Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Daniel Reger' 'James R. Gardinier' 'Radu F. Semeniuc' 'Mark D. Smith' _publ_contact_author_name 'Dr Daniel Reger' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia South Carolina 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email REGER@MAIL.CHEM.SC.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Silver Complexes of 1,1',3,3'-tetrakis(pyrazol-1-yl)propane:  the 'Quadruple Pyrazolyl Embrace' as a Supramolecular Tecton ; data_jg143iis _database_code_CSD 204327 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H41 Ag3 N22 O9' _chemical_formula_weight 1249.52 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 21.7230(15) _cell_length_b 14.9693(10) _cell_length_c 14.8892(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.9640(10) _cell_angle_gamma 90.00 _cell_volume 4823.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 6032 _cell_measurement_theta_min 2.232 _cell_measurement_theta_max 25.022 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3502 _exptl_absorpt_correction_T_max 0.5816 _exptl_absorpt_process_details '(SADABS, Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 16502 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4259 _reflns_number_gt 3561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _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^)+(0.0544P)^2^+5.5958P] 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 SHELXL _refine_ls_extinction_coef 0.00033(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4259 _refine_ls_number_parameters 363 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.45917(3) 0.7500 0.04567(16) Uani 1 2 d S . . Ag2 Ag 0.685223(18) 0.12524(2) 0.63386(3) 0.07021(17) Uani 1 1 d . . . C1 C 0.62215(14) 0.3988(2) 0.63445(19) 0.0272(6) Uani 1 1 d . . . H1 H 0.6568 0.3876 0.5959 0.033 Uiso 1 1 calc R . . C2 C 0.62359(14) 0.3239(2) 0.7040(2) 0.0290(7) Uani 1 1 d . . . H2A H 0.5894 0.3332 0.7429 0.035 Uiso 1 1 calc R . . H2B H 0.6162 0.2663 0.6723 0.035 Uiso 1 1 calc R . . C3 C 0.68399(14) 0.3180(2) 0.7633(2) 0.0309(7) Uani 1 1 d . . . H3 H 0.6875 0.3725 0.8022 0.037 Uiso 1 1 calc R . . C11 C 0.55909(18) 0.3904(2) 0.4852(2) 0.0398(8) Uani 1 1 d . . . H11 H 0.5917 0.3924 0.4467 0.048 Uiso 1 1 calc R . . C12 C 0.4984(2) 0.3830(2) 0.4589(3) 0.0497(10) Uani 1 1 d . . . H12 H 0.4796 0.3786 0.3990 0.060 Uiso 1 1 calc R . . C13 C 0.46890(18) 0.3833(2) 0.5389(3) 0.0446(9) Uani 1 1 d . . . H13 H 0.4254 0.3796 0.5416 0.053 Uiso 1 1 calc R . . C21 C 0.67516(16) 0.5469(2) 0.6554(2) 0.0398(8) Uani 1 1 d . . . H21 H 0.7064 0.5382 0.6154 0.048 Uiso 1 1 calc R . . C22 C 0.66606(19) 0.6222(2) 0.7036(2) 0.0471(10) Uani 1 1 d . . . H22 H 0.6893 0.6760 0.7045 0.057 Uiso 1 1 calc R . . C23 C 0.61535(16) 0.6033(2) 0.7515(2) 0.0340(7) Uani 1 1 d . . . H23 H 0.5981 0.6438 0.7915 0.041 Uiso 1 1 calc R . . C31 C 0.68934(17) 0.2391(3) 0.9133(2) 0.0463(9) Uani 1 1 d . A . H31 H 0.6977 0.2891 0.9516 0.056 Uiso 1 1 calc R . . C32 C 0.6819(2) 0.1522(3) 0.9398(3) 0.0594(12) Uani 1 1 d . A . H32 H 0.6841 0.1296 0.9996 0.071 Uiso 1 1 calc R . . C33 C 0.67046(18) 0.1049(3) 0.8605(3) 0.0535(11) Uani 1 1 d . . . H33 H 0.6633 0.0423 0.8579 0.064 Uiso 1 1 calc R A . C41 C 0.79129(16) 0.3614(2) 0.7275(2) 0.0390(8) Uani 1 1 d . A . H41 H 0.8008 0.4028 0.7752 0.047 Uiso 1 1 calc R . . C42 C 0.82878(16) 0.3373(3) 0.6623(2) 0.0439(9) Uani 1 1 d . A . H42 H 0.8693 0.3583 0.6551 0.053 Uiso 1 1 calc R . . C43 C 0.79482(17) 0.2754(2) 0.6087(2) 0.0413(8) Uani 1 1 d . . . H43 H 0.8095 0.2466 0.5578 0.050 Uiso 1 1 calc R A . N11 N 0.50963(12) 0.38934(18) 0.61093(19) 0.0357(6) Uani 1 1 d . . . N12 N 0.56531(12) 0.39464(16) 0.57609(16) 