# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Thomas A. Kaden' _publ_contact_author_address ; Department of Chemistry University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email TH.KADEN@UNIBAS.CH #============================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Towards the encapsulation of Ag(I) in S6-thioether cages ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address R.Alberto ; University of Zurich Inorganic Chemistry Laboratory Winterthurer Str. 190 CH-8057 Zurich Switzerland ; K.Ortner ; University of Zurich Inorganic Chemistry Laboratory Winterthurer Str. 190 CH-8057 Zurich Switzerland ; D.Angst ; Paul Scherrer Institute Inorganic Chemistry Laboratory Winterthurer Str. 190 CH-5232 Villingen Switzerland ; P.A.Schubiger ; Paul Scherrer Institute Inorganic Chemistry Laboratory Winterthurer Str. 190 CH-5232 Villingen Switzerland ; T.A.Kaden ; University of Basel Inorganic Chemistry Laboratory Spitalstr. 51 CH-4936 Basel Switzerland ; U.Abram ; Free University of Berlin Institute of Chemistry Fabeckstrasse 34-36 D-14195 Berlin Germany ; #=============== STRUCTURE I ============================ data_ligand9 _database_code_depnum_ccdc_archive 'CCDC 292370' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Cryptant-S6-Me2 ; _chemical_name_common Cryptant-S6-Me2 _chemical_melting_point ? _chemical_formula_moiety 'C19 H36 S6' _chemical_formula_sum 'C19 H36 S6' _chemical_formula_weight 456.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.432(1) _cell_length_b 27.584(2) _cell_length_c 9.901(1) _cell_angle_alpha 90.00 _cell_angle_beta 114.26(1) _cell_angle_gamma 90.00 _cell_volume 2348.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.68 _cell_measurement_theta_max 23.86 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 5.374 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4995 _exptl_absorpt_correction_T_max 0.4995 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 6 _diffrn_reflns_number 4265 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.39 _diffrn_reflns_theta_max 64.00 _reflns_number_total 3831 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction PLATON _computing_structure_solution SHELXS97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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^)+(0.1619P)^2^+12.7043P] 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 SHELXL _refine_ls_extinction_coef 0.0035(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 3831 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.2235 _refine_ls_wR_factor_gt 0.1989 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.000 _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 C1 C -0.2903(11) 0.4740(3) 0.1877(11) 0.055(2) Uani 1 1 d . . . H1A H -0.3537 0.4872 0.2351 0.082 Uiso 1 1 calc R . . H1B H -0.3571 0.4605 0.0922 0.082 Uiso 1 1 calc R . . H1C H -0.2270 0.4996 0.1738 0.082 Uiso 1 1 calc R . . C2 C -0.1851(9) 0.4343(3) 0.2851(9) 0.0422(17) Uani 1 1 d . . . C3 C -0.0867(11) 0.4145(3) 0.2057(10) 0.050(2) Uani 1 1 d . . . H3A H -0.0470 0.4423 0.1703 0.060 Uiso 1 1 calc R . . H3B H -0.1566 0.3966 0.1181 0.060 Uiso 1 1 calc R . . S1 S 0.0756(2) 0.37560(8) 0.3073(3) 0.0517(6) Uani 1 1 d . . . C4 C -0.2802(10) 0.3923(3) 0.3071(10) 0.0481(19) Uani 1 1 d . . . H4A H -0.2089 0.3681 0.3727 0.058 Uiso 1 1 calc R . . H4B H -0.3393 0.3768 0.2113 0.058 Uiso 1 1 calc R . . S2 S -0.4147(3) 0.41203(9) 0.3862(3) 0.0617(7) Uani 1 1 d . . . C5 C -0.0814(10) 0.4556(3) 0.4372(9) 0.0476(19) Uani 1 1 d . . . H5A H -0.0126 0.4301 0.4982 0.057 Uiso 1 1 calc R . . H5B H -0.1475 0.4662 0.4864 0.057 Uiso 1 1 calc R . . S3 S 0.0356(3) 0.50616(8) 0.4277(2) 0.0527(6) Uani 1 1 d . . . C6 C -0.0040(11) 0.3159(3) 0.2582(10) 0.0481(19) Uani 1 1 d . . . H6A H -0.0897 0.3117 0.2887 0.058 Uiso 1 1 calc R . . H6B H -0.0458 0.3120 0.1504 0.058 Uiso 1 1 calc R . . C7 C 0.1183(10) 0.2776(3) 0.3314(10) 0.049(2) Uani 1 1 d . . . H7A H 0.1980 0.2802 0.2922 0.059 Uiso 1 1 calc R . . H7B H 0.0696 0.2456 0.3033 0.059 Uiso 1 1 calc R . . C8 C 0.1979(10) 0.2802(3) 0.4998(9) 0.051(2) Uani 1 1 d . . . H8A H 0.2523 0.3113 0.5304 0.062 Uiso 1 1 calc R . . H8B H 0.2745 0.2541 0.5379 0.062 Uiso 1 1 calc R . . S4 S 0.0523(3) 0.27439(9) 0.5741(2) 0.0541(6) Uani 1 1 d . . . C9 C -0.4782(10) 0.3544(4) 0.4236(11) 0.058(2) Uani 1 1 d . . . H9A H -0.5672 0.3597 0.4488 0.069 Uiso 1 1 calc R . . H9B H -0.5150 0.3351 0.3325 0.069 Uiso 1 1 calc R . . C10 C -0.3569(10) 0.3249(3) 0.5471(10) 0.052(2) Uani 1 1 d . . . H10A H -0.4009 0.2930 0.5509 0.063 Uiso 1 1 calc R . . H10B H -0.2671 0.3198 0.5229 0.063 Uiso 1 1 calc R . . C11 C -0.3015(11) 0.3478(4) 0.6978(10) 0.055(2) Uani 1 1 d . . . H11A H -0.3832 0.3443 0.7342 0.066 Uiso 1 1 calc R . . H11B H -0.2865 0.3826 0.6878 0.066 Uiso 1 1 calc R . . S5 S -0.1244(3) 0.32318(10) 0.8335(2) 0.0598(6) Uani 1 1 d . . . C12 C 0.1931(11) 0.5012(3) 0.6067(10) 0.051(2) Uani 1 1 d . . . H12A H 0.2453 0.5327 0.6335 0.061 Uiso 1 1 calc R . . H12B H 0.1506 0.4936 0.6795 0.061 Uiso 1 1 calc R . . C13 C 0.3135(10) 0.4628(3) 0.6170(10) 0.052(2) Uani 1 1 d . . . H13A H 0.2595 0.4336 0.5652 0.063 Uiso 1 1 calc R . . H13B H 0.3768 0.4748 0.5666 0.063 Uiso 1 1 calc R . . C14 C 0.4192(11) 0.4497(3) 0.7746(10) 0.054(2) Uani 1 1 d . . . H14A H 0.4691 0.4795 0.8264 0.064 Uiso 1 1 calc R . . H14B H 0.5015 0.4285 0.7723 0.064 Uiso 1 1 calc R . . S6 S 0.3297(3) 0.42010(8) 0.8824(2) 0.0519(6) Uani 1 1 d . . . C15 C 0.1622(11) 0.2800(3) 0.7726(9) 0.049(2) Uani 1 1 d . . . H15A H 0.1154 0.2584 0.8217 0.059 Uiso 1 1 calc R . . H15B H 0.2681 0.2683 0.7972 0.059 Uiso 1 1 calc R . . C16 C 0.0137(10) 0.3565(3) 0.7847(9) 0.0458(18) Uani 1 1 d . . . H16A H -0.0282 0.3598 0.6767 0.055 Uiso 1 1 calc R . . H16B H 0.0261 0.3892 0.8269 0.055 Uiso 1 1 calc R . . C17 C 0.2843(10) 0.3620(3) 0.7913(9) 0.0448(18) Uani 1 1 d . . . H17A H 0.2354 0.3668 0.6838 0.054 Uiso 1 1 calc R . . H17B H 0.3807 0.3437 0.8152 0.054 Uiso 1 1 calc R . . C18 C 0.1734(10) 0.3322(3) 0.8396(8) 0.0424(18) Uani 1 1 d . . . C19 C 0.2448(12) 0.3257(4) 1.0087(9) 0.055(2) Uani 1 1 d . . . H19A H 0.3454 0.3101 1.0400 0.082 Uiso 1 1 calc R . . H19B H 0.1767 0.3058 1.0369 0.082 Uiso 1 1 calc R . . H19C H 0.2575 0.3572 1.0559 0.082 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 C1 0.051(5) 0.050(5) 0.057(5) 0.012(4) 0.015(4) 0.007(4) C2 0.043(4) 0.042(4) 0.045(4) 0.008(3) 0.022(3) 0.000(3) C3 0.068(6) 0.039(4) 0.051(5) 0.003(4) 0.033(4) 0.001(4) S1 0.0456(11) 0.0447(11) 0.0677(13) -0.0059(9) 0.0262(10) -0.0010(9) C4 0.044(4) 0.044(4) 0.063(5) 0.003(4) 0.028(4) -0.004(4) S2 0.0567(14) 0.0548(13) 0.0896(18) 0.0196(12) 0.0464(13) 0.0120(10) C5 0.054(5) 0.046(4) 0.051(4) 0.005(4) 0.030(4) 0.005(4) S3 0.0617(13) 0.0458(11) 0.0524(12) 0.0019(9) 0.0251(10) -0.0085(10) C6 0.061(5) 0.038(4) 0.049(4) -0.003(3) 0.026(4) 0.001(4) C7 0.057(5) 0.042(4) 0.054(5) -0.004(4) 0.028(4) 0.005(4) C8 0.049(5) 0.055(5) 0.049(5) 0.002(4) 0.019(4) 0.010(4) S4 0.0589(13) 0.0593(13) 0.0499(11) -0.0094(10) 0.0282(10) -0.0150(11) C9 0.043(5) 0.067(6) 0.065(5) 0.018(5) 0.023(4) -0.003(4) C10 0.048(5) 0.053(5) 0.062(5) 0.001(4) 0.030(4) -0.003(4) C11 0.060(5) 0.058(5) 0.059(5) -0.002(4) 0.037(4) -0.005(4) S5 0.0583(14) 0.0728(15) 0.0523(12) 0.0105(11) 0.0266(11) -0.0107(11) C12 0.057(5) 