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Acta Cryst. (2007). E63, m1990-m1991    [ doi:10.1107/S1600536807030218 ]

[mu]3-Iodido-tri-[mu]3-sulfido-tris[(triphenylphosphine)silver(I)][thioxotungsten(VI)] dichloromethane 0.45-solvate

A. Beheshti, W. Clegg, S. H. Dale and R. Hyvadi

Abstract top

In the title complex, [WAg3IS4(C18H15P)3]·0.45CH2Cl2, the W atom has almost regular tetrahedral coordination geometry, with one terminal and three triply bridging S atoms; the Ag atoms have tetrahedral coordination geometry distorted by expanded P-Ag-S and contracted S-Ag-S angles, the fourth site being occupied by a triply bridging I atom. The bridging S and I atoms, together with the W and three Ag atoms, form a pseudo-cubane core with small angles at the non-metal vertices, resulting in short W...Ag distances. The dichloromethane solvent molecule is disordered over two inversion-related sites with common Cl-atom sites and with a refined occupancy factor of 0.449 (4) for each site.

Comment top

The title complex was obtained as an unexpected decomposition product in an attempt to prepare a WS4/Ag/Zn mixed-metal complex containing phosphine and heterocyclic thione ligands. It features a pseudo-cubane WS3Ag3I core with a typical geometry involving wide angles at the metal corners and narrow angles at the S and I atoms, giving short W···Ag distances [2.9737 (5)–3.0310 (8) Å] that do not represent formal direct metal-metal bonds.

The W atom has an almost regular tetrahedral coordination geometry, with the terminal W═S bond significantly shorter than the bonds to triply-bridging S atoms. The coordination of the Ag atoms is rather distorted tetrahedral, with the smallest angle in each case between the two Ag—S bonds and the largest angles between Ag—S and Ag—P bonds, as a consequence of the steric demands of the triphenylphosphine ligands.

Very similar structures have been found for related complexes in which one or more of the following substitutions are made: Mo for W, O for the terminal S, Cl or Br for I, pyridyl for one of the phenyl rings on each phosphine ligand (Jin et al., 1999, 2000; Sakane et al., 1996; Wang et al., 2003; Lang et al., 1992, 1993; Zhu et al., 1992; Wu et al., 1992). Some of these are actually isomorphous and probably isostructural with the title complex, although the solvent is water rather than dichloromethane in one case, but coordinates are not available for all of the structures.

Related literature top

For similar structures, see: Jin et al. (1999, 2000); Sakane et al. (1996); Wang et al. (2003); Lang et al. (1992, 1993); Zhu et al. (1992); Wu et al. (1992).

Experimental top

This compound is an unexpected product in the attempted preparation of [WS4Ag(PPh3)IZn(Diap)2] (Diap = 1,3-diazepane-2-thione). An aqueous solution of (Diap)2Zn(OAc)2·H2O (0.05 mmol, 0.023 g) was added to an aqueous solution of (NH4)2[WS4] (0.05 mmol, 0.017 g) in a total volume of 5 ml of water and the mixture was stirred for 2 min. The yellow precipitate was separated by centrifugation and washed with EtOH (2 × 5 ml) and Et2O (2 × 5 ml). The yellow product, which is soluble in all common organic solvents, was dissolved in CH2Cl2 (10 ml) and solid AgI (0.05 mmol, 0.011 g) and PPh3 (0.05 mmol, 0.013 g) were added. The mixture was stirred for 30 min and then filtered. The filtrate was evaporated under vacuum. The residue was washed with diethyl ether (2 × 5 ml) and dried in vacuo to give a yellow powder. Single crystals were obtained by slow diffusion of diethyl ether into an acetone solution of the complex. On leaving the solution to stand in a refrigerator overnight, air-stable yellow crystals were deposited.

The FT—IR spectrum in the range 4000–400 cm−1 shows all the expected strong phosphine bands, which remain practically unshifted from those of the uncomplexed ligand. The spectrum also displays a doublet at 419.4 and 438.8 cm−1, which is attributed to ν(W—µ3-S) vibrations. A strong band at 510 cm−1 is due to the δ(C—H) vibrations of the PPh3 ligands It is difficult to identify features due to the W—S(terminal) and Ag—P absorptions, because the PPh3 ligands give rise to a strong band in the same positions as expected for these features. The electronic absorption spectrum of the complex in DMF solution appears to be mainly of intraligand character, presenting two broad bands with maxima at 291 and 401.5 nm. These absorptions can be assigned as charge-transfer bands of the type (π)S→ (d)W arising from the WS4 group; these are red-shifted compared to the free [WS4]2− anion.

