# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- complete_incl_ins.cif' # 1. Submission Details _publ_contact_author_name 'Ullrich Englert' _publ_contact_author_address ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; _publ_contact_author_email ullrich.englert@ac.rwth-aachen.de _publ_contact_author_fax 0049-241-8092288 _publ_contact_author_phone 0049-241-8094666 _publ_requested_category FP _publ_requested_coeditor_name ? _publ_contact_letter ; ?? ; # 2. Processing Summary (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. Titl and Author List _publ_section_title ; Ordered Bimetallic Coordination Networks featuring Rare Earth and Silver Cations ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' C.Merkens ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; U.Englert ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; # 4. Text _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Program for Reduction of Data Collected on Bruker CCD Area Detector Diffractometer, Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Program for Bruker CCD X-ray Diffractometer Control. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ; _publ_section_acknowledgements ; ; data_1a _database_code_depnum_ccdc_archive 'CCDC 845893' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1a _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Ce N3 O8' _chemical_formula_sum 'C18 H22 Ce N3 O8' _chemical_formula_weight 548.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 18.4080(25) _cell_length_b 9.2193(13) _cell_length_c 12.2629(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.1776(18) _cell_angle_gamma 90.00 _cell_volume 2075.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8128 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.68 _exptl_crystal_description plate _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 2.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5160 _exptl_absorpt_correction_T_max 0.8068 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12059 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.70 _reflns_number_total 3204 _reflns_number_gt 3108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0218P)^2^+1.9136P] 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 3204 _refine_ls_number_parameters 144 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0445 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Ce1 Ce 0.5000 0.129237(11) 0.2500 0.00822(4) Uani 1 2 d S . . O1 O 0.56222(6) -0.08802(12) 0.32321(9) 0.0133(2) Uani 1 1 d . . . O2 O 0.43170(6) 0.21654(12) 0.07843(8) 0.0129(2) Uani 1 1 d . . . O3 O 0.37731(6) 0.21987(12) 0.28327(9) 0.0154(2) Uani 1 1 d . . . C1 C 0.59232(9) -0.30842(17) 0.41341(13) 0.0175(3) Uani 1 1 d . . . H1A H 0.6339 -0.2518 0.4442 0.026 Uiso 1 1 calc R . . H1B H 0.6098 -0.3984 0.3818 0.026 Uiso 1 1 calc R . . H1C H 0.5602 -0.3317 0.4713 0.026 Uiso 1 1 calc R . . C2 C 0.55086(8) -0.22142(15) 0.32573(12) 0.0114(2) Uani 1 1 d . . . C3 C 0.5000 -0.2939(2) 0.2500 0.0120(4) Uani 1 2 d S . . C4 C 0.5000 -0.4476(2) 0.2500 0.0133(4) Uani 1 2 d S . . C5 C 0.36557(9) 0.34021(18) -0.06591(12) 0.0156(3) Uani 1 1 d . . . H5C H 0.3913 0.4320 -0.0749 0.023 Uiso 1 1 calc R . . H5D H 0.3135 0.3539 -0.0858 0.023 Uiso 1 1 calc R . . H5E H 0.3849 0.2663 -0.1134 0.023 Uiso 1 1 calc R . . C6 C 0.37629(8) 0.29174(15) 0.05144(11) 0.0109(2) Uani 1 1 d . . . C7 C 0.32407(8) 0.33475(16) 0.12587(12) 0.0115(2) Uani 1 1 d . . . C8 C 0.32649(8) 0.29244(16) 0.23813(12) 0.0120(3) Uani 1 1 d . . . C9 C 0.26411(9) 0.33370(19) 0.30506(13) 0.0181(3) Uani 1 1 d . . . H9A H 0.2210 0.2766 0.2810 0.027 Uiso 1 1 calc R . . H9B H 0.2533 0.4372 0.2952 0.027 Uiso 1 1 calc R . . H9C H 0.2775 0.3142 0.3825 0.027 Uiso 1 1 calc R . . C10 C 0.26482(8) 0.42514(16) 0.08554(12) 0.0128(3) Uani 1 1 d . . . N1 N 0.5000 -0.5731(2) 0.2500 0.0187(4) Uani 1 2 d S . . N2 N 0.21755(7) 0.49946(16) 0.05516(11) 0.0182(3) Uani 1 1 d . . . O4 O 0.43866(6) 0.02061(13) 0.41475(9) 0.0146(2) Uani 1 1 d D . . H4A H 0.3978(11) 0.036(3) 0.422(2) 0.035(7) Uiso 1 1 d D . . H4B H 0.4469(14) -0.043(2) 0.4556(18) 0.035(7) 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 Ce1 0.00883(6) 0.00696(6) 0.00874(6) 0.000 -0.00028(4) 0.000 O1 0.0137(5) 0.0099(5) 0.0160(5) 0.0000(4) -0.0016(4) 0.0001(4) O2 0.0117(5) 0.0147(5) 0.0121(5) 0.0000(4) 0.0003(4) 0.0036(4) O3 0.0143(5) 0.0178(5) 0.0143(5) 0.0043(4) 0.0018(4) 0.0041(4) C1 0.0208(7) 0.0137(7) 0.0174(7) 0.0029(5) -0.0026(6) 0.0032(6) C2 0.0119(6) 0.0106(6) 0.0120(6) 0.0004(5) 0.0030(5) 0.0024(5) C3 0.0131(9) 0.0101(9) 0.0131(9) 0.000 0.0027(7) 0.000 C4 0.0131(9) 0.0142(9) 0.0128(9) 0.000 0.0017(7) 0.000 C5 0.0161(7) 0.0196(7) 0.0111(6) 0.0023(5) 0.0010(5) 0.0035(6) C6 0.0110(6) 0.0100(6) 0.0115(6) -0.0002(5) 0.0004(5) -0.0005(5) C7 0.0098(6) 0.0125(6) 0.0123(6) 0.0002(5) 0.0006(5) 0.0016(5) C8 0.0112(6) 0.0120(6) 0.0128(6) -0.0006(5) 0.0012(5) -0.0007(5) C9 0.0158(7) 0.0248(8) 0.0142(7) 0.0004(6) 0.0038(5) 0.0049(6) C10 0.0118(6) 0.0141(6) 0.0127(6) 0.0001(5) 0.0026(5) -0.0002(5) N1 0.0183(9) 0.0142(9) 0.0228(9) 0.000 -0.0037(7) 0.000 N2 0.0148(6) 0.0216(7) 0.0184(6) 0.0015(5) 0.0020(5) 0.0040(5) O4 0.0118(5) 0.0173(5) 0.0148(5) 0.0064(4) 0.0010(4) -0.0001(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 Ce1 O1 2.4454(11) 6_656 ? Ce1 O1 2.4454(11) . ? Ce1 O3 2.4697(11) . ? Ce1 O3 2.4697(11) 6_656 ? Ce1 O2 2.5039(10) . ? Ce1 O2 2.5040(11) 6_656 ? Ce1 O4 2.5869(11) . ? Ce1 O4 2.5869(11) 6_656 ? Ce1 N1 2.744(2) 1_565 ? O1 C2 1.2482(18) . ? O2 C6 1.2577(17) . ? O3 C8 1.2465(18) . ? C1 C2 1.504(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.4347(17) . ? C3 C4 1.417(3) . ? C3 C2 1.4346(17) 6_656 ? C4 N1 1.157(3) . ? C5 C6 1.506(2) . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C6 C7 1.429(2) . ? C7 C8 1.428(2) . ? C7 C10 1.432(2) . ? C8 C9 1.508(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.148(2) . ? N1 Ce1 2.744(2) 1_545 ? O4 H4A 0.777(19) . ? O4 H4B 0.782(19) . ? 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 Ce1 O1 70.02(5) 6_656 . ? O1 Ce1 O3 85.89(4) 6_656 . ? O1 Ce1 O3 128.75(4) . . ? O1 Ce1 O3 128.75(4) 6_656 6_656 ? O1 Ce1 O3 85.89(4) . 6_656 ? O3 Ce1 O3 140.45(5) . 6_656 ? O1 Ce1 O2 76.21(4) 6_656 . ? O1 Ce1 O2 139.89(4) . . ? O3 Ce1 O2 67.72(3) . . ? O3 Ce1 O2 99.30(4) 6_656 . ? O1 Ce1 O2 139.89(4) 6_656 6_656 ? O1 Ce1 O2 76.21(4) . 6_656 ? O3 Ce1 O2 99.30(4) . 6_656 ? O3 Ce1 O2 67.72(4) 6_656 6_656 ? O2 Ce1 O2 142.50(5) . 6_656 ? O1 Ce1 O4 75.54(4) 6_656 . ? O1 Ce1 O4 67.39(4) . . ? O3 Ce1 O4 62.97(4) . . ? O3 Ce1 O4 135.76(4) 6_656 . ? O2 Ce1 O4 124.03(4) . . ? O2 Ce1 O4 71.89(4) 6_656 . ? O1 Ce1 O4 67.39(4) 6_656 6_656 ? O1 Ce1 O4 75.54(4) . 6_656 ? O3 Ce1 O4 135.76(4) . 6_656 ? O3 Ce1 O4 62.97(4) 6_656 6_656 ? O2 Ce1 O4 71.89(4) . 6_656 ? O2 Ce1 O4 124.03(4) 6_656 6_656 ? O4 Ce1 O4 134.45(5) . 6_656 ? O1 Ce1 N1 144.99(3) 6_656 1_565 ? O1 Ce1 N1 144.99(3) . 1_565 ? O3 Ce1 N1 70.23(3) . 1_565 ? O3 Ce1 N1 70.23(3) 6_656 1_565 ? O2 Ce1 N1 71.25(3) . 1_565 ? O2 Ce1 N1 71.25(2) 6_656 1_565 ? O4 Ce1 N1 112.78(3) . 1_565 ? O4 Ce1 N1 112.78(3) 6_656 1_565 ? C2 O1 Ce1 137.84(9) . . ? C6 O2 Ce1 138.27(9) . . ? C8 O3 Ce1 140.72(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.04(14) . . ? O1 C2 C1 117.77(13) . . ? C3 C2 C1 119.19(13) . . ? C4 C3 C2 117.74(9) . 6_656 ? C4 C3 C2 117.74(9) . . ? C2 C3 C2 124.52(18) 6_656 . ? N1 C4 C3 180.0 . . ? C6 C5 H5C 109.5 . . ? C6 C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? C6 C5 H5E 109.5 . . ? H5C C5 H5E 109.5 . . ? H5D C5 H5E 109.5 . . ? O2 C6 C7 123.73(13) . . ? O2 C6 C5 117.53(13) . . ? C7 C6 C5 118.73(13) . . ? C8 C7 C6 124.38(13) . . ? C8 C7 C10 117.47(13) . . ? C6 C7 C10 118.15(13) . . ? O3 C8 C7 122.97(13) . . ? O3 C8 C9 118.06(13) . . ? C7 C8 C9 118.96(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C7 178.53(17) . . ? C4 N1 Ce1 180.0 . 1_545 ? Ce1 O4 H4A 120.0(19) . . ? Ce1 O4 H4B 135.8(19) . . ? H4A O4 H4B 102(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.904 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.089 data_1b _database_code_depnum_ccdc_archive 'CCDC 845894' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1b _chemical_melting_point ? _chemical_formula_moiety 'C18 H24 Ce N3 O9, C2 H3 N1' _chemical_formula_sum 'C20 H27 Ce N4 O9' _chemical_formula_weight 607.58 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' Ce Ce -0.2486 2.6331 '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 11.1998(11) _cell_length_b 11.7328(12) _cell_length_c 12.3746(13) _cell_angle_alpha 62.7220(12) _cell_angle_beta 84.0719(13) _cell_angle_gamma 64.4427(11) _cell_volume 1294.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.153 _cell_measurement_theta_max 31.273 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5951 _exptl_absorpt_correction_T_max 0.8397 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20765 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 31.73 _reflns_number_total 8061 _reflns_number_gt 7593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0252P)^2^+0.3771P] 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 8061 _refine_ls_number_parameters 338 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ce1 Ce 0.930004(8) 0.557547(9) 0.731692(8) 0.00950(3) Uani 1 1 d . . . O1 O 1.10495(12) 0.58266(14) 0.59565(12) 0.0147(2) Uani 1 1 d . . . O2 O 1.09550(12) 0.58979(14) 0.81661(12) 0.0163(3) Uani 1 1 d . . . O3 O 0.86654(12) 0.81896(13) 0.62299(12) 0.0163(3) Uani 1 1 d . . . O4 O 0.68620(12) 0.70385(13) 0.70396(12) 0.0154(2) Uani 1 1 d . . . O5 O 1.05846(13) 0.33800(13) 0.70194(12) 0.0162(3) Uani 1 1 d . . . O6 O 1.05032(13) 0.33379(13) 0.92731(12) 0.0156(2) Uani 1 1 d . . . O7 O 0.79582(14) 0.41220(15) 0.80390(13) 0.0186(3) Uani 1 1 d D . . H7D H 0.723(2) 0.451(3) 0.775(2) 0.033(7) Uiso 1 1 d D . . H7E H 0.804(3) 0.339(2) 0.856(2) 0.042(8) Uiso 1 1 d D . . O8 O 0.83191(14) 0.62004(15) 0.52841(13) 0.0164(3) Uani 1 1 d D . . H8A H 0.757(2) 0.666(3) 0.507(2) 0.029(7) Uiso 1 1 d D . . H8B H 0.865(3) 0.612(3) 0.474(2) 0.037(8) Uiso 1 1 d D . . O9 O 0.85109(14) 0.61964(15) 0.90329(13) 0.0172(3) Uani 1 1 d D . . H9A H 0.896(3) 0.617(3) 0.952(2) 0.043(8) Uiso 1 1 d D . . H9B H 0.776(2) 0.660(3) 0.915(3) 0.034(7) Uiso 1 1 d D . . C1 C 1.29948(19) 0.5708(2) 0.49568(18) 0.0187(4) Uani 1 1 d . . . H1A H 1.3616 0.4723 0.5157 0.028 Uiso 1 1 calc R . . H1B H 1.3497 0.6266 0.4801 0.028 Uiso 1 1 calc R . . H1C H 1.2387 0.6120 0.4225 0.028 Uiso 1 1 calc R . . C2 C 1.22011(17) 0.57321(18) 0.60175(16) 0.0133(3) Uani 1 1 d . . . C3 C 1.27921(17) 0.56549(19) 0.70344(17) 0.0147(3) Uani 1 1 d . . . C4 C 1.20999(17) 0.58284(19) 0.80256(17) 0.0147(3) Uani 1 1 d . . . C5 C 1.2749(2) 0.5985(2) 0.89288(19) 0.0234(4) Uani 1 1 d . . . H5A H 1.2800 0.6899 0.8522 0.035 Uiso 1 1 calc R . . H5B H 1.3650 0.5208 0.9235 0.035 Uiso 1 1 calc R . . H5C H 1.2219 0.5948 0.9615 0.035 Uiso 1 1 calc R . . C6 C 1.41479(19) 0.5427(2) 0.70503(18) 0.0186(4) Uani 1 1 d . . . C7 C 0.7905(2) 1.0668(2) 0.5448(2) 0.0275(5) Uani 1 1 d . . . H7A H 0.7946 1.0939 0.6079 0.041 Uiso 1 1 calc R . . H7B H 0.7169 1.1443 0.4810 0.041 Uiso 1 1 calc R . . H7C H 0.8746 1.0483 0.5086 0.041 Uiso 1 1 calc R . . C8 C 0.76813(18) 0.93383(19) 0.60187(17) 0.0160(3) Uani 1 1 d . . . C9 C 0.63757(17) 0.94516(18) 0.62994(17) 0.0153(3) Uani 1 1 d . . . C10 C 0.60367(17) 0.82811(19) 0.67927(16) 0.0149(3) Uani 1 1 d . . . C11 C 0.46250(18) 0.8527(2) 0.70445(19) 0.0220(4) Uani 1 1 d . . . H11A H 0.4497 0.7700 0.7174 0.033 Uiso 1 1 calc R . . H11B H 0.4008 0.9377 0.6344 0.033 Uiso 1 1 calc R . . H11C H 0.4451 0.8665 0.7779 0.033 Uiso 1 1 calc R . . C12 C 0.53187(19) 1.0819(2) 0.60307(18) 0.0191(4) Uani 1 1 d . . . C13 C 1.1061(2) 0.1252(2) 0.69391(18) 0.0223(4) Uani 1 1 d . . . H13A H 1.0446 0.1871 0.6180 0.034 Uiso 1 1 calc R . . H13B H 1.0864 0.0436 0.7446 0.034 Uiso 1 1 calc R . . H13C H 1.1979 0.0912 0.6742 0.034 Uiso 1 1 calc R . . C14 C 1.08952(17) 0.20758(19) 0.76293(17) 0.0145(3) Uani 1 1 d . . . C15 C 1.11004(18) 0.13452(18) 0.89426(17) 0.0149(3) Uani 1 1 d . . . C16 C 1.08906(17) 0.20220(19) 0.96940(16) 0.0146(3) Uani 1 1 d . . . C17 C 1.1134(2) 0.1145(2) 1.10720(17) 0.0209(4) Uani 1 1 d . . . H17A H 1.2027 0.0921 1.1363 0.031 Uiso 1 1 calc R . . H17B H 1.1066 0.0258 1.1302 0.031 Uiso 1 1 calc R . . H17C H 1.0467 0.1686 1.1444 0.031 Uiso 1 1 calc R . . C18 C 1.15142(19) -0.0156(2) 0.95382(17) 0.0179(4) Uani 1 1 d . . . N1 N 1.52514(17) 0.5200(2) 0.71033(18) 0.0264(4) Uani 1 1 d . . . N2 N 0.44404(18) 1.19043(19) 0.58231(17) 0.0267(4) Uani 1 1 d . . . N3 N 1.18477(19) -0.13659(18) 1.00370(16) 0.0256(4) Uani 1 1 d . . . N4 N 0.6050(2) 0.7828(2) 0.9778(2) 0.0365(5) Uani 1 1 d . . . C19 C 0.5514(2) 0.7984(2) 1.0558(2) 0.0295(5) Uani 1 1 d . . . C20 C 0.4796(3) 0.8202(3) 1.1550(2) 0.0436(7) Uani 1 1 d . . . H20A H 0.4280 0.9224 1.1284 0.065 Uiso 1 1 calc R . . H20B H 0.5434 0.7782 1.2264 0.065 Uiso 1 1 calc R . . H20C H 0.4191 0.7746 1.1771 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.00893(5) 0.00924(5) 0.01019(5) -0.00480(4) 0.00122(3) -0.00349(3) O1 0.0122(6) 0.0189(6) 0.0157(6) -0.0091(5) 0.0037(5) -0.0082(5) O2 0.0143(6) 0.0226(7) 0.0168(6) -0.0109(5) 0.0042(5) -0.0107(5) O3 0.0151(6) 0.0123(6) 0.0196(7) -0.0066(5) 0.0031(5) -0.0055(5) O4 0.0128(6) 0.0124(6) 0.0188(6) -0.0070(5) -0.0002(5) -0.0032(5) O5 0.0203(6) 0.0112(6) 0.0147(6) -0.0060(5) 0.0034(5) -0.0051(5) O6 0.0176(6) 0.0117(6) 0.0146(6) -0.0054(5) -0.0023(5) -0.0037(5) O7 0.0147(6) 0.0150(6) 0.0216(7) -0.0023(6) -0.0007(5) -0.0087(5) O8 0.0135(6) 0.0204(7) 0.0139(6) -0.0097(5) 0.0012(5) -0.0043(5) O9 0.0153(6) 0.0233(7) 0.0167(7) -0.0132(6) 0.0027(5) -0.0073(6) C1 0.0189(9) 0.0231(9) 0.0212(9) -0.0139(8) 0.0087(7) -0.0125(8) C2 0.0130(7) 0.0108(7) 0.0160(8) -0.0061(6) 0.0035(6) -0.0056(6) C3 0.0113(7) 0.0159(8) 0.0184(9) -0.0082(7) 0.0025(6) -0.0070(7) C4 0.0150(8) 0.0139(8) 0.0164(8) -0.0065(7) 0.0013(6) -0.0077(7) C5 0.0236(10) 0.0360(11) 0.0239(10) -0.0188(9) 0.0062(8) -0.0193(9) C6 0.0177(9) 0.0216(9) 0.0209(9) -0.0122(8) 0.0039(7) -0.0101(7) C7 0.0267(10) 0.0138(9) 0.0372(12) -0.0064(9) 0.0000(9) -0.0097(8) C8 0.0190(8) 0.0128(8) 0.0140(8) -0.0055(7) -0.0001(6) -0.0054(7) C9 0.0140(8) 0.0112(8) 0.0168(8) -0.0071(7) -0.0010(6) -0.0009(6) C10 0.0139(8) 0.0171(8) 0.0129(8) -0.0079(7) 0.0000(6) -0.0048(7) C11 0.0125(8) 0.0236(10) 0.0267(10) -0.0111(8) 0.0022(7) -0.0057(7) C12 0.0193(9) 0.0178(9) 