Hexaaqua-gallium(III) trinitrate trihydrate.

The title compound, [Ga(H(2)O)(6)](NO(3))(3)·3H(2)O, is isostructural to other known M(III) nitrate hydrates (M = Al, Cr, Fe). The structure contains two distinct octa-hedral Ga(OH(2))(6) units (each of symmetry) which are involved in inter-molecular hydrogen bonding with the three nitrate anions and three water mol-ecules within the asymmetric unit.

Related literature

For the the aluminium analogue, see: Lazar, Ribár, Divjaković & 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 = 417.89

Monoclinic,

a = 13.9609 (6) Å

b = 9.6498 (5) Å

c = 10.9743 (5) Å

β = 95.448 (1)°

V = 1471.78 (12) Å3

Z = 4

Mo Kα radiation

μ = 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 > 2σ(I)

R int = 0.015

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.058

S = 1.05

3037 reflections

274 parameters

18 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.48 e Å−3

Δρmin = −0.33 e Å−3

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 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809028086/mg2076sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809028086/mg2076Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ga(H2O)6](NO3)3·3H2O	F(000) = 856
Mr = 417.89	Dx = 1.886 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5403 reflections
a = 13.9609 (6) Å	θ = 2.3–28.3°
b = 9.6498 (5) Å	µ = 1.97 mm−1
c = 10.9743 (5) Å	T = 296 K
β = 95.448 (1)°	Irregular, colourless
V = 1471.78 (12) Å3	0.40 × 0.34 × 0.29 mm
Z = 4

Bruker APEXII CCD diffractometer	3037 independent reflections
Radiation source: fine-focus sealed tube	2509 reflections with I > 2σ(I)
graphite	Rint = 0.015
φ and ω scans	θmax = 26.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −17→17
Tmin = 0.479, Tmax = 0.564	k = −12→10
10587 measured reflections	l = −13→13

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0301P)2 + 0.4119P] where P = (Fo2 + 2Fc2)/3
3037 reflections	(Δ/σ)max < 0.001
274 parameters	Δρmax = 0.48 e Å−3
18 restraints	Δρmin = −0.33 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
Ga1	0.5000	0.0000	0.0000	0.01867 (8)
Ga2	0.0000	0.0000	0.5000	0.02131 (8)
N1	0.19260 (10)	0.00919 (13)	0.12573 (13)	0.0285 (3)
N2	0.29851 (9)	0.18907 (14)	0.70878 (11)	0.0268 (3)
N3	0.78610 (9)	0.28563 (14)	0.71869 (11)	0.0293 (3)
O1	0.57018 (8)	0.08802 (13)	0.13967 (10)	0.0306 (3)
H2	0.6187 (12)	0.132 (2)	0.1335 (19)	0.051 (6)*
H1	0.5546 (14)	0.088 (2)	0.2093 (15)	0.051 (6)*
O2	0.57327 (8)	0.10539 (13)	−0.11126 (10)	0.0294 (2)
H4	0.5629 (16)	0.1854 (17)	−0.121 (2)	0.053 (7)*
H3	0.6243 (12)	0.082 (2)	−0.1307 (18)	0.054 (6)*
O3	0.40601 (8)	0.14903 (12)	−0.00574 (10)	0.0269 (2)
H6	0.3964 (15)	0.190 (2)	0.0569 (16)	0.051 (6)*
H5	0.3607 (13)	0.150 (2)	−0.0550 (17)	0.051 (6)*
O4	0.07132 (8)	0.09427 (14)	0.63446 (10)	0.0327 (3)
H8	0.0636 (14)	0.093 (2)	0.7077 (14)	0.043 (5)*
H7	0.1244 (12)	0.121 (2)	0.6219 (19)	0.051 (6)*
O5	0.07408 (9)	0.10908 (14)	0.39031 (10)	0.0339 (3)
H10	0.0971 (15)	0.084 (2)	0.3275 (17)	0.065 (7)*
H9	0.0633 (16)	0.1911 (17)	0.381 (2)	0.054 (7)*
O6	−0.09607 (8)	0.14720 (14)	0.49563 (11)	0.0358 (3)
H12	−0.1406 (13)	0.147 (2)	0.4446 (18)	0.054 (7)*
H11	−0.1078 (16)	0.183 (2)	0.5582 (17)	0.055 (7)*
O7	0.11323 (8)	0.04401 (15)	0.16045 (11)	0.0439 (3)
O8	0.26475 (9)	−0.00369 (13)	0.19969 (12)	0.0430 (3)
O9	0.19968 (11)	−0.01084 (15)	0.01616 (12)	0.0529 (4)
O10	0.72635 (8)	0.25702 (13)	0.62972 (10)	0.0369 (3)
O11	0.87278 (8)	0.26164 (15)	0.71226 (11)	0.0473 (3)
O12	0.75836 (8)	0.33667 (15)	0.81328 (10)	0.0424 (3)
O13	0.26276 (8)	0.16544 (14)	0.80530 (10)	0.0395 (3)
O14	0.24653 (7)	0.18488 (13)	0.60783 (9)	0.0339 (3)
O15	0.38523 (7)	0.21721 (14)	0.70780 (10)	0.0400 (3)
O16	0.53516 (9)	0.12179 (13)	0.37069 (11)	0.0333 (3)
H14	0.4793 (11)	0.108 (2)	0.3864 (17)	0.043 (6)*
H13	0.5662 (15)	0.076 (2)	0.4232 (18)	0.063 (7)*
O17	0.05170 (9)	0.38374 (14)	0.36978 (11)	0.0362 (3)
H15	0.0906 (14)	0.427 (2)	0.4140 (19)	0.057 (7)*
H16	0.0021 (13)	0.420 (2)	0.383 (2)	0.056 (7)*
O18	0.35675 (10)	0.02473 (15)	0.45021 (13)	0.0410 (3)
H17	0.3188 (14)	0.075 (2)	0.482 (2)	0.064 (8)*
H18	0.3232 (17)	−0.016 (2)	0.399 (2)	0.062 (8)*

