# Electronic Supplementary Material (ESI) for CrystEngComm # 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_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 Ag N, Cl O4' _chemical_formula_sum 'C12 H15 Ag Cl N O4' _chemical_formula_weight 380.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8079(4) _cell_length_b 12.2447(4) _cell_length_c 12.5250(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1350.82(10) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 9567 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 32.07 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6298 _exptl_absorpt_correction_T_max 0.8094 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31161 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3097 _reflns_number_gt 2998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.0979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.037(19) _refine_ls_number_reflns 3097 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.009488(16) 0.592619(12) 0.190466(12) 0.02550(5) Uani 1 1 d . . . C1 C -0.1073(2) 0.86187(18) 0.47760(17) 0.0242(4) Uani 1 1 d . . . H1A H -0.0466 0.8076 0.5110 0.029 Uiso 1 1 calc R . . C2 C -0.0827(2) 0.97090(19) 0.50095(18) 0.0284(5) Uani 1 1 d . . . H2A H -0.0049 0.9904 0.5499 0.034 Uiso 1 1 calc R . . C3 C -0.1703(3) 1.05241(19) 0.4539(2) 0.0325(5) Uani 1 1 d . . . H3A H -0.1532 1.1271 0.4706 0.039 Uiso 1 1 calc R . . C4 C -0.2830(3) 1.02246(19) 0.38217(19) 0.0341(5) Uani 1 1 d . . . H4A H -0.3438 1.0774 0.3498 0.041 Uiso 1 1 calc R . . C5 C -0.3085(2) 0.91328(19) 0.35687(17) 0.0264(4) Uani 1 1 d . . . H5A H -0.3853 0.8947 0.3068 0.032 Uiso 1 1 calc R . . C6 C -0.2218(2) 0.83014(17) 0.40464(15) 0.0194(4) Uani 1 1 d . . . C7 C -0.1528(2) 0.63603(17) 0.42921(17) 0.0206(4) Uani 1 1 d . . . H7A H -0.2030 0.5644 0.4194 0.025 Uiso 1 1 calc R . . H7B H -0.1453 0.6496 0.5069 0.025 Uiso 1 1 calc R . . C8 C 0.0059(2) 0.62932(15) 0.38379(14) 0.0198(3) Uani 1 1 d . . . H8A H 0.0577 0.6959 0.3699 0.024 Uiso 1 1 calc R . . C9 C 0.0786(2) 0.53546(18) 0.36175(17) 0.0250(4) Uani 1 1 d . . . H9A H 0.0302 0.4674 0.3747 0.030 Uiso 1 1 calc R . . H9B H 0.1786 0.5372 0.3332 0.030 Uiso 1 1 calc R . . C10 C -0.3226(2) 0.69181(18) 0.28094(17) 0.0236(4) Uani 1 1 d . . . H10A H -0.4205 0.7312 0.2760 0.028 Uiso 1 1 calc R . . H10B H -0.3450 0.6126 0.2811 0.028 Uiso 1 1 calc R . . C11 C -0.2287(2) 0.71838(17) 0.18362(17) 0.0237(4) Uani 1 1 d . . . H11A H -0.1655 0.7812 0.1867 0.028 Uiso 1 1 calc R . . C12 C -0.2279(3) 0.6599(2) 0.09281(18) 0.0348(5) Uani 1 1 d . . . H12A H -0.2896 0.5966 0.0867 0.042 Uiso 1 1 calc R . . H12B H -0.1655 0.6819 0.0348 0.042 Uiso 1 1 calc R . . N1 N -0.24925(18) 0.72050(14) 0.38197(13) 0.0201(3) Uani 1 1 d . . . Cl1 Cl 0.25597(6) 0.83815(4) 0.23024(4) 0.02143(10) Uani 1 1 d . . . O1 O 0.13803(18) 0.80283(13) 0.15838(14) 0.0349(4) Uani 1 1 d . . . O2 O 0.3767(2) 0.8847(2) 0.17092(17) 0.0684(7) Uani 1 1 d . . . O3 O 0.31033(17) 0.74836(13) 0.29276(15) 0.0356(4) Uani 1 1 d . . . O4 O 0.1950(3) 0.91810(19) 0.30167(18) 0.0708(7) 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 0.02611(7) 0.03171(9) 0.01869(8) -0.00072(6) 0.00030(6) 0.00809(7) C1 0.0240(9) 0.0286(11) 0.0201(10) -0.0043(8) 0.0040(8) -0.0014(8) C2 0.0283(10) 0.0322(12) 0.0245(12) -0.0090(10) 0.0096(9) -0.0065(9) C3 0.0446(13) 0.0215(11) 0.0314(13) -0.0047(9) 0.0195(11) -0.0053(9) C4 0.0499(14) 0.0252(12) 0.0271(12) 0.0057(10) 0.0148(11) 0.0071(10) C5 0.0298(9) 0.0282(11) 0.0212(10) 0.0006(10) 0.0031(8) 0.0030(9) C6 0.0186(8) 0.0242(10) 0.0155(9) 0.0000(8) 0.0054(7) -0.0012(7) C7 0.0210(8) 0.0214(10) 0.0194(10) 0.0028(8) 0.0034(8) -0.0020(7) C8 0.0216(8) 0.0220(8) 0.0158(8) 0.0006(7) -0.0027(9) -0.0028(8) C9 0.0255(10) 0.0284(11) 0.0212(11) 0.0012(9) -0.0064(8) 0.0031(8) C10 0.0167(8) 0.0282(11) 0.0259(11) -0.0037(9) -0.0023(7) -0.0017(7) C11 0.0249(8) 0.0267(10) 0.0197(10) 0.0007(9) -0.0030(9) 0.0062(8) C12 0.0404(12) 0.0417(14) 0.0223(12) -0.0001(10) -0.0074(10) 0.0152(11) N1 0.0188(7) 0.0221(8) 0.0195(8) 0.0004(7) 0.0004(7) -0.0006(6) Cl1 0.0240(2) 0.0194(2) 0.0209(2) 0.00319(18) -0.00152(18) -0.00164(17) O1 0.0318(8) 0.0318(9) 0.0411(10) -0.0025(7) -0.0128(7) -0.0040(6) O2 0.0475(11) 0.1074(19) 0.0501(14) 0.0439(13) -0.0071(9) -0.0409(12) O3 0.0269(7) 0.0327(9) 0.0472(11) 0.0177(8) -0.0034(7) 0.0026(6) O4 0.1004(17) 0.0641(14) 0.0479(12) -0.0320(11) -0.0303(12) 0.0530(13) _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 C9 2.386(2) . ? Ag1 C12 2.424(2) . ? Ag1 C3 2.454(2) 3_545 ? Ag1 C8 2.4665(18) . ? Ag1 C11 2.4715(18) . ? C1 C2 1.384(3) . ? C1 C6 1.415(3) . ? C1 H1A 0.9500 . ? C2 C3 1.392(3) . ? C2 H2A 0.9500 . ? C3 C4 1.389(4) . ? C3 Ag1 2.454(2) 3 ? C3 H3A 0.9500 . ? C4 C5 1.392(3) . ? C4 H4A 0.9500 . ? C5 C6 1.406(3) . ? C5 H5A 0.9500 . ? C6 N1 1.393(3) . ? C7 N1 1.463(3) . ? C7 C8 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.345(3) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 N1 1.463(3) . ? C10 C11 1.508(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.344(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? Cl1 O2 1.4165(18) . ? Cl1 O4 1.4306(19) . ? Cl1 O3 1.4322(16) . ? Cl1 O1 1.4409(16) . ? 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 C9 Ag1 C12 144.24(8) . . ? C9 Ag1 C3 113.19(8) . 3_545 ? C12 Ag1 C3 102.03(8) . 3_545 ? C9 Ag1 C8 32.12(7) . . ? C12 Ag1 C8 118.48(7) . . ? C3 Ag1 C8 136.45(8) 3_545 . ? C9 Ag1 C11 117.91(7) . . ? C12 Ag1 C11 31.85(7) . . ? C3 Ag1 C11 127.14(8) 3_545 . ? C8 Ag1 C11 87.90(7) . . ? C2 C1 C6 120.9(2) . . ? C2 C1 H1A 119.6 . . ? C6 C1 H1A 119.6 . . ? C1 C2 C3 121.0(2) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C4 C3 C2 118.7(2) . . ? C4 C3 Ag1 92.15(15) . 3 ? C2 C3 Ag1 95.64(14) . 3 ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? Ag1 C3 H3A 82.3 3 . ? C3 C4 C5 121.1(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 120.7(2) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? N1 C6 C5 121.09(18) . . ? N1 C6 C1 121.33(19) . . ? C5 C6 C1 117.6(2) . . ? N1 C7 C8 115.03(16) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 124.39(18) . . ? C9 C8 Ag1 70.66(11) . . ? C7 C8 Ag1 109.19(13) . . ? C9 C8 H8A 117.8 . . ? C7 C8 H8A 117.8 . . ? Ag1 C8 H8A 90.1 . . ? C8 C9 Ag1 77.22(12) . . ? C8 C9 H9A 120.0 . . ? Ag1 C9 H9A 105.3 . . ? C8 C9 H9B 120.0 . . ? Ag1 C9 H9B 87.5 . . ? H9A C9 H9B 120.0 . . ? N1 C10 C11 113.91(15) . . ? N1 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N1 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 124.9(2) . . ? C12 C11 Ag1 72.12(12) . . ? C10 C11 Ag1 105.40(12) . . ? C12 C11 H11A 117.5 . . ? C10 C11 H11A 117.5 . . ? Ag1 C11 H11A 92.6 . . ? C11 C12 Ag1 76.03(12) . . ? C11 C12 H12A 120.0 . . ? Ag1 C12 H12A 102.6 . . ? C11 C12 H12B 120.0 . . ? Ag1 C12 H12B 91.4 . . ? H12A C12 H12B 120.0 . . ? C6 N1 C7 119.86(16) . . ? C6 N1 C10 118.96(17) . . ? C7 N1 C10 115.85(16) . . ? O2 Cl1 O4 109.53(18) . . ? O2 Cl1 O3 110.15(12) . . ? O4 Cl1 O3 107.99(13) . . ? O2 Cl1 O1 109.52(12) . . ? O4 Cl1 O1 109.00(12) . . ? O3 Cl1 O1 110.61(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.371 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 940152' ####################################################################### # # 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_complex7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H14 Ag Cl N2 O4' _chemical_formula_weight 381.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6852(4) _cell_length_b 8.1924(3) _cell_length_c 12.8192(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.738(2) _cell_angle_gamma 90.00 _cell_volume 1313.00(8) _cell_formula_units_Z 4 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 26.44 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3739 _exptl_absorpt_correction_T_max 0.5960 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26401 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0114 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.44 _reflns_number_total 2682 _reflns_number_gt 2484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+1.3464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2682 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.003 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 Cl1 Cl 0.70589(4) 0.82322(6) 0.88076(4) 0.01662(11) Uani 1 1 d . . . O1 O 0.66803(17) 0.9790(2) 0.83723(15) 0.0454(5) Uani 1 1 d . . . O2 O 0.64823(16) 0.7787(3) 0.96242(15) 0.0428(5) Uani 1 1 d . . . O3 O 0.81753(12) 0.8344(2) 0.92327(14) 0.0339(4) Uani 1 1 d . . . O4 O 0.68878(14) 0.7048(2) 0.79714(13) 0.0317(4) Uani 1 1 d . . . Ag1 Ag 0.699132(13) 1.250122(18) 0.917913(12) 0.02218(7) Uani 1 1 d . . . N1 N 0.71747(13) 1.1776(2) 1.10167(13) 0.0181(3) Uani 1 1 d . . . C1 C 0.61862(16) 1.1625(3) 1.12742(17) 0.0217(4) Uani 1 1 d . . . H1A H 0.5624 1.1251 1.0742 0.026 Uiso 1 1 calc R . . C2 C 0.59455(17) 1.1975(3) 1.22525(18) 0.0245(4) Uani 1 1 d . . . H2A H 0.5236 1.1870 1.2392 0.029 Uiso 1 1 calc R . . C3 C 0.67771(19) 1.2491(3) 1.30364(19) 0.0249(5) Uani 1 1 d . . . H3A H 0.6640 1.2748 1.3724 0.030 Uiso 1 1 calc R . . C4 C 0.77966(18) 1.2629(2) 1.28138(18) 0.0212(4) Uani 1 1 d . . . H4A H 0.8370 1.2974 1.3343 0.025 Uiso 1 1 calc R . . C5 C 0.79762(16) 1.2248(2) 1.17796(16) 0.0155(4) Uani 1 1 d . . . N2 N 0.89818(14) 1.2355(2) 1.15091(14) 0.0174(4) Uani 1 1 d . . . C6 C 0.99189(16) 1.2864(2) 1.22682(16) 0.0165(4) Uani 1 1 d . . . H6A H 0.9696 1.3669 1.2765 0.020 Uiso 1 1 calc R . . H6B H 1.0437 1.3405 1.1884 0.020 Uiso 1 1 calc R . . C7 C 1.04565(15) 1.1437(2) 1.28884(15) 0.0174(4) Uani 