Supplementary Material (ESI) for Analyst This journal is © The Royal Society of Chemistry 2001 Summary of Data CCDC 154168 --------------- Authors: I.Yoon,Y.H.Lee,S.S.Lee,S.C.Lee,S.B.Park Compound: C40 H52 Ag2 F6 N1 O7 P1 S4 Unit cell parameters: a 23.8522(15) b 7.5310(4) c 14.0178(8) beta 106.009(2) space group C2 ---------- X-Sun-Data-Type: ciffile X-Sun-Data-Name: 154168.cif X-Sun-Charset: us-ascii X-Sun-Content-Lines: 477 data_[Ag2(I)2(NO3)](PF6) _database_code_CSD 154168 _publ_requested_journal 'The Analyst' _journal_coden_Cambridge ? _publ_contact_author_name 'Prof Shim Sung Lee' _publ_contact_author_address ; Prof Shim Sung Lee Dept of Chemistry & Research Inst of Natural Sciences Gyeongsang National University Chinju 660-701 KOREA ; _publ_contact_author_email 'sslee@nongae.gsnu.ac.kr' loop_ _publ_author_name _publ_author_address 'Il Yoon' ; Department of Chemistry and Research Institute of Natural Sciences, Gyeongsang National University, Chinju 660-701, S. Korea ; 'Yoon Hee Lee' ; Department of Chemistry and Research Institute of Natural Sciences, Gyeongsang National University, Chinju 660-701, S. Korea ; 'Shim Sung Lee' ; Department of Chemistry and Research Institute of Natural Sciences, Gyeongsang National University, Chinju 660-701, S. Korea ; 'Sang Cheol Lee' ; Department of Chemistry, Inje University, Kimhae 621-749, S. Korea ; 'Sung Bae Park' ; Department of Chemistry, Inje University, Kimhae 621-749, S. Korea ; _publ_section_title ; S2O2-donor cyclic and acyclic ionophores for Ag(I), and a new nitrate- bridged dimeric Ag(I) complex of the acyclic ionophore with an unusual structure ; _publ_section_reference ; Siemens, SMART and SAINT. Area detector Control and Intergration Software. Version 4.0, Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 1996. G. M. Sheldrick, SHELXTL. Structure Determination Programs. Version 5.03, Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 1996. ; _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Ag2 F6 N O7 P S4' _chemical_formula_weight 1147.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 23.8522(15) _cell_length_b 7.5310(4) _cell_length_c 14.0178(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.009(2) _cell_angle_gamma 90.00 _cell_volume 2420.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used 7809 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 28.29 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Siemens, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7809 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4790 _reflns_number_gt 4355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SHELXTL (Sheldrick, 1996)' _computing_structure_solution 'SHELXTL' _computing_structure_refinement 