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Cummins CC, Huang C, Miller TJ, et al. The stannylphosphide anion reagent sodium bis(triphenylstannyl) phosphide: synthesis, structural characterization, and reactions with indium, tin, and gold electrophiles. Inorg Chem. 2014;53(7):3678-87doi: 10.1021/ic403178j.
Cummins, C. C., Huang, C., Miller, T. J., Reintinger, M. W., Stauber, J. M., Tannou, I., Tofan, D., Toubaei, A., Velian, A., & Wu, G. (2014). The stannylphosphide anion reagent sodium bis(triphenylstannyl) phosphide: synthesis, structural characterization, and reactions with indium, tin, and gold electrophiles. Inorganic chemistry, 53(7), 3678-87. https://doi.org/10.1021/ic403178j
Cummins, Christopher C, et al. "The stannylphosphide anion reagent sodium bis(triphenylstannyl) phosphide: synthesis, structural characterization, and reactions with indium, tin, and gold electrophiles." Inorganic chemistry vol. 53,7 (2014): 3678-87. doi: https://doi.org/10.1021/ic403178j
Cummins CC, Huang C, Miller TJ, Reintinger MW, Stauber JM, Tannou I, Tofan D, Toubaei A, Velian A, Wu G. The stannylphosphide anion reagent sodium bis(triphenylstannyl) phosphide: synthesis, structural characterization, and reactions with indium, tin, and gold electrophiles. Inorg Chem. 2014 Apr 07;53(7):3678-87. doi: 10.1021/ic403178j. Epub 2014 Mar 12. PMID: 24621383.
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Inorg Chem. 2014 Apr 07;53(7):3678-87. doi: 10.1021/ic403178j. Epub 2014 Mar 12.

The stannylphosphide anion reagent sodium bis(triphenylstannyl) phosphide: synthesis, structural characterization, and reactions with indium, tin, and gold electrophiles.

Inorganic chemistry

Christopher C Cummins, Chao Huang, Tabitha J Miller, Markus W Reintinger, Julia M Stauber, Isabelle Tannou, Daniel Tofan, Abouzar Toubaei, Alexandra Velian, Gang Wu

Affiliations

  1. Department of Chemistry, Massachusetts Institute of Technology , Cambridge, Massachusetts 02139-4307, United States.

PMID: 24621383 DOI: 10.1021/ic403178j

Abstract

Treatment of P4 with in situ generated [Na][SnPh3] leads to the formation of the sodium monophosphide [Na][P(SnPh3)2] and the Zintl salt [Na]3[P7]. The former was isolated in 46% yield as the crystalline salt [Na(benzo-15-crown-5)][P(SnPh3)2] and used to prepare the homoleptic phosphine P(SnPh3)3, isolated in 67% yield, as well as the indium derivative (XL)2InP(SnPh3)2 (XL = S(CH2)2NMe2), isolated in 84% yield, and the gold complex (Ph3P)AuP(SnPh3)2. The compounds [Na(benzo-15-crown-5)][P(SnPh3)2], P(SnPh3)3, (XL)2InP(SnPh3)2, and (Ph3P)AuP(SnPh3)2 were characterized using multinuclear NMR spectroscopy and X-ray crystallography. The bonding in (Ph3P)AuP(SnPh3)2 was dissected using natural bond orbital (NBO) methods, in response to the observation from the X-ray crystal structure that the dative P:→Au bond is slightly shorter than the shared electron-pair P-Au bond. The bonding in (XL)2InP(SnPh3)2 was also interrogated using (31)P and (13)C solid-state NMR and computational methods. Co-product [Na]3[P7] was isolated in 57% yield as the stannyl heptaphosphide P7(SnPh3)3, following salt metathesis with ClSnPh3. Additionally, we report that treatment of P4 with sodium naphthalenide in dimethoxyethane at 22 °C is a convenient and selective method for the independent synthesis of Zintl ion [Na]3[P7]. The latter was isolated as the silylated heptaphosphide P7(SiMe3)3, in 67% yield, or as the stannyl heptaphosphide P7(SnPh3)3 in 65% yield by salt metathesis with ClSiMe3 or ClSnPh3, respectively.

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