0.048(5) 0.050(5) -0.008(4) 0.024(4) -0.009(4) C13 0.053(5) 0.053(5) 0.059(5) -0.011(4) 0.031(4) -0.007(4) C14 0.053(5) 0.048(5) 0.059(5) -0.003(4) 0.023(4) -0.010(4) S6 0.0580(13) 0.0465(11) 0.0543(12) -0.0098(9) 0.0263(10) -0.0098(10) C15 0.066(5) 0.036(4) 0.053(5) 0.001(3) 0.031(4) -0.003(4) C16 0.047(4) 0.043(4) 0.051(4) 0.003(4) 0.024(4) 0.000(4) C17 0.042(4) 0.045(4) 0.057(5) -0.002(4) 0.030(4) 0.000(3) C18 0.052(5) 0.039(4) 0.039(4) 0.004(3) 0.021(4) -0.001(3) C19 0.064(6) 0.057(5) 0.043(4) -0.002(4) 0.022(4) 0.002(4) _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 C1 C2 1.526(11) . ? C2 C4 1.535(11) . ? C2 C5 1.536(12) . ? C2 C3 1.542(11) . ? C3 S1 1.800(9) . ? S1 C6 1.792(8) . ? C4 S2 1.826(8) . ? S2 C9 1.791(9) . ? C5 S3 1.805(9) . ? S3 C12 1.790(9) . ? C6 C7 1.512(12) . ? C7 C8 1.523(12) . ? C8 S4 1.813(9) . ? S4 C15 1.813(9) . ? C9 C10 1.522(13) . ? C10 C11 1.503(13) . ? C11 S5 1.793(10) . ? S5 C16 1.815(8) . ? C12 C13 1.525(13) . ? C13 C14 1.510(13) . ? C14 S6 1.805(9) . ? S6 C17 1.803(8) . ? C15 C18 1.571(11) . ? C16 C18 1.530(12) . ? C17 C18 1.552(11) . ? C18 C19 1.537(11) . ? 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 C1 C2 C4 111.4(7) . . ? C1 C2 C5 109.4(7) . . ? C4 C2 C5 108.9(7) . . ? C1 C2 C3 107.7(7) . . ? C4 C2 C3 108.3(7) . . ? C5 C2 C3 111.2(7) . . ? C2 C3 S1 118.6(6) . . ? C6 S1 C3 103.3(4) . . ? C2 C4 S2 112.7(6) . . ? C9 S2 C4 100.1(4) . . ? C2 C5 S3 113.6(5) . . ? C12 S3 C5 99.5(4) . . ? C7 C6 S1 111.1(6) . . ? C6 C7 C8 115.3(7) . . ? C7 C8 S4 109.0(6) . . ? C8 S4 C15 103.9(4) . . ? C10 C9 S2 115.8(7) . . ? C11 C10 C9 114.4(8) . . ? C10 C11 S5 114.9(7) . . ? C11 S5 C16 99.1(4) . . ? C13 C12 S3 114.3(6) . . ? C14 C13 C12 113.1(7) . . ? C13 C14 S6 116.6(6) . . ? C17 S6 C14 100.4(4) . . ? C18 C15 S4 116.4(6) . . ? C18 C16 S5 113.1(6) . . ? C18 C17 S6 111.6(5) . . ? C16 C18 C19 111.4(7) . . ? C16 C18 C17 110.4(6) . . ? C19 C18 C17 110.3(7) . . ? C16 C18 C15 111.6(7) . . ? C19 C18 C15 106.1(7) . . ? C17 C18 C15 107.0(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 64.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.428 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.093 ############################### STRUCTURE 4 ######################## data_ag24 _database_code_depnum_ccdc_archive 'CCDC 292371' _audit_creation_method SHELXL-97 _chemical_name_systematic 'S6-Ethylenecagesilver(I) trifluoromethylsulfonate' _chemical_name_common 'S6-Ethylenecagesilver(i) trifluoromethylsulfonate' _chemical_formula_moiety 'C21 H38 Ag F3 O3 S7' _chemical_formula_sum 'C21 H38 Ag F3 O3 S7' _chemical_formula_weight 727.80 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' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 10.3960(10) _cell_length_b 15.421(2) _cell_length_c 18.421(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2953.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 6.88 _cell_measurement_theta_max 13.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_correction_T_min 0.9050 _exptl_absorpt_correction_T_max 0.9552 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 5.5 _diffrn_reflns_number 6656 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 26.49 _reflns_number_total 6098 _reflns_number_gt 3743 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'PLATON, HELENA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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 w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+11.7659P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(6) _refine_ls_number_reflns 6098 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1410 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.79144(9) 0.02072(6) 0.97389(4) 0.0644(3) Uani 1 d . . . C1 C 0.3694(12) 0.1156(8) 0.8885(6) 0.070(3) Uani 1 d . . . H1 H 0.3261 0.1723 0.8947 0.084 Uiso 1 calc R . . C2 C 0.5136(11) 0.1308(8) 0.8893(6) 0.067(3) Uani 1 d . . . H2A H 0.5394 0.1574 0.8432 0.081 Uiso 1 calc R . . H2B H 0.5577 0.0748 0.8934 0.081 Uiso 1 calc R . . C3 C 0.5558(13) 0.1890(8) 0.9516(6) 0.073(4) Uani 1 d . . . H3A H 0.5080 0.1726 0.9953 0.087 Uiso 1 calc R . . H3B H 0.5327 0.2490 0.9398 0.087 Uiso 1 calc R . . S4 S 0.7313(3) 0.18456(18) 0.97214(17) 0.0646(7) Uani 1 d . . . C5 C 0.8074(14) 0.2247(7) 0.8918(6) 0.072(3) Uani 1 d . . . H5A H 0.7569 0.2075 0.8493 0.087 Uiso 1 calc R . . H5B H 0.8095 0.2883 0.8935 0.087 Uiso 1 calc R . . C6 C 0.9453(14) 0.1900(9) 0.8840(7) 0.084(4) Uani 1 d . . . H6A H 0.9919 0.2020 0.9291 0.101 Uiso 1 calc R . . H6B H 0.9881 0.2224 0.8451 0.101 Uiso 1 calc R . . S7 S 0.9595(3) 0.0757(2) 0.86442(15) 0.0622(8) Uani 1 d . . . C8 C 0.9129(10) 0.0746(7) 0.7694(5) 0.054(3) Uani 1 d . . . H8A H 0.8232 0.0936 0.7652 0.064 Uiso 1 calc R . . H8B H 0.9664 0.1160 0.7426 0.064 Uiso 1 calc R . . C9 C 0.9267(9) -0.0146(7) 0.7353(5) 0.054(3) Uani 1 d . . . H9A H 0.9911 -0.0471 0.7630 0.065 Uiso 1 calc R . . H9B H 0.9603 -0.0073 0.6860 0.065 Uiso 1 calc R . . C10 C 0.8044(11) -0.0695(7) 0.7310(5) 0.054(3) Uani 1 d . . . H10 H 0.8311 -0.1271 0.7127 0.065 Uiso 1 calc R . . C12 C 0.3292(13) 0.0567(9) 0.9522(6) 0.077(4) Uani 1 d . . . H12A H 0.3427 0.0892 0.9972 0.093 Uiso 1 calc R . . H12B H 0.2366 0.0460 0.9479 0.093 Uiso 1 calc R . . C13 C 0.3953(12) -0.0304(10) 0.9604(6) 0.081(4) Uani 1 d . . . H13A H 0.4260 -0.0495 0.9127 0.097 Uiso 1 calc R . . H13B H 0.3324 -0.0731 0.9776 0.097 Uiso 1 calc R . . S14 S 0.5290(3) -0.0279(2) 1.02248(15) 0.0770(8) Uani 1 d . . . C15 C 0.5703(12) -0.1410(8) 1.0263(7) 0.081(4) Uani 1 d . . . H15A H 0.6289 -0.1499 1.0673 0.098 Uiso 1 calc R . . H15B H 0.4919 -0.1741 1.0363 0.098 Uiso 1 calc R . . C16 C 0.6327(13) -0.1777(8) 0.9586(7) 0.075(4) Uani 1 d . . . H16A H 0.5827 -0.1603 0.9159 0.090 Uiso 1 calc R . . H16B H 0.6321 -0.2412 0.9611 0.090 Uiso 1 calc R . . S17 S 0.7985(3) -0.13956(19) 0.94860(14) 0.0638(7) Uani 1 d . . . C18 C 0.8258(11) -0.1439(7) 0.8532(6) 0.063(3) Uani 1 d . . . H18A H 0.9161 -0.1289 0.8443 0.076 Uiso 1 calc R . . H18B H 0.8137 -0.2040 0.8373 0.076 Uiso 1 calc R . . C19 C 0.7416(9) -0.0852(7) 0.8046(5) 0.052(3) Uani 1 d . . . H19A H 0.6575 -0.1126 0.7974 0.063 Uiso 1 calc R . . H19B H 0.7278 -0.0295 0.8289 0.063 Uiso 1 calc R . . C22 C 0.3267(12) 0.0767(7) 0.8145(6) 0.068(3) Uani 1 d . . . H22A H 0.3836 0.0283 0.8022 0.082 Uiso 1 calc R . . H22B H 0.2392 0.0538 0.8193 0.082 Uiso 1 calc R . . C23 C 0.3295(11) 0.1418(9) 0.7541(7) 0.072(3) Uani 1 d . . . H23A H 0.4190 0.1510 0.7392 0.087 Uiso 1 calc R . . H23B H 0.2962 0.1972 0.7722 0.087 Uiso 1 calc R . . S24 S 0.2384(3) 0.1103(2) 0.67689(18) 0.0695(9) Uani 1 d . . . C25 C 0.3259(9) 0.0167(8) 0.6445(5) 0.058(3) Uani 1 d . . . H25A H 0.3512 -0.0189 0.6862 0.069 Uiso 1 calc R . . H25B H 0.2688 -0.0183 0.6139 0.069 Uiso 1 calc R . . C26 C 0.4440(9) 0.0399(6) 0.6018(5) 0.046(2) Uani 1 d . . . H26A H 0.5026 0.0741 0.6321 0.055 Uiso 1 calc R . . H26B H 0.4198 0.0752 0.5597 0.055 Uiso 1 calc R . . S27 S 0.5246(3) -0.05804(18) 0.57144(14) 0.0511(6) Uani 1 d . . . C28 C 0.6076(9) -0.0943(7) 0.6504(5) 0.047(2) Uani 1 d . . . H28A H 0.5453 -0.1015 0.6899 0.056 Uiso 1 calc R . . H28B H 0.6453 -0.1513 0.6404 0.056 Uiso 1 calc R . . C29 C 0.7138(11) -0.0333(7) 0.6758(5) 0.055(2) Uani 1 d . . . H29A H 0.7639 -0.0154 0.6333 0.065 Uiso 1 calc R . . H29B H 0.6737 