Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Content-Length: 32305 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 935 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Faure, Rene' 'Haj, Mohammad Abul' 'Quiros, Miguel' 'Salas, Juan M' _publ_contact_author_name 'Miguel Quir\'os' -publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email 'mquiros@ugr.es' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_section_title ; Silver complexes with triazolopyrimidine ligands containing an exocyclic oxygen atom: X-ray evidence for an unusual tautomeric form. ; data_compound1 _database_code_CSD 157473 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C10 H8 Ag2 N10 O8' _chemical_formula_weight 612.00 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 5.3881(7) _cell_length_b 18.245(2) _cell_length_c 8.7100(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.946(9) _cell_angle_gamma 90.00 _cell_volume 848.04(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 12.41 _exptl_crystal_description 'prismatic' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 54.31 _diffrn_reflns_number 3099 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 29.99 _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.898 _reflns_number_total 2227 _reflns_number_gt 1645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 2227 _refine_ls_number_parameters 139 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.116 _refine_diff_density_min -3.128 _refine_diff_density_rms 0.370 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 0.29425(11) 0.44307(3) 0.53102(5) 0.0399(2) Uani 1 1 d . . . N1 N 0.2359(13) 0.5582(3) 0.9634(6) 0.0412(15) Uani 1 1 d . . . C2 C 0.1781(14) 0.5113(4) 0.8489(7) 0.0362(15) Uani 1 1 d . . . H2 H 0.0519 0.4766 0.8501 0.043 Uiso 1 1 d R . . N3 N 0.3134(11) 0.5167(3) 0.7290(5) 0.0310(12) Uani 1 1 d . . . C3A C 0.4730(14) 0.5717(3) 0.7723(6) 0.0300(13) Uani 1 1 d . . . N4 N 0.6527(10) 0.6005(3) 0.6965(5) 0.0276(11) Uani 1 1 d . . . C5 C 0.7867(13) 0.6559(3) 0.7662(6) 0.0319(14) Uani 1 1 d . . . O5 O 0.9630(10) 0.6811(3) 0.6926(6) 0.0410(12) Uani 1 1 d D . . H5 H 1.026(16) 0.718(3) 0.744(9) 0.049 Uiso 1 1 d D . . C6 C 0.7410(15) 0.6833(4) 0.9146(7) 0.0386(15) Uani 1 1 d . . . H6 H 0.8373 0.7217 0.9612 0.046 Uiso 1 1 d R . . C7 C 0.5605(15) 0.6539(4) 0.9855(7) 0.0374(15) Uani 1 1 d . . . H7 H 0.5274 0.6711 1.0811 0.045 Uiso 1 1 d R . . N8 N 0.4274(11) 0.5978(3) 0.9125(5) 0.0313(11) Uani 1 1 d . . . N1N N -0.1162(13) 0.3452(3) 0.6736(7) 0.0405(15) Uani 1 1 d . . . O1N O 0.1175(11) 0.3400(3) 0.6919(7) 0.0473(13) Uani 1 1 d . . . O2N O -0.2427(12) 0.2903(3) 0.7022(9) 0.0637(17) Uani 1 1 