# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Pablo Espinet' _publ_contact_author_address ; IU CINQUIMA/Quimica Inorganica, Facultad de Ciencias, Universidad de Valladolid. E-47071 Valladolid, Spain ; _publ_contact_author_email espinet@qi.uva.es _publ_contact_author_phone '+34 983 423231' _publ_contact_author_fax '+34 983 423013' _publ_section_title ; Photosensitive Azobispyridine Gold(I) and Silver (I) Complexes ; _publ_contact_letter ; please consider this cif submission for publication in Dalton Trans. amc51 is compound 8 in the MS abpypac is compound 9 in the MS mba25bm is compound 11 in the MS ; loop_ _publ_author_name _publ_author_address M.Bardaji ; IU CINQUIMA/Quimica Inorganica, Facultad de Ciencias, Universidad de Valladolid. E-47071 Valladolid, Spain ; M.Barrio ; IU CINQUIMA/Quimica Inorganica, Facultad de Ciencias, Universidad de Valladolid. E-47071 Valladolid, Spain ; P.Espinet ; IU CINQUIMA/Quimica Inorganica, Facultad de Ciencias, Universidad de Valladolid. E-47071 Valladolid, Spain ; ######################################################################### data_amc51 _database_code_depnum_ccdc_archive 'CCDC 792813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Au2 F6 N4 O6 P2 S2' _chemical_formula_weight 1400.82 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2095(5) _cell_length_b 9.6233(4) _cell_length_c 15.0245(6) _cell_angle_alpha 106.432(4) _cell_angle_beta 96.593(4) _cell_angle_gamma 100.039(4) _cell_volume 1238.48(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4682 _cell_measurement_theta_min 3.0389 _cell_measurement_theta_max 28.7523 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.1762 _exptl_crystal_size_mid 0.1097 _exptl_crystal_size_min 0.0389 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 6.140 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details ; 'Thu Jan 21 09:15:57 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4757 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8327 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.82 _reflns_number_total 5119 _reflns_number_gt 3894 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; 'Thu Jan 21 09:15:57 2010' ; _computing_cell_refinement ; 'Thu Jan 21 09:15:57 2010' ; _computing_data_reduction ; 'Thu Jan 21 09:15:57 2010' ; _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^)+(0.0440P)^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 5119 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 Au1 Au 0.90928(3) 0.19718(3) 0.844629(15) 0.04174(10) Uani 1 1 d . . . P1 P 0.74037(18) 0.11152(17) 0.71246(10) 0.0403(4) Uani 1 1 d . . . N1 N 1.0734(5) 0.2749(5) 0.9653(3) 0.0391(11) Uani 1 1 d . . . C1 C 1.1626(8) 0.4099(7) 0.9919(5) 0.0532(17) Uani 1 1 d . . . H1 H 1.1484 0.4739 0.9571 0.064 Uiso 1 1 calc R . . C2 C 1.2743(8) 0.4566(8) 1.0687(5) 0.063(2) Uani 1 1 d . . . H2 H 1.3331 0.5522 1.0868 0.075 Uiso 1 1 calc R . . C3 C 1.2989(8) 0.3628(9) 1.1185(5) 0.065(2) Uani 1 1 d . . . H3 H 1.3762 0.3921 1.1700 0.078 Uiso 1 1 calc R . . C4 C 1.2077(8) 0.2238(8) 1.0914(4) 0.0581(19) Uani 1 1 d . . . H4 H 1.2211 0.1582 1.1251 0.070 Uiso 1 1 calc R . . C5 C 1.0976(7) 0.1833(7) 1.0148(4) 0.0412(14) Uani 1 1 d . . . N2 N 0.9930(6) 0.0440(5) 0.9773(3) 0.0435(12) Uani 1 1 d . . . C11 C 0.5687(7) 0.1753(7) 0.7258(4) 0.0440(15) Uani 1 1 d . . . C12 C 0.5063(8) 0.2429(8) 0.6658(5) 0.0599(18) Uani 1 1 d . . . H12 H 0.5509 0.2541 0.6151 0.072 Uiso 1 1 calc R . . C13 C 0.3763(10) 0.2944(10) 0.6816(7) 0.083(3) Uani 1 1 d . . . H13 H 0.3357 0.3428 0.6426 0.099 Uiso 1 1 calc R . . C14 C 0.3092(10) 0.2738(10) 0.7539(7) 0.087(3) Uani 1 1 d . . . H14 H 0.2216 0.3068 0.7639 0.105 Uiso 1 1 calc R . . C15 C 0.3698(10) 0.2045(10) 0.8123(6) 0.083(2) Uani 1 1 d . . . H15 H 0.3220 0.1890 0.8611 0.100 Uiso 1 1 calc R . . C16 C 0.4996(9) 0.1581(9) 0.7996(5) 0.065(2) Uani 1 1 d . . . H16 H 0.5418 0.1145 0.8411 0.078 Uiso 1 1 calc R . . C21 C 0.8107(7) 0.1620(7) 0.6164(4) 0.0438(15) Uani 1 1 d . . . C22 C 0.9042(8) 0.2996(8) 0.6346(5) 0.0563(18) Uani 1 1 d . . . H22 H 0.9331 0.3637 0.6959 0.068 Uiso 1 1 calc R . . C23 C 0.9542(10) 0.3409(9) 0.5602(6) 0.075(2) Uani 1 1 d . . . H23 H 1.0151 0.4342 0.5718 0.090 Uiso 1 1 calc R . . C24 C 0.9159(10) 0.2478(10) 0.4717(6) 0.078(2) Uani 1 1 d . . . H24 H 0.9513 0.2767 0.4227 0.094 Uiso 1 1 calc R . . C25 C 0.8255(10) 0.1113(10) 0.4534(5) 0.075(2) Uani 1 1 d . . . H25 H 0.7998 0.0470 0.3920 0.090 Uiso 1 1 calc R . . C26 C 0.7719(8) 0.0684(8) 0.5257(4) 0.0613(19) Uani 1 1 d . . . H26 H 0.7093 -0.0244 0.5129 0.074 Uiso 1 1 calc R . . C31 C 0.6878(7) -0.0892(7) 0.6748(4) 0.0450(15) Uani 1 1 d . . . C32 C 0.7990(9) -0.1678(8) 0.6819(5) 0.0646(19) Uani 1 1 d . . . H32 H 0.8975 -0.1170 0.7064 0.077 Uiso 1 1 calc R . . C33 C 0.7645(12) -0.3203(10) 0.6531(6) 0.088(3) Uani 1 1 d . . . H33 H 0.8389 -0.3735 0.6570 0.106 Uiso 1 1 calc R . . C34 C 0.6189(14) -0.3920(9) 0.6187(6) 0.091(3) Uani 1 1 d . . . H34 H 0.5940 -0.4951 0.6001 0.109 Uiso 1 1 calc R . . C35 C 0.5087(12) -0.3158(10) 0.6111(7) 0.097(3) Uani 1 1 d . . . H35 H 0.4106 -0.3669 0.5854 0.116 Uiso 1 1 calc R . . C36 C 0.5427(9) -0.1653(8) 0.6410(6) 0.072(2) Uani 1 1 d . . . H36 H 0.4669 -0.1134 0.6385 0.086 Uiso 1 1 calc R . . S1 S 0.1714(2) 0.6913(2) 0.80700(14) 0.0711(6) Uani 1 1 d . . . O1 O 0.0748(7) 0.6060(8) 0.8476(4) 0.099(2) Uani 1 1 d . . . O2 O 0.1204(10) 0.8207(11) 0.7984(7) 0.155(4) Uani 1 1 d . . . O3 O 0.2230(10) 0.6152(10) 0.7287(5) 0.158(4) Uani 1 1 d . . . C41 C 0.3294(12) 0.7802(14) 0.8980(8) 0.102(3) Uani 1 1 d . . . F1 F 0.3849(8) 0.6676(12) 0.9199(7) 0.197(4) Uani 1 1 d . . . F2 F 0.2994(9) 0.8595(12) 0.9705(5) 0.205(5) Uani 1 1 d . . . F3 F 0.4399(7) 0.8508(7) 0.8686(5) 0.132(2) 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 Au1 0.04604(16) 0.04091(15) 0.04044(14) 0.01775(10) 0.00485(10) 0.00823(10) P1 0.0467(10) 0.0352(9) 0.0404(8) 0.0146(7) 0.0070(7) 0.0080(7) N1 0.046(3) 0.043(3) 0.030(2) 0.014(2) 0.008(2) 0.007(2) C1 0.059(4) 0.041(4) 0.061(4) 0.019(3) 0.017(4) 0.003(3) C2 0.070(5) 0.041(4) 0.066(4) 0.016(3) 0.005(4) -0.009(4) C3 0.061(5) 0.068(5) 0.055(4) 0.020(4) -0.008(4) -0.007(4) C4 0.066(5) 0.058(4) 0.052(4) 0.029(3) -0.004(3) 0.007(4) C5 0.050(4) 0.040(3) 0.035(3) 0.015(3) 0.006(3) 0.011(3) N2 0.048(3) 0.043(3) 0.047(3) 