0.0188 0.6961 0.065 Uiso 1 calc R . . S30 S 0.8508(3) -0.2680(2) 1.18063(18) 0.0633(8) Uani 1 d . . . O31 O 0.9345(7) -0.3389(6) 1.1979(5) 0.075(2) Uani 1 d . . . O32 O 0.8552(10) -0.2463(7) 1.1027(5) 0.103(3) Uani 1 d . . . O33 O 0.8489(8) -0.1975(6) 1.2281(5) 0.081(3) Uani 1 d . . . C34 C 0.715(2) -0.3140(7) 1.1917(9) 0.148(10) Uani 1 d . . . F35 F 0.6764(6) -0.3796(5) 1.1406(5) 0.089(2) Uani 1 d . . . F36 F 0.6790(8) -0.3475(5) 1.2545(4) 0.102(3) Uani 1 d . . . F37 F 0.6011(7) -0.2581(5) 1.1763(6) 0.100(3) Uani 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 0.0711(6) 0.0619(5) 0.0603(4) -0.0049(4) -0.0111(5) -0.0001(5) C1 0.062(8) 0.076(9) 0.073(7) -0.022(6) 0.008(6) 0.005(7) C2 0.064(8) 0.075(9) 0.063(6) -0.011(6) -0.014(6) 0.010(7) C3 0.094(9) 0.055(7) 0.069(7) -0.021(6) -0.017(7) 0.018(7) S4 0.073(2) 0.0538(16) 0.0671(14) -0.0127(14) -0.0186(16) 0.0022(15) C5 0.091(10) 0.046(7) 0.079(7) -0.003(6) -0.011(7) -0.015(7) C6 0.087(10) 0.094(11) 0.071(8) 0.000(7) -0.015(7) -0.045(9) S7 0.0510(17) 0.079(2) 0.0565(15) 0.0007(14) -0.0089(13) -0.0080(16) C8 0.048(6) 0.058(8) 0.054(6) 0.007(5) -0.001(5) -0.012(5) C9 0.045(6) 0.059(7) 0.058(5) 0.005(6) -0.001(4) -0.005(6) C10 0.052(6) 0.050(6) 0.062(6) 0.009(5) 0.002(5) -0.006(6) C12 0.085(9) 0.093(9) 0.053(6) -0.006(6) 0.010(6) -0.020(8) C13 0.079(8) 0.105(11) 0.059(7) 0.009(8) 0.002(6) -0.020(8) S14 0.091(2) 0.088(2) 0.0523(13) -0.0002(18) -0.0025(16) -0.012(2) C15 0.081(9) 0.095(10) 0.068(7) 0.030(8) -0.003(8) -0.019(8) C16 0.086(9) 0.059(8) 0.081(9) 0.016(6) 0.005(7) -0.026(7) S17 0.0671(18) 0.0622(18) 0.0619(15) 0.0182(13) -0.0127(14) -0.0056(17) C18 0.058(8) 0.052(7) 0.079(7) -0.002(6) 0.004(6) 0.003(6) C19 0.047(6) 0.055(7) 0.054(5) -0.003(5) -0.006(5) -0.002(5) C22 0.065(8) 0.061(8) 0.079(7) -0.002(6) 0.002(6) -0.002(6) C23 0.049(7) 0.077(9) 0.091(8) -0.001(7) 0.014(6) 0.005(6) S24 0.0500(19) 0.073(2) 0.0850(19) -0.0046(16) 0.0086(15) 0.0079(15) C25 0.045(6) 0.066(7) 0.062(5) -0.010(6) 0.005(4) -0.004(6) C26 0.036(5) 0.041(7) 0.059(5) 0.001(4) 0.000(4) 0.007(4) S27 0.0562(16) 0.0496(16) 0.0474(13) -0.0021(11) 0.0023(12) -0.0010(14) C28 0.044(6) 0.045(6) 0.052(5) -0.003(5) -0.003(4) -0.011(5) C29 0.054(6) 0.054(7) 0.055(5) 0.000(5) -0.001(5) -0.008(6) S30 0.0419(15) 0.065(2) 0.083(2) -0.0050(17) -0.0064(14) 0.0051(15) O31 0.051(5) 0.079(6) 0.094(6) 0.011(5) -0.013(4) 0.026(4) O32 0.093(7) 0.139(9) 0.077(6) 0.053(6) 0.009(5) 0.005(6) O33 0.049(5) 0.078(6) 0.117(7) -0.036(5) 0.011(5) -0.014(4) C34 0.30(3) 0.005(5) 0.136(12) 0.006(7) 0.138(16) -0.004(10) F35 0.055(4) 0.073(5) 0.139(6) -0.031(4) 0.002(4) -0.006(4) F36 0.101(7) 0.091(6) 0.114(6) 0.016(5) 0.009(5) -0.038(5) F37 0.049(4) 0.056(5) 0.194(9) -0.009(5) -0.023(5) 0.013(4) _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 S17 2.516(3) . ? Ag S4 2.603(3) . ? Ag S27 2.687(3) 4_655 ? Ag S7 2.800(3) . ? Ag S14 2.967(3) . ? C1 C2 1.517(16) . ? C1 C12 1.541(16) . ? C1 C22 1.553(15) . ? C2 C3 1.522(14) . ? C3 S4 1.864(13) . ? S4 C5 1.789(12) . ? C5 C6 1.538(19) . ? C6 S7 1.805(14) . ? S7 C8 1.817(10) . ? C8 C9 1.519(15) . ? C9 C10 1.530(14) . ? C10 C29 1.494(14) . ? C10 C19 1.523(13) . ? C12 C13 1.516(17) . ? C13 S14 1.800(12) . ? S14 C15 1.797(13) . ? C15 C16 1.516(17) . ? C16 S17 1.831(12) . ? S17 C18 1.782(11) . ? C18 C19 1.545(14) . ? C22 C23 1.499(16) . ? C23 S24 1.776(13) . ? S24 C25 1.807(11) . ? C25 C26 1.502(13) . ? C26 S27 1.815(9) . ? S27 C28 1.781(10) . ? S27 Ag 2.687(3) 4_654 ? C28 C29 1.523(13) . ? S30 O33 1.395(8) . ? S30 O31 1.434(8) . ? S30 O32 1.474(8) . ? S30 C34 1.60(2) . ? C34 F36 1.320(14) . ? C34 F35 1.438(18) . ? C34 F37 1.49(2) . ? 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 S17 Ag S4 163.37(10) . . ? S17 Ag S27 108.26(9) . 4_655 ? S4 Ag S27 88.36(9) . 4_655 ? S17 Ag S7 98.39(10) . . ? S4 Ag S7 81.21(10) . . ? S27 Ag S7 88.43(8) 4_655 . ? S17 Ag S14 80.48(11) . . ? S4 Ag S14 91.61(10) . . ? S27 Ag S14 120.45(9) 4_655 . ? S7 Ag S14 150.18(9) . . ? C2 C1 C12 110.6(11) . . ? C2 C1 C22 110.5(9) . . ? C12 C1 C22 111.3(10) . . ? C1 C2 C3 112.6(10) . . ? C2 C3 S4 114.4(8) . . ? C5 S4 C3 104.6(6) . . ? C5 S4 Ag 103.9(4) . . ? C3 S4 Ag 105.9(4) . . ? C6 C5 S4 111.7(9) . . ? C5 C6 S7 115.8(9) . . ? C6 S7 C8 100.3(6) . . ? C6 S7 Ag 95.8(5) . . ? C8 S7 Ag 121.6(4) . . ? C9 C8 S7 112.4(7) . . ? C8 C9 C10 116.4(9) . . ? C29 C10 C19 113.3(9) . . ? C29 C10 C9 110.6(8) . . ? C19 C10 C9 113.4(8) . . ? C13 C12 C1 118.4(11) . . ? C12 C13 S14 113.2(9) . . ? C15 S14 C13 100.9(7) . . ? C15 S14 Ag 92.2(4) . . ? C13 S14 Ag 121.6(4) . . ? C16 C15 S14 115.6(8) . . ? C15 C16 S17 111.4(9) . . ? C18 S17 C16 103.7(6) . . ? C18 S17 Ag 102.9(4) . . ? C16 S17 Ag 105.6(4) . . ? C19 C18 S17 117.3(8) . . ? C10 C19 C18 111.4(9) . . ? C23 C22 C1 112.8(10) . . ? C22 C23 S24 113.6(9) . . ? C23 S24 C25 102.4(5) . . ? C26 C25 S24 113.2(8) . . ? C25 C26 S27 109.9(7) . . ? C28 S27 C26 103.5(5) . . ? C28 S27 Ag 105.6(3) . 4_654 ? C26 S27 Ag 110.9(3) . 4_654 ? C29 C28 S27 114.1(7) . . ? C10 C29 C28 115.8(8) . . ? O33 S30 O31 117.7(6) . . ? O33 S30 O32 115.7(6) . . ? O31 S30 O32 111.7(6) . . ? O33 S30 C34 104.7(6) . . ? O31 S30 C34 99.8(7) . . ? O32 S30 C34 104.6(8) . . ? F36 C34 F35 102.7(10) . . ? F36 C34 F37 99.9(13) . . ? F35 C34 F37 93.6(16) . . ? F36 C34 S30 122.4(18) . . ? F35 C34 S30 118.3(10) . . ? F37 C34 S30 114.9(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.823 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.093 #################################### STRUCTURE 5 ###################### data_agcage _database_code_depnum_ccdc_archive 'CCDC 292372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ag2(3-S6-cage-3-NO2)(triflat)2] x 2 AN' _chemical_formula_moiety '[Ag2(3-S6-cage-3-NO2)(triflat)2] x 2 AN' _chemical_formula_sum 'C35 H60 Ag2 F6 N4 O10 S8' _chemical_formula_weight 1283.09 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' 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' F F 0.0171 0.0103 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.614(8) _cell_length_b 13.491(2) _cell_length_c 18.364(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.70(2) _cell_angle_gamma 90.00 _cell_volume 5041(3) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.32 _cell_measurement_theta_max 13.56 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.75096 _exptl_absorpt_correction_T_max 0.87360 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 7.5 _diffrn_reflns_number 12148 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.96 _reflns_number_total 5466 _reflns_number_gt 3365 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction 'HELENA, PLATON (Spek, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1997), SCHAKAL (Keller, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+13.4022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary PATTERSON _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5466 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.30946(2) 0.50960(3) 0.21119(2) 0.04497(14) Uani 1 d . . . O1 O 0.5540(2) 0.8089(3) 0.5517(2) 0.0661(13) Uani 1 d . . . O2 O 0.5742(3) 0.9255(4) 0.4847(3) 0.0879(17) Uani 1 d . . . N3 N 0.5501(2) 0.8455(3) 0.4903(3) 0.0447(11) Uani 1 d . . . C4 C 0.5124(2) 0.7912(4) 0.4143(3) 0.0317(10) Uani 1 d . . . C5 C 0.4979(2) 0.6870(3) 0.4362(2) 