# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kb2009 _audit_creation_date 2013-08-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ; bis(pyridine-N-oxide)silver nitrate ; _chemical_name_systematic ; bis(pyridine-N-oxide)silver nitrate ; _chemical_formula_moiety 'C10 H10 Ag N3 O5' _chemical_formula_sum 'C10 H10 Ag N3 O5' _chemical_formula_weight 360.08 _chemical_melting_point ? _chemical_oxdiff_formula 'Ag C15 H15 N4 O6' 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' Ag Ag -0.8971 1.1015 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.2360(4) _cell_length_b 8.7680(5) _cell_length_c 8.7895(4) _cell_angle_alpha 77.874(5) _cell_angle_beta 80.894(4) _cell_angle_gamma 72.726(5) _cell_volume 589.44(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3238 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.0650 _cell_measurement_theta_min 3.6930 _exptl_absorpt_coefficient_mu 1.731 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.029 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 356 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4593 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 29.03 _diffrn_reflns_theta_min 3.06 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.9988 _diffrn_measured_fraction_theta_max 0.8507 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -46.00 53.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 77.0000 60.0000 99 #__ type_ start__ end____ width___ exp.time_ 2 omega 11.00 46.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 77.0000 -180.0000 35 #__ type_ start__ end____ width___ exp.time_ 3 omega -11.00 55.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 -60.0000 66 #__ type_ start__ end____ width___ exp.time_ 4 omega 19.00 84.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 -30.0000 65 #__ type_ start__ end____ width___ exp.time_ 5 omega 63.00 89.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega -11.00 69.00 1.0000 80.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 77.0000 -180.0000 80 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0657758000 _diffrn_orient_matrix_UB_12 -0.0310853000 _diffrn_orient_matrix_UB_13 0.0459598000 _diffrn_orient_matrix_UB_21 0.0462992000 _diffrn_orient_matrix_UB_22 -0.0792913000 _diffrn_orient_matrix_UB_23 -0.0127600000 _diffrn_orient_matrix_UB_31 0.0418425000 _diffrn_orient_matrix_UB_32 -0.0120398000 _diffrn_orient_matrix_UB_33 0.0678997000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 2531 _reflns_number_total 2664 _reflns_odcompleteness_completeness 99.88 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.527 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0166 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+0.1685P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0433 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C13(H13), C16(H16), C14(H14), C15(H15), C11(H11), C10(H10), C12(H12), C17(H17), C19(H19), C18(H18) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.159098(14) 0.310635(14) 0.473557(14) 0.01795(5) Uani 1 1 d . . . N9 N 0.29109(17) 0.21753(16) 0.17401(16) 0.0169(3) Uani 1 1 d . . . O2 O 0.15561(14) 0.55370(14) 0.54168(14) 0.0184(2) Uani 1 1 d . . . O4 O 0.39254(15) 0.23878(15) 0.25686(15) 0.0217(3) Uani 1 1 d . . . O3 O 0.10546(15) 0.12901(14) 0.69157(14) 0.0203(2) Uani 1 1 d . . . O5 O 0.13632(15) 0.23453(15) 0.22958(15) 0.0215(3) Uani 1 1 d . . . N8 N -0.01367(16) 0.18736(16) 0.80163(15) 0.0152(3) Uani 1 1 d . . . N7 N 0.26180(16) 0.64327(16) 0.47608(15) 0.0140(3) Uani 1 1 d . . . C13 C 0.3540(2) 0.8776(2) 0.4620(2) 0.0193(3) Uani 1 1 d . . . H13 H 0.3421 0.9737 0.4970 0.023 Uiso 1 1 calc R . . C16 C -0.1485(2) 0.3898(2) 0.95679(19) 0.0187(3) Uani 1 1 d . . . H16 H -0.1559 0.4889 0.9837 0.022 Uiso 1 1 calc R . . C14 C 0.2434(2) 0.7842(2) 0.5262(2) 0.0174(3) Uani 1 1 d . . . H14 H 0.1566 0.8178 0.6034 0.021 Uiso 1 1 calc R . . C15 C -0.0264(2) 0.3322(2) 0.84032(19) 0.0164(3) Uani 1 1 d . . . H15 H 0.0474 0.3930 0.7883 0.020 Uiso 1 1 calc R . . C11 C 0.4982(2) 0.6849(2) 0.29604(19) 0.0169(3) Uani 1 1 d . . . H11 H 0.5832 0.6504 0.2177 0.020 Uiso 1 1 calc R . . C10 C 0.3870(2) 0.59247(19) 0.36327(18) 0.0146(3) Uani 1 1 d . . . H10 H 0.3983 0.4951 0.3309 0.018 Uiso 1 1 calc R . . C12 C 0.4827(2) 0.8291(2) 0.3457(2) 0.0191(3) Uani 1 1 d . . . H12 H 0.5571 0.8920 0.3018 0.023 Uiso 1 1 calc R . . C17 C -0.2603(2) 0.3008(2) 1.0339(2) 0.0193(3) Uani 1 1 d . . . H17 H -0.3434 0.3393 1.1120 0.023 Uiso 1 1 calc R . . C19 C -0.1206(2) 0.0973(2) 0.87593(19) 0.0166(3) Uani 1 1 d . . . H19 H -0.1100 -0.0024 0.8487 0.020 Uiso 1 1 calc R . . C18 C -0.2450(2) 0.1527(2) 0.99169(19) 0.0179(3) Uani 1 1 d . . . H18 H -0.3186 0.0909 1.0415 0.022 Uiso 1 1 calc R . . O6 O 0.34006(15) 0.18237(15) 0.04198(14) 0.0254(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01670(7) 0.01811(8) 0.01762(8) -0.00327(5) 0.00414(5) -0.00552(5) N9 0.0166(7) 0.0143(7) 0.0182(7) -0.0010(5) 0.0016(5) -0.0050(5) O2 0.0150(5) 0.0174(6) 0.0224(6) -0.0029(5) 0.0056(5) -0.0081(5) O4 0.0190(6) 0.0237(6) 0.0249(6) -0.0047(5) -0.0014(5) -0.0095(5) O3 0.0176(6) 0.0182(6) 0.0203(6) -0.0028(5) 0.0071(5) -0.0029(5) O5 0.0144(5) 0.0267(7) 0.0234(6) -0.0070(5) 0.0046(5) -0.0068(5) N8 0.0116(6) 0.0165(7) 0.0148(6) 0.0009(5) -0.0009(5) -0.0026(5) N7 0.0104(6) 0.0158(6) 0.0150(6) -0.0006(5) -0.0009(5) -0.0042(5) C13 0.0198(8) 0.0147(8) 0.0241(8) -0.0026(6) -0.0062(7) -0.0042(6) C16 0.0198(8) 0.0188(8) 0.0174(8) -0.0021(6) -0.0032(6) -0.0050(6) C14 0.0151(7) 0.0171(8) 0.0188(8) -0.0039(6) -0.0012(6) -0.0025(6) C15 0.0145(7) 0.0180(8) 0.0174(8) 0.0000(6) -0.0019(6) -0.0074(6) C11 0.0124(7) 0.0203(8) 0.0152(7) 0.0004(6) -0.0004(6) -0.0031(6) C10 0.0144(7) 0.0143(7) 0.0135(7) -0.0016(6) -0.0015(6) -0.0020(6) C12 0.0149(7) 0.0208(8) 0.0217(8) 0.0037(6) -0.0054(6) -0.0081(6) C17 0.0157(8) 0.0235(9) 0.0157(8) -0.0013(6) -0.0001(6) -0.0032(6) C19 0.0143(7) 0.0163(8) 0.0186(8) 0.0016(6) -0.0039(6) -0.0054(6) C18 0.0135(7) 0.0201(8) 0.0185(8) 0.0033(6) -0.0017(6) -0.0067(6) O6 0.0276(7) 0.0304(8) 0.0181(6) -0.0077(5) 0.0066(5) -0.0101(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 O2 2.5225(12) 2_566 ? Ag1 O2 2.3228(12) . ? Ag1 O4 2.5193(12) . ? Ag1 O3 2.2958(12) . ? Ag1 O5 2.4253(13) . ? N9 O4 1.2669(18) . ? N9 O5 1.2674(17) . ? N9 O6 1.2380(18) . ? O2 Ag1 2.5225(12) 2_566 ? O2 N7 1.3312(17) . ? O3 N8 1.3303(17) . ? N8 C15 1.353(2) . ? N8 C19 1.357(2) . ? N7 C14 1.357(2) . ? N7 C10 1.354(2) . ? C13 H13 0.9300 . ? C13 C14 1.380(2) . ? C13 C12 1.386(2) . ? C16 H16 0.9300 . ? C16 C15 1.380(2) . ? C16 C17 1.387(2) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C11 H11 0.9300 . ? C11 C10 1.383(2) . ? C11 C12 1.387(2) . ? C10 H10 0.9300 . ? C12 H12 0.9300 . ? C17 H17 0.9300 . ? C17 C18 1.389(2) . ? C19 H19 0.9300 . ? C19 C18 1.379(2) . ? C18 H18 0.9300 . ? 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 O2 Ag1 O2 82.91(4) . 2_566 ? O2 Ag1 O4 110.58(4) . . ? O2 Ag1 O5 133.33(4) . . ? O4 Ag1 O2 129.37(4) . 2_566 ? O3 Ag1 O2 91.87(4) . 2_566 ? O3 Ag1 O2 110.79(4) . . ? O3 Ag1 O4 123.86(4) . . ? O3 Ag1 O5 113.78(4) . . ? O5 Ag1 O2 82.55(4) . 2_566 ? O5 Ag1 O4 52.10(4) . . ? O4 N9 O5 118.07(13) . . ? O6 N9 O4 121.48(13) . . ? O6 N9 O5 120.45(14) . . ? Ag1 O2 Ag1 97.09(4) . 2_566 ? N7 O2 Ag1 116.52(9) . 2_566 ? N7 O2 Ag1 125.06(9) . . ? N9 O4 Ag1 92.68(9) . . ? N8 O3 Ag1 117.00(9) . . ? N9 O5 Ag1 97.12(9) . . ? O3 N8 C15 120.79(13) . . ? O3 N8 C19 118.52(14) . . ? C15 N8 C19 120.68(14) . . ? O2 N7 C14 118.71(13) . . ? O2 N7 C10 120.23(13) . . ? C10 N7 C14 121.05(14) . . ? C14 C13 H13 119.8 . . ? C14 C13 C12 120.42(16) . . ? C12 C13 H13 119.8 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.38(16) . . ? C17 C16 H16 119.8 . . ? N7 C14 C13 119.77(15) . . ? N7 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? N8 C15 C16 120.16(15) . . ? N8 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.86(15) . . ? C12 C11 H11 120.1 . . ? N7 C10 C11 120.22(15) . . ? N7 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C13 C12 C11 118.67(15) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C16 C17 H17 120.8 . . ? C16 C17 C18 118.34(15) . . ? C18 C17 H17 120.8 . . ? N8 C19 H19 119.8 . . ? N8 C19 C18 120.38(15) . . ? C18 C19 H19 119.8 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.06(15) . . ? C19 C18 H18 120.0 . . ? _database_code_depnum_ccdc_archive 'CCDC 958484' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kb2015 _audit_creation_date 2013-08-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H13 Ag N2 O5 S' _chemical_formula_sum 'C11 H13 Ag N2 O5 S' _chemical_formula_weight 393.16 _chemical_melting_point ? _chemical_oxdiff_formula 'Ag C15 H15 N3 O3 C H3 S O3' 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' Ag Ag -0.8971 1.1015 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 11.6002(2) _cell_length_b 6.90176(12) _cell_length_c 17.1007(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.866(2) _cell_angle_gamma 90.00 _cell_volume 1323.28(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3386 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.0130 _cell_measurement_theta_min 3.6320 _exptl_absorpt_coefficient_mu 1.701 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_unetI/netI 0.0260 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 5428 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.20 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.9980 _diffrn_measured_fraction_theta_max 0.8547 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -17.00 16.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -99.0000 -30.0000 33 #__ type_ start__ end____ width___ exp.time_ 2 omega -88.00 44.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 0.0000 -150.0000 132 #__ type_ start__ end____ width___ exp.time_ 3 omega -26.00 26.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 57.0000 -120.0000 52 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0452835000 _diffrn_orient_matrix_UB_12 0.0511630000 _diffrn_orient_matrix_UB_13 0.0124651000 _diffrn_orient_matrix_UB_21 0.0270019000 _diffrn_orient_matrix_UB_22 -0.0251386000 _diffrn_orient_matrix_UB_23 0.0407820000 _diffrn_orient_matrix_UB_31 0.0349925000 _diffrn_orient_matrix_UB_32 0.0855496000 _diffrn_orient_matrix_UB_33 0.0044740000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 2504 _reflns_number_total 2707 _reflns_odcompleteness_completeness 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.372 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef 0.0019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 183 _refine_ls_number_reflns 2707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0189 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+0.8894P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0444 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C13(H13), C12(H12), C19(H19), C17(H17), C18(H18), C14(H14), C20(H20), C11(H11), C15(H15), C16(H16) 2.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.938903(13) 0.65975(2) 0.225906(9) 0.01282(7) Uani 1 1 d . . . S7 S 0.68005(4) 0.61022(7) 0.09924(3) 0.01188(11) Uani 1 1 d . . . O2 O 0.72401(13) 0.6488(2) 0.18621(9) 0.0173(3) Uani 1 1 d . . . C13 C 1.2011(2) 0.8348(3) 0.00230(13) 0.0163(4) Uani 1 1 d . . . H13 H 1.2438 0.8133 -0.0361 0.020 Uiso 1 1 calc R . . O6 O 0.61437(13) 0.4293(2) 0.08276(9) 0.0163(3) Uani 1 1 d . . . C12 C 1.08848(19) 0.7565(3) -0.00763(12) 0.0149(4) Uani 1 1 d . . . H12 H 1.0547 0.6818 -0.0530 0.018 Uiso 1 1 calc R . . O5 O 0.77349(13) 0.6277(2) 0.05696(10) 0.0210(3) Uani 1 1 d . . . C8 C 0.57686(19) 0.7969(3) 0.06173(13) 0.0171(4) Uani 1 1 d . . . H8A H 0.5172 0.7992 0.0916 0.026 Uiso 1 1 calc R . . H8B H 0.5396 0.7740 0.0056 0.026 Uiso 1 1 calc R . . H8C H 0.6177 0.9191 0.0676 0.026 Uiso 1 1 calc R . . C19 C 1.36680(19) 0.6391(3) 0.27216(13) 0.0170(4) Uani 1 1 d . . . H19 H 1.4046 0.7069 0.3187 0.020 Uiso 1 1 calc R . . C17 C 1.36989(18) 0.4936(3) 0.14670(13) 0.0157(4) Uani 1 1 d . . . H17 H 1.4100 0.4604 0.1080 0.019 Uiso 1 1 calc R . . C18 C 1.42964(18) 0.5879(3) 0.21632(13) 0.0172(5) Uani 1 1 d . . . H18 H 1.5104 0.6166 0.2257 0.021 Uiso 1 1 calc R . . C14 C 1.24891(19) 0.9452(3) 0.07014(13) 0.0160(4) Uani 1 1 d . . . H14 H 1.3240 1.0006 0.0772 0.019 Uiso 1 1 calc R . . O4 O 1.07896(12) 0.4418(2) 0.17862(9) 0.0141(3) Uani 1 1 d . . . N9 N 1.07624(15) 0.8969(2) 0.11625(10) 0.0118(3) Uani 1 1 d . . . N10 N 1.19221(14) 0.4935(2) 0.19076(10) 0.0106(3) Uani 1 1 d . . . C20 C 1.24856(19) 0.5894(3) 0.25863(12) 0.0143(4) Uani 1 1 d . . . H20 H 1.2070 0.6220 0.2966 0.017 Uiso 1 1 calc R . . O3 O 1.01452(13) 0.9269(2) 0.17109(9) 0.0176(3) Uani 1 1 d . . . C11 C 1.02651(18) 0.7897(3) 0.04994(12) 0.0130(4) Uani 1 1 d . . . H11 H 0.9505 0.7384 0.0432 0.016 Uiso 1 1 calc R . . C15 C 1.18600(18) 0.9738(3) 0.12739(12) 0.0141(4) Uani 1 1 d . . . H15 H 1.2192 1.0459 0.1736 0.017 Uiso 1 1 calc R . . C16 C 1.25113(18) 0.4483(3) 0.13428(12) 0.0128(4) Uani 1 1 d . . . H16 H 1.2110 0.3862 0.0868 0.015 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 0.01219(10) 0.01318(10) 0.01451(10) 0.00276(6) 0.00603(6) 0.00127(6) S7 0.0096(2) 0.0146(2) 0.0118(2) -0.00138(19) 0.00327(19) -0.00112(19) O2 0.0154(8) 0.0230(8) 0.0118(7) -0.0018(6) 0.0003(6) 0.0008(6) C13 0.0218(11) 0.0134(10) 0.0171(11) 0.0017(8) 0.0110(9) 0.0029(9) O6 0.0149(7) 0.0141(7) 0.0198(8) -0.0013(6) 0.0041(6) -0.0036(6) C12 0.0221(11) 0.0118(10) 0.0115(10) -0.0012(8) 0.0057(9) 0.0003(9) O5 0.0164(8) 0.0251(8) 0.0260(9) -0.0045(7) 0.0136(7) -0.0048(7) C8 0.0182(11) 0.0174(10) 0.0146(11) 0.0011(9) 0.0022(8) -0.0001(9) C19 0.0186(11) 0.0154(10) 0.0157(11) 0.0001(8) 0.0018(9) -0.0028(9) C17 0.0159(11) 0.0141(10) 0.0202(11) 0.0019(9) 0.0102(9) 0.0009(9) C18 0.0127(10) 0.0176(11) 0.0206(12) 0.0039(9) 0.0029(9) -0.0015(8) C14 0.0152(10) 0.0126(10) 0.0220(11) 0.0015(9) 0.0078(9) 0.0003(8) O4 0.0081(7) 0.0170(7) 0.0181(8) 0.0008(6) 0.0049(6) -0.0009(6) N9 0.0157(9) 0.0109(8) 0.0113(9) 0.0005(7) 0.0078(7) -0.0009(7) N10 0.0106(8) 0.0100(8) 0.0119(8) 0.0029(7) 0.0041(6) 0.0009(7) C20 0.0204(11) 0.0130(9) 0.0103(10) -0.0012(8) 0.0058(8) 0.0019(9) O3 0.0243(8) 0.0161(7) 0.0179(8) -0.0047(6) 0.0153(7) -0.0053(6) C11 0.0136(10) 0.0103(9) 0.0144(10) -0.0003(8) 0.0024(8) -0.0020(8) C15 0.0178(11) 0.0113(9) 0.0126(10) 0.0002(8) 0.0027(8) -0.0028(8) C16 0.0177(10) 0.0092(9) 0.0122(10) -0.0006(8) 0.0055(8) 0.0000(8) _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 O2 2.4108(15) . ? Ag1 O4 2.4961(13) . ? Ag1 O4 2.5828(14) 2_755 ? Ag1 O3 2.3386(14) . ? Ag1 O3 2.3430(14) 2_745 ? S7 O2 1.4676(15) . ? S7 O6 1.4525(15) . ? S7 O5 1.4541(15) . ? S7 C8 1.764(2) . ? C13 H13 0.9300 . ? C13 C12 1.383(3) . ? C13 C14 1.380(3) . ? C12 H12 0.9300 . ? C12 C11 1.379(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C19 H19 0.9300 . ? C19 C18 1.388(3) . ? C19 C20 1.375(3) . ? C17 H17 0.9300 . ? C17 C18 1.378(3) . ? C17 C16 1.375(3) . ? C18 H18 0.9300 . ? C14 H14 0.9300 . ? C14 C15 1.377(3) . ? O4 Ag1 2.5829(14) 2_745 ? O4 N10 1.325(2) . ? N9 O3 1.334(2) . ? N9 C11 1.353(3) . ? N9 C15 1.347(3) . ? N10 C20 1.350(3) . ? N10 C16 1.355(2) . ? C20 H20 0.9300 . ? O3 Ag1 2.3431(14) 2_755 ? C11 H11 0.9300 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? 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 O2 Ag1 O4 87.53(5) . 2_755 ? O2 Ag1 O4 127.00(5) . . ? O4 Ag1 O4 145.43(2) . 2_755 ? O3 Ag1 O2 102.26(5) 2_745 . ? O3 Ag1 O2 112.27(5) . . ? O3 Ag1 O4 94.72(5) 2_745 2_755 ? O3 Ag1 O4 76.02(5) . 2_755 ? O3 Ag1 O4 90.17(5) . . ? O3 Ag1 O4 77.67(5) 2_745 . ? O3 Ag1 O3 143.541(18) . 2_745 ? O2 S7 C8 105.26(9) . . ? O6 S7 O2 112.40(9) . . ? O6 S7 O5 113.30(9) . . ? O6 S7 C8 106.52(9) . . ? O5 S7 O2 112.29(9) . . ? O5 S7 C8 106.35(10) . . ? S7 O2 Ag1 110.88(8) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C14 C13 C12 118.83(19) . . ? C13 C12 H12 120.1 . . ? C11 C12 C13 119.8(2) . . ? C11 C12 H12 120.1 . . ? S7 C8 H8A 109.5 . . ? S7 C8 H8B 109.5 . . ? S7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C20 C19 C18 119.9(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.20(18) . . ? C19 C18 H18 120.7 . . ? C17 C18 C19 118.57(19) . . ? C17 C18 H18 120.7 . . ? C13 C14 H14 119.8 . . ? C15 C14 C13 120.31(19) . . ? C15 C14 H14 119.8 . . ? Ag1 O4 Ag1 94.87(4) . 2_745 ? N10 O4 Ag1 109.95(10) . 2_745 ? N10 O4 Ag1 119.22(11) . . ? O3 N9 C11 118.92(16) . . ? O3 N9 C15 119.87(17) . . ? C15 N9 C11 121.20(17) . . ? O4 N10 C20 120.57(16) . . ? O4 N10 C16 119.15(16) . . ? C20 N10 C16 120.28(17) . . ? C19 C20 H20 119.7 . . ? N10 C20 C19 120.61(18) . . ? N10 C20 H20 119.7 . . ? Ag1 O3 Ag1 106.10(5) . 2_755 ? N9 O3 Ag1 124.96(11) . 2_755 ? N9 O3 Ag1 118.94(11) . . ? C12 C11 H11 120.0 . . ? N9 C11 C12 120.07(19) . . ? N9 C11 H11 120.0 . . ? C14 C15 H15 120.1 . . ? N9 C15 C14 119.82(19) . . ? N9 C15 H15 120.1 . . ? C17 C16 H16 119.8 . . ? N10 C16 C17 120.40(19) . . ? N10 C16 H16 119.8 . . ? _database_code_depnum_ccdc_archive 'CCDC 958485' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kb2011 _audit_creation_date 2013-08-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H15 Ag N3 O3, C F3 O3 S' _chemical_formula_sum 'C16 H15 Ag F3 N3 O6 S' _chemical_formula_weight 542.24 _chemical_melting_point ? _chemical_oxdiff_formula 'Ag C30 H30 N8 O8 C F3 S O3' 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' 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' 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' _space_group_crystal_system tetragonal _space_group_IT_number 88 _space_group_name_H-M_alt 'I 41/a' _space_group_name_Hall '-I 4ad' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y+3/4, x+1/4, z+1/4' 3 '-x, -y+1/2, z' 4 'y+1/4, -x+1/4, z+1/4' 5 'x+1/2, y+1/2, z+1/2' 6 '-y+5/4, x+3/4, z+3/4' 7 '-x+1/2, -y+1, z+1/2' 8 'y+3/4, -x+3/4, z+3/4' 9 '-x, -y, -z' 10 'y-3/4, -x-1/4, -z-1/4' 11 'x, y-1/2, -z' 12 '-y-1/4, x-1/4, -z-1/4' 13 '-x+1/2, -y+1/2, -z+1/2' 14 'y-1/4, -x+1/4, -z+1/4' 15 'x+1/2, y, -z+1/2' 16 '-y+1/4, x+1/4, -z+1/4' _cell_length_a 25.9649(5) _cell_length_b 25.9649(5) _cell_length_c 11.8154(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7965.6(3) _cell_formula_units_Z 16 _cell_measurement_reflns_used 12255 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.9700 _cell_measurement_theta_min 3.2970 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 4320 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 19449 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.92 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.9981 _diffrn_measured_fraction_theta_max 0.8944 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -8.00 22.