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Direct measurements of triplet phase relationships for non-centrosymmetric light-atom organic structures with medium-size unit cells are reported. The phase information can be extracted from the three- beam profiles of a Renninger ψ-scan experiment. The measurements were carried out with a special ψ-circle diffractometer installed on a rotating Cu-anode generator. The incident-beam divergence is reduced to 0.02°. The experimental results confirm the theoretical considerations of paper I of this work [Hümmer & Billy (1986). Acta Cryst. A42, 127-133]. As triplet phases of +90° can be distinguished, the absolute structure can be determined unambiguously. The measurements show that the triplet-phase-dependent interference effects may be superposed on phase-independent Umweganregung or Aufhellung effects. By a comparison of the ψ-scan profiles of two centrosymmetrically related three-beam cases, the triplet phases of which have opposite signs, it is possible to evaluate the phase-independent effects and to determine the value of the triplet phase with an accuracy of at least 90°.

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