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The title compound, [AlCl2(C4H8O)4][AlCl3(C2H5)], was prepared by the unsymmetrical cleavage reaction of the EtAlCl2 dimer with tetra­hydro­furan (THF). The [AlCl2(THF)4]+ cation forms an approximately regular octahedron, and the [AlCl3Et]- anion is tetrahedral.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804006312/dn6130sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804006312/dn6130Isup2.hkl
Contains datablock I

CCDC reference: 238665

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.036
  • wR factor = 0.096
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of Tmax/Tmin expected RT(exp) is > 1.10 Absorption corrections should be applied. Tmin and Tmax expected: 0.779 0.908 RT(exp) = 1.166 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.16
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 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: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXTL (Bruker, 1998); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Dichlorotetrakis(tetrahydrofuran)aluminium trichloroethylaluminate top
Crystal data top
[AlCl2(C4H8O)4][AlCl3(C2H5)]F(000) = 1152
Mr = 548.69Dx = 1.395 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 60 reflections
a = 8.8285 (17) Åθ = 8.2–25.4°
b = 20.225 (3) ŵ = 0.64 mm1
c = 14.638 (3) ÅT = 120 K
β = 91.353 (15)°Prism, colourless
V = 2613.0 (8) Å30.40 × 0.40 × 0.15 mm
Z = 4
Data collection top
Kuma KM-4 CCD
diffractometer
3905 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.052
Enhance (Oxford Diffraction) monochromatorθmax = 25.0°, θmin = 3.3°
Detector resolution: 16.3 pixels mm-1h = 1010
ω scansk = 1924
15493 measured reflectionsl = 1716
4485 independent 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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.05P)2 + 1.2019P]
where P = (Fo2 + 2Fc2)/3
4485 reflections(Δ/σ)max = 0.001
262 parametersΔρmax = 0.35 e Å3
0 restraintsΔρmin = 0.35 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. 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
Cl20.47500 (6)0.31537 (3)0.43665 (4)0.01953 (14)
Cl10.79654 (6)0.26337 (3)0.66753 (4)0.01966 (14)
Al10.63554 (7)0.28865 (3)0.55183 (4)0.01484 (16)
O10.46838 (16)0.25698 (7)0.62367 (10)0.0168 (3)
O30.80373 (16)0.31891 (7)0.48021 (10)0.0177 (3)
O20.65951 (16)0.20028 (7)0.50178 (10)0.0176 (3)
O40.60906 (17)0.37611 (7)0.60228 (10)0.0185 (3)
C30.3155 (3)0.17927 (12)0.69795 (17)0.0257 (5)
H3A0.30190.15670.75720.031*
H3B0.27980.14990.64780.031*
C10.3116 (2)0.28095 (12)0.61861 (18)0.0253 (5)
H1A0.26340.27010.55870.030*
H1B0.30770.32940.62780.030*
