# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Peng Cheng' _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; Structures and Luminescent Properties of a Series of Ln-Ag Heterometallic Coordination Polymers ; loop_ _publ_author_name 'Peng Cheng' 'Shi Wei' 'Xiao-Qing Zhao' 'Bin Zhao' #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 637079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag Eu N2 O14' _chemical_formula_sum 'C14 H18 Ag Eu N2 O14' _chemical_formula_weight 698.13 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.598(4) _cell_length_b 7.3645(18) _cell_length_c 19.757(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.849(4) _cell_angle_gamma 90.00 _cell_volume 2098.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4389 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 3.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4755 _exptl_absorpt_correction_T_max 0.6923 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10103 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3699 _reflns_number_gt 2990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+18.6782P] 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 3699 _refine_ls_number_parameters 289 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.890 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.79578(5) 0.04105(11) 0.13846(4) 0.0192(3) Uani 1 1 d U . . Ag1 Ag 0.87902(16) 0.5033(3) 0.00702(16) 0.0874(8) Uani 1 1 d U . . O1 O 0.7938(8) 0.2545(16) 0.0438(6) 0.032(3) Uani 1 1 d . . . O2 O 0.7369(10) 0.3740(19) -0.0562(7) 0.045(3) Uani 1 1 d . . . O3 O 0.6976(8) -0.2267(16) 0.1385(6) 0.029(3) Uani 1 1 d . . . O4 O 0.5963(9) -0.4304(17) 0.0870(7) 0.039(3) Uani 1 1 d . . . O5 O 0.8685(8) -0.1714(16) 0.0688(6) 0.032(3) Uani 1 1 d . . . O6 O 0.9939(10) -0.3023(19) 0.0384(8) 0.050(4) Uani 1 1 d . . . O7 O 0.8670(8) 0.3167(16) 0.1941(6) 0.028(3) Uani 1 1 d . . . O8 O 0.9821(9) 0.5191(18) 0.2148(8) 0.045(4) Uani 1 1 d . . . O9 O 0.8950(8) -0.1577(16) 0.2201(6) 0.031(3) Uani 1 1 d . . . H9A H 0.9553 -0.1002 0.2368 0.037 Uiso 1 1 d R . . H9B H 0.9225 -0.2310 0.2083 0.037 Uiso 1 1 d R . . O10 O 0.7473(8) 0.0480(16) 0.2507(6) 0.028(3) Uani 1 1 d . . . H10A H 0.7648 0.0971 0.2783 0.034 Uiso 1 1 d R . . H10B H 0.7100 -0.0459 0.2619 0.034 Uiso 1 1 d R . . O11 O 0.6621(8) 0.2424(16) 0.1437(6) 0.032(3) Uani 1 1 d . . . H11A H 0.6612 0.2708 0.1881 0.039 Uiso 1 1 d R . . H11B H 0.6525 0.3245 0.1282 0.039 Uiso 1 1 d R . . N1 N 0.6784(10) -0.0178(18) 0.0299(7) 0.024(3) Uani 1 1 d . . . N2 N 0.9643(9) 0.1016(19) 0.1267(7) 0.025(3) Uani 1 1 d . . . C1 C 0.7371(12) 0.254(2) -0.0118(8) 0.026(4) Uani 1 1 d . . . C2 C 0.6712(11) 0.096(2) -0.0233(8) 0.025(3) Uani 1 1 d . . . C3 C 0.6107(13) 0.066(3) -0.0835(10) 0.037(4) Uani 1 1 d . . . H3 H 0.6066 0.1470 -0.1198 0.044 Uiso 1 1 calc R . . C4 C 0.5569(14) -0.089(3) -0.0879(10) 0.045(5) Uani 1 1 d . . . H4 H 0.5158 -0.1132 -0.1277 0.054 Uiso 1 1 calc R . . C5 C 0.5639(13) -0.208(3) -0.0332(9) 0.035(4) Uani 1 1 d . . . H5 H 0.5275 -0.3123 -0.0354 0.042 Uiso 1 1 calc R . . C6 C 0.6265(11) -0.169(2) 0.0246(8) 0.025(4) Uani 1 1 d . . . C7 C 0.6402(12) -0.287(2) 0.0889(8) 0.028(4) Uani 1 1 d . . . C8 C 0.9548(12) -0.175(2) 0.0652(9) 0.027(4) Uani 1 1 d . . . C9 C 1.0117(12) -0.017(2) 0.0952(9) 0.030(4) Uani 1 1 d . . . C10 C 1.1037(13) 0.003(3) 0.0904(11) 0.043(5) Uani 1 1 d . . . H10 H 1.1355 -0.0835 0.0689 0.051 Uiso 1 1 calc R . . C11 C 1.1475(14) 0.158(3) 0.1186(12) 0.051(6) Uani 1 1 d . . . H11 H 1.2101 0.1760 0.1165 0.061 Uiso 1 1 calc R . . C12 C 1.0989(13) 0.284(3) 0.1497(11) 0.043(5) Uani 1 1 d . . . H12 H 1.1277 0.3906 0.1674 0.052 Uiso 1 1 calc R . . C13 C 1.0076(11) 0.253(2) 0.1544(9) 0.026(4) Uani 1 1 d . . . C14 C 0.9486(11) 0.372(2) 0.1908(9) 0.028(4) Uani 1 1 d . . . O12 O 0.3036(10) 0.532(2) 0.1909(8) 0.059(4) Uani 1 1 d . . . H12A H 0.2907 0.5689 0.1526 0.071 Uiso 1 1 d R . . H12B H 0.2646 0.5903 0.2104 0.071 Uiso 1 1 d R . . O13 O 0.1635(11) 0.674(3) 0.2554(11) 0.085(6) Uani 1 1 d . . . H13A H 0.1709 0.7880 0.2536 0.102 Uiso 1 1 d R . . H13B H 0.1086 0.6337 0.2447 0.102 Uiso 1 1 d R . . O14 O 0.0082(11) 0.050(3) 0.3030(9) 0.073(6) Uani 1 1 d . . . H14A H -0.0021 0.0426 0.3442 0.088 Uiso 1 1 d R . . H14B H 0.0644 0.0617 0.2974 0.088 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 Eu1 0.0217(5) 0.0152(5) 0.0215(5) -0.0012(3) 0.0061(3) -0.0019(3) Ag1 0.0642(11) 0.0572(11) 0.1455(16) -0.0455(11) 0.0307(11) -0.0287(9) O1 0.033(7) 0.026(6) 0.038(7) 0.006(5) 0.005(6) -0.012(5) O2 0.058(9) 0.033(8) 0.043(8) 0.014(6) 0.008(7) -0.012(7) O3 0.037(7) 0.024(6) 0.027(6) 0.004(5) 0.003(5) -0.011(5) O4 0.048(8) 0.023(7) 0.044(7) 0.011(6) 0.001(6) -0.017(6) O5 0.037(7) 0.020(6) 0.041(7) -0.013(5) 0.011(6) -0.006(5) O6 0.046(8) 0.030(7) 0.082(11) -0.030(8) 0.030(8) -0.008(6) O7 0.025(6) 0.022(6) 0.039(7) -0.012(5) 0.011(5) -0.005(5) O8 0.031(7) 0.030(7) 0.073(10) -0.025(7) 0.010(7) -0.005(6) O9 0.031(6) 0.023(6) 0.037(7) 0.000(5) 0.002(5) 0.008(5) O10 0.037(6) 0.025(6) 0.025(6) -0.004(5) 0.010(5) -0.007(5) O11 0.041(7) 0.022(6) 0.035(7) 0.000(5) 0.011(6) 0.005(5) N1 0.032(8) 0.017(7) 0.024(7) 0.004(6) 0.008(6) -0.004(6) N2 0.024(7) 0.020(7) 0.031(7) -0.007(6) 0.012(6) -0.001(6) C1 0.032(9) 0.022(9) 0.026(9) 0.000(7) 0.008(7) -0.004(7) C2 0.026(8) 0.022(8) 0.028(8) 0.004(7) 0.010(7) 0.003(7) C3 0.043(11) 0.030(10) 0.036(10) 0.009(8) 0.001(8) -0.005(8) C4 0.044(12) 0.055(13) 0.032(10) 0.007(9) -0.010(9) -0.015(10) C5 0.036(10) 0.034(10) 0.034(10) 0.008(8) -0.002(8) -0.015(8) C6 0.026(9) 0.021(8) 0.029(8) 0.000(7) 0.005(7) -0.007(7) C7 0.031(9) 0.024(9) 0.028(9) 0.008(7) 0.006(7) -0.004(7) C8 0.032(10) 0.021(9) 0.031(9) -0.008(7) 0.011(7) -0.002(7) C9 0.033(10) 0.027(9) 0.033(9) -0.008(8) 0.013(8) 0.000(7) C10 0.029(10) 0.044(12) 0.057(12) -0.023(10) 0.012(9) 0.003(9) C11 0.027(10) 0.050(13) 0.082(16) -0.026(12) 0.025(10) -0.010(9) C12 0.030(10) 0.041(12) 0.062(13) -0.021(10) 0.016(9) -0.013(9) C13 0.026(9) 0.020(8) 0.035(9) -0.004(7) 0.011(7) -0.002(7) C14 0.026(9) 0.017(8) 0.042(10) -0.013(8) 0.006(7) 0.001(7) O12 0.039(8) 0.075(12) 0.063(10) 0.015(9) 0.006(7) 0.002(8) O13 0.045(10) 0.086(14) 0.126(17) -0.043(13) 0.019(10) -0.009(9) O14 0.042(9) 0.108(16) 0.073(12) -0.032(11) 0.020(8) -0.016(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O10 2.429(12) . ? Eu1 O5 2.432(12) . ? Eu1 O3 2.438(11) . ? Eu1 O1 2.439(12) . ? Eu1 O7 2.461(11) . ? Eu1 O11 2.466(11) . ? Eu1 O9 2.475(11) . ? Eu1 N2 2.545(13) . ? Eu1 N1 2.567(13) . ? Ag1 O6 2.219(13) 1_565 ? Ag1 O1 2.390(12) . ? Ag1 O2 2.444(14) . ? O1 C1 1.27(2) . ? O2 C1 1.24(2) . ? O3 C7 1.27(2) . ? O4 C7 1.24(2) . ? O5 C8 1.27(2) . ? O6 C8 1.25(2) . ? O6 Ag1 2.219(13) 1_545 ? O7 C14 1.27(2) . ? O8 C14 1.25(2) . ? O9 H9A 0.9865 . ? O9 H9B 0.7327 . ? O10 H10A 0.6721 . ? O10 H10B 0.9284 . ? O11 H11A 0.9034 . ? O11 H11B 0.6826 . ? N1 C2 1.34(2) . ? N1 C6 1.34(2) . ? N2 C9 1.33(2) . ? N2 C13 1.35(2) . ? C1 C2 1.50(2) . ? C2 C3 1.39(2) . ? C3 C4 1.38(3) . ? C3 H3 0.9300 . ? C4 C5 1.38(3) . ? C4 H4 0.9300 . ? C5 C6 1.38(2) . ? C5 H5 0.9300 . ? C6 C7 1.53(2) . ? C8 C9 1.50(2) . ? C9 C10 1.37(3) . ? C10 C11 1.38(3) . ? C10 H10 0.9300 . ? C11 C12 1.37(3) . ? C11 H11 0.9300 . ? C12 C13 1.37(2) . ? C12 H12 0.9300 . ? C13 C14 1.49(2) . ? O12 H12A 0.7997 . ? O12 H12B 0.8499 . ? O13 H13A 0.8492 . ? O13 H13B 0.8501 . ? O14 H14A 0.8515 . ? O14 H14B 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 O10 Eu1 O5 138.0(4) . . ? O10 Eu1 O3 76.3(4) . . ? O5 Eu1 O3 77.8(4) . . ? O10 Eu1 O1 135.6(4) . . ? O5 Eu1 O1 86.3(4) . . ? O3 Eu1 O1 125.7(4) . . ? O10 Eu1 O7 74.8(4) . . ? O5 Eu1 O7 126.3(4) . . ? O3 Eu1 O7 151.0(4) . . ? O1 Eu1 O7 76.4(4) . . ? O10 Eu1 O11 66.8(4) . . ? O5 Eu1 O11 145.9(4) . . ? O3 Eu1 O11 91.0(4) . . ? O1 Eu1 O11 74.2(4) . . ? O7 Eu1 O11 76.6(4) . . ? O10 Eu1 O9 69.0(4) . . ? O5 Eu1 O9 74.1(4) . . ? O3 Eu1 O9 78.8(4) . . ? O1 Eu1 O9 144.8(4) . . ? O7 Eu1 O9 91.8(4) . . ? O11 Eu1 O9 135.7(4) . . ? O10 Eu1 N2 120.1(4) . . ? O5 Eu1 N2 63.2(4) . . ? O3 Eu1 N2 135.9(4) . . ? O1 Eu1 N2 73.4(4) . . ? O7 Eu1 N2 63.1(4) . . ? O11 Eu1 N2 132.9(4) . . ? O9 Eu1 N2 71.7(4) . . ? O10 Eu1 N1 121.0(4) . . ? O5 Eu1 N1 73.3(4) . . ? O3 Eu1 N1 63.1(4) . . ? O1 Eu1 N1 62.7(4) . . ? O7 Eu1 N1 133.9(4) . . ? O11 Eu1 N1 72.9(4) . . ? O9 Eu1 N1 133.9(4) . . ? N2 Eu1 N1 118.9(4) . . ? O6 Ag1 O1 144.7(5) 1_565 . ? O6 Ag1 O2 160.0(6) 1_565 . ? O1 Ag1 O2 54.3(4) . . ? C1 O1 Ag1 92.2(10) . . ? C1 O1 Eu1 126.2(10) . . ? Ag1 O1 Eu1 141.4(5) . . ? C1 O2 Ag1 90.4(10) . . ? C7 O3 Eu1 126.9(10) . . ? C8 O5 Eu1 124.6(10) . . ? C8 O6 Ag1 103.1(11) . 1_545 ? C14 O7 Eu1 125.4(10) . . ? Eu1 O9 H9A 111.5 . . ? Eu1 O9 H9B 121.5 . . ? H9A O9 H9B 85.3 . . ? Eu1 O10 H10A 128.8 . . ? Eu1 O10 H10B 117.8 . . ? H10A O10 H10B 111.7 . . ? Eu1 O11 H11A 108.1 . . ? Eu1 O11 H11B 128.6 . . ? H11A O11 H11B 101.4 . . ? C2 N1 C6 119.0(14) . . ? C2 N1 Eu1 120.8(11) . . ? C6 N1 Eu1 120.1(10) . . ? C9 N2 C13 119.2(14) . . ? C9 N2 Eu1 120.5(11) . . ? C13 N2 Eu1 120.3(10) . . ? O2 C1 O1 122.6(15) . . ? O2 C1 C2 120.7(15) . . ? O1 C1 C2 116.7(14) . . ? N1 C2 C3 122.4(16) . . ? N1 C2 C1 113.3(14) . . ? C3 C2 C1 124.3(15) . . ? C4 C3 C2 118.1(17) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 120.1(17) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 118.2(16) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? N1 C6 C5 122.3(15) . . ? N1 C6 C7 114.0(14) . . ? C5 C6 C7 123.7(15) . . ? O4 C7 O3 126.9(15) . . ? O4 C7 C6 117.5(15) . . ? O3 C7 C6 115.6(14) . . ? O6 C8 O5 123.9(16) . . ? O6 C8 C9 119.1(16) . . ? O5 C8 C9 117.0(14) . . ? N2 C9 C10 123.1(17) . . ? N2 C9 C8 113.6(15) . . ? C10 C9 C8 123.3(16) . . ? C9 C10 C11 117.5(18) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C12 C11 C10 120.1(18) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 119.2(18) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N2 C13 C12 120.8(16) . . ? N2 C13 C14 114.4(14) . . ? C12 C13 C14 124.8(16) . . ? O8 C14 O7 125.2(15) . . ? O8 C14 C13 118.2(15) . . ? O7 C14 C13 116.6(14) . . ? H12A O12 H12B 100.6 . . ? H13A O13 H13B 117.1 . . ? H14A O14 H14B 116.7 . . ? 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 O6 Ag1 O1 C1 174.5(10) 1_565 . . . ? O2 Ag1 O1 C1 3.9(10) . . . . ? O6 Ag1 O1 Eu1 -9.5(15) 1_565 . . . ? O2 Ag1 O1 Eu1 179.9(12) . . . . ? O10 Eu1 O1 C1 -102.7(14) . . . . ? O5 Eu1 O1 C1 77.8(14) . . . . ? O3 Eu1 O1 C1 5.8(16) . . . . ? O7 Eu1 O1 C1 -153.4(14) . . . . ? O11 Eu1 O1 C1 -73.8(14) . . . . ? O9 Eu1 O1 C1 133.2(13) . . . . ? N2 Eu1 O1 C1 141.0(14) . . . . ? N1 Eu1 O1 C1 4.8(13) . . . . ? O10 Eu1 O1 Ag1 82.2(10) . . . . ? O5 Eu1 O1 Ag1 -97.2(9) . . . . ? O3 Eu1 O1 Ag1 -169.3(8) . . . . ? O7 Eu1 O1 Ag1 31.5(9) . . . . ? O11 Eu1 O1 Ag1 111.2(10) . . . . ? O9 Eu1 O1 Ag1 -41.8(13) . . . . ? N2 Eu1 O1 Ag1 -34.1(9) . . . . ? N1 Eu1 O1 Ag1 -170.3(11) . . . . ? O6 Ag1 O2 C1 -168.0(14) 1_565 . . . ? O1 Ag1 O2 C1 -4.0(10) . . . . ? O10 Eu1 O3 C7 141.2(14) . . . . ? O5 Eu1 O3 C7 -72.0(14) . . . . ? O1 Eu1 O3 C7 4.3(16) . . . . ? O7 Eu1 O3 C7 138.9(13) . . . . ? O11 Eu1 O3 C7 75.5(14) . . . . ? O9 Eu1 O3 C7 -147.9(14) . . . . ? N2 Eu1 O3 C7 -99.5(14) . . . . ? N1 Eu1 O3 C7 5.3(13) . . . . ? O10 Eu1 O5 C8 -96.2(14) . . . . ? O3 Eu1 O5 C8 -149.0(14) . . . . ? O1 Eu1 O5 C8 83.2(14) . . . . ? O7 Eu1 O5 C8 13.0(15) . . . . ? O11 Eu1 O5 C8 137.8(13) . . . . ? O9 Eu1 O5 C8 -67.3(13) . . . . ? N2 Eu1 O5 C8 9.9(13) . . . . ? N1 Eu1 O5 C8 145.7(14) . . . . ? O10 Eu1 O7 C14 139.5(14) . . . . ? O5 Eu1 O7 C14 0.4(15) . . . . ? O3 Eu1 O7 C14 141.9(13) . . . . ? O1 Eu1 O7 C14 -74.6(14) . . . . ? O11 Eu1 O7 C14 -151.3(14) . . . . ? O9 Eu1 O7 C14 71.9(14) . . . . ? N2 Eu1 O7 C14 3.5(13) . . . . ? N1 Eu1 O7 C14 -101.8(14) . . . . ? O10 Eu1 N1 C2 126.8(12) . . . . ? O5 Eu1 N1 C2 -96.7(13) . . . . ? O3 Eu1 N1 C2 178.8(14) . . . . ? O1 Eu1 N1 C2 -2.1(12) . . . . ? O7 Eu1 N1 C2 28.0(15) . . . . ? O11 Eu1 N1 C2 78.7(12) . . . . ? O9 Eu1 N1 C2 -143.3(11) . . . . ? N2 Eu1 N1 C2 -51.4(13) . . . . ? O10 Eu1 N1 C6 -56.4(13) . . . . ? O5 Eu1 N1 C6 80.1(12) . . . . ? O3 Eu1 N1 C6 -4.4(12) . . . . ? O1 Eu1 N1 C6 174.7(14) . . . . ? O7 Eu1 N1 C6 -155.3(11) . . . . ? O11 Eu1 N1 C6 -104.6(13) . . . . ? O9 Eu1 N1 C6 33.4(15) . . . . ? N2 Eu1 N1 C6 125.4(12) . . . . ? O10 Eu1 N2 C9 125.5(12) . . . . ? O5 Eu1 N2 C9 -6.6(12) . . . . ? O3 Eu1 N2 C9 23.8(15) . . . . ? O1 Eu1 N2 C9 -100.9(13) . . . . ? O7 Eu1 N2 C9 176.2(14) . . . . ? O11 Eu1 N2 C9 -149.4(12) . . . . ? O9 Eu1 N2 C9 74.4(13) . . . . ? N1 Eu1 N2 C9 -56.3(14) . . . . ? O10 Eu1 N2 C13 -52.4(14) . . . . ? O5 Eu1 N2 C13 175.5(14) . . . . ? O3 Eu1 N2 C13 -154.1(11) . . . . ? O1 Eu1 N2 C13 81.2(12) . . . . ? O7 Eu1 N2 C13 -1.6(12) . . . . ? O11 Eu1 N2 C13 32.7(15) . . . . ? O9 Eu1 N2 C13 -103.5(13) . . . . ? N1 Eu1 N2 C13 125.9(12) . . . . ? Ag1 O2 C1 O1 7.2(18) . . . . ? Ag1 O2 C1 C2 -170.4(14) . . . . ? Ag1 O1 C1 O2 -7.4(18) . . . . ? Eu1 O1 C1 O2 175.7(13) . . . . ? Ag1 O1 C1 C2 170.3(13) . . . . ? Eu1 O1 C1 C2 -7(2) . . . . ? C6 N1 C2 C3 1(3) . . . . ? Eu1 N1 C2 C3 177.9(13) . . . . ? C6 N1 C2 C1 -176.7(15) . . . . ? Eu1 N1 C2 C1 0.1(19) . . . . ? O2 C1 C2 N1 -178.4(16) . . . . ? O1 C1 C2 N1 4(2) . . . . ? O2 C1 C2 C3 4(3) . . . . ? O1 C1 C2 C3 -173.9(17) . . . . ? N1 C2 C3 C4 0(3) . . . . ? C1 C2 C3 C4 177.3(18) . . . . ? C2 C3 C4 C5 0(3) . . . . ? C3 C4 C5 C6 -1(3) . . . . ? C2 N1 C6 C5 -2(3) . . . . ? Eu1 N1 C6 C5 -178.6(14) . . . . ? C2 N1 C6 C7 -179.4(15) . . . . ? Eu1 N1 C6 C7 3.8(19) . . . . ? C4 C5 C6 N1 2(3) . . . . ? C4 C5 C6 C7 179.0(19) . . . . ? Eu1 O3 C7 O4 173.3(14) . . . . ? Eu1 O3 C7 C6 -5(2) . . . . ? N1 C6 C7 O4 -178.2(16) . . . . ? C5 C6 C7 O4 4(3) . . . . ? N1 C6 C7 O3 1(2) . . . . ? C5 C6 C7 O3 -176.9(17) . . . . ? Ag1 O6 C8 O5 -2(2) 1_545 . . . ? Ag1 O6 C8 C9 178.1(13) 1_545 . . . ? Eu1 O5 C8 O6 167.9(14) . . . . ? Eu1 O5 C8 C9 -12(2) . . . . ? C13 N2 C9 C10 1(3) . . . . ? Eu1 N2 C9 C10 -176.6(15) . . . . ? C13 N2 C9 C8 -178.3(15) . . . . ? Eu1 N2 C9 C8 4(2) . . . . ? O6 C8 C9 N2 -175.2(17) . . . . ? O5 C8 C9 N2 5(2) . . . . ? O6 C8 C9 C10 5(3) . . . . ? O5 C8 C9 C10 -174.9(19) . . . . ? N2 C9 C10 C11 -1(3) . . . . ? C8 C9 C10 C11 178(2) . . . . ? C9 C10 C11 C12 0(4) . . . . ? C10 C11 C12 C13 2(4) . . . . ? C9 N2 C13 C12 1(3) . . . . ? Eu1 N2 C13 C12 178.5(15) . . . . ? C9 N2 C13 C14 -177.7(16) . . . . ? Eu1 N2 C13 C14 0.2(19) . . . . ? C11 C12 C13 N2 -2(3) . . . . ? C11 C12 C13 C14 176(2) . . . . ? Eu1 O7 C14 O8 174.4(14) . . . . ? Eu1 O7 C14 C13 -5(2) . . . . ? N2 C13 C14 O8 -176.5(17) . . . . ? C12 C13 C14 O8 5(3) . . . . ? N2 C13 C14 O7 3(2) . . . . ? C12 C13 C14 O7 -175.