Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807057728/fj2066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807057728/fj2066Isup2.hkl |
CCDC reference: 672682
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.039
- wR factor = 0.098
- Data-to-parameter ratio = 27.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su .. 0.10
Alert level G REFLT03_ALERT_4_G ALERT: MoKa measured Friedel data cannot be used to determine absolute structure in a light-atom study EXCEPT under VERY special conditions. It is preferred that Friedel data is merged in such cases. From the CIF: _diffrn_reflns_theta_max 29.16 From the CIF: _reflns_number_total 6434 Count of symmetry unique reflns 3772 Completeness (_total/calc) 170.57% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2662 Fraction of Friedel pairs measured 0.706 Are heavy atom types Z>Si present no PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Al1 (3) 2.81 PLAT794_ALERT_5_G Check Predicted Bond Valency for Al2 (3) 2.64 PLAT794_ALERT_5_G Check Predicted Bond Valency for Al3 (3) 2.82
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 3 ALERT type 5 Informative message, check
The crystal structure of the title compound was first described in the enantiomorphic space group P41212 [Amma (1963); see Folting et al. (1991), Turova et al. (1979) and Turova et al. (1978) for later reports]. For a comment on the occurrence of compounds crystallizing in pairs of enantiomorphic space groups, see Ng (2007).
The aluminium isopropoxide was an unexpected product from reaction of trimethyl aluminium (0.72 g, 0.01 mmol; 5 ml of 2M solution in toluene) and 1-methoxy-2-propanol (0.1 mol, 7.2 g, 10 ml). The solid obtained after removing the excess 1-methoxy-2-propanol under reduced pressure was recrystallized from mixture of hexane and dichloromethane (1:1).
Hydrogen atoms were placed in calculated positions (C–H 0.96 – 0.98 Å), and were included in refinement in the riding model approximation, with U(H) set to 1.2 to 1.5 times Ueq(C).
Data collection: X-RED32 (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2005); data reduction: X-AREA (Stoe & Cie, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997\bbr00); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[Al4(C3H7O)12] | Dx = 1.128 Mg m−3 |
Mr = 816.95 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, P43212 | Cell parameters from 5826 reflections |
Hall symbol: P 4nw 2abw | θ = 1.8–29.2° |
a = 12.331 (2) Å | µ = 0.15 mm−1 |
c = 31.641 (6) Å | T = 293 K |
V = 4811.1 (14) Å3 | Irregular block, colorless |
Z = 4 | 0.50 × 0.50 × 0.45 mm |
F(000) = 1792 |
Stoe IPDS-II imaging-plate diffractometer | 6434 independent reflections |
