# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sun, Wei-Yin' _publ_contact_author_email sunwy@nju.edu.cn loop_ _publ_author_name M.Chen M.-S.Chen T.Okamura M.-F.Lv W.-Y.Sun N.Ueyama data_1 _database_code_depnum_ccdc_archive 'CCDC 803742' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Ag N6 Nd O12' _chemical_formula_sum 'C20 H18 Ag N6 Nd O12' _chemical_formula_weight 786.51 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8023(11) _cell_length_b 12.190(2) _cell_length_c 14.598(2) _cell_angle_alpha 79.2400(10) _cell_angle_beta 77.460(3) _cell_angle_gamma 80.735(2) _cell_volume 1151.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4940 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour pale-purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 3.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4713 _exptl_absorpt_correction_T_max 0.5430 _exptl_absorpt_process_details 'SADBAS (Bruker,2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 5738 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3979 _reflns_number_gt 3892 _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^)+(0.0726P)^2^+1.8797P] 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 3979 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.27002(7) 0.92379(4) 1.00814(3) 0.02928(15) Uani 1 1 d . . . Nd1 Nd 0.16454(4) 0.514997(19) 0.695630(16) 0.01487(12) Uani 1 1 d . . . C1 C 0.2841(8) 0.6060(4) 1.0143(4) 0.0192(10) Uani 1 1 d . . . H1 H 0.1654 0.5723 1.0307 0.023 Uiso 1 1 calc R . . C2 C 0.3904(8) 0.6160(4) 0.9218(4) 0.0186(10) Uani 1 1 d . . . C3 C 0.5689(8) 0.6666(4) 0.8963(4) 0.0197(10) Uani 1 1 d . . . H3 H 0.6428 0.6721 0.8344 0.024 Uiso 1 1 calc R . . C4 C 0.6335(7) 0.7082(4) 0.9649(3) 0.0174(10) Uani 1 1 d . . . C5 C 0.5265(8) 0.6992(4) 1.0579(4) 0.0198(10) Uani 1 1 d . . . H5 H 0.5707 0.7286 1.1031 0.024 Uiso 1 1 calc R . . C6 C 0.3529(7) 0.6458(4) 1.0826(4) 0.0175(10) Uani 1 1 d . . . C7 C 0.9244(8) 0.7975(4) 0.8533(3) 0.0215(11) Uani 1 1 d . . . H7 H 0.9026 0.7812 0.7968 0.026 Uiso 1 1 calc R . . C8 C 0.8972(8) 0.8042(5) 1.0014(4) 0.0235(11) Uani 1 1 d . . . H8 H 0.8554 0.7943 1.0671 0.028 Uiso 1 1 calc R . . C9 C 0.3181(8) 0.5711(4) 0.8471(4) 0.0179(10) Uani 1 1 d . . . C10 C 0.2476(7) 0.6318(4) 1.1857(3) 0.0173(10) Uani 1 1 d . . . C11 C 0.2166(8) 0.9446(4) 0.5738(4) 0.0196(10) Uani 1 1 d . . . H11 H 0.1824 0.9374 0.6397 0.024 Uiso 1 1 calc R . . C12 C 0.2421(8) 0.8496(4) 0.5305(3) 0.0176(10) Uani 1 1 d . . . C13 C 0.2910(7) 0.8599(4) 0.4326(3) 0.0185(10) Uani 1 1 d . . . H13 H 0.3073 0.7971 0.4027 0.022 Uiso 1 1 calc R . . C14 C 0.3151(7) 0.9643(4) 0.3803(3) 0.0186(10) Uani 1 1 d . . . C15 C 0.2881(8) 1.0597(4) 0.4221(4) 0.0198(10) Uani 1 1 d . . . H15 H 0.3011 1.1299 0.3848 0.024 Uiso 1 1 calc R . . C16 C 0.2414(7) 1.0497(4) 0.5203(4) 0.0183(10) Uani 1 1 d . . . C17 C 0.2625(8) 0.9348(4) 0.2236(4) 0.0217(11) Uani 1 1 d . . . H17 H 0.1479 0.8978 0.2458 0.026 Uiso 1 1 calc R . . C18 C 0.5179(8) 1.0204(5) 0.2179(4) 0.0254(12) Uani 1 1 d . . . H18 H 0.6145 1.0535 0.2359 0.030 Uiso 1 1 calc R . . C19 C 0.2169(8) 0.7357(4) 0.5883(3) 0.0188(10) Uani 1 1 d . . . C20 C 0.2150(8) 1.1533(4) 0.5668(4) 0.0204(11) Uani 1 1 d . . . N1 N 0.8102(6) 0.7650(3) 0.9409(3) 0.0182(9) Uani 1 1 d . . . N2 N 1.0656(7) 0.8534(4) 0.8587(3) 0.0250(10) Uani 1 1 d . . . N3 N 1.0472(7) 0.8576(4) 0.9543(3) 0.0243(10) Uani 1 1 d . . . N4 N 0.3621(7) 0.9743(3) 0.2785(3) 0.0190(9) Uani 1 1 d . . . N5 N 0.3501(7) 0.9559(4) 0.1355(3) 0.0233(10) Uani 1 1 d . . . N6 N 0.5145(7) 1.0120(4) 0.1311(3) 0.0250(10) Uani 1 1 d . . . O1 O 0.1376(6) 0.5531(3) 0.8610(3) 0.0273(9) Uani 1 1 d . . . O2 O 0.4414(5) 0.5548(3) 0.7711(3) 0.0253(8) Uani 1 1 d . . . O3 O 0.1048(6) 0.5711(3) 1.2064(3) 0.0296(9) Uani 1 1 d . . . O4 O 0.3027(6) 0.6777(3) 1.2436(3) 0.0272(8) Uani 1 1 d . . . O5 O 0.1696(7) 0.7267(3) 0.6763(2) 0.0292(9) Uani 1 1 d . . . O6 O 0.2418(6) 0.6516(3) 0.5461(3) 0.0268(8) Uani 1 1 d . . . O7 O 0.1879(6) 1.1413(3) 0.6545(3) 0.0292(9) Uani 1 1 d . . . O8 O 0.2248(7) 1.2459(3) 0.5112(3) 0.0313(9) Uani 1 1 d . . . O9 O 0.5193(6) 0.4522(4) 0.6060(3) 0.0366(10) Uani 1 1 d . . . H9A H 0.5856 0.4247 0.5572 0.044 Uiso 1 1 d R . . H9B H 0.5661 0.4164 0.6541 0.044 Uiso 1 1 d R . . O10 O 0.0664(9) 0.4251(4) 0.5808(4) 0.0641(18) Uani 1 1 d . . . H10A H 0.1460 0.3669 0.5664 0.077 Uiso 1 1 d R . . H10B H -0.0444 0.4005 0.6095 0.077 Uiso 0.50 1 d PR . . H10C H 0.0361 0.4706 0.5328 0.077 Uiso 0.50 1 d PR . . O11 O 0.2820(6) 0.3000(3) 0.7490(3) 0.0325(9) Uani 1 1 d . . . H11A H 0.2687 0.2494 0.7187 0.039 Uiso 1 1 d R . . H11B H 0.4077 0.3000 0.7473 0.039 Uiso 1 1 d R . . O12 O -0.1795(6) 0.6267(3) 0.6671(3) 0.0314(9) Uani 1 1 d . . . H12A H -0.1960 0.6650 0.6137 0.038 Uiso 1 1 d R . . H12B H -0.2930 0.6062 0.6969 0.038 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0320(3) 0.0399(3) 0.0218(2) -0.00767(18) -0.00570(18) -0.0179(2) Nd1 0.01779(18) 0.01444(17) 0.01336(17) -0.00225(10) -0.00196(11) -0.00618(11) C1 0.019(2) 0.014(2) 0.026(3) -0.0029(19) -0.006(2) -0.0035(19) C2 0.019(3) 0.019(2) 0.021(3) -0.0019(19) -0.008(2) -0.007(2) C3 0.025(3) 0.017(2) 0.018(3) -0.0040(19) -0.003(2) -0.005(2) C4 0.018(2) 0.015(2) 0.020(3) -0.0016(19) -0.005(2) -0.0066(19) C5 0.019(3) 0.023(3) 0.020(3) -0.007(2) -0.008(2) -0.003(2) C6 0.017(2) 0.013(2) 0.021(3) -0.0022(19) -0.002(2) -0.0030(19) C7 0.024(3) 0.024(3) 0.019(3) -0.007(2) -0.004(2) -0.007(2) C8 0.023(3) 0.033(3) 0.018(3) -0.008(2) -0.001(2) -0.014(2) C9 0.022(3) 0.017(2) 0.017(3) -0.0044(19) -0.005(2) -0.003(2) C10 0.018(2) 0.018(2) 0.016(2) -0.0002(19) -0.0067(19) 0.000(2) C11 0.021(3) 0.020(3) 0.015(2) 0.0012(19) -0.0040(19) -0.001(2) C12 0.018(2) 0.018(2) 0.018(2) -0.0002(19) -0.0056(19) -0.0049(19) C13 0.020(2) 0.016(2) 0.019(3) -0.0025(19) -0.002(2) -0.0020(19) C14 0.018(2) 0.024(3) 0.014(2) -0.0011(19) -0.0032(19) -0.005(2) C15 0.019(2) 0.015(2) 0.025(3) -0.001(2) -0.004(2) -0.0041(19) C16 0.013(2) 0.018(2) 0.024(3) -0.005(2) -0.0053(19) 0.0015(19) C17 0.030(3) 0.019(2) 0.018(3) -0.0030(19) -0.005(2) -0.009(2) C18 0.027(3) 0.036(3) 0.018(3) -0.007(2) -0.003(2) -0.014(2) C19 0.021(2) 0.019(3) 0.016(3) -0.0016(19) -0.0023(19) -0.005(2) C20 0.016(2) 0.023(3) 0.024(3) -0.007(2) -0.007(2) -0.003(2) N1 0.019(2) 0.021(2) 0.017(2) -0.0036(16) -0.0035(16) -0.0079(17) N2 0.024(2) 0.028(2) 0.025(2) -0.0063(19) -0.0010(19) -0.0117(19) N3 0.022(2) 0.028(2) 0.025(2) -0.0077(19) -0.0027(18) -0.0094(19) N4 0.022(2) 0.021(2) 0.014(2) -0.0025(16) -0.0007(16) -0.0061(17) N5 0.025(2) 0.027(2) 0.020(2) -0.0032(18) -0.0026(18) -0.0104(19) N6 0.026(2) 0.033(3) 0.018(2) 0.0009(18) -0.0032(18) -0.016(2) O1 0.023(2) 0.039(2) 0.022(2) -0.0062(16) -0.0023(15) -0.0134(17) O2 0.0213(19) 0.035(2) 0.024(2) -0.0126(16) -0.0046(15) -0.0050(16) O3 0.025(2) 0.043(2) 0.023(2) -0.0046(17) 0.0027(16) -0.0212(18) O4 0.031(2) 0.032(2) 0.0224(19) -0.0077(16) -0.0054(16) -0.0084(17) O5 0.055(3) 0.0181(18) 0.0152(19) -0.0037(14) -0.0031(17) -0.0101(18) O6 0.042(2) 0.0181(18) 0.0192(19) -0.0047(14) 0.0009(16) -0.0084(17) O7 0.047(2) 0.0232(19) 0.019(2) -0.0083(15) -0.0036(17) -0.0072(18) O8 0.056(3) 0.0129(18) 0.025(2) -0.0021(15) -0.0093(19) -0.0027(18) O9 0.036(2) 0.046(3) 0.025(2) -0.0113(18) 0.0022(17) 0.001(2) O10 0.078(4) 0.054(3) 0.082(4) -0.046(3) -0.061(3) 0.030(3) O11 0.033(2) 0.025(2) 0.043(2) -0.0122(18) -0.0097(19) -0.0015(17) O12 0.023(2) 0.039(2) 0.028(2) 0.0048(17) -0.0040(16) -0.0050(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N5 2.164(4) 1_656 ? Ag1 N3 2.171(4) . ? Ag1 N6 2.318(4) 2_776 ? Nd1 O3 2.329(4) 2_567 ? Nd1 O10 2.422(4) . ? Nd1 O6 2.498(4) . ? Nd1 O1 2.506(4) . ? Nd1 O2 2.528(4) . ? Nd1 O5 2.548(4) . ? Nd1 O9 2.556(4) . ? Nd1 O12 2.587(4) . ? Nd1 O11 2.636(4) . ? C1 C6 1.379(7) . ? C1 C2 1.381(7) . ? C1 H1 0.9300 . ? C2 C3 1.397(7) . ? C2 C9 1.507(7) . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 N1 1.429(6) . ? C5 C6 1.387(7) . ? C5 H5 0.9300 . ? C6 C10 1.511(7) . ? C7 N2 1.287(6) . ? C7 N1 1.369(6) . ? C7 H7 0.9300 . ? C8 N3 1.296(7) . ? C8 N1 1.354(6) . ? C8 H8 0.9300 . ? C9 O1 1.249(6) . ? C9 O2 1.264(6) . ? C10 O4 1.245(6) . ? C10 O3 1.266(6) . ? C11 C16 1.386(7) . ? C11 C12 1.390(7) . ? C11 H11 0.9300 . ? C12 C13 1.381(7) . ? C12 C19 1.498(7) . ? C13 C14 1.371(7) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 N4 1.436(6) . ? C15 C16 1.387(7) . ? C15 H15 0.9300 . ? C16 C20 1.509(7) . ? C17 N5 1.292(7) . ? C17 N4 1.349(7) . ? C17 H17 0.9300 . ? C18 N6 1.295(7) . ? C18 N4 1.349(7) . ? C18 H18 0.9300 . ? C19 O5 1.243(6) . ? C19 O6 1.263(6) . ? C20 O7 1.237(6) . ? C20 O8 1.263(7) . ? N2 N3 1.384(6) . ? N5 N6 1.387(6) . ? N5 Ag1 2.164(4) 1_454 ? N6 Ag1 2.318(4) 2_776 ? O3 Nd1 2.329(4) 2_567 ? O9 H9A 0.8501 . ? O9 H9B 0.8499 . ? O10 H10A 0.8500 . ? O10 H10B 0.8500 . ? O10 H10C 0.8500 . ? O11 H11A 0.8499 . ? O11 H11B 0.8500 . ? O12 H12A 0.8500 . ? O12 H12B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N3 144.18(17) 1_656 . ? N5 Ag1 N6 114.00(16) 1_656 2_776 ? N3 Ag1 N6 101.74(16) . 2_776 ? O3 Nd1 O10 80.73(19) 2_567 . ? O3 Nd1 O6 140.78(14) 2_567 . ? O10 Nd1 O6 77.95(18) . . ? O3 Nd1 O1 71.75(13) 2_567 . ? O10 Nd1 O1 152.34(19) . . ? O6 Nd1 O1 126.01(12) . . ? O3 Nd1 O2 118.24(13) 2_567 . ? O10 Nd1 O2 148.92(16) . . ? O6 Nd1 O2 96.22(13) . . ? O1 Nd1 O2 51.71(12) . . ? O3 Nd1 O5 121.20(14) 2_567 . ? O10 Nd1 O5 123.26(16) . . ? O6 Nd1 O5 51.42(11) . . ? O1 Nd1 O5 75.43(12) . . ? O2 Nd1 O5 70.12(13) . . ? O3 Nd1 O9 136.94(15) 2_567 . ? O10 Nd1 O9 81.66(18) . . ? O6 Nd1 O9 71.33(14) . . ? O1 Nd1 O9 116.90(13) . . ? O2 Nd1 O9 67.69(13) . . ? O5 Nd1 O9 101.28(14) . . ? O3 Nd1 O12 69.16(14) 2_567 . ? O10 Nd1 O12 75.15(15) . . ? O6 Nd1 O12 73.72(13) . . ? O1 Nd1 O12 97.01(13) . . ? O2 Nd1 O12 133.03(13) . . ? O5 Nd1 O12 68.14(14) . . ? O9 Nd1 O12 141.25(13) . . ? O3 Nd1 O11 69.76(14) 2_567 . ? O10 Nd1 O11 77.05(15) . . ? O6 Nd1 O11 134.71(13) . . ? O1 Nd1 O11 90.61(13) . . ? O2 Nd1 O11 86.55(13) . . ? O5 Nd1 O11 156.67(14) . . ? O9 Nd1 O11 68.13(13) . . ? O12 Nd1 O11 133.20(13) . . ? C6 C1 C2 120.4(5) . . ? C6 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C1 C2 C3 120.3(5) . . ? C1 C2 C9 120.7(4) . . ? C3 C2 C9 119.0(5) . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 121.3(5) . . ? C3 C4 N1 120.5(4) . . ? C5 C4 N1 118.2(4) . . ? C4 C5 C6 119.3(5) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.0(5) . . ? C1 C6 C10 122.4(4) . . ? C5 C6 C10 117.6(4) . . ? N2 C7 N1 111.7(4) . . ? N2 C7 H7 124.1 . . ? N1 C7 H7 124.1 . . ? N3 C8 N1 110.1(5) . . ? N3 C8 H8 125.0 . . ? N1 C8 H8 125.0 . . ? O1 C9 O2 121.8(5) . . ? O1 C9 C2 119.3(5) . . ? O2 C9 C2 118.9(5) . . ? O4 C10 O3 124.5(5) . . ? O4 C10 C6 120.5(4) . . ? O3 C10 C6 115.0(4) . . ? C16 C11 C12 121.0(5) . . ? C16 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 C19 119.2(5) . . ? C11 C12 C19 121.0(4) . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 122.2(5) . . ? C13 C14 N4 118.3(5) . . ? C15 C14 N4 119.4(4) . . ? C14 C15 C16 119.2(4) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C11 C16 C15 119.0(5) . . ? C11 C16 C20 121.4(5) . . ? C15 C16 C20 119.6(4) . . ? N5 C17 N4 109.9(5) . . ? N5 C17 H17 125.1 . . ? N4 C17 H17 125.1 . . ? N6 C18 N4 110.7(5) . . ? N6 C18 H18 124.7 . . ? N4 C18 H18 124.7 . . ? O5 C19 O6 121.7(4) . . ? O5 C19 C12 119.3(4) . . ? O6 C19 C12 119.0(4) . . ? O7 C20 O8 125.5(5) . . ? O7 C20 C16 118.5(5) . . ? O8 C20 C16 116.0(5) . . ? C8 N1 C7 103.9(4) . . ? C8 N1 C4 126.8(4) . . ? C7 N1 C4 129.2(4) . . ? C7 N2 N3 105.8(4) . . ? C8 N3 N2 108.4(4) . . ? C8 N3 Ag1 128.8(4) . . ? N2 N3 Ag1 122.2(3) . . ? C18 N4 C17 105.3(4) . . ? C18 N4 C14 128.0(4) . . ? C17 N4 C14 126.6(4) . . ? C17 N5 N6 107.8(4) . . ? C17 N5 Ag1 130.7(4) . 1_454 ? N6 N5 Ag1 121.5(3) . 1_454 ? C18 N6 N5 106.3(4) . . ? C18 N6 Ag1 129.2(4) . 2_776 ? N5 N6 Ag1 124.5(3) . 2_776 ? C9 O1 Nd1 93.8(3) . . ? C9 O2 Nd1 92.3(3) . . ? C10 O3 Nd1 156.0(3) . 2_567 ? C19 O5 Nd1 92.5(3) . . ? C19 O6 Nd1 94.4(3) . . ? Nd1 O9 H9A 144.7 . . ? Nd1 O9 H9B 96.8 . . ? H9A O9 H9B 108.2 . . ? Nd1 O10 H10A 114.3 . . ? Nd1 O10 H10B 104.5 . . ? H10A O10 H10B 104.8 . . ? Nd1 O10 H10C 113.7 . . ? H10A O10 H10C 113.5 . . ? H10B O10 H10C 104.8 . . ? Nd1 O11 H11A 122.2 . . ? Nd1 O11 H11B 101.7 . . ? H11A O11 H11B 108.6 . . ? Nd1 O12 H12A 122.9 . . ? Nd1 O12 H12B 122.7 . . ? H12A O12 H12B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(8) . . . . ? C6 C1 C2 C9 179.0(4) . . . . ? C1 C2 C3 C4 -1.4(7) . . . . ? C9 C2 C3 C4 179.6(5) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C2 C3 C4 N1 -177.2(4) . . . . ? C3 C4 C5 C6 1.0(8) . . . . ? N1 C4 C5 C6 179.1(4) . . . . ? C2 C1 C6 C5 1.9(7) . . . . ? C2 C1 C6 C10 -177.0(5) . . . . ? C4 C5 C6 C1 -2.4(7) . . . . ? C4 C5 C6 C10 176.6(4) . . . . ? C1 C2 C9 O1 19.6(7) . . . . ? C3 C2 C9 O1 -161.4(5) . . . . ? C1 C2 C9 O2 -161.9(5) . . . . ? C3 C2 C9 O2 17.1(7) . . . . ? C1 C6 C10 O4 -173.3(5) . . . . ? C5 C6 C10 O4 7.7(7) . . . . ? C1 C6 C10 O3 6.9(7) . . . . ? C5 C6 C10 O3 -172.0(4) . . . . ? C16 C11 C12 C13 -0.6(8) . . . . ? C16 C11 C12 C19 179.5(5) . . . . ? C11 C12 C13 C14 0.6(8) . . . . ? C19 C12 C13 C14 -179.6(5) . . . . ? C12 C13 C14 C15 -1.3(8) . . . . ? C12 C13 C14 N4 -178.8(4) . . . . ? C13 C14 C15 C16 2.1(8) . . . . ? N4 C14 C15 C16 179.6(5) . . . . ? C12 C11 C16 C15 1.4(8) . . . . ? C12 C11 C16 C20 -179.7(5) . . . . ? C14 C15 C16 C11 -2.1(7) . . . . ? C14 C15 C16 C20 179.0(4) . . . . ? C13 C12 C19 O5 -178.8(5) . . . . ? C11 C12 C19 O5 1.0(8) . . . . ? C13 C12 C19 O6 0.3(7) . . . . ? C11 C12 C19 O6 -179.8(5) . . . . ? C11 C16 C20 O7 6.2(7) . . . . ? C15 C16 C20 O7 -174.9(5) . . . . ? C11 C16 C20 O8 -174.4(5) . . . . ? C15 C16 C20 O8 4.5(7) . . . . ? N3 C8 N1 C7 1.3(6) . . . . ? N3 C8 N1 C4 -175.8(5) . . . . ? N2 C7 N1 C8 -1.2(6) . . . . ? N2 C7 N1 C4 175.8(5) . . . . ? C3 C4 N1 C8 -176.0(5) . . . . ? C5 C4 N1 C8 5.9(7) . . . . ? C3 C4 N1 C7 7.6(8) . . . . ? C5 C4 N1 C7 -170.5(5) . . . . ? N1 C7 N2 N3 0.7(6) . . . . ? N1 C8 N3 N2 -0.9(6) . . . . ? N1 C8 N3 Ag1 -172.3(3) . . . . ? C7 N2 N3 C8 0.1(6) . . . . ? C7 N2 N3 Ag1 172.2(3) . . . . ? N5 Ag1 N3 C8 -8.8(7) 1_656 . . . ? N6 Ag1 N3 C8 175.0(5) 2_776 . . . ? N5 Ag1 N3 N2 -179.0(3) 1_656 . . . ? N6 Ag1 N3 N2 4.8(4) 2_776 . . . ? N6 C18 N4 C17 1.0(6) . . . . ? N6 C18 N4 C14 178.5(5) . . . . ? N5 C17 N4 C18 -0.5(6) . . . . ? N5 C17 N4 C14 -178.1(5) . . . . ? C13 C14 N4 C18 -126.2(6) . . . . ? C15 C14 N4 C18 56.2(8) . . . . ? C13 C14 N4 C17 50.8(7) . . . . ? C15 C14 N4 C17 -126.8(6) . . . . ? N4 C17 N5 N6 -0.1(6) . . . . ? N4 C17 N5 Ag1 -177.3(4) . . . 1_454 ? N4 C18 N6 N5 -1.1(6) . . . . ? N4 C18 N6 Ag1 178.4(4) . . . 2_776 ? C17 N5 N6 C18 0.7(6) . . . . ? Ag1 N5 N6 C18 178.3(4) 1_454 . . . ? C17 N5 N6 Ag1 -178.8(4) . . . 2_776 ? Ag1 N5 N6 Ag1 -1.3(6) 1_454 . . 2_776 ? O2 C9 O1 Nd1 -6.9(5) . . . . ? C2 C9 O1 Nd1 171.6(4) . . . . ? O3 Nd1 O1 C9 157.3(3) 2_567 . . . ? O10 Nd1 O1 C9 151.3(4) . . . . ? O6 Nd1 O1 C9 -62.5(4) . . . . ? O2 Nd1 O1 C9 3.7(3) . . . . ? O5 Nd1 O1 C9 -72.2(3) . . . . ? O9 Nd1 O1 C9 23.2(4) . . . . ? O12 Nd1 O1 C9 -137.4(3) . . . . ? O11 Nd1 O1 C9 88.9(3) . . . . ? O1 C9 O2 Nd1 6.9(5) . . . . ? C2 C9 O2 Nd1 -171.6(4) . . . . ? O3 Nd1 O2 C9 -32.4(3) 2_567 . . . ? O10 Nd1 O2 C9 -154.9(4) . . . . ? O6 Nd1 O2 C9 128.2(3) . . . . ? O1 Nd1 O2 C9 -3.7(3) . . . . ? O5 Nd1 O2 C9 83.1(3) . . . . ? O9 Nd1 O2 C9 -165.0(3) . . . . ? O12 Nd1 O2 C9 54.7(3) . . . . ? O11 Nd1 O2 C9 -97.2(3) . . . . ? O4 C10 O3 Nd1 4.2(12) . . . 