Crystal structure of (benzoylacetonato-κ2O,O′)dichloridodimethoxido niobium(V), C12H15Cl2NbO4

Leandra Herbst, Hendrik G. Visser, Andreas Roodt
2013 Zeitschrift für Kristallographie - New Crystal Structures  
C 12 H 15 Cl 2 NbO 4 ,triclinic, P1 (no. 2), a =7.899(2) Å, b =9.774(1) Å, c =10.780(2) Å, a =89.510 (3) Source of material NbCl 5 (0.1002 g, 0.37 mmol) was carefully dissolved in absolute methanol (5 ml) (Care: exothermicr eaction) and 1-phenyl-1,3butanedione (phacacH) (0.0603 g; 0.37 mmol) was added dropwise to the solution. The solution was stirred for 40 minutes and then left to stand at 293Kfor crystallization. Yellow plate-like crystals, suitable for single crystal X-Ray diffraction,
more » ... y diffraction, formed after 24 hours. (Yield: 0.1082 g, 76%). UV/Vis: l MeOH max =308 nm, e =1 94 cm -1 ·M -1 ; IR: n CO 1518.8, 1588.7 cm -1 . 1 HN MR (600 MHz, methanol-d 4 ): d =8.05 (m, Ph-5H), 4.87 (s, 1H),3.29 (s, OMe-6H), 2.21 (s,3H). 13 CNMR (600 MHz, methanol-d 4 ): d =194. 13, 182.96, 134.68, 132.13, 128.45, 126.63, 48.53, 26.01, 24.21. 93 Nb NMR (600 MHz, methanol-d 4 ): d =-1075.47 Experimental details Themethyland aromatic Hatoms were placed in geometrically idealizedpositions andconstrained to ride on theirparentatoms, with C-H =0 .95 and 0.98 Åa nd U iso (H) =1 .5U eq (C) and 1.2U eq (C), respectively. The highest peak is located 0.75 Åfrom Nb1 and the deepest hole is situated 0.58 Åfrom Cl1.
doi:10.1515/ncrs.2013.0212 fatcat:ajdfygex2jeaxmjiwc7dqgkka4