Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011523/dn6136sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011523/dn6136Isup2.hkl |
CCDC reference: 245267
Data collection: APEX2 (Bruker–Nonius, 2004); cell refinement: APEX2 and SAINT (Bruker–Nonius, 2004); data reduction: SAINT and XPREP (Sheldrick, 2003); program(s) used to solve structure: XS (Sheldrick, 2001); program(s) used to refine structure: XL (Sheldrick, 2001); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: XCIF (Sheldrick, 2001).
[Al4(CH3)6O2(C25H21O2P2)2]·2C4H8O | F(000) = 1112 |
Mr = 1205.12 | Dx = 1.234 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5174 reflections |
a = 13.0087 (2) Å | θ = 2.2–23.8° |
b = 18.5644 (3) Å | µ = 0.22 mm−1 |
c = 13.7312 (2) Å | T = 100 K |
β = 102.117 (1)° | Cube, colorless |
V = 3242.19 (9) Å3 | 0.19 × 0.14 × 0.14 mm |
Z = 2 |
Bruker SMART APEX CCD area-detector diffractometer | 6623 independent reflections |
Radiation source: fine-focus sealed tube, Siemens KFFMO2K-90 | 5264 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
Detector resolution: 8.33 pixels mm-1 | θmax = 26.4°, θmin = 1.9° |
φ and ω scans | h = −16→13 |
Absorption correction: multi-scan (Blessing, 1995) | k = −23→23 |
Tmin = 0.960, Tmax = 0.971 | l = −17→17 |
47479 measured reflections |
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)] = 0.062 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.173 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0936P)2 + 2.8045P] where P = (Fo2 + 2Fc2)/3 |
6623 reflections | (Δ/σ)max = 0.002 |
323 parameters | Δρmax = 0.89 e Å−3 |
0 restraints | Δρmin = −0.38 e Å−3 |
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. Asymetric unit is one half molecule of [Me6Al4(µ3-O)2{µ- (Ph2P(O))2CH}2] and one molecule of THF. The solvent molecule THF was completely disordered and was modelled with spek's SQUEEZE (Spek 2003). 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 | 0.51781 (7) | 0.13590 (5) | −0.11532 (6) | 0.0421 (2) | |
Al2 | 0.46736 (6) | 0.03576 (4) | 0.06943 (6) | 0.0316 (2) | |
O1 | 0.64524 (18) | 0.17197 (12) | −0.05762 (14) | 0.0479 (5) | |
O2 | 0.56631 (16) | 0.06409 (11) | 0.16889 (13) | 0.0424 (5) | |
O3 | 0.50657 (14) | 0.05647 (10) | −0.04522 (13) | 0.0326 (4) | |
P1 | 0.70468 (6) | 0.20492 (4) | 0.04047 (5) | 0.03228 (19) | |
P2 | 0.64366 (5) | 0.12372 (4) | 0.21474 (5) | 0.03026 (18) | |
C1 | 0.7173 (2) | 0.29943 (14) | 0.0162 (2) | 0.0356 (6) | |
C2 | 0.7097 (3) | 0.32284 (18) | −0.0811 (2) | 0.0494 (8) | |
H2 | 0.6966 | 0.2891 | −0.1343 | 0.059* | |
C3 | 0.7211 (3) | 0.39511 (19) | −0.1007 (3) | 0.0597 (9) | |
