Buy article online - an online subscription or single-article purchase is required to access this article.
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.
Supporting information
CCDC reference: 150759
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.
Crystal data top
(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) Å3 | Parallelepiped, colorless |
Z = 4 | 0.12 × 0.06 × 0.05 mm |
Data collection top
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 top
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)] = 0.058 | H-atom parameters constrained |
wR(F2) = 0.136 | Calculated w = 1/[σ2(Fo2) + (0.0573P)2 + 3.0698P] where P = (Fo2 + 2Fc2)/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+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0130 (77) |
Special details top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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—O3i | 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—O8ii | 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—P2i | 1.530 (3) | C5—H5A | 0.97 |
O8—Al1ii | 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—O3i | 111.3 (2) | H2A—C2—H2B | 107.3 |
O4—P2—O3i | 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) |
O3i—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—O8ii | 111.3 (2) | H3A—C3—H3B | 106.1 |
O1—Al1—O8ii | 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) |
O8ii—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 |
P2i—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—Al1ii | 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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2···O4ii | 0.82 | 1.67 | 2.457 (4) | 159 |
N1—H1A···O2iii | 0.89 | 2.00 | 2.885 (5) | 177 |
N1—H1B···O6 | 0.89 | 1.89 | 2.745 (5) | 162 |
N1—H1C···O7iv | 0.89 | 1.86 | 2.727 (5) | 163 |
N2—H2C···O6v | 0.89 | 1.88 | 2.750 (5) | 165 |
N2—H2D···O4vi | 0.89 | 2.05 | 2.869 (5) | 153 |
N2—H2E···O7v | 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. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.