α-Tris(2,4-pentanedionato-κ²O,O′)aluminium(III) at 240, 210, 180, 150 and 110 K: a new δ phase at 110 K

The crystal structure of the title compound, [Al(C₅H₇O₂)₃], has been investigated by a multi-temperature measurement to provide information on thermal vibrations and disorder in the structure. At 110 K, the structure of a new δ polymorph could be determined. A disorder–order phase transition takes place between 150 and 110 K and is klassengleich. The unit-cell volume increases by a factor of three and the diffraction pattern shows weak supercell reflections.

S1. Comment

The crystal structures of trivalent metal acetylacetonate complexes can be grouped into several isomorphous series [an overview is given by Sabolović et al. (2004)]. According to an old nomenclature by Astbury & Gilbert (1926), the α polymorph crystallizes in the monoclinic crystal system with space group P2₁/c. The β and γ polymorphs crystallize in the orthorhombic crystal system with space groups Pbca and Pna2₁, respectively. Two different polymorphs of Al(acac)₃ (acac is acetylacetonate or 2,4-pentanedionate) have been previously investigated, namely the α and γ polymorphs. Both polymorphs can occur in the same crystallization batch. All previous crystallographic studies of the α polymorph were carried out at room temperature, according to a search of the Cambridge Structural Database (Version 5.28 of November 2006; Allen, 2002). Recently, we redetermined the crystal structure of the γ polymorph at 110 K, which contains four independent molecules (von Chrzanowski et al., 2006). In the course of our studies on Al(acac)₃, we have now redetermined the crystal structure of α-Al(acac)₃ by a multi-temperature measurement at 240, (Ia), 210, (Ib), 180, (Ic), 150, (Id), and 110 K, (Ie), in order to investigate the behaviour of atoms C11 and C15, which showed anomalous displacement parameters/disorder in the known studies of α polymorphs (Morosin, 1965; Diaz-Acosta et al., 2001; Fackler & Avdeef, 1974). At a temperature of 110 K, we found a new δ polymorph, (Ie), which is a superstructure of the α polymorph. The phase transition occurs between 150 and 110 K.

The transformation matrix from the high-temperature α polymorph to the low-temperature δ polymorph is (101/010/201). The determinant of this matrix is 3 and thus the volume is increased by a factor of three. The space group remains P2₁/c and the phase transition is therefore klassengleich. In the asymmetric unit of the δ polymorph there are three independent molecules (Fig. 1). All molecules have an approximate non crystallographic D₃ symmetry with r.m.s. deviations between 0.127 and 0.176 Å from ideal symmetry (Pilati & Forni, 1998). The molecules occupy pseudo-special positions with centers of gravity at (0.27, 0.23, 0.26), (0.40, 0.78, 0.07) and (0.06, 3/4, 0.40). All three molecules have essentially the same geometry as can be seen in a quaternion fit (Fig. 2a). This quaternion fit (Mackay, 1984) considers only the molecular structures, but does not take the crystal packing into account. The packing effects can be seen by the application of the transformation matrix to the α polymorph on the atomic coordinates of the δ polymorph. The result of this operation can be seen in Fig. 2(b). Two of the acac ligands have only very small deviations after this averaging, while the third ligand (C11x–C15x) is severely affected by the packing. The latter ligand corresponds to the ligand with large displacement parameters in the α polymorph. We therefore consider this phase transition as a disorder–order phase transition.

The ADDSYM routine of the program PLATON (Spek, 2003) indicates pseudo-translational symmetry for the δ polymorph. This pseudo-translational symmetry can also be seen in the X-ray intensities. Reflections with h + 2l = 3n correspond to the subcell and are much stronger than the other reflections. Nevertheless, the weak supercell reflections are clearly present and prevent a transformation to the subcell (Fig. 3). The strongest superstructure reflection is (220) with I/σ(I) of 157.29. The average I/σ(I) of the subcell reflections is 44.43, while the supercell reflections have an average I/σ(I) of 13.60. A test on pseudo-translational symmetry based on normalized structure factors from measured data (Cascarano et al., 1985) as implemented in the program SIR97 (Altomare et al., 1999) results in a value of 70% for the mean fractional scattering power of the electron density for reflections with h ± 1l = 3n and with h + 2l = 3n. The corresponding <E**2> value for these reflections is 2.409.

Despite the pseudo-translational symmetry, a full-matrix least-squares refinement with SHELXL97 (Sheldrick, 1997) can be performed with default refinement parameters and without restraints or constraints. No correlation matrix elements were larger than 0.5. The weighting scheme for the refinement was optimized by SHELXL97 based on all 11 232 unique reflections and results in a goodness-of-fit of 1.046. The corresponding goodness-of-fit for the 3741 strong subcell reflections without re-refinement and with the same weighting scheme is 1.418, and for the 7491 weak supercell reflections 0.881. Obviously, the weighted sigmas of the subcell reflections are underestimated and those of the supercell reflections overestimated in the refinement. A manual correction of the sigmas based on normal probability plots for subcell and supercell reflections did not change the outcome of the refinement.

The phase transition from the high-temperature α phase to the low-temperature δ phase breaks the translational symmetry for the C11–C15 acac ligand (see above). Nevertheless, the anisotropicity of some methyl groups is still rather large, but this now concerns also methyl groups of other acac ligands. Indeed, rigid-body analyses (Schomaker & Trueblood, 1998) for the three molecules result in relatively high agreement factors of R = 0.156–0.187 (R = {Σ[(U_obs - U_calc)²]/Σ(U_obs²)}^1/2). Difference plots (Hummel et al., 1990) between the observed displacement parameters and the rigid-body models (Fig. 4) make the large internal motions of the methyl groups visible. These internal motions are also reflected in a relatively large variation of the bond lengths. For example, the Al—O distances vary between 1.8704 (9) and 1.8924 (9) Å. The corresponding Al—O distances in the γ-polymorph (von Chrzanowski et al., 2006) are 1.8728 (13)–1.8947 (12) Å and show a similar variation. Because Al^III does not express Jahn–Teller distortions, this variation can only be explained by internal thermal motion. The thermal motion also explains why the Al—O distances of the crystal structure determinations are shorter than the 1.9159 Å obtained from quantum chemical calculations (Diaz-Acosta et al., 2001).

As expected, a temperature-dependent measurement of the α polymorph shows a decreasing thermal motion with decreasing temperature (Fig. 5). The eigenvalues of translation T_i and libration L_i tensors obtained from rigid-body analyses (PLATON; Spek, 2003) show that this decrease is linear (Fig. 6). In the whole temperature range, the agreement factors are rather high (R = 0.155–0.167). The corresponding internal motion is visualized by difference plots (Hummel et al., 1990) between the observed displacement parameters and the rigid-body models for (Ia)–(Id) (Fig. 7). The non-rigid behaviour is mainly expressed by only one acac ligand (C11–C15). This is the same ligand that breaks the translational symmetry in the δ phase. Quantum chemical calculations have proven the presence of out-of-plane deformations in isolated Al(acac)₃ molecules (Diaz-Acosta et al., 2001). However, from the observed phase transition we assume the anisotropicity of C11–C15 is a property of the crystal packing.

Related literature

For related literature, see: Allen (2002); Altomare et al. (1999); Astbury & Gilbert (1926); Cascarano et al. (1985); Chrzanowski et al. (2006); Diaz-Acosta, Baker, Cordes & Pulay (2001); Fackler & Avdeef (1974); Hummel et al. (1990); Mackay (1984); Morosin (1965); Pilati & Forni (1998); Sabolović et al. (2004); Schomaker & Trueblood (1998); Sheldrick (1997); Spek (2003).

S2. Experimental

Crystals were obtained by slow evaporation of a solution of the commercially available material (Aldrich) in ethyl acetate at room temperature. In the batch, plate- and needle-shaped crystals were present. For data collection, a plate-shaped crystal was selected.

S3. Refinement

The X-ray intensities of (Ia)–(Ie) were obtained with two different exposure times and rotation angles of 1. 364 ϕ and 252 ω scans were measured with an exposure time of 45 s per frame, and 167 ϕ scans with an exposure time of 9 s per frame. All H atoms were introduced in geometrically idealized positions, refined with a riding model and subsequently confirmed in a difference Fourier map. Their isotropic displacement parameters were constrained, with U_iso(H) values of 1.2U_eq(C) for H atoms of the central CH groups and 1.5U_eq(C) for methyl H atoms.

Computing details

For all compounds, data collection: COLLECT (Nonius, 1999); cell refinement: PEAKREF (Schreurs, 2005). Data reduction: EVAL14 (Duisenberg et al., 2003) for (Ia), (Ib), (Ic), (Id); EVAL15 (Xian et al., 2006) for (Ie). Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) for (Ia), (Ie); coordinates were taken from (Ia) for (Ib), (Ic), (Id). For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: manual editing of SHELXL97 output.

Figures

	Fig. 1. : Displacement ellipsoid plot and atomic numbering scheme of the three independent molecules in the asymmetric unit of (Ie). Ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity.
	Fig. 2. : (a) Quaternion fit of the three independent molecules of (Ie). (b) Transformation of the three independent molecules of (Ie) into an average structure using the transformation matrix between the δ and the α polymorph. [In the online version of the journal, yellow atoms represent molecule 1 (x = 1), red atoms molecule 2 (x = 2) and orange atoms molecule 3 (x = 3).]
	Fig. 3. : Simulated precession photograph of (Ie) using the reflection file of the refinement (Barbour, 1999) showing the h0l plane. Intensities are drawn on a logarithmic scale. [in the online version of the journal, red dots represent strong reflections of the subcell; gray dots represent weak reflections of the supercell. The base vectors of the reciprocal subcell are drawn with red and of the supercell with gray lines.] The transformation matrix used to generate the subcell is (1/3 0 1/3 / 0 1 0 / 2/3 0 1/3).
	Fig. 4. : Peanut plot (Hummel et al., 1990) of (Ie) showing the difference between the measured displacement parameters and the parameters obtained by three independent rigid-body analyses using the program THMA11 (Schomaker & Trueblood, 1998). A scale factor of 3.08 was used for the r.m.s. surfaces. [In the online version of the journal, blue lines indicate positive differences and red lines negative ones.] All molecules are drawn independently in the same orientation and do not represent the crystal packing.
	Fig. 5. : Displacement ellipsoid plots and atomic numbering scheme of (Ia)–(Id). Ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity. All plots are drawn in the same orientation and have the same labelling scheme.
	Fig. 6. : Eigenvalues of translation Ti (top) and liberation Li (bottom) tensors from rigid-body analyses (PLATON; Spek, 2003) as a function of temperature.
	Fig. 7. : Peanut plots of (Ia)–(Id) showing the difference between the measured displacement parameters and the parameters obtained by rigid-body analyses using the program THMA11 (Schomaker & Trueblood, 1998). A scale factor of 3.08 was used for the r.m.s. surfaces. [In the online version of the journal, blue lines indicate positive differences and red lines negative ones.]

(Ia) Tris(pentane-2,4-dionato-κ²O,O')aluminium(III)

Crystal data

[Al(C5H7O2)3]	F(000) = 688
Mr = 324.30	Dx = 1.285 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 12689 reflections
a = 13.9140 (7) Å	θ = 2.7–27.5°
b = 7.50076 (17) Å	µ = 0.15 mm^−1
c = 16.2547 (6) Å	T = 240 K
β = 98.806 (2)°	Hexagonal prism, colourless
V = 1676.44 (11) Å^3	0.42 × 0.39 × 0.18 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	3870 independent reflections
Radiation source: rotating anode	3065 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
ϕ and ω scans	θmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −18→18
Tmin = 0.67, Tmax = 0.97	k = −9→9
29848 measured reflections	l = −21→21

