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以负三价、五啮的N-乙酰水杨酰肼(ashz3-)作为配体,合成了二个大环六核氮杂金属冠醚犤MnⅢ6(ashz)6(MeOH)6犦·6MeOH(1)和犤MnⅢ6(ashz)6(DMF)6犦·3DMF(2)。晶体学数据是:配合物1,三方晶系,空间群R3珔,a=b=24.806(2),c=11.260(1)?,Z=3,μ=1.007mm-1,R=0.0572,wR=0.1142;配合物2,三方晶系,空间群R3珔,a=b=26.629(3),c=23.298(4)?,Z=6,μ=0.856mm-1,R=0.0671,wR=0.1661。这两个配合物属18-氮杂金属冠醚-6结构类型,冠醚分子具有晶体学C3i对称性。配体ashz3-通过它的肼基的N-N桥连金属原子,从而形成有中央空穴的六核锰的大环配合物。变温磁化率(4～275K)研究表明,配合物1中金属离子间存在着反铁磁性耦合。
Two macrocyclic hexa-aza metal crown ethers, Mn 6, 6H 6 (OH 6) 6MeOH, were synthesized with negatively charged trivalent pentasodium N-acetylsalicyloylhydrazide (ashz3-) And 犤 Mn 6 6 (DMF) 6 犦 · 3DMF (2). The crystallographic data are: complex 1, triclinic system, space group R3 珔, a = b = 24.806 (2), c = 11.260 (1) wR = 0.1142; complex 2, trigonal system, space group R3 珔, a = b = 26.629 (3), c = 23.298 (4) ?, Z = 6, μ = 0.856mm-1, R = = 0.1661. The two complexes belong to the 18-aza metal crown-6 structure type and the crown ether molecules have crystallographic C3i symmetry. The ligand ashz3- bridges the metal atom through its hydrazino N-N, forming a macrocyclic hexa-nuclear manganese macrocyclic complex. The results show that there is an antiferromagnetic coupling between the metal ions in the complex 1.