Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yoichi Habata' _publ_contact_author_address ; Chemistry Toho University 2-2-1 Miyama Funabashi Chiba 274-8510 JAPAN ; _publ_contact_author_email HABATA@CHEM.SCI.TOHO-U.AC.JP _publ_section_title ; Dimetallo[3.3]para- and metacyclophanes by self-assembly of pyridylmethyl armed-monoazatrithia- and monoazadithiaoxa-12-crown-4 ethers with Ag+ ions ; loop_ _publ_author_name 'Yoichi Habata' 'Futoshi Osaka' # Attachment '3a_NS2O_4Py_AgOTf.cif' data_nso4ag_p21_n _database_code_depnum_ccdc_archive 'CCDC 285525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H46 Ag2 Cl6 F6 N4 O8 S6' _chemical_formula_weight 1349.53 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2800(9) _cell_length_b 11.3451(7) _cell_length_c 17.5634(8) _cell_angle_alpha 90.00 _cell_angle_beta 123.776(3) _cell_angle_gamma 90.00 _cell_volume 2530.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.409 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4566 _exptl_absorpt_correction_T_max 0.5826 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18531 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6288 _reflns_number_gt 5342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0449P)^2^+2.0165P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6288 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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 Ag1 Ag 0.302281(14) 0.837179(19) 0.879975(13) 0.04945(8) Uani 1 1 d . . . S2 S 0.22766(5) 0.78021(6) 0.71503(4) 0.04573(14) Uani 1 1 d . . . S4 S 0.21667(6) 0.81389(7) 0.97717(5) 0.05760(18) Uani 1 1 d . . . O1 O 0.14753(15) 0.63327(16) 0.82191(13) 0.0481(4) Uani 1 1 d . . . N1 N 0.16201(14) 0.99012(17) 0.80305(13) 0.0377(4) Uani 1 1 d . . . N2 N 0.52432(15) 1.16025(19) 1.00703(14) 0.0426(4) Uani 1 1 d . . . C1 C 0.1149(2) 0.9982(3) 0.8565(2) 0.0523(6) Uani 1 1 d . . . H1A H 0.0486 1.0402 0.8204 0.063 Uiso 1 1 calc R . . H1B H 0.1611 1.0448 0.9109 0.063 Uiso 1 1 calc R . . C2 C 0.0948(2) 0.8804(3) 0.8858(2) 0.0556(6) Uani 1 1 d . . . H2A H 0.0599 0.8274 0.8337 0.067 Uiso 1 1 calc R . . H2B H 0.0483 0.8923 0.9066 0.067 Uiso 1 1 calc R . . C3 C 0.1769(3) 0.6604(3) 0.9687(2) 0.0599(7) Uani 1 1 d . . . H3A H 0.2132 0.6271 1.0298 0.072 Uiso 1 1 calc R . . H3B H 0.1020 0.6576 0.9430 0.072 Uiso 1 1 calc R . . C4 C 0.1995(2) 0.5856(3) 0.9111(2) 0.0582(7) Uani 1 1 d . . . H4A H 0.2748 0.5831 0.9382 0.070 Uiso 1 1 calc R . . H4B H 0.1753 0.5057 0.9082 0.070 Uiso 1 1 calc R . . C5 C 0.1733(2) 0.5764(2) 0.7654(2) 0.0545(6) Uani 1 1 d . . . H5A H 0.1374 0.5011 0.7449 0.065 Uiso 1 1 calc R . . H5B H 0.2486 0.5622 0.7994 0.065 Uiso 1 1 calc R . . C6 C 0.1399(2) 0.6544(2) 0.6841(2) 0.0527(6) Uani 1 1 d . . . H6A H 0.0689 0.6824 0.6588 0.063 Uiso 1 1 calc R . . H6B H 0.1394 0.6086 0.6371 0.063 Uiso 1 1 calc R . . C7 C 0.1369(2) 0.9019(2) 0.66184(16) 0.0467(6) Uani 1 1 d . . . H7A H 0.1742 0.9681 0.6577 0.056 Uiso 1 1 calc R . . H7B H 0.0818 0.8793 0.5999 0.056 Uiso 1 1 calc R . . C8 C 0.08619(17) 0.9421(2) 0.71037(16) 0.0428(5) Uani 1 1 d . . . H8A H 0.0344 1.0023 0.6736 0.051 Uiso 1 1 calc R . . H8B H 0.0494 0.8760 0.7154 0.051 Uiso 1 1 calc R . . C9 C 0.19629(18) 1.1098(2) 0.79569(17) 0.0443(5) Uani 1 1 d . . . H9A H 0.1535 1.1684 0.8007 0.053 Uiso 1 1 calc R . . H9B H 0.1854 1.1185 0.7360 0.053 Uiso 1 1 calc R . . C10 C 0.31117(17) 1.1315(2) 0.86953(15) 0.0370(4) Uani 1 1 d . . . C11 C 0.3425(2) 1.1830(3) 0.95212(19) 0.0494(6) Uani 1 1 d . . . H11 H 0.2928 1.2101 0.9628 0.059 Uiso 1 1 calc R . . C12 C 0.4494(2) 1.1939(3) 1.01923(18) 0.0523(6) Uani 1 1 d . . . H12 H 0.4697 1.2262 1.0754 0.063 Uiso 1 1 calc R . . C13 C 0.4929(2) 1.1151(3) 0.92606(18) 0.0493(6) Uani 1 1 d . . . H13 H 0.5439 1.0931 0.9154 0.059 Uiso 1 1 calc R . . C14 C 0.3887(2) 1.0989(3) 0.85689(17) 0.0483(6) Uani 1 1 d . . . H14 H 0.3708 1.0659 0.8015 0.058 Uiso 1 1 calc R . . S3 S 0.84193(5) 0.80556(5) 0.45601(4) 0.04416(14) Uani 1 1 d . . . F1 F 0.7738(3) 0.6673(2) 0.31538(17) 0.1164(11) Uani 1 1 d . . . F2 F 0.8867(3) 0.5881(2) 0.4466(2) 0.1385(13) Uani 1 1 d . . . F3 F 0.7299(3) 0.6146(3) 0.4062(2) 0.1310(13) Uani 1 1 d . . . O2 O 0.92496(19) 0.8389(2) 0.44544(17) 0.0757(7) Uani 1 1 d . . . O3 O 0.7493(2) 0.8742(3) 0.4030(2) 0.0881(8) Uani 1 1 d . . . O4 O 0.87399(17) 0.7804(2) 0.54819(13) 0.0606(5) Uani 1 1 d . . . C15 C 0.8048(4) 0.6628(3) 0.4023(3) 0.0740(10) Uani 1 1 d . . . Cl1 Cl 0.55486(12) 0.38609(12) 0.78897(11) 0.1185(5) Uani 1 1 d . . . Cl2 Cl 0.43035(9) 0.59341(9) 0.74805(8) 0.0895(3) Uani 1 1 d . . . Cl3 Cl 0.49257(12) 0.45998(17) 0.90659(10) 0.1297(6) Uani 1 1 d . . . C16 C 0.5292(3) 0.5049(3) 0.8336(2) 0.0639(8) Uani 1 1 d . . . H16 H 0.5936 0.5521 0.8690 0.077 Uiso 1 1 calc R . . 