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The μ3-SH dicapped trisilver compound [Ag3(μ-dppm)33-SH)2]SbF6·2CH2Cl2 [dppm is bis­(di­phenyl­phosphino)­methane, C25H22P2], formed by the reaction between [Ag2(μ-dppm)2(MeCN)2](SbF6)2 and [Pd(phen)(tdt)] (phen is o-phenanthroline and tdt is toluene-3,4-­di­thiol­ate) through the disruption of C—S bonds, exhibits a trigonal bipyramid core, with two μ3-SH ligands at the apices. The Ag atoms are located in tetrahedral environments with P2S2 donors.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803009668/na6228sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803009668/na6228Isup2.hkl
Contains datablock I

CCDC reference: 214773

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.019 Å
  • R factor = 0.080
  • wR factor = 0.210
  • Data-to-parameter ratio = 17.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_420 Alert C D-H Without Acceptor S1 - H6A ? PLAT_420 Alert C D-H Without Acceptor S2 - H6B ? PLAT_731 Alert C Bond Calc 1.726(19), Rep 1.726(5) .... 3.80 su-Ratio C4 -CL02 1.555 1.555 PLAT_731 Alert C Bond Calc 1.72(2), Rep 1.720(5) .... 4.00 su-Ratio C5 -CL03 1.555 1.555 PLAT_731 Alert C Bond Calc 1.72(2), Rep 1.721(5) .... 4.00 su-Ratio C5 -CL04 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check

Comment top

There is considerable interest in designing novel metal complexes with mixed phosphorus- and sulfur-containing ligands owing to their unique optical and optoelectronic properties (Yam et al., 2000; Tang et al., 2002). It is well known that S2− and SH as versatile coordination groups could exhibit various bonding modes to produce metal cluster complexes with diverse structural topologies (Kitagawa et al., 1990; Su et al., 1998). Here we reported the crystal structure of a trisilver complex, [Ag3(µ-dppm)33-S)2]SbF6, (I), which resulted from the self-assembly between the metal components [Pd(phen)(tdt)] (phen is phenanthroline and tdt is 3,4-toluenedithiolate) and [Ag22-dppm)2(MeCN)4](SbF6)2 through the disruption of C—S of tdt.

A perspective drawing of the complex cation with the atomic numbering scheme is depicted in Fig. 1 and selected bonding parameters are presented in Table 1. The complex consists of the coordination [Ag3(µ-dppm)33-S)2]+ cation, an SbF6 anion and dichloromethane solvent molecules. The µ3-SH dicapped trisilver complex exhibits a trigonal bipyramid coordination core, with two µ3-SH ligands in the apices and the three Ag atoms in equatorial sites. The Ag atoms are located at distorted tetrahedral environments with a P2S2 chromophore. The Ag—Ag distances are in the range of 3.337 (1)–3.477 (1) Å, which are shorter than the sum of van der Waals radii for two Ag atoms, indicating a weak metal–metal contact that is operative in the complex. The Ag—S distances are in the range 2.661 (3)–2.825 (3) Å and the Ag—P bond distances are in the range 2.465 (2)–2.491 (3) Å, close to those found in other similar complexes of silver (Albano et al., 1999; Meyer et al., 1989; Lang et al., 1993; Henkel et al., 1988).

Experimental top

The title compound was isolated by the reaction between [Ag22-dppm)2(MeCN)4](SbF6)2 (Diez et al., 1987) and [Pd(phen)(tdt)] (Scott & Richard, 1996) in an equimolar ratio in dichloromethane under anaerobic condition for 12 h. Well shaped pale yellow crystals suitable for X-ray diffraction study were grown by slow diffusion of diethyl ether into a dichloromethane solution at room temperature.

Refinement top