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.885 _refine_diff_density_min -2.818 _refine_diff_density_rms 0.228 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 640098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H31 Ag2 Ce N7 O13' _chemical_formula_weight 1185.59 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.244(3) _cell_length_b 10.7134(13) _cell_length_c 18.651(2) _cell_angle_alpha 90.00 _cell_angle_beta 122.111(2) _cell_angle_gamma 90.00 _cell_volume 4272.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.03 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 2.029 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.749886 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11766 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4358 _reflns_number_gt 3424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+10.4225P] 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 4358 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ce1 Ce 0.5000 0.10346(3) 0.7500 0.03114(9) Uani 1 2 d S . . Ag1 Ag 0.199118(17) 0.20120(4) 0.38235(2) 0.06458(13) Uani 1 1 d . . . N2 N 0.5000 0.3397(4) 0.7500 0.0332(9) Uani 1 2 d S . . N1 N 0.45861(13) -0.0035(3) 0.60928(18) 0.0361(7) Uani 1 1 d . . . C1 C 0.40520(17) 0.0352(4) 0.5410(2) 0.0401(9) Uani 1 1 d . . . O3 O 0.56082(11) -0.0595(2) 0.74801(17) 0.0443(6) Uani 1 1 d . . . O5 O 0.54371(12) 0.2012(2) 0.68103(17) 0.0441(7) Uani 1 1 d . . . N4 N 0.23342(15) 0.3456(3) 0.3353(2) 0.0493(8) Uani 1 1 d . . . O1 O 0.40063(11) 0.1694(2) 0.63727(16) 0.0422(6) Uani 1 1 d . . . C7 C 0.55265(18) -0.1221(3) 0.6840(3) 0.0432(9) Uani 1 1 d . . . C8 C 0.52488(16) 0.4020(4) 0.7134(2) 0.0381(8) Uani 1 1 d . . . O6 O 0.57623(16) 0.3637(3) 0.6396(2) 0.0724(10) Uani 1 1 d . . . C11 C 0.55117(18) 0.3191(4) 0.6743(3) 0.0437(10) Uani 1 1 d . . . C5 C 0.49309(17) -0.0907(3) 0.6015(2) 0.0401(9) Uani 1 1 d . . . N3 N 0.17468(17) 0.0188(4) 0.4072(2) 0.0588(10) Uani 1 1 d . . . O2 O 0.32036(14) 0.1707(3) 0.50438(19) 0.0698(9) Uani 1 1 d . . . O4 O 0.58829(14) -0.2001(3) 0.6847(2) 0.0636(9) Uani 1 1 d . . . C3 C 0.4196(2) -0.1037(5) 0.4537(3) 0.0639(13) Uani 1 1 d . . . H3 H 0.4066 -0.1372 0.4008 0.077 Uiso 1 1 calc R . . C6 C 0.37163(18) 0.1322(4) 0.5601(3) 0.0437(9) Uani 1 1 d . . . C17 C 0.28968(19) 0.3383(4) 0.3451(3) 0.0523(11) Uani 1 1 d . . . H17 H 0.3124 0.2648 0.3669 0.063 Uiso 1 1 calc R . . C4 C 0.4741(2) -0.1439(4) 0.5242(3) 0.0554(12) Uani 1 1 d . . . H4 H 0.4980 -0.2062 0.5198 0.066 Uiso 1 1 calc R . . C12 C 0.1477(2) 0.0081(5) 0.4511(3) 0.0683(13) Uani 1 1 d . . . H12 H 0.1376 0.0802 0.4690 0.082 Uiso 1 1 calc R . . C2 C 0.3843(2) -0.0138(4) 0.4618(3) 0.0569(11) Uani 1 1 d . . . H2 H 0.3470 0.0136 0.4147 0.068 Uiso 1 1 calc R . . C18 C 0.3158(2) 0.4327(5) 0.3248(3) 0.0644(13) Uani 1 1 d . . . H18 H 0.3551 0.4236 0.3324 0.077 Uiso 1 1 calc R . . C21 C 0.2016(2) 0.4510(5) 0.3029(3) 0.0605(12) Uani 1 1 d . . . H21 H 0.1621 0.4578 0.2948 0.073 Uiso 1 1 calc R . . C20 C 0.2242(2) 0.5500(4) 0.2808(3) 0.0648(13) Uani 1 1 d . . . H20 H 0.2004 0.6220 0.2581 0.078 Uiso 1 1 calc R . . C19 C 0.2825(2) 0.5415(5) 0.2927(3) 0.0665(13) Uani 1 1 d . . . H19 H 0.2993 0.6082 0.2794 0.080 Uiso 1 1 calc R . . C10 C 0.5000 0.5957(6) 0.7500 0.0574(16) Uani 1 2 d S . . H10 H 0.5000 0.6825 0.7500 0.069 Uiso 1 2 calc SR . . C9 C 0.52578(19) 0.5315(4) 0.7119(3) 0.0501(10) Uani 1 1 d . . . H9 H 0.5433 0.5736 0.6858 0.060 Uiso 1 1 calc R . . C16 C 0.1872(3) -0.0855(6) 0.3813(4) 0.0881(18) Uani 1 1 d . . . H16 H 0.2062 -0.0797 0.3503 0.106 Uiso 1 1 calc R . . C15 C 0.1738(4) -0.2015(6) 0.3978(5) 0.106(2) Uani 1 1 d . . . H15 H 0.1827 -0.2726 0.3775 0.127 Uiso 1 1 calc R . . C14 C 0.1473(3) -0.2108(6) 0.4440(4) 0.097(2) Uani 1 1 d . . . H14 H 0.1382 -0.2887 0.4568 0.116 Uiso 1 1 calc R . . C13 C 0.1341(3) -0.1055(6) 0.4714(4) 0.0928(19) Uani 1 1 d . . . H13 H 0.1160 -0.1100 0.5037 0.111 Uiso 1 1 calc R . . O7 O 0.4699(6) 0.4457(13) 0.4906(8) 0.180(5) Uani 0.50 1 d P . . 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 Ce1 0.03126(16) 0.02695(15) 0.03504(16) 0.000 0.01751(13) 0.000 Ag1 0.0601(2) 0.0585(2) 0.0759(3) 0.01533(19) 0.0367(2) -0.00565(17) N2 0.029(2) 0.033(2) 0.038(2) 0.000 0.018(2) 0.000 N1 0.0386(17) 0.0324(17) 0.0391(17) 0.0007(14) 0.0220(15) -0.0061(14) C1 0.041(2) 0.036(2) 0.042(2) 0.0017(17) 0.0211(19) -0.0090(17) O3 0.0412(15) 0.0399(15) 0.0502(16) -0.0025(12) 0.0232(13) 0.0058(12) O5 0.0542(17) 0.0352(16) 0.0579(17) -0.0039(12) 0.0399(15) -0.0058(12) N4 0.0412(19) 0.053(2) 0.054(2) 0.0091(17) 0.0251(17) 0.0009(16) O1 0.0357(14) 0.0406(15) 0.0425(16) 0.0012(12) 0.0155(13) 0.0059(11) C7 0.047(2) 0.027(2) 0.066(3) -0.0027(18) 0.038(2) -0.0027(17) C8 0.0335(19) 0.034(2) 0.043(2) -0.0023(17) 0.0181(17) -0.0041(17) O6 0.102(3) 0.050(2) 0.112(3) -0.0027(18) 0.088(2) -0.0140(17) C11 0.042(2) 0.042(2) 0.051(2) -0.0053(19) 0.028(2) -0.0084(18) C5 0.047(2) 0.030(2) 0.053(2) -0.0063(18) 0.033(2) -0.0111(17) N3 0.063(2) 0.052(2) 0.063(2) 0.0058(19) 0.035(2) -0.0038(19) O2 0.0483(19) 0.082(2) 0.0497(19) 0.0056(17) 0.0065(16) 0.0114(17) O4 0.063(2) 0.0469(19) 0.088(2) -0.0109(16) 0.0450(19) 0.0114(15) C3 0.088(4) 0.064(3) 0.048(3) -0.018(2) 0.043(3) -0.022(3) C6 0.038(2) 0.043(2) 0.043(2) 0.0083(18) 0.017(2) -0.0025(17) C17 0.051(3) 0.051(3) 0.057(3) 0.004(2) 0.029(2) 0.010(2) C4 0.074(3) 0.046(3) 0.065(3) -0.017(2) 0.050(3) -0.012(2) C12 0.087(4) 0.056(3) 0.073(3) -0.012(3) 0.050(3) -0.017(3) C2 0.068(3) 0.057(3) 0.039(2) -0.002(2) 0.024(2) -0.011(2) C18 0.050(3) 0.075(4) 0.080(3) 0.010(3) 0.042(3) -0.001(2) C21 0.041(2) 0.072(3) 0.071(3) 0.020(3) 0.032(2) 0.011(2) C20 0.068(3) 0.052(3) 0.080(3) 0.022(3) 0.043(3) 0.014(2) C19 0.070(3) 0.063(3) 0.079(3) 0.011(3) 0.049(3) -0.009(3) C10 0.072(4) 0.029(3) 0.073(4) 0.000 0.039(4) 0.000 C9 0.059(3) 0.034(2) 0.060(3) 0.0015(19) 0.033(2) -0.0059(19) C16 0.128(5) 0.064(4) 0.113(5) 0.022(3) 0.092(4) 0.021(3) C15 0.161(7) 0.057(4) 0.130(6) 0.003(4) 0.098(6) 0.012(4) C14 0.130(6) 0.054(4) 0.114(5) 0.009(4) 0.070(5) -0.019(4) C13 0.118(5) 0.080(4) 0.105(5) -0.002(4) 0.077(4) -0.033(4) O7 0.191(14) 0.195(15) 0.144(10) 0.033(10) 0.083(11) 0.015(10) _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 Ce1 O3 2.338(2) . ? Ce1 O3 2.338(3) 2_656 ? Ce1 O5 2.341(2) . ? Ce1 O5 2.341(2) 2_656 ? Ce1 O1 2.368(2) 2_656 ? Ce1 O1 2.368(2) . ? Ce1 N1 2.526(3) . ? Ce1 N1 2.526(3) 2_656 ? Ce1 N2 2.531(4) . ? Ag1 N3 2.172(4) . ? Ag1 N4 2.173(3) . ? N2 C8 1.327(4) . ? N2 C8 1.327(4) 2_656 ? N1 C5 1.336(5) . ? N1 C1 1.337(5) . ? C1 C2 1.381(6) . ? C1 C6 1.499(6) . ? O3 C7 1.287(5) . ? O5 C11 1.293(5) . ? N4 C21 1.330(5) . ? N4 C17 1.335(5) . ? O1 C6 1.283(5) . ? C7 O4 1.223(4) . ? C7 C5 1.510(6) . ? C8 C9 1.387(5) . ? C8 C11 1.509(5) . ? O6 C11 1.217(5) . ? C5 C4 1.379(5) . ? N3 C12 1.319(6) . ? N3 C16 1.321(7) . ? O2 C6 1.223(5) . ? C3 C4 1.372(6) . ? C3 C2 1.374(6) . ? C3 H3 0.9300 . ? C17 C18 1.366(6) . ? C17 H17 0.9300 . ? C4 H4 0.9300 . ? C12 C13 1.372(7) . ? C12 H12 0.9300 . ? C2 H2 0.9300 . ? C18 C19 1.374(6) . ? C18 H18 0.9300 . ? C21 C20 1.367(6) . ? C21 H21 0.9300 . ? C20 C19 1.368(6) . ? C20 H20 0.9300 . ? C19 H19 0.9300 . ? C10 C9 1.377(5) . ? C10 C9 1.377(5) 2_656 ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? C16 C15 1.366(8) . ? C16 H16 0.9300 . ? C15 C14 1.346(8) . ? C15 H15 0.9300 . ? C14 C13 1.352(8) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? O7 O7 1.79(2) 5_666 ? 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 O3 Ce1 O3 83.42(13) . 2_656 ? O3 Ce1 O5 79.63(9) . . ? O3 Ce1 O5 148.03(9) 2_656 . ? O3 Ce1 O5 148.03(9) . 2_656 ? O3 Ce1 O5 79.62(9) 2_656 2_656 ? O5 Ce1 O5 126.82(13) . 2_656 ? O3 Ce1 O1 80.92(9) . 2_656 ? O3 Ce1 O1 127.11(9) 2_656 2_656 ? O5 Ce1 O1 76.59(9) . 2_656 ? O5 Ce1 O1 87.98(9) 2_656 2_656 ? O3 Ce1 O1 127.11(9) . . ? O3 Ce1 O1 80.92(9) 2_656 . ? O5 Ce1 O1 87.98(9) . . ? O5 Ce1 O1 76.59(9) 2_656 . ? O1 Ce1 O1 145.28(13) 2_656 . ? O3 Ce1 N1 63.71(9) . . ? O3 Ce1 N1 76.43(9) 2_656 . ? O5 Ce1 N1 71.79(9) . . ? O5 Ce1 N1 135.96(9) 2_656 . ? O1 Ce1 N1 135.73(9) 2_656 . ? O1 Ce1 N1 63.57(9) . . ? O3 Ce1 N1 76.43(9) . 2_656 ? O3 Ce1 N1 63.70(9) 2_656 2_656 ? O5 Ce1 N1 135.96(9) . 2_656 ? O5 Ce1 N1 71.78(9) 2_656 2_656 ? O1 Ce1 N1 63.57(9) 2_656 2_656 ? O1 Ce1 N1 135.73(9) . 2_656 ? N1 Ce1 N1 126.02(14) . 2_656 ? O3 Ce1 N2 138.29(6) . . ? O3 Ce1 N2 138.29(6) 2_656 . ? O5 Ce1 N2 63.41(6) . . ? O5 Ce1 N2 63.41(6) 2_656 . ? O1 Ce1 N2 72.64(6) 2_656 . ? O1 Ce1 N2 72.64(6) . . ? N1 Ce1 N2 116.99(7) . . ? N1 Ce1 N2 116.99(7) 2_656 . ? N3 Ag1 N4 161.14(15) . . ? C8 N2 C8 119.6(5) . 2_656 ? C8 N2 Ce1 120.2(2) . . ? C8 N2 Ce1 120.2(2) 2_656 . ? C5 N1 C1 119.9(3) . . ? C5 N1 Ce1 119.8(2) . . ? C1 N1 Ce1 120.0(2) . . ? N1 C1 C2 121.3(4) . . ? N1 C1 C6 113.6(3) . . ? C2 C1 C6 125.1(4) . . ? C7 O3 Ce1 128.4(2) . . ? C11 O5 Ce1 128.8(2) . . ? C21 N4 C17 116.9(4) . . ? C21 N4 Ag1 121.0(3) . . ? C17 N4 Ag1 121.8(3) . . ? C6 O1 Ce1 127.4(2) . . ? O4 C7 O3 126.3(4) . . ? O4 C7 C5 119.4(4) . . ? O3 C7 C5 114.3(3) . . ? N2 C8 C9 122.1(4) . . ? N2 C8 C11 113.8(3) . . ? C9 C8 C11 124.1(4) . . ? O6 C11 O5 125.3(4) . . ? O6 C11 C8 120.9(4) . . ? O5 C11 C8 113.8(3) . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C7 113.5(3) . . ? C4 C5 C7 125.3(4) . . ? C12 N3 C16 117.1(4) . . ? C12 N3 Ag1 120.7(3) . . ? C16 N3 Ag1 122.2(3) . . ? C4 C3 C2 119.6(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? O2 C6 O1 124.3(4) . . ? O2 C6 C1 120.6(4) . . ? O1 C6 C1 115.1(3) . . ? N4 C17 C18 123.6(4) . . ? N4 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N3 C12 C13 122.5(5) . . ? N3 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C17 C18 C19 118.4(4) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? N4 C21 C20 123.2(4) . . ? N4 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C21 C20 C19 118.9(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C19 C18 118.9(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C9 C10 C9 120.0(6) . 2_656 ? C9 C10 H10 120.0 . . ? C9 C10 H10 120.0 2_656 . ? C10 C9 C8 118.1(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N3 C16 C15 123.5(5) . . ? N3 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C14 C15 C16 118.6(6) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? 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 O3 Ce1 N2 C8 29.1(2) . . . . ? O3 Ce1 N2 C8 -150.9(2) 2_656 . . . ? O5 Ce1 N2 C8 -1.12(19) . . . . ? O5 Ce1 N2 C8 178.88(19) 2_656 . . . ? O1 Ce1 N2 C8 82.26(19) 2_656 . . . ? O1 Ce1 N2 C8 -97.74(19) . . . . ? N1 Ce1 N2 C8 -50.79(19) . . . . ? N1 Ce1 N2 C8 129.21(19) 2_656 . . . ? O3 Ce1 N2 C8 -150.9(2) . . . 2_656 ? O3 Ce1 N2 C8 29.1(2) 2_656 . . 2_656 ? O5 Ce1 N2 C8 178.88(19) . . . 2_656 ? O5 Ce1 N2 C8 -1.12(19) 2_656 . . 2_656 ? O1 Ce1 N2 C8 -97.74(19) 2_656 . . 2_656 ? O1 Ce1 N2 C8 82.26(19) . . . 2_656 ? N1 Ce1 N2 C8 129.21(19) . . . 2_656 ? N1 Ce1 N2 C8 -50.79(19) 2_656 . . 2_656 ? O3 Ce1 N1 C5 -5.3(2) . . . . ? O3 Ce1 N1 C5 -94.6(3) 2_656 . . . ? O5 Ce1 N1 C5 81.9(3) . . . . ? O5 Ce1 N1 C5 -153.5(2) 2_656 . . . ? O1 Ce1 N1 C5 35.3(3) 2_656 . . . ? O1 Ce1 N1 C5 178.9(3) . . . . ? N1 Ce1 N1 C5 -52.2(2) 2_656 . . . ? N2 Ce1 N1 C5 127.8(2) . . . . ? O3 Ce1 N1 C1 -179.0(3) . . . . ? O3 Ce1 N1 C1 91.8(3) 2_656 . . . ? O5 Ce1 N1 C1 -91.8(3) . . . . ? O5 Ce1 N1 C1 32.8(3) 2_656 . . . ? O1 Ce1 N1 C1 -138.3(2) 2_656 . . . ? O1 Ce1 N1 C1 5.3(2) . . . . ? N1 Ce1 N1 C1 134.1(3) 2_656 . . . ? N2 Ce1 N1 C1 -45.9(3) . . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Ce1 N1 C1 C2 174.1(3) . . . . ? C5 N1 C1 C6 179.5(3) . . . . ? Ce1 N1 C1 C6 -6.9(4) . . . . ? O3 Ce1 O3 C7 83.7(3) 2_656 . . . ? O5 Ce1 O3 C7 -69.1(3) . . . . ? O5 Ce1 O3 C7 141.9(3) 2_656 . . . ? O1 Ce1 O3 C7 -147.0(3) 2_656 . . . ? O1 Ce1 O3 C7 10.3(3) . . . . ? N1 Ce1 O3 C7 5.6(3) . . . . ? N1 Ce1 O3 C7 148.1(3) 2_656 . . . ? N2 Ce1 O3 C7 -96.3(3) . . . . ? O3 Ce1 O5 C11 -157.7(3) . . . . ? O3 Ce1 O5 C11 143.1(3) 2_656 . . . ? O5 Ce1 O5 C11 2.4(3) 2_656 . . . ? O1 Ce1 O5 C11 -74.7(3) 2_656 . . . ? O1 Ce1 O5 C11 73.9(3) . . . . ? N1 Ce1 O5 C11 136.7(3) . . . . ? N1 Ce1 O5 C11 -99.9(3) 2_656 . . . ? N2 Ce1 O5 C11 2.4(3) . . . . ? N3 Ag1 N4 C21 136.9(4) . . . . ? N3 Ag1 N4 C17 -49.7(6) . . . . ? O3 Ce1 O1 C6 -7.7(3) . . . . ? O3 Ce1 O1 C6 -82.2(3) 2_656 . . . ? O5 Ce1 O1 C6 67.7(3) . . . . ? O5 Ce1 O1 C6 -163.6(3) 2_656 . . . ? O1 Ce1 O1 C6 130.4(3) 2_656 . . . ? N1 Ce1 O1 C6 -2.9(3) . . . . ? N1 Ce1 O1 C6 -118.5(3) 2_656 . . . ? N2 Ce1 O1 C6 130.4(3) . . . . ? Ce1 O3 C7 O4 173.8(3) . . . . ? Ce1 O3 C7 C5 -5.1(4) . . . . ? C8 N2 C8 C9 -0.1(3) 2_656 . . . ? Ce1 N2 C8 C9 179.9(3) . . . . ? C8 N2 C8 C11 -179.8(3) 2_656 . . . ? Ce1 N2 C8 C11 0.2(3) . . . . ? Ce1 O5 C11 O6 177.5(3) . . . . ? Ce1 O5 C11 C8 -3.1(5) . . . . ? N2 C8 C11 O6 -179.0(4) . . . . ? C9 C8 C11 O6 1.4(6) . . . . ? N2 C8 C11 O5 1.6(5) . . . . ? C9 C8 C11 O5 -178.1(4) . . . . ? C1 N1 C5 C4 -1.2(5) . . . . ? Ce1 N1 C5 C4 -174.9(3) . . . . ? C1 N1 C5 C7 178.7(3) . . . . ? Ce1 N1 C5 C7 5.0(4) . . . . ? O4 C7 C5 N1 -179.5(3) . . . . ? O3 C7 C5 N1 -0.5(5) . . . . ? O4 C7 C5 C4 0.4(6) . . . . ? O3 C7 C5 C4 179.4(4) . . . . ? N4 Ag1 N3 C12 -178.4(4) . . . . ? N4 Ag1 N3 C16 3.3(7) . . . . ? Ce1 O1 C6 O2 -179.4(3) . . . . ? Ce1 O1 C6 C1 0.6(5) . . . . ? N1 C1 C6 O2 -175.7(4) . . . . ? C2 C1 C6 O2 3.3(6) . . . . ? N1 C1 C6 O1 4.3(5) . . . . ? C2 C1 C6 O1 -176.8(4) . . . . ? C21 N4 C17 C18 0.9(7) . . . . ? Ag1 N4 C17 C18 -172.7(4) . . . . ? C2 C3 C4 C5 -1.5(7) . . . . ? N1 C5 C4 C3 1.8(6) . . . . ? C7 C5 C4 C3 -178.1(4) . . . . ? C16 N3 C12 C13 1.4(8) . . . . ? Ag1 N3 C12 C13 -177.0(4) . . . . ? C4 C3 C2 C1 0.8(7) . . . . ? N1 C1 C2 C3 -0.3(6) . . . . ? C6 C1 C2 C3 -179.2(4) . . . . ? N4 C17 C18 C19 0.2(7) . . . . ? C17 N4 C21 C20 -0.9(7) . . . . ? Ag1 N4 C21 C20 172.8(4) . . . . ? N4 C21 C20 C19 -0.3(8) . . . . ? C21 C20 C19 C18 1.4(8) . . . . ? C17 C18 C19 C20 -1.4(8) . . . . ? C9 C10 C9 C8 -0.1(3) 2_656 . . . ? N2 C8 C9 C10 0.2(5) . . . . ? C11 C8 C9 C10 179.9(3) . . . . ? C12 N3 C16 C15 0.0(9) . . . . ? Ag1 N3 C16 C15 178.4(5) . . . . ? N3 C16 C15 C14 -1.2(11) . . . . ? C16 C15 C14 C13 0.9(11) . . . . ? C15 C14 C13 C12 0.3(10) . . . . ? N3 C12 C13 C14 -1.