0.024(2) 0.008(2) 0.013(3) C11 0.044(4) 0.037(3) 0.048(3) 0.011(3) 0.005(3) 0.006(3) C12 0.056(5) 0.063(5) 0.071(4) 0.031(4) 0.016(4) 0.017(4) C13 0.062(5) 0.087(6) 0.119(7) 0.051(6) 0.017(5) 0.035(5) C14 0.061(6) 0.079(6) 0.128(8) 0.023(6) 0.034(6) 0.034(5) C15 0.077(6) 0.097(7) 0.083(5) 0.025(5) 0.040(5) 0.029(5) C16 0.063(5) 0.078(5) 0.061(4) 0.022(4) 0.024(4) 0.025(4) C21 0.046(4) 0.048(4) 0.047(3) 0.028(3) 0.011(3) 0.014(3) C22 0.068(5) 0.047(4) 0.063(4) 0.028(3) 0.021(4) 0.013(4) C23 0.098(6) 0.058(5) 0.092(6) 0.051(5) 0.039(5) 0.019(4) C24 0.102(7) 0.088(6) 0.066(5) 0.046(5) 0.040(5) 0.025(5) C25 0.094(6) 0.090(6) 0.046(4) 0.026(4) 0.017(4) 0.019(5) C26 0.069(5) 0.063(5) 0.050(4) 0.020(3) 0.015(4) 0.004(4) C31 0.053(4) 0.042(4) 0.043(3) 0.016(3) 0.011(3) 0.009(3) C32 0.062(5) 0.052(5) 0.083(5) 0.020(4) 0.021(4) 0.018(4) C33 0.114(8) 0.052(5) 0.103(7) 0.017(5) 0.033(6) 0.036(5) C34 0.138(9) 0.029(4) 0.101(7) 0.017(4) 0.039(6) 0.000(6) C35 0.093(7) 0.044(5) 0.133(8) 0.006(5) 0.024(6) -0.003(5) C36 0.062(5) 0.044(4) 0.094(6) 0.002(4) 0.013(4) 0.003(4) S1 0.0743(14) 0.0761(14) 0.0663(12) 0.0278(11) 0.0182(10) 0.0119(11) O1 0.078(4) 0.127(6) 0.110(5) 0.071(4) 0.029(4) 0.005(4) O2 0.138(7) 0.162(8) 0.222(9) 0.128(7) 0.017(6) 0.074(6) O3 0.170(8) 0.150(8) 0.120(6) -0.008(5) 0.084(6) -0.006(6) C41 0.073(7) 0.130(9) 0.119(8) 0.054(8) 0.034(6) 0.023(7) F1 0.104(5) 0.288(11) 0.278(10) 0.213(10) 0.016(6) 0.052(6) F2 0.126(6) 0.281(12) 0.114(5) -0.062(6) 0.010(5) 0.013(7) F3 0.082(4) 0.125(5) 0.193(7) 0.080(5) 0.016(4) -0.013(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 Au1 N1 2.083(4) . ? Au1 P1 2.2272(15) . ? P1 C21 1.800(6) . ? P1 C11 1.805(7) . ? P1 C31 1.810(6) . ? N1 C5 1.334(7) . ? N1 C1 1.335(8) . ? C1 C2 1.366(9) . ? C2 C3 1.357(10) . ? C3 C4 1.371(9) . ? C4 C5 1.359(8) . ? C5 N2 1.429(8) . ? N2 N2 1.242(9) 2_757 ? C11 C16 1.375(9) . ? C11 C12 1.382(9) . ? C12 C13 1.392(11) . ? C13 C14 1.355(12) . ? C14 C15 1.370(12) . ? C15 C16 1.362(11) . ? C21 C26 1.370(9) . ? C21 C22 1.383(9) . ? C22 C23 1.387(9) . ? C23 C24 1.343(11) . ? C24 C25 1.363(11) . ? C25 C26 1.379(9) . ? C31 C36 1.368(9) . ? C31 C32 1.387(10) . ? C32 C33 1.374(11) . ? C33 C34 1.363(13) . ? C34 C35 1.364(13) . ? C35 C36 1.356(11) . ? S1 O3 1.381(7) . ? S1 O1 1.410(6) . ? S1 O2 1.438(8) . ? S1 C41 1.780(11) . ? C41 F2 1.231(12) . ? C41 F3 1.314(11) . ? C41 F1 1.378(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Au1 P1 177.85(14) . . ? C21 P1 C11 108.0(3) . . ? C21 P1 C31 106.5(3) . . ? C11 P1 C31 105.9(3) . . ? C21 P1 Au1 112.1(2) . . ? C11 P1 Au1 112.85(19) . . ? C31 P1 Au1 111.0(2) . . ? C5 N1 C1 118.3(5) . . ? C5 N1 Au1 119.0(4) . . ? C1 N1 Au1 122.6(4) . . ? N1 C1 C2 121.8(6) . . ? C3 C2 C1 119.6(6) . . ? C2 C3 C4 118.8(6) . . ? C5 C4 C3 119.2(6) . . ? N1 C5 C4 122.3(6) . . ? N1 C5 N2 111.2(5) . . ? C4 C5 N2 126.5(5) . . ? N2 N2 C5 114.0(6) 2_757 . ? C16 C11 C12 119.1(7) . . ? C16 C11 P1 118.4(5) . . ? C12 C11 P1 122.4(5) . . ? C11 C12 C13 119.8(7) . . ? C14 C13 C12 119.8(8) . . ? C13 C14 C15 120.3(8) . . ? C16 C15 C14 120.5(8) . . ? C15 C16 C11 120.4(8) . . ? C26 C21 C22 119.3(6) . . ? C26 