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: difference Fourier map
wR(F^2) = 0.124	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0624P)^2 + 0.4307P] where P = (Fo^2 + 2Fc^2)/3
3870 reflections	(Δ/σ)max = 0.001
205 parameters	Δρmax = 0.20 e Å^−3
0 restraints	Δρmin = −0.23 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Al1	0.24092 (4)	0.26883 (6)	0.46909 (3)	0.03907 (14)
O1	0.25837 (8)	0.49812 (15)	0.51624 (7)	0.0459 (3)
O2	0.36430 (8)	0.19692 (15)	0.52316 (7)	0.0449 (3)
O3	0.29757 (9)	0.34582 (15)	0.37698 (7)	0.0476 (3)
O4	0.22156 (9)	0.03783 (15)	0.42402 (7)	0.0467 (3)
O5	0.12031 (9)	0.34222 (17)	0.41210 (7)	0.0517 (3)
O6	0.18450 (8)	0.19100 (16)	0.56059 (7)	0.0456 (3)
C1	0.32393 (18)	0.7527 (3)	0.58860 (13)	0.0631 (5)
H1A	0.2958	0.8265	0.5421	0.095*
H1B	0.3876	0.7984	0.6115	0.095*
H1C	0.2821	0.7546	0.6312	0.095*
C2	0.33365 (13)	0.5644 (2)	0.55920 (9)	0.0436 (4)
C3	0.42009 (14)	0.4713 (3)	0.58034 (12)	0.0549 (4)
H3	0.4741	0.5327	0.6088	0.066*
C4	0.43123 (12)	0.2926 (2)	0.56178 (10)	0.0450 (4)
C5	0.52624 (14)	0.2009 (3)	0.59030 (15)	0.0675 (6)
H5A	0.5182	0.1154	0.6335	0.101*
H5B	0.5747	0.2885	0.6122	0.101*
H5C	0.5472	0.1394	0.5437	0.101*
C6	0.34988 (15)	0.3609 (3)	0.24651 (11)	0.0595 (5)
H6A	0.3488	0.4877	0.2581	0.089*
H6B	0.3138	0.3376	0.1916	0.089*
H6C	0.4166	0.3218	0.2484	0.089*
C7	0.30408 (11)	0.2612 (2)	0.31064 (9)	0.0415 (4)
C8	0.27354 (13)	0.0859 (2)	0.29557 (10)	0.0489 (4)
H8	0.2790	0.0356	0.2435	0.059*
C9	0.23562 (11)	−0.0183 (2)	0.35305 (9)	0.0397 (3)
C10	0.20886 (14)	−0.2097 (2)	0.33432 (12)	0.0523 (4)
H10A	0.2423	−0.2852	0.3780	0.078*
H10B	0.2278	−0.2431	0.2814	0.078*
H10C	0.1392	−0.2244	0.3314	0.078*
C11	−0.04668 (18)	0.3823 (4)	0.36881 (15)	0.0927 (9)
H11A	−0.0294	0.4930	0.3439	0.139*
H11B	−0.1032	0.4014	0.3960	0.139*
H11C	−0.0615	0.2924	0.3258	0.139*
C12	0.03733 (14)	0.3201 (3)	0.43199 (12)	0.0598 (5)
C13	0.02115 (15)	0.2413 (4)	0.50601 (14)	0.0796 (8)
H13	−0.0435	0.2261	0.5151	0.096*
C14	0.09533 (14)	0.1837 (3)	0.56725 (11)	0.0558 (5)
C15	0.07407 (18)	0.1090 (4)	0.64809 (14)	0.0859 (8)
H15A	0.1160	0.0075	0.6638	0.129*
H15B	0.0066	0.0715	0.6418	0.129*
H15C	0.0858	0.1998	0.6910	0.129*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Al1	0.0471 (3)	0.0398 (3)	0.0304 (2)	0.0051 (2)	0.00612 (19)	−0.00091 (18)
O1	0.0565 (7)	0.0417 (6)	0.0388 (6)	0.0090 (5)	0.0053 (5)	−0.0042 (5)
O2	0.0451 (6)	0.0453 (6)	0.0445 (6)	0.0088 (5)	0.0080 (5)	−0.0023 (5)
O3	0.0657 (8)	0.0435 (6)	0.0354 (6)	−0.0025 (5)	0.0139 (5)	−0.0034 (5)
O4	0.0609 (7)	0.0412 (6)	0.0382 (6)	−0.0009 (5)	0.0082 (5)	−0.0020 (5)
O5	0.0550 (7)	0.0580 (8)	0.0390 (6)	0.0097 (6)	−0.0025 (5)	0.0016 (5)
O6	0.0464 (6)	0.0559 (7)	0.0352 (6)	0.0059 (5)	0.0082 (5)	0.0031 (5)
C1	0.0938 (16)	0.0434 (10)	0.0534 (11)	−0.0048 (10)	0.0150 (11)	−0.0063 (8)
C2	0.0600 (10)	0.0414 (8)	0.0308 (7)	−0.0043 (7)	0.0113 (7)	0.0016 (6)
C3	0.0520 (10)	0.0542 (11)	0.0570 (11)	−0.0085 (8)	0.0039 (8)	−0.0028 (9)
C4	0.0406 (8)	0.0582 (10)	0.0384 (8)	0.0017 (8)	0.0127 (7)	0.0055 (7)
C5	0.0440 (10)	0.0844 (15)	0.0740 (14)	0.0123 (10)	0.0086 (9)	0.0034 (12)
C6	0.0711 (13)	0.0705 (13)	0.0392 (9)	−0.0070 (10)	0.0163 (8)	−0.0008 (9)
C7	0.0423 (8)	0.0513 (9)	0.0299 (7)	0.0076 (7)	0.0023 (6)	0.0009 (6)
C8	0.0601 (10)	0.0514 (10)	0.0352 (8)	0.0036 (8)	0.0071 (7)	−0.0087 (7)
C9	0.0361 (7)	0.0432 (8)	0.0363 (8)	0.0083 (6)	−0.0058 (6)	−0.0051 (6)
C10	0.0539 (10)	0.0456 (9)	0.0530 (10)	0.0021 (8)	−0.0058 (8)	−0.0091 (8)
C11	0.0691 (15)	0.132 (2)	0.0666 (14)	0.0285 (15)	−0.0228 (12)	−0.0108 (15)
C12	0.0506 (11)	0.0767 (13)	0.0476 (10)	0.0104 (10)	−0.0072 (8)	−0.0119 (9)
C13	0.0411 (11)	0.142 (2)	0.0548 (12)	−0.0019 (12)	0.0048 (9)	0.0001 (13)
C14	0.0500 (10)	0.0754 (13)	0.0429 (9)	−0.0076 (9)	0.0100 (8)	−0.0044 (9)
C15	0.0711 (14)	0.133 (2)	0.0571 (13)	−0.0221 (15)	0.0198 (11)	0.0116 (14)

Geometric parameters (Å, º)

Al1—O5	1.8712 (13)	C6—C7	1.502 (2)
Al1—O6	1.8779 (12)	C6—H6A	0.9700
Al1—O1	1.8834 (12)	C6—H6B	0.9700
Al1—O2	1.8838 (12)	C6—H6C	0.9700
Al1—O4	1.8844 (12)	C7—C8	1.392 (2)
Al1—O3	1.8862 (12)	C8—C9	1.383 (2)
O1—C2	1.268 (2)	C8—H8	0.9400
O2—C4	1.264 (2)	C9—C10	1.502 (2)
O3—C7	1.2667 (19)	C10—H10A	0.9700
O4—C9	1.2710 (18)	C10—H10B	0.9700
O5—C12	1.257 (2)	C10—H10C	0.9700
O6—C14	1.263 (2)	C11—C12	1.507 (3)
C1—C2	1.504 (2)	C11—H11A	0.9700
C1—H1A	0.9700	C11—H11B	0.9700
C1—H1B	0.9700	C11—H11C	0.9700
C1—H1C	0.9700	C12—C13	1.389 (3)
C2—C3	1.387 (3)	C13—C14	1.389 (3)
C3—C4	1.388 (3)	C13—H13	0.9400
C3—H3	0.9400	C14—C15	1.499 (3)
C4—C5	1.500 (2)	C15—H15A	0.9700
C5—H5A	0.9700	C15—H15B	0.9700
C5—H5B	0.9700	C15—H15C	0.9700
C5—H5C	0.9700
O5—Al1—O6	91.81 (6)	C7—C6—H6A	109.5
O5—Al1—O1	89.02 (6)	C7—C6—H6B	109.5
O6—Al1—O1	90.29 (5)	H6A—C6—H6B	109.5
O5—Al1—O2	178.00 (6)	C7—C6—H6C	109.5
O6—Al1—O2	90.18 (5)	H6A—C6—H6C	109.5
O1—Al1—O2	91.15 (5)	H6B—C6—H6C	109.5
O5—Al1—O4	90.81 (6)	O3—C7—C8	124.31 (15)
O6—Al1—O4	88.27 (5)	O3—C7—C6	115.75 (15)
O1—Al1—O4	178.55 (6)	C8—C7—C6	119.93 (15)
O2—Al1—O4	89.08 (5)	C9—C8—C7	123.56 (15)
O5—Al1—O3	88.23 (6)	C9—C8—H8	118.2
O6—Al1—O3	179.71 (6)	C7—C8—H8	118.2
O1—Al1—O3	90.00 (5)	O4—C9—C8	123.58 (15)
O2—Al1—O3	89.78 (6)	O4—C9—C10	115.65 (15)
O4—Al1—O3	91.44 (5)	C8—C9—C10	120.76 (15)
C2—O1—Al1	128.76 (11)	C9—C10—H10A	109.5
C4—O2—Al1	128.21 (11)	C9—C10—H10B	109.5
C7—O3—Al1	127.98 (11)	H10A—C10—H10B	109.5
C9—O4—Al1	128.68 (11)	C9—C10—H10C	109.5
C12—O5—Al1	128.57 (12)	H10A—C10—H10C	109.5
C14—O6—Al1	128.07 (12)	H10B—C10—H10C	109.5
C2—C1—H1A	109.5	C12—C11—H11A	109.5
C2—C1—H1B	109.5	C12—C11—H11B	109.5
H1A—C1—H1B	109.5	H11A—C11—H11B	109.5
C2—C1—H1C	109.5	C12—C11—H11C	109.5
H1A—C1—H1C	109.5	H11A—C11—H11C	109.5
H1B—C1—H1C	109.5	H11B—C11—H11C	109.5
O1—C2—C3	123.44 (15)	O5—C12—C13	123.78 (17)
O1—C2—C1	115.86 (16)	O5—C12—C11	115.5 (2)
C3—C2—C1	120.69 (17)	C13—C12—C11	120.7 (2)
C2—C3—C4	123.59 (17)	C14—C13—C12	123.49 (19)
C2—C3—H3	118.2	C14—C13—H13	118.3
C4—C3—H3	118.2	C12—C13—H13	118.3
O2—C4—C3	123.94 (16)	O6—C14—C13	123.87 (18)
O2—C4—C5	116.14 (17)	O6—C14—C15	114.81 (18)
C3—C4—C5	119.90 (18)	C13—C14—C15	121.33 (19)
C4—C5—H5A	109.5	C14—C15—H15A	109.5
C4—C5—H5B	109.5	C14—C15—H15B	109.5
H5A—C5—H5B	109.5	H15A—C15—H15B	109.5
C4—C5—H5C	109.5	C14—C15—H15C	109.5
H5A—C5—H5C	109.5	H15A—C15—H15C	109.5
H5B—C5—H5C	109.5	H15B—C15—H15C	109.5
O5—Al1—O1—C2	−171.36 (13)	Al1—O1—C2—C3	−0.9 (2)
O6—Al1—O1—C2	96.83 (13)	Al1—O1—C2—C1	−179.56 (12)
O2—Al1—O1—C2	6.65 (13)	O1—C2—C3—C4	−4.7 (3)
O3—Al1—O1—C2	−83.13 (13)	C1—C2—C3—C4	173.94 (17)
O6—Al1—O2—C4	−100.77 (14)	Al1—O2—C4—C3	8.6 (2)
O1—Al1—O2—C4	−10.47 (14)	Al1—O2—C4—C5	−173.26 (12)
O4—Al1—O2—C4	170.96 (13)	C2—C3—C4—O2	0.7 (3)
O3—Al1—O2—C4	79.52 (13)	C2—C3—C4—C5	−177.38 (17)
O5—Al1—O3—C7	−84.21 (14)	Al1—O3—C7—C8	−3.5 (2)
O1—Al1—O3—C7	−173.23 (14)	Al1—O3—C7—C6	177.59 (12)
O2—Al1—O3—C7	95.62 (14)	O3—C7—C8—C9	−2.5 (3)
O4—Al1—O3—C7	6.55 (14)	C6—C7—C8—C9	176.35 (16)
O5—Al1—O4—C9	81.93 (14)	Al1—O4—C9—C8	3.0 (2)
O6—Al1—O4—C9	173.71 (13)	Al1—O4—C9—C10	−177.42 (11)
O2—Al1—O4—C9	−96.08 (13)	C7—C8—C9—O4	2.8 (3)
O3—Al1—O4—C9	−6.32 (14)	C7—C8—C9—C10	−176.81 (16)
O6—Al1—O5—C12	−6.58 (17)	Al1—O5—C12—C13	3.8 (3)
O1—Al1—O5—C12	−96.84 (17)	Al1—O5—C12—C11	−175.12 (15)
O4—Al1—O5—C12	81.72 (16)	O5—C12—C13—C14	2.2 (4)
O3—Al1—O5—C12	173.14 (16)	C11—C12—C13—C14	−179.0 (2)
O5—Al1—O6—C14	5.97 (16)	Al1—O6—C14—C13	−2.6 (3)
O1—Al1—O6—C14	95.00 (16)	Al1—O6—C14—C15	178.10 (16)
O2—Al1—O6—C14	−173.85 (16)	C12—C13—C14—O6	−2.8 (4)
O4—Al1—O6—C14	−84.78 (16)	C12—C13—C14—C15	176.5 (2)

(Ib) Tris(pentane-2,4-dionato-κ²O,O')aluminium(III)

