In the present paper, the synthesis and structure determination of a new three-dimensional microporous fluorogallophosphate, named Mu-12, is reported. This material (Ga20P16O72F4[C2N2H10]4) was obtained by hydrothermal synthesis in the presence of ethylenediamine as organic template, using the fluoride route. Its structure was determined by single-crystal X-ray diffraction. The symmetry is monoclinic, space group P21/n, with the following unit-cell parameters:  a = 14.3753(9) Å, b = 11.9410(7) Å, c = 10.1760(6) Å, and β = 91.102(5)°. The three-dimensional framework of Mu-12 can completely be built from ladder chains obtained by connection of four-membered rings (4MR), which consist of 2 Ga and 2 P atoms. These chains are connected to each other in the a and b directions through GaO6 octahedra. The resulting three-dimensional framework displays a one-dimensional channel system parallel to the [100] direction delimited by 9-MR openings and hosting the protonated amine. This material was characterized by elemental and thermal analyses, XRD, SEM, and 13C, 19F, and 31P solid-state NMR spectroscopy.

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