0.0187(9) -0.0096(7) -0.0021(7) -0.0046(7) C13 0.0317(11) 0.0172(9) 0.0198(9) -0.0112(8) 0.0045(8) -0.0095(8) C14 0.0138(8) 0.0137(8) 0.0165(8) -0.0083(7) 0.0036(6) -0.0053(6) C15 0.0164(8) 0.0110(7) 0.0160(8) -0.0050(7) 0.0014(6) -0.0060(6) C16 0.0123(8) 0.0153(8) 0.0157(8) -0.0064(7) 0.0006(6) -0.0061(6) C17 0.0282(10) 0.0179(9) 0.0130(8) -0.0049(7) -0.0002(7) -0.0090(8) C18 0.0210(9) 0.0158(8) 0.0165(9) -0.0069(7) 0.0019(7) -0.0081(7) N1 0.0190(8) 0.0378(10) 0.0320(10) -0.0212(9) 0.0061(7) -0.0156(8) N2 0.0248(9) 0.0199(8) 0.0295(10) -0.0135(8) -0.0044(7) -0.0010(7) N3 0.0328(10) 0.0181(8) 0.0231(9) -0.0075(7) 0.0030(7) -0.0110(7) N4 0.0281(10) 0.0429(12) 0.0331(11) -0.0212(10) 0.0054(8) -0.0074(9) C19 0.0292(11) 0.0253(11) 0.0292(11) -0.0140(9) 0.0013(9) -0.0058(9) C20 0.0583(17) 0.0359(14) 0.0335(14) -0.0218(12) 0.0151(12) -0.0137(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 Ce1 O2 2.4605(13) . ? Ce1 O1 2.4743(12) . ? Ce1 O4 2.4758(13) . ? Ce1 O3 2.5013(13) . ? Ce1 O8 2.5016(14) . ? Ce1 O9 2.5092(14) . ? Ce1 O6 2.5227(13) . ? Ce1 O5 2.5304(13) . ? Ce1 O7 2.5500(14) . ? O1 C2 1.253(2) . ? O2 C4 1.248(2) . ? O3 C8 1.247(2) . ? O4 C10 1.249(2) . ? O5 C14 1.252(2) . ? O6 C16 1.255(2) . ? O7 H7D 0.77(2) . ? O7 H7E 0.77(2) . ? O8 H8A 0.769(19) . ? O8 H8B 0.76(2) . ? O9 H9A 0.81(2) . ? O9 H9B 0.81(2) . ? C1 C2 1.512(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.430(2) . ? C3 C6 1.425(2) . ? C3 C4 1.429(3) . ? C4 C5 1.511(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.148(2) . ? C7 C8 1.512(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.430(3) . ? C9 C10 1.427(3) . ? C9 C12 1.428(2) . ? C10 C11 1.506(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.152(3) . ? C13 C14 1.506(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.435(3) . ? C15 C16 1.422(3) . ? C15 C18 1.428(2) . ? C16 C17 1.512(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.150(2) . ? N4 C19 1.128(3) . ? C19 C20 1.459(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 Ce1 O1 68.11(4) . . ? O2 Ce1 O4 124.38(4) . . ? O1 Ce1 O4 132.37(4) . . ? O2 Ce1 O3 74.21(4) . . ? O1 Ce1 O3 75.20(4) . . ? O4 Ce1 O3 67.28(4) . . ? O2 Ce1 O8 139.48(4) . . ? O1 Ce1 O8 75.45(4) . . ? O4 Ce1 O8 70.19(4) . . ? O3 Ce1 O8 80.02(4) . . ? O2 Ce1 O9 67.76(4) . . ? O1 Ce1 O9 133.59(4) . . ? O4 Ce1 O9 67.16(4) . . ? O3 Ce1 O9 79.76(4) . . ? O8 Ce1 O9 137.11(5) . . ? O2 Ce1 O6 71.85(4) . . ? O1 Ce1 O6 105.31(4) . . ? O4 Ce1 O6 122.32(4) . . ? O3 Ce1 O6 142.73(4) . . ? O8 Ce1 O6 136.91(4) . . ? O9 Ce1 O6 73.58(4) . . ? O2 Ce1 O5 106.21(4) . . ? O1 Ce1 O5 68.46(4) . . ? O4 Ce1 O5 129.15(4) . . ? O3 Ce1 O5 139.83(4) . . ? O8 Ce1 O5 74.92(4) . . ? O9 Ce1 O5 138.79(4) . . ? O6 Ce1 O5 66.19(4) . . ? O2 Ce1 O7 139.33(5) . . ? O1 Ce1 O7 138.22(5) . . ? O4 Ce1 O7 66.30(4) . . ? O3 Ce1 O7 133.36(4) . . ? O8 Ce1 O7 80.60(5) . . ? O9 Ce1 O7 86.52(5) . . ? O6 Ce1 O7 70.88(4) . . ? O5 Ce1 O7 72.54(5) . . ? C2 O1 Ce1 138.55(12) . . ? C4 O2 Ce1 139.74(12) . . ? C8 O3 Ce1 139.49(12) . . ? C10 O4 Ce1 140.27(12) . . ? C14 O5 Ce1 136.37(12) . . ? C16 O6 Ce1 137.96(12) . . ? Ce1 O7 H7D 117(2) . . ? Ce1 O7 H7E 137(2) . . ? H7D O7 H7E 105(3) . . ? Ce1 O8 H8A 121(2) . . ? Ce1 O8 H8B 131(2) . . ? H8A O8 H8B 107(3) . . ? Ce1 O9 H9A 127(2) . . ? Ce1 O9 H9B 128(2) . . ? H9A O9 H9B 104(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.24(16) . . ? O1 C2 C1 118.02(16) . . ? C3 C2 C1 118.73(15) . . ? C6 C3 C4 117.56(16) . . ? C6 C3 C2 118.20(16) . . ? C4 C3 C2 124.23(15) . . ? O2 C4 C3 122.92(16) . . ? O2 C4 C5 117.73(17) . . ? C3 C4 C5 119.31(16) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.5(2) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 123.53(17) . . ? O3 C8 C7 117.32(17) . . ? C9 C8 C7 119.14(16) . . ? C10 C9 C12 116.89(16) . . ? C10 C9 C8 124.02(16) . . ? C12 C9 C8 119.04(17) . . ? O4 C10 C9 123.16(16) . . ? O4 C10 C11 117.39(17) . . ? C9 C10 C11 119.45(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.0(2) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.97(16) . . ? O5 C14 C13 117.82(16) . . ? C15 C14 C13 119.21(16) . . ? C16 C15 C18 117.64(16) . . ? C16 C15 C14 124.34(16) . . ? C18 C15 C14 118.01(16) . . ? O6 C16 C15 123.24(17) . . ? O6 C16 C17 116.95(16) . . ? C15 C16 C17 119.81(16) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 178.8(2) . . ? N4 C19 C20 178.9(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.512 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.100 data_2 _database_code_depnum_ccdc_archive 'CCDC 845895' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 2 _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Eu N3 O8, 2(H2 O)' _chemical_formula_sum 'C18 H26 Eu N3 O10' _chemical_formula_weight 596.38 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9692(7) _cell_length_b 8.6871(7) _cell_length_c 30.244(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.4850(10) _cell_angle_gamma 90.00 _cell_volume 2330.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6159 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.01 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6376 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34300 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 30.92 _reflns_number_total 6962 _reflns_number_gt 6106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0241P)^2^+0.8600P] 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 6962 _refine_ls_number_parameters 319 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _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 0.156172(13) 0.794118(13) 0.118280(4) 0.00984(4) Uani 1 1 d . . . O1 O 0.28143(18) 0.57093(19) 0.09553(6) 0.0137(3) Uani 1 1 d . . . O2 O 0.4127(2) 0.79854(19) 0.15099(6) 0.0160(4) Uani 1 1 d . . . O3 O 0.1215(2) 0.5978(2) 0.17040(6) 0.0169(4) Uani 1 1 d . . . O4 O 0.0971(2) 0.9037(2) 0.18585(6) 0.0188(4) Uani 1 1 d . . . O5 O -0.02832(19) 0.64065(19) 0.07615(6) 0.0137(3) Uani 1 1 d . . . O6 O -0.06474(19) 0.9404(2) 0.09843(6) 0.0160(4) Uani 1 1 d . . . C1 C 0.4299(3) 0.3566(3) 0.08102(8) 0.0146(5) Uani 1 1 d . . . H1A H 0.3332 0.3214 0.0648 0.022 Uiso 1 1 calc R . . H1B H 0.4684 0.2803 0.1037 0.022 Uiso 1 1 calc R . . H1C H 0.5023 0.3695 0.0600 0.022 Uiso 1 1 calc R . . C2 C 0.4082(3) 0.5076(3) 0.10324(8) 0.0112(4) Uani 1 1 d . . . C3 C 0.5336(3) 0.5730(3) 0.13180(8) 0.0117(5) Uani 1 1 d . . . C4 C 0.5288(3) 0.7175(3) 0.15318(8) 0.0136(5) Uani 1 1 d . . . C5 C 0.6709(3) 0.7789(3) 0.18069(9) 0.0179(5) Uani 1 1 d . . . H5A H 0.6591 0.8891 0.1861 0.027 Uiso 1 1 calc R . . H5B H 0.7565 0.7631 0.1644 0.027 Uiso 1 1 calc R . . H5C H 0.6893 0.7242 0.2093 0.027 Uiso 1 1 calc R . . C6 C 0.6712(3) 0.4879(3) 0.13777(8) 0.0148(5) Uani 1 1 d . . . C7 C 0.0752(3) 0.4185(3) 0.22586(9) 0.0194(5) Uani 1 1 d . . . H7A H -0.0308 0.3865 0.2213 0.029 Uiso 1 1 calc R . . H7B H 0.1148 0.4149 0.2578 0.029 Uiso 1 1 calc R . . H7C H 0.1336 0.3489 0.2096 0.029 Uiso 1 1 calc R . . C8 C 0.0872(3) 0.5803(3) 0.20883(8) 0.0139(5) Uani 1 1 d . . . C9 C 0.0558(3) 0.7068(3) 0.23612(8) 0.0146(5) Uani 1 1 d . . . C10 C 0.0593(3) 0.8631(3) 0.22212(8) 0.0162(5) Uani 1 1 d . . . C11 C 0.0142(4) 0.9878(3) 0.25237(10) 0.0271(6) Uani 1 1 d . . . H11A H 0.0863 0.9906 0.2801 0.041 Uiso 1 1 calc R . . H11B H -0.0868 0.9662 0.2594 0.041 Uiso 1 1 calc R . . H11C H 0.0140 1.0876 0.2372 0.041 Uiso 1 1 calc R . . C12 C 0.0193(3) 0.6763(3) 0.27950(9) 0.0173(5) Uani 1 1 d . . . C13 C -0.2193(3) 0.5142(3) 0.02768(9) 0.0170(5) Uani 1 1 d . . . H13A H -0.1694 0.5101 0.0010 0.026 Uiso 1 1 calc R . . H13B H -0.3283 0.5249 0.0187 0.026 Uiso 1 1 calc R . . H13C H -0.1982 0.4193 0.0450 0.026 Uiso 1 1 calc R . . C14 C -0.1608(3) 0.6498(3) 0.05590(8) 0.0128(5) Uani 1 1 d . . . C15 C -0.2526(3) 0.7821(3) 0.05875(8) 0.0126(5) Uani 1 1 d . . . C16 C -0.1987(3) 0.9215(3) 0.08051(8) 0.0133(5) Uani 1 1 d . . . C17 C -0.3061(3) 1.0535(3) 0.08231(9) 0.0195(5) Uani 1 1 d . . . H17A H -0.2563 1.1348 0.1015 0.029 Uiso 1 1 calc R . . H17B H -0.3953 1.0175 0.0945 0.029 Uiso 1 1 calc R . . H17C H -0.3366 1.0942 0.0521 0.029 Uiso 1 1 calc R . . C18 C -0.4063(3) 0.7793(3) 0.03845(8) 0.0151(5) Uani 1 1 d . . . N1 N 0.7816(2) 0.4181(3) 0.14224(8) 0.0215(5) Uani 1 1 d . . . N2 N -0.0075(3) 0.6534(3) 0.31491(8) 0.0231(5) Uani 1 1 d . . . N3 N -0.5313(3) 0.7788(3) 0.02300(8) 0.0197(5) Uani 1 1 d . . . O7 O 0.1787(2) 0.8603(2) 0.04044(6) 0.0146(4) Uani 1 1 d D . . H7D H 0.256(2) 0.842(3) 0.0317(9) 0.018 Uiso 1 1 d D . . H7E H 0.110(2) 0.845(3) 0.0204(8) 0.018 Uiso 1 1 d D . . O8 O 0.2469(2) 1.0571(2) 0.12020(6) 0.0158(4) Uani 1 1 d D . . H8A H 0.320(2) 1.077(3) 0.1374(8) 0.019 Uiso 1 1 d D . . H8B H 0.188(3) 1.130(3) 0.1213(9) 0.019 Uiso 1 1 d D . . O9 O 0.0581(2) 1.3100(2) 0.10980(7) 0.0181(4) Uani 1 1 d D . . H9A H 0.097(3) 1.389(2) 0.1075(10) 0.022 Uiso 1 1 d D . . H9B H -0.019(2) 1.324(3) 0.1197(10) 0.022 Uiso 1 1 d D . . O10 O -0.0533(2) 0.8183(2) -0.02504(6) 0.0186(4) Uani 1 1 d D . . H10A H -0.094(3) 0.899(2) -0.0301(9) 0.022 Uiso 1 1 d D . . H10B H -0.048(4) 0.776(3) -0.0486(7) 0.022 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 Eu1 0.00933(6) 0.00862(6) 0.01124(6) -0.00028(4) 0.00046(4) 0.00109(4) O1 0.0102(8) 0.0131(8) 0.0169(9) -0.0012(7) -0.0006(7) 0.0019(6) O2 0.0111(8) 0.0135(9) 0.0221(10) -0.0037(7) -0.0026(7) 0.0014(7) O3 0.0243(10) 0.0114(9) 0.0154(9) 0.0009(7) 0.0042(7) 0.0010(7) O4 0.0308(11) 0.0114(9) 0.0155(9) -0.0003(7) 0.0078(8) 0.0016(8) O5 0.0114(8) 0.0095(8) 0.0190(9) -0.0010(7) -0.0019(7) 0.0000(6) O6 0.0126(8) 0.0126(9) 0.0216(9) -0.0014(7) -0.0013(7) 0.0011(7) C1 0.0149(12) 0.0134(12) 0.0159(12) -0.0021(9) 0.0031(9) 0.0022(9) C2 0.0128(11) 0.0112(11) 0.0104(11) 0.0027(8) 0.0044(9) 0.0011(9) C3 0.0102(11) 0.0138(11) 0.0112(11) 0.0023(9) 0.0016(9) 0.0018(9) C4 0.0116(11) 0.0150(12) 0.0139(12) 0.0026(9) 0.0007(9) -0.0008(9) C5 0.0143(12) 0.0168(13) 0.0215(13) -0.0016(10) -0.0011(10) 0.0002(10) C6 0.0145(12) 0.0153(12) 0.0140(12) -0.0002(9) 0.0003(9) -0.0020(9) C7 0.0261(14) 0.0136(12) 0.0181(13) 0.0044(10) 0.0013(11) 0.0010(10) C8 0.0126(11) 0.0143(12) 0.0141(11) 0.0006(9) -0.0009(9) -0.0007(9) C9 0.0138(12) 0.0162(12) 0.0136(12) 0.0002(9) 0.0011(9) 0.0014(9) C10 0.0175(12) 0.0163(13) 0.0144(12) -0.0015(10) 0.0015(10) -0.0008(10) C11 0.0450(19) 0.0179(14) 0.0215(14) -0.0030(11) 0.0150(13) 0.0016(13) C12 0.0192(13) 0.0145(12) 0.0174(13) 0.0012(10) -0.0001(10) 0.0001(10) C13 0.0185(13) 0.0125(12) 0.0191(13) -0.0023(10) -0.0008(10) -0.0013(10) C14 0.0128(11) 0.0129(11) 0.0129(11) 0.0005(9) 0.0028(9) -0.0020(9) C15 0.0098(11) 0.0141(12) 0.0139(11) 0.0004(9) 0.0016(9) 0.0009(9) C16 0.0135(11) 0.0143(12) 0.0124(11) 0.0012(9) 0.0032(9) 0.0013(9) C17 0.0153(12) 0.0172(13) 0.0247(14) -0.0034(11) -0.0013(10) 0.0066(10) C18 0.0166(13) 0.0157(12) 0.0136(12) 0.0000(9) 0.0042(10) 0.0008(9) N1 0.0154(11) 0.0226(12) 0.0255(12) -0.0041(10) -0.0006(9) 0.0027(9) N2 0.0314(14) 0.0213(12) 0.0168(11) 0.0009(9) 0.0039(10) 0.0041(10) N3 0.0154(11) 0.0250(13) 0.0185(11) -0.0021(9) 0.0018(9) 0.0025(9) O7 0.0113(8) 0.0194(9) 0.0133(8) -0.0004(7) 0.0020(7) 0.0015(7) O8 0.0145(9) 0.0123(9) 0.0191(9) -0.0006(7) -0.0023(7) -0.0006(7) O9 0.0179(10) 0.0127(9) 0.0238(10) -0.0028(8) 0.0040(8) 0.0023(7) O10 0.0225(10) 0.0178(10) 0.0147(9) -0.0003(7) 0.0001(8) 0.0034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5 2.3488(16) . ? Eu1 O6 2.3557(17) . ? Eu1 O2 2.3672(17) . ? Eu1 O3 2.3740(17) . ? Eu1 O4 2.3840(17) . ? Eu1 O1 2.3922(17) . ? Eu1 O8 2.4233(18) . ? Eu1 O7 2.4606(17) . ? O1 C2 1.253(3) . ? O2 C4 1.250(3) . ? O3 C8 1.255(3) . ? O4 C10 1.246(3) . ? O5 C14 1.257(3) . ? O6 C16 1.254(3) . ? C1 C2 1.500(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.431(3) . ? C3 C4 1.416(3) . ? C3 C6 1.427(3) . ? C4 C5 1.513(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.152(3) . ? C7 C8 1.506(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.427(3) . ? C9 C12 1.423(4) . ? C9 C10 1.425(4) . ? C10 C11 1.511(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.149(3) . ? C13 C14 1.503(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.424(3) . ? C15 C18 1.424(4) . ? C15 C16 1.428(3) . ? C16 C17 1.503(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.149(3) . ? O7 H7D 0.796(16) . ? O7 H7E 0.812(16) . ? O8 H8A 0.795(16) . ? O8 H8B 0.830(17) . ? O9 H9A 0.781(16) . ? O9 H9B 0.804(16) . ? O10 H10A 0.796(16) . ? O10 H10B 0.809(16) . ? 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 70.68(6) . . ? O5 Eu1 O2 143.08(6) . . ? O6 Eu1 O2 145.79(6) . . ? O5 Eu1 O3 78.55(6) . . ? O6 Eu1 O3 111.65(6) . . ? O2 Eu1 O3 87.06(6) . . ? O5 Eu1 O4 117.63(6) . . ? O6 Eu1 O4 73.63(6) . . ? O2 Eu1 O4 87.74(6) . . ? O3 Eu1 O4 69.52(6) . . ? O5 Eu1 O1 72.97(6) . . ? O6 Eu1 O1 140.97(6) . . ? O2 Eu1 O1 70.40(6) . . ? O3 Eu1 O1 73.85(6) . . ? O4 Eu1 O1 138.02(6) . . ? O5 Eu1 O8 139.06(6) . . ? O6 Eu1 O8 76.38(6) . . ? O2 Eu1 O8 70.88(6) . . ? O3 Eu1 O8 137.56(6) . . ? O4 Eu1 O8 73.70(6) . . ? O1 Eu1 O8 126.93(6) . . ? O5 Eu1 O7 76.37(6) . . ? O6 Eu1 O7 79.32(6) . . ? O2 Eu1 O7 100.61(6) . . ? O3 Eu1 O7 147.20(6) . . ? O4 Eu1 O7 141.89(6) . . ? O1 Eu1 O7 78.81(6) . . ? O8 Eu1 O7 74.20(6) . . ? C2 O1 Eu1 138.90(15) . . ? C4 O2 Eu1 139.77(16) . . ? C8 O3 Eu1 140.92(16) . . ? C10 O4 Eu1 139.95(17) . . ? C14 O5 Eu1 140.21(16) . . ? C16 O6 Eu1 139.12(16) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.3(2) . . ? O1 C2 C1 118.3(2) . . ? C3 C2 C1 118.3(2) . . ? C4 C3 C6 119.0(2) . . ? C4 C3 C2 123.6(2) . . ? C6 C3 C2 117.4(2) . . ? O2 C4 C3 123.8(2) . . ? O2 C4 C5 117.3(2) . . ? C3 C4 C5 118.9(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 179.2(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.6(2) . . ? O3 C8 C7 118.0(2) . . ? C9 C8 C7 119.4(2) . . ? C12 C9 C10 118.0(2) . . ? C12 C9 C8 118.8(2) . . ? C10 C9 C8 123.2(2) . . ? O4 C10 C9 123.6(2) . . ? O4 C10 C11 117.5(2) . . ? C9 C10 C11 118.9(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.6(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.4(2) . . ? O5 C14 C13 116.9(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C18 119.4(2) . . ? C14 C15 C16 123.6(2) . . ? C18 C15 C16 117.0(2) . . ? O6 C16 C15 123.2(2) . . ? O6 C16 C17 117.6(2) . . ? C15 C16 C17 119.2(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 178.3(3) . . ? Eu1 O7 H7D 118(2) . . ? Eu1 O7 H7E 121(2) . . ? H7D O7 H7E 109(2) . . ? Eu1 O8 H8A 118(2) . . ? Eu1 O8 H8B 121(2) . . ? H8A O8 H8B 106(2) . . ? H9A O9 H9B 109(2) . . ? H10A O10 H10B 108(2) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.107 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.130 data_3 _database_code_depnum_ccdc_archive 'CCDC 845896' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 3 _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 N3 O8 Yb, 2(H2 O)' _chemical_formula_sum 'C18 H26 N3 O10 Yb' _chemical_formula_weight 617.46 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.868(2) _cell_length_b 8.633(2) _cell_length_c 30.120(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.002(4) _cell_angle_gamma 90.00 _cell_volume 2283.