C21 P1 121.6(5) . . ? C22 C21 P1 119.1(5) . . ? C21 C22 C23 119.2(7) . . ? C24 C23 C22 120.9(7) . . ? C23 C24 C25 120.3(7) . . ? C24 C25 C26 120.1(7) . . ? C21 C26 C25 120.2(7) . . ? C36 C31 C32 119.1(6) . . ? C36 C31 P1 122.4(6) . . ? C32 C31 P1 118.4(5) . . ? C33 C32 C31 120.4(8) . . ? C34 C33 C32 118.6(9) . . ? C33 C34 C35 121.5(8) . . ? C36 C35 C34 119.8(9) . . ? C35 C36 C31 120.5(8) . . ? O3 S1 O1 117.0(5) . . ? O3 S1 O2 114.2(6) . . ? O1 S1 O2 112.7(5) . . ? O3 S1 C41 107.5(6) . . ? O1 S1 C41 104.2(4) . . ? O2 S1 C41 98.9(6) . . ? F2 C41 F3 111.8(12) . . ? F2 C41 F1 107.9(11) . . ? F3 C41 F1 104.1(9) . . ? F2 C41 S1 114.0(8) . . ? F3 C41 S1 112.4(8) . . ? F1 C41 S1 105.9(9) . . ? _diffrn_measured_fraction_theta_max 0.792 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.9896 _refine_diff_density_max 1.282 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.129 #======END data_abpypac _database_code_depnum_ccdc_archive 'CCDC 792814' #TrackingRef '- publicB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Au2 F6 N4 O6 P2 S2' _chemical_formula_weight 1028.42 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 '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/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 25.1997(11) _cell_length_b 8.7245(4) _cell_length_c 7.2138(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.326(4) _cell_angle_gamma 90.00 _cell_volume 1543.28(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1836 _cell_measurement_theta_min 2.8986 _cell_measurement_theta_max 29.4132 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.4068 _exptl_crystal_size_mid 0.1248 _exptl_crystal_size_min 0.0379 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 9.809 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details ; 'Tue Jan 26 11:16:18 2010' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4757 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3116 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 29.47 _reflns_number_total 1892 _reflns_number_gt 1469 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; 'Tue Jan 26 11:16:18 2010' ; _computing_cell_refinement ; 'Tue Jan 26 11:16:18 2010' ; _computing_data_reduction ; 'Tue Jan 26 11:16:18 2010' ; _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. We solved the structure with a 0.5 occupancy for the N(2) atom, therefore we are assuming a 50% disorder between N2 and N2B versus N2A and N2C as the best solution to solve the molecule in the C2/m space group with reasonable bond distances; the highest residual density peaks are very close to the gold center. ; _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^)+(0.0893P)^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 1892 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Au1 Au 0.337308(18) 0.5000 0.08494(6) 0.0467(2) Uani 1 2 d S . . P1 P 0.27168(13) 0.5000 0.2450(4) 0.0420(7) Uani 1 2 d S . . N1 N 0.3981(4) 0.5000 -0.0688(15) 0.049(3) Uani 1 2 d S . . C1 C 0.4153(4) 0.3662(17) -0.1280(17) 0.071(3) Uani 1 1 d . . . H1 H 0.4048 0.2733 -0.0843 0.085 Uiso 1 1 calc R . . C2 C 0.4486(5) 0.370(2) -0.254(2) 