2_567 ? C6 C10 O3 Nd1 -176.1(7) . . . 2_567 ? O6 C19 O5 Nd1 0.0(5) . . . . ? C12 C19 O5 Nd1 179.1(4) . . . . ? O3 Nd1 O5 C19 -132.5(3) 2_567 . . . ? O10 Nd1 O5 C19 -32.6(4) . . . . ? O6 Nd1 O5 C19 0.0(3) . . . . ? O1 Nd1 O5 C19 169.9(3) . . . . ? O2 Nd1 O5 C19 115.8(3) . . . . ? O9 Nd1 O5 C19 54.8(3) . . . . ? O12 Nd1 O5 C19 -86.2(3) . . . . ? O11 Nd1 O5 C19 115.0(4) . . . . ? O5 C19 O6 Nd1 0.0(6) . . . . ? C12 C19 O6 Nd1 -179.1(4) . . . . ? O3 Nd1 O6 C19 94.0(4) 2_567 . . . ? O10 Nd1 O6 C19 152.6(3) . . . . ? O1 Nd1 O6 C19 -12.1(4) . . . . ? O2 Nd1 O6 C19 -58.4(3) . . . . ? O5 Nd1 O6 C19 0.0(3) . . . . ? O9 Nd1 O6 C19 -122.3(3) . . . . ? O12 Nd1 O6 C19 74.7(3) . . . . ? O11 Nd1 O6 C19 -149.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.560 _refine_diff_density_min -1.636 _refine_diff_density_rms 0.171 data_2 _database_code_depnum_ccdc_archive 'CCDC 803743' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2011-03-04 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. SHELX97 Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common (EuAg(L01)2(H2O)4) _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Ag Eu N6 O12' _chemical_formula_sum 'C20 H18 Ag Eu N6 O12' _chemical_formula_weight 794.23 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.770(3) _cell_length_b 12.168(6) _cell_length_c 14.601(7) _cell_angle_alpha 79.594(17) _cell_angle_beta 77.637(17) _cell_angle_gamma 80.502(18) _cell_volume 1145.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 10518 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 3.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5288 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 10804 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5170 _reflns_number_gt 4964 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0352P)^2^+0.8889P] 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 5170 _refine_ls_number_parameters 388 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.086 _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 Eu1 Eu 0.162928(19) 0.016186(9) 0.695206(9) 0.01003(6) Uani 1 1 d D . . Ag1 Ag 0.26874(4) 0.423851(19) 0.007679(16) 0.01925(7) Uani 1 1 d . . . O1 O 0.1316(3) 0.05405(18) 0.85965(15) 0.0185(4) Uani 1 1 d . . . O2 O 0.4383(3) 0.05233(17) 0.77038(15) 0.0168(4) Uani 1 1 d . . . O3 O 0.1062(3) 0.06789(18) 1.20842(16) 0.0209(4) Uani 1 1 d . . . O4 O 0.3036(3) 0.17653(16) 1.24530(15) 0.0177(4) Uani 1 1 d . . . O5 O 0.1715(4) 0.22443(16) 0.67783(15) 0.0198(4) Uani 1 1 d . . . O6 O 0.2379(3) 0.14936(16) 0.54654(15) 0.0181(4) Uani 1 1 d . . . O7 O 0.1868(4) 0.64348(17) 0.65679(15) 0.0198(4) Uani 1 1 d . . . O8 O 0.2270(4) 0.74707(16) 0.51194(16) 0.0229(5) Uani 1 1 d . . . O9 O 0.5153(4) -0.0460(2) 0.60598(17) 0.0239(5) Uani 1 1 d D . . H11 H 0.577(6) -0.075(3) 0.559(2) 0.029 Uiso 1 1 d D . . H12 H 0.599(5) -0.072(3) 0.641(3) 0.029 Uiso 1 1 d D . . O10 O 0.0658(5) -0.0732(2) 0.5825(2) 0.0412(8) Uani 1 1 d D . . H13 H 0.133(6) -0.127(3) 0.559(3) 0.049 Uiso 1 1 d D . . H14 H 0.032(17) -0.036(3) 0.533(4) 0.049 Uiso 0.50 1 d PD . . H14B H -0.041(6) -0.102(6) 0.596(3) 0.049 Uiso 0.50 1 d PD . . O11 O 0.2808(4) -0.19480(18) 0.74958(18) 0.0215(5) Uani 1 1 d D . . H15 H 0.256(6) -0.241(3) 0.720(3) 0.026 Uiso 1 1 d D . . H16 H 0.406(3) -0.206(3) 0.743(3) 0.026 Uiso 1 1 d D . . O12 O -0.1778(4) 0.12820(18) 0.66647(17) 0.0213(4) Uani 1 1 d D . . H17 H -0.192(6) 0.164(3) 0.6139(18) 0.026 Uiso 1 1 d D . . H18 H -0.281(4) 0.097(3) 0.687(3) 0.026 Uiso 1 1 d D . . N11 N 0.8076(4) 0.26496(19) 0.94014(18) 0.0136(4) Uani 1 1 d . . . N12 N 1.0450(4) 0.3581(2) 0.95384(19) 0.0170(5) Uani 1 1 d . . . N13 N 1.0629(4) 0.3540(2) 0.85757(18) 0.0167(5) Uani 1 1 d . . . N111 N 0.3630(4) 0.47417(18) 0.27921(18) 0.0129(4) Uani 1 1 d . . . N112 N 0.5156(4) 0.5111(2) 0.13150(18) 0.0176(5) Uani 1 1 d . . . N113 N 0.3510(4) 0.4550(2) 0.13495(18) 0.0153(5) Uani 1 1 d . . . C1 C 0.6302(4) 0.2084(2) 0.9646(2) 0.0122(5) Uani 1 1 d . . . C2 C 0.5652(4) 0.1657(2) 0.8958(2) 0.0133(5) Uani 1 1 d . . . H1 H 0.6405 0.1706 0.8327 0.016 Uiso 1 1 calc R . . C3 C 0.3862(4) 0.1153(2) 0.9216(2) 0.0123(5) Uani 1 1 d . . . C4 C 0.2793(4) 0.1034(2) 1.0153(2) 0.0127(5) Uani 1 1 d . . . H2 H 0.1594 0.0676 1.0321 0.015 Uiso 1 1 calc R . . C5 C 0.3501(4) 0.1447(2) 1.0840(2) 0.0118(5) Uani 1 1 d . . . C6 C 0.5238(4) 0.1985(2) 1.0578(2) 0.0133(5) Uani 1 1 d . . . H3 H 0.5703 0.2286 1.1038 0.016 Uiso 1 1 calc R . . C11 C 0.8939(4) 0.3050(2) 1.0014(2) 0.0164(5) Uani 1 1 d . . . H4 H 0.8507 0.2957 1.0683 0.020 Uiso 1 1 calc R . . C12 C 0.9202(4) 0.2970(2) 0.8524(2) 0.0151(5) Uani 1 1 d . . . H5 H 0.8970 0.2798 0.7949 0.018 Uiso 1 1 calc R . . C31 C 0.3134(4) 0.0710(2) 0.8462(2) 0.0121(5) Uani 1 1 d . . . C51 C 0.2460(4) 0.1293(2) 1.1877(2) 0.0127(5) Uani 1 1 d . . . C101 C 0.3145(4) 0.4641(2) 0.3808(2) 0.0124(5) Uani 1 1 d . . . C102 C 0.2897(4) 0.3585(2) 0.4333(2) 0.0131(5) Uani 1 1 d . . . H6 H 0.3059 0.2943 0.4025 0.016 Uiso 1 1 calc R . . C103 C 0.2407(4) 0.3484(2) 0.5320(2) 0.0119(5) Uani 1 1 d . . . C104 C 0.2164(4) 0.4439(2) 0.5764(2) 0.0127(5) Uani 1 1 d . . . H7 H 0.1833 0.4369 0.6436 0.015 Uiso 1 1 calc R . . C105 C 0.2407(4) 0.5499(2) 0.5221(2) 0.0126(5) Uani 1 1 d . . . C106 C 0.2904(4) 0.5596(2) 0.4233(2) 0.0127(5) Uani 1 1 d . . . H8 H 0.3076 0.6310 0.3857 0.015 Uiso 1 1 calc R . . C111 C 0.5184(5) 0.5209(2) 0.2188(2) 0.0189(6) Uani 1 1 d . . . H9 H 0.6159 0.5560 0.2373 0.023 Uiso 1 1 calc R . . C112 C 0.2623(5) 0.4338(2) 0.2240(2) 0.0151(5) Uani 1 1 d . . . H10 H 0.1453 0.3959 0.2466 0.018 Uiso 1 1 calc R . . C131 C 0.2167(4) 0.2338(2) 0.5893(2) 0.0135(5) Uani 1 1 d . . . C151 C 0.2153(4) 0.6547(2) 0.5685(2) 0.0144(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01207(9) 0.01080(8) 0.00753(9) -0.00076(5) -0.00092(6) -0.00432(5) Ag1 0.02048(13) 0.02766(12) 0.01319(13) -0.00437(9) -0.00331(10) -0.01188(10) O1 0.0186(10) 0.0281(10) 0.0122(10) -0.0033(8) -0.0031(9) -0.0122(9) O2 0.0135(9) 0.0244(10) 0.0151(10) -0.0091(8) -0.0034(9) -0.0028(8) O3 0.0173(10) 0.0295(11) 0.0170(11) -0.0009(8) -0.0006(9) -0.0130(9) O4 0.0209(10) 0.0203(9) 0.0130(10) -0.0042(7) -0.0039(9) -0.0033(8) O5 0.0343(12) 0.0149(9) 0.0097(10) 0.0008(7) -0.0006(9) -0.0090(9) O6 0.0265(11) 0.0133(9) 0.0138(10) -0.0021(7) 0.0002(9) -0.0063(8) O7 0.0271(12) 0.0183(9) 0.0149(11) -0.0034(8) -0.0039(9) -0.0050(9) O8 0.0401(14) 0.0128(9) 0.0152(11) -0.0020(8) -0.0056(10) -0.0012(9) O9 0.0214(11) 0.0328(12) 0.0138(11) -0.0063(9) 0.0007(10) 0.0045(9) O10 0.0447(16) 0.0406(14) 0.0518(19) -0.0352(14) -0.0353(15) 0.0211(13) O11 0.0211(11) 0.0185(10) 0.0263(13) -0.0053(8) -0.0071(10) -0.0012(9) O12 0.0175(10) 0.0248(10) 0.0192(12) 0.0037(8) -0.0038(10) -0.0034(8) N11 0.0127(11) 0.0160(10) 0.0131(12) -0.0033(8) -0.0021(10) -0.0045(9) N12 0.0164(12) 0.0209(11) 0.0154(13) -0.0032(9) -0.0027(10) -0.0071(9) N13 0.0171(12) 0.0215(11) 0.0129(12) -0.0043(9) -0.0009(10) -0.0069(10) N111 0.0153(11) 0.0131(10) 0.0104(11) -0.0001(8) -0.0022(10) -0.0041(9) N112 0.0175(12) 0.0245(12) 0.0120(12) -0.0003(9) -0.0018(10) -0.0108(10) N113 0.0172(12) 0.0177(11) 0.0126(12) -0.0019(9) -0.0028(10) -0.0068(9) C1 0.0107(12) 0.0122(11) 0.0144(13) -0.0018(9) -0.0020(11) -0.0042(9) C2 0.0150(13) 0.0150(12) 0.0096(13) -0.0009(9) -0.0014(11) -0.0038(10) C3 0.0132(12) 0.0117(11) 0.0134(13) -0.0013(9) -0.0048(11) -0.0030(10) C4 0.0115(12) 0.0131(11) 0.0141(14) -0.0003(9) -0.0037(11) -0.0033(10) C5 0.0111(12) 0.0119(11) 0.0120(13) -0.0003(9) -0.0032(11) -0.0008(9) C6 0.0139(13) 0.0153(12) 0.0124(13) -0.0027(9) -0.0035(11) -0.0043(10) C11 0.0159(13) 0.0227(13) 0.0134(14) -0.0039(10) -0.0029(12) -0.0089(11) C12 0.0143(13) 0.0184(13) 0.0131(14) -0.0042(10) -0.0005(11) -0.0047(10) C31 0.0162(13) 0.0104(11) 0.0109(13) -0.0012(9) -0.0045(11) -0.0027(10) C51 0.0105(12) 0.0144(11) 0.0118(13) 0.0004(9) -0.0012(11) -0.0012(10) C101 0.0125(12) 0.0167(12) 0.0079(12) -0.0006(9) -0.0018(11) -0.0029(10) C102 0.0133(12) 0.0122(11) 0.0139(14) -0.0019(10) -0.0019(11) -0.0030(10) C103 0.0111(12) 0.0129(11) 0.0110(13) -0.0003(9) -0.0003(11) -0.0041(9) C104 0.0129(12) 0.0152(12) 0.0096(13) -0.0005(9) -0.0023(11) -0.0020(10) C105 0.0097(12) 0.0136(12) 0.0145(14) -0.0022(10) -0.0026(11) -0.0004(10) C106 0.0132(12) 0.0117(11) 0.0134(13) -0.0001(9) -0.0032(11) -0.0036(10) C111 0.0198(14) 0.0227(14) 0.0162(15) -0.0005(11) -0.0041(12) -0.0103(12) C112 0.0181(14) 0.0153(12) 0.0131(14) -0.0013(10) -0.0032(12) -0.0063(10) C131 0.0141(12) 0.0142(12) 0.0124(13) -0.0008(10) -0.0031(11) -0.0031(10) C151 0.0140(13) 0.0137(12) 0.0161(14) -0.0042(10) -0.0025(12) -0.0019(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 Eu1 O3 2.311(2) 2_557 ? Eu1 O10 2.381(2) . ? Eu1 O6 2.475(2) . ? Eu1 O1 2.484(2) . ? Eu1 O2 2.489(2) . ? Eu1 O5 2.510(2) . ? Eu1 O9 2.528(3) . ? Eu1 O12 2.555(2) . ? Eu1 O11 2.592(2) . ? Eu1 C31 2.839(3) . ? Eu1 C131 2.852(3) . ? Ag1 N113 2.162(3) . ? Ag1 N12 2.165(2) 1_454 ? Ag1 N112 2.327(3) 2_665 ? O1 C31 1.250(4) . ? O2 C31 1.272(4) . ? O3 C51 1.255(4) . ? O3 Eu1 2.311(2) 2_557 ? O4 C51 1.257(3) . ? O5 C131 1.251(4) . ? O6 C131 1.269(3) . ? O7 C151 1.247(4) . ? O8 C151 1.272(4) . ? O9 H11 0.833(19) . ? O9 H12 0.827(19) . ? O10 H13 0.813(19) . ? O10 H14 0.83(2) . ? O10 H14B 0.829(19) . ? O11 H15 0.821(19) . ? O11 H16 0.821(19) . ? O12 H17 0.826(19) . ? O12 H18 0.822(19) . ? N11 C11 1.362(4) . ? N11 C12 1.369(4) . ? N11 C1 1.430(3) . ? N12 C11 1.303(4) . ? N12 N13 1.394(4) . ? N12 Ag1 2.165(2) 1_656 ? N13 C12 1.301(4) . ? N111 C111 1.352(4) . ? N111 C112 1.358(4) . ? N111 C101 1.437(4) . ? N112 C111 1.306(4) . ? N112 N113 1.387(3) . ? N112 Ag1 2.327(3) 2_665 ? N113 C112 1.309(4) . ? C1 C2 1.388(4) . ? C1 C6 1.391(4) . ? C2 C3 1.397(4) . ? C2 H1 0.9500 . ? C3 C4 1.398(4) . ? C3 C31 1.510(4) . ? C4 C5 1.399(4) . ? C4 H2 0.9500 . ? C5 C6 1.389(4) . ? C5 C51 1.519(4) . ? C6 H3 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? C101 C106 1.384(4) . ? C101 C102 1.388(4) . ? C102 C103 1.395(4) . ? C102 H6 0.9500 . ? C103 C104 1.401(4) . ? C103 C131 1.506(4) . ? C104 C105 1.401(4) . ? C104 H7 0.9500 . ? C105 C106 1.397(4) . ? C105 C151 1.519(4) . ? C106 H8 0.9500 . ? C111 H9 0.9500 . ? C112 H10 0.9500 . ? 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 Eu1 O10 80.54(11) 2_557 . ? O3 Eu1 O6 140.24(8) 2_557 . ? O10 Eu1 O6 77.45(10) . . ? O3 Eu1 O1 71.05(8) 2_557 . ? O10 Eu1 O1 151.46(10) . . ? O6 Eu1 O1 127.11(7) . . ? O3 Eu1 O2 118.06(8) 2_557 . ? O10 Eu1 O2 148.45(9) . . ? O6 Eu1 O2 97.33(8) . . ? O1 Eu1 O2 52.56(7) . . ? O3 Eu1 O5 121.36(8) 2_557 . ? O10 Eu1 O5 124.10(9) . . ? O6 Eu1 O5 52.37(7) . . ? O1 Eu1 O5 75.31(7) . . ? O2 Eu1 O5 70.13(7) . . ? O3 Eu1 O9 137.46(8) 2_557 . ? O10 Eu1 O9 81.64(10) . . ? O6 Eu1 O9 70.85(8) . . ? O1 Eu1 O9 117.77(8) . . ? O2 Eu1 O9 67.45(8) . . ? O5 Eu1 O9 100.58(8) . . ? O3 Eu1 O12 69.27(8) 2_557 . ? O10 Eu1 O12 75.33(9) . . ? O6 Eu1 O12 73.31(8) . . ? O1 Eu1 O12 96.55(8) . . ? O2 Eu1 O12 133.57(7) . . ? O5 Eu1 O12 68.59(8) . . ? O9 Eu1 O12 140.70(8) . . ? O3 Eu1 O11 69.90(8) 2_557 . ? O10 Eu1 O11 77.73(9) . . ? O6 Eu1 O11 134.88(8) . . ? O1 Eu1 O11 89.72(8) . . ? O2 Eu1 O11 85.05(7) . . ? O5 Eu1 O11 155.19(7) . . ? O9 Eu1 O11 68.70(8) . . ? O12 Eu1 O11 133.89(7) . . ? O3 Eu1 C31 95.24(9) 2_557 . ? O10 Eu1 C31 166.71(8) . . ? O6 Eu1 C31 112.69(8) . . ? O1 Eu1 C31 26.08(8) . . ? O2 Eu1 C31 26.60(8) . . ? O5 Eu1 C31 68.84(7) . . ? O9 Eu1 C31 93.41(9) . . ? O12 Eu1 C31 115.13(8) . . ? O11 Eu1 C31 88.97(8) . . ? O3 Eu1 C131 135.90(8) 2_557 . ? O10 Eu1 C131 101.23(10) . . ? O6 Eu1 C131 26.38(7) . . ? O1 Eu1 C131 101.04(8) . . ? O2 Eu1 C131 83.05(8) . . ? O5 Eu1 C131 25.99(8) . . ? O9 Eu1 C131 85.44(8) . . ? O12 Eu1 C131 68.74(8) . . ? O11 Eu1 C131 154.06(8) . . ? C31 Eu1 C131 90.60(8) . . ? N113 Ag1 N12 144.15(10) . 1_454 ? N113 Ag1 N112 113.84(9) . 2_665 ? N12 Ag1 N112 101.94(10) 1_454 2_665 ? C31 O1 Eu1 93.02(18) . . ? C31 O2 Eu1 92.24(17) . . ? C51 O3 Eu1 156.0(2) . 2_557 ? C131 O5 Eu1 92.44(16) . . ? C131 O6 Eu1 93.61(18) . . ? Eu1 O9 H11 143(3) . . ? Eu1 O9 H12 114(3) . . ? H11 O9 H12 98(4) . . ? Eu1 O10 H13 125(4) . . ? Eu1 O10 H14 121(2) . . ? H13 O10 H14 98(7) . . ? Eu1 O10 H14B 121(2) . . ? H13 O10 H14B 94(3) . . ? H14 O10 H14B 91(8) . . ? Eu1 O11 H15 117(3) . . ? Eu1 O11 H16 110(3) . . ? H15 O11 H16 103(4) . . ? Eu1 O12 H17 122(3) . . ? Eu1 O12 H18 117(3) . . ? H17 O12 H18 106(4) . . ? C11 N11 C12 104.8(2) . . ? C11 N11 C1 126.1(3) . . ? C12 N11 C1 129.0(2) . . ? C11 N12 N13 108.9(2) . . ? C11 N12 Ag1 128.5(2) . 1_656 ? N13 N12 Ag1 122.08(18) . 1_656 ? C12 N13 N12 105.5(2) . . ? C111 N111 C112 105.6(3) . . ? C111 N111 C101 128.4(2) . . ? C112 N111 C101 126.0(2) . . ? C111 N112 N113 106.7(2) . . ? C111 N112 Ag1 128.9(2) . 2_665 ? N113 N112 Ag1 124.33(19) . 2_665 ? C112 N113 N112 107.5(2) . . ? C112 N113 Ag1 130.6(2) . . ? N112 N113 Ag1 121.82(19) . . ? C2 C1 C6 121.0(3) . . ? C2 C1 N11 120.2(3) . . ? C6 C1 N11 118.8(2) . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H1 120.8 . . ? C3 C2 H1 120.8 . . ? C2 C3 C4 121.1(2) . . ? C2 C3 C31 118.3(3) . . ? C4 C3 C31 120.6(2) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H2 120.2 . . ? C5 C4 H2 120.2 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 C51 118.7(2) . . ? C4 C5 C51 121.9(3) . . ? C5 C6 C1 120.4(3) . . ? C5 C6 H3 119.8 . . ? C1 C6 H3 119.8 . . ? N12 C11 N11 109.4(3) . . ? N12 C11 H4 125.3 . . ? N11 C11 H4 125.3 . . ? N13 C12 N11 111.4(3) . . ? N13 C12 H5 124.3 . . ? N11 C12 H5 124.3 . . ? O1 C31 O2 121.6(3) . . ? O1 C31 C3 119.1(3) . . ? O2 C31 C3 119.2(3) . . ? O1 C31 Eu1 60.90(15) . . ? O2 C31 Eu1 61.16(14) . . ? C3 C31 Eu1 172.85(17) . . ? O3 C51 O4 125.2(3) . . ? O3 C51 C5 115.3(2) . . ? O4 C51 C5 119.5(2) . . ? C106 C101 C102 122.1(3) . . ? C106 C101 N111 119.3(2) . . ? C102 C101 N111 118.6(2) . . ? C101 C102 C103 118.8(2) . . ? C101 C102 H6 120.6 . . ? C103 C102 H6 120.6 . . ? C102 C103 C104 120.0(2) . . ? C102 C103 C131 119.1(2) . . ? C104 C103 C131 120.9(3) . . ? C103 C104 C105 120.2(3) . . ? C103 C104 H7 119.9 . . ? C105 C104 H7 119.9 . . ? C106 C105 C104 119.6(2) . . ? C106 C105 C151 119.1(2) . . ? C104 C105 C151 121.3(3) . . ? C101 C106 C105 119.2(2) . . ? C101 C106 H8 120.4 . . ? C105 C106 H8 120.4 . . ? N112 C111 N111 110.5(3) . . ? N112 C111 H9 124.7 . . ? N111 C111 H9 124.7 . . ? N113 C112 N111 109.6(3) . . ? N113 C112 H10 125.2 . . ? N111 C112 H10 125.2 . . ? O5 C131 O6 121.6(2) . . ? O5 C131 C103 119.3(2) . . ? O6 C131 C103 119.1(3) . . ? O5 C131 Eu1 61.56(14) . . ? O6 C131 Eu1 60.01(15) . . ? C103 C131 Eu1 178.45(19) . . ? O7 C151 O8 126.0(3) . . ? O7 C151 C105 118.4(2) . . ? O8 C151 C105 115.6(3) . . ? 