	U11	U22	U33	U12	U13	U23
Ga1	0.01679 (12)	0.02124 (13)	0.01796 (12)	0.00073 (8)	0.00156 (8)	−0.00138 (8)
Ga2	0.01777 (12)	0.02999 (15)	0.01606 (12)	−0.00007 (8)	0.00097 (8)	−0.00210 (8)
N1	0.0297 (7)	0.0278 (8)	0.0280 (7)	−0.0019 (5)	0.0029 (6)	0.0003 (5)
N2	0.0238 (6)	0.0302 (7)	0.0261 (6)	−0.0027 (5)	0.0002 (5)	0.0037 (5)
N3	0.0290 (7)	0.0308 (7)	0.0275 (7)	0.0044 (6)	−0.0005 (5)	−0.0004 (5)
O1	0.0271 (6)	0.0417 (7)	0.0227 (6)	−0.0094 (5)	0.0012 (4)	−0.0071 (5)
O2	0.0258 (6)	0.0284 (7)	0.0356 (6)	0.0032 (5)	0.0116 (5)	0.0065 (5)
O3	0.0245 (5)	0.0316 (6)	0.0240 (6)	0.0097 (5)	−0.0002 (4)	−0.0029 (5)
O4	0.0246 (6)	0.0536 (8)	0.0196 (6)	−0.0108 (5)	0.0018 (4)	−0.0078 (5)
O5	0.0395 (6)	0.0376 (8)	0.0265 (6)	−0.0047 (6)	0.0119 (5)	0.0013 (5)
O6	0.0314 (6)	0.0480 (8)	0.0269 (6)	0.0158 (5)	−0.0024 (5)	−0.0064 (5)
O7	0.0317 (6)	0.0576 (8)	0.0446 (7)	0.0009 (6)	0.0141 (5)	−0.0047 (6)
O8	0.0379 (7)	0.0536 (9)	0.0361 (7)	0.0013 (5)	−0.0045 (5)	0.0039 (5)
O9	0.0524 (9)	0.0741 (11)	0.0329 (7)	0.0144 (7)	0.0072 (6)	−0.0110 (6)
O10	0.0353 (6)	0.0431 (7)	0.0301 (6)	0.0072 (5)	−0.0080 (5)	−0.0057 (5)
O11	0.0271 (6)	0.0721 (10)	0.0422 (7)	0.0116 (6)	0.0006 (5)	−0.0133 (6)
O12	0.0339 (6)	0.0605 (9)	0.0324 (6)	0.0064 (6)	0.0018 (5)	−0.0149 (6)
O13	0.0301 (6)	0.0633 (9)	0.0255 (6)	−0.0049 (6)	0.0053 (5)	0.0088 (6)
O14	0.0262 (5)	0.0503 (7)	0.0242 (5)	−0.0054 (5)	−0.0023 (4)	0.0028 (5)
O15	0.0214 (5)	0.0629 (9)	0.0350 (6)	−0.0103 (5)	−0.0009 (4)	0.0128 (6)
O16	0.0336 (6)	0.0346 (7)	0.0323 (6)	0.0031 (5)	0.0066 (5)	0.0016 (5)
O17	0.0311 (6)	0.0496 (8)	0.0279 (6)	−0.0003 (6)	0.0024 (5)	−0.0019 (5)
O18	0.0383 (7)	0.0469 (8)	0.0365 (7)	−0.0027 (6)	−0.0027 (6)	−0.0091 (6)

