Penta­ammonium hepta­sodium bis­[penta­kis(μ2-oxido)deca­oxido­bis­(μ5-phosphato)penta­molybdenum(VI)] henicosa­hydrate

Bih, H.; Bih, L.; Manoun, B.; Azrour, M.; Lazor, P.; El Ammari, L.

doi:10.1107/S160053681000601X

Volume 66
Part 3
Pages i20-i21
March 2010

Received 22 January 2010
Accepted 14 February 2010
Online 20 February 2010

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (P-O) = 0.001 Å
R = 0.022
wR = 0.057
Data-to-parameter ratio = 40.1
Details

Pentaammonium heptasodium bis[pentakis(₂-oxido)decaoxidobis(₅-phosphato)pentamolybdenum(VI)] henicosahydrate

Hssain Bih,^a Lahcen Bih,^b Bouchaid Manoun,^b Mohamed Azrour,^b Peter Lazor ^c and Lahcen El Ammari ^d ^*

^aLaboratoire de Chimie des Matériaux et de l'Environnement, FSTG-Marrakech, Morocco,^bEquipe Sciences des Matériaux, Faculté des Sciences et Techniques, Errachidia, Morocco,^cDepartment of Earth-Geology, Uppsala University, Sweden, and ^dLaboratoire de Chimie du Solide Appliquée, Faculté des Sciences, Université Mohammed V-Agdal, Avenue Ibn Battouta, BP 1014, Rabat, Morocco
Correspondence e-mail: l_elammari@fsr.ac.ma

The title compound, (NH₄)₅Na₇[Mo₅P₂O₂₃]₂·21H₂O, was prepared under atmospheric conditions in aqueous solution at room temperature. The structure contains the [Mo₅P₂O₂₃]^6- heteropolyoxometallate anion, which has been previously reported a number of times with a variety of differing counter-cations. Each anion is built up of five MoO₆ octahedra sharing an edge and forming a ring which is closed by common corners of the terminal octahedra. The rings are closed on both sides by two asymmetric PO₄ tetrahedra, sharing three corners with three MoO₆ octahedra. The anions are chiral and the two independent anions in the asymmetric unit were arbitarily chosen with the same chirality, but the centrosymmetric crystal contains both enantiomers. The structure can alternatively be described as a succession of layers parallel to (101), formed by the [Mo₅P₂O₂₃]^6- anions and linked by sodium chains. Water molecules and ammonium ions fill the remaining space and ensure the cohesion through extensive N-HO and O-HO hydrogen bonding.

Related literature

For ammonium polyoxomolybophosphates, see: Boeyens et al. (1976); Ferrari & Nanni (1939); Ilhan et al. (2007); Andersen & Villadsen (1993); Xu et al.(1998). For background to the heteropolyoxometallate anion, see: Hedman & Strandberg (1979); Long et al. (2007); Pope (1983); Strandberg (1973). For examples of hybrid compounds see: Ma et al. (2006); Wu et al. (2009).

Experimental

Crystal data

(NH₄)₅Na₇[Mo₅P₂O₂₃]₂·21H₂O
M_r = 2448.76
Triclinic, $[P \overline 1]$
a = 9.2299 (3) Å
b = 18.3516 (6) Å
c = 19.7918 (6) Å
= 73.860 (1)°
= 85.323 (3)°
= 75.772 (2)°
V = 3121.17 (17) Å³
Z = 2
Mo K radiation
= 2.23 mm^-1
T = 298 K
0.42 × 0.14 × 0.08 mm

Data collection

Bruker X8 APEXII Diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005) T_min = 0.695, T_max = 0.837
132450 measured reflections
33626 independent reflections
28095 reflections with I > 2(I)
R_int = 0.024

