Issue 91, 2015

Concise template syntheses of gallium phosphates driven by in situ direct alkylation of aliphatic and aromatic precursors by methanol

Abstract

A family of open-framework gallium phosphates (GaPOs), namely [dmdabco]0.5[Ga(HPO4)2] (1, dmdabco = N,N′-dimethyl-1,4-diazabicyclo[2,2,2]octane), [tmpip]0.5[Ga3(OH)(PO4)3]·(H2O)0.25 (2, tmpip = N,N,N′,N′-tetramethyl-piperazinium), [mpy][Ga3F(PO4)3]·(H2O)0.25 (3, mpy = N-methyl-pyridine), [dmbpy]0.5[Ga2(HPO4)2(PO4)] (4, dmbpy = N,N′-dimethyl-4,4′-bipyridine), and [Hmpip]2[Ga7(OH)(PO4)6(HPO4)2] (5, mpip = N-methylpiperazine) have been fabricated under hydro(solvo)thermal conditions and structurally characterized. The in situ-template-synthesis strategy is firstly used to construct the gallium phosphates. The in situ generated dmdabco2+, tmpip2+, mpy+ and dmbpy2+ templates were derived from the methylation of two distinct types of organic-amine precursors under methanol media: aliphatic 1,4-diazabicyclo[2,2,2]octane (dabco) in 1, 1,4-dimethylpiperazine or 1-methylpiperazine or piperazine (pip) in 2, and aromatic pyridine (py) in 3 and 4,4′-bipyridine (bpy) in 4. Such a unique in situ methylation feature is different from classic Eschweiler–Clarke methylation in which excessive formic acid and formaldehyde is needed. Compound 1 exhibits infinite inorganic chains connected by hydrogen bonds to generate a 3D supramolecular framework; compounds 2 and 3 are isomorphous and constructed from a Ga6P6 secondary building unit (SBUs), forming a 3D pcu architecture with intersecting 8-membered channels; compound 4 possesses an inorganic layered structure and compound 5 features an interesting 3D open-framework architecture with helical channels.

Graphical abstract: Concise template syntheses of gallium phosphates driven by in situ direct alkylation of aliphatic and aromatic precursors by methanol

Supplementary files

Article information

Article type
Paper
Submitted
25 Jun 2015
Accepted
26 Aug 2015
First published
26 Aug 2015

RSC Adv., 2015,5, 74811-74820

Concise template syntheses of gallium phosphates driven by in situ direct alkylation of aliphatic and aromatic precursors by methanol

G. Wang, J. Li, L. Wei, X. Zhang and Z. Bao, RSC Adv., 2015, 5, 74811 DOI: 10.1039/C5RA12300C

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