[Journal logo]

Volume 69 
Part 8 
Pages m475-m476  
August 2013  

Received 4 July 2013
Accepted 24 July 2013
Online 31 July 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.005 Å
R = 0.035
wR = 0.075
Data-to-parameter ratio = 17.3
Details
Open access

trans-Acetyldicarbonyl([eta]5-cyclopentadienyl)[tris(furan-2-yl)phosphane-[kappa]P]molybdenum(II)

aDepartment of Chemistry, Carleton College, 1 N. College St, Northfield, MN 55057, USA, and bDepartment of Chemistry, St Catherine University, 2004 Randolph Ave., St Paul, MN 55105, USA
Correspondence e-mail: mwhited@carleton.edu

The title compound, [Mo(C5H5)(C2H3O)(C12H9O3P)(CO)2], was prepared by reaction of [Mo(C5H5)(CO)3(CH3)] with tris(furan-2-yl)phosphane. The MoII atom exhibits a four-legged piano-stool coordination geometry with the acetyl and phosphine ligands trans to each other. The O atom of the acetyl ligand points down, away from the Cp ring. In the crystal, molecules form centrosymmetrical dimers via [pi]-[pi] interactions between furyl rings [the centroid-centroid distance is 3.396 (4) Å]. The dimers are linked by C-H...O hydrogen bonds into layers parallel to (100).

Related literature

For synthetic details for a related complex, see: Gladysz et al. (1979[Gladysz, J. A., Williams, G. M., Tam, W., Johnson, D. L., Parker, D. W. & Selover, J. C. (1979). Inorg. Chem. 18, 553-558.]). For related structures, see: Churchill & Fennessey (1968[Churchill, M. R. & Fennessey, J. P. (1968). Inorg. Chem. 7, 953-959.]); Barnett et al. (1972[Barnett, K. W., Pollman, T. G. & Solomon, T. W. (1972). J. Organomet. Chem. 36, C23-C26.]); Michelini-Rodriguez et al. (1993[Michelini-Rodriguez, I., Romero, A. L., Kapoor, R. N., Cervanres-Lee, F. & Pannell, K. H. (1993). Organometallics, 12, 1221-1224.]); Adams et al. (1997[Adams, H., Bailey, N. A., Blenkiron, P. & Morris, M. J. (1997). J. Chem. Soc. Dalton Trans. pp. 3589-3598.], 2000[Adams, H., Bailey, N. A., Blenkiron, P. & Morris, M. J. (2000). J. Chem. Soc. Dalton Trans. pp. 3074-3081.]); Whited et al. (2012[Whited, M. T., Boerma, J. W., McClellan, M. J., Padilla, C. E. & Janzen, D. E. (2012). Acta Cryst. E68, m1158-m1159.]).

[Scheme 1]

Experimental

Crystal data
  • [Mo(C5H5)(C2H3O)(C12H9O3P)(CO)2]

  • Mr = 492.28

  • Monoclinic, P 21 /c

  • a = 8.050 (2) Å

  • b = 15.762 (4) Å

  • c = 16.073 (4) Å

  • [beta] = 102.852 (8)°

  • V = 1988.4 (9) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.78 mm-1

  • T = 173 K

  • 0.24 × 0.17 × 0.15 mm

Data collection
  • Rigaku XtaLAB mini diffractometer

  • Absorption correction: multi-scan (REQAB; Rigaku, 1998[Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.709, Tmax = 0.890

  • 16222 measured reflections

  • 4539 independent reflections

  • 3799 reflections with I > 2[sigma](I)

  • Rint = 0.044

Refinement
  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.075

  • S = 1.06

  • 4539 reflections

  • 263 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.55 e Å-3

  • [Delta][rho]min = -0.52 e Å-3

Table 1
Selected bond lengths (Å)

Mo1-P1 2.4189 (8)
Mo1-C1 2.253 (4)
Mo1-C3 1.968 (3)
Mo1-C4 1.982 (3)
Mo1-C5 2.341 (4)
Mo1-C6 2.332 (4)
Mo1-C7 2.359 (3)
Mo1-C8 2.374 (4)
Mo1-C9 2.382 (4)
O1-C1 1.227 (4)
O2-C3 1.150 (4)
O3-C4 1.148 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C8-H8...O1i 1.00 2.38 3.324 (4) 158
C11-H11...O1i 0.95 2.40 3.166 (5) 137
Symmetry code: (i) [x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}].

Data collection: CrystalClear (Rigaku Americas and Rigaku, 2011[Rigaku Americas and Rigaku (2011). CrystalClear. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: CrystalStructure (Rigaku Americas and Rigaku, 2010[Rigaku Americas and Rigaku (2010). CrystalStructure. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.]); software used to prepare material for publication: CrystalStructure.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: KQ2007 ).


Acknowledgements

The authors gratefully acknowledge St. Catherine University and NSF-MRI award #1125975 "MRI Consortium: Acquisition of a Single Crystal X-ray Diffractometer for a Regional PUI Molecular Structure Facility". Additional funding was provided by a grant to Carleton College from the Howard Hughes Medical Institute and from the Department of Chemistry at Carleton College.

References

Adams, H., Bailey, N. A., Blenkiron, P. & Morris, M. J. (1997). J. Chem. Soc. Dalton Trans. pp. 3589-3598.  [CrossRef]
Adams, H., Bailey, N. A., Blenkiron, P. & Morris, M. J. (2000). J. Chem. Soc. Dalton Trans. pp. 3074-3081.  [CrossRef]
Barnett, K. W., Pollman, T. G. & Solomon, T. W. (1972). J. Organomet. Chem. 36, C23-C26.  [CrossRef] [ChemPort]
Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Churchill, M. R. & Fennessey, J. P. (1968). Inorg. Chem. 7, 953-959.  [CrossRef] [ChemPort] [Web of Science]
Gladysz, J. A., Williams, G. M., Tam, W., Johnson, D. L., Parker, D. W. & Selover, J. C. (1979). Inorg. Chem. 18, 553-558.  [CrossRef] [ChemPort] [Web of Science]
Michelini-Rodriguez, I., Romero, A. L., Kapoor, R. N., Cervanres-Lee, F. & Pannell, K. H. (1993). Organometallics, 12, 1221-1224.
Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan.
Rigaku Americas and Rigaku (2010). CrystalStructure. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
Rigaku Americas and Rigaku (2011). CrystalClear. Rigaku Americas, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Whited, M. T., Boerma, J. W., McClellan, M. J., Padilla, C. E. & Janzen, D. E. (2012). Acta Cryst. E68, m1158-m1159.  [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m475-m476   [ doi:10.1107/S160053681302059X ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.