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -99.0000 90.0000 30 #__ type_ start__ end____ width___ exp.time_ 2 omega -89.00 -25.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 154.0000 141.0000 64 #__ type_ start__ end____ width___ exp.time_ 3 omega -2.00 91.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 0.0000 -90.0000 93 #__ type_ start__ end____ width___ exp.time_ 4 omega -70.00 -44.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -178.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega -3.00 38.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 38.0000 30.0000 41 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0202426000 _diffrn_orient_matrix_UB_12 0.0141466000 _diffrn_orient_matrix_UB_13 -0.0256817000 _diffrn_orient_matrix_UB_21 -0.0103845000 _diffrn_orient_matrix_UB_22 0.0232058000 _diffrn_orient_matrix_UB_23 0.0220563000 _diffrn_orient_matrix_UB_31 0.0151125000 _diffrn_orient_matrix_UB_32 -0.0030077000 _diffrn_orient_matrix_UB_33 0.0495257000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 3749 _reflns_number_total 4065 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.537 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4065 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0201 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+14.3198P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.0512 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C25(H25), C12(H12), C11(H11), C23(H23), C21(H21), C17(H17), C20(H20), C24(H24), C19(H19), C15(H15), C13(H13), C16(H16), C18(H18), C22(H22), C14(H14) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.257073(5) 0.515446(5) 0.838734(11) 0.01909(5) Uani 1 1 d . . . O2 O 0.33724(5) 0.50751(5) 0.72104(11) 0.0230(3) Uani 1 1 d . . . O3 O 0.21597(5) 0.56896(5) 0.70426(10) 0.0189(3) Uani 1 1 d . . . O4 O 0.23473(5) 0.43568(5) 0.73270(10) 0.0182(3) Uani 1 1 d . . . N10 N 0.26246(6) 0.39250(6) 0.73805(12) 0.0161(3) Uani 1 1 d . . . N9 N 0.16504(6) 0.57034(6) 0.70000(12) 0.0161(3) Uani 1 1 d . . . C25 C 0.24470(7) 0.35004(7) 0.68572(15) 0.0187(4) Uani 1 1 d . . . H25 H 0.2139 0.3513 0.6457 0.022 Uiso 1 1 calc R . . C12 C 0.44800(8) 0.56080(9) 0.58694(17) 0.0275(4) Uani 1 1 d . . . H12 H 0.4744 0.5502 0.5391 0.033 Uiso 1 1 calc R . . C11 C 0.41083(7) 0.52616(8) 0.62099(16) 0.0224(4) Uani 1 1 d . . . H11 H 0.4122 0.4922 0.5963 0.027 Uiso 1 1 calc R . . C23 C 0.31782(8) 0.30252(8) 0.75171(17) 0.0251(4) Uani 1 1 d . . . H23 H 0.3362 0.2719 0.7572 0.030 Uiso 1 1 calc R . . C21 C 0.30749(7) 0.39167(7) 0.79591(15) 0.0202(4) Uani 1 1 d . . . H21 H 0.3195 0.4215 0.8305 0.024 Uiso 1 1 calc R . . C17 C 0.08930(8) 0.61156(8) 0.63565(18) 0.0268(4) Uani 1 1 d . . . H17 H 0.0737 0.6377 0.5941 0.032 Uiso 1 1 calc R . . C20 C 0.13644(8) 0.53469(7) 0.75479(16) 0.0213(4) Uani 1 1 d . . . H20 H 0.1526 0.5083 0.7943 0.026 Uiso 1 1 calc R . . N8 N 0.37237(6) 0.54156(6) 0.69015(12) 0.0187(3) Uani 1 1 d . . . C24 C 0.27224(8) 0.30471(7) 0.69148(16) 0.0224(4) Uani 1 1 d . . . H24 H 0.2601 0.2755 0.6547 0.027 Uiso 1 1 calc R . . C19 C 0.08351(8) 0.53725(8) 0.75234(17) 0.0263(4) Uani 1 1 d . . . H19 H 0.0641 0.5127 0.7905 0.032 Uiso 1 1 calc R . . C15 C 0.37018(8) 0.59051(8) 0.72816(16) 0.0246(4) Uani 1 1 d . . . H15 H 0.3437 0.6005 0.7765 0.030 Uiso 1 1 calc R . . C13 C 0.44609(9) 0.61129(9) 0.62382(18) 0.0309(5) Uani 1 1 d . . . H13 H 0.4707 0.6350 0.6005 0.037 Uiso 1 1 calc R . . C16 C 0.14211(8) 0.60810(7) 0.63971(16) 0.0218(4) Uani 1 1 d . . . H16 H 0.1622 0.6319 0.6007 0.026 Uiso 1 1 calc R . . C18 C 0.05923(8) 0.57618(8) 0.69341(18) 0.0266(4) Uani 1 1 d . . . H18 H 0.0235 0.5786 0.6925 0.032 Uiso 1 1 calc R . . C22 C 0.33551(8) 0.34686(8) 0.80366(17) 0.0242(4) Uani 1 1 d . . . H22 H 0.3663 0.3464 0.8438 0.029 Uiso 1 1 calc R . . C14 C 0.40690(9) 0.62576(8) 0.69577(18) 0.0304(5) Uani 1 1 d . . . H14 H 0.4053 0.6594 0.7225 0.036 Uiso 1 1 calc R . . S1 S 0.520624(18) 0.601741(19) 0.29694(4) 0.02400(11) Uani 1 1 d . . . F28 F 0.48890(5) 0.68540(5) 0.39866(11) 0.0385(3) Uani 1 1 d . . . O5 O 0.55103(7) 0.59190(6) 0.39630(15) 0.0414(4) Uani 1 1 d . . . F27 F 0.55515(5) 0.69666(5) 0.29227(13) 0.0436(4) Uani 1 1 d . . . C26 C 0.51093(8) 0.67109(8) 0.30097(18) 0.0280(4) Uani 1 1 d . . . O6 O 0.46947(6) 0.58109(6) 0.30063(13) 0.0324(3) Uani 1 1 d . . . O7 O 0.54692(6) 0.59420(6) 0.19057(15) 0.0405(4) Uani 1 1 d . . . F29 F 0.47993(6) 0.68668(6) 0.21751(12) 0.0473(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02002(8) 0.02308(8) 0.01416(8) -0.00151(5) -0.00164(5) 0.00285(5) O2 0.0198(7) 0.0295(7) 0.0196(6) 0.0060(6) 0.0002(5) -0.0025(6) O3 0.0158(6) 0.0237(7) 0.0173(6) -0.0003(5) -0.0016(5) -0.0001(5) O4 0.0211(6) 0.0163(6) 0.0172(6) -0.0001(5) 0.0001(5) 0.0035(5) N10 0.0183(7) 0.0162(7) 0.0138(7) 0.0010(6) 0.0038(6) 0.0000(6) N9 0.0166(7) 0.0168(7) 0.0150(7) -0.0015(6) -0.0014(6) -0.0012(6) C25 0.0195(9) 0.0204(9) 0.0162(8) 0.0017(7) 0.0020(7) -0.0035(7) C12 0.0199(10) 0.0366(12) 0.0259(10) 0.0028(9) 0.0018(8) 0.0030(9) C11 0.0217(9) 0.0259(10) 0.0197(9) -0.0008(8) 0.0005(7) 0.0051(8) C23 0.0266(10) 0.0198(9) 0.0290(10) 0.0039(8) 0.0036(8) 0.0039(8) C21 0.0204(9) 0.0204(9) 0.0196(9) -0.0014(7) -0.0005(7) -0.0019(7) C17 0.0260(10) 0.0203(10) 0.0342(11) 0.0014(8) -0.0069(9) 0.0041(8) C20 0.0252(10) 0.0198(9) 0.0189(9) 0.0028(7) -0.0013(8) -0.0035(8) N8 0.0174(7) 0.0248(8) 0.0139(7) 0.0046(6) -0.0023(6) 0.0025(6) C24 0.0283(10) 0.0157(9) 0.0232(9) -0.0003(7) 0.0036(8) -0.0035(8) C19 0.0243(10) 0.0287(10) 0.0258(10) 0.0005(8) 0.0014(8) -0.0087(8) C15 0.0279(10) 0.0275(10) 0.0184(9) -0.0013(8) -0.0005(8) 0.0081(8) C13 0.0302(11) 0.0325(11) 0.0301(11) 0.0075(9) -0.0038(9) -0.0063(9) C16 0.0258(10) 0.0171(9) 0.0226(9) 0.0031(7) -0.0013(8) -0.0009(8) C18 0.0186(9) 0.0292(11) 0.0318(10) -0.0062(9) -0.0027(8) -0.0006(8) C22 0.0207(9) 0.0263(10) 0.0254(10) 0.0019(8) -0.0007(8) 0.0021(8) C14 0.0374(12) 0.0228(10) 0.0309(11) 0.0012(8) -0.0054(9) 0.0015(9) S1 0.0180(2) 0.0211(2) 0.0328(3) -0.0047(2) -0.00063(19) 0.00087(18) F28 0.0427(8) 0.0298(7) 0.0429(8) -0.0081(6) 0.0141(6) 0.0056(6) O5 0.0434(10) 0.0256(8) 0.0550(11) -0.0049(7) -0.0213(8) 0.0057(7) F27 0.0352(7) 0.0257(7) 0.0699(10) -0.0049(7) 0.0159(7) -0.0068(6) C26 0.0257(10) 0.0250(10) 0.0334(11) -0.0010(9) 0.0058(9) 0.0029(8) O6 0.0241(7) 0.0333(8) 0.0400(8) -0.0048(7) 0.0031(6) -0.0068(6) O7 0.0291(8) 0.0410(9) 0.0513(10) -0.0190(8) 0.0146(7) -0.0019(7) F29 0.0516(9) 0.0431(8) 0.0473(8) 0.0135(7) -0.0042(7) 0.0160(7) _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 Ag1 3.0191(2) 8_454 ? Ag1 Ag1 3.0190(2) 2 ? Ag1 O2 2.4621(13) 2 ? Ag1 O2 2.5117(13) . ? Ag1 O3 2.3651(12) . ? Ag1 O4 2.4892(12) . ? Ag1 O4 2.3957(12) 2 ? O2 Ag1 2.4621(13) 8_454 ? O2 N8 1.322(2) . ? O3 N9 1.3238(19) . ? O4 Ag1 2.3956(12) 8_454 ? O4 N10 1.3339(19) . ? N10 C25 1.345(2) . ? N10 C21 1.354(2) . ? N9 C20 1.352(2) . ? N9 C16 1.350(2) . ? C25 H25 0.9300 . ? C25 C24 1.379(3) . ? C12 H12 0.9300 . ? C12 C11 1.379(3) . ? C12 C13 1.382(3) . ? C11 H11 0.9300 . ? C11 N8 1.351(2) . ? C23 H23 0.9300 . ? C23 C24 1.382(3) . ? C23 C22 1.383(3) . ? C21 H21 0.9300 . ? C21 C22 1.375(3) . ? C17 H17 0.9300 . ? C17 C16 1.375(3) . ? C17 C18 1.386(3) . ? C20 H20 0.9300 . ? C20 C19 1.376(3) . ? N8 C15 1.349(3) . ? C24 H24 0.9300 . ? C19 H19 0.9300 . ? C19 C18 1.380(3) . ? C15 H15 0.9300 . ? C15 C14 1.376(3) . ? C13 H13 0.9300 . ? C13 C14 1.378(3) . ? C16 H16 0.9300 . ? C18 H18 0.9300 . ? C22 H22 0.9300 . ? C14 H14 0.9300 . ? S1 O5 1.4377(17) . ? S1 C26 1.819(2) . ? S1 O6 1.4331(15) . ? S1 O7 1.4437(16) . ? F28 C26 1.341(2) . ? F27 C26 1.330(2) . ? C26 F29 1.336(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag1 Ag1 Ag1 163.197(5) 2 8_454 ? O2 Ag1 Ag1 134.13(3) . 2 ? O2 Ag1 Ag1 53.38(3) 2 2 ? O2 Ag1 Ag1 51.88(3) . 8_454 ? O2 Ag1 Ag1 141.16(3) 2 8_454 ? O2 Ag1 O2 122.76(2) 2 . ? O2 Ag1 O4 156.02(4) 2 . ? O3 Ag1 Ag1 59.27(3) . 8_454 ? O3 Ag1 Ag1 127.75(3) . 2 ? O3 Ag1 O2 92.88(4) . . ? O3 Ag1 O2 84.97(4) . 2 ? O3 Ag1 O4 92.61(4) . . ? O3 Ag1 O4 162.28(4) . 2 ? O4 Ag1 Ag1 50.44(3) . 8_454 ? O4 Ag1 Ag1 125.84(3) 2 8_454 ? O4 Ag1 Ag1 53.24(3) 2 2 ? O4 Ag1 Ag1 112.79(3) . 2 ? O4 Ag1 O2 81.46(4) 2 . ? O4 Ag1 O2 81.15(4) . . ? O4 Ag1 O2 84.07(4) 2 2 ? O4 Ag1 O4 102.999(19) 2 . ? Ag1 O2 Ag1 74.74(4) 8_454 . ? N8 O2 Ag1 132.06(11) . . ? N8 O2 Ag1 116.75(10) . 8_454 ? N9 O3 Ag1 119.49(10) . . ? Ag1 O4 Ag1 76.32(4) 8_454 . ? N10 O4 Ag1 123.34(10) . . ? N10 O4 Ag1 112.05(9) . 8_454 ? O4 N10 C25 118.81(15) . . ? O4 N10 C21 120.21(15) . . ? C25 N10 C21 120.98(16) . . ? O3 N9 C20 120.79(15) . . ? O3 N9 C16 118.70(15) . . ? C16 N9 C20 120.51(16) . . ? N10 C25 H25 120.0 . . ? N10 C25 C24 119.93(17) . . ? C24 C25 H25 120.0 . . ? C11 C12 H12 120.0 . . ? C11 C12 C13 120.09(19) . . ? C13 C12 H12 120.0 . . ? C12 C11 H11 120.0 . . ? N8 C11 C12 120.04(18) . . ? N8 C11 H11 120.0 . . ? C24 C23 H23 120.7 . . ? C24 C23 C22 118.60(18) . . ? C22 C23 H23 120.7 . . ? N10 C21 H21 119.9 . . ? N10 C21 C22 120.25(17) . . ? C22 C21 H21 119.9 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.10(19) . . ? C18 C17 H17 120.0 . . ? N9 C20 H20 119.8 . . ? N9 C20 C19 120.36(18) . . ? C19 C20 H20 119.8 . . ? O2 N8 C11 118.63(16) . . ? O2 N8 C15 120.61(16) . . ? C15 N8 C11 120.76(17) . . ? C25 C24 C23 120.31(18) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C20 C19 H19 119.9 . . ? C20 C19 C18 120.15(19) . . ? C18 C19 H19 119.9 . . ? N8 C15 H15 119.8 . . ? N8 C15 C14 120.32(19) . . ? C14 C15 H15 119.8 . . ? C12 C13 H13 120.7 . . ? C14 C13 C12 118.7(2) . . ? C14 C13 H13 120.7 . . ? N9 C16 C17 120.37(18) . . ? N9 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C17 C18 H18 120.8 . . ? C19 C18 C17 118.48(19) . . ? C19 C18 H18 120.8 . . ? C23 C22 H22 120.0 . . ? C21 C22 C23 119.92(18) . . ? C21 C22 H22 120.0 . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O5 S1 C26 103.34(10) . . ? O5 S1 O7 115.28(11) . . ? O6 S1 O5 114.69(10) . . ? O6 S1 C26 103.97(10) . . ? O6 S1 O7 114.46(10) . . ? O7 S1 C26 102.86(10) . . ? F28 C26 S1 110.86(14) . . ? F27 C26 S1 111.88(14) . . ? F27 C26 F28 107.23(17) . . ? F27 C26 F29 108.17(18) . . ? F29 C26 S1 111.36(15) . . ? F29 C26 F28 107.13(17) . . ? _database_code_depnum_ccdc_archive 'CCDC 958486' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_nrb98 _audit_creation_date 2013-08-02 _audit_creation_method ; Olex2 1.2-beta (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ; tris(pyridine-N-oxide) silver bistriflimide ; _chemical_name_systematic ; tris(pyridine-N-oxide) silver bis(trifluoromethylsulfonyl)imide ; _chemical_formula_moiety 'C15 H15 Ag N3 O3, C2 F6 N O4 S2' _chemical_formula_sum 'C17 H15 Ag F6 N4 O7 S2' _chemical_formula_weight 673.32 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 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' 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' _space_group_crystal_system trigonal _space_group_IT_number 159 _space_group_name_H-M_alt 'P 3 1 c' _space_group_name_Hall 'P 3 -2c' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 'y, x, z+1/2' 5 '-x, -x+y, z+1/2' 6 'x-y, -y, z+1/2' _cell_length_a 25.4018(11) _cell_length_b 25.4018(11) _cell_length_c 12.5772(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7028.2(5) _cell_formula_units_Z 12 _cell_measurement_reflns_used 7110 _cell_measurement_temperature 99.97(12) _cell_measurement_theta_max 29.0782 _cell_measurement_theta_min 2.7721 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4008 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0341 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 17457 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 29.14 _diffrn_reflns_theta_min 2.78 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.885 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -20.00 25.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -16.9951 -99.0000 0.0000 45 #__ type_ start__ end____ width___ exp.time_ 2 omega 13.00 89.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.7138 38.0000 0.0000 76 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0270203000 _diffrn_orient_matrix_UB_12 0.0217419000 _diffrn_orient_matrix_UB_13 -0.0260236000 _diffrn_orient_matrix_UB_21 -0.0002380000 _diffrn_orient_matrix_UB_22 -0.0234378000 _diffrn_orient_matrix_UB_23 -0.0309134000 _diffrn_orient_matrix_UB_31 -0.0176898000 _diffrn_orient_matrix_UB_32 0.0041105000 _diffrn_orient_matrix_UB_33 -0.0392301000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 6650 _reflns_number_total 8083 _reflns_odcompleteness_completeness 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.736 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.082 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 818 _refine_ls_number_reflns 8083 _refine_ls_number_restraints 725 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0324 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+5.8297P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0659 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.6667 -0.3333 -0.92873(4) 0.01700(13) Uani 1 3 d S . . Ag2 Ag -0.6667 -0.3333 -0.67056(4) 0.01674(12) Uani 1 3 d S . . Ag3 Ag -0.6667 -0.3333 -0.42366(5) 0.01936(13) Uani 1 3 d S . . Ag4 Ag -0.6667 -0.3333 -0.16919(4) 0.01791(13) Uani 1 3 d S . . N13 N -0.5594(3) -0.2100(3) -1.0487(4) 0.0193(14) Uani 0.778(4) 1 d PD . 1 C19 C -0.5342(4) -0.1490(5) -1.0658(7) 0.028(2) Uani 0.778(4) 1 d P . 1 H19 H -0.5586 -0.1317 -1.0759 0.033 Uiso 0.778(4) 1 calc PR . 1 C20 C -0.4705(5) -0.1130(6) -1.0678(10) 0.027(2) Uani 0.778(4) 1 d P . 1 H20 H -0.4526 -0.0713 -1.0787 0.033 Uiso 0.778(4) 1 calc PR . 1 C21 C -0.4334(4) -0.1386(3) -1.0537(8) 0.029(2) Uani 0.778(4) 1 d P . 1 H21 H -0.3912 -0.1146 -1.0548 0.035 Uiso 0.778(4) 1 calc PR . 1 C22 C -0.4620(3) -0.2021(4) -1.0377(6) 0.0227(18) Uani 0.778(4) 1 d P . 1 H22 H -0.4386 -0.2205 -1.0287 0.027 Uiso 0.778(4) 1 calc PR . 1 C23 C -0.5250(3) -0.2370(3) -1.0354(6) 0.0216(17) Uani 0.778(4) 1 d P . 1 H23 H -0.5437 -0.2787 -1.0247 0.026 Uiso 0.778(4) 1 calc PR . 1 N13' N -0.5397(11) -0.2335(7) -1.054(2) 0.0193(14) Uani 0.222(4) 1 d PD . 2 C19' C -0.4830(16) -0.2117(19) -1.035(3) 0.028(2) Uani 0.222(4) 1 d P . 2 H19' H -0.4691 -0.2377 -1.0141 0.033 Uiso 0.222(4) 1 calc PR . 2 C20' C -0.4454(18) -0.1551(17) -1.045(3) 0.027(2) Uani 0.222(4) 1 d P . 2 H20' H -0.4043 -0.1415 -1.0338 0.033 Uiso 0.222(4) 1 calc PR . 2 C21' C -0.460(2) -0.118(2) -1.069(4) 0.029(2) Uani 0.222(4) 1 d P . 2 H21' H -0.4320 -0.0770 -1.0775 0.035 Uiso 0.222(4) 1 calc PR . 2 C22' C -0.5193(17) -0.140(2) -1.083(3) 0.0227(18) Uani 0.222(4) 1 d P . 2 H22' H -0.5326 -0.1120 -1.0956 0.027 Uiso 0.222(4) 1 calc PR . 2 C23' C -0.5599(15) -0.1975(14) -1.080(2) 0.0216(17) Uani 0.222(4) 1 d P . 2 H23' H -0.6007 -0.2119 -1.0951 0.026 Uiso 0.222(4) 1 calc PR . 2 N14 N -0.5525(2) -0.3309(2) -0.7998(4) 0.0145(11) Uani 0.783(4) 1 d PD . 1 C24 C -0.4916(2) -0.2992(3) -0.8096(4) 0.0203(12) Uani 0.783(4) 1 d P . 1 H24 H -0.4717 -0.2571 -0.8154 0.024 Uiso 0.783(4) 1 calc PR . 1 C25 C -0.4590(3) -0.3287(3) -0.8109(5) 0.0236(13) Uani 0.783(4) 1 d P . 1 H25 H -0.4170 -0.3067 -0.8196 0.028 Uiso 0.783(4) 1 calc PR . 1 C26 C -0.4879(4) -0.3907(3) -0.7995(10) 0.0218(17) Uani 0.783(4) 1 d P . 1 H26 H -0.4657 -0.4107 -0.7962 0.026 Uiso 0.783(4) 1 calc PR . 1 C27 C -0.5510(3) -0.4229(3) -0.7929(5) 0.0273(14) Uani 0.783(4) 1 d P . 1 H27 H -0.5715 -0.4651 -0.7887 0.033 Uiso 0.783(4) 1 calc PR . 1 C28 C -0.5831(3) -0.3925(3) -0.7926(5) 0.0194(13) Uani 0.783(4) 1 d P . 1 H28 H -0.6253 -0.4138 -0.7876 0.023 Uiso 0.783(4) 1 calc PR . 1 C29 C -0.7149(2) -0.1984(2) -0.5573(4) 0.0257(11) Uani 1 1 d . . . H29 H -0.6765 -0.1640 -0.5542 0.031 Uiso 1 1 calc R . . C30 C -0.7658(2) -0.1926(2) -0.5654(4) 0.0316(12) Uani 1 1 d . . . H30 H -0.7617 -0.1541 -0.5669 0.038 Uiso 1 1 calc R . . C31 C -0.8226(2) -0.2433(2) -0.5711(4) 0.0266(11) Uani 1 1 d . . . H31 H -0.8570 -0.2395 -0.5781 0.032 Uiso 1 1 calc R . . C32 C -0.8276(2) -0.3000(2) -0.5664(4) 0.0241(10) Uani 1 1 d . . . H32 H -0.8658 -0.3348 -0.5691 0.029 Uiso 1 1 calc R . . C33 C -0.77656(19) -0.3052(2) -0.5579(3) 0.0185(9) Uani 1 1 d . . . H33 H -0.7801 -0.3434 -0.5550 0.022 Uiso 1 1 calc R . . C34 C -0.7928(2) -0.4626(2) -0.2875(4) 0.0264(11) Uani 1 1 d . . . H34 H -0.7911 -0.4252 -0.2849 0.032 Uiso 1 1 calc R . . C35 C -0.8482(2) -0.5156(2) -0.2839(4) 0.0282(12) Uani 1 1 d . . . H35 H -0.8839 -0.5139 -0.2782 0.034 Uiso 1 1 calc R . . C36 C -0.8507(2) -0.5711(2) -0.2888(4) 0.0280(11) Uani 1 1 d . . . H36 H -0.8879 -0.6071 -0.2866 0.034 Uiso 1 1 calc R . . C37 C -0.7967(2) -0.5723(2) -0.2972(4) 0.0264(11) Uani 1 1 d . . . H37 H -0.7974 -0.6092 -0.3014 0.032 Uiso 1 1 calc R . . C38 C -0.7424(2) -0.5186(2) -0.2993(3) 0.0200(10) Uani 1 1 d . . . H38 H -0.7063 -0.5194 -0.3038 0.024 Uiso 1 1 calc R . . N15 N -0.72101(16) -0.25463(16) -0.5538(3) 0.0171(8) Uani 1 1 d . . . N16 N -0.74062(16) -0.46507(16) -0.2949(3) 0.0187(8) Uani 1 1 d . . . O7 O -0.61976(17) -0.24341(17) -1.0443(3) 0.0209(8) Uani 0.778(4) 1 d PD . 1 O8 O -0.58285(16) -0.30026(17) -0.7969(3) 0.0184(8) Uani 0.783(4) 1 d PD . 