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 Eu1 O1 C31 157.03(18) 2_557 . . . ? O10 Eu1 O1 C31 151.26(18) . . . . ? O6 Eu1 O1 C31 -63.55(19) . . . . ? O2 Eu1 O1 C31 4.26(15) . . . . ? O5 Eu1 O1 C31 -71.75(16) . . . . ? O9 Eu1 O1 C31 22.63(18) . . . . ? O12 Eu1 O1 C31 -137.55(16) . . . . ? O11 Eu1 O1 C31 88.24(17) . . . . ? C131 Eu1 O1 C31 -68.01(17) . . . . ? O3 Eu1 O2 C31 -33.54(18) 2_557 . . . ? O10 Eu1 O2 C31 -154.4(2) . . . . ? O6 Eu1 O2 C31 127.71(16) . . . . ? O1 Eu1 O2 C31 -4.18(14) . . . . ? O5 Eu1 O2 C31 82.21(16) . . . . ? O9 Eu1 O2 C31 -166.60(17) . . . . ? O12 Eu1 O2 C31 53.79(19) . . . . ? O11 Eu1 O2 C31 -97.63(16) . . . . ? C131 Eu1 O2 C31 105.47(16) . . . . ? O3 Eu1 O5 C131 -131.97(17) 2_557 . . . ? O10 Eu1 O5 C131 -31.6(2) . . . . ? O6 Eu1 O5 C131 -0.15(16) . . . . ? O1 Eu1 O5 C131 171.59(19) . . . . ? O2 Eu1 O5 C131 116.59(19) . . . . ? O9 Eu1 O5 C131 55.42(18) . . . . ? O12 Eu1 O5 C131 -85.15(18) . . . . ? O11 Eu1 O5 C131 117.0(2) . . . . ? C31 Eu1 O5 C131 145.0(2) . . . . ? O3 Eu1 O6 C131 95.94(19) 2_557 . . . ? O10 Eu1 O6 C131 153.89(19) . . . . ? O1 Eu1 O6 C131 -9.9(2) . . . . ? O2 Eu1 O6 C131 -57.72(17) . . . . ? O5 Eu1 O6 C131 0.15(16) . . . . ? O9 Eu1 O6 C131 -120.73(18) . . . . ? O12 Eu1 O6 C131 75.66(17) . . . . ? O11 Eu1 O6 C131 -148.04(16) . . . . ? C31 Eu1 O6 C131 -35.14(19) . . . . ? C11 N12 N13 C12 -0.5(3) . . . . ? Ag1 N12 N13 C12 171.80(18) 1_656 . . . ? C111 N112 N113 C112 0.0(3) . . . . ? Ag1 N112 N113 C112 -178.46(19) 2_665 . . . ? C111 N112 N113 Ag1 177.1(2) . . . . ? Ag1 N112 N113 Ag1 -1.4(3) 2_665 . . . ? N12 Ag1 N113 C112 1.4(3) 1_454 . . . ? N112 Ag1 N113 C112 177.6(2) 2_665 . . . ? N12 Ag1 N113 N112 -174.87(18) 1_454 . . . ? N112 Ag1 N113 N112 1.3(3) 2_665 . . . ? C11 N11 C1 C2 -176.1(3) . . . . ? C12 N11 C1 C2 8.3(4) . . . . ? C11 N11 C1 C6 4.6(4) . . . . ? C12 N11 C1 C6 -171.0(3) . . . . ? C6 C1 C2 C3 2.0(4) . . . . ? N11 C1 C2 C3 -177.3(2) . . . . ? C1 C2 C3 C4 -2.8(4) . . . . ? C1 C2 C3 C31 178.8(2) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C31 C3 C4 C5 179.7(2) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C3 C4 C5 C51 -177.0(2) . . . . ? C4 C5 C6 C1 -1.8(4) . . . . ? C51 C5 C6 C1 176.3(2) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? N11 C1 C6 C5 179.6(2) . . . . ? N13 N12 C11 N11 -0.1(3) . . . . ? Ag1 N12 C11 N11 -171.78(18) 1_656 . . . ? C12 N11 C11 N12 0.7(3) . . . . ? C1 N11 C11 N12 -175.8(2) . . . . ? N12 N13 C12 N11 0.9(3) . . . . ? C11 N11 C12 N13 -1.0(3) . . . . ? C1 N11 C12 N13 175.3(2) . . . . ? Eu1 O1 C31 O2 -7.8(3) . . . . ? Eu1 O1 C31 C3 171.8(2) . . . . ? Eu1 O2 C31 O1 7.8(3) . . . . ? Eu1 O2 C31 C3 -171.8(2) . . . . ? C2 C3 C31 O1 -160.8(2) . . . . ? C4 C3 C31 O1 20.8(4) . . . . ? C2 C3 C31 O2 18.8(4) . . . . ? C4 C3 C31 O2 -159.6(2) . . . . ? O3 Eu1 C31 O1 -21.75(17) 2_557 . . . ? O10 Eu1 C31 O1 -92.5(5) . . . . ? O6 Eu1 C31 O1 129.30(16) . . . . ? O2 Eu1 C31 O1 -172.4(3) . . . . ? O5 Eu1 C31 O1 99.91(17) . . . . ? O9 Eu1 C31 O1 -160.06(16) . . . . ? O12 Eu1 C31 O1 47.78(18) . . . . ? O11 Eu1 C31 O1 -91.46(17) . . . . ? C131 Eu1 C31 O1 114.48(17) . . . . ? O3 Eu1 C31 O2 150.68(16) 2_557 . . . ? O10 Eu1 C31 O2 79.9(5) . . . . ? O6 Eu1 C31 O2 -58.27(17) . . . . ? O1 Eu1 C31 O2 172.4(3) . . . . ? O5 Eu1 C31 O2 -87.65(16) . . . . ? O9 Eu1 C31 O2 12.38(16) . . . . ? O12 Eu1 C31 O2 -139.78(15) . . . . ? O11 Eu1 C31 O2 80.97(16) . . . . ? C131 Eu1 C31 O2 -73.09(16) . . . . ? Eu1 O3 C51 O4 7.7(7) 2_557 . . . ? Eu1 O3 C51 C5 -172.6(4) 2_557 . . . ? C6 C5 C51 O3 -171.3(2) . . . . ? C4 C5 C51 O3 6.7(4) . . . . ? C6 C5 C51 O4 8.4(4) . . . . ? C4 C5 C51 O4 -173.6(2) . . . . ? C111 N111 C101 C106 54.1(4) . . . . ? C112 N111 C101 C106 -128.4(3) . . . . ? C111 N111 C101 C102 -127.0(3) . . . . ? C112 N111 C101 C102 50.5(4) . . . . ? C106 C101 C102 C103 -0.5(4) . . . . ? N111 C101 C102 C103 -179.4(2) . . . . ? C101 C102 C103 C104 0.3(4) . . . . ? C101 C102 C103 C131 -179.1(2) . . . . ? C102 C103 C104 C105 0.1(4) . . . . ? C131 C103 C104 C105 179.5(2) . . . . ? C103 C104 C105 C106 -0.3(4) . . . . ? C103 C104 C105 C151 -179.9(2) . . . . ? C102 C101 C106 C105 0.3(4) . . . . ? N111 C101 C106 C105 179.2(2) . . . . ? C104 C105 C106 C101 0.1(4) . . . . ? C151 C105 C106 C101 179.7(2) . . . . ? N113 N112 C111 N111 -0.2(3) . . . . ? Ag1 N112 C111 N111 178.25(19) 2_665 . . . ? C112 N111 C111 N112 0.2(3) . . . . ? C101 N111 C111 N112 178.1(3) . . . . ? N112 N113 C112 N111 0.1(3) . . . . ? Ag1 N113 C112 N111 -176.57(18) . . . . ? C111 N111 C112 N113 -0.2(3) . . . . ? C101 N111 C112 N113 -178.2(2) . . . . ? Eu1 O5 C131 O6 0.3(3) . . . . ? Eu1 O5 C131 C103 178.5(2) . . . . ? Eu1 O6 C131 O5 -0.3(3) . . . . ? Eu1 O6 C131 C103 -178.5(2) . . . . ? C102 C103 C131 O5 -179.6(3) . . . . ? C104 C103 C131 O5 1.0(4) . . . . ? C102 C103 C131 O6 -1.3(4) . . . . ? C104 C103 C131 O6 179.3(3) . . . . ? O3 Eu1 C131 O5 65.8(2) 2_557 . . . ? O10 Eu1 C131 O5 153.75(18) . . . . ? O6 Eu1 C131 O5 179.7(3) . . . . ? O1 Eu1 C131 O5 -8.29(19) . . . . ? O2 Eu1 C131 O5 -57.92(18) . . . . ? O9 Eu1 C131 O5 -125.72(18) . . . . ? O12 Eu1 C131 O5 84.50(18) . . . . ? O11 Eu1 C131 O5 -121.2(2) . . . . ? C31 Eu1 C131 O5 -32.35(18) . . . . ? O3 Eu1 C131 O6 -113.92(18) 2_557 . . . ? O10 Eu1 C131 O6 -25.98(19) . . . . ? O1 Eu1 C131 O6 171.98(16) . . . . ? O2 Eu1 C131 O6 122.35(17) . . . . ? O5 Eu1 C131 O6 -179.7(3) . . . . ? O9 Eu1 C131 O6 54.55(17) . . . . ? O12 Eu1 C131 O6 -95.23(18) . . . . ? O11 Eu1 C131 O6 59.0(3) . . . . ? C31 Eu1 C131 O6 147.92(17) . . . . ? C106 C105 C151 O7 -174.4(3) . . . . ? C104 C105 C151 O7 5.1(4) . . . . ? C106 C105 C151 O8 5.1(4) . . . . ? C104 C105 C151 O8 -175.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.622 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.225 data_3 _database_code_depnum_ccdc_archive 'CCDC 803744' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2011-03-04 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Ag N6 O12 Tb' _chemical_formula_sum 'C20 H18 Ag N6 O12 Tb' _chemical_formula_weight 801.19 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' Ag Ag -0.8971 1.1015 '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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.755(3) _cell_length_b 12.104(4) _cell_length_c 14.524(5) _cell_angle_alpha 79.526(13) _cell_angle_beta 77.666(14) _cell_angle_gamma 80.439(15) _cell_volume 1130.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 10280 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 4.052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6874 _exptl_absorpt_correction_T_max 0.8547 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 10769 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5148 _reflns_number_gt 4829 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0250P)^2^+0.9202P] 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 5148 _refine_ls_number_parameters 388 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.839335(17) 0.982873(10) 0.804873(8) 0.01069(5) Uani 1 1 d D . . Ag1 Ag -0.26870(3) 0.576259(19) 0.492476(14) 0.01890(6) Uani 1 1 d . . . O1 O 0.8720(3) 0.94466(17) 0.64147(13) 0.0178(4) Uani 1 1 d . . . O2 O 0.5644(3) 0.94831(17) 0.73032(14) 0.0174(4) Uani 1 1 d . . . O3 O 0.8948(3) 0.93300(18) 0.29076(14) 0.0210(4) Uani 1 1 d . . . O4 O 0.6978(3) 0.82447(16) 0.25400(13) 0.0174(4) Uani 1 1 d . . . O5 O 0.8297(3) 0.77649(16) 0.82119(13) 0.0202(4) Uani 1 1 d . . . O6 O 0.7636(3) 0.85136(16) 0.95302(14) 0.0191(4) Uani 1 1 d . . . O7 O 0.8127(3) 0.35571(17) 0.84192(14) 0.0198(4) Uani 1 1 d . . . O8 O 0.7729(3) 0.25206(16) 0.98730(15) 0.0230(4) Uani 1 1 d . . . O9 O 1.1774(3) 0.87159(18) 0.83272(15) 0.0208(4) Uani 1 1 d D . . H11 H 1.282(4) 0.900(3) 0.807(2) 0.025 Uiso 1 1 d D . . H12 H 1.185(5) 0.832(3) 0.8844(14) 0.025 Uiso 1 1 d D . . O10 O 0.9353(4) 1.0719(2) 0.9164(2) 0.0393(7) Uani 1 1 d D . . H13 H 0.889(6) 1.130(2) 0.941(3) 0.047 Uiso 1 1 d D . . H14 H 0.972(14) 1.026(4) 0.961(3) 0.047 Uiso 0.50 1 d PD . . H14B H 1.048(5) 1.088(5) 0.884(3) 0.047 Uiso 0.50 1 d PD . . O11 O 0.7210(3) 1.19077(19) 0.75042(17) 0.0246(5) Uani 1 1 d D . . H15 H 0.599(3) 1.193(3) 0.761(3) 0.030 Uiso 1 1 d D . . H16 H 0.742(6) 1.235(3) 0.784(2) 0.030 Uiso 1 1 d D . . O12 O 0.4895(3) 1.0447(2) 0.89415(16) 0.0270(5) Uani 1 1 d D . . H17 H 0.408(5) 1.067(3) 0.858(2) 0.032 Uiso 1 1 d D . . H18 H 0.447(6) 1.068(3) 0.9466(18) 0.032 Uiso 1 1 d D . . N11 N 0.1943(3) 0.73479(19) 0.55955(15) 0.0123(4) Uani 1 1 d . . . N12 N -0.0443(3) 0.6413(2) 0.54663(17) 0.0166(5) Uani 1 1 d . . . N13 N -0.0610(3) 0.6456(2) 0.64263(17) 0.0166(5) Uani 1 1 d . . . N111 N 0.6371(3) 0.52615(19) 1.22046(16) 0.0126(4) Uani 1 1 d . . . N112 N 0.4846(3) 0.4890(2) 1.36842(16) 0.0172(5) Uani 1 1 d . . . N113 N 0.6482(3) 0.54559(19) 1.36513(16) 0.0153(4) Uani 1 1 d . . . C1 C 0.3720(4) 0.7918(2) 0.53579(19) 0.0121(5) Uani 1 1 d . . . C2 C 0.4374(4) 0.8342(2) 0.60414(18) 0.0135(5) Uani 1 1 d . . . H1 H 0.3625 0.8286 0.6677 0.016 Uiso 1 1 calc R . . C3 C 0.6153(4) 0.8855(2) 0.57858(18) 0.0120(5) Uani 1 1 d . . . C4 C 0.7227(4) 0.8971(2) 0.48417(18) 0.0124(5) Uani 1 1 d . . . H2 H 0.8433 0.9328 0.4671 0.015 Uiso 1 1 calc R . . C5 C 0.6510(4) 0.8558(2) 0.41562(18) 0.0124(5) Uani 1 1 d . . . C6 C 0.4769(4) 0.8019(2) 0.44218(19) 0.0129(5) Uani 1 1 d . . . H3 H 0.4295 0.7718 0.3961 0.015 Uiso 1 1 calc R . . C11 C 0.1070(4) 0.6955(2) 0.49894(19) 0.0164(5) Uani 1 1 d . . . H4 H 0.1492 0.7057 0.4316 0.020 Uiso 1 1 calc R . . C12 C 0.0825(4) 0.7024(2) 0.64790(19) 0.0150(5) Uani 1 1 d . . . H5 H 0.1067 0.7192 0.7056 0.018 Uiso 1 1 calc R . . C31 C 0.6894(4) 0.9291(2) 0.65391(18) 0.0119(5) Uani 1 1 d . . . C51 C 0.7560(4) 0.8714(2) 0.31128(18) 0.0123(5) Uani 1 1 d . . . C101 C 0.6855(4) 0.5364(2) 1.11825(18) 0.0124(5) Uani 1 1 d . . . C102 C 0.7097(4) 0.6420(2) 1.06637(18) 0.0127(5) Uani 1 1 d . . . H6 H 0.6929 0.7065 1.0974 0.015 Uiso 1 1 calc R . . C103 C 0.7592(4) 0.6520(2) 0.96729(18) 0.0120(5) Uani 1 1 d . . . C104 C 0.7848(4) 0.5559(2) 0.92304(18) 0.0123(5) Uani 1 1 d . . . H7 H 0.8198 0.5629 0.8555 0.015 Uiso 1 1 calc R . . C105 C 0.7594(4) 0.4498(2) 0.97720(18) 0.0124(5) Uani 1 1 d . . . C106 C 0.7097(4) 0.4401(2) 1.07631(19) 0.0134(5) Uani 1 1 d . . . H8 H 0.6928 0.3685 1.1144 0.016 Uiso 1 1 calc R . . C111 C 0.4806(4) 0.4786(2) 1.2814(2) 0.0181(5) Uani 1 1 d . . . H9 H 0.3829 0.4430 1.2631 0.022 Uiso 1 1 calc R . . C112 C 0.7369(4) 0.5673(2) 1.27550(19) 0.0148(5) Uani 1 1 d . . . H10 H 0.8533 0.6060 1.2527 0.018 Uiso 1 1 calc R . . C131 C 0.7850(4) 0.7663(2) 0.91002(18) 0.0133(5) Uani 1 1 d . . . C151 C 0.7847(4) 0.3445(2) 0.93109(19) 0.0140(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01491(7) 0.01021(7) 0.00707(7) -0.00135(4) -0.00038(4) -0.00415(4) Ag1 0.02124(10) 0.02619(12) 0.01214(10) -0.00480(8) -0.00241(8) -0.01023(8) O1 0.0199(9) 0.0260(11) 0.0102(9) -0.0046(8) -0.0010(7) -0.0114(8) O2 0.0168(9) 0.0235(10) 0.0142(9) -0.0091(8) -0.0036(7) -0.0011(7) O3 0.0194(9) 0.0300(11) 0.0136(9) -0.0012(8) 0.0013(8) -0.0114(8) O4 0.0211(9) 0.0191(10) 0.0123(9) -0.0049(8) -0.0034(7) -0.0007(7) O5 0.0370(11) 0.0142(9) 0.0085(9) -0.0007(7) 0.0004(8) -0.0080(8) O6 0.0297(10) 0.0130(9) 0.0126(9) -0.0022(7) 0.0016(8) -0.0045(8) O7 0.0286(10) 0.0185(10) 0.0130(9) -0.0048(8) -0.0033(8) -0.0030(8) O8 0.0399(12) 0.0112(9) 0.0161(10) -0.0032(8) -0.0041(9) 0.0011(8) O9 0.0192(9) 0.0231(11) 0.0175(10) 0.0024(8) -0.0041(8) -0.0010(8) O10 0.0459(14) 0.0361(14) 0.0483(16) -0.0334(13) -0.0328(13) 0.0203(11) O11 0.0230(10) 0.0223(11) 0.0306(12) -0.0084(9) -0.0074(9) -0.0009(9) O12 0.0257(11) 0.0365(13) 0.0160(11) -0.0080(10) -0.0001(9) 0.0037(9) N11 0.0121(9) 0.0142(10) 0.0106(10) -0.0034(8) 0.0008(8) -0.0040(8) N12 0.0166(10) 0.0203(12) 0.0143(11) -0.0036(9) -0.0026(9) -0.0056(9) N13 0.0178(10) 0.0188(12) 0.0142(11) -0.0036(9) -0.0017(9) -0.0058(9) N111 0.0156(10) 0.0136(10) 0.0074(10) 0.0000(8) -0.0005(8) -0.0021(8) N112 0.0179(10) 0.0227(12) 0.0113(11) -0.0006(9) -0.0006(9) -0.0083(9) N113 0.0185(10) 0.0164(11) 0.0117(11) -0.0021(9) -0.0007(8) -0.0068(8) C1 0.0122(10) 0.0103(11) 0.0138(12) -0.0012(9) -0.0019(9) -0.0028(9) C2 0.0152(11) 0.0130(12) 0.0109(12) -0.0017(10) -0.0005(9) -0.0004(9) C3 0.0146(11) 0.0096(11) 0.0117(12) -0.0009(9) -0.0040(9) -0.0004(9) C4 0.0132(11) 0.0120(12) 0.0118(12) -0.0004(9) -0.0029(9) -0.0020(9) C5 0.0137(11) 0.0117(12) 0.0109(12) -0.0012(9) -0.0017(9) -0.0011(9) C6 0.0139(11) 0.0137(12) 0.0113(12) -0.0031(10) -0.0014(9) -0.0026(9) C11 0.0156(11) 0.0217(14) 0.0132(12) -0.0039(11) -0.0019(10) -0.0059(10) C12 0.0155(11) 0.0171(13) 0.0128(12) -0.0050(10) -0.0002(10) -0.0036(10) C31 0.0170(11) 0.0087(11) 0.0097(11) -0.0007(9) -0.0033(9) -0.0006(9) C51 0.0118(11) 0.0136(12) 0.0098(11) 0.0000(9) -0.0013(9) -0.0002(9) C101 0.0131(11) 0.0163(12) 0.0067(11) 0.0001(9) -0.0010(9) -0.0020(9) C102 0.0130(11) 0.0119(12) 0.0133(12) -0.0052(10) -0.0010(9) -0.0002(9) C103 0.0124(11) 0.0124(12) 0.0103(11) 0.0005(9) -0.0017(9) -0.0017(9) C104 0.0125(11) 0.0149(12) 0.0090(11) -0.0019(10) -0.0008(9) -0.0019(9) C105 0.0120(10) 0.0128(12) 0.0131(12) -0.0039(10) -0.0031(9) -0.0007(9) C106 0.0155(11) 0.0103(12) 0.0140(12) -0.0005(10) -0.0024(10) -0.0024(9) C111 0.0183(12) 0.0230(14) 0.0140(13) -0.0002(11) -0.0029(10) -0.0088(10) C112 0.0195(12) 0.0139(12) 0.0111(12) -0.0013(10) -0.0009(10) -0.0055(9) C131 0.0149(11) 0.0130(12) 0.0111(12) -0.0005(10) -0.0014(9) -0.0026(9) C151 0.0135(11) 0.0132(12) 0.0158(13) -0.0037(10) -0.0037(10) -0.0004(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 Tb1 O3 2.284(2) 2_776 ? Tb1 O10 2.350(2) . ? Tb1 O6 2.445(2) . ? Tb1 O1 2.457(2) . ? Tb1 O2 2.465(2) . ? Tb1 O5 2.477(2) . ? Tb1 O12 2.506(2) . ? Tb1 O9 2.524(2) . ? Tb1 O11 2.545(2) . ? Tb1 C31 2.819(3) . ? Tb1 C131 2.822(3) . ? Ag1 N113 2.153(2) 1_454 ? Ag1 N12 2.161(2) . ? Ag1 N112 2.319(2) 2_567 ? O1 C31 1.249(3) . ? O2 C31 1.275(3) . ? O3 C51 1.247(3) . ? O3 Tb1 2.2845(19) 2_776 ? O4 C51 1.247(3) . ? O5 C131 1.249(3) . ? O6 C131 1.271(3) . ? O7 C151 1.254(3) . ? O8 C151 1.262(3) . ? O9 H11 0.827(18) . ? O9 H12 0.820(10) . ? O10 H13 0.833(18) . ? O10 H14 0.828(10) . ? O10 H14B 0.834(19) . ? O11 H15 0.803(19) . ? O11 H16 0.832(19) . ? O12 H17 0.821(19) . ? O12 H18 0.839(19) . ? N11 C11 1.347(4) . ? N11 C12 1.368(3) . ? N11 C1 1.431(3) . ? N12 C11 1.308(3) . ? N12 N13 1.384(3) . ? N13 C12 1.300(3) . ? N111 C112 1.352(4) . ? N111 C111 1.360(3) . ? N111 C101 1.437(3) . ? N112 C111 1.299(4) . ? N112 N113 1.382(3) . ? N112 Ag1 2.319(2) 2_567 ? N113 C112 1.311(3) . ? N113 Ag1 2.153(2) 1_656 ? C1 C2 1.376(4) . ? C1 C6 1.386(4) . ? C2 C3 1.393(4) . ? C2 H1 0.9500 . ? C3 C4 1.402(3) . ? C3 C31 1.502(4) . ? C4 C5 1.394(4) . ? C4 H2 0.9500 . ? C5 C6 1.388(4) . ? C5 C51 1.522(3) . ? C6 H3 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? C101 C102 1.376(4) . ? C101 C106 1.381(4) . ? C102 C103 1.393(3) . ? C102 H6 0.9500 . ? C103 C104 1.398(4) . ? C103 C131 1.496(3) . ? C104 C105 1.396(4) . ? C104 H7 0.9500 . ? C105 C106 1.394(4) . ? C105 C151 1.514(4) . ? C106 H8 0.9500 . ? C111 H9 0.9500 . ? C112 H10 0.9500 . ? 