Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dongfeng Xue' _publ_contact_author_address ; School of Chemical Engineering Dalian University of Technology 158 Zhongshan Road Dalian Liaoning 116012 CHINA ; _publ_contact_author_email DFXUE@CHEM.DLUT.EDU.CN _publ_section_title ; Self-assembly of three-dimensional 4d-4f coordination frameworks based on one-dimensional inorganic heterometallic chains and linear organic linkers ; loop_ _publ_author_name 'Dongfeng Xue' 'Xiaojun Gu' #==========================================================END data_2 _database_code_depnum_ccdc_archive 'CCDC 299741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H9.50 Ag Eu N2.50 O9' _chemical_formula_weight 652.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2636(18) _cell_length_b 10.409(3) _cell_length_c 11.639(3) _cell_angle_alpha 100.486(3) _cell_angle_beta 101.062(3) _cell_angle_gamma 95.619(3) _cell_volume 841.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 4.923 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4682 _diffrn_reflns_av_R_equivalents 0.0119 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3334 _reflns_number_gt 3204 _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^)+(0.0369P)^2^+6.4592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3334 _refine_ls_number_parameters 284 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu -0.24305(3) 0.47472(2) -0.43321(2) 0.01129(9) Uani 1 1 d . . . Ag1 Ag 0.79086(7) 0.74889(5) 0.21219(5) 0.03814(15) Uani 1 1 d . . . O3 O 1.4371(6) 1.2374(4) 0.6281(4) 0.0295(10) Uani 1 1 d . . . O5 O -0.3997(5) 0.5290(4) -0.2735(3) 0.0209(8) Uani 1 1 d . . . O1 O -0.0386(5) 0.6262(3) -0.5055(3) 0.0151(7) Uani 1 1 d . . . O8 O -0.0331(5) 0.6335(4) -0.2614(3) 0.0212(8) Uani 1 1 d . . . O7 O -0.0137(5) 0.4252(4) -0.2511(3) 0.0212(8) Uani 1 1 d . . . N1 N 0.9905(7) 0.9254(5) 0.3070(4) 0.0238(10) Uani 1 1 d . . . N2 N 0.5417(7) 0.6785(5) 0.0667(4) 0.0197(9) Uani 1 1 d . . . C10 C 0.2224(7) 0.5927(5) -0.1196(5) 0.0164(10) Uani 1 1 d . . . C8 C 0.3650(8) 0.6702(6) 0.0885(5) 0.0222(11) Uani 1 1 d . . . H2 H 0.3511 0.6935 0.1671 0.027 Uiso 1 1 calc R . . C1 C 1.1802(8) 0.9312(5) 0.3232(5) 0.0235(12) Uani 1 1 d . . . H3 H 1.2299 0.8584 0.2886 0.028 Uiso 1 1 calc R . . C12 C 0.5571(8) 0.6426(5) -0.0471(5) 0.0183(10) Uani 1 1 d . . . H4 H 0.6778 0.6470 -0.0632 0.022 Uiso 1 1 calc R . . C3 C 1.2340(7) 1.1496(5) 0.4427(5) 0.0158(10) Uani 1 1 d . . . C5 C 0.9216(8) 1.0324(5) 0.3569(5) 0.0216(11) Uani 1 1 d . . . H6 H 0.7910 1.0303 0.3455 0.026 Uiso 1 1 calc R . . C2 C 1.3027(8) 1.0394(6) 0.3885(5) 0.0222(11) Uani 1 1 d . . . H8 H 1.4326 1.0392 0.3968 0.027 Uiso 1 1 calc R . . C14 C 0.0469(7) 0.5475(5) -0.2180(5) 0.0177(11) Uani 1 1 d . . . C7 C 1.3763(7) 1.2577(5) 0.5282(5) 0.0162(10) Uani 1 1 d . . . C4 C 1.0367(7) 1.1457(5) 0.4245(5) 0.0170(10) Uani 1 1 d . . . C9 C 0.2047(8) 0.6289(6) -0.0009(5) 0.0205(11) Uani 1 1 d . . . H13 H 0.0856 0.6251 0.0176 0.025 Uiso 1 1 calc R . . C11 C 0.4028(7) 0.5991(5) -0.1426(4) 0.0157(10) Uani 1 1 d . . . C15 C 0.811(3) 0.9886(12) -0.0182(11) 0.148(9) Uani 1 1 d D . . C18 C 0.885(4) 0.904(2) -0.0962(16) 0.137(10) Uani 1 1 d . . . C17 C 1.071(5) 0.9194(15) -0.0771(15) 0.186(15) Uani 0.50 1 d P . . N3 N 1.071(5) 0.9194(15) -0.0771(15) 0.186(15) Uani 0.50 1 d P . . O10 O 0.511(5) 0.9770(16) -0.0390(17) 0.092(6) Uani 0.50 1 d P . . O9 O 0.486(5) 0.929(3) -0.132(2) 0.149(10) Uani 0.50 1 d PD . . C16 C 0.601(4) 0.982(8) -0.031(4) 0.21(5) Uiso 0.50 1 d PD . . O6 O -0.3066(5) 0.4365(4) -0.6479(3) 0.0187(8) Uani 1 1 d . . . O2 O -0.2178(5) 0.2384(4) -0.5040(4) 0.0212(8) Uani 1 1 d . . . O4 O -0.4303(5) 0.6422(3) -0.4865(3) 0.0154(7) Uani 1 1 d . . . C6 C 0.9452(7) 1.2587(5) 0.4779(5) 0.0152(10) Uani 1 1 d . . . C13 C 0.4390(7) 0.5603(5) -0.2673(4) 0.0147(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 Eu1 0.00797(14) 0.01391(14) 0.01150(13) 0.00099(9) 0.00206(9) 0.00220(9) Ag1 0.0298(3) 0.0426(3) 0.0302(3) -0.0090(2) -0.0012(2) -0.0061(2) O3 0.033(2) 0.032(2) 0.020(2) 0.0087(17) -0.0023(17) -0.0005(19) O5 0.0125(18) 0.034(2) 0.0161(18) 0.0027(16) 0.0051(14) 0.0059(16) O1 0.0119(17) 0.0142(17) 0.0185(18) 0.0023(14) 0.0036(14) 0.0005(13) O8 0.0157(19) 0.025(2) 0.0200(19) 0.0010(16) -0.0010(15) 0.0035(15) O7 0.0164(19) 0.023(2) 0.023(2) 0.0027(16) 0.0023(15) 0.0011(15) N1 0.024(3) 0.017(2) 0.027(3) -0.0011(19) 0.003(2) -0.0003(19) N2 0.018(2) 0.021(2) 0.016(2) -0.0012(17) -0.0026(17) 0.0034(18) C10 0.015(3) 0.019(3) 0.015(2) 0.0029(19) 0.0033(19) 0.0040(19) C8 0.025(3) 0.026(3) 0.014(2) -0.001(2) 0.004(2) 0.007(2) C1 0.024(3) 0.016(3) 0.029(3) -0.002(2) 0.007(2) 0.009(2) C12 0.014(3) 0.020(3) 0.020(3) 0.002(2) 0.004(2) 0.002(2) C3 0.016(3) 0.014(2) 0.017(2) 0.0031(19) 0.004(2) 0.0031(19) C5 0.015(3) 0.020(3) 0.028(3) 0.001(2) 0.005(2) 0.004(2) C2 0.018(3) 0.021(3) 0.029(3) 0.003(2) 0.007(2) 0.004(2) C14 0.012(2) 0.027(3) 0.014(2) 0.001(2) 0.0061(19) 0.001(2) C7 0.011(2) 0.017(3) 0.021(3) 0.002(2) 0.006(2) 0.0050(19) C4 0.016(3) 0.014(2) 0.021(3) 0.003(2) 0.003(2) 0.0008(19) C9 0.017(3) 0.028(3) 0.015(2) 0.000(2) 0.005(2) 0.005(2) C11 0.016(3) 0.017(2) 0.013(2) 0.0005(19) 0.0029(19) 0.0034(19) C15 0.36(3) 0.039(6) 0.052(7) 0.018(5) 0.039(12) 0.024(11) C18 0.29(3) 0.065(9) 0.047(8) 0.018(7) 