# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Professor Ping Liu' _publ_contact_author_address ; Fujian Institute of Research on The Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian 350002 P. R. China ; _publ_contact_author_email pliu@fjirsm.ac.cn _publ_contact_author_fax '86 591 83714648' _publ_contact_author_phone '86 591 83704960' _publ_section_title ; Synthesis, structures, and photoluminescent properties of two ligand unsupported silver(I) coordination polymers from isonicotinate anions ; loop_ _publ_author_name 'Ping Liu' 'Yun Chen' 'Mei-Hua Huang' 'Zheng Liu' 'Jian Wang' #========================================================================== data_shelxl _database_code_depnum_ccdc_archive 'CCDC 253117' #========================================================================== # CHEMICAL DAT _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Ag3 N3 O7' _chemical_formula_weight 629.82 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' _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 8.1686(16) _cell_length_b 10.4479(18) _cell_length_c 10.8106(17) _cell_angle_alpha 62.257(7) _cell_angle_beta 69.159(7) _cell_angle_gamma 80.817(9) _cell_volume 763.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 3.855 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5762 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3399 _reflns_number_gt 3134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^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 3399 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.12594(3) 0.11802(2) -0.00650(2) 0.01542(7) Uani 1 1 d . . . Ag2 Ag 0.48059(3) 0.13813(2) 0.02111(2) 0.01403(7) Uani 1 1 d . . . Ag3 Ag 0.25860(3) 0.39793(2) -0.00435(2) 0.01640(7) Uani 1 1 d . . . C1 C 0.5545(4) 0.7684(3) -0.7163(3) 0.0118(5) Uani 1 1 d . . . C2 C 0.4795(3) 0.6875(3) -0.5502(3) 0.0109(5) Uani 1 1 d . . . C3 C 0.3143(4) 0.6247(3) -0.4825(3) 0.0137(6) Uani 1 1 d . . . H3 H 0.2443 0.6345 -0.5402 0.016 Uiso 1 1 calc R . . C4 C 0.2516(4) 0.5475(3) -0.3303(3) 0.0149(6) Uani 1 1 d . . . H4 H 0.1375 0.5062 -0.2854 0.018 Uiso 1 1 calc R . . C5 C 0.5069(4) 0.5895(3) -0.3091(3) 0.0152(6) Uani 1 1 d . . . H5 H 0.5745 0.5785 -0.2492 0.018 Uiso 1 1 calc R . . C6 C 0.5772(4) 0.6675(3) -0.4608(3) 0.0145(6) Uani 1 1 d . . . H6 H 0.6919 0.7073 -0.5035 0.017 Uiso 1 1 calc R . . C7 C 0.2646(3) 0.1476(3) 0.3028(3) 0.0122(5) Uani 1 1 d . . . C8 C 0.1855(3) 0.0897(3) 0.4687(3) 