Crystal data

[Al(C5H7O2)3]	F(000) = 688
Mr = 324.30	Dx = 1.298 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 13500 reflections
a = 13.8640 (6) Å	θ = 2.5–27.5°
b = 7.4755 (3) Å	µ = 0.15 mm^−1
c = 16.2080 (11) Å	T = 210 K
β = 98.821 (2)°	Hexagonal prism, colourless
V = 1659.94 (15) Å^3	0.42 × 0.39 × 0.18 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	3823 independent reflections
Radiation source: rotating anode	3133 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.025
ϕ and ω scans	θmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −18→18
Tmin = 0.70, Tmax = 0.97	k = −9→9
29627 measured reflections	l = −21→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.039	Hydrogen site location: difference Fourier map
wR(F^2) = 0.114	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.057P)^2 + 0.4987P] where P = (Fo^2 + 2Fc^2)/3
3823 reflections	(Δ/σ)max < 0.001
205 parameters	Δρmax = 0.21 e Å^−3
0 restraints	Δρmin = −0.25 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Al1	0.24082 (3)	0.26895 (6)	0.46901 (3)	0.03361 (13)
O1	0.25852 (8)	0.49881 (14)	0.51632 (6)	0.0393 (3)
O2	0.36460 (8)	0.19675 (14)	0.52302 (7)	0.0385 (2)
O3	0.29746 (8)	0.34609 (14)	0.37664 (6)	0.0411 (3)
O4	0.22130 (8)	0.03729 (14)	0.42382 (6)	0.0405 (3)
O5	0.11984 (8)	0.34302 (16)	0.41203 (7)	0.0446 (3)
O6	0.18443 (8)	0.19074 (15)	0.56071 (6)	0.0389 (3)
C1	0.32446 (16)	0.7541 (2)	0.58904 (12)	0.0540 (5)
H1A	0.2960	0.8282	0.5425	0.081*
H1B	0.3884	0.8001	0.6119	0.081*
H1C	0.2827	0.7557	0.6319	0.081*
C2	0.33421 (12)	0.5652 (2)	0.55935 (9)	0.0374 (3)
C3	0.42108 (12)	0.4721 (2)	0.58041 (11)	0.0467 (4)
H3	0.4753	0.5337	0.6088	0.056*
C4	0.43200 (11)	0.2926 (2)	0.56170 (9)	0.0388 (3)
C5	0.52737 (13)	0.2005 (3)	0.59007 (13)	0.0578 (5)
H5A	0.5199	0.1169	0.6344	0.087*
H5B	0.5765	0.2887	0.6106	0.087*
H5C	0.5474	0.1363	0.5435	0.087*
C6	0.35038 (14)	0.3605 (3)	0.24593 (10)	0.0510 (4)
H6A	0.3529	0.4871	0.2593	0.077*
H6B	0.3120	0.3428	0.1913	0.077*
H6C	0.4161	0.3160	0.2457	0.077*
C7	0.30413 (10)	0.2610 (2)	0.31016 (9)	0.0355 (3)
C8	0.27340 (12)	0.0854 (2)	0.29496 (9)	0.0420 (4)
H8	0.2788	0.0350	0.2427	0.050*
C9	0.23530 (10)	−0.0191 (2)	0.35266 (9)	0.0344 (3)
C10	0.20818 (12)	−0.2108 (2)	0.33397 (11)	0.0446 (4)
H10A	0.2407	−0.2865	0.3784	0.067*
H10B	0.2283	−0.2452	0.2815	0.067*
H10C	0.1381	−0.2248	0.3300	0.067*
C11	−0.04766 (16)	0.3834 (4)	0.36890 (14)	0.0798 (7)
H11A	−0.0309	0.4962	0.3452	0.120*
H11B	−0.1048	0.3994	0.3959	0.120*
H11C	−0.0615	0.2950	0.3249	0.120*
C12	0.03655 (13)	0.3206 (3)	0.43206 (11)	0.0518 (4)
C13	0.02028 (13)	0.2410 (4)	0.50621 (13)	0.0682 (6)
H13	−0.0445	0.2257	0.5154	0.082*
C14	0.09492 (13)	0.1831 (3)	0.56746 (10)	0.0485 (4)
C15	0.07378 (16)	0.1074 (4)	0.64851 (13)	0.0731 (7)
H15A	0.1156	0.0050	0.6639	0.110*
H15B	0.0060	0.0705	0.6423	0.110*
H15C	0.0861	0.1979	0.6917	0.110*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Al1	0.0406 (2)	0.0346 (2)	0.0258 (2)	0.00459 (18)	0.00554 (17)	−0.00092 (17)
O1	0.0477 (6)	0.0362 (6)	0.0334 (5)	0.0076 (5)	0.0046 (5)	−0.0041 (4)
O2	0.0393 (6)	0.0382 (6)	0.0384 (6)	0.0073 (4)	0.0070 (4)	−0.0018 (4)
O3	0.0577 (7)	0.0369 (6)	0.0304 (5)	−0.0019 (5)	0.0119 (5)	−0.0026 (4)
O4	0.0531 (6)	0.0359 (6)	0.0328 (5)	−0.0009 (5)	0.0079 (5)	−0.0019 (4)
O5	0.0471 (6)	0.0509 (7)	0.0333 (5)	0.0081 (5)	−0.0016 (5)	0.0012 (5)
O6	0.0396 (6)	0.0482 (6)	0.0295 (5)	0.0049 (5)	0.0069 (4)	0.0023 (4)
C1	0.0806 (13)	0.0370 (9)	0.0454 (10)	−0.0033 (8)	0.0129 (9)	−0.0054 (7)
C2	0.0529 (9)	0.0353 (8)	0.0254 (7)	−0.0036 (7)	0.0109 (6)	0.0018 (6)
C3	0.0444 (9)	0.0462 (9)	0.0484 (9)	−0.0069 (7)	0.0041 (7)	−0.0025 (7)
C4	0.0347 (7)	0.0506 (9)	0.0331 (7)	0.0023 (7)	0.0112 (6)	0.0050 (6)
C5	0.0381 (9)	0.0718 (13)	0.0636 (12)	0.0103 (9)	0.0079 (8)	0.0029 (10)
C6	0.0610 (11)	0.0597 (11)	0.0346 (8)	−0.0065 (9)	0.0139 (7)	0.0004 (8)
C7	0.0351 (7)	0.0441 (8)	0.0264 (7)	0.0070 (6)	0.0019 (6)	0.0006 (6)
C8	0.0533 (9)	0.0437 (9)	0.0290 (7)	0.0033 (7)	0.0065 (6)	−0.0069 (6)
C9	0.0313 (7)	0.0372 (8)	0.0316 (7)	0.0072 (6)	−0.0053 (5)	−0.0042 (6)
C10	0.0466 (9)	0.0382 (8)	0.0452 (9)	0.0020 (7)	−0.0050 (7)	−0.0070 (7)
C11	0.0586 (13)	0.113 (2)	0.0592 (13)	0.0257 (13)	−0.0195 (10)	−0.0090 (13)
C12	0.0449 (9)	0.0649 (12)	0.0415 (9)	0.0095 (8)	−0.0068 (7)	−0.0112 (8)
C13	0.0359 (9)	0.119 (2)	0.0485 (10)	−0.0013 (11)	0.0041 (8)	−0.0002 (11)
C14	0.0442 (9)	0.0643 (11)	0.0378 (8)	−0.0060 (8)	0.0091 (7)	−0.0037 (8)
C15	0.0610 (12)	0.1118 (19)	0.0491 (11)	−0.0179 (12)	0.0162 (9)	0.0115 (12)

Geometric parameters (Å, º)

Al1—O5	1.8702 (12)	C6—C7	1.501 (2)
Al1—O6	1.8756 (11)	C6—H6A	0.9700
Al1—O2	1.8820 (11)	C6—H6B	0.9700
Al1—O1	1.8823 (11)	C6—H6C	0.9700
Al1—O4	1.8836 (11)	C7—C8	1.391 (2)
Al1—O3	1.8845 (11)	C8—C9	1.384 (2)
O1—C2	1.2684 (19)	C8—H8	0.9400
O2—C4	1.2650 (19)	C9—C10	1.501 (2)
O3—C7	1.2667 (17)	C10—H10A	0.9700
O4—C9	1.2706 (17)	C10—H10B	0.9700
O5—C12	1.258 (2)	C10—H10C	0.9700
O6—C14	1.2637 (19)	C11—C12	1.505 (2)
C1—C2	1.505 (2)	C11—H11A	0.9700
C1—H1A	0.9700	C11—H11B	0.9700
C1—H1B	0.9700	C11—H11C	0.9700
C1—H1C	0.9700	C12—C13	1.390 (3)
C2—C3	1.387 (2)	C13—C14	1.389 (3)
C3—C4	1.389 (2)	C13—H13	0.9400
C3—H3	0.9400	C14—C15	1.500 (3)
C4—C5	1.499 (2)	C15—H15A	0.9700
C5—H5A	0.9700	C15—H15B	0.9700
C5—H5B	0.9700	C15—H15C	0.9700
C5—H5C	0.9700
O5—Al1—O6	91.86 (5)	C7—C6—H6A	109.5
O5—Al1—O2	177.96 (5)	C7—C6—H6B	109.5
O6—Al1—O2	90.18 (5)	H6A—C6—H6B	109.5
O5—Al1—O1	88.97 (5)	C7—C6—H6C	109.5
O6—Al1—O1	90.34 (5)	H6A—C6—H6C	109.5
O2—Al1—O1	91.13 (5)	H6B—C6—H6C	109.5
O5—Al1—O4	90.90 (5)	O3—C7—C8	124.36 (14)
O6—Al1—O4	88.23 (5)	O3—C7—C6	115.84 (14)
O2—Al1—O4	89.06 (5)	C8—C7—C6	119.79 (14)
O1—Al1—O4	178.56 (5)	C9—C8—C7	123.47 (14)
O5—Al1—O3	88.20 (5)	C9—C8—H8	118.3
O6—Al1—O3	179.65 (5)	C7—C8—H8	118.3
O2—Al1—O3	89.76 (5)	O4—C9—C8	123.60 (14)
O1—Al1—O3	90.00 (5)	O4—C9—C10	115.58 (14)
O4—Al1—O3	91.43 (5)	C8—C9—C10	120.82 (14)
C2—O1—Al1	128.77 (10)	C9—C10—H10A	109.5
C4—O2—Al1	128.29 (10)	C9—C10—H10B	109.5
C7—O3—Al1	128.01 (10)	H10A—C10—H10B	109.5
C9—O4—Al1	128.70 (10)	C9—C10—H10C	109.5
C12—O5—Al1	128.49 (11)	H10A—C10—H10C	109.5
C14—O6—Al1	128.08 (11)	H10B—C10—H10C	109.5
C2—C1—H1A	109.5	C12—C11—H11A	109.5
C2—C1—H1B	109.5	C12—C11—H11B	109.5
H1A—C1—H1B	109.5	H11A—C11—H11B	109.5
C2—C1—H1C	109.5	C12—C11—H11C	109.5
H1A—C1—H1C	109.5	H11A—C11—H11C	109.5
H1B—C1—H1C	109.5	H11B—C11—H11C	109.5
O1—C2—C3	123.57 (14)	O5—C12—C13	123.88 (16)
O1—C2—C1	115.82 (15)	O5—C12—C11	115.46 (18)
C3—C2—C1	120.60 (15)	C13—C12—C11	120.65 (19)
C2—C3—C4	123.38 (15)	C14—C13—C12	123.33 (17)
C2—C3—H3	118.3	C14—C13—H13	118.3
C4—C3—H3	118.3	C12—C13—H13	118.3
O2—C4—C3	123.95 (15)	O6—C14—C13	123.91 (16)
O2—C4—C5	116.20 (15)	O6—C14—C15	114.79 (16)
C3—C4—C5	119.82 (16)	C13—C14—C15	121.29 (17)
C4—C5—H5A	109.5	C14—C15—H15A	109.5
C4—C5—H5B	109.5	C14—C15—H15B	109.5
H5A—C5—H5B	109.5	H15A—C15—H15B	109.5
C4—C5—H5C	109.5	C14—C15—H15C	109.5
H5A—C5—H5C	109.5	H15A—C15—H15C	109.5
H5B—C5—H5C	109.5	H15B—C15—H15C	109.5
O5—Al1—O1—C2	−171.33 (12)	Al1—O1—C2—C3	−0.8 (2)
O6—Al1—O1—C2	96.82 (12)	Al1—O1—C2—C1	−179.44 (11)
O2—Al1—O1—C2	6.63 (12)	O1—C2—C3—C4	−4.8 (3)
O3—Al1—O1—C2	−83.13 (12)	C1—C2—C3—C4	173.78 (15)
O6—Al1—O2—C4	−100.86 (13)	Al1—O2—C4—C3	8.6 (2)
O1—Al1—O2—C4	−10.51 (13)	Al1—O2—C4—C5	−173.19 (11)
O4—Al1—O2—C4	170.92 (12)	C2—C3—C4—O2	0.8 (3)
O3—Al1—O2—C4	79.49 (12)	C2—C3—C4—C5	−177.37 (16)
O5—Al1—O3—C7	−84.52 (13)	Al1—O3—C7—C8	−3.2 (2)
O2—Al1—O3—C7	95.39 (13)	Al1—O3—C7—C6	177.93 (11)
O1—Al1—O3—C7	−173.49 (13)	O3—C7—C8—C9	−2.7 (2)
O4—Al1—O3—C7	6.33 (13)	C6—C7—C8—C9	176.15 (15)
O5—Al1—O4—C9	81.93 (13)	Al1—O4—C9—C8	3.1 (2)
O6—Al1—O4—C9	173.76 (12)	Al1—O4—C9—C10	−177.31 (10)
O2—Al1—O4—C9	−96.03 (12)	C7—C8—C9—O4	2.7 (2)
O3—Al1—O4—C9	−6.29 (13)	C7—C8—C9—C10	−176.87 (14)
O6—Al1—O5—C12	−6.70 (15)	Al1—O5—C12—C13	3.8 (3)
O1—Al1—O5—C12	−97.00 (15)	Al1—O5—C12—C11	−175.12 (14)
O4—Al1—O5—C12	81.56 (15)	O5—C12—C13—C14	2.2 (4)
O3—Al1—O5—C12	172.96 (15)	C11—C12—C13—C14	−178.9 (2)
O5—Al1—O6—C14	6.19 (15)	Al1—O6—C14—C13	−2.8 (3)
O2—Al1—O6—C14	−173.71 (15)	Al1—O6—C14—C15	177.90 (14)
O1—Al1—O6—C14	95.17 (15)	C12—C13—C14—O6	−2.7 (4)
O4—Al1—O6—C14	−84.65 (15)	C12—C13—C14—C15	176.5 (2)

(Ic) Tris(pentane-2,4-dionato-κ²O,O')aluminium(III)

