A simple molecule with a complex crystal structure: interplay of 31P solid-state NMR spectroscopy and single-crystal x-ray diffraction in the structure determination of a ruthenium diphosphine diamine complex.
A comprehensive 31P solid-state NMR study of Ru(eta1-Ph2PCH2CH2OCH3)2(eta2-en)Cl2 (en = ethylenediamine) (1), by 1D (contact time variation, inversion-recovery, SPARTAN) and 2D techniques (homonuclear J-resolved, SECSY) indicated that the crystal structure of 1 should be complex. The single-crystal x-ray structure determination confirmed the presence of eight independent molecules in the asymmetric unit, with 31P isotropic chemical shifts in the range 27.3-40.1 ppm, while the spans of the phosphorus chemical shift tensors are of the order of 170 ppm. Based on unique structural features and NMR data, one molecule has been tentatively assigned.
Institut für Anorganische Chemie, Universität Tübingen, Auf der Morgenstelle 18, D-72076 Tübingen, Germany.
Klaus
K
Eichele
Christiane
C
Nachtigal
Susanne
S
Jung
Hermann A
HA
Mayer
Ekkehard
E
Lindner
Markus
M
Ströbele
D000465:Algorithms; D003198:Computer Simulation; D003460:Crystallization / Q000379:methods; D003461:Crystallography / Q000379:methods; D003959:Diamines / Q000032:analysis / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D008968:Molecular Conformation; D044367:Phase Transition; D010720:Phosphines / Q000032:analysis / Q000737:chemistry*; D010758:Phosphorus; D011208:Powders; D012428:Ruthenium / Q000032:analysis / Q000737:chemistry*; D014961:X-Ray Diffraction / Q000379:methods*
D003959:Diamines; D010720:Phosphines; D011208:Powders; D010758:Phosphorus; D012428:Ruthenium