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Synthesis and characterization of metallophosphenium ion complexes derived from aminohalophosphites. Crystal and molecular structure of Mo(η5-C5H5)(CO)2[POCH 2CH2NC(CH3)3]
Hutchins, Larry D.,Duesler, Eileen N.,Paine, Robert T.
, p. 399 - 403 (2008/10/08)
The reactions of RNCH2CH2OPX (R = CH3, C2H5, C(CH3)3, C6H5; X = F, Cl) with NaMo(η5-C5H5)(CO)3 in THF at 25°C result in the formation of a series of metallophosphenium ion complexes Mo(η5-C5H5)(CO)2[POCH 2CH2NR]. The complexes have been characterized by infrared and 1H, 13C, and 31P NMR spectroscopy, and a single-crystal X-ray diffraction analysis of Mo(η5-C5H5)(CO)2[POCH 2CH2NC(CH3)3] has been completed. The compound crystallizes in the monoclinic space group P21/n with a = 12.072 (2) A?, b = 9.957 (2) A?, c = 13.349 (3) A?, β = 108.09 (1)°, Z = 4, V = 1525.2 (5) A?3, and ρ = 1.58 g cm-3. Least-squares refinement gave Rf = 3.5% and RwF = 3.0% on 2310 unique reflections with I > 2.5σ(I). The molecular structure displays a pseudooctahedral molybdenum atom bonded to a (η5-C5H5) ring, two terminal carbonyls, and the phosphorus atom of the phosphenium ion [POCH2CH2NC(CH3)3+]. The phosphenium ion is planar and the Mo-P bond distance, 2.207 (1) A?, is short.
