4 C23 C24 C28 -32.7(9) . . . . ? O10 C23 C24 C25 -28.8(9) . . . . ? N4 C23 C24 C25 149.5(6) . . . . ? C28 C24 C25 C26 2.3(8) . . . . ? C23 C24 C25 C26 -179.8(6) . . . . ? C24 C25 C26 N3 -2.2(10) . . . . ? N3 C27 C28 C24 -1.2(11) . . . . ? C25 C24 C28 C27 -0.7(9) . . . . ? C23 C24 C28 C27 -178.5(6) . . . . ? C11 C12 N1 C13 -2.2(11) . . . . ? C11 C12 N1 Ag1 167.4(5) . . . . ? C14 C13 N1 C12 2.9(10) . . . . ? C14 C13 N1 Ag1 -166.8(5) . . . . ? N3 Ag1 N1 C12 13.3(14) 5_776 . . . ? Ag1 Ag1 N1 C12 -83.9(5) 2_755 . . . ? N3 Ag1 N1 C13 -177.4(9) 5_776 . . . ? Ag1 Ag1 N1 C13 85.4(5) 2_755 . . . ? O5 C9 N2 C4 -5.2(10) . . . . ? C10 C9 N2 C4 174.5(5) . . . . ? C5 C4 N2 C9 -38.6(8) . . . . ? C3 C4 N2 C9 142.8(6) . . . . ? C25 C26 N3 C27 0.3(10) . . . . ? C25 C26 N3 Ag1 169.9(5) . . . 5_776 ? C28 C27 N3 C26 1.4(10) . . . . ? C28 C27 N3 Ag1 -167.7(5) . . . 5_776 ? O10 C23 N4 C20 4.6(10) . . . . ? C24 C23 N4 C20 -173.5(5) . . . . ? C21 C20 N4 C23 -149.7(6) . . . . ? C19 C20 N4 C23 34.4(9) . . . . ? O2 C1 O1 Gd1 -4.2(5) . . . . ? C2 C1 O1 Gd1 174.5(5) . . . . ? O3 Gd1 O1 C1 -157.8(3) 2_655 . . . ? O9 Gd1 O1 C1 -78.1(3) 1_545 . . . ? O8 Gd1 O1 C1 151.6(3) 5_676 . . . ? O4 Gd1 O1 C1 -29.0(5) 6_566 . . . ? O6 Gd1 O1 C1 55.5(3) . . . . ? O7 Gd1 O1 C1 98.3(3) . . . . ? O2 Gd1 O1 C1 2.4(3) . . . . ? O1 C1 O2 Gd1 4.3(5) . . . . ? C2 C1 O2 Gd1 -174.4(5) . . . . ? O3 Gd1 O2 C1 21.6(4) 2_655 . . . ? O9 Gd1 O2 C1 87.1(3) 1_545 . . . ? O8 Gd1 O2 C1 -121.7(4) 5_676 . . . ? O4 Gd1 O2 C1 160.6(3) 6_566 . . . ? O6 Gd1 O2 C1 -129.0(3) . . . . ? O7 Gd1 O2 C1 -76.0(3) . . . . ? O1 Gd1 O2 C1 -2.4(3) . . . . ? O4 C8 O3 Gd1 31.0(16) . . . 2_655 ? C6 C8 O3 Gd1 -150.5(10) . . . 2_655 ? O3 C8 O4 Gd1 -11.3(8) . . . 6_565 ? C6 C8 O4 Gd1 170.1(3) . . . 6_565 ? O7 C15 O6 Gd1 -6.2(6) . . . . ? C16 C15 O6 Gd1 173.9(5) . . . . ? O3 Gd1 O6 C15 -32.1(5) 2_655 . . . ? O9 Gd1 O6 C15 152.6(3) 1_545 . . . ? O8 Gd1 O6 C15 -77.5(4) 5_676 . . . ? O4 Gd1 O6 C15 -157.2(4) 6_566 . . . ? O7 Gd1 O6 C15 3.4(3) . . . . ? O2 Gd1 O6 C15 99.5(4) . . . . ? O1 Gd1 O6 C15 58.1(4) . . . . ? O6 C15 O7 Gd1 6.2(6) . . . . ? C16 C15 O7 Gd1 -174.0(5) . . . . ? O3 Gd1 O7 C15 158.3(4) 2_655 . . . ? O9 Gd1 O7 C15 -120.1(4) 1_545 . . . ? O8 Gd1 O7 C15 86.1(4) 5_676 . . . ? O4 Gd1 O7 C15 19.1(4) 6_566 . . . ? O6 Gd1 O7 C15 -3.4(3) . . . . ? O2 Gd1 O7 C15 -76.5(4) . . . . ? O1 Gd1 O7 C15 -128.7(4) . . . . ? O9 C22 O8 Gd1 -67.6(7) . . . 5_676 ? C18 C22 O8 Gd1 115.3(5) . . . 5_676 ? O8 C22 O9 Gd1 52.4(8) . . . 1_565 ? C18 C22 O9 Gd1 -130.5(5) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.923 _refine_diff_density_min -3.387 _refine_diff_density_rms 0.210 data_5 _database_code_depnum_ccdc_archive 'CCDC 760889' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 Ag N4 O13 Tb' _chemical_formula_weight 889.30 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.572(2) _cell_length_b 10.7584(8) _cell_length_c 20.6212(16) _cell_angle_alpha 90.00 _cell_angle_beta 110.8560(10) _cell_angle_gamma 90.00 _cell_volume 5716.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7490 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 28.19 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 3.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5379 _exptl_absorpt_correction_T_max 0.7391 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14133 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5147 _reflns_number_gt 4547 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0989P)^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 5147 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1353 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.48227(2) 0.55007(7) 0.16442(3) 0.0548(2) Uani 1 1 d . . . Tb1 Tb 0.948981(9) 0.62394(2) 0.031190(13) 0.01440(14) Uani 1 1 d . . . C1 C 0.9044(2) 0.6116(5) 0.1368(3) 0.0208(13) Uani 1 1 d . . . C2 C 0.8814(2) 0.5936(6) 0.1918(3) 0.0209(12) Uani 1 1 d . . . C3 C 0.9135(2) 0.5733(5) 0.2603(3) 0.0205(12) Uani 1 1 d . . . H3 H 0.9494 0.5803 0.2734 0.025 Uiso 1 1 calc R . . C4 C 0.8909(2) 0.5421(5) 0.3092(3) 0.0186(12) Uani 1 1 d . . . C5 C 0.9237(2) 0.5219(5) 0.3840(3) 0.0198(12) Uani 1 1 d . . . C6 C 0.8377(2) 0.5303(5) 0.2896(3) 0.0209(12) Uani 1 1 d . . . H6 H 0.8231 0.5037 0.3215 0.025 Uiso 1 1 calc R . . C7 C 0.8060(2) 0.5584(5) 0.2218(3) 0.0222(12) Uani 1 1 d . . . C8 C 0.8280(2) 0.5902(6) 0.1732(3) 0.0242(13) Uani 1 1 d . . . H8 H 0.8069 0.6092 0.1280 0.029 Uiso 1 1 calc R . . C9 C 0.7241(2) 0.4731(6) 0.2236(3) 0.0294(14) Uani 1 1 d . . . C10 C 0.6668(2) 0.4964(6) 0.2003(3) 0.0271(13) Uani 1 1 d . . . C11 C 0.6342(3) 0.3958(7) 0.1909(4) 0.0345(16) Uani 1 1 d . . . H11 H 0.6475 0.3155 0.1955 0.041 Uiso 1 1 calc R . . C12 C 0.5822(3) 0.4148(7) 0.1747(4) 0.0376(16) Uani 1 1 d . . . H12 H 0.5606 0.3458 0.1677 0.045 Uiso 1 1 calc R . . C13 C 0.5924(3) 0.6252(7) 0.1764(4) 0.0387(19) Uani 1 1 d . . . H13 H 0.5782 0.7046 0.1708 0.046 Uiso 1 1 calc R . . C14 C 0.6454(3) 0.6138(6) 0.1926(4) 0.0314(16) Uani 1 1 d . . . H14 H 0.6662 0.6840 0.1982 0.038 Uiso 1 1 calc R . . C15 C 0.9105(2) 0.8663(5) 0.0088(3) 0.0188(12) Uani 1 1 d . . . C16 C 0.8932(2) 0.9992(5) -0.0071(3) 0.0209(12) Uani 1 1 d . . . C17 C 0.8414(2) 1.0304(5) -0.0336(3) 0.0222(12) Uani 1 1 d . . . H17 H 0.8162 0.9686 -0.0453 0.027 Uiso 1 1 calc R . . C18 C 0.8271(2) 1.1550(5) -0.0427(3) 0.0202(12) Uani 1 1 d . . . C19 C 0.8652(2) 1.2467(5) -0.0235(3) 0.0249(13) Uani 1 1 d . . . H19 H 0.8557 1.3301 -0.0281 0.030 Uiso 1 1 calc R . . C20 C 0.9171(2) 1.2143(5) 0.0026(3) 0.0202(12) Uani 1 1 d . . . C21 C 0.9319(2) 1.0906(5) 0.0098(3) 0.0198(12) Uani 1 1 d . . . H21 H 0.9668 1.0687 0.0254 0.024 Uiso 1 1 calc R . . C22 C 0.9582(2) 1.3134(5) 0.0283(3) 0.0201(12) Uani 1 1 d . . . C23 C 0.7535(2) 1.2881(6) -0.1075(3) 0.0284(14) Uani 1 1 d . . . C24 C 0.6969(2) 1.3171(6) -0.1247(3) 0.0237(13) Uani 1 1 d . . . C25 C 0.6583(3) 1.2300(6) -0.1346(4) 0.0364(16) Uani 1 1 d . . . H25 H 0.6664 1.1457 -0.1301 0.044 Uiso 1 1 calc R . . C26 C 0.6080(3) 1.2683(7) -0.1511(4) 0.0401(17) Uani 1 1 d . . . H26 H 0.5824 1.2082 -0.1582 0.048 Uiso 1 1 calc R . . C27 C 0.6309(3) 1.4713(6) -0.1495(3) 0.0344(16) Uani 1 1 d . . . H27 H 0.6216 1.5548 -0.1552 0.041 Uiso 1 1 calc R . . C28 C 0.6824(3) 1.4407(6) -0.1332(3) 0.0312(15) Uani 1 1 d . . . H28 H 0.7071 1.5025 -0.1279 0.037 Uiso 1 1 calc R . . N1 N 0.5608(2) 0.5287(6) 0.1684(3) 0.0372(14) Uani 1 1 d . . . N2 N 0.75138(18) 0.5577(5) 0.2015(3) 0.0264(12) Uani 1 1 d . . . H2 H 0.7342 0.6145 0.1732 0.032 Uiso 1 1 calc R . . N3 N 0.5939(2) 1.3877(5) -0.1575(3) 0.0320(13) Uani 1 1 d . . . N4 N 0.77324(18) 1.1875(5) -0.0691(3) 0.0259(11) Uani 1 1 d . . . H4 H 0.7520 1.1387 -0.0595 0.031 Uiso 1 1 calc R . . O1 O 0.87595(17) 0.6072(4) 0.0736(2) 0.0297(10) Uani 1 1 d . . . O2 O 0.95288(17) 0.6284(4) 0.1539(2) 0.0322(11) Uani 1 1 d . . . O3 O 0.96663(16) 0.5755(4) 0.4063(2) 0.0299(10) Uani 1 1 d . . . O4 O 0.90582(16) 0.4543(4) 0.4195(2) 0.0280(10) Uani 1 1 d . . . O5 O 0.74334(19) 0.3835(4) 0.2610(3) 0.0412(13) Uani 1 1 d . . . O6 O 0.88639(15) 0.7811(3) -0.0301(2) 0.0247(9) Uani 1 1 d . . . O7 O 0.94986(17) 0.8445(4) 0.0619(2) 0.0291(10) Uani 1 1 d . . . O8 O 1.00318(15) 1.2891(4) 0.0307(2) 0.0265(9) Uani 1 1 d . . . O9 O 0.94435(16) 1.4122(4) 0.0475(2) 0.0291(10) Uani 1 1 d . . . O10 O 0.7794(2) 1.3603(6) -0.1273(4) 0.0608(19) Uani 1 1 d . . . O1W O 0.28374(19) 0.7699(5) 0.3902(3) 0.0511(14) Uani 1 1 d . . . H1WA H 0.2659 0.7833 0.4156 0.061 Uiso 1 1 d R . . H1WB H 0.3148 0.7548 0.4163 0.061 Uiso 1 1 d R . . O2W O 0.2807(2) 0.0088(5) 0.5125(3) 0.0530(14) Uani 1 1 d . . . H2WA H 0.3099 -0.0270 0.5312 0.064 Uiso 1 1 d R . . H2WB H 0.2803 0.0436 0.4753 0.064 Uiso 1 1 d R . . O3W O 0.5000 0.6744(6) 0.7500 0.051(2) Uani 1 2 d S . . H3WA H 0.5294 0.6733 0.7826 0.061 Uiso 0.50 1 d PR . . H3WB H 0.4853 0.7438 0.7501 0.061 Uiso 0.50 1 d PR . . O4W O 0.2233(6) 0.8132(11) 0.4698(9) 0.090(5) Uani 0.50 1 d P . . H4WB H 0.2273 0.8877 0.4845 0.108 Uiso 0.50 1 d PR . . H4WA H 0.1959 0.8080 0.4340 0.108 Uiso 0.50 1 d PR . . 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 Ag1 0.0224(3) 0.0870(5) 0.0585(4) 0.0107(3) 0.0186(3) 0.0153(3) Tb1 0.0149(2) 0.01079(19) 0.0185(2) -0.00005(9) 0.00718(13) 0.00081(9) C1 0.022(3) 0.021(3) 0.023(3) 0.003(2) 0.013(3) 0.003(2) C2 0.020(3) 0.023(3) 0.022(3) 0.000(2) 0.011(2) 0.000(2) C3 0.019(3) 0.018(3) 0.026(3) 0.002(2) 0.010(2) 0.001(2) C4 0.023(3) 0.015(3) 0.020(3) 0.002(2) 0.009(2) 0.000(2) C5 0.018(3) 0.016(3) 0.026(3) -0.004(2) 0.008(2) 0.000(2) C6 0.019(3) 0.024(3) 0.023(3) 0.001(2) 0.011(2) -0.001(2) C7 0.016(3) 0.027(3) 0.024(3) -0.001(2) 0.007(2) 0.000(2) C8 0.020(3) 0.035(3) 0.018(3) 0.004(3) 0.007(2) -0.001(3) C9 0.024(3) 0.037(4) 0.025(3) -0.004(3) 0.006(3) 0.000(3) C10 0.024(3) 0.036(3) 0.023(3) 0.004(3) 0.011(3) 0.000(3) C11 0.026(4) 0.041(4) 0.038(4) -0.001(3) 0.013(3) 0.001(3) C12 0.029(4) 0.043(4) 0.042(4) -0.001(3) 0.014(3) -0.007(3) C13 0.031(4) 0.049(5) 0.043(5) 0.011(3) 0.021(3) 0.011(3) C14 0.021(3) 0.040(4) 0.037(4) 0.003(3) 0.014(3) -0.001(3) C15 0.018(3) 0.014(3) 0.026(3) 0.000(2) 0.010(3) 0.002(2) C16 0.026(3) 0.013(3) 0.025(3) -0.002(2) 0.011(2) 0.002(2) C17 0.024(3) 0.018(3) 0.026(3) 0.002(2) 0.010(2) -0.001(2) C18 0.016(3) 0.022(3) 0.023(3) 0.004(2) 0.007(2) 0.004(2) C19 0.028(3) 0.013(3) 0.038(4) 0.002(2) 0.016(3) 0.005(2) C20 0.025(3) 0.013(3) 0.027(3) 0.000(2) 0.015(2) 0.001(2) C21 0.021(3) 0.016(3) 0.026(3) -0.003(2) 0.013(3) 0.000(2) C22 0.020(3) 0.017(3) 0.025(3) 0.009(2) 0.009(2) 0.001(2) C23 0.022(3) 0.032(3) 0.032(3) 0.005(3) 0.012(3) 0.004(3) C24 0.022(3) 0.027(3) 0.023(3) 0.005(3) 0.009(2) 0.004(3) C25 0.037(4) 0.028(3) 0.048(4) 0.009(3) 0.019(3) 0.007(3) C26 0.029(4) 0.034(4) 0.057(5) 0.009(3) 0.016(3) -0.003(3) C27 0.034(4) 0.036(4) 0.035(4) 0.007(3) 0.015(3) 0.015(3) C28 0.032(4) 0.027(3) 0.037(4) -0.001(3) 0.015(3) -0.001(3) N1 0.021(3) 0.051(4) 0.040(3) 0.004(3) 0.011(2) 0.000(3) N2 0.012(2) 0.044(3) 0.024(3) 0.010(2) 0.008(2) 0.004(2) N3 0.024(3) 0.042(3) 0.034(3) 0.005(2) 0.016(3) 0.008(2) N4 0.020(3) 0.022(3) 0.037(3) 0.006(2) 0.012(2) 0.002(2) O1 0.023(2) 0.042(3) 0.027(3) 0.0028(19) 0.013(2) 0.0015(19) O2 0.020(2) 0.051(3) 0.029(3) 0.0043(19) 0.013(2) 0.0021(19) O3 0.022(2) 0.038(2) 0.026(2) -0.004(2) 0.0045(18) -0.001(2) O4 0.027(2) 0.032(2) 0.025(2) 0.0074(19) 0.0092(18) 0.0006(18) O5 0.023(3) 0.040(3) 0.057(4) 0.011(2) 0.009(2) 0.002(2) O6 0.024(2) 0.0104(18) 0.033(2) -0.0014(17) 0.0022(18) -0.0005(16) O7 0.034(3) 0.0147(19) 0.031(3) -0.0017(19) 0.002(2) 0.0029(18) O8 0.021(2) 0.024(2) 0.036(2) 0.0072(18) 0.0134(18) 0.0008(17) O9 0.035(3) 0.012(2) 0.043(3) 0.0003(19) 0.017(2) -0.0033(18) O10 0.025(3) 0.078(4) 0.083(5) 0.050(3) 0.023(3) 0.008(3) O1W 0.037(3) 0.069(4) 0.044(3) 0.000(3) 0.010(2) 0.001(3) O2W 0.043(3) 0.068(4) 0.045(3) 0.007(3) 0.012(3) 0.015(3) O3W 0.062(5) 0.023(4) 0.076(6) 0.000 0.037(5) 0.000 O4W 0.126(13) 0.044(7) 0.148(15) -0.013(8) 0.107(12) -0.019(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.149(5) . ? Ag1 N3 2.161(5) 5_675 ? Ag1 Ag1 3.3099(14) 2_655 ? Tb1 O3 2.283(4) 2_755 ? Tb1 O9 2.312(4) 1_545 ? Tb1 O8 2.333(4) 5_775 ? Tb1 O4 2.340(4) 6_565 ? Tb1 O6 2.425(4) . ? Tb1 O7 2.454(4) . ? Tb1 O1 2.471(4) . ? Tb1 O2 2.495(5) . ? C1 O1 1.261(8) . ? C1 O2 1.269(8) . ? C1 C2 1.495(8) . ? C2 C8 1.382(8) . ? C2 C3 1.391(8) . ? C3 C4 1.403(8) . ? C3 H3 0.9300 . ? C4 C6 1.382(8) . ? C4 C5 1.501(8) . ? C5 O3 1.247(7) . ? C5 O4 1.252(7) . ? C6 C7 1.393(8) . ? C6 H6 0.9300 . ? C7 C8 1.386(8) . ? C7 N2 1.412(7) . ? C8 H8 0.9300 . ? C9 O5 1.230(8) . ? C9 N2 1.358(8) . ? C9 C10 1.501(8) . ? C10 C11 1.375(9) . ? C10 C14 1.379(9) . ? C11 C12 1.366(9) . ? C11 H11 0.9300 . ? C12 N1 1.346(9) . ? C12 H12 0.9300 . ? C13 N1 1.328(9) . ? C13 C14 1.382(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.244(7) . ? C15 O7 1.258(7) . ? C15 C16 1.506(7) . ? C16 C17 1.376(8) . ? C16 C21 1.402(8) . ? C17 C18 1.391(8) . ? C17 H17 0.9300 . ? C18 C19 1.391(8) . ? C18 N4 1.432(7) . ? C19 C20 1.383(8) . ? C19 H19 0.9300 . ? C20 C21 1.384(8) . ? C20 C22 1.509(8) . ? C21 H21 0.9300 . ? C22 O9 1.242(8) . ? C22 O8 1.250(7) . ? C23 O10 1.221(8) . ? C23 N4 1.337(8) . ? C23 C24 1.504(8) . ? C24 C25 1.377(9) . ? C24 C28 1.381(9) . ? C25 C26 1.370(10) . ? C25 H25 0.9300 . ? C26 N3 1.335(9) . ? C26 H26 0.9300 . ? C27 N3 1.324(9) . ? C27 C28 1.379(9) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N2 H2 0.8600 . ? N3 Ag1 2.161(5) 5_675 ? N4 H4 0.8600 . ? O3 Tb1 2.283(4) 2_755 ? O4 Tb1 2.340(4) 6_566 ? O8 Tb1 2.333(4) 5_775 ? O9 Tb1 2.312(4) 1_565 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8502 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? O4W H4WB 0.8500 . ? O4W H4WA 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 168.0(2) . 5_675 ? N1 Ag1 Ag1 92.74(16) . 2_655 ? N3 Ag1 Ag1 88.94(16) 5_675 2_655 ? O3 Tb1 O9 77.94(16) 2_755 1_545 ? O3 Tb1 O8 74.88(15) 2_755 5_775 ? O9 Tb1 O8 123.09(15) 1_545 5_775 ? O3 Tb1 O4 122.18(15) 2_755 6_565 ? O9 Tb1 O4 75.76(15) 1_545 6_565 ? O8 Tb1 O4 78.13(15) 5_775 6_565 ? O3 Tb1 O6 147.84(14) 2_755 . ? O9 Tb1 O6 134.15(14) 1_545 . ? O8 Tb1 O6 82.60(14) 5_775 . ? O4 Tb1 O6 73.71(14) 6_565 . ? O3 Tb1 O7 99.24(15) 2_755 . ? O9 Tb1 O7 155.63(18) 1_545 . ? O8 Tb1 O7 78.32(15) 5_775 . ? O4 Tb1 O7 123.81(14) 6_565 . ? O6 Tb1 O7 53.14(14) . . ? O3 Tb1 O1 125.37(15) 2_755 . ? O9 Tb1 O1 77.43(15) 1_545 . ? O8 Tb1 O1 156.00(14) 5_775 . ? O4 Tb1 O1 97.41(15) 6_565 . ? O6 Tb1 O1 73.56(14) . . ? O7 Tb1 O1 85.06(15) . . ? O3 Tb1 O2 76.38(15) 2_755 . ? O9 Tb1 O2 81.71(16) 1_545 . ? O8 Tb1 O2 135.94(15) 5_775 . ? O4 Tb1 O2 145.92(15) 6_565 . ? O6 Tb1 O2 106.32(14) . . ? O7 Tb1 O2 74.16(15) . . ? O1 Tb1 O2 52.32(15) . . ? O1 C1 O2 119.9(6) . . ? O1 C1 C2 120.3(5) . . ? O2 C1 C2 119.8(6) . . ? C8 C2 C3 120.5(5) . . ? C8 C2 C1 119.3(5) . . ? C3 C2 C1 120.1(5) . . ? C2 C3 C4 118.8(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C6 C4 C3 120.6(5) . . ? C6 C4 C5 118.5(5) . . ? C3 C4 C5 120.9(5) . . ? O3 C5 O4 125.0(6) . . ? O3 C5 C4 117.3(5) . . ? O4 C5 C4 117.7(5) . . ? C4 C6 C7 119.6(5) . . ? C4 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 120.0(5) . . ? C8 C7 N2 118.9(5) . . ? C6 C7 N2 121.1(5) . . ? C2 C8 C7 120.2(6) . . ? C2 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? O5 C9 N2 124.7(6) . . ? O5 C9 C10 120.1(6) . . ? N2 C9 C10 115.2(5) . . ? C11 C10 C14 118.3(6) . . ? C11 C10 C9 118.3(6) . . ? C14 C10 C9 123.3(6) . . ? C12 C11 C10 119.5(7) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N1 C12 C11 123.1(7) . . ? N1 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N1 C13 C14 123.4(6) . . ? N1 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C10 C14 C13 118.7(6) . . ? C10 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? O6 C15 O7 121.4(5) . . ? O6 C15 C16 120.3(5) . . ? O7 C15 C16 118.3(5) . . ? C17 C16 C21 121.2(5) . . ? C17 C16 C15 121.4(5) . . ? C21 C16 C15 117.3(5) . . ? C16 C17 C18 119.5(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.8(5) . . ? C19 C18 N4 120.7(5) . . ? C17 C18 N4 119.5(5) . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 C22 119.0(5) . . ? C19 C20 C22 120.2(5) . . ? C20 C21 C16 118.6(5) . . ? C20 C21 H21 120.7 . . ? C16 C21 H21 120.7 . . ? O9 C22 O8 125.5(6) . . ? O9 C22 C20 116.0(5) . . ? O8 C22 C20 118.5(5) . . ? O10 C23 N4 123.3(6) . . ? O10 C23 C24 118.1(6) . . ? N4 C23 C24 118.5(5) . . ? C25 C24 C28 117.7(6) . . ? C25 C24 C23 125.1(6) . . ? C28 C24 C23 117.2(6) . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N3 C26 C25 123.2(6) . . ? N3 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N3 C27 C28 123.3(6) . . ? N3 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C27 C28 C24 119.1(6) . . ? C27 C28 H28 120.4 . . ? C24 C28 H28 120.4 . . ? C13 N1 C12 116.9(6) . . ? C13 N1 Ag1 122.0(5) . . ? C12 N1 Ag1 120.2(4) . . ? C9 N2 C7 124.3(5) . . ? C9 N2 H2 117.9 . . ? C7 N2 H2 117.9 . . ? C27 N3 C26 117.3(6) . . ? C27 N3 Ag1 119.0(4) . 5_675 ? C26 N3 Ag1 123.1(5) . 5_675 ? C23 N4 C18 124.9(5) . . ? C23 N4 H4 117.6 . . ? C18 N4 H4 117.6 . . ? C1 O1 Tb1 94.5(4) . . ? C1 O2 Tb1 93.2(4) . . ? C5 O3 Tb1 162.9(4) . 2_755 ? C5 O4 Tb1 128.0(4) . 6_566 ? C15 O6 Tb1 93.4(3) . . ? C15 O7 Tb1 91.7(3) . . ? C22 O8 Tb1 129.8(4) . 5_775 ? C22 O9 Tb1 139.3(4) . 1_565 ? H1WA O1W H1WB 108.5 . . ? H2WA O2W H2WB 108.4 . . ? H3WA O3W H3WB 109.5 . . ? H4WB O4W H4WA 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C8 -9.4(9) . . . . ? O2 C1 C2 C8 172.4(6) . . . . ? O1 C1 C2 C3 166.9(5) . . . . ? O2 C1 C2 C3 -11.3(9) . . . . ? C8 C2 C3 C4 3.7(9) . . . . ? C1 C2 C3 C4 -172.5(5) . . . . ? C2 C3 C4 C6 0.8(8) . . . . ? C2 C3 C4 C5 -178.7(5) . . . . ? C6 C4 C5 O3 -153.7(5) . . . . ? C3 C4 C5 O3 25.8(8) . . . . ? C6 C4 C5 O4 25.3(7) . . . . ? C3 C4 C5 O4 -155.3(5) . . . . ? C3 C4 C6 C7 -4.7(8) . . . . ? C5 C4 C6 C7 174.8(5) . . . . ? C4 C6 C7 C8 4.2(9) . . . . ? C4 C6 C7 N2 -174.5(5) . . . . ? C3 C2 C8 C7 -4.2(10) . . . . ? C1 C2 C8 C7 172.1(6) . . . . ? C6 C7 C8 C2 0.2(9) . . . . ? N2 C7 C8 C2 179.0(6) . . . . ? O5 C9 C10 C11 -31.1(9) . . . . ? N2 C9 C10 C11 149.9(6) . . . . ? O5 C9 C10 C14 144.2(7) . . . . ? N2 C9 C10 C14 -34.8(9) . . . . ? C14 C10 C11 C12 -0.3(10) . . . . ? C9 C10 C11 C12 175.2(6) . . . . ? C10 C11 C12 N1 -1.1(11) . . . . ? C11 C10 C14 C13 0.6(10) . . . . ? C9 C10 C14 C13 -174.7(6) . . . . ? N1 C13 C14 C10 0.6(11) . . . . ? O6 C15 C16 C17 38.1(9) . . . . ? O7 C15 C16 C17 -142.4(6) . . . . ? O6 C15 C16 C21 -145.3(6) . . . . ? O7 C15 C16 C21 34.2(8) . . . . ? C21 C16 C17 C18 -1.2(9) . . . . ? C15 C16 C17 C18 175.3(5) . . . . ? C16 C17 C18 C19 -1.5(9) . . . . ? C16 C17 C18 N4 -178.9(5) . . . . ? C17 C18 C19 C20 2.1(9) . . . . ? N4 C18 C19 C20 179.4(5) . . . . ? C18 C19 C20 C21 0.1(9) . . . . ? C18 C19 C20 C22 -175.4(5) . . . . ? C19 C20 C21 C16 -2.7(9) . . . . ? C22 C20 C21 C16 172.9(5) . . . . ? C17 C16 C21 C20 3.3(9) . . . . ? C15 C16 C21 C20 -173.3(5) . . . . ? C21 C20 C22 O9 -151.2(6) . . . . ? C19 C20 C22 O9 24.3(8) . . . . ? C21 C20 C22 O8 26.7(8) . . . . ? C19 C20 C22 O8 -157.7(6) . . . . ? O10 C23 C24 C25 150.2(7) . . . . ? N4 C23 C24 C25 -32.5(10) . . . . ? O10 C23 C24 C28 -27.7(9) . . . . ? N4 C23 C24 C28 149.6(6) . . . . ? C28 C24 C25 C26 -1.1(10) . . . . ? C23 C24 C25 C26 -179.0(7) . . . . ? C24 C25 C26 N3 -0.8(12) . . . . ? N3 C27 C28 C24 0.1(10) . . . . ? C25 C24 C28 C27 1.4(9) . . . . ? C23 C24 C28 C27 179.4(6) . . . . ? C14 C13 N1 C12 -2.0(11) . . . . ? C14 C13 N1 Ag1 167.0(6) . . . . ? C11 C12 N1 C13 2.2(11) . . . . ? C11 C12 N1 Ag1 -167.0(6) . . . . ? N3 Ag1 N1 C13 13.9(14) 5_675 . . . ? Ag1 Ag1 N1 C13 -84.0(6) 2_655 . . . ? N3 Ag1 N1 C12 -177.5(9) 5_675 . . . ? Ag1 Ag1 N1 C12 84.7(5) 2_655 . . . ? O5 C9 N2 C7 -4.0(10) . . . . ? C10 C9 N2 C7 174.9(5) . . . . ? C8 C7 N2 C9 142.4(6) . . . . ? C6 C7 N2 C9 -38.9(9) . . . . ? C28 C27 N3 C26 -1.9(11) . . . . ? C28 C27 N3 Ag1 168.9(5) . . . 5_675 ? C25 C26 N3 C27 2.2(11) . . . . ? C25 C26 N3 Ag1 -168.2(6) . . . 5_675 ? O10 C23 N4 C18 3.9(11) . . . . ? C24 C23 N4 C18 -173.3(6) . . . . ? C19 C18 N4 C23 33.3(9) . . . . ? C17 C18 N4 C23 -149.4(6) . . . . ? O2 C1 O1 Tb1 3.8(6) . . . . ? C2 C1 O1 Tb1 -174.4(5) . . . . ? O3 Tb1 O1 C1 21.9(4) 2_755 . . . ? O9 Tb1 O1 C1 87.1(3) 1_545 . . . ? O8 Tb1 O1 C1 -122.0(4) 5_775 . . . ? O4 Tb1 O1 C1 160.6(3) 6_565 . . . ? O6 Tb1 O1 C1 -128.8(4) . . . . ? O7 Tb1 O1 C1 -75.9(3) . . . . ? O2 Tb1 O1 C1 -2.1(3) . . . . ? O1 C1 O2 Tb1 -3.7(5) . . . . ? C2 C1 O2 Tb1 174.5(5) . . . . ? O3 Tb1 O2 C1 -157.9(4) 2_755 . . . ? O9 Tb1 O2 C1 -78.4(3) 1_545 . . . ? O8 Tb1 O2 C1 151.6(3) 5_775 . . . ? O4 Tb1 O2 C1 -29.6(5) 6_565 . . . ? O6 Tb1 O2 C1 55.3(3) . . . . ? O7 Tb1 O2 C1 98.2(3) . . . . ? O1 Tb1 O2 C1 2.1(3) . . . . ? O4 C5 O3 Tb1 29.3(18) . . . 2_755 ? C4 C5 O3 Tb1 -151.8(11) . . . 2_755 ? O3 C5 O4 Tb1 -11.3(8) . . . 6_566 ? C4 C5 O4 Tb1 169.8(4) . . . 6_566 ? O7 C15 O6 Tb1 -5.9(6) . . . . ? C16 C15 O6 Tb1 173.6(5) . . . . ? O3 Tb1 O6 C15 -32.2(5) 2_755 . . . ? O9 Tb1 O6 C15 152.4(4) 1_545 . . . ? O8 Tb1 O6 C15 -77.7(4) 5_775 . . . ? O4 Tb1 O6 C15 -157.5(4) 6_565 . . . ? O7 Tb1 O6 C15 3.2(3) . . . . ? O1 Tb1 O6 C15 99.5(4) . . . . ? O2 Tb1 O6 C15 58.1(4) . . . . ? O6 C15 O7 Tb1 5.8(6) . . . . ? C16 C15 O7 Tb1 -173.7(5) . . . . ? O3 Tb1 O7 C15 158.6(4) 2_755 . . . ? O9 Tb1 O7 C15 -120.2(4) 1_545 . . . ? O8 Tb1 O7 C15 86.3(4) 5_775 . . . ? O4 Tb1 O7 C15 19.3(4) 6_565 . . . ? O6 Tb1 O7 C15 -3.2(3) . . . . ? O1 Tb1 O7 C15 -76.3(4) . . . . ? O2 Tb1 O7 C15 -128.5(4) . . . . ? O9 C22 O8 Tb1 -67.2(8) . . . 5_775 ? C20 C22 O8 Tb1 115.1(5) . . . 5_775 ? O8 C22 O9 Tb1 51.1(9) . . . 1_565 ? C20 C22 O9 Tb1 -131.1(5) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.420 _refine_diff_density_min -1.801 _refine_diff_density_rms 0.214 data_6 _database_code_depnum_ccdc_archive 'CCDC 760890' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 Ag La N4 O11' _chemical_formula_weight 833.24 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' H H 0.0000 0.0000 '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 10.5151(10) _cell_length_b 11.1900(11) _cell_length_c 13.7534(13) _cell_angle_alpha 107.969(2) _cell_angle_beta 106.7870(10) _cell_angle_gamma 103.220(2) _cell_volume 1381.1(2) _cell_formula_units_Z 2 _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 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 2.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5854 _exptl_absorpt_correction_T_max 0.7383 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6891 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4801 _reflns_number_gt 4597 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0641P)^2^+1.1790P] 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 4801 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ag1 Ag 1.38028(4) 1.23142(5) 1.05143(3) 0.05412(15) Uani 1 1 d . . . La1 La 0.865178(19) 0.548045(17) -0.113267(14) 0.01457(10) Uani 1 1 d . . . C1 C 0.5071(4) 0.4440(4) -0.2946(3) 0.0203(7) Uani 1 1 d . . . C2 C 0.3614(4) 0.4280(4) -0.2937(3) 0.0204(7) Uani 1 1 d . . . C3 C 0.2467(4) 0.3824(4) -0.3939(3) 0.0211(7) Uani 1 1 d . . . H3 H 0.2617 0.3719 -0.4590 0.025 Uiso 1 1 calc R . . C4 C 0.1105(4) 0.3527(4) -0.3965(3) 0.0190(7) Uani 1 1 d . . . C5 C 0.0871(4) 0.3679(4) -0.3003(3) 0.0205(7) Uani 1 1 d . . . H5 H -0.0049 0.3460 -0.3028 0.025 Uiso 1 1 calc R . . C6 C 0.2017(4) 0.4161(4) -0.1997(3) 0.0203(7) Uani 1 1 d . . . C7 C 0.3388(4) 0.4452(4) -0.1967(3) 0.0222(8) Uani 1 1 d . . . H7 H 0.4153 0.4763 -0.1297 0.027 Uiso 1 1 calc R . . C8 C 0.1738(4) 0.4311(3) -0.0974(3) 0.0196(7) Uani 1 1 d . . . C9 C -0.0241(4) 0.3460(4) -0.5773(3) 0.0219(8) Uani 1 1 d . . . C10 C -0.1708(4) 0.2896(4) -0.6658(3) 0.0243(8) Uani 1 1 d . . . C11 C -0.1867(5) 0.2672(5) -0.7737(4) 0.0368(10) Uani 1 1 d . . . H11 H -0.1080 0.2793 -0.7926 0.044 Uiso 1 1 calc R . . C12 C -0.3205(5) 0.2266(6) -0.8530(4) 0.0419(12) Uani 1 1 d . . . H12 H -0.3301 0.2092 -0.9259 0.050 Uiso 1 1 calc R . . C13 C -0.4210(5) 0.2306(6) -0.7265(4) 0.0451(12) Uani 1 1 d . . . H13 H -0.5013 0.2187 -0.7096 0.054 Uiso 1 1 calc R . . C14 C -0.2918(5) 0.2674(5) -0.6431(4) 0.0398(11) Uani 1 1 d . . . H14 H -0.2857 0.2773 -0.5721 0.048 Uiso 1 1 calc R . . C15 C 1.1842(4) 0.7592(4) 0.1045(3) 0.0189(7) Uani 1 1 d . . . C16 C 1.2093(4) 0.8992(4) 0.1802(3) 0.0217(8) Uani 1 1 d . . . C17 C 1.2568(4) 0.9369(4) 0.2939(3) 0.0223(8) Uani 1 1 d . . . H17 H 1.2804 0.8775 0.3243 0.027 Uiso 1 1 calc R . . C18 C 1.2691(4) 1.0630(4) 0.3626(3) 0.0226(8) Uani 1 1 d . . . C19 C 1.2353(4) 1.1515(4) 0.3178(3) 0.0232(8) Uani 1 1 d . . . H19 H 1.2413 1.2353 0.3636 0.028 Uiso 1 1 calc R . . C20 C 1.1922(4) 1.1155(4) 0.2036(3) 0.0210(7) Uani 1 1 d . . . C21 C 1.1784(4) 0.9899(4) 0.1350(3) 0.0204(7) Uani 1 1 d . . . H21 H 1.1486 0.9656 0.0589 0.024 Uiso 1 1 calc R . . C22 C 1.1533(4) 1.2132(4) 0.1569(3) 0.0200(7) Uani 1 1 d . . . C23 C 1.2457(5) 1.0252(4) 0.5213(3) 0.0305(9) Uani 1 1 d . . . C24 C 1.2834(5) 1.0798(4) 0.6444(3) 0.0269(8) Uani 1 1 d . . . C25 C 1.1735(5) 1.0573(5) 0.6810(4) 0.0368(10) Uani 1 1 d . . . H25 H 1.0800 1.0132 0.6304 0.044 Uiso 1 1 calc R . . C26 C 1.2050(5) 1.1009(5) 0.7926(4) 0.0380(10) Uani 1 1 d . . . H26 H 1.1307 1.0860 0.8163 0.046 Uiso 1 1 calc R . . C27 C 1.4419(5) 1.1861(5) 0.8335(4) 0.0385(11) Uani 1 1 d . . . H27 H 1.5344 1.2303 0.8858 0.046 Uiso 1 1 calc R . . C28 C 1.4202(5) 1.1470(5) 0.7225(3) 0.0330(9) Uani 1 1 d . . . H28 H 1.4961 1.1655 0.7010 0.040 Uiso 1 1 calc R . . N1 N -0.4369(4) 0.2109(4) -0.8310(3) 0.0369(9) Uani 1 1 d . . . N2 N -0.0102(3) 0.3007(3) -0.4968(3) 0.0236(7) Uani 1 1 d . . . H2 H -0.0803 0.2345 -0.5068 0.028 Uiso 1 1 calc R . . N3 N 1.3384(4) 1.1644(4) 0.8700(3) 0.0354(8) Uani 1 1 d . . . N4 N 1.3116(4) 1.1013(3) 0.4797(3) 0.0251(7) Uani 1 1 d . . . H4 H 1.3811 1.1746 0.5243 0.030 Uiso 1 1 calc R . . O1 O 0.6117(3) 0.5253(3) -0.2079(2) 0.0263(6) Uani 1 1 d . . . O2 O 0.5148(3) 0.3721(3) -0.3812(2) 0.0318(7) Uani 1 1 d . . . O3 O 0.2679(3) 0.4383(3) -0.0136(2) 0.0314(7) Uani 1 1 d . . . O4 O 0.0536(3) 0.4363(3) -0.0965(2) 0.0210(5) Uani 1 1 d . . . O5 O 0.0726(3) 0.4286(3) -0.5795(2) 0.0304(6) Uani 1 1 d . . . O6 O 1.1079(3) 0.7206(3) 0.0037(2) 0.0250(6) Uani 1 1 d . . . O7 O 1.2398(3) 0.6898(2) 0.1474(2) 0.0228(6) Uani 1 1 d . . . O8 O 1.1136(3) 1.2977(3) 0.2117(2) 0.0272(6) Uani 1 1 d . . . O9 O 1.1625(3) 1.2087(3) 0.0663(2) 0.0236(6) Uani 1 1 d . . . O10 O 1.1549(5) 0.9147(4) 0.4629(3) 0.0612(12) Uani 1 1 d . . . O1W O 0.7954(3) 0.4189(3) -0.3245(2) 0.0246(6) Uani 1 1 d . . . H1WB H 0.7057 0.3946 -0.3547 0.030 Uiso 1 1 d R . . H1WA H 0.8295 0.4727 -0.3502 0.030 Uiso 1 1 d 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 Ag1 0.0309(2) 0.1105(4) 0.0292(2) 0.0304(2) 0.01295(16) 0.0341(2) La1 0.01485(14) 0.01368(13) 0.01366(13) 0.00444(9) 0.00417(9) 0.00554(9) C1 0.0164(18) 0.0239(18) 0.0175(17) 0.0086(15) 0.0034(14) 0.0055(15) C2 0.0170(18) 0.0201(18) 0.0208(18) 0.0057(15) 0.0061(15) 0.0059(15) C3 0.0185(18) 0.0244(18) 0.0162(17) 0.0060(14) 0.0060(15) 0.0042(15) C4 0.0166(17) 0.0191(17) 0.0174(17) 0.0078(14) 0.0021(14) 0.0045(14) C5 0.0147(17) 0.0209(18) 0.0226(18) 0.0074(15) 0.0046(15) 0.0058(14) C6 0.0205(18) 0.0191(18) 0.0180(17) 0.0057(14) 0.0052(15) 0.0069(15) C7 0.0189(18) 0.0273(19) 0.0161(17) 0.0071(15) 0.0042(14) 0.0065(15) C8 0.0204(18) 0.0166(17) 0.0219(18) 0.0061(14) 0.0091(15) 0.0074(14) C9 0.0190(19) 0.0254(19) 0.0188(18) 0.0066(15) 0.0066(15) 0.0072(16) C10 0.0206(19) 0.027(2) 0.0215(18) 0.0098(16) 0.0034(15) 0.0070(16) C11 0.024(2) 0.064(3) 0.027(2) 0.021(2) 0.0112(18) 0.017(2) C12 0.031(2) 0.073(3) 0.023(2) 0.021(2) 0.0085(19) 0.020(2) C13 0.024(2) 0.078(4) 0.034(2) 0.026(2) 0.0119(19) 0.012(2) C14 0.025(2) 0.065(3) 0.028(2) 0.025(2) 0.0081(18) 0.008(2) C15 0.0157(17) 0.0151(17) 0.0225(18) 0.0054(14) 0.0063(15) 0.0035(14) C16 0.0205(18) 0.0172(18) 0.0242(19) 0.0063(15) 0.0076(15) 0.0053(15) C17 0.0245(19) 0.0185(18) 0.0213(18) 0.0085(15) 0.0048(15) 0.0075(15) C18 0.0245(19) 0.0206(18) 0.0191(18) 0.0073(15) 0.0062(15) 0.0053(15) C19 0.027(2) 0.0170(18) 0.0229(18) 0.0050(15) 0.0098(16) 0.0078(16) C20 0.0213(18) 0.0188(18) 0.0231(18) 0.0094(15) 0.0077(15) 0.0074(15) C21 0.0212(18) 0.0176(17) 0.0170(16) 0.0056(14) 0.0036(14) 0.0042(15) C22 0.0167(17) 0.0158(17) 0.0223(18) 0.0068(15) 0.0036(15) 0.0031(14) C23 0.037(2) 0.024(2) 0.023(2) 0.0076(17) 0.0085(18) 0.0052(18) C24 0.035(2) 0.024(2) 0.0233(19) 0.0122(16) 0.0115(17) 0.0102(17) C25 0.029(2) 0.042(3) 0.030(2) 0.0110(19) 0.0079(18) 0.005(2) C26 0.032(2) 0.051(3) 0.032(2) 0.018(2) 0.0158(19) 0.011(2) C27 0.031(2) 0.056(3) 0.025(2) 0.017(2) 0.0049(18) 0.014(2) C28 0.033(2) 0.047(3) 0.027(2) 0.0185(19) 0.0147(18) 0.017(2) N1 0.0242(18) 0.053(2) 0.0260(18) 0.0139(17) 0.0019(15) 0.0128(17) N2 0.0166(15) 0.0257(16) 0.0210(16) 0.0096(13) 0.0020(13) 0.0009(13) N3 0.036(2) 0.052(2) 0.0251(18) 0.0187(17) 0.0127(16) 0.0222(19) N4 0.0318(18) 0.0157(15) 0.0154(15) 0.0027(12) 0.0020(13) 0.0010(13) O1 0.0152(13) 0.0363(15) 0.0188(13) 0.0071(12) 0.0022(11) 0.0051(12) O2 0.0182(13) 0.0414(17) 0.0240(14) 0.0005(13) 0.0092(11) 0.0058(13) O3 0.0262(15) 0.0558(19) 0.0202(14) 0.0183(13) 0.0105(12) 0.0220(14) O4 0.0190(13) 0.0230(13) 0.0203(12) 0.0064(10) 0.0085(10) 0.0083(11) O5 0.0235(14) 0.0387(17) 0.0252(14) 0.0151(13) 0.0078(12) 0.0029(13) O6 0.0256(14) 0.0187(13) 0.0210(13) 0.0034(11) 0.0038(11) 0.0039(11) O7 0.0216(13) 0.0129(12) 0.0298(14) 0.0065(11) 0.0068(11) 0.0055(10) O8 0.0385(16) 0.0226(14) 0.0301(14) 0.0123(12) 0.0188(13) 0.0181(13) O9 0.0280(14) 0.0222(13) 0.0238(13) 0.0105(11) 0.0113(11) 0.0113(11) O10 0.082(3) 0.037(2) 0.0299(18) 0.0033(15) 0.0186(19) -0.020(2) O1W 0.0229(14) 0.0289(14) 0.0213(13) 0.0106(11) 0.0077(11) 0.0083(12) _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 Ag1 N1 2.236(4) 1_767 ? Ag1 N3 2.246(3) . ? Ag1 O9 2.322(3) 1_556 ? La1 O7 2.472(2) 2_765 ? La1 O6 2.508(3) . ? La1 O8 2.511(3) 2_775 ? La1 O1 2.519(3) . ? La1 O3 2.524(3) 2_665 ? La1 O4 2.567(2) 1_655 ? La1 O1W 2.600(3) . ? La1 O4 2.698(2) 2_665 ? La1 O9 2.701(3) 2_775 ? La1 C22 2.949(4) 2_775 ? La1 C8 2.988(4) 2_665 ? C1 O2 1.252(5) . ? C1 O1 1.255(5) . ? C1 C2 1.505(5) . ? C2 C7 1.385(5) . ? C2 C3 1.392(5) . ? C3 C4 1.382(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(5) . ? C4 N2 1.417(5) . ? C5 C6 1.392(5) . ? C5 H5 0.9300 . ? C6 C7 1.389(5) . ? C6 C8 1.487(5) . ? C7 H7 0.9300 . ? C8 O3 1.249(5) . ? C8 O4 1.282(5) . ? C8 La1 2.988(4) 2_665 ? C9 O5 1.222(5) . ? C9 N2 1.338(5) . ? C9 C10 1.502(5) . ? C10 C11 1.378(6) . ? C10 C14 1.383(6) . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 N1 1.330(6) . ? C12 H12 0.9300 . ? C13 N1 1.338(6) . ? C13 C14 1.372(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.258(4) . ? C15 O7 1.259(4) . ? C15 C16 1.501(5) . ? C16 C17 1.385(5) . ? C16 C21 1.394(5) . ? C17 C18 1.387(5) . ? C17 H17 0.9300 . ? C18 C19 1.378(5) . ? C18 N4 1.430(5) . ? C19 C20 1.395(5) . ? C19 H19 0.9300 . ? C20 C21 1.378(5) . ? C20 C22 1.504(5) . ? C21 H21 0.9300 . ? C22 O8 1.249(5) . ? C22 O9 1.264(4) . ? C22 La1 2.949(4) 2_775 ? C23 O10 1.221(5) . ? C23 N4 1.339(5) . ? C23 C24 1.504(5) . ? C24 C28 1.379(6) . ? C24 C25 1.390(6) . ? C25 C26 1.369(6) . ? C25 H25 0.9300 . ? C26 N3 1.349(6) . ? C26 H26 0.9300 . ? C27 N3 1.328(6) . ? C27 C28 1.385(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 Ag1 2.236(4) 1_343 ? N2 H2 0.8600 . ? N4 H4 0.8600 . ? O3 La1 2.524(3) 2_665 ? O4 La1 2.567(2) 1_455 ? O4 La1 2.698(2) 2_665 ? O7 La1 2.472(2) 2_765 ? O8 La1 2.511(3) 2_775 ? O9 Ag1 2.322(3) 1_554 ? O9 La1 2.701(3) 2_775 ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 121.39(14) 1_767 . ? N1 Ag1 O9 124.30(12) 1_767 1_556 ? N3 Ag1 O9 106.76(12) . 1_556 ? O7 La1 O6 132.80(9) 2_765 . ? O7 La1 O8 142.09(9) 2_765 2_775 ? O6 La1 O8 76.56(9) . 2_775 ? O7 La1 O1 83.91(9) 2_765 . ? O6 La1 O1 141.78(9) . . ? O8 La1 O1 77.01(9) 2_775 . ? O7 La1 O3 77.73(10) 2_765 2_665 ? O6 La1 O3 105.52(9) . 2_665 ? O8 La1 O3 122.38(9) 2_775 2_665 ? O1 La1 O3 67.36(8) . 2_665 ? O7 La1 O4 68.99(8) 2_765 1_655 ? O6 La1 O4 69.44(8) . 1_655 ? O8 La1 O4 114.09(8) 2_775 1_655 ? O1 La1 O4 147.80(9) . 1_655 ? O3 La1 O4 120.36(8) 2_665 1_655 ? O7 La1 O1W 75.67(8) 2_765 . ? O6 La1 O1W 119.79(8) . . ? O8 La1 O1W 67.65(8) 2_775 . ? O1 La1 O1W 73.49(8) . . ? O3 La1 O1W 134.37(9) 2_665 . ? O4 La1 O1W 82.92(8) 1_655 . ? O7 La1 O4 79.38(8) 2_765 2_665 ? O6 La1 O4 69.67(8) . 2_665 ? O8 La1 O4 138.51(8) 2_775 2_665 ? O1 La1 O4 116.95(8) . 2_665 ? O3 La1 O4 49.77(8) 2_665 2_665 ? O4 La1 O4 75.85(8) 1_655 2_665 ? O1W La1 O4 151.73(8) . 2_665 ? O7 La1 O9 147.44(8) 2_765 2_775 ? O6 La1 O9 72.68(8) . 2_775 ? O8 La1 O9 49.85(8) 2_775 2_775 ? O1 La1 O9 69.20(9) . 2_775 ? O3 La1 O9 75.20(9) 2_665 2_775 ? O4 La1 O9 141.71(8) 1_655 2_775 ? O1W La1 O9 111.87(8) . 2_775 ? O4 La1 O9 96.32(8) 2_665 2_775 ? O7 La1 C22 151.13(9) 2_765 2_775 ? O6 La1 C22 76.00(9) . 2_775 ? O8 La1 C22 24.82(9) 2_775 2_775 ? O1 La1 C22 68.46(10) . 2_775 ? O3 La1 C22 98.20(10) 2_665 2_775 ? O4 La1 C22 133.34(9) 1_655 2_775 ? O1W La1 C22 88.17(9) . 2_775 ? O4 La1 C22 120.00(9) 2_665 2_775 ? O9 La1 C22 25.37(9) 2_775 2_775 ? O7 La1 C8 77.81(9) 2_765 2_665 ? O6 La1 C8 87.54(9) . 2_665 ? O8 La1 C8 134.47(9) 2_775 2_665 ? O1 La1 C8 91.69(9) . 2_665 ? O3 La1 C8 24.38(9) 2_665 2_665 ? O4 La1 C8 98.92(9) 1_655 2_665 ? O1W La1 C8 150.74(9) . 2_665 ? O4 La1 C8 25.40(9) 2_665 2_665 ? O9 La1 C8 84.77(9) 2_775 2_665 ? C22 La1 C8 110.10(10) 2_775 2_665 ? O7 La1 La1 70.05(6) 2_765 2_765 ? O6 La1 La1 63.73(6) . 2_765 ? O8 La1 La1 137.63(7) 2_775 2_765 ? O1 La1 La1 144.81(6) . 2_765 ? O3 La1 La1 83.85(6) 2_665 2_765 ? O4 La1 La1 39.03(5) 1_655 2_765 ? O1W La1 La1 119.72(6) . 2_765 ? O4 La1 La1 36.81(5) 2_665 2_765 ? O9 La1 La1 123.81(6) 2_775 2_765 ? C22 La1 La1 138.49(7) 2_775 2_765 ? C8 La1 La1 60.60(7) 2_665 2_765 ? O2 C1 O1 124.8(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 117.9(3) . . ? C7 C2 C3 119.9(3) . . ? C7 C2 C1 120.9(3) . . ? C3 C2 C1 118.9(3) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 N2 117.4(3) . . ? C3 C4 N2 122.1(3) . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.9(3) . . ? C7 C6 C8 121.2(3) . . ? C5 C6 C8 118.8(3) . . ? C2 C7 C6 120.0(3) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O3 C8 O4 121.1(3) . . ? O3 C8 C6 119.5(3) . . ? O4 C8 C6 119.5(3) . . ? O3 C8 La1 56.52(18) . 2_665 ? O4 C8 La1 64.58(18) . 2_665 ? C6 C8 La1 175.6(3) . 2_665 ? O5 C9 N2 123.8(3) . . ? O5 C9 C10 121.4(3) . . ? N2 C9 C10 114.8(3) . . ? C11 C10 C14 117.9(4) . . ? C11 C10 C9 119.1(4) . . ? C14 C10 C9 122.9(3) . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N1 C12 C11 123.5(4) . . ? N1 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? N1 C13 C14 123.1(4) . . ? N1 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C10 119.3(4) . . ? C13 C14 H14 120.3 . . ? C10 C14 H14 120.3 . . ? O6 C15 O7 125.5(3) . . ? O6 C15 C16 117.2(3) . . ? O7 C15 C16 117.3(3) . . ? C17 C16 C21 119.9(3) . . ? C17 C16 C15 120.5(3) . . ? C21 C16 C15 119.5(3) . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 N4 119.2(3) . . ? C17 C18 N4 120.9(3) . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 C22 121.0(3) . . ? C19 C20 C22 118.7(3) . . ? C20 C21 C16 119.7(3) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? O8 C22 O9 122.5(3) . . ? O8 C22 C20 117.2(3) . . ? O9 C22 C20 120.3(3) . . ? O8 C22 La1 57.55(18) . 2_775 ? O9 C22 La1 66.27(18) . 2_775 ? C20 C22 La1 166.4(2) . 2_775 ? O10 C23 N4 122.5(4) . . ? O10 C23 C24 119.1(4) . . ? N4 C23 C24 118.4(4) . . ? C28 C24 C25 118.5(4) . . ? C28 C24 C23 123.9(4) . . ? C25 C24 C23 117.6(4) . . ? C26 C25 C24 119.0(4) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N3 C26 C25 123.3(4) . . ? N3 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N3 C27 C28 123.9(4) . . ? N3 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? C24 C28 C27 118.4(4) . . ? C24 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C12 N1 C13 117.1(4) . . ? C12 N1 Ag1 115.9(3) . 1_343 ? C13 N1 Ag1 122.8(3) . 1_343 ? C9 N2 C4 125.4(3) . . ? C9 N2 H2 117.3 . . ? C4 N2 H2 117.3 . . ? C27 N3 C26 116.9(4) . . ? C27 N3 Ag1 122.2(3) . . ? C26 N3 Ag1 120.8(3) . . ? C23 N4 C18 121.4(3) . . ? C23 N4 H4 119.3 . . ? C18 N4 H4 119.3 . . ? C1 O1 La1 136.9(2) . . ? C8 O3 La1 99.1(2) . 2_665 ? C8 O4 La1 151.2(2) . 1_455 ? C8 O4 La1 90.0(2) . 2_665 ? La1 O4 La1 104.15(8) 1_455 2_665 ? C15 O6 La1 131.0(2) . . ? C15 O7 La1 128.7(2) . 2_765 ? C22 O8 La1 97.6(2) . 2_775 ? C22 O9 Ag1 118.7(2) . 1_554 ? C22 O9 La1 88.4(2) . 2_775 ? Ag1 O9 La1 107.05(10) 1_554 2_775 ? La1 O1W H1WB 106.5 . . ? La1 O1W H1WA 109.0 . . ? H1WB O1W H1WA 106.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 147.3(4) . . . . ? O1 C1 C2 C7 -30.7(5) . . . . ? O2 C1 C2 C3 -26.3(5) . . . . ? O1 C1 C2 C3 155.7(4) . . . . ? C7 C2 C3 C4 -0.9(6) . . . . ? C1 C2 C3 C4 172.8(3) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? C2 C3 C4 N2 -177.3(3) . . . . ? C3 C4 C5 C6 1.3(6) . . . . ? N2 C4 C5 C6 178.8(3) . . . . ? C4 C5 C6 C7 -1.8(5) . . . . ? C4 C5 C6 C8 -179.7(3) . . . . ? C3 C2 C7 C6 0.4(6) . . . . ? C1 C2 C7 C6 -173.1(3) . . . . ? C5 C6 C7 C2 0.9(6) . . . . ? C8 C6 C7 C2 178.8(3) . . . . ? C7 C6 C8 O3 -17.3(5) . . . . ? C5 C6 C8 O3 160.6(4) . . . . ? C7 C6 C8 O4 162.7(3) . . . . ? C5 C6 C8 O4 -19.3(5) . . . . ? C7 C6 C8 La1 -41(3) . . . 2_665 ? C5 C6 C8 La1 137(3) . . . 2_665 ? O5 C9 C10 C11 35.9(6) . . . . ? N2 C9 C10 C11 -145.4(4) . . . . ? O5 C9 C10 C14 -139.6(5) . . . . ? N2 C9 C10 C14 39.1(6) . . . . ? C14 C10 C11 C12 1.2(7) . . . . ? C9 C10 C11 C12 -174.4(4) . . . . ? C10 C11 C12 N1 1.9(8) . . . . ? N1 C13 C14 C10 2.0(9) . . . . ? C11 C10 C14 C13 -3.1(7) . . . . ? C9 C10 C14 C13 172.4(5) . . . . ? O6 C15 C16 C17 161.9(3) . . . . ? O7 C15 C16 C17 -17.3(5) . . . . ? O6 C15 C16 C21 -15.2(5) . . . . ? O7 C15 C16 C21 165.6(3) . . . . ? C21 C16 C17 C18 2.2(6) . . . . ? C15 C16 C17 C18 -174.9(4) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C16 C17 C18 N4 177.1(3) . . . . ? C17 C18 C19 C20 -1.6(6) . . . . ? N4 C18 C19 C20 -179.4(3) . . . . ? C18 C19 C20 C21 2.3(6) . . . . ? C18 C19 C20 C22 178.8(3) . . . . ? C19 C20 C21 C16 -0.7(6) . . . . ? C22 C20 C21 C16 -177.1(3) . . . . ? C17 C16 C21 C20 -1.5(6) . . . . ? C15 C16 C21 C20 175.6(3) . . . . ? C21 C20 C22 O8 152.0(4) . . . . ? C19 C20 C22 O8 -24.4(5) . . . . ? C21 C20 C22 O9 -28.6(5) . . . . ? C19 C20 C22 O9 155.0(4) . . . . ? C21 C20 C22 La1 -144.1(9) . . . 2_775 ? C19 C20 C22 La1 39.5(13) . . . 2_775 ? O10 C23 C24 C28 138.3(5) . . . . ? N4 C23 C24 C28 -42.9(6) . . . . ? O10 C23 C24 C25 -39.7(6) . . . . ? N4 C23 C24 C25 139.2(4) . . . . ? C28 C24 C25 C26 -0.8(7) . . . . ? C23 C24 C25 C26 177.3(4) . . . . ? C24 C25 C26 N3 -0.5(8) . . . . ? C25 C24 C28 C27 1.4(6) . . . . ? C23 C24 C28 C27 -176.6(4) . . . . ? N3 C27 C28 C24 -0.8(7) . . . . ? C11 C12 N1 C13 -3.0(8) . . . . ? C11 C12 N1 Ag1 154.7(4) . . . 1_343 ? C14 C13 N1 C12 1.0(8) . . . . ? C14 C13 N1 Ag1 -155.0(4) . . . 1_343 ? O5 C9 N2 C4 8.6(6) . . . . ? C10 C9 N2 C4 -170.0(3) . . . . ? C5 C4 N2 C9 137.6(4) . . . . ? C3 C4 N2 C9 -45.0(6) . . . . ? C28 C27 N3 C26 -0.4(7) . . . . ? C28 C27 N3 Ag1 -179.7(4) . . . . ? C25 C26 N3 C27 1.1(7) . . . . ? C25 C26 N3 Ag1 -179.6(4) . . . . ? N1 Ag1 N3 C27 -41.1(4) 1_767 . . . ? O9 Ag1 N3 C27 168.1(4) 1_556 . . . ? N1 Ag1 N3 C26 139.6(4) 1_767 . . . ? O9 Ag1 N3 C26 -11.2(4) 1_556 . . . ? O10 C23 N4 C18 6.6(7) . . . . ? C24 C23 N4 C18 -172.3(4) . . . . ? C19 C18 N4 C23 125.3(4) . . . . ? C17 C18 N4 C23 -52.4(6) . . . . ? O2 C1 O1 La1 -27.9(6) . . . . ? C2 C1 O1 La1 149.9(3) . . . . ? O7 La1 O1 C1 -47.8(4) 2_765 . . . ? O6 La1 O1 C1 146.5(3) . . . . ? O8 La1 O1 C1 99.2(4) 2_775 . . . ? O3 La1 O1 C1 -127.0(4) 2_665 . . . ? O4 La1 O1 C1 -15.6(4) 1_655 . . . ? O1W La1 O1 C1 29.0(3) . . . . ? O4 La1 O1 C1 -122.6(3) 2_665 . . . ? O9 La1 O1 C1 150.9(4) 2_775 . . . ? C22 La1 O1 C1 123.6(4) 2_775 . . . ? C8 La1 O1 C1 -125.4(4) 2_665 . . . ? La1 La1 O1 C1 -89.5(4) 2_765 . . . ? O4 C8 O3 La1 2.1(4) . . . 2_665 ? C6 C8 O3 La1 -177.8(3) . . . 2_665 ? O3 C8 O4 La1 118.7(4) . . . 1_455 ? C6 C8 O4 La1 -61.4(6) . . . 1_455 ? La1 C8 O4 La1 120.6(5) 2_665 . . 1_455 ? O3 C8 O4 La1 -1.9(4) . . . 2_665 ? C6 C8 O4 La1 178.0(3) . . . 2_665 ? O7 C15 O6 La1 67.6(5) . . . . ? C16 C15 O6 La1 -111.5(3) . . . . ? O7 La1 O6 C15 -52.4(3) 2_765 . . . ? O8 La1 O6 C15 155.4(3) 2_775 . . . ? O1 La1 O6 C15 108.0(3) . . . . ? O3 La1 O6 C15 35.1(3) 2_665 . . . ? O4 La1 O6 C15 -82.1(3) 1_655 . . . ? O1W La1 O6 C15 -150.6(3) . . . . ? O4 La1 O6 C15 -0.1(3) 2_665 . . . ? O9 La1 O6 C15 103.7(3) 2_775 . . . ? C22 La1 O6 C15 129.8(3) 2_775 . . . ? C8 La1 O6 C15 18.4(3) 2_665 . . . ? La1 La1 O6 C15 -39.8(3) 2_765 . . . ? O6 C15 O7 La1 -42.1(5) . . . 2_765 ? C16 C15 O7 La1 137.0(3) . . . 2_765 ? O9 C22 O8 La1 -13.9(4) . . . 2_775 ? C20 C22 O8 La1 165.5(3) . . . 2_775 ? O8 C22 O9 Ag1 121.4(3) . . . 1_554 ? C20 C22 O9 Ag1 -58.0(4) . . . 1_554 ? La1 C22 O9 Ag1 108.58(18) 2_775 . . 1_554 ? O8 C22 O9 La1 12.8(4) . . . 2_775 ? C20 C22 O9 La1 -166.5(3) . . . 2_775 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.745 _refine_diff_density_min -2.388 _refine_diff_density_rms 0.131 data_7 _database_code_depnum_ccdc_archive 'CCDC 760891' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 Ag N4 O11 Pr' _chemical_formula_weight 835.24 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 '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 10.499(2) _cell_length_b 11.141(2) _cell_length_c 13.738(3) _cell_angle_alpha 107.772(3) _cell_angle_beta 106.823(3) _cell_angle_gamma 102.759(4) _cell_volume 1377.9(5) _cell_formula_units_Z 2 _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 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 2.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6316 _exptl_absorpt_correction_T_max 0.7511 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6873 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4784 _reflns_number_gt 4628 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0700P)^2^+2.2675P] 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 4784 _refine_ls_number_parameters 406 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.11656(5) 0.76720(7) 1.44976(4) 0.06028(17) Uani 1 1 d . . . Pr1 Pr 0.636413(19) 0.453281(18) 0.612252(15) 0.01472(10) Uani 1 1 d U . . C1 C 0.3222(4) 0.2435(4) 0.3986(3) 0.0185(8) Uani 1 1 d . . . C2 C 0.2941(4) 0.1021(4) 0.3221(3) 0.0211(8) Uani 1 1 d . . . C3 C 0.2461(5) 0.0663(4) 0.2084(3) 0.0245(9) Uani 1 1 d . . . H3 H 0.2241 0.1273 0.1787 0.029 Uiso 1 1 calc R . . C4 C 0.2310(5) -0.0615(4) 0.1386(3) 0.0241(8) Uani 1 1 d . . . C5 C 0.2633(4) -0.1520(4) 0.1838(3) 0.0241(9) Uani 1 1 d . . . H5 H 0.2553 -0.2367 0.1379 0.029 Uiso 1 1 calc R . . C6 C 0.3075(4) -0.1164(4) 0.2974(3) 0.0213(8) Uani 1 1 d . . . C7 C 0.3233(4) 0.0100(4) 0.3671(3) 0.0215(8) Uani 1 1 d . . . H7 H 0.3530 0.0333 0.4431 0.026 Uiso 1 1 calc R . . C8 C 0.3429(4) -0.2164(4) 0.3437(3) 0.0207(8) Uani 1 1 d . . . C9 C 0.2558(5) -0.0227(5) -0.0199(4) 0.0327(10) Uani 1 1 d . . . C10 C 0.2165(5) -0.0775(5) -0.1431(4) 0.0299(10) Uani 1 1 d . . . C11 C 0.0797(5) -0.1419(5) -0.2204(4) 0.0357(11) Uani 1 1 d . . . H11 H 0.0045 -0.1582 -0.1979 0.043 Uiso 1 1 calc R . . C12 C 0.0560(6) -0.1814(6) -0.3306(4) 0.0431(13) Uani 1 1 d . . . H12 H -0.0369 -0.2239 -0.3816 0.052 Uiso 1 1 calc R . . C13 C 0.2941(5) -0.1004(6) -0.2922(4) 0.0406(12) Uani 1 1 d . . . H13 H 0.3682 -0.0870 -0.3163 0.049 Uiso 1 1 calc R . . C14 C 0.3252(5) -0.0571(5) -0.1809(4) 0.0390(11) Uani 1 1 d . . . H14 H 0.4186 -0.0144 -0.1308 0.047 Uiso 1 1 calc R . . C15 C 0.3267(4) 0.5677(4) 0.5970(3) 0.0207(8) Uani 1 1 d . . . C16 C 0.2983(4) 0.5840(4) 0.6996(3) 0.0191(8) Uani 1 1 d . . . C17 C 0.4120(4) 0.6318(4) 0.7998(3) 0.0210(8) Uani 1 1 d . . . H17 H 0.5039 0.6526 0.8022 0.025 Uiso 1 1 calc R . . C18 C 0.3878(4) 0.6482(4) 0.8961(3) 0.0207(8) Uani 1 1 d . . . C19 C 0.2511(4) 0.6196(4) 0.8931(3) 0.0220(8) Uani 1 1 d . . . H19 H 0.2355 0.6305 0.9581 0.026 Uiso 1 1 calc R . . C20 C 0.1371(4) 0.5743(4) 0.7929(3) 0.0215(8) Uani 1 1 d . . . C21 C 0.1601(4) 0.5556(4) 0.6958(3) 0.0214(8) Uani 1 1 d . . . H21 H 0.0842 0.5242 0.6286 0.026 Uiso 1 1 calc R . . C22 C -0.0092(4) 0.5599(4) 0.7934(3) 0.0217(8) Uani 1 1 d . . . C23 C 0.5216(4) 