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.04 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 4.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38454 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 34.05 _reflns_number_total 8852 _reflns_number_gt 6972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0254P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8852 _refine_ls_number_parameters 319 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.152240(17) 0.795770(16) 0.117122(5) 0.01018(5) Uani 1 1 d . . . O1 O 0.2751(3) 0.5816(3) 0.09328(8) 0.0139(5) Uani 1 1 d . . . O2 O 0.3988(3) 0.8034(3) 0.15101(9) 0.0161(5) Uani 1 1 d . . . O3 O 0.1215(3) 0.6011(3) 0.16715(8) 0.0154(5) Uani 1 1 d . . . O4 O 0.0941(3) 0.9062(3) 0.18224(9) 0.0186(6) Uani 1 1 d . . . O5 O -0.0265(3) 0.6418(3) 0.07785(9) 0.0142(5) Uani 1 1 d . . . O6 O -0.0610(3) 0.9417(3) 0.09882(9) 0.0159(5) Uani 1 1 d . . . C1 C 0.4231(4) 0.3612(4) 0.08053(12) 0.0145(7) Uani 1 1 d . . . H1A H 0.3266 0.3278 0.0633 0.022 Uiso 1 1 calc R . . H1B H 0.4568 0.2840 0.1036 0.022 Uiso 1 1 calc R . . H1C H 0.5002 0.3720 0.0604 0.022 Uiso 1 1 calc R . . C2 C 0.4008(4) 0.5146(4) 0.10240(11) 0.0117(6) Uani 1 1 d . . . C3 C 0.5248(4) 0.5773(4) 0.13262(12) 0.0111(6) Uani 1 1 d . . . C4 C 0.5183(4) 0.7229(4) 0.15393(12) 0.0138(7) Uani 1 1 d . . . C5 C 0.6584(5) 0.7850(4) 0.18201(14) 0.0186(8) Uani 1 1 d . . . H5A H 0.6451 0.8958 0.1874 0.028 Uiso 1 1 calc R . . H5B H 0.7467 0.7698 0.1662 0.028 Uiso 1 1 calc R . . H5C H 0.6747 0.7299 0.2107 0.028 Uiso 1 1 calc R . . C6 C 0.6630(4) 0.4905(4) 0.13944(12) 0.0145(7) Uani 1 1 d . . . C7 C 0.0829(5) 0.4198(4) 0.22373(13) 0.0195(8) Uani 1 1 d . . . H7A H -0.0229 0.3837 0.2188 0.029 Uiso 1 1 calc R . . H7B H 0.1206 0.4183 0.2559 0.029 Uiso 1 1 calc R . . H7C H 0.1459 0.3516 0.2079 0.029 Uiso 1 1 calc R . . C8 C 0.0907(4) 0.5827(4) 0.20618(12) 0.0146(7) Uani 1 1 d . . . C9 C 0.0592(4) 0.7088(4) 0.23402(12) 0.0147(7) Uani 1 1 d . . . C10 C 0.0586(4) 0.8662(4) 0.21914(12) 0.0161(7) Uani 1 1 d . . . C11 C 0.0115(5) 0.9917(5) 0.24904(14) 0.0252(9) Uani 1 1 d . . . H11A H 0.0706 0.9824 0.2789 0.038 Uiso 1 1 calc R . . H11B H -0.0972 0.9813 0.2513 0.038 Uiso 1 1 calc R . . H11C H 0.0304 1.0932 0.2363 0.038 Uiso 1 1 calc R . . C12 C 0.0278(5) 0.6784(4) 0.27838(13) 0.0184(8) Uani 1 1 d . . . C13 C -0.2179(4) 0.5138(4) 0.02958(13) 0.0176(7) Uani 1 1 d . . . H13A H -0.1653 0.5070 0.0031 0.026 Uiso 1 1 calc R . . H13B H -0.3275 0.5261 0.0201 0.026 Uiso 1 1 calc R . . H13C H -0.1996 0.4189 0.0474 0.026 Uiso 1 1 calc R . . C14 C -0.1587(4) 0.6509(4) 0.05750(12) 0.0120(6) Uani 1 1 d . . . C15 C -0.2520(4) 0.7850(4) 0.05965(12) 0.0129(7) Uani 1 1 d . . . C16 C -0.1960(4) 0.9245(4) 0.08112(12) 0.0131(7) Uani 1 1 d . . . C17 C -0.3027(4) 1.0585(4) 0.08289(13) 0.0179(8) Uani 1 1 d . . . H17A H -0.2544 1.1369 0.1037 0.027 Uiso 1 1 calc R . . H17B H -0.3966 1.0222 0.0932 0.027 Uiso 1 1 calc R . . H17C H -0.3269 1.1038 0.0529 0.027 Uiso 1 1 calc R . . C18 C -0.4054(4) 0.7825(4) 0.03891(12) 0.0154(7) Uani 1 1 d . . . N1 N 0.7728(4) 0.4202(4) 0.14477(12) 0.0213(7) Uani 1 1 d . . . N2 N 0.0066(4) 0.6560(4) 0.31434(11) 0.0224(7) Uani 1 1 d . . . N3 N -0.5315(4) 0.7818(4) 0.02303(12) 0.0196(7) Uani 1 1 d . . . O7 O 0.1757(3) 0.8599(3) 0.04187(9) 0.0154(5) Uani 1 1 d D . . H7D H 0.259(2) 0.831(5) 0.0352(13) 0.019 Uiso 1 1 d D . . H7E H 0.112(3) 0.829(5) 0.0226(11) 0.019 Uiso 1 1 d D . . O8 O 0.2415(3) 1.0518(3) 0.11820(9) 0.0155(5) Uani 1 1 d D . . H8A H 0.318(3) 1.063(5) 0.1353(12) 0.019 Uiso 1 1 d D . . H8B H 0.187(4) 1.127(4) 0.1199(13) 0.019 Uiso 1 1 d D . . O9 O 0.0517(3) 1.3108(3) 0.11013(10) 0.0174(6) Uani 1 1 d D . . H9A H 0.082(4) 1.399(3) 0.1077(15) 0.021 Uiso 1 1 d D . . H9B H -0.026(3) 1.321(4) 0.1217(15) 0.021 Uiso 1 1 d D . . O10 O -0.0535(4) 0.8166(3) -0.02482(9) 0.0194(6) Uani 1 1 d D . . H10A H -0.095(5) 0.898(3) -0.0306(13) 0.023 Uiso 1 1 d D . . H10B H -0.035(5) 0.779(4) -0.0482(10) 0.023 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 Yb1 0.00953(8) 0.00869(7) 0.01203(7) -0.00010(5) 0.00041(5) 0.00087(5) O1 0.0111(12) 0.0154(12) 0.0146(12) -0.0010(9) 0.0001(10) 0.0029(10) O2 0.0125(13) 0.0130(12) 0.0214(13) -0.0026(10) -0.0028(11) 0.0011(10) O3 0.0200(14) 0.0129(12) 0.0135(12) -0.0005(9) 0.0029(10) -0.0014(10) O4 0.0295(16) 0.0115(12) 0.0158(13) 0.0004(10) 0.0072(12) 0.0018(11) O5 0.0121(12) 0.0092(11) 0.0203(13) -0.0002(9) -0.0015(10) 0.0002(9) O6 0.0112(13) 0.0144(12) 0.0211(13) -0.0017(10) -0.0007(11) 0.0016(10) C1 0.0139(17) 0.0123(16) 0.0179(17) -0.0022(13) 0.0045(14) 0.0010(13) C2 0.0141(17) 0.0114(15) 0.0102(14) 0.0030(12) 0.0040(13) 0.0016(13) C3 0.0083(15) 0.0117(15) 0.0127(15) 0.0003(12) -0.0007(13) 0.0012(12) C4 0.0144(18) 0.0124(16) 0.0150(16) 0.0014(12) 0.0032(14) -0.0020(13) C5 0.0136(18) 0.0169(18) 0.0234(19) -0.0035(15) -0.0043(15) -0.0010(14) C6 0.0101(16) 0.0182(17) 0.0146(16) 0.0022(13) -0.0005(13) -0.0003(13) C7 0.029(2) 0.0124(17) 0.0161(17) 0.0017(13) -0.0005(16) 0.0020(15) C8 0.0124(17) 0.0144(17) 0.0154(16) 0.0018(13) -0.0037(14) -0.0015(13) C9 0.0169(18) 0.0151(16) 0.0115(15) 0.0028(13) 0.0003(14) 0.0020(14) C10 0.0180(19) 0.0142(17) 0.0155(17) -0.0012(13) 0.0003(14) -0.0014(14) C11 0.041(3) 0.0167(19) 0.021(2) -0.0028(15) 0.0136(19) 0.0035(18) C12 0.020(2) 0.0153(18) 0.0186(18) 0.0019(14) -0.0008(16) 0.0014(14) C13 0.0188(19) 0.0139(17) 0.0190(18) -0.0024(14) -0.0013(15) -0.0008(14) C14 0.0118(16) 0.0126(15) 0.0118(15) -0.0002(12) 0.0025(13) -0.0027(13) C15 0.0107(16) 0.0119(16) 0.0164(16) -0.0003(12) 0.0028(14) 0.0011(13) C16 0.0121(17) 0.0137(16) 0.0138(16) -0.0001(12) 0.0029(13) 0.0037(13) C17 0.0141(18) 0.0167(18) 0.0228(19) -0.0017(14) 0.0021(15) 0.0055(14) C18 0.0156(18) 0.0176(18) 0.0137(16) -0.0009(13) 0.0043(14) 0.0014(14) N1 0.0168(17) 0.0217(17) 0.0239(17) -0.0035(13) -0.0021(14) 0.0000(13) N2 0.032(2) 0.0198(16) 0.0160(16) 0.0010(13) 0.0037(15) 0.0018(15) N3 0.0136(16) 0.0237(17) 0.0212(17) -0.0046(13) 0.0015(13) 0.0017(13) O7 0.0143(13) 0.0182(13) 0.0139(12) -0.0027(10) 0.0022(11) 0.0020(11) O8 0.0158(14) 0.0118(12) 0.0178(13) -0.0010(10) -0.0015(11) 0.0003(10) O9 0.0189(15) 0.0128(12) 0.0209(14) -0.0015(10) 0.0044(12) -0.0003(11) O10 0.0248(16) 0.0187(14) 0.0140(13) 0.0015(10) -0.0002(12) 0.0027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O5 2.271(3) . ? Yb1 O6 2.275(3) . ? Yb1 O2 2.282(3) . ? Yb1 O3 2.299(3) . ? Yb1 O4 2.303(3) . ? Yb1 O1 2.311(2) . ? Yb1 O8 2.347(3) . ? Yb1 O7 2.370(3) . ? Yb1 H8A 2.75(4) . ? O1 C2 1.252(4) . ? O2 C4 1.260(4) . ? O3 C8 1.254(4) . ? O4 C10 1.246(4) . ? O5 C14 1.248(4) . ? O6 C16 1.249(4) . ? C1 C2 1.504(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.433(5) . ? C3 C4 1.416(5) . ? C3 C6 1.427(5) . ? C4 C5 1.501(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.139(5) . ? C7 C8 1.507(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.425(5) . ? C9 C12 1.426(5) . ? C9 C10 1.431(5) . ? C10 C11 1.505(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.141(5) . ? C13 C14 1.504(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.430(5) . ? C15 C18 1.415(5) . ? C15 C16 1.423(5) . ? C16 C17 1.500(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.153(5) . ? O7 H7D 0.828(18) . ? O7 H7E 0.799(18) . ? O8 H8A 0.797(18) . ? O8 H8B 0.816(18) . ? O9 H9A 0.810(18) . ? O9 H9B 0.820(18) . ? O10 H10A 0.803(18) . ? O10 H10B 0.814(18) . ? 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 Yb1 O6 72.64(9) . . ? O5 Yb1 O2 143.69(9) . . ? O6 Yb1 O2 143.60(9) . . ? O5 Yb1 O3 77.03(9) . . ? O6 Yb1 O3 113.15(10) . . ? O2 Yb1 O3 85.50(9) . . ? O5 Yb1 O4 117.60(10) . . ? O6 Yb1 O4 72.54(10) . . ? O2 Yb1 O4 85.49(10) . . ? O3 Yb1 O4 71.55(9) . . ? O5 Yb1 O1 72.24(9) . . ? O6 Yb1 O1 141.24(9) . . ? O2 Yb1 O1 72.43(9) . . ? O3 Yb1 O1 73.91(9) . . ? O4 Yb1 O1 140.10(9) . . ? O5 Yb1 O8 140.21(9) . . ? O6 Yb1 O8 75.49(10) . . ? O2 Yb1 O8 70.49(9) . . ? O3 Yb1 O8 138.61(9) . . ? O4 Yb1 O8 73.34(9) . . ? O1 Yb1 O8 125.80(9) . . ? O5 Yb1 O7 77.67(9) . . ? O6 Yb1 O7 79.60(9) . . ? O2 Yb1 O7 102.41(10) . . ? O3 Yb1 O7 146.29(9) . . ? O4 Yb1 O7 141.02(9) . . ? O1 Yb1 O7 77.40(9) . . ? O8 Yb1 O7 73.67(9) . . ? O5 Yb1 H8A 155.5(6) . . ? O6 Yb1 H8A 89.2(6) . . ? O2 Yb1 H8A 55.6(6) . . ? O3 Yb1 H8A 126.3(7) . . ? O4 Yb1 H8A 70.1(9) . . ? O1 Yb1 H8A 118.2(7) . . ? O8 Yb1 H8A 15.5(6) . . ? O7 Yb1 H8A 83.0(8) . . ? C2 O1 Yb1 138.2(2) . . ? C4 O2 Yb1 139.4(2) . . ? C8 O3 Yb1 140.2(2) . . ? C10 O4 Yb1 139.4(2) . . ? C14 O5 Yb1 139.4(2) . . ? C16 O6 Yb1 138.8(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.1(3) . . ? O1 C2 C1 118.5(3) . . ? C3 C2 C1 118.4(3) . . ? C4 C3 C6 119.3(3) . . ? C4 C3 C2 123.2(3) . . ? C6 C3 C2 117.4(3) . . ? O2 C4 C3 123.0(3) . . ? O2 C4 C5 117.7(3) . . ? C3 C4 C5 119.3(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 179.5(5) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.8(3) . . ? O3 C8 C7 118.3(3) . . ? C9 C8 C7 118.9(3) . . ? C8 C9 C12 119.4(3) . . ? C8 C9 C10 122.2(3) . . ? C12 C9 C10 118.4(3) . . ? O4 C10 C9 123.6(3) . . ? O4 C10 C11 117.4(3) . . ? C9 C10 C11 119.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.0(5) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.6(3) . . ? O5 C14 C13 117.1(3) . . ? C15 C14 C13 120.2(3) . . ? C18 C15 C16 117.8(3) . . ? C18 C15 C14 119.6(3) . . ? C16 C15 C14 122.5(3) . . ? O6 C16 C15 123.2(3) . . ? O6 C16 C17 117.7(3) . . ? C15 C16 C17 119.1(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 178.2(4) . . ? Yb1 O7 H7D 111(3) . . ? Yb1 O7 H7E 118(3) . . ? H7D O7 H7E 107(3) . . ? Yb1 O8 H8A 112(3) . . ? Yb1 O8 H8B 123(3) . . ? H8A O8 H8B 109(3) . . ? H9A O9 H9B 104(3) . . ? H10A O10 H10B 108(3) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.478 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.231 data_4a _database_code_depnum_ccdc_archive 'CCDC 845897' #TrackingRef '- complete_incl_ins.cif' _vrf_PLAT021_4a ; PROBLEM: Ratio Unique / Expected Reflections too High ... 1.551 RESPONSE: non-merohedral twin, equally indexed reflections for different domains retained unmerged ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4a _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Ag Ce N4 O9' _chemical_formula_sum 'C24 H26 Ag Ce N4 O9' _chemical_formula_weight 762.48 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3395(14) _cell_length_b 15.475(3) _cell_length_c 16.273(3) _cell_angle_alpha 74.775(3) _cell_angle_beta 83.984(4) _cell_angle_gamma 90.269(4) _cell_volume 1531.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3371 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.72 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 750 _exptl_absorpt_coefficient_mu 2.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6721 _exptl_absorpt_correction_T_max 0.7378 _exptl_absorpt_process_details TWINABS _exptl_special_details 'non-merohedral twin' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24803 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.79 _reflns_number_total 14839 _reflns_number_gt 11142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _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 14839 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.009 _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 0.03771(4) 0.799615(15) 0.758744(15) 0.01199(6) Uani 1 1 d . . . Ag1 Ag 0.39738(5) 0.69641(2) 1.26878(2) 0.01972(8) Uani 1 1 d . . . O1 O -0.1260(4) 0.74181(19) 0.90771(17) 0.0174(6) Uani 1 1 d . . . O2 O 0.2738(4) 0.83321(17) 0.86224(16) 0.0156(6) Uani 1 1 d . . . O3 O 0.3334(4) 0.76577(17) 0.65603(16) 0.0158(6) Uani 1 1 d . . . O4 O -0.0397(4) 0.85038(18) 0.60690(17) 0.0168(6) Uani 1 1 d . . . O5 O 0.2664(5) 0.93247(18) 0.68931(17) 0.0180(6) Uani 1 1 d . . . O6 O -0.0881(4) 0.93768(19) 0.80025(18) 0.0189(7) Uani 1 1 d . . . O7 O 0.2313(5) 0.66745(18) 0.83071(18) 0.0197(7) Uani 1 1 d . . . O8 O -0.0666(4) 0.65799(19) 0.71981(18) 0.0179(6) Uani 1 1 d . . . O9 O -0.3571(5) 0.8026(2) 0.7555(2) 0.0209(7) Uani 1 1 d . . . H9A H -0.445(8) 0.818(3) 0.789(3) 0.031 Uiso 1 1 d . . . H9B H -0.408(8) 0.791(3) 0.721(3) 0.031 Uiso 1 1 d . . . N1 N 0.2070(6) 0.7009(3) 1.1583(2) 0.0283(9) Uani 1 1 d . . . N2 N 0.2472(6) 0.7276(3) 0.3869(2) 0.0273(9) Uani 1 1 d . . . N3 N 0.3729(6) 1.1779(3) 0.7984(3) 0.0315(10) Uani 1 1 d . . . N4 N 0.4018(6) 0.4239(3) 0.7198(3) 0.0272(9) Uani 1 1 d . . . C1 C -0.2115(7) 0.6599(3) 1.0517(3) 0.0286(11) Uani 1 1 d . . . H1A H -0.3438 0.6484 1.0295 0.043 Uiso 1 1 calc R . . H1B H -0.2430 0.6887 1.0983 0.043 Uiso 1 1 calc R . . H1C H -0.1428 0.6030 1.0733 0.043 Uiso 1 1 calc R . . C2 C -0.0650(6) 0.7207(3) 0.9807(3) 0.0174(9) Uani 1 1 d . . . C3 C 0.1277(7) 0.7536(3) 1.0019(3) 0.0172(9) Uani 1 1 d . . . C4 C 0.2795(6) 0.8125(3) 0.9418(2) 0.0142(8) Uani 1 1 d . . . C5 C 0.4594(7) 0.8547(3) 0.9740(3) 0.0216(9) Uani 1 1 d . . . H5A H 0.5937 0.8485 0.9406 0.032 Uiso 1 1 calc R . . H5B H 0.4672 0.8245 1.0346 0.032 Uiso 1 1 calc R . . H5C H 0.4337 0.9184 0.9677 0.032 Uiso 1 1 calc R . . C6 C 0.1700(6) 0.7248(3) 1.0883(3) 0.0191(9) Uani 1 1 d . . . C7 C -0.0940(7) 0.8801(3) 0.4614(3) 0.0258(10) Uani 1 1 d . . . H7A H -0.2391 0.8930 0.4810 0.039 Uiso 1 1 calc R . . H7B H -0.0984 0.8406 0.4234 0.039 Uiso 1 1 calc R . . H7C H -0.0175 0.9363 0.4302 0.039 Uiso 1 1 calc R . . C8 C 0.0183(6) 0.8349(3) 0.5376(3) 0.0172(9) Uani 1 1 d . . . C9 C 0.1910(6) 0.7773(3) 0.5254(3) 0.0178(9) Uani 1 1 d . . . C10 C 0.3433(6) 0.7489(3) 0.5846(3) 0.0156(8) Uani 1 1 d . . . C11 C 0.5279(7) 0.6957(3) 0.5613(3) 0.0231(10) Uani 1 1 d . . . H11A H 0.6414 0.6992 0.5968 0.035 Uiso 1 1 calc R . . H11B H 0.5807 0.7203 0.5007 0.035 Uiso 1 1 calc R . . H11C H 0.4815 0.6329 0.5711 0.035 Uiso 1 1 calc R . . C12 C 0.2214(7) 0.7507(3) 0.4480(3) 0.0203(10) Uani 1 1 d . . . C13 C 0.5438(7) 1.0401(3) 0.6671(3) 0.0238(10) Uani 1 1 d . . . H13A H 0.6541 1.0127 0.7026 0.036 Uiso 