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.981 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.094 # Attachment 'all.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 640099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 Ag N2 O13.50 Pr' _chemical_formula_sum 'C14 H17 Ag N2 O13.50 Pr' _chemical_formula_weight 678.08 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8009(16) _cell_length_b 10.7176(11) _cell_length_c 12.8757(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.468(2) _cell_angle_gamma 90.00 _cell_volume 2014.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5515 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 3.437 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.523578 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11124 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.34 _reflns_number_total 4096 _reflns_number_gt 3418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+2.1663P] 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 SHELXL _refine_ls_extinction_coef 0.00074(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4096 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Pr1 Pr 0.277788(15) 0.80542(2) 0.646194(16) 0.01817(10) Uani 1 1 d . . . Ag1 Ag 0.37925(4) 1.27323(5) 0.62302(5) 0.07068(19) Uani 1 1 d . . . O1 O 0.1603(2) 0.9354(3) 0.7175(2) 0.0344(8) Uani 1 1 d . . . O2 O 0.0695(3) 1.1035(3) 0.7116(3) 0.0452(9) Uani 1 1 d . . . O3 O 0.2825(2) 0.7895(3) 0.4507(2) 0.0268(7) Uani 1 1 d . . . O4 O 0.2299(2) 0.8356(3) 0.2824(2) 0.0294(7) Uani 1 1 d . . . O5 O 0.3498(2) 0.5973(3) 0.6280(3) 0.0314(7) Uani 1 1 d . . . O6 O 0.4673(2) 0.4688(3) 0.6237(3) 0.0386(8) Uani 1 1 d . . . O7 O 0.3569(2) 1.0074(3) 0.6289(2) 0.0313(7) Uani 1 1 d . . . O8 O 0.4831(3) 1.1227(3) 0.6305(3) 0.0428(9) Uani 1 1 d . . . O9 O 0.3628(2) 0.8619(3) 0.8246(2) 0.0395(9) Uani 1 1 d . . . H9A H 0.3532 0.8165 0.8758 0.047 Uiso 1 1 d R . . H9B H 0.4167 0.8909 0.8273 0.047 Uiso 1 1 d R . . O10 O 0.1408(2) 0.6837(3) 0.5657(3) 0.0418(9) Uani 1 1 d . . . H10A H 0.1278 0.6974 0.4992 0.050 Uiso 1 1 d R . . H10B H 0.1246 0.6319 0.5967 0.050 Uiso 1 1 d R . . O11 O 0.2494(4) 1.3813(4) 0.6229(5) 0.0835(15) Uani 1 1 d . . . H11C H 0.2195 1.3831 0.5634 0.100 Uiso 1 1 d R . . H11B H 0.2335 1.4154 0.6769 0.100 Uiso 1 1 d R . . N1 N 0.1741(2) 0.9557(3) 0.5173(3) 0.0207(7) Uani 1 1 d . . . N2 N 0.4503(3) 0.7971(3) 0.6267(3) 0.0235(8) Uani 1 1 d . . . C1 C 0.1175(3) 1.0279(4) 0.6707(3) 0.0289(10) Uani 1 1 d . . . C2 C 0.1251(3) 1.0438(4) 0.5562(3) 0.0233(9) Uani 1 1 d . . . C3 C 0.0847(3) 1.1416(5) 0.4948(4) 0.0353(11) Uani 1 1 d . . . H3 H 0.0525 1.2035 0.5238 0.042 Uiso 1 1 calc R . . C4 C 0.0936(4) 1.1450(5) 0.3898(4) 0.0382(12) Uani 1 1 d . . . H4 H 0.0670 1.2097 0.3472 0.046 Uiso 1 1 calc R . . C5 C 0.1420(3) 1.0524(4) 0.3477(3) 0.0308(10) Uani 1 1 d . . . H5 H 0.1482 1.0530 0.2770 0.037 Uiso 1 1 calc R . . C6 C 0.1809(3) 0.9587(4) 0.4151(3) 0.0210(9) Uani 1 1 d . . . C7 C 0.2354(3) 0.8523(4) 0.3788(3) 0.0208(9) Uani 1 1 d . . . C8 C 0.4329(3) 0.5757(4) 0.6250(3) 0.0275(10) Uani 1 1 d . . . C9 C 0.4941(3) 0.6879(4) 0.6239(4) 0.0263(10) Uani 1 1 d . . . C10 C 0.5862(4) 0.6810(5) 0.6223(4) 0.0390(12) Uani 1 1 d . . . H10 H 0.6148 0.6041 0.6192 0.047 Uiso 1 1 calc R . . C11 C 0.6362(4) 0.7914(5) 0.6253(5) 0.0463(14) Uani 1 1 d . . . H11A H 0.6990 0.7894 0.6251 0.056 Uiso 1 1 calc R . . C12 C 0.5914(4) 0.9036(5) 0.6286(4) 0.0422(13) Uani 1 1 d . . . H12 H 0.6234 0.9785 0.6313 0.051 Uiso 1 1 calc R . . C13 C 0.4980(3) 0.9029(4) 0.6279(3) 0.0281(10) Uani 1 1 d . . . C14 C 0.4423(3) 1.0205(4) 0.6290(3) 0.0282(10) Uani 1 1 d . . . O12 O 0.0546(2) 0.7007(3) 0.3541(3) 0.0384(8) Uani 1 1 d . . . H12A H 0.0785 0.6660 0.3057 0.046 Uiso 1 1 d R . . H12B H 0.0381 0.7763 0.3441 0.046 Uiso 1 1 d R . . O13 O 0.2111(6) 0.0568(9) 0.9215(6) 0.072(3) Uani 0.50 1 d P . . H13A H 0.2222 0.1133 0.8804 0.086 Uiso 0.50 1 d PR . . H13B H 0.2235 0.0714 0.9874 0.086 Uiso 0.50 1 d PR . . O14 O 0.9963(4) 1.0452(5) 0.8833(4) 0.0617(16) Uani 0.75 1 d P . . O14' O 0.9231(11) 0.9502(14) 0.9148(10) 0.045(4) Uani 0.25 1 d P . . 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 Pr1 0.01992(14) 0.01913(14) 0.01576(13) 0.00085(9) 0.00387(9) 0.00104(9) Ag1 0.0783(4) 0.0448(3) 0.0842(4) -0.0015(3) -0.0007(3) 0.0099(3) O1 0.042(2) 0.0377(19) 0.0252(16) 0.0049(14) 0.0120(14) 0.0161(15) O2 0.062(3) 0.045(2) 0.0323(19) -0.0004(16) 0.0202(18) 0.0241(19) O3 0.0329(18) 0.0299(16) 0.0177(15) 0.0006(12) 0.0049(13) 0.0098(14) O4 0.0373(19) 0.0348(17) 0.0167(15) -0.0034(13) 0.0059(14) 0.0086(14) O5 0.0265(18) 0.0209(16) 0.048(2) 0.0020(14) 0.0107(15) 0.0006(13) O6 0.0337(19) 0.0267(17) 0.055(2) 0.0028(16) 0.0052(16) 0.0089(15) O7 0.0323(18) 0.0228(16) 0.0393(18) 0.0006(14) 0.0074(15) -0.0035(13) O8 0.048(2) 0.0260(18) 0.055(2) 0.0022(16) 0.0096(18) -0.0128(16) O9 0.042(2) 0.048(2) 0.0254(17) 0.0076(15) -0.0013(15) -0.0229(17) O10 0.041(2) 0.052(2) 0.0285(18) 0.0128(16) -0.0077(16) -0.0169(17) O11 0.083(4) 0.055(3) 0.112(4) -0.011(3) 0.016(3) 0.000(3) N1 0.0238(18) 0.0247(18) 0.0139(16) -0.0018(14) 0.0043(14) 0.0030(15) N2 0.026(2) 0.0230(18) 0.0218(18) -0.0005(14) 0.0050(15) -0.0035(15) C1 0.033(3) 0.029(2) 0.027(2) -0.0020(19) 0.010(2) 0.008(2) C2 0.022(2) 0.024(2) 0.023(2) -0.0010(17) 0.0036(18) 0.0046(17) C3 0.044(3) 0.031(2) 0.032(3) 0.002(2) 0.008(2) 0.016(2) C4 0.052(3) 0.033(3) 0.027(2) 0.007(2) 0.000(2) 0.011(2) C5 0.040(3) 0.031(2) 0.020(2) 0.0017(19) 0.002(2) 0.002(2) C6 0.024(2) 0.021(2) 0.018(2) -0.0025(16) 0.0039(17) -0.0023(17) C7 0.019(2) 0.022(2) 0.023(2) 0.0004(17) 0.0057(17) -0.0041(17) C8 0.031(3) 0.026(2) 0.026(2) 0.0009(18) 0.0053(19) 0.0077(19) C9 0.023(2) 0.031(2) 0.025(2) -0.0004(18) 0.0045(18) 0.0046(18) C10 0.032(3) 0.040(3) 0.046(3) -0.001(2) 0.009(2) 0.007(2) C11 0.030(3) 0.054(4) 0.059(4) -0.007(3) 0.018(3) -0.005(2) C12 0.034(3) 0.043(3) 0.052(3) -0.005(3) 0.014(2) -0.013(2) C13 0.029(2) 0.033(2) 0.022(2) -0.0021(19) 0.0041(19) -0.008(2) C14 0.036(3) 0.025(2) 0.023(2) 0.0011(18) 0.005(2) -0.007(2) O12 0.041(2) 0.040(2) 0.0338(19) -0.0027(15) 0.0076(16) 0.0036(16) O13 0.094(7) 0.093(7) 0.029(4) -0.030(4) 0.011(4) -0.035(6) O14 0.077(4) 0.064(4) 0.050(3) 0.014(3) 0.026(3) 0.024(3) O14' 0.057(10) 0.048(9) 0.027(7) 0.007(6) -0.001(7) 0.013(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 Pr1 O7 2.488(3) . ? Pr1 O10 2.489(3) . ? Pr1 O5 2.499(3) . ? Pr1 O4 2.504(3) 4_576 ? Pr1 O9 2.505(3) . ? Pr1 O1 2.517(3) . ? Pr1 O3 2.536(3) . ? Pr1 N2 2.608(4) . ? Pr1 N1 2.620(3) . ? Ag1 O8 2.220(4) . ? Ag1 O11 2.243(5) . ? Ag1 O6 2.466(3) 1_565 ? O1 C1 1.273(5) . ? O2 C1 1.250(5) . ? O3 C7 1.258(5) . ? O4 C7 1.244(5) . ? O4 Pr1 2.504(3) 4_575 ? O5 C8 1.258(5) . ? O6 C8 1.255(5) . ? O6 Ag1 2.466(3) 1_545 ? O7 C14 1.273(6) . ? O8 C14 1.249(5) . ? O9 H9A 0.8501 . ? O9 H9B 0.8504 . ? O10 H10A 0.8589 . ? O10 H10B 0.7460 . ? O11 H11C 0.8200 . ? O11 H11B 0.8527 . ? N1 C6 1.337(5) . ? N1 C2 1.337(5) . ? N2 C13 1.334(6) . ? N2 C9 1.342(5) . ? C1 C2 1.508(6) . ? C2 C3 1.387(6) . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 C5 1.385(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 C7 1.514(6) . ? C8 C9 1.507(6) . ? C9 C10 1.368(7) . ? C10 C11 1.393(8) . ? C10 H10 0.9300 . ? C11 C12 1.378(8) . ? C11 H11A 0.9300 . ? C12 C13 1.380(7) . ? C12 H12 0.9300 . ? C13 C14 1.507(7) . ? O12 H12A 0.8504 . ? O12 H12B 0.8501 . ? O13 H13A 0.8373 . ? O13 H13B 0.8527 . ? O14 O14' 1.588(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Pr1 O10 141.41(10) . . ? O7 Pr1 O5 123.62(11) . . ? O10 Pr1 O5 79.88(11) . . ? O7 Pr1 O4 141.18(10) . 4_576 ? O10 Pr1 O4 70.76(10) . 4_576 ? O5 Pr1 O4 72.63(11) . 4_576 ? O7 Pr1 O9 72.48(10) . . ? O10 Pr1 O9 139.51(11) . . ? O5 Pr1 O9 98.27(11) . . ? O4 Pr1 O9 70.19(10) 4_576 . ? O7 Pr1 O1 85.08(11) . . ? O10 Pr1 O1 82.97(12) . . ? O5 Pr1 O1 149.23(11) . . ? O4 Pr1 O1 77.68(11) 4_576 . ? O9 Pr1 O1 78.75(12) . . ? O7 Pr1 O3 83.09(10) . . ? O10 Pr1 O3 72.84(11) . . ? O5 Pr1 O3 76.40(10) . . ? O4 Pr1 O3 135.39(10) 4_576 . ? O9 Pr1 O3 146.59(11) . . ? O1 Pr1 O3 122.21(10) . . ? O7 Pr1 N2 62.53(11) . . ? O10 Pr1 N2 133.28(12) . . ? O5 Pr1 N2 61.38(10) . . ? O4 Pr1 N2 116.17(11) 4_576 . ? O9 Pr1 N2 75.17(11) . . ? O1 Pr1 N2 143.14(11) . . ? O3 Pr1 N2 73.44(11) . . ? O7 Pr1 N1 69.13(10) . . ? O10 Pr1 N1 72.91(11) . . ? O5 Pr1 N1 134.70(10) . . ? O4 Pr1 N1 127.65(11) 4_576 . ? O9 Pr1 N1 125.87(11) . . ? O1 Pr1 N1 61.50(10) . . ? O3 Pr1 N1 61.41(10) . . ? N2 Pr1 N1 116.16(11) . . ? O8 Ag1 O11 164.23(16) . . ? O8 Ag1 O6 104.83(12) . 1_565 ? O11 Ag1 O6 90.74(15) . 1_565 ? C1 O1 Pr1 125.4(3) . . ? C7 O3 Pr1 126.2(3) . . ? C7 O4 Pr1 143.7(3) . 4_575 ? C8 O5 Pr1 127.0(3) . . ? C8 O6 Ag1 124.1(3) . 1_545 ? C14 O7 Pr1 125.3(3) . . ? C14 O8 Ag1 107.9(3) . . ? Pr1 O9 H9A 116.8 . . ? Pr1 O9 H9B 116.9 . . ? H9A O9 H9B 116.9 . . ? Pr1 O10 H10A 111.1 . . ? Pr1 O10 H10B 118.6 . . ? H10A O10 H10B 128.4 . . ? Ag1 O11 H11C 110.1 . . ? Ag1 O11 H11B 125.0 . . ? H11C O11 H11B 124.9 . . ? C6 N1 C2 119.0(4) . . ? C6 N1 Pr1 120.5(3) . . ? C2 N1 Pr1 119.6(3) . . ? C13 N2 C9 119.0(4) . . ? C13 N2 Pr1 119.6(3) . . ? C9 N2 Pr1 121.1(3) . . ? O2 C1 O1 125.4(4) . . ? O2 C1 C2 118.6(4) . . ? O1 C1 C2 116.1(4) . . ? N1 C2 C3 122.0(4) . . ? N1 C2 C1 114.8(3) . . ? C3 C2 C1 123.2(4) . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 117.5(4) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? N1 C6 C5 122.8(4) . . ? N1 C6 C7 114.5(4) . . ? C5 C6 C7 122.7(4) . . ? O4 C7 O3 126.4(4) . . ? O4 C7 C6 117.7(4) . . ? O3 C7 C6 115.8(4) . . ? O6 C8 O5 124.7(4) . . ? O6 C8 C9 118.9(4) . . ? O5 C8 C9 116.4(4) . . ? N2 C9 C10 122.3(4) . . ? N2 C9 C8 113.7(4) . . ? C10 C9 C8 124.0(4) . . ? C9 C10 C11 118.7(5) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 119.1(5) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 118.8(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N2 C13 C12 122.2(4) . . ? N2 C13 C14 114.9(4) . . ? C12 C13 C14 122.9(4) . . ? O8 C14 O7 125.1(4) . . ? O8 C14 C13 118.0(4) . . ? O7 C14 C13 116.9(4) . . ? H12A O12 H12B 116.6 . . ? H13A O13 H13B 117.7 . . ? 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 O7 Pr1 O1 C1 55.1(4) . . . . ? O10 Pr1 O1 C1 -88.1(4) . . . . ? O5 Pr1 O1 C1 -144.6(3) . . . . ? O4 Pr1 O1 C1 -159.9(4) 4_576 . . . ? O9 Pr1 O1 C1 128.2(4) . . . . ? O3 Pr1 O1 C1 -23.6(4) . . . . ? N2 Pr1 O1 C1 82.6(4) . . . . ? N1 Pr1 O1 C1 -13.8(3) . . . . ? O7 Pr1 O3 C7 -72.0(3) . . . . ? O10 Pr1 O3 C7 77.5(3) . . . . ? O5 Pr1 O3 C7 160.9(4) . . . . ? O4 Pr1 O3 C7 114.0(3) 4_576 . . . ? O9 Pr1 O3 C7 -114.7(4) . . . . ? O1 Pr1 O3 C7 7.7(4) . . . . ? N2 Pr1 O3 C7 -135.3(4) . . . . ? N1 Pr1 O3 C7 -2.0(3) . . . . ? O7 Pr1 O5 C8 11.5(4) . . . . ? O10 Pr1 O5 C8 158.1(4) . . . . ? O4 Pr1 O5 C8 -129.1(4) 4_576 . . . ? O9 Pr1 O5 C8 -62.9(4) . . . . ? O1 Pr1 O5 C8 -144.8(3) . . . . ? O3 Pr1 O5 C8 83.4(4) . . . . ? N2 Pr1 O5 C8 5.1(4) . . . . ? N1 Pr1 O5 C8 104.7(4) . . . . ? O10 Pr1 O7 C14 -133.1(3) . . . . ? O5 Pr1 O7 C14 -13.5(4) . . . . ? O4 Pr1 O7 C14 91.3(4) 4_576 . . . ? O9 Pr1 O7 C14 74.9(3) . . . . ? O1 Pr1 O7 C14 154.6(3) . . . . ? O3 Pr1 O7 C14 -82.1(3) . . . . ? N2 Pr1 O7 C14 -7.2(3) . . . . ? N1 Pr1 O7 C14 -144.0(4) . . . . ? O11 Ag1 O8 C14 10.2(8) . . . . ? O6 Ag1 O8 C14 -179.2(3) 1_565 . . . ? O7 Pr1 N1 C6 87.1(3) . . . . ? O10 Pr1 N1 C6 -85.8(3) . . . . ? O5 Pr1 N1 C6 -30.1(4) . . . . ? O4 Pr1 N1 C6 -133.5(3) 4_576 . . . ? O9 Pr1 N1 C6 134.8(3) . . . . ? O1 Pr1 N1 C6 -177.0(3) . . . . ? O3 Pr1 N1 C6 -6.4(3) . . . . ? N2 Pr1 N1 C6 44.6(3) . . . . ? O7 Pr1 N1 C2 -82.0(3) . . . . ? O10 Pr1 N1 C2 105.1(3) . . . . ? O5 Pr1 N1 C2 160.9(3) . . . . ? O4 Pr1 N1 C2 57.4(3) 4_576 . . . ? O9 Pr1 N1 C2 -34.3(4) . . . . ? O1 Pr1 N1 C2 13.9(3) . . . . ? O3 Pr1 N1 C2 -175.5(3) . . . . ? N2 Pr1 N1 C2 -124.5(3) . . . . ? O7 Pr1 N2 C13 6.7(3) . . . . ? O10 Pr1 N2 C13 142.8(3) . . . . ? O5 Pr1 N2 C13 -179.3(3) . . . . ? O4 Pr1 N2 C13 -129.6(3) 4_576 . . . ? O9 Pr1 N2 C13 -71.0(3) . . . . ? O1 Pr1 N2 C13 -24.6(4) . . . . ? O3 Pr1 N2 C13 97.5(3) . . . . ? N1 Pr1 N2 C13 52.1(3) . . . . ? O7 Pr1 N2 C9 -178.6(4) . . . . ? O10 Pr1 N2 C9 -42.5(4) . . . . ? O5 Pr1 N2 C9 -4.6(3) . . . . ? O4 Pr1 N2 C9 45.1(3) 4_576 . . . ? O9 Pr1 N2 C9 103.7(3) . . . . ? O1 Pr1 N2 C9 150.1(3) . . . . ? O3 Pr1 N2 C9 -87.8(3) . . . . ? N1 Pr1 N2 C9 -133.2(3) . . . . ? Pr1 O1 C1 O2 -168.9(4) . . . . ? Pr1 O1 C1 C2 12.3(6) . . . . ? C6 N1 C2 C3 -3.1(6) . . . . ? Pr1 N1 C2 C3 166.1(3) . . . . ? C6 N1 C2 C1 176.8(4) . . . . ? Pr1 N1 C2 C1 -14.0(5) . . . . ? O2 C1 C2 N1 -177.0(4) . . . . ? O1 C1 C2 N1 1.9(6) . . . . ? O2 C1 C2 C3 2.9(7) . . . . ? O1 C1 C2 C3 -178.2(4) . . . . ? N1 C2 C3 C4 1.9(7) . . . . ? C1 C2 C3 C4 -177.9(5) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C2 N1 C6 C5 2.5(6) . . . . ? Pr1 N1 C6 C5 -166.6(3) . . . . ? C2 N1 C6 C7 -178.2(4) . . . . ? Pr1 N1 C6 C7 12.7(5) . . . . ? C4 C5 C6 N1 -0.7(7) . . . . ? C4 C5 C6 C7 180.0(4) . . . . ? Pr1 O4 C7 O3 5.3(8) 4_575 . . . ? Pr1 O4 C7 C6 -175.1(3) 4_575 . . . ? Pr1 O3 C7 O4 -171.5(3) . . . . ? Pr1 O3 C7 C6 8.9(5) . . . . ? N1 C6 C7 O4 166.6(4) . . . . ? C5 C6 C7 O4 -14.1(6) . . . . ? N1 C6 C7 O3 -13.8(5) . . . . ? C5 C6 C7 O3 165.5(4) . . . . ? Ag1 O6 C8 O5 1.4(7) 1_545 . . . ? Ag1 O6 C8 C9 -179.2(3) 1_545 . . . ? Pr1 O5 C8 O6 174.3(3) . . . . ? Pr1 O5 C8 C9 -5.0(6) . . . . ? C13 N2 C9 C10 0.1(7) . . . . ? Pr1 N2 C9 C10 -174.6(4) . . . . ? C13 N2 C9 C8 178.9(4) . . . . ? Pr1 N2 C9 C8 4.2(5) . . . . ? O6 C8 C9 N2 -179.2(4) . . . . ? O5 C8 C9 N2 0.2(6) . . . . ? O6 C8 C9 C10 -0.4(7) . . . . ? O5 C8 C9 C10 179.0(5) . . . . ? N2 C9 C10 C11 1.0(8) . . . . ? C8 C9 C10 C11 -177.7(5) . . . . ? C9 C10 C11 C12 -0.7(9) . . . . ? C10 C11 C12 C13 -0.5(9) . . . . ? C9 N2 C13 C12 -1.5(7) . . . . ? Pr1 N2 C13 C12 173.3(4) . . . . ? C9 N2 C13 C14 178.9(4) . . . . ? Pr1 N2 C13 C14 -6.3(5) . . . . ? C11 C12 C13 N2 1.7(8) . . . . ? C11 C12 C13 C14 -178.7(5) . . . . ? Ag1 O8 C14 O7 -3.4(6) . . . . ? Ag1 O8 C14 C13 177.0(3) . . . . ? Pr1 O7 C14 O8 -172.8(3) . . . . ? Pr1 O7 C14 C13 6.9(5) . . . . ? N2 C13 C14 O8 179.8(4) . . . . ? C12 C13 C14 O8 0.1(7) . . . . ? N2 C13 C14 O7 0.1(6) . . . . ? C12 C13 C14 O7 -179.