# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1873 data_1 #====================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. C. S. 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@info.kanagawa-u.ac.jp ' #====================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and crystal structure of three silver(I) complexes with (S)-(+)-5-oxo-2-tetrahydrofuran carboxylic acid (S-Hothf) and its isomeric forms (R-Hothf and R,S-Hothf) showing wide spectra of effective antibacterial and antifungal activities. Chiral helical polymers in the solid-state formed by self-assembly of the dimeric [Ag(othf)]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 Hiratsuka, Kanagawa 259-1293, Japan ; ' Satoshi Takahashi ' ; Department of Materials Science, Kanagawa University Hiratsuka, Kanagawa 259-1293, Japan ; ' Ryusuke Noguchi ' ; Department of Materials Science, Kanagawa University 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' _computing_structure_solution "DIRDIF92 PATTY (Beurskens, 1992)" _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.564(2) _cell_length_b 5.416(2) _cell_length_c 12.867(2) _cell_angle_alpha 90 _cell_angle_beta 109.34(1) _cell_angle_gamma 90 _cell_volume 628.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.1 _cell_measurement_theta_max 14.6 #------------------------------------------------------------------------------ _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 '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 2.503 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 473.92 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Ag2 O8 ' _chemical_formula_moiety 'C10 H10 Ag2 O8 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 456.00 _exptl_absorpt_coefficient_mu 3.140 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_correction_T_min 0.879 _exptl_special_details ; The scan width was (1.42+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_% -0.10 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 1 0 2 -2 -1 1 -1 _diffrn_reflns_number 1683 _reflns_number_total 1593 _reflns_number_gt 1158 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.02057 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.09876 _diffrn_orient_matrix_UB_12 0.02562 _diffrn_orient_matrix_UB_13 -0.05787 _diffrn_orient_matrix_UB_21 -0.04788 _diffrn_orient_matrix_UB_22 0.00565 _diffrn_orient_matrix_UB_23 0.05826 _diffrn_orient_matrix_UB_31 0.01532 _diffrn_orient_matrix_UB_32 0.18278 _diffrn_orient_matrix_UB_33 0.00631 #------------------------------------------------------------------------------ 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 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 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) -0.32464(7) -0.4754(2) -0.29021(5) 0.0519(2) Uani d . 1.00 . Ag(1a) -0.16576(6) -0.0292 -0.27193(5) 0.0431(2) Uani d . 1.00 . O(1) -0.5037(6) -0.251(1) -0.3962(5) 0.045(2) Uani d . 1.00 . O(2) -0.4007(5) 0.099(1) -0.3151(4) 0.045(2) Uani d . 1.00 . O(3) -0.8863(6) -0.361(1) -0.5658(5) 0.061(2) Uani d . 1.00 . O(4) -0.7474(5) -0.023(1) -0.5209(3) 0.042(1) Uani d . 1.00 . O(1a) 0.0245(6) -0.272(1) -0.1923(4) 0.041(2) Uani d . 1.00 . O(2a) -0.1063(5) -0.6085(9) -0.1805(4) 0.040(2) Uani d . 1.00 . O(3a) 0.4619(7) -0.299(1) -0.0992(5) 0.086(3) Uani d . 1.00 . O(4a) 0.2731(5) -0.556(1) -0.1436(4) 0.044(2) Uani d . 1.00 . C(2) -0.8241(8) -0.208(2) -0.4985(7) 0.041(3) Uani d . 