Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination

Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination

Received 29 July 2014 Accepted 19 October 2014 | Lennard Krause, Regine Herbst-Irmer, George M. Sheldrick and Dietmar Stalke*
The study compares the quality of diffraction data obtained using silver and molybdenum microfocus X-ray sources for single-crystal structure determination. The experiments were conducted on two 30 W air-cooled Incoatec μS microfocus sources with multilayer optics mounted on a Bruker D8 goniometer and a SMART APEX II CCD detector. The data were analyzed, processed, and refined using standard Bruker software. The results show that Ag Kα radiation can be beneficial when heavy elements are involved, as it reduces absorption. A numerical absorption correction based on crystal face positions and indices was found to be limited in effectiveness due to the highly focused microsource beams. However, empirical corrections implemented in SADABS, originally intended for conventional sealed-tube sources, performed well in correcting variations in the effective volume of the irradiated crystal. For three of the six model compounds studied (two Ag and one Mo), the final SHELXL R1 against all data after applying empirical corrections was below 1%. The study suggests that the requirement for a numerical absorption correction for strongly absorbing crystals may need revision.The study compares the quality of diffraction data obtained using silver and molybdenum microfocus X-ray sources for single-crystal structure determination. The experiments were conducted on two 30 W air-cooled Incoatec μS microfocus sources with multilayer optics mounted on a Bruker D8 goniometer and a SMART APEX II CCD detector. The data were analyzed, processed, and refined using standard Bruker software. The results show that Ag Kα radiation can be beneficial when heavy elements are involved, as it reduces absorption. A numerical absorption correction based on crystal face positions and indices was found to be limited in effectiveness due to the highly focused microsource beams. However, empirical corrections implemented in SADABS, originally intended for conventional sealed-tube sources, performed well in correcting variations in the effective volume of the irradiated crystal. For three of the six model compounds studied (two Ag and one Mo), the final SHELXL R1 against all data after applying empirical corrections was below 1%. The study suggests that the requirement for a numerical absorption correction for strongly absorbing crystals may need revision.
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