H3 | 0.7163 | 0.4108 | −0.1674 | 0.072* | |
C4 | 0.7392 (3) | 0.44428 (18) | −0.0248 (3) | 0.0576 (9) | |
H4 | 0.7459 | 0.4939 | −0.0390 | 0.069* | |
C5 | 0.7476 (3) | 0.42214 (17) | 0.0710 (3) | 0.0529 (8) | |
H5 | 0.7608 | 0.4564 | 0.1236 | 0.063* | |
C6 | 0.7370 (2) | 0.34969 (15) | 0.0925 (2) | 0.0433 (7) | |
H6 | 0.7432 | 0.3346 | 0.1596 | 0.052* | |
C7 | 0.8343 (2) | 0.16606 (14) | 0.0614 (2) | 0.0389 (6) | |
C8 | 0.9078 (2) | 0.18236 (17) | 0.1462 (3) | 0.0472 (8) | |
H8 | 0.8904 | 0.2146 | 0.1940 | 0.057* | |
C9 | 1.0078 (3) | 0.1517 (2) | 0.1620 (4) | 0.0713 (12) | |
H9 | 1.0585 | 0.1618 | 0.2210 | 0.086* | |
C10 | 1.0322 (4) | 0.1057 (2) | 0.0895 (5) | 0.0806 (15) | |
H10 | 1.0999 | 0.0842 | 0.0996 | 0.097* | |
C11 | 0.9596 (4) | 0.0913 (2) | 0.0043 (4) | 0.0784 (14) | |
H11 | 0.9781 | 0.0608 | −0.0449 | 0.094* | |
C12 | 0.8602 (3) | 0.12035 (17) | −0.0110 (3) | 0.0590 (10) | |
H12 | 0.8098 | 0.1096 | −0.0700 | 0.071* | |
C13 | 0.6535 (2) | 0.19737 (15) | 0.1443 (2) | 0.0317 (6) | |
H13 | 0.605 (2) | 0.2308 (17) | 0.145 (2) | 0.036 (8)* | |
C14 | 0.6001 (2) | 0.15336 (19) | 0.3241 (2) | 0.0436 (7) | |
C15 | 0.6247 (3) | 0.2223 (2) | 0.3621 (3) | 0.0656 (11) | |
H15 | 0.6647 | 0.2539 | 0.3302 | 0.079* | |
C16 | 0.5913 (5) | 0.2448 (3) | 0.4463 (3) | 0.0986 (18) | |
H16 | 0.6087 | 0.2917 | 0.4724 | 0.118* | |
C17 | 0.5330 (5) | 0.1995 (3) | 0.4921 (3) | 0.0986 (18) | |
H17 | 0.5097 | 0.2153 | 0.5497 | 0.118* | |
C18 | 0.5082 (3) | 0.1319 (3) | 0.4556 (3) | 0.0830 (15) | |
H18 | 0.4668 | 0.1013 | 0.4875 | 0.100* | |
C19 | 0.5435 (3) | 0.1067 (2) | 0.3707 (2) | 0.0601 (10) | |
H19 | 0.5285 | 0.0590 | 0.3467 | 0.072* | |
C20 | 0.7668 (2) | 0.07750 (14) | 0.2565 (2) | 0.0338 (6) | |
C21 | 0.8358 (2) | 0.09901 (15) | 0.3430 (2) | 0.0406 (7) | |
H21 | 0.8180 | 0.1382 | 0.3807 | 0.049* | |
C22 | 0.9305 (3) | 0.06327 (18) | 0.3744 (3) | 0.0536 (8) | |
H22 | 0.9777 | 0.0777 | 0.4337 | 0.064* | |
C23 | 0.9557 (3) | 0.00615 (19) | 0.3182 (3) | 0.0607 (10) | |
H23 | 1.0209 | −0.0182 | 0.3390 | 0.073* | |
C24 | 0.8872 (3) | −0.01546 (18) | 0.2329 (3) | 0.0586 (9) | |
H24 | 0.9053 | −0.0545 | 0.1951 | 0.070* | |
C25 | 0.7923 (3) | 0.01930 (17) | 0.2019 (2) | 0.0466 (7) | |
H25 | 0.7445 | 0.0037 | 0.1436 | 0.056* | |
C26 | 0.3262 (2) | 0.05986 (19) | 0.0857 (3) | 0.0507 (8) | |
H26A | 0.3167 | 0.0430 | 0.1509 | 0.076* | |
H26B | 0.2743 | 0.0365 | 0.0331 | 0.076* | |
H26C | 0.3164 | 0.1122 | 0.0813 | 0.076* | |
C27 | 0.5275 (3) | 0.1071 (2) | −0.2506 (2) | 0.0664 (11) | |
H27A | 0.5825 | 0.0705 | −0.2470 | 0.100* | |
H27B | 0.5450 | 0.1492 | −0.2870 | 0.100* | |
