Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107005707/av3070sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107005707/av3070Iasup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107005707/av3070Ibsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107005707/av3070Icsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107005707/av3070Idsup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270107005707/av3070Iesup6.hkl |
CCDC references: 641792; 641793; 641794; 641795; 641796
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.
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 Uiso(H) values of 1.2Ueq(C) for H atoms of the central CH groups and 1.5Ueq(C) for methyl H atoms.
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.
[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) Å3 | 0.42 × 0.39 × 0.18 mm |
Z = 4 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.041 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.124 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0624P)2 + 0.4307P] where P = (Fo2 + 2Fc2)/3 |
3870 reflections | (Δ/σ)max = 0.001 |
205 parameters | Δρmax = 0.20 e Å−3 |
0 restraints | Δρmin = −0.23 e Å−3 |
[Al(C5H7O2)3] | V = 1676.44 (11) Å3 |
Mr = 324.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.9140 (7) Å | µ = 0.15 mm−1 |
b = 7.50076 (17) Å | T = 240 K |
c = 16.2547 (6) Å | 0.42 × 0.39 × 0.18 mm |
β = 98.806 (2)° |
Nonius KappaCCD diffractometer | 3870 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 3065 reflections with I > 2σ(I) |
Tmin = 0.67, Tmax = 0.97 | Rint = 0.026 |
29848 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.124 | H-atom parameters constrained |
S = 1.08 | Δρmax = 0.20 e Å−3 |
3870 reflections | Δρmin = −0.23 e Å−3 |
205 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.24092 (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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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) |
[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) Å3 | 0.42 × 0.39 × 0.18 mm |
Z = 4 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.114 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.057P)2 + 0.4987P] where P = (Fo2 + 2Fc2)/3 |
3823 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.21 e Å−3 |
0 restraints | Δρmin = −0.25 e Å−3 |
[Al(C5H7O2)3] | V = 1659.94 (15) Å3 |
Mr = 324.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.8640 (6) Å | µ = 0.15 mm−1 |
b = 7.4755 (3) Å | T = 210 K |
c = 16.2080 (11) Å | 0.42 × 0.39 × 0.18 mm |
β = 98.821 (2)° |
Nonius KappaCCD diffractometer | 3823 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 3133 reflections with I > 2σ(I) |
Tmin = 0.70, Tmax = 0.97 | Rint = 0.025 |
29627 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.114 | H-atom parameters constrained |
S = 1.07 | Δρmax = 0.21 e Å−3 |
3823 reflections | Δρmin = −0.25 e Å−3 |
205 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.24082 (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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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) |
[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) Å3 | 0.42 × 0.39 × 0.18 mm |
Z = 4 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.037 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.103 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0496P)2 + 0.5412P] where P = (Fo2 + 2Fc2)/3 |
3801 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.22 e Å−3 |
0 restraints | Δρmin = −0.25 e Å−3 |
[Al(C5H7O2)3] | V = 1651.42 (16) Å3 |
Mr = 324.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.8385 (7) Å | µ = 0.15 mm−1 |
b = 7.4614 (3) Å | T = 180 K |
c = 16.1873 (11) Å | 0.42 × 0.39 × 0.18 mm |
β = 98.871 (2)° |
Nonius KappaCCD diffractometer | 3801 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 3201 reflections with I > 2σ(I) |
Tmin = 0.73, Tmax = 0.97 | Rint = 0.023 |
29482 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 0 restraints |
wR(F2) = 0.103 | H-atom parameters constrained |
S = 1.08 | Δρmax = 0.22 e Å−3 |
3801 reflections | Δρmin = −0.25 e Å−3 |
205 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.24071 (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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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) |
[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) Å3 | 0.42 × 0.39 × 0.18 mm |
Z = 4 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0455P)2 + 0.6404P] where P = (Fo2 + 2Fc2)/3 |
3771 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 0.26 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
[Al(C5H7O2)3] | V = 1637.57 (9) Å3 |
Mr = 324.30 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.7961 (5) Å | µ = 0.15 mm−1 |
b = 7.44012 (17) Å | T = 150 K |
c = 16.1488 (5) Å | 0.42 × 0.39 × 0.18 mm |
β = 98.914 (3)° |
