Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Rongbin Huang Department of Chemistry Xiamen University Xiamen, 361005 P. R. China ; _publ_contact_author_phone 86-592-2185191 _publ_contact_author_fax 86-592-2183047 _publ_contact_author_email rbhuang@xmu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, Crystal structure and Optical properties of [AgU3O6(OAc)6] [Zn(H2O)4(CH3CH2OH)2]: A Novel Compound Containing Closed-shell 3d10, 4d10 and 5d10 Metal Ions Simultaneously ; loop_ _publ_author_name _publ_author_address 'Geng-Geng Luo' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Li-Rong Lin' ; Department of chemistry, Xiamen University, Xiamen 361005, People's Republic of China ; 'Lan-Sun Zheng' ; State key Laboratory for Physical Chemistry of Solid Surfaces, Xiamen University, Xiamen 361005, People's Republic of China ; _publ_section_exptl_refinement ; All H atoms were placed geometrically with C-H distances of 0.93\%A, N-H distances of 0.86\%A and refined using a riding atom model with their isotropic displacement factors, J~iso~ fixed at 1.2 time the U~eq~ of the parent C and N atom. ; _publ_contact_author_name 'Rongbin Huang' data_p _database_code_depnum_ccdc_archive 'CCDC 648777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ag U3 O6 (OAc)9 Zn (H2O)4 (CH3CH2OH)2 ' _chemical_formula_sum 'C22 H47 Ag O30 U3 Zn' _chemical_formula_weight 1678.93 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' U U -9.6767 9.6646 '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 22.909(7) _cell_length_b 13.973(4) _cell_length_c 16.233(5) _cell_angle_alpha 90.00 _cell_angle_beta 119.901(5) _cell_angle_gamma 90.00 _cell_volume 4505(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3566 _cell_measurement_theta_min 2.582 _cell_measurement_theta_max 24.679 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 11.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2014 _exptl_absorpt_correction_T_max 0.2708 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11699 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4343 _reflns_number_gt 3288 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4343 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 Zn1 Zn 0.2500 0.7500 0.0000 0.0291(4) Uani 1 2 d S . . Ag1 Ag 0.5000 0.25078(8) 0.2500 0.0426(4) Uani 1 2 d S . . U1 U 0.5000 0.54062(4) 0.2500 0.03601(19) Uani 1 2 d S . . U2 U 0.64703(2) 0.08460(3) 0.25406(3) 0.03285(15) Uani 1 1 d . . . C1 C 