0.0110(5) Uani 1 1 d . . . C9 C 0.0378(4) 0.1542(3) 0.5291(3) 0.0139(5) Uani 1 1 d . . . H9 H -0.0103 0.2374 0.4662 0.017 Uiso 1 1 calc R . . C10 C -0.0398(4) 0.0975(3) 0.6809(3) 0.0144(6) Uani 1 1 d . . . H10 H -0.1404 0.1434 0.7204 0.017 Uiso 1 1 calc R . . C11 C 0.1688(4) -0.0807(3) 0.7160(3) 0.0184(6) Uani 1 1 d . . . H11 H 0.2164 -0.1620 0.7811 0.022 Uiso 1 1 calc R . . C12 C 0.2535(4) -0.0297(3) 0.5650(3) 0.0148(6) Uani 1 1 d . . . H12 H 0.3561 -0.0756 0.5283 0.018 Uiso 1 1 calc R . . N1 N 0.3464(3) 0.5287(2) -0.2433(2) 0.0141(5) Uani 1 1 d . . . N2 N 0.0232(3) -0.0209(3) 0.7744(2) 0.0146(5) Uani 1 1 d . . . N3 N 0.7935(3) 0.3235(3) 0.9549(2) 0.0141(5) Uani 1 1 d . . . O1 O 0.3880(3) 0.0777(2) 0.2554(2) 0.0176(4) Uani 1 1 d . . . O2 O 0.1951(3) 0.2602(2) 0.2293(2) 0.0192(4) Uani 1 1 d . . . O3 O 0.7135(3) 0.8027(2) -0.7674(2) 0.0186(4) Uani 1 1 d . . . O4 O 0.4516(3) 0.7902(2) -0.7869(2) 0.0167(4) Uani 1 1 d . . . O5 O 0.9207(3) 0.3806(2) 0.9499(2) 0.0191(4) Uani 1 1 d . . . O6 O 0.8129(3) 0.2067(2) 0.9446(2) 0.0223(5) Uani 1 1 d . . . O7 O 0.6456(3) 0.3817(2) 0.9737(2) 0.0222(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01448(12) 0.02001(13) 0.00511(10) -0.00250(8) 0.00151(8) -0.00355(8) Ag2 0.01645(12) 0.01847(13) 0.00509(10) -0.00507(8) -0.00036(8) -0.00223(8) Ag3 0.02291(13) 0.01533(12) 0.00423(11) -0.00086(8) -0.00156(8) -0.00035(9) C1 0.0169(13) 0.0101(13) 0.0070(11) -0.0050(10) -0.0003(10) -0.0013(10) C2 0.0166(13) 0.0074(12) 0.0064(11) -0.0026(10) -0.0016(10) -0.0007(10) C3 0.0134(13) 0.0160(14) 0.0104(12) -0.0053(11) -0.0039(11) 0.0020(10) C4 0.0136(13) 0.0143(14) 0.0099(12) -0.0021(11) -0.0011(10) 0.0009(10) C5 0.0206(14) 0.0160(14) 0.0092(12) -0.0047(11) -0.0057(11) -0.0014(11) C6 0.0161(13) 0.0157(14) 0.0104(12) -0.0051(11) -0.0014(11) -0.0051(11) C7 0.0141(13) 0.0145(14) 0.0064(11) -0.0031(10) -0.0004(10) -0.0071(10) C8 0.0135(13) 0.0139(13) 0.0052(11) -0.0043(10) -0.0006(10) -0.0046(10) C9 0.0146(13) 0.0147(14) 0.0089(12) -0.0031(10) -0.0033(10) 0.0012(10) C10 0.0115(12) 0.0197(15) 0.0093(12) -0.0061(11) -0.0005(10) -0.0007(10) C11 0.0213(15) 0.0178(15) 0.0075(12) -0.0010(11) -0.0030(11) 0.0035(11) C12 0.0171(14) 0.0148(14) 0.0094(12) -0.0050(11) -0.0021(11) 0.0020(11) N1 0.0188(12) 0.0141(12) 0.0051(10) -0.0026(9) -0.0007(9) -0.0019(9) N2 0.0159(12) 0.0169(12) 0.0068(10) -0.0038(9) 0.0007(9) -0.0037(9) N3 0.0157(11) 0.0174(12) 0.0049(10) -0.0019(9) -0.0019(9) -0.0018(9) O1 0.0202(10) 