Abstract A new 3D-layered inorganic-organic hybrid, [D/L-C6H13O2N-H]3[(PO4)W12O36].4.5H2O (1), as racemic material in the solid phase, has been synthesized and fully characterized by elemental microanalysis, single crystal X-ray diffraction, and infrared, Raman, and proton nuclear magnetic resonance spectroscopies. The most unique structural feature of 1 is its three-dimensional inorganic infinite tunnel-like framework that results in weak van der Waals interactions along the a-axis. A weak interlayer interaction between the titled layers provides a desirable condition to explore its potential as a host in a host-guest complex. The racemization has been observed in the crystal structure with the centric space group (P21/c). The latter consists of α-[(PO4)W12O36]3-and [D/L-C6H13O2N-H]+ moieties with water molecules linked together by a complex network of hydrogen bond interactions.

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