# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chun-Nam Lok' _publ_contact_author_email cnlok@hku.hk loop_ _publ_author_name 'Kun Yan' 'Chun-Nam Lok' 'Chi-Ming Che' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 773697' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C34 H36 Au N4 O4 S2), Cl4' _chemical_formula_sum 'C136 H144 Au4 Cl4 N16 O16 S8' _chemical_formula_weight 3428.0 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' Au Au -2.0133 8.8022 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.501(5) _cell_length_b 5.6650(10) _cell_length_c 24.806(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.36(3) _cell_angle_gamma 90.00 _cell_volume 3428.0(12) _cell_formula_units_Z 1 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 4 _cell_measurement_theta_max 35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 0.64 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 'marresearch IPDS mar300' _diffrn_measurement_method oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11239 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.63 _reflns_number_total 3010 _reflns_number_gt 2192 _reflns_threshold_expression >2sigma(I) _computing_data_collection marcontrol _computing_cell_refinement scalepack _computing_data_reduction denzo _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+6.3122P] 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 3010 _refine_ls_number_parameters 179 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0427(4) 0.2709(14) 0.1136(3) 0.053(2) Uani 1 1 d . A . C2 C -0.0085(5) 0.5311(19) 0.1606(5) 0.084(3) Uani 1 1 d . A . H2A H -0.0326 0.4778 0.1870 0.101 Uiso 1 1 calc R . . H2B H -0.0204 0.6853 0.1472 0.101 Uiso 1 1 calc R . . C3 C 0.0505(5) 0.5375(19) 0.1848(5) 0.081(3) Uani 1 1 d . A . H3A H 0.0660 0.6942 0.1822 0.097 Uiso 1 1 calc R . . H3B H 0.0537 0.4885 0.2224 0.097 Uiso 1 1 calc R . . C4 C -0.0583(5) 0.290(3) 0.0894(6) 0.066(14) Uiso 0.50 1 d PG A 1 C5 C -0.0809(6) 0.389(2) 0.0411(6) 0.053(4) Uiso 0.50 1 d PG A 1 H5 H -0.0640 0.5181 0.0265 0.063 Uiso 0.50 1 calc PR A 1 C6 C -0.1287(5) 0.296(2) 0.0149(4) 0.054(4) Uiso 0.50 1 d PG A 1 H6 H -0.1439 0.3629 -0.0174 0.065 Uiso 0.50 1 calc PR A 1 C7 C -0.1539(4) 0.104(2) 0.0368(5) 0.052(4) Uiso 0.50 1 d PG A 1 C8 C -0.1313(5) 0.0038(19) 0.0850(5) 0.063(5) Uiso 0.50 1 d PG A 1 H8 H -0.1482 -0.1251 0.0997 0.076 Uiso 0.50 1 calc PR A 1 C9 C -0.0835(6) 0.097(3) 0.1113(5) 0.057(4) Uiso 0.50 1 d PG A 1 H9 H -0.0684 0.0301 0.1436 0.068 Uiso 0.50 1 calc PR A 1 C10 C -0.2165(10) 0.045(4) -0.0429(8) 0.073(6) Uiso 0.50 1 d PD A 1 H10A H -0.2490 -0.0428 -0.0543 0.110 Uiso 0.50 1 calc PR A 1 H10B H -0.1878 0.0026 -0.0649 0.110 Uiso 0.50 1 calc PR A 1 H10C H -0.2240 0.2111 -0.0467 0.110 Uiso 0.50 1 calc PR A 1 O1 O -0.1996(7) -0.007(2) 0.0127(7) 0.077(4) Uiso 0.50 1 d PD A 1 C4' C -0.0568(6) 0.295(3) 0.0842(6) 0.041(9) Uiso 0.50 1 d PG A 2 C5' C -0.0714(6) 0.449(2) 0.0417(7) 0.071(6) Uiso 0.50 1 d PG A 2 H5' H -0.0497 0.5804 0.0364 0.085 Uiso 0.50 1 calc PR A 2 C7' C -0.1183(7) 0.407(2) 0.0071(5) 0.070(5) Uiso 0.50 1 d PG A 2 H7' H -0.1281 0.5101 -0.0213 0.084 Uiso 0.50 1 calc PR A 2 C8' C -0.1507(5) 0.211(3) 0.0151(6) 0.062(5) Uiso 0.50 1 d PG A 2 C6' C -0.1361(5) 0.057(2) 0.0576(6) 0.064(5) Uiso 0.50 1 d PG A 2 H6' H -0.1578 -0.0745 0.0629 0.077 Uiso 0.50 1 calc PR A 2 C9' C -0.0892(6) 0.099(2) 0.0922(6) 0.072(6) Uiso 0.50 1 d PG A 2 H9' H -0.0794 -0.0042 0.1206 0.086 Uiso 0.50 1 calc PR A 2 C10' C -0.2202(12) -0.044(4) -0.0216(14) 0.088(7) Uiso 0.50 1 d PD A 2 H10D H -0.2497 -0.0551 -0.0499 0.132 Uiso 0.50 1 calc PR A 2 