Trisodium bis­{1-[iminio­(morpholino)meth­yl]guanidinium} bis­[hexa­hydrogen­hexa­molybdoaluminate(III)] chloride icosa­hydrate

Wang, F.; Cao, R.-G.; Pan, Y.-B.; Liu, S.-X.

doi:10.1107/S1600536808022745

Volume 64
Part 8
Pages m1069-m1070
August 2008

Received 17 June 2008
Accepted 19 July 2008
Online 26 July 2008

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.009 Å
Disorder in main residue
R = 0.035
wR = 0.093
Data-to-parameter ratio = 13.7
Details

Trisodium bis{1-[iminio(morpholino)methyl]guanidinium} bis[hexahydrogenhexamolybdoaluminate(III)] chloride icosahydrate

Feng Wang,^a Rui-Ge Cao,^a Yi-Bing Pan ^a and Shu-Xia Liu ^a ^*

^aKey Laboratory of Polyoxometalates Science of the Ministry of Education, College of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China
Correspondence e-mail: liusx@nenu.edu.cn

In the title compound, Na₃(C₆H₁₅N₅O)₂[Al(OH)₆Mo₆O₁₈]₂Cl·20H₂O, the [Al(OH)₆Mo₆O₁₈]^3- polyoxoanion has a B-type Anderson structure exhibiting approximate D_3d symmetry. There are two types of sodium cations: the Na⁺ cations of type I have a distorted octahedral coordination geometry formed by six O atoms and are statistically distributed over two positions with equal occupancies, while the coordination polyhedra of the two Na⁺ cations of type II share one Cl anion located on an inversion center. The latter fragment, containing a Cl anion and two sodium cations, links two polyoxoanions into centrosymmetric blocks. The diprotonated 1-[imino(morpholino)methyl]guanidinium cations and uncordinated water molecules contribute to extensive N-HO and O-HO hydrogen bonding, resulting in the formation a three-dimensional supramolecular structure.

Related literature

For related literature, see: Cao et al. (2007); Cheng et al. (2007); Lee et al. (1991); Li et al. (2005); Pope (1983); Shivaiah et al. (2003); Wang et al. (2007). For general background, see: Brown & Altermatt (1985).

Experimental

Crystal data

Na₃(C₆H₁₅N₅O)₂[Al(OH)₆Mo₆O₁₈]₂Cl·20H₂O
M_r = 2796.54
Triclinic, $[P \overline 1]$
a = 10.1070 (6) Å
b = 11.3869 (7) Å
c = 17.2548 (10) Å
= 81.6980 (10)°
= 75.3140 (10)°
= 77.0570 (10)°
V = 1864.03 (19) Å³
Z = 1
Mo K radiation
= 2.15 mm^-1
T = 296 (2) K
0.31 × 0.25 × 0.22 mm

Data collection

Bruker SMART diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1997) T_min = 0.528, T_max = 0.624
9902 measured reflections
6882 independent reflections
6108 reflections with I > 2(I)
R_int = 0.021

Refinement

R[F² > 2(F²)] = 0.034
wR(F²) = 0.092
S = 1.06
6882 reflections
503 parameters
H-atom parameters constrained
_max = 1.36 e Å^-3
_min = -1.29 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2O8ⁱ	0.90	2.00	2.855 (5)	158
N3-H3O7ⁱⁱ	0.90	1.86	2.750 (5)	173
N5-H6O9ⁱⁱⁱ	0.90	1.92	2.821 (5)	179
O1-H8O31	0.85	1.79	2.631 (5)	170
O3-H10O32	0.85	1.87	2.715 (5)	169
O4-H11O27^iv	0.85	1.90	2.736 (4)	170
O5-H12O30^v	0.85	1.94	2.769 (5)	164
O6-H13O28^iv	0.85	1.91	2.737 (4)	164
O26-H14O19^vi	0.85	2.11	2.919 (5)	159
O26-H15O35^vii	0.85	2.13	2.898 (5)	150
O27-H16O34^vii	0.85	2.12	2.918 (5)	155
O27-H17O35^viii	0.85	1.95	2.784 (5)	169
O28-H18O17^vii	0.85	2.04	2.845 (5)	158
O28-H19O16^vii	0.85	1.98	2.790 (5)	160
O29-H20O20^vi	0.85	2.08	2.853 (5)	152
O29-H21O12^v	0.84	1.90	2.735 (5)	168
O30-H22O21^vi	0.85	2.11	2.890 (5)	152
O30-H23O33^v	0.85	1.93	2.640 (7)	141
O31-H24O32	0.86	2.09	2.889 (7)	154
O31-H25O29	0.86	2.08	2.885 (6)	155
O32-H26O33	0.85	2.00	2.632 (8)	130
O32-H27O23^ix	0.85	2.03	2.843 (6)	160
O33-H29O10	0.85	1.96	2.812 (6)	176
O34-H30O14ⁱⁱ	0.85	2.14	2.991 (5)	175
O34-H31O11^ix	0.85	1.94	2.756 (5)	161
O35-H32O34	0.85	2.03	2.768 (5)	145
O35-H33O18	0.85	2.14	2.927 (5)	155
Symmetry codes: (i) x, y+1, z; (ii) x-1, y+1, z; (iii) -x+1, -y+1, -z+1; (iv) -x+2, -y, -z+1; (v) -x+2, -y, -z; (vi) x, y-1, z; (vii) -x+1, -y, -z+1; (viii) x+1, y-1, z; (ix) x-1, y, z.

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); 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 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CV2425 ).

Acknowledgements

This work was supported by the National Science Foundation of China (grant No. 20571014), the Program for New Century Excellent Talents in Universities (NCET-07-0169), and the Analysis and Testing Foundation of Northeast Normal University.

References

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