# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Loeb, Stephen J.' ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; 'Beauchamp, Derek A.' ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_name 'Stephen J. Loeb' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email 'loeb@uwindsor.ca' _publ_requested_journal 'ChemCommun' _publ_requested_coeditor_name ? _publ_contact_letter ; These three structures are part of a study on the coordination chemistry of the ligand 4-(2-pyridyl)-pyrimidine ; _publ_section_title ; Molecular squares, rectangles and infinite helical chains utilizing the simple "corner" ligand 4-(2-pyridyl)-pyrimidine ; data_[AgL]4[BF4]4 L=4-(2-pyridyl)-pyrimidine _database_code_CSD 191503 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Ag4 B4 F16 N12' _chemical_formula_weight 1407.42 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8407(14) _cell_length_b 9.2136(16) _cell_length_c 17.007(3) _cell_angle_alpha 102.984(3) _cell_angle_beta 94.837(3) _cell_angle_gamma 101.366(3) _cell_volume 1163.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.036253 _exptl_absorpt_correction_T_max 0.058390 _exptl_absorpt_process_details ? _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 APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 4067 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 20.81 _reflns_number_total 2402 _reflns_number_gt 2291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.1957P)^2^+1.7409P] 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 0.035(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2402 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2396 _refine_ls_wR_factor_gt 0.2352 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Ag1 Ag -0.28972(10) 1.04621(8) 0.24186(5) 0.0717(7) Uani 1 1 d . . . Ag2 Ag -0.11275(11) 1.37640(9) 0.62124(4) 0.0762(7) Uani 1 1 d . . . N1 N -0.3993(10) 1.2309(10) 0.2001(5) 0.059(2) Uani 1 1 d . . . N2 N -0.2856(10) 1.2445(8) 0.3573(4) 0.0552(19) Uani 1 1 d . . . N3 N -0.2135(10) 1.3702(9) 0.4992(5) 0.062(2) Uani 1 1 d . . . N4 N -0.0780(10) 1.5829(9) 0.7376(5) 0.059(2) Uani 1 1 d . . . N5 N 0.0396(9) 1.3245(8) 0.7276(4) 0.0527(19) Uani 1 1 d . . . N6 N 0.1742(9) 1.1539(8) 0.7835(4) 0.0551(19) Uani 1 1 d . . . C1 C -0.4545(13) 1.2214(14) 0.1212(6) 0.070(3) Uani 1 1 d . . . H1A H -0.4480 1.1352 0.0819 0.084 Uiso 1 1 calc R . . C2 C -0.5190(14) 1.3334(14) 0.0976(7) 0.075(3) Uani 1 1 d . . . H2A H -0.5534 1.3237 0.0426 0.090 Uiso 1 1 calc R . . C3 C -0.5338(13) 1.4590(15) 0.1532(7) 0.078(4) Uani 1 1 d . . . H3A H -0.5801 1.5352 0.1374 0.093 Uiso 1 1 calc R . . C4 C -0.4754(11) 1.4715(11) 0.2383(6) 0.061(2) Uani 1 1 d . . . H4A H -0.4828 1.5557 0.2789 0.073 Uiso 1 1 calc R . . C5 C -0.4108(11) 1.3571(10) 0.2558(5) 0.053(2) Uani 1 1 d . . . C6 C -0.3399(11) 1.3648(10) 0.3422(6) 0.049(2) Uani 1 1 d . . . C7 C -0.3287(15) 1.4958(11) 0.4049(6) 0.068(3) Uani 1 1 d . . . H7A H -0.3639 1.5813 0.3949 0.081 Uiso 1 1 calc R . . C8 C -0.2648(16) 1.4922(11) 0.4801(7) 0.073(3) Uani 1 1 d . . . H8A H -0.2550 1.5791 0.5219 0.088 Uiso 1 1 calc R . . C9 C -0.2226(12) 1.2511(11) 0.4331(6) 0.060(2) Uani 1 1 d . . . H9A H -0.1809 1.1677 0.4422 0.071 Uiso 1 1 calc R . . C10 C -0.1253(13) 1.7122(11) 0.7386(6) 0.063(3) Uani 1 1 d . . . H10A H -0.1712 1.7283 0.6899 0.076 Uiso 1 1 calc R . . C11 C -0.1088(14) 1.8288(10) 0.8115(8) 0.079(4) Uani 1 1 d . . . H11A H -0.1419 1.9200 0.8106 0.094 Uiso 1 1 calc R . . C12 C -0.0453(13) 1.8040(12) 0.8804(7) 0.068(3) Uani 1 1 d . . . H12A H -0.0349 1.8777 0.9290 0.081 Uiso 1 1 calc R . . C13 C 0.0068(13) 1.6661(11) 0.8806(7) 0.066(3) Uani 1 1 d . . . H13A H 0.0515 1.6470 0.9287 0.079 Uiso 1 1 calc R . . C14 C -0.0106(10) 1.5611(9) 0.8076(5) 0.047(2) Uani 1 1 d . . . C15 C 0.0509(10) 1.4154(9) 0.8035(5) 0.049(2) Uani 1 1 d . . . C16 C 0.1209(12) 1.3773(11) 0.8676(5) 0.062(2) Uani 1 1 d . . . H16A H 0.1291 1.4397 0.9197 0.074 Uiso 1 1 calc R . . C17 C 0.1820(12) 1.2425(11) 0.8562(6) 0.060(2) Uani 1 1 d . . . H17A H 0.2294 1.2152 0.9013 0.072 Uiso 1 1 calc R . . C18 C 0.0992(13) 1.1984(11) 0.7215(6) 0.065(3) Uani 1 1 d . . . H18A H 0.0883 1.1346 0.6696 0.078 Uiso 1 1 calc R . . B1 B 0.2492(16) 1.0979(14) 0.4510(10) 0.080(4) Uani 1 1 d . . . B2 B -0.3015(15) 1.1942(12) 0.9059(7) 0.065(3) Uani 1 1 d . . . F1 F 0.221(3) 1.1308(15) 0.5328(8) 0.225(7) Uani 1 1 d . . . F2 F 0.2328(18) 0.9487(10) 0.4309(8) 0.170(4) Uani 1 1 d . . . F3 F 0.1032(13) 1.1334(12) 0.4159(8) 0.160(4) Uani 1 1 d . . . F4 F 0.3762(15) 1.1959(15) 0.4414(11) 0.178(6) Uani 1 1 d . . . F5 F -0.2827(12) 1.1695(10) 0.8262(4) 0.118(3) Uani 1 1 d . . . F6 F -0.4758(8) 1.1487(8) 0.9162(4) 0.097(2) Uani 1 1 d . . . F7 F -0.2052(12) 1.1141(9) 0.9424(5) 0.107(2) Uani 1 1 d . . . F8 F -0.2415(10) 1.3493(7) 0.9446(4) 0.0882(19) 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 0.0890(9) 0.0548(9) 0.0731(9) 0.0062(5) 0.0043(5) 0.0343(5) Ag2 0.1020(10) 0.0700(9) 0.0517(8) 0.0115(5) -0.0083(5) 0.0197(5) N1 0.061(4) 0.060(5) 0.055(5) 0.014(4) -0.001(4) 0.014(3) N2 0.070(4) 0.045(4) 0.052(5) 0.005(3) 0.010(4) 0.024(4) N3 0.070(5) 0.060(5) 0.057(5) 0.009(4) 0.011(4) 0.022(4) N4 0.065(4) 0.056(5) 0.055(5) 0.015(4) 0.006(4) 0.015(4) N5 0.064(4) 0.040(4) 0.049(5) 0.002(4) 0.001(3) 0.015(3) N6 0.066(4) 0.050(4) 0.052(5) 0.012(4) 0.005(3) 0.021(3) C1 0.075(6) 0.086(8) 0.053(7) 0.026(6) 0.003(5) 0.022(6) C2 0.082(7) 0.088(8) 0.054(6) 0.013(6) 0.008(5) 0.021(6) C3 0.063(6) 0.107(10) 0.092(9) 0.070(8) 0.009(5) 0.034(6) C4 0.056(5) 0.053(5) 0.077(7) 0.019(5) 0.008(4) 0.015(4) C5 0.059(5) 0.047(5) 0.053(5) 0.015(5) 0.007(4) 0.013(4) C6 0.051(5) 0.042(5) 0.055(6) 0.010(4) 0.003(4) 0.015(4) C7 0.104(7) 0.051(6) 0.057(6) 0.013(5) 0.001(5) 0.041(5) C8 0.109(8) 0.046(6) 0.057(7) -0.003(5) -0.003(6) 0.025(5) C9 0.071(6) 0.051(5) 0.059(7) 0.010(5) 0.003(5) 0.026(4) C10 0.079(6) 0.057(6) 0.063(6) 0.018(5) 0.014(5) 0.030(5) C11 0.077(7) 0.037(6) 0.131(13) 0.011(7) 0.037(7) 0.036(5) C12 0.076(6) 0.057(6) 0.069(7) 0.004(5) 0.000(5) 0.028(5) C13 0.072(6) 0.056(6) 0.068(7) 0.008(5) 0.012(5) 0.016(5) C14 0.043(4) 0.043(5) 0.050(6) 0.001(4) 0.007(4) 0.010(4) C15 0.053(5) 0.043(5) 0.051(6) 0.012(4) 0.008(4) 0.010(4) C16 0.067(5) 0.068(6) 