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 Tb1 O10 80.36(10) 2_776 . ? O3 Tb1 O6 140.52(7) 2_776 . ? O10 Tb1 O6 77.45(10) . . ? O3 Tb1 O1 71.05(7) 2_776 . ? O10 Tb1 O1 151.30(9) . . ? O6 Tb1 O1 127.23(7) . . ? O3 Tb1 O2 118.12(7) 2_776 . ? O10 Tb1 O2 148.02(8) . . ? O6 Tb1 O2 97.36(7) . . ? O1 Tb1 O2 53.03(6) . . ? O3 Tb1 O5 121.56(7) 2_776 . ? O10 Tb1 O5 124.67(9) . . ? O6 Tb1 O5 52.96(7) . . ? O1 Tb1 O5 74.81(7) . . ? O2 Tb1 O5 70.09(7) . . ? O3 Tb1 O12 137.34(8) 2_776 . ? O10 Tb1 O12 81.51(9) . . ? O6 Tb1 O12 70.37(7) . . ? O1 Tb1 O12 118.18(7) . . ? O2 Tb1 O12 67.23(8) . . ? O5 Tb1 O12 100.48(8) . . ? O3 Tb1 O9 69.22(8) 2_776 . ? O10 Tb1 O9 75.59(8) . . ? O6 Tb1 O9 73.83(7) . . ? O1 Tb1 O9 96.01(7) . . ? O2 Tb1 O9 133.88(7) . . ? O5 Tb1 O9 68.92(8) . . ? O12 Tb1 O9 140.80(7) . . ? O3 Tb1 O11 69.95(8) 2_776 . ? O10 Tb1 O11 78.02(9) . . ? O6 Tb1 O11 134.59(7) . . ? O1 Tb1 O11 89.64(7) . . ? O2 Tb1 O11 84.23(7) . . ? O5 Tb1 O11 154.32(8) . . ? O12 Tb1 O11 68.65(8) . . ? O9 Tb1 O11 134.21(7) . . ? O3 Tb1 C31 95.21(8) 2_776 . ? O10 Tb1 C31 166.39(8) . . ? O6 Tb1 C31 112.93(8) . . ? O1 Tb1 C31 26.25(7) . . ? O2 Tb1 C31 26.88(7) . . ? O5 Tb1 C31 68.60(7) . . ? O12 Tb1 C31 93.51(8) . . ? O9 Tb1 C31 115.05(7) . . ? O11 Tb1 C31 88.37(8) . . ? O3 Tb1 C131 136.22(8) 2_776 . ? O10 Tb1 C131 101.53(10) . . ? O6 Tb1 C131 26.73(7) . . ? O1 Tb1 C131 100.81(8) . . ? O2 Tb1 C131 83.08(8) . . ? O5 Tb1 C131 26.24(7) . . ? O12 Tb1 C131 85.23(8) . . ? O9 Tb1 C131 69.07(7) . . ? O11 Tb1 C131 153.73(7) . . ? C31 Tb1 C131 90.60(8) . . ? N113 Ag1 N12 144.26(8) 1_454 . ? N113 Ag1 N112 113.60(9) 1_454 2_567 ? N12 Ag1 N112 102.07(9) . 2_567 ? C31 O1 Tb1 93.26(15) . . ? C31 O2 Tb1 92.20(16) . . ? C51 O3 Tb1 155.95(19) . 2_776 ? C131 O5 Tb1 92.50(16) . . ? C131 O6 Tb1 93.37(15) . . ? Tb1 O9 H11 118(3) . . ? Tb1 O9 H12 120(2) . . ? H11 O9 H12 114(4) . . ? Tb1 O10 H13 134(3) . . ? Tb1 O10 H14 112(5) . . ? H13 O10 H14 104(3) . . ? Tb1 O10 H14B 97.7(10) . . ? H13 O10 H14B 102(3) . . ? H14 O10 H14B 101(8) . . ? Tb1 O11 H15 102(3) . . ? Tb1 O11 H16 115(3) . . ? H15 O11 H16 104(4) . . ? Tb1 O12 H17 111(3) . . ? Tb1 O12 H18 133(3) . . ? H17 O12 H18 112(4) . . ? C11 N11 C12 104.7(2) . . ? C11 N11 C1 126.9(2) . . ? C12 N11 C1 128.3(2) . . ? C11 N12 N13 108.3(2) . . ? C11 N12 Ag1 128.6(2) . . ? N13 N12 Ag1 122.43(16) . . ? C12 N13 N12 105.8(2) . . ? C112 N111 C111 105.8(2) . . ? C112 N111 C101 125.9(2) . . ? C111 N111 C101 128.3(2) . . ? C111 N112 N113 107.4(2) . . ? C111 N112 Ag1 128.22(19) . 2_567 ? N113 N112 Ag1 124.39(17) . 2_567 ? C112 N113 N112 107.4(2) . . ? C112 N113 Ag1 130.47(19) . 1_656 ? N112 N113 Ag1 121.99(16) . 1_656 ? C2 C1 C6 121.2(2) . . ? C2 C1 N11 120.9(2) . . ? C6 C1 N11 118.0(2) . . ? C1 C2 C3 118.9(2) . . ? C1 C2 H1 120.5 . . ? C3 C2 H1 120.5 . . ? C2 C3 C4 120.7(2) . . ? C2 C3 C31 118.8(2) . . ? C4 C3 C31 120.5(2) . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H2 120.3 . . ? C3 C4 H2 120.3 . . ? C6 C5 C4 119.6(2) . . ? C6 C5 C51 119.0(2) . . ? C4 C5 C51 121.4(2) . . ? C1 C6 C5 120.2(3) . . ? C1 C6 H3 119.9 . . ? C5 C6 H3 119.9 . . ? N12 C11 N11 109.9(2) . . ? N12 C11 H4 125.1 . . ? N11 C11 H4 125.1 . . ? N13 C12 N11 111.2(2) . . ? N13 C12 H5 124.4 . . ? N11 C12 H5 124.4 . . ? O1 C31 O2 121.0(2) . . ? O1 C31 C3 119.8(2) . . ? O2 C31 C3 119.2(2) . . ? O1 C31 Tb1 60.49(14) . . ? O2 C31 Tb1 60.92(14) . . ? C3 C31 Tb1 173.01(17) . . ? O3 C51 O4 125.6(2) . . ? O3 C51 C5 115.3(2) . . ? O4 C51 C5 119.1(2) . . ? C102 C101 C106 122.8(2) . . ? C102 C101 N111 118.3(2) . . ? C106 C101 N111 118.9(2) . . ? C101 C102 C103 118.5(2) . . ? C101 C102 H6 120.8 . . ? C103 C102 H6 120.8 . . ? C102 C103 C104 119.9(2) . . ? C102 C103 C131 119.0(2) . . ? C104 C103 C131 121.1(2) . . ? C105 C104 C103 120.6(2) . . ? C105 C104 H7 119.7 . . ? C103 C104 H7 119.7 . . ? C106 C105 C104 119.3(2) . . ? C106 C105 C151 119.0(2) . . ? C104 C105 C151 121.7(2) . . ? C101 C106 C105 118.9(2) . . ? C101 C106 H8 120.5 . . ? C105 C106 H8 120.5 . . ? N112 C111 N111 109.9(2) . . ? N112 C111 H9 125.1 . . ? N111 C111 H9 125.1 . . ? N113 C112 N111 109.5(2) . . ? N113 C112 H10 125.2 . . ? N111 C112 H10 125.2 . . ? O5 C131 O6 121.2(2) . . ? O5 C131 C103 119.7(2) . . ? O6 C131 C103 119.2(2) . . ? O5 C131 Tb1 61.27(14) . . ? O6 C131 Tb1 59.90(13) . . ? C103 C131 Tb1 178.64(19) . . ? O7 C151 O8 125.7(3) . . ? O7 C151 C105 118.3(2) . . ? O8 C151 C105 116.0(2) . . ? 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 Tb1 O1 C31 -155.93(17) 2_776 . . . ? O10 Tb1 O1 C31 -150.71(17) . . . . ? O6 Tb1 O1 C31 64.24(18) . . . . ? O2 Tb1 O1 C31 -4.00(14) . . . . ? O5 Tb1 O1 C31 72.27(16) . . . . ? O12 Tb1 O1 C31 -21.65(18) . . . . ? O9 Tb1 O1 C31 138.49(16) . . . . ? O11 Tb1 O1 C31 -87.05(16) . . . . ? C131 Tb1 O1 C31 68.71(16) . . . . ? O3 Tb1 O2 C31 34.23(17) 2_776 . . . ? O10 Tb1 O2 C31 154.06(19) . . . . ? O6 Tb1 O2 C31 -127.87(15) . . . . ? O1 Tb1 O2 C31 3.91(14) . . . . ? O5 Tb1 O2 C31 -81.72(15) . . . . ? O12 Tb1 O2 C31 167.06(17) . . . . ? O9 Tb1 O2 C31 -53.25(18) . . . . ? O11 Tb1 O2 C31 97.82(15) . . . . ? C131 Tb1 O2 C31 -105.23(16) . . . . ? O3 Tb1 O5 C131 132.11(15) 2_776 . . . ? O10 Tb1 O5 C131 31.40(19) . . . . ? O6 Tb1 O5 C131 -0.06(15) . . . . ? O1 Tb1 O5 C131 -172.06(17) . . . . ? O2 Tb1 O5 C131 -116.43(17) . . . . ? O12 Tb1 O5 C131 -55.48(17) . . . . ? O9 Tb1 O5 C131 85.18(16) . . . . ? O11 Tb1 O5 C131 -117.47(19) . . . . ? C31 Tb1 O5 C131 -145.15(17) . . . . ? O3 Tb1 O6 C131 -96.55(18) 2_776 . . . ? O10 Tb1 O6 C131 -153.85(17) . . . . ? O1 Tb1 O6 C131 9.78(19) . . . . ? O2 Tb1 O6 C131 58.21(16) . . . . ? O5 Tb1 O6 C131 0.06(14) . . . . ? O12 Tb1 O6 C131 120.80(17) . . . . ? O9 Tb1 O6 C131 -75.44(16) . . . . ? O11 Tb1 O6 C131 147.36(15) . . . . ? C31 Tb1 O6 C131 35.41(17) . . . . ? N113 Ag1 N12 C11 8.7(3) 1_454 . . . ? N112 Ag1 N12 C11 -174.9(2) 2_567 . . . ? N113 Ag1 N12 N13 178.51(17) 1_454 . . . ? N112 Ag1 N12 N13 -5.1(2) 2_567 . . . ? C11 N12 N13 C12 -0.2(3) . . . . ? Ag1 N12 N13 C12 -171.77(17) . . . . ? C111 N112 N113 C112 0.1(3) . . . . ? Ag1 N112 N113 C112 178.79(18) 2_567 . . . ? C111 N112 N113 Ag1 -176.62(19) . . . 1_656 ? Ag1 N112 N113 Ag1 2.1(3) 2_567 . . 1_656 ? C11 N11 C1 C2 175.7(3) . . . . ? C12 N11 C1 C2 -8.3(4) . . . . ? C11 N11 C1 C6 -4.9(4) . . . . ? C12 N11 C1 C6 171.1(2) . . . . ? C6 C1 C2 C3 -1.6(4) . . . . ? N11 C1 C2 C3 177.7(2) . . . . ? C1 C2 C3 C4 2.0(4) . . . . ? C1 C2 C3 C31 -178.5(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C31 C3 C4 C5 179.9(2) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C3 C4 C5 C51 177.0(2) . . . . ? C2 C1 C6 C5 -0.2(4) . . . . ? N11 C1 C6 C5 -179.6(2) . . . . ? C4 C5 C6 C1 1.7(4) . . . . ? C51 C5 C6 C1 -176.6(2) . . . . ? N13 N12 C11 N11 0.8(3) . . . . ? Ag1 N12 C11 N11 171.75(17) . . . . ? C12 N11 C11 N12 -1.1(3) . . . . ? C1 N11 C11 N12 175.7(2) . . . . ? N12 N13 C12 N11 -0.5(3) . . . . ? C11 N11 C12 N13 1.0(3) . . . . ? C1 N11 C12 N13 -175.7(2) . . . . ? Tb1 O1 C31 O2 7.2(3) . . . . ? Tb1 O1 C31 C3 -172.0(2) . . . . ? Tb1 O2 C31 O1 -7.2(3) . . . . ? Tb1 O2 C31 C3 172.0(2) . . . . ? C2 C3 C31 O1 159.3(2) . . . . ? C4 C3 C31 O1 -21.2(4) . . . . ? C2 C3 C31 O2 -19.9(3) . . . . ? C4 C3 C31 O2 159.6(2) . . . . ? O3 Tb1 C31 O1 22.79(16) 2_776 . . . ? O10 Tb1 C31 O1 93.0(4) . . . . ? O6 Tb1 C31 O1 -128.87(15) . . . . ? O2 Tb1 C31 O1 172.9(3) . . . . ? O5 Tb1 C31 O1 -99.13(16) . . . . ? O12 Tb1 C31 O1 160.98(16) . . . . ? O9 Tb1 C31 O1 -46.68(17) . . . . ? O11 Tb1 C31 O1 92.49(16) . . . . ? C131 Tb1 C31 O1 -113.76(16) . . . . ? O3 Tb1 C31 O2 -150.12(15) 2_776 . . . ? O10 Tb1 C31 O2 -79.9(4) . . . . ? O6 Tb1 C31 O2 58.21(16) . . . . ? O1 Tb1 C31 O2 -172.9(3) . . . . ? O5 Tb1 C31 O2 87.95(15) . . . . ? O12 Tb1 C31 O2 -11.94(15) . . . . ? O9 Tb1 C31 O2 140.40(14) . . . . ? O11 Tb1 C31 O2 -80.43(15) . . . . ? C131 Tb1 C31 O2 73.32(15) . . . . ? Tb1 O3 C51 O4 -7.9(6) 2_776 . . . ? Tb1 O3 C51 C5 172.9(3) 2_776 . . . ? C6 C5 C51 O3 171.1(2) . . . . ? C4 C5 C51 O3 -7.1(3) . . . . ? C6 C5 C51 O4 -8.1(3) . . . . ? C4 C5 C51 O4 173.7(2) . . . . ? C112 N111 C101 C102 -50.0(3) . . . . ? C111 N111 C101 C102 127.1(3) . . . . ? C112 N111 C101 C106 128.8(3) . . . . ? C111 N111 C101 C106 -54.2(4) . . . . ? C106 C101 C102 C103 0.5(4) . . . . ? N111 C101 C102 C103 179.2(2) . . . . ? C101 C102 C103 C104 -0.5(4) . . . . ? C101 C102 C103 C131 179.7(2) . . . . ? C102 C103 C104 C105 0.6(4) . . . . ? C131 C103 C104 C105 -179.7(2) . . . . ? C103 C104 C105 C106 -0.5(4) . . . . ? C103 C104 C105 C151 179.6(2) . . . . ? C102 C101 C106 C105 -0.4(4) . . . . ? N111 C101 C106 C105 -179.1(2) . . . . ? C104 C105 C106 C101 0.5(4) . . . . ? C151 C105 C106 C101 -179.6(2) . . . . ? N113 N112 C111 N111 0.3(3) . . . . ? Ag1 N112 C111 N111 -178.42(17) 2_567 . . . ? C112 N111 C111 N112 -0.5(3) . . . . ? C101 N111 C111 N112 -178.0(2) . . . . ? N112 N113 C112 N111 -0.3(3) . . . . ? Ag1 N113 C112 N111 175.94(17) 1_656 . . . ? C111 N111 C112 N113 0.5(3) . . . . ? C101 N111 C112 N113 178.1(2) . . . . ? Tb1 O5 C131 O6 0.1(3) . . . . ? Tb1 O5 C131 C103 -178.9(2) . . . . ? Tb1 O6 C131 O5 -0.1(3) . . . . ? Tb1 O6 C131 C103 178.9(2) . . . . ? C102 C103 C131 O5 179.9(2) . . . . ? C104 C103 C131 O5 0.1(4) . . . . ? C102 C103 C131 O6 0.9(4) . . . . ? C104 C103 C131 O6 -178.9(2) . . . . ? O3 Tb1 C131 O5 -66.0(2) 2_776 . . . ? O10 Tb1 C131 O5 -154.07(16) . . . . ? O6 Tb1 C131 O5 179.9(3) . . . . ? O1 Tb1 C131 O5 7.80(17) . . . . ? O2 Tb1 C131 O5 58.01(16) . . . . ? O12 Tb1 C131 O5 125.61(17) . . . . ? O9 Tb1 C131 O5 -84.56(16) . . . . ? O11 Tb1 C131 O5 119.7(2) . . . . ? C31 Tb1 C131 O5 32.14(16) . . . . ? O3 Tb1 C131 O6 114.09(16) 2_776 . . . ? O10 Tb1 C131 O6 26.05(17) . . . . ? O1 Tb1 C131 O6 -172.09(15) . . . . ? O2 Tb1 C131 O6 -121.88(16) . . . . ? O5 Tb1 C131 O6 -179.9(3) . . . . ? O12 Tb1 C131 O6 -54.27(16) . . . . ? O9 Tb1 C131 O6 95.56(16) . . . . ? O11 Tb1 C131 O6 -60.2(3) . . . . ? C31 Tb1 C131 O6 -147.74(16) . . . . ? C106 C105 C151 O7 174.2(2) . . . . ? C104 C105 C151 O7 -5.9(4) . . . . ? C106 C105 C151 O8 -4.9(3) . . . . ? C104 C105 C151 O8 175.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.038 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.188 data_4 _database_code_depnum_ccdc_archive 'CCDC 803745' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H10 Ag N6 Nd O8' _chemical_formula_sum 'C20 H10 Ag N6 Nd O8' _chemical_formula_weight 714.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4621(10) _cell_length_b 17.0741(11) _cell_length_c 9.1373(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.4250(10) _cell_angle_gamma 90.00 _cell_volume 2037.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4651 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour pale-purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4590 _exptl_absorpt_correction_T_max 0.5372 _exptl_absorpt_process_details 'SADBAS (Bruker,2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 5094 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1801 _reflns_number_gt 1725 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^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 1801 _refine_ls_number_parameters 164 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.065 _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 0.0000 0.406904(13) -0.2500 0.01354(14) Uani 1 2 d S . . Ag1 Ag 0.5000 0.35867(3) 1.2500 0.03985(18) Uani 1 2 d S . . C1 C 0.2644(3) 0.3277(2) 0.2491(5) 0.0203(8) Uani 1 1 d . . . H1 H 0.2496 0.3188 0.1409 0.024 Uiso 1 1 calc R . . C2 C 0.3354(3) 0.2812(2) 0.3688(5) 0.0202(8) Uani 1 1 d . . . C3 C 0.3624(3) 0.2971(2) 0.5322(4) 0.0210(8) Uani 1 1 d . . . H3 H 0.4110 0.2666 0.6128 0.025 Uiso 1 1 calc R . . C4 C 0.3162(3) 0.3583(2) 0.5719(4) 0.0196(8) Uani 1 1 d . . . C5 C 0.2411(3) 0.4030(2) 0.4535(5) 0.0225(9) Uani 1 1 d . . . H5 H 0.2083 0.4429 0.4823 0.027 Uiso 1 1 calc R . . C6 C 0.2155(3) 0.3875(2) 0.2909(4) 0.0183(7) Uani 1 1 d . . . C7 C 0.3857(3) 0.3360(3) 0.8727(5) 0.0293(9) Uani 1 1 d . . . H7 H 0.3919 0.2817 0.8744 0.035 Uiso 1 1 calc R . . C8 C 0.3538(4) 0.4547(3) 0.7937(5) 0.0403(11) Uani 1 1 d . . . H8 H 0.3332 0.4988 0.7277 0.048 Uiso 1 1 calc R . . C9 C 0.3893(4) 0.2150(2) 0.3270(6) 0.0278(9) Uani 1 1 d U . . C10 C 0.1396(3) 0.4404(2) 0.1628(4) 0.0177(8) Uani 1 1 d . . . N1 N 0.3493(3) 0.38049(19) 0.7380(4) 0.0228(7) Uani 1 1 d . . . N2 N 0.4109(3) 0.3799(2) 0.9996(4) 0.0335(8) Uani 1 1 d . . . N3 N 0.3904(3) 0.4565(3) 0.9509(4) 0.0453(11) Uani 1 1 d . . . O1 O 0.3776(3) 0.2081(2) 0.1841(4) 0.0490(9) Uani 1 1 d U . . O2 O 0.4488(3) 0.17140(19) 0.4382(4) 0.0498(9) Uani 1 1 d U . . O3 O 0.1270(2) 0.43114(17) 0.0198(3) 0.0243(6) Uani 1 1 d . . . O4 O 0.0966(2) 0.49227(18) 0.2078(3) 0.0380(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0152(2) 0.0148(2) 0.0099(2) 0.000 0.00477(14) 0.000 Ag1 0.0442(3) 0.0527(3) 0.0122(3) 0.000 0.0021(2) 0.000 C1 0.0230(19) 0.0224(18) 0.0156(17) -0.0023(13) 0.0085(15) 0.0003(14) C2 0.019(2) 0.0225(19) 0.020(2) -0.0019(14) 0.0093(18) 0.0049(14) C3 0.0186(19) 0.0238(18) 0.0177(19) 0.0027(15) 0.0051(15) 0.0046(15) C4 0.0226(19) 0.0232(18) 0.0110(17) -0.0004(14) 0.0054(16) 0.0000(14) C5 0.021(2) 0.025(2) 0.019(2) -0.0027(13) 0.0072(18) 0.0055(14) C6 0.0170(18) 0.0216(17) 0.0131(17) -0.0008(14) 0.0033(15) 0.0028(15) C7 0.033(2) 0.034(2) 0.0123(19) 0.0033(16) 0.0021(17) 0.0043(18) C8 0.061(3) 0.032(2) 0.018(2) -0.0052(18) 0.008(2) 0.011(2) C9 0.034(2) 0.029(2) 0.027(2) 0.0029(15) 0.0191(17) 0.0093(16) C10 0.0184(18) 0.018(2) 0.0134(18) -0.0013(14) 0.0037(15) 0.0016(14) N1 0.0254(17) 0.0242(17) 0.0161(16) 0.0001(13) 0.0065(14) 0.0070(14) N2 0.037(2) 0.039(2) 0.0164(17) 0.0009(16) 0.0038(16) 0.0077(18) N3 0.060(3) 0.043(2) 0.0179(18) -0.0024(17) 0.0025(18) 0.017(2) O1 0.060(2) 0.0560(19) 0.0218(16) -0.0046(14) 0.0084(15) 0.0329(17) O2 0.072(2) 0.052(2) 0.0334(17) 0.0143(14) 0.0301(16) 0.0387(17) O3 0.0251(14) 0.0304(15) 0.0121(13) -0.0008(11) 0.0029(11) 0.0039(12) O4 0.0475(18) 0.0408(18) 0.0195(14) 0.0015(12) 0.0086(13) 0.0279(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 Nd1 O4 2.351(3) 6_565 ? Nd1 O4 2.351(3) 5_565 ? Nd1 O3 2.394(3) . ? Nd1 O3 2.394(3) 2_554 ? Nd1 O2 2.527(3) 7 ? Nd1 O2 2.527(3) 8_455 ? Nd1 O1 2.537(3) 8_455 ? Nd1 O1 2.537(3) 7 ? Nd1 C9 2.891(4) 8_455 ? Nd1 C9 2.891(4) 7 ? Ag1 N2 2.120(3) 2_657 ? Ag1 N2 2.120(3) . ? C1 C6 1.386(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.398(6) . ? C2 C9 1.512(6) . ? C3 C4 1.370(5) . ? C3 H3 0.9300 . ? C4 C5 1.387(5) . ? C4 N1 1.432(5) . ? C5 C6 1.394(6) . ? C5 H5 0.9300 . ? C6 C10 1.512(5) . ? C7 N2 1.295(6) . ? C7 N1 1.347(5) . ? C7 H7 0.9300 . ? C8 N3 1.301(5) . ? C8 N1 1.356(6) . ? C8 H8 0.9300 . ? C9 O1 1.248(6) . ? C9 O2 1.255(5) . ? C9 Nd1 2.891(4) 7 ? C10 O3 1.249(5) . ? C10 O4 1.249(5) . ? N2 N3 1.372(6) . ? O1 Nd1 2.537(3) 7 ? O2 Nd1 2.527(3) 7 ? O4 Nd1 2.351(3) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Nd1 O4 85.85(17) 6_565 5_565 ? O4 Nd1 O3 78.18(10) 6_565 . ? O4 Nd1 O3 87.23(10) 5_565 . ? O4 Nd1 O3 87.23(10) 6_565 2_554 ? O4 Nd1 O3 78.18(10) 5_565 2_554 ? O3 Nd1 O3 160.09(14) . 2_554 ? O4 Nd1 O2 84.69(11) 6_565 7 ? O4 Nd1 O2 150.16(10) 5_565 7 ? O3 Nd1 O2 118.22(11) . 7 ? O3 Nd1 O2 73.15(11) 2_554 7 ? O4 Nd1 O2 150.16(10) 6_565 8_455 ? O4 Nd1 O2 84.69(11) 5_565 8_455 ? O3 Nd1 O2 73.15(11) . 8_455 ? O3 Nd1 O2 118.22(11) 2_554 8_455 ? O2 Nd1 O2 116.11(15) 7 8_455 ? O4 Nd1 O1 158.60(11) 6_565 8_455 ? O4 Nd1 O1 101.67(13) 5_565 8_455 ? O3 Nd1 O1 121.78(10) . 8_455 ? O3 Nd1 O1 74.98(10) 2_554 8_455 ? O2 Nd1 O1 78.90(13) 7 8_455 ? O2 Nd1 O1 51.21(10) 8_455 8_455 ? O4 Nd1 O1 101.67(13) 6_565 7 ? O4 Nd1 O1 158.60(11) 5_565 7 ? O3 Nd1 O1 74.98(10) . 