0.0286(6) Uani 1 1 d . . . N21 N 0.59402(11) 0.52101(17) 0.73398(16) 0.0279(6) Uani 1 1 d . . . N22 N 0.63199(11) 0.48709(17) 0.67429(15) 0.0254(5) Uani 1 1 d . . . N31 N 0.67065(14) 0.1572(2) 0.7877(2) 0.0442(7) Uani 1 1 d . . . N32 N 0.68255(12) 0.23971(19) 0.82243(18) 0.0353(6) Uani 1 1 d . . . N41 N 0.73929(13) 0.26122(19) 0.63739(17) 0.0366(7) Uani 1 1 d . . . N42 N 0.73806(12) 0.31496(17) 0.71098(17) 0.0316(6) Uani 1 1 d . . . N1 N 0.78523(16) 0.0082(2) 0.56957(19) 0.0482(8) Uani 1 1 d . . . O1 O 0.74777(19) -0.0065(2) 0.6275(2) 0.0848(12) Uani 1 1 d . . . O2 O 0.78023(14) 0.07787(18) 0.52451(18) 0.0595(8) Uani 1 1 d . . . O3 O 0.82625(15) -0.04669(19) 0.55827(19) 0.0613(8) Uani 1 1 d . . . N2 N 0.5931(4) 0.0765(7) 0.5087(6) 0.063(2) Uani 0.50 1 d P A 1 O4 O 0.6251(3) 0.0252(4) 0.5605(6) 0.079(2) Uani 0.50 1 d P A 1 O5 O 0.5966(10) 0.1554(14) 0.5224(14) 0.075(5) Uani 0.50 1 d P A 1 O6 O 0.5617(4) 0.0440(5) 0.4421(5) 0.086(2) Uani 0.50 1 d P A 1 N51 N 0.5846(11) 0.137(2) 0.5387(17) 0.081(7) Uani 0.50 1 d P A 2 C51 C 0.5386(5) 0.1339(7) 0.5036(7) 0.066(3) Uani 0.50 1 d P A 2 C52 C 0.4751(5) 0.1371(8) 0.4585(9) 0.089(3) Uani 0.50 1 d P A 2 H52A H 0.4500 0.1784 0.4910 0.133 Uiso 0.50 1 calc PR A 2 H52B H 0.4568 0.0773 0.4585 0.133 Uiso 0.50 1 calc PR A 2 H52C H 0.4766 0.1577 0.3963 0.133 Uiso 0.50 1 calc PR A 2 N61 N 0.5000 0.2295(4) 0.2500 0.0856(18) Uani 1 2 d SD . 3 C61 C 0.4764(5) 0.2031(7) 0.3137(7) 0.072(3) Uani 0.50 1 d PD B 3 C62 C 0.4452(6) 0.1704(8) 0.3896(7) 0.087(3) Uani 0.50 1 d PD B 3 H62A H 0.4731 0.1750 0.4448 0.130 Uiso 0.50 1 calc PR B 3 H62B H 0.4333 0.1079 0.3792 0.130 Uiso 0.50 1 calc PR B 3 H62C H 0.4082 0.2064 0.3960 0.130 Uiso 0.50 1 calc PR B 3 N81 N 0.5421(8) 1.0086(10) 0.2984(11) 0.075 Uiso 0.25 1 d PD C 4 C81 C 0.5156(9) 0.9401(11) 0.3048(14) 0.075 Uiso 0.25 1 d PD . 4 C82 C 0.5049(10) 0.8468(10) 0.3258(14) 0.075 Uiso 0.25 1 d PD D 4 N82 N 0.4990(8) 0.8754(10) 0.2795(10) 0.075 Uiso 0.25 1 d PD . 5 C83 C 0.5194(7) 0.9442(11) 0.2555(16) 0.075 Uiso 0.25 1 d PD . 5 C84 C 0.5661(8) 1.0071(12) 0.2306(14) 0.075 Uiso 0.25 1 d PD E 5 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 0.0351(2) 0.0415(2) 0.0640(3) 0.000 0.02497(19) 0.000 Ag2 0.0823(3) 0.0387(2) 0.0966(3) -0.01164(16) 0.0480(2) -0.00158(15) C1 0.0257(16) 0.0293(16) 0.0265(15) -0.0010(12) 0.0028(12) 0.0040(13) C2 0.0289(17) 0.0270(16) 0.0312(15) 0.0028(12) 0.0035(13) 0.0028(13) C3 0.0295(17) 0.0312(17) 0.0326(16) 0.0068(13) 0.0061(13) 0.0059(13) C11 0.054(2) 0.0336(18) 0.0297(16) 0.0014(14) -0.0077(16) -0.0017(16) C12 0.063(3) 0.037(2) 0.044(2) 0.0044(16) -0.0230(19) -0.0047(18) C13 0.035(2) 0.0322(19) 0.063(2) -0.0008(16) -0.0160(18) 0.0013(15) C21 0.0332(19) 0.052(2) 0.0352(17) -0.0038(15) 0.0087(15) -0.0167(16) C22 0.056(2) 0.045(2) 0.0410(19) -0.0095(16) 0.0077(18) -0.0246(18) C23 0.039(2) 0.0320(18) 0.0303(16) -0.0048(13) -0.0008(14) -0.0023(14) C31 0.040(2) 0.061(2) 0.0382(19) 0.0172(17) 0.0044(16) 0.0134(18) C32 0.054(3) 0.071(3) 0.055(2) 0.035(2) 0.014(2) 0.021(2) C33 0.045(2) 0.043(2) 0.075(3) 0.028(2) 0.020(2) 0.0125(18) C41 0.0303(19) 0.042(2) 0.0451(19) 0.0055(15) 0.0030(15) 0.0043(15) C42 0.0305(19) 0.050(2) 0.053(2) 0.0117(17) 0.0113(16) 0.0059(16) C43 0.041(2) 0.042(2) 0.0434(19) 0.0113(16) 0.0164(16) 0.0134(16) N11 0.0253(15) 0.0345(15) 0.0463(16) -0.0037(12) -0.0027(13) 0.0022(11) N12 0.0308(15) 0.0253(13) 0.0287(13) -0.0016(10) -0.0039(11) 0.0017(11) N21 0.0258(14) 0.0311(14) 0.0267(12) -0.0010(10) 0.0023(10) 0.0013(11) N22 0.0220(13) 0.0301(14) 0.0240(12) 0.0021(10) 0.0010(10) 0.0000(10) N31 0.0435(18) 0.0341(16) 0.0569(18) 0.0130(14) 0.0153(15) 0.0095(13) N32 0.0317(15) 0.0378(16) 0.0368(15) 0.0120(12) 