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Volume 69 
Part 8 
Pages m469-m470  
August 2013  

Received 24 June 2013
Accepted 16 July 2013
Online 24 July 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](N-C) = 0.009 Å
Disorder in main residue
R = 0.052
wR = 0.175
Data-to-parameter ratio = 10.2
Details
Open access

Diammonium tetrakis(isothiocyanato)zincate-1,4,10,13,16-hexaoxacyclooctadecane-water (1/2/1)

aResearch and Development Centre, Bharathiyar University, Coimbatore 641 046, India,bDepartment of Physics, Rajeswari Vedachalam Government Arts College, Chengalpet 603 001, India, and cDepartment of Physics, The New College (Autonomous), Chennai 600 014, India
Correspondence e-mail: drkrr2007@gmail.com, mnizam_new@yahoo.in

The title compound, (NH4)2[Zn(NCS)4]·2C12H24O6·H2O, the result of the reaction of ammonium thiocyanate, 18-crown-6 and zinc(II) chloride in aqueous solution, exhibits an unusual supramolecular structure. The Zn atom, two of the thiocyanate chains and a water molecule, disordered over two positions, lie on a mirror plane. The macrocycle adopts a conformation with approximate D3d symmetry. The ammonium molecules are contained within the bowl of the macrocycle via extensive N-H...O hydrogen bonds and the complex molecules are linked via N-H...S hydrogen bonds, forming chains along the c-axis direction. The macrocycle is disordered over two positions [refined occupancy ratio = 0.666 (8):0.334 (8)]. The S atoms of two isothiocyanate ligands are disordered within and about the mirror plane.

Related literature

For background to crown ether/ammonium ion complexes, see: Fender et al. (2002[Fender, N. S., Kahwa, I. A. & Fronczek, F. R. (2002). J. Solid State Chem. 163, 286-293.]); Kryatova et al. (2004[Kryatova, O. P., Korendovych, I. V. & Rybak-Akimova, E. V. (2004). Tetrahedron, 60, 4579-4588.]); Akutagawa et al. (2002[Akutagawa, T., Hashimoto, A., Nishihara, S., Hasegawa, T. & Nakamura, T. (2002). J. Supramol. Chem. 2, 175-186.]); Ramesh et al. (2012[Ramesh, V., Rajarajan, K., Kumar, K. S., Subashini, A. & NizamMohideen, M. (2012). Acta Cryst. E68, m335-m336.]).

[Scheme 1]

Experimental

Crystal data
  • (NH4)2[Zn(NCS)4]·2C12H24O6·H2O

  • Mr = 880.41

  • Orthorhombic, P n m a

  • a = 22.7875 (12) Å

  • b = 23.6254 (12) Å

  • c = 8.5593 (5) Å

  • V = 4608.0 (4) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.77 mm-1

  • T = 293 K

  • 0.30 × 0.25 × 0.20 mm

Data collection
  • Bruker Kappa APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004[Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.]) Tmin = 0.802, Tmax = 0.861

  • 24101 measured reflections

  • 4641 independent reflections

  • 2467 reflections with I > 2[sigma](I)

  • Rint = 0.058

Refinement
  • R[F2 > 2[sigma](F2)] = 0.052

  • wR(F2) = 0.175

  • S = 1.00

  • 4641 reflections

  • 454 parameters

  • 276 restraints

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

  • [Delta][rho]max = 0.72 e Å-3

  • [Delta][rho]min = -0.24 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N4-H4H...O1 0.88 (1) 2.44 (4) 3.069 (8) 129 (4)
N4-H4E...O2 0.87 (1) 2.06 (1) 2.934 (8) 176 (5)
N4-H4G...O4 0.88 (1) 1.97 (2) 2.829 (7) 166 (4)
N4-H4G...O5 0.88 (1) 2.53 (4) 3.010 (8) 115 (3)
N4-H4H...O6 0.88 (1) 2.05 (3) 2.850 (8) 150 (5)
N4-H4F...S1i 0.87 (1) 2.63 (2) 3.441 (4) 156 (4)
Symmetry code: (i) x, y, z-1.

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: APEX2 and SAINT (Bruker, 2004[Bruker (2004). APEX2, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT and XPREP (Bruker, 2004[Bruker (2004). APEX2, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); 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 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and Mercury (Macrae et al., 2008[Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2617 ).


Acknowledgements

The authors are thankful to the SAIF, IIT Madras, for the data collection. KR thanks the University Grants Commission, Government of India, for financial support granted under a Major Research Project [F. No.41-1008/2012 (SR)].

References

Akutagawa, T., Hashimoto, A., Nishihara, S., Hasegawa, T. & Nakamura, T. (2002). J. Supramol. Chem. 2, 175-186.  [CSD] [CrossRef] [ChemPort]
Bruker (2004). APEX2, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Fender, N. S., Kahwa, I. A. & Fronczek, F. R. (2002). J. Solid State Chem. 163, 286-293.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Kryatova, O. P., Korendovych, I. V. & Rybak-Akimova, E. V. (2004). Tetrahedron, 60, 4579-4588.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Ramesh, V., Rajarajan, K., Kumar, K. S., Subashini, A. & NizamMohideen, M. (2012). Acta Cryst. E68, m335-m336.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Spek, A. L. (2009). Acta Cryst. D65, 148-155.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m469-m470   [ doi:10.1107/S1600536813019739 ]

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