Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Edward Szlyk' 'Tadeusz Glowiak' 'Artur Golinski' 'Andrzej Surdykowski' 'Iwona Szymanska' ; A.Wojtczak ; _publ_contact_author_name 'Dr Edward Szlyk' _publ_contact_author_address ; Department of Chemistry Nicholas Copernicus University Torun 87-100 POLAND ; _publ_contact_author_email ESZLYK@CHEM.UNI.TORUN.PL _publ_section_title ; X Ray crystal dtructure of [Ag4(u-dppm)2(u-C2F5COO)4]. Synthesis and Spectroscopy of Silver(I) Perfluorinated Carboxylate Complexes with Bis(diphenylphosphino)methane ; data_silver2 _database_code_CSD 208152 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H22 Ag2 F10 O4 P2' _chemical_formula_weight 926.17 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.079(5) _cell_length_b 13.725(3) _cell_length_c 20.382(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.56(3) _cell_angle_gamma 90.00 _cell_volume 6651(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _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 'Kuma KM4CCD automatic diffractometer' _diffrn_measurement_method 'profile data from omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21280 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7170 _reflns_number_gt 6333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4CCD software 1998' _computing_cell_refinement 'Kuma KM4CCD software 1998' _computing_data_reduction 'Kuma KM4CCD software 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+20.2550P] 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_number_reflns 7170 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.198443(9) 0.162388(15) 0.019841(10) 0.01634(6) Uani 1 d . . . Ag2 Ag 0.251659(9) 0.295172(16) 0.142759(11) 0.01854(7) Uani 1 d . . . P11 P 0.16612(3) 0.07964(5) 0.10149(3) 0.01343(14) Uani 1 d . . . P12 P 0.25322(3) 0.17416(5) 0.22490(4) 0.01456(14) Uani 1 d . . . O1 O 0.29665(8) 0.17644(14) 0.01760(11) 0.0191(4) Uani 1 d . . . O2 O 0.30881(9) 0.09321(16) -0.07214(11) 0.0240(5) Uani 1 d . . . O3 O 0.18267(9) 0.13222(16) -0.09861(10) 0.0217(4) Uani 1 d . . . O4 O 0.16219(9) 0.06761(16) -0.20452(11) 0.0235(5) Uani 1 d . . . F1 F 0.31186(10) 0.00535(18) 0.08554(13) 0.0511(7) Uani 1 d . . . F2 F 0.33621(12) -0.06372(15) 0.00464(12) 0.0545(7) Uani 1 d . . . F3 F 0.4258(4) 0.0847(8) 0.0480(7) 0.084(5) Uani 0.50 d P . . F31 F 0.4274(5) 0.0367(8) 0.0259(6) 0.071(3) Uani 0.50 d P . . F4 F 0.3951(6) 0.1102(11) 0.1334(7) 0.091(5) Uani 0.50 d P . . F41 F 0.4139(4) 0.1101(8) 0.1112(6) 0.065(4) Uani 0.50 d P . . F5 F 0.42471(9) -0.03809(18) 0.11557(13) 0.0482(6) Uani 1 d . . . F6 F 0.07126(9) -0.01618(16) -0.19473(11) 0.0396(5) Uani 1 d . . . F7 F 0.10784(9) -0.00758(15) -0.08260(10) 0.0342(5) Uani 1 d . . . F8 F 0.05121(9) 0.18806(18) -0.19193(12) 