All H atoms were included in calculated positions, with C—H distances of 0.93 (sp2) and 0.97 Å (sp3), and H–S distances of 1.20 Å. They were included in the refinement in riding motion approximation with Uiso = 1.2Ueq (1.5Ueq for sp3) of the carrier atom.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level.
(I) top
Crystal data top
[Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2F(000) = 3880
Mr = 1948.45Dx = 1.597 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8192 reflections
a = 16.0813 (1) Åθ = 1.3–25.0°
b = 18.0049 (2) ŵ = 1.40 mm1
c = 28.1089 (3) ÅT = 293 K
β = 95.417 (1)°Prism, pale yellow
V = 8102.36 (13) Å30.72 × 0.60 × 0.46 mm
Z = 4
Data collection top
Siemens SMART CCD
diffractometer
14088 independent reflections
Radiation source: fine-focus sealed tube10084 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.047
ω scansθmax = 25.0°, θmin = 1.3°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 1019
Tmin = 0.354, Tmax = 0.525k = 1321
25151 measured reflectionsl = 3332
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.080Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.210H-atom parameters constrained
S = 1.21 w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P]
where P = (Fo2 + 2Fc2)/3
14088 reflections(Δ/σ)max = 0.006
807 parametersΔρmax = 1.50 e Å3
4 restraintsΔρmin = 1.23 e Å3
Crystal data top
[Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2V = 8102.36 (13) Å3
Mr = 1948.45Z = 4
Monoclinic, P21/nMo Kα radiation
a = 16.0813 (1) ŵ = 1.40 mm1
b = 18.0049 (2) ÅT = 293 K
c = 28.1089 (3) Å0.72 × 0.60 × 0.46 mm
β = 95.417 (1)°
Data collection top
Siemens SMART CCD
diffractometer
14088 independent reflections
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
10084 reflections with I > 2σ(I)
Tmin = 0.354, Tmax = 0.525Rint = 0.047
25151 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0804 restraints
wR(F2) = 0.210H-atom parameters constrained
S = 1.21 w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P]
where P = (Fo2 + 2Fc2)/3
14088 reflectionsΔρmax = 1.50 e Å3
807 parametersΔρmin = 1.23 e Å3
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*/Ueq
Sb0.43562 (5)0.77857 (6)0.55439 (3)0.0669 (3)
Ag10.85356 (5)0.82543 (5)0.75823 (3)0.0451 (2)
Ag20.95905 (5)0.82429 (5)0.66155 (3)0.0502 (2)
Ag31.06476 (5)0.78051 (5)0.77001 (3)0.0504 (2)
S10.93674 (15)0.70518 (14)0.72450 (9)0.0439 (6)
H6A0.92050.64050.71920.053*
S20.98644 (16)0.91081 (14)0.73817 (9)0.0459 (6)
H6B1.00320.97540.74360.055*
P10.86185 (14)0.82298 (15)0.84624 (8)0.0375 (5)
P20.72572 (15)0.81252 (14)0.70314 (8)0.0378 (5)
P30.82164 (16)0.83775 (16)0.61517 (9)0.0431 (6)
P41.09318 (15)0.80107 (15)0.62814 (9)0.0399 (6)
P51.19248 (15)0.77796 (15)0.72685 (9)0.0395 (6)
P61.04429 (15)0.75885 (15)0.85566 (9)0.0398 (6)
C10.9362 (5)0.7533 (6)0.8724 (3)0.041 (2)
H1A0.91440.70450.86360.050*
H1B0.93820.75720.90700.050*
C20.7399 (6)0.7836 (5)0.6414 (3)0.039 (2)
H2A0.75470.73140.64130.047*
H2B0.68750.78960.62170.047*
C31.1890 (6)0.8241 (6)0.6673 (3)0.043 (2)
H3A1.19180.87750.67180.051*
H3B1.23750.80910.65160.051*
C41.0629 (19)1.0853 (8)0.6681 (7)0.234 (15)*
H4A1.08911.06340.69720.281*
H4B1.00421.09260.67230.281*
C51.1936 (11)0.5080 (14)0.4072 (7)0.190 (11)*
H5A1.24150.48440.42450.228*
H5B1.21260.55420.39420.228*
C1110.8910 (6)0.9090 (6)0.8772 (4)0.048 (2)
C1120.8949 (8)0.9738 (7)0.8509 (4)0.064 (3)
H11B0.88380.97230.81790.077*
C1130.9155 (10)1.0416 (8)0.8735 (6)0.090 (5)
H11E0.91921.08460.85550.108*
C1140.9304 (10)1.0443 (9)0.9230 (6)0.091 (5)
H11D0.94411.08910.93820.109*
C1150.9250 (9)0.9810 (8)0.9491 (5)0.075 (4)
H11C0.93370.98290.98230.091*
C1160.9065 (7)0.9141 (7)0.9268 (4)0.062 (3)
