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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.

X-ray diffraction study of a single crystal of B2F4 indicates a planar, centrosymmetric molecule with B–B=1.67±0.045 A, B–F=1.32±0.035 A and angle F–B–F=120°. There are two molecules in a monoclinic unit cell of symmetry P21/n and parameters of a=5.49, b=6.53, c=4.83, and β=102.5°.

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