[Zn(C7H4NOaS)E(HEO)4].2H20 AND [Cd(CTH4NO3S)E(H20)4].2H20molecule [0(4)] giving the shortest M-O distance involved in the shortest, and presumably strongest, intermolecular H-bonding. The orientation of the two C7H4NOaS ligands, which are basically coplanar, is such that the ligand planes are close to the plane containing the two nitrogens, the metal and the 0(4) oxygens. The dihedral angle between the two planes defined by the ligand ring atoms and the M, N and 0(4) atoms is ~16 °, and that between the ligand plane and the M,N,O(5) plane is ~72 °. Such an arrangement will place the lone pairs on the sp 2 N atoms approximately parallel to the M--O(5) bonds, and it is possible that these will exert some repulsive effect on the 0(5) water molecules leading to a weakening of these bonds. It is the M-O(5) bond that suffers Jahn-Teller elongation in the Cu complex, and in such distortions it is invariably the weakest bonds that are lengthened. The results of thermal studies of the seven hexahydrates (Haider, Malik & Wadsten, 1983) indicate that the energy of dehydration is minimum for the Cu complex and maximum for the Ni complex. All six H20 molecules are removed within 350-490 K. The energy of dehydration, which is related to the binding energy of the H20 molecules in the crystal, increases in the order Cu < Cd 3 for other alkyl substituents. Vetter, Strametz & Nrth (1963) also prepared the tert-butyl derivative and proposed a dimeric structure. The crystal structure of the methyl analogue (Weiss & Eisenhuth, 1967) showed it to be trimeric with a six-membered [AsN] a ring. We report here the structure of [t-BuNAsC1] 2, prepared by a new route.

P4S10 (1) kann mit Silicium–Stickstoffverbindungen abgebaut werden. 1 reagiert mit (CH3)3Si–N(CH3)2 (2a) bzw. (CH3)3Si–N(C2H5)2 (2 b) zu S = P[N(CH3)2]2SSi(CH3)3 (3a) bzw. 3b. Die Umsetzung von 1 mit [(CH3)3Si]2S (4) ergibt in hoher Ausbeute SP[SSi(CH3)3]3 (6). Um den Reaktionsverlauf aufklären zu können, wurde (C6H5PS2)2 (7) als Modellsubstanz mit 2a bzw. 4 umgesetzt, wobei C6H5P(S)[N(CH3)2]SSi(CH3)3 (9) bzw. C6H5P(S)[SSi(CH3)3]2 (10) entstehen, Der Reaktionsmechanismus wird diskutiert. Die Kernresonanzdaten und Massenspektren werden mitgeteilt.

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