0.0217(11) 0.0065(8) -0.0060(8) 0.0000(8) 0.0011(8) O2 0.0274(11) 0.0173(11) 0.0041(8) 0.0004(8) -0.0030(8) 0.0011(9) O3 0.0179(10) 0.0270(11) 0.0054(8) -0.0043(8) 0.0025(8) -0.0101(8) O4 0.0186(10) 0.0234(11) 0.0050(8) -0.0055(8) -0.0018(8) 0.0011(8) O5 0.0115(10) 0.0211(11) 0.0221(11) -0.0075(9) -0.0029(8) -0.0058(8) O6 0.0260(11) 0.0220(12) 0.0240(11) -0.0146(9) -0.0089(9) 0.0033(9) O7 0.0134(10) 0.0262(12) 0.0279(11) -0.0125(9) -0.0086(9) 0.0040(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 O3 2.1356(19) 2_664 ? Ag1 N2 2.159(2) 2_556 ? Ag1 Ag2 3.0649(6) . ? Ag1 Ag3 3.2894(6) . ? Ag2 O4 2.1557(19) 2_664 ? Ag2 O1 2.1648(19) . ? Ag2 Ag3 2.9699(6) . ? Ag2 Ag2 3.0776(7) 2_655 ? Ag3 O2 2.1546(18) . ? Ag3 N1 2.183(2) . ? C1 O4 1.254(3) . ? C1 O3 1.255(3) . ? C1 C2 1.511(3) . ? C2 C3 1.386(4) . ? C2 C6 1.386(4) . ? C3 C4 1.384(4) . ? C4 N1 1.348(4) . ? C5 N1 1.345(4) . ? C5 C6 1.386(4) . ? C7 O1 1.248(3) . ? C7 O2 1.255(3) . ? C7 C8 1.513(3) . ? C8 C9 1.388(4) . ? C8 C12 1.389(4) . ? C9 C10 1.386(4) . ? C10 N2 1.348(4) . ? C11 N2 1.341(4) . ? C11 C12 1.389(4) . ? N2 Ag1 2.159(2) 2_556 ? N3 O5 1.252(3) . ? N3 O7 1.255(3) . ? N3 O6 1.257(3) . ? O3 Ag1 2.1356(19) 2_664 ? O4 Ag2 2.1557(19) 2_664 ? 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 O3 Ag1 N2 175.03(9) 2_664 2_556 ? O3 Ag1 Ag2 79.73(6) 2_664 . ? N2 Ag1 Ag2 98.19(6) 2_556 . ? O3 Ag1 Ag3 87.62(6) 2_664 . ? N2 Ag1 Ag3 94.94(7) 2_556 . ? Ag2 Ag1 Ag3 55.593(10) . . ? O4 Ag2 O1 174.24(8) 2_664 . ? O4 Ag2 Ag3 89.70(6) 2_664 . ? O1 Ag2 Ag3 85.22(6) . . ? O4 Ag2 Ag1 78.44(5) 2_664 . ? O1 Ag2 Ag1 96.98(6) . . ? Ag3 Ag2 Ag1 66.037(13) . . ? O4 Ag2 Ag2 74.09(6) 2_664 2_655 ? O1 Ag2 Ag2 108.53(6) . 2_655 ? Ag3 Ag2 Ag2 142.535(14) . 2_655 ? Ag1 Ag2 Ag2 77.568(12) . 2_655 ? O2 Ag3 N1 174.83(8) . . ? O2 Ag3 Ag2 74.86(6) . . ? N1 Ag3 Ag2 100.60(6) . . ? O2 Ag3 Ag1 83.45(6) . . ? N1 Ag3 Ag1 96.33(6) . . ? Ag2 Ag3 Ag1 58.369(14) . . ? O4 C1 O3 127.7(2) . . ? O4 C1 C2 116.2(2) . . ? O3 C1 C2 116.1(2) . . ? C3 C2 C6 117.7(2) . . ? C3 C2 C1 121.2(2) . . ? C6 C2 C1 121.0(2) . . ? C4 C3 C2 119.7(3) . . ? N1 C4 C3 122.5(3) . . ? N1 C5 C6 122.4(3) . . ? C5 C6 C2 119.8(2) . . ? O1 C7 O2 127.8(2) . . ? O1 C7 C8 116.9(2) . . ? O2 C7 C8 115.2(2) . . ? C9 C8 C12 117.9(2) . . ? C9 C8 C7 119.9(2) . . ? C12 C8 C7 122.2(2) . . ? C10 C9 C8 120.1(2) . . ? N2 C10 C9 122.0(3) . . ? N2 C11 C12 123.3(3) . . ? C8 C12 C11 118.8(3) . . ? C5 N1 C4 117.8(2) . . ? C5 N1 Ag3 118.46(18) . . ? C4 N1 Ag3 123.71(18) . . ? C11 N2 C10 117.8(2) . . ? C11 N2 Ag1 122.75(18) . 