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The title centrosymmetric alumoxane compound, [Al4(CH3)63-O)2(μ-{Ph2P(O)}2CH)2]·C4H8O, is dimeric in the solid state as its THF disolvate, with a central Al2O2 ring core connected to terminal Me2Al units through oxo and non-chelating phosphinate anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011523/dn6136sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011523/dn6136Isup2.hkl
Contains datablock I

CCDC reference: 245267

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.062
  • wR factor = 0.173
  • Data-to-parameter ratio = 20.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.08 Ratio PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 149.00 A   3
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.35 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C16 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Al1 PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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).

Bis[µ2-bis(diphenylphosphinoyl)methanido-κ2O:O']hexamethyldi-µ3-oxo- dialuminium(III) tetrahydrofuran disolvate top
Crystal data top
[Al4(CH3)6O2(C25H21O2P2)2]·2C4H8OF(000) = 1112
Mr = 1205.12Dx = 1.234 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5174 reflections
a = 13.0087 (2) Åθ = 2.2–23.8°
b = 18.5644 (3) ŵ = 0.22 mm1
c = 13.7312 (2) ÅT = 100 K
β = 102.117 (1)°Cube, colorless
V = 3242.19 (9) Å30.19 × 0.14 × 0.14 mm
Z = 2
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
6623 independent reflections
Radiation source: fine-focus sealed tube, Siemens KFFMO2K-905264 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 8.33 pixels mm-1θmax = 26.4°, θmin = 1.9°
φ and ω scansh = 1613
Absorption correction: multi-scan
(Blessing, 1995)
k = 2323
Tmin = 0.960, Tmax = 0.971l = 1717
47479 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.062Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.173H 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 parametersΔρmax = 0.89 e Å3
0 restraintsΔρmin = 0.38 e Å3
Special details top

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 [Me6Al43-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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Al10.51781 (7)0.13590 (5)0.11532 (6)0.0421 (2)
Al20.46736 (6)0.03576 (4)0.06943 (6)0.0316 (2)
O10.64524 (18)0.17197 (12)0.05762 (14)0.0479 (5)
O20.56631 (16)0.06409 (11)0.16889 (13)0.0424 (5)
O30.50657 (14)0.05647 (10)0.04522 (13)0.0326 (4)
P10.70468 (6)0.20492 (4)0.04047 (5)0.03228 (19)
P20.64366 (5)0.12372 (4)0.21474 (5)0.03026 (18)
C10.7173 (2)0.29943 (14)0.0162 (2)0.0356 (6)
