Polymerization of nuclear substituted styrene by ZIEGLER type catalysts has been studied by NATTA et a1.l) and they found many crystalline polymers, but polymerization of p-methylstyrene by alkylsodium has not been reported. We carried out polymerization of p-methylstyrene with n-amylsodium or Aljin catalyst in n-hexane a t low temperature. The polymers obtained-by these catalysts are suggested t o contain stereospecific polymer. c _Under nitrogen atmosphere 0.51 g. of metallic sodium was in 20 ml. of dry n-hexane, to which 1.07 g. of n-amyl chloride was added dropwise. The mixture was stirred a t 0°C. for 3 hours. Then 5 ml. of p-methylstyrene dissolved in 15 ml. of dry n-hexane were added dropwise to this catalyst. The polymerization mixture was stirred for 24 hours at 0 "C. and precipitated with methanol. Then the solid product was treated with aqueous hydrochloric acid followed by extraction with benzene or acetone.

The crystal structure of dichlorobis(acetoxime)palladium, PdCl2(C3H6NOH)2, has been determined from three-dimensional single-crystal X-ray photographic data. The crystals belong to the monoclinic system (space group P21/a), with two formula units in a cell with dimensions: a=8.709±0.007, b=13.996±0.005, c=4.756±0.006 Å, and β=95.60±0.05°. The structure was established by the heavy-atom method and was refined by the block-diagonal least-squares procedure. The Pd atoms are spaced at intervals of 4.76 Å along the c-axis and have a trans planar coordination, with two Cl atoms at 2.30 Å and two N atoms of the oxime groups at 2.03 Å. The oxime plane is twisted about the Pd–N bond by 72.7° from the coordination plane defined by the Pd, Cl, and N atoms. The complex molecules are hydrogen-bonded with each other in strings of an indefinite length along the c-axis, and the hydrogen-bond distance between the O atom of the oxime and the Cl atom is 3.07 Å.

The crystal structure of dichlorobis(cyclohexanone oxime)palladium, PdC12(C6H1ONOH)2, has been determined from three-dimensional X-ray photographic data. The crystals belong to the triclinic space group PI, with these cell parameters: a=8.81 A, b=9.19 A, c=4.99 A; The unit cell contains one molecule of the complex. The palladium atoms are spaced at intervals of 4.99 A along the c-axis and have a square planar coordination, with two chlorine atoms at 2.24 A and two nitrogen atoms of the oxime group at 2.08 A. The complexes are hydrogen-bonded with each other in strings of indefinite length along the c-axis, and the hydrogen bond distance between the oxygen atom of the hydroxyimino group and the chlorine atom is 2.93 A.

The crystal structure of bis(nitrosocyclohexane), (C6H11NO)2, has been determined by means of three-dimensional X-ray analysis by the photographic method. The crystal belongs to the triclinic space group P \bar1, with cell parameters, a=10.133 A, b=6.758 A, c=5.583 A, α=121°42′, β=96°50′, γ=78°06′. The unit cell contains one molecule. The nitrogen and oxygen atoms and the carbon atoms bound to nitroso-groups, CNO–O′N′C′, are almost coplanar, and the oxygen atoms take a trans configuration around the N–N′ bond. The cyclohexane ring takes a chair form and the nitrogen atom is bound to an equatorial bond. The CNO-O′N′C′ plane is twisted from the cyclohexane ring by 73°.

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