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High-resolution neutron-diffraction techniques have been used to determine the crystal structure of deuterated squaric acid, D 2 C 4 O 4 , in its ordered phase at 298 K. Comparison with H 2 C 4 O 4  at the same temperature reveals the effects of deuteration alone on the crystal structure. The main changes are seen in the geometry of the O – H(D)…O bonds: the overall O … O bondlength increases by ∼ 0.020 Å on deuteration, and the O – D bond in D 2 C 4 O 4  is ∼ 0.015 Å shorter than O – H in H 2 C 4 O 4 . These changes probably account for much of the increase in the H(D)-ordering temperature,  T c  , in this system, from 371 K in H 2 C 4 O 4  to 516 K in D 2 C 4 O 4 .

The effect of deuteration on the crystal structure of squaric acid (H 2 C 4 O 4 ) in its ordered phase*