0.024(14) -0.003(15) C17 0.45(4) 0.039(7) 0.053(8) 0.018(6) 0.022(18) 0.021(17) N3 0.45(4) 0.039(7) 0.053(8) 0.018(6) 0.022(18) 0.021(17) O10 0.18(2) 0.036(9) 0.072(14) 0.030(9) 0.038(15) 0.038(11) O9 0.22(3) 0.13(2) 0.095(18) 0.023(16) 0.037(19) 0.02(2) O6 0.0150(18) 0.027(2) 0.0131(17) 0.0018(15) 0.0030(14) 0.0029(15) O2 0.0133(19) 0.0191(19) 0.032(2) 0.0046(16) 0.0084(16) 0.0016(15) O4 0.0114(17) 0.0132(17) 0.0207(18) 0.0016(14) 0.0034(14) 0.0009(13) C6 0.014(3) 0.014(2) 0.016(2) 0.0045(19) 0.0010(19) 0.0036(19) C13 0.015(3) 0.015(2) 0.014(2) 0.0009(18) 0.0036(19) -0.0012(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 Eu1 O5 2.371(4) . ? Eu1 O6 2.403(4) . ? Eu1 O4 2.410(4) . ? Eu1 O1 2.430(3) . ? Eu1 O4 2.480(4) 2_464 ? Eu1 O2 2.484(4) . ? Eu1 O8 2.488(4) . ? Eu1 O1 2.551(4) 2_564 ? Eu1 O7 2.597(4) . ? Eu1 C14 2.873(5) . ? Eu1 C6 2.880(5) 1_444 ? Eu1 Eu1 3.8837(10) 2_464 ? Ag1 N2 2.189(4) . ? Ag1 N1 2.195(5) . ? Ag1 O7 2.588(4) 2_665 ? O3 C7 1.226(7) . ? O5 C13 1.258(6) 1_455 ? O1 C6 1.271(6) 2_675 ? O1 Eu1 2.551(4) 2_564 ? O8 C14 1.245(7) . ? O7 C14 1.269(7) . ? O7 Ag1 2.588(4) 2_665 ? N1 C5 1.347(7) . ? N1 C1 1.348(8) . ? N2 C12 1.338(7) . ? N2 C8 1.353(7) . ? C10 C11 1.385(7) . ? C10 C9 1.399(7) . ? C10 C14 1.511(7) . ? C8 C9 1.377(8) . ? C8 H2 0.9300 . ? C1 C2 1.368(8) . ? C1 H3 0.9300 . ? C12 C11 1.391(7) . ? C12 H4 0.9300 . ? C3 C2 1.390(7) . ? C3 C4 1.404(7) . ? C3 C7 1.515(7) . ? C5 C4 1.387(7) . ? C5 H6 0.9300 . ? C2 H8 0.9300 . ? C7 O4 1.285(6) 2_675 ? C4 C6 1.502(7) . ? C9 H13 0.9300 . ? C11 C13 1.515(7) . ? C15 C18 1.37(3) . ? C15 N3 1.40(2) 2_775 ? C15 C17 1.40(2) 2_775 ? C15 C16 1.499(19) . ? C18 C17 1.31(4) . ? C17 C15 1.40(2) 2_775 ? O10 O10 1.00(3) 2_675 ? O10 O9 1.08(3) . ? O10 C16 1.303(19) 2_675 ? O9 C16 1.30(2) . ? C16 O10 1.303(19) 2_675 ? O6 C13 1.247(6) 2_564 ? O2 C6 1.246(6) 1_444 ? O4 C7 1.285(6) 2_675 ? O4 Eu1 2.480(4) 2_464 ? C6 O2 1.246(6) 1_666 ? C6 O1 1.271(6) 2_675 ? C6 Eu1 2.880(5) 1_666 ? C13 O6 1.247(6) 2_564 ? C13 O5 1.258(6) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Eu1 O6 139.79(13) . . ? O5 Eu1 O4 75.05(13) . . ? O6 Eu1 O4 74.48(13) . . ? O5 Eu1 O1 126.51(13) . . ? O6 Eu1 O1 67.74(12) . . ? O4 Eu1 O1 74.05(12) . . ? O5 Eu1 O4 76.02(13) . 2_464 ? O6 Eu1 O4 71.15(12) . 2_464 ? O4 Eu1 O4 74.85(13) . 2_464 ? O1 Eu1 O4 133.48(12) . 2_464 ? O5 Eu1 O2 117.77(13) . . ? O6 Eu1 O2 73.58(13) . . ? O4 Eu1 O2 140.12(13) . . ? O1 Eu1 O2 114.04(12) . . ? O4 Eu1 O2 72.68(12) 2_464 . ? O5 Eu1 O8 68.69(13) . . ? O6 Eu1 O8 137.67(13) . . ? O4 Eu1 O8 92.09(12) . . ? O1 Eu1 O8 69.99(13) . . ? O4 Eu1 O8 144.50(12) 2_464 . ? O2 Eu1 O8 127.74(13) . . ? O5 Eu1 O1 144.66(12) . 2_564 ? O6 Eu1 O1 74.12(12) . 2_564 ? O4 Eu1 O1 137.01(12) . 2_564 ? O1 Eu1 O1 67.27(14) . 2_564 ? O4 Eu1 O1 120.43(11) 2_464 2_564 ? O2 Eu1 O1 51.65(11) . 2_564 ? O8 Eu1 O1 91.78(12) . 2_564 ? O5 Eu1 O7 76.59(13) . . ? O6 Eu1 O7 141.92(12) . . ? O4 Eu1 O7 140.25(12) . . ? O1 Eu1 O7 102.15(12) . . ? O4 Eu1 O7 123.78(12) 2_464 . ? O2 Eu1 O7 78.40(13) . . ? O8 Eu1 O7 51.47(13) . . ? O1 Eu1 O7 68.32(12) 2_564 . ? O5 Eu1 C14 73.49(14) . . ? O6 Eu1 C14 145.03(13) . . ? O4 Eu1 C14 117.17(14) . . ? O1 Eu1 C14 83.40(14) . . ? O4 Eu1 C14 142.19(13) 2_464 . ? O2 Eu1 C14 102.68(15) . . ? O8 Eu1 C14 25.57(14) . . ? O1 Eu1 C14 76.79(13) 2_564 . ? O7 Eu1 C14 26.20(14) . . ? O5 Eu1 C6 136.12(14) . 1_444 ? O6 Eu1 C6 70.87(13) . 1_444 ? O4 Eu1 C6 145.26(13) . 1_444 ? O1 Eu1 C6 90.50(13) . 1_444 ? O4 Eu1 C6 95.93(13) 2_464 1_444 ? O2 Eu1 C6 25.52(13) . 1_444 ? O8 Eu1 C6 111.95(14) . 1_444 ? O1 Eu1 C6 26.18(13) 2_564 1_444 ? O7 Eu1 C6 72.69(13) . 1_444 ? C14 Eu1 C6 90.85(15) . 1_444 ? O5 Eu1 Eu1 71.68(9) . 2_464 ? O6 Eu1 Eu1 68.14(9) . 2_464 ? O4 Eu1 Eu1 38.06(8) . 2_464 ? O1 Eu1 Eu1 105.60(9) . 2_464 ? O4 Eu1 Eu1 36.79(8) 2_464 2_464 ? O2 Eu1 Eu1 106.62(9) . 2_464 ? O8 Eu1 Eu1 122.86(9) . 2_464 ? O1 Eu1 Eu1 141.01(8) 2_564 2_464 ? O7 Eu1 Eu1 146.32(9) . 2_464 ? C14 Eu1 Eu1 141.99(10) . 2_464 ? C6 Eu1 Eu1 125.16(10) 1_444 2_464 ? N2 Ag1 N1 143.06(18) . . ? N2 Ag1 O7 114.92(15) . 2_665 ? N1 Ag1 O7 97.81(16) . 2_665 ? C13 O5 Eu1 133.9(3) 1_455 . ? C6 O1 Eu1 142.7(3) 2_675 . ? C6 O1 Eu1 91.5(3) 2_675 2_564 ? Eu1 O1 Eu1 112.73(14) . 2_564 ? C14 O8 Eu1 94.8(3) . . ? C14 O7 Ag1 120.7(3) . 2_665 ? C14 O7 Eu1 89.1(3) . . ? Ag1 O7 Eu1 136.87(16) 2_665 . ? C5 N1 C1 117.5(5) . . ? C5 N1 Ag1 118.7(4) . . ? C1 N1 Ag1 123.7(4) . . ? C12 N2 C8 117.2(5) . . ? C12 N2 Ag1 121.7(4) . . ? C8 N2 Ag1 121.1(4) . . ? C11 C10 C9 118.1(5) . . ? C11 C10 C14 122.1(4) . . ? C9 C10 C14 119.8(5) . . ? N2 C8 C9 122.8(5) . . ? N2 C8 H2 118.6 . . ? C9 C8 H2 118.6 . . ? N1 C1 C2 122.9(5) . . ? N1 C1 H3 118.6 . . ? C2 C1 H3 118.6 . . ? N2 C12 C11 123.8(5) . . ? N2 C12 H4 118.1 . . ? C11 C12 H4 118.1 . . ? C2 C3 C4 117.3(5) . . ? C2 C3 C7 117.6(5) . . ? C4 C3 C7 124.7(5) . . ? N1 C5 C4 123.0(5) . . ? N1 C5 H6 118.5 . . ? C4 C5 H6 118.5 . . ? C1 C2 C3 120.3(5) . . ? C1 C2 H8 119.8 . . ? C3 C2 H8 119.8 . . ? O8 C14 O7 123.2(5) . . ? O8 C14 C10 117.7(5) . . ? O7 C14 C10 119.1(5) . . ? O8 C14 Eu1 59.6(3) . . ? O7 C14 Eu1 64.7(3) . . ? C10 C14 Eu1 169.5(3) . . ? O3 C7 O4 126.4(5) . 