1.00 . C(3) -0.8174(9) -0.191(2) -0.3802(7) 0.044(3) Uani d . 1.00 . C(4) -0.7480(8) 0.053(2) -0.3418(6) 0.045(2) Uani d . 1.00 . C(5) -0.6595(8) 0.095(1) -0.4204(6) 0.039(2) Uani d . 1.00 . C(6) -0.5086(7) -0.027(2) -0.3753(6) 0.038(2) Uani d . 1.00 . C(2a) 0.3626(8) -0.390(2) -0.0754(7) 0.047(3) Uani d . 1.00 . C(3a) 0.315(1) -0.353(2) 0.0230(7) 0.064(3) Uani d . 1.00 . C(4a) 0.2084(9) -0.564(2) 0.0178(6) 0.051(3) Uani d . 1.00 . C(5a) 0.1544(8) -0.628(1) -0.1040(6) 0.038(2) Uani d . 1.00 . C(6a) 0.0128(7) -0.487(2) -0.1650(5) 0.029(2) Uani d . 1.00 . H(1) 0.1371 -0.8021 -0.1133 0.042 Uiso calc . 1.00 . H(2) 0.2604 -0.1962 0.0233 0.075 Uiso calc . 1.00 . H(3) 0.3936 -0.3524 0.0947 0.075 Uiso calc . 1.00 . H(4) -0.7559 -0.3222 -0.3336 0.052 Uiso calc . 1.00 . H(5) -0.9133 -0.2075 -0.3702 0.052 Uiso calc . 1.00 . H(6) -0.8246 0.1818 -0.3532 0.051 Uiso calc . 1.00 . H(7) -0.6872 0.0613 -0.2677 0.051 Uiso calc . 1.00 . H(8) 0.1302 -0.5202 0.0447 0.061 Uiso calc . 1.00 . H(9) 0.2627 -0.6994 0.0628 0.061 Uiso calc . 1.00 . H(10) -0.6500 0.2734 -0.4314 0.045 Uiso calc . 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) 0.0459(4) 0.0307(4) 0.0659(5) 0.0030(3) 0.0008(3) 0.0013(4) Ag(1a) 0.0395(3) 0.0325(4) 0.0531(4) 0.0038(3) 0.0096(3) 0.0056(4) O(1) 0.037(3) 0.024(3) 0.065(4) 0.004(3) 0.003(3) -0.013(3) O(2) 0.032(3) 0.034(3) 0.057(4) 0.000(3) -0.001(3) 0.000(3) O(3) 0.047(4) 0.072(5) 0.067(4) -0.023(3) 0.024(3) -0.033(4) O(4) 0.030(2) 0.057(4) 0.032(3) -0.002(4) 0.001(2) -0.001(4) O(1a) 0.039(3) 0.031(3) 0.052(4) -0.002(3) 0.014(3) 0.010(3) O(2a) 0.031(3) 0.038(3) 0.049(3) -0.003(2) 0.008(3) 0.007(3) O(3a) 0.050(4) 0.100(6) 0.099(5) -0.030(4) 0.012(4) 0.025(5) O(4a) 0.037(3) 0.061(4) 0.037(3) 0.003(3) 0.015(2) -0.008(3) C(2) 0.027(4) 0.050(6) 0.049(6) 0.001(4) 0.014(4) -0.003(5) C(3) 0.046(5) 0.054(6) 0.041(5) 0.002(5) 0.023(4) 0.002(5) C(4) 0.038(4) 0.055(6) 0.040(5) 0.007(5) 0.009(4) -0.024(5) C(5) 0.044(5) 0.028(4) 0.040(5) 0.001(4) 0.005(4) -0.001(4) C(6) 0.025(4) 0.049(5) 0.037(4) -0.001(5) 0.009(3) -0.010(6) C(2a) 0.033(5) 0.043(6) 0.054(6) -0.002(4) -0.002(4) 0.012(5) C(3a) 0.074(7) 0.056(7) 0.039(5) 0.021(6) -0.010(5) -0.012(5) C(4a) 0.058(5) 0.070(7) 0.025(4) 0.016(6) 0.011(4) 0.014(5) C(5a) 0.032(4) 0.026(4) 0.054(5) 0.005(3) 0.013(4) 0.014(4) C(6a) 0.042(4) 0.023(4) 0.024(4) -0.004(4) 0.014(3) -0.009(4) #====================================================================== # 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) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000045(4) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.013 _refine_ls_number_reflns 1158 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_all 0.0190 _refine_ls_wR_factor_ref 0.0190 _refine_ls_goodness_of_fit_all 1.317 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.55 _refine_diff_density_max 0.46 #====================================================================== # 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(1a) Ag(1) 2.822(1) 1_555 1_555 yes Ag(1a) O(2) 2.240(5) 1_555 1_555 yes Ag(1a) O(3) 2.475(6) 1_555 1_555 yes Ag(1a) O(1a) 2.203(6) 1_555 1_555 yes Ag(1) O(1) 2.173(6) 1_555 1_555 yes Ag(1) O(2) 2.404(6) 1_555 1_555 yes Ag(1) O(2a) 2.218(5) 1_555 1_555 yes O(1) C(6) 1.25(1) 1_555 1_555 yes O(2) C(6) 1.27(1) 1_555 1_555 yes O(3) C(2) 1.20(1) 1_555 1_555 yes O(4) C(2) 1.33(1) 1_555 1_555 yes O(4) C(5) 1.438(9) 1_555 1_555 