Radiation source: medium-focus sealed tube | 5960 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Rotation method scans | θmax = 29.2°, θmin = 1.8° |
Absorption correction: analytical (X-SHAPE; Stoe & Cie, 2003) | h = −16→16 |
Tmin = 0.937, Tmax = 0.955 | k = −5→16 |
15084 measured reflections | l = −35→43 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.098 | w = 1/[σ2(Fo2) + (0.0478P)2 + 1.3524P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
6434 reflections | Δρmax = 0.23 e Å−3 |
236 parameters | Δρmin = −0.28 e Å−3 |
0 restraints | Absolute structure: Flack (Flack, 1983), 2626 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.0 (1) |
[Al4(C3H7O)12] | Z = 4 |
Mr = 816.95 | Mo Kα radiation |
Tetragonal, P43212 | µ = 0.15 mm−1 |
a = 12.331 (2) Å | T = 293 K |
c = 31.641 (6) Å | 0.50 × 0.50 × 0.45 mm |
V = 4811.1 (14) Å3 |
Stoe IPDS-II imaging-plate diffractometer | 6434 independent reflections |
Absorption correction: analytical (X-SHAPE; Stoe & Cie, 2003) | 5960 reflections with I > 2σ(I) |
Tmin = 0.937, Tmax = 0.955 | Rint = 0.035 |
15084 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | H-atom parameters constrained |
wR(F2) = 0.098 | Δρmax = 0.23 e Å−3 |
S = 1.05 | Δρmin = −0.28 e Å−3 |
6434 reflections | Absolute structure: Flack (Flack, 1983), 2626 Friedel pairs |
236 parameters | Absolute structure parameter: 0.0 (1) |
0 restraints |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.20008 (4) | 1.20008 (4) | 0.0000 | 0.02227 (13) | |
Al2 | 0.03496 (4) | 1.03496 (4) | 0.0000 | 0.01840 (12) | |
Al3 | 0.02619 (4) | 0.88003 (4) | 0.067181 (14) | 0.02167 (10) | |
O1 | 0.33153 (10) | 1.16747 (11) | 0.01112 (4) | 0.0313 (3) | |
O2 | 0.09447 (9) | 1.15025 (9) | 0.03410 (3) | 0.0212 (2) | |
O3 | 0.12112 (9) | 0.92722 (9) | 0.02795 (3) | 0.0206 (2) | |
O4 | −0.06114 (9) | 0.97909 (9) | 0.04264 (3) | 0.0213 (2) | |
O5 | 0.04236 (11) | 0.91991 (11) | 0.11805 (4) | 0.0333 (3) | |
O6 | 0.00240 (11) | 0.74607 (10) | 0.05657 (4) | 0.0314 (3) | |
C1 | 0.48650 (17) | 1.27513 (19) | −0.00848 (7) | 0.0456 (5) | |
H1A | 0.4402 | 1.3279 | −0.0216 | 0.068* | |
H1B | 0.5086 | 1.2225 | −0.0291 | 0.068* | |
H1C | 0.5494 | 1.3106 | 0.0029 | 0.068* | |
C2 | 0.42514 (14) | 1.21869 (15) | 0.02697 (6) | 0.0319 (4) | |
H2 | 0.4033 | 1.2731 | 0.0479 | 0.038* | |
C3 | 0.49532 (18) | 1.1342 (2) | 0.04860 (8) | 0.0488 (5) | |
H3A | 0.4546 | 1.0999 | 0.0707 | 0.073* | |
H3B | 0.5583 | 1.1685 | 0.0604 | 0.073* | |
H3C | 0.5175 | 1.0806 | 0.0283 | 0.073* | |
C4 | 0.00339 (18) | 1.28344 (18) | 0.07859 (6) | 0.0395 (4) | |
H4A | −0.0648 | 1.2659 | 0.0656 | 0.059* | |
H4B | 0.0369 | 1.3420 | 0.0635 | 0.059* | |
H4C | −0.0085 | 1.3048 | 0.1074 | 0.059* | |
C5 | 0.07732 (14) | 1.18432 (14) | 0.07744 (5) | 0.0254 (3) | |