Refinement

R[F² > 2(F²)] = 0.022
wR(F²) = 0.057
S = 1.09
33626 reflections
839 parameters
H-atom parameters constrained
_max = 0.99 e Å^-3
_min = -0.76 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1-H11O12Bⁱ	0.86	2.02	2.8415 (18)	160
N1-H11NO12A	0.87	2.07	2.750 (2)	135
O1-H12O16Aⁱⁱ	0.86	2.55	3.383 (2)	164
N1-H12NO20	0.87	2.13	2.963 (3)	161
N1-H13NO18Bⁱⁱⁱ	0.87	2.37	2.909 (2)	121
N1-H14NO23Bⁱⁱⁱ	0.87	2.29	2.922 (2)	130
O2-H21O21B^iv	0.86	2.29	3.1414 (17)	172
N2-H21NO5Aⁱⁱ	0.87	2.10	2.8892 (19)	151
N2-H21NO13A	0.87	2.59	3.146 (2)	123
O2-H22O20A	0.86	2.07	2.9134 (18)	165
N2-H22NO9A	0.87	2.20	3.036 (2)	162
N2-H23NO1A	0.87	1.98	2.837 (2)	171
N2-H24NO15Aⁱⁱ	0.87	2.06	2.9121 (19)	167
O3-H31O23Aⁱⁱⁱ	0.86	1.86	2.7120 (16)	174
N3-H31NO5B^v	0.87	1.95	2.8066 (19)	170
O3-H32O14Bⁱⁱⁱ	0.86	2.00	2.8440 (16)	165
N3-H32NO9Bⁱⁱⁱ	0.87	2.09	2.9533 (19)	173
N3-H33NO1Bⁱⁱⁱ	0.87	2.04	2.8410 (19)	152
N3-H34NO15B^v	0.87	2.19	3.017 (2)	159
O4-H41O10ⁱⁱ	0.86	1.89	2.743 (2)	172
N4-H41NO1A	0.87	2.00	2.8544 (19)	171
O4-H42O23A	0.86	2.57	3.403 (2)	164
N4-H42NO5Aⁱⁱ	0.87	2.02	2.8757 (19)	169
N4-H43NO12Aⁱⁱⁱ	0.87	2.44	3.123 (2)	136
N4-H43NO22A	0.87	2.26	2.9312 (19)	134
N4-H44NO17Aⁱⁱⁱ	0.87	2.23	2.958 (2)	142
O5-H51O9A	0.86	2.40	3.0367 (18)	132
O5-H51O15B^vi	0.86	2.42	3.201 (2)	151
N5-H51NO1Bⁱⁱⁱ	0.87	2.03	2.8649 (19)	162
O5-H52O2A	0.86	1.97	2.8118 (18)	167
N5-H52NO5B^v	0.87	1.96	2.8251 (17)	175
N5-H53NO13Bⁱⁱⁱ	0.87	2.55	2.9140 (18)	106
N5-H54NO21B^v	0.87	2.45	3.0098 (18)	123
N5-H54NO17Bⁱ	0.87	2.28	3.0203 (19)	144
O6-H61O10A	0.86	2.01	2.8234 (17)	159
O6-H62O20B^iv	0.86	1.84	2.6971 (16)	176
O7-H71O3ⁱⁱⁱ	0.86	1.89	2.7347 (19)	167
O7-H72O6A^vii	0.86	2.09	2.9430 (16)	173
O8-H81O6	0.86	1.87	2.7221 (19)	174
O8-H82O2B^vii	0.86	2.01	2.8642 (16)	171
O9-H91O5A^vii	0.86	1.90	2.7476 (18)	171
O9-H92O13A^vi	0.86	2.34	2.9118 (19)	124
O9-H92O14B^vi	0.86	2.58	3.0630 (18)	117
O1-H01O9B^vii	0.86	2.20	2.985 (2)	152
O10-H102O6A	0.86	2.10	2.893 (2)	153
O11-H111O17A^viii	0.86	2.58	2.987 (2)	110
O11-H112O17A^viii	0.86	2.58	2.987 (2)	110
O11-H112O21A	0.86	2.39	3.126 (2)	143
O12-H121O9^ix	0.86	2.04	2.891 (2)	171
O12-H122O18Aⁱⁱⁱ	0.86	2.01	2.834 (2)	160
O13-H131O19A^ix	0.86	2.13	2.944 (2)	158
O13-H132O2Bⁱⁱⁱ	0.86	2.12	2.904 (2)	151
O14-H141O11	0.86	1.92	2.772 (2)	171
O14-H142O6Bⁱⁱⁱ	0.86	2.17	2.9073 (18)	143
O15-H151O6B^vi	0.86	2.01	2.8578 (17)	169
O15-H152O15B^vi	0.86	2.37	3.0264 (18)	134
O15-H152O9A	0.86	2.43	3.192 (2)	148
O16-H161O13^x	0.86	1.92	2.769 (2)	171
O16-H162O20B^iv	0.86	2.39	3.220 (2)	163
O17-H171O1Bⁱ	0.86	2.44	3.167 (2)	143
O17-H172O16B^iv	0.86	2.18	2.949 (2)	149
O18-H181O1A	0.86	2.35	3.105 (2)	147
O18-H182O11Bⁱ	0.86	2.34	2.874 (2)	121
O19-H191O21	0.86	2.48	3.270 (4)	154
O19-H192O2	0.86	1.99	2.830 (3)	166
O20-H201O21	0.86	1.87	2.716 (3)	166
O20-H202O17Aⁱⁱⁱ	0.86	1.93	2.757 (2)	162
O21-H211O1A	0.86	1.93	2.784 (3)	169
O21-H212O18Bⁱⁱⁱ	0.86	2.44	2.992 (3)	123
Symmetry codes: (i) x, y, z-1; (ii) x-1, y, z; (iii) -x+1, -y+1, -z+1; (iv) x+1, y, z-1; (v) -x, -y+1, -z+1; (vi) -x, -y+2, -z+1; (vii) -x+1, -y+2, -z+1; (viii) -x+2, -y+1, -z+1; (ix) x, y-1, z; (x) -x+1, -y+1, -z.

