Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chaudhuri, Nirmalendu Ray' 'Konar, Sanjit' 'Lu, Tian-Huey' 'Maji, Tapas Kumar' 'Mostafa, Golam' 'Zangrando, Ennio' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; Self-assembly of new thre-dimensional molecular architectures of Cd(II) and Ag(I) using croconate as a building block ; data_complex1 _database_code_CSD 183156 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H6 Cd N2 O5' _chemical_formula_sum 'C5 H6 Cd N2 O5' _chemical_formula_weight 286.53 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' 'Cd' 'Cd' -0.8075 1.2024 '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 n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.668(3) _cell_length_b 7.668(3) _cell_length_c 13.882(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 816.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Thin rod' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.667 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6867 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4551 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1012 _reflns_number_gt 755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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. The maximum difference peaks are within 1A from Cadmium atom and arise due to series termination error; ; _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^)+(0.0790P)^2^+4.6572P] 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 1012 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.009 _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 Cd Cd 0.99358(9) 0.2500 0.32343(6) 0.0337(3) Uani 1 2 d S . . O1 O 0.6757(10) 0.2500 0.3168(5) 0.0362(18) Uani 1 2 d S . . O2 O 0.8802(9) 0.2500 0.4891(5) 0.0351(17) Uani 1 2 d S . . O3 O 0.6429(12) 0.2500 0.6569(5) 0.050(2) Uani 1 2 d S . . O4 O 0.2876(11) 0.2500 0.5834(8) 0.068(3) Uani 1 2 d S . . O5 O 0.3099(10) 0.2500 0.3675(7) 0.057(2) Uani 1 2 d S . . C1 C 0.6124(12) 0.2500 0.4017(7) 0.026(2) Uani 1 2 d S . . C2 C 0.7157(12) 0.2500 0.4878(7) 0.027(2) Uani 1 2 d S . . C3 C 0.6003(12) 0.2500 0.5720(7) 0.028(2) Uani 1 2 d S . . C4 C 0.4164(13) 0.2500 0.5319(9) 0.042(3) Uani 1 2 d S . . C5 C 0.4294(14) 0.2500 0.4295(9) 0.039(3) Uani 1 2 d S . . N N 1.0026(7) -0.0343(11) 0.3244(5) 0.0381(16) Uani 1 1 d . . . H0A H 0.9876 -0.0742 0.2647 0.057 Uiso 1 1 calc R . . H0B H 0.9182 -0.0753 0.3621 0.057 Uiso 1 1 calc R . . H0C H 1.1055 -0.0696 0.3466 0.057 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 Cd 0.0366(5) 0.0289(5) 0.0356(5) 0.000 0.0130(3) 0.000 O1 0.038(4) 0.050(5) 0.021(3) 0.000 0.004(3) 0.000 O2 0.019(3) 0.059(5) 0.028(4) 0.000 -0.001(3) 0.000 O3 0.056(5) 0.078(7) 0.017(3) 0.000 0.004(3) 0.000 O4 0.034(4) 0.094(8) 0.076(7) 0.000 0.024(5) 0.000 O5 0.031(4) 0.076(7) 0.065(6) 0.000 -0.021(5) 0.000 C1 0.019(4) 0.028(5) 0.031(5) 0.000 -0.005(4) 0.000 C2 0.026(5) 0.029(5) 