2_675 ? O3 C7 C3 116.7(5) . . ? O4 C7 C3 116.8(5) 2_675 . ? C5 C4 C3 118.9(5) . . ? C5 C4 C6 118.7(5) . . ? C3 C4 C6 122.4(5) . . ? C8 C9 C10 119.6(5) . . ? C8 C9 H13 120.2 . . ? C10 C9 H13 120.2 . . ? C10 C11 C12 118.6(5) . . ? C10 C11 C13 122.7(5) . . ? C12 C11 C13 118.7(5) . . ? C18 C15 N3 121(2) . 2_775 ? C18 C15 C17 121(2) . 2_775 ? N3 C15 C17 0.0(18) 2_775 2_775 ? C18 C15 C16 120(2) . . ? N3 C15 C16 118(2) 2_775 . ? C17 C15 C16 118(2) 2_775 . ? C17 C18 C15 115(2) . . ? C18 C17 C15 124(3) . 2_775 ? O10 O10 O9 161(6) 2_675 . ? O10 O10 C16 28(3) 2_675 2_675 ? O9 O10 C16 133(4) . 2_675 ? O10 O9 C16 29(3) . . ? O9 C16 O10 104(3) . 2_675 ? O9 C16 C15 121(3) . . ? O10 C16 C15 136(3) 2_675 . ? C13 O6 Eu1 138.8(3) 2_564 . ? C6 O2 Eu1 95.3(3) 1_444 . ? C7 O4 Eu1 126.6(3) 2_675 . ? C7 O4 Eu1 118.8(3) 2_675 2_464 ? Eu1 O4 Eu1 105.15(13) . 2_464 ? O2 C6 O1 121.3(5) 1_666 2_675 ? O2 C6 C4 120.1(5) 1_666 . ? O1 C6 C4 118.6(5) 2_675 . ? O2 C6 Eu1 59.2(3) 1_666 1_666 ? O1 C6 Eu1 62.3(3) 2_675 1_666 ? C4 C6 Eu1 176.7(4) . 1_666 ? O6 C13 O5 127.3(5) 2_564 1_655 ? O6 C13 C11 116.6(4) 2_564 . ? O5 C13 C11 116.1(4) 1_655 . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.633 _refine_diff_density_min -2.252 _refine_diff_density_rms 0.160 data_1 _database_code_depnum_ccdc_archive 'CCDC 299742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H9.50 Ag N2.50 Nd O9' _chemical_formula_weight 644.88 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.350(3) _cell_length_b 10.453(4) _cell_length_c 11.652(4) _cell_angle_alpha 100.265(5) _cell_angle_beta 101.038(4) _cell_angle_gamma 96.057(5) _cell_volume 855.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 4.209 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4748 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3395 _reflns_number_gt 2678 _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^)+(0.0615P)^2^+2.2088P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3395 _refine_ls_number_parameters 296 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.24274(6) 0.52743(5) 0.43165(4) 0.01492(19) Uani 1 1 d . . . Ag1 Ag -0.21020(12) -0.25107(9) 0.21199(8) 0.0420(3) Uani 1 1 d . . . O1 O 0.0399(8) 0.3713(6) 0.5032(6) 0.0196(14) Uani 1 1 d . . . O3 O 0.4270(8) 0.3551(6) 0.4832(6) 0.0173(13) Uani 1 1 d . . . O4 O 0.4395(10) 0.2357(7) 0.6250(6) 0.0335(17) Uani 1 1 d . . . O5 O 0.4040(9) 0.4710(7) 0.2715(6) 0.0245(15) Uani 1 1 d . . . N1 N -0.0111(11) -0.0751(8) 0.3056(8) 0.0269(19) Uani 1 1 d . . . C1 C 0.1773(14) -0.0705(9) 0.3221(9) 0.026(2) Uani 1 1 d . . . H1A H 0.2258 -0.1433 0.2883 0.01(2) Uiso 1 1 d R . . C2 C 0.2991(13) 0.0382(9) 0.3873(9) 0.026(2) Uani 1 1 d . . . H2A H 0.4274 0.0383 0.3949 0.04(3) Uiso 1 1 d R . . C3 C 0.2334(12) 0.1490(9) 0.4424(8) 0.0192(19) Uani 1 1 d . . . C4 C 0.0379(12) 0.1455(9) 0.4247(8) 0.0177(19) Uani 1 1 d . . . C5 C -0.0760(14) 0.0307(9) 0.3554(9) 0.025(2) Uani 1 1 d . . . H5A H -0.2052 0.0284 0.3434 0.01(2) Uiso 1 1 d R . . C6 C -0.0540(12) 0.2558(9) 0.4738(8) 0.0175(19) Uani 1 1 d . . . C7 C 0.3751(12) 0.2557(9) 0.5260(8) 0.0185(19) Uani 1 1 d . . . O9 O 0.511(5) -0.022(3) -0.035(2) 0.066(7) Uani 0.50 1 d P . . O10 O 0.543(5) 0.073(3) 0.126(4) 0.125(14) Uani 0.50 1 d P . . N3 N 0.109(4) 0.0908(17) 0.0905(15) 0.099(7) Uani 0.50 1 d P . . C15 C 0.186(3) 0.0105(16) 0.0183(15) 0.084(6) Uani 1 1 d . . . C16 C 0.109(4) 0.0908(17) 0.0905(15) 0.099(7) Uani 0.50 1 d P . . C17 C 0.387(8) 0.017(6) 0.037(7) 0.13(3) Uani 0.50 1 d PU . . C18 C 0.082(4) -0.0843(17) -0.0770(17) 0.103(8) Uani 1 1 d . . . O2 O 0.2149(8) 0.7645(6) 0.5068(6) 0.0233(15) Uani 1 1 d . . . O6 O 0.3076(9) 0.5626(6) 0.6498(6) 0.0216(14) Uani 1 1 d . . . O8 O 0.0304(9) 0.3675(6) 0.2566(6) 0.0251(15) Uani 1 1 d . . . N2 N -0.4591(11) -0.3207(8) 0.0686(7) 0.0233(18) Uani 1 1 d . . . C8 C -0.4443(12) -0.3577(9) -0.0453(8) 0.021(2) Uani 1 1 d . . . C12 C -0.6336(13) -0.3295(10) 0.0910(8) 0.024(2) Uani 1 1 d . . . H8A H -0.3249 -0.3535 -0.0615 0.03(3) Uiso 1 1 d R . . C9 C -0.5956(12) -0.4013(9) -0.1399(8) 0.0197(19) Uani 1 1 d . . . C10 C -0.7748(12) -0.4073(9) -0.1163(8) 0.020(2) Uani 1 1 d . . . C13 C -0.5613(12) -0.4417(8) -0.2650(8) 0.0168(18) Uani 1 1 d . . . C11 C -0.7899(14) -0.3706(9) 0.0004(9) 0.026(2) Uani 1 1 d . . . C14 C -0.9479(12) -0.4536(9) -0.2138(8) 0.0178(19) Uani 1 1 d . . . H11A H -0.9078 -0.3736 0.0183 0.05(3) Uiso 1 1 d R . . H12A H -0.6479 -0.3077 0.1693 0.08(5) Uiso 1 1 d R . . O7 O 0.0098(9) 0.5759(6) 0.2480(6) 0.0246(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0118(3) 0.0163(3) 0.0161(3) 0.00133(18) 0.00338(18) 0.00243(18) Ag1 0.0327(5) 0.0461(6) 0.0341(5) -0.0088(4) -0.0024(4) -0.0060(4) O1 0.015(3) 0.018(3) 0.020(3) -0.003(3) -0.001(3) -0.004(3) O3 0.012(3) 0.015(3) 0.023(3) 0.001(3) 0.004(3) -0.001(2) O4 0.040(4) 0.027(4) 0.026(4) 0.007(3) -0.005(3) -0.005(3) O5 0.018(3) 0.035(4) 0.021(4) 0.000(3) 0.006(3) 0.009(3) N1 0.026(4) 0.017(4) 0.031(5) 0.000(4) 0.000(4) -0.004(3) C1 0.028(5) 0.019(5) 0.031(6) 0.003(4) 0.008(4) 0.009(4) C2 0.019(5) 0.021(5) 0.036(6) 0.003(4) 0.005(4) 0.002(4) C3 0.021(5) 0.015(4) 0.025(5) 0.007(4) 0.008(4) 0.006(4) C4 0.014(4) 0.019(5) 0.018(5) -0.002(4) 0.003(4) 0.000(4) C5 0.023(5) 0.019(5) 0.036(6) 0.006(4) 0.012(4) 0.004(4) C6 0.016(4) 0.017(5) 0.019(5) 0.000(4) 0.004(4) 0.006(4) C7 0.016(4) 0.019(5) 0.019(5) -0.001(4) 0.000(4) 0.004(4) O9 0.10(2) 0.057(17) 0.048(18) 0.005(14) 0.03(2) 