0.045(5) 0.005(5) 0.002(4) 0.016(5) C17 0.069(6) 0.061(6) 0.053(6) 0.012(5) 0.007(4) 0.029(5) C18 0.074(6) 0.060(6) 0.058(6) 0.007(5) 0.003(4) 0.019(5) B1 0.055(7) 0.056(8) 0.127(12) 0.022(7) -0.006(7) 0.017(6) B2 0.077(8) 0.053(7) 0.066(8) 0.007(5) -0.003(5) 0.033(5) F1 0.34(2) 0.169(11) 0.117(8) -0.001(7) 0.034(10) -0.008(12) F2 0.230(12) 0.076(6) 0.214(11) 0.038(6) 0.037(9) 0.051(6) F3 0.122(7) 0.141(8) 0.239(12) 0.079(8) 0.027(7) 0.044(6) F4 0.107(7) 0.160(10) 0.283(18) 0.069(10) 0.055(8) 0.037(7) F5 0.147(7) 0.131(7) 0.061(5) 0.010(4) 0.012(4) 0.013(5) F6 0.070(4) 0.098(5) 0.113(5) 0.001(4) 0.014(3) 0.019(3) F7 0.129(6) 0.096(5) 0.098(5) 0.012(4) -0.018(4) 0.060(4) F8 0.113(5) 0.061(4) 0.087(5) 0.018(3) -0.006(4) 0.019(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 Ag1 N6 2.184(7) 2_576 ? Ag1 N1 2.270(8) . ? Ag1 N2 2.356(7) . ? Ag2 N3 2.141(8) . ? Ag2 N5 2.276(7) . ? Ag2 N4 2.372(8) . ? N1 C5 1.349(12) . ? N1 C1 1.353(13) . ? N2 C9 1.325(12) . ? N2 C6 1.331(12) . ? N3 C8 1.361(13) . ? N3 C9 1.369(12) . ? N4 C10 1.312(13) . ? N4 C14 1.334(12) . ? N5 C18 1.322(12) . ? N5 C15 1.356(11) . ? N6 C17 1.309(12) . ? N6 C18 1.347(13) . ? N6 Ag1 2.184(7) 2_576 ? C1 C2 1.357(17) . ? C2 C3 1.352(17) . ? C3 C4 1.453(15) . ? C4 C5 1.335(13) . ? C5 C6 1.508(13) . ? C6 C7 1.402(14) . ? C7 C8 1.343(16) . ? C10 C11 1.424(16) . ? C11 C12 1.319(15) . ? C12 C13 1.410(15) . ? C13 C14 1.369(14) . ? C14 C15 1.503(13) . ? C15 C16 1.328(13) . ? C16 C17 1.396(13) . ? B1 F4 1.254(16) . ? B1 F2 1.317(16) . ? B1 F3 1.376(16) . ? B1 F1 1.402(19) . ? B2 F5 1.349(14) . ? B2 F7 1.359(14) . ? B2 F6 1.386(14) . ? B2 F8 1.399(13) . ? 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 N6 Ag1 N1 150.8(3) 2_576 . ? N6 Ag1 N2 135.3(3) 2_576 . ? N1 Ag1 N2 71.8(3) . . ? N3 Ag2 N5 160.8(3) . . ? N3 Ag2 N4 126.8(3) . . ? N5 Ag2 N4 70.8(3) . . ? C5 N1 C1 117.5(9) . . ? C5 N1 Ag1 119.3(6) . . ? C1 N1 Ag1 123.2(8) . . ? C9 N2 C6 118.4(8) . . ? C9 N2 Ag1 126.1(6) . . ? C6 N2 Ag1 115.3(6) . . ? C8 N3 C9 113.6(8) . . ? C8 N3 Ag2 121.6(6) . . ? C9 N3 Ag2 124.7(7) . . ? C10 N4 C14 118.5(8) . . ? C10 N4 Ag2 125.3(7) . . ? C14 N4 Ag2 116.2(6) . . ? C18 N5 C15 117.1(8) . . ? C18 N5 Ag2 123.1(6) . . ? C15 N5 Ag2 119.2(5) . . ? C17 N6 C18 115.9(8) . . ? C17 N6 Ag1 124.3(6) . 2_576 ? C18 N6 Ag1 119.7(6) . 2_576 ? N1 C1 C2 122.3(11) . . ? C3 C2 C1 120.6(10) . . ? C2 C3 C4 118.1(10) . . ? C5 C4 C3 117.2(10) . . ? C4 C5 N1 124.4(9) . . ? C4 C5 C6 120.4(8) . . ? N1 C5 C6 115.2(8) . . ? N2 C6 C7 120.7(8) . . ? N2 C6 C5 118.2(8) . . ? C7 C6 C5 121.1(8) . . ? C8 C7 C6 117.0(9) . . ? C7 C8 N3 124.5(9) . . ? N2 C9 N3 125.6(9) . . ? N4 C10 C11 122.5(9) . . ? C12 C11 C10 118.2(9) . . ? C11 C12 C13 120.2(9) . . ? C14 C13 C12 117.8(10) . . ? N4 C14 C13 122.8(8) . . ? N4 C14 C15 117.0(7) . . ? C13 C14 C15 120.2(8) . . ? C16 C15 N5 120.2(8) . . ? C16 C15 C14 124.2(8) . . ? N5 C15 C14 115.5(7) . . ? C15 C16 C17 119.3(9) . . ? N6 C17 C16 121.5(8) . . ? N5 C18 N6 125.8(9) . . ? F4 B1 F2 126.2(14) . . ? F4 B1 F3 104.8(12) . . ? F2 B1 F3 109.3(13) . . ? F4 B1 F1 109.4(14) . . ? F2 B1 F1 104.2(13) . . ? F3 B1 F1 100.0(13) . . ? F5 B2 F7 109.8(9) . . ? F5 B2 F6 111.0(9) . . ? F7 B2 F6 108.7(10) . . ? F5 B2 F8 110.3(9) . . ? F7 B2 F8 108.2(8) . . ? F6 B2 F8 108.9(8) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.489 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.183 #===END data_[AgL]4[CF3SO3]4L=4-(2-pyridyl)-pyrimidine _database_code_CSD 191504 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Ag4 F12 N12 O12 S4' _chemical_formula_weight 1656.