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Tetrameric fluorophosphazene, (NPF(2))(4), planar or puckered?

A J Elias¹, B Twamley, R Haist

¹Contribution from the Department of Chemistry, University of Idaho, Moscow, Idaho, 83844-2343, USA.

Journal of the American Chemical Society

|October 18, 2001

Summary

The eight-membered heterocycle N(4)P(4)F(8) is not planar, contrary to previous findings. This study reveals a puckered ring structure, especially below a phase transition temperature of -74°C.

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Area of Science:

Inorganic chemistry
Solid-state chemistry
Crystallography

Background:

Previous structural determination of N(4)P(4)F(8) suggested a planar eight-membered heterocycle.
Understanding the precise molecular geometry of inorganic ring systems is crucial for predicting their properties and reactivity.

Purpose of the Study:

To redetermine the crystal structure of N(4)P(4)F(8) using multiple experimental techniques.
To clarify the structural behavior of the N(4)P(4) ring system, particularly concerning its planarity and phase transitions.

Main Methods:

Single-crystal X-ray diffraction
Gas electron diffraction (GED)
Differential scanning calorimetry (DSC)
Computational structure optimizations (HF/6-31G, B3LYP/6-31G)

Main Results:

The eight-membered N(4)P(4)F(8) heterocycle is definitively not planar.
Above the phase transition temperature (-74°C), the ring is disordered and puckered, appearing pseudoplanar.
Below the phase transition, the ring adopts a saddle (K form) conformation, similar to N(4)P(4)Cl(8).
The low-temperature unit cell is derived from the high-temperature phase by doubling the c-axis and reducing symmetry.

Conclusions:

The experimental and computational data conclusively refute the previous report of a planar N(4)P(4)F(8) structure.
The study provides a detailed understanding of the puckered, non-planar structure of N(4)P(4)F(8) and its conformational changes across a phase transition.