Refinement top

Hydrogen atoms were positioned geometrically and refined with a riding model, with C—H = 0.95 or 0.99 Å and with Uiso = 1.2Ueq(C). The dichloromethane solvent molecule is disordered equally over two positions close to an inversion centre, sharing the Cl atom sites; no restraints were used, and the anisotropic displacement parameters indicate that the disorder is actually more complicated. The largest residual electron density peaks are close to W and Cl atoms.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: EVALCCD (Duisenberg et al., 2003); data reduction: EVALCCD; program(s) used to solve structure: SHELXTL (Sheldrick, 2005); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Figures top
[Figure 1] Fig. 1. The molecular structure with atom labels and 40% probability ellipsoids for non-H atoms. H atoms and the solvent molecule have been omitted.
µ3-Iodido-tri-µ3-sulfido- tris[(triphenylphosphine)silver(I)][thioxotungsten(VI)] dichloromethane 0.45-solvate top
Crystal data top
[WAg3IS4(C18H15P)3]·0.45CH2Cl2Z = 2
Mr = 1587.63F000 = 1530
Triclinic, P1Dx = 1.894 Mg m−3
a = 12.113 (3) ÅMo Kα radiation
λ = 0.71073 Å
b = 13.3231 (14) ÅCell parameters from 643 reflections
c = 20.0301 (14) Åθ = 2.5–27.5º
α = 74.671 (8)ºµ = 3.97 mm−1
β = 87.659 (11)ºT = 150 (2) K
γ = 63.692 (10)ºBlock, yellow
V = 2783.7 (8) Å30.37 × 0.22 × 0.18 mm
Data collection top
Nonius KappaCCD
diffractometer		12444 independent reflections
Radiation source: fine-focus sealed tube10245 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.049
T = 150(2) Kθmax = 27.5º
φ and ω scansθmin = 4.4º
Absorption correction: numerical
(SHELXTL; Sheldrick, 2005)		h = −15→15
Tmin = 0.321, Tmax = 0.545k = −16→17
38642 measured reflectionsl = −25→26
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)] = 0.028H-atom parameters constrained
wR(F2) = 0.068  w = 1/[σ2(Fo2) + (0.0275P)2 + 1.8123P]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.001
12444 reflectionsΔρmax = 1.21 e Å−3
614 parametersΔρmin = −0.98 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[WAg3IS4(C18H15P)3]·0.45CH2Cl2γ = 63.692 (10)º
Mr = 1587.63V = 2783.7 (8) Å3
Triclinic, P1Z = 2
a = 12.113 (3) ÅMo Kα
b = 13.3231 (14) ŵ = 3.97 mm−1
c = 20.0301 (14) ÅT = 150 (2) K
α = 74.671 (8)º0.37 × 0.22 × 0.18 mm
β = 87.659 (11)º
Data collection top
Nonius KappaCCD
diffractometer		12444 independent reflections
Absorption correction: numerical
(SHELXTL; Sheldrick, 2005)		10245 reflections with I > 2σ(I)
Tmin = 0.321, Tmax = 0.545Rint = 0.049
38642 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028614 parameters
wR(F2) = 0.068H-atom parameters constrained
S = 0.98Δρmax = 1.21 e Å−3
12444 reflectionsΔρmin = −0.98 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
W0.105460 (12)0.535347 (11)0.148656 (7)0.01491 (4)
Ag10.25207 (3)0.58341 (3)0.240876 (15)0.02614 (7)
Ag20.17124 (3)0.35043 (2)0.282604 (15)0.03036 (8)
Ag30.37164 (3)0.35425 (2)0.156496 (17)0.02844 (7)
S10.04814 (8)0.57272 (8)0.25178 (5)0.01983 (18)
S20.16114 (9)0.34801 (8)0.15507 (5)0.02232 (19)
S30.25794 (8)0.58312 (7)0.11261 (5)0.01902 (18)
S4−0.05180 (9)0.63984 (9)0.07374 (5)0.0313 (2)
I0.43103 (2)0.326826 (19)0.307325 (12)0.02289 (6)
P10.32368 (8)0.68707 (8)0.29432 (5)0.01763 (19)
C10.3168 (3)0.6609 (3)0.38846 (19)0.0203 (7)
C20.3521 (3)0.5466 (3)0.42839 (19)0.0242 (8)
H20.37470.48640.40610.029*
C30.3546 (4)0.5203 (3)0.5001 (2)0.0300 (9)
H30.38020.44190.52660.036*
