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Volume 69 
Part 11 
Pages m570-m571  
November 2013  

Received 31 July 2013
Accepted 20 September 2013
Online 2 October 2013

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.006 Å
R = 0.052
wR = 0.094
Data-to-parameter ratio = 13.8
Details
Open access

catena-Poly[2,2',2''-nitrilo­tris­(ethan­aminium) [tri-[mu]-oxido-tris­[dioxido­vanadate(V)]] monohydrate]

aDepartment of Chemistry, Haverford College, 370 Lancaster Avenue, Haverford, PA 19041, USA, and bDepartment of Chemistry, Youngstown State University, 1 University Plaza, Youngstown, OH 44555, USA
Correspondence e-mail: anorquis@haverford.edu

The title compound, {(C6H21N4)[V3O9]·H2O}n, crystallizes as a salt with [trenH3]3+ cations [tren is tris­(2-amino­eth­yl)amine], and one-dimensional anionic {[VVO3]-}n (metavanadate) chains along the c-axis direction. Three crystallographically distinct VV sites and one occluded water mol­ecule are present for every [trenH3]3+ cation in the unit cell. The {[VVO3]-}n chains are composed of vertex-sharing [VO4] tetra­hedra and have a repeat unit of six tetra­hedra. Each tetra­hedron in the chain contains two terminal and two [mu]2-bridging oxide ligands. The [trenH3]3+ cations, {[VVO3]-}n anions and occluded water mol­ecules participate in an extensive three-dimensonal hydrogen-bonding network. The three terminal ammonium sites of the [trenH3]3+ cations each form strong N-H...O hydrogen bonds to terminal oxide ligands on the {[VVO3]-}n chain. Each occluded water mol­ecule also donates two O-H...O hydrogen bonds to the terminal oxide ligands.

Related literature

For properties of organically templated metal oxides, see: Cheetham et al. (1999[Cheetham, A. K., Ferey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3292.]). A host of amine-templated metavanadate chains with connectivities identical to the title compound have been reported previously, for examples, see: Riou & Ferey (1996[Riou, D. & Ferey, G. (1996). J. Solid State Chem. 124, 151-154.]); Roman et al. (1991[Roman, P., Aranzabe, A., Luque, A. & Gutierrez-Zorrilla, J. (1991). Mater. Res. Bull. 26, 19-27.]); Smith et al. (2012[Smith, M. D., Blau, S. M., Chang, K. B., Tran, T. T., Zeller, M., Halasyamani, P. S., Schrier, J. & Norquist, A. J. (2012). J. Solid State Chem. 195, 86-93.]). Metavanadate chains with repeat units of six tetra­hedra are known to exist, see: Lin et al. (2003[Lin, B. Z., Li, Z., Pei, X. K. & Liu, P. D. (2003). J. Mol. Struct. 660, 181-186.]); Tyrselová et al. (1995[Tyrselová, J., Kuchta, L. & Pavelcík, F. (1995). Acta Cryst. C51, 1752-1754.]). For details of the H-atom treatment in the refinement, see: Cooper et al. (2010[Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107.]).

[Scheme 1]

Experimental

Crystal data
  • (C6H21N4)[V3O9]·H2O

  • Mr = 464.09

  • Monoclinic, P 21 /c

  • a = 9.6624 (14) Å

  • b = 10.9179 (15) Å

  • c = 15.768 (2) Å

  • [beta] = 100.565 (2)°

  • V = 1635.2 (4) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.73 mm-1

  • T = 100 K

  • 0.26 × 0.20 × 0.16 mm

Data collection
  • Bruker SMART APEX CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.623, Tmax = 0.746

  • 14279 measured reflections

  • 4719 independent reflections

  • 3195 reflections with I > 2.0[sigma](I)

  • Rint = 0.061

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

  • wR(F2) = 0.094

  • S = 1.00

  • 2860 reflections

  • 208 parameters

  • H-atom parameters not refined

  • [Delta][rho]max = 1.44 e Å-3

  • [Delta][rho]min = -0.68 e Å-3

Table 1
Selected bond lengths (Å)