0.091(5) Uani 1 1 d . . . H2 H 0.4598 0.2774 -0.2965 0.109 Uiso 1 1 calc R . . C3 C 0.4656(7) 0.5000 -0.317(2) 0.082(6) Uani 1 2 d S . . N2 N 0.5009(9) 0.445(2) -0.444(2) 0.065(5) Uani 0.50 1 d P . . C10 C 0.2278(4) 0.3368(13) 0.1975(16) 0.061(3) Uani 1 1 d . . . H10A H 0.2010 0.3428 0.2726 0.092 Uiso 1 1 calc R . . H10B H 0.2490 0.2451 0.2296 0.092 Uiso 1 1 calc R . . H10C H 0.2099 0.3349 0.0648 0.092 Uiso 1 1 calc R . . C11 C 0.2994(6) 0.5000 0.4980(19) 0.065(4) Uani 1 2 d S . . H11A H 0.3221 0.5886 0.5327 0.098 Uiso 0.50 1 calc PR . . H11B H 0.3206 0.4089 0.5335 0.098 Uiso 0.50 1 calc PR . . H11C H 0.2701 0.5025 0.5629 0.098 Uiso 0.50 1 calc SR . . S1 S 0.3634(2) 0.0000 0.4091(9) 0.0989(17) Uani 1 2 d S . . O1 O 0.3940(11) 0.0000 0.600(3) 0.193(12) Uani 1 2 d S . . O2 O 0.3366(11) 0.124(4) 0.354(4) 0.38(2) Uani 1 1 d . . . C12 C 0.4121(10) 0.0000 0.282(3) 0.101(7) Uani 1 2 d S . . F1 F 0.3944(9) 0.0000 0.100(2) 0.174(8) Uani 1 2 d S . . F2 F 0.4440(7) 0.114(2) 0.320(2) 0.253(11) 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 Au1 0.0439(3) 0.0572(4) 0.0455(3) 0.000 0.02387(19) 0.000 P1 0.0423(17) 0.0477(19) 0.0429(14) 0.000 0.0238(12) 0.000 N1 0.042(6) 0.060(7) 0.053(5) 0.000 0.027(4) 0.000 C1 0.049(6) 0.084(8) 0.088(7) -0.007(7) 0.034(5) 0.007(6) C2 0.055(7) 0.136(14) 0.096(8) -0.029(9) 0.045(6) 0.004(8) C3 0.040(8) 0.15(2) 0.065(9) 0.000 0.031(7) 0.000 N2 0.084(12) 0.059(11) 0.068(11) 0.006(7) 0.053(11) 0.015(9) C10 0.064(6) 0.054(6) 0.077(6) -0.005(5) 0.039(5) -0.013(5) C11 0.066(10) 0.085(12) 0.047(6) 0.000 0.020(6) 0.000 S1 0.076(3) 0.115(5) 0.115(4) 0.000 0.041(3) 0.000 O1 0.21(2) 0.29(4) 0.091(12) 0.000 0.067(14) 0.000 O2 0.35(3) 0.50(5) 0.36(3) 0.21(3) 0.20(3) 0.36(4) C12 0.093(15) 0.13(2) 0.080(12) 0.000 0.013(11) 0.000 F1 0.202(19) 0.22(2) 0.095(10) 0.000 0.028(11) 0.000 F2 0.225(15) 0.34(3) 0.234(16) -0.081(16) 0.124(13) -0.189(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 Au1 N1 2.088(10) . ? Au1 P1 2.225(3) . ? P1 C10 1.787(10) . ? P1 C10 1.787(10) 6_565 ? P1 C11 1.797(13) . ? N1 C1 1.348(14) . ? N1 C1 1.348(14) 6_565 ? C1 C2 1.371(16) . ? C2 C3 1.331(18) . ? C3 C2 1.331(18) 6_565 ? C3 N2 1.50(2) 6_565 ? C3 N2 1.50(2) . ? N2 N2 0.79(3) 2_654 ? N2 N2 0.95(4) 6_565 ? N2 N2 1.24(3) 5_664 ? S1 O2 1.28(2) 6 ? S1 O2 1.28(2) . ? S1 O1 1.41(2) . ? S1 C12 1.69(3) . ? C12 F2 1.267(17) . ? C12 F2 1.267(17) 6 ? C12 F1 1.28(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 N1 Au1 P1 179.2(3) . . ? C10 P1 C10 105.7(8) . 6_565 ? C10 P1 C11 105.8(5) . . ? C10 P1 C11 105.8(5) 6_565 . ? C10 P1 Au1 113.7(3) . . ? C10 P1 Au1 113.7(3) 6_565 . ? C11 P1 Au1 111.5(5) . . ? C1 N1 C1 119.9(13) . 6_565 ? C1 N1 Au1 119.8(7) . . ? C1 N1 Au1 119.8(7) 6_565 . ? N1 C1 C2 118.7(14) . . ? C3 C2 C1 122.7(15) . . ? C2 C3 C2 117.2(16) 6_565 . ? C2 C3 N2 102.8(10) 6_565 6_565 ? C2 C3 N2 140.0(12) . 6_565 ? C2 C3 N2 140.0(12) 6_565 . ? C2 C3 N2 102.8(10) . . ? N2 C3 N2 37.2(15) 6_565 . ? N2 N2 N2 90.000(9) 2_654 6_565 ? N2 N2 N2 50.2(16) 2_654 5_664 ? N2 N2 N2 39.8(16) 6_565 5_664 ? N2 N2 C3 136(4) 2_654 . ? N2 N2 C3 71.4(7) 6_565 . ? N2 N2 C3 102.4(18) 5_664 . ? O2 S1 O2 114(3) 6 . ? O2 S1 O1 115.5(16) 6 . ? O2 S1 O1 115.5(16) . . ? O2 S1 C12 103.1(13) 6 . ? O2 S1 C12 103.1(13) . . ? O1 S1 C12 103.0(13) . . ? F2 C12 F2 103(3) . 