H10E H -0.2346 -0.0594 0.0129 0.132 Uiso 0.50 1 calc PR A 2 H10F H -0.1943 -0.1682 -0.0258 0.132 Uiso 0.50 1 calc PR A 2 O1' O -0.1936(7) 0.180(3) -0.0247(6) 0.085(4) Uiso 0.50 1 d PD A 2 C11 C 0.1350(2) 0.3301(12) 0.1584(3) 0.059(2) Uani 1 1 d G A . C12 C 0.1696(3) 0.4927(10) 0.1370(3) 0.080(3) Uani 1 1 d G . . H12 H 0.1549 0.6237 0.1183 0.096 Uiso 1 1 calc R . . C13 C 0.2260(3) 0.4596(12) 0.1437(3) 0.088(3) Uani 1 1 d G . . H13 H 0.2491 0.5684 0.1294 0.106 Uiso 1 1 calc R . . C14 C 0.2479(2) 0.2637(14) 0.1718(3) 0.080(3) Uani 1 1 d G . . C15 C 0.2133(3) 0.1011(11) 0.1931(3) 0.089(3) Uani 1 1 d G . . H15 H 0.2279 -0.0300 0.2119 0.106 Uiso 1 1 calc R . . C16 C 0.1568(3) 0.1342(11) 0.1865(3) 0.081(3) Uani 1 1 d G . . H16 H 0.1337 0.0254 0.2008 0.097 Uiso 1 1 calc R . . C17 C 0.3290(8) 0.052(3) 0.1991(9) 0.165(9) Uani 1 1 d . . . H17A H 0.3679 0.0672 0.1981 0.247 Uiso 1 1 calc R . . H17B H 0.3164 -0.0880 0.1801 0.247 Uiso 1 1 calc R . . H17C H 0.3205 0.0427 0.2361 0.247 Uiso 1 1 calc R . . Au1 Au 0.0000 0.0000 0.0000 0.0575(2) Uani 1 2 d S . . S1 S 0.06464(11) 0.0614(5) 0.07125(11) 0.0733(8) Uani 1 1 d . . . N1 N -0.0071(3) 0.3598(13) 0.1158(3) 0.0593(19) Uani 1 1 d . . . N2 N 0.0774(3) 0.3683(13) 0.1511(3) 0.060(2) Uani 1 1 d . . . O2 O 0.3033(3) 0.246(2) 0.1748(4) 0.124(3) Uani 1 1 d . . . Cl1 Cl -0.008(4) -0.013(11) 0.247(3) 0.19(2) Uani 0.25 1 d P . . Cl1' Cl -0.0102(16) 0.025(10) 0.251(3) 0.076(14) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.051(6) 0.056(5) 0.053(5) -0.001(4) 0.004(4) 0.013(4) C2 0.074(8) 0.092(8) 0.086(8) -0.034(6) 0.000(6) 0.012(6) C3 0.058(6) 0.093(8) 0.092(8) -0.044(6) 0.005(6) 0.011(5) C11 0.046(6) 0.069(6) 0.060(6) -0.004(4) 0.001(4) -0.002(4) C12 0.074(7) 0.089(8) 0.076(7) 0.006(5) 0.007(6) 0.009(6) C13 0.064(7) 0.104(9) 0.099(9) 0.016(6) 0.015(6) 0.007(6) C14 0.045(6) 0.110(9) 0.083(8) -0.007(6) -0.002(5) 0.005(6) C15 0.065(8) 0.081(7) 0.116(10) 0.011(7) -0.011(7) 0.014(6) C16 0.056(7) 0.076(7) 0.111(9) 0.008(6) 0.000(6) -0.001(5) C17 0.085(12) 0.24(2) 0.167(19) 0.068(14) 0.000(12) 0.059(13) Au1 0.0457(3) 0.0692(4) 0.0576(3) -0.0115(2) 0.0056(2) 0.0008(3) S1 0.0484(14) 0.0959(17) 0.0733(16) -0.0308(12) -0.0071(12) 0.0173(12) N1 0.044(5) 0.065(5) 0.067(5) -0.009(3) 0.000(4) 0.008(3) N2 0.044(5) 0.070(5) 0.065(5) -0.017(4) -0.002(4) 0.010(4) O2 0.041(5) 0.189(9) 0.140(8) 0.024(7) 0.000(5) 0.022(6) Cl1 0.40(6) 0.07(2) 0.11(2) -0.02(2) 0.11(3) -0.09(4) Cl1' 0.10(4) 0.045(13) 0.085(12) -0.006(14) 0.01(2) 0.001(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.322(10) . ? C1 N1 1.324(11) . ? C1 S1 1.705(8) . ? C2 N1 1.479(12) . ? C2 C3 1.513(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.467(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C4 N1 1.418(11) . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 O1 1.371(19) . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 O1 1.432(19) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C4' C5' 1.3900 . ? C4' C9' 1.3900 . ? C4' N1 1.433(11) . ? C5' C7' 1.3900 . ? C5' H5' 0.9300 . ? C7' C8' 1.3900 . ? C7' H7' 0.9300 . ? C8' O1' 1.384(17) . ? C8' C6' 1.3900 . ? C6' C9' 1.3900 . ? C6' H6' 0.9300 . ? C9' H9' 0.9300 . ? C10' O1' 1.432(19) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C11 N2 1.421(9) . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 O2 1.357(9) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O2 1.377(16) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? Au1 S1 2.287(3) . ? Au1 S1 2.287(3) 5 ? Cl1 Cl1 0.42(19) 2 ? Cl1 Cl1' 0.50(11) 2 ? Cl1' Cl1 0.50(11) 2 ? Cl1' Cl1' 0.51(7) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 110.3(7) . . ? N2 C1 S1 120.3(7) . . ? N1 C1 S1 129.4(7) . . ? N1 C2 C3 103.0(9) . . ? N1 C2 H2A 111.2 . . ? C3 C2 H2A 111.2 . . ? N1 C2 H2B 111.2 . . ? C3 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? N2 C3 C2 102.9(8) . . ? N2 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? N2 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? C5 C4 C9 120.0 . . ? C5 C4 N1 123.3(10) . . ? C9 C4 N1 116.5(10) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? O1 C7 C6 124.2(10) . . ? O1 C7 C8 115.7(10) . . ? C6 C7 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 O1 C10 118.5(16) . . ? C5' C4' C9' 120.0 . . ? C5' C4' N1 113.5(10) . . ? C9' C4' N1 126.5(10) . . ? C7' C5' C4' 120.0 . . ? C7' C5' H5' 120.0 . . ? C4' C5' H5' 120.0 . . ? C5' C7' C8' 120.0 . . ? C5' C7' H7' 120.0 . . ? C8' C7' H7' 120.0 . . ? O1' C8' C6' 125.8(12) . . ? O1' C8' C7' 114.0(12) . . ? C6' C8' C7' 120.0 . . ? C9' C6' C8' 120.0 . . ? C9' C6' H6' 120.0 . . ? C8' C6' H6' 120.0 . . ? C6' C9' C4' 120.0 . . ? C6' C9' H9' 120.0 . . ? C4' C9' H9' 120.0 . . ? O1' C10' H10D 109.5 . . ? O1' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? O1' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C8' O1' C10' 113.2(17) . . ? C12 C11 C16 120.0 . . ? C12 C11 N2 118.9(6) . . ? C16 C11 N2 121.1(6) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? O2 C14 C13 115.0(7) . . ? O2 C14 C15 125.0(7) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 Au1 S1 180.00(14) . 5 ? C1 S1 Au1 110.3(3) . . ? C1 N1 C4 130.7(11) . . ? C1 N1 C4' 128.2(10) . . ? C1 N1 C2 111.5(8) . . ? C4 N1 C2 116.7(11) . . ? C4' N1 C2 120.0(11) . . ? C1 N2 C11 126.3(7) . . ? C1 N2 C3 112.3(8) . . ? C11 N2 C3 121.3(7) . . ? C14 O2 C17 119.8(12) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.566 _refine_diff_density_min -2.277 _refine_diff_density_rms 0.190 data_yk3 _database_code_depnum_ccdc_archive 'CCDC 773698' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 Ag N4 O4 S2, C F3 O3 S, C H2 Cl2' _chemical_formula_sum 'C36 H38 Ag Cl2 F3 N4 O7 S3' _chemical_formula_weight 970.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0856(19) _cell_length_b 13.665(2) _cell_length_c 14.212(2) _cell_angle_alpha 72.566(3) _cell_angle_beta 83.781(3) _cell_angle_gamma 66.621(3) _cell_volume 2055.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6592 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.790 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 CCD Area Detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19439 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.58 _reflns_number_total 9439 _reflns_number_gt 4396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0420P)^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 9439 _refine_ls_number_parameters 518 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.40530(2) 0.05966(2) 0.40578(2) 0.06134(10) Uani 1 1 d . . . S1 S 0.19653(8) 0.08398(8) 0.42560(7) 0.0554(3) Uani 1 1 d . . . S2 S 0.61120(8) 0.03598(7) 0.36481(7) 0.0504(2) Uani 1 1 d . . . O1 O 0.6303(2) -0.1056(2) 0.1240(2) 0.0813(9) Uani 1 1 d D . . O2 O -0.3300(3) 0.3216(2) 0.5899(2) 0.0983(10) Uani 1 1 d D . . O3 O 0.1482(3) 0.3253(3) 0.5935(3) 0.1274(13) Uani 1 1 d D . . O4 O 1.1255(2) -0.0746(2) 0.1239(2) 0.0912(10) Uani 1 1 d D . . N1 N 0.0191(2) 0.2416(2) 0.3031(2) 0.0545(8) Uani 1 1 d . . . N2 N 0.1854(2) 0.1710(2) 0.2253(2) 0.0522(8) Uani 1 1 d . . . N3 N 0.5209(3) 0.2612(2) 0.3258(2) 0.0581(9) Uani 1 1 d . . . N4 N 0.6892(2) 0.1911(2) 0.2506(2) 0.0530(8) Uani 1 1 d . . . C1 C 0.1326(3) 0.1666(3) 0.3145(3) 