1 1 d . . . H7A H 1.0906 1.0760 1.2552 0.021 Uiso 1 1 calc R . . C8 C 1.03434(16) 1.1059(3) 1.38803(17) 0.0228(4) Uani 1 1 d . . . H8A H 0.9900 1.1709 1.4241 0.027 Uiso 1 1 calc R . . H8B H 1.0707 1.0141 1.4223 0.027 Uiso 1 1 calc R . . C9 C 0.91993(16) 1.1535(3) 1.05579(15) 0.0188(4) Uani 1 1 d . . . H9A H 0.8771 1.0519 1.0459 0.023 Uiso 1 1 calc R . . H9B H 0.9963 1.1219 1.0671 0.023 Uiso 1 1 calc R . . C10 C 0.89599(18) 1.2525(3) 0.95596(18) 0.0236(5) Uani 1 1 d . . . H10A H 0.9035 1.1990 0.8919 0.028 Uiso 1 1 calc R . . C11 C 0.86520(18) 1.4082(3) 0.94865(19) 0.0306(5) Uani 1 1 d . . . H11A H 0.8565 1.4669 1.0105 0.037 Uiso 1 1 calc R . . H11B H 0.8519 1.4604 0.8816 0.037 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 Cl1 0.0152(2) 0.0194(2) 0.0144(2) -0.00122(17) -0.00015(16) -0.00192(17) O1 0.0658(13) 0.0216(8) 0.0388(10) -0.0002(7) -0.0194(9) 0.0066(8) O2 0.0293(10) 0.0749(14) 0.0259(9) -0.0007(9) 0.0094(8) -0.0196(9) O3 0.0139(7) 0.0513(11) 0.0353(9) -0.0110(8) 0.0007(6) -0.0028(7) O4 0.0396(10) 0.0286(8) 0.0237(8) -0.0110(7) -0.0040(7) -0.0023(7) Ag1 0.01838(11) 0.02669(11) 0.01848(11) 0.00217(6) -0.00548(7) -0.00113(6) N1 0.0155(8) 0.0226(8) 0.0150(8) 0.0016(7) -0.0010(6) -0.0031(7) C1 0.0153(9) 0.0252(10) 0.0226(10) 0.0048(8) -0.0022(8) -0.0043(8) C2 0.0170(10) 0.0291(11) 0.0283(11) 0.0029(9) 0.0065(8) 0.0001(9) C3 0.0226(12) 0.0309(12) 0.0229(11) -0.0033(8) 0.0090(9) 0.0029(8) C4 0.0174(10) 0.0294(11) 0.0160(10) -0.0041(8) 0.0004(8) 0.0000(8) C5 0.0131(9) 0.0168(9) 0.0161(9) 0.0014(7) 0.0010(7) 0.0003(7) N2 0.0117(8) 0.0266(9) 0.0133(8) -0.0028(6) 0.0003(7) -0.0004(6) C6 0.0131(9) 0.0202(9) 0.0151(9) -0.0011(7) -0.0007(7) -0.0016(7) C7 0.0128(9) 0.0205(9) 0.0176(9) -0.0031(8) -0.0015(7) -0.0015(7) C8 0.0183(10) 0.0267(10) 0.0222(10) 0.0045(8) 0.0004(8) -0.0012(8) C9 0.0146(9) 0.0266(10) 0.0146(9) -0.0031(8) 0.0008(7) 0.0023(8) C10 0.0158(10) 0.0412(14) 0.0137(10) -0.0002(8) 0.0023(8) -0.0041(8) C11 0.0255(11) 0.0367(13) 0.0274(11) 0.0112(10) -0.0020(9) -0.0119(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 O2 1.4223(18) . ? Cl1 O3 1.4318(16) . ? Cl1 O4 1.4351(16) . ? Cl1 O1 1.4423(17) . ? O1 Ag1 2.4537(17) . ? Ag1 C8 2.374(2) 4_585 ? Ag1 N1 2.4022(16) . ? Ag1 C11 2.447(2) . ? Ag1 C10 2.462(2) . ? Ag1 C7 2.4889(19) 4_585 ? N1 C5 1.343(3) . ? N1 C1 1.355(3) . ? C1 C2 1.370(3) . ? C1 H1A 0.9500 . ? C2 C3 1.394(3) . ? C2 H2A 0.9500 . ? C3 C4 1.375(3) . ? C3 H3A 0.9500 . ? C4 C5 1.418(3) . ? C4 H4A 0.9500 . ? C5 N2 1.380(3) . ? N2 C9 1.459(2) . ? N2 C6 1.464(3) . ? C6 C7 1.510(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.340(3) . ? C7 Ag1 2.4890(18) 4_686 ? C7 H7A 0.9500 . ? C8 Ag1 2.374(2) 4_686 ? C8 H8A 0.9500 . ? C8 H8B 0.9500 . ? C9 C10 1.502(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.332(3) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C11 H11B 0.9500 . ? 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 Cl1 O3 109.57(11) . . ? O2 Cl1 O4 110.16(12) . . ? O3 Cl1 O4 110.03(10) . . ? O2 Cl1 O1 109.44(13) . . ? O3 Cl1 O1 109.50(12) . . ? O4 Cl1 O1 108.12(11) . . ? Cl1 O1 Ag1 128.22(10) . . ? C8 Ag1 N1 102.57(7) 4_585 . ? C8 Ag1 C11 118.26(8) 4_585 . ? N1 Ag1 C11 92.01(7) . . ? C8 Ag1 O1 107.90(7) 4_585 . ? N1 Ag1 O1 99.87(6) . . ? C11 Ag1 O1 128.28(8) . . ? C8 Ag1 C10 149.74(8) 4_585 . ? N1 Ag1 C10 83.17(7) . . ? C11 Ag1 C10 31.49(8) . . ? O1 Ag1 C10 100.15(7) . . ? C8 Ag1 C7 31.87(7) 4_585 4_585 ? N1 Ag1 C7 132.33(6) . 4_585 ? C11 Ag1 C7 118.52(7) . 4_585 ? O1 Ag1 C7 89.09(6) . 4_585 ? C10 Ag1 C7 141.44(7) . 4_585 ? C5 N1 C1 117.82(17) . . ? C5 N1 Ag1 125.37(13) . . ? C1 N1 Ag1 108.75(13) . . ? N1 C1 C2 124.21(19) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? C1 C2 C3 117.7(2) . . ? C1 C2 H2A 121.2 . . ? C3 C2 H2A 121.2 . . ? C4 C3 C2 119.9(2) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 N2 116.97(18) . . ? N1 C5 C4 121.53(19) . . ? N2 C5 C4 121.51(19) . . ? C5 N2 C9 119.62(17) . . ? C5 N2 C6 122.16(17) . . ? C9 N2 C6 116.09(16) . . ? N2 C6 C7 111.88(16) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 124.57(19) . . ? C8 C7 Ag1 69.34(12) . 4_686 ? C6 C7 Ag1 108.20(12) . 4_686 ? C8 C7 H7A 117.7 . . ? C6 C7 H7A 117.7 . . ? Ag1 C7 H7A 92.5 4_686 . ? C7 C8 Ag1 78.78(12) . 4_686 ? C7 C8 H8A 120.0 . . ? Ag1 C8 H8A 102.8 4_686 . ? C7 C8 H8B 120.0 . . ? Ag1 C8 H8B 88.5 4_686 . ? H8A C8 H8B 120.0 . . ? N2 C9 C10 115.06(17) . . ? N2 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? N2 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 126.3(2) . . ? C11 C10 Ag1 73.64(14) . . ? C9 C10 Ag1 102.50(13) . . ? C11 C10 H10A 116.9 . . ? C9 C10 H10A 116.9 . . ? Ag1 C10 H10A 94.1 . . ? C10 C11 Ag1 74.87(14) . . ? C10 C11 H11A 120.0 . . ? Ag1 C11 H11A 100.6 . . ? C10 C11 H11B 120.0 . . ? Ag1 C11 H11B 94.4 . . ? H11A C11 H11B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.426 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 940153' ####################################################################### # # 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_complex8 _audit_creation_date 2013-05-13 _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 'C20 H26 Ag2 N6, 2(Cl O4)' _chemical_formula_sum 'C20 H26 Ag2 Cl2 N6 O8' _chemical_formula_weight 765.11 _chemical_absolute_configuration ? _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' 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' Cl Cl 0.1484 0.1585 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_H-M_alt 'P 21 21 2' _space_group_name_Hall 'P 2 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 15.3229(9) _cell_length_b 21.2905(11) _cell_length_c 8.0381(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2622.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_temperature 114(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_correction_T_min 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description ? _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_unetI/netI 0.0727 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 14890 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.403 _diffrn_reflns_theta_min 1.913 _diffrn_ambient_temperature 114(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.755 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.994 _reflns_number_gt 3444 _reflns_number_total 5371 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _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 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution ? _refine_diff_density_max 0.908 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.105 _refine_ls_abs_structure_details ; Flack x determined using 1152 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.051(18) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 399 _refine_ls_number_reflns 5371 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0478 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0628P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.1199 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C5') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C6') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Others Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2)=Sof(H2A)=Sof(C3')=Sof(H3'A)=Sof(H3'B)= Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(C6)=Sof(H6A)=Sof(H6B)=1-FVAR(1) Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2')=Sof(H2'A)=Sof(C3)=Sof(H3A)=Sof(H3B)= Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(C5')=Sof(H5'A)=Sof(C6')=Sof(H6'A)=Sof(H6'B)= FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C14(H14A,H14B), C3(H3A,H3B), C4'(H4'A,H4'B), C3'(H3'A,H3'B), C4(H4A,H4B) 4.b Aromatic/amide H refined with riding coordinates: C19(H19), C18(H18), C17(H17), C9(H9), C12(H12), C15(H15), C8(H8), C7(H7), C2'(H2'A), C5'(H5'A), C2(H2A), C5(H5A) 4.c X=CH2 refined with riding coordinates: C11(H11A,H11B), C16(H16A,H16B), C1(H1A,H1B), C6'(H6'A,H6'B), C1'(H1'A,H1'B), C6(H6A,H6B) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.91925(6) 0.79911(4) -0.14663(12) 0.0578(3) Uani 1 1 d . . . . . Ag2 Ag 0.67988(6) 1.05128(4) -0.32645(12) 0.0545(3) Uani 1 1 d . . . . . Cl2 Cl 1.0000 1.0000 -0.8830(5) 0.0508(10) Uani 1 2 d S T P . . Cl1 Cl 0.65594(19) 0.77351(15) 0.4424(5) 0.0614(9) Uani 1 1 d . . . . . Cl3 Cl 1.0000 0.5000 -0.2492(5) 0.0719(15) Uani 1 2 d S T P . . O6 O 0.9374(8) 1.0276(7) -0.9870(16) 0.145(6) Uani 1 1 d . . . . . O3 O 0.5766(9) 0.7845(8) 0.366(2) 0.179(7) Uani 1 1 d . . . . . O8 O 1.0725(6) 0.5156(4) -0.3489(11) 0.079(3) Uani 1 1 d . . . . . O7 O 0.9796(8) 0.5518(5) -0.1472(13) 0.113(4) Uani 1 1 d . . . . . O4 O 0.6700(8) 0.8204(6) 0.565(3) 0.189(9) Uani 1 1 d . . . . . O2 O 0.6408(9) 0.7202(6) 0.5254(18) 0.137(5) Uani 1 1 d . . . . . O5 O 1.0353(12) 1.0457(7) -0.7855(17) 0.175(8) Uani 1 1 d . . . . . O1 O 0.7255(9) 0.7676(9) 0.3433(18) 0.176(7) Uani 1 1 d . . . . . N6 N 0.8350(5) 0.9318(3) -0.3532(10) 0.0344(18) Uani 1 1 d . . . . . N5 N 0.7143(7) 0.9582(4) -0.1912(13) 0.066(3) Uani 1 1 d . . . . . N2 N 0.8423(8) 0.7076(6) -0.0687(18) 0.116(6) Uani 1 1 d . . . . . C19 C 0.6738(12) 0.9501(6) -0.0490(18) 0.087(5) Uani 1 1 d . . . . . H19 H 0.6252 0.9764 -0.0263 0.105 Uiso 1 1 calc R U . . . C20 C 0.7879(7) 0.9236(5) -0.2134(13) 0.040(3) Uani 1 1 d . . . . . C18 C 0.6956(7) 0.9073(6) 0.0678(14) 0.058(3) Uani 1 1 d . . . . . H18 H 0.6612 0.8992 0.1638 0.070 Uiso 1 1 calc R U . . . C17 C 0.7682(11) 0.8782(9) 0.036(2) 0.108(6) Uani 1 1 d . . . . . H17 H 0.7903 0.8512 0.1202 0.129 Uiso 1 1 calc R U . . . C10 C 0.8592(7) 0.6701(5) 0.0532(13) 0.039(2) Uani 1 