Synthesis and Crystal Structures of Copper(I) and Gold(I) Complexes [C(NH 2 ) 3 ] 2 [M 2 (1,2–dithiosquarate) 2 ], M = Cu, Au, Containing Short M···M Distances, and of the Gold(III) Complex ( cyclo PrPh 3 P)[Au(1,2‐dithiosquarate) 2 ]

The new compounds [C(NH 2 ) 3 ] 2 [Cu 2 (dtsq) 2 ] ( 1 ), [C(NH 2 ) 3 ] 2 ‐[Au 2 (dtsq) 2 ] · H 2 O ( 2 ), and ( cyclo PrPh 3 P)[Au(dtsq) 2 ] ( 3 , cyclo Pr = cyclopropyl) have been prepared from CuSO 4 · 5 H 2 O, KAuCl 4 , and K 2 dtsq · H 2 O (dtsq = dianion of 1,2‐dithiosquaric acid, C 4 O 2 S 2− 2 ). Compounds 1 and 2 contain pairs of metal atoms with short intermetallic distances of 2.587(2) (Cu···Cu) and 2.846(2) Å (Au···Au). Cu(I) is trigonally coordinated to three sulfur atoms of three different ligands and lies 0.51 Å above the S 3 plane. It is oriented towards the copper atom of a second CuS 3 unit related to the first one by a center of inversion. Au(I) shows a linear coordination, leading to the formation of Au 2 (dtsq) 2− 2 dimers. These have intermolecular Au···Au distances of 3.259(2) Å. Compound 3 contains isolated Au(dtsq) − 2 ions with square planar coordination geometry stacked along the a axis at 4.708 Å distance.