Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_DJW9806 _database_code_CSD 182733 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Goodgame, D.' 'Grachvogel, David A.' 'Williams, David J.' _publ_contact_author_name 'Prof D Goodgame' _publ_contact_author_address ; Chemistry Department Imperial College of Science LONDON SW7 2AY U.K. ; _publ_contact_author_email 'D.GOODGAME@IC.AC.UK' _publ_section_title ; Combination of weak covalent, hydrogen bonding, and Ag...pi interactions in the formation of a 3D porous network Ag(pypd)2(CIO4).CH2CI2 by the ambidentate ligand 1-(4'-pyridyl)pyridin-4-one ; _audit_creation_method shelxl _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'Ag(pypd)2 (ClO4) [pypd = 1-(4'-pyridyl)pyridin-4-one]' _chemical_formula_structural 'Ag(pypd)2 (ClO4) . CH2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C21 H18 Ag Cl3 N4 O6' _chemical_formula_weight 636.61 _chemical_melting_point ? _chemical_compound_source ? 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 P21/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 14.8703(9) _cell_length_b 19.2390(14) _cell_length_c 8.4894(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.937(6) _cell_angle_gamma 90.00 _cell_volume 2425.5(3) _cell_formula_units_z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 4.94 _cell_measurement_theta_max 12.48 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method ? _exptl_crystal_f_000 1272 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type ellipsoidal _exptl_absorpt_correction_t_min 0.5112 _exptl_absorpt_correction_t_max 0.5883 _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 'siemens p4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.06 _diffrn_reflns_number 4568 _diffrn_reflns_av_r_equivalents 0.0347 _diffrn_reflns_av_sigmai/neti 0.0763 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4257 _reflns_number_observed 2778 _reflns_observed_criterion >2sigma(i) _computing_data_collection 'siemens xscans' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4257 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_obs 0.0562 _refine_ls_wR_factor_all 0.1400 _refine_ls_wR_factor_obs 0.1190 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag Ag 0.73284(4) 0.71490(3) 0.33972(8) 0.0546(2) Uani 1 d . . N1 N 0.8121(4) 0.7985(3) 0.4493(7) 0.0477(14) Uani 1 d . . C2 C 0.8732(5) 0.7841(4) 0.5652(9) 0.053(2) Uani 1 d . . H2A H 0.8852(5) 0.7377(4) 0.5888(9) 0.063 Uiso 1 calc