Very Large Breathing Effect in the First Nanoporous Chromium(III)-Based Solids: MIL-53 or CrIII(OH)·{O2C−C6H4−CO2}·{HO2C−C6H4−CO2H}x·H2Oy

Serre, Christian, Millange, Franck, Thouvenot, Christelle, Noguès, Marc, Marsolier, Gérard, Louër, Daniel, Férey, Gérard·2002·Journal of the American Chemical Society

DOI 10.1021/ja0276974

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Abstract

The first three-dimensional chromium(III) dicarboxylate, MIL-53as or Cr(III)(OH) x [O(2)C-C(6)H(4)-CO(2)].[HO(2)C-C(6)H(4)-CO(2)H](0.75), has been obtained under hydrothermal conditions (as: as-synthesized). The free acid can be removed by calcination giving the resulting solid, MIL-53ht or Cr(III)(OH) x [O(2)C-C(6)H(4)-CO(2)]. At room temperature, MIL-53ht adsorbs atmospheric water immediately to give Cr(III)(OH) x [O(2)C-C(6)H(4)-CO(2)] x H(2)O or MIL-53lt (lt: low-temperature form, ht: high-temperature form). Both structures, which have been determined by using X-ray powder diffraction data, are built up from chains of chromium(III) octahedra linked through terephthalate dianions. This creates a three-dimensional structure with an array of one-dimensional large pore channels filled with free disordered terephthalic molecules (MIL-53as) or water molecules (MIL-53lt); when the free molecules are removed, this leads to a nanoporous solid (MIL-53ht) with a Langmuir surface area over 1500 m(2)/g. The transition between the hydrated form (MIL-53lt) and the anhydrous solid (MIL-53ht) is fully reversible and followed by a very high breathing effect (more than 5 A), the pores being clipped in the presence of water molecules (MIL-53lt) and reopened when the channels are empty (MIL-53ht). The thermal behavior of the two solids has been investigated using TGA and X-ray thermodiffractometry. The sorption properties of MIL-53lt have also been studied using several organic solvents. Finally, magnetism measurements performed on MIL-53as and MIL-53lt revealed that these two phases are antiferromagnetic with Néel temperatures T(N) of 65 and 55 K, respectively. Crystal data for MIL-53as is as follows: orthorhombic space group Pnam with a = 17.340(1) A, b = 12.178(1) A, c = 6.822(1) A, and Z = 4. Crystal data for MIL-53ht is as follows: orthorhombic space group Imcm with a = 16.733(1) A, b = 13.038(1) A, c = 6.812(1) A, and Z = 4. Crystal data for MIL-53lt is as follows: monoclinic space group C2/c with a = 19.685(4) A, b = 7.849(1) A, c = 6.782(1) A, beta = 104.90(1) degrees, and Z = 4.

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Authors: Serre, C., Millange, F., Thouvenot, C., Noguès, M., Marsolier, G., Louër, D., & Férey, G.
Venue: Journal of the American Chemical Society
Publisher: American Chemical Society (ACS)
Published: 2002-10-19
Volume: 124
Issue: 45
Pages: 13519-13526
ISSN: 0002-7863 (ISSN-L)
1520-5126
DOI: 10.1021/ja0276974
OpenAlex: W2318044185
Cited by: 1,980
References: 0
FWCI: 20.42
Type: journal article
Language: en
Open access: closed

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Very Large Breathing Effect in the First Nanoporous Chromium(III)-Based Solids: MIL-53 or CrIII(OH)·{O2C−C6H4−CO2}·{HO2C−C6H4−CO2H}x·H2Oy

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