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.399 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.128 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 640100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Ag N2 O14 Sm' _chemical_formula_weight 696.52 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.621(2) _cell_length_b 7.3491(10) _cell_length_c 19.765(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.776(2) _cell_angle_gamma 90.00 _cell_volume 2098.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5795 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 26.40 _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 3.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.626759 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADBAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11414 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4293 _reflns_number_gt 3638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+14.8708P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4293 _refine_ls_number_parameters 296 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.827 _refine_ls_shift/su_max 0.054 _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 Sm1 Sm 0.29579(4) 0.45879(7) 0.13841(3) 0.0200(2) Uani 1 1 d U . . Ag1 Ag 0.37926(11) -0.0024(2) 0.00728(12) 0.0923(6) Uani 1 1 d U . . O1 O 0.1969(6) 0.7274(11) 0.1381(4) 0.0300(18) Uani 1 1 d . . . O2 O 0.0954(7) 0.9301(12) 0.0864(5) 0.042(2) Uani 1 1 d . . . O3 O 0.2936(6) 0.2450(12) 0.0427(4) 0.035(2) Uani 1 1 d . . . O4 O 0.2371(8) 0.1269(14) -0.0569(5) 0.049(3) Uani 1 1 d . . . O5 O 0.3693(6) 0.6740(12) 0.0682(4) 0.034(2) Uani 1 1 d . . . O6 O 0.4945(7) 0.8029(13) 0.0379(6) 0.052(3) Uani 1 1 d . . . O7 O 0.3676(5) 0.1820(11) 0.1936(4) 0.0304(18) Uani 1 1 d . . . O8 O 0.4831(6) -0.0184(12) 0.2148(6) 0.047(3) Uani 1 1 d . . . O9 O 0.1621(6) 0.2546(11) 0.1446(4) 0.0306(18) Uani 1 1 d D . . H9A H 0.158(9) 0.145(5) 0.131(5) 0.037 Uiso 1 1 d D . . H9B H 0.133(8) 0.333(10) 0.118(5) 0.037 Uiso 1 1 d D . . O10 O 0.2473(6) 0.4511(11) 0.2515(4) 0.0299(18) Uani 1 1 d . . . H10A H 0.2132 0.5334 0.2648 0.036 Uiso 1 1 d R . . H10B H 0.2773 0.3842 0.2824 0.036 Uiso 1 1 d R . . O11 O 0.3962(6) 0.6575(11) 0.2201(4) 0.0326(19) Uani 1 1 d . . . H11A H 0.4080 0.7679 0.2115 0.039 Uiso 1 1 d R . . H11B H 0.4398 0.5976 0.2439 0.039 Uiso 1 1 d R . . N1 N 0.1782(6) 0.5181(12) 0.0294(5) 0.0229(19) Uani 1 1 d . . . N2 N 0.4643(6) 0.3972(13) 0.1265(5) 0.025(2) Uani 1 1 d . . . C1 C 0.1404(8) 0.7865(16) 0.0883(6) 0.028(2) Uani 1 1 d . . . C2 C 0.1262(8) 0.6675(15) 0.0247(6) 0.025(2) Uani 1 1 d . . . C3 C 0.0642(9) 0.7082(18) -0.0329(6) 0.037(3) Uani 1 1 d . . . H3 H 0.0282 0.8128 -0.0347 0.044 Uiso 1 1 calc R . . C4 C 0.0564(10) 0.590(2) -0.0883(7) 0.044(3) Uani 1 1 d . . . H4 H 0.0160 0.6161 -0.1283 0.053 Uiso 1 1 calc R . . C5 C 0.1098(9) 0.4331(19) -0.0834(7) 0.038(3) Uani 1 1 d . . . H5 H 0.1047 0.3504 -0.1194 0.045 Uiso 1 1 calc R . . C6 C 0.1710(8) 0.4024(16) -0.0233(6) 0.026(2) Uani 1 1 d . . . C7 C 0.2369(9) 0.2461(16) -0.0124(6) 0.031(3) Uani 1 1 d . . . C8 C 0.4552(9) 0.6770(16) 0.0652(6) 0.032(3) Uani 1 1 d . . . C9 C 0.5123(9) 0.5183(16) 0.0953(6) 0.030(3) Uani 1 1 d . . . C10 C 0.6034(10) 0.4953(19) 0.0900(8) 0.044(3) Uani 1 1 d . . . H10 H 0.6345 0.5813 0.0676 0.053 Uiso 1 1 calc R . . C11 C 0.6488(10) 0.343(2) 0.1184(9) 0.053(4) Uani 1 1 d . . . H11 H 0.7113 0.3263 0.1163 0.064 Uiso 1 1 calc R . . C12 C 0.5999(9) 0.215(2) 0.1503(8) 0.045(4) Uani 1 1 d . . . H12 H 0.6285 0.1097 0.1687 0.054 Uiso 1 1 calc R . . C13 C 0.5082(8) 0.2485(16) 0.1540(6) 0.029(3) Uani 1 1 d . . . C14 C 0.4488(8) 0.1253(16) 0.1906(6) 0.030(3) Uani 1 1 d . . . O12 O 0.8035(8) 0.9665(16) 0.1914(6) 0.057(3) Uani 1 1 d U . . H12A H 0.7789 0.9942 0.1461 0.069 Uiso 1 1 d R . . H12B H 0.8268 0.8504 0.2023 0.069 Uiso 1 1 d R . . O13 O 0.9914(8) 0.9464(17) 0.1980(7) 0.067(3) Uani 1 1 d U . . H13A H 0.9997 0.9413 0.1544 0.080 Uiso 1 1 d R . . H13B H 0.9523 1.0394 0.2123 0.080 Uiso 1 1 d R . . O14 O 0.8358(10) 0.326(2) 0.2452(7) 0.081(4) Uani 1 1 d U . . H14A H 0.8843 0.2840 0.2716 0.098 Uiso 1 1 d R . . H14B H 0.8156 0.2627 0.2093 0.098 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 Sm1 0.0220(3) 0.0174(3) 0.0207(3) 0.0014(2) 0.0040(2) 0.0021(2) Ag1 0.0645(9) 0.0610(8) 0.1565(14) 0.0520(9) 0.0332(9) 0.0313(7) O1 0.035(5) 0.029(4) 0.024(4) -0.003(3) -0.003(3) 0.009(4) O2 0.052(6) 0.029(5) 0.041(5) -0.010(4) -0.005(4) 0.017(4) O3 0.040(5) 0.030(5) 0.033(5) -0.005(4) 0.001(4) 0.011(4) O4 0.066(7) 0.041(6) 0.039(5) -0.016(5) 0.001(5) 0.014(5) O5 0.037(5) 0.027(4) 0.038(5) 0.015(4) 0.012(4) 0.009(4) O6 0.048(6) 0.035(5) 0.078(7) 0.030(5) 0.028(5) 0.008(5) O7 0.026(4) 0.028(4) 0.039(5) 0.011(4) 0.012(4) 0.003(3) O8 0.034(5) 0.028(5) 0.078(7) 0.028(5) 0.007(5) 0.003(4) O9 0.035(5) 0.024(4) 0.032(4) 0.002(3) 0.002(4) -0.004(4) O10 0.043(5) 0.026(4) 0.023(4) 0.001(3) 0.012(3) 0.006(4) O11 0.034(5) 0.024(4) 0.038(5) 0.001(4) 0.000(4) -0.003(4) N1 0.028(5) 0.020(4) 0.021(4) 0.000(4) 0.004(4) 0.003(4) N2 0.025(5) 0.022(5) 0.029(5) 0.007(4) 0.006(4) 0.003(4) C1 0.029(6) 0.025(6) 0.032(6) -0.006(5) 0.007(5) 0.002(5) C2 0.029(6) 0.021(5) 0.025(5) 0.001(4) 0.001(5) 0.005(5) C3 0.041(7) 0.035(7) 0.033(7) -0.006(5) 0.000(6) 0.017(6) C4 0.047(8) 0.051(8) 0.030(7) -0.003(6) -0.012(6) 0.012(7) C5 0.042(7) 0.039(7) 0.030(6) -0.009(5) -0.002(5) 0.009(6) C6 0.028(6) 0.023(5) 0.027(6) -0.002(5) 0.005(5) 0.000(5) C7 0.039(7) 0.023(6) 0.033(6) -0.001(5) 0.010(5) 0.002(5) C8 0.040(7) 0.025(6) 0.032(6) 0.007(5) 0.014(5) 0.005(5) C9 0.033(6) 0.027(6) 0.032(6) 0.009(5) 0.011(5) 0.001(5) C10 0.039(7) 0.038(7) 0.059(9) 0.020(7) 0.020(7) 0.002(6) C11 0.030(7) 0.059(10) 0.076(11) 0.034(9) 0.023(7) 0.011(7) C12 0.032(7) 0.037(7) 0.069(10) 0.026(7) 0.015(7) 0.013(6) C13 0.027(6) 0.024(6) 0.037(6) 0.011(5) 0.009(5) 0.001(5) C14 0.028(6) 0.022(6) 0.040(7) 0.011(5) 0.007(5) 0.003(5) O12 0.057(3) 0.058(3) 0.057(3) -0.0011(18) 0.0083(18) 0.0002(18) O13 0.066(4) 0.068(4) 0.066(4) -0.0025(18) 0.0104(18) -0.0004(18) O14 0.081(4) 0.082(4) 0.082(4) -0.0023(18) 0.0122(19) 0.0002(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.446(8) . ? Sm1 O10 2.446(8) . ? Sm1 O5 2.457(8) . ? Sm1 O3 2.455(8) . ? Sm1 O7 2.465(8) . ? Sm1 O9 2.482(8) . ? Sm1 O11 2.485(8) . ? Sm1 N2 2.551(9) . ? Sm1 N1 2.581(9) . ? Sm1 H9B 2.52(12) . ? Ag1 O6 2.223(10) 1_545 ? Ag1 O3 2.374(8) . ? Ag1 O4 2.455(10) . ? O1 C1 1.263(14) . ? O2 C1 1.240(14) . ? O3 C7 1.264(15) . ? O4 C7 1.242(15) . ? O5 C8 1.267(15) . ? O6 C8 1.253(15) . ? O6 Ag1 2.223(10) 1_565 ? O7 C14 1.269(14) . ? O8 C14 1.234(14) . ? O9 H9A 0.852(19) . ? O9 H9B 0.850(18) . ? O10 H10A 0.8506 . ? O10 H10B 0.8517 . ? O11 H11A 0.8519 . ? O11 H11B 0.8540 . ? N1 C6 1.337(14) . ? N1 C2 1.330(14) . ? N2 C9 1.341(15) . ? N2 C13 1.340(15) . ? C1 C2 1.519(15) . ? C2 C3 1.376(16) . ? C3 C4 1.388(18) . ? C3 H3 0.9300 . ? C4 C5 1.388(19) . ? C4 H4 0.9300 . ? C5 C6 1.393(17) . ? C5 H5 0.9300 . ? C6 C7 1.493(16) . ? C8 C9 1.503(16) . ? C9 C10 1.363(18) . ? C10 C11 1.375(19) . ? C10 H10 0.9300 . ? C11 C12 1.388(19) . ? C11 H11 0.9300 . ? C12 C13 1.376(17) . ? C12 H12 0.9300 . ? C13 C14 1.513(15) . ? O12 H12A 0.9346 . ? O12 H12B 0.9317 . ? O13 H13A 0.8901 . ? O13 H13B 0.9605 . ? O14 H14A 0.8694 . ? O14 H14B 0.8623 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O10 76.5(3) . . ? O1 Sm1 O5 77.8(3) . . ? O10 Sm1 O5 138.0(3) . . ? O1 Sm1 O3 125.2(3) . . ? O10 Sm1 O3 135.9(3) . . ? O5 Sm1 O3 86.1(3) . . ? O1 Sm1 O7 151.4(3) . . ? O10 Sm1 O7 74.9(3) . . ? O5 Sm1 O7 126.0(3) . . ? O3 Sm1 O7 76.5(3) . . ? O1 Sm1 O9 91.1(3) . . ? O10 Sm1 O9 66.5(3) . . ? O5 Sm1 O9 146.4(3) . . ? O3 Sm1 O9 74.5(3) . . ? O7 Sm1 O9 76.4(3) . . ? O1 Sm1 O11 79.5(3) . . ? O10 Sm1 O11 69.2(3) . . ? O5 Sm1 O11 73.9(3) . . ? O3 Sm1 O11 144.5(3) . . ? O7 Sm1 O11 91.6(3) . . ? O9 Sm1 O11 135.6(3) . . ? O1 Sm1 N2 136.2(3) . . ? O10 Sm1 N2 119.9(3) . . ? O5 Sm1 N2 63.3(3) . . ? O3 Sm1 N2 73.4(3) . . ? O7 Sm1 N2 62.8(3) . . ? O9 Sm1 N2 132.5(3) . . ? O11 Sm1 N2 71.4(3) . . ? O1 Sm1 N1 62.8(3) . . ? O10 Sm1 N1 121.2(3) . . ? O5 Sm1 N1 73.3(3) . . ? O3 Sm1 N1 62.4(3) . . ? O7 Sm1 N1 133.9(3) . . ? O9 Sm1 N1 73.4(3) . . ? O11 Sm1 N1 134.1(3) . . ? N2 Sm1 N1 118.9(3) . . ? O1 Sm1 H9B 75.7(16) . . ? O10 Sm1 H9B 75(2) . . ? O5 Sm1 H9B 128.8(14) . . ? O3 Sm1 H9B 75(3) . . ? O7 Sm1 H9B 95.5(8) . . ? O9 Sm1 H9B 19.6(7) . . ? O11 Sm1 H9B 140(3) . . ? N2 Sm1 H9B 145(2) . . ? N1 Sm1 H9B 55.7(15) . . ? O6 Ag1 O3 145.6(4) 1_545 . ? O6 Ag1 O4 159.5(4) 1_545 . ? O3 Ag1 O4 54.0(3) . . ? C1 O1 Sm1 126.6(7) . . ? C7 O3 Ag1 93.2(7) . . ? C7 O3 Sm1 126.1(7) . . ? Ag1 O3 Sm1 140.5(4) . . ? C7 O4 Ag1 90.0(8) . . ? C8 O5 Sm1 124.1(7) . . ? C8 O6 Ag1 102.4(8) . 1_565 ? C14 O7 Sm1 126.1(7) . . ? Sm1 O9 H9A 126(9) . . ? Sm1 O9 H9B 83(9) . . ? H9A O9 H9B 116(4) . . ? Sm1 O10 H10A 122.1 . . ? Sm1 O10 H10B 118.7 . . ? H10A O10 H10B 116.8 . . ? Sm1 O11 H11A 123.2 . . ? Sm1 O11 H11B 111.8 . . ? H11A O11 H11B 116.3 . . ? C6 N1 C2 119.7(10) . . ? C6 N1 Sm1 120.4(7) . . ? C2 N1 Sm1 119.9(7) . . ? C9 N2 C13 118.4(10) . . ? C9 N2 Sm1 120.3(7) . . ? C13 N2 Sm1 121.2(7) . . ? O2 C1 O1 126.7(11) . . ? O2 C1 C2 117.4(11) . . ? O1 C1 C2 115.9(10) . . ? N1 C2 C3 122.3(10) . . ? N1 C2 C1 114.4(10) . . ? C3 C2 C1 123.3(10) . . ? C2 C3 C4 118.8(12) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.1(12) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 118.4(12) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 121.6(11) . . ? N1 C6 C7 113.9(10) . . ? C5 C6 C7 124.4(11) . . ? O4 C7 O3 122.3(12) . . ? O4 C7 C6 120.7(12) . . ? O3 C7 C6 117.0(10) . . ? O6 C8 O5 123.8(11) . . ? O6 C8 C9 118.7(11) . . ? O5 C8 C9 117.5(10) . . ? N2 C9 C10 122.6(11) . . ? N2 C9 C8 113.6(10) . . ? C10 C9 C8 123.8(11) . . ? C9 C10 C11 119.1(12) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 119.0(12) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 118.6(12) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? N2 C13 C12 122.2(11) . . ? N2 C13 C14 114.0(10) . . ? C12 C13 C14 123.7(11) . . ? O8 C14 O7 126.2(11) . . ? O8 C14 C13 118.0(10) . . ? O7 C14 C13 115.8(10) . . ? H12A O12 H12B 119.6 . . ? H13A O13 H13B 119.4 . . ? H14A O14 H14B 116.7 . . ? 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 O10 Sm1 O1 C1 -141.7(10) . . . . ? O5 Sm1 O1 C1 71.8(10) . . . . ? O3 Sm1 O1 C1 -4.4(11) . . . . ? O7 Sm1 O1 C1 -138.9(9) . . . . ? O9 Sm1 O1 C1 -76.2(10) . . . . ? O11 Sm1 O1 C1 147.4(10) . . . . ? N2 Sm1 O1 C1 98.9(10) . . . . ? N1 Sm1 O1 C1 -5.5(9) . . . . ? O6 Ag1 O3 C7 -174.8(7) 1_545 . . . ? O4 Ag1 O3 C7 -3.6(7) . . . . ? O6 Ag1 O3 Sm1 8.7(10) 1_545 . . . ? O4 Ag1 O3 Sm1 179.9(8) . . . . ? O1 Sm1 O3 C7 -6.1(11) . . . . ? O10 Sm1 O3 C7 102.5(10) . . . . ? O5 Sm1 O3 C7 -78.2(10) . . . . ? O7 Sm1 O3 C7 153.4(10) . . . . ? O9 Sm1 O3 C7 74.1(10) . . . . ? O11 Sm1 O3 C7 -133.2(9) . . . . ? N2 Sm1 O3 C7 -141.4(10) . . . . ? N1 Sm1 O3 C7 -5.0(9) . . . . ? O1 Sm1 O3 Ag1 169.6(5) . . . . ? O10 Sm1 O3 Ag1 -81.9(8) . . . . ? O5 Sm1 O3 Ag1 97.5(7) . . . . ? O7 Sm1 O3 Ag1 -31.0(6) . . . . ? O9 Sm1 O3 Ag1 -110.3(7) . . . . ? O11 Sm1 O3 Ag1 42.5(9) . . . . ? N2 Sm1 O3 Ag1 34.2(6) . . . . ? N1 Sm1 O3 Ag1 170.7(8) . . . . ? O6 Ag1 O4 C7 169.4(9) 1_545 . . . ? O3 Ag1 O4 C7 3.7(7) . . . . ? O1 Sm1 O5 C8 149.1(10) . . . . ? O10 Sm1 O5 C8 95.7(10) . . . . ? O3 Sm1 O5 C8 -83.7(10) . . . . ? O7 Sm1 O5 C8 -13.4(11) . . . . ? O9 Sm1 O5 C8 -137.9(9) . . . . ? O11 Sm1 O5 C8 66.6(10) . . . . ? N2 Sm1 O5 C8 -10.3(9) . . . . ? N1 Sm1 O5 C8 -145.9(10) . . . . ? O1 Sm1 O7 C14 -142.1(9) . . . . ? O10 Sm1 O7 C14 -139.3(10) . . . . ? O5 Sm1 O7 C14 -0.2(11) . . . . ? O3 Sm1 O7 C14 74.8(10) . . . . ? O9 Sm1 O7 C14 151.8(10) . . . . ? O11 Sm1 O7 C14 -71.4(10) . . . . ? N2 Sm1 O7 C14 -3.3(10) . . . . ? N1 Sm1 O7 C14 101.7(10) . . . . ? O1 Sm1 N1 C6 -178.2(9) . . . . ? O10 Sm1 N1 C6 -126.3(8) . . . . ? O5 Sm1 N1 C6 97.2(9) . . . . ? O3 Sm1 N1 C6 2.8(8) . . . . ? O7 Sm1 N1 C6 -27.0(10) . . . . ? O9 Sm1 N1 C6 -78.2(8) . . . . ? O11 Sm1 N1 C6 143.3(8) . . . . ? N2 Sm1 N1 C6 51.7(9) . . . . ? O1 Sm1 N1 C2 3.8(8) . . . . ? O10 Sm1 N1 C2 55.7(9) . . . . ? O5 Sm1 N1 C2 -80.8(8) . . . . ? O3 Sm1 N1 C2 -175.2(9) . . . . ? O7 Sm1 N1 C2 155.0(7) . . . . ? O9 Sm1 N1 C2 103.8(8) . . . . ? O11 Sm1 N1 C2 -34.7(10) . . . . ? N2 Sm1 N1 C2 -126.3(8) . . . . ? O1 Sm1 N2 C9 -22.7(11) . . . . ? O10 Sm1 N2 C9 -125.0(9) . . . . ? O5 Sm1 N2 C9 7.2(8) . . . . ? O3 Sm1 N2 C9 101.2(9) . . . . ? O7 Sm1 N2 C9 -175.6(10) . . . . ? O9 Sm1 N2 C9 150.6(8) . . . . ? O11 Sm1 N2 C9 -73.7(9) . . . . ? N1 Sm1 N2 C9 57.0(10) . . . . ? O1 Sm1 N2 C13 153.9(8) . . . . ? O10 Sm1 N2 C13 51.7(10) . . . . ? O5 Sm1 N2 C13 -176.2(10) . . . . ? O3 Sm1 N2 C13 -82.1(9) . . . . ? O7 Sm1 N2 C13 1.0(9) . . . . ? O9 Sm1 N2 C13 -32.7(11) . . . . ? O11 Sm1 N2 C13 102.9(9) . . . . ? N1 Sm1 N2 C13 -126.3(9) . . . . ? Sm1 O1 C1 O2 -174.0(10) . . . . ? Sm1 O1 C1 C2 6.4(15) . . . . ? C6 N1 C2 C3 0.2(17) . . . . ? Sm1 N1 C2 C3 178.2(9) . . . . ? C6 N1 C2 C1 179.5(10) . . . . ? Sm1 N1 C2 C1 -2.5(13) . . . . ? O2 C1 C2 N1 178.3(11) . . . . ? O1 C1 C2 N1 -2.1(15) . . . . ? O2 C1 C2 C3 -2.5(18) . . . . ? O1 C1 C2 C3 177.2(12) . . . . ? N1 C2 C3 C4 -1(2) . . . . ? C1 C2 C3 C4 -180.0(13) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C2 N1 C6 C5 -0.5(17) . . . . ? Sm1 N1 C6 C5 -178.5(9) . . . . ? C2 N1 C6 C7 176.9(10) . . . . ? Sm1 N1 C6 C7 -1.1(13) . . . . ? C4 C5 C6 N1 1(2) . . . . ? C4 C5 C6 C7 -175.9(12) . . . . ? Ag1 O4 C7 O3 -6.6(13) . . . . ? Ag1 O4 C7 C6 170.9(10) . . . . ? Ag1 O3 C7 O4 6.9(13) . . . . ? Sm1 O3 C7 O4 -175.9(9) . . . . ? Ag1 O3 C7 C6 -170.8(9) . . . . ? Sm1 O3 C7 C6 6.4(15) . . . . ? N1 C6 C7 O4 179.2(12) . . . . ? C5 C6 C7 O4 -4(2) . . . . ? N1 C6 C7 O3 -3.1(16) . . . . ? C5 C6 C7 O3 174.2(12) . . . . ? Ag1 O6 C8 O5 2.9(16) 1_565 . . . ? Ag1 O6 C8 C9 -178.0(9) 1_565 . . . ? Sm1 O5 C8 O6 -168.7(10) . . . . ? Sm1 O5 C8 C9 12.2(15) . . . . ? C13 N2 C9 C10 0.5(19) . . . . ? Sm1 N2 C9 C10 177.3(11) . . . . ? C13 N2 C9 C8 178.8(11) . . . . ? Sm1 N2 C9 C8 -4.5(14) . . . . ? O6 C8 C9 N2 176.3(12) . . . . ? O5 C8 C9 N2 -4.5(17) . . . . ? O6 C8 C9 C10 -5(2) . . . . ? O5 C8 C9 C10 173.7(14) . . . . ? N2 C9 C10 C11 -1(2) . . . . ? C8 C9 C10 C11 -178.8(14) . . . . ? C9 C10 C11 C12 1(3) . . . . ? C10 C11 C12 C13 -2(3) . . . . ? C9 N2 C13 C12 -1.0(19) . . . . ? Sm1 N2 C13 C12 -177.7(11) . . . . ? C9 N2 C13 C14 177.4(11) . . . . ? Sm1 N2 C13 C14 0.7(14) . . . . ? C11 C12 C13 N2 2(2) . . . . ? C11 C12 C13 C14 -176.6(14) . . . . ? Sm1 O7 C14 O8 -175.5(11) . . . . ? Sm1 O7 C14 C13 4.8(16) . . . . ? N2 C13 C14 O8 177.0(12) . . . . ? C12 C13 C14 O8 -5(2) . . . . ? N2 C13 C14 O7 -3.4(17) . . . . ? C12 C13 C14 O7 175.