Synthesis, structural and magnetic characterisation of iron(ii/iii), cobalt(ii) and copper(ii) cluster complexes of the polytopic ligand: N-(2-pyridyl)-3-carboxypropanamide

Russell M.E.; Hawes C.S.; Ferguson A.; Polson M.I.J.; Chilton N.F.; Moubaraki B.; Murray K.S.; Kruger P.E.

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Synthesis, structural and magnetic characterisation of iron(ii/iii), cobalt(ii) and copper(ii) cluster complexes of the polytopic ligand: N-(2-pyridyl)-3-carboxypropanamide

机译：N-（2-吡啶基）-3-羧基丙酰胺的铁（ii / iii），钴（ii）和铜（ii）簇络合物的合成，结构和磁性表征

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Herein we describe the synthesis, structural and magnetic characterisation of three transition metal cluster complexes that feature the polytopic ligand N-(2-pyridyl)-3-carboxypropanamide (H2L): [Fe_3~ (III)Fe_2~ (II)(HL)_6(O)(H_ 2O)_3][ClO_4]_5·3MeCN· 4H_2O, 1, [Co_8(HL)_8(O)(OH)_4(MeOH)_ 3(H_2O)]-[ClO_4]3·5MeOH· 2H_2O, 2, and [Cu_6(Lox)_4(MeOH)(H_ 2O)_3]·MeOH, 3. Complex 1 is a mixed valence penta-nuclear iron cluster containing the archetypal {Fe_3~ (III)O} triangular basic carboxylate cluster at its core, with two Fe(ii) ions above and below the core coordinated to three bidentate pyridyl-amide groups. The structure of the octanuclear Co(ii) complex, 2, is based upon a central Co_4 square with the remaining four Co(ii) centres at the 'wing-tips' of the complex. The cluster core is replete with bridging oxide, hydroxide and carboxylate groups. Cluster 3 contains an oxidised derivative of the ligand, L_(ox), generated in situ through hydroxylation of an α-carbon atom. This hexanuclear cluster has a 'barrel-like' core and contains Cu(ii) ions in both square planar and square-based pyramidal geometries. Bridging between Cu(ii) centres is furnished by alkoxide and carboxylate groups. Magnetic studies on 1-3 reveals dominant antiferro-magnetic interactions for 1 and 2, leading to small non-zero spin ground states, while 3 shows ferro-magnetic exchange between the Cu(ii) centres to give an S = 3 spin ground state.

机译：在这里，我们描述了三种具有多位配体N-（2-吡啶基）-3-羧基丙酰胺（H2L）的过渡金属簇合物的合成，结构和磁性表征：[Fe_3〜（III）Fe_2〜（II）（HL） _6（O）（H_2O）_3] [ClO_4] _5·3MeCN·4H_2O，1，[Co_8（HL）_8（O）（OH）_4（MeOH）_ 3（H_2O）]-[ClO_4] 3·5MeOH ·2H_2O，2和[Cu_6（Lox）_4（MeOH）（H_2O）_3]·MeOH，3。配合物1是包含原型{Fe_3〜（III）O}三角碱性的混合价五核铁簇羧酸盐簇在其核心，在核心的上方和下方有两个Fe（ii）离子与三个双齿吡啶基-酰胺基配位。八核Co（ii）配合物2的结构基于中心Co_4正方形，其余四个Co（ii）中心位于配合物的“翼尖”。簇芯充满了桥接的氧化物，氢氧化物和羧酸盐基团。簇3包含通过α-碳原子的羟基化原位产生的配体的氧化衍生物L_（ox）。该六核簇具有“桶状”核，并且在正方形平面和基于正方形的金字塔形几何结构中均包含Cu（ii）离子。 Cu（ii）中心之间的桥接由醇盐和羧酸盐基团提供。 1-3的磁性研究表明1和2的主要反铁磁相互作用导致小的非零自旋基态，而3表示Cu（ii）中心之间的铁磁交换产生S = 3的自旋基态。

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《Dalton transactions: An international journal of inorganic chemistry》 |2013年第37期|共8页
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Russell M.E.; Hawes C.S.; Ferguson A.; Polson M.I.J.; Chilton N.F.; Moubaraki B.; Murray K.S.; Kruger P.E.;
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synthesis; characterisation; iron;

机译：合成;表征;铁;

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Synthesis, structural and magnetic characterisation of iron(ii/iii), cobalt(ii) and copper(ii) cluster complexes of the polytopic ligand: N-(2-pyridyl)-3-carboxypropanamide

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