0.7490(6) -0.0313(8) 0.2587(9) 0.036(3) Uani 1 1 d . . . C2 C 0.8052(8) -0.0886(11) 0.2636(15) 0.080(6) Uani 1 1 d . . . H2A H 0.8036 -0.1523 0.2844 0.120 Uiso 1 1 calc R . . H2B H 0.8473 -0.0593 0.3077 0.120 Uiso 1 1 calc R . . H2C H 0.8011 -0.0910 0.2018 0.120 Uiso 1 1 calc R . . C3 C 0.6122(6) 0.0746(9) 0.3987(9) 0.040(3) Uani 1 1 d . . . C4 C 0.5910(8) 0.0685(11) 0.4704(12) 0.070(5) Uani 1 1 d . . . H4A H 0.6221 0.0289 0.5222 0.105 Uiso 1 1 calc R . . H4B H 0.5467 0.0411 0.4423 0.105 Uiso 1 1 calc R . . H4C H 0.5904 0.1314 0.4937 0.105 Uiso 1 1 calc R . . C5 C 0.5770(6) 0.2185(9) 0.1047(9) 0.046(3) Uani 1 1 d . . . C6 C 0.5430(8) 0.2905(12) 0.0313(13) 0.079(5) Uani 1 1 d . . . H6A H 0.5065 0.2613 -0.0239 0.119 Uiso 1 1 calc R . . H6B H 0.5743 0.3177 0.0148 0.119 Uiso 1 1 calc R . . H6C H 0.5258 0.3399 0.0544 0.119 Uiso 1 1 calc R . . C7 C 0.6133(6) 0.4351(10) 0.3852(10) 0.050(3) Uani 1 1 d . . . C8 C 0.6706(8) 0.3817(11) 0.4569(12) 0.076(5) Uani 1 1 d . . . H8A H 0.6761 0.3949 0.5185 0.114 Uiso 1 1 calc R . . H8B H 0.7105 0.4005 0.4559 0.114 Uiso 1 1 calc R . . H8C H 0.6630 0.3145 0.4438 0.114 Uiso 1 1 calc R . . C9 C 0.5000 0.7429(12) 0.2500 0.043(4) Uani 1 2 d S . . C10 C 0.5000 0.8509(13) 0.2500 0.067(6) Uani 1 2 d S . . H10A H 0.4739 0.8738 0.1859 0.101 Uiso 0.50 1 calc PR . . H10B H 0.5454 0.8738 0.2772 0.101 Uiso 0.50 1 calc PR . . H10C H 0.4807 0.8738 0.2869 0.101 Uiso 0.50 1 calc PR . . C11 C 0.3104(7) 0.7071(10) 0.2173(10) 0.056(4) Uani 1 1 d . . . H11A H 0.3134 0.6381 0.2144 0.067 Uiso 1 1 calc R . . H11B H 0.2652 0.7222 0.2043 0.067 Uiso 1 1 calc R . . C12 C 0.3584(8) 0.7387(13) 0.3135(10) 0.069(5) Uani 1 1 d . . . H12A H 0.3495 0.7062 0.3581 0.104 Uiso 1 1 calc R . . H12B H 0.3540 0.8065 0.3184 0.104 Uiso 1 1 calc R . . H12C H 0.4033 0.7243 0.3272 0.104 Uiso 1 1 calc R . . O1 O 0.5856(4) -0.0003(6) 0.1904(7) 0.050(2) Uani 1 1 d . . . O2 O 0.7078(4) 0.1713(6) 0.3176(6) 0.048(2) Uani 1 1 d . . . O3 O 0.5881(5) 0.1348(6) 0.3343(8) 0.059(3) Uani 1 1 d . . . O4 O 0.6552(4) 0.0185(6) 0.4008(6) 0.045(2) Uani 1 1 d . . . O5 O 0.7368(4) -0.0342(5) 0.3245(6) 0.045(2) Uani 1 1 d . . . O6 O 0.7120(4) 0.0204(6) 0.1862(7) 0.049(2) Uani 1 1 d . . . O7 O 0.6226(4) 0.1654(6) 0.1070(6) 0.048(2) Uani 1 1 d . . . O8 O 0.5645(4) 0.2093(6) 0.1693(7) 0.052(2) Uani 1 1 d . . . O9 O 0.6149(4) 0.5247(6) 0.3869(7) 0.055(2) Uani 1 1 d . . . O10 O 0.5619(4) 0.3951(6) 0.3240(8) 0.058(3) Uani 1 1 d . . . O11 O 0.4691(4) 