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.529 _refine_diff_density_min -2.722 _refine_diff_density_rms 0.177 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 640101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Ag Dy N2 O14' _chemical_formula_weight 708.67 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5183(17) _cell_length_b 7.3640(9) _cell_length_c 19.696(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.020(2) _cell_angle_gamma 90.00 _cell_volume 2079.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4770 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.29 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 4.583 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.643503 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11301 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.36 _reflns_number_total 4220 _reflns_number_gt 3369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^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 4220 _refine_ls_number_parameters 299 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.283 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.204092(17) 0.95957(3) 0.361520(12) 0.01880(8) Uani 1 1 d . . . Ag1 Ag 0.1131(6) 1.5175(10) 0.4768(8) 0.0505(17) Uani 0.38(3) 1 d P . 1 Ag1' Ag 0.1253(2) 1.4806(10) 0.5050(6) 0.0617(14) Uani 0.62(3) 1 d P . 2 O1 O 0.3008(3) 1.2239(4) 0.35961(18) 0.0272(9) Uani 1 1 d . . . O2 O 0.4018(3) 1.4296(5) 0.4115(2) 0.0379(10) Uani 1 1 d . . . O3 O 0.2612(3) 0.6284(5) 0.5558(2) 0.0448(11) Uani 1 1 d . . . O4 O 0.2044(3) 0.7470(4) 0.45445(18) 0.0292(9) Uani 1 1 d . . . O5 O 0.1355(3) 0.6889(4) 0.30512(18) 0.0279(9) Uani 1 1 d . . . O6 O 0.0211(3) 0.4827(5) 0.2836(2) 0.0429(11) Uani 1 1 d . . . O7 O 0.1333(3) 1.1707(5) 0.43163(19) 0.0303(9) Uani 1 1 d . . . O8 O 0.0072(3) 1.3009(5) 0.4614(2) 0.0453(12) Uani 1 1 d . . . O9 O 0.3377(2) 0.7607(4) 0.35728(18) 0.0282(9) Uani 1 1 d D . . H9A H 0.3324 0.6578 0.3757 0.034 Uiso 1 1 d RD . . H9B H 0.3474 0.7595 0.3157 0.034 Uiso 1 1 d RD . . O10 O 0.2522(2) 0.9515(4) 0.25084(16) 0.0270(8) Uani 1 1 d D . . H10A H 0.2788 1.0220 0.2263 0.032 Uiso 1 1 d RD . . H10B H 0.2320 0.8957 0.2141 0.032 Uiso 1 1 d RD . . O11 O 0.1056(3) 1.1568(4) 0.28148(19) 0.0314(9) Uani 1 1 d D . . H11A H 0.0689 1.0904 0.2537 0.038 Uiso 1 1 d RD . . H11B H 0.0814 1.2551 0.2937 0.038 Uiso 1 1 d RD . . N1 N 0.3195(3) 1.0183(5) 0.4686(2) 0.0224(9) Uani 1 1 d . . . N2 N 0.0376(3) 0.8973(5) 0.3729(2) 0.0221(10) Uani 1 1 d . . . C1 C 0.3568(4) 1.2858(6) 0.4099(3) 0.0248(12) Uani 1 1 d . . . C2 C 0.3722(4) 1.1680(6) 0.4734(3) 0.0233(12) Uani 1 1 d . . . C3 C 0.4348(4) 1.2091(7) 0.5324(3) 0.0341(14) Uani 1 1 d . . . H3 H 0.4706 1.3144 0.5348 0.041 Uiso 1 1 calc R . . C4 C 0.4427(4) 1.0905(8) 0.5874(3) 0.0425(16) Uani 1 1 d . . . H4 H 0.4840 1.1148 0.6274 0.051 Uiso 1 1 calc R . . C5 C 0.3885(4) 0.9353(8) 0.5823(3) 0.0381(15) Uani 1 1 d . . . H5 H 0.3930 0.8536 0.6187 0.046 Uiso 1 1 calc R . . C6 C 0.3277(4) 0.9039(7) 0.5223(3) 0.0254(12) Uani 1 1 d . . . C7 C 0.2615(4) 0.7479(7) 0.5107(3) 0.0273(13) Uani 1 1 d . . . C8 C 0.0542(4) 0.6295(7) 0.3075(3) 0.0282(13) Uani 1 1 d . . . C9 C -0.0065(4) 0.7503(7) 0.3444(3) 0.0261(12) Uani 1 1 d . . . C10 C -0.0988(4) 0.7162(8) 0.3478(3) 0.0396(16) Uani 1 1 d . . . H10 H -0.1275 0.6113 0.3284 0.048 Uiso 1 1 calc R . . C11 C -0.1482(4) 0.8411(8) 0.3805(4) 0.0498(18) Uani 1 1 d . . . H11 H -0.2108 0.8218 0.3834 0.060 Uiso 1 1 calc R . . C12 C -0.1031(4) 0.9938(7) 0.4086(3) 0.0409(16) Uani 1 1 d . . . H12 H -0.1348 1.0806 0.4303 0.049 Uiso 1 1 calc R . . C13 C -0.0104(4) 1.0162(6) 0.4042(3) 0.0259(12) Uani 1 1 d . . . C14 C 0.0473(4) 1.1751(7) 0.4346(3) 0.0290(13) Uani 1 1 d . . . O12 O 0.1971(3) 0.0377(6) 0.8089(2) 0.0571(13) Uani 1 1 d D . . H12A H 0.2381 0.0843 0.7873 0.069 Uiso 1 1 d RD . . H12B H 0.2080 0.0484 0.8526 0.069 Uiso 1 1 d RD . . O13 O 0.9916(3) 0.9557(7) 0.1967(2) 0.0702(15) Uani 1 1 d D . . H13A H 0.9329 0.9462 0.1942 0.084 Uiso 1 1 d RD . . H13B H 1.0119 1.0032 0.1621 0.084 Uiso 1 1 d RD . . O14 O 0.6612(3) 0.8211(7) 0.2534(3) 0.0841(18) Uani 1 1 d D . . H14A H 0.6062 0.8641 0.2459 0.101 Uiso 1 1 d RD . . H14B H 0.6701 0.7189 0.2769 0.101 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01898(13) 0.01658(12) 0.02126(13) -0.00120(11) 0.00450(9) -0.00201(11) Ag1 0.0490(17) 0.0335(14) 0.071(4) -0.0065(19) 0.0164(19) -0.0187(12) Ag1' 0.0534(8) 0.0430(13) 0.088(3) -0.0175(19) 0.0098(13) -0.0203(8) O1 0.032(2) 0.0250(19) 0.024(2) 0.0011(16) 0.0006(17) -0.0093(17) O2 0.047(3) 0.024(2) 0.040(2) 0.0066(17) -0.0014(19) -0.0172(19) O3 0.064(3) 0.034(2) 0.035(2) 0.0120(19) 0.003(2) -0.013(2) O4 0.037(2) 0.0240(19) 0.026(2) 0.0058(16) 0.0019(18) -0.0077(17) O5 0.023(2) 0.0255(19) 0.037(2) -0.0115(16) 0.0095(17) -0.0015(17) O6 0.031(2) 0.024(2) 0.075(3) -0.025(2) 0.014(2) -0.0064(18) O7 0.028(2) 0.0273(19) 0.038(2) -0.0102(17) 0.0098(18) -0.0051(17) O8 0.042(3) 0.032(2) 0.067(3) -0.027(2) 0.024(2) -0.004(2) O9 0.030(2) 0.0270(19) 0.028(2) 0.0019(16) 0.0067(18) 0.0036(17) O10 0.036(2) 0.0271(18) 0.0205(19) -0.0012(16) 0.0124(16) -0.0061(18) O11 0.030(2) 0.0233(18) 0.040(2) -0.0033(17) 0.0020(18) 0.0065(17) N1 0.025(2) 0.016(2) 0.027(2) 0.0024(18) 0.0064(19) 0.0009(19) N2 0.024(2) 0.020(2) 0.023(2) -0.0044(18) 0.0077(19) -0.0008(19) C1 0.027(3) 0.019(3) 0.028(3) 0.001(2) 0.004(3) -0.003(2) C2 0.023(3) 0.020(3) 0.027(3) -0.004(2) 0.005(2) -0.003(2) C3 0.037(4) 0.032(3) 0.032(3) 0.000(3) 0.001(3) -0.014(3) C4 0.047(4) 0.048(4) 0.028(3) 0.002(3) -0.011(3) -0.013(3) C5 0.042(4) 0.041(3) 0.029(3) 0.011(3) -0.002(3) -0.007(3) C6 0.025(3) 0.027(3) 0.025(3) -0.002(2) 0.005(2) -0.001(2) C7 0.032(3) 0.021(3) 0.031(3) 0.002(2) 0.011(3) 0.003(2) C8 0.025(3) 0.024(3) 0.036(3) -0.003(2) 0.006(3) 0.002(3) C9 0.024(3) 0.023(3) 0.033(3) -0.005(2) 0.009(2) -0.005(2) C10 0.033(4) 0.035(3) 0.054(4) -0.019(3) 0.015(3) -0.011(3) C11 0.024(4) 0.054(4) 0.076(5) -0.025(4) 0.019(3) -0.009(3) C12 0.031(3) 0.038(4) 0.059(4) -0.018(3) 0.023(3) -0.001(3) C13 0.026(3) 0.024(3) 0.030(3) -0.004(2) 0.011(2) -0.001(2) C14 0.033(4) 0.025(3) 0.031(3) -0.003(2) 0.012(3) -0.004(3) O12 0.044(3) 0.081(3) 0.047(3) -0.013(3) 0.007(2) -0.003(3) O13 0.042(3) 0.107(4) 0.063(3) -0.032(3) 0.013(2) -0.020(3) O14 0.044(3) 0.082(4) 0.127(5) 0.051(4) 0.014(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O10 2.392(3) . ? Dy1 O1 2.404(3) . ? Dy1 O4 2.408(3) . ? Dy1 O7 2.414(3) . ? Dy1 O5 2.419(3) . ? Dy1 O11 2.436(3) . ? Dy1 O9 2.443(3) . ? Dy1 N2 2.505(4) . ? Dy1 N1 2.516(4) . ? Ag1 O8 2.203(5) . ? Ag1 O4 2.234(7) 1_565 ? Ag1 O3 2.581(12) 1_565 ? Ag1' O8 2.229(5) . ? Ag1' O3 2.337(5) 1_565 ? Ag1' O4 2.552(11) 1_565 ? O1 C1 1.264(6) . ? O2 C1 1.243(6) . ? O3 C7 1.251(6) . ? O3 Ag1' 2.337(5) 1_545 ? O3 Ag1 2.581(12) 1_545 ? O4 C7 1.276(7) . ? O4 Ag1 2.234(7) 1_545 ? O4 Ag1' 2.552(11) 1_545 ? O5 C8 1.267(6) . ? O6 C8 1.245(6) . ? O7 C14 1.260(6) . ? O8 C14 1.254(6) . ? O9 H9A 0.8493 . ? O9 H9B 0.8522 . ? O10 H10A 0.8425 . ? O10 H10B 0.8434 . ? O11 H11A 0.8540 . ? O11 H11B 0.8552 . ? N1 C2 1.336(6) . ? N1 C6 1.344(6) . ? N2 C13 1.329(6) . ? N2 C9 1.336(6) . ? C1 C2 1.509(7) . ? C2 C3 1.392(7) . ? C3 C4 1.382(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(7) . ? C4 H4 0.9300 . ? C5 C6 1.378(8) . ? C5 H5 0.9300 . ? C6 C7 1.492(7) . ? C8 C9 1.517(7) . ? C9 C10 1.375(8) . ? C10 C11 1.387(8) . ? C10 H10 0.9300 . ? C11 C12 1.374(8) . ? C11 H11 0.9300 . ? C12 C13 1.371(8) . ? C12 H12 0.9300 . ? C13 C14 1.508(7) . ? O12 H12A 0.8549 . ? O12 H12B 0.8544 . ? O13 H13A 0.8477 . ? O13 H13B 0.8591 . ? O14 H14A 0.8495 . ? O14 H14B 0.8831 . ? 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 O10 Dy1 O1 75.60(11) . . ? O10 Dy1 O4 135.30(12) . . ? O1 Dy1 O4 127.37(12) . . ? O10 Dy1 O7 138.49(12) . . ? O1 Dy1 O7 77.85(12) . . ? O4 Dy1 O7 86.21(12) . . ? O10 Dy1 O5 73.67(12) . . ? O1 Dy1 O5 149.25(12) . . ? O4 Dy1 O5 76.40(12) . . ? O7 Dy1 O5 127.73(12) . . ? O10 Dy1 O11 69.56(12) . . ? O1 Dy1 O11 78.00(12) . . ? O4 Dy1 O11 144.12(13) . . ? O7 Dy1 O11 74.13(12) . . ? O5 Dy1 O11 92.10(12) . . ? O10 Dy1 O9 66.86(12) . . ? O1 Dy1 O9 90.92(12) . . ? O4 Dy1 O9 74.32(12) . . ? O7 Dy1 O9 144.84(13) . . ? O5 Dy1 O9 76.24(12) . . ? O11 Dy1 O9 136.41(12) . . ? O10 Dy1 N2 120.07(13) . . ? O1 Dy1 N2 136.36(12) . . ? O4 Dy1 N2 72.50(13) . . ? O7 Dy1 N2 64.07(12) . . ? O5 Dy1 N2 63.71(12) . . ? O11 Dy1 N2 71.95(13) . . ? O9 Dy1 N2 132.56(12) . . ? O10 Dy1 N1 121.11(13) . . ? O1 Dy1 N1 63.90(12) . . ? O4 Dy1 N1 63.48(12) . . ? O7 Dy1 N1 72.39(13) . . ? O5 Dy1 N1 134.30(12) . . ? O11 Dy1 N1 133.32(12) . . ? O9 Dy1 N1 72.75(12) . . ? N2 Dy1 N1 118.78(13) . . ? O8 Ag1 O4 160.6(9) . 1_565 ? O8 Ag1 O3 144.0(8) . 1_565 ? O4 Ag1 O3 54.22(19) 1_565 1_565 ? O8 Ag1' O3 171.3(5) . 1_565 ? O8 Ag1' O4 132.2(6) . 1_565 ? O3 Ag1' O4 53.69(17) 1_565 1_565 ? C1 O1 Dy1 125.8(3) . . ? C7 O3 Ag1' 96.9(5) . 1_545 ? C7 O3 Ag1 83.7(5) . 1_545 ? Ag1' O3 Ag1 13.28(9) 1_545 1_545 ? C7 O4 Ag1 99.1(5) . 1_545 ? C7 O4 Dy1 125.4(3) . . ? Ag1 O4 Dy1 135.4(5) 1_545 . ? C7 O4 Ag1' 86.4(4) . 1_545 ? Ag1 O4 Ag1' 12.7(2) 1_545 1_545 ? Dy1 O4 Ag1' 148.1(3) . 1_545 ? C8 O5 Dy1 125.9(3) . . ? C14 O7 Dy1 123.9(3) . . ? C14 O8 Ag1 103.5(4) . . ? C14 O8 Ag1' 102.8(4) . . ? Ag1 O8 Ag1' 16.03(12) . . ? Dy1 O9 H9A 113.2 . . ? Dy1 O9 H9B 106.9 . . ? H9A O9 H9B 116.2 . . ? Dy1 O10 H10A 137.1 . . ? Dy1 O10 H10B 133.0 . . ? H10A O10 H10B 86.4 . . ? Dy1 O11 H11A 108.4 . . ? Dy1 O11 H11B 123.2 . . ? H11A O11 H11B 115.0 . . ? C2 N1 C6 118.8(4) . . ? C2 N1 Dy1 120.0(3) . . ? C6 N1 Dy1 121.2(3) . . ? C13 N2 C9 118.4(4) . . ? C13 N2 Dy1 120.3(3) . . ? C9 N2 Dy1 121.1(3) . . ? O2 C1 O1 126.7(5) . . ? O2 C1 C2 117.4(5) . . ? O1 C1 C2 115.9(4) . . ? N1 C2 C3 122.1(5) . . ? N1 C2 C1 113.9(4) . . ? C3 C2 C1 124.0(5) . . ? C4 C3 C2 118.6(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.3(5) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 118.8(5) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 122.4(5) . . ? N1 C6 C7 112.7(5) . . ? C5 C6 C7 124.9(5) . . ? O3 C7 O4 122.6(5) . . ? O3 C7 C6 120.4(5) . . ? O4 C7 C6 116.9(4) . . ? O6 C8 O5 126.4(5) . . ? O6 C8 C9 118.1(5) . . ? O5 C8 C9 115.5(4) . . ? N2 C9 C10 122.3(5) . . ? N2 C9 C8 113.6(5) . . ? C10 C9 C8 124.0(5) . . ? C9 C10 C11 118.7(5) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 118.8(6) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 118.9(5) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N2 C13 C12 122.8(5) . . ? N2 C13 C14 113.3(4) . . ? C12 C13 C14 123.9(5) . . ? O8 C14 O7 124.5(5) . . ? O8 C14 C13 118.4(5) . . ? O7 C14 C13 117.1(5) . . ? H12A O12 H12B 115.6 . . ? H13A O13 H13B 117.0 . . ? H14A O14 H14B 117.7 . . ? 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 O10 Dy1 O1 C1 -142.7(4) . . . . ? O4 Dy1 O1 C1 -6.1(5) . . . . ? O7 Dy1 O1 C1 69.5(4) . . . . ? O5 Dy1 O1 C1 -140.9(4) . . . . ? O11 Dy1 O1 C1 145.6(4) . . . . ? O9 Dy1 O1 C1 -76.9(4) . . . . ? N2 Dy1 O1 C1 98.6(4) . . . . ? N1 Dy1 O1 C1 -6.7(4) . . . . ? O10 Dy1 O4 C7 103.7(4) . . . . ? O1 Dy1 O4 C7 -5.3(5) . . . . ? O7 Dy1 O4 C7 -76.9(4) . . . . ? O5 Dy1 O4 C7 152.8(4) . . . . ? O11 Dy1 O4 C7 -132.9(4) . . . . ? O9 Dy1 O4 C7 73.5(4) . . . . ? N2 Dy1 O4 C7 -140.9(4) . . . . ? N1 Dy1 O4 C7 -4.7(4) . . . . ? O10 Dy1 O4 Ag1 -80.9(3) . . . 1_545 ? O1 Dy1 O4 Ag1 170.0(2) . . . 1_545 ? O7 Dy1 O4 Ag1 98.4(3) . . . 1_545 ? O5 Dy1 O4 Ag1 -31.9(3) . . . 1_545 ? O11 Dy1 O4 Ag1 42.4(4) . . . 1_545 ? O9 Dy1 O4 Ag1 -111.2(3) . . . 1_545 ? N2 Dy1 O4 Ag1 34.4(3) . . . 1_545 ? N1 Dy1 O4 Ag1 170.6(3) . . . 1_545 ? O10 Dy1 O4 Ag1' -81.7(4) . . . 1_545 ? O1 Dy1 O4 Ag1' 169.2(3) . . . 1_545 ? O7 Dy1 O4 Ag1' 97.7(3) . . . 1_545 ? O5 Dy1 O4 Ag1' -32.7(3) . . . 1_545 ? O11 Dy1 O4 Ag1' 41.7(4) . . . 1_545 ? O9 Dy1 O4 Ag1' -111.9(3) . . . 1_545 ? N2 Dy1 O4 Ag1' 33.7(3) . . . 1_545 ? N1 Dy1 O4 Ag1' 169.8(4) . . . 1_545 ? O10 Dy1 O5 C8 -140.1(4) . . . . ? O1 Dy1 O5 C8 -142.0(4) . . . . ? O4 Dy1 O5 C8 73.5(4) . . . . ? O7 Dy1 O5 C8 -0.7(5) . . . . ? O11 Dy1 O5 C8 -72.2(4) . . . . ? O9 Dy1 O5 C8 150.3(4) . . . . ? N2 Dy1 O5 C8 -3.5(4) . . . . ? N1 Dy1 O5 C8 102.1(4) . . . . ? O10 Dy1 O7 C14 96.1(4) . . . . ? O1 Dy1 O7 C14 147.3(4) . . . . ? O4 Dy1 O7 C14 -83.2(4) . . . . ? O5 Dy1 O7 C14 -13.6(5) . . . . ? O11 Dy1 O7 C14 66.5(4) . . . . ? O9 Dy1 O7 C14 -138.8(4) . . . . ? N2 Dy1 O7 C14 -10.8(4) . . . . ? N1 Dy1 O7 C14 -146.5(4) . . . . ? O4 Ag1 O8 C14 76.9(12) 1_565 . . . ? O3 Ag1 O8 C14 -80.0(6) 1_565 . . . ? O4 Ag1 O8 Ag1' 166.3(16) 1_565 . . . ? O3 Ag1 O8 Ag1' 9.4(5) 1_565 . . . ? O3 Ag1' O8 C14 -41(4) 1_565 . . . ? O4 Ag1' O8 C14 89.1(4) 1_565 . . . ? O3 Ag1' O8 Ag1 -136(4) 1_565 . . . ? O4 Ag1' O8 Ag1 -5.3(6) 1_565 . . . ? O10 Dy1 N1 C2 55.6(4) . . . . ? O1 Dy1 N1 C2 3.9(3) . . . . ? O4 Dy1 N1 C2 -175.6(4) . . . . ? O7 Dy1 N1 C2 -80.9(3) . . . . ? O5 Dy1 N1 C2 153.1(3) . . . . ? O11 Dy1 N1 C2 -34.8(4) . . . . ? O9 Dy1 N1 C2 103.7(4) . . . . ? N2 Dy1 N1 C2 -126.7(3) . . . . ? O10 Dy1 N1 C6 -126.2(3) . . . . ? O1 Dy1 N1 C6 -178.0(4) . . . . ? O4 Dy1 N1 C6 2.6(3) . . . . ? O7 Dy1 N1 C6 97.2(4) . . . . ? O5 Dy1 N1 C6 -28.7(4) . . . . ? O11 Dy1 N1 C6 143.3(3) . . . . ? O9 Dy1 N1 C6 -78.1(4) . . . . ? N2 Dy1 N1 C6 51.5(4) . . . . ? O10 Dy1 N2 C13 -125.6(4) . . . . ? O1 Dy1 N2 C13 -24.6(5) . . . . ? O4 Dy1 N2 C13 101.7(4) . . . . ? O7 Dy1 N2 C13 7.3(4) . . . . ? O5 Dy1 N2 C13 -175.2(4) . . . . ? O11 Dy1 N2 C13 -73.4(4) . . . . ? O9 Dy1 N2 C13 149.3(3) . . . . ? N1 Dy1 N2 C13 56.7(4) . . . . ? O10 Dy1 N2 C9 50.4(4) . . . . ? O1 Dy1 N2 C9 151.4(3) . . . . ? O4 Dy1 N2 C9 -82.4(4) . . . . ? O7 Dy1 N2 C9 -176.7(4) . . . . ? O5 Dy1 N2 C9 0.8(4) . . . . ? O11 Dy1 N2 C9 102.5(4) . . . . ? O9 Dy1 N2 C9 -34.8(4) . . . . ? N1 Dy1 N2 C9 -127.3(4) . . . . ? Dy1 O1 C1 O2 -173.9(4) . . . . ? Dy1 O1 C1 C2 8.3(6) . . . . ? C6 N1 C2 C3 -0.3(7) . . . . ? Dy1 N1 C2 C3 177.9(4) . . . . ? C6 N1 C2 C1 -179.9(4) . . . . ? Dy1 N1 C2 C1 -1.7(5) . . . . ? O2 C1 C2 N1 178.2(5) . . . . ? O1 C1 C2 N1 -3.8(7) . . . . ? O2 C1 C2 C3 -1.4(8) . . . . ? O1 C1 C2 C3 176.6(5) . . . . ? N1 C2 C3 C4 0.3(8) . . . . ? C1 C2 C3 C4 179.9(5) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C3 C4 C5 C6 -0.2(9) . . . . ? C2 N1 C6 C5 0.0(7) . . . . ? Dy1 N1 C6 C5 -178.2(4) . . . . ? C2 N1 C6 C7 177.3(4) . . . . ? Dy1 N1 C6 C7 -0.9(5) . . . . ? C4 C5 C6 N1 0.3(9) . . . . ? C4 C5 C6 C7 -176.7(5) . . . . ? Ag1' O3 C7 O4 -7.2(6) 1_545 . . . ? Ag1 O3 C7 O4 -6.1(5) 1_545 . . . ? Ag1' O3 C7 C6 170.3(4) 1_545 . . . ? Ag1 O3 C7 C6 171.4(5) 1_545 . . . ? Ag1 O4 C7 O3 7.1(6) 1_545 . . . ? Dy1 O4 C7 O3 -176.3(4) . . . . ? Ag1' O4 C7 O3 6.6(5) 1_545 . . . ? Ag1 O4 C7 C6 -170.5(4) 1_545 . . . ? Dy1 O4 C7 C6 6.1(6) . . . . ? Ag1' O4 C7 C6 -171.0(4) 1_545 . . . ? N1 C6 C7 O3 179.3(5) . . . . ? C5 C6 C7 O3 -3.5(8) . . . . ? N1 C6 C7 O4 -3.1(7) . . . . ? C5 C6 C7 O4 174.1(5) . . . . ? Dy1 O5 C8 O6 -173.5(4) . . . . ? Dy1 O5 C8 C9 5.4(7) . . . . ? C13 N2 C9 C10 -1.6(8) . . . . ? Dy1 N2 C9 C10 -177.6(4) . . . . ? C13 N2 C9 C8 177.3(5) . . . . ? Dy1 N2 C9 C8 1.2(6) . . . . ? O6 C8 C9 N2 174.9(5) . . . . ? O5 C8 C9 N2 -4.0(7) . . . . ? O6 C8 C9 C10 -6.3(9) . . . . ? O5 C8 C9 C10 174.8(5) . . . . ? N2 C9 C10 C11 1.5(9) . . . . ? C8 C9 C10 C11 -177.2(6) . . . . ? C9 C10 C11 C12 -0.2(10) . . . . ? C10 C11 C12 C13 -0.9(10) . . . . ? C9 N2 C13 C12 0.3(8) . . . . ? Dy1 N2 C13 C12 176.4(4) . . . . ? C9 N2 C13 C14 179.6(4) . . . . ? Dy1 N2 C13 C14 -4.3(6) . . . . ? C11 C12 C13 N2 0.9(9) . . . . ? C11 C12 C13 C14 -178.3(6) . . . . ? Ag1 O8 C14 O7 12.2(8) . . . . ? Ag1' O8 C14 O7 -4.2(8) . . . . ? Ag1 O8 C14 C13 -168.4(6) . . . . ? Ag1' O8 C14 C13 175.1(5) . . . . ? Dy1 O7 C14 O8 -167.7(4) . . . . ? Dy1 O7 C14 C13 12.9(7) . . . . ? N2 C13 C14 O8 175.5(5) . . . . ? C12 C13 C14 O8 -5.2(8) . . . . ? N2 C13 C14 O7 -5.0(7) . . . . ? C12 C13 C14 O7 174.