H11A0.90440.87130.94520.075*
C1210.7649 (6)0.7946 (6)0.8712 (4)0.045 (2)
C1220.7619 (7)0.7718 (7)0.9189 (4)0.060 (3)
H12A0.81070.77010.93950.072*
C1230.6869 (7)0.7519 (8)0.9353 (5)0.074 (4)
H12D0.68570.73640.96680.088*
C1240.6142 (8)0.7547 (9)0.9060 (5)0.081 (4)
H12E0.56400.74130.91750.097*
C1250.6157 (7)0.7773 (8)0.8597 (5)0.073 (4)
H12C0.56630.77930.83970.088*
C1260.6903 (6)0.7973 (7)0.8425 (4)0.058 (3)
H12B0.69020.81290.81100.069*
C2110.6545 (6)0.8904 (5)0.6991 (3)0.040 (2)
C2120.6682 (7)0.9479 (7)0.7316 (4)0.061 (3)
H21B0.71410.94530.75430.073*
C2130.6155 (9)1.0098 (7)0.7314 (6)0.080 (4)
H21D0.62601.04760.75370.096*
C2140.5482 (10)1.0133 (8)0.6978 (6)0.085 (5)
H21C0.51361.05480.69670.102*
C2150.5312 (9)0.9569 (9)0.6659 (5)0.085 (4)
H21E0.48350.95860.64450.102*
C2160.5856 (7)0.8971 (7)0.6658 (4)0.066 (3)
H21A0.57550.86030.64270.079*
C2210.6650 (6)0.7331 (5)0.7222 (3)0.038 (2)
C2220.7083 (7)0.6687 (6)0.7358 (4)0.054 (3)
H22B0.76600.66670.73510.065*
C2230.6661 (9)0.6082 (7)0.7503 (5)0.077 (4)
H22D0.69580.56530.75940.092*
C2240.5822 (8)0.6091 (8)0.7518 (5)0.073 (4)*
H22E0.55490.56670.76110.088*
C2250.5375 (8)0.6714 (8)0.7399 (6)0.084 (4)
H22C0.48020.67250.74200.100*
C2260.5793 (7)0.7342 (7)0.7242 (5)0.066 (3)
H22A0.54910.77670.71520.079*
C3110.8260 (7)0.7952 (7)0.5559 (4)0.056 (3)
C3120.8098 (8)0.8336 (9)0.5136 (4)0.078 (4)
H31B0.78850.88160.51330.093*
C3130.8268 (10)0.7972 (14)0.4695 (4)0.120 (8)
H31D0.81510.82130.44040.144*
C3140.8590 (14)0.7298 (13)0.4710 (9)0.127 (7)*
H31F0.87230.70830.44260.153*
C3150.8737 (11)0.6903 (11)0.5123 (7)0.111 (6)*
H31E0.89410.64210.51200.133*
C3160.8570 (9)0.7246 (8)0.5552 (5)0.076 (4)
H31A0.86740.69870.58380.091*
C3210.7754 (7)0.9291 (6)0.6047 (4)0.054 (3)
C3220.8136 (9)0.9905 (7)0.6266 (5)0.072 (4)
H32B0.86400.98500.64540.086*
C3230.7768 (12)1.0617 (8)0.6207 (6)0.093 (5)
H32D0.80201.10290.63590.112*
C3240.7040 (11)1.0688 (11)0.5923 (6)0.100 (5)*
H32E0.68061.11580.58800.120*
C3250.6638 (9)1.0102 (9)0.5701 (5)0.088 (5)
H32A0.61431.01720.55070.106*
C3260.6983 (8)0.9389 (8)0.5769 (5)0.074 (4)
H32C0.67030.89790.56310.089*
C4111.1048 (6)0.8548 (6)0.5741 (3)0.045 (2)
C4121.0348 (8)0.8602 (9)0.5416 (5)0.082 (4)
H41C0.98570.83660.54820.098*
C4131.0365 (10)0.9000 (9)0.4995 (6)0.088 (4)*
H41E0.98900.90310.47800.106*
C4141.1080 (10)0.9346 (9)0.4900 (5)0.088 (4)
H41A1.10890.96240.46220.105*
C4151.1766 (10)0.9291 (9)0.5198 (5)0.095 (5)
H41D1.22560.95200.51240.114*
C4161.1752 (8)0.8891 (8)0.5621 (4)0.073 (4)
H41B1.22370.88580.58280.088*
C4211.1129 (6)0.7062 (5)0.6093 (4)0.042 (2)
C4221.0635 (8)0.6485 (7)0.6228 (5)0.065 (3)
H42B1.01960.65860.64100.077*
C4231.0779 (10)0.5767 (8)0.6097 (6)0.089 (4)
H42D1.04330.53900.61880.106*
C4241.1425 (10)0.5599 (8)0.5834 (5)0.082 (4)
H42E1.15280.51100.57510.098*
C4251.1919 (9)0.6160 (8)0.5693 (6)0.086 (4)
H42C1.23590.60480.55130.103*
C4261.1777 (8)0.6894 (7)0.5814 (5)0.065 (3)
H42A1.21110.72710.57100.078*
C5111.2820 (6)0.8242 (6)0.7601 (4)0.046 (2)
C5121.3536 (7)0.8471 (6)0.7396 (4)0.060 (3)
H51C1.35670.84150.70700.072*
C5131.4206 (7)0.8783 (7)0.7681 (6)0.075 (4)
H51B1.46910.89220.75480.090*
C5141.4140 (9)0.8883 (7)0.8159 (5)0.077 (4)
H51D1.45840.90930.83490.093*
C5151.3443 (9)0.8684 (8)0.8361 (5)0.076 (4)*
H51E1.34060.87600.86850.092*
C5161.2786 (7)0.8367 (6)0.8080 (4)0.056 (3)
H51A1.23070.82340.82200.067*
C5211.2316 (6)0.6843 (6)0.7174 (4)0.046 (2)
C5221.1877 (9)0.6255 (7)0.7346 (5)0.071 (4)
H52B1.13750.63400.74760.086*
C5231.2197 (11)0.5525 (10)0.7322 (6)0.100 (5)*
H52E1.19080.51310.74440.120*
C5241.2906 (10)0.5395 (10)0.7128 (6)0.089 (4)*
