# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sun, Yaguang' _publ_contact_author_email yaguangsun@yahoo.com.cn _publ_section_title ; Hydrothermal synthesis, crystal structure and properties of Ag(I)-4f compounds based on 1H-benzimidazole - 5, 6 - dicarboxylic acid ; loop_ _publ_author_name Y.Sun Y.Wu G.Xiong P.F.Smet F.Ding M.Guo M.Zhu E.Gao P.Dirk ; F.Verpoort ; data_5 _database_code_depnum_ccdc_archive 'CCDC 735026' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Ag Dy N4 O10.50' _chemical_formula_weight 722.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.326(5) _cell_length_b 8.4517(17) _cell_length_c 17.748(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3798.8(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3401 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.92 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 5.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4657 _exptl_absorpt_correction_T_max 0.6900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29664 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.92 _reflns_number_total 4546 _reflns_number_gt 3580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4546 _refine_ls_number_parameters 315 _refine_ls_number_restraints 385 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.523842(6) 0.334562(18) 0.217695(9) 0.00450(4) Uani 1 1 d U . . Ag1 Ag 0.772677(11) 0.53797(3) 0.449971(16) 0.01392(7) Uani 1 1 d D . . O1 O 0.52428(9) 0.1353(3) 0.12883(14) 0.0089(5) Uani 1 1 d U . . O2 O 0.47814(9) -0.0775(3) 0.16109(13) 0.0074(6) Uani 1 1 d . . . O3 O 0.55939(10) -0.2226(3) 0.24019(13) 0.0078(6) Uani 1 1 d . . . O4 O 0.58073(10) -0.4579(3) 0.19286(14) 0.0117(5) Uani 1 1 d U . . O5 O 0.61050(10) 0.2502(3) 0.21445(12) 0.0103(6) Uani 1 1 d . . . O6 O 0.66074(11) 0.0399(3) 0.23494(15) 0.0201(7) Uani 1 1 d . . . O7 O 0.53026(9) 0.0878(3) 0.28892(12) 0.0072(6) Uani 1 1 d . . . O8 O 0.52365(10) -0.0635(3) 0.38857(14) 0.0107(6) Uani 1 1 d . . . O9 O 0.75380(11) 0.5875(4) 0.30101(14) 0.0264(8) Uani 1 1 d D . . H9A H 0.7868 0.5804 0.2938 0.040 Uiso 1 1 d RD . . H9B H 0.7360 0.5668 0.2596 0.040 Uiso 1 1 d RD . . N1 N 0.60934(12) -0.1254(3) -0.11113(16) 0.0101(7) Uani 1 1 d . . . H1 H 0.5960 -0.0590 -0.1425 0.012 Uiso 1 1 calc R . . N2 N 0.65979(12) -0.3165(3) -0.06603(16) 0.0105(7) Uani 1 1 d . . . N3 N 0.70785(12) 0.4023(4) 0.48946(16) 0.0115(7) Uani 1 1 d . . . N4 N 0.64623(13) 0.3060(3) 0.56505(16) 0.0129(8) Uani 1 1 d . . . H4 H 0.6290 0.2871 0.6058 0.015 Uiso 1 1 calc R . . C1 C 0.51754(14) -0.0103(4) 0.12931(19) 0.0073(7) Uani 1 1 d U . . C2 C 0.55557(14) -0.1057(4) 0.08339(19) 0.0083(7) Uani 1 1 d U . . C3 C 0.56247(14) -0.0536(4) 0.00983(18) 0.0081(7) Uani 1 1 d U . . H3 H 0.5449 0.0356 -0.0079 0.010 Uiso 1 1 calc R . . C4 C 0.59636(15) -0.1388(4) -0.0363(2) 0.0098(8) Uani 1 1 d U . . C5 C 0.64632(14) -0.2334(4) -0.1268(2) 0.0105(8) Uani 1 1 d U . . H5 H 0.6609 -0.2486 -0.1744 0.013 Uiso 1 1 calc R . . C6 C 0.62720(14) -0.2621(4) -0.0085(2) 0.0086(7) Uani 1 1 d U . . C7 C 0.61967(15) -0.3171(4) 0.0640(2) 0.0101(8) Uani 1 1 d U . . H7 H 0.6389 -0.4027 0.0822 0.012 Uiso 1 1 calc R . . C8 C 0.58277(14) -0.2417(4) 0.10892(19) 0.0082(7) Uani 1 1 d U . . C9 C 0.57378(13) -0.3098(4) 0.1865(2) 0.0067(7) Uani 1 1 d U . . C10 C 0.63437(15) 0.1507(4) 0.2579(2) 0.0099(8) Uani 1 1 d U . . C11 C 0.63226(14) 0.1884(4) 0.3410(2) 0.0076(7) Uani 1 1 d U . . C12 C 0.67430(14) 0.2746(4) 0.37065(19) 0.0093(7) Uani 1 1 d U . . H12 H 0.7019 0.3083 0.3400 0.011 Uiso 1 1 calc R . . C13 C 0.67396(14) 0.3087(4) 0.4471(2) 0.0089(7) Uani 1 1 d U . . C14 C 0.68887(14) 0.3948(4) 0.5591(2) 0.0120(8) Uani 1 1 d U . . H14 H 0.7042 0.4470 0.5997 0.014 Uiso 1 1 calc R . . C15 C 0.63430(14) 0.2494(4) 0.4948(2) 0.0081(7) Uani 1 1 d U . . C16 C 0.59208(15) 0.1593(4) 0.4657(2) 0.0110(8) Uani 1 1 d U . . H16 H 0.5658 0.1195 0.4971 0.013 Uiso 1 1 calc R . . C17 C 0.59110(14) 0.1323(4) 0.3886(2) 0.0084(7) Uani 1 1 d U . . C18 C 0.54570(14) 0.0478(4) 0.3552(2) 0.0089(7) Uani 1 1 d U . . O11 O 0.7500 0.7500 0.6056(6) 0.188(5) Uani 1 2 d S . . H11A H 0.7255 0.8186 0.6061 0.226 Uiso 0.25 1 d PR . . H11B H 0.7688 0.7353 0.6447 0.226 Uiso 0.25 1 d PR . . O10 O 0.70425(18) 0.4532(6) 0.1851(2) 0.168(3) Uani 1 1 d D . . H10A H 0.6786 0.5105 0.1706 0.202 Uiso 0.50 1 d PRD . . H10B H 0.7051(8) 0.3579(10) 0.1700(17) 0.202 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.00884(9) 0.00056(8) 0.00409(9) -0.00003(6) 0.00048(6) 0.00073(6) Ag1 0.01353(14) 0.01403(14) 0.01419(15) -0.00041(12) 0.00000(11) -0.00630(12) O1 0.0110(7) 0.0072(7) 0.0087(8) -0.0003(6) -0.0002(6) 0.0005(6) O2 0.0123(12) 0.0057(11) 0.0043(12) -0.0004(10) 0.0002(9) 0.0014(10) O3 0.0113(12) 0.0079(11) 0.0043(12) -0.0017(11) -0.0001(9) -0.0011(10) O4 0.0126(7) 0.0090(7) 0.0135(8) 0.0015(6) 0.0014(6) -0.0002(6) O5 0.0144(13) 0.0095(12) 0.0071(12) 0.0016(10) -0.0017(10) 0.0026(11) O6 0.0292(16) 0.0195(14) 0.0115(13) -0.0024(12) -0.0008(12) 0.0142(13) O7 0.0121(12) 0.0044(12) 0.0050(12) 0.0003(10) -0.0004(9) -0.0016(10) O8 0.0198(14) 0.0053(12) 0.0069(12) 0.0019(11) -0.0001(10) -0.0063(11) O9 0.0193(15) 0.0332(17) 0.0268(16) -0.0042(14) -0.0002(13) 0.0081(15) N1 0.0126(15) 0.0112(14) 0.0065(15) -0.0007(13) 0.0002(12) -0.0003(13) N2 0.0110(15) 0.0092(15) 0.0112(16) -0.0014(13) 0.0005(12) 0.0006(12) N3 0.0148(15) 0.0099(14) 0.0097(16) -0.0026(13) 0.0012(12) -0.0033(13) N4 0.0200(17) 0.0148(16) 0.0039(15) -0.0009(13) 0.0034(12) -0.0064(14) C1 0.0108(14) 0.0039(14) 0.0073(15) 0.0008(13) -0.0037(12) 0.0013(13) C2 0.0126(15) 0.0055(13) 0.0069(15) -0.0022(13) 0.0023(13) -0.0036(13) C3 0.0137(15) 0.0029(13) 0.0076(15) -0.0020(13) 0.0021(13) 0.0029(12) C4 0.0120(15) 0.0078(14) 0.0096(16) -0.0021(13) -0.0018(13) -0.0002(13) C5 0.0111(15) 0.0112(15) 0.0092(16) -0.0040(14) 0.0018(13) 0.0005(14) C6 0.0082(14) 0.0061(14) 0.0116(15) -0.0028(13) 0.0008(12) -0.0005(13) C7 0.0148(16) 0.0044(14) 0.0110(15) 0.0013(13) -0.0040(13) 0.0019(13) C8 0.0121(15) 0.0040(14) 0.0084(15) 0.0000(13) 0.0008(12) -0.0037(13) C9 0.0030(14) 0.0069(14) 0.0103(15) 0.0000(14) -0.0011(12) -0.0011(12) C10 0.0112(15) 0.0105(15) 0.0078(15) 0.0023(14) 0.0000(13) -0.0031(13) C11 0.0099(14) 0.0052(13) 0.0078(14) -0.0008(13) -0.0014(12) 0.0017(12) C12 0.0099(14) 0.0075(14) 0.0106(15) 0.0020(13) 0.0018(12) 0.0008(13) C13 0.0095(15) 0.0079(14) 0.0092(15) 0.0023(13) -0.0025(12) -0.0010(13) C14 0.0126(16) 0.0118(16) 0.0115(17) -0.0045(15) -0.0014(14) -0.0026(15) C15 0.0129(15) 0.0043(13) 0.0071(14) 0.0001(12) 0.0003(12) -0.0002(13) C16 0.0152(16) 0.0082(15) 0.0097(16) 0.0020(13) 0.0021(13) -0.0024(13) C17 0.0122(15) 0.0045(14) 0.0084(15) 0.0006(13) -0.0023(12) 0.0023(13) C18 0.0132(15) 0.0055(14) 0.0079(15) -0.0035(13) -0.0014(13) 0.0015(13) O11 0.185(11) 0.184(9) 0.197(11) 0.000 0.000 0.060(10) O10 0.117(3) 0.349(7) 0.040(3) 0.013(4) -0.016(3) -0.180(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.277(2) 3_655 ? Dy1 O3 2.288(2) 3_655 ? Dy1 O1 2.307(2) . ? Dy1 O5 2.308(3) . ? Dy1 O4 2.312(2) 1_565 ? Dy1 O8 2.397(2) 3_655 ? Dy1 O7 2.445(2) . ? Dy1 O7 2.544(2) 3_655 ? Dy1 C18 2.833(3) 3_655 ? Ag1 N3 2.122(3) . ? Ag1 N2 2.126(3) 8_766 ? O1 C1 1.242(4) . ? O2 C1 1.279(4) . ? O2 Dy1 2.277(2) 3_645 ? O3 C9 1.258(4) . ? O3 Dy1 2.288(2) 3_645 ? O4 C9 1.269(4) . ? O4 Dy1 2.312(2) 1_545 ? O5 C10 1.291(4) . ? O6 C10 1.220(4) . ? O7 C18 1.285(4) . ? O7 Dy1 2.544(2) 3_645 ? O8 C18 1.244(4) . ? O8 Dy1 2.397(2) 3_645 ? O9 H9A 0.8481 . ? O9 H9B 0.8801 . ? N1 C5 1.337(5) . ? N1 C4 1.373(5) . ? N1 H1 0.8600 . ? N2 C5 1.331(4) . ? N2 C6 1.391(5) . ? N2 Ag1 2.126(3) 8_745 ? N3 C14 1.328(4) . ? N3 C13 1.388(5) . ? N4 C14 1.319(5) . ? N4 C15 1.369(5) . ? N4 H4 0.8600 . ? C1 C2 1.498(5) . ? C2 C3 1.389(5) . ? C2 C8 1.414(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9300 . ? C4 C6 1.392(5) . ? C5 H5 0.9300 . ? C6 C7 1.382(5) . ? C7 C8 1.384(5) . ? C7 H7 0.9300 . ? C8 C9 1.510(5) . ? C10 C11 1.510(5) . ? C11 C12 1.393(5) . ? C11 C17 1.424(5) . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 C15 1.406(5) . ? C14 H14 0.9300 . ? C15 C16 1.411(5) . ? C16 C17 1.387(5) . ? C16 H16 0.9300 . ? C17 C18 1.478(5) . ? C18 Dy1 2.833(3) 3_645 ? O11 H11A 0.8500 . ? O11 H11B 0.8500 . ? O10 H10A 0.8498 . ? O10 H10B 0.849(9) . ? 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 O2 Dy1 O3 74.93(8) 3_655 3_655 ? O2 Dy1 O1 152.18(8) 3_655 . ? O3 Dy1 O1 94.22(8) 3_655 . ? O2 Dy1 O5 98.36(8) 3_655 . ? O3 Dy1 O5 144.96(8) 3_655 . ? O1 Dy1 O5 75.69(8) . . ? O2 Dy1 O4 86.91(8) 3_655 1_565 ? O3 Dy1 O4 142.80(8) 3_655 1_565 ? O1 Dy1 O4 114.85(9) . 1_565 ? O5 Dy1 O4 68.72(9) . 1_565 ? O2 Dy1 O8 127.95(8) 3_655 3_655 ? O3 Dy1 O8 82.57(8) 3_655 3_655 ? O1 Dy1 O8 74.16(8) . 3_655 ? O5 Dy1 O8 124.64(8) . 3_655 ? O4 Dy1 O8 83.69(8) 1_565 3_655 ? O2 Dy1 O7 77.97(8) 3_655 . ? O3 Dy1 O7 73.27(8) 3_655 . ? O1 Dy1 O7 74.35(8) . . ? O5 Dy1 O7 71.70(8) . . ? O4 Dy1 O7 134.78(8) 1_565 . ? O8 Dy1 O7 138.33(8) 3_655 . ? O2 Dy1 O7 75.93(8) 3_655 3_655 ? O3 Dy1 O7 72.33(8) 3_655 3_655 ? O1 Dy1 O7 125.81(8) . 3_655 ? O5 Dy1 O7 140.44(8) . 3_655 ? O4 Dy1 O7 71.87(8) 1_565 3_655 ? O8 Dy1 O7 52.48(8) 3_655 3_655 ? O7 Dy1 O7 141.038(18) . 3_655 ? O2 Dy1 C18 102.13(9) 3_655 3_655 ? O3 Dy1 C18 73.20(9) 3_655 3_655 ? O1 Dy1 C18 98.93(9) . 3_655 ? O5 Dy1 C18 140.92(9) . 3_655 ? O4 Dy1 C18 79.50(9) 1_565 3_655 ? O8 Dy1 C18 25.83(9) 3_655 3_655 ? O7 Dy1 C18 145.14(9) . 3_655 ? O7 Dy1 C18 26.97(8) 3_655 3_655 ? N3 Ag1 N2 168.36(11) . 8_766 ? C1 O1 Dy1 135.9(2) . . ? C1 O2 Dy1 125.4(2) . 3_645 ? C9 O3 Dy1 129.6(2) . 3_645 ? C9 O4 Dy1 132.7(2) . 1_545 ? C10 O5 Dy1 129.2(2) . . ? C18 O7 Dy1 135.9(2) . . ? C18 O7 Dy1 89.2(2) . 3_645 ? Dy1 O7 Dy1 131.16(10) . 3_645 ? C18 O8 Dy1 97.1(2) . 3_645 ? H9A O9 H9B 111.4 . . ? C5 N1 C4 108.2(3) . . ? C5 N1 H1 125.9 . . ? C4 N1 H1 125.9 . . ? C5 N2 C6 105.5(3) . . ? C5 N2 Ag1 128.3(2) . 8_745 ? C6 N2 Ag1 124.8(2) . 8_745 ? C14 N3 C13 104.6(3) . . ? C14 N3 Ag1 127.9(2) . . ? C13 N3 Ag1 127.4(2) . . ? C14 N4 C15 107.8(3) . . ? C14 N4 H4 126.1 . . ? C15 N4 H4 126.1 . . ? O1 C1 O2 123.4(3) . . ? O1 C1 C2 116.2(3) . . ? O2 C1 C2 120.2(3) . . ? C3 C2 C8 119.8(3) . . ? C3 C2 C1 114.9(3) . . ? C8 C2 C1 125.2(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? N1 C4 C3 132.5(3) . . ? N1 C4 C6 105.6(3) . . ? C3 C4 C6 121.8(3) . . ? N2 C5 N1 111.8(3) . . ? N2 C5 H5 124.1 . . ? N1 C5 H5 124.1 . . ? C7 C6 N2 130.8(3) . . ? C7 C6 C4 120.2(3) . . ? N2 C6 C4 108.7(3) . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C2 121.2(3) . . ? C7 C8 C9 116.9(3) . . ? C2 C8 C9 121.9(3) . . ? O3 C9 O4 123.5(3) . . ? O3 C9 C8 120.7(3) . . ? O4 C9 C8 115.8(3) . . ? O6 C10 O5 123.9(3) . . ? O6 C10 C11 120.5(3) . . ? O5 C10 C11 115.4(3) . . ? C12 C11 C17 120.6(3) . . ? C12 C11 C10 116.9(3) . . ? C17 C11 C10 122.4(3) . . ? C13 C12 C11 118.3(3) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C12 C13 N3 130.1(3) . . ? C12 C13 C15 121.3(3) . . ? N3 C13 C15 108.6(3) . . ? N4 C14 N3 113.5(3) . . ? N4 C14 H14 123.3 . . ? N3 C14 H14 123.3 . . ? N4 C15 C13 105.4(3) . . ? N4 C15 C16 133.5(3) . . ? C13 C15 C16 120.9(3) . . ? C17 C16 C15 117.6(3) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C11 121.2(3) . . ? C16 C17 C18 119.3(3) . . ? C11 C17 C18 119.5(3) . . ? O8 C18 O7 119.9(3) . . ? O8 C18 C17 121.6(3) . . ? O7 C18 C17 118.5(3) . . ? O8 C18 Dy1 57.12(18) . 3_645 ? O7 C18 Dy1 63.87(18) . 3_645 ? C17 C18 Dy1 167.0(2) . 3_645 ? H11A O11 H11B 120.0 . . ? H10A O10 H10B 117.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Dy1 O1 C1 9.5(4) 3_655 . . . ? O3 Dy1 O1 C1 -55.8(3) 3_655 . . . ? O5 Dy1 O1 C1 90.2(3) . . . . ? O4 Dy1 O1 C1 148.1(3) 1_565 . . . ? O8 Dy1 O1 C1 -136.8(3) 3_655 . . . ? O7 Dy1 O1 C1 15.6(3) . . . . ? O7 Dy1 O1 C1 -127.0(3) 3_655 . . . ? C18 Dy1 O1 C1 -129.4(3) 3_655 . . . ? O2 Dy1 O5 C10 55.7(3) 3_655 . . . ? O3 Dy1 O5 C10 -20.0(3) 3_655 . . . ? O1 Dy1 O5 C10 -96.6(3) . . . . ? O4 Dy1 O5 C10 139.0(3) 1_565 . . . ? O8 Dy1 O5 C10 -155.3(3) 3_655 . . . ? O7 Dy1 O5 C10 -18.6(3) . . . . ? O7 Dy1 O5 C10 133.7(3) 3_655 . . . ? C18 Dy1 O5 C10 176.9(3) 3_655 . . . ? O2 Dy1 O7 C18 -23.8(3) 3_655 . . . ? O3 Dy1 O7 C18 -101.4(3) 3_655 . . . ? O1 Dy1 O7 C18 159.1(3) . . . . ? O5 Dy1 O7 C18 79.4(3) . . . . ? O4 Dy1 O7 C18 49.4(3) 1_565 . . . ? O8 Dy1 O7 C18 -158.7(3) 3_655 . . . ? O7 Dy1 O7 C18 -72.6(3) 3_655 . . . ? C18 Dy1 O7 C18 -117.8(3) 3_655 . . . ? O2 Dy1 O7 Dy1 127.05(14) 3_655 . . 3_645 ? O3 Dy1 O7 Dy1 49.38(12) 3_655 . . 3_645 ? O1 Dy1 O7 Dy1 -50.06(12) . . . 3_645 ? O5 Dy1 O7 Dy1 -129.82(14) . . . 3_645 ? O4 Dy1 O7 Dy1 -159.75(11) 1_565 . . 3_645 ? O8 Dy1 O7 Dy1 -7.9(2) 3_655 . . 3_645 ? O7 Dy1 O7 Dy1 78.26(16) 3_655 . . 3_645 ? C18 Dy1 O7 Dy1 33.0(2) 3_655 . . 