# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2198 data_B005289M_[Ag(R-Hpyrrld)]2 #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_contact_author_name ' Kenji Nomiya' _publ_contact_author_address ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-463/59-4111(Ext.2717) ' _publ_contact_author_fax ' +81-463/58-9684 ' _publ_contact_author_email ' nomiya@chem.kanagawa-u.ac.jp ' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Water-soluble silver(I) complexes with (R)-(+)-2-pyrrolidone-5-carboxylic acid (R-H2pyrrld) and its racemic ligand showing wide spectra of effective antimicrobial activities. Chiral helical polymer and polymer sheet structures in the solid state formed by self-assembly of dimeric [Ag(Hpyrrld)]2 cores ; _publ_section_title_footnote ; ENTER ANY FOOTNOTES TO TITLE ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Kenji Nomiya ' ? ; Department of Materials Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Satoshi Takahashi ' ? ; Department of Materials Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Ryusuke Noguchi ' ? ; Department of Materials Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; #============================================================================== # TEXT _publ_section_abstract ; ; _publ_section_exptl_refinement ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; _publ_section_figure_captions ; ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution 'Direct Method(SIR97)' _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 5.196(1) _cell_length_b 12.740(3) _cell_length_c 9.716(2) _cell_angle_alpha 90 _cell_angle_beta 94.820(3) _cell_angle_gamma 90 _cell_volume 640.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 7395 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.446 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 471.95 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H12 Ag2 N2 O6 ' _chemical_formula_moiety 'C10 H12 Ag2 N2 O6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 456.00 _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_max 1.482 _exptl_absorpt_correction_T_min 0.700 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'RAXIS-RAPID' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 1491 _reflns_number_total 1491 _reflns_number_gt 1192 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.07260 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00500 _diffrn_orient_matrix_UB_12 -0.07792 _diffrn_orient_matrix_UB_13 -0.01230 _diffrn_orient_matrix_UB_21 -0.06345 _diffrn_orient_matrix_UB_22 -0.00804 _diffrn_orient_matrix_UB_23 0.09379 _diffrn_orient_matrix_UB_31 -0.18236 _diffrn_orient_matrix_UB_32 0.00493 _diffrn_orient_matrix_UB_33 -0.04149 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 20 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 24 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 12 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ag 0 4 -1.085 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ag(1) 0.0117(2) 0.4633 -0.2130(1) 0.0475(3) 1.000 Uani d . 