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Acta Cryst. (2008). E64, m269    [ doi:10.1107/S1600536807067311 ]

Bis[[mu]-bis(diphenylphosphino)methane-[kappa]2P:P']bis[(4-toluenesulfonato-[kappa]O)silver(I)] monohydrate

Z. Ma, J. Sun, B. Liu, M. Hu and Y. Xing

Abstract top

The title complex, [Ag2(C7H7O3S)2(C25H22P2)2]·H2O, was obtained by the reaction of silver toluenesulfonate with diphenylphosphinomethane (dppm) in acetonitrile. There are two unique half-molecules of the complex in the asymmetric unit, together with one water molecule, which is disordered over two positions with site occupancy factors of 0.6 and 0.4. In each centrosymmetric neutral dimeric molecule, two Ag atoms are bridged by a pair of dppm ligands to give an eight-membered Ag2P4C2 ring with a distorted AgOP2 trigonal-planar environment. The Ag-Ag distances of 2.9215 (9) and 3.027 (1) Å indicate a direct bonding interaction.

Comment top

There has been, in recent years, considerable interest in the study of compounds of dppm (Effendy et al., 2005; Fournier, Decken & Harvey, 2004; Forunier, Lebrun et al., 2004), since this diphosphine is a very convenient ligand to coordinate to silver ions, to form complexes with interesting structures. These compounds have attracted considerable interest because they can be used as building blocks for reactions with other chemical groups to construct complexes which often display interesting properties (Chen et al., 2004; Youm et al., 2000).

The molecules of the title complex (1) (Fig. 1) are centrosymmetric, with the two toluenesulfonate ions coordinated to two silver atoms lying trans to each other. The structure contains two crystallographically independent complex molecules.

The structure consists of a neutral dimeric molecule with two silver atoms bridged by a pair of dppm ligands to give an eight-membered Ag2P4C2 ring, similar to the structures of [Ag(dppm)(O2CCF3)]2, [Ag(dppm)(O2CCH2Ph)]2 and [Ag(dppm)(O2CCH2Ph)]2. There are several reported examples, which show similar distorted triangle structures (Effendy et al., 2005; Fournier, Decken & Harvey, 2004; Forunier, Lebrun et al., 2004; Hong et al., 1997). Each silver ion is coordinated by two phosphorus atoms from two dppm molecules and one oxygen atom from one toluenesulfonate ligand. Therefore, each silver atom is in a highly distorted AgOP2 trigonal-planar coordination environment. There is a metal-metal contact between the two silver ions in each molecule of the title complex. The distances between the two silver atoms are 2.9215 (9) Å and 3.027 (1) Å in the two molecules.

One water molecule is contained in the asymmetric unit and it is disordered over two alternative sites. This water originates from the moisture contained in the solvents, acetonitrile and diethyl ether, which were used in the synthesis. There are no hydrogen bonds between the water molecules and oxygen atoms of the toluenesulfonate ligands.

Related literature top

For similar structures, see: Chen et al. (2004); Effendy et al. (2005); Fournier, Decken & Harvey (2004); Forunier, Lebrun et al. (2004); Hong et al. (1997); Youm et al. (2000).

For related literature, see: Fournier, Decken & Harvey (2004); Fournier, Lebrun, Drouin, Decken & Harvey (2004).

Experimental top

The title compound was obtained by the reaction of silver toluenesulfonate (AgSO3C6H4CH3) and diphenylphosphinomethane (dppm) in acetonitrile. In a 50 cm3 flask fitted with a funnel, silver toluenesulfonate (1.0 g, 3.6 mmol) was dissolved in 20 cm3 of acetonitrile. To this solution was added dropwise an equimolar quantity of diphenylphosphinomethane (dppm) (1.4 g, 3.6 mmol) dissolved in 20 cm3 of acetonitrile, over a period of half an hour with stirring. The mixture was then stirred for 24 h. The solution was concentrated and the white solid formed by adding a large quantity of diethyl ether was filtered off and washed with diethyl ether (2 × 10 cm3) (yield 81%). All processes were undertaken under dinitrogen gas. Slow evaporation of an acetonitrile solution of the title complex led to the formation of colorless crystals, which were suitable for X-ray characterization.

Refinement top

All H atoms were positioned geometrically and refined using a riding model with C—H = 0.93–0.97 Å and with Uiso(H) = 1.2Ueq(C). The occupancy factors of the disordered water molecule were initially refined and then fixed. H atoms were not included for this molecule.