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1267(13) _cell_length_b 10.4529(14) _cell_length_c 13.5037(19) _cell_angle_alpha 81.403(2) _cell_angle_beta 72.533(2) _cell_angle_gamma 89.410(2) _cell_volume 1347.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.046101 _exptl_absorpt_correction_T_max 0.066283 _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 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5794 _diffrn_reflns_av_R_equivalents 0.0091 _diffrn_reflns_av_sigmaI/netI 0.0113 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3843 _reflns_number_gt 3361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0821P)^2^+4.1309P] 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 3843 _refine_ls_number_parameters 379 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.490 _refine_ls_shift/su_mean 0.032 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 0.06808(6) 0.75914(5) 0.24990(4) 0.0674(2) Uani 1 1 d . . . Ag2 Ag 0.38429(6) 0.25172(5) 0.12865(4) 0.0653(2) Uani 1 1 d . . . N1 N 0.1951(5) 0.3335(5) 0.2232(4) 0.0537(12) Uani 1 1 d . . . N2 N 0.0817(5) 0.5258(5) 0.2675(4) 0.0539(13) Uani 1 1 d . . . N3 N -0.1041(6) 0.6607(6) 0.3989(4) 0.0646(15) Uani 1 1 d . . . N4 N 0.4379(6) 0.8574(5) -0.0484(4) 0.0574(13) Uani 1 1 d . . . N5 N 0.2289(6) 0.8591(5) 0.0900(4) 0.0557(13) Uani 1 1 d . . . N6 N -0.0103(6) 0.9663(6) 0.1884(5) 0.0765(18) Uani 1 1 d . . . C1 C 0.1776(7) 0.4598(7) 0.2073(5) 0.0593(17) Uani 1 1 d . . . H1A H 0.2388 0.5071 0.1477 0.071 Uiso 1 1 calc R A . C2 C 0.1014(7) 0.2666(7) 0.3073(6) 0.0611(17) Uani 1 1 d . . . H2A H 0.1084 0.1774 0.3218 0.073 Uiso 1 1 calc R A . C3 C -0.0032(7) 0.3253(6) 0.3718(5) 0.0577(16) Uani 1 1 d . . . H3A H -0.0692 0.2769 0.4278 0.069 Uiso 1 1 calc R . . C4 C -0.0095(6) 0.4575(6) 0.3523(4) 0.0442(13) Uani 1 1 d . . . C5 C -0.1154(6) 0.5318(6) 0.4220(5) 0.0484(14) Uani 1 1 d . . . C6 C -0.2167(8) 0.4693(8) 0.5073(6) 0.071(2) Uani 1 1 d . . . H6A H -0.2207 0.3794 0.5228 0.086 Uiso 1 1 calc R A . C7 C -0.3124(9) 0.5412(11) 0.5699(7) 0.091(3) Uani 1 1 d . . . H7A H -0.3825 0.5004 0.6274 0.109 Uiso 1 1 calc R . . C8 C -0.3031(9) 0.6729(11) 0.5465(7) 0.087(3) Uani 1 1 d . . . H8A H -0.3665 0.7235 0.5873 0.104 Uiso 1 1 calc R A . C9 C -0.1978(10) 0.7287(9) 0.4612(7) 0.087(3) Uani 1 1 d . . . H9A H -0.1909 0.8186 0.4458 0.105 Uiso 1 1 calc R . . C10 C 0.3435(7) 0.8046(6) 0.0409(5) 0.0596(17) Uani 1 1 d . . . H10A H 0.3600 0.7224 0.0711 0.072 Uiso 1 1 calc R . . C12 C 0.2978(8) 1.0388(6) -0.0409(6) 0.0640(18) Uani 1 1 d . . . H12A H 0.2835 1.1226 -0.0692 0.077 Uiso 1 1 calc R . . C13 C 0.4128(7) 0.9760(7) -0.0879(6) 0.0639(18) Uani 