Ga1—O1	1.9354 (10)	Ga2—O5	1.9654 (11)
Ga1—O1i	1.9354 (10)	N1—O9	1.2311 (19)
Ga1—O3	1.9438 (10)	N1—O8	1.2385 (18)
Ga1—O3i	1.9438 (10)	N1—O7	1.2513 (18)
Ga1—O2	1.9515 (11)	N2—O13	1.2343 (16)
Ga1—O2i	1.9515 (11)	N2—O15	1.2418 (16)
Ga2—O4ii	1.9280 (10)	N2—O14	1.2660 (16)
Ga2—O4	1.9280 (10)	N3—O11	1.2407 (17)
Ga2—O6ii	1.9510 (12)	N3—O12	1.2435 (17)
Ga2—O6	1.9510 (12)	N3—O10	1.2533 (16)
Ga2—O5ii	1.9654 (11)
O1—Ga1—O1i	180.0	O6ii—Ga2—O6	180.00 (8)
O1—Ga1—O3	89.45 (5)	O4ii—Ga2—O5ii	87.28 (5)
O1i—Ga1—O3	90.55 (5)	O4—Ga2—O5ii	92.72 (5)
O1—Ga1—O3i	90.55 (5)	O6ii—Ga2—O5ii	89.74 (6)
O1i—Ga1—O3i	89.45 (5)	O6—Ga2—O5ii	90.26 (6)
O3—Ga1—O3i	180.0	O4ii—Ga2—O5	92.72 (5)
O1—Ga1—O2	90.62 (5)	O4—Ga2—O5	87.28 (5)
O1i—Ga1—O2	89.38 (5)	O6ii—Ga2—O5	90.26 (6)
O3—Ga1—O2	89.23 (5)	O6—Ga2—O5	89.74 (6)
O3i—Ga1—O2	90.77 (5)	O5ii—Ga2—O5	180.0
O1—Ga1—O2i	89.38 (5)	O9—N1—O8	119.25 (15)
O1i—Ga1—O2i	90.62 (5)	O9—N1—O7	119.68 (14)
O3—Ga1—O2i	90.77 (5)	O8—N1—O7	121.06 (14)
O3i—Ga1—O2i	89.23 (5)	O13—N2—O15	121.45 (12)
O2—Ga1—O2i	179.999 (2)	O13—N2—O14	120.01 (12)
O4ii—Ga2—O4	180.0	O15—N2—O14	118.54 (12)
O4ii—Ga2—O6ii	88.81 (5)	O11—N3—O12	120.28 (13)
O4—Ga2—O6ii	91.19 (5)	O11—N3—O10	119.68 (13)
O4ii—Ga2—O6	91.19 (5)	O12—N3—O10	120.04 (12)
O4—Ga2—O6	88.81 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O18—H18···O8	0.80 (2)	2.26 (2)	2.9348 (18)	142 (2)
O16—H14···O18	0.83 (2)	2.07 (2)	2.8732 (19)	164 (2)
O5—H10···O7	0.82 (2)	1.91 (2)	2.7052 (17)	163 (2)
O1—H1···O16	0.81 (2)	1.85 (2)	2.6474 (16)	168 (2)
O4—H7···O14	0.81 (2)	1.83 (2)	2.6399 (15)	175 (2)
O5—H9···O17	0.81 (2)	1.87 (2)	2.676 (2)	174 (2)
O18—H17···O14	0.82 (2)	2.08 (2)	2.8729 (18)	163 (2)