0.0055(12) 0.0102(12) N41 0.0378(17) 0.0387(16) 0.0345(14) 0.0044(12) 0.0095(12) 0.0101(12) N42 0.0268(14) 0.0332(15) 0.0352(14) 0.0078(11) 0.0042(11) 0.0100(11) N1 0.075(2) 0.0391(18) 0.0311(15) -0.0015(13) 0.0076(15) 0.0112(17) O1 0.155(3) 0.0480(18) 0.0610(18) 0.0146(14) 0.063(2) 0.022(2) O2 0.083(2) 0.0453(16) 0.0545(16) 0.0181(13) 0.0323(15) 0.0188(14) O3 0.072(2) 0.0518(17) 0.0585(17) -0.0065(13) -0.0054(15) 0.0226(15) N2 0.064(6) 0.064(6) 0.065(6) -0.006(5) 0.019(5) -0.023(5) O4 0.068(4) 0.051(4) 0.115(6) -0.021(4) -0.009(4) -0.003(3) O5 0.092(12) 0.064(7) 0.072(7) -0.014(5) 0.028(6) -0.006(6) O6 0.095(6) 0.083(5) 0.077(5) -0.010(4) -0.002(4) -0.022(4) N51 0.043(8) 0.13(2) 0.070(11) -0.014(10) -0.005(8) -0.010(8) C51 0.058(7) 0.071(7) 0.072(6) 0.005(5) 0.023(6) -0.011(5) C52 0.064(7) 0.088(8) 0.111(9) 0.006(7) -0.005(6) -0.002(6) N61 0.082(5) 0.077(4) 0.099(5) 0.000 0.016(4) 0.000 C61 0.070(7) 0.059(6) 0.084(7) 0.007(5) -0.008(5) -0.006(5) C62 0.087(8) 0.071(7) 0.102(8) 0.022(6) 0.006(7) -0.011(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 Ag1 N21 2.274(2) . ? Ag1 N21 2.274(2) 2_656 ? Ag1 N11 2.345(3) . ? Ag1 N11 2.345(3) 2_656 ? Ag2 O4 2.213(6) . ? Ag2 N41 2.348(3) . ? Ag2 N31 2.388(3) . ? Ag2 O1 2.401(3) . ? Ag2 O5 2.47(2) . ? Ag2 N51 2.51(2) . ? C1 N12 1.448(4) . ? C1 N22 1.457(4) . ? C1 C2 1.525(4) . ? C2 C3 1.519(4) . ? C3 N42 1.465(4) . ? C3 N32 1.468(4) . ? C11 C12 1.348(6) . ? C11 N12 1.349(4) . ? C12 C13 1.400(6) . ? C13 N11 1.333(4) . ? C21 N22 1.344(4) . ? C21 C22 1.359(5) . ? C22 C23 1.391(5) . ? C23 N21 1.333(4) . ? C31 N32 1.348(4) . ? C31 C32 1.372(6) . ? C32 C33 1.381(6) . ? C33 N31 1.337(5) . ? C41 N42 1.354(4) . ? C41 C42 1.369(5) . ? C42 C43 1.392(5) . ? C43 N41 1.331(4) . ? N11 N12 1.359(4) . ? N21 N22 1.362(3) . ? N31 N32 1.355(4) . ? N41 N42 1.361(4) . ? N1 O3 1.234(4) . ? N1 O2 1.240(4) . ? N1 O1 1.255(4) . ? N2 O5 1.20(3) . ? N2 O6 1.253(11) . ? N2 O4 1.254(11) . ? N51 C51 1.09(3) . ? C51 C52 1.481(16) . ? N61 C61 1.185(10) 2_655 ? N61 C61 1.185(10) . ? C61 C62 1.451(12) . ? N81 C81 1.183(11) . ? C81 C82 1.454(13) . ? C81 C81 1.71(4) 2_655 ? N82 N82 0.88(3) 2_655 ? N82 C83 1.188(11) . ? N82 C83 1.21(2) 2_655 ? C83 C83 0.85(3) 2_655 ? C83 N82 1.21(2) 2_655 ? C83 C84 1.455(13) . ? 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 N21 Ag1 N21 131.95(13) . 2_656 ? N21 Ag1 N11 86.52(9) . . ? N21 Ag1 N11 115.07(9) 2_656 . ? N21 Ag1 N11 115.07(9) . 2_656 ? N21 Ag1 N11 86.52(9) 2_656 2_656 ? N11 Ag1 N11 127.06(14) . 2_656 ? O4 Ag2 N41 150.5(2) . . ? O4 Ag2 N31 119.2(2) . . ? N41 Ag2 N31 84.98(10) . . ? O4 Ag2 O1 74.7(2) . . ? N41 Ag2 O1 115.41(12) . . ? N31 Ag2 O1 108.96(10) . . ? O4 Ag2 O5 53.1(5) . . ? N41 Ag2 O5 102.4(4) . . ? N31 Ag2 O5 116.5(4) . . ? O1 Ag2 O5 122.3(5) . . ? O4 Ag2 N51 46.9(8) . . ? N41 Ag2 N51 111.4(7) . . ? N31 Ag2 N51 110.3(7) . . ? O1 Ag2 N51 120.1(8) . . ? O5 Ag2 N51 10.7(8) . . ? N12 C1 N22 111.7(2) . . ? N12 C1 C2 110.0(2) . . ? N22 C1 C2 113.4(2) . . ? C3 C2 C1 113.8(2) . . ? N42 C3 N32 110.7(2) . . ? N42 C3 C2 112.7(2) . . ? N32 C3 C2 109.4(3) . . ? C12 C11 N12 107.8(3) . . ? C11 C12 C13 105.1(3) . . ? N11 C13 C12 111.4(3) . . ? N22 C21 C22 107.8(3) . . ? C21 C22 C23 105.1(3) . . ? N21 C23 C22 111.4(3) . . ? N32 C31 C32 106.8(4) . . ? C31 C32 C33 104.9(3) . . ? N31 C33 C32 112.3(4) . . ? N42 C41 C42 106.6(3) . . ? C41 C42 C43 105.3(3) . . ? N41 C43 C42 111.9(3) . . ? C13 N11 N12 104.3(3) . . ? C13 N11 Ag1 129.6(2) . . ? N12 N11 Ag1 117.48(19) . . ? C11 N12 N11 111.4(3) . . ? C11 N12 C1 127.6(3) . . ? N11 N12 C1 120.9(2) . . ? C23 N21 N22 104.6(2) . . ? C23 N21 Ag1 131.0(2) . . ? N22 N21 Ag1 121.13(18) . . ? C21 N22 N21 111.2(3) . . ? C21 N22 C1 