H52D1.31120.49120.71210.107*
C5251.3336 (9)0.5960 (9)0.6938 (6)0.087 (5)
H52C1.38180.58600.67900.105*
C5261.3042 (7)0.6698 (7)0.6967 (5)0.070 (3)
H52A1.33400.70870.68460.083*
C6111.0875 (6)0.6706 (6)0.8791 (4)0.049 (3)
C6121.1532 (8)0.6397 (7)0.8590 (5)0.073 (4)
H61A1.17570.66440.83410.088*
C6131.1876 (11)0.5723 (10)0.8747 (6)0.103 (5)*
H61E1.23300.55260.86090.123*
C6141.1540 (9)0.5353 (8)0.9105 (6)0.089 (5)
H61C1.17620.48960.92070.107*
C6151.0884 (9)0.5642 (8)0.9317 (5)0.082 (4)
H61D1.06560.53830.95600.099*
C6161.0560 (8)0.6323 (7)0.9169 (5)0.067 (3)
H61B1.01280.65300.93220.081*
C6211.0957 (6)0.8292 (6)0.8955 (3)0.042 (2)
C6221.1073 (7)0.9003 (6)0.8784 (4)0.056 (3)
H62A1.08890.91180.84690.068*
C6231.1455 (9)0.9537 (8)0.9074 (5)0.084 (4)
H62C1.15291.00100.89530.101*
C6241.1728 (9)0.9386 (9)0.9535 (5)0.077 (4)*
H62E1.19890.97530.97280.093*
C6251.1621 (8)0.8702 (9)0.9713 (5)0.083 (4)
H62D1.18110.86041.00290.099*
C6261.1227 (7)0.8133 (7)0.9432 (4)0.061 (3)
H62B1.11490.76640.95590.074*
F10.3936 (11)0.6861 (8)0.5616 (7)0.222 (8)
Cl011.0705 (4)1.0238 (4)0.6219 (2)0.151 (2)*
F20.4760 (12)0.8702 (7)0.5496 (6)0.208 (7)
Cl021.1079 (3)1.1709 (3)0.6601 (2)0.1267 (16)*
F30.4648 (8)0.7500 (9)0.4966 (4)0.188 (7)
Cl031.1216 (8)0.5280 (8)0.4468 (5)0.291 (6)*
F40.5366 (8)0.7528 (10)0.5827 (6)0.218 (8)
Cl041.1579 (7)0.4512 (7)0.3603 (4)0.260 (5)*
F50.3993 (9)0.8078 (10)0.6122 (4)0.195 (7)
F60.3304 (10)0.8001 (9)0.5284 (6)0.198 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb0.0529 (5)0.0906 (7)0.0572 (5)0.0049 (4)0.0043 (4)0.0166 (4)
Ag10.0387 (4)0.0583 (5)0.0375 (4)0.0006 (4)0.0017 (3)0.0018 (4)
Ag20.0355 (4)0.0709 (6)0.0443 (4)0.0015 (4)0.0038 (3)0.0004 (4)
Ag30.0385 (4)0.0690 (6)0.0440 (4)0.0018 (4)0.0051 (3)0.0046 (4)
S10.0389 (13)0.0388 (13)0.0541 (15)0.0026 (11)0.0048 (11)0.0023 (11)
S20.0483 (14)0.0392 (14)0.0503 (15)0.0030 (11)0.0051 (11)0.0032 (11)
P10.0333 (12)0.0438 (14)0.0351 (12)0.0032 (11)0.0012 (10)0.0017 (11)
P20.0354 (12)0.0414 (14)0.0357 (12)0.0013 (11)0.0016 (10)0.0015 (10)
P30.0369 (13)0.0532 (16)0.0387 (13)0.0013 (12)0.0009 (10)0.0007 (12)
P40.0333 (12)0.0500 (16)0.0372 (13)0.0007 (11)0.0067 (10)0.0017 (11)
P50.0318 (12)0.0466 (15)0.0398 (13)0.0001 (11)0.0023 (10)0.0009 (11)
P60.0324 (12)0.0495 (15)0.0373 (13)0.0030 (11)0.0022 (10)0.0024 (11)
C10.032 (5)0.052 (6)0.039 (5)0.005 (4)0.000 (4)0.001 (4)
C20.036 (5)0.041 (5)0.041 (5)0.008 (4)0.005 (4)0.002 (4)
C30.039 (5)0.047 (6)0.044 (5)0.004 (5)0.010 (4)0.004 (5)
C1110.040 (5)0.058 (7)0.045 (6)0.003 (5)0.000 (4)0.005 (5)
C1120.079 (8)0.059 (8)0.053 (7)0.013 (6)0.001 (6)0.001 (6)
C1130.118 (13)0.055 (9)0.097 (12)0.014 (8)0.014 (10)0.003 (8)
C1140.098 (11)0.078 (11)0.097 (12)0.013 (9)0.007 (9)0.041 (9)
C1150.089 (10)0.080 (10)0.056 (8)0.007 (8)0.000 (7)0.028 (7)
C1160.069 (8)0.066 (8)0.050 (7)0.003 (6)0.008 (6)0.002 (6)
C1210.046 (6)0.043 (6)0.047 (6)0.002 (5)0.008 (4)0.004 (5)
C1220.047 (6)0.086 (9)0.048 (6)0.003 (6)0.003 (5)0.013 (6)
C1230.053 (7)0.105 (11)0.065 (8)0.005 (7)0.012 (6)0.014 (7)
C1240.044 (7)0.117 (12)0.084 (10)0.012 (7)0.030 (7)0.010 (9)
C1250.033 (6)0.112 (11)0.075 (9)0.003 (6)0.003 (5)0.006 (8)
C1260.031 (5)0.086 (9)0.055 (6)0.002 (5)0.001 (5)0.001 (6)
C2110.035 (5)0.046 (6)0.039 (5)0.004 (4)0.004 (4)0.001 (4)
C2120.049 (6)0.060 (7)0.073 (8)0.002 (6)0.002 (6)0.003 (6)
C2130.084 (10)0.049 (8)0.110 (12)0.010 (7)0.022 (9)0.025 (7)
C2140.080 (10)0.063 (9)0.115 (13)0.028 (8)0.029 (9)0.030 (9)
C2150.076 (9)0.097 (12)0.080 (10)0.042 (9)0.004 (7)0.016 (9)
C2160.061 (7)0.079 (9)0.057 (7)0.024 (7)0.006 (6)0.000 (6)
