An X-ray powder study of the structure and microstructure of trans-dichloridobis(1,5-diamino-1H-tetrazole-κN4)palladium(II)

• Published in: Zeitschrift für Kristallographie. Crystalline materials Vol. 227; no. 10; pp. 702 - 709
• Main Authors: Ivashkevich, Ludmila S., Lyakhov, Alexander S., Serebryanskaya, Tatiyana V., Gaponik, Pavel N., Ivashkevich, Oleg A.
• Format: Journal Article
• Language: English
• Published: München Oldenbourg Wissenschaftsverlag GmbH 01.10.2012; Oldenbourg
• Subjects: Condensed matter: structure, mechanical and thermal properties; Cross-disciplinary physics: materials science; rheology; Exact sciences and technology; Materials science; Microstrains; Organic compounds; Other materials; Physics; Powder structure analysis; Specific materials; Structure of solids and liquids; crystallography; Structure of specific crystalline solids; Tetrazoles; X-ray diffraction; Rietveld method; Space groups; Square planar complex; Organometallic compounds; X-ray diffraction; Palladium; Tetrazoles; XRD; Monoclinic lattices; Direct method; Phenomenological model; Line broadening; Unit cell; Powder pattern; Anisotropy; Supramolecular structure; Microstrain; Powder structure analysis; Ligands; Microstructure; Intramolecular hydrogen bond; Crystal structure
• ISSN: 2194-4946; 2196-7105
• DOI: 10.1524/zkri.2012.1561

The crystal structure of the coordination compound [PdCl (CH ], -dichloridobis(1,5-diamino-1 -tetrazole- )palladium(II), has been determined from X-ray powder diffraction data collected at room temperature. The structure has been solved by direct methods and refined using Rietveld analysis. The complex crystallizes in the monoclinic space group , with Z=2. The unit cell dimensions are =5.73491(4), =11.94450(4), =8.61685(4)Å, and =99.6367(6)° with cell volume =581.930(5)Å . A slightly distorted square-planar coordination geometry is formed around the Pd atom by two Cl atoms and two tetrazole ring N atoms of two 1,5-diamino-1H-tetrazole ligands, which are in a configuration. In the complex molecule, the planes of the tetrazole rings are inclined at 53.7(3)° with respect to the coordination plane. Intermolecular hydrogen bonds of the amino groups N—H···Cl and N—H···N are responsible for formation of a three-dimensional supramolecular network. The powder pattern of the compound was strongly affected by the anisotropic line broadening. The width of the Bragg peaks was interpreted by a phenomenological microstructural approach in terms of anisotropic strain effect to complete the Rietveld refinement.