114184-47-3Relevant academic research and scientific papers
Synthesis and alkylation of an iron phosphane complex. Crystal and molecular structure determinations for CpFe(CO)2{P(C6H5){N[Si(CH3) 3]2}} and CpFe(CO)2{P(CH3)(C6H5){N[Si(CH 3)3]2+}}(O3SCF 3-)
McNamara, William F.,Reisacher,Duesler, Eileen N.,Paine, Robert T.
, p. 1313 - 1317 (1988)
The reactions of NaFe(C5H5)(CO)2 and NaFe[(CH3)5C5](CO)2 with (C6H5)P(Cl){N[Si(CH3)3]2} form iron phosphane compounds (C5H5)Fe(CO)2{P(C6H 5){N[Si(CH3)3]2}} (1) and [(CH3)5C5]Fe(CO)2{P(C 6H5){N[Si-(CH3)3]2}} (2) which have been characterized by spectroscopic methods, and the crystal and molecular structure of 1 has been determined by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/n with a = 10.871 (2) ?, b = 18.231 (4) ?, c = 11.561 (2) ?, β = 95.89 (2)°, Z = 4, V = 2279.1 (7) ?3, and ρ = 1.30 g cm-3. Least-squares refinement gave RF = 5.5% and RwF = 5.2% on 2894 unique data with F > 5σ(F). The molecular structure contains a CpFe(CO)2 unit bonded to a pyramidal P(C6H5){N[Si(CH3)3]2} fragment through a long Fe-P bond distance, 2.338 (1) ?. Reactions of 1 with (CH3)3OBF4 and CH3O3SCF3 result in methylation of the phosphorus center, and the products have been characterized by spectroscopic methods. The crystal and molecular structure of (C5H5)Fe-(CO)2{P(CH3)(C 6H5){N[Si(CH3)3]2}} +(O3SCF3-) has been determined by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/n with a = 11.571 (4) ?, b = 17.590 (5) ?, c = 14.200 (3) ?, β = 104.91 (2)°, Z = 4, V = 2792 (1) ?3, and ρ = 1.45 g cm-3. Least-squares refinement gave RF = 9.4% and RwF = 9.7% on 2966 unique reflections with F > 5σ(F). The molecular structure is related to the structure of 1 with the addition of a methyl group on the pyramidal phosphorus center. The addition results in a shorter Fe-P bond distance, Fe-P = 2.263 (3) ?, and P-CH3 = 1.82 (1) ?.
