Kr. Dunbar et al., A MIXED-METAL SALT COMPRISED OF METAL-METAL BONDED DINUCLEAR IONS - STRUCTURE AND PROPERTIES OF [RH2(OAC)2(MECN)6][RE2CL8], Inorganica Chimica Acta, 217(1-2), 1994, pp. 79-84
The unusual salt [Rh2(OAc)2(MeCN)6][Re2Cl8] (1) is produced from a met
hathetic reaction of the salt [NBu4n]2[Re2Cl8] with [Rh2(OAc)2(MeCN)6]
[BF4]2. Crystal data for 1: Pccn, a = 27.42(l), b = 26.736(4), c = 18.
137(5) angstrom, V = 13.296(7) angstrom3, Z = 16, D(calc) = 2.450 g/cm
3, mu(Mo Kalpha) = 90.05 cm-1, R = 0.078, R(w) = 0.109 for 483 paramet
ers and 5229 data with F(o)2 > 3sigma(F(o))2. The new salt constitutes
the only example of a structure wherein the octachlorodirhenate unit
is present in three different crystallographic environments in the sam
e unit cell. The asymmetric unit contains two independent [Rh2]2+ cati
ons together with one [Re2Cl8]2- anion at full occupancy and two dirhe
nium anions each at half-occupancy. The synthesis, structure, key spec
troscopic properties and solution behavior of 1 are presented and disc
ussed.