V1-O1 1.613 (3)
V1-O2 1.651 (3)
V1-O3 1.773 (4)
V1-O4 1.793 (3)
V2-V3 3.2585 (11)
V2-O4 1.793 (3)
V2-O5 1.654 (3)
V2-O6 1.623 (4)
V2-O7 1.778 (3)
V3-O3i 1.769 (4)
V3-O7 1.793 (3)
V3-O8 1.651 (4)
V3-O9 1.632 (3)
Symmetry code: (i) [x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O10-H1...O1i 0.95 2.06 2.997 (6) 170 (1)
O10-H2...O9ii 0.95 1.83 2.739 (6) 160 (1)
N2-H7...O8iii 0.95 1.97 2.864 (6) 155 (1)
N2-H8...O1iii 0.95 2.18 2.951 (6) 138 (1)
N2-H9...O5iv 0.95 1.98 2.850 (6) 152 (1)
C4-H13...O9iii 0.97 2.50 3.447 (6) 167 (1)
N3-H14...O5iv 0.95 2.00 2.912 (6) 162 (1)
N3-H15...O2iv 0.95 1.87 2.819 (6) 176 (1)
N3-H16...O6v 0.95 2.03 2.853 (6) 144 (1)
N3-H16...O10v 0.95 2.23 2.925 (6) 129 (1)
C6-H19...O6v 0.97 2.54 3.222 (6) 127 (1)
N4-H21...O4v 0.95 2.14 3.013 (6) 152 (1)
N4-H22...O2vi 0.95 1.94 2.796 (6) 150 (1)
N4-H23...O5iv 0.95 1.90 2.803 (6) 157 (1)
Symmetry codes: (i) [x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]; (ii) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iii) -x+1, -y+1, -z+1; (iv) x-1, y, z; (v) -x+1, -y+2, -z+1; (vi) [x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2009[Bruker (2009). SAINT and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). SAINT and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS86 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003[Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.]); molecular graphics: CAMERON (Watkin et al., 1996[Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England.]); software used to prepare material for publication: CRYSTALS.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HP2060 ).


Acknowledgements

The authors acknowledge support from the NSF (Award No. CHE-0911121), the Henry Dreyfus Teacher-Scholar Awards Program, and grants to Haverford College from the HHMI Undergraduate Science Education Program. MZ acknowledges support for the purchase of a diffractometer from the NSF Grant 0087210, the Ohio Board of Regents Grant CAP-491, and Youngstown State University.

References

Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.  [Web of Science] [CrossRef] [IUCr Journals]
Bruker (2008). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2009). SAINT and APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Cheetham, A. K., Ferey, G. & Loiseau, T. (1999). Angew. Chem. Int. Ed. 38, 3268-3292.  [Web of Science] [CrossRef] [ChemPort]
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Lin, B. Z., Li, Z., Pei, X. K. & Liu, P. D. (2003). J. Mol. Struct. 660, 181-186.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Riou, D. & Ferey, G. (1996). J. Solid State Chem. 124, 151-154.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Roman, P., Aranzabe, A., Luque, A. & Gutierrez-Zorrilla, J. (1991). Mater. Res. Bull. 26, 19-27.  [CSD] [CrossRef] [ChemPort] [Web of Science]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Smith, M. D., Blau, S. M., Chang, K. B., Tran, T. T., Zeller, M., Halasyamani, P. S., Schrier, J. & Norquist, A. J. (2012). J. Solid State Chem. 195, 86-93.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Tyrselová, J., Kuchta, L. & Pavelcík, F. (1995). Acta Cryst. C51, 1752-1754.  [CSD] [CrossRef] [IUCr Journals]
Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England.


Acta Cryst (2013). E69, m570-m571   [ doi:10.1107/S1600536813026056 ]

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