7 ? O3 Nd1 O1 121.78(10) 2_554 7 ? O2 Nd1 O1 51.21(10) 7 7 ? O2 Nd1 O1 78.90(13) 8_455 7 ? O1 Nd1 O1 78.60(19) 8_455 7 ? O4 Nd1 C9 175.81(11) 6_565 8_455 ? O4 Nd1 C9 93.26(13) 5_565 8_455 ? O3 Nd1 C9 97.69(12) . 8_455 ? O3 Nd1 C9 96.60(12) 2_554 8_455 ? O2 Nd1 C9 98.02(12) 7 8_455 ? O2 Nd1 C9 25.68(12) 8_455 8_455 ? O1 Nd1 C9 25.54(12) 8_455 8_455 ? O1 Nd1 C9 77.78(13) 7 8_455 ? O4 Nd1 C9 93.26(13) 6_565 7 ? O4 Nd1 C9 175.81(11) 5_565 7 ? O3 Nd1 C9 96.60(12) . 7 ? O3 Nd1 C9 97.69(12) 2_554 7 ? O2 Nd1 C9 25.68(12) 7 7 ? O2 Nd1 C9 98.02(12) 8_455 7 ? O1 Nd1 C9 77.78(13) 8_455 7 ? O1 Nd1 C9 25.54(12) 7 7 ? C9 Nd1 C9 87.92(18) 8_455 7 ? N2 Ag1 N2 160.3(2) 2_657 . ? C6 C1 C2 119.8(3) . . ? C6 C1 H1 120.1 . . ? C2 C1 H1 120.1 . . ? C1 C2 C3 120.3(3) . . ? C1 C2 C9 121.1(4) . . ? C3 C2 C9 118.5(4) . . ? C4 C3 C2 119.1(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 N1 120.2(3) . . ? C5 C4 N1 118.3(3) . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.0(3) . . ? C1 C6 C10 120.9(3) . . ? C5 C6 C10 118.9(3) . . ? N2 C7 N1 109.9(4) . . ? N2 C7 H7 125.0 . . ? N1 C7 H7 125.0 . . ? N3 C8 N1 111.6(4) . . ? N3 C8 H8 124.2 . . ? N1 C8 H8 124.2 . . ? O1 C9 O2 121.9(4) . . ? O1 C9 C2 118.8(4) . . ? O2 C9 C2 119.2(4) . . ? O1 C9 Nd1 61.2(2) . 7 ? O2 C9 Nd1 60.7(2) . 7 ? C2 C9 Nd1 177.4(3) . 7 ? O3 C10 O4 124.3(3) . . ? O3 C10 C6 117.7(3) . . ? O4 C10 C6 117.9(3) . . ? C7 N1 C8 104.3(3) . . ? C7 N1 C4 129.9(3) . . ? C8 N1 C4 125.8(3) . . ? C7 N2 N3 108.8(3) . . ? C7 N2 Ag1 132.4(3) . . ? N3 N2 Ag1 117.3(3) . . ? C8 N3 N2 105.3(4) . . ? C9 O1 Nd1 93.3(3) . 7 ? C9 O2 Nd1 93.6(3) . 7 ? C10 O3 Nd1 143.3(3) . . ? C10 O4 Nd1 171.2(3) . 5_565 ? 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 C6 C1 C2 C3 -3.8(6) . . . . ? C6 C1 C2 C9 179.3(4) . . . . ? C1 C2 C3 C4 1.3(6) . . . . ? C9 C2 C3 C4 178.2(4) . . . . ? C2 C3 C4 C5 2.1(6) . . . . ? C2 C3 C4 N1 -174.1(4) . . . . ? C3 C4 C5 C6 -2.9(6) . . . . ? N1 C4 C5 C6 173.4(4) . . . . ? C2 C1 C6 C5 3.0(6) . . . . ? C2 C1 C6 C10 178.5(3) . . . . ? C4 C5 C6 C1 0.3(6) . . . . ? C4 C5 C6 C10 -175.2(4) . . . . ? C1 C2 C9 O1 8.0(7) . . . . ? C3 C2 C9 O1 -169.0(4) . . . . ? C1 C2 C9 O2 -176.0(4) . . . . ? C3 C2 C9 O2 7.0(7) . . . . ? C1 C6 C10 O3 -3.9(6) . . . . ? C5 C6 C10 O3 171.6(4) . . . . ? C1 C6 C10 O4 178.7(4) . . . . ? C5 C6 C10 O4 -5.7(6) . . . . ? N2 C7 N1 C8 -0.4(5) . . . . ? N2 C7 N1 C4 177.3(4) . . . . ? N3 C8 N1 C7 0.2(6) . . . . ? N3 C8 N1 C4 -177.7(4) . . . . ? C3 C4 N1 C7 -33.3(6) . . . . ? C5 C4 N1 C7 150.4(4) . . . . ? C3 C4 N1 C8 144.0(4) . . . . ? C5 C4 N1 C8 -32.3(6) . . . . ? N1 C7 N2 N3 0.5(6) . . . . ? N1 C7 N2 Ag1 -165.1(3) . . . . ? N2 Ag1 N2 C7 162.6(5) 2_657 . . . ? N2 Ag1 N2 N3 -2.1(3) 2_657 . . . ? N1 C8 N3 N2 0.1(6) . . . . ? C7 N2 N3 C8 -0.4(6) . . . . ? Ag1 N2 N3 C8 167.7(4) . . . . ? O2 C9 O1 Nd1 1.2(5) . . . 7 ? C2 C9 O1 Nd1 177.0(4) . . . 7 ? O1 C9 O2 Nd1 -1.2(5) . . . 7 ? C2 C9 O2 Nd1 -177.0(4) . . . 7 ? O4 C10 O3 Nd1 -58.1(6) . . . . ? C6 C10 O3 Nd1 124.7(4) . . . . ? O4 Nd1 O3 C10 134.9(4) 6_565 . . . ? O4 Nd1 O3 C10 48.6(4) 5_565 . . . ? O3 Nd1 O3 C10 91.2(4) 2_554 . . . ? O2 Nd1 O3 C10 -147.8(4) 7 . . . ? O2 Nd1 O3 C10 -36.7(4) 8_455 . . . ? O1 Nd1 O3 C10 -53.4(5) 8_455 . . . ? O1 Nd1 O3 C10 -119.4(4) 7 . . . ? C9 Nd1 O3 C10 -44.3(4) 8_455 . . . ? C9 Nd1 O3 C10 -133.1(4) 7 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.802 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.139 data_5 _database_code_depnum_ccdc_archive 'CCDC 803746' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2010-04-14 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H10 Ag Eu N6 O8 ' _chemical_formula_sum 'C20 H10 Ag Eu N6 O8 ' _chemical_formula_weight 722.16 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 14.358(5) _cell_length_b 16.949(6) _cell_length_c 9.127(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.676(15) _cell_angle_gamma 90.00 _cell_volume 2001.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9067 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1393 _exptl_absorpt_coefficient_mu 4.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5747 _exptl_absorpt_correction_T_max 0.8193 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 9287 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2280 _reflns_number_gt 2222 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0184P)^2^+3.3041P] 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 2280 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0406 _refine_ls_wR_factor_gt 0.0404 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.5000 0.907321(7) 0.2500 0.00889(5) Uani 1 2 d S . . Ag1 Ag 0.5000 0.640799(16) 1.2500 0.02658(7) Uani 1 2 d S . . O1 O 0.44878(16) 0.83093(11) 0.4368(2) 0.0357(4) Uani 1 1 d . . . O2 O 0.37868(14) 0.79330(11) 0.1813(2) 0.0322(4) Uani 1 1 d . . . O3 O 0.12676(11) 0.56754(8) 0.01599(17) 0.0158(3) Uani 1 1 d . . . O4 O 0.09509(13) 0.50649(10) 0.20463(18) 0.0260(4) Uani 1 1 d . . . N1 N 0.34817(13) 0.61999(10) 0.7359(2) 0.0158(3) Uani 1 1 d . . . N2 N 0.41090(15) 0.62015(12) 0.9997(2) 0.0227(4) Uani 1 1 d . . . N3 N 0.38894(17) 0.54263(12) 0.9490(2) 0.0306(5) Uani 1 1 d . . . C1 C 0.31521(15) 0.64196(11) 0.5698(2) 0.0139(4) Uani 1 1 d . . . C2 C 0.36264(15) 0.70409(12) 0.5299(3) 0.0153(4) Uani 1 1 d . . . H1 H 0.4125 0.7357 0.6128 0.018 Uiso 1 1 calc R . . C3 C 0.33636(16) 0.71967(11) 0.3669(3) 0.0145(4) Uani 1 1 d . . . C4 C 0.26386(15) 0.67280(11) 0.2450(2) 0.0142(4) Uani 1 1 d . . . H2 H 0.2484 0.6820 0.1342 0.017 Uiso 1 1 calc R . . C5 C 0.21422(15) 0.61230(11) 0.2876(2) 0.0132(4) Uani 1 1 d . . . C6 C 0.23890(16) 0.59727(11) 0.4497(3) 0.0156(4) Uani 1 1 d . . . H3 H 0.2040 0.5568 0.4784 0.019 Uiso 1 1 calc R . . C11 C 0.38618(16) 0.66509(13) 0.8718(3) 0.0198(4) Uani 1 1 d . . . H4 H 0.3937 0.7208 0.8739 0.024 Uiso 1 1 calc R . . C12 C 0.35198(19) 0.54473(13) 0.7914(3) 0.0260(5) Uani 1 1 d . . . H5 H 0.3303 0.4995 0.7233 0.031 Uiso 1 1 calc R . . C31 C 0.39055(16) 0.78611(11) 0.3256(3) 0.0163(4) Uani 1 1 d . . . C51 C 0.13764(14) 0.55857(11) 0.1585(2) 0.0128(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01102(7) 0.00816(7) 0.00688(8) 0.000 0.00331(5) 0.000 Ag1 0.02959(13) 0.03406(14) 0.00884(12) 0.000 0.00154(10) 0.000 O1 0.0570(11) 0.0331(9) 0.0276(9) -0.0145(7) 0.0284(9) -0.0308(9) O2 0.0395(10) 0.0365(9) 0.0146(8) 0.0022(7) 0.0061(7) -0.0239(8) O3 0.0172(6) 0.0188(7) 0.0085(7) 0.0005(5) 0.0030(6) -0.0012(5) O4 0.0323(8) 0.0278(8) 0.0134(7) -0.0008(6) 0.0057(6) -0.0187(7) N1 0.0173(8) 0.0177(8) 0.0103(8) -0.0002(6) 0.0039(7) -0.0044(6) N2 0.0243(9) 0.0263(9) 0.0117(9) -0.0002(7) 0.0024(7) -0.0047(8) N3 0.0397(11) 0.0255(10) 0.0170(9) 0.0025(8) 0.0032(9) -0.0110(9) C1 0.0163(9) 0.0157(8) 0.0089(9) 0.0007(7) 0.0046(7) -0.0010(7) C2 0.0147(9) 0.0149(8) 0.0141(10) -0.0019(7) 0.0043(8) -0.0036(7) C3 0.0155(9) 0.0126(8) 0.0171(11) 0.0005(7) 0.0084(8) -0.0023(7) C4 0.0165(8) 0.0150(8) 0.0115(9) 0.0011(7) 0.0064(7) -0.0007(7) C5 0.0148(8) 0.0127(8) 0.0108(9) -0.0002(7) 0.0043(7) -0.0022(7) C6 0.0184(9) 0.0147(9) 0.0133(10) 0.0006(7) 0.0064(8) -0.0041(7) C11 0.0225(10) 0.0214(10) 0.0109(9) -0.0024(8) 0.0030(8) -0.0007(8) C12 0.0363(12) 0.0198(10) 0.0143(10) 0.0021(8) 0.0039(9) -0.0089(9) C31 0.0168(9) 0.0137(8) 0.0191(11) 0.0013(7) 0.0086(8) -0.0023(7) C51 0.0137(8) 0.0124(8) 0.0102(9) 0.0005(7) 0.0031(7) -0.0007(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 Eu1 O4 2.3131(16) 4 ? Eu1 O4 2.3132(16) 3 ? Eu1 O3 2.3578(16) 7_565 ? Eu1 O3 2.3578(16) 8_566 ? Eu1 O1 2.4925(18) . ? Eu1 O1 2.4925(18) 2_655 ? Eu1 O2 2.4931(17) 2_655 ? Eu1 O2 2.4931(17) . ? Eu1 C31 2.847(2) . ? Eu1 C31 2.847(2) 2_655 ? Ag1 N2 2.108(2) 2_657 ? Ag1 N2 2.108(2) . ? O1 C31 1.253(3) . ? O2 C31 1.259(3) . ? O3 C51 1.251(3) . ? O3 Eu1 2.3578(16) 7_565 ? O4 C51 1.246(2) . ? O4 Eu1 2.3132(16) 3_445 ? N1 C11 1.354(3) . ? N1 C12 1.365(3) . ? N1 C1 1.428(3) . ? N2 C11 1.308(3) . ? N2 N3 1.383(3) . ? N3 C12 1.300(3) . ? C1 C2 1.385(3) . ? C1 C6 1.391(3) . ? C2 C3 1.393(3) . ? C2 H1 0.9500 . ? C3 C4 1.396(3) . ? C3 C31 1.506(3) . ? C4 C5 1.397(3) . ? C4 H2 0.9500 . ? C5 C6 1.387(3) . ? C5 C51 1.518(3) . ? C6 H3 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O4 86.79(10) 4 3 ? O4 Eu1 O3 78.51(6) 4 7_565 ? O4 Eu1 O3 86.36(6) 3 7_565 ? O4 Eu1 O3 86.36(6) 4 8_566 ? O4 Eu1 O3 78.51(6) 3 8_566 ? O3 Eu1 O3 159.18(7) 7_565 8_566 ? O4 Eu1 O1 83.28(7) 4 . ? O4 Eu1 O1 150.69(6) 3 . ? O3 Eu1 O1 118.26(6) 7_565 . ? O3 Eu1 O1 73.40(6) 8_566 . ? O4 Eu1 O1 150.69(6) 4 2_655 ? O4 Eu1 O1 83.28(7) 3 2_655 ? O3 Eu1 O1 73.40(6) 7_565 2_655 ? O3 Eu1 O1 118.26(6) 8_566 2_655 ? O1 Eu1 O1 117.41(9) . 2_655 ? O4 Eu1 O2 157.01(6) 4 2_655 ? O4 Eu1 O2 101.88(7) 3 2_655 ? O3 Eu1 O2 122.85(5) 7_565 2_655 ? O3 Eu1 O2 74.79(6) 8_566 2_655 ? O1 Eu1 O2 78.85(7) . 2_655 ? O1 Eu1 O2 52.28(6) 2_655 2_655 ? O4 Eu1 O2 101.88(7) 4 . ? O4 Eu1 O2 157.01(6) 3 . ? O3 Eu1 O2 74.79(6) 7_565 . ? O3 Eu1 O2 122.85(5) 8_566 . ? O1 Eu1 O2 52.28(6) . . ? O1 Eu1 O2 78.85(7) 2_655 . ? O2 Eu1 O2 78.37(10) 2_655 . ? O4 Eu1 C31 92.88(7) 4 . ? O4 Eu1 C31 176.65(6) 3 . ? O3 Eu1 C31 96.84(6) 7_565 . ? O3 Eu1 C31 98.14(6) 8_566 . ? O1 Eu1 C31 26.08(6) . . ? O1 Eu1 C31 98.55(7) 2_655 . ? O2 Eu1 C31 77.22(7) 2_655 . ? O2 Eu1 C31 26.20(6) . . ? O4 Eu1 C31 176.65(6) 4 2_655 ? O4 Eu1 C31 92.88(7) 3 2_655 ? O3 Eu1 C31 98.14(6) 7_565 2_655 ? O3 Eu1 C31 96.84(6) 8_566 2_655 ? O1 Eu1 C31 98.55(7) . 2_655 ? O1 Eu1 C31 26.08(6) 2_655 2_655 ? O2 Eu1 C31 26.20(6) 2_655 2_655 ? O2 Eu1 C31 77.22(7) . 2_655 ? C31 Eu1 C31 87.64(9) . 2_655 ? N2 Ag1 N2 160.89(11) 2_657 . ? C31 O1 Eu1 92.97(14) . . ? C31 O2 Eu1 92.80(13) . . ? C51 O3 Eu1 141.81(13) . 7_565 ? C51 O4 Eu1 171.54(14) . 3_445 ? C11 N1 C12 104.60(18) . . ? C11 N1 C1 129.94(18) . . ? C12 N1 C1 125.40(18) . . ? C11 N2 N3 108.65(18) . . ? C11 N2 Ag1 132.33(16) . . ? N3 N2 Ag1 117.63(14) . . ? C12 N3 N2 105.60(18) . . ? C2 C1 C6 121.07(19) . . ? C2 C1 N1 120.15(17) . . ? C6 C1 N1 118.69(18) . . ? C1 C2 C3 119.21(18) . . ? C1 C2 H1 120.4 . . ? C3 C2 H1 120.4 . . ? C2 C3 C4 120.47(18) . . ? C2 C3 C31 118.60(18) . . ? C4 C3 C31 120.9(2) . . ? C3 C4 C5 119.33(19) . . ? C3 C4 H2 120.3 . . ? C5 C4 H2 120.3 . . ? C6 C5 C4 120.42(18) . . ? C6 C5 C51 118.82(17) . . ? C4 C5 C51 120.64(18) . . ? C5 C6 C1 119.36(18) . . ? C5 C6 H3 120.3 . . ? C1 C6 H3 120.3 . . ? N2 C11 N1 109.57(19) . . ? N2 C11 H4 125.2 . . ? N1 C11 H4 125.2 . . ? N3 C12 N1 111.6(2) . . ? N3 C12 H5 124.2 . . ? N1 C12 H5 124.2 . . ? O1 C31 O2 121.9(2) . . ? O1 C31 C3 119.1(2) . . ? O2 C31 C3 118.92(19) . . ? O1 C31 Eu1 60.95(12) . . ? O2 C31 Eu1 61.00(11) . . ? C3 C31 Eu1 177.60(14) . . ? O4 C51 O3 125.38(18) . . ? O4 C51 C5 117.33(18) . . ? O3 C51 C5 117.16(17) . . ? 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 O4 Eu1 O1 C31 110.85(15) 4 . . . ? O4 Eu1 O1 C31 -178.12(13) 3 . . . ? O3 Eu1 O1 C31 37.77(16) 7_565 . . . ? O3 Eu1 O1 C31 -160.95(16) 8_566 . . . ? O1 Eu1 O1 C31 -47.26(13) 2_655 . . . ? O2 Eu1 O1 C31 -83.68(15) 2_655 . . . ? O2 Eu1 O1 C31 0.17(13) . . . . ? C31 Eu1 O1 C31 -66.31(17) 2_655 . . . ? O4 Eu1 O2 C31 -71.87(15) 4 . . . ? O4 Eu1 O2 C31 177.69(15) 3 . . . ? O3 Eu1 O2 C31 -146.32(15) 7_565 . . . ? O3 Eu1 O2 C31 21.49(17) 8_566 . . . ? O1 Eu1 O2 C31 -0.17(13) . . . . ? O1 Eu1 O2 C31 138.05(15) 2_655 . . . ? O2 Eu1 O2 C31 84.64(14) 2_655 . . . ? C31 Eu1 O2 C31 111.43(15) 2_655 . . . ? N2 Ag1 N2 C11 -162.2(2) 2_657 . . . ? N2 Ag1 N2 N3 2.59(16) 2_657 . . . ? C11 N2 N3 C12 0.2(3) . . . . ? Ag1 N2 N3 C12 -167.98(17) . . . . ? C11 N1 C1 C2 32.4(3) . . . . ? C12 N1 C1 C2 -144.2(2) . . . . ? C11 N1 C1 C6 -151.0(2) . . . . ? C12 N1 C1 C6 32.4(3) . . . . ? C6 C1 C2 C3 -2.8(3) . . . . ? N1 C1 C2 C3 173.80(18) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C1 C2 C3 C31 -178.46(18) . . . . ? C2 C3 C4 C5 3.0(3) . . . . ? C31 C3 C4 C5 -179.25(18) . . . . ? C3 C4 C5 C6 -2.0(3) . . . . ? C3 C4 C5 C51 -177.97(17) . . . . ? C4 C5 C6 C1 -1.3(3) . . . . ? C51 C5 C6 C1 174.72(18) . . . . ? C2 C1 C6 C5 3.8(3) . . . . ? N1 C1 C6 C5 -172.85(18) . . . . ? N3 N2 C11 N1 -0.1(3) . . . . ? Ag1 N2 C11 N1 165.72(16) . . . . ? C12 N1 C11 N2 -0.1(3) . . . . ? C1 N1 C11 N2 -177.2(2) . . . . ? N2 N3 C12 N1 -0.2(3) . . . . ? C11 N1 C12 N3 0.2(3) . . . . ? C1 N1 C12 N3 177.5(2) . . . . ? Eu1 O1 C31 O2 -0.3(2) . . . . ? Eu1 O1 C31 C3 177.26(16) . . . . ? Eu1 O2 C31 O1 0.3(2) . . . . ? Eu1 O2 C31 C3 -177.26(16) . . . . ? C2 C3 C31 O1 -8.0(3) . . . . ? C4 C3 C31 O1 174.2(2) . . . . ? C2 C3 C31 O2 169.7(2) . . . . ? C4 C3 C31 O2 -8.1(3) . . . . ? O4 Eu1 C31 O1 -68.32(15) 4 . . . ? O3 Eu1 C31 O1 -147.08(15) 7_565 . . . ? O3 Eu1 C31 O1 18.42(15) 8_566 . . . ? O1 Eu1 C31 O1 138.75(13) 2_655 . . . ? O2 Eu1 C31 O1 90.71(15) 2_655 . . . ? O2 Eu1 C31 O1 -179.7(2) . . . . ? C31 Eu1 C31 O1 114.99(16) 2_655 . . . ? O4 Eu1 C31 O2 111.38(15) 4 . . . ? O3 Eu1 C31 O2 32.62(15) 7_565 . . . ? O3 Eu1 C31 O2 -161.88(14) 8_566 . . . ? O1 Eu1 C31 O2 179.7(2) . . . . ? O1 Eu1 C31 O2 -41.54(15) 2_655 . . . ? O2 Eu1 C31 O2 -89.59(16) 2_655 . . . ? C31 Eu1 C31 O2 -65.30(14) 2_655 . . . ? Eu1 O3 C51 O4 60.0(3) 7_565 . . . ? Eu1 O3 C51 C5 -124.11(19) 7_565 . . . ? C6 C5 C51 O4 4.9(3) . . . . ? C4 C5 C51 O4 -179.05(19) . . . . ? C6 C5 C51 O3 -171.34(18) . . . . ? C4 C5 C51 O3 4.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.832 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.111 data_6 _database_code_depnum_ccdc_archive 'CCDC 803747' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2010-07-30 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H10 Ag N6 O8 Tb' _chemical_formula_sum 'C20 H10 Ag N6 O8 Tb' _chemical_formula_weight 729.12 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' Ag Ag -0.8971 1.1015 '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' 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 14.326(5) _cell_length_b 16.855(6) _cell_length_c 9.095(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.654(17) _cell_angle_gamma 90.00 _cell_volume 1979.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9018 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1402 _exptl_absorpt_coefficient_mu 4.