d . . . O3N O -0.2144(13) 0.4032(4) 0.6279(10) 0.073(2) 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 Ag 0.0516(5) 0.0431(3) 0.0277(3) -0.00959(18) 0.0155(2) -0.0119(2) N1 0.048(4) 0.051(3) 0.027(2) -0.003(2) 0.017(3) -0.004(3) C2 0.036(4) 0.045(3) 0.030(3) -0.001(3) 0.012(3) 0.002(3) N3 0.036(3) 0.034(2) 0.025(2) -0.0037(18) 0.012(2) 0.000(2) C3A 0.038(4) 0.031(3) 0.022(2) 0.000(2) 0.007(2) 0.005(3) N4 0.031(3) 0.028(2) 0.026(2) -0.0004(17) 0.012(2) 0.000(2) C5 0.038(4) 0.035(3) 0.023(2) -0.001(2) 0.005(2) -0.001(3) O5 0.046(3) 0.043(2) 0.036(2) -0.0041(19) 0.014(2) -0.014(2) C6 0.049(5) 0.038(3) 0.028(3) -0.007(2) 0.001(3) -0.004(3) C7 0.047(5) 0.043(3) 0.022(2) -0.007(2) 0.006(3) 0.002(3) N8 0.033(3) 0.040(3) 0.022(2) -0.0038(19) 0.008(2) 0.002(2) N1N 0.050(5) 0.036(3) 0.035(3) 0.002(2) 0.004(3) -0.007(3) O1N 0.033(3) 0.051(3) 0.058(3) 0.005(2) 0.007(2) 0.000(2) O2N 0.045(4) 0.055(3) 0.092(5) 0.011(3) 0.012(3) -0.009(3) O3N 0.059(4) 0.047(3) 0.106(6) 0.015(3) -0.018(4) 0.012(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 Ag N3 2.177(5) . ? Ag N4 2.190(5) 3_666 ? Ag O1N 2.603(6) . ? Ag O3N 2.763(7) 1_655 ? Ag Ag 3.1393(11) 3_666 ? N1 C2 1.318(9) . ? N1 N8 1.382(8) . ? C2 N3 1.358(8) . ? N3 C3A 1.341(9) . ? C3A N4 1.352(8) . ? C3A N8 1.364(7) . ? N4 C5 1.338(8) . ? N4 Ag 2.190(5) 3_666 ? C5 O5 1.301(8) . ? C5 C6 1.439(8) . ? C6 C7 1.335(11) . ? C7 N8 1.356(8) . ? N1N O3N 1.224(8) . ? N1N O1N 1.251(9) . ? N1N O2N 1.256(8) . ? 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 N3 Ag N4 160.5(2) . 3_666 ? N3 Ag O1N 90.02(19) . . ? N4 Ag O1N 109.14(18) 3_666 . ? N3 Ag O3N 89.0(2) . 1_655 ? N4 Ag O3N 86.6(2) 3_666 1_655 ? O1N Ag O3N 93.0(2) . 1_655 ? N3 Ag Ag 76.73(15) . 3_666 ? N4 Ag Ag 84.32(14) 3_666 3_666 ? O1N Ag Ag 152.93(13) . 3_666 ? O3N Ag Ag 63.72(15) 1_655 3_666 ? C2 N1 N8 101.8(5) . . ? N1 C2 N3 116.0(7) . . ? C3A N3 C2 103.3(5) . . ? C3A N3 Ag 130.0(4) . . ? C2 N3 Ag 126.3(5) . . ? N3 C3A N4 128.9(5) . . ? N3 C3A N8 109.0(6) . . ? N4 C3A N8 122.1(6) . . ? C5 N4 C3A 116.8(5) . . ? C5 N4 Ag 123.7(4) . 3_666 ? C3A N4 Ag 119.5(4) . 3_666 ? O5 C5 N4 115.4(5) . . ? O5 C5 C6 123.2(6) . . ? N4 C5 C6 121.5(6) . . ? C7 C6 C5 120.1(6) . . ? C6 C7 N8 117.3(6) . . ? C7 N8 C3A 122.3(6) . . ? C7 N8 N1 127.9(5) . . ? C3A N8 N1 109.8(5) . . ? O3N N1N O1N 119.3(6) . . ? O3N N1N O2N 122.1(7) . . ? O1N N1N O2N 118.6(6) . . ? N1N O1N Ag 108.3(4) . . ? 