C40.3204 (4)0.6067 (4)0.5335 (2)0.0315 (9)
H40.32110.58840.58270.038*
C50.2849 (4)0.7202 (4)0.4944 (2)0.0335 (10)
H50.26120.78030.51690.040*
C60.2836 (4)0.7473 (3)0.4220 (2)0.0268 (8)
H60.25990.82550.39570.032*
C70.2375 (3)0.8447 (3)0.26030 (19)0.0227 (8)
C80.1089 (4)0.8910 (4)0.2542 (2)0.0358 (10)
H80.07080.84060.26570.043*
C90.0363 (4)1.0109 (4)0.2313 (2)0.0454 (12)
H9−0.05131.04230.22840.054*
C100.0915 (5)1.0837 (4)0.2129 (2)0.0433 (12)
H100.04191.16570.19780.052*
C110.2174 (5)1.0387 (3)0.2161 (2)0.0400 (11)
H110.25471.08950.20180.048*
C120.2914 (4)0.9193 (3)0.2400 (2)0.0299 (9)
H120.37890.88890.24240.036*
C130.4860 (3)0.6514 (3)0.28289 (18)0.0183 (7)
C140.5505 (4)0.6868 (3)0.32088 (19)0.0252 (8)
H140.51080.72610.35470.030*
C150.6706 (4)0.6648 (4)0.3094 (2)0.0336 (10)
H150.71320.69080.33410.040*
C160.7295 (4)0.6042 (4)0.2612 (2)0.0398 (11)
H160.81240.58930.25300.048*
C170.6687 (4)0.5656 (4)0.2255 (2)0.0361 (10)
H170.71030.52270.19350.043*
C180.5467 (3)0.5893 (3)0.2362 (2)0.0270 (8)
H180.50470.56280.21140.032*
P20.14681 (9)0.22050 (8)0.38378 (5)0.02021 (19)
C190.1090 (3)0.2784 (3)0.45942 (18)0.0209 (8)
C200.1687 (3)0.3413 (3)0.47205 (19)0.0242 (8)
H200.22530.35470.44100.029*
C210.1456 (4)0.3843 (3)0.5299 (2)0.0290 (9)
H210.18590.42750.53810.035*
C220.0646 (4)0.3645 (3)0.5754 (2)0.0294 (9)
H220.04990.39340.61510.035*
C230.0042 (4)0.3028 (3)0.5636 (2)0.0306 (9)
H23−0.05190.28960.59500.037*
C240.0260 (4)0.2599 (3)0.5053 (2)0.0272 (8)
H24−0.01590.21800.49700.033*
C250.0217 (3)0.1831 (3)0.37216 (18)0.0208 (8)
C26−0.0861 (4)0.2707 (3)0.3318 (2)0.0302 (9)
H26−0.09040.34490.30950.036*
C27−0.1862 (4)0.2500 (4)0.3242 (2)0.0349 (10)
H27−0.25920.31010.29690.042*
C28−0.1806 (4)0.1417 (4)0.3563 (2)0.0331 (10)
H28−0.25000.12780.35150.040*
C29−0.0741 (4)0.0546 (4)0.3949 (2)0.0336 (10)
H29−0.0697−0.02000.41600.040*
C300.0277 (4)0.0744 (3)0.4037 (2)0.0263 (8)
H300.10040.01390.43100.032*
C310.2853 (3)0.0832 (3)0.4146 (2)0.0222 (8)
C320.3116 (4)0.0162 (3)0.4846 (2)0.0302 (9)
H320.25570.04240.51790.036*
C330.4182 (4)−0.0872 (4)0.5048 (2)0.0388 (11)
H330.4352−0.13270.55190.047*
C340.4995 (4)−0.1242 (4)0.4570 (3)0.0440 (12)
H340.5724−0.19590.47130.053*
C350.4775 (4)−0.0600 (4)0.3889 (3)0.0406 (11)
H350.5354−0.08680.35650.049*
C360.3702 (4)0.0449 (3)0.3669 (2)0.0289 (9)
H360.35510.08990.31980.035*
P30.55628 (8)0.23800 (8)0.10917 (5)0.02003 (19)
C370.6526 (3)0.0897 (3)0.16250 (19)0.0194 (7)
C380.6651 (4)0.0684 (3)0.2341 (2)0.0330 (10)
H380.62110.13050.25440.040*
C390.7405 (4)−0.0420 (3)0.2768 (2)0.0363 (10)
H390.7479−0.05510.32580.044*
C400.8041 (4)−0.1317 (3)0.2475 (2)0.0289 (9)
H400.8568−0.20700.27630.035*
C410.7920 (4)−0.1133 (3)0.1771 (2)0.0432 (12)
H410.8357−0.17610.15730.052*
C420.7158 (4)−0.0028 (3)0.1343 (2)0.0387 (11)
H420.70720.00910.08550.046*
C430.5242 (3)0.2135 (3)0.02780 (19)0.0227 (8)
C440.4232 (4)0.1924 (3)0.0225 (2)0.0329 (9)
H440.37030.19590.05910.039*
C450.3990 (4)0.1662 (4)−0.0364 (3)0.0433 (11)
H450.33030.1508−0.03980.052*
C460.4756 (5)0.1626 (4)−0.0901 (3)0.0478 (12)
H460.45950.1440−0.13010.057*
C470.5745 (5)0.1857 (4)−0.0858 (2)0.0435 (11)
H470.62570.1843−0.12310.052*
C480.5998 (4)0.2113 (3)−0.0268 (2)0.0307 (9)
H480.66830.2271−0.02370.037*
C490.6616 (3)0.3046 (3)0.09070 (18)0.0217 (8)
C500.6130 (4)0.4248 (3)0.0786 (2)0.0274 (8)
H500.52680.47010.08000.033*
C510.6905 (4)0.4789 (3)0.0644 (2)0.0331 (9)
H510.65640.56100.05590.040*
C520.8155 (4)0.4147 (4)0.0625 (2)0.0326 (9)