1 O9 O -0.67113(13) -0.25894(14) -0.5475(2) 0.0223(7) Uani 1 1 d . . . O10 O -0.68696(14) -0.41438(14) -0.2965(2) 0.0225(7) Uani 1 1 d . . . Ag5 Ag 0.0000 0.0000 -0.63339(4) 0.01726(14) Uani 1 3 d S . . Ag6 Ag 0.0000 0.0000 -0.37657(5) 0.01708(14) Uani 1 3 d S . . C39 C -0.1275(2) -0.0030(2) -0.5106(3) 0.0172(10) Uani 1 1 d . . . H39 H -0.0898 0.0322 -0.5058 0.021 Uiso 1 1 calc R . . C40 C -0.1794(2) 0.0010(2) -0.5176(3) 0.0198(10) Uani 1 1 d . . . H40 H -0.1766 0.0389 -0.5165 0.024 Uiso 1 1 calc R . . C41 C -0.2355(2) -0.0509(2) -0.5264(4) 0.0252(11) Uani 1 1 d . . . H41 H -0.2708 -0.0485 -0.5322 0.030 Uiso 1 1 calc R . . C42 C -0.2380(2) -0.1063(2) -0.5262(4) 0.0238(10) Uani 1 1 d . . . H42 H -0.2754 -0.1419 -0.5311 0.029 Uiso 1 1 calc R . . C43 C -0.1855(2) -0.1095(2) -0.5186(3) 0.0178(9) Uani 1 1 d . . . H43 H -0.1874 -0.1470 -0.5190 0.021 Uiso 1 1 calc R . . C44 C 0.0408(2) -0.1408(2) -0.2596(3) 0.0202(10) Uani 1 1 d . . . H44 H 0.0016 -0.1740 -0.2645 0.024 Uiso 1 1 calc R . . C45 C 0.0894(2) -0.1501(2) -0.2572(4) 0.0259(11) Uani 1 1 d . . . H45 H 0.0832 -0.1893 -0.2609 0.031 Uiso 1 1 calc R . . C46 C 0.1477(2) -0.1009(2) -0.2492(4) 0.0270(11) Uani 1 1 d . . . H46 H 0.1811 -0.1066 -0.2455 0.032 Uiso 1 1 calc R . . C47 C 0.1553(2) -0.0426(2) -0.2468(4) 0.0242(11) Uani 1 1 d . . . H47 H 0.1941 -0.0088 -0.2436 0.029 Uiso 1 1 calc R . . C48 C 0.1056(2) -0.0354(2) -0.2490(4) 0.0229(10) Uani 1 1 d . . . H48 H 0.1106 0.0035 -0.2464 0.027 Uiso 1 1 calc R . . N17 N -0.13107(17) -0.05750(18) -0.5106(3) 0.0186(8) Uani 1 1 d . . . N18 N 0.04887(16) -0.08433(17) -0.2551(3) 0.0171(8) Uani 1 1 d . . . O11 O -0.08081(14) -0.06166(15) -0.5049(2) 0.0204(7) Uani 1 1 d . . . O12 O 0.00011(13) -0.07754(14) -0.2555(2) 0.0186(7) Uani 1 1 d . . . C49 C -0.7018(5) -0.8658(5) -0.3272(6) 0.0327(9) Uani 0.402(17) 1 d PDU A 1 F50 F -0.7076(8) -0.9069(6) -0.2535(10) 0.0364(11) Uani 0.402(17) 1 d PDU A 1 F51 F -0.6450(5) -0.8186(7) -0.313(2) 0.0357(10) Uani 0.402(17) 1 d PDU A 1 F52 F -0.7405(5) -0.8474(7) -0.2956(11) 0.0404(11) Uani 0.402(17) 1 d PDU A 1 S53 S -0.71318(8) -0.89547(7) -0.45805(14) 0.0222(3) Uani 0.789(3) 1 d PDU A 1 O54 O -0.6868(2) -0.8420(3) -0.5222(6) 0.0381(11) Uani 0.789(3) 1 d PDU A 1 O55 O -0.77757(17) -0.93680(18) -0.4648(3) 0.0296(8) Uani 0.789(3) 1 d PDU A 1 N56 N -0.6705(2) -0.92314(19) -0.4534(4) 0.0268(7) Uani 0.789(3) 1 d PDU A 1 S57 S -0.6890(2) -0.9917(2) -0.4587(7) 0.0218(6) Uani 0.789(3) 1 d PDU A 1 O58 O -0.6503(3) -1.0028(2) -0.3915(4) 0.0273(10) Uani 0.789(3) 1 d PU A 1 O59 O -0.7518(3) -1.0364(2) -0.4632(6) 0.0331(12) Uani 0.789(3) 1 d PU A 1 C60 C -0.6625(5) -0.9958(4) -0.5889(8) 0.0235(17) Uani 0.789(3) 1 d P A 1 F61 F -0.6018(2) -0.9561(2) -0.6012(4) 0.0397(11) Uani 0.789(3) 1 d P A 1 F62 F -0.6718(2) -1.0503(2) -0.6151(4) 0.0354(11) Uani 0.789(3) 1 d P A 1 F63 F -0.6889(3) -0.9782(2) -0.6648(6) 0.0379(14) Uani 0.789(3) 1 d P A 1 C49' C -0.7017(5) -0.8604(4) -0.3183(7) 0.0327(9) Uani 0.381(17) 1 d PDU A 2 F50' F -0.7212(6) -0.9017(5) -0.2446(8) 0.0364(11) Uani 0.381(17) 1 d PDU A 2 F51' F -0.6426(5) -0.8204(8) -0.305(2) 0.0357(10) Uani 0.381(17) 1 d PDU A 2 F52' F -0.7311(5) -0.8292(6) -0.3271(11) 0.0404(11) Uani 0.381(17) 1 d PDU A 2 S53' S -0.6850(3) -0.8809(3) -0.4415(5) 0.0222(3) Uani 0.211(3) 1 d PDU A 2 O54' O -0.7048(9) -0.8507(12) -0.514(3) 0.0381(11) Uani 0.211(3) 1 d PDU A 2 O55' O -0.6206(4) -0.8551(6) -0.4264(12) 0.0296(8) Uani 0.211(3) 1 d PDU A 2 N56' N -0.7203(6) -0.9511(4) -0.4685(15) 0.0268(7) Uani 0.211(3) 1 d PDU A 2 S57' S -0.6980(11) -1.0003(9) -0.459(3) 0.0218(6) Uani 0.211(3) 1 d P A 2 O58' O -0.6540(11) -0.9826(9) -0.3742(15) 0.0273(10) Uani 0.211(3) 1 d P A 2 O59' O -0.7527(11) -1.0570(8) -0.460(3) 0.0331(12) Uani 0.211(3) 1 d P A 2 C60' C -0.655(3) -0.9799(19) -0.606(4) 0.0235(17) Uani 0.211(3) 1 d P A 2 F61' F -0.6097(11) -0.9387(10) -0.596(2) 0.0397(11) Uani 0.211(3) 1 d P A 2 F62' F -0.6487(9) -1.0342(10) -0.5915(17) 0.0354(11) Uani 0.211(3) 1 d P A 2 F63' F -0.7010(16) -0.9995(11) -0.660(3) 0.0379(14) Uani 0.211(3) 1 d P A 2 C49" C -0.7107(6) -0.8793(6) -0.3185(8) 0.0327(9) Uani 0.218(3) 1 d PD B 3 F50" F -0.7696(6) -0.8949(7) -0.3064(10) 0.0364(11) Uani 0.218(3) 1 d PD B 3 F51" F -0.7032(10) -0.9161(9) -0.2491(16) 0.0357(10) Uani 0.218(3) 1 d PD B 3 F52" F -0.6822(6) -0.8228(6) -0.2741(11) 0.0404(11) Uani 0.218(3) 1 d PD B 3 O7' O -0.5772(6) -0.2933(6) -1.0540(11) 0.0209(8) Uani 0.222(4) 1 d PD . 2 O8' O -0.6576(6) -0.4015(6) -0.8095(10) 0.0184(8) Uani 0.217(4) 1 d PD . 2 N14' N -0.6048(7) -0.4014(7) -0.8072(17) 0.0145(11) Uani 0.217(4) 1 d PD . 2 C24' C -0.5519(10) -0.3501(11) -0.8254(19) 0.0203(12) Uani 0.217(4) 1 d PD . 2 H24' H -0.5517 -0.3143 -0.8413 0.024 Uiso 0.217(4) 1 calc PR . 2 C25' C -0.4977(10) -0.3504(10) -0.8208(17) 0.0236(13) Uani 0.217(4) 1 d PD . 2 H25' H -0.4607 -0.3143 -0.8257 0.028 Uiso 0.217(4) 1 calc PR . 2 C26' C -0.4997(18) -0.4051(9) -0.809(4) 0.0218(17) Uani 0.217(4) 1 d PD . 2 H26' H -0.4648 -0.4079 -0.8162 0.026 Uiso 0.217(4) 1 calc PR . 2 C27' C -0.5547(9) -0.4557(11) -0.7856(19) 0.0273(14) Uani 0.217(4) 1 d PD . 2 H27' H -0.5554 -0.4914 -0.7663 0.033 Uiso 0.217(4) 1 calc PR . 2 C28' C -0.6085(9) -0.4554(9) -0.7900(15) 0.0194(13) Uani 0.217(4) 1 d PD . 2 H28' H -0.6458 -0.4909 -0.7815 0.023 Uiso 0.217(4) 1 calc PR . 2 C64 C -0.5156(10) -0.4763(10) -0.4877(19) 0.0305(18) Uani 0.725(3) 1 d PU C 1 F65 F -0.4770(6) -0.4934(4) -0.5006(9) 0.0312(15) Uani 0.725(3) 1 d PU C 1 F66 F -0.4830(3) -0.4148(3) -0.4746(5) 0.0385(13) Uani 0.725(3) 1 d PU C 1 F67 F -0.5483(2) -0.4867(2) -0.5757(4) 0.0453(12) Uani 0.725(3) 1 d PU C 1 S68 S -0.56109(18) -0.5083(2) -0.3681(4) 0.0217(6) Uani 0.725(3) 1 d PU C 1 O69 O -0.6052(6) -0.4846(6) -0.3629(6) 0.0235(15) Uani 0.725(3) 1 d PU C 1 O70 O -0.5225(4) -0.4931(3) -0.2848(8) 0.0365(17) Uani 0.725(3) 1 d PU C 1 N71 N -0.5932(2) -0.5768(2) -0.4094(5) 0.0260(11) Uani 0.725(3) 1 d PU C 1 S72 S -0.6534(2) -0.6307(3) -0.3706(5) 0.0215(7) Uani 0.725(3) 1 d PU C 1 O73 O -0.6771(3) -0.6764(3) -0.4526(5) 0.0361(14) Uani 0.725(3) 1 d PU C 1 O74 O -0.6998(9) -0.6172(10) -0.3260(12) 0.035(2) Uani 0.725(3) 1 d PU C 1 C75 C -0.6333(4) -0.6653(3) -0.2653(6) 0.0344(15) Uani 0.725(3) 1 d PU C 1 F76 F -0.6810(3) -0.7135(2) -0.2264(4) 0.0544(13) Uani 0.725(3) 1 d PU C 1 F77 F -0.6042(2) -0.6259(2) -0.1881(3) 0.0484(11) Uani 0.725(3) 1 d PU C 1 F78 F -0.5953(3) -0.6835(3) -0.3007(4) 0.0446(13) Uani 0.725(3) 1 d PU C 1 C64' C -0.522(3) -0.483(3) -0.479(5) 0.0305(18) Uani 0.275(3) 1 d PU C 2 F65' F -0.4784(17) -0.5058(13) -0.483(3) 0.0312(15) Uani 0.275(3) 1 d PU C 2 F66' F -0.4992(9) -0.4284(9) -0.5055(15) 0.0385(13) Uani 0.275(3) 1 d PU C 2 F67' F -0.5627(6) -0.5191(7) -0.5564(10) 0.0453(12) Uani 0.275(3) 1 d PU C 2 S68' S -0.5703(6) -0.5030(6) -0.3596(12) 0.0217(6) Uani 0.275(3) 1 d PU C 2 O69' O -0.6003(19) -0.4804(19) -0.388(2) 0.0235(15) Uani 0.275(3) 1 d PU C 2 O70' O -0.5139(13) -0.4719(9) -0.277(3) 0.0365(17) Uani 0.275(3) 1 d PU C 2 N71' N -0.5902(7) -0.5736(7) -0.3404(13) 0.0260(11) Uani 0.275(3) 1 d PU C 2 S72' S -0.6621(7) -0.6250(8) -0.3700(15) 0.0215(7) Uani 0.275(3) 1 d PU C 2 O73' O -0.6659(7) -0.6430(7) -0.4782(12) 0.0361(14) Uani 0.275(3) 1 d PU C 2 O74' O -0.693(3) -0.613(3) -0.305(4) 0.035(2) Uani 0.275(3) 1 d PU C 2 C75' C -0.6575(11) -0.6884(9) -0.2949(16) 0.0344(15) Uani 0.275(3) 1 d PU C 2 F76' F -0.6521(8) -0.6784(7) -0.1934(11) 0.0544(13) Uani 0.275(3) 1 d PU C 2 F77' F -0.7090(6) -0.7369(5) -0.3142(9) 0.0484(11) Uani 0.275(3) 1 d PU C 2 F78' F -0.6113(9) -0.6950(9) -0.3346(14) 0.0446(13) Uani 0.275(3) 1 d PU C 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 Ag1 0.01622(17) 0.01622(17) 0.0186(3) 0.000 0.000 0.00811(9) Ag2 0.01501(18) 0.01501(18) 0.0202(3) 0.000 0.000 0.00750(9) Ag3 0.01689(18) 0.01689(18) 0.0243(3) 0.000 0.000 0.00845(9) Ag4 0.01612(18) 0.01612(18) 0.0215(3) 0.000 0.000 0.00806(9) N13 0.022(3) 0.016(3) 0.010(3) -0.001(2) 0.001(2) 0.002(2) C19 0.024(5) 0.034(5) 0.028(5) 0.000(4) 0.006(3) 0.016(5) C20 0.028(6) 0.020(4) 0.032(4) 0.003(3) 0.010(4) 0.010(3) C21 0.016(4) 0.019(5) 0.035(4) -0.011(4) -0.001(3) -0.004(3) C22 0.018(4) 0.026(4) 0.019(3) 0.003(3) 0.001(3) 0.007(4) C23 0.023(4) 0.019(3) 0.022(4) 0.001(3) 0.004(3) 0.010(3) N13' 0.022(3) 0.016(3) 0.010(3) -0.001(2) 0.001(2) 0.002(2) C19' 0.024(5) 0.034(5) 0.028(5) 0.000(4) 0.006(3) 0.016(5) C20' 0.028(6) 0.020(4) 0.032(4) 0.003(3) 0.010(4) 0.010(3) C21' 0.016(4) 0.019(5) 0.035(4) -0.011(4) -0.001(3) -0.004(3) C22' 0.018(4) 0.026(4) 0.019(3) 0.003(3) 0.001(3) 0.007(4) C23' 0.023(4) 0.019(3) 0.022(4) 0.001(3) 0.004(3) 0.010(3) N14 0.015(2) 0.016(3) 0.013(2) 0.0016(19) 0.0004(19) 0.008(2) C24 0.017(3) 0.023(3) 0.022(3) -0.001(2) 0.001(2) 0.010(3) C25 0.021(3) 0.027(3) 0.025(3) 0.002(3) 0.005(3) 0.013(3) C26 0.020(5) 0.023(4) 0.027(4) -0.010(4) -0.007(4) 0.015(4) C27 0.030(3) 0.021(4) 0.032(3) 0.000(3) 0.000(3) 0.014(3) C28 0.020(3) 0.019(3) 0.022(3) 0.002(2) 0.002(3) 0.012(3) C29 0.029(3) 0.017(2) 0.031(2) 0.006(2) 0.006(2) 0.011(2) C30 0.047(3) 0.029(3) 0.032(3) 0.003(2) 0.002(2) 0.029(3) C31 0.024(3) 0.033(3) 0.032(3) 0.005(2) 0.002(2) 0.021(2) C32 0.022(3) 0.027(3) 0.024(2) 0.002(2) 0.000(2) 0.012(2) C33 0.017(2) 0.014(2) 0.022(2) -0.0001(18) -0.0001(19) 0.0059(19) C34 0.026(3) 0.024(3) 0.033(3) -0.001(2) -0.001(2) 0.015(2) C35 0.017(2) 0.028(3) 0.036(3) 0.006(2) 0.000(2) 0.009(2) C36 0.023(3) 0.023(3) 0.028(3) 0.004(2) 0.002(2) 0.004(2) C37 0.030(3) 0.019(2) 0.027(2) 0.002(2) 0.001(2) 0.011(2) C38 0.022(2) 0.023(2) 0.015(2) 0.0019(18) 0.0008(19) 0.011(2) N15 0.018(2) 0.0184(19) 0.0181(18) -0.0013(16) -0.0013(16) 0.0116(17) N16 0.017(2) 0.0138(18) 0.0221(18) 0.0000(16) -0.0017(16) 0.0058(16) O7 0.014(2) 0.019(2) 0.0255(18) -0.0021(17) 0.0004(15) 0.0043(17) O8 0.0144(19) 0.020(2) 0.0240(18) -0.0017(16) -0.0008(16) 0.0114(17) O9 0.0162(17) 0.0232(18) 0.0310(17) -0.0036(15) -0.0021(13) 0.0124(14) O10 0.0163(16) 0.0162(17) 0.0282(17) -0.0004(14) -0.0013(14) 0.0031(14) Ag5 0.0181(2) 0.0181(2) 0.0155(3) 0.000 0.000 0.00907(11) Ag6 0.0183(2) 0.0183(2) 0.0146(3) 0.000 0.000 0.00915(10) C39 0.018(2) 0.018(2) 0.016(2) 0.0008(17) 0.0004(18) 0.0098(19) C40 0.026(3) 0.022(3) 0.016(2) -0.0005(18) -0.0016(19) 0.016(2) C41 0.025(3) 0.036(3) 0.024(2) -0.001(2) -0.006(2) 0.022(3) C42 0.020(2) 0.023(3) 0.026(2) -0.0027(19) -0.0058(19) 0.009(2) C43 0.015(2) 0.016(2) 0.020(2) -0.0018(18) -0.0040(17) 0.006(2) C44 0.020(2) 0.020(2) 0.016(2) -0.0032(18) 0.0026(18) 0.007(2) C45 0.032(3) 0.024(3) 0.026(2) -0.001(2) 0.005(2) 0.018(2) C46 0.026(3) 0.036(3) 0.027(3) -0.003(2) -0.003(2) 0.022(2) C47 0.020(3) 0.023(3) 0.025(2) -0.005(2) -0.004(2) 0.007(2) C48 0.023(3) 0.021(3) 0.026(2) -0.005(2) -0.002(2) 0.011(2) N17 0.016(2) 0.025(2) 0.0154(17) -0.0006(16) -0.0028(15) 0.0110(18) N18 0.0168(19) 0.020(2) 0.0144(18) -0.0024(15) -0.0003(15) 0.0095(16) O11 0.0160(17) 0.0253(18) 0.0239(16) -0.0008(14) -0.0012(13) 0.0132(15) O12 0.0170(17) 0.0226(17) 0.0181(15) 0.0000(13) 0.0007(12) 0.0111(14) C49 0.0326(17) 0.028(2) 0.0378(15) -0.0151(14) -0.0057(14) 0.0155(16) F50 0.034(3) 0.051(3) 0.0278(11) -0.006(2) 0.0103(15) 0.0249(17) F51 0.0304(15) 0.0341(19) 0.041(3) -0.0174(15) -0.0134(14) 0.0150(13) F52 0.036(2) 0.050(4) 0.042(3) -0.015(2) 0.000(2) 0.027(2) S53 0.0201(9) 0.0173(8) 0.0271(7) -0.0034(6) -0.0017(7) 0.0078(7) O54 0.032(2) 0.0216(19) 0.0460(17) 0.0087(17) -0.015(3) 0.0022(19) O55 0.0213(13) 0.0210(18) 0.040(2) -0.0048(15) -0.0046(12) 0.0061(11) N56 0.0234(12) 0.0175(11) 0.0370(16) -0.0094(12) -0.0034(13) 0.0083(10) S57 0.0224(19) 0.0153(16) 0.0249(6) -0.0026(15) -0.0012(16) 0.0074(13) O58 0.037(2) 0.029(3) 0.017(2) -0.0032(19) -0.0038(19) 0.017(2) O59 0.0201(16) 0.0204(18) 0.049(2) -0.001(3) 0.0062(16) 0.0025(19) C60 0.034(4) 0.024(6) 0.021(4) 0.013(3) 0.010(3) 0.020(5) F61 0.032(2) 0.043(3) 0.050(2) 0.019(2) 0.0165(18) 0.023(2) F62 0.049(4) 0.027(3) 0.034(3) -0.0105(18) 0.003(2) 0.022(3) F63 0.044(4) 0.049(4) 0.0283(18) 0.009(3) -0.004(2) 0.029(4) C49' 0.0326(17) 0.028(2) 0.0378(15) -0.0151(14) -0.0057(14) 0.0155(16) F50' 0.034(3) 0.051(3) 0.0278(11) -0.006(2) 0.0103(15) 0.0249(17) F51' 0.0304(15) 0.0341(19) 0.041(3) -0.0174(15) -0.0134(14) 0.0150(13) F52' 0.036(2) 0.050(4) 0.042(3) -0.015(2) 0.000(2) 0.027(2) S53' 0.0201(9) 0.0173(8) 0.0271(7) -0.0034(6) -0.0017(7) 0.0078(7) O54' 0.032(2) 0.0216(19) 0.0460(17) 0.0087(17) -0.015(3) 0.0022(19) O55' 0.0213(13) 0.0210(18) 0.040(2) -0.0048(15) -0.0046(12) 0.0061(11) N56' 0.0234(12) 0.0175(11) 0.0370(16) -0.0094(12) -0.0034(13) 0.0083(10) S57' 0.0224(19) 0.0153(16) 0.0249(6) -0.0026(15) -0.0012(16) 0.0074(13) O58' 0.037(2) 0.029(3) 0.017(2) -0.0032(19) -0.0038(19) 0.017(2) O59' 0.0201(16) 0.0204(18) 0.049(2) -0.001(3) 0.0062(16) 0.0025(19) C60' 0.034(4) 0.024(6) 0.021(4) 0.013(3) 0.010(3) 0.020(5) F61' 0.032(2) 0.043(3) 0.050(2) 0.019(2) 0.0165(18) 0.023(2) F62' 0.049(4) 0.027(3) 0.034(3) -0.0105(18) 0.003(2) 0.022(3) F63' 0.044(4) 0.049(4) 0.0283(18) 0.009(3) -0.004(2) 0.029(4) C49" 0.0326(17) 0.028(2) 0.0378(15) -0.0151(14) -0.0057(14) 0.0155(16) F50" 0.034(3) 0.051(3) 0.0278(11) -0.006(2) 0.0103(15) 0.0249(17) F51" 0.0304(15) 0.0341(19) 0.041(3) -0.0174(15) -0.0134(14) 0.0150(13) F52" 0.036(2) 0.050(4) 0.042(3) -0.015(2) 0.000(2) 0.027(2) O7' 0.014(2) 0.019(2) 0.0255(18) -0.0021(17) 0.0004(15) 0.0043(17) O8' 0.0144(19) 0.020(2) 0.0240(18) -0.0017(16) -0.0008(16) 0.0114(17) N14' 0.015(2) 0.016(3) 0.013(2) 0.0016(19) 0.0004(19) 0.008(2) C24' 0.017(3) 0.023(3) 0.022(3) -0.001(2) 0.001(2) 0.010(3) C25' 0.021(3) 0.027(3) 0.025(3) 0.002(3) 0.005(3) 0.013(3) C26' 0.020(5) 0.023(4) 0.027(4) -0.010(4) -0.007(4) 0.015(4) C27' 0.030(3) 0.021(4) 0.032(3) 0.000(3) 0.000(3) 0.014(3) C28' 0.020(3) 0.019(3) 0.022(3) 0.002(2) 0.002(3) 0.012(3) C64 0.026(4) 0.034(4) 0.027(4) 0.003(3) 0.002(3) 0.011(3) F65 0.0313(18) 0.027(4) 0.041(4) 0.010(3) 0.008(3) 0.018(3) F66 0.035(4) 0.021(3) 0.048(4) 0.008(2) 0.010(2) 0.005(3) F67 0.035(3) 0.069(4) 0.023(2) 0.016(2) 0.0006(18) 0.019(3) S68 0.0150(15) 0.0203(11) 0.0355(11) 0.0041(8) 0.0065(10) 0.0131(7) O69 0.028(3) 0.023(3) 0.019(5) 0.006(4) 0.012(4) 0.012(2) O70 0.026(3) 0.041(5) 0.030(3) 0.000(4) -0.007(2) 0.008(4) N71 0.020(2) 0.021(2) 0.034(2) 0.005(2) 0.008(2) 0.0080(17) S72 0.0155(17) 0.0218(13) 0.0284(6) 0.0031(8) 0.0004(11) 0.0101(8) O73 0.033(3) 0.034(3) 0.033(3) -0.008(3) -0.016(2) 0.010(3) O74 0.024(5) 0.024(3) 0.052(7) 0.003(5) 0.003(4) 0.008(3) C75 0.055(4) 0.015(3) 0.026(3) -0.005(3) -0.004(3) 0.011(3) F76 0.073(4) 0.030(3) 0.046(3) 0.018(2) 0.020(3) 0.015(3) F77 0.069(3) 0.035(2) 0.037(2) -0.0052(19) -0.013(2) 0.023(2) F78 0.061(4) 0.042(3) 0.042(4) -0.001(3) -0.007(2) 0.034(3) C64' 0.026(4) 0.034(4) 0.027(4) 0.003(3) 0.002(3) 0.011(3) F65' 0.0313(18) 0.027(4) 0.041(4) 0.010(3) 0.008(3) 0.018(3) F66' 0.035(4) 0.021(3) 0.048(4) 0.008(2) 0.010(2) 0.005(3) F67' 0.035(3) 0.069(4) 0.023(2) 0.016(2) 0.0006(18) 0.019(3) S68' 0.0150(15) 0.0203(11) 0.0355(11) 0.0041(8) 0.0065(10) 0.0131(7) O69' 0.028(3) 0.023(3) 0.019(5) 0.006(4) 0.012(4) 0.012(2) O70' 0.026(3) 0.041(5) 0.030(3) 0.000(4) -0.007(2) 0.008(4) N71' 0.020(2) 0.021(2) 0.034(2) 0.005(2) 0.008(2) 0.0080(17) S72' 0.0155(17) 0.0218(13) 0.0284(6) 0.0031(8) 0.0004(11) 0.0101(8) O73' 0.033(3) 0.034(3) 0.033(3) -0.008(3) -0.016(2) 0.010(3) O74' 0.024(5) 0.024(3) 0.052(7) 0.003(5) 0.003(4) 0.008(3) C75' 0.055(4) 0.015(3) 0.026(3) -0.005(3) -0.004(3) 0.011(3) F76' 0.073(4) 0.030(3) 0.046(3) 0.018(2) 0.020(3) 0.015(3) F77' 0.069(3) 0.035(2) 0.037(2) -0.0052(19) -0.013(2) 0.023(2) F78' 0.061(4) 0.042(3) 0.042(4) -0.001(3) -0.007(2) 0.034(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 Ag1 O7 2.455(4) 3_445 ? Ag1 O7 2.455(4) 2_455 ? Ag1 O7 2.455(4) . ? Ag1 O8 2.490(4) 3_445 ? Ag1 O8 2.490(4) . ? Ag1 O8 2.490(4) 2_455 ? Ag1 O7' 2.524(13) . ? Ag1 O7' 2.524(13) 3_445 ? Ag1 O7' 2.524(13) 2_455 ? Ag1 O8' 2.388(13) . ? Ag1 O8' 2.388(13) 2_455 ? Ag1 O8' 2.388(13) 3_445 ? Ag2 Ag3 3.1054(8) . ? Ag2 O8 2.444(4) . ? Ag2 O8 2.444(4) 2_455 ? Ag2 O8 2.444(4) 3_445 ? Ag2 O9 2.489(3) 2_455 ? Ag2 O9 2.489(3) . ? Ag2 O9 2.489(3) 3_445 ? Ag2 O8' 2.551(13) 3_445 ? Ag2 O8' 2.551(13) 2_455 ? Ag2 O8' 2.551(13) . ? Ag3 Ag4 3.2004(8) . ? Ag3 O9 2.494(3) . ? Ag3 O9 2.494(3) 2_455 ? Ag3 O9 2.495(3) 3_445 ? Ag3 O10 2.449(3) . ? Ag3 O10 2.449(3) 2_455 ? Ag3 O10 2.449(3) 3_445 ? Ag4 Ag1 3.0244(7) 1_556 ? Ag4 O7 2.527(4) 3_446 ? Ag4 O7 2.527(4) 1_556 ? Ag4 O7 2.527(4) 2_456 ? Ag4 O10 2.451(3) 3_445 ? Ag4 O10 2.451(3) 2_455 ? Ag4 O10 2.451(3) . ? Ag4 O7' 2.447(13) 3_446 ? Ag4 O7' 2.447(13) 1_556 ? Ag4 O7' 2.447(13) 2_456 ? N13 C19 1.366(12) . ? N13 C23 1.363(8) . ? N13 O7 1.331(7) . ? C19 C20 1.406(14) . ? C20 C21 1.399(15) . ? C21 C22 1.413(11) . ? C22 C23 1.390(9) . ? N13' C19' 1.28(4) . ? N13' C23' 1.29(4) . ? N13' O7' 1.330(11) . ? C19' C20' 1.27(5) . ? C20' C21' 1.22(7) . ? C21' C22' 1.33(6) . ? C22' C23' 1.31(5) . ? N14 C24 1.345(7) . ? N14 C28 1.358(7) . ? N14 O8 1.341(6) . ? C24 C25 1.369(8) . ? C25 C26 1.371(9) . ? C26 C27 1.392(11) . ? C27 C28 1.375(9) . ? C29 C30 1.377(7) . ? C29 N15 1.358(5) . ? C30 C31 1.373(7) . ? C31 C32 1.383(6) . ? C32 C33 1.372(6) . ? C33 N15 1.353(5) . ? C34 C35 1.377(7) . ? C34 N16 1.362(5) . ? C35 C36 1.381(7) . ? C36 C37 1.393(7) . ? C37 C38 1.371(6) . ? C38 N16 1.339(6) . ? N15 O9 1.327(4) . ? N16 O10 1.327(4) . ? O7 Ag4 2.527(4) 1_554 ? Ag5 Ag6 3.2300(8) . ? Ag5 Ag6 3.0586(8) 4_554 ? Ag5 O11 2.463(3) . ? Ag5 O11 2.463(3) 3 ? Ag5 O11 2.463(3) 2 ? Ag5 O12 2.499(3) 6_554 ? Ag5 O12 2.499(3) 4_554 ? Ag5 O12 2.499(3) 5_554 ? Ag6 Ag5 3.0585(8) 4 ? Ag6 O11 2.461(3) 2 ? Ag6 O11 2.461(3) . ? Ag6 O11 2.461(3) 3 ? Ag6 O12 2.491(3) . ? Ag6 O12 2.491(3) 2 ? Ag6 O12 2.491(3) 3 ? C39 C40 1.374(6) . ? C39 N17 1.342(5) . ? C40 C41 1.380(7) . ? C41 C42 1.376(7) . ? C42 C43 1.380(6) . ? C43 N17 1.356(6) . ? C44 C45 1.367(6) . ? C44 N18 1.345(6) . ? C45 C46 1.384(6) . ? C46 C47 1.393(7) . ? C47 C48 1.365(6) . ? C48 N18 1.355(6) . ? N17 O11 1.335(4) . ? N18 O12 1.333(4) . ? O12 Ag5 2.499(3) 4 ? C49 F50 1.347(7) . ? C49 F51 1.350(7) . ? C49 F52 1.343(7) . ? C49 S53 1.772(8) . ? S53 O54 1.427(4) . ? S53 O55 1.438(4) . ? S53 N56 1.561(4) . ? N56 S57 1.561(6) . ? S57 O58 1.427(9) . ? S57 O59 1.423(7) . ? S57 C60 1.794(14) . ? C60 F61 1.365(12) . ? C60 F62 1.323(11) . ? C60 F63 1.365(13) . ? C49' F50' 1.299(7) . ? C49' F51' 1.338(7) . ? C49' F52' 1.339(7) . ? C49' S53' 1.752(9) . ? S53' O54' 1.436(8) . ? S53' O55' 1.439(8) . ? S53' N56' 1.582(8) . ? N56' S57' 1.61(3) . ? S57' O58' 1.45(4) . ? S57' O59' 1.42(3) . ? S57' C60' 2.06(6) . ? C60' F61' 1.11(6) . ? C60' F62' 1.48(5) . ? C60' F63' 1.22(7) . ? C49" F50" 1.352(8) . ? C49" F51" 1.361(8) . ? C49" F52" 1.363(8) . ? O7' Ag4 2.447(13) 1_554 ? O8' N14' 1.340(11) . ? N14' C24' 1.344(19) . ? N14' C28' 1.345(18) . ? C24' C25' 1.380(19) . ? C25' C26' 1.374(19) . ? C26' C27' 1.376(19) . ? C27' C28' 1.371(18) . ? C64 F65 1.26(3) . ? C64 F66 1.36(2) . ? C64 F67 1.33(3) . ? C64 S68 1.822(19) . ? S68 O69 1.516(16) . ? S68 O70 1.352(11) . ? S68 N71 1.594(7) . ? N71 S72 1.535(8) . ? S72 O73 1.440(8) . ? S72 O74 1.49(3) . ? S72 C75 1.799(9) . ? C75 F76 1.313(9) . ? C75 F77 1.325(8) . ? C75 F78 1.338(11) . ? C64' F65' 1.50(9) . ? C64' F66' 1.24(7) . ? C64' F67' 1.39(7) . ? C64' S68' 1.84(6) . ? S68' O69' 1.21(5) . ? S68' O70' 1.62(3) . ? S68' N71' 1.62(2) . ? N71' S72' 1.67(2) . ? S72' O73' 1.42(2) . ? S72' O74' 1.26(7) . ? S72' C75' 1.92(3) . ? C75' F76' 1.30(3) . ? C75' F77' 1.29(2) . ? C75' F78' 1.36(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Ag1 O7 88.54(13) 2_455 3_445 ? O7 Ag1 O7 88.54(13) . 