0.6537(4) 1.0770(3) 0.0242(9) Uani 1 1 d . . . C24 C 0.6679(4) 0.7094(4) 1.1665(4) 0.0258(9) Uani 1 1 d . . . C25 C 0.7892(5) 0.7296(6) 1.1439(4) 0.0417(12) Uani 1 1 d . . . H25 H 0.7833 0.7180 1.0726 0.050 Uiso 1 1 calc R . . C26 C 0.9173(5) 0.7664(7) 1.2265(5) 0.0492(15) Uani 1 1 d . . . H26 H 0.9973 0.7777 1.2092 0.059 Uiso 1 1 calc R . . C27 C 0.8158(6) 0.7714(6) 1.3529(4) 0.0448(13) Uani 1 1 d . . . H27 H 0.8246 0.7877 1.4255 0.054 Uiso 1 1 calc R . . C28 C 0.6832(5) 0.7328(6) 1.2740(4) 0.0385(12) Uani 1 1 d . . . H28 H 0.6046 0.7226 1.2930 0.046 Uiso 1 1 calc R . . N1 N 0.1599(5) -0.1621(5) -0.3690(3) 0.0388(10) Uani 1 1 d . . . N2 N 0.1881(4) -0.0988(4) 0.0223(3) 0.0267(8) Uani 1 1 d . . . H2 H 0.1179 -0.1710 -0.0220 0.032 Uiso 1 1 calc R . . N3 N 0.9337(4) 0.7871(5) 1.3313(3) 0.0398(10) Uani 1 1 d . . . N4 N 0.5073(4) 0.6997(4) 0.9968(3) 0.0250(8) Uani 1 1 d . . . H4 H 0.5767 0.7663 1.0070 0.030 Uiso 1 1 calc R . . O1 O 0.4005(3) 0.2808(3) 0.4983(2) 0.0259(6) Uani 1 1 d . . . O2 O 0.2648(3) 0.3135(3) 0.3568(2) 0.0233(6) Uani 1 1 d . . . O3 O 0.3328(3) -0.2132(3) 0.4333(2) 0.0235(6) Uani 1 1 d . . . O4 O 0.3826(3) -0.3025(3) 0.2887(2) 0.0263(6) Uani 1 1 d . . . O5 O 0.3462(5) 0.0862(4) 0.0377(3) 0.0645(14) Uani 1 1 d . . . O6 O 0.4458(3) 0.5611(3) 0.5960(2) 0.0215(6) Uani 1 1 d . . . O7 O 0.2331(3) 0.5626(4) 0.5131(2) 0.0311(7) Uani 1 1 d . . . O8 O -0.0173(3) 0.6322(3) 0.8800(3) 0.0333(7) Uani 1 1 d . . . O9 O -0.1127(3) 0.4794(3) 0.7065(2) 0.0265(6) Uani 1 1 d . . . O10 O 0.4250(3) 0.5708(3) 1.0797(3) 0.0328(7) Uani 1 1 d . . . O1W O 0.7012(3) 0.5811(3) 0.8191(2) 0.0242(6) Uani 1 1 d U . . H1WB H 0.7854 0.6344 0.8432 0.029 Uiso 1 1 d R . . H1WA H 0.7061 0.5232 0.8472 0.029 Uiso 1 1 d 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 Ag1 0.0353(2) 0.1271(5) 0.0351(2) 0.0387(3) 0.01884(19) 0.0414(3) Pr1 0.01714(14) 0.01509(14) 0.01728(14) 0.00880(10) 0.00876(10) 0.00897(9) C1 0.0191(18) 0.0155(18) 0.026(2) 0.0115(16) 0.0129(16) 0.0058(15) C2 0.023(2) 0.0176(19) 0.026(2) 0.0097(16) 0.0108(17) 0.0092(16) C3 0.031(2) 0.021(2) 0.025(2) 0.0132(17) 0.0100(18) 0.0126(17) C4 0.029(2) 0.023(2) 0.024(2) 0.0126(17) 0.0119(17) 0.0095(17) C5 0.031(2) 0.021(2) 0.026(2) 0.0113(17) 0.0137(18) 0.0113(17) C6 0.0220(19) 0.022(2) 0.026(2) 0.0133(17) 0.0108(16) 0.0105(16) C7 0.025(2) 0.0202(19) 0.0219(19) 0.0118(16) 0.0094(16) 0.0079(16) C8 0.0203(19) 0.0186(19) 0.026(2) 0.0113(16) 0.0090(16) 0.0068(16) C9 0.042(3) 0.031(2) 0.027(2) 0.0144(19) 0.014(2) 0.009(2) C10 0.038(3) 0.030(2) 0.030(2) 0.0177(19) 0.017(2) 0.0142(19) C11 0.038(3) 0.051(3) 0.032(2) 0.023(2) 0.020(2) 0.021(2) C12 0.033(3) 0.070(4) 0.035(3) 0.027(3) 0.015(2) 0.022(3) C13 0.037(3) 0.055(3) 0.041(3) 0.025(2) 0.023(2) 0.018(2) C14 0.034(3) 0.045(3) 0.035(3) 0.016(2) 0.014(2) 0.009(2) C15 0.028(2) 0.0169(18) 0.025(2) 0.0083(16) 0.0164(17) 0.0116(16) C16 0.0220(19) 0.0217(19) 0.0207(19) 0.0116(16) 0.0118(16) 0.0106(16) C17 0.0196(19) 0.027(2) 0.024(2) 0.0140(17) 0.0111(16) 0.0125(16) C18 0.0209(19) 0.023(2) 0.0201(19) 0.0110(16) 0.0068(16) 0.0079(16) C19 0.023(2) 0.028(2) 0.0195(19) 0.0115(16) 0.0107(16) 0.0101(17) C20 0.0192(19) 0.027(2) 0.024(2) 0.0114(17) 0.0119(16) 0.0103(16) C21 0.0200(19) 0.026(2) 0.0194(19) 0.0086(16) 0.0084(16) 0.0095(16) C22 0.022(2) 0.028(2) 0.022(2) 0.0148(17) 0.0107(17) 0.0110(17) C23 0.025(2) 0.030(2) 0.022(2) 0.0116(17) 0.0126(17) 0.0116(18) C24 0.026(2) 0.032(2) 0.027(2) 0.0169(18) 0.0114(18) 0.0133(18) C25 0.033(3) 0.068(4) 0.035(3) 0.030(3) 0.018(2) 0.017(2) C26 0.027(3) 0.084(4) 0.040(3) 0.029(3) 0.015(2) 0.015(3) C27 0.035(3) 0.076(4) 0.026(2) 0.020(3) 0.012(2) 0.022(3) C28 0.026(2) 0.067(3) 0.030(2) 0.023(2) 0.014(2) 0.020(2) N1 0.040(2) 0.060(3) 0.033(2) 0.026(2) 0.0202(19) 0.028(2) N2 0.036(2) 0.0199(17) 0.0202(17) 0.0077(14) 0.0086(15) 0.0053(15) N3 0.028(2) 0.059(3) 0.032(2) 0.020(2) 0.0072(17) 0.0166(19) N4 0.0170(17) 0.0319(19) 0.0249(18) 0.0152(15) 0.0050(14) 0.0045(14) O1 0.0284(15) 0.0209(14) 0.0248(15) 0.0076(12) 0.0080(13) 0.0067(12) O2 0.0223(14) 0.0181(14) 0.0323(16) 0.0130(12) 0.0089(12) 0.0095(11) O3 0.0304(15) 0.0241(14) 0.0274(15) 0.0150(12) 0.0167(13) 0.0157(12) O4 0.0409(17) 0.0239(15) 0.0325(16) 0.0186(13) 0.0236(14) 0.0218(13) O5 0.089(3) 0.040(2) 0.038(2) 0.0079(18) 0.028(2) -0.021(2) O6 0.0197(14) 0.0266(15) 0.0245(14) 0.0104(12) 0.0131(11) 0.0128(12) O7 0.0296(16) 0.055(2) 0.0243(15) 0.0224(15) 0.0163(13) 0.0263(15) O8 0.0222(15) 0.0435(19) 0.0290(16) 0.0048(14) 0.0140(13) 0.0097(14) O9 0.0174(14) 0.0372(17) 0.0234(15) 0.0103(13) 0.0069(12) 0.0103(13) O10 0.0287(16) 0.0425(19) 0.0305(17) 0.0203(15) 0.0134(13) 0.0069(14) O1W 0.0241(15) 0.0281(15) 0.0277(15) 0.0140(12) 0.0133(12) 0.0132(12) _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 Ag1 N3 2.232(4) . ? Ag1 N1 2.239(4) 1_667 ? Ag1 O3 2.315(3) 1_666 ? Pr1 O2 2.426(3) 2_666 ? Pr1 O1 2.468(3) . ? Pr1 O4 2.473(3) 2_656 ? Pr1 O9 2.481(3) 1_655 ? Pr1 O7 2.482(3) 2_666 ? Pr1 O6 2.542(3) . ? Pr1 O1W 2.559(3) . ? Pr1 O3 2.669(3) 2_656 ? Pr1 O6 2.680(3) 2_666 ? Pr1 C8 2.920(4) 2_656 ? Pr1 C15 2.956(4) 2_666 ? C1 O1 1.255(5) . ? C1 O2 1.258(5) . ? C1 C2 1.508(5) . ? C2 C3 1.389(6) . ? C2 C7 1.396(6) . ? C3 C4 1.397(6) . ? C3 H3 0.9300 . ? C4 C5 1.388(6) . ? C4 N2 1.424(5) . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 C7 1.382(6) . ? C6 C8 1.504(5) . ? C7 H7 0.9300 . ? C8 O4 1.256(5) . ? C8 O3 1.258(5) . ? C8 Pr1 2.920(4) 2_656 ? C9 O5 1.212(6) . ? C9 N2 1.353(6) . ? C9 C10 1.505(6) . ? C10 C11 1.379(7) . ? C10 C14 1.386(7) . ? C11 C12 1.368(7) . ? C11 H11 0.9300 . ? C12 N1 1.348(7) . ? C12 H12 0.9300 . ? C13 N1 1.356(7) . ? C13 C14 1.367(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.256(5) . ? C15 O6 1.273(5) . ? C15 C16 1.491(5) . ? C15 Pr1 2.956(4) 2_666 ? C16 C17 1.386(6) . ? C16 C21 1.397(6) . ? C17 C18 1.384(6) . ? C17 H17 0.9300 . ? C18 C19 1.385(6) . ? C18 N4 1.418(5) . ? C19 C20 1.393(6) . ? C19 H19 0.9300 . ? C20 C21 1.385(6) . ? C20 C22 1.511(5) . ? C21 H21 0.9300 . ? C22 O8 1.255(5) . ? C22 O9 1.256(5) . ? C23 O10 1.230(5) . ? C23 N4 1.335(6) . ? C23 C24 1.508(6) . ? C24 C28 1.373(6) . ? C24 C25 1.384(7) . ? C25 C26 1.361(7) . ? C25 H25 0.9300 . ? C26 N3 1.339(7) . ? C26 H26 0.9300 . ? C27 N3 1.341(7) . ? C27 C28 1.369(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 Ag1 2.239(4) 1_443 ? N2 H2 0.8600 . ? N4 H4 0.8600 . ? O2 Pr1 2.426(3) 2_666 ? O3 Ag1 2.315(3) 1_444 ? O3 Pr1 2.669(3) 2_656 ? O4 Pr1 2.473(3) 2_656 ? O6 Pr1 2.680(3) 2_666 ? O7 Pr1 2.482(3) 2_666 ? O9 Pr1 2.481(3) 1_455 ? O1W H1WB 0.8500 . ? O1W H1WA 0.8501 . ? 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 N3 Ag1 N1 121.60(16) . 1_667 ? N3 Ag1 O3 124.05(13) . 1_666 ? N1 Ag1 O3 106.71(13) 1_667 1_666 ? O2 Pr1 O1 133.19(10) 2_666 . ? O2 Pr1 O4 142.14(10) 2_666 2_656 ? O1 Pr1 O4 76.10(10) . 2_656 ? O2 Pr1 O9 83.47(10) 2_666 1_655 ? O1 Pr1 O9 141.80(10) . 1_655 ? O4 Pr1 O9 77.60(10) 2_656 1_655 ? O2 Pr1 O7 78.32(11) 2_666 2_666 ? O1 Pr1 O7 104.94(11) . 2_666 ? O4 Pr1 O7 122.15(10) 2_656 2_666 ? O9 Pr1 O7 67.42(10) 1_655 2_666 ? O2 Pr1 O6 69.52(9) 2_666 . ? O1 Pr1 O6 69.65(10) . . ? O4 Pr1 O6 112.94(9) 2_656 . ? O9 Pr1 O6 147.41(10) 1_655 . ? O7 Pr1 O6 121.53(9) 2_666 . ? O2 Pr1 O1W 75.81(10) 2_666 . ? O1 Pr1 O1W 119.50(10) . . ? O4 Pr1 O1W 67.56(10) 2_656 . ? O9 Pr1 O1W 73.74(9) 1_655 . ? O7 Pr1 O1W 135.17(10) 2_666 . ? O6 Pr1 O1W 81.98(9) . . ? O2 Pr1 O3 147.45(9) 2_666 2_656 ? O1 Pr1 O3 71.93(10) . 2_656 ? O4 Pr1 O3 50.46(9) 2_656 2_656 ? O9 Pr1 O3 70.00(10) 1_655 2_656 ? O7 Pr1 O3 74.34(10) 2_666 2_656 ? O6 Pr1 O3 141.11(9) . 2_656 ? O1W Pr1 O3 112.54(9) . 2_656 ? O2 Pr1 O6 78.84(9) 2_666 2_666 ? O1 Pr1 O6 69.89(9) . 2_666 ? O4 Pr1 O6 139.02(9) 2_656 2_666 ? O9 Pr1 O6 117.34(9) 1_655 2_666 ? O7 Pr1 O6 50.27(9) 2_666 2_666 ? O6 Pr1 O6 75.91(9) . 2_666 ? O1W Pr1 O6 150.90(9) . 2_666 ? O3 Pr1 O6 96.52(8) 2_656 2_666 ? O2 Pr1 C8 151.71(10) 2_666 2_656 ? O1 Pr1 C8 75.05(10) . 2_656 ? O4 Pr1 C8 25.24(10) 2_656 2_656 ? O9 Pr1 C8 69.37(11) 1_655 2_656 ? O7 Pr1 C8 97.59(11) 2_666 2_656 ? O6 Pr1 C8 132.33(10) . 2_656 ? O1W Pr1 C8 88.72(10) . 2_656 ? O3 Pr1 C8 25.50(10) 2_656 2_656 ? O6 Pr1 C8 120.19(10) 2_666 2_656 ? O2 Pr1 C15 77.69(10) 2_666 2_666 ? O1 Pr1 C15 87.29(11) . 2_666 ? O4 Pr1 C15 134.86(10) 2_656 2_666 ? O9 Pr1 C15 92.07(11) 1_655 2_666 ? O7 Pr1 C15 24.78(11) 2_666 2_666 ? O6 Pr1 C15 99.34(10) . 2_666 ? O1W Pr1 C15 151.11(10) . 2_666 ? O3 Pr1 C15 84.59(9) 2_656 2_666 ? O6 Pr1 C15 25.50(10) 2_666 2_666 ? C8 Pr1 C15 110.07(11) 2_656 2_666 ? O2 Pr1 Pr1 70.01(7) 2_666 2_666 ? O1 Pr1 Pr1 64.00(7) . 2_666 ? O4 Pr1 Pr1 137.04(7) 2_656 2_666 ? O9 Pr1 Pr1 144.97(7) 1_655 2_666 ? O7 Pr1 Pr1 84.66(7) 2_666 2_666 ? O6 Pr1 Pr1 39.13(6) . 2_666 ? O1W Pr1 Pr1 118.85(6) . 2_666 ? O3 Pr1 Pr1 123.66(6) 2_656 2_666 ? O6 Pr1 Pr1 36.77(6) 2_666 2_666 ? C8 Pr1 Pr1 137.98(8) 2_656 2_666 ? C15 Pr1 Pr1 60.84(8) 2_666 2_666 ? O1 C1 O2 125.7(4) . . ? O1 C1 C2 117.2(3) . . ? O2 C1 C2 117.1(4) . . ? C3 C2 C7 120.5(4) . . ? C3 C2 C1 120.1(4) . . ? C7 C2 C1 119.3(4) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 N2 119.4(4) . . ? C3 C4 N2 121.0(4) . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.8(4) . . ? C7 C6 C8 120.5(4) . . ? C5 C6 C8 118.7(4) . . ? C6 C7 C2 119.2(4) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? O4 C8 O3 122.0(4) . . ? O4 C8 C6 117.0(4) . . ? O3 C8 C6 121.0(4) . . ? O4 C8 Pr1 57.1(2) . 2_656 ? O3 C8 Pr1 66.0(2) . 2_656 ? C6 C8 Pr1 167.5(3) . 2_656 ? O5 C9 N2 122.6(4) . . ? O5 C9 C10 119.5(4) . . ? N2 C9 C10 117.9(4) . . ? C11 C10 C14 118.2(4) . . ? C11 C10 C9 124.4(4) . . ? C14 C10 C9 117.4(4) . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N1 C12 C11 123.5(5) . . ? N1 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? N1 C13 C14 122.9(5) . . ? N1 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C13 C14 C10 119.5(5) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? O7 C15 O6 121.0(4) . . ? O7 C15 C16 119.3(4) . . ? O6 C15 C16 119.7(4) . . ? O7 C15 Pr1 56.0(2) . 2_666 ? O6 C15 Pr1 65.0(2) . 2_666 ? C16 C15 Pr1 174.8(3) . 2_666 ? C17 C16 C21 120.4(4) . . ? C17 C16 C15 118.8(4) . . ? C21 C16 C15 120.8(4) . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 120.4(4) . . ? C19 C18 N4 121.9(4) . . ? C17 C18 N4 117.6(4) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 C22 120.7(4) . . ? C19 C20 C22 119.0(4) . . ? C20 C21 C16 119.5(4) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? O8 C22 O9 125.2(4) . . ? O8 C22 C20 117.2(4) . . ? O9 C22 C20 117.5(4) . . ? O10 C23 N4 123.9(4) . . ? O10 C23 C24 120.7(4) . . ? N4 C23 C24 115.3(4) . . ? C28 C24 C25 117.7(4) . . ? C28 C24 C23 119.6(4) . . ? C25 C24 C23 122.6(4) . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? N3 C26 C25 123.2(5) . . ? N3 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N3 C27 C28 123.6(5) . . ? N3 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? C27 C28 C24 119.2(4) . . ? C27 C28 H28 120.4 . . ? C24 C28 H28 120.4 . . ? C12 N1 C13 116.6(4) . . ? C12 N1 Ag1 122.3(4) . 1_443 ? C13 N1 Ag1 121.1(3) . 1_443 ? C9 N2 C4 121.1(4) . . ? C9 N2 H2 119.4 . . ? C4 N2 H2 119.4 . . ? C26 N3 C27 116.4(4) . . ? C26 N3 Ag1 123.2(4) . . ? C27 N3 Ag1 116.1(3) . . ? C23 N4 C18 125.8(4) . . ? C23 N4 H4 117.1 . . ? C18 N4 H4 117.1 . . ? C1 O1 Pr1 131.4(3) . . ? C1 O2 Pr1 129.1(2) . 2_666 ? C8 O3 Ag1 119.2(3) . 1_444 ? C8 O3 Pr1 88.5(2) . 2_656 ? Ag1 O3 Pr1 107.99(11) 1_444 2_656 ? C8 O4 Pr1 97.7(2) . 2_656 ? C15 O6 Pr1 152.8(3) . . ? C15 O6 Pr1 89.5(2) . 2_666 ? Pr1 O6 Pr1 104.09(9) . 2_666 ? C15 O7 Pr1 99.3(2) . 2_666 ? C22 O9 Pr1 137.6(3) . 1_455 ? Pr1 O1W H1WB 105.1 . . ? Pr1 O1W H1WA 105.1 . . ? H1WB O1W H1WA 106.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -160.6(4) . . . . ? O2 C1 C2 C3 19.5(6) . . . . ? O1 C1 C2 C7 16.3(5) . . . . ? O2 C1 C2 C7 -163.6(4) . . . . ? C7 C2 C3 C4 -2.0(6) . . . . ? C1 C2 C3 C4 174.9(4) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C2 C3 C4 N2 -177.2(4) . . . . ? C3 C4 C5 C6 1.3(6) . . . . ? N2 C4 C5 C6 179.0(4) . . . . ? C4 C5 C6 C7 -1.6(6) . . . . ? C4 C5 C6 C8 -179.4(4) . . . . ? C5 C6 C7 C2 0.0(6) . . . . ? C8 C6 C7 C2 177.9(4) . . . . ? C3 C2 C7 C6 1.7(6) . . . . ? C1 C2 C7 C6 -175.2(4) . . . . ? C7 C6 C8 O4 -151.7(4) . . . . ? C5 C6 C8 O4 26.2(6) . . . . ? C7 C6 C8 O3 28.4(6) . . . . ? C5 C6 C8 O3 -153.7(4) . . . . ? C7 C6 C8 Pr1 149.7(11) . . . 2_656 ? C5 C6 C8 Pr1 -32.4(15) . . . 2_656 ? O5 C9 C10 C11 -137.5(6) . . . . ? N2 C9 C10 C11 42.8(7) . . . . ? O5 C9 C10 C14 40.0(7) . . . . ? N2 C9 C10 C14 -139.7(5) . . . . ? C14 C10 C11 C12 -0.9(7) . . . . ? C9 C10 C11 C12 176.6(5) . . . . ? C10 C11 C12 N1 0.6(9) . . . . ? N1 C13 C14 C10 0.7(8) . . . . ? C11 C10 C14 C13 0.3(8) . . . . ? C9 C10 C14 C13 -177.4(5) . . . . ? O7 C15 C16 C17 -159.6(4) . . . . ? O6 C15 C16 C17 19.4(6) . . . . ? Pr1 C15 C16 C17 -135(3) 2_666 . . . ? O7 C15 C16 C21 18.6(6) . . . . ? O6 C15 C16 C21 -162.5(4) . . . . ? Pr1 C15 C16 C21 43(3) 2_666 . . . ? C21 C16 C17 C18 1.5(6) . . . . ? C15 C16 C17 C18 179.7(4) . . . . ? C16 C17 C18 C19 -1.1(6) . . . . ? C16 C17 C18 N4 -178.9(4) . . . . ? C17 C18 C19 C20 -0.2(6) . . . . ? N4 C18 C19 C20 177.4(4) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C18 C19 C20 C22 -172.6(4) . . . . ? C19 C20 C21 C16 -0.8(6) . . . . ? C22 C20 C21 C16 172.9(4) . . . . ? C17 C16 C21 C20 -0.5(6) . . . . ? C15 C16 C21 C20 -178.7(4) . . . . ? C21 C20 C22 O8 -148.1(4) . . . . ? C19 C20 C22 O8 25.7(6) . . . . ? C21 C20 C22 O9 30.1(6) . . . . ? C19 C20 C22 O9 -156.2(4) . . . . ? O10 C23 C24 C28 -36.5(6) . . . . ? N4 C23 C24 C28 144.2(5) . . . . ? O10 C23 C24 C25 138.8(5) . . . . ? N4 C23 C24 C25 -40.4(6) . . . . ? C28 C24 C25 C26 2.5(8) . . . . ? C23 C24 C25 C26 -173.0(5) . . . . ? C24 C25 C26 N3 -1.2(10) . . . . ? N3 C27 C28 C24 -0.6(9) . . . . ? C25 C24 C28 C27 -1.6(8) . . . . ? C23 C24 C28 C27 174.0(5) . . . . ? C11 C12 N1 C13 0.3(8) . . . . ? C11 C12 N1 Ag1 178.5(4) . . . 1_443 ? C14 C13 N1 C12 -1.0(8) . . . . ? C14 C13 N1 Ag1 -179.2(4) . . . 