2_556 ? C10 N2 Ag1 119.18(18) . 2_556 ? O5 N3 O7 119.7(2) . . ? O5 N3 O6 120.1(2) . . ? O7 N3 O6 120.2(2) . . ? C7 O1 Ag2 118.19(17) . . ? C7 O2 Ag3 132.32(18) . . ? C1 O3 Ag1 126.37(17) . 2_664 ? C1 O4 Ag2 127.05(17) . 2_664 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.869 _refine_diff_density_min -1.207 _refine_diff_density_rms 0.117 #========================================================================== data_I _database_code_depnum_ccdc_archive 'CCDC 253118' #========================================================================== # CHEMICAL DAT _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24.50 H20 Ag4 N4 O9.50' _chemical_formula_weight 953.93 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' 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' _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 8.6509(12) _cell_length_b 12.618(2) _cell_length_c 14.000(3) _cell_angle_alpha 107.936(10) _cell_angle_beta 99.633(6) _cell_angle_gamma 90.210(7) _cell_volume 1430.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 2.757 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10946 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6442 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+6.8239P] 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 6442 _refine_ls_number_parameters 407 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ag1 Ag -0.11478(4) 0.51475(3) 0.60634(3) 0.02015(9) Uani 1 1 d . . . Ag2 Ag 0.12013(4) 0.65700(3) 0.75249(3) 0.02153(10) Uani 1 1 d . . . Ag3 Ag 0.99029(5) 1.03837(3) 1.25647(3) 0.02490(10) Uani 1 1 d . . . Ag4 Ag 1.01111(4) 1.13788(3) 1.10452(3) 0.01940(9) Uani 1 1 d . . . C1 C 1.5952(6) 1.3336(4) 1.5206(4) 0.0244(10) Uani 1 1 d . . . H1 H 1.6358 1.3205 1.5831 0.029 Uiso 1 1 calc R . . C2 C 1.4636(6) 1.2694(4) 1.4589(4) 0.0221(10) Uani 1 1 d . . . H2 H 1.4176 1.2124 1.4782 0.027 Uiso 1 1 calc R . . C3 C 1.4002(6) 1.2896(4) 1.3687(4) 0.0199(9) Uani 1 1 d . . . C4 C 1.4718(6) 1.3731(4) 1.3436(4) 0.0203(10) Uani 1 1 d . . . H4 H 1.4296 1.3903 1.2833 0.024 Uiso 1 1 calc R . . C5 C 1.6065(6) 1.4318(4) 1.4077(4) 0.0221(10) Uani 1 1 d . . . H5 H 1.6572 1.4871 1.3886 0.026 Uiso 1 1 calc R . . C6 C 1.2589(6) 1.2203(4) 1.2981(3) 0.0196(9) Uani 1 1 d . . . C7 C 0.7471(6) 0.9472(4) 1.0609(4) 0.0207(10) Uani 1 1 d . . . C8 C 0.6072(5) 0.8763(4) 0.9909(4) 0.0196(9) Uani 1 1 d . . . C9 