[Journal logo]

Volume 64 
Part 2 
Pages m369-m370  
February 2008  

Received 5 January 2008
Accepted 11 January 2008
Online 16 January 2008

[wk2075sup1]
[3d view]

[Cited in]
[Download citation]
Key indicators
Single-crystal X-ray study
T = 122 K
Mean [sigma](C-C) = 0.003 Å
R = 0.032
wR = 0.146
Data-to-parameter ratio = 12.2
Details
Open access

cis-Difluoridobis(1,10-phenanthroline)chromium(III) perchlorate monohydrate

Torben Birk,a* Jesper Bendixa and Högni Weihea

aDepartment of Chemistry, University of Copenhagen, Universitetsparken 5, DK-2100 København Ø, Denmark
Correspondence e-mail: Birk@kiku.dk

The title complex, [CrF2(C12H8N2)2]ClO4·H2O, displays a slightly distorted octahedral coordination geometry around the central chromium(III) ion. The Cr environment is composed of a cis arrangement of two 1,10-phenanthroline [average CrIII-N = 2.0726 (10) Å] and two fluoride [average CrIII-F = 1.8533 (6) Å] ligands. The water molecule forms a hydrogen bond to fluorine in a neighbouring cation.

Related literature

For details of the general synthesis of amine-containing difluorido complexes of chromium(III), see: Glerup et al. (1970[Glerup, J., Josephsen, J., Michelsen, K., Pedersen, E. & Schäffer, C. E. (1970). Acta Chem. Scand. 24, 247-254.]). For the structure of the analogous 2,2'-bipyridine complex, see: Yamaguchi-Terasaki et al. (2007[Yamaguchi-Terasaki, Y., Fujihara, T., Nagasawa, A. & Kaizaki, S. (2007). Acta Cryst. E63, m593-m595.]). For related literature, see: Brencic et al. (1981[Brencic, J. V., Leban, I. & Polanc, I. (1981). Monatsh. Chem. 112, 1359-1368.], 1987[Brencic, J. V., Ceh, B. & Leban, I. (1987). Z. Anorg. Allg. Chem. 551, 109-115.]); Delavar & Staples (1981[Delavar, M. & Staples, P. J. (1981). J. Chem. Soc. Dalton Trans. pp. 981-985.]); Kaizaki & Takemoto (1990[Kaizaki, S. & Takemoto, H. (1990). Inorg. Chem. 29, 4960-4964.]); Kane-Maguire et al. (1986[Kane-Maguire, N. A. P., Wallace, K. C. & Speece, D. G. (1986). Inorg. Chem. 25, 4650-4654.]).

[Scheme 1]

Experimental

Crystal data

  • [CrF2(C12H8N2)2]ClO4·H2O

  • Mr = 567.87

  • Triclinic, [P \overline 1]

  • a = 7.6930 (10) Å

  • b = 9.4640 (8) Å

  • c = 16.0610 (17) Å

  • [alpha] = 79.750 (7)°

  • [beta] = 83.228 (12)°

  • [gamma] = 88.115 (8)°

  • V = 1142.6 (2) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.68 mm-1

  • T = 122 (1) K

  • 0.44 × 0.41 × 0.16 mm
Data collection

  • Nonius KappaCCD area-detector diffractometer

  • Absorption correction: Gaussian integration (Coppens, 1970[Coppens, P. (1970). Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall & C. P. Huber, pp. 255-270. Copenhagen: Munksgaard.]) Tmin = 0.794, Tmax = 0.913

  • 28606 measured reflections

  • 4014 independent reflections

  • 3851 reflections with I > 2[sigma](I)

  • Rint = 0.025
Refinement

  • R[F2 > 2[sigma](F2)] = 0.031

  • wR(F2) = 0.145

  • S = 1.41

  • 4014 reflections

  • 329 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.79 e Å-3

  • [Delta][rho]min = -0.51 e Å-3

Table 1
Selected geometric parameters (Å, °)

Cr1-F2 1.8444 (10)
Cr1-F1 1.8621 (10)
Cr1-N4 2.0566 (15)
Cr1-N2 2.0607 (15)
Cr1-N3 2.0797 (16)
Cr1-N1 2.0934 (15)
F2-Cr1-F1 95.92 (5)
F2-Cr1-N4 92.33 (5)
F1-Cr1-N4 91.42 (5)
F2-Cr1-N2 91.83 (6)
F1-Cr1-N2 91.86 (5)
N4-Cr1-N2 174.40 (5)
F2-Cr1-N3 89.38 (5)
F1-Cr1-N3 170.08 (5)
N4-Cr1-N3 79.95 (6)
N2-Cr1-N3 96.36 (6)
F2-Cr1-N1 170.54 (5)
F1-Cr1-N1 88.67 (5)
N4-Cr1-N1 95.83 (6)
N2-Cr1-N1 79.72 (6)
N3-Cr1-N1 87.34 (6)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O5-H5B...F1i 1.03 1.69 2.7183 (19) 175
Symmetry code: (i) x-1, y, z.

Data collection: COLLECT (Nonius, 1999[Nonius (1999). COLLECT. Nonius BV, Delft, The Netherlands.]); cell refinement: COLLECT; data reduction: EvalCCD (Duisenberg et al., 2003[Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229.]); 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: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WK2075 ).

Acknowledgements

The authors are grateful to Mr Flemming Hansen (Centre of Crystallographic Studies, University of Copenhagen) for collection of the X-ray diffraction data.

References

Brencic, J. V., Ceh, B. & Leban, I. (1987). Z. Anorg. Allg. Chem. 551, 109-115.
Brencic, J. V., Leban, I. & Polanc, I. (1981). Monatsh. Chem. 112, 1359-1368.
Coppens, P. (1970). Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall & C. P. Huber, pp. 255-270. Copenhagen: Munksgaard.
Delavar, M. & Staples, P. J. (1981). J. Chem. Soc. Dalton Trans. pp. 981-985.  [CrossRef]
Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229.  [ISI] [CrossRef] [details]
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  [CrossRef] [details]
Glerup, J., Josephsen, J., Michelsen, K., Pedersen, E. & Schäffer, C. E. (1970). Acta Chem. Scand. 24, 247-254.  [CrossRef] [ChemPort]
Kaizaki, S. & Takemoto, H. (1990). Inorg. Chem. 29, 4960-4964.  [CrossRef] [ChemPort] [ISI]
Kane-Maguire, N. A. P., Wallace, K. C. & Speece, D. G. (1986). Inorg. Chem. 25, 4650-4654.  [CrossRef] [ChemPort]
Nonius (1999). COLLECT. Nonius BV, Delft, The Netherlands.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Yamaguchi-Terasaki, Y., Fujihara, T., Nagasawa, A. & Kaizaki, S. (2007). Acta Cryst. E63, m593-m595.  [CSD] [CrossRef] [details]

Acta Cryst (2008). E64, m369-m370   [ doi:10.1107/S1600536808001153 ]

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.