C100.9837 (3)0.31408 (12)0.36528 (17)0.0258 (5)
H10A1.00420.32720.30160.031*
H10B1.03530.27160.37890.031*
C70.7672 (3)0.10324 (12)0.44157 (18)0.0291 (6)
H7A0.82430.06290.45930.035*
H7B0.79380.11610.37870.035*
C50.5392 (3)0.16308 (11)0.45296 (17)0.0227 (5)
H5A0.52210.18080.39050.027*
H5B0.44300.16530.48620.027*
C40.4770 (3)0.19952 (11)0.68594 (16)0.0222 (5)
H4A0.52500.21200.74530.027*
H4B0.53600.16320.65870.027*
C150.7101 (3)0.45242 (12)0.70427 (17)0.0257 (5)
H15A0.81640.43700.70960.031*
H15B0.68790.48100.75720.031*
C160.6020 (3)0.39503 (11)0.69796 (15)0.0220 (5)
H16A0.63520.35840.73850.026*
H16B0.49820.40860.71400.026*
C120.9428 (3)0.35148 (13)0.51593 (17)0.0273 (6)
H12A1.00030.32150.55740.033*
H12B0.91760.39230.54970.033*
C90.8167 (3)0.30944 (12)0.38103 (15)0.0230 (5)
H9A0.76080.34430.34680.028*
H9B0.77670.26570.36210.028*
C140.6810 (3)0.48889 (13)0.61445 (18)0.0342 (6)
H14A0.77740.50410.58840.041*
H14B0.61470.52770.62380.041*
C111.0329 (3)0.36743 (12)0.43253 (16)0.0244 (5)
H11A1.14320.36500.44620.029*
H11B1.00780.41200.40870.029*
C130.6034 (3)0.43859 (11)0.55146 (17)0.0247 (5)
H13A0.49720.45170.53770.030*
H13B0.65770.43460.49330.030*
C80.7974 (3)0.15879 (11)0.50819 (17)0.0241 (5)
H8A0.81310.14150.57100.029*
H8B0.88800.18440.49100.029*
C60.5976 (3)0.09299 (12)0.44966 (18)0.0257 (5)
H6A0.55490.06890.39610.031*
H6B0.57370.06850.50610.031*
C20.2341 (3)0.24514 (13)0.69502 (19)0.0315 (6)
H2A0.12460.23940.68110.038*
H2B0.24700.26910.75360.038*
Cl30.39133 (7)0.53896 (3)0.79798 (5)0.03016 (16)
Cl50.16786 (7)0.46593 (3)0.63051 (4)0.03142 (17)
Cl40.00148 (7)0.55262 (3)0.81153 (5)0.03151 (17)
Al20.18087 (8)0.48612 (3)0.77608 (5)0.02221 (17)
C180.1770 (3)0.41525 (14)0.95133 (18)0.0351 (6)
H18A0.17480.37230.98220.053*
H18B0.08760.44100.96770.053*
H18C0.26890.43920.97040.053*
C170.1766 (3)0.40473 (12)0.84755 (18)0.0286 (6)
H17A0.08480.37940.82940.034*
H17B0.26580.37760.83210.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl20.0169 (3)0.0247 (3)0.0170 (3)0.0008 (2)0.0012 (2)0.0031 (2)
Cl10.0166 (3)0.0249 (3)0.0174 (3)0.0004 (2)0.0021 (2)0.0026 (2)
Al10.0129 (3)0.0172 (3)0.0144 (3)0.0000 (2)0.0004 (3)0.0010 (3)
O10.0137 (7)0.0186 (8)0.0184 (8)0.0026 (6)0.0038 (6)0.0057 (6)
O30.0144 (7)0.0251 (9)0.0136 (8)0.0038 (6)0.0008 (6)0.0020 (6)
O20.0125 (7)0.0200 (8)0.0203 (8)0.0013 (6)0.0026 (6)0.0019 (6)
O40.0236 (8)0.0167 (8)0.0153 (8)0.0003 (6)0.0029 (6)0.0020 (6)
C30.0238 (12)0.0298 (13)0.0235 (13)0.0073 (10)0.0008 (10)0.0064 (10)
C10.0121 (10)0.0308 (13)0.0332 (14)0.0059 (9)0.0055 (10)0.0084 (11)
C100.0239 (12)0.0301 (14)0.0238 (13)0.0012 (10)0.0094 (10)0.0010 (10)