C 0.5287(6) 0.7978(4) 1.0193(4) 0.0217(10) Uani 1 1 d . . . H9 H 0.5647 0.7850 1.0825 0.026 Uiso 1 1 calc R . . C10 C 0.3961(6) 0.7378(4) 0.9533(4) 0.0233(10) Uani 1 1 d . . . H10 H 0.3435 0.6836 0.9727 0.028 Uiso 1 1 calc R . . C11 C 0.4168(6) 0.8294(4) 0.8371(4) 0.0207(10) Uani 1 1 d . . . H11 H 0.3773 0.8421 0.7743 0.025 Uiso 1 1 calc R . . C12 C 0.5522(6) 0.8905(4) 0.8974(4) 0.0210(10) Uani 1 1 d . . . H12 H 0.6060 0.9412 0.8746 0.025 Uiso 1 1 calc R . . C13 C 0.0063(6) 0.4463(4) 0.7961(3) 0.0188(9) Uani 1 1 d . . . C14 C 0.0082(6) 0.3751(4) 0.8658(3) 0.0186(9) Uani 1 1 d . . . C15 C -0.1024(6) 0.2863(4) 0.8422(3) 0.0204(10) Uani 1 1 d . . . H15 H -0.1797 0.2693 0.7820 0.025 Uiso 1 1 calc R . . C16 C -0.0982(6) 0.2228(4) 0.9082(4) 0.0241(10) Uani 1 1 d . . . H16 H -0.1705 0.1601 0.8903 0.029 Uiso 1 1 calc R . . C17 C 0.1104(6) 0.3328(4) 1.0193(4) 0.0197(9) Uani 1 1 d . . . H17 H 0.1834 0.3501 1.0815 0.024 Uiso 1 1 calc R . . C18 C 0.1177(6) 0.3979(4) 0.9556(4) 0.0220(10) Uani 1 1 d . . . H18 H 0.1961 0.4569 0.9733 0.026 Uiso 1 1 calc R . . C19 C 0.0204(6) 0.7201(4) 0.5562(3) 0.0185(9) Uani 1 1 d . . . C20 C 0.0212(6) 0.7909(4) 0.4858(3) 0.0186(9) Uani 1 1 d . . . C21 C 0.1415(6) 0.8698(4) 0.5002(4) 0.0219(10) Uani 1 1 d . . . H21 H 0.2273 0.8815 0.5552 0.026 Uiso 1 1 calc R . . C22 C 0.1352(6) 0.9314(4) 0.4333(4) 0.0228(10) Uani 1 1 d . . . H22 H 0.2189 0.9848 0.4431 0.027 Uiso 1 1 calc R . . C23 C -0.1001(6) 0.8414(4) 0.3407(4) 0.0242(10) Uani 1 1 d . . . H23 H -0.1841 0.8310 0.2849 0.029 Uiso 1 1 calc R . . C24 C -0.1023(6) 0.7754(4) 0.4041(4) 0.0203(9) Uani 1 1 d . . . H24 H -0.1858 0.7211 0.3919 0.024 Uiso 1 1 calc R . . C25 C 0.5249(12) 0.4450(9) 0.8433(8) 0.026(2) Uani 0.50 1 d P . . H25A H 0.6226 0.4193 0.8194 0.038 Uiso 0.50 1 calc PR . . H25B H 0.5234 0.4323 0.9087 0.038 Uiso 0.50 1 calc PR . . H25C H 0.5187 0.5248 0.8518 0.038 Uiso 0.50 1 calc PR . . H10A H 0.492(14) 0.246(7) 0.713(8) 0.14(5) Uiso 1 1 d D . . H11A H 0.581(4) 0.065(4) 0.725(4) 0.018(13) Uiso 1 1 d D . . N1 N 1.6674(5) 1.4130(3) 1.4959(3) 0.0210(8) Uani 1 1 d . . . N2 N 0.3398(5) 0.7536(3) 0.8637(3) 0.0223(9) Uani 1 1 d . . . N3 N 0.0052(5) 0.2473(3) 0.9966(3) 0.0198(8) Uani 1 1 d . . . N4 N 0.0155(5) 0.9190(3) 0.3552(3) 0.0225(9) Uani 1 1 d . . . O1 O 1.2298(5) 1.1279(3) 1.3112(3) 0.0356(10) Uani 1 1 d . . . O2 O 1.1853(4) 1.2588(3) 1.2328(3) 0.0238(7) Uani 1 1 d . . . O3 O 0.7714(5) 0.9476(3) 1.1514(3) 0.0350(9) Uani 1 1 d . . . O4 