1 d . . . . . N3 N 0.9330(5) 0.6815(4) 0.1474(12) 0.046(2) Uani 1 1 d . . . . . C9 C 0.7701(10) 0.6959(8) -0.159(2) 0.115(7) Uani 1 1 d . . . . . H9 H 0.7541 0.7257 -0.2411 0.138 Uiso 1 1 calc R U . . . N4 N 0.8152(8) 0.8826(7) -0.1054(14) 0.101(5) Uani 1 1 d . . . . . C11 C 0.8974(11) 0.8107(7) -0.4350(17) 0.081(4) Uani 1 1 d . . . . . H11A H 0.8367 0.8189 -0.4260 0.098 Uiso 1 1 calc R U . . . H11B H 0.9172 0.7700 -0.4651 0.098 Uiso 1 1 calc R U . . . C12 C 0.9541(8) 0.8556(5) -0.4059(14) 0.048(3) Uani 1 1 d . . . . . H12 H 1.0146 0.8466 -0.4154 0.058 Uiso 1 1 calc R U . . . C13 C 0.9268(9) 0.9202(6) -0.3584(19) 0.072(4) Uani 1 1 d . . . . . H13A H 0.9513 0.9296 -0.2472 0.087 Uiso 1 1 calc R U . . . H13B H 0.9534 0.9501 -0.4381 0.087 Uiso 1 1 calc R U . . . C14 C 0.7884(10) 0.9522(7) -0.5080(17) 0.076(4) Uani 1 1 d . . . . . H14A H 0.7276 0.9369 -0.5015 0.091 Uiso 1 1 calc R U . . . H14B H 0.8163 0.9311 -0.6040 0.091 Uiso 1 1 calc R U . . . C15 C 0.7859(16) 1.0198(6) -0.543(2) 0.107(8) Uani 1 1 d . . . . . H15 H 0.7569 1.0348 -0.6394 0.128 Uiso 1 1 calc R U . . . C16 C 0.8225(12) 1.0587(10) -0.444(3) 0.130(10) Uani 1 1 d . . . . . H16A H 0.8516 1.0439 -0.3472 0.156 Uiso 1 1 calc R U . . . H16B H 0.8206 1.1024 -0.4672 0.156 Uiso 1 1 calc R U . . . N1 N 0.8131(9) 0.6209(4) 0.0876(12) 0.082(4) Uani 1 1 d . . . . . C8 C 0.7211(7) 0.6472(5) -0.1415(14) 0.046(3) Uani 1 1 d . . . . . H8 H 0.6743 0.6378 -0.2147 0.055 Uiso 1 1 calc R U . . . C7 C 0.7419(11) 0.6115(6) -0.0127(19) 0.089(5) Uani 1 1 d . . . . . H7 H 0.7048 0.5770 0.0120 0.106 Uiso 1 1 calc R U . . . C1 C 0.9735(14) 0.5569(12) 0.272(3) 0.061(7) Uani 0.512(15) 1 d . . P A 1 H1A H 0.9642 0.5635 0.1569 0.073 Uiso 0.512(15) 1 calc R U P A 1 H1B H 0.9939 0.5173 0.3109 0.073 Uiso 0.512(15) 1 calc R U P A 1 C2' C 0.957(3) 0.607(3) 0.390(7) 0.046(16) Uani 0.512(15) 1 d . . P A 1 H2'A H 0.9656 0.6010 0.5057 0.055 Uiso 0.512(15) 1 calc R U P A 1 C3 C 0.9261(14) 0.6657(11) 0.327(3) 0.050(6) Uani 0.512(15) 1 d . . P A 1 H3A H 0.9571 0.6991 0.3892 0.060 Uiso 0.512(15) 1 calc R U P A 1 H3B H 0.8636 0.6691 0.3576 0.060 Uiso 0.512(15) 1 calc R U P A 1 C4' C 1.0115(13) 0.6967(11) 0.065(3) 0.052(6) Uani 0.512(15) 1 d . . P A 1 H4'A H 1.0089 0.6822 -0.0520 0.062 Uiso 0.512(15) 1 calc R U P A 1 H4'B H 1.0612 0.6755 0.1202 0.062 Uiso 0.512(15) 1 calc R U P A 1 C5' C 1.0239(18) 0.7662(13) 0.071(4) 0.033(6) Uani 0.512(15) 1 d . U P A 1 H5'A H 1.0732 0.7840 0.0165 0.040 Uiso 0.512(15) 1 calc R U P A 1 C6' C 0.969(2) 0.8035(14) 0.148(4) 0.064(8) Uani 0.512(15) 1 d . U P A 1 H6'A H 0.9194 0.7864 0.2023 0.076 Uiso 0.512(15) 1 calc R U P A 1 H6'B H 0.9788 0.8476 0.1488 0.076 Uiso 0.512(15) 1 calc R U P A 1 C1' C 0.8975(16) 0.6423(12) 0.478(3) 0.056(7) Uani 0.488(15) 1 d . . P A 2 H1'A H 0.8747 0.6824 0.4502 0.067 Uiso 0.488(15) 1 calc R U P A 2 H1'B H 0.8797 0.6220 0.5776 0.067 Uiso 0.488(15) 1 calc R U P A 2 C2 C 0.957(5) 0.613(4) 0.372(9) 0.08(3) Uani 0.488(15) 1 d . U P A 2 H2A H 0.9778 0.5730 0.4067 0.090 Uiso 0.488(15) 1 calc R U P A 2 C3' C 0.9902(15) 0.6358(11) 0.223(3) 0.048(7) Uani 0.488(15) 1 d . . P A 2 H3'A H 1.0479 0.6553 0.2431 0.057 Uiso 0.488(15) 1 calc R U P A 2 H3'B H 0.9987 0.6003 0.1450 0.057 Uiso 0.488(15) 1 calc R U P A 2 C4 C 0.9548(14) 0.7512(9) 0.203(2) 0.038(6) Uani 0.488(15) 1 d . . P A 2 H4A H 0.8986 0.7731 0.2214 0.045 Uiso 0.488(15) 1 calc R U P A 2 H4B H 0.9844 0.7488 0.3126 0.045 Uiso 0.488(15) 1 calc R U P A 2 C5 C 1.009(2) 0.7918(19) 0.094(5) 0.056(10) Uani 0.488(15) 1 d . U P A 2 H5A H 1.0143 0.8358 0.1104 0.068 Uiso 0.488(15) 1 calc R U P A 2 C6 C 1.0491(18) 0.7627(13) -0.027(4) 0.061(8) Uani 0.488(15) 1 d . . P A 2 H6A H 1.0424 0.7187 -0.0403 0.073 Uiso 0.488(15) 1 calc R U P A 2 H6B H 1.0849 0.7857 -0.1022 0.073 Uiso 0.488(15) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0661(6) 0.0437(5) 0.0637(6) 0.0169(5) -0.0079(5) -0.0022(5) Ag2 0.0588(5) 0.0464(5) 0.0585(5) -0.0109(5) 0.0075(5) 0.0043(4) Cl2 0.049(2) 0.066(3) 0.037(2) 0.000 0.000 0.006(2) Cl1 0.0467(18) 0.0538(18) 0.084(2) 0.0162(17) -0.0106(16) -0.0092(13) Cl3 0.134(4) 0.055(3) 0.027(2) 0.000 0.000 -0.033(3) O6 0.116(10) 0.195(15) 0.124(10) -0.021(10) -0.052(8) 0.075(10) O3 0.109(10) 0.175(14) 0.254(19) 0.074(15) -0.071(13) -0.033(10) O8 0.113(7) 0.074(6) 0.050(5) 0.005(5) 0.006(6) -0.022(5) O7 0.170(11) 0.088(7) 0.080(7) -0.046(7) 0.042(7) -0.038(8) O4 0.083(8) 0.125(11) 0.36(2) -0.140(14) 0.042(12) -0.027(8) O2 0.146(11) 0.118(10) 0.146(11) 0.061(9) -0.061(9) -0.064(9) O5 0.263(18) 0.126(10) 0.137(12) 0.009(9) -0.131(13) -0.082(12) O1 0.137(11) 0.28(2) 0.109(9) -0.029(12) 0.059(10) -0.073(13) N6 0.033(4) 0.041(5) 0.029(4) 0.001(4) -0.001(4) -0.002(3) N5 0.098(8) 0.043(5) 0.057(6) 0.012(5) 0.034(6) 0.011(6) N2 0.110(10) 0.110(10) 0.128(11) 0.096(9) -0.082(9) -0.068(9) C19 0.143(14) 0.036(6) 0.083(10) 0.001(8) 0.052(10) 0.022(9) C20 0.036(6) 0.040(6) 0.043(7) 0.006(5) -0.003(5) -0.010(5) C18 0.047(7) 0.094(10) 0.034(6) -0.008(7) 0.007(5) -0.009(7) C17 0.106(13) 0.143(16) 0.075(11) 0.051(11) 0.026(10) 0.061(12) C10 0.044(6) 0.031(5) 0.043(6) 0.006(5) -0.013(5) 0.005(5) N3 0.033(5) 0.052(5) 0.055(6) 0.019(5) -0.013(5) -0.003(4) C9 0.087(10) 0.115(13) 0.142(15) 0.091(13) -0.068(11) -0.057(10) N4 0.084(8) 0.143(11) 0.074(8) 0.070(8) 0.050(7) 0.069(8) C11 0.101(11) 0.067(9) 0.076(9) -0.011(8) 0.019(9) 0.014(9) C12 0.059(7) 0.027(5) 0.058(8) -0.007(5) 0.018(6) -0.002(5) C13 0.079(9) 0.064(8) 0.073(9) 0.010(8) 0.002(9) -0.004(7) C14 0.093(10) 0.071(9) 0.063(8) -0.002(8) 0.012(8) -0.004(9) C15 0.22(2) 0.039(8) 0.065(10) 0.018(7) 0.068(12) 0.064(11) C16 0.110(14) 0.131(17) 0.149(19) 0.097(15) 0.099(14) 0.077(14) N1 0.140(11) 0.039(5) 0.066(7) 0.019(5) -0.069(7) -0.042(7) C8 0.048(6) 0.043(6) 0.046(7) 0.003(6) -0.012(6) 0.009(5) C7 0.129(13) 0.058(8) 0.079(10) 0.018(8) -0.049(9) -0.054(9) C1 0.057(15) 0.060(16) 0.065(16) 0.007(14) 0.020(12) 0.011(13) C2' 0.032(18) 0.06(3) 0.04(2) 0.041(19) 0.017(12) 0.020(14) C3 0.042(12) 0.053(13) 0.055(15) 0.005(12) -0.012(13) -0.018(11) C4' 0.044(12) 0.072(16) 0.039(12) 0.009(12) -0.020(10) 0.029(12) C5' 0.027(10) 0.036(11) 0.036(11) 0.005(10) 0.001(9) -0.007(9) C6' 0.068(12) 0.066(13) 0.056(12) 0.002(11) -0.012(10) -0.005(10) C1' 0.061(16) 0.066(16) 0.042(14) 0.004(13) 0.009(12) -0.034(14) C2 0.07(3) 0.08(3) 0.08(3) 0.004(14) 0.001(13) -0.007(13) C3' 0.046(13) 0.049(14) 0.048(15) -0.001(11) -0.001(11) 0.001(11) C4 0.063(14) 0.028(11) 0.023(11) 0.005(9) -0.025(9) -0.005(10) C5 0.057(14) 0.054(14) 0.058(15) -0.004(12) 0.002(11) 0.002(12) C6 0.053(17) 0.052(17) 0.08(2) 0.036(17) -0.018(15) -0.013(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.361(11) . ? Ag1 N4 2.410(11) . ? Ag1 C11 2.355(14) . ? Ag1 C12 2.465(11) . ? Ag1 C5' 2.47(3) . ? Ag1 C6' 2.49(3) . ? Ag1 C5 2.38(4) . ? Ag1 C6 2.34(2) . ? Ag2 N5 2.320(9) . ? Ag2 C15 2.472(16) . ? Ag2 C16 2.386(15) . ? Ag2 N1 2.428(9) 3_655 ? Ag2 C1 2.39(2) 3_655 ? Ag2 C2' 2.46(6) 3_655 ? Ag2 C1' 2.58(2) 3_655 ? Ag2 C2 2.51(8) 3_655 ? Cl2 O6 1.402(11) 2_775 ? Cl2 O6 1.402(11) . ? Cl2 O5 1.361(11) . ? Cl2 O5 1.361(11) 2_775 ? Cl1 O3 1.384(13) . ? Cl1 O4 1.417(13) . ? Cl1 O2 1.336(11) . ? Cl1 O1 1.336(13) . ? Cl3 O8 1.409(9) . ? Cl3 O8 1.409(9) 2_765 ? Cl3 O7 1.410(9) . ? Cl3 O7 1.410(9) 2_765 ? N6 C20 1.347(12) . ? N6 C13 1.428(15) . ? N6 C14 1.499(16) . ? N5 C19 1.312(16) . ? N5 C20 1.361(14) . ? N2 C10 1.290(14) . ? N2 C9 1.345(16) . ? C19 H19 0.9500 . ? C19 C18 1.351(18) . ? C20 N4 1.300(14) . ? C18 H18 0.9500 . ? C18 C17 1.298(18) . ? C17 H17 0.9500 . ? C17 N4 1.348(17) . ? C10 N3 1.383(12) . ? C10 N1 1.292(14) . ? N3 C3 1.49(2) . ? N3 C4' 1.41(2) . ? N3 C3' 1.44(2) . ? N3 C4 1.59(2) . ? C9 H9 0.9500 . ? C9 C8 1.287(17) . ? C11 H11A 0.9500 . ? C11 H11B 0.9500 . ? C11 C12 1.313(17) . ? C12 H12 0.9500 . ? C12 C13 1.487(16) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.467(19) . ? C15 H15 0.9500 . ? C15 C16 1.28(3) . ? C16 H16A 0.9500 . ? C16 H16B 0.9500 . ? N1 Ag2 2.428(9) 3_645 ? N1 C7 1.372(17) . ? C8 H8 0.9500 . ? C8 C7 1.323(16) . ? C7 H7 0.9500 . ? C1 Ag2 2.39(2) 3_645 ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C1 C2' 1.45(7) . ? C2' Ag2 2.46(6) 3_645 ? C2' H2'A 0.9500 . ? C2' C3 1.43(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4' H4'A 0.9900 . ? C4' H4'B 0.9900 . ? C4' C5' 1.49(4) . ? C5' H5'A 0.9500 . ? C5' C6' 1.31(4) . ? C6' H6'A 0.9500 . ? C6' H6'B 0.9500 . ? C1' Ag2 2.58(2) 3_645 ? C1' H1'A 0.9500 . ? C1' H1'B 0.9500 . ? C1' C2 1.39(8) . ? C2 Ag2 2.51(8) 3_645 ? C2 H2A 0.9500 . ? C2 C3' 1.39(7) . ? C3' H3'A 0.9900 . ? C3' H3'B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.49(4) . ? C5 H5A 0.9500 . ? C5 C6 1.30(5) . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N4 104.0(5) . . ? N2 Ag1 C11 106.1(5) . . ? N2 Ag1 C12 137.3(4) . . ? N2 Ag1 C5' 84.4(7) . . ? N2 Ag1 C6' 86.1(8) . . ? N2 Ag1 C5 91.1(10) . . ? N2 Ag1 C6 92.4(7) . . ? N4 Ag1 C12 84.2(3) . . ? N4 Ag1 C5' 122.8(8) . . ? N4 Ag1 C6' 92.5(8) . . ? N4 Ag1 C5 108.6(11) . . ? C11 Ag1 N4 88.0(5) . . ? C11 Ag1 C12 31.5(4) . . ? C11 Ag1 C5' 144.8(9) . . ? C11 Ag1 C6' 167.4(8) . . ? C11 Ag1 C5 152.7(10) . . ? C11 Ag1 C6 124.0(10) . . ? C12 Ag1 C6' 136.0(8) . . ? C5' Ag1 C12 126.5(7) . . ? C5' Ag1 C6' 30.7(10) . . ? C5 Ag1 C12 126.4(10) . . ? C6 Ag1 N4 138.6(10) . . ? C6 Ag1 C12 108.9(8) . . ? C6 Ag1 C5 32.1(11) . . ? N5 Ag2 C15 87.1(4) . . ? N5 Ag2 C16 92.0(5) . . ? N5 Ag2 N1 98.1(3) . 3_655 ? N5 Ag2 C1 100.4(7) . 3_655 ? N5 Ag2 C2' 134.6(14) . 3_655 ? N5 Ag2 C1' 165.4(7) . 3_655 ? N5 Ag2 C2 135(2) . 3_655 ? C15 Ag2 C2' 123.0(14) . 3_655 ? C15 Ag2 C1' 100.0(6) . 