'SHELXTL' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.7979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4790 _refine_ls_number_parameters 277 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max '< 0.001' _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag -0.474998(10) -0.31201(4) -0.871806(18) 0.06213(10) Uani 1 1 d . . . S1 S -0.37487(4) -0.44195(16) -0.80448(7) 0.0617(2) Uani 1 1 d . . . S2 S -0.57150(4) -0.46300(13) -0.93093(7) 0.0571(2) Uani 1 1 d . . . O1 O -0.43001(14) -0.1707(5) -0.6905(2) 0.0797(9) Uani 1 1 d . . . O2 O -0.54661(14) -0.1184(5) -0.7982(3) 0.0761(8) Uani 1 1 d . . . C1 C -0.2882(3) -0.7837(9) -0.7407(5) 0.0915(16) Uani 1 1 d . . . H1 H -0.2900 -0.7435 -0.8065 0.110 Uiso 1 1 calc R . . C2 C -0.2390(3) -0.8718(9) -0.6852(6) 0.109(2) Uani 1 1 d . . . H2 H -0.2071 -0.8910 -0.7133 0.131 Uiso 1 1 calc R . . C3 C -0.2348(4) -0.9316(10) -0.5921(6) 0.115(3) Uani 1 1 d . . . H3 H -0.2001 -0.9914 -0.5548 0.138 Uiso 1 1 calc R . . C4 C -0.2802(4) -0.9060(10) -0.5522(5) 0.112(2) Uani 1 1 d . . . H4 H -0.2780 -0.9502 -0.4870 0.134 Uiso 1 1 calc R . . C5 C -0.3303(2) -0.8148(11) -0.6066(3) 0.0873(13) Uani 1 1 d . . . H5 H -0.3619 -0.7946 -0.5777 0.105 Uiso 1 1 calc R . . C6 C -0.3345(2) -0.7534(6) -0.7022(3) 0.0698(11) Uani 1 1 d . . . C7 C -0.38929(19) -0.6625(7) -0.7613(4) 0.0691(10) Uani 1 1 d . . . H7A H -0.4157 -0.6512 -0.7209 0.083 Uiso 1 1 calc R . . H7B H -0.4078 -0.7347 -0.8176 0.083 Uiso 1 1 calc R . . C8 C -0.34504(16) -0.3238(8) -0.6898(3) 0.0676(9) Uani 1 1 d . . . H8A H -0.3140 -0.3934 -0.6485 0.081 Uiso 1 1 calc R . . H8B H -0.3284 -0.2145 -0.7044 0.081 Uiso 1 1 calc R . . C9 C -0.3875(2) -0.2823(7) -0.6330(3) 0.0719(12) Uani 1 1 d . . . H9A H -0.4051 -0.3897 -0.6181 0.086 Uiso 1 1 calc R . . H9B H -0.3681 -0.2250 -0.5716 0.086 Uiso 1 1 calc R . . C10 C -0.4742(3) -0.1338(9) -0.6411(4) 0.0944(17) Uani 1 1 d . . . H10A H -0.4576 -0.0705 -0.5805 0.113 Uiso 1 1 calc R . . H10B H -0.4906 -0.2427 -0.6255 0.113 Uiso 1 1 calc R . . C11 C -0.5187(3) -0.0277(10) -0.7073(4) 0.0998(19) Uani 1 1 d . . . H11A H -0.5476 0.0037 -0.6743 0.120 Uiso 1 1 calc R . . H11B H -0.5015 0.0801 -0.7225 0.120 Uiso 1 1 calc R . . C12 C -0.5963(2) -0.2213(7) -0.7973(4) 0.0810(13) Uani 1 1 d . . . H12A H -0.6255 -0.1466 -0.7829 0.097 Uiso 1 1 calc R . . H12B H -0.5857 -0.3106 -0.7467 0.097 Uiso 1 1 calc R . . C13 C -0.61976(16) -0.3068(8) -0.8960(3) 0.0749(11) Uani 1 1 d . . . H13A H -0.6295 -0.2154 -0.9456 0.090 Uiso 1 1 calc R . . H13B H -0.6552 -0.3673 -0.8964 0.090 Uiso 1 1 calc R . . C14 C -0.57173(16) -0.6511(6) -0.8488(3) 0.0554(8) Uani 1 1 d . . . H14A H -0.5437 -0.7373 -0.8569 0.066 Uiso 1 1 calc R . . H14B H -0.5600 -0.6110 -0.7812 0.066 Uiso 1 1 calc R . . C15 C -0.63049(16) -0.7376(5) -0.8693(3) 0.0579(9) Uani 1 1 d . . . C16 C -0.65435(16) -0.8225(8) -0.9587(3) 