0.0299(10) Uani 1 d . . . H5A H 0.4727 0.6918 0.4709 0.036 Uiso 1 calc R . . H5B H 0.5391 0.6545 0.4641 0.036 Uiso 1 calc R . . C6 C 0.4600(2) 0.6224(3) 0.3673(3) 0.0323(10) Uani 1 d . . . H6A H 0.4175 0.6519 0.3407 0.039 Uiso 1 calc R . . H6B H 0.4840 0.6185 0.3312 0.039 Uiso 1 calc R . . C7 C 0.4510(2) 0.5196(3) 0.3947(3) 0.0320(10) Uani 1 d . . . H7A H 0.4310 0.5257 0.4345 0.038 Uiso 1 calc R . . H7B H 0.4940 0.4902 0.4185 0.038 Uiso 1 calc R . . S8 S 0.40145(6) 0.43499(9) 0.32104(7) 0.0335(3) Uani 1 d . . . C9 C 0.4609(2) 0.3747(4) 0.2861(3) 0.0370(11) Uani 1 d . . . H9A H 0.4918 0.3394 0.3292 0.044 Uiso 1 calc R . . H9B H 0.4379 0.3255 0.2481 0.044 Uiso 1 calc R . . C10 C 0.5000 0.4399(5) 0.2500 0.0299(14) Uani 1 d S . . H10A H 0.5296 0.4820 0.2892 0.036 Uiso 0.50 calc PR . . H10B H 0.4704 0.4820 0.2108 0.036 Uiso 0.50 calc PR . . C11 C 0.5564(2) 0.7944(4) 0.3649(3) 0.0376(11) Uani 1 d . . . H11A H 0.5669 0.8632 0.3588 0.045 Uiso 1 calc R . . H11B H 0.5317 0.7692 0.3139 0.045 Uiso 1 calc R . . C12 C 0.6207(3) 0.7366(4) 0.3954(3) 0.0480(14) Uani 1 d . . . H12A H 0.6459 0.7591 0.4470 0.058 Uiso 1 calc R . . H12B H 0.6115 0.6666 0.3980 0.058 Uiso 1 calc R . . C13 C 0.6595(3) 0.7524(5) 0.3421(4) 0.0565(16) Uani 1 d . . . H13A H 0.6759 0.8198 0.3474 0.068 Uiso 1 calc R A 1 H13B H 0.6312 0.7428 0.2890 0.068 Uiso 1 calc R A 1 S14A S 0.72830(7) 0.66583(11) 0.36499(8) 0.0386(5) Uani 0.915(5) d P . 1 S14B S 0.3144(8) 0.6888(15) 0.1835(11) 0.055(6) Uani 0.085(5) d P . 2 C15 C 0.7854(3) 0.7323(4) 0.3310(3) 0.0465(13) Uani 1 d . . . H15A H 0.7824 0.8016 0.3434 0.056 Uiso 1 calc R B 1 H15B H 0.8291 0.7103 0.3620 0.056 Uiso 1 calc R B 1 C16 C 0.7821(3) 0.7284(4) 0.2486(3) 0.0558(16) Uani 1 d . . . H16A H 0.8215 0.7596 0.2456 0.067 Uiso 1 calc R . . H16B H 0.7839 0.6591 0.2352 0.067 Uiso 1 calc R . . C17 C 0.7266(3) 0.7725(4) 0.1895(3) 0.0512(15) Uani 1 d . . . H17A H 0.6880 0.7323 0.1836 0.061 Uiso 1 calc R . . H17B H 0.7348 0.7706 0.1407 0.061 Uiso 1 calc R . . C21 C 0.4508(2) 0.8543(4) 0.3768(3) 0.0344(11) Uani 1 d . . . H21A H 0.4647 0.9200 0.3675 0.041 Uiso 1 calc R . . H21B H 0.4266 0.8256 0.3269 0.041 Uiso 1 calc R . . C22 C 0.4046(3) 0.8649(4) 0.4221(3) 0.0422(13) Uani 1 d . . . H22A H 0.4294 0.8885 0.4736 0.051 Uiso 1 calc R . . H22B H 0.3875 0.7998 0.4276 0.051 Uiso 1 calc R . . C23 C 0.3471(3) 0.9343(4) 0.3869(3) 0.0420(13) Uani 1 d . . . H23A H 0.3643 0.9998 0.3834 0.050 Uiso 1 calc R . . H23B H 0.3221 0.9386 0.4218 0.050 Uiso 1 calc R . . S24 S 0.29147(6) 0.89964(9) 0.29183(7) 0.0348(3) Uani 1 d . . . O31 O 0.3220(2) 0.3936(4) 0.1091(2) 0.0750(14) Uani 1 d . . . S32 S 0.34794(7) 0.41187(11) 0.04851(8) 0.0460(3) Uani 1 d . . . O33 O 0.3775(3) 0.3304(4) 0.0245(3) 0.0867(16) Uani 1 d . . . O34 O 0.3859(2) 0.5003(4) 0.0591(3) 0.0810(15) Uani 1 d . . . C35 C 0.2771(3) 0.4409(7) -0.0345(4) 0.072(2) Uani 1 d . . . F36 F 0.2923(2) 0.4545(4) -0.0979(2) 0.0975(15) Uani 1 d . . . F37 F 0.2439(2) 0.5164(4) -0.0229(2) 0.0976(15) Uani 1 d . . . F38 F 0.2358(2) 0.3625(4) -0.0510(3) 0.1139(19) Uani 1 d . . . N41 N 0.4122(5) 0.0738(9) 0.2526(6) 0.155(4) Uani 1 d . . . C42 C 0.4180(6) 0.0934(7) 0.1975(6) 0.104(3) Uani 1 d . . . C43 C 0.4255(5) 0.1209(7) 0.1315(5) 0.109(3) Uani 1 d . . . H43A H 0.4088 0.0699 0.0934 0.163 Uiso 1 calc R . . H43B H 0.4713 0.1312 0.1397 0.163 Uiso 1 calc R . . H43C H 0.4018 0.1813 0.1136 0.163 Uiso 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 Ag 0.0347(2) 0.0479(3) 0.0465(2) -0.0053(2) 0.00599(16) 0.00017(19) O1 0.072(3) 0.074(3) 0.036(2) -0.017(2) -0.004(2) -0.001(2) O2 0.121(5) 0.058(3) 0.071(3) -0.025(3) 0.014(3) -0.042(3) N3 0.038(2) 0.043(3) 0.043(3) -0.013(2) 0.001(2) 0.004(2) C4 0.027(2) 0.034(3) 0.030(2) -0.005(2) 0.0041(19) -0.001(2) C5 0.028(2) 0.032(3) 0.026(2) 0.0009(19) 0.0055(19) 0.0068(19) C6 0.030(2) 0.031(3) 0.030(2) 0.001(2) 0.0016(19) -0.001(2) C7 0.031(2) 0.034(3) 0.028(2) -0.001(2) 0.0060(19) 0.000(2) S8 0.0276(6) 0.0313(6) 0.0412(7) -0.0015(5) 0.0109(5) -0.0049(5) C9 0.036(3) 0.031(3) 0.043(3) 0.000(2) 0.012(2) 0.001(2) C10 0.027(3) 0.026(3) 0.032(3) 0.000 0.004(3) 0.000 C11 0.033(3) 0.035(3) 0.045(3) 0.000(2) 0.014(2) -0.004(2) C12 0.039(3) 0.053(4) 0.055(3) 0.001(3) 0.020(3) 0.004(3) C13 0.046(3) 0.054(4) 0.069(4) 0.019(3) 0.019(3) 0.018(3) S14A 0.0335(9) 0.0395(8) 0.0399(8) 0.0034(6) 0.0086(7) 0.0058(6) S14B 0.032(10) 0.064(12) 0.067(13) -0.018(9) 0.015(9) -0.028(8) C15 0.043(3) 0.040(3) 0.054(3) 0.012(3) 0.012(3) 0.004(2) C16 0.063(4) 0.038(3) 0.071(4) 0.005(3) 0.030(3) 0.009(3) C17 0.068(4) 0.039(3) 0.043(3) -0.004(3) 0.015(3) 0.008(3) C21 0.037(3) 0.028(3) 0.034(2) -0.003(2) 0.007(2) 0.002(2) C22 0.045(3) 0.043(3) 0.032(2) -0.003(2) 0.003(2) 0.013(2) C23 0.040(3) 0.041(3) 0.037(3) -0.012(2) 0.002(2) 0.011(2) S24 0.0372(7) 0.0287(6) 0.0331(6) -0.0032(5) 0.0050(5) 0.0003(5) O31 0.089(4) 0.088(4) 0.058(3) -0.016(3) 0.039(3) -0.006(3) S32 0.0461(8) 0.0437(8) 0.0524(8) -0.0079(6) 0.0221(7) -0.0023(6) O33 0.110(4) 0.079(3) 0.087(3) -0.005(3) 0.053(3) 0.033(3) O34 0.059(3) 0.071(3) 0.100(4) -0.005(3) 0.010(3) -0.022(3) C35 0.058(4) 0.105(6) 0.060(4) -0.023(4) 0.028(4) -0.005(4) F36 0.091(3) 0.148(4) 0.050(2) 0.000(3) 0.018(2) -0.001(3) F37 0.081(3) 0.117(4) 0.076(3) -0.018(3) 0.002(2) 0.040(3) F38 0.080(3) 0.152(5) 0.105(3) -0.060(3) 0.025(3) -0.054(3) N41 0.157(9) 0.190(11) 0.120(7) 0.054(8) 0.048(7) 0.017(8) C42 0.163(10) 0.081(6) 0.099(7) 0.012(5) 0.085(7) 0.010(6) C43 0.138(9) 0.094(7) 0.093(6) 0.001(5) 0.036(6) -0.010(6) _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 S14B 2.48(2) . ? Ag S14A 2.5090(16) 2_655 ? Ag S8 2.5164(15) . ? Ag O31 2.526(4) . ? Ag S24 2.6231(15) 4_545 ? O1 N3 1.208(6) . ? O2 N3 1.217(6) . ? N3 C4 1.544(6) . ? C4 C11 1.521(7) . ? C4 C5 1.524(6) . ? C4 C21 1.533(6) . ? C5 C6 1.526(6) . ? C6 C7 1.510(6) . ? C7 S8 1.817(4) . ? S8 C9 1.811(5) . ? C9 C10 1.518(6) . ? C10 C9 1.518(6) 2_655 ? C11 C12 1.526(7) . ? C12 C13 1.501(8) . ? C13 S14B 1.206(19) 2_655 ? C13 S14A 1.825(6) . ? S14A C15 1.800(6) . ? S14A Ag 2.5090(16) 2_655 ? S14B C13 1.206(19) 2_655 ? S14B C15 2.165(19) 2_655 ? C15 C16 1.490(8) . ? C15 S14B 2.165(19) 2_655 ? C16 C17 1.448(8) . ? C17 S24 1.817(5) 2_655 ? C21 C22 1.507(7) . ? C22 C23 1.515(6) . ? C23 S24 1.816(5) . ? S24 C17 1.817(5) 2_655 ? S24 Ag 2.6231(15) 4 ? O31 S32 1.427(5) . ? S32 O33 1.415(5) . ? S32 O34 1.424(5) . ? S32 C35 1.802(7) . ? C35 F37 1.305(8) . ? C35 F36 1.325(8) . ? C35 F38 1.351(9) . ? N41 C42 1.093(10) . ? C42 C43 1.329(11) . ? 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 S14B Ag S14A 25.2(4) . 2_655 ? S14B Ag S8 118.5(4) . . ? S14A Ag S8 143.47(5) 2_655 . ? S14B Ag O31 115.4(5) . . ? S14A Ag O31 101.70(12) 2_655 . ? S8 Ag O31 95.38(12) . . ? S14B Ag S24 129.8(4) . 4_545 ? S14A Ag S24 110.57(5) 2_655 4_545 ? S8 Ag S24 102.56(5) . 4_545 ? O31 Ag S24 85.99(12) . 4_545 ? O1 N3 O2 123.0(5) . . ? O1 N3 C4 119.9(4) . . ? O2 N3 C4 117.1(5) . . ? C11 C4 C5 114.1(4) . . ? C11 C4 C21 109.8(4) . . ? C5 C4 C21 113.9(4) . . ? C11 C4 N3 106.2(4) . . ? C5 C4 N3 107.0(4) . . ? C21 C4 N3 104.9(4) . . ? C4 C5 C6 114.1(4) . . ? C7 C6 C5 110.0(4) . . ? C6 C7 S8 116.1(3) . . ? C9 S8 C7 103.6(2) . . ? C9 S8 Ag 111.06(17) . . ? C7 S8 Ag 116.96(16) . . ? C10 C9 S8 117.4(3) . . ? C9 C10 C9 109.2(5) . 