H5 | 0.0430 | 1.1251 | 0.0932 | 0.031* | |
C6 | 0.18536 (16) | 1.21142 (16) | 0.09791 (6) | 0.0346 (4) | |
H6A | 0.2316 | 1.1488 | 0.0972 | 0.052* | |
H6B | 0.1736 | 1.2328 | 0.1267 | 0.052* | |
H6C | 0.2192 | 1.2698 | 0.0828 | 0.052* | |
C7 | 0.25561 (15) | 0.79397 (15) | 0.00599 (6) | 0.0322 (4) | |
H7A | 0.2264 | 0.7945 | −0.0221 | 0.048* | |
H7B | 0.2204 | 0.7385 | 0.0223 | 0.048* | |
H7C | 0.3321 | 0.7796 | 0.0048 | 0.048* | |
C8 | 0.23637 (13) | 0.90413 (14) | 0.02667 (5) | 0.0248 (3) | |
H8 | 0.2729 | 0.9603 | 0.0100 | 0.030* | |
C9 | 0.28248 (15) | 0.90408 (17) | 0.07120 (6) | 0.0341 (4) | |
H9A | 0.2702 | 0.9736 | 0.0840 | 0.051* | |
H9B | 0.3590 | 0.8898 | 0.0701 | 0.051* | |
H9C | 0.2474 | 0.8488 | 0.0876 | 0.051* | |
C10 | −0.19215 (17) | 1.0540 (2) | 0.09220 (7) | 0.0432 (5) | |
H10A | −0.1545 | 1.1221 | 0.0911 | 0.065* | |
H10B | −0.1642 | 1.0113 | 0.1151 | 0.065* | |
H10C | −0.2681 | 1.0668 | 0.0965 | 0.065* | |
C11 | −0.17585 (13) | 0.99427 (14) | 0.05127 (5) | 0.0259 (3) | |
H11 | −0.2068 | 1.0382 | 0.0284 | 0.031* | |
C12 | −0.23402 (17) | 0.88716 (19) | 0.05205 (7) | 0.0443 (5) | |
H12A | −0.2225 | 0.8501 | 0.0257 | 0.066* | |
H12B | −0.3102 | 0.8992 | 0.0561 | 0.066* | |
H12C | −0.2064 | 0.8437 | 0.0748 | 0.066* | |
C13 | 0.0016 (2) | 0.8282 (2) | 0.18290 (7) | 0.0537 (6) | |
H13A | −0.0136 | 0.7621 | 0.1680 | 0.081* | |
H13B | −0.0641 | 0.8690 | 0.1862 | 0.081* | |
H13C | 0.0309 | 0.8114 | 0.2102 | 0.081* | |
C14 | 0.08284 (16) | 0.89431 (16) | 0.15819 (5) | 0.0315 (4) | |
H14 | 0.1498 | 0.8523 | 0.1550 | 0.038* | |
C15 | 0.1084 (2) | 0.99959 (18) | 0.18109 (6) | 0.0459 (5) | |
H15A | 0.1598 | 1.0407 | 0.1649 | 0.069* | |
H15B | 0.1386 | 0.9836 | 0.2084 | 0.069* | |
H15C | 0.0430 | 1.0409 | 0.1845 | 0.069* | |
C16 | −0.0992 (2) | 0.58198 (18) | 0.05267 (8) | 0.0489 (5) | |
H16A | −0.1571 | 0.6202 | 0.0389 | 0.073* | |
H16B | −0.1287 | 0.5242 | 0.0694 | 0.073* | |
H16C | −0.0510 | 0.5525 | 0.0318 | 0.073* | |
C17 | −0.03744 (16) | 0.65919 (14) | 0.08080 (6) | 0.0314 (4) | |
H17 | −0.0874 | 0.6881 | 0.1021 | 0.038* | |
C18 | 0.05522 (19) | 0.60221 (18) | 0.10331 (7) | 0.0442 (5) | |
H18A | 0.0930 | 0.6532 | 0.1209 | 0.066* | |
H18B | 0.1044 | 0.5727 | 0.0828 | 0.066* | |
H18C | 0.0268 | 0.5447 | 0.1205 | 0.066* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.02132 (19) | 0.02132 (19) | 0.0242 (3) | −0.0026 (2) | −0.00022 (18) | 0.00022 (18) |
Al2 | 0.01869 (17) | 0.01869 (17) | 0.0178 (3) | 0.0004 (2) | −0.00008 (16) | 0.00008 (16) |
Al3 | 0.0245 (2) | 0.0214 (2) | 0.01904 (19) | 0.00060 (17) | 0.00050 (17) | 0.00200 (16) |
O1 | 0.0229 (6) | 0.0323 (6) | 0.0386 (7) | −0.0037 (5) | −0.0041 (5) | −0.0029 (5) |
O2 | 0.0237 (5) | 0.0206 (5) | 0.0193 (5) | −0.0019 (4) | 0.0000 (4) | −0.0022 (4) |