C2210.038 (5)0.035 (5)0.041 (5)0.002 (4)0.001 (4)0.009 (4)
C2220.043 (6)0.057 (7)0.064 (7)0.002 (5)0.011 (5)0.003 (6)
C2230.077 (9)0.051 (7)0.108 (11)0.003 (7)0.035 (8)0.012 (7)
C2250.052 (7)0.081 (10)0.120 (12)0.021 (7)0.016 (8)0.004 (9)
C2260.054 (7)0.062 (8)0.081 (9)0.001 (6)0.006 (6)0.001 (7)
C3110.044 (6)0.075 (8)0.049 (6)0.007 (6)0.006 (5)0.001 (6)
C3120.080 (9)0.111 (11)0.040 (6)0.009 (8)0.002 (6)0.009 (7)
C3130.096 (12)0.23 (2)0.029 (7)0.038 (14)0.003 (7)0.021 (10)
C3160.094 (10)0.076 (9)0.059 (8)0.001 (8)0.019 (7)0.021 (7)
C3210.054 (6)0.057 (7)0.052 (6)0.010 (5)0.011 (5)0.006 (5)
C3220.089 (10)0.064 (9)0.064 (8)0.012 (7)0.015 (7)0.009 (6)
C3230.150 (15)0.045 (8)0.089 (11)0.025 (9)0.037 (10)0.000 (7)
C3250.062 (8)0.113 (13)0.090 (10)0.027 (9)0.014 (7)0.042 (9)
C3260.063 (8)0.076 (9)0.082 (9)0.006 (7)0.001 (7)0.017 (7)
C4110.047 (6)0.045 (6)0.043 (5)0.002 (5)0.009 (4)0.007 (5)
C4120.067 (8)0.114 (12)0.062 (8)0.005 (8)0.002 (6)0.041 (8)
C4140.102 (11)0.094 (11)0.066 (9)0.002 (9)0.000 (8)0.033 (8)
C4150.097 (11)0.121 (13)0.067 (9)0.040 (10)0.005 (8)0.040 (9)
C4160.068 (8)0.093 (10)0.058 (7)0.025 (7)0.002 (6)0.025 (7)
C4210.030 (5)0.043 (6)0.051 (6)0.007 (4)0.002 (4)0.003 (5)
C4220.065 (8)0.049 (7)0.082 (9)0.003 (6)0.017 (6)0.004 (6)
C4230.091 (11)0.064 (9)0.114 (12)0.010 (8)0.024 (9)0.001 (9)
C4240.093 (11)0.054 (8)0.098 (11)0.006 (8)0.005 (9)0.016 (8)
C4250.066 (8)0.075 (10)0.122 (13)0.002 (8)0.028 (8)0.019 (9)
C4260.062 (7)0.056 (8)0.078 (8)0.002 (6)0.016 (6)0.006 (6)
C5110.042 (5)0.043 (6)0.054 (6)0.002 (5)0.002 (4)0.001 (5)
C5120.056 (7)0.061 (7)0.064 (7)0.009 (6)0.014 (6)0.006 (6)
C5130.036 (6)0.073 (9)0.115 (12)0.009 (6)0.001 (7)0.016 (8)
C5140.076 (9)0.061 (8)0.087 (10)0.003 (7)0.033 (8)0.021 (7)
C5160.056 (7)0.058 (7)0.053 (7)0.008 (5)0.003 (5)0.002 (5)
C5210.037 (5)0.051 (6)0.049 (6)0.003 (5)0.008 (4)0.001 (5)
C5220.079 (9)0.053 (8)0.085 (9)0.013 (7)0.024 (7)0.000 (7)
C5250.067 (9)0.093 (11)0.102 (11)0.020 (8)0.004 (8)0.030 (9)
C5260.054 (7)0.058 (8)0.097 (10)0.007 (6)0.007 (7)0.017 (7)
C6110.042 (6)0.042 (6)0.060 (7)0.009 (5)0.013 (5)0.002 (5)
C6120.057 (7)0.069 (8)0.094 (10)0.025 (7)0.004 (7)0.010 (7)
C6140.070 (9)0.064 (9)0.125 (13)0.026 (7)0.030 (9)0.008 (9)
C6150.079 (10)0.078 (10)0.087 (10)0.004 (8)0.009 (8)0.030 (8)
C6160.059 (7)0.071 (8)0.073 (8)0.019 (6)0.010 (6)0.019 (7)
C6210.032 (5)0.055 (6)0.040 (5)0.004 (5)0.005 (4)0.006 (5)
C6220.063 (7)0.059 (7)0.047 (6)0.016 (6)0.003 (5)0.006 (5)
C6230.095 (11)0.063 (9)0.096 (11)0.030 (8)0.016 (9)0.001 (8)
C6250.068 (8)0.120 (13)0.056 (8)0.005 (8)0.016 (6)0.015 (8)
C6260.059 (7)0.078 (9)0.045 (6)0.001 (6)0.005 (5)0.006 (6)
F10.230 (17)0.152 (13)0.29 (2)0.089 (12)0.057 (15)0.010 (13)
F20.30 (2)0.106 (9)0.224 (16)0.068 (11)0.075 (14)0.018 (10)
F30.164 (11)0.303 (18)0.107 (8)0.075 (11)0.065 (8)0.117 (10)
F40.123 (10)0.263 (17)0.245 (17)0.069 (11)0.096 (10)0.113 (14)
F50.182 (13)0.30 (2)0.107 (9)0.027 (12)0.055 (9)0.078 (11)
Geometric parameters (Å, º) top
Sb—F21.783 (12)C224—H22E0.9300
Sb—F41.801 (11)C225—C2261.407 (17)
Sb—F31.808 (9)C225—H22C0.9300
Sb—F11.815 (13)C226—H22A0.9300
Sb—F61.820 (17)C311—C3161.366 (18)
Sb—F51.853 (11)C311—C3121.379 (16)
Ag1—P22.465 (2)C312—C3131.45 (2)
Ag1—P12.465 (2)C312—H31B0.9300
Ag1—S22.734 (3)C313—C3141.32 (3)
Ag1—S12.760 (3)C313—H31D0.9300
Ag1—Ag23.3369 (11)C314—C3151.36 (3)
Ag2—P42.468 (2)C314—H31F0.9300
Ag2—P32.469 (3)C315—C3161.40 (2)
Ag2—S22.661 (3)C315—H31E0.9300
Ag2—S12.825 (3)C316—H31A0.9300
Ag3—P52.483 (3)C321—C3221.380 (17)
Ag3—P62.491 (3)C321—C3261.413 (16)
Ag3—S12.686 (3)C322—C3231.415 (19)
