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Volume 69 
Part 9 
Page m514  
September 2013  

Received 15 August 2013
Accepted 16 August 2013
Online 23 August 2013

Key indicators
Single-crystal Synchrotron study
T = 99 K
Mean [sigma](C-C) = 0.003 Å
R = 0.036
wR = 0.099
Data-to-parameter ratio = 19.9
Details
Open access

trans-Difluoridotetrakis(pyridine-[kappa]N)chromium(III) perchlorate from synchrotron radiation

aPohang Accelerator Laboratory, POSTECH, Pohang 790-784, Republic of Korea, and bDepartment of Chemistry, Andong National University, Andong 760-749, Republic of Korea
Correspondence e-mail: jhchoi@andong.ac.kr

The are two independent complex cations in the title salt, [CrF2(C5H5N)4]ClO4, each located on a centre of inversion, as well as an independent perchlorate counter-ion. The complex cations adopt slightly distorted octahedral coordination environments around the CrIII ion, defined by four pyridine (py) N atoms in the equatorial plane and two F- ligands in the axial positions; intramolecular C-H...F contacts are noted. The mean Cr-N(py) and Cr-F bond lengths are 2.088 (6) and 1.8559 (10) Å, respectively. The three-dimensional architecture is sustained by hydrogen bonds involving the pyridine C-H groups as donors, and F and O atoms as acceptors.

Related literature

For background to geometric isomerism in transition metal comlexes, see: Knight & Scott (2003[Knight, P. D. & Scott, P. (2003). Coord. Chem. Rev. 242, 125-143.]); Ronconi & Sadler (2007[Ronconi, L. & Sadler, P. J. (2007). Coord. Chem. Rev. 251, 1633-1648.]). For the synthesis, see: Glerup et al. (1970[Glerup, J., Josephsen, J., Michelsen, K. E., Pedersen, E. & Schäffer, C. E. (1970). Acta Chem. Scand. 24, 247-254.]). For the structure of trans-[Cr(py)4F2]PF6, see: Fochi et al. (1991[Fochi, G., Stäahle, J. & Ging, F. (1991). Inorg. Chem. 30, 4669-4671.]).

[Scheme 1]

Experimental

Crystal data
  • [CrF2(C5H5N)4]ClO4

  • Mr = 505.85

  • Triclinic, [P \overline 1]

  • a = 9.5690 (19) Å

  • b = 10.615 (2) Å

  • c = 12.663 (3) Å

  • [alpha] = 68.46 (3)°

  • [beta] = 68.31 (3)°

  • [gamma] = 79.38 (3)°

  • V = 1109.9 (5) Å3

  • Z = 2

  • Synchrotron radiation

  • [lambda] = 0.63001 Å

  • [mu] = 0.49 mm-1

  • T = 99 K

  • 0.03 × 0.03 × 0.02 mm

Data collection
  • ADSC Q210 CCD area-detector

  • Absorption correction: empirical (HKL3000sm; Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]) Tmin = 0.985, Tmax = 0.993

  • 11523 measured reflections

  • 5842 independent reflections

  • 4912 reflections with I > 2[sigma](I)

  • Rint = 0.020

Refinement
  • R[F2 > 2[sigma](F2)] = 0.036

  • wR(F2) = 0.099

  • S = 1.05

  • 5842 reflections

  • 293 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.51 e Å-3

  • [Delta][rho]min = -0.61 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C1-H1...F1 0.95 2.36 2.892 (2) 115
C6-H6...F1 0.95 2.31 2.874 (2) 118
C11-H11...F2 0.95 2.32 2.879 (2) 117
C16-H16...F2 0.95 2.39 2.915 (2) 115
C14-H14...O1P 0.95 2.61 3.154 (2) 117
C9-H9...O2P 0.95 2.63 3.320 (3) 130
C1-H1...O3Pi 0.95 2.41 3.107 (2) 130
C4-H4...O1Pii 0.95 2.51 3.368 (2) 150
C5-H5...F1iii 0.95 2.38 2.900 (2) 114
C10-H10...F1iii 0.95 2.31 2.863 (2) 117
C15-H15...F2iv 0.95 2.29 2.856 (2) 117
C20-H20...F2iv 0.95 2.34 2.860 (2) 114
C15-H15...O3Pv 0.95 2.64 3.466 (2) 146
C19-H19...O2Pvi 0.95 2.58 3.227 (3) 125
Symmetry codes: (i) x-1, y+1, z; (ii) x-1, y, z; (iii) -x, -y+2, -z; (iv) -x, -y+2, -z+1; (v) -x+1, -y+1, -z+1; (vi) x, y+1, z.

Data collection: PAL ADSC Quantum-210 ADX Software (Arvai & Nielsen, 1983[Arvai, A. J. & Nielsen, C. (1983). ADSC Quantum-210 ADX. Area Detector System Corporation, Poway, CA, USA.]); cell refinement: HKL3000sm (Otwinowski & Minor, 1997[Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.]); data reduction: HKL3000sm; program(s) used to solve structure: SHELX-2013-XS (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELX-2013-XL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2007[Brandenburg, K. (2007). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK5248 ).


Acknowledgements

This work was supported by a grant from the 2012 Academic Research Fund of Andong National University. The experiment at the PLS-II 2D-SMC beamline was supported in part by MEST and POSTECH.

References

Arvai, A. J. & Nielsen, C. (1983). ADSC Quantum-210 ADX. Area Detector System Corporation, Poway, CA, USA.
Brandenburg, K. (2007). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Fochi, G., Stäahle, J. & Ging, F. (1991). Inorg. Chem. 30, 4669-4671.  [CSD] [CrossRef] [ChemPort] [ISI]
Glerup, J., Josephsen, J., Michelsen, K. E., Pedersen, E. & Schäffer, C. E. (1970). Acta Chem. Scand. 24, 247-254.  [CrossRef] [ChemPort]
Knight, P. D. & Scott, P. (2003). Coord. Chem. Rev. 242, 125-143.  [ISI] [CrossRef] [ChemPort]
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Ronconi, L. & Sadler, P. J. (2007). Coord. Chem. Rev. 251, 1633-1648.  [ISI] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m514  [ doi:10.1107/S1600536813023052 ]

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