O3 | 0.0198 (5) | 0.0209 (5) | 0.0213 (5) | 0.0022 (4) | −0.0011 (4) | 0.0016 (4) |
O4 | 0.0204 (5) | 0.0225 (5) | 0.0209 (5) | 0.0007 (4) | 0.0025 (4) | 0.0013 (4) |
O5 | 0.0397 (7) | 0.0402 (7) | 0.0201 (5) | 0.0037 (6) | −0.0025 (5) | 0.0009 (5) |
O6 | 0.0410 (7) | 0.0237 (6) | 0.0295 (6) | −0.0027 (5) | 0.0033 (5) | 0.0044 (5) |
C1 | 0.0304 (10) | 0.0500 (12) | 0.0562 (12) | −0.0068 (8) | 0.0108 (9) | −0.0115 (10) |
C2 | 0.0215 (8) | 0.0356 (9) | 0.0384 (9) | −0.0017 (7) | −0.0023 (7) | −0.0119 (7) |
C3 | 0.0353 (11) | 0.0579 (14) | 0.0533 (12) | 0.0062 (10) | −0.0174 (9) | −0.0117 (11) |
C4 | 0.0455 (11) | 0.0412 (10) | 0.0319 (9) | 0.0118 (9) | 0.0003 (8) | −0.0096 (8) |
C5 | 0.0306 (8) | 0.0250 (8) | 0.0208 (6) | −0.0008 (6) | 0.0015 (6) | −0.0030 (6) |
C6 | 0.0366 (10) | 0.0387 (10) | 0.0285 (8) | −0.0056 (8) | −0.0045 (7) | −0.0086 (7) |
C7 | 0.0305 (9) | 0.0298 (9) | 0.0364 (9) | 0.0072 (7) | 0.0019 (7) | −0.0021 (7) |
C8 | 0.0206 (7) | 0.0262 (8) | 0.0275 (7) | 0.0027 (6) | −0.0006 (6) | 0.0025 (6) |
C9 | 0.0282 (9) | 0.0410 (10) | 0.0330 (8) | 0.0067 (7) | −0.0070 (7) | −0.0021 (7) |
C10 | 0.0310 (10) | 0.0516 (13) | 0.0471 (11) | −0.0002 (8) | 0.0100 (8) | −0.0193 (9) |
C11 | 0.0194 (7) | 0.0303 (8) | 0.0279 (7) | 0.0029 (6) | 0.0030 (6) | 0.0045 (6) |
C12 | 0.0323 (10) | 0.0462 (12) | 0.0545 (12) | −0.0112 (9) | 0.0162 (9) | −0.0144 (10) |
C13 | 0.0759 (17) | 0.0562 (14) | 0.0289 (9) | −0.0167 (12) | 0.0121 (10) | 0.0010 (9) |
C14 | 0.0403 (10) | 0.0345 (9) | 0.0197 (7) | 0.0013 (7) | −0.0013 (7) | 0.0020 (6) |
C15 | 0.0611 (14) | 0.0456 (11) | 0.0311 (8) | −0.0035 (10) | −0.0083 (9) | −0.0058 (8) |
C16 | 0.0571 (14) | 0.0316 (10) | 0.0581 (13) | −0.0116 (10) | −0.0023 (11) | 0.0011 (10) |
C17 | 0.0388 (10) | 0.0233 (8) | 0.0319 (8) | −0.0007 (7) | 0.0063 (7) | 0.0046 (6) |
C18 | 0.0532 (13) | 0.0340 (10) | 0.0454 (11) | 0.0064 (9) | 0.0025 (10) | 0.0110 (9) |
Al1—O1i | 1.7066 (13) | C6—H6B | 0.9600 |
Al1—O1 | 1.7066 (13) | C6—H6C | 0.9600 |
Al1—O2 | 1.7994 (12) | C7—C8 | 1.526 (2) |
Al1—O2i | 1.7994 (12) | C7—H7A | 0.9600 |
Al1—Al2 | 2.8794 (9) | C7—H7B | 0.9600 |
Al2—O3i | 1.9172 (11) | C7—H7C | 0.9600 |
Al2—O3 | 1.9172 (11) | C8—C9 | 1.519 (2) |
Al2—O4 | 1.9234 (11) | C8—H8 | 0.9800 |
Al2—O4i | 1.9234 (11) | C9—H9A | 0.9600 |
Al2—O2 | 1.9297 (12) | C9—H9B | 0.9600 |
Al2—O2i | 1.9297 (12) | C9—H9C | 0.9600 |
Al2—Al3i | 2.8601 (7) | C10—C11 | 1.503 (2) |
Al2—Al3 | 2.8601 (6) | C10—H10A | 0.9600 |
Al3—O5 | 1.6946 (13) | C10—H10B | 0.9600 |
Al3—O6 | 1.7110 (14) | C10—H10C | 0.9600 |
Al3—O4 | 1.8039 (12) | C11—C12 | 1.503 (3) |
Al3—O3 | 1.8027 (12) | C11—H11 | 0.9800 |
O1—C2 | 1.408 (2) | C12—H12A | 0.9600 |
O2—C5 | 1.4496 (18) | C12—H12B | 0.9600 |