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3924 _exptl_absorpt_correction_T_max 0.8025 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 9173 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2257 _reflns_number_gt 2207 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0294P)^2^+2.6963P] 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 2257 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.5000 0.407451(7) 0.2500 0.00903(7) Uani 1 2 d S . . Ag2 Ag 0.5000 0.139812(18) 1.2500 0.02715(8) Uani 1 2 d S . . O1 O 0.44850(17) 0.33171(12) 0.4349(3) 0.0342(5) Uani 1 1 d . . . O2 O 0.37936(16) 0.29358(12) 0.1797(2) 0.0316(5) Uani 1 1 d . . . O3 O 0.12485(12) 0.06716(10) 0.01387(19) 0.0158(3) Uani 1 1 d . . . O4 O 0.09357(14) 0.00618(10) 0.2039(2) 0.0249(4) Uani 1 1 d . . . N11 N 0.34790(15) 0.11976(11) 0.7350(2) 0.0166(4) Uani 1 1 d . . . N12 N 0.41081(17) 0.11935(13) 0.9992(3) 0.0228(4) Uani 1 1 d . . . N13 N 0.38848(19) 0.04140(14) 0.9477(3) 0.0309(5) Uani 1 1 d . . . C1 C 0.31468(17) 0.14213(13) 0.5684(3) 0.0147(4) Uani 1 1 d . . . C2 C 0.36269(17) 0.20429(13) 0.5288(3) 0.0153(4) Uani 1 1 d . . . H1 H 0.4130 0.2359 0.6119 0.018 Uiso 1 1 calc R . . C3 C 0.33602(18) 0.21976(12) 0.3650(3) 0.0149(4) Uani 1 1 d . . . C4 C 0.26306(17) 0.17294(13) 0.2430(3) 0.0149(4) Uani 1 1 d . . . H3 H 0.2476 0.1820 0.1318 0.018 Uiso 1 1 calc R . . C5 C 0.21291(17) 0.11247(13) 0.2860(3) 0.0132(4) Uani 1 1 d . . . C6 C 0.2375(2) 0.09766(12) 0.4486(3) 0.0157(5) Uani 1 1 d . . . H2 H 0.2020 0.0576 0.4777 0.019 Uiso 1 1 calc R . . C11 C 0.38615(18) 0.16473(14) 0.8714(3) 0.0196(5) Uani 1 1 d . . . H4 H 0.3939 0.2208 0.8739 0.023 Uiso 1 1 calc R . . C12 C 0.3513(2) 0.04407(16) 0.7897(3) 0.0267(5) Uani 1 1 d . . . H5 H 0.3291 -0.0012 0.7208 0.032 Uiso 1 1 calc R . . C31 C 0.39056(18) 0.28659(13) 0.3234(3) 0.0162(5) Uani 1 1 d . . . C51 C 0.13576(16) 0.05843(12) 0.1570(3) 0.0129(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01090(9) 0.00803(8) 0.00736(10) 0.000 0.00322(6) 0.000 Ag2 0.03042(16) 0.03423(16) 0.00932(14) 0.000 0.00158(11) 0.000 O1 0.0515(12) 0.0319(10) 0.0277(10) -0.0122(8) 0.0252(10) -0.0273(9) O2 0.0382(11) 0.0353(9) 0.0151(9) 0.0039(8) 0.0057(8) -0.0225(9) O3 0.0172(7) 0.0180(7) 0.0098(7) 0.0008(6) 0.0036(6) -0.0004(6) O4 0.0307(9) 0.0257(9) 0.0138(8) -0.0004(7) 0.0053(7) -0.0172(7) N11 0.0185(9) 0.0174(9) 0.0113(9) 0.0005(7) 0.0041(7) -0.0040(8) N12 0.0239(10) 0.0261(10) 0.0127(10) -0.0003(8) 0.0025(8) -0.0043(9) N13 0.0405(13) 0.0264(11) 0.0166(10) 0.0021(9) 0.0038(9) -0.0127(10) C1 0.0161(10) 0.0159(9) 0.0105(10) 0.0012(8) 0.0044(8) -0.0008(8) C2 0.0143(10) 0.0148(9) 0.0148(11) -0.0007(8) 0.0044(8) -0.0018(8) C3 0.0151(10) 0.0128(9) 0.0180(12) 0.0011(8) 0.0083(9) -0.0018(7) C4 0.0164(10) 0.0163(9) 0.0128(10) 0.0020(8) 0.0072(8) 0.0002(8) C5 0.0142(10) 0.0122(8) 0.0106(10) -0.0008(8) 0.0030(8) -0.0024(8) C6 0.0187(11) 0.0152(10) 0.0129(12) 0.0008(7) 0.0067(9) -0.0032(8) C11 0.0223(11) 0.0198(11) 0.0122(11) -0.0020(8) 0.0033(9) -0.0011(9) C12 0.0371(14) 0.0202(11) 0.0155(11) 0.0024(10) 0.0045(10) -0.0090(11) C31 0.0167(11) 0.0135(9) 0.0201(12) 0.0018(8) 0.0096(9) -0.0022(8) C51 0.0128(9) 0.0125(9) 0.0106(10) 0.0009(8) 0.0024(8) 0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O4 2.2864(17) 4 ? Tb1 O4 2.2865(17) 3 ? Tb1 O3 2.3292(18) 8_556 ? Tb1 O3 2.3292(18) 7 ? Tb1 O1 2.4653(19) 2_655 ? Tb1 O1 2.4653(19) . ? Tb1 O2 2.4743(19) 2_655 ? Tb1 O2 2.4744(19) . ? Tb1 C31 2.821(2) . ? Tb1 C31 2.821(2) 2_655 ? Ag2 N12 2.105(2) . ? Ag2 N12 2.105(2) 2_657 ? O1 C31 1.252(3) . ? O2 C31 1.252(3) . ? O3 C51 1.250(3) . ? O3 Tb1 2.3291(18) 7 ? O4 C51 1.244(3) . ? O4 Tb1 2.2865(17) 3_445 ? N11 C11 1.351(3) . ? N11 C12 1.363(3) . ? N11 C1 1.428(3) . ? N12 C11 1.306(3) . ? N12 N13 1.385(3) . ? N13 C12 1.300(3) . ? C1 C2 1.384(3) . ? C1 C6 1.389(3) . ? C2 C3 1.393(3) . ? C2 H1 0.9500 . ? C3 C4 1.393(3) . ? C3 C31 1.509(3) . ? C4 C5 1.397(3) . ? C4 H3 0.9500 . ? C5 C6 1.386(3) . ? C5 C51 1.518(3) . ? C6 H2 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O4 86.59(10) 4 3 ? O4 Tb1 O3 85.81(6) 4 8_556 ? O4 Tb1 O3 78.79(6) 3 8_556 ? O4 Tb1 O3 78.79(6) 4 7 ? O4 Tb1 O3 85.82(6) 3 7 ? O3 Tb1 O3 158.82(8) 8_556 7 ? O4 Tb1 O1 150.96(6) 4 2_655 ? O4 Tb1 O1 83.08(7) 3 2_655 ? O3 Tb1 O1 118.36(7) 8_556 2_655 ? O3 Tb1 O1 73.46(7) 7 2_655 ? O4 Tb1 O1 83.08(7) 4 . ? O4 Tb1 O1 150.96(6) 3 . ? O3 Tb1 O1 73.46(7) 8_556 . ? O3 Tb1 O1 118.36(7) 7 . ? O1 Tb1 O1 117.62(10) 2_655 . ? O4 Tb1 O2 156.41(6) 4 2_655 ? O4 Tb1 O2 102.28(8) 3 2_655 ? O3 Tb1 O2 74.77(6) 8_556 2_655 ? O3 Tb1 O2 123.22(6) 7 2_655 ? O1 Tb1 O2 52.62(7) 2_655 2_655 ? O1 Tb1 O2 78.68(8) . 2_655 ? O4 Tb1 O2 102.28(8) 4 . ? O4 Tb1 O2 156.41(6) 3 . ? O3 Tb1 O2 123.21(6) 8_556 . ? O3 Tb1 O2 74.77(6) 7 . ? O1 Tb1 O2 78.68(8) 2_655 . ? O1 Tb1 O2 52.62(7) . . ? O2 Tb1 O2 78.27(11) 2_655 . ? O4 Tb1 C31 93.00(8) 4 . ? O4 Tb1 C31 177.19(7) 3 . ? O3 Tb1 C31 98.42(7) 8_556 . ? O3 Tb1 C31 96.83(7) 7 . ? O1 Tb1 C31 98.54(7) 2_655 . ? O1 Tb1 C31 26.31(7) . . ? O2 Tb1 C31 77.07(8) 2_655 . ? O2 Tb1 C31 26.31(7) . . ? O4 Tb1 C31 177.19(7) 4 2_655 ? O4 Tb1 C31 92.99(8) 3 2_655 ? O3 Tb1 C31 96.83(7) 8_556 2_655 ? O3 Tb1 C31 98.42(7) 7 2_655 ? O1 Tb1 C31 26.31(7) 2_655 2_655 ? O1 Tb1 C31 98.55(7) . 2_655 ? O2 Tb1 C31 26.31(7) 2_655 2_655 ? O2 Tb1 C31 77.07(8) . 2_655 ? C31 Tb1 C31 87.55(10) . 2_655 ? N12 Ag2 N12 161.13(12) . 2_657 ? C31 O1 Tb1 92.92(15) . . ? C31 O2 Tb1 92.50(14) . . ? C51 O3 Tb1 142.02(14) . 7 ? C51 O4 Tb1 171.46(16) . 3_445 ? C11 N11 C12 104.7(2) . . ? C11 N11 C1 130.0(2) . . ? C12 N11 C1 125.3(2) . . ? C11 N12 N13 108.7(2) . . ? C11 N12 Ag2 132.22(18) . . ? N13 N12 Ag2 117.70(16) . . ? C12 N13 N12 105.4(2) . . ? C2 C1 C6 121.4(2) . . ? C2 C1 N11 120.09(19) . . ? C6 C1 N11 118.5(2) . . ? C1 C2 C3 118.9(2) . . ? C1 C2 H1 120.5 . . ? C3 C2 H1 120.5 . . ? C2 C3 C4 120.6(2) . . ? C2 C3 C31 118.4(2) . . ? C4 C3 C31 121.0(2) . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H3 120.3 . . ? C5 C4 H3 120.3 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 C51 118.71(19) . . ? C4 C5 C51 120.8(2) . . ? C5 C6 C1 119.2(2) . . ? C5 C6 H2 120.4 . . ? C1 C6 H2 120.4 . . ? N12 C11 N11 109.6(2) . . ? N12 C11 H4 125.2 . . ? N11 C11 H4 125.2 . . ? N13 C12 N11 111.6(2) . . ? N13 C12 H5 124.2 . . ? N11 C12 H5 124.2 . . ? O2 C31 O1 122.0(2) . . ? O2 C31 C3 119.1(2) . . ? O1 C31 C3 118.9(2) . . ? O2 C31 Tb1 61.19(12) . . ? O1 C31 Tb1 60.78(13) . . ? C3 C31 Tb1 177.60(16) . . ? O4 C51 O3 125.5(2) . . ? O4 C51 C5 117.3(2) . . ? O3 C51 C5 117.08(19) . . ? 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 O4 Tb1 O1 C31 111.37(17) 4 . . . ? O4 Tb1 O1 C31 -178.63(14) 3 . . . ? O3 Tb1 O1 C31 -160.96(17) 8_556 . . . ? O3 Tb1 O1 C31 38.11(18) 7 . . . ? O1 Tb1 O1 C31 -47.14(14) 2_655 . . . ? O2 Tb1 O1 C31 -83.68(16) 2_655 . . . ? O2 Tb1 O1 C31 0.12(15) . . . . ? C31 Tb1 O1 C31 -66.33(19) 2_655 . . . ? O4 Tb1 O2 C31 -71.37(16) 4 . . . ? O4 Tb1 O2 C31 178.36(16) 3 . . . ? O3 Tb1 O2 C31 21.68(19) 8_556 . . . ? O3 Tb1 O2 C31 -145.97(17) 7 . . . ? O1 Tb1 O2 C31 138.29(17) 2_655 . . . ? O1 Tb1 O2 C31 -0.12(15) . . . . ? O2 Tb1 O2 C31 84.51(16) 2_655 . . . ? C31 Tb1 O2 C31 111.42(16) 2_655 . . . ? N12 Ag2 N12 C11 -162.2(2) 2_657 . . . ? N12 Ag2 N12 N13 2.67(17) 2_657 . . . ? C11 N12 N13 C12 0.1(3) . . . . ? Ag2 N12 N13 C12 -168.14(19) . . . . ? C11 N11 C1 C2 32.8(4) . . . . ? C12 N11 C1 C2 -144.0(2) . . . . ? C11 N11 C1 C6 -150.4(2) . . . . ? C12 N11 C1 C6 32.8(3) . . . . ? C6 C1 C2 C3 -3.1(3) . . . . ? N11 C1 C2 C3 173.6(2) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C1 C2 C3 C31 -178.7(2) . . . . ? C2 C3 C4 C5 3.1(3) . . . . ? C31 C3 C4 C5 -179.0(2) . . . . ? C3 C4 C5 C6 -1.8(3) . . . . ? C3 C4 C5 C51 -177.85(19) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C51 C5 C6 C1 174.3(2) . . . . ? C2 C1 C6 C5 4.3(3) . . . . ? N11 C1 C6 C5 -172.4(2) . . . . ? N13 N12 C11 N11 -0.1(3) . . . . ? Ag2 N12 C11 N11 165.85(18) . . . . ? C12 N11 C11 N12 0.0(3) . . . . ? C1 N11 C11 N12 -177.3(2) . . . . ? N12 N13 C12 N11 -0.1(3) . . . . ? C11 N11 C12 N13 0.1(3) . . . . ? C1 N11 C12 N13 177.6(2) . . . . ? Tb1 O2 C31 O1 0.2(3) . . . . ? Tb1 O2 C31 C3 -177.27(18) . . . . ? Tb1 O1 C31 O2 -0.2(3) . . . . ? Tb1 O1 C31 C3 177.27(18) . . . . ? C2 C3 C31 O2 169.2(2) . . . . ? C4 C3 C31 O2 -8.8(3) . . . . ? C2 C3 C31 O1 -8.4(3) . . . . ? C4 C3 C31 O1 173.6(2) . . . . ? O4 Tb1 C31 O2 112.00(16) 4 . . . ? O3 Tb1 C31 O2 -161.80(16) 8_556 . . . ? O3 Tb1 C31 O2 32.94(17) 7 . . . ? O1 Tb1 C31 O2 -41.28(17) 2_655 . . . ? O1 Tb1 C31 O2 179.8(3) . . . . ? O2 Tb1 C31 O2 -89.64(18) 2_655 . . . ? C31 Tb1 C31 O2 -65.25(15) 2_655 . . . ? O4 Tb1 C31 O1 -67.78(17) 4 . . . ? O3 Tb1 C31 O1 18.43(17) 8_556 . . . ? O3 Tb1 C31 O1 -146.84(16) 7 . . . ? O1 Tb1 C31 O1 138.94(14) 2_655 . . . ? O2 Tb1 C31 O1 90.58(17) 2_655 . . . ? O2 Tb1 C31 O1 -179.8(3) . . . . ? C31 Tb1 C31 O1 114.97(18) 2_655 . . . ? Tb1 O3 C51 O4 60.9(3) 7 . . . ? Tb1 O3 C51 C5 -123.8(2) 7 . . . ? C6 C5 C51 O4 4.3(3) . . . . ? C4 C5 C51 O4 -179.6(2) . . . . ? C6 C5 C51 O3 -171.4(2) . . . . ? C4 C5 C51 O3 4.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.330 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.161 data_7 _database_code_depnum_ccdc_archive 'CCDC 803748' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2011-03-03 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Ag Er N6 O10' _chemical_formula_sum 'C20 H14 Ag Er N6 O10' _chemical_formula_weight 773.50 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.580(2) _cell_length_b 9.975(3) _cell_length_c 14.591(6) _cell_angle_alpha 92.161(14) _cell_angle_beta 92.420(13) _cell_angle_gamma 109.510(12) _cell_volume 1037.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9640 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 5.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5185 _exptl_absorpt_correction_T_max 0.7867 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 9743 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4654 _reflns_number_gt 4521 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0258P)^2^+0.6693P] 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 4654 _refine_ls_number_parameters 356 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0477 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.467328(13) 0.516862(10) 0.282746(6) 0.00887(4) Uani 1 1 d . . . Ag1 Ag -0.04190(3) 0.01656(3) 0.878315(14) 0.02643(6) Uani 1 1 d . . . O1 O 0.3258(3) 0.3482(2) 0.39428(12) 0.0193(4) Uani 1 1 d . . . O2 O 0.4542(3) 0.27387(19) 0.27941(12) 0.0174(4) Uani 1 1 d . . . O3 O 0.4637(2) -0.24021(19) 0.27627(11) 0.0142(3) Uani 1 1 d . . . O4 O 0.3352(2) -0.36766(19) 0.39073(12) 0.0151(3) Uani 1 1 d . . . O5 O 0.2659(2) 0.4241(2) -0.21279(13) 0.0249(4) Uani 1 1 d . . . O6 O -0.0133(3) 0.2836(2) -0.27100(12) 0.0240(4) Uani 1 1 d . . . O7 O 0.3826(2) 0.4847(2) 0.12521(12) 0.0232(4) Uani 1 1 d . . . O8 O 0.1507(2) 0.4270(2) 0.21656(12) 0.0186(4) Uani 1 1 d . . . O9 O 0.6932(3) 0.5796(2) 0.40779(13) 0.0246(4) Uani 1 1 d D . . H11 H 0.787(3) 0.557(4) 0.401(2) 0.030 Uiso 1 1 d D . . H12 H 0.685(5) 0.590(4) 0.4634(8) 0.030 Uiso 1 1 d D . . O10 O 0.9563(3) 0.4541(3) 0.39073(17) 0.0343(5) Uani 1 1 d D . . H13 H 1.059(4) 0.498(4) 0.423(2) 0.041 Uiso 1 1 d D . . H14 H 0.986(5) 0.436(4) 0.3352(16) 0.041 Uiso 1 1 d D . . N112 N -0.7047(3) 0.0931(2) 0.05303(14) 0.0157(4) Uani 1 1 d . . . N113 N -0.7339(3) 0.0972(2) -0.04074(14) 0.0168(4) Uani 1 1 d . . . N111 N -0.4324(3) 0.1943(2) -0.00372(13) 0.0125(4) Uani 1 1 d . . . N12 N 0.1030(3) -0.0021(3) 0.75397(15) 0.0201(4) Uani 1 1 d . . . N13 N 0.1754(3) -0.1133(3) 0.75910(15) 0.0232(5) Uani 1 1 d . . . N11 N 0.1821(3) -0.0451(2) 0.61733(13) 0.0137(4) Uani 1 1 d . . . C1 C 0.2309(3) -0.0319(3) 0.52416(15) 0.0117(4) Uani 1 1 d . . . C2 C 0.2623(3) 0.0960(3) 0.48276(16) 0.0125(4) Uani 1 1 d . . . H1 H 0.2415 0.1738 0.5145 0.015 Uiso 1 1 calc R . . C3 C 0.3247(3) 0.1091(2) 0.39397(16) 0.0116(4) Uani 1 1 d . . . C4 C 0.3582(3) -0.0044(3) 0.34796(15) 0.0120(4) Uani 1 1 d . . . H2 H 0.4013 0.0049 0.2876 0.014 Uiso 1 1 calc R . . C5 C 0.3279(3) -0.1314(2) 0.39116(15) 0.0111(4) Uani 1 1 d . . . C6 C 0.2596(3) -0.1470(3) 0.47837(16) 0.0128(4) Uani 1 1 d . . . H3 H 0.2328 -0.2355 0.5065 0.015 Uiso 1 1 calc R . . C11 C 0.1107(3) 0.0382(3) 0.67011(16) 0.0161(5) Uani 1 1 d . . . H4 H 0.0726 0.1138 0.6489 0.019 Uiso 1 1 calc R . . C12 C 0.2190(4) -0.1365(3) 0.67666(17) 0.0198(5) Uani 1 1 d . . . H5 H 0.2703 -0.2080 0.6595 0.024 Uiso 1 1 calc R . . C31 C 0.3691(3) 0.2512(3) 0.35304(16) 0.0128(4) Uani 1 1 d . . . C51 C 0.3754(3) -0.2538(2) 0.34904(15) 0.0112(4) Uani 1 1 d . . . C101 C -0.2342(3) 0.2572(3) -0.01236(15) 0.0116(4) Uani 1 1 d . . . C102 C -0.1141(3) 0.3098(3) 0.06503(16) 0.0130(4) Uani 1 1 d . . . H6 H -0.1619 0.3038 0.1245 0.016 Uiso 1 1 calc R . . C103 C 0.0771(3) 0.3714(3) 0.05434(16) 0.0121(4) Uani 1 1 d . . . C104 C 0.1487(3) 0.3833(2) -0.03271(16) 0.0121(4) Uani 1 1 d . . . H7 H 0.2794 0.4267 -0.0392 0.015 Uiso 1 1 calc R . . C105 C 0.0274(3) 0.3312(3) -0.10998(15) 0.0116(4) Uani 1 1 d . . . C106 C -0.1644(3) 0.2661(3) -0.09980(16) 0.0122(4) Uani 1 1 d . . . H8 H -0.2471 0.2280 -0.1523 0.015 Uiso 1 1 calc R . . C111 C -0.5246(3) 0.1518(3) 0.07335(16) 0.0169(5) Uani 1 1 d . . . H9 H -0.4668 0.1630 0.1335 0.020 Uiso 1 1 calc R . . C112 C -0.5701(3) 0.1585(3) -0.07285(16) 0.0168(5) Uani 1 1 d . . . H10 H -0.5492 0.1759 -0.1357 0.020 Uiso 1 1 calc R . . C131 C 0.0966(3) 0.3462(3) -0.20632(16) 0.0142(5) Uani 1 1 d . . . C151 C 0.2099(3) 0.4307(3) 0.13692(16) 0.0128(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.00896(6) 0.00868(6) 0.00906(6) 0.00055(4) 0.00107(4) 0.00300(4) Ag1 0.01607(10) 0.04227(14) 0.02047(10) 0.00715(9) 0.00990(8) 0.00754(9) O1 0.0315(10) 0.0136(9) 0.0175(8) 0.0038(7) 0.0086(7) 0.0126(8) O2 0.0249(9) 0.0129(8) 0.0166(8) 0.0037(7) 0.0081(7) 0.0082(8) O3 0.0173(8) 0.0123(8) 0.0142(8) 0.0020(6) 0.0046(6) 0.0061(7) O4 0.0197(8) 0.0113(8) 0.0157(8) 0.0033(6) 0.0056(6) 0.0064(7) O5 0.0111(8) 0.0390(12) 0.0169(9) -0.0018(8) 0.0033(7) -0.0015(8) O6 0.0154(9) 0.0364(12) 0.0156(8) -0.0081(8) -0.0009(7) 0.0039(8) O7 0.0103(8) 0.0401(12) 0.0133(8) 0.0002(8) 0.0002(6) 0.0008(8) O8 0.0125(8) 0.0268(10) 0.0137(8) -0.0013(7) 0.0003(6) 0.0033(8) O9 0.0197(9) 0.0383(12) 0.0176(9) -0.0045(8) -0.0046(7) 0.0132(9) O10 0.0247(11) 0.0351(13) 0.0415(13) 0.0018(10) 0.0054(9) 0.0074(10) N112 0.0136(9) 0.0181(11) 0.0135(9) 0.0009(8) 0.0037(7) 0.0025(8) N113 0.0135(9) 0.0221(11) 0.0140(9) 0.0031(8) 0.0021(8) 0.0044(9) N111 0.0098(9) 0.0140(10) 0.0119(9) 0.0002(7) 0.0010(7) 0.0017(8) N12 0.0182(10) 0.0260(12) 0.0153(10) 0.0016(9) 0.0038(8) 0.0062(9) N13 0.0294(12) 0.0247(12) 0.0177(10) 0.0081(9) 0.0065(9) 0.0106(10) N11 0.0151(9) 0.0137(10) 0.0133(9) 0.0022(8) 0.0033(7) 0.0057(8) C1 0.0112(10) 0.0124(11) 0.0106(10) -0.0002(8) -0.0010(8) 0.0030(9) C2 0.0124(10) 0.0119(11) 0.0132(10) -0.0015(8) -0.0003(8) 0.0043(9) C3 0.0124(10) 0.0092(11) 0.0133(10) 0.0026(8) 0.0003(8) 0.0036(9) C4 0.0124(10) 0.0115(11) 0.0118(10) 0.0008(8) 0.0005(8) 0.0037(9) C5 0.0096(10) 0.0104(11) 0.0128(10) -0.0013(8) -0.0002(8) 0.0030(9) C6 0.0149(10) 0.0104(11) 0.0133(10) 0.0020(8) 0.0010(8) 0.0043(9) C11 0.0164(11) 0.0183(12) 0.0137(10) -0.0010(9) 0.0014(9) 0.0062(10) C12 0.0244(13) 0.0185(13) 0.0178(11) 0.0049(10) 0.0030(10) 0.0082(11) C31 0.0146(10) 0.0113(11) 0.0137(10) 0.0007(9) 0.0000(8) 0.0060(9) C51 0.0100(10) 0.0107(10) 0.0121(10) -0.0011(8) -0.0019(8) 0.0031(9) C101 0.0080(10) 0.0120(11) 0.0141(10) 0.0021(8) 0.0016(8) 0.0020(9) C102 0.0138(11) 0.0125(11) 0.0125(10) 0.0023(8) 0.0016(8) 0.0039(9) C103 0.0122(10) 0.0109(11) 0.0131(10) 0.0009(8) -0.0009(8) 0.0039(9) C104 0.0093(10) 0.0116(11) 0.0148(10) 0.0000(8) 0.0004(8) 0.0027(9) C105 0.0109(10) 0.0116(11) 0.0126(10) 0.0006(8) 0.0015(8) 0.0039(9) C106 0.0105(10) 0.0134(11) 0.0123(10) -0.0004(8) 0.0001(8) 0.0035(9) C111 0.0129(11) 0.0217(13) 0.0126(10) 0.0000(9) 0.0013(8) 0.0012(10) C112 0.0101(10) 0.0240(13) 0.0138(11) 0.0039(9) 0.0004(8) 0.0022(10) C131 0.0102(10) 0.0177(12) 0.0147(11) -0.0003(9) 0.0023(8) 0.0047(9) C151 0.0129(10) 0.0126(11) 0.0128(10) 0.0008(8) -0.0026(8) 0.0044(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 Er1 O5 2.2138(19) 2_665 ? Er1 O7 2.341(2) . ? Er1 O4 2.3618(17) 1_565 ? Er1 O9 2.363(2) . ? Er1 O2 2.3910(19) . ? Er1 O1 2.404(2) . ? Er1 O8 2.4081(19) . ? Er1 O3 2.4378(19) 1_565 ? Er1 C151 2.732(2) . ? Er1 C31 2.753(3) . ? Er1 C51 2.758(2) 1_565 ? Ag1 N112 2.175(2) 2_456 ? Ag1 N12 2.194(2) . ? Ag1 N113 2.436(2) 1_656 ? O1 C31 1.261(3) . ? O2 C31 1.265(3) . ? O3 C51 1.266(3) . ? O3 Er1 2.4378(19) 1_545 ? O4 C51 1.261(3) . ? O4 Er1 2.3618(17) 1_545 ? O5 C131 1.268(3) . ? O5 Er1 2.2138(18) 2_665 ? O6 C131 1.232(3) . ? O7 C151 1.259(3) . ? O8 C151 1.261(3) . ? O9 H11 0.821(10) . ? O9 H12 0.822(10) . ? O10 H13 0.862(19) . ? O10 H14 0.878(19) . ? N112 C111 1.309(3) . ? N112 N113 1.381(3) . ? N112 Ag1 2.175(2) 2_456 ? N113 C112 1.303(3) . ? N113 Ag1 2.436(2) 1_454 ? N111 C111 1.355(3) . ? N111 C112 1.367(3) . ? N111 C101 1.435(3) . ? N12 C11 1.300(3) . ? N12 N13 1.394(3) . ? N13 C12 1.294(3) . ? N11 C11 1.366(3) . ? N11 C12 1.367(3) . ? N11 C1 1.423(3) . ? C1 C2 1.384(3) . ? C1 C6 1.391(3) . ? C2 C3 1.394(3) . ? C2 H1 0.9500 . ? C3 C4 1.395(3) . ? C3 C31 1.497(3) . ? C4 C5 1.390(3) . ? C4 H2 0.9500 . ? C5 C6 1.389(3) . ? C5 C51 1.502(3) . ? C6 H3 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? C51 Er1 2.758(2) 1_545 ? C101 C102 1.389(3) . ? C101 C106 1.396(3) . ? C102 C103 1.390(3) . ? C102 H6 0.9500 . ? C103 C104 1.396(3) . ? C103 C151 1.504(3) . ? C104 C105 1.391(3) . ? C104 H7 0.9500 . ? C105 C106 1.397(3) . ? C105 C131 1.516(3) . ? C106 H8 0.9500 . ? C111 H9 0.9500 . ? C112 H10 0.9500 . ? 