0000000001316533
AUTHOR
Yasuhide Inokuma
X-ray snapshot observation of palladium-mediated aromatic bromination in a porous complex
Pd-mediated aromatic bromination is intriguing to synthetic and organometallic chemists due to both its synthetic utility and, more importantly, a proposed mechanism involving an uncommon Pd(IV)/Pd(II) catalytic cycle. Here, we report an X-ray snapshot observation of a Pd reaction center during a Pd-mediated aromatic bromination in a single crystal of a porous coordination network crystalline scaffold. Upon treatment of a single crystal with N-bromosuccinimide, sequential X-ray snapshots revealed that the aryl-Pd(II)-L species embedded in the network pores was converted to the brominated aryl product through a transient aryl-Pd(II)-Br species, which is normally unobservable because of its r…
X-ray analysis on the nanogram to microgram scale using porous complexes
X-ray single-crystal diffraction (SCD) analysis has the intrinsic limitation that the target molecules must be obtained as single crystals. Here we report a protocol for SCD analysis that does not require the crystallization of the sample. In our method, tiny crystals of porous complexes are soaked in a solution of the target, such that the complexes can absorb the target molecules. Crystallographic analysis clearly determines the absorbed guest structures along with the host frameworks. Because the SCD analysis is carried out on only one tiny crystal of the complex, the required sample mass is of the nanogram–microgram order. We demonstrate that as little as about 80 nanograms of a sample …
CCDC 1003159: Experimental Crystal Structure Determination
Related Article: Koki Ikemoto , Yasuhide Inokuma , Kari Rissanen , and Makoto Fujita|2014|J.Am.Chem.Soc.|136|6892|doi:10.1021/ja502996h
CCDC 967380: Experimental Crystal Structure Determination
Related Article: Koki Ikemoto , Yasuhide Inokuma , Kari Rissanen , and Makoto Fujita|2014|J.Am.Chem.Soc.|136|6892|doi:10.1021/ja502996h
CCDC 967381: Experimental Crystal Structure Determination
Related Article: Koki Ikemoto , Yasuhide Inokuma , Kari Rissanen , and Makoto Fujita|2014|J.Am.Chem.Soc.|136|6892|doi:10.1021/ja502996h
CCDC 967379: Experimental Crystal Structure Determination
Related Article: Koki Ikemoto , Yasuhide Inokuma , Kari Rissanen , and Makoto Fujita|2014|J.Am.Chem.Soc.|136|6892|doi:10.1021/ja502996h