3_645 ? N2 Ag1 N3 C14 8.3(8) 8_766 . . . ? N2 Ag1 N3 C13 -175.7(5) 8_766 . . . ? Dy1 O1 C1 O2 49.8(5) . . . . ? Dy1 O1 C1 C2 -136.3(3) . . . . ? Dy1 O2 C1 O1 -91.2(4) 3_645 . . . ? Dy1 O2 C1 C2 95.0(3) 3_645 . . . ? O1 C1 C2 C3 -49.9(4) . . . . ? O2 C1 C2 C3 124.3(4) . . . . ? O1 C1 C2 C8 131.5(4) . . . . ? O2 C1 C2 C8 -54.3(5) . . . . ? C8 C2 C3 C4 0.0(5) . . . . ? C1 C2 C3 C4 -178.7(3) . . . . ? C5 N1 C4 C3 176.9(4) . . . . ? C5 N1 C4 C6 -0.7(4) . . . . ? C2 C3 C4 N1 175.6(4) . . . . ? C2 C3 C4 C6 -7.0(5) . . . . ? C6 N2 C5 N1 2.9(4) . . . . ? Ag1 N2 C5 N1 -164.1(2) 8_745 . . . ? C4 N1 C5 N2 -1.4(4) . . . . ? C5 N2 C6 C7 171.9(4) . . . . ? Ag1 N2 C6 C7 -20.6(5) 8_745 . . . ? C5 N2 C6 C4 -3.3(4) . . . . ? Ag1 N2 C6 C4 164.3(2) 8_745 . . . ? N1 C4 C6 C7 -173.3(3) . . . . ? C3 C4 C6 C7 8.7(5) . . . . ? N1 C4 C6 N2 2.5(4) . . . . ? C3 C4 C6 N2 -175.5(3) . . . . ? N2 C6 C7 C8 -177.8(4) . . . . ? C4 C6 C7 C8 -3.1(5) . . . . ? C6 C7 C8 C2 -3.8(5) . . . . ? C6 C7 C8 C9 177.2(3) . . . . ? C3 C2 C8 C7 5.4(5) . . . . ? C1 C2 C8 C7 -176.0(3) . . . . ? C3 C2 C8 C9 -175.7(3) . . . . ? C1 C2 C8 C9 2.9(5) . . . . ? Dy1 O3 C9 O4 -86.0(4) 3_645 . . . ? Dy1 O3 C9 C8 92.7(3) 3_645 . . . ? Dy1 O4 C9 O3 65.5(5) 1_545 . . . ? Dy1 O4 C9 C8 -113.3(3) 1_545 . . . ? C7 C8 C9 O3 151.0(3) . . . . ? C2 C8 C9 O3 -28.0(5) . . . . ? C7 C8 C9 O4 -30.2(5) . . . . ? C2 C8 C9 O4 150.8(3) . . . . ? Dy1 O5 C10 O6 130.0(3) . . . . ? Dy1 O5 C10 C11 -55.8(4) . . . . ? O6 C10 C11 C12 80.9(4) . . . . ? O5 C10 C11 C12 -93.5(4) . . . . ? O6 C10 C11 C17 -95.6(4) . . . . ? O5 C10 C11 C17 89.9(4) . . . . ? C17 C11 C12 C13 -2.2(5) . . . . ? C10 C11 C12 C13 -178.9(3) . . . . ? C11 C12 C13 N3 -173.8(3) . . . . ? C11 C12 C13 C15 4.2(5) . . . . ? C14 N3 C13 C12 179.3(4) . . . . ? Ag1 N3 C13 C12 2.6(6) . . . . ? C14 N3 C13 C15 1.0(4) . . . . ? Ag1 N3 C13 C15 -175.7(2) . . . . ? C15 N4 C14 N3 -0.7(4) . . . . ? C13 N3 C14 N4 -0.2(4) . . . . ? Ag1 N3 C14 N4 176.5(2) . . . . ? C14 N4 C15 C13 1.3(4) . . . . ? C14 N4 C15 C16 -175.0(4) . . . . ? C12 C13 C15 N4 -179.9(3) . . . . ? N3 C13 C15 N4 -1.5(4) . . . . ? C12 C13 C15 C16 -3.1(5) . . . . ? N3 C13 C15 C16 175.4(3) . . . . ? N4 C15 C16 C17 175.5(4) . . . . ? C13 C15 C16 C17 -0.3(5) . . . . ? C15 C16 C17 C11 2.3(5) . . . . ? C15 C16 C17 C18 -175.9(3) . . . . ? C12 C11 C17 C16 -1.1(5) . . . . ? C10 C11 C17 C16 175.4(3) . . . . ? C12 C11 C17 C18 177.1(3) . . . . ? C10 C11 C17 C18 -6.5(5) . . . . ? Dy1 O8 C18 O7 12.7(3) 3_645 . . . ? Dy1 O8 C18 C17 -164.7(3) 3_645 . . . ? Dy1 O7 C18 O8 146.6(2) . . . . ? Dy1 O7 C18 O8 -11.8(3) 3_645 . . . ? Dy1 O7 C18 C17 -35.9(5) . . . . ? Dy1 O7 C18 C17 165.6(3) 3_645 . . . ? Dy1 O7 C18 Dy1 158.5(3) . . . 3_645 ? C16 C17 C18 O8 -37.1(5) . . . . ? C11 C17 C18 O8 144.8(3) . . . . ? C16 C17 C18 O7 145.5(3) . . . . ? C11 C17 C18 O7 -32.7(5) . . . . ? C16 C17 C18 Dy1 -117.2(11) . . . 3_645 ? C11 C17 C18 Dy1 64.6(12) . . . 3_645 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.733 _refine_diff_density_min -2.222 _refine_diff_density_rms 0.241 data_7 _database_code_depnum_ccdc_archive 'CCDC 735027' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Ag Er N4 O10' _chemical_formula_weight 718.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.285(5) _cell_length_b 8.4759(17) _cell_length_c 17.765(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3807.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3353 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.02 _exptl_crystal_description square _exptl_crystal_colour Pink _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 5.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7713 _exptl_absorpt_correction_T_max 0.8983 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23773 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3353 _reflns_number_gt 3140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+13.6853P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00102(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3353 _refine_ls_number_parameters 313 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.076 _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 O7 O 0.03070(14) 0.0874(5) 0.71188(19) 0.0170(8) Uani 1 1 d . . . O8 O 0.02555(15) -0.0666(5) 0.6126(2) 0.0246(9) Uani 1 1 d . . . C18 C 0.0467(2) 0.0464(6) 0.6461(3) 0.0184(11) Uani 1 1 d . . . C17 C 0.0923(2) 0.1337(6) 0.6120(3) 0.0154(11) Uani 1 1 d . . . C13 C 0.1337(2) 0.1912(7) 0.6592(3) 0.0187(11) Uani 1 1 d . . . C12 C 0.1745(2) 0.2773(7) 0.6287(3) 0.0216(12) Uani 1 1 d . . . H12 H 0.2018 0.3143 0.6591 0.026 Uiso 1 1 calc R . . O6 O 0.11016(15) 0.2514(5) 0.78571(19) 0.0223(9) Uani 1 1 d . . . O5 O 0.1643(2) 0.0543(7) 0.7661(3) 0.0551(16) Uani 1 1 d . . . C14 C 0.1361(2) 0.1586(6) 0.7430(3) 0.0211(12) Uani 1 1 d . . . O1 O 0.47632(14) 1.1353(5) 0.3709(2) 0.0190(8) Uani 1 1 d . . . O4 O 0.42090(16) 0.5403(5) 0.3091(2) 0.0293(10) Uani 1 1 d . . . Er1 Er 0.523252(9) 0.83331(3) 0.217628(12) 0.01310(12) Uani 1 1 d . . . Ag2 Ag 0.272328(17) 0.53857(6) 0.54787(3) 0.03073(16) Uani 1 1 d . . . C9 C 0.4824(2) 0.9896(7) 0.3706(3) 0.0150(11) Uani 1 1 d . . . O2 O 0.52120(13) 0.9202(5) 0.3385(2) 0.0177(8) Uani 1 1 d . . . C1 C 0.4267(2) 0.6886(6) 0.3144(3) 0.0174(11) Uani 1 1 d . . . N4 N 0.38982(18) 0.8750(6) 0.6104(2) 0.0216(10) Uani 1 1 d . . . H4A H 0.4034 0.9397 0.6423 0.026 Uiso 1 1 calc R . . C2 C 0.4164(2) 0.7588(6) 0.3895(3) 0.0164(11) Uani 1 1 d . . . O3 O 0.43990(14) 0.7746(5) 0.2595(2) 0.0194(8) Uani 1 1 d . . . C5 C 0.3518(2) 0.7690(7) 0.6251(3) 0.0225(12) Uani 1 1 d . . . H5 H 0.3363 0.7560 0.6721 0.027 Uiso 1 1 calc R . . C3 C 0.3792(2) 0.6849(6) 0.4351(3) 0.0207(12) Uani 1 1 d . . . H3 H 0.3594 0.6004 0.4171 0.025 Uiso 1 1 calc R . . C8 C 0.44400(19) 0.8954(6) 0.4162(3) 0.0157(10) Uani 1 1 d . . . C6 C 0.4033(2) 0.8623(7) 0.5358(3) 0.0178(11) Uani 1 1 d . . . C7 C 0.43708(19) 0.9459(6) 0.4903(3) 0.0177(11) Uani 1 1 d . . . H7 H 0.4549 1.0340 0.5084 0.021 Uiso 1 1 calc R . . N2 N 0.14738(18) 0.2989(6) 0.4341(3) 0.0243(11) Uani 1 1 d . . . H2A H 0.1305 0.2771 0.3934 0.029 Uiso 1 1 calc R . . N1 N 0.20833(18) 0.4002(6) 0.5090(3) 0.0256(11) Uani 1 1 d . . . C16 C 0.0932(2) 0.1559(6) 0.5346(3) 0.0182(12) Uani 1 1 d . . . H16 H 0.0673 0.1135 0.5034 0.022 Uiso 1 1 calc R . . C11 C 0.1744(2) 0.3083(7) 0.5517(3) 0.0190(11) Uani 1 1 d . . . C4 C 0.37218(19) 0.7402(7) 0.5081(3) 0.0182(11) Uani 1 1 d . . . C15 C 0.1349(2) 0.2452(7) 0.5059(3) 0.0171(11) Uani 1 1 d . . . N3 N 0.33873(19) 0.6854(6) 0.5652(3) 0.0223(11) Uani 1 1 d . . . C10 C 0.1902(2) 0.3900(8) 0.4394(3) 0.0261(13) Uani 1 1 d . . . H10 H 0.2056 0.4409 0.3986 0.031 Uiso 1 1 calc R . . O9 O 0.2021(6) 0.038(2) 0.3167(9) 0.238(7) Uani 1 1 d U . . H9A H 0.1737 0.0717 0.3367 0.286 Uiso 1 1 d R . . H9B H 0.2050 -0.0585 0.3046 0.286 Uiso 1 1 d R . . O10 O 0.2534(3) 0.9158(9) 0.2003(4) 0.0163(15) Uani 0.50 1 d PU . . O11 O 0.2500 0.7500 0.3979(19) 0.360(16) Uani 1 2 d SU . . H11A H 0.2397 0.7029 0.3583 0.432 Uiso 0.50 1 d PR . . H11B H 0.2547 0.8493 0.3975 0.432 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.0208(19) 0.013(2) 0.0172(19) 0.0000(15) 0.0021(14) -0.0037(15) O8 0.036(2) 0.021(2) 0.0172(19) -0.0040(17) 0.0031(16) -0.0117(17) C18 0.024(3) 0.016(3) 0.015(3) 0.003(2) -0.001(2) 0.001(2) C17 0.018(3) 0.012(3) 0.017(3) 0.000(2) 0.001(2) 0.002(2) C13 0.020(3) 0.019(3) 0.017(3) -0.001(2) 0.003(2) 0.004(2) C12 0.018(3) 0.024(3) 0.024(3) -0.001(2) -0.004(2) -0.001(2) O6 0.020(2) 0.026(2) 0.021(2) -0.0068(17) 0.0002(15) 0.0042(17) O5 0.074(4) 0.067(4) 0.024(2) 0.004(2) 0.000(2) 0.051(3) C14 0.022(3) 0.020(3) 0.021(3) 0.000(2) 0.000(2) 0.004(2) O1 0.033(2) 0.010(2) 0.0140(19) 0.0022(15) 0.0009(15) -0.0011(15) O4 0.030(2) 0.017(2) 0.041(2) -0.0083(19) 0.011(2) -0.0010(17) Er1 0.01657(17) 0.00986(17) 0.01285(17) -0.00003(8) 0.00083(9) 0.00188(8) Ag2 0.0227(3) 0.0341(3) 0.0354(3) 0.0013(2) 0.00031(19) -0.01323(19) C9 0.020(3) 0.016(3) 0.009(2) -0.001(2) -0.004(2) -0.004(2) O2 0.0161(18) 0.022(2) 0.0150(18) -0.0026(16) -0.0001(14) -0.0004(14) C1 0.014(3) 0.014(3) 0.024(3) -0.004(2) 0.001(2) -0.001(2) N4 0.025(2) 0.023(3) 0.016(2) -0.003(2) 0.0004(19) -0.003(2) C2 0.018(2) 0.011(3) 0.020(3) -0.003(2) -0.001(2) -0.001(2) O3 0.0183(19) 0.023(2) 0.0167(18) 0.0013(17) -0.0005(15) -0.0005(16) C5 0.021(3) 0.032(3) 0.015(3) 0.004(2) 0.005(2) -0.005(2) C3 0.025(3) 0.015(3) 0.022(3) -0.004(2) 0.001(2) -0.004(2) C8 0.016(2) 0.012(3) 0.019(3) 0.001(2) -0.001(2) 0.000(2) C6 0.021(3) 0.018(3) 0.015(3) 0.000(2) 0.002(2) 0.000(2) C7 0.015(3) 0.016(3) 0.022(3) -0.002(2) -0.002(2) -0.001(2) N2 0.023(3) 0.032(3) 0.017(2) 0.004(2) -0.0020(19) -0.010(2) N1 0.023(2) 0.029(3) 0.025(3) 0.006(2) 0.002(2) -0.007(2) C16 0.019(3) 0.017(3) 0.019(3) -0.002(2) -0.003(2) -0.003(2) C11 0.013(3) 0.021(3) 0.022(3) 0.000(2) 0.003(2) -0.002(2) C4 0.017(3) 0.015(3) 0.022(3) 0.003(2) 0.004(2) -0.001(2) C15 0.022(3) 0.018(3) 0.011(2) 0.000(2) -0.001(2) -0.001(2) N3 0.020(2) 0.025(3) 0.021(2) 0.001(2) 0.004(2) -0.0044(19) C10 0.027(3) 0.033(4) 0.018(3) 0.007(3) 0.001(2) -0.015(3) O9 0.238(7) 0.238(7) 0.238(7) 0.0003(10) 0.0000(10) 0.0004(10) O10 0.0157(17) 0.0161(17) 0.0172(17) -0.0012(10) -0.0010(10) -0.0008(10) O11 0.360(16) 0.360(16) 0.360(16) 0.000 0.000 0.0001(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 O7 C18 1.284(6) . ? O7 Er1 2.439(4) 6_556 ? O7 Er1 2.552(4) 8_646 ? O8 C18 1.247(7) . ? O8 Er1 2.392(4) 8_646 ? C18 C17 1.500(7) . ? C18 Er1 2.828(5) 8_646 ? C17 C16 1.387(7) . ? C17 C13 1.427(8) . ? C13 C12 1.377(8) . ? C13 C14 1.515(8) . ? C12 C11 1.393(8) . ? C12 H12 0.9300 . ? O6 C14 1.275(7) . ? O6 Er1 2.305(4) 6_556 ? O5 C14 1.208(7) . ? O1 C9 1.244(7) . ? O1 Er1 2.300(4) 3_655 ? O4 C1 1.268(6) . ? O4 Er1 2.302(4) 3_645 ? Er1 O2 2.270(4) . ? Er1 O3 2.290(4) . ? Er1 O1 2.300(4) 3_645 ? Er1 O4 2.302(4) 3_655 ? Er1 O6 2.305(4) 6_666 ? Er1 O8 2.392(4) 8_665 ? Er1 O7 2.439(4) 6_666 ? Er1 O7 2.552(4) 8_665 ? Er1 C18 2.828(5) 8_665 ? Ag2 N3 2.113(5) . ? Ag2 N1 2.115(5) . ? C9 O2 1.278(6) . ? C9 C8 1.496(7) . ? C1 O3 1.263(7) . ? C1 C2 1.484(7) . ? N4 C5 1.342(7) . ? N4 C6 1.372(7) . ? N4 H4A 0.8600 . ? C2 C3 1.390(8) . ? C2 C8 1.433(7) . ? C5 N3 1.319(7) . ? C5 H5 0.9300 . ? C3 C4 1.390(8) . ? C3 H3 0.9300 . ? C8 C7 1.394(7) . ? C6 C7 1.374(7) . ? C6 C4 1.390(8) . ? C7 H7 0.9300 . ? N2 C10 1.332(7) . ? N2 C15 1.390(7) . ? N2 H2A 0.8600 . ? N1 C10 1.321(7) . ? N1 C11 1.385(7) . ? C16 C15 1.396(7) . ? C16 H16 0.9300 . ? C11 C15 1.396(7) . ? C4 N3 1.400(7) . ? C10 H10 0.9300 . ? O9 H9A 0.8501 . ? O9 H9B 0.8500 . ? O11 H11A 0.8500 . ? O11 H11B 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 C18 O7 Er1 136.3(3) . 6_556 ? C18 O7 Er1 88.6(3) . 8_646 ? Er1 O7 Er1 131.26(14) 6_556 8_646 ? C18 O8 Er1 97.0(3) . 8_646 ? O8 C18 O7 120.5(5) . . ? O8 C18 C17 121.0(5) . . ? O7 C18 C17 118.4(5) . . ? O8 C18 Er1 57.1(3) . 8_646 ? O7 C18 Er1 64.4(3) . 8_646 ? C17 C18 Er1 168.0(4) . 8_646 ? C16 C17 C13 121.7(5) . . ? C16 C17 C18 118.7(5) . . ? C13 C17 C18 119.6(5) . . ? C12 C13 C17 120.0(5) . . ? C12 C13 C14 116.9(5) . . ? C17 C13 C14 123.1(5) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 O6 Er1 131.4(3) . 6_556 ? O5 C14 O6 123.5(6) . . ? O5 C14 C13 119.5(5) . . ? O6 C14 C13 116.8(5) . . ? C9 O1 Er1 136.1(3) . 3_655 ? C1 O4 Er1 134.4(4) . 3_645 ? O2 Er1 O3 75.06(12) . . ? O2 Er1 O1 152.05(14) . 3_645 ? O3 Er1 O1 93.89(13) . 3_645 ? O2 Er1 O4 87.82(15) . 3_655 ? O3 Er1 O4 142.88(14) . 3_655 ? O1 Er1 O4 114.35(14) 3_645 3_655 ? O2 Er1 O6 98.27(12) . 6_666 ? O3 Er1 O6 145.12(14) . 6_666 ? O1 Er1 O6 76.00(13) 3_645 6_666 ? O4 Er1 O6 68.87(14) 3_655 6_666 ? O2 Er1 O8 127.62(13) . 8_665 ? O3 Er1 O8 81.70(13) . 8_665 ? O1 Er1 O8 74.24(13) 3_645 8_665 ? O4 Er1 O8 83.40(15) 3_655 8_665 ? O6 Er1 O8 125.34(12) 6_666 8_665 ? O2 Er1 O7 78.08(13) . 6_666 ? O3 Er1 O7 73.66(13) . 6_666 ? O1 Er1 O7 74.15(13) 3_645 6_666 ? O4 Er1 O7 135.24(14) 3_655 6_666 ? O6 Er1 O7 71.47(13) 6_666 6_666 ? O8 Er1 O7 138.03(13) 8_665 6_666 ? O2 Er1 O7 75.62(12) . 8_665 ? O3 Er1 O7 72.80(13) . 8_665 ? O1 Er1 O7 126.25(12) 3_645 8_665 ? O4 Er1 O7 71.11(13) 3_655 8_665 ? O6 Er1 O7 139.72(14) 6_666 8_665 ? O8 Er1 O7 52.67(12) 8_665 8_665 ? O7 Er1 O7 141.56(3) 6_666 8_665 ? O2 Er1 C18 101.73(14) . 8_665 ? O3 Er1 C18 73.10(14) . 8_665 ? O1 Er1 C18 99.32(14) 3_645 8_665 ? O4 Er1 C18 78.69(15) 3_655 8_665 ? O6 Er1 C18 140.94(14) 6_666 8_665 ? O8 Er1 C18 25.95(14) 8_665 8_665 ? O7 Er1 C18 145.55(14) 6_666 8_665 ? O7 Er1 C18 26.99(13) 8_665 8_665 ? N3 Ag2 N1 169.30(18) . . ? O1 C9 O2 123.6(5) . . ? O1 C9 C8 116.6(5) . . ? O2 C9 C8 119.6(5) . . ? C9 O2 Er1 126.1(3) . . ? O3 C1 O4 123.0(5) . . ? O3 C1 C2 120.6(5) . . ? O4 C1 C2 116.4(5) . . ? C5 N4 C6 108.2(5) . . ? C5 N4 H4A 125.9 . . ? C6 N4 H4A 125.9 . . ? C3 C2 C8 120.1(5) . . ? C3 C2 C1 117.5(5) . . ? C8 C2 C1 122.4(5) . . ? C1 O3 Er1 128.3(3) . . ? N3 C5 N4 112.5(5) . . ? N3 C5 H5 123.7 . . ? N4 C5 H5 123.7 . . ? C2 C3 C4 118.5(5) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C7 C8 C2 119.9(5) . . ? C7 C8 C9 115.4(5) . . ? C2 C8 C9 124.6(4) . . ? N4 C6 C7 133.0(5) . . ? N4 C6 C4 105.1(5) . . ? C7 C6 C4 121.8(5) . . ? C6 C7 C8 118.4(5) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C10 N2 C15 108.0(5) . . ? C10 N2 H2A 126.0 . . ? C15 N2 H2A 126.0 . . ? C10 N1 C11 105.1(5) . . ? C10 N1 Ag2 127.5(4) . . ? C11 N1 Ag2 127.3(4) . . ? C17 C16 C15 116.6(5) . . ? C17 C16 H16 121.7 . . ? C15 C16 H16 121.7 . . ? N1 C11 C12 130.1(5) . . ? N1 C11 C15 109.8(5) . . ? C12 C11 C15 120.2(5) . . ? C6 C4 C3 120.6(5) . . ? C6 C4 N3 109.4(5) . . ? C3 C4 N3 129.9(5) . . ? N2 C15 C16 133.2(5) . . ? N2 C15 C11 104.4(5) . . ? C16 C15 C11 122.4(5) . . ? C5 N3 C4 104.8(5) . . ? C5 N3 Ag2 129.3(4) . . ? C4 N3 Ag2 124.7(4) . . ? N1 C10 N2 112.8(5) . . ? N1 C10 H10 123.6 . . ? N2 C10 H10 123.6 . . ? H9A O9 H9B 120.0 . . ? H11A O11 H11B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Er1 O8 C18 O7 -11.9(5) 8_646 . . . ? Er1 O8 C18 C17 166.0(4) 8_646 . . . ? Er1 O7 C18 O8 -147.3(4) 6_556 . . . ? Er1 O7 C18 O8 11.1(5) 8_646 . . . ? Er1 O7 C18 C17 34.8(7) 6_556 . . . ? Er1 O7 C18 C17 -166.9(4) 8_646 . . . ? Er1 O7 C18 Er1 -158.4(4) 6_556 . . 