Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #============================================================================== _audit_creation_date '2001-12-27' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address ' Kenji Nomiya ' ; Department of Materials Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Hironari Yokoyama ' ; Department of Materials Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; _publ_contact_author_name 'Prof Kenji Nomiya' _publ_contact_author_address ; Department of Materials Science, Faculty of science Kanagawa University Tsuchiya Hiratsuka Kanagawa 259-1293 Japan ; _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_section_title ; Syntheses, crystal structures and antimicrobial activities of polymeric silver(I) complexes with three amino acids (aspartic acid (H2asp), glycine (Hgly) and asparagine (Hasn)) ; #============================================================================== _publ_contact_letter ; Dear Sir: We have submitted our article to J. Chem. Soc. Dalton Trans. (Paper ref. B200684G). Herein, we send the crystal data in CIF file. Sincerely, Kenji Nomiya ; _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 ' data_{[Ag2(D-Hasp)(L-Hasp)]1.5H2O}n _database_code_CSD 178114 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 5.6255(6) _cell_length_b 22.469(2) _cell_length_c 5.6114(6) _cell_angle_alpha 90 _cell_angle_beta 100.766(9) _cell_angle_gamma 90 _cell_volume 696.8(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 506.95 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H15 Ag2 N2 O9.50 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 494.00 _exptl_absorpt_coefficient_mu 28.53 _exptl_absorpt_correction_type ; ¥y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.941 _exptl_special_details ; The scan width was (1.26+0.30tan¥q)¥% with an ¥w scan speed of 4¥% 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_% -2.15 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 0 0 1 8 -1 1 6 -1 _diffrn_reflns_number 4895 _reflns_number_total 1681 _reflns_number_gt 1193 _reflns_threshold_expression I>2.00¥s(I) _diffrn_reflns_av_R_equivalents 0.03180 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.09014 _diffrn_orient_matrix_UB_12 0.02946 _diffrn_orient_matrix_UB_13 -0.08292 _diffrn_orient_matrix_UB_21 0.15542 _diffrn_orient_matrix_UB_22 -0.02070 _diffrn_orient_matrix_UB_23 0.06730 _diffrn_orient_matrix_UB_31 -0.02145 _diffrn_orient_matrix_UB_32 -0.02616 _diffrn_orient_matrix_UB_33 -0.14663 #------------------------------------------------------------------------------ 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 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 30 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 19 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) 0.98334(7) 0.03726(1) -0.20992(6) 0.0329(1) 1.000 . Uani d ? O(1) 0.7286(6) 0.0853(1) -0.0158(6) 0.038(1) 1.000 . Uani d ? O(2) 0.8018(7) 0.0353(1) 0.3357(6) 0.0362(9) 1.000 . Uani d ? O(3) 0.1548(6) 0.1329(1) 0.7315(6) 0.038(1) 1.000 . Uani d ? O(4) 0.3310(6) 0.2047(1) 0.5596(6) 0.039(1) 1.000 . Uani d ? O(5) 0.9226(7) 0.2840(2) 0.4729(8) 0.057(1) 1.000 . Uani d ? N(1) 0.5333(6) 0.1782(2) 0.1604(6) 0.026(1) 1.000 . Uani d ? C(1) 0.7178(7) 0.0783(2) 0.2017(8) 0.023(1) 1.000 . Uani d ? C(2) 0.6000(8) 0.1272(2) 0.3301(8) 0.023(1) 1.000 . Uani d ? C(3) 0.3834(8) 0.1051(2) 0.4301(8) 0.027(1) 1.000 . Uani d ? C(4) 0.2821(7) 0.1515(2) 0.5815(8) 0.022(1) 1.000 . Uani d ? H(1) 0.7287 0.1544 0.4190 0.029 1.000 . Uiso c ? H(2) 0.4489 0.2071 0.2341 0.032 1.000 . Uiso c ? H(3) 0.4371 0.1644 0.0149 0.032 1.000 . Uiso c ? H(4) 0.6787 0.1955 0.1253 0.032 1.000 . Uiso c ? H(5) 0.3809 0.0624 0.5144 0.029 1.000 . Uiso c ? H(6) 0.2489 0.0980 0.2818 0.029 1.000 . Uiso c ? H(7) 1.0021 0.3076 0.3754 0.029 1.000 . Uiso c ? H(8) 1.0093 0.2515 0.5395 0.029 1.000 . Uiso c ? 