3_655 ? C16 Ag2 C15 30.4(7) . . ? C16 Ag2 N1 103.4(7) . 3_655 ? C16 Ag2 C2' 131.7(14) . 3_655 ? C16 Ag2 C1' 100.6(7) . 3_655 ? N1 Ag2 C15 133.8(7) 3_655 . ? N1 Ag2 C2' 84.7(12) 3_655 3_655 ? N1 Ag2 C1' 86.3(6) 3_655 3_655 ? C1 Ag2 C15 141.9(8) 3_655 . ? C1 Ag2 C16 165.5(7) 3_655 . ? C1 Ag2 N1 82.5(7) 3_655 3_655 ? C1 Ag2 C2' 34.7(15) 3_655 3_655 ? C2 Ag2 C15 126.1(18) 3_655 . ? C2 Ag2 C16 132(2) 3_655 . ? C2 Ag2 N1 80.4(18) 3_655 3_655 ? C2 Ag2 C1' 32(2) 3_655 3_655 ? O6 Cl2 O6 106.8(11) 2_775 . ? O5 Cl2 O6 111.8(10) 2_775 . ? O5 Cl2 O6 108.4(9) . . ? O5 Cl2 O6 111.8(10) . 2_775 ? O5 Cl2 O6 108.4(9) 2_775 2_775 ? O5 Cl2 O5 109.7(13) . 2_775 ? O3 Cl1 O4 108.9(10) . . ? O2 Cl1 O3 102.4(9) . . ? O2 Cl1 O4 106.2(11) . . ? O1 Cl1 O3 116.8(11) . . ? O1 Cl1 O4 111.0(9) . . ? O1 Cl1 O2 110.9(11) . . ? O8 Cl3 O8 110.7(8) 2_765 . ? O7 Cl3 O8 108.7(6) . . ? O7 Cl3 O8 109.9(7) 2_765 . ? O7 Cl3 O8 108.7(6) 2_765 2_765 ? O7 Cl3 O8 109.9(7) . 2_765 ? O7 Cl3 O7 108.9(10) 2_765 . ? C20 N6 C13 121.9(9) . . ? C20 N6 C14 118.4(9) . . ? C13 N6 C14 119.7(10) . . ? C19 N5 Ag2 114.5(9) . . ? C19 N5 C20 115.7(11) . . ? C20 N5 Ag2 126.2(7) . . ? C10 N2 Ag1 127.8(8) . . ? C10 N2 C9 117.2(11) . . ? C9 N2 Ag1 114.9(9) . . ? N5 C19 H19 117.3 . . ? N5 C19 C18 125.3(13) . . ? C18 C19 H19 117.3 . . ? N6 C20 N5 118.9(9) . . ? N4 C20 N6 118.2(10) . . ? N4 C20 N5 122.9(10) . . ? C19 C18 H18 123.3 . . ? C17 C18 C19 113.4(13) . . ? C17 C18 H18 123.3 . . ? C18 C17 H17 116.9 . . ? C18 C17 N4 126.3(14) . . ? N4 C17 H17 116.9 . . ? N2 C10 N3 118.0(10) . . ? N2 C10 N1 123.7(10) . . ? N1 C10 N3 118.2(9) . . ? C10 N3 C3 115.7(11) . . ? C10 N3 C4' 118.7(11) . . ? C10 N3 C3' 127.4(12) . . ? C10 N3 C4 119.5(10) . . ? C4' N3 C3 124.6(12) . . ? C3' N3 C4 112.6(12) . . ? N2 C9 H9 117.6 . . ? C8 C9 N2 124.9(13) . . ? C8 C9 H9 117.6 . . ? C20 N4 Ag1 128.0(8) . . ? C20 N4 C17 115.9(11) . . ? C17 N4 Ag1 114.7(9) . . ? Ag1 C11 H11A 94.8 . . ? Ag1 C11 H11B 96.3 . . ? H11A C11 H11B 120.0 . . ? C12 C11 Ag1 78.9(9) . . ? C12 C11 H11A 120.0 . . ? C12 C11 H11B 120.0 . . ? Ag1 C12 H12 100.4 . . ? C11 C12 Ag1 69.6(8) . . ? C11 C12 H12 118.9 . . ? C11 C12 C13 122.2(12) . . ? C13 C12 Ag1 100.0(8) . . ? C13 C12 H12 118.9 . . ? N6 C13 C12 116.4(11) . . ? N6 C13 H13A 108.2 . . ? N6 C13 H13B 108.2 . . ? C12 C13 H13A 108.2 . . ? C12 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? N6 C14 H14A 108.0 . . ? N6 C14 H14B 108.0 . . ? N6 C14 C15 117.1(14) . . ? H14A C14 H14B 107.3 . . ? C15 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? Ag2 C15 H15 100.2 . . ? C14 C15 Ag2 98.6(10) . . ? C14 C15 H15 119.8 . . ? C16 C15 Ag2 71.0(9) . . ? C16 C15 C14 120.4(18) . . ? C16 C15 H15 119.8 . . ? Ag2 C16 H16A 94.8 . . ? Ag2 C16 H16B 96.6 . . ? C15 C16 Ag2 78.5(13) . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? C10 N1 Ag2 129.8(7) . 3_645 ? C10 N1 C7 115.2(10) . . ? C7 N1 Ag2 114.3(8) . 3_645 ? C9 C8 H8 123.0 . . ? C9 C8 C7 114.0(12) . . ? C7 C8 H8 123.0 . . ? N1 C7 H7 117.7 . . ? C8 C7 N1 124.6(12) . . ? C8 C7 H7 117.7 . . ? Ag2 C1 H1A 92.2 3_645 . ? Ag2 C1 H1B 102.7 3_645 . ? H1A C1 H1B 120.0 . . ? C2' C1 Ag2 75(2) . 3_645 ? C2' C1 H1A 120.0 . . ? C2' C1 H1B 120.0 . . ? Ag2 C2' H2'A 105.2 3_645 . ? C1 C2' Ag2 70(3) . 3_645 ? C1 C2' H2'A 120.8 . . ? C3 C2' Ag2 94(3) . 3_645 ? C3 C2' C1 118(4) . . ? C3 C2' H2'A 120.9 . . ? N3 C3 H3A 107.0 . . ? N3 C3 H3B 107.0 . . ? C2' C3 N3 121(3) . . ? C2' C3 H3A 107.0 . . ? C2' C3 H3B 107.0 . . ? H3A C3 H3B 106.8 . . ? N3 C4' H4'A 109.9 . . ? N3 C4' H4'B 109.9 . . ? N3 C4' C5' 108.8(19) . . ? H4'A C4' H4'B 108.3 . . ? C5' C4' H4'A 109.9 . . ? C5' C4' H4'B 109.9 . . ? Ag1 C5' H5'A 94.6 . . ? C4' C5' Ag1 100.2(15) . . ? C4' C5' H5'A 118.9 . . ? C6' C5' Ag1 75.3(16) . . ? C6' C5' C4' 122(2) . . ? C6' C5' H5'A 118.9 . . ? Ag1 C6' H6'A 100.4 . . ? Ag1 C6' H6'B 95.4 . . ? C5' C6' Ag1 74.0(16) . . ? C5' C6' H6'A 120.0 . . ? C5' C6' H6'B 120.0 . . ? H6'A C6' H6'B 120.0 . . ? Ag2 C1' H1'A 113.3 3_645 . ? Ag2 C1' H1'B 85.7 3_645 . ? H1'A C1' H1'B 120.0 . . ? C2 C1' Ag2 71(4) . 3_645 ? C2 C1' H1'A 120.0 . . ? C2 C1' H1'B 120.0 . . ? Ag2 C2 H2A 81.4 3_645 . ? C1' C2 Ag2 77(3) . 3_645 ? C1' C2 H2A 116.2 . . ? C1' C2 C3' 128(7) . . ? C3' C2 Ag2 111(4) . 3_645 ? C3' C2 H2A 116.2 . . ? N3 C3' C2 112(4) . . ? N3 C3' H3'A 109.2 . . ? N3 C3' H3'B 109.2 . . ? C2 C3' H3'A 109.2 . . ? C2 C3' H3'B 109.2 . . ? H3'A C3' H3'B 107.9 . . ? N3 C4 H4A 107.4 . . ? N3 C4 H4B 107.4 . . ? H4A C4 H4B 107.0 . . ? C5 C4 N3 120(2) . . ? C5 C4 H4A 107.4 . . ? C5 C4 H4B 107.4 . . ? Ag1 C5 H5A 95.7 . . ? C4 C5 Ag1 101.3(19) . . ? C4 C5 H5A 122.3 . . ? C6 C5 Ag1 72.4(18) . . ? C6 C5 C4 115(3) . . ? C6 C5 H5A 122.3 . . ? Ag1 C6 H6A 100.9 . . ? Ag1 C6 H6B 93.5 . . ? C5 C6 Ag1 75.5(19) . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? _shelx_estimated_absorpt_T_max 0.902 _shelx_estimated_absorpt_T_min 0.630 _shelx_hkl_checksum 46064 _database_code_depnum_ccdc_archive 'CCDC 940154' ####################################################################### # # 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_complex9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Ag2 N6 O, 2(C F3 O3 S)' _chemical_formula_sum 'C22 H28 Ag2 F6 N6 O7 S2' _chemical_formula_weight 882.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.6969(3) _cell_length_b 12.9740(3) _cell_length_c 20.0150(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3037.39(13) _cell_formula_units_Z 4 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9844 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6114 _exptl_absorpt_correction_T_max 0.9146 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58870 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5366 _reflns_number_gt 5028 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(15) _refine_ls_number_reflns 5366 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0431 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag2 Ag 0.62062(2) 0.742137(19) -0.148173(10) 0.02172(6) Uani 1 1 d . . . C11 C 0.7694(3) 0.4602(3) 0.00740(14) 0.0201(7) Uani 1 1 d . . . H11A H 0.8036 0.3992 0.0243 0.024 Uiso 1 1 calc R . . C12 C 0.8398(3) 0.5394(3) -0.01238(14) 0.0222(7) Uani 1 1 d . . . H12A H 0.9207 0.5348 -0.0089 0.027 Uiso 1 1 calc R . . C13 C 0.7866(3) 0.6258(2) -0.03759(14) 0.0206(8) Uani 1 1 d . . . H13A H 0.8326 0.6825 -0.0509 0.025 Uiso 1 1 calc R . . C14 C 0.6113(3) 0.5528(2) -0.02208(13) 0.0132(6) Uani 1 1 d . . . C15 C 0.4211(3) 0.4714(2) -0.02357(14) 0.0200(7) Uani 1 1 d . . . H15A H 0.4602 0.4133 -0.0460 0.024 Uiso 1 1 calc R . . H15B H 0.3506 0.4864 -0.0492 0.024 Uiso 1 1 calc R . . C16 C 0.3873(3) 0.4373(2) 0.04564(16) 0.0234(7) Uani 1 1 d . . . H16A H 0.3405 0.3777 0.0491 0.028 Uiso 1 1 calc R . . C17 C 0.4169(3) 0.4830(3) 0.10175(15) 0.0279(8) Uani 1 1 d . . . H17A H 0.4637 0.5428 0.1007 0.033 Uiso 1 1 calc R . . H17B H 0.3916 0.4560 0.1433 0.033 Uiso 1 1 calc R . . C18 C 0.4416(3) 0.6588(2) -0.04254(13) 0.0175(6) Uani 1 1 d . . . H18A H 0.4876 0.7148 -0.0224 0.021 Uiso 1 1 calc R . . H18B H 0.3649 0.6606 -0.0216 0.021 Uiso 1 1 calc R . . C19 C 0.4288(3) 0.6799(2) -0.11648(15) 0.0224(7) Uani 1 1 d . . . H19A H 0.3926 0.7425 -0.1292 0.027 Uiso 1 1 calc R . . C20 C 0.4644(3) 0.6177(3) -0.16507(15) 0.0264(8) Uani 1 1 d . . . H20A H 0.5010 0.5544 -0.1543 0.032 Uiso 1 1 calc R . . H20B H 0.4532 0.6365 -0.2105 0.032 Uiso 1 1 calc R . . N4 N 0.6551(2) 0.4647(2) 0.00406(11) 0.0172(6) Uani 1 1 d . . . N5 N 0.6729(2) 0.6335(2) -0.04412(11) 0.0172(6) Uani 1 1 d . . . N6 N 0.4950(2) 0.5611(2) -0.02681(11) 0.0157(6) Uani 1 1 d . . . Ag1 Ag 0.56296(2) 0.349760(19) 0.079430(11) 0.02121(6) Uani 1 1 d . . . C1 C 0.7498(3) 0.4520(3) 0.29135(15) 0.0231(8) Uani 1 1 d . . . H1A H 0.7633 0.4757 0.3355 0.028 Uiso 1 1 calc R . . C2 C 0.7364(3) 0.5236(3) 0.24139(16) 0.0261(8) Uani 1 1 d . . . H2A H 0.7426 0.5954 0.2498 0.031 Uiso 1 1 calc R . . C3 C 0.7136(3) 0.4856(2) 0.17834(16) 0.0219(8) Uani 1 1 d . . . H3A H 0.7055 0.5329 0.1424 0.026 Uiso 1 1 calc R . . C4 C 0.7192(3) 0.3204(2) 0.21774(14) 0.0152(7) Uani 1 1 d . . . C5 C 0.6970(3) 0.1437(2) 0.25862(14) 0.0188(7) Uani 1 1 d . . . H5A H 0.6465 0.0872 0.2435 0.023 Uiso 1 1 calc R . . H5B H 0.6591 0.1779 0.2969 0.023 Uiso 1 1 calc R . . C6 C 0.8080(3) 0.0979(2) 0.28231(14) 0.0212(7) Uani 1 1 d . . . H6A H 0.8035 0.0468 0.3162 0.025 Uiso 1 1 calc R . . C7 C 0.9118(3) 0.1220(3) 0.26037(15) 0.0238(8) Uani 1 1 d . . . H7A H 0.9208 0.1727 0.2265 0.029 Uiso 1 1 calc R . . H7B H 0.9770 0.0886 0.2786 0.029 Uiso 1 1 calc R . . C8 C 0.7274(3) 0.1789(2) 0.13721(14) 0.0185(7) Uani 1 1 d . . . H8A H 0.7629 0.1098 0.1405 0.022 Uiso 1 1 calc R . . H8B H 0.7827 0.2248 0.1144 0.022 Uiso 1 1 calc R . . C9 C 0.6215(3) 0.1705(2) 0.09418(13) 0.0199(7) Uani 1 1 d . . . H9A H 0.6329 0.1572 0.0480 0.024 Uiso 1 1 calc R . . C10 C 0.5143(3) 0.1798(2) 0.11482(16) 0.0241(8) Uani 1 1 d . . . H10A H 0.4986 0.1930 0.1606 0.029 Uiso 1 1 calc R . . H10B H 0.4532 0.1732 0.0839 0.029 Uiso 1 1 calc R . . N1 N 0.7445(2) 0.3502(2) 0.28059(11) 0.0183(5) Uani 1 1 d . . . N2 N 0.7024(2) 0.38548(19) 0.16596(11) 0.0184(6) Uani 1 1 d . . . N3 N 0.7084(2) 0.21807(19) 0.20473(11) 0.0162(6) Uani 1 1 d . . . S1 S 0.03519(7) 0.33485(6) 0.10417(3) 0.01901(18) Uani 1 1 d . . . O1 O -0.02608(19) 0.27987(17) 0.05299(10) 0.0257(5) Uani 1 1 d . . . O2 O 0.0994(2) 0.42182(16) 0.08024(13) 0.0360(6) Uani 1 1 d . . . O3 O -0.0258(2) 0.3503(2) 0.16516(10) 0.0363(6) Uani 1 1 d . . . C21 C 0.1481(3) 0.2449(3) 0.12761(15) 0.0247(7) Uani 1 1 d . . . F1 F 0.22005(15) 0.22826(14) 0.07722(11) 0.0355(5) Uani 1 