Hydroxypivaldehyde represents an important intermediate in the production of neopentyl glycol, which in turn is widely applied in the production of e.g. polyesters, plasticizers, synthetic resin paints and lubricants.

The reactions of As 2 O 3 , SbCl 3 , and (BiO) 2 CO 3 with oleum (65 % SO 3 ) yielded single crystals of As(S 2 O 7 )(HS 2 O 7 ) [monoclinic, P2 1 /c, Z = 4, a = 16.549(1), b = 6.6743(5), c = 9.9498(6) Å, β = 102.672(8)°, V = 1072.672(8) Å 3 ], Sb 2 (SO 4 ) 2 (S 2 O 7 ) [monoclinic, P2 1 /n, Z = 4, a = 9.1586(2), b = 6.9981(2), c = 17.7956(4) Å, β = 100.9690(8)°, V = 1119.73(5) Å 3 ], and Bi 2 (S 2 O 7 ) 3 [triclinic, P1, Z = 2, a = 6.5734(1), b = 10.1954(2), c = 11.5121(2) Å, α = 90.996(1)°, β = 96.976(1)°, γ = 94.870(1)°, V = 762.75(2) Å 3 ]. As(S 2 O 7 )(HS 2 O 7 ) shows the arsenic atoms in a trigonal pyramidal coordination of the * Prof. Dr. M. S. Wickleder

evacuated glass tubes, 150°C fo (I), 250°C for (II) and (III), 24 h). (I), (II), and (III) crystallize in the monoclinic space group P2 1 /c (Z = 4), P2 1 /n (Z = 4), and the triclinic space group P1 (Z = 2, single crystal XRD), respectively. (I) shows the As atoms in a trigonal pyramidal coordination of O atoms of one chelating S2 and one monodentate HS2 group. Hydrogen bonding in (I) results in layers. (II) shows the Sb 3+ cations in a seesaw-type coordination of O from both anions. In (III) the Bi 3+ cations are in a square prismatic O coordination of disulfate units. Linkages in (II) and (III) result in complex three-dimensional structures. -(LOGEMANN, C.; KLEINEBERG, H.; OHLERT, J.; WICKLEDER*, M. S.; Z. Anorg. Allg. Chem. 639 (2013) 15, 2796-2803, http://dx.