0.5411(6) 0.3280(7) 0.058(3) Uani 1 1 d . . . O12 O 0.5517(4) 0.6986(6) 0.3060(6) 0.044(2) Uani 1 1 d . . . O13 O 0.3197(4) 0.7476(6) 0.1464(6) 0.0392(19) Uani 1 1 d . . . H13B H 0.3530 0.7238 0.1479 0.059 Uiso 1 1 calc R . . O1W O 0.3134(4) 0.8508(6) -0.0039(6) 0.048(2) Uani 1 1 d . . . H1WA H 0.3451 0.8594 0.0499 0.072 Uiso 1 1 calc R . . H1WB H 0.3275 0.8326 -0.0388 0.072 Uiso 1 1 d R . . O2W O 0.1975(4) 0.8531(5) 0.0260(6) 0.0393(19) Uani 1 1 d . . . H2WD H 0.1952 0.9017 -0.0037 0.059 Uiso 1 1 calc R . . H2WA H 0.2168 0.8650 0.0830 0.059 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0313(10) 0.0253(9) 0.0260(10) -0.0001(7) 0.0105(8) 0.0001(7) Ag1 0.0393(8) 0.0253(6) 0.0603(10) 0.000 0.0226(7) 0.000 U1 0.0314(3) 0.0250(3) 0.0368(4) 0.000 0.0059(3) 0.000 U2 0.0362(3) 0.0301(2) 0.0314(3) 0.00752(19) 0.0162(2) 0.00418(17) C1 0.041(7) 0.033(6) 0.036(7) 0.006(6) 0.023(6) -0.002(5) C2 0.083(12) 0.070(10) 0.124(18) 0.014(11) 0.080(14) 0.024(9) C3 0.050(7) 0.046(7) 0.030(7) 0.015(6) 0.025(6) 0.018(6) C4 0.084(11) 0.083(11) 0.060(11) 0.035(9) 0.050(10) 0.034(9) C5 0.042(8) 0.056(8) 0.031(7) 0.017(6) 0.011(6) 0.002(6) C6 0.071(11) 0.082(11) 0.085(14) 0.039(11) 0.039(11) 0.013(9) C7 0.032(7) 0.051(8) 0.040(8) 0.007(7) -0.002(6) -0.002(6) C8 0.069(11) 0.056(9) 0.056(10) 0.015(8) -0.004(8) 0.021(8) C9 0.041(11) 0.032(9) 0.059(13) 0.000 0.027(11) 0.000 C10 0.072(15) 0.035(11) 0.076(17) 0.000 0.023(13) 0.000 C11 0.052(9) 0.065(9) 0.050(9) 0.010(8) 0.025(8) -0.021(7) C12 0.063(10) 0.110(13) 0.019(7) 0.006(8) 0.009(7) 0.007(9) O1 0.045(5) 0.051(5) 0.050(6) 0.016(5) 0.020(5) -0.001(4) O2 0.045(5) 0.042(5) 0.040(5) 0.008(4) 0.009(4) -0.002(4) O3 0.073(7) 0.049(5) 0.066(7) 0.023(5) 0.043(6) 0.033(5) O4 0.056(5) 0.046(5) 0.043(5) 0.018(4) 0.031(5) 0.017(4) O5 0.053(5) 0.039(5) 0.039(5) 0.020(4) 0.020(5) 0.026(4) O6 0.056(6) 0.049(5) 0.040(6) -0.006(5) 0.022(5) -0.008(4) O7 0.057(6) 0.061(5) 0.034(5) 0.020(4) 0.029(5) 0.013(4) O8 0.055(6) 0.061(6) 0.046(6) 0.025(5) 0.031(5) 0.028(5) O9 0.043(5) 0.028(5) 0.048(6) 0.000(4) -0.013(4) -0.005(4) O10 0.042(5) 0.031(5) 0.067(7) 0.002(4) 0.001(5) 0.005(4) O11 0.053(6) 0.053(6) 0.059(7) 0.011(5) 0.022(5) 0.001(5) O12 0.027(4) 0.039(5) 0.050(6) -0.005(4) 0.007(4) -0.005(4) O13 0.028(4) 0.054(5) 0.028(5) 0.011(4) 0.008(4) 0.003(3) O1W 0.058(6) 0.049(5) 0.040(5) -0.019(4) 0.027(5) -0.021(4) O2W 0.048(5) 0.030(4) 0.029(5) 0.002(4) 0.012(4) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1W 