yes O(1a) C(6a) 1.24(1) 1_555 1_555 yes O(2a) C(6a) 1.271(9) 1_555 1_555 yes O(3a) C(2a) 1.20(1) 1_555 1_555 yes O(4a) C(2a) 1.35(1) 1_555 1_555 yes O(4a) C(5a) 1.443(9) 1_555 1_555 yes C(2) C(3) 1.51(1) 1_555 1_555 yes C(3) C(4) 1.49(1) 1_555 1_555 yes C(3) H(4) 0.99 1_555 1_555 no C(3) H(5) 0.97 1_555 1_555 no C(4) C(5) 1.54(1) 1_555 1_555 yes C(4) H(6) 0.99 1_555 1_555 no C(4) H(7) 0.94 1_555 1_555 no C(5) C(6) 1.52(1) 1_555 1_555 yes C(5) H(10) 0.99 1_555 1_555 no C(2a) C(3a) 1.49(1) 1_555 1_555 yes C(3a) C(4a) 1.52(1) 1_555 1_555 yes C(3a) H(2) 1.00 1_555 1_555 no C(3a) H(3) 0.98 1_555 1_555 no C(4a) C(5a) 1.52(1) 1_555 1_555 yes C(4a) H(8) 0.95 1_555 1_555 no C(4a) H(9) 0.97 1_555 1_555 no C(5a) C(6a) 1.53(1) 1_555 1_555 yes C(5a) H(1) 0.96 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(1a) O(2) 77.1(2) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(3) 119.9(2) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(1a) 82.4(2) 1_555 1_555 1_555 yes O(2) Ag(1a) O(3) 98.1(2) 1_555 1_555 1_555 yes O(2) Ag(1a) O(1a) 155.2(2) 1_555 1_555 1_555 yes O(3) Ag(1a) O(1a) 104.2(2) 2_454 2_454 2_454 yes Ag(1a) Ag(1) O(1) 82.2(2) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(2) 164.1(1) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(2a) 81.8(1) 1_555 1_555 1_555 yes O(1) Ag(1) O(2) 108.1(2) 1_555 1_555 1_555 yes O(1) Ag(1) O(2a) 164.0(2) 1_555 1_555 1_555 yes O(2) Ag(1) O(2a) 87.3(2) 1_545 1_545 1_545 yes Ag(1) O(1) C(6) 119.1(6) 1_555 1_555 1_555 yes Ag(1a) O(2) Ag(1) 91.7(2) 1_555 1_555 1_555 yes Ag(1a) O(2) C(6) 122.0(6) 1_555 1_555 1_555 yes Ag(1) O(2) C(6) 138.5(6) 1_565 1_565 1_565 yes Ag(1a) O(3) C(2) 132.1(6) 2_444 2_444 2_444 yes C(2) O(4) C(5) 110.0(7) 1_555 1_555 1_555 yes Ag(1a) O(1a) C(6a) 123.9(6) 1_555 1_555 1_555 yes Ag(1) O(2a) C(6a) 122.5(6) 1_555 1_555 1_555 yes C(2a) O(4a) C(5a) 110.8(7) 1_555 1_555 1_555 yes O(3) C(2) O(4) 122.7(9) 1_555 1_555 1_555 yes O(3) C(2) C(3) 128(1) 1_555 1_555 1_555 yes O(4) C(2) C(3) 109.4(8) 1_555 1_555 1_555 yes C(2) C(3) C(4) 104.8(9) 1_555 1_555 1_555 yes C(2) C(3) H(4) 112.7 1_555 1_555 1_555 no C(2) C(3) H(5) 113.7 1_555 1_555 1_555 no C(4) C(3) H(4) 109.1 1_555 1_555 1_555 no C(4) C(3) H(5) 112.0 1_555 1_555 1_555 no H(4) C(3) H(5) 104.7 1_555 1_555 1_555 no C(3) C(4) C(5) 101.2(8) 1_555 1_555 1_555 yes C(3) C(4) H(6) 110.5 1_555 1_555 1_555 no C(3) C(4) H(7) 115.8 1_555 1_555 1_555 no C(5) C(4) H(6) 110.1 1_555 1_555 1_555 no C(5) C(4) H(7) 111.8 1_555 1_555 1_555 no H(6) C(4) H(7) 107.3 1_555 1_555 1_555 no O(4) C(5) C(4) 103.9(7) 1_555 1_555 1_555 yes O(4) C(5) C(6) 110.4(7) 1_555 1_555 1_555 yes O(4) C(5) H(10) 111.2 1_555 1_555 1_555 no C(4) C(5) C(6) 110.3(7) 1_555 1_555 1_555 yes C(4) C(5) H(10) 109.6 1_555 1_555 1_555 no C(6) C(5) H(10) 111.2 1_555 1_555 1_555 no O(1) C(6) O(2) 125.3(9) 1_555 1_555 1_555 yes O(1) C(6) C(5) 116.1(8) 1_555 1_555 1_555 yes O(2) C(6) C(5) 118(1) 1_555 1_555 1_555 yes O(3a) C(2a) O(4a) 120(1) 1_555 1_555 1_555 yes O(3a) C(2a) C(3a) 131(1) 1_555 1_555 1_555 yes O(4a) C(2a) C(3a) 109.4(8) 1_555 1_555 1_555 yes C(2a) C(3a) C(4a) 104.6(8) 1_555 1_555 1_555 yes C(2a) C(3a) H(2) 115.0 1_555 1_555 1_555 no C(2a) C(3a) H(3) 116.2 1_555 1_555 1_555 no C(4a) C(3a) H(2) 107.5 1_555 1_555 1_555 no C(4a) C(3a) H(3) 109.9 1_555 1_555 1_555 no H(2) C(3a) H(3) 103.4 1_555 1_555 1_555 no C(3a) C(4a) C(5a) 102.1(8) 1_555 1_555 1_555 yes C(3a) C(4a) H(8) 113.0 1_555 1_555 