C70.0241 (13)0.0282 (14)0.0351 (15)0.0037 (10)0.0016 (11)0.0085 (11)
C50.0191 (11)0.0237 (12)0.0250 (13)0.0035 (9)0.0027 (10)0.0059 (10)
C40.0219 (11)0.0211 (12)0.0236 (13)0.0003 (9)0.0000 (10)0.0089 (10)
C150.0273 (12)0.0261 (13)0.0236 (13)0.0035 (10)0.0002 (10)0.0038 (10)
C160.0283 (13)0.0223 (12)0.0155 (11)0.0005 (10)0.0045 (10)0.0030 (9)
C120.0158 (11)0.0397 (15)0.0263 (14)0.0110 (10)0.0003 (10)0.0032 (11)
C90.0255 (12)0.0310 (13)0.0127 (11)0.0043 (10)0.0051 (9)0.0018 (10)
C140.0476 (16)0.0233 (13)0.0318 (15)0.0108 (12)0.0027 (13)0.0005 (11)
C110.0178 (11)0.0288 (13)0.0267 (13)0.0031 (10)0.0030 (10)0.0012 (10)
C130.0329 (13)0.0177 (12)0.0236 (13)0.0007 (10)0.0004 (10)0.0062 (10)
C80.0180 (11)0.0220 (12)0.0322 (14)0.0071 (9)0.0007 (10)0.0023 (10)
C60.0250 (12)0.0230 (12)0.0291 (13)0.0005 (10)0.0009 (10)0.0065 (10)
C20.0193 (12)0.0406 (15)0.0350 (15)0.0008 (11)0.0094 (11)0.0092 (12)
Cl30.0246 (3)0.0251 (3)0.0407 (4)0.0036 (2)0.0014 (3)0.0058 (3)
Cl50.0336 (3)0.0344 (4)0.0261 (3)0.0006 (3)0.0012 (3)0.0078 (3)
Cl40.0259 (3)0.0324 (3)0.0362 (4)0.0077 (2)0.0006 (3)0.0062 (3)
Al20.0216 (4)0.0202 (4)0.0248 (4)0.0008 (3)0.0004 (3)0.0028 (3)
C180.0275 (14)0.0410 (16)0.0368 (16)0.0028 (11)0.0024 (12)0.0091 (12)
C170.0251 (13)0.0248 (13)0.0359 (15)0.0010 (10)0.0017 (11)0.0026 (11)
Geometric parameters (Å, º) top
Cl2—Al12.2429 (9)C15—C161.504 (3)
Cl1—Al12.2443 (9)C15—C141.524 (4)
Al1—O41.9331 (16)C15—H15A0.9900
Al1—O31.9371 (16)C15—H15B0.9900
Al1—O11.9409 (16)C16—H16A0.9900
Al1—O21.9450 (16)C16—H16B0.9900
O1—C11.467 (3)C12—C111.508 (3)
O1—C41.478 (3)C12—H12A0.9900
O3—C91.472 (3)C12—H12B0.9900
O3—C121.478 (3)C9—H9A0.9900
O2—C51.473 (3)C9—H9B0.9900
O2—C81.479 (3)C14—C131.525 (3)
O4—C161.455 (3)C14—H14A0.9900
O4—C131.467 (3)C14—H14B0.9900
C3—C41.498 (3)C11—H11A0.9900
C3—C21.514 (4)C11—H11B0.9900
C3—H3A0.9900C13—H13A0.9900
C3—H3B0.9900C13—H13B0.9900
C1—C21.510 (3)C8—H8A0.9900
C1—H1A0.9900C8—H8B0.9900
C1—H1B0.9900C6—H6A0.9900
C10—C91.501 (3)C6—H6B0.9900
C10—C111.517 (3)C2—H2A0.9900
C10—H10A0.9900C2—H2B0.9900
C10—H10B0.9900Cl3—Al22.1608 (10)
C7—C81.507 (3)Cl5—Al22.1701 (10)
C7—C61.519 (3)Cl4—Al22.1506 (9)
C7—H7A0.9900Al2—C171.951 (3)
C7—H7B0.9900C18—C171.534 (4)
C5—C61.510 (3)C18—H18A0.9800
C5—H5A0.9900C18—H18B0.9800
C5—H5B0.9900C18—H18C0.9800
C4—H4A0.9900C17—H17A0.9900
C4—H4B0.9900C17—H17B0.9900
O4—Al1—O391.07 (7)C15—C16—H16A111.2
O4—Al1—O189.69 (7)O4—C16—H16B111.2
O3—Al1—O1179.12 (7)C15—C16—H16B111.2
O4—Al1—O2179.20 (7)H16A—C16—H16B109.1
O3—Al1—O289.71 (7)O3—C12—C11105.01 (18)
O1—Al1—O289.53 (7)O3—C12—H12A110.7
O4—Al1—Cl289.24 (5)C11—C12—H12A110.7
O3—Al1—Cl289.76 (5)O3—C12—H12B110.7
O1—Al1—Cl290.67 (5)C11—C12—H12B110.7