126.9(3) . . ? N21 N22 C1 121.9(2) . . ? C33 N31 N32 103.8(3) . . ? C33 N31 Ag2 132.1(3) . . ? N32 N31 Ag2 120.76(19) . . ? C31 N32 N31 112.1(3) . . ? C31 N32 C3 127.0(3) . . ? N31 N32 C3 120.8(3) . . ? C43 N41 N42 104.2(3) . . ? C43 N41 Ag2 126.6(2) . . ? N42 N41 Ag2 119.05(18) . . ? C41 N42 N41 112.0(3) . . ? C41 N42 C3 126.8(3) . . ? N41 N42 C3 121.2(3) . . ? O3 N1 O2 121.1(3) . . ? O3 N1 O1 119.7(3) . . ? O2 N1 O1 119.2(3) . . ? N1 O1 Ag2 106.6(2) . . ? O5 N2 O6 122.6(14) . . ? O5 N2 O4 118.3(13) . . ? O6 N2 O4 119.0(10) . . ? N2 O4 Ag2 99.3(6) . . ? N2 O5 Ag2 88.2(13) . . ? C51 N51 Ag2 172(2) . . ? N51 C51 C52 176(2) . . ? C61 N61 C61 140.9(12) 2_655 . ? N61 C61 C62 177.8(10) . . ? N81 C81 C82 159.6(18) . . ? N81 C81 C81 94.5(15) . 2_655 ? C82 C81 C81 98.5(11) . 2_655 ? N82 N82 C83 69.5(15) 2_655 . ? N82 N82 C83 67.2(13) 2_655 2_655 ? C83 N82 C83 41.3(16) . 2_655 ? C83 C83 N82 70.5(14) 2_655 . ? C83 C83 N82 68.2(15) 2_655 2_655 ? N82 C83 N82 43.3(15) . 2_655 ? C83 C83 C84 131(2) 2_655 . ? N82 C83 C84 157.5(16) . . ? N82 C83 C84 131(2) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 C1 C2 C3 175.0(2) . . . . ? N22 C1 C2 C3 -59.0(3) . . . . ? C1 C2 C3 N42 -51.7(3) . . . . ? C1 C2 C3 N32 -175.3(2) . . . . ? N12 C11 C12 C13 0.1(4) . . . . ? C11 C12 C13 N11 -0.8(4) . . . . ? N22 C21 C22 C23 -0.1(4) . . . . ? C21 C22 C23 N21 -0.1(4) . . . . ? N32 C31 C32 C33 -0.2(4) . . . . ? C31 C32 C33 N31 0.1(5) . . . . ? N42 C41 C42 C43 -0.2(4) . . . . ? C41 C42 C43 N41 0.3(4) . . . . ? C12 C13 N11 N12 1.1(4) . . . . ? C12 C13 N11 Ag1 147.1(3) . . . . ? N21 Ag1 N11 C13 -132.7(3) . . . . ? N21 Ag1 N11 C13 2.6(3) 2_656 . . . ? N11 Ag1 N11 C13 108.2(3) 2_656 . . . ? N21 Ag1 N11 N12 9.7(2) . . . . ? N21 Ag1 N11 N12 145.0(2) 2_656 . . . ? N11 Ag1 N11 N12 -109.4(2) 2_656 . . . ? C12 C11 N12 N11 0.5(4) . . . . ? C12 C11 N12 C1 176.9(3) . . . . ? C13 N11 N12 C11 -1.0(3) . . . . ? Ag1 N11 N12 C11 -151.9(2) . . . . ? C13 N11 N12 C1 -177.7(3) . . . . ? Ag1 N11 N12 C1 31.4(3) . . . . ? N22 C1 N12 C11 107.6(3) . . . . ? C2 C1 N12 C11 -125.5(3) . . . . ? N22 C1 N12 N11 -76.3(3) . . . . ? C2 C1 N12 N11 50.6(3) . . . . ? C22 C23 N21 N22 0.2(4) . . . . ? C22 C23 N21 Ag1 -158.8(2) . . . . ? N21 Ag1 N21 C23 17.8(2) 2_656 . . . ? N11 Ag1 N21 C23 138.9(3) . . . . ? N11 Ag1 N21 C23 -91.5(3) 2_656 . . . ? N21 Ag1 N21 N22 -138.2(2) 2_656 . . . ? N11 Ag1 N21 N22 -17.2(2) . . . . ? N11 Ag1 N21 N22 112.5(2) 2_656 . . . ? C22 C21 N22 N21 0.3(4) . . . . ? C22 C21 N22 C1 176.6(3) . . . . ? C23 N21 N22 C21 -0.3(3) . . . . ? Ag1 N21 N22 C21 161.3(2) . . . . ? C23 N21 N22 C1 -176.9(3) . . . . ? Ag1 N21 N22 C1 -15.3(3) . . . . ? N12 C1 N22 C21 -110.0(3) . . . . ? C2 C1 N22 C21 124.9(3) . . . . ? N12 C1 N22 N21 66.0(3) . . . . ? C2 C1 N22 N21 -59.1(3) . . . . ? C32 C33 N31 N32 0.0(4) . . . . ? C32 C33 N31 Ag2 158.7(3) . . . . ? O4 Ag2 N31 C33 55.6(4) . . . . ? N41 Ag2 N31 C33 -142.2(4) . . . . ? O1 Ag2 N31 C33 -27.1(4) . . . . ? O5 Ag2 N31 C33 116.3(6) . . . . ? N51 Ag2 N31 C33 106.8(8) . . . . ? O4 Ag2 N31 N32 -148.7(3) . . . . ? N41 Ag2 N31 N32 13.5(2) . . . . ? O1 Ag2 N31 N32 128.6(2) . . . . ? O5 Ag2 N31 N32 -87.9(5) . . . . ? N51 Ag2 N31 N32 -97.5(8) . . . . ? C32 C31 N32 N31 0.3(4) . . . . ? C32 C31 N32 C3 177.2(3) . . . . ? C33 N31 N32 C31 -0.2(4) . . . . ? Ag2 N31 N32 C31 -161.9(2) . . . . ? C33 N31 N32 C3 -177.4(3) . . . . ? Ag2 N31 N32 C3 21.0(4) . . . . ? N42 C3 N32 C31 113.4(3) . . . . ? C2 C3 N32 C31 -121.8(3) . . . . ? N42 C3 N32 N31 -69.9(4) . . . . ? C2 C3 N32 N31 54.9(4) . . . . ? C42 C43 N41 N42 -0.3(4) . . . . ? C42 C43 N41 Ag2 -144.6(2) . . . . ? O4 Ag2 N41 C43 -81.8(5) . . . . ? N31 Ag2 N41 C43 131.2(3) . . . . ? O1 Ag2 N41 C43 22.6(3) . . . . ? O5 