Abstract
The structures of (3,3′,4,4′-tetramethyl-1,1′-diphosphaferrocen-2-yl)carboxylic acid (1) and its bis-[W(CO)5] pentane solvate complex (2) have been determined by X-ray analysis. The compound 1 crystallizes in the monoclinic P21 /n space group with Z = 4; a = 7.8404(9), b = 14.9441(16), c = 11.7730(14) Å, β = 92.773(10)°, V = 1377.8(3) Å3, and Dcalc = 1.553 g cm−3. The compound 2 crystallizes in the triclinic \(P\bar 1\) space group with two complex molecules and one pentane molecule in the unit cell. Cell parameters: a = 10.7070(2), b = 12.577(2), c = 13.239(3) Å, α = 84.00(2), β = 77.58(1), γ = 66.06(1)°, V = 1591.0(5) Å3, and Dcalc = 2.100 g cm−3 .The fully eclipsed conformation of the phospholyl rings with P···P secondary bonding of 3.353(1) Å is observed in 1 and a partially eclipsed conformation is found in 2. The 10 possible conformations of 1,1′-diphosphaferrocenes were described as the function of conformational parameter θ and observed geometry of the phospholyl rings.7 We suppose that the earlier conclusions concerning the destabilizing nature of 1,1′-diphosphaferrocene conformations with θ < 100° cannot be considered as general. The mode of W – P coordination, the structural changes of 1 by W(CO)5 coordination, the structural effect of phospholyl rings substitution by the –COOH group, and hydrogen bonds are analyzed.
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de Lauzon, G.; Deschamps, B.; Fischer, J.; Mathey, F.; Mitschler, A. J. Am. Chem. Soc. 1980, 102, 994.
Hitchcock, P.B.; Lawless, G.A.; Marziano, I. J. Organomet. Chem. 1997, 527, 305.
Qiao, S.; Hoic, D.A.; Fu, G.C. Organometallics 1998, 17, 773.
Zakrzewski, J.; Klys, A.; Bukowska-Strzyzewska M.; Tosik, A. Organometallics 1998, submitted.
Ashe III, A.J.; Kampf, J.W.; Pilotek, S.; Rousseau, R. Organometallics 1994, 13, 4067.
de Lauzon, G.; Deschamps, B.; Mathey, F. Nouv. J. Chim. 1980, 4, 683.
Ashe III, A.J.; Al.-Ahmad, S. Advan. Organometal. Chem. 1996, 39, 326.
Atwood, D.A.; Cowley, A.H.; Dennis, S.M. Inorg. Chem. 1993, 32, 1527.
Silver, J.; Zakrzewski, J.; Tosik, A.; Bukowska-Strzyżewska, M. J. Organomet. Chem. 1997, 540, 169.
Sheldrick, G.M. (1997) SHELXL-97. Release 97-1. Program for the Refinement of Crystal Structures; University of Göttingen: Germany.
Sheldrick, G.M. (1997) SHELXS-97. Release 97-1. Program for the Solution of Crystal Structures; University of Göttingen: Germany.
North, A.C.T.; Phillips, D.C.; Mathews, F.S. Acta Crystallogr. 1968, A24, 351.
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Sieroń, L., Tosik, A. & Bukowska-Strzyżewska, M. Crystal structure of (3,3′,4,4′-tetramethyl-1,1′-diphosphaferrocen-2-yl) carboxylic acid and its bis-[W(CO)5] complex·0.5C5H12: Conformation of 1,1′-diphosphaferrocenes. Journal of Chemical Crystallography 28, 621–628 (1998). https://doi.org/10.1023/A:1022413026427
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DOI: https://doi.org/10.1023/A:1022413026427