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) 0.0491(2) 0.0242(2) 0.0302(2) 0.0124(2) 0.0200(1) 0.0012(2) O(1) 0.054(2) 0.034(2) 0.030(2) 0.018(2) 0.022(2) 0.005(1) O(2) 0.054(2) 0.029(2) 0.029(2) 0.019(2) 0.016(1) 0.005(1) O(3) 0.045(2) 0.033(2) 0.044(2) -0.003(2) 0.031(2) -0.005(1) O(4) 0.053(2) 0.025(2) 0.050(2) 0.001(1) 0.034(2) -0.006(1) O(5) 0.053(2) 0.052(2) 0.079(3) 0.016(2) 0.046(2) 0.026(2) N(1) 0.032(2) 0.025(2) 0.025(2) 0.003(1) 0.015(2) 0.002(1) C(1) 0.019(2) 0.024(2) 0.030(2) 0.002(2) 0.011(2) -0.004(2) C(2) 0.026(2) 0.021(2) 0.024(2) 0.003(2) 0.009(2) 0.001(2) C(3) 0.029(2) 0.023(2) 0.035(2) -0.003(2) 0.018(2) -0.003(2) C(4) 0.021(2) 0.023(2) 0.025(2) -0.000(2) 0.009(2) -0.003(2) #============================================================================== # 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) + 0.00037|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000004(2) _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 1193 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_all 0.0370 _refine_ls_wR_factor_ref 0.0370 _refine_ls_goodness_of_fit_all 1.217 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.43 _refine_diff_density_max 0.53 #============================================================================== # 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) 2.8679(8) . . ? Ag(1) O(1) 2.234(3) . . ? Ag(1) O(2) 2.223(3) . . ? Ag(1) O(3) 2.403(4) . . ? O(1) C(1) 1.243(6) . . ? O(2) C(1) 1.260(6) . . ? O(3) C(4) 1.273(5) . . ? O(4) C(4) 1.237(5) . . ? O(5) H(7) 0.93 . . no O(5) H(8) 0.92 . . no N(1) C(2) 1.493(6) . . ? N(1) H(2) 0.94 . . no N(1) H(3) 0.94 . . no N(1) H(4) 0.96 . . no C(1) C(2) 1.530(6) . . ? C(2) C(3) 1.517(6) . . ? C(2) H(1) 1.01 . . no C(3) C(4) 1.523(6) . . ? C(3) H(5) 1.07 . . no C(3) H(6) 1.03 . . 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) 80.27(9) 3_755 3_755 3_755 ? Ag(1) Ag(1) O(2) 82.90(9) 3_755 3_755 3_755 ? Ag(1) Ag(1) O(3) 131.9(1) 3_755 3_755 3_755 ? O(1) Ag(1) O(2) 161.1(1) . . . ? O(1) Ag(1) O(3) 86.8(1) . . . ? O(2) Ag(1) O(3) 110.9(1) 3_755 3_755 3_755 ? Ag(1) O(1) C(1) 124.8(3) . . . ? Ag(1) O(2) C(1) 122.6(3) 3_755 3_755 3_755 ? Ag(1) O(3) C(4) 132.4(3) 1_456 1_456 1_456 ? H(7) O(5) H(8) 114.5 . . . no C(2) N(1) H(2) 109.6 . . . no C(2) N(1) H(3) 109.5 . . . no C(2) N(1) H(4) 108.7 . . . no H(2) N(1) H(3) 110.6 . . . no H(2) N(1) H(4) 109.3 . . . no H(3) N(1) H(4) 109.2 . . . no O(1) C(1) O(2) 127.0(4) . . . ? O(1) C(1) C(2) 118.4(4) . . . ? O(2) C(1) C(2) 114.6(4) . . . ? N(1) C(2) C(1) 109.3(4) . . . ? N(1) C(2) C(3) 111.3(4) . . . ? N(1) C(2) H(1) 85.5 . . . no C(1) C(2) C(3) 112.8(4) . . . ? C(1) C(2) H(1) 109.6 . . . no C(3) C(2) H(1) 124.7 . . . no C(2) C(3) C(4) 113.1(4) . . . ? C(2) C(3) H(5) 122.3 . . . no C(2) C(3) H(6) 105.8 . . . no C(4) C(3) H(5) 109.3 . . . no C(4) C(3) H(6) 105.1 . . . no H(5) C(3) H(6) 98.8 . . . no O(3) C(4) O(4) 123.1(4) . . . ? O(3) C(4) C(3) 117.3(4) . . . ? O(4) C(4) C(3) 119.5(4) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(2) 2.564(4) . 1_554 no Ag(1) C(1) 3.484(5) . 1_554 no O(1) H(7) 2.9797 . 4_554 no O(1) H(5) 3.0184 . 1_554 no O(1) O(5) 3.137(6) . 4_554 no O(1) C(3) 3.373(7) . 1_554 no O(1) C(4) 3.392(6) . 1_554 no O(1) O(3) 3.444(5) . 1_554 no O(2) H(5) 2.6289 . 3_656 no O(2) H(6) 2.9474 . 1_655 no O(2) O(2) 3.059(7) . 3_756 no O(2) O(3) 3.469(5) . 1_655 no O(2) C(3) 3.577(6) . 1_655 no O(3) H(7) 1.8531 . 4_455 no O(3) H(3) 2.1466 . 1_556 no O(3) H(1) 2.7356 . 1_455 no O(3) O(5) 2.772(5) . 4_455 no O(3) H(8) 2.9329 . 1_455 no O(3) N(1) 3.074(6) . 1_556 no O(3) C(2) 3.494(6) . 1_455 no O(4) H(8) 2.0782 . 1_455 no O(4) H(2) 2.2560 . 4 no O(4) H(3) 2.6711 . 1_556 no O(4) H(7) 2.8044 . 4_455 no O(4) O(5) 2.877(5) . 1_455 no O(4) N(1) 2.881(5) . 4 no O(4) H(4) 2.9531 . 4 no O(4) H(7) 3.0213 . 1_455 no O(4) H(3) 3.0219 . 4 no O(4) N(1) 3.403(6) . 1_556 no O(4) O(4) 3.467(4) . 4 no O(4) O(4) 3.467(4) . 4_554 no O(4) O(5) 3.566(5) . 4_455 no O(5) H(4) 1.8060 . 4 no O(5) H(8) 2.6891 . 4_554 no O(5) N(1) 2.736(5) . 4 no O(5) H(4) 2.9396 . . no O(5) H(3) 3.0162 . 4 no O(5) H(7) 3.0278 . 4 no O(5) H(2) 3.0553 . 4_655 no O(5) O(5) 3.196(4) . 4 no O(5) O(5) 3.196(4) . 4_554 no O(5) N(1) 3.477(6) . . no O(5) N(1) 3.504(6) . 