1.00 Ag(1a) -0.4460(2) 0.4058(1) -0.3880(1) 0.0475(3) 1.000 Uani d . 1.00 O(1a) -0.226(2) 0.2671(8) -0.429(1) 0.056(3) 1.000 Uani d . 1.00 O(1) -0.198(2) 0.6111(9) -0.190(2) 0.066(4) 1.000 Uani d . 1.00 O(2a) 0.132(2) 0.3149(8) -0.301(1) 0.045(3) 1.000 Uani d . 1.00 O(2) -0.577(2) 0.5577(8) -0.299(1) 0.043(3) 1.000 Uani d . 1.00 O(3a) -0.225(2) -0.0814(9) -0.410(1) 0.050(3) 1.000 Uani d . 1.00 O(3) -0.250(3) 0.9355(9) -0.013(1) 0.074(4) 1.000 Uani d . 1.00 N(1a) -0.046(3) 0.0741(9) -0.471(1) 0.040(3) 1.000 Uani d . 1.00 N(1) -0.382(3) 0.8110(9) -0.171(2) 0.047(4) 1.000 Uani d . 1.00 C(2a) -0.065(3) -0.011(1) -0.388(2) 0.047(4) 1.000 Uani d . 1.00 C(2) -0.383(3) 0.860(1) -0.050(2) 0.044(4) 1.000 Uani d . 1.00 C(3a) 0.142(4) 0.000(2) -0.271(3) 0.076(7) 1.000 Uani d . 1.00 C(3) -0.589(4) 0.808(1) 0.032(2) 0.056(5) 1.000 Uani d . 1.00 C(4) -0.668(3) 0.710(1) -0.046(2) 0.051(5) 1.000 Uani d . 1.00 C(4a) 0.281(4) 0.099(1) -0.290(3) 0.088(7) 1.000 Uani d . 1.00 C(5a) 0.137(3) 0.153(1) -0.414(2) 0.040(4) 1.000 Uani d . 1.00 C(5) -0.565(3) 0.723(1) -0.189(2) 0.045(4) 1.000 Uani d . 1.00 C(6) -0.435(3) 0.623(1) -0.227(2) 0.040(4) 1.000 Uani d . 1.00 C(6a) -0.003(3) 0.255(1) -0.378(2) 0.041(4) 1.000 Uani d . 1.00 H(1) 0.2830 0.1407 -0.2108 0.107 1.000 Uiso c . 1.00 H(2) 0.4554 0.0836 -0.3101 0.107 1.000 Uiso c . 1.00 H(3) 0.2554 -0.0581 -0.2724 0.094 1.000 Uiso c . 1.00 H(4) 0.0624 0.0018 -0.1875 0.094 1.000 Uiso c . 1.00 H(5) -0.8472 0.7026 -0.0546 0.061 1.000 Uiso c . 1.00 H(6) -0.5889 0.6499 -0.0010 0.061 1.000 Uiso c . 1.00 H(7) -0.5126 0.7929 0.1231 0.068 1.000 Uiso c . 1.00 H(8) -0.7285 0.8547 0.0380 0.068 1.000 Uiso c . 1.00 H(11) 0.2540 0.1692 -0.4823 0.046 1.000 Uiso c . 1.00 H(12) -0.7018 0.7397 -0.2555 0.055 1.000 Uiso c . 1.00 H(13) -0.1438 0.0813 -0.5587 0.046 1.000 Uiso c . 1.00 H(14) -0.2702 0.8315 -0.2398 0.057 1.000 Uiso c . 1.00 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0467(6) 0.0309(5) 0.0648(8) 0.0038(5) 0.0040(5) -0.0008(5) Ag(1a) 0.0498(7) 0.0313(5) 0.0608(8) 0.0074(5) 0.0014(5) -0.0050(5) O(1a) 0.037(5) 0.033(5) 0.10(1) 0.001(5) 0.002(6) -0.016(6) O(1) 0.038(6) 0.035(6) 0.12(1) 0.016(5) -0.027(7) -0.024(6) O(2a) 0.039(6) 0.032(5) 0.063(7) 0.004(4) 0.002(5) -0.012(5) O(2) 0.053(6) 0.030(5) 0.046(7) -0.004(5) 0.007(5) -0.008(4) O(3a) 0.055(6) 0.042(6) 0.052(6) -0.014(5) -0.006(5) 0.001(5) O(3) 0.12(1) 0.043(7) 0.050(8) -0.017(7) -0.033(8) -0.004(5) N(1a) 0.057(8) 0.028(5) 0.032(7) 0.002(6) -0.013(5) -0.006(4) N(1) 0.056(8) 0.026(5) 0.058(9) -0.003(5) -0.003(6) -0.004(5) C(2a) 0.053(9) 0.032(8) 0.05(1) 0.012(7) -0.015(7) -0.001(6) C(2) 0.054(9) 0.041(7) 0.032(9) 0.018(7) -0.027(7) -0.010(6) C(3a) 0.05(1) 0.07(1) 0.10(2) -0.02(1) -0.00(1) 0.02(1) C(3) 