O3—H6···O15iii	0.81 (2)	1.90 (2)	2.7150 (16)	175 (2)
O1—H2···O10iii	0.81 (2)	1.85 (2)	2.6545 (16)	175 (2)
O2—H4···O16iii	0.79 (2)	1.90 (2)	2.6895 (18)	175 (2)
O4—H8···O17iv	0.82 (2)	1.82 (2)	2.6312 (16)	171 (2)
O17—H15···O9iv	0.81 (2)	1.98 (2)	2.7791 (19)	171 (2)
O3—H5···O13v	0.79 (2)	1.96 (2)	2.7454 (16)	171 (2)
O6—H12···O12vi	0.80 (2)	1.93 (2)	2.7179 (16)	174 (2)
O16—H13···O18vii	0.82 (2)	1.93 (2)	2.7525 (19)	177 (3)
O6—H11···O11viii	0.80 (2)	1.90 (2)	2.6938 (17)	176 (2)
O2—H3···O8i	0.79 (2)	1.94 (2)	2.7269 (17)	169 (2)
O17—H16···O7ix	0.80 (2)	2.03 (2)	2.7675 (18)	154 (2)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O18—H18⋯O8	0.801 (16)	2.26 (2)	2.9348 (18)	142 (2)
O16—H14⋯O18	0.825 (15)	2.072 (15)	2.8732 (19)	163.8 (19)
O5—H10⋯O7	0.823 (16)	1.908 (17)	2.7052 (17)	163 (2)
O1—H1⋯O16	0.814 (15)	1.846 (16)	2.6474 (16)	168 (2)
O4—H7⋯O14	0.809 (15)	1.833 (15)	2.6399 (15)	175 (2)
O5—H9⋯O17	0.810 (16)	1.869 (16)	2.676 (2)	174 (2)
O18—H17⋯O14	0.816 (16)	2.082 (17)	2.8729 (18)	163 (2)
O3—H6⋯O15i	0.814 (15)	1.903 (16)	2.7150 (16)	175 (2)
O1—H2⋯O10i	0.808 (15)	1.848 (16)	2.6545 (16)	175 (2)
O2—H4⋯O16i	0.790 (16)	1.901 (16)	2.6895 (18)	175 (2)
O4—H8⋯O17ii	0.821 (15)	1.816 (15)	2.6312 (16)	171 (2)
O17—H15⋯O9ii	0.808 (15)	1.977 (16)	2.7791 (19)	171 (2)
O3—H5⋯O13iii	0.792 (15)	1.961 (16)	2.7454 (16)	171 (2)
O6—H12⋯O12iv	0.796 (15)	1.926 (16)	2.7179 (16)	174 (2)
O16—H13⋯O18v	0.820 (16)	1.934 (16)	2.7525 (19)	177 (3)
O6—H11⋯O11vi	0.800 (15)	1.895 (16)	2.6938 (17)	176 (2)
O2—H3⋯O8vii	0.794 (15)	1.943 (16)	2.7269 (17)	169 (2)
O17—H16⋯O7viii	0.802 (16)	2.026 (18)	2.7675 (18)	154 (2)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .