title: High-pressure single crystal X-ray diffraction study of the linear metal chain compound Co3(dpa)4Br2·CH2Cl2.
abstract: The crystal structure of the linear metal chain compound Co3(dpa)4Br2·CH2Cl2 (1) has been investigated up to a pressure of 13.6(2) GPa in a diamond anvil cell (DAC) using single crystal X-ray diffraction. The structure remains orthorhombic as the unit cell volume is reduced by 30% at 12.8 GPa. At 13.6(2) GPa the diffraction pattern is of very poor quality and not even reliable unit cell parameters can be determined. Peak broadening resulting from non-hydrostatic conditions was avoided by annealing the loaded DAC prior to data collection, allowing reliable structural models to be refined up to a pressure of 11.8(2) GPa. On increasing pressure, the disordered CH2Cl2 crystal solvent molecule gradually becomes redistributed from one site to another. Hirshfeld surface analysis suggests that the redistribution is a result of repulsive HH interactions. Pressure also affects the molecular geometry, in particular the Co-Co and Co-Br bond lengths which decrease by 4% and 12%, respectively, at 11.8(2) GPa.
authors.affiliation: Department of Chemistry and iNANO, Aarhus University, Langelandsgade 140, 8000 Aarhus C, Denmark. bo@chem.au.dk.
authors.forename: S R
authors.initials: SR
authors.lastname: Madsen
authors.forename: J
authors.initials: J
authors.lastname: Overgaard
authors.forename: D
authors.initials: D
authors.lastname: Stalke
authors.forename: B B
authors.initials: BB
authors.lastname: Iversen