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 Ag1 0.03088(10) 0.05731(13) 0.04341(12) 0.00450(8) 0.01024(8) -0.00434(7) S2 0.0448(3) 0.0504(3) 0.0493(3) -0.0037(3) 0.0307(3) -0.0019(3) S4 0.0558(4) 0.0716(5) 0.0400(3) -0.0017(3) 0.0233(3) -0.0152(3) O1 0.0476(10) 0.0485(10) 0.0488(10) 0.0060(8) 0.0271(8) 0.0053(8) N1 0.0301(8) 0.0393(10) 0.0353(9) -0.0028(7) 0.0130(7) -0.0018(7) N2 0.0321(9) 0.0526(12) 0.0355(10) -0.0010(8) 0.0141(8) -0.0043(8) C1 0.0492(14) 0.0524(15) 0.0613(16) -0.0086(12) 0.0344(13) -0.0002(11) C2 0.0482(14) 0.0653(17) 0.0626(17) -0.0031(14) 0.0366(13) -0.0038(13) C3 0.0580(17) 0.0711(19) 0.0516(15) 0.0126(13) 0.0310(14) -0.0089(14) C4 0.0538(15) 0.0537(16) 0.0590(16) 0.0152(13) 0.0264(13) 0.0001(12) C5 0.0557(15) 0.0425(13) 0.0685(18) -0.0033(12) 0.0365(14) 0.0009(11) C6 0.0614(16) 0.0459(14) 0.0518(15) -0.0133(11) 0.0320(13) -0.0085(12) C7 0.0480(13) 0.0494(14) 0.0316(11) 0.0009(10) 0.0153(10) -0.0037(11) C8 0.0291(10) 0.0455(13) 0.0368(11) -0.0021(9) 0.0078(9) -0.0010(9) C9 0.0339(11) 0.0388(12) 0.0423(12) 0.0018(10) 0.0100(9) -0.0014(9) C10 0.0321(10) 0.0361(11) 0.0342(11) -0.0002(8) 0.0130(9) -0.0026(8) C11 0.0357(12) 0.0618(16) 0.0503(14) -0.0158(12) 0.0236(11) -0.0028(11) C12 0.0435(13) 0.0712(18) 0.0393(13) -0.0171(12) 0.0213(11) -0.0086(12) C13 0.0391(12) 0.0645(16) 0.0474(13) -0.0076(12) 0.0259(11) -0.0023(11) C14 0.0435(13) 0.0619(16) 0.0377(12) -0.0121(11) 0.0215(10) -0.0060(11) S3 0.0430(3) 0.0401(3) 0.0424(3) -0.0003(2) 0.0194(3) -0.0014(2) F1 0.204(3) 0.0908(17) 0.0708(14) -0.0289(12) 0.086(2) -0.0336(18) F2 0.228(4) 0.0660(15) 0.148(3) 0.0131(16) 0.121(3) 0.053(2) F3 0.180(3) 0.118(2) 0.109(2) -0.0513(17) 0.089(2) -0.103(2) O2 0.0614(13) 0.0965(18) 0.0677(14) 0.0135(12) 0.0350(12) -0.0185(12) O3 0.0664(15) 0.0828(17) 0.0879(18) 0.0041(14) 0.0260(13) 0.0287(13) O4 0.0662(13) 0.0698(13) 0.0454(10) -0.0071(9) 0.0308(10) -0.0131(10) C15 0.117(3) 0.0546(18) 0.0633(19) -0.0127(15) 0.058(2) -0.0136(19) Cl1 0.1345(11) 0.0854(7) 0.1564(12) -0.0130(8) 0.0937(10) 0.0327(7) Cl2 0.0972(7) 0.0703(6) 0.1035(7) 0.0252(5) 0.0574(6) 0.0231(5) Cl3 0.1259(11) 0.1891(16) 0.0990(9) 0.0505(10) 0.0779(9) 0.0361(10) C16 0.0555(16) 0.0619(18) 0.075(2) -0.0071(15) 0.0367(15) -0.0001(14) _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 Ag1 N2 2.2611(19) 3_677 ? Ag1 N1 2.4920(19) . ? Ag1 S2 2.5373(7) . ? Ag1 S4 2.6792(8) . ? S2 C7 1.806(3) . ? S2 C6 1.823(3) . ? S4 C2 1.814(3) . ? S4 C3 1.823(3) . ? O1 C5 1.411(3) . ? O1 C4 1.412(3) . ? N1 C1 1.469(3) . ? N1 C8 1.480(3) . ? N1 C9 1.486(3) . ? N2 C13 1.325(3) . ? N2 C12 1.331(3) . ? N2 Ag1 2.2611(19) 3_677 ? C1 C2 1.525(4) . ? C3 C4 1.500(5) . ? C5 C6 1.508(4) . ? C7 C8 1.507(4) . ? C9 C10 1.514(3) . ? C10 C14 1.372(3) . ? C10 C11 1.379(3) . ? C11 C12 1.390(4) . ? C13 C14 1.376(4) . ? S3 O3 1.418(2) . ? S3 O2 1.431(2) . ? S3 O4 1.436(2) . ? S3 C15 1.799(3) . ? F1 C15 1.325(4) . ? F2 C15 1.344(5) . ? F3 C15 1.303(5) . ? Cl1 C16 1.711(3) . ? Cl2 C16 1.739(4) . ? Cl3 C16 1.736(4) . ? 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 N2 Ag1 N1 134.57(7) 3_677 . ? N2 Ag1 S2 124.67(6) 3_677 . ? N1 Ag1 S2 81.56(5) . . ? N2 Ag1 S4 101.01(6) 3_677 . ? N1 Ag1 S4 80.60(5) . . ? S2 Ag1 S4 129.32(2) . . ? C7 S2 C6 102.62(13) . . ? C7 S2 Ag1 97.15(8) . . ? C6 S2 Ag1 109.22(10) . . ? C2 S4 C3 101.15(15) . . ? C2 S4 Ag1 91.19(9) . . ? C3 S4 Ag1 107.49(11) . . ? C5 O1 C4 113.6(2) . . ? C1 N1 C8 111.33(19) . . ? C1 N1 C9 108.7(2) . . ? C8 N1 C9 109.78(19) . . ? C1 N1 Ag1 106.05(15) . . ? C8 N1 Ag1 104.56(14) . . ? C9 N1 Ag1 116.40(13) . . ? C13 N2 C12 116.9(2) . . ? C13 N2 Ag1 119.71(17) . 3_677 ? C12 N2 Ag1 123.20(17) . 3_677 ? N1 C1 C2 115.1(2) . . ? C1 C2 S4 111.3(2) . . ? C4 C3 S4 113.9(2) . . ? O1 C4 C3 109.4(2) . . ? O1 C5 C6 108.6(2) . . ? C5 C6 S2 111.8(2) . . ? C8 C7 S2 115.32(17) . . ? N1 C8 C7 113.54(19) . . ? N1 C9 C10 111.76(19) . . ? C14 C10 C11 117.2(2) . . ? C14 C10 C9 120.8(2) . . ? C11 C10 C9 122.0(2) . . ? C10 C11 C12 119.1(2) . . ? N2 C12 C11 123.2(2) . . ? N2 C13 C14 123.4(2) . . ? C10 C14 C13 120.0(2) . . ? O3 S3 O2 113.76(18) . . ? O3 S3 O4 116.07(16) . . ? O2 S3 O4 115.31(14) . . ? O3 S3 C15 103.97(19) . . ? O2 S3 C15 102.36(18) . . ? O4 S3 C15 102.84(15) . . ? F3 C15 F1 108.3(4) . . ? F3 C15 F2 105.5(3) . . ? F1 C15 F2 108.2(3) . . ? F3 C15 S3 112.4(3) . . ? F1 C15 S3 112.1(2) . . ? F2 C15 S3 110.1(3) . . ? Cl1 C16 Cl3 110.9(2) . . ? Cl1 C16 Cl2 111.6(2) . . ? Cl3 C16 Cl2 109.02(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.673 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.065 # Attachment '4a_NS3_4Py_AgOTf.cif' data_4pyns3ag_p_1 _database_code_depnum_ccdc_archive 'CCDC 285526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H50 Ag2 F6 N6 O8 S8' _chemical_formula_weight 1257.02 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6613(7) _cell_length_b 10.9064(9) _cell_length_c 13.7569(11) _cell_angle_alpha 81.397(2) _cell_angle_beta 72.0280(10) _cell_angle_gamma 72.695(2) _cell_volume 1177.77(17) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4313 _exptl_absorpt_correction_T_max 0.5177 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8782 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.35 _reflns_number_total 5793 _reflns_number_gt 5041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0498P)^2^+0.7215P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5793 