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear (Rigaku, 2000); data reduction: CrystalClear (Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1993); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. The structure of one molecule of the title complex, showing the atom labeling scheme and 20% probability displacement ellipsoids. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The structure of the other independent molecule of the title complex, showing the atom labeling scheme and 20% probability displacement ellipsoids. H atoms have been omitted for clarity.
Bis[µ-bis(diphenylphosphino)methane-κ2P:P']bis[(4-toluenesulfonato-\ κO)silver(I)] monohydrate top
Crystal data top
[Ag2(C7H7O3S)2(C25H22P2)2]·H2OZ = 2
Mr = 1344.86F000 = 1372
Triclinic, P1Dx = 1.490 Mg m−3
a = 11.239 (2) ÅMo Kα radiation
λ = 0.71073 Å
b = 11.802 (2) ÅCell parameters from 27870 reflections
c = 23.363 (5) Åθ = 0.9–27.5º
α = 103.86 (3)ºµ = 0.88 mm−1
β = 93.79 (3)ºT = 293 (2) K
γ = 91.95 (3)ºPrism, colorless
V = 2998.1 (10) Å30.36 × 0.31 × 0.28 mm
Data collection top
Rigaku Weissenberg IP
diffractometer		11383 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.029
Monochromator: graphiteθmax = 27.5º
T = 293(2) Kθmin = 0.9º
ω scansh = −14→14
Absorption correction: nonek = 0→15
27870 measured reflectionsl = −30→29
13424 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.131  w = 1/[σ2(Fo2) + (0.0589P)2 + 6.0201P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
13424 reflectionsΔρmax = 0.71 e Å−3
721 parametersΔρmin = −1.86 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Ag2(C7H7O3S)2(C25H22P2)2]·H2Oγ = 91.95 (3)º
Mr = 1344.86V = 2998.1 (10) Å3
Triclinic, P1Z = 2
a = 11.239 (2) ÅMo Kα
b = 11.802 (2) ŵ = 0.88 mm−1
c = 23.363 (5) ÅT = 293 (2) K
α = 103.86 (3)º0.36 × 0.31 × 0.28 mm
β = 93.79 (3)º
Data collection top
Rigaku Weissenberg IP
diffractometer		13424 independent reflections
Absorption correction: none11383 reflections with I > 2σ(I)
27870 measured reflectionsRint = 0.029
Refinement top
R[F2 > 2σ(F2)] = 0.042721 parameters
wR(F2) = 0.131H-atom parameters constrained
S = 1.05Δρmax = 0.71 e Å−3
13424 reflectionsΔρmin = −1.86 e Å−3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ag10.11622 (2)0.48402 (2)0.475474 (11)0.03703 (8)
Ag20.52075 (3)−0.12811 (4)−0.005498 (15)0.05974 (11)
S10.17891 (10)0.82300 (8)0.53039 (5)0.0482 (2)
S20.32006 (9)−0.14579 (10)0.12284 (4)0.0468 (2)
P10.20944 (7)0.48870 (7)0.57271 (4)0.02923 (16)
P20.02266 (7)0.42514 (8)0.37653 (4)0.03273 (18)
P30.33812 (8)−0.17322 (7)−0.06908 (4)0.03266 (17)
P40.72861 (7)−0.07571 (7)0.02262 (4)0.03080 (17)
O10.2033 (3)−0.1768 (3)0.09323 (16)0.0647 (9)
O20.3227 (4)−0.0401 (3)0.16896 (17)0.0817 (11)
O30.4092 (3)−0.1455 (4)0.08136 (16)0.0742 (11)