4_655 no O(5) C(2) 3.557(6) . 4 no O(5) C(4) 3.559(6) . 4_654 no O(5) C(4) 3.587(6) . 1_655 no N(1) C(4) 3.346(6) . 1_554 no C(1) H(6) 2.9704 . 1_655 no C(4) H(3) 2.4425 . 1_556 no C(4) H(7) 2.6480 . 4_455 no C(4) H(8) 2.7058 . 1_455 no H(2) H(8) 2.6772 . 4_454 no H(3) H(7) 2.5060 . 4_454 no H(4) H(8) 2.3325 . 4_554 no H(4) H(7) 2.4968 . 4_554 no H(7) H(8) 2.3122 . 4_554 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ag(1) Ag(1) O(1) C(1) . . . . -16.4(4) no Ag(1) Ag(1) O(2) C(1) . . . . 6.6(4) no Ag(1) O(1) C(1) O(2) . . . . -17.5(7) no Ag(1) O(1) C(1) C(2) . . . . 159.9(3) no Ag(1) O(2) C(1) O(1) . . . . -4.1(7) no Ag(1) O(2) C(1) C(2) . . . . 173.4(3) no O(1) Ag(1) Ag(1) O(1) . . . . 180.0000 no O(1) Ag(1) Ag(1) O(2) . . . . -8.6(2) no O(1) Ag(1) O(2) C(1) . . . . -33.7(7) no O(1) C(1) C(2) N(1) . . . . -4.0(6) no O(1) C(1) C(2) C(3) . . . . 120.4(5) no O(2) Ag(1) Ag(1) O(2) . . . . -180.0000 no O(2) Ag(1) Ag(1) O(3) . . . . 68.2(2) no O(2) Ag(1) O(1) C(1) . . . . -43.6(7) no O(2) C(1) C(2) N(1) . . . . 173.7(4) no O(2) C(1) C(2) C(3) . . . . -61.9(6) no O(3) C(4) C(3) C(2) . . . . -158.8(4) no O(4) C(4) C(3) C(2) . . . . 19.3(7) no N(1) C(2) C(3) C(4) . . . . -63.0(5) no C(1) C(2) C(3) C(4) . . . . 173.7(4) no #------------------------------------------------------------------------------ #============================================================================== data_{[Ag(gly)]2H2O}n _database_code_CSD 178115 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ? _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 8.905(2) _cell_length_b 6.404(2) _cell_length_c 15.355(1) _cell_angle_alpha 90 _cell_angle_beta 97.86(1) _cell_angle_gamma 90 _cell_volume 867.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _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 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.924 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 381.87 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H10 Ag2 N2 O5 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 728.00 _exptl_absorpt_coefficient_mu 44.94 _exptl_absorpt_correction_type ; ¥y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.490 _exptl_special_details ; The scan width was (1.31+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_% 2.28 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 2 -1 2 3 -1 1 1 _diffrn_reflns_number 2308 _reflns_number_total 2174 _reflns_number_gt 1569 _reflns_threshold_expression I>2.00¥s(I) _diffrn_reflns_av_R_equivalents 0.02490 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04986 _diffrn_orient_matrix_UB_12 0.00425 _diffrn_orient_matrix_UB_13 0.05450 _diffrn_orient_matrix_UB_21 0.10179 _diffrn_orient_matrix_UB_22 -0.00096 _diffrn_orient_matrix_UB_23 0.03674 _diffrn_orient_matrix_UB_31 0.00198 _diffrn_orient_matrix_UB_32 0.15608 _diffrn_orient_matrix_UB_33 -0.00126 #------------------------------------------------------------------------------ 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 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 20 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ag 0 8 -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) -0.35555(4) 0.24798(7) -0.07520(2) 0.0378(1) 1.000 . Uani d ? Ag(2) -1.17235(4) 0.13495(7) -0.23744(2) 0.0385(1) 1.000 . Uani d ? O(1) -0.8426(4) 0.2338(8) -0.2682(2) 0.046(1) 1.000 . Uani d ? O(2) -0.9576(3) 0.1255(6) -0.1565(2) 0.0365(9) 1.000 . Uani d ? O(3) -1.3925(4) 0.1045(7) -0.3080(2) 0.0399(9) 1.000 . Uani d ? O(4) -1.3306(4) 0.2661(6) -0.4272(2) 0.041(1) 1.000 . Uani d ? O(5) -0.5168(5) 0.2688(8) 0.0690(3) 0.059(1) 1.000 . Uani d ? N(1) -0.1329(4) 0.2080(6) -0.0028(3) 0.0288(9) 1.000 . Uani d ? N(2) -0.5611(4) 0.2449(7) -0.1664(3) 0.035(1) 1.000 . Uani d ? C(1) -0.6956(5) 0.1871(8) -0.1277(3) 0.028(1) 1.000 . Uani d ? C(2) -0.8429(5) 0.1850(7) -0.1913(3) 0.026(1) 1.000 . Uani d ? C(3) -1.4227(5) 0.1831(7) -0.3844(3) 0.025(1) 1.000 . Uani d ? C(4) -1.5879(5) 0.1628(7) -0.4243(3) 0.027(1) 1.000 . Uani d ? H(1) -0.0586 0.2212 -0.0411 0.035 1.000 . Uiso c ? H(3) -0.5768 0.3805 -0.1909 0.042 1.000 . Uiso c ? H(4) -0.5493 0.1477 -0.2118 0.042 1.000 . Uiso c ? H(5) -0.6800 0.0500 -0.1036 0.033 1.000 . Uiso c ? H(6) -0.7067 0.2825 -0.0819 0.033 1.000 . Uiso c ? H(7) -1.6498 0.1580 -0.3787 0.033 1.000 . Uiso c ? H(8) -1.6012 0.0386 -0.4582 0.033 1.000 . Uiso c ? H(2) -0.1254 0.0702 0.0227 0.035 1.000 . Uiso c ? 