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(NBu4)[CoCl3(PPh3)] reacts with Se(SiMe3)2 to form the new clusters [Co8Se8(PPh3)6][CoCl3(PPh3)] (6) and [Co8Se8(PPh3)6][Co6Se8(PPh3)6] (7). The structures of 6 and 7 have been determ ined by X-ray diffraction. 6 and 7 crystallize in the space group P1̄ with two formula units per unit cell and with the following lattice constants at 180 K: 6: a = 1413.8(10), b - 2224.2(23), c = 2348.4(17) pm, α = 86.06(5), β = 86.58(5), γ = 76.11(5)°; 7: a = 1465.9(4), b = 1627.6(6), c = 2505.7(6) pm, α - 98.69(2), β = 96.23(2), γ = 113.06(2)°. The cluster structures of the [Co8Se8(PPh3)6]n (n = 0, 1 +) depend on the total number of electrons in the cluster units.
MoF4(NCl) has been prepared as a yellow crystal powder by the reaction of diluted fluorine with MoCl3(N3S2) at room temperature. The compound is associated via fluorine bridges, according to the IR spectrum. With acetonitrile, the monomeric complex [CH3CN -MoF4(NCl)] is obtained, which was characterized by its IR and 19F NMR spectra as well as by an X-ray structure determination. Crystal data: space group Pm, Z = 2 (1068 observed, independent reflexions, R = 0.03). Lattice dimensions at -90 °C: a = 507.1. b = 704.8, c = 995.8 pm, β = 102.02°. The unit cell contains two crystallographically independent molecules [CH3CN -MoF4(NCl)], the Mo≡N-Cl groups being linear (bond angles 176°, 178°) with bond lengths MoN = 172 and NCI = 159, 162 pm. In the trans position to the MoNCl group, the nitrogen atom of the acetonitrile molecule is coordinated.
(η5-C5H5)Fe(CO)2Br reacts with Se(SiMe3)2 to form the title compound 1, which has been characterized by X-ray crystal structural analysis. 1 crystallizes in the space group P212121 with 4 formula units per unit cell. 1 consists of [Se{Fe(CO)2(C5H 5)}3]+- cations and [Fe4Se4Br4]2--anions, the latter with a heterocubane structure.