O40.2356 (3)0.8514 (3)0.58977 (13)0.0560 (7)
O50.0663 (3)0.8772 (3)0.52626 (17)0.0671 (9)
O60.1714 (4)0.6974 (3)0.50571 (16)0.0792 (12)
O70.5206 (6)−0.4429 (5)−0.0011 (4)0.088 (2)0.60
O7'0.5506 (10)−0.3613 (10)−0.0078 (6)0.089 (3)0.40
C20.3684 (3)0.5306 (3)0.58370 (14)0.0331 (7)
C60.7859 (3)−0.1123 (3)0.08989 (15)0.0333 (7)
C70.0743 (3)0.2859 (3)0.33560 (15)0.0378 (7)
C80.3349 (3)−0.1564 (3)−0.14428 (15)0.0376 (7)
C90.2753 (3)−0.3222 (3)−0.07880 (17)0.0393 (7)
C120.0512 (3)0.5273 (3)0.33133 (16)0.0383 (7)
C130.8185 (3)−0.1551 (3)−0.03427 (15)0.0357 (7)
C140.1999 (3)0.3577 (3)0.60008 (16)0.0367 (7)
C150.2273 (4)−0.1704 (4)−0.17894 (17)0.0478 (9)
H15A0.1569−0.1888−0.16360.057*
C170.8550 (4)−0.1080 (4)−0.07943 (17)0.0467 (9)
H17A0.8406−0.0307−0.07910.056*
C190.7052 (3)−0.1347 (3)0.12909 (16)0.0400 (8)
H19A0.6235−0.13710.11930.048*
C200.7485 (4)−0.1536 (4)0.18303 (18)0.0496 (9)
H20A0.6952−0.16740.20970.060*
C210.3563 (4)−0.2598 (4)0.15795 (17)0.0463 (9)
C220.2751 (4)0.8784 (3)0.48523 (18)0.0473 (9)
C230.4493 (3)0.4454 (4)0.5664 (2)0.0512 (10)
H23A0.42190.36810.55120.061*
C240.1552 (4)0.2805 (4)0.29251 (19)0.0538 (10)
H24A0.17960.34790.28160.065*
C260.9490 (4)−0.1326 (4)0.15803 (19)0.0517 (10)
H26A1.0306−0.13310.16760.062*
C270.9081 (3)−0.1125 (3)0.10436 (17)0.0417 (8)
H27A0.9622−0.09920.07790.050*
C290.8692 (4)−0.1519 (4)0.19723 (18)0.0534 (10)
H29A0.8971−0.16390.23360.064*
C300.4389 (4)−0.1289 (4)−0.16758 (18)0.0478 (9)
H30A0.5112−0.1184−0.14470.057*
C310.2081 (4)−0.3538 (4)−0.0374 (2)0.0537 (10)
H31A0.1895−0.2975−0.00440.064*
C320.0403 (4)0.1840 (4)0.3511 (2)0.0542 (10)
H32A−0.01200.18700.38060.065*
C330.0006 (4)0.5106 (4)0.27401 (18)0.0517 (10)
H33A−0.05340.44760.25830.062*
C380.4246 (4)0.9528 (4)0.4089 (2)0.0553 (10)
C390.1301 (4)0.6226 (4)0.3540 (2)0.0530 (10)
H39A0.16430.63570.39250.064*
C400.8402 (4)−0.2709 (4)−0.0359 (2)0.0565 (11)
H40A0.8163−0.3039−0.00590.068*
C410.1347 (4)0.2598 (3)0.5671 (2)0.0506 (9)
H41A0.09560.26100.53090.061*
C420.9330 (5)−0.2888 (4)−0.1265 (2)0.0646 (13)
H42A0.9712−0.3339−0.15760.078*
C430.3292 (6)−0.3750 (5)0.1302 (2)0.0782 (16)
H43A0.2921−0.39460.09210.094*
C450.4113 (3)0.6444 (4)0.6055 (2)0.0571 (12)
H45A0.35860.70350.61630.069*
C460.2370 (4)0.9589 (5)0.4548 (2)0.0614 (12)
H46A0.16140.98810.45920.074*
C480.0302 (5)0.5871 (5)0.2401 (2)0.0638 (12)
H48A−0.00400.57500.20160.077*
C490.3296 (5)−0.1306 (4)−0.25938 (19)0.0649 (13)
H49A0.3280−0.1222−0.29800.078*
C500.9128 (4)−0.1759 (4)−0.12514 (19)0.0577 (11)
H50A0.9380−0.1435−0.15510.069*
C510.2566 (4)0.3543 (4)0.6541 (2)0.0566 (11)
H51A0.29930.42030.67720.068*
C530.4351 (5)−0.1169 (5)−0.2258 (2)0.0630 (12)
H53A0.5052−0.0994−0.24160.076*
C540.8970 (5)−0.3371 (4)−0.0820 (3)0.0697 (14)
H54A0.9111−0.4147−0.08300.084*
C550.2253 (5)−0.1568 (4)−0.23639 (19)0.0595 (11)
