2,4,6-Triamino-1,3,5-triazine-1,3-diium aqua-penta-fluoridoaluminate.

The title compound, (C(3)H(8)N(6))[AlF(5)(H(2)O)], was obtained by solvothermal synthesis from the reaction of aluminium hydroxide, 1,3,5-triazine-2,4,6-triamine (melamine), aqueous HF and water at 323 K for 48 h. The structure consists of [AlF(5)(H(2)O)](2-) octa-hedra and diprotonated melaminium cations. Cohesion is ensured by a three-dimensional network of hydrogen bonds.

Related literature

For related literature, see: Adil, Ben Ali et al. (2006 ▶); Adil, Leblanc & Maisonneuve (2006 ▶); Farrugia (1999 ▶); Goreshnik et al. (2002 ▶, 2003 ▶); Rother et al. (1996 ▶, 1998 ▶); Schroder et al. (1993 ▶); Tang et al. (2001 ▶).

Experimental

Crystal data

(C3H8N6)[AlF5(H2O)]

M = 268.13

Monoclinic,

a = 7.571 (2) Å

b = 8.823 (2) Å

c = 13.484 (5) Å

β = 105.53 (3)°

V = 867.8 (5) Å3

Z = 4

Mo Kα radiation

μ = 0.31 mm−1

T = 298 (2) K

0.20 × 0.13 × 0.08 mm

Data collection

Siemens AED2 diffractometer

Absorption correction: none

2500 measured reflections

2500 independent reflections

1441 reflections with I > 2σ(I)

3 standard reflections frequency: 120 min intensity decay: 4%

Refinement

R[F 2 > 2σ(F 2)] = 0.054

wR(F 2) = 0.133

S = 1.04

2500 reflections

152 parameters

2 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.46 e Å−3

Δρmin = −0.48 e Å−3

Data collection: STADI4 (Stoe & Cie, 1998 ▶); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1998 ▶); 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 DIAMOND (Brandenburg, 2005 ▶); software used to prepare material for publication: SHELXL97, enCIFer (Version 1.2; Allen et al., 2004 ▶) and WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808004091/dn2317sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808004091/dn2317Isup2.hkl

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

(C3H8N6)[AlF5(H2O)]	F000 = 544
Mr = 268.13	Dx = 2.052 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 30 reflections
a = 7.571 (2) Å	θ = 28–32º
b = 8.823 (2) Å	µ = 0.31 mm−1
c = 13.484 (5) Å	T = 298 (2) K
β = 105.53 (3)º	Parallepiped, colourless
V = 867.8 (5) Å3	0.20 × 0.13 × 0.08 mm
Z = 4

Siemens AED2 diffractometer	Rint = 0.0000
Radiation source: fine-focus sealed tube	θmax = 30.0º
Monochromator: graphite	θmin = 2.8º
T = 298(2) K	h = −10→10
2θ/ω scans	k = 0→12
Absorption correction: none	l = 0→18
2500 measured reflections	3 standard reflections
2500 independent reflections	every 120 min
1441 reflections with I > 2σ(I)	intensity decay: 4%