0.0477(9) Uani 1 1 d . . . C2 C -0.0113(4) 0.3042(4) 0.2000(3) 0.0754(13) Uani 1 1 d . . . H2A H -0.0301 0.3825 0.1902 0.090 Uiso 1 1 calc R . . H2B H -0.0796 0.2958 0.1784 0.090 Uiso 1 1 calc R . . C3 C 0.1008(3) 0.2536(3) 0.1457(3) 0.0657(12) Uani 1 1 d . . . H3A H 0.0854 0.2183 0.1014 0.079 Uiso 1 1 calc R . . H3B H 0.1317 0.3092 0.1081 0.079 Uiso 1 1 calc R . . C4 C 0.3018(3) 0.1000(3) 0.2032(2) 0.0480(9) Uani 1 1 d . . . C5 C 0.3338(3) -0.0140(3) 0.2269(3) 0.0635(11) Uani 1 1 d . . . H5A H 0.2806 -0.0457 0.2612 0.076 Uiso 1 1 calc R . . C6 C 0.4441(4) -0.0797(3) 0.1996(3) 0.0680(12) Uani 1 1 d . . . H6A H 0.4656 -0.1561 0.2162 0.082 Uiso 1 1 calc R . . C7 C 0.5246(3) -0.0337(3) 0.1474(3) 0.0579(10) Uani 1 1 d D . . C8 C 0.4917(3) 0.0795(3) 0.1239(3) 0.0584(10) Uani 1 1 d . . . H8A H 0.5447 0.1114 0.0895 0.070 Uiso 1 1 calc R . . C9 C 0.3805(3) 0.1461(3) 0.1512(2) 0.0536(10) Uani 1 1 d . . . H9A H 0.3588 0.2226 0.1343 0.064 Uiso 1 1 calc R . . C10 C -0.0666(3) 0.2624(3) 0.3795(3) 0.0512(10) Uani 1 1 d . . . C11 C -0.1162(3) 0.3665(3) 0.3924(3) 0.0749(13) Uani 1 1 d . . . H11A H -0.0910 0.4218 0.3538 0.090 Uiso 1 1 calc R . . C12 C -0.2045(4) 0.3899(3) 0.4634(4) 0.0842(14) Uani 1 1 d . . . H12A H -0.2375 0.4605 0.4724 0.101 Uiso 1 1 calc R . . C13 C -0.2429(3) 0.3081(3) 0.5201(3) 0.0646(11) Uani 1 1 d D . . C14 C -0.1924(3) 0.2039(3) 0.5062(3) 0.0623(11) Uani 1 1 d . . . H14A H -0.2176 0.1483 0.5442 0.075 Uiso 1 1 calc R . . C15 C -0.1050(3) 0.1814(3) 0.4367(3) 0.0566(10) Uani 1 1 d . . . H15A H -0.0714 0.1105 0.4283 0.068 Uiso 1 1 calc R . . C16 C 0.7191(4) -0.0646(4) 0.0752(4) 0.0990(16) Uani 1 1 d D . . H16A H 0.7899 -0.1253 0.0652 0.148 Uiso 1 1 calc R . . H16B H 0.7395 -0.0282 0.1150 0.148 Uiso 1 1 calc R . . H16C H 0.6878 -0.0125 0.0126 0.148 Uiso 1 1 calc R . . C17 C -0.3757(5) 0.4234(4) 0.6168(4) 0.141(2) Uani 1 1 d D . . H17A H -0.4354 0.4212 0.6669 0.212 Uiso 1 1 calc R . . H17B H -0.4115 0.4845 0.5599 0.212 Uiso 1 1 calc R . . H17C H -0.3109 0.4329 0.6415 0.212 Uiso 1 1 calc R . . C18 C 0.6069(3) 0.1661(3) 0.3143(2) 0.0457(9) Uani 1 1 d . . . C19 C 0.6503(4) 0.3119(3) 0.2080(3) 0.0878(16) Uani 1 1 d . . . H19A H 0.6264 0.3339 0.1394 0.105 Uiso 1 1 calc R . . H19B H 0.7143 0.3362 0.2124 0.105 Uiso 1 1 calc R . . C20 C 0.5455(4) 0.3590(3) 0.2692(3) 0.0778(14) Uani 1 1 d . . . H20A H 0.5661 0.3926 0.3124 0.093 Uiso 1 1 calc R . . H20B H 0.4768 0.4141 0.2282 0.093 Uiso 1 1 calc R . . C21 C 0.4262(3) 0.2723(3) 0.3969(3) 0.0514(10) Uani 1 1 d . . . C22 C 0.4507(3) 0.2346(3) 0.4966(3) 0.0631(11) Uani 1 1 d . A . H22A H 0.5302 0.1987 0.5192 0.076 Uiso 1 1 calc R . . C23 C 0.3591(4) 0.2499(3) 0.5622(3) 0.0746(13) Uani 1 1 d . . . H23A H 0.3762 0.2219 0.6295 0.090 Uiso 1 1 calc R A . C24 C 0.2407(4) 0.3066(3) 0.5297(3) 0.0700(12) Uani 1 1 d D A . C25 C 0.2166(4) 0.3453(3) 0.4309(3) 0.0765(13) Uani 1 1 d . . . H25A H 0.1371 0.3837 0.4085 0.092 Uiso 1 1 calc R A . C26 C 0.3081(3) 0.3284(3) 0.3639(3) 0.0656(12) Uani 1 1 d . A . H26A H 0.2907 0.3546 0.2967 0.079 Uiso 1 1 calc R . . C27 C 0.7988(3) 0.1179(3) 0.2206(3) 0.0498(9) Uani 1 1 d . . . C28 C 0.8358(3) 0.1462(3) 0.1230(3) 0.0605(11) Uani 1 1 d . . . H28A H 0.7871 0.2104 0.0776 0.073 Uiso 1 1 calc R . . C29 C 0.9431(4) 0.0797(3) 0.0946(3) 0.0683(12) Uani 1 1 d . . . H29A H 0.9667 0.0988 0.0294 0.082 Uiso 1 1 calc R . . C30 C 1.0181(3) -0.0158(3) 0.1601(3) 0.0635(11) Uani 1 1 d D . . C31 C 0.9823(3) -0.0444(3) 0.2566(3) 0.0632(11) Uani 1 1 d . . . H31A H 1.0316 -0.1087 0.3015 0.076 Uiso 1 1 calc R . . C32 C 0.8727(3) 0.0226(3) 0.2866(3) 0.0589(10) Uani 1 1 d . . . H32A