0.025(5) 0.000 -0.006(4) 0.000 C3 0.021(4) 0.031(5) 0.033(5) 0.000 0.001(4) 0.000 C4 0.021(5) 0.047(7) 0.056(7) 0.000 0.013(5) 0.000 C5 0.027(5) 0.039(6) 0.050(7) 0.000 -0.017(5) 0.000 N 0.037(4) 0.038(4) 0.039(4) 0.003(3) -0.004(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N 2.181(9) 7_565 ? Cd N 2.181(9) . ? Cd O1 2.396(7) 6_656 ? Cd O1 2.439(8) . ? Cd O2 2.459(7) . ? Cd O5 2.502(8) 1_655 ? O1 C1 1.274(12) . ? O1 Cd 2.396(7) 6_556 ? O2 C2 1.262(12) . ? O3 C3 1.223(12) . ? O4 C4 1.220(13) . ? O5 C5 1.258(13) . ? O5 Cd 2.502(8) 1_455 ? C1 C2 1.434(13) . ? C1 C5 1.455(15) . ? C2 C3 1.466(13) . ? C3 C4 1.516(15) . ? C4 C5 1.425(17) . ? 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 N Cd N 176.3(3) 7_565 . ? N Cd O1 89.22(16) 7_565 6_656 ? N Cd O1 89.22(16) . 6_656 ? N Cd O1 91.82(14) 7_565 . ? N Cd O1 91.82(14) . . ? O1 Cd O1 123.49(16) 6_656 . ? N Cd O2 90.32(17) 7_565 . ? N Cd O2 90.32(17) . . ? O1 Cd O2 165.1(2) 6_656 . ? O1 Cd O2 71.5(2) . . ? N Cd O5 88.16(14) 7_565 1_655 ? N Cd O5 88.16(14) . 1_655 ? O1 Cd O5 68.5(3) 6_656 1_655 ? O1 Cd O5 168.0(3) . 1_655 ? O2 Cd O5 96.6(3) . 1_655 ? C1 O1 Cd 122.0(6) . 6_556 ? C1 O1 Cd 110.2(6) . . ? Cd O1 Cd 127.8(3) 6_556 . ? C2 O2 Cd 109.9(6) . . ? C5 O5 Cd 150.9(9) . 1_455 ? O1 C1 C2 124.1(9) . . ? O1 C1 C5 127.8(9) . . ? C2 C1 C5 108.1(8) . . ? O2 C2 C1 124.4(9) . . ? O2 C2 C3 126.3(8) . . ? C1 C2 C3 109.4(8) . . ? O3 C3 C2 127.4(9) . . ? O3 C3 C4 127.0(10) . . ? C2 C3 C4 105.6(8) . . ? O4 C4 C5 129.9(11) . . ? O4 C4 C3 122.6(12) . . ? C5 C4 C3 107.5(9) . . ? O5 C5 C4 129.2(11) . . ? O5 C5 C1 121.4(11) . . ? C4 C5 C1 109.4(9) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 3.641 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.406 #===END data_complex2 _database_code_CSD 183157 _audit_creation_method SHELXL-97 _chemical_name_systematic ; silver(i)sodium(i)croconate solvated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H4 Ag Na O7' _chemical_formula_weight 306.94 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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 bcm' _symmetry_Int_Tables_number 57 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.890(4) _cell_length_b 6.243(4) _cell_length_c 14.452(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 802.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.575 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4327 _exptl_absorpt_correction_T_max 1.1093 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1886 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.59 _reflns_number_total 959 _reflns_number_gt 809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'nonius xpress' _computing_cell_refinement 'mosflm (j. appl. cryst., 1993, 21, 67)' _computing_data_reduction 'mosflm (j. appl. cryst., 1993, 21, 67)' _computing_structure_solution 'shelxs-97 (sheldrick, 1990)' _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics 'ortep3/windows (farrugia,1997)' _computing_publication_material 'wingx 1.63 (farrugia, 1999)' _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^)+(0.0564P)^2^+0.9462P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 959 _refine_ls_number_parameters 75 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.080 _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 Ag Ag 1.03120(5) 0.7500 0.5000 0.0526(3) Uani 1 2 d S . . C1 C 0.9921(3) 0.6114(5) 0.3001(2) 0.0313(6) Uani 1 1 d . . . C2 C 0.8348(3) 0.5965(5) 0.33191(19) 0.0323(6) Uani 1 1 d . . . C3 C 0.7370(5) 0.5801(7) 0.2500 0.0357(9) Uani 1 2 d S . . O1 O 1.1029(2) 0.6240(4) 0.35408(15) 0.0382(5) Uani 1 1 d . . . O2 O 0.7955(3) 0.5961(4) 0.41462(15) 0.0422(6) Uani 1 1 d . . . O3 O 0.5979(4) 0.5562(8) 0.2500 0.0557(10) Uani 1 2 d S . . Na Na 0.5857(3) 0.7500 0.5000 0.0405(5) Uani 1 2 d S . . O1W O 0.4110(3) 0.5570(4) 0.40299(17) 0.0445(6) Uani 1 1 d D . . H1 H 0.311(3) 0.596(7) 0.379(3) 0.053 Uiso 1 1 d D . . H2 H 0.474(4) 0.546(7) 0.347(2) 0.053 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 Ag 0.0540(4) 0.0751(4) 0.0289(3) -0.01155(15) 0.000 0.000 C1 0.0350(13) 0.0312(13) 0.0278(15) -0.0007(11) -0.0020(12) 0.0001(11) C2 0.0362(14) 0.0358(14) 0.0249(14) -0.0006(11) 0.0015(11) 0.0016(12) C3 0.0308(19) 0.045(2) 0.031(2) 0.000 0.000 0.0000(17) O1 0.0345(11) 0.0499(13) 0.0303(11) -0.0024(9) -0.0051(9) 0.0006(10) O2 0.0434(12) 0.0551(14) 0.0281(11) -0.0011(10) 0.0039(9) 0.0035(10) O3 0.0322(16) 0.096(3) 0.0387(19) 0.000 0.000 -0.0053(18) Na 0.0395(10) 0.0443(10) 0.0377(12) 0.0002(7) 0.000 0.000 O1W 0.0361(12) 0.0569(14) 0.0403(14) 0.0041(11) -0.0003(10) 0.0015(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 Ag O1 2.339(2) 3_566 ? Ag O1 2.339(2) . ? Ag O2 2.614(3) . ? Ag O2 2.614(3) 3_566 ? Ag Ag 3.170(2) 7_755 ? Ag Ag 3.170(2) 7_765 ? C1 O1 1.260(4) . ? C1 C1 1.447(6) 6_556 ? C1 C2 1.475(4) . ? C2 O2 1.245(3) . ? C2 C3 1.472(4) . ? C3 O3 1.246(6) . ? C3 C2 1.472(4) 6_556 ? O2 Na 2.434(3) . ? Na O1W 2.375(3) 7_665 ? Na O1W 2.375(3) 5_666 ? Na O1W 2.414(3) . ? Na O1W 2.414(3) 3_566 ? Na O2 2.434(3) 3_566 ? Na Na 3.474(3) 5_666 ? Na Na 3.474(3) 5_676 ? O1W Na 2.375(3) 5_666 ? 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 Ag O1 148.38(11) 3_566 . ? O1 Ag O2 140.12(7) 3_566 . ? O1 Ag O2 70.69(8) . . ? O1 Ag O2 70.69(8) 3_566 3_566 ? O1 Ag O2 140.12(7) . 3_566 ? O2 Ag O2 73.48(10) . 3_566 ? O1 Ag Ag 112.25(6) 3_566 7_755 ? O1 Ag Ag 73.54(6) . 7_755 ? O2 Ag Ag 59.87(6) . 7_755 ? O2 Ag Ag 102.80(6) 3_566 7_755 ? O1 Ag Ag 73.54(6) 3_566 7_765 ? O1 Ag Ag 112.25(6) . 7_765 ? O2 Ag Ag 102.80(6) . 7_765 ? O2 Ag Ag 59.87(6) 3_566 7_765 ? Ag Ag Ag 159.84(4) 7_755 7_765 ? O1 C1 C1 128.30(18) . 6_556 ? O1 C1 C2 123.5(3) . . ? C1 C1 C2 108.18(15) 6_556 . ? O2 C2 C3 127.3(3) . . ? O2 C2 C1 124.4(3) . . ? C3 C2 C1 108.3(3) . . ? O3 C3 C2 126.48(18) . . ? O3 C3 C2 126.48(18) . 