The neutral phospha(III)guanidine compounds, Ph2PC{NR}{NHR}
(1a, R = Cy; 1b, R =
iPr), are reported. NMR spectroscopic data indicated the presence of the Esyn isomer in solution and structural studies confirmed this in the solid-state. Reaction of 1a with M(CO)4(pip)2
[M = Mo, W; pip = piperidine] proceeded via displacement of the piperidine ligands to generate the complexes M[Ph2PC{NCy}{NHCy}](CO)4
(2a, M = Mo; 3a, M = W). The X-ray structure of 2a and 3a were solved, showing the first structurally characterised examples of 1-aza-3-phospha-4-metallacyclobut-1-ene rings.
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