1 1 d . . . H13A H 0.4756 1.0174 -0.1495 0.077 Uiso 1 1 calc R . . C11 C 0.2040(7) 0.9774(5) 0.0484(5) 0.0482(14) Uani 1 1 d . . . C14 C 0.0727(7) 1.0370(6) 0.1034(5) 0.0519(15) Uani 1 1 d . . . C15 C 0.0390(8) 1.1601(7) 0.0670(6) 0.0686(19) Uani 1 1 d . . . H15A H 0.0990 1.2081 0.0071 0.082 Uiso 1 1 calc R . . C16 C -0.0824(9) 1.2113(8) 0.1191(8) 0.082(2) Uani 1 1 d . . . H16A H -0.1058 1.2940 0.0953 0.098 Uiso 1 1 calc R . . C17 C -0.1679(9) 1.1390(10) 0.2060(8) 0.092(3) Uani 1 1 d . . . H17A H -0.2507 1.1714 0.2436 0.110 Uiso 1 1 calc R . . C18 C -0.1301(9) 1.0180(10) 0.2369(8) 0.099(3) Uani 1 1 d . . . H18A H -0.1909 0.9679 0.2953 0.119 Uiso 1 1 calc R . . S2 S 0.37418(18) 0.47754(17) -0.11052(13) 0.0577(4) Uani 1 1 d D A -1 O4 O 0.5101(7) 0.5178(11) -0.1678(6) 0.167(5) Uani 1 1 d D A -1 O5 O 0.2945(9) 0.5650(7) -0.0521(6) 0.127(3) Uani 1 1 d D A -1 O6 O 0.3620(9) 0.3501(6) -0.0533(6) 0.125(3) Uani 1 1 d D A -1 C20 C 0.2902(9) 0.4598(8) -0.2045(6) 0.082(2) Uani 1 1 d D A -1 F4 F 0.1644(8) 0.4331(13) -0.1646(7) 0.214(6) Uani 1 1 d D A -1 F5 F 0.2860(12) 0.5630(8) -0.2651(6) 0.179(4) Uani 1 1 d D A -1 F6 F 0.3486(10) 0.3785(8) -0.2668(6) 0.171(4) Uani 1 1 d D A -1 S1 S 0.2719(2) 0.9289(2) 0.3666(2) 0.0951(8) Uani 1 1 d D B -1 O1 O 0.3056(7) 1.0240(6) 0.2779(5) 0.106(2) Uani 1 1 d D B -1 O2 O 0.2070(14) 0.8179(9) 0.3685(10) 0.275(10) Uani 1 1 d D B -1 O3 O 0.2093(19) 0.9874(12) 0.4619(8) 0.44(2) Uani 1 1 d D B -1 C19 C 0.4273(10) 0.8823(12) 0.3919(10) 0.216(13) Uani 1 1 d D B -1 F1 F 0.4982(16) 0.828(2) 0.3189(11) 0.58(3) Uani 1 1 d D B -1 F2 F 0.5048(14) 0.9733(16) 0.3879(16) 0.365(15) Uani 1 1 d D B -1 F3 F 0.4045(9) 0.8089(9) 0.4829(7) 0.183(4) Uani 1 1 d D B -1 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 0.0687(4) 0.0523(3) 0.0665(4) 0.0078(3) -0.0065(3) 0.0013(3) Ag2 0.0587(4) 0.0663(4) 0.0644(4) -0.0183(3) -0.0054(3) 0.0141(3) N1 0.055(3) 0.050(3) 0.050(3) -0.006(2) -0.006(2) 0.007(2) N2 0.051(3) 0.051(3) 0.048(3) -0.001(2) -0.001(2) 0.007(2) N3 0.075(4) 0.060(4) 0.050(3) -0.006(3) -0.007(3) 0.017(3) N4 0.055(3) 0.054(3) 0.056(3) -0.007(3) -0.007(3) 0.004(2) N5 0.062(3) 0.045(3) 0.051(3) -0.002(2) -0.007(3) 0.007(2) N6 0.056(3) 0.068(4) 0.085(4) 0.008(3) -0.001(3) 0.017(3) C1 0.059(4) 0.058(4) 0.046(3) -0.001(3) 0.002(3) 0.003(3) C2 0.063(4) 0.047(4) 0.067(4) -0.005(3) -0.013(4) 0.008(3) C3 0.052(4) 0.055(4) 0.054(4) 0.005(3) -0.005(3) -0.003(3) C4 0.040(3) 0.049(3) 0.040(3) -0.003(3) -0.009(2) 0.001(2) C5 0.045(3) 0.057(4) 0.043(3) -0.007(3) -0.013(3) 0.006(3) C6 0.065(4) 0.066(4) 0.066(4) -0.009(4) 0.006(4) -0.005(4) C7 0.058(5) 0.124(8) 0.070(5) -0.020(5) 0.015(4) -0.003(5) C8 0.072(5) 0.116(8) 0.065(5) -0.028(5) -0.004(4) 0.033(5) C9 0.102(6) 0.083(6) 0.068(5) -0.018(4) -0.012(5) 0.035(5) C10 0.063(4) 0.047(4) 0.058(4) -0.004(3) -0.004(3) 0.012(3) C12 0.076(5) 0.040(3) 0.067(4) 0.004(3) -0.015(4) 0.008(3) C13 0.063(4) 0.052(4) 0.062(4) 0.003(3) -0.002(3) -0.003(3) C11 0.057(4) 0.038(3) 0.050(3) -0.006(3) -0.016(3) 0.005(3) C14 0.053(4) 0.044(3) 0.060(4) -0.012(3) -0.017(3) 0.009(3) C15 0.075(5) 0.048(4) 