O3—C8 | 1.4499 (19) | C12—H12C | 0.9600 |
O4—C11 | 1.4527 (19) | C13—C14 | 1.509 (3) |
O5—C14 | 1.4007 (19) | C13—H13A | 0.9600 |
O6—C17 | 1.406 (2) | C13—H13B | 0.9600 |
C1—C2 | 1.522 (3) | C13—H13C | 0.9600 |
C1—H1A | 0.9600 | C14—C15 | 1.520 (3) |
C1—H1B | 0.9600 | C14—H14 | 0.9800 |
C1—H1C | 0.9600 | C15—H15A | 0.9600 |
C2—C3 | 1.518 (3) | C15—H15B | 0.9600 |
C2—H2 | 0.9800 | C15—H15C | 0.9600 |
C3—H3A | 0.9600 | C16—C17 | 1.509 (3) |
C3—H3B | 0.9600 | C16—H16A | 0.9600 |
C3—H3C | 0.9600 | C16—H16B | 0.9600 |
C4—C5 | 1.525 (3) | C16—H16C | 0.9600 |
C4—H4A | 0.9600 | C17—C18 | 1.519 (3) |
C4—H4B | 0.9600 | C17—H17 | 0.9800 |
C4—H4C | 0.9600 | C18—H18A | 0.9600 |
C5—C6 | 1.519 (2) | C18—H18B | 0.9600 |
C5—H5 | 0.9800 | C18—H18C | 0.9600 |
C6—H6A | 0.9600 | ||
O1i—Al1—O1 | 119.34 (9) | H4A—C4—H4B | 109.5 |
O1i—Al1—O2 | 106.11 (6) | C5—C4—H4C | 109.5 |
O1—Al1—O2 | 118.89 (6) | H4A—C4—H4C | 109.5 |
O1i—Al1—O2i | 118.89 (6) | H4B—C4—H4C | 109.5 |
O1—Al1—O2i | 106.11 (6) | O2—C5—C6 | 109.83 (14) |
O2—Al1—O2i | 82.26 (7) | O2—C5—C4 | 110.00 (14) |
O1i—Al1—Al2 | 120.33 (5) | C6—C5—C4 | 109.74 (15) |
O1—Al1—Al2 | 120.33 (5) | O2—C5—H5 | 109.1 |
O2—Al1—Al2 | 41.13 (4) | C6—C5—H5 | 109.1 |
O2i—Al1—Al2 | 41.13 (4) | C4—C5—H5 | 109.1 |
O3i—Al2—O3 | 168.73 (8) | C5—C6—H6A | 109.5 |
O3i—Al2—O4 | 95.46 (5) | C5—C6—H6B | 109.5 |
O3—Al2—O4 | 76.68 (5) | H6A—C6—H6B | 109.5 |
O3i—Al2—O4i | 76.68 (5) | C5—C6—H6C | 109.5 |
O3—Al2—O4i | 95.46 (5) | H6A—C6—H6C | 109.5 |
O4—Al2—O4i | 92.91 (7) | H6B—C6—H6C | 109.5 |
O3i—Al2—O2 | 96.50 (5) | C8—C7—H7A | 109.5 |
O3—Al2—O2 | 92.40 (5) | C8—C7—H7B | 109.5 |
O4—Al2—O2 | 96.08 (5) | H7A—C7—H7B | 109.5 |
O4i—Al2—O2 | 169.22 (5) | C8—C7—H7C | 109.5 |
O3i—Al2—O2i | 92.40 (5) | H7A—C7—H7C | 109.5 |
O3—Al2—O2i | 96.50 (5) | H7B—C7—H7C | 109.5 |
O4—Al2—O2i | 169.22 (5) | O3—C8—C9 | 109.93 (13) |
O4i—Al2—O2i | 96.08 (5) | O3—C8—C7 | 109.82 (14) |
O2—Al2—O2i | 75.67 (7) | C9—C8—C7 | 109.82 (14) |
O3i—Al2—Al3i | 38.30 (3) | O3—C8—H8 | 109.1 |
O3—Al2—Al3i | 133.38 (4) | C9—C8—H8 | 109.1 |
O4—Al2—Al3i | 95.53 (4) | C7—C8—H8 | 109.1 |
O4i—Al2—Al3i | 38.38 (3) | C8—C9—H9A | 109.5 |
O2—Al2—Al3i | 134.23 (4) | C8—C9—H9B | 109.5 |
O2i—Al2—Al3i | 95.21 (4) | H9A—C9—H9B | 109.5 |
O3i—Al2—Al3 | 133.38 (4) | C8—C9—H9C | 109.5 |
O3—Al2—Al3 | 38.30 (3) | H9A—C9—H9C | 109.5 |
O4—Al2—Al3 | 38.38 (3) | H9B—C9—H9C | 109.5 |
O4i—Al2—Al3 | 95.53 (4) | C11—C10—H10A | 109.5 |
O2—Al2—Al3 | 95.21 (3) | C11—C10—H10B | 109.5 |
O2i—Al2—Al3 | 134.23 (4) | H10A—C10—H10B | 109.5 |
Al3i—Al2—Al3 | 120.12 (3) | C11—C10—H10C | 109.5 |
O3i—Al2—Al1 | 95.63 (4) | H10A—C10—H10C | 109.5 |
O3—Al2—Al1 | 95.63 (4) | H10B—C10—H10C | 109.5 |
O4—Al2—Al1 | 133.55 (4) | O4—C11—C10 | 110.79 (14) |