0.0436(5) Uani 1 d . . . F9 F 0.00459(9) 0.08830(19) -0.14954(12) 0.0469(6) Uani 1 d . . . F10 F 0.07150(9) 0.17301(17) -0.08134(11) 0.0403(5) Uani 1 d . . . C1 C 0.31127(12) 0.1046(2) -0.01121(15) 0.0196(6) Uani 1 d . . . C2 C 0.33893(13) 0.0208(2) 0.03917(16) 0.0218(6) Uani 1 d . . . C3 C 0.39981(16) 0.0382(3) 0.0788(2) 0.0476(11) Uani 1 d . . . C4 C 0.15274(12) 0.0834(2) -0.14993(15) 0.0187(6) Uani 1 d . . . C5 C 0.09760(14) 0.0441(2) -0.14176(15) 0.0236(6) Uani 1 d . . . C6 C 0.05555(14) 0.1244(3) -0.14130(17) 0.0290(7) Uani 1 d . . . C7 C 0.21977(12) 0.0592(2) 0.18593(15) 0.0161(5) Uani 1 d . . . C11 C 0.13803(12) -0.0423(2) 0.07704(14) 0.0161(5) Uani 1 d . . . C12 C 0.17483(14) -0.1182(2) 0.07655(16) 0.0247(6) Uani 1 d . . . C13 C 0.15431(16) -0.2105(2) 0.05372(18) 0.0292(7) Uani 1 d . . . C14 C 0.09684(16) -0.2269(2) 0.03011(19) 0.0308(7) Uani 1 d . . . C15 C 0.06016(15) -0.1518(3) 0.0298(2) 0.0336(8) Uani 1 d . . . C16 C 0.08050(13) -0.0598(2) 0.05336(17) 0.0246(7) Uani 1 d . . . C21 C 0.11055(12) 0.1464(2) 0.12092(14) 0.0158(5) Uani 1 d . . . C22 C 0.08974(12) 0.2316(2) 0.08430(15) 0.0182(6) Uani 1 d . . . C23 C 0.04631(13) 0.2830(2) 0.09734(17) 0.0233(6) Uani 1 d . . . C24 C 0.02422(14) 0.2499(2) 0.14737(18) 0.0268(7) Uani 1 d . . . C25 C 0.04490(15) 0.1659(3) 0.18409(19) 0.0296(7) Uani 1 d . . . C26 C 0.08802(13) 0.1137(2) 0.17141(16) 0.0212(6) Uani 1 d . . . C31 C 0.21570(12) 0.2090(2) 0.28416(15) 0.0184(6) Uani 1 d . . . C32 C 0.18120(14) 0.2909(2) 0.26807(17) 0.0259(7) Uani 1 d . . . C33 C 0.14991(16) 0.3183(3) 0.3104(2) 0.0351(8) Uani 1 d . . . C34 C 0.15291(15) 0.2646(3) 0.36865(19) 0.0344(8) Uani 1 d . . . C35 C 0.18807(17) 0.1840(3) 0.38570(19) 0.0325(8) Uani 1 d . . . C36 C 0.21861(14) 0.1555(2) 0.34337(17) 0.0246(6) Uani 1 d . . . C41 C 0.32288(12) 0.1362(2) 0.27735(15) 0.0199(6) Uani 1 d . . . C42 C 0.33246(14) 0.0470(2) 0.31290(17) 0.0252(7) Uani 1 d . . . C43 C 0.38664(15) 0.0198(3) 0.35101(19) 0.0327(8) Uani 1 d . . . C44 C 0.43120(15) 0.0799(3) 0.3539(2) 0.0392(9) Uani 1 d . . . C45 C 0.42238(15) 0.1684(3) 0.3199(2) 0.0378(9) Uani 1 d . . . C46 C 0.36813(14) 0.1972(2) 0.28161(17) 0.0260(7) Uani 1 d . . . H12 H 0.2121(15) -0.107(2) 0.0910(17) 0.017(8) Uiso 1 d . . . H13 H 0.1785(16) -0.262(3) 0.057(2) 0.032(10) Uiso 1 d . . . H14 H 0.0833(18) -0.289(3) 0.017(2) 0.042(12) Uiso 1 d . . . H15 H 0.0194(18) -0.162(3) 0.016(2) 0.038(11) Uiso 1 d . . . H16 H 0.0563(17) -0.012(3) 0.055(2) 0.034(10) Uiso 1 d . . . H22 H 0.1083(16) 0.258(3) 0.048(2) 0.033(10) Uiso 1 d . . . H23 H 0.0309(14) 0.342(3) 0.0694(18) 0.021(9) Uiso 1 d . . . H24 H -0.0024(16) 0.286(3) 0.1554(19) 0.027(10) Uiso 1 d . . . H25 H 0.0299(18) 0.141(3) 0.218(2) 0.049(12) Uiso 1 d . . . H26 H 0.1028(14) 0.059(3) 0.1980(18) 0.021(9) Uiso 1 d . . . H32 H 0.1777(16) 0.327(3) 0.224(2) 0.030(10) Uiso 1 d . . . H33 H 0.1275(17) 0.375(3) 0.298(2) 0.035(11) Uiso 1 d . . . H34 H 0.1328(18) 0.284(3) 0.399(2) 0.041(11) Uiso 1 d . . . H35 H 0.1899(17) 0.150(3) 0.421(2) 0.034(11) Uiso 1 d . . . H36 H 0.2422(14) 0.105(3) 0.3545(17) 0.020(9) Uiso 1 d . . . H42 H 0.3030(15) 0.005(3) 0.3102(18) 0.025(9) Uiso 1 d . . . H43 H 0.3891(17) -0.042(3) 0.373(2) 0.042(11) Uiso 1 d . . . H44 H 0.467(2) 0.062(4) 0.380(3) 0.063(15) Uiso 1 d . . . H45 H 0.452(2) 0.209(3) 0.324(2) 0.048(13) Uiso 1 d . . . H46 H 0.3624(14) 0.260(3) 0.2577(18) 0.021(8) Uiso 1 d . . . H71 H 0.2464(14) 0.022(2) 0.1761(16) 0.014(8) Uiso 1 d . . . H72 H 0.2043(15) 0.025(3) 0.2128(19) 0.025(9) Uiso 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 0.01993(11) 0.01765(11) 0.01368(11) 0.00098(8) 0.00849(8) -0.00201(8) Ag2 0.02342(12) 0.01684(11) 0.01525(11) 0.00268(8) 0.00599(8) -0.00283(9) P11 0.0149(3) 0.0147(3) 0.0116(3) -0.0005(3) 0.0056(3) -0.0016(3) P12 0.0154(3) 0.0156(3) 0.0125(3) 0.0009(3) 0.0042(3) -0.0018(3) O1 0.0194(10) 0.0161(10) 0.0237(11) 0.0033(8) 0.0095(8) 0.0012(8) O2 0.0307(12) 0.0238(11) 0.0190(11) 0.0038(9) 0.0102(9) 0.0090(9) O3 0.0258(11) 0.0267(11) 0.0129(9) -0.0035(8) 0.0067(8) -0.0082(9) O4 0.0340(12) 0.0216(11) 0.0187(10) -0.0042(8) 0.0137(9) -0.0055(9) F1 0.0515(14) 0.0542(14) 0.0643(16) 0.0414(13) 0.0418(13) 0.0273(12) F2 0.0892(19) 0.0187(10) 0.0406(13) -0.0014(9) -0.0007(13) 0.0136(11) F3 0.020(3) 0.095(8) 0.126(12) 0.085(8) 0.005(5) -0.007(5) F31 0.025(3) 0.136(10) 0.060(5) 0.053(6) 0.023(3) 0.022(6) F4 0.111(11) 0.065(5) 0.053(6) -0.013(4) -0.035(6) 0.012(7) F41 0.046(5) 0.029(3) 0.085(10) -0.010(5) -0.029(5) -0.003(3) F5 0.0284(11) 0.0503(14) 0.0567(15) 0.0316(12) 0.0009(10) 0.0085(10) F6 0.0423(12) 0.0464(13) 0.0371(12) -0.0255(10) 0.0223(10) -0.0258(10) F7 0.0423(11) 0.0337(11) 0.0336(11) 0.0095(9) 0.0222(9) -0.0052(9) F8 0.0348(12) 0.0540(14) 0.0410(13) 0.0173(11) 0.0106(10) 0.0115(10) F9 0.0230(10) 0.0708(17) 0.0507(14) -0.0132(12) 0.0171(10) -0.0122(11) F10 0.0340(11) 0.0498(13) 0.0373(12) -0.0180(10) 0.0115(9) 0.0022(10) C1 0.0133(13) 0.0241(15) 0.0221(15) 0.0056(12) 0.0067(11) 0.0039(11) C2 0.0224(14) 0.0161(14) 0.0279(16) 0.0017(12) 0.0095(12) -0.0010(12) C3 0.032(2) 0.044(2) 0.053(3) 0.029(2) -0.0059(18) -0.0055(18) C4 0.0221(14) 0.0181(14) 0.0157(13) 0.0030(11) 0.0056(11) 0.0003(12) C5 0.0310(16) 0.0248(15) 0.0155(14) -0.0039(12) 0.0083(12) -0.0078(13) C6 0.0250(16) 0.0389(19) 0.0244(16) -0.0050(14) 0.0099(13) -0.0024(15) C7 0.0173(13) 0.0162(13) 0.0153(13) 0.0013(11) 0.0060(11) -0.0006(11) C11 0.0216(13) 0.0156(13) 0.0121(12) -0.0016(10) 0.0070(11) -0.0051(11) C12 0.0251(16) 0.0232(15) 0.0240(16) -0.0055(12) 0.0054(13) 0.0019(13) C13 0.0401(19) 0.0167(15) 