Crystal data

[Al(C5H7O2)3]	F(000) = 688
Mr = 324.30	Dx = 1.304 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 14128 reflections
a = 13.8385 (7) Å	θ = 2.7–27.5°
b = 7.4614 (3) Å	µ = 0.15 mm^−1
c = 16.1873 (11) Å	T = 180 K
β = 98.871 (2)°	Hexagonal prism, colourless
V = 1651.42 (16) Å^3	0.42 × 0.39 × 0.18 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	3801 independent reflections
Radiation source: rotating anode	3201 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.023
ϕ and ω scans	θmax = 27.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −17→17
Tmin = 0.73, Tmax = 0.97	k = −9→9
29482 measured reflections	l = −21→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.037	Hydrogen site location: difference Fourier map
wR(F^2) = 0.103	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0496P)^2 + 0.5412P] where P = (Fo^2 + 2Fc^2)/3
3801 reflections	(Δ/σ)max < 0.001
205 parameters	Δρmax = 0.22 e Å^−3
0 restraints	Δρmin = −0.25 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Al1	0.24071 (3)	0.26924 (6)	0.46892 (2)	0.02861 (12)
O1	0.25861 (7)	0.49954 (13)	0.51639 (6)	0.0336 (2)
O2	0.36499 (7)	0.19656 (13)	0.52284 (6)	0.0329 (2)
O3	0.29746 (8)	0.34657 (13)	0.37634 (6)	0.0351 (2)
O4	0.22093 (7)	0.03714 (13)	0.42360 (6)	0.0347 (2)
O5	0.11932 (8)	0.34385 (15)	0.41200 (6)	0.0382 (2)
O6	0.18445 (7)	0.19053 (14)	0.56086 (6)	0.0332 (2)
C1	0.32520 (14)	0.7553 (2)	0.58923 (10)	0.0449 (4)
H1A	0.2959	0.8302	0.5422	0.067*
H1B	0.3901	0.8020	0.6119	0.067*
H1C	0.2834	0.7570	0.6329	0.067*
C2	0.33473 (11)	0.56592 (19)	0.55951 (8)	0.0319 (3)
C3	0.42193 (11)	0.4728 (2)	0.58047 (10)	0.0395 (3)
H3	0.4769	0.5352	0.6092	0.047*
C4	0.43290 (10)	0.2928 (2)	0.56149 (9)	0.0329 (3)
C5	0.52847 (12)	0.2003 (3)	0.58965 (12)	0.0490 (4)
H5A	0.5213	0.1171	0.6352	0.074*
H5B	0.5786	0.2897	0.6095	0.074*
H5C	0.5480	0.1336	0.5427	0.074*
C6	0.35076 (12)	0.3604 (2)	0.24538 (9)	0.0427 (4)
H6A	0.3561	0.4877	0.2601	0.064*
H6B	0.3104	0.3466	0.1904	0.064*
H6C	0.4161	0.3114	0.2436	0.064*
C7	0.30423 (10)	0.26115 (19)	0.30970 (8)	0.0298 (3)
C8	0.27325 (11)	0.0849 (2)	0.29431 (9)	0.0357 (3)
H8	0.2787	0.0338	0.2415	0.043*
C9	0.23492 (9)	−0.01968 (18)	0.35221 (8)	0.0292 (3)
C10	0.20772 (11)	−0.2121 (2)	0.33363 (10)	0.0377 (3)
H10A	0.2408	−0.2885	0.3786	0.057*
H10B	0.2279	−0.2470	0.2805	0.057*
H10C	0.1368	−0.2262	0.3297	0.057*
C11	−0.04869 (14)	0.3845 (3)	0.36913 (12)	0.0671 (6)
H11A	−0.0319	0.4994	0.3457	0.101*
H11B	−0.1067	0.3995	0.3964	0.101*
H11C	−0.0624	0.2958	0.3242	0.101*
C12	0.03572 (12)	0.3210 (2)	0.43236 (10)	0.0437 (4)
C13	0.01938 (12)	0.2409 (3)	0.50653 (11)	0.0573 (5)
H13	−0.0462	0.2256	0.5159	0.069*
C14	0.09463 (11)	0.1821 (2)	0.56770 (9)	0.0403 (4)
C15	0.07355 (14)	0.1057 (3)	0.64881 (11)	0.0608 (5)
H15A	0.1163	0.0025	0.6644	0.091*
H15B	0.0051	0.0675	0.6424	0.091*
H15C	0.0855	0.1974	0.6926	0.091*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Al1	0.0346 (2)	0.0294 (2)	0.02197 (19)	0.00400 (16)	0.00491 (15)	−0.00063 (15)
O1	0.0407 (5)	0.0311 (5)	0.0286 (5)	0.0067 (4)	0.0040 (4)	−0.0036 (4)
O2	0.0330 (5)	0.0330 (5)	0.0330 (5)	0.0060 (4)	0.0065 (4)	−0.0019 (4)
O3	0.0492 (6)	0.0314 (5)	0.0263 (5)	−0.0017 (4)	0.0107 (4)	−0.0023 (4)
O4	0.0459 (6)	0.0307 (5)	0.0277 (5)	−0.0012 (4)	0.0067 (4)	−0.0014 (4)
O5	0.0404 (6)	0.0436 (6)	0.0285 (5)	0.0063 (5)	−0.0014 (4)	0.0016 (4)
O6	0.0334 (5)	0.0413 (6)	0.0251 (5)	0.0049 (4)	0.0055 (4)	0.0022 (4)
C1	0.0659 (11)	0.0318 (8)	0.0380 (8)	−0.0029 (7)	0.0108 (8)	−0.0046 (6)
C2	0.0449 (8)	0.0308 (7)	0.0216 (6)	−0.0033 (6)	0.0098 (5)	0.0011 (5)
C3	0.0373 (8)	0.0401 (8)	0.0405 (8)	−0.0056 (6)	0.0041 (6)	−0.0021 (7)
C4	0.0298 (7)	0.0427 (8)	0.0280 (6)	0.0024 (6)	0.0099 (5)	0.0039 (6)
C5	0.0324 (8)	0.0608 (11)	0.0539 (10)	0.0094 (7)	0.0066 (7)	0.0020 (8)
C6	0.0505 (9)	0.0503 (10)	0.0291 (7)	−0.0046 (7)	0.0116 (6)	0.0005 (7)
C7	0.0292 (6)	0.0368 (7)	0.0224 (6)	0.0057 (5)	0.0011 (5)	0.0010 (5)
C8	0.0443 (8)	0.0381 (8)	0.0245 (6)	0.0026 (6)	0.0049 (6)	−0.0062 (6)
C9	0.0262 (6)	0.0318 (7)	0.0269 (6)	0.0067 (5)	−0.0045 (5)	−0.0032 (5)
C10	0.0397 (8)	0.0327 (7)	0.0375 (8)	0.0013 (6)	−0.0040 (6)	−0.0052 (6)
C11	0.0502 (11)	0.0943 (17)	0.0492 (10)	0.0222 (11)	−0.0161 (8)	−0.0066 (11)
C12	0.0382 (8)	0.0546 (10)	0.0347 (8)	0.0084 (7)	−0.0061 (6)	−0.0097 (7)
C13	0.0308 (8)	0.0986 (16)	0.0418 (9)	0.0000 (9)	0.0035 (7)	0.0003 (10)
C14	0.0376 (8)	0.0517 (9)	0.0322 (7)	−0.0037 (7)	0.0073 (6)	−0.0028 (7)
C15	0.0509 (10)	0.0916 (15)	0.0420 (9)	−0.0135 (10)	0.0136 (8)	0.0100 (10)

Geometric parameters (Å, º)

Al1—O5	1.8718 (11)	C6—C7	1.501 (2)
Al1—O6	1.8770 (10)	C6—H6A	0.9800
Al1—O1	1.8831 (11)	C6—H6B	0.9800
Al1—O4	1.8842 (11)	C6—H6C	0.9800
Al1—O2	1.8843 (10)	C7—C8	1.394 (2)
Al1—O3	1.8864 (10)	C8—C9	1.386 (2)
O1—C2	1.2709 (17)	C8—H8	0.9500
O2—C4	1.2684 (18)	C9—C10	1.502 (2)
O3—C7	1.2688 (16)	C10—H10A	0.9800
O4—C9	1.2734 (16)	C10—H10B	0.9800
O5—C12	1.262 (2)	C10—H10C	0.9800
O6—C14	1.2664 (18)	C11—C12	1.506 (2)
C1—C2	1.505 (2)	C11—H11A	0.9800
C1—H1A	0.9800	C11—H11B	0.9800
C1—H1B	0.9800	C11—H11C	0.9800
C1—H1C	0.9800	C12—C13	1.390 (3)
C2—C3	1.388 (2)	C13—C14	1.393 (2)
C3—C4	1.391 (2)	C13—H13	0.9500
C3—H3	0.9500	C14—C15	1.501 (2)
C4—C5	1.499 (2)	C15—H15A	0.9800
C5—H5A	0.9800	C15—H15B	0.9800
C5—H5B	0.9800	C15—H15C	0.9800
C5—H5C	0.9800
O5—Al1—O6	91.88 (5)	C7—C6—H6A	109.5
O5—Al1—O1	88.91 (5)	C7—C6—H6B	109.5
O6—Al1—O1	90.37 (5)	H6A—C6—H6B	109.5
O5—Al1—O4	90.93 (5)	C7—C6—H6C	109.5
O6—Al1—O4	88.17 (5)	H6A—C6—H6C	109.5
O1—Al1—O4	178.53 (5)	H6B—C6—H6C	109.5
O5—Al1—O2	177.93 (5)	O3—C7—C8	124.40 (13)
O6—Al1—O2	90.18 (5)	O3—C7—C6	115.97 (13)
O1—Al1—O2	91.17 (5)	C8—C7—C6	119.62 (13)
O4—Al1—O2	89.04 (5)	C9—C8—C7	123.33 (13)
O5—Al1—O3	88.28 (5)	C9—C8—H8	118.3
O6—Al1—O3	179.58 (5)	C7—C8—H8	118.3
O1—Al1—O3	90.02 (5)	O4—C9—C8	123.62 (13)
O4—Al1—O3	91.44 (4)	O4—C9—C10	115.55 (13)
O2—Al1—O3	89.66 (5)	C8—C9—C10	120.83 (13)
C2—O1—Al1	128.71 (9)	C9—C10—H10A	109.5
C4—O2—Al1	128.28 (10)	C9—C10—H10B	109.5
C7—O3—Al1	128.03 (10)	H10A—C10—H10B	109.5
C9—O4—Al1	128.76 (9)	C9—C10—H10C	109.5
C12—O5—Al1	128.35 (10)	H10A—C10—H10C	109.5
C14—O6—Al1	128.14 (10)	H10B—C10—H10C	109.5
C2—C1—H1A	109.5	C12—C11—H11A	109.5
C2—C1—H1B	109.5	C12—C11—H11B	109.5
H1A—C1—H1B	109.5	H11A—C11—H11B	109.5
C2—C1—H1C	109.5	C12—C11—H11C	109.5
H1A—C1—H1C	109.5	H11A—C11—H11C	109.5
H1B—C1—H1C	109.5	H11B—C11—H11C	109.5
O1—C2—C3	123.69 (13)	O5—C12—C13	124.12 (14)
O1—C2—C1	115.81 (13)	O5—C12—C11	115.23 (16)
C3—C2—C1	120.49 (14)	C13—C12—C11	120.64 (17)
C2—C3—C4	123.33 (14)	C12—C13—C14	123.10 (16)
C2—C3—H3	118.3	C12—C13—H13	118.5
C4—C3—H3	118.3	C14—C13—H13	118.5
O2—C4—C3	123.89 (13)	O6—C14—C13	123.96 (15)
O2—C4—C5	116.18 (14)	O6—C14—C15	114.92 (14)
C3—C4—C5	119.90 (14)	C13—C14—C15	121.11 (15)
C4—C5—H5A	109.5	C14—C15—H15A	109.5
C4—C5—H5B	109.5	C14—C15—H15B	109.5
H5A—C5—H5B	109.5	H15A—C15—H15B	109.5
C4—C5—H5C	109.5	C14—C15—H15C	109.5
H5A—C5—H5C	109.5	H15A—C15—H15C	109.5
H5B—C5—H5C	109.5	H15B—C15—H15C	109.5
O5—Al1—O1—C2	−171.32 (11)	Al1—O1—C2—C3	−0.7 (2)
O6—Al1—O1—C2	96.80 (11)	Al1—O1—C2—C1	−179.55 (10)
O2—Al1—O1—C2	6.61 (11)	O1—C2—C3—C4	−4.8 (2)
O3—Al1—O1—C2	−83.04 (11)	C1—C2—C3—C4	174.02 (14)
O6—Al1—O2—C4	−101.05 (12)	Al1—O2—C4—C3	8.9 (2)
O1—Al1—O2—C4	−10.67 (12)	Al1—O2—C4—C5	−173.12 (10)
O4—Al1—O2—C4	170.78 (11)	C2—C3—C4—O2	0.5 (2)
O3—Al1—O2—C4	79.34 (11)	C2—C3—C4—C5	−177.38 (14)
O5—Al1—O3—C7	−84.73 (12)	Al1—O3—C7—C8	−3.0 (2)
O1—Al1—O3—C7	−173.64 (12)	Al1—O3—C7—C6	178.11 (10)
O4—Al1—O3—C7	6.15 (12)	O3—C7—C8—C9	−2.7 (2)
O2—Al1—O3—C7	95.19 (12)	C6—C7—C8—C9	176.09 (13)
O5—Al1—O4—C9	82.09 (12)	Al1—O4—C9—C8	3.04 (19)
O6—Al1—O4—C9	173.95 (11)	Al1—O4—C9—C10	−177.46 (9)
O2—Al1—O4—C9	−95.84 (12)	C7—C8—C9—O4	2.7 (2)
O3—Al1—O4—C9	−6.21 (12)	C7—C8—C9—C10	−176.74 (13)
O6—Al1—O5—C12	−6.74 (14)	Al1—O5—C12—C13	3.8 (3)
O1—Al1—O5—C12	−97.07 (14)	Al1—O5—C12—C11	−175.14 (12)
O4—Al1—O5—C12	81.46 (14)	O5—C12—C13—C14	2.1 (3)
O3—Al1—O5—C12	172.87 (14)	C11—C12—C13—C14	−179.06 (18)
O5—Al1—O6—C14	6.53 (14)	Al1—O6—C14—C13	−3.4 (3)
O1—Al1—O6—C14	95.45 (13)	Al1—O6—C14—C15	177.73 (12)
O4—Al1—O6—C14	−84.34 (13)	C12—C13—C14—O6	−2.2 (3)
O2—Al1—O6—C14	−173.38 (13)	C12—C13—C14—C15	176.56 (19)

(Id) Tris(pentane-2,4-dionato-κ²O,O')aluminium(III)

Crystal data

[Al(C5H7O2)3]	F(000) = 688
Mr = 324.30	Dx = 1.315 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 15180 reflections
a = 13.7961 (5) Å	θ = 2.7–27.5°
b = 7.44012 (17) Å	µ = 0.15 mm^−1
c = 16.1488 (5) Å	T = 150 K
β = 98.914 (3)°	Hexagonal prism, colourless
V = 1637.57 (9) Å^3	0.42 × 0.39 × 0.18 mm
Z = 4

