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C22H24O3, triclinic, PI (No. 2), a = 6.0591(3) A, b = 15.2931(9) A, c = 20.501(1) A, a = 98.598(2)°, P = 97.471(3)°, 7 = 96.224(3)°, V= 1846.5 A 3 , Z = 4, Rgt(F) = 0.057, wRKi{F) = 0.048, T 173 K. Source of material The compound was prepared as in [1] and recrystallised from an heptane solution as colorless crystals; mp 343 K 345 K. Discussion The structure is one of three isomers isolated from the reaction of 3,6-diphenyl-l,2-dioxine with /-butyl stabilised phosphorus ylide [1]. In this isomer the phenyl group occupies a position opposite to the other substituents. There are two independent molecules in the asymmetric unit that differ from each other in the relative orientations of the substituents. The major disparity is found with the orientation of the phenyl groups as best exemplified in the C( 1 )/C(3)/C(31 )/C(32) and C(l)/C(3)/C(31)/C(36) torsion angles of 124.4(2)° and 50.7(3)° for molecule a and -3.7(4)° and 175.2(2)° for molecule b. Table 1. Data collection and handling. Crystal: colourless block, size 0 . 1 2 x 0 . 1 2 x 0 . 2 0 mm Wavelength: Mo Ka radiation (0.7107 Â) H: 0.79 cm" 1 Diffractometer, scan mode: Nonius Kappa CCD, to/29 26max: 55.06° N(hkl)measured, N(hkl)unique: 8330,8330 Criterion for I0bs, iV(M/)gt: /o b s > 3 a(/obsJ, 3955 N(param)Kn„ed: 451 Programs: teXsan [2], SIR97 [3] Table 2. Atomic coordinates and displacement parameters (in Â).

The structure of the title compound, C 16 H 26 O, has shown that the plane of the benzene ring lies almost perpendicular [87.9 (2)°] to the plane C(2),C(3),C(4).

The structure of the title compound, [CoCl(C 8 H 21 N 5 )]2ClO 4 , consists of octahedral [Co(trenenim)Cl] 2+ cations [where trenenim = N,N-bis(2-aminoethyl-N'-(2-aminoethylidene)ethane-1,2-diamine] with two perchlorate anions acting as counterions. The bond lengths and angles about N(2) and C(3) provide clear evidence for the presence of an imine bond. A short Co-N(2) distance of 1.863 (2) A reflects the fact that this N atom is an imine N atom. The corresponding Co-N distance in the related saturated system [Co(trenen)Cl] 2+ [where trenen = N,N,N'-tris-(2-aminoethyl)ethane-1,2-diamine] is also substantially shorter than the others. In both cases, the secondary N atom on the appended arm has a stronger affinity for Co III than the primary and tertiary N atoms within the ligand framework

Di [3-(4'-methoxyphenyl)-2,2,4,4-tetramethylpentan-3-yl] oxalate (4a) and the analogous bis tetrahydropyranyl ether (4b) have been synthesized, and X-ray crystallography of the former shows an almost symmetrically staggered relationship of the t-butyl groups with respect to the plane of the benzene ring.

NaGdSiO4.0.213Na OH, M r = 280.8, te- tragonal, 14, a = 11.748 (6), c = 5.450 (3)A, U = 752.2 A 3, Z = 8, D c = 4.96 g cm -3, /a(Mo Ka) = 171.5 cm-~; final R = 0.028 for 1176 reflections. The Gd atom has distorted eightfold coordination; of the two Na atoms one is seven coordinate and the other ten coordinate; the Si atom is tetrahedral. The Na ÷ and OH- ions partially occupy the 4(e) and 2(a) sites respectively.