8_646 ? O8 C18 C17 C16 35.9(8) . . . . ? O7 C18 C17 C16 -146.2(5) . . . . ? Er1 C18 C17 C16 113.2(17) 8_646 . . . ? O8 C18 C17 C13 -143.9(5) . . . . ? O7 C18 C17 C13 34.0(7) . . . . ? Er1 C18 C17 C13 -66.6(19) 8_646 . . . ? C16 C17 C13 C12 3.0(8) . . . . ? C18 C17 C13 C12 -177.2(5) . . . . ? C16 C17 C13 C14 -175.3(5) . . . . ? C18 C17 C13 C14 4.5(8) . . . . ? C17 C13 C12 C11 0.7(8) . . . . ? C14 C13 C12 C11 179.1(5) . . . . ? Er1 O6 C14 O5 -133.0(6) 6_556 . . . ? Er1 O6 C14 C13 51.4(7) 6_556 . . . ? C12 C13 C14 O5 -79.4(8) . . . . ? C17 C13 C14 O5 99.0(7) . . . . ? C12 C13 C14 O6 96.5(6) . . . . ? C17 C13 C14 O6 -85.2(7) . . . . ? Er1 O1 C9 O2 49.9(7) 3_655 . . . ? Er1 O1 C9 C8 -135.3(4) 3_655 . . . ? O1 C9 O2 Er1 -90.2(6) . . . . ? C8 C9 O2 Er1 95.1(5) . . . . ? O3 Er1 O2 C9 -39.8(4) . . . . ? O1 Er1 O2 C9 -109.2(5) 3_645 . . . ? O4 Er1 O2 C9 106.9(4) 3_655 . . . ? O6 Er1 O2 C9 175.2(4) 6_666 . . . ? O8 Er1 O2 C9 27.0(5) 8_665 . . . ? O7 Er1 O2 C9 -115.9(4) 6_666 . . . ? O7 Er1 O2 C9 35.8(4) 8_665 . . . ? C18 Er1 O2 C9 28.9(4) 8_665 . . . ? Er1 O4 C1 O3 63.9(8) 3_645 . . . ? Er1 O4 C1 C2 -116.8(5) 3_645 . . . ? O3 C1 C2 C3 149.0(5) . . . . ? O4 C1 C2 C3 -30.4(7) . . . . ? O3 C1 C2 C8 -32.4(8) . . . . ? O4 C1 C2 C8 148.2(5) . . . . ? O4 C1 O3 Er1 -86.4(6) . . . . ? C2 C1 O3 Er1 94.3(5) . . . . ? O2 Er1 O3 C1 -59.1(4) . . . . ? O1 Er1 O3 C1 94.8(4) 3_645 . . . ? O4 Er1 O3 C1 -124.4(4) 3_655 . . . ? O6 Er1 O3 C1 23.9(6) 6_666 . . . ? O8 Er1 O3 C1 168.2(5) 8_665 . . . ? O7 Er1 O3 C1 22.6(4) 6_666 . . . ? O7 Er1 O3 C1 -138.4(5) 8_665 . . . ? C18 Er1 O3 C1 -166.6(5) 8_665 . . . ? C6 N4 C5 N3 0.1(7) . . . . ? C8 C2 C3 C4 -4.1(8) . . . . ? C1 C2 C3 C4 174.5(5) . . . . ? C3 C2 C8 C7 5.7(8) . . . . ? C1 C2 C8 C7 -172.8(5) . . . . ? C3 C2 C8 C9 -176.3(5) . . . . ? C1 C2 C8 C9 5.2(8) . . . . ? O1 C9 C8 C7 -50.4(6) . . . . ? O2 C9 C8 C7 124.7(5) . . . . ? O1 C9 C8 C2 131.6(5) . . . . ? O2 C9 C8 C2 -53.4(7) . . . . ? C5 N4 C6 C7 175.7(6) . . . . ? C5 N4 C6 C4 -1.7(6) . . . . ? N4 C6 C7 C8 176.3(6) . . . . ? C4 C6 C7 C8 -6.6(8) . . . . ? C2 C8 C7 C6 -0.3(8) . . . . ? C9 C8 C7 C6 -178.5(5) . . . . ? N3 Ag2 N1 C10 -7.6(14) . . . . ? N3 Ag2 N1 C11 176.7(9) . . . . ? C13 C17 C16 C15 -3.6(8) . . . . ? C18 C17 C16 C15 176.6(5) . . . . ? C10 N1 C11 C12 -179.5(6) . . . . ? Ag2 N1 C11 C12 -3.1(9) . . . . ? C10 N1 C11 C15 -1.0(7) . . . . ? Ag2 N1 C11 C15 175.4(4) . . . . ? C13 C12 C11 N1 174.8(6) . . . . ? C13 C12 C11 C15 -3.5(9) . . . . ? N4 C6 C4 C3 -173.9(5) . . . . ? C7 C6 C4 C3 8.3(8) . . . . ? N4 C6 C4 N3 2.6(6) . . . . ? C7 C6 C4 N3 -175.2(5) . . . . ? C2 C3 C4 C6 -2.7(8) . . . . ? C2 C3 C4 N3 -178.4(5) . . . . ? C10 N2 C15 C16 175.3(6) . . . . ? C10 N2 C15 C11 -1.7(7) . . . . ? C17 C16 C15 N2 -175.9(6) . . . . ? C17 C16 C15 C11 0.7(8) . . . . ? N1 C11 C15 N2 1.7(6) . . . . ? C12 C11 C15 N2 -179.6(5) . . . . ? N1 C11 C15 C16 -175.7(5) . . . . ? C12 C11 C15 C16 2.9(9) . . . . ? N4 C5 N3 C4 1.5(7) . . . . ? N4 C5 N3 Ag2 -165.9(4) . . . . ? C6 C4 N3 C5 -2.6(6) . . . . ? C3 C4 N3 C5 173.6(6) . . . . ? C6 C4 N3 Ag2 165.6(4) . . . . ? C3 C4 N3 Ag2 -18.3(8) . . . . ? N1 Ag2 N3 C5 155.4(9) . . . . ? N1 Ag2 N3 C4 -9.7(13) . . . . ? C11 N1 C10 N2 -0.1(7) . . . . ? Ag2 N1 C10 N2 -176.5(4) . . . . ? C15 N2 C10 N1 1.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.444 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.154 data_3 _database_code_depnum_ccdc_archive 'CCDC 735028' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Ag Gd N4 O10.50' _chemical_formula_weight 718.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.287(5) _cell_length_b 8.5525(17) _cell_length_c 17.827(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3855.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.02 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 4.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3453 _exptl_absorpt_correction_T_max 0.4663 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23975 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3401 _reflns_number_gt 3178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+27.8445P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00134(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3401 _refine_ls_number_parameters 313 _refine_ls_number_restraints 894 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.110 _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 O3 O 1.02063(14) 0.9226(5) 0.6598(2) 0.0178(8) Uani 1 1 d U . . O6 O 0.53151(15) 0.0886(5) 0.2892(2) 0.0176(8) Uani 1 1 d U . . O5 O 0.52660(17) -0.0618(5) 0.3886(2) 0.0256(9) Uani 1 1 d U . . C14 C 0.5479(2) 0.0493(7) 0.3548(3) 0.0184(10) Uani 1 1 d U . . C13 C 0.5936(2) 0.1350(7) 0.3884(3) 0.0183(10) Uani 1 1 d U . . C2 C 0.9434(2) 0.8947(7) 0.5822(3) 0.0173(10) Uani 1 1 d U . . O4 O 0.97524(16) 1.1347(5) 0.6275(2) 0.0208(9) Uani 1 1 d U . . C1 C 0.9819(2) 0.9902(7) 0.6281(3) 0.0165(11) Uani 1 1 d U . . O2 O 0.93882(15) 0.7777(5) 0.7390(2) 0.0199(8) Uani 1 1 d U . . C9 C 0.9254(2) 0.6915(7) 0.6851(4) 0.0207(11) Uani 1 1 d U . . C8 C 0.9160(2) 0.7600(7) 0.6094(3) 0.0185(10) Uani 1 1 d U . . C7 C 0.8791(2) 0.6854(7) 0.5634(4) 0.0233(11) Uani 1 1 d U . . H7 H 0.8596 0.6009 0.5811 0.028 Uiso 1 1 calc R . . Gd1 Gd 0.523617(10) 0.33565(3) 0.216921(15) 0.01309(13) Uani 1 1 d U . . Ag2 Ag 0.773099(19) 0.53877(6) 0.45135(3) 0.03137(18) Uani 1 1 d U . . O7 O 0.61211(16) 0.2533(5) 0.2146(2) 0.0216(9) Uani 1 1 d U . . C16 C 0.6757(2) 0.2798(8) 0.3708(4) 0.0234(10) Uani 1 1 d U . . H16 H 0.7029 0.3166 0.3404 0.028 Uiso 1 1 calc R . . N2 N 0.88972(19) 0.8737(6) 0.3884(3) 0.0220(10) Uani 1 1 d U . . H2A H 0.9034 0.9378 0.3567 0.026 Uiso 1 1 calc R . . C15 C 0.6753(2) 0.3104(7) 0.4474(3) 0.0201(11) Uani 1 1 d U . . N1 N 0.8392(2) 0.6861(6) 0.4336(3) 0.0247(10) Uani 1 1 d U . . C18 C 0.6374(2) 0.1603(7) 0.2583(4) 0.0222(11) Uani 1 1 d U . . C5 C 0.8523(2) 0.7681(8) 0.3739(4) 0.0252(12) Uani 1 1 d U . . H5 H 0.8371 0.7540 0.3269 0.030 Uiso 1 1 calc R . . C12 C 0.5946(2) 0.1592(7) 0.4649(3) 0.0196(11) Uani 1 1 d U . . H12 H 0.5686 0.1176 0.4960 0.023 Uiso 1 1 calc R . . C3 C 0.9367(2) 0.9457(7) 0.5095(3) 0.0185(10) Uani 1 1 d U . . H3 H 0.9545 1.0335 0.4919 0.022 Uiso 1 1 calc R . . O8 O 0.6652(2) 0.0533(6) 0.2351(3) 0.0452(12) Uani 1 1 d U . . C17 C 0.6348(2) 0.1936(7) 0.3412(3) 0.0200(10) Uani 1 1 d U . . N3 N 0.7089(2) 0.4018(6) 0.4908(3) 0.0252(10) Uani 1 1 d U . . C6 C 0.8721(2) 0.7391(7) 0.4909(4) 0.0196(10) Uani 1 1 d U . . C4 C 0.9025(2) 0.8615(7) 0.4632(3) 0.0189(11) Uani 1 1 d U . . O9 O 0.7543(3) 0.5883(9) 0.2975(4) 0.0697(16) Uani 1 1 d U . . H9A H 0.7310 0.6289 0.2692 0.084 Uiso 1 1 d R . . H9B H 0.7459 0.5555 0.3409 0.084 Uiso 1 1 d R . . C11 C 0.6362(2) 0.2486(7) 0.4943(3) 0.0184(10) Uani 1 1 d U . . C10 C 0.6909(3) 0.3918(8) 0.5597(4) 0.0287(12) Uani 1 1 d U . . H10 H 0.7063 0.4426 0.6003 0.034 Uiso 1 1 calc R . . O11 O 0.7971(3) 0.4622(10) 0.6789(5) 0.095(2) Uani 1 1 d U . . H11A H 0.7710 0.4402 0.7071 0.114 Uiso 1 1 d R . . H11B H 0.8280 0.4684 0.6973 0.114 Uiso 1 1 d R . . O1 O 0.91902(17) 0.5459(5) 0.6915(3) 0.0284(10) Uani 1 1 d U . . N4 N 0.6483(2) 0.3011(6) 0.5651(3) 0.0242(10) Uani 1 1 d U . . H4A H 0.6314 0.2793 0.6056 0.029 Uiso 1 1 calc R . . O10 O 0.2500 0.2500 0.381(3) 0.42(3) Uani 1 2 d S . . H10A H 0.2339 0.2748 0.3408 0.505 Uiso 0.50 1 d PR . . H10B H 0.2332 0.2071 0.4167 0.505 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0175(17) 0.0194(19) 0.0163(19) 0.0023(16) -0.0010(15) -0.0019(15) O6 0.0211(17) 0.0155(18) 0.0164(18) 0.0010(15) -0.0034(14) -0.0008(15) O5 0.036(2) 0.023(2) 0.017(2) 0.0054(17) -0.0055(17) -0.0100(18) C14 0.022(2) 0.017(2) 0.017(2) -0.0015(19) -0.0004(19) 0.0022(19) C13 0.021(2) 0.016(2) 0.018(2) 0.0006(19) -0.0017(19) 0.0022(19) C2 0.018(2) 0.015(2) 0.019(2) 0.0002(19) -0.0012(19) -0.0011(18) O4 0.031(2) 0.0129(19) 0.019(2) -0.0023(16) 0.0002(16) -0.0021(16) C1 0.021(2) 0.013(2) 0.016(2) 0.001(2) 0.0014(19) -0.0038(19) O2 0.0200(18) 0.0202(19) 0.0195(19) -0.0003(16) 0.0001(15) -0.0010(16) C9 0.018(2) 0.017(2) 0.027(3) 0.003(2) 0.000(2) 0.000(2) C8 0.018(2) 0.016(2) 0.022(2) -0.0003(19) -0.0013(19) -0.0015(19) C7 0.023(2) 0.020(2) 0.028(2) 0.002(2) -0.001(2) -0.0039(19) Gd1 0.01652(18) 0.00922(18) 0.01352(19) -0.00014(10) 0.00058(10) 0.00188(10) Ag2 0.0227(3) 0.0349(3) 0.0364(3) -0.0017(2) -0.0001(2) -0.0140(2) O7 0.0214(18) 0.025(2) 0.0183(19) 0.0047(16) -0.0003(15) 0.0049(16) C16 0.023(2) 0.026(2) 0.021(2) -0.001(2) 0.0000(19) -0.0003(19) N2 0.023(2) 0.022(2) 0.021(2) 0.0020(19) -0.0015(19) -0.0048(19) C15 0.019(2) 0.023(2) 0.019(2) -0.002(2) -0.001(2) -0.004(2) N1 0.023(2) 0.027(2) 0.024(2) -0.0026(19) -0.0012(19) -0.0053(19) C18 0.025(2) 0.021(2) 0.020(2) -0.001(2) 0.000(2) 0.005(2) C5 0.024(2) 0.028(3) 0.024(3) -0.002(2) -0.003(2) -0.006(2) C12 0.020(2) 0.020(2) 0.019(2) 0.0007(19) 0.0000(19) -0.0031(19) C3 0.020(2) 0.016(2) 0.020(2) 0.0014(19) -0.0004(19) -0.0025(19) O8 0.055(3) 0.047(3) 0.033(2) -0.003(2) 0.001(2) 0.027(2) C17 0.021(2) 0.021(2) 0.018(2) 0.0014(19) -0.0010(19) 0.0032(19) N3 0.022(2) 0.029(2) 0.024(2) -0.004(2) -0.0011(19) -0.007(2) C6 0.015(2) 0.020(2) 0.023(2) -0.002(2) -0.0016(19) -0.0045(19) C4 0.019(2) 0.017(2) 0.020(2) 0.000(2) -0.001(2) -0.0011(19) O9 0.061(3) 0.077(4) 0.071(4) -0.011(3) 0.002(3) 0.003(3) C11 0.019(2) 0.021(2) 0.015(2) 0.000(2) 0.0007(19) -0.004(2) C10 0.027(2) 0.034(3) 0.026(3) -0.005(2) -0.001(2) -0.008(2) O11 0.087(4) 0.104(4) 0.095(4) 0.007(4) 0.003(4) 0.009(4) O1 0.028(2) 0.018(2) 0.039(2) 0.0068(18) -0.0084(19) -0.0025(17) N4 0.023(2) 0.030(2) 0.020(2) -0.002(2) 0.0018(19) -0.006(2) O10 0.34(4) 0.49(6) 0.43(6) 0.000 0.000 0.25(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O3 C1 1.270(7) . ? O3 Gd1 2.322(4) 6_666 ? O6 C14 1.286(7) . ? O6 Gd1 2.483(4) . ? O6 Gd1 2.576(4) 3_645 ? O5 C14 1.246(7) . ? O5 Gd1 2.433(4) 3_645 ? C14 C13 1.494(8) . ? C14 Gd1 2.870(6) 3_645 ? C13 C12 1.381(9) . ? C13 C17 1.430(8) . ? C2 C3 1.378(8) . ? C2 C8 1.429(8) . ? C2 C1 1.511(8) . ? O4 C1 1.247(7) . ? O4 Gd1 2.345(4) 8_766 ? O2 C9 1.258(8) . ? O2 Gd1 2.337(4) 6_666 ? C9 O1 1.260(7) . ? C9 C8 1.491(9) . ? C8 C7 1.396(8) . ? C7 C6 1.382(9) . ? C7 H7 0.9300 . ? Gd1 O3 2.322(4) 6_556 ? Gd1 O2 2.337(4) 6_556 ? Gd1 O4 2.345(4) 8_745 ? Gd1 O7 2.346(4) . ? Gd1 O1 2.354(4) 8_755 ? Gd1 O5 2.433(4) 3_655 ? Gd1 O6 2.576(4) 3_655 ? Gd1 C14 2.870(6) 3_655 ? Ag2 N1 2.118(5) . ? Ag2 N3 2.121(5) . ? Ag2 H9B 2.0913 . ? O7 C18 1.283(7) . ? C16 C17 1.375(8) . ? C16 C15 1.391(9) . ? C16 H16 0.9300 . ? N2 C5 1.334(8) . ? N2 C4 1.376(8) . ? N2 H2A 0.8600 . ? C15 N3 1.390(8) . ? C15 C11 1.399(8) . ? N1 C5 1.316(8) . ? N1 C6 1.394(8) . ? C18 O8 1.226(8) . ? C18 C17 1.507(9) . ? C5 H5 0.9300 . ? C12 C11 1.402(8) . ? C12 H12 0.9300 . ? C3 C4 1.397(8) . ? C3 H3 0.9300 . ? N3 C10 1.313(8) . ? C6 C4 1.390(8) . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? C11 N4 1.373(8) . ? C10 N4 1.332(8) . ? C10 H10 0.9300 . ? O11 H11A 0.8500 . ? O11 H11B 0.8499 . ? O1 Gd1 2.354(4) 8_756 ? N4 H4A 0.8600 . ? O10 H10A 0.8499 . ? O10 H10B 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 C1 O3 Gd1 126.4(4) . 6_666 ? C14 O6 Gd1 136.1(4) . . ? C14 O6 Gd1 89.6(3) . 3_645 ? Gd1 O6 Gd1 130.50(16) . 3_645 ? C14 O5 Gd1 97.3(4) . 3_645 ? O5 C14 O6 120.0(5) . . ? O5 C14 C13 121.0(5) . . ? O6 C14 C13 119.0(5) . . ? O5 C14 Gd1 57.2(3) . 3_645 ? O6 C14 Gd1 63.8(3) . 3_645 ? C13 C14 Gd1 168.0(4) . 3_645 ? C12 C13 C17 121.0(6) . . ? C12 C13 C14 118.9(5) . . ? C17 C13 C14 120.0(5) . . ? C3 C2 C8 120.9(5) . . ? C3 C2 C1 114.6(5) . . ? C8 C2 C1 124.5(5) . . ? C1 O4 Gd1 135.9(4) . 8_766 ? O4 C1 O3 124.0(5) . . ? O4 C1 C2 116.3(5) . . ? O3 C1 C2 119.4(5) . . ? C9 O2 Gd1 129.0(4) . 6_666 ? O2 C9 O1 123.0(6) . . ? O2 C9 C8 120.3(5) . . ? O1 C9 C8 116.7(6) . . ? C7 C8 C2 119.6(6) . . ? C7 C8 C9 117.3(5) . . ? C2 C8 C9 123.1(5) . . ? C6 C7 C8 118.9(6) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? O3 Gd1 O2 73.74(13) 6_556 6_556 ? O3 Gd1 O4 151.54(15) 6_556 8_745 ? O2 Gd1 O4 94.84(14) 6_556 8_745 ? O3 Gd1 O7 98.28(13) 6_556 . ? O2 Gd1 O7 144.82(15) 6_556 . ? O4 Gd1 O7 75.88(14) 8_745 . ? O3 Gd1 O1 87.59(16) 6_556 8_755 ? O2 Gd1 O1 142.39(14) 6_556 8_755 ? O4 Gd1 O1 114.90(16) 8_745 8_755 ? O7 Gd1 O1 68.80(15) . 8_755 ? O3 Gd1 O5 126.83(14) 6_556 3_655 ? O2 Gd1 O5 81.80(15) 6_556 3_655 ? O4 Gd1 O5 75.22(14) 8_745 3_655 ? O7 Gd1 O5 126.32(14) . 3_655 ? O1 Gd1 O5 84.10(16) 8_755 3_655 ? O3 Gd1 O6 77.53(14) 6_556 . ? O2 Gd1 O6 73.66(14) 6_556 . ? O4 Gd1 O6 74.22(14) 8_745 . ? O7 Gd1 O6 71.16(14) . . ? O1 Gd1 O6 134.47(15) 8_755 . ? O5 Gd1 O6 138.58(14) 3_655 . ? O3 Gd1 O6 75.72(13) 6_556 3_655 ? O2 Gd1 O6 72.29(14) 6_556 3_655 ? O4 Gd1 O6 126.41(14) 8_745 3_655 ? O7 Gd1 O6 140.13(14) . 3_655 ? O1 Gd1 O6 71.57(14) 8_755 3_655 ? O5 Gd1 O6 51.84(13) 3_655 3_655 ? O6 Gd1 O6 141.28(3) . 3_655 ? O3 Gd1 C14 101.39(16) 6_556 3_655 ? O2 Gd1 C14 72.96(15) 6_556 3_655 ? O4 Gd1 C14 99.86(16) 8_745 3_655 ? O7 Gd1 C14 141.60(15) . 3_655 ? O1 Gd1 C14 79.39(16) 8_755 3_655 ? O5 Gd1 C14 25.51(16) 3_655 3_655 ? O6 Gd1 C14 145.43(15) . 3_655 ? O6 Gd1 C14 26.61(15) 3_655 3_655 ? N1 Ag2 N3 169.2(2) . . ? N1 Ag2 H9B 94.5 . . ? N3 Ag2 H9B 95.6 . . ? C18 O7 Gd1 130.5(4) . . ? C17 C16 C15 118.1(6) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C5 N2 C4 107.7(5) . . ? C5 N2 H2A 126.2 . . ? C4 N2 H2A 126.2 . . ? N3 C15 C16 130.4(6) . . ? N3 C15 C11 108.2(5) . . ? C16 C15 C11 121.4(6) . . ? C5 N1 C6 105.7(5) . . ? C5 N1 Ag2 129.5(4) . . ? C6 N1 Ag2 123.7(4) . . ? O8 C18 O7 122.9(6) . . ? O8 C18 C17 119.7(6) . . ? O7 C18 C17 117.2(5) . . ? N1 C5 N2 112.5(6) . . ? N1 C5 H5 123.8 . . ? N2 C5 H5 123.8 . . ? C13 C12 C11 117.7(6) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C2 C3 C4 118.0(5) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C16 C17 C13 120.7(6) . . ? C16 C17 C18 116.4(5) . . ? C13 C17 C18 122.8(5) . . ? C10 N3 C15 105.8(5) . . ? C10 N3 Ag2 127.7(4) . . ? C15 N3 Ag2 126.5(4) . . ? C7 C6 C4 120.8(5) . . ? C7 C6 N1 130.9(6) . . ? C4 C6 N1 108.3(5) . . ? N2 C4 C6 105.8(5) . . ? N2 C4 C3 132.9(6) . . ? C6 C4 C3 121.4(6) . . ? H9A O9 H9B 120.0 . . ? N4 C11 C15 105.6(5) . . ? N4 C11 C12 133.5(5) . . ? C15 C11 C12 120.9(6) . . ? N3 C10 N4 112.7(6) . . ? N3 C10 H10 123.6 . . ? N4 C10 H10 123.6 . . ? H11A O11 H11B 120.0 . . ? C9 O1 Gd1 133.9(4) . 8_756 ? C10 N4 C11 107.7(5) . . ? C10 N4 H4A 126.1 . . ? C11 N4 H4A 126.1 . . ? H10A O10 H10B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Gd1 O5 C14 O6 12.0(6) 3_645 . . . ? Gd1 O5 C14 C13 -166.0(5) 3_645 . . . ? Gd1 O6 C14 O5 147.1(4) . . . . ? Gd1 O6 C14 O5 -11.2(5) 3_645 . . . ? Gd1 O6 C14 C13 -34.9(8) . . . . ? Gd1 O6 C14 C13 166.8(5) 3_645 . . . ? Gd1 O6 C14 Gd1 158.3(5) . . . 