2_455 ? O7 Ag1 O7 88.54(13) . 3_445 ? O7 Ag1 O8 92.57(12) 3_445 . ? O7 Ag1 O8 92.58(12) . 2_455 ? O7 Ag1 O8 173.06(14) . 3_445 ? O7 Ag1 O8 98.33(12) . . ? O7 Ag1 O8 98.33(12) 2_455 2_455 ? O7 Ag1 O8 98.33(12) 3_445 3_445 ? O7 Ag1 O8 173.06(14) 2_455 . ? O7 Ag1 O8 173.06(14) 3_445 2_455 ? O7 Ag1 O8 92.57(12) 2_455 3_445 ? O7 Ag1 O7' 48.3(3) 2_455 2_455 ? O7 Ag1 O7' 45.3(3) . 2_455 ? O7 Ag1 O7' 105.1(3) 3_445 2_455 ? O7 Ag1 O7' 105.1(3) . 3_445 ? O7 Ag1 O7' 45.3(3) 2_455 3_445 ? O7 Ag1 O7' 48.3(3) . . ? O7 Ag1 O7' 48.3(3) 3_445 3_445 ? O7 Ag1 O7' 45.3(3) 3_445 . ? O7 Ag1 O7' 105.1(3) 2_455 . ? O8 Ag1 O8 80.49(13) 2_455 . ? O8 Ag1 O8 80.49(13) 2_455 3_445 ? O8 Ag1 O8 80.49(13) . 3_445 ? O8 Ag1 O7' 137.5(3) 2_455 3_445 ? O8 Ag1 O7' 137.5(3) . 2_455 ? O8 Ag1 O7' 132.5(3) . 3_445 ? O8 Ag1 O7' 80.5(3) 3_445 3_445 ? O8 Ag1 O7' 80.5(3) 2_455 2_455 ? O8 Ag1 O7' 132.5(3) 3_445 2_455 ? O8 Ag1 O7' 80.5(3) . . ? O8 Ag1 O7' 137.5(3) 3_445 . ? O8 Ag1 O7' 132.5(3) 2_455 . ? O7' Ag1 O7' 85.1(4) 2_455 3_445 ? O7' Ag1 O7' 85.1(4) 2_455 . ? O7' Ag1 O7' 85.1(4) 3_445 . ? O8' Ag1 O7 117.0(3) 2_455 3_445 ? O8' Ag1 O7 78.0(3) . 3_445 ? O8' Ag1 O7 117.0(3) . 2_455 ? O8' Ag1 O7 150.3(3) 3_445 3_445 ? O8' Ag1 O7 150.3(3) 2_455 2_455 ? O8' Ag1 O7 78.0(3) 3_445 2_455 ? O8' Ag1 O7 117.0(3) 3_445 . ? O8' Ag1 O7 150.3(3) . . ? O8' Ag1 O7 78.0(3) 2_455 . ? O8' Ag1 O8 32.6(3) 3_445 2_455 ? O8' Ag1 O8 56.6(3) 2_455 2_455 ? O8' Ag1 O8 32.6(3) . 3_445 ? O8' Ag1 O8 97.9(3) 2_455 3_445 ? O8' Ag1 O8 56.6(3) . . ? O8' Ag1 O8 97.9(3) . 2_455 ? O8' Ag1 O8 56.6(3) 3_445 3_445 ? O8' Ag1 O8 32.6(3) 2_455 . ? O8' Ag1 O8 97.9(3) 3_445 . ? O8' Ag1 O7' 85.6(4) 3_445 2_455 ? O8' Ag1 O7' 106.9(4) 2_455 2_455 ? O8' Ag1 O7' 164.2(4) 3_445 . ? O8' Ag1 O7' 85.6(4) . 3_445 ? O8' Ag1 O7' 164.2(4) . 2_455 ? O8' Ag1 O7' 85.6(4) 2_455 . ? O8' Ag1 O7' 106.9(4) . . ? O8' Ag1 O7' 106.9(4) 3_445 3_445 ? O8' Ag1 O7' 164.2(4) 2_455 3_445 ? O8' Ag1 O8' 84.7(5) 2_455 . ? O8' Ag1 O8' 84.7(5) 3_445 . ? O8' Ag1 O8' 84.7(5) 3_445 2_455 ? Ag3 Ag2 Ag1 180.0 . . ? O8 Ag2 Ag1 49.46(9) 3_445 . ? O8 Ag2 Ag1 49.45(9) . . ? O8 Ag2 Ag1 49.45(9) 2_455 . ? O8 Ag2 Ag3 130.55(9) 2_455 . ? O8 Ag2 Ag3 130.54(9) 3_445 . ? O8 Ag2 Ag3 130.55(9) . . ? O8 Ag2 O8 82.31(13) . 3_445 ? O8 Ag2 O8 82.31(13) 2_455 3_445 ? O8 Ag2 O8 82.31(13) 2_455 . ? O8 Ag2 O9 81.13(11) . 3_445 ? O8 Ag2 O9 149.46(11) . 2_455 ? O8 Ag2 O9 149.46(11) 2_455 3_445 ? O8 Ag2 O9 81.13(11) 3_445 2_455 ? O8 Ag2 O9 120.39(11) . . ? O8 Ag2 O9 120.39(11) 3_445 3_445 ? O8 Ag2 O9 81.14(11) 2_455 . ? O8 Ag2 O9 149.47(11) 3_445 . ? O8 Ag2 O9 120.39(11) 2_455 2_455 ? O8 Ag2 O8' 55.2(3) 2_455 2_455 ? O8 Ag2 O8' 31.8(3) 2_455 3_445 ? O8 Ag2 O8' 55.2(3) . . ? O8 Ag2 O8' 31.8(3) 3_445 . ? O8 Ag2 O8' 94.9(3) . 3_445 ? O8 Ag2 O8' 31.8(3) . 2_455 ? O8 Ag2 O8' 94.9(3) 3_445 2_455 ? O8 Ag2 O8' 55.2(3) 3_445 3_445 ? O8 Ag2 O8' 94.9(3) 2_455 . ? O9 Ag2 Ag1 128.47(7) . . ? O9 Ag2 Ag1 128.47(7) 2_455 . ? O9 Ag2 Ag1 128.46(7) 3_445 . ? O9 Ag2 Ag3 51.54(7) 3_445 . ? O9 Ag2 Ag3 51.53(7) 2_455 . ? O9 Ag2 Ag3 51.53(7) . . ? O9 Ag2 O9 85.39(11) 2_455 3_445 ? O9 Ag2 O9 85.39(11) . 3_445 ? O9 Ag2 O9 85.39(11) . 2_455 ? O9 Ag2 O8' 96.5(3) 3_445 . ? O9 Ag2 O8' 174.6(3) 3_445 3_445 ? O9 Ag2 O8' 174.6(3) . . ? O9 Ag2 O8' 99.8(3) 2_455 . ? O9 Ag2 O8' 96.5(3) 2_455 3_445 ? O9 Ag2 O8' 96.5(3) . 2_455 ? O9 Ag2 O8' 174.6(3) 2_455 2_455 ? O9 Ag2 O8' 99.8(3) . 3_445 ? O9 Ag2 O8' 99.8(3) 3_445 2_455 ? O8' Ag2 Ag1 46.8(3) 3_445 . ? O8' Ag2 Ag1 46.8(3) 2_455 . ? O8' Ag2 Ag1 46.8(3) . . ? O8' Ag2 Ag3 133.2(3) 3_445 . ? O8' Ag2 Ag3 133.2(3) . . ? O8' Ag2 Ag3 133.2(3) 2_455 . ? O8' Ag2 O8' 78.3(5) 3_445 . ? O8' Ag2 O8' 78.2(5) 3_445 2_455 ? O8' Ag2 O8' 78.2(5) 2_455 . ? Ag2 Ag3 Ag4 180.0 . . ? O9 Ag3 Ag2 51.38(7) . . ? O9 Ag3 Ag2 51.38(7) 2_455 . ? O9 Ag3 Ag2 51.38(7) 3_445 . ? O9 Ag3 Ag4 128.62(7) . . ? O9 Ag3 Ag4 128.62(7) 2_455 . ? O9 Ag3 Ag4 128.62(7) 3_445 . ? O9 Ag3 O9 85.15(11) 2_455 3_445 ? O9 Ag3 O9 85.16(11) . 2_455 ? O9 Ag3 O9 85.16(11) . 3_445 ? O10 Ag3 Ag2 130.76(7) . . ? O10 Ag3 Ag2 130.76(7) 3_445 . ? O10 Ag3 Ag2 130.76(7) 2_455 . ? O10 Ag3 Ag4 49.24(7) 3_445 . ? O10 Ag3 Ag4 49.24(7) 2_455 . ? O10 Ag3 Ag4 49.24(7) . . ? O10 Ag3 O9 88.63(9) 2_455 3_445 ? O10 Ag3 O9 105.81(10) . 3_445 ? O10 Ag3 O9 166.91(10) . . ? O10 Ag3 O9 105.82(10) 3_445 2_455 ? O10 Ag3 O9 105.81(10) 2_455 . ? O10 Ag3 O9 166.91(10) 3_445 3_445 ? O10 Ag3 O9 88.63(9) . 2_455 ? O10 Ag3 O9 88.63(9) 3_445 . ? O10 Ag3 O9 166.91(10) 2_455 2_455 ? O10 Ag3 O10 81.99(11) 2_455 . ? O10 Ag3 O10 81.99(11) 3_445 . ? O10 Ag3 O10 81.99(11) 3_445 2_455 ? Ag1 Ag4 Ag3 180.0 1_556 . ? O7 Ag4 Ag1 51.55(9) 2_456 1_556 ? O7 Ag4 Ag1 51.55(9) 1_556 1_556 ? O7 Ag4 Ag1 51.55(9) 3_446 1_556 ? O7 Ag4 Ag3 128.45(9) 2_456 . ? O7 Ag4 Ag3 128.45(9) 1_556 . ? O7 Ag4 Ag3 128.45(9) 3_446 . ? O7 Ag4 O7 85.41(13) 1_556 3_446 ? O7 Ag4 O7 85.41(13) 2_456 3_446 ? O7 Ag4 O7 85.41(13) 2_456 1_556 ? O10 Ag4 Ag1 130.80(7) . 1_556 ? O10 Ag4 Ag1 130.80(7) 2_455 1_556 ? O10 Ag4 Ag1 130.80(7) 3_445 1_556 ? O10 Ag4 Ag3 49.20(7) 2_455 . ? O10 Ag4 Ag3 49.20(7) . . ? O10 Ag4 Ag3 49.20(7) 3_445 . ? O10 Ag4 O7 106.15(12) . 2_456 ? O10 Ag4 O7 166.34(11) 3_445 3_446 ? O10 Ag4 O7 166.34(11) 2_455 2_456 ? O10 Ag4 O7 88.23(11) 3_445 2_456 ? O10 Ag4 O7 106.14(12) 2_455 3_446 ? O10 Ag4 O7 166.34(11) . 1_556 ? O10 Ag4 O7 88.23(11) 2_455 1_556 ? O10 Ag4 O7 88.23(11) . 3_446 ? O10 Ag4 O7 106.15(11) 3_445 1_556 ? O10 Ag4 O10 81.93(11) 3_445 . ? O10 Ag4 O10 81.93(11) 2_455 . ? O10 Ag4 O10 81.93(11) 3_445 2_455 ? O7' Ag4 Ag1 53.7(3) 3_446 1_556 ? O7' Ag4 Ag1 53.7(3) 2_456 1_556 ? O7' Ag4 Ag1 53.7(3) 1_556 1_556 ? O7' Ag4 Ag3 126.3(3) 2_456 . ? O7' Ag4 Ag3 126.3(3) 1_556 . ? O7' Ag4 Ag3 126.3(3) 3_446 . ? O7' Ag4 O7 105.2(3) 1_556 2_456 ? O7' Ag4 O7 45.3(3) 3_446 2_456 ? O7' Ag4 O7 48.4(3) 3_446 3_446 ? O7' Ag4 O7 45.3(3) 1_556 3_446 ? O7' Ag4 O7 48.4(3) 1_556 1_556 ? O7' Ag4 O7 48.4(3) 2_456 2_456 ? O7' Ag4 O7 105.2(3) 2_456 3_446 ? O7' Ag4 O7 105.2(3) 3_446 1_556 ? O7' Ag4 O7 45.3(3) 2_456 1_556 ? O7' Ag4 O10 119.8(3) 3_446 3_445 ? O7' Ag4 O10 148.3(3) 3_446 2_455 ? O7' Ag4 O10 119.8(3) 2_456 2_455 ? O7' Ag4 O10 79.2(3) 1_556 2_455 ? O7' Ag4 O10 148.3(3) 2_456 . ? O7' Ag4 O10 79.2(3) 2_456 3_445 ? O7' Ag4 O10 148.3(3) 1_556 3_445 ? O7' Ag4 O10 119.8(3) 1_556 . ? O7' Ag4 O10 79.2(3) 3_446 . ? O7' Ag4 O7' 88.5(4) 1_556 3_446 ? O7' Ag4 O7' 88.5(4) 2_456 3_446 ? O7' Ag4 O7' 88.5(4) 2_456 1_556 ? C23 N13 C19 122.3(7) . . ? O7 N13 C19 117.9(6) . . ? O7 N13 C23 119.9(6) . . ? N13 C19 C20 118.4(9) . . ? C21 C20 C19 121.2(10) . . ? C20 C21 C22 117.9(9) . . ? C23 C22 C21 120.1(8) . . ? N13 C23 C22 120.1(7) . . ? C19' N13' C23' 120(3) . . ? C19' N13' O7' 120(3) . . ? C23' N13' O7' 120(2) . . ? C20' C19' N13' 121(4) . . ? C21' C20' C19' 123(5) . . ? C20' C21' C22' 116(5) . . ? C23' C22' C21' 123(4) . . ? N13' C23' C22' 116(3) . . ? C24 N14 C28 121.3(5) . . ? O8 N14 C24 118.5(5) . . ? O8 N14 C28 120.2(5) . . ? N14 C24 C25 120.3(6) . . ? C24 C25 C26 120.3(7) . . ? C25 C26 C27 118.6(9) . . ? C28 C27 C26 120.2(7) . . ? N14 C28 C27 119.3(6) . . ? N15 C29 C30 119.7(5) . . ? C31 C30 C29 120.4(5) . . ? C30 C31 C32 118.7(5) . . ? C33 C32 C31 120.3(5) . . ? N15 C33 C32 119.9(4) . . ? N16 C34 C35 120.1(4) . . ? C34 C35 C36 119.9(5) . . ? C35 C36 C37 118.9(5) . . ? C38 C37 C36 119.5(5) . . ? N16 C38 C37 121.0(4) . . ? C33 N15 C29 120.9(4) . . ? O9 N15 C29 118.5(4) . . ? O9 N15 C33 120.6(4) . . ? C38 N16 C34 120.7(4) . . ? O10 N16 C34 120.6(4) . . ? O10 N16 C38 118.8(4) . . ? Ag1 O7 Ag4 74.74(11) . 1_554 ? N13 O7 Ag1 119.1(3) . . ? N13 O7 Ag4 115.0(3) . 1_554 ? Ag2 O8 Ag1 82.30(11) . . ? N14 O8 Ag1 115.4(3) . . ? N14 O8 Ag2 118.2(3) . . ? Ag2 O9 Ag3 77.09(9) . . ? N15 O9 Ag2 115.7(2) . . ? N15 O9 Ag3 120.4(2) . . ? Ag3 O10 Ag4 81.55(10) . . ? N16 O10 Ag3 120.5(2) . . ? N16 O10 Ag4 119.2(2) . . ? Ag6 Ag5 Ag6 180.0 4_554 . ? O11 Ag5 Ag6 131.03(7) . 4_554 ? O11 Ag5 Ag6 48.97(7) . . ? O11 Ag5 Ag6 48.97(7) 3 . ? O11 Ag5 Ag6 48.97(7) 2 . ? O11 Ag5 Ag6 131.03(7) 2 4_554 ? O11 Ag5 Ag6 131.03(7) 3 4_554 ? O11 Ag5 O11 81.58(11) 3 2 ? O11 Ag5 O11 81.58(11) . 2 ? O11 Ag5 O11 81.58(11) . 3 ? O11 Ag5 O12 89.85(10) 3 6_554 ? O11 Ag5 O12 89.84(10) . 4_554 ? O11 Ag5 O12 103.28(10) . 5_554 ? O11 Ag5 O12 103.28(10) 2 6_554 ? O11 Ag5 O12 103.28(10) 3 4_554 ? O11 Ag5 O12 89.84(10) 2 5_554 ? O11 Ag5 O12 169.48(10) 3 5_554 ? O11 Ag5 O12 169.48(10) 2 4_554 ? O11 Ag5 O12 169.49(10) . 6_554 ? O12 Ag5 Ag6 52.08(7) 4_554 4_554 ? O12 Ag5 Ag6 52.08(7) 6_554 4_554 ? O12 Ag5 Ag6 52.08(7) 5_554 4_554 ? O12 Ag5 Ag6 127.92(7) 5_554 . ? O12 Ag5 Ag6 127.92(7) 6_554 . ? O12 Ag5 Ag6 127.92(7) 4_554 . ? O12 Ag5 O12 86.19(10) 6_554 5_554 ? O12 Ag5 O12 86.19(10) 4_554 5_554 ? O12 Ag5 O12 86.19(10) 4_554 6_554 ? Ag5 Ag6 Ag5 180.0 4 . ? O11 Ag6 Ag5 49.03(7) 3 . ? O11 Ag6 Ag5 49.03(7) 2 . ? O11 Ag6 Ag5 49.03(7) . . ? O11 Ag6 Ag5 130.97(7) 3 4 ? O11 Ag6 Ag5 130.97(7) 2 4 ? O11 Ag6 Ag5 130.97(7) . 4 ? O11 Ag6 O11 81.67(11) . 2 ? O11 Ag6 O11 81.67(11) . 3 ? O11 Ag6 O11 81.67(11) 2 3 ? O11 Ag6 O12 89.55(9) 2 . ? O11 Ag6 O12 169.31(10) 3 . ? O11 Ag6 O12 169.31(10) 2 3 ? O11 Ag6 O12 103.18(10) 3 3 ? O11 Ag6 O12 89.55(9) . 3 ? O11 Ag6 O12 89.55(9) 3 2 ? O11 Ag6 O12 103.18(10) . . ? O11 Ag6 O12 169.31(10) . 2 ? O11 Ag6 O12 103.18(10) 2 2 ? O12 Ag6 Ag5 52.31(7) . 4 ? O12 Ag6 Ag5 52.31(7) 3 4 ? O12 Ag6 Ag5 52.31(7) 2 4 ? O12 Ag6 Ag5 127.69(7) . . ? O12 Ag6 Ag5 127.69(7) 3 . ? O12 Ag6 Ag5 127.69(7) 2 . ? O12 Ag6 O12 86.51(10) 2 3 ? O12 Ag6 O12 86.52(10) 2 . ? O12 Ag6 O12 86.52(10) . 3 ? N17 C39 C40 120.2(4) . . ? C39 C40 C41 120.4(4) . . ? C42 C41 C40 118.3(5) . . ? C41 C42 C43 120.6(5) . . ? N17 C43 C42 119.5(4) . . ? N18 C44 C45 120.9(4) . . ? C44 C45 C46 119.8(5) . . ? C45 C46 C47 118.6(4) . . ? C48 C47 C46 119.8(5) . . ? N18 C48 C47 120.5(4) . . ? C39 N17 C43 121.0(4) . . ? O11 N17 C39 120.5(4) . . ? O11 N17 C43 118.5(4) . . ? C44 N18 C48 120.4(4) . . ? O12 N18 C44 118.8(4) . . ? O12 N18 C48 120.8(4) . . ? Ag6 O11 Ag5 82.00(10) . . ? N17 O11 Ag5 116.1(2) . . ? N17 O11 Ag6 120.8(2) . . ? Ag6 O12 Ag5 75.61(9) . 4 ? N18 O12 Ag5 117.8(2) . 4 ? N18 O12 Ag6 118.2(2) . . ? F50 C49 F51 104.6(9) . . ? F50 C49 S53 112.2(8) . . ? F51 C49 S53 112.1(13) . . ? F52 C49 F50 104.4(7) . . ? F52 C49 F51 107.1(9) . . ? F52 C49 S53 115.5(9) . . ? O54 S53 C49 102.8(5) . . ? O54 S53 O55 118.9(3) . . ? O54 S53 N56 110.4(4) . . ? O55 S53 C49 104.4(4) . . ? O55 S53 N56 117.8(3) . . ? N56 S53 C49 98.9(4) . . ? S57 N56 S53 127.6(4) . . ? N56 S57 C60 101.0(5) . . ? O58 S57 N56 110.1(4) . . ? O58 S57 C60 102.2(6) . . ? O59 S57 N56 119.0(5) . . ? O59 S57 O58 118.2(5) . . ? O59 S57 C60 102.7(7) . . ? F61 C60 S57 112.3(8) . . ? F62 C60 S57 114.4(5) . . ? F62 C60 F61 106.9(8) . . ? F62 C60 F63 107.9(9) . . ? F63 C60 S57 111.0(8) . . ? F63 C60 F61 103.7(5) . . ? F50' C49' F51' 110.7(10) . . ? F50' C49' F52' 115.9(8) . . ? F50' C49' S53' 116.3(7) . . ? F51' C49' F52' 107.9(9) . . ? F51' C49' S53' 89.5(14) . . ? F52' C49' S53' 113.1(8) . . ? O54' S53' C49' 101.7(17) . . ? O54' S53' O55' 117.7(12) . . ? O54' S53' N56' 108.2(15) . . ? O55' S53' C49' 97.9(8) . . ? O55' S53' N56' 114.5(8) . . ? N56' S53' C49' 116.0(9) . . ? S53' N56' S57' 129.6(13) . . ? N56' S57' C60' 95(2) . . ? O58' S57' N56' 109.1(19) . . ? O58' S57' C60' 111(2) . . ? O59' S57' N56' 104(2) . . ? O59' S57' O58' 122(3) . . ? O59' S57' C60' 112(3) . . ? F61' C60' S57' 108(4) . . ? F61' C60' F62' 108(4) . . ? F61' C60' F63' 141(4) . . ? F62' C60' S57' 87(2) . . ? F63' C60' S57' 97(3) . . ? F63' C60' F62' 102(4) . . ? F50" C49" F51" 104.0(14) . . ? F50" C49" F52" 100.9(12) . . ? F51" C49" F52" 106.1(14) . . ? Ag4 O7' Ag1 74.9(3) 1_554 . ? N13' O7' Ag1 116.6(16) . . ? N13' O7' Ag4 117.3(13) . 1_554 ? Ag1 O8' Ag2 82.1(4) . . ? N14' O8' Ag1 118.1(11) . . ? N14' O8' Ag2 114.5(12) . . ? O8' N14' C24' 120.9(15) . . ? O8' N14' C28' 116.2(15) . . ? C24' N14' C28' 122.9(18) . . ? N14' C24' C25' 120(2) . . ? C26' C25' C24' 118(3) . . ? C25' C26' C27' 118(3) . . ? C28' C27' C26' 122(3) . . ? N14' C28' C27' 116.7(18) . . ? F65 C64 F66 106.2(15) . . ? F65 C64 F67 110(2) . . ? F65 C64 S68 112.4(17) . . ? F66 C64 S68 107.3(17) . . ? F67 C64 F66 106.7(19) . . ? F67 C64 S68 113.9(13) . . ? O69 S68 C64 106.8(11) . . ? O69 S68 N71 111.8(6) . . ? O70 S68 C64 107.7(9) . . ? O70 S68 O69 115.2(7) . . ? O70 S68 N71 117.8(5) . . ? N71 S68 C64 94.7(9) . . ? S72 N71 S68 127.4(4) . . ? N71 S72 C75 105.7(4) . . ? O73 S72 N71 108.7(5) . . ? O73 S72 O74 113.2(7) . . ? O73 S72 C75 103.9(4) . . ? O74 S72 N71 117.6(9) . . ? O74 S72 C75 106.6(8) . . ? F76 C75 S72 112.0(7) . . ? F76 C75 F77 109.8(6) . . ? F76 C75 F78 106.9(6) . . ? F77 C75 S72 110.9(5) . . ? F77 C75 F78 106.2(7) . . ? F78 C75 S72 110.7(6) . . ? F65' C64' S68' 116(4) . . ? F66' C64' F65' 113(4) . . ? F66' C64' F67' 109(5) . . ? F66' C64' S68' 115(5) . . ? F67' C64' F65' 99(5) . . ? F67' C64' S68' 103(3) . . ? O69' S68' C64' 96(3) . . ? O69' S68' O70' 125(2) . . ? O69' S68' N71' 130(2) . . ? O70' S68' C64' 95(2) . . ? O70' S68' N71' 99.0(13) . . ? N71' S68' C64' 103(3) . . ? S68' N71' S72' 116.5(11) . . ? N71' S72' C75' 92.5(11) . . ? O73' S72' N71' 109.6(13) . . ? O73' S72' C75' 103.0(12) . . ? O74' S72' N71' 103(2) . . ? O74' S72' O73' 138(3) . . ? O74' S72' C75' 100(3) . . ? F76' C75' S72' 111.5(16) . . ? F76' C75' F78' 112(2) . . ? F77' C75' S72' 104.6(16) . . ? F77' C75' F76' 109.2(19) . . ? F77' C75' F78' 109.5(18) . . ? F78' C75' S72' 110.0(16) . . ? _database_code_depnum_ccdc_archive 'CCDC 958487' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kb2002 _audit_creation_date 2013-08-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ; tris(pyridine-N-oxide) silver bistriflimide ; _chemical_name_systematic ; tris(pyridine-N-oxide) silver bis(trifluoromethylsulfonyl)imide ; _chemical_formula_moiety 'C45 H45 Ag3 N9 O9, 3(C2 F6 N O4 S2)' _chemical_formula_sum 'C51 H45 Ag3 F18 N12 O21 S6' _chemical_formula_weight 2019.93 _chemical_melting_point ? _chemical_oxdiff_formula 'Ag C2 F6 S2 O4 N C10 H10 O2 N2' 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' 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' 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' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_H-M_alt 'R -3' _space_group_name_Hall '-R 3' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 'x+2/3, y+1/3, z+1/3' 5 '-y+2/3, x-y+1/3, z+1/3' 6 '-x+y+2/3, -x+1/3, z+1/3' 7 'x+1/3, y+2/3, z+2/3' 8 '-y+1/3, x-y+2/3, z+2/3' 9 '-x+y+1/3, -x+2/3, z+2/3' 10 '-x, -y, -z' 11 'y, -x+y, -z' 12 'x-y, x, -z' 13 '-x+2/3, -y+1/3, -z+1/3' 14 'y+2/3, -x+y+1/3, -z+1/3' 15 'x-y+2/3, x+1/3, -z+1/3' 16 '-x+1/3, -y+2/3, -z+2/3' 17 'y+1/3, -x+y+2/3, -z+2/3' 18 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 25.5554(4) _cell_length_b 25.5554(4) _cell_length_c 56.4189(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 31909.5(9) _cell_formula_units_Z 18 _cell_measurement_reflns_used 40166 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.1457 _cell_measurement_theta_min 2.6840 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 18036 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_unetI/netI 0.0148 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 70 _diffrn_reflns_limit_l_min -70 _diffrn_reflns_number 53899 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.76 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -78.00 -1.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -57.0000 -120.0000 154 #__ type_ start__ end____ width___ exp.time_ 2 omega -32.00 52.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 57.0000 150.0000 168 #__ type_ start__ end____ width___ exp.time_ 3 omega -8.00 23.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -99.0000 150.0000 62 #__ type_ start__ end____ width___ exp.time_ 4 omega -9.00 55.00 0.5000 45.