1_443 ? O5 C9 N2 C4 -7.3(8) . . . . ? C10 C9 N2 C4 172.3(4) . . . . ? C5 C4 N2 C9 -125.4(5) . . . . ? C3 C4 N2 C9 52.3(6) . . . . ? C25 C26 N3 C27 -0.9(10) . . . . ? C25 C26 N3 Ag1 154.9(5) . . . . ? C28 C27 N3 C26 1.8(9) . . . . ? C28 C27 N3 Ag1 -155.8(5) . . . . ? N1 Ag1 N3 C26 168.8(5) 1_667 . . . ? O3 Ag1 N3 C26 23.4(5) 1_666 . . . ? N1 Ag1 N3 C27 -35.2(5) 1_667 . . . ? O3 Ag1 N3 C27 179.3(4) 1_666 . . . ? O10 C23 N4 C18 -9.4(7) . . . . ? C24 C23 N4 C18 169.8(4) . . . . ? C19 C18 N4 C23 46.1(6) . . . . ? C17 C18 N4 C23 -136.2(4) . . . . ? O2 C1 O1 Pr1 -65.5(5) . . . . ? C2 C1 O1 Pr1 114.6(3) . . . . ? O2 Pr1 O1 C1 49.5(4) 2_666 . . . ? O4 Pr1 O1 C1 -158.4(4) 2_656 . . . ? O9 Pr1 O1 C1 -110.7(3) 1_655 . . . ? O7 Pr1 O1 C1 -38.3(4) 2_666 . . . ? O6 Pr1 O1 C1 80.2(3) . . . . ? O1W Pr1 O1 C1 147.9(3) . . . . ? O3 Pr1 O1 C1 -106.0(3) 2_656 . . . ? O6 Pr1 O1 C1 -1.7(3) 2_666 . . . ? C8 Pr1 O1 C1 -132.4(4) 2_656 . . . ? C15 Pr1 O1 C1 -20.8(3) 2_666 . . . ? Pr1 Pr1 O1 C1 37.9(3) 2_666 . . . ? O1 C1 O2 Pr1 42.3(5) . . . 2_666 ? C2 C1 O2 Pr1 -137.8(3) . . . 2_666 ? O4 C8 O3 Ag1 -121.4(4) . . . 1_444 ? C6 C8 O3 Ag1 58.5(4) . . . 1_444 ? Pr1 C8 O3 Ag1 -109.8(2) 2_656 . . 1_444 ? O4 C8 O3 Pr1 -11.6(4) . . . 2_656 ? C6 C8 O3 Pr1 168.3(3) . . . 2_656 ? O3 C8 O4 Pr1 12.6(4) . . . 2_656 ? C6 C8 O4 Pr1 -167.3(3) . . . 2_656 ? O7 C15 O6 Pr1 -119.7(5) . . . . ? C16 C15 O6 Pr1 61.4(7) . . . . ? Pr1 C15 O6 Pr1 -121.0(5) 2_666 . . . ? O7 C15 O6 Pr1 1.4(4) . . . 2_666 ? C16 C15 O6 Pr1 -177.6(3) . . . 2_666 ? O2 Pr1 O6 C15 -158.9(6) 2_666 . . . ? O1 Pr1 O6 C15 44.5(6) . . . . ? O4 Pr1 O6 C15 -19.7(6) 2_656 . . . ? O9 Pr1 O6 C15 -122.9(5) 1_655 . . . ? O7 Pr1 O6 C15 140.0(5) 2_666 . . . ? O1W Pr1 O6 C15 -81.1(6) . . . . ? O3 Pr1 O6 C15 35.1(6) 2_656 . . . ? O6 Pr1 O6 C15 118.0(6) 2_666 . . . ? C8 Pr1 O6 C15 -0.3(6) 2_656 . . . ? C15 Pr1 O6 C15 128.1(5) 2_666 . . . ? Pr1 Pr1 O6 C15 118.0(6) 2_666 . . . ? O2 Pr1 O6 Pr1 83.15(11) 2_666 . . 2_666 ? O1 Pr1 O6 Pr1 -73.44(11) . . . 2_666 ? O4 Pr1 O6 Pr1 -137.64(10) 2_656 . . 2_666 ? O9 Pr1 O6 Pr1 119.11(16) 1_655 . . 2_666 ? O7 Pr1 O6 Pr1 22.01(15) 2_666 . . 2_666 ? O1W Pr1 O6 Pr1 160.93(11) . . . 2_666 ? O3 Pr1 O6 Pr1 -82.83(15) 2_656 . . 2_666 ? O6 Pr1 O6 Pr1 0.0 2_666 . . 2_666 ? C8 Pr1 O6 Pr1 -118.21(13) 2_656 . . 2_666 ? C15 Pr1 O6 Pr1 10.13(12) 2_666 . . 2_666 ? O6 C15 O7 Pr1 -1.5(4) . . . 2_666 ? C16 C15 O7 Pr1 177.4(3) . . . 2_666 ? O8 C22 O9 Pr1 26.0(7) . . . 1_455 ? C20 C22 O9 Pr1 -151.9(3) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.613 _refine_diff_density_min -2.977 _refine_diff_density_rms 0.155 data_8 _database_code_depnum_ccdc_archive 'CCDC 760892' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H18 Ag N4 Nd O11' _chemical_formula_weight 838.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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' H H 0.0000 0.0000 '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 10.4585(11) _cell_length_b 11.0901(12) _cell_length_c 13.6890(15) _cell_angle_alpha 107.747(2) _cell_angle_beta 106.8520(10) _cell_angle_gamma 102.640(2) _cell_volume 1362.6(3) _cell_formula_units_Z 2 _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 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 2.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6445 _exptl_absorpt_correction_T_max 0.7757 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6953 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4847 _reflns_number_gt 4468 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0484P)^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 4847 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.11620(4) -0.26702(6) 0.05076(3) 0.05461(16) Uani 1 1 d . . . Nd1 Nd 1.36393(2) 0.04657(2) 0.888277(16) 0.01395(9) Uani 1 1 d . . . C1 C 1.3225(4) 0.7433(4) 0.8988(3) 0.0175(8) Uani 1 1 d . . . C2 C 1.2937(4) 0.6021(4) 0.8231(3) 0.0194(9) Uani 1 1 d . . . C3 C 1.2459(5) 0.5659(4) 0.7094(3) 0.0221(9) Uani 1 1 d . . . H3 H 1.2238 0.6271 0.6795 0.027 Uiso 1 1 calc R . . C4 C 1.2310(5) 0.4384(4) 0.6401(3) 0.0217(9) Uani 1 1 d . . . C5 C 1.2635(5) 0.3475(4) 0.6844(3) 0.0235(9) Uani 1 1 d . . . H5 H 1.2557 0.2628 0.6382 0.028 Uiso 1 1 calc R . . C6 C 1.3079(4) 0.3830(4) 0.7985(3) 0.0188(9) Uani 1 1 d . . . C7 C 1.3232(4) 0.5095(4) 0.8673(3) 0.0203(9) Uani 1 1 d . . . H7 H 1.3534 0.5330 0.9436 0.024 Uiso 1 1 calc R . . C8 C 1.3439(4) 0.2832(4) 0.8443(3) 0.0194(9) Uani 1 1 d . . . C9 C 1.2549(5) 0.4761(5) 0.4802(4) 0.0284(10) Uani 1 1 d . . . C10 C 1.2166(5) 0.4224(5) 0.3571(4) 0.0285(10) Uani 1 1 d . . . C11 C 1.3245(5) 0.4426(5) 0.3190(4) 0.0342(11) Uani 1 1 d . . . H11 H 1.4183 0.4861 0.3689 0.041 Uiso 1 1 calc R . . C12 C 1.2926(6) 0.3981(5) 0.2073(4) 0.0374(12) Uani 1 1 d . . . H12 H 1.3668 0.4098 0.1828 0.045 Uiso 1 1 calc R . . C13 C 1.0558(5) 0.3191(6) 0.1690(4) 0.0383(12) Uani 1 1 d . . . H13 H 0.9627 0.2764 0.1176 0.046 Uiso 1 1 calc R . . C14 C 1.0794(5) 0.3589(5) 0.2795(4) 0.0330(11) Uani 1 1 d . . . H14 H 1.0038 0.3434 0.3021 0.040 Uiso 1 1 calc R . . C15 C 0.6730(4) -0.0671(4) 0.9037(3) 0.0186(9) Uani 1 1 d . . . C16 C 0.7024(4) -0.0835(4) 0.8008(3) 0.0176(8) Uani 1 1 d . . . C17 C 0.8404(4) -0.0553(4) 0.8045(3) 0.0189(9) Uani 1 1 d . . . H17 H 0.9163 -0.0242 0.8721 0.023 Uiso 1 1 calc R . . C18 C 0.8650(4) -0.0731(4) 0.7080(3) 0.0192(9) Uani 1 1 d . . . C19 C 0.7498(4) -0.1194(4) 0.6071(3) 0.0200(9) Uani 1 1 d . . . H19 H 0.7652 -0.1312 0.5418 0.024 Uiso 1 1 calc R . . C20 C 0.6144(4) -0.1474(4) 0.6043(3) 0.0185(8) Uani 1 1 d . . . C21 C 0.5892(4) -0.1326(4) 0.6999(3) 0.0193(9) Uani 1 1 d . . . H21 H 0.4966 -0.1555 0.6967 0.023 Uiso 1 1 calc R . . C22 C 1.0100(4) -0.0593(4) 0.7072(3) 0.0193(9) Uani 1 1 d . . . C23 C 0.4799(4) -0.1532(4) 0.4226(3) 0.0211(9) Uani 1 1 d . . . C24 C 0.3323(4) -0.2096(4) 0.3340(3) 0.0225(9) Uani 1 1 d . . . C25 C 0.3173(5) -0.2318(6) 0.2266(4) 0.0340(12) Uani 1 1 d . . . H25 H 0.3964 -0.2189 0.2079 0.041 Uiso 1 1 calc R . . C26 C 0.1830(5) -0.2737(6) 0.1467(4) 0.0403(13) Uani 1 1 d . . . H26 H 0.1731 -0.2928 0.0733 0.048 Uiso 1 1 calc R . . C27 C 0.0833(5) -0.2678(6) 0.2745(4) 0.0432(14) Uani 1 1 d . . . H27 H 0.0029 -0.2799 0.2918 0.052 Uiso 1 1 calc R . . C28 C 0.2123(5) -0.2305(6) 0.3573(4) 0.0350(12) Uani 1 1 d . . . H28 H 0.2189 -0.2193 0.4290 0.042 Uiso 1 1 calc R . . N1 N 1.1593(4) 0.3382(5) 0.1313(3) 0.0358(10) Uani 1 1 d . . . N2 N 1.1885(4) 0.4010(4) 0.5223(3) 0.0237(8) Uani 1 1 d . . . H2 H 1.1186 0.3284 0.4779 0.028 Uiso 1 1 calc R . . N3 N 0.0671(4) -0.2879(5) 0.1696(3) 0.0370(10) Uani 1 1 d . . . N4 N 0.4934(4) -0.1999(4) 0.5032(3) 0.0230(8) Uani 1 1 d . . . H4 H 0.4238 -0.2665 0.4931 0.028 Uiso 1 1 calc R . . O1 O 1.4022(3) 0.7814(3) 0.9990(2) 0.0230(6) Uani 1 1 d . . . O2 O 1.2655(3) 0.8144(3) 0.8578(2) 0.0228(6) Uani 1 1 d . . . O3 O 1.3336(3) 0.2862(3) 0.9347(2) 0.0217(6) Uani 1 1 d . . . O4 O 1.3825(3) 0.1967(3) 0.7896(2) 0.0246(7) Uani 1 1 d . . . O5 O 1.3473(5) 0.5857(4) 0.5380(3) 0.0574(13) Uani 1 1 d . . . O6 O 0.5538(3) -0.0608(3) 0.9041(2) 0.0197(6) Uani 1 1 d . . . O7 O 0.7659(3) -0.0624(3) 0.9874(2) 0.0289(7) Uani 1 1 d . . . O8 O 1.0191(3) -0.1319(3) 0.6207(2) 0.0310(8) Uani 1 1 d . . . O9 O 1.1140(3) 0.0215(3) 0.7941(2) 0.0240(7) Uani 1 1 d . . . O10 O 0.5751(3) -0.0701(3) 0.4207(2) 0.0288(7) Uani 1 1 d . . . O1W O 1.3003(3) -0.0811(3) 0.6829(2) 0.0228(6) Uani 1 1 d . . . H1WB H 1.3469 -0.0324 0.6589 0.027 Uiso 1 1 d R . . H1WA H 1.2125 -0.0989 0.6476 0.027 Uiso 1 1 d 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 Ag1 0.0300(2) 0.1158(4) 0.0290(2) 0.0328(3) 0.01343(18) 0.0358(3) Nd1 0.01488(13) 0.01464(13) 0.01361(13) 0.00617(9) 0.00508(9) 0.00705(9) C1 0.015(2) 0.019(2) 0.022(2) 0.0106(18) 0.0098(17) 0.0066(17) C2 0.019(2) 0.017(2) 0.023(2) 0.0088(18) 0.0067(17) 0.0078(17) C3 0.026(2) 0.020(2) 0.023(2) 0.0112(18) 0.0089(18) 0.0098(18) C4 0.024(2) 0.020(2) 0.019(2) 0.0087(18) 0.0069(18) 0.0044(18) C5 0.029(2) 0.018(2) 0.022(2) 0.0053(18) 0.0102(19) 0.0078(19) C6 0.017(2) 0.018(2) 0.024(2) 0.0127(18) 0.0062(17) 0.0063(17) C7 0.020(2) 0.022(2) 0.017(2) 0.0078(17) 0.0052(17) 0.0068(17) C8 0.016(2) 0.018(2) 0.023(2) 0.0104(18) 0.0048(18) 0.0046(17) C9 0.033(3) 0.025(2) 0.023(2) 0.010(2) 0.008(2) 0.004(2) C10 0.037(3) 0.027(2) 0.024(2) 0.013(2) 0.013(2) 0.011(2) C11 0.025(2) 0.043(3) 0.029(3) 0.012(2) 0.007(2) 0.007(2) C12 0.036(3) 0.049(3) 0.039(3) 0.023(3) 0.021(2) 0.019(3) C13 0.030(3) 0.060(4) 0.026(3) 0.019(2) 0.008(2) 0.019(3) C14 0.035(3) 0.049(3) 0.027(2) 0.023(2) 0.017(2) 0.019(2) C15 0.023(2) 0.016(2) 0.021(2) 0.0073(17) 0.0124(18) 0.0068(17) C16 0.019(2) 0.021(2) 0.016(2) 0.0086(17) 0.0090(17) 0.0094(17) C17 0.016(2) 0.024(2) 0.016(2) 0.0080(17) 0.0046(17) 0.0083(17) C18 0.016(2) 0.022(2) 0.020(2) 0.0101(18) 0.0064(17) 0.0071(17) C19 0.022(2) 0.026(2) 0.0117(19) 0.0074(17) 0.0058(17) 0.0089(18) C20 0.017(2) 0.019(2) 0.021(2) 0.0100(17) 0.0051(17) 0.0070(17) C21 0.015(2) 0.024(2) 0.022(2) 0.0098(18) 0.0079(17) 0.0094(17) C22 0.016(2) 0.024(2) 0.017(2) 0.0091(18) 0.0038(17) 0.0072(18) C23 0.019(2) 0.028(2) 0.019(2) 0.0096(18) 0.0095(18) 0.0081(19) C24 0.019(2) 0.024(2) 0.024(2) 0.0101(19) 0.0051(18) 0.0082(18) C25 0.021(2) 0.061(3) 0.027(2) 0.022(2) 0.011(2) 0.018(2) C26 0.030(3) 0.071(4) 0.021(2) 0.019(3) 0.006(2) 0.021(3) C27 0.024(3) 0.073(4) 0.041(3) 0.032(3) 0.014(2) 0.017(3) C28 0.026(3) 0.058(3) 0.021(2) 0.019(2) 0.009(2) 0.010(2) N1 0.036(2) 0.055(3) 0.025(2) 0.021(2) 0.0129(19) 0.022(2) N2 0.031(2) 0.0185(19) 0.0135(17) 0.0046(15) 0.0034(15) 0.0040(16) N3 0.024(2) 0.060(3) 0.023(2) 0.015(2) 0.0037(17) 0.017(2) N4 0.0142(18) 0.031(2) 0.0186(18) 0.0116(16) 0.0002(14) 0.0037(16) O1 0.0273(17) 0.0180(15) 0.0190(15) 0.0066(12) 0.0045(13) 0.0058(13) O2 0.0209(15) 0.0189(15) 0.0278(16) 0.0098(13) 0.0056(13) 0.0093(13) O3 0.0251(16) 0.0247(16) 0.0235(15) 0.0151(13) 0.0112(13) 0.0133(13) O4 0.0327(18) 0.0243(16) 0.0284(16) 0.0139(14) 0.0176(14) 0.0178(14) O5 0.077(3) 0.039(2) 0.029(2) 0.0055(18) 0.019(2) -0.019(2) O6 0.0165(15) 0.0242(16) 0.0200(14) 0.0069(12) 0.0096(12) 0.0089(12) O7 0.0254(17) 0.052(2) 0.0198(16) 0.0187(15) 0.0119(14) 0.0227(16) O8 0.0209(17) 0.039(2) 0.0244(16) 0.0023(15) 0.0098(14) 0.0083(15) O9 0.0162(15) 0.0331(18) 0.0197(15) 0.0092(14) 0.0048(12) 0.0075(13) O10 0.0240(17) 0.0377(19) 0.0232(16) 0.0162(15) 0.0071(14) 0.0045(15) O1W 0.0220(16) 0.0263(17) 0.0218(15) 0.0097(13) 0.0097(13) 0.0091(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.235(4) . ? Ag1 N1 2.243(4) 2_655 ? Ag1 O3 2.309(3) 2_656 ? Nd1 O2 2.409(3) 1_545 ? Nd1 O1 2.445(3) 2_867 ? Nd1 O4 2.453(3) . ? Nd1 O7 2.457(3) 2_757 ? Nd1 O9 2.465(3) . ? Nd1 O6 2.521(3) 1_655 ? Nd1 O1W 2.535(3) . ? Nd1 O3 2.650(3) . ? Nd1 O6 2.663(3) 2_757 ? Nd1 C15 2.931(4) 2_757 ? C1 O2 1.254(5) . ? C1 O1 1.260(5) . ? C1 C2 1.497(6) . ? C2 C3 1.384(6) . ? C2 C7 1.387(6) . ? C3 C4 1.387(6) . ? C3 H3 0.9300 . ? C4 C5 1.380(6) . ? C4 N2 1.436(5) . ? C5 C6 1.390(6) . ? C5 H5 0.9300 . ? C6 C7 1.375(6) . ? C6 C8 1.493(5) . ? C7 H7 0.9300 . ? C8 O4 1.245(5) . ? C8 O3 1.264(5) . ? C9 O5 1.222(6) . ? C9 N2 1.334(6) . ? C9 C10 1.499(6) . ? C10 C11 1.378(7) . ? C10 C14 1.379(7) . ? C11 C12 1.365(7) . ? C11 H11 0.9300 . ? C12 N1 1.342(6) . ? C12 H12 0.9300 . ? C13 N1 1.332(6) . ? C13 C14 1.369(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O7 1.247(5) . ? C15 O6 1.264(5) . ? C15 C16 1.494(5) . ? C15 Nd1 2.931(4) 2_757 ? C16 C21 1.385(5) . ? C16 C17 1.390(6) . ? C17 C18 1.382(6) . ? C17 H17 0.9300 . ? C18 C19 1.399(6) . ? C18 C22 1.494(6) . ? C19 C20 1.368(6) . ? C19 H19 0.9300 . ? C20 C21 1.378(6) . ? C20 N4 1.424(5) . ? C21 H21 0.9300 . ? C22 O8 1.255(5) . ? C22 O9 1.255(5) . ? C23 O10 1.212(5) . ? C23 N4 1.339(5) . ? C23 C24 1.509(6) . ? C24 C25 1.369(6) . ? C24 C28 1.371(6) . ? C25 C26 1.378(6) . ? C25 H25 0.9300 . ? C26 N3 1.326(6) . ? C26 H26 0.9300 . ? C27 N3 1.337(6) . ? C27 C28 1.364(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N1 Ag1 2.243(4) 2_655 ? N2 H2 0.8600 . ? N4 H4 0.8600 . ? O1 Nd1 2.445(3) 2_867 ? O2 Nd1 2.409(3) 1_565 ? O3 Ag1 2.309(3) 2_656 ? O6 Nd1 2.521(3) 1_455 ? O6 Nd1 2.663(3) 2_757 ? O7 Nd1 2.457(3) 2_757 ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? 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 N3 Ag1 N1 121.46(15) . 2_655 ? N3 Ag1 O3 124.61(12) . 2_656 ? N1 Ag1 O3 106.23(13) 2_655 2_656 ? O2 Nd1 O1 133.54(9) 1_545 2_867 ? O2 Nd1 O4 142.20(10) 1_545 . ? O1 Nd1 O4 75.81(10) 2_867 . ? O2 Nd1 O7 78.19(11) 1_545 2_757 ? O1 Nd1 O7 105.05(10) 2_867 2_757 ? O4 Nd1 O7 122.11(10) . 2_757 ? O2 Nd1 O9 83.60(10) 1_545 . ? O1 Nd1 O9 141.36(10) 2_867 . ? O4 Nd1 O9 77.38(10) . . ? O7 Nd1 O9 67.47(9) 2_757 . ? O2 Nd1 O6 69.70(9) 1_545 1_655 ? O1 Nd1 O6 69.88(9) 2_867 1_655 ? O4 Nd1 O6 112.81(9) . 1_655 ? O7 Nd1 O6 121.74(9) 2_757 1_655 ? O9 Nd1 O6 147.51(10) . 1_655 ? O2 Nd1 O1W 75.74(10) 1_545 . ? O1 Nd1 O1W 119.35(9) 2_867 . ? O4 Nd1 O1W 67.75(9) . . ? O7 Nd1 O1W 135.20(10) 2_757 . ? O9 Nd1 O1W 73.92(9) . . ? O6 Nd1 O1W 81.61(9) 1_655 . ? O2 Nd1 O3 147.35(9) 1_545 . ? O1 Nd1 O3 71.50(9) 2_867 . ? O4 Nd1 O3 50.68(9) . . ? O7 Nd1 O3 74.17(10) 2_757 . ? O9 Nd1 O3 70.02(10) . . ? O6 Nd1 O3 140.93(9) 1_655 . ? O1W Nd1 O3 113.08(9) . . ? O2 Nd1 O6 78.80(9) 1_545 2_757 ? O1 Nd1 O6 70.07(9) 2_867 2_757 ? O4 Nd1 O6 139.00(9) . 2_757 ? O7 Nd1 O6 50.38(9) 2_757 2_757 ? O9 Nd1 O6 117.52(9) . 2_757 ? O6 Nd1 O6 76.03(9) 1_655 2_757 ? O1W Nd1 O6 150.65(9) . 2_757 ? O3 Nd1 O6 96.23(8) . 2_757 ? O2 Nd1 C15 77.53(10) 1_545 2_757 ? O1 Nd1 C15 87.50(11) 2_867 2_757 ? O4 Nd1 C15 134.91(10) . 2_757 ? O7 Nd1 C15 24.83(10) 2_757 2_757 ? O9 Nd1 C15 92.17(11) . 2_757 ? O6 Nd1 C15 99.49(10) 1_655 2_757 ? O1W Nd1 C15 151.00(11) . 2_757 ? O3 Nd1 C15 84.39(10) . 2_757 ? O6 Nd1 C15 25.55(10) 2_757 2_757 ? O2 Nd1 Nd1 70.08(7) 1_545 2_857 ? O1 Nd1 Nd1 64.25(7) 2_867 2_857 ? O4 Nd1 Nd1 136.98(7) . 2_857 ? O7 Nd1 Nd1 84.77(7) 2_757 2_857 ? O9 Nd1 Nd1 145.25(7) . 2_857 ? O6 Nd1 Nd1 39.24(6) 1_655 2_857 ? O1W Nd1 Nd1 118.57(6) . 2_857 ? O3 Nd1 Nd1 123.36(6) . 2_857 ? O6 Nd1 Nd1 36.78(6) 2_757 2_857 ? C15 Nd1 Nd1 60.89(8) 2_757 2_857 ? O2 C1 O1 125.0(4) . . ? O2 C1 C2 117.8(3) . . ? O1 C1 C2 117.2(4) . . ? C3 C2 C7 119.9(4) . . ? C3 C2 C1 120.0(4) . . ? C7 C2 C1 120.0(4) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 N2 119.0(4) . . ? C3 C4 N2 120.9(4) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.2(4) . . ? C7 C6 C8 121.1(4) . . ? C5 C6 C8 118.7(4) . . ? C6 C7 C2 120.1(4) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O4 C8 O3 121.7(4) . . ? O4 C8 C6 117.6(4) . . ? O3 C8 C6 120.7(4) . . ? O5 C9 N2 122.7(4) . . ? O5 C9 C10 118.7(4) . . ? N2 C9 C10 118.6(4) . . ? C11 C10 C14 117.9(4) . . ? C11 C10 C9 118.1(4) . . ? C14 C10 C9 124.0(4) . . ? C12 C11 C10 119.4(5) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N1 C12 C11 123.1(5) . . ? N1 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N1 C13 C14 123.3(5) . . ? N1 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C10 119.3(5) . . ? C13 C14 H14 120.4 . . ? C10 C14 H14 120.4 . . ? O7 C15 O6 121.1(4) . . ? O7 C15 C16 119.1(4) . . ? O6 C15 C16 119.8(4) . . ? O7 C15 Nd1 55.8(2) . 