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 O5 H5 O2N 0.85(2) 1.78(4) 2.588(8) 157(9) 2_656 #===END data_compound2 _database_code_CSD 157474 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C10 H12 Ag2 Cl2 N8 O12' _chemical_formula_weight 722.92 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' 'Cl' 'Cl' 0.1484 0.1585 '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 5.6419(11) _cell_length_b 8.6644(17) _cell_length_c 11.136(2) _cell_angle_alpha 74.07(3) _cell_angle_beta 81.49(3) _cell_angle_gamma 76.53(3) _cell_volume 507.02(17) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'Flat' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 2.277 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 295(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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2580 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.04 _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.871 _reflns_number_total 2580 _reflns_number_gt 2001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Enraf Nonius)' _computing_cell_refinement 'DENZO-SMN (Enraf Nonius)' _computing_data_reduction 'DENZO-SMN (Enraf Nonius)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (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^)+(0.0700P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 2580 _refine_ls_number_parameters 163 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.214 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.151 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 0.21431(7) 0.54241(5) 0.40481(4) 0.03778(17) Uani 1 1 d . . . N1 N 0.2721(8) 0.9228(6) 0.5810(5) 0.0356(10) Uani 1 1 d . . . C2 C 0.3372(9) 0.8329(6) 0.5008(5) 0.0318(10) Uani 1 1 d . . . H2 H 0.4702 0.8450 0.4413 0.038 Uiso 1 1 d R . . N3 N 0.1987(8) 0.7194(5) 0.5092(4) 0.0304(9) Uani 1 1 d . . . C3A C 0.0338(8) 0.7402(6) 0.6055(5) 0.0255(9) Uani 1 1 d . . . N4 N -0.1498(7) 0.6614(5) 0.6544(4) 0.0271(8) Uani 1 1 d . . . C5 C -0.2905(9) 0.7068(6) 0.7506(5) 0.0283(10) Uani 1 1 d . . . O5 O -0.4645(8) 0.6252(5) 0.7960(4) 0.0437(10) Uani 1 1 d D . . H5 H -0.539(12) 0.654(9) 0.863(4) 0.052 Uiso 1 1 d D . . C6 C -0.2529(10) 0.8345(7) 0.7988(5) 0.0341(11) Uani 1 1 d . . . H6 H -0.3558 0.8645 0.8655 0.041 Uiso 1 1 d R . . C7 C -0.0679(10) 0.9115(6) 0.7469(5) 0.0340(11) Uani 1 1 d . . . H7 H -0.0390 0.9954 0.7764 0.041 Uiso 1 1 d R . . N8 N 0.0748(7) 0.8617(5) 0.6499(4) 0.0281(8) Uani 1 1 d . . . Cl Cl -0.2926(3) 0.7258(2) 0.18600(14) 0.0433(3) Uani 1 1 d . . . O1P O -0.1793(9) 0.6089(7) 0.1158(5) 0.0616(13) Uani 1 1 d . . . O2P O -0.5431(13) 0.7743(11) 0.1753(10) 0.130(4) Uani 1 1 d . . . O3P O -0.282(2) 0.6554(17) 0.3091(7) 0.213(8) Uani 1 1 d . . . O4P O -0.185(3) 0.8510(19) 0.1556(18) 0.285(11) Uani 1 1 d . . . O1W O -0.7360(9) 0.7102(8) 0.9768(5) 0.0594(13) Uani 1 1 d D . . H11W H -0.869(9) 0.675(10) 1.007(7) 0.071 Uiso 1 1 d D . . H12W H -0.679(16) 0.729(11) 1.037(6) 0.071 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 0.0407(3) 0.0392(3) 0.0437(3) -0.0260(2) 0.01053(18) -0.01835(18) N1 0.034(2) 0.040(2) 0.041(2) -0.016(2) 0.0037(19) -0.0198(19) C2 0.030(2) 0.036(3) 0.033(3) -0.011(2) 0.001(2) -0.013(2) N3 0.030(2) 0.031(2) 0.034(2) -0.0140(19) 0.0054(17) -0.0131(17) C3A 0.026(2) 0.023(2) 0.029(2) -0.0101(19) 0.0021(18) -0.0078(17) N4 0.0277(19) 0.0250(19) 0.034(2) -0.0151(18) 0.0054(16) -0.0113(15) C5 0.032(2) 0.028(2) 0.028(2) -0.013(2) 0.0051(19) -0.0092(19) O5 0.047(2) 0.048(2) 0.044(2) -0.024(2) 0.0222(18) -0.0273(18) C6 0.039(3) 0.036(3) 0.031(3) -0.017(2) 0.005(2) -0.008(2) C7 0.045(3) 0.032(3) 0.032(3) -0.018(2) 0.003(2) -0.015(2) N8 0.0263(19) 0.031(2) 0.032(2) -0.0132(18) 0.0004(16) -0.0102(16) Cl 0.0395(7) 0.0573(9) 0.0414(7) -0.0221(7) 0.0040(6) -0.0192(6) O1P 0.053(3) 0.068(3) 0.073(3) -0.038(3) 0.022(2) -0.022(2) O2P 0.079(5) 0.141(7) 0.209(10) -0.135(7) -0.060(6) 0.042(5) O3P 0.224(12) 0.256(14) 0.054(4) -0.039(7) -0.018(6) 0.158(11) O4P 0.289(16) 0.294(16) 0.41(2) -0.298(17) 0.257(16) -0.263(15) O1W 0.043(2) 0.099(4) 0.049(3) -0.037(3) 0.017(2) -0.031(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 Ag N3 2.144(4) . ? Ag N4 2.167(4) 2_566 ? Ag O3P 2.997(12) . ? Ag Ag 3.0559(13) 2_566 ? N1 C2 1.301(7) . ? N1 N8 1.381(6) . ? C2 N3 1.368(6) . ? N3 C3A 1.335(6) . ? C3A N4 1.339(6) . ? C3A N8 1.356(6) . ? N4 C5 1.329(7) . ? N4 Ag 2.167(4) 2_566 ? C5 O5 1.304(6) . ? C5 C6 1.423(7) . ? C6 C7 1.343(8) . ? C7 N8 1.355(7) . ? Cl O4P 1.304(9) . ? Cl O3P 1.342(8) . ? Cl O2P 1.391(7) . ? Cl O1P 1.425(5) . ? 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 N3 Ag N4 162.54(16) . 2_566 ? N3 Ag O3P 100.0(3) . . ? N4 Ag O3P 74.5(3) 2_566 . ? N3 Ag Ag 81.97(12) . 2_566 ? N4 Ag Ag 80.75(11) 2_566 2_566 ? O3P Ag Ag 64.0(2) . 2_566 ? C2 N1 N8 101.9(4) . . ? N1 C2 N3 116.1(5) . . ? C3A N3 C2 102.9(4) . . ? C3A N3 Ag 124.1(3) . . ? C2 N3 Ag 133.0(4) . . ? N3 C3A N4 128.6(4) . . ? N3 C3A N8 109.0(4) . . ? N4 C3A N8 122.4(4) . . ? C5 N4 C3A 116.6(4) . . ? C5 N4 Ag 118.8(3) . 2_566 ? C3A N4 Ag 124.4(3) . 2_566 ? O5 C5 N4 114.4(4) . . ? O5 C5 C6 123.4(5) . . ? N4 C5 C6 122.3(4) . . ? C7 C6 C5 119.4(5) . . ? C6 C7 N8 117.2(5) . . ? C7 N8 C3A 122.1(4) . . ? C7 N8 N1 127.8(4) . . ? C3A N8 N1 110.1(4) . . ? O4P Cl O3P 109.3(11) . . ? O4P Cl O2P 111.7(10) . . ? O3P Cl O2P 102.5(7) . . ? O4P Cl O1P 111.1(5) . . ? O3P Cl O1P 109.8(5) . . ? O2P Cl O1P 112.1(4) . . ? Cl O3P Ag 117.2(7) . . ? 