0.06(1) 0.042(8) 0.06(1) 0.005(8) -0.007(9) -0.003(7) C(4) 0.037(7) 0.049(8) 0.07(1) -0.010(7) 0.009(7) -0.017(7) C(4a) 0.08(1) 0.028(7) 0.14(2) -0.015(9) -0.06(1) -0.00(1) C(5a) 0.033(7) 0.035(7) 0.050(9) -0.009(6) -0.007(6) -0.006(6) C(5) 0.053(9) 0.025(6) 0.05(1) 0.011(7) -0.016(7) -0.001(6) C(6) 0.058(9) 0.024(6) 0.037(8) 0.008(6) 0.012(7) -0.005(5) C(6a) 0.045(8) 0.027(6) 0.053(9) -0.010(6) 0.016(7) 0.004(6) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00160|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000001911 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1192 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_all 0.0690 _refine_ls_wR_factor_ref 0.0690 _refine_ls_goodness_of_fit_all 1.216 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_shift/su_max 0.0300 _refine_ls_shift/su_mean 0.0032 _refine_diff_density_min -1.42 _refine_diff_density_max 0.96 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) Ag(1a) 2.899(2) 1_555 1_555 yes Ag(1) O(1) 2.20(1) 1_555 1_555 yes Ag(1) O(2a) 2.19(1) 1_555 1_555 yes Ag(1) O(3) 2.46(1) 1_555 1_555 yes Ag(1a) O(1a) 2.16(1) 1_555 1_555 yes Ag(1a) O(2) 2.25(1) 1_555 1_555 yes O(1a) C(6a) 1.23(2) 1_555 1_555 yes O(1) C(6) 1.26(2) 1_555 1_555 yes O(2a) C(6a) 1.24(2) 1_555 1_555 yes O(2) C(6) 1.28(2) 1_555 1_555 yes O(3a) C(2a) 1.23(2) 1_555 1_555 yes O(3) C(2) 1.22(2) 1_555 1_555 yes N(1a) C(2a) 1.36(2) 1_555 1_555 yes N(1a) C(5a) 1.46(2) 1_555 1_555 yes N(1a) H(13) 0.96 1_555 1_555 no N(1) C(2) 1.33(2) 1_555 1_555 yes N(1) C(5) 1.47(2) 1_555 1_555 yes N(1) H(14) 0.96 1_555 1_555 no C(2a) C(3a) 1.50(3) 1_555 1_555 yes C(2) C(3) 1.54(3) 1_555 1_555 yes C(3a) C(4a) 1.47(3) 1_555 1_555 yes C(3a) H(3) 0.95 1_555 1_555 no C(3a) H(4) 0.95 1_555 1_555 no C(3) C(4) 1.50(3) 1_555 1_555 yes C(3) H(7) 0.96 1_555 1_555 no C(3) H(8) 0.94 1_555 1_555 no C(4) C(5) 1.53(3) 1_555 1_555 yes C(4) H(5) 0.94 1_555 1_555 no C(4) H(6) 0.96 1_555 1_555 no C(4a) C(5a) 1.53(3) 1_555 1_555 yes C(4a) H(1) 0.94 1_555 1_555 no C(4a) H(2) 0.96 1_555 1_555 no C(5a) C(6a) 1.55(2) 1_555 1_555 yes C(5a) H(11) 0.96 1_555 1_555 no C(5) C(6) 1.51(2) 1_555 1_555 yes C(5) H(12) 0.94 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag(1a) Ag(1) O(1) 83.5(3) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(2a) 78.5(3) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(3) 144.6(4) 1_555 1_555 1_555 yes O(1) Ag(1) O(2a) 160.3(5) 1_555 1_555 1_555 yes O(1) Ag(1) O(3) 104.4(6) 1_555 1_555 1_555 yes O(2a) Ag(1) O(3) 94.9(5) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(1a) 83.9(3) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(2) 79.5(3) 1_555 1_555 1_555 yes O(1a) Ag(1a) O(2) 163.2(5) 1_555 1_555 1_555 yes Ag(1a) O(1a) C(6a) 121(1) 1_555 1_555 1_555 yes Ag(1) O(1) C(6) 123(1) 1_555 1_555 1_555 yes Ag(1) O(2a) C(6a) 127(1) 1_555 1_555 1_555 yes Ag(1a) O(2) C(6) 126(1) 1_555 1_555 1_555 yes