3_645 ? O5 C14 C13 C12 -36.4(8) . . . . ? O6 C14 C13 C12 145.7(6) . . . . ? Gd1 C14 C13 C12 -114.0(19) 3_645 . . . ? O5 C14 C13 C17 145.0(6) . . . . ? O6 C14 C13 C17 -33.0(8) . . . . ? Gd1 C14 C13 C17 67(2) 3_645 . . . ? Gd1 O4 C1 O3 -48.6(9) 8_766 . . . ? Gd1 O4 C1 C2 136.6(5) 8_766 . . . ? Gd1 O3 C1 O4 89.8(6) 6_666 . . . ? Gd1 O3 C1 C2 -95.6(6) 6_666 . . . ? C3 C2 C1 O4 50.1(7) . . . . ? C8 C2 C1 O4 -131.0(6) . . . . ? C3 C2 C1 O3 -124.9(6) . . . . ? C8 C2 C1 O3 54.0(8) . . . . ? Gd1 O2 C9 O1 85.9(7) 6_666 . . . ? Gd1 O2 C9 C8 -94.2(6) 6_666 . . . ? C3 C2 C8 C7 -4.5(9) . . . . ? C1 C2 C8 C7 176.6(5) . . . . ? C3 C2 C8 C9 174.3(5) . . . . ? C1 C2 C8 C9 -4.5(9) . . . . ? O2 C9 C8 C7 -150.2(6) . . . . ? O1 C9 C8 C7 29.6(8) . . . . ? O2 C9 C8 C2 30.9(9) . . . . ? O1 C9 C8 C2 -149.2(6) . . . . ? C2 C8 C7 C6 3.4(9) . . . . ? C9 C8 C7 C6 -175.6(5) . . . . ? C14 O6 Gd1 O3 -25.4(5) . . . 6_556 ? Gd1 O6 Gd1 O3 125.5(2) 3_645 . . 6_556 ? C14 O6 Gd1 O2 -101.8(5) . . . 6_556 ? Gd1 O6 Gd1 O2 49.1(2) 3_645 . . 6_556 ? C14 O6 Gd1 O4 158.1(5) . . . 8_745 ? Gd1 O6 Gd1 O4 -51.0(2) 3_645 . . 8_745 ? C14 O6 Gd1 O7 78.0(5) . . . . ? Gd1 O6 Gd1 O7 -131.1(2) 3_645 . . . ? C14 O6 Gd1 O1 48.5(6) . . . 8_755 ? Gd1 O6 Gd1 O1 -160.6(2) 3_645 . . 8_755 ? C14 O6 Gd1 O5 -158.0(5) . . . 3_655 ? Gd1 O6 Gd1 O5 -7.1(3) 3_645 . . 3_655 ? C14 O6 Gd1 O6 -72.5(5) . . . 3_655 ? Gd1 O6 Gd1 O6 78.4(3) 3_645 . . 3_655 ? C14 O6 Gd1 C14 -117.4(5) . . . 3_655 ? Gd1 O6 Gd1 C14 33.5(4) 3_645 . . 3_655 ? O3 Gd1 O7 C18 52.9(5) 6_556 . . . ? O2 Gd1 O7 C18 -20.6(6) 6_556 . . . ? O4 Gd1 O7 C18 -98.7(5) 8_745 . . . ? O1 Gd1 O7 C18 137.0(5) 8_755 . . . ? O5 Gd1 O7 C18 -157.9(5) 3_655 . . . ? O6 Gd1 O7 C18 -20.8(5) . . . . ? O6 Gd1 O7 C18 130.5(5) 3_655 . . . ? C14 Gd1 O7 C18 173.2(5) 3_655 . . . ? C17 C16 C15 N3 -175.0(6) . . . . ? C17 C16 C15 C11 3.5(9) . . . . ? N3 Ag2 N1 C5 -153.2(10) . . . . ? N3 Ag2 N1 C6 12.9(14) . . . . ? Gd1 O7 C18 O8 131.7(6) . . . . ? Gd1 O7 C18 C17 -52.4(7) . . . . ? C6 N1 C5 N2 -2.1(7) . . . . ? Ag2 N1 C5 N2 165.9(4) . . . . ? C4 N2 C5 N1 -0.1(8) . . . . ? C17 C13 C12 C11 2.6(9) . . . . ? C14 C13 C12 C11 -176.0(5) . . . . ? C8 C2 C3 C4 -0.2(8) . . . . ? C1 C2 C3 C4 178.7(5) . . . . ? C15 C16 C17 C13 -1.1(9) . . . . ? C15 C16 C17 C18 -178.8(5) . . . . ? C12 C13 C17 C16 -2.0(9) . . . . ? C14 C13 C17 C16 176.6(5) . . . . ? C12 C13 C17 C18 175.5(5) . . . . ? C14 C13 C17 C18 -5.8(9) . . . . ? O8 C18 C17 C16 80.9(8) . . . . ? O7 C18 C17 C16 -95.1(7) . . . . ? O8 C18 C17 C13 -96.8(8) . . . . ? O7 C18 C17 C13 87.2(7) . . . . ? C16 C15 N3 C10 179.7(7) . . . . ? C11 C15 N3 C10 1.0(7) . . . . ? C16 C15 N3 Ag2 2.9(10) . . . . ? C11 C15 N3 Ag2 -175.8(4) . . . . ? N1 Ag2 N3 C10 4.6(15) . . . . ? N1 Ag2 N3 C15 -179.3(9) . . . . ? C8 C7 C6 C4 2.4(9) . . . . ? C8 C7 C6 N1 178.9(6) . . . . ? C5 N1 C6 C7 -173.3(7) . . . . ? Ag2 N1 C6 C7 17.8(9) . . . . ? C5 N1 C6 C4 3.5(7) . . . . ? Ag2 N1 C6 C4 -165.3(4) . . . . ? C5 N2 C4 C6 2.3(7) . . . . ? C5 N2 C4 C3 -176.6(7) . . . . ? C7 C6 C4 N2 173.6(6) . . . . ? N1 C6 C4 N2 -3.6(7) . . . . ? C7 C6 C4 C3 -7.3(9) . . . . ? N1 C6 C4 C3 175.5(5) . . . . ? C2 C3 C4 N2 -175.2(6) . . . . ? C2 C3 C4 C6 6.1(9) . . . . ? N3 C15 C11 N4 -1.7(7) . . . . ? C16 C15 C11 N4 179.5(6) . . . . ? N3 C15 C11 C12 175.9(5) . . . . ? C16 C15 C11 C12 -2.9(9) . . . . ? C13 C12 C11 N4 176.5(6) . . . . ? C13 C12 C11 C15 -0.2(9) . . . . ? C15 N3 C10 N4 0.1(8) . . . . ? Ag2 N3 C10 N4 176.8(4) . . . . ? O2 C9 O1 Gd1 -66.2(9) . . . 8_756 ? C8 C9 O1 Gd1 114.0(6) . . . 8_756 ? N3 C10 N4 C11 -1.2(8) . . . . ? C15 C11 N4 C10 1.7(7) . . . . ? C12 C11 N4 C10 -175.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.034 _refine_diff_density_min -2.488 _refine_diff_density_rms 0.152 data_2 _database_code_depnum_ccdc_archive 'CCDC 735029' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Ag N4 O10.50 Sm' _chemical_formula_weight 711.54 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 8.5955(17) _cell_length_b 25.363(5) _cell_length_c 17.822(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3885.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3414 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25 _exptl_crystal_description square _exptl_crystal_colour light _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 4.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4961 _exptl_absorpt_correction_T_max 0.6405 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24390 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3414 _reflns_number_gt 3253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+12.5835P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3414 _refine_ls_number_parameters 312 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.16303(2) 1.023868(7) 0.783622(10) 0.01231(8) Uani 1 1 d . . . Ag1 Ag 0.46100(4) 0.773427(13) 0.45053(2) 0.03027(11) Uani 1 1 d . . . O1 O 0.0755(3) 1.02043(10) 0.65899(15) 0.0170(6) Uani 1 1 d . . . O2 O -0.1346(3) 0.97471(11) 0.62637(16) 0.0212(6) Uani 1 1 d . . . O3 O 0.2203(3) 0.93867(10) 0.73875(15) 0.0188(6) Uani 1 1 d . . . O4 O 0.4514(3) 0.91822(11) 0.69216(18) 0.0268(7) Uani 1 1 d . . . O5 O 0.0591(3) 0.97284(12) 0.89020(16) 0.0263(7) Uani 1 1 d . . . O6 O 0.4105(3) 1.03171(10) 0.70994(15) 0.0163(6) Uani 1 1 d . . . O7 O 0.2463(3) 1.11306(10) 0.78577(15) 0.0205(6) Uani 1 1 d . . . O8 O 0.4502(4) 1.16364(16) 0.7645(2) 0.0499(11) Uani 1 1 d . . . N1 N 0.1263(4) 0.88983(13) 0.38797(19) 0.0217(7) Uani 1 1 d . . . H1 H 0.0618 0.9033 0.3564 0.026 Uiso 1 1 d R . . N2 N 0.3146(4) 0.83945(14) 0.4330(2) 0.0231(8) Uani 1 1 d . . . N3 N -0.4037(4) 0.79066(13) 0.9899(2) 0.0242(8) Uani 1 1 d . . . N4 N -0.3040(4) 0.85112(14) 1.0649(2) 0.0245(8) Uani 1 1 d . . . H4 H -0.2833 0.8680 1.1055 0.029 Uiso 1 1 d R . . C1 C 0.0100(4) 0.98160(15) 0.6275(2) 0.0155(8) Uani 1 1 d . . . C2 C 0.1056(4) 0.94327(14) 0.5818(2) 0.0149(8) Uani 1 1 d . . . C3 C 0.0548(4) 0.93667(14) 0.5087(2) 0.0162(8) Uani 1 1 d . . . H3 H -0.0327 0.9543 0.4910 0.019 Uiso 1 1 calc R . . C4 C 0.1391(5) 0.90274(16) 0.4626(2) 0.0174(8) Uani 1 1 d . . . C5 C 0.2327(5) 0.85247(16) 0.3731(2) 0.0241(9) Uani 1 1 d . . . H5 H 0.2470 0.8375 0.3260 0.029 Uiso 1 1 calc R . . C6 C 0.2605(5) 0.87243(14) 0.4906(2) 0.0176(8) Uani 1 1 d . . . C7 C 0.3137(5) 0.87961(16) 0.5630(2) 0.0202(9) Uani 1 1 d . . . H7 H 0.3980 0.8603 0.5808 0.024 Uiso 1 1 calc R . . C8 C 0.2397(4) 0.91598(14) 0.6086(2) 0.0161(8) Uani 1 1 d . . . C9 C 0.3065(4) 0.92521(14) 0.6851(2) 0.0169(8) Uani 1 1 d . . . C10 C -0.0506(4) 0.95181(15) 0.8555(2) 0.0166(8) Uani 1 1 d . . . C11 C -0.1361(4) 0.90582(15) 0.8883(2) 0.0158(8) Uani 1 1 d . . . C12 C -0.1609(4) 0.90484(16) 0.9655(2) 0.0175(8) Uani 1 1 d . . . H12 H -0.1197 0.9307 0.9967 0.021 Uiso 1 1 calc R . . C13 C -0.2502(5) 0.86337(15) 0.9941(2) 0.0177(8) Uani 1 1 d . . . C14 C -0.3937(5) 0.80865(17) 1.0591(2) 0.0264(10) Uani 1 1 d . . . H14 H -0.4442 0.7932 1.0997 0.032 Uiso 1 1 calc R . . C15 C -0.3120(5) 0.82445(15) 0.9468(2) 0.0191(8) Uani 1 1 d . . . C16 C -0.2803(5) 0.82419(15) 0.8700(2) 0.0200(8) Uani 1 1 d . . . H16 H -0.3165 0.7972 0.8394 0.024 Uiso 1 1 calc R . . C17 C -0.1939(4) 0.86508(15) 0.8410(2) 0.0165(8) Uani 1 1 d . . . C18 C 0.3406(5) 1.13740(16) 0.7422(2) 0.0200(9) Uani 1 1 d . . . O11 O 0.2500 0.7500 0.6119(12) 0.284(10) Uani 1 2 d S . . H11A H 0.2735 0.7550 0.5661 0.426 Uiso 0.50 1 d PR . . H11B H 0.2168 0.7755 0.6384 0.426 Uiso 0.50 1 d PR . . O9 O 0.4132(6) 0.74653(19) 0.7998(3) 0.0723(13) Uani 1 1 d . . . H9A H 0.3569 0.7574 0.7637 0.108 Uiso 1 1 d R . . H9B H 0.4455 0.7142 0.7992 0.108 Uiso 1 1 d R . . O10 O 0.5376(12) 0.7974(3) 0.6804(5) 0.176(4) Uani 1 1 d . . . H10A H 0.5174 0.7648 0.6764 0.264 Uiso 1 1 d R . . H10B H 0.5715 0.8145 0.6428 0.264 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.00964(12) 0.01573(12) 0.01157(12) -0.00059(7) -0.00015(7) -0.00191(7) Ag1 0.0356(2) 0.02232(18) 0.0329(2) -0.00010(14) 0.00146(15) 0.01423(15) O1 0.0208(14) 0.0176(13) 0.0126(14) -0.0026(11) -0.0024(11) 0.0038(11) O2 0.0125(14) 0.0342(17) 0.0169(15) -0.0008(12) 0.0026(11) 0.0021(12) O3 0.0227(15) 0.0182(14) 0.0154(14) 0.0004(11) 0.0004(12) 0.0014(12) O4 0.0142(15) 0.0261(15) 0.0401(19) -0.0094(14) -0.0092(13) 0.0024(12) O5 0.0247(16) 0.0388(18) 0.0154(15) 0.0068(13) -0.0062(12) -0.0162(13) O6 0.0134(14) 0.0190(13) 0.0165(14) 0.0043(11) 0.0018(11) 0.0013(11) O7 0.0262(15) 0.0180(14) 0.0174(15) 0.0010(11) 0.0059(12) -0.0038(12) O8 0.054(2) 0.071(3) 0.0246(18) 0.0034(18) -0.0061(17) -0.042(2) N1 0.0265(19) 0.0219(18) 0.0167(18) -0.0007(14) -0.0020(15) 0.0042(15) N2 0.0260(19) 0.0224(18) 0.0208(19) -0.0041(14) 0.0019(15) 0.0058(15) N3 0.030(2) 0.0218(17) 0.0204(19) 0.0017(15) 0.0043(15) -0.0080(16) N4 0.032(2) 0.0247(19) 0.0163(18) -0.0025(14) 0.0013(15) -0.0103(16) C1 0.0133(19) 0.022(2) 0.0111(19) 0.0026(15) 0.0002(15) 0.0031(16) C2 0.0138(19) 0.0143(18) 0.0167(19) 0.0002(15) 0.0011(15) -0.0010(15) C3 0.0163(19) 0.0162(19) 0.016(2) 0.0006(15) -0.0015(15) 0.0028(15) C4 0.018(2) 0.0192(19) 0.015(2) 0.0004(15) 0.0006(15) -0.0004(16) C5 0.032(2) 0.023(2) 0.017(2) -0.0044(17) 0.0013(18) 0.0080(19) C6 0.0174(19) 0.0152(18) 0.020(2) -0.0016(15) 0.0030(16) 0.0030(16) C7 0.0141(19) 0.022(2) 0.024(2) 0.0004(17) -0.0026(16) 0.0031(16) C8 0.0140(19) 0.0152(18) 0.019(2) 0.0008(15) 0.0001(16) 0.0004(15) C9 0.016(2) 0.0120(18) 0.022(2) 0.0006(16) -0.0047(17) 0.0004(15) C10 0.0107(18) 0.022(2) 0.017(2) 0.0009(16) 0.0027(15) -0.0009(16) C11 0.0121(18) 0.0164(19) 0.019(2) 0.0024(15) 0.0006(15) 0.0006(15) C12 0.017(2) 0.020(2) 0.015(2) -0.0013(16) -0.0034(15) -0.0042(16) C13 0.022(2) 0.0173(18) 0.0141(19) -0.0002(15) 0.0011(15) -0.0006(16) C14 0.034(2) 0.025(2) 0.021(2) 0.0025(17) 0.0071(19) -0.0095(19) C15 0.022(2) 0.0167(19) 0.019(2) 0.0033(16) 0.0002(16) -0.0030(16) C16 0.024(2) 0.0177(19) 0.019(2) -0.0016(16) -0.0013(17) -0.0006(17) C17 0.0169(19) 0.0174(19) 0.015(2) -0.0001(15) -0.0001(15) 0.0036(15) C18 0.023(2) 0.022(2) 0.015(2) -0.0009(17) -0.0015(16) -0.0027(17) O11 0.30(2) 0.25(2) 0.29(3) 0.000 0.000 -0.09(2) O9 0.083(4) 0.058(3) 0.076(3) -0.003(3) 0.015(3) 0.013(3) O10 0.296(13) 0.118(6) 0.114(6) 0.016(5) -0.026(7) -0.098(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 Sm1 O1 2.347(3) . ? Sm1 O3 2.356(3) . ? Sm1 O2 2.367(3) 3_576 ? Sm1 O7 2.373(3) . ? Sm1 O4 2.378(3) 3_476 ? Sm1 O5 2.466(3) . ? Sm1 O6 2.508(3) . ? Sm1 O6 2.591(3) 3_476 ? Sm1 C10 2.890(4) . ? Ag1 N2 2.118(3) . ? Ag1 N3 2.118(3) 8_675 ? O1 C1 1.266(5) . ? O2 C1 1.255(5) . ? O2 Sm1 2.367(3) 3_476 ? O3 C9 1.256(5) . ? O4 C9 1.264(5) . ? O4 Sm1 2.378(3) 3_576 ? O5 C10 1.248(5) . ? O6 C10 1.283(5) 3_576 ? O6 Sm1 2.591(3) 3_576 ? O7 C18 1.281(5) . ? O8 C18 1.220(5) . ? N1 C5 1.343(5) . ? N1 C4 1.375(5) . ? N1 H1 0.8600 . ? N2 C5 1.321(5) . ? N2 C6 1.403(5) . ? N3 C14 1.318(6) . ? N3 C15 1.396(5) . ? N3 Ag1 2.118(3) 8_476 ? N4 C14 1.329(6) . ? N4 C13 1.378(5) . ? N4 H4 0.8601 . ? C1 C2 1.510(5) . ? C2 C3 1.385(5) . ? C2 C8 1.427(5) . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C6 1.388(6) . ? C5 H5 0.9300 . ? C6 C7 1.382(6) . ? C7 C8 1.385(6) . ? C7 H7 0.9300 . ? C8 C9 1.498(5) . ? C10 O6 1.283(5) 3_476 ? C10 C11 1.497(5) . ? C11 C12 1.391(6) . ? C11 C17 1.424(5) . ? C12 C13 1.399(6) . ? C12 H12 0.9300 . ? C13 C15 1.403(6) . ? C14 H14 0.9300 . ? C15 C16 1.395(6) . ? C16 C17 1.377(6) . ? C16 H16 0.9300 . ? C17 C18 1.512(6) 3_476 ? C18 C17 1.512(6) 3_576 ? O11 H11A 0.8500 . ? O11 H11B 0.8501 . ? O9 H9A 0.8501 . ? O9 H9B 0.8657 . ? O10 H10A 0.8500 . ? O10 H10B 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O3 73.24(9) . . ? O1 Sm1 O2 151.36(10) . 3_576 ? O3 Sm1 O2 95.18(10) . 3_576 ? O1 Sm1 O7 98.47(9) . . ? O3 Sm1 O7 144.75(10) . . ? O2 Sm1 O7 75.69(10) 3_576 . ? O1 Sm1 O4 87.11(10) . 3_476 ? O3 Sm1 O4 142.02(10) . 3_476 ? O2 Sm1 O4 115.47(10) 3_576 3_476 ? O7 Sm1 O4 68.83(10) . 3_476 ? O1 Sm1 O5 126.41(9) . . ? O3 Sm1 O5 81.71(10) . . ? O2 Sm1 O5 75.65(10) 3_576 . ? O7 Sm1 O5 126.67(9) . . ? O4 Sm1 O5 84.68(11) 3_476 . ? O1 Sm1 O6 77.24(9) . . ? O3 Sm1 O6 73.60(9) . . ? O2 Sm1 O6 74.34(10) 3_576 . ? O7 Sm1 O6 71.15(9) . . ? O4 Sm1 O6 134.03(10) 3_476 . ? O5 Sm1 O6 138.78(9) . . ? O1 Sm1 O6 75.71(9) . 3_476 ? O3 Sm1 O6 72.01(9) . 3_476 ? O2 Sm1 O6 126.45(9) 3_576 3_476 ? O7 Sm1 O6 140.42(9) . 3_476 ? O4 Sm1 O6 71.77(9) 3_476 3_476 ? O5 Sm1 O6 51.45(9) . 3_476 ? O6 Sm1 O6 140.99(2) . 3_476 ? O1 Sm1 C10 101.10(10) . . ? O3 Sm1 C10 72.75(10) . . ? O2 Sm1 C10 100.15(10) 3_576 . ? O7 Sm1 C10 141.94(10) . . ? O4 Sm1 C10 79.87(11) 3_476 . ? O5 Sm1 C10 25.39(10) . . ? O6 Sm1 C10 145.21(10) . . ? O6 Sm1 C10 26.36(10) 3_476 . ? N2 Ag1 N3 169.03(14) . 8_675 ? C1 O1 Sm1 126.2(2) . . ? C1 O2 Sm1 135.6(3) . 3_476 ? C9 O3 Sm1 129.1(2) . . ? C9 O4 Sm1 133.2(3) . 3_576 ? C10 O5 Sm1 96.7(2) . . ? C10 O6 Sm1 136.3(2) 3_576 . ? C10 O6 Sm1 90.0(2) 3_576 3_576 ? Sm1 O6 Sm1 130.12(10) . 3_576 ? C18 O7 Sm1 129.8(3) . . ? C5 N1 C4 107.8(3) . . ? C5 N1 H1 126.1 . . ? C4 N1 H1 126.1 . . ? C5 N2 C6 105.4(3) . . ? C5 N2 Ag1 129.3(3) . . ? C6 N2 Ag1 124.1(3) . . ? C14 N3 C15 105.5(3) . . ? C14 N3 Ag1 127.7(3) . 8_476 ? C15 N3 Ag1 126.8(3) . 8_476 ? C14 N4 C13 107.9(3) . . ? C14 N4 H4 126.0 . . ? C13 N4 H4 126.1 . . ? O2 C1 O1 123.8(4) . . ? O2 C1 C2 116.1(3) . . ? O1 C1 C2 119.9(3) . . ? C3 C2 C8 120.7(3) . . ? C3 C2 C1 114.4(3) . . ? C8 C2 C1 124.8(3) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? N1 C4 C6 106.0(3) . . ? N1 C4 C3 132.6(4) . . ? C6 C4 C3 121.4(4) . . ? N2 C5 N1 112.3(4) . . ? N2 C5 H5 123.9 . . ? N1 C5 H5 123.9 . . ? C7 C6 C4 120.7(4) . . ? C7 C6 N2 130.7(4) . . ? C4 C6 N2 108.5(4) . . ? C6 C7 C8 119.0(4) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C2 119.8(4) . . ? C7 C8 C9 117.6(3) . . ? C2 C8 C9 122.6(3) . . ? O3 C9 O4 122.9(4) . . ? O3 C9 C8 120.6(3) . . ? O4 C9 C8 116.5(4) . . ? O5 C10 O6 120.5(4) . 3_476 ? O5 C10 C11 120.7(4) . . ? O6 C10 C11 118.7(3) 3_476 . ? O5 C10 Sm1 57.9(2) . . ? O6 C10 Sm1 63.67(19) 3_476 . ? C11 C10 Sm1 167.8(3) . . ? C12 C11 C17 121.3(4) . . ? C12 C11 C10 118.3(4) . . ? C17 C11 C10 120.3(4) . . ? C11 C12 C13 117.3(4) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? N4 C13 C12 133.5(4) . . ? N4 C13 C15 105.3(3) . . ? C12 C13 C15 121.1(4) . . ? N3 C14 N4 113.0(4) . . ? N3 C14 H14 123.5 . . ? N4 C14 H14 123.5 . . ? C16 C15 N3 130.4(4) . . ? C16 C15 C13 121.3(4) . . ? N3 C15 C13 108.3(3) . . ? C17 C16 C15 118.1(4) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 C11 120.8(4) . . ? C16 C17 C18 116.3(3) . 