Gigantic coordination molecules assembled from a large number of metal ions and organic ligands are structurally and functionally challenging to characterize. Here we show that a heterometallic cluster [Ni₃₆Gd₁₀₂(OH)₁₃₂(mmt)₁₈(dmpa)₁₈(H₂dmpa)₂₄(CH₃COO)₈₄(SO₄)₁₈(NO₃)₁₈(H₂O)₃₀]·Br₆(NO₃)₆·(H₂O)x·(CH₃OH)y, (1, x ≈ 130, y ≈ 60), shaped like a "Star of David", can be synthesized using a "mixed-ligand" and "sulfate-template" strategy. In terms of metal nuclearity number, 1 is the second largest 3d-4f cluster to date. In the solid state, 1 is porous after removing the lattice guests. The N₂ adsoption experiment reveals that the BET and Langmuir surface areas are 299.8 and 412.0 cm² g⁻¹, respectively. CO₂ adsorption at 298 K gives the amount of 45 cm³ g⁻¹ for 1. More importantly, 1 is soluble in common organic solvents and exhibits high solution stability revealed by high resolution MALDI-TOF mass spectroscopy, small-angle X-ray scattering (SAXS), and low-dose transmission electron microscopy. The solubility and the potential open metal sites owing to the labile coordinating components prompted us to investigate the photocatalytic properties of 1, which displays high selectivity and efficiency for reduction of CO₂ to CO with turnover number and turnover frequency of 29700 and 1.2 s⁻¹, respectively. These values are higher than most catalysts working under the same conditions, presumably due to the strong Ni-CO₂ binding effect. In addition, the large percentage of Gd(III) in 1 leads to a large magnetic entropy change (41.3 J·kg⁻¹·K⁻¹) at 2.0 K for ΔH = 7 T.
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Chen et al. (2020) studied this question.
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