1_555 no C(3a) C(4a) H(9) 108.8 1_555 1_555 1_555 no C(5a) C(4a) H(8) 113.1 1_555 1_555 1_555 no C(5a) C(4a) H(9) 112.1 1_555 1_555 1_555 no H(8) C(4a) H(9) 107.7 1_555 1_555 1_555 no O(4a) C(5a) C(4a) 105.3(7) 1_555 1_555 1_555 yes O(4a) C(5a) C(6a) 110.6(7) 1_555 1_555 1_555 yes O(4a) C(5a) H(1) 110.2 1_555 1_555 1_555 no C(4a) C(5a) C(6a) 111.0(7) 1_555 1_555 1_555 yes C(4a) C(5a) H(1) 109.8 1_555 1_555 1_555 no C(6a) C(5a) H(1) 109.8 1_555 1_555 1_555 no O(1a) C(6a) O(2a) 127.2(8) 1_555 1_555 1_555 yes O(1a) C(6a) C(5a) 118.0(8) 1_555 1_555 1_555 yes O(2a) C(6a) C(5a) 114.8(8) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #====================================================================== # End of CIF #====================================================================== data_2 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _cell_length_a 9.560(2) _cell_length_b 5.417(2) _cell_length_c 12.858(2) _cell_angle_alpha 90 _cell_angle_beta 109.37(1) _cell_angle_gamma 90 _cell_volume 628.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.3 #------------------------------------------------------------------------------ _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 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.506 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 473.92 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Ag2 O8 ' _chemical_formula_moiety 'C10 H10 Ag2 O8 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 456.00 _exptl_absorpt_coefficient_mu 3.144 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.863 _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_% -0.71 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 1 2 -1 0 2 -1 2 _diffrn_reflns_number 1682 _reflns_number_total 1592 _reflns_number_gt 973 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03461 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.10882 _diffrn_orient_matrix_UB_12 0.02617 _diffrn_orient_matrix_UB_13 0.01676 _diffrn_orient_matrix_UB_21 0.01378 _diffrn_orient_matrix_UB_22 0.00835 _diffrn_orient_matrix_UB_23 0.08048 _diffrn_orient_matrix_UB_31 0.01623 _diffrn_orient_matrix_UB_32 -0.18257 _diffrn_orient_matrix_UB_33 0.00608 #------------------------------------------------------------------------------ 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 Ag 0 4 -1.085 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 20 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #====================================================================== # 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) 0.3246(1) 0.4602 0.28999(8) 0.0512(3) Uani d . 1.00 . Ag(1a) 0.16553(9) 0.0140(2) 0.27173(7) 0.0427(3) Uani d . 1.00 . O(1) 0.5040(9) 0.233(2) 0.3971(7) 0.046(3) Uani d . 1.00 . O(2) 0.4031(8) -0.111(1) 0.3142(6) 0.038(2) Uani d . 1.00 . O(3) 0.8867(9) 0.342(2) 0.5665(7) 0.061(3) Uani d . 1.00 . O(4) 0.7473(7) 0.004(2) 0.5206(5) 0.041(2) Uani d . 1.00 . O(1a) -0.0249(9) 0.257(2) 0.1929(7) 0.040(2) Uani d . 1.00 . O(2a) 0.1059(8) 0.595(1) 0.1807(6) 0.040(2) Uani d . 1.00 . O(3a) -0.461(1) 0.288(2) 0.0988(8) 0.085(4) Uani d . 1.00 . O(4a) -0.2721(8) 0.544(2) 0.1439(6) 0.039(2) Uani d . 1.00 . C(2) 0.827(1) 0.193(3) 0.498(1) 0.043(4) Uani d . 1.00 . C(3) 0.818(1) 0.174(3) 0.379(1) 0.046(4) Uani d . 1.00 . C(4) 0.747(1) -0.073(3) 0.342(1) 0.049(4) Uani d . 1.00 . C(5) 0.658(1) -0.112(2) 0.419(1) 0.040(4) Uani d . 