1 1 calc R . . H13B H 0.5460 1.1048 0.6609 0.036 Uiso 1 1 calc R . . H13C H 0.5705 1.0289 0.6105 0.036 Uiso 1 1 calc R . . C14 C 0.3288(7) 0.9997(3) 0.7095(3) 0.0179(9) Uani 1 1 d . . . C15 C 0.2092(7) 1.0389(3) 0.7680(3) 0.0189(9) Uani 1 1 d . . . C16 C 0.0018(7) 1.0064(3) 0.8088(3) 0.0183(9) Uani 1 1 d . . . C17 C -0.1203(7) 1.0574(3) 0.8644(3) 0.0339(13) Uani 1 1 d . . . H17A H -0.1615 1.1149 0.8286 0.051 Uiso 1 1 calc R . . H17B H -0.0308 1.0683 0.9065 0.051 Uiso 1 1 calc R . . H17C H -0.2479 1.0223 0.8943 0.051 Uiso 1 1 calc R . . C18 C 0.2966(7) 1.1168(3) 0.7853(3) 0.0204(9) Uani 1 1 d . . . C19 C 0.4927(7) 0.5595(3) 0.8564(3) 0.0242(10) Uani 1 1 d . . . H19A H 0.6188 0.5982 0.8317 0.036 Uiso 1 1 calc R . . H19B H 0.5161 0.4996 0.8481 0.036 Uiso 1 1 calc R . . H19C H 0.4661 0.5551 0.9178 0.036 Uiso 1 1 calc R . . C20 C 0.3026(7) 0.5990(3) 0.8123(3) 0.0173(9) Uani 1 1 d . . . C21 C 0.2131(7) 0.5587(3) 0.7543(3) 0.0183(9) Uani 1 1 d . . . C22 C 0.0260(7) 0.5886(3) 0.7139(3) 0.0182(9) Uani 1 1 d . . . C23 C -0.0614(7) 0.5336(3) 0.6598(3) 0.0291(12) Uani 1 1 d . . . H23A H -0.2166 0.5357 0.6652 0.044 Uiso 1 1 calc R . . H23B H -0.0191 0.4714 0.6795 0.044 Uiso 1 1 calc R . . H23C H -0.0050 0.5583 0.5997 0.044 Uiso 1 1 calc R . . C24 C 0.3148(7) 0.4827(3) 0.7350(3) 0.0214(9) 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 0.01159(10) 0.01330(12) 0.01050(11) -0.00236(9) -0.00073(9) 0.00025(9) Ag1 0.02707(18) 0.01764(18) 0.01549(17) -0.00572(14) -0.00343(14) 0.00346(15) O1 0.0173(14) 0.0234(17) 0.0100(15) -0.0024(13) 0.0002(12) -0.0017(12) O2 0.0148(13) 0.0180(15) 0.0127(14) -0.0014(12) -0.0024(12) -0.0014(13) O3 0.0163(14) 0.0173(15) 0.0133(14) -0.0037(12) 0.0001(13) -0.0013(13) O4 0.0196(15) 0.0183(16) 0.0118(15) -0.0026(13) -0.0023(12) 0.0035(12) O5 0.0243(15) 0.0133(15) 0.0152(15) -0.0026(12) 0.0001(13) -0.0043(13) O6 0.0172(14) 0.0188(17) 0.0222(17) -0.0080(14) -0.0022(13) -0.0009(12) O7 0.0233(15) 0.0171(16) 0.0175(16) -0.0018(13) -0.0040(13) 0.0050(13) O8 0.0139(14) 0.0176(16) 0.0225(17) -0.0054(13) -0.0023(12) -0.0003(12) O9 0.0138(15) 0.0301(19) 0.0220(19) -0.0116(15) -0.0046(13) 0.0043(13) N1 0.030(2) 0.033(2) 0.021(2) -0.0053(18) -0.0042(19) -0.011(2) N2 0.037(2) 0.027(2) 0.019(2) -0.0090(18) -0.0008(18) 0.0024(18) N3 0.031(2) 0.027(2) 0.037(3) -0.010(2) -0.0014(19) -0.0026(19) N4 0.028(2) 0.022(2) 0.031(2) -0.0071(19) -0.0041(18) 0.0033(18) C1 0.029(3) 0.035(3) 0.016(2) 0.002(2) 0.000(2) -0.012(2) C2 0.020(2) 0.017(2) 0.015(2) -0.0050(18) 0.0022(17) 0.0005(17) C3 0.022(2) 0.021(2) 0.009(2) -0.0037(18) -0.0039(17) -0.0013(18) C4 0.0131(18) 0.015(2) 0.016(2) -0.0068(17) -0.0021(17) 0.0063(17) C5 0.021(2) 0.024(2) 0.021(2) -0.0088(19) -0.0034(19) -0.0041(19) C6 0.020(2) 0.021(2) 0.017(2) -0.0062(19) -0.0012(18) -0.0032(18) C7 0.028(2) 0.034(3) 0.014(2) -0.0012(19) -0.010(2) 0.007(2) C8 0.020(2) 0.017(2) 0.013(2) 0.0005(18) -0.0011(17) -0.0051(17) C9 0.019(2) 0.022(2) 0.012(2) -0.0044(18) 0.0016(17) -0.0015(18) C10 0.016(2) 0.013(2) 0.016(2) -0.0021(17) 0.0020(17) -0.0020(17) C11 0.024(2) 0.024(3) 0.023(3) -0.011(2) -0.0006(19) 0.0041(19) C12 0.023(2) 0.023(2) 0.012(2) 0.0007(19) -0.0012(18) -0.0010(19) C13 0.023(2) 0.020(2) 0.024(2) -0.0011(19) 0.004(2) 0.000(2) C14 0.022(2) 0.012(2) 0.016(2) 0.0036(17) -0.0041(19) 0.0049(19) C15 0.022(2) 0.014(2) 0.018(2) 0.0002(19) -0.0052(18) -0.0027(17) C16 0.021(2) 0.016(2) 0.019(2) -0.0062(18) -0.0035(18) 0.0024(18) C17 0.029(3) 0.030(3) 0.048(3) -0.024(3) 0.005(2) -0.002(2) C18 0.023(2) 0.019(2) 0.019(2) -0.0067(18) 0.001(2) 0.002(2) C19 0.024(2) 0.019(2) 0.026(3) 0.0021(19) -0.005(2) 0.002(2) C20 0.0136(18) 0.015(2) 0.018(2) 0.0026(17) 0.0056(18) -0.0021(18) C21 0.022(2) 0.012(2) 0.016(2) 0.0026(18) 0.0017(18) -0.0007(17) C22 0.019(2) 0.014(2) 0.020(2) -0.0025(18) 0.0013(18) -0.0059(18) C23 0.028(2) 0.024(3) 0.040(3) -0.013(2) -0.013(2) 0.000(2) C24 0.018(2) 0.020(2) 0.022(2) 0.0007(19) 0.002(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O5 2.452(3) . ? Ce1 O1 2.466(3) . ? Ce1 O7 2.475(3) . ? Ce1 O4 2.490(3) . ? Ce1 O9 2.509(3) . ? Ce1 O6 2.514(3) . ? Ce1 O2 2.515(3) . ? Ce1 O3 2.529(3) . ? Ce1 O8 2.539(3) . ? Ag1 N2 2.223(4) 1_556 ? Ag1 N4 2.238(4) 2_667 ? Ag1 N1 2.255(4) . ? Ag1 N3 2.371(4) 2_677 ? O1 C2 1.249(5) . ? O2 C4 1.253(4) . ? O3 C10 1.253(4) . ? O4 C8 1.233(5) . ? O5 C14 1.245(5) . ? O6 C16 1.250(5) . ? O7 C20 1.249(5) . ? O8 C22 1.247(5) . ? O9 H9A 0.82(5) . ? O9 H9B 0.74(5) . ? N1 C6 1.150(5) . ? N2 C12 1.139(5) . ? N2 Ag1 2.223(4) 1_554 ? N3 C18 1.139(5) . ? N3 Ag1 2.371(4) 2_677 ? N4 C24 1.135(5) . ? N4 Ag1 2.238(4) 2_667 ? C1 C2 1.509(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.430(5) . ? C3 C6 1.414(6) . ? C3 C4 1.429(5) . ? C4 C5 1.517(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.506(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.446(6) . ? C9 C12 1.418(6) . ? C9 C10 1.425(6) . ? C10 C11 1.507(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.514(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.415(6) . ? C15 C18 1.430(6) . ? C15 C16 1.435(6) . ? C16 C17 1.509(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.516(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.421(6) . ? C21 C24 1.434(6) . ? C21 C22 1.436(6) . ? C22 C23 1.516(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 Ce1 O1 131.43(9) . . ? O5 Ce1 O7 114.07(9) . . ? O1 Ce1 O7 70.89(9) . . ? O5 Ce1 O4 72.75(9) . . ? O1 Ce1 O4 143.84(9) . . ? O7 Ce1 O4 129.50(9) . . ? O5 Ce1 O9 121.38(11) . . ? O1 Ce1 O9 72.79(10) . . ? O7 Ce1 O9 124.55(11) . . ? O4 Ce1 O9 71.22(10) . . ? O5 Ce1 O6 67.14(9) . . ? O1 Ce1 O6 76.12(9) . . ? O7 Ce1 O6 133.64(9) . . ? O4 Ce1 O6 96.11(9) . . ? O9 Ce1 O6 72.56(10) . . ? O5 Ce1 O2 69.59(9) . . ? O1 Ce1 O2 69.16(9) . . ? O7 Ce1 O2 67.21(9) . . ? O4 Ce1 O2 142.29(9) . . ? O9 Ce1 O2 132.21(10) . . ? O6 Ce1 O2 71.14(9) . . ? O5 Ce1 O3 68.31(9) . . ? O1 Ce1 O3 140.44(9) . . ? O7 Ce1 O3 69.55(9) . . ? O4 Ce1 O3 67.73(9) . . ? O9 Ce1 O3 131.69(10) . . ? O6 Ce1 O3 135.35(9) . . ? O2 Ce1 O3 96.09(9) . . ? O5 Ce1 O8 135.45(9) . . ? O1 Ce1 O8 92.27(9) . . ? O7 Ce1 O8 67.16(9) . . ? O4 Ce1 O8 74.77(9) . . ? O9 Ce1 O8 74.02(10) . . ? O6 Ce1 O8 146.52(9) . . ? O2 Ce1 O8 134.19(9) . . ? O3 Ce1 O8 71.61(9) . . ? N2 Ag1 N4 119.39(14) 1_556 2_667 ? N2 Ag1 N1 120.27(15) 1_556 . ? N4 Ag1 N1 106.03(14) 2_667 . ? N2 Ag1 N3 104.27(14) 1_556 2_677 ? N4 Ag1 N3 105.92(14) 2_667 2_677 ? N1 Ag1 N3 97.73(14) . 2_677 ? C2 O1 Ce1 137.0(3) . . ? C4 O2 Ce1 137.2(3) . . ? C10 O3 Ce1 134.9(3) . . ? C8 O4 Ce1 138.6(3) . . ? C14 O5 Ce1 136.1(3) . . ? C16 O6 Ce1 134.6(3) . . ? C20 O7 Ce1 136.3(3) . . ? C22 O8 Ce1 134.8(3) . . ? Ce1 O9 H9A 127(3) . . ? Ce1 O9 H9B 122(4) . . ? H9A O9 H9B 111(5) . . ? C6 N1 Ag1 155.0(4) . . ? C12 N2 Ag1 162.6(4) . 1_554 ? C18 N3 Ag1 141.5(4) . 2_677 ? C24 N4 Ag1 161.9(4) . 2_667 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.5(4) . . ? O1 C2 C1 117.1(4) . . ? C3 C2 C1 118.3(4) . . ? C6 C3 C4 118.3(4) . . ? C6 C3 C2 117.2(4) . . ? C4 C3 C2 124.5(4) . . ? O2 C4 C3 124.1(4) . . ? O2 C4 C5 116.5(4) . . ? C3 C4 C5 119.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 179.1(5) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 C9 123.4(4) . . ? O4 C8 C7 118.1(4) . . ? C9 C8 C7 118.5(4) . . ? C12 C9 C10 116.8(4) . . ? C12 C9 C8 119.1(4) . . ? C10 C9 C8 124.0(4) . . ? O3 C10 C9 123.5(4) . . ? O3 C10 C11 117.2(4) . . ? C9 C10 C11 119.2(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.4(5) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 123.5(4) . . ? O5 C14 C13 116.4(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C18 118.3(4) . . ? C14 C15 C16 123.5(4) . . ? C18 C15 C16 118.1(4) . . ? O6 C16 C15 123.7(4) . . ? O6 C16 C17 116.8(4) . . ? C15 C16 C17 119.4(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 177.7(5) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 C21 123.1(4) . . ? O7 C20 C19 116.0(4) . . ? C21 C20 C19 120.9(4) . . ? C20 C21 C24 118.1(4) . . ? C20 C21 C22 124.4(4) . . ? C24 C21 C22 117.5(4) . . ? O8 C22 C21 123.6(4) . . ? O8 C22 C23 118.2(4) . . ? C21 C22 C23 118.1(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C21 177.6(5) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.977 _refine_diff_density_min -1.933 _refine_diff_density_rms 0.187 data_5a _database_code_depnum_ccdc_archive 'CCDC 845898' #TrackingRef '- complete_incl_ins.cif' _vrf_PLAT021_5a ; PROBLEM: Ratio Unique / Expected Reflections too High ... 1.211 RESPONSE: non-merohedral twin, equally indexed reflections for different domains retained unmerged ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5a _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Ag Eu N4 O9' _chemical_formula_sum 'C24 H26 Ag Eu N4 O9' _chemical_formula_weight 774.32 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 6.2589(7) _cell_length_b 15.4445(16) _cell_length_c 16.1802(17) _cell_angle_alpha 75.2210(14) _cell_angle_beta 83.8603(16) _cell_angle_gamma 89.9936(16) _cell_volume 1503.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9182 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 30.55 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5328 _exptl_absorpt_correction_T_max 0.6655 _exptl_absorpt_process_details TWINABS _exptl_special_details 'non-merohedral twin' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD Area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33480 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 30.62 _reflns_number_total 11184 _reflns_number_gt 10411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SAINT' _computing_data_reduction 'BRUKER SAINT' _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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _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 11184 _refine_ls_number_parameters 367 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.010 _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 0.04746(3) 0.798674(11) 0.758499(11) 0.00988(5) Uani 1 1 d D . . Ag1 Ag 0.39586(5) 0.699162(19) 1.267205(19) 0.01802(7) Uani 1 1 d . . . O1 O -0.1217(4) 0.74040(18) 0.90218(17) 0.0168(5) Uani 1 1 d . . . O2 O 0.2773(4) 0.83335(17) 0.85979(16) 0.0143(5) Uani 1 1 d . . . O3 O 0.3370(4) 0.76379(17) 0.65773(16) 0.0143(5) Uani 1 1 d . . . O4 O -0.0378(4) 0.85152(18) 0.61203(17) 0.0156(5) Uani 1 1 d . . . O5 O 0.2755(4) 0.92618(17) 0.68893(17) 0.0164(5) Uani 1 1 d . . . O6 O -0.0848(4) 0.93230(18) 0.79936(18) 0.0171(6) Uani 1 1 d . . . O7 O 0.2423(4) 0.67141(17) 0.82915(17) 0.0174(6) Uani 1 1 d . . . O8 O -0.0608(4) 0.66142(18) 0.72033(18) 0.0161(5) Uani 1 1 d . . . O9 O -0.3415(4) 0.7999(2) 0.75611(18) 0.0176(5) Uani 1 1 d D . . H9A H -0.388(3) 0.793(3) 0.8100(12) 0.026 Uiso 1 1 d D . . H9B H -0.465(4) 0.809(3) 0.741(2) 0.026 Uiso 1 1 d D . . N1 N 0.2015(6) 0.7027(3) 1.1565(2) 0.0267(8) Uani 1 1 d . . . N2 N 0.2414(6) 0.7306(3) 0.3856(2) 0.0271(8) Uani 1 1 d . . . N3 N 0.3718(6) 1.1758(3) 0.7968(3) 0.0284(8) Uani 1 1 d . . . N4 N 0.4005(6) 0.4215(2) 0.7226(3) 0.0273(8) Uani 1 1 d . . . C1 C -0.2138(7) 0.6593(3) 1.0467(3) 0.0268(10) Uani 1 1 d . . . H1A H -0.3442 0.6459 1.0232 0.040 Uiso 1 1 calc R . . H1B H -0.2524 0.6885 1.0932 0.040 Uiso 1 1 calc R . . H1C H -0.1409 0.6034 1.0694 0.040 Uiso 1 1 calc R . . C2 C -0.0654(6) 0.7209(2) 0.9765(2) 0.0149(7) Uani 1 1 d . . . C3 C 0.1268(6) 0.7541(3) 0.9989(2) 0.0154(7) Uani 1 1 d . . . C4 C 0.2819(6) 0.8125(2) 0.9398(2) 0.0133(7) Uani 1 1 d . . . C5 C 0.4604(6) 0.8560(3) 0.9726(2) 0.0193(8) Uani 1 1 d . . . H5A H 0.5950 0.8557 0.9357 0.029 Uiso 1 1 calc R . . H5B H 0.4775 0.8226 1.0316 0.029 Uiso 1 1 calc R . . H5C H 0.4242 0.9180 0.9716 0.029 Uiso 1 1 calc R . . C6 C 0.1663(6) 0.7268(3) 1.0866(3) 0.0182(8) Uani 1 1 d . . . C7 C -0.0996(7) 0.8841(3) 0.4666(2) 0.0243(9) Uani 1 1 d . . . H7A H -0.2446 0.8982 0.4879 0.036 Uiso 1 1 calc R . . H7B H -0.1095 0.8457 0.4273 0.036 Uiso 1 1 calc R . . H7C H -0.0204 0.9397 0.4359 0.036 Uiso 1 1 calc R . . C8 C 0.0166(6) 0.8361(2) 0.5413(2) 0.0143(7) Uani 1 1 d . . . C9 C 0.1881(6) 0.7781(3) 0.5271(2) 0.0148(7) Uani 1 1 d . . . C10 C 0.3463(6) 0.7483(2) 0.5857(2) 0.0145(7) Uani 1 1 d . . . C11 C 0.5330(7) 0.6963(3) 0.5586(3) 0.0227(9) Uani 1 1 d . . . H11A H 0.6476 0.6966 0.5953 0.034 Uiso 1 1 calc R . . H11B H 0.5873 0.7240 0.4986 0.034 Uiso 1 1 calc R . . H11C H 0.4854 0.6344 0.5644 0.034 Uiso 1 1 calc R . . C12 C 0.2158(7) 0.7535(3) 0.4482(3) 0.0189(8) Uani 1 1 d . . . C13 C 0.5500(7) 1.0368(3) 0.6638(3) 0.0213(8) Uani 1 1 d . . . H13A H 0.6654 1.0084 0.6967 0.032 Uiso 1 1 calc R . . H13B H 0.5512 1.1010 0.6604 0.032 Uiso 1 1 calc R . . H13C H 0.5721 1.0280 0.6056 0.032 Uiso 1 1 calc R . . C14 C 0.3354(6) 0.9948(2) 0.7080(2) 0.0148(7) Uani 1 1 d . . . C15 C 0.2104(7) 1.0349(2) 0.7667(3) 0.0166(7) Uani 1 1 d . . . C16 C 0.0028(7) 1.0020(3) 0.8073(3) 0.0183(8) Uani 1 1 d . . . C17 C -0.1220(8) 1.0545(3) 0.8621(3) 0.0315(11) Uani 1 1 d . . . H17A H -0.1489 1.1143 0.8266 0.047 Uiso 1 1 calc R . . H17B H -0.0389 1.0601 0.9086 0.047 Uiso 1 1 calc R . . H17C H -0.2594 1.0232 0.8868 0.047 Uiso 1 1 calc R . . C18 C 0.2973(7) 1.1132(3) 0.7830(3) 0.0201(8) Uani 1 1 d . . . C19 C 0.4975(7) 0.5600(3) 0.8586(3) 0.0207(8) Uani 1 1 d . . . H19A H 0.6265 0.5982 0.8356 0.031 Uiso 1 1 calc R . . H19B H 0.5215 0.5004 0.8492 0.031 Uiso 1 1 calc R . . H19C H 0.4669 0.5549 0.9203 0.031 Uiso 1 1 calc R . . C20 C 0.3098(6) 0.6009(2) 0.8133(2) 0.0149(7) Uani 1 1 d . . . C21 C 0.2170(6) 0.5594(3) 0.7552(3) 0.0170(7) Uani 1 1 d . . . C22 C 0.0287(6) 0.5909(2) 0.7145(2) 0.0154(7) Uani 1 1 d . . . C23 C -0.0668(8) 0.5352(3) 0.6625(3) 0.0285(10) Uani 1 1 d . . . H23A H -0.2193 0.5485 0.6593 0.043 Uiso 1 1 calc R . . H23B H -0.0526 0.4715 0.6902 0.043 Uiso 1 1 calc R . . H23C H 0.0094 0.5494 0.6043 0.043 Uiso 1 1 calc R . . C24 C 0.3152(7) 0.4826(2) 0.7371(3) 0.0189(7) 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 0.00915(8) 0.01197(8) 0.00898(8) -0.00355(6) -0.00089(6) 0.00088(6) Ag1 0.02585(16) 0.01592(13) 0.01459(13) -0.00726(10) -0.00436(11) 0.00463(12) O1 0.0147(13) 0.0228(14) 0.0121(12) -0.0031(11) -0.0016(10) -0.0006(11) O2 0.0147(12) 0.0163(12) 0.0120(11) -0.0033(10) -0.0030(11) 0.0011(11) O3 0.0133(12) 0.0168(12) 0.0138(12) -0.0053(10) -0.0024(11) 0.0005(11) O4 0.0158(13) 0.0199(13) 0.0116(12) -0.0044(10) -0.0029(10) 0.0024(11) O5 0.0193(14) 0.0161(12) 0.0136(12) -0.0036(10) -0.0007(11) -0.0023(11) O6 0.0150(13) 0.0153(13) 0.0232(14) -0.0086(11) -0.0028(11) 