(IUCr) Hexaaquagallium(III) trinitrate trihydrate

Volume 65
Part 8
Page i65
August 2009

Received 9 July 2009
Accepted 16 July 2009
Online 22 July 2009

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (O-N) = 0.002 Å
R = 0.021
wR = 0.058
Data-to-parameter ratio = 11.1
Details

Hexaaquagallium(III) trinitrate trihydrate

Arthur D. Hendsbee,^a Cory C. Pye ^a and Jason D. Masuda ^a ^*

^aDepartment of Chemistry, Saint Mary's University, Halifax, Nova Scotia, Canada B3H 3C3
Correspondence e-mail: jason.masuda@smu.ca

The title compound, [Ga(H₂O)₆](NO₃)₃·3H₂O, is isostructural to other known M^III nitrate hydrates (M = Al, Cr, Fe). The structure contains two distinct octahedral Ga(OH₂)₆ units (each of $[\overline{1}]$ symmetry) which are involved in intermolecular hydrogen bonding with the three nitrate anions and three water molecules within the asymmetric unit.

Related literature

For the the aluminium analogue, see: Lazar, Ribár, Divjakovic & Mészáros (1991). For the chromium analogue, see: Lazar, Ribár & Prelesnik (1991). For the iron analogue, see: Hair & Beattie (1977). For ionic radii, see: Shannon & Prewitt (1969). Gallium nitrate, used in the preparation, easily forms supersaturated solutions, see: Rudolph et al. (2002), and hence the sample was cooled to 248 K and a seed crystal was introduced to initiate crystallization.

Experimental

Crystal data

[Ga(H₂O)₆](NO₃)₃·3H₂O
M_r = 417.89
Monoclinic, P 2₁ /c
a = 13.9609 (6) Å
b = 9.6498 (5) Å
c = 10.9743 (5) Å
= 95.448 (1)°
V = 1471.78 (12) Å³
Z = 4
Mo K radiation
= 1.97 mm^-1
T = 296 K
0.40 × 0.34 × 0.29 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008) T_min = 0.479, T_max = 0.564
10587 measured reflections
3037 independent reflections
2509 reflections with I > 2(I)
R_int = 0.015

Refinement

R[F² > 2(F²)] = 0.021
wR(F²) = 0.058
S = 1.05
3037 reflections
274 parameters
18 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.48 e Å^-3
_min = -0.33 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O18-H18O8	0.801 (16)	2.26 (2)	2.9348 (18)	142 (2)
O16-H14O18	0.825 (15)	2.072 (15)	2.8732 (19)	163.8 (19)
O5-H10O7	0.823 (16)	1.908 (17)	2.7052 (17)	163 (2)
O1-H1O16	0.814 (15)	1.846 (16)	2.6474 (16)	168 (2)
O4-H7O14	0.809 (15)	1.833 (15)	2.6399 (15)	175 (2)
O5-H9O17	0.810 (16)	1.869 (16)	2.676 (2)	174 (2)
O18-H17O14	0.816 (16)	2.082 (17)	2.8729 (18)	163 (2)
O3-H6O15ⁱ	0.814 (15)	1.903 (16)	2.7150 (16)	175 (2)
O1-H2O10ⁱ	0.808 (15)	1.848 (16)	2.6545 (16)	175 (2)
O2-H4O16ⁱ	0.790 (16)	1.901 (16)	2.6895 (18)	175 (2)
O4-H8O17ⁱⁱ	0.821 (15)	1.816 (15)	2.6312 (16)	171 (2)
O17-H15O9ⁱⁱ	0.808 (15)	1.977 (16)	2.7791 (19)	171 (2)
O3-H5O13ⁱⁱⁱ	0.792 (15)	1.961 (16)	2.7454 (16)	171 (2)
O6-H12O12^iv	0.796 (15)	1.926 (16)	2.7179 (16)	174 (2)
O16-H13O18^v	0.820 (16)	1.934 (16)	2.7525 (19)	177 (3)
O6-H11O11^vi	0.800 (15)	1.895 (16)	2.6938 (17)	176 (2)
O2-H3O8^vii	0.794 (15)	1.943 (16)	2.7269 (17)	169 (2)
O17-H16O7^viii	0.802 (16)	2.026 (18)	2.7675 (18)	154 (2)
Symmetry codes: (i) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (ii) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) x, y, z-1; (iv) $[x-1, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (v) -x+1, -y, -z+1; (vi) x-1, y, z; (vii) -x+1, -y, -z; (viii) $[-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); 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); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: MG2076 ).

Acknowledgements

The authors thank Saint Mary's University, the Saint Mary's University Student Employment Experience Program (ADH) and the Natural Sciences and Engineering Research Council (CCP) for financial support.

References

Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Hair, N. J. & Beattie, J. K. (1977). Inorg. Chem. 16, 245-250.
Lazar, D., Ribár, B., Divjakovic, V. & Mészáros, Cs. (1991). Acta Cryst. C47, 1060-1062.
Lazar, D., Ribár, B. & Prelesnik, B. (1991). Acta Cryst. C47, 2282-2285.
Rudolph, W. W., Pye, C. C. & Irmer, G. (2002). J. Raman Spectrosc. 33, 177-190.
Shannon, R. D. & Prewitt, C. T. (1969). Acta Cryst. B25, 925-946.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

inorganic compounds