0.024(17) O10 0.11(3) 0.10(3) 0.16(4) 0.05(3) -0.02(2) 0.01(2) N3 0.19(2) 0.058(10) 0.052(10) 0.022(8) 0.027(14) 0.019(14) C15 0.159(19) 0.050(9) 0.045(9) 0.008(8) 0.029(11) 0.020(11) C16 0.19(2) 0.058(10) 0.052(10) 0.022(8) 0.027(14) 0.019(14) C17 0.15(5) 0.12(4) 0.21(6) 0.13(4) 0.16(5) 0.09(4) C18 0.21(3) 0.041(10) 0.052(11) 0.016(8) 0.013(15) 0.017(14) O2 0.014(3) 0.022(3) 0.033(4) 0.002(3) 0.009(3) -0.002(3) O6 0.020(3) 0.026(4) 0.019(3) 0.002(3) 0.005(3) 0.005(3) O8 0.018(3) 0.023(4) 0.033(4) 0.002(3) 0.005(3) 0.003(3) N2 0.030(4) 0.021(4) 0.012(4) -0.004(3) -0.003(3) -0.003(4) C8 0.012(4) 0.029(5) 0.021(5) 0.002(4) 0.004(4) 0.005(4) C12 0.023(5) 0.028(5) 0.018(5) -0.002(4) 0.004(4) 0.007(4) C9 0.017(5) 0.021(5) 0.023(5) 0.004(4) 0.007(4) 0.010(4) C10 0.017(4) 0.019(5) 0.026(5) 0.003(4) 0.009(4) 0.003(4) C13 0.022(5) 0.014(4) 0.014(5) 0.000(4) 0.005(4) -0.002(4) C11 0.025(5) 0.024(5) 0.025(5) -0.004(4) 0.005(4) 0.008(4) C14 0.015(4) 0.025(5) 0.014(5) 0.002(4) 0.007(4) 0.002(4) O7 0.020(3) 0.026(4) 0.027(4) 0.007(3) 0.003(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O5 2.416(6) . ? Nd1 O6 2.447(6) . ? Nd1 O3 2.455(6) . ? Nd1 O1 2.455(6) . ? Nd1 O2 2.520(6) . ? Nd1 O3 2.529(6) 2_666 ? Nd1 O8 2.530(7) . ? Nd1 O1 2.607(6) 2_566 ? Nd1 O7 2.633(6) . ? Nd1 C14 2.929(9) 2_455 ? Nd1 C6 2.938(8) 2_566 ? Nd1 Nd1 3.9551(16) 2_666 ? Ag1 N2 2.187(8) . ? Ag1 N1 2.195(8) . ? Ag1 O7 2.587(6) 1_545 ? O1 C6 1.280(10) . ? O1 Nd1 2.607(6) 2_566 ? O3 C7 1.284(11) . ? O3 Nd1 2.529(6) 2_666 ? O4 C7 1.223(11) . ? O5 C13 1.239(10) 2 ? N1 C5 1.333(12) . ? N1 C1 1.355(12) . ? C1 C2 1.374(14) . ? C1 H1A 0.9299 . ? C2 C3 1.400(13) . ? C2 H2A 0.9300 . ? C3 C4 1.407(12) . ? C3 C7 1.502(13) . ? C4 C5 1.406(13) . ? C4 C6 1.480(11) . ? C5 H5A 0.9300 . ? C6 O2 1.249(10) 2_566 ? C6 Nd1 2.938(8) 2_566 ? O9 C17 0.76(5) 2_655 ? O9 O9 0.91(4) 2_655 ? O9 O10 1.08(4) 2_655 ? O9 C17 1.40(6) . ? O10 O9 1.08(4) 2_655 ? O10 C17 1.38(8) . ? N3 C15 1.33(2) . ? N3 C18 1.38(3) 2 ? C15 C18 1.39(3) . ? C15 C17 1.44(6) . ? C17 O9 0.76(5) 2_655 ? C18 C16 1.38(3) 2 ? C18 N3 1.38(3) 2 ? O2 C6 1.249(10) 2_566 ? O6 C13 1.255(11) 1_666 ? O8 C14 1.260(11) 2_455 ? N2 C8 1.344(12) . ? N2 C12 1.354(12) . ? C8 C9 1.380(13) . ? C8 H8A 0.9301 . ? C12 C11 1.375(13) . ? C12 H12A 0.9290 . ? C9 C10 1.393(12) . ? C9 C13 1.520(12) . ? C10 C11 1.374(13) . ? C10 C14 1.505(13) . ? C13 O5 1.239(10) 2 ? C13 O6 1.255(11) 1_444 ? C11 H11A 0.9280 . ? C14 O8 1.260(11) 2_455 ? C14 O7 1.275(11) 2_455 ? C14 Nd1 2.929(9) 2_455 ? O7 C14 1.275(11) 2_455 ? O7 Ag1 2.587(6) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Nd1 O6 138.5(2) . . ? O5 Nd1 O3 73.7(2) . . ? O6 Nd1 O3 74.4(2) . . ? O5 Nd1 O1 125.3(2) . . ? O6 Nd1 O1 67.7(2) . . ? O3 Nd1 O1 72.9(2) . . ? O5 Nd1 O2 119.7(2) . . ? O6 Nd1 O2 73.4(2) . . ? O3 Nd1 O2 140.8(2) . . ? O1 Nd1 O2 113.7(2) . . ? O5 Nd1 O3 76.2(2) . 2_666 ? O6 Nd1 O3 70.4(2) . 2_666 ? O3 Nd1 O3 75.0(2) . 2_666 ? O1 Nd1 O3 132.3(2) . 2_666 ? O2 Nd1 O3 73.51(19) . 2_666 ? O5 Nd1 O8 69.0(2) . . ? O6 Nd1 O8 137.4(2) . . ? O3 Nd1 O8 91.4(2) . . ? O1 Nd1 O8 69.8(2) . . ? O2 Nd1 O8 127.6(2) . . ? O3 Nd1 O8 145.1(2) 2_666 . ? O5 Nd1 O1 146.4(2) . 2_566 ? O6 Nd1 O1 73.9(2) . 2_566 ? O3 Nd1 O1 136.44(19) . 2_566 ? O1 Nd1 O1 67.8(2) . 2_566 ? O2 Nd1 O1 50.75(19) . 2_566 ? O3 Nd1 O1 120.07(19) 2_666 2_566 ? O8 Nd1 O1 92.10(19) . 2_566 ? O5 Nd1 O7 78.1(2) . . ? O6 Nd1 O7 142.2(2) . . ? O3 Nd1 O7 139.3(2) . . ? O1 Nd1 O7 101.7(2) . . ? O2 Nd1 O7 79.1(2) . . ? O3 Nd1 O7 125.48(19) 2_666 . ? O8 Nd1 O7 50.8(2) . . ? O1 Nd1 O7 68.6(2) 2_566 . ? O5 Nd1 C14 74.7(2) . 2_455 ? O6 Nd1 C14 144.6(2) . 2_455 ? O3 Nd1 C14 116.4(2) . 2_455 ? O1 Nd1 C14 83.0(2) . 2_455 ? O2 Nd1 C14 102.8(2) . 2_455 ? O3 Nd1 C14 143.6(2) 2_666 2_455 ? O8 Nd1 C14 25.4(2) . 2_455 ? O1 Nd1 C14 77.0(2) 2_566 2_455 ? O7 Nd1 C14 25.8(2) . 2_455 ? O5 Nd1 C6 138.1(2) . 2_566 ? O6 Nd1 C6 70.6(2) . 2_566 ? O3 Nd1 C6 144.9(2) . 2_566 ? O1 Nd1 C6 90.6(2) . 2_566 ? O2 Nd1 C6 25.0(2) . 2_566 ? O3 Nd1 C6 96.0(2) 2_666 2_566 ? O8 Nd1 C6 112.1(2) . 2_566 ? O1 Nd1 C6 25.8(2) 2_566 2_566 ? O7 Nd1 C6 73.4(2) . 2_566 ? C14 Nd1 C6 91.2(2) 2_455 2_566 ? O5 Nd1 Nd1 70.93(15) . 2_666 ? O6 Nd1 Nd1 67.57(14) . 2_666 ? O3 Nd1 Nd1 38.15(14) . 2_666 ? O1 Nd1 Nd1 104.38(14) . 2_666 ? O2 Nd1 Nd1 107.43(15) . 2_666 ? O3 Nd1 Nd1 36.84(13) 2_666 2_666 ? O8 Nd1 Nd1 122.65(14) . 2_666 ? O1 Nd1 Nd1 140.38(14) 2_566 2_666 ? O7 Nd1 Nd1 147.37(14) . 2_666 ? C14 Nd1 Nd1 142.26(17) 2_455 2_666 ? C6 Nd1 Nd1 125.11(18) 2_566 2_666 ? N2 Ag1 N1 142.9(3) . . ? N2 Ag1 O7 115.0(3) . 1_545 ? N1 Ag1 O7 97.9(3) . 1_545 ? C6 O1 Nd1 142.6(6) . . ? C6 O1 Nd1 91.7(5) . 2_566 ? Nd1 O1 Nd1 112.2(2) . 2_566 ? C7 O3 Nd1 127.5(5) . . ? C7 O3 Nd1 117.1(5) . 2_666 ? Nd1 O3 Nd1 105.0(2) . 2_666 ? C13 O5 Nd1 135.2(6) 2 . ? C5 N1 C1 117.5(8) . . ? C5 N1 Ag1 119.1(7) . . ? C1 N1 Ag1 123.3(6) . . ? N1 C1 C2 122.1(9) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 121.1(9) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.4 . . ? C2 C3 C4 117.1(9) . . ? C2 C3 C7 117.7(8) . . ? C4 C3 C7 124.9(8) . . ? C5 C4 C3 117.8(8) . . ? C5 C4 C6 118.4(8) . . ? C3 C4 C6 123.8(8) . . ? N1 C5 C4 124.3(9) . . ? N1 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? O2 C6 O1 120.7(8) 2_566 . ? O2 C6 C4 120.8(8) 2_566 . ? O1 C6 C4 118.3(8) . . ? O2 C6 Nd1 58.5(4) 2_566 2_566 ? O1 C6 Nd1 62.5(4) . 