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) 0.0195(2) 0.0576(3) 0.0329(2) -0.0020(2) -0.0084(1) -0.0013(2) Ag(2) 0.0213(2) 0.0599(3) 0.0317(2) 0.0005(2) -0.0059(1) 0.0057(2) O(1) 0.025(2) 0.087(3) 0.024(2) -0.004(2) -0.004(1) 0.009(2) O(2) 0.020(1) 0.055(2) 0.032(2) -0.001(2) -0.003(1) 0.007(2) O(3) 0.021(2) 0.068(2) 0.028(2) -0.001(2) -0.007(1) 0.007(2) O(4) 0.021(2) 0.062(2) 0.039(2) -0.001(2) 0.002(1) 0.014(2) O(5) 0.038(2) 0.104(4) 0.033(2) -0.003(2) -0.003(2) -0.001(2) N(1) 0.015(2) 0.042(2) 0.027(2) 0.001(2) -0.004(1) 0.000(2) N(2) 0.021(2) 0.055(3) 0.028(2) -0.002(2) -0.002(1) 0.004(2) C(1) 0.017(2) 0.044(3) 0.019(2) -0.000(2) -0.004(1) 0.002(2) C(2) 0.020(2) 0.030(2) 0.025(2) 0.000(2) -0.002(2) -0.003(2) C(3) 0.018(2) 0.032(2) 0.022(2) -0.000(2) -0.001(2) -0.002(2) C(4) 0.022(2) 0.039(2) 0.021(2) -0.003(2) 0.000(2) 0.002(2) #============================================================================== # 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) + 0.00063|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000118(3) _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 1569 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_all 0.0430 _refine_ls_wR_factor_ref 0.0430 _refine_ls_goodness_of_fit_all 1.237 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_shift/su_max 0.3186 _refine_ls_shift/su_mean 0.0087 _refine_diff_density_min -1.36 _refine_diff_density_max 0.95 #============================================================================== # 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) N(1) 2.152(4) . . ? Ag(1) N(2) 2.147(4) . . ? Ag(2) O(2) 2.134(4) . . ? Ag(2) O(3) 2.115(4) . . ? O(1) C(2) 1.222(6) . . ? O(2) C(2) 1.275(6) . . ? O(3) C(3) 1.271(6) . . ? O(4) C(3) 1.238(6) . . ? N(1) C(4) 1.471(6) . . ? N(1) H(1) 0.95 . . no N(1) H(2) 0.96 . . no N(2) C(1) 1.455(6) . . ? N(2) H(3) 0.95 . . no N(2) H(4) 0.95 . . no C(1) C(2) 1.524(7) . . ? C(1) H(5) 0.96 . . no C(1) H(6) 0.95 . . no C(3) C(4) 1.520(7) . . ? C(4) H(7) 0.95 . . no C(4) H(8) 0.95 . . 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 N(1) Ag(1) N(2) 168.2(2) . . . ? O(2) Ag(2) O(3) 171.7(2) . . . ? Ag(2) O(2) C(2) 116.9(3) . . . ? Ag(2) O(3) C(3) 120.0(3) . . . ? Ag(1) N(1) C(4) 119.0(3) . . . ? Ag(1) N(1) H(1) 109.9 . . . no Ag(1) N(1) H(2) 109.1 . . . no C(4) N(1) H(1) 108.8 4_655 4_655 4_655 no C(4) N(1) H(2) 100.7 4_655 4_655 4_655 no H(1) N(1) H(2) 108.6 . . . no Ag(1) N(2) C(1) 114.3(3) . . . ? Ag(1) N(2) H(3) 108.4 . . . no Ag(1) N(2) H(4) 108.3 . . . no C(1) N(2) H(3) 108.0 . . . no C(1) N(2) H(4) 108.2 . . . no H(3) N(2) H(4) 109.5 . . . no N(2) C(1) C(2) 115.1(4) . . . ? N(2) C(1) H(5) 107.9 . . . no N(2) C(1) H(6) 108.4 . . . no C(2) C(1) H(5) 107.8 . . . no C(2) C(1) H(6) 108.3 . . . no H(5) C(1) H(6) 109.2 . . . no O(1) C(2) O(2) 126.2(5) . . . ? O(1) C(2) C(1) 120.1(4) . . . ? O(2) C(2) C(1) 113.7(4) . . . ? O(3) C(3) O(4) 126.0(4) . . . ? O(3) C(3) C(4) 114.1(4) . . . ? O(4) C(3) C(4) 119.8(4) . . . ? N(1) C(4) C(3) 115.0(4) 4_354 4_354 4_354 ? N(1) C(4) H(7) 120.1 4_354 4_354 4_354 no N(1) C(4) H(8) 91.3 4_354 4_354 4_354 no C(3) C(4) H(7) 109.4 . . . no C(3) C(4) H(8) 109.5 . . . no H(7) C(4) H(8) 109.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(5) 2.802(5) . . no Ag(1) Ag(2) 3.2408(7) . 1_655 no Ag(1) O(5) 3.303(6) . 3_465 no Ag(1) O(4) 3.501(4) . 2_344 no Ag(1) O(5) 3.505(6) . 3_455 no Ag(2) O(3) 3.123(5) . 2_254 no Ag(2) O(4) 3.457(5) . 2_244 no Ag(2) C(3) 3.487(5) . 2_244 no Ag(2) Ag(2) 3.488(1) . 2_254 no Ag(2) Ag(2) 3.488(1) . 2_244 no Ag(2) O(3) 3.500(5) . 2_244 no Ag(2) O(5) 3.502(5) . 4_454 no O(1) H(3) 2.4306 . 2_344 no O(1) H(7) 2.6187 . 1_655 no O(1) O(5) 2.756(6) . 4_454 no O(1) H(4) 2.8224 . 