Ag2 N41 C43 -112.7(5) . . . . ? N51 Ag2 N41 C43 -118.9(7) . . . . ? O4 Ag2 N41 N42 138.6(4) . . . . ? N31 Ag2 N41 N42 -8.4(2) . . . . ? O1 Ag2 N41 N42 -117.1(2) . . . . ? O5 Ag2 N41 N42 107.7(5) . . . . ? N51 Ag2 N41 N42 101.4(7) . . . . ? C42 C41 N42 N41 0.0(4) . . . . ? C42 C41 N42 C3 179.5(3) . . . . ? C43 N41 N42 C41 0.2(3) . . . . ? Ag2 N41 N42 C41 147.7(2) . . . . ? C43 N41 N42 C3 -179.3(3) . . . . ? Ag2 N41 N42 C3 -31.8(3) . . . . ? N32 C3 N42 C41 -101.6(4) . . . . ? C2 C3 N42 C41 135.4(3) . . . . ? N32 C3 N42 N41 77.8(3) . . . . ? C2 C3 N42 N41 -45.2(4) . . . . ? O3 N1 O1 Ag2 174.2(3) . . . . ? O2 N1 O1 Ag2 -5.9(4) . . . . ? O4 Ag2 O1 N1 105.4(4) . . . . ? N41 Ag2 O1 N1 -45.0(3) . . . . ? N31 Ag2 O1 N1 -138.5(3) . . . . ? O5 Ag2 O1 N1 80.6(5) . . . . ? N51 Ag2 O1 N1 92.9(7) . . . . ? O5 N2 O4 Ag2 -11.2(13) . . . . ? O6 N2 O4 Ag2 164.9(7) . . . . ? N41 Ag2 O4 N2 -32.8(8) . . . . ? N31 Ag2 O4 N2 108.8(6) . . . . ? O1 Ag2 O4 N2 -147.7(6) . . . . ? O5 Ag2 O4 N2 6.0(7) . . . . ? N51 Ag2 O4 N2 17.4(9) . . . . ? O6 N2 O5 Ag2 -166.1(9) . . . . ? O4 N2 O5 Ag2 9.9(11) . . . . ? O4 Ag2 O5 N2 -6.2(7) . . . . ? N41 Ag2 O5 N2 155.4(8) . . . . ? N31 Ag2 O5 N2 -114.0(9) . . . . ? O1 Ag2 O5 N2 24.2(11) . . . . ? N51 Ag2 O5 N2 -57(6) . . . . ? O4 Ag2 N51 C51 52(18) . . . . ? N41 Ag2 N51 C51 -152(18) . . . . ? N31 Ag2 N51 C51 -60(18) . . . . ? O1 Ag2 N51 C51 68(18) . . . . ? O5 Ag2 N51 C51 173(24) . . . . ? Ag2 N51 C51 C52 112(25) . . . . ? C61 N61 C61 C62 -86(29) 2_655 . . . ? N82 N82 C83 C83 78(3) 2_655 . . 2_655 ? C83 N82 C83 N82 -78(3) 2_655 . . 2_655 ? N82 N82 C83 C84 -86(7) 2_655 . . . ? C83 N82 C83 C84 -164(8) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.718 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.071 data_jg123iis _database_code_CSD 204328 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Ag2 F6 N16 O6 S2' _chemical_formula_weight 1130.60 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 9.8259(5) _cell_length_b 10.4688(5) _cell_length_c 12.3726(6) _cell_angle_alpha 96.8090(10) _cell_angle_beta 111.2290(10) _cell_angle_gamma 107.9600(10) _cell_volume 1089.84(9) _cell_formula_units_Z 2 _cell_measurement_temperature 220.0(2) _cell_measurement_reflns_used 7613 _cell_measurement_theta_min 2.404 _cell_measurement_theta_max 26.386 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6166 _exptl_absorpt_correction_T_max 0.7728 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 9992 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4444 _reflns_number_gt 3544 _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^)+(0.0292P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4444 _refine_ls_number_parameters 363 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.017 _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 Ag Ag 0.33379(3) 0.10331(2) 0.46222(2) 0.05739(10) Uani 1 1 d . . . C1 C 0.6579(3) 0.3378(3) 0.7087(2) 0.0421(6) Uani 1 1 d . . . H1 H 0.7482 0.4141 0.7751 0.038(6) Uiso 1 1 calc R . . C2 C 0.6952(3) 0.2063(3) 0.7126(2) 0.0389(6) Uani 1 1 d . . . H2A H 0.6902 0.1763 0.7836 0.049(7) Uiso 1 1 calc R . . H2B H 0.6161 0.1315 0.6412 0.041(7) Uiso 1 1 calc R . . C3 C 0.8591(3) 0.2332(3) 0.7169(2) 0.0392(6) Uani 1 1 d . . . H3 H 0.9277 0.3290 0.7674 0.027(6) Uiso 1 1 calc R . . C11 C 0.5045(4) 0.4129(3) 0.8090(3) 0.0547(7) Uani 1 1 d . . . H11 H 0.5842 0.4964 0.8628 0.067(9) Uiso 1 1 calc R . . C12 C 0.3533(4) 0.3595(3) 0.7964(3) 0.0608(8) Uani 1 1 d . . . H12 H 0.3073 0.3978 0.8394 0.074(9) Uiso 1 1 calc R . . C13 C 0.2818(3) 0.2373(3) 0.7071(3) 0.0538(7) Uani 1 1 d . . . H13 H 0.1756 0.1777 0.6792 0.054(8) Uiso 1 1 calc R . . C21 C 0.7194(3) 0.5046(3) 0.5868(3) 