Ag3—S22.771 (3)C322—H32B0.9300
S1—H6A1.2000C323—C3241.36 (2)
S2—H6B1.2000C323—H32D0.9300
P1—C1111.816 (11)C324—C3251.36 (2)
P1—C11.838 (9)C324—H32E0.9300
P1—C1211.842 (10)C325—C3261.406 (19)
P2—C2111.808 (10)C325—H32A0.9300
P2—C2211.839 (10)C326—H32C0.9300
P2—C21.847 (9)C411—C4161.359 (15)
P3—C3211.818 (12)C411—C4121.384 (16)
P3—C3111.842 (12)C412—C4131.386 (19)
P3—C21.845 (9)C412—H41C0.9300
P4—C4211.824 (10)C413—C4141.36 (2)
P4—C4111.825 (10)C413—H41E0.9300
P4—C31.854 (10)C414—C4151.32 (2)
P5—C5211.827 (11)C414—H41A0.9300
P5—C5111.840 (10)C415—C4161.394 (17)
P5—C31.865 (9)C415—H41D0.9300
P6—C6111.832 (10)C416—H41B0.9300
P6—C6211.834 (10)C421—C4221.383 (15)
P6—C11.846 (9)C421—C4261.395 (15)
C1—H1A0.9700C422—C4231.370 (18)
C1—H1B0.9700C422—H42B0.9300
C2—H2A0.9700C423—C4241.366 (19)
C2—H2B0.9700C423—H42D0.9300
C3—H3A0.9700C424—C4251.366 (19)
C3—H3B0.9700C424—H42E0.9300
C4—Cl011.720 (5)C425—C4261.390 (18)
C4—Cl021.726 (5)C425—H42C0.9300
C4—H4A0.9700C426—H42A0.9300
C4—H4B0.9700C511—C5161.372 (15)
C5—Cl031.720 (5)C511—C5121.396 (15)
C5—Cl041.721 (5)C512—C5131.400 (16)
C5—H5A0.9700C512—H51C0.9300
C5—H5B0.9700C513—C5141.369 (19)
C111—C1121.385 (15)C513—H51B0.9300
C111—C1161.395 (15)C514—C5151.351 (19)
C112—C1131.400 (18)C514—H51D0.9300
C112—H11B0.9300C515—C5161.380 (17)
C113—C1141.39 (2)C515—H51E0.9300
C113—H11E0.9300C516—H51A0.9300
C114—C1151.36 (2)C521—C5261.378 (16)
C114—H11D0.9300C521—C5221.384 (15)
C115—C1161.377 (17)C522—C5231.42 (2)
C115—H11C0.9300C522—H52B0.9300
C116—H11A0.9300C523—C5241.33 (2)
C121—C1261.381 (14)C523—H52E0.9300
C121—C1221.409 (14)C524—C5251.37 (2)
C122—C1231.378 (16)C524—H52D0.9300
C122—H12A0.9300C525—C5261.416 (18)
C123—C1241.365 (18)C525—H52C0.9300
C123—H12D0.9300C526—H52A0.9300
C124—C1251.366 (18)C611—C6121.363 (16)
C124—H12E0.9300C611—C6161.400 (16)
C125—C1261.383 (15)C612—C6131.39 (2)
C125—H12C0.9300C612—H61A0.9300
C126—H12B0.9300C613—C6141.36 (2)
C211—C2121.384 (15)C613—H61E0.9300
C211—C2161.386 (14)C614—C6151.36 (2)
C212—C2131.399 (17)C614—H61C0.9300
C212—H21B0.9300C615—C6161.381 (18)
C213—C2141.37 (2)C615—H61D0.9300
C213—H21D0.9300C616—H61B0.9300
C214—C2151.36 (2)C621—C6221.386 (15)
C214—H21C0.9300C621—C6261.399 (14)
C215—C2161.388 (17)C622—C6231.369 (17)
C215—H21E0.9300C622—H62A0.9300
C216—H21A0.9300C623—C6241.356 (19)
C221—C2261.385 (15)C623—H62C0.9300
C221—C2221.389 (14)C624—C6251.35 (2)
C222—C2231.365 (16)C624—H62E0.9300
C222—H22B0.9300C625—C6261.408 (17)
C223—C2241.355 (18)C625—H62D0.9300
C223—H22D0.9300C626—H62B0.9300
C224—C2251.356 (19)
F2—Sb—F487.3 (9)C214—C215—H21E120.3
F2—Sb—F393.9 (7)C216—C215—H21E120.3
F4—Sb—F391.4 (7)C211—C216—C215121.9 (13)
F2—Sb—F1177.8 (8)C211—C216—H21A119.0
F4—Sb—F192.5 (9)C215—C216—H21A119.0
F3—Sb—F188.3 (8)C226—C221—C222118.4 (10)
F2—Sb—F696.0 (8)C226—C221—P2124.0 (8)
F4—Sb—F6176.1 (9)C222—C221—P2117.6 (7)
F3—Sb—F690.6 (7)C223—C222—C221119.9 (10)
F1—Sb—F684.2 (8)C223—C222—H22B120.1
F2—Sb—F587.2 (7)C221—C222—H22B120.1
F4—Sb—F591.8 (7)C224—C223—C222121.7 (13)
F3—Sb—F5176.6 (6)C224—C223—H22D119.2
F1—Sb—F590.7 (8)C222—C223—H22D119.2
F6—Sb—F586.1 (7)C223—C224—C225120.5 (13)
P2—Ag1—P1126.27 (8)C223—C224—H22E119.7
P2—Ag1—S2123.04 (9)C225—C224—H22E119.7
P1—Ag1—S2104.35 (8)C224—C225—C226119.0 (12)
P2—Ag1—S196.47 (8)C224—C225—H22C120.5
P1—Ag1—S1110.40 (8)C226—C225—H22C120.5
S2—Ag1—S187.51 (8)C221—C226—C225120.6 (12)
P2—Ag1—Ag286.89 (6)C221—C226—H22A119.7
P1—Ag1—Ag2146.48 (6)C225—C226—H22A119.7
S2—Ag1—Ag250.81 (6)C316—C311—C312119.6 (12)
S1—Ag1—Ag254.21 (6)C316—C311—P3116.4 (9)
P4—Ag2—P3125.91 (9)C312—C311—P3123.4 (11)
P4—Ag2—S2108.86 (9)C311—C312—C313118.4 (15)