Ag(1) O(3) C(2) 127(1) 2 2 2 yes C(2a) N(1a) C(5a) 114(1) 1_555 1_555 1_555 yes C(2a) N(1a) H(13) 122.8 1_555 1_555 1_555 no C(5a) N(1a) H(13) 123.0 1_555 1_555 1_555 no C(2) N(1) C(5) 115(2) 1_555 1_555 1_555 yes C(2) N(1) H(14) 122.3 1_555 1_555 1_555 no C(5) N(1) H(14) 123.1 1_555 1_555 1_555 no O(3a) C(2a) N(1a) 124(2) 1_555 1_555 1_555 yes O(3a) C(2a) C(3a) 129(2) 1_555 1_555 1_555 yes N(1a) C(2a) C(3a) 106(2) 1_555 1_555 1_555 yes O(3) C(2) N(1) 126(2) 1_555 1_555 1_555 yes O(3) C(2) C(3) 126(2) 1_555 1_555 1_555 yes N(1) C(2) C(3) 108(2) 1_555 1_555 1_555 yes C(2a) C(3a) C(4a) 108(2) 1_555 1_555 1_555 yes C(2a) C(3a) H(3) 108.8 1_555 1_555 1_555 no C(2a) C(3a) H(4) 108.3 1_555 1_555 1_555 no C(4a) C(3a) H(3) 111.0 1_555 1_555 1_555 no C(4a) C(3a) H(4) 110.3 1_555 1_555 1_555 no H(3) C(3a) H(4) 110.0 1_555 1_555 1_555 no C(2) C(3) C(4) 105(2) 1_555 1_555 1_555 yes C(2) C(3) H(7) 108.5 1_555 1_555 1_555 no C(2) C(3) H(8) 109.6 1_555 1_555 1_555 no C(4) C(3) H(7) 111.8 1_555 1_555 1_555 no C(4) C(3) H(8) 111.9 1_555 1_555 1_555 no H(7) C(3) H(8) 109.7 1_555 1_555 1_555 no C(3) C(4) C(5) 106(2) 1_555 1_555 1_555 yes C(3) C(4) H(5) 110.9 1_555 1_555 1_555 no C(3) C(4) H(6) 110.1 1_555 1_555 1_555 no C(5) C(4) H(5) 110.7 1_555 1_555 1_555 no C(5) C(4) H(6) 109.5 1_555 1_555 1_555 no H(5) C(4) H(6) 109.9 1_555 1_555 1_555 no C(3a) C(4a) C(5a) 106(2) 1_555 1_555 1_555 yes C(3a) C(4a) H(1) 110.8 1_555 1_555 1_555 no C(3a) C(4a) H(2) 109.7 1_555 1_555 1_555 no C(5a) C(4a) H(1) 111.0 1_555 1_555 1_555 no C(5a) C(4a) H(2) 109.9 1_555 1_555 1_555 no H(1) C(4a) H(2) 109.5 1_555 1_555 1_555 no N(1a) C(5a) C(4a) 104(1) 1_555 1_555 1_555 yes N(1a) C(5a) C(6a) 111(1) 1_555 1_555 1_555 yes N(1a) C(5a) H(11) 108.7 1_555 1_555 1_555 no C(4a) C(5a) C(6a) 114(2) 1_555 1_555 1_555 yes C(4a) C(5a) H(11) 109.9 1_555 1_555 1_555 no C(6a) C(5a) H(11) 108.6 1_555 1_555 1_555 no N(1) C(5) C(4) 104(1) 1_555 1_555 1_555 yes N(1) C(5) C(6) 112(2) 1_555 1_555 1_555 yes N(1) C(5) H(12) 110.7 1_555 1_555 1_555 no C(4) C(5) C(6) 109(1) 1_555 1_555 1_555 yes C(4) C(5) H(12) 110.3 1_555 1_555 1_555 no C(6) C(5) H(12) 110.3 1_555 1_555 1_555 no O(1) C(6) O(2) 126(2) 1_555 1_555 1_555 yes O(1) C(6) C(5) 118(2) 1_555 1_555 1_555 yes O(2) C(6) C(5) 116(2) 1_555 1_555 1_555 yes O(1a) C(6a) O(2a) 130(2) 1_555 1_555 1_555 yes O(1a) C(6a) C(5a) 117(2) 1_555 1_555 1_555 yes O(2a) C(6a) C(5a) 114(2) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #============================================================================== data_B005289M_[Ag2(R-Hpyrrld)(S-Hpyrrld)] #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution 'Direct Method (SIR97)' _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 7.459(1) _cell_length_b 5.312(5) _cell_length_c 15.961(1) _cell_angle_alpha 90 _cell_angle_beta 92.11(1) _cell_angle_gamma 90 _cell_volume 631.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 471.95 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H12 Ag2 N2 O6 ' _chemical_formula_moiety 'C10 H12 Ag2 N2 O6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 456.00 _exptl_absorpt_coefficient_mu 3.117 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.752 _exptl_special_details ; The scan width was (1.05+0.30tan\q)\% with an \w scan speed of 8\% per minute (up to 6 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.94 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 0 2 -1 -4 2 1 -4 _diffrn_reflns_number 1721 _reflns_number_total 1605 _reflns_number_gt 875 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04733 _diffrn_reflns_av_sigmaI/netI 0.111 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.11353 _diffrn_orient_matrix_UB_12 0.01592 _diffrn_orient_matrix_UB_13 -0.03101 _diffrn_orient_matrix_UB_21 0.07108 _diffrn_orient_matrix_UB_22 -0.04505 _diffrn_orient_matrix_UB_23 0.05220 _diffrn_orient_matrix_UB_31 -0.00766 _diffrn_orient_matrix_UB_32 -0.18209 _diffrn_orient_matrix_UB_33 -0.01563 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 20 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 24 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 12 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ag 0 4 -1.085 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ag(1) 0.48329(7) 0.2135(1) 0.55453(3) 0.0381(1) 1.000 Uani d . 1.00 O(1) 0.6826(5) 0.3535(8) 0.4683(2) 0.042(1) 1.000 Uani d . 1.00 O(2) 0.2834(5) -0.0218(8) 0.6156(3) 0.039(1) 1.000 Uani d . 1.00 O(3) 0.5686(6) 0.4217(9) 0.6889(3) 0.050(2) 1.000 Uani d . 1.00 N(1) 0.0858(6) -0.327(1) 0.7223(3) 0.034(2) 1.000 Uani d . 1.00 C(2) -0.0409(8) -0.164(1) 0.7405(4) 0.034(2) 1.000 Uani d . 1.00 C(3) -0.1427(8) -0.095(1) 0.6613(4) 0.043(2) 1.000 Uani d . 1.00 C(4) -0.0818(8) -0.286(2) 0.5976(4) 0.049(2) 1.000 Uani d . 1.00 C(5) 0.0985(8) -0.384(1) 0.6338(4) 0.035(2) 1.000 Uani d . 1.00 C(6) 0.2488(7) -0.241(1) 0.5921(3) 0.030(2) 1.000 Uani d . 1.00 H(1) -0.0669 -0.2090 0.5447 0.059 1.000 Uiso c . 1.00 H(2) -0.1661 -0.4196 0.5919 0.059 1.000 Uiso c . 1.00 H(3) 0.1095 -0.5604 0.6250 0.042 1.000 Uiso c . 1.00 H(4) -0.1132 0.0714 0.6443 0.051 1.000 Uiso c . 1.00 H(5) -0.2681 -0.1064 0.6683 0.051 1.000 Uiso c . 1.00 H(6) 0.1643 -0.4016 0.7638 0.042 1.000 Uiso c . 1.00 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0449(3) 0.0367(3) 0.0339(2) -0.0055(3) 0.0156(2) -0.0001(3) O(1) 0.053(3) 0.044(3) 0.031(2) -0.011(2) 0.022(2) -0.014(2) O(2) 0.046(3) 0.036(3) 0.037(3) -0.012(2) 0.017(2) -0.007(2) O(3) 0.070(3) 0.052(3) 0.029(3) -0.020(3) 0.012(2) -0.003(2) N(1) 0.040(3) 0.039(3) 0.024(3) 0.010(3) 0.006(2) 0.001(3) C(2) 0.040(4) 0.033(4) 0.031(3) -0.002(3) 0.010(3) 0.002(3) C(3) 0.036(4) 0.053(5) 0.039(4) 0.007(3) 0.004(3) 0.013(4) C(4) 0.042(4) 0.070(5) 0.035(4) -0.023(4) 0.001(3) -0.005(4) C(5) 0.048(4) 0.027(3) 0.031(3) -0.007(3) 