Nonius KappaCCD diffractometer | 3771 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 3248 reflections with I > 2σ(I) |
Tmin = 0.74, Tmax = 0.98 | Rint = 0.023 |
29260 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.05 | Δρmax = 0.26 e Å−3 |
3771 reflections | Δρmin = −0.26 e Å−3 |
205 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.24065 (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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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) |
[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) Å3 | 0.42 × 0.39 × 0.18 mm |
Z = 12 |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.038 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.111 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0512P)2 + 1.8338P] where P = (Fo2 + 2Fc2)/3 |
11232 reflections | (Δ/σ)max = 0.001 |
613 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
[Al(C5H7O2)3] | V = 4882.8 (3) Å3 |
Mr = 324.30 | Z = 12 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.7424 (11) Å | µ = 0.15 mm−1 |
b = 7.4467 (2) Å | T = 110 K |
c = 29.6165 (13) Å | 0.42 × 0.39 × 0.18 mm |
β = 103.221 (2)° |
Nonius KappaCCD diffractometer | 11232 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | 8990 reflections with I > 2σ(I) |
Tmin = 0.66, Tmax = 0.98 | Rint = 0.036 |
83926 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.111 | H-atom parameters constrained |
S = 1.05 | Δρmax = 0.34 e Å−3 |
11232 reflections | Δρmin = −0.26 e Å−3 |
613 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.266240 (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* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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) |
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) |
Experimental details
(Ia) | (Ib) | (Ic) | (Id) | |
Crystal data | ||||
Chemical formula | [Al(C5H7O2)3] | [Al(C5H7O2)3] | [Al(C5H7O2)3] | [Al(C5H7O2)3] |
Mr | 324.30 | 324.30 | 324.30 | 324.30 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 240 | 210 | 180 | 150 |
a, b, c (Å) | 13.9140 (7), 7.50076 (17), 16.2547 (6) | 13.8640 (6), 7.4755 (3), 16.2080 (11) | 13.8385 (7), 7.4614 (3), 16.1873 (11) | 13.7961 (5), 7.44012 (17), 16.1488 (5) |
β (°) | 98.806 (2) | 98.821 (2) | 98.871 (2) | 98.914 (3) |
V (Å3) | 1676.44 (11) | 1659.94 (15) | 1651.42 (16) | 1637.57 (9) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.15 | 0.15 | 0.15 | 0.15 |
Crystal size (mm) | 0.42 × 0.39 × 0.18 | 0.42 × 0.39 × 0.18 | 0.42 × 0.39 × 0.18 | 0.42 × 0.39 × 0.18 |
Data collection | ||||
Diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2002) | Multi-scan (SADABS; Sheldrick, 2002) | Multi-scan (SADABS; Sheldrick, 2002) | Multi-scan (SADABS; Sheldrick, 2002) |
Tmin, Tmax | 0.67, 0.97 | 0.70, 0.97 | 0.73, 0.97 | 0.74, 0.98 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 29848, 3870, 3065 | 29627, 3823, 3133 | 29482, 3801, 3201 | 29260, 3771, 3248 |
Rint | 0.026 | 0.025 | 0.023 | 0.023 |
(sin θ/λ)max (Å−1) | 0.650 | 0.650 | 0.650 | 0.650 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.124, 1.08 | 0.039, 0.114, 1.07 | 0.037, 0.103, 1.08 | 0.034, 0.094, 1.05 |
No. of reflections | 3870 | 3823 | 3801 | 3771 |
No. of parameters | 205 | 205 | 205 | 205 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.20, −0.23 | 0.21, −0.25 | 0.22, −0.25 | 0.26, −0.26 |
(Ie) | |
Crystal data | |
Chemical formula | [Al(C5H7O2)3] |
Mr | 324.30 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 110 |
a, b, c (Å) | 22.7424 (11), 7.4467 (2), 29.6165 (13) |
β (°) | 103.221 (2) |
V (Å3) | 4882.8 (3) |
Z | 12 |
Radiation type | Mo Kα |
µ (mm−1) | 0.15 |
Crystal size (mm) | 0.42 × 0.39 × 0.18 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2002) |
Tmin, Tmax | 0.66, 0.98 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 83926, 11232, 8990 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.111, 1.05 |
No. of reflections | 11232 |
No. of parameters | 613 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.34, −0.26 |
Computer programs: COLLECT (Nonius, 1999), PEAKREF (Schreurs, 2005), EVAL14 (Duisenberg et al., 2003), EVAL15 (Xian et al., 2006), SHELXS97 (Sheldrick, 1997), coordinates were taken from (Ia), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003), manual editing of SHELXL97 output.
Al1—O51 | 1.8704 (9) | Al2—O42 | 1.8853 (10) |
Al1—O41 | 1.8837 (10) | Al2—O22 | 1.8890 (9) |
Al1—O61 | 1.8847 (9) | Al2—O32 | 1.8904 (10) |
Al1—O21 | 1.8867 (9) | Al3—O63 | 1.8735 (10) |
Al1—O11 | 1.8894 (10) | Al3—O13 | 1.8824 (10) |
Al1—O31 | 1.8924 (9) | Al3—O53 | 1.8838 (10) |
Al2—O62 | 1.8757 (10) | Al3—O43 | 1.8857 (10) |
Al2—O52 | 1.8793 (10) | Al3—O33 | 1.8902 (10) |
Al2—O12 | 1.8848 (10) | Al3—O23 | 1.8910 (10) |
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[(Uobs - Ucalc)2]/Σ(Uobs2)}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 AlIII 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 Ti and libration Li 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.