2_655 ? C4 C11 C12 116.3(4) . . ? C13 C12 C11 109.1(5) . . ? S14B C13 C12 126.1(11) 2_655 . ? S14B C13 S14A 35.2(9) 2_655 . ? C12 C13 S14A 110.5(4) . . ? C15 S14A C13 101.7(3) . . ? C15 S14A Ag 110.9(2) . 2_655 ? C13 S14A Ag 108.8(2) . 2_655 ? C13 S14B C15 109.7(13) 2_655 2_655 ? C13 S14B Ag 146.3(13) 2_655 . ? C15 S14B Ag 100.3(6) 2_655 . ? C16 C15 S14A 122.0(4) . . ? C16 C15 S14B 99.2(6) . 2_655 ? S14A C15 S14B 30.1(5) . 2_655 ? C17 C16 C15 119.5(5) . . ? C16 C17 S24 115.0(4) . 2_655 ? C22 C21 C4 116.2(4) . . ? C21 C22 C23 115.1(4) . . ? C22 C23 S24 115.7(3) . . ? C23 S24 C17 100.1(3) . 2_655 ? C23 S24 Ag 98.70(17) . 4 ? C17 S24 Ag 107.9(2) 2_655 4 ? S32 O31 Ag 129.8(3) . . ? O33 S32 O34 113.2(3) . . ? O33 S32 O31 116.5(3) . . ? O34 S32 O31 113.5(3) . . ? O33 S32 C35 104.4(3) . . ? O34 S32 C35 102.7(4) . . ? O31 S32 C35 104.6(3) . . ? F37 C35 F36 110.4(7) . . ? F37 C35 F38 106.8(6) . . ? F36 C35 F38 104.7(6) . . ? F37 C35 S32 112.9(5) . . ? F36 C35 S32 112.4(5) . . ? F38 C35 S32 109.2(6) . . ? N41 C42 C43 177.7(13) . . ? _diffrn_measured_fraction_theta_max 0.477 _diffrn_reflns_theta_full 26.96 _diffrn_measured_fraction_theta_full 0.477 _refine_diff_density_max 1.488 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.101 #----END ################## STRUCTURE 2 ###################################### data_ligand11 _database_code_depnum_ccdc_archive 'CCDC 633283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-S6-Hydroxy cage ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H36 O S6' _chemical_formula_sum 'C19 H36 O S6' _chemical_formula_weight 472.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 18.186(4) _cell_length_b 26.587(4) _cell_length_c 10.255(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.160(10) _cell_angle_gamma 90.00 _cell_volume 4864.6(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.40 _cell_measurement_theta_max 20.08 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 5.239 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.5877 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% .5 _diffrn_reflns_number 9737 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 5.23 _diffrn_reflns_theta_max 65.00 _reflns_number_total 8238 _reflns_number_gt 5657 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction HELENA _computing_structure_solution SHELXS _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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^)+(0.0754P)^2^+4.3216P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00048(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8238 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.006 _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 O1 O 0.14427(17) -0.01144(12) 0.4621(4) 0.0851(10) Uani 1 1 d . . . H1 H 0.1233 -0.0384 0.4422 0.128 Uiso 1 1 calc R . . C2 C 0.2225(2) -0.01949(15) 0.5040(5) 0.0695(12) Uani 1 1 d . . . H2A H 0.2416 -0.0357 0.4327 0.083 Uiso 1 1 calc R . . H2B H 0.2305 -0.0422 0.5796 0.083 Uiso 1 1 calc R . . C3 C 0.2671(2) 0.02930(14) 0.5432(4) 0.0591(10) Uani 1 1 d . . . C4 C 0.2547(2) 0.06687(15) 0.4263(4) 0.0607(10) Uani 1 1 d . . . H4A H 0.2861 0.0962 0.4507 0.073 Uiso 1 1 calc R . . H4B H 0.2029 0.0779 0.4091 0.073 Uiso 1 1 calc R . . S5 S 0.27622(7) 0.03934(4) 0.27605(12) 0.0744(3) Uani 1 1 d . . . C6 C 0.2541(3) 0.09147(18) 0.1616(5) 0.0752(13) Uani 1 1 d . . . H6A H 0.2504 0.0790 0.0717 0.090 Uiso 1 1 calc R . . H6B H 0.2054 0.1048 0.1690 0.090 Uiso 1 1 calc R . . C7 C 0.3112(2) 0.13408(17) 0.1847(5) 0.0713(12) Uani 1 1 d . . . H7A H 0.2923 0.1620 0.1271 0.086 Uiso 1 1 calc R . . H7B H 0.3168 0.1455 0.2759 0.086 Uiso 1 1 calc R . . C8 C 0.3875(3) 0.11903(19) 0.1587(5) 0.0773(13) Uani 1 1 d . . . H8A H 0.3863 0.1211 0.0638 0.093 Uiso 1 1 calc R . . H8B H 0.3967 0.0842 0.1850 0.093 Uiso 1 1 calc R . . S9 S 0.46486(7) 0.15678(5) 0.24397(14) 0.0812(4) Uani 1 1 d . . . C10 C 0.4758(3) 0.12906(16) 0.4087(5) 0.0672(11) Uani 1 1 d . . . H10A H 0.4267 0.1197 0.4245 0.081 Uiso 1 1 calc R . . H10B H 0.5052 0.0985 0.4108 0.081 Uiso 1 1 calc R . . C11 C 0.3504(2) 0.01680(16) 0.5807(5) 0.0656(11) Uani 1 1 d . . . H11A H 0.3783 0.0479 0.5999 0.079 Uiso 1 1 calc R . . H11B H 0.3660 0.0013 0.5048 0.079 Uiso 1 1 calc R . . S12 S 0.37483(7) -0.02468(5) 0.72198(15) 0.0874(4) Uani 1 1 d . . . C13 C 0.4731(3) -0.01015(17) 0.7658(5) 0.0775(13) Uani 1 1 d . . . H13A H 0.4981 -0.0372 0.8205 0.093 Uiso 1 1 calc R . . H13B H 0.4934 -0.0091 0.6851 0.093 Uiso 1 1 calc R . . C14 C 0.4916(3) 0.03923(17) 0.8400(5) 0.0766(13) Uani 1 1 d . . . H14A H 0.4885 0.0344 0.9325 0.092 Uiso 1 1 calc R . . H14B H 0.4545 0.0642 0.8030 0.092 Uiso 1 1 calc R . . C15 C 0.5694(3) 0.05900(19) 0.8324(5) 0.0847(15) Uani 1 1 d . . . H15A H 0.6059 0.0327 0.8609 0.102 Uiso 1 1 calc R . . H15B H 0.5813 0.0869 0.8937 0.102 Uiso 1 1 calc R . . S16 S 0.57825(7) 0.07970(5) 0.66831(14) 0.0809(4) Uani 1 1 d . . . C17 C 0.5192(2) 0.13537(16) 0.6552(5) 0.0683(12) Uani 1 1 d . . . H17A H 0.4692 0.1255 0.6652 0.082 Uiso 1 1 calc R . . H17B H 0.5390 0.1581 0.7275 0.082 Uiso 1 1 calc R . . C18 C 0.2371(2) 0.05292(16) 0.6604(5) 0.0683(11) Uani 1 1 d . . . H18A H 0.2333 0.0265 0.7239 0.082 Uiso 1 1 calc R . . H18B H 0.1867 0.0651 0.6266 0.082 Uiso 1 1 calc R . . S19 S 0.29096(7) 0.10424(4) 0.74908(13) 0.0755(3) Uani 1 1 d . . . C20 C 0.2430(2) 0.15945(16) 0.6712(6) 0.0763(13) Uani 1 1 d . . . H20A H 0.2392 0.1576 0.5757 0.092 Uiso 1 1 calc R . . H20B H 0.1926 0.1608 0.6895 0.092 Uiso 1 1 calc R . . C21 C 0.2861(3) 0.20691(17) 0.7249(6) 0.0804(14) Uani 1 1 d . . . H21A H 0.2594 0.2359 0.6821 0.097 Uiso 1 1 calc R . . H21B H 0.2861 0.2094 0.8193 0.097 Uiso 1 1 calc R . . C22 C 0.3661(3) 0.20926(17) 0.7052(5) 0.0741(13) Uani 1 1 d . . . H22A H 0.3945 0.1817 0.7525 0.089 Uiso 1 1 calc R . . H22B H 0.3888 0.2406 0.7412 0.089 Uiso 1 1 calc R . . S23 S 0.36913(7) 0.20525(5) 0.53017(13) 0.0788(4) Uani 1 1 d . . . C24 C 0.4675(3) 0.21229(16) 0.5286(5) 0.0746(13) Uani 1 1 d . . . H24A H 0.4722 0.2331 0.4531 0.090 Uiso 1 1 calc R . . H24B H 0.4903 0.2305 0.6081 0.090 Uiso 1 1 calc R . . C25 C 0.5137(2) 0.16370(15) 0.5218(5) 0.0675(12) Uani 1 1 d . . . C26 C 0.5917(3) 0.1793(2) 0.5032(6) 0.0932(17) Uani 1 1 d . . . H26A H 0.6142 0.2008 0.5752 0.140 Uiso 1 1 calc R . . H26B H 0.5879 0.1970 0.4206 0.140 Uiso 1 1 calc R . . H26C H 0.6222 0.1499 0.5021 0.140 Uiso 1 1 calc R . . O31A O 0.9938(4) 0.1243(3) 0.6340(6) 0.099(3) Uani 0.563(10) 1 d P . . H31 H 0.950(8) 0.118(5) 0.643(14) 0.148 Uiso 0.563(10) 1 d P . . C32 C 1.0022(3) 0.15567(19) 0.5395(5) 0.0768(13) Uani 1 1 d . . . H32A H 0.9885 0.1331 0.6038 0.115 Uiso 0.437(10) 1 calc PR . . H32B H 0.9781 0.1875 0.5446 0.115 Uiso 1 1 calc R . . H32C H 1.0556 0.1602 0.5574 0.115 Uiso 1 1 calc R . . C33 C 0.9771(2) 0.13343(14) 0.3989(4) 0.0546(9) Uani 1 1 d . . . C34 C 0.9984(2) 0.16907(14) 0.2944(4) 0.0567(10) Uani 1 1 d . . . H34A H 0.9775 0.2020 0.3051 0.068 Uiso 1 1 calc R . . H34B H 0.9758 0.1568 0.2067 0.068 Uiso 1 1 calc R . . S35 S 1.09828(6) 0.17546(4) 0.30365(13) 0.0709(3) Uani 1 1 d . . . C36 C 1.0972(3) 0.22353(17) 0.1771(6) 0.0798(14) Uani 1 1 d . . . H36A H 1.0480 0.2391 0.1594 0.096 Uiso 1 1 calc R . . H36B H 1.1333 0.2493 0.2125 0.096 Uiso 1 1 calc R . . C37 C 1.1145(3) 0.20538(18) 0.0473(6) 0.0809(14) Uani 1 1 d . . . H37A H 1.1651 0.1920 0.0640 0.097 