0.078(5) -0.006(3) -0.018(4) 0.013(3) C16 0.083(6) 0.060(5) 0.107(7) -0.019(5) -0.033(5) 0.026(4) C17 0.065(5) 0.097(7) 0.110(7) -0.025(6) -0.016(5) 0.035(5) C18 0.070(5) 0.095(7) 0.101(7) 0.002(5) 0.012(5) 0.022(5) S2 0.0580(10) 0.0605(10) 0.0564(9) -0.0088(8) -0.0200(8) 0.0058(8) O4 0.080(5) 0.298(14) 0.107(6) -0.042(7) 0.001(4) -0.060(7) O5 0.185(8) 0.119(6) 0.111(5) -0.061(5) -0.076(6) 0.075(6) O6 0.210(9) 0.071(4) 0.120(5) 0.011(4) -0.100(6) 0.002(5) C20 0.086(6) 0.090(6) 0.084(6) -0.016(5) -0.044(5) 0.019(5) F4 0.091(5) 0.413(18) 0.150(7) -0.034(9) -0.058(5) -0.052(7) F5 0.302(12) 0.151(7) 0.126(6) -0.005(5) -0.135(8) 0.053(7) F6 0.224(9) 0.185(8) 0.174(7) -0.123(7) -0.122(7) 0.087(7) S1 0.0740(13) 0.0691(13) 0.1186(19) 0.0322(13) -0.0157(13) -0.0079(11) O1 0.095(4) 0.070(4) 0.113(5) 0.029(3) 0.005(4) 0.015(3) O2 0.43(2) 0.155(9) 0.341(17) 0.128(10) -0.332(17) -0.150(12) O3 0.74(5) 0.190(13) 0.160(11) -0.031(10) 0.196(19) 0.16(2) C19 0.159(15) 0.205(18) 0.27(3) 0.145(19) -0.133(18) -0.087(15) F1 0.32(2) 0.73(5) 0.39(3) 0.27(3) 0.16(2) 0.37(3) F2 0.230(14) 0.42(2) 0.44(3) 0.22(2) -0.231(17) -0.210(17) F3 0.176(8) 0.209(9) 0.172(7) 0.070(7) -0.112(7) -0.048(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.337(6) . ? Ag1 N5 2.378(5) . ? Ag1 N6 2.415(6) . ? Ag1 N2 2.422(5) . ? Ag2 N1 2.203(5) . ? Ag2 N4 2.207(5) 2_665 ? Ag2 O6 2.592(6) . ? N1 C1 1.324(8) . ? N1 C2 1.345(9) . ? N2 C1 1.326(8) . ? N2 C4 1.345(8) . ? N3 C5 1.335(9) . ? N3 C9 1.342(10) . ? N4 C10 1.339(8) . ? N4 C13 1.328(9) . ? N4 Ag2 2.207(5) 2_665 ? N5 C10 1.322(8) . ? N5 C11 1.334(8) . ? N6 C14 1.323(9) . ? N6 C18 1.345(10) . ? C2 C3 1.360(10) . ? C3 C4 1.372(9) . ? C4 C5 1.495(8) . ? C5 C6 1.373(10) . ? C6 C7 1.380(12) . ? C7 C8 1.363(14) . ? C8 C9 1.370(13) . ? C12 C13 1.363(10) . ? C12 C11 1.364(9) . ? C11 C14 1.495(9) . ? C14 C15 1.384(9) . ? C15 C16 1.368(11) . ? C16 C17 1.355(13) . ? C17 C18 1.359(13) . ? S2 O4 1.394(6) . ? S2 O5 1.388(6) . ? S2 O6 1.423(6) . ? S2 C20 1.757(8) . ? C20 F4 1.241(10) . ? C20 F5 1.261(10) . ? C20 F6 1.298(9) . ? S1 O2 1.333(7) . ? S1 O1 1.394(6) . ? S1 O3 1.473(8) . ? S1 C19 1.757(9) . ? C19 F2 1.224(12) . ? C19 F1 1.240(13) . ? C19 F3 1.306(10) . ? F1 F2 1.905(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N5 175.0(2) . . ? N3 Ag1 N6 108.7(2) . . ? N5 Ag1 N6 68.87(19) . . ? N3 Ag1 N2 69.53(18) . . ? N5 Ag1 N2 110.58(17) . . ? N6 Ag1 N2 154.5(2) . . ? N1 Ag2 N4 171.7(2) . 2_665 ? N1 Ag2 O6 96.4(2) . . ? N4 Ag2 O6 89.0(2) 2_665 . ? C1 N1 C2 115.4(5) . . ? C1 N1 Ag2 119.7(4) . . ? C2 N1 Ag2 124.3(4) . . ? C1 N2 C4 117.0(5) . . ? C1 N2 Ag1 126.4(4) . . ? C4 N2 Ag1 116.3(4) . . ? C5 N3 C9 117.6(7) . . ? C5 N3 Ag1 119.9(4) . . ? C9 N3 Ag1 122.5(6) . . ? C10 N4 C13 115.5(6) . . ? C10 N4 Ag2 121.7(4) . 2_665 ? C13 N4 Ag2 122.7(4) . 