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.054	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.133	w = 1/[σ2(Fo2) + (0.0437P)2 + 0.9389P] where P = (Fo2 + 2Fc2)/3
S = 1.04	(Δ/σ)max < 0.001
2500 reflections	Δρmax = 0.46 e Å−3
152 parameters	Δρmin = −0.48 e Å−3
2 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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
Al1	0.2088 (1)	0.2232 (1)	0.30136 (7)	0.0163 (2)
F1	0.0457 (3)	0.0750 (2)	0.30467 (16)	0.0288 (5)
F2	0.2911 (3)	0.1978 (2)	0.44074 (14)	0.0251 (4)
F3	0.3778 (3)	0.0880 (2)	0.28702 (17)	0.0299 (5)
F4	0.3610 (3)	0.3839 (2)	0.31272 (16)	0.0267 (5)
F5	0.1237 (3)	0.2429 (2)	0.16732 (14)	0.0304 (5)
O1W	0.0310 (3)	0.3648 (3)	0.32584 (18)	0.0214 (5)
H1W	−0.062 (5)	0.324 (5)	0.346 (4)	0.062 (12)*
H2W	−0.007 (7)	0.444 (4)	0.284 (3)	0.062 (12)*
N1	0.7845 (4)	0.2143 (3)	−0.0619 (2)	0.0202 (6)
N2	0.6746 (4)	0.1144 (3)	0.0739 (2)	0.0195 (6)
H2	0.6499	0.0359	0.1056	0.023*
N3	0.6895 (4)	0.3729 (3)	0.0557 (2)	0.0203 (6)
H3	0.6714	0.4633	0.0748	0.024*
N4	0.7594 (4)	−0.0423 (3)	−0.0409 (2)	0.0232 (6)
H4A	0.7996	−0.0586	−0.0938	0.028*
H4B	0.7310	−0.1173	−0.0074	0.028*
N5	0.5822 (4)	0.2735 (3)	0.1861 (2)	0.0271 (6)
H5A	0.5543	0.1966	0.2181	0.033*
H5B	0.5664	0.3638	0.2063	0.033*
N6	0.8013 (4)	0.4736 (3)	−0.0717 (2)	0.0293 (7)
H6A	0.8446	0.4652	−0.1242	0.035*
H6B	0.7850	0.5619	−0.0486	0.035*
C1	0.7414 (4)	0.0960 (3)	−0.0113 (2)	0.0179 (6)
C2	0.6481 (4)	0.2534 (4)	0.1076 (2)	0.0191 (6)
C3	0.7602 (4)	0.3525 (4)	−0.0271 (2)	0.0199 (6)

	U11	U22	U33	U12	U13	U23
Al1	0.0209 (5)	0.0127 (4)	0.0176 (4)	−0.0002 (4)	0.0090 (3)	−0.0014 (4)
F1	0.0359 (13)	0.0199 (10)	0.0351 (11)	−0.0115 (9)	0.0175 (10)	−0.0075 (9)
F2	0.0330 (11)	0.0214 (10)	0.0204 (9)	0.0027 (8)	0.0063 (8)	0.0020 (8)
F3	0.0355 (13)	0.0191 (10)	0.0413 (12)	0.0089 (9)	0.0207 (10)	0.0013 (9)
F4	0.0292 (12)	0.0191 (9)	0.0379 (11)	−0.0069 (8)	0.0197 (10)	−0.0054 (9)
F5	0.0435 (13)	0.0312 (11)	0.0188 (9)	0.0044 (10)	0.0122 (9)	−0.0009 (8)
O1W	0.0240 (13)	0.0179 (11)	0.0251 (12)	0.0055 (10)	0.0113 (10)	0.0066 (9)
N1	0.0263 (14)	0.0171 (13)	0.0202 (13)	−0.0005 (11)	0.0114 (11)	0.0003 (11)
N2	0.0256 (15)	0.0133 (12)	0.0236 (13)	−0.0001 (11)	0.0134 (12)	0.0016 (10)
N3	0.0260 (15)	0.0125 (12)	0.0240 (13)	−0.0006 (10)	0.0097 (12)	−0.0026 (10)
N4	0.0354 (18)	0.0180 (13)	0.0204 (13)	0.0015 (12)	0.0152 (12)	−0.0003 (11)
N5	0.0340 (17)	0.0241 (14)	0.0288 (15)	−0.0016 (13)	0.0181 (13)	−0.0034 (13)
N6	0.0402 (19)	0.0190 (14)	0.0328 (16)	−0.0052 (13)	0.0166 (15)	0.0020 (12)
C1	0.0200 (16)	0.0181 (15)	0.0166 (14)	0.0008 (12)	0.0065 (12)	−0.0002 (12)
C2	0.0168 (15)	0.0205 (15)	0.0204 (14)	−0.0022 (12)	0.0056 (12)	−0.0025 (12)
C3	0.0192 (16)	0.0177 (15)	0.0228 (15)	−0.0005 (12)	0.0056 (13)	0.0006 (13)