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.008 _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 Ag1 Ag 0.64125(3) 0.71132(2) 0.595610(16) 0.04954(8) Uani 1 1 d . . . C1 C 0.6970(3) 0.5860(2) 0.82541(18) 0.0404(5) Uani 1 1 d . . . H1A H 0.6863 0.5337 0.8894 0.049 Uiso 1 1 calc R . . H1B H 0.6742 0.6745 0.8413 0.049 Uiso 1 1 calc R . . C2 C 0.8770(3) 0.5431(3) 0.7586(2) 0.0462(6) Uani 1 1 d . . . H2A H 0.9009 0.4533 0.7459 0.055 Uiso 1 1 calc R . . H2B H 0.9519 0.5487 0.7966 0.055 Uiso 1 1 calc R . . C3 C 0.9362(3) 0.7802(3) 0.6779(2) 0.0463(6) Uani 1 1 d . . . H3A H 0.8458 0.8043 0.7398 0.056 Uiso 1 1 calc R . . H3B H 1.0423 0.7654 0.6936 0.056 Uiso 1 1 calc R . . C4 C 0.9213(4) 0.8895(3) 0.5961(2) 0.0500(6) Uani 1 1 d . . . H4A H 1.0090 0.8621 0.5338 0.060 Uiso 1 1 calc R . . H4B H 0.9430 0.9618 0.6179 0.060 Uiso 1 1 calc R . . C5 C 0.5775(3) 1.0093(2) 0.6847(2) 0.0450(5) Uani 1 1 d . . . H5A H 0.6103 0.9562 0.7419 0.054 Uiso 1 1 calc R . . H5B H 0.5844 1.0955 0.6886 0.054 Uiso 1 1 calc R . . C6 C 0.3977(3) 1.0136(2) 0.6924(2) 0.0454(5) Uani 1 1 d . . . H6A H 0.3688 1.0639 0.6331 0.055 Uiso 1 1 calc R . . H6B H 0.3244 1.0589 0.7524 0.055 Uiso 1 1 calc R . . C7 C 0.3654(3) 0.7936(2) 0.8283(2) 0.0448(5) Uani 1 1 d . . . H7A H 0.4552 0.8164 0.8435 0.054 Uiso 1 1 calc R . . H7B H 0.2605 0.8305 0.8784 0.054 Uiso 1 1 calc R . . C8 C 0.3992(3) 0.6481(2) 0.8360(2) 0.0428(5) Uani 1 1 d . . . H8A H 0.3811 0.6182 0.9076 0.051 Uiso 1 1 calc R . . H8B H 0.3173 0.6267 0.8115 0.051 Uiso 1 1 calc R . . C9 C 0.5722(3) 0.4399(2) 0.78062(19) 0.0400(5) Uani 1 1 d . . . H9A H 0.4979 0.4171 0.8451 0.048 Uiso 1 1 calc R . . H9B H 0.6854 0.3870 0.7775 0.048 Uiso 1 1 calc R . . C10 C 0.5198(3) 0.4095(2) 0.69429(17) 0.0332(4) Uani 1 1 d . . . C11 C 0.3581(3) 0.4010(2) 0.70683(18) 0.0398(5) Uani 1 1 d . . . H11 H 0.2759 0.4194 0.7688 0.048 Uiso 1 1 calc R . . C12 C 0.3197(3) 0.3650(2) 0.62670(19) 0.0401(5) Uani 1 1 d . . . H12 H 0.2106 0.3598 0.6366 0.048 Uiso 1 1 calc R . . C13 C 0.5871(3) 0.3454(2) 0.52373(18) 0.0408(5) Uani 1 1 d . . . H13 H 0.6667 0.3264 0.4610 0.049 Uiso 1 1 calc R . . C14 C 0.6357(3) 0.3809(2) 0.59996(19) 0.0398(5) Uani 1 1 d . . . H14 H 0.7457 0.3855 0.5879 0.048 Uiso 1 1 calc R . . C16 C 0.8979(6) 0.0890(5) 0.8384(3) 0.0875(12) Uani 1 1 d . . . H16A H 0.7794 0.0975 0.8543 0.131 Uiso 1 1 calc R . . H16B H 0.9190 0.1281 0.8894 0.131 Uiso 1 1 calc R . . H16C H 0.9579 -0.0005 0.8376 0.131 Uiso 1 1 calc R . . C17 C 0.9540(4) 0.1522(3) 0.7392(3) 0.0583(7) Uani 1 1 d . . . C18 C 0.30839(15) 0.14531(11) 0.97430(8) 0.0308(2) Uani 1.83 1 d P . . F1 F 0.2495(4) 0.0499(2) 0.9573(2) 0.0926(8) Uani 0.94 1 d P . . F2 F 0.4257(3) 0.1776(2) 0.8889(2) 0.0958(8) Uani 0.94 1 d P . . F3 F 0.3432(3) 0.1322(2) 1.0639(2) 0.0860(7) Uani 0.94 1 d P . . N1 N 0.5689(2) 0.57723(17) 0.77885(14) 0.0339(4) Uani 1 1 d . . . N2 N 0.4314(3) 0.33721(19) 0.53604(15) 0.0377(4) Uani 1 1 d . . . N3 N 0.9970(4) 0.2027(3) 0.6623(3) 0.0742(8) Uani 1 1 d . . . O1 O 0.1792(3) 0.3971(2) 0.98064(19) 0.0687(6) Uani 1.06 1 d P . . O2 O 0.0594(4) 0.2993(3) 0.9039(2) 0.0861(8) Uani 1.06 1 d P . . O3 O 0.0090(3) 0.2764(3) 1.0767(2) 0.1018(10) Uani 1.06 1 d P . . S1 S 0.92611(8) 0.63273(6) 0.63660(5) 0.04431(14) Uani 1 1 d . . . S2 S 0.72147(9) 0.94507(6) 0.56599(5) 0.04612(15) Uani 1 1 d . . . S3 S 0.35231(8) 0.85939(6) 0.70063(5) 0.04443(14) Uani 1 1 d . . . S4A S 0.11245(15) 0.29885(13) 0.98703(9) 0.0597(3) Uani 0.69 1 d P . . 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 Ag1 0.05194(13) 0.05696(14) 0.04774(13) -0.01896(9) -0.02219(9) -0.01013(9) C1 0.0499(13) 0.0442(12) 0.0366(11) -0.0041(9) -0.0184(10) -0.0189(10) C2 0.0455(13) 0.0443(13) 0.0533(14) 0.0015(11) -0.0230(11) -0.0112(10) C3 0.0459(13) 0.0533(14) 0.0493(14) -0.0003(11) -0.0201(11) -0.0219(11) C4 0.0527(15) 0.0554(15) 0.0483(14) 0.0004(12) -0.0121(12) -0.0278(12) C5 0.0564(15) 0.0393(12) 0.0431(13) -0.0093(10) -0.0140(11) -0.0148(11) C6 0.0527(14) 0.0354(11) 0.0474(13) -0.0076(10) -0.0181(11) -0.0039(10) C7 0.0460(13) 0.0441(13) 0.0416(13) -0.0124(10) -0.0053(10) -0.0104(10) C8 0.0414(12) 0.0423(12) 0.0426(12) -0.0087(10) -0.0028(10) -0.0146(10) C9 0.0539(14) 0.0345(11) 0.0392(12) -0.0027(9) -0.0207(10) -0.0146(10) C10 0.0428(11) 0.0278(9) 0.0328(10) -0.0035(8) -0.0144(9) -0.0102(8) C11 0.0409(12) 0.0460(12) 0.0334(11) -0.0081(9) -0.0065(9) -0.0146(10) C12 0.0358(11) 0.0450(12) 0.0435(12) -0.0082(10) -0.0121(9) -0.0132(9) C13 0.0388(12) 0.0469(13) 0.0357(11) -0.0127(10) -0.0073(9) -0.0083(10) C14 0.0344(11) 0.0441(12) 0.0430(12) -0.0084(10) -0.0103(9) -0.0116(9) C16 0.097(3) 0.090(3) 0.084(3) 0.007(2) -0.026(2) -0.044(2) C17 0.0498(16) 0.0480(15) 0.079(2) -0.0094(15) -0.0213(15) -0.0093(12) C18 0.0415(6) 0.0293(5) 0.0229(5) -0.0065(4) -0.0063(4) -0.0117(4) F1 0.150(3) 0.0609(13) 0.0859(16) -0.0041(11) -0.0469(16) -0.0426(15) F2 0.0939(18) 0.0767(15) 0.0758(15) -0.0045(12) 0.0176(13) -0.0055(13) F3 0.0974(17) 0.0706(13) 0.1018(18) -0.0228(12) -0.0605(15) 