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FJ2276 ).

Acknowledgements

The authors thank the Unit of Support for Technical and Scientific Research (UATRS, CNRST) for making the present work possible. They also thank H. Zouihri for his helpful technical assistance during the X-ray measurements. The authors are also grateful to the Swedish Research Council and the Swedish International Development Co-operation Agency (Sida) for the financial grant (MENA) offered in support of this work.

References

Andersen, E. K. & Villadsen, J. (1993). Acta Chem. Scand. 47, 748-752.
Boeyens, J. C. A., McDougal, G. J. & van Smit, J. (1976). J. Solid State Chem. 18, 191-199.
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Ferrari, A. & Nanni, O. (1939). Gazz. Chim. Ital. 69, 301-303.
Hedman, B. & Strandberg, R. (1979). Acta Cryst. B35, 278-284.
Ilhan, S., Kahruman, C. & Yusufoglu, I. (2007). J. Anal. Appl. Pyrolysis, 78, 363-370.
Long, D. L., Burkholder, E. & Cronin, L. (2007). Chem. Soc. Rev. 36, 105-121.
Ma, Y., Lu, Y., Wang, E., Xu, X., Guo, Y., Bai, X. & Xu, L. (2006). J. Mol. Struct. 784, 18-23.
Pope, M. T. (1983). Heteropoly and Isopoly Oxometalates. New York: Springer.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Strandberg, R. (1973). Acta Chem. Scand. 3 1004-1017
Wu, L., Ma, H., Han, Z. & Li, C. (2009). Solid State Sci. 11, 43-48
Xu, Y., Xu, J.-Q., Yang, G.-Y., Yang, G.-D., Xing, Y., Lin, Y.-H. & Jia, H.-Q. (1998). Acta Cryst. C54, 9-11.