Catalyst for change: grad student catches error in chem experiments, prompts retraction

ACS Catalysis has retracted a 2012 research letter from a chemistry lab that discovered an error in their experiments.

According to last author Rory Waterman at the University of Vermont, an undetected reaction caused his lab to mistakenly mischaracterize the products of an iridium catalyst. The diligence of a graduate student brought it all to light, he noted: “In short, it was the ability of one of my group members to be a very good scientist.”

The letter, titled “High Activity and Selectivity for Silane Dehydrocoupling by an Iridium Catalyst,” was published in February. It has only accumulated 5 citations, according to Thomson Scientific’s Web of Knowledge.

According to the retraction notice:

This Letter has been retracted at the request of the authors due to incorrect product characterization, which undermines the conclusions of the work. The reaction of phenylsilane with iridium catalysts was reported accurately and has been successfully reproduced. However, the original product formulation, (SiHPh)₁₀, is incorrect. Under the conditions reported, the catalyst does not significantly dehydrocouple phenylsilane, rather it is a redistribution catalyst with the major product being diphenylsilane, Ph₂SiH₂. The incorrect product assignment partially arose from catalytic heterodehydrocoupling the diphenylsilane product with adventitious water during workup with Fluorosil. The resultant siloxane products were misidentified as the proposed cyclo-silane product (SiHPh)₁₀.

Waterman told us:

We made our observations in on-going studies with that iridium system. In the course of that work, we identified that the products were undergoing a reaction during purification that led to our original misassignment. The reactions themselves and data have been reproducible for more than four years. The pivotal factor in identifying the error was the ability of the graduate student researcher to be confident with the data he was collecting and the resultant conclusion, even if it was not consistent with the literature (even if it was ourselves!). In short, it was the ability of one of my group members to be a very good scientist.

Fortunately, this does not affect any other projects in my group. Other projects are independent of this particular reaction and this catalyst. The correct results with the expanded studies will be the subject of a forthcoming submission for publication. Hopefully, we will be getting the most accurate story out there soon.

A nice example of doing the right thing.

Hat tip: Rolf Degen

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