[H₃N(CH₂)₅NH₃]·AlP₂O₈H, a one-dimensional aluminophosphate

The structure of the title compound, pentane-1,5-di­ammonium aluminium(III) hydrogen bis(phosphate), (C₅H₁₆N₂)[AlP₂O₈H], obtained solvothermally at 473 K, has been determined by single-crystal X-ray diffraction. It consists of one-dimensional [AlP₂O₈H]^2- macroanions, connected to each other by pentane­di­ammonium cations. Contrary to similar compounds with P/Al = 2, the three-dimensional structure is mainly obtained via a network of hydrogen bonds.

Computing details

Data collection: SMART (Siemens, 1996a); cell refinement: SMART; data reduction: SHELXTL96 (Siemens, 1996b); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: DIAMOND (Bergerhoff, 1996); software used to prepare material for publication: SHELXTL.

(I)

Crystal data

(C5H16N2)[AlHP2O8]	F(000) = 672
Mr = 322.13	Dx = 1.621 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 7.8783 (2) Å	Cell parameters from 5007 reflections
b = 10.4689 (1) Å	θ = 2.3–29.8°
c = 16.0680 (4) Å	µ = 0.43 mm^−1
β = 95.147 (1)°	T = 296 K
V = 1319.90 (5) Å^3	Parallelepiped, colorless
Z = 4	0.12 × 0.06 × 0.05 mm

Data collection

Siemens SMART diffractometer	3421 independent reflections
Radiation source: fine-focus sealed tube	1901 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
ω scans	θmax = 29.8°, θmin = 2.3°
Absorption correction: semi-empirical (using intensity measurements) SADABS (Sheldrick, 1996)	h = −10→10
Tmin = 0.844, Tmax = 0.978	k = −14→13
8939 measured reflections	l = −21→9

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.058	H-atom parameters constrained
wR(F^2) = 0.136	Calculated w = 1/[σ^2(Fo^2) + (0.0573P)^2 + 3.0698P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max < 0.001
2521 reflections	Δρmax = 1.36 e Å^−3
167 parameters	Δρmin = −0.60 e Å^−3
4 restraints	Extinction correction: SHELXL93 (Sheldrick, 1993), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0130 (77)

Special details

Experimental. 'Blessing, Acta Cryst. (1995) A51 33–38'