H520.86770.45210.05350.039*
C530.8652 (4)0.2947 (4)0.0739 (2)0.0312 (9)
H530.95130.25000.07180.037*
C540.7887 (3)0.2403 (3)0.0882 (2)0.0280 (9)
H540.82320.15820.09650.034*
Cl1.0901 (3)0.0109 (3)0.0356 (2)0.182 (3)0.898 (9)
C550.9850 (12)0.0868 (12)−0.0452 (9)0.092 (6)0.449 (4)
H55A0.92490.1672−0.04590.111*0.449 (4)
H55B1.03080.0882−0.08730.111*0.449 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W0.01416 (8)0.01395 (7)0.01676 (7)−0.00668 (6)0.00146 (5)−0.00376 (5)
Ag10.02735 (16)0.03518 (17)0.02890 (16)−0.02200 (14)0.00552 (12)−0.01526 (13)
Ag20.04511 (19)0.02228 (15)0.02184 (15)−0.01689 (14)0.00866 (13)−0.00086 (12)
Ag30.02171 (16)0.02078 (15)0.03969 (18)−0.00569 (12)0.01081 (13)−0.01155 (13)
S10.0169 (4)0.0212 (4)0.0242 (5)−0.0092 (4)0.0078 (3)−0.0104 (4)
S20.0280 (5)0.0185 (4)0.0258 (5)−0.0137 (4)0.0043 (4)−0.0089 (4)
S30.0196 (5)0.0173 (4)0.0197 (4)−0.0094 (4)0.0049 (3)−0.0029 (3)
S40.0236 (5)0.0308 (5)0.0320 (6)−0.0084 (4)−0.0086 (4)−0.0021 (4)
I0.02200 (13)0.01956 (12)0.02312 (13)−0.00603 (10)0.00018 (9)−0.00527 (9)
P10.0166 (5)0.0186 (5)0.0205 (5)−0.0101 (4)0.0028 (3)−0.0061 (4)
C10.0201 (19)0.0212 (18)0.0222 (19)−0.0111 (15)0.0039 (14)−0.0070 (15)
C20.026 (2)0.0240 (19)0.024 (2)−0.0136 (16)0.0041 (15)−0.0056 (16)
C30.028 (2)0.030 (2)0.027 (2)−0.0133 (18)0.0026 (16)0.0009 (17)
C40.030 (2)0.045 (3)0.021 (2)−0.018 (2)0.0048 (16)−0.0080 (18)
C50.039 (2)0.041 (2)0.028 (2)−0.020 (2)0.0113 (18)−0.0184 (19)
C60.031 (2)0.025 (2)0.027 (2)−0.0135 (17)0.0047 (16)−0.0111 (16)
C70.026 (2)0.0211 (19)0.0200 (19)−0.0088 (16)0.0016 (15)−0.0069 (15)
C80.024 (2)0.037 (2)0.034 (2)−0.0096 (19)0.0050 (17)0.0030 (19)
C90.029 (2)0.041 (3)0.037 (3)0.005 (2)0.0020 (19)−0.002 (2)
C100.052 (3)0.021 (2)0.036 (3)0.002 (2)−0.008 (2)−0.0063 (19)
C110.059 (3)0.021 (2)0.038 (3)−0.018 (2)−0.010 (2)−0.0034 (18)
C120.034 (2)0.023 (2)0.034 (2)−0.0143 (18)−0.0036 (18)−0.0066 (17)
C130.0166 (18)0.0184 (17)0.0188 (18)−0.0097 (15)0.0005 (13)0.0001 (14)
C140.028 (2)0.028 (2)0.0212 (19)−0.0157 (17)−0.0014 (15)−0.0048 (16)
C150.028 (2)0.039 (2)0.036 (2)−0.022 (2)−0.0080 (18)−0.0006 (19)
C160.018 (2)0.044 (3)0.050 (3)−0.014 (2)0.0038 (19)−0.001 (2)
C170.027 (2)0.039 (2)0.042 (3)−0.014 (2)0.0114 (19)−0.014 (2)
C180.025 (2)0.031 (2)0.027 (2)−0.0131 (18)0.0035 (16)−0.0107 (17)
P20.0224 (5)0.0175 (5)0.0189 (5)−0.0093 (4)0.0024 (4)−0.0016 (4)
C190.0211 (19)0.0179 (18)0.0204 (19)−0.0075 (15)0.0013 (14)−0.0025 (14)
C200.023 (2)0.026 (2)0.023 (2)−0.0125 (17)0.0043 (15)−0.0042 (16)
C210.028 (2)0.027 (2)0.031 (2)−0.0122 (18)−0.0014 (17)−0.0075 (17)
C220.028 (2)0.028 (2)0.022 (2)−0.0044 (17)0.0003 (16)−0.0069 (16)
C230.026 (2)0.036 (2)0.027 (2)−0.0132 (18)0.0099 (16)−0.0074 (18)
C240.026 (2)0.029 (2)0.030 (2)−0.0164 (18)0.0043 (16)−0.0064 (17)
C250.025 (2)0.0205 (18)0.0159 (18)−0.0101 (16)−0.0001 (14)−0.0042 (14)
C260.030 (2)0.023 (2)0.031 (2)−0.0094 (17)−0.0072 (17)0.0006 (17)
C270.029 (2)0.033 (2)0.037 (3)−0.0099 (19)−0.0058 (18)−0.0071 (19)
C280.029 (2)0.043 (3)0.037 (2)−0.021 (2)0.0017 (18)−0.017 (2)
C290.041 (3)0.032 (2)0.037 (2)−0.026 (2)0.0030 (19)−0.0072 (19)
C300.026 (2)0.022 (2)0.027 (2)−0.0113 (17)−0.0017 (16)−0.0003 (16)
C310.0197 (19)0.0176 (18)0.028 (2)−0.0093 (15)−0.0018 (15)−0.0025 (15)
C320.030 (2)0.027 (2)0.030 (2)−0.0143 (18)−0.0019 (17)0.0007 (17)
C330.037 (3)0.026 (2)0.045 (3)−0.012 (2)−0.019 (2)0.0029 (19)
C340.027 (2)0.021 (2)0.078 (4)−0.0050 (19)−0.012 (2)−0.012 (2)