3_476 ? C11 C17 C18 122.9(3) . 3_476 ? O8 C18 O7 123.6(4) . . ? O8 C18 C17 119.6(4) . 3_576 ? O7 C18 C17 116.8(3) . 3_576 ? H11A O11 H11B 120.0 . . ? H9A O9 H9B 118.8 . . ? H10A O10 H10B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Sm1 O1 C1 38.9(3) . . . . ? O2 Sm1 O1 C1 108.2(3) 3_576 . . . ? O7 Sm1 O1 C1 -176.2(3) . . . . ? O4 Sm1 O1 C1 -108.1(3) 3_476 . . . ? O5 Sm1 O1 C1 -26.9(3) . . . . ? O6 Sm1 O1 C1 115.4(3) . . . . ? O6 Sm1 O1 C1 -36.2(3) 3_476 . . . ? C10 Sm1 O1 C1 -29.0(3) . . . . ? O1 Sm1 O3 C9 61.1(3) . . . . ? O2 Sm1 O3 C9 -92.2(3) 3_576 . . . ? O7 Sm1 O3 C9 -19.7(4) . . . . ? O4 Sm1 O3 C9 123.0(3) 3_476 . . . ? O5 Sm1 O3 C9 -166.8(3) . . . . ? O6 Sm1 O3 C9 -20.2(3) . . . . ? O6 Sm1 O3 C9 141.1(3) 3_476 . . . ? C10 Sm1 O3 C9 168.8(3) . . . . ? O1 Sm1 O5 C10 -4.9(3) . . . . ? O3 Sm1 O5 C10 -66.9(2) . . . . ? O2 Sm1 O5 C10 -164.5(3) 3_576 . . . ? O7 Sm1 O5 C10 136.1(2) . . . . ? O4 Sm1 O5 C10 77.5(3) 3_476 . . . ? O6 Sm1 O5 C10 -120.1(2) . . . . ? O6 Sm1 O5 C10 6.7(2) 3_476 . . . ? O1 Sm1 O6 C10 26.1(3) . . . 3_576 ? O3 Sm1 O6 C10 102.2(4) . . . 3_576 ? O2 Sm1 O6 C10 -157.4(4) 3_576 . . 3_576 ? O7 Sm1 O6 C10 -77.6(3) . . . 3_576 ? O4 Sm1 O6 C10 -47.0(4) 3_476 . . 3_576 ? O5 Sm1 O6 C10 157.8(3) . . . 3_576 ? O6 Sm1 O6 C10 73.2(3) 3_476 . . 3_576 ? C10 Sm1 O6 C10 117.3(3) . . . 3_576 ? O1 Sm1 O6 Sm1 -125.44(15) . . . 3_576 ? O3 Sm1 O6 Sm1 -49.42(14) . . . 3_576 ? O2 Sm1 O6 Sm1 50.97(14) 3_576 . . 3_576 ? O7 Sm1 O6 Sm1 130.85(16) . . . 3_576 ? O4 Sm1 O6 Sm1 161.46(13) 3_476 . . 3_576 ? O5 Sm1 O6 Sm1 6.3(2) . . . 3_576 ? O6 Sm1 O6 Sm1 -78.40(17) 3_476 . . 3_576 ? C10 Sm1 O6 Sm1 -34.3(2) . . . 3_576 ? O1 Sm1 O7 C18 -53.9(3) . . . . ? O3 Sm1 O7 C18 19.0(4) . . . . ? O2 Sm1 O7 C18 97.5(3) 3_576 . . . ? O4 Sm1 O7 C18 -137.4(4) 3_476 . . . ? O5 Sm1 O7 C18 156.9(3) . . . . ? O6 Sm1 O7 C18 19.5(3) . . . . ? O6 Sm1 O7 C18 -131.7(3) 3_476 . . . ? C10 Sm1 O7 C18 -174.3(3) . . . . ? N3 Ag1 N2 C5 -152.4(7) 8_675 . . . ? N3 Ag1 N2 C6 13.1(9) 8_675 . . . ? Sm1 O2 C1 O1 -48.8(6) 3_476 . . . ? Sm1 O2 C1 C2 137.1(3) 3_476 . . . ? Sm1 O1 C1 O2 90.8(4) . . . . ? Sm1 O1 C1 C2 -95.4(4) . . . . ? O2 C1 C2 C3 50.0(5) . . . . ? O1 C1 C2 C3 -124.4(4) . . . . ? O2 C1 C2 C8 -131.3(4) . . . . ? O1 C1 C2 C8 54.4(5) . . . . ? C8 C2 C3 C4 -0.1(6) . . . . ? C1 C2 C3 C4 178.7(3) . . . . ? C5 N1 C4 C6 1.6(5) . . . . ? C5 N1 C4 C3 -176.5(4) . . . . ? C2 C3 C4 N1 -175.8(4) . . . . ? C2 C3 C4 C6 6.3(6) . . . . ? C6 N2 C5 N1 -2.2(5) . . . . ? Ag1 N2 C5 N1 165.4(3) . . . . ? C4 N1 C5 N2 0.4(5) . . . . ? N1 C4 C6 C7 173.8(4) . . . . ? C3 C4 C6 C7 -7.9(6) . . . . ? N1 C4 C6 N2 -3.0(4) . . . . ? C3 C4 C6 N2 175.4(4) . . . . ? C5 N2 C6 C7 -173.1(4) . . . . ? Ag1 N2 C6 C7 18.4(6) . . . . ? C5 N2 C6 C4 3.2(5) . . . . ? Ag1 N2 C6 C4 -165.3(3) . . . . ? C4 C6 C7 C8 2.8(6) . . . . ? N2 C6 C7 C8 178.8(4) . . . . ? C6 C7 C8 C2 3.3(6) . . . . ? C6 C7 C8 C9 -176.3(4) . . . . ? C3 C2 C8 C7 -4.7(6) . . . . ? C1 C2 C8 C7 176.7(4) . . . . ? C3 C2 C8 C9 174.9(4) . . . . ? C1 C2 C8 C9 -3.8(6) . . . . ? Sm1 O3 C9 O4 86.3(4) . . . . ? Sm1 O3 C9 C8 -94.4(4) . . . . ? Sm1 O4 C9 O3 -68.2(5) 3_576 . . . ? Sm1 O4 C9 C8 112.5(4) 3_576 . . . ? C7 C8 C9 O3 -150.4(4) . . . . ? C2 C8 C9 O3 30.1(6) . . . . ? C7 C8 C9 O4 29.0(5) . . . . ? C2 C8 C9 O4 -150.6(4) . . . . ? Sm1 O5 C10 O6 -12.3(4) . . . 3_476 ? Sm1 O5 C10 C11 165.8(3) . . . . ? O1 Sm1 C10 O5 176.0(2) . . . . ? O3 Sm1 C10 O5 107.6(3) . . . . ? O2 Sm1 C10 O5 15.3(3) 3_576 . . . ? O7 Sm1 C10 O5 -64.4(3) . . . . ? O4 Sm1 C10 O5 -99.0(3) 3_476 . . . ? O6 Sm1 C10 O5 92.4(3) . . . . ? O6 Sm1 C10 O5 -168.2(4) 3_476 . . . ? O1 Sm1 C10 O6 -15.8(2) . . . 3_476 ? O3 Sm1 C10 O6 -84.2(2) . . . 3_476 ? O2 Sm1 C10 O6 -176.5(2) 3_576 . . 3_476 ? O7 Sm1 C10 O6 103.8(2) . . . 3_476 ? O4 Sm1 C10 O6 69.2(2) 3_476 . . 3_476 ? O5 Sm1 C10 O6 168.2(4) . . . 3_476 ? O6 Sm1 C10 O6 -99.4(2) . . . 3_476 ? O1 Sm1 C10 C11 88.6(13) . . . . ? O3 Sm1 C10 C11 20.3(13) . . . . ? O2 Sm1 C10 C11 -72.1(13) 3_576 . . . ? O7 Sm1 C10 C11 -151.8(12) . . . . ? O4 Sm1 C10 C11 173.6(13) 3_476 . . . ? O5 Sm1 C10 C11 -87.3(13) . . . . ? O6 Sm1 C10 C11 5.1(14) . . . . ? O6 Sm1 C10 C11 104.4(14) 3_476 . . . ? O5 C10 C11 C12 36.4(5) . . . . ? O6 C10 C11 C12 -145.5(4) 3_476 . . . ? Sm1 C10 C11 C12 116.3(12) . . . . ? O5 C10 C11 C17 -145.3(4) . . . . ? O6 C10 C11 C17 32.8(5) 3_476 . . . ? Sm1 C10 C11 C17 -65.4(14) . . . . ? C17 C11 C12 C13 -2.6(6) . . . . ? C10 C11 C12 C13 175.7(3) . . . . ? C14 N4 C13 C12 175.6(5) . . . . ? C14 N4 C13 C15 -1.2(5) . . . . ? C11 C12 C13 N4 -176.3(4) . . . . ? C11 C12 C13 C15 0.0(6) . . . . ? C15 N3 C14 N4 0.1(5) . . . . ? Ag1 N3 C14 N4 -177.0(3) 8_476 . . . ? C13 N4 C14 N3 0.7(5) . . . . ? C14 N3 C15 C16 -179.9(5) . . . . ? Ag1 N3 C15 C16 -2.8(7) 8_476 . . . ? C14 N3 C15 C13 -0.9(5) . . . . ? Ag1 N3 C15 C13 176.3(3) 8_476 . . . ? N4 C13 C15 C16 -179.6(4) . . . . ? C12 C13 C15 C16 3.2(6) . . . . ? N4 C13 C15 N3 1.3(5) . . . . ? C12 C13 C15 N3 -176.0(4) . . . . ? N3 C15 C16 C17 175.2(4) . . . . ? C13 C15 C16 C17 -3.8(6) . . . . ? C15 C16 C17 C11 1.2(6) . . . . ? C15 C16 C17 C18 178.7(4) . . . 3_476 ? C12 C11 C17 C16 2.0(6) . . . . ? C10 C11 C17 C16 -176.3(4) . . . . ? C12 C11 C17 C18 -175.3(4) . . . 3_476 ? C10 C11 C17 C18 6.4(6) . . . 3_476 ? Sm1 O7 C18 O8 -129.2(4) . . . . ? Sm1 O7 C18 C17 54.0(5) . . . 3_576 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.724 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.112 data_4 _database_code_depnum_ccdc_archive 'CCDC 735030' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Ag N4 O10.50 Tb' _chemical_formula_weight 720.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.287(5) _cell_length_b 8.5525(17) _cell_length_c 17.827(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3855.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11983 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.02 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 4.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3311 _exptl_absorpt_correction_T_max 0.4514 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24363 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3397 _reflns_number_gt 3243 _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^)+(0.0416P)^2^+27.8445P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00121(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3397 _refine_ls_number_parameters 313 _refine_ls_number_restraints 894 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3 O 1.02135(12) 0.9221(4) 0.66009(18) 0.0085(6) Uani 1 1 d U . . O6 O 0.53068(12) 0.0873(4) 0.28953(18) 0.0085(7) Uani 1 1 d U . . O5 O 0.52439(13) -0.0622(4) 0.38953(19) 0.0117(7) Uani 1 1 d U . . C14 C 0.54621(18) 0.0487(5) 0.3553(3) 0.0090(8) Uani 1 1 d U . . C13 C 0.59198(18) 0.1331(5) 0.3890(3) 0.0086(8) Uani 1 1 d U . . C2 C 0.94436(18) 0.8940(5) 0.5830(3) 0.0080(8) Uani 1 1 d U . . O4 O 0.97540(12) 1.1354(4) 0.62836(19) 0.0093(7) Uani 1 1 d U . . C1 C 0.98254(18) 0.9895(5) 0.6287(3) 0.0079(9) Uani 1 1 d U . . O2 O 0.94002(12) 0.7786(4) 0.73975(18) 0.0081(6) Uani 1 1 d U . . C9 C 0.92590(18) 0.6913(5) 0.6862(3) 0.0101(9) Uani 1 1 d U . . C8 C 0.91695(18) 0.7587(6) 0.6094(3) 0.0100(8) Uani 1 1 d U . . C7 C 0.8804(2) 0.6836(5) 0.5637(3) 0.0113(9) Uani 1 1 d U . . H7 H 0.8612 0.5985 0.5815 0.014 Uiso 1 1 calc R . . Tb1 Tb 0.524069(8) 0.33538(2) 0.217126(12) 0.00555(11) Uani 1 1 d U . . Ag1 Ag 0.773005(14) 0.53836(4) 0.44959(2) 0.01394(13) Uani 1 1 d U . . O7 O 0.61165(13) 0.2511(4) 0.21424(17) 0.0102(7) Uani 1 1 d U . . C16 C 0.67469(18) 0.2755(5) 0.3701(3) 0.0105(8) Uani 1 1 d U . . H16 H 0.7021 0.3096 0.3394 0.013 Uiso 1 1 calc R . . N2 N 0.89102(15) 0.8738(5) 0.3884(2) 0.0105(8) Uani 1 1 d U . . H2A H 0.9046 0.9390 0.3571 0.013 Uiso 1 1 calc R . . C15 C 0.67421(19) 0.3098(5) 0.4469(3) 0.0099(9) Uani 1 1 d U . . N1 N 0.84047(16) 0.6843(5) 0.4330(2) 0.0115(8) Uani 1 1 d U . . C18 C 0.63482(18) 0.1521(5) 0.2582(3) 0.0083(9) Uani 1 1 d U . . C5 C 0.85350(18) 0.7671(6) 0.3729(3) 0.0113(9) Uani 1 1 d U . . H5 H 0.8385 0.7530 0.3258 0.014 Uiso 1 1 calc R . . C12 C 0.59298(19) 0.1605(5) 0.4660(3) 0.0099(9) Uani 1 1 d U . . H12 H 0.5669 0.1206 0.4975 0.012 Uiso 1 1 calc R . . C3 C 0.93756(18) 0.9452(5) 0.5097(3) 0.0078(8) Uani 1 1 d U . . H3 H 0.9550 1.0336 0.4921 0.009 Uiso 1 1 calc R . . O8 O 0.66042(14) 0.0390(4) 0.2353(2) 0.0181(8) Uani 1 1 d U . . C17 C 0.63301(18) 0.1892(5) 0.3412(3) 0.0086(8) Uani 1 1 d U . . N3 N 0.70825(16) 0.4031(5) 0.4890(2) 0.0113(8) Uani 1 1 d U . . C6 C 0.87301(17) 0.7379(5) 0.4908(3) 0.0090(8) Uani 1 1 d U . . C4 C 0.90380(19) 0.8603(5) 0.4632(3) 0.0086(9) Uani 1 1 d U . . O9 O 0.75492(15) 0.5868(5) 0.3013(2) 0.0247(8) Uani 1 1 d U . . H9A H 0.7316 0.6275 0.2731 0.030 Uiso 1 1 d R . . H9B H 0.7465 0.5540 0.3447 0.030 Uiso 1 1 d R . . C11 C 0.63475(18) 0.2506(6) 0.4941(3) 0.0093(8) Uani 1 1 d U . . C10 C 0.68981(19) 0.3966(6) 0.5590(3) 0.0142(9) Uani 1 1 d U . . H10 H 0.7052 0.4487 0.5992 0.017 Uiso 1 1 calc R . . O11 O 0.7971(3) 0.4622(9) 0.6822(4) 0.0832(17) Uani 1 1 d U . . H11A H 0.7711 0.4402 0.7104 0.100 Uiso 1 1 d R . . H11B H 0.8281 0.4685 0.7006 0.100 Uiso 1 1 d R . . O1 O 0.91864(13) 0.5444(4) 0.6936(2) 0.0125(7) Uani 1 1 d U . . N4 N 0.64693(17) 0.3074(5) 0.5648(2) 0.0118(8) Uani 1 1 d U . . H4A H 0.6297 0.2883 0.6055 0.014 Uiso 1 1 calc R . . O10 O 0.2500 0.2500 0.3934(9) 0.158(6) Uani 1 2 d S . . H10A H 0.2339 0.2748 0.3532 0.190 Uiso 0.50 1 d PR . . H10B H 0.2332 0.2071 0.4292 0.190 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3 0.0066(14) 0.0111(15) 0.0079(16) 0.0018(12) 0.0001(12) -0.0014(12) O6 0.0078(15) 0.0094(15) 0.0082(15) 0.0010(12) -0.0003(12) -0.0002(12) O5 0.0147(16) 0.0109(16) 0.0095(16) 0.0025(13) -0.0019(13) -0.0057(13) C14 0.0098(18) 0.0084(18) 0.0087(19) -0.0022(15) 0.0009(16) 0.0012(16) C13 0.0079(18) 0.0077(17) 0.0103(19) 0.0006(15) 0.0006(16) 0.0020(15) C2 0.0068(18) 0.0084(18) 0.0088(18) 0.0000(15) 0.0014(16) 0.0018(15) O4 0.0128(16) 0.0067(15) 0.0083(16) -0.0011(12) 0.0013(13) -0.0008(12) C1 0.0085(19) 0.009(2) 0.0063(19) 0.0012(16) 0.0042(16) -0.0009(16) O2 0.0066(14) 0.0104(15) 0.0074(15) -0.0003(12) 0.0016(12) -0.0005(12) C9 0.0057(19) 0.0113(19) 0.013(2) 0.0013(17) 0.0023(17) 0.0029(16) C8 0.0081(18) 0.0102(18) 0.0116(19) 0.0006(16) 0.0010(16) 0.0001(16) C7 0.0103(19) 0.0112(18) 0.0126(19) 0.0002(16) 0.0006(17) 0.0016(16) Tb1 0.00592(15) 0.00464(15) 0.00609(15) -0.00015(7) 0.00033(8) 0.00074(7) Ag1 0.0096(2) 0.0174(2) 0.0148(2) -0.00013(14) -0.00018(15) -0.00667(14) O7 0.0083(15) 0.0124(15) 0.0098(15) 0.0026(12) 0.0007(12) 0.0018(13) C16 0.0089(17) 0.0115(18) 0.0111(18) 0.0000(15) 0.0020(16) 0.0019(16) N2 0.0097(18) 0.0116(18) 0.0100(18) -0.0011(15) 0.0015(15) -0.0021(15) C15 0.0087(19) 0.0106(18) 0.0104(19) 0.0007(16) -0.0022(17) -0.0004(16) N1 0.0091(18) 0.0140(18) 0.0114(18) -0.0008(14) 0.0001(15) -0.0018(14) C18 0.0063(19) 0.0110(19) 0.0077(19) 0.0002(16) -0.0001(17) 0.0012(16) C5 0.0083(19) 0.016(2) 0.010(2) -0.0011(17) -0.0001(17) -0.0016(17) C12 0.0086(19) 0.0108(19) 0.0104(19) 0.0022(15) -0.0001(16) -0.0014(15) C3 0.0078(18) 0.0071(18) 0.0084(19) 0.0010(15) 0.0017(16) 0.0000(15) O8 0.0194(17) 0.0227(18) 0.0123(16) -0.0029(14) -0.0014(14) 0.0106(14) C17 0.0083(18) 0.0096(17) 0.0079(18) -0.0002(15) -0.0005(16) 0.0036(15) N3 0.0108(17) 0.0139(18) 0.0091(18) -0.0009(15) -0.0011(15) -0.0029(15) C6 0.0050(18) 0.0108(19) 0.0110(19) -0.0017(16) 0.0005(16) -0.0003(16) C4 0.0072(19) 0.0097(18) 0.009(2) 0.0002(16) 0.0005(16) 0.0028(16) O9 0.0191(18) 0.030(2) 0.0251(19) -0.0004(16) 0.0010(17) 0.0061(16) C11 0.0108(19) 0.0093(18) 0.0078(19) 0.0005(16) 0.0008(17) -0.0002(16) C10 0.013(2) 0.019(2) 0.011(2) -0.0031(17) -0.0014(17) -0.0027(18) O11 0.059(3) 0.134(4) 0.056(3) 0.006(3) 0.007(3) 0.050(3) O1 0.0108(16) 0.0090(16) 0.0177(17) 0.0027(13) -0.0038(14) -0.0005(12) N4 0.0130(19) 0.0144(18) 0.0081(18) -0.0010(15) 0.0029(15) -0.0042(15) O10 0.140(13) 0.193(17) 0.141(14) 0.000 0.000 0.035(14) _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 O3 C1 1.268(6) . ? O3 Tb1 2.312(3) 6_666 ? O6 C14 1.280(6) . ? O6 Tb1 2.489(3) . ? O6 Tb1 2.563(3) 3_645 ? O5 C14 1.255(6) . ? O5 Tb1 2.426(3) 3_645 ? C14 C13 1.491(6) . ? C14 Tb1 2.855(5) 3_645 ? C13 C12 1.392(7) . ? C13 C17 1.427(7) . ? C2 C3 1.389(7) . ? C2 C8 1.429(7) . ? C2 C1 1.505(6) . ? O4 C1 1.261(6) . ? O4 Tb1 2.330(3) 8_766 ? O2 C9 1.263(6) . ? O2 Tb1 2.312(3) 6_666 ? C9 O1 1.277(6) . ? C9 C8 1.502(7) . ? C8 C7 1.390(7) . ? C7 C6 1.393(7) . ? C7 H7 0.9300 . ? Tb1 O3 2.312(3) 6_556 ? Tb1 O2 2.312(3) 6_556 ? Tb1 O4 2.330(3) 8_745 ? Tb1 O7 2.330(3) . ? Tb1 O1 2.339(3) 8_755 ? Tb1 O5 2.426(3) 3_655 ? Tb1 O6 2.563(3) 3_655 ? Tb1 C14 2.855(5) 3_655 ? Ag1 N1 2.135(4) . ? Ag1 N3 2.125(4) . ? Ag1 H9B 1.9909 . ? O7 C18 1.294(6) . ? C16 C17 1.386(7) . ? C16 C15 1.401(7) . ? C16 H16 0.9300 . ? N2 C5 1.345(6) . ? N2 C4 1.378(6) . ? N2 H2A 0.8600 . ? C15 N3 1.393(6) . ? C15 C11 1.400(7) . ? N1 C5 1.325(6) . ? N1 C6 1.397(6) . ? C18 O8 1.233(6) . ? C18 C17 1.513(7) . ? C5 H5 0.9300 . ? C12 C11 1.400(7) . ? C12 H12 0.9300 . ? C3 C4 1.394(7) . ? C3 H3 0.9300 . ? N3 C10 1.332(6) . ? C6 C4 1.394(7) . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? C11 N4 1.386(6) . ? C10 N4 1.330(6) . ? C10 H10 0.9300 . ? O11 H11A 0.8500 . ? O11 H11B 0.8499 . ? O1 Tb1 2.339(3) 8_756 ? N4 H4A 0.8600 . ? O10 H10A 0.8499 . ? O10 H10B 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 C1 O3 Tb1 125.9(3) . 6_666 ? C14 O6 Tb1 135.7(3) . . ? C14 O6 Tb1 89.5(3) . 3_645 ? Tb1 O6 Tb1 131.01(13) . 3_645 ? C14 O5 Tb1 96.5(3) . 3_645 ? O5 C14 O6 120.4(4) . . ? O5 C14 C13 120.7(4) . . ? O6 C14 C13 118.9(4) . . ? O5 C14 Tb1 57.6(2) . 3_645 ? O6 C14 Tb1 63.9(2) . 3_645 ? C13 C14 Tb1 167.2(3) . 3_645 ? C12 C13 C17 121.3(4) . . ? C12 C13 C14 119.6(4) . . ? C17 C13 C14 119.1(4) . . ? C3 C2 C8 120.4(4) . . ? C3 C2 C1 114.7(4) . . ? C8 C2 C1 124.9(4) . . ? C1 O4 Tb1 136.2(3) . 