Rapid kinetics, complex and diverse reaction intermediates, and difficult screening make the study of assembly mechanisms of high-nuclearity lanthanide clusters challenging. Here, we synthesize a double-cage dysprosium cluster [Dy₆₀(H₂L¹)₂₄(OAc)₇₁(O)₅(OH)₃(H₂O)₂₇]·6H₂O·6CH₃OH·7CH₃CN (Dy₆₀) by using a multidentate chelate-coordinated diacylhydrazone ligand. Two Dy₃₀ cages are included in the Dy₆₀ structure, which are connected via an OAc⁻ moiety. The core of Dy₆₀ is composed of 8 triangular Dy₃ and 12-fold linear Dy₃ units. We further change the alkali added in the reaction system and successfully obtain a single cage-shaped cluster [Dy₃₀(H₂L¹)₁₂(OAc)₃₆(OH)₄(H₂O)₁₂]·2OH·10H₂O·12CH₃OH·13CH₃CN (Dy₃₀) with a perfect spherical cavity, which could be considered an intermediate in Dy₆₀ formation. Time-dependent, high-resolution electrospray ionization mass spectrometry (HRESI-MS) is used to track the formation of Dy₆₀. A possible self-assembly mechanism is proposed. We track the formation of Dy₃₀ and the six intermediate fragments are screened.

快速的动力学、复杂多样的反应中间体和困难的筛选使得高核镧系元素团簇组装机制的研究具有挑战性。在这里，我们合成了双笼形镝簇 [Dy ₆₀ (H ₂ L ¹ ) ₂₄ (OAc) ₇₁ (O) ₅ (OH) ₃ (H ₂ O) ₂₇ ]·6H ₂ O·6CH ₃ OH·7CH ₃ CN ( Dy ₆₀ ) 通过使用多齿螯合物配位的二酰基腙配体。Dy ₆₀中包含两个Dy ₃₀笼结构，它们通过 OAc ^-部分连接。Dy ₆₀的核心由8个三角形Dy ₃和12个线性Dy ₃单元组成。我们进一步改变了反应体系中加入的碱，成功获得了单笼状团簇[Dy ₃₀ (H ₂ L ¹ ) ₁₂ (OAc) ₃₆ (OH) ₄ (H ₂ O) ₁₂ ]·2OH·10H ₂ O ·12CH ₃ OH·13CH ₃ CN ( Dy ₃₀ ) 具有完美的球形空腔，可作为Dy的中间体₆₀阵型。随时间变化的高分辨率电喷雾电离质谱 (HRESI-MS) 用于追踪Dy ₆₀的形成。提出了一种可能的自组装机制。我们跟踪Dy ₃₀的形成并筛选了六个中间片段。