H27C | 0.4600 | 0.0872 | −0.2852 | 0.100* | |
C28 | 0.4081 (4) | 0.2038 (3) | −0.0984 (4) | 0.0979 (17) | |
H28A | 0.3400 | 0.1871 | −0.1365 | 0.147* | |
H28B | 0.4237 | 0.2515 | −0.1224 | 0.147* | |
H28C | 0.4055 | 0.2069 | −0.0277 | 0.147* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.0455 (5) | 0.0409 (5) | 0.0361 (5) | −0.0053 (4) | −0.0005 (4) | 0.0123 (4) |
Al2 | 0.0279 (4) | 0.0364 (4) | 0.0314 (4) | −0.0047 (3) | 0.0084 (3) | −0.0020 (3) |
O1 | 0.0628 (14) | 0.0473 (12) | 0.0338 (10) | −0.0259 (11) | 0.0105 (10) | −0.0045 (9) |
O2 | 0.0472 (12) | 0.0508 (12) | 0.0284 (9) | −0.0216 (10) | 0.0064 (8) | −0.0009 (9) |
O3 | 0.0336 (10) | 0.0347 (10) | 0.0285 (9) | −0.0061 (8) | 0.0039 (7) | 0.0038 (8) |
P1 | 0.0373 (4) | 0.0279 (3) | 0.0318 (4) | −0.0059 (3) | 0.0077 (3) | −0.0021 (3) |
P2 | 0.0298 (3) | 0.0358 (4) | 0.0257 (3) | −0.0043 (3) | 0.0071 (3) | −0.0037 (3) |
C1 | 0.0311 (14) | 0.0304 (13) | 0.0434 (15) | −0.0012 (11) | 0.0038 (11) | 0.0034 (12) |
C2 | 0.0558 (19) | 0.0454 (18) | 0.0426 (16) | −0.0094 (15) | 0.0001 (14) | 0.0062 (14) |
C3 | 0.064 (2) | 0.0485 (19) | 0.060 (2) | −0.0070 (17) | −0.0021 (17) | 0.0210 (17) |
C4 | 0.0483 (19) | 0.0344 (16) | 0.087 (3) | 0.0019 (14) | 0.0081 (18) | 0.0144 (17) |
C5 | 0.0523 (19) | 0.0317 (15) | 0.073 (2) | 0.0036 (14) | 0.0091 (17) | −0.0065 (16) |
C6 | 0.0482 (17) | 0.0319 (15) | 0.0481 (17) | 0.0014 (13) | 0.0061 (14) | −0.0021 (13) |
C7 | 0.0438 (16) | 0.0254 (13) | 0.0536 (17) | −0.0001 (12) | 0.0239 (14) | 0.0045 (12) |
C8 | 0.0347 (15) | 0.0385 (16) | 0.072 (2) | 0.0049 (12) | 0.0191 (15) | 0.0164 (15) |
C9 | 0.0389 (18) | 0.065 (2) | 0.110 (3) | 0.0055 (17) | 0.016 (2) | 0.038 (2) |
C10 | 0.060 (2) | 0.061 (2) | 0.138 (4) | 0.031 (2) | 0.060 (3) | 0.045 (3) |
C11 | 0.095 (3) | 0.050 (2) | 0.112 (4) | 0.026 (2) | 0.070 (3) | 0.021 (2) |
C12 | 0.082 (3) | 0.0340 (16) | 0.075 (2) | 0.0078 (16) | 0.049 (2) | 0.0034 (16) |
C13 | 0.0272 (13) | 0.0327 (14) | 0.0345 (13) | 0.0024 (11) | 0.0050 (10) | −0.0007 (11) |
C14 | 0.0358 (15) | 0.067 (2) | 0.0288 (13) | 0.0121 (14) | 0.0090 (11) | −0.0006 (14) |
C15 | 0.093 (3) | 0.061 (2) | 0.0460 (19) | 0.026 (2) | 0.0209 (19) | −0.0101 (17) |
C16 | 0.161 (5) | 0.091 (3) | 0.052 (2) | 0.053 (4) | 0.041 (3) | −0.007 (2) |
C17 | 0.120 (4) | 0.125 (5) | 0.060 (3) | 0.056 (4) | 0.040 (3) | −0.012 (3) |
C18 | 0.058 (2) | 0.154 (5) | 0.042 (2) | 0.008 (3) | 0.0221 (17) | 0.017 (3) |
C19 | 0.0472 (19) | 0.099 (3) | 0.0355 (16) | −0.0003 (19) | 0.0129 (14) | −0.0004 (17) |
C20 | 0.0382 (15) | 0.0277 (13) | 0.0381 (14) | −0.0005 (11) | 0.0141 (11) | 0.0020 (11) |