2_757 ? O6 C15 Nd1 65.3(2) . 2_757 ? C16 C15 Nd1 174.5(3) . 2_757 ? C21 C16 C17 119.9(4) . . ? C21 C16 C15 118.9(4) . . ? C17 C16 C15 121.2(4) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 119.2(4) . . ? C17 C18 C22 121.4(4) . . ? C19 C18 C22 119.0(4) . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 N4 122.3(4) . . ? C21 C20 N4 116.8(4) . . ? C20 C21 C16 119.6(4) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? O8 C22 O9 124.7(4) . . ? O8 C22 C18 117.7(4) . . ? O9 C22 C18 117.5(4) . . ? O10 C23 N4 124.2(4) . . ? O10 C23 C24 121.6(4) . . ? N4 C23 C24 114.1(4) . . ? C25 C24 C28 118.4(4) . . ? C25 C24 C23 118.7(4) . . ? C28 C24 C23 122.8(4) . . ? C24 C25 C26 118.9(4) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? N3 C26 C25 123.0(4) . . ? N3 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? N3 C27 C28 122.9(5) . . ? N3 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C27 C28 C24 119.4(4) . . ? C27 C28 H28 120.3 . . ? C24 C28 H28 120.3 . . ? C13 N1 C12 117.0(4) . . ? C13 N1 Ag1 122.1(3) . 2_655 ? C12 N1 Ag1 120.8(3) . 2_655 ? C9 N2 C4 121.7(4) . . ? C9 N2 H2 119.2 . . ? C4 N2 H2 119.2 . . ? C26 N3 C27 117.3(4) . . ? C26 N3 Ag1 115.5(3) . . ? C27 N3 Ag1 123.2(3) . . ? C23 N4 C20 124.9(4) . . ? C23 N4 H4 117.6 . . ? C20 N4 H4 117.6 . . ? C1 O1 Nd1 131.6(3) . 2_867 ? C1 O2 Nd1 129.5(3) . 1_565 ? C8 O3 Ag1 118.6(3) . 2_656 ? C8 O3 Nd1 88.3(2) . . ? Ag1 O3 Nd1 108.15(11) 2_656 . ? C8 O4 Nd1 98.1(2) . . ? C15 O6 Nd1 153.0(3) . 1_455 ? C15 O6 Nd1 89.1(2) . 2_757 ? Nd1 O6 Nd1 103.97(9) 1_455 2_757 ? C15 O7 Nd1 99.4(2) . 2_757 ? C22 O9 Nd1 137.6(3) . . ? Nd1 O1W H1WB 109.4 . . ? Nd1 O1W H1WA 109.4 . . ? H1WB O1W H1WA 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 20.1(6) . . . . ? O1 C1 C2 C3 -160.0(4) . . . . ? O2 C1 C2 C7 -163.9(4) . . . . ? O1 C1 C2 C7 16.0(6) . . . . ? C7 C2 C3 C4 -1.6(6) . . . . ? C1 C2 C3 C4 174.4(4) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C2 C3 C4 N2 -176.8(4) . . . . ? C3 C4 C5 C6 1.5(7) . . . . ? N2 C4 C5 C6 178.6(4) . . . . ? C4 C5 C6 C7 -1.8(6) . . . . ? C4 C5 C6 C8 -179.3(4) . . . . ? C5 C6 C7 C2 0.3(6) . . . . ? C8 C6 C7 C2 177.8(4) . . . . ? C3 C2 C7 C6 1.4(6) . . . . ? C1 C2 C7 C6 -174.6(4) . . . . ? C7 C6 C8 O4 -152.0(4) . . . . ? C5 C6 C8 O4 25.5(6) . . . . ? C7 C6 C8 O3 28.8(6) . . . . ? C5 C6 C8 O3 -153.7(4) . . . . ? O5 C9 C10 C11 39.2(7) . . . . ? N2 C9 C10 C11 -139.4(5) . . . . ? O5 C9 C10 C14 -138.0(5) . . . . ? N2 C9 C10 C14 43.3(7) . . . . ? C14 C10 C11 C12 -0.8(8) . . . . ? C9 C10 C11 C12 -178.2(5) . . . . ? C10 C11 C12 N1 2.0(8) . . . . ? N1 C13 C14 C10 0.1(8) . . . . ? C11 C10 C14 C13 -0.2(7) . . . . ? C9 C10 C14 C13 177.1(5) . . . . ? O7 C15 C16 C21 158.8(4) . . . . ? O6 C15 C16 C21 -19.8(6) . . . . ? O7 C15 C16 C17 -18.8(6) . . . . ? O6 C15 C16 C17 162.6(4) . . . . ? C21 C16 C17 C18 1.5(6) . . . . ? C15 C16 C17 C18 179.0(4) . . . . ? C16 C17 C18 C19 0.2(6) . . . . ? C16 C17 C18 C22 -172.7(4) . . . . ? C17 C18 C19 C20 -0.4(6) . . . . ? C22 C18 C19 C20 172.6(4) . . . . ? C18 C19 C20 C21 -1.0(7) . . . . ? C18 C19 C20 N4 -177.4(4) . . . . ? C19 C20 C21 C16 2.7(6) . . . . ? N4 C20 C21 C16 179.2(4) . . . . ? C17 C16 C21 C20 -2.9(6) . . . . ? C15 C16 C21 C20 179.5(4) . . . . ? C17 C18 C22 O8 147.5(4) . . . . ? C19 C18 C22 O8 -25.5(6) . . . . ? C17 C18 C22 O9 -30.6(6) . . . . ? C19 C18 C22 O9 156.5(4) . . . . ? O10 C23 C24 C25 36.9(7) . . . . ? N4 C23 C24 C25 -145.1(4) . . . . ? O10 C23 C24 C28 -138.4(5) . . . . ? N4 C23 C24 C28 39.7(6) . . . . ? C28 C24 C25 C26 0.2(8) . . . . ? C23 C24 C25 C26 -175.2(5) . . . . ? C24 C25 C26 N3 3.1(9) . . . . ? N3 C27 C28 C24 1.3(9) . . . . ? C25 C24 C28 C27 -2.3(8) . . . . ? C23 C24 C28 C27 172.9(5) . . . . ? C14 C13 N1 C12 1.0(8) . . . . ? C14 C13 N1 Ag1 178.6(4) . . . 2_655 ? C11 C12 N1 C13 -2.0(8) . . . . ? C11 C12 N1 Ag1 -179.7(4) . . . 2_655 ? O5 C9 N2 C4 -6.1(8) . . . . ? C10 C9 N2 C4 172.6(4) . . . . ? C5 C4 N2 C9 -125.3(5) . . . . ? C3 C4 N2 C9 51.7(6) . . . . ? C25 C26 N3 C27 -4.1(9) . . . . ? C25 C26 N3 Ag1 154.1(5) . . . . ? C28 C27 N3 C26 1.8(9) . . . . ? C28 C27 N3 Ag1 -154.5(5) . . . . ? N1 Ag1 N3 C26 34.8(5) 2_655 . . . ? O3 Ag1 N3 C26 179.9(4) 2_656 . . . ? N1 Ag1 N3 C27 -168.5(4) 2_655 . . . ? O3 Ag1 N3 C27 -23.4(5) 2_656 . . . ? O10 C23 N4 C20 8.4(7) . . . . ? C24 C23 N4 C20 -169.6(4) . . . . ? C19 C20 N4 C23 -46.2(6) . . . . ? C21 C20 N4 C23 137.3(4) . . . . ? O2 C1 O1 Nd1 -64.8(5) . . . 2_867 ? C2 C1 O1 Nd1 115.3(4) . . . 2_867 ? O1 C1 O2 Nd1 42.2(5) . . . 1_565 ? C2 C1 O2 Nd1 -137.9(3) . . . 1_565 ? O4 C8 O3 Ag1 -121.0(4) . . . 2_656 ? C6 C8 O3 Ag1 58.2(4) . . . 2_656 ? O4 C8 O3 Nd1 -11.2(4) . . . . ? C6 C8 O3 Nd1 168.0(3) . . . . ? O2 Nd1 O3 C8 -121.7(3) 1_545 . . . ? O1 Nd1 O3 C8 92.8(2) 2_867 . . . ? O4 Nd1 O3 C8 6.2(2) . . . . ? O7 Nd1 O3 C8 -154.9(2) 2_757 . . . ? O9 Nd1 O3 C8 -83.6(2) . . . . ? O6 Nd1 O3 C8 83.9(3) 1_655 . . . ? O1W Nd1 O3 C8 -22.0(3) . . . . ? O6 Nd1 O3 C8 159.3(2) 2_757 . . . ? C15 Nd1 O3 C8 -178.0(2) 2_757 . . . ? Nd1 Nd1 O3 C8 132.5(2) 2_857 . . . ? O2 Nd1 O3 Ag1 -2.1(2) 1_545 . . 2_656 ? O1 Nd1 O3 Ag1 -147.60(13) 2_867 . . 2_656 ? O4 Nd1 O3 Ag1 125.84(16) . . . 2_656 ? O7 Nd1 O3 Ag1 -35.30(11) 2_757 . . 2_656 ? O9 Nd1 O3 Ag1 36.00(10) . . . 2_656 ? O6 Nd1 O3 Ag1 -156.52(10) 1_655 . . 2_656 ? O1W Nd1 O3 Ag1 97.62(11) . . . 2_656 ? O6 Nd1 O3 Ag1 -81.06(11) 2_757 . . 2_656 ? C15 Nd1 O3 Ag1 -58.37(12) 2_757 . . 2_656 ? Nd1 Nd1 O3 Ag1 -107.84(9) 2_857 . . 2_656 ? O3 C8 O4 Nd1 12.2(4) . . . . ? C6 C8 O4 Nd1 -166.9(3) . . . . ? O2 Nd1 O4 C8 129.7(3) 1_545 . . . ? O1 Nd1 O4 C8 -83.9(3) 2_867 . . . ? O7 Nd1 O4 C8 15.2(3) 2_757 . . . ? O9 Nd1 O4 C8 68.0(3) . . . . ? O6 Nd1 O4 C8 -144.5(2) 1_655 . . . ? O1W Nd1 O4 C8 145.6(3) . . . . ? O3 Nd1 O4 C8 -6.4(2) . . . . ? O6 Nd1 O4 C8 -49.6(3) 2_757 . . . ? C15 Nd1 O4 C8 -12.3(3) 2_757 . . . ? Nd1 Nd1 O4 C8 -105.8(2) 2_857 . . . ? O7 C15 O6 Nd1 119.0(5) . . . 1_455 ? C16 C15 O6 Nd1 -62.4(7) . . . 1_455 ? Nd1 C15 O6 Nd1 120.1(6) 2_757 . . 1_455 ? O7 C15 O6 Nd1 -1.1(4) . . . 2_757 ? C16 C15 O6 Nd1 177.5(3) . . . 2_757 ? O6 C15 O7 Nd1 1.2(4) . . . 2_757 ? C16 C15 O7 Nd1 -177.4(3) . . . 2_757 ? O8 C22 O9 Nd1 -26.4(7) . . . . ? C18 C22 O9 Nd1 151.5(3) . . . . ? O2 Nd1 O9 C22 -49.1(4) 1_545 . . . ? O1 Nd1 O9 C22 145.0(4) 2_867 . . . ? O4 Nd1 O9 C22 98.0(4) . . . . ? O7 Nd1 O9 C22 -129.0(4) 2_757 . . . ? O6 Nd1 O9 C22 -14.8(5) 1_655 . . . ? O1W Nd1 O9 C22 27.8(4) . . . . ? O3 Nd1 O9 C22 150.4(4) . . . . ? O6 Nd1 O9 C22 -123.0(4) 2_757 . . . ? C15 Nd1 O9 C22 -126.3(4) 2_757 . . . ? Nd1 Nd1 O9 C22 -89.4(4) 2_857 . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.766 _refine_diff_density_min -1.754 _refine_diff_density_rms 0.123 data_9 _database_code_depnum_ccdc_archive 'CCDC 760893' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Ag Dy N4 O12' _chemical_formula_weight 874.85 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8607(10) _cell_length_b 11.3727(12) _cell_length_c 13.7453(14) _cell_angle_alpha 73.704(2) _cell_angle_beta 70.7470(10) _cell_angle_gamma 83.917(2) _cell_volume 1396.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3768 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.95 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 3.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5771 _exptl_absorpt_correction_T_max 0.7253 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7019 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4847 _reflns_number_gt 4360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0725P)^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 4847 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Ag1 Ag 0.45034(7) 0.68849(7) -0.51508(4) 0.039 Uani 1 1 d . . . Dy1 Dy -0.15385(3) 0.06185(3) 0.60977(2) 0.01391(10) Uani 1 1 d . . . C1 C 0.1155(7) 0.2245(6) 0.4122(5) 0.0192(15) Uani 1 1 d . . . C2 C 0.1482(7) 0.3526(6) 0.3441(5) 0.0169(14) Uani 1 1 d . . . C3 C 0.1820(8) 0.3752(7) 0.2342(5) 0.0231(16) Uani 1 1 d . . . H3 H 0.1844 0.3116 0.2033 0.028 Uiso 1 1 calc R . . C4 C 0.2124(7) 0.4955(6) 0.1706(5) 0.0206(15) Uani 1 1 d . . . C5 C 0.2173(8) 0.5881(6) 0.2179(5) 0.0229(16) Uani 1 1 d . . . H5 H 0.2380 0.6678 0.1759 0.027 Uiso 1 1 calc R . . C6 C 0.1915(7) 0.5618(6) 0.3272(5) 0.0199(15) Uani 1 1 d . . . C7 C 0.1513(7) 0.4451(6) 0.3909(5) 0.0205(15) Uani 1 1 d . . . H7 H 0.1265 0.4288 0.4647 0.025 Uiso 1 1 calc R . . C8 C 0.2069(8) 0.4686(7) -0.0008(5) 0.0245(16) Uani 1 1 d . . . C9 C 0.2667(8) 0.5204(7) -0.1191(6) 0.0258(16) Uani 1 1 d . . . C10 C 0.1842(8) 0.5182(7) -0.1827(6) 0.0288(17) Uani 1 1 d . . . H10 H 0.0917 0.4874 -0.1523 0.035 Uiso 1 1 calc R . . C11 C 0.2414(9) 0.5626(8) -0.2918(6) 0.0334(19) Uani 1 1 d . . . H11 H 0.1842 0.5620 -0.3336 0.040 Uiso 1 1 calc R . . C12 C 0.4527(9) 0.6073(9) -0.2793(6) 0.039(2) Uani 1 1 d . . . H12 H 0.5456 0.6371 -0.3121 0.047 Uiso 1 1 calc R . . C13 C 0.4047(8) 0.5664(9) -0.1679(6) 0.036(2) Uani 1 1 d . . . H13 H 0.4632 0.5698 -0.1278 0.044 Uiso 1 1 calc R . . C14 C 0.2177(7) 0.6570(7) 0.3767(5) 0.0221(16) Uani 1 1 d . . . C15 C -0.1913(7) 0.0878(6) 0.4064(5) 0.0200(15) Uani 1 1 d . . . C16 C -0.2248(7) 0.1046(6) 0.3046(5) 0.0172(14) Uani 1 1 d . . . C17 C -0.3579(7) 0.0703(6) 0.3075(5) 0.0192(14) Uani 1 1 d . . . H17 H -0.4279 0.0407 0.3727 0.023 Uiso 1 1 calc R . . C18 C -0.3856(7) 0.0805(7) 0.2132(5) 0.0209(15) Uani 1 1 d . . . C19 C -0.2810(7) 0.1247(7) 0.1164(5) 0.0201(15) Uani 1 1 d . . . H19 H -0.3008 0.1335 0.0531 0.024 Uiso 1 1 calc R . . C20 C -0.1482(7) 0.1557(7) 0.1129(5) 0.0206(15) Uani 1 1 d . . . C21 C -0.1182(7) 0.1463(6) 0.2059(5) 0.0200(15) Uani 1 1 d . . . H21 H -0.0283 0.1674 0.2033 0.024 Uiso 1 1 calc R . . C22 C -0.0111(7) 0.1561(7) -0.0724(5) 0.0233(16) Uani 1 1 d . . . C23 C 0.1218(7) 0.1988(7) -0.1634(5) 0.0229(15) Uani 1 1 d . . . C24 C 0.1150(8) 0.2181(8) -0.2652(6) 0.0320(18) Uani 1 1 d . . . H24 H 0.0285 0.2086 -0.2753 0.038 Uiso 1 1 calc R . . C25 C 0.2353(8) 0.2512(8) -0.3512(6) 0.0352(19) Uani 1 1 d . . . H25 H 0.2286 0.2646 -0.4194 0.042 Uiso 1 1 calc R . . C26 C 0.3700(8) 0.2440(8) -0.2426(6) 0.0335(19) Uani 1 1 d . . . H26 H 0.4582 0.2513 -0.2340 0.040 Uiso 1 1 calc R . . C27 C 0.2524(8) 0.2118(7) -0.1523(6) 0.0289(17) Uani 1 1 d . . . H27 H 0.2615 0.1991 -0.0849 0.035 Uiso 1 1 calc R . . C28 C -0.5282(7) 0.0447(7) 0.2156(5) 0.0238(16) Uani 1 1 d . . . N1 N 0.3743(7) 0.6064(7) -0.3411(5) 0.0332(16) Uani 1 1 d . . . N2 N 0.2476(7) 0.5260(6) 0.0590(4) 0.0273(14) Uani 1 1 d . . . H2 H 0.3015 0.5887 0.0244 0.033 Uiso 1 1 calc R . . N3 N 0.3639(7) 0.2651(6) -0.3405(5) 0.0304(15) Uani 1 1 d . . . N4 N -0.0346(6) 0.1958(6) 0.0154(4) 0.0218(13) Uani 1 1 d . . . H4 H 0.0231 0.2492 0.0124 0.026 Uiso 1 1 calc R . . O1 O 0.0209(5) 0.2108(5) 0.5020(4) 0.0271(12) Uani 1 1 d . . . O2 O 0.1884(5) 0.1407(4) 0.3740(4) 0.0255(11) Uani 1 1 d . . . O3 O 0.2447(6) 0.6187(5) 0.4616(4) 0.0386(14) Uani 1 1 d . . . O4 O 0.2159(6) 0.7688(4) 0.3242(4) 0.0288(12) Uani 1 1 d . . . O5 O 0.1248(6) 0.3825(5) 0.0383(4) 0.0380(14) Uani 1 1 d . . . O6 O -0.0710(5) 0.0415(5) 0.4127(4) 0.0222(11) Uani 1 1 d . . . O7 O -0.2825(5) 0.1194(5) 0.4831(4) 0.0274(12) Uani 1 1 d . . . O8 O -0.6024(5) -0.0274(4) 0.2993(3) 0.0198(10) Uani 1 1 d . . . O9 O -0.5679(6) 0.0882(6) 0.1344(4) 0.0456(17) Uani 1 1 d . . . O10 O -0.0935(6) 0.0889(6) -0.0797(4) 0.0413(15) Uani 1 1 d . . . O1W O -0.1647(5) -0.0179(5) 0.7902(3) 0.0233(11) Uani 1 1 d . . . H1WB H -0.2511 -0.0323 0.8299 0.028 Uiso 1 1 d R . . H1WA H -0.1297 0.0322 0.8109 0.028 Uiso 1 1 d R . . O2W O 0.5047(8) 0.3146(7) 0.9939(6) 0.078(3) Uani 1 1 d . . . H2WA H 0.4807 0.2451 1.0378 0.093 Uiso 1 1 d R . . H2WB H 0.4388 0.3663 1.0114 0.093 Uiso 1 1 d 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 Ag1 0.025 0.062 0.022 -0.007 0.002 -0.010 Dy1 0.01154(17) 0.01500(18) 0.01527(17) -0.00592(12) -0.00206(12) -0.00222(12) C1 0.016(3) 0.019(4) 0.024(4) -0.009(3) -0.005(3) -0.002(3) C2 0.010(3) 0.015(3) 0.023(3) -0.004(3) -0.002(3) -0.005(3) C3 0.026(4) 0.019(4) 0.026(4) -0.012(3) -0.004(3) -0.004(3) C4 0.023(4) 0.019(4) 0.019(3) -0.005(3) -0.005(3) -0.004(3) C5 0.026(4) 0.016(4) 0.023(4) -0.001(3) -0.004(3) -0.005(3) C6 0.017(4) 0.018(4) 0.026(4) -0.009(3) -0.005(3) -0.005(3) C7 0.020(4) 0.019(4) 0.019(3) -0.006(3) -0.001(3) 0.002(3) C8 0.025(4) 0.023(4) 0.026(4) -0.009(3) -0.006(3) 0.000(3) C9 0.025(4) 0.028(4) 0.024(4) -0.009(3) -0.004(3) -0.005(3) C10 0.025(4) 0.031(4) 0.028(4) -0.006(3) -0.006(3) -0.005(3) C11 0.032(5) 0.045(5) 0.024(4) -0.011(4) -0.009(3) 0.001(4) C12 0.024(4) 0.062(6) 0.027(4) -0.005(4) -0.004(3) -0.008(4) C13 0.021(4) 0.061(6) 0.030(4) -0.014(4) -0.008(3) -0.008(4) C14 0.013(3) 0.030(4) 0.024(4) -0.017(3) 0.002(3) -0.003(3) C15 0.025(4) 0.016(4) 0.017(3) 0.002(3) -0.005(3) -0.010(3) C16 0.015(3) 0.019(4) 0.016(3) -0.004(3) -0.004(3) -0.001(3) C17 0.010(3) 0.023(4) 0.022(3) -0.007(3) 0.000(3) 0.000(3) C18 0.014(3) 0.030(4) 0.018(3) -0.008(3) -0.003(3) -0.001(3) C19 0.015(3) 0.030(4) 0.016(3) -0.008(3) -0.004(3) -0.002(3) C20 0.019(4) 0.026(4) 0.016(3) -0.008(3) 0.000(3) -0.002(3) C21 0.014(3) 0.021(4) 0.029(4) -0.013(3) -0.009(3) 0.004(3) C22 0.018(4) 0.037(4) 0.015(3) -0.009(3) -0.002(3) -0.005(3) C23 0.020(4) 0.027(4) 0.020(3) -0.010(3) -0.001(3) 0.000(3) C24 0.023(4) 0.047(5) 0.026(4) -0.008(4) -0.006(3) -0.004(4) C25 0.027(4) 0.053(6) 0.024(4) -0.009(4) -0.008(3) 0.000(4) C26 0.019(4) 0.054(6) 0.023(4) -0.006(4) 0.000(3) -0.011(4) C27 0.025(4) 0.041(5) 0.020(4) -0.012(3) -0.003(3) -0.004(3) C28 0.013(3) 0.036(4) 0.021(4) -0.012(3) 0.001(3) -0.008(3) N1 0.028(4) 0.047(4) 0.023(3) -0.008(3) -0.006(3) -0.005(3) N2 0.034(4) 0.024(3) 0.022(3) -0.004(3) -0.004(3) -0.015(3) N3 0.024(3) 0.039(4) 0.021(3) -0.008(3) 0.003(3) -0.003(3) N4 0.012(3) 0.029(3) 0.022(3) -0.008(3) 0.001(2) -0.009(2) O1 0.030(3) 0.024(3) 0.020(2) -0.007(2) 0.005(2) -0.008(2) O2 0.021(3) 0.018(3) 0.029(3) -0.008(2) 0.006(2) -0.004(2) O3 0.049(4) 0.038(3) 0.038(3) -0.014(3) -0.022(3) -0.007(3) O4 0.035(3) 0.017(3) 0.029(3) -0.014(2) 0.006(2) -0.005(2) O5 0.043(3) 0.043(4) 0.028(3) -0.009(3) -0.003(3) -0.023(3) O6 0.013(2) 0.031(3) 0.023(2) -0.008(2) -0.007(2) 0.005(2) O7 0.021(3) 0.045(3) 0.018(2) -0.015(2) -0.005(2) 0.006(2) O8 0.008(2) 0.023(3) 0.024(2) -0.004(2) -0.0015(19) -0.0006(19) O9 0.028(3) 0.075(5) 0.029(3) 0.004(3) -0.010(3) -0.030(3) O10 0.029(3) 0.065(4) 0.034(3) -0.027(3) 0.003(3) -0.025(3) O1W 0.015(2) 0.034(3) 0.021(2) -0.012(2) -0.003(2) -0.002(2) O2W 0.062(5) 0.065(5) 0.087(6) 0.023(4) -0.028(4) -0.024(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 Ag1 N3 2.189(6) 2_664 ? Ag1 N1 2.206(6) . ? Ag1 O3 2.400(5) 1_554 ? Dy1 O4 2.296(5) 2_566 ? Dy1 O2 2.302(5) 2_556 ? Dy1 O8 2.332(4) 2_456 ? Dy1 O1 2.358(5) . ? Dy1 O6 2.365(4) 2_556 ? Dy1 O1W 2.360(4) . ? Dy1 O7 2.389(5) . ? Dy1 O6 2.629(4) . ? C1 O1 1.257(8) . ? C1 O2 1.260(8) . ? C1 C2 1.497(9) . ? C2 C7 1.385(9) . ? C2 C3 1.389(9) . ? C3 C4 1.404(10) . ? C3 H3 0.9300 . ? C4 N2 1.403(9) . ? C4 C5 1.396(9) . ? C5 C6 1.387(10) . ? C5 H5 0.9300 . ? C6 C7 1.384(9) . ? C6 C14 1.514(9) . ? C7 H7 0.9300 . ? C8 O5 1.220(9) . ? C8 N2 1.355(9) . ? C8 C9 1.498(10) . ? C9 C13 1.387(10) . ? C9 C10 1.382(10) . ? C10 C11 1.379(10) . ? C10 H10 0.9300 . ? C11 N1 1.337(10) . ? C11 H11 0.9300 . ? C12 N1 1.327(10) . ? C12 C13 1.398(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O3 1.230(9) . ? C14 O4 1.276(9) . ? C15 O7 1.252(8) . ? C15 O6 1.265(8) . ? C15 C16 1.499(9) . ? C16 C17 1.393(9) . ? C16 C21 1.405(9) . ? C17 C18 1.382(9) . ? C17 H17 0.9300 . ? C18 C19 1.384(9) . ? C18 C28 1.492(9) . ? C19 C20 1.374(9) . ? C19 H19 0.9300 . ? C20 C21 1.377(9) . ? C20 N4 1.426(8) . ? C21 H21 0.9300 . ? C22 O10 1.217(8) . ? C22 N4 1.346(8) . ? C22 C23 1.494(9) . ? C23 C24 1.377(10) . ? C23 C27 1.373(10) . ? C24 C25 1.366(10) . ? C24 H24 0.9300 . ? C25 N3 1.354(10) . ? C25 H25 0.9300 . ? C26 N3 1.320(9) . ? C26 C27 1.380(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O8 1.255(8) . ? C28 O9 1.258(9) . ? N2 H2 0.8600 . ? N3 Ag1 2.189(6) 2_664 ? N4 H4 0.8600 . ? O2 Dy1 2.302(5) 2_556 ? O3 Ag1 2.400(5) 1_556 ? O4 Dy1 2.296(5) 2_566 ? O6 Dy1 2.365(4) 2_556 ? O8 Dy1 2.332(4) 2_456 ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? 