P3—Ag2—S2116.19 (9)C311—C312—H31B120.8
P4—Ag2—S1106.08 (8)C313—C312—H31B120.8
P3—Ag2—S1104.18 (9)C314—C313—C312119.5 (17)
S2—Ag2—S187.62 (8)C314—C313—H31D120.2
P4—Ag2—Ag1147.21 (7)C312—C313—H31D120.2
P3—Ag2—Ag186.04 (6)C313—C314—C315123 (2)
S2—Ag2—Ag152.78 (6)C313—C314—H31F118.5
S1—Ag2—Ag152.42 (5)C315—C314—H31F118.5
P5—Ag3—P6131.32 (9)C314—C315—C316118.1 (19)
P5—Ag3—S1112.96 (9)C314—C315—H31E120.9
P6—Ag3—S1102.47 (9)C316—C315—H31E120.9
P5—Ag3—S2103.27 (9)C311—C316—C315121.3 (15)
P6—Ag3—S2110.31 (9)C311—C316—H31A119.3
S1—Ag3—S288.23 (8)C315—C316—H31A119.3
Ag3—S1—Ag179.33 (7)C322—C321—C326118.5 (12)
Ag3—S1—Ag277.18 (7)C322—C321—P3119.6 (9)
Ag1—S1—Ag273.38 (7)C326—C321—P3121.7 (9)
Ag3—S1—H6A134.2C321—C322—C323120.5 (14)
Ag1—S1—H6A134.2C321—C322—H32B119.7
Ag2—S1—H6A134.2C323—C322—H32B119.7
Ag2—S2—Ag176.40 (7)C324—C323—C322118.8 (15)
Ag2—S2—Ag378.54 (7)C324—C323—H32D120.6
Ag1—S2—Ag378.33 (7)C322—C323—H32D120.6
Ag2—S2—H6B133.5C325—C324—C323122.9 (17)
Ag1—S2—H6B133.5C325—C324—H32E118.5
Ag3—S2—H6B133.5C323—C324—H32E118.5
C111—P1—C1105.1 (5)C324—C325—C326118.8 (15)
C111—P1—C121104.1 (5)C324—C325—H32A120.6
C1—P1—C121101.6 (5)C326—C325—H32A120.6
C111—P1—Ag1116.9 (4)C325—C326—C321120.2 (14)
C1—P1—Ag1112.7 (3)C325—C326—H32C119.9
C121—P1—Ag1114.8 (3)C321—C326—H32C119.9
C211—P2—C221105.7 (4)C416—C411—C412116.7 (10)
C211—P2—C2107.1 (4)C416—C411—P4126.9 (9)
C221—P2—C299.8 (4)C412—C411—P4116.4 (8)
C211—P2—Ag1116.9 (3)C411—C412—C413121.2 (13)
C221—P2—Ag1108.9 (3)C411—C412—H41C119.4
C2—P2—Ag1116.6 (3)C413—C412—H41C119.4
C321—P3—C311106.3 (5)C414—C413—C412119.5 (15)
C321—P3—C2104.3 (5)C414—C413—H41E120.3
C311—P3—C2103.4 (5)C412—C413—H41E120.3
C321—P3—Ag2120.4 (4)C415—C414—C413120.8 (14)
C311—P3—Ag2109.1 (4)C415—C414—H41A119.6
C2—P3—Ag2111.9 (3)C413—C414—H41A119.6
C421—P4—C411102.7 (5)C414—C415—C416120.0 (14)
C421—P4—C3103.0 (4)C414—C415—H41D120.0
C411—P4—C3103.3 (4)C416—C415—H41D120.0
C421—P4—Ag2116.8 (3)C411—C416—C415121.8 (12)
C411—P4—Ag2112.9 (3)C411—C416—H41B119.1
C3—P4—Ag2116.3 (3)C415—C416—H41B119.1
C521—P5—C511103.1 (4)C422—C421—C426118.0 (10)
C521—P5—C3105.2 (5)C422—C421—P4120.3 (8)
C511—P5—C3102.1 (5)C426—C421—P4121.7 (8)
C521—P5—Ag3113.6 (4)C423—C422—C421121.4 (12)
C511—P5—Ag3112.8 (3)C423—C422—H42B119.3
C3—P5—Ag3118.3 (3)C421—C422—H42B119.3
C611—P6—C621104.2 (5)C424—C423—C422120.7 (14)
C611—P6—C1101.3 (5)C424—C423—H42D119.6
C621—P6—C1105.2 (4)C422—C423—H42D119.6
C611—P6—Ag3113.8 (4)C423—C424—C425119.1 (13)
C621—P6—Ag3112.9 (3)C423—C424—H42E120.5
C1—P6—Ag3118.0 (3)C425—C424—H42E120.5
P1—C1—P6117.0 (5)C424—C425—C426121.3 (13)
P1—C1—H1A108.1C424—C425—H42C119.3
P6—C1—H1A108.1C426—C425—H42C119.3
P1—C1—H1B108.1C425—C426—C421119.5 (12)
P6—C1—H1B108.1C425—C426—H42A120.3
H1A—C1—H1B107.3C421—C426—H42A120.3
P3—C2—P2112.5 (5)C516—C511—C512117.8 (10)
P3—C2—H2A109.1C516—C511—P5118.1 (8)
P2—C2—H2A109.1C512—C511—P5124.1 (8)
P3—C2—H2B109.1C511—C512—C513120.2 (12)
P2—C2—H2B109.1C511—C512—H51C119.9
H2A—C2—H2B107.8C513—C512—H51C119.9
P4—C3—P5112.7 (5)C514—C513—C512119.1 (12)
P4—C3—H3A109.0C514—C513—H51B120.4
P5—C3—H3A109.0C512—C513—H51B120.4
P4—C3—H3B109.0C515—C514—C513121.4 (12)
P5—C3—H3B109.0C515—C514—H51D119.3
H3A—C3—H3B107.8C513—C514—H51D119.3
Cl01—C4—Cl02114.6 (7)C514—C515—C516119.4 (13)
Cl01—C4—H4A108.6C514—C515—H51E120.3
Cl02—C4—H4A108.6C516—C515—H51E120.3
Cl01—C4—H4B108.6C511—C516—C515122.0 (12)
Cl02—C4—H4B108.6C511—C516—H51A119.0
H4A—C4—H4B107.6C515—C516—H51A119.0
Cl03—C5—Cl04115.0 (11)C526—C521—C522118.8 (11)
Cl03—C5—H5A108.5C526—C521—P5123.6 (9)
Cl04—C5—H5A108.5C522—C521—P5117.5 (9)
