本文分為三部分，第一部分以L1為多芽配位基，與Ni(OAc)2·4H2O及LnCl3·6H2O反應，合成一系列[NiIILnIII(L1)2(OH2)(η2-OAc)(μ2-OAc)Cl]·0.5MeCN(Ln = Y(1), Gd(2), Tb(3), Dy(4), Ho(5), Er(6))錯化物，以X光單晶繞射確認其結構。Ni(II)為扭曲的八面體構型，而Ln(III)為扭曲的十二面體構型，以醋酸根離子及L1橋接Ln(III)及Ni(II)離子。從直流磁化率(direct current susceptibility, DC)測量結果，顯示化合物2·Gd—4·Dy金屬間存有鐵磁性(ferromagnetic)作用力。由於Y(III)為逆磁性離子，在1·Y中磁化率隨著溫度下降，可歸因於分子間存有反鐵磁性(antiferromagnetic)作用力，或者是Ni(II)離子的自旋軌域耦合所導致。交流磁化率(alternating current susceptibility, AC)的量測，顯示化合物4·Dy在零磁場下觀察到磁緩現象，其磁異向能(Ueff)為46.3 K。
第二部分以L2作為多芽配位基，與Ni(ClO4)2·6H2O及Ln(ClO4)3 (aq, 50%)反應，合成一系列[NiIILnIII(L2)2(OH2)4(μ2-ClO4)](ClO4)2 (Ln = Y(7), Gd(8), Dy(9), Er(10))錯合物，並以X光單晶繞射確認其結構。Ni(II)為扭曲的八面體構型，而Ln(III)為十二面體構型，以過氯酸根離子與L2橋接Ln(III)及Ni(II)離子。直流磁化率測量結果，顯示化合物8·Gd—9·Dy金屬間存有鐵磁性作用力，而7·Y的磁化率隨著溫度下降，可能是由於分子間的反鐵磁性作用力，或是Ni(II)離子的自旋軌域耦合。在交流磁化率的量測部份，化合物9·Dy在零外加磁場下觀察到磁緩現象，其磁異向能(Ueff)為341.9 K，是至今鎳-鑭系金屬單分子磁鐵中磁異向能最高的，而10·Er在外加磁場下，在低溫範圍有明顯的拖尾訊號產生，是由於量子穿隧效應所導致。藉由比較4·Dy和9·Dy的配位環境和磁異向軸的差異，探討結構對於磁性表現的影響。
最後一個章節中，我們利用L3作為多芽配體，與Ni(ClO4)2·6H2O及Ln(ClO4)3 (aq, 50%)反應，合成一系列[NiII2LnIII(L3)4(OH2)4](ClO4)3 (Ln = Y(11), Gd(12), Tb(13), Dy(14))錯合物，由X光單晶繞射確認其結構。在交流磁化率的量測中，化合物14·Dy在零外加磁場下，於低溫範圍觀察到顯著的量子穿隧效應，其磁異向能(Ueff)為1.86 K。

This work contains three parts. The first part, a family of isostructural dinuclear heterometallic complexes [NiIILnIII(L1)2(OH2)(η2-OAc)(μ2-OAc)Cl]·0.5MeCN (Ln = Y(1), Gd(2), Tb(3), Dy(4), Ho(5), Er(6)) have been successfully synthesized by using β-diketone ligand of L1, and further determined the structures by single crystal X-ray crystallography. Structural studies demonstrate that Ln(III) ions are triangular dodecahedron geometry and Ni(II) ions are slightly distorted octahedral configuration. These two metal centers are bridged by two β-diketone ligands and one μ2-acetate group leading to a [NiIILnIII(μ-O)2(μ2-OAc)] core. Direct current (DC) magnetic susceptibility measurements reveal the presence of intramolecular ferromagnetic interactions in complexes 2·Gd—4·Dy. For 1·Y, existence of intermolecular antiferromagnetic interactions and/or spin-orbit coupling of Ni(II) ion could be observed. Alternating current (AC) magnetic susceptibility data indicate complexes 4·Dy exhibiting slow relaxations of the magnetization without DC field, and possessing the energy barrier (Ueff) of 46.3 K.
For the second part, a series of isostructural dinuclear heterometallic complexes [NiIILnIII(L2)2(OH2)4(μ2-ClO4)](ClO4)2 (Ln = Y(7), Gd(8), Dy(9), Er(10)) were successfully synthesized by using β-diketone ligand of L2. The structures were further identified by single crystal X-ray crystallography. The geometry of Ln(III) ions are triangular dodecahedron and Ni(II) ions are slightly distorted octahedral. The Ln(III) and Ni(II) ions are bridged by two β-diketone ligands and one μ2-perchlorate group, resulting in a [NiIILnIII (μ-O)2(μ2-ClO4)] core. DC magnetic susceptibility measurements display the presence of intramolecular ferromagnetic interactions in
complexes 8·Gd—9·Dy. In the AC magnetic susceptibility, complex 9·Dy performs slow relaxations of magnetization without applied DC field. Furthermore, the anisotropy energy of 9·Dy exhibits the highest Ueff(341.9 K) of all Ni-Ln complexes reported. By discussing the structural difference and the orientation of anisotropy axis, the factors leading to the variation of magnetic properties were comprehended.
The last part, a series of isostructural trinuclear heterometallic complexes [NiII2LnIII(L3)4(OH2)4](ClO4)3 (Ln = Y(11), Gd(12), Tb(13), Dy(14)) were synthesized by using a β-diketone ligand of L3. The structure of these four complexes were further determined by single crystal X-ray crystallography. DC magnetic susceptibility measurements reveal the presence of intramolecular ferromagnetic interactions in complexes 12·Gd—14·Dy. AC magnetic susceptibility data indicate complex 14·Dy presenting slightly slow relaxation and strong quantum tunneling of magnetization (QTM).

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