8_766 ? O4 C1 O3 124.2(4) . . ? O4 C1 C2 116.3(4) . . ? O3 C1 C2 119.3(4) . . ? C9 O2 Tb1 129.4(3) . 6_666 ? O2 C9 O1 123.0(4) . . ? O2 C9 C8 120.3(4) . . ? O1 C9 C8 116.7(4) . . ? C7 C8 C2 120.3(4) . . ? C7 C8 C9 117.2(4) . . ? C2 C8 C9 122.6(4) . . ? C6 C7 C8 118.8(4) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? O3 Tb1 O2 74.05(11) 6_556 6_556 ? O3 Tb1 O4 151.47(12) 6_556 8_745 ? O2 Tb1 O4 94.42(11) 6_556 8_745 ? O3 Tb1 O7 98.53(11) 6_556 . ? O2 Tb1 O7 144.74(11) 6_556 . ? O4 Tb1 O7 75.67(11) 8_745 . ? O3 Tb1 O1 86.74(12) 6_556 8_755 ? O2 Tb1 O1 142.15(11) 6_556 8_755 ? O4 Tb1 O1 115.81(12) 8_745 8_755 ? O7 Tb1 O1 69.12(11) . 8_755 ? O3 Tb1 O5 127.67(11) 6_556 3_655 ? O2 Tb1 O5 82.65(11) 6_556 3_655 ? O4 Tb1 O5 74.68(11) 8_745 3_655 ? O7 Tb1 O5 125.08(11) . 3_655 ? O1 Tb1 O5 84.03(12) 8_755 3_655 ? O3 Tb1 O6 77.57(11) 6_556 . ? O2 Tb1 O6 73.16(11) 6_556 . ? O4 Tb1 O6 74.10(11) 8_745 . ? O7 Tb1 O6 71.58(11) . . ? O1 Tb1 O6 134.67(11) 8_755 . ? O5 Tb1 O6 138.43(11) 3_655 . ? O3 Tb1 O6 76.00(11) 6_556 3_655 ? O2 Tb1 O6 72.26(11) 6_556 3_655 ? O4 Tb1 O6 126.05(11) 8_745 3_655 ? O7 Tb1 O6 140.56(11) . 3_655 ? O1 Tb1 O6 71.58(11) 8_755 3_655 ? O5 Tb1 O6 52.22(11) 3_655 3_655 ? O6 Tb1 O6 140.95(2) . 3_655 ? O3 Tb1 C14 101.80(13) 6_556 3_655 ? O2 Tb1 C14 73.27(12) 6_556 3_655 ? O4 Tb1 C14 99.53(12) 8_745 3_655 ? O7 Tb1 C14 141.20(12) . 3_655 ? O1 Tb1 C14 79.40(12) 8_755 3_655 ? O5 Tb1 C14 25.90(13) 3_655 3_655 ? O6 Tb1 C14 145.17(12) . 3_655 ? O6 Tb1 C14 26.63(12) 3_655 3_655 ? N1 Ag1 N3 168.61(16) . . ? N1 Ag1 H9B 95.7 . . ? N3 Ag1 H9B 95.1 . . ? C18 O7 Tb1 128.3(3) . . ? C17 C16 C15 117.9(4) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C5 N2 C4 107.9(4) . . ? C5 N2 H2A 126.1 . . ? C4 N2 H2A 126.1 . . ? N3 C15 C16 129.9(4) . . ? N3 C15 C11 108.9(4) . . ? C16 C15 C11 121.2(4) . . ? C5 N1 C6 106.0(4) . . ? C5 N1 Ag1 128.5(3) . . ? C6 N1 Ag1 124.1(3) . . ? O8 C18 O7 123.4(5) . . ? O8 C18 C17 120.2(4) . . ? O7 C18 C17 116.2(4) . . ? N1 C5 N2 111.8(4) . . ? N1 C5 H5 124.1 . . ? N2 C5 H5 124.1 . . ? C13 C12 C11 117.3(4) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C2 C3 C4 118.1(4) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C16 C17 C13 120.6(4) . . ? C16 C17 C18 116.9(4) . . ? C13 C17 C18 122.4(4) . . ? C10 N3 C15 105.3(4) . . ? C10 N3 Ag1 127.0(3) . . ? C15 N3 Ag1 127.6(3) . . ? C7 C6 C4 120.3(4) . . ? C7 C6 N1 131.2(4) . . ? C4 C6 N1 108.4(4) . . ? N2 C4 C6 105.9(4) . . ? N2 C4 C3 132.5(4) . . ? C6 C4 C3 121.6(4) . . ? H9A O9 H9B 120.0 . . ? N4 C11 C15 105.2(4) . . ? N4 C11 C12 133.3(4) . . ? C15 C11 C12 121.5(4) . . ? N3 C10 N4 112.5(4) . . ? N3 C10 H10 123.7 . . ? N4 C10 H10 123.7 . . ? H11A O11 H11B 120.0 . . ? C9 O1 Tb1 133.0(3) . 8_756 ? C10 N4 C11 108.1(4) . . ? C10 N4 H4A 126.0 . . ? C11 N4 H4A 126.0 . . ? H10A O10 H10B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O5 C14 O6 12.4(5) 3_645 . . . ? Tb1 O5 C14 C13 -165.1(4) 3_645 . . . ? Tb1 O6 C14 O5 146.9(3) . . . . ? Tb1 O6 C14 O5 -11.6(4) 3_645 . . . ? Tb1 O6 C14 C13 -35.7(6) . . . . ? Tb1 O6 C14 C13 165.9(4) 3_645 . . . ? Tb1 O6 C14 Tb1 158.5(4) . . . 3_645 ? O5 C14 C13 C12 -37.2(7) . . . . ? O6 C14 C13 C12 145.4(4) . . . . ? Tb1 C14 C13 C12 -115.6(14) 3_645 . . . ? O5 C14 C13 C17 145.1(5) . . . . ? O6 C14 C13 C17 -32.4(6) . . . . ? Tb1 C14 C13 C17 66.7(16) 3_645 . . . ? Tb1 O4 C1 O3 -48.8(7) 8_766 . . . ? Tb1 O4 C1 C2 136.6(4) 8_766 . . . ? Tb1 O3 C1 O4 89.7(5) 6_666 . . . ? Tb1 O3 C1 C2 -95.8(5) 6_666 . . . ? C3 C2 C1 O4 50.3(6) . . . . ? C8 C2 C1 O4 -130.8(5) . . . . ? C3 C2 C1 O3 -124.6(5) . . . . ? C8 C2 C1 O3 54.3(6) . . . . ? Tb1 O2 C9 O1 86.3(5) 6_666 . . . ? Tb1 O2 C9 C8 -93.5(5) 6_666 . . . ? C3 C2 C8 C7 -4.5(7) . . . . ? C1 C2 C8 C7 176.7(4) . . . . ? C3 C2 C8 C9 175.3(4) . . . . ? C1 C2 C8 C9 -3.5(7) . . . . ? O2 C9 C8 C7 -151.3(4) . . . . ? O1 C9 C8 C7 28.8(6) . . . . ? O2 C9 C8 C2 28.8(7) . . . . ? O1 C9 C8 C2 -151.0(4) . . . . ? C2 C8 C7 C6 3.1(7) . . . . ? C9 C8 C7 C6 -176.8(4) . . . . ? C14 O6 Tb1 O3 -24.4(4) . . . 6_556 ? Tb1 O6 Tb1 O3 126.53(18) 3_645 . . 6_556 ? C14 O6 Tb1 O2 -101.3(4) . . . 6_556 ? Tb1 O6 Tb1 O2 49.67(17) 3_645 . . 6_556 ? C14 O6 Tb1 O4 159.0(4) . . . 8_745 ? Tb1 O6 Tb1 O4 -50.12(17) 3_645 . . 8_745 ? C14 O6 Tb1 O7 79.1(4) . . . . ? Tb1 O6 Tb1 O7 -129.96(19) 3_645 . . . ? C14 O6 Tb1 O1 48.2(5) . . . 8_755 ? Tb1 O6 Tb1 O1 -160.91(15) 3_645 . . 8_755 ? C14 O6 Tb1 O5 -158.4(4) . . . 3_655 ? Tb1 O6 Tb1 O5 -7.5(3) 3_645 . . 3_655 ? C14 O6 Tb1 O6 -72.7(4) . . . 3_655 ? Tb1 O6 Tb1 O6 78.2(2) 3_645 . . 3_655 ? C14 O6 Tb1 C14 -117.3(4) . . . 3_655 ? Tb1 O6 Tb1 C14 33.7(3) 3_645 . . 3_655 ? O3 Tb1 O7 C18 55.3(4) 6_556 . . . ? O2 Tb1 O7 C18 -19.1(5) 6_556 . . . ? O4 Tb1 O7 C18 -96.2(4) 8_745 . . . ? O1 Tb1 O7 C18 138.5(4) 8_755 . . . ? O5 Tb1 O7 C18 -155.3(3) 3_655 . . . ? O6 Tb1 O7 C18 -18.5(4) . . . . ? O6 Tb1 O7 C18 133.6(3) 3_655 . . . ? C14 Tb1 O7 C18 176.4(3) 3_655 . . . ? C17 C16 C15 N3 -174.4(5) . . . . ? C17 C16 C15 C11 4.0(7) . . . . ? N3 Ag1 N1 C5 -154.1(7) . . . . ? N3 Ag1 N1 C6 10.3(10) . . . . ? Tb1 O7 C18 O8 128.5(4) . . . . ? Tb1 O7 C18 C17 -56.5(5) . . . . ? C6 N1 C5 N2 -1.9(5) . . . . ? Ag1 N1 C5 N2 164.7(3) . . . . ? C4 N2 C5 N1 0.3(5) . . . . ? C17 C13 C12 C11 2.4(7) . . . . ? C14 C13 C12 C11 -175.2(4) . . . . ? C8 C2 C3 C4 -0.5(7) . . . . ? C1 C2 C3 C4 178.4(4) . . . . ? C15 C16 C17 C13 -2.0(7) . . . . ? C15 C16 C17 C18 -179.3(4) . . . . ? C12 C13 C17 C16 -1.2(7) . . . . ? C14 C13 C17 C16 176.5(4) . . . . ? C12 C13 C17 C18 175.9(4) . . . . ? C14 C13 C17 C18 -6.4(7) . . . . ? O8 C18 C17 C16 83.6(6) . . . . ? O7 C18 C17 C16 -91.5(5) . . . . ? O8 C18 C17 C13 -93.6(6) . . . . ? O7 C18 C17 C13 91.2(5) . . . . ? C16 C15 N3 C10 179.6(5) . . . . ? C11 C15 N3 C10 1.0(5) . . . . ? C16 C15 N3 Ag1 2.9(7) . . . . ? C11 C15 N3 Ag1 -175.7(3) . . . . ? N1 Ag1 N3 C10 7.3(11) . . . . ? N1 Ag1 N3 C15 -176.7(7) . . . . ? C8 C7 C6 C4 3.3(7) . . . . ? C8 C7 C6 N1 178.4(5) . . . . ? C5 N1 C6 C7 -172.8(5) . . . . ? Ag1 N1 C6 C7 19.8(7) . . . . ? C5 N1 C6 C4 2.8(5) . . . . ? Ag1 N1 C6 C4 -164.6(3) . . . . ? C5 N2 C4 C6 1.4(5) . . . . ? C5 N2 C4 C3 -176.1(5) . . . . ? C7 C6 C4 N2 173.5(4) . . . . ? N1 C6 C4 N2 -2.6(5) . . . . ? C7 C6 C4 C3 -8.6(7) . . . . ? N1 C6 C4 C3 175.3(4) . . . . ? C2 C3 C4 N2 -175.7(5) . . . . ? C2 C3 C4 C6 7.0(7) . . . . ? N3 C15 C11 N4 -1.4(5) . . . . ? C16 C15 C11 N4 179.8(4) . . . . ? N3 C15 C11 C12 175.9(4) . . . . ? C16 C15 C11 C12 -2.8(7) . . . . ? C13 C12 C11 N4 176.0(5) . . . . ? C13 C12 C11 C15 -0.5(7) . . . . ? C15 N3 C10 N4 -0.1(6) . . . . ? Ag1 N3 C10 N4 176.6(3) . . . . ? O2 C9 O1 Tb1 -68.0(6) . . . 8_756 ? C8 C9 O1 Tb1 111.9(4) . . . 8_756 ? N3 C10 N4 C11 -0.8(6) . . . . ? C15 C11 N4 C10 1.4(5) . . . . ? C12 C11 N4 C10 -175.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.737 _refine_diff_density_min -2.586 _refine_diff_density_rms 0.145 # Attachment 'dt-art-05-2010-000579-File006-v1-0.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 735031' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Ag Ce N4 O10' _chemical_formula_weight 692.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 6.9529(14) _cell_length_b 22.109(4) _cell_length_c 11.875(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1825.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6253 _cell_measurement_theta_min 2.517 _cell_measurement_theta_max 27.880 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 3.611 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7610 _exptl_absorpt_correction_T_max 0.8690 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11206 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3140 _reflns_number_gt 3081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+5.9248P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.495(15) _refine_ls_number_reflns 3140 _refine_ls_number_parameters 325 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.137 _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 Ce1 Ce 0.67310(3) 1.002950(10) 0.16801(3) 0.00416(7) Uani 1 1 d . . . Ag1 Ag 0.24144(4) 0.840687(14) 0.15498(3) 0.00859(8) Uani 1 1 d . . . O1 O 0.9733(4) 1.08389(13) 0.1792(3) 0.0098(7) Uani 1 1 d . . . O2 O 0.8451(5) 1.04849(15) 0.3362(3) 0.0114(8) Uani 1 1 d . . . O3 O 1.2384(5) 1.04868(15) 0.4848(3) 0.0098(8) Uani 1 1 d . . . O4 O 1.0158(5) 1.06921(15) 0.6105(3) 0.0102(7) Uani 1 1 d . . . O5 O 0.6757(5) 0.93666(14) 0.3540(3) 0.0062(7) Uani 1 1 d . . . O6 O 0.5512(5) 0.89695(15) 0.2006(3) 0.0100(7) Uani 1 1 d . . . O7 O 0.3466(5) 0.92851(15) 0.4974(3) 0.0071(7) Uani 1 1 d . . . O8 O 0.4614(5) 0.88604(13) 0.6508(3) 0.0117(7) Uani 1 1 d . . . O9 O 0.3665(6) 1.0184(2) 0.2784(3) 0.0169(9) Uani 1 1 d D . . H9A H 0.350(7) 1.024(3) 0.3487(11) 0.020 Uiso 1 1 d D . . H9B H 0.275(5) 1.029(3) 0.236(3) 0.020 Uiso 1 1 d D . . O10 O 0.3603(6) 0.99111(19) 0.0511(4) 0.0136(9) Uani 1 1 d D . . H10A H 0.337(7) 1.008(2) -0.012(3) 0.016 Uiso 1 1 d D . . H10B H 0.267(5) 0.972(2) 0.080(4) 0.016 Uiso 1 1 d D . . N1 N 0.9937(7) 1.3124(2) 0.3318(4) 0.0069(9) Uani 1 1 d D . . H1 H 0.978(8) 1.332(2) 0.271(2) 0.008 Uiso 1 1 d D . . N2 N 1.1069(6) 1.30697(18) 0.5080(3) 0.0068(8) Uani 1 1 d . . . N3 N 0.5755(6) 0.66977(17) 0.3088(3) 0.0058(8) Uani 1 1 d . . . N4 N 0.4804(6) 0.6609(2) 0.4874(4) 0.0074(9) Uani 1 1 d D . . H4 H 0.467(8) 0.643(2) 0.550(2) 0.009 Uiso 1 1 d D . . C1 C 0.9400(7) 1.0883(2) 0.2833(4) 0.0079(10) Uani 1 1 d . . . C2 C 1.0000(8) 1.1439(2) 0.3472(4) 0.0059(11) Uani 1 1 d U . . C3 C 0.9731(7) 1.1991(2) 0.2950(4) 0.0062(10) Uani 1 1 d . . . H3 H 0.9308 1.2013 0.2208 0.007 Uiso 1 1 calc R . . C4 C 1.0108(7) 1.2513(2) 0.3561(4) 0.0047(9) Uani 1 1 d U . . C5 C 1.0545(7) 1.3425(2) 0.4242(5) 0.0070(10) Uani 1 1 d . . . H5 H 1.0591 1.3845 0.4283 0.008 Uiso 1 1 calc R . . C6 C 1.0798(7) 1.2485(2) 0.4673(4) 0.0059(10) Uani 1 1 d U . . C7 C 1.1059(7) 1.1924(2) 0.5208(4) 0.0068(10) Uani 1 1 d . . . H7 H 1.1501 1.1901 0.5946 0.008 Uiso 1 1 calc R . . C8 C 1.0636(7) 1.1405(2) 0.4600(4) 0.0051(9) Uani 1 1 d . . . C9 C 1.1043(7) 1.0816(2) 0.5212(4) 0.0047(9) Uani 1 1 d U . . C10 C 0.5900(7) 0.8940(2) 0.3057(4) 0.0069(10) Uani 1 1 d . . . C11 C 0.5458(7) 0.8352(2) 0.3646(5) 0.0080(10) Uani 1 1 d . . . C12 C 0.5770(7) 0.7833(2) 0.3019(4) 0.0055(9) Uani 1 1 d . . . H12 H 0.6151 0.7858 0.2270 0.007 Uiso 1 1 calc R . . C13 C 0.5501(7) 0.7269(2) 0.3534(4) 0.0062(9) Uani 1 1 d . . . C14 C 0.5338(7) 0.6321(2) 0.3920(4) 0.0060(10) Uani 1 1 d . . . H14 H 0.5406 0.5902 0.3856 0.007 Uiso 1 1 calc R . . C15 C 0.4900(7) 0.7228(2) 0.4656(4) 0.0052(9) Uani 1 1 d . . . C16 C 0.4562(7) 0.7744(2) 0.5282(4) 0.0079(10) Uani 1 1 d . . . H16 H 0.4155 0.7717 0.6026 0.009 Uiso 1 1 calc R . . C17 C 0.4838(8) 0.8302(3) 0.4782(4) 0.0067(12) Uani 1 1 d . . . C18 C 0.4283(7) 0.8852(2) 0.5452(4) 0.0084(10) 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 Ce1 0.00634(11) 0.00289(11) 0.00326(11) 0.00011(11) 0.00016(12) -0.00043(8) Ag1 0.00931(15) 0.00946(16) 0.00701(15) -0.00025(17) 0.00161(18) -0.00088(12) O1 0.0164(16) 0.0102(15) 0.0028(18) 0.0005(15) 0.0000(14) -0.0008(12) O2 0.0174(19) 0.0080(17) 0.0088(18) 0.0008(14) -0.0026(15) -0.0067(14) O3 0.0124(19) 0.0064(18) 0.0105(19) 0.0002(14) -0.0012(15) 0.0021(15) O4 0.0148(18) 0.0086(18) 0.0072(17) 0.0018(13) 0.0032(14) -0.0003(14) O5 0.0068(18) 0.0030(16) 0.0087(17) -0.0001(14) -0.0016(14) -0.0039(14) O6 0.0143(18) 0.0111(17) 0.0046(17) 0.0003(13) -0.0028(13) -0.0035(13) O7 0.0081(16) 0.0048(17) 0.0084(18) 0.0009(14) 0.0015(14) -0.0007(13) O8 0.0245(17) 0.0062(15) 0.0045(18) 0.0001(15) 0.0006(18) 0.0027(12) O9 0.012(2) 0.029(2) 0.009(2) 0.0013(19) 0.0037(16) 0.008(2) O10 0.0113(19) 0.018(2) 0.012(2) 0.0062(17) -0.0009(15) -0.0049(18) N1 0.007(2) 0.006(2) 0.008(2) 0.0010(18) 0.0011(18) 0.0008(18) N2 0.006(2) 0.006(2) 0.008(2) 0.0007(17) 0.0016(17) -0.0007(16) N3 0.008(2) 0.0023(19) 0.007(2) -0.0016(15) 0.0014(16) 0.0000(16) N4 0.008(2) 0.006(2) 0.009(2) 0.0010(17) 0.0007(17) 0.0017(18) C1 0.006(2) 0.006(2) 0.012(3) 0.000(2) -0.0027(19) 0.0026(19) C2 0.0055(14) 0.0063(14) 0.0060(13) 0.0006(9) 0.0009(9) -0.0009(9) C3 0.004(2) 0.006(2) 0.009(2) -0.001(2) -0.0017(19) -0.0026(18) C4 0.0045(12) 0.0045(12) 0.0050(12) 0.0011(9) 0.0010(9) 0.0007(9) C5 0.007(2) 0.004(2) 0.010(2) -0.001(2) 0.003(2) -0.0009(19) C6 0.0051(13) 0.0060(13) 0.0066(13) -0.0003(9) 0.0004(9) -0.0001(9) C7 0.005(2) 0.011(3) 0.005(2) 0.0012(19) -0.0001(19) 0.0005(19) C8 0.004(2) 0.006(2) 0.005(2) -0.0006(19) 0.0016(18) -0.0023(19) C9 0.0049(12) 0.0048(12) 0.0046(12) -0.0007(9) -0.0010(9) -0.0014(9) C10 0.006(2) 0.007(2) 0.007(2) 0.0034(19) 0.0023(19) 0.0042(19) C11 0.004(2) 0.006(2) 0.014(3) -0.001(2) -0.004(2) -0.0015(19) C12 0.006(2) 0.008(2) 0.003(2) 0.0039(19) 0.0000(18) -0.0012(19) C13 0.006(2) 0.005(2) 0.008(2) -0.0020(19) -0.0017(19) 0.0011(18) C14 0.005(2) 0.006(2) 0.007(3) 0.0022(18) -0.0027(19) 0.001(2) C15 0.004(2) 0.002(2) 0.009(2) 0.001(2) -0.0020(19) -0.0009(19) C16 0.002(2) 0.014(3) 0.008(2) 0.000(2) -0.0029(19) 0.002(2) C17 0.006(2) 0.010(3) 0.004(3) 0.000(2) -0.0020(19) 0.001(2) C18 0.004(2) 0.009(2) 0.012(3) 0.001(2) 0.0001(19) -0.0025(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O6 2.522(3) . ? Ce1 O9 2.526(4) . ? Ce1 O3 2.533(3) 2_774 ? Ce1 O7 2.534(3) 2_674 ? Ce1 O2 2.536(4) . ? Ce1 O10 2.593(4) . ? Ce1 O8 2.634(3) 2_674 ? Ce1 O5 2.651(3) . ? Ce1 O1 2.752(3) . ? Ce1 O4 2.773(3) 2_774 ? Ce1 C18 2.957(5) 2_674 ? Ce1 C10 2.967(5) . ? Ag1 N2 2.171(4) 4_644 ? Ag1 N3 2.173(4) 3_465 ? Ag1 O6 2.545(3) . ? O1 C1 1.261(6) . ? O2 C1 1.268(6) . ? O3 C9 1.259(6) . ? O3 Ce1 2.533(3) 2_775 ? O4 C9 1.256(6) . ? O4 Ce1 2.773(3) 2_775 ? O5 C10 1.254(6) . ? O6 C10 1.278(6) . ? O7 C18 1.251(6) . ? O7 Ce1 2.534(3) 2_675 ? O8 C18 1.275(6) . ? O8 Ce1 2.634(3) 2_675 ? O9 H9A 0.850(10) . ? O9 H9B 0.851(10) . ? O10 H10A 0.854(10) . ? O10 H10B 0.854(10) . ? N1 C5 1.352(7) . ? N1 C4 1.385(7) . ? N1 H1 0.846(10) . ? N2 C5 1.319(6) . ? N2 C6 1.393(6) . ? N2 Ag1 2.171(4) 4_655 ? N3 C14 1.325(6) . ? N3 C13 1.381(6) . ? N3 Ag1 2.173(4) 3_565 ? N4 C14 1.351(6) . ? N4 C15 1.393(7) . ? N4 H4 0.848(10) . ? C1 C2 1.503(7) . ? C2 C3 1.383(7) . ? C2 C8 1.412(7) . ? C3 C4 1.388(7) . ? C3 H3 0.9300 . ? C4 C6 1.406(7) . ? C5 H5 0.9300 . ? C6 C7 1.407(7) . ? C7 C8 1.388(7) . ? C7 H7 0.9300 . ? C8 C9 1.519(6) . ? C9 Ce1 2.987(5) 2_775 ? C10 C11 1.509(7) . ? C11 C12 1.385(7) . ? C11 C17 1.420(7) . ? C12 C13 1.401(7) . ? C12 H12 0.9300 . ? C13 C15 1.400(7) . ? C14 H14 0.9300 . ? C15 C16 1.382(7) . ? C16 C17 1.382(7) . ? C16 H16 0.9300 . ? C17 C18 1.502(7) . ? C18 Ce1 2.957(5) 2_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ce1 O9 76.24(13) . . ? O6 Ce1 O3 78.16(11) . 