A single crystal, three-dimensional X-ray study of catena-p-chloro-(cyclooctatetraene)copper( I ) has been carried out. The structure consists of continuous chains formed by the copper and chlorine atoms extending through the crystal in the a direction with one olefinic bond closely bound to each copper atom. The carbon atoms of the bonded olefinic group are approximately coplanar with the copper and adjacent chlorine atoms of the chain, and the coordination about the copper(1) may be described as a distorted trigonal arrangement. The bond distances and the bond angles associated with the closely bound atoms are: CI-Cu-Cl, 106.4 f 0.1'; CI-Cu-(C1-C2 center), 123.1 f 0 2 O , 130.1 f 0.2'; Cu-C,, 2.073 f 0.010 b.; CU-C~, 2.097 f 0.007 A. A variety of weighting schemes was used in the least-squares data refinement procedures to test the sensitivity of the resulting interatomic distances to the weighting scheme and thus provide a test for systematic errors. Cu-Cl, 2.288 f 0.002 b., 2.284 f 0.002 b.; (9) 0.A crystal structure determination of the compound formed by the reaction of copper(1) chloride and bicyclo[2.2.1] hepta-2,5-diene (norbornadiene) shows that the complex exists as a tetramer, (CTH&!uCl)a, in the solid state with 3 symmetry.The copper and chlorine atoms form an eight-membered tube-shaped ring with one double bond of the olefin coordinated to the copper atom and lying in the plane defined by the copper atom and adjacent chlorine atoms, The copper atom is coordinated to the olefin in an ex0 configuration; one double bond of the olefin is not coordinated. The distorted trigonal planar coordination about copper is similar to that found for potassium dicyanocuprate( I), cyclooctatetraenecopper( I ) chloride, and 2-butynecopper( I) chloride,

The crystal structure of norbornadiene palladium chloride has been refined with data obtained by counter methods from crystals maintained at liquid nitrogen temperature. After refinement the conventional discrepancy index R = 0.0275. The carbon--carbon single bond distances in the norbornadiene molecule are normal: 1"547, 1.552, 1.554 (+ 0.006)/~; the double bond distances are barely significantly longer than normal: 1.366, 1.366 (+0.010) ~. The observed double bond distance is now compatible with the infrared spectrum of the complexed olefin.

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