The performance of the Siemens SMART CCD (charge-coupled device) area detector has been tested to assess its suitability for accurate electron-density (ED) determination. 92043 diffraction intensities (14701 unique reflections, 65 h experiment) have been collected on a reference crystal of methyl 2-[(4-butyl-2-methyl-6-oxo-5-(4-[2-(1H-tetrazol-5-yl)phenyl]benzyl)-1,2- dihydropyrimidin-1-yl)methyl]-3-thiophenecarboxylate (C30- H30N6O3S) at T = 120 K and compared with those (51 485, 14 699 unique, 600 h) obtained from a previous collection at T = 18 K on the same crystal using a diffractometer equipped with a conventional detector. Results from spherical and multipolar refinements (agreement factors, standard uncertainties of refined variables and geometries after correction for thermal motion) have also been compared. The λ/2 contamination, which affects area detectors but not well tuned conventional detectors, has been carefully investigated and proved to be a negligible source of errors (which can anyway be easily corrected). The encouraging results of this test prove that area detectors are also well suited for charge-density studies, offering a cheap and fast data-collection mode, without loss of accuracy, which can be exploited for ED studies on large systems. © 1998 International Union of Crystallography.
A test of the suitability of CCD area detectors for accurate electron-density studies
Macchi, Piero;
1998-01-01
Abstract
The performance of the Siemens SMART CCD (charge-coupled device) area detector has been tested to assess its suitability for accurate electron-density (ED) determination. 92043 diffraction intensities (14701 unique reflections, 65 h experiment) have been collected on a reference crystal of methyl 2-[(4-butyl-2-methyl-6-oxo-5-(4-[2-(1H-tetrazol-5-yl)phenyl]benzyl)-1,2- dihydropyrimidin-1-yl)methyl]-3-thiophenecarboxylate (C30- H30N6O3S) at T = 120 K and compared with those (51 485, 14 699 unique, 600 h) obtained from a previous collection at T = 18 K on the same crystal using a diffractometer equipped with a conventional detector. Results from spherical and multipolar refinements (agreement factors, standard uncertainties of refined variables and geometries after correction for thermal motion) have also been compared. The λ/2 contamination, which affects area detectors but not well tuned conventional detectors, has been carefully investigated and proved to be a negligible source of errors (which can anyway be easily corrected). The encouraging results of this test prove that area detectors are also well suited for charge-density studies, offering a cheap and fast data-collection mode, without loss of accuracy, which can be exploited for ED studies on large systems. © 1998 International Union of Crystallography.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