2_566 ? C4 C6 Nd1 179.0(7) . 2_566 ? O4 C7 O3 126.1(9) . . ? O4 C7 C3 117.2(8) . . ? O3 C7 C3 116.5(8) . . ? C17 O9 O9 114(10) 2_655 2_655 ? C17 O9 O10 97(7) 2_655 2_655 ? O9 O9 O10 149(8) 2_655 2_655 ? C17 O9 C17 144(6) 2_655 . ? O9 O9 C17 30(5) 2_655 . ? O10 O9 C17 120(5) 2_655 . ? O9 O10 C17 33(2) 2_655 . ? C15 N3 C18 122(2) . 2 ? N3 C15 C18 123(2) . . ? N3 C15 C17 121(4) . . ? C18 C15 C17 116(4) . . ? O9 C17 O10 51(6) 2_655 . ? O9 C17 O9 36(6) 2_655 . ? O10 C17 O9 87(4) . . ? O9 C17 C15 169(8) 2_655 . ? O10 C17 C15 138(6) . . ? O9 C17 C15 135(6) . . ? C16 C18 N3 0(2) 2 2 ? C16 C18 C15 115(2) 2 . ? N3 C18 C15 115(2) 2 . ? C6 O2 Nd1 96.5(5) 2_566 . ? C13 O6 Nd1 139.3(6) 1_666 . ? C14 O8 Nd1 95.3(5) 2_455 . ? C8 N2 C12 117.4(8) . . ? C8 N2 Ag1 121.1(6) . . ? C12 N2 Ag1 121.5(6) . . ? N2 C8 C9 123.9(8) . . ? N2 C8 H8A 118.1 . . ? C9 C8 H8A 118.0 . . ? N2 C12 C11 121.3(9) . . ? N2 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C8 C9 C10 118.3(8) . . ? C8 C9 C13 119.2(8) . . ? C10 C9 C13 122.6(8) . . ? C11 C10 C9 117.8(9) . . ? C11 C10 C14 120.2(8) . . ? C9 C10 C14 122.0(8) . . ? O5 C13 O6 127.0(8) 2 1_444 ? O5 C13 C9 116.2(8) 2 . ? O6 C13 C9 116.7(8) 1_444 . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? O8 C14 O7 122.1(8) 2_455 2_455 ? O8 C14 C10 117.6(8) 2_455 . ? O7 C14 C10 120.3(8) 2_455 . ? O8 C14 Nd1 59.4(5) 2_455 2_455 ? O7 C14 Nd1 64.0(5) 2_455 2_455 ? C10 C14 Nd1 169.6(6) . 2_455 ? C14 O7 Ag1 120.4(5) 2_455 1_565 ? C14 O7 Nd1 90.2(5) 2_455 . ? Ag1 O7 Nd1 136.3(3) 1_565 . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.748 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.245 #=======================================================END data_3 _database_code_depnum_ccdc_archive 'CCDC 619370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Ag N3 Nd O7.50' _chemical_formula_weight 642.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.070(4) _cell_length_b 8.8346(19) _cell_length_c 22.339(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3961.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 3.631 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23574 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.20 _reflns_number_total 5050 _reflns_number_gt 3629 _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^)+(0.0357P)^2^+1.4163P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5050 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.233286(12) 0.34953(3) 0.450096(10) 0.02031(8) Uani 1 1 d . . . Ag1 Ag 0.12584(2) 0.08638(4) 0.329800(18) 0.03982(12) Uani 1 1 d . . . C16 C 0.1399(2) 0.5846(5) 0.32808(19) 0.0233(9) Uani 1 1 d . . . O6 O 0.22922(15) 0.5972(3) 0.39944(13) 0.0263(7) Uani 1 1 d . . . O7 O 0.16203(17) 0.3372(3) 0.36740(14) 0.0315(8) Uani 1 1 d . . . O5 O 0.31646(16) 0.3092(3) 0.36951(15) 0.0335(8) Uani 1 1 d . . . N3 N 0.0880(2) 0.3546(4) 0.29241(18) 0.0334(9) Uani 1 1 d . . . O2 O 0.2600(2) 0.2282(5) 0.54827(15) 0.0534(11) Uani 1 1 d . . . O1 O 0.1822(2) 0.5283(4) 0.51700(15) 0.0485(10) Uani 1 1 d . . . C7 C -0.0080(3) 0.1327(6) 0.4014(2) 0.0354(12) Uani 1 1 d . . . H7A H -0.0009 0.2308 0.3877 0.042 Uiso 1 1 calc R . . C17 C 0.1310(2) 0.4251(5) 0.3302(2) 0.0257(10) Uani 1 1 d . . . O4 O 0.13731(17) 0.2096(5) 0.48430(16) 0.0463(10) Uani 1 1 d . . . N2 N 0.03541(19) 0.0256(5) 0.38572(16) 0.0298(9) Uani 1 1 d . . . C5 C 0.1326(3) 0.0786(7) 0.1926(3) 0.0530(16) Uani 1 1 d . . . H5A H 0.0992 0.1488 0.2004 0.064 Uiso 1 1 calc R . . N1 N 0.1661(2) 0.0224(5) 0.23808(18) 0.0399(11) Uani 1 1 d . . . C2 C 0.2281(3) -0.1236(6) 0.1687(2) 0.0457(14) Uani 1 1 d . . . H2A H 0.2619 -0.1939 0.1623 0.055 Uiso 1 1 calc R . . C1 C 0.2133(3) -0.0770(7) 0.2260(2) 0.0444(14) Uani 1 1 d . . . H1A H 0.2376 -0.1174 0.2576 0.053 Uiso 1 1 calc R . . O3 O 0.33099(18) 0.4677(5) 0.48753(16) 0.0469(10) Uani 1 1 d . . . C15 C 0.1008(2) 0.6664(5) 0.2879(2) 0.0311(11) Uani 1 1 d . . . H15A H 0.1047 0.7712 0.2861 0.037 Uiso 1 1 calc R . . C3 C 0.1933(3) -0.0666(5) 0.1215(2) 0.0335(11) Uani 1 1 d . . . C8 C -0.0624(2) 0.1059(6) 0.4366(2) 0.0335(12) Uani 1 1 d . . . H8A H -0.0912 0.1844 0.4466 0.040 Uiso 1 1 calc R . . C11 C 0.0242(2) -0.1153(5) 0.4054(2) 0.0328(11) Uani 1 1 d . . . H11A H 0.0539 -0.1914 0.3948 0.039 Uiso 1 1 calc R . . C14 C 0.0565(3) 0.5934(6) 0.2510(2) 0.0427(14) Uani 1 1 d . . . H14A H 0.0298 0.6473 0.2245 0.051 Uiso 1 1 calc R . . C4 C 0.1448(3) 0.0379(7) 0.1335(2) 0.0506(16) Uani 1 1 d . . . H4A H 0.1203 0.0811 0.1026 0.061 Uiso 1 1 calc R . . C13 C 0.0529(3) 0.4389(6) 0.2545(2) 0.0439(14) Uani 1 1 d . . . H13A H 0.0239 0.3895 0.2285 0.053 Uiso 1 1 calc R . . O1W O 0.0496(4) 0.5050(10) 0.4577(4) 0.065(3) Uani 0.50 1 d P . . C6 C 0.2067(3) -0.1130(6) 0.0570(2) 0.0385(13) Uani 1 1 d . . . C18 C 0.1860(2) 0.6667(5) 0.36724(18) 0.0224(9) Uani 1 1 d . . . C10 C -0.0297(2) -0.1517(5) 0.4407(2) 0.0306(11) Uani 1 1 d . . . H10A H -0.0361 -0.2510 0.4533 0.037 Uiso 1 1 calc R . . C9 C -0.0743(2) -0.0402(6) 0.45731(19) 0.0276(10) Uani 1 1 d . . . C12 C -0.1318(2) -0.0758(7) 0.4988(2) 0.0349(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02352(13) 0.01948(13) 0.01793(12) 0.00121(9) -0.00019(9) 0.00265(10) Ag1 0.0546(3) 0.0284(2) 0.0365(2) -0.00591(17) 