2_665 ? C10 N5 C11 118.0(5) . . ? C10 N5 Ag1 123.4(4) . . ? C11 N5 Ag1 118.5(4) . . ? C14 N6 C18 117.2(7) . . ? C14 N6 Ag1 118.0(4) . . ? C18 N6 Ag1 124.7(6) . . ? N1 C1 N2 126.8(6) . . ? N1 C2 C3 122.0(6) . . ? C2 C3 C4 118.6(6) . . ? N2 C4 C3 120.1(5) . . ? N2 C4 C5 117.2(5) . . ? C3 C4 C5 122.7(5) . . ? N3 C5 C6 122.1(6) . . ? N3 C5 C4 116.9(5) . . ? C6 C5 C4 121.0(6) . . ? C5 C6 C7 119.3(8) . . ? C8 C7 C6 119.2(8) . . ? C7 C8 C9 118.3(8) . . ? N3 C9 C8 123.5(9) . . ? N5 C10 N4 125.7(6) . . ? C13 C12 C11 119.2(6) . . ? N4 C13 C12 122.0(6) . . ? N5 C11 C12 119.5(6) . . ? N5 C11 C14 117.5(5) . . ? C12 C11 C14 123.0(6) . . ? N6 C14 C15 121.4(6) . . ? N6 C14 C11 116.9(5) . . ? C15 C14 C11 121.7(6) . . ? C16 C15 C14 120.1(8) . . ? C17 C16 C15 118.7(8) . . ? C16 C17 C18 118.5(8) . . ? N6 C18 C17 124.0(9) . . ? O4 S2 O5 116.7(6) . . ? O4 S2 O6 113.7(6) . . ? O5 S2 O6 112.8(5) . . ? O4 S2 C20 105.6(4) . . ? O5 S2 C20 103.7(4) . . ? O6 S2 C20 102.4(4) . . ? S2 O6 Ag2 134.6(4) . . ? F4 C20 F5 100.1(9) . . ? F4 C20 F6 110.9(9) . . ? F5 C20 F6 104.6(8) . . ? F4 C20 S2 112.7(7) . . ? F5 C20 S2 114.2(7) . . ? F6 C20 S2 113.3(6) . . ? O2 S1 O1 121.4(6) . . ? O2 S1 O3 112.0(7) . . ? O1 S1 O3 110.3(6) . . ? O2 S1 C19 104.7(5) . . ? O1 S1 C19 107.5(4) . . ? O3 S1 C19 98.1(7) . . ? F2 C19 F1 101.3(11) . . ? F2 C19 F3 108.7(10) . . ? F1 C19 F3 111.9(12) . . ? F2 C19 S1 113.9(9) . . ? F1 C19 S1 108.9(9) . . ? F3 C19 S1 111.7(7) . . ? C19 F1 F2 39.0(6) . . ? C19 F2 F1 39.7(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.272 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.109 #===END data_[AgL][NO3]-polymer L=4-(2-pyridyl)-pyrimidine _database_code_CSD 191505 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H7 Ag N4 O3' _chemical_formula_weight 327.06 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.432(2) _cell_length_b 10.860(5) _cell_length_c 18.009(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.486(6) _cell_angle_gamma 90.00 _cell_volume 1050.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.920 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.085055 _exptl_absorpt_correction_T_max 0.145189 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 4381 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1490 _reflns_number_gt 1408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0394P)^2^+1.4361P] 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 1490 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Ag1 Ag -0.00436(7) 0.95099(3) 0.775873(18) 0.06495(18) Uani 1 1 d . . . N1 N 0.0490(5) 0.7812(3) 0.69921(16) 0.0413(7) Uani 1 1 d . . . N2 N 0.2589(6) 0.5994(3) 0.67317(17) 0.0475(7) Uani 1 1 d . . . N3 N -0.2891(6) 0.9626(3) 0.66262(18) 0.0497(8) Uani 1 1 d . . . N4 N -0.2774(7) 0.8318(3) 0.8940(2) 0.0589(9) Uani 1 1 d . . . O1 O -0.3454(7) 0.8437(4) 0.82578(19) 0.0885(11) Uani 1 1 d . . . O2 O -0.0739(8) 0.8717(4) 0.9199(2) 0.1012(13) Uani 1 1 d . . . O3 O -0.4132(8) 0.7830(4) 0.9336(2) 0.0989(13) Uani 1 1 d . . . C1 C 0.2275(7) 0.6988(3) 0.7135(2) 0.0460(9) Uani 1 1 d . . . H1A H 0.3435 0.7117 0.7562 0.055 Uiso 1 1 calc R . . C2 C 0.0931(8) 0.5841(4) 0.6113(2) 0.0527(10) Uani 1 1 d . . . H2A H 0.1088 0.5163 0.5807 0.063 Uiso 1 1 calc R . . C3 C -0.0983(7) 0.6643(3) 0.5914(2) 0.0492(9) Uani 1 1 d . . . H3A H -0.2113 0.6523 0.5479 0.059 Uiso 1 1 calc R . . C4 C -0.1195(6) 0.7641(3) 0.63776(19) 0.0405(8) Uani 1 1 d . . . C5 