2_774 ? O9 Ce1 O3 135.38(14) . 2_774 ? O6 Ce1 O7 131.31(10) . 2_674 ? O9 Ce1 O7 106.76(12) . 2_674 ? O3 Ce1 O7 66.16(11) 2_774 2_674 ? O6 Ce1 O2 113.99(11) . . ? O9 Ce1 O2 86.32(13) . . ? O3 Ce1 O2 137.79(13) 2_774 . ? O7 Ce1 O2 114.70(11) 2_674 . ? O6 Ce1 O10 72.93(12) . . ? O9 Ce1 O10 65.40(11) . . ? O3 Ce1 O10 72.45(13) 2_774 . ? O7 Ce1 O10 65.59(11) 2_674 . ? O2 Ce1 O10 148.99(13) . . ? O6 Ce1 O8 139.32(10) . 2_674 ? O9 Ce1 O8 67.34(13) . 2_674 ? O3 Ce1 O8 116.08(11) 2_774 2_674 ? O7 Ce1 O8 50.34(11) 2_674 2_674 ? O2 Ce1 O8 81.86(11) . 2_674 ? O10 Ce1 O8 75.82(12) . 2_674 ? O6 Ce1 O5 50.26(10) . . ? O9 Ce1 O5 69.39(12) . . ? O3 Ce1 O5 117.71(10) 2_774 . ? O7 Ce1 O5 175.78(11) 2_674 . ? O2 Ce1 O5 63.91(10) . . ? O10 Ce1 O5 113.33(12) . . ? O8 Ce1 O5 125.59(11) 2_674 . ? O6 Ce1 O1 148.39(10) . . ? O9 Ce1 O1 121.81(13) . . ? O3 Ce1 O1 98.64(11) 2_774 . ? O7 Ce1 O1 71.99(10) 2_674 . ? O2 Ce1 O1 49.18(11) . . ? O10 Ce1 O1 136.66(11) . . ? O8 Ce1 O1 70.56(10) 2_674 . ? O5 Ce1 O1 108.31(10) . . ? O6 Ce1 O4 76.43(11) . 2_774 ? O9 Ce1 O4 149.75(12) . 2_774 ? O3 Ce1 O4 48.68(11) 2_774 2_774 ? O7 Ce1 O4 100.92(10) 2_674 2_774 ? O2 Ce1 O4 93.12(11) . 2_774 ? O10 Ce1 O4 117.66(12) . 2_774 ? O8 Ce1 O4 142.54(11) 2_674 2_774 ? O5 Ce1 O4 83.21(10) . 2_774 ? O1 Ce1 O4 78.14(9) . 2_774 ? O6 Ce1 C18 140.62(12) . 2_674 ? O9 Ce1 C18 86.64(14) . 2_674 ? O3 Ce1 C18 90.66(12) 2_774 2_674 ? O7 Ce1 C18 24.83(12) 2_674 2_674 ? O2 Ce1 C18 99.71(12) . 2_674 ? O10 Ce1 C18 67.69(13) . 2_674 ? O8 Ce1 C18 25.54(12) 2_674 2_674 ? O5 Ce1 C18 151.04(12) . 2_674 ? O1 Ce1 C18 70.17(12) . 2_674 ? O4 Ce1 C18 123.10(12) 2_774 2_674 ? O6 Ce1 C10 25.30(12) . . ? O9 Ce1 C10 70.09(14) . . ? O3 Ce1 C10 98.91(12) 2_774 . ? O7 Ce1 C10 156.25(12) 2_674 . ? O2 Ce1 C10 88.86(12) . . ? O10 Ce1 C10 92.86(13) . . ? O8 Ce1 C10 136.86(12) 2_674 . ? O5 Ce1 C10 24.99(12) . . ? O1 Ce1 C10 130.44(12) . . ? O4 Ce1 C10 79.66(12) 2_774 . ? C18 Ce1 C10 154.71(12) 2_674 . ? N2 Ag1 N3 153.78(14) 4_644 3_465 ? N2 Ag1 O6 85.88(13) 4_644 . ? N3 Ag1 O6 108.80(13) 3_465 . ? C1 O1 Ce1 87.7(3) . . ? C1 O2 Ce1 97.5(3) . . ? C9 O3 Ce1 98.3(3) . 2_775 ? C9 O4 Ce1 87.2(3) . 2_775 ? C10 O5 Ce1 91.8(3) . . ? C10 O6 Ce1 97.2(3) . . ? C10 O6 Ag1 111.2(3) . . ? Ce1 O6 Ag1 134.90(14) . . ? C18 O7 Ce1 96.9(3) . 2_675 ? C18 O8 Ce1 91.5(3) . 2_675 ? Ce1 O9 H9A 130(3) . . ? Ce1 O9 H9B 111(3) . . ? H9A O9 H9B 116(2) . . ? Ce1 O10 H10A 126(3) . . ? Ce1 O10 H10B 118(3) . . ? H10A O10 H10B 116(2) . . ? C5 N1 C4 106.5(4) . . ? C5 N1 H1 119(4) . . ? C4 N1 H1 133(4) . . ? C5 N2 C6 104.6(4) . . ? C5 N2 Ag1 122.4(3) . 4_655 ? C6 N2 Ag1 131.6(3) . 4_655 ? C14 N3 C13 105.1(4) . . ? C14 N3 Ag1 132.6(3) . 3_565 ? C13 N3 Ag1 119.2(3) . 3_565 ? C14 N4 C15 107.1(4) . . ? C14 N4 H4 123(4) . . ? C15 N4 H4 129(4) . . ? O1 C1 O2 121.8(4) . . ? O1 C1 C2 120.6(4) . . ? O2 C1 C2 117.5(5) . . ? O1 C1 Ce1 67.3(2) . . ? O2 C1 Ce1 57.5(2) . . ? C2 C1 Ce1 157.3(3) . . ? C3 C2 C8 121.0(5) . . ? C3 C2 C1 117.2(5) . . ? C8 C2 C1 121.5(4) . . ? C2 C3 C4 118.3(5) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 N1 133.2(5) . . ? C3 C4 C6 121.3(5) . . ? N1 C4 C6 105.6(5) . . ? N2 C5 N1 114.0(4) . . ? N2 C5 H5 123.0 . . ? N1 C5 H5 123.0 . . ? N2 C6 C4 109.4(4) . . ? N2 C6 C7 130.1(4) . . ? C4 C6 C7 120.5(5) . . ? C8 C7 C6 117.8(4) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C2 121.1(5) . . ? C7 C8 C9 114.8(4) . . ? C2 C8 C9 123.9(4) . . ? O4 C9 O3 121.8(4) . . ? O4 C9 C8 120.0(4) . . ? O3 C9 C8 117.9(4) . . ? O4 C9 Ce1 68.0(3) . 2_775 ? O3 C9 Ce1 57.0(2) . 2_775 ? C8 C9 Ce1 155.9(3) . 2_775 ? O5 C10 O6 120.6(4) . . ? O5 C10 C11 122.2(4) . . ? O6 C10 C11 117.0(4) . . ? O5 C10 Ce1 63.2(2) . . ? O6 C10 Ce1 57.5(2) . . ? C11 C10 Ce1 174.2(3) . . ? C12 C11 C17 119.7(5) . . ? C12 C11 C10 115.7(5) . . ? C17 C11 C10 124.6(5) . . ? C11 C12 C13 118.7(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N3 C13 C15 110.1(4) . . ? N3 C13 C12 129.0(4) . . ? C15 C13 C12 120.9(5) . . ? N3 C14 N4 112.9(4) . . ? N3 C14 H14 123.6 . . ? N4 C14 H14 123.6 . . ? C16 C15 N4 134.7(5) . . ? C16 C15 C13 120.6(5) . . ? N4 C15 C13 104.7(4) . . ? C15 C16 C17 118.9(5) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C11 121.2(5) . . ? C16 C17 C18 117.3(5) . . ? C11 C17 C18 121.3(5) . . ? O7 C18 O8 121.1(4) . . ? O7 C18 C17 119.7(5) . . ? O8 C18 C17 119.2(4) . . ? O7 C18 Ce1 58.3(2) . 2_675 ? O8 C18 Ce1 62.9(2) . 2_675 ? C17 C18 Ce1 177.1(4) . 2_675 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Ce1 O1 C1 -78.5(3) . . . . ? O9 Ce1 O1 C1 39.8(3) . . . . ? O3 Ce1 O1 C1 -159.9(3) 2_774 . . . ? O7 Ce1 O1 C1 138.7(3) 2_674 . . . ? O2 Ce1 O1 C1 -10.7(2) . . . . ? O10 Ce1 O1 C1 126.6(3) . . . . ? O8 Ce1 O1 C1 85.4(3) 2_674 . . . ? O5 Ce1 O1 C1 -36.8(3) . . . . ? O4 Ce1 O1 C1 -115.5(3) 2_774 . . . ? C18 Ce1 O1 C1 112.5(3) 2_674 . . . ? C10 Ce1 O1 C1 -50.3(3) . . . . ? O6 Ce1 O2 C1 158.7(3) . . . . ? O9 Ce1 O2 C1 -128.2(3) . . . . ? O3 Ce1 O2 C1 59.7(3) 2_774 . . . ? O7 Ce1 O2 C1 -21.4(3) 2_674 . . . ? O10 Ce1 O2 C1 -104.6(3) . . . . ? O8 Ce1 O2 C1 -60.5(3) 2_674 . . . ? O5 Ce1 O2 C1 163.0(3) . . . . ? O1 Ce1 O2 C1 10.7(3) . . . . ? O4 Ce1 O2 C1 82.1(3) 2_774 . . . ? C18 Ce1 O2 C1 -42.2(3) 2_674 . . . ? C10 Ce1 O2 C1 161.7(3) . . . . ? O6 Ce1 O5 C10 -2.1(3) . . . . ? O9 Ce1 O5 C10 86.9(3) . . . . ? O3 Ce1 O5 C10 -44.5(3) 2_774 . . . ? O7 Ce1 O5 C10 111.5(14) 2_674 . . . ? O2 Ce1 O5 C10 -176.9(3) . . . . ? O10 Ce1 O5 C10 37.2(3) . . . . ? O8 Ce1 O5 C10 126.1(3) 2_674 . . . ? O1 Ce1 O5 C10 -155.2(3) . . . . ? O4 Ce1 O5 C10 -80.1(3) 2_774 . . . ? C18 Ce1 O5 C10 122.9(3) 2_674 . . . ? O9 Ce1 O6 C10 -72.4(3) . . . . ? O3 Ce1 O6 C10 144.5(3) 2_774 . . . ? O7 Ce1 O6 C10 -172.8(3) 2_674 . . . ? O2 Ce1 O6 C10 7.2(3) . . . . ? O10 Ce1 O6 C10 -140.5(3) . . . . ? O8 Ce1 O6 C10 -99.1(3) 2_674 . . . ? O5 Ce1 O6 C10 2.1(3) . . . . ? O1 Ce1 O6 C10 57.2(4) . . . . ? O4 Ce1 O6 C10 94.5(3) 2_774 . . . ? C18 Ce1 O6 C10 -139.2(3) 2_674 . . . ? O9 Ce1 O6 Ag1 57.49(19) . . . . ? O3 Ce1 O6 Ag1 -85.6(2) 2_774 . . . ? O7 Ce1 O6 Ag1 -42.9(2) 2_674 . . . ? O2 Ce1 O6 Ag1 137.05(18) . . . . ? O10 Ce1 O6 Ag1 -10.59(19) . . . . ? O8 Ce1 O6 Ag1 30.8(3) 2_674 . . . ? O5 Ce1 O6 Ag1 132.0(2) . . . . ? O1 Ce1 O6 Ag1 -172.89(15) . . . . ? O4 Ce1 O6 Ag1 -135.6(2) 2_774 . . . ? C18 Ce1 O6 Ag1 -9.3(3) 2_674 . . . ? C10 Ce1 O6 Ag1 129.9(4) . . . . ? N2 Ag1 O6 C10 -138.0(3) 4_644 . . . ? N3 Ag1 O6 C10 19.8(3) 3_465 . . . ? N2 Ag1 O6 Ce1 96.8(2) 4_644 . . . ? N3 Ag1 O6 Ce1 -105.5(2) 3_465 . . . ? Ce1 O1 C1 O2 19.3(4) . . . . ? Ce1 O1 C1 C2 -156.1(4) . . . . ? Ce1 O2 C1 O1 -21.2(5) . . . . ? Ce1 O2 C1 C2 154.4(4) . . . . ? O6 Ce1 C1 O1 131.5(2) . . . . ? O9 Ce1 C1 O1 -146.2(3) . . . . ? O3 Ce1 C1 O1 23.6(3) 2_774 . . . ? O7 Ce1 C1 O1 -38.8(3) 2_674 . . . ? O2 Ce1 C1 O1 160.5(4) . . . . ? O10 Ce1 C1 O1 -83.5(3) . . . . ? O8 Ce1 C1 O1 -85.6(3) 2_674 . . . ? O5 Ce1 C1 O1 145.3(3) . . . . ? O4 Ce1 C1 O1 62.1(3) 2_774 . . . ? C18 Ce1 C1 O1 -61.6(3) 2_674 . . . ? C10 Ce1 C1 O1 140.7(2) . . . . ? O6 Ce1 C1 O2 -29.0(4) . . . . ? O9 Ce1 C1 O2 53.2(3) . . . . ? O3 Ce1 C1 O2 -136.9(3) 2_774 . . . ? O7 Ce1 C1 O2 160.6(3) 2_674 . . . ? O10 Ce1 C1 O2 116.0(3) . . . . ? O8 Ce1 C1 O2 113.9(3) 2_674 . . . ? O5 Ce1 C1 O2 -15.2(3) . . . . ? O1 Ce1 C1 O2 -160.5(4) . . . . ? O4 Ce1 C1 O2 -98.4(3) 2_774 . . . ? C18 Ce1 C1 O2 137.9(3) 2_674 . . . ? C10 Ce1 C1 O2 -19.8(3) . . . . ? O6 Ce1 C1 C2 -113.1(9) . . . . ? O9 Ce1 C1 C2 -30.9(9) . . . . ? O3 Ce1 C1 C2 139.0(9) 2_774 . . . ? O7 Ce1 C1 C2 76.5(9) 2_674 . . . ? O2 Ce1 C1 C2 -84.1(9) . . . . ? O10 Ce1 C1 C2 31.9(10) . . . . ? O8 Ce1 C1 C2 29.8(9) 2_674 . . . ? O5 Ce1 C1 C2 -99.3(9) . . . . ? O1 Ce1 C1 C2 115.4(10) . . . . ? O4 Ce1 C1 C2 177.5(9) 2_774 . . . ? C18 Ce1 C1 C2 53.8(9) 2_674 . . . ? C10 Ce1 C1 C2 -103.9(9) . . . . ? O1 C1 C2 C3 41.0(7) . . . . ? O2 C1 C2 C3 -134.7(5) . . . . ? Ce1 C1 C2 C3 -63.6(11) . . . . ? O1 C1 C2 C8 -145.1(5) . . . . ? O2 C1 C2 C8 39.3(7) . . . . ? Ce1 C1 C2 C8 110.4(8) . . . . ? C8 C2 C3 C4 0.2(7) . . . . ? C1 C2 C3 C4 174.2(4) . . . . ? C2 C3 C4 N1 -177.6(5) . . . . ? C2 C3 C4 C6 1.8(7) . . . . ? C5 N1 C4 C3 -179.3(5) . . . . ? C5 N1 C4 C6 1.3(5) . . . . ? C6 N2 C5 N1 0.5(6) . . . . ? Ag1 N2 C5 N1 168.6(3) 4_655 . . . ? C4 N1 C5 N2 -1.2(6) . . . . ? C5 N2 C6 C4 0.4(5) . . . . ? Ag1 N2 C6 C4 -166.2(3) 4_655 . . . ? C5 N2 C6 C7 -177.7(5) . . . . ? Ag1 N2 C6 C7 15.7(8) 4_655 . . . ? C3 C4 C6 N2 179.4(4) . . . . ? N1 C4 C6 N2 -1.1(6) . . . . ? C3 C4 C6 C7 -2.3(8) . . . . ? N1 C4 C6 C7 177.2(4) . . . . ? N2 C6 C7 C8 178.6(5) . . . . ? C4 C6 C7 C8 0.7(7) . . . . ? C6 C7 C8 C2 1.2(7) . . . . ? C6 C7 C8 C9 177.2(4) . . . . ? C3 C2 C8 C7 -1.8(8) . . . . ? C1 C2 C8 C7 -175.5(5) . . . . ? C3 C2 C8 C9 -177.4(5) . . . . ? C1 C2 C8 C9 8.9(8) . . . . ? Ce1 O4 C9 O3 19.6(4) 2_775 . . . ? Ce1 O4 C9 C8 -154.6(4) 2_775 . . . ? Ce1 O3 C9 O4 -21.8(5) 2_775 . . . ? Ce1 O3 C9 C8 152.5(4) 2_775 . . . ? C7 C8 C9 O4 62.2(6) . . . . ? C2 C8 C9 O4 -121.9(6) . . . . ? C7 C8 C9 O3 -112.2(5) . . . . ? C2 C8 C9 O3 63.7(6) . . . . ? C7 C8 C9 Ce1 -41.0(10) . . . 2_775 ? C2 C8 C9 Ce1 134.8(7) . . . 2_775 ? Ce1 O5 C10 O6 3.7(4) . . . . ? Ce1 O5 C10 C11 177.6(4) . . . . ? Ce1 O6 C10 O5 -3.9(5) . . . . ? Ag1 O6 C10 O5 -148.3(4) . . . . ? Ce1 O6 C10 C11 -178.1(4) . . . . ? Ag1 O6 C10 C11 37.5(5) . . . . ? Ag1 O6 C10 Ce1 -144.3(2) . . . . ? O6 Ce1 C10 O5 176.2(5) . . . . ? O9 Ce1 C10 O5 -83.7(3) . . . . ? O3 Ce1 C10 O5 141.1(3) 2_774 . . . ? O7 Ce1 C10 O5 -170.2(3) 2_674 . . . ? O2 Ce1 C10 O5 2.8(3) . . . . ? O10 Ce1 C10 O5 -146.3(3) . . . . ? O8 Ce1 C10 O5 -74.0(3) 2_674 . . . ? O1 Ce1 C10 O5 31.6(3) . . . . ? O4 Ce1 C10 O5 96.1(3) 2_774 . . . ? C18 Ce1 C10 O5 -107.9(4) 2_674 . . . ? O9 Ce1 C10 O6 100.0(3) . . . . ? O3 Ce1 C10 O6 -35.2(3) 2_774 . . . ? O7 Ce1 C10 O6 13.6(5) 2_674 . . . ? O2 Ce1 C10 O6 -173.5(3) . . . . ? O10 Ce1 C10 O6 37.5(3) . . . . ? O8 Ce1 C10 O6 109.7(3) 2_674 . . . ? O5 Ce1 C10 O6 -176.2(5) . . . . ? O1 Ce1 C10 O6 -144.6(2) . . . . ? O4 Ce1 C10 O6 -80.1(3) 2_774 . . . ? C18 Ce1 C10 O6 75.9(4) 2_674 . . . ? O6 Ce1 C10 C11 17(3) . . . . ? O9 Ce1 C10 C11 117(3) . . . . ? O3 Ce1 C10 C11 -18(3) 2_774 . . . ? O7 Ce1 C10 C11 30(3) 2_674 . . . ? O2 Ce1 C10 C11 -157(3) . . . . ? O10 Ce1 C10 C11 54(3) . . . . ? O8 Ce1 C10 C11 127(3) 2_674 . . . ? O5 Ce1 C10 C11 -159(3) . . . . ? O1 Ce1 C10 C11 -128(3) . . . . ? O4 Ce1 C10 C11 -63(3) 2_774 . . . ? C18 Ce1 C10 C11 93(3) 2_674 . . . ? O5 C10 C11 C12 -137.7(5) . . . . ? O6 C10 C11 C12 36.5(6) . . . . ? Ce1 C10 C11 C12 21(4) . . . . ? O5 C10 C11 C17 39.8(7) . . . . ? O6 C10 C11 C17 -146.1(5) . . . . ? Ce1 C10 C11 C17 -162(3) . . . . ? C17 C11 C12 C13 -1.3(7) . . . . ? C10 C11 C12 C13 176.2(4) . . . . ? C14 N3 C13 C15 -0.6(5) . . . . ? Ag1 N3 C13 C15 -163.1(3) 3_565 . . . ? C14 N3 C13 C12 179.2(5) . . . . ? Ag1 N3 C13 C12 16.7(7) 3_565 . . . ? C11 C12 C13 N3 -178.8(5) . . . . ? C11 C12 C13 C15 1.0(7) . . . . ? C13 N3 C14 N4 0.9(6) . . . . ? Ag1 N3 C14 N4 160.0(3) 3_565 . . . ? C15 N4 C14 N3 -0.8(6) . . . . ? C14 N4 C15 C16 -179.0(5) . . . . ? C14 N4 C15 C13 0.3(5) . . . . ? N3 C13 C15 C16 179.7(4) . . . . ? C12 C13 C15 C16 -0.1(7) . . . . ? N3 C13 C15 N4 0.2(5) . . . . ? C12 C13 C15 N4 -179.6(4) . . . . ? N4 C15 C16 C17 179.0(5) . . . . ? C13 C15 C16 C17 -0.3(7) . . . . ? C15 C16 C17 C11 0.0(7) . . . . ? C15 C16 C17 C18 174.5(5) . . . . ? C12 C11 C17 C16 0.9(7) . . . . ? C10 C11 C17 C16 -176.4(5) . . . . ? C12 C11 C17 C18 -173.5(5) . . . . ? C10 C11 C17 C18 9.2(7) . . . . ? Ce1 O7 C18 O8 4.1(5) 2_675 . . . ? Ce1 O7 C18 C17 -177.7(4) 2_675 . . . ? Ce1 O8 C18 O7 -3.9(5) 2_675 . . . ? Ce1 O8 C18 C17 177.8(4) 2_675 . . . ? C16 C17 C18 O7 -139.7(5) . . . . ? C11 C17 C18 O7 34.9(7) . . . . ? C16 C17 C18 O8 38.6(7) . . . . ? C11 C17 C18 O8 -146.9(5) . . . . ? C16 C17 C18 Ce1 176(7) . . . 2_675 ? C11 C17 C18 Ce1 -10(8) . . . 2_675 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.413 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.083 data_6 _database_code_depnum_ccdc_archive 'CCDC 738829' #TrackingRef 'dt-art-05-2010-000579-File006-v1-0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H13 Ag Ho N4 O10.50' _chemical_formula_weight 726.12 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' 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 25.370(5) _cell_length_b 8.4884(17) _cell_length_c 17.806(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3834.6(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3380 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.02 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 5.