2_354 no O(1) H(5) 2.8499 . 2_354 no O(1) C(1) 3.353(7) . 2_354 no O(1) N(2) 3.364(7) . 2_344 no O(1) C(2) 3.427(7) . 2_354 no O(1) N(2) 3.495(7) . 2_354 no O(1) C(4) 3.547(6) . 1_655 no O(2) H(1) 2.1824 . 1_455 no O(2) H(2) 2.4329 . 3_455 no O(2) H(3) 2.8719 . 2_344 no O(2) N(1) 3.049(5) . 1_455 no O(2) C(3) 3.121(6) . 2_244 no O(2) C(4) 3.217(7) . 2_244 no O(2) N(1) 3.263(6) . 3_455 no O(2) O(4) 3.342(6) . 2_244 no O(2) O(3) 3.361(6) . 2_254 no O(3) H(4) 2.1846 . 1_455 no O(3) N(2) 2.947(6) . 1_455 no O(3) C(2) 3.573(7) . 2_244 no O(4) H(2) 2.4376 . 2_354 no O(4) H(1) 2.4934 . 4_354 no O(4) H(8) 2.6422 . 3_254 no O(4) H(6) 2.7698 . 4_454 no O(4) N(1) 2.787(5) . 4_354 no O(4) O(5) 2.812(6) . 4_454 no O(4) H(2) 2.8335 . 4_354 no O(4) N(1) 3.029(6) . 2_354 no O(4) C(1) 3.468(6) . 4_454 no O(4) C(4) 3.580(7) . 3_254 no O(5) H(6) 2.6758 . . no O(5) H(5) 2.6956 . 3_455 no O(5) H(3) 2.9695 . 3_465 no O(5) C(1) 3.258(7) . . no O(5) N(2) 3.484(8) . 3_465 no O(5) C(1) 3.528(8) . 3_455 no O(5) N(2) 3.585(7) . . no N(1) H(2) 2.9582 . 3 no N(1) H(5) 2.9860 . 3_455 no N(1) N(1) 3.557(9) . 3 no N(1) C(3) 3.569(7) . 2_354 no N(2) C(2) 3.597(7) . 2_354 no C(1) H(2) 2.9259 . 3_455 no C(2) H(3) 2.6894 . 2_344 no C(3) H(1) 2.6136 . 4_354 no C(3) H(2) 2.6614 . 4_354 no C(3) H(8) 2.8358 . 3_254 no C(3) H(4) 3.0271 . 1_455 no C(4) H(2) 1.9032 . 4_354 no C(4) H(1) 1.9901 . 4_354 no C(4) H(8) 2.9296 . 3_254 no C(4) H(6) 3.0552 . 2_244 no H(1) H(2) 2.4743 . 3 no H(1) H(8) 2.4825 . 2_354 no H(4) H(7) 2.5967 . 1_655 no H(5) H(2) 2.3930 . 3_455 no H(6) H(8) 2.5068 . 2_254 no H(7) H(2) 2.3362 . 4_354 no H(8) H(8) 2.4025 . 3_254 no H(8) H(2) 2.5278 . 4_354 no H(2) H(2) 2.5899 . 3 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ag(1) N(2) C(1) C(2) . . . . 179.7(4) no Ag(2) O(2) C(2) O(1) . . . . -5.2(7) no Ag(2) O(2) C(2) C(1) . . . . 176.2(3) no Ag(2) O(3) C(3) O(4) . . . . 6.1(8) no Ag(2) O(3) C(3) C(4) . . . . -175.8(3) no O(1) C(2) C(1) N(2) . . . . -1.5(8) no O(2) Ag(2) O(3) C(3) . . . . -154.7(9) no O(2) C(2) C(1) N(2) . . . . 177.2(4) no O(3) Ag(2) O(2) C(2) . . . . 144.2(9) no O(3) C(3) C(4) N(1) . . . . 166.8(4) no O(4) C(3) C(4) N(1) . . . . -15.0(7) no N(1) Ag(1) N(2) C(1) . . . . 125.1(8) no N(2) Ag(1) N(1) C(4) . . . . 172.8(7) no #------------------------------------------------------------------------------ #============================================================================== data_[Ag(L-asn)]n _database_code_CSD 178154 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 7.4245(9) _cell_length_b 8.019(2) _cell_length_c 21.537(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1282.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 10.6 _cell_measurement_theta_max 14.1 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' _symmetry_Int_Tables_number 20 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, -y, -z' ' -x, -y,1/2+z' ' -x, +y,1/2-z' '1/2+x,1/2+y, +z' '1/2+x,1/2-y, -z' '1/2-x,1/2-y,1/2+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 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.476 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 238.98 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H7 Ag N2 O3 ' _chemical_formula_moiety 'C4 H7 Ag N2 O3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 928.00 _exptl_absorpt_coefficient_mu 30.78 _exptl_absorpt_correction_type ; ¥y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.832 _exptl_special_details ; The scan width was (1.05+0.30tan¥q)¥% with an ¥w scan speed of 2¥% 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_% -2.29 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -3 2 -4 -4 1 -1 -2 _diffrn_reflns_number 3133 _reflns_number_total 2929 _reflns_number_gt 2560 _reflns_threshold_expression I>2.00¥s(I) _diffrn_reflns_av_R_equivalents 0.01690 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.61 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05970 _diffrn_orient_matrix_UB_12 0.01809 _diffrn_orient_matrix_UB_13 -0.04107 _diffrn_orient_matrix_UB_21 0.11920 _diffrn_orient_matrix_UB_22 -0.02845 _diffrn_orient_matrix_UB_23 0.01885 _diffrn_orient_matrix_UB_31 -0.01922 _diffrn_orient_matrix_UB_32 -0.12007 _diffrn_orient_matrix_UB_33 -0.01066 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 56 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ag 0 8 -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) 0.62080(3) 0.06387(3) 0.57617(1) 0.03433(5) 1.000 . Uani d ? O(1) 0.8892(3) 0.0072(2) 0.59906(9) 0.0329(5) 1.000 . Uani d ? O(2) 0.9967(3) 0.2243(3) 0.5449(1) 0.0348(6) 1.000 . Uani d ? O(3) 1.1467(3) 0.2376(2) 0.68931(9) 0.0371(6) 1.000 . Uani d ? N(1) 1.3485(2) 0.1468(3) 0.5715(1) 0.0233(5) 1.000 . Uani d ? N(2) 1.2348(4) 0.0524(4) 0.7619(1) 0.0412(7) 1.000 . Uani d ? C(1) 1.0162(3) 0.0969(3) 0.5762(1) 0.0222(6) 1.000 . Uani d ? C(2) 1.2067(3) 0.0267(3) 0.5886(1) 0.0207(6) 1.000 . Uani d ? C(3) 1.2298(3) -0.0356(3) 0.6543(1) 0.0232(6) 1.000 . Uani d ? C(4) 1.2014(3) 0.0966(3) 0.7032(1) 0.0270(7) 1.000 . Uani d ? H(1) 1.2213 -0.0673 0.5623 0.025 1.000 . Uiso c ? H(2) 1.3303 0.1830 0.5300 0.028 1.000 . Uiso c ? H(3) 1.3438 0.2400 0.5987 0.028 1.000 . Uiso c ? H(4) 1.1453 -0.1226 0.6613 0.028 1.000 . Uiso c ? H(5) 1.3485 -0.0782 0.6587 0.028 1.000 . Uiso c ? H(6) 1.2188 0.1310 0.7944 0.049 1.000 . Uiso c ? H(7) 1.2738 -0.0575 0.7710 0.049 1.000 . Uiso c ? 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) 0.01549(8) 0.0426(1) 0.0449(1) 0.0011(1) -0.0003(1) -0.0005(1) O(1) 0.0171(8) 0.0327(9) 0.049(1) -0.0006(8) 0.0005(9) 0.0029(8) O(2) 0.027(1) 0.040(1) 0.038(1) 0.0045(9) -0.0051(8) 0.015(1) O(3) 0.053(1) 0.025(1) 0.033(1) 0.007(1) -0.001(1) -0.0021(8) N(1) 0.0157(9) 0.0259(9) 0.028(1) 0.0007(8) 0.004(1) 0.0016(9) N(2) 0.062(2) 0.036(1) 0.026(1) 0.008(2) -0.009(1) -0.005(1) C(1) 0.022(1) 0.025(1) 0.020(1) -0.0011(9) -0.003(1) -0.004(1) C(2) 0.015(1) 0.023(1) 0.024(1) 0.0013(9) 0.0001(9) -0.000(1) C(3) 0.021(1) 0.021(1) 0.028(1) 0.004(1) -0.001(1) 0.002(1) C(4) 0.026(1) 0.029(2) 0.026(1) -0.000(1) -0.001(1) 0.005(1) #============================================================================== # 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) + 0.00010|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 -0.0093(2) _refine_ls_number_reflns 2560 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_all 0.0240 _refine_ls_wR_factor_ref 0.0240 _refine_ls_goodness_of_fit_all 1.165 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.43 _refine_diff_density_max 0.39 #============================================================================== # 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) O(1) 2.103(2) . . ? Ag(1) N(1) 2.131(2) . . ? O(1) C(1) 1.284(3) . . ? O(2) C(1) 1.233(3) . . ? O(3) C(4) 1.238(4) . . ? N(1) C(2) 1.474(3) . . ? N(1) H(2) 0.95 . . no N(1) H(3) 0.95 . . no N(2) C(4) 1.336(4) . . ? N(2) H(6) 0.95 . . no N(2) H(7) 0.95 . . no C(1) C(2) 1.546(3) . . ? C(2) C(3) 1.510(4) . . ? C(2) H(1) 0.95 . . no C(3) C(4) 1.510(4) . . ? C(3) H(4) 0.95 . . no C(3) H(5) 0.95 . . 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 O(1) Ag(1) N(1) 167.93(9) . . . ? Ag(1) O(1) C(1) 119.0(2) . . . ? Ag(1) N(1) C(2) 117.5(2) 1_655 1_655 1_655 ? Ag(1) N(1) H(2) 106.0 1_655 1_655 1_655 no Ag(1) N(1) H(3) 104.5 1_655 1_655 1_655 no C(2) N(1) H(2) 109.5 . . . no C(2) N(1) H(3) 109.5 . . . no H(2) N(1) H(3) 109.6 . . . no C(4) N(2) H(6) 119.8 . . . no C(4) N(2) H(7) 119.9 . . . no H(6) N(2) H(7) 120.2 . . . no O(1) C(1) O(2) 126.0(2) . . . ? O(1) C(1) C(2) 113.7(2) . . . ? O(2) C(1) C(2) 120.3(2) . . . ? N(1) C(2) C(1) 111.8(2) . . . ? N(1) C(2) C(3) 111.7(2) . . . ? N(1) C(2) H(1) 106.7 . . . no C(1) C(2) C(3) 112.8(2) . . . ? C(1) C(2) H(1) 106.8 . . . no C(3) C(2) H(1) 106.5 . . . no C(2) C(3) C(4) 113.9(2) . . . ? C(2) C(3) H(4) 108.5 . . . no C(2) C(3) H(5) 108.5 . . . no C(4) C(3) H(4) 108.2 . . . no C(4) C(3) H(5) 108.2 . . . no H(4) C(3) H(5) 109.4 . . . no O(3) C(4) N(2) 122.2(3) . . . ? O(3) C(4) C(3) 121.2(3) . . . ? N(2) C(4) C(3) 116.6(3) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(2) 2.952(2) . 5_445 no Ag(1) O(2) 3.244(2) . 6_456 no Ag(1) Ag(1) 3.4371(9) . 