0.0029(12) N1 0.0367(9) 0.0325(9) 0.0361(9) -0.0079(7) -0.0111(7) -0.0106(7) N2 0.0417(10) 0.0366(9) 0.0388(10) -0.0093(8) -0.0155(8) -0.0088(8) N3 0.0650(18) 0.0729(19) 0.081(2) -0.0012(16) -0.0235(16) -0.0125(15) O1 0.0704(14) 0.0529(11) 0.0851(16) -0.0204(10) -0.0283(12) -0.0055(10) O2 0.111(2) 0.0872(17) 0.0840(17) 0.0114(13) -0.0660(16) -0.0291(15) O3 0.0529(14) 0.116(2) 0.100(2) 0.0168(17) 0.0067(13) -0.0093(14) S1 0.0379(3) 0.0463(3) 0.0462(3) -0.0075(3) -0.0088(2) -0.0082(2) S2 0.0558(4) 0.0491(3) 0.0350(3) -0.0013(2) -0.0147(3) -0.0149(3) S3 0.0435(3) 0.0441(3) 0.0507(3) -0.0118(3) -0.0191(3) -0.0086(2) S4A 0.0606(6) 0.0755(7) 0.0496(6) 0.0020(5) -0.0218(5) -0.0242(5) _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 Ag1 N2 2.2682(19) 2_666 ? Ag1 S1 2.5683(7) . ? Ag1 S3 2.6497(7) . ? Ag1 S2 2.7779(7) . ? C1 N1 1.473(3) . ? C1 C2 1.518(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 S1 1.808(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.515(4) . ? C3 S1 1.818(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 S2 1.811(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.515(4) . ? C5 S2 1.810(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 S3 1.818(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.519(3) . ? C7 S3 1.820(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N1 1.472(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.486(3) . ? C9 C10 1.505(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.386(3) . ? C10 C11 1.387(3) . ? C11 C12 1.383(3) . ? C11 H11 0.9300 . ? C12 N2 1.333(3) . ? C12 H12 0.9300 . ? C13 N2 1.335(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.443(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N3 1.125(5) . ? C18 F3 1.335(3) . ? C18 F1 1.364(2) . ? C18 F2 1.375(3) . ? C18 S4A 1.9820(18) . ? N2 Ag1 2.2682(19) 2_666 ? O1 S4A 1.342(2) . ? O2 S4A 1.356(3) . ? O3 S4A 1.320(3) . ? 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 N2 Ag1 S1 128.79(5) 2_666 . ? N2 Ag1 S3 101.89(5) 2_666 . ? S1 Ag1 S3 129.25(2) . . ? N2 Ag1 S2 114.40(5) 2_666 . ? S1 Ag1 S2 81.37(2) . . ? S3 Ag1 S2 79.81(2) . . ? N1 C1 C2 114.33(19) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C1 C2 S1 115.88(18) . . ? C1 C2 H2A 108.3 . . ? S1 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? S1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C4 C3 S1 111.58(19) . . ? C4 C3 H3A 109.3 . . ? S1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? S1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 S2 116.34(18) . . ? C3 C4 H4A 108.2 . . ? S2 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? S2 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C6 C5 S2 111.47(17) . . ? C6 C5 H5A 109.3 . . ? S2 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? S2 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 S3 116.45(18) . . ? C5 C6 H6A 108.2 . . ? S3 C6 H6A 108.2 . . ? C5 C6 H6B 108.2 . . ? S3 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C8 C7 S3 110.64(17) . . ? C8 C7 H7A 109.5 . . ? S3 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? S3 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N1 C8 C7 115.5(2) . . ? N1 C8 H8A 108.4 . . ? C7 C8 H8A 108.4 . . ? N1 C8 H8B 108.4 . . ? C7 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? N1 C9 C10 113.86(19) . . ? N1 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N1 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C14 C10 C11 117.1(2) . . ? C14 C10 C9 120.7(2) . . ? C11 C10 C9 122.1(2) . . ? C12 C11 C10 119.6(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? N2 C12 C11 123.3(2) . . ? N2 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N2 C13 C14 123.1(2) . . ? N2 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.7(2) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C16 179.3(4) . . ? F3 C18 F1 114.95(18) . . ? F3 C18 F2 117.2(2) . . ? F1 C18 F2 111.75(19) . . ? F3 C18 S4A 103.91(12) . . ? F1 C18 S4A 103.65(15) . . ? F2 C18 S4A 103.31(13) . . ? C8 N1 C1 110.97(18) . . ? C8 N1 C9 108.57(18) . . ? C1 N1 C9 109.15(18) . . ? C12 N2 C13 117.2(2) . . ? C12 N2 Ag1 121.88(16) . 2_666 ? C13 N2 Ag1 120.80(16) . 2_666 ? C2 S1 C3 100.43(13) . . ? C2 S1 Ag1 102.83(9) . . ? C3 S1 Ag1 100.18(9) . . ? C5 S2 C4 102.56(13) . . ? C5 S2 Ag1 96.17(8) . . ? C4 S2 Ag1 98.47(9) . . ? C6 S3 C7 102.65(12) . . ? C6 S3 Ag1 103.25(9) . . ? C7 S3 Ag1 97.72(9) . . ? O3 S4A O1 115.8(2) . . ? O3 S4A O2 116.0(2) . . ? O1 S4A O2 111.95(18) . . ? O3 S4A C18 103.55(15) . . ? O1 S4A C18 103.66(12) . . ? O2 S4A C18 103.86(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.787 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.073 # Attachment '3b_NS2O_3Py_AgPF6.cif' data_ns2o3py_p_1 _database_code_depnum_ccdc_archive 'CCDC 285527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H50 Ag2 F12 N6 O2 P2 S4' _chemical_formula_weight 1184.70 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4105(12) _cell_length_b 10.3316(15) _cell_length_c 13.900(2) _cell_angle_alpha 95.302(3) _cell_angle_beta 98.218(3) _cell_angle_gamma 109.098(3) _cell_volume 1117.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5912 _exptl_absorpt_correction_T_max 0.6403 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8157 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.36 _reflns_number_total 5470 _reflns_number_gt 4668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0790P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5470 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _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 C15 C 0.1971(6) 0.3554(5) 0.8557(4) 0.0856(14) Uani 1 1 d . . . H15A H 0.2306 0.4544 0.8683 0.128 Uiso 1 1 calc R . . H15B H 0.2795 0.3263 0.8945 0.128 Uiso 1 1 calc R . . H15C H 0.0867 0.3142 0.8726 0.128 Uiso 1 1 calc R . . Ag1 Ag -0.09506(3) 0.84888(2) 0.645491(15) 0.04201(10) Uani 1 1 d . . . S2 S 0.00273(11) 0.96084(8) 0.83439(5) 0.04508(17) Uani 1 1 d . . . S1 S -0.22154(10) 0.58789(8) 0.58260(5) 0.04603(18) Uani 1 1 d . . . P1 P 0.68430(12) 0.28447(10) 0.90955(6) 0.0507(2) Uani 1 1 d . . . N1 N 0.1647(3) 0.7851(2) 0.69143(15) 0.0326(4) Uani 1 1 d . . . C11 C 0.2153(3) 0.9777(3) 0.51642(19) 0.0342(5) Uani 1 1 d . . . H11 H 0.1762 1.0288 0.5600 0.041 Uiso 1 1 calc R . . O1 O -0.3618(3) 0.7284(2) 0.75354(15) 0.0463(5) Uani 1 1 d . . . N2 N 0.1924(3) 0.9935(2) 0.42149(16) 0.0356(4) Uani 1 1 d . . . C9 C 0.3195(3) 0.8771(3) 0.66103(18) 0.0369(5) Uani 1 1 d . . . H9A H 0.4124 0.8419 0.6768 0.044 Uiso 1 1 calc R . . H9B H 0.3530 0.9687 0.6986 0.044 Uiso 1 1 calc R . . C2 C -0.0531(4) 0.5424(3) 0.6525(2) 0.0463(6) Uani 1 1 d . . . H2A H -0.0652 0.5463 0.7210 0.056 Uiso 1 1 calc R . . H2B H -0.0639 0.4483 0.6280 0.056 Uiso 1 1 calc R . . C10 C 0.2946(3) 0.8888(3) 0.55336(18) 0.0325(5) Uani 1 1 d . . . C12 C 0.2494(4) 0.9189(3) 0.35986(19) 0.0401(6) Uani 1 1 d . . . H12 H 0.2314 0.9268 0.2934 0.048 Uiso 1 1 calc R . . C14 C 0.3571(4) 0.8169(3) 0.4882(2) 0.0387(6) Uani 1 1 d . . . H14 H 0.4149 0.7593 0.5104 0.046 Uiso 1 1 calc R . . C8 C 0.1978(4) 0.7916(3) 0.79959(19) 0.0420(6) Uani 1 1 d . . . H8A H 0.3070 0.7798 0.8194 0.050 Uiso 1 1 calc R . . H8B H 0.1100 0.7149 0.8174 0.050 Uiso 1 1 calc R . . C1 C 0.1231(4) 0.6411(3) 0.6446(2) 0.0411(6) Uani 1 1 d . . . H1A H 0.2091 0.6058 0.6742 0.049 Uiso 1 1 calc R . . H1B H 0.1302 0.6414 0.5755 0.049 Uiso 1 1 calc R . . F5 F 0.8395(4) 0.3293(4) 0.9984(2) 0.1083(10) Uani 1 1 d . . . F1 F 0.8031(4) 0.3602(3) 0.8383(2) 0.0972(9) Uani 1 1 d . . . C13 C 0.3326(4) 0.8316(3) 0.3894(2) 0.0421(6) Uani 1 1 d . . . H13 H 0.3720 0.7831 0.3443 0.050 Uiso 1 1 calc R . . C7 C 0.2011(4) 0.9261(3) 0.8566(2) 0.0480(7) Uani 1 1 d . . . H7A H 0.2910 1.0024 0.8399 0.058 Uiso 1 1 calc R . . H7B H 0.2307 0.9235 0.9262 0.058 Uiso 1 1 calc R . . C4 C -0.3796(4) 0.5870(3) 0.7496(3) 0.0525(7) Uani 1 1 d . . . H4A H -0.4783 0.5387 0.7773 0.063 Uiso 1 1 calc R . . H4B H -0.2788 0.5785 0.7881 0.063 Uiso 1 1 calc R . . C3 C -0.4021(4) 0.5227(3) 0.6440(3) 0.0547(8) Uani 1 1 d . . . H3A H -0.5005 0.5360 0.6064 0.066 Uiso 1 1 calc R . . H3B H -0.4284 0.4237 0.6422 0.066 Uiso 1 1 calc R . . F4 F 0.5620(4) 0.2076(4) 0.9780(2) 0.1056(10) Uani 1 1 d . . . C6 C -0.1326(4) 0.8352(4) 0.8981(2) 0.0545(8) Uani 1 1 d . . . H6A H -0.1024 0.7522 0.8944 0.065 Uiso 1 1 calc R . . H6B H -0.1141 0.8733 0.9669 0.065 Uiso 1 1 calc R . . F3 F 0.6452(6) 0.4207(4) 0.9387(3) 0.1325(14) Uani 1 1 d . . . F2 F 0.5280(4) 0.2442(4) 0.82018(19) 0.1064(10) Uani 1 1 d . . . C5 C -0.3202(4) 0.7985(4) 0.8522(3) 0.0564(8) Uani 1 1 d . . . H5A H -0.3906 0.7401 0.8920 0.068 Uiso 1 1 calc R . . H5B H -0.3475 0.8828 0.8528 0.068 Uiso 1 1 calc R . . F6 F 0.7203(6) 0.1495(4) 0.8785(3) 0.1357(15) Uani 1 1 d . . . C16 C 0.1890(5) 0.3126(5) 0.7539(4) 0.0759(11) Uani 1 1 d . . . N3 N 0.1845(7) 0.2768(6) 0.6734(4) 0.1186(17) 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 C15 0.070(3) 0.084(3) 0.104(4) 0.009(3) 0.029(3) 0.024(2) Ag1 0.05293(15) 0.04323(14) 0.03623(13) 0.01461(9) 0.00809(9) 0.02279(11) S2 0.0569(4) 0.0495(4) 0.0306(3) 0.0032(3) 0.0090(3) 0.0209(3) S1 0.0531(4) 0.0431(4) 0.0381(4) 0.0040(3) 0.0037(3) 0.0140(3) P1 0.0610(5) 0.0665(5) 0.0344(4) 0.0139(3) 0.0161(3) 0.0304(4) N1 0.0378(11) 0.0381(11) 0.0251(9) 0.0114(8) 0.0093(8) 0.0139(9) C11 0.0385(13) 0.0377(13) 0.0308(12) 0.0084(10) 0.0104(10) 0.0164(10) O1 0.0498(11) 0.0493(11) 0.0427(11) 0.0077(9) 0.0054(9) 0.0221(9) N2 0.0420(12) 0.0394(11) 0.0297(10) 0.0108(8) 0.0098(9) 0.0170(9) C9 0.0383(13) 0.0436(14) 0.0293(12) 0.0113(10) 0.0080(10) 0.0123(11) C2 0.0523(17) 0.0403(15) 0.0521(17) 0.0166(13) 0.0150(13) 0.0187(13) C10 0.0336(12) 0.0327(12) 0.0306(11) 0.0101(9) 0.0082(9) 0.0082(10) C12 0.0539(16) 0.0417(14) 0.0268(11) 0.0082(10) 0.0123(11) 0.0164(12) C14 0.0453(14) 0.0380(13) 0.0401(14) 0.0131(11) 0.0136(11) 0.0196(11) C8 0.0453(14) 0.0592(17) 0.0276(12) 0.0165(11) 0.0082(10) 0.0227(13) C1 0.0489(15) 0.0368(13) 0.0452(15) 0.0119(11) 0.0181(12) 0.0196(12) F5 0.091(2) 0.152(3) 0.0665(16) 0.0427(18) -0.0109(14) 0.0247(19) F1 0.0823(17) 0.136(2) 0.0803(18) 0.0596(17) 0.0325(14) 0.0284(16) C13 0.0575(17) 0.0434(14) 0.0333(13) 0.0077(11) 0.0180(12) 0.0234(13) C7 0.0467(16) 0.0619(18) 0.0277(12) 0.0009(12) 0.0032(11) 0.0116(14) C4 0.0497(17) 0.0495(17) 0.063(2) 0.0195(15) 0.0194(15) 0.0159(14) C3 0.0459(16) 0.0414(16) 0.068(2) 0.0018(14) 0.0077(15) 0.0069(13) F4 0.100(2) 0.156(3) 0.0667(16) 0.0380(17) 0.0473(16) 0.033(2) C6 0.0587(19) 0.078(2) 0.0250(12) 0.0077(13) 0.0129(12) 0.0182(17) F3 0.216(4) 0.129(3) 0.093(2) 0.006(2) 0.025(3) 0.118(3) F2 0.0817(18) 0.174(3) 0.0538(14) 0.0158(17) 0.0037(13) 0.0346(19) C5 0.0546(18) 0.074(2) 0.0445(16) 0.0032(15) 0.0176(14) 0.0258(17) F6 0.232(4) 0.103(2) 0.136(3) 0.039(2) 0.093(3) 0.114(3) C16 0.055(2) 0.069(3) 0.095(3) 0.010(2) 0.013(2) 0.0109(19) N3 0.108(4) 0.119(4) 0.105(4) 0.001(3) 0.012(3) 0.015(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 C15 C16 1.427(7) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? Ag1 N2 2.263(2) 2_576 ? Ag1 N1 2.497(2) . ? Ag1 S1 2.5668(9) . ? Ag1 S2 2.6661(8) . ? Ag1 O1 2.884(2) . ? S2 C7 1.809(3) . ? S2 C6 1.816(3) . ? S1 C3 1.815(4) . ? S1 C2 1.816(3) . ? P1 F6 1.557(3) . ? P1 F4 1.574(3) . ? P1 F5 1.575(3) . ? P1 F3 1.577(3) . ? P1 F1 1.583(3) . ? P1 F2 1.589(3) . ? N1 C1 1.475(3) . ? N1 C8 1.481(3) . ? N1 C9 1.483(3) . ? C11 N2 1.339(3) . ? C11 C10 1.394(3) . ? C11 H11 0.9300 . ? O1 C4 1.414(4) . ? O1 C5 1.429(4) . ? N2 C12 1.340(3) . ? N2 Ag1 2.263(2) 2_576 ? C9 C10 1.503(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C2 C1 1.526(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C10 C14 1.384(4) . ? C12 C13 1.368(4) . ? C12 H12 0.9300 . ? C14 C13 1.389(4) . ? C14 H14 0.9300 . ? C8 C7 1.525(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C13 H13 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C4 C3 1.514(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 C5 1.522(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C16 N3 1.137(7) . ? 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 C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 Ag1 N1 144.18(8) 2_576 . ? N2 Ag1 S1 123.49(6) 2_576 . ? N1 Ag1 S1 80.41(5) . . ? N2 Ag1 S2 101.88(6) 2_576 . ? N1 Ag1 S2 79.10(5) . . ? S1 Ag1 S2 124.86(3) . . ? N2 Ag1 O1 100.45(7) 2_576 . ? N1 Ag1 O1 113.01(6) . . ? S1 Ag1 O1 72.39(5) . . ? S2 Ag1 O1 69.85(5) . . ? C7 S2 C6 101.96(16) . . ? C7 S2 Ag1 97.43(9) . . ? C6 S2 Ag1 104.49(11) . . ? C3 S1 C2 103.86(16) . . ? C3 S1 Ag1 105.06(11) . . ? C2 S1 Ag1 96.48(10) . . ? F6 P1 F4 90.5(2) . . ? F6 P1 F5 90.7(2) . . ? F4 P1 F5 89.73(17) . . ? F6 P1 F3 178.7(2) . . ? F4 P1 F3 89.9(2) . . ? F5 P1 F3 90.6(2) . . ? F6 P1 F1 89.39(19) . . ? F4 P1 F1 178.45(18) . . ? F5 P1 F1 91.81(17) . . ? F3 P1 F1 90.2(2) . . ? F6 P1 F2 91.0(2) . . ? F4 P1 F2 90.88(17) . . ? F5 P1 F2 178.2(2) . . ? F3 P1 F2 87.7(2) . . ? F1 P1 F2 87.58(16) . . ? C1 N1 C8 109.3(2) . . ? C1 N1 C9 110.1(2) . . ? C8 N1 C9 109.0(2) . . ? C1 N1 Ag1 106.92(16) . . ? C8 N1 Ag1 107.79(15) . . ? C9 N1 Ag1 113.62(15) . . ? N2 C11 C10 123.5(2) . . ? N2 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C4 O1 C5 112.2(3) . . ? C4 O1 Ag1 106.39(16) . . ? C5 O1 Ag1 110.89(19) . . ? C11 N2 C12 117.3(2) . . ? C11 N2 Ag1 127.16(17) . 2_576 ? C12 N2 Ag1 115.10(17) . 2_576 ? N1 C9 C10 113.5(2) . . ? N1 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N1 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C1 C2 S1 110.9(2) . . ? C1 C2 H2A 109.5 . . ? S1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C14 C10 C11 117.6(2) . . ? C14 C10 C9 121.1(2) . . ? C11 C10 C9 121.2(2) . . ? N2 C12 C13 123.5(2) . . ? N2 C12 H12 118.2 . . ? C13 C12 H12 118.2 . . ? C10 C14 C13 119.3(2) . . ? C10 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N1 C8 C7 114.3(2) . . ? N1 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C1 C2 114.9(2) . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C12 C13 C14 118.7(2) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C8 C7 S2 115.0(2) . . ? C8 C7 H7A 108.5 . . ? S2 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? S2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? O1 C4 C3 109.7(3) . . ? O1 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O1 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C3 S1 116.5(2) . . ? C4 C3 H3A 108.2 . . ? S1 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? S1 C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C5 C6 S2 110.4(2) . . ? C5 C6 H6A 109.6 . . ? S2 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? S2 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O1 C5 C6 113.0(3) . . ? O1 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? O1 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N3 C16 C15 178.6(6) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.277 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.113 # Attachment '4b_NS3_3Py_AgOTf.cif' data_3pyns3_ag_p21_c _database_code_depnum_ccdc_archive 'CCDC 285528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H50 Ag2 F6 N6 O6 S8' _chemical_formula_weight 1225.02 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.4836(8) _cell_length_b 12.5433(7) _cell_length_c 13.7270(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.8150(10) _cell_angle_gamma 90.00 _cell_volume 2360.