O4i—Al2—Al1 | 133.55 (4) | O4—C11—C12 | 110.76 (14) |
O2—Al2—Al1 | 37.83 (3) | C10—C11—C12 | 110.65 (16) |
O2i—Al2—Al1 | 37.83 (3) | O4—C11—H11 | 108.2 |
Al3i—Al2—Al1 | 119.938 (16) | C10—C11—H11 | 108.2 |
Al3—Al2—Al1 | 119.938 (15) | C12—C11—H11 | 108.2 |
O5—Al3—O6 | 119.13 (7) | C11—C12—H12A | 109.5 |
O5—Al3—O4 | 106.41 (6) | C11—C12—H12B | 109.5 |
O6—Al3—O4 | 117.83 (6) | H12A—C12—H12B | 109.5 |
O5—Al3—O3 | 118.94 (7) | C11—C12—H12C | 109.5 |
O6—Al3—O3 | 106.72 (6) | H12A—C12—H12C | 109.5 |
O4—Al3—O3 | 82.69 (5) | H12B—C12—H12C | 109.5 |
O5—Al3—Al2 | 120.50 (5) | C14—C13—H13A | 109.5 |
O6—Al3—Al2 | 120.36 (5) | C14—C13—H13B | 109.5 |
O4—Al3—Al2 | 41.45 (4) | H13A—C13—H13B | 109.5 |
O3—Al3—Al2 | 41.24 (4) | C14—C13—H13C | 109.5 |
C2—O1—Al1 | 138.27 (12) | H13A—C13—H13C | 109.5 |
C5—O2—Al1 | 125.02 (10) | H13B—C13—H13C | 109.5 |
C5—O2—Al2 | 133.39 (10) | O5—C14—C13 | 110.79 (17) |
Al1—O2—Al2 | 101.03 (5) | O5—C14—C15 | 108.29 (16) |
C8—O3—Al3 | 126.32 (10) | C13—C14—C15 | 110.60 (17) |
C8—O3—Al2 | 131.78 (10) | O5—C14—H14 | 109.0 |
Al3—O3—Al2 | 100.46 (6) | C13—C14—H14 | 109.0 |
C11—O4—Al3 | 125.99 (10) | C15—C14—H14 | 109.0 |
C11—O4—Al2 | 133.27 (9) | C14—C15—H15A | 109.5 |
Al3—O4—Al2 | 100.18 (5) | C14—C15—H15B | 109.5 |
C14—O5—Al3 | 146.90 (13) | H15A—C15—H15B | 109.5 |
C17—O6—Al3 | 133.51 (12) | C14—C15—H15C | 109.5 |
C2—C1—H1A | 109.5 | H15A—C15—H15C | 109.5 |
C2—C1—H1B | 109.5 | H15B—C15—H15C | 109.5 |
H1A—C1—H1B | 109.5 | C17—C16—H16A | 109.5 |
C2—C1—H1C | 109.5 | C17—C16—H16B | 109.5 |
H1A—C1—H1C | 109.5 | H16A—C16—H16B | 109.5 |
H1B—C1—H1C | 109.5 | C17—C16—H16C | 109.5 |
O1—C2—C3 | 108.66 (16) | H16A—C16—H16C | 109.5 |
O1—C2—C1 | 110.51 (16) | H16B—C16—H16C | 109.5 |
C3—C2—C1 | 111.28 (17) | O6—C17—C16 | 109.60 (16) |
O1—C2—H2 | 108.8 | O6—C17—C18 | 110.21 (16) |
C3—C2—H2 | 108.8 | C16—C17—C18 | 111.36 (17) |
C1—C2—H2 | 108.8 | O6—C17—H17 | 108.5 |
C2—C3—H3A | 109.5 | C16—C17—H17 | 108.5 |
C2—C3—H3B | 109.5 | C18—C17—H17 | 108.5 |
H3A—C3—H3B | 109.5 | C17—C18—H18A | 109.5 |
C2—C3—H3C | 109.5 | C17—C18—H18B | 109.5 |
H3A—C3—H3C | 109.5 | H18A—C18—H18B | 109.5 |
H3B—C3—H3C | 109.5 | C17—C18—H18C | 109.5 |
C5—C4—H4A | 109.5 | H18A—C18—H18C | 109.5 |
C5—C4—H4B | 109.5 | H18B—C18—H18C | 109.5 |
O1i—Al1—Al2—O3i | 13.79 (6) | Al1—Al2—O2—C5 | −171.47 (17) |
O1—Al1—Al2—O3i | −166.21 (6) | O3i—Al2—O2—Al1 | −90.82 (6) |
O2—Al1—Al2—O3i | 93.36 (6) | O3—Al2—O2—Al1 | 96.10 (5) |
O2i—Al1—Al2—O3i | −86.64 (6) | O4—Al2—O2—Al1 | 172.95 (5) |
O1i—Al1—Al2—O3 | −166.21 (6) | O4i—Al2—O2—Al1 | −40.7 (3) |
O1—Al1—Al2—O3 | 13.79 (6) | O2i—Al2—O2—Al1 | 0.0 |
O2—Al1—Al2—O3 | −86.64 (6) | Al3i—Al2—O2—Al1 | −83.23 (6) |
O2i—Al1—Al2—O3 | 93.36 (6) | Al3—Al2—O2—Al1 | 134.39 (4) |