2_556 no Ag(1) O(3) 3.580(2) . 5_445 no O(1) H(3) 2.1689 . 5_445 no O(1) H(6) 2.6248 . 4_756 no O(1) N(1) 2.966(3) . 5_445 no O(1) H(2) 3.0266 . 5_445 no O(1) N(2) 3.153(4) . 4_756 no O(1) O(3) 3.419(3) . 5_445 no O(2) H(2) 2.1636 . 6_456 no O(2) H(1) 2.6674 . 5_455 no O(2) N(1) 2.925(3) . 6_456 no O(2) C(2) 3.377(4) . 5_455 no O(3) H(7) 1.9433 . 8_756 no O(3) H(5) 2.7418 . 5_455 no O(3) H(6) 2.8666 . 4_756 no O(3) N(2) 2.872(4) . 8_756 no O(3) N(2) 3.367(4) . 4_756 no O(3) O(3) 3.403(4) . 4_756 no N(2) C(4) 3.343(4) . 4_756 no N(2) N(2) 3.524(6) . 4_756 no C(3) H(6) 2.9172 . 8_746 no C(4) H(7) 2.8341 . 8_756 no H(1) H(2) 2.3384 . 2_556 no H(4) H(6) 2.4145 . 8_746 no H(5) H(6) 2.5894 . 8_746 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ag(1) O(1) C(1) O(2) . . . . 5.9(4) no Ag(1) O(1) C(1) C(2) . . . . -171.4(2) no O(1) C(1) C(2) N(1) . . . . -170.0(2) no O(1) C(1) C(2) C(3) . . . . -43.0(3) no O(2) C(1) C(2) N(1) . . . . 12.5(4) no O(2) C(1) C(2) C(3) . . . . 139.4(3) no O(3) C(4) C(3) C(2) . . . . 6.7(4) no N(1) C(2) C(3) C(4) . . . . 66.8(3) no N(2) C(4) C(3) C(2) . . . . -174.6(2) no C(1) C(2) C(3) C(4) . . . . -60.2(3) no #------------------------------------------------------------------------------ #============================================================================== data_[Ag(D-asn)]n _database_code_CSD 178155 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 7.422(2) _cell_length_b 8.011(3) _cell_length_c 21.526(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1279.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.7 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' _symmetry_Int_Tables_number 20 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, -y, -z' ' -x, -y,1/2+z' ' -x, +y,1/2-z' '1/2+x,1/2+y, +z' '1/2+x,1/2-y, -z' '1/2-x,1/2-y,1/2+z' '1/2-x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 238.98 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H7 Ag N2 O3 ' _chemical_formula_moiety 'C4 H7 Ag N2 O3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 928.00 _exptl_absorpt_coefficient_mu 30.83 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.890 _exptl_special_details ; The scan width was (1.52+0.30tan\q)\% with an \w scan speed of 2\% 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_% -1.15 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 0 0 2 3 0 2 -6 _diffrn_reflns_number 869 _reflns_number_total 856 _reflns_number_gt 785 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02269 _diffrn_orient_matrix_UB_12 0.11315 _diffrn_orient_matrix_UB_13 -0.01799 _diffrn_orient_matrix_UB_21 0.02882 _diffrn_orient_matrix_UB_22 0.05206 _diffrn_orient_matrix_UB_23 0.04104 _diffrn_orient_matrix_UB_31 0.12964 _diffrn_orient_matrix_UB_32 0.00823 _diffrn_orient_matrix_UB_33 -0.01227 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 56 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 24 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ag 0 8 -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) 0.12011(4) -0.43654(4) -0.07620(1) 0.03191(8) 1.000 . Uani d ? O(1) 0.3892(4) -0.4935(4) -0.0989(2) 0.0325(7) 1.000 . Uani d ? O(2) 0.4961(4) -0.2762(4) -0.0446(1) 0.0335(7) 1.000 . Uani d ? O(3) 0.6461(5) -0.2631(3) -0.1891(1) 0.0339(7) 1.000 . Uani d ? N(1) 0.8474(4) -0.3546(4) -0.0714(1) 0.0220(7) 1.000 . Uani d ? N(2) 0.7346(7) -0.4493(4) -0.2618(2) 0.039(1) 1.000 . Uani d ? C(1) 0.5151(5) -0.4033(4) -0.0763(2) 0.0206(8) 1.000 . Uani d ? C(2) 0.7066(5) -0.4734(4) -0.0885(2) 0.0172(8) 1.000 . Uani d ? C(3) 0.7290(5) -0.5366(4) -0.1542(2) 0.0215(8) 1.000 . Uani d ? C(4) 0.7016(5) -0.4043(5) -0.2034(2) 0.0255(9) 1.000 . Uani d ? H(1) 0.7204 -0.5676 -0.0614 0.021 1.000 . Uiso c ? H(2) 0.8319 -0.3225 -0.0291 0.026 1.000 . Uiso c ? H(3) 0.8373 -0.2586 -0.0971 0.026 1.000 . Uiso c ? H(4) 0.6418 -0.6236 -0.1613 0.026 1.000 . Uiso c ? H(5) 0.8462 -0.5838 -0.1586 0.026 1.000 . Uiso c ? H(6) 0.7724 -0.5606 -0.2702 0.044 1.000 . Uiso c ? H(7) 0.7227 -0.3713 -0.2944 0.044 1.000 . Uiso c ? 