C21 | 0.0371 (15) | 0.0290 (14) | 0.0529 (17) | −0.0001 (11) | 0.0030 (13) | 0.0044 (12) |
C22 | 0.0414 (17) | 0.0441 (18) | 0.070 (2) | 0.0024 (14) | −0.0005 (16) | 0.0114 (16) |
C23 | 0.0450 (19) | 0.0461 (19) | 0.093 (3) | 0.0141 (15) | 0.0179 (19) | 0.0191 (19) |
C24 | 0.065 (2) | 0.0400 (17) | 0.078 (3) | 0.0121 (16) | 0.032 (2) | 0.0006 (17) |
C25 | 0.0535 (18) | 0.0419 (17) | 0.0477 (17) | 0.0022 (14) | 0.0182 (14) | −0.0059 (14) |
C26 | 0.0391 (17) | 0.055 (2) | 0.062 (2) | −0.0013 (14) | 0.0213 (15) | −0.0110 (16) |
C27 | 0.075 (2) | 0.085 (3) | 0.0321 (16) | −0.039 (2) | −0.0045 (16) | 0.0118 (17) |
C28 | 0.103 (4) | 0.081 (3) | 0.112 (4) | 0.049 (3) | 0.029 (3) | 0.049 (3) |
Al1—O3 | 1.7837 (19) | C10—H10 | 0.9500 |
Al1—O1 | 1.809 (2) | C11—C12 | 1.377 (6) |
Al1—C28 | 1.955 (5) | C11—H11 | 0.9500 |
Al1—C27 | 1.962 (4) | C12—H12 | 0.9500 |
Al2—O2 | 1.750 (2) | C13—H13 | 0.88 (3) |
Al2—O3i | 1.790 (2) | C14—C19 | 1.378 (5) |
Al2—O3 | 1.7955 (19) | C14—C15 | 1.394 (5) |
Al2—C26 | 1.948 (3) | C15—C16 | 1.383 (5) |
Al2—Al2i | 2.6075 (16) | C15—H15 | 0.9500 |
O1—P1 | 1.533 (2) | C16—C17 | 1.370 (8) |
O2—P2 | 1.5390 (19) | C16—H16 | 0.9500 |
O3—Al2i | 1.790 (2) | C17—C18 | 1.365 (7) |
P1—C13 | 1.701 (3) | C17—H17 | 0.9500 |
P1—C1 | 1.800 (3) | C18—C19 | 1.420 (5) |
P1—C7 | 1.800 (3) | C18—H18 | 0.9500 |
P2—C13 | 1.695 (3) | C19—H19 | 0.9500 |
P2—C14 | 1.799 (3) | C20—C21 | 1.388 (4) |
P2—C20 | 1.802 (3) | C20—C25 | 1.394 (4) |
C1—C6 | 1.385 (4) | C21—C22 | 1.386 (4) |
C1—C2 | 1.389 (4) | C21—H21 | 0.9500 |
C2—C3 | 1.383 (5) | C22—C23 | 1.390 (5) |
C2—H2 | 0.9500 | C22—H22 | 0.9500 |
C3—C4 | 1.368 (5) | C23—C24 | 1.374 (5) |
C3—H3 | 0.9500 | C23—H23 | 0.9500 |
C4—C5 | 1.361 (5) | C24—C25 | 1.379 (5) |
C4—H4 | 0.9500 | C24—H24 | 0.9500 |
C5—C6 | 1.390 (4) | C25—H25 | 0.9500 |
C5—H5 | 0.9500 | C26—H26A | 0.9800 |
C6—H6 | 0.9500 | C26—H26B | 0.9800 |
C7—C8 | 1.376 (5) | C26—H26C | 0.9800 |
C7—C12 | 1.401 (4) | C27—H27A | 0.9800 |
C8—C9 | 1.395 (5) | C27—H27B | 0.9800 |
C8—H8 | 0.9500 | C27—H27C | 0.9800 |
C9—C10 | 1.398 (7) | C28—H28A | 0.9800 |
C9—H9 | 0.9500 | C28—H28B | 0.9800 |
C10—C11 | 1.366 (7) | C28—H28C | 0.9800 |
O3—Al1—O1 | 103.94 (10) | C10—C11—C12 | 120.8 (4) |
O3—Al1—C28 | 108.93 (17) | C10—C11—H11 | 119.6 |
O1—Al1—C28 | 109.5 (2) | C12—C11—H11 | 119.6 |
O3—Al1—C27 | 108.32 (14) | C11—C12—C7 | 119.1 (4) |
O1—Al1—C27 | 106.28 (13) | C11—C12—H12 | 120.4 |
C28—Al1—C27 | 118.8 (2) | C7—C12—H12 | 120.4 |
O2—Al2—O3i | 107.19 (10) | P2—C13—P1 | 129.37 (17) |
O2—Al2—O3 | 108.80 (9) | P2—C13—H13 | 115.1 (19) |
O3i—Al2—O3 | 86.69 (9) | P1—C13—H13 | 110.6 (19) |