H55A0.1533−0.1655−0.25940.071*
C560.1858 (5)0.1565 (4)0.6406 (3)0.0690 (14)
H56A0.18190.08850.65390.083*
C570.1992 (5)0.1740 (5)0.2660 (2)0.0671 (14)
H57A0.25450.17070.23790.081*
C580.6119 (4)0.5862 (5)0.5946 (2)0.0620 (12)
H58A0.69350.60510.59920.074*
C590.5332 (4)0.6708 (4)0.6112 (3)0.0713 (15)
H59A0.56180.74770.62660.086*
C600.1949 (6)−0.5531 (4)−0.0928 (3)0.0740 (15)
H60A0.1672−0.6303−0.09790.089*
C610.2631 (7)−0.5224 (4)−0.1333 (3)0.092 (2)
H61A0.2832−0.5794−0.16570.110*
C620.1624 (5)0.0729 (5)0.2808 (2)0.0672 (14)
H62A0.19130.00160.26210.081*
C640.3126 (5)0.9959 (5)0.4174 (2)0.0660 (13)
H64A0.28721.05140.39750.079*
C660.3889 (5)0.8387 (4)0.4794 (2)0.0590 (11)
H66A0.41630.78730.50140.071*
C670.5707 (4)0.4744 (5)0.5714 (2)0.0624 (12)
H67A0.62420.41680.55890.075*
C680.1278 (5)0.1597 (4)0.5881 (3)0.0678 (13)
H68A0.08300.09410.56610.081*
C700.1094 (5)0.6806 (5)0.2626 (3)0.0705 (14)
H70A0.12960.73130.23940.085*
C730.1676 (5)−0.4697 (4)−0.0447 (3)0.0663 (13)
H73A0.1219−0.4903−0.01670.080*
C780.4108 (5)−0.2348 (5)0.2141 (2)0.0680 (13)
H78A0.4303−0.15740.23370.082*
C810.4107 (5)−0.4374 (5)0.2148 (3)0.0704 (14)
C830.0827 (5)0.0782 (4)0.3233 (3)0.0674 (13)
H83A0.05730.01020.33350.081*
C840.1582 (5)0.6988 (5)0.3191 (3)0.0723 (14)
H84A0.21100.76280.33460.087*
C850.4626 (5)0.8747 (4)0.4412 (2)0.0632 (12)
H85A0.53850.84610.43720.076*
C870.3025 (6)−0.4082 (4)−0.1268 (2)0.0752 (16)
H87A0.3481−0.3887−0.15510.090*
C880.2498 (5)0.2531 (5)0.6737 (3)0.0716 (14)
H88A0.28910.25060.70960.086*
C900.4370 (6)−0.3222 (6)0.2419 (3)0.0800 (17)
H90A0.4736−0.30250.28010.096*
C960.1402 (3)0.5998 (3)0.62743 (14)0.0318 (6)
H96A0.15890.67630.62090.038*
H96B0.17350.59900.66670.038*
C970.7757 (3)0.0787 (3)0.03314 (15)0.0337 (7)
H97A0.78830.0948−0.00490.040*
H97B0.85070.09540.05730.040*
C980.5038 (5)0.9900 (5)0.3662 (2)0.0739 (15)
H98A0.57680.95000.36560.111*
H98B0.52141.07280.37860.111*
H98C0.46360.97090.32730.111*
C990.4362 (7)−0.5352 (7)0.2452 (4)0.107 (2)
H99A0.4112−0.60900.21870.161*
H99B0.3933−0.52440.28010.161*
H99C0.5203−0.53400.25590.161*
C1010.3570 (7)−0.4622 (5)0.1587 (3)0.0879 (19)
H10A0.3385−0.53980.13910.105*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.02949 (13)0.05165 (17)0.02728 (12)0.00223 (10)−0.00020 (9)0.00493 (10)
Ag20.03214 (16)0.1020 (3)0.04636 (18)−0.00563 (16)−0.00490 (12)0.02374 (18)
S10.0611 (6)0.0363 (5)0.0468 (5)−0.0101 (4)−0.0032 (4)0.0132 (4)
S20.0446 (5)0.0581 (6)0.0402 (5)0.0047 (4)0.0103 (4)0.0144 (4)
P10.0275 (4)0.0300 (4)0.0289 (4)0.0025 (3)−0.0004 (3)0.0051 (3)
P20.0282 (4)0.0415 (5)0.0263 (4)0.0019 (3)0.0013 (3)0.0040 (3)
P30.0328 (4)0.0324 (4)0.0320 (4)0.0027 (3)0.0011 (3)0.0065 (3)
P40.0304 (4)0.0321 (4)0.0316 (4)0.0038 (3)0.0027 (3)0.0107 (3)
O10.0455 (17)0.080 (2)0.073 (2)0.0070 (15)0.0001 (15)0.0274 (18)