1 d . . . F2 F 0.2100(2) 0.28105(18) 0.17798(11) 0.0552(7) Uani 1 1 d . . . F3 F 0.10662(17) 0.15334(15) 0.14532(9) 0.0355(5) Uani 1 1 d . . . S2 S 0.59857(8) 0.78151(6) 0.11857(4) 0.0235(2) Uani 1 1 d . . . O4 O 0.6298(3) 0.8571(2) 0.07003(12) 0.0663(10) Uani 1 1 d . . . O5 O 0.6851(2) 0.70844(18) 0.13307(14) 0.0451(7) Uani 1 1 d . . . O6 O 0.4858(2) 0.7391(2) 0.11193(12) 0.0418(7) Uani 1 1 d . . . C22 C 0.5898(3) 0.8603(3) 0.19329(14) 0.0284(8) Uani 1 1 d . . . F4 F 0.5559(3) 0.8046(2) 0.24500(10) 0.0709(9) Uani 1 1 d . . . F5 F 0.51628(19) 0.93665(18) 0.18690(12) 0.0539(7) Uani 1 1 d . . . F6 F 0.68992(19) 0.90109(17) 0.20930(11) 0.0446(6) Uani 1 1 d . . . O7 O 0.6595(4) 0.8699(2) -0.06456(14) 0.0560(10) Uani 1 1 d . . . H77A H 0.644(4) 0.858(4) -0.024(3) 0.087(18) Uiso 1 1 d . . . H77B H 0.622(4) 0.923(4) -0.068(2) 0.076(18) Uiso 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 Ag2 0.02659(14) 0.02061(13) 0.01796(10) 0.00138(11) 0.00429(10) -0.00153(12) C11 0.018(2) 0.023(2) 0.0193(16) -0.0022(14) -0.0040(13) 0.0059(15) C12 0.0155(18) 0.030(2) 0.0211(15) -0.0012(14) -0.0048(13) 0.0011(15) C13 0.0199(18) 0.024(2) 0.0183(15) -0.0034(14) -0.0008(13) -0.0089(15) C14 0.0148(17) 0.0153(17) 0.0094(13) -0.0034(12) -0.0016(12) -0.0028(15) C15 0.0154(18) 0.0184(18) 0.0260(16) 0.0010(14) -0.0038(14) -0.0043(14) C16 0.0123(17) 0.0189(17) 0.0391(18) 0.0067(15) 0.0092(15) -0.0008(15) C17 0.031(2) 0.0277(19) 0.0255(16) 0.0067(14) 0.0126(15) 0.0084(16) C18 0.0137(15) 0.0169(16) 0.0218(14) -0.0006(13) 0.0035(13) 0.0002(16) C19 0.0171(17) 0.0224(18) 0.0278(16) 0.0097(14) -0.0045(15) 0.0027(15) C20 0.024(2) 0.036(2) 0.0196(16) 0.0027(14) -0.0055(13) -0.0033(16) N4 0.0166(15) 0.0188(15) 0.0163(12) 0.0003(11) -0.0004(10) 0.0012(12) N5 0.0152(14) 0.0195(16) 0.0169(12) -0.0007(11) -0.0005(10) -0.0041(12) N6 0.0135(15) 0.0151(15) 0.0186(12) 0.0012(11) -0.0005(11) -0.0001(12) Ag1 0.02276(13) 0.01901(13) 0.02186(11) 0.00449(10) -0.00130(11) 0.00059(12) C1 0.0278(19) 0.0225(19) 0.0191(16) -0.0050(14) -0.0034(14) 0.0026(16) C2 0.034(2) 0.0151(18) 0.0288(18) 0.0004(14) -0.0055(15) -0.0004(16) C3 0.026(2) 0.0185(18) 0.0211(16) 0.0036(14) -0.0021(14) -0.0003(15) C4 0.0139(16) 0.0194(18) 0.0123(14) -0.0011(13) 0.0012(12) -0.0020(13) C5 0.0261(18) 0.0142(16) 0.0162(14) 0.0000(13) 0.0022(13) -0.0027(16) C6 0.034(2) 0.0161(17) 0.0136(15) 0.0035(13) -0.0043(15) -0.0008(16) C7 0.024(2) 0.025(2) 0.0218(15) -0.0018(13) -0.0046(13) 0.0042(15) C8 0.0210(18) 0.0170(17) 0.0175(15) -0.0006(12) -0.0004(13) 0.0057(14) C9 0.0304(19) 0.0137(16) 0.0155(14) -0.0010(12) -0.0013(14) -0.0045(16) C10 0.033(2) 0.0187(18) 0.0207(15) 0.0008(14) -0.0064(15) -0.0060(15) N1 0.0213(14) 0.0169(14) 0.0166(12) -0.0034(12) -0.0027(10) -0.0005(13) N2 0.0221(15) 0.0158(14) 0.0173(13) 0.0002(10) -0.0017(11) -0.0027(12) N3 0.0223(15) 0.0157(14) 0.0105(12) 0.0020(10) 0.0005(10) 0.0003(12) S1 0.0196(4) 0.0180(4) 0.0194(4) 0.0010(3) -0.0001(3) 0.0010(4) O1 0.0252(13) 0.0269(14) 0.0249(11) -0.0006(10) -0.0081(9) 0.0011(10) O2 0.0397(16) 0.0169(12) 0.0513(14) 0.0085(11) 0.0044(13) -0.0059(11) O3 0.0341(15) 0.0488(16) 0.0260(12) -0.0040(12) 0.0070(10) 0.0124(14) C21 0.0210(18) 0.0231(19) 0.0299(16) -0.0036(16) -0.0037(13) -0.0008(17) F1 0.0215(11) 0.0266(12) 0.0584(12) -0.0045(11) 0.0145(10) 0.0002(9) F2 0.0484(15) 0.0597(17) 0.0576(13) -0.0203(12) -0.0371(12) 0.0101(13) F3 0.0369(12) 0.0281(11) 0.0415(10) 0.0134(10) -0.0011(10) 0.0030(10) S2 0.0335(5) 0.0173(4) 0.0197(4) -0.0016(3) -0.0004(3) 0.0041(4) O4 0.138(3) 0.0371(16) 0.0236(13) 0.0083(13) 0.0262(16) -0.004(2) O5 0.0255(15) 0.0199(13) 0.090(2) -0.0089(14) -0.0043(15) 0.0079(12) O6 0.0310(14) 0.0425(16) 0.0517(14) -0.0222(14) -0.0190(12) 0.0042(14) C22 0.030(2) 0.032(2) 0.0223(16) -0.0046(15) -0.0003(14) -0.0063(18) F4 0.104(2) 0.0881(19) 0.0207(10) 0.0006(11) 0.0131(12) -0.0500(18) F5 0.0329(14) 0.0437(15) 0.0853(17) -0.0369(13) 0.0019(12) 0.0078(12) F6 0.0325(13) 0.0428(14) 0.0584(14) -0.0185(11) -0.0088(11) -0.0132(11) O7 0.124(3) 0.0198(16) 0.0248(15) 0.0040(12) 0.0043(16) 0.0064(18) _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 Ag2 O7 2.399(3) . ? Ag2 N1 2.441(2) 2_664 ? Ag2 C20 2.462(3) . ? Ag2 C19 2.467(3) . ? Ag2 C7 2.569(3) 2_664 ? Ag2 N5 2.588(2) . ? Ag2 C6 2.634(3) 2_664 ? C11 N4 1.340(4) . ? C11 C12 1.375(5) . ? C11 H11A 0.9500 . ? C12 C13 1.378(4) . ? C12 H12A 0.9500 . ? C13 N5 1.340(4) . ? C13 H13A 0.9500 . ? C14 N5 1.345(4) . ? C14 N4 1.358(4) . ? C14 N6 1.368(4) . ? C15 N6 1.451(4) . ? C15 C16 1.507(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.317(4) . ? C16 Ag1 2.444(3) . ? C16 H16A 0.9500 . ? C17 Ag1 2.471(3) . ? C17 H17A 0.9500 . ? C17 H17B 0.9500 . ? C18 N6 1.448(4) . ? C18 C19 1.513(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.331(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C20 H20B 0.9500 . ? N4 Ag1 2.379(3) . ? Ag1 C10 2.385(3) . ? Ag1 N2 2.424(2) . ? Ag1 C9 2.443(3) . ? C1 N1 1.339(4) . ? C1 C2 1.374(4) . ? C1 H1A 0.9500 . ? C2 C3 1.381(4) . ? C2 H2A 0.9500 . ? C3 N2 1.329(4) . ? C3 H3A 0.9500 . ? C4 N2 1.351(4) . ? C4 N1 1.349(4) . ? C4 N3 1.359(4) . ? C5 N3 1.453(4) . ? C5 C6 1.505(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.328(4) . ? C6 Ag2 2.634(3) 2_665 ? C6 H6A 0.9500 . ? C7 Ag2 2.569(3) 2_665 ? C7 H7A 0.9500 . ? C7 H7B 0.9500 . ? C8 N3 1.461(4) . ? C8 C9 1.512(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.325(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C10 H10B 0.9500 . ? N1 Ag2 2.441(2) 2_665 ? S1 O3 1.428(2) . ? S1 O2 1.437(2) . ? S1 O1 1.439(2) . ? S1 C21 1.824(3) . ? C21 F2 1.327(4) . ? C21 F1 1.331(3) . ? C21 F3 1.331(4) . ? S2 O5 1.416(3) . ? S2 O4 1.428(3) . ? S2 O6 1.435(2) . ? S2 C22 1.814(3) . ? C22 F4 1.323(4) . ? C22 F5 1.318(4) . ? C22 F6 1.325(4) . ? O7 H77A 0.85(5) . ? O7 H77B 0.83(5) . ? 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 Ag2 N1 128.63(11) . 2_664 ? O7 Ag2 C20 133.61(11) . . ? N1 Ag2 C20 94.44(10) 2_664 . ? O7 Ag2 C19 102.64(12) . . ? N1 Ag2 C19 125.26(10) 2_664 . ? C20 Ag2 C19 31.34(10) . . ? O7 Ag2 C7 92.92(10) . 2_664 ? N1 Ag2 C7 90.92(9) 2_664 2_664 ? C20 Ag2 C7 104.03(11) . 2_664 ? C19 Ag2 C7 105.86(10) . 2_664 ? O7 Ag2 N5 76.72(9) . . ? N1 Ag2 N5 92.86(8) 2_664 . ? C20 Ag2 N5 85.91(9) . . ? C19 Ag2 N5 80.20(9) . . ? C7 Ag2 N5 169.07(9) 2_664 . ? O7 Ag2 C6 76.36(10) . 2_664 ? N1 Ag2 C6 82.73(9) 2_664 2_664 ? C20 Ag2 C6 132.79(10) . 2_664 ? C19 Ag2 C6 132.96(10) . 2_664 ? C7 Ag2 C6 29.54(10) 2_664 2_664 ? N5 Ag2 C6 141.20(9) . 2_664 ? N4 C11 C12 123.5(3) . . ? N4 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 116.3(3) . . ? C11 C12 H12A 121.9 . . ? C13 C12 H12A 121.9 . . ? N5 C13 C12 123.0(3) . . ? N5 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? N5 C14 N4 125.4(3) . . ? N5 C14 N6 116.7(3) . . ? N4 C14 N6 117.9(3) . . ? N6 C15 C16 115.6(3) . . ? N6 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? N6 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C15 125.6(3) . . ? C17 C16 Ag1 75.6(2) . . ? C15 C16 Ag1 99.8(2) . . ? C17 C16 H16A 117.2 . . ? C15 C16 H16A 117.2 . . ? Ag1 C16 H16A 94.9 . . ? C16 C17 Ag1 73.3(2) . . ? C16 C17 H17A 120.0 . . ? Ag1 C17 H17A 99.8 . . ? C16 C17 H17B 120.0 . . ? Ag1 C17 H17B 96.7 . . ? H17A C17 H17B 120.0 . . ? N6 C18 C19 114.5(3) . . ? N6 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? N6 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 125.0(3) . . ? C20 C19 Ag2 74.1(2) . . ? C18 C19 Ag2 102.8(2) . . ? C20 C19 H19A 117.5 . . ? C18 C19 H19A 117.5 . . ? Ag2 C19 H19A 93.3 . . ? C19 C20 Ag2 74.6(2) . . ? C19 C20 H20A 120.0 . . ? Ag2 C20 H20A 101.6 . . ? C19 C20 H20B 120.0 . . ? Ag2 C20 H20B 93.7 . . ? H20A C20 H20B 120.0 . . ? C11 N4 C14 115.6(3) . . ? C11 N4 Ag1 113.2(2) . . ? C14 N4 Ag1 126.9(2) . . ? C13 N5 C14 116.2(3) . . ? C13 N5 Ag2 110.69(19) . . ? C14 N5 Ag2 124.13(18) . . ? C14 N6 C18 120.9(3) . . ? C14 N6 C15 121.8(3) . . ? C18 N6 C15 117.0(2) . . ? N4 Ag1 C10 151.13(10) . . ? N4 Ag1 N2 91.62(8) . . ? C10 Ag1 N2 97.18(10) . . ? N4 Ag1 C16 85.09(9) . . ? C10 Ag1 C16 108.14(11) . . ? N2 Ag1 C16 132.45(10) . . ? N4 Ag1 C9 123.11(10) . . ? C10 Ag1 C9 31.84(10) . . ? N2 Ag1 C9 84.66(9) . . ? C16 Ag1 C9 135.38(11) . . ? N4 Ag1 C17 89.41(10) . . ? C10 Ag1 C17 115.35(12) . . ? N2 Ag1 C17 101.67(10) . . ? C16 Ag1 C17 31.07(10) . . ? C9 Ag1 C17 146.94(11) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 116.5(3) . . ? C3 C2 H2A 121.7 . . ? C1 C2 H2A 121.7 . . ? N2 C3 C2 122.5(3) . . ? N2 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? N2 C4 N1 124.6(3) . . ? N2 C4 N3 116.7(2) . . ? N1 C4 N3 118.6(3) . . ? N3 C5 C6 114.6(3) . . ? N3 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? N3 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C5 126.3(3) . . ? C7 C6 Ag2 72.52(19) . 2_665 ? C5 C6 Ag2 97.37(19) . 2_665 ? C7 C6 H6A 116.9 . . ? C5 C6 H6A 116.9 . . ? Ag2 C6 H6A 101.0 2_665 . ? C6 C7 Ag2 77.94(19) . 2_665 ? C6 C7 H7A 120.0 . . ? Ag2 C7 H7A 92.9 2_665 . ? C6 C7 H7B 120.0 . . ? Ag2 C7 H7B 99.1 2_665 . ? H7A C7 H7B 120.0 . . ? N3 C8 C9 115.3(2) . . ? N3 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? N3 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 126.2(3) . . ? C10 C9 Ag1 71.7(2) . . ? C8 C9 Ag1 103.26(19) . . ? C10 C9 H9A 116.9 . . ? C8 C9 H9A 116.9 . . ? Ag1 C9 H9A 95.4 . . ? C9 C10 Ag1 76.5(2) . . ? C9 C10 H10A 120.0 . . ? Ag1 C10 H10A 99.5 . . ? C9 C10 H10B 120.0 . . ? Ag1 C10 H10B 93.9 . . ? H10A C10 H10B 120.0 . . ? C1 N1 C4 116.3(3) . . ? C1 N1 Ag2 111.13(19) . 2_665 ? C4 N1 Ag2 123.1(2) . 