0.0663(9) Uani 1 1 d . . . H16 H -0.6337 -0.8213 -1.0085 0.080 Uiso 1 1 calc R . . C17 C -0.7076(2) -0.9096(8) -0.9779(5) 0.0842(14) Uani 1 1 d . . . H17 H -0.7231 -0.9721 -1.0392 0.101 Uiso 1 1 calc R . . C18 C -0.7379(2) -0.9041(9) -0.9068(5) 0.0944(18) Uani 1 1 d . . . H18 H -0.7754 -0.9602 -0.9197 0.113 Uiso 1 1 calc R . . C19 C -0.7151(2) -0.8202(12) -0.8189(5) 0.0970(15) Uani 1 1 d . . . H19 H -0.7364 -0.8186 -0.7700 0.116 Uiso 1 1 calc R . . C20 C -0.6617(2) -0.7376(7) -0.7990(4) 0.0775(12) Uani 1 1 d . . . H20 H -0.6460 -0.6797 -0.7363 0.093 Uiso 1 1 calc R . . O3 O -0.45762(17) -0.0388(7) -0.9484(3) 0.0965(12) Uani 1 1 d . . . O4 O -0.5000 0.2060(8) -1.0000 0.126(2) Uani 1 2 d S . . N N -0.5000 0.0421(6) -1.0000 0.0638(12) Uani 1 2 d S . . P P -0.5000 -0.6220(2) -0.5000 0.0738(5) Uani 1 2 d S . . F1 F -0.5137(2) -0.6217(5) -0.3951(2) 0.1080(12) Uani 1 1 d . . . F2 F -0.5469(2) -0.7727(7) -0.5362(3) 0.159(2) Uani 1 1 d . . . F3 F -0.5470(2) -0.4732(6) -0.5360(3) 0.1237(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.05032(14) 0.07359(19) 0.05996(15) 0.00528(16) 0.01097(10) -0.00286(18) S1 0.0484(5) 0.0804(7) 0.0557(5) -0.0005(4) 0.0133(4) 0.0005(5) S2 0.0534(5) 0.0588(5) 0.0547(4) 0.0097(4) 0.0073(4) -0.0060(4) O1 0.0683(17) 0.093(2) 0.0717(18) -0.0128(17) 0.0084(14) 0.0135(18) O2 0.0615(17) 0.073(2) 0.090(2) -0.0110(16) 0.0140(15) 0.0022(15) C1 0.090(3) 0.082(4) 0.102(3) -0.001(3) 0.026(3) 0.020(3) C2 0.086(4) 0.096(5) 0.144(6) 0.000(4) 0.029(4) 0.028(3) C3 0.105(5) 0.078(4) 0.134(6) 0.000(4) -0.012(5) 0.000(4) C4 0.125(6) 0.098(4) 0.085(4) 0.004(3) -0.019(4) -0.024(4) C5 0.089(3) 0.088(3) 0.076(2) -0.010(3) 0.009(2) -0.019(4) C6 0.074(3) 0.060(2) 0.071(2) -0.0119(17) 0.013(2) -0.0048(19) C7 0.059(2) 0.067(2) 0.079(3) -0.012(2) 0.0143(19) -0.007(2) C8 0.0551(17) 0.071(2) 0.0679(19) -0.002(2) 0.0014(15) -0.004(2) C9 0.076(2) 0.077(3) 0.0571(18) -0.0091(19) 0.0092(17) -0.009(2) C10 0.103(4) 0.102(4) 0.077(3) -0.018(3) 0.022(3) 0.022(3) C11 0.103(4) 0.101(4) 0.086(3) -0.029(3) 0.011(3) 0.026(3) C12 0.069(3) 0.074(3) 0.105(4) 0.005(3) 0.032(3) 0.012(2) C13 0.0502(16) 0.060(2) 0.105(3) 0.013(3) 0.0053(18) 0.006(3) C14 0.0524(18) 0.055(2) 0.0588(18) 0.0099(15) 0.0150(15) 0.0023(16) C15 0.0513(19) 0.0512(18) 0.075(2) 0.0143(17) 0.0244(17) 0.0057(15) C16 0.0552(17) 0.067(2) 0.076(2) 0.006(3) 0.0180(16) 0.003(3) C17 0.074(3) 0.067(3) 0.104(4) 0.008(3) 0.011(3) -0.009(2) C18 0.059(3) 0.092(4) 0.134(5) 0.029(4) 0.029(3) 0.001(3) C19 0.075(3) 0.111(4) 0.123(4) 0.013(5) 0.056(3) -0.002(4) C20 0.080(3) 0.075(3) 0.089(3) 0.002(2) 0.043(3) 0.005(2) O3 0.081(2) 0.110(3) 0.096(2) 0.039(2) 0.0189(19) -0.021(2) O4 0.185(6) 0.049(3) 0.188(6) 0.000 0.123(6) 0.000 N 0.092(4) 0.047(3) 0.064(3) 0.000 0.041(3) 0.000 P 0.1175(14) 