C350.031 (2)0.036 (2)0.067 (3)−0.017 (2)0.012 (2)−0.030 (2)
C360.027 (2)0.024 (2)0.037 (2)−0.0119 (17)0.0080 (17)−0.0120 (17)
P30.0187 (5)0.0153 (4)0.0220 (5)−0.0040 (4)0.0030 (4)−0.0053 (4)
C370.0191 (18)0.0171 (17)0.0217 (19)−0.0083 (15)0.0048 (14)−0.0052 (14)
C380.038 (2)0.0189 (19)0.028 (2)0.0028 (17)−0.0044 (18)−0.0102 (17)
C390.042 (3)0.030 (2)0.021 (2)−0.0032 (19)−0.0021 (18)−0.0040 (17)
C400.029 (2)0.0180 (19)0.034 (2)−0.0092 (17)−0.0018 (17)−0.0004 (16)
C410.056 (3)0.018 (2)0.040 (3)0.001 (2)−0.002 (2)−0.0139 (19)
C420.056 (3)0.021 (2)0.027 (2)−0.004 (2)0.003 (2)−0.0098 (17)
C430.0198 (19)0.0166 (18)0.023 (2)−0.0013 (15)−0.0009 (15)−0.0047 (15)
C440.031 (2)0.027 (2)0.038 (2)−0.0101 (18)0.0007 (18)−0.0077 (18)
C450.039 (3)0.045 (3)0.049 (3)−0.018 (2)−0.006 (2)−0.018 (2)
C460.059 (3)0.048 (3)0.031 (3)−0.017 (3)−0.010 (2)−0.013 (2)
C470.053 (3)0.052 (3)0.023 (2)−0.021 (2)0.005 (2)−0.011 (2)
C480.034 (2)0.034 (2)0.023 (2)−0.0154 (19)0.0020 (17)−0.0057 (17)
C490.0218 (19)0.0220 (19)0.0184 (18)−0.0079 (16)0.0012 (14)−0.0043 (15)
C500.027 (2)0.0207 (19)0.031 (2)−0.0076 (17)0.0029 (16)−0.0066 (16)
C510.042 (3)0.023 (2)0.035 (2)−0.0167 (19)0.0056 (19)−0.0067 (17)
C520.045 (3)0.042 (2)0.022 (2)−0.030 (2)0.0044 (18)−0.0062 (18)
C530.023 (2)0.037 (2)0.030 (2)−0.0130 (18)−0.0003 (16)−0.0020 (18)
C540.024 (2)0.025 (2)0.033 (2)−0.0100 (17)0.0039 (16)−0.0072 (17)
Cl0.096 (2)0.203 (4)0.203 (4)0.028 (2)−0.019 (2)−0.152 (3)
C550.042 (8)0.072 (10)0.119 (14)−0.006 (7)0.044 (9)0.001 (9)
Geometric parameters (Å, °) top
W—S12.2621 (9)C24—H240.950
W—S22.2464 (9)C25—C261.399 (5)
W—S32.2423 (10)C25—C301.389 (5)
W—S42.1440 (11)C26—H260.950
Ag1—S12.5341 (11)C26—C271.380 (6)
Ag1—S32.5683 (9)C27—H270.950
Ag1—I3.0689 (7)C27—C281.388 (6)
Ag1—P12.3927 (9)C28—H280.950
Ag2—S12.5631 (10)C28—C291.375 (6)
Ag2—S22.5718 (10)C29—H290.950
Ag2—I3.0683 (9)C29—C301.396 (5)
Ag2—P22.3961 (10)C30—H300.950
Ag3—S22.5892 (11)C31—C321.410 (5)
Ag3—S32.6319 (10)C31—C361.394 (5)
Ag3—I3.0231 (5)C32—H320.950
Ag3—P32.4150 (10)C32—C331.378 (6)
P1—C11.830 (4)C33—H330.950
P1—C71.823 (4)C33—C341.368 (7)
P1—C131.827 (4)C34—H340.950
C1—C21.396 (5)C34—C351.370 (7)
C1—C61.385 (5)C35—H350.950
C2—H20.950C35—C361.395 (6)
C2—C31.383 (5)C36—H360.950
C3—H30.950P3—C371.830 (4)
C3—C41.381 (5)P3—C431.833 (4)
C4—H40.950P3—C491.829 (4)
C4—C51.382 (6)C37—C381.387 (5)
C5—H50.950C37—C421.386 (5)
C5—C61.396 (5)C38—H380.950
C6—H60.950C38—C391.392 (5)
C7—C81.395 (5)C39—H390.950
C7—C121.386 (5)C39—C401.373 (5)
C8—H80.950C40—H400.950
C8—C91.390 (6)C40—C411.368 (6)
C9—H90.950C41—H410.950
C9—C101.375 (7)C41—C421.397 (6)
C10—H100.950C42—H420.950
C10—C111.366 (7)C43—C441.385 (5)
C11—H110.950C43—C481.395 (5)
C11—C121.389 (5)C44—H440.950
C12—H120.950C44—C451.391 (6)
C13—C141.405 (5)C45—H450.950
C13—C181.384 (5)C45—C461.387 (7)
C14—H140.950C46—H460.950
C14—C151.373 (5)C46—C471.374 (7)
C15—H150.950C47—H470.950
C15—C161.392 (6)C47—C481.394 (6)
C16—H160.950C48—H480.950
C16—C171.376 (6)C49—C501.393 (5)
C17—H170.950C49—C541.397 (5)
C17—C181.389 (5)C50—H500.950
C18—H180.950C50—C511.397 (5)
P2—C191.830 (4)C51—H510.950
P2—C251.833 (4)C51—C521.375 (6)
P2—C311.819 (4)C52—H520.950
C19—C201.397 (5)C52—C531.392 (6)
C19—C241.393 (5)C53—H530.950
C20—H200.950C53—C541.390 (5)
C20—C211.390 (5)C54—H540.950
C21—H210.950Cl—C551.851 (17)
C21—C221.375 (5)Cl—C55i1.862 (16)
C22—H220.950C55—Cli1.862 (16)
C22—C231.384 (6)C55—H55A0.990
C23—H230.950C55—H55B0.990
C23—C241.397 (5)
S1—W—S2111.00 (3)C21—C22—C23120.4 (4)