2_665 ? C3 N2 C4 117.0(2) . . ? C3 N2 Ag1 112.7(2) . . ? C4 N2 Ag1 121.77(19) . . ? C4 N3 C5 121.0(2) . . ? C4 N3 C8 120.2(2) . . ? C5 N3 C8 118.0(2) . . ? O3 S1 O2 115.80(16) . . ? O3 S1 O1 115.44(14) . . ? O2 S1 O1 114.33(14) . . ? O3 S1 C21 103.39(14) . . ? O2 S1 C21 102.11(15) . . ? O1 S1 C21 103.09(14) . . ? F2 C21 F1 106.7(3) . . ? F2 C21 F3 108.2(3) . . ? F1 C21 F3 106.7(3) . . ? F2 C21 S1 111.4(2) . . ? F1 C21 S1 111.5(2) . . ? F3 C21 S1 112.0(2) . . ? O5 S2 O4 114.59(19) . . ? O5 S2 O6 114.77(16) . . ? O4 S2 O6 115.81(19) . . ? O5 S2 C22 104.38(17) . . ? O4 S2 C22 100.87(16) . . ? O6 S2 C22 103.89(15) . . ? F4 C22 F5 106.9(3) . . ? F4 C22 F6 107.1(3) . . ? F5 C22 F6 107.4(3) . . ? F4 C22 S2 110.7(2) . . ? F5 C22 S2 112.3(2) . . ? F6 C22 S2 112.0(2) . . ? Ag2 O7 H77A 120(4) . . ? Ag2 O7 H77B 115(4) . . ? H77A O7 H77B 97(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.464 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 940155' ####################################################################### # # 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_complex10 _audit_creation_date 2013-05-18 _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 'C19 H24 Ag2 F3 N4 O3 S3, C F3 O3 S' _chemical_formula_sum 'C20 H24 Ag2 F6 N4 O6 S4' _chemical_formula_weight 874.41 _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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8652(3) _cell_length_b 14.0587(5) _cell_length_c 14.8864(6) _cell_angle_alpha 113.746(2) _cell_angle_beta 92.329(2) _cell_angle_gamma 90.687(2) _cell_volume 1504.73(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9968 _cell_measurement_temperature 117(2) _cell_measurement_theta_max 0.00 _cell_measurement_theta_min 0.00 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.779319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max 25.05 _exptl_transmission_factor_min 2.58 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0378 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 30605 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.984 _diffrn_reflns_theta_min 2.581 _diffrn_ambient_temperature 117.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5123 _reflns_number_total 6514 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.53A (Bruker, 2008)' _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 ; SHELXL, 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 1.384 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.132 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 455 _refine_ls_number_reflns 6514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0451 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0662P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1241 _refine_ls_wR_factor_ref 0.1297 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Others Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(C5')=Sof(H5')=Sof(C6')=Sof(H6'A)=Sof(H6'B)= Sof(N2')=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8')=Sof(S2')=Sof(C16')= Sof(H16C)=Sof(H16D)=Sof(C17')=Sof(H17A)=1-FVAR(1) Sof(N2)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)= Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8)=Sof(S2)=Sof(C16)=Sof(H16A)=Sof(H16B)= Sof(C17)=Sof(H17)=FVAR(1) 3.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C7(H7A,H7B), C4'(H4'A,H4'B), C7'(H7'A,H7'B), C13(H13A,H13B), C16(H16A,H16B), C16'(H16C,H16D) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C5(H5), C8(H8), C5'(H5'), C8'(H8'), C11(H11), C14(H14), C17(H17), C17'(H17A) 3.c X=CH2 refined with riding coordinates: C6(H6A,H6B), C6'(H6'A,H6'B), C9(H9A,H9B), C15(H15A,H15B), C18(H17',H18) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.26031(5) 0.07228(3) 0.32881(3) 0.03330(13) Uani 1 1 d . . . . . Ag2 Ag 0.24600(4) -0.37996(3) -0.21650(2) 0.02874(12) Uani 1 1 d . . . . . S4 S 0.72581(13) -0.40351(8) -0.17818(8) 0.0230(2) Uani 1 1 d . . . . . O4 O 0.8869(4) -0.3622(3) -0.1922(2) 0.0322(7) Uani 1 1 d . . . . . O5 O 0.7002(4) -0.5143(2) -0.2305(3) 0.0399(8) Uani 1 1 d . . . . . O6 O 0.5808(4) -0.3440(2) -0.1818(3) 0.0344(8) Uani 1 1 d . . . . . C20 C 0.7430(6) -0.3861(4) -0.0500(4) 0.0358(11) Uani 1 1 d . . . . . F4 F 0.6057(4) -0.4222(3) -0.0237(2) 0.0556(9) Uani 1 1 d . . . . . F5 F 0.7653(4) -0.2870(3) 0.0100(2) 0.0647(10) Uani 1 1 d . . . . . F6 F 0.8760(4) -0.4358(3) -0.0324(2) 0.0511(9) Uani 1 1 d . . . . . S1 S 0.2667(2) -0.29502(10) 0.16624(11) 0.0484(4) Uani 1 1 d . . . . . C1 C 0.2598(7) -0.2518(4) 0.2907(4) 0.0410(12) Uani 1 1 d . . . . . H1 H 0.2597 -0.2956 0.3254 0.049 Uiso 1 1 calc R U . . . C2 C 0.2545(6) -0.1493(4) 0.3325(4) 0.0351(11) Uani 1 1 d . . . . . H2 H 0.2492 -0.1124 0.4016 0.042 Uiso 1 1 calc R U . . . N1 N 0.2572(5) -0.0988(3) 0.2695(3) 0.0293(9) Uani 1 1 d . . . . . C3 C 0.2646(9) -0.1664(4) 0.1791(4) 0.0475(15) Uani 1 1 d . . . . . N2 N 0.3028(10) -0.1407(5) 0.1016(4) 0.0306(15) Uani 0.662(7) 1 d . . P A 1 C4 C 0.3429(11) -0.0362(6) 0.1116(6) 0.045(2) Uani 0.662(7) 1 d . . P A 1 H4A H 0.4498 -0.0117 0.1526 0.054 Uiso 0.662(7) 1 calc R U P A 1 H4B H 0.3646 -0.0386 0.0457 0.054 Uiso 0.662(7) 1 calc R U P A 1 C5 C 0.2166(13) 0.0378(7) 0.1535(6) 0.040(2) Uani 0.662(7) 1 d . . P A 1 H5 H 0.1027 0.0119 0.1475 0.048 Uiso 0.662(7) 1 calc R U P A 1 C6 C 0.2430(14) 0.1413(8) 0.2009(9) 0.041(3) Uani 0.662(7) 1 d . . P A 1 H6A H 0.3548 0.1708 0.2086 0.050 Uiso 0.662(7) 1 calc R U P A 1 H6B H 0.1499 0.1849 0.2265 0.050 Uiso 0.662(7) 1 calc R U P A 1 C7 C 0.3413(10) -0.2218(6) 0.0058(6) 0.0347(18) Uani 0.662(7) 1 d . . P A 1 H7A H 0.3501 -0.2895 0.0111 0.042 Uiso 0.662(7) 1 calc R U P A 1 H7B H 0.4521 -0.2050 -0.0146 0.042 Uiso 0.662(7) 1 calc R U P A 1 C8 C 0.2057(12) -0.2292(6) -0.0690(6) 0.0261(19) Uani 0.662(7) 1 d . . P A 1 H8 H 0.0954 -0.2551 -0.0652 0.031 Uiso 0.662(7) 1 calc R U P A 1 C4' C 0.157(2) -0.0359(10) 0.1113(9) 0.033(4) Uani 0.338(7) 1 d . . P A 2 H4'A H 0.0536 -0.0126 0.1487 0.039 Uiso 0.338(7) 1 calc R U P A 2 H4'B H 0.1332 -0.0366 0.0452 0.039 Uiso 0.338(7) 1 calc R U P A 2 C5' C 0.303(2) 0.0463(13) 0.1635(13) 0.034(4) Uiso 0.338(7) 1 d . . P A 2 H5' H 0.4146 0.0202 0.1565 0.041 Uiso 0.338(7) 1 calc R U P A 2 C6' C 0.293(2) 0.1507(19) 0.2179(16) 0.030(5) Uiso 0.338(7) 1 d . . P A 2 H6'A H 0.1850 0.1822 0.2279 0.036 Uiso 0.338(7) 1 calc R U P A 2 H6'B H 0.3935 0.1918 0.2456 0.036 Uiso 0.338(7) 1 calc R U P A 2 N2' N 0.187(2) -0.1419(9) 0.0997(8) 0.030(3) Uani 0.338(7) 1 d . . P A 2 C7' C 0.1527(18) -0.2272(12) 0.0011(10) 0.035(4) Uani 0.338(7) 1 d . . P A 2 H7'A H 0.1492 -0.2950 0.0067 0.043 Uiso 0.338(7) 1 calc R U P A 2 H7'B H 0.0409 -0.2178 -0.0268 0.043 Uiso 0.338(7) 1 calc R U P A 2 C8' C 0.288(2) -0.2257(12) -0.0637(13) 0.027(4) Uani 0.338(7) 1 d . . P A 2 H8' H 0.4018 -0.2415 -0.0530 0.033 Uiso 0.338(7) 1 calc R U P A 2 C9 C 0.2378(8) -0.1990(4) -0.1440(4) 0.0415(13) Uani 1 1 d . . . . . H9A H 0.3479 -0.1731 -0.1483 0.050 Uiso 1 1 calc R U . A 1 H9B H 0.1498 -0.2042 -0.1915 0.050 Uiso 1 1 calc R U . A 1 S2 S 0.2576(5) -0.5312(3) -0.5682(3) 0.0341(8) Uani 0.662(7) 1 d . . P A 1 S2' S 0.2092(11) -0.5580(6) -0.5585(6) 0.0411(17) Uani 0.338(7) 1 d . . P A 2 C10 C 0.2957(8) -0.4068(6) -0.5182(4) 0.0551(17) Uani 1 1 d . . . . . C11 C 0.2876(6) -0.3662(4) -0.4216(4) 0.0399(12) Uani 1 1 d . . . . . H11 H 0.3122 -0.2945 -0.3833 0.048 Uiso 1 1 calc R U . . . N3 N 0.2414(5) -0.4336(3) -0.3792(3) 0.0370(10) Uani 1 1 d . . . . . C12 C 0.2136(6) -0.5294(4) -0.4484(4) 0.0406(14) Uani 1 1 d . . . . . N4 N 0.1632(6) -0.6121(4) -0.4315(4) 0.0601(16) Uani 1 1 d . . . . . C13 C 0.1369(7) -0.7138(4) -0.5143(5) 0.063(2) Uani 1 1 d . . . . . H13A H 0.1114 -0.7039 -0.5755 0.075 Uiso 1 1 calc R U . . . H13B H 0.0386 -0.7513 -0.5027 0.075 Uiso 1 1 calc R U . . . C14 C 0.2953(6) -0.7777(4) -0.5253(4) 0.0421(13) Uani 1 1 d . . . . . H14 H 0.3920 -0.7569 -0.5499 0.051 Uiso 1 1 calc R U . . . C15 C 0.3098(10) -0.8597(5) -0.5035(5) 0.068(2) Uani 1 1 d . . . . . H15A H 0.2162 -0.8831 -0.4786 0.081 Uiso 1 1 calc R U . . . H15B H 0.4140 -0.8952 -0.5127 0.081 Uiso 1 1 calc R U . . . C16 C 0.1119(8) -0.6019(5) -0.3417(5) 0.0269(16) Uani 0.662(7) 1 d . . P A 1 H16A H 0.0647 -0.6695 -0.3466 0.032 Uiso 0.662(7) 1 calc R U P A 1 H16B H 0.0204 -0.5508 -0.3212 0.032 Uiso 0.662(7) 1 calc R U P A 1 C17 C 0.2563(11) -0.5667(6) -0.2654(7) 0.0287(17) Uani 0.662(7) 1 d . . P A 1 H17 H 0.3693 -0.5758 -0.2870 0.034 Uiso 0.662(7) 1 calc R U P A 1 C16' C 0.256(2) -0.6230(14) -0.3211(13) 0.044(4) Uani 0.338(7) 1 d . . P A 2 H16C H 0.2496 -0.6966 -0.3298 0.053 Uiso 0.338(7) 1 calc R U P A 2 H16D H 0.3781 -0.6009 -0.3124 0.053 Uiso 0.338(7) 1 calc R U P A 2 C17' C 0.168(2) -0.5589(13) -0.2324(16) 0.042(4) Uani 0.338(7) 1 d . . P A 2 H17A H 0.0490 -0.5515 -0.2384 0.050 Uiso 0.338(7) 1 calc R U P A 2 C18 C 0.2330(8) -0.5195(5) -0.1603(5) 0.0450(13) Uani 1 1 d . . . . . H17' H 0.1215 -0.5094 -0.1366 0.054 Uiso 1 1 calc R U . A 1 H18 H 0.3293 -0.4986 -0.1154 0.054 Uiso 1 1 calc R U . A 1 S3 S -0.22658(16) 0.06239(12) 0.33835(10) 0.0457(4) Uani 1 1 d . . . . . C19 C -0.2366(7) -0.0790(5) 0.2559(7) 0.063(2) Uani 1 1 d . . . . . O1 O -0.2067(13) 0.0657(9) 0.4311(5) 0.202(5) Uani 1 1 d . . . . . O2 O -0.3806(5) 0.1030(3) 0.3095(4) 0.0677(14) Uani 1 1 d . . . . . O3 O -0.0784(5) 0.1028(3) 0.3083(3) 0.0535(10) Uani 1 1 d . . . . . F1 F -0.2541(16) -0.0881(6) 0.1714(7) 0.251(6) Uani 1 1 d . . . . . F2 F -0.1096(7) -0.1233(4) 0.2638(9) 0.257(6) Uani 1 1 d . . . . . F3 F -0.3711(7) -0.1196(5) 0.2762(9) 0.215(5) Uani 1 1 d . . . . . H10 H 0.335(8) -0.368(5) -0.562(5) 0.07(2) Uiso 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 