0.0596(8) Uani 1 1 d . . . H21 H 0.7941 0.5830 0.6499 0.058(9) Uiso 1 1 calc R . . C22 C 0.6691(4) 0.4964(4) 0.4672(4) 0.0698(10) Uani 1 1 d . . . H22 H 0.7017 0.5669 0.4311 0.073(9) Uiso 1 1 calc R . . C23 C 0.5604(4) 0.3627(4) 0.4106(3) 0.0631(9) Uani 1 1 d . . . H23 H 0.5055 0.3275 0.3268 0.069(10) Uiso 1 1 calc R . . C31 C 0.9522(3) 0.3255(3) 0.5665(3) 0.0500(7) Uani 1 1 d . . . H31 H 1.0295 0.4124 0.6158 0.045(7) Uiso 1 1 calc R . . C32 C 0.9110(4) 0.2739(3) 0.4477(3) 0.0619(8) Uani 1 1 d . . . H32 H 0.9530 0.3179 0.3986 0.048(7) Uiso 1 1 calc R . . C33 C 0.7958(4) 0.1447(3) 0.4152(3) 0.0602(8) Uani 1 1 d . . . H33 H 0.7460 0.0846 0.3376 0.071(10) Uiso 1 1 calc R . . C41 C 1.0538(3) 0.1769(3) 0.8794(2) 0.0550(7) Uani 1 1 d . . . H41 H 1.1136 0.2671 0.9303 0.052(8) Uiso 1 1 calc R . . C42 C 1.0786(4) 0.0603(4) 0.8993(3) 0.0680(9) Uani 1 1 d . . . H42 H 1.1588 0.0531 0.9657 0.079(10) Uiso 1 1 calc R . . C43 C 0.9622(4) -0.0455(4) 0.8025(3) 0.0676(9) Uani 1 1 d . . . H43 H 0.9498 -0.1395 0.7927 0.085(11) Uiso 1 1 calc R . . N11 N 0.3813(2) 0.2138(2) 0.6653(2) 0.0487(5) Uani 1 1 d . . . N12 N 0.5190(2) 0.3240(2) 0.73026(19) 0.0428(5) Uani 1 1 d . . . N21 N 0.5419(3) 0.2888(2) 0.4890(2) 0.0504(6) Uani 1 1 d . . . N22 N 0.6421(2) 0.3792(2) 0.5980(2) 0.0445(5) Uani 1 1 d . . . N31 N 0.7626(3) 0.1141(2) 0.5060(2) 0.0519(6) Uani 1 1 d . . . N32 N 0.8608(2) 0.2279(2) 0.59941(18) 0.0411(5) Uani 1 1 d . . . N41 N 0.8691(3) 0.0017(2) 0.7242(2) 0.0592(6) Uani 1 1 d . . . N42 N 0.9286(2) 0.1406(2) 0.77367(18) 0.0433(5) Uani 1 1 d . . . S1A S 0.14182(8) 0.63571(7) 0.91731(6) 0.0496(3) Uani 0.598(3) 1 d PD A 1 O1A O 0.1881(5) 0.5249(5) 0.9476(6) 0.0848(14) Uani 0.598(3) 1 d P A 1 O2A O 0.1261(6) 0.7138(6) 1.0059(5) 0.115(2) Uani 0.598(3) 1 d P A 1 O3A O 0.0276(5) 0.6050(5) 0.8010(4) 0.0924(16) Uani 0.598(3) 1 d P A 1 C51A C 0.3181(11) 0.7545(8) 0.9103(9) 0.072(2) Uani 0.598(3) 1 d PD A 1 F1A F 0.2957(14) 0.8635(10) 0.8778(9) 0.094(3) Uani 0.598(3) 1 d PD A 1 F2A F 0.3593(8) 0.6977(5) 0.8344(6) 0.141(2) Uani 0.598(3) 1 d PD A 1 F3A F 0.4396(11) 0.8040(9) 1.0223(8) 0.102(3) Uani 0.598(3) 1 d P A 1 S1B S 0.14182(8) 0.63571(7) 0.91731(6) 0.0496(3) Uani 0.40 1 d PD A 2 O1B O 0.0108(9) 0.6819(8) 0.8824(8) 0.094(2) Uani 0.402(3) 1 d P A 2 O2B O 0.1224(10) 0.5382(8) 0.8239(10) 0.124(4) Uani 0.402(3) 1 d P A 2 O3B O 0.1703(8) 0.5995(10) 1.0270(7) 0.103(3) Uani 0.402(3) 1 d P A 2 C51B C 0.3224(17) 0.7809(13) 0.9446(15) 0.072(2) Uani 0.40 1 d PD A 2 F1B F 0.296(3) 0.8339(19) 0.8526(14) 0.140(7) Uani 0.402(3) 1 d PD A 2 F2B F 0.3312(12) 0.8844(7) 1.0281(6) 0.162(4) Uani 0.402(3) 1 d PD A 2 F3B F 0.4339(18) 0.7466(19) 0.9637(14) 0.151(7) Uani 0.402(3) 1 d P A 2 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 0.05917(16) 0.05036(15) 0.05482(16) 0.00988(10) 0.02100(12) 0.01579(11) C1 0.0384(14) 0.0449(15) 0.0463(15) 0.0109(12) 0.0197(12) 0.0182(12) C2 0.0405(13) 0.0480(15) 0.0387(14) 0.0166(12) 0.0221(12) 0.0220(12) C3 0.0389(13) 0.0450(15) 0.0389(14) 0.0110(11) 0.0187(12) 0.0195(11) C11 0.0644(19) 0.0621(19) 0.0468(17) 0.0092(15) 0.0252(15) 0.0355(16) C12 0.071(2) 0.079(2) 0.063(2) 0.0228(17) 0.0449(17) 0.0466(18) C13 0.0503(17) 0.0673(19) 0.0673(19) 0.0271(16) 0.0390(15) 0.0317(15) C21 0.0488(17) 0.0470(18) 0.105(3) 0.0360(19) 0.0452(19) 0.0253(15) C22 0.065(2) 0.083(2) 0.110(3) 0.069(2) 0.060(2) 0.0467(19) C23 0.0633(19) 0.095(3) 0.068(2) 0.050(2) 0.0425(18) 0.0481(19) C31 0.0472(16) 0.0512(17) 0.068(2) 0.0274(15) 0.0353(15) 0.0225(14) C32 0.083(2) 0.072(2) 0.070(2) 0.0403(18) 0.0573(19) 0.0423(18) C33 0.095(2) 0.063(2) 0.0494(18) 0.0248(16) 0.0460(18) 0.0423(18) C41 0.0494(16) 0.076(2) 0.0383(16) 0.0122(15) 0.0156(14) 0.0269(16) C42 