H 0.8490 0.0031 0.3517 0.071 Uiso 1 1 calc R . . C33 C 0.1513(8) 0.2582(7) 0.6834(6) 0.125(4) Uani 0.581(6) 1 d PD A 1 H33A H 0.0761 0.2872 0.7155 0.187 Uiso 0.581(6) 1 calc PR A 1 H33B H 0.2159 0.2531 0.7208 0.187 Uiso 0.581(6) 1 calc PR A 1 H33C H 0.1640 0.1857 0.6792 0.187 Uiso 0.581(6) 1 calc PR A 1 C33' C 0.0316(7) 0.3410(12) 0.5905(10) 0.129(5) Uani 0.419(6) 1 d PD A 2 H33D H -0.0054 0.3512 0.6520 0.194 Uiso 0.419(6) 1 calc PR A 2 H33E H 0.0254 0.2773 0.5797 0.194 Uiso 0.419(6) 1 calc PR A 2 H33F H -0.0088 0.4057 0.5378 0.194 Uiso 0.419(6) 1 calc PR A 2 C34 C 1.1924(4) -0.1845(3) 0.1804(4) 0.1025(17) Uani 1 1 d D . . H34A H 1.2594 -0.2192 0.1426 0.154 Uiso 1 1 calc R . . H34B H 1.1416 -0.2260 0.1970 0.154 Uiso 1 1 calc R . . H34C H 1.2217 -0.1826 0.2397 0.154 Uiso 1 1 calc R . . S3 S 0.21350(10) 0.53840(8) 0.08367(9) 0.0700(3) Uani 1 1 d . . . O5 O 0.2472(3) 0.4220(2) 0.1137(2) 0.0872(10) Uani 1 1 d . . . O6 O 0.2043(3) 0.5863(3) -0.0197(2) 0.1370(16) Uani 1 1 d . . . O7 O 0.2698(3) 0.5749(3) 0.1392(4) 0.1601(18) Uani 1 1 d . . . C35 C 0.0607(4) 0.5912(4) 0.1218(3) 0.0785(14) Uani 1 1 d . . . F1 F -0.0106(3) 0.5665(2) 0.0752(2) 0.1245(11) Uani 1 1 d . . . F2 F 0.0459(3) 0.5486(3) 0.2153(2) 0.1390(13) Uani 1 1 d . . . F3 F 0.0131(2) 0.7008(2) 0.1017(2) 0.1164(10) Uani 1 1 d . . . C36 C 1.3563(4) -0.6480(4) -0.0970(3) 0.0882(15) Uani 1 1 d . . . H36A H 1.3621 -0.7242 -0.0782 0.106 Uiso 1 1 calc R . . H36B H 1.2952 -0.6084 -0.0568 0.106 Uiso 1 1 calc R . . Cl1 Cl 1.49442(12) -0.64557(13) -0.07649(12) 0.1194(5) Uani 1 1 d . . . Cl2 Cl 1.31540(15) -0.58645(13) -0.22035(11) 0.1301(6) 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 0.05366(17) 0.05936(18) 0.0700(2) -0.01502(15) -0.00336(14) -0.02199(14) S1 0.0531(5) 0.0551(6) 0.0462(5) 0.0006(4) -0.0027(4) -0.0187(5) S2 0.0515(5) 0.0418(5) 0.0510(5) -0.0045(4) -0.0021(4) -0.0165(4) O1 0.0705(18) 0.0628(16) 0.106(2) -0.0410(16) 0.0083(16) -0.0097(15) O2 0.098(2) 0.099(2) 0.109(2) -0.0600(18) 0.0441(18) -0.0380(18) O3 0.122(3) 0.125(3) 0.147(3) -0.075(2) 0.073(2) -0.049(2) O4 0.0682(19) 0.099(2) 0.104(2) -0.0576(18) 0.0221(16) -0.0141(17) N1 0.0476(17) 0.0483(17) 0.0516(18) 0.0005(14) -0.0028(15) -0.0119(14) N2 0.0506(17) 0.0477(16) 0.0448(17) -0.0016(14) -0.0099(14) -0.0107(14) N3 0.0540(18) 0.0403(16) 0.069(2) -0.0094(15) 0.0156(16) -0.0151(15) N4 0.0523(17) 0.0379(16) 0.0605(19) -0.0077(14) 0.0103(15) -0.0156(14) C1 0.052(2) 0.0451(19) 0.046(2) -0.0055(16) -0.0053(17) -0.0236(17) C2 0.065(3) 0.078(3) 0.063(3) -0.006(2) -0.008(2) -0.016(2) C3 0.062(2) 0.078(3) 0.051(2) -0.005(2) -0.008(2) -0.029(2) C4 0.051(2) 0.045(2) 0.042(2) -0.0083(16) -0.0040(17) -0.0141(17) C5 0.076(2) 0.058(2) 0.066(3) -0.021(2) 0.007(2) -0.035(2) C6 0.084(3) 0.039(2) 0.083(3) -0.022(2) 0.000(2) -0.021(2) C7 0.064(2) 0.050(2) 0.058(2) -0.0241(19) -0.008(2) -0.012(2) C8 0.060(2) 0.062(2) 0.052(2) -0.0174(19) 0.0028(19) -0.022(2) C9 0.066(2) 0.0366(19) 0.050(2) -0.0061(17) 0.0008(19) -0.0147(18) C10 0.0430(19) 0.045(2) 0.059(2) -0.0098(18) -0.0006(18) -0.0129(17) C11 0.070(3) 0.051(2) 0.099(3) -0.014(2) 0.010(2) -0.026(2) C12 0.080(3) 0.050(2) 0.120(4) -0.036(3) 0.012(3) -0.017(2) C13 0.057(2) 0.065(2) 0.075(3) -0.034(2) 0.008(2) -0.019(2) C14 0.063(2) 0.061(2) 0.070(3) -0.022(2) 0.016(2) -0.032(2) C15 0.059(2) 0.053(2) 0.065(2) -0.0219(19) 0.0018(19) -0.0258(19) C16 0.070(3) 0.096(3) 0.135(4) -0.056(3) 0.025(3) -0.025(3) C17 0.152(5) 0.109(4) 0.154(5) -0.079(4) 0.061(4) -0.026(4) C18 0.0471(19) 0.0454(19) 0.0402(19) -0.0082(16) -0.0034(16) -0.0151(17) C19 0.086(3) 0.046(2) 0.110(4) -0.012(2) 