R . C3 C 0.9193(5) 0.8343(3) 0.6517(9) 0.048(2) Uani 1 d . . H3A H 0.9604(5) 0.8217(3) 0.7330(9) 0.058 Uiso 1 calc R . C4 C 0.9037(4) 0.9044(3) 0.6163(8) 0.0406(15) Uani 1 d . . C5 C 0.8388(5) 0.9192(3) 0.4981(9) 0.051(2) Uani 1 d . . H5A H 0.8248(5) 0.9651(3) 0.4723(9) 0.061 Uiso 1 calc R . C6 C 0.7950(5) 0.8653(4) 0.4191(9) 0.048(2) Uani 1 d . . H6A H 0.7512(5) 0.8761(4) 0.3408(9) 0.058 Uiso 1 calc R . N7 N 0.9533(4) 0.9581(3) 0.6969(7) 0.0447(13) Uani 1 d . . C8 C 1.0390(5) 0.9476(3) 0.7545(10) 0.052(2) Uani 1 d . . H8A H 1.0658(5) 0.9046(3) 0.7399(10) 0.063 Uiso 1 calc R . C9 C 1.0863(5) 0.9975(4) 0.8317(11) 0.063(2) Uani 1 d . . H9A H 1.1438(5) 0.9867(4) 0.8725(11) 0.075 Uiso 1 calc R . C10 C 1.0535(5) 1.0660(4) 0.8550(10) 0.052(2) Uani 1 d . . O10 O 1.0957(4) 1.1122(3) 0.9253(9) 0.077(2) Uani 1 d . . C11 C 0.9627(5) 1.0749(4) 0.7857(11) 0.059(2) Uani 1 d . . H11A H 0.9354(5) 1.1182(4) 0.7933(11) 0.071 Uiso 1 calc R . C12 C 0.9176(5) 1.0246(4) 0.7130(10) 0.054(2) Uani 1 d . . H12A H 0.8599(5) 1.0337(4) 0.6707(10) 0.065 Uiso 1 calc R . N13 N 0.6853(4) 0.6075(3) 0.3087(8) 0.0458(14) Uani 1 d . . C14 C 0.7120(5) 0.5594(4) 0.4121(10) 0.057(2) Uani 1 d . . H14A H 0.7617(5) 0.5694(4) 0.4793(10) 0.068 Uiso 1 calc R . C15 C 0.6710(5) 0.4952(4) 0.4274(10) 0.055(2) Uani 1 d . . H15A H 0.6924(5) 0.4626(4) 0.5010(10) 0.066 Uiso 1 calc R . C16 C 0.5961(4) 0.4820(3) 0.3267(7) 0.0373(13) Uani 1 d . . C17 C 0.5687(5) 0.5305(3) 0.2177(9) 0.050(2) Uani 1 d . . H17A H 0.5196(5) 0.5222(3) 0.1481(9) 0.060 Uiso 1 calc R . C18 C 0.6154(6) 0.5922(4) 0.2127(9) 0.054(2) Uani 1 d . . H18A H 0.5967(6) 0.6249(4) 0.1374(9) 0.065 Uiso 1 calc R . N19 N 0.5474(4) 0.4181(2) 0.3390(6) 0.0365(11) Uani 1 d . . C20 C 0.5406(5) 0.3847(3) 0.4810(8) 0.046(2) Uani 1 d . . H20A H 0.5740(5) 0.4011(3) 0.5688(8) 0.056 Uiso 1 calc R . C21 C 0.4881(5) 0.3297(4) 0.4968(9) 0.051(2) Uani 1 d . . H21A H 0.4865(5) 0.3085(4) 0.5950(9) 0.062 Uiso 1 calc R . C22 C 0.4336(5) 0.3019(3) 0.3669(8) 0.0417(15) Uani 1 d . . O22 O 0.3774(4) 0.2540(3) 0.3842(6) 0.0562(13) Uani 1 d . . C23 C 0.4476(5) 0.3349(3) 0.2201(8) 0.046(2) Uani 1 d . . H23A H 0.4181(5) 0.3177(3) 0.1290(8) 0.056 Uiso 1 calc R . C24 C 0.5016(5) 0.3897(3) 0.2091(8) 0.047(2) Uani 1 d . . H24A H 0.5087(5) 0.4095(3) 0.1105(8) 0.056 Uiso 1 calc R . Cl Cl 0.31340(13) 0.58340(10) 0.1188(2) 0.0538(4) Uani 1 d . . O1 O 0.3415(7) 0.5150(4) 0.1616(12) 0.116(3) Uani 1 d . . O2 O 0.3884(5) 0.6293(5) 0.1257(11) 