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 O5 H5 O1W 0.87(2) 1.66(3) 2.514(6) 167(7) . O1W H11W O1P 0.86(2) 2.08(3) 2.924(6) 167(8) 1_456 O1W H12W O2P 0.85(2) 1.99(2) 2.837(9) 180(9) 1_556 #===END data_compound3 _database_code_CSD 157475 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C5 H4 Ag Cl N4 O5' _chemical_formula_weight 343.44 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' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'C c' 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' _cell_length_a 6.6046(10) _cell_length_b 14.487(2) _cell_length_c 9.9594(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.379(10) _cell_angle_gamma 90.00 _cell_volume 951.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 4.97 _cell_measurement_theta_max 12.43 _exptl_crystal_description 'needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4279 _exptl_absorpt_correction_T_max 0.9079 _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0200 0.00 -1.00 0.00 0.0200 1.00 0.00 0.00 0.3500 -1.00 0.00 0.00 0.3500 0.00 0.00 1.00 0.2000 0.00 0.00 -1.00 0.2000 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1845 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 29.99 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 1716 _reflns_number_gt 1648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (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^)+(0.0800P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(7) _refine_ls_number_reflns 1716 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.901 _refine_diff_density_min -1.430 _refine_diff_density_rms 0.162 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 0.5000 0.37389(5) 0.5000 0.0469(2) Uani 1 1 d . . . N1 N 0.1619(11) 0.3522(5) 0.4652(7) 0.0354(12) Uani 1 1 d . . . C2 C -0.0040(18) 0.3639(6) 0.5278(7) 0.0389(18) Uani 1 1 d . . . H2 H -0.0046 0.3652 0.6212 0.047 Uiso 1 1 d R . . N3 N -0.1770(13) 0.3729(5) 0.4476(7) 0.0388(14) Uani 1 1 d . . . C3A C -0.1094(11) 0.3631(5) 0.3248(8) 0.0313(13) Uani 1 1 d . . . N4 N -0.2131(13) 0.3652(5) 0.2037(7) 0.0391(15) Uani 1 1 d . . . H4 H -0.3418 0.3748 0.1972 0.047 Uiso 1 1 d R . . C5 C -0.1039(14) 0.3516(7) 0.0911(8) 0.0409(17) Uani 1 1 d . . . H5 H -0.1732 0.3526 0.0071 0.049 Uiso 1 1 d R . . C6 C 0.0957(12) 0.3372(7) 0.0980(8) 0.0405(16) Uani 1 1 d . . . H6 H 0.1611 0.3307 0.0184 0.049 Uiso 1 1 d R . . C7 C 0.2144(10) 0.3321(5) 0.2234(8) 0.0332(14) Uani 1 1 d . . . O7 O 0.3931(9) 0.3141(5) 0.2424(7) 0.0456(14) Uani 1 1 d . . . N8 N 0.0933(9) 0.3511(4) 0.3318(6) 0.0276(10) Uani 1 1 d . . . Cl Cl 0.4515(5) 0.58807(13) 0.3192(2) 0.0455(5) Uani 1 1 d . . . O1P O 0.4839(17) 0.5629(7) 0.4574(7) 0.071(2) Uani 1 1 d . . . O2P O 0.348(3) 0.6678(8) 0.3001(14) 0.111(6) Uani 1 1 d . . . O3P O 0.644(3) 0.602(2) 0.266(2) 0.193(13) Uani 1 1 