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) 0.0136(1) 0.0391(2) 0.0431(2) 0.0010(1) 0.0004(1) 0.0007(1) O(1) 0.014(1) 0.032(1) 0.051(2) -0.003(1) -0.002(1) -0.002(1) O(2) 0.022(1) 0.042(2) 0.036(1) 0.005(1) 0.002(1) -0.012(1) O(3) 0.050(2) 0.023(1) 0.029(1) 0.007(1) 0.001(1) 0.002(1) N(1) 0.012(1) 0.025(1) 0.029(1) -0.000(1) -0.001(1) -0.002(1) N(2) 0.058(2) 0.035(2) 0.024(2) 0.004(2) 0.004(2) -0.003(1) C(1) 0.018(2) 0.024(1) 0.020(2) 0.000(1) 0.002(1) 0.002(1) C(2) 0.010(1) 0.019(2) 0.023(2) 0.003(1) -0.000(1) 0.000(1) C(3) 0.023(2) 0.020(2) 0.021(1) 0.004(1) 0.004(1) -0.004(1) C(4) 0.024(2) 0.026(2) 0.026(2) -0.002(1) 0.001(1) -0.003(1) #============================================================================== # 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) + 0.00026|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000151 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.0683(2) _refine_ls_number_reflns 785 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0171 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_all 0.0280 _refine_ls_wR_factor_ref 0.0280 _refine_ls_goodness_of_fit_all 1.191 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.34 _refine_diff_density_max 0.33 #============================================================================== # 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) O(1) 2.106(3) . . ? Ag(1) N(1) 2.131(3) . . ? O(1) C(1) 1.276(5) . . ? O(2) C(1) 1.235(5) . . ? O(3) C(4) 1.243(5) . . ? N(1) C(2) 1.460(5) . . ? N(1) H(2) 0.95 . . no N(1) H(3) 0.95 . . no N(2) C(4) 1.329(5) . . ? N(2) H(6) 0.95 . . no N(2) H(7) 0.94 . . no C(1) C(2) 1.551(5) . . ? C(2) C(3) 1.512(5) . . ? C(2) H(1) 0.96 . . no C(3) C(4) 1.512(5) . . ? C(3) H(4) 0.96 . . no C(3) H(5) 0.95 . . 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 O(1) Ag(1) N(1) 168.2(1) . . . ? Ag(1) O(1) C(1) 118.9(3) . . . ? Ag(1) N(1) C(2) 117.8(2) 1_655 1_655 1_655 ? Ag(1) N(1) H(2) 104.1 1_655 1_655 1_655 no Ag(1) N(1) H(3) 107.2 1_655 1_655 1_655 no C(2) N(1) H(2) 109.3 . . . no C(2) N(1) H(3) 109.0 . . . no H(2) N(1) H(3) 109.1 . . . no C(4) N(2) H(6) 119.2 . . . no C(4) N(2) H(7) 120.4 . . . no H(6) N(2) H(7) 120.4 . . . no O(1) C(1) O(2) 126.4(4) . . . ? O(1) C(1) C(2) 113.7(3) . . . ? O(2) C(1) C(2) 119.8(3) . . . ? N(1) C(2) C(1) 112.2(3) . . . ? N(1) C(2) C(3) 112.0(3) . . . ? N(1) C(2) H(1) 106.5 . . . no C(1) C(2) C(3) 112.3(3) . . . ? C(1) C(2) H(1) 106.3 . . . no C(3) C(2) H(1) 107.1 . . . no C(2) C(3) C(4) 114.0(3) . . . ? C(2) C(3) H(4) 108.4 . . . no C(2) C(3) H(5) 109.0 . . . no C(4) C(3) H(4) 107.8 . . . no C(4) C(3) H(5) 109.4 . . . no H(4) C(3) H(5) 108.1 . . . no O(3) C(4) N(2) 122.8(4) . . . ? O(3) C(4) C(3) 120.6(4) . . . ? N(2) C(4) C(3) 116.6(4) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ag(1) O(2) 2.952(4) . 5_445 no Ag(1) O(2) 3.242(3) . 6_445 no Ag(1) Ag(1) 3.4343(8) . 2_545 no Ag(1) O(3) 3.576(3) . 5_445 no O(1) H(3) 2.1594 . 5_445 no O(1) H(7) 2.6320 . 4_654 no O(1) N(1) 2.970(5) . 5_445 no O(1) N(2) 3.157(5) . 4_654 no O(1) O(3) 3.419(5) . 5_445 no O(2) H(2) 2.1496 . 6_445 no O(2) H(1) 2.6665 . 5_455 no O(2) N(1) 2.924(5) . 6_445 no O(2) C(2) 3.376(5) . 5_455 no O(2) N(1) 3.600(5) . 5_455 no O(3) H(6) 1.9409 . 8_654 no O(3) H(5) 2.7299 . 5_455 no O(3) N(2) 2.868(5) . 8_654 no O(3) H(7) 2.8938 . 4_654 no O(3) N(2) 3.366(6) . 4_654 no O(3) O(3) 3.403(7) . 4_654 no N(2) C(4) 3.342(7) . 4_654 no N(2) N(2) 3.52(1) . 4_654 no C(3) H(7) 2.9230 . 8_644 no C(4) H(6) 2.8184 . 8_654 no H(1) H(2) 2.2914 . 2_545 no H(4) H(7) 2.4205 . 8_644 no H(5) H(7) 2.5677 . 8_644 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ag(1) O(1) C(1) O(2) . . . . -4.8(5) no Ag(1) O(1) C(1) C(2) . . . . 171.4(2) no O(1) C(1) C(2) N(1) . . . . 170.4(3) no O(1) C(1) C(2) C(3) . . . . 43.2(4) no O(2) C(1) C(2) N(1) . . . . -13.1(5) no O(2) C(1) C(2) C(3) . . . . -140.4(3) no O(3) C(4) C(3) C(2) . . . . -7.4(6) no N(1) C(2) C(3) C(4) . . . . -66.6(4) no N(2) C(4) C(3) C(2) . . . . 174.5(4) no C(1) C(2) C(3) C(4) . . . . 60.7(4) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================