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.169 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.136 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 640103' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag N2 O14 Tb' _chemical_formula_sum 'C14 H18 Ag N2 O14 Tb' _chemical_formula_weight 705.09 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4474(17) _cell_length_b 7.3600(8) _cell_length_c 19.480(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.416(6) _cell_angle_gamma 90.00 _cell_volume 2049.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6408 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 4.456 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6642 _exptl_absorpt_correction_T_max 0.8419 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18211 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4869 _reflns_number_gt 4149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0448P)^2^+0.2644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4869 _refine_ls_number_parameters 335 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0765 _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 Tb1 Tb 0.793676(12) 0.54690(3) 0.137617(9) 0.00825(7) Uani 1 1 d . . . Ag1 Ag 0.87356(14) 0.0217(6) -0.0098(4) 0.0239(6) Uani 0.61(2) 1 d P . . Ag1' Ag 0.8815(4) -0.0058(9) 0.0139(8) 0.0275(14) Uani 0.39(2) 1 d P . . N1 N 0.9620(2) 0.6068(5) 0.12514(16) 0.0104(7) Uani 1 1 d . . . N2 N 0.6770(2) 0.4868(5) 0.02956(17) 0.0101(7) Uani 1 1 d . . . O1 O 0.86497(19) 0.3328(4) 0.06659(14) 0.0137(6) Uani 1 1 d . . . O2 O 0.9917(2) 0.2006(4) 0.03590(16) 0.0205(7) Uani 1 1 d . . . O3 O 0.86367(18) 0.8214(4) 0.19204(14) 0.0117(6) Uani 1 1 d . . . O4 O 0.9798(2) 1.0254(4) 0.21296(16) 0.0188(7) Uani 1 1 d . . . O5 O 0.69513(19) 0.2835(4) 0.13984(13) 0.0128(6) Uani 1 1 d . . . O6 O 0.5942(2) 0.0750(4) 0.08835(15) 0.0158(6) Uani 1 1 d . . . O7 O 0.79321(19) 0.7581(4) 0.04319(14) 0.0140(6) Uani 1 1 d . . . O8 O 0.7369(2) 0.8777(4) -0.05919(15) 0.0187(7) Uani 1 1 d . . . C1 C 0.9517(3) 0.3260(6) 0.0635(2) 0.0154(8) Uani 1 1 d . . . C2 C 1.0100(3) 0.4836(6) 0.0942(2) 0.0132(8) Uani 1 1 d . . . C3 C 1.1046(3) 0.5015(6) 0.0908(2) 0.0192(9) Uani 1 1 d . . . H3 H 1.1373 0.4099 0.0698 0.023 Uiso 1 1 calc R . . C4 C 1.1507(3) 0.6566(7) 0.1188(2) 0.0241(10) Uani 1 1 d . . . H4 H 1.2153 0.6741 0.1166 0.029 Uiso 1 1 calc R . . C5 C 1.1002(3) 0.7855(6) 0.1502(2) 0.0187(9) Uani 1 1 d . . . H5 H 1.1297 0.8934 0.1692 0.022 Uiso 1 1 calc R . . C6 C 1.0069(3) 0.7547(6) 0.1533(2) 0.0132(8) Uani 1 1 d . . . C7 C 0.9458(3) 0.8793(6) 0.1891(2) 0.0127(8) Uani 1 1 d . . . C8 C 0.6386(3) 0.2200(6) 0.0893(2) 0.0125(8) Uani 1 1 d . . . C9 C 0.6243(3) 0.3368(5) 0.0249(2) 0.0111(8) Uani 1 1 d . . . C10 C 0.5615(3) 0.2942(6) -0.0345(2) 0.0148(8) Uani 1 1 d . . . H10 H 0.5251 0.1864 -0.0367 0.018 Uiso 1 1 calc R . . C11 C 0.5539(3) 0.4138(6) -0.0901(2) 0.0170(9) Uani 1 1 d . . . H11 H 0.5113 0.3891 -0.1310 0.020 Uiso 1 1 calc R . . C12 C 0.6085(3) 0.5691(6) -0.0859(2) 0.0165(9) Uani 1 1 d . . . H12 H 0.6045 0.6517 -0.1237 0.020 Uiso 1 1 calc R . . C13 C 0.6696(3) 0.6013(6) -0.0245(2) 0.0119(8) Uani 1 1 d . . . C14 C 0.7362(3) 0.7582(5) -0.0133(2) 0.0126(8) Uani 1 1 d . . . O9 O 0.8924(2) 0.3479(4) 0.21824(15) 0.0141(6) Uani 1 1 d D . . H9A H 0.936(3) 0.412(6) 0.242(2) 0.021 Uiso 1 1 d D . . H9B H 0.923(3) 0.247(5) 0.208(2) 0.021 Uiso 1 1 d D . . O10 O 0.7475(2) 0.5565(4) 0.25052(14) 0.0120(6) Uani 1 1 d D . . H10A H 0.710(3) 0.485(6) 0.266(2) 0.018 Uiso 1 1 d D . . H10B H 0.768(3) 0.629(6) 0.280(2) 0.018 Uiso 1 1 d D . . O11 O 0.6602(2) 0.7472(4) 0.14376(15) 0.0135(6) Uani 1 1 d D . . H11A H 0.651(3) 0.847(5) 0.125(2) 0.020 Uiso 1 1 d D . . H11B H 0.658(3) 0.767(7) 0.1865(15) 0.020 Uiso 1 1 d D . . O12 O 0.4947(2) 0.0689(5) 0.20344(17) 0.0248(8) Uani 1 1 d D . . H12A H 0.436(2) 0.062(8) 0.199(3) 0.037 Uiso 1 1 d D . . H12B H 0.507(4) 0.069(7) 0.1606(17) 0.037 Uiso 1 1 d D . . O13 O 0.3057(2) 0.0224(5) 0.19463(17) 0.0215(7) Uani 1 1 d D . . H13A H 0.262(3) 0.044(7) 0.218(3) 0.032 Uiso 1 1 d D . . H13B H 0.293(4) 0.038(8) 0.1505(15) 0.032 Uiso 1 1 d D . . O14 O 0.3352(2) 0.6613(5) 0.2414(2) 0.0316(9) Uani 1 1 d D . . H14A H 0.394(2) 0.641(9) 0.247(3) 0.047 Uiso 1 1 d D . . H14B H 0.332(4) 0.778(4) 0.235(3) 0.047 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.00726(10) 0.00747(11) 0.01023(10) -0.00027(7) 0.00199(6) -0.00059(7) Ag1 0.0184(4) 0.0166(6) 0.0364(15) -0.0065(8) 0.0030(6) -0.0070(3) Ag1' 0.0190(8) 0.0156(11) 0.050(4) -0.0114(16) 0.0115(14) -0.0081(7) N1 0.0103(16) 0.0087(16) 0.0129(16) -0.0004(13) 0.0042(12) 0.0007(13) N2 0.0070(15) 0.0120(17) 0.0119(16) 0.0012(13) 0.0033(12) -0.0003(13) O1 0.0105(14) 0.0137(15) 0.0178(14) -0.0039(11) 0.0051(11) -0.0019(11) O2 0.0164(16) 0.0150(16) 0.0327(17) -0.0117(13) 0.0119(13) -0.0012(13) O3 0.0077(13) 0.0116(14) 0.0164(13) -0.0028(11) 0.0041(10) -0.0009(11) O4 0.0134(15) 0.0127(16) 0.0306(17) -0.0077(13) 0.0041(12) -0.0014(12) O5 0.0131(14) 0.0138(15) 0.0114(13) 0.0004(11) 0.0012(10) -0.0017(11) O6 0.0164(15) 0.0118(15) 0.0185(14) 0.0017(11) 0.0003(11) -0.0046(11) O7 0.0133(14) 0.0138(15) 0.0147(14) 0.0009(11) 0.0013(11) -0.0038(11) O8 0.0218(16) 0.0155(16) 0.0182(15) 0.0056(13) 0.0009(12) -0.0062(13) C1 0.018(2) 0.013(2) 0.0155(19) 0.0001(16) 0.0061(16) -0.0006(17) C2 0.0114(19) 0.016(2) 0.0140(19) -0.0047(16) 0.0062(14) -0.0008(15) C3 0.016(2) 0.018(2) 0.025(2) -0.0080(18) 0.0071(17) 0.0034(17) C4 0.010(2) 0.030(3) 0.033(3) -0.009(2) 0.0067(17) -0.0043(19) C5 0.013(2) 0.017(2) 0.026(2) -0.0076(18) 0.0051(16) -0.0071(17) C6 0.0113(19) 0.014(2) 0.0145(19) -0.0011(16) 0.0037(14) -0.0014(16) C7 0.0104(19) 0.011(2) 0.0169(19) -0.0032(16) 0.0005(14) -0.0017(15) C8 0.012(2) 0.011(2) 0.0142(19) 0.0031(15) 0.0040(15) 0.0014(15) C9 0.0079(18) 0.0099(19) 0.0153(19) 0.0001(15) 0.0015(14) 0.0019(15) C10 0.013(2) 0.013(2) 0.018(2) -0.0003(16) 0.0015(15) -0.0023(16) C11 0.014(2) 0.021(2) 0.015(2) 0.0010(16) -0.0020(15) -0.0055(17) C12 0.016(2) 0.019(2) 0.0143(19) 0.0022(16) 0.0020(15) 0.0000(17) C13 0.0135(19) 0.010(2) 0.0123(18) -0.0016(15) 0.0031(14) 0.0002(15) C14 0.013(2) 0.011(2) 0.0149(19) -0.0014(15) 0.0050(15) 0.0028(16) O9 0.0118(15) 0.0117(15) 0.0183(14) -0.0003(12) 0.0003(11) 0.0008(11) O10 0.0126(14) 0.0132(15) 0.0112(13) -0.0019(11) 0.0047(10) -0.0036(11) O11 0.0131(15) 0.0119(16) 0.0151(14) 0.0010(12) 0.0007(11) 0.0032(12) O12 0.0167(16) 0.035(2) 0.0220(16) 0.0102(14) 0.0005(13) 0.0026(15) O13 0.0163(16) 0.0281(19) 0.0200(16) 0.0047(14) 0.0028(12) 0.0004(14) O14 0.0146(16) 0.028(2) 0.051(2) 0.0167(18) 0.0019(15) 0.0004(15) _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 Tb1 O10 2.391(3) . ? Tb1 O7 2.408(3) . ? Tb1 O5 2.409(3) . ? Tb1 O1 2.424(3) . ? Tb1 O3 2.432(3) . ? Tb1 O11 2.444(3) . ? Tb1 O9 2.447(3) . ? Tb1 N1 2.518(3) . ? Tb1 N2 2.536(3) . ? Ag1 Ag1' 0.503(9) . ? Ag1 O2 2.235(3) . ? Ag1 O8 2.321(4) 1_545 ? Ag1 O7 2.556(7) 1_545 ? Ag1' O2 2.197(4) . ? Ag1' O7 2.277(8) 1_545 ? Ag1' O8 2.501(10) 1_545 ? N1 C2 1.338(5) . ? N1 C6 1.343(5) . ? N2 C9 1.336(5) . ? N2 C13 1.340(5) . ? O1 C1 1.264(5) . ? O2 C1 1.251(5) . ? O3 C7 1.270(5) . ? O4 C7 1.243(5) . ? O5 C8 1.272(4) . ? O6 C8 1.244(5) . ? O7 C14 1.275(4) . ? O7 Ag1' 2.277(8) 1_565 ? O7 Ag1 2.556(7) 1_565 ? O8 C14 1.255(5) . ? O8 Ag1 2.321(4) 1_565 ? O8 Ag1' 2.501(10) 1_565 ? C1 C2 1.505(6) . ? C2 C3 1.384(6) . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C6 1.376(6) . ? C5 H5 0.9500 . ? C6 C7 1.513(6) . ? C8 C9 1.510(5) . ? C9 C10 1.397(5) . ? C10 C11 1.387(6) . ? C10 H10 0.9500 . ? C11 C12 1.384(6) . ? C11 H11 0.9500 . ? C12 C13 1.399(5) . ? C12 H12 0.9500 . ? C13 C14 1.499(6) . ? O9 H9A 0.87(3) . ? O9 H9B 0.90(3) . ? O10 H10A 0.84(3) . ? O10 H10B 0.81(3) . ? O11 H11A 0.82(3) . ? O11 H11B 0.85(3) . ? O12 H12A 0.85(3) . ? O12 H12B 0.88(3) . ? O13 H13A 0.85(3) . ? O13 H13B 0.86(3) . ? O14 H14A 0.85(3) . ? O14 H14B 0.87(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Tb1 O7 135.54(10) . . ? O10 Tb1 O5 76.23(9) . . ? O7 Tb1 O5 126.70(9) . . ? O10 Tb1 O1 138.02(10) . . ? O7 Tb1 O1 86.42(10) . . ? O5 Tb1 O1 77.80(10) . . ? O10 Tb1 O3 74.27(9) . . ? O7 Tb1 O3 75.59(9) . . ? O5 Tb1 O3 150.42(9) . . ? O1 Tb1 O3 127.20(9) . . ? O10 Tb1 O11 66.96(10) . . ? O7 Tb1 O11 74.57(10) . . ? O5 Tb1 O11 90.69(10) . . ? O1 Tb1 O11 145.52(9) . . ? O3 Tb1 O11 76.01(9) . . ? O10 Tb1 O9 69.04(10) . . ? O7 Tb1 O9 144.39(10) . . ? O5 Tb1 O9 78.29(9) . . ? O1 Tb1 O9 73.79(9) . . ? O3 Tb1 O9 92.95(9) . . ? O11 Tb1 O9 136.00(10) . . ? O10 Tb1 N1 119.16(10) . . ? O7 Tb1 N1 73.02(10) . . ? O5 Tb1 N1 136.41(10) . . ? O1 Tb1 N1 64.01(10) . . ? O3 Tb1 N1 63.30(10) . . ? O11 Tb1 N1 132.77(10) . . ? O9 Tb1 N1 71.74(10) . . ? O10 Tb1 N2 121.83(10) . . ? O7 Tb1 N2 63.34(10) . . ? O5 Tb1 N2 63.37(10) . . ? O1 Tb1 N2 72.50(10) . . ? O3 Tb1 N2 133.65(10) . . ? O11 Tb1 N2 73.29(10) . . ? O9 Tb1 N2 133.03(10) . . ? N1 Tb1 N2 118.99(10) . . ? Ag1' Ag1 O2 79.2(5) . . ? Ag1' Ag1 O8 105.2(7) . 1_545 ? O2 Ag1 O8 171.0(2) . 1_545 ? Ag1' Ag1 O7 51.5(6) . 1_545 ? O2 Ag1 O7 130.7(4) . 1_545 ? O8 Ag1 O7 53.96(12) 1_545 1_545 ? Ag1 Ag1' O2 87.8(5) . . ? Ag1 Ag1' O7 118.5(8) . 1_545 ? O2 Ag1' O7 153.5(9) . 1_545 ? Ag1 Ag1' O8 63.6(8) . 1_545 ? O2 Ag1' O8 150.4(8) . 1_545 ? O7 Ag1' O8 55.20(12) 1_545 1_545 ? C2 N1 C6 118.8(3) . . ? C2 N1 Tb1 119.8(3) . . ? C6 N1 Tb1 121.2(3) . . ? C9 N2 C13 119.1(3) . . ? C9 N2 Tb1 120.2(2) . . ? C13 N2 Tb1 120.6(3) . . ? C1 O1 Tb1 124.0(3) . . ? C1 O2 Ag1' 103.1(3) . . ? C1 O2 Ag1 103.4(3) . . ? Ag1' O2 Ag1 13.0(2) . . ? C7 O3 Tb1 126.2(3) . . ? C8 O5 Tb1 126.6(2) . . ? C14 O7 Ag1' 95.6(5) . 1_565 ? C14 O7 Tb1 126.1(3) . . ? Ag1' O7 Tb1 138.2(4) 1_565 . ? C14 O7 Ag1 85.7(3) . 1_565 ? Ag1' O7 Ag1 10.0(3) 1_565 1_565 ? Tb1 O7 Ag1 148.05(18) . 1_565 ? C14 O8 Ag1 96.9(3) . 1_565 ? C14 O8 Ag1' 85.9(4) . 1_565 ? Ag1 O8 Ag1' 11.19(15) 1_565 1_565 ? O2 C1 O1 124.9(4) . . ? O2 C1 C2 118.2(4) . . ? O1 C1 C2 116.8(4) . . ? N1 C2 C3 122.5(4) . . ? N1 C2 C1 113.9(3) . . ? C3 C2 C1 123.6(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.6(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C6 C5 C4 119.1(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 122.3(4) . . ? N1 C6 C7 113.6(3) . . ? C5 C6 C7 124.2(4) . . ? O4 C7 O3 126.4(4) . . ? O4 C7 C6 118.1(4) . . ? O3 C7 C6 115.5(3) . . ? O6 C8 O5 126.7(4) . . ? O6 C8 C9 117.9(3) . . ? O5 C8 C9 115.4(3) . . ? N2 C9 C10 122.4(4) . . ? N2 C9 C8 114.0(3) . . ? C10 C9 C8 123.7(4) . . ? C11 C10 C9 118.2(4) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.2(4) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? N2 C13 C12 122.2(4) . . ? N2 C13 C14 113.3(3) . . ? C12 C13 C14 124.4(4) . . ? O8 C14 O7 122.9(4) . . ? O8 C14 C13 120.6(3) . . ? O7 C14 C13 116.4(3) . . ? Tb1 O9 H9A 109(3) . . ? Tb1 O9 H9B 128(3) . . ? H9A O9 H9B 103(4) . . ? Tb1 O10 H10A 126(3) . . ? Tb1 O10 H10B 123(4) . . ? H10A O10 H10B 111(5) . . ? Tb1 O11 H11A 127(4) . . ? Tb1 O11 H11B 107(3) . . ? H11A O11 H11B 105(5) . . ? H12A O12 H12B 104(5) . . ? H13A O13 H13B 117(5) . . ? H14A O14 H14B 102(6) . . ? 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 O8 Ag1 Ag1' O2 -171.89(18) 1_545 . . . ? O7 Ag1 Ag1' O2 -177.5(4) 1_545 . . . ? O2 Ag1 Ag1' O7 177.5(4) . . . 1_545 ? O8 Ag1 Ag1' O7 5.7(6) 1_545 . . 1_545 ? O2 Ag1 Ag1' O8 171.89(18) . . . 1_545 ? O7 Ag1 Ag1' O8 -5.7(6) 1_545 . . 1_545 ? O10 Tb1 N1 C2 124.1(3) . . . . ? O7 Tb1 N1 C2 -102.7(3) . . . . ? O5 Tb1 N1 C2 23.2(3) . . . . ? O1 Tb1 N1 C2 -8.3(3) . . . . ? O3 Tb1 N1 C2 175.2(3) . . . . ? O11 Tb1 N1 C2 -151.3(3) . . . . ? O9 Tb1 N1 C2 72.1(3) . . . . ? N2 Tb1 N1 C2 -57.6(3) . . . . ? O10 Tb1 N1 C6 -51.1(3) . . . . ? O7 Tb1 N1 C6 82.1(3) . . . . ? O5 Tb1 N1 C6 -152.1(3) . . . . ? O1 Tb1 N1 C6 176.5(3) . . . . ? O3 Tb1 N1 C6 0.0(3) . . . . ? O11 Tb1 N1 C6 33.5(3) . . . . ? O9 Tb1 N1 C6 -103.1(3) . . . . ? N2 Tb1 N1 C6 127.2(3) . . . . ? O10 Tb1 N2 C9 -55.9(3) . . . . ? O7 Tb1 N2 C9 175.1(3) . . . . ? O5 Tb1 N2 C9 -4.6(3) . . . . ? O1 Tb1 N2 C9 80.3(3) . . . . ? O3 Tb1 N2 C9 -154.6(3) . . . . ? O11 Tb1 N2 C9 -104.1(3) . . . . ? O9 Tb1 N2 C9 34.3(3) . . . . ? N1 Tb1 N2 C9 125.8(3) . . . . ? O10 Tb1 N2 C13 126.4(3) . . . . ? O7 Tb1 N2 C13 -2.5(3) . . . . ? O5 Tb1 N2 C13 177.8(3) . . . . ? O1 Tb1 N2 C13 -97.4(3) . . . . ? O3 Tb1 N2 C13 27.8(4) . . . . ? O11 Tb1 N2 C13 78.3(3) . . . . ? O9 Tb1 N2 C13 -143.4(3) . . . . ? N1 Tb1 N2 C13 -51.8(3) . . . . ? O10 Tb1 O1 C1 -94.2(3) . . . . ? O7 Tb1 O1 C1 84.2(3) . . . . ? O5 Tb1 O1 C1 -147.0(3) . . . . ? O3 Tb1 O1 C1 15.3(3) . . . . ? O11 Tb1 O1 C1 140.0(3) . . . . ? O9 Tb1 O1 C1 -65.9(3) . . . . ? N1 Tb1 O1 C1 11.4(3) . . . . ? N2 Tb1 O1 C1 147.3(3) . . . . ? Ag1 Ag1' O2 C1 92.9(6) . . . . ? O7 Ag1' O2 C1 -82.2(6) 1_545 . . . ? O8 Ag1' O2 C1 78.1(6) 1_545 . . . ? O7 Ag1' O2 Ag1 -175.2(9) 1_545 . . . ? O8 Ag1' O2 Ag1 -14.8(6) 1_545 . . . ? Ag1' Ag1 O2 C1 -90.2(6) . . . . ? O8 Ag1 O2 C1 30(3) 1_545 . . . ? O7 Ag1 O2 C1 -87.6(3) 1_545 . . . ? O8 Ag1 O2 Ag1' 120(3) 1_545 . . . ? O7 Ag1 O2 Ag1' 2.5(5) 1_545 . . . ? O10 Tb1 O3 C7 138.3(3) . . . . ? O7 Tb1 O3 C7 -74.8(3) . . . . ? O5 Tb1 O3 C7 142.3(3) . . . . ? O1 Tb1 O3 C7 -0.8(4) . . . . ? O11 Tb1 O3 C7 -152.1(3) . . . . ? O9 Tb1 O3 C7 71.1(3) . . . . ? N1 Tb1 O3 C7 3.2(3) . . . . ? N2 Tb1 O3 C7 -102.5(3) . . . . ? O10 Tb1 O5 C8 143.9(3) . . . . ? O7 Tb1 O5 C8 6.7(4) . . . . ? O1 Tb1 O5 C8 -69.4(3) . . . . ? O3 Tb1 O5 C8 139.9(3) . . . . ? O11 Tb1 O5 C8 77.8(3) . . . . ? O9 Tb1 O5 C8 -145.1(3) . . . . ? N1 Tb1 O5 C8 -98.1(3) . . . . ? N2 Tb1 O5 C8 7.0(3) . . . . ? O10 Tb1 O7 C14 -104.5(3) . . . . ? O5 Tb1 O7 C14 5.1(4) . . . . ? O1 Tb1 O7 C14 77.0(3) . . . . ? O3 Tb1 O7 C14 -153.1(3) . . . . ? O11 Tb1 O7 C14 -73.9(3) . . . . ? O9 Tb1 O7 C14 132.4(3) . . . . ? N1 Tb1 O7 C14 140.9(3) . . . . ? N2 Tb1 O7 C14 4.8(3) . . . . ? O10 Tb1 O7 Ag1' 79.9(3) . . . 