[(N-Lithio-N-mesitylsulfonyloxy-tert-butylcarbamate)2·(thf)3]: Crystal Structure of a Nitrenoid

✍ Scribed by Prof. Dr. Gernot Boche; Christiane Boie; Ferdinand Bosold; Dr. Klaus Harms; Michael Marsch

• Publisher: John Wiley and Sons
• Year: 1994
• Tongue: English
• Weight: 372 KB
• Volume: 33
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.199401151

✦ Synopsis

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ence peak and hole: 310 enm-', R1 (F > 4a(F)) = 0.040 and wR2 = 0.095 (all data); R values as defined above. Data of both structures were collected on a Stoe-Siemens-AED diffractometer. The intensities of the rapidly cooled crystals in an oil drop [27] were collected by the 2 O/w method. Both structures were solved by direct methods (SHELXS-90) [28] and refined by full-matrix leastsquares on F1 [29]. The silicon/germanium disorder in 1, which is caused by symmetry could be resolved. The refinement of occupancy for the central silicon atoms and the germanium atom resulted in values of 2/3 and li3, respectively. The refinement in the space group C2/c was not successful. Due to the disorder of the crown ether molecule caused by the mirror plane, two crown ether molecules with an occupancy of 1/2 each were refined. 1-2 and 1-3 distances of chemically equivalent bonds were refined by using distance restraints. Further details of the crystal structure investigations are available on request from the Director of the Cambridge Crystallographic Data Centre, 12