0.02235(19) -0.00904(19) C16 0.028(2) 0.021(2) 0.020(2) 0.0009(18) -0.0050(18) -0.0020(19) O6 0.0301(17) 0.0222(16) 0.0266(17) 0.0001(13) -0.0119(14) -0.0004(14) O7 0.0398(19) 0.0171(16) 0.0377(19) 0.0051(14) -0.0156(15) 0.0006(15) O5 0.041(2) 0.0159(16) 0.043(2) -0.0019(14) 0.0170(16) -0.0007(14) N3 0.043(2) 0.024(2) 0.033(2) -0.0006(18) -0.0132(19) -0.0039(19) O2 0.082(3) 0.045(3) 0.033(2) 0.0143(18) -0.020(2) 0.003(2) O1 0.066(3) 0.052(3) 0.027(2) -0.0082(18) 0.0070(18) 0.022(2) C7 0.046(3) 0.029(3) 0.032(3) 0.007(2) 0.005(2) -0.002(2) C17 0.029(2) 0.024(2) 0.024(2) -0.0020(19) -0.0028(19) 0.002(2) O4 0.032(2) 0.056(3) 0.051(2) 0.021(2) 0.0060(17) -0.0078(18) N2 0.031(2) 0.034(2) 0.024(2) 0.0039(17) 0.0027(17) -0.0013(18) C5 0.064(4) 0.053(4) 0.043(3) -0.001(3) 0.012(3) 0.029(3) N1 0.056(3) 0.035(3) 0.028(2) -0.0046(19) 0.008(2) 0.005(2) C2 0.054(4) 0.049(4) 0.034(3) -0.003(2) 0.008(3) 0.014(3) C1 0.051(3) 0.057(4) 0.026(3) -0.001(2) 0.003(2) 0.011(3) O3 0.037(2) 0.059(3) 0.044(2) -0.0035(19) -0.0156(17) -0.0078(19) C15 0.038(3) 0.019(2) 0.036(3) 0.002(2) -0.011(2) -0.001(2) C3 0.043(3) 0.027(3) 0.031(3) -0.002(2) 0.010(2) -0.006(2) C8 0.029(3) 0.034(3) 0.037(3) 0.006(2) 0.010(2) 0.010(2) C11 0.029(3) 0.030(3) 0.040(3) -0.002(2) 0.008(2) 0.002(2) C14 0.057(4) 0.035(3) 0.036(3) 0.002(2) -0.027(3) 0.004(3) C4 0.065(4) 0.055(4) 0.032(3) 0.004(3) 0.002(3) 0.023(3) C13 0.057(4) 0.032(3) 0.042(3) -0.002(2) -0.025(3) -0.002(3) O1W 0.052(5) 0.058(6) 0.084(6) 0.018(5) 0.019(5) 0.023(5) C6 0.051(3) 0.038(3) 0.026(3) -0.008(2) 0.012(2) -0.020(3) C18 0.025(2) 0.024(2) 0.018(2) 0.0025(18) -0.0009(17) -0.0028(19) C10 0.030(3) 0.025(2) 0.037(3) 0.004(2) 0.004(2) -0.005(2) C9 0.023(2) 0.036(3) 0.023(2) 0.001(2) 0.0011(18) -0.003(2) C12 0.028(3) 0.052(4) 0.025(3) 0.001(2) 0.002(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O7 2.339(3) . ? Nd1 O3 2.374(4) . ? Nd1 O6 2.465(3) . ? Nd1 O4 2.413(3) . ? Nd1 O5 2.481(3) . ? Nd1 O2 2.499(3) . ? Nd1 O1 2.404(3) . ? Nd1 O6 2.610(3) 8_655 ? Nd1 C18 2.943(4) 8_655 ? Ag1 N2 2.268(4) . ? Ag1 N1 2.274(4) . ? Ag1 O7 2.478(3) . ? Ag1 N3 2.625(4) . ? C16 C15 1.394(6) . ? C16 C17 1.422(6) . ? C16 C18 1.465(6) . ? O6 C18 1.283(5) . ? O6 Nd1 2.610(3) 8_665 ? O7 C17 1.297(5) . ? O5 C18 1.261(5) 8_655 ? N3 C13 1.330(6) . ? N3 C17 1.359(6) . ? O2 C6 1.233(7) 2 ? O1 C6 1.264(7) 7_566 ? C7 N2 1.333(6) . ? C7 C8 1.366(6) . ? O4 C12 1.246(6) 5_556 ? N2 C11 1.339(6) . ? C5 N1 1.315(7) . ? C5 C4 1.391(7) . ? N1 C1 1.319(7) . ? C2 C3 1.362(7) . ? C2 C1 1.377(7) . ? O3 C12 1.250(6) 4_556 ? C15 C14 1.373(6) . ? C3 C4 1.369(7) . ? C3 C6 1.523(7) . ? C8 C9 1.392(7) . ? C11 C10 1.376(6) . ? C14 C13 1.370(7) . ? C6 O1 1.264(7) 7_565 ? C6 O2 1.233(7) 2_554 ? C18 O5 1.261(5) 8_665 ? C18 Nd1 2.943(4) 8_665 ? C10 C9 1.381(7) . ? C9 C12 1.514(6) . ? C12 O4 1.246(6) 5_556 ? C12 O3 1.250(6) 4_456 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Nd1 O3 143.51(12) . . ? O7 Nd1 O6 70.04(10) . . ? O3 Nd1 O6 78.38(12) . . ? O7 Nd1 O4 74.81(12) . . ? O3 Nd1 O4 140.65(13) . . ? O6 Nd1 O4 125.02(12) . . ? O7 Nd1 O5 80.30(12) . . ? O3 Nd1 O5 76.29(12) . . ? O6 Nd1 O5 79.44(10) . . ? O4 Nd1 O5 133.88(12) . . ? O7 Nd1 O2 143.56(13) . . ? O3 Nd1 O2 72.66(14) . . ? O6 Nd1 O2 142.24(12) . . ? O4 Nd1 O2 70.97(13) . . ? O5 Nd1 O2 115.50(13) . . ? O7 Nd1 O1 105.13(12) . . ? O3 Nd1 O1 81.05(14) . . ? O6 Nd1 O1 71.83(12) . . ? O4 Nd1 O1 78.42(14) . . ? O5 Nd1 O1 146.37(12) . . ? O2 Nd1 O1 80.08(13) . . ? O7 Nd1 O6 78.11(10) . 8_655 ? O3 Nd1 O6 106.86(12) . 8_655 ? O6 Nd1 O6 124.65(12) . 8_655 ? O4 Nd1 O6 85.97(12) . 8_655 ? O5 Nd1 O6 50.86(9) . 8_655 ? O2 Nd1 O6 87.26(12) . 8_655 ? O1 Nd1 O6 162.42(12) . 8_655 ? O7 Nd1 C18 79.28(12) . 8_655 ? O3 Nd1 C18 90.48(13) . 8_655 ? O6 Nd1 C18 102.53(11) . 8_655 ? O4 Nd1 C18 110.92(13) . 8_655 ? O5 Nd1 C18 25.08(10) . 8_655 ? O2 Nd1 C18 101.43(13) . 8_655 ? O1 Nd1 C18 170.57(14) . 8_655 ? O6 Nd1 C18 25.83(10) 8_655 8_655 ? N2 Ag1 N1 136.22(15) . . ? N2 Ag1 O7 105.04(13) . . ? N1 Ag1 O7 115.05(14) . . ? N2 Ag1 N3 99.04(14) . . ? N1 Ag1 N3 92.33(15) . . ? O7 Ag1 N3 52.10(11) . . ? C15 C16 C17 117.7(4) . . ? C15 C16 C18 118.9(4) . . ? C17 C16 C18 123.4(4) . . ? C18 O6 Nd1 134.8(3) . . ? C18 O6 Nd1 91.7(2) . 8_665 ? Nd1 O6 Nd1 123.33(12) . 8_665 ? C17 O7 Nd1 140.5(3) . . ? C17 O7 Ag1 100.2(3) . . ? Nd1 O7 Ag1 119.26(12) . . ? C18 O5 Nd1 98.4(3) 8_655 . ? C13 N3 C17 118.4(4) . . ? C13 N3 Ag1 149.5(3) . . ? C17 N3 Ag1 91.8(3) . . ? C6 O2 Nd1 127.5(4) 2 . ? C6 O1 Nd1 131.5(4) 7_566 . ? N2 C7 C8 123.4(5) . . ? O7 C17 N3 115.4(4) . . ? O7 C17 C16 123.7(4) . . ? N3 C17 C16 120.9(4) . . ? C12 O4 Nd1 130.8(3) 5_556 . ? C11 N2 C7 117.6(4) . . ? C11 N2 Ag1 122.4(3) . . ? C7 N2 Ag1 120.0(3) . . ? N1 C5 C4 123.1(5) . . ? C5 N1 C1 117.4(4) . . ? C5 N1 Ag1 114.8(4) . . ? C1 N1 Ag1 127.2(4) . . ? C3 C2 C1 119.9(5) . . ? N1 C1 C2 123.0(5) . . ? C12 O3 Nd1 156.3(4) 4_556 . ? C14 C15 C16 120.5(4) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 C6 119.5(5) . . ? C2 C3 C6 122.9(5) . . ? C7 C8 C9 119.2(4) . . ? N2 C11 C10 122.5(4) . . ? C15 C14 C13 118.0(5) . . ? C3 C4 C5 119.0(5) . . ? N3 C13 C14 124.5(5) . . ? O1 C6 O2 126.0(5) 7_565 2_554 ? O1 C6 C3 116.2(5) 7_565 . ? O2 C6 C3 117.8(5) 2_554 . ? O5 C18 O6 118.8(4) 8_665 . ? O5 C18 C16 119.5(4) 8_665 . ? O6 C18 C16 121.7(4) . . ? O5 C18 Nd1 56.5(2) 8_665 8_665 ? O6 C18 Nd1 62.5(2) . 