Uiso 1 1 calc R . . H37B H 1.1136 0.2341 -0.0114 0.097 Uiso 1 1 calc R . . C38 C 1.0617(2) 0.16526(17) -0.0246(6) 0.0783(13) Uani 1 1 d . . . H38A H 1.0587 0.1375 0.0356 0.094 Uiso 1 1 calc R . . H38B H 1.0816 0.1524 -0.0992 0.094 Uiso 1 1 calc R . . S39 S 0.96770(7) 0.19063(4) -0.08482(15) 0.0806(4) Uani 1 1 d . . . C40 C 0.9159(2) 0.13202(16) -0.0943(5) 0.0642(11) Uani 1 1 d . . . H40A H 0.9319 0.1105 -0.1600 0.077 Uiso 1 1 calc R . . H40B H 0.9285 0.1151 -0.0090 0.077 Uiso 1 1 calc R . . C41 C 0.8915(2) 0.12617(14) 0.3668(4) 0.0585(10) Uani 1 1 d . . . H41A H 0.8771 0.1037 0.4321 0.070 Uiso 1 1 calc R . . H41B H 0.8774 0.1104 0.2803 0.070 Uiso 1 1 calc R . . S42 S 0.84071(6) 0.18516(4) 0.36649(13) 0.0734(3) Uani 1 1 d . . . C43 C 0.7474(3) 0.1654(2) 0.3474(8) 0.109(2) Uani 1 1 d . . . H43A H 0.7457 0.1363 0.4039 0.131 Uiso 1 1 calc R . . H43B H 0.7188 0.1920 0.3790 0.131 Uiso 1 1 calc R . . C44 C 0.7125(4) 0.1529(2) 0.2192(7) 0.111(2) Uani 1 1 d . . . H44A H 0.6650 0.1369 0.2226 0.133 Uiso 1 1 calc R . . H44B H 0.7434 0.1285 0.1843 0.133 Uiso 1 1 calc R . . C45 C 0.6974(3) 0.1992(2) 0.1190(7) 0.107(2) Uani 1 1 d . . . H45A H 0.7339 0.2254 0.1483 0.128 Uiso 1 1 calc R . . H45B H 0.6480 0.2128 0.1191 0.128 Uiso 1 1 calc R . . S46 S 0.70359(7) 0.17966(6) -0.05020(14) 0.0851(4) Uani 1 1 d . . . C47 C 0.8051(2) 0.17216(16) -0.0274(5) 0.0676(11) Uani 1 1 d . . . H47A H 0.8277 0.2051 -0.0305 0.081 Uiso 1 1 calc R . . H47B H 0.8236 0.1582 0.0602 0.081 Uiso 1 1 calc R . . C48 C 1.0151(2) 0.08174(15) 0.3986(4) 0.0616(11) Uani 1 1 d . . . H48A H 0.9942 0.0597 0.4576 0.074 Uiso 1 1 calc R . . H48B H 1.0679 0.0859 0.4363 0.074 Uiso 1 1 calc R . . S49 S 1.00753(6) 0.05011(4) 0.24025(11) 0.0634(3) Uani 1 1 d . . . C50 C 0.9336(3) 0.00495(15) 0.2494(4) 0.0683(12) Uani 1 1 d . . . H50A H 0.9512 -0.0189 0.3203 0.082 Uiso 1 1 calc R . . H50B H 0.8907 0.0225 0.2708 0.082 Uiso 1 1 calc R . . C51 C 0.9096(3) -0.02346(14) 0.1194(5) 0.0683(12) Uani 1 1 d . . . H51A H 0.9512 -0.0441 0.1046 0.082 Uiso 1 1 calc R . . H51B H 0.8687 -0.0458 0.1281 0.082 Uiso 1 1 calc R . . C52 C 0.8847(2) 0.00972(15) -0.0019(4) 0.0639(11) Uani 1 1 d . . . H52A H 0.8699 -0.0113 -0.0798 0.077 Uiso 1 1 calc R . . H52B H 0.9265 0.0304 -0.0157 0.077 Uiso 1 1 calc R . . S53 S 0.80741(6) 0.04974(4) 0.01668(12) 0.0658(3) Uani 1 1 d . . . C54 C 0.7941(2) 0.08574(16) -0.1362(4) 0.0658(11) Uani 1 1 d . . . H54A H 0.8133 0.0660 -0.2017 0.079 Uiso 1 1 calc R . . H54B H 0.7406 0.0897 -0.1682 0.079 Uiso 1 1 calc R . . C55 C 0.8305(2) 0.13841(16) -0.1307(4) 0.0619(11) Uani 1 1 d . . . O31B O 0.8358(5) 0.1401(3) -0.3543(8) 0.086(3) Uani 0.437(10) 1 d P . . H31B H 0.847(9) 0.109(6) -0.362(15) 0.129 Uiso 0.437(10) 1 d P . . C56 C 0.8074(3) 0.1624(2) -0.2690(5) 0.0845(15) Uani 1 1 d . . . H56A H 0.8233 0.1413 -0.3342 0.127 Uiso 0.563(10) 1 calc PR . . H56B H 0.8306 0.1949 -0.2692 0.127 Uiso 1 1 calc R . . H56C H 0.7539 0.1661 -0.2900 0.127 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 O1 0.0639(19) 0.072(2) 0.112(3) -0.0003(18) -0.0029(18) -0.0215(16) C2 0.066(3) 0.050(2) 0.087(3) 0.000(2) 0.002(2) -0.010(2) C3 0.056(2) 0.046(2) 0.073(3) -0.0008(19) 0.006(2) -0.0068(17) C4 0.056(2) 0.050(2) 0.074(3) -0.007(2) 0.006(2) -0.0005(18) S5 0.0912(8) 0.0551(6) 0.0735(7) -0.0060(5) 0.0075(6) 0.0035(6) C6 0.062(3) 0.079(3) 0.076(3) 0.003(2) -0.007(2) 0.001(2) C7 0.059(3) 0.068(3) 0.082(3) 0.007(2) 0.000(2) 0.013(2) C8 0.065(3) 0.086(3) 0.076(3) 0.005(3) 0.003(2) 0.011(2) S9 0.0699(7) 0.0834(8) 0.0885(9) 0.0171(7) 0.0104(6) -0.0008(6) C10 0.064(3) 0.056(2) 0.079(3) 0.004(2) 0.007(2) 0.002(2) C11 0.058(2) 0.058(2) 0.077(3) 0.005(2) 0.004(2) 0.0006(19) S12 0.0766(8) 0.0679(7) 0.1113(11) 0.0289(7) 0.0025(7) 0.0001(6) C13 0.075(3) 0.062(3) 0.089(3) 0.006(2) -0.003(3) 0.015(2) C14 0.084(3) 0.066(3) 0.074(3) 0.009(2) -0.001(2) 0.013(2) C15 0.071(3) 0.078(3) 0.090(4) 0.003(3) -0.022(3) 0.010(3) S16 0.0592(7) 0.0766(8) 0.1013(10) 0.0070(7) 0.0015(6) 0.0174(6) C17 0.060(3) 0.059(2) 0.082(3) -0.002(2) 0.002(2) 0.004(2) C18 0.061(3) 0.059(2) 0.084(3) 0.001(2) 0.009(2) -0.006(2) S19 0.0740(7) 0.0644(7) 0.0802(8) -0.0099(6) -0.0046(6) 0.0040(5) C20 0.055(2) 0.065(3) 0.104(4) -0.010(3) 0.003(2) 0.011(2) C21 0.073(3) 0.058(3) 0.109(4) -0.020(3) 0.012(3) 0.008(2) C22 0.066(3) 0.060(3) 0.091(3) -0.017(2) 0.003(2) 0.000(2) S23 0.0646(7) 0.0773(8) 0.0890(9) -0.0011(6) 0.0009(6) 0.0155(6) C24 0.075(3) 0.052(2) 0.094(4) 0.004(2) 0.008(3) -0.003(2) C25 0.051(2) 0.055(2) 0.092(3) 0.000(2) 0.004(2) -0.0064(19) C26 0.059(3) 0.089(4) 0.130(5) 0.005(3) 0.014(3) -0.013(3) O31A 0.116(6) 0.123(6) 0.052(4) 0.007(4) 0.007(4) 0.015(5) C32 0.075(3) 0.082(3) 0.066(3) -0.014(3) -0.006(2) 0.006(2) C33 0.054(2) 0.050(2) 0.055(2) -0.0041(17) -0.0014(18) 0.0005(17) C34 0.050(2) 0.049(2) 0.067(3) 0.0012(18) 0.0020(19) -0.0018(17) S35 0.0472(5) 0.0725(7) 0.0878(8) 0.0014(6) 0.0000(5) -0.0035(5) C36 0.062(3) 0.062(3) 0.113(4) 0.004(3) 0.012(3) -0.015(2) C37 0.054(3) 0.073(3) 0.112(4) 0.018(3) 0.007(3) -0.004(2) C38 0.062(3) 0.065(3) 0.108(4) -0.003(3) 0.016(3) -0.006(2) S39 0.0599(7) 0.0629(7) 0.1111(10) 0.0220(6) -0.0033(6) -0.0089(5) C40 0.058(2) 0.061(2) 0.070(3) 0.009(2) 0.001(2) -0.0077(19) C41 0.056(2) 0.051(2) 0.067(3) 0.0060(19) 0.009(2) -0.0005(18) S42 0.0601(6) 0.0651(7) 0.0957(9) 0.0123(6) 0.0166(6) 0.0114(5) C43 0.067(3) 0.104(4) 0.156(7) 0.042(4) 0.017(4) 0.007(3) C44 0.119(5) 0.106(5) 0.117(5) -0.010(4) 0.045(4) -0.040(4) C45 0.065(3) 0.086(4) 0.158(6) -0.029(4) -0.011(3) 0.029(3) S46 0.0630(7) 0.0997(9) 0.0853(9) -0.0010(7) -0.0039(6) 0.0081(6) C47 0.059(2) 0.063(3) 0.075(3) 0.002(2) -0.002(2) -0.004(2) C48 0.060(2) 0.056(2) 0.062(3) 0.0003(19) -0.006(2) 0.0056(19) S49 0.0646(6) 0.0555(6) 0.0690(7) -0.0034(5) 0.0096(5) 0.0002(5) C50 0.083(3) 0.052(2) 0.070(3) 0.008(2) 0.014(2) -0.006(2) C51 0.077(3) 0.040(2) 0.088(3) -0.005(2) 0.015(2) -0.004(2) C52 0.069(3) 0.054(2) 0.069(3) -0.011(2) 0.014(2) -0.006(2) S53 0.0642(6) 0.0577(6) 0.0761(7) -0.0024(5) 0.0148(5) -0.0036(5) C54 0.057(2) 0.065(3) 0.068(3) -0.002(2) -0.007(2) -0.008(2) C55 0.053(2) 0.066(3) 0.061(3) 0.005(2) -0.0036(19) -0.0040(19) O31B 0.102(6) 0.099(6) 0.058(5) 0.001(5) 0.014(4) 0.011(5) C56 0.076(3) 0.105(4) 0.066(3) 0.021(3) -0.001(3) 0.005(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 O1 C2 1.420(5) . ? C2 C3 1.542(5) . ? C3 C11 1.526(6) . ? C3 C4 1.543(6) . ? C3 C18 1.546(6) . ? C4 S5 1.816(4) . ? S5 C6 1.810(5) . ? C6 C7 1.524(6) . ? C7 C8 1.516(6) . ? C8 S9 1.810(5) . ? S9 C10 1.818(5) . ? C10 C25 1.536(6) . ? C11 S12 1.806(4) . ? S12 C13 1.798(5) . ? C13 C14 1.522(6) . ? C14 C15 1.526(7) . ? C15 S16 1.806(5) . ? S16 C17 1.819(4) . ? C17 C25 1.548(6) . ? C18 S19 1.818(4) . ? S19 C20 1.812(5) . ? C20 C21 1.531(6) . ? C21 C22 1.508(6) . ? C22 S23 1.810(5) . ? S23 C24 1.802(5) . ? C24 C25 1.550(6) . ? C25 C26 1.526(6) . ? C32 C33 1.543(6) . ? C33 C34 1.535(6) . ? C33 C41 1.539(5) . ? C33 C48 1.539(5) . ? C34 S35 1.808(4) . ? S35 C36 1.819(5) . ? C36 C37 1.505(7) . ? C37 C38 1.527(6) . ? C38 S39 1.830(5) . ? S39 C40 1.813(4) . ? C40 C55 1.536(6) . ? C41 S42 1.820(4) . ? S42 C43 1.750(6) . ? C43 C44 1.385(8) . ? C44 C45 1.591(9) . ? C45 S46 1.835(7) . ? S46 C47 1.826(4) . ? C47 C55 1.527(6) . ? C48 S49 1.810(4) . ? S49 C50 1.818(4) . ? C50 C51 1.521(6) . ? C51 C52 1.521(6) . ? C52 S53 1.803(4) . ? S53 C54 1.812(4) . ? C54 C55 1.545(6) . ? C55 C56 1.538(6) . ? 