S1—W—S3110.99 (3)H22—C22—C23119.8
S1—W—S4107.87 (4)C22—C23—H23120.0
S2—W—S3110.95 (3)C22—C23—C24119.9 (4)
S2—W—S4107.43 (4)H23—C23—C24120.0
S3—W—S4108.45 (4)C19—C24—C23120.1 (3)
S1—Ag1—S393.35 (3)C19—C24—H24120.0
S1—Ag1—I99.88 (3)C23—C24—H24120.0
S1—Ag1—P1128.00 (3)P2—C25—C26117.6 (3)
S3—Ag1—I99.25 (2)P2—C25—C30123.1 (3)
S3—Ag1—P1126.77 (3)C26—C25—C30119.3 (3)
I—Ag1—P1103.73 (3)C25—C26—H26119.8
S1—Ag2—S292.71 (3)C25—C26—C27120.4 (4)
S1—Ag2—I99.23 (3)H26—C26—C27119.8
S1—Ag2—P2123.93 (3)C26—C27—H27119.9
S2—Ag2—I103.11 (3)C26—C27—C28120.2 (4)
S2—Ag2—P2128.24 (3)H27—C27—C28119.9
I—Ag2—P2104.95 (3)C27—C28—H28120.2
S2—Ag3—S390.19 (3)C27—C28—C29119.6 (4)
S2—Ag3—I103.92 (3)H28—C28—C29120.2
S2—Ag3—P3126.86 (3)C28—C29—H29119.6
S3—Ag3—I98.97 (2)C28—C29—C30120.9 (4)
S3—Ag3—P3122.69 (3)H29—C29—C30119.6
I—Ag3—P3109.54 (3)C25—C30—C29119.5 (4)
W—S1—Ag176.58 (3)C25—C30—H30120.2
W—S1—Ag275.80 (3)C29—C30—H30120.2
Ag1—S1—Ag288.04 (3)P2—C31—C32122.9 (3)
W—S2—Ag275.89 (3)P2—C31—C36118.2 (3)
W—S2—Ag377.27 (3)C32—C31—C36119.0 (3)
Ag2—S2—Ag383.52 (3)C31—C32—H32119.9
W—S3—Ag176.20 (3)C31—C32—C33120.1 (4)
W—S3—Ag376.44 (3)H32—C32—C33119.9
Ag1—S3—Ag387.30 (3)C32—C33—H33120.0
Ag1—I—Ag270.505 (16)C32—C33—C34120.0 (4)
Ag1—I—Ag372.199 (14)H33—C33—C34120.0
Ag2—I—Ag368.704 (14)C33—C34—H34119.4
Ag1—P1—C1116.19 (11)C33—C34—C35121.2 (4)
Ag1—P1—C7113.08 (12)H34—C34—C35119.4
Ag1—P1—C13112.69 (12)C34—C35—H35120.0
C1—P1—C7104.13 (16)C34—C35—C36120.1 (4)
C1—P1—C13103.49 (16)H35—C35—C36120.0
C7—P1—C13106.22 (16)C31—C36—C35119.6 (4)
P1—C1—C2117.8 (3)C31—C36—H36120.2
P1—C1—C6123.5 (3)C35—C36—H36120.2
C2—C1—C6118.6 (3)Ag3—P3—C37117.03 (12)
C1—C2—H2119.7Ag3—P3—C43113.15 (12)
C1—C2—C3120.6 (4)Ag3—P3—C49112.36 (12)
H2—C2—C3119.7C37—P3—C43102.27 (16)
C2—C3—H3119.6C37—P3—C49104.46 (16)
C2—C3—C4120.7 (4)C43—P3—C49106.46 (17)
H3—C3—C4119.6P3—C37—C38119.1 (3)
C3—C4—H4120.4P3—C37—C42122.7 (3)
C3—C4—C5119.2 (4)C38—C37—C42118.2 (3)
H4—C4—C5120.4C37—C38—H38119.3
C4—C5—H5119.7C37—C38—C39121.4 (4)
C4—C5—C6120.5 (4)H38—C38—C39119.3
H5—C5—C6119.7C38—C39—H39120.4
C1—C6—C5120.4 (4)C38—C39—C40119.3 (4)
C1—C6—H6119.8H39—C39—C40120.4
C5—C6—H6119.8C39—C40—H40119.8
P1—C7—C8116.6 (3)C39—C40—C41120.4 (4)
P1—C7—C12124.4 (3)H40—C40—C41119.8
C8—C7—C12119.0 (4)C40—C41—H41119.9
C7—C8—H8119.9C40—C41—C42120.3 (4)
C7—C8—C9120.2 (4)H41—C41—C42119.9
H8—C8—C9119.9C37—C42—C41120.3 (4)
C8—C9—H9120.0C37—C42—H42119.8
C8—C9—C10119.9 (4)C41—C42—H42119.8
H9—C9—C10120.0P3—C43—C44117.7 (3)
C9—C10—H10119.9P3—C43—C48122.4 (3)
C9—C10—C11120.2 (4)C44—C43—C48119.8 (4)
H10—C10—C11119.9C43—C44—H44120.0
C10—C11—H11119.6C43—C44—C45120.1 (4)
C10—C11—C12120.7 (4)H44—C44—C45120.0
H11—C11—C12119.6C44—C45—H45120.1
C7—C12—C11119.9 (4)C44—C45—C46119.7 (4)
C7—C12—H12120.0H45—C45—C46120.1
C11—C12—H12120.0C45—C46—H46119.7
P1—C13—C14120.8 (3)C45—C46—C47120.5 (4)
P1—C13—C18119.9 (3)H46—C46—C47119.7
C14—C13—C18119.3 (3)C46—C47—H47120.0
C13—C14—H14119.8C46—C47—C48120.0 (4)
C13—C14—C15120.3 (4)H47—C47—C48120.0
H14—C14—C15119.8C43—C48—C47119.8 (4)
C14—C15—H15120.2C43—C48—H48120.1
C14—C15—C16119.6 (4)C47—C48—H48120.1
H15—C15—C16120.2P3—C49—C50118.5 (3)
C15—C16—H16119.7P3—C49—C54122.9 (3)
C15—C16—C17120.6 (4)C50—C49—C54118.6 (3)
H16—C16—C17119.7C49—C50—H50119.9
C16—C17—H17120.0C49—C50—C51120.2 (4)
C16—C17—C18120.0 (4)H50—C50—C51119.9
H17—C17—C18120.0C50—C51—H51119.6
C13—C18—C17120.2 (4)C50—C51—C52120.8 (4)
C13—C18—H18119.9H51—C51—C52119.6
C17—C18—H18119.9C51—C52—H52120.2
