The organic-inorganic hybrid compound (C13H28N2) BiCl5 was synthesized by solvothermal method. The crystal structure was solved by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic system space group Cmc21 with (4)？？, (6)？？, (3)？？, and . The crystal structure was refined down to . It consists of corrugated layers of [BiCl5]2？ chains, separated by organic [H2TMDP]2+ cations (TMDP=1,3-Bis(4-piperidyl)propane = C13H26N2). The crystal cohesion is achieved by hydrogen bonds joining the organic and inorganic layers. The influence of the organic cations' flexibility is discussed. Raman and infrared spectra of the title compound were recorded in the range of 50–400 and 400–4000？cm？1, respectively. Semiempirical parameter model three (PM3) method has been performed to derive the calculated IR spectrum. The crystal shape morphology was simulated using the Bravais-Friedel and Donnay-Harker model. 1. Introduction Halobismuthates organic-inorganic hybrids are interesting systems because of the opportunity to combine the organic and the inorganic materials’ proprieties. Nowadays, these compounds are the subject of intense investigations in many fields like optoelectronics and semiconducting [1–4]. The anionic sublattices of these materials are often built up by distorted [BiX6]3？ octahedra ( ). These octahedra can be isolated or linked by corners, edges, or faces leading to low dimensional inorganic framework. It is still a great challenge to control the structure dimensionalities of metal-halide anionic frameworks. In fact, the structural type depends on the experimental conditions, such as the solvent, ratio of reagents, and temperature. The organic cation size, charge, steric encumbrance, and the conformation can have a decisive influence. The organic moiety can be used as physical and electronic barrier, contributing to original electrical and optical behavior [5–8]. In these materials the crystal packing is directed by the interactions between the components constituting the solid such as hydrogen bonding, Van Der Waals, and electrostatic interactions. In this work we present the results of the structural and spectroscopic studies on a new pentachlorobismuthate-based hybrid compound. Semiempirical parameter model three (PM3) computations are used in order to perform the vibrational analysis of the studied structure. 2. Materials and Methods 2.1. Synthesis In a 23？mL teflon autoclave, a mixture of bismuth chloride BiCl3 and 1,3-bis(4-pyridyl) propane (TMDP) in molar ratio 1？:？2 was dissolved in 10？mL of absolute ethanol. The
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