Data collection

Nonius KappaCCD diffractometer	3771 independent reflections
Radiation source: rotating anode	3248 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.023
ϕ and ω scans	θmax = 27.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −17→17
Tmin = 0.74, Tmax = 0.98	k = −9→9
29260 measured reflections	l = −20→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: difference Fourier map
wR(F^2) = 0.094	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0455P)^2 + 0.6404P] where P = (Fo^2 + 2Fc^2)/3
3771 reflections	(Δ/σ)max < 0.001
205 parameters	Δρmax = 0.26 e Å^−3
0 restraints	Δρmin = −0.26 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Al1	0.24065 (3)	0.26972 (5)	0.46881 (2)	0.02358 (11)
O1	0.25881 (7)	0.50063 (12)	0.51643 (5)	0.0276 (2)
O2	0.36545 (6)	0.19660 (12)	0.52262 (6)	0.0273 (2)
O3	0.29744 (7)	0.34722 (12)	0.37594 (5)	0.0291 (2)
O4	0.22046 (7)	0.03713 (12)	0.42335 (5)	0.0288 (2)
O5	0.11878 (7)	0.34509 (13)	0.41201 (6)	0.0316 (2)
O6	0.18457 (7)	0.19064 (13)	0.56095 (5)	0.0273 (2)
C1	0.32596 (12)	0.75682 (19)	0.58974 (9)	0.0369 (3)
H1A	0.2977	0.8327	0.5425	0.055*
H1B	0.3910	0.8027	0.6134	0.055*
H1C	0.2832	0.7587	0.6328	0.055*
C2	0.33535 (10)	0.56719 (17)	0.55974 (7)	0.0262 (3)
C3	0.42302 (10)	0.4740 (2)	0.58064 (9)	0.0325 (3)
H3	0.4783	0.5364	0.6094	0.039*
C4	0.43368 (9)	0.29314 (19)	0.56141 (8)	0.0274 (3)
C5	0.52971 (11)	0.2004 (2)	0.58929 (10)	0.0403 (3)
H5A	0.5228	0.1168	0.6349	0.060*
H5B	0.5800	0.2900	0.6091	0.060*
H5C	0.5490	0.1338	0.5421	0.060*
C6	0.35147 (11)	0.3602 (2)	0.24476 (8)	0.0345 (3)
H6A	0.3577	0.4878	0.2597	0.052*
H6B	0.3108	0.3474	0.1897	0.052*
H6C	0.4167	0.3097	0.2428	0.052*
C7	0.30435 (9)	0.26160 (18)	0.30919 (7)	0.0245 (3)
C8	0.27311 (10)	0.08460 (19)	0.29371 (8)	0.0293 (3)
H8	0.2785	0.0333	0.2407	0.035*
C9	0.23456 (9)	−0.02008 (17)	0.35182 (7)	0.0238 (3)
C10	0.20720 (10)	−0.21297 (18)	0.33328 (9)	0.0306 (3)
H10A	0.2389	−0.2892	0.3791	0.046*
H10B	0.2290	−0.2492	0.2808	0.046*
H10C	0.1358	−0.2264	0.3278	0.046*
C11	−0.04996 (13)	0.3857 (3)	0.36939 (11)	0.0537 (5)
H11A	−0.0330	0.5006	0.3456	0.081*
H11B	−0.1079	0.4015	0.3970	0.081*
H11C	−0.0642	0.2965	0.3245	0.081*
C12	0.03487 (11)	0.3217 (2)	0.43253 (9)	0.0353 (3)
C13	0.01861 (11)	0.2406 (3)	0.50675 (10)	0.0453 (4)
H13	−0.0471	0.2249	0.5162	0.054*
C14	0.09429 (10)	0.1815 (2)	0.56779 (8)	0.0328 (3)
C15	0.07335 (13)	0.1039 (3)	0.64897 (10)	0.0489 (4)
H15A	0.1166	0.0008	0.6645	0.073*
H15B	0.0048	0.0647	0.6424	0.073*
H15C	0.0850	0.1955	0.6930	0.073*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Al1	0.0284 (2)	0.0244 (2)	0.01814 (18)	0.00330 (15)	0.00413 (14)	−0.00063 (14)
O1	0.0335 (5)	0.0262 (5)	0.0228 (4)	0.0054 (4)	0.0036 (4)	−0.0026 (4)
O2	0.0274 (5)	0.0272 (5)	0.0276 (5)	0.0047 (4)	0.0054 (4)	−0.0015 (4)
O3	0.0410 (5)	0.0257 (5)	0.0219 (4)	−0.0012 (4)	0.0091 (4)	−0.0021 (4)
O4	0.0383 (5)	0.0258 (5)	0.0227 (4)	−0.0009 (4)	0.0057 (4)	−0.0013 (4)
O5	0.0338 (5)	0.0360 (5)	0.0232 (4)	0.0050 (4)	−0.0007 (4)	0.0015 (4)
O6	0.0273 (4)	0.0341 (5)	0.0207 (4)	0.0041 (4)	0.0048 (3)	0.0018 (4)
C1	0.0537 (9)	0.0259 (7)	0.0318 (7)	−0.0019 (6)	0.0091 (6)	−0.0035 (6)
C2	0.0370 (7)	0.0253 (6)	0.0178 (5)	−0.0021 (5)	0.0085 (5)	0.0008 (5)
C3	0.0305 (7)	0.0336 (7)	0.0330 (7)	−0.0041 (6)	0.0031 (5)	−0.0016 (6)
C4	0.0254 (6)	0.0360 (7)	0.0223 (6)	0.0018 (5)	0.0085 (5)	0.0039 (5)
C5	0.0278 (7)	0.0495 (9)	0.0435 (8)	0.0079 (6)	0.0058 (6)	0.0013 (7)
C6	0.0405 (8)	0.0402 (8)	0.0237 (6)	−0.0038 (6)	0.0083 (5)	0.0011 (6)
C7	0.0240 (6)	0.0305 (7)	0.0182 (5)	0.0051 (5)	0.0006 (4)	0.0013 (5)
C8	0.0366 (7)	0.0310 (7)	0.0204 (6)	0.0016 (5)	0.0047 (5)	−0.0051 (5)
C9	0.0213 (6)	0.0258 (6)	0.0220 (6)	0.0054 (5)	−0.0034 (4)	−0.0020 (5)
C10	0.0321 (7)	0.0270 (7)	0.0302 (7)	0.0008 (5)	−0.0028 (5)	−0.0046 (5)
C11	0.0415 (9)	0.0727 (13)	0.0409 (9)	0.0173 (9)	−0.0131 (7)	−0.0053 (9)
C12	0.0320 (7)	0.0414 (8)	0.0294 (7)	0.0067 (6)	−0.0045 (6)	−0.0075 (6)
C13	0.0252 (7)	0.0752 (12)	0.0350 (8)	0.0006 (7)	0.0031 (6)	0.0003 (8)
C14	0.0317 (7)	0.0406 (8)	0.0264 (6)	−0.0030 (6)	0.0057 (5)	−0.0020 (6)
C15	0.0421 (9)	0.0711 (12)	0.0352 (8)	−0.0107 (8)	0.0110 (7)	0.0079 (8)

Geometric parameters (Å, º)

Al1—O5	1.8721 (10)	C6—C7	1.5008 (18)
Al1—O6	1.8750 (9)	C6—H6A	0.9800
Al1—O1	1.8830 (10)	C6—H6B	0.9800
Al1—O4	1.8836 (10)	C6—H6C	0.9800
Al1—O2	1.8846 (10)	C7—C8	1.3961 (19)
Al1—O3	1.8867 (10)	C8—C9	1.3874 (18)
O1—C2	1.2730 (16)	C8—H8	0.9500
O2—C4	1.2694 (16)	C9—C10	1.5022 (18)
O3—C7	1.2683 (15)	C10—H10A	0.9800
O4—C9	1.2740 (15)	C10—H10B	0.9800
O5—C12	1.2645 (18)	C10—H10C	0.9800
O6—C14	1.2691 (16)	C11—C12	1.505 (2)
C1—C2	1.5038 (18)	C11—H11A	0.9800
C1—H1A	0.9800	C11—H11B	0.9800
C1—H1B	0.9800	C11—H11C	0.9800
C1—H1C	0.9800	C12—C13	1.391 (2)
C2—C3	1.3898 (19)	C13—C14	1.392 (2)
C3—C4	1.394 (2)	C13—H13	0.9500
C3—H3	0.9500	C14—C15	1.501 (2)
C4—C5	1.4997 (19)	C15—H15A	0.9800
C5—H5A	0.9800	C15—H15B	0.9800
C5—H5B	0.9800	C15—H15C	0.9800
C5—H5C	0.9800
O5—Al1—O6	91.89 (4)	C7—C6—H6A	109.5
O5—Al1—O1	88.82 (4)	C7—C6—H6B	109.5
O6—Al1—O1	90.42 (4)	H6A—C6—H6B	109.5
O5—Al1—O4	90.97 (5)	C7—C6—H6C	109.5
O6—Al1—O4	88.09 (4)	H6A—C6—H6C	109.5
O1—Al1—O4	178.49 (4)	H6B—C6—H6C	109.5
O5—Al1—O2	177.91 (5)	O3—C7—C8	124.35 (12)
O6—Al1—O2	90.19 (4)	O3—C7—C6	116.19 (12)
O1—Al1—O2	91.20 (4)	C8—C7—C6	119.45 (11)
O4—Al1—O2	89.08 (4)	C9—C8—C7	123.26 (12)
O5—Al1—O3	88.34 (4)	C9—C8—H8	118.4
O6—Al1—O3	179.50 (5)	C7—C8—H8	118.4
O1—Al1—O3	90.03 (4)	O4—C9—C8	123.65 (12)
O4—Al1—O3	91.46 (4)	O4—C9—C10	115.52 (12)
O2—Al1—O3	89.57 (4)	C8—C9—C10	120.82 (12)
C2—O1—Al1	128.74 (9)	C9—C10—H10A	109.5
C4—O2—Al1	128.23 (9)	C9—C10—H10B	109.5
C7—O3—Al1	128.12 (9)	H10A—C10—H10B	109.5
C9—O4—Al1	128.77 (9)	C9—C10—H10C	109.5
C12—O5—Al1	128.28 (9)	H10A—C10—H10C	109.5
C14—O6—Al1	128.10 (9)	H10B—C10—H10C	109.5
C2—C1—H1A	109.5	C12—C11—H11A	109.5
C2—C1—H1B	109.5	C12—C11—H11B	109.5
H1A—C1—H1B	109.5	H11A—C11—H11B	109.5
C2—C1—H1C	109.5	C12—C11—H11C	109.5
H1A—C1—H1C	109.5	H11A—C11—H11C	109.5
H1B—C1—H1C	109.5	H11B—C11—H11C	109.5
O1—C2—C3	123.77 (12)	O5—C12—C13	124.19 (13)
O1—C2—C1	115.88 (12)	O5—C12—C11	115.22 (14)
C3—C2—C1	120.33 (13)	C13—C12—C11	120.57 (15)
C2—C3—C4	123.06 (13)	C12—C13—C14	122.96 (14)
C2—C3—H3	118.5	C12—C13—H13	118.5
C4—C3—H3	118.5	C14—C13—H13	118.5
O2—C4—C3	124.08 (12)	O6—C14—C13	124.07 (13)
O2—C4—C5	116.16 (13)	O6—C14—C15	114.89 (13)
C3—C4—C5	119.74 (13)	C13—C14—C15	121.03 (14)
C4—C5—H5A	109.5	C14—C15—H15A	109.5
C4—C5—H5B	109.5	C14—C15—H15B	109.5
H5A—C5—H5B	109.5	H15A—C15—H15B	109.5
C4—C5—H5C	109.5	C14—C15—H15C	109.5
H5A—C5—H5C	109.5	H15A—C15—H15C	109.5
H5B—C5—H5C	109.5	H15B—C15—H15C	109.5
O5—Al1—O1—C2	−171.44 (10)	Al1—O1—C2—C3	−0.50 (18)
O6—Al1—O1—C2	96.67 (10)	Al1—O1—C2—C1	−179.40 (9)
O2—Al1—O1—C2	6.47 (11)	O1—C2—C3—C4	−4.9 (2)
O3—Al1—O1—C2	−83.11 (10)	C1—C2—C3—C4	173.93 (12)
O6—Al1—O2—C4	−100.98 (11)	Al1—O2—C4—C3	8.77 (18)
O1—Al1—O2—C4	−10.55 (11)	Al1—O2—C4—C5	−173.02 (9)
O4—Al1—O2—C4	170.93 (10)	C2—C3—C4—O2	0.7 (2)
O3—Al1—O2—C4	79.47 (11)	C2—C3—C4—C5	−177.50 (13)
O5—Al1—O3—C7	−85.05 (11)	Al1—O3—C7—C8	−2.74 (18)
O1—Al1—O3—C7	−173.86 (11)	Al1—O3—C7—C6	178.53 (9)
O4—Al1—O3—C7	5.88 (11)	O3—C7—C8—C9	−2.9 (2)
O2—Al1—O3—C7	94.94 (11)	C6—C7—C8—C9	175.82 (12)
O5—Al1—O4—C9	82.41 (11)	Al1—O4—C9—C8	2.83 (18)
O6—Al1—O4—C9	174.27 (11)	Al1—O4—C9—C10	−177.63 (8)
O2—Al1—O4—C9	−95.51 (11)	C7—C8—C9—O4	2.8 (2)
O3—Al1—O4—C9	−5.96 (11)	C7—C8—C9—C10	−176.68 (12)
O6—Al1—O5—C12	−6.99 (12)	Al1—O5—C12—C13	3.9 (2)
O1—Al1—O5—C12	−97.38 (12)	Al1—O5—C12—C11	−175.07 (11)
O4—Al1—O5—C12	81.13 (12)	O5—C12—C13—C14	2.1 (3)
O3—Al1—O5—C12	172.56 (12)	C11—C12—C13—C14	−179.00 (16)
O5—Al1—O6—C14	6.92 (12)	Al1—O6—C14—C13	−3.8 (2)
O1—Al1—O6—C14	95.75 (12)	Al1—O6—C14—C15	177.36 (11)
O4—Al1—O6—C14	−83.98 (12)	C12—C13—C14—O6	−2.1 (3)
O2—Al1—O6—C14	−173.05 (12)	C12—C13—C14—C15	176.66 (16)

(Ie) Tris(pentane-2,4-dionato-κ²O,O')aluminium(III)