C20.7097 (3)0.32284 (18)0.0811 (2)0.0494 (8)
H20.69660.28910.13430.059*
C30.7211 (3)0.39511 (19)0.1007 (3)0.0597 (9)
H30.71630.41080.16740.072*
C40.7392 (3)0.44428 (18)0.0248 (3)0.0576 (9)
H40.74590.49390.03900.069*
C50.7476 (3)0.42214 (17)0.0710 (3)0.0529 (8)
H50.76080.45640.12360.063*
C60.7370 (2)0.34969 (15)0.0925 (2)0.0433 (7)
H60.74320.33460.15960.052*
C70.8343 (2)0.16606 (14)0.0614 (2)0.0389 (6)
C80.9078 (2)0.18236 (17)0.1462 (3)0.0472 (8)
H80.89040.21460.19400.057*
C91.0078 (3)0.1517 (2)0.1620 (4)0.0713 (12)
H91.05850.16180.22100.086*
C101.0322 (4)0.1057 (2)0.0895 (5)0.0806 (15)
H101.09990.08420.09960.097*
C110.9596 (4)0.0913 (2)0.0043 (4)0.0784 (14)
H110.97810.06080.04490.094*
C120.8602 (3)0.12035 (17)0.0110 (3)0.0590 (10)
H120.80980.10960.07000.071*
C130.6535 (2)0.19737 (15)0.1443 (2)0.0317 (6)
H130.605 (2)0.2308 (17)0.145 (2)0.036 (8)*
C140.6001 (2)0.15336 (19)0.3241 (2)0.0436 (7)
C150.6247 (3)0.2223 (2)0.3621 (3)0.0656 (11)
H150.66470.25390.33020.079*
C160.5913 (5)0.2448 (3)0.4463 (3)0.0986 (18)
H160.60870.29170.47240.118*
C170.5330 (5)0.1995 (3)0.4921 (3)0.0986 (18)
H170.50970.21530.54970.118*
C180.5082 (3)0.1319 (3)0.4556 (3)0.0830 (15)
H180.46680.10130.48750.100*
C190.5435 (3)0.1067 (2)0.3707 (2)0.0601 (10)
H190.52850.05900.34670.072*
C200.7668 (2)0.07750 (14)0.2565 (2)0.0338 (6)
C210.8358 (2)0.09901 (15)0.3430 (2)0.0406 (7)
H210.81800.13820.38070.049*
C220.9305 (3)0.06327 (18)0.3744 (3)0.0536 (8)
H220.97770.07770.43370.064*
C230.9557 (3)0.00615 (19)0.3182 (3)0.0607 (10)
H231.02090.01820.33900.073*
C240.8872 (3)0.01546 (18)0.2329 (3)0.0586 (9)
H240.90530.05450.19510.070*
C250.7923 (3)0.01930 (17)0.2019 (2)0.0466 (7)
H250.74450.00370.14360.056*
C260.3262 (2)0.05986 (19)0.0857 (3)0.0507 (8)
H26A0.31670.04300.15090.076*
H26B0.27430.03650.03310.076*
H26C0.31640.11220.08130.076*
C270.5275 (3)0.1071 (2)0.2506 (2)0.0664 (11)
H27A0.58250.07050.24700.100*
H27B0.54500.14920.28700.100*
H27C0.46000.08720.28520.100*
C280.4081 (4)0.2038 (3)0.0984 (4)0.0979 (17)
H28A0.34000.18710.13650.147*
H28B0.42370.25150.12240.147*
H28C0.40550.20690.02770.147*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.0455 (5)0.0409 (5)0.0361 (5)0.0053 (4)0.0005 (4)0.0123 (4)
Al20.0279 (4)0.0364 (4)0.0314 (4)0.0047 (3)0.0084 (3)0.0020 (3)
O10.0628 (14)0.0473 (12)0.0338 (10)0.0259 (11)0.0105 (10)0.0045 (9)
O20.0472 (12)0.0508 (12)0.0284 (9)0.0216 (10)0.0064 (8)0.0009 (9)
O30.0336 (10)0.0347 (10)0.0285 (9)0.0061 (8)0.0039 (7)0.0038 (8)
P10.0373 (4)0.0279 (3)0.0318 (4)0.0059 (3)0.0077 (3)0.0021 (3)
P20.0298 (3)0.0358 (4)0.0257 (3)0.0043 (3)0.0071 (3)0.0037 (3)
C10.0311 (14)0.0304 (13)0.0434 (15)0.0012 (11)0.0038 (11)0.0034 (12)