C -0.3192(7) 0.8588(3) 0.62153(19) 0.0411(8) Uani 1 1 d . . . C6 C -0.5229(7) 0.8407(4) 0.5675(2) 0.0499(9) Uani 1 1 d . . . H6A H -0.5397 0.7684 0.5396 0.060 Uiso 1 1 calc R . . C7 C -0.7018(8) 0.9316(4) 0.5553(3) 0.0610(11) Uani 1 1 d . . . H7A H -0.8413 0.9207 0.5193 0.073 Uiso 1 1 calc R . . C8 C -0.6730(9) 1.0371(4) 0.5965(3) 0.0652(12) Uani 1 1 d . . . H8A H -0.7926 1.0990 0.5894 0.078 Uiso 1 1 calc R . . C9 C -0.4625(9) 1.0501(4) 0.6487(3) 0.0598(11) Uani 1 1 d . . . H9A H -0.4401 1.1233 0.6757 0.072 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 Ag1 0.0737(3) 0.0618(3) 0.0589(3) -0.02046(15) 0.00816(18) -0.02081(16) N1 0.0441(16) 0.0385(16) 0.0395(15) -0.0004(13) 0.0001(13) -0.0008(13) N2 0.0526(18) 0.0401(17) 0.0486(18) 0.0045(14) 0.0033(15) 0.0040(14) N3 0.056(2) 0.0446(18) 0.0480(18) -0.0015(14) 0.0070(15) 0.0019(15) N4 0.062(2) 0.0501(19) 0.065(2) 0.0049(17) 0.0106(19) 0.0014(17) O1 0.094(3) 0.111(3) 0.057(2) 0.0030(19) 0.0009(18) -0.026(2) O2 0.087(3) 0.103(3) 0.102(3) 0.022(2) -0.022(2) -0.037(2) O3 0.091(3) 0.110(3) 0.103(3) 0.035(2) 0.037(2) -0.007(2) C1 0.048(2) 0.047(2) 0.0402(19) 0.0051(16) -0.0005(15) -0.0028(18) C2 0.063(2) 0.042(2) 0.051(2) -0.0053(18) 0.0035(19) 0.0017(19) C3 0.056(2) 0.045(2) 0.043(2) -0.0049(16) -0.0060(17) 0.0022(18) C4 0.0437(19) 0.0406(19) 0.0368(18) 0.0038(15) 0.0044(15) -0.0049(15) C5 0.046(2) 0.0400(19) 0.0393(18) 0.0050(15) 0.0109(15) -0.0010(16) C6 0.047(2) 0.053(2) 0.049(2) 0.0034(17) 0.0035(17) -0.0019(18) C7 0.047(2) 0.069(3) 0.064(3) 0.012(2) 0.001(2) 0.007(2) C8 0.057(3) 0.067(3) 0.074(3) 0.014(2) 0.016(2) 0.020(2) C9 0.070(3) 0.050(2) 0.062(3) 0.0009(19) 0.019(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.204(3) 2_556 ? Ag1 N1 2.347(3) . ? Ag1 N3 2.374(3) . ? Ag1 O1 2.468(4) . ? N1 C1 1.316(5) . ? N1 C4 1.341(5) . ? N2 C1 1.326(5) . ? N2 C2 1.336(5) . ? N2 Ag1 2.204(3) 2_546 ? N3 C9 1.335(5) . ? N3 C5 1.345(5) . ? N4 O2 1.215(5) . ? N4 O3 1.220(5) . ? N4 O1 1.237(5) . ? C2 C3 1.364(6) . ? C3 C4 1.383(5) . ? C4 C5 1.493(5) . ? C5 C6 1.375(5) . ? C6 C7 1.379(6) . ? C7 C8 1.361(7) . ? C8 C9 1.377(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 N2 Ag1 N1 134.42(11) 2_556 . ? N2 Ag1 N3 126.60(11) 2_556 . ? N1 Ag1 N3 69.99(10) . . ? N2 Ag1 O1 129.38(12) 2_556 . ? N1 Ag1 O1 90.43(12) . . ? N3 Ag1 O1 84.78(12) . . ? C1 N1 C4 117.5(3) . . ? C1 N1 Ag1 124.7(2) . . ? C4 N1 Ag1 117.8(2) . . ? C1 N2 C2 115.7(3) . . ? C1 N2 Ag1 119.1(2) . 2_546 ? C2 N2 Ag1 123.2(3) . 2_546 ? C9 N3 C5 117.9(4) . . ? C9 N3 Ag1 123.4(3) . . ? C5 N3 Ag1 116.1(2) . . ? O2 N4 O3 121.7(4) . . ? O2 N4 O1 117.7(4) . . ? O3 N4 O1 120.5(4) . . ? N4 O1 Ag1 106.3(3) . . ? N1 C1 N2 126.6(3) . . ? N2 C2 C3 122.2(4) . . ? C2 C3 C4 118.0(3) . . ? N1 C4 C3 120.0(3) . . ? N1 C4 C5 117.0(3) . . ? C3 C4 C5 123.0(3) . . ? N3 C5 C6 121.9(3) . . ? N3 C5 C4 116.3(3) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C7 119.0(4) . . ? C8 C7 C6 119.6(4) . . ? C7 C8 C9 118.4(4) . . ? N3 C9 C8 123.2(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.451 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.066 #===END