1_565 ? O5 Tb1 O7 Ag1' -170.5(2) . . . 1_565 ? O1 Tb1 O7 Ag1' -98.6(2) . . . 1_565 ? O3 Tb1 O7 Ag1' 31.3(2) . . . 1_565 ? O11 Tb1 O7 Ag1' 110.5(2) . . . 1_565 ? O9 Tb1 O7 Ag1' -43.2(3) . . . 1_565 ? N1 Tb1 O7 Ag1' -34.7(2) . . . 1_565 ? N2 Tb1 O7 Ag1' -170.8(3) . . . 1_565 ? O10 Tb1 O7 Ag1 82.0(3) . . . 1_565 ? O5 Tb1 O7 Ag1 -168.4(2) . . . 1_565 ? O1 Tb1 O7 Ag1 -96.5(3) . . . 1_565 ? O3 Tb1 O7 Ag1 33.4(2) . . . 1_565 ? O11 Tb1 O7 Ag1 112.6(3) . . . 1_565 ? O9 Tb1 O7 Ag1 -41.1(4) . . . 1_565 ? N1 Tb1 O7 Ag1 -32.6(3) . . . 1_565 ? N2 Tb1 O7 Ag1 -168.7(3) . . . 1_565 ? Ag1' O2 C1 O1 -9.1(7) . . . . ? Ag1 O2 C1 O1 4.2(5) . . . . ? Ag1' O2 C1 C2 172.4(5) . . . . ? Ag1 O2 C1 C2 -174.3(4) . . . . ? Tb1 O1 C1 O2 168.5(3) . . . . ? Tb1 O1 C1 C2 -12.9(5) . . . . ? C6 N1 C2 C3 0.8(6) . . . . ? Tb1 N1 C2 C3 -174.6(3) . . . . ? C6 N1 C2 C1 -178.9(3) . . . . ? Tb1 N1 C2 C1 5.7(4) . . . . ? O2 C1 C2 N1 -177.3(4) . . . . ? O1 C1 C2 N1 4.1(5) . . . . ? O2 C1 C2 C3 3.0(6) . . . . ? O1 C1 C2 C3 -175.6(4) . . . . ? N1 C2 C3 C4 -2.0(7) . . . . ? C1 C2 C3 C4 177.7(4) . . . . ? C2 C3 C4 C5 1.2(7) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C2 N1 C6 C5 1.4(6) . . . . ? Tb1 N1 C6 C5 176.6(3) . . . . ? C2 N1 C6 C7 -177.7(3) . . . . ? Tb1 N1 C6 C7 -2.4(4) . . . . ? C4 C5 C6 N1 -2.2(7) . . . . ? C4 C5 C6 C7 176.8(4) . . . . ? Tb1 O3 C7 O4 174.9(3) . . . . ? Tb1 O3 C7 C6 -5.6(5) . . . . ? N1 C6 C7 O4 -175.5(4) . . . . ? C5 C6 C7 O4 5.5(6) . . . . ? N1 C6 C7 O3 4.9(5) . . . . ? C5 C6 C7 O3 -174.1(4) . . . . ? Tb1 O5 C8 O6 172.7(3) . . . . ? Tb1 O5 C8 C9 -8.1(5) . . . . ? C13 N2 C9 C10 0.0(6) . . . . ? Tb1 N2 C9 C10 -177.6(3) . . . . ? C13 N2 C9 C8 -179.6(4) . . . . ? Tb1 N2 C9 C8 2.8(4) . . . . ? O6 C8 C9 N2 -177.8(4) . . . . ? O5 C8 C9 N2 2.9(5) . . . . ? O6 C8 C9 C10 2.6(6) . . . . ? O5 C8 C9 C10 -176.7(4) . . . . ? N2 C9 C10 C11 -0.4(6) . . . . ? C8 C9 C10 C11 179.2(4) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C9 N2 C13 C12 0.0(6) . . . . ? Tb1 N2 C13 C12 177.6(3) . . . . ? C9 N2 C13 C14 -177.0(3) . . . . ? Tb1 N2 C13 C14 0.7(5) . . . . ? C11 C12 C13 N2 0.3(6) . . . . ? C11 C12 C13 C14 176.9(4) . . . . ? Ag1 O8 C14 O7 7.8(4) 1_565 . . . ? Ag1' O8 C14 O7 5.9(4) 1_565 . . . ? Ag1 O8 C14 C13 -169.3(3) 1_565 . . . ? Ag1' O8 C14 C13 -171.2(4) 1_565 . . . ? Ag1' O7 C14 O8 -6.5(4) 1_565 . . . ? Tb1 O7 C14 O8 176.4(3) . . . . ? Ag1 O7 C14 O8 -7.0(4) 1_565 . . . ? Ag1' O7 C14 C13 170.7(3) 1_565 . . . ? Tb1 O7 C14 C13 -6.3(5) . . . . ? Ag1 O7 C14 C13 170.2(3) 1_565 . . . ? N2 C13 C14 O8 -179.4(4) . . . . ? C12 C13 C14 O8 3.8(6) . . . . ? N2 C13 C14 O7 3.3(5) . . . . ? C12 C13 C14 O7 -173.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.830 _refine_diff_density_min -1.410 _refine_diff_density_rms 0.169 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 650356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Ag Ce N2 O14' _chemical_formula_sum 'C14 H18 Ag Ce N2 O14' _chemical_formula_weight 686.29 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.656(3) _cell_length_b 7.3077(15) _cell_length_c 19.705(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.71(3) _cell_angle_gamma 90.00 _cell_volume 2091.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5038 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 3.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6317 _exptl_absorpt_correction_T_max 0.6659 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _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 15133 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3692 _reflns_number_gt 3308 _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^)+(0.0291P)^2^+2.1764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3692 _refine_ls_number_parameters 295 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.587 _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 Ce1 Ce 0.793080(19) 0.94908(4) 0.137652(15) 0.00898(11) Uani 1 1 d . . . Ag1 Ag 0.87785(4) 0.49549(8) 0.00723(4) 0.0469(2) Uani 1 1 d U . . C1 C 0.6325(4) 1.2799(8) 0.0863(3) 0.0116(11) Uani 1 1 d . . . C2 C 0.6211(4) 1.1621(7) 0.0226(3) 0.0120(11) Uani 1 1 d . . . C3 C 0.5596(4) 1.2056(8) -0.0359(3) 0.0171(13) Uani 1 1 d . . . H3 H 0.5239 1.3111 -0.0377 0.021 Uiso 1 1 calc R . . C4 C 0.5538(4) 1.0870(8) -0.0907(3) 0.0189(13) Uani 1 1 d . . . H4 H 0.5134 1.1118 -0.1302 0.023 Uiso 1 1 calc R . . C5 C 0.6078(4) 0.9311(8) -0.0870(3) 0.0154(12) Uani 1 1 d . . . H5 H 0.6044 0.8502 -0.1237 0.018 Uiso 1 1 calc R . . C6 C 0.6672(4) 0.8986(8) -0.0272(3) 0.0134(12) Uani 1 1 d . . . C7 C 0.7320(4) 0.7380(8) -0.0173(3) 0.0148(12) Uani 1 1 d . . . C8 C 0.9521(4) 0.6098(8) 0.1850(3) 0.0138(12) Uani 1 1 d . . . C9 C 1.0105(4) 0.7394(8) 0.1491(3) 0.0154(12) Uani 1 1 d . . . C10 C 1.1032(4) 0.7093(8) 0.1450(3) 0.0208(14) Uani 1 1 d . . . H10A H 1.1320 0.6026 0.1624 0.025 Uiso 1 1 calc R . . C11 C 1.1516(4) 0.8411(9) 0.1146(3) 0.0264(15) Uani 1 1 d . . . H11 H 1.2140 0.8254 0.1118 0.032 Uiso 1 1 calc R . . C12 C 1.1062(4) 0.9968(9) 0.0883(3) 0.0209(14) Uani 1 1 d . . . H12 H 1.1377 1.0881 0.0681 0.025 Uiso 1 1 calc R . . C13 C 1.0138(4) 1.0142(8) 0.0925(3) 0.0140(12) Uani 1 1 d . . . C14 C 0.9566(4) 1.1750(8) 0.0633(3) 0.0149(12) Uani 1 1 d . . . N1 N 0.6734(3) 1.0116(6) 0.0267(2) 0.0114(10) Uani 1 1 d . . . N2 N 0.9662(3) 0.8884(6) 0.1226(2) 0.0112(10) Uani 1 1 d . . . O1 O 0.7882(3) 0.7362(5) 0.03832(19) 0.0166(9) Uani 1 1 d . . . O2 O 0.7322(3) 0.6194(6) -0.0624(2) 0.0229(10) Uani 1 1 d . . . O3 O 0.6895(3) 1.2216(5) 0.13605(19) 0.0145(9) Uani 1 1 d . . . O4 O 0.5862(3) 1.4232(5) 0.0857(2) 0.0183(9) Uani 1 1 d . . . O5 O 0.8697(2) 0.6604(5) 0.1879(2) 0.0146(9) Uani 1 1 d . . . O6 O 0.9876(3) 0.4642(5) 0.2088(2) 0.0201(9) Uani 1 1 d . . . O7 O 0.8712(3) 1.1706(5) 0.06720(19) 0.0152(9) Uani 1 1 d . . . O8 O 0.9962(3) 1.3030(5) 0.0368(2) 0.0224(10) Uani 1 1 d . . . O9 O 0.7464(3) 0.9386(5) 0.25470(19) 0.0127(8) Uani 1 1 d . . . H9A H 0.7755 0.8756 0.2926 0.015 Uiso 1 1 d R . . H9B H 0.7015 1.0274 0.2751 0.015 Uiso 1 1 d R . . O10 O 0.8977(2) 1.1495(5) 0.22148(19) 0.0140(8) Uani 1 1 d . . . H10C H 0.9386 1.0689 0.2431 0.017 Uiso 1 1 d R . . H10B H 0.9194 1.2549 0.2139 0.017 Uiso 1 1 d R . . O11 O 0.6572(3) 0.7400(6) 0.1458(2) 0.0149(9) Uani 1 1 d . . . H11A H 0.650(5) 0.731(9) 0.181(3) 0.018 Uiso 1 1 d . . . H11B H 0.641(4) 0.640(9) 0.125(3) 0.018 Uiso 1 1 d . . . O12 O 0.6916(3) 0.5230(6) 0.8032(2) 0.0237(10) Uani 1 1 d . . . H12A H 0.7090 0.5197 0.8444 0.028 Uiso 1 1 d R . . H12B H 0.7351 0.5758 0.7840 0.028 Uiso 1 1 d R . . O13 O 0.1693(3) 0.3437(6) 0.2611(2) 0.0329(12) Uani 1 1 d . . . H13A H 0.1637 0.2265 0.2717 0.039 Uiso 1 1 d R . . H13B H 0.1121 0.3545 0.2405 0.039 Uiso 1 1 d R . . O14 O 0.0064(3) 0.9158(6) 0.2950(2) 0.0229(10) Uani 1 1 d . . . H14A H -0.0147 0.9272 0.3368 0.027 Uiso 1 1 d R . . H14B H 0.0630 0.9416 0.2965 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 Ce1 0.00752(16) 0.00894(18) 0.01035(17) 0.00078(12) 0.00071(11) 0.00100(12) Ag1 0.0236(3) 0.0283(3) 0.0920(5) 0.0306(3) 0.0196(3) 0.0145(2) C1 0.012(3) 0.013(3) 0.010(3) 0.002(2) 0.001(2) -0.002(2) C2 0.008(3) 0.012(3) 0.016(3) 0.000(2) 0.002(2) 0.001(2) C3 0.014(3) 0.016(3) 0.020(3) 0.001(3) -0.002(2) 0.004(2) C4 0.019(3) 0.025(3) 0.012(3) -0.001(3) -0.004(2) 0.003(3) C5 0.016(3) 0.018(3) 0.011(3) -0.004(2) -0.002(2) -0.002(2) C6 0.010(3) 0.014(3) 0.017(3) 0.000(2) 0.001(2) -0.002(2) C7 0.017(3) 0.013(3) 0.015(3) 0.000(2) 0.006(2) -0.001(2) C8 0.013(3) 0.011(3) 0.017(3) 0.003(2) 0.003(2) 0.001(2) C9 0.013(3) 0.016(3) 0.017(3) 0.002(2) 0.003(2) 0.003(2) C10 0.015(3) 0.019(3) 0.029(3) 0.011(3) 0.005(3) 0.008(3) C11 0.011(3) 0.031(4) 0.039(4) 0.013(3) 0.009(3) 0.004(3) C12 0.018(3) 0.021(3) 0.025(3) 0.012(3) 0.005(3) -0.002(3) C13 0.012(3) 0.015(3) 0.016(3) 0.004(2) 0.004(2) 0.001(2) C14 0.019(3) 0.010(3) 0.016(3) 0.003(2) 0.005(2) 0.002(2) N1 0.011(2) 0.011(2) 0.012(2) 0.0005(19) 0.0013(18) -0.0003(19) N2 0.011(2) 0.009(2) 0.013(2) 0.0035(19) 0.0003(18) 0.0028(19) O1 0.016(2) 0.017(2) 0.015(2) -0.0010(17) -0.0015(17) 0.0044(17) O2 0.029(2) 0.020(2) 0.019(2) -0.0073(19) -0.0008(18) 0.0069(19) O3 0.015(2) 0.015(2) 0.013(2) -0.0002(17) -0.0006(16) 0.0030(16) O4 0.017(2) 0.015(2) 0.021(2) -0.0037(18) -0.0038(17) 0.0071(17) O5 0.0104(19) 0.013(2) 0.020(2) 0.0059(17) 0.0028(16) 0.0017(16) O6 0.013(2) 0.015(2) 0.032(2) 0.0116(19) 0.0013(18) 0.0023(17) O7 0.014(2) 0.015(2) 0.018(2) 0.0054(17) 0.0051(16) 0.0024(16) O8 0.019(2) 0.014(2) 0.036(3) 0.011(2) 0.0112(19) 0.0037(18) O9 0.0133(18) 0.013(2) 0.0126(18) 0.0002(16) 0.0035(15) 0.0020(16) O10 0.0134(19) 0.009(2) 0.019(2) 0.0013(17) 0.0013(16) -0.0005(16) O11 0.017(2) 0.015(2) 0.013(2) 0.0000(18) 0.0015(18) -0.0032(17) O12 0.016(2) 0.034(3) 0.022(2) -0.004(2) 0.0022(18) -0.0020(19) O13 0.016(2) 0.033(3) 0.048(3) 0.016(2) 0.000(2) 0.001(2) O14 0.015(2) 0.030(3) 0.024(2) 0.007(2) 0.0027(18) 0.0018(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O9 2.493(4) . ? Ce1 O1 2.494(4) . ? Ce1 O3 2.502(4) . ? Ce1 O7 2.507(4) . ? Ce1 O5 2.528(4) . ? Ce1 O11 2.533(4) . ? Ce1 O10 2.558(4) . ? Ce1 N2 2.632(4) . ? Ce1 N1 2.653(4) . ? Ag1 O8 2.248(4) 1_545 ? Ag1 O1 2.326(4) . ? Ag1 O2 2.545(4) . ? Ag1 O8 2.599(4) 3_775 ? C1 O4 1.247(7) . ? C1 O3 1.273(6) . ? C1 C2 1.513(8) . ? C2 N1 1.337(7) . ? C2 C3 1.401(8) . ? C3 C4 1.378(8) . ? C3 H3 0.9300 . ? C4 C5 1.384(8) . ? C4 H4 0.9300 . ? C5 C6 1.388(8) . ? C5 H5 0.9300 . ? C6 N1 1.339(7) . ? C6 C7 1.505(8) . ? C7 O2 1.242(7) . ? C7 O1 1.279(7) . ? C8 O6 1.248(7) . ? C8 O5 1.272(6) . ? C8 C9 1.514(8) . ? C9 N2 1.337(7) . ? C9 C10 1.389(8) . ? C10 C11 1.380(8) . ? C10 H10A 0.9300 . ? C11 C12 1.383(8) . ? C11 H11 0.9300 . ? C12 C13 1.374(8) . ? C12 H12 0.9300 . ? C13 N2 1.339(7) . ? C13 C14 1.512(8) . ? C14 O8 1.252(7) . ? C14 O7 1.263(7) . ? O8 Ag1 2.248(4) 1_565 ? O8 Ag1 2.599(4) 3_775 ? O9 H9A 0.9303 . ? O9 H9B 1.0423 . ? O10 H10C 0.9050 . ? O10 H10B 0.8542 . ? O11 H11A 0.72(7) . ? O11 H11B 0.86(7) . ? O12 H12A 0.8178 . ? O12 H12B 0.8739 . ? O13 H13A 0.8879 . ? O13 H13B 0.8849 . ? O14 H14A 0.9221 . ? O14 H14B 0.8476 . ? 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 O9 Ce1 O1 136.43(13) . . ? O9 Ce1 O3 78.15(12) . . ? O1 Ce1 O3 122.23(12) . . ? O9 Ce1 O7 137.25(12) . . ? O1 Ce1 O7 86.28(13) . . ? O3 Ce1 O7 78.51(13) . . ? O9 Ce1 O5 76.98(12) . . ? O1 Ce1 O5 75.59(12) . . ? O3 Ce1 O5 154.94(13) . . ? O7 Ce1 O5 122.93(12) . . ? O9 Ce1 O11 66.85(13) . . ? O1 Ce1 O11 74.57(14) . . ? O3 Ce1 O11 89.99(13) . . ? O7 Ce1 O11 147.83(13) . . ? O5 Ce1 O11 77.48(13) . . ? O9 Ce1 O10 68.60(12) . . ? O1 Ce1 O10 144.63(12) . . ? O3 Ce1 O10 82.10(12) . . ? O7 Ce1 O10 73.09(12) . . ? O5 Ce1 O10 91.66(12) . . ? O11 Ce1 O10 135.44(13) . . ? O9 Ce1 N2 119.17(13) . . ? O1 Ce1 N2 74.49(13) . . ? O3 Ce1 N2 136.52(13) . . ? O7 Ce1 N2 61.79(13) . . ? O5 Ce1 N2 61.27(13) . . ? O11 Ce1 N2 133.15(14) . . ? O10 Ce1 N2 70.49(13) . . ? O9 Ce1 N1 122.32(13) . . ? O1 Ce1 N1 60.96(13) . . ? O3 Ce1 N1 61.28(13) . . ? O7 Ce1 N1 74.52(13) . . ? O5 Ce1 N1 132.54(13) . . ? O11 Ce1 N1 73.60(13) . . ? O10 Ce1 N1 134.93(13) . . ? N2 Ce1 N1 118.50(14) . . ? O8 Ag1 O1 148.01(15) 1_545 . ? O8 Ag1 O2 157.62(15) 1_545 . ? O1 Ag1 O2 53.87(13) . . ? O8 Ag1 O8 83.29(14) 1_545 3_775 ? O1 Ag1 O8 96.36(14) . 3_775 ? O2 Ag1 O8 101.55(14) . 3_775 ? O4 C1 O3 126.1(5) . . ? O4 C1 C2 118.1(5) . . ? O3 C1 C2 115.8(5) . . ? N1 C2 C3 122.4(5) . . ? N1 C2 C1 114.8(5) . . ? C3 C2 C1 122.7(5) . . ? C4 C3 C2 117.9(5) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 118.4(5) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? N1 C6 C5 122.3(5) . . ? N1 C6 C7 113.8(5) . . ? C5 C6 C7 123.9(5) . . ? O2 C7 O1 122.9(5) . . ? O2 C7 C6 120.8(5) . . ? O1 C7 C6 116.3(5) . . ? O6 C8 O5 125.5(5) . . ? O6 C8 C9 118.4(5) . . ? O5 C8 C9 116.0(5) . . ? N2 C9 C10 122.2(5) . . ? N2 C9 C8 114.6(5) . . ? C10 C9 C8 123.1(5) . . ? C11 C10 C9 118.6(5) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 118.8(6) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N2 C13 C12 122.7(5) . . ? N2 C13 C14 114.0(5) . . ? C12 C13 C14 123.3(5) . . ? O8 C14 O7 124.2(5) . . ? O8 C14 C13 118.3(5) . . ? O7 C14 C13 117.4(5) . . ? C2 N1 C6 118.9(5) . . ? C2 N1 Ce1 120.1(3) . . ? C6 N1 Ce1 120.9(3) . . ? C9 N2 C13 118.5(5) . . ? C9 N2 Ce1 121.2(4) . . ? C13 N2 Ce1 120.1(3) . . ? C7 O1 Ag1 96.0(3) . . ? C7 O1 Ce1 127.8(4) . . ? Ag1 O1 Ce1 136.13(16) . . ? C7 O2 Ag1 86.8(3) . . ? C1 O3 Ce1 127.7(3) . . ? C8 O5 Ce1 126.8(3) . . ? C14 O7 Ce1 125.4(3) . . ? C14 O8 Ag1 101.0(3) . 1_565 ? C14 O8 Ag1 162.3(4) . 3_775 ? Ag1 O8 Ag1 96.71(14) 1_565 3_775 ? Ce1 O9 H9A 127.2 . . ? Ce1 O9 H9B 127.1 . . ? H9A O9 H9B 104.1 . . ? Ce1 O10 H10C 103.5 . . ? Ce1 O10 H10B 127.5 . . ? H10C O10 H10B 115.4 . . ? Ce1 O11 H11A 110(5) . . ? Ce1 O11 H11B 131(4) . . ? H11A O11 H11B 109(7) . . ? H12A O12 H12B 107.1 . . ? H13A O13 H13B 94.7 . . ? H14A O14 H14B 113.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.368 _refine_diff_density_min -2.631 _refine_diff_density_rms 0.113 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 650357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Ag N2 Nd O14' _chemical_formula_weight 690.41 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.582(3) _cell_length_b 7.3325(15) _cell_length_c 19.606(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.99(3) _cell_angle_gamma 90.00 _cell_volume 2076.