Ag2—P2—C19114.01 (12)C51—C52—C53119.7 (4)
Ag2—P2—C25113.98 (12)H52—C52—C53120.2
Ag2—P2—C31113.57 (12)C52—C53—H53120.1
C19—P2—C25103.73 (16)C52—C53—C54119.9 (4)
C19—P2—C31104.17 (17)H53—C53—C54120.1
C25—P2—C31106.36 (16)C49—C54—C53120.9 (4)
P2—C19—C20118.0 (3)C49—C54—H54119.6
P2—C19—C24122.7 (3)C53—C54—H54119.6
C20—C19—C24119.2 (3)C55—Cl—C55i81.4 (7)
C19—C20—H20119.9Cl—C55—Cli98.6 (7)
C19—C20—C21120.2 (3)Cl—C55—H55A112.1
H20—C20—C21119.9Cli—C55—H55A112.1
C20—C21—H21119.9Cl—C55—H55B112.1
C20—C21—C22120.3 (4)Cli—C55—H55B112.1
H21—C21—C22119.9H55A—C55—H55B109.7
C21—C22—H22119.8
S2—W—S1—Ag1109.50 (3)C7—P1—C13—C1467.3 (3)
S2—W—S1—Ag218.11 (4)C7—P1—C13—C18−112.4 (3)
S3—W—S1—Ag1−14.38 (3)P1—C13—C14—C15−176.7 (3)
S3—W—S1—Ag2−105.76 (3)C18—C13—C14—C153.1 (5)
S4—W—S1—Ag1−133.06 (3)C13—C14—C15—C16−1.8 (6)
S4—W—S1—Ag2135.56 (3)C14—C15—C16—C17−0.4 (6)
S3—Ag1—S1—W11.70 (3)C15—C16—C17—C181.5 (7)
S3—Ag1—S1—Ag287.57 (3)P1—C13—C18—C17177.7 (3)
I—Ag1—S1—W−88.30 (2)C14—C13—C18—C17−2.1 (6)
I—Ag1—S1—Ag2−12.43 (2)C16—C17—C18—C13−0.2 (6)
P1—Ag1—S1—W155.48 (3)S1—Ag2—P2—C19−33.44 (14)
P1—Ag1—S1—Ag2−128.65 (4)S1—Ag2—P2—C2585.41 (13)
S2—Ag2—S1—W−14.70 (3)S1—Ag2—P2—C31−152.55 (13)
S2—Ag2—S1—Ag1−91.35 (3)S2—Ag2—P2—C19−160.48 (13)
I—Ag2—S1—W89.05 (2)S2—Ag2—P2—C25−41.64 (14)
I—Ag2—S1—Ag112.41 (3)S2—Ag2—P2—C3180.40 (14)
P2—Ag2—S1—W−155.83 (3)I—Ag2—P2—C1978.89 (13)
P2—Ag2—S1—Ag1127.52 (4)I—Ag2—P2—C25−162.27 (13)
S1—W—S2—Ag2−18.04 (4)I—Ag2—P2—C31−40.23 (13)
S1—W—S2—Ag3−104.46 (3)Ag2—P2—C19—C20−40.0 (3)
S3—W—S2—Ag2105.85 (3)Ag2—P2—C19—C24141.6 (3)
S3—W—S2—Ag319.43 (4)C25—P2—C19—C20−164.6 (3)
S4—W—S2—Ag2−135.76 (4)C25—P2—C19—C2417.1 (3)
S4—W—S2—Ag3137.82 (4)C31—P2—C19—C2084.3 (3)
S1—Ag2—S2—W14.80 (3)C31—P2—C19—C24−94.1 (3)
S1—Ag2—S2—Ag393.26 (3)P2—C19—C20—C21−178.2 (3)
I—Ag2—S2—W−85.33 (3)C24—C19—C20—C210.2 (5)
I—Ag2—S2—Ag3−6.87 (2)C19—C20—C21—C220.5 (6)
P2—Ag2—S2—W153.28 (4)C20—C21—C22—C23−0.7 (6)
P2—Ag2—S2—Ag3−128.27 (4)C21—C22—C23—C240.2 (6)
S3—Ag3—S2—W−15.35 (3)P2—C19—C24—C23177.7 (3)
S3—Ag3—S2—Ag2−92.29 (3)C20—C19—C24—C23−0.7 (6)
I—Ag3—S2—W83.94 (3)C22—C23—C24—C190.5 (6)
I—Ag3—S2—Ag27.00 (2)Ag2—P2—C25—C26−37.4 (3)
P3—Ag3—S2—W−148.00 (3)Ag2—P2—C25—C30145.3 (3)
P3—Ag3—S2—Ag2135.06 (4)C19—P2—C25—C2687.2 (3)
S1—W—S3—Ag114.20 (3)C19—P2—C25—C30−90.1 (3)
S1—W—S3—Ag3104.73 (3)C31—P2—C25—C26−163.3 (3)
S2—W—S3—Ag1−109.70 (3)C31—P2—C25—C3019.4 (4)
S2—W—S3—Ag3−19.17 (4)P2—C25—C26—C27−176.4 (3)
S4—W—S3—Ag1132.53 (3)C30—C25—C26—C271.0 (6)
S4—W—S3—Ag3−136.94 (3)C25—C26—C27—C28−0.4 (6)
S1—Ag1—S3—W−11.82 (3)C26—C27—C28—C29−0.8 (6)
S1—Ag1—S3—Ag3−88.52 (3)C27—C28—C29—C301.4 (6)
I—Ag1—S3—W88.76 (3)P2—C25—C30—C29176.9 (3)
I—Ag1—S3—Ag312.06 (2)C26—C25—C30—C29−0.4 (6)
P1—Ag1—S3—W−156.29 (3)C28—C29—C30—C25−0.8 (6)
P1—Ag1—S3—Ag3127.02 (4)Ag2—P2—C31—C32153.2 (3)
S2—Ag3—S3—W15.43 (3)Ag2—P2—C31—C36−24.9 (3)
S2—Ag3—S3—Ag191.89 (3)C19—P2—C31—C3228.6 (3)
I—Ag3—S3—W−88.69 (2)C19—P2—C31—C36−149.5 (3)
I—Ag3—S3—Ag1−12.24 (2)C25—P2—C31—C32−80.6 (3)
P3—Ag3—S3—W151.06 (3)C25—P2—C31—C36101.2 (3)
P3—Ag3—S3—Ag1−132.48 (3)P2—C31—C32—C33−180.0 (3)
S2—Ag3—I—Ag1−81.71 (3)C36—C31—C32—C33−1.8 (5)
S2—Ag3—I—Ag2−6.25 (2)C31—C32—C33—C340.8 (6)
S3—Ag3—I—Ag110.72 (2)C32—C33—C34—C350.4 (6)
S3—Ag3—I—Ag286.19 (2)C33—C34—C35—C36−0.6 (6)
P3—Ag3—I—Ag1140.24 (3)P2—C31—C36—C35179.9 (3)
P3—Ag3—I—Ag2−144.30 (3)C32—C31—C36—C351.7 (5)
S1—Ag2—I—Ag1−10.84 (2)C34—C35—C36—C31−0.5 (6)
S1—Ag2—I—Ag3−88.71 (2)S2—Ag3—P3—C37−81.18 (13)
S2—Ag2—I—Ag184.15 (2)S2—Ag3—P3—C4337.35 (14)