0.0275(17) -0.0040(13) 0.0060(14) 0.0047(14) C14 0.042(2) 0.0200(16) 0.0328(18) -0.0100(14) 0.0155(15) -0.0110(15) C15 0.0269(17) 0.0336(19) 0.043(2) -0.0165(16) 0.0148(15) -0.0120(15) C16 0.0200(14) 0.0255(16) 0.0316(17) -0.0103(13) 0.0128(13) -0.0050(13) C21 0.0165(13) 0.0153(13) 0.0167(13) -0.0016(10) 0.0070(10) -0.0002(11) C22 0.0184(13) 0.0180(14) 0.0174(13) 0.0002(11) 0.0045(11) -0.0028(11) C23 0.0193(14) 0.0205(15) 0.0270(16) 0.0000(13) 0.0028(12) -0.0012(12) C24 0.0218(15) 0.0255(16) 0.0357(18) -0.0033(14) 0.0128(14) 0.0045(14) C25 0.0309(17) 0.0319(18) 0.0324(18) 0.0045(15) 0.0190(15) 0.0038(15) C26 0.0236(15) 0.0210(14) 0.0212(14) 0.0037(12) 0.0104(12) 0.0007(13) C31 0.0175(13) 0.0216(14) 0.0157(13) -0.0058(11) 0.0049(11) -0.0035(12) C32 0.0309(17) 0.0230(15) 0.0221(16) -0.0067(13) 0.0060(13) 0.0020(13) C33 0.0344(19) 0.0345(19) 0.036(2) -0.0129(16) 0.0108(16) 0.0056(16) C34 0.0331(18) 0.041(2) 0.0331(19) -0.0173(16) 0.0163(15) -0.0051(16) C35 0.045(2) 0.0356(19) 0.0237(17) -0.0036(15) 0.0197(16) -0.0078(16) C36 0.0291(16) 0.0220(15) 0.0258(16) 0.0007(13) 0.0129(13) -0.0014(14) C41 0.0218(14) 0.0228(15) 0.0158(14) -0.0010(11) 0.0073(11) -0.0028(12) C42 0.0227(15) 0.0246(16) 0.0280(16) 0.0059(13) 0.0075(13) -0.0011(13) C43 0.0274(17) 0.0312(18) 0.0369(19) 0.0115(15) 0.0067(14) 0.0049(15) C44 0.0202(16) 0.053(2) 0.040(2) 0.0146(18) 0.0035(15) 0.0065(16) C45 0.0183(15) 0.051(2) 0.039(2) 0.0123(18) 0.0014(14) -0.0074(16) C46 0.0236(15) 0.0285(17) 0.0235(16) 0.0067(13) 0.0043(13) -0.0039(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 O3 2.356(2) . ? Ag1 O1 2.356(2) 7 ? Ag1 P11 2.3612(8) . ? Ag1 O1 2.485(2) . ? Ag1 Ag2 3.0415(7) . ? Ag2 O2 2.308(2) 7 ? Ag2 O3 2.336(2) 7 ? Ag2 P12 2.3498(8) . ? P11 C21 1.814(3) . ? P11 C11 1.822(3) . ? P11 C7 1.838(3) . ? P12 C41 1.810(3) . ? P12 C31 1.816(3) . ? P12 C7 1.844(3) . ? O1 C1 1.261(4) . ? O1 Ag1 2.356(2) 7 ? O2 C1 1.234(4) . ? O2 Ag2 2.308(2) 7 ? O3 C4 1.267(4) . ? O3 Ag2 2.336(2) 7 ? O4 C4 1.228(4) . ? F1 C2 1.344(4) . ? F2 C2 1.347(4) . ? F3 F31 0.806(15) . ? F3 C3 1.218(10) . ? F3 F41 1.453(17) . ? F31 C3 1.454(11) . ? F4 F41 0.750(15) . ? F4 C3 1.521(13) . ? F41 C3 1.176(11) . ? F5 C3 1.323(4) . ? F6 C5 1.354(3) . ? F7 C5 1.352(4) . ? F8 C6 1.330(4) . ? F9 C6 1.331(4) . ? F10 C6 1.337(4) . ? C1 C2 1.551(4) . ? C2 C3 1.502(5) . ? C4 C5 1.542(4) . ? C5 C6 1.527(5) . ? C7 H71 0.91(3) . ? C7 H72 0.90(4) . ? C11 C16 1.389(4) . ? C11 C12 1.395(4) . ? C12 C13 1.391(5) . ? C12 H12 0.90(3) . ? C13 C14 1.385(5) . ? C13 H13 0.92(4) . ? C14 C15 1.380(5) . ? C14 H14 0.92(4) . ? C15 C16 1.389(5) . ? C15 H15 0.98(4) . ? C16 H16 0.90(4) . ? C21 C22 1.396(4) . ? C21 C26 1.397(4) . ? C22 C23 1.392(4) . ? C22 H22 1.05(4) . ? C23 C24 1.383(5) . ? C23 H23 1.00(4) . ? C24 C25 