Al1—F5	1.757 (2)	N3—C2	1.347 (4)
Al1—F3	1.797 (2)	N3—C3	1.374 (4)
Al1—F4	1.807 (2)	N3—H3	0.8600
Al1—F1	1.807 (2)	N4—C1	1.302 (4)
Al1—F2	1.829 (2)	N4—H4A	0.8600
Al1—O1W	1.929 (2)	N4—H4B	0.8600
O1W—H1W	0.90 (4)	N5—C2	1.299 (4)
O1W—H2W	0.90 (4)	N5—H5A	0.8600
N1—C1	1.334 (4)	N5—H5B	0.8600
N1—C3	1.337 (4)	N6—C3	1.304 (4)
N2—C2	1.342 (4)	N6—H6A	0.8600
N2—C1	1.383 (4)	N6—H6B	0.8600
N2—H2	0.8600
F5—Al1—F3	91.76 (11)	C2—N3—H3	119.5
F5—Al1—F4	93.42 (11)	C3—N3—H3	119.5
F3—Al1—F4	94.23 (10)	C1—N4—H4A	120.0
F5—Al1—F1	91.84 (11)	C1—N4—H4B	120.0
F3—Al1—F1	91.90 (10)	H4A—N4—H4B	120.0
F4—Al1—F1	171.80 (10)	C2—N5—H5A	120.0
F5—Al1—F2	177.98 (12)	C2—N5—H5B	120.0
F3—Al1—F2	88.45 (11)	H5A—N5—H5B	120.0
F4—Al1—F2	88.57 (10)	C3—N6—H6A	120.0
F1—Al1—F2	86.15 (10)	C3—N6—H6B	120.0
F5—Al1—O1W	91.80 (11)	H6A—N6—H6B	120.0
F3—Al1—O1W	176.37 (11)	N4—C1—N1	121.1 (3)
F4—Al1—O1W	86.32 (10)	N4—C1—N2	117.1 (3)
F1—Al1—O1W	87.23 (10)	N1—C1—N2	121.8 (3)
F2—Al1—O1W	87.97 (10)	N5—C2—N2	121.7 (3)
H1W—O1W—H2W	111 (4)	N5—C2—N3	120.7 (3)
C1—N1—C3	117.3 (3)	N2—C2—N3	117.6 (3)
C2—N2—C1	120.6 (3)	N6—C3—N1	120.9 (3)
C2—N2—H2	119.7	N6—C3—N3	117.4 (3)
C1—N2—H2	119.7	N1—C3—N3	121.7 (3)
C2—N3—C3	121.0 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···N1i	0.90 (4)	1.94 (5)	2.789 (3)	156 (5)
O1W—H2W···F1ii	0.90 (4)	1.63 (4)	2.515 (3)	169 (5)
N2—H2···F4iii	0.86	1.75	2.601 (3)	169
N3—H3···F2iv	0.86	2.11	2.871 (3)	148
N3—H3···F3iv	0.86	2.28	2.990 (3)	140
N3—H3···F1iv	0.86	2.52	2.953 (4)	112
N4—H4A···F5v	0.86	2.07	2.763 (3)	138
N4—H4B···F2iii	0.86	1.89	2.739 (3)	168
N5—H5A···F3	0.86	2.06	2.837 (3)	151
N5—H5B···F3iv	0.86	2.02	2.804 (4)	151
N5—H5B···F4	0.86	2.39	2.863 (3)	115
N6—H6A···F1vi	0.86	2.04	2.836 (4)	154
N6—H6B···F2iv	0.86	2.08	2.860 (4)	150

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯N1i	0.90 (4)	1.94 (5)	2.789 (3)	156 (5)
O1W—H2W⋯F1ii	0.90 (4)	1.63 (4)	2.515 (3)	169 (5)
N2—H2⋯F4iii	0.86	1.75	2.601 (3)	169
N3—H3⋯F2iv	0.86	2.11	2.871 (3)	148
N3—H3⋯F3iv	0.86	2.28	2.990 (3)	140
N3—H3⋯F1iv	0.86	2.52	2.953 (4)	112
N4—H4A⋯F5v	0.86	2.07	2.763 (3)	138
N4—H4B⋯F2iii	0.86	1.89	2.739 (3)	168
N5—H5A⋯F3	0.86	2.06	2.837 (3)	151
N5—H5B⋯F3iv	0.86	2.02	2.804 (4)	151
N5—H5B⋯F4	0.86	2.39	2.863 (3)	115
N6—H6A⋯F1vi	0.86	2.04	2.836 (4)	154
N6—H6B⋯F2iv	0.86	2.08	2.860 (4)	150

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