0.106(3) Uani 1 d . . O3 O 0.2550(7) 0.6064(5) 0.2284(14) 0.137(4) Uani 1 d . . O4 O 0.2738(8) 0.5825(5) -0.0307(11) 0.134(4) Uani 1 d . . C30 C 0.2202(8) -0.2320(6) -0.0119(16) 0.095(3) Uani 1 d . . H30A H 0.2404(8) -0.2126(6) -0.1095(16) 0.114 Uiso 1 calc R . H30B H 0.2496(8) -0.2766(6) 0.0046(16) 0.114 Uiso 1 calc R . Cl31 Cl 0.2524(2) -0.1766(2) 0.1435(4) 0.1066(10) Uani 1 d . . Cl32 Cl 0.1049(3) -0.2443(3) -0.0295(6) 0.1330(14) Uani 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 0.0562(3) 0.0390(3) 0.0681(4) -0.0092(3) -0.0027(2) -0.0136(3) N1 0.049(3) 0.041(3) 0.052(3) -0.006(2) -0.001(3) -0.015(2) C2 0.057(4) 0.036(3) 0.064(4) -0.004(4) -0.008(3) 0.001(3) C3 0.048(4) 0.038(3) 0.057(4) 0.000(3) -0.013(3) -0.001(3) C4 0.040(3) 0.032(3) 0.050(4) -0.002(3) 0.000(3) -0.002(2) C5 0.056(4) 0.036(3) 0.059(4) 0.005(3) -0.013(3) -0.003(3) C6 0.052(4) 0.044(3) 0.047(4) 0.001(3) -0.008(3) -0.014(3) N7 0.037(3) 0.038(3) 0.059(4) -0.009(3) -0.008(3) 0.001(2) C8 0.047(4) 0.033(3) 0.076(5) -0.007(3) -0.007(4) -0.002(3) C9 0.044(4) 0.046(4) 0.095(6) -0.009(4) -0.025(4) 0.002(3) C10 0.048(4) 0.044(4) 0.065(5) -0.001(3) -0.005(4) -0.004(3) O10 0.069(4) 0.049(3) 0.108(5) -0.024(3) -0.031(4) -0.004(3) C11 0.048(4) 0.038(3) 0.089(6) -0.013(4) -0.008(4) 0.003(3) C12 0.047(4) 0.040(3) 0.074(5) -0.005(3) -0.008(4) 0.009(3) N13 0.042(3) 0.032(3) 0.063(4) -0.002(2) -0.007(3) -0.008(2) C14 0.045(4) 0.041(3) 0.081(5) -0.002(3) -0.024(4) -0.004(3) C15 0.050(4) 0.041(3) 0.072(5) 0.012(3) -0.024(4) -0.004(3) C16 0.042(3) 0.033(3) 0.037(3) -0.005(2) 0.003(3) -0.006(2) C17 0.061(4) 0.039(3) 0.047(4) 0.001(3) -0.021(3) -0.009(3) C18 0.069(5) 0.042(4) 0.050(4) 0.010(3) -0.012(4) -0.009(3) N19 0.043(3) 0.030(2) 0.036(3) -0.001(2) -0.003(2) -0.007(2) C20 0.057(4) 0.043(3) 0.038(4) -0.001(3) -0.008(3) -0.008(3) C21 0.063(5) 0.046(4) 0.044(4) 0.006(3) -0.012(3) -0.011(3) C22 0.047(4) 0.029(3) 0.049(4) 0.001(2) -0.001(3) 0.001(2) O22 0.068(3) 0.043(2) 0.057(3) 0.010(2) -0.009(3) -0.017(2) C23 0.063(4) 0.040(3) 0.035(3) -0.007(3) -0.006(3) -0.004(3) C24 0.065(4) 0.045(3) 0.031(3) -0.001(3) -0.005(3) -0.012(3) Cl 0.0515(10) 0.0580(10) 0.0510(10) -0.0022(8) -0.0067(8) -0.0009(8) O1 0.130(7) 0.072(4) 0.140(8) 0.016(5) -0.035(6) 0.011(5) O2 0.082(5) 0.109(6) 0.126(7) 0.006(5) -0.001(5) -0.029(4) O3 0.127(8) 0.120(7) 0.172(10) -0.017(7) 0.077(8) -0.012(6) O4 0.191(10) 0.110(6) 0.092(6) 0.010(5) -0.077(7) -0.029(7) C30 0.111(9) 0.077(7) 