O2—Al2—C26 | 113.48 (13) | C19—C14—C15 | 120.4 (3) |
O3i—Al2—C26 | 117.44 (12) | C19—C14—P2 | 119.2 (3) |
O3—Al2—C26 | 119.97 (13) | C15—C14—P2 | 120.4 (3) |
O2—Al2—Al2i | 115.13 (9) | C16—C15—C14 | 120.2 (4) |
O3i—Al2—Al2i | 43.43 (6) | C16—C15—H15 | 119.9 |
O3—Al2—Al2i | 43.26 (6) | C14—C15—H15 | 119.9 |
C26—Al2—Al2i | 131.32 (11) | C17—C16—C15 | 120.0 (5) |
P1—O1—Al1 | 141.21 (14) | C17—C16—H16 | 120.0 |
P2—O2—Al2 | 147.82 (14) | C15—C16—H16 | 120.0 |
Al1—O3—Al2i | 130.57 (11) | C18—C17—C16 | 120.4 (4) |
Al1—O3—Al2 | 136.12 (12) | C18—C17—H17 | 119.8 |
Al2i—O3—Al2 | 93.31 (9) | C16—C17—H17 | 119.8 |
O1—P1—C13 | 119.33 (12) | C17—C18—C19 | 120.8 (4) |
O1—P1—C1 | 105.99 (12) | C17—C18—H18 | 119.6 |
C13—P1—C1 | 107.59 (13) | C19—C18—H18 | 119.6 |
O1—P1—C7 | 105.25 (14) | C14—C19—C18 | 118.1 (4) |
C13—P1—C7 | 110.56 (13) | C14—C19—H19 | 121.0 |
C1—P1—C7 | 107.54 (12) | C18—C19—H19 | 121.0 |
O2—P2—C13 | 117.92 (12) | C21—C20—C25 | 120.0 (3) |
O2—P2—C14 | 105.54 (13) | C21—C20—P2 | 120.5 (2) |
C13—P2—C14 | 107.71 (15) | C25—C20—P2 | 119.6 (2) |
O2—P2—C20 | 104.42 (13) | C22—C21—C20 | 120.0 (3) |
C13—P2—C20 | 113.39 (13) | C22—C21—H21 | 120.0 |
C14—P2—C20 | 107.16 (13) | C20—C21—H21 | 120.0 |
C6—C1—C2 | 118.8 (3) | C21—C22—C23 | 119.4 (3) |
C6—C1—P1 | 121.8 (2) | C21—C22—H22 | 120.3 |
C2—C1—P1 | 119.5 (2) | C23—C22—H22 | 120.3 |
C3—C2—C1 | 120.1 (3) | C24—C23—C22 | 120.6 (3) |
C3—C2—H2 | 119.9 | C24—C23—H23 | 119.7 |
C1—C2—H2 | 119.9 | C22—C23—H23 | 119.7 |
C4—C3—C2 | 120.5 (3) | C23—C24—C25 | 120.3 (3) |
C4—C3—H3 | 119.8 | C23—C24—H24 | 119.8 |
C2—C3—H3 | 119.8 | C25—C24—H24 | 119.8 |
C5—C4—C3 | 120.1 (3) | C24—C25—C20 | 119.7 (3) |
C5—C4—H4 | 120.0 | C24—C25—H25 | 120.2 |
C3—C4—H4 | 120.0 | C20—C25—H25 | 120.2 |
C4—C5—C6 | 120.4 (3) | Al2—C26—H26A | 109.5 |
C4—C5—H5 | 119.8 | Al2—C26—H26B | 109.5 |
C6—C5—H5 | 119.8 | H26A—C26—H26B | 109.5 |
C1—C6—C5 | 120.1 (3) | Al2—C26—H26C | 109.5 |
C1—C6—H6 | 119.9 | H26A—C26—H26C | 109.5 |
C5—C6—H6 | 119.9 | H26B—C26—H26C | 109.5 |
C8—C7—C12 | 120.4 (3) | Al1—C27—H27A | 109.5 |
C8—C7—P1 | 120.5 (2) | Al1—C27—H27B | 109.5 |
C12—C7—P1 | 119.1 (3) | H27A—C27—H27B | 109.5 |
C7—C8—C9 | 120.1 (4) | Al1—C27—H27C | 109.5 |
C7—C8—H8 | 119.9 | H27A—C27—H27C | 109.5 |
C9—C8—H8 | 119.9 | H27B—C27—H27C | 109.5 |
C8—C9—C10 | 118.8 (4) | Al1—C28—H28A | 109.5 |
C8—C9—H9 | 120.6 | Al1—C28—H28B | 109.5 |
C10—C9—H9 | 120.6 | H28A—C28—H28B | 109.5 |
C11—C10—C9 | 120.7 (4) | Al1—C28—H28C | 109.5 |
C11—C10—H10 | 119.7 | H28A—C28—H28C | 109.5 |
C9—C10—H10 | 119.7 | H28B—C28—H28C | 109.5 |
Symmetry code: (i) −x+1, −y, −z. |