Abstract: | A novel borophosphate, Zn3(C6H14N2)3B6P12O39(OH)12] · (C6H14N2)HPO4] has been synthesised under mild hydrothermal conditions at T = 165 °C. The chiral crystal structure was determined by single crystal X‐ray diffraction data (trigonal, R3 (no. 146), Z = 3, a = 2089.55(4) pm, c = 1237.03(4) pm, V = 4677.5(2) · 106 pm3, R1 = 0.066, wR2 = 0.164 for 5100 observed reflections). The title compound can be considered as an ordered composite of the two different and neutral structures which fit into each other: An open framework of composition Zn3(C6H14N2)3B6P12O39(OH)12] and columns of composition (C6H14N2)HPO4]. The framework structure is formed by mixed octahedral‐tetrahedral secondary building units, in a three‐dimensional arrangement reflecting a hierarchical derivative of the NbO structure type. The underlying NbO topology is illustrated with the help of Periodic Nodal Surfaces. The composite nature of the compound is resolved in the spatial segregation of two frameworks with a separating surface. |