S2—Ag2—I—Ag36.27 (2)S2—Ag3—P3—C49157.96 (13)
P2—Ag2—I—Ag1−139.79 (3)S3—Ag3—P3—C37159.75 (13)
P2—Ag2—I—Ag3142.33 (3)S3—Ag3—P3—C43−81.72 (13)
S1—Ag1—I—Ag210.99 (2)S3—Ag3—P3—C4938.89 (13)
S1—Ag1—I—Ag384.07 (2)I—Ag3—P3—C3744.64 (13)
S3—Ag1—I—Ag2−84.09 (2)I—Ag3—P3—C43163.17 (13)
S3—Ag1—I—Ag3−11.00 (2)I—Ag3—P3—C49−76.23 (13)
P1—Ag1—I—Ag2144.30 (3)Ag3—P3—C37—C38−36.4 (4)
P1—Ag1—I—Ag3−142.62 (3)Ag3—P3—C37—C42144.7 (3)
S1—Ag1—P1—C151.69 (14)C43—P3—C37—C38−160.6 (3)
S1—Ag1—P1—C7−68.66 (14)C43—P3—C37—C4220.4 (4)
S1—Ag1—P1—C13170.85 (12)C49—P3—C37—C3888.6 (3)
S3—Ag1—P1—C1−175.74 (13)C49—P3—C37—C42−90.4 (4)
S3—Ag1—P1—C763.92 (14)P3—C37—C38—C39−177.8 (3)
S3—Ag1—P1—C13−56.57 (13)C42—C37—C38—C391.2 (6)
I—Ag1—P1—C1−62.83 (13)C37—C38—C39—C400.1 (7)
I—Ag1—P1—C7176.82 (13)C38—C39—C40—C41−1.0 (7)
I—Ag1—P1—C1356.33 (12)C39—C40—C41—C420.6 (7)
Ag1—P1—C1—C241.8 (3)P3—C37—C42—C41177.4 (4)
Ag1—P1—C1—C6−141.1 (3)C38—C37—C42—C41−1.6 (7)
C7—P1—C1—C2166.8 (3)C40—C41—C42—C370.7 (7)
C7—P1—C1—C6−16.1 (4)Ag3—P3—C43—C44−39.6 (3)
C13—P1—C1—C2−82.3 (3)Ag3—P3—C43—C48142.8 (3)
C13—P1—C1—C694.8 (3)C37—P3—C43—C4487.2 (3)
P1—C1—C2—C3176.9 (3)C37—P3—C43—C48−90.4 (3)
C6—C1—C2—C3−0.4 (6)C49—P3—C43—C44−163.5 (3)
C1—C2—C3—C41.0 (6)C49—P3—C43—C4818.9 (3)
C2—C3—C4—C5−0.8 (6)P3—C43—C44—C45−176.1 (3)
C3—C4—C5—C60.0 (6)C48—C43—C44—C451.7 (6)
P1—C1—C6—C5−177.6 (3)C43—C44—C45—C46−0.8 (6)
C2—C1—C6—C5−0.5 (6)C44—C45—C46—C47−0.5 (7)
C4—C5—C6—C10.6 (6)C45—C46—C47—C481.0 (7)
Ag1—P1—C7—C846.9 (3)C46—C47—C48—C43−0.1 (7)
Ag1—P1—C7—C12−132.4 (3)P3—C43—C48—C47176.4 (3)
C1—P1—C7—C8−80.1 (3)C44—C43—C48—C47−1.2 (6)
C1—P1—C7—C12100.6 (3)Ag3—P3—C49—C50−24.5 (3)
C13—P1—C7—C8171.0 (3)Ag3—P3—C49—C54155.5 (3)
C13—P1—C7—C12−8.3 (4)C37—P3—C49—C50−152.3 (3)
P1—C7—C8—C9177.4 (3)C37—P3—C49—C5427.6 (4)
C12—C7—C8—C9−3.2 (6)C43—P3—C49—C5099.9 (3)
C7—C8—C9—C101.7 (7)C43—P3—C49—C54−80.1 (3)
C8—C9—C10—C110.9 (7)P3—C49—C50—C51179.9 (3)
C9—C10—C11—C12−2.0 (7)C54—C49—C50—C510.0 (6)
P1—C7—C12—C11−178.6 (3)C49—C50—C51—C52−0.4 (6)
C8—C7—C12—C112.0 (6)C50—C51—C52—C531.0 (6)
C10—C11—C12—C70.5 (6)C51—C52—C53—C54−1.2 (6)
Ag1—P1—C13—C14−168.3 (2)C52—C53—C54—C490.8 (6)
Ag1—P1—C13—C1811.9 (3)P3—C49—C54—C53179.9 (3)
C1—P1—C13—C14−42.0 (3)C50—C49—C54—C53−0.2 (6)
C1—P1—C13—C18138.2 (3)C55i—Cl—C55—Cli0.0
Symmetry codes: (i) −x+2, −y, −z.
Table 1
Selected geometric parameters (Å, °) top
W—S12.2621 (9)Ag2—S12.5631 (10)
W—S22.2464 (9)Ag2—S22.5718 (10)
W—S32.2423 (10)Ag2—I3.0683 (9)
W—S42.1440 (11)Ag2—P22.3961 (10)
Ag1—S12.5341 (11)Ag3—S22.5892 (11)
Ag1—S32.5683 (9)Ag3—S32.6319 (10)
Ag1—I3.0689 (7)Ag3—I3.0231 (5)
Ag1—P12.3927 (9)Ag3—P32.4150 (10)
S1—W—S2111.00 (3)S2—Ag3—S390.19 (3)
S1—W—S3110.99 (3)S2—Ag3—I103.92 (3)
S1—W—S4107.87 (4)S2—Ag3—P3126.86 (3)
S2—W—S3110.95 (3)S3—Ag3—I98.97 (2)
S2—W—S4107.43 (4)S3—Ag3—P3122.69 (3)
S3—W—S4108.45 (4)I—Ag3—P3109.54 (3)
S1—Ag1—S393.35 (3)W—S1—Ag176.58 (3)
S1—Ag1—I99.88 (3)W—S1—Ag275.80 (3)
S1—Ag1—P1128.00 (3)Ag1—S1—Ag288.04 (3)
S3—Ag1—I99.25 (2)W—S2—Ag275.89 (3)
S3—Ag1—P1126.77 (3)W—S2—Ag377.27 (3)
I—Ag1—P1103.73 (3)Ag2—S2—Ag383.52 (3)
S1—Ag2—S292.71 (3)W—S3—Ag176.20 (3)
S1—Ag2—I99.23 (3)W—S3—Ag376.44 (3)
S1—Ag2—P2123.93 (3)Ag1—S3—Ag387.30 (3)
S2—Ag2—I103.11 (3)Ag1—I—Ag270.505 (16)
S2—Ag2—P2128.24 (3)Ag1—I—Ag372.199 (14)
I—Ag2—P2104.95 (3)Ag2—I—Ag368.704 (14)
Acknowledgements top

We thank the EPSRC (UK) and Shahid Chamran University for financial support.

references
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