6_556 ? C2 C3 C2 107.0(4) . 6_556 ? C1 O1 Ag 111.5(2) . . ? C2 O2 Na 134.5(2) . . ? C2 O2 Ag 103.2(2) . . ? Na O2 Ag 103.29(10) . . ? O1W Na O1W 178.61(16) 7_665 5_666 ? O1W Na O1W 93.89(10) 7_665 . ? O1W Na O1W 87.01(10) 5_666 . ? O1W Na O1W 87.01(10) 7_665 3_566 ? O1W Na O1W 93.89(10) 5_666 3_566 ? O1W Na O1W 99.93(15) . 3_566 ? O1W Na O2 88.36(10) 7_665 3_566 ? O1W Na O2 90.57(10) 5_666 3_566 ? O1W Na O2 169.82(11) . 3_566 ? O1W Na O2 90.09(9) 3_566 3_566 ? O1W Na O2 90.57(10) 7_665 . ? O1W Na O2 88.36(10) 5_666 . ? O1W Na O2 90.09(9) . . ? O1W Na O2 169.82(11) 3_566 . ? O2 Na O2 79.95(14) 3_566 . ? O1W Na Na 136.93(10) 7_665 5_666 ? O1W Na Na 43.96(7) 5_666 5_666 ? O1W Na Na 43.06(7) . 5_666 ? O1W Na Na 99.57(11) 3_566 5_666 ? O2 Na Na 133.70(8) 3_566 5_666 ? O2 Na Na 88.94(7) . 5_666 ? O1W Na Na 43.96(6) 7_665 5_676 ? O1W Na Na 136.93(10) 5_666 5_676 ? O1W Na Na 99.57(11) . 5_676 ? O1W Na Na 43.06(7) 3_566 5_676 ? O2 Na Na 88.94(7) 3_566 5_676 ? O2 Na Na 133.70(8) . 5_676 ? Na Na Na 127.95(14) 5_666 5_676 ? Na O1W Na 92.99(10) 5_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O2 0.5(5) . . . . ? C1 C1 C2 O2 -178.8(3) 6_556 . . . ? O1 C1 C2 C3 -178.9(3) . . . . ? C1 C1 C2 C3 1.8(3) 6_556 . . . ? O2 C2 C3 O3 -2.5(7) . . . . ? C1 C2 C3 O3 176.9(5) . . . . ? O2 C2 C3 C2 177.8(2) . . . 6_556 ? C1 C2 C3 C2 -2.9(5) . . . 6_556 ? C1 C1 O1 Ag 157.45(8) 6_556 . . . ? C2 C1 O1 Ag -21.7(4) . . . . ? O1 Ag O1 C1 -170.2(2) 3_566 . . . ? O2 Ag O1 C1 20.7(2) . . . . ? O2 Ag O1 C1 -6.5(3) 3_566 . . . ? Ag Ag O1 C1 83.9(2) 7_755 . . . ? Ag Ag O1 C1 -75.6(2) 7_765 . . . ? C3 C2 O2 Na -38.8(5) . . . . ? C1 C2 O2 Na 142.0(3) . . . . ? C3 C2 O2 Ag -162.9(3) . . . . ? C1 C2 O2 Ag 17.9(4) . . . . ? O1 Ag O2 C2 169.37(18) 3_566 . . . ? O1 Ag O2 C2 -19.57(19) . . . . ? O2 Ag O2 C2 142.6(2) 3_566 . . . ? Ag Ag O2 C2 -101.3(2) 7_755 . . . ? Ag Ag O2 C2 89.8(2) 7_765 . . . ? O1 Ag O2 Na 26.74(16) 3_566 . . . ? O1 Ag O2 Na -162.20(11) . . . . ? O2 Ag O2 Na 0.0 3_566 . . . ? Ag Ag O2 Na 116.07(9) 7_755 . . . ? Ag Ag O2 Na -52.81(8) 7_765 . . . ? C2 O2 Na O1W -35.8(3) . . . 7_665 ? Ag O2 Na O1W 88.24(10) . . . 7_665 ? C2 O2 Na O1W 145.1(3) . . . 5_666 ? Ag O2 Na O1W -90.87(10) . . . 5_666 ? C2 O2 Na O1W 58.1(3) . . . . ? Ag O2 Na O1W -177.88(9) . . . . ? C2 O2 Na O1W -112.0(5) . . . 3_566 ? Ag O2 Na O1W 12.1(5) . . . 3_566 ? C2 O2 Na O2 -124.1(3) . . . 3_566 ? Ag O2 Na O2 0.0 . . . 3_566 ? C2 O2 Na Na 101.1(3) . . . 5_666 ? Ag O2 Na Na -134.83(8) . . . 5_666 ? C2 O2 Na Na -45.3(4) . . . 5_676 ? Ag O2 Na Na 78.74(14) . . . 5_676 ? O1W Na O1W Na 178.93(13) 7_665 . . 5_666 ? O1W Na O1W Na 0.0 5_666 . . 5_666 ? O1W Na O1W Na -93.43(9) 3_566 . . 5_666 ? O2 Na O1W Na 76.4(5) 3_566 . . 5_666 ? O2 Na O1W Na 88.36(10) . . . 5_666 ? Na Na O1W Na -137.14(11) 5_676 . . 5_666 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.847 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.123