1.00 . C(6) 0.508(1) 0.016(3) 0.3760(8) 0.032(3) Uani d . 1.00 . C(2a) -0.361(1) 0.374(3) 0.075(1) 0.047(4) Uani d . 1.00 . C(3a) -0.316(2) 0.336(3) -0.024(1) 0.056(5) Uani d . 1.00 . C(4a) -0.207(1) 0.547(3) -0.0181(9) 0.055(4) Uani d . 1.00 . C(5a) -0.153(1) 0.615(2) 0.106(1) 0.040(4) Uani d . 1.00 . C(6a) -0.011(1) 0.479(3) 0.1661(8) 0.036(3) Uani d . 1.00 . H(1) 0.7581 0.3138 0.3318 0.053 Uiso calc . 1.00 . H(2) 0.9145 0.1947 0.3686 0.053 Uiso calc . 1.00 . H(3) -0.3920 0.3508 -0.0979 0.079 Uiso calc . 1.00 . H(4) -0.2606 0.1879 -0.0287 0.079 Uiso calc . 1.00 . H(5) -0.1242 0.5049 -0.0429 0.062 Uiso calc . 1.00 . H(6) -0.2560 0.6876 -0.0659 0.062 Uiso calc . 1.00 . H(7) 0.6841 -0.0684 0.2672 0.054 Uiso calc . 1.00 . H(8) 0.8222 -0.1914 0.3511 0.054 Uiso calc . 1.00 . H(9) -0.1397 0.7948 0.1092 0.042 Uiso calc . 1.00 . H(10) 0.6484 -0.2844 0.4308 0.041 Uiso calc . 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) 0.0469(6) 0.0280(6) 0.0660(8) 0.0031(5) 0.0018(5) 0.0019(6) Ag(1a) 0.0401(5) 0.0313(6) 0.0517(6) 0.0035(5) 0.0087(4) 0.0041(5) O(1) 0.039(5) 0.021(5) 0.071(7) 0.007(4) 0.009(5) -0.017(4) O(2) 0.037(4) 0.019(4) 0.048(6) -0.008(3) -0.001(4) -0.004(4) O(3) 0.052(6) 0.077(8) 0.056(6) -0.020(5) 0.019(5) -0.029(6) O(4) 0.032(4) 0.053(5) 0.030(4) -0.004(5) 0.002(3) 0.007(6) O(1a) 0.038(5) 0.028(5) 0.050(5) -0.000(4) 0.011(4) 0.010(4) O(2a) 0.032(4) 0.032(5) 0.046(5) -0.003(4) 0.001(4) -0.003(4) O(3a) 0.066(7) 0.082(8) 0.100(9) -0.020(7) 0.018(7) 0.022(7) O(4a) 0.038(4) 0.041(5) 0.039(5) 0.001(4) 0.015(4) -0.002(5) C(2) 0.029(7) 0.039(8) 0.07(1) 0.007(6) 0.026(7) -0.001(8) C(3) 0.046(8) 0.055(9) 0.06(1) 0.006(7) 0.041(8) 0.003(8) C(4) 0.042(7) 0.052(9) 0.041(8) 0.025(7) -0.002(6) -0.022(7) C(5) 0.039(7) 0.019(7) 0.056(9) 0.004(5) 0.005(6) 0.002(6) C(6) 0.030(5) 0.038(7) 0.025(6) -0.011(7) 0.004(5) 0.001(7) C(2a) 0.036(8) 0.046(9) 0.051(9) -0.006(6) 0.002(6) 0.012(7) C(3a) 0.065(9) 0.06(1) 0.041(9) 0.024(8) 0.006(8) -0.005(8) C(4a) 0.059(8) 0.08(1) 0.026(6) 0.023(9) 0.011(6) 0.004(8) C(5a) 0.043(7) 0.028(7) 0.049(8) -0.001(6) 0.014(6) 0.012(6) C(6a) 0.033(6) 0.033(7) 0.036(7) 0.007(7) 0.004(5) -0.007(7) #====================================================================== # 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 -0.0013 _refine_ls_number_reflns 973 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_all 0.0260 _refine_ls_wR_factor_ref 0.0260 _refine_ls_goodness_of_fit_all 1.256 _refine_ls_goodness_of_fit_ref 1.260 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.56 _refine_diff_density_max 0.71 #====================================================================== # 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) 2.823(2) 1_555 1_555 yes Ag(1) O(1) 2.187(9) 1_555 1_555 yes Ag(1) O(2) 2.431(8) 1_555 1_555 yes Ag(1) O(2a) 2.219(8) 1_555 1_555 yes Ag(1a) O(1a) 2.203(9) 1_555 1_555 yes Ag(1a) O(2) 2.256(8) 1_555 1_555 yes Ag(1a) O(3) 2.477(9) 1_555 1_555 yes O(1) C(6) 1.21(2) 1_555 1_555 yes O(1a) C(6a) 1.27(2) 1_555 1_555 yes O(2) C(6) 1.26(1) 1_555 1_555 yes O(2a) C(6a) 1.24(1) 1_555 1_555 yes O(3) C(2) 1.19(2) 1_555 1_555 yes O(3a) C(2a) 1.20(2) 1_555 1_555 yes O(4) C(2) 1.36(2) 1_555 1_555 yes O(4) C(5) 1.45(1) 1_555 1_555 yes O(4a) C(2a) 1.36(2) 1_555 1_555 yes O(4a) C(5a) 1.43(1) 1_555 1_555 yes C(2) C(3) 1.51(2) 1_555 1_555 yes C(2a) C(3a) 1.48(2) 1_555 1_555 yes C(3) C(4) 1.50(2) 1_555 1_555 yes C(3) H(1) 1.02 1_555 1_555 no C(3) H(2) 