O 0.8274(4) 1.0008(3) 1.0216(3) 0.0250(7) Uani 1 1 d . . . O5 O 0.1299(4) 0.5060(3) 0.8084(3) 0.0315(9) Uani 1 1 d . . . O6 O -0.1174(4) 0.4412(3) 0.7338(3) 0.0280(8) Uani 1 1 d . . . O7 O -0.0608(4) 0.6309(3) 0.5224(3) 0.0237(7) Uani 1 1 d . . . O8 O 0.1059(4) 0.7597(3) 0.6438(3) 0.0238(7) Uani 1 1 d . . . O9 O 0.4039(9) 0.3891(8) 0.7756(8) 0.059(3) Uani 0.50 1 d P . . H9A H 0.3578 0.4313 0.7454 0.088 Uiso 0.50 1 calc PR . . O10 O 0.5371(16) 0.1933(12) 0.6749(11) 0.080(4) Uani 0.50 1 d PD . . O11 O 0.4859(16) 0.0404(19) 0.6929(10) 0.145(9) Uani 0.50 1 d PD . . 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 0.02184(19) 0.02122(18) 0.01739(18) 0.01073(14) -0.00530(13) -0.00782(14) Ag2 0.02371(19) 0.02257(19) 0.01832(18) 0.01233(15) -0.00737(14) -0.00891(14) Ag3 0.0312(2) 0.02399(19) 0.01912(19) 0.01369(15) -0.00965(15) -0.01287(16) Ag4 0.02311(19) 0.01906(18) 0.01582(17) 0.00914(14) -0.00397(13) -0.00692(14) C1 0.025(3) 0.024(2) 0.021(2) 0.006(2) -0.0021(19) -0.001(2) C2 0.021(2) 0.021(2) 0.024(2) 0.008(2) -0.0008(19) -0.0010(19) C3 0.019(2) 0.019(2) 0.019(2) 0.0028(18) 0.0001(18) -0.0003(18) C4 0.019(2) 0.022(2) 0.016(2) 0.0021(18) 0.0003(17) -0.0027(19) C5 0.019(2) 0.024(2) 0.020(2) 0.0040(19) -0.0005(18) -0.0032(19) C6 0.021(2) 0.019(2) 0.017(2) 0.0039(18) 0.0004(18) -0.0032(18) C7 0.021(2) 0.016(2) 0.021(2) 0.0033(18) -0.0017(18) -0.0018(18) C8 0.016(2) 0.018(2) 0.019(2) 0.0005(18) -0.0012(17) -0.0005(18) C9 0.021(2) 0.024(2) 0.018(2) 0.0073(19) -0.0033(18) -0.0023(19) C10 0.022(2) 0.026(2) 0.020(2) 0.008(2) -0.0029(19) -0.006(2) C11 0.018(2) 0.022(2) 0.018(2) 0.0021(18) 0.0001(17) -0.0002(19) C12 0.021(2) 0.019(2) 0.019(2) 0.0020(18) 0.0024(18) -0.0042(19) C13 0.024(2) 0.016(2) 0.017(2) 0.0065(18) 0.0029(18) 0.0014(18) C14 0.020(2) 0.022(2) 0.018(2) 0.0102(18) 0.0058(18) 0.0038(18) C15 0.025(2) 0.022(2) 0.014(2) 0.0092(18) -0.0024(18) -0.0030(19) C16 0.025(3) 0.027(3) 0.023(2) 0.015(2) -0.0018(19) -0.004(2) C17 0.021(2) 0.019(2) 0.018(2) 0.0059(18) 0.0014(18) 0.0027(19) C18 0.025(3) 0.021(2) 0.021(2) 0.0088(19) 0.0015(19) -0.0015(19) C19 0.021(2) 0.025(2) 0.013(2) 0.0108(19) 0.0059(17) 0.0061(19) C20 0.028(3) 0.015(2) 0.013(2) 0.0046(17) 0.0045(18) 0.0022(19) C21 0.026(3) 0.019(2) 0.020(2) 0.0087(19) -0.0021(19) -0.0058(19) C22 0.026(3) 0.023(2) 0.019(2) 0.0078(19) 0.0000(19) -0.005(2) C23 0.028(3) 0.025(2) 0.021(2) 0.012(2) -0.0016(19) 0.000(2) C24 0.023(2) 0.020(2) 0.020(2) 0.0111(19) 