Open AccessImage‐Plate Synchrotron Laue Data Collection and Subsequent Structural Analysis of a Small Test Crystal of a Nickel‐Containing Aluminophosphate
Author(s) -
Snell E.,
Habash J.,
Helliwell M.,
Helliwell J. R.,
Raftery J.,
Kaucic V.,
Campbell J. W.
Publication year - 1995
Publication title -
journal of synchrotron radiation
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.172
H-Index - 99
ISSN - 1600-5775
DOI - 10.1107/s0909049594009180
Subject(s) - synchrotron , crystal (programming language) , lambda , monochromatic color , optics , nickel , crystal structure , synchrotron radiation , physics , beamline , crystallography , materials science , chemistry , computer science , beam (structure) , metallurgy , programming language
Image plates have advantages over photographic films, which include wider dynamic range, higher detector quantum efficiency, reduced exposure time and large size. In this study, an on‐line image‐plate system has been used to record crystallographic data from a small crystal. In particular, synchrotron Laue data were recorded with λ min = 0.455, λ max = 1.180 Å, in 20 images 10° apart and with an exposure time of 0.3 s each from a crystal (0.02 × 0.05 × 0.25 mm) of a nickel‐containing aluminophosphate, NiAPO. The Laue data were analyzed with the Daresbury Laue software, including the application of an absorption correction. The structure was solved by a combination of the Patterson method and successive difference Fourier calculations using SHELXS 86 and SHELXL 93; the final R value for 1934 unique reflections (all data) and 310 parameters was 7.90%. The structure agrees with that determined by monochromatic diffractometry using the same crystal and reported by Helliwell, Gallois, Kariuki, Kaucic & Helliwell [ Acta Cryst. (1993), B 49 , 420–428] with an r.m.s. deviation of 0.03 Å. Hence, this study shows the image‐plate device to be very effective for synchrotron data collection and subsequent structure analysis from small crystals, i.e. 0.02 × 0.05 × 0.25 mm, in chemical crystallography as well as providing further confirmation of the practicability of Laue data in structure solution and refinement.