6 ? F2 C12 F1 105.8(17) . . ? F2 C12 F1 105.8(17) 6 . ? F2 C12 S1 112.9(15) . . ? F2 C12 S1 112.9(15) 6 . ? F1 C12 S1 115(2) . . ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.907 _refine_diff_density_min -2.009 _refine_diff_density_rms 0.228 #======END data_mba25bm _database_code_depnum_ccdc_archive 'CCDC 792815' #TrackingRef '- publicB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Ag2 F6 N4 O6 P2 S2' _chemical_formula_weight 1222.62 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.362(6) _cell_length_b 10.197(6) _cell_length_c 14.119(9) _cell_angle_alpha 101.554(11) _cell_angle_beta 103.206(11) _cell_angle_gamma 93.791(12) _cell_volume 1276.8(13) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818676 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; SADABS; a Program for Absorption Correction with the Siemens SMART system (1996). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12646 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.35 _reflns_number_total 6189 _reflns_number_gt 3043 _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^)+(0.0776P)^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 6189 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.005 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 0.21590(5) 0.37826(5) 0.39545(3) 0.0575(2) Uani 1 1 d . . . P1 P 0.11224(16) 0.23909(15) 0.23726(11) 0.0475(4) Uani 1 1 d . . . N1 N 0.2634(5) 0.5937(5) 0.4849(3) 0.0502(12) Uani 1 1 d . . . N2 N 0.4805(5) 0.4416(4) 0.4752(3) 0.0453(11) Uani 1 1 d . . . O1 O 0.1906(6) 0.3137(8) 0.5481(4) 0.132(3) Uani 1 1 d . . . C1 C 0.1607(7) 0.6749(7) 0.4958(5) 0.0675(18) Uani 1 1 d . . . H1 H 0.0626 0.6421 0.4646 0.081 Uiso 1 1 calc R . . C2 C 0.1924(8) 0.8060(7) 0.5514(5) 0.076(2) Uani 1 1 d . . . H2 H 0.1172 0.8597 0.5579 0.091 Uiso 1 1 calc R . . C3 C 0.3363(9) 0.8548(7) 0.5964(6) 0.081(2) Uani 1 1 d . . . H3 H 0.3614 0.9433 0.6328 0.097 Uiso 1 1 calc R . . C4 C 0.4441(7) 0.7701(6) 0.5870(5) 0.0688(18) Uani 1 1 d . . . H4 H 0.5429 0.8002 0.6180 0.083 Uiso 1 1 calc R . . C5 C 0.4033(6) 0.6420(5) 0.5315(4) 0.0452(13) Uani 1 1 d . . . C11 C 0.1824(6) 0.0759(6) 0.2233(4) 0.0512(14) Uani 1 1 d . . . C12 C 0.2038(8) 0.0148(7) 0.3046(5) 0.0705(18) Uani 1 1 d . . . H12 H 0.1779 0.0557 0.3623 0.085 Uiso 1 1 calc R . . C13 C 0.2623(10) -0.1044(8) 0.2999(7) 0.093(2) Uani 1 1 d . . . H13 H 0.2774 -0.1442 0.3547 0.111 Uiso 1 1 calc R . . C14 C 0.2991(9) -0.1660(8) 0.2141(8) 0.098(3) Uani 1 1 d . . . H14 H 0.3398 -0.2470 0.2117 0.117 Uiso 1 1 calc R . . C15 C 0.2772(8) -0.1114(8) 0.1335(6) 0.079(2) Uani 1 1 d . . . H15 H 0.3002 -0.1547 0.0753 0.095 Uiso 1 1 calc R . . C16 C 0.2191(7) 0.0120(7) 0.1390(5) 0.0638(17) Uani 1 1 d . . . H16 H 0.2051 0.0514 0.0841 0.077 Uiso 1 1 calc R . . C21 C 0.1584(6) 0.3142(6) 0.1401(4) 0.0528(14) Uani 1 1 d . . . C22 C 0.2883(7) 0.3997(7) 0.1638(5) 0.0636(17) Uani 1 1 d . . . H22 H 0.3496 0.4181 0.2279 0.076 Uiso 1 1 calc R . . C23 C 0.3262(9) 0.4579(8) 0.0909(7) 0.086(2) Uani 