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4231 _exptl_absorpt_correction_T_max 0.5746 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24212 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3380 _reflns_number_gt 3253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+14.0446P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3380 _refine_ls_number_parameters 312 _refine_ls_number_restraints 948 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.007 _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 Ho1 Ho 0.023361(7) 0.33426(2) 0.282486(9) 0.01060(7) Uani 1 1 d U . . Ag1 Ag 0.272687(13) 0.53837(5) 0.04826(2) 0.02782(10) Uani 1 1 d U . . O1 O 0.02106(10) 0.4221(3) 0.16116(15) 0.0147(6) Uani 1 1 d U . . O2 O -0.02401(11) 0.6361(3) 0.12882(16) 0.0172(6) Uani 1 1 d U . . O3 O -0.05985(10) 0.2756(3) 0.24011(15) 0.0160(6) Uani 1 1 d U . . O4 O -0.07975(12) 0.0422(3) 0.19172(18) 0.0247(7) Uani 1 1 d U . . O5 O 0.02522(11) -0.0646(4) 0.11239(16) 0.0223(7) Uani 1 1 d U . . O6 O 0.03099(10) 0.0881(3) 0.21145(14) 0.0146(6) Uani 1 1 d U . . O7 O 0.11021(11) 0.2522(4) 0.28540(14) 0.0188(6) Uani 1 1 d U . . O8 O 0.16337(15) 0.0503(5) 0.26565(19) 0.0414(9) Uani 1 1 d U . . N1 N -0.10972(13) 0.3749(4) -0.11071(18) 0.0183(7) Uani 1 1 d U . . H1 H -0.0963 0.4402 -0.1423 0.022 Uiso 1 1 calc R . . N2 N -0.16045(14) 0.1854(4) -0.06548(19) 0.0195(8) Uani 1 1 d U . . N3 N 0.20822(13) 0.4005(5) 0.00945(19) 0.0211(8) Uani 1 1 d U . . N4 N 0.14745(14) 0.3008(4) -0.06521(19) 0.0210(8) Uani 1 1 d U . . H4 H 0.1307 0.2792 -0.1059 0.025 Uiso 1 1 calc R . . C1 C -0.01728(15) 0.4898(5) 0.1293(2) 0.0125(8) Uani 1 1 d U . . C2 C -0.05565(15) 0.3946(5) 0.0832(2) 0.0134(8) Uani 1 1 d U . . C3 C -0.06259(15) 0.4465(5) 0.0103(2) 0.0139(8) Uani 1 1 d U . . H3 H -0.0451 0.5353 -0.0074 0.017 Uiso 1 1 calc R . . C4 C -0.09666(16) 0.3617(5) -0.0358(2) 0.0155(8) Uani 1 1 d U . . C5 C -0.14719(16) 0.2677(5) -0.1256(2) 0.0206(9) Uani 1 1 d U . . H5 H -0.1621 0.2531 -0.1728 0.025 Uiso 1 1 calc R . . C6 C -0.12750(15) 0.2393(5) -0.0079(2) 0.0160(8) Uani 1 1 d U . . C7 C -0.12001(17) 0.1843(5) 0.0645(2) 0.0187(9) Uani 1 1 d U . . H7 H -0.1393 0.0989 0.0824 0.022 Uiso 1 1 calc R . . C8 C -0.08310(15) 0.2589(5) 0.1100(2) 0.0145(8) Uani 1 1 d U . . C9 C -0.07337(15) 0.1892(5) 0.1859(2) 0.0157(8) Uani 1 1 d U . . C10 C 0.04665(16) 0.0480(5) 0.1460(2) 0.0146(8) Uani 1 1 d U . . C11 C 0.09230(15) 0.1340(5) 0.1121(2) 0.0135(8) Uani 1 1 d U . . C12 C 0.09316(16) 0.1583(5) 0.0344(2) 0.0166(8) Uani 1 1 d U . . H12 H 0.0671 0.1172 0.0033 0.020 Uiso 1 1 calc R . . C13 C 0.13486(15) 0.2469(5) 0.0057(2) 0.0166(8) Uani 1 1 d U . . C14 C 0.18989(17) 0.3917(6) -0.0598(2) 0.0230(9) Uani 1 1 d U . . H14 H 0.2051 0.4435 -0.1004 0.028 Uiso 1 1 calc R . . C15 C 0.17414(16) 0.3086(5) 0.0524(2) 0.0173(8) Uani 1 1 d U . . C16 C 0.17455(16) 0.2766(5) 0.1291(2) 0.0183(8) Uani 1 1 d U . . H16 H 0.2019 0.3121 0.1595 0.022 Uiso 1 1 calc R . . C17 C 0.13330(16) 0.1910(5) 0.1591(2) 0.0160(8) Uani 1 1 d U . . C18 C 0.13527(16) 0.1573(5) 0.2422(2) 0.0176(9) Uani 1 1 d U . . O9 O 0.25405(17) 0.5869(5) 0.1986(2) 0.0557(11) Uani 1 1 d U . . H9B H 0.2783 0.5733 0.2310 0.067 Uiso 1 1 d R . . H9A H 0.2453 0.4984 0.1791 0.067 Uiso 1 1 d R . . O10 O 0.6994(3) 0.5280(11) 0.1826(4) 0.147(4) Uani 1 1 d . . . H10A H 0.7197 0.5071 0.2193 0.176 Uiso 1 1 d R . . H10B H 0.7124 0.5583 0.1410 0.176 Uiso 1 1 d R . . O11 O 0.7500 0.2500 0.6088(8) 0.190(6) Uani 1 2 d S . . H11A H 0.7741 0.2246 0.5779 0.228 Uiso 0.50 1 d PR . . H11B H 0.7578 0.2717 0.6540 0.228 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01335(12) 0.00942(12) 0.00903(11) 0.00005(6) -0.00079(6) 0.00175(6) Ag1 0.02062(18) 0.0335(2) 0.0293(2) 0.00062(15) 0.00071(14) -0.01314(15) O1 0.0141(13) 0.0188(15) 0.0112(13) 0.0025(11) -0.0015(10) -0.0016(11) O2 0.0285(16) 0.0109(15) 0.0122(14) -0.0026(11) -0.0001(11) -0.0021(12) O3 0.0172(14) 0.0187(15) 0.0120(13) -0.0007(11) 0.0010(11) 0.0013(12) O4 0.0239(15) 0.0142(16) 0.0361(17) 0.0074(13) -0.0115(14) -0.0035(13) O5 0.0337(17) 0.0193(16) 0.0140(14) -0.0038(12) 0.0061(12) -0.0118(13) O6 0.0168(13) 0.0133(15) 0.0136(13) -0.0023(11) 0.0038(10) -0.0017(11) O7 0.0178(14) 0.0229(16) 0.0157(14) -0.0060(12) 0.0022(11) 0.0057(13) O8 0.054(2) 0.047(2) 0.0228(17) 0.0040(15) 0.0019(16) 0.0308(19) N1 0.0191(17) 0.0220(19) 0.0139(16) 0.0035(14) -0.0025(13) -0.0044(15) N2 0.0166(17) 0.023(2) 0.0185(18) -0.0019(14) -0.0032(14) -0.0049(14) N3 0.0190(17) 0.026(2) 0.0183(18) 0.0036(15) 0.0017(14) -0.0069(16) N4 0.0222(18) 0.028(2) 0.0126(17) 0.0015(14) -0.0011(14) -0.0064(16) C1 0.0176(19) 0.012(2) 0.0078(17) 0.0010(14) 0.0032(14) -0.0028(15) C2 0.0136(18) 0.0125(19) 0.0140(18) -0.0037(15) -0.0013(14) -0.0012(15) C3 0.0154(18) 0.0126(19) 0.0137(18) 0.0026(14) -0.0009(15) -0.0012(15) C4 0.0158(19) 0.017(2) 0.0137(19) 0.0001(15) -0.0006(15) 0.0007(16) C5 0.022(2) 0.026(2) 0.0134(19) 0.0005(17) -0.0039(16) -0.0035(19) C6 0.0124(18) 0.019(2) 0.0162(19) -0.0029(16) -0.0019(15) -0.0035(16) C7 0.020(2) 0.014(2) 0.023(2) 0.0027(16) -0.0006(16) -0.0027(16) C8 0.0147(17) 0.0118(19) 0.0170(18) 0.0013(15) -0.0005(15) -0.0008(15) C9 0.0120(18) 0.015(2) 0.020(2) 0.0028(16) 0.0005(15) 0.0000(15) C10 0.0188(19) 0.0136(19) 0.0113(17) 0.0028(14) -0.0002(15) 0.0003(16) C11 0.0153(18) 0.0131(19) 0.0121(18) -0.0008(15) 0.0001(14) 0.0005(15) C12 0.0170(19) 0.018(2) 0.0148(19) -0.0026(15) -0.0013(15) -0.0015(16) C13 0.0174(19) 0.020(2) 0.0127(18) -0.0001(15) -0.0010(15) -0.0009(17) C14 0.022(2) 0.030(2) 0.017(2) 0.0084(18) 0.0025(16) -0.0126(19) C15 0.0140(19) 0.019(2) 0.0190(19) 0.0019(16) 0.0019(16) -0.0011(16) C16 0.0173(18) 0.022(2) 0.0158(18) 0.0004(16) -0.0034(16) -0.0010(17) C17 0.0148(18) 0.018(2) 0.0156(19) -0.0005(15) 0.0020(15) 0.0045(15) C18 0.016(2) 0.021(2) 0.016(2) 0.0019(16) 0.0003(16) 0.0017(17) O9 0.048(2) 0.055(3) 0.064(3) 0.011(2) -0.010(2) 0.005(2) O10 0.107(5) 0.229(10) 0.103(5) -0.028(6) -0.034(4) 0.076(6) O11 0.171(12) 0.220(15) 0.179(13) 0.000 0.000 -0.056(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1 2.286(3) . ? Ho1 O3 2.297(3) . ? Ho1 O2 2.307(3) 3_545 ? Ho1 O7 2.311(3) . ? Ho1 O4 2.318(3) 3 ? Ho1 O5 2.400(3) 3 ? Ho1 O6 2.450(3) . ? Ho1 O6 2.560(3) 3 ? Ho1 C10 2.841(4) 3 ? Ag1 N3 2.127(4) . ? Ag1 N2 2.128(4) 6_665 ? O1 C1 1.265(5) . ? O2 C1 1.253(5) . ? O2 Ho1 2.307(3) 3 ? O3 C9 1.260(5) . ? O4 C9 1.262(5) . ? O4 Ho1 2.318(3) 3_545 ? O5 C10 1.252(5) . ? O5 Ho1 2.400(3) 3_545 ? O6 C10 1.277(5) . ? O6 Ho1 2.560(3) 3_545 ? O7 C18 1.283(5) . ? O8 C18 1.228(5) . ? N1 C5 1.342(5) . ? N1 C4 1.378(5) . ? N1 H1 0.8600 . ? N2 C5 1.322(5) . ? N2 C6 1.400(5) . ? N2 Ag1 2.128(3) 6 ? N3 C14 1.320(5) . ? N3 C15 1.394(5) . ? N4 C14 1.328(6) . ? N4 C13 1.380(5) . ? N4 H4 0.8600 . ? C1 C2 1.508(5) . ? C2 C3 1.382(5) . ? C2 C8 1.427(6) . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C6 1.392(6) . ? C5 H5 0.9300 . ? C6 C7 1.384(6) . ? C7 C8 1.391(6) . ? C7 H7 0.9300 . ? C8 C9 1.497(5) . ? C10 C11 1.496(5) . ? C10 Ho1 2.841(4) 3_545 ? C11 C12 1.398(6) . ? C11 C17 1.420(6) . ? C12 C13 1.395(6) . ? C12 H12 0.9300 . ? C13 C15 1.400(6) . ? C14 H14 0.9300 . ? C15 C16 1.392(6) . ? C16 C17 1.381(6) . ? C16 H16 0.9300 . ? C17 C18 1.507(6) . ? O9 H9B 0.8506 . ? O9 H9A 0.8565 . ? O10 H10A 0.8500 . ? O10 H10B 0.8499 . ? O11 H11A 0.8500 . ? O11 H11B 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 O1 Ho1 O3 74.74(9) . . ? O1 Ho1 O2 152.22(10) . 3_545 ? O3 Ho1 O2 94.21(10) . 3_545 ? O1 Ho1 O7 98.27(9) . . ? O3 Ho1 O7 144.92(10) . . ? O2 Ho1 O7 76.00(10) 3_545 . ? O1 Ho1 O4 87.39(11) . 3 ? O3 Ho1 O4 142.89(10) . 3 ? O2 Ho1 O4 114.53(11) 3_545 3 ? O7 Ho1 O4 68.70(10) . 3 ? O1 Ho1 O5 127.39(10) . 3 ? O3 Ho1 O5 82.05(10) . 3 ? O2 Ho1 O5 74.37(10) 3_545 3 ? O7 Ho1 O5 125.43(9) . 3 ? O4 Ho1 O5 83.69(11) 3 3 ? O1 Ho1 O6 78.02(10) . . ? O3 Ho1 O6 73.63(9) . . ? O2 Ho1 O6 74.39(10) 3_545 . ? O7 Ho1 O6 71.30(10) . . ? O4 Ho1 O6 134.66(10) 3 . ? O5 Ho1 O6 138.44(10) 3 . ? O1 Ho1 O6 75.62(9) . 3 ? O3 Ho1 O6 72.61(10) . 3 ? O2 Ho1 O6 126.05(9) 3_545 3 ? O7 Ho1 O6 140.00(10) . 3 ? O4 Ho1 O6 71.53(10) 3 3 ? O5 Ho1 O6 52.38(9) 3 3 ? O6 Ho1 O6 141.44(2) . 3 ? O1 Ho1 C10 101.49(11) . 3 ? O3 Ho1 C10 73.20(10) . 3 ? O2 Ho1 C10 99.40(11) 3_545 3 ? O7 Ho1 C10 141.12(10) . 3 ? O4 Ho1 C10 79.08(11) 3 3 ? O5 Ho1 C10 25.95(10) 3 3 ? O6 Ho1 C10 145.65(10) . 3 ? O6 Ho1 C10 26.72(10) 3 3 ? N3 Ag1 N2 169.29(13) . 6_665 ? C1 O1 Ho1 126.3(2) . . ? C1 O2 Ho1 135.8(3) . 3 ? C9 O3 Ho1 128.9(2) . . ? C9 O4 Ho1 133.6(3) . 3_545 ? C10 O5 Ho1 97.1(2) . 3_545 ? C10 O6 Ho1 136.3(3) . . ? C10 O6 Ho1 89.0(2) . 3_545 ? Ho1 O6 Ho1 130.79(11) . 3_545 ? C18 O7 Ho1 130.4(3) . . ? C5 N1 C4 107.8(3) . . ? C5 N1 H1 126.1 . . ? C4 N1 H1 126.1 . . ? C5 N2 C6 105.6(3) . . ? C5 N2 Ag1 129.0(3) . 6 ? C6 N2 Ag1 124.2(3) . 6 ? C14 N3 C15 105.2(3) . . ? C14 N3 Ag1 127.3(3) . . ? C15 N3 Ag1 127.4(3) . . ? C14 N4 C13 108.3(3) . . ? C14 N4 H4 125.9 . . ? C13 N4 H4 125.9 . . ? O2 C1 O1 123.9(4) . . ? O2 C1 C2 116.1(3) . . ? O1 C1 C2 119.8(4) . . ? C3 C2 C8 120.6(3) . . ? C3 C2 C1 114.9(3) . . ? C8 C2 C1 124.5(3) . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? N1 C4 C6 105.8(3) . . ? N1 C4 C3 132.7(4) . . ? C6 C4 C3 121.6(4) . . ? N2 C5 N1 112.2(4) . . ? N2 C5 H5 123.9 . . ? N1 C5 H5 123.9 . . ? C7 C6 C4 120.5(4) . . ? C7 C6 N2 130.8(4) . . ? C4 C6 N2 108.5(3) . . ? C6 C7 C8 118.7(4) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C7 C8 C2 120.1(4) . . ? C7 C8 C9 117.2(4) . . ? C2 C8 C9 122.7(3) . . ? O3 C9 O4 123.2(4) . . ? O3 C9 C8 120.5(4) . . ? O4 C9 C8 116.3(4) . . ? O5 C10 O6 120.3(4) . . ? O5 C10 C11 121.0(3) . . ? O6 C10 C11 118.6(3) . . ? O5 C10 Ho1 57.0(2) . 3_545 ? O6 C10 Ho1 64.3(2) . 3_545 ? C11 C10 Ho1 167.6(3) . 3_545 ? C12 C11 C17 121.4(4) . . ? C12 C11 C10 118.9(3) . . ? C17 C11 C10 119.7(3) . . ? C13 C12 C11 117.0(4) . . ? C13 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? N4 C13 C12 133.6(4) . . ? N4 C13 C15 104.8(3) . . ? C12 C13 C15 121.6(4) . . ? N3 C14 N4 112.7(4) . . ? N3 C14 H14 123.6 . . ? N4 C14 H14 123.6 . . ? C16 C15 N3 130.0(4) . . ? C16 C15 C13 121.0(4) . . ? N3 C15 C13 108.9(4) . . ? C17 C16 C15 118.4(4) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C11 120.4(4) . . ? C16 C17 C18 117.0(4) . . ? C11 C17 C18 122.6(4) . . ? O8 C18 O7 123.2(4) . . ? O8 C18 C17 119.6(4) . . ? O7 C18 C17 116.9(3) . . ? H9B O9 H9A 110.1 . . ? H10A O10 H10B 120.0 . . ? H11A O11 H11B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ho1 O1 C1 39.4(3) . . . . ? O2 Ho1 O1 C1 108.7(3) 3_545 . . . ? O7 Ho1 O1 C1 -175.7(3) . . . . ? O4 Ho1 O1 C1 -107.7(3) 3 . . . ? O5 Ho1 O1 C1 -27.7(4) 3 . . . ? O6 Ho1 O1 C1 115.5(3) . . . . ? O6 Ho1 O1 C1 -36.1(3) 3 . . . ? C10 Ho1 O1 C1 -29.4(3) 3 . . . ? O1 Ho1 O3 C9 60.0(3) . . . . ? O2 Ho1 O3 C9 -94.1(3) 3_545 . . . ? O7 Ho1 O3 C9 -22.6(4) . . . . ? O4 Ho1 O3 C9 124.0(3) 3 . . . ? O5 Ho1 O3 C9 -167.7(3) 3 . . . ? O6 Ho1 O3 C9 -21.7(3) . . . . ? O6 Ho1 O3 C9 139.4(3) 3 . . . ? C10 Ho1 O3 C9 167.3(3) 3 . . . ? O1 Ho1 O6 C10 24.1(4) . . . . ? O3 Ho1 O6 C10 101.5(4) . . . . ? O2 Ho1 O6 C10 -159.2(4) 3_545 . . . ? O7 Ho1 O6 C10 -79.1(4) . . . . ? O4 Ho1 O6 C10 -50.0(4) 3 . . . ? O5 Ho1 O6 C10 158.2(3) 3 . . . ? O6 Ho1 O6 C10 71.7(4) 3 . . . ? C10 Ho1 O6 C10 117.0(3) 3 . . . ? O1 Ho1 O6 Ho1 -126.09(16) . . . 3_545 ? O3 Ho1 O6 Ho1 -48.69(14) . . . 3_545 ? O2 Ho1 O6 Ho1 50.61(14) 3_545 . . 3_545 ? O7 Ho1 O6 Ho1 130.79(17) . . . 3_545 ? O4 Ho1 O6 Ho1 159.87(13) 3 . . 3_545 ? O5 Ho1 O6 Ho1 8.1(2) 3 . . 3_545 ? O6 Ho1 O6 Ho1 -78.43(19) 3 . . 3_545 ? C10 Ho1 O6 Ho1 -33.2(3) 3 . . 3_545 ? O1 Ho1 O7 C18 -54.0(4) . . . . ? O3 Ho1 O7 C18 21.2(4) . . . . ? O2 Ho1 O7 C18 98.3(4) 3_545 . . . ? O4 Ho1 O7 C18 -137.9(4) 3 . . . ? O5 Ho1 O7 C18 157.1(3) 3 . . . ? O6 Ho1 O7 C18 20.3(3) . . . . ? O6 Ho1 O7 C18 -131.5(3) 3 . . . ? C10 Ho1 O7 C18 -174.1(3) 3 . . . ? N2 Ag1 N3 C14 -7.5(10) 6_665 . . . ? N2 Ag1 N3 C15 177.2(6) 6_665 . . . ? Ho1 O2 C1 O1 -48.7(6) 3 . . . ? Ho1 O2 C1 C2 136.3(3) 3 . . . ? Ho1 O1 C1 O2 90.2(4) . . . . ? Ho1 O1 C1 C2 -95.0(4) . . . . ? O2 C1 C2 C3 49.9(5) . . . . ? O1 C1 C2 C3 -125.4(4) . . . . ? O2 C1 C2 C8 -131.0(4) . . . . ? O1 C1 C2 C8 53.8(5) . . . . ? C8 C2 C3 C4 -0.6(6) . . . . ? C1 C2 C3 C4 178.6(3) . . . . ? C5 N1 C4 C6 1.2(5) . . . . ? C5 N1 C4 C3 -176.5(4) . . . . ? C2 C3 C4 N1 -175.4(4) . . . . ? C2 C3 C4 C6 7.2(6) . . . . ? C6 N2 C5 N1 -2.4(5) . . . . ? Ag1 N2 C5 N1 165.2(3) 6 . . . ? C4 N1 C5 N2 0.8(5) . . . . ? N1 C4 C6 C7 173.2(4) . . . . ? C3 C4 C6 C7 -8.8(6) . . . . ? N1 C4 C6 N2 -2.7(5) . . . . ? C3 C4 C6 N2 175.3(4) . . . . ? C5 N2 C6 C7 -172.1(4) . . . . ? Ag1 N2 C6 C7 19.5(6) 6 . . . ? C5 N2 C6 C4 3.1(5) . . . . ? Ag1 N2 C6 C4 -165.2(3) 6 . . . ? C4 C6 C7 C8 3.4(6) . . . . ? N2 C6 C7 C8 178.2(4) . . . . ? C6 C7 C8 C2 3.1(6) . . . . ? C6 C7 C8 C9 -175.9(4) . . . . ? C3 C2 C8 C7 -4.6(6) . . . . ? C1 C2 C8 C7 176.3(4) . . . . ? C3 C2 C8 C9 174.3(4) . . . . ? C1 C2 C8 C9 -4.8(6) . . . . ? Ho1 O3 C9 O4 86.6(5) . . . . ? Ho1 O3 C9 C8 -93.8(4) . . . . ? Ho1 O4 C9 O3 -65.2(6) 3_545 . . . ? Ho1 O4 C9 C8 115.2(4) 3_545 . . . ? C7 C8 C9 O3 -149.9(4) . . . . ? C2 C8 C9 O3 31.2(6) . . . . ? C7 C8 C9 O4 29.8(5) . . . . ? C2 C8 C9 O4 -149.1(4) . . . . ? Ho1 O5 C10 O6 -12.0(4) 3_545 . . . ? Ho1 O5 C10 C11 165.5(3) 3_545 . . . ? Ho1 O6 C10 O5 -146.8(3) . . . . ? Ho1 O6 C10 O5 11.1(4) 3_545 . . . ? Ho1 O6 C10 C11 35.7(5) . . . . ? Ho1 O6 C10 C11 -166.4(3) 3_545 . . . ? Ho1 O6 C10 Ho1 -157.9(3) . . . 3_545 ? O5 C10 C11 C12 36.6(6) . . . . ? O6 C10 C11 C12 -145.9(4) . . . . ? Ho1 C10 C11 C12 113.5(12) 3_545 . . . ? O5 C10 C11 C17 -144.3(4) . . . . ? O6 C10 C11 C17 33.2(6) . . . . ? Ho1 C10 C11 C17 -67.4(14) 3_545 . . . ? C17 C11 C12 C13 -2.7(6) . . . . ? C10 C11 C12 C13 176.3(4) . . . . ? C14 N4 C13 C12 174.9(5) . . . . ? C14 N4 C13 C15 -2.0(5) . . . . ? C11 C12 C13 N4 -176.4(4) . . . . ? C11 C12 C13 C15 0.1(6) . . . . ? C15 N3 C14 N4 -0.7(5) . . . . ? Ag1 N3 C14 N4 -176.8(3) . . . . ? C13 N4 C14 N3 1.8(6) . . . . ? C14 N3 C15 C16 -179.7(5) . . . . ? Ag1 N3 C15 C16 -3.6(7) . . . . ? C14 N3 C15 C13 -0.6(5) . . . . ? Ag1 N3 C15 C13 175.5(3) . . . . ? N4 C13 C15 C16 -179.2(4) . . . . ? C12 C13 C15 C16 3.4(7) . . . . ? N4 C13 C15 N3 1.6(5) . . . . ? C12 C13 C15 N3 -175.8(4) . . . . ? N3 C15 C16 C17 174.8(4) . . . . ? C13 C15 C16 C17 -4.2(6) . . . . ? C15 C16 C17 C11 1.6(6) . . . . ? C15 C16 C17 C18 179.4(4) . . . . ? C12 C11 C17 C16 1.9(6) . . . . ? C10 C11 C17 C16 -177.1(4) . . . . ? C12 C11 C17 C18 -175.8(4) . . . . ? C10 C11 C17 C18 5.1(6) . . . . ? Ho1 O7 C18 O8 -132.3(4) . . . . ? Ho1 O7 C18 C17 53.4(5) . . . . ? C16 C17 C18 O8 -79.3(5) . . . . ? C11 C17 C18 O8 98.5(5) . . . . ? C16 C17 C18 O7 95.2(5) . . . . ? C11 C17 C18 O7 -87.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.662 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.140