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 -99.0000 90.0000 128 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0317519000 _diffrn_orient_matrix_UB_12 -0.0171552000 _diffrn_orient_matrix_UB_13 -0.0016300000 _diffrn_orient_matrix_UB_21 -0.0008878000 _diffrn_orient_matrix_UB_22 0.0270306000 _diffrn_orient_matrix_UB_23 -0.0016025000 _diffrn_orient_matrix_UB_31 0.0043237000 _diffrn_orient_matrix_UB_32 -0.0012861000 _diffrn_orient_matrix_UB_33 -0.0123658000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 12956 _reflns_number_total 14480 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.742 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1045 _refine_ls_number_reflns 14480 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0361 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+190.5742P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.0874 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O5) = Uanis(O5') Uanis(N14) = Uanis(N14') Uanis(C39) = Uanis(C39') Uanis(C40) = Uanis(C40') Uanis(C41) = Uanis(C41') Uanis(C42) = Uanis(C42') Uanis(C43) = Uanis(C43') Uanis(S72) = Uanis(S72') Uanis(O73) = Uanis(O73') Uanis(O74) = Uanis(O74') Uanis(C75) = Uanis(C75') Uanis(F76) = Uanis(F76') Uanis(F77) = Uanis(F77') Uanis(F78) = Uanis(F78') 3. Same fragment restrains {O5, N14, C39, C40, C41, C42, C43} as {O5', N14', C39', C40', C41', C42', C43'} {S72, O73, O74, C75, F76, F77, F78} as {S72', O73', O74', C75', F76', F77', F78'} 4. Others Sof(S72')=Sof(O73')=Sof(O74')=Sof(C75')=Sof(F76')=Sof(F77')=Sof(F78')=1-FVAR(1) Sof(S72)=Sof(O73)=Sof(O74)=Sof(C75)=Sof(F76)=Sof(F77)=Sof(F78)=FVAR(1) Sof(O5')=Sof(N14')=Sof(C39')=Sof(H39')=Sof(C40')=Sof(H40')=Sof(C41')= Sof(H41')=Sof(C42')=Sof(H42')=Sof(C43')=Sof(H43')=1-FVAR(2) Sof(O5)=Sof(N14)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)= Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=FVAR(2) 5.a Riding coordinates: C21(H21) 5.b Aromatic/amide H refined with riding coordinates: C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C39'(H39'), C40'(H40'), C41'(H41'), C42'(H42'), C43'(H43'), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.6667 0.3333 0.3333 0.01447(10) Uani 1 6 d S . . Ag2 Ag 0.6667 0.3333 0.277486(6) 0.01501(8) Uani 1 3 d S . . Ag3 Ag 0.6667 0.3333 0.221480(6) 0.01351(8) Uani 1 3 d S . . Ag4 Ag 0.6667 0.3333 0.164340(6) 0.01447(8) Uani 1 3 d S . . Ag5 Ag 0.6667 0.3333 0.109743(6) 0.01391(8) Uani 1 3 d S . . Ag6 Ag 0.6667 0.3333 0.055643(5) 0.01328(7) Uani 1 3 d S . . Ag7 Ag 0.6667 0.3333 -0.000960(5) 0.01232(7) Uani 1 3 d S . . Ag8 Ag 0.6667 0.3333 -0.055976(6) 0.01452(8) Uani 1 3 d S . . Ag9 Ag 0.6667 0.3333 -0.109891(6) 0.01503(8) Uani 1 3 d S . . Ag10 Ag 0.6667 0.3333 -0.1667 0.01690(10) Uani 1 6 d S . . O1 O 0.74915(8) 0.35220(8) 0.30524(3) 0.0193(4) Uani 1 1 d . . . O2 O 0.74527(8) 0.40397(9) 0.24927(3) 0.0191(4) Uani 1 1 d . . . O3 O 0.58607(8) 0.27306(8) 0.19267(3) 0.0170(4) Uani 1 1 d . . . O4 O 0.74082(8) 0.41174(8) 0.13688(3) 0.0181(4) Uani 1 1 d . A . O6 O 0.70869(8) 0.29036(9) 0.02758(3) 0.0201(4) Uani 1 1 d . A . O7 O 0.74256(9) 0.33277(8) -0.02847(3) 0.0178(4) Uani 1 1 d . A . O8 O 0.68829(8) 0.26956(9) -0.08279(3) 0.0185(4) Uani 1 1 d . A . O9 O 0.63500(9) 0.24932(9) -0.13824(3) 0.0198(4) Uani 1 1 d . A . N10 N 0.79790(10) 0.40710(10) 0.30563(4) 0.0159(4) Uani 1 1 d . . . N11 N 0.79815(10) 0.40561(10) 0.24763(4) 0.0153(4) Uani 1 1 d . . . N12 N 0.53626(10) 0.27714(10) 0.19328(4) 0.0134(4) Uani 1 1 d . A . N13 N 0.74625(10) 0.46631(10) 0.13576(4) 0.0150(4) Uani 1 1 d . . . N15 N 0.76894(10) 0.31420(10) 0.02882(4) 0.0178(5) Uani 1 1 d . . . N16 N 0.74925(10) 0.28445(10) -0.02626(4) 0.0155(4) Uani 1 1 d . . . N17 N 0.74356(10) 0.27663(10) -0.08378(4) 0.0158(4) Uani 1 1 d . . . N18 N 0.66673(10) 0.22101(11) -0.13805(4) 0.0174(5) Uani 1 1 d . . . C19 C 0.79211(12) 0.45661(12) 0.30659(5) 0.0187(5) Uani 1 1 d . . . H19 H 0.7538 0.4525 0.3069 0.022 Uiso 1 1 calc R . . C20 C 0.84254(13) 0.51323(13) 0.30718(5) 0.0209(6) Uani 1 1 d . . . H20 H 0.8383 0.5473 0.3079 0.025 Uiso 1 1 calc R . . C21 C 0.89944(13) 0.51957(13) 0.30664(5) 0.0227(6) Uani 1 1 d . . . H21 H 0.9324 0.5580 0.3065 0.027 Uiso 1 1 d R . . C22 C 0.90426(13) 0.46807(13) 0.30554(5) 0.0223(6) Uani 1 1 d . . . H22 H 0.9422 0.4713 0.3051 0.027 Uiso 1 1 calc R . . C23 C 0.85309(12) 0.41212(13) 0.30509(5) 0.0189(6) Uani 1 1 d . . . H23 H 0.8564 0.3775 0.3044 0.023 Uiso 1 1 calc R . . C24 C 0.80038(13) 0.35406(13) 0.24586(5) 0.0203(6) Uani 1 1 d . . . H24 H 0.7649 0.3168 0.2464 0.024 Uiso 1 1 calc R . . C25 C 0.85525(13) 0.35671(14) 0.24320(5) 0.0237(6) Uani 1 1 d . . . H25 H 0.8568 0.3212 0.2418 0.028 Uiso 1 1 calc R . . C26 C 0.90794(13) 0.41194(14) 0.24268(5) 0.0240(6) Uani 1 1 d . . . H26 H 0.9451 0.4141 0.2407 0.029 Uiso 1 1 calc R . . C27 C 0.90444(13) 0.46395(14) 0.24509(5) 0.0240(6) Uani 1 1 d . . . H27 H 0.9395 0.5016 0.2450 0.029 Uiso 1 1 calc R . . C28 C 0.84922(12) 0.45998(12) 0.24761(5) 0.0191(6) Uani 1 1 d . . . H28 H 0.8469 0.4950 0.2493 0.023 Uiso 1 1 calc R . . C29 C 0.48238(12) 0.22556(12) 0.19462(5) 0.0165(5) Uani 1 1 d . . . H29 H 0.4808 0.1884 0.1951 0.020 Uiso 1 1 calc R A . C30 C 0.42970(12) 0.22799(13) 0.19531(5) 0.0203(6) Uani 1 1 d . A . H30 H 0.3926 0.1925 0.1963 0.024 Uiso 1 1 calc R . . C31 C 0.43181(12) 0.28301(13) 0.19456(5) 0.0203(6) Uani 1 1 d . . . H31 H 0.3965 0.2850 0.1950 0.024 Uiso 1 1 calc R A . C32 C 0.48778(12) 0.33531(12) 0.19313(5) 0.0183(5) Uani 1 1 d . A . H32 H 0.4901 0.3728 0.1926 0.022 Uiso 1 1 calc R . . C33 C 0.53995(12) 0.33196(12) 0.19249(4) 0.0158(5) Uani 1 1 d . . . H33 H 0.5774 0.3670 0.1915 0.019 Uiso 1 1 calc R A . C34 C 0.69693(13) 0.47230(13) 0.13402(5) 0.0203(6) Uani 1 1 d . A . H34 H 0.6586 0.4383 0.1342 0.024 Uiso 1 1 calc R . . C35 C 0.70341(13) 0.52888(13) 0.13193(5) 0.0239(6) Uani 1 1 d . . . H35 H 0.6694 0.5329 0.1305 0.029 Uiso 1 1 calc R A . C36 C 0.76001(14) 0.57951(13) 0.13197(5) 0.0255(6) Uani 1 1 d . A . H36 H 0.7646 0.6178 0.1304 0.031 Uiso 1 1 calc R . . C37 C 0.80993(14) 0.57230(13) 0.13438(5) 0.0257(6) Uani 1 1 d . . . H37 H 0.8486 0.6059 0.1348 0.031 Uiso 1 1 calc R A . C38 C 0.80209(12) 0.51527(12) 0.13621(5) 0.0194(6) Uani 1 1 d . A . H38 H 0.8356 0.5104 0.1378 0.023 Uiso 1 1 calc R . . O5 O 0.60839(9) 0.24529(9) 0.08236(4) 0.0189(5) Uani 0.915(4) 1 d PD A 1 N14 N 0.62612(14) 0.20425(13) 0.08283(5) 0.0168(6) Uani 0.915(4) 1 d PD A 1 C39 C 0.58398(17) 0.14547(15) 0.08618(8) 0.0215(8) Uani 0.915(4) 1 d PD A 1 H39 H 0.5438 0.1345 0.0886 0.026 Uiso 0.915(4) 1 calc PR A 1 C40 C 0.6007(2) 0.1020(2) 0.0860(2) 0.0242(9) Uani 0.915(4) 1 d PD A 1 H40 H 0.5716 0.0616 0.0881 0.029 Uiso 0.915(4) 1 calc PR A 1 C41 C 0.6603(2) 0.11789(17) 0.08285(9) 0.0247(9) Uani 0.915(4) 1 d PD A 1 H41 H 0.6718 0.0887 0.0825 0.030 Uiso 0.915(4) 1 calc PR A 1 C42 C 0.70301(16) 0.17901(16) 0.08013(6) 0.0217(7) Uani 0.915(4) 1 d PD A 1 H42 H 0.7437 0.1911 0.0784 0.026 Uiso 0.915(4) 1 calc PR A 1 C43 C 0.68477(16) 0.22119(14) 0.07998(6) 0.0183(7) Uani 0.915(4) 1 d PD A 1 H43 H 0.7132 0.2618 0.0779 0.022 Uiso 0.915(4) 1 calc PR A 1 O5' O 0.6972(9) 0.2809(8) 0.0834(4) 0.0189(5) Uani 0.085(4) 1 d PD A 2 N14' N 0.6638(14) 0.2203(10) 0.0833(6) 0.0168(6) Uani 0.085(4) 1 d PD A 2 C39' C 0.6042(13) 0.1913(15) 0.0879(8) 0.0215(8) Uani 0.085(4) 1 d PD A 2 H39' H 0.5846 0.2129 0.0910 0.026 Uiso 0.085(4) 1 calc PR A 2 C40' C 0.5726(17) 0.1290(15) 0.0881(12) 0.0242(9) Uani 0.085(4) 1 d PD A 2 H40' H 0.5306 0.1084 0.0887 0.029 Uiso 0.085(4) 1 calc PR A 2 C41' C 0.603(2) 0.0970(18) 0.087(3) 0.0247(9) Uani 0.085(4) 1 d PD A 2 H41' H 0.5824 0.0551 0.0879 0.030 Uiso 0.085(4) 1 calc PR A 2 C42' C 0.666(2) 0.1304(17) 0.0852(12) 0.0217(7) Uani 0.085(4) 1 d PD A 2 H42' H 0.6903 0.1139 0.0891 0.026 Uiso 0.085(4) 1 calc PR A 2 C43' C 0.6907(15) 0.1888(15) 0.0770(7) 0.0183(7) Uani 0.085(4) 1 d PD A 2 H43' H 0.7249 0.2059 0.0675 0.022 Uiso 0.085(4) 1 calc PR A 2 C44 C 0.80512(13) 0.37449(13) 0.02637(5) 0.0211(6) Uani 1 1 d . A . H44 H 0.7888 0.3994 0.0240 0.025 Uiso 1 1 calc R . . C45 C 0.86724(14) 0.39843(15) 0.02740(5) 0.0295(7) Uani 1 1 d . . . H45 H 0.8929 0.4398 0.0257 0.035 Uiso 1 1 calc R A . C46 C 0.89126(14) 0.36109(16) 0.03095(5) 0.0295(7) Uani 1 1 d . A . H46 H 0.9328 0.3769 0.0316 0.035 Uiso 1 1 calc R . . C47 C 0.85232(15) 0.30018(16) 0.03342(5) 0.0299(7) Uani 1 1 d . . . H47 H 0.8676 0.2744 0.0359 0.036 Uiso 1 1 calc R A . C48 C 0.79122(14) 0.27708(14) 0.03233(5) 0.0239(6) Uani 1 1 d . A . H48 H 0.7651 0.2357 0.0340 0.029 Uiso 1 1 calc R . . C49 C 0.70058(12) 0.22902(12) -0.02351(5) 0.0180(5) Uani 1 1 d . A . H49 H 0.6620 0.2241 -0.0238 0.022 Uiso 1 1 calc R . . C50 C 0.70787(14) 0.17988(13) -0.02033(5) 0.0222(6) Uani 1 1 d . . . H50 H 0.6742 0.1418 -0.0183 0.027 Uiso 1 1 calc R A . C51 C 0.76505(14) 0.18655(14) -0.02014(5) 0.0235(6) Uani 1 1 d . A . H51 H 0.7702 0.1534 -0.0177 0.028 Uiso 1 1 calc R . . C52 C 0.81419(14) 0.24346(14) -0.02359(5) 0.0250(6) Uani 1 1 d . . . H52 H 0.8530 0.2489 -0.0239 0.030 Uiso 1 1 calc R A . C53 C 0.80563(12) 0.29226(13) -0.02655(5) 0.0194(6) Uani 1 1 d . A . H53 H 0.8388 0.3307 -0.0288 0.023 Uiso 1 1 calc R . . C54 C 0.74958(13) 0.22697(12) -0.08178(5) 0.0187(6) Uani 1 1 d . A . H54 H 0.7156 0.1891 -0.0797 0.022 Uiso 1 1 calc R . . C55 C 0.80575(13) 0.23269(13) -0.08283(5) 0.0225(6) Uani 1 1 d . . . H55 H 0.8098 0.1986 -0.0813 0.027 Uiso 1 1 calc R A . C56 C 0.85660(14) 0.28883(14) -0.08618(5) 0.0253(6) Uani 1 1 d . A . H56 H 0.8949 0.2930 -0.0869 0.030 Uiso 1 1 calc R . . C57 C 0.84903(13) 0.33858(13) -0.08841(5) 0.0237(6) Uani 1 1 d . . . H57 H 0.8825 0.3766 -0.0909 0.028 Uiso 1 1 calc R A . C58 C 0.79222(13) 0.33207(12) -0.08694(5) 0.0193(6) Uani 1 1 d . A . H58 H 0.7874 0.3657 -0.0881 0.023 Uiso 1 1 calc R . . C59 C 0.63752(13) 0.16082(13) -0.13423(5) 0.0219(6) Uani 1 1 d . A . H59 H 0.5961 0.1400 -0.1315 0.026 Uiso 1 1 calc R . . C60 C 0.66897(14) 0.13031(14) -0.13433(5) 0.0256(6) Uani 1 1 d . . . H60 H 0.6487 0.0889 -0.1316 0.031 Uiso 1 1 calc R A . C61 C 0.73033(14) 0.16062(14) -0.13840(5) 0.0254(6) Uani 1 1 d . A . H61 H 0.7517 0.1400 -0.1388 0.030 Uiso 1 1 calc R . . C62 C 0.75942(14) 0.22257(14) -0.14191(5) 0.0238(6) Uani 1 1 d . . . H62 H 0.8010 0.2441 -0.1444 0.029 Uiso 1 1 calc R A . C63 C 0.72703(13) 0.25230(13) -0.14175(5) 0.0196(6) Uani 1 1 d . A . H63 H 0.7466 0.2938 -0.1442 0.023 Uiso 1 1 calc R . . C64 C 0.16461(14) -0.13540(14) -0.06811(5) 0.0285(7) Uani 1 1 d . . . F65 F 0.14061(10) -0.19428(9) -0.07226(4) 0.0417(5) Uani 1 1 d . . . F66 F 0.20427(9) -0.10594(9) -0.08530(3) 0.0343(4) Uani 1 1 d . . . F67 F 0.12108(8) -0.12150(9) -0.06939(4) 0.0384(5) Uani 1 1 d . . . S68 S 0.20048(3) -0.11812(3) -0.038727(12) 0.02159(15) Uani 1 1 d . B . O69 O 0.15064(10) -0.14897(11) -0.02293(4) 0.0331(5) Uani 1 1 d . . . O70 O 0.24339(9) -0.13853(9) -0.04040(4) 0.0256(4) Uani 1 1 d . . . N71 N 0.22802(11) -0.04776(11) -0.03587(4) 0.0249(5) Uani 1 1 d . . . S72 S 0.2973(4) 0.0027(3) -0.04285(12) 0.0184(7) Uani 0.655(3) 1 d PD B 1 O73 O 0.3017(2) 0.0606(2) -0.04463(7) 0.0242(9) Uani 0.655(3) 1 d PD B 1 O74 O 0.3253(3) -0.0141(4) -0.06069(11) 0.0341(14) Uani 0.655(3) 1 d PD B 1 C75 C 0.3385(2) 0.0091(2) -0.01531(9) 0.0276(11) Uani 0.655(3) 1 d PD B 1 F76 F 0.3978(5) 0.0431(6) -0.0194(4) 0.0417(10) Uani 0.655(3) 1 d PD B 1 F77 F 0.32269(13) 0.03395(14) 0.00179(5) 0.0370(7) Uani 0.655(3) 1 d PD B 1 F78 F 0.3285(2) -0.04530(18) -0.00807(9) 0.0521(10) Uani 0.655(3) 1 d PD B 1 S72' S 0.2912(8) -0.0041(7) -0.0419(2) 0.0184(7) Uani 0.345(3) 1 d PD B 2 O73' O 0.2997(5) 0.0534(5) -0.03558(14) 0.0242(9) Uani 0.345(3) 1 d PD B 2 O74' O 0.3100(7) -0.0100(8) -0.0651(2) 0.0341(14) Uani 0.345(3) 1 d PD B 2 C75' C 0.3431(4) -0.0132(4) -0.02220(17) 0.0276(11) Uani 0.345(3) 1 d PD B 2 F76' F 0.3923(10) 0.0403(11) -0.0184(7) 0.0417(10) Uani 0.345(3) 1 d PD B 2 F77' F 0.3173(4) -0.0375(4) -0.00160(12) 0.0370(7) Uani 0.345(3) 1 d PD B 2 F78' F 0.3599(3) -0.0512(3) -0.03049(12) 0.0521(10) Uani 0.345(3) 1 d PD B 2 C79 C 0.44961(14) -0.06213(15) 0.04995(6) 0.0294(7) Uani 1 1 d . . . F80 F 0.50877(9) -0.03843(11) 0.04841(4) 0.0501(6) Uani 1 1 d . . . F81 F 0.42438(9) -0.12234(9) 0.04985(3) 0.0386(5) Uani 1 1 d . . . F82 F 0.43001(9) -0.04641(9) 0.03083(3) 0.0357(4) Uani 1 1 d . . . S83 S 0.43123(3) -0.03606(3) 0.077436(12) 0.02064(14) Uani 1 1 d . . . O84 O 0.45286(10) -0.05936(10) 0.09557(4) 0.0282(5) Uani 1 1 d . . . O85 O 0.45975(9) 0.02792(9) 0.07450(4) 0.0272(5) Uani 1 1 d . . . N86 N 0.35993(11) -0.07157(11) 0.07801(4) 0.0219(5) Uani 1 1 d . . . S87 S 0.31986(3) -0.04580(3) 0.067692(12) 0.01844(14) Uani 1 1 d . . . O88 O 0.25968(9) -0.09554(9) 0.06501(4) 0.0272(5) Uani 1 1 d . . . O89 O 0.34516(10) -0.00293(10) 0.04895(4) 0.0298(5) Uani 1 1 d . . . C90 C 0.31279(14) -0.00322(13) 0.09249(5) 0.0243(6) Uani 1 1 d . . . F91 F 0.28978(10) -0.03829(10) 0.11153(3) 0.0410(5) Uani 1 1 d . . . F92 F 0.36474(9) 0.04402(9) 0.09832(4) 0.0415(5) Uani 1 1 d . . . F93 F 0.27482(8) 0.01570(8) 0.08630(3) 0.0311(4) Uani 1 1 d . . . C94 C 0.53957(13) 0.51410(14) 0.14888(5) 0.0238(6) Uani 1 1 d . . . F95 F 0.49556(8) 0.52756(9) 0.14963(3) 0.0327(4) Uani 1 1 d . . . F96 F 0.58282(8) 0.55379(9) 0.13469(3) 0.0304(4) Uani 1 1 d . . . F97 F 0.51788(10) 0.45997(9) 0.13936(4) 0.0422(5) Uani 1 1 d . . . S98 S 0.56792(3) 0.51446(3) 0.178813(12) 0.01776(14) Uani 1 1 d . . . O99 O 0.60951(9) 0.49296(9) 0.17548(4) 0.0258(5) Uani 1 1 d . . . O100 O 0.51386(9) 0.47829(9) 0.19201(4) 0.0245(4) Uani 1 1 d . . . N101 N 0.59706(10) 0.58203(10) 0.18706(4) 0.0208(5) Uani 1 1 d . . . S102 S 0.66683(3) 0.62830(3) 0.183952(14) 0.02534(16) Uani 1 1 d . . . O103 O 0.70452(11) 0.62070(11) 0.20064(6) 0.0514(8) Uani 1 1 d . . . O104 O 0.68772(12) 0.64073(12) 0.16036(5) 0.0570(9) Uani 1 1 d . . . C105 C 0.66597(14) 0.69510(14) 0.19421(6) 0.0296(7) Uani 1 1 d . . . F106 F 0.72158(9) 0.74183(8) 0.19227(4) 0.0430(5) Uani 1 1 d . . . F107 F 0.65023(11) 0.69114(11) 0.21650(4) 0.0593(7) Uani 1 1 d . . . F108 F 0.62938(11) 0.70599(10) 0.18156(6) 0.0706(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01425(14) 0.01425(14) 0.0149(2) 0.000 0.000 0.00712(7) Ag2 0.01494(11) 0.01494(11) 0.01516(17) 0.000 0.000 0.00747(5) Ag3 0.01309(11) 0.01309(11) 0.01436(16) 0.000 0.000 0.00654(5) Ag4 0.01411(11) 0.01411(11) 0.01518(16) 0.000 0.000 0.00705(5) Ag5 0.01333(11) 0.01333(11) 0.01508(16) 0.000 0.000 0.00667(5) Ag6 0.01386(11) 0.01386(11) 0.01212(16) 0.000 0.000 0.00693(5) Ag7 0.01231(10) 0.01231(10) 0.01232(16) 0.000 0.000 0.00616(5) Ag8 0.01577(11) 0.01577(11) 0.01203(16) 0.000 0.000 0.00788(5) Ag9 0.01620(11) 0.01620(11) 0.01268(16) 0.000 0.000 0.00810(6) Ag10 0.01918(15) 0.01918(15) 0.0123(2) 0.000 0.000 0.00959(8) O1 0.0147(9) 0.0125(9) 0.0257(10) 0.0005(8) -0.0002(8) 0.0030(8) O2 0.0141(9) 0.0199(10) 0.0239(10) -0.0009(8) 0.0004(8) 0.0088(8) O3 0.0109(9) 0.0189(10) 0.0226(10) -0.0009(8) 0.0006(7) 0.0085(8) O4 0.0200(10) 0.0117(9) 0.0232(10) 0.0000(7) 0.0012(8) 0.0083(8) O6 0.0145(9) 0.0221(10) 0.0230(10) -0.0007(8) -0.0002(8) 0.0087(8) O7 0.0211(10) 0.0156(9) 0.0203(9) -0.0009(7) -0.0011(8) 0.0118(8) O8 0.0146(9) 0.0207(10) 0.0209(9) -0.0001(8) -0.0004(7) 0.0093(8) O9 0.0217(10) 0.0216(10) 0.0220(10) 0.0005(8) 0.0010(8) 0.0152(9) N10 0.0152(11) 0.0161(11) 0.0150(10) -0.0011(9) -0.0013(9) 0.0067(9) N11 0.0126(11) 0.0170(11) 0.0154(10) -0.0003(9) -0.0009(8) 0.0066(9) N12 0.0129(10) 0.0146(11) 0.0139(10) -0.0002(8) -0.0001(8) 0.0079(9) N13 0.0164(11) 0.0131(11) 0.0151(10) 0.0008(8) 0.0025(8) 0.0071(9) N15 0.0184(12) 0.0228(12) 0.0145(11) -0.0005(9) 0.0010(9) 0.0119(10) N16 0.0176(11) 0.0180(11) 0.0138(10) -0.0019(9) -0.0013(9) 0.0111(10) N17 0.0163(11) 0.0189(11) 0.0136(10) -0.0005(9) 0.0009(8) 0.0098(10) N18 0.0211(12) 0.0227(12) 0.0126(10) 0.0007(9) 0.0000(9) 0.0142(10) C19 0.0179(14) 0.0205(14) 0.0192(13) -0.0011(11) -0.0002(10) 0.0108(12) C20 0.0237(15) 0.0159(13) 0.0215(14) -0.0017(11) -0.0007(11) 0.0088(12) C21 0.0189(14) 0.0181(14) 0.0219(14) -0.0026(11) -0.0005(11) 0.0023(12) C22 0.0146(13) 0.0272(15) 0.0235(14) -0.0025(12) -0.0020(11) 0.0092(12) C23 0.0193(14) 0.0215(14) 0.0187(13) -0.0022(11) -0.0024(11) 0.0123(12) C24 0.0171(14) 0.0168(13) 0.0256(14) -0.0019(11) -0.0030(11) 0.0074(11) C25 0.0227(15) 0.0256(15) 0.0269(15) -0.0020(12) -0.0009(12) 0.0151(13) C26 0.0159(14) 0.0329(17) 0.0229(14) 0.0003(12) 0.0011(11) 0.0120(13) C27 0.0151(14) 0.0240(15) 0.0252(15) 0.0006(12) -0.0008(11) 0.0040(12) C28 0.0203(14) 0.0169(13) 0.0172(13) -0.0003(10) -0.0009(11) 0.0072(11) C29 0.0165(13) 0.0114(12) 0.0194(13) -0.0006(10) -0.0003(10) 0.0053(11) C30 0.0152(13) 0.0171(14) 0.0258(14) 0.0007(11) 0.0024(11) 0.0060(11) C31 0.0168(13) 0.0254(15) 0.0229(14) -0.0008(11) 0.0003(11) 0.0137(12) C32 0.0218(14) 0.0184(14) 0.0194(13) -0.0015(11) -0.0013(11) 0.0136(12) C33 0.0158(13) 0.0131(12) 0.0160(12) -0.0006(10) 0.0003(10) 0.0053(11) C34 0.0163(13) 0.0185(14) 0.0262(14) -0.0010(11) 0.0016(11) 0.0088(11) C35 0.0229(15) 0.0225(15) 0.0301(15) -0.0006(12) 0.0017(12) 0.0144(13) C36 0.0294(16) 0.0148(14) 0.0330(16) 0.0015(12) 0.0019(13) 0.0115(13) C37 0.0224(15) 0.0157(14) 0.0316(16) 0.0005(12) 0.0002(12) 0.0040(12) C38 0.0156(13) 0.0198(14) 0.0205(13) -0.0004(11) -0.0004(11) 0.0070(11) O5 0.0198(11) 0.0167(11) 0.0232(11) 0.0015(8) -0.0001(8) 0.0114(9) N14 0.0209(17) 0.0136(13) 0.0160(13) 0.0018(10) 0.0003(11) 0.0086(13) C39 0.0216(19) 0.016(2) 0.0234(17) -0.0015(18) -0.0033(15) 0.0066(15) C40 0.0303(18) 0.0149(17) 0.026(2) 0.0015(17) -0.0016(15) 0.0101(15) C41 0.034(2) 0.0170(18) 0.026(2) -0.0075(17) 0.0007(15) 0.0141(18) C42 0.0264(18) 0.0257(19) 0.0180(16) 0.0006(13) 0.0031(13) 0.0166(14) C43 0.0210(17) 0.0168(15) 0.0172(15) 0.0012(12) 0.0027(13) 0.0095(14) O5' 0.0198(11) 0.0167(11) 0.0232(11) 0.0015(8) -0.0001(8) 0.0114(9) N14' 0.0209(17) 0.0136(13) 0.0160(13) 0.0018(10) 0.0003(11) 0.0086(13) C39' 0.0216(19) 0.016(2) 0.0234(17) -0.0015(18) -0.0033(15) 0.0066(15) C40' 0.0303(18) 0.0149(17) 0.026(2) 0.0015(17) -0.0016(15) 0.0101(15) C41' 0.034(2) 0.0170(18) 0.026(2) -0.0075(17) 0.0007(15) 0.0141(18) C42' 0.0264(18) 0.0257(19) 0.0180(16) 0.0006(13) 0.0031(13) 0.0166(14) C43' 0.0210(17) 0.0168(15) 0.0172(15) 0.0012(12) 0.0027(13) 0.0095(14) C44 0.0204(14) 0.0206(14) 0.0220(14) -0.0016(11) -0.0022(11) 0.0101(12) C45 0.0236(16) 0.0327(17) 0.0286(16) -0.0055(13) -0.0027(13) 0.0115(14) C46 0.0203(15) 0.050(2) 0.0232(15) -0.0061(14) -0.0053(12) 0.0214(15) C47 0.0320(17) 0.048(2) 0.0219(15) 0.0010(14) -0.0018(13) 0.0292(16) C48 0.0307(16) 0.0309(16) 0.0182(13) 0.0029(12) 0.0020(12) 0.0216(14) C49 0.0146(13) 0.0213(14) 0.0192(13) -0.0010(11) 0.0005(10) 0.0099(11) C50 0.0261(15) 0.0160(14) 0.0240(14) -0.0019(11) -0.0017(12) 0.0102(12) C51 0.0318(16) 0.0265(15) 0.0222(14) -0.0036(12) -0.0041(12) 0.0221(14) C52 0.0223(15) 0.0351(17) 0.0256(15) -0.0066(13) -0.0038(12) 0.0204(14) C53 0.0136(13) 