Rajca Andrzej, Takahashi Masahiro, Pink Maren, Spagnol Gaëlle, Rajca Suchada
Department of Chemistry, University of Nebraska, Lincoln, Nebraska 68588-0304, USA.
J Am Chem Soc. 2007 Aug 22;129(33):10159-70. doi: 10.1021/ja0712017. Epub 2007 Jul 27.
Nitroxide diradicals, in which nitroxides are annelated to m-phenylene forming tricyclic benzobisoxazine-like structures, have been synthesized and characterized by X-ray crystallography, magnetic resonance (EPR and 1H NMR) spectroscopy, as well as magnetic studies in solution and in solid state. For the octamethyl derivative of benzobisoxazine nitroxide diradical, the conformationally constrained nitroxide moieties are coplanar with the m-phenylene, leading to large values of 2J (2J/k > 200 K in solution and 2J/k >> 300 K in the solid state). For the diradical, in which all ortho and para positions of the m-phenylene are sterically shielded, distortion of the nitroxide moieties from coplanarity is moderate, such that the singlet-triplet gaps remain large in both solution (2J/k > 200 K) and the solid state (2J/k approximately 400-800 K), though an onset of thermal depopulation of the triplet ground state is detectable near room temperature. These diradicals have robust triplet ground states with strong ferromagnetic coupling and good stability at ambient conditions. Magnetic behavior of the nitroxide diradicals at low temperature is best fit to the model of one-dimensional S = 1 Heisenberg chains with intrachain antiferromagnetic coupling. The antiferromagnetic coupling between the S = 1 diradicals may be associated with the methyl nitroxide C-H- - -O contacts, including nonclassical hydrogen bonds. These unprecedented organic S = 1 antiferromagnetic chains are highly isotropic, compared to those of the extensively studied Ni(II)-based chains.
氮氧双自由基,其中氮氧化物与间亚苯基稠合形成三环苯并双恶嗪样结构,已通过X射线晶体学、磁共振(EPR和1H NMR)光谱以及溶液和固态中的磁性研究进行了合成和表征。对于苯并双恶嗪氮氧双自由基的八甲基衍生物,构象受限的氮氧化物部分与间亚苯基共面,导致溶液中2J值较大(2J/k > 200 K),固态中2J/k >> 300 K。对于间亚苯基所有邻位和对位均被空间屏蔽的双自由基,氮氧化物部分偏离共面的扭曲程度适中,使得在溶液(2J/k > 200 K)和固态(2J/k约为400 - 800 K)中,单重态 - 三重态能隙仍然较大,尽管在室温附近可检测到三重态基态的热去极化开始。这些双自由基具有稳健的三重态基态,在环境条件下具有强铁磁耦合和良好的稳定性。氮氧双自由基在低温下的磁行为最符合具有链内反铁磁耦合的一维S = 1海森堡链模型。S = 1双自由基之间的反铁磁耦合可能与甲基氮氧化物的C - H - - - O接触有关,包括非经典氢键。与广泛研究的基于Ni(II)的链相比,这些前所未有的有机S = 1反铁磁链具有高度各向同性。