O20.116 (3)0.062 (2)0.061 (2)0.013 (2)0.005 (2)0.0021 (17)
O30.0556 (19)0.117 (3)0.068 (2)0.0161 (19)0.0280 (17)0.050 (2)
O40.0642 (19)0.0592 (18)0.0449 (15)−0.0055 (14)−0.0003 (14)0.0153 (13)
O50.0529 (18)0.073 (2)0.084 (2)−0.0070 (16)−0.0007 (17)0.0381 (19)
O60.130 (3)0.0410 (17)0.064 (2)−0.0213 (19)0.004 (2)0.0114 (15)
O70.067 (4)0.050 (3)0.160 (7)0.009 (3)−0.008 (4)0.053 (4)
O7'0.082 (7)0.069 (7)0.118 (9)0.015 (5)−0.014 (6)0.030 (6)
C20.0264 (15)0.0412 (18)0.0313 (15)0.0033 (12)0.0000 (12)0.0085 (13)
C60.0345 (16)0.0326 (16)0.0344 (16)0.0028 (12)0.0027 (13)0.0113 (13)
C70.0299 (16)0.048 (2)0.0319 (16)0.0082 (14)−0.0004 (13)0.0017 (14)
C80.0439 (19)0.0366 (18)0.0310 (16)0.0032 (14)0.0050 (14)0.0050 (13)
C90.0424 (19)0.0316 (17)0.0433 (19)0.0044 (14)−0.0026 (15)0.0089 (14)
C120.0389 (18)0.0421 (19)0.0348 (17)0.0054 (14)0.0071 (14)0.0094 (14)
C130.0320 (16)0.0399 (18)0.0337 (16)0.0027 (13)0.0000 (13)0.0066 (14)
C140.0344 (17)0.0363 (17)0.0409 (18)0.0047 (13)0.0044 (14)0.0112 (14)
C150.048 (2)0.054 (2)0.0384 (19)−0.0008 (17)−0.0033 (16)0.0061 (17)
C170.054 (2)0.046 (2)0.042 (2)0.0077 (17)0.0102 (17)0.0110 (16)
C190.0395 (18)0.0420 (19)0.0430 (19)0.0068 (14)0.0072 (15)0.0174 (15)
C200.058 (2)0.057 (2)0.041 (2)0.0102 (19)0.0128 (18)0.0231 (18)
C210.045 (2)0.058 (2)0.0385 (19)0.0019 (17)0.0085 (15)0.0154 (17)
C220.062 (2)0.0354 (19)0.045 (2)−0.0049 (17)−0.0005 (18)0.0123 (16)
C230.0357 (19)0.043 (2)0.069 (3)0.0072 (15)0.0046 (18)0.0010 (19)
C240.048 (2)0.065 (3)0.047 (2)0.0126 (19)0.0138 (18)0.0066 (19)
C260.041 (2)0.062 (3)0.052 (2)0.0079 (18)−0.0085 (17)0.018 (2)
C270.0354 (18)0.049 (2)0.0443 (19)0.0025 (15)0.0019 (15)0.0177 (16)
C290.066 (3)0.059 (3)0.038 (2)0.013 (2)−0.0041 (18)0.0182 (18)
C300.048 (2)0.052 (2)0.044 (2)0.0070 (17)0.0105 (17)0.0117 (17)
C310.065 (3)0.039 (2)0.058 (2)0.0033 (18)0.011 (2)0.0123 (18)
C320.046 (2)0.057 (3)0.061 (3)0.0145 (18)0.0103 (19)0.015 (2)
C330.054 (2)0.061 (3)0.039 (2)0.0014 (19)0.0009 (17)0.0129 (18)
C380.066 (3)0.048 (2)0.050 (2)−0.011 (2)0.002 (2)0.0095 (18)
C390.054 (2)0.055 (2)0.049 (2)−0.0085 (19)0.0034 (18)0.0128 (19)
C400.075 (3)0.039 (2)0.059 (3)0.0149 (19)0.021 (2)0.0144 (18)
C410.054 (2)0.037 (2)0.057 (2)−0.0024 (17)−0.0037 (19)0.0087 (17)
C420.067 (3)0.061 (3)0.055 (3)0.003 (2)0.020 (2)−0.011 (2)
C430.111 (5)0.067 (3)0.053 (3)−0.006 (3)−0.012 (3)0.015 (2)
C450.0327 (19)0.040 (2)0.088 (3)0.0046 (15)0.0014 (19)−0.006 (2)
C460.053 (3)0.071 (3)0.069 (3)−0.001 (2)0.001 (2)0.037 (2)
C480.073 (3)0.081 (3)0.044 (2)0.015 (3)0.008 (2)0.027 (2)
C490.101 (4)0.060 (3)0.033 (2)0.009 (3)0.008 (2)0.0095 (19)
C500.064 (3)0.069 (3)0.040 (2)0.005 (2)0.0167 (19)0.008 (2)
C510.068 (3)0.056 (3)0.049 (2)−0.005 (2)−0.008 (2)0.024 (2)
C530.075 (3)0.070 (3)0.047 (2)0.009 (2)0.022 (2)0.016 (2)