0.98 1_555 1_555 no C(3a) C(4a) 1.53(2) 1_555 1_555 yes C(3a) H(3) 0.99 1_555 1_555 no C(3a) H(4) 0.98 1_555 1_555 no C(4) C(5) 1.52(2) 1_555 1_555 yes C(4) H(7) 0.95 1_555 1_555 no C(4) H(8) 0.94 1_555 1_555 no C(4a) C(5a) 1.55(2) 1_555 1_555 yes C(4a) H(5) 0.97 1_555 1_555 no C(4a) H(6) 0.99 1_555 1_555 no C(5) C(6) 1.52(2) 1_555 1_555 yes C(5) H(10) 0.95 1_555 1_555 no C(5a) C(6a) 1.51(2) 1_555 1_555 yes C(5a) H(9) 0.98 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) 81.9(2) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(2) 164.6(2) 1_555 1_555 1_555 yes Ag(1a) Ag(1) O(2a) 82.0(2) 1_555 1_555 1_555 yes O(1) Ag(1) O(2) 108.2(3) 1_555 1_555 1_555 yes O(1) Ag(1) O(2a) 163.8(3) 1_555 1_555 1_555 yes O(2) Ag(1) O(2a) 87.3(3) 1_565 1_565 1_565 ? Ag(1) Ag(1a) O(1a) 82.3(2) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(2) 76.4(2) 1_555 1_555 1_555 yes Ag(1) Ag(1a) O(3) 120.4(3) 1_555 1_555 1_555 yes O(1a) Ag(1a) O(2) 154.5(3) 1_555 1_555 1_555 yes O(1a) Ag(1a) O(3) 104.2(3) 1_555 1_555 1_555 yes O(2) Ag(1a) O(3) 98.7(3) 1_555 1_555 1_555 yes Ag(1) O(1) C(6) 118.9(9) 1_555 1_555 1_555 yes Ag(1a) O(1a) C(6a) 123.1(8) 1_555 1_555 1_555 yes Ag(1) O(2) Ag(1a) 90.7(3) 1_545 1_545 1_545 ? Ag(1) O(2) C(6) 138.6(9) 1_545 1_545 1_545 ? Ag(1a) O(2) C(6) 121.3(9) 1_555 1_555 1_555 yes Ag(1) O(2a) C(6a) 122.9(9) 1_555 1_555 1_555 yes Ag(1a) O(3) C(2) 134(1) 2_656 2_656 2_656 ? C(2) O(4) C(5) 110(1) 1_555 1_555 1_555 yes C(2a) O(4a) C(5a) 111(1) 1_555 1_555 1_555 yes O(3) C(2) O(4) 121(1) 1_555 1_555 1_555 yes O(3) C(2) C(3) 131(2) 1_555 1_555 1_555 yes O(4) C(2) C(3) 109(1) 1_555 1_555 1_555 yes O(3a) C(2a) O(4a) 118(2) 1_555 1_555 1_555 yes O(3a) C(2a) C(3a) 131(2) 1_555 1_555 1_555 yes O(4a) C(2a) C(3a) 111(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 104(1) 1_555 1_555 1_555 yes C(2) C(3) H(1) 112.5 1_555 1_555 1_555 no C(2) C(3) H(2) 112.6 1_555 1_555 1_555 no C(4) C(3) H(1) 111.8 1_555 1_555 1_555 no C(4) C(3) H(2) 114.1 1_555 1_555 1_555 no H(1) C(3) H(2) 101.6 1_555 1_555 1_555 no C(2a) C(3a) C(4a) 104(1) 1_555 1_555 1_555 yes C(2a) C(3a) H(3) 119.0 1_555 1_555 1_555 no C(2a) C(3a) H(4) 119.1 1_555 1_555 1_555 no C(4a) C(3a) H(3) 104.8 1_555 1_555 1_555 no C(4a) C(3a) H(4) 104.0 1_555 1_555 1_555 no H(3) C(3a) H(4) 104.1 1_555 1_555 1_555 no C(3) C(4) C(5) 102(1) 1_555 1_555 1_555 yes C(3) C(4) H(7) 111.2 1_555 1_555 1_555 no C(3) C(4) H(8) 108.5 1_555 1_555 1_555 no C(5) C(4) H(7) 111.4 1_555 1_555 1_555 no C(5) C(4) H(8) 113.1 1_555 1_555 1_555 no H(7) C(4) H(8) 110.1 1_555 1_555 1_555 no C(3a) C(4a) C(5a) 102(1) 1_555 1_555 1_555 yes C(3a) C(4a) H(5) 114.9 1_555 1_555 1_555 no C(3a) C(4a) H(6) 111.6 1_555 1_555 1_555 no C(5a) C(4a) H(5) 111.4 1_555 1_555 1_555 no C(5a) C(4a) H(6) 112.6 1_555 1_555 1_555 no H(5) C(4a) H(6) 104.2 1_555 1_555 1_555 no O(4) C(5) C(4) 104(1) 1_555 1_555 1_555 yes O(4) C(5) C(6) 109(1) 1_555 1_555 1_555 yes O(4) C(5) H(10) 110.2 1_555 1_555 1_555 no C(4) C(5) C(6) 111(1) 1_555 1_555 1_555 yes C(4) C(5) H(10) 110.0 1_555 1_555 1_555 no C(6) C(5) H(10) 112.1 1_555 1_555 1_555 no O(4a) C(5a) C(4a) 105(1) 1_555 1_555 1_555 yes O(4a) C(5a) C(6a) 112(1) 1_555 1_555 1_555 yes O(4a) C(5a) H(9) 111.2 1_555 1_555 1_555 no C(4a) C(5a) C(6a) 110(1) 1_555 1_555 1_555 yes C(4a) C(5a) H(9) 105.9 1_555 1_555 1_555 no C(6a) C(5a) H(9) 112.4 1_555 1_555 1_555 no O(1) C(6) O(2) 126(1) 1_555 1_555 1_555 yes O(1) C(6) C(5) 117(1) 1_555 1_555 1_555 yes O(2) C(6) C(5) 116(1) 1_555 1_555 1_555 yes O(1a) C(6a) O(2a) 127(1) 1_555 1_555 1_555 yes O(1a) C(6a) C(5a) 116(1) 1_555 1_555 1_555 yes O(2a) C(6a) C(5a) 116(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #====================================================================== # End of CIF #====================================================================== data_3 #====================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997) ' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 23.766(4) _cell_length_b 5.466(1) _cell_length_c 10.128(1) _cell_angle_alpha 90 _cell_angle_beta 102.58(1) _cell_angle_gamma 90 _cell_volume 1284.2(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 'C 2/c ' _symmetry_Int_Tables_number 15 _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' ' -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' '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 'cubic' _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 2.451 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 473.92 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Ag2 O8 ' _chemical_formula_moiety 'C10 H10 Ag2 O8 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 912.00 _exptl_absorpt_coefficient_mu 3.075 _exptl_absorpt_correction_type ; "\y scans (North,Phillips & Matthews, 1968)" ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.833 _exptl_special_details ; The scan width was (1.73+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_% -0.21 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 1 3 -3 1 3 -5 1 3 _diffrn_reflns_number 1666 _reflns_number_total 1627 _reflns_number_gt 1090 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.01710 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00194 _diffrn_orient_matrix_UB_12 0.00175 _diffrn_orient_matrix_UB_13 0.09764 _diffrn_orient_matrix_UB_21 0.04081 _diffrn_orient_matrix_UB_22 -0.05832 _diffrn_orient_matrix_UB_23 0.02539 _diffrn_orient_matrix_UB_31 0.01376 _diffrn_orient_matrix_UB_32 0.17339 _diffrn_orient_matrix_UB_33 0.00754 #------------------------------------------------------------------------------ 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 40 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)" ; O 0 32 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) 0.52301(2) 0.20895(7) -0.04614(4) 0.0575(2) Uani d . 1.00 . O(1) 0.5659(1) -0.0249(5) -0.1680(3) 0.0397(8) Uani d . 1.00 . O(2) 0.5352(1) 0.6395(6) -0.0820(3) 0.0500(9) Uani d . 1.00 . O(3) 0.6781(2) -0.014(1) -0.3774(4) 0.092(2) Uani d . 1.00 . O(4) 0.6139(1) -0.2839(6) -0.3367(3) 0.0464(9) Uani d . 1.00 . C(2) 0.6640(2) -0.156(1) -0.3002(4) 0.047(1) Uani d . 1.00 . C(3) 0.6947(2) -0.226(1) -0.1626(5) 0.053(1) Uani d . 1.00 . C(4) 0.6620(2) -0.444(1) -0.1270(5) 0.062(2) Uani d . 1.00 . C(5) 0.6025(2) -0.4099(7) -0.2198(4) 0.044(1) Uani d . 1.00 . C(6) 0.5645(2) -0.2515(7) -0.1516(4) 0.036(1) Uani d . 1.00 . H(1) 0.7338 -0.2633 -0.1615 0.060 Uiso calc . 1.00 . H(2) 0.6938 -0.0934 -0.1006 0.060 Uiso calc . 1.00 . H(3) 0.6792 -0.5960 -0.1479 0.072 Uiso calc . 1.00 . H(4) 0.6601 -0.4481 -0.0345 0.072 Uiso calc . 1.00 . H(5) 0.5845 -0.5613 -0.2462 0.052 Uiso calc . 