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 O5 Er1 O7 74.23(7) 2_665 . ? O5 Er1 O4 135.10(7) 2_665 1_565 ? O7 Er1 O4 124.65(7) . 1_565 ? O5 Er1 O9 77.75(7) 2_665 . ? O7 Er1 O9 151.98(7) . . ? O4 Er1 O9 76.75(7) 1_565 . ? O5 Er1 O2 90.15(7) 2_665 . ? O7 Er1 O2 87.94(7) . . ? O4 Er1 O2 126.90(6) 1_565 . ? O9 Er1 O2 91.93(7) . . ? O5 Er1 O1 134.94(7) 2_665 . ? O7 Er1 O1 124.33(7) . . ? O4 Er1 O1 72.38(6) 1_565 . ? O9 Er1 O1 76.69(8) . . ? O2 Er1 O1 54.57(6) . . ? O5 Er1 O8 128.95(7) 2_665 . ? O7 Er1 O8 54.78(6) . . ? O4 Er1 O8 83.07(6) 1_565 . ? O9 Er1 O8 153.17(7) . . ? O2 Er1 O8 86.15(7) . . ? O1 Er1 O8 80.49(7) . . ? O5 Er1 O3 90.66(7) 2_665 1_565 ? O7 Er1 O3 88.21(7) . 1_565 ? O4 Er1 O3 54.44(6) 1_565 1_565 ? O9 Er1 O3 92.37(7) . 1_565 ? O2 Er1 O3 175.70(6) . 1_565 ? O1 Er1 O3 126.75(6) . 1_565 ? O8 Er1 O3 90.07(7) . 1_565 ? O5 Er1 C151 101.47(7) 2_665 . ? O7 Er1 C151 27.39(7) . . ? O4 Er1 C151 105.67(7) 1_565 . ? O9 Er1 C151 176.89(7) . . ? O2 Er1 C151 85.05(7) . . ? O1 Er1 C151 102.06(8) . . ? O8 Er1 C151 27.48(7) . . ? O3 Er1 C151 90.66(7) 1_565 . ? O5 Er1 C31 113.40(8) 2_665 . ? O7 Er1 C31 107.51(7) . . ? O4 Er1 C31 99.60(7) 1_565 . ? O9 Er1 C31 83.38(8) . . ? O2 Er1 C31 27.34(6) . . ? O1 Er1 C31 27.23(6) . . ? O8 Er1 C31 82.75(7) . . ? O3 Er1 C31 153.84(6) 1_565 . ? C151 Er1 C31 94.23(7) . . ? O5 Er1 C51 114.20(8) 2_665 1_565 ? O7 Er1 C51 107.34(7) . 1_565 ? O4 Er1 C51 27.11(7) 1_565 1_565 ? O9 Er1 C51 84.32(7) . 1_565 ? O2 Er1 C51 153.75(7) . 1_565 ? O1 Er1 C51 99.44(7) . 1_565 ? O8 Er1 C51 85.70(7) . 1_565 ? O3 Er1 C51 27.33(6) 1_565 1_565 ? C151 Er1 C51 98.72(7) . 1_565 ? C31 Er1 C51 126.61(7) . 1_565 ? N112 Ag1 N12 140.91(8) 2_456 . ? N112 Ag1 N113 121.85(8) 2_456 1_656 ? N12 Ag1 N113 86.69(8) . 1_656 ? C31 O1 Er1 91.99(15) . . ? C31 O2 Er1 92.47(14) . . ? C51 O3 Er1 90.57(14) . 1_545 ? C51 O4 Er1 94.24(14) . 1_545 ? C131 O5 Er1 151.44(17) . 2_665 ? C151 O7 Er1 93.85(14) . . ? C151 O8 Er1 90.71(14) . . ? Er1 O9 H11 116(3) . . ? Er1 O9 H12 133(3) . . ? H11 O9 H12 107(3) . . ? H13 O10 H14 107(4) . . ? C111 N112 N113 107.6(2) . . ? C111 N112 Ag1 138.58(17) . 2_456 ? N113 N112 Ag1 113.64(15) . 2_456 ? C112 N113 N112 106.8(2) . . ? C112 N113 Ag1 129.01(17) . 1_454 ? N112 N113 Ag1 124.12(15) . 1_454 ? C111 N111 C112 104.55(19) . . ? C111 N111 C101 128.2(2) . . ? C112 N111 C101 127.2(2) . . ? C11 N12 N13 108.8(2) . . ? C11 N12 Ag1 138.75(19) . . ? N13 N12 Ag1 110.62(16) . . ? C12 N13 N12 105.8(2) . . ? C11 N11 C12 104.8(2) . . ? C11 N11 C1 128.9(2) . . ? C12 N11 C1 125.9(2) . . ? C2 C1 C6 121.0(2) . . ? C2 C1 N11 120.6(2) . . ? C6 C1 N11 118.2(2) . . ? C1 C2 C3 119.2(2) . . ? C1 C2 H1 120.4 . . ? C3 C2 H1 120.4 . . ? C2 C3 C4 120.4(2) . . ? C2 C3 C31 118.1(2) . . ? C4 C3 C31 121.3(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H2 120.2 . . ? C3 C4 H2 120.2 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 C51 117.0(2) . . ? C4 C5 C51 122.4(2) . . ? C5 C6 C1 119.3(2) . . ? C5 C6 H3 120.3 . . ? C1 C6 H3 120.3 . . ? N12 C11 N11 109.2(2) . . ? N12 C11 H4 125.4 . . ? N11 C11 H4 125.4 . . ? N13 C12 N11 111.4(2) . . ? N13 C12 H5 124.3 . . ? N11 C12 H5 124.3 . . ? O1 C31 O2 121.0(2) . . ? O1 C31 C3 119.2(2) . . ? O2 C31 C3 119.8(2) . . ? O1 C31 Er1 60.78(13) . . ? O2 C31 Er1 60.20(13) . . ? C3 C31 Er1 177.17(16) . . ? O4 C51 O3 120.7(2) . . ? O4 C51 C5 118.4(2) . . ? O3 C51 C5 120.7(2) . . ? O4 C51 Er1 58.64(12) . 1_545 ? O3 C51 Er1 62.11(12) . 1_545 ? C5 C51 Er1 176.38(16) . 1_545 ? C102 C101 C106 120.6(2) . . ? C102 C101 N111 120.4(2) . . ? C106 C101 N111 119.0(2) . . ? C101 C102 C103 119.1(2) . . ? C101 C102 H6 120.5 . . ? C103 C102 H6 120.5 . . ? C102 C103 C104 121.0(2) . . ? C102 C103 C151 120.2(2) . . ? C104 C103 C151 118.8(2) . . ? C105 C104 C103 119.6(2) . . ? C105 C104 H7 120.2 . . ? C103 C104 H7 120.2 . . ? C104 C105 C106 119.8(2) . . ? C104 C105 C131 121.8(2) . . ? C106 C105 C131 118.4(2) . . ? C101 C106 C105 119.9(2) . . ? C101 C106 H8 120.1 . . ? C105 C106 H8 120.1 . . ? N112 C111 N111 110.3(2) . . ? N112 C111 H9 124.9 . . ? N111 C111 H9 124.9 . . ? N113 C112 N111 110.8(2) . . ? N113 C112 H10 124.6 . . ? N111 C112 H10 124.6 . . ? O6 C131 O5 125.6(2) . . ? O6 C131 C105 118.5(2) . . ? O5 C131 C105 116.0(2) . . ? O7 C151 O8 120.3(2) . . ? O7 C151 C103 118.7(2) . . ? O8 C151 C103 121.0(2) . . ? O7 C151 Er1 58.77(12) . . ? O8 C151 Er1 61.81(12) . . ? C103 C151 Er1 173.99(16) . . ? 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 O5 Er1 O1 C31 -44.55(18) 2_665 . . . ? O7 Er1 O1 C31 57.96(16) . . . . ? O4 Er1 O1 C31 178.31(16) 1_565 . . . ? O9 Er1 O1 C31 -101.59(15) . . . . ? O2 Er1 O1 C31 0.59(13) . . . . ? O8 Er1 O1 C31 92.63(15) . . . . ? O3 Er1 O1 C31 175.52(13) 1_565 . . . ? C151 Er1 O1 C31 75.49(15) . . . . ? C51 Er1 O1 C31 176.61(14) 1_565 . . . ? O5 Er1 O2 C31 149.30(15) 2_665 . . . ? O7 Er1 O2 C31 -136.48(15) . . . . ? O4 Er1 O2 C31 -3.29(17) 1_565 . . . ? O9 Er1 O2 C31 71.55(15) . . . . ? O1 Er1 O2 C31 -0.58(13) . . . . ? O8 Er1 O2 C31 -81.65(15) . . . . ? C151 Er1 O2 C31 -109.19(15) . . . . ? C51 Er1 O2 C31 -9.5(2) 1_565 . . . ? O5 Er1 O7 C151 173.93(18) 2_665 . . . ? O4 Er1 O7 C151 -51.67(18) 1_565 . . . ? O9 Er1 O7 C151 173.44(15) . . . . ? O2 Er1 O7 C151 83.20(16) . . . . ? O1 Er1 O7 C151 39.83(18) . . . . ? O8 Er1 O7 C151 -3.54(14) . . . . ? O3 Er1 O7 C151 -94.88(16) 1_565 . . . ? C31 Er1 O7 C151 63.83(17) . . . . ? C51 Er1 O7 C151 -75.08(17) 1_565 . . . ? O5 Er1 O8 C151 0.40(19) 2_665 . . . ? O7 Er1 O8 C151 3.53(14) . . . . ? O4 Er1 O8 C151 145.42(15) 1_565 . . . ? O9 Er1 O8 C151 -173.33(16) . . . . ? O2 Er1 O8 C151 -86.67(15) . . . . ? O1 Er1 O8 C151 -141.37(16) . . . . ? O3 Er1 O8 C151 91.29(15) 1_565 . . . ? C31 Er1 O8 C151 -113.93(16) . . . . ? C51 Er1 O8 C151 118.30(15) 1_565 . . . ? C111 N112 N113 C112 -0.1(3) . . . . ? Ag1 N112 N113 C112 -176.60(17) 2_456 . . . ? C111 N112 N113 Ag1 -176.46(17) . . . 1_454 ? Ag1 N112 N113 Ag1 7.0(2) 2_456 . . 1_454 ? N112 Ag1 N12 C11 90.7(3) 2_456 . . . ? N113 Ag1 N12 C11 -129.2(3) 1_656 . . . ? N112 Ag1 N12 N13 -71.1(2) 2_456 . . . ? N113 Ag1 N12 N13 69.02(18) 1_656 . . . ? C11 N12 N13 C12 -1.5(3) . . . . ? Ag1 N12 N13 C12 165.93(18) . . . . ? C11 N11 C1 C2 19.5(4) . . . . ? C12 N11 C1 C2 -152.0(2) . . . . ? C11 N11 C1 C6 -165.2(2) . . . . ? C12 N11 C1 C6 23.3(4) . . . . ? C6 C1 C2 C3 -0.4(3) . . . . ? N11 C1 C2 C3 174.8(2) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C1 C2 C3 C31 -176.2(2) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C31 C3 C4 C5 175.3(2) . . . . ? C3 C4 C5 C6 1.9(3) . . . . ? C3 C4 C5 C51 -175.0(2) . . . . ? C4 C5 C6 C1 -3.3(3) . . . . ? C51 C5 C6 C1 173.7(2) . . . . ? C2 C1 C6 C5 2.5(3) . . . . ? N11 C1 C6 C5 -172.7(2) . . . . ? N13 N12 C11 N11 1.5(3) . . . . ? Ag1 N12 C11 N11 -160.5(2) . . . . ? C12 N11 C11 N12 -1.0(3) . . . . ? C1 N11 C11 N12 -173.9(2) . . . . ? N12 N13 C12 N11 0.9(3) . . . . ? C11 N11 C12 N13 0.0(3) . . . . ? C1 N11 C12 N13 173.2(2) . . . . ? Er1 O1 C31 O2 -1.1(2) . . . . ? Er1 O1 C31 C3 176.76(19) . . . . ? Er1 O2 C31 O1 1.1(2) . . . . ? Er1 O2 C31 C3 -176.74(19) . . . . ? C2 C3 C31 O1 -9.3(3) . . . . ? C4 C3 C31 O1 175.6(2) . . . . ? C2 C3 C31 O2 168.6(2) . . . . ? C4 C3 C31 O2 -6.6(3) . . . . ? O5 Er1 C31 O1 147.24(14) 2_665 . . . ? O7 Er1 C31 O1 -132.77(14) . . . . ? O4 Er1 C31 O1 -1.63(15) 1_565 . . . ? O9 Er1 C31 O1 73.68(15) . . . . ? O2 Er1 C31 O1 -179.0(2) . . . . ? O8 Er1 C31 O1 -83.30(15) . . . . ? O3 Er1 C31 O1 -8.2(2) 1_565 . . . ? C151 Er1 C31 O1 -108.32(15) . . . . ? C51 Er1 C31 O1 -4.17(17) 1_565 . . . ? O5 Er1 C31 O2 -33.80(16) 2_665 . . . ? O7 Er1 C31 O2 46.19(15) . . . . ? O4 Er1 C31 O2 177.33(14) 1_565 . . . ? O9 Er1 C31 O2 -107.36(15) . . . . ? O1 Er1 C31 O2 179.0(2) . . . . ? O8 Er1 C31 O2 95.66(14) . . . . ? O3 Er1 C31 O2 170.81(13) 1_565 . . . ? C151 Er1 C31 O2 70.64(15) . . . . ? C51 Er1 C31 O2 174.79(13) 1_565 . . . ? Er1 O4 C51 O3 -1.7(2) 1_545 . . . ? Er1 O4 C51 C5 -177.59(17) 1_545 . . . ? Er1 O3 C51 O4 1.7(2) 1_545 . . . ? Er1 O3 C51 C5 177.44(18) 1_545 . . . ? C6 C5 C51 O4 6.4(3) . . . . ? C4 C5 C51 O4 -176.6(2) . . . . ? C6 C5 C51 O3 -169.5(2) . . . . ? C4 C5 C51 O3 7.5(3) . . . . ? C111 N111 C101 C102 -14.0(4) . . . . ? C112 N111 C101 C102 169.0(2) . . . . ? C111 N111 C101 C106 166.7(2) . . . . ? C112 N111 C101 C106 -10.3(4) . . . . ? C106 C101 C102 C103 -0.1(4) . . . . ? N111 C101 C102 C103 -179.4(2) . . . . ? C101 C102 C103 C104 1.2(4) . . . . ? C101 C102 C103 C151 179.3(2) . . . . ? C102 C103 C104 C105 -0.8(4) . . . . ? C151 C103 C104 C105 -178.9(2) . . . . ? C103 C104 C105 C106 -0.7(3) . . . . ? C103 C104 C105 C131 177.7(2) . . . . ? C102 C101 C106 C105 -1.4(4) . . . . ? N111 C101 C106 C105 177.9(2) . . . . ? C104 C105 C106 C101 1.8(4) . . . . ? C131 C105 C106 C101 -176.7(2) . . . . ? N113 N112 C111 N111 -0.3(3) . . . . ? Ag1 N112 C111 N111 174.83(19) 2_456 . . . ? C112 N111 C111 N112 0.6(3) . . . . ? C101 N111 C111 N112 -176.9(2) . . . . ? N112 N113 C112 N111 0.5(3) . . . . ? Ag1 N113 C112 N111 176.61(16) 1_454 . . . ? C111 N111 C112 N113 -0.7(3) . . . . ? C101 N111 C112 N113 176.9(2) . . . . ? Er1 O5 C131 O6 -28.7(6) 2_665 . . . ? Er1 O5 C131 C105 151.5(3) 2_665 . . . ? C104 C105 C131 O6 171.7(2) . . . . ? C106 C105 C131 O6 -9.9(3) . . . . ? C104 C105 C131 O5 -8.6(4) . . . . ? C106 C105 C131 O5 169.9(2) . . . . ? Er1 O7 C151 O8 6.4(3) . . . . ? Er1 O7 C151 C103 -173.69(19) . . . . ? Er1 O8 C151 O7 -6.2(3) . . . . ? Er1 O8 C151 C103 173.9(2) . . . . ? C102 C103 C151 O7 179.4(2) . . . . ? C104 C103 C151 O7 -2.5(3) . . . . ? C102 C103 C151 O8 -0.7(4) . . . . ? C104 C103 C151 O8 177.4(2) . . . . ? O5 Er1 C151 O7 -5.96(17) 2_665 . . . ? O4 Er1 C151 O7 137.91(16) 1_565 . . . ? O2 Er1 C151 O7 -95.10(16) . . . . ? O1 Er1 C151 O7 -147.25(16) . . . . ? O8 Er1 C151 O7 173.7(3) . . . . ? O3 Er1 C151 O7 84.84(16) 1_565 . . . ? C31 Er1 C151 O7 -120.88(16) . . . . ? C51 Er1 C151 O7 111.07(16) 1_565 . . . ? O5 Er1 C151 O8 -179.68(15) 2_665 . . . ? O7 Er1 C151 O8 -173.7(3) . . . . ? O4 Er1 C151 O8 -35.82(16) 1_565 . . . ? O2 Er1 C151 O8 91.17(15) . . . . ? O1 Er1 C151 O8 39.02(16) . . . . ? O3 Er1 C151 O8 -88.88(15) 1_565 . . . ? C31 Er1 C151 O8 65.39(15) . . . . ? C51 Er1 C151 O8 -62.66(16) 1_565 . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.402 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.161 data_8 _database_code_depnum_ccdc_archive 'CCDC 803749' #TrackingRef '- CE-ART-12-2010-000921-rev.cif' _audit_creation_date 2011-03-03 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Ag N6 O10 Yb' _chemical_formula_sum 'C20 H14 Ag N6 O10 Yb' _chemical_formula_weight 779.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.550(2) _cell_length_b 9.951(4) _cell_length_c 14.564(5) _cell_angle_alpha 92.128(16) _cell_angle_beta 92.460(13) _cell_angle_gamma 109.383(15) _cell_volume 1029.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9707 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 5.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4902 _exptl_absorpt_correction_T_max 0.6654 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 9840 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4685 _reflns_number_gt 4571 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0294P)^2^+1.0502P] 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 4685 _refine_ls_number_parameters 355 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.032274(14) -0.016449(10) 0.217385(7) 0.00887(5) Uani 1 1 d . . . Ag1 Ag 1.45832(3) 0.51741(3) 0.378359(17) 0.02677(7) Uani 1 1 d . . . O1 O 0.1150(3) 0.0151(3) 0.37404(14) 0.0232(5) Uani 1 1 d . . . O2 O 0.3472(3) 0.0731(2) 0.28230(14) 0.0188(4) Uani 1 1 d . . . O3 O 0.2319(3) 0.0741(3) 0.71306(15) 0.0246(5) Uani 1 1 d . . . O4 O 0.5113(3) 0.2143(3) 0.77160(15) 0.0242(5) Uani 1 1 d . . . O5 O 0.0440(3) 0.2251(2) 0.22179(14) 0.0176(4) Uani 1 1 d . . . O6 O 0.1722(3) 0.1512(2) 0.10640(14) 0.0199(4) Uani 1 1 d . . . O7 O 0.0356(3) 0.7413(2) 0.22480(13) 0.0145(4) Uani 1 1 d . . . O8 O 0.1640(3) 0.8687(2) 0.11033(14) 0.0152(4) Uani 1 1 d . . . O9 O -0.1914(3) -0.0792(3) 0.09390(16) 0.0251(5) Uani 1 1 d D . . H11 H -0.283(4) -0.056(4) 0.100(3) 0.030 Uiso 1 1 d D . . H12 H -0.163(6) -0.074(5) 0.0411(14) 0.030 Uiso 1 1 d D . . O10 O 0.5440(4) 0.0458(3) 0.1082(2) 0.0358(6) Uani 1 1 d D . . H13 H 0.451(5) -0.004(4) 0.074(3) 0.043 Uiso 1 1 d D . . H14 H 0.525(7) 0.076(5) 0.1614(19) 0.043 Uiso 1 1 d D . . N11 N 0.9315(3) 0.3053(2) 0.50374(15) 0.0122(4) Uani 1 1 d . . . N12 N 1.2043(3) 0.4069(3) 0.44679(16) 0.0153(4) Uani 1 1 d . . . N13 N 1.2335(3) 0.4030(3) 0.54081(17) 0.0168(5) Uani 1 1 d . . . N111 N 0.3191(3) 0.5453(2) -0.11634(16) 0.0141(4) Uani 1 1 d . . . N113 N 0.3270(4) 0.6140(3) -0.25843(19) 0.0249(6) Uani 1 1 d . . . N112 N 0.3980(4) 0.5017(3) -0.25326(17) 0.0209(5) Uani 1 1 d . . . C1 C 0.7323(3) 0.2422(3) 0.51219(18) 0.0114(5) Uani 1 1 d . . . C2 C 0.6131(4) 0.1901(3) 0.43458(18) 0.0127(5) Uani 1 1 d . . . H1 H 0.6614 0.1963 0.3751 0.015 Uiso 1 1 calc R . . C3 C 0.4209(4) 0.1283(3) 0.44525(18) 0.0123(5) Uani 1 1 d . . . C4 C 0.3496(4) 0.1158(3) 0.53254(18) 0.0121(5) Uani 1 1 d . . . H2 H 0.2186 0.0716 0.5390 0.015 Uiso 1 1 calc R . . C5 C 0.4706(4) 0.1680(3) 0.61009(18) 0.0118(5) Uani 1 1 d . . . C6 C 0.6631(4) 0.2336(3) 0.59988(18) 0.0117(5) Uani 1 1 d . . . H3 H 0.7462 0.2720 0.6524 0.014 Uiso 1 1 calc R . . C11 C 1.0243(4) 0.3477(3) 0.42624(19) 0.0170(5) Uani 1 1 d . . . H4 H 0.9665 0.3359 0.3659 0.020 Uiso 1 1 calc R . . C12 C 1.0691(4) 0.3415(3) 0.57300(19) 0.0171(5) Uani 1 1 d . . . H5 H 1.0481 0.3243 0.6360 0.020 Uiso 1 1 calc R . . C31 C 0.2883(4) 0.0690(3) 0.36250(18) 0.0128(5) Uani 1 1 d . . . C51 C 0.4011(4) 0.1525(3) 0.70675(19) 0.0148(5) Uani 1 1 d . . . C101 C 0.2693(4) 0.5321(3) -0.02340(18) 0.0128(5) Uani 1 1 d . . . C102 C 0.2371(4) 0.4039(3) 0.01829(19) 0.0131(5) Uani 1 1 d . . . H6 H 0.2578 0.3258 -0.0134 0.016 Uiso 1 1 calc R . . C103 C 0.1742(4) 0.3906(3) 