Azine bridged silver coordination polymers: Powder X-ray diffraction route to crystal structure determination of silver benzotriazole

• Published in: Journal of solid state chemistry 2006-04, Vol.179 (4), p.1053-1059
• Main Authors: Rajeswaran, Manju, Blanton, Thomas N., Giesen, David J., Whitcomb, David R., Zumbulyadis, Nicholas, Antalek, Brian J., Neumann, Marcus M., Misture, Scott T.
• Format: Article
• Language: English
• Subjects: ANNEALING; Benzotriazole; Condensed matter: structure, mechanical and thermal properties; DFT; Exact sciences and technology; INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; LATTICE PARAMETERS; MONOCLINIC LATTICES; MONOCRYSTALS; MONTE CARLO METHOD; Monte Carlo simulated annealing; NMR; NUCLEAR MAGNETIC RESONANCE; Organic compounds; Organometalloidal and organometallic compounds; Photothermographic material; Physics; Powder X-ray diffraction; Silver benzotriazole; Silver complex; SILVER COMPLEXES; Structure; Structure of solids and liquids; crystallography; Structure of specific crystalline solids; Synchrotron; X-RAY DIFFRACTION
• ISSN: 0022-4596; 1095-726X
• DOI: 10.1016/j.jssc.2006.01.022

In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, using a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic, ( P2 1 /c), with unit cell dimensions, a=14.8052(3) Å, b=3.7498(4) Å, c=12.3495(12) Å, and β=114.200(6)°. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer. The unit cell packing showing infinite cross-linked chains in the structure of AgBZT.