C20.0558 (19)0.0454 (18)0.0426 (16)0.0094 (15)0.0001 (14)0.0062 (14)
C30.064 (2)0.0485 (19)0.060 (2)0.0070 (17)0.0021 (17)0.0210 (17)
C40.0483 (19)0.0344 (16)0.087 (3)0.0019 (14)0.0081 (18)0.0144 (17)
C50.0523 (19)0.0317 (15)0.073 (2)0.0036 (14)0.0091 (17)0.0065 (16)
C60.0482 (17)0.0319 (15)0.0481 (17)0.0014 (13)0.0061 (14)0.0021 (13)
C70.0438 (16)0.0254 (13)0.0536 (17)0.0001 (12)0.0239 (14)0.0045 (12)
C80.0347 (15)0.0385 (16)0.072 (2)0.0049 (12)0.0191 (15)0.0164 (15)
C90.0389 (18)0.065 (2)0.110 (3)0.0055 (17)0.016 (2)0.038 (2)
C100.060 (2)0.061 (2)0.138 (4)0.031 (2)0.060 (3)0.045 (3)
C110.095 (3)0.050 (2)0.112 (4)0.026 (2)0.070 (3)0.021 (2)
C120.082 (3)0.0340 (16)0.075 (2)0.0078 (16)0.049 (2)0.0034 (16)
C130.0272 (13)0.0327 (14)0.0345 (13)0.0024 (11)0.0050 (10)0.0007 (11)
C140.0358 (15)0.067 (2)0.0288 (13)0.0121 (14)0.0090 (11)0.0006 (14)
C150.093 (3)0.061 (2)0.0460 (19)0.026 (2)0.0209 (19)0.0101 (17)
C160.161 (5)0.091 (3)0.052 (2)0.053 (4)0.041 (3)0.007 (2)
C170.120 (4)0.125 (5)0.060 (3)0.056 (4)0.040 (3)0.012 (3)
C180.058 (2)0.154 (5)0.042 (2)0.008 (3)0.0221 (17)0.017 (3)
C190.0472 (19)0.099 (3)0.0355 (16)0.0003 (19)0.0129 (14)0.0004 (17)
C200.0382 (15)0.0277 (13)0.0381 (14)0.0005 (11)0.0141 (11)0.0020 (11)
C210.0371 (15)0.0290 (14)0.0529 (17)0.0001 (11)0.0030 (13)0.0044 (12)
C220.0414 (17)0.0441 (18)0.070 (2)0.0024 (14)0.0005 (16)0.0114 (16)
C230.0450 (19)0.0461 (19)0.093 (3)0.0141 (15)0.0179 (19)0.0191 (19)
C240.065 (2)0.0400 (17)0.078 (3)0.0121 (16)0.032 (2)0.0006 (17)
C250.0535 (18)0.0419 (17)0.0477 (17)0.0022 (14)0.0182 (14)0.0059 (14)
C260.0391 (17)0.055 (2)0.062 (2)0.0013 (14)0.0213 (15)0.0110 (16)
C270.075 (2)0.085 (3)0.0321 (16)0.039 (2)0.0045 (16)0.0118 (17)
C280.103 (4)0.081 (3)0.112 (4)0.049 (3)0.029 (3)0.049 (3)
Geometric parameters (Å, º) top
Al1—O31.7837 (19)C10—H100.9500
Al1—O11.809 (2)C11—C121.377 (6)
Al1—C281.955 (5)C11—H110.9500
Al1—C271.962 (4)C12—H120.9500
Al2—O21.750 (2)C13—H130.88 (3)
Al2—O3i1.790 (2)C14—C191.378 (5)
Al2—O31.7955 (19)C14—C151.394 (5)
Al2—C261.948 (3)C15—C161.383 (5)
Al2—Al2i2.6075 (16)C15—H150.9500
O1—P11.533 (2)C16—C171.370 (8)
O2—P21.5390 (19)C16—H160.9500
O3—Al2i1.790 (2)C17—C181.365 (7)
P1—C131.701 (3)C17—H170.9500
P1—C11.800 (3)C18—C191.420 (5)
P1—C71.800 (3)C18—H180.9500
P2—C131.695 (3)C19—H190.9500
P2—C141.799 (3)C20—C211.388 (4)
P2—C201.802 (3)C20—C251.394 (4)
C1—C61.385 (4)C21—C221.386 (4)
C1—C21.389 (4)C21—H210.9500
C2—C31.383 (5)C22—C231.390 (5)
C2—H20.9500C22—H220.9500
C3—C41.368 (5)C23—C241.374 (5)
C3—H30.9500C23—H230.9500
C4—C51.361 (5)C24—C251.379 (5)
C4—H40.9500C24—H240.9500
C5—C61.390 (4)C25—H250.9500
C5—H50.9500C26—H26A0.9800
