Tetrakis(diethyl ether)tetra-μ4-oxido-octakis(pentafluorophenyl)octazinc

Molecules of the title compound, [Zn8(C6F5)8O4(C4H10O)4], are located on a special position of site symmetry . As a result, there is just one quarter-molecule in the asymmetric unit. The title compound features a Zn4O4 cube. Each Zn atom in the cube carries a pentafluorophenyl substituent. Each O atom is bonded to a further Zn atom, which is connected to a pentafluorophenyl substituent and the O atom of a diethyl ether molecule. All ether C atoms are disordered over two sets of sites with a site occupation factor of 0.51 (2) for the major occupied site.

Molecules of the title compound, [Zn 8 (C 6 F 5 ) 8 O 4 (C 4 H 10 O) 4 ], are located on a special position of site symmetry 4. As a result, there is just one quarter-molecule in the asymmetric unit. The title compound features a Zn 4 O 4 cube. Each Zn atom in the cube carries a pentafluorophenyl substituent. Each O atom is bonded to a further Zn atom, which is connected to a pentafluorophenyl substituent and the O atom of a diethyl ether molecule. All ether C atoms are disordered over two sets of sites with a site occupation factor of 0.51 (2) for the major occupied site.
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: KJ2188). towards water has not yet been investigated well. Very recently we have studied the chemical behavior of a series of mesityl derivatives of group 12 elements (Hayashi et al., 2011). It has been shown that the Zn derivative Zn[Mes] 2 is more reactive towards acids than M[Mes] 2 (M = Cd, Hg). In this paper we report the crystal structure of the product which was obtained from the 1 : 1 reaction of (Et 2 O) 2 Zn[C 6 F 5 ] 2 with water. Bis(pentafluorophenyl)zinc was synthesized by slight modification of the method reported in the literature via conversion of Mg[C 6 F 5 ]Br with ZnCl 2 in diethyl ether (Noltes & van den Hurk, 1964;Sun et al., 1998). It is interesting to note that the partial hydrolysis of (Et 2 O) 2 Zn[C 6 F 5 ] 2 yields the oxide [C 6 F 5 (Et 2 O)ZnOZnC 6 F 5 ] 4 whereas the 1 : 1 reaction of the corresponding Cd[C 6 F 5 ] 2 with water produces the hydroxy derivative [C 6 F 5 CdOH] 4 (Weidenbruch et al., 1989). In the solid state the Cd hydroxide [C 6 F 5 CdOH] 4 also displays a heterocubane structure.
Molecules of the title compound, C 64 H 40 F 40 O 8 Zn 8 , are located on a special position of site symmetry 4. As a result of that, there is just a quarter of a molecule in the asymmetric unit. The title compound features an Zn 4 O 4 cube. Each Zn atom in the cube carries a pentafluorophenyl substituent. Each O atom is bonded to a further Zn atom which is connected to a pentafluorophenyl substituent and the O atom of a diethyl ether molecule.

Experimental
All transformations were carried out under an atmosphere of dry nitrogen using Schlenk techniques. Solvents (diethyl ether, toluene) were freshly distilled from sodium/benzophenone and hexane from sodium prior to use. NMR spectra were recorded on a Bruker Avance 300 ( 1 H, 19 F{ 1 H} and a DPX 250 ( 13 C{ 1 H}). Chemical shift values ( 1 H, 13 C{ 1 H}) are reported in p.p.m. relative to SiMe 4 and were referenced to residual solvent signals. The 19 F{ 1 H} NMR chemical shift values were referenced to external CFCl 3 . The MALDI spectrum was recorded on a FISONS Instruments VG TofSpec using ATT as a matrix. Abbreviations: d = doublet, t = triplet, q = quartet, m = multiplet, br = broad, n.o. = signal not observed.
Under stirring, a solution of Mg[C 6 F 5 ]Br in diethyl ether (79.4 mmol, 100 ml) was added via canula and the mixture was allowed to warm to room temperature over night. Insoluble material was removed by filtration and the solvent was evaporated under reduced pressure. A viscous brown slurry was obtained which was heated to 140°C for a period of approximately 3 h. The residue obtained was dissolved in a 2 : 1 mixture of toluene and hexane and stored at -30°C for 24 h. After the first crystal crop of (Et 2 O) 2 Zn[C 6 F 5 ] 2 had been separated the mother liquor was stored at -30°C for a period of approximately two months yielding crystals of the title compound. This can be attributed to the intrusion of moisture over the period of