mol) of phosphorous trichloride in 75 ml of ether that had been cooled to -50°. The reaction was allowed to warm to room temperature and stirred for 30 min. After centrifugation, Supplementary Material Available. The derivation of K matrix 1 will appear following these pages in the microfilm edition of this volume of the journal. Photocopies of the supplementary material from this paper only on microfiche (105 X 148 mm, 24 X reduction, negatives) containing all of the supplementary material for the papers in this issue may be obtained from the Journals Department,

Naphthalene-tetrakis(si1ver perchlorate) tetrahydrate, CloH&4gC10&.4HzO, has been prepared and its crystal structure determined by three-dimensional X-ray diffraction techniques from 1796 reflections measured with an automatic diffractometer at ambient room temperature. The cfystals are triclinicoPi, Z = 1, P&d 2.81 g cm-*, Pobsd = 2.8 g cm-*, with reduced cell constants a = 7.298 (1) A, b = 11.870 (1) 3, c = 7.166 (1) 4, a = 91.86 (l)', , P = 100.53 (l)', and y = 102.38 (1)'. The A-centered cell, a = 11.870 (1) A, b = 9.247 (1) A, c = 11.123 (1) A, cy = 88.93 (l)', 0 = 96.88 (l)", and y = 101.21 (l)", was used for the structure solution and refinement by full-matrix least squares including anisotropic temperature factors for all nonhydrogen atoms to a final R of (13) (a)

Bis(~-o-hydroxybenzoato)bis(o-hydroxybenzoato)tetraaquodicadmium(II) (I) and tris(pyridine)bis(o-hydroxybenzoat0)-cadmium(I1) (11) have been shown by X-ray diffraction to consist of pentagonal-bipyramidal seven-coordinate Cd(I1). In the former, the coordination sphere is made up of five carboxyl oxygen atoms in the equatorial plane (one bridging) and two oxygen atoms of water molecules in the axial positions. The latter has four carboxyl oxygen atoms and one pyridine nitrogen atom in the equatorial plane and two axial pyridine nitrogen atoms to complete the coordination sphere. The solid-state MAS '%d NMR chemical shifts of these compounds are -31 and +61 ppm, respectively. The lI3Cd NMR chemical shifts of these and other Cd-containing compounds are correlated with the number of lone pairs that are directed toward the Cd atom. The shielded chemical shifts of a number of Cd model compounds as well as Cd-containing macromolecules are discussed. Crystal data (I): a = 7.747 (3) A, b = 12.455 (3) A, c = 15.725 (7) A, p = 96.23 (3)", 2 = 4, P2Ja, pohd = 1.83 (2) g/cm3, pcald = 1.86 g/cm3, N O = 5058, NV = 208, R , = 0.028. Crystal data (11): a = g/cm3, N O = 4944, NV = 428, RF = 0.029. For both I and 11, structures were refined by full-matrix least squares with anisotropic temperature factors and absorption corrections. 10.187 (4) A, b = 14.846 (5) A, C = 17.965 (5) A, p = 93.79 (3)", z = 4, P2l/ll, pobsd = 1.54 (2) g/Cm3, pcalcd = 1.53

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