0.044(3) -0.021(2) C20 0.080(3) 0.044(2) 0.097(3) -0.010(2) 0.024(3) -0.024(2) C21 0.050(2) 0.0427(19) 0.058(2) -0.0127(18) 0.0049(18) -0.0169(17) C22 0.055(2) 0.059(2) 0.063(3) -0.011(2) -0.003(2) -0.013(2) C23 0.090(3) 0.070(3) 0.054(2) -0.019(2) 0.006(2) -0.020(2) C24 0.066(3) 0.069(3) 0.081(3) -0.038(2) 0.027(2) -0.027(2) C25 0.050(2) 0.082(3) 0.093(3) -0.035(3) -0.001(2) -0.013(2) C26 0.061(2) 0.070(3) 0.060(3) -0.021(2) 0.001(2) -0.018(2) C27 0.054(2) 0.0427(19) 0.054(2) -0.0169(17) 0.0057(18) -0.0179(17) C28 0.065(2) 0.052(2) 0.060(2) -0.0156(19) 0.006(2) -0.019(2) C29 0.077(3) 0.066(2) 0.070(3) -0.035(2) 0.018(2) -0.028(2) C30 0.054(2) 0.071(2) 0.083(3) -0.047(2) 0.010(2) -0.025(2) C31 0.051(2) 0.058(2) 0.077(3) -0.022(2) -0.004(2) -0.0145(19) C32 0.058(2) 0.066(2) 0.057(2) -0.020(2) 0.0040(19) -0.027(2) C33 0.137(8) 0.102(6) 0.144(8) -0.056(6) 0.084(6) -0.061(6) C33' 0.094(9) 0.202(14) 0.123(11) -0.087(10) 0.043(8) -0.070(9) C34 0.074(3) 0.079(3) 0.164(5) -0.067(3) 0.017(3) -0.018(3) S3 0.0740(7) 0.0446(6) 0.0839(8) -0.0156(5) 0.0027(6) -0.0173(5) O5 0.117(2) 0.0408(15) 0.0799(19) -0.0150(14) 0.0121(17) -0.0100(16) O6 0.145(3) 0.097(3) 0.086(2) 0.023(2) 0.047(2) -0.009(2) O7 0.088(2) 0.113(3) 0.312(5) -0.112(3) -0.042(3) -0.022(2) C35 0.089(3) 0.071(3) 0.057(3) -0.013(2) -0.007(2) -0.014(3) F1 0.107(2) 0.123(2) 0.148(3) -0.021(2) -0.028(2) -0.0531(18) F2 0.128(2) 0.152(3) 0.079(2) -0.0199(19) 0.0274(18) -0.011(2) F3 0.096(2) 0.0667(17) 0.156(3) -0.0344(17) -0.0078(18) 0.0048(15) C36 0.096(3) 0.082(3) 0.082(3) -0.028(3) 0.024(3) -0.031(3) Cl1 0.0897(9) 0.1207(11) 0.1397(12) -0.0325(10) 0.0024(9) -0.0353(8) Cl2 0.1439(13) 0.1229(12) 0.1026(11) -0.0100(9) -0.0155(10) -0.0414(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S1 2.4067(11) . ? Ag1 S2 2.4075(10) . ? Ag1 Ag1 3.2894(7) 2_656 ? S1 C1 1.694(3) . ? S2 C18 1.688(3) . ? O1 C7 1.347(4) . ? O1 C16 1.426(5) . ? O2 C13 1.361(4) . ? O2 C17 1.431(5) . ? O3 C33 1.326(7) . ? O3 C33' 1.342(7) . ? O3 C24 1.353(4) . ? O4 C30 1.368(4) . ? O4 C34 1.416(4) . ? N1 C1 1.338(4) . ? N1 C10 1.428(4) . ? N1 C2 1.459(4) . ? N2 C1 1.352(4) . ? N2 C4 1.422(4) . ? N2 C3 1.473(4) . ? N3 C18 1.346(4) . ? N3 C21 1.434(4) . ? N3 C20 1.463(5) . ? N4 C18 1.347(4) . ? N4 C27 1.420(4) . ? N4 C19 1.469(4) . ? C2 C3 1.503(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.376(5) . ? C4 C5 1.388(5) . ? C5 C6 1.372(5) . ? C5 H5A 0.9300 . ? C6 C7 1.393(5) . ? C6 H6A 0.9300 . ? C7 C8 1.376(5) . ? C8 C9 1.383(5) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.369(5) . ? C10 C15 1.375(5) . ? C11 C12 1.395(6) . ? C11 H11A 0.9300 . ? C12 C13 1.381(6) . ? C12 H12A 0.9300 . ? C13 C14 1.375(5) . ? C14 C15 1.372(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 C20 1.492(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.377(5) . ? C21 C26 1.380(5) . ? C22 C23 1.359(5) . ? C22 H22A 0.9300 . ? C23 C24 1.382(5) . ? C23 H23A 0.9300 . ? C24 C25 1.364(6) . ? C25 C26 1.373(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C32 1.379(5) . ? C27 C28 1.399(5) . ? C28 C29 1.357(5) . ? C28 H28A 0.9300 . ? C29 C30 1.381(5) . ? C29 H29A 0.9300 . ? C30 C31 1.380(5) . ? C31 C32 1.387(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C33' H33D 0.9600 . ? C33' H33E 0.9600 . ? C33' H33F 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? S3 O7 1.398(4) . ? S3 O5 1.413(3) . ? S3 O6 1.415(3) . ? S3 C35 1.785(5) . ? C35 F2 1.305(5) . ? C35 F3 1.324(5) . ? C35 F1 1.335(5) . ? C36 Cl2 1.732(4) . ? C36 Cl1 1.740(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? 