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) 0.0785(3) 0.0284(2) 0.0816(3) 0.0059(2) 0.0528(2) 0.0009(2) O(1) 0.045(2) 0.029(2) 0.050(2) -0.001(1) 0.022(1) -0.001(1) O(2) 0.064(2) 0.027(1) 0.075(2) 0.004(1) 0.050(2) 0.008(1) O(3) 0.083(3) 0.132(4) 0.062(2) -0.049(3) 0.020(2) 0.028(2) O(4) 0.042(2) 0.062(2) 0.039(2) -0.013(1) 0.018(1) -0.005(1) C(2) 0.038(2) 0.064(3) 0.042(2) -0.013(2) 0.016(2) -0.002(2) C(3) 0.040(2) 0.078(4) 0.045(2) 0.009(2) 0.016(2) 0.001(2) C(4) 0.068(3) 0.059(3) 0.071(3) 0.036(3) 0.039(3) 0.022(2) C(5) 0.060(3) 0.025(2) 0.060(2) -0.002(2) 0.041(2) -0.005(2) C(6) 0.039(2) 0.030(2) 0.044(2) 0.002(1) 0.019(2) 0.001(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) + 0.00090|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 1090 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_all 0.0550 _refine_ls_wR_factor_ref 0.0550 _refine_ls_goodness_of_fit_all 1.439 _refine_ls_goodness_of_fit_ref 1.440 _refine_ls_shift/su_max 0.0200 _refine_ls_shift/su_mean 0.0032 _refine_diff_density_min -1.18 _refine_diff_density_max 0.83 #====================================================================== # 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) 2.781(1) 1_555 1_555 yes Ag(1) O(1) 2.178(3) 1_555 1_555 yes Ag(1) O(2) 2.408(4) 1_555 1_555 yes Ag(1) O(2) 2.250(3) 1_555 1_555 yes O(1) C(6) 1.251(6) 1_555 1_555 yes O(2) C(6) 1.246(6) 1_555 1_555 yes O(3) C(2) 1.201(7) 1_555 1_555 yes O(4) C(2) 1.362(6) 1_555 1_555 yes O(4) C(5) 1.445(6) 1_555 1_555 yes C(2) C(3) 1.475(8) 1_555 1_555 yes C(3) C(4) 1.508(9) 1_555 1_555 yes C(3) H(1) 0.95 1_555 1_555 no C(3) H(2) 0.96 1_555 1_555 no C(4) C(5) 1.529(8) 1_555 1_555 yes C(4) H(3) 0.97 1_555 1_555 no C(4) H(4) 0.95 1_555 1_555 no C(5) C(6) 1.521(6) 1_555 1_555 yes C(5) H(5) 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(1) Ag(1) O(1) 88.57(9) 3_655 3_655 3_655 yes Ag(1) Ag(1) O(2) 157.27(8) 3_655 3_655 3_655 yes Ag(1) Ag(1) O(2) 76.8(1) 3_655 3_655 3_655 yes O(1) Ag(1) O(2) 113.7(1) 1_555 1_555 1_555 yes O(1) Ag(1) O(2) 164.8(1) 1_555 1_555 1_555 yes O(2) Ag(1) O(2) 80.6(1) 1_555 1_555 1_555 yes Ag(1) O(1) C(6) 118.5(3) 1_555 1_555 1_555 yes Ag(1) O(2) Ag(1) 99.4(1) 1_555 1_555 1_555 yes Ag(1) O(2) C(6) 130.8(3) 1_555 1_555 1_555 yes Ag(1) O(2) C(6) 129.8(3) 3_665 3_665 3_665 yes C(2) O(4) C(5) 109.4(4) 1_555 1_555 1_555 yes O(3) C(2) O(4) 120.5(5) 1_555 1_555 1_555 yes O(3) C(2) C(3) 129.3(5) 1_555 1_555 1_555 yes O(4) C(2) C(3) 110.3(5) 1_555 1_555 1_555 yes C(2) C(3) C(4) 104.8(5) 1_555 1_555 1_555 yes C(2) C(3) H(1) 110.3 1_555 1_555 1_555 no C(2) C(3) H(2) 110.3 1_555 1_555 1_555 no C(4) C(3) H(1) 112.4 1_555 1_555 1_555 no C(4) C(3) H(2) 110.6 1_555 1_555 1_555 no H(1) C(3) H(2) 108.4 1_555 1_555 1_555 no C(3) C(4) C(5) 102.3(4) 1_555 1_555 1_555 yes C(3) C(4) H(3) 111.2 1_555 1_555 1_555 no C(3) C(4) H(4) 113.2 1_555 1_555 1_555 no C(5) C(4) H(3) 110.3 1_555 1_555 1_555 no C(5) C(4) H(4) 111.9 1_555 1_555 1_555 no H(3) C(4) H(4) 107.8 1_555 1_555 1_555 no O(4) C(5) C(4) 104.4(4) 1_555 1_555 1_555 yes O(4) C(5) C(6) 109.7(4) 1_555 1_555 1_555 yes O(4) C(5) H(5) 109.9 1_555 1_555 1_555 no C(4) C(5) C(6) 110.5(4) 1_555 1_555 1_555 yes C(4) C(5) H(5) 111.7 1_555 1_555 1_555 no C(6) C(5) H(5) 110.6 1_555 1_555 1_555 no O(1) C(6) O(2) 125.6(5) 1_555 1_555 1_555 yes O(1) C(6) C(5) 117.9(4) 1_555 1_555 1_555 yes O(2) C(6) C(5) 116.5(4) 1_545 1_545 1_545 yes #------------------------------------------------------------------------------ #===================================================================== # End of CIF #======================================================================