Crystal data

[Al(C5H7O2)3]	F(000) = 2064
Mr = 324.30	Dx = 1.323 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 37277 reflections
a = 22.7424 (11) Å	θ = 1.8–27.5°
b = 7.4467 (2) Å	µ = 0.15 mm^−1
c = 29.6165 (13) Å	T = 110 K
β = 103.221 (2)°	Hexagonal prism, colourless
V = 4882.8 (3) Å^3	0.42 × 0.39 × 0.18 mm
Z = 12

Data collection

Nonius KappaCCD diffractometer	11232 independent reflections
Radiation source: rotating anode	8990 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
ϕ and ω scans	θmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −29→29
Tmin = 0.66, Tmax = 0.98	k = −9→9
83926 measured reflections	l = −38→38

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.038	Hydrogen site location: difference Fourier map
wR(F^2) = 0.111	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0512P)^2 + 1.8338P] where P = (Fo^2 + 2Fc^2)/3
11232 reflections	(Δ/σ)max = 0.001
613 parameters	Δρmax = 0.34 e Å^−3
0 restraints	Δρmin = −0.26 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Al1	0.266240 (16)	0.23797 (5)	0.263289 (12)	0.01514 (9)
O11	0.24162 (4)	0.00709 (12)	0.23997 (3)	0.01853 (19)
O21	0.26978 (4)	0.31780 (12)	0.20351 (3)	0.01883 (19)
O31	0.34809 (4)	0.16641 (12)	0.27374 (3)	0.01876 (19)
O41	0.28831 (4)	0.47085 (12)	0.28573 (3)	0.01918 (19)
O51	0.26693 (4)	0.15542 (13)	0.32305 (3)	0.02024 (19)
O61	0.18470 (4)	0.30855 (13)	0.25335 (3)	0.01965 (19)
C11	0.21872 (6)	−0.24808 (18)	0.19157 (5)	0.0252 (3)
H11A	0.2389	−0.3228	0.2178	0.038*
H11B	0.2283	−0.2932	0.1630	0.038*
H11C	0.1749	−0.2527	0.1886	0.038*
C21	0.24022 (5)	−0.05708 (17)	0.19968 (4)	0.0178 (3)
C31	0.25605 (6)	0.04028 (18)	0.16398 (4)	0.0218 (3)
H31	0.2574	−0.0203	0.1360	0.026*
C41	0.26996 (5)	0.22322 (18)	0.16770 (4)	0.0184 (3)
C51	0.28387 (7)	0.3204 (2)	0.12697 (5)	0.0275 (3)
H51A	0.2498	0.3982	0.1130	0.041*
H51B	0.2906	0.2328	0.1040	0.041*
H51C	0.3203	0.3935	0.1374	0.041*
C61	0.45413 (6)	0.1588 (2)	0.30037 (5)	0.0250 (3)
H61A	0.4471	0.0315	0.2925	0.038*
H61B	0.4771	0.1698	0.3325	0.038*
H61C	0.4770	0.2133	0.2796	0.038*
C71	0.39450 (5)	0.25326 (18)	0.29486 (4)	0.0172 (2)
C81	0.39327 (6)	0.42857 (18)	0.31163 (4)	0.0210 (3)
H81	0.4301	0.4806	0.3281	0.025*
C91	0.34070 (6)	0.53032 (17)	0.30525 (4)	0.0167 (2)
C101	0.34257 (6)	0.72294 (18)	0.32123 (4)	0.0214 (3)
H10A	0.3208	0.7987	0.2958	0.032*
H10B	0.3847	0.7629	0.3306	0.032*
H10C	0.3235	0.7324	0.3476	0.032*
C111	0.23944 (7)	0.0711 (2)	0.39181 (5)	0.0302 (3)
H11D	0.2606	−0.0432	0.3912	0.045*
H11E	0.2024	0.0507	0.4027	0.045*
H11F	0.2657	0.1546	0.4128	0.045*
C121	0.22363 (6)	0.14976 (18)	0.34380 (4)	0.0209 (3)
C131	0.16547 (6)	0.2097 (2)	0.32466 (5)	0.0291 (3)
H131	0.1357	0.1984	0.3424	0.035*
C141	0.14872 (6)	0.28631 (19)	0.28032 (5)	0.0228 (3)
C151	0.08433 (6)	0.3432 (2)	0.26160 (6)	0.0355 (4)
H15A	0.0821	0.4222	0.2348	0.053*
H15B	0.0697	0.4077	0.2857	0.053*
H15C	0.0592	0.2368	0.2521	0.053*
Al2	0.398382 (17)	0.78593 (5)	0.071077 (13)	0.01698 (9)
O12	0.42417 (4)	1.01742 (12)	0.09265 (3)	0.02006 (19)
O22	0.39249 (4)	0.71437 (12)	0.13108 (3)	0.02006 (19)
O32	0.31710 (4)	0.86337 (12)	0.05864 (3)	0.02072 (19)
O42	0.37465 (4)	0.55312 (12)	0.04928 (3)	0.0213 (2)
O52	0.40169 (4)	0.85966 (13)	0.01102 (3)	0.0217 (2)
O62	0.47864 (4)	0.70554 (13)	0.08354 (3)	0.01979 (19)
C12	0.45177 (6)	1.27368 (18)	0.13946 (5)	0.0260 (3)
H12A	0.4947	1.2750	0.1389	0.039*
H12B	0.4468	1.3198	0.1693	0.039*
H12C	0.4292	1.3495	0.1144	0.039*
C22	0.42823 (5)	1.08412 (17)	0.13291 (4)	0.0187 (3)
C32	0.41348 (6)	0.99220 (19)	0.16974 (5)	0.0236 (3)
H32	0.4151	1.0549	0.1979	0.028*
C42	0.39642 (5)	0.81148 (19)	0.16699 (4)	0.0196 (3)
C52	0.38358 (7)	0.7197 (2)	0.20889 (5)	0.0279 (3)
H52A	0.3470	0.6464	0.1996	0.042*
H52B	0.3776	0.8102	0.2314	0.042*
H52C	0.4178	0.6425	0.2230	0.042*
C62	0.21116 (6)	0.8767 (2)	0.03182 (5)	0.0248 (3)
H62A	0.1874	0.8235	0.0522	0.037*
H62B	0.1886	0.8672	−0.0005	0.037*
H62C	0.2190	1.0034	0.0399	0.037*
C72	0.27016 (6)	0.77833 (18)	0.03777 (4)	0.0179 (3)
C82	0.27038 (6)	0.60195 (19)	0.02158 (4)	0.0218 (3)
H82	0.2334	0.5518	0.0048	0.026*
C92	0.32240 (6)	0.49614 (17)	0.02893 (4)	0.0179 (3)
C102	0.31939 (6)	0.30352 (18)	0.01321 (4)	0.0223 (3)
H10D	0.3389	0.2916	−0.0129	0.033*
H10E	0.2770	0.2663	0.0034	0.033*
H10F	0.3402	0.2272	0.0389	0.033*
C112	0.42919 (7)	0.8862 (2)	−0.06056 (5)	0.0293 (3)
H11G	0.4041	0.7955	−0.0799	0.044*
H11H	0.4671	0.9005	−0.0706	0.044*
H11I	0.4076	1.0010	−0.0637	0.044*
C122	0.44277 (6)	0.82728 (18)	−0.01073 (4)	0.0210 (3)
C132	0.49728 (6)	0.74131 (19)	0.00868 (5)	0.0242 (3)
H132	0.5249	0.7193	−0.0104	0.029*
C142	0.51279 (6)	0.68643 (17)	0.05502 (4)	0.0198 (3)
C152	0.57331 (6)	0.6038 (2)	0.07493 (5)	0.0272 (3)
H15D	0.6000	0.6938	0.0933	0.041*
H15E	0.5911	0.5613	0.0497	0.041*
H15F	0.5685	0.5024	0.0949	0.041*
Al3	0.067589 (17)	0.75773 (5)	0.399724 (13)	0.01828 (9)
O13	0.09427 (4)	0.98843 (12)	0.42106 (3)	0.0210 (2)
O23	0.05918 (4)	0.69004 (12)	0.45946 (3)	0.02054 (19)
O33	−0.01282 (4)	0.84299 (12)	0.38616 (3)	0.0234 (2)
O43	0.04168 (4)	0.52609 (12)	0.37825 (3)	0.0223 (2)
O53	0.07388 (4)	0.82466 (14)	0.33967 (3)	0.0262 (2)
O63	0.14713 (4)	0.67189 (13)	0.41436 (3)	0.01970 (19)
C13	0.12045 (6)	1.24807 (18)	0.46711 (5)	0.0269 (3)
H13A	0.1634	1.2489	0.4665	0.040*
H13B	0.1155	1.2949	0.4970	0.040*
H13C	0.0979	1.3237	0.4420	0.040*
C23	0.09675 (5)	1.05853 (17)	0.46081 (5)	0.0200 (3)
C33	0.08002 (6)	0.96961 (19)	0.49733 (5)	0.0254 (3)
H33	0.0807	1.0343	0.5251	0.031*
C43	0.06226 (6)	0.78926 (19)	0.49493 (5)	0.0210 (3)
C53	0.04731 (7)	0.7007 (2)	0.53649 (5)	0.0305 (3)
H53A	0.0078	0.6418	0.5273	0.046*
H53B	0.0461	0.7915	0.5602	0.046*
H53C	0.0783	0.6110	0.5491	0.046*
C63	−0.11941 (6)	0.85826 (19)	0.36565 (5)	0.0247 (3)
H63A	−0.1107	0.9794	0.3783	0.037*
H63B	−0.1453	0.7956	0.3828	0.037*
H63C	−0.1401	0.8662	0.3328	0.037*
C73	−0.06132 (6)	0.75625 (17)	0.37024 (4)	0.0180 (3)
C83	−0.06337 (6)	0.57532 (18)	0.35749 (5)	0.0224 (3)
H83	−0.1016	0.5224	0.3449	0.027*
C93	−0.01185 (6)	0.46880 (17)	0.36238 (4)	0.0176 (2)
C103	−0.01703 (6)	0.27343 (18)	0.34896 (5)	0.0225 (3)
H10G	−0.0001	0.2546	0.3218	0.034*
H10H	−0.0597	0.2379	0.3416	0.034*
H10I	0.0053	0.2006	0.3748	0.034*
C113	0.10442 (8)	0.8294 (3)	0.26841 (5)	0.0434 (4)
H11J	0.0950	0.7211	0.2493	0.065*
H11K	0.1408	0.8861	0.2625	0.065*
H11L	0.0705	0.9135	0.2606	0.065*
C123	0.11515 (7)	0.7795 (2)	0.31885 (5)	0.0276 (3)
C133	0.16815 (7)	0.6885 (2)	0.33987 (5)	0.0298 (3)
H133	0.1957	0.6566	0.3215	0.036*
C143	0.18211 (6)	0.64306 (19)	0.38669 (5)	0.0219 (3)
C153	0.24182 (6)	0.5591 (2)	0.40839 (5)	0.0290 (3)
H15G	0.2677	0.6481	0.4277	0.043*
H15H	0.2613	0.5174	0.3840	0.043*
H15I	0.2355	0.4570	0.4276	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Al1	0.01391 (18)	0.01679 (19)	0.01467 (18)	−0.00143 (14)	0.00312 (14)	−0.00030 (14)
O11	0.0192 (4)	0.0186 (4)	0.0171 (4)	−0.0031 (4)	0.0027 (3)	−0.0003 (3)
O21	0.0205 (4)	0.0193 (5)	0.0173 (4)	−0.0030 (4)	0.0056 (3)	0.0007 (4)
O31	0.0158 (4)	0.0196 (5)	0.0206 (4)	−0.0008 (3)	0.0035 (3)	−0.0027 (4)
O41	0.0173 (4)	0.0190 (5)	0.0202 (4)	−0.0003 (4)	0.0022 (3)	−0.0024 (4)
O51	0.0204 (5)	0.0235 (5)	0.0167 (4)	0.0005 (4)	0.0040 (4)	0.0011 (4)
O61	0.0160 (4)	0.0230 (5)	0.0197 (4)	−0.0005 (4)	0.0035 (3)	0.0002 (4)
C11	0.0254 (7)	0.0178 (7)	0.0301 (7)	0.0006 (5)	0.0015 (6)	−0.0044 (5)
C21	0.0123 (6)	0.0183 (6)	0.0213 (6)	0.0030 (5)	0.0007 (5)	−0.0019 (5)
C31	0.0238 (7)	0.0234 (7)	0.0188 (6)	0.0021 (5)	0.0062 (5)	−0.0031 (5)
C41	0.0135 (6)	0.0258 (7)	0.0163 (6)	0.0010 (5)	0.0042 (5)	0.0015 (5)
C51	0.0306 (7)	0.0336 (8)	0.0210 (7)	−0.0028 (6)	0.0114 (6)	0.0039 (6)
C61	0.0165 (6)	0.0318 (8)	0.0249 (7)	0.0035 (5)	0.0005 (5)	−0.0031 (6)
C71	0.0162 (6)	0.0230 (6)	0.0122 (5)	−0.0005 (5)	0.0029 (4)	0.0021 (5)
C81	0.0170 (6)	0.0235 (7)	0.0207 (6)	−0.0036 (5)	0.0006 (5)	−0.0013 (5)
C91	0.0206 (6)	0.0187 (6)	0.0109 (5)	−0.0032 (5)	0.0036 (5)	0.0020 (5)
C101	0.0273 (7)	0.0183 (6)	0.0178 (6)	−0.0028 (5)	0.0036 (5)	−0.0016 (5)
C111	0.0355 (8)	0.0372 (8)	0.0184 (7)	−0.0085 (7)	0.0069 (6)	0.0029 (6)
C121	0.0258 (7)	0.0211 (6)	0.0167 (6)	−0.0062 (5)	0.0066 (5)	−0.0035 (5)
C131	0.0229 (7)	0.0444 (9)	0.0229 (7)	−0.0018 (6)	0.0111 (6)	−0.0017 (6)
C141	0.0186 (6)	0.0260 (7)	0.0243 (7)	−0.0006 (5)	0.0061 (5)	−0.0067 (5)
C151	0.0202 (7)	0.0495 (10)	0.0373 (8)	0.0076 (7)	0.0075 (6)	−0.0066 (7)
Al2	0.01516 (19)	0.01800 (19)	0.01682 (18)	−0.00129 (14)	0.00163 (14)	0.00091 (15)
O12	0.0206 (5)	0.0201 (5)	0.0184 (4)	−0.0032 (4)	0.0023 (4)	0.0010 (4)
O22	0.0202 (5)	0.0208 (5)	0.0197 (4)	−0.0024 (4)	0.0058 (4)	0.0013 (4)
O32	0.0176 (4)	0.0191 (5)	0.0240 (5)	−0.0008 (4)	0.0017 (4)	−0.0011 (4)
O42	0.0190 (5)	0.0197 (5)	0.0229 (5)	−0.0003 (4)	0.0001 (4)	−0.0011 (4)
O52	0.0221 (5)	0.0234 (5)	0.0179 (4)	0.0012 (4)	0.0014 (4)	0.0020 (4)
O62	0.0164 (4)	0.0243 (5)	0.0183 (4)	−0.0003 (4)	0.0032 (3)	0.0030 (4)
C12	0.0253 (7)	0.0198 (7)	0.0310 (7)	−0.0019 (5)	0.0026 (6)	−0.0032 (6)
C22	0.0126 (6)	0.0188 (6)	0.0226 (6)	0.0021 (5)	−0.0004 (5)	−0.0014 (5)
C32	0.0262 (7)	0.0253 (7)	0.0197 (6)	0.0010 (5)	0.0062 (5)	−0.0025 (5)
C42	0.0126 (6)	0.0272 (7)	0.0194 (6)	0.0026 (5)	0.0042 (5)	0.0038 (5)
C52	0.0275 (7)	0.0362 (8)	0.0223 (7)	−0.0015 (6)	0.0105 (6)	0.0064 (6)
C62	0.0186 (6)	0.0292 (7)	0.0250 (7)	0.0031 (5)	0.0013 (5)	−0.0016 (6)
C72	0.0162 (6)	0.0236 (6)	0.0136 (6)	−0.0007 (5)	0.0024 (5)	0.0032 (5)
C82	0.0182 (6)	0.0237 (7)	0.0214 (6)	−0.0037 (5)	0.0000 (5)	−0.0020 (5)
C92	0.0221 (6)	0.0198 (6)	0.0116 (5)	−0.0032 (5)	0.0035 (5)	0.0023 (5)
C102	0.0275 (7)	0.0212 (7)	0.0176 (6)	−0.0030 (5)	0.0039 (5)	−0.0013 (5)
C112	0.0396 (8)	0.0299 (8)	0.0169 (6)	−0.0034 (6)	0.0033 (6)	0.0012 (6)
C122	0.0273 (7)	0.0183 (6)	0.0167 (6)	−0.0055 (5)	0.0034 (5)	−0.0020 (5)
C132	0.0258 (7)	0.0279 (7)	0.0201 (6)	0.0008 (6)	0.0076 (5)	−0.0012 (5)
C142	0.0201 (6)	0.0168 (6)	0.0223 (6)	−0.0022 (5)	0.0047 (5)	−0.0015 (5)
C152	0.0220 (7)	0.0292 (8)	0.0304 (7)	0.0054 (6)	0.0062 (6)	0.0021 (6)
Al3	0.01498 (19)	0.01725 (19)	0.0211 (2)	−0.00244 (14)	0.00095 (15)	0.00296 (15)
O13	0.0193 (5)	0.0193 (5)	0.0228 (5)	−0.0044 (4)	0.0015 (4)	0.0032 (4)
O23	0.0191 (5)	0.0184 (5)	0.0250 (5)	−0.0020 (4)	0.0069 (4)	0.0027 (4)
O33	0.0167 (4)	0.0171 (5)	0.0333 (5)	−0.0019 (4)	−0.0010 (4)	0.0017 (4)
O43	0.0182 (5)	0.0191 (5)	0.0276 (5)	−0.0009 (4)	0.0010 (4)	0.0006 (4)
O53	0.0254 (5)	0.0278 (5)	0.0219 (5)	−0.0044 (4)	−0.0020 (4)	0.0054 (4)
O63	0.0161 (4)	0.0245 (5)	0.0184 (4)	−0.0007 (4)	0.0037 (3)	0.0028 (4)
C13	0.0240 (7)	0.0187 (7)	0.0358 (8)	−0.0037 (5)	0.0020 (6)	0.0003 (6)
C23	0.0126 (6)	0.0180 (6)	0.0272 (7)	0.0011 (5)	0.0002 (5)	0.0009 (5)
C33	0.0264 (7)	0.0239 (7)	0.0268 (7)	−0.0016 (6)	0.0077 (6)	−0.0006 (6)
C43	0.0144 (6)	0.0252 (7)	0.0241 (7)	0.0012 (5)	0.0057 (5)	0.0033 (5)
C53	0.0340 (8)	0.0316 (8)	0.0295 (7)	−0.0040 (6)	0.0145 (6)	0.0051 (6)
C63	0.0175 (6)	0.0257 (7)	0.0292 (7)	0.0005 (5)	0.0015 (5)	−0.0010 (6)
C73	0.0166 (6)	0.0214 (6)	0.0151 (6)	−0.0009 (5)	0.0020 (5)	0.0043 (5)
C83	0.0174 (6)	0.0219 (7)	0.0253 (7)	−0.0043 (5)	−0.0005 (5)	−0.0010 (5)
C93	0.0213 (6)	0.0187 (6)	0.0125 (5)	−0.0034 (5)	0.0031 (5)	0.0012 (5)
C103	0.0270 (7)	0.0198 (7)	0.0194 (6)	−0.0019 (5)	0.0027 (5)	−0.0019 (5)
C113	0.0522 (11)	0.0557 (11)	0.0191 (7)	−0.0152 (9)	0.0013 (7)	0.0068 (7)
C123	0.0312 (8)	0.0317 (8)	0.0181 (6)	−0.0127 (6)	0.0020 (6)	0.0016 (6)
C133	0.0275 (7)	0.0418 (9)	0.0215 (7)	−0.0058 (6)	0.0087 (6)	−0.0019 (6)
C143	0.0182 (6)	0.0240 (7)	0.0234 (6)	−0.0045 (5)	0.0047 (5)	−0.0016 (5)
C153	0.0215 (7)	0.0358 (8)	0.0309 (8)	0.0021 (6)	0.0085 (6)	0.0003 (6)