0.100(8) -0.006(6) 0.022(7) -0.005(6) Cl31 0.111(2) 0.098(2) 0.112(2) -0.004(2) 0.018(2) -0.029(2) Cl32 0.101(2) 0.161(3) 0.136(3) -0.037(3) -0.004(2) -0.006(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 Ag N1 2.174(5) . ? Ag N13 2.195(5) . ? Ag O22 2.559(5) 2_655 ? N1 C6 1.332(9) . ? N1 C2 1.334(9) . ? C2 C3 1.375(10) . ? C3 C4 1.399(9) . ? C4 C5 1.386(10) . ? C4 N7 1.424(8) . ? C5 C6 1.381(10) . ? N7 C8 1.358(9) . ? N7 C12 1.394(8) . ? C8 C9 1.340(10) . ? C9 C10 1.423(10) . ? C10 O10 1.226(9) . ? C10 C11 1.455(10) . ? C11 C12 1.313(10) . ? N13 C18 1.321(9) . ? N13 C14 1.323(10) . ? C14 C15 1.388(10) . ? C15 C16 1.391(9) . ? C16 C17 1.362(9) . ? C16 N19 1.433(7) . ? C17 C18 1.375(10) . ? N19 C20 1.375(9) . ? N19 C24 1.379(8) . ? C20 C21 1.324(10) . ? C21 C22 1.438(10) . ? C22 O22 1.257(8) . ? C22 C23 1.424(10) . ? O22 Ag 2.559(5) 2_645 ? C23 C24 1.332(10) . ? Cl O4 1.372(8) . ? Cl O3 1.378(9) . ? Cl O1 1.422(8) . ? Cl O2 1.422(8) . ? C30 Cl32 1.731(13) . ? C30 Cl31 1.743(12) . ? 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 N1 Ag N13 155.7(2) . . ? N1 Ag O22 114.4(2) . 2_655 ? N13 Ag O22 89.9(2) . 2_655 ? C6 N1 C2 117.3(6) . . ? C6 N1 Ag 122.5(5) . . ? C2 N1 Ag 119.7(5) . . ? N1 C2 C3 123.4(7) . . ? C2 C3 C4 119.3(7) . . ? C5 C4 C3 117.1(6) . . ? C5 C4 N7 121.5(6) . . ? C3 C4 N7 121.4(6) . . ? C6 C5 C4 119.4(6) . . ? N1 C6 C5 123.4(7) . . ? C8 N7 C12 117.2(6) . . ? C8 N7 C4 121.2(6) . . ? C12 N7 C4 121.6(6) . . ? C9 C8 N7 121.9(7) . . ? C8 C9 C10 123.8(7) . . ? O10 C10 C9 124.7(7) . . ? O10 C10 C11 123.5(7) . . ? C9 C10 C11 111.8(6) . . ? C12 C11 C10 122.9(7) . . ? C11 C12 N7 122.3(7) . . ? C18 N13 C14 116.9(6) . . ? C18 N13 Ag 121.6(5) . . ? C14 N13 Ag 119.7(5) . . ? N13 C14 C15 124.5(6) . . ? C14 C15 C16 116.5(6) . . ? C17 C16 C15 119.6(6) . . ? C17 C16 N19 120.2(6) . . ? C15 C16 N19 120.2(6) . . ? C16 C17 C18 118.5(6) . . ? N13 C18 C17 123.8(7) . . ? C20 N19 C24 117.4(5) . . ? C20 N19 C16 121.7(5) . . ? C24 N19 C16 120.8(5) . . ? C21 C20 N19 122.2(6) . . ? C20 C21 C22 122.1(7) . . ? O22 C22 C23 123.8(6) . . ? O22 C22 C21 122.4(6) . . ? C23 C22 C21 113.8(6) . . ? C22 O22 Ag 122.2(4) . 2_645 ? C24 C23 C22 122.0(6) . . ? C23 C24 N19 122.2(6) . . ? O4 Cl O3 111.9(8) . . ? O4 Cl O1 109.4(6) . . ? O3 Cl O1 108.1(7) . . ? O4 Cl O2 110.1(6) . . ? O3 Cl O2 107.1(6) . . ? O1 Cl O2 110.1(5) . . ? Cl32 C30 Cl31 112.4(7) . . ? _refine_diff_density_max 0.721 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.091