The crystal and molecular structure of MO(CO)~[P(CHZ)~N~] has been determined by single-crystal x-ray diffraction techniques using a GE 490 automated diffractometer system. The compound crystallizes in the space group Pbca with eight formula weights in a unit cell of dimensions a = 14.357 (2) A, b = 26.509 (2) A, and c = 8.1528 (6) A. The structure was solved by means of a three-dimensional Patterson function and refined by block-diagonal least squares to a value of R = 0.069 for 1194 statistically significant reflections. The ligand has been shown to bind to the molybdenum through the phosphorus with a Mo-P bond of 2.48 A. The rigidity of the phosphorus cage which exists both in the solid and in solution allows for a crystallographic estimate of Tolman's widely used steric factor, the "ligand cone angle". Infrared spectral properties are compared to metal carbonyl derivatives of other phosphorus cage compounds.

The crystal and molecular structure of 2‐thia‐1,3,5‐triaza‐7‐phosphaadamantane 2,2‐dioxide (C5H10SPO2N3) has been determined by single crystal x‐ray diffraction techniques. The compound crystallizes in the space group P21/c with four formula weights per unit cell of dimensions a = 6.129 (1) Å, b = 12.440 (2) Å, c = 14.028 (2) Å, β = 127.31 (1)°. The structure was solved by direct methods and refined to a final value of R = 0.079.

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