Abstract

A new organic-inorganic hybrid salt pipéridinium trans-diaquabis(oxalato)- chromate(III) tetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]·4H2O (1), has been synthesized in water and characterized by FTIR and UV-Vis spectroscopies, elemental and thermal analyses and by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic non-centrosymmetric space group Cmc21 with the unit cell parameters a = 7.4329(3), b = 9.9356(5), c = 23.6756(11) Å, α = β = γ = 90°, V = 1748.45(14) Å3 and Z = 4. The structure of 1 consists of [Cr(C2O4)2(H2O)2]- mononuclear anions, piperidinium cations and uncoordinated water molecules. The CrIII ion in the complex [Cr(C2O4)2(H2O)2]- is coordinated in a slightly distorted octahedral environment by four O atoms from two chelating oxalate dianions in the equatorial plane, and two O atoms from trans-coordinated water molecules occupying the apical positions. In the crystal, N-H···O and O-H···O hydrogen bond interactions connect the components into a 3-D framework. The IR spectrum of 1 is consistent with the presence of the various molecular building constituents, namely oxalato and aqua ligands, piperidinium cations and solvent water molecules. The UV-Vis spectrum shows two absorption bands around 564 and 416 nm which are compatible with an anionic chromium(III) complex in an octahedral environment. Thermal analysis shows a three-step decomposition of 1, leading to formation of a metal oxide residue.

Highlights

  • A great interest has been paid to the synthesis of novel organic-inorganic hybrid salt due to their structural diversity [1] and potential applications in gas storage [2], ion exchange and catalysis [3], photoluminescence [4] [5] and magnetism [6]

  • In continuation of the systematic search for other members of this family of materials, we report the synthesis, characterization and thermal analysis of a new organic-inorganic hybrid salt, piperidinium trans-diaquabis(oxalatoκ2O1,O2)chromate(III) tetrahydrate, (C5H10NH2)[Cr(C2O4)2(H2O)2]∙4H2O (1)

  • Packing diagram of 1, viewed along the b axis, showing its layered structure formed of pillars of alternating [Cr(C2O4)2(H2O)2]– complex anions and piperidinium (C5H10NH2)+ cations plus H2O molecules of crystallization (Figure 5)

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Summary

Introduction

A great interest has been paid to the synthesis of novel organic-inorganic hybrid salt due to their structural diversity [1] and potential applications in gas storage [2], ion exchange and catalysis [3], photoluminescence [4] [5] and magnetism [6] In this respect, the diaquabis(oxalato)metalate(III) complex anions, [MIII(C2O4)2(H2O)2]−, have been extensively used as building blocks for the generation of multifunctional materials formed by two distinct molecular networks, each furnishing a particular structural and physical property [7] [8] [9] [10]. Two aspects of focal relevance are associated with 1: a) its framework is non-centrosymmetric; b) the number of solvent water molecules per formula unit seems to be the highest obtained so far for this family of bis(oxalato)metalate(III) salts

Materials and Physical Measurements
Crystal Structure Determination and Refinement
Results and Discussion
Infrared Spectrum of 1
UV-Vis Spectrum of 1
Thermal Analysis of 1
Crystal Structure of 1
Conclusion
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