Tigyer Benjamin R, Zeller Matthias, Zaleski Curtis M
Acta Crystallogr Sect E Struct Rep Online. 2011 Aug 1;67(Pt 8):m1041-2. doi: 10.1107/S160053681102602X. Epub 2011 Jul 9.
The title compound [Mn(6)(C(7)H(4)NO(3))(5)(CH(3)CO(2))(2)(C(5)H(8)N(2))(4)(C(3)H(7)NO)(2)]·(C(2)H(5))(2)O·C(3)H(7)NO·CH(3)OH·0.12H(2)O, abbreviated as Mn(II)(OAc)(2)15-MC(MnIII(N)shi)-54(DMF)2·diethyl ether·DMF·MeOH·0.12H(2)O (where (-)OAc is acetate, MC is metallacrown, shi(3-) is salicylhydroximate, EtIM is n-ethylimidazole, DMF is N,N-dimethylformamide, and MeOH is methanol) contains five Mn(III) ions as members of the metallacrown ring and an Mn(II) ion bound in the central cavity. The central Mn(II) ion is seven-coordinate with a distorted face-capped trigonal-prismatic geometry. The five Mn(III) ions of the metallacrown ring are six-coordinate with distorted octa-hedral geometries. The configuration of the Mn(III) ions about the metallacrown ring follow a ΔΛΔPP pattern, with P representing planar. The four 1-ethyl-imidazole ligands are bound to four different Mn(III) ions. A diethyl ether solvent mol-ecule was found to be disordered over two mutually exclusive sites with an occupancy ratio of 0.568 (7):0.432 (7). A methanol solvent mol-ecule was found to be disordered over two mutually exclusive sites by being hydrogen bonded either to a dimethyl-formamide solvent mol-ecule (major occupancy component) or to an O atom of the main mol-ecule (minor occupancy component). The occupancy ratio refined to 0.678 (11):0.322 (11). Associated with the minor component is a partially occupied water mol-ecule [total occupancy 0.124 (15)].
标题化合物[Mn(6)(C(7)H(4)NO(3))(5)(CH(3)CO(2))(2)(C(5)H(8)N(2))(4)(C(3)H(7)NO)(2)]·(C(2)H(5))(2)O·C(3)H(7)NO·CH(3)OH·0.12H(2)O,简称为Mn(II)(OAc)(2)15-MC(MnIII(N)shi)-54(DMF)2·二乙醚·DMF·甲醇·0.12H(2)O(其中(-)OAc为乙酸根,MC为金属冠醚,shi(3-)为水杨羟肟酸根,EtIM为N-乙基咪唑,DMF为N,N-二甲基甲酰胺,MeOH为甲醇)包含五个作为金属冠醚环成员的Mn(III)离子和一个结合在中心腔中的Mn(II)离子。中心Mn(II)离子为七配位,具有扭曲的面帽三角棱柱几何构型。金属冠醚环的五个Mn(III)离子为六配位,具有扭曲的八面体几何构型。金属冠醚环周围Mn(III)离子的构型遵循ΔΛΔPP模式,P表示平面。四个1-乙基咪唑配体与四个不同的Mn(III)离子结合。发现一个二乙醚溶剂分子在两个相互排斥的位置上无序,占有率为0.568 (7):0.432 (7)。发现一个甲醇溶剂分子通过氢键与一个二甲基甲酰胺溶剂分子(主要占有率组分)或主分子的一个O原子(次要占有率组分)结合而在两个相互排斥的位置上无序。占有率精修为0.678 (11):0.322 (11)。与次要组分相关联的是一个部分占据的水分子[总占有率0.124 (15)]。