nitrate acetic acid solvate

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O(H2O)3]NO3БCH3CO2H, the trinuclear [Cr3(CH3CO2)6O-. (H2O)3] cluster .... О:О 3 oxido tris aquachromium(III)] nitrate acetic acid solvate. M. J. Maah, С. I.
electronic reprint Acta Crystallographica Section E

Structure Reports Online ISSN 1600-5368

Editors: W.T. A. Harrison, J. Simpson and M. Weil

Hexa-µ2-acetato-κ12O :O -µ3-oxido-tris[aquachromium(III)] nitrate acetic acid solvate Mohd Jamil Maah, Che Ibrahim Abdullah, Seng Neon Gan, Aishah Mohd Jelan and Seik Weng Ng

Acta Cryst. (2008). E64, m1310

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ISSN 1600-5368

Volume 61 Part 11 November 2005

Acta Crystallographica Section E

Structure Reports Online Editors: W. Clegg and D. G. Watson

Inorganic compounds

Metal-organic compounds

Organic compounds

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Crystallography Journals Online is available from journals.iucr.org Acta Cryst. (2008). E64, m1310

Maah et al. · [Cr3 (C2 H3 O2 )6 O(H2 O)3 ]NO3 ·C2 H4 O2

metal-organic compounds ˚ c = 15.0427 (2) A  = 91.532 (1) ˚3 V = 2553.62 (5) A Z=4

Acta Crystallographica Section E

Structure Reports Online

Mo K radiation  = 1.35 mm1 T = 100 (2) K 0.20  0.10  0.05 mm

ISSN 1600-5368

Data collection

Hexa-l2-acetato-j12O:O0 -l3-oxido-tris[aquachromium(III)] nitrate acetic acid solvate

Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996) Tmin = 0.774, Tmax = 0.936

22819 measured reflections 5836 independent reflections 5092 reflections with I > 2(I) Rint = 0.046

Refinement

Mohd Jamil Maah,a* Che Ibrahim Abdullah,a Seng Neon Gan,a Aishah Mohd Jelanb and Seik Weng Nga a

Department of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and bCentre for Foundation Studies in Science, University of Malaya, 50603 Kuala Lumpur, Malaysia Correspondence e-mail: [email protected] Received 15 September 2008; accepted 16 September 2008 ˚; Key indicators: single-crystal X-ray study; T = 100 K; mean (C–C) = 0.008 A R factor = 0.068; wR factor = 0.225; data-to-parameter ratio = 16.3.

In the crystal structure of the title salt, [Cr3(C2H3O2)6O(H2O)3]NO3CH3CO2H, the trinuclear [Cr3(CH3CO2)6O(H2O)3] cluster cation has an oxide O atom that is connected to three water-coordinated CrIII atoms, the three metal atoms forming the points of an equilateral triangle. Each of the six acetate carboxylate groups bridges a Cr–O–Cr fragment. The cluster cation interacts with the nitrate counter-ion and solvent molecules through O—H  O hydrogen bonds, forming a three-dimensional hydrogen-bonded network.

R[F 2 > 2(F 2)] = 0.067 wR(F 2) = 0.224 S = 1.38 5836 reflections

359 parameters H-atom parameters constrained ˚ 3 max = 1.77 e A ˚ 3 min = 1.33 e A

Table 1

˚ ,  ). Hydrogen-bond geometry (A D—H  A

D—H

H  A

D  A

D—H  A

O1w—H11  O16 O1w—H12  O12i O2w—H21  O14 O2w—H22  O18ii O3w—H31  O14iii O3w—H32  O5iii O15—H15  O18iv

0.84 0.84 0.84 0.84 0.84 0.84 0.84

1.96 2.06 1.92 1.93 2.28 2.42 1.81

2.769 2.873 2.668 2.725 2.781 3.244 2.624

162 162 147 157 118 165 163

Symmetry codes: (i) x þ 1; y þ 1; z þ 1; x; y þ 32; z  12; (iv) x  1; y þ 32; z þ 12.

(ii)

(6) (5) (6) (6) (5) (6) (6)

x þ 1; y  12; z þ 32;

(iii)

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XSEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2008).

Related literature For crystal structure reports of [Cr3(C2H3O2)6O(H2O)3]+ salts, see: Anson et al. (1997); Fujihara et al. (1998); Glowiak et al. (1996); Karu et al. (1993); Winpenny et al. (2005).

We thank the University of Malaya (JPJ Vote) for supporting this sudy. Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK2306).

References

Experimental Crystal data [Cr3(C2H3O2)6O(H2O)3]NO3C2H4O2 Mr = 702.37

m1310

Maah et al.

Monoclinic, P21 =c ˚ a = 11.7034 (1) A ˚ b = 14.5102 (2) A

Anson, C. E., Bourke, J. P., Cannon, R. D., Jayasooriya, U. A., Molinier, M. & Powell, A. K. (1997). Inorg. Chem. 36, 1265–1267. Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Fujihara, T., Aonahata, J., Kumakura, S., Nagasawa, A., Murakami, K. & Ito, T. (1998). Inorg. Chem. 37, 3779–3784. Glowiak, T., Kozlowski, H., Erre, L. S. & Micera, G. (1996). Inorg. Chim. Acta, 248, 99–102. Karu, E., Anson, C. E., Cannon, R. D., Jayasooriya, U. A. & Powell, A. K. (1993). Acta Cryst. C49, 1929–1932. Sheldrick, G. M. (1996). SADABS. University of Go¨ttingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Westrip, S. P. (2008). publCIF. In preparation. Winpenny, R., Smith, A., Parkin, A., Parsons, S. & Messenger, D. (2005). Private communication (deposition No. 278285). CCDC, Cambridge, England.

doi:10.1107/S1600536808029681

electronic reprint

Acta Cryst. (2008). E64, m1310

 

 

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