0.067(2) 0.100(3) 0.0509(19) 0.0328(19) 0.0190(17) 0.051(2) C43 0.085(2) 0.072(2) 0.061(2) 0.0287(18) 0.0250(19) 0.0514(19) N11 0.0449(13) 0.0522(14) 0.0590(15) 0.0132(11) 0.0314(12) 0.0204(11) N12 0.0435(12) 0.0489(13) 0.0458(12) 0.0124(10) 0.0238(10) 0.0242(11) N21 0.0516(14) 0.0617(15) 0.0509(14) 0.0271(12) 0.0275(12) 0.0266(12) N22 0.0426(12) 0.0468(13) 0.0596(15) 0.0252(11) 0.0293(12) 0.0234(10) N31 0.0699(16) 0.0500(14) 0.0431(13) 0.0136(11) 0.0312(12) 0.0229(12) N32 0.0439(12) 0.0460(12) 0.0444(12) 0.0152(10) 0.0264(10) 0.0207(10) N41 0.0667(16) 0.0539(15) 0.0537(15) 0.0174(12) 0.0134(13) 0.0319(13) N42 0.0421(12) 0.0552(14) 0.0393(12) 0.0137(10) 0.0176(10) 0.0259(11) S1A 0.0515(4) 0.0527(5) 0.0395(4) 0.0047(3) 0.0163(3) 0.0198(3) O1A 0.062(3) 0.076(3) 0.127(5) 0.049(3) 0.044(3) 0.026(2) O2A 0.099(4) 0.112(4) 0.109(4) -0.047(3) 0.073(4) 0.001(3) O3A 0.077(3) 0.104(4) 0.052(3) 0.014(2) 0.001(2) 0.011(3) C51A 0.092(3) 0.063(4) 0.049(7) 0.017(4) 0.026(4) 0.015(3) F1A 0.106(4) 0.060(3) 0.121(8) 0.043(3) 0.045(5) 0.034(3) F2A 0.186(5) 0.118(4) 0.201(6) 0.050(4) 0.170(5) 0.058(4) F3A 0.052(3) 0.106(5) 0.112(5) 0.063(4) 0.007(4) 0.005(3) S1B 0.0515(4) 0.0527(5) 0.0395(4) 0.0047(3) 0.0163(3) 0.0198(3) O1B 0.105(5) 0.094(5) 0.126(7) 0.053(5) 0.062(5) 0.067(4) O2B 0.092(5) 0.085(5) 0.157(8) -0.068(5) 0.077(6) -0.007(4) O3B 0.069(4) 0.112(7) 0.071(5) 0.054(5) -0.002(4) -0.012(4) C51B 0.092(3) 0.063(4) 0.049(7) 0.017(4) 0.026(4) 0.015(3) F1B 0.164(10) 0.174(16) 0.067(5) 0.070(9) 0.057(6) 0.020(10) F2B 0.220(10) 0.077(4) 0.097(5) 0.001(4) 0.054(6) -0.038(5) F3B 0.051(5) 0.210(17) 0.172(16) 0.110(13) 0.034(9) 0.021(9) _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 N21 2.230(2) . ? Ag N41 2.285(2) 2_656 ? Ag N31 2.320(2) 2_656 ? Ag N11 2.449(2) . ? C1 N12 1.451(3) . ? C1 N22 1.454(3) . ? C1 C2 1.531(3) . ? C2 C3 1.526(3) . ? C3 N32 1.454(3) . ? C3 N42 1.457(3) . ? C11 N12 1.343(3) . ? C11 C12 1.358(4) . ? C12 C13 1.379(4) . ? C13 N11 1.330(3) . ? C21 N22 1.350(3) . ? C21 C22 1.362(5) . ? C22 C23 1.376(5) . ? C23 N21 1.339(3) . ? C31 N32 1.347(3) . ? C31 C32 1.364(4) . ? C32 C33 1.367(4) . ? C33 N31 1.326(3) . ? C41 N42 1.341(3) . ? C41 C42 1.350(4) . ? C42 C43 1.372(5) . ? C43 N41 1.331(4) . ? N11 N12 1.356(3) . ? N21 N22 1.358(3) . ? N31 N32 1.357(3) . ? N31 Ag 2.320(2) 2_656 ? N41 N42 1.355(3) . ? N41 Ag 2.285(2) 2_656 ? S1A O2A 1.371(4) . ? S1A O3A 1.390(4) . ? S1A O1A 1.414(4) . ? S1A C51A 1.833(6) . ? C51A F2A 1.300(9) . ? C51A F1A 1.308(12) . ? C51A F3A 1.365(14) . ? C51B F3B 1.21(3) . ? C51B F1B 1.302(17) . ? C51B F2B 1.364(12) . ? 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 N21 Ag N41 120.27(8) . 2_656 ? N21 Ag N31 148.32(8) . 2_656 ? N41 Ag N31 82.57(8) 2_656 2_656 ? N21 Ag N11 84.91(8) . . ? N41 Ag N11 139.92(8) 2_656 . ? N31 Ag N11 90.04(8) 2_656 . ? N12 C1 N22 110.5(2) . . ? N12 C1 C2 111.6(2) . . ? N22 C1 C2 113.2(2) . . ? C3 C2 C1 110.7(2) . . ? N32 C3 N42 110.62(19) . . ? N32 C3 C2 112.67(19) . . ? N42 C3 C2 112.4(2) . . ? N12 C11 C12 107.2(3) . . ? C11 C12 C13 105.2(3) . . ? N11 C13 C12 111.8(3) . . ? N22 C21 C22 107.3(3) . . ? C21 C22 C23 105.2(3) . . ? N21 C23 C22 112.0(3) . . ? N32 C31 C32 106.8(3) . . ? C31 C32 C33 105.5(3) . . ? N31 C33 C32 112.1(3) . . ? N42 C41 C42 107.6(3) . . ? C41 C42 C43 105.6(3) . . ? N41 C43 C42 111.4(3) . . ? C13 N11 N12 104.2(2) . . ? C13 N11 Ag 130.2(2) . . ? N12 N11 Ag 117.16(15) . . ? C11 N12 N11 111.5(2) . . ? C11 N12 C1 127.6(2) . . ? N11 N12 C1 120.9(2) . . ? C23 N21 N22 104.1(2) . . ? C23 N21 Ag 128.2(2) . . ? N22 N21 Ag 122.97(16) . . ? C21 N22 N21 111.3(2) . . ? C21 N22 C1 127.3(3) . . ? N21 N22 C1 121.3(2) . . ? C33 N31 N32 104.3(2) . . ? C33 N31 Ag 128.3(2) . 