0.0011(10) O7 0.0212(14) 0.0168(13) 0.0149(13) -0.0044(10) -0.0044(11) 0.0046(11) O8 0.0113(12) 0.0170(13) 0.0212(14) -0.0075(11) -0.0006(11) 0.0006(10) O9 0.0138(12) 0.0274(15) 0.0137(13) -0.0090(12) -0.0022(11) 0.0045(12) N1 0.0279(19) 0.035(2) 0.0154(16) -0.0038(15) -0.0023(15) -0.0061(17) N2 0.035(2) 0.031(2) 0.0184(17) -0.0122(16) -0.0023(16) 0.0046(17) N3 0.027(2) 0.0236(19) 0.037(2) -0.0128(17) 0.0009(17) -0.0047(15) N4 0.030(2) 0.0203(18) 0.034(2) -0.0094(16) -0.0092(17) 0.0060(15) C1 0.026(2) 0.033(2) 0.0155(19) 0.0018(17) 0.0008(17) -0.0132(19) C2 0.0156(17) 0.0155(17) 0.0128(16) -0.0037(14) 0.0016(13) -0.0018(14) C3 0.0187(18) 0.0177(18) 0.0100(16) -0.0031(14) -0.0030(14) 0.0014(14) C4 0.0123(16) 0.0159(16) 0.0150(16) -0.0085(13) -0.0051(14) 0.0049(14) C5 0.0181(19) 0.026(2) 0.0159(17) -0.0082(15) -0.0031(15) -0.0037(16) C6 0.0197(19) 0.0181(18) 0.0171(18) -0.0050(15) -0.0027(15) -0.0022(15) C7 0.028(2) 0.031(2) 0.0143(18) -0.0036(16) -0.0067(17) 0.0077(19) C8 0.0145(17) 0.0171(17) 0.0110(16) -0.0025(14) -0.0030(13) -0.0004(14) C9 0.0170(18) 0.0168(17) 0.0109(16) -0.0052(14) 0.0004(13) -0.0006(14) C10 0.0151(17) 0.0125(15) 0.0152(16) -0.0030(13) 0.0008(15) -0.0014(14) C11 0.020(2) 0.025(2) 0.024(2) -0.0102(17) 0.0015(16) 0.0071(16) C12 0.0199(19) 0.0206(19) 0.0170(18) -0.0058(15) -0.0030(15) 0.0017(15) C13 0.0174(19) 0.0186(18) 0.026(2) -0.0042(16) 0.0014(16) -0.0048(15) C14 0.0142(17) 0.0123(15) 0.0162(17) 0.0001(13) -0.0041(15) -0.0012(14) C15 0.024(2) 0.0087(15) 0.0183(18) -0.0057(14) -0.0031(15) 0.0018(14) C16 0.0210(19) 0.0151(17) 0.0207(19) -0.0072(15) -0.0049(16) 0.0040(15) C17 0.027(2) 0.029(2) 0.045(3) -0.023(2) 0.003(2) 0.0005(19) C18 0.022(2) 0.0144(17) 0.0232(19) -0.0043(15) -0.0029(17) 0.0015(16) C19 0.0195(19) 0.0167(18) 0.025(2) -0.0013(15) -0.0078(17) 0.0037(15) C20 0.0134(17) 0.0174(17) 0.0114(15) 0.0001(13) 0.0013(14) -0.0012(14) C21 0.0180(18) 0.0133(17) 0.0201(19) -0.0058(15) 0.0000(15) 0.0024(14) C22 0.0137(17) 0.0139(16) 0.0189(18) -0.0056(14) 0.0005(14) 0.0010(14) C23 0.029(2) 0.023(2) 0.042(3) -0.018(2) -0.014(2) 0.0026(18) C24 0.0209(19) 0.0141(17) 0.0213(18) -0.0033(14) -0.0041(17) 0.0009(16) _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 2.389(3) . ? Eu1 O1 2.396(3) . ? Eu1 O7 2.410(3) . ? Eu1 O4 2.419(3) . ? Eu1 O9 2.439(3) . ? Eu1 O6 2.441(3) . ? Eu1 O2 2.449(3) . ? Eu1 O3 2.459(3) . ? Eu1 O8 2.468(3) . ? Eu1 H9A 2.755(18) . ? Ag1 N2 2.218(4) 1_556 ? Ag1 N4 2.239(4) 2_667 ? Ag1 N1 2.260(4) . ? Ag1 N3 2.361(4) 2_677 ? O1 C2 1.251(4) . ? O2 C4 1.255(4) . ? O3 C10 1.244(4) . ? O4 C8 1.241(4) . ? O5 C14 1.246(4) . ? O6 C16 1.250(5) . ? O7 C20 1.245(4) . ? O8 C22 1.245(4) . ? O9 H9A 0.867(17) . ? O9 H9B 0.838(18) . ? N1 C6 1.142(5) . ? N2 C12 1.150(5) . ? N2 Ag1 2.218(4) 1_554 ? N3 C18 1.155(5) . ? N3 Ag1 2.361(4) 2_677 ? N4 C24 1.147(5) . ? N4 Ag1 2.239(4) 2_667 ? C1 C2 1.511(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.425(5) . ? C3 C6 1.422(5) . ? C3 C4 1.426(5) . ? C4 C5 1.513(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.507(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.435(5) . ? C9 C12 1.416(5) . ? C9 C10 1.437(5) . ? C10 C11 1.507(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.514(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.428(5) . ? C15 C18 1.422(5) . ? C15 C16 1.423(6) . ? C16 C17 1.507(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.505(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.433(5) . ? C21 C24 1.417(5) . ? C21 C22 1.436(5) . ? C22 C23 1.510(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 O1 134.21(9) . . ? O5 Eu1 O7 113.01(10) . . ? O1 Eu1 O7 70.99(9) . . ? O5 Eu1 O4 71.95(9) . . ? O1 Eu1 O4 141.17(9) . . ? O7 Eu1 O4 132.15(9) . . ? O5 Eu1 O9 122.51(10) . . ? O1 Eu1 O9 71.14(9) . . ? O7 Eu1 O9 124.48(10) . . ? O4 Eu1 O9 70.12(9) . . ? O5 Eu1 O6 69.12(9) . . ? O1 Eu1 O6 76.69(9) . . ? O7 Eu1 O6 133.56(9) . . ? O4 Eu1 O6 93.67(9) . . ? O9 Eu1 O6 71.97(10) . . ? O5 Eu1 O2 69.90(9) . . ? O1 Eu1 O2 70.92(9) . . ? O7 Eu1 O2 67.07(9) . . ? O4 Eu1 O2 141.81(9) . . ? O9 Eu1 O2 131.87(9) . . ? O6 Eu1 O2 71.39(9) . . ? O5 Eu1 O3 67.70(9) . . ? O1 Eu1 O3 140.30(9) . . ? O7 Eu1 O3 69.52(9) . . ? O4 Eu1 O3 69.56(9) . . ? O9 Eu1 O3 131.11(9) . . ? O6 Eu1 O3 136.65(9) . . ? O2 Eu1 O3 97.01(8) . . ? O5 Eu1 O8 134.88(9) . . ? O1 Eu1 O8 90.23(9) . . ? O7 Eu1 O8 68.68(9) . . ? O4 Eu1 O8 75.90(9) . . ? O9 Eu1 O8 72.45(9) . . ? O6 Eu1 O8 144.38(9) . . ? O2 Eu1 O8 135.45(9) . . ? O3 Eu1 O8 71.90(9) . . ? O5 Eu1 H9A 128.6(10) . . ? O1 Eu1 H9A 54.0(5) . . ? O7 Eu1 H9A 115.5(8) . . ? O4 Eu1 H9A 87.6(5) . . ? O9 Eu1 H9A 17.9(4) . . ? O6 Eu1 H9A 65.7(10) . . ? O2 Eu1 H9A 115.2(5) . . ? O3 Eu1 H9A 147.0(7) . . ? O8 Eu1 H9A 79.7(9) . . ? N2 Ag1 N4 119.81(15) 1_556 2_667 ? N2 Ag1 N1 119.77(15) 1_556 . ? N4 Ag1 N1 105.57(14) 2_667 . ? N2 Ag1 N3 103.59(14) 1_556 2_677 ? N4 Ag1 N3 106.03(14) 2_667 2_677 ? N1 Ag1 N3 99.15(14) . 2_677 ? C2 O1 Eu1 136.9(2) . . ? C4 O2 Eu1 136.7(2) . . ? C10 O3 Eu1 134.9(3) . . ? C8 O4 Eu1 137.8(2) . . ? C14 O5 Eu1 135.7(3) . . ? C16 O6 Eu1 134.3(3) . . ? C20 O7 Eu1 136.9(2) . . ? C22 O8 Eu1 135.2(2) . . ? Eu1 O9 H9A 102.2(14) . . ? Eu1 O9 H9B 164(3) . . ? H9A O9 H9B 93(2) . . ? C6 N1 Ag1 153.9(3) . . ? C12 N2 Ag1 162.0(4) . 1_554 ? C18 N3 Ag1 142.1(4) . 2_677 ? C24 N4 Ag1 162.5(4) . 2_667 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.2(3) . . ? O1 C2 C1 117.4(3) . . ? C3 C2 C1 118.4(3) . . ? C6 C3 C2 117.4(3) . . ? C6 C3 C4 117.8(3) . . ? C2 C3 C4 124.7(3) . . ? O2 C4 C3 123.7(3) . . ? O2 C4 C5 116.2(3) . . ? C3 C4 C5 120.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.9(5) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 C9 123.3(3) . . ? O4 C8 C7 117.4(3) . . ? C9 C8 C7 119.3(3) . . ? C12 C9 C8 118.9(3) . . ? C12 C9 C10 117.0(3) . . ? C8 C9 C10 124.0(3) . . ? O3 C10 C9 123.0(3) . . ? O3 C10 C11 118.3(4) . . ? C9 C10 C11 118.7(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 177.5(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 123.2(4) . . ? O5 C14 C13 116.6(3) . . ? C15 C14 C13 120.2(3) . . ? C18 C15 C16 118.9(4) . . ? C18 C15 C14 117.6(4) . . ? C16 C15 C14 123.5(3) . . ? O6 C16 C15 123.8(4) . . ? O6 C16 C17 117.5(4) . . ? C15 C16 C17 118.7(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 178.5(5) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 C21 122.9(4) . . ? O7 C20 C19 116.4(3) . . ? C21 C20 C19 120.6(3) . . ? C24 C21 C20 118.5(4) . . ? C24 C21 C22 117.8(4) . . ? C20 C21 C22 123.7(3) . . ? O8 C22 C21 123.3(4) . . ? O8 C22 C23 118.3(4) . . ? C21 C22 C23 118.3(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C21 177.9(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.738 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.142 data_5b _database_code_depnum_ccdc_archive 'CCDC 845899' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5b _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Ag Eu N4 O8, 2(H O0.50)' _chemical_formula_sum 'C24 H26 Ag Eu N4 O9' _chemical_formula_weight 774.32 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 'P 2 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' _cell_length_a 7.7092(8) _cell_length_b 9.1132(10) _cell_length_c 12.2839(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 863.01(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5517 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.83 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6068 _exptl_absorpt_correction_T_max 0.6988 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13773 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.69 _reflns_number_total 2695 _reflns_number_gt 2666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; One water molecule is situated in general position close to Wyckoff position 1d. It has therefore been assigned site occupancy of 0.25. 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^)+(0.0519P)^2^+0.7233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(18) _refine_ls_number_reflns 2695 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.023 _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 Eu1 Eu 1.0000 0.5000 0.5000 0.01814(10) Uani 1 4 d S . . Ag2 Ag 0.5000 0.0000 1.0000 0.02857(12) Uani 1 4 d S . . O1 O 0.7580(4) 0.3680(4) 0.5613(2) 0.0319(7) Uani 1 1 d . . . O2 O 1.0787(4) 0.3537(4) 0.6559(3) 0.0337(7) Uani 1 1 d . . . C1 C 0.5124(12) 0.2892(9) 0.6597(5) 0.0641(19) Uani 1 1 d . . . H1A H 0.4529 0.3363 0.5985 0.096 Uiso 1 1 calc R . . H1B H 0.4715 0.3321 0.7282 0.096 Uiso 1 1 calc R . . H1C H 0.4875 0.1837 0.6592 0.096 Uiso 1 1 calc R . . C2 C 0.7058(6) 0.3130(6) 0.6492(4) 0.0344(10) Uani 1 1 d . . . C3 C 0.8179(6) 0.2748(6) 0.7363(4) 0.0323(9) Uani 1 1 d . . . C4 C 1.0013(12) 0.2965(4) 0.7339(3) 0.0343(7) Uani 1 1 d . . . C5 C 1.1069(8) 0.2422(11) 0.8300(5) 0.078(3) Uani 1 1 d . . . H5A H 1.2105 0.1911 0.8034 0.117 Uiso 1 1 calc R . . H5B H 1.0367 0.1745 0.8735 0.117 Uiso 1 1 calc R . . H5C H 1.1419 0.3259 0.8750 0.117 Uiso 1 1 calc R . . C6 C 0.7411(7) 0.2010(7) 0.8268(4) 0.0433(12) Uani 1 1 d . . . N1 N 0.6761(7) 0.1448(6) 0.8989(4) 0.0542(13) Uani 1 1 d . . . O3 O 0.884(2) -0.005(4) 0.5410(11) 0.065(4) Uiso 0.25 1 d P . . H3A H 0.7817 -0.0011 0.5235 0.097 Uiso 0.25 1 d PR . . H3B H 0.8734 -0.0033 0.6073 0.097 Uiso 0.25 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 Eu1 0.01194(13) 0.02699(15) 0.01548(14) 0.000 0.000 0.000 Ag2 0.0278(2) 0.0388(3) 0.0191(2) 0.000 0.000 0.000 O1 0.0224(14) 0.0475(18) 0.0259(15) 0.0095(13) -0.0003(11) -0.0109(13) O2 0.0181(14) 0.054(2) 0.0293(15) 0.0155(14) -0.0005(12) 0.0032(13) C1 0.028(3) 0.110(5) 0.055(3) 0.031(3) -0.007(4) -0.021(5) C2 0.0213(19) 0.053(3) 0.029(2) 0.0121(19) 0.0021(16) -0.0054(18) C3 0.022(2) 0.047(2) 0.027(2) 0.0125(18) 0.0039(15) 0.0034(17) C4 0.0248(16) 0.050(2) 0.0281(16) 0.0133(14) -0.007(3) 0.005(4) C5 0.030(3) 0.155(8) 0.049(4) 0.057(4) -0.005(3) 0.004(4) C6 0.031(2) 0.063(3) 0.036(3) 0.019(2) 0.006(2) 0.006(2) N1 0.047(3) 0.072(3) 0.044(3) 0.029(2) 0.011(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.344(3) 2_765 ? Eu1 O1 2.344(3) 4_566 ? Eu1 O1 2.344(3) 3_756 ? Eu1 O1 2.344(3) . ? Eu1 O2 2.411(3) . ? Eu1 O2 2.412(3) 3_756 ? Eu1 O2 2.412(3) 2_765 ? Eu1 O2 2.412(3) 4_566 ? Ag2 N1 2.265(5) . ? Ag2 N1 2.265(5) 2_655 ? Ag2 N1 2.265(5) 4_557 ? Ag2 N1 2.265(5) 3_657 ? O1 C2 1.256(5) . ? O2 C4 1.243(6) . ? C1 C2 1.512(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.419(6) . ? C3 C6 1.427(6) . ? C3 C4 1.428(10) . ? C4 C5 1.517(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.139(6) . ? O3 O3 1.01(3) 4_556 ? O3 O3 1.79(3) 2_755 ? O3 H3A 0.8201 . ? O3 H3B 0.8195 . ? 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 Eu1 O1 118.23(17) 2_765 4_566 ? O1 Eu1 O1 74.54(16) 2_765 3_756 ? O1 Eu1 O1 142.53(15) 4_566 3_756 ? O1 Eu1 O1 142.52(15) 2_765 . ? O1 Eu1 O1 74.54(16) 4_566 . ? O1 Eu1 O1 118.23(17) 3_756 . ? O1 Eu1 O2 80.11(11) 2_765 . ? O1 Eu1 O2 137.67(10) 4_566 . ? O1 Eu1 O2 76.77(11) 3_756 . ? O1 Eu1 O2 70.21(11) . . ? O1 Eu1 O2 137.67(10) 2_765 3_756 ? O1 Eu1 O2 80.11(11) 4_566 3_756 ? O1 Eu1 O2 70.21(11) 3_756 3_756 ? O1 Eu1 O2 76.77(11) . 3_756 ? O2 Eu1 O2 112.88(18) . 3_756 ? O1 Eu1 O2 70.21(11) 2_765 2_765 ? O1 Eu1 O2 76.77(11) 4_566 2_765 ? O1 Eu1 O2 137.67(10) 3_756 2_765 ? O1 Eu1 O2 80.11(11) . 2_765 ? O2 Eu1 O2 74.81(17) . 2_765 ? O2 Eu1 O2 150.84(15) 3_756 2_765 ? O1 Eu1 O2 76.77(11) 2_765 4_566 ? O1 Eu1 O2 70.21(11) 4_566 4_566 ? O1 Eu1 O2 80.11(11) 3_756 4_566 ? O1 Eu1 O2 137.67(10) . 4_566 ? O2 Eu1 O2 150.84(15) . 4_566 ? O2 Eu1 O2 74.81(17) 3_756 4_566 ? O2 Eu1 O2 112.88(18) 2_765 4_566 ? N1 Ag2 N1 113.5(3) . 2_655 ? N1 Ag2 N1 106.3(3) . 4_557 ? N1 Ag2 N1 108.7(3) 2_655 4_557 ? N1 Ag2 N1 108.7(3) . 3_657 ? N1 Ag2 N1 106.3(3) 2_655 3_657 ? N1 Ag2 N1 113.5(3) 4_557 3_657 ? C2 O1 Eu1 137.4(3) . . ? C4 O2 Eu1 136.3(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.5(4) . . ? O1 C2 C1 116.5(4) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C6 116.8(4) . . ? C2 C3 C4 123.6(4) . . ? C6 C3 C4 119.5(4) . . ? O2 C4 C3 123.3(5) . . ? O2 C4 C5 118.6(7) . . ? C3 C4 C5 118.1(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 178.1(6) . . ? C6 N1 Ag2 162.2(6) . . ? O3 O3 O3 89.8(4) 4_556 2_755 ? O3 O3 H3A 74.7 4_556 . ? O3 O3 H3A 164.0 2_755 . ? O3 O3 H3B 171.7 4_556 . ? O3 O3 H3B 95.8 2_755 . ? H3A O3 H3B 99.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.69 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.406 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.187 data_6b _database_code_depnum_ccdc_archive 'CCDC 845900' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 6b _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Ag N4 O8 Yb, C2 H3 N, H2 O' _chemical_formula_sum 'C26 H29 Ag N5 O9 Yb' _chemical_formula_weight 836.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P222 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' _cell_length_a 7.6835(2) _cell_length_b 8.6805(2) _cell_length_c 12.3540(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 823.97(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7143 _cell_measurement_theta_min 8.50 _cell_measurement_theta_max 65.86 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 409 _exptl_absorpt_coefficient_mu 10.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1742 _exptl_absorpt_correction_T_max 0.5760 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9836 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 8.50 _diffrn_reflns_theta_max 66.33 _reflns_number_total 1371 _reflns_number_gt 1365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; One acetonitrile molecule is disordered over two postions. One water molecule occupies Wyckoff position 1a and shows orientational disorder. 