2.047(7) 7_565 ? Zn1 O1W 2.047(7) . ? Zn1 O2W 2.051(7) . ? Zn1 O2W 2.051(7) 7_565 ? Zn1 O13 2.101(8) 7_565 ? Zn1 O13 2.101(8) . ? Ag1 O3 2.412(9) 2_655 ? Ag1 O3 2.412(9) . ? Ag1 O10 2.414(9) . ? Ag1 O10 2.414(9) 2_655 ? Ag1 O8 2.483(8) . ? Ag1 O8 2.483(8) 2_655 ? U1 O11 1.732(9) . ? U1 O11 1.732(9) 2_655 ? U1 O10 2.427(8) 2_655 ? U1 O10 2.427(8) . ? U1 O12 2.455(8) . ? U1 O12 2.455(8) 2_655 ? U1 O9 2.467(8) 2_655 ? U1 O9 2.467(8) . ? U1 C9 2.826(16) . ? U1 C7 2.838(13) 2_655 ? U1 C7 2.838(13) . ? U2 O1 1.734(9) . ? U2 O2 1.743(8) . ? U2 O3 2.402(8) . ? U2 O6 2.423(8) . ? U2 O8 2.432(8) . ? U2 O5 2.439(7) . ? U2 O7 2.440(8) . ? U2 O4 2.473(8) . ? U2 C1 2.812(11) . ? U2 C3 2.835(11) . ? U2 C5 2.841(12) . ? C1 O5 1.231(13) . ? C1 O6 1.277(14) . ? C1 C2 1.485(16) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O3 1.236(14) . ? C3 O4 1.246(12) . ? C3 C4 1.470(16) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O8 1.224(13) . ? C5 O7 1.267(14) . ? C5 C6 1.454(19) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O10 1.232(15) . ? C7 O9 1.253(15) . ? C7 C8 1.452(18) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O12 1.241(11) 2_655 ? C9 O12 1.241(11) . ? C9 C10 1.51(2) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O13 1.392(14) . ? C11 C12 1.46(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O13 H13B 0.8200 . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8199 . ? O2W H2WD 0.8200 . ? O2W H2WA 0.8201 . ? 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 O1W Zn1 O1W 180.000(1) 7_565 . ? O1W Zn1 O2W 88.8(3) 7_565 . ? O1W Zn1 O2W 91.2(3) . . ? O1W Zn1 O2W 91.2(3) 7_565 7_565 ? O1W Zn1 O2W 88.8(3) . 7_565 ? O2W Zn1 O2W 180.0(5) . 7_565 ? O1W Zn1 O13 84.0(3) 7_565 7_565 ? O1W Zn1 O13 96.0(3) . 7_565 ? O2W Zn1 O13 91.6(3) . 7_565 ? O2W Zn1 O13 88.4(3) 7_565 7_565 ? O1W Zn1 O13 96.0(3) 7_565 . ? O1W Zn1 O13 84.0(3) . . ? O2W Zn1 O13 88.4(3) . . ? O2W Zn1 O13 91.6(3) 7_565 . ? O13 Zn1 O13 180.0(4) 7_565 . ? O3 Ag1 O3 95.6(5) 2_655 . ? O3 Ag1 O10 164.1(3) 2_655 . ? O3 Ag1 O10 99.3(3) . . ? O3 Ag1 O10 99.3(3) 2_655 2_655 ? O3 Ag1 O10 164.1(3) . 2_655 ? O10 Ag1 O10 66.6(4) . 2_655 ? O3 Ag1 O8 95.4(3) 2_655 . ? O3 Ag1 O8 66.0(3) . . ? O10 Ag1 O8 95.8(3) . . ? O10 Ag1 O8 106.8(3) 2_655 . ? O3 Ag1 O8 66.0(3) 2_655 2_655 ? O3 Ag1 O8 95.4(3) . 2_655 ? O10 Ag1 O8 106.8(3) . 2_655 ? O10 Ag1 O8 95.8(3) 2_655 2_655 ? O8 Ag1 O8 153.0(4) . 2_655 ? O11 U1 O11 179.5(6) . 2_655 ? O11 U1 O10 90.8(4) . 