d . . . O4P O 0.378(5) 0.5170(9) 0.2463(16) 0.194(13) 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 Ag 0.0209(2) 0.0791(4) 0.0408(3) -0.0037(3) 0.00248(18) -0.0029(4) N1 0.016(3) 0.054(3) 0.037(3) -0.001(3) 0.002(2) -0.005(3) C2 0.034(4) 0.052(4) 0.031(5) 0.000(2) 0.006(4) -0.006(4) N3 0.023(3) 0.058(4) 0.035(3) -0.006(2) 0.005(3) 0.004(3) C3A 0.015(3) 0.041(3) 0.038(3) 0.005(2) 0.000(3) -0.001(2) N4 0.025(3) 0.057(4) 0.035(3) 0.003(3) -0.001(3) 0.006(3) C5 0.025(4) 0.066(5) 0.031(3) 0.005(3) -0.001(3) -0.001(3) C6 0.020(3) 0.060(4) 0.042(4) -0.002(3) 0.011(3) -0.002(3) C7 0.010(3) 0.047(3) 0.043(3) 0.000(3) 0.011(2) -0.002(2) O7 0.007(2) 0.070(4) 0.060(4) -0.002(3) 0.009(2) 0.004(2) N8 0.010(2) 0.038(2) 0.035(3) 0.001(2) 0.004(2) -0.0015(19) Cl 0.0631(14) 0.0430(8) 0.0299(7) -0.0007(6) -0.0016(8) 0.0061(10) O1P 0.075(6) 0.103(6) 0.036(3) 0.014(3) -0.003(4) -0.001(6) O2P 0.145(16) 0.071(6) 0.121(10) 0.019(6) 0.033(10) 0.045(8) O3P 0.085(14) 0.39(4) 0.114(14) 0.059(16) 0.063(12) 0.048(17) O4P 0.36(4) 0.086(8) 0.120(10) -0.009(7) -0.119(16) -0.061(15) _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 N3 2.226(8) 1_655 ? Ag N1 2.262(7) . ? Ag O7 2.760(7) . ? Ag O1P 2.772(10) . ? Ag O3P 2.78(2) 2_565 ? N1 C2 1.303(12) . ? N1 N8 1.378(9) . ? C2 N3 1.361(13) . ? N3 C3A 1.334(11) . ? N3 Ag 2.226(8) 1_455 ? C3A N8 1.348(9) . ? C3A N4 1.352(10) . ? N4 C5 1.383(12) . ? C5 C6 1.332(12) . ? C6 C7 1.436(12) . ? C7 O7 1.213(9) . ? C7 N8 1.408(9) . ? Cl O4P 1.334(12) . ? Cl O2P 1.349(11) . ? Cl O3P 1.423(19) . ? Cl O1P 1.427(7) . ? 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 N3 Ag N1 156.1(3) 1_655 . ? N3 Ag O7 88.6(2) 1_655 . ? N1 Ag O7 67.5(2) . . ? N3 Ag O1P 90.0(3) 1_655 . ? N1 Ag O1P 94.9(3) . . ? O7 Ag O1P 99.3(2) . . ? N3 Ag O3P 86.8(4) 1_655 2_565 ? N1 Ag O3P 116.3(4) . 2_565 ? O7 Ag O3P 168.1(6) . 2_565 ? O1P Ag O3P 91.6(6) . 2_565 ? C2 N1 N8 103.0(6) . . ? C2 N1 Ag 139.3(6) . . ? N8 N1 Ag 114.5(5) . . ? N1 C2 N3 115.6(7) . . ? C3A N3 C2 102.3(7) . . ? C3A N3 Ag 126.4(6) . 1_455 ? C2 N3 Ag 130.2(6) . 1_455 ? N3 C3A N8 110.6(7) . . ? N3 C3A N4 129.5(8) . . ? N8 C3A N4 119.9(8) . . ? C3A N4 C5 117.3(8) . . ? C6 C5 N4 122.8(8) . . ? C5 C6 C7 122.7(7) . . ? O7 C7 N8 120.9(8) . . ? O7 C7 C6 128.5(8) . . ? N8 C7 C6 110.6(6) . . ? C7 O7 Ag 105.7(6) . . ? C3A N8 N1 108.5(6) . . ? C3A N8 C7 126.4(7) . . ? N1 N8 C7 124.9(6) . . ? O4P Cl O2P 114.9(13) . . ? O4P Cl O3P 102.0(16) . . ? O2P Cl O3P 106.5(13) . . ? O4P Cl O1P 110.9(8) . . ? O2P Cl O1P 113.6(7) . . ? O3P Cl O1P 108.0(11) . . ? Cl O1P Ag 113.7(5) . . ? 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 N4 H4 O7 0.86 2.03 2.753(10) 140.7 1_455