0.0235(14) 0.0201(13) -0.0043(11) -0.0008(10) 0.0086(11) C54 0.0223(14) 0.0146(13) 0.0181(13) 0.0003(10) 0.0013(11) 0.0084(11) C55 0.0265(15) 0.0180(14) 0.0272(15) 0.0020(11) 0.0046(12) 0.0144(12) C56 0.0213(15) 0.0250(15) 0.0331(16) 0.0023(13) 0.0053(12) 0.0142(13) C57 0.0191(14) 0.0176(14) 0.0297(15) 0.0023(12) 0.0043(12) 0.0056(12) C58 0.0214(14) 0.0161(13) 0.0209(13) 0.0006(11) -0.0008(11) 0.0098(12) C59 0.0205(14) 0.0223(15) 0.0219(14) 0.0017(11) 0.0007(11) 0.0099(12) C60 0.0323(17) 0.0202(15) 0.0262(15) 0.0028(12) 0.0016(13) 0.0146(13) C61 0.0304(16) 0.0305(16) 0.0239(14) 0.0018(12) 0.0018(12) 0.0216(14) C62 0.0218(15) 0.0335(17) 0.0194(14) 0.0005(12) 0.0011(11) 0.0163(13) C63 0.0202(14) 0.0213(14) 0.0160(13) 0.0008(11) 0.0010(11) 0.0095(12) C64 0.0293(17) 0.0268(16) 0.0272(16) -0.0035(13) -0.0059(13) 0.0123(14) F65 0.0487(13) 0.0257(10) 0.0411(11) -0.0097(8) -0.0162(9) 0.0114(9) F66 0.0387(11) 0.0411(11) 0.0222(9) 0.0004(8) -0.0003(8) 0.0193(9) F67 0.0274(10) 0.0470(12) 0.0432(11) 0.0000(9) -0.0098(8) 0.0203(9) S68 0.0193(3) 0.0239(4) 0.0208(3) -0.0006(3) -0.0001(3) 0.0101(3) O69 0.0251(12) 0.0381(13) 0.0299(12) 0.0033(10) 0.0061(9) 0.0112(10) O70 0.0241(11) 0.0226(11) 0.0308(11) 0.0004(9) -0.0013(9) 0.0123(9) N71 0.0199(13) 0.0262(13) 0.0298(13) -0.0081(11) -0.0030(10) 0.0123(11) S72 0.0177(17) 0.0160(17) 0.0204(6) -0.0003(9) -0.0004(8) 0.0074(15) O73 0.0319(14) 0.0180(16) 0.025(3) -0.001(2) -0.009(2) 0.0138(13) O74 0.031(4) 0.0250(17) 0.037(3) -0.004(2) 0.015(2) 0.007(2) C75 0.028(2) 0.014(3) 0.037(3) 0.0006(19) -0.011(2) 0.007(2) F76 0.020(2) 0.0369(16) 0.066(2) -0.0119(14) -0.014(2) 0.0130(13) F77 0.0372(16) 0.0432(17) 0.0199(13) -0.0006(11) -0.0012(11) 0.0120(13) F78 0.061(3) 0.0295(16) 0.066(3) -0.0041(18) -0.033(2) 0.0226(16) S72' 0.0177(17) 0.0160(17) 0.0204(6) -0.0003(9) -0.0004(8) 0.0074(15) O73' 0.0319(14) 0.0180(16) 0.025(3) -0.001(2) -0.009(2) 0.0138(13) O74' 0.031(4) 0.0250(17) 0.037(3) -0.004(2) 0.015(2) 0.007(2) C75' 0.028(2) 0.014(3) 0.037(3) 0.0006(19) -0.011(2) 0.007(2) F76' 0.020(2) 0.0369(16) 0.066(2) -0.0119(14) -0.014(2) 0.0130(13) F77' 0.0372(16) 0.0432(17) 0.0199(13) -0.0006(11) -0.0012(11) 0.0120(13) F78' 0.061(3) 0.0295(16) 0.066(3) -0.0041(18) -0.033(2) 0.0226(16) C79 0.0250(16) 0.0391(19) 0.0284(16) -0.0049(14) -0.0004(13) 0.0193(15) F80 0.0255(10) 0.0783(17) 0.0458(12) -0.0119(11) 0.0075(9) 0.0254(11) F81 0.0469(12) 0.0412(12) 0.0398(11) -0.0132(9) -0.0064(9) 0.0311(10) F82 0.0392(11) 0.0452(12) 0.0241(9) 0.0002(8) 0.0030(8) 0.0220(10) S83 0.0176(3) 0.0235(4) 0.0224(3) 0.0000(3) 0.0006(3) 0.0114(3) O84 0.0308(12) 0.0361(13) 0.0276(11) -0.0007(9) -0.0025(9) 0.0242(10) O85 0.0194(10) 0.0218(11) 0.0359(12) 0.0025(9) -0.0006(9) 0.0070(9) N86 0.0203(12) 0.0198(12) 0.0269(13) 0.0039(10) 0.0039(10) 0.0110(10) S87 0.0165(3) 0.0181(3) 0.0206(3) 0.0009(3) 0.0008(3) 0.0086(3) O88 0.0195(10) 0.0213(11) 0.0380(12) -0.0040(9) 0.0014(9) 0.0082(9) O89 0.0252(11) 0.0352(13) 0.0272(11) 0.0121(9) 0.0025(9) 0.0139(10) C90 0.0257(15) 0.0228(15) 0.0279(15) -0.0017(12) -0.0013(12) 0.0148(13) F91 0.0632(14) 0.0510(13) 0.0275(10) 0.0077(9) 0.0134(9) 0.0426(12) F92 0.0287(10) 0.0365(11) 0.0600(13) -0.0248(10) -0.0146(9) 0.0169(9) F93 0.0276(10) 0.0279(10) 0.0469(11) -0.0010(8) -0.0012(8) 0.0206(8) C94 0.0205(14) 0.0268(16) 0.0237(14) -0.0012(12) -0.0006(11) 0.0114(13) F95 0.0225(9) 0.0517(12) 0.0301(9) 0.0080(8) 0.0008(7) 0.0233(9) F96 0.0246(9) 0.0434(11) 0.0231(9) 0.0076(8) 0.0043(7) 0.0168(9) F97 0.0443(12) 0.0357(11) 0.0396(11) -0.0161(9) -0.0108(9) 0.0147(10) S98 0.0139(3) 0.0147(3) 0.0240(3) 0.0026(3) -0.0003(3) 0.0066(3) O99 0.0205(10) 0.0195(10) 0.0408(12) 0.0013(9) -0.0018(9) 0.0125(9) O100 0.0173(10) 0.0204(10) 0.0311(11) 0.0086(9) 0.0028(8) 0.0058(9) N101 0.0148(11) 0.0159(12) 0.0294(13) -0.0007(10) 0.0011(10) 0.0059(10) S102 0.0163(3) 0.0164(3) 0.0386(4) -0.0049(3) 0.0037(3) 0.0046(3) O103 0.0230(12) 0.0263(13) 0.106(2) 0.0017(14) -0.0184(14) 0.0132(11) O104 0.0419(16) 0.0426(16) 0.0469(16) -0.0155(13) 0.0221(13) -0.0086(13) C105 0.0240(16) 0.0190(15) 0.0457(19) -0.0069(13) -0.0102(14) 0.0108(13) F106 0.0281(10) 0.0185(9) 0.0735(15) -0.0083(9) -0.0072(10) 0.0050(8) F107 0.0499(14) 0.0552(15) 0.0563(15) -0.0283(12) 0.0120(11) 0.0141(12) F108 0.0565(15) 0.0312(12) 0.132(2) -0.0096(14) -0.0481(16) 0.0276(12) _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 Ag2 3.1508(3) . ? Ag1 Ag2 3.1508(3) 16_655 ? Ag1 O1 2.4842(19) 18_545 ? Ag1 O1 2.4842(19) 16_655 ? Ag1 O1 2.4842(19) . ? Ag1 O1 2.4843(19) 3_665 ? Ag1 O1 2.4843(19) 17 ? Ag1 O1 2.4843(19) 2_655 ? Ag2 Ag3 3.1598(4) . ? Ag2 O1 2.4722(19) 2_655 ? Ag2 O1 2.4722(19) 3_665 ? Ag2 O1 2.4723(19) . ? Ag2 O2 2.4905(19) 3_665 ? Ag2 O2 2.4905(19) 2_655 ? Ag2 O2 2.4905(19) . ? Ag3 Ag4 3.2238(4) . ? Ag3 O2 2.4748(19) 3_665 ? Ag3 O2 2.4748(19) . ? Ag3 O2 2.4748(19) 2_655 ? Ag3 O3 2.4665(18) 2_655 ? Ag3 O3 2.4666(18) . ? Ag3 O3 2.4665(18) 3_665 ? Ag4 Ag5 3.0803(4) . ? Ag4 O3 2.4490(18) 3_665 ? Ag4 O3 2.4489(18) . ? Ag4 O3 2.4490(18) 2_655 ? Ag4 O4 2.4918(18) 2_655 ? Ag4 O4 2.4918(18) 3_665 ? Ag4 O4 2.4917(19) . ? Ag5 Ag6 3.0522(4) . ? Ag5 O4 2.4806(19) 3_665 ? Ag5 O4 2.4807(19) 2_655 ? Ag5 O4 2.4807(19) . ? Ag5 O5 2.513(2) 2_655 ? Ag5 O5 2.513(2) . ? Ag5 O5 2.513(2) 3_665 ? Ag5 O5' 2.38(2) . ? Ag5 O5' 2.38(2) 2_655 ? Ag5 O5' 2.38(2) 3_665 ? Ag6 Ag7 3.1935(4) . ? Ag6 O6 2.4587(19) . ? Ag6 O6 2.4586(19) 3_665 ? Ag6 O6 2.4586(19) 2_655 ? Ag6 O5 2.490(2) . ? Ag6 O5 2.490(2) 3_665 ? Ag6 O5 2.490(2) 2_655 ? Ag6 O5' 2.43(2) . ? Ag6 O5' 2.43(2) 2_655 ? Ag6 O5' 2.43(2) 3_665 ? Ag7 Ag8 3.1039(4) . ? Ag7 O6 2.4762(19) 3_665 ? Ag7 O6 2.4762(19) . ? Ag7 O6 2.4762(19) 2_655 ? Ag7 O7 2.4898(19) 2_655 ? Ag7 O7 2.4898(19) 3_665 ? Ag7 O7 2.4897(19) . ? Ag8 Ag9 3.0418(4) . ? Ag8 O7 2.4893(18) 2_655 ? Ag8 O7 2.4893(18) 3_665 ? Ag8 O7 2.4894(18) . ? Ag8 O8 2.4799(19) . ? Ag8 O8 2.4798(19) 2_655 ? Ag8 O8 2.4798(19) 3_665 ? Ag9 Ag10 3.2032(3) . ? Ag9 O8 2.4900(19) 3_665 ? Ag9 O8 2.4900(19) 2_655 ? Ag9 O8 2.4899(19) . ? Ag9 O9 2.4664(19) 2_655 ? Ag9 O9 2.4665(19) . ? Ag9 O9 2.4664(19) 3_665 ? Ag10 Ag9 3.2036(3) 16_654 ? Ag10 O9 2.4698(19) 3_665 ? Ag10 O9 2.4698(19) 2_655 ? Ag10 O9 2.4699(19) 16_654 ? Ag10 O9 2.4700(19) 18_544 ? Ag10 O9 2.4697(19) . ? Ag10 O9 2.4699(19) 17_554 ? O1 N10 1.332(3) . ? O2 N11 1.334(3) . ? O3 N12 1.329(3) . ? O4 N13 1.332(3) . ? O6 N15 1.345(3) . ? O7 N16 1.335(3) . ? O8 N17 1.332(3) . ? O9 N18 1.329(3) . ? N10 C19 1.346(3) . ? N10 C23 1.351(3) . ? N11 C24 1.350(4) . ? N11 C28 1.349(3) . ? N12 C29 1.351(3) . ? N12 C33 1.357(3) . ? N13 C34 1.347(3) . ? N13 C38 1.348(3) . ? N15 C44 1.350(4) . ? N15 C48 1.343(4) . ? N16 C49 1.348(3) . ? N16 C53 1.352(3) . ? N17 C54 1.357(3) . ? N17 C58 1.350(4) . ? N18 C59 1.350(4) . ? N18 C63 1.351(4) . ? C19 H19 0.9300 . ? C19 C20 1.375(4) . ? C20 H20 0.9300 . ? C20 C21 1.381(4) . ? C21 H21 0.9196 . ? C21 C22 1.383(4) . ? C22 H22 0.9300 . ? C22 C23 1.373(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C24 C25 1.378(4) . ? C25 H25 0.9300 . ? C25 C26 1.381(4) . ? C26 H26 0.9300 . ? C26 C27 1.383(4) . ? C27 H27 0.9300 . ? C27 C28 1.371(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C29 C30 1.379(4) . ? C30 H30 0.9300 . ? C30 C31 1.381(4) . ? C31 H31 0.9300 . ? C31 C32 1.388(4) . ? C32 H32 0.9300 . ? C32 C33 1.378(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C34 C35 1.376(4) . ? C35 H35 0.9300 . ? C35 C36 1.377(4) . ? C36 H36 0.9300 . ? C36 C37 1.384(4) . ? C37 H37 0.9300 . ? C37 C38 1.372(4) . ? C38 H38 0.9300 . ? O5 N14 1.335(3) . ? N14 C39 1.354(4) . ? N14 C43 1.346(4) . ? C39 H39 0.9300 . ? C39 C40 1.376(5) . ? C40 H40 0.9300 . ? C40 C41 1.379(5) . ? C41 H41 0.9300 . ? C41 C42 1.396(5) . ? C42 H42 0.9300 . ? C42 C43 1.372(5) . ? C43 H43 0.9300 . ? O5' N14' 1.344(17) . ? N14' C39' 1.344(18) . ? N14' C43' 1.341(18) . ? C39' H39' 0.9300 . ? C39' C40' 1.378(19) . ? C40' H40' 0.9300 . ? C40' C41' 1.38(2) . ? C41' H41' 0.9300 . ? C41' C42' 1.40(2) . ? C42' H42' 0.9300 . ? C42' C43' 1.38(2) . ? C43' H43' 0.9300 . ? C44 H44 0.9300 . ? C44 C45 1.388(4) . ? C45 H45 0.9300 . ? C45 C46 1.383(5) . ? C46 H46 0.9300 . ? C46 C47 1.372(5) . ? C47 H47 0.9300 . ? C47 C48 1.367(4) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C49 C50 1.370(4) . ? C50 H50 0.9300 . ? C50 C51 1.384(4) . ? C51 H51 0.9300 . ? C51 C52 1.380(4) . ? C52 H52 0.9300 . ? C52 C53 1.380(4) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C54 C55 1.370(4) . ? C55 H55 0.9300 . ? C55 C56 1.385(4) . ? C56 H56 0.9300 . ? C56 C57 1.384(4) . ? C57 H57 0.9300 . ? C57 C58 1.379(4) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C59 C60 1.371(4) . ? C60 H60 0.9300 . ? C60 C61 1.377(4) . ? C61 H61 0.9300 . ? C61 C62 1.386(4) . ? C62 H62 0.9300 . ? C62 C63 1.375(4) . ? C63 H63 0.9300 . ? C64 F65 1.331(4) . ? C64 F66 1.331(4) . ? C64 F67 1.328(4) . ? C64 S68 1.838(3) . ? S68 O69 1.426(2) . ? S68 O70 1.434(2) . ? S68 N71 1.578(3) . ? N71 S72 1.634(9) . ? N71 S72' 1.473(19) . ? S72 O73 1.428(6) . ? S72 O74 1.422(7) . ? S72 C75 1.838(7) . ? C75 F76 1.338(11) . ? C75 F77 1.324(6) . ? C75 F78 1.346(6) . ? S72' O73' 1.418(13) . ? S72' O74' 1.426(13) . ? S72' C75' 1.833(12) . ? C75' F76' 1.333(15) . ? C75' F77' 1.328(11) . ? C75' F78' 1.330(11) . ? C79 F80 1.321(4) . ? C79 F81 1.338(4) . ? C79 F82 1.333(4) . ? C79 S83 1.839(3) . ? S83 O84 1.427(2) . ? S83 O85 1.428(2) . ? S83 N86 1.578(2) . ? N86 S87 1.580(2) . ? S87 O88 1.432(2) . ? S87 O89 1.424(2) . ? S87 C90 1.836(3) . ? C90 F91 1.333(4) . ? C90 F92 1.314(4) . ? C90 F93 1.329(3) . ? C94 F95 1.331(3) . ? C94 F96 1.331(3) . ? C94 F97 1.320(4) . ? C94 S98 1.836(3) . ? S98 O99 1.432(2) . ? S98 O100 1.428(2) . ? S98 N101 1.571(2) . ? N101 S102 1.581(2) . ? S102 O103 1.428(3) . ? S102 O104 1.410(3) . ? S102 C105 1.813(3) . ? C105 F106 1.327(4) . ? C105 F107 1.309(4) . ? C105 F108 1.312(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag2 Ag1 Ag2 180.0 . 16_655 ? O1 Ag1 Ag2 129.64(4) 17 . ? O1 Ag1 Ag2 129.64(4) 18_545 . ? O1 Ag1 Ag2 129.64(4) 16_655 . ? O1 Ag1 Ag2 50.36(4) . . ? O1 Ag1 Ag2 50.36(4) 3_665 . ? O1 Ag1 Ag2 50.36(4) 2_655 . ? O1 Ag1 Ag2 50.36(4) 17 16_655 ? O1 Ag1 Ag2 50.36(4) 18_545 16_655 ? O1 Ag1 Ag2 50.36(4) 16_655 16_655 ? O1 Ag1 Ag2 129.64(4) . 16_655 ? O1 Ag1 Ag2 129.64(4) 3_665 16_655 ? O1 Ag1 Ag2 129.64(4) 2_655 16_655 ? O1 Ag1 O1 96.34(7) 3_665 17 ? O1 Ag1 O1 179.996(1) 2_655 17 ? O1 Ag1 O1 96.34(7) . 18_545 ? O1 Ag1 O1 96.34(7) . 17 ? O1 Ag1 O1 83.65(7) . 3_665 ? O1 Ag1 O1 83.66(7) . 2_655 ? O1 Ag1 O1 83.65(7) 3_665 2_655 ? O1 Ag1 O1 179.997(2) 3_665 18_545 ? O1 Ag1 O1 96.35(7) 2_655 16_655 ? O1 Ag1 O1 83.66(7) 18_545 16_655 ? O1 Ag1 O1 83.66(7) 17 16_655 ? O1 Ag1 O1 96.34(7) 3_665 16_655 ? O1 Ag1 O1 96.35(7) 2_655 18_545 ? O1 Ag1 O1 83.66(7) 17 18_545 ? O1 Ag1 O1 179.997(1) . 16_655 ? Ag1 Ag2 Ag3 180.0 . . ? O1 Ag2 Ag1 50.70(4) 2_655 . ? O1 Ag2 Ag1 50.70(4) 3_665 . ? O1 Ag2 Ag1 50.70(4) . . ? O1 Ag2 Ag3 129.30(4) 3_665 . ? O1 Ag2 Ag3 129.30(4) . . ? O1 Ag2 Ag3 129.30(4) 2_655 . ? O1 Ag2 O1 84.15(7) 3_665 . ? O1 Ag2 O1 84.16(7) 3_665 2_655 ? O1 Ag2 O1 84.16(7) . 2_655 ? O1 Ag2 O2 87.91(6) 2_655 2_655 ? O1 Ag2 O2 166.21(6) . 2_655 ? O1 Ag2 O2 87.91(6) . . ? O1 Ag2 O2 166.21(6) 3_665 . ? O1 Ag2 O2 166.21(6) 2_655 3_665 ? O1 Ag2 O2 106.27(6) . 3_665 ? O1 Ag2 O2 106.27(6) 2_655 . ? O1 Ag2 O2 87.91(6) 3_665 3_665 ? O1 Ag2 O2 106.27(6) 3_665 2_655 ? O2 Ag2 Ag1 129.74(4) 2_655 . ? O2 Ag2 Ag1 129.74(4) . . ? O2 Ag2 Ag1 129.74(4) 3_665 . ? O2 Ag2 Ag3 50.26(4) . . ? O2 Ag2 Ag3 50.26(4) 2_655 . ? O2 Ag2 Ag3 50.26(4) 3_665 . ? O2 Ag2 O2 83.51(7) 3_665 2_655 ? O2 Ag2 O2 83.51(6) . 2_655 ? O2 Ag2 O2 83.51(6) 3_665 . ? Ag2 Ag3 Ag4 180.0 . . ? O2 Ag3 Ag2 50.70(4) 2_655 . ? O2 Ag3 Ag2 50.70(4) . . ? O2 Ag3 Ag2 50.70(4) 3_665 . ? O2 Ag3 Ag4 129.30(4) 2_655 . ? O2 Ag3 Ag4 129.30(4) . . ? O2 Ag3 Ag4 129.30(4) 3_665 . ? O2 Ag3 O2 84.16(7) 3_665 . ? O2 Ag3 O2 84.15(7) . 2_655 ? O2 Ag3 O2 84.15(7) 3_665 2_655 ? O3 Ag3 Ag2 131.22(4) 2_655 . ? O3 Ag3 Ag2 131.22(4) . . ? O3 Ag3 Ag2 131.22(4) 3_665 . ? O3 Ag3 Ag4 48.78(4) 2_655 . ? O3 Ag3 Ag4 48.78(4) . . ? O3 Ag3 Ag4 48.78(4) 3_665 . ? O3 Ag3 O2 173.06(6) 2_655 2_655 ? O3 Ag3 O2 93.05(6) . 2_655 ? O3 Ag3 O2 101.91(6) 3_665 2_655 ? O3 Ag3 O2 93.04(6) 2_655 3_665 ? O3 Ag3 O2 101.91(6) . 3_665 ? O3 Ag3 O2 93.04(6) 3_665 . ? O3 Ag3 O2 173.06(6) . . ? O3 Ag3 O2 173.06(6) 3_665 3_665 ? O3 Ag3 O2 101.91(6) 2_655 . ? O3 Ag3 O3 81.30(6) 2_655 . ? O3 Ag3 O3 81.30(6) 2_655 3_665 ? O3 Ag3 O3 81.30(6) . 3_665 ? Ag5 Ag4 Ag3 180.0 . . ? O3 Ag4 Ag3 49.25(4) . . ? O3 Ag4 Ag3 49.25(4) 2_655 . ? O3 Ag4 Ag3 49.25(4) 3_665 . ? O3 Ag4 Ag5 130.75(4) 3_665 . ? O3 Ag4 Ag5 130.75(4) 2_655 . ? O3 Ag4 Ag5 130.75(4) . . ? O3 Ag4 O3 82.01(6) . 2_655 ? O3 Ag4 O3 82.01(6) 2_655 3_665 ? O3 Ag4 O3 82.01(6) . 3_665 ? O3 Ag4 O4 105.68(6) 3_665 2_655 ? O3 Ag4 O4 166.87(6) . . ? O3 Ag4 O4 88.47(6) 2_655 3_665 ? O3 Ag4 O4 105.68(6) . 3_665 ? O3 Ag4 O4 88.47(6) 3_665 . ? O3 Ag4 O4 105.68(6) 2_655 . ? O3 Ag4 O4 166.87(6) 3_665 3_665 ? O3 Ag4 O4 166.87(6) 2_655 2_655 ? O3 Ag4 O4 88.47(6) . 2_655 ? O4 Ag4 Ag3 128.44(4) 2_655 . ? O4 Ag4 Ag3 128.44(4) 3_665 . ? O4 Ag4 Ag3 128.44(4) . . ? O4 Ag4 Ag5 51.56(4) . . ? O4 Ag4 Ag5 51.56(4) 3_665 . ? O4 Ag4 Ag5 51.56(4) 2_655 . ? O4 Ag4 O4 85.43(6) . 3_665 ? O4 Ag4 O4 85.43(6) . 2_655 ? O4 Ag4 O4 85.42(6) 3_665 2_655 ? Ag6 Ag5 Ag4 180.0 . . ? O4 Ag5 Ag4 51.89(4) 2_655 . ? O4 Ag5 Ag4 51.88(4) . . ? O4 Ag5 Ag4 51.89(4) 3_665 . ? O4 Ag5 Ag6 128.11(4) 3_665 . ? O4 Ag5 Ag6 128.11(4) 2_655 . ? O4 Ag5 Ag6 128.12(4) . . ? O4 Ag5 O4 85.90(6) 3_665 . ? O4 Ag5 O4 85.90(6) . 2_655 ? O4 Ag5 O4 85.90(6) 3_665 2_655 ? O4 Ag5 O5 85.88(6) . 2_655 ? O4 Ag5 O5 103.66(6) 3_665 2_655 ? O4 Ag5 O5 85.88(6) 2_655 3_665 ? O4 Ag5 O5 103.66(6) . 3_665 ? O4 Ag5 O5 103.66(6) 2_655 . ? O4 Ag5 O5 166.90(6) . . ? O4 Ag5 O5 85.88(6) 3_665 . ? O4 Ag5 O5 166.90(6) 3_665 3_665 ? O4 Ag5 O5 166.90(6) 2_655 2_655 ? O5 Ag5 Ag4 127.93(5) . . ? O5 Ag5 Ag4 127.93(5) 2_655 . ? O5 Ag5 Ag4 127.93(5) 3_665 . ? O5 Ag5 Ag6 52.07(5) 2_655 . ? O5 Ag5 Ag6 52.07(5) . . ? O5 Ag5 Ag6 52.07(5) 3_665 . ? O5 Ag5 O5 86.17(7) 2_655 . ? O5 Ag5 O5 86.17(7) 2_655 3_665 ? O5 Ag5 O5 86.17(7) . 3_665 ? O5' Ag5 Ag4 128.6(5) . . ? O5' Ag5 Ag4 128.6(5) 2_655 . ? O5' Ag5 Ag4 128.6(5) 3_665 . ? O5' Ag5 Ag6 51.4(5) . . ? O5' Ag5 Ag6 51.4(5) 2_655 . ? O5' Ag5 Ag6 51.4(5) 3_665 . ? O5' Ag5 O4 147.8(5) 3_665 . ? O5' Ag5 O4 147.8(5) . 2_655 ? O5' Ag5 O4 120.5(5) 2_655 2_655 ? O5' Ag5 O4 78.6(5) 3_665 2_655 ? O5' Ag5 O4 78.6(5) . 3_665 ? O5' Ag5 O4 120.5(5) . . ? O5' Ag5 O4 78.6(5) 2_655 . ? O5' Ag5 O4 120.5(5) 3_665 3_665 ? O5' Ag5 O4 147.8(5) 2_655 3_665 ? O5' Ag5 O5 44.8(5) 3_665 . ? O5' Ag5 O5 103.4(5) . 3_665 ? O5' Ag5 O5 44.8(5) 2_655 3_665 ? O5' Ag5 O5 47.6(5) 3_665 3_665 ? O5' Ag5 O5 103.4(5) 2_655 . ? O5' Ag5 O5 44.8(5) . 2_655 ? O5' Ag5 O5 47.6(5) 2_655 2_655 ? O5' Ag5 O5 47.6(5) . . ? O5' Ag5 O5 103.4(5) 3_665 2_655 ? O5' Ag5 O5' 85.1(8) . 2_655 ? O5' Ag5 O5' 85.1(8) . 3_665 ? O5' Ag5 O5' 85.1(8) 2_655 3_665 ? Ag5 Ag6 Ag7 180.0 . . ? O6 Ag6 Ag5 130.09(4) . . ? O6 Ag6 Ag5 130.09(4) 2_655 . ? O6 Ag6 Ag5 130.09(4) 3_665 . ? O6 Ag6 Ag7 49.91(4) . . ? O6 Ag6 Ag7 49.91(4) 3_665 . ? O6 Ag6 Ag7 49.91(4) 2_655 . ? O6 Ag6 O6 82.99(7) . 3_665 ? O6 Ag6 O6 82.99(7) . 2_655 ? O6 Ag6 O6 82.99(7) 3_665 2_655 ? O6 Ag6 O5 89.80(7) . 2_655 ? O6 Ag6 O5 100.58(7) 3_665 3_665 ? O6 Ag6 O5 171.54(6) . 3_665 ? O6 Ag6 O5 100.58(7) . . ? O6 Ag6 O5 89.80(7) 3_665 . ? O6 Ag6 O5 171.54(6) 2_655 . ? O6 Ag6 O5 171.54(6) 3_665 2_655 ? O6 Ag6 O5 100.58(7) 2_655 2_655 ? O6 Ag6 O5 89.80(7) 2_655 3_665 ? O5 Ag6 Ag5 52.75(5) 3_665 . ? O5 Ag6 Ag5 52.75(5) . . ? O5 Ag6 Ag5 52.75(5) 2_655 . ? O5 Ag6 Ag7 127.25(5) 3_665 . ? O5 Ag6 Ag7 127.25(5) . . ? O5 Ag6 Ag7 127.25(5) 2_655 . ? O5 Ag6 O5 87.16(7) . 3_665 ? O5 Ag6 O5 87.16(7) 2_655 3_665 ? O5 Ag6 O5 87.16(7) 2_655 . ? O5' Ag6 Ag5 49.8(5) . . ? O5' Ag6 Ag5 49.8(5) 2_655 . ? O5' Ag6 Ag5 49.8(5) 3_665 . ? O5' Ag6 Ag7 130.2(5) 2_655 . ? O5' Ag6 Ag7 130.2(5) . . ? O5' Ag6 Ag7 130.2(5) 3_665 . ? O5' Ag6 O6 80.6(5) . . ? O5' Ag6 O6 80.6(5) 3_665 3_665 ? O5' Ag6 O6 141.1(5) . 2_655 ? O5' Ag6 O6 129.2(5) 2_655 . ? O5' Ag6 O6 129.2(5) . 3_665 ? O5' Ag6 O6 141.1(5) 2_655 3_665 ? O5' Ag6 O6 141.1(5) 3_665 . ? O5' Ag6 O6 80.6(5) 2_655 2_655 ? O5' Ag6 O6 129.2(5) 3_665 2_655 ? O5' Ag6 O5 47.4(5) 3_665 3_665 ? O5' Ag6 O5 44.6(5) 3_665 . ? O5' Ag6 O5 44.6(5) 2_655 3_665 ? O5' Ag6 O5 102.6(5) . 3_665 ? O5' Ag6 O5 102.6(5) 2_655 . ? O5' Ag6 O5 44.6(5) . 2_655 ? O5' Ag6 O5 47.4(5) 2_655 2_655 ? O5' Ag6 O5 47.4(5) . . ? O5' Ag6 O5 102.6(5) 3_665 2_655 ? O5' Ag6 O5' 82.9(8) . 2_655 ? O5' Ag6 O5' 82.9(8) . 3_665 ? O5' Ag6 O5' 82.9(8) 2_655 3_665 ? Ag8 Ag7 Ag6 180.0 . . ? O6 Ag7 Ag6 49.44(4) . . ? O6 Ag7 Ag6 49.43(4) 2_655 . ? O6 Ag7 Ag6 49.43(4) 3_665 . ? O6 Ag7 Ag8 130.56(4) . . ? O6 Ag7 Ag8 130.57(4) 2_655 . ? O6 Ag7 Ag8 130.57(4) 3_665 . ? O6 Ag7 O6 82.28(7) . 2_655 ? O6 Ag7 O6 82.28(7) 2_655 3_665 ? O6 Ag7 O6 82.28(7) . 3_665 ? O6 Ag7 O7 113.92(6) 3_665 2_655 ? O6 Ag7 O7 83.75(6) 2_655 2_655 ? O6 Ag7 O7 113.92(6) . 3_665 ? O6 Ag7 O7 83.74(6) . . ? O6 Ag7 O7 113.92(6) 2_655 . ? O6 Ag7 O7 156.90(6) 3_665 . ? O6 Ag7 O7 156.90(6) 2_655 3_665 ? O6 Ag7 O7 156.90(6) . 2_655 ? O6 Ag7 O7 83.75(6) 3_665 3_665 ? O7 Ag7 Ag6 128.57(4) 2_655 . ? O7 Ag7 Ag6 128.57(4) 3_665 . ? O7 Ag7 Ag6 128.57(4) . . ? O7 Ag7 Ag8 51.43(4) . . ? O7 Ag7 Ag8 51.43(4) 3_665 . ? O7 Ag7 Ag8 51.43(4) 2_655 . ? O7 Ag7 O7 85.23(6) . 3_665 ? O7 Ag7 O7 85.24(6) . 2_655 ? O7 Ag7 O7 85.23(6) 3_665 2_655 ? Ag9 Ag8 Ag7 180.0 . . ? O7 Ag8 Ag7 51.44(4) . . ? O7 Ag8 Ag7 51.44(4) 3_665 . ? O7 Ag8 Ag7 51.44(4) 2_655 . ? O7 Ag8 Ag9 128.56(4) . . ? O7 Ag8 Ag9 128.56(4) 3_665 . ? O7 Ag8 Ag9 128.56(4) 2_655 . ? O7 Ag8 O7 85.25(6) . 3_665 ? O7 Ag8 O7 85.25(6) . 2_655 ? O7 Ag8 O7 85.25(6) 3_665 2_655 ? O8 Ag8 Ag7 127.59(4) . . ? O8 Ag8 Ag7 127.59(4) 3_665 . ? O8 Ag8 Ag7 127.59(4) 2_655 . ? O8 Ag8 Ag9 52.41(4) 2_655 . ? O8 Ag8 Ag9 52.41(4) 3_665 . ? O8 Ag8 Ag9 52.41(4) . . ? O8 Ag8 O7 168.59(6) . 