O1i—Al1—Al2—O4 | −89.25 (7) | O5—Al3—O3—C8 | 63.16 (14) |
O1—Al1—Al2—O4 | 90.75 (7) | O6—Al3—O3—C8 | −75.17 (13) |
O2—Al1—Al2—O4 | −9.69 (7) | O4—Al3—O3—C8 | 167.90 (12) |
O2i—Al1—Al2—O4 | 170.31 (7) | Al2—Al3—O3—C8 | 167.58 (15) |
O1i—Al1—Al2—O4i | 90.75 (7) | O5—Al3—O3—Al2 | −104.43 (7) |
O1—Al1—Al2—O4i | −89.25 (7) | O6—Al3—O3—Al2 | 117.25 (6) |
O2—Al1—Al2—O4i | 170.31 (7) | O4—Al3—O3—Al2 | 0.32 (5) |
O2i—Al1—Al2—O4i | −9.69 (7) | O3i—Al2—O3—C8 | 146.61 (13) |
O1i—Al1—Al2—O2 | −79.57 (7) | O4—Al2—O3—C8 | −166.87 (13) |
O1—Al1—Al2—O2 | 100.43 (7) | O4i—Al2—O3—C8 | 101.43 (13) |
O2i—Al1—Al2—O2 | 180.0 | O2—Al2—O3—C8 | −71.19 (13) |
O1i—Al1—Al2—O2i | 100.43 (7) | O2i—Al2—O3—C8 | 4.65 (13) |
O1—Al1—Al2—O2i | −79.57 (7) | Al3i—Al2—O3—C8 | 108.15 (13) |
O2—Al1—Al2—O2i | 180.0 | Al3—Al2—O3—C8 | −166.57 (16) |
O1i—Al1—Al2—Al3i | 45.23 (5) | Al1—Al2—O3—C8 | −33.39 (13) |
O1—Al1—Al2—Al3i | −134.77 (5) | O3i—Al2—O3—Al3 | −46.8 (2) |
O2—Al1—Al2—Al3i | 124.80 (6) | O4—Al2—O3—Al3 | −0.30 (5) |
O2i—Al1—Al2—Al3i | −55.20 (6) | O4i—Al2—O3—Al3 | −92.01 (6) |
O1i—Al1—Al2—Al3 | −134.77 (5) | O2—Al2—O3—Al3 | 95.38 (6) |
O1—Al1—Al2—Al3 | 45.23 (5) | O2i—Al2—O3—Al3 | 171.22 (5) |
O2—Al1—Al2—Al3 | −55.20 (6) | Al3i—Al2—O3—Al3 | −85.28 (6) |
O2i—Al1—Al2—Al3 | 124.80 (6) | Al1—Al2—O3—Al3 | 133.17 (4) |
O3i—Al2—Al3—O5 | −90.94 (8) | O5—Al3—O4—C11 | −69.86 (13) |
O3—Al2—Al3—O5 | 100.37 (8) | O6—Al3—O4—C11 | 66.96 (13) |
O4—Al2—Al3—O5 | −80.11 (8) | O3—Al3—O4—C11 | 172.05 (12) |
O4i—Al2—Al3—O5 | −167.81 (7) | Al2—Al3—O4—C11 | 172.37 (15) |
O2—Al2—Al3—O5 | 13.10 (7) | O5—Al3—O4—Al2 | 117.77 (7) |
O2i—Al2—Al3—O5 | 88.15 (8) | O6—Al3—O4—Al2 | −105.41 (7) |
Al3i—Al2—Al3—O5 | −136.51 (6) | O3—Al3—O4—Al2 | −0.32 (5) |
Al1—Al2—Al3—O5 | 43.49 (6) | O3i—Al2—O4—C11 | 0.60 (14) |
O3i—Al2—Al3—O6 | 88.04 (8) | O3—Al2—O4—C11 | −171.21 (14) |
O3—Al2—Al3—O6 | −80.66 (8) | O4i—Al2—O4—C11 | −76.28 (13) |
O4—Al2—Al3—O6 | 98.86 (8) | O2—Al2—O4—C11 | 97.76 (14) |
O4i—Al2—Al3—O6 | 11.16 (7) | O2i—Al2—O4—C11 | 137.2 (2) |
O2—Al2—Al3—O6 | −167.92 (7) | Al3i—Al2—O4—C11 | −37.88 (13) |
O2i—Al2—Al3—O6 | −92.88 (8) | Al3—Al2—O4—C11 | −171.51 (16) |
Al3i—Al2—Al3—O6 | 42.46 (6) | Al1—Al2—O4—C11 | 103.72 (13) |
Al1—Al2—Al3—O6 | −137.54 (6) | O3i—Al2—O4—Al3 | 172.12 (5) |
O3i—Al2—Al3—O4 | −10.83 (7) | O3—Al2—O4—Al3 | 0.30 (5) |
O3—Al2—Al3—O4 | −179.52 (8) | O4i—Al2—O4—Al3 | 95.23 (6) |
O4i—Al2—Al3—O4 | −87.70 (8) | O2—Al2—O4—Al3 | −90.73 (5) |
O2—Al2—Al3—O4 | 93.21 (6) | O2i—Al2—O4—Al3 | −51.3 (3) |
O2i—Al2—Al3—O4 | 168.26 (8) | Al3i—Al2—O4—Al3 | 133.63 (4) |
Al3i—Al2—Al3—O4 | −56.40 (5) | Al1—Al2—O4—Al3 | −84.77 (6) |
Al1—Al2—Al3—O4 | 123.60 (5) | O6—Al3—O5—C14 | 35.9 (3) |
O3i—Al2—Al3—O3 | 168.70 (7) | O4—Al3—O5—C14 | 172.1 (2) |