Geometric parameters (Å, º)

Al1—O51	1.8704 (9)	C62—C72	1.5032 (17)
Al1—O41	1.8837 (10)	C62—H62A	0.9800
Al1—O61	1.8847 (9)	C62—H62B	0.9800
Al1—O21	1.8867 (9)	C62—H62C	0.9800
Al1—O11	1.8894 (10)	C72—C82	1.3987 (19)
Al1—O31	1.8924 (9)	C82—C92	1.3965 (18)
O11—C21	1.2788 (15)	C82—H82	0.9500
O21—C41	1.2739 (15)	C92—C102	1.5048 (18)
O31—C71	1.2735 (15)	C102—H10D	0.9800
O41—C91	1.2786 (15)	C102—H10E	0.9800
O51—C121	1.2750 (15)	C102—H10F	0.9800
O61—C141	1.2780 (15)	C112—C122	1.5023 (17)
C11—C21	1.5053 (18)	C112—H11G	0.9800
C11—H11A	0.9800	C112—H11H	0.9800
C11—H11B	0.9800	C112—H11I	0.9800
C11—H11C	0.9800	C122—C132	1.3969 (19)
C21—C31	1.3955 (18)	C132—C142	1.3978 (18)
C31—C41	1.3972 (19)	C132—H132	0.9500
C31—H31	0.9500	C142—C152	1.4999 (18)
C41—C51	1.5012 (17)	C152—H15D	0.9800
C51—H51A	0.9800	C152—H15E	0.9800
C51—H51B	0.9800	C152—H15F	0.9800
C51—H51C	0.9800	Al3—O63	1.8735 (10)
C61—C71	1.5032 (17)	Al3—O13	1.8824 (10)
C61—H61A	0.9800	Al3—O53	1.8838 (10)
C61—H61B	0.9800	Al3—O43	1.8857 (10)
C61—H61C	0.9800	Al3—O33	1.8902 (10)
C71—C81	1.3992 (18)	Al3—O23	1.8910 (10)
C81—C91	1.3914 (18)	O13—C23	1.2771 (16)
C81—H81	0.9500	O23—C43	1.2730 (16)
C91—C101	1.5080 (18)	O33—C73	1.2720 (15)
C101—H10A	0.9800	O43—C93	1.2740 (15)
C101—H10B	0.9800	O53—C123	1.2801 (18)
C101—H10C	0.9800	O63—C143	1.2842 (15)
C111—C121	1.5034 (18)	C13—C23	1.5072 (18)
C111—H11D	0.9800	C13—H13A	0.9800
C111—H11E	0.9800	C13—H13B	0.9800
C111—H11F	0.9800	C13—H13C	0.9800
C121—C131	1.388 (2)	C23—C33	1.3935 (19)
C131—C141	1.402 (2)	C33—C43	1.3996 (19)
C131—H131	0.9500	C33—H33	0.9500
C141—C151	1.5034 (19)	C43—C53	1.5021 (18)
C151—H15A	0.9800	C53—H53A	0.9800
C151—H15B	0.9800	C53—H53B	0.9800
C151—H15C	0.9800	C53—H53C	0.9800
Al2—O62	1.8757 (10)	C63—C73	1.5030 (17)
Al2—O52	1.8793 (10)	C63—H63A	0.9800
Al2—O12	1.8848 (10)	C63—H63B	0.9800
Al2—O42	1.8853 (10)	C63—H63C	0.9800
Al2—O22	1.8890 (9)	C73—C83	1.3972 (19)
Al2—O32	1.8904 (10)	C83—C93	1.3947 (18)
O12—C22	1.2754 (15)	C83—H83	0.9500
O22—C42	1.2723 (16)	C93—C103	1.5056 (18)
O32—C72	1.2732 (15)	C103—H10G	0.9800
O42—C92	1.2757 (15)	C103—H10H	0.9800
O52—C122	1.2734 (16)	C103—H10I	0.9800
O62—C142	1.2793 (15)	C113—C123	1.5042 (19)
C12—C22	1.5064 (18)	C113—H11J	0.9800
C12—H12A	0.9800	C113—H11K	0.9800
C12—H12B	0.9800	C113—H11L	0.9800
C12—H12C	0.9800	C123—C133	1.399 (2)
C22—C32	1.3920 (18)	C133—C143	1.3918 (19)
C32—C42	1.3978 (19)	C133—H133	0.9500
C32—H32	0.9500	C143—C153	1.4994 (19)
C42—C52	1.5029 (17)	C153—H15G	0.9800
C52—H52A	0.9800	C153—H15H	0.9800
C52—H52B	0.9800	C153—H15I	0.9800
C52—H52C	0.9800
O51—Al1—O41	91.42 (4)	C72—C62—H62A	109.5
O51—Al1—O61	91.98 (4)	C72—C62—H62B	109.5
O41—Al1—O61	88.38 (4)	H62A—C62—H62B	109.5
O51—Al1—O21	177.04 (4)	C72—C62—H62C	109.5
O41—Al1—O21	88.62 (4)	H62A—C62—H62C	109.5
O61—Al1—O21	90.99 (4)	H62B—C62—H62C	109.5
O51—Al1—O11	89.11 (4)	O32—C72—C82	124.41 (12)
O41—Al1—O11	178.19 (4)	O32—C72—C62	116.20 (12)
O61—Al1—O11	89.88 (4)	C82—C72—C62	119.38 (12)
O21—Al1—O11	90.93 (4)	C92—C82—C72	123.08 (12)
O51—Al1—O31	87.57 (4)	C92—C82—H82	118.5
O41—Al1—O31	91.65 (4)	C72—C82—H82	118.5
O61—Al1—O31	179.55 (4)	O42—C92—C82	123.39 (12)
O21—Al1—O31	89.47 (4)	O42—C92—C102	115.78 (12)
O11—Al1—O31	90.09 (4)	C82—C92—C102	120.83 (12)
C21—O11—Al1	128.55 (8)	C92—C102—H10D	109.5
C41—O21—Al1	128.02 (9)	C92—C102—H10E	109.5
C71—O31—Al1	127.66 (8)	H10D—C102—H10E	109.5
C91—O41—Al1	128.60 (8)	C92—C102—H10F	109.5
C121—O51—Al1	128.80 (9)	H10D—C102—H10F	109.5
C141—O61—Al1	127.87 (9)	H10E—C102—H10F	109.5
C21—C11—H11A	109.5	C122—C112—H11G	109.5
C21—C11—H11B	109.5	C122—C112—H11H	109.5
H11A—C11—H11B	109.5	H11G—C112—H11H	109.5
C21—C11—H11C	109.5	C122—C112—H11I	109.5
H11A—C11—H11C	109.5	H11G—C112—H11I	109.5
H11B—C11—H11C	109.5	H11H—C112—H11I	109.5
O11—C21—C31	123.85 (12)	O52—C122—C132	124.29 (12)
O11—C21—C11	116.09 (11)	O52—C122—C112	115.59 (12)
C31—C21—C11	120.04 (12)	C132—C122—C112	120.11 (12)
C21—C31—C41	122.67 (12)	C122—C132—C142	122.61 (12)
C21—C31—H31	118.7	C122—C132—H132	118.7
C41—C31—H31	118.7	C142—C132—H132	118.7
O21—C41—C31	124.13 (12)	O62—C142—C132	124.12 (12)
O21—C41—C51	116.36 (12)	O62—C142—C152	115.29 (11)
C31—C41—C51	119.47 (12)	C132—C142—C152	120.57 (12)
C41—C51—H51A	109.5	C142—C152—H15D	109.5
C41—C51—H51B	109.5	C142—C152—H15E	109.5
H51A—C51—H51B	109.5	H15D—C152—H15E	109.5
C41—C51—H51C	109.5	C142—C152—H15F	109.5
H51A—C51—H51C	109.5	H15D—C152—H15F	109.5
H51B—C51—H51C	109.5	H15E—C152—H15F	109.5
C71—C61—H61A	109.5	O63—Al3—O13	90.78 (4)
C71—C61—H61B	109.5	O63—Al3—O53	91.77 (4)
H61A—C61—H61B	109.5	O13—Al3—O53	89.27 (4)
C71—C61—H61C	109.5	O63—Al3—O43	88.66 (4)
H61A—C61—H61C	109.5	O13—Al3—O43	179.40 (5)
H61B—C61—H61C	109.5	O53—Al3—O43	90.51 (5)
O31—C71—C81	124.51 (12)	O63—Al3—O33	178.85 (5)
O31—C71—C61	116.18 (11)	O13—Al3—O33	89.24 (4)
C81—C71—C61	119.28 (12)	O53—Al3—O33	89.38 (4)
C91—C81—C71	123.11 (12)	O43—Al3—O33	91.32 (4)
C91—C81—H81	118.4	O63—Al3—O23	89.51 (4)
C71—C81—H81	118.4	O13—Al3—O23	91.31 (4)
O41—C91—C81	123.76 (12)	O53—Al3—O23	178.58 (5)
O41—C91—C101	115.33 (11)	O43—Al3—O23	88.92 (4)
C81—C91—C101	120.91 (11)	O33—Al3—O23	89.34 (4)
C91—C101—H10A	109.5	C23—O13—Al3	128.72 (9)
C91—C101—H10B	109.5	C43—O23—Al3	128.26 (9)
H10A—C101—H10B	109.5	C73—O33—Al3	128.53 (9)
C91—C101—H10C	109.5	C93—O43—Al3	129.00 (9)
H10A—C101—H10C	109.5	C123—O53—Al3	127.42 (9)
H10B—C101—H10C	109.5	C143—O63—Al3	128.00 (9)
C121—C111—H11D	109.5	C23—C13—H13A	109.5
C121—C111—H11E	109.5	C23—C13—H13B	109.5
H11D—C111—H11E	109.5	H13A—C13—H13B	109.5
C121—C111—H11F	109.5	C23—C13—H13C	109.5
H11D—C111—H11F	109.5	H13A—C13—H13C	109.5
H11E—C111—H11F	109.5	H13B—C13—H13C	109.5
O51—C121—C131	124.15 (12)	O13—C23—C33	123.98 (12)
O51—C121—C111	115.13 (12)	O13—C23—C13	115.86 (12)
C131—C121—C111	120.72 (12)	C33—C23—C13	120.15 (13)
C121—C131—C141	122.86 (12)	C23—C33—C43	122.92 (13)
C121—C131—H131	118.6	C23—C33—H33	118.5
C141—C131—H131	118.6	C43—C33—H33	118.5
O61—C141—C131	124.21 (12)	O23—C43—C33	124.02 (12)
O61—C141—C151	116.23 (12)	O23—C43—C53	116.19 (12)
C131—C141—C151	119.54 (12)	C33—C43—C53	119.76 (13)
C141—C151—H15A	109.5	C43—C53—H53A	109.5
C141—C151—H15B	109.5	C43—C53—H53B	109.5
