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We present here a narrative of an incident that occurred in a chemistry laboratory while purifying benzene using a distillation apparatus. The incident resulted in an injury to a graduate student and a fire that caused approximately $3.5 million in damage including repair/refurbishment costs. Unfortunately, due to the extent of the fire, a direct cause of the incident could not be determined. The lessons learned from this incident that could have potentially prevented the incident altogether, or at least reduced damage, include performing a risk assessment of both the experiment and the situation at the time, maintaining proper housekeeping of the lab, maintaining an updated and accurate chemical inventory, checking in on long duration experiments, always calling for back-up, ensuring the lab and buildings are up to code, wearing proper personal protective equipment, and always calling 911 in an emergency.more » « less
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null (Ed.)The 2.2.2-cryptand ligand (crypt) that is heavily used in reductions of rare-earth metal complexes to encapsulate alkali metals has been found to function as a bidentate ligand to rare-earth metal ions in some cases. The X-ray crystal structures of the reduced dinitrogen metal complex, [{(R 2 N) 2 Ce(crypt-κ 2 -O,O′)} 2 (μ–η 2 :η 2 -N 2 )] (R = SiMe 3 ), and the ytterbium metallocene, (C 5 Me 5 ) 2 Yb(crypt-κ 2 -O,O′), are presented to demonstrate this binding mode. The implications of this available binding mode in rare-earth metal cryptand chemistry are discussed.more » « less
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null (Ed.)N , N ′-Di- tert -butylcarbodiimide, Me 3 CN=C=NCMe 3 , undergoes reductive cleavage in the presence of the Gd II complex, [K(18-crown-6) 2 ][Gd II (N R 2 ) 3 ] ( R = SiMe 3 ), to form a new type of ligand, the tert -butylcyanamide anion, (Me 3 CNCN) − . This new ligand can bind metals with one or two donor atoms as demonstrated by the isolation of a single crystal containing potassium salts of both end-on and side-on bound tert -butylcyanamide anions, (Me 3 CNCN) − . The crystal contains [K(18-crown-6)(H 2 O)][NCNCMe 3 - kN ], in which one ( t BuNCN) − anion is coordinated end-on to potassium ligated by 18-crown-6 and water, as well as [K(18-crown-6)][η 2 -NCNCMe 3 ], in which an 18-crown-6 potassium is coordinated side-on to the terminal N—C linkage. This single crystal also contains one equivalent of 1,3-di- tert -butyl urea, (C 9 H 20 N 2 O), which is involved in hydrogen bonding that may stabilize the whole assembly, namely, aqua( tert -butylcyanamidato)(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium(I)–( tert -butylcyanamidato)(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium(I)– N , N ′-di- tert -butylcarbodiimide (1/1/1) [K(C 5 H 9 N 2 )(C 12 H 24 O 6 )]·[K(C 5 H 9 N 2 )(C 12 H 24 O 6 )(H 2 O)]·C 9 H 20 N 2 .more » « less