C540.087 (4)0.041 (2)0.079 (3)0.014 (2)0.022 (3)0.006 (2)
C550.074 (3)0.061 (3)0.038 (2)0.003 (2)−0.012 (2)0.0054 (19)
C560.075 (3)0.055 (3)0.092 (4)0.012 (2)0.024 (3)0.042 (3)
C570.065 (3)0.086 (4)0.048 (2)0.030 (3)0.017 (2)0.002 (2)
C580.0260 (18)0.084 (3)0.069 (3)0.0000 (19)0.0031 (18)0.005 (2)
C590.040 (2)0.053 (3)0.106 (4)−0.0103 (19)0.001 (2)−0.007 (3)
C600.104 (4)0.032 (2)0.084 (4)−0.005 (2)−0.009 (3)0.015 (2)
C610.161 (7)0.030 (2)0.078 (4)0.000 (3)0.026 (4)0.000 (2)
C620.065 (3)0.067 (3)0.059 (3)0.029 (2)−0.005 (2)−0.006 (2)
C640.069 (3)0.070 (3)0.070 (3)−0.010 (2)−0.007 (2)0.041 (3)
C660.075 (3)0.046 (2)0.060 (3)0.009 (2)0.009 (2)0.019 (2)
C670.034 (2)0.070 (3)0.077 (3)0.0134 (19)0.008 (2)0.003 (2)
C680.075 (3)0.036 (2)0.092 (4)−0.004 (2)0.010 (3)0.014 (2)
C700.077 (3)0.071 (3)0.076 (3)0.011 (3)0.022 (3)0.038 (3)
C730.077 (3)0.047 (3)0.082 (3)−0.003 (2)0.012 (3)0.028 (2)
C780.072 (3)0.074 (3)0.055 (3)−0.008 (3)−0.014 (2)0.017 (2)
C810.068 (3)0.078 (4)0.077 (3)0.006 (3)0.008 (3)0.041 (3)
C830.061 (3)0.054 (3)0.086 (4)0.017 (2)0.004 (3)0.014 (2)
C840.077 (3)0.066 (3)0.078 (4)−0.014 (3)0.013 (3)0.026 (3)
C850.074 (3)0.048 (2)0.070 (3)0.010 (2)0.016 (2)0.015 (2)
C870.115 (5)0.044 (2)0.066 (3)0.005 (3)0.035 (3)0.005 (2)
C880.083 (4)0.075 (3)0.070 (3)0.001 (3)−0.001 (3)0.046 (3)
C900.083 (4)0.105 (5)0.058 (3)−0.005 (3)−0.012 (3)0.038 (3)
C960.0271 (15)0.0364 (17)0.0297 (15)0.0019 (12)0.0007 (12)0.0042 (12)
C970.0359 (17)0.0314 (16)0.0344 (16)0.0023 (12)0.0045 (13)0.0088 (13)
C980.085 (4)0.072 (3)0.064 (3)−0.018 (3)0.011 (3)0.016 (3)
C990.115 (6)0.107 (5)0.122 (6)0.010 (4)0.008 (5)0.073 (5)
C1010.122 (5)0.060 (3)0.083 (4)−0.006 (3)−0.004 (4)0.024 (3)
Geometric parameters (Å, °) top
Ag1—P22.4067 (11)C38—C851.385 (7)
Ag1—P12.4255 (11)C38—C981.510 (7)
Ag1—O62.491 (3)C39—C841.392 (7)
Ag1—Ag1i2.9215 (9)C39—H39A0.930
Ag2—P42.4033 (11)C40—C541.378 (6)
Ag2—P32.4181 (12)C40—H40A0.930
Ag2—O32.500 (3)C41—C681.384 (6)
Ag2—Ag2ii3.0278 (11)C41—H41A0.930
S1—O51.445 (4)C42—C501.353 (7)
S1—O41.446 (3)C42—C541.376 (8)
S1—O61.454 (3)C42—H42A0.930
S1—C221.773 (4)C43—C1011.387 (8)
S2—O11.436 (3)C43—H43A0.930
S2—O21.438 (4)C45—C591.386 (6)
S2—O31.439 (3)C45—H45A0.930
S2—C211.781 (4)C46—C641.390 (7)
P1—C141.812 (4)C46—H46A0.930
P1—C21.823 (3)C48—C701.371 (8)
P1—C961.832 (3)C48—H48A0.930
P2—C121.817 (4)C49—C531.360 (7)
P2—C71.827 (4)C49—C551.378 (8)
P2—C96i1.837 (3)C49—H49A0.930
P3—C81.813 (4)C50—H50A0.930
P3—C91.828 (4)C51—C881.379 (6)
P3—C97ii1.837 (3)C51—H51A0.930
P4—C61.811 (3)C53—H53A0.930
P4—C131.820 (4)C54—H54A0.930
P4—C971.835 (3)C55—H55A0.930
O7—O7'1.060 (12)C56—C681.360 (8)
O7—O7iii1.423 (12)C56—C881.365 (8)
C2—C451.375 (5)C56—H56A0.930
C2—C231.384 (5)C57—C621.376 (8)
C6—C191.393 (5)C57—H57A0.930
C6—C271.393 (5)C58—C671.354 (7)