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 O1 C2 C3 113.5(3) . . ? C11 C3 C2 109.3(3) . . ? C11 C3 C4 109.0(3) . . ? C2 C3 C4 110.6(3) . . ? C11 C3 C18 112.1(4) . . ? C2 C3 C18 107.3(4) . . ? C4 C3 C18 108.7(3) . . ? C3 C4 S5 112.0(3) . . ? C6 S5 C4 100.6(2) . . ? C7 C6 S5 114.2(3) . . ? C8 C7 C6 113.3(4) . . ? C7 C8 S9 114.9(4) . . ? C8 S9 C10 99.2(2) . . ? C25 C10 S9 114.3(3) . . ? C3 C11 S12 114.4(3) . . ? C13 S12 C11 98.5(2) . . ? C14 C13 S12 115.0(3) . . ? C13 C14 C15 112.9(4) . . ? C14 C15 S16 113.8(3) . . ? C15 S16 C17 99.1(2) . . ? C25 C17 S16 113.4(3) . . ? C3 C18 S19 117.1(3) . . ? C20 S19 C18 102.7(2) . . ? C21 C20 S19 109.9(3) . . ? C22 C21 C20 115.2(4) . . ? C21 C22 S23 110.2(3) . . ? C24 S23 C22 102.9(2) . . ? C25 C24 S23 117.5(3) . . ? C26 C25 C10 111.1(4) . . ? C26 C25 C17 109.9(4) . . ? C10 C25 C17 108.6(3) . . ? C26 C25 C24 107.7(4) . . ? C10 C25 C24 111.5(4) . . ? C17 C25 C24 108.0(4) . . ? C34 C33 C41 108.1(3) . . ? C34 C33 C48 112.1(3) . . ? C41 C33 C48 108.9(3) . . ? C34 C33 C32 110.3(3) . . ? C41 C33 C32 110.6(4) . . ? C48 C33 C32 107.0(3) . . ? C33 C34 S35 114.1(3) . . ? C34 S35 C36 99.0(2) . . ? C37 C36 S35 115.5(3) . . ? C36 C37 C38 115.5(4) . . ? C37 C38 S39 111.4(3) . . ? C40 S39 C38 98.2(2) . . ? C55 C40 S39 114.1(3) . . ? C33 C41 S42 112.6(3) . . ? C43 S42 C41 102.8(3) . . ? C44 C43 S42 115.7(5) . . ? C43 C44 C45 114.8(5) . . ? C44 C45 S46 111.0(4) . . ? C47 S46 C45 98.9(2) . . ? C55 C47 S46 114.1(3) . . ? C33 C48 S49 117.4(3) . . ? C48 S49 C50 100.9(2) . . ? C51 C50 S49 111.8(3) . . ? C52 C51 C50 114.8(3) . . ? C51 C52 S53 111.8(3) . . ? C52 S53 C54 101.3(2) . . ? C55 C54 S53 117.6(3) . . ? C47 C55 C40 108.9(3) . . ? C47 C55 C56 109.3(4) . . ? C40 C55 C56 110.7(4) . . ? C47 C55 C54 111.9(4) . . ? C40 C55 C54 108.3(3) . . ? C56 C55 C54 107.7(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.754 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.057 ######################## STRUCTURE 3 ################################## data_ag14 _database_code_depnum_ccdc_archive 'CCDC 633284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(S6-Cage-C4-OH-CH3)(tosylato)silver(I)] polymer ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H49 Ag O4 S7' _chemical_formula_sum 'C29 H49 Ag O4 S7' _chemical_formula_weight 793.97 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' O O 0.0106 0.0060 '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 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 10.707(4) _cell_length_b 17.737(4) _cell_length_c 19.081(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.61(2) _cell_angle_gamma 90.00 _cell_volume 3522(2) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 11.50 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details DIFABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 CAD4 _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% .5 _diffrn_reflns_number 6398 _diffrn_reflns_av_R_equivalents 0.1338 _diffrn_reflns_av_sigmaI/netI 0.4892 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5419 _reflns_number_gt 1717 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'PLATON,HELENA (Spek, 1995)' _computing_structure_solution SHELXS86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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^)+(0.0000P)^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 5419 _refine_ls_number_parameters 361 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.3303 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.000 _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 0.34702(13) 0.14419(6) 0.07720(6) 0.0407(4) Uani 1 1 d . . . O1 O 0.4067(11) 0.1309(5) -0.1948(5) 0.071(4) Uani 1 1 d . . . H1 H 0.4404 0.1389 -0.1516 0.107 Uiso 1 1 calc R . . C2 C 0.2885(15) 0.0920(7) -0.2007(7) 0.050(5) Uani 1 1 d . . . H2A H 0.2495 0.0826 -0.2518 0.060 Uiso 1 1 calc R . . H2B H 0.2297 0.1242 -0.1818 0.060 Uiso 1 1 calc R . . C3 C 0.3040(14) 0.0184(7) -0.1609(7) 0.025(4) Uani 1 1 d . . . C11 C 0.3563(13) 0.0292(7) -0.0798(6) 0.040(4) Uani 1 1 d . . . H11A H 0.4276 0.0652 -0.0724 0.047 Uiso 1 1 calc R . . H11B H 0.3914 -0.0190 -0.0590 0.047 Uiso 1 1 calc R . . S12 S 0.2427(4) 0.0620(2) -0.03128(18) 0.0398(11) Uani 1 1 d . . . C13 C 0.1944(15) -0.0257(8) 0.0034(7) 0.086(7) Uani 1 1 d . . . H13A H 0.1031 -0.0337 -0.0187 0.103 Uiso 1 1 calc R . . H13B H 0.2420 -0.0668 -0.0128 0.103 Uiso 1 1 calc R . . C14 C 0.2127(15) -0.0318(7) 0.0806(7) 0.060(6) Uani 1 1 d . . . H14A H 0.1810 0.0146 0.0984 0.072 Uiso 1 1 calc R . . H14B H 0.3052 -0.0349 0.1023 0.072 Uiso 1 1 calc R . . C15 C 0.1474(15) -0.0984(7) 0.1070(7) 0.052(5) Uani 1 1 d . . . H15A H 0.1553 -0.0931 0.1590 0.063 Uiso 1 1 calc R . . H15B H 0.0557 -0.0975 0.0834 0.063 Uiso 1 1 calc R . . C16 C 0.2023(13) -0.1737(7) 0.0929(7) 0.048(5) Uani 1 1 d . . . H16A H 0.2905 -0.1773 0.1221 0.058 Uiso 1 1 calc R . . H16B H 0.2060 -0.1758 0.0421 0.058 Uiso 1 1 calc R . . S17 S 0.1136(5) -0.2536(2) 0.1120(2) 0.0535(14) Uani 1 1 d . . . C18 C -0.0226(12) -0.2556(8) 0.0352(6) 0.048(4) Uani 1 1 d . . . H18A H -0.0984 -0.2691 0.0530 0.057 Uiso 1 1 calc R . . H18B H -0.0362 -0.2040 0.0165 0.057 Uiso 1 1 calc R . . C21 C 0.1746(12) -0.0236(7) -0.1795(6) 0.035(4) Uani 1 1 d . . . H21A H 0.1111 0.0063 -0.1620 0.042 Uiso 1 1 calc R . . H21B H 0.1846 -0.0717 -0.1536 0.042 Uiso 1 1 calc R . . S22 S 0.1121(4) -0.0422(3) -0.27530(19) 0.0590(14) Uani 1 1 d . . . C23 C -0.0181(16) -0.1126(12) -0.2693(9) 0.103(9) Uani 1 1 d . . . H23A H -0.0498 -0.1356 -0.3169 0.123 Uiso 1 1 calc R . . H23B H 0.0203 -0.1528 -0.2359 0.123 Uiso 1 1 calc R . . C24 C -0.1211(19) -0.0836(11) -0.2469(9) 0.101(8) Uani 1 1 d . . . H24A H -0.1508 -0.0381 -0.2751 0.121 Uiso 1 1 calc R . . H24B H -0.0921 -0.0684 -0.1963 0.121 Uiso 1 1 calc R . . C25 C -0.2352(17) -0.1378(9) -0.2539(7) 0.099(7) Uani 1 1 d . . . H25A H -0.3019 -0.1118 -0.2356 0.119 Uiso 1 1 calc R . . H25B H -0.2706 -0.1472 -0.3054 0.119 Uiso 1 1 calc R . . C26 C -0.2108(14) -0.2124(7) -0.2168(6) 0.045(5) Uani 1 1 d . . . H26A H -0.1452 -0.2400 -0.2344 0.054 Uiso 1 1 calc R . . H26B H -0.2899 -0.2424 -0.2271 0.054 Uiso 1 1 calc R . . S27 S -0.1569(4) -0.19718(19) -0.12076(19) 0.0411(12) Uani 1 1 d . . . C28 C -0.1414(12) -0.2983(6) -0.0857(7) 0.035(4) Uani 1 1 d . . . H28A H -0.2156 -0.3109 -0.0661 0.042 Uiso 1 1 calc R . . H28B H -0.1402 -0.3331 -0.1255 0.042 Uiso 1 1 calc R . . C31 C 0.4047(13) -0.0290(7) -0.1911(6) 0.038(4) Uani 1 1 d . . . H31A H 0.4869 -0.0021 -0.1813 0.045 Uiso 1 1 calc R . . H31B H 0.3743 -0.0340 -0.2435 0.045 Uiso 1 1 calc R . . S32 S 0.4286(4) -0.12200(19) -0.15066(18) 0.0440(12) Uani 1 1 d . . . C33 C 0.4046(14) -0.1838(6) -0.2287(6) 0.051(5) Uani 1 1 d . . . H33A H 0.3232 -0.1712 -0.2625 0.062 Uiso 1 1 calc R . . H33B H 0.4741 -0.1761 -0.2535 0.062 Uiso 1 1 calc R . . C34 C 0.4025(18) -0.2670(8) -0.2056(8) 0.080(6) Uiso 1 1 d D . . H34A H 0.4047 -0.3008 -0.2460 0.096 Uiso 1 1 calc R . . H34B H 0.4759 -0.2784 -0.1655 0.096 Uiso 1 1 calc R . . C35 C 0.280(2) -0.2748(12) -0.1831(12) 0.157(11) Uiso 1 1 d D . . H35A H 0.2734 -0.2309 -0.1529 0.188 Uiso 1 1 calc R . . H35B H 0.2108 -0.2697 -0.2269 0.188 Uiso 1 1 calc R . . C36 C 0.251(3) -0.3369(15) -0.1471(13) 0.262(16) Uani 1 1 d D . . H36A H 0.3122 -0.3367 -0.1000 0.314 Uiso 1 1 calc R . . H36B H 0.2724 -0.3808 -0.1732 0.314 Uiso 1 1 calc R . . S37 S 0.1054(5) -0.3554(3) -0.1306(2) 0.0981(18) Uani 1 1 d . . . C38 C 0.1019(13) -0.2940(7) -0.0564(7) 0.041(4) Uani 1 1 d . . . H38A H 0.1782 -0.3029 -0.0175 0.049 Uiso 1 1 calc R . . H38B H 0.1041 -0.2415 -0.0720 0.049 Uiso 1 1 calc R . . C4 C -0.0199(15) -0.3069(8) -0.0280(7) 0.034(4) Uani 1 1 d . . . C5 C -0.0227(13) -0.3906(7) -0.0003(6) 0.055(5) Uani 1 1 d . . . H5A H 0.0541 -0.4002 0.0372 0.082 Uiso 1 1 calc R . . H5B H -0.0260 -0.4252 -0.0400 0.082 Uiso 1 1 calc R . . H5C H -0.0980 -0.3977 0.0190 0.082 Uiso 1 1 calc R . . O40 O 0.4001(9) 0.2637(4) 0.0281(4) 0.051(3) Uani 1 1 d . . . O41 O 0.5197(11) 0.2007(6) -0.0484(6) 0.077(4) Uani 1 1 d . . . O42 O 0.3049(11) 0.2396(6) -0.0966(5) 0.081(4) Uani 1 1 d . . . S43 S 0.4210(5) 0.2558(2) -0.0445(2) 0.0474(14) Uani 1 1 d . . . C51 C 0.4745(15) 0.3431(7) -0.0657(6) 0.038(4) Uani 1 1 d . . . C52 C 0.4006(16) 0.4046(9) -0.0656(7) 0.058(5) Uani 1 1 d . . . H52 H 0.3222 0.3989 -0.0520 0.070 Uiso 1 1 calc R . . C53 C 0.4341(15) 0.4752(8) -0.0843(7) 0.042(4) Uani 1 1 d . . . H53 H 0.3773 0.5157 -0.0849 0.050 Uiso 1 1 calc R . . C54 C 0.5533(16) 0.4878(8) -0.1028(7) 0.036(4) Uani 1 1 d . . . C55 C 0.6239(16) 0.4256(9) -0.1027(7) 0.058(6) Uani 1 1 d . . . H55 H 0.7020 0.4314 -0.1164 0.069 Uiso 1 1 calc R . . C56 C 0.5936(13) 0.3544(9) -0.0845(6) 0.048(4) Uani 1 1 d . . . H56 H 0.6505 0.3140 -0.0844 0.057 Uiso 1 1 calc R . . C57 C 0.5916(14) 0.5635(7) -0.1259(6) 0.055(5) Uani 1 1 d . . . H57A H 0.6783 0.5752 -0.0994 0.082 Uiso 1 1 calc R . . H57B H 0.5330 0.6016 -0.1161 0.082 Uiso 1 1 calc R . . H57C H 0.5881 0.5626 -0.1771 0.082 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 0.0427(9) 0.0390(7) 0.0399(7) 0.0027(7) 0.0090(6) 0.0031(9) O1 0.119(12) 0.050(8) 0.056(7) 0.006(6) 0.042(8) 0.002(8) C2 0.082(17) 0.036(10) 0.037(9) 0.003(8) 0.024(11) 0.011(10) C3 0.029(11) 0.018(8) 0.027(8) 0.006(7) 0.005(8) 0.004(8) C11 0.039(12) 0.026(8) 0.051(10) 0.010(7) 0.006(9) 0.020(9) S12 0.038(3) 0.048(2) 0.036(2) -0.001(2) 0.014(2) -0.007(2) C13 0.073(16) 0.099(14) 0.086(14) 0.034(12) 0.018(12) -0.061(13) C14 0.090(17) 0.032(10) 0.065(12) 0.019(9) 0.031(12) -0.008(10) C15 0.080(16) 0.040(10) 0.045(10) 0.009(8) 0.032(10) 0.007(11) C16 0.013(11) 0.056(11) 0.070(12) 0.016(8) -0.003(9) -0.009(9) S17 0.055(4) 0.051(3) 0.053(3) 0.017(2) 0.009(3) 0.002(3) C18 0.020(11) 0.077(12) 0.039(9) 0.010(9) -0.006(9) 0.009(10) C21 0.019(11) 0.047(9) 0.036(9) -0.018(7) 0.004(8) 0.006(8) S22 0.049(4) 0.091(4) 0.035(2) -0.012(2) 0.005(2) -0.006(3) C23 0.016(14) 0.20(2) 0.081(15) -0.060(14) -0.010(12) -0.024(15) C24 0.10(2) 0.12(2) 0.067(14) 0.022(13) -0.009(15) -0.077(17) C25 0.16(2) 0.072(13) 0.032(9) 0.020(10) -0.034(11) -0.051(16) C26 0.040(12) 0.042(10) 0.049(10) -0.005(8) 0.004(9) -0.032(9) S27 0.041(3) 0.041(2) 0.041(2) -0.0040(19) 0.008(2) 0.001(2) C28 0.009(10) 0.020(8) 0.077(12) 0.006(8) 0.010(9) 0.005(8) C31 0.030(11) 0.046(9) 0.029(8) 0.006(7) -0.007(8) 0.021(9) S32 0.041(3) 0.042(3) 0.046(2) -0.0043(19) 0.003(2) 0.003(2) C33 0.047(13) 0.053(10) 0.052(10) -0.010(8) 0.007(9) -0.018(9) C36 0.33(5) 0.28(4) 0.24(3) -0.08(3) 0.20(3) -0.04(4) S37 0.074(5) 0.135(5) 0.096(4) -0.035(4) 0.042(3) 0.022(5) C38 0.023(11) 0.024(8) 0.069(11) -0.006(8) -0.002(9) 0.006(8) C4 0.032(13) 0.040(10) 0.030(9) 0.020(8) 0.004(9) -0.002(9) C5 0.022(12) 0.086(13) 0.054(10) 0.008(9) 0.003(9) -0.003(10) O40 0.065(9) 0.043(6) 0.049(6) 0.001(5) 0.022(6) -0.018(6) O41 0.092(11) 0.055(7) 0.112(10) 0.003(7) 0.079(9) -0.009(8) O42 0.094(11) 0.082(9) 0.057(7) -0.002(6) -0.005(7) -0.064(8) S43 0.063(4) 0.034(3) 0.050(3) -0.004(2) 0.024(3) -0.014(3) C51 0.064(14) 0.007(9) 0.039(9) -0.006(7) 0.007(9) 0.016(9) C52 0.058(15) 0.056(12) 0.066(11) 0.005(10) 0.027(11) -0.041(11) C53 0.037(13) 0.036(10) 0.051(10) -0.001(8) 0.009(10) 0.011(9) C54 0.032(13) 0.033(10) 0.040(10) -0.010(8) 0.000(9) -0.008(10) C55 0.054(16) 0.055(12) 0.072(13) 0.028(10) 0.030(12) -0.008(11) C56 0.031(12) 0.065(11) 0.060(10) 0.020(10) 0.037(9) 0.016(11) C57 0.075(15) 0.033(9) 0.062(11) -0.004(8) 0.030(10) -0.008(10) _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 O40 2.438(8) . ? Ag1 S32 2.511(4) 3_655 ? Ag1 S27 2.552(4) 3 ? Ag1 S12 2.563(4) . ? O1 C2 1.421(15) . ? C2 C3 1.501(15) . ? C3 C11 1.528(14) . ? C3 C21 1.539(16) . ? C3 C31 1.579(15) . ? C11 S12 1.790(13) . ? S12 C13 1.812(13) . ? C13 C14 1.445(15) . ? C14 C15 1.519(16) . ? C15 C16 1.508(15) . ? C16 S17 1.791(12) . ? S17 C18 1.808(12) . ? C18 C4 1.517(16) . ? C21 S22 1.823(10) . ? S22 C23 1.896(19) . ? C23 C24 1.37(2) . ? C24 C25 1.535(19) . ? C25 C26 1.495(16) . ? C26 S27 1.807(11) . ? S27 C28 1.908(11) . ? S27 Ag1 2.552(4) 3 ? C28 C4 1.502(16) . ? C31 S32 1.814(12) . ? S32 C33 1.818(11) . ? S32 Ag1 2.511(4) 3_655 ? C33 C34 1.543(16) . ? C34 C35 1.481(14) . ? C35 C36 1.372(14) . ? C36 S37 1.69(2) . ? S37 C38 1.793(12) . ? C38 C4 1.543(17) . ? C4 C5 1.577(15) . ? O40 S43 1.460(8) . ? O41 S43 1.455(10) . ? O42 S43 1.427(10) . ? S43 C51 1.731(13) . ? C51 C52 1.348(18) . ? C51 C56 1.418(17) . ? C52 C53 1.373(16) . ? C53 C54 1.420(19) . ? C54 C55 1.336(17) . ? C54 C57 1.500(15) . ? C55 C56 1.369(17) . ? 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 O40 Ag1 S32 94.1(2) . 3_655 ? O40 Ag1 S27 94.6(2) . 3 ? S32 Ag1 S27 127.41(12) 3_655 3 ? O40 Ag1 S12 106.3(2) . . ? S32 Ag1 S12 122.64(13) 3_655 . ? S27 Ag1 S12 104.07(13) 3 . ? O1 C2 C3 113.1(13) . . ? C2 C3 C11 111.9(10) . . ? C2 C3 C21 108.5(12) . . ? C11 C3 C21 113.0(11) . . ? C2 C3 C31 106.3(11) . . ? C11 C3 C31 108.5(11) . . ? C21 C3 C31 108.3(10) . . ? C3 C11 S12 115.6(10) . . ? C11 S12 C13 101.4(7) . . ? C11 S12 Ag1 112.5(5) . . ? C13 S12 Ag1 107.5(5) . . ? C14 C13 S12 117.1(11) . . ? C13 C14 C15 115.7(12) . . ? C16 C15 C14 113.6(12) . . ? C15 C16 S17 114.6(10) . . ? C16 S17 C18 102.4(6) . . ? C4 C18 S17 119.5(10) . . ? C3 C21 S22 114.7(9) . . ? C21 S22 C23 99.2(7) . . ? C24 C23 S22 115.3(16) . . ? C23 C24 C25 114.8(18) . . ? C26 C25 C24 117.8(15) . . ? C25 C26 S27 109.1(9) . . ? C26 S27 C28 101.3(6) . . ? C26 S27 Ag1 107.2(5) . 3 ? C28 S27 Ag1 104.0(4) . 3 ? C4 C28 S27 110.0(9) . . ? C3 C31 S32 111.6(9) . . ? C31 S32 C33 102.7(5) . . ? C31 S32 Ag1 113.6(5) . 3_655 ? C33 S32 Ag1 107.2(5) . 3_655 ? C34 C33 S32 110.6(9) . . ? C35 C34 C33 104.2(15) . . ? C36 C35 C34 123(2) . . ? C35 C36 S37 125(2) . . ? C36 S37 C38 102.8(10) . . ? C4 C38 S37 111.4(10) . . ? C28 C4 C18 110.3(12) . . ? C28 C4 C38 112.6(11) . . ? C18 C4 C38 111.5(12) . . ? C28 C4 C5 105.0(12) . . ? C18 C4 C5 107.0(10) . . ? C38 C4 C5 110.0(12) . . ? S43 O40 Ag1 112.5(4) . . ? O42 S43 O41 110.6(7) . . ? O42 S43 O40 112.2(6) . . ? O41 S43 O40 112.9(6) . . ? O42 S43 C51 107.4(7) . . ? O41 S43 C51 107.7(7) . . ? O40 S43 C51 105.6(6) . . ? C52 C51 C56 116.7(14) . . ? C52 C51 S43 119.8(13) . . ? C56 C51 S43 123.6(12) . . ? C51 C52 C53 123.3(16) . . ? C52 C53 C54 120.9(15) . . ? C55 C54 C53 114.3(14) . . ? C55 C54 C57 123.1(16) . . ? C53 C54 C57 122.5(14) . . ? C54 C55 C56 126.5(17) . . ? C55 C56 C51 118.4(15) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.534 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.125