Cl03—C5—H5B108.5C521—C522—C523119.7 (13)
Cl04—C5—H5B108.5C521—C522—H52B120.2
H5A—C5—H5B107.5C523—C522—H52B120.2
C112—C111—C116117.6 (11)C524—C523—C522120.8 (17)
C112—C111—P1119.1 (8)C524—C523—H52E119.6
C116—C111—P1123.2 (9)C522—C523—H52E119.6
C111—C112—C113120.9 (12)C523—C524—C525121.0 (17)
C111—C112—H11B119.6C523—C524—H52D119.5
C113—C112—H11B119.6C525—C524—H52D119.5
C114—C113—C112119.7 (14)C524—C525—C526119.4 (14)
C114—C113—H11E120.2C524—C525—H52C120.3
C112—C113—H11E120.2C526—C525—H52C120.3
C115—C114—C113119.8 (13)C521—C526—C525120.3 (13)
C115—C114—H11D120.1C521—C526—H52A119.9
C113—C114—H11D120.1C525—C526—H52A119.9
C114—C115—C116120.5 (12)C612—C611—C616117.6 (11)
C114—C115—H11C119.8C612—C611—P6119.2 (10)
C116—C115—H11C119.8C616—C611—P6123.2 (8)
C115—C116—C111121.6 (12)C611—C612—C613121.7 (14)
C115—C116—H11A119.2C611—C612—H61A119.1
C111—C116—H11A119.2C613—C612—H61A119.1
C126—C121—C122117.5 (10)C614—C613—C612119.3 (16)
C126—C121—P1119.2 (8)C614—C613—H61E120.3
C122—C121—P1123.3 (8)C612—C613—H61E120.3
C123—C122—C121120.1 (11)C613—C614—C615120.9 (14)
C123—C122—H12A119.9C613—C614—H61C119.5
C121—C122—H12A119.9C615—C614—H61C119.5
C124—C123—C122121.1 (12)C614—C615—C616119.5 (14)
C124—C123—H12D119.5C614—C615—H61D120.3
C122—C123—H12D119.5C616—C615—H61D120.3
C123—C124—C125119.6 (11)C615—C616—C611120.9 (12)
C123—C124—H12E120.2C615—C616—H61B119.6
C125—C124—H12E120.2C611—C616—H61B119.6
C124—C125—C126120.3 (11)C622—C621—C626118.8 (10)
C124—C125—H12C119.9C622—C621—P6119.5 (8)
C126—C125—H12C119.9C626—C621—P6121.7 (9)
C121—C126—C125121.4 (11)C623—C622—C621120.6 (11)
C121—C126—H12B119.3C623—C622—H62A119.7
C125—C126—H12B119.3C621—C622—H62A119.7
C212—C211—C216116.7 (10)C624—C623—C622121.0 (13)
C212—C211—P2118.6 (8)C624—C623—H62C119.5
C216—C211—P2124.8 (8)C622—C623—H62C119.5
C211—C212—C213122.3 (12)C625—C624—C623119.8 (14)
C211—C212—H21B118.8C625—C624—H62E120.1
C213—C212—H21B118.8C623—C624—H62E120.1
C214—C213—C212118.6 (13)C624—C625—C626121.6 (13)
C214—C213—H21D120.7C624—C625—H62D119.2
C212—C213—H21D120.7C626—C625—H62D119.2
C215—C214—C213121.0 (13)C621—C626—C625118.2 (12)
C215—C214—H21C119.5C621—C626—H62B120.9
C213—C214—H21C119.5C625—C626—H62B120.9
C214—C215—C216119.5 (13)

Experimental details

Crystal data
Chemical formula[Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2
Mr1948.45
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)16.0813 (1), 18.0049 (2), 28.1089 (3)
β (°) 95.417 (1)
V3)8102.36 (13)
Z4
Radiation typeMo Kα
µ (mm1)1.40
Crystal size (mm)0.72 × 0.60 × 0.46
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionEmpirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.354, 0.525
No. of measured, independent and
observed [I > 2σ(I)] reflections
25151, 14088, 10084
Rint0.047
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.080, 0.210, 1.21
No. of reflections14088
No. of parameters807
No. of restraints4
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.50, 1.23

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), XPREP (Siemens, 1994), SHELXTL (Siemens, 1994), SHELXTL.

Selected geometric parameters (Å, º) top
Ag1—P22.465 (2)Ag2—S22.661 (3)
Ag1—P12.465 (2)Ag2—S12.825 (3)
Ag1—S22.734 (3)Ag3—P52.483 (3)
Ag1—S12.760 (3)Ag3—P62.491 (3)
Ag1—Ag23.3369 (11)Ag3—S12.686 (3)
Ag2—P42.468 (2)Ag3—S22.771 (3)
Ag2—P32.469 (3)
P2—Ag1—P1126.27 (8)P4—Ag2—P3125.91 (9)
P2—Ag1—S196.47 (8)P3—Ag2—S2116.19 (9)
P2—Ag1—Ag286.89 (6)P5—Ag3—S2103.27 (9)
P1—Ag1—Ag2146.48 (6)Ag3—S1—Ag179.33 (7)
S2—Ag1—Ag250.81 (6)Ag3—S1—Ag277.18 (7)
S1—Ag1—Ag254.21 (6)Ag1—S1—Ag273.38 (7)
 

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