O2—Al1—Cl290.61 (5)H12A—C12—H12B108.8
O4—Al1—Cl190.02 (5)O3—C9—C10104.05 (18)
O3—Al1—Cl190.03 (5)O3—C9—H9A110.9
O1—Al1—Cl189.55 (5)C10—C9—H9A110.9
O2—Al1—Cl190.13 (5)O3—C9—H9B110.9
Cl2—Al1—Cl1179.22 (4)C10—C9—H9B110.9
C1—O1—C4109.02 (16)H9A—C9—H9B109.0
C1—O1—Al1126.31 (13)C15—C14—C13105.3 (2)
C4—O1—Al1124.40 (13)C15—C14—H14A110.7
C9—O3—C12108.90 (16)C13—C14—H14A110.7
C9—O3—Al1124.83 (13)C15—C14—H14B110.7
C12—O3—Al1126.18 (13)C13—C14—H14B110.7
C5—O2—C8108.88 (16)H14A—C14—H14B108.8
C5—O2—Al1124.66 (13)C12—C11—C10102.98 (19)
C8—O2—Al1126.44 (13)C12—C11—H11A111.2
C16—O4—C13105.06 (16)C10—C11—H11A111.2
C16—O4—Al1128.09 (13)C12—C11—H11B111.2
C13—O4—Al1126.70 (13)C10—C11—H11B111.2
C4—C3—C2102.03 (19)H11A—C11—H11B109.1
C4—C3—H3A111.4O4—C13—C14104.98 (19)
C2—C3—H3A111.4O4—C13—H13A110.8
C4—C3—H3B111.4C14—C13—H13A110.8
C2—C3—H3B111.4O4—C13—H13B110.8
H3A—C3—H3B109.2C14—C13—H13B110.8
O1—C1—C2104.34 (18)H13A—C13—H13B108.8
O1—C1—H1A110.9O2—C8—C7104.44 (18)
C2—C1—H1A110.9O2—C8—H8A110.9
O1—C1—H1B110.9C7—C8—H8A110.9
C2—C1—H1B110.9O2—C8—H8B110.9
H1A—C1—H1B108.9C7—C8—H8B110.9
C9—C10—C11102.25 (18)H8A—C8—H8B108.9
C9—C10—H10A111.3C5—C6—C7102.26 (19)
C11—C10—H10A111.3C5—C6—H6A111.3
C9—C10—H10B111.3C7—C6—H6A111.3
C11—C10—H10B111.3C5—C6—H6B111.3
H10A—C10—H10B109.2C7—C6—H6B111.3
C8—C7—C6102.16 (19)H6A—C6—H6B109.2
C8—C7—H7A111.3C1—C2—C3102.71 (19)
C6—C7—H7A111.3C1—C2—H2A111.2
C8—C7—H7B111.3C3—C2—H2A111.2
C6—C7—H7B111.3C1—C2—H2B111.2
H7A—C7—H7B109.2C3—C2—H2B111.2
O2—C5—C6104.62 (18)H2A—C2—H2B109.1
O2—C5—H5A110.8C17—Al2—Cl4112.00 (8)
C6—C5—H5A110.8C17—Al2—Cl3111.41 (8)
O2—C5—H5B110.8Cl4—Al2—Cl3106.89 (4)
C6—C5—H5B110.8C17—Al2—Cl5111.50 (9)
H5A—C5—H5B108.9Cl4—Al2—Cl5109.42 (4)
O1—C4—C3104.60 (18)Cl3—Al2—Cl5105.31 (4)
O1—C4—H4A110.8C17—C18—H18A109.5
C3—C4—H4A110.8C17—C18—H18B109.5
O1—C4—H4B110.8H18A—C18—H18B109.5
C3—C4—H4B110.8C17—C18—H18C109.5
H4A—C4—H4B108.9H18A—C18—H18C109.5
C16—C15—C14103.07 (19)H18B—C18—H18C109.5
C16—C15—H15A111.1C18—C17—Al2114.48 (18)
C14—C15—H15A111.1C18—C17—H17A108.6
C16—C15—H15B111.1Al2—C17—H17A108.6
C14—C15—H15B111.1C18—C17—H17B108.6
H15A—C15—H15B109.1Al2—C17—H17B108.6
O4—C16—C15102.74 (18)H17A—C17—H17B107.6
O4—C16—H16A111.2
C4—O1—C1—C211.6 (2)O3—C12—C11—C1028.5 (2)
C8—O2—C5—C612.6 (2)C9—C10—C11—C1240.4 (2)
C1—O1—C4—C314.5 (2)C16—O4—C13—C1431.4 (2)
C2—C3—C4—O134.5 (2)C15—C14—C13—O46.7 (3)
C13—O4—C16—C1544.1 (2)C5—O2—C8—C713.8 (2)
C14—C15—C16—O438.6 (2)C6—C7—C8—O234.4 (2)
C9—O3—C12—C115.6 (2)O2—C5—C6—C733.7 (2)
C12—O3—C9—C1019.9 (2)C8—C7—C6—C542.0 (2)
C11—C10—C9—O337.1 (2)O1—C1—C2—C332.9 (3)
C16—C15—C14—C1319.3 (3)C4—C3—C2—C141.6 (2)
 

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