0.0435(2) 0.01800(19) 0.0305(2) 0.00108(15) 0.00707(16) 0.00508(15) Ag2 0.0324(2) 0.0242(2) 0.02169(19) 0.00110(15) -0.00010(14) -0.00054(14) S4 0.0197(5) 0.0198(5) 0.0294(6) 0.0096(5) 0.0025(4) 0.0023(4) O4 0.0187(14) 0.0414(19) 0.041(2) 0.0208(16) 0.0061(13) 0.0006(13) O5 0.051(2) 0.0206(17) 0.043(2) 0.0071(16) 0.0040(17) 0.0009(15) O6 0.0235(15) 0.0317(18) 0.054(2) 0.0232(17) -0.0034(15) 0.0045(13) C20 0.026(2) 0.048(3) 0.030(3) 0.011(2) 0.005(2) 0.004(2) F4 0.0346(16) 0.095(3) 0.0497(19) 0.041(2) 0.0137(14) 0.0010(16) F5 0.061(2) 0.068(2) 0.0375(19) -0.0074(18) 0.0016(16) 0.0017(18) F6 0.0324(15) 0.086(2) 0.0449(18) 0.0364(18) 0.0036(13) 0.0183(16) S1 0.0798(10) 0.0178(6) 0.0444(8) 0.0086(6) 0.0095(7) 0.0050(6) C1 0.057(3) 0.030(3) 0.043(3) 0.022(2) 0.006(3) 0.003(2) C2 0.047(3) 0.033(3) 0.028(3) 0.014(2) 0.003(2) 0.005(2) N1 0.046(2) 0.0184(18) 0.023(2) 0.0066(16) 0.0051(17) 0.0040(16) C3 0.093(5) 0.017(2) 0.028(3) 0.005(2) 0.005(3) 0.005(3) N2 0.045(4) 0.022(3) 0.020(3) 0.004(2) 0.001(3) -0.001(3) C4 0.059(5) 0.045(5) 0.027(4) 0.011(4) 0.000(4) -0.009(4) C5 0.049(6) 0.039(5) 0.037(5) 0.022(4) -0.020(4) -0.010(4) C6 0.037(6) 0.026(5) 0.062(7) 0.021(5) -0.013(5) -0.005(4) C7 0.035(4) 0.036(4) 0.023(4) 0.001(3) -0.001(3) 0.004(3) C8 0.021(4) 0.020(4) 0.024(4) -0.004(3) 0.000(4) 0.000(4) C4' 0.067(10) 0.013(7) 0.011(6) -0.002(5) 0.010(6) 0.002(7) N2' 0.045(8) 0.020(6) 0.018(6) 0.000(5) 0.009(6) -0.003(6) C7' 0.034(7) 0.039(8) 0.020(7) -0.002(6) 0.002(6) -0.013(6) C8' 0.007(6) 0.017(7) 0.040(11) -0.006(6) -0.007(8) 0.004(7) C9 0.062(3) 0.027(3) 0.026(3) 0.001(2) 0.000(2) 0.006(2) S2 0.0358(16) 0.045(2) 0.0172(11) 0.0080(11) 0.0014(10) 0.0056(12) S2' 0.053(4) 0.042(4) 0.021(3) 0.005(2) 0.001(3) 0.016(3) C10 0.059(4) 0.076(4) 0.031(3) 0.023(3) 0.002(3) 0.026(3) C11 0.036(3) 0.049(3) 0.034(3) 0.016(3) -0.003(2) 0.003(2) N3 0.031(2) 0.039(2) 0.026(2) -0.0036(19) 0.0049(17) -0.0085(18) C12 0.020(2) 0.049(3) 0.031(3) -0.008(2) 0.0037(19) 0.001(2) N4 0.057(3) 0.033(3) 0.055(3) -0.020(2) 0.023(3) -0.011(2) C13 0.035(3) 0.035(3) 0.072(4) -0.027(3) 0.006(3) 0.000(2) C14 0.030(2) 0.036(3) 0.036(3) -0.009(2) 0.000(2) -0.006(2) C15 0.107(6) 0.044(4) 0.035(3) 0.000(3) -0.017(4) -0.008(4) C16 0.024(3) 0.017(3) 0.033(4) 0.004(3) 0.007(3) -0.003(3) C17 0.024(4) 0.023(4) 0.041(5) 0.014(4) 0.013(4) 0.002(3) C16' 0.063(12) 0.031(9) 0.033(9) 0.006(8) 0.009(8) 0.016(8) C17' 0.037(10) 0.027(8) 0.061(13) 0.018(9) 0.000(10) -0.003(8) C18 0.038(3) 0.045(3) 0.060(4) 0.029(3) 0.008(3) 0.001(3) S3 0.0324(7) 0.0698(10) 0.0294(7) 0.0142(7) 0.0033(5) -0.0028(6) C19 0.034(3) 0.044(4) 0.104(6) 0.022(4) 0.004(3) -0.005(3) O1 0.254(11) 0.317(13) 0.068(5) 0.116(7) -0.013(6) -0.084(9) O2 0.040(2) 0.052(3) 0.100(4) 0.020(3) -0.004(2) 0.0015(19) O3 0.044(2) 0.051(2) 0.064(3) 0.022(2) 0.0089(19) -0.0033(18) F1 0.384(16) 0.109(6) 0.137(7) -0.079(6) 0.014(9) -0.001(8) F2 0.061(3) 0.070(4) 0.583(19) 0.073(7) -0.007(6) 0.025(3) F3 0.060(3) 0.100(4) 0.491(15) 0.124(7) 0.019(5) -0.021(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 N1 2.202(4) . ? Ag1 C5 2.464(8) . ? Ag1 C6 2.462(12) . ? Ag1 C5' 2.377(17) . ? Ag1 C6' 2.35(2) . ? Ag1 C14 2.343(5) 1_566 ? Ag1 C15 2.299(6) 1_566 ? Ag2 C8 2.395(8) . ? Ag2 C8' 2.436(16) . ? Ag2 C9 2.332(5) . ? Ag2 N3 2.226(4) . ? Ag2 C17 2.429(8) . ? Ag2 C17' 2.496(16) . ? Ag2 C18 2.425(5) . ? S4 O4 1.445(3) . ? S4 O5 1.440(3) . ? S4 O6 1.435(3) . ? S4 C20 1.822(5) . ? C20 F4 1.326(6) . ? C20 F5 1.322(6) . ? C20 F6 1.339(6) . ? S1 C1 1.705(6) . ? S1 C3 1.740(5) . ? C1 H1 0.9500 . ? C1 C2 1.322(7) . ? C2 H2 0.9500 . ? C2 N1 1.386(6) . ? N1 C3 1.302(6) . ? C3 N2 1.383(8) . ? C3 N2' 1.470(15) . ? N2 C4 1.446(10) . ? N2 C7 1.470(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.418(13) . ? C5 H5 0.9500 . ? C5 C6 1.347(13) . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.482(11) . ? C8 H8 0.9500 . ? C8 C9 1.375(10) . ? C4' H4'A 0.9900 . ? C4' H4'B 0.9900 . ? C4' C5' 1.56(2) . ? C4' N2' 1.453(18) . ? C5' H5' 0.9500 . ? C5' C6' 1.37(3) . ? C6' H6'A 0.9500 . ? C6' H6'B 0.9500 . ? N2' C7' 1.486(17) . ? C7' H7'A 0.9900 . ? C7' H7'B 0.9900 . ? C7' C8' 1.47(2) . ? C8' H8' 0.9500 . ? C8' C9 1.430(19) . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? S2 C10 1.619(8) . ? S2 C12 1.820(7) . ? S2' C10 2.061(11) . ? S2' C12 1.521(9) . ? C10 C11 1.320(8) . ? C10 H10 1.06(7) . ? C11 H11 0.9500 . ? C11 N3 1.387(7) . ? N3 C12 1.335(6) . ? C12 N4 1.343(8) . ? N4 C13 1.469(6) . ? N4 C16 1.365(9) . ? N4 C16' 1.837(18) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.519(7) . ? C14 Ag1 2.343(5) 1_544 ? C14 H14 0.9500 . ? C14 C15 1.323(9) . ? C15 Ag1 2.299(6) 1_544 ? C15 H15A 0.9500 . ? C15 H15B 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.501(11) . ? C17 H17 0.9500 . ? C17 C18 1.453(11) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C16' C17' 1.47(3) . ? C17' H17A 0.9500 . ? C17' C18 1.090(18) . ? C18 H17' 0.9500 . ? C18 H18 0.9500 . ? S3 C19 1.868(7) . ? S3 O1 1.365(6) . ? S3 O2 1.466(4) . ? S3 O3 1.453(4) . ? C19 F1 1.213(12) . ? C19 F2 1.210(8) . ? C19 F3 1.298(9) . ? 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 N1 Ag1 C5 82.0(2) . . ? N1 Ag1 C6 113.5(3) . . ? N1 Ag1 C5' 84.0(4) . . ? N1 Ag1 C6' 117.6(6) . . ? N1 Ag1 C14 143.03(19) . 1_566 ? N1 Ag1 C15 109.9(2) . 1_566 ? C6 Ag1 C5 31.7(3) . . ? C6' Ag1 C5' 33.6(7) . . ? C14 Ag1 C5 134.9(3) 1_566 . ? C14 Ag1 C6 103.3(3) 1_566 . ? C14 Ag1 C5' 130.6(5) 1_566 . ? C14 Ag1 C6' 98.0(6) 1_566 . ? C15 Ag1 C5 167.9(3) 1_566 . ? C15 Ag1 C6 136.1(3) 1_566 . ? C15 Ag1 C5' 157.4(5) 1_566 . ? C15 Ag1 C6' 129.7(6) 1_566 . ? C15 Ag1 C14 33.1(2) 1_566 1_566 ? C8 Ag2 C17 137.3(3) . . ? C8 Ag2 C18 102.5(3) . . ? C8' Ag2 C17' 126.3(7) . . ? C9 Ag2 C8 33.8(2) . . ? C9 Ag2 C8' 34.8(4) . . ? C9 Ag2 C17 170.9(2) . . ? C9 Ag2 C17' 154.1(5) . . ? C9 Ag2 C18 136.1(2) . . ? N3 Ag2 C8 142.0(2) . . ? N3 Ag2 C8' 142.6(5) . . ? N3 Ag2 C9 109.41(18) . . ? N3 Ag2 C17 79.7(2) . . ? N3 Ag2 C17' 91.0(5) . . ? N3 Ag2 C18 114.2(2) . . ? C18 Ag2 C8' 102.8(5) . . ? C18 Ag2 C17 34.8(2) . . ? C18 Ag2 C17' 25.5(4) . . ? O4 S4 C20 103.5(2) . . ? O5 S4 O4 115.1(2) . . ? O5 S4 C20 103.2(2) . . ? O6 S4 O4 114.99(19) . . ? O6 S4 O5 114.5(2) . . ? O6 S4 C20 103.2(2) . . ? F4 C20 S4 112.3(3) . . ? F4 C20 F6 106.9(4) . . ? F5 C20 S4 111.6(4) . . ? F5 C20 F4 107.6(4) . . ? F5 C20 F6 106.6(4) . . ? F6 C20 S4 111.5(3) . . ? C1 S1 C3 88.8(2) . . ? S1 C1 H1 124.5 . . ? C2 C1 S1 111.1(4) . . ? C2 C1 H1 124.5 . . ? C1 C2 H2 122.0 . . ? C1 C2 N1 116.0(5) . . ? N1 C2 H2 122.0 . . ? C2 N1 Ag1 120.2(3) . . ? C3 N1 Ag1 129.7(3) . . ? C3 N1 C2 110.0(4) . . ? N1 C3 S1 114.2(4) . . ? N1 C3 N2 123.9(5) . . ? N1 C3 N2' 118.9(6) . . ? N2 C3 S1 120.7(4) . . ? N2' C3 S1 119.4(6) . . ? C3 N2 C4 124.1(6) . . ? C3 N2 C7 120.7(6) . . ? C4 N2 C7 114.0(6) . . ? N2 C4 H4A 108.4 . . ? N2 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C5 C4 N2 115.7(8) . . ? C5 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? Ag1 C5 H5 95.2 . . ? C4 C5 Ag1 101.1(5) . . ? C4 C5 H5 117.0 . . ? C6 C5 Ag1 74.0(6) . . ? C6 C5 C4 126.1(10) . . ? C6 C5 H5 117.0 . . ? Ag1 C6 H6A 99.7 . . ? Ag1 C6 H6B 95.9 . . ? C5 C6 Ag1 74.2(6) . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? N2 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? N2 C7 C8 110.2(6) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? Ag2 C8 H8 90.0 . . ? C7 C8 Ag2 109.4(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 Ag2 70.6(4) . . ? C9 C8 C7 120.7(8) . . ? C9 C8 H8 119.6 . . ? H4'A C4' H4'B 107.3 . . ? C5' C4' H4'A 108.1 . . ? C5' C4' H4'B 108.1 . . ? N2' C4' H4'A 108.1 . . ? N2' C4' H4'B 108.1 . . ? N2' C4' C5' 116.9(14) . . ? Ag1 C5' H5' 100.2 . . ? C4' C5' Ag1 99.1(10) . . ? C4' C5' H5' 115.4 . . ? C6' C5' Ag1 71.9(12) . . ? C6' C5' C4' 129.2(16) . . ? C6' C5' H5' 115.4 . . ? Ag1 C6' H6'A 95.3 . . ? Ag1 C6' H6'B 100.2 . . ? C5' C6' Ag1 74.4(12) . . ? C5' C6' H6'A 120.0 . . ? C5' C6' H6'B 120.0 . . ? H6'A C6' H6'B 120.0 . . ? C3 N2' C7' 119.2(11) . . ? C4' N2' C3 122.3(10) . . ? C4' N2' C7' 118.2(12) . . ? N2' C7' H7'A 109.8 . . ? N2' C7' H7'B 109.8 . . ? H7'A C7' H7'B 108.3 . . ? C8' C7' N2' 109.2(12) . . ? C8' C7' H7'A 109.8 . . ? C8' C7' H7'B 109.8 . . ? Ag2 C8' H8' 93.3 . . ? C7' C8' Ag2 107.7(10) . . ? C7' C8' H8' 121.8 . . ? C9 C8' Ag2 68.6(7) . . ? C9 C8' C7' 116.3(13) . . ? C9 C8' H8' 121.8 . . ? Ag2 C9 H9A 106.9 . . ? Ag2 C9 H9B 87.5 . . ? C8 C9 Ag2 75.6(4) . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? C8' C9 Ag2 76.6(6) . . ? H9A C9 H9B 120.0 . . ? C10 S2 C12 90.0(3) . . ? C12 S2' C10 84.3(5) . . ? S2 C10 H10 119(3) . . ? S2' C10 H10 130(3) . . ? C11 C10 S2 113.5(6) . . ? C11 C10 S2' 103.3(5) . . ? C11 C10 H10 127(4) . . ? C10 C11 H11 121.7 . . ? C10 C11 N3 116.5(6) . . ? N3 C11 H11 121.7 . . ? C11 N3 Ag2 120.6(3) . . ? C12 N3 Ag2 128.9(4) . . ? C12 N3 C11 110.1(4) . . ? N3 C12 S2 109.8(5) . . ? N3 C12 S2' 125.0(6) . . ? N3 C12 N4 124.8(5) . . ? N4 C12 S2 125.4(4) . . ? N4 C12 S2' 109.6(5) . . ? C12 N4 C13 119.6(6) . . ? C12 N4 C16 121.6(5) . . ? C12 N4 C16' 116.9(7) . . ? C13 N4 C16' 112.3(7) . . ? C16 N4 C13 118.1(6) . . ? N4 C13 H13A 109.6 . . ? N4 C13 H13B 109.6 . . ? N4 C13 C14 110.2(5) . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? Ag1 C14 H14 90.0 1_544 . ? C13 C14 Ag1 108.3(3) . 1_544 ? C13 C14 H14 117.2 . . ? C15 C14 Ag1 71.6(3) . 1_544 ? C15 C14 C13 125.6(6) . . ? C15 C14 H14 117.2 . . ? Ag1 C15 H15A 105.6 1_544 . ? Ag1 C15 H15B 89.1 1_544 . ? C14 C15 Ag1 75.3(4) . 