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^)+(0.0273P)^2^+2.8566P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 1371 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 0.5000 1.0000 0.0310(2) Uani 1 4 d S . . Yb2 Yb 0.5000 0.0000 0.5000 0.01658(19) Uani 1 4 d S . . O1 O 0.4156(6) 0.1492(6) 0.6475(4) 0.0307(11) Uani 1 1 d . . . O2 O 0.7362(6) 0.1346(5) 0.5575(3) 0.0275(10) Uani 1 1 d . . . C1 C 0.7546(11) 0.2958(10) 0.8238(6) 0.0422(19) Uani 1 1 d . . . C2 C 0.6768(9) 0.2278(9) 0.7307(5) 0.0321(16) Uani 1 1 d . . . C3 C 0.4941(17) 0.2108(8) 0.7262(4) 0.0377(15) Uani 1 1 d . . . C4 C 0.7890(9) 0.1920(8) 0.6445(5) 0.0279(15) Uani 1 1 d . . . C5 C 0.3859(13) 0.2684(17) 0.8191(8) 0.086(5) Uani 1 1 d . . . H5A H 0.3085 0.3506 0.7938 0.129 Uiso 1 1 calc R . . H5B H 0.4625 0.3086 0.8759 0.129 Uiso 1 1 calc R . . H5C H 0.3161 0.1835 0.8483 0.129 Uiso 1 1 calc R . . C6 C 0.9832(16) 0.2215(11) 0.6529(6) 0.054(2) Uani 1 1 d . . . H6A H 1.0417 0.1802 0.5887 0.080 Uiso 1 1 calc R . . H6B H 1.0290 0.1706 0.7178 0.080 Uiso 1 1 calc R . . H6C H 1.0044 0.3326 0.6578 0.080 Uiso 1 1 calc R . . N1 N 0.8220(11) 0.3511(10) 0.8974(6) 0.064(2) Uani 1 1 d . . . N3 N 0.5000 0.5000 0.5000 0.106(6) Uiso 1 4 d SD . . C9 C 0.357(2) 0.5000 0.5000 0.059(5) Uiso 0.50 2 d SPD . . C10 C 0.207(4) 0.5000 0.5000 0.087(8) Uiso 0.50 2 d SP . . H10A H 0.1644 0.4551 0.5678 0.131 Uiso 0.25 1 d PR . . H10B H 0.1644 0.4389 0.4388 0.131 Uiso 0.25 1 d PR . . H10C H 0.1644 0.6060 0.4934 0.131 Uiso 0.25 1 d PR . . O3 O 0.0000 0.0000 0.0000 0.230(14) Uiso 1 4 d S . . H3A H 0.0846 0.0576 0.0000 0.276 Uiso 0.25 1 d PR . . H3B H -0.0846 0.0576 0.0000 0.276 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0280(4) 0.0479(5) 0.0171(4) 0.000 0.000 0.000 Yb2 0.0191(3) 0.0177(3) 0.0130(3) 0.000 0.000 0.000 O1 0.024(2) 0.049(3) 0.020(2) -0.008(2) -0.0016(19) 0.004(2) O2 0.023(2) 0.038(3) 0.021(2) -0.002(2) -0.0033(19) -0.012(2) C1 0.036(5) 0.056(5) 0.034(4) -0.009(4) -0.008(4) 0.011(4) C2 0.031(4) 0.039(4) 0.027(4) -0.005(3) -0.009(3) 0.000(3) C3 0.035(3) 0.052(4) 0.026(3) -0.013(3) 0.001(5) 0.014(7) C4 0.030(4) 0.028(4) 0.026(4) 0.000(3) -0.006(3) -0.003(3) C5 0.033(5) 0.176(13) 0.048(6) -0.065(7) -0.004(4) 0.021(6) C6 0.034(5) 0.094(6) 0.033(3) -0.010(4) -0.003(5) -0.011(7) N1 0.054(5) 0.089(6) 0.048(4) -0.035(4) -0.027(4) 0.017(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 Ag1 N1 2.269(8) 3_757 ? Ag1 N1 2.269(8) 2_765 ? Ag1 N1 2.269(8) 4_567 ? Ag1 N1 2.269(8) . ? Yb2 O2 2.272(4) . ? Yb2 O2 2.272(4) 2_655 ? Yb2 O2 2.272(4) 3_656 ? Yb2 O2 2.272(4) 4_556 ? Yb2 O1 2.328(5) 4_556 ? Yb2 O1 2.328(5) 2_655 ? Yb2 O1 2.328(5) 3_656 ? Yb2 O1 2.328(5) . ? O1 C3 1.263(10) . ? O2 C4 1.252(8) . ? C1 N1 1.152(10) . ? C1 C2 1.424(10) . ? C2 C4 1.406(10) . ? C2 C3 1.413(14) . ? C3 C5 1.502(11) . ? C4 C6 1.518(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N3 C9 1.101(16) . ? N3 C9 1.101(16) 2_665 ? C9 C10 1.15(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O3 H3A 0.8203 . ? O3 H3B 0.8203 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 105.9(4) 3_757 2_765 ? N1 Ag1 N1 112.1(5) 3_757 4_567 ? N1 Ag1 N1 110.5(4) 2_765 4_567 ? N1 Ag1 N1 110.5(4) 3_757 . ? N1 Ag1 N1 112.1(5) 2_765 . ? N1 Ag1 N1 105.9(4) 4_567 . ? O2 Yb2 O2 143.6(2) . 2_655 ? O2 Yb2 O2 118.1(2) . 3_656 ? O2 Yb2 O2 74.0(2) 2_655 3_656 ? O2 Yb2 O2 74.0(2) . 4_556 ? O2 Yb2 O2 118.1(2) 2_655 4_556 ? O2 Yb2 O2 143.6(2) 3_656 4_556 ? O2 Yb2 O1 138.86(16) . 4_556 ? O2 Yb2 O1 74.71(15) 2_655 4_556 ? O2 Yb2 O1 79.57(17) 3_656 4_556 ? O2 Yb2 O1 72.04(16) 4_556 4_556 ? O2 Yb2 O1 79.57(17) . 2_655 ? O2 Yb2 O1 72.04(16) 2_655 2_655 ? O2 Yb2 O1 138.86(16) 3_656 2_655 ? O2 Yb2 O1 74.71(15) 4_556 2_655 ? O1 Yb2 O1 112.4(3) 4_556 2_655 ? O2 Yb2 O1 74.71(15) . 3_656 ? O2 Yb2 O1 138.86(16) 2_655 3_656 ? O2 Yb2 O1 72.04(16) 3_656 3_656 ? O2 Yb2 O1 79.57(17) 4_556 3_656 ? O1 Yb2 O1 76.9(2) 4_556 3_656 ? O1 Yb2 O1 147.7(2) 2_655 3_656 ? O2 Yb2 O1 72.04(16) . . ? O2 Yb2 O1 79.57(17) 2_655 . ? O2 Yb2 O1 74.71(15) 3_656 . ? O2 Yb2 O1 138.86(16) 4_556 . ? O1 Yb2 O1 147.7(2) 4_556 . ? O1 Yb2 O1 76.9(2) 2_655 . ? O1 Yb2 O1 112.4(3) 3_656 . ? C3 O1 Yb2 134.9(6) . . ? C4 O2 Yb2 137.0(4) . . ? N1 C1 C2 178.0(9) . . ? C4 C2 C3 123.9(6) . . ? C4 C2 C1 116.5(7) . . ? C3 C2 C1 119.5(6) . . ? O1 C3 C2 123.3(7) . . ? O1 C3 C5 117.7(11) . . ? C2 C3 C5 119.0(7) . . ? O2 C4 C2 122.6(7) . . ? O2 C4 C6 116.4(6) . . ? C2 C4 C6 120.9(6) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 N1 Ag1 161.8(8) . . ? C9 N3 C9 180.000(3) . 2_665 ? N3 C9 C10 180.000(9) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H3A O3 H3B 104.9 . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 66.5 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.415 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.128 data_6c _database_code_depnum_ccdc_archive 'CCDC 845901' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 6c _chemical_melting_point ? _chemical_formula_moiety '4(C24 H24 Ag N4 O8 Yb), H2 O' _chemical_formula_sum 'C96 H98 Ag4 N16 O33 Yb4' _chemical_formula_weight 3127.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F 2 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x, -y+1/2, -z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 17.1271(10) _cell_length_b 24.7427(14) _cell_length_c 30.1824(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12790.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3529 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.40 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6072 _exptl_absorpt_coefficient_mu 3.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4045 _exptl_absorpt_correction_T_max 0.5215 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44572 _diffrn_reflns_av_R_equivalents 0.1468 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6585 _reflns_number_gt 5487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; One of the symmetrically independent acacCN ligands attached to Yb1 shows orientally disorder with equal site occupancy for the alternative atom sites. The distance between the thus generated alternative terminal N-positions amounts to 1.07(3) A. A water molecule is situated at Wyckoff position 8g and shows orientational disorder over two positions. 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^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(10) _refine_ls_number_reflns 6585 _refine_ls_number_parameters 347 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.028 _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 Yb1 Yb 0.2500 0.511292(18) 0.7500 0.01671(15) Uani 1 2 d S . . Yb2 Yb 0.22865(3) 1.0000 0.5000 0.02484(15) Uani 1 2 d S . . Ag1 Ag 0.49599(7) 0.76180(2) 0.62314(2) 0.0286(3) Uani 1 1 d . . . O1 O 0.1541(4) 1.0224(2) 0.55870(19) 0.0257(15) Uani 1 1 d . . . O2 O 0.1617(4) 1.0775(2) 0.48171(19) 0.0283(16) Uani 1 1 d . . . C1 C 0.0951(8) 1.0607(4) 0.6226(3) 0.052(4) Uani 1 1 d . . . H1A H 0.1323 1.0403 0.6407 0.078 Uiso 1 1 calc R . . H1B H 0.0442 1.0426 0.6230 0.078 Uiso 1 1 calc R . . H1C H 0.0897 1.0973 0.6346 0.078 Uiso 1 1 calc R . . C2 C 0.1250(6) 1.0638(4) 0.5747(3) 0.027(2) Uani 1 1 d . . . C3 C 0.1160(6) 1.1127(4) 0.5495(3) 0.030(2) Uani 1 1 d . . . C4 C 0.1349(6) 1.1165(3) 0.5039(4) 0.029(2) Uani 1 1 d . . . C5 C 0.1209(8) 1.1689(4) 0.4780(4) 0.056(4) Uani 1 1 d . . . H5A H 0.1694 1.1801 0.4635 0.084 Uiso 1 1 calc R . . H5B H 0.1037 1.1973 0.4985 0.084 Uiso 1 1 calc R . . H5C H 0.0805 1.1628 0.4556 0.084 Uiso 1 1 calc R . . C6 C 0.0875(6) 1.1588(4) 0.5701(4) 0.031(3) Uani 1 1 d . . . N1 N 0.0652(6) 1.1982(4) 0.5872(3) 0.046(3) Uani 1 1 d . . . O3 O 0.3157(4) 0.5404(2) 0.68949(19) 0.0251(15) Uani 1 1 d . . . O4 O 0.3220(3) 0.5861(2) 0.77169(18) 0.0188(13) Uani 1 1 d . . . C7 C 0.3445(5) 0.5842(3) 0.6762(3) 0.018(2) Uani 1 1 d . . . C8 C 0.3626(6) 0.6274(3) 0.7051(3) 0.020(2) Uani 1 1 d . . . C9 C 0.3509(6) 0.6253(3) 0.7514(4) 0.026(2) Uani 1 1 d . . . C10 C 0.3732(8) 0.6742(4) 0.7802(4) 0.051(3) Uani 1 1 d . . . H10A H 0.4287 0.6721 0.7879 0.077 Uiso 1 1 calc R . . H10B H 0.3418 0.6741 0.8073 0.077 Uiso 1 1 calc R . . H10C H 0.3633 0.7076 0.7637 0.077 Uiso 1 1 calc R . . C11 C 0.3587(7) 0.5911(4) 0.6277(3) 0.038(3) Uani 1 1 d . . . H11A H 0.4148 0.5886 0.6217 0.057 Uiso 1 1 calc R . . H11B H 0.3395 0.6266 0.6182 0.057 Uiso 1 1 calc R . . H11C H 0.3311 0.5627 0.6113 0.057 Uiso 1 1 calc R . . C12 C 0.3961(7) 0.6740(4) 0.6854(3) 0.031(3) Uani 1 1 d . . . N2 N 0.4209(6) 0.7120(4) 0.6704(3) 0.046(3) Uani 1 1 d . . . O5 O 0.2982(4) 0.9705(3) 0.5589(2) 0.044(2) Uani 1 1 d . . . O6 O 0.3028(5) 0.9286(3) 0.4766(2) 0.051(2) Uani 1 1 d . . . C13 C 0.3525(10) 0.9185(7) 0.6187(4) 0.118(8) Uani 1 1 d . . . H13A H 0.3686 0.9525 0.6326 0.178 Uiso 1 1 calc R . . H13B H 0.3957 0.8926 0.6199 0.178 Uiso 1 1 calc R . . H13C H 0.3074 0.9037 0.6345 0.178 Uiso 1 1 calc R . . C14 C 0.3308(8) 0.9288(6) 0.5710(4) 0.069(5) Uani 1 1 d . . . C15 C 0.3471(8) 0.8856(6) 0.5417(5) 0.070(5) Uani 1 1 d . . . C16 C 0.3366(8) 0.8902(6) 0.4952(6) 0.069(4) Uani 1 1 d . . . C17 C 0.3640(10) 0.8426(5) 0.4668(5) 0.088(6) Uani 1 1 d . . . H17A H 0.3291 0.8118 0.4714 0.132 Uiso 1 1 calc R . . H17B H 0.4173 0.8326 0.4754 0.132 Uiso 1 1 calc R . . H17C H 0.3633 0.8530 0.4355 0.132 Uiso 1 1 calc R . . N3 N 0.4116(9) 0.8013(6) 0.5747(5) 0.112(6) Uani 1 1 d U . . C18 C 0.3841(11) 0.8409(7) 0.5599(5) 0.102(6) Uani 1 1 d U . . O7A O 0.2550(8) 0.4399(4) 0.7024(4) 0.027(3) Uiso 0.50 1 d P . 1 O8A O 0.1251(6) 0.4847(4) 0.7376(4) 0.025(3) Uiso 0.50 1 d P . 1 C19A C 0.2481(14) 0.3663(8) 0.6536(7) 0.053(6) Uiso 0.50 1 d P . 1 H19A H 0.2844 0.3848 0.6337 0.079 Uiso 0.50 1 calc PR . 1 H19B H 0.2085 0.3472 0.6362 0.079 Uiso 0.50 1 calc PR . 1 H19C H 0.2769 0.3402 0.6718 0.079 Uiso 0.50 1 calc PR . 1 C20A C 0.2086(10) 0.4075(7) 0.6836(6) 0.020(4) Uiso 0.50 1 d P . 1 C21A C 0.1224(11) 0.4102(8) 0.6883(7) 0.019(4) Uiso 0.50 1 d P . 1 C22A C 0.0912(11) 0.4488(7) 0.7162(6) 0.025(4) Uiso 0.50 1 d P . 1 C23A C 0.001(2) 0.4474(9) 0.7221(7) 0.069(7) Uiso 0.50 1 d P . 1 H23A H -0.0124 0.4277 0.7492 0.104 Uiso 0.50 1 calc PR . 1 H23B H -0.0229 0.4292 0.6965 0.104 Uiso 0.50 1 calc PR . 1 H23C H -0.0192 0.4844 0.7241 0.104 Uiso 0.50 1 calc PR . 1 C24A C 0.0797(12) 0.3706(8) 0.6676(7) 0.026(5) Uiso 0.50 1 d P . 1 N4A N 0.0418(11) 0.3391(7) 0.6478(6) 0.041(5) Uiso 0.50 1 d P . 1 O7B O 0.3173(7) 0.4842(5) 0.8098(4) 0.026(3) Uiso 0.50 1 d P . 2 O8B O 0.3248(8) 0.4389(5) 0.7287(4) 0.036(3) Uiso 0.50 1 d P . 2 C19B C 0.3547(16) 0.4325(9) 0.8762(8) 0.053(7) Uiso 0.50 1 d P . 2 H19D H 0.3486 0.4679 0.8904 0.079 Uiso 0.50 1 calc PR . 2 H19E H 0.4054 0.4171 0.8843 0.079 Uiso 0.50 1 calc PR . 2 H19F H 0.3129 0.4084 0.8862 0.079 Uiso 0.50 1 calc PR . 2 C20B C 0.3501(12) 0.4392(8) 0.8249(7) 0.030(5) Uiso 0.50 1 d P . 2 C21B C 0.3650(13) 0.3973(9) 0.7954(8) 0.031(5) Uiso 0.50 1 d P . 2 C22B C 0.3589(14) 0.3974(8) 0.7482(10) 0.048(6) Uiso 0.50 1 d P . 2 C23B C 0.389(2) 0.3450(12) 0.7210(12) 0.105(12) Uiso 0.50 1 d P . 2 H23D H 0.3622 0.3127 0.7321 0.158 Uiso 0.50 1 calc PR . 2 H23E H 0.4454 0.3408 0.7252 0.158 Uiso 0.50 1 calc PR . 2 H23F H 0.3775 0.3497 0.6895 0.158 Uiso 0.50 1 calc PR . 2 C24B C 0.3982(13) 0.3524(10) 0.8157(8) 0.036(6) Uiso 0.50 1 d P . 2 N4B N 0.4246(12) 0.3117(8) 0.8323(7) 0.054(6) Uiso 0.50 1 d P . 2 O10D O 0.5000 0.5000 0.0260(7) 0.080(7) Uiso 0.50 2 d SP . . H10D H 0.5000 0.5074 0.0000 0.096 Uiso 0.50 2 d SPR . . H10E H 0.5464 0.5043 0.0318 0.096 Uiso 0.25 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 Yb1 0.0245(3) 0.0111(3) 0.0146(2) 0.000 -0.0007(2) 0.000 Yb2 0.0306(3) 0.0192(3) 0.0248(3) 0.0101(3) 0.000 0.000 Ag1 0.0486(6) 0.0161(5) 0.0212(3) -0.0003(3) 0.0034(6) -0.0034(4) O1 0.038(4) 0.012(3) 0.027(4) -0.002(3) -0.005(3) 0.003(3) O2 0.045(4) 0.017(3) 0.023(4) 0.000(3) -0.011(3) 0.006(3) C1 0.100(12) 0.028(6) 0.028(6) -0.012(5) 0.011(7) 0.006(6) C2 0.029(6) 0.017(5) 0.034(6) 0.003(4) -0.010(5) 0.005(4) C3 0.038(6) 0.021(5) 0.033(6) -0.001(4) -0.009(5) -0.001(5) C4 0.041(5) 0.014(4) 0.031(6) 0.008(5) -0.003(6) 0.003(4) C5 0.109(11) 0.015(5) 0.045(7) -0.001(5) -0.006(7) 0.028(6) C6 0.036(6) 0.021(5) 0.037(7) 0.000(5) -0.007(5) 0.011(5) N1 0.056(7) 0.037(6) 0.046(6) 0.006(5) -0.001(5) 0.009(5) O3 0.044(4) 0.017(3) 0.014(3) -0.008(3) 0.008(3) -0.003(3) O4 0.026(4) 0.017(3) 0.013(3) 0.004(2) -0.001(3) -0.004(3) C7 0.025(5) 0.010(4) 0.018(5) -0.003(4) 0.008(4) -0.004(4) C8 0.029(6) 0.017(5) 0.013(5) 0.001(3) 0.003(4) -0.005(4) C9 0.026(5) 0.020(4) 0.032(5) -0.007(6) 0.009(5) -0.005(4) C10 0.078(10) 0.041(7) 0.035(7) 0.003(5) -0.020(6) -0.030(7) C11 0.063(9) 0.027(6) 0.025(6) 0.001(5) 0.005(6) -0.008(6) C12 0.046(7) 0.029(6) 0.019(6) -0.004(4) 0.003(5) -0.013(5) N2 0.079(8) 0.034(5) 0.025(5) 0.003(4) 0.013(5) -0.038(5) O5 0.030(4) 0.063(5) 0.041(4) 0.034(4) -0.004(3) 0.007(4) O6 0.058(5) 0.052(5) 0.044(5) 0.032(4) 0.013(4) 0.026(4) C13 0.109(15) 0.21(2) 0.033(9) 0.040(11) 0.029(9) 0.105(14) C14 0.054(9) 0.111(13) 0.043(8) 0.045(8) 0.038(7) 0.038(9) C15 0.057(9) 0.097(12) 0.056(9) 0.056(8) 0.035(7) 0.045(8) C16 0.074(9) 0.077(10) 0.055(10) 0.031(8) 0.022(9) 0.048(8) C17 0.119(15) 0.068(10) 0.077(11) 0.056(9) 0.025(10) 0.046(10) N3 0.125(11) 0.119(10) 0.092(10) 0.058(8) 0.011(8) 0.092(9) C18 0.117(12) 0.126(12) 0.063(10) 0.059(9) 0.051(9) 0.087(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 Yb1 O7B 2.245(11) 12_556 ? Yb1 O7B 2.245(11) . ? Yb1 O3 2.263(6) 12_556 ? Yb1 O3 2.263(6) . ? Yb1 O8A 2.269(11) 12_556 ? Yb1 O8A 2.269(11) . ? Yb1 O7A 2.278(11) . ? Yb1 O7A 2.278(11) 12_556 ? Yb1 O8B 2.293(13) . ? Yb1 O8B 2.293(13) 12_556 ? Yb1 O4 2.319(6) . ? Yb1 O4 2.319(5) 12_556 ? Yb2 O1 2.254(6) 3_576 ? Yb2 O1 2.254(6) . ? Yb2 O5 2.262(6) 3_576 ? Yb2 O5 2.262(6) . ? Yb2 O6 2.287(7) . ? Yb2 O6 2.287(7) 3_576 ? Yb2 O2 2.301(6) 3_576 ? Yb2 O2 2.301(6) . ? Ag1 N4A 2.197(18) 13 ? Ag1 N1 2.248(10) 13_545 ? Ag1 N3 2.276(11) . ? Ag1 N4B 2.28(2) 8_656 ? Ag1 N2 2.282(8) . ? O1 C2 1.236(10) . ? O2 C4 1.261(11) . ? C1 C2 1.536(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.438(12) . ? C3 C6 1.387(13) . ? C3 C4 1.417(15) . ? C4 C5 1.532(13) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.168(12) . ? N1 Ag1 2.248(10) 13_455 ? O3 C7 1.256(10) . ? O4 C9 1.249(10) . ? C7 C8 1.413(11) . ? C7 C11 1.496(12) . ? C8 C9 1.415(14) . ? C8 C12 1.418(12) . ? C9 C10 1.537(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.126(12) . ? O5 C14 1.229(14) . ? O6 C16 1.246(13) . ? C13 C14 1.507(17) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.41(2) . ? C15 C18 1.387(17) . ? C15 C16 1.42(2) . ? C16 C17 1.529(18) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N3 C18 1.175(16) . ? O7A C20A 1.26(2) . ? O8A C22A 1.24(2) . ? C19A C20A 1.52(3) . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A C21A 1.48(3) . ? C21A C24A 1.37(3) . ? C21A C22A 1.38(3) . ? C22A C23A 1.56(4) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C24A N4A 1.18(2) . ? N4A Ag1 2.197(18) 13_445 ? O7B C20B 1.33(2) . ? O8B C22B 1.32(2) . ? C19B C20B 1.56(3) . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B C21B 1.39(3) . ? C21B C24B 1.39(3) . ? C21B C22B 1.43(4) . ? C22B C23B 1.62(4) . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B N4B 1.21(3) . ? N4B Ag1 2.28(2) 8_646 ? O10D O10D 1.57(4) 3_565 ? O10D H10D 0.8055 . ? O10D H10E 0.8203 . ? 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 O7B Yb1 O7B 145.2(6) 12_556 . ? O7B Yb1 O3 119.3(3) 12_556 12_556 ? O7B Yb1 O3 72.6(3) . 12_556 ? O7B Yb1 O3 72.6(3) 12_556 . ? O7B Yb1 O3 119.3(3) . . ? O3 Yb1 O3 142.9(3) 12_556 . ? O7B Yb1 O8A 122.0(4) 12_556 12_556 ? O7B Yb1 O8A 45.3(4) . 12_556 ? O3 Yb1 O8A 115.4(3) 12_556 12_556 ? O3 Yb1 O8A 75.9(3) . 12_556 ? O7B Yb1 O8A 45.3(4) 12_556 . ? O7B Yb1 O8A 122.0(4) . . ? O3 Yb1 O8A 75.9(3) 12_556 . ? O3 Yb1 O8A 115.4(3) . . ? O8A Yb1 O8A 146.3(5) 12_556 . ? O7B Yb1 O7A 44.0(4) 12_556 . ? O7B Yb1 O7A 104.8(4) . . ? O3 Yb1 O7A 140.7(3) 12_556 . ? O3 Yb1 O7A 73.7(3) . . ? O8A Yb1 O7A 81.0(4) 12_556 . ? O8A Yb1 O7A 72.9(4) . . ? O7B Yb1 O7A 104.8(4) 12_556 12_556 ? O7B Yb1 O7A 44.0(4) . 12_556 ? O3 Yb1 O7A 73.7(3) 12_556 12_556 ? O3 Yb1 O7A 140.7(3) . 12_556 ? O8A Yb1 O7A 72.9(4) 12_556 12_556 ? O8A Yb1 O7A 81.0(4) . 12_556 ? O7A Yb1 O7A 78.3(6) . 12_556 ? O7B Yb1 O8B 80.1(5) 12_556 . ? O7B Yb1 O8B 72.8(4) . . ? O3 Yb1 O8B 138.8(4) 12_556 . ? O3 Yb1 O8B 75.2(4) . . ? O8A Yb1 O8B 45.0(4) 12_556 . ? O8A Yb1 O8B 104.7(4) . . ? O7A Yb1 O8B 36.6(5) . . ? O7A Yb1 O8B 65.9(4) 12_556 . ? O7B Yb1 O8B 72.8(4) 12_556 12_556 ? O7B Yb1 O8B 80.1(5) . 12_556 ? O3 Yb1 O8B 75.2(4) 12_556 12_556 ? O3 Yb1 O8B 138.8(4) . 12_556 ? O8A Yb1 O8B 104.7(4) 12_556 12_556 ? O8A Yb1 O8B 45.0(4) . 12_556 ? O7A Yb1 O8B 65.9(4) . 12_556 ? O7A Yb1 O8B 36.6(5) 12_556 12_556 ? O8B Yb1 O8B 77.3(7) . 12_556 ? O7B Yb1 O4 137.6(3) 12_556 . ? O7B Yb1 O4 74.8(3) . . ? O3 Yb1 O4 77.4(2) 12_556 . ? O3 Yb1 O4 73.1(2) . . ? O8A Yb1 O4 71.6(3) 12_556 . ? O8A Yb1 O4 141.2(3) . . ? O7A Yb1 O4 141.0(4) . . ? O7A Yb1 O4 117.5(3) 12_556 . ? O8B Yb1 O4 113.9(4) . . ? O8B Yb1 O4 147.3(4) 12_556 . ? O7B Yb1 O4 74.8(3) 12_556 12_556 ? O7B Yb1 O4 137.6(3) . 12_556 ? O3 Yb1 O4 73.1(2) 12_556 12_556 ? O3 Yb1 O4 77.4(2) . 12_556 ? O8A Yb1 O4 141.2(3) 12_556 12_556 ? O8A Yb1 O4 71.6(3) . 12_556 ? O7A Yb1 O4 117.5(3) . 12_556 ? O7A Yb1 O4 141.0(4) 12_556 12_556 ? O8B Yb1 O4 147.3(4) . 12_556 ? O8B Yb1 O4 113.9(4) 12_556 12_556 ? O4 Yb1 O4 74.0(3) . 12_556 ? O1 Yb2 O1 110.9(3) 3_576 . ? O1 Yb2 O5 76.1(2) 3_576 3_576 ? O1 Yb2 O5 146.9(2) . 3_576 ? O1 Yb2 O5 146.9(2) 3_576 . ? O1 Yb2 O5 76.1(2) . . ? O5 Yb2 O5 116.4(3) 3_576 . ? O1 Yb2 O6 83.2(3) 3_576 . ? O1 Yb2 O6 138.4(2) . . ? O5 Yb2 O6 73.4(3) 3_576 . ? O5 Yb2 O6 72.6(3) . . ? O1 Yb2 O6 138.4(2) 3_576 3_576 ? O1 Yb2 O6 83.2(3) . 3_576 ? O5 Yb2 O6 72.6(3) 3_576 3_576 ? O5 Yb2 O6 73.4(3) . 3_576 ? O6 Yb2 O6 112.6(4) . 3_576 ? O1 Yb2 O2 72.6(2) 3_576 3_576 ? O1 Yb2 O2 74.6(2) . 3_576 ? O5 Yb2 O2 136.1(3) 3_576 3_576 ? O5 Yb2 O2 78.8(2) . 3_576 ? O6 Yb2 O2 73.0(3) . 3_576 ? O6 Yb2 O2 147.8(2) 3_576 3_576 ? O1 Yb2 O2 74.6(2) 3_576 . ? O1 Yb2 O2 72.6(2) . . ? O5 Yb2 O2 78.8(2) 3_576 . ? O5 Yb2 O2 136.1(3) . . ? O6 Yb2 O2 147.8(2) . . ? O6 Yb2 O2 73.0(3) 3_576 . ? O2 Yb2 O2 120.2(3) 3_576 . ? N4A Ag1 N1 125.7(5) 13 13_545 ? N4A Ag1 N3 94.1(6) 13 . ? N1 Ag1 N3 109.0(4) 13_545 . ? N4A Ag1 N4B 27.7(6) 13 8_656 ? N1 Ag1 N4B 110.4(6) 13_545 8_656 ? N3 Ag1 N4B 121.7(7) . 8_656 ? N4A Ag1 N2 117.4(5) 13 . ? N1 Ag1 N2 102.7(3) 13_545 . ? N3 Ag1 N2 106.0(5) . . ? N4B Ag1 N2 105.1(6) 8_656 . ? C2 O1 Yb2 137.6(6) . . ? C4 O2 Yb2 133.8(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.3(10) . . ? O1 C2 C1 117.4(8) . . ? C3 C2 C1 120.3(9) . . ? C6 C3 C4 117.5(9) . . ? C6 C3 C2 119.5(10) . . ? C4 C3 C2 123.0(9) . . ? O2 C4 C3 123.2(9) . . ? O2 C4 C5 115.8(10) . . ? C3 C4 C5 120.9(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 178.4(13) . . ? C6 N1 Ag1 166.0(10) . 13_455 ? C7 O3 Yb1 136.6(5) . . ? C9 O4 Yb1 133.9(6) . . ? O3 C7 C8 122.9(8) . . ? O3 C7 C11 118.4(8) . . ? C8 C7 C11 118.7(8) . . ? C7 C8 C9 123.5(8) . . ? C7 C8 C12 116.4(8) . . ? C9 C8 C12 120.0(8) . . ? O4 C9 C8 124.6(8) . . ? O4 C9 C10 115.7(10) . . ? C8 C9 C10 119.7(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C8 177.8(13) . . ? C12 N2 Ag1 156.1(9) . . ? C14 O5 Yb2 138.1(10) . . ? C16 O6 Yb2 135.0(9) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.5(13) . . ? O5 C14 C13 122.6(14) . . ? C15 C14 C13 114.8(12) . . ? C18 C15 C14 116.4(14) . . ? C18 C15 C16 120.8(14) . . ? C14 C15 C16 122.2(12) . . ? O6 C16 C15 124.4(14) . . ? O6 C16 C17 118.6(14) . . ? C15 C16 C17 116.8(11) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 N3 Ag1 148.9(17) . . ? N3 C18 C15 176(2) . . ? C20A O7A Yb1 138.8(12) . . ? C22A O8A Yb1 137.2(11) . . ? O7A C20A C21A 123.5(16) . . ? O7A C20A C19A 114.5(16) . . ? C21A C20A C19A 122.0(17) . . ? C24A C21A C22A 124.3(18) . . ? C24A C21A C20A 117.0(17) . . ? C22A C21A C20A 118.4(17) . . ? O8A C22A C21A 129.0(18) . . ? O8A C22A C23A 115.0(17) . . ? C21A C22A C23A 116.0(18) . . ? N4A C24A C21A 176(2) . . ? C24A N4A Ag1 161.0(18) . 13_445 ? C20B O7B Yb1 138.1(12) . . ? C22B O8B Yb1 137.0(16) . . ? C20B C19B H19D 109.5 . . ? C20B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C20B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O7B C20B C21B 118.9(18) . . ? O7B C20B C19B 116.9(17) . . ? C21B C20B C19B 123.2(19) . . ? C24B C21B C20B 113(2) . . ? C24B C21B C22B 118(2) . . ? C20B C21B C22B 129(2) . . ? O8B C22B C21B 119(2) . . ? O8B C22B C23B 123(3) . . ? C21B C22B C23B 119(2) . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? N4B C24B C21B 177(3) . . ? C24B N4B Ag1 157(2) . 8_646 ? H10D O10D H10E 100.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.580 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.163 data_5d _database_code_depnum_ccdc_archive 'CCDC 845902' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5d _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Ag Eu N4 O8' _chemical_formula_sum 'C24 H24 Ag Eu N4 O8' _chemical_formula_weight 756.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8902(3) _cell_length_b 21.1723(9) _cell_length_c 16.0292(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.1973(6) _cell_angle_gamma 90.00 _cell_volume 2677.72(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9352 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.63 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 3.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6048 _exptl_absorpt_correction_T_max 0.7069 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40017 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 30.70 _reflns_number_total 7943 _reflns_number_gt 7083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0220P)^2^+2.3424P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7943 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.95811(2) 0.998003(8) 0.110724(11) 0.01551(4) Uani 1 1 d . . . Eu1 Eu 0.516323(13) 0.811897(5) 0.497515(6) 0.00995(4) Uani 1 1 d . . . O1 O 0.4094(2) 0.79019(8) 0.63325(10) 0.0176(3) Uani 1 1 d . . . O2 O 0.2898(2) 0.88488(8) 0.53190(10) 0.0156(3) Uani 1 1 d . . . O3 O 0.7471(2) 0.79347(8) 0.59350(10) 0.0163(3) Uani 1 1 d . . . O4 O 0.6301(2) 0.91040(7) 0.54359(10) 0.0163(3) Uani 1 1 d . . . O5 O 0.7740(2) 0.82040(8) 0.42289(10) 0.0179(3) Uani 1 1 d . . . O6 O 0.46140(19) 0.84726(7) 0.35876(10) 0.0142(3) Uani 1 1 d . . . O7 O 0.5777(2) 0.70331(7) 0.47973(10) 0.0144(3) Uani 1 1 d . . . O8 O 0.26228(19) 0.75661(7) 0.46754(10) 0.0150(3) Uani 1 1 d . . . C1 C 0.4174(4) 0.80563(13) 0.77898(16) 0.0312(7) Uani 1 1 d . . . H1A H 0.5368 0.8125 0.7934 0.047 Uiso 1 1 calc R . . H1B H 0.3914 0.7605 0.7825 0.047 Uiso 1 1 calc R . . H1C H 0.3454 0.8289 0.8180 0.047 Uiso 1 1 calc R . . C2 C 0.3845(3) 0.82862(11) 0.69159(14) 0.0167(5) Uani 1 1 d . . . C3 C 0.3227(3) 0.89106(11) 0.67829(14) 0.0148(4) Uani 1 1 d . . . C4 C 0.2659(3) 0.91387(11) 0.59864(14) 0.0145(4) Uani 1 1 d . . . C5 C 0.1731(3) 0.97589(12) 0.59392(16) 0.0213(5) Uani 1 1 d . . . H5A H 0.2505 1.0088 0.5743 0.032 Uiso 1 1 calc R . . H5B H 0.1308 0.9871 0.6494 0.032 Uiso 1 1 calc R . . H5C H 0.0775 0.9721 0.5550 0.032 Uiso 1 1 calc R . . C6 C 0.3150(3) 0.93197(12) 0.74883(15) 0.0190(5) Uani 1 1 d . . . C7 C 0.9311(3) 0.78781(12) 0.70950(17) 0.0263(6) Uani 1 1 d . . . H7A H 1.0316 0.8136 0.7210 0.039 Uiso 1 1 calc R . . H7B H 0.9655 0.7482 0.6830 0.039 Uiso 1 1 calc R . . H7C H 0.8726 0.7786 0.7620 0.039 Uiso 1 1 calc R . . C8 C 0.8134(3) 0.82329(11) 0.65205(14) 0.0160(4) Uani 1 1 d . . . C9 C 0.7820(3) 0.88893(11) 0.66727(15) 0.0170(5) Uani 1 1 d . . . C10 C 0.6935(3) 0.92959(11) 0.61070(15) 0.0156(4) Uani 1 1 d . . . C11 C 0.6750(4) 0.99861(11) 0.63133(18) 0.0232(6) Uani 1 1 d . . . H11A H 0.7871 1.0168 0.6422 0.035 Uiso 1 1 calc R . . H11B H 0.6041 1.0033 0.6810 0.035 Uiso 1 1 calc R . . H11C H 0.6219 1.0206 0.5842 0.035 Uiso 1 1 calc R . . C12 C 0.8463(3) 0.91634(12) 0.74201(16) 0.0215(5) Uani 1 1 d . . . C13 C 1.0186(3) 0.85319(12) 0.35092(16) 0.0209(5) Uani 1 1 d . . . H13A H 1.0663 0.8611 0.4065 0.031 Uiso 1 1 calc R . . H13B H 1.0425 0.8893 0.3146 0.031 Uiso 1 1 calc R . . H13C H 1.0698 0.8150 0.3273 0.031 Uiso 1 1 calc R . . C14 C 0.8299(3) 0.84426(10) 0.35763(14) 0.0141(4) Uani 1 1 d . . . C15 C 0.7219(3) 0.86307(10) 0.28998(14) 0.0130(4) Uani 1 1 d . . . C16 C 0.5415(3) 0.86149(10) 0.29397(14) 0.0127(4) Uani 1 1 d . . . C17 C 0.4419(3) 0.87627(12) 0.21562(14) 0.0201(5) Uani 1 1 d . . . H17A H 0.4526 0.8412 0.1762 0.030 Uiso 1 1 calc R . . H17B H 0.4862 0.9149 0.1902 0.030 Uiso 1 1 calc R . . H17C H 0.3222 0.8823 0.2298 0.030 Uiso 1 1 calc R . . C18 C 0.8017(3) 0.88427(11) 0.21596(15) 0.0156(4) Uani 1 1 d . . . C19 C 0.5987(3) 0.59167(11) 0.48304(16) 0.0188(5) Uani 1 1 d . . . H19A H 0.5611 0.5661 0.4355 0.028 Uiso 1 1 calc R . . H19B H 0.5810 0.5680 0.5348 0.028 Uiso 1 1 calc R . . H19C H 0.7195 0.6015 0.4771 0.028 Uiso 1 1 calc R . . C20 C 0.4985(3) 0.65207(11) 0.48575(13) 0.0123(4) Uani 1 1 d . . . C21 C 0.3183(3) 0.64904(10) 0.49242(13) 0.0114(4) Uani 1 1 d . . . C22 C 0.2077(3) 0.70195(10) 0.48023(13) 0.0123(4) Uani 1 1 d . . . C23 C 0.0195(3) 0.69139(12) 0.47872(17) 0.0194(5) Uani 1 1 d . . . H23A H -0.0386 0.7321 0.4729 0.029 Uiso 1 1 calc R . . H23B H -0.0155 0.6711 0.5308 0.029 Uiso 1 1 calc R . . H23C H -0.0101 0.6641 0.4315 0.029 Uiso 1 1 calc R . . C24 C 0.2411(3) 0.58934(10) 0.50320(13) 0.0123(4) Uani 1 1 d . . . N1 N 0.3161(3) 0.96454(11) 0.80629(14) 0.0268(5) Uani 1 1 d . . . N2 N 0.8948(3) 0.93902(11) 0.80258(15) 0.0298(5) Uani 1 1 d . . . N3 N 0.8713(3) 0.90077(10) 0.15689(13) 0.0211(4) Uani 1 1 d . . . N4 N 0.1730(2) 0.54159(9) 0.51173(12) 0.0163(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01868(9) 0.01536(9) 0.01249(9) -0.00178(6) 0.00001(7) -0.00088(6) Eu1 0.01199(6) 0.00908(6) 0.00880(6) 0.00004(4) 0.00032(4) -0.00059(4) O1 0.0255(9) 0.0153(8) 0.0121(8) 0.0016(6) 0.0047(7) 0.0036(7) O2 0.0179(8) 0.0160(8) 0.0131(8) 0.0015(6) 0.0004(6) 0.0024(6) O3 0.0192(8) 0.0137(8) 0.0159(8) -0.0013(6) -0.0042(6) -0.0010(6) O4 0.0189(8) 0.0128(8) 0.0172(8) -0.0010(6) -0.0014(6) -0.0019(6) O5 0.0134(8) 0.0244(9) 0.0159(8) 0.0058(7) 0.0018(6) 0.0020(7) O6 0.0145(8) 0.0168(8) 0.0112(7) 0.0018(6) 0.0013(6) -0.0001(6) O7 0.0128(7) 0.0117(7) 0.0186(8) -0.0025(6) 0.0003(6) -0.0011(6) O8 0.0131(7) 0.0120(8) 0.0198(8) 0.0010(6) -0.0004(6) -0.0005(6) C1 0.0531(19) 0.0288(15) 0.0116(12) 0.0045(10) 0.0016(12) 0.0133(13) C2 0.0187(11) 0.0190(11) 0.0125(11) 0.0011(9) 0.0041(9) 0.0007(9) C3 0.0170(10) 0.0145(11) 0.0128(10) -0.0016(8) 0.0021(8) 0.0024(8) C4 0.0132(10) 0.0150(11) 0.0152(11) 0.0019(8) 0.0027(8) 0.0016(8) C5 0.0252(13) 0.0198(12) 0.0191(12) 0.0017(10) 0.0017(10) 0.0089(10) C6 0.0202(12) 0.0195(12) 0.0173(12) 0.0016(9) 0.0024(9) 0.0052(9) C7 0.0291(14) 0.0201(13) 0.0296(14) 0.0028(11) -0.0151(11) -0.0039(11) C8 0.0163(11) 0.0174(11) 0.0143(11) 0.0010(9) 0.0000(9) -0.0039(9) C9 0.0179(11) 0.0177(11) 0.0155(11) -0.0028(9) -0.0008(9) -0.0059(9) C10 0.0144(10) 0.0119(10) 0.0206(12) -0.0028(9) 0.0043(9) -0.0045(8) C11 0.0269(14) 0.0130(11) 0.0297(14) -0.0047(10) 0.0035(11) -0.0017(9) C12 0.0200(12) 0.0220(13) 0.0224(13) -0.0031(10) -0.0004(10) -0.0050(10) C13 0.0133(11) 0.0253(13) 0.0242(13) 0.0047(10) 0.0012(9) -0.0024(9) C14 0.0142(10) 0.0125(10) 0.0158(11) -0.0009(8) 0.0012(8) 0.0024(8) C15 0.0154(10) 0.0125(10) 0.0110(10) 0.0009(8) 0.0017(8) -0.0014(8) C16 0.0160(10) 0.0089(10) 0.0133(10) -0.0009(8) 0.0000(8) -0.0001(8) C17 0.0204(11) 0.0275(13) 0.0125(11) 0.0041(10) -0.0005(9) 0.0014(10) C18 0.0153(10) 0.0142(11) 0.0173(11) 0.0012(9) 0.0001(9) 0.0003(8) C19 0.0159(11) 0.0139(11) 0.0267(13) -0.0013(9) -0.0009(9) 0.0018(9) C20 0.0140(10) 0.0137(10) 0.0091(10) -0.0014(8) -0.0021(8) 0.0001(8) C21 0.0121(10) 0.0102(10) 0.0120(10) 0.0001(8) 0.0004(8) -0.0005(8) C22 0.0118(10) 0.0153(10) 0.0099(10) -0.0005(8) 0.0012(8) -0.0001(8) C23 0.0117(10) 0.0174(12) 0.0292(13) 0.0021(10) 0.0009(9) 0.0001(9) C24 0.0129(10) 0.0150(10) 0.0090(10) -0.0018(8) 0.0001(8) 0.0034(8) N1 0.0338(13) 0.0282(12) 0.0185(11) -0.0025(9) 0.0016(9) 0.0076(10) N2 0.0323(13) 0.0311(13) 0.0258(12) -0.0073(10) -0.0042(10) -0.0069(10) N3 0.0219(10) 0.0204(10) 0.0210(11) 0.0039(8) 0.0036(8) 0.0004(8) N4 0.0168(9) 0.0158(10) 0.0163(10) -0.0010(8) 0.0023(8) -0.0005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.246(2) 3_776 ? Ag1 N3 2.293(2) . ? Ag1 N4 2.400(2) 2_655 ? Ag1 N4 2.4728(19) 4_675 ? Eu1 O7 2.3669(15) . ? Eu1 O5 2.3690(16) . ? Eu1 O8 2.3690(16) . ? Eu1 O1 2.3811(16) . ? Eu1 O6 2.3850(15) . ? Eu1 O4 2.3867(16) . ? Eu1 O3 2.4114(16) . ? Eu1 O2 2.4274(16) . ? O1 C2 1.256(3) . ? O2 C4 1.248(3) . ? O3 C8 1.245(3) . ? O4 C10 1.253(3) . ? O5 C14 1.244(3) . ? O6 C16 1.254(3) . ? O7 C20 1.256(3) . ? O8 C22 1.252(3) . ? C1 C2 1.505(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.425(3) . ? C3 C6 1.426(3) . ? C3 C4 1.435(3) . ? C4 C5 1.505(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.151(3) . ? C7 C8 1.506(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.433(3) . ? C9 C12 1.423(3) . ? C9 C10 1.430(3) . ? C10 C11 1.505(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.148(3) . ? C13 C14 1.505(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.434(3) . ? C15 C18 1.418(3) . ? C15 C16 1.425(3) . ? C16 C17 1.512(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.150(3) . ? C19 C20 1.505(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.427(3) . ? C21 C24 1.414(3) . ? C21 C22 1.433(3) . ? C22 C23 1.501(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N4 1.153(3) . ? N2 Ag1 2.246(2) 3_776 ? N4 Ag1 2.400(2) 2_645 ? N4 Ag1 2.4728(19) 4_476 ? 