C6—H60.9500C26—H26B0.9800
C7—C81.376 (5)C26—H26C0.9800
C7—C121.401 (4)C27—H27A0.9800
C8—C91.395 (5)C27—H27B0.9800
C8—H80.9500C27—H27C0.9800
C9—C101.398 (7)C28—H28A0.9800
C9—H90.9500C28—H28B0.9800
C10—C111.366 (7)C28—H28C0.9800
O3—Al1—O1103.94 (10)C10—C11—C12120.8 (4)
O3—Al1—C28108.93 (17)C10—C11—H11119.6
O1—Al1—C28109.5 (2)C12—C11—H11119.6
O3—Al1—C27108.32 (14)C11—C12—C7119.1 (4)
O1—Al1—C27106.28 (13)C11—C12—H12120.4
C28—Al1—C27118.8 (2)C7—C12—H12120.4
O2—Al2—O3i107.19 (10)P2—C13—P1129.37 (17)
O2—Al2—O3108.80 (9)P2—C13—H13115.1 (19)
O3i—Al2—O386.69 (9)P1—C13—H13110.6 (19)
O2—Al2—C26113.48 (13)C19—C14—C15120.4 (3)
O3i—Al2—C26117.44 (12)C19—C14—P2119.2 (3)
O3—Al2—C26119.97 (13)C15—C14—P2120.4 (3)
O2—Al2—Al2i115.13 (9)C16—C15—C14120.2 (4)
O3i—Al2—Al2i43.43 (6)C16—C15—H15119.9
O3—Al2—Al2i43.26 (6)C14—C15—H15119.9
C26—Al2—Al2i131.32 (11)C17—C16—C15120.0 (5)
P1—O1—Al1141.21 (14)C17—C16—H16120.0
P2—O2—Al2147.82 (14)C15—C16—H16120.0
Al1—O3—Al2i130.57 (11)C18—C17—C16120.4 (4)
Al1—O3—Al2136.12 (12)C18—C17—H17119.8
Al2i—O3—Al293.31 (9)C16—C17—H17119.8
O1—P1—C13119.33 (12)C17—C18—C19120.8 (4)
O1—P1—C1105.99 (12)C17—C18—H18119.6
C13—P1—C1107.59 (13)C19—C18—H18119.6
O1—P1—C7105.25 (14)C14—C19—C18118.1 (4)
C13—P1—C7110.56 (13)C14—C19—H19121.0
C1—P1—C7107.54 (12)C18—C19—H19121.0
O2—P2—C13117.92 (12)C21—C20—C25120.0 (3)
O2—P2—C14105.54 (13)C21—C20—P2120.5 (2)
C13—P2—C14107.71 (15)C25—C20—P2119.6 (2)
O2—P2—C20104.42 (13)C22—C21—C20120.0 (3)
C13—P2—C20113.39 (13)C22—C21—H21120.0
C14—P2—C20107.16 (13)C20—C21—H21120.0
C6—C1—C2118.8 (3)C21—C22—C23119.4 (3)
C6—C1—P1121.8 (2)C21—C22—H22120.3
C2—C1—P1119.5 (2)C23—C22—H22120.3
C3—C2—C1120.1 (3)C24—C23—C22120.6 (3)
C3—C2—H2119.9C24—C23—H23119.7
C1—C2—H2119.9C22—C23—H23119.7
C4—C3—C2120.5 (3)C23—C24—C25120.3 (3)
C4—C3—H3119.8C23—C24—H24119.8
C2—C3—H3119.8C25—C24—H24119.8
C5—C4—C3120.1 (3)C24—C25—C20119.7 (3)
C5—C4—H4120.0C24—C25—H25120.2
C3—C4—H4120.0C20—C25—H25120.2
C4—C5—C6120.4 (3)Al2—C26—H26A109.5
C4—C5—H5119.8Al2—C26—H26B109.5
C6—C5—H5119.8H26A—C26—H26B109.5
C1—C6—C5120.1 (3)Al2—C26—H26C109.5
C1—C6—H6119.9H26A—C26—H26C109.5
C5—C6—H6119.9H26B—C26—H26C109.5
C8—C7—C12120.4 (3)Al1—C27—H27A109.5
C8—C7—P1120.5 (2)Al1—C27—H27B109.5
C12—C7—P1119.1 (3)H27A—C27—H27B109.5
C7—C8—C9120.1 (4)Al1—C27—H27C109.5
C7—C8—H8119.9H27A—C27—H27C109.5
C9—C8—H8119.9H27B—C27—H27C109.5
C8—C9—C10118.8 (4)Al1—C28—H28A109.5
C8—C9—H9120.6Al1—C28—H28B109.5
C10—C9—H9120.6H28A—C28—H28B109.5
C11—C10—C9120.7 (4)Al1—C28—H28C109.5
C11—C10—H10119.7H28A—C28—H28C109.5
C9—C10—H10119.7H28B—C28—H28C109.5
Symmetry code: (i) x+1, y, z.
 

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