O4—Al2—Al3—O3 | 179.52 (8) | O3—Al3—O5—C14 | −97.3 (2) |
O4i—Al2—Al3—O3 | 91.82 (6) | Al2—Al3—O5—C14 | −145.1 (2) |
O2—Al2—Al3—O3 | −87.26 (7) | O5—Al3—O6—C17 | 21.18 (19) |
O2i—Al2—Al3—O3 | −12.22 (7) | O4—Al3—O6—C17 | −110.12 (16) |
Al3i—Al2—Al3—O3 | 123.12 (6) | O3—Al3—O6—C17 | 159.41 (16) |
Al1—Al2—Al3—O3 | −56.88 (6) | Al2—Al3—O6—C17 | −157.81 (15) |
O1i—Al1—O1—C2 | 25.16 (16) | Al1—O1—C2—C3 | 152.14 (16) |
O2—Al1—O1—C2 | −107.20 (18) | Al1—O1—C2—C1 | −85.5 (2) |
O2i—Al1—O1—C2 | 162.84 (17) | Al1—O2—C5—C6 | −32.61 (18) |
Al2—Al1—O1—C2 | −154.84 (16) | Al2—O2—C5—C6 | 137.16 (13) |
O1i—Al1—O2—C5 | −69.64 (13) | Al1—O2—C5—C4 | 88.28 (16) |
O1—Al1—O2—C5 | 68.26 (13) | Al2—O2—C5—C4 | −101.95 (17) |
O2i—Al1—O2—C5 | 172.44 (15) | Al3—O3—C8—C9 | −37.91 (19) |
Al2—Al1—O2—C5 | 172.44 (15) | Al2—O3—C8—C9 | 125.61 (13) |
O1i—Al1—O2—Al2 | 117.92 (6) | Al3—O3—C8—C7 | 83.03 (15) |
O1—Al1—O2—Al2 | −104.18 (7) | Al2—O3—C8—C7 | −113.45 (14) |
O2i—Al1—O2—Al2 | 0.0 | Al3—O4—C11—C10 | 77.18 (18) |
O3i—Al2—O2—C5 | 97.71 (14) | Al2—O4—C11—C10 | −113.17 (16) |
O3—Al2—O2—C5 | −75.37 (14) | Al3—O4—C11—C12 | −46.01 (19) |
O4—Al2—O2—C5 | 1.48 (14) | Al2—O4—C11—C12 | 123.65 (15) |
O4i—Al2—O2—C5 | 147.8 (2) | Al3—O5—C14—C13 | −85.5 (3) |
O2i—Al2—O2—C5 | −171.47 (17) | Al3—O5—C14—C15 | 153.1 (2) |
Al3i—Al2—O2—C5 | 105.30 (13) | Al3—O6—C17—C16 | 148.14 (16) |
Al3—Al2—O2—C5 | −37.08 (14) | Al3—O6—C17—C18 | −89.0 (2) |
Symmetry code: (i) y−1, x+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Al4(C3H7O)12] |
Mr | 816.95 |
Crystal system, space group | Tetragonal, P43212 |
Temperature (K) | 293 |
a, c (Å) | 12.331 (2), 31.641 (6) |
V (Å3) | 4811.1 (14) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.15 |
Crystal size (mm) | 0.50 × 0.50 × 0.45 |
Data collection | |
Diffractometer | Stoe IPDS-II imaging-plate diffractometer |
Absorption correction | Analytical (X-SHAPE; Stoe & Cie, 2003) |
Tmin, Tmax | 0.937, 0.955 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15084, 6434, 5960 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.686 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.098, 1.05 |
No. of reflections | 6434 |
No. of parameters | 236 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.23, −0.28 |
Absolute structure | Flack (Flack, 1983), 2626 Friedel pairs |
Absolute structure parameter | 0.0 (1) |
Computer programs: X-RED32 (Stoe & Cie, 2001), X-AREA (Stoe & Cie, 2005), SHELXS97 (Sheldrick, 1997\bbr00), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
Some achiral metal-organic compounds crystallize in one of the eleven pairs of enantiomorphic space groups; however, examples of the same compound belonging to one of each pair are rare. There is a short comment on such examples (Ng, 2007).