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Volume 69 
Part 7 
Pages m376-m377  
July 2013  

Received 31 May 2013
Accepted 4 June 2013
Online 12 June 2013

Key indicators
Single-crystal Synchrotron study
T = 98 K
Mean [sigma](C-C) = 0.002 Å
R = 0.030
wR = 0.085
Data-to-parameter ratio = 20.2
Details
Open access

cis-(1,4,8,11-Tetraazacyclotetradecane-[kappa]N4)bis(thiocyanato-[kappa]N)chromium(III) thiocyanate

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 crystal structure of [Cr(NCS)2(cyclam)]NCS (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4) has been determined by using synchrotron radiation at 98 K. The CrIII atom is in a slightly distorted octahedral environment with four N atoms of the macrocyclic ligand and two N-coordinated NCS- anions in cis positions. The average Cr-N(cyclam) and Cr-NCS bond lengths are 2.085 (5) and 1.996 (15) Å, respectively. In the crystal, the uncoordinating SCN- anion is hydrogen bonded through N-H...S and N-H...N interactions to neighbouring complex cations.

Related literature

For the synthesis, see: Ferguson & Tobe (1970[Ferguson, J. & Tobe, M. L. (1970). Inorg. Chim. Acta 4, 109-112.]); For spectroscopic studies, see: Choi & Park (2003[Choi, J. H. & Park, Y. U. (2003). Bull. Korean Chem. Soc. 24, 384-388.]); Poon & Pun (1980[Poon, C. K. & Pun, K. C. (1980). Inorg. Chem. 19, 568-569.]). For related structures, see: Forsellini et al. (1986[Forsellini, E., Parasassi, T., Bombieri, G., Tobe, M. L. & Sosa, M. E. (1986). Acta Cryst. C42, 563-565.]); Friesen et al. (1997[Friesen, D. A., Quail, J. W., Waltz, W. L. & Nashiem, R. E. (1997). Acta Cryst. C53, 687-691.]); Meyer et al. (1998[Meyer, K., Bendix, J., Bill, E., Weyhermüller, T. & Weighardt, K. (1998). Inorg. Chem. 37, 5180-5188.]); Choi et al. (2004a[Choi, J.-H., Oh, I.-G., Lim, W.-T. & Park, K.-M. (2004a). Acta Cryst. C60, m238-m240.],b[Choi, J. H., Oh, I. G., Suzuki, T. & Kaizaki, S. (2004b). J. Mol. Struct. 694, 39-44.], 2009[Choi, J. H. (2009). Inorg. Chim. Acta, 362, 4231-4236.]); Subhan et al. (2011[Subhan, M. A., Choi, J. H. & Ng, S. W. (2011). Z. Anorg. Allg. Chem. 637, 2193-2197.]).

[Scheme 1]

Experimental

Crystal data
  • [Cr(NCS)2(C10H24N4)]NCS

  • Mr = 426.57

  • Monoclinic, P 21 /c

  • a = 10.590 (2) Å

  • b = 7.6970 (15) Å

  • c = 23.750 (5) Å

  • [beta] = 94.70 (3)°

  • V = 1929.4 (7) Å3

  • Z = 4

  • Synchrotron radiation

  • [lambda] = 0.740 Å

  • [mu] = 1.03 mm-1

  • T = 98 K

  • 0.01 × 0.01 × 0.01 mm

Data collection
  • ADSC Q210 CCD area-detector diffractometer

  • Absorption correction: empirical (HKL-3000 SCALEPACK; 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 = 0.988, Tmax = 0.989

  • 16587 measured reflections

  • 4727 independent reflections

  • 3998 reflections with I > 2[sigma](I)

  • Rint = 0.038

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.085

  • S = 1.07

  • 4727 reflections

  • 234 parameters

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

  • [Delta][rho]max = 0.38 e Å-3

  • [Delta][rho]min = -0.46 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1N1...S2i 0.86 (2) 2.59 (2) 3.4138 (15) 160.1 (17)
N2-H1N2...S4ii 0.77 (2) 2.66 (2) 3.3521 (14) 149.8 (18)
N3-H1N3...N7ii 0.834 (19) 2.119 (19) 2.9238 (19) 162.0 (17)
N4-H1N4...N7iii 0.851 (19) 2.150 (19) 2.947 (2) 155.9 (17)
Symmetry codes: (i) [-x+2, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iii) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: ADSC Quantum-210 ADX (Arvai & Nielsen, 1983[Arvai, A. J. & Nielsen, C. (1983). ADSC Quantum-210 ADX. Area Detector System Corporation, Poway, CA, USA.]); cell refinement: HKL-3000 (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: HKL-3000; program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008)[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]; program(s) used to refine structure: SHELXL2013 (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: LR2107 ).


Acknowledgements

The research was supported by a grant from the 2012 International Academic Exchange Program of Andong National University. The experiment at 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.
Choi, J. H. (2009). Inorg. Chim. Acta, 362, 4231-4236.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Choi, J.-H., Oh, I.-G., Lim, W.-T. & Park, K.-M. (2004a). Acta Cryst. C60, m238-m240.  [CSD] [CrossRef] [IUCr Journals]
Choi, J. H., Oh, I. G., Suzuki, T. & Kaizaki, S. (2004b). J. Mol. Struct. 694, 39-44.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Choi, J. H. & Park, Y. U. (2003). Bull. Korean Chem. Soc. 24, 384-388.  [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Ferguson, J. & Tobe, M. L. (1970). Inorg. Chim. Acta 4, 109-112.  [CrossRef] [ChemPort]
Forsellini, E., Parasassi, T., Bombieri, G., Tobe, M. L. & Sosa, M. E. (1986). Acta Cryst. C42, 563-565.  [CrossRef] [IUCr Journals]
Friesen, D. A., Quail, J. W., Waltz, W. L. & Nashiem, R. E. (1997). Acta Cryst. C53, 687-691.  [CSD] [CrossRef] [IUCr Journals]
Meyer, K., Bendix, J., Bill, E., Weyhermüller, T. & Weighardt, K. (1998). Inorg. Chem. 37, 5180-5188.  [Web of Science] [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.
Poon, C. K. & Pun, K. C. (1980). Inorg. Chem. 19, 568-569.  [CrossRef] [ChemPort] [Web of Science]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Subhan, M. A., Choi, J. H. & Ng, S. W. (2011). Z. Anorg. Allg. Chem. 637, 2193-2197.  [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m376-m377   [ doi:10.1107/S1600536813015456 ]

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