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 on F² for ALL reflections except for 900 with very negative F² or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The observed criterion of F² > σ(F²) is used only for calculating R-factor-obs 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
P1	0.55909 (13)	0.78402 (9)	0.02396 (7)	0.0280 (3)
P2	0.09646 (13)	1.05563 (11)	0.13485 (6)	0.0290 (3)
Al1	0.24723 (13)	0.95928 (11)	−0.02995 (7)	0.0246 (4)
O1	0.1684 (4)	0.9724 (3)	0.0667 (2)	0.0379 (7)
O2	0.6564 (4)	0.7078 (3)	−0.0386 (2)	0.0373 (7)
H2	0.7123	0.7571	−0.0649	0.056*
O3	0.0882 (4)	0.9116 (3)	−0.1048 (2)	0.0381 (7)
O4	0.1982 (4)	1.1793 (3)	0.1459 (2)	0.0467 (9)
O5	0.4005 (4)	0.8408 (3)	−0.0252 (2)	0.0435 (8)
O6	0.5116 (4)	0.6993 (3)	0.0927 (2)	0.0466 (8)
O7	0.1067 (5)	0.9814 (4)	0.2149 (2)	0.0521 (9)
O8	0.6701 (4)	0.8956 (3)	0.0585 (2)	0.0398 (8)
N1	0.5653 (6)	0.4525 (4)	0.1464 (2)	0.0438 (10)
H1A	0.4934	0.4053	0.1133	0.066*
H1B	0.5704	0.5309	0.1254	0.066*
H1C	0.5288	0.4565	0.1972	0.066*
C1	0.7372 (9)	0.3936 (7)	0.1518 (5)	0.077 (2)
H1D	0.7840	0.4038	0.0984	0.092*
H1E	0.7258	0.3028	0.1618	0.092*
C2	0.8618 (10)	0.4488 (8)	0.2194 (5)	0.088 (2)
H2A	0.8225	0.4271	0.2732	0.105*
H2B	0.9709	0.4071	0.2162	0.105*
C3	0.8903 (13)	0.5913 (9)	0.2175 (5)	0.110 (3)
H3A	0.7912	0.6290	0.2395	0.132*
H3B	0.9855	0.6077	0.2587	0.132*
C4	0.9232 (15)	0.6711 (14)	0.1428 (8)	0.153 (5)
H4A	0.8502	0.6411	0.0950	0.184*
H4B	0.8917	0.7587	0.1534	0.184*
C5	1.1025 (11)	0.6688 (10)	0.1213 (5)	0.099 (3)
H5A	1.1363	0.5802	0.1162	0.118*
H5B	1.1062	0.7081	0.0669	0.118*
N2	1.2290 (5)	0.7318 (4)	0.1793 (3)	0.0439 (9)
H2C	1.3301	0.7296	0.1586	0.066*
H2D	1.2357	0.6916	0.2283	0.066*
H2E	1.1984	0.8127	0.1863	0.066*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
P1	0.0276 (5)	0.0230 (5)	0.0341 (6)	0.0016 (4)	0.0063 (4)	0.0016 (4)
P2	0.0259 (5)	0.0418 (6)	0.0193 (5)	−0.0018 (4)	0.0019 (4)	−0.0034 (4)
Al1	0.0218 (6)	0.0289 (6)	0.0233 (6)	0.0004 (4)	0.0024 (4)	−0.0027 (4)
O1	0.041 (2)	0.048 (2)	0.0262 (15)	0.0047 (14)	0.0096 (12)	−0.0020 (13)
O2	0.036 (2)	0.0285 (15)	0.049 (2)	0.0033 (12)	0.0141 (13)	−0.0019 (13)
O3	0.0279 (15)	0.049 (2)	0.037 (2)	−0.0003 (13)	−0.0009 (12)	−0.0117 (13)
O4	0.042 (2)	0.060 (2)	0.039 (2)	−0.019 (2)	0.0100 (14)	−0.016 (2)
O5	0.036 (2)	0.046 (2)	0.047 (2)	0.0153 (14)	−0.0034 (14)	−0.0090 (14)
O6	0.055 (2)	0.032 (2)	0.056 (2)	−0.0010 (14)	0.022 (2)	0.0116 (14)
O7	0.060 (2)	0.073 (2)	0.024 (2)	0.015 (2)	0.0098 (14)	0.0063 (15)
O8	0.045 (2)	0.036 (2)	0.038 (2)	−0.0117 (14)	0.0052 (13)	−0.0015 (13)
N1	0.067 (3)	0.030 (2)	0.037 (2)	−0.006 (2)	0.016 (2)	−0.003 (2)
C1	0.080 (4)	0.070 (4)	0.080 (5)	0.012 (3)	0.000 (4)	−0.026 (3)
C2	0.073 (4)	0.123 (7)	0.067 (4)	−0.002 (4)	0.008 (3)	−0.005 (4)
C3	0.097 (6)	0.158 (10)	0.077 (5)	−0.056 (6)	0.015 (4)	−0.002 (6)
C4	0.169 (13)	0.130 (10)	0.153 (12)	−0.019 (9)	−0.024 (10)	0.010 (8)
C5	0.099 (6)	0.134 (7)	0.063 (4)	−0.075 (5)	0.004 (4)	−0.007 (4)
N2	0.041 (2)	0.052 (2)	0.039 (2)	−0.002 (2)	0.006 (2)	0.012 (2)

Geometric parameters (Å, º)