8_665 ? C16 C18 Nd1 174.1(3) . 8_665 ? C11 C10 C9 119.7(4) . . ? C10 C9 C8 117.5(4) . . ? C10 C9 C12 120.7(5) . . ? C8 C9 C12 121.8(4) . . ? O4 C12 O3 126.7(5) 5_556 4_456 ? O4 C12 C9 116.8(5) 5_556 . ? O3 C12 C9 116.5(5) 4_456 . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 29.20 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.924 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.149 #=========================================================END data_4 _database_code_depnum_ccdc_archive 'CCDC 619371' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 Ag Eu N3 O7.50' _chemical_formula_weight 650.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.954(2) _cell_length_b 8.8187(9) _cell_length_c 22.344(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3931.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 4.207 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23107 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.15 _reflns_number_total 4944 _reflns_number_gt 4210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+3.3561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4944 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.232968(7) 0.154133(16) 0.449677(6) 0.01852(5) Uani 1 1 d . . . Ag1 Ag 0.128059(14) 0.41935(3) 0.331135(12) 0.03668(8) Uani 1 1 d . . . O6 O 0.22950(10) -0.0944(2) 0.40182(9) 0.0234(4) Uani 1 1 d . . . O1 O 0.26206(14) 0.2810(3) 0.54411(10) 0.0424(6) Uani 1 1 d . . . O5 O 0.31567(11) 0.1940(2) 0.37067(10) 0.0317(5) Uani 1 1 d . . . N3 N 0.08837(15) 0.1487(3) 0.29306(13) 0.0335(6) Uani 1 1 d . . . O7 O 0.16319(12) 0.1666(2) 0.36768(10) 0.0307(5) Uani 1 1 d . . . O2 O 0.18003(12) -0.0140(3) 0.51695(10) 0.0379(6) Uani 1 1 d . . . N2 N 0.03567(13) 0.4778(3) 0.38564(11) 0.0290(6) Uani 1 1 d . . . O3 O 0.13948(11) 0.2974(3) 0.48188(11) 0.0397(6) Uani 1 1 d . . . C7 C -0.00765(17) 0.3682(4) 0.40062(15) 0.0329(7) Uani 1 1 d . . . H7A H -0.0001 0.2707 0.3863 0.039 Uiso 1 1 calc R . . O4 O 0.32978(11) 0.0392(3) 0.48757(11) 0.0400(6) Uani 1 1 d . . . N1 N 0.16719(16) 0.4818(3) 0.23828(12) 0.0377(7) Uani 1 1 d . . . C17 C 0.13209(14) 0.0788(3) 0.33074(13) 0.0228(6) Uani 1 1 d . . . C11 C 0.02343(16) 0.6174(4) 0.40656(14) 0.0305(7) Uani 1 1 d . . . H11A H 0.0529 0.6951 0.3965 0.037 Uiso 1 1 calc R . . C8 C -0.06316(17) 0.3933(4) 0.43632(15) 0.0333(7) Uani 1 1 d . . . H8A H -0.0921 0.3141 0.4456 0.040 Uiso 1 1 calc R . . C1 C 0.1330(2) 0.4224(5) 0.19373(17) 0.0488(10) Uani 1 1 d . . . H1A H 0.0994 0.3529 0.2027 0.059 Uiso 1 1 calc R . . C14 C 0.0567(2) -0.0917(4) 0.25168(17) 0.0422(9) Uani 1 1 d . . . H14A H 0.0301 -0.1462 0.2251 0.051 Uiso 1 1 calc R . . C5 C 0.2145(2) 0.5819(5) 0.22450(16) 0.0451(9) Uani 1 1 d . . . H5A H 0.2398 0.6239 0.2552 0.054 Uiso 1 1 calc R . . C13 C 0.05310(19) 0.0641(4) 0.25511(16) 0.0412(9) Uani 1 1 d . . . H13A H 0.0240 0.1135 0.2291 0.049 Uiso 1 1 calc R . . O1W O 0.0486(4) -0.0023(9) 0.4566(3) 0.076(2) Uani 0.50 1 d P . . C9 C -0.07502(14) 0.5377(4) 0.45804(13) 0.0252(6) Uani 1 1 d . . . C12 C -0.13305(14) 0.5701(4) 0.49961(14) 0.0289(7) Uani 1 1 d . . . C10 C -0.03116(16) 0.6513(4) 0.44251(14) 0.0294(7) Uani 1 1 d . . . H10A H -0.0380 0.7499 0.4560 0.035 Uiso 1 1 calc R . . C2 C 0.1442(2) 0.4577(5) 0.13408(16) 0.0492(10) Uani 1 1 d . . . H2A H 0.1196 0.4107 0.1040 0.059 Uiso 1 1 calc R . . C3 C 0.19239(17) 0.5633(4) 0.12009(14) 0.0297(7) Uani 1 1 d . . . C4 C 0.2277(2) 0.6261(5) 0.16605(16) 0.0440(9) Uani 1 1 d . . . H4A H 0.2605 0.6985 0.1583 0.053 Uiso 1 1 calc R . . C6 C 0.20503(18) 0.6029(4) 0.05519(13) 0.0308(7) Uani 1 1 d . . . C15 C 0.10145(17) -0.1634(4) 0.28937(15) 0.0319(7) Uani 1 1 d . . . H15A H 0.1057 -0.2684 0.2880 0.038 Uiso 1 1 calc R . . C16 C 0.14015(14) -0.0807(3) 0.32927(13) 0.0222(6) Uani 1 1 d . . . C18 C 0.18694(14) -0.1634(3) 0.36901(12) 0.0199(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02102(8) 0.01731(8) 0.01722(8) -0.00126(5) -0.00006(5) -0.00172(5) Ag1 0.04926(16) 0.02712(14) 0.03366(14) 0.00498(10) 0.01997(11) 0.00765(12) O6 0.0281(10) 0.0173(10) 0.0247(11) -0.0026(8) -0.0078(8) 0.0007(8) O1 0.0634(18) 0.0336(14) 0.0302(13) -0.0093(11) -0.0155(12) -0.0019(13) O5 0.0374(12) 0.0170(10) 0.0407(13) 0.0024(9) 0.0158(10) 0.0018(9) N3 0.0408(16) 0.0232(14) 0.0364(15) 0.0021(12) -0.0128(13) 0.0036(12) O7 0.0418(13) 0.0191(11) 0.0312(12) -0.0028(9) -0.0140(10) 0.0014(10) O2 0.0491(14) 0.0391(14) 0.0255(12) 0.0062(10) 0.0070(10) -0.0100(12) N2 0.0274(13) 0.0323(15) 0.0273(13) -0.0014(11) 0.0051(11) 0.0018(12) O3 0.0320(12) 0.0420(15) 0.0452(15) -0.0134(12) 0.0088(11) 0.0063(11) C7 0.0359(17) 0.0274(17) 0.0354(18) -0.0089(14) 0.0069(14) 0.0004(14) O4 0.0308(12) 0.0456(15) 0.0436(14) 0.0005(12) -0.0147(11) 0.0017(11) N1 0.0540(18) 0.0348(16) 0.0243(14) 0.0020(12) 0.0082(13) -0.0031(14) C17 0.0245(14) 0.0218(14) 0.0220(14) 0.0012(11) -0.0042(11) 0.0013(12) C11 0.0277(15) 0.0314(17) 0.0325(17) 0.0025(13) 0.0058(13) -0.0034(14) C8 0.0301(16) 0.0323(18) 0.0376(18) -0.0041(14) 0.0097(14) -0.0069(15) C1 0.062(2) 0.050(2) 0.034(2) 0.0025(17) 0.0110(18) -0.025(2) C14 0.053(2) 0.0292(18) 0.044(2) -0.0026(15) -0.0267(17) -0.0037(17) C5 0.054(2) 0.054(3) 0.0278(18) 0.0004(16) 