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7873 _exptl_absorpt_correction_T_max 0.8055 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17348 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.30 _reflns_number_total 5853 _reflns_number_gt 4805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0500P)^2^+0.6384P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5853 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 C10 C 0.29875(17) -0.12230(18) 0.41654(17) 0.0426(5) Uani 1 1 d . . . Ag1 Ag 0.425247(13) 0.084421(16) 0.303356(14) 0.05139(8) Uani 1 1 d . . . S3 S 0.44495(4) -0.01380(5) 0.14025(4) 0.04632(14) Uani 1 1 d . . . S2 S 0.46119(5) 0.25939(5) 0.17536(5) 0.05383(16) Uani 1 1 d . . . S1 S 0.29575(5) 0.21821(6) 0.31092(5) 0.05822(17) Uani 1 1 d . . . S4 S 0.03720(7) 0.29108(8) 0.42711(7) 0.0849(3) Uani 1 1 d . . . C11 C 0.39242(16) -0.09706(16) 0.47795(17) 0.0400(4) Uani 1 1 d . . . H11 H 0.4397 -0.0873 0.4463 0.048 Uiso 1 1 calc R . . N1 N 0.27089(13) -0.03247(16) 0.24734(14) 0.0428(4) Uani 1 1 d . . . N2 N 0.41904(14) -0.08590(14) 0.58067(14) 0.0418(4) Uani 1 1 d . . . C6 C 0.4022(2) 0.08513(19) 0.03915(18) 0.0497(5) Uani 1 1 d . . . H6A H 0.4039 0.0553 -0.0254 0.060 Uiso 1 1 calc R . . H6B H 0.3352 0.1037 0.0312 0.060 Uiso 1 1 calc R . . C7 C 0.3398(2) -0.10026(19) 0.11284(18) 0.0501(6) Uani 1 1 d . . . H7A H 0.3194 -0.1189 0.0404 0.060 Uiso 1 1 calc R . . H7B H 0.3594 -0.1656 0.1518 0.060 Uiso 1 1 calc R . . C12 C 0.35025(18) -0.09950(19) 0.62532(18) 0.0467(5) Uani 1 1 d . . . H12 H 0.3673 -0.0909 0.6962 0.056 Uiso 1 1 calc R . . C14 C 0.22954(18) -0.1376(2) 0.4657(2) 0.0526(6) Uani 1 1 d . . . H14 H 0.1659 -0.1559 0.4276 0.063 Uiso 1 1 calc R . . C2 C 0.19013(18) 0.1489(2) 0.2272(2) 0.0564(6) Uani 1 1 d . . . H2A H 0.1312 0.1835 0.2303 0.068 Uiso 1 1 calc R . . H2B H 0.1906 0.1527 0.1568 0.068 Uiso 1 1 calc R . . C4 C 0.3359(2) 0.3047(2) 0.1377(2) 0.0580(6) Uani 1 1 d . . . H4A H 0.3286 0.3679 0.0952 0.070 Uiso 1 1 calc R . . H4B H 0.2934 0.2498 0.0971 0.070 Uiso 1 1 calc R . . C13 C 0.25551(18) -0.1256(2) 0.5707(2) 0.0550(6) Uani 1 1 d . . . H13 H 0.2096 -0.1350 0.6043 0.066 Uiso 1 1 calc R . . C5 C 0.4648(2) 0.1847(2) 0.0638(2) 0.0564(6) Uani 1 1 d . . . H5A H 0.4445 0.2315 0.0044 0.068 Uiso 1 1 calc R . . H5B H 0.5319 0.1643 0.0740 0.068 Uiso 1 1 calc R . . C3 C 0.3061(2) 0.3300(2) 0.2311(2) 0.0646(7) Uani 1 1 d . . . H3A H 0.2437 0.3662 0.2079 0.078 Uiso 1 1 calc R . . H3B H 0.3533 0.3797 0.2739 0.078 Uiso 1 1 calc R . . C9 C 0.27438(18) -0.13489(19) 0.30199(17) 0.0472(5) Uani 1 1 d . . . H9A H 0.3228 -0.1806 0.2883 0.057 Uiso 1 1 calc R . . H9B H 0.2116 -0.1699 0.2748 0.057 Uiso 1 1 calc R . . C1 C 0.18976(18) 0.0326(2) 0.2589(2) 0.0545(6) Uani 1 1 d . . . H1A H 0.1922 0.0300 0.3303 0.065 Uiso 1 1 calc R . . H1B H 0.1286 0.0006 0.2179 0.065 Uiso 1 1 calc R . . O3 O 0.1343(2) 0.3315(2) 0.4705(2) 0.1055(9) Uani 1 1 d . . . F3 F -0.0334(2) 0.1014(2) 0.4324(3) 0.1451(12) Uani 1 1 d . . . F2 F 0.0688(3) 0.1507(2) 0.5727(2) 0.1331(10) Uani 1 1 d . . . F1 F 0.1163(3) 0.1052(2) 0.4522(3) 0.1487(13) Uani 1 1 d . . . O2 O 0.0054(3) 0.2819(3) 0.3193(2) 0.1394(14) Uani 1 1 d . . . C15 C 0.0474(2) 0.1578(3) 0.4726(3) 0.0755(9) Uani 1 1 d . . . O1 O -0.0307(3) 0.3337(4) 0.4701(4) 0.186(2) Uani 1 1 d . . . C8 C 0.25315(18) -0.0548(2) 0.13683(18) 0.0512(5) Uani 1 1 d . . . H8A H 0.2336 0.0110 0.0984 0.061 Uiso 1 1 calc R . . H8B H 0.1992 -0.1045 0.1131 0.061 Uiso 1 1 calc R . . N3 N 0.7285(3) 0.0915(2) 0.1664(3) 0.0813(8) Uani 1 1 d . . . C17 C 0.8063(3) 0.0791(2) 0.1680(2) 0.0668(8) Uani 1 1 d . . . C16 C 0.9053(3) 0.0653(4) 0.1694(4) 0.1034(14) Uani 1 1 d . . . H16A H 0.9437 0.1253 0.2027 0.155 Uiso 1 1 calc R . . H16B H 0.9066 0.0599 0.1002 0.155 Uiso 1 1 calc R . . H16C H 0.9317 0.0013 0.2064 0.155 Uiso 1 1 calc R . . 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 C10 0.0408(11) 0.0428(11) 0.0423(11) 0.0055(9) 0.0107(9) 0.0024(9) Ag1 0.04214(11) 0.06432(14) 0.04117(11) -0.00233(8) 0.00434(8) 0.00265(8) S3 0.0464(3) 0.0511(3) 0.0419(3) 0.0027(2) 0.0148(2) 0.0054(2) S2 0.0461(3) 0.0549(3) 0.0539(3) -0.0029(3) 0.0069(3) -0.0086(3) S1 0.0523(4) 0.0683(4) 0.0505(3) -0.0123(3) 0.0116(3) 0.0052(3) S4 0.0762(5) 0.0887(6) 0.0710(5) -0.0093(4) -0.0024(4) 0.0277(5) C11 0.0366(10) 0.0438(11) 0.0401(11) 0.0040(8) 0.0130(9) 0.0019(8) N1 0.0360(9) 0.0510(10) 0.0384(9) 0.0040(8) 0.0078(7) 0.0005(8) N2 0.0386(9) 0.0461(10) 0.0388(9) 0.0018(7) 0.0098(8) 0.0034(8) C6 0.0582(15) 0.0525(13) 0.0363(11) 0.0027(9) 0.0124(11) -0.0001(11) C7 0.0635(15) 0.0482(13) 0.0357(11) -0.0047(9) 0.0122(11) -0.0059(11) C12 0.0465(12) 0.0556(14) 0.0387(11) 0.0028(9) 0.0147(10) 0.0086(10) C14 0.0373(11) 0.0648(15) 0.0530(14) 0.0061(11) 0.0108(10) -0.0033(11) C2 0.0380(12) 0.0632(15) 0.0621(16) 0.0083(12) 0.0079(11) 