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 S1 Ag1 S2 172.77(4) . . ? S1 Ag1 Ag1 121.72(3) . 2_656 ? S2 Ag1 Ag1 64.87(2) . 2_656 ? C1 S1 Ag1 104.11(12) . . ? C18 S2 Ag1 104.88(12) . . ? C7 O1 C16 118.9(3) . . ? C13 O2 C17 118.5(4) . . ? C33 O3 C33' 86.4(7) . . ? C33 O3 C24 123.5(5) . . ? C33' O3 C24 134.7(7) . . ? C30 O4 C34 118.3(3) . . ? C1 N1 C10 126.5(3) . . ? C1 N1 C2 112.1(3) . . ? C10 N1 C2 121.4(3) . . ? C1 N2 C4 127.7(3) . . ? C1 N2 C3 111.3(3) . . ? C4 N2 C3 120.7(3) . . ? C18 N3 C21 127.1(3) . . ? C18 N3 C20 112.3(3) . . ? C21 N3 C20 119.6(3) . . ? C18 N4 C27 128.8(3) . . ? C18 N4 C19 110.8(3) . . ? C27 N4 C19 120.4(3) . . ? N1 C1 N2 109.3(3) . . ? N1 C1 S1 123.5(3) . . ? N2 C1 S1 127.2(3) . . ? N1 C2 C3 103.8(3) . . ? N1 C2 H2A 111.0 . . ? C3 C2 H2A 111.0 . . ? N1 C2 H2B 111.0 . . ? C3 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N2 C3 C2 103.4(3) . . ? N2 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? N2 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? C9 C4 C5 119.6(3) . . ? C9 C4 N2 119.2(3) . . ? C5 C4 N2 121.0(3) . . ? C6 C5 C4 119.7(4) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? O1 C7 C8 125.1(4) . . ? O1 C7 C6 116.2(3) . . ? C8 C7 C6 118.7(3) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C4 C9 C8 120.5(3) . . ? C4 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C15 119.3(3) . . ? C11 C10 N1 119.4(3) . . ? C15 C10 N1 121.2(3) . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? O2 C13 C14 115.6(4) . . ? O2 C13 C12 125.2(4) . . ? C14 C13 C12 119.2(4) . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C10 120.8(4) . . ? C14 C15 H15A 119.6 . . ? C10 C15 H15A 119.6 . . ? O1 C16 H16A 109.5 . . ? O1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 N4 108.7(3) . . ? N3 C18 S2 127.2(3) . . ? N4 C18 S2 124.0(3) . . ? N4 C19 C20 104.1(3) . . ? N4 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? N4 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 109.0 . . ? N3 C20 C19 102.6(3) . . ? N3 C20 H20A 111.2 . . ? C19 C20 H20A 111.2 . . ? N3 C20 H20B 111.2 . . ? C19 C20 H20B 111.2 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C26 119.5(3) . . ? C22 C21 N3 121.5(3) . . ? C26 C21 N3 118.8(3) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? O3 C24 C25 119.1(4) . . ? O3 C24 C23 121.7(4) . . ? C25 C24 C23 119.2(4) . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C21 119.7(4) . . ? C25 C26 H26A 120.2 . . ? C21 C26 H26A 120.2 . . ? C32 C27 C28 119.1(3) . . ? C32 C27 N4 121.6(3) . . ? C28 C27 N4 119.2(3) . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 121.6(4) . . ? C28 C29 H29A 119.2 . . ? C30 C29 H29A 119.2 . . ? O4 C30 C31 124.5(4) . . ? O4 C30 C29 116.5(4) . . ? C31 C30 C29 119.0(3) . . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C27 C32 C31 120.4(4) . . ? C27 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? O3 C33 H33A 109.5 . . ? O3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 C33' H33D 109.5 . . ? O3 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? O3 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O7 S3 O5 113.1(2) . . ? O7 S3 O6 118.3(3) . . ? O5 S3 O6 114.3(2) . . ? O7 S3 C35 101.7(2) . . ? O5 S3 C35 104.1(2) . . ? O6 S3 C35 102.6(2) . . ? F2 C35 F3 108.7(4) . . ? F2 C35 F1 104.5(4) . . ? F3 C35 F1 105.0(4) . . ? F2 C35 S3 113.3(3) . . ? F3 C35 S3 113.2(4) . . ? F1 C35 S3 111.5(3) . . ? Cl2 C36 Cl1 110.1(3) . . ? Cl2 C36 H36A 109.6 . . ? Cl1 C36 H36A 109.6 . . ? Cl2 C36 H36B 109.6 . . ? Cl1 C36 H36B 109.6 . . ? H36A C36 H36B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 Ag1 S1 C1 170.79(13) 2_656 . . . ? Ag1 Ag1 S2 