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 N3 Ag1 N1 146.5(2) 2_664 . ? N3 Ag1 O3 115.2(2) 2_664 1_554 ? N1 Ag1 O3 92.3(2) . 1_554 ? O4 Dy1 O2 149.60(16) 2_566 2_556 ? O4 Dy1 O8 79.37(17) 2_566 2_456 ? O2 Dy1 O8 74.31(16) 2_556 2_456 ? O4 Dy1 O1 73.35(17) 2_566 . ? O2 Dy1 O1 136.61(16) 2_556 . ? O8 Dy1 O1 145.27(17) 2_456 . ? O4 Dy1 O6 124.98(18) 2_566 2_556 ? O2 Dy1 O6 71.70(17) 2_556 2_556 ? O8 Dy1 O6 140.71(16) 2_456 2_556 ? O1 Dy1 O6 73.82(17) . 2_556 ? O4 Dy1 O1W 77.39(17) 2_566 . ? O2 Dy1 O1W 81.62(17) 2_556 . ? O8 Dy1 O1W 75.84(16) 2_456 . ? O1 Dy1 O1W 117.42(17) . . ? O6 Dy1 O1W 80.23(16) 2_556 . ? O4 Dy1 O7 96.78(18) 2_566 . ? O2 Dy1 O7 89.05(18) 2_556 . ? O8 Dy1 O7 71.34(16) 2_456 . ? O1 Dy1 O7 90.77(18) . . ? O6 Dy1 O7 126.45(16) 2_556 . ? O1W Dy1 O7 147.18(17) . . ? O4 Dy1 O6 130.91(17) 2_566 . ? O2 Dy1 O6 75.07(16) 2_556 . ? O8 Dy1 O6 114.39(15) 2_456 . ? O1 Dy1 O6 71.14(15) . . ? O6 Dy1 O6 74.95(16) 2_556 . ? O1W Dy1 O6 150.14(16) . . ? O7 Dy1 O6 51.66(15) . . ? O4 Dy1 Dy1 140.88(12) 2_566 2_556 ? O2 Dy1 Dy1 69.02(11) 2_556 2_556 ? O8 Dy1 Dy1 137.32(12) 2_456 2_556 ? O1 Dy1 Dy1 67.65(12) . 2_556 ? O6 Dy1 Dy1 39.79(11) 2_556 2_556 ? O1W Dy1 Dy1 118.27(11) . 2_556 ? O7 Dy1 Dy1 86.75(11) . 2_556 ? O6 Dy1 Dy1 35.16(10) . 2_556 ? O1 C1 O2 126.5(7) . . ? O1 C1 C2 117.5(6) . . ? O2 C1 C2 116.1(6) . . ? C7 C2 C3 121.2(6) . . ? C7 C2 C1 119.7(6) . . ? C3 C2 C1 119.0(6) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? N2 C4 C5 117.8(6) . . ? N2 C4 C3 122.4(6) . . ? C5 C4 C3 119.6(6) . . ? C6 C5 C4 120.4(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.9(6) . . ? C5 C6 C14 120.5(6) . . ? C7 C6 C14 119.3(6) . . ? C2 C7 C6 119.7(6) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O5 C8 N2 122.9(6) . . ? O5 C8 C9 121.8(7) . . ? N2 C8 C9 115.3(6) . . ? C13 C9 C10 118.6(7) . . ? C13 C9 C8 122.2(7) . . ? C10 C9 C8 119.1(6) . . ? C11 C10 C9 118.9(7) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? N1 C11 C10 123.8(7) . . ? N1 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? N1 C12 C13 124.2(8) . . ? N1 C12 H12 117.9 . . ? C13 C12 H12 117.9 . . ? C9 C13 C12 117.8(7) . . ? C9 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? O3 C14 O4 126.3(7) . . ? O3 C14 C6 116.8(7) . . ? O4 C14 C6 116.8(6) . . ? O7 C15 O6 121.5(6) . . ? O7 C15 C16 119.6(6) . . ? O6 C15 C16 118.9(6) . . ? C17 C16 C21 119.8(6) . . ? C17 C16 C15 120.1(6) . . ? C21 C16 C15 119.9(6) . . ? C18 C17 C16 119.8(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.8(6) . . ? C17 C18 C28 120.1(6) . . ? C19 C18 C28 120.0(6) . . ? C20 C19 C18 120.7(6) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.5(6) . . ? C19 C20 N4 122.8(6) . . ? C21 C20 N4 116.8(6) . . ? C20 C21 C16 119.4(6) . . ? C20 C21 H21 120.3 . . ? C16 C21 H21 120.3 . . ? O10 C22 N4 122.7(6) . . ? O10 C22 C23 120.1(6) . . ? N4 C22 C23 117.2(6) . . ? C24 C23 C27 117.9(7) . . ? C24 C23 C22 117.5(6) . . ? C27 C23 C22 124.5(6) . . ? C25 C24 C23 120.0(7) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? N3 C25 C24 122.3(7) . . ? N3 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N3 C26 C27 123.5(7) . . ? N3 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C23 C27 C26 119.1(7) . . ? C23 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? O8 C28 O9 123.5(6) . . ? O8 C28 C18 117.8(6) . . ? O9 C28 C18 118.7(6) . . ? C12 N1 C11 116.7(6) . . ? C12 N1 Ag1 122.0(5) . . ? C11 N1 Ag1 121.1(5) . . ? C8 N2 C4 127.8(6) . . ? C8 N2 H2 116.1 . . ? C4 N2 H2 116.1 . . ? C26 N3 C25 117.3(6) . . ? C26 N3 Ag1 124.2(5) . 2_664 ? C25 N3 Ag1 118.4(5) . 2_664 ? C22 N4 C20 124.8(6) . . ? C22 N4 H4 117.6 . . ? C20 N4 H4 117.6 . . ? C1 O1 Dy1 134.7(4) . . ? C1 O2 Dy1 135.9(4) . 2_556 ? C14 O3 Ag1 121.1(5) . 1_556 ? C14 O4 Dy1 127.8(4) . 2_566 ? C15 O6 Dy1 166.5(4) . 2_556 ? C15 O6 Dy1 87.6(4) . . ? Dy1 O6 Dy1 105.05(16) 2_556 . ? C15 O7 Dy1 99.2(4) . . ? C28 O8 Dy1 136.7(4) . 2_456 ? Dy1 O1W H1WB 110.7 . . ? Dy1 O1W H1WA 110.6 . . ? H1WB O1W H1WA 108.9 . . ? H2WA O2W H2WB 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 38.8(9) . . . . ? O2 C1 C2 C7 -139.8(6) . . . . ? O1 C1 C2 C3 -144.3(7) . . . . ? O2 C1 C2 C3 37.0(9) . . . . ? C7 C2 C3 C4 -3.3(10) . . . . ? C1 C2 C3 C4 179.9(6) . . . . ? C2 C3 C4 N2 179.9(7) . . . . ? C2 C3 C4 C5 4.2(11) . . . . ? N2 C4 C5 C6 -176.4(7) . . . . ? C3 C4 C5 C6 -0.4(11) . . . . ? C4 C5 C6 C7 -4.3(11) . . . . ? C4 C5 C6 C14 171.1(6) . . . . ? C3 C2 C7 C6 -1.3(10) . . . . ? C1 C2 C7 C6 175.5(6) . . . . ? C5 C6 C7 C2 5.1(10) . . . . ? C14 C6 C7 C2 -170.2(6) . . . . ? O5 C8 C9 C13 -145.2(8) . . . . ? N2 C8 C9 C13 36.3(11) . . . . ? O5 C8 C9 C10 32.2(11) . . . . ? N2 C8 C9 C10 -146.2(7) . . . . ? C13 C9 C10 C11 -0.5(12) . . . . ? C8 C9 C10 C11 -178.0(7) . . . . ? C9 C10 C11 N1 1.2(13) . . . . ? C10 C9 C13 C12 -0.4(12) . . . . ? C8 C9 C13 C12 177.0(8) . . . . ? N1 C12 C13 C9 0.9(14) . . . . ? C5 C6 C14 O3 -154.0(7) . . . . ? C7 C6 C14 O3 21.4(10) . . . . ? C5 C6 C14 O4 23.1(10) . . . . ? C7 C6 C14 O4 -161.5(6) . . . . ? O7 C15 C16 C17 -45.4(10) . . . . ? O6 C15 C16 C17 134.4(7) . . . . ? O7 C15 C16 C21 139.4(7) . . . . ? O6 C15 C16 C21 -40.9(9) . . . . ? C21 C16 C17 C18 -1.6(10) . . . . ? C15 C16 C17 C18 -176.9(6) . . . . ? C16 C17 C18 C19 0.0(11) . . . . ? C16 C17 C18 C28 -179.7(7) . . . . ? C17 C18 C19 C20 1.7(11) . . . . ? C28 C18 C19 C20 -178.7(7) . . . . ? C18 C19 C20 C21 -1.7(11) . . . . ? C18 C19 C20 N4 176.8(7) . . . . ? C19 C20 C21 C16 0.1(11) . . . . ? N4 C20 C21 C16 -178.5(6) . . . . ? C17 C16 C21 C20 1.6(10) . . . . ? C15 C16 C21 C20 176.9(6) . . . . ? O10 C22 C23 C24 33.5(11) . . . . ? N4 C22 C23 C24 -146.1(7) . . . . ? O10 C22 C23 C27 -141.8(8) . . . . ? N4 C22 C23 C27 38.7(11) . . . . ? C27 C23 C24 C25 -1.1(12) . . . . ? C22 C23 C24 C25 -176.7(8) . . . . ? C23 C24 C25 N3 0.6(13) . . . . ? C24 C23 C27 C26 0.4(12) . . . . ? C22 C23 C27 C26 175.6(8) . . . . ? N3 C26 C27 C23 1.0(13) . . . . ? C17 C18 C28 O8 -21.6(10) . . . . ? C19 C18 C28 O8 158.8(7) . . . . ? C17 C18 C28 O9 158.3(7) . . . . ? C19 C18 C28 O9 -21.3(11) . . . . ? C13 C12 N1 C11 -0.3(14) . . . . ? C13 C12 N1 Ag1 174.1(7) . . . . ? C10 C11 N1 C12 -0.7(13) . . . . ? C10 C11 N1 Ag1 -175.2(6) . . . . ? N3 Ag1 N1 C12 29.0(9) 2_664 . . . ? O3 Ag1 N1 C12 175.2(7) 1_554 . . . ? N3 Ag1 N1 C11 -156.8(6) 2_664 . . . ? O3 Ag1 N1 C11 -10.6(7) 1_554 . . . ? O5 C8 N2 C4 3.8(13) . . . . ? C9 C8 N2 C4 -177.8(7) . . . . ? C5 C4 N2 C8 -156.1(7) . . . . ? C3 C4 N2 C8 28.1(12) . . . . ? C27 C26 N3 C25 -1.5(13) . . . . ? C27 C26 N3 Ag1 -178.3(6) . . . 2_664 ? C24 C25 N3 C26 0.7(13) . . . . ? C24 C25 N3 Ag1 177.7(7) . . . 2_664 ? O10 C22 N4 C20 6.6(12) . . . . ? C23 C22 N4 C20 -173.9(6) . . . . ? C19 C20 N4 C22 -33.8(11) . . . . ? C21 C20 N4 C22 144.8(7) . . . . ? O2 C1 O1 Dy1 -35.2(11) . . . . ? C2 C1 O1 Dy1 146.3(5) . . . . ? O4 Dy1 O1 C1 -164.3(7) 2_566 . . . ? O2 Dy1 O1 C1 22.0(8) 2_556 . . . ? O8 Dy1 O1 C1 -124.6(6) 2_456 . . . ? O6 Dy1 O1 C1 60.5(6) 2_556 . . . ? O1W Dy1 O1 C1 130.0(6) . . . . ? O7 Dy1 O1 C1 -67.5(7) . . . . ? O6 Dy1 O1 C1 -18.8(6) . . . . ? Dy1 Dy1 O1 C1 18.7(6) 2_556 . . . ? O1 C1 O2 Dy1 29.8(11) . . . 2_556 ? C2 C1 O2 Dy1 -151.7(5) . . . 2_556 ? O4 C14 O3 Ag1 -47.8(9) . . . 1_556 ? C6 C14 O3 Ag1 128.9(5) . . . 1_556 ? O3 C14 O4 Dy1 -32.0(10) . . . 2_566 ? C6 C14 O4 Dy1 151.3(5) . . . 2_566 ? O7 C15 O6 Dy1 160.4(15) . . . 2_556 ? C16 C15 O6 Dy1 -19(2) . . . 2_556 ? O7 C15 O6 Dy1 0.6(6) . . . . ? C16 C15 O6 Dy1 -179.1(5) . . . . ? O4 Dy1 O6 C15 -61.2(4) 2_566 . . . ? O2 Dy1 O6 C15 100.6(4) 2_556 . . . ? O8 Dy1 O6 C15 35.9(4) 2_456 . . . ? O1 Dy1 O6 C15 -107.1(4) . . . . ? O6 Dy1 O6 C15 175.2(5) 2_556 . . . ? O1W Dy1 O6 C15 140.4(4) . . . . ? O7 Dy1 O6 C15 -0.3(4) . . . . ? Dy1 Dy1 O6 C15 175.2(5) 2_556 . . . ? O4 Dy1 O6 Dy1 123.5(2) 2_566 . . 2_556 ? O2 Dy1 O6 Dy1 -74.6(2) 2_556 . . 2_556 ? O8 Dy1 O6 Dy1 -139.29(17) 2_456 . . 2_556 ? O1 Dy1 O6 Dy1 77.7(2) . . . 2_556 ? O6 Dy1 O6 Dy1 0.0 2_556 . . 2_556 ? O1W Dy1 O6 Dy1 -34.8(4) . . . 2_556 ? O7 Dy1 O6 Dy1 -175.5(3) . . . 2_556 ? O6 C15 O7 Dy1 -0.7(7) . . . . ? C16 C15 O7 Dy1 179.1(5) . . . . ? O4 Dy1 O7 C15 138.7(4) 2_566 . . . ? O2 Dy1 O7 C15 -71.3(4) 2_556 . . . ? O8 Dy1 O7 C15 -145.0(5) 2_456 . . . ? O1 Dy1 O7 C15 65.3(4) . . . . ? O6 Dy1 O7 C15 -5.0(5) 2_556 . . . ? O1W Dy1 O7 C15 -144.1(4) . . . . ? O6 Dy1 O7 C15 0.3(4) . . . . ? Dy1 Dy1 O7 C15 -2.2(4) 2_556 . . . ? O9 C28 O8 Dy1 -30.8(11) . . . 2_456 ? C18 C28 O8 Dy1 149.0(5) . . . 2_456 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.979 _refine_diff_density_min -2.305 _refine_diff_density_rms 0.208 data_10 _database_code_depnum_ccdc_archive 'CCDC 760894' #TrackingRef 'sunwy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Ag Er N4 O12' _chemical_formula_weight 879.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.8334(14) _cell_length_b 11.3098(17) _cell_length_c 13.721(2) _cell_angle_alpha 73.916(3) _cell_angle_beta 70.673(2) _cell_angle_gamma 83.962(3) _cell_volume 1383.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4850 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.24 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 854 _exptl_absorpt_coefficient_mu 3.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5173 _exptl_absorpt_correction_T_max 0.6587 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6926 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4796 _reflns_number_gt 4408 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0637P)^2^+0.6046P] 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 4796 _refine_ls_number_parameters 409 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 1.04940(6) 1.30980(6) 0.01448(4) 0.039 Uani 1 1 d . . . Er1 Er 0.34566(2) 1.06186(2) 1.109377(18) 0.01391(8) Uani 1 1 d U . . C8 C 0.2805(6) 0.3448(5) 1.1225(5) 0.0229(13) Uani 1 1 d . . . C6 C 0.3081(6) 0.4387(5) 1.1717(5) 0.0200(12) Uani 1 1 d . . . C7 C 0.3499(6) 0.5536(5) 1.1098(4) 0.0212(13) Uani 1 1 d . . . H7 H 0.3763 0.5690 1.0359 0.025 Uiso 1 1 calc R . . C2 C 0.3539(6) 0.6489(5) 1.1552(4) 0.0174(12) Uani 1 1 d . . . C3 C 0.3197(6) 0.6251(5) 1.2653(5) 0.0222(13) Uani 1 1 d . . . H3 H 0.3180 0.6883 1.2970 0.027 Uiso 1 1 calc R . . C4 C 0.2875(6) 0.5034(5) 1.3286(5) 0.0219(13) Uani 1 1 d . . . C5 C 0.2836(6) 0.4127(6) 1.2805(5) 0.0243(13) Uani 1 1 d . . . H5 H 0.2640 0.3324 1.3220 0.029 Uiso 1 1 calc R . . C1 C 0.3871(6) 0.7782(6) 1.0883(5) 0.0224(13) Uani 1 1 d . . . C9 C 0.2937(6) 0.5308(6) 1.5006(5) 0.0264(14) Uani 1 1 d . . . C10 C 0.2322(6) 0.4773(5) 1.6191(5) 0.0228(13) Uani 1 1 d . . . C11 C 0.3145(7) 0.4806(6) 1.6829(5) 0.0299(15) Uani 1 1 d . . . H11 H 0.4070 0.5125 1.6526 0.036 Uiso 1 1 calc R . . C12 C 0.2575(7) 0.4359(6) 1.7921(5) 0.0306(15) Uani 1 1 d . . . H12 H 0.3152 0.4342 1.8342 0.037 Uiso 1 1 calc R . . C13 C 0.0452(7) 0.3934(8) 1.7782(5) 0.0410(19) Uani 1 1 d . . . H13 H -0.0479 0.3633 1.8106 0.049 Uiso 1 1 calc R . . C14 C 0.0957(7) 0.4346(7) 1.6673(5) 0.0360(17) Uani 1 1 d . . . H14 H 0.0368 0.4330 1.6268 0.043 Uiso 1 1 calc R . . C22 C -0.0299(6) 1.0442(6) 0.7171(5) 0.0259(14) Uani 1 1 d . . . C18 C 0.1140(6) 1.0814(5) 0.7142(5) 0.0204(12) Uani 1 1 d . . . C19 C 0.2182(6) 1.1240(5) 0.6165(4) 0.0198(12) Uani 1 1 d . . . H19 H 0.1982 1.1316 0.5533 0.024 Uiso 1 1 calc R . . C20 C 0.3516(6) 1.1549(5) 0.6132(4) 0.0185(12) Uani 1 1 d . . . C21 C 0.3818(6) 1.1446(6) 0.7073(5) 0.0227(13) Uani 1 1 d . . . H21 H 0.4719 1.1659 0.7048 0.027 Uiso 1 1 calc R . . C16 C 0.2763(6) 1.1023(5) 0.8053(4) 0.0185(12) Uani 1 1 d . . . C17 C 0.1427(6) 1.0710(6) 0.8083(5) 0.0221(13) Uani 1 1 d . . . H17 H 0.0720 1.0429 0.8737 0.027 Uiso 1 1 calc R . . C15 C 0.3104(6) 1.0855(5) 0.9051(4) 0.0147(11) Uani 1 1 d . . . C23 C 0.4870(6) 1.1559(6) 0.4281(5) 0.0241(13) Uani 1 1 d . . . C24 C 0.6213(6) 1.2004(6) 0.3364(5) 0.0249(13) Uani 1 1 d . . . C25 C 0.6138(7) 1.2218(7) 0.2339(5) 0.0353(17) Uani 1 1 d . . . H25 H 0.5266 1.2147 0.2234 0.042 Uiso 1 1 calc R . . C26 C 0.7361(7) 1.2537(7) 0.1479(5) 0.0322(16) Uani 1 1 d . . . H26 H 0.7296 1.2693 0.0794 0.039 Uiso 1 1 calc R . . C27 C 0.8702(7) 1.2414(6) 0.2577(5) 0.0301(15) Uani 1 1 d . . . H27 H 0.9591 1.2471 0.2661 0.036 Uiso 1 1 calc R . . C28 C 0.7518(7) 1.2109(6) 0.3478(5) 0.0283(14) Uani 1 1 d . . . H28 H 0.7607 1.1977 0.4154 0.034 Uiso 1 1 calc R . . N3 N 0.8628(6) 1.2631(5) 0.1590(4) 0.0285(12) Uani 