0.10706(18) 0.0119(5) Uani 1 1 d . . . C104 C 0.1405(4) 0.5042(3) 0.15341(18) 0.0121(5) Uani 1 1 d . . . H7 H 0.0969 0.4946 0.2139 0.015 Uiso 1 1 calc R . . C105 C 0.1716(4) 0.6320(3) 0.10999(18) 0.0115(5) Uani 1 1 d . . . C106 C 0.2405(4) 0.6471(3) 0.02279(18) 0.0131(5) Uani 1 1 d . . . H8 H 0.2679 0.7359 -0.0052 0.016 Uiso 1 1 calc R . . C111 C 0.2826(4) 0.6371(3) -0.1760(2) 0.0205(6) Uani 1 1 d . . . H9 H 0.2310 0.7088 -0.1590 0.025 Uiso 1 1 calc R . . C112 C 0.3894(4) 0.4617(3) -0.16972(19) 0.0164(5) Uani 1 1 d . . . H10 H 0.4264 0.3852 -0.1486 0.020 Uiso 1 1 calc R . . C131 C 0.1294(4) 0.2479(3) 0.14783(19) 0.0135(5) Uani 1 1 d . . . C151 C 0.1232(4) 0.7544(3) 0.15210(18) 0.0112(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.00935(7) 0.00978(6) 0.00760(7) 0.00030(4) 0.00091(4) 0.00334(4) Ag1 0.01669(11) 0.04423(15) 0.01886(12) 0.00736(10) 0.00969(9) 0.00780(10) O1 0.0110(9) 0.0411(13) 0.0113(10) -0.0011(9) -0.0010(7) 0.0011(9) O2 0.0136(9) 0.0285(11) 0.0122(9) -0.0018(8) -0.0004(7) 0.0047(8) O3 0.0110(9) 0.0382(13) 0.0174(10) -0.0021(9) 0.0029(8) -0.0012(9) O4 0.0162(10) 0.0376(13) 0.0145(10) -0.0076(9) -0.0001(8) 0.0041(9) O5 0.0262(11) 0.0141(9) 0.0150(10) 0.0030(7) 0.0075(8) 0.0089(8) O6 0.0335(12) 0.0140(9) 0.0166(10) 0.0035(8) 0.0085(9) 0.0126(9) O7 0.0183(9) 0.0139(9) 0.0122(9) 0.0010(7) 0.0041(7) 0.0061(8) O8 0.0200(10) 0.0125(9) 0.0148(9) 0.0029(7) 0.0062(8) 0.0068(8) O9 0.0201(11) 0.0408(14) 0.0162(10) -0.0056(10) -0.0049(9) 0.0140(10) O10 0.0278(13) 0.0366(15) 0.0412(16) 0.0022(12) 0.0054(11) 0.0078(11) N11 0.0093(10) 0.0155(10) 0.0100(10) 0.0015(8) 0.0017(8) 0.0016(8) N12 0.0132(11) 0.0200(12) 0.0121(11) 0.0008(9) 0.0036(8) 0.0042(9) N13 0.0132(11) 0.0244(12) 0.0121(11) 0.0032(9) 0.0016(9) 0.0048(10) N111 0.0167(11) 0.0142(11) 0.0123(11) 0.0021(8) 0.0023(9) 0.0062(9) N113 0.0333(15) 0.0275(14) 0.0172(13) 0.0065(10) 0.0071(11) 0.0135(12) N112 0.0199(12) 0.0281(13) 0.0146(12) 0.0009(10) 0.0039(9) 0.0078(11) C1 0.0080(11) 0.0112(11) 0.0139(12) 0.0013(9) 0.0015(9) 0.0017(9) C2 0.0145(12) 0.0138(12) 0.0102(12) 0.0024(9) 0.0019(9) 0.0049(10) C3 0.0125(12) 0.0121(11) 0.0121(12) 0.0006(9) -0.0013(9) 0.0038(10) C4 0.0102(11) 0.0127(11) 0.0126(12) -0.0001(9) -0.0004(9) 0.0031(9) C5 0.0111(12) 0.0135(12) 0.0111(12) 0.0003(9) 0.0017(9) 0.0046(10) C6 0.0102(11) 0.0126(11) 0.0108(12) -0.0007(9) -0.0010(9) 0.0022(9) C11 0.0150(13) 0.0233(14) 0.0100(12) 0.0013(10) 0.0023(10) 0.0028(11) C12 0.0113(12) 0.0271(15) 0.0110(12) 0.0047(11) 0.0010(10) 0.0036(11) C31 0.0144(12) 0.0135(12) 0.0109(12) 0.0015(9) -0.0009(9) 0.0053(10) C51 0.0119(12) 0.0198(13) 0.0131(13) -0.0001(10) 0.0024(10) 0.0057(10) C101 0.0148(12) 0.0135(12) 0.0111(12) 0.0002(9) 0.0002(9) 0.0060(10) C102 0.0145(12) 0.0125(12) 0.0131(12) -0.0017(9) 0.0001(10) 0.0059(10) C103 0.0121(11) 0.0107(12) 0.0122(12) 0.0012(9) -0.0001(9) 0.0030(9) C104 0.0129(11) 0.0136(12) 0.0096(11) 0.0011(9) 0.0007(9) 0.0040(10) C105 0.0119(11) 0.0104(11) 0.0118(12) -0.0017(9) -0.0009(9) 0.0037(9) C106 0.0143(12) 0.0114(12) 0.0132(12) 0.0016(9) -0.0002(10) 0.0038(10) C111 0.0273(15) 0.0210(14) 0.0159(14) 0.0055(11) 0.0035(11) 0.0108(12) C112 0.0152(13) 0.0200(13) 0.0138(13) -0.0020(10) 0.0011(10) 0.0061(11) C131 0.0158(12) 0.0127(12) 0.0125(12) 0.0014(9) -0.0003(10) 0.0056(10) C151 0.0110(11) 0.0105(11) 0.0115(12) -0.0021(9) -0.0025(9) 0.0036(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 Yb1 O3 2.189(2) 2_556 ? Yb1 O1 2.321(2) . ? Yb1 O9 2.331(2) . ? Yb1 O8 2.341(2) 1_545 ? Yb1 O5 2.374(2) . ? Yb1 O2 2.383(2) . ? Yb1 O6 2.385(2) . ? Yb1 O7 2.426(2) 1_545 ? Yb1 C31 2.711(3) . ? Yb1 C131 2.732(3) . ? Yb1 C151 2.741(3) 1_545 ? Ag1 N12 2.174(2) . ? Ag1 N112 2.194(3) 2_765 ? Ag1 N13 2.429(3) 2_866 ? O1 C31 1.260(3) . ? O2 C31 1.265(3) . ? O3 C51 1.266(4) . ? O3 Yb1 2.189(2) 2_556 ? O4 C51 1.230(4) . ? O5 C131 1.268(3) . ? O6 C131 1.255(3) . ? O7 C151 1.261(3) . ? O7 Yb1 2.426(2) 1_565 ? O8 C151 1.263(3) . ? O8 Yb1 2.341(2) 1_565 ? O9 H11 0.808(15) . ? O9 H12 0.806(15) . ? O10 H13 0.843(19) . ? O10 H14 0.858(19) . ? N11 C11 1.360(3) . ? N11 C12 1.364(4) . ? N11 C1 1.437(3) . ? N12 C11 1.305(4) . ? N12 N13 1.382(3) . ? N13 C12 1.305(4) . ? N13 Ag1 2.429(3) 2_866 ? N111 C112 1.363(4) . ? N111 C111 1.368(4) . ? N111 C101 1.420(3) . ? N113 C111 1.293(4) . ? N113 N112 1.394(4) . ? N112 C112 1.292(4) . ? N112 Ag1 2.194(3) 2_765 ? C1 C2 1.385(4) . ? C1 C6 1.395(4) . ? C2 C3 1.394(4) . ? C2 H1 0.9500 . ? C3 C4 1.396(4) . ? C3 C31 1.501(4) . ? C4 C5 1.391(4) . ? C4 H2 0.9500 . ? C5 C6 1.398(4) . ? C5 C51 1.519(4) . ? C6 H3 0.9500 . ? C11 H4 0.9500 . ? C12 H5 0.9500 . ? C101 C102 1.385(4) . ? C101 C106 1.389(4) . ? C102 C103 1.392(4) . ? C102 H6 0.9500 . ? C103 C104 1.395(4) . ? C103 C131 1.498(4) . ? C104 C105 1.395(4) . ? C104 H7 0.9500 . ? C105 C106 1.387(4) . ? C105 C151 1.500(3) . ? C106 H8 0.9500 . ? C111 H9 0.9500 . ? C112 H10 0.9500 . ? C151 Yb1 2.741(3) 1_565 ? 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 Yb1 O1 73.80(8) 2_556 . ? O3 Yb1 O9 77.85(9) 2_556 . ? O1 Yb1 O9 151.65(8) . . ? O3 Yb1 O8 135.30(8) 2_556 1_545 ? O1 Yb1 O8 124.80(8) . 1_545 ? O9 Yb1 O8 76.70(8) . 1_545 ? O3 Yb1 O5 89.66(8) 2_556 . ? O1 Yb1 O5 87.57(8) . . ? O9 Yb1 O5 92.36(8) . . ? O8 Yb1 O5 127.36(7) 1_545 . ? O3 Yb1 O2 129.09(8) 2_556 . ? O1 Yb1 O2 55.36(7) . . ? O9 Yb1 O2 152.94(8) . . ? O8 Yb1 O2 82.88(7) 1_545 . ? O5 Yb1 O2 86.02(8) . . ? O3 Yb1 O6 134.79(8) 2_556 . ? O1 Yb1 O6 124.59(8) . . ? O9 Yb1 O6 76.76(9) . . ? O8 Yb1 O6 72.45(7) 1_545 . ? O5 Yb1 O6 54.96(7) . . ? O2 Yb1 O6 80.30(8) . . ? O3 Yb1 O7 90.52(8) 2_556 1_545 ? O1 Yb1 O7 87.96(8) . 1_545 ? O9 Yb1 O7 92.28(8) . 1_545 ? O8 Yb1 O7 54.74(7) 1_545 1_545 ? O5 Yb1 O7 175.29(7) . 1_545 ? O2 Yb1 O7 90.21(7) . 1_545 ? O6 Yb1 O7 127.13(7) . 1_545 ? O3 Yb1 C31 101.28(9) 2_556 . ? O1 Yb1 C31 27.63(8) . . ? O9 Yb1 C31 177.07(8) . . ? O8 Yb1 C31 105.67(8) 1_545 . ? O5 Yb1 C31 84.82(8) . . ? O2 Yb1 C31 27.81(8) . . ? O6 Yb1 C31 102.19(8) . . ? O7 Yb1 C31 90.52(7) 1_545 . ? O3 Yb1 C131 113.19(9) 2_556 . ? O1 Yb1 C131 107.49(9) . . ? O9 Yb1 C131 83.67(9) . . ? O8 Yb1 C131 99.77(8) 1_545 . ? O5 Yb1 C131 27.63(8) . . ? O2 Yb1 C131 82.49(8) . . ? O6 Yb1 C131 27.33(8) . . ? O7 Yb1 C131 154.30(7) 1_545 . ? C31 Yb1 C131 94.16(8) . . ? O3 Yb1 C151 114.11(9) 2_556 1_545 ? O1 Yb1 C151 107.30(8) . 1_545 ? O9 Yb1 C151 84.17(8) . 1_545 ? O8 Yb1 C151 27.36(7) 1_545 1_545 ? O5 Yb1 C151 154.45(8) . 1_545 ? O2 Yb1 C151 85.78(8) . 1_545 ? O6 Yb1 C151 99.77(8) . 1_545 ? O7 Yb1 C151 27.38(7) 1_545 1_545 ? C31 Yb1 C151 98.73(8) . 1_545 ? C131 Yb1 C151 127.04(8) . 1_545 ? N12 Ag1 N112 140.42(10) . 2_765 ? N12 Ag1 N13 121.90(9) . 2_866 ? N112 Ag1 N13 86.99(9) 2_765 2_866 ? C31 O1 Yb1 93.67(17) . . ? C31 O2 Yb1 90.68(16) . . ? C51 O3 Yb1 151.0(2) . 2_556 ? C131 O5 Yb1 92.09(16) . . ? C131 O6 Yb1 91.94(17) . . ? C151 O7 Yb1 90.36(15) . 1_565 ? C151 O8 Yb1 94.22(16) . 1_565 ? Yb1 O9 H11 116(3) . . ? Yb1 O9 H12 122(3) . . ? H11 O9 H12 111(4) . . ? H13 O10 H14 119(5) . . ? C11 N11 C12 104.6(2) . . ? C11 N11 C1 128.1(2) . . ? C12 N11 C1 127.2(2) . . ? C11 N12 N13 107.7(2) . . ? C11 N12 Ag1 138.6(2) . . ? N13 N12 Ag1 113.56(17) . . ? C12 N13 N12 106.8(2) . . ? C12 N13 Ag1 128.98(19) . 2_866 ? N12 N13 Ag1 124.08(17) . 2_866 ? C112 N111 C111 104.2(2) . . ? C112 N111 C101 129.4(2) . . ? C111 N111 C101 125.9(2) . . ? C111 N113 N112 105.7(2) . . ? C112 N112 N113 108.5(2) . . ? C112 N112 Ag1 139.4(2) . 2_765 ? N113 N112 Ag1 110.21(18) . 2_765 ? C2 C1 C6 121.1(2) . . ? C2 C1 N11 120.2(2) . . ? C6 C1 N11 118.6(2) . . ? C1 C2 C3 118.8(2) . . ? C1 C2 H1 120.6 . . ? C3 C2 H1 120.6 . . ? C2 C3 C4 120.9(2) . . ? C2 C3 C31 120.0(2) . . ? C4 C3 C31 119.0(2) . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H2 120.1 . . ? C3 C4 H2 120.1 . . ? C4 C5 C6 119.6(2) . . ? C4 C5 C51 121.9(2) . . ? C6 C5 C51 118.4(2) . . ? C1 C6 C5 119.7(2) . . ? C1 C6 H3 120.2 . . ? C5 C6 H3 120.2 . . ? N12 C11 N11 110.2(2) . . ? N12 C11 H4 124.9 . . ? N11 C11 H4 124.9 . . ? N13 C12 N11 110.7(2) . . ? N13 C12 H5 124.7 . . ? N11 C12 H5 124.7 . . ? O1 C31 O2 119.9(3) . . ? O1 C31 C3 118.7(2) . . ? O2 C31 C3 121.3(2) . . ? O1 C31 Yb1 58.70(14) . . ? O2 C31 Yb1 61.51(14) . . ? C3 C31 Yb1 173.92(18) . . ? O4 C51 O3 125.6(3) . . ? O4 C51 C5 118.5(2) . . ? O3 C51 C5 115.9(2) . . ? C102 C101 C106 120.6(3) . . ? C102 C101 N111 120.6(2) . . ? C106 C101 N111 118.6(2) . . ? C101 C102 C103 119.4(2) . . ? C101 C102 H6 120.3 . . ? C103 C102 H6 120.3 . . ? C102 C103 C104 120.5(2) . . ? C102 C103 C131 118.0(2) . . ? C104 C103 C131 121.2(2) . . ? C105 C104 C103 119.2(2) . . ? C105 C104 H7 120.4 . . ? C103 C104 H7 120.4 . . ? C106 C105 C104 120.3(2) . . ? C106 C105 C151 117.4(2) . . ? C104 C105 C151 122.3(2) . . ? C105 C106 C101 119.8(2) . . ? C105 C106 H8 120.1 . . ? C101 C106 H8 120.1 . . ? N113 C111 N111 111.6(3) . . ? N113 C111 H9 124.2 . . ? N111 C111 H9 124.2 . . ? N112 C112 N111 109.9(3) . . ? N112 C112 H10 125.0 . . ? N111 C112 H10 125.0 . . ? O6 C131 O5 121.0(2) . . ? O6 C131 C103 119.1(2) . . ? O5 C131 C103 119.8(2) . . ? O6 C131 Yb1 60.73(14) . . ? O5 C131 Yb1 60.28(14) . . ? C103 C131 Yb1 177.35(19) . . ? O7 C151 O8 120.7(2) . . ? O7 C151 C105 121.0(2) . . ? O8 C151 C105 118.3(2) . . ? O7 C151 Yb1 62.25(13) . 1_565 ? O8 C151 Yb1 58.42(13) . 1_565 ? C105 C151 Yb1 176.18(18) . 1_565 ? 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 Yb1 O1 C31 -173.82(19) 2_556 . . . ? O9 Yb1 O1 C31 -173.94(17) . . . . ? O8 Yb1 O1 C31 51.8(2) 1_545 . . . ? O5 Yb1 O1 C31 -83.47(18) . . . . ? O2 Yb1 O1 C31 3.37(16) . . . . ? O6 Yb1 O1 C31 -40.1(2) . . . . ? O7 Yb1 O1 C31 95.04(18) 1_545 . . . ? C131 Yb1 O1 C31 -64.04(18) . . . . ? C151 Yb1 O1 C31 75.38(18) 1_545 . . . ? O3 Yb1 O2 C31 0.1(2) 2_556 . . . ? O1 Yb1 O2 C31 -3.35(16) . . . . ? O9 Yb1 O2 C31 173.84(17) . . . . ? O8 Yb1 O2 C31 -145.11(17) 1_545 . . . ? O5 Yb1 O2 C31 86.45(16) . . . . ? O6 Yb1 O2 C31 141.56(17) . . . . ? O7 Yb1 O2 C31 -90.72(16) 1_545 . . . ? C131 Yb1 O2 C31 114.00(17) . . . . ? C151 Yb1 O2 C31 -117.76(17) 1_545 . . . ? O3 Yb1 O5 C131 -149.36(17) 2_556 . . . ? O1 Yb1 O5 C131 136.84(17) . . . . ? O9 Yb1 O5 C131 -71.54(17) . . . . ? O8 Yb1 O5 C131 3.5(2) 1_545 . . . ? O2 Yb1 O5 C131 81.41(17) . . . . ? O6 Yb1 O5 C131 0.47(15) . . . . ? C31 Yb1 O5 C131 109.28(17) . . . . ? C151 Yb1 O5 C131 9.9(3) 1_545 . . . ? O3 Yb1 O6 C131 44.6(2) 2_556 . . . ? O1 Yb1 O6 C131 -57.35(19) . . . . ? O9 Yb1 O6 C131 102.04(18) . . . . ? O8 Yb1 O6 C131 -177.95(18) 1_545 . . . ? O5 Yb1 O6 C131 -0.47(15) . . . . ? O2 Yb1 O6 C131 -92.41(17) . . . . ? O7 Yb1 O6 C131 -175.24(15) 1_545 . . . ? C31 Yb1 O6 C131 -75.15(17) . . . . ? C151 Yb1 O6 C131 -176.38(16) 1_545 . . . ? N112 Ag1 N12 C11 -46.5(4) 2_765 . . . ? N13 Ag1 N12 C11 -177.5(3) 2_866 . . . ? N112 Ag1 N12 N13 138.50(18) 2_765 . . . ? N13 Ag1 N12 N13 7.5(3) 2_866 . . . ? C11 N12 N13 C12 -0.1(3) . . . . ? Ag1 N12 N13 C12 176.45(19) . . . . ? C11 N12 N13 Ag1 175.80(19) . . . 2_866 ? Ag1 N12 N13 Ag1 -7.7(3) . . . 2_866 ? C111 N113 N112 C112 1.2(4) . . . . ? C111 N113 N112 Ag1 -166.5(2) . . . 2_765 ? C11 N11 C1 C2 13.8(4) . . . . ? C12 N11 C1 C2 -169.3(3) . . . . ? C11 N11 C1 C6 -166.9(3) . . . . ? C12 N11 C1 C6 10.0(4) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? N11 C1 C2 C3 179.3(2) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C1 C2 C3 C31 -179.2(2) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C31 C3 C4 C5 179.0(2) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C3 C4 C5 C51 -177.9(2) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? N11 C1 C6 C5 -177.7(2) . . . . ? C4 C5 C6 C1 -1.8(4) . . . . ? C51 C5 C6 C1 176.5(2) . . . . ? N13 N12 C11 N11 0.5(3) . . . . ? Ag1 N12 C11 N11 -174.6(2) . . . . ? C12 N11 C11 N12 -0.8(3) . . . . ? C1 N11 C11 N12 176.7(2) . . . . ? N12 N13 C12 N11 -0.4(3) . . . . ? Ag1 N13 C12 N11 -176.02(18) 2_866 . . . ? C11 N11 C12 N13 0.7(3) . . . . ? C1 N11 C12 N13 -176.7(2) . . . . ? Yb1 O1 C31 O2 -6.0(3) . . . . ? Yb1 O1 C31 C3 173.6(2) . . . . ? Yb1 O2 C31 O1 5.9(3) . . . . ? Yb1 O2 C31 C3 -173.8(2) . . . . ? C2 C3 C31 O1 -179.3(3) . . . . ? C4 C3 C31 O1 3.0(4) . . . . ? C2 C3 C31 O2 0.4(4) . . . . ? C4 C3 C31 O2 -177.3(2) . . . . ? O3 Yb1 C31 O1 6.05(19) 2_556 . . . ? O8 Yb1 C31 O1 -137.93(17) 1_545 . . . ? O5 Yb1 C31 O1 94.67(18) . . . . ? O2 Yb1 C31 O1 -174.1(3) . . . . ? O6 Yb1 C31 O1 147.13(17) . . . . ? O7 Yb1 C31 O1 -84.59(18) 1_545 . . . ? C131 Yb1 C31 O1 120.70(18) . . . . ? C151 Yb1 C31 O1 -110.82(18) 1_545 . . . ? O3 Yb1 C31 O2 -179.90(16) 2_556 . . . ? O1 Yb1 C31 O2 174.1(3) . . . . ? O8 Yb1 C31 O2 36.12(17) 1_545 . . . ? O5 Yb1 C31 O2 -91.28(16) . . . . ? O6 Yb1 C31 O2 -38.82(17) . . . . ? O7 Yb1 C31 O2 89.46(16) 1_545 . . . ? C131 Yb1 C31 O2 -65.24(17) . . . . ? C151 Yb1 C31 O2 63.23(17) 1_545 . . . ? Yb1 O3 C51 O4 29.8(6) 2_556 . . . ? Yb1 O3 C51 C5 -151.1(3) 2_556 . . . ? C4 C5 C51 O4 -172.3(3) . . . . ? C6 C5 C51 O4 9.5(4) . . . . ? C4 C5 C51 O3 8.5(4) . . . . ? C6 C5 C51 O3 -169.7(3) . . . . ? C112 N111 C101 C102 -18.7(4) . . . . ? C111 N111 C101 C102 152.0(3) . . . . ? C112 N111 C101 C106 165.7(3) . . . . ? C111 N111 C101 C106 -23.5(4) . . . . ? C106 C101 C102 C103 0.4(4) . . . . ? N111 C101 C102 C103 -175.0(2) . . . . ? C101 C102 C103 C104 1.1(4) . . . . ? C101 C102 C103 C131 176.3(2) . . . . ? C102 C103 C104 C105 -0.4(4) . . . . ? C131 C103 C104 C105 -175.4(2) . . . . ? C103 C104 C105 C106 -1.9(4) . . . . ? C103 C104 C105 C151 174.7(2) . . . . ? C104 C105 C106 C101 3.4(4) . . . . ? C151 C105 C106 C101 -173.4(2) . . . . ? C102 C101 C106 C105 -2.7(4) . . . . ? N111 C101 C106 C105 172.9(2) . . . . ? N112 N113 C111 N111 -0.4(4) . . . . ? C112 N111 C111 N113 -0.5(4) . . . . ? C101 N111 C111 N113 -173.1(3) . . . . ? N113 N112 C112 N111 -1.6(3) . . . . ? Ag1 N112 C112 N111 160.5(2) 2_765 . . . ? C111 N111 C112 N112 1.3(3) . . . . ? C101 N111 C112 N112 173.6(3) . . . . ? Yb1 O6 C131 O5 0.8(3) . . . . ? Yb1 O6 C131 C103 -177.0(2) . . . . ? Yb1 O5 C131 O6 -0.8(3) . . . . ? Yb1 O5 C131 C103 176.9(2) . . . . ? C102 C103 C131 O6 9.1(4) . . . . ? C104 C103 C131 O6 -175.8(3) . . . . ? C102 C103 C131 O5 -168.8(3) . . . . ? C104 C103 C131 O5 6.4(4) . . . . ? O3 Yb1 C131 O6 -147.16(16) 2_556 . . . ? O1 Yb1 C131 O6 133.39(17) . . . . ? O9 Yb1 C131 O6 -73.30(17) . . . . ? O8 Yb1 C131 O6 1.98(18) 1_545 . . . ? O5 Yb1 C131 O6 179.2(3) . . . . ? O2 Yb1 C131 O6 83.38(17) . . . . ? O7 Yb1 C131 O6 8.8(3) 1_545 . . . ? C31 Yb1 C131 O6 108.68(17) . . . . ? C151 Yb1 C131 O6 4.5(2) 1_545 . . . ? O3 Yb1 C131 O5 33.67(18) 2_556 . . . ? O1 Yb1 C131 O5 -45.77(18) . . . . ? O9 Yb1 C131 O5 107.53(17) . . . . ? O8 Yb1 C131 O5 -177.18(16) 1_545 . . . ? O2 Yb1 C131 O5 -95.78(17) . . . . ? O6 Yb1 C131 O5 -179.2(3) . . . . ? O7 Yb1 C131 O5 -170.40(15) 1_545 . . . ? C31 Yb1 C131 O5 -70.48(17) . . . . ? C151 Yb1 C131 O5 -174.69(15) 1_545 . . . ? Yb1 O7 C151 O8 -1.3(3) 1_565 . . . ? Yb1 O7 C151 C105 -177.6(2) 1_565 . . . ? Yb1 O8 C151 O7 1.3(3) 1_565 . . . ? Yb1 O8 C151 C105 177.77(19) 1_565 . . . ? C106 C105 C151 O7 169.9(2) . . . . ? C104 C105 C151 O7 -6.9(4) . . . . ? C106 C105 C151 O8 -6.6(4) . . . . ? C104 C105 C151 O8 176.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.962 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.175