C18 -118.46(13) 2_656 . . . ? C10 N1 C1 N2 179.6(3) . . . . ? C2 N1 C1 N2 -0.5(4) . . . . ? C10 N1 C1 S1 -2.0(5) . . . . ? C2 N1 C1 S1 177.9(3) . . . . ? C4 N2 C1 N1 -174.7(3) . . . . ? C3 N2 C1 N1 -1.6(4) . . . . ? C4 N2 C1 S1 7.1(5) . . . . ? C3 N2 C1 S1 -179.9(3) . . . . ? Ag1 S1 C1 N1 -147.2(3) . . . . ? Ag1 S1 C1 N2 30.9(3) . . . . ? C1 N1 C2 C3 2.2(4) . . . . ? C10 N1 C2 C3 -177.9(3) . . . . ? C1 N2 C3 C2 2.9(4) . . . . ? C4 N2 C3 C2 176.5(3) . . . . ? N1 C2 C3 N2 -2.9(4) . . . . ? C1 N2 C4 C9 -127.1(4) . . . . ? C3 N2 C4 C9 60.4(5) . . . . ? C1 N2 C4 C5 57.6(5) . . . . ? C3 N2 C4 C5 -114.9(4) . . . . ? C9 C4 C5 C6 0.9(6) . . . . ? N2 C4 C5 C6 176.3(3) . . . . ? C4 C5 C6 C7 -0.6(6) . . . . ? C16 O1 C7 C8 3.1(6) . . . . ? C16 O1 C7 C6 -176.7(4) . . . . ? C5 C6 C7 O1 -179.8(4) . . . . ? C5 C6 C7 C8 0.4(6) . . . . ? O1 C7 C8 C9 179.8(3) . . . . ? C6 C7 C8 C9 -0.4(6) . . . . ? C5 C4 C9 C8 -1.0(5) . . . . ? N2 C4 C9 C8 -176.4(3) . . . . ? C7 C8 C9 C4 0.8(6) . . . . ? C1 N1 C10 C11 121.4(4) . . . . ? C2 N1 C10 C11 -58.4(5) . . . . ? C1 N1 C10 C15 -62.1(5) . . . . ? C2 N1 C10 C15 118.0(4) . . . . ? C15 C10 C11 C12 0.3(6) . . . . ? N1 C10 C11 C12 176.8(4) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C17 O2 C13 C14 172.4(4) . . . . ? C17 O2 C13 C12 -8.5(6) . . . . ? C11 C12 C13 O2 -178.5(4) . . . . ? C11 C12 C13 C14 0.5(7) . . . . ? O2 C13 C14 C15 179.1(3) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C13 C14 C15 C10 -0.2(6) . . . . ? C11 C10 C15 C14 0.1(6) . . . . ? N1 C10 C15 C14 -176.3(3) . . . . ? C21 N3 C18 N4 -170.5(3) . . . . ? C20 N3 C18 N4 -1.8(4) . . . . ? C21 N3 C18 S2 12.5(6) . . . . ? C20 N3 C18 S2 -178.8(3) . . . . ? C27 N4 C18 N3 175.9(3) . . . . ? C19 N4 C18 N3 -6.2(4) . . . . ? C27 N4 C18 S2 -6.9(5) . . . . ? C19 N4 C18 S2 170.9(3) . . . . ? Ag1 S2 C18 N3 21.5(3) . . . . ? Ag1 S2 C18 N4 -155.1(3) . . . . ? C18 N4 C19 C20 11.3(5) . . . . ? C27 N4 C19 C20 -170.6(3) . . . . ? C18 N3 C20 C19 8.6(5) . . . . ? C21 N3 C20 C19 178.2(4) . . . . ? N4 C19 C20 N3 -11.3(5) . . . . ? C18 N3 C21 C22 62.0(5) . . . . ? C20 N3 C21 C22 -105.9(4) . . . . ? C18 N3 C21 C26 -122.2(4) . . . . ? C20 N3 C21 C26 69.8(5) . . . . ? C26 C21 C22 C23 1.9(6) . . . . ? N3 C21 C22 C23 177.6(4) . . . . ? C21 C22 C23 C24 -2.3(6) . . . . ? C33 O3 C24 C25 150.9(7) . . . . ? C33' O3 C24 C25 27.5(12) . . . . ? C33 O3 C24 C23 -29.6(9) . . . . ? C33' O3 C24 C23 -153.0(10) . . . . ? C22 C23 C24 O3 -178.3(4) . . . . ? C22 C23 C24 C25 1.3(7) . . . . ? O3 C24 C25 C26 179.7(4) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C24 C25 C26 C21 -0.5(7) . . . . ? C22 C21 C26 C25 -0.5(6) . . . . ? N3 C21 C26 C25 -176.3(4) . . . . ? C18 N4 C27 C32 -39.9(6) . . . . ? C19 N4 C27 C32 142.4(4) . . . . ? C18 N4 C27 C28 143.5(4) . . . . ? C19 N4 C27 C28 -34.2(5) . . . . ? C32 C27 C28 C29 0.2(6) . . . . ? N4 C27 C28 C29 176.9(4) . . . . ? C27 C28 C29 C30 -0.5(6) . . . . ? C34 O4 C30 C31 15.6(6) . . . . ? C34 O4 C30 C29 -165.8(4) . . . . ? C28 C29 C30 O4 -178.2(4) . . . . ? C28 C29 C30 C31 0.5(6) . . . . ? O4 C30 C31 C32 178.2(4) . . . . ? C29 C30 C31 C32 -0.3(6) . . . . ? C28 C27 C32 C31 -0.1(6) . . . . ? N4 C27 C32 C31 -176.6(3) . . . . ? C30 C31 C32 C27 0.1(6) . . . . ? O7 S3 C35 F2 -63.4(4) . . . . ? O5 S3 C35 F2 54.3(4) . . . . ? O6 S3 C35 F2 173.7(4) . . . . ? O7 S3 C35 F3 60.9(4) . . . . ? O5 S3 C35 F3 178.6(3) . . . . ? O6 S3 C35 F3 -62.0(4) . . . . ? O7 S3 C35 F1 179.0(3) . . . . ? O5 S3 C35 F1 -63.3(3) . . . . ? O6 S3 C35 F1 56.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.559 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.070