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6704 _cell_measurement_theta_min 1.6362 _cell_measurement_theta_max 27.9123 _exptl_crystal_description PRISM _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 3.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6406 _exptl_absorpt_correction_T_max 0.7215 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20051 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3665 _reflns_number_gt 3503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+9.4772P] 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 3665 _refine_ls_number_parameters 289 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.630 _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 Nd1 Nd 0.79324(2) 0.54911(4) 0.137648(16) 0.00866(13) Uani 1 1 d . . . Ag1 Ag 0.87750(4) 1.00514(9) 0.00556(5) 0.0486(2) Uani 1 1 d U . . C1 C 0.9498(4) 0.8859(9) 0.1867(3) 0.0134(13) Uani 1 1 d . . . C2 C 1.0085(4) 0.7578(9) 0.1502(3) 0.0141(13) Uani 1 1 d . . . C3 C 1.1018(5) 0.7879(10) 0.1465(4) 0.0201(15) Uani 1 1 d . . . H3 H 1.1307 0.8938 0.1647 0.024 Uiso 1 1 calc R . . C4 C 1.1511(5) 0.6582(10) 0.1155(4) 0.0246(16) Uani 1 1 d . . . H4 H 1.2137 0.6747 0.1127 0.030 Uiso 1 1 calc R . . C5 C 1.1051(5) 0.5027(10) 0.0885(4) 0.0190(15) Uani 1 1 d . . . H5 H 1.1366 0.4119 0.0681 0.023 Uiso 1 1 calc R . . C6 C 1.0119(5) 0.4857(9) 0.0927(3) 0.0130(13) Uani 1 1 d . . . C7 C 0.9544(4) 0.3255(9) 0.0636(3) 0.0141(13) Uani 1 1 d . . . C8 C 0.7336(4) 0.7603(9) -0.0163(3) 0.0153(14) Uani 1 1 d . . . C9 C 0.6676(4) 0.6012(9) -0.0262(3) 0.0124(13) Uani 1 1 d . . . C10 C 0.6082(5) 0.5691(9) -0.0866(3) 0.0173(14) Uani 1 1 d . . . H10 H 0.6051 0.6499 -0.1234 0.021 Uiso 1 1 calc R . . C11 C 0.5532(5) 0.4133(10) -0.0910(3) 0.0191(14) Uani 1 1 d . . . H11 H 0.5123 0.3886 -0.1307 0.023 Uiso 1 1 calc R . . C12 C 0.5602(4) 0.2955(9) -0.0351(3) 0.0167(14) Uani 1 1 d . . . H12 H 0.5244 0.1902 -0.0367 0.020 Uiso 1 1 calc R . . C13 C 0.6222(4) 0.3384(8) 0.0232(3) 0.0111(12) Uani 1 1 d . . . C14 C 0.6347(4) 0.2194(9) 0.0873(3) 0.0127(13) Uani 1 1 d . . . N1 N 0.9646(4) 0.6099(7) 0.1234(3) 0.0122(11) Uani 1 1 d . . . N2 N 0.6745(4) 0.4877(7) 0.0278(3) 0.0110(11) Uani 1 1 d . . . O2 O 0.9852(3) 1.0311(6) 0.2104(3) 0.0191(10) Uani 1 1 d . . . O3 O 0.8675(3) 0.8327(6) 0.1894(2) 0.0131(9) Uani 1 1 d . . . O4 O 0.8685(3) 0.3302(6) 0.0669(2) 0.0151(9) Uani 1 1 d . . . O5 O 0.9946(3) 0.1973(6) 0.0370(3) 0.0219(11) Uani 1 1 d . . . O6 O 0.7334(3) 0.8791(7) -0.0612(2) 0.0212(11) Uani 1 1 d . . . O7 O 0.7900(3) 0.7619(6) 0.0397(2) 0.0147(9) Uani 1 1 d . . . O8 O 0.6915(3) 0.2794(6) 0.1374(2) 0.0143(9) Uani 1 1 d . . . O9 O 0.5888(3) 0.0762(6) 0.0862(2) 0.0171(10) Uani 1 1 d . . . O10 O 0.8959(3) 0.3486(6) 0.2204(2) 0.0141(9) Uani 1 1 d . . . H10A H 0.9418 0.3994 0.2461 0.017 Uiso 1 1 d R . . H10B H 0.9232 0.2497 0.2124 0.017 Uiso 1 1 d R . . O11 O 0.7470(3) 0.5599(6) 0.2534(2) 0.0131(9) Uani 1 1 d . . . H11A H 0.7741 0.6284 0.2883 0.016 Uiso 1 1 d R . . H11B H 0.7056 0.4855 0.2659 0.016 Uiso 1 1 d R . . O12 O 0.6584(3) 0.7558(6) 0.1453(2) 0.0133(9) Uani 1 1 d . . . H12A H 0.6508 0.7771 0.1902 0.016 Uiso 1 1 d R . . H12B H 0.6434 0.8472 0.1230 0.016 Uiso 1 1 d R . . O13 O 0.3320(3) 0.6565(8) 0.2394(3) 0.0311(13) Uani 1 1 d . . . H13A H 0.3929 0.6295 0.2534 0.037 Uiso 1 1 d R . . H13B H 0.3377 0.7737 0.2269 0.037 Uiso 1 1 d R . . O14 O 0.3072(3) 0.0220(7) 0.1958(2) 0.0217(11) Uani 1 1 d . . . H14A H 0.2628 0.0637 0.2202 0.026 Uiso 1 1 d R . . H14B H 0.2865 0.0539 0.1491 0.026 Uiso 1 1 d R . . O15 O 0.0061(3) 0.5781(7) 0.2956(2) 0.0227(11) Uani 1 1 d . . . H15A H -0.0108 0.5803 0.3379 0.027 Uiso 1 1 d R . . H15B H 0.0780 0.5730 0.2964 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 Nd1 0.00817(19) 0.0085(2) 0.00966(19) -0.00054(12) 0.00227(13) -0.00083(12) Ag1 0.0232(3) 0.0283(4) 0.0984(6) -0.0340(4) 0.0226(4) -0.0143(3) C1 0.013(3) 0.011(3) 0.017(3) -0.002(3) 0.002(3) 0.001(3) C2 0.013(3) 0.014(3) 0.016(3) -0.001(3) 0.003(2) -0.002(3) C3 0.017(3) 0.020(4) 0.024(4) -0.009(3) 0.005(3) -0.007(3) C4 0.012(3) 0.027(4) 0.036(4) -0.009(3) 0.007(3) -0.003(3) C5 0.015(3) 0.021(4) 0.022(4) -0.010(3) 0.005(3) 0.000(3) C6 0.016(3) 0.013(3) 0.012(3) -0.003(3) 0.006(3) 0.000(3) C7 0.018(3) 0.012(3) 0.013(3) 0.000(3) 0.005(3) -0.002(3) C8 0.018(3) 0.013(3) 0.017(3) 0.000(3) 0.009(3) 0.001(3) C9 0.013(3) 0.013(3) 0.012(3) 0.000(3) 0.004(2) 0.001(3) C10 0.017(3) 0.020(4) 0.015(3) 0.005(3) 0.003(3) 0.001(3) C11 0.019(3) 0.023(4) 0.014(3) 0.001(3) -0.004(3) -0.004(3) C12 0.015(3) 0.016(3) 0.018(3) 0.001(3) 0.001(3) -0.004(3) C13 0.010(3) 0.009(3) 0.014(3) -0.001(2) 0.003(2) 0.000(2) C14 0.011(3) 0.014(3) 0.014(3) 0.000(3) 0.006(2) 0.002(3) N1 0.012(3) 0.012(3) 0.012(3) -0.003(2) 0.003(2) -0.001(2) N2 0.012(3) 0.012(3) 0.010(3) 0.000(2) 0.005(2) 0.000(2) O2 0.013(2) 0.012(2) 0.032(3) -0.009(2) 0.002(2) -0.0015(19) O3 0.010(2) 0.013(2) 0.017(2) -0.0034(18) 0.0025(17) -0.0009(18) O4 0.015(2) 0.013(2) 0.018(2) -0.0048(18) 0.0069(18) -0.0029(18) O5 0.021(3) 0.013(2) 0.034(3) -0.011(2) 0.012(2) -0.003(2) O6 0.028(3) 0.019(3) 0.016(2) 0.006(2) 0.001(2) -0.005(2) O7 0.014(2) 0.016(2) 0.014(2) 0.0019(18) 0.0011(18) -0.0048(19) O8 0.016(2) 0.013(2) 0.013(2) 0.0014(18) -0.0008(18) -0.0034(18) O9 0.018(2) 0.012(2) 0.021(2) 0.0037(19) -0.0013(19) -0.0051(19) O10 0.011(2) 0.013(2) 0.018(2) -0.0024(18) 0.0004(18) 0.0022(18) O11 0.016(2) 0.013(2) 0.011(2) -0.0016(17) 0.0043(17) -0.0022(18) O12 0.014(2) 0.014(2) 0.012(2) 0.0008(18) 0.0015(17) 0.0022(18) O13 0.016(3) 0.031(3) 0.046(3) 0.017(3) 0.002(2) 0.001(2) O14 0.015(2) 0.028(3) 0.022(3) 0.005(2) 0.001(2) 0.001(2) O15 0.018(2) 0.031(3) 0.019(2) -0.006(2) 0.002(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O11 2.457(4) . ? Nd1 O7 2.469(4) . ? Nd1 O8 2.472(4) . ? Nd1 O4 2.475(4) . ? Nd1 O3 2.494(4) . ? Nd1 O12 2.504(4) . ? Nd1 O10 2.521(4) . ? Nd1 N1 2.591(5) . ? Nd1 N2 2.609(5) . ? Ag1 O5 2.233(5) 1_565 ? Ag1 O7 2.345(4) . ? Ag1 O6 2.493(5) . ? C1 O2 1.244(8) . ? C1 O3 1.271(8) . ? C1 C2 1.516(9) . ? C2 N1 1.330(8) . ? C2 C3 1.389(9) . ? C3 C4 1.384(10) . ? C3 H3 0.9300 . ? C4 C5 1.389(10) . ? C4 H4 0.9300 . ? C5 C6 1.379(9) . ? C5 H5 0.9300 . ? C6 N1 1.335(8) . ? C6 C7 1.507(9) . ? C7 O5 1.258(8) . ? C7 O4 1.264(8) . ? C8 O6 1.239(8) . ? C8 O7 1.277(8) . ? C8 C9 1.507(9) . ? C9 N2 1.339(8) . ? C9 C10 1.387(9) . ? C10 C11 1.391(10) . ? C10 H10 0.9300 . ? C11 C12 1.387(9) . ? C11 H11 0.9300 . ? C12 C13 1.392(9) . ? C12 H12 0.9300 . ? C13 N2 1.331(8) . ? C13 C14 1.519(9) . ? C14 O9 1.244(8) . ? C14 O8 1.272(8) . ? O5 Ag1 2.233(5) 1_545 ? O10 H10A 0.8646 . ? O10 H10B 0.8523 . ? O11 H11A 0.8957 . ? O11 H11B 0.8731 . ? O12 H12A 0.9146 . ? O12 H12B 0.8139 . ? O13 H13A 0.9140 . ? O13 H13B 0.9005 . ? O14 H14A 0.9105 . ? O14 H14B 0.9522 . ? O15 H15A 0.8985 . ? O15 H15B 1.0472 . ? 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 O11 Nd1 O7 136.01(14) . . ? O11 Nd1 O8 77.65(14) . . ? O7 Nd1 O8 123.85(14) . . ? O11 Nd1 O4 137.59(15) . . ? O7 Nd1 O4 86.36(15) . . ? O8 Nd1 O4 78.03(15) . . ? O11 Nd1 O3 75.90(14) . . ? O7 Nd1 O3 75.52(14) . . ? O8 Nd1 O3 153.42(14) . . ? O4 Nd1 O3 124.58(14) . . ? O11 Nd1 O12 66.80(14) . . ? O7 Nd1 O12 74.56(14) . . ? O8 Nd1 O12 90.47(15) . . ? O4 Nd1 O12 147.06(14) . . ? O3 Nd1 O12 76.76(14) . . ? O11 Nd1 O10 68.86(14) . . ? O7 Nd1 O10 144.51(14) . . ? O8 Nd1 O10 80.64(14) . . ? O4 Nd1 O10 73.29(14) . . ? O3 Nd1 O10 92.24(14) . . ? O12 Nd1 O10 135.66(14) . . ? O11 Nd1 N1 119.12(16) . . ? O7 Nd1 N1 73.88(16) . . ? O8 Nd1 N1 136.45(16) . . ? O4 Nd1 N1 62.73(15) . . ? O3 Nd1 N1 61.97(15) . . ? O12 Nd1 N1 132.82(16) . . ? O10 Nd1 N1 71.00(15) . . ? O11 Nd1 N2 122.16(15) . . ? O7 Nd1 N2 61.84(15) . . ? O8 Nd1 N2 62.01(15) . . ? O4 Nd1 N2 73.78(15) . . ? O3 Nd1 N2 132.90(15) . . ? O12 Nd1 N2 73.57(15) . . ? O10 Nd1 N2 134.20(15) . . ? N1 Nd1 N2 118.69(16) . . ? O5 Ag1 O7 145.75(17) 1_565 . ? O5 Ag1 O6 159.20(18) 1_565 . ? O7 Ag1 O6 54.25(15) . . ? O2 C1 O3 126.3(6) . . ? O2 C1 C2 118.3(6) . . ? O3 C1 C2 115.4(5) . . ? N1 C2 C3 122.0(6) . . ? N1 C2 C1 114.8(5) . . ? C3 C2 C1 123.2(6) . . ? C4 C3 C2 119.1(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.6(6) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 118.6(6) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 122.7(6) . . ? N1 C6 C7 114.1(6) . . ? C5 C6 C7 123.2(6) . . ? O5 C7 O4 124.3(6) . . ? O5 C7 C6 118.2(6) . . ? O4 C7 C6 117.5(6) . . ? O6 C8 O7 122.8(6) . . ? O6 C8 C9 120.9(6) . . ? O7 C8 C9 116.2(6) . . ? N2 C9 C10 122.6(6) . . ? N2 C9 C8 113.7(5) . . ? C10 C9 C8 123.6(6) . . ? C9 C10 C11 118.5(6) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 119.0(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 118.5(6) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? N2 C13 C12 122.8(6) . . ? N2 C13 C14 114.6(5) . . ? C12 C13 C14 122.7(6) . . ? O9 C14 O8 126.6(6) . . ? O9 C14 C13 117.9(6) . . ? O8 C14 C13 115.5(5) . . ? C2 N1 C6 119.0(5) . . ? C2 N1 Nd1 121.1(4) . . ? C6 N1 Nd1 119.8(4) . . ? C13 N2 C9 118.7(5) . . ? C13 N2 Nd1 120.4(4) . . ? C9 N2 Nd1 120.9(4) . . ? C1 O3 Nd1 126.7(4) . . ? C7 O4 Nd1 124.5(4) . . ? C7 O5 Ag1 101.8(4) . 1_545 ? C8 O6 Ag1 88.2(4) . . ? C8 O7 Ag1 94.2(4) . . ? C8 O7 Nd1 127.1(4) . . ? Ag1 O7 Nd1 138.64(19) . . ? C14 O8 Nd1 127.2(4) . . ? Nd1 O10 H10A 117.8 . . ? Nd1 O10 H10B 129.0 . . ? H10A O10 H10B 97.5 . . ? Nd1 O11 H11A 125.1 . . ? Nd1 O11 H11B 121.9 . . ? H11A O11 H11B 112.6 . . ? Nd1 O12 H12A 111.2 . . ? Nd1 O12 H12B 128.3 . . ? H12A O12 H12B 108.5 . . ? H13A O13 H13B 99.6 . . ? H14A O14 H14B 105.6 . . ? H15A O15 H15B 112.8 . . ? 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 N1 -176.9(6) . . . . ? O3 C1 C2 N1 2.6(8) . . . . ? O2 C1 C2 C3 5.1(10) . . . . ? O3 C1 C2 C3 -175.4(6) . . . . ? N1 C2 C3 C4 -1.5(10) . . . . ? C1 C2 C3 C4 176.4(6) . . . . ? C2 C3 C4 C5 0.5(11) . . . . ? C3 C4 C5 C6 1.2(11) . . . . ? C4 C5 C6 N1 -2.1(10) . . . . ? C4 C5 C6 C7 178.3(6) . . . . ? N1 C6 C7 O5 -176.2(6) . . . . ? C5 C6 C7 O5 3.4(10) . . . . ? N1 C6 C7 O4 4.5(8) . . . . ? C5 C6 C7 O4 -175.9(6) . . . . ? O6 C8 C9 N2 -178.2(6) . . . . ? O7 C8 C9 N2 3.5(8) . . . . ? O6 C8 C9 C10 4.7(10) . . . . ? O7 C8 C9 C10 -173.6(6) . . . . ? N2 C9 C10 C11 0.4(10) . . . . ? C8 C9 C10 C11 177.2(6) . . . . ? C9 C10 C11 C12 -0.5(10) . . . . ? C10 C11 C12 C13 0.1(10) . . . . ? C11 C12 C13 N2 0.3(10) . . . . ? C11 C12 C13 C14 179.5(6) . . . . ? N2 C13 C14 O9 -179.0(6) . . . . ? C12 C13 C14 O9 1.7(9) . . . . ? N2 C13 C14 O8 1.6(8) . . . . ? C12 C13 C14 O8 -177.7(6) . . . . ? C3 C2 N1 C6 0.7(9) . . . . ? C1 C2 N1 C6 -177.4(6) . . . . ? C3 C2 N1 Nd1 176.3(5) . . . . ? C1 C2 N1 Nd1 -1.8(7) . . . . ? C5 C6 N1 C2 1.1(10) . . . . ? C7 C6 N1 C2 -179.3(5) . . . . ? C5 C6 N1 Nd1 -174.5(5) . . . . ? C7 C6 N1 Nd1 5.1(7) . . . . ? O11 Nd1 N1 C2 -51.7(5) . . . . ? O7 Nd1 N1 C2 82.4(5) . . . . ? O8 Nd1 N1 C2 -155.1(4) . . . . ? O4 Nd1 N1 C2 176.7(5) . . . . ? O3 Nd1 N1 C2 0.5(4) . . . . ? O12 Nd1 N1 C2 32.6(5) . . . . ? O10 Nd1 N1 C2 -102.8(5) . . . . ? N2 Nd1 N1 C2 126.5(5) . . . . ? O11 Nd1 N1 C6 123.8(4) . . . . ? O7 Nd1 N1 C6 -102.0(5) . . . . ? O8 Nd1 N1 C6 20.5(6) . . . . ? O4 Nd1 N1 C6 -7.8(4) . . . . ? O3 Nd1 N1 C6 176.1(5) . . . . ? O12 Nd1 N1 C6 -151.8(4) . . . . ? O10 Nd1 N1 C6 72.8(5) . . . . ? N2 Nd1 N1 C6 -57.9(5) . . . . ? C12 C13 N2 C9 -0.3(9) . . . . ? C14 C13 N2 C9 -179.7(5) . . . . ? C12 C13 N2 Nd1 -177.5(5) . . . . ? C14 C13 N2 Nd1 3.1(7) . . . . ? C10 C9 N2 C13 0.0(9) . . . . ? C8 C9 N2 C13 -177.1(5) . . . . ? C10 C9 N2 Nd1 177.2(5) . . . . ? C8 C9 N2 Nd1 0.1(7) . . . . ? O11 Nd1 N2 C13 -55.9(5) . . . . ? O7 Nd1 N2 C13 175.2(5) . . . . ? O8 Nd1 N2 C13 -4.2(4) . . . . ? O4 Nd1 N2 C13 80.6(5) . . . . ? O3 Nd1 N2 C13 -156.9(4) . . . . ? O12 Nd1 N2 C13 -103.8(5) . . . . ? O10 Nd1 N2 C13 35.1(5) . . . . ? N1 Nd1 N2 C13 125.9(4) . . . . ? O11 Nd1 N2 C9 127.0(4) . . . . ? O7 Nd1 N2 C9 -1.9(4) . . . . ? O8 Nd1 N2 C9 178.6(5) . . . . ? O4 Nd1 N2 C9 -96.5(5) . . . . ? O3 Nd1 N2 C9 25.9(5) . . . . ? O12 Nd1 N2 C9 79.1(5) . . . . ? O10 Nd1 N2 C9 -142.1(4) . . . . ? N1 Nd1 N2 C9 -51.2(5) . . . . ? O2 C1 O3 Nd1 177.0(5) . . . . ? C2 C1 O3 Nd1 -2.5(8) . . . . ? O11 Nd1 O3 C1 135.8(5) . . . . ? O7 Nd1 O3 C1 -78.0(5) . . . . ? O8 Nd1 O3 C1 141.6(5) . . . . ? O4 Nd1 O3 C1 -2.9(5) . . . . ? O12 Nd1 O3 C1 -155.2(5) . . . . ? O10 Nd1 O3 C1 68.2(5) . . . . ? N1 Nd1 O3 C1 1.2(5) . . . . ? N2 Nd1 O3 C1 -103.2(5) . . . . ? O5 C7 O4 Nd1 167.8(5) . . . . ? C6 C7 O4 Nd1 -12.9(8) . . . . ? O11 Nd1 O4 C7 -93.3(5) . . . . ? O7 Nd1 O4 C7 84.8(5) . . . . ? O8 Nd1 O4 C7 -149.5(5) . . . . ? O3 Nd1 O4 C7 15.1(5) . . . . ? O12 Nd1 O4 C7 138.7(5) . . . . ? O10 Nd1 O4 C7 -65.8(5) . . . . ? N1 Nd1 O4 C7 11.0(5) . . . . ? N2 Nd1 O4 C7 146.5(5) . . . . ? O4 C7 O5 Ag1 -1.5(7) . . . 1_545 ? C6 C7 O5 Ag1 179.3(5) . . . 1_545 ? O7 C8 O6 Ag1 7.3(6) . . . . ? C9 C8 O6 Ag1 -170.9(5) . . . . ? O5 Ag1 O6 C8 -170.7(5) 1_565 . . . ? O7 Ag1 O6 C8 -4.1(4) . . . . ? O6 C8 O7 Ag1 -7.8(7) . . . . ? C9 C8 O7 Ag1 170.5(5) . . . . ? O6 C8 O7 Nd1 175.7(5) . . . . ? C9 C8 O7 Nd1 -6.0(8) . . . . ? O5 Ag1 O7 C8 175.6(4) 1_565 . . . ? O6 Ag1 O7 C8 4.0(3) . . . . ? O5 Ag1 O7 Nd1 -8.5(5) 1_565 . . . ? O6 Ag1 O7 Nd1 179.8(4) . . . . ? O11 Nd1 O7 C8 -104.0(5) . . . . ? O8 Nd1 O7 C8 5.0(6) . . . . ? O4 Nd1 O7 C8 77.9(5) . . . . ? O3 Nd1 O7 C8 -154.9(5) . . . . ? O12 Nd1 O7 C8 -75.0(5) . . . . ? O10 Nd1 O7 C8 132.1(5) . . . . ? N1 Nd1 O7 C8 140.6(5) . . . . ? N2 Nd1 O7 C8 4.4(5) . . . . ? O11 Nd1 O7 Ag1 81.2(4) . . . . ? O8 Nd1 O7 Ag1 -169.9(3) . . . . ? O4 Nd1 O7 Ag1 -96.9(3) . . . . ? O3 Nd1 O7 Ag1 30.2(3) . . . . ? O12 Nd1 O7 Ag1 110.2(3) . . . . ? O10 Nd1 O7 Ag1 -42.8(4) . . . . ? N1 Nd1 O7 Ag1 -34.3(3) . . . . ? N2 Nd1 O7 Ag1 -170.4(4) . . . . ? O9 C14 O8 Nd1 174.4(5) . . . . ? C13 C14 O8 Nd1 -6.3(7) . . . . ? O11 Nd1 O8 C14 142.9(5) . . . . ? O7 Nd1 O8 C14 5.1(5) . . . . ? O4 Nd1 O8 C14 -72.1(5) . . . . ? O3 Nd1 O8 C14 137.1(5) . . . . ? O12 Nd1 O8 C14 76.8(5) . . . . ? O10 Nd1 O8 C14 -146.9(5) . . . . ? N1 Nd1 O8 C14 -97.6(5) . . . . ? N2 Nd1 O8 C14 5.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.648 _refine_diff_density_min -2.489 _refine_diff_density_rms 0.128