C7—C321.385 (6)C58—C591.359 (7)
C7—C241.393 (5)C58—H58A0.930
C8—C301.383 (5)C59—H59A0.930
C8—C151.392 (5)C60—C611.360 (9)
C9—C311.377 (6)C60—C731.365 (8)
C9—C871.379 (6)C60—H60A0.930
C12—C391.385 (5)C61—C871.374 (7)
C12—C331.386 (5)C61—H61A0.930
C13—C171.383 (5)C62—C831.374 (8)
C13—C401.388 (5)C62—H62A0.930
C14—C411.381 (5)C64—H64A0.930
C14—C511.386 (5)C66—C851.386 (7)
C15—C551.388 (6)C66—H66A0.930
C15—H15A0.930C67—H67A0.930
C17—C501.387 (6)C68—H68A0.930
C17—H17A0.930C70—C841.361 (8)
C19—C201.391 (5)C70—H70A0.930
C19—H19A0.930C73—H73A0.930
C20—C291.374 (6)C78—C901.375 (8)
C20—H20A0.930C78—H78A0.930
C21—C781.370 (6)C81—C1011.367 (8)
C21—C431.373 (7)C81—C901.369 (8)
C22—C461.380 (6)C81—C991.518 (8)
C22—C661.381 (7)C83—H83A0.930
C23—C671.386 (6)C84—H84A0.930
C23—H23A0.930C85—H85A0.930
C24—C571.384 (6)C87—H87A0.930
C24—H24A0.930C88—H88A0.930
C26—C291.374 (6)C90—H90A0.930
C26—C271.383 (5)C96—P2i1.837 (3)
C26—H26A0.930C96—H96A0.970
C27—H27A0.930C96—H96B0.970
C29—H29A0.930C97—P3ii1.837 (3)
C30—C531.399 (6)C97—H97A0.970
C30—H30A0.930C97—H97B0.970
C31—C731.394 (6)C98—H98A0.960
C31—H31A0.930C98—H98B0.960
C32—C831.379 (6)C98—H98C0.960
C32—H32A0.930C99—H99A0.960
C33—C481.382 (6)C99—H99B0.960
C33—H33A0.930C99—H99C0.960
C38—C641.382 (7)C101—H10A0.930
P2—Ag1—P1164.99 (3)C13—C40—H40A119.9
P2—Ag1—O6112.29 (10)C14—C41—C68119.7 (4)
P1—Ag1—O682.57 (10)C14—C41—H41A120.1
P2—Ag1—Ag1i91.08 (3)C68—C41—H41A120.1
P1—Ag1—Ag1i90.23 (3)C50—C42—C54120.0 (4)
O6—Ag1—Ag1i92.55 (11)C50—C42—H42A120.0
P4—Ag2—P3158.11 (3)C54—C42—H42A120.0
P4—Ag2—O3111.55 (9)C21—C43—C101120.3 (5)
P3—Ag2—O390.29 (9)C21—C43—H43A119.8
P4—Ag2—Ag2ii88.54 (4)C101—C43—H43A119.8
P3—Ag2—Ag2ii87.92 (4)C2—C45—C59119.8 (4)
O3—Ag2—Ag2ii95.78 (10)C2—C45—H45A120.1
O5—S1—O4112.8 (2)C59—C45—H45A120.1
O5—S1—O6113.6 (2)C22—C46—C64119.3 (5)
O4—S1—O6110.8 (2)C22—C46—H46A120.3
O5—S1—C22107.0 (2)C64—C46—H46A120.3
O4—S1—C22107.45 (19)C70—C48—C33120.7 (5)
O6—S1—C22104.5 (2)C70—C48—H48A119.7
O1—S2—O2112.5 (2)C33—C48—H48A119.7
O1—S2—O3111.5 (2)C53—C49—C55120.2 (4)
O2—S2—O3113.8 (3)C53—C49—H49A119.9
O1—S2—C21106.5 (2)C55—C49—H49A119.9
O2—S2—C21106.5 (2)C42—C50—C17120.7 (4)
O3—S2—C21105.5 (2)C42—C50—H50A119.7
C14—P1—C2103.14 (16)C17—C50—H50A119.7
C14—P1—C96104.78 (16)C88—C51—C14119.9 (4)
C2—P1—C96104.75 (15)C88—C51—H51A120.1
C14—P1—Ag1118.76 (12)C14—C51—H51A120.1
C2—P1—Ag1115.51 (11)C49—C53—C30120.6 (5)
C96—P1—Ag1108.56 (11)C49—C53—H53A119.7
C12—P2—C7105.20 (17)C30—C53—H53A119.7
C12—P2—C96i106.36 (16)C42—C54—C40120.3 (5)
C7—P2—C96i103.85 (16)C42—C54—H54A119.8
C12—P2—Ag1114.08 (12)C40—C54—H54A119.8
C7—P2—Ag1112.04 (12)C49—C55—C15120.2 (4)
C96i—P2—Ag1114.38 (11)C49—C55—H55A119.9
C8—P3—C9102.78 (17)C15—C55—H55A119.9
C8—P3—C97ii105.92 (16)C68—C56—C88120.1 (4)
C9—P3—C97ii104.90 (16)C68—C56—H56A119.9