1.383(5) . ? C24 H24 0.88(4) . ? C25 C26 1.388(5) . ? C25 H25 0.95(5) . ? C26 H26 0.93(4) . ? C31 C32 1.393(4) . ? C31 C36 1.395(4) . ? C32 C33 1.390(5) . ? C32 H32 1.00(4) . ? C33 C34 1.379(6) . ? C33 H33 0.94(4) . ? C34 C35 1.388(6) . ? C34 H34 0.96(4) . ? C35 C36 1.381(5) . ? C35 H35 0.85(4) . ? C36 H36 0.89(4) . ? C41 C46 1.391(4) . ? C41 C42 1.404(4) . ? C42 C43 1.384(5) . ? C42 H42 0.93(4) . ? C43 C44 1.374(5) . ? C43 H43 0.96(4) . ? C44 C45 1.382(6) . ? C44 H44 0.92(5) . ? C45 C46 1.393(5) . ? C45 H45 0.91(5) . ? C46 H46 0.97(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ag1 O1 80.92(7) . 7 ? O3 Ag1 P11 130.88(5) . . ? O1 Ag1 P11 138.16(5) 7 . ? O3 Ag1 O1 80.73(8) . . ? O1 Ag1 O1 76.52(7) 7 . ? P11 Ag1 O1 127.94(5) . . ? O3 Ag1 Ag2 146.73(5) . . ? O1 Ag1 Ag2 69.50(5) 7 . ? P11 Ag1 Ag2 82.34(2) . . ? O1 Ag1 Ag2 77.94(5) . . ? O2 Ag2 O3 83.14(8) 7 7 ? O2 Ag2 P12 140.53(6) 7 . ? O3 Ag2 P12 136.22(6) 7 . ? O2 Ag2 Ag1 81.67(6) 7 . ? O3 Ag2 Ag1 96.70(5) 7 . ? P12 Ag2 Ag1 93.83(3) . . ? C21 P11 C11 105.47(13) . . ? C21 P11 C7 104.90(13) . . ? C11 P11 C7 102.72(13) . . ? C21 P11 Ag1 111.76(10) . . ? C11 P11 Ag1 116.00(9) . . ? C7 P11 Ag1 114.85(10) . . ? C41 P12 C31 106.86(13) . . ? C41 P12 C7 103.25(14) . . ? C31 P12 C7 104.52(13) . . ? C41 P12 Ag2 114.73(10) . . ? C31 P12 Ag2 113.16(10) . . ? C7 P12 Ag2 113.32(10) . . ? C1 O1 Ag1 122.07(18) . 7 ? C1 O1 Ag1 112.63(18) . . ? Ag1 O1 Ag1 103.48(7) 7 . ? C1 O2 Ag2 110.87(18) . 7 ? C4 O3 Ag2 102.26(17) . 7 ? C4 O3 Ag1 143.22(19) . . ? Ag2 O3 Ag1 114.25(9) 7 . ? O2 C1 O1 129.7(3) . . ? O2 C1 C2 116.2(3) . . ? O1 C1 C2 114.0(3) . . ? F1 C2 F2 106.2(3) . . ? F1 C2 C3 107.5(3) . . ? F2 C2 C3 107.0(3) . . ? F1 C2 C1 111.3(2) . . ? F2 C2 C1 110.8(3) . . ? C3 C2 C1 113.7(3) . . ? F41 C3 F3 74.7(8) . . ? F41 C3 F5 110.0(7) . . ? F3 C3 F5 118.2(6) . . ? F41 C3 F31 107.4(8) . . ? F3 C3 F31 33.7(7) . . ? F5 C3 F31 99.1(5) . . ? F41 C3 C2 120.5(6) . . ? F3 C3 C2 115.2(6) . . ? F5 C3 C2 113.2(3) . . ? F31 C3 C2 103.9(6) . . ? F41 C3 F4 28.9(8) . . ? F3 C3 F4 102.4(8) . . ? F5 C3 F4 103.4(6) . . ? F31 C3 F4 135.9(7) . . ? C2 C3 F4 101.2(6) . . ? O4 C4 O3 127.3(3) . . ? O4 C4 C5 118.3(3) . . ? O3 C4 C5 114.3(2) . . ? F7 C5 F6 107.2(3) . . ? F7 C5 C6 108.0(3) . . ? F6 C5 C6 106.5(3) . . ? F7 C5 C4 111.0(3) . . ? F6 C5 C4 110.8(2) . . ? C6 C5 C4 113.1(3) . . ? F8 C6 F9 108.0(3) . . ? F8 C6 F10 108.0(3) . . ? F9 C6 F10 107.3(3) . . ? F8 C6 C5 110.8(3) . . ? F9 C6 C5 111.6(3) . . ? F10 C6 C5 111.1(3) . . ? P11 C7 P12 111.71(15) . . ? P11 C7 H71 104(2) . . ? P12 C7 H71 108(2) . . ? P11 C7 H72 109(2) . . ? P12 C7 H72 114(2) . . ? H71 C7 H72 109(3) . . ? C16 C11 C12 118.9(3) . . ? C16 C11 P11 121.5(2) . . ? C12 C11 P11 119.3(2) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 120(2) . . ? C11 C12 H12 119(2) . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120(2) . . ? C12 C13 H13 120(2) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120(3) . . ? C13 C14 H14 120(3) . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 122(2) . . ? C16 C15 H15 118(2) . . ? C15 C16 C11 120.3(3) . . ? C15 C16 H16 120(2) . . ? C11 C16 H16 120(2) . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P11 119.3(2) . . ? C26 C21 P11 121.2(2) . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 121(2) . . ? C21 C22 H22 119(2) . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 121(2) . . ? C22 C23 H23 119(2) . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H24 117(2) . . ? C25 C24 H24 123(2) . . ? C24 C25 C26 120.7(3) . . ? C24 C25 H25 122(3) . . ? C26 C25 H25 118(3) . . ? C25 C26 C21 119.5(3) . . ? C25 C26 H26 120(2) . . ? C21 C26 H26 121(2) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P12 118.1(2) . . ? C36 C31 P12 122.8(2) . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 121(2) . . ? C31 C32 H32 119(2) . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 122(2) . . ? C32 C33 H33 118(2) . . ? C33 C34 C35 119.8(3) . . ? C33 C34 H34 121(3) . . ? C35 C34 H34 119(3) . . ? C36 C35 C34 120.3(3) . . ? C36 C35 H35 119(3) . . ? C34 C35 H35 120(3) . . ? C35 C36 C31 120.3(3) . . ? C35 C36 H36 121(2) . . ? C31 C36 H36 118(2) . . ? C46 C41 C42 119.4(3) . . ? C46 C41 P12 118.6(2) . . ? C42 C41 P12 122.0(2) . . ? C43 C42 C41 120.0(3) . . ? C43 C42 H42 119(2) . . ? C41 C42 H42 121(2) . . ? C44 C43 C42 120.1(3) . . ? C44 C43 H43 126(3) . . ? C42 C43 H43 114(3) . . ? C43 C44 C45 120.5(3) . . ? C43 C44 H44 120(3) . . ? C45 C44 H44 119(3) . . ? C44 C45 C46 120.2(3) . . ? C44 C45 H45 119(3) . . ? C46 C45 H45 121(3) . . ? C41 C46 C45 119.8(3) . . ? C41 C46 H46 121(2) . . ? C45 C46 H46 119(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 O3 Ag1 Ag2 O2 60.90(11) . . . 7 ? O1 Ag1 Ag2 O2 32.21(8) 7 . . 7 ? P11 Ag1 Ag2 O2 -116.31(6) . . . 7 ? O1 Ag1 Ag2 O2 112.16(7) . . . 7 ? O3 Ag1 Ag2 O3 -21.12(15) . . . 7 ? O1 Ag1 Ag2 O3 -49.81(8) 7 . . 7 ? P11 Ag1 Ag2 O3 161.67(6) . . . 7 ? O1 Ag1 Ag2 O3 30.13(7) . . . 7 ? O3 Ag1 Ag2 P12 -158.55(10) . . . . ? O1 Ag1 Ag2 P12 172.76(5) 7 . . . ? P11 Ag1 Ag2 P12 24.24(3) . . . . ? O1 Ag1 Ag2 P12 -107.29(5) . . . . ? O3 Ag1 P11 C21 -104.84(12) . . . . ? O1 Ag1 P11 C21 25.98(13) 7 . . . ? O1 Ag1 P11 C21 141.29(11) . . . . ? Ag2 Ag1 P11 C21 73.14(10) . . . . ? O3 Ag1 P11 C11 16.10(13) . . . . ? O1 Ag1 P11 C11 146.92(13) 7 . . . ? O1 Ag1 P11 C11 -97.77(12) . . . . ? Ag2 Ag1 P11 C11 -165.92(11) . . . . ? O3 Ag1 P11 C7 135.83(13) . . . . ? O1 Ag1 P11 C7 -93.36(13) 7 . . . ? O1 Ag1 P11 C7 21.96(13) . . . . ? Ag2 Ag1 P11 C7 -46.20(11) . . . . ? O2 Ag2 P12 C41 -164.10(13) 7 . . . ? O3 