0.0020(18) -0.0041(19) C25 0.020(5) 0.027(5) 0.032(5) 0.015(4) -0.001(4) 0.009(4) N1 0.018(2) 0.021(2) 0.018(2) 0.0022(16) -0.0043(15) -0.0060(16) N2 0.020(2) 0.020(2) 0.022(2) 0.0028(16) -0.0022(16) -0.0027(16) N3 0.026(2) 0.0193(19) 0.0161(19) 0.0093(16) 0.0015(16) -0.0019(16) N4 0.031(2) 0.022(2) 0.0161(19) 0.0101(16) 0.0022(16) -0.0020(17) O1 0.035(2) 0.0254(19) 0.040(2) 0.0152(17) -0.0209(17) -0.0115(16) O2 0.0305(19) 0.0219(17) 0.0195(17) 0.0095(14) 0.0003(14) 0.0005(15) O3 0.034(2) 0.041(2) 0.030(2) 0.0204(18) -0.0136(16) -0.0178(18) O4 0.0216(18) 0.0240(18) 0.0252(18) 0.0044(15) -0.0012(14) -0.0064(14) O5 0.030(2) 0.037(2) 0.036(2) 0.0277(18) -0.0037(16) -0.0035(17) O6 0.0232(19) 0.033(2) 0.0271(19) 0.0152(16) -0.0073(15) -0.0027(15) O7 0.0280(19) 0.0251(18) 0.0209(17) 0.0129(15) 0.0014(14) -0.0015(15) O8 0.0297(19) 0.0195(16) 0.0222(18) 0.0116(14) -0.0047(14) -0.0040(14) O9 0.013(4) 0.059(6) 0.064(6) -0.034(5) -0.003(4) 0.008(4) O10 0.071(9) 0.084(9) 0.094(10) 0.024(8) 0.046(8) 0.021(7) O11 0.055(8) 0.27(2) 0.059(8) -0.018(11) -0.006(6) 0.086(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 Ag1 O7 2.233(3) . ? Ag1 O6 2.253(4) . ? Ag1 N1 2.318(4) 1_344 ? Ag1 Ag2 2.8031(6) . ? Ag2 O5 2.268(3) . ? Ag2 O8 2.272(3) . ? Ag2 N2 2.312(4) . ? Ag2 Ag4 3.0962(7) 2_677 ? Ag3 O1 2.253(4) . ? Ag3 O3 2.253(4) . ? Ag3 N4 2.325(4) 1_656 ? Ag3 Ag4 2.8118(6) . ? Ag4 O4 2.234(3) . ? Ag4 O2 2.283(4) . ? Ag4 N3 2.335(4) 1_665 ? Ag4 Ag2 3.0962(7) 2_677 ? C1 N1 1.340(6) . ? C1 C2 1.390(7) . ? C2 C3 1.388(7) . ? C3 C4 1.383(7) . ? C3 C6 1.514(6) . ? C4 C5 1.395(7) . ? C5 N1 1.349(6) . ? C6 O2 1.248(6) . ? C6 O1 1.266(6) . ? C7 O3 1.247(6) . ? C7 O4 1.264(6) . ? C7 C8 1.510(6) . ? C8 C12 1.381(7) . ? C8 C9 1.388(7) . ? C9 C10 1.396(7) . ? C10 N2 1.342(6) . ? C11 N2 1.339(6) . ? C11 C12 1.393(7) . ? C13 O6 1.250(6) . ? C13 O5 1.263(6) . ? C13 C14 1.515(6) . ? C14 C15 1.392(7) . ? C14 C18 1.392(7) . ? C15 C16 1.394(6) . ? C16 N3 1.348(6) . ? C17 N3 1.333(6) . ? C17 C18 1.394(7) . ? C19 O7 1.241(6) . ? C19 O8 1.272(6) . ? C19 C20 1.521(6) . ? C20 C21 1.384(7) . ? C20 C24 1.392(7) . ? C21 C22 1.385(7) . ? C22 N4 1.344(6) . ? C23 N4 1.343(6) . ? C23 C24 1.394(6) . ? C25 O9 1.320(13) . ? N1 Ag1 2.318(4) 1_766 ? N3 Ag4 2.335(4) 1_445 ? N4 Ag3 2.325(4) 1_454 ? 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 Ag1 O6 160.75(13) . . ? O7 Ag1 N1 100.55(14) . 1_344 ? O6 Ag1 N1 97.82(14) . 