2_655 ? O11 U1 O10 89.6(4) 2_655 2_655 ? O11 U1 O10 89.6(4) . . ? O11 U1 O10 90.8(4) 2_655 . ? O10 U1 O10 66.2(4) 2_655 . ? O11 U1 O12 91.3(4) . . ? O11 U1 O12 88.2(4) 2_655 . ? O10 U1 O12 172.5(3) 2_655 . ? O10 U1 O12 121.0(3) . . ? O11 U1 O12 88.2(3) . 2_655 ? O11 U1 O12 91.3(4) 2_655 2_655 ? O10 U1 O12 121.0(3) 2_655 2_655 ? O10 U1 O12 172.5(3) . 2_655 ? O12 U1 O12 51.9(4) . 2_655 ? O11 U1 O9 91.0(4) . 2_655 ? O11 U1 O9 89.1(4) 2_655 2_655 ? O10 U1 O9 51.7(3) 2_655 2_655 ? O10 U1 O9 117.9(3) . 2_655 ? O12 U1 O9 121.0(3) . 2_655 ? O12 U1 O9 69.3(3) 2_655 2_655 ? O11 U1 O9 89.1(4) . . ? O11 U1 O9 91.0(4) 2_655 . ? O10 U1 O9 117.9(3) 2_655 . ? O10 U1 O9 51.7(3) . . ? O12 U1 O9 69.3(3) . . ? O12 U1 O9 121.0(3) 2_655 . ? O9 U1 O9 169.7(4) 2_655 . ? O11 U1 C9 89.8(3) . . ? O11 U1 C9 89.8(3) 2_655 . ? O10 U1 C9 146.9(2) 2_655 . ? O10 U1 C9 146.9(2) . . ? O12 U1 C9 25.97(19) . . ? O12 U1 C9 25.97(19) 2_655 . ? O9 U1 C9 95.17(18) 2_655 . ? O9 U1 C9 95.17(18) . . ? O11 U1 C7 91.0(4) . 2_655 ? O11 U1 C7 89.2(4) 2_655 2_655 ? O10 U1 C7 25.6(3) 2_655 2_655 ? O10 U1 C7 91.8(4) . 2_655 ? O12 U1 C7 147.2(3) . 2_655 ? O12 U1 C7 95.4(3) 2_655 2_655 ? O9 U1 C7 26.1(3) 2_655 2_655 ? O9 U1 C7 143.5(3) . 2_655 ? C9 U1 C7 121.3(3) . 2_655 ? O11 U1 C7 89.2(4) . . ? O11 U1 C7 91.0(4) 2_655 . ? O10 U1 C7 91.8(4) 2_655 . ? O10 U1 C7 25.6(3) . . ? O12 U1 C7 95.4(3) . . ? O12 U1 C7 147.2(3) 2_655 . ? O9 U1 C7 143.5(3) 2_655 . ? O9 U1 C7 26.1(3) . . ? C9 U1 C7 121.3(3) . . ? C7 U1 C7 117.4(6) 2_655 . ? O1 U2 O2 179.1(4) . . ? O1 U2 O3 90.8(4) . . ? O2 U2 O3 88.6(4) . . ? O1 U2 O6 88.6(3) . . ? O2 U2 O6 92.0(3) . . ? O3 U2 O6 173.7(3) . . ? O1 U2 O8 89.0(4) . . ? O2 U2 O8 90.2(4) . . ? O3 U2 O8 67.0(3) . . ? O6 U2 O8 119.3(3) . . ? O1 U2 O5 93.4(4) . . ? O2 U2 O5 87.5(3) . . ? O3 U2 O5 121.0(3) . . ? O6 U2 O5 52.8(3) . . ? O8 U2 O5 171.6(3) . . ? O1 U2 O7 90.6(4) . . ? O2 U2 O7 89.0(4) . . ? O3 U2 O7 118.6(3) . . ? O6 U2 O7 67.6(3) . . ? O8 U2 O7 51.7(3) . . ? O5 U2 O7 120.1(3) . . ? O1 U2 O4 88.1(4) . . ? O2 U2 O4 92.0(4) . . ? O3 U2 O4 51.6(3) . . ? O6 U2 O4 122.1(3) . . ? O8 U2 O4 118.5(3) . . ? O5 U2 O4 69.7(3) . . ? O7 U2 O4 170.1(3) . . ? O1 U2 C1 92.2(4) . . ? O2 U2 C1 88.6(4) . . ? O3 U2 C1 146.9(3) . . ? O6 U2 C1 26.9(3) . . ? O8 U2 C1 146.0(3) . . ? O5 U2 C1 25.9(3) . . ? O7 U2 C1 94.3(3) . . ? O4 U2 C1 95.5(3) . . ? O1 U2 C3 88.8(4) . . ? O2 U2 C3 91.0(4) . . ? O3 U2 C3 25.6(3) . . ? O6 U2 C3 148.1(3) . . ? O8 