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Successful phasing of synchrotron through-the-substrate microdiffraction data by  δ -recycling direct-methods largely depends on the number of missing intensities caused by the limited sample rotation range [J. Rius, Direct phasing from Patterson syntheses by  δ  recycling.  Acta Cryst. A  2012 ,  68 , 77–81]. Particularly, for the unfavorable triclinic system, dataset completeness resulting from a single series of consecutive  ϕ -scans covering a total  ϕ  interval of ±35° is around 41%. This value is not enough for the routinary solution of a crystal structure by  δ -recycling but can be increased by ~29% by applying the orthogonal  χ  strategy consisting of merging the information of two series of orthogonal  ϕ -scans collected at the same microvolume of the polished thin section. Test calculations using simulated and experimental tts-data of the triclinic mineral axinite confirm that, with the help of the orthogonal  χ  strategy, crystal structures can be solved routinely. Since data in the ±35  ϕ -interval are normally accessible even for relatively thick glass-substrates (1–1.5 mm), a crystal structure can be determined from a single microvolume. For high-symmetry phases, due to the Laue symmetry redundancy, a single series of  ϕ -scans normally suffices for the application of  δ -recycling. However, when for experimental causes this series is incomplete, the orthogonal  χ  strategy also provides a simple way to increase the completeness which besides allowing solving the structure, is also beneficial for the subsequent refinement.

Increasing data completeness in synchrotron tts-microdiffraction experiments for δ -recycling phasing of low-symmetry compounds