1_344 ? O7 Ag1 Ag2 79.63(9) . . ? O6 Ag1 Ag2 81.39(9) . . ? N1 Ag1 Ag2 172.36(10) 1_344 . ? O5 Ag2 O8 159.86(14) . . ? O5 Ag2 N2 96.38(14) . . ? O8 Ag2 N2 96.16(14) . . ? O5 Ag2 Ag1 79.50(10) . . ? O8 Ag2 Ag1 85.85(9) . . ? N2 Ag2 Ag1 171.24(10) . . ? O5 Ag2 Ag4 113.46(11) . 2_677 ? O8 Ag2 Ag4 84.94(9) . 2_677 ? N2 Ag2 Ag4 75.70(10) . 2_677 ? Ag1 Ag2 Ag4 113.01(2) . 2_677 ? O1 Ag3 O3 160.80(15) . . ? O1 Ag3 N4 98.91(14) . 1_656 ? O3 Ag3 N4 94.77(15) . 1_656 ? O1 Ag3 Ag4 78.08(10) . . ? O3 Ag3 Ag4 85.02(10) . . ? N4 Ag3 Ag4 163.71(10) 1_656 . ? O4 Ag4 O2 161.15(13) . . ? O4 Ag4 N3 104.07(14) . 1_665 ? O2 Ag4 N3 93.76(13) . 1_665 ? O4 Ag4 Ag3 79.03(9) . . ? O2 Ag4 Ag3 82.34(9) . . ? N3 Ag4 Ag3 169.45(10) 1_665 . ? O4 Ag4 Ag2 112.85(9) . 2_677 ? O2 Ag4 Ag2 62.27(9) . 2_677 ? N3 Ag4 Ag2 84.48(10) 1_665 2_677 ? Ag3 Ag4 Ag2 85.037(19) . 2_677 ? N1 C1 C2 123.0(5) . . ? C3 C2 C1 119.2(5) . . ? C4 C3 C2 118.3(5) . . ? C4 C3 C6 120.6(4) . . ? C2 C3 C6 121.0(4) . . ? C3 C4 C5 119.3(5) . . ? N1 C5 C4 122.5(5) . . ? O2 C6 O1 127.0(4) . . ? O2 C6 C3 117.3(4) . . ? O1 C6 C3 115.7(4) . . ? O3 C7 O4 126.6(5) . . ? O3 C7 C8 117.1(4) . . ? O4 C7 C8 116.3(4) . . ? C12 C8 C9 118.5(4) . . ? C12 C8 C7 120.2(4) . . ? C9 C8 C7 121.4(4) . . ? C8 C9 C10 118.9(4) . . ? N2 C10 C9 122.8(5) . . ? N2 C11 C12 123.0(5) . . ? C8 C12 C11 119.1(5) . . ? O6 C13 O5 126.9(4) . . ? O6 C13 C14 117.0(4) . . ? O5 C13 C14 116.1(4) . . ? C15 C14 C18 118.4(4) . . ? C15 C14 C13 120.4(4) . . ? C18 C14 C13 121.1(4) . . ? C14 C15 C16 119.0(4) . . ? N3 C16 C15 122.2(5) . . ? N3 C17 C18 122.7(4) . . ? C14 C18 C17 119.0(5) . . ? O7 C19 O8 127.3(4) . . ? O7 C19 C20 117.4(4) . . ? O8 C19 C20 115.3(4) . . ? C21 C20 C24 119.1(4) . . ? C21 C20 C19 121.9(4) . . ? C24 C20 C19 119.1(4) . . ? C20 C21 C22 119.0(4) . . ? N4 C22 C21 122.8(5) . . ? N4 C23 C24 122.9(5) . . ? C20 C24 C23 118.3(4) . . ? C1 N1 C5 117.7(4) . . ? C1 N1 Ag1 119.4(3) . 1_766 ? C5 N1 Ag1 122.8(3) . 1_766 ? C11 N2 C10 117.7(4) . . ? C11 N2 Ag2 118.3(3) . . ? C10 N2 Ag2 124.0(3) . . ? C17 N3 C16 118.6(4) . . ? C17 N3 Ag4 120.0(3) . 1_445 ? C16 N3 Ag4 121.3(3) . 1_445 ? C23 N4 C22 118.0(4) . . ? C23 N4 Ag3 119.4(3) . 1_454 ? C22 N4 Ag3 122.3(3) . 1_454 ? C6 O1 Ag3 121.9(3) . . ? C6 O2 Ag4 116.6(3) . . ? C7 O3 Ag3 119.1(3) . . ? C7 O4 Ag4 126.7(3) . . ? C13 O5 Ag2 119.9(3) . . ? C13 O6 Ag1 119.2(3) . . ? C19 O7 Ag1 128.1(3) . . ? C19 O8 Ag2 118.0(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.522 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.141