2_656 ? N32 N31 Ag 121.20(15) . 2_656 ? C31 N32 N31 111.3(2) . . ? C31 N32 C3 128.1(2) . . ? N31 N32 C3 120.6(2) . . ? C43 N41 N42 104.5(2) . . ? C43 N41 Ag 132.5(2) . 2_656 ? N42 N41 Ag 122.78(16) . 2_656 ? C41 N42 N41 110.9(2) . . ? C41 N42 C3 126.5(2) . . ? N41 N42 C3 122.6(2) . . ? O2A S1A O3A 116.6(4) . . ? O2A S1A O1A 115.1(4) . . ? O3A S1A O1A 114.9(3) . . ? O2A S1A C51A 103.1(3) . . ? O3A S1A C51A 102.2(4) . . ? O1A S1A C51A 101.8(5) . . ? F2A C51A F1A 106.8(8) . . ? F2A C51A F3A 110.2(10) . . ? F1A C51A F3A 106.0(8) . . ? F2A C51A S1A 113.2(5) . . ? F1A C51A S1A 111.1(9) . . ? F3A C51A S1A 109.3(7) . . ? F3B C51B F1B 110.8(15) . . ? F3B C51B F2B 119.4(15) . . ? F1B C51B F2B 100.2(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 C1 C2 C3 -167.7(2) . . . . ? N22 C1 C2 C3 66.8(3) . . . . ? C1 C2 C3 N32 -80.3(3) . . . . ? C1 C2 C3 N42 153.9(2) . . . . ? N12 C11 C12 C13 -0.3(3) . . . . ? C11 C12 C13 N11 0.1(3) . . . . ? N22 C21 C22 C23 0.2(3) . . . . ? C21 C22 C23 N21 -0.2(3) . . . . ? N32 C31 C32 C33 -0.7(3) . . . . ? C31 C32 C33 N31 0.6(4) . . . . ? N42 C41 C42 C43 -0.8(3) . . . . ? C41 C42 C43 N41 0.7(4) . . . . ? C12 C13 N11 N12 0.2(3) . . . . ? C12 C13 N11 Ag -145.8(2) . . . . ? N21 Ag N11 C13 131.1(2) . . . . ? N41 Ag N11 C13 -1.8(3) 2_656 . . . ? N31 Ag N11 C13 -80.2(2) 2_656 . . . ? N21 Ag N11 N12 -11.37(17) . . . . ? N41 Ag N11 N12 -144.23(16) 2_656 . . . ? N31 Ag N11 N12 137.31(18) 2_656 . . . ? C12 C11 N12 N11 0.4(3) . . . . ? C12 C11 N12 C1 178.6(2) . . . . ? C13 N11 N12 C11 -0.4(3) . . . . ? Ag N11 N12 C11 150.91(18) . . . . ? C13 N11 N12 C1 -178.7(2) . . . . ? Ag N11 N12 C1 -27.4(3) . . . . ? N22 C1 N12 C11 -103.7(3) . . . . ? C2 C1 N12 C11 129.5(3) . . . . ? N22 C1 N12 N11 74.3(3) . . . . ? C2 C1 N12 N11 -52.6(3) . . . . ? C22 C23 N21 N22 0.1(3) . . . . ? C22 C23 N21 Ag 155.8(2) . . . . ? N41 Ag N21 C23 8.7(3) 2_656 . . . ? N31 Ag N21 C23 140.1(2) 2_656 . . . ? N11 Ag N21 C23 -138.2(2) . . . . ? N41 Ag N21 N22 160.29(17) 2_656 . . . ? N31 Ag N21 N22 -68.4(2) 2_656 . . . ? N11 Ag N21 N22 13.41(18) . . . . ? C22 C21 N22 N21 -0.2(3) . . . . ? C22 C21 N22 C1 179.5(2) . . . . ? C23 N21 N22 C21 0.0(3) . . . . ? Ag N21 N22 C21 -157.25(17) . . . . ? C23 N21 N22 C1 -179.6(2) . . . . ? Ag N21 N22 C1 23.1(3) . . . . ? N12 C1 N22 C21 107.8(3) . . . . ? C2 C1 N22 C21 -126.2(3) . . . . ? N12 C1 N22 N21 -72.6(3) . . . . ? C2 C1 N22 N21 53.4(3) . . . . ? C32 C33 N31 N32 -0.2(3) . . . . ? C32 C33 N31 Ag -152.2(2) . . . 2_656 ? C32 C31 N32 N31 0.6(3) . . . . ? C32 C31 N32 C3 -179.8(2) . . . . ? C33 N31 N32 C31 -0.2(3) . . . . ? Ag N31 N32 C31 154.28(17) 2_656 . . . ? C33 N31 N32 C3 -179.9(2) . . . . ? Ag N31 N32 C3 -25.4(3) 2_656 . . . ? N42 C3 N32 C31 -107.8(3) . . . . ? C2 C3 N32 C31 125.5(3) . . . . ? N42 C3 N32 N31 71.7(3) . . . . ? C2 C3 N32 N31 -55.0(3) . . . . ? C42 C43 N41 N42 -0.2(4) . . . . ? C42 C43 N41 Ag 174.2(2) . . . 2_656 ? C42 C41 N42 N41 0.8(3) . . . . ? C42 C41 N42 C3 179.5(2) . . . . ? C43 N41 N42 C41 -0.4(3) . . . . ? Ag N41 N42 C41 -175.45(18) 2_656 . . . ? C43 N41 N42 C3 -179.2(2) . . . . ? Ag N41 N42 C3 5.7(3) 2_656 . . . ? N32 C3 N42 C41 121.2(3) . . . . ? C2 C3 N42 C41 -111.9(3) . . . . ? N32 C3 N42 N41 -60.2(3) . . . . ? C2 C3 N42 N41 66.7(3) . . . . ? O2A S1A C51A F2A 176.8(9) . . . . ? O3A S1A C51A F2A -61.9(10) . . . . ? O1A S1A C51A F2A 57.2(10) . . . . ? O2A S1A C51A F1A -63.1(8) . . . . ? O3A S1A C51A F1A 58.3(7) . . . . ? O1A S1A C51A F1A 177.3(7) . . . . ? O2A S1A C51A F3A 53.6(9) . . . . ? O3A S1A C51A F3A 174.9(8) . . . . ? O1A S1A C51A F3A -66.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.447 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.062