P1—O6	1.490 (3)	C1—C2	1.512 (8)
P1—O8	1.533 (3)	C1—H1D	0.97
P1—O5	1.537 (3)	C1—H1E	0.97
P1—O2	1.539 (3)	C2—C3	1.509 (9)
P2—O7	1.499 (3)	C2—H2A	0.97
P2—O4	1.525 (3)	C2—H2B	0.97
P2—O3^i	1.530 (3)	C3—C4	1.503 (9)
P2—O1	1.546 (3)	C3—H3A	0.97
Al1—O5	1.727 (3)	C3—H3B	0.97
Al1—O1	1.729 (3)	C4—C5	1.484 (9)
Al1—O8^ii	1.731 (3)	C4—H4A	0.97
Al1—O3	1.731 (3)	C4—H4B	0.97
O2—H2	0.82	C5—N2	1.459 (8)
O3—P2^i	1.530 (3)	C5—H5A	0.97
O8—Al1^ii	1.731 (3)	C5—H5B	0.97
N1—C1	1.483 (8)	N2—H2C	0.89
N1—H1A	0.89	N2—H2D	0.89
N1—H1B	0.89	N2—H2E	0.89
N1—H1C	0.89
O6—P1—O8	111.0 (2)	C2—C1—H1E	108.6 (5)
O6—P1—O5	111.4 (2)	H1D—C1—H1E	107.6
O8—P1—O5	107.6 (2)	C3—C2—C1	116.8 (7)
O6—P1—O2	110.4 (2)	C3—C2—H2A	108.1 (5)
O8—P1—O2	109.3 (2)	C1—C2—H2A	108.1 (5)
O5—P1—O2	107.1 (2)	C3—C2—H2B	108.1 (5)
O7—P2—O4	110.6 (2)	C1—C2—H2B	108.1 (4)
O7—P2—O3^i	111.3 (2)	H2A—C2—H2B	107.3
O4—P2—O3^i	108.8 (2)	C4—C3—C2	127.0 (9)
O7—P2—O1	108.7 (2)	C4—C3—H3A	105.6 (7)
O4—P2—O1	109.8 (2)	C2—C3—H3A	105.6 (5)
O3^i—P2—O1	107.6 (2)	C4—C3—H3B	105.6 (6)
O5—Al1—O1	108.9 (2)	C2—C3—H3B	105.6 (5)
O5—Al1—O8^ii	111.3 (2)	H3A—C3—H3B	106.1
O1—Al1—O8^ii	110.0 (2)	C5—C4—C3	114.4 (9)
O5—Al1—O3	106.4 (2)	C5—C4—H4A	108.7 (7)
O1—Al1—O3	110.6 (2)	C3—C4—H4A	108.7 (7)
O8^ii—Al1—O3	109.6 (2)	C5—C4—H4B	108.7 (7)
P2—O1—Al1	149.8 (2)	C3—C4—H4B	108.7 (7)
P1—O2—H2	109.47 (12)	H4A—C4—H4B	107.6
P2^i—O3—Al1	139.7 (2)	N2—C5—C4	117.0 (9)
P1—O5—Al1	146.4 (2)	N2—C5—H5A	108.0 (5)
P1—O8—Al1^ii	142.0 (2)	C4—C5—H5A	108.0 (7)
C1—N1—H1A	109.5 (3)	N2—C5—H5B	108.0 (4)
C1—N1—H1B	109.5 (4)	C4—C5—H5B	108.0 (6)
H1A—N1—H1B	109.5	H5A—C5—H5B	107.3
C1—N1—H1C	109.5 (3)	C5—N2—H2C	109.5 (4)
H1A—N1—H1C	109.5	C5—N2—H2D	109.5 (4)
H1B—N1—H1C	109.5	H2C—N2—H2D	109.5
N1—C1—C2	114.5 (5)	C5—N2—H2E	109.5 (5)
N1—C1—H1D	108.6 (4)	H2C—N2—H2E	109.5
C2—C1—H1D	108.6 (4)	H2D—N2—H2E	109.5
N1—C1—H1E	108.6 (3)

Symmetry codes: (i) −x, −y+2, −z; (ii) −x+1, −y+2, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O4^ii	0.82	1.67	2.457 (4)	159
N1—H1A···O2^iii	0.89	2.00	2.885 (5)	177
N1—H1B···O6	0.89	1.89	2.745 (5)	162
N1—H1C···O7^iv	0.89	1.86	2.727 (5)	163
N2—H2C···O6^v	0.89	1.88	2.750 (5)	165
N2—H2D···O4^vi	0.89	2.05	2.869 (5)	153
N2—H2E···O7^v	0.89	1.98	2.861 (6)	171

Symmetry codes: (ii) −x+1, −y+2, −z; (iii) −x+1, −y+1, −z; (iv) −x+1/2, y−1/2, −z+1/2; (v) x+1, y, z; (vi) −x+3/2, y−1/2, −z+1/2.