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Volume 64 
Part 8 
Page o1449  
August 2008  

Received 23 June 2008
Accepted 2 July 2008
Online 9 July 2008

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Key indicators
Single-crystal X-ray study
T = 228 K
Mean [sigma](C-C) = 0.002 Å
R = 0.042
wR = 0.118
Data-to-parameter ratio = 23.9
Details
Open access

P,P-Diphenyl-N-(1,1,2,2-tetraphenyl-1[lambda]5-diphosphanylidene)phosphinous amide

Diane A. Dickiea and Richard A. Kempa*+

aDepartment of Chemistry and Chemical Biology, MSC03 2060, 1 University of New Mexico, Albuquerque, NM 87131, USA
Correspondence e-mail: rakemp@unm.edu

The title compound, C36H30NP3, a structural isomer of tris(diphenylphosphino)amine, was unexpectedly isolated as the sole phosphorus-containing product from the reaction of Mg[N(PPh2)2]2(THF)2 (THF is tetrahydrofuran) with CO2. Its identity was confirmed by 31P NMR spectroscopy and single-crystal X-ray diffraction. The geometry at the two P(III) atoms is trigonal pyramidal, while the P(V) atom adopts a distorted tetrahedral geometry.

Related literature

For the original synthesis and spectroscopic characterization of the title compound, see: Nöth & Meinel (1967[Nöth, N. & Meinel, L. (1967). Z. Anorg. Allg. Chem. 349, 225-240.]); Meinel & Nöth (1970[Meinel, L. & Nöth, H. (1970). Z. Anorg. Allg. Chem. 373, 36-47.]). For the crystallographic characterization of the structural isomer N[P(C6H5)2]3, see: Ellermann et al. (1987[Ellermann, J., Köck, E., Zimmermann, H. & Gomm, M. (1987). Acta Cryst. C43, 1795-1798.]). For related literature, see: Bruno et al. (2004[Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144.]).

[Scheme 1]

Experimental

Crystal data

  • C36H30NP3

  • Mr = 569.52

  • Monoclinic, P 21 /n

  • a = 9.3026 (13) Å

  • b = 10.8167 (15) Å

  • c = 29.750 (4) Å

  • [beta] = 98.589 (6)°

  • V = 2960.0 (7) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.23 mm-1

  • T = 228 (2) K

  • 0.57 × 0.51 × 0.18 mm
Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.88, Tmax = 0.96

  • 76797 measured reflections

  • 11496 independent reflections

  • 9167 reflections with I > 2[sigma](I)

  • Rint = 0.029
Refinement

  • R[F2 > 2[sigma](F2)] = 0.042

  • wR(F2) = 0.118

  • S = 1.05

  • 11496 reflections

  • 481 parameters

  • All H-atom parameters refined

  • [Delta][rho]max = 0.41 e Å-3

  • [Delta][rho]min = -0.29 e Å-3

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 1999[Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2008[Westrip, S. P. (2008). publCIF. In preparation.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: AT2581 ).

Acknowledgements

The authors thank Eileen Duesler (UNM) for the X-ray data collection. Funding was provided by the Natural Sciences and Engineering Research Council of Canada (NSERC PDF to DAD), the National Science Foundation (grant Nos. CHE-0213165 and CHE-0443580) and the Sandia LDRD Program (grant Nos. 105932 and 113486). Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under contract No. DE-AC04-94AL85000.

References

Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2003). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2004). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144.  [ISI] [CrossRef] [PubMed] [ChemPort]
Ellermann, J., Köck, E., Zimmermann, H. & Gomm, M. (1987). Acta Cryst. C43, 1795-1798.  [CrossRef] [details]
Meinel, L. & Nöth, H. (1970). Z. Anorg. Allg. Chem. 373, 36-47.  [CrossRef] [ChemPort]
Nöth, N. & Meinel, L. (1967). Z. Anorg. Allg. Chem. 349, 225-240.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2008). publCIF. In preparation.

Acta Cryst (2008). E64, o1449  [ doi:10.1107/S1600536808020412 ]

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