Preparative and structural studies of diazadiphosphetidines. Part 9. X-Ray and nuclear magnetic resonance investigations of (Ph2FPNMe) n

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Abstract
It has been established by X-ray and n.m.r. analyses that the compund (Ph2FPNMe)n can be prepared as a dimer with a diazadiphosphetiding ring. The 1H spectrum of the NMe group may be explained in terms of a slow pseudorotation between two conformations. The two values of 3JPH(16.78 and 6.17 Hz) are considerably different, and involve coupling paths through axial and equatorial P–N bonds. Crystals of (Ph2FPNMe)2 are triclinic, space group P, with a= 9.849(2), b= 14.858(3), c= 8.236 (1)Å, α= 93.53(2), β= 94.70(2), γ= 104.04(2)°, Z= 2. There are two independent crystallographically centrosymmetric molecules within the unit cell. Distorted trigonal-bipyramidal co-ordination is observed at phosphorus with mean bond lengths; P–F 1.683(3), P–N eq 1.652(3), P–Nax 1.780(1), and P–C 1.835(4)Å. The Structure was solved by direct methods and refined to R 0.063 for 3 299 diffractometer-measured unique reflections.

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