H15A—C151—H15B	109.5	H53A—C53—H53B	109.5
C141—C151—H15C	109.5	C43—C53—H53C	109.5
H15A—C151—H15C	109.5	H53A—C53—H53C	109.5
H15B—C151—H15C	109.5	H53B—C53—H53C	109.5
O62—Al2—O52	91.82 (4)	C73—C63—H63A	109.5
O62—Al2—O12	90.68 (4)	C73—C63—H63B	109.5
O52—Al2—O12	88.68 (4)	H63A—C63—H63B	109.5
O62—Al2—O42	87.90 (4)	C73—C63—H63C	109.5
O52—Al2—O42	90.85 (4)	H63A—C63—H63C	109.5
O12—Al2—O42	178.49 (5)	H63B—C63—H63C	109.5
O62—Al2—O22	90.00 (4)	O33—C73—C83	124.22 (12)
O52—Al2—O22	178.18 (5)	O33—C73—C63	116.52 (12)
O12—Al2—O22	91.30 (4)	C83—C73—C63	119.25 (12)
O42—Al2—O22	89.22 (4)	C93—C83—C73	123.03 (12)
O62—Al2—O32	179.13 (5)	C93—C83—H83	118.5
O52—Al2—O32	88.60 (4)	C73—C83—H83	118.5
O12—Al2—O32	90.10 (4)	O43—C93—C83	123.85 (12)
O42—Al2—O32	91.33 (4)	O43—C93—C103	115.55 (12)
O22—Al2—O32	89.59 (4)	C83—C93—C103	120.60 (12)
C22—O12—Al2	128.57 (8)	C93—C103—H10G	109.5
C42—O22—Al2	128.28 (9)	C93—C103—H10H	109.5
C72—O32—Al2	128.09 (9)	H10G—C103—H10H	109.5
C92—O42—Al2	129.07 (9)	C93—C103—H10I	109.5
C122—O52—Al2	128.05 (9)	H10G—C103—H10I	109.5
C142—O62—Al2	128.02 (9)	H10H—C103—H10I	109.5
C22—C12—H12A	109.5	C123—C113—H11J	109.5
C22—C12—H12B	109.5	C123—C113—H11K	109.5
H12A—C12—H12B	109.5	H11J—C113—H11K	109.5
C22—C12—H12C	109.5	C123—C113—H11L	109.5
H12A—C12—H12C	109.5	H11J—C113—H11L	109.5
H12B—C12—H12C	109.5	H11K—C113—H11L	109.5
O12—C22—C32	124.20 (12)	O53—C123—C133	124.41 (13)
O12—C22—C12	115.64 (12)	O53—C123—C113	116.31 (14)
C32—C22—C12	120.15 (12)	C133—C123—C113	119.28 (14)
C22—C32—C42	122.76 (12)	C143—C133—C123	122.56 (13)
C22—C32—H32	118.6	C143—C133—H133	118.7
C42—C32—H32	118.6	C123—C133—H133	118.7
O22—C42—C32	124.15 (12)	O63—C143—C133	124.18 (13)
O22—C42—C52	116.23 (12)	O63—C143—C153	115.37 (12)
C32—C42—C52	119.58 (12)	C133—C143—C153	120.43 (12)
C42—C52—H52A	109.5	C143—C153—H15G	109.5
C42—C52—H52B	109.5	C143—C153—H15H	109.5
H52A—C52—H52B	109.5	H15G—C153—H15H	109.5
C42—C52—H52C	109.5	C143—C153—H15I	109.5
H52A—C52—H52C	109.5	H15G—C153—H15I	109.5
H52B—C52—H52C	109.5	H15H—C153—H15I	109.5
O51—Al1—O11—C21	−167.25 (10)	Al2—O12—C22—C32	−0.01 (19)
O61—Al1—O11—C21	100.77 (10)	Al2—O12—C22—C12	178.86 (8)
O21—Al1—O11—C21	9.78 (11)	O12—C22—C32—C42	4.5 (2)
O31—Al1—O11—C21	−79.68 (10)	C12—C22—C32—C42	−174.34 (12)
O41—Al1—O21—C41	166.64 (10)	Al2—O22—C42—C32	−8.12 (19)
O61—Al1—O21—C41	−105.01 (10)	Al2—O22—C42—C52	173.98 (9)
O11—Al1—O21—C41	−15.11 (11)	C22—C32—C42—O22	−0.3 (2)
O31—Al1—O21—C41	74.97 (10)	C22—C32—C42—C52	177.56 (12)
O51—Al1—O31—C71	−82.82 (10)	Al2—O32—C72—C82	3.18 (18)
O41—Al1—O31—C71	8.53 (10)	Al2—O32—C72—C62	−178.42 (8)
O21—Al1—O31—C71	97.14 (10)	O32—C72—C82—C92	3.6 (2)
O11—Al1—O31—C71	−171.93 (10)	C62—C72—C82—C92	−174.75 (12)
O51—Al1—O41—C91	80.06 (10)	Al2—O42—C92—C82	−4.23 (18)
O61—Al1—O41—C91	172.00 (10)	Al2—O42—C92—C102	176.34 (8)
O21—Al1—O41—C91	−96.97 (10)	C72—C82—C92—O42	−3.1 (2)
O31—Al1—O41—C91	−7.55 (10)	C72—C82—C92—C102	176.32 (12)
O41—Al1—O51—C121	91.30 (11)	Al2—O52—C122—C132	−6.24 (19)
O61—Al1—O51—C121	2.88 (11)	Al2—O52—C122—C112	173.04 (9)
O11—Al1—O51—C121	−86.97 (11)	O52—C122—C132—C142	−1.9 (2)
O31—Al1—O51—C121	−177.11 (11)	C112—C122—C132—C142	178.85 (13)
O51—Al1—O61—C141	−3.96 (11)	Al2—O62—C142—C132	6.87 (19)
O41—Al1—O61—C141	−95.32 (11)	Al2—O62—C142—C152	−174.88 (9)
O21—Al1—O61—C141	176.09 (11)	C122—C132—C142—O62	1.6 (2)
O11—Al1—O61—C141	85.15 (11)	C122—C132—C142—C152	−176.59 (13)
Al1—O11—C21—C31	−1.88 (18)	O63—Al3—O13—C23	−95.95 (11)
Al1—O11—C21—C11	179.43 (8)	O53—Al3—O13—C23	172.29 (11)
O11—C21—C31—C41	−5.8 (2)	O33—Al3—O13—C23	82.90 (11)
C11—C21—C31—C41	172.84 (12)	O23—Al3—O13—C23	−6.42 (11)
Al1—O21—C41—C31	12.69 (18)	O63—Al3—O23—C43	100.60 (11)
Al1—O21—C41—C51	−169.74 (9)	O13—Al3—O23—C43	9.83 (11)
C21—C31—C41—O21	0.2 (2)	O43—Al3—O23—C43	−170.73 (11)
C21—C31—C41—C51	−177.28 (12)	O33—Al3—O23—C43	−79.39 (11)
Al1—O31—C71—C81	−5.14 (18)	O13—Al3—O33—C73	−177.96 (11)
Al1—O31—C71—C61	176.66 (8)	O53—Al3—O33—C73	92.76 (11)
O31—C71—C81—C91	−2.6 (2)	O43—Al3—O33—C73	2.27 (11)
C61—C71—C81—C91	175.51 (12)	O23—Al3—O33—C73	−86.64 (11)
Al1—O41—C91—C81	3.04 (17)	O63—Al3—O43—C93	177.71 (11)
Al1—O41—C91—C101	−177.33 (8)	O53—Al3—O43—C93	−90.53 (11)
C71—C81—C91—O41	3.8 (2)	O33—Al3—O43—C93	−1.14 (11)
C71—C81—C91—C101	−175.85 (11)	O23—Al3—O43—C93	88.18 (11)
Al1—O51—C121—C131	−1.0 (2)	O63—Al3—O53—C123	13.35 (12)
Al1—O51—C121—C111	178.77 (9)	O13—Al3—O53—C123	104.11 (12)
O51—C121—C131—C141	−1.2 (2)	O43—Al3—O53—C123	−75.33 (12)
C111—C121—C131—C141	179.09 (14)	O33—Al3—O53—C123	−166.64 (12)
Al1—O61—C141—C131	3.2 (2)	O13—Al3—O63—C143	−101.66 (11)
Al1—O61—C141—C151	−175.16 (10)	O53—Al3—O63—C143	−12.36 (11)
C121—C131—C141—O61	0.0 (2)	O43—Al3—O63—C143	78.11 (11)
C121—C131—C141—C151	178.32 (14)	O23—Al3—O63—C143	167.03 (11)
O62—Al2—O12—C22	−95.42 (11)	Al3—O13—C23—C33	1.11 (19)
O52—Al2—O12—C22	172.78 (11)	Al3—O13—C23—C13	−179.90 (9)
O22—Al2—O12—C22	−5.41 (11)	O13—C23—C33—C43	4.2 (2)
O32—Al2—O12—C22	84.18 (11)	C13—C23—C33—C43	−174.79 (12)
O62—Al2—O22—C42	100.11 (11)	Al3—O23—C43—C33	−8.01 (19)
O12—Al2—O22—C42	9.43 (11)	Al3—O23—C43—C53	173.86 (9)
O42—Al2—O22—C42	−171.99 (11)	C23—C33—C43—O23	−0.6 (2)
O32—Al2—O22—C42	−80.66 (11)	C23—C33—C43—C53	177.50 (13)
O52—Al2—O32—C72	83.55 (11)	Al3—O33—C73—C83	−3.07 (19)
O12—Al2—O32—C72	172.22 (10)	Al3—O33—C73—C63	176.38 (9)
O42—Al2—O32—C72	−7.27 (11)	O33—C73—C83—C93	2.1 (2)
O22—Al2—O32—C72	−96.48 (11)	C63—C73—C83—C93	−177.32 (12)
O62—Al2—O42—C92	−172.54 (11)	Al3—O43—C93—C83	0.78 (18)
O52—Al2—O42—C92	−80.76 (11)	Al3—O43—C93—C103	−178.84 (8)
O22—Al2—O42—C92	97.43 (11)	C73—C83—C93—O43	−0.9 (2)
O32—Al2—O42—C92	7.86 (11)	C73—C83—C93—C103	178.68 (12)
O62—Al2—O52—C122	10.46 (11)	Al3—O53—C123—C133	−8.7 (2)
O12—Al2—O52—C122	101.10 (11)	Al3—O53—C123—C113	171.24 (10)
O42—Al2—O52—C122	−77.46 (11)	O53—C123—C133—C143	−2.2 (2)
O32—Al2—O52—C122	−168.77 (11)	C113—C123—C133—C143	177.89 (14)
O52—Al2—O62—C142	−10.76 (11)	Al3—O63—C143—C133	6.6 (2)
O12—Al2—O62—C142	−99.46 (11)	Al3—O63—C143—C153	−175.06 (9)
O42—Al2—O62—C142	80.03 (11)	C123—C133—C143—O63	3.4 (2)
O22—Al2—O62—C142	169.24 (11)	C123—C133—C143—C153	−174.95 (14)