0.0581(9) 0.0554(7) 0.000 0.0400(8) 0.000 F1 0.171(4) 0.101(2) 0.0711(16) 0.0131(16) 0.066(2) 0.025(2) F2 0.227(5) 0.138(4) 0.142(4) -0.047(3) 0.102(4) -0.095(4) F3 0.151(4) 0.128(3) 0.099(3) 0.034(2) 0.045(3) 0.051(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag O3 2.409(4) . yes Ag S2 2.4952(10) . yes Ag S1 2.5117(10) . yes S1 C8 1.803(4) . ? S1 C7 1.832(5) . ? S2 C13 1.805(5) . ? S2 C14 1.826(4) . ? O1 C9 1.390(6) . ? O1 C10 1.437(7) . ? O2 C12 1.418(6) . ? O2 C11 1.437(6) . ? C1 C6 1.375(8) . ? C1 C2 1.386(9) . ? C2 C3 1.358(11) . ? C3 C4 1.364(12) . ? C4 C5 1.407(10) . ? C5 C6 1.395(7) . ? C6 C7 1.506(6) . ? C8 C9 1.485(6) . ? C10 C11 1.444(9) . ? C12 C13 1.489(8) . ? C14 C15 1.500(5) . ? C15 C16 1.381(7) . ? C15 C20 1.390(6) . ? C16 C17 1.389(7) . ? C17 C18 1.384(8) . ? C18 C19 1.358(10) . ? C19 C20 1.374(8) . ? O3 N 1.230(5) . ? O4 N 1.235(8) . ? N O3 1.230(5) 2_453 ? P F3 1.567(4) 2_454 ? P F3 1.567(4) . ? P F2 1.575(4) 2_454 ? P F2 1.575(4) . ? P F1 1.592(3) . ? P F1 1.592(3) 2_454 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ag S2 119.83(9) . . yes O3 Ag S1 103.75(10) . . yes S2 Ag S1 129.92(4) . . yes C8 S1 C7 102.5(2) . . ? C8 S1 Ag 104.08(16) . . ? C7 S1 Ag 103.39(14) . . ? C13 S2 C14 102.8(2) . . ? C13 S2 Ag 102.23(17) . . ? C14 S2 Ag 107.88(12) . . ? C9 O1 C10 110.6(4) . . ? C12 O2 C11 115.8(5) . . ? C6 C1 C2 120.5(6) . . ? C3 C2 C1 121.7(7) . . ? C2 C3 C4 119.4(7) . . ? C3 C4 C5 119.9(7) . . ? C6 C5 C4 120.5(6) . . ? C1 C6 C5 118.0(5) . . ? C1 C6 C7 121.9(5) . . ? C5 C6 C7 120.0(5) . . ? C6 C7 S1 112.4(3) . . ? C9 C8 S1 115.0(3) . . ? O1 C9 C8 108.2(4) . . ? O1 C10 C11 107.8(5) . . ? O2 C11 C10 112.7(5) . . ? O2 C12 C13 109.2(4) . . ? C12 C13 S2 115.4(3) . . ? C15 C14 S2 112.4(3) . . ? C16 C15 C20 118.4(4) . . ? C16 C15 C14 120.3(4) . . ? C20 C15 C14 121.3(4) . . ? C15 C16 C17 121.4(4) . . ? C18 C17 C16 118.5(5) . . ? C19 C18 C17 120.6(5) . . ? C18 C19 C20 120.8(5) . . ? C19 C20 C15 120.3(5) . . ? N O3 Ag 118.1(3) . . ? O3 N O3 120.6(6) 2_453 . ? O3 N O4 119.7(3) 2_453 . ? O3 N O4 119.7(3) . . ? F3 P F3 88.7(4) 2_454 . ? F3 P F2 91.7(3) 2_454 2_454 ? F3 P F2 179.5(3) . 2_454 ? F3 P F2 179.5(3) 2_454 . ? F3 P F2 91.7(3) . . ? F2 P F2 87.8(5) 2_454 . ? F3 P F1 90.7(2) 2_454 . ? F3 P F1 89.2(2) . . ? F2 P F1 90.7(2) 2_454 . ? F2 P F1 89.4(2) . . ? F3 P F1 89.2(2) 2_454 2_454 ? F3 P F1 90.7(2) . 2_454 ? F2 P F1 89.4(2) 2_454 2_454 ? F2 P F1 90.7(2) . 2_454 ? F1 P F1 179.9(4) . 2_454 ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C10 C11 O2 61.8(8) . . . . yes O1 C9 C8 S1 -62.6(5) . . . . yes O2 C12 C13 S2 63.2(5) . . . . yes N O3 Ag S1 170.1(3) . . . . yes N O3 Ag S2 15.7(4) . . . . yes _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.480 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.089