Ag2 P12 C41 10.55(14) 7 . . . ? Ag1 Ag2 P12 C41 114.36(11) . . . . ? O2 Ag2 P12 C31 -41.12(14) 7 . . . ? O3 Ag2 P12 C31 133.53(12) 7 . . . ? Ag1 Ag2 P12 C31 -122.66(10) . . . . ? O2 Ag2 P12 C7 77.65(14) 7 . . . ? O3 Ag2 P12 C7 -107.70(13) 7 . . . ? Ag1 Ag2 P12 C7 -3.88(10) . . . . ? O3 Ag1 O1 C1 -50.94(19) . . . . ? O1 Ag1 O1 C1 -133.7(2) 7 . . . ? P11 Ag1 O1 C1 84.6(2) . . . . ? Ag2 Ag1 O1 C1 154.75(19) . . . . ? O3 Ag1 O1 Ag1 82.80(8) . . . 7 ? O1 Ag1 O1 Ag1 0.0 7 . . 7 ? P11 Ag1 O1 Ag1 -141.67(5) . . . 7 ? Ag2 Ag1 O1 Ag1 -71.51(6) . . . 7 ? O1 Ag1 O3 C4 -137.2(3) 7 . . . ? P11 Ag1 O3 C4 12.1(4) . . . . ? O1 Ag1 O3 C4 145.1(3) . . . . ? Ag2 Ag1 O3 C4 -164.3(3) . . . . ? O1 Ag1 O3 Ag2 50.20(9) 7 . . 7 ? P11 Ag1 O3 Ag2 -160.55(5) . . . 7 ? O1 Ag1 O3 Ag2 -27.50(9) . . . 7 ? Ag2 Ag1 O3 Ag2 23.11(16) . . . 7 ? F41 F3 F31 C3 17(2) . . . . ? C3 F4 F41 F3 29(4) . . . . ? F31 F3 F41 F4 -57(6) . . . . ? C3 F3 F41 F4 -36(5) . . . . ? F31 F3 F41 C3 -21(3) . . . . ? Ag2 O2 C1 O1 -17.0(4) 7 . . . ? Ag2 O2 C1 C2 166.25(19) 7 . . . ? Ag1 O1 C1 O2 -31.5(4) 7 . . . ? Ag1 O1 C1 O2 92.5(3) . . . . ? Ag1 O1 C1 C2 145.28(19) 7 . . . ? Ag1 O1 C1 C2 -90.7(2) . . . . ? O2 C1 C2 F1 -141.4(3) . . . . ? O1 C1 C2 F1 41.4(4) . . . . ? O2 C1 C2 F2 -23.5(4) . . . . ? O1 C1 C2 F2 159.3(3) . . . . ? O2 C1 C2 C3 97.0(4) . . . . ? O1 C1 C2 C3 -80.2(4) . . . . ? F4 F41 C3 F3 164(2) . . . . ? F4 F41 C3 F5 -81(2) . . . . ? F3 F41 C3 F5 115.0(7) . . . . ? F4 F41 C3 F31 171.7(19) . . . . ? F3 F41 C3 F31 8.0(10) . . . . ? F4 F41 C3 C2 53(2) . . . . ? F3 F41 C3 C2 -110.5(7) . . . . ? F3 F41 C3 F4 -164(2) . . . . ? F31 F3 C3 F41 166.1(18) . . . . ? F31 F3 C3 F5 61.3(18) . . . . ? F41 F3 C3 F5 -104.8(8) . . . . ? F41 F3 C3 F31 -166.1(18) . . . . ? F31 F3 C3 C2 -77.0(16) . . . . ? F41 F3 C3 C2 116.9(8) . . . . ? F31 F3 C3 F4 174.1(15) . . . . ? F41 F3 C3 F4 8.0(10) . . . . ? F3 F31 C3 F41 -14.0(18) . . . . ? F3 F31 C3 F5 -128.5(15) . . . . ? F3 F31 C3 C2 114.7(16) . . . . ? F3 F31 C3 F4 -8(2) . . . . ? F1 C2 C3 F41 -69.6(8) . . . . ? F2 C2 C3 F41 176.7(8) . . . . ? C1 C2 C3 F41 54.1(9) . . . . ? F1 C2 C3 F3 -156.0(8) . . . . ? F2 C2 C3 F3 90.3(8) . . . . ? C1 C2 C3 F3 -32.4(9) . . . . ? F1 C2 C3 F5 63.7(5) . . . . ? F2 C2 C3 F5 -50.1(5) . . . . ? C1 C2 C3 F5 -172.7(3) . . . . ? F1 C2 C3 F31 170.2(5) . . . . ? F2 C2 C3 F31 56.4(5) . . . . ? C1 C2 C3 F31 -66.2(6) . . . . ? F1 C2 C3 F4 -46.4(7) . . . . ? F2 C2 C3 F4 -160.1(6) . . . . ? C1 C2 C3 F4 77.3(7) . . . . ? F41 F4 C3 F3 -16(2) . . . . ? F41 F4 C3 F5 107(2) . . . . ? F41 F4 C3 F31 -11(3) . . . . ? F41 F4 C3 C2 -135(2) . . . . ? Ag2 O3 C4 O4 10.0(4) 7 . . . ? Ag1 O3 C4 O4 -163.2(2) . . . . ? Ag2 O3 C4 C5 -167.6(2) 7 . . . ? Ag1 O3 C4 C5 19.3(5) . . . . ? O4 C4 C5 F7 128.3(3) . . . . ? O3 C4 C5 F7 -54.0(3) . . . . ? O4 C4 C5 F6 9.3(4) . . . . ? O3 C4 C5 F6 -173.0(3) . . . . ? O4 C4 C5 C6 -110.2(3) . . . . ? O3 C4 C5 C6 67.6(3) . . . . ? F7 C5 C6 F8 169.1(3) . . . . ? F6 C5 C6 F8 -76.0(3) . . . . ? C4 C5 C6 F8 45.9(4) . . . . ? F7 C5 C6 F9 -70.5(3) . . . . ? F6 C5 C6 F9 44.3(3) . . . . ? C4 C5 C6 F9 166.2(3) . . . . ? F7 C5 C6 F10 49.1(3) . . . . ? F6 C5 C6 F10 164.0(3) . . . . ? C4 C5 C6 F10 -74.1(3) . . . . ? C21 P11 C7 P12 -67.35(18) . . . . ? C11 P11 C7 P12 -177.41(15) . . . . ? Ag1 P11 C7 P12 55.74(17) . . . . ? C41 P12 C7 P11 -151.33(15) . . . . ? C31 P12 C7 P11 97.03(17) . . . . ? Ag2 P12 C7 P11 -26.61(18) . . . . ? C21 P11 C11 C16 22.1(3) . . . . ? C7 P11 C11 C16 131.8(3) . . . . ? Ag1 P11 C11 C16 -102.1(2) . . . . ? C21 P11 C11 C12 -163.3(2) . . . . ? C7 P11 C11 C12 -53.7(3) . . . . ? Ag1 P11 C11 C12 72.5(2) . . . . ? C16 C11 C12 C13 -1.0(5) . . . . ? P11 C11 C12 C13 -175.7(3) . . . . ? C11 C12 C13 C14 1.1(5) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C13 C14 C15 C16 -0.3(6) . . . . ? C14 C15 C16 C11 0.4(5) . . . . ? C12 C11 C16 C15 0.2(5) . . . . ? P11 C11 C16 C15 174.8(3) . . . . ? C11 P11 C21 C22 -122.1(2) . . . . ? C7 P11 C21 C22 129.9(2) . . . . ? Ag1 P11 C21 C22 4.8(3) . . . . ? C11 P11 C21 C26 57.4(3) . . . . ? C7 P11 C21 C26 -50.6(3) . . . . ? Ag1 P11 C21 C26 -175.7(2) . . . . ? C26 C21 C22 C23 -0.8(4) . . . . ? P11 C21 C22 C23 178.7(2) . . . . ? C21 C22 C23 C24 0.8(5) . . . . ? C22 C23 C24 C25 -0.4(5) . . . . ? C23 C24 C25 C26 0.1(5) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C22 C21 C26 C25 0.5(5) . . . . ? P11 C21 C26 C25 -179.0(3) . . . . ? C41 P12 C31 C32 139.8(2) . . . . ? C7 P12 C31 C32 -111.1(2) . . . . ? Ag2 P12 C31 C32 12.6(3) . . . . ? C41 P12 C31 C36 -42.3(3) . . . . ? C7 P12 C31 C36 66.7(3) . . . . ? Ag2 P12 C31 C36 -169.6(2) . . . . ? C36 C31 C32 C33 -0.4(5) . . . . ? P12 C31 C32 C33 177.5(3) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C32 C33 C34 C35 1.2(6) . . . . ? C33 C34 C35 C36 -2.2(6) . . . . ? C34 C35 C36 C31 1.9(5) . . . . ? C32 C31 C36 C35 -0.6(5) . . . . ? P12 C31 C36 C35 -178.4(3) . . . . ? C31 P12 C41 C46 -107.1(3) . . . . ? C7 P12 C41 C46 143.0(3) . . . . ? Ag2 P12 C41 C46 19.2(3) . . . . ? C31 P12 C41 C42 73.7(3) . . . . ? C7 P12 C41 C42 -36.2(3) . . . . ? Ag2 P12 C41 C42 -160.0(2) . . . . ? C46 C41 C42 C43 -0.9(5) . . . . ? P12 C41 C42 C43 178.4(3) . . . . ? C41 C42 C43 C44 -0.3(6) . . . . ? C42 C43 C44 C45 1.0(6) . . . . ? C43 C44 C45 C46 -0.6(7) . . . . ? C42 C41 C46 C45 1.3(5) . . . . ? P12 C41 C46 C45 -178.0(3) . . . . ? C44 C45 C46 C41 -0.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.473 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.473 _refine_diff_density_max 0.850 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.099