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Thermolysis of a benzene solution containing Fe(CO) 5 and ferrocenylacetylene yielded three new compounds: [Fe(CO) 2 {η 5 -2,5-Fc 2 C 5 H 2 CO}C(Fc)dCH] (1), [Fe(CO) 2 {η 2 :η 2 -2,5-Fc 2 C 4 H 2 -Fe(CO) 3 }-µ-CO] (2), and [Fe(CO) 3 {η 2 :η 2 -2,5-Fc 2 C 4 H 2 CO}] (3). When a benzene solution containing ferrocenylacetylene and M(CO) 6 (M ) Mo, W) was refluxed, 1,2,4-triferrocenylbenzene (4) was formed. In contrast to the reaction of ferrocenylacetylene with Fe(CO) 5 , which leads to cyclization with insertion of a CO molecule, in the reaction with M(CO) 6 no insertion of CO takes place during cyclization. However, if the reactions with M(CO) 6 are carried out in the presence of S 8 -powder or Se-powder, insertion of these chalcogen atoms during cyclization does take place and 2,5-diferrocenylthiophene (5) and 2,5-diferrocenylselenophene (6) are formed respectively, along with 4. All new compounds were characterized by IR and 1 H and 13 C NMR spectroscopy. Structures of 1-5 were established by singlecrystal X-ray crystallography.

(Triphenylphosphine)(selenourea)gold(I) chloride [Ph3PAuSeC‐ (NH2)2]+ Cl‐ (1) and the corresponding dppm derivative dppm[AuSeC(NH2)2]22+ 2l‐ (2) are prepared from SeC‐ (NH2)2 and the appropriate chloro(phosphine)gold(I) complex. The reaction between 1 and aqueous Na2CO3 leads to the neutral complex μ‐selenido{bis[(triphenylphosphine)gold(I)]} (Ph3PAu)2Se (3). An analogous reaction with 2 leads to a dark red oil, which has not yet been characterized. The reaction between 3, Ph3PAuCl, and AgSbF6 leads to the ionic complex [(Ph3PAu)3Se]+SbF6‐ (4) in good yield. X‐ray structure analyses of 1,2, and 3 confirm the expected linear geometry at the gold atom and reveal short intramolecular Au – Au contacts for 2 and 3. Short nonbonding distances between the nitrogen atoms of the amino groups and the chloride ions in the crystal structures of 1 and 2 probably indicate hydrogen bonds.

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