1 1 d . . . N4 N 0.4646(5) 1.1977(5) 0.5151(4) 0.0228(11) Uani 1 1 d . . . H4 H 0.5212 1.2530 0.5114 0.027 Uiso 1 1 calc R . . N1 N 0.1237(6) 0.3951(5) 1.8398(4) 0.0315(13) Uani 1 1 d . . . N2 N 0.2513(6) 0.4738(5) 1.4413(4) 0.0274(12) Uani 1 1 d . . . H2 H 0.1955 0.4120 1.4763 0.033 Uiso 1 1 calc R . . O1 O 0.2825(5) 0.2311(4) 1.1731(3) 0.0294(10) Uani 1 1 d . . . O2 O 0.2530(5) 0.3822(4) 1.0377(4) 0.0354(11) Uani 1 1 d . . . O3 O 0.4839(4) 0.7910(4) 0.9984(3) 0.0270(10) Uani 1 1 d . . . O4 O 0.3144(4) 0.8595(3) 1.1265(3) 0.0242(9) Uani 1 1 d . . . O5 O 0.3749(5) 0.6161(4) 1.4628(3) 0.0338(11) Uani 1 1 d . . . O6 O 0.2209(4) 1.1183(4) 0.9831(3) 0.0266(10) Uani 1 1 d . . . O7 O 0.4295(4) 1.0366(4) 0.9133(3) 0.0207(8) Uani 1 1 d U . . O8 O -0.1038(4) 0.9733(4) 0.8013(3) 0.0209(9) Uani 1 1 d . . . O9 O -0.0695(5) 1.0900(6) 0.6368(4) 0.0495(16) Uani 1 1 d . . . O10 O 0.4038(5) 1.0908(5) 0.4201(4) 0.0420(13) Uani 1 1 d . . . O2W O 0.0055(6) 0.3133(6) 0.4944(5) 0.074(2) Uani 1 1 d . . . H2WA H -0.0625 0.3627 0.5150 0.089 Uiso 1 1 d R . . H2WB H -0.0026 0.2451 0.5416 0.089 Uiso 1 1 d R . . O1W O 0.3340(4) 0.9853(4) 1.2875(3) 0.0223(9) Uani 1 1 d . . . H1WA H 0.2922 0.9177 1.3239 0.027 Uiso 1 1 d R . . H1WB H 0.3717 1.0249 1.3163 0.027 Uiso 1 1 d 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 Ag1 0.029 0.061 0.019 -0.004 0.000 -0.011 Er1 0.01601(14) 0.01320(14) 0.01264(14) -0.00331(10) -0.00380(10) -0.00323(9) C8 0.023(3) 0.018(3) 0.023(3) -0.007(3) 0.002(3) -0.006(2) C6 0.022(3) 0.020(3) 0.018(3) -0.006(2) -0.006(2) -0.003(2) C7 0.021(3) 0.025(3) 0.016(3) -0.006(3) -0.003(2) -0.003(2) C2 0.020(3) 0.008(3) 0.022(3) -0.002(2) -0.003(2) -0.007(2) C3 0.028(3) 0.020(3) 0.023(3) -0.013(3) -0.006(3) -0.003(2) C4 0.030(3) 0.015(3) 0.019(3) -0.002(2) -0.006(3) -0.006(2) C5 0.026(3) 0.021(3) 0.022(3) -0.006(3) -0.001(3) -0.006(3) C1 0.021(3) 0.027(3) 0.022(3) -0.008(3) -0.007(3) -0.006(3) C9 0.025(3) 0.036(4) 0.019(3) -0.008(3) -0.007(3) -0.002(3) C10 0.029(3) 0.020(3) 0.017(3) -0.004(2) -0.005(3) -0.004(2) C11 0.025(3) 0.041(4) 0.022(3) -0.009(3) -0.006(3) -0.003(3) C12 0.033(4) 0.032(4) 0.026(4) -0.003(3) -0.010(3) -0.004(3) C13 0.022(3) 0.074(6) 0.020(4) -0.003(3) -0.002(3) -0.010(3) C14 0.032(4) 0.054(5) 0.026(4) -0.008(3) -0.014(3) -0.008(3) C22 0.023(3) 0.035(4) 0.021(3) -0.009(3) -0.005(3) -0.008(3) C18 0.018(3) 0.024(3) 0.020(3) -0.006(2) -0.006(2) -0.004(2) C19 0.020(3) 0.024(3) 0.013(3) -0.003(2) -0.003(2) -0.004(2) C20 0.017(3) 0.026(3) 0.012(3) -0.008(2) -0.003(2) -0.002(2) C21 0.015(3) 0.029(3) 0.023(3) -0.010(3) -0.004(2) 0.003(2) C16 0.020(3) 0.016(3) 0.017(3) -0.004(2) -0.003(2) 0.001(2) C17 0.015(3) 0.025(3) 0.020(3) -0.003(2) 0.000(2) -0.004(2) C15 0.017(3) 0.013(3) 0.015(3) -0.001(2) -0.006(2) -0.007(2) C23 0.020(3) 0.037(4) 0.014(3) -0.005(3) -0.003(2) -0.006(3) C24 0.025(3) 0.029(3) 0.018(3) -0.008(3) -0.001(3) -0.004(3) C25 0.025(3) 0.058(5) 0.020(3) -0.008(3) -0.004(3) -0.002(3) C26 0.027(3) 0.045(4) 0.018(3) -0.002(3) -0.002(3) -0.002(3) C27 0.022(3) 0.033(4) 0.032(4) -0.009(3) -0.002(3) -0.009(3) C28 0.031(3) 0.033(4) 0.019(3) -0.007(3) -0.005(3) -0.004(3) N3 0.028(3) 0.030(3) 0.021(3) -0.003(2) -0.001(2) -0.004(2) N4 0.017(2) 0.035(3) 0.014(2) -0.005(2) 0.0009(19) -0.012(2) N1 0.032(3) 0.036(3) 0.022(3) -0.003(2) -0.004(2) -0.002(2) N2 0.042(3) 0.021(3) 0.017(3) -0.002(2) -0.006(2) -0.014(2) O1 0.039(3) 0.021(2) 0.024(2) -0.0099(19) 0.0021(19) -0.0066(19) O2 0.051(3) 0.030(3) 0.036(3) -0.010(2) -0.025(2) -0.005(2) O3 0.031(2) 0.019(2) 0.023(2) -0.0065(18) 0.0049(19) -0.0075(18) O4 0.029(2) 0.009(2) 0.028(2) -0.0072(17) 0.0022(18) -0.0028(17) O5 0.046(3) 0.032(3) 0.023(2) -0.004(2) -0.005(2) -0.025(2) O6 0.024(2) 0.040(3) 0.016(2) -0.0112(19) -0.0067(18) 0.0050(19) O7 0.023(2) 0.024(2) 0.0150(14) -0.0052(16) -0.0054(16) -0.0014(17) O8 0.020(2) 0.019(2) 0.021(2) -0.0016(17) -0.0048(17) -0.0065(16) O9 0.029(3) 0.092(4) 0.020(3) 0.014(3) -0.012(2) -0.034(3) O10 0.039(3) 0.062(4) 0.031(3) -0.025(2) 0.001(2) -0.028(3) O2W 0.064(4) 0.054(4) 0.084(5) 0.025(3) -0.029(4) -0.021(3) O1W 0.028(2) 0.021(2) 0.021(2) -0.0044(17) -0.0103(18) -0.0077(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.189(5) . ? Ag1 N1 2.218(5) 1_663 ? Ag1 O2 2.386(5) 1_664 ? Er1 O1 2.265(4) 1_565 ? Er1 O4 2.279(4) . ? Er1 O8 2.306(4) 2_577 ? Er1 O3 2.312(4) 2_677 ? Er1 O1W 2.324(4) . ? Er1 O7 2.333(4) 2_677 ? Er1 O6 2.355(4) . ? Er1 O7 2.628(4) . ? C8 O2 1.232(8) . ? C8 O1 1.282(7) . ? C8 C6 1.495(8) . ? C6 C7 1.360(8) . ? C6 C5 1.380(8) . ? C7 C2 1.396(8) . ? C7 H7 0.9300 . ? C2 C3 1.387(8) . ? C2 C1 1.499(8) . ? C3 C4 1.413(8) . ? C3 H3 0.9300 . ? C4 C5 1.375(8) . ? C4 N2 1.416(8) . ? C5 H5 0.9300 . ? C1 O4 1.229(7) . ? C1 O3 1.265(7) . ? C9 O5 1.203(7) . ? C9 N2 1.350(8) . ? C9 C10 1.502(8) . ? C10 C14 1.358(9) . ? C10 C11 1.385(9) . ? C11 C12 1.378(9) . ? C11 H11 0.9300 . ? C12 N1 1.327(8) . ? C12 H12 0.9300 . ? C13 N1 1.324(9) . ? C13 C14 1.391(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C22 O9 1.249(8) . ? C22 O8 1.249(7) . ? C22 C18 1.503(8) . ? C18 C17 1.382(8) . ? C18 C19 1.384(8) . ? C19 C20 1.376(8) . ? C19 H19 0.9300 . ? C20 C21 1.389(8) . ? C20 N4 1.430(7) . ? C21 C16 1.392(8) . ? C21 H21 0.9300 . ? C16 C17 1.381(8) . ? C16 C15 1.473(8) . ? C17 H17 0.9300 . ? C15 O6 1.258(7) . ? C15 O7 1.268(7) . ? C23 O10 1.207(7) . ? C23 N4 1.347(8) . ? C23 C24 1.506(8) . ? C24 C28 1.363(9) . ? C24 C25 1.385(9) . ? C25 C26 1.373(9) . ? C25 H25 0.9300 . ? C26 N3 1.322(8) . ? C26 H26 0.9300 . ? C27 N3 1.333(8) . ? C27 C28 1.378(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? N4 H4 0.8600 . ? N1 Ag1 2.218(5) 1_447 ? N2 H2 0.8600 . ? O1 Er1 2.265(4) 1_545 ? O2 Ag1 2.386(5) 1_446 ? O3 Er1 2.312(4) 2_677 ? O7 Er1 2.333(4) 2_677 ? O8 Er1 2.306(4) 2_577 ? O2W H2WA 0.8501 . ? O2W H2WB 0.8501 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8499 . ? 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 N3 Ag1 N1 145.8(2) . 1_663 ? N3 Ag1 O2 115.16(19) . 1_664 ? N1 Ag1 O2 92.33(19) 1_663 1_664 ? O1 Er1 O4 149.88(15) 1_565 . ? O1 Er1 O8 79.54(15) 1_565 2_577 ? O4 Er1 O8 74.52(14) . 2_577 ? O1 Er1 O3 73.52(15) 1_565 2_677 ? O4 Er1 O3 136.18(14) . 2_677 ? O8 Er1 O3 145.14(15) 2_577 2_677 ? O1 Er1 O1W 77.54(15) 1_565 . ? O4 Er1 O1W 81.50(15) . . ? O8 Er1 O1W 75.97(14) 2_577 . ? O3 Er1 O1W 118.05(15) 2_677 . ? O1 Er1 O7 124.45(15) 1_565 2_677 ? O4 Er1 O7 72.17(14) . 2_677 ? O8 Er1 O7 141.56(14) 2_577 2_677 ? O3 Er1 O7 73.17(14) 2_677 2_677 ? O1W Er1 O7 80.62(14) . 2_677 ? O1 Er1 O6 96.27(16) 1_565 . ? O4 Er1 O6 89.95(16) . . ? O8 Er1 O6 71.69(14) 2_577 . ? O3 Er1 O6 89.51(16) 2_677 . ? O1W Er1 O6 147.66(14) . . ? O7 Er1 O6 126.31(13) 2_677 . ? O1 Er1 O7 131.32(14) 1_565 . ? O4 Er1 O7 74.45(13) . . ? O8 Er1 O7 113.90(13) 2_577 . ? O3 Er1 O7 71.18(14) 2_677 . ? O1W Er1 O7 149.71(14) . . ? O7 Er1 O7 74.72(14) 2_677 . ? O6 Er1 O7 51.63(13) . . ? O1 Er1 Er1 140.71(11) 1_565 2_677 ? O4 Er1 Er1 68.93(10) . 2_677 ? O8 Er1 Er1 137.11(10) 2_577 2_677 ? O3 Er1 Er1 67.30(10) 2_677 2_677 ? O1W Er1 Er1 118.60(10) . 2_677 ? O7 Er1 Er1 39.96(9) 2_677 2_677 ? O6 Er1 Er1 86.37(10) . 2_677 ? O7 Er1 Er1 34.76(8) . 2_677 ? O2 C8 O1 124.4(6) . . ? O2 C8 C6 117.7(5) . . ? O1 C8 C6 117.9(6) . . ? C7 C6 C5 119.2(6) . . ? C7 C6 C8 119.8(5) . . ? C5 C6 C8 120.9(5) . . ? C6 C7 C2 121.3(5) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C3 C2 C7 119.5(5) . . ? C3 C2 C1 118.9(5) . . ? C7 C2 C1 121.5(5) . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.4(6) . . ? C5 C4 N2 119.1(5) . . ? C3 C4 N2 121.5(5) . . ? C4 C5 C6 121.3(6) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.3 . . ? O4 C1 O3 127.6(6) . . ? O4 C1 C2 115.9(5) . . ? O3 C1 C2 116.5(5) . . ? O5 C9 N2 123.6(6) . . ? O5 C9 C10 122.3(6) . . ? N2 C9 C10 114.1(5) . . ? C14 C10 C11 118.4(6) . . ? C14 C10 C9 123.0(6) . . ? C11 C10 C9 118.4(5) . . ? C12 C11 C10 119.0(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? N1 C12 C11 122.9(6) . . ? N1 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? N1 C13 C14 123.0(6) . . ? N1 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C10 C14 C13 119.0(6) . . ? C10 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O9 C22 O8 124.6(6) . . ? O9 C22 C18 117.8(5) . . ? O8 C22 C18 117.5(5) . . ? C17 C18 C19 120.4(5) . . ? C17 C18 C22 120.3(5) . . ? C19 C18 C22 119.3(5) . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.4(5) . . ? C19 C20 N4 122.5(5) . . ? C21 C20 N4 117.1(5) . . ? C20 C21 C16 119.6(5) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? C17 C16 C21 119.8(5) . . ? C17 C16 C15 120.4(5) . . ? C21 C16 C15 119.7(5) . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? O6 C15 O7 119.7(5) . . ? O6 C15 C16 120.2(5) . . ? O7 C15 C16 120.1(5) . . ? O10 C23 N4 123.4(5) . . ? O10 C23 C24 120.6(5) . . ? N4 C23 C24 115.9(5) . . ? C28 C24 C25 118.1(6) . . ? C28 C24 C23 124.3(6) . . ? C25 C24 C23 117.4(6) . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N3 C26 C25 122.4(6) . . ? N3 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N3 C27 C28 122.9(6) . . ? N3 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C24 C28 C27 119.1(6) . . ? C24 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C26 N3 C27 118.1(5) . . ? C26 N3 Ag1 118.3(4) . . ? C27 N3 Ag1 123.7(4) . . ? C23 N4 C20 123.4(5) . . ? C23 N4 H4 118.3 . . ? C20 N4 H4 118.3 . . ? C13 N1 C12 117.7(6) . . ? C13 N1 Ag1 122.0(4) . 1_447 ? C12 N1 Ag1 119.7(4) . 1_447 ? C9 N2 C4 127.8(5) . . ? C9 N2 H2 116.1 . . ? C4 N2 H2 116.1 . . ? C8 O1 Er1 129.8(4) . 1_545 ? C8 O2 Ag1 121.3(4) . 1_446 ? C1 O3 Er1 135.2(4) . 2_677 ? C1 O4 Er1 135.6(4) . . ? C15 O6 Er1 100.9(3) . . ? C15 O7 Er1 166.8(4) . 2_677 ? C15 O7 Er1 87.8(3) . . ? Er1 O7 Er1 105.28(14) 2_677 . ? C22 O8 Er1 136.5(4) . 2_577 ? H2WA O2W H2WB 110.8 . . ? Er1 O1W H1WA 120.0 . . ? Er1 O1W H1WB 120.0 . . ? H1WA O1W H1WB 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C8 C6 C7 -21.9(9) . . . . ? O1 C8 C6 C7 160.3(5) . . . . ? O2 C8 C6 C5 154.2(6) . . . . ? O1 C8 C6 C5 -23.6(9) . . . . ? C5 C6 C7 C2 -6.7(9) . . . . ? C8 C6 C7 C2 169.5(5) . . . . ? C6 C7 C2 C3 2.3(9) . . . . ? C6 C7 C2 C1 -174.4(5) . . . . ? C7 C2 C3 C4 2.7(9) . . . . ? C1 C2 C3 C4 179.6(5) . . . . ? C2 C3 C4 C5 -3.3(9) . . . . ? C2 C3 C4 N2 -179.7(6) . . . . ? C3 C4 C5 C6 -1.1(9) . . . . ? N2 C4 C5 C6 175.4(6) . . . . ? C7 C6 C5 C4 6.1(9) . . . . ? C8 C6 C5 C4 -170.1(6) . . . . ? C3 C2 C1 O4 -37.7(8) . . . . ? C7 C2 C1 O4 139.1(6) . . . . ? C3 C2 C1 O3 143.8(6) . . . . ? C7 C2 C1 O3 -39.4(8) . . . . ? O5 C9 C10 C14 143.4(7) . . . . ? N2 C9 C10 C14 -37.5(9) . . . . ? O5 C9 C10 C11 -31.3(9) . . . . ? N2 C9 C10 C11 147.8(6) . . . . ? C14 C10 C11 C12 2.7(10) . . . . ? C9 C10 C11 C12 177.7(6) . . . . ? C10 C11 C12 N1 -3.5(10) . . . . ? C11 C10 C14 C13 -1.5(10) . . . . ? C9 C10 C14 C13 -176.2(7) . . . . ? N1 C13 C14 C10 0.9(12) . . . . ? O9 C22 C18 C17 157.2(6) . . . . ? O8 C22 C18 C17 -20.1(9) . . . . ? O9 C22 C18 C19 -24.0(9) . . . . ? O8 C22 C18 C19 158.7(6) . . . . ? C17 C18 C19 C20 0.7(9) . . . . ? C22 C18 C19 C20 -178.2(6) . . . . ? C18 C19 C20 C21 -0.5(9) . . . . ? C18 C19 C20 N4 179.1(5) . . . . ? C19 C20 C21 C16 0.2(9) . . . . ? N4 C20 C21 C16 -179.4(5) . . . . ? C20 C21 C16 C17 0.0(9) . . . . ? C20 C21 C16 C15 176.9(5) . . . . ? C21 C16 C17 C18 0.1(9) . . . . ? C15 C16 C17 C18 -176.8(5) . . . . ? C19 C18 C17 C16 -0.5(9) . . . . ? C22 C18 C17 C16 178.4(6) . . . . ? C17 C16 C15 O6 -45.0(8) . . . . ? C21 C16 C15 O6 138.0(6) . . . . ? C17 C16 C15 O7 134.2(6) . . . . ? C21 C16 C15 O7 -42.7(8) . . . . ? O10 C23 C24 C28 -141.6(7) . . . . ? N4 C23 C24 C28 41.1(9) . . . . ? O10 C23 C24 C25 32.8(10) . . . . ? N4 C23 C24 C25 -144.5(6) . . . . ? C28 C24 C25 C26 -0.5(10) . . . . ? C23 C24 C25 C26 -175.3(6) . . . . ? C24 C25 C26 N3 1.1(11) . . . . ? C25 C24 C28 C27 -0.5(10) . . . . ? C23 C24 C28 C27 173.9(6) . . . . ? N3 C27 C28 C24 1.1(10) . . . . ? C25 C26 N3 C27 -0.5(10) . . . . ? C25 C26 N3 Ag1 178.3(6) . . . . ? C28 C27 N3 C26 -0.6(10) . . . . ? C28 C27 N3 Ag1 -179.3(5) . . . . ? N1 Ag1 N3 C26 22.3(7) 1_663 . . . ? O2 Ag1 N3 C26 162.6(5) 1_664 . . . ? N1 Ag1 N3 C27 -159.0(5) 1_663 . . . ? O2 Ag1 N3 C27 -18.7(6) 1_664 . . . ? O10 C23 N4 C20 9.8(10) . . . . ? C24 C23 N4 C20 -173.0(5) . . . . ? C19 C20 N4 C23 -35.8(9) . . . . ? C21 C20 N4 C23 143.8(6) . . . . ? C14 C13 N1 C12 -1.4(12) . . . . ? C14 C13 N1 Ag1 -173.0(6) . . . 1_447 ? C11 C12 N1 C13 2.8(11) . . . . ? C11 C12 N1 Ag1 174.6(5) . . . 1_447 ? O5 C9 N2 C4 -2.3(11) . . . . ? C10 C9 N2 C4 178.6(6) . . . . ? C5 C4 N2 C9 154.9(6) . . . . ? C3 C4 N2 C9 -28.7(10) . . . . ? O2 C8 O1 Er1 32.9(9) . . . 1_545 ? C6 C8 O1 Er1 -149.4(4) . . . 1_545 ? O1 C8 O2 Ag1 47.6(8) . . . 1_446 ? C6 C8 O2 Ag1 -130.0(5) . . . 1_446 ? O4 C1 O3 Er1 33.2(10) . . . 2_677 ? C2 C1 O3 Er1 -148.5(4) . . . 2_677 ? O3 C1 O4 Er1 -27.9(10) . . . . ? C2 C1 O4 Er1 153.7(4) . . . . ? O1 Er1 O4 C1 -160.8(5) 1_565 . . . ? O8 Er1 O4 C1 167.7(6) 2_577 . . . ? O3 Er1 O4 C1 7.5(7) 2_677 . . . ? O1W Er1 O4 C1 -114.6(6) . . . . ? O7 Er1 O4 C1 -31.8(6) 2_677 . . . ? O6 Er1 O4 C1 96.7(6) . . . . ? O7 Er1 O4 C1 46.8(6) . . . . ? Er1 Er1 O4 C1 10.6(5) 2_677 . . . ? O7 C15 O6 Er1 0.1(6) . . . . ? C16 C15 O6 Er1 179.3(4) . . . . ? O1 Er1 O6 C15 139.4(3) 1_565 . . . ? O4 Er1 O6 C15 -70.1(4) . . . . ? O8 Er1 O6 C15 -143.8(4) 2_577 . . . ? O3 Er1 O6 C15 66.1(4) 2_677 . . . ? O1W Er1 O6 C15 -144.0(3) . . . . ? O7 Er1 O6 C15 -2.5(4) 2_677 . . . ? O7 Er1 O6 C15 0.0(3) . . . . ? Er1 Er1 O6 C15 -1.2(3) 2_677 . . . ? O6 C15 O7 Er1 171.5(13) . . . 2_677 ? C16 C15 O7 Er1 -7.7(19) . . . 2_677 ? O6 C15 O7 Er1 -0.1(5) . . . . ? C16 C15 O7 Er1 -179.3(5) . . . . ? O1 Er1 O7 C15 -59.3(4) 1_565 . . . ? O4 Er1 O7 C15 102.7(3) . . . . ? O8 Er1 O7 C15 37.9(3) 2_577 . . . ? O3 Er1 O7 C15 -104.9(3) 2_677 . . . ? O1W Er1 O7 C15 141.4(3) . . . . ? O7 Er1 O7 C15 178.0(4) 2_677 . . . ? O6 Er1 O7 C15 0.0(3) . . . . ? Er1 Er1 O7 C15 178.0(4) 2_677 . . . ? O1 Er1 O7 Er1 122.72(19) 1_565 . . 2_677 ? O4 Er1 O7 Er1 -75.32(16) . . . 2_677 ? O8 Er1 O7 Er1 -140.09(14) 2_577 . . 2_677 ? O3 Er1 O7 Er1 77.05(17) 2_677 . . 2_677 ? O1W Er1 O7 Er1 -36.6(3) . . . 2_677 ? O7 Er1 O7 Er1 0.000(1) 2_677 . . 2_677 ? O6 Er1 O7 Er1 -178.0(2) . . . 2_677 ? O9 C22 O8 Er1 -27.2(10) . . . 2_577 ? C18 C22 O8 Er1 150.0(4) . . . 2_577 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.744 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.171