0.0063(11) C4 0.0543(14) 0.0425(13) 0.0678(16) 0.0053(11) 0.0064(13) 0.0003(11) C13 0.0438(13) 0.0731(16) 0.0535(14) 0.0105(12) 0.0231(11) 0.0055(12) C5 0.0594(15) 0.0619(15) 0.0475(13) 0.0062(11) 0.0167(12) -0.0048(12) C3 0.0582(16) 0.0429(13) 0.085(2) -0.0140(13) 0.0125(14) 0.0016(12) C9 0.0469(12) 0.0475(12) 0.0419(12) 0.0022(9) 0.0071(10) -0.0039(10) C1 0.0353(11) 0.0651(15) 0.0631(15) 0.0122(12) 0.0160(11) 0.0048(11) O3 0.107(2) 0.0907(18) 0.0872(18) 0.0078(14) -0.0131(15) -0.0152(16) F3 0.0959(19) 0.145(2) 0.166(3) -0.004(2) 0.0026(19) -0.0440(17) F2 0.179(3) 0.123(2) 0.0830(17) 0.0081(14) 0.0221(17) -0.028(2) F1 0.150(3) 0.1037(18) 0.229(4) 0.004(2) 0.111(3) 0.0475(18) O2 0.170(3) 0.134(3) 0.0697(17) 0.0002(17) -0.0235(19) -0.013(2) C15 0.0531(16) 0.093(2) 0.076(2) -0.0177(17) 0.0145(15) -0.0021(16) O1 0.151(4) 0.188(4) 0.228(5) -0.015(4) 0.073(4) 0.101(3) C8 0.0446(12) 0.0642(14) 0.0359(11) 0.0035(10) 0.0007(9) -0.0075(11) N3 0.080(2) 0.095(2) 0.0696(18) -0.0003(14) 0.0250(16) -0.0042(16) C17 0.080(2) 0.0699(18) 0.0464(14) -0.0098(12) 0.0149(15) -0.0092(16) C16 0.074(2) 0.136(4) 0.097(3) -0.039(3) 0.023(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 C11 1.383(3) . ? C10 C14 1.390(3) . ? C10 C9 1.505(3) . ? Ag1 N2 2.3033(19) 3_656 ? Ag1 S1 2.5437(7) . ? Ag1 N1 2.5749(19) . ? Ag1 S3 2.6504(6) . ? Ag1 S2 2.9605(7) . ? S3 C7 1.807(3) . ? S3 C6 1.815(2) . ? S2 C4 1.811(3) . ? S2 C5 1.811(3) . ? S1 C2 1.812(3) . ? S1 C3 1.815(3) . ? S4 O2 1.406(3) . ? S4 O1 1.406(4) . ? S4 O3 1.432(3) . ? S4 C15 1.774(4) . ? C11 N2 1.344(3) . ? C11 H11 0.9300 . ? N1 C9 1.480(3) . ? N1 C1 1.481(3) . ? N1 C8 1.481(3) . ? N2 C12 1.338(3) . ? N2 Ag1 2.3033(19) 3_656 ? C6 C5 1.516(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.509(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C13 1.374(4) . ? C12 H12 0.9300 . ? C14 C13 1.376(4) . ? C14 H14 0.9300 . ? C2 C1 1.523(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C3 1.513(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C13 H13 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? F3 C15 1.326(4) . ? F2 C15 1.310(4) . ? F1 C15 1.299(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N3 C17 1.130(5) . ? C17 C16 1.438(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 C11 C10 C14 117.1(2) . . ? C11 C10 C9 120.9(2) . . ? C14 C10 C9 122.0(2) . . ? N2 Ag1 S1 122.48(5) 3_656 . ? N2 Ag1 N1 140.65(6) 3_656 . ? S1 Ag1 N1 78.89(5) . . ? N2 Ag1 S3 103.85(5) 3_656 . ? S1 Ag1 S3 128.53(2) . . ? N1 Ag1 S3 78.62(4) . . ? N2 Ag1 S2 94.81(5) 3_656 . ? S1 Ag1 S2 78.95(2) . . ? N1 Ag1 S2 123.15(4) . . ? S3 Ag1 S2 75.864(19) . . ? C7 S3 C6 101.21(12) . . ? C7 S3 Ag1 98.15(8) . . ? C6 S3 Ag1 103.00(8) . . ? C4 S2 C5 102.73(13) . . ? C4 S2 Ag1 92.89(9) . . ? C5 S2 Ag1 100.21(8) . . ? C2 S1 C3 101.85(13) . . ? C2 S1 Ag1 98.08(9) . . ? C3 S1 Ag1 106.21(10) . . ? O2 S4 O1 115.9(3) . . ? O2 S4 O3 114.3(2) . . ? O1 S4 O3 114.7(3) . . ? O2 S4 C15 104.76(19) . . ? O1 S4 C15 101.6(3) . . ? O3 S4 C15 103.18(16) . . ? N2 C11 C10 123.8(2) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? C9 N1 C1 108.84(18) . . ? C9 N1 C8 108.75(19) . . ? C1 N1 C8 109.40(19) . . ? C9 N1 Ag1 117.28(13) . . ? C1 N1 Ag1 107.26(15) . . ? C8 N1 Ag1 105.09(13) . . ? C12 N2 C11 117.6(2) . . ? C12 N2 Ag1 113.08(15) . 3_656 ? C11 N2 Ag1 127.71(15) . 3_656 ? C5 C6 S3 111.16(18) . . ? C5 C6 H6A 109.4 . . ? S3 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? S3 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 S3 115.59(17) . . ? C8 C7 H7A 108.4 . . ? S3 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? S3 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? N2 C12 C13 122.7(2) . . ? N2 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C13 C14 C10 119.8(2) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? C1 C2 S1 111.02(17) . . ? C1 C2 H2A 109.4 . . ? S1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? S1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C3 C4 S2 110.9(2) . . ? C3 C4 H4A 109.5 . . ? S2 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C12 C13 C14 119.0(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C6 C5 S2 115.87(18) . . ? C6 C5 H5A 108.3 . . ? S2 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? S2 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C4 C3 S1 116.86(18) . . ? C4 C3 H3A 108.1 . . ? S1 C3 H3A 108.1 . . ? C4 C3 H3B 108.1 . . ? S1 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? N1 C9 C10 113.4(2) . . ? N1 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N1 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N1 C1 C2 115.0(2) . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? F1 C15 F2 104.7(4) . . ? F1 C15 F3 106.0(3) . . ? F2 C15 F3 106.2(4) . . ? F1 C15 S4 112.7(3) . . ? F2 C15 S4 113.4(3) . . ? F3 C15 S4 113.2(3) . . ? N1 C8 C7 114.41(19) . . ? N1 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N3 C17 C16 179.0(4) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.731 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.065