0.0023(16) -0.019(2) C13 0.052(2) 0.0312(19) 0.041(2) 0.0019(15) -0.0265(17) 0.0042(17) O1W 0.066(4) 0.075(5) 0.088(5) -0.013(4) 0.016(4) -0.025(4) C9 0.0190(13) 0.0310(16) 0.0255(15) -0.0019(12) 0.0030(11) 0.0024(12) C12 0.0204(14) 0.0397(19) 0.0266(16) 0.0001(13) 0.0009(12) 0.0050(14) C10 0.0293(15) 0.0268(16) 0.0320(17) -0.0029(13) 0.0036(13) 0.0038(13) C2 0.065(3) 0.054(2) 0.0286(18) -0.0028(17) 0.0059(17) -0.026(2) C3 0.0393(17) 0.0258(16) 0.0241(15) 0.0014(12) 0.0112(13) 0.0020(14) C4 0.050(2) 0.052(2) 0.0302(19) 0.0021(16) 0.0052(16) -0.0193(18) C6 0.0407(18) 0.0297(17) 0.0219(15) 0.0039(12) 0.0098(13) 0.0129(15) C15 0.0408(18) 0.0192(15) 0.0357(17) -0.0008(13) -0.0139(15) -0.0008(14) C16 0.0252(14) 0.0210(14) 0.0205(14) -0.0010(11) -0.0035(11) -0.0005(12) C18 0.0239(13) 0.0176(13) 0.0182(13) -0.0004(10) -0.0012(11) 0.0003(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O7 2.304(2) . ? Eu1 O4 2.340(2) . ? Eu1 O2 2.361(2) . ? Eu1 O3 2.365(2) . ? Eu1 O6 2.440(2) . ? Eu1 O5 2.442(2) . ? Eu1 O1 2.458(2) . ? Eu1 O6 2.573(2) 8_665 ? Eu1 C18 2.897(3) 8_665 ? Eu1 Eu1 4.4614(4) 8_655 ? Eu1 Eu1 4.4614(4) 8_665 ? Ag1 N2 2.269(3) . ? Ag1 N1 2.284(3) . ? Ag1 O7 2.475(2) . ? O6 C18 1.276(3) . ? O6 Eu1 2.573(2) 8_655 ? O1 C6 1.241(5) 2_565 ? O5 C18 1.259(3) 8_665 ? N3 C13 1.331(4) . ? N3 C17 1.360(4) . ? O7 C17 1.291(3) . ? O2 C6 1.262(4) 7_566 ? N2 C7 1.339(4) . ? N2 C11 1.339(4) . ? O3 C12 1.246(4) 5_566 ? C7 C8 1.383(4) . ? O4 C12 1.250(4) 4_556 ? N1 C1 1.316(5) . ? N1 C5 1.329(5) . ? C17 C16 1.416(4) . ? C11 C10 1.386(4) . ? C8 C9 1.383(5) . ? C1 C2 1.387(5) . ? C14 C13 1.378(5) . ? C14 C15 1.381(5) . ? C5 C4 1.388(5) . ? C9 C10 1.375(5) . ? C9 C12 1.512(4) . ? C12 O3 1.246(4) 5_566 ? C12 O4 1.250(4) 4_456 ? C2 C3 1.374(5) . ? C3 C4 1.363(5) . ? C3 C6 1.513(4) . ? C6 O1 1.241(5) 2_564 ? C6 O2 1.262(4) 7_565 ? C15 C16 1.387(4) . ? C16 C18 1.481(4) . ? C18 O5 1.259(3) 8_655 ? C18 Eu1 2.897(3) 8_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Eu1 O4 143.84(8) . . ? O7 Eu1 O2 105.42(8) . . ? O4 Eu1 O2 82.35(9) . . ? O7 Eu1 O3 74.91(8) . . ? O4 Eu1 O3 140.57(9) . . ? O2 Eu1 O3 77.81(9) . . ? O7 Eu1 O6 71.17(7) . . ? O4 Eu1 O6 78.05(8) . . ? O2 Eu1 O6 72.66(8) . . ? O3 Eu1 O6 126.22(8) . . ? O7 Eu1 O5 80.02(9) . . ? O4 Eu1 O5 76.47(8) . . ? O2 Eu1 O5 148.54(8) . . ? O3 Eu1 O5 132.53(8) . . ? O6 Eu1 O5 80.31(7) . . ? O7 Eu1 O1 143.48(8) . . ? O4 Eu1 O1 72.04(9) . . ? O2 Eu1 O1 81.09(9) . . ? O3 Eu1 O1 71.46(9) . . ? O6 Eu1 O1 142.37(8) . . ? O5 Eu1 O1 113.29(9) . . ? O7 Eu1 O6 78.71(7) . 8_665 ? O4 Eu1 O6 106.46(8) . 8_665 ? O2 Eu1 O6 159.40(8) . 8_665 ? O3 Eu1 O6 84.01(8) . 8_665 ? O6 Eu1 O6 126.89(8) . 8_665 ? O5 Eu1 O6 51.60(6) . 8_665 ? O1 Eu1 O6 84.01(8) . 8_665 ? O7 Eu1 C18 79.17(8) . 8_665 ? O4 Eu1 C18 90.59(8) . 8_665 ? O2 Eu1 C18 172.67(8) . 8_665 ? O3 Eu1 C18 109.13(9) . 8_665 ? O6 Eu1 C18 104.00(7) . 8_665 ? O5 Eu1 C18 25.50(7) . 8_665 ? O1 Eu1 C18 98.68(9) . 8_665 ? O6 Eu1 C18 26.13(7) 8_665 8_665 ? O7 Eu1 Eu1 98.01(5) . 8_655 ? O4 Eu1 Eu1 56.37(6) . 8_655 ? O2 Eu1 Eu1 56.45(6) . 8_655 ? O3 Eu1 Eu1 130.39(6) . 8_655 ? O6 Eu1 Eu1 27.92(5) . 8_655 ? O5 Eu1 Eu1 92.26(5) . 8_655 ? O1 Eu1 Eu1 114.46(7) . 8_655 ? O6 Eu1 Eu1 143.84(4) 8_665 8_655 ? C18 Eu1 Eu1 117.71(5) 8_665 8_655 ? O7 Eu1 Eu1 92.57(5) . 8_665 ? O4 Eu1 Eu1 107.59(6) . 8_665 ? O2 Eu1 Eu1 133.55(6) . 8_665 ? O3 Eu1 Eu1 65.94(6) . 8_665 ? O6 Eu1 Eu1 153.15(5) . 8_665 ? O5 Eu1 Eu1 75.80(5) . 8_665 ? O1 Eu1 Eu1 60.92(7) . 8_665 ? O6 Eu1 Eu1 26.36(4) 8_665 8_665 ? C18 Eu1 Eu1 50.72(5) 8_665 8_665 ? Eu1 Eu1 Eu1 162.474(7) 8_655 8_665 ? N2 Ag1 N1 135.29(11) . . ? N2 Ag1 O7 104.93(9) . . ? N1 Ag1 O7 114.82(10) . . ? C18 O6 Eu1 134.33(18) . . ? C18 O6 Eu1 91.24(16) . 8_655 ? Eu1 O6 Eu1 125.72(8) . 8_655 ? C6 O1 Eu1 132.2(2) 2_565 . ? C18 O5 Eu1 97.88(18) 8_665 . ? C13 N3 C17 118.7(3) . . ? C17 O7 Eu1 140.40(19) . . ? C17 O7 Ag1 101.13(17) . . ? Eu1 O7 Ag1 118.46(8) . . ? C6 O2 Eu1 130.1(2) 7_566 . ? C7 N2 C11 117.3(3) . . ? C7 N2 Ag1 119.7(2) . . ? C11 N2 Ag1 123.0(2) . . ? C12 O3 Eu1 133.1(2) 5_566 . ? N2 C7 C8 123.1(3) . . ? C12 O4 Eu1 155.1(2) 4_556 . ? C1 N1 C5 117.3(3) . . ? C1 N1 Ag1 114.4(2) . . ? C5 N1 Ag1 127.8(2) . . ? O7 C17 N3 115.6(3) . . ? O7 C17 C16 123.8(3) . . ? N3 C17 C16 120.6(3) . . ? N2 C11 C10 123.0(3) . . ? C7 C8 C9 119.1(3) . . ? N1 C1 C2 123.6(3) . . ? C13 C14 C15 117.2(3) . . ? N1 C5 C4 122.6(4) . . ? N3 C13 C14 124.5(3) . . ? C10 C9 C8 118.3(3) . . ? C10 C9 C12 120.3(3) . . ? C8 C9 C12 121.4(3) . . ? O3 C12 O4 125.9(3) 5_566 4_456 ? O3 C12 C9 117.4(3) 5_566 . ? O4 C12 C9 116.7(3) 4_456 . ? C9 C10 C11 119.3(3) . . ? C3 C2 C1 119.0(4) . . ? C4 C3 C2 117.7(3) . . ? C4 C3 C6 122.8(3) . . ? C2 C3 C6 119.4(3) . . ? C3 C4 C5 119.8(3) . . ? O1 C6 O2 125.9(3) 2_564 7_565 ? O1 C6 C3 118.0(3) 2_564 . ? O2 C6 C3 116.1(3) 7_565 . ? C14 C15 C16 120.7(3) . . ? C15 C16 C17 118.3(3) . . ? C15 C16 C18 118.5(3) . . ? C17 C16 C18 123.2(3) . . ? O5 C18 O6 119.1(3) 8_655 . ? O5 C18 C16 118.9(3) 8_655 . ? O6 C18 C16 122.0(2) . . ? O5 C18 Eu1 56.61(15) 8_655 8_655 ? O6 C18 Eu1 62.63(14) . 8_655 ? C16 C18 Eu1 174.1(2) . 8_655 ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.926 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.111 #======================================================END