1_544 ? C14 C15 H15A 120.0 . . ? C14 C15 H15B 120.0 . . ? H15A C15 H15B 120.0 . . ? N4 C16 H16A 109.3 . . ? N4 C16 H16B 109.3 . . ? N4 C16 C17 111.7(6) . . ? H16A C16 H16B 107.9 . . ? C17 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? Ag2 C17 H17 98.0 . . ? C16 C17 Ag2 99.8(5) . . ? C16 C17 H17 118.2 . . ? C18 C17 Ag2 72.4(4) . . ? C18 C17 C16 123.7(8) . . ? C18 C17 H17 118.2 . . ? N4 C16' H16C 109.2 . . ? N4 C16' H16D 109.2 . . ? H16C C16' H16D 107.9 . . ? C17' C16' N4 111.9(13) . . ? C17' C16' H16C 109.2 . . ? C17' C16' H16D 109.2 . . ? Ag2 C17' H17A 95.2 . . ? C16' C17' Ag2 101.4(13) . . ? C16' C17' H17A 118.3 . . ? C18 C17' Ag2 73.6(9) . . ? C18 C17' C16' 123.4(18) . . ? C18 C17' H17A 118.3 . . ? Ag2 C18 H17' 98.7 . . ? Ag2 C18 H18 98.3 . . ? C17 C18 Ag2 72.7(4) . . ? C17 C18 H17' 120.0 . . ? C17 C18 H18 120.0 . . ? C17' C18 Ag2 80.9(9) . . ? H17' C18 H18 120.0 . . ? O1 S3 C19 104.9(6) . . ? O1 S3 O2 119.8(5) . . ? O1 S3 O3 113.2(4) . . ? O2 S3 C19 104.0(3) . . ? O3 S3 C19 104.2(3) . . ? O3 S3 O2 109.1(3) . . ? F1 C19 S3 108.6(6) . . ? F1 C19 F2 108.4(10) . . ? F1 C19 F3 108.1(9) . . ? F2 C19 S3 112.7(6) . . ? F2 C19 F3 111.3(8) . . ? F3 C19 S3 107.5(6) . . ? _shelx_estimated_absorpt_T_max 0.852 _shelx_estimated_absorpt_T_min 0.497 _shelx_hkl_checksum 31566 _database_code_depnum_ccdc_archive 'CCDC 940156' ####################################################################### # # 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_complex11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H16 Ag Cl N2 O4' _chemical_formula_weight 431.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1378(4) _cell_length_b 10.7654(3) _cell_length_c 13.2121(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.584(2) _cell_angle_gamma 90.00 _cell_volume 1605.35(8) _cell_formula_units_Z 4 _cell_measurement_temperature 116(2) _cell_measurement_reflns_used 6377 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 24.08 _exptl_crystal_description plate _exptl_crystal_colour colour-less _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.827068 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 116(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28656 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2846 _reflns_number_gt 2195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2846 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.6943(5) 0.5927(4) 0.2523(4) 0.0319(5) Uani 0.79(3) 1 d P . 1 Ag1' Ag 0.7109(15) 0.575(2) 0.2686(17) 0.033(2) Uani 0.21(3) 1 d P . 2 Cl1 Cl 1.02481(10) 0.73157(11) 0.35253(8) 0.0365(3) Uani 1 1 d . . . O1 O 1.1156(4) 0.7762(4) 0.4444(3) 0.0775(13) Uani 1 1 d . . . O2 O 0.9688(4) 0.8258(4) 0.2752(3) 0.0651(11) Uani 1 1 d . . . O3 O 1.0693(3) 0.6390(4) 0.2979(3) 0.0518(9) Uani 1 1 d . . . O4 O 0.9353(3) 0.6748(3) 0.3845(3) 0.0519(9) Uani 1 1 d . . . N1 N 0.6630(3) 0.5857(3) 0.4090(3) 0.0320(9) Uani 1 1 d . . . C1 C 0.7074(4) 0.5028(5) 0.4872(4) 0.0391(11) Uani 1 1 d . . . H1A H 0.7585 0.4406 0.4781 0.047 Uiso 1 1 calc R . . C2 C 0.6827(4) 0.5020(5) 0.5825(4) 0.0400(12) Uani 1 1 d . . . H2A H 0.7159 0.4401 0.6364 0.048 Uiso 1 1 calc R . . C3 C 0.6108(4) 0.5909(4) 0.5970(4) 0.0347(11) Uani 1 1 d . . . H3A H 0.5925 0.5910 0.6611 0.042 Uiso 1 1 calc R . . C4 C 0.5625(4) 0.6842(4) 0.5163(3) 0.0281(10) Uani 1 1 d . . . C5 C 0.4869(4) 0.7763(4) 0.5257(3) 0.0352(11) Uani 1 1 d . . . H5A H 0.4671 0.7800 0.5889 0.042 Uiso 1 1 calc R . . C6 C 0.4414(4) 0.8608(5) 0.4456(4) 0.0394(12) Uani 1 1 d . . . H6A H 0.3897 0.9234 0.4530 0.047 Uiso 1 1 calc R . . C7 C 0.4698(4) 0.8576(4) 0.3503(3) 0.0336(10) Uani 1 1 d . . . H7A H 0.4376 0.9184 0.2952 0.040 Uiso 1 1 calc R . . C8 C 0.5428(4) 0.7677(4) 0.3376(3) 0.0264(9) Uani 1 1 d . . . C9 C 0.5904(4) 0.6775(4) 0.4204(3) 0.0246(9) Uani 1 1 d . . . N2 N 0.5707(3) 0.7618(3) 0.2393(3) 0.0341(9) Uani 1 1 d . . . C10 C 0.4580(5) 0.7338(5) 0.1413(3) 0.0510(14) Uani 1 1 d . . . H10A H 0.3978 0.7981 0.1359 0.061 Uiso 1 1 calc R . . H10B H 0.4759 0.7375 0.0740 0.061 Uiso 1 1 calc R . . C11 C 0.4103(5) 0.6133(5) 0.1493(4) 0.0488(14) Uani 1 1 d . . . H11A H 0.4575 0.5431 0.1489 0.059 Uiso 1 1 calc R . . C12 C 0.3067(5) 0.5922(6) 0.1572(5) 0.0639(17) Uani 1 1 d . . . H12A H 0.2567 0.6598 0.1579 0.077 Uiso 1 1 calc R . . H12B H 0.2821 0.5094 0.1622 0.077 Uiso 1 1 calc R . . C13 C 0.6157(5) 0.8838(5) 0.2136(4) 0.0429(12) Uani 1 1 d . . . H13A H 0.6348 0.8751 0.1472 0.051 Uiso 1 1 calc R . . H13B H 0.5538 0.9484 0.1998 0.051 Uiso 1 1 calc R . . C14 C 0.7218(5) 0.9206(5) 0.3054(4) 0.0513(15) Uani 1 1 d . . . H14A H 0.7900 0.8696 0.3218 0.062 Uiso 1 1 calc R . . C15 C 0.7306(4) 1.0252(5) 0.3711(4) 0.0428(13) Uani 1 1 d . . . H15A H 0.6643 1.0785 0.3573 0.051 Uiso 1 1 calc R . . H15B H 0.8029 1.0428 0.4295 0.051 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 0.0392(13) 0.0335(7) 0.0311(8) 0.0025(6) 0.0224(9) 0.0123(7) Ag1' 0.026(3) 0.041(5) 0.033(4) -0.014(3) 0.010(3) 0.013(3) Cl1 0.0437(7) 0.0347(6) 0.0352(6) 0.0008(5) 0.0195(5) 0.0015(5) O1 0.076(3) 0.075(3) 0.077(3) -0.034(2) 0.022(2) -0.027(2) O2 0.083(3) 0.062(3) 0.067(2) 0.025(2) 0.047(2) 0.026(2) O3 0.054(2) 0.049(2) 0.060(2) -0.0100(18) 0.0296(19) 0.0078(19) O4 0.064(2) 0.054(2) 0.049(2) -0.0041(17) 0.0334(18) -0.0112(19) N1 0.037(2) 0.028(2) 0.038(2) -0.0011(16) 0.0220(17) 0.0031(17) C1 0.038(3) 0.040(3) 0.048(3) 0.000(2) 0.026(2) 0.009(2) C2 0.041(3) 0.044(3) 0.037(3) 0.009(2) 0.018(2) 0.007(2) C3 0.040(3) 0.040(3) 0.030(2) -0.0005(19) 0.019(2) -0.004(2) C4 0.031(2) 0.032(3) 0.027(2) -0.0046(18) 0.0163(18) -0.0059(19) C5 0.047(3) 0.035(3) 0.033(2) 0.0003(19) 0.026(2) 0.006(2) C6 0.047(3) 0.036(3) 0.049(3) -0.005(2) 0.033(2) 0.007(2) C7 0.047(3) 0.029(2) 0.035(2) 0.0013(19) 0.027(2) 0.004(2) C8 0.036(2) 0.021(2) 0.030(2) -0.0026(17) 0.0215(19) -0.0059(19) C9 0.027(2) 0.024(2) 0.030(2) -0.0094(17) 0.0185(18) -0.0071(18) N2 0.055(3) 0.024(2) 0.040(2) -0.0027(16) 0.0366(19) -0.0031(18) C10 0.074(4) 0.058(4) 0.026(2) 0.009(2) 0.023(2) 0.024(3) C11 0.065(4) 0.042(3) 0.032(3) -0.006(2) 0.008(3) -0.002(3) C12 0.052(4) 0.076(5) 0.051(3) 0.001(3) 0.004(3) -0.004(3) C13 0.056(3) 0.041(3) 0.044(3) 0.004(2) 0.034(3) 0.000(2) C14 0.046(3) 0.072(4) 0.045(3) 0.016(3) 0.028(3) -0.013(3) C15 0.043(3) 0.063(4) 0.029(2) 0.001(2) 0.021(2) -0.016(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 N1 2.240(5) . ? Ag1 C15 2.261(5) 2_645 ? Ag1 C14 2.372(7) 2_645 ? Ag1 N2 2.324(6) . ? Ag1' N1 2.142(17) . ? Ag1' C14 2.228(16) 2_645 ? Ag1' C15 2.272(15) 2_645 ? Cl1 O1 1.391(4) . ? Cl1 O2 1.422(4) . ? Cl1 O4 1.438(3) . ? Cl1 O3 1.447(4) . ? N1 C1 1.320(6) . ? N1 C9 1.370(5) . ? C1 C2 1.398(6) . ? C1 H1A 0.9500 . ? C2 C3 1.356(7) . ? C2 H2A 0.9500 . ? C3 C4 1.424(6) . ? C3 H3A 0.9500 . ? C4 C5 1.388(6) . ? C4 C9 1.428(5) . ? C5 C6 1.350(6) . ? C5 H5A 0.9500 . ? C6 C7 1.423(6) . ? C6 H6A 0.9500 . ? C7 C8 1.364(6) . ? C7 H7A 0.9500 . ? C8 C9 1.417(6) . ? C8 N2 1.459(5) . ? N2 C13 1.509(6) . ? N2 C10 1.528(6) . ? C10 C11 1.440(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.319(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.462(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.402(7) . ? C14 Ag1' 2.228(16) 2_655 ? C14 Ag1 2.372(7) 2_655 ? C14 H14A 0.9500 . ? C15 Ag1 2.261(5) 2_655 ? C15 Ag1' 2.271(15) 2_655 ? C15 H15A 0.9500 . ? C15 H15B 0.9500 . ? 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 N1 Ag1 C15 155.0(3) . 2_645 ? N1 Ag1 C14 120.6(3) . 2_645 ? C15 Ag1 C14 35.13(19) 2_645 2_645 ? N1 Ag1 N2 76.74(17) . . ? C15 Ag1 N2 128.3(3) 2_645 . ? C14 Ag1 N2 158.4(3) 2_645 . ? N1 Ag1' C14 133.0(13) . 2_645 ? N1 Ag1' C15 169.3(13) . 2_645 ? C14 Ag1' C15 36.3(3) 2_645 2_645 ? O1 Cl1 O2 113.3(3) . . ? O1 Cl1 O4 109.4(2) . . ? O2 Cl1 O4 107.5(2) . . ? O1 Cl1 O3 110.6(3) . . ? O2 Cl1 O3 107.5(2) . . ? O4 Cl1 O3 108.3(2) . . ? C1 N1 C9 119.7(4) . . ? C1 N1 Ag1' 118.5(8) . . ? C9 N1 Ag1' 121.8(8) . . ? C1 N1 Ag1 125.9(3) . . ? C9 N1 Ag1 114.3(3) . . ? N1 C1 C2 123.2(4) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 122.7(4) . . ? C5 C4 C9 119.7(4) . . ? C3 C4 C9 117.6(4) . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 121.0(4) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C8 C7 C6 120.4(4) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C9 119.3(4) . . ? C7 C8 N2 120.9(4) . . ? C9 C8 N2 119.7(4) . . ? N1 C9 C8 120.3(3) . . ? N1 C9 C4 120.4(4) . . ? C8 C9 C4 119.3(4) . . ? C8 N2 C13 112.6(3) . . ? C8 N2 C10 109.6(3) . . ? C13 N2 C10 105.4(4) . . ? C8 N2 Ag1 108.8(3) . . ? C13 N2 Ag1 114.9(3) . . ? C10 N2 Ag1 105.1(3) . . ? C11 C10 N2 111.9(4) . . ? C11 C10 H10A 109.2 . . ? N2 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? N2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 125.6(6) . . ? C12 C11 H11A 117.2 . . ? C10 C11 H11A 117.2 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? C14 C13 N2 109.3(4) . . ? C14 C13 H13A 109.8 . . ? N2 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? N2 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 125.1(5) . . ? C15 C14 Ag1' 73.5(7) . 2_655 ? C13 C14 Ag1' 101.0(7) . 2_655 ? C15 C14 Ag1 68.1(3) . 2_655 ? C13 C14 Ag1 107.2(3) . 2_655 ? C15 C14 H14A 117.4 . . ? C13 C14 H14A 117.4 . . ? Ag1' C14 H14A 95.8 2_655 . ? Ag1 C14 H14A 94.8 2_655 . ? C14 C15 Ag1 76.8(3) . 2_655 ? C14 C15 Ag1' 70.2(7) . 2_655 ? C14 C15 H15A 120.0 . . ? Ag1 C15 H15A 101.8 2_655 . ? Ag1' C15 H15A 101.4 2_655 . ? C14 C15 H15B 120.0 . . ? Ag1 C15 H15B 91.4 2_655 . ? Ag1' C15 H15B 98.1 2_655 . ? H15A C15 H15B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.977 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.097 #===END _database_code_depnum_ccdc_archive 'CCDC 940157'