U2 C3 92.5(3) . . ? O5 U2 C3 95.6(3) . . ? O7 U2 C3 144.2(3) . . ? O4 U2 C3 26.0(3) . . ? C1 U2 C3 121.5(3) . . ? O1 U2 C5 89.8(4) . . ? O2 U2 C5 89.5(4) . . ? O3 U2 C5 92.3(3) . . ? O6 U2 C5 94.0(3) . . ? O8 U2 C5 25.3(3) . . ? O5 U2 C5 146.5(3) . . ? O7 U2 C5 26.4(3) . . ? O4 U2 C5 143.8(3) . . ? C1 U2 C5 120.7(4) . . ? C3 U2 C5 117.8(4) . . ? O5 C1 O6 119.0(10) . . ? O5 C1 C2 120.1(12) . . ? O6 C1 C2 120.8(12) . . ? O5 C1 U2 59.9(6) . . ? O6 C1 U2 59.3(6) . . ? C2 C1 U2 177.1(10) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 O4 117.7(10) . . ? O3 C3 C4 121.6(10) . . ? O4 C3 C4 120.7(11) . . ? O3 C3 U2 57.2(6) . . ? O4 C3 U2 60.5(6) . . ? C4 C3 U2 177.5(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O8 C5 O7 117.2(11) . . ? O8 C5 C6 121.1(12) . . ? O7 C5 C6 121.7(12) . . ? O8 C5 U2 58.3(6) . . ? O7 C5 U2 58.9(6) . . ? C6 C5 U2 177.4(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O10 C7 O9 118.4(12) . . ? O10 C7 C8 122.1(13) . . ? O9 C7 C8 119.4(12) . . ? O10 C7 U1 58.2(6) . . ? O9 C7 U1 60.2(6) . . ? C8 C7 U1 178.0(11) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O12 C9 O12 120.1(15) 2_655 . ? O12 C9 C10 119.9(7) 2_655 . ? O12 C9 C10 119.9(7) . . ? O12 C9 U1 60.1(7) 2_655 . ? O12 C9 U1 60.1(7) . . ? C10 C9 U1 180.000(3) . . ? 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 . . ? O13 C11 C12 114.7(11) . . ? O13 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? O13 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 O3 U2 97.2(7) . . ? C3 O3 Ag1 146.2(8) . . ? U2 O3 Ag1 115.2(4) . . ? C3 O4 U2 93.4(7) . . ? C1 O5 U2 94.2(7) . . ? C1 O6 U2 93.8(7) . . ? C5 O7 U2 94.7(7) . . ? C5 O8 U2 96.4(7) . . ? C5 O8 Ag1 152.0(8) . . ? U2 O8 Ag1 111.6(3) . . ? C7 O9 U1 93.7(7) . . ? C7 O10 Ag1 150.2(9) . . ? C7 O10 U1 96.2(8) . . ? Ag1 O10 U1 113.6(4) . . ? C9 O12 U1 94.0(8) . . ? C11 O13 Zn1 126.7(7) . . ? C11 O13 H13B 109.5 . . ? Zn1 O13 H13B 102.2 . . ? Zn1 O1W H1WA 109.5 . . ? Zn1 O1W H1WB 109.7 . . ? H1WA O1W H1WB 109.7 . . ? Zn1 O2W H2WD 109.5 . . ? Zn1 O2W H2WA 109.4 . . ? H2WD O2W H2WA 109.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13B O12 0.82 1.96 2.733(10) 158.1 2_655 O1W H1WA O4 0.82 2.36 2.759(11) 110.4 2_665 O1W H1WB O7 0.82 1.95 2.728(10) 158.8 5_665 O2W H2WD O9 0.82 2.08 2.708(11) 132.9 8_465 O2W H2WA O5 0.82 1.94 2.645(11) 143.0 2_665 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.339 _refine_diff_density_min -1.683 _refine_diff_density_rms 0.266