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Volume 65 
Part 7 
Page m776  
July 2009  

Received 30 May 2009
Accepted 8 June 2009
Online 17 June 2009


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Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.003 Å
Disorder in main residue
R = 0.035
wR = 0.092
Data-to-parameter ratio = 17.0
Details

trans-Bis(acetonitrile-[kappa]N)bis{1,2-bis[bis(3-hydroxypropyl)phosphino]ethane-[kappa]2P,P'}iron(II) dichloride

J. W. Gohdes,a Lev N. Zakharovb and David R. Tylerb*

aDepartment of Chemistry, Pacific University, 2043 College Way, Forest Grove, OR, USA, and bDepartment of Chemistry, 1253 University of Oregon, Eugene, Oregon 97403-1253, USA
Correspondence e-mail: dtyler@uoregon.edu

In the title compound, [Fe(CH3CN)2(C14H32O4P2)2]Cl2, the FeII atom lies on a crystallographic inversion center and has a distorted trans-FeN2P4 octahedral coordination environment arising from two P,P'-bidentate 1,2-bis[bis(3-hydroxypropyl)phosphino]ethane ligands in the equatorial plane and two acetonitrile molecules in the axial positions. One of the pendant -(CH2)3OH groups of the ligand is disordered over two sets of sites in a 0.597 (5):0.403 (5) ratio. In the crystal, O-H...Cl and O-H...O hydrogen bonding helps to establish the packing.

Related literature

For related compounds containing bidentate phosphine ligands, see: Gilbertson et al. (2007[Gilbertson, J. D., Szymczak, N. K., Crossland, J. L., Miller, W. K., Lyon, D. K., Foxman, B. M., Davis, J. & Tyler, D. R. (2007). Inorg. Chem. 46, 1205-1214.]); Miller et al. (2002[Miller, W. K., Gilbertson, J. D., Leiva-Paredes, C., Bernatis, P. R., Weakley, T. J. R., Lyon, K. D. & Tyler, D. R. (2002). Inorg. Chem. 41, 5453-5465.]); Martins et al. (1998[Martins, L. M. D. R. S., Duarte, M. T., Galvao, A. M., Resende, C., Pombiero, A. J. L., Henderson, R. A. & Evans, D. J. (1998). J. Chem. Soc. Dalton Trans. pp. 3311-3318.]); Barron et al. (1987[Barron, A. R., Wilkinson, G., Motevalli, M. & Hursthouse, M. B. (1987). Polyhedron, 6, 1089-1095.]); George et al. (1997[George, A. V., Field, L. D., Malouf, E. Y., McQueen, A. E. D., Pike, S. R., Purches, G. R., Hambley, T. W., Buys, I. E., White, A. H., Hockless, D. C. R. & Skelton, B. W. (1997). J. Organomet. Chem. 538, 101-110.]); Edwards et al. (2006[Edwards, P. E., Harrison, A., Newman, P. D. & Zhang, W. (2006). Inorg. Chim. Acta, 359, 3549-3556.]). For reference structural data, see: Allen et al. (1987[Allen, F. H., Kennard, O., Watson, D. G., Brammer, L., Orpen, A. G. & Taylor, R. (1987). J. Chem. Soc. Perkin Trans. 2, pp. S1-19.]).

[Scheme 1]

Experimental

Crystal data

  • [Fe(C2H3N)2(C14H32O4P2)2]Cl2

  • Mr = 861.53

  • Orthorhombic, P b c a

  • a = 18.3024 (12) Å

  • b = 11.5220 (8) Å

  • c = 19.8413 (13) Å

  • V = 4184.1 (5) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.69 mm-1

  • T = 173 K

  • 0.22 × 0.18 × 0.17 mm
Data collection

  • Bruker APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.863, Tmax = 0.892

  • 24288 measured reflections

  • 4571 independent reflections

  • 4122 reflections with I > 2[sigma](I)

  • Rint = 0.024
Refinement

  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.092

  • S = 1.04

  • 4571 reflections

  • 269 parameters

  • 7 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.88 e Å-3

  • [Delta][rho]min = -1.01 e Å-3

Table 1
Selected bond lengths (Å)

Fe1-N1 1.9077 (14)
Fe1-P1 2.2884 (4)
Fe1-P2 2.3049 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O1-H1O...Cl1 0.928 (17) 2.126 (18) 3.0493 (16) 173 (3)
O2-H2O...Cl1i 0.976 (18) 2.23 (2) 3.1777 (19) 164 (3)
O3-H3O...O1i 0.924 (17) 1.841 (18) 2.741 (2) 164 (2)
O4-H4O...Cl1ii 0.98 (2) 1.95 (2) 2.931 (6) 177 (3)
O4A-H4OA...Cl1ii 0.98 (2) 2.84 (11) 3.490 (10) 125 (9)
Symmetry codes: (i) x, y-1, z; (ii) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}].

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB2994 ).

Acknowledgements

We thank the NSF (CHE-0809393) for funding.

References

Allen, F. H., Kennard, O., Watson, D. G., Brammer, L., Orpen, A. G. & Taylor, R. (1987). J. Chem. Soc. Perkin Trans. 2, pp. S1-19.
Barron, A. R., Wilkinson, G., Motevalli, M. & Hursthouse, M. B. (1987). Polyhedron, 6, 1089-1095.  [CrossRef] [ChemPort]
Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Edwards, P. E., Harrison, A., Newman, P. D. & Zhang, W. (2006). Inorg. Chim. Acta, 359, 3549-3556.  [CrossRef] [ChemPort]
George, A. V., Field, L. D., Malouf, E. Y., McQueen, A. E. D., Pike, S. R., Purches, G. R., Hambley, T. W., Buys, I. E., White, A. H., Hockless, D. C. R. & Skelton, B. W. (1997). J. Organomet. Chem. 538, 101-110.  [CrossRef] [ChemPort]
Gilbertson, J. D., Szymczak, N. K., Crossland, J. L., Miller, W. K., Lyon, D. K., Foxman, B. M., Davis, J. & Tyler, D. R. (2007). Inorg. Chem. 46, 1205-1214.  [CrossRef] [PubMed] [ChemPort]
Martins, L. M. D. R. S., Duarte, M. T., Galvao, A. M., Resende, C., Pombiero, A. J. L., Henderson, R. A. & Evans, D. J. (1998). J. Chem. Soc. Dalton Trans. pp. 3311-3318.  [CrossRef]
Miller, W. K., Gilbertson, J. D., Leiva-Paredes, C., Bernatis, P. R., Weakley, T. J. R., Lyon, K. D. & Tyler, D. R. (2002). Inorg. Chem. 41, 5453-5465.  [CrossRef] [PubMed] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]

Acta Cryst (2009). E65, m776  [ doi:10.1107/S1600536809021758 ]

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