1 1 d . . . H23 H 0.4146 0.5142 0.1066 0.103 Uiso 1 1 calc R . . C24 C 0.2373(11) 0.4346(9) -0.0031(7) 0.098(3) Uani 1 1 d . . . H24 H 0.2630 0.4765 -0.0506 0.118 Uiso 1 1 calc R . . C25 C 0.1073(10) 0.3471(10) -0.0270(6) 0.100(3) Uani 1 1 d . . . H25 H 0.0469 0.3280 -0.0914 0.120 Uiso 1 1 calc R . . C26 C 0.0685(8) 0.2889(8) 0.0447(5) 0.077(2) Uani 1 1 d . . . H26 H -0.0193 0.2318 0.0287 0.093 Uiso 1 1 calc R . . C31 C -0.0884(6) 0.2043(6) 0.1993(4) 0.0510(14) Uani 1 1 d . . . C32 C -0.1618(7) 0.0784(7) 0.1529(5) 0.0609(16) Uani 1 1 d . . . H32 H -0.1094 0.0051 0.1406 0.073 Uiso 1 1 calc R . . C33 C -0.3166(8) 0.0618(8) 0.1244(5) 0.080(2) Uani 1 1 d . . . H33 H -0.3669 -0.0236 0.0947 0.096 Uiso 1 1 calc R . . C34 C -0.3941(8) 0.1687(10) 0.1396(6) 0.091(2) Uani 1 1 d . . . H34 H -0.4966 0.1572 0.1172 0.109 Uiso 1 1 calc R . . C35 C -0.3218(8) 0.2923(9) 0.1874(7) 0.091(2) Uani 1 1 d . . . H35 H -0.3751 0.3648 0.2005 0.109 Uiso 1 1 calc R . . C36 C -0.1684(7) 0.3109(7) 0.2170(5) 0.0722(19) Uani 1 1 d . . . H36 H -0.1194 0.3961 0.2491 0.087 Uiso 1 1 calc R . . O2 O 0.4035(9) 0.4037(8) 0.6798(5) 0.156(3) Uani 1 1 d . . . O3 O 0.3783(9) 0.1823(8) 0.5902(6) 0.155(3) Uani 1 1 d . . . S1 S 0.3045(2) 0.2928(2) 0.62278(14) 0.0713(5) Uani 1 1 d . . . C6 C 0.2093(14) 0.2373(10) 0.7055(8) 0.111(3) Uani 1 1 d . . . F1 F 0.1236(8) 0.3233(7) 0.7344(5) 0.166(3) Uani 1 1 d . . . F2 F 0.1247(9) 0.1234(7) 0.6648(7) 0.192(4) Uani 1 1 d . . . F3 F 0.3059(9) 0.2179(9) 0.7854(5) 0.197(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0491(3) 0.0633(3) 0.0456(3) -0.0039(2) -0.00143(19) -0.0012(2) P1 0.0415(8) 0.0515(9) 0.0410(8) 0.0026(7) 0.0015(6) -0.0012(7) N1 0.041(3) 0.052(3) 0.050(3) 0.002(2) 0.004(2) 0.011(2) N2 0.039(2) 0.045(3) 0.046(3) -0.002(2) 0.010(2) 0.001(2) O1 0.058(3) 0.266(9) 0.100(4) 0.114(5) 0.013(3) 0.021(4) C1 0.051(4) 0.074(5) 0.072(4) 0.010(4) 0.007(3) 0.019(3) C2 0.072(5) 0.072(5) 0.080(5) 0.006(4) 0.016(4) 0.038(4) C3 0.086(5) 0.054(4) 0.090(5) -0.005(4) 0.014(4) 0.012(4) C4 0.063(4) 0.054(4) 0.071(4) -0.008(3) -0.003(3) 0.012(3) C5 0.045(3) 0.047(3) 0.042(3) 0.003(2) 0.010(2) 0.011(3) C11 0.040(3) 0.053(3) 0.051(3) 0.001(3) 0.004(3) -0.008(3) C12 0.073(5) 0.067(5) 0.071(5) 0.019(4) 0.014(4) 0.008(4) C13 0.114(7) 0.069(5) 0.095(6) 0.031(5) 0.015(5) 0.016(5) C14 0.095(6) 0.064(5) 0.125(8) 0.010(5) 0.018(6) 0.019(4) C15 0.078(5) 0.073(5) 0.074(5) -0.007(4) 0.015(4) 0.014(4) C16 0.056(4) 0.067(4) 0.056(4) 0.000(3) 0.002(3) 0.002(3) C21 0.044(3) 0.060(4) 0.051(3) 0.008(3) 0.009(3) 0.005(3) C22 0.053(4) 0.071(4) 0.065(4) 0.013(3) 0.016(3) 0.001(3) C23 0.070(5) 0.090(6) 0.105(6) 0.025(5) 0.038(5) -0.005(4) C24 0.115(7) 0.110(7) 0.085(6) 0.047(5) 0.039(6) 0.005(6) C25 0.097(6) 0.136(8) 0.068(5) 0.043(5) 0.010(5) 0.000(6) C26 0.064(4) 0.109(6) 0.051(4) 0.023(4) 0.002(3) -0.013(4) C31 0.046(3) 0.059(4) 0.044(3) 0.011(3) 0.004(3) -0.001(3) C32 0.055(4) 0.064(4) 0.057(4) 0.011(3) 0.006(3) -0.001(3) C33 0.059(4) 0.087(5) 0.078(5) 0.011(4) 0.001(4) -0.020(4) C34 0.049(4) 0.121(7) 0.102(6) 0.041(6) 0.006(4) -0.001(5) C35 0.060(5) 0.105(6) 0.114(7) 0.035(5) 0.020(5) 0.026(5) C36 