2_655 ? O8 Ag8 O7 86.91(6) 3_665 3_665 ? O8 Ag8 O7 168.59(6) 2_655 3_665 ? O8 Ag8 O7 86.92(6) . . ? O8 Ag8 O7 102.37(6) 2_655 . ? O8 Ag8 O7 102.37(6) 3_665 2_655 ? O8 Ag8 O7 86.91(6) 2_655 2_655 ? O8 Ag8 O7 168.59(6) 3_665 . ? O8 Ag8 O7 102.37(6) . 3_665 ? O8 Ag8 O8 86.67(6) . 2_655 ? O8 Ag8 O8 86.67(6) . 3_665 ? O8 Ag8 O8 86.67(6) 2_655 3_665 ? Ag8 Ag9 Ag10 180.0 . . ? O8 Ag9 Ag8 52.11(4) 3_665 . ? O8 Ag9 Ag8 52.11(4) 2_655 . ? O8 Ag9 Ag8 52.11(4) . . ? O8 Ag9 Ag10 127.89(4) 2_655 . ? O8 Ag9 Ag10 127.89(4) . . ? O8 Ag9 Ag10 127.89(4) 3_665 . ? O8 Ag9 O8 86.23(6) . 3_665 ? O8 Ag9 O8 86.23(6) 2_655 3_665 ? O8 Ag9 O8 86.23(6) . 2_655 ? O9 Ag9 Ag8 130.41(4) 2_655 . ? O9 Ag9 Ag8 130.42(4) . . ? O9 Ag9 Ag8 130.41(4) 3_665 . ? O9 Ag9 Ag10 49.59(4) 2_655 . ? O9 Ag9 Ag10 49.59(4) 3_665 . ? O9 Ag9 Ag10 49.58(4) . . ? O9 Ag9 O8 84.96(6) 2_655 2_655 ? O9 Ag9 O8 161.28(6) 3_665 . ? O9 Ag9 O8 84.96(6) . . ? O9 Ag9 O8 109.59(6) 2_655 . ? O9 Ag9 O8 161.28(6) . 2_655 ? O9 Ag9 O8 84.96(6) 3_665 3_665 ? O9 Ag9 O8 109.59(6) . 3_665 ? O9 Ag9 O8 109.59(6) 3_665 2_655 ? O9 Ag9 O8 161.28(6) 2_655 3_665 ? O9 Ag9 O9 82.50(7) 2_655 . ? O9 Ag9 O9 82.51(7) 2_655 3_665 ? O9 Ag9 O9 82.50(7) . 3_665 ? Ag9 Ag10 Ag9 180.0 . 16_654 ? O9 Ag10 Ag9 130.51(4) 16_654 . ? O9 Ag10 Ag9 49.49(4) 2_655 . ? O9 Ag10 Ag9 49.49(4) 3_665 . ? O9 Ag10 Ag9 130.51(4) 18_544 . ? O9 Ag10 Ag9 49.50(4) . . ? O9 Ag10 Ag9 130.51(4) 17_554 . ? O9 Ag10 Ag9 49.49(4) 16_654 16_654 ? O9 Ag10 Ag9 130.51(4) 2_655 16_654 ? O9 Ag10 Ag9 130.51(4) 3_665 16_654 ? O9 Ag10 Ag9 49.49(4) 18_544 16_654 ? O9 Ag10 Ag9 130.50(4) . 16_654 ? O9 Ag10 Ag9 49.49(4) 17_554 16_654 ? O9 Ag10 O9 82.37(7) 2_655 3_665 ? O9 Ag10 O9 179.993(1) . 16_654 ? O9 Ag10 O9 82.36(7) 17_554 16_654 ? O9 Ag10 O9 97.63(7) 18_544 2_655 ? O9 Ag10 O9 82.36(7) 18_544 16_654 ? O9 Ag10 O9 97.63(7) 18_544 . ? O9 Ag10 O9 82.36(7) 18_544 17_554 ? O9 Ag10 O9 97.63(7) . 17_554 ? O9 Ag10 O9 82.37(7) . 3_665 ? O9 Ag10 O9 97.64(7) 17_554 3_665 ? O9 Ag10 O9 97.64(7) 16_654 3_665 ? O9 Ag10 O9 180.00(11) 18_544 3_665 ? O9 Ag10 O9 82.37(7) . 2_655 ? O9 Ag10 O9 179.996(1) 17_554 2_655 ? O9 Ag10 O9 97.63(7) 16_654 2_655 ? Ag2 O1 Ag1 78.94(6) . . ? N10 O1 Ag1 116.74(15) . . ? N10 O1 Ag2 118.24(15) . . ? Ag3 O2 Ag2 79.04(6) . . ? N11 O2 Ag2 120.29(15) . . ? N11 O2 Ag3 114.78(14) . . ? Ag4 O3 Ag3 81.97(5) . . ? N12 O3 Ag3 117.88(14) . . ? N12 O3 Ag4 120.34(14) . . ? Ag5 O4 Ag4 76.56(5) . . ? N13 O4 Ag4 120.71(14) . . ? N13 O4 Ag5 116.99(14) . . ? Ag6 O6 Ag7 80.65(6) . . ? N15 O6 Ag6 114.90(14) . . ? N15 O6 Ag7 119.02(15) . . ? Ag8 O7 Ag7 77.13(5) . . ? N16 O7 Ag7 114.06(14) . . ? N16 O7 Ag8 121.62(14) . . ? Ag8 O8 Ag9 75.48(5) . . ? N17 O8 Ag8 120.38(14) . . ? N17 O8 Ag9 116.91(14) . . ? Ag9 O9 Ag10 80.92(6) . . ? N18 O9 Ag9 116.40(15) . . ? N18 O9 Ag10 117.02(15) . . ? O1 N10 C19 120.4(2) . . ? O1 N10 C23 118.8(2) . . ? C19 N10 C23 120.8(2) . . ? O2 N11 C24 120.7(2) . . ? O2 N11 C28 118.4(2) . . ? C28 N11 C24 120.9(2) . . ? O3 N12 C29 118.3(2) . . ? O3 N12 C33 120.4(2) . . ? C29 N12 C33 121.3(2) . . ? O4 N13 C34 120.6(2) . . ? O4 N13 C38 118.6(2) . . ? C34 N13 C38 120.8(2) . . ? O6 N15 C44 119.2(2) . . ? C48 N15 O6 118.8(2) . . ? C48 N15 C44 122.1(2) . . ? O7 N16 C49 120.4(2) . . ? O7 N16 C53 118.8(2) . . ? C49 N16 C53 120.8(2) . . ? O8 N17 C54 118.5(2) . . ? O8 N17 C58 120.4(2) . . ? C58 N17 C54 121.1(2) . . ? O9 N18 C59 118.8(2) . . ? O9 N18 C63 120.1(2) . . ? C59 N18 C63 121.1(2) . . ? N10 C19 H19 119.9 . . ? N10 C19 C20 120.3(3) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.1(3) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 118.4 . . ? C20 C21 C22 118.6(3) . . ? C22 C21 H21 123.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? N10 C23 C22 120.3(3) . . ? N10 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? N11 C24 H24 120.0 . . ? N11 C24 C25 119.9(3) . . ? C25 C24 H24 120.0 . . ? C24 C25 H25 120.0 . . ? C24 C25 C26 120.1(3) . . ? C26 C25 H25 120.0 . . ? C25 C26 H26 120.6 . . ? C25 C26 C27 118.8(3) . . ? C27 C26 H26 120.6 . . ? C26 C27 H27 120.1 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.1 . . ? N11 C28 C27 120.4(3) . . ? N11 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? N12 C29 H29 120.0 . . ? N12 C29 C30 120.0(2) . . ? C30 C29 H29 120.0 . . ? C29 C30 H30 119.9 . . ? C29 C30 C31 120.2(3) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 120.7 . . ? C30 C31 C32 118.6(3) . . ? C32 C31 H31 120.7 . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.3(3) . . ? C33 C32 H32 119.8 . . ? N12 C33 C32 119.5(2) . . ? N12 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? N13 C34 H34 120.1 . . ? N13 C34 C35 119.9(3) . . ? C35 C34 H34 120.1 . . ? C34 C35 H35 119.8 . . ? C34 C35 C36 120.4(3) . . ? C36 C35 H35 119.8 . . ? C35 C36 H36 120.6 . . ? C35 C36 C37 118.7(3) . . ? C37 C36 H36 120.6 . . ? C36 C37 H37 120.2 . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120.2 . . ? N13 C38 C37 120.6(3) . . ? N13 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? Ag6 O5 Ag5 75.18(6) . . ? N14 O5 Ag5 114.17(17) . . ? N14 O5 Ag6 115.94(17) . . ? O5 N14 C39 118.7(3) . . ? O5 N14 C43 120.4(3) . . ? C43 N14 C39 120.9(3) . . ? N14 C39 H39 120.0 . . ? N14 C39 C40 120.0(3) . . ? C40 C39 H39 120.0 . . ? C39 C40 H40 119.8 . . ? C39 C40 C41 120.4(4) . . ? C41 C40 H40 119.8 . . ? C40 C41 H41 120.8 . . ? C40 C41 C42 118.3(4) . . ? C42 C41 H41 120.8 . . ? C41 C42 H42 120.1 . . ? C43 C42 C41 119.8(3) . . ? C43 C42 H42 120.1 . . ? N14 C43 C42 120.5(3) . . ? N14 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? Ag5 O5' Ag6 78.8(6) . . ? N14' O5' Ag5 117.1(17) . . ? N14' O5' Ag6 115.9(19) . . ? O5' N14' C39' 122(2) . . ? C43' N14' O5' 118(2) . . ? C43' N14' C39' 120(2) . . ? N14' C39' H39' 120.5 . . ? N14' C39' C40' 119(2) . . ? C40' C39' H39' 120.5 . . ? C39' C40' H40' 119.8 . . ? C39' C40' C41' 120(3) . . ? C41' C40' H40' 119.8 . . ? C40' C41' H41' 121.3 . . ? C40' C41' C42' 117(3) . . ? C42' C41' H41' 121.3 . . ? C41' C42' H42' 121.7 . . ? C43' C42' C41' 117(3) . . ? C43' C42' H42' 121.7 . . ? N14' C43' C42' 118(2) . . ? N14' C43' H43' 121.0 . . ? C42' C43' H43' 121.0 . . ? N15 C44 H44 120.7 . . ? N15 C44 C45 118.6(3) . . ? C45 C44 H44 120.7 . . ? C44 C45 H45 119.8 . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 120.8 . . ? C47 C46 C45 118.5(3) . . ? C47 C46 H46 120.8 . . ? C46 C47 H47 119.7 . . ? C48 C47 C46 120.6(3) . . ? C48 C47 H47 119.7 . . ? N15 C48 C47 119.8(3) . . ? N15 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? N16 C49 H49 120.0 . . ? N16 C49 C50 120.1(3) . . ? C50 C49 H49 120.0 . . ? C49 C50 H50 119.8 . . ? C49 C50 C51 120.5(3) . . ? C51 C50 H50 119.8 . . ? C50 C51 H51 120.7 . . ? C52 C51 C50 118.5(3) . . ? C52 C51 H51 120.7 . . ? C51 C52 H52 120.1 . . ? C51 C52 C53 119.8(3) . . ? C53 C52 H52 120.1 . . ? N16 C53 C52 120.3(3) . . ? N16 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? N17 C54 H54 120.0 . . ? N17 C54 C55 120.0(3) . . ? C55 C54 H54 120.0 . . ? C54 C55 H55 119.8 . . ? C54 C55 C56 120.5(3) . . ? C56 C55 H55 119.8 . . ? C55 C56 H56 120.8 . . ? C57 C56 C55 118.3(3) . . ? C57 C56 H56 120.8 . . ? C56 C57 H57 119.8 . . ? C58 C57 C56 120.4(3) . . ? C58 C57 H57 119.8 . . ? N17 C58 C57 119.8(3) . . ? N17 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? N18 C59 H59 120.0 . . ? N18 C59 C60 120.0(3) . . ? C60 C59 H59 120.0 . . ? C59 C60 H60 119.8 . . ? C59 C60 C61 120.5(3) . . ? C61 C60 H60 119.8 . . ? C60 C61 H61 120.8 . . ? C60 C61 C62 118.4(3) . . ? C62 C61 H61 120.8 . . ? C61 C62 H62 119.9 . . ? C63 C62 C61 120.2(3) . . ? C63 C62 H62 119.9 . . ? N18 C63 C62 119.8(3) . . ? N18 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? F65 C64 S68 108.8(2) . . ? F66 C64 F65 107.5(3) . . ? F66 C64 S68 112.0(2) . . ? F67 C64 F65 108.6(3) . . ? F67 C64 F66 108.2(3) . . ? F67 C64 S68 111.6(2) . . ? O69 S68 C64 103.34(14) . . ? O69 S68 O70 118.30(14) . . ? O69 S68 N71 109.41(14) . . ? O70 S68 C64 103.51(14) . . ? O70 S68 N71 115.77(13) . . ? N71 S68 C64 104.52(14) . . ? S68 N71 S72 124.4(3) . . ? S72' N71 S68 122.4(5) . . ? S72' N71 S72 2.4(7) . . ? N71 S72 C75 102.3(4) . . ? O73 S72 N71 109.2(5) . . ? O73 S72 C75 102.9(4) . . ? O74 S72 N71 116.3(6) . . ? O74 S72 O73 118.2(6) . . ? O74 S72 C75 105.8(5) . . ? F76 C75 S72 108.9(9) . . ? F76 C75 F78 106.9(9) . . ? F77 C75 S72 111.1(4) . . ? F77 C75 F76 109.5(9) . . ? F77 C75 F78 109.2(5) . . ? F78 C75 S72 111.2(4) . . ? N71 S72' C75' 110.6(9) . . ? O73' S72' N71 105.6(11) . . ? O73' S72' O74' 117.2(13) . . ? O73' S72' C75' 103.4(9) . . ? O74' S72' N71 115.6(12) . . ? O74' S72' C75' 103.9(10) . . ? F76' C75' S72' 109.9(17) . . ? F77' C75' S72' 111.7(9) . . ? F77' C75' F76' 109.4(19) . . ? F77' C75' F78' 103.4(8) . . ? F78' C75' S72' 113.5(8) . . ? F78' C75' F76' 108.8(19) . . ? F80 C79 F81 108.1(3) . . ? F80 C79 F82 108.9(3) . . ? F80 C79 S83 109.3(2) . . ? F81 C79 S83 110.9(2) . . ? F82 C79 F81 107.8(3) . . ? F82 C79 S83 111.8(2) . . ? O84 S83 C79 103.36(14) . . ? O84 S83 O85 118.59(13) . . ? O84 S83 N86 108.79(13) . . ? O85 S83 C79 103.90(14) . . ? O85 S83 N86 116.25(13) . . ? N86 S83 C79 103.86(14) . . ? S83 N86 S87 123.73(15) . . ? N86 S87 C90 104.04(13) . . ? O88 S87 N86 107.54(13) . . ? O88 S87 C90 103.08(13) . . ? O89 S87 N86 117.05(13) . . ? O89 S87 O88 118.53(13) . . ? O89 S87 C90 104.56(14) . . ? F91 C90 S87 110.9(2) . . ? F92 C90 S87 112.4(2) . . ? F92 C90 F91 108.6(3) . . ? F92 C90 F93 108.5(2) . . ? F93 C90 S87 108.8(2) . . ? F93 C90 F91 107.4(2) . . ? F95 C94 S98 110.6(2) . . ? F96 C94 F95 108.0(2) . . ? F96 C94 S98 112.0(2) . . ? F97 C94 F95 108.5(2) . . ? F97 C94 F96 107.9(2) . . ? F97 C94 S98 109.7(2) . . ? O99 S98 C94 104.12(13) . . ? O99 S98 N101 115.20(13) . . ? O100 S98 C94 102.98(13) . . ? O100 S98 O99 118.91(13) . . ? O100 S98 N101 109.31(13) . . ? N101 S98 C94 104.30(14) . . ? S98 N101 S102 121.79(15) . . ? N101 S102 C105 97.39(14) . . ? O103 S102 N101 114.23(15) . . ? O103 S102 C105 104.13(16) . . ? O104 S102 N101 115.57(15) . . ? O104 S102 O103 116.62(19) . . ? O104 S102 C105 105.71(17) . . ? F106 C105 S102 108.0(2) . . ? F107 C105 S102 112.4(2) . . ? F107 C105 F106 107.4(3) . . ? F107 C105 F108 108.4(3) . . ? F108 C105 S102 111.8(2) . . ? F108 C105 F106 108.7(3) . . ? _database_code_depnum_ccdc_archive 'CCDC 958488' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_kb2010 _audit_creation_date 2013-08-09 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H40 Ag3 N8 O8, 3(C F3 O3 S)' _chemical_formula_sum 'C43 H40 Ag3 F9 N8 O17 S3' _chemical_formula_weight 1531.62 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Ag C16 H15 F3 S O3 N3' 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' 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' 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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 7.0275(3) _cell_length_b 25.8608(10) _cell_length_c 14.6674(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.519(3) _cell_angle_gamma 90.00 _cell_volume 2665.49(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8184 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.1360 _cell_measurement_theta_min 2.9950 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.81739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13133 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.78 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 15.9631 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_measured_fraction_theta_max 0.6850 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 -39.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -178.0000 -30.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega -51.00 49.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 -77.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 3 omega 10.00 82.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 57.0000 30.0000 72 #__ type_ start__ end____ width___ exp.time_ 4 omega -20.00 5.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1513 -99.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 5 omega 11.00 36.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.8701 57.0000 -120.0000 25 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1000549000 _diffrn_orient_matrix_UB_12 0.0030107000 _diffrn_orient_matrix_UB_13 -0.0033052000 _diffrn_orient_matrix_UB_21 -0.0123388000 _diffrn_orient_matrix_UB_22 0.0267510000 _diffrn_orient_matrix_UB_23 -0.0088017000 _diffrn_orient_matrix_UB_31 0.0055720000 _diffrn_orient_matrix_UB_32 0.0051963000 _diffrn_orient_matrix_UB_33 0.0474425000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 8638 _reflns_number_total 9023 _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.667 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.088 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 749 _refine_ls_number_reflns 9023 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0311 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+1.0040P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0616 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.34075(5) 0.712089(13) 0.81638(2) 0.01996(9) Uani 1 1 d . . . Ag2 Ag 0.74156(6) 0.665124(16) 0.73672(2) 0.01702(8) Uani 1 1 d . . . Ag3 Ag 1.15696(5) 0.613938(13) 0.67922(2) 0.01892(9) Uani 1 1 d . . . O1 O 0.2309(5) 0.72126(15) 0.9606(2) 0.0266(9) Uani 1 1 d . . . N2 N 0.2962(5) 0.75845(16) 1.0140(3) 0.0162(9) Uani 1 1 d . . . C3 C 0.2859(7) 0.7523(2) 1.1053(3) 0.0225(11) Uani 1 1 d . . . H3 H 0.2347 0.7221 1.1292 0.027 Uiso 1 1 calc R . . C4 C 0.3505(7) 0.7903(2) 1.1631(3) 0.0244(12) Uani 1 1 d . . . H4 H 0.3466 0.7851 1.2258 0.029 Uiso 1 1 calc R . . C5 C 0.4211(7) 0.8363(2) 1.1293(4) 0.0260(12) Uani 1 1 d . . . H5 H 0.4641 0.8623 1.1681 0.031 Uiso 1 1 calc R . . C6 C 0.4255(7) 0.8423(2) 1.0351(4) 0.0256(12) Uani 1 1 d . . . H6 H 0.4719 0.8727 1.0100 0.031 Uiso 1 1 calc R . . C7 C 0.3617(6) 0.80333(19) 0.9793(3) 0.0184(11) Uani 1 1 d . . . H7 H 0.3636 0.8079 0.9164 0.022 Uiso 1 1 calc R . . O8 O 0.6804(5) 0.70540(13) 0.8869(2) 0.0183(7) Uani 1 1 d . . . N9 N 0.7611(5) 0.74934(15) 0.9149(3) 0.0132(9) Uani 1 1 d . . . C10 C 0.7990(7) 0.7559(2) 1.0051(3) 0.0172(11) Uani 1 1 d . . . H10 H 0.7723 0.7295 1.0460 0.021 Uiso 1 1 calc R . . C11 C 0.8770(7) 0.8017(2) 1.0362(3) 0.0216(12) Uani 1 1 d . . . H11 H 0.8994 0.8064 1.0982 0.026 Uiso 1 1 calc R . . C12 C 0.9215(7) 0.8402(2) 0.9757(3) 0.0219(11) Uani 1 1 d . . . H12 H 0.9757 0.8709 0.9959 0.026 Uiso 1 1 calc R . . C13 C 0.8840(6) 0.83235(19) 0.8836(3) 0.0204(11) Uani 1 1 d . . . H13 H 0.9156 0.8577 0.8414 0.024 Uiso 1 1 calc R . . C14 C 0.8004(7) 0.78728(19) 0.8549(3) 0.0186(11) Uani 1 1 d . . . H14 H 0.7705 0.7828 0.7935 0.022 Uiso 1 1 calc R . . O15 O 0.4301(5) 0.62149(13) 0.7827(2) 0.0170(8) Uani 1 1 d . . . N16 N 0.4752(6) 0.58340(16) 0.8400(3) 0.0156(9) Uani 1 1 d . . . C17 C 0.4794(7) 0.53466(18) 0.8085(3) 0.0206(11) Uani 1 1 d . . . H17 H 0.4436 0.5280 0.7484 0.025 Uiso 1 1 calc R . . C18 C 0.5355(7) 0.49468(19) 0.8635(3) 0.0232(11) Uani 1 1 d . . . H18 H 0.5394 0.4612 0.8405 0.028 Uiso 1 1 calc R . . C19 C 0.5863(7) 0.50387(19) 0.9534(3) 0.0222(11) Uani 1 1 d . . . H19 H 0.6261 0.4771 0.9914 0.027 Uiso 1 1 calc R . . C20 C 0.5760(7) 0.5548(2) 0.9853(3) 0.0221(12) Uani 1 1 d . . . H20 H 0.6054 0.5622 1.0459 0.027 Uiso 1 1 calc R . . C21 C 0.5224(7) 0.5936(2) 0.9273(3) 0.0157(10) Uani 1 1 d . . . H21 H 0.5186 0.6275 0.9484 0.019 Uiso 1 1 calc R . . O22 O 0.5517(5) 0.74075(14) 0.6934(2) 0.0193(8) Uani 1 1 d . . . N23 N 0.5439(6) 0.76096(17) 0.6103(3) 0.0157(9) Uani 1 1 d . . . C24 C 0.5782(7) 0.81186(19) 0.6000(3) 0.0186(10) Uani 1 1 d . . . H24 H 0.6000 0.8323 0.6512 0.022 Uiso 1 1 calc R . . C25 C 0.5814(7) 0.8340(2) 0.5149(3) 0.0254(12) Uani 1 1 d . . . H25 H 0.6057 0.8691 0.5086 0.030 Uiso 1 1 calc R . . C26 C 0.5483(7) 0.8038(2) 0.4389(4) 0.0283(13) Uani 1 1 d . . . H26 H 0.5513 0.8181 0.3808 0.034 Uiso 1 1 calc R . . C27 C 0.5109(7) 0.7521(2) 0.4510(3) 0.0250(12) Uani 1 1 d . . . H27 H 0.4856 0.7314 0.4005 0.030 Uiso 1 1 calc R . . C28 C 0.5105(6) 0.7304(2) 0.5374(3) 0.0203(11) Uani 1 1 d . . . H28 H 0.4875 0.6953 0.5450 0.024 Uiso 1 1 calc R . . O29 O 1.0704(5) 0.70777(14) 0.7145(2) 0.0187(8) Uani 1 1 d . . . N30 N 1.0663(6) 0.74336(15) 0.6475(3) 0.0141(9) Uani 1 1 d . . . C31 C 1.0123(7) 0.72960(19) 0.5630(3) 0.0152(10) Uani 1 1 d . . . H31 H 0.9794 0.6955 0.5506 0.018 Uiso 1 1 calc R . . C32 C 1.0058(6) 0.76602(19) 0.4949(3) 0.0169(10) Uani 1 1 d . . . H32 H 0.9661 0.7566 0.4366 0.020 Uiso 1 1 calc R . . C33 C 1.0577(6) 0.8165(2) 0.5127(3) 0.0220(11) Uani 1 1 d . . . H33 H 1.0557 0.8413 0.4667 0.026 Uiso 1 1 calc R . . C34 C 1.1130(6) 0.82954(19) 0.6010(3) 0.0204(11) Uani 1 1 d . . . H34 H 1.1471 0.8634 0.6146 0.025 Uiso 1 1 calc R . . C35 C 1.1177(6) 0.79262(19) 0.6679(3) 0.0171(10) Uani 1 1 d . . . H35 H 1.1557 0.8013 0.7268 0.021 Uiso 1 1 calc R . . O36 O 0.9372(5) 0.59073(13) 0.7903(2) 0.0167(7) Uani 1 1 d . . . N37 N 0.9928(6) 0.57952(16) 0.8756(3) 0.0153(9) Uani 1 1 d . . . C38 C 1.0315(6) 0.53018(18) 0.8963(3) 0.0160(10) Uani 1 1 d . . . H38 H 1.0251 0.5050 0.8512 0.019 Uiso 1 1 calc R . . C39 C 1.0804(7) 0.5167(2) 0.9841(3) 0.0227(11) Uani 1 1 d . . . H39 H 1.1062 0.4823 0.9985 0.027 Uiso 1 1 calc R . . C40 C 1.0912(7) 0.5542(2) 1.0508(3) 0.0269(12) Uani 1 1 d . . . H40 H 1.1218 0.5455 1.1107 0.032 Uiso 1 1 calc R . . C41 C 1.0560(7) 0.6048(2) 1.0271(3) 0.0257(12) Uani 1 1 d . . . H41 H 1.0654 0.6306 1.0711 0.031 Uiso 1 1 calc R . . C42 C 1.0068(7) 0.6176(2) 0.9386(3) 0.0208(11) Uani 1 1 d . . . H42 H 0.9837 0.6518 0.9226 0.025 Uiso 1 1 calc R . . O43 O 0.8268(5) 0.62418(13) 0.5950(2) 0.0195(8) Uani 1 1 d . . . N44 N 0.7502(5) 0.58123(16) 0.5595(3) 0.0147(9) Uani 1 1 d . . . C45 C 0.6930(7) 0.58146(19) 0.4716(3) 0.0169(11) Uani 1 1 d . . . H45 H 0.7018 0.6117 0.4376 0.020 Uiso 1 1 calc R . . C46 C 0.6225(7) 0.53774(19) 0.4321(3) 0.0183(11) Uani 1 1 d . . . H46 H 0.5822 0.5383 0.3716 0.022 Uiso 1 1 calc R . . C47 C 0.6106(7) 0.4922(2) 0.4821(3) 0.0211(11) Uani 1 1 d . . . H47 H 0.5638 0.4621 0.4556 0.025 Uiso 1 1 calc R . . C48 C 0.6698(7) 0.49283(19) 0.5717(3) 0.0224(11) Uani 1 1 d . . . H48 H 0.6609 0.4630 0.6068 0.027 Uiso 1 1 calc R . . C49 C 0.7424(7) 0.5376(2) 0.6099(3) 0.0211(12) Uani 1 1 d . . . H49 H 0.7856 0.5377 0.6700 0.025 Uiso 1 1 calc R . . O50 O 1.2893(5) 0.61814(15) 0.5404(2) 0.0227(8) Uani 1 1 d . . . N51 N 1.2122(5) 0.58918(16) 0.4748(3) 0.0170(9) Uani 1 1 d . . . C52 C 1.1842(6) 0.6098(2) 0.3913(3) 0.0194(10) Uani 1 1 d . . . H52 H 1.2133 0.6444 0.3813 0.023 Uiso 1 1 calc R . . C53 C 1.1137(7) 0.58057(19) 0.3215(3) 0.0217(11) Uani 1 1 d . . . H53 H 1.0969 0.5952 0.2641 0.026 Uiso 1 1 calc R . . C54 C 1.0669(7) 0.5292(2) 0.3356(3) 0.0204(11) Uani 1 1 d . . . H54 H 1.0188 0.5089 0.2884 0.025 Uiso 1 1 calc R . . C55 C 1.0939(7) 0.50883(19) 0.4227(3) 0.0212(11) Uani 1 1 d . . . H55 H 1.0630 0.4745 0.4344 0.025 Uiso 1 1 calc R . . C56 C 1.1653(7) 0.53906(19) 0.4905(3) 0.0162(10) Uani 1 1 d . . . H56 H 1.1823 0.5252 0.5486 0.019 Uiso 1 1 calc R . . S57 S 0.19457(17) 0.43206(5) 0.67143(8) 0.0174(3) Uani 1 1 d . . . O58 O 0.1399(5) 0.41858(13) 0.5794(2) 0.0242(8) Uani 1 1 d . . . O59 O 0.1544(5) 0.48474(13) 0.6967(2) 0.0210(8) Uani 1 1 d . . . O60 O 0.3783(5) 0.41346(13) 0.7003(2) 0.0278(8) Uani 1 1 d . . . C61 C 0.0312(7) 0.3948(2) 0.7415(4) 0.0261(12) Uani 1 1 d . . . F62 F -0.1502(4) 0.40818(14) 0.7250(3) 0.0509(10) Uani 1 1 d . . . F63 F 0.0470(5) 0.34428(12) 0.7271(2) 0.0361(8) Uani 1 1 d . . . F64 F 0.0644(5) 0.40305(13) 0.8305(2) 0.0423(9) Uani 1 1 d . . . S65 S 0.68276(18) 0.41817(5) 0.20481(8) 0.0212(3) Uani 1 1 d . . . O66 O 0.7727(5) 0.43469(16) 0.1223(2) 0.0356(10) Uani 1 1 d . . . O67 O 0.7658(5) 0.43723(14) 0.2881(2) 0.0346(9) Uani 1 1 d . . . O68 O 0.6292(5) 0.36430(13) 0.2065(2) 0.0254(8) Uani 1 1 d . . . C69 C 0.4532(7) 0.45058(19) 0.2015(4) 0.0246(12) Uani 1 1 d . . . F70 F 0.4704(5) 0.50178(11) 0.2033(2) 0.0351(8) Uani 1 1 d . . . F71 F 0.3455(5) 0.43633(14) 0.2717(2) 0.0454(9) Uani 1 1 d . . . F72 F 0.3552(4) 0.43911(12) 0.1252(2) 0.0340(7) Uani 1 1 d . . . S73 S 0.81174(17) 0.69501(5) 0.25332(8) 0.0183(3) Uani 1 1 d . . . O74 O 0.7326(5) 0.74483(13) 0.2329(2) 0.0274(9) Uani 1 1 d . . . O75 O 0.9757(5) 0.68148(14) 0.2001(2) 0.0283(9) Uani 1 1 d . . . O76 O 0.8252(5) 0.68192(13) 0.3485(2) 0.0233(8) Uani 1 1 d . . . C77 C 0.6303(7) 0.6503(2) 0.2112(3) 0.0262(12) Uani 1 1 d . . . F78 F 0.5974(4) 0.65625(12) 0.12138(18) 0.0321(8) Uani 1 1 d . . . F79 F 0.4636(4) 0.65838(15) 0.2528(2) 0.0459(9) Uani 1 1 d . . . F80 F 0.6806(5) 0.60125(12) 0.2247(2) 0.0420(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0181(2) 0.0257(2) 0.01607(18) -0.00260(18) -0.00134(15) 0.00196(18) Ag2 0.01641(15) 0.01605(16) 0.01867(18) 0.00161(17) 0.00417(14) 0.00105(14) Ag3 0.0177(2) 0.0258(2) 0.01324(17) -0.00073(17) -0.00063(15) 0.00090(18) O1 0.027(2) 0.031(2) 0.0217(18) -0.0081(17) 0.0029(15) -0.0086(18) N2 0.0108(19) 0.020(2) 0.017(2) -0.0003(19) 0.0045(16) -0.0019(18) C3 0.025(3) 0.022(3) 0.020(3) 0.002(2) 0.002(2) 0.003(2) C4 0.018(3) 0.038(3) 0.017(2) -0.001(3) -0.002(2) 0.003(3) C5 0.021(3) 0.025(3) 0.031(3) -0.005(3) 0.000(2) 0.003(2) C6 0.018(3) 0.022(3) 0.037(3) 0.002(3) 0.001(2) -0.002(2) C7 0.011(2) 0.022(3) 0.022(3) 0.006(2) 0.003(2) 0.002(2) O8 0.0224(19) 0.0154(18) 0.0171(16) 0.0003(15) 0.0010(14) -0.0041(16) N9 0.0101(19) 0.015(2) 0.015(2) 0.0022(17) -0.0060(16) -0.0006(17) C10 0.014(2) 0.021(3) 0.016(3) 0.003(2) 0.005(2) -0.001(2) C11 0.013(2) 0.031(3) 0.021(3) -0.009(2) -0.004(2) 0.004(2) C12 0.015(2) 0.019(3) 0.032(3) -0.008(2) 0.002(2) 0.002(2) C13 0.014(2) 0.021(3) 0.027(3) 0.003(2) 0.001(2) -0.001(2) C14 0.015(2) 0.021(3) 0.020(3) 0.004(2) 0.002(2) -0.002(2) O15 0.0149(18) 0.018(2) 0.0178(17) 0.0034(15) -0.0072(14) -0.0009(15) N16 0.015(2) 0.019(2) 0.0122(19) 0.0027(18) 0.0027(16) -0.0018(18) C17 0.020(3) 0.019(3) 0.022(3) -0.007(2) 0.000(2) -0.003(2) C18 0.026(3) 0.015(2) 0.029(3) 0.001(2) 0.001(2) -0.002(2) C19 0.019(3) 0.020(3) 0.027(3) 0.006(2) 0.004(2) 0.000(2) C20 0.021(3) 0.029(3) 0.016(3) 0.005(2) -0.003(2) -0.007(2) C21 0.013(2) 0.019(3) 0.015(2) -0.002(2) 0.0012(19) -0.004(2) O22 0.0214(19) 0.0240(19) 0.0125(16) 0.0062(15) 0.0007(14) 0.0069(16) N23 0.012(2) 0.022(2) 0.013(2) -0.0002(19) -0.0023(16) 0.0033(18) C24 0.017(2) 0.014(2) 0.025(3) -0.001(2) 0.005(2) 0.000(2) C25 0.023(3) 0.021(3) 0.032(3) 0.010(2) 0.010(2) 0.004(2) C26 0.016(3) 0.047(4) 0.023(3) 0.018(3) 0.001(2) 0.004(3) C27 0.014(2) 0.044(4) 0.017(3) -0.006(3) 0.002(2) 0.002(2) C28 0.013(2) 0.023(3) 0.024(3) -0.002(2) -0.002(2) -0.002(2) O29 0.0214(19) 0.0190(19) 0.0157(16) 0.0031(17) 0.0022(14) 0.0005(17) N30 0.015(2) 0.013(2) 0.014(2) -0.0006(17) 0.0020(16) 0.0014(17) C31 0.015(2) 0.014(2) 0.017(2) -0.003(2) 0.0029(19) -0.004(2) C32 0.013(2) 0.022(3) 0.016(2) -0.001(2) 0.0017(19) -0.001(2) C33 0.018(2) 0.022(3) 0.026(3) 0.006(2) 0.004(2) -0.002(2) C34 0.013(2) 0.018(3) 0.030(3) -0.005(2) 0.003(2) 0.000(2) C35 0.009(2) 0.022(3) 0.020(3) -0.004(2) -0.0014(19) -0.001(2) O36 0.0183(18) 0.0220(18) 0.0098(15) 0.0035(14) -0.0020(13) 0.0034(15) N37 0.014(2) 0.019(2) 0.013(2) -0.0013(18) 0.0012(16) 0.0021(18) C38 0.016(2) 0.014(2) 0.018(2) -0.004(2) 0.0045(19) -0.002(2) C39 0.026(3) 0.019(3) 0.023(3) 0.005(2) -0.001(2) 0.005(2) C40 0.029(3) 0.042(3) 0.010(2) -0.002(2) 0.001(2) 0.000(3) C41 0.026(3) 0.029(3) 0.022(3) -0.010(3) -0.001(2) 0.005(2) C42 0.021(2) 0.019(3) 0.023(2) -0.007(2) 0.004(2) -0.001(2) O43 0.0210(19) 0.019(2) 0.0184(17) -0.0038(15) 0.0013(14) -0.0068(16) N44 0.014(2) 0.017(2) 0.013(2) -0.0011(17) 0.0016(16) -0.0010(17) C45 0.017(2) 0.020(3) 0.014(2) 0.002(2) 0.0040(19) 0.005(2) C46 0.016(3) 0.023(3) 0.016(2) 0.000(2) 0.001(2) -0.005(2) C47 0.018(2) 0.019(3) 0.027(3) -0.005(2) 0.002(2) -0.003(2) C48 0.026(3) 0.016(3) 0.025(3) 0.005(2) 0.004(2) -0.003(2) C49 0.018(3) 0.028(3) 0.017(2) 0.004(2) 0.006(2) 0.000(2) O50 0.0208(18) 0.029(2) 0.0182(17) -0.0075(17) 0.0030(14) -0.0057(17) N51 0.015(2) 0.018(2) 0.018(2) 0.0001(19) 0.0074(17) -0.0016(18) C52 0.021(2) 0.015(2) 0.022(2) 0.002(2) 0.004(2) -0.001(2) C53 0.022(3) 0.025(3) 0.017(2) 0.000(2) 0.001(2) 0.007(2) C54 0.017(3) 0.024(3) 0.020(2) -0.006(2) 0.000(2) 0.004(2) C55 0.017(2) 0.019(3) 0.028(3) 0.002(2) 0.006(2) 0.002(2) C56 0.014(2) 0.016(3) 0.018(2) 0.004(2) 0.0036(19) 0.002(2) S57 0.0221(6) 0.0153(6) 0.0148(6) 0.0006(5) 0.0002(5) 0.0005(5) O58 0.036(2) 0.0190(19) 0.0174(17) -0.0042(16) 0.0014(15) 0.0009(16) O59 0.0275(19) 0.0192(18) 0.0163(17) -0.0014(15) -0.0011(14) 0.0015(16) O60 0.0244(19) 0.027(2) 0.032(2) 0.0032(18) -0.0027(16) 0.0052(17) C61 0.028(3) 0.022(3) 0.028(3) 0.008(3) 0.002(2) 0.004(2) F62 0.0235(17) 0.060(3) 0.069(3) 0.034(2) 0.0113(17) 0.0060(18) F63 0.049(2) 0.0198(16) 0.0397(19) 0.0061(15) -0.0006(16) -0.0056(16) F64 0.071(2) 0.0355(19) 0.0205(16) 0.0071(15) 0.0147(16) 0.0034(18) S65 0.0236(7) 0.0203(7) 0.0197(6) 0.0021(6) -0.0024(5) 0.0039(6) O66 0.031(2) 0.045(2) 0.030(2) 0.016(2) 0.0074(17) 0.011(2) O67 0.046(2) 0.026(2) 0.031(2) 0.0010(18) -0.0206(18) -0.0009(19) O68 0.036(2) 0.0163(18) 0.0233(19) -0.0009(17) -0.0026(16) 0.0090(17) C69 0.026(3) 0.020(3) 0.027(3) -0.002(2) 0.000(2) 0.004(2) F70 0.048(2) 0.0175(16) 0.0397(19) -0.0024(15) -0.0066(16) 0.0065(15) F71 0.049(2) 0.044(2) 0.044(2) 0.0119(18) 0.0269(17) 0.0140(18) F72 0.0275(16) 0.0345(18) 0.0397(19) 0.0014(16) -0.0124(14) 0.0003(15) S73 0.0233(6) 0.0170(6) 0.0147(6) -0.0004(5) 0.0025(5) -0.0024(5) O74 0.039(2) 0.0187(19) 0.0248(19) 0.0037(16) -0.0041(17) 0.0022(17) O75 0.031(2) 0.029(2) 0.0255(19) -0.0031(17) 0.0120(16) -0.0057(17) O76 0.034(2) 0.023(2) 0.0125(16) 0.0001(15) 0.0006(15) 0.0011(16) C77 0.028(3) 0.030(3) 0.020(3) 0.003(2) 0.001(2) -0.011(2) F78 0.0458(19) 0.0315(18) 0.0187(14) -0.0011(14) -0.0072(13) -0.0114(16) F79 0.0321(18) 0.068(3) 0.0376(18) -0.006(2) 0.0094(15) -0.0198(19) F80 0.067(2) 0.0188(17) 0.0396(19) 0.0045(15) -0.0114(17) -0.0164(17) _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 Ag2 3.2915(5) . ? Ag1 O1 2.271(3) . ? Ag1 O8 2.599(3) . ? Ag1 O15 2.477(3) . ? Ag1 O22 2.459(3) . ? Ag1 O29 2.409(3) 1_455 ? Ag2 Ag3 3.3211(5) . ? Ag2 O8 2.478(3) . ? Ag2 O15 2.559(3) . ? Ag2 O22 2.448(3) . ? Ag2 O29 2.584(3) . ? Ag2 O36 2.488(3) . ? Ag2 O43 2.413(3) . ? Ag3 O15 2.444(3) 1_655 ? Ag3 O29 2.556(4) . ? Ag3 O36 2.333(3) . ? Ag3 O43 2.632(3) . ? Ag3 O50 2.248(3) . ? O1 N2 1.320(5) . ? N2 C3 1.352(6) . ? N2 C7 1.350(6) . ? C3 H3 0.9300 . ? C3 C4 1.373(7) . ? C4 H4 0.9300 . ? C4 C5 1.382(7) . ? C5 H5 0.9300 . ? C5 C6 1.390(7) . ? C6 H6 0.9300 . ? C6 C7 1.371(7) . ? C7 H7 0.9300 . ? O8 N9 1.333(5) . ? N9 C10 1.357(6) . ? N9 C14 1.349(6) . ? C10 H10 0.9300 . ? C10 C11 1.380(7) . ? C11 H11 0.9300 . ? C11 C12 1.371(7) . ? C12 H12 0.9300 . ? C12 C13 1.388(7) . ? C13 H13 0.9300 . ? C13 C14 1.370(7) . ? C14 H14 0.9300 . ? O15 Ag3 2.444(3) 1_455 ? O15 N16 1.331(5) . ? N16 C17 1.343(6) . ? N16 C21 1.347(6) . ? C17 H17 0.9300 . ? C17 C18 1.367(7) . ? C18 H18 0.9300 . ? C18 C19 1.383(7) . ? C19 H19 0.9300 . ? C19 C20 1.401(7) . ? C20 H20 0.9300 . ? C20 C21 1.366(7) . ? C21 H21 0.9300 . ? O22 N23 1.327(5) . ? N23 C24 1.347(6) . ? N23 C28 1.348(6) . ? C24 H24 0.9300 . ? C24 C25 1.373(7) . ? C25 H25 0.9300 . ? C25 C26 1.378(7) . ? C26 H26 0.9300 . ? C26 C27 1.374(8) . ? C27 H27 0.9300 . ? C27 C28 1.387(7) . ? C28 H28 0.9300 . ? O29 Ag1 2.409(3) 1_655 ? O29 N30 1.347(5) . ? N30 C31 1.341(6) . ? N30 C35 1.357(6) . ? C31 H31 0.9300 . ? C31 C32 1.373(7) . ? C32 H32 0.9300 . ? C32 C33 1.380(7) . ? C33 H33 0.9300 . ? C33 C34 1.390(7) . ? C34 H34 0.9300 . ? C34 C35 1.369(7) . ? C35 H35 0.9300 . ? O36 N37 1.339(5) . ? N37 C38 1.339(6) . ? N37 C42 1.354(6) . ? C38 H38 0.9300 . ? C38 C39 1.375(6) . ? C39 H39 0.9300 . ? C39 C40 1.380(7) . ? C40 H40 0.9300 . ? C40 C41 1.375(8) . ? C41 H41 0.9300 . ? C41 C42 1.380(6) . ? C42 H42 0.9300 . ? O43 N44 1.338(5) . ? N44 C45 1.347(6) . ? N44 C49 1.351(6) . ? C45 H45 0.9300 . ? C45 C46 1.361(7) . ? C46 H46 0.9300 . ? C46 C47 1.390(7) . ? C47 H47 0.9300 . ? C47 C48 1.375(7) . ? C48 H48 0.9300 . ? C48 C49 1.382(7) . ? C49 H49 0.9300 . ? O50 N51 1.332(5) . ? N51 C52 1.348(6) . ? N51 C56 1.358(6) . ? C52 H52 0.9300 . ? C52 C53 1.363(7) . ? C53 H53 0.9300 . ? C53 C54 1.386(7) . ? C54 H54 0.9300 . ? C54 C55 1.392(7) . ? C55 H55 0.9300 . ? C55 C56 1.358(7) . ? C56 H56 0.9300 . ? S57 O58 1.442(3) . ? S57 O59 1.440(4) . ? S57 O60 1.438(3) . ? S57 C61 1.823(5) . ? C61 F62 1.341(6) . ? C61 F63 1.328(6) . ? C61 F64 1.342(6) . ? S65 O66 1.435(4) . ? S65 O67 1.437(4) . ? S65 O68 1.443(4) . ? S65 C69 1.818(5) . ? C69 F70 1.330(6) . ? C69 F71 1.335(6) . ? C69 F72 1.342(6) . ? S73 O74 1.434(4) . ? S73 O75 1.441(3) . ? S73 O76 1.439(3) . ? S73 C77 1.824(5) . ? C77 F78 1.344(5) . ? C77 F79 1.342(6) . ? C77 F80 1.332(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 Ag1 Ag2 131.95(10) . . ? O1 Ag1 O8 87.41(11) . . ? O1 Ag1 O15 111.94(13) . . ? O1 Ag1 O22 149.78(13) . . ? O1 Ag1 O29 108.04(12) . 1_455 ? O8 Ag1 Ag2 48.00(7) . . ? O15 Ag1 Ag2 50.27(8) . . ? O15 Ag1 O8 77.46(11) . . ? O22 Ag1 Ag2 47.74(8) . . ? O22 Ag1 O8 75.80(11) . . ? O22 Ag1 O15 89.04(11) . . ? O29 Ag1 Ag2 115.81(8) 1_455 . ? O29 Ag1 O8 163.80(11) 1_455 . ? O29 Ag1 O15 91.85(11) 1_455 . ? O29 Ag1 O22 92.08(11) 1_455 . ? Ag1 Ag2 Ag3 173.829(15) . . ? O8 Ag2 Ag1 51.20(8) . . ? O8 Ag2 Ag3 123.59(8) . . ? O8 Ag2 O15 78.19(11) . . ? O8 Ag2 O29 95.46(11) . . ? O8 Ag2 O36 98.29(11) . . ? O15 Ag2 Ag1 48.11(7) . . ? O15 Ag2 Ag3 130.33(7) . . ? O15 Ag2 O29 171.79(11) . . ? O22 Ag2 Ag1 48.02(8) . . ? O22 Ag2 Ag3 136.95(8) . . ? O22 Ag2 O8 78.26(11) . . ? O22 Ag2 O15 87.43(11) . . ? O22 Ag2 O29 96.45(11) . . ? O22 Ag2 O36 176.44(12) . . ? O29 Ag2 Ag1 131.03(8) . . ? O29 Ag2 Ag3 49.38(8) . . ? O36 Ag2 Ag1 130.21(7) . . ? O36 Ag2 Ag3 44.55(7) . . ? O36 Ag2 O15 92.72(11) . . ? O36 Ag2 O29 82.97(11) . . ? O43 Ag2 Ag1 133.44(8) . . ? O43 Ag2 Ag3 51.74(8) . . ? O43 Ag2 O8 175.33(13) . . ? O43 Ag2 O15 104.66(11) . . ? O43 Ag2 O22 105.42(11) . . ? O43 Ag2 O29 81.35(11) . . ? O43 Ag2 O36 77.99(11) . . ? O15 Ag3 Ag2 119.85(8) 1_655 . ? O15 Ag3 O29 89.17(11) 1_655 . ? O15 Ag3 O43 165.34(11) 1_655 . ? O29 Ag3 Ag2 50.11(8) . . ? O29 Ag3 O43 77.82(10) . . ? O36 Ag3 Ag2 48.43(8) . . ? O36 Ag3 O15 96.20(11) . 1_655 ? O36 Ag3 O29 86.71(11) . . ? O36 Ag3 O43 76.54(11) . . ? O43 Ag3 Ag2 46.04(7) . . ? O50 Ag3 Ag2 125.62(9) . . ? O50 Ag3 O15 103.26(12) . 1_655 ? O50 Ag3 O29 103.81(12) . . ? O50 Ag3 O36 157.88(12) . . ? O50 Ag3 O43 86.59(11) . . ? N2 O1 Ag1 120.6(3) . . ? O1 N2 C3 118.7(4) . . ? O1 N2 C7 121.4(4) . . ? C7 N2 C3 119.8(4) . . ? N2 C3 H3 119.8 . . ? N2 C3 C4 120.5(5) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.8(5) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 121.2 . . ? C4 C5 C6 117.6(5) . . ? C6 C5 H5 121.2 . . ? C5 C6 H6 119.9 . . ? C7 C6 C5 120.1(5) . . ? C7 C6 H6 119.9 . . ? N2 C7 C6 121.1(5) . . ? N2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? Ag2 O8 Ag1 80.80(9) . . ? N9 O8 Ag1 116.9(3) . . ? N9 O8 Ag2 123.7(3) . . ? O8 N9 C10 119.1(4) . . ? O8 N9 C14 120.5(4) . . ? C14 N9 C10 120.3(4) . . ? N9 C10 H10 119.9 . . ? N9 C10 C11 120.3(5) . . ? C11 C10 H10 119.9 . . ? C10 C11 H11 120.0 . . ? C12 C11 C10 120.0(5) . . ? C12 C11 H11 120.0 . . ? C11 C12 H12 120.6 . . ? C11 C12 C13 118.8(5) . . ? C13 C12 H12 120.6 . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.0(5) . . ? C14 C13 H13 120.0 . . ? N9 C14 C13 120.5(5) . . ? N9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? Ag1 O15 Ag2 81.62(10) . . ? Ag3 O15 Ag1 90.02(11) 1_455 . ? Ag3 O15 Ag2 122.72(13) 1_455 . ? N16 O15 Ag1 129.3(3) . . ? N16 O15 Ag2 107.0(2) . . ? N16 O15 Ag3 120.9(3) . 1_455 ? O15 N16 C17 118.9(4) . . ? O15 N16 C21 120.7(4) . . ? C17 N16 C21 120.4(4) . . ? N16 C17 H17 119.6 . . ? N16 C17 C18 120.9(4) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.2(5) . . ? C19 C18 H18 119.9 . . ? C18 C19 H19 121.1 . . ? C18 C19 C20 117.8(5) . . ? C20 C19 H19 121.1 . . ? C19 C20 H20 120.1 . . ? C21 C20 C19 119.9(5) . . ? C21 C20 H20 120.1 . . ? N16 C21 C20 120.8(5) . . ? N16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? Ag2 O22 Ag1 84.24(10) . . ? N23 O22 Ag1 140.6(3) . . ? N23 O22 Ag2 124.8(3) . . ? O22 N23 C24 118.8(4) . . ? O22 N23 C28 120.2(4) . . ? C24 N23 C28 121.0(4) . . ? N23 C24 H24 119.6 . . ? N23 C24 C25 120.9(5) . . ? C25 C24 H24 119.6 . . ? C24 C25 H25 120.2 . . ? C24 C25 C26 119.7(5) . . ? C26 C25 H25 120.2 . . ? C25 C26 H26 120.8 . . ? C27 C26 C25 118.5(5) . . ? C27 C26 H26 120.8 . . ? C26 C27 H27 119.5 . . ? C26 C27 C28 120.9(5) . . ? C28 C27 H27 119.5 . . ? N23 C28 C27 119.1(5) . . ? N23 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? Ag1 O29 Ag2 130.01(13) 1_655 . ? Ag1 O29 Ag3 88.95(11) 1_655 . ? Ag3 O29 Ag2 80.51(10) . . ? N30 O29 Ag1 115.6(3) . 1_655 ? N30 O29 Ag2 111.8(2) . . ? N30 O29 Ag3 120.3(3) . . ? O29 N30 C35 118.5(4) . . ? C31 N30 O29 119.8(4) . . ? C31 N30 C35 121.7(4) . . ? N30 C31 H31 120.1 . . ? N30 C31 C32 119.8(5) . . ? C32 C31 H31 120.1 . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.3(5) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 120.8 . . ? C32 C33 C34 118.5(5) . . ? C34 C33 H33 120.8 . . ? C33 C34 H34 119.9 . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34 119.9 . . ? N30 C35 C34 119.5(4) . . ? N30 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? Ag3 O36 Ag2 87.02(10) . . ? N37 O36 Ag2 128.2(3) . . ? N37 O36 Ag3 121.2(3) . . ? O36 N37 C42 120.0(4) . . ? C38 N37 O36 118.4(4) . . ? C38 N37 C42 121.7(4) . . ? N37 C38 H38 119.9 . . ? N37 C38 C39 120.2(4) . . ? C39 C38 H38 119.9 . . ? C38 C39 H39 120.1 . . ? C38 C39 C40 119.8(5) . . ? C40 C39 H39 120.1 . . ? C39 C40 H40 120.6 . . ? C41 C40 C39 118.8(5) . . ? C41 C40 H40 120.6 . . ? C40 C41 H41 119.7 . . ? C40 C41 C42 120.6(5) . . ? C42 C41 H41 119.7 . . ? N37 C42 C41 118.9(5) . . ? N37 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? Ag2 O43 Ag3 82.22(10) . . ? N44 O43 Ag2 126.7(3) . . ? N44 O43 Ag3 116.7(3) . . ? O43 N44 C45 119.0(4) . . ? O43 N44 C49 119.9(4) . . ? C45 N44 C49 120.9(4) . . ? N44 C45 H45 119.8 . . ? N44 C45 C46 120.5(5) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 119.9 . . ? C45 C46 C47 120.2(5) . . ? C47 C46 H46 119.9 . . ? C46 C47 H47 120.8 . . ? C48 C47 C46 118.4(5) . . ? C48 C47 H47 120.8 . . ? C47 C48 H48 119.8 . . ? C47 C48 C49 120.3(5) . . ? C49 C48 H48 119.8 . . ? N44 C49 C48 119.7(4) . . ? N44 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? N51 O50 Ag3 117.3(3) . . ? O50 N51 C52 119.3(4) . . ? O50 N51 C56 120.8(4) . . ? C52 N51 C56 119.9(4) . . ? N51 C52 H52 119.6 . . ? N51 C52 C53 120.7(5) . . ? C53 C52 H52 119.6 . . ? C52 C53 H53 119.8 . . ? C52 C53 C54 120.4(5) . . ? C54 C53 H53 119.8 . . ? C53 C54 H54 121.0 . . ? C53 C54 C55 118.0(5) . . ? C55 C54 H54 121.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 C54 120.1(5) . . ? C56 C55 H55 120.0 . . ? N51 C56 C55 120.9(4) . . ? N51 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? O58 S57 C61 103.6(2) . . ? O59 S57 O58 114.7(2) . . ? O59 S57 C61 103.2(2) . . ? O60 S57 O58 115.2(2) . . ? O60 S57 O59 114.7(2) . . ? O60 S57 C61 103.0(2) . . ? F62 C61 S57 111.4(3) . . ? F62 C61 F64 106.9(4) . . ? F63 C61 S57 112.1(4) . . ? F63 C61 F62 107.8(5) . . ? F63 C61 F64 107.2(4) . . ? F64 C61 S57 111.1(4) . . ? O66 S65 O67 115.9(2) . . ? O66 S65 O68 114.8(2) . . ? O66 S65 C69 103.7(2) . . ? O67 S65 O68 114.9(2) . . ? O67 S65 C69 102.6(2) . . ? O68 S65 C69 102.4(2) . . ? F70 C69 S65 112.2(4) . . ? F70 C69 F71 108.1(4) . . ? F70 C69 F72 106.4(4) . . ? F71 C69 S65 111.2(4) . . ? F71 C69 F72 107.0(4) . . ? F72 C69 S65 111.7(3) . . ? O74 S73 O75 114.6(2) . . ? O74 S73 O76 115.9(2) . . ? O74 S73 C77 103.3(2) . . ? O75 S73 C77 102.9(2) . . ? O76 S73 O75 115.0(2) . . ? O76 S73 C77 102.7(2) . . ? F78 C77 S73 111.9(3) . . ? F79 C77 S73 111.0(4) . . ? F79 C77 F78 106.6(4) . . ? F80 C77 S73 111.7(4) . . ? F80 C77 F78 107.3(4) . . ? F80 C77 F79 108.1(4) . . ? _database_code_depnum_ccdc_archive 'CCDC 958489'