0.006(3) -0.005(3) C(6) 0.037(3) 0.030(4) 0.022(3) 0.000(3) 0.003(2) 0.006(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 875 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_all 0.0250 _refine_ls_wR_factor_ref 0.0250 _refine_ls_goodness_of_fit_all 1.233 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.57 _refine_diff_density_max 0.62 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) Ag(1) 2.875(2) 1_555 1_555 yes Ag(1) O(1) 2.193(4) 1_555 1_555 yes Ag(1) O(2) 2.200(4) 1_555 1_555 yes Ag(1) O(3) 2.476(5) 1_555 1_555 yes O(1) C(6) 1.259(7) 1_555 1_555 yes O(2) C(6) 1.247(8) 1_555 1_555 yes O(3) C(2) 1.239(7) 1_555 1_555 yes N(1) C(2) 1.322(8) 1_555 1_555 yes N(1) C(5) 1.452(7) 1_555 1_555 yes N(1) H(6) 0.95 1_555 1_555 no C(2) C(3) 1.497(9) 1_555 1_555 yes C(3) C(4) 1.52(1) 1_555 1_555 yes C(3) H(4) 0.95 1_555 1_555 no C(3) H(5) 0.95 1_555 1_555 no C(4) C(5) 1.536(9) 1_555 1_555 yes C(4) H(1) 0.95 1_555 1_555 no C(4) H(2) 0.95 1_555 1_555 no C(5) C(6) 1.528(8) 1_555 1_555 yes C(5) H(3) 0.95 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag(1) Ag(1) O(1) 79.2(1) 3_656 3_656 3_656 yes Ag(1) Ag(1) O(2) 84.0(1) 3_656 3_656 3_656 yes Ag(1) Ag(1) O(3) 148.4(1) 3_656 3_656 3_656 yes O(1) Ag(1) O(2) 163.1(2) 1_555 1_555 1_555 yes O(1) Ag(1) O(3) 103.5(2) 1_555 1_555 1_555 yes O(2) Ag(1) O(3) 91.5(2) 1_555 1_555 1_555 yes Ag(1) O(1) C(6) 128.5(4) 1_555 1_555 1_555 yes Ag(1) O(2) C(6) 122.2(4) 1_555 1_555 1_555 yes Ag(1) O(3) C(2) 125.3(5) 1_555 1_555 1_555 yes C(2) N(1) C(5) 115.1(6) 1_555 1_555 1_555 yes C(2) N(1) H(6) 123.0 1_555 1_555 1_555 no C(5) N(1) H(6) 121.9 1_555 1_555 1_555 no O(3) C(2) N(1) 125.8(7) 2_546 2_546 2_546 yes O(3) C(2) C(3) 125.6(7) 2_546 2_546 2_546 yes N(1) C(2) C(3) 108.6(6) 1_555 1_555 1_555 yes C(2) C(3) C(4) 104.3(6) 1_555 1_555 1_555 yes C(2) C(3) H(4) 110.7 1_555 1_555 1_555 no C(2) C(3) H(5) 110.8 1_555 1_555 1_555 no C(4) C(3) H(4) 110.6 1_555 1_555 1_555 no C(4) C(3) H(5) 110.9 1_555 1_555 1_555 no H(4) C(3) H(5) 109.5 1_555 1_555 1_555 no C(3) C(4) C(5) 104.7(5) 1_555 1_555 1_555 yes C(3) C(4) H(1) 110.9 1_555 1_555 1_555 no C(3) C(4) H(2) 110.5 1_555 1_555 1_555 no C(5) C(4) H(1) 110.6 1_555 1_555 1_555 no C(5) C(4) H(2) 110.4 1_555 1_555 1_555 no H(1) C(4) H(2) 109.6 1_555 1_555 1_555 no N(1) C(5) C(4) 102.0(5) 1_555 1_555 1_555 yes N(1) C(5) C(6) 113.2(6) 1_555 1_555 1_555 yes N(1) C(5) H(3) 111.0 1_555 1_555 1_555 no C(4) C(5) C(6) 108.2(6) 1_555 1_555 1_555 yes C(4) C(5) H(3) 111.0 1_555 1_555 1_555 no C(6) C(5) H(3) 110.9 1_555 1_555 1_555 no O(1) C(6) O(2) 126.1(6) 3_656 3_656 3_656 yes O(1) C(6) C(5) 114.9(6) 3_656 3_656 3_656 yes O(2) C(6) C(5) 118.7(6) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #============================================================================== # End of CIF #==============================================================================