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A new chemical mass‐spectrometric method for mapping short range order in crystalline solid‐solutions of enantiomers undergoing topochemical reactions is described. We have applied this method to assigning the microstructure of the racemic mixtures of the diacrylates 1 and 2, each one in two dimorphic modifications and which undergo topochemical (2π + 2π) photocyclodimerisation and photocyclopolymerisation. All crystalline phases are disordered with respect to the enantiomeric sec ‐butyl group. While the two polymorphs of 1 and polymorph α of 2 form random solid‐solutions, polymorph β of 2 forms partially ordered crystals in which the degree of order depends on the method of crystallization. It could be established that in the latter system the degree of order across the two independent centres of inversion is measurably different. The scope and limitation of this new method are discussed.
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Addadi et al. (1976) studied this question.
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