0.047(4) 0.076(5) 0.088(5) 0.015(4) 0.010(3) -0.001(3) O2 0.182(7) 0.136(6) 0.112(5) 0.006(4) 0.003(5) -0.077(5) O3 0.166(7) 0.145(6) 0.210(8) 0.064(6) 0.120(7) 0.076(6) S1 0.0690(11) 0.0823(13) 0.0650(11) 0.0277(10) 0.0117(9) 0.0071(10) C6 0.170(10) 0.089(7) 0.106(7) 0.045(6) 0.064(7) 0.059(7) F1 0.233(7) 0.187(6) 0.144(5) 0.068(5) 0.132(6) 0.101(6) F2 0.226(8) 0.116(5) 0.282(10) 0.062(6) 0.152(8) -0.014(5) F3 0.208(7) 0.288(10) 0.146(6) 0.157(7) 0.041(5) 0.059(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.263(5) . ? Ag1 P1 2.3457(18) . ? Ag1 O1 2.432(5) . ? Ag1 N2 2.458(4) . ? P1 C21 1.817(6) . ? P1 C11 1.820(6) . ? P1 C31 1.821(6) . ? N1 C1 1.325(7) . ? N1 C5 1.335(7) . ? N2 N2 1.238(8) 2_666 ? N2 C5 1.434(7) 2_666 ? O1 S1 1.379(5) . ? C1 C2 1.383(9) . ? C2 C3 1.364(10) . ? C3 C4 1.383(9) . ? C4 C5 1.362(8) . ? C5 N2 1.434(7) 2_666 ? C11 C16 1.366(8) . ? C11 C12 1.394(8) . ? C12 C13 1.362(10) . ? C13 C14 1.378(12) . ? C14 C15 1.345(11) . ? C15 C16 1.398(9) . ? C21 C26 1.380(8) . ? C21 C22 1.382(8) . ? C22 C23 1.386(10) . ? C23 C24 1.361(11) . ? C24 C25 1.393(12) . ? C25 C26 1.375(10) . ? C31 C36 1.375(9) . ? C31 C32 1.375(8) . ? C32 C33 1.402(9) . ? C33 C34 1.357(11) . ? C34 C35 1.357(11) . ? C35 C36 1.390(9) . ? O2 S1 1.393(6) . ? O3 S1 1.414(7) . ? S1 C6 1.775(10) . ? C6 F1 1.296(10) . ? C6 F2 1.308(13) . ? C6 F3 1.333(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 P1 144.81(12) . . ? N1 Ag1 O1 87.0(2) . . ? P1 Ag1 O1 122.2(2) . . ? N1 Ag1 N2 68.10(15) . . ? P1 Ag1 N2 126.62(11) . . ? O1 Ag1 N2 87.65(17) . . ? C21 P1 C11 105.9(3) . . ? C21 P1 C31 103.8(3) . . ? C11 P1 C31 106.2(3) . . ? C21 P1 Ag1 110.8(2) . . ? C11 P1 Ag1 112.16(19) . . ? C31 P1 Ag1 116.97(19) . . ? C1 N1 C5 117.5(5) . . ? C1 N1 Ag1 124.2(4) . . ? C5 N1 Ag1 118.3(3) . . ? N2 N2 C5 115.8(5) 2_666 2_666 ? N2 N2 Ag1 117.5(5) 2_666 . ? C5 N2 Ag1 126.7(3) 2_666 . ? S1 O1 Ag1 125.9(3) . . ? N1 C1 C2 123.2(6) . . ? C3 C2 C1 118.6(6) . . ? C2 C3 C4 118.8(6) . . ? C5 C4 C3 118.9(6) . . ? N1 C5 C4 123.1(5) . . ? N1 C5 N2 120.4(5) . 2_666 ? C4 C5 N2 116.5(5) . 2_666 ? C16 C11 C12 118.3(6) . . ? C16 C11 P1 123.7(5) . . ? C12 C11 P1 117.9(5) . . ? C13 C12 C11 120.4(7) . . ? C12 C13 C14 119.9(8) . . ? C15 C14 C13 121.3(8) . . ? C14 C15 C16 118.7(7) . . ? C11 C16 C15 121.4(7) . . ? C26 C21 C22 119.5(6) . . ? C26 C21 P1 122.3(5) . . ? C22 C21 P1 118.2(5) . . ? C21 C22 C23 119.3(7) . . ? C24 C23 C22 121.6(7) . . ? C23 C24 C25 119.0(8) . . ? C26 C25 C24 119.9(8) . . ? C25 C26 C21 120.7(7) . . ? C36 C31 C32 119.3(6) . . ? C36 C31 P1 117.5(5) . . ? C32 C31 P1 123.2(5) . . ? C31 C32 C33 119.2(6) . . ? C34 C33 C32 120.9(7) . . ? C33 C34 C35 119.8(7) . . ? C34 C35 C36 120.2(8) . . ? C31 C36 C35 120.5(7) . . ? O1 S1 O2 118.1(5) . . ? O1 S1 O3 112.5(5) . . ? O2 S1 O3 111.7(6) . . ? O1 S1 C6 102.5(5) . . ? O2 S1 C6 106.0(5) . . ? O3 S1 C6 104.3(4) . . ? F1 C6 F2 106.1(11) . . ? F1 C6 F3 109.0(9) . . ? F2 C6 F3 107.1(8) . . ? F1 C6 S1 111.8(6) . . ? F2 C6 S1 112.7(8) . . ? F3 C6 S1 110.0(9) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.915 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.094 #======END