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 N2 Ag1 N3 119.18(8) 3_776 . ? N2 Ag1 N4 119.87(8) 3_776 2_655 ? N3 Ag1 N4 118.74(7) . 2_655 ? N2 Ag1 N4 104.14(8) 3_776 4_675 ? N3 Ag1 N4 96.25(7) . 4_675 ? N4 Ag1 N4 84.27(7) 2_655 4_675 ? O7 Eu1 O5 80.60(6) . . ? O7 Eu1 O8 70.67(5) . . ? O5 Eu1 O8 131.46(6) . . ? O7 Eu1 O1 89.76(6) . . ? O5 Eu1 O1 141.58(6) . . ? O8 Eu1 O1 77.74(6) . . ? O7 Eu1 O6 103.25(6) . . ? O5 Eu1 O6 70.05(5) . . ? O8 Eu1 O6 79.34(5) . . ? O1 Eu1 O6 148.08(6) . . ? O7 Eu1 O4 144.01(5) . . ? O5 Eu1 O4 76.55(6) . . ? O8 Eu1 O4 144.25(5) . . ? O1 Eu1 O4 91.15(6) . . ? O6 Eu1 O4 94.66(6) . . ? O7 Eu1 O3 76.43(5) . . ? O5 Eu1 O3 71.77(6) . . ? O8 Eu1 O3 133.31(5) . . ? O1 Eu1 O3 69.82(6) . . ? O6 Eu1 O3 141.27(5) . . ? O4 Eu1 O3 70.22(5) . . ? O7 Eu1 O2 142.82(5) . . ? O5 Eu1 O2 134.43(6) . . ? O8 Eu1 O2 74.78(5) . . ? O1 Eu1 O2 69.62(5) . . ? O6 Eu1 O2 83.13(5) . . ? O4 Eu1 O2 69.50(5) . . ? O3 Eu1 O2 120.86(5) . . ? C2 O1 Eu1 127.76(15) . . ? C4 O2 Eu1 128.42(14) . . ? C8 O3 Eu1 135.52(15) . . ? C10 O4 Eu1 134.26(15) . . ? C14 O5 Eu1 139.74(15) . . ? C16 O6 Eu1 139.20(15) . . ? C20 O7 Eu1 136.69(14) . . ? C22 O8 Eu1 135.67(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.0(2) . . ? O1 C2 C1 117.2(2) . . ? C3 C2 C1 119.8(2) . . ? C2 C3 C6 117.4(2) . . ? C2 C3 C4 123.4(2) . . ? C6 C3 C4 119.1(2) . . ? O2 C4 C3 123.3(2) . . ? O2 C4 C5 117.5(2) . . ? C3 C4 C5 119.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.1(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 123.2(2) . . ? O3 C8 C7 117.7(2) . . ? C9 C8 C7 119.1(2) . . ? C12 C9 C10 117.4(2) . . ? C12 C9 C8 118.5(2) . . ? C10 C9 C8 124.1(2) . . ? O4 C10 C9 122.8(2) . . ? O4 C10 C11 117.7(2) . . ? C9 C10 C11 119.5(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.5(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.5(2) . . ? O5 C14 C13 117.7(2) . . ? C15 C14 C13 119.8(2) . . ? C18 C15 C16 119.4(2) . . ? C18 C15 C14 117.1(2) . . ? C16 C15 C14 123.4(2) . . ? O6 C16 C15 123.3(2) . . ? O6 C16 C17 118.4(2) . . ? C15 C16 C17 118.32(19) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 177.8(3) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 C21 122.7(2) . . ? O7 C20 C19 118.03(19) . . ? C21 C20 C19 119.2(2) . . ? C24 C21 C20 118.6(2) . . ? C24 C21 C22 116.92(19) . . ? C20 C21 C22 124.1(2) . . ? O8 C22 C21 122.3(2) . . ? O8 C22 C23 118.4(2) . . ? C21 C22 C23 119.2(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C21 177.8(2) . . ? C12 N2 Ag1 160.4(2) . 3_776 ? C18 N3 Ag1 133.01(19) . . ? C24 N4 Ag1 116.09(16) . 2_645 ? C24 N4 Ag1 133.95(17) . 4_476 ? Ag1 N4 Ag1 95.73(7) 2_645 4_476 ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.160 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.117 data_6d _database_code_depnum_ccdc_archive 'CCDC 845903' #TrackingRef '- complete_incl_ins.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 6d _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Ag N4 O8 Yb' _chemical_formula_sum 'C24 H24 Ag N4 O8 Yb' _chemical_formula_weight 777.38 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.8841(5) _cell_length_b 21.0206(13) _cell_length_c 15.8536(10) _cell_angle_alpha 90.00 _cell_angle_beta 89.7194(8) _cell_angle_gamma 90.00 _cell_volume 2627.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6931 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 4.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3466 _exptl_absorpt_correction_T_max 0.5259 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38991 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 30.68 _reflns_number_total 7741 _reflns_number_gt 7195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0212P)^2^+2.6470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7741 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.485637(10) 0.188770(4) 0.500649(5) 0.00785(3) Uani 1 1 d . . . Ag1 Ag 0.04253(2) 0.001531(7) 0.889019(11) 0.01324(4) Uani 1 1 d . . . O1 O 0.5915(2) 0.21185(7) 0.36915(9) 0.0140(3) Uani 1 1 d . . . O2 O 0.70743(19) 0.11685(7) 0.47013(9) 0.0127(3) Uani 1 1 d . . . O3 O 0.37703(19) 0.09225(7) 0.45827(10) 0.0133(3) Uani 1 1 d . . . O4 O 0.2631(2) 0.20904(7) 0.40652(10) 0.0134(3) Uani 1 1 d . . . O5 O 0.2335(2) 0.18077(8) 0.57206(10) 0.0145(3) Uani 1 1 d . . . O6 O 0.54442(19) 0.15372(7) 0.63475(9) 0.0116(3) Uani 1 1 d . . . O7 O 0.42081(19) 0.29352(7) 0.52069(10) 0.0123(3) Uani 1 1 d . . . O8 O 0.73398(19) 0.24069(7) 0.53042(10) 0.0124(3) Uani 1 1 d . . . C1 C 0.5889(4) 0.19821(12) 0.22161(15) 0.0262(6) Uani 1 1 d . . . H1A H 0.4673 0.2052 0.2130 0.039 Uiso 1 1 calc R . . H1B H 0.6307 0.1669 0.1806 0.039 Uiso 1 1 calc R . . H1C H 0.6498 0.2384 0.2139 0.039 Uiso 1 1 calc R . . C2 C 0.6180(3) 0.17372(11) 0.30982(14) 0.0134(4) Uani 1 1 d . . . C3 C 0.6781(3) 0.11047(10) 0.32240(13) 0.0126(4) Uani 1 1 d . . . C4 C 0.7335(3) 0.08760(10) 0.40289(13) 0.0117(4) Uani 1 1 d . . . C5 C 0.8285(3) 0.02541(11) 0.40725(15) 0.0186(5) Uani 1 1 d . . . H5A H 0.9236 0.0296 0.4464 0.028 Uiso 1 1 calc R . . H5B H 0.8717 0.0144 0.3510 0.028 Uiso 1 1 calc R . . H5C H 0.7518 -0.0082 0.4271 0.028 Uiso 1 1 calc R . . C6 C 0.6845(3) 0.06932(11) 0.25106(14) 0.0163(4) Uani 1 1 d . . . C7 C 0.3293(3) 0.00228(10) 0.37176(17) 0.0193(5) Uani 1 1 d . . . H7A H 0.3887 -0.0190 0.4180 0.029 Uiso 1 1 calc R . . H7B H 0.3943 -0.0030 0.3194 0.029 Uiso 1 1 calc R . . H7C H 0.2165 -0.0166 0.3651 0.029 Uiso 1 1 calc R . . C8 C 0.3115(3) 0.07214(10) 0.39145(14) 0.0131(4) Uani 1 1 d . . . C9 C 0.2223(3) 0.11233(11) 0.33439(14) 0.0144(4) Uani 1 1 d . . . C10 C 0.1933(3) 0.17892(11) 0.34926(14) 0.0138(4) Uani 1 1 d . . . C11 C 0.0731(3) 0.21448(12) 0.29242(16) 0.0232(5) Uani 1 1 d . . . H11A H 0.0481 0.2563 0.3169 0.035 Uiso 1 1 calc R . . H11B H -0.0324 0.1902 0.2867 0.035 Uiso 1 1 calc R . . H11C H 0.1256 0.2200 0.2367 0.035 Uiso 1 1 calc R . . C12 C 0.1558(3) 0.08415(11) 0.26017(15) 0.0180(5) Uani 1 1 d . . . C13 C -0.0116(3) 0.14713(12) 0.64519(15) 0.0174(4) Uani 1 1 d . . . H13A H -0.0609 0.1832 0.6757 0.026 Uiso 1 1 calc R . . H13B H -0.0357 0.1077 0.6760 0.026 Uiso 1 1 calc R . . H13C H -0.0610 0.1447 0.5887 0.026 Uiso 1 1 calc R . . C14 C 0.1765(3) 0.15593(10) 0.63781(13) 0.0114(4) Uani 1 1 d . . . C15 C 0.2844(3) 0.13669(10) 0.70575(13) 0.0114(4) Uani 1 1 d . . . C16 C 0.4650(3) 0.13893(9) 0.70093(13) 0.0107(4) Uani 1 1 d . . . C17 C 0.5654(3) 0.12346(12) 0.77886(13) 0.0168(4) Uani 1 1 d . . . H17A H 0.6845 0.1165 0.7634 0.025 Uiso 1 1 calc R . . H17B H 0.5196 0.0849 0.8051 0.025 Uiso 1 1 calc R . . H17C H 0.5575 0.1589 0.8188 0.025 Uiso 1 1 calc R . . C18 C 0.2044(3) 0.11534(11) 0.78084(14) 0.0144(4) Uani 1 1 d . . . C19 C 0.3970(3) 0.40615(11) 0.51688(15) 0.0169(4) Uani 1 1 d . . . H19A H 0.2758 0.3960 0.5197 0.025 Uiso 1 1 calc R . . H19B H 0.4202 0.4313 0.4661 0.025 Uiso 1 1 calc R . . H19C H 0.4291 0.4307 0.5669 0.025 Uiso 1 1 calc R . . C20 C 0.4985(2) 0.34539(11) 0.51377(13) 0.0104(4) Uani 1 1 d . . . C21 C 0.6787(3) 0.34917(10) 0.50575(13) 0.0099(4) Uani 1 1 d . . . C22 C 0.7888(3) 0.29577(10) 0.51823(13) 0.0102(4) Uani 1 1 d . . . C23 C 0.9774(3) 0.30650(11) 0.52036(16) 0.0170(4) Uani 1 1 d . . . H23A H 1.0357 0.2655 0.5245 0.025 Uiso 1 1 calc R . . H23B H 1.0060 0.3327 0.5694 0.025 Uiso 1 1 calc R . . H23C H 1.0134 0.3283 0.4686 0.025 Uiso 1 1 calc R . . C24 C 0.7566(3) 0.40927(10) 0.49555(13) 0.0107(4) Uani 1 1 d . . . N1 N 0.6827(3) 0.03635(10) 0.19300(13) 0.0236(5) Uani 1 1 d . . . N2 N 0.1051(3) 0.06104(11) 0.19958(14) 0.0255(5) Uani 1 1 d . . . N3 N 0.1334(3) 0.09884(10) 0.84040(12) 0.0181(4) Uani 1 1 d . . . N4 N 0.8260(2) 0.45731(9) 0.48743(12) 0.0145(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.00958(5) 0.00755(5) 0.00642(5) 0.00009(3) 0.00003(3) -0.00041(3) Ag1 0.01606(8) 0.01345(8) 0.01020(8) -0.00177(6) -0.00005(6) -0.00082(5) O1 0.0208(8) 0.0123(7) 0.0088(7) 0.0020(6) 0.0013(6) 0.0030(6) O2 0.0155(7) 0.0119(7) 0.0106(7) 0.0002(6) 0.0007(6) 0.0023(6) O3 0.0157(7) 0.0100(7) 0.0141(7) 0.0005(6) -0.0006(6) -0.0017(6) O4 0.0165(8) 0.0109(7) 0.0127(7) -0.0003(6) -0.0036(6) -0.0012(6) O5 0.0125(7) 0.0186(8) 0.0123(7) 0.0034(6) 0.0009(6) 0.0011(6) O6 0.0128(7) 0.0125(7) 0.0094(7) 0.0012(6) 0.0003(5) -0.0007(6) O7 0.0107(7) 0.0097(7) 0.0164(8) -0.0028(6) 0.0001(6) -0.0014(5) O8 0.0133(7) 0.0097(7) 0.0143(7) 0.0002(6) -0.0004(6) -0.0004(5) C1 0.0484(17) 0.0220(13) 0.0082(10) 0.0035(9) -0.0009(10) 0.0104(11) C2 0.0143(10) 0.0152(10) 0.0107(10) 0.0018(8) 0.0030(8) 0.0009(8) C3 0.0154(10) 0.0109(10) 0.0114(9) -0.0004(8) 0.0032(8) 0.0021(8) C4 0.0115(9) 0.0112(10) 0.0126(10) 0.0007(8) 0.0020(7) 0.0002(7) C5 0.0226(12) 0.0168(11) 0.0162(11) 0.0018(9) 0.0009(9) 0.0097(9) C6 0.0185(11) 0.0159(11) 0.0145(10) 0.0019(8) 0.0025(8) 0.0033(8) C7 0.0245(13) 0.0107(11) 0.0226(13) -0.0037(8) 0.0025(10) -0.0028(8) C8 0.0127(10) 0.0123(10) 0.0144(10) -0.0007(8) 0.0035(8) -0.0039(8) C9 0.0153(10) 0.0145(10) 0.0133(10) -0.0024(8) -0.0014(8) -0.0037(8) C10 0.0129(10) 0.0158(10) 0.0128(10) 0.0024(8) -0.0006(8) -0.0022(8) C11 0.0263(13) 0.0188(12) 0.0247(13) 0.0021(10) -0.0140(10) -0.0003(10) C12 0.0179(11) 0.0192(11) 0.0168(11) -0.0022(9) -0.0002(9) -0.0038(9) C13 0.0108(10) 0.0218(12) 0.0197(11) 0.0032(9) 0.0005(8) -0.0008(8) C14 0.0130(9) 0.0093(9) 0.0119(9) -0.0019(8) 0.0024(7) 0.0012(7) C15 0.0137(10) 0.0099(9) 0.0106(9) 0.0011(7) 0.0024(7) -0.0013(7) C16 0.0149(10) 0.0076(9) 0.0095(9) -0.0015(7) 0.0002(7) 0.0007(7) C17 0.0174(10) 0.0232(12) 0.0098(10) 0.0029(9) -0.0004(8) -0.0002(9) C18 0.0146(10) 0.0133(10) 0.0152(10) 0.0001(8) -0.0007(8) 0.0014(8) C19 0.0137(10) 0.0127(10) 0.0243(12) -0.0025(9) -0.0017(9) 0.0019(8) C20 0.0110(9) 0.0120(10) 0.0081(9) -0.0010(7) -0.0008(7) -0.0002(7) C21 0.0109(9) 0.0096(9) 0.0091(9) 0.0006(7) -0.0003(7) -0.0010(7) C22 0.0108(9) 0.0115(9) 0.0082(9) -0.0003(7) 0.0003(7) -0.0006(7) C23 0.0110(10) 0.0147(11) 0.0251(12) 0.0028(9) 0.0014(9) -0.0010(8) C24 0.0107(9) 0.0133(10) 0.0080(9) 0.0003(7) 0.0000(7) 0.0022(7) N1 0.0321(12) 0.0229(11) 0.0159(10) -0.0042(8) 0.0015(8) 0.0063(9) N2 0.0268(11) 0.0283(12) 0.0215(11) -0.0083(9) -0.0027(9) -0.0050(9) N3 0.0196(10) 0.0181(10) 0.0166(9) 0.0040(8) 0.0035(8) -0.0002(8) N4 0.0154(9) 0.0123(9) 0.0157(9) 0.0005(7) 0.0017(7) -0.0003(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 Yb1 O7 2.2823(15) . ? Yb1 O5 2.2888(15) . ? Yb1 O8 2.2928(15) . ? Yb1 O1 2.2936(15) . ? Yb1 O6 2.2994(15) . ? Yb1 O3 2.3036(15) . ? Yb1 O4 2.3476(15) . ? Yb1 O2 2.3599(15) . ? Ag1 N2 2.252(2) 3_556 ? Ag1 N3 2.299(2) . ? Ag1 N4 2.4075(19) 2_646 ? Ag1 N4 2.4642(19) 4_466 ? O1 C2 1.253(3) . ? O2 C4 1.247(3) . ? O3 C8 1.254(3) . ? O4 C10 1.238(3) . ? O5 C14 1.248(3) . ? O6 C16 1.258(2) . ? O7 C20 1.255(3) . ? O8 C22 1.250(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.426(3) . ? C3 C6 1.424(3) . ? C3 C4 1.434(3) . ? C4 C5 1.508(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.153(3) . ? C7 C8 1.508(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.426(3) . ? C9 C12 1.420(3) . ? C9 C10 1.438(3) . ? C10 C11 1.509(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.150(3) . ? C13 C14 1.498(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.434(3) . ? C15 C18 1.418(3) . ? C15 C16 1.426(3) . ? C16 C17 1.506(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.149(3) . ? C19 C20 1.508(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.428(3) . ? C21 C24 1.414(3) . ? C21 C22 1.433(3) . ? C22 C23 1.505(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N4 1.155(3) . ? N2 Ag1 2.252(2) 3_556 ? N4 Ag1 2.4074(19) 2_656 ? N4 Ag1 2.4642(19) 4_665 ? 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 Yb1 O5 78.97(5) . . ? O7 Yb1 O8 72.72(5) . . ? O5 Yb1 O8 132.34(6) . . ? O7 Yb1 O1 90.15(5) . . ? O5 Yb1 O1 140.93(6) . . ? O8 Yb1 O1 77.24(6) . . ? O7 Yb1 O6 103.09(5) . . ? O5 Yb1 O6 72.40(5) . . ? O8 Yb1 O6 77.65(5) . . ? O1 Yb1 O6 146.52(5) . . ? O7 Yb1 O3 143.80(5) . . ? O5 Yb1 O3 75.90(6) . . ? O8 Yb1 O3 142.97(5) . . ? O1 Yb1 O3 93.17(6) . . ? O6 Yb1 O3 93.69(5) . . ? O7 Yb1 O4 75.27(5) . . ? O5 Yb1 O4 71.21(5) . . ? O8 Yb1 O4 133.31(5) . . ? O1 Yb1 O4 69.73(6) . . ? O6 Yb1 O4 143.18(5) . . ? O3 Yb1 O4 72.21(5) . . ? O7 Yb1 O2 144.27(5) . . ? O5 Yb1 O2 134.04(5) . . ? O8 Yb1 O2 73.41(5) . . ? O1 Yb1 O2 71.53(5) . . ? O6 Yb1 O2 80.32(5) . . ? O3 Yb1 O2 69.64(5) . . ? O4 Yb1 O2 122.77(5) . . ? N2 Ag1 N3 118.13(8) 3_556 . ? N2 Ag1 N4 120.52(8) 3_556 2_646 ? N3 Ag1 N4 118.79(7) . 2_646 ? N2 Ag1 N4 103.97(7) 3_556 4_466 ? N3 Ag1 N4 96.53(7) . 4_466 ? N4 Ag1 N4 85.43(7) 2_646 4_466 ? C2 O1 Yb1 127.30(14) . . ? C4 O2 Yb1 127.58(14) . . ? C8 O3 Yb1 134.30(14) . . ? C10 O4 Yb1 135.20(15) . . ? C14 O5 Yb1 138.82(14) . . ? C16 O6 Yb1 138.45(14) . . ? C20 O7 Yb1 135.82(14) . . ? C22 O8 Yb1 134.73(14) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.1(2) . . ? O1 C2 C1 116.9(2) . . ? C3 C2 C1 120.0(2) . . ? C6 C3 C2 117.75(19) . . ? C6 C3 C4 119.56(19) . . ? C2 C3 C4 122.68(19) . . ? O2 C4 C3 123.10(19) . . ? O2 C4 C5 117.90(19) . . ? C3 C4 C5 119.00(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.3(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.9(2) . . ? O3 C8 C7 117.7(2) . . ? C9 C8 C7 119.4(2) . . ? C12 C9 C8 117.6(2) . . ? C12 C9 C10 118.9(2) . . ? C8 C9 C10 123.4(2) . . ? O4 C10 C9 123.2(2) . . ? O4 C10 C11 117.9(2) . . ? C9 C10 C11 119.0(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.7(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.18(19) . . ? O5 C14 C13 118.00(19) . . ? C15 C14 C13 119.81(19) . . ? C18 C15 C16 119.72(19) . . ? C18 C15 C14 117.16(19) . . ? C16 C15 C14 123.11(19) . . ? O6 C16 C15 123.06(19) . . ? O6 C16 C17 118.41(19) . . ? C15 C16 C17 118.52(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 177.3(2) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O7 C20 C21 122.7(2) . . ? O7 C20 C19 118.33(18) . . ? C21 C20 C19 118.90(19) . . ? C24 C21 C20 119.43(19) . . ? C24 C21 C22 116.92(18) . . ? C20 C21 C22 123.16(19) . . ? O8 C22 C21 122.51(19) . . ? O8 C22 C23 118.44(19) . . ? C21 C22 C23 119.00(19) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C21 177.5(2) . . ? C12 N2 Ag1 161.9(2) . 3_556 ? C18 N3 Ag1 133.94(18) . . ? C24 N4 Ag1 116.90(16) . 2_656 ? C24 N4 Ag1 134.72(16) . 4_665 ? Ag1 N4 Ag1 94.57(7) 2_656 4_665 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.060 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.120