C8—P3—Ag2120.08 (13)C88—C56—H56A119.9
C9—P3—Ag2114.48 (12)C62—C57—C24121.1 (5)
C97ii—P3—Ag2107.44 (11)C62—C57—H57A119.5
C6—P4—C13104.61 (16)C24—C57—H57A119.5
C6—P4—C97104.25 (16)C67—C58—C59119.6 (4)
C13—P4—C97105.29 (16)C67—C58—H58A120.2
C6—P4—Ag2115.22 (11)C59—C58—H58A120.2
C13—P4—Ag2109.60 (11)C58—C59—C45121.1 (4)
C97—P4—Ag2116.76 (12)C58—C59—H59A119.4
S2—O3—Ag2165.2 (2)C45—C59—H59A119.4
S1—O6—Ag1167.0 (3)C61—C60—C73119.4 (4)
O7'—O7—O7iii173.8 (14)C61—C60—H60A120.3
C45—C2—C23118.5 (3)C73—C60—H60A120.3
C45—C2—P1122.7 (3)C60—C61—C87120.7 (5)
C23—C2—P1118.7 (3)C60—C61—H61A119.6
C19—C6—C27119.8 (3)C87—C61—H61A119.6
C19—C6—P4118.7 (3)C83—C62—C57119.4 (5)
C27—C6—P4121.4 (3)C83—C62—H62A120.3
C32—C7—C24118.8 (4)C57—C62—H62A120.3
C32—C7—P2119.4 (3)C38—C64—C46121.9 (4)
C24—C7—P2121.6 (3)C38—C64—H64A119.1
C30—C8—C15119.4 (4)C46—C64—H64A119.1
C30—C8—P3120.4 (3)C22—C66—C85120.5 (4)
C15—C8—P3120.2 (3)C22—C66—H66A119.7
C31—C9—C87118.2 (4)C85—C66—H66A119.7
C31—C9—P3122.1 (3)C58—C67—C23120.3 (4)
C87—C9—P3119.6 (3)C58—C67—H67A119.9
C39—C12—C33118.8 (4)C23—C67—H67A119.9
C39—C12—P2118.9 (3)C56—C68—C41120.6 (5)
C33—C12—P2122.3 (3)C56—C68—H68A119.7
C17—C13—C40118.9 (4)C41—C68—H68A119.7
C17—C13—P4122.0 (3)C84—C70—C48119.5 (5)
C40—C13—P4118.7 (3)C84—C70—H70A120.2
C41—C14—C51119.3 (4)C48—C70—H70A120.2
C41—C14—P1119.9 (3)C60—C73—C31120.3 (5)
C51—C14—P1120.8 (3)C60—C73—H73A119.8
C55—C15—C8119.9 (4)C31—C73—H73A119.8
C55—C15—H15A120.0C21—C78—C90121.2 (5)
C8—C15—H15A120.0C21—C78—H78A119.4
C13—C17—C50120.0 (4)C90—C78—H78A119.4
C13—C17—H17A120.0C101—C81—C90117.2 (5)
C50—C17—H17A120.0C101—C81—C99120.2 (6)
C20—C19—C6119.2 (4)C90—C81—C99122.6 (6)
C20—C19—H19A120.4C62—C83—C32120.1 (5)
C6—C19—H19A120.4C62—C83—H83A119.9
C29—C20—C19120.6 (4)C32—C83—H83A119.9
C29—C20—H20A119.7C70—C84—C39120.8 (5)
C19—C20—H20A119.7C70—C84—H84A119.6
C78—C21—C43117.9 (5)C39—C84—H84A119.6
C78—C21—S2120.8 (4)C38—C85—C66120.8 (5)
C43—C21—S2121.3 (4)C38—C85—H85A119.6
C46—C22—C66119.5 (4)C66—C85—H85A119.6
C46—C22—S1120.9 (4)C61—C87—C9120.9 (5)
C66—C22—S1119.6 (3)C61—C87—H87A119.5
C2—C23—C67120.6 (4)C9—C87—H87A119.5
C2—C23—H23A119.7C56—C88—C51120.4 (5)
C67—C23—H23A119.7C56—C88—H88A119.8
C57—C24—C7119.5 (5)C51—C88—H88A119.8
C57—C24—H24A120.2C81—C90—C78121.6 (5)
C7—C24—H24A120.2C81—C90—H90A119.2
C29—C26—C27120.1 (4)C78—C90—H90A119.2
C29—C26—H26A119.9P1—C96—P2i112.06 (17)
C27—C26—H26A119.9P1—C96—H96A109.2
C26—C27—C6120.0 (4)P2i—C96—H96A109.2
C26—C27—H27A120.0P1—C96—H96B109.2
C6—C27—H27A120.0P2i—C96—H96B109.2
C20—C29—C26120.4 (4)H96A—C96—H96B107.9
C20—C29—H29A119.8P4—C97—P3ii110.50 (18)
C26—C29—H29A119.8P4—C97—H97A109.6
C8—C30—C53119.7 (4)P3ii—C97—H97A109.6
C8—C30—H30A120.2P4—C97—H97B109.6
C53—C30—H30A120.2P3ii—C97—H97B109.6
C9—C31—C73120.4 (4)H97A—C97—H97B108.1
C9—C31—H31A119.8C38—C98—H98A