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The title compound, [Al{(CH3)2SO}6]Cl3, crystallizes in the trigonal space group R\overline 3. In this structure, the O atoms of six di­methyl sulfoxide (DMSO) mol­ecules are bonded to the Al3+ ion in the form of a trigonally distorted octahedron. The Al3+ ion is situated at special site 3b (symmetry \overline 3), while the Cl ions are situated at special sites 3a and 6c (symmetries \overline 3 and 3). Considering only the Al3+ ions separately, they are arranged in a slightly distorted cubic close-packed arrangement. In this crystal structure, the Cl ions occupy both the tetrahedral sites and the octahedral sites, giving a Cl:Al3+ ratio of 3:1. This geometric condition results in a distorted rhombododecahedral arrangement of Cl ions around the Al3+ ions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020464/br6120sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020464/br6120Isup2.hkl
Contains datablock I

CCDC reference: 225683

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](Al-O) = 0.001 Å
  • R factor = 0.026
  • wR factor = 0.068
  • Data-to-parameter ratio = 30.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 29.98 From the CIF: _reflns_number_total 1340 From the CIF: _diffrn_reflns_limit_ max hkl 12. 14. 30. From the CIF: _diffrn_reflns_limit_ min hkl -12. -14. -30. TEST1: Expected hkl limits for theta max Calculated maximum hkl 14. 14. 30. Calculated minimum hkl -14. -14. -30.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 0 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: COLLECT (Nonius, 1999); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2000); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and local programs.

hexakisdimethylsulfoxidealuminium(III) trichloride top
Crystal data top
[Al(C2H6OS)6]Cl3Dx = 1.461 Mg m3
Mr = 602.14Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3Cell parameters from 1340 reflections
Hall symbol: -R 3θ = 3.0–30.0°
a = 10.3760 (6) ŵ = 0.85 mm1
c = 22.0210 (12) ÅT = 150 K
V = 2053.2 (2) Å3Fragment, colourless
Z = 30.25 × 0.20 × 0.15 mm
F(000) = 948
Data collection top
Nonius KappaCCD
diffractometer
1340 independent reflections
Radiation source: fine-focus sealed tube, KappaCCD1266 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.012
φ and ω scansθmax = 30.0°, θmin = 3.9°
Absorption correction: multi-scan
(HKL SCALEPACK; Otwinowski & Minor, 1997)'
h = 1212
Tmin = 0.816, Tmax = 0.883k = 1414
2680 measured reflectionsl = 3030
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.026 w = 1/[σ2(Fo2) + (0.0316P)2 + 2.3297P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.068(Δ/σ)max < 0.001
S = 1.11Δρmax = 0.50 e Å3
1340 reflectionsΔρmin = 0.43 e Å3
44 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0018 (3)
Primary atom site location: structure-invariant direct methods
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
Cl10.00000.00000.00000.02766 (17)
Cl20.00000.00000.25090.03096 (14)
C10.24971 (17)0.24361 (15)0.12848 (6)0.0321 (3)
H1A0.18550.14970.10930.039*
H1B0.22160.23940.17030.039*
H1C0.35080.26470.12620.039*
C20.30666 (14)0.37757 (14)0.01919 (6)0.0271 (3)
H2A0.31540.45690.00610.032*
H2B0.24110.28370.00030.032*
H2C0.40300.38740.02460.032*
S0.23359 (3)0.38616 (3)0.090813 (13)0.01964 (11)
Al0.33330.66670.16670.01667 (17)
O0.35982 (9)0.53114 (9)0.11850 (4)0.02161 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cl10.0216 (3)0.0220.0398 (4)0.0110.0000.000
Cl20.0334 (3)0.0330.0260 (3)0.0170.0000.000
C10.0406 (7)0.0220 (6)0.0334 (7)0.0154 (5)0.0013 (5)0.0055 (5)
C20.0277 (6)0.0240 (6)0.0246 (6)0.0094 (5)0.0027 (4)0.0024 (4)
S0.01714 (15)0.01628 (14)0.02438 (16)0.00753 (10)0.00040 (9)0.00070 (9)
Al0.0149 (2)0.0149 (2)0.0201 (4)0.00747 (11)0.0000.000
O0.0181 (4)0.0184 (4)0.0278 (4)0.0088 (3)0.0010 (3)0.0051 (3)
Geometric parameters (Å, º) top
C1—S1.7751 (13)S—O1.5427 (8)
C1—H1A0.9600Al—Oi1.8880 (8)
C1—H1B0.9599Al—Oii1.8880 (8)
C1—H1C0.9601Al—Oiii1.8880 (8)
C2—S1.7715 (12)Al—Oiv1.8880 (8)
C2—H2A0.9600Al—O1.8880 (8)
C2—H2B0.9599Al—Ov1.8880 (8)
C2—H2C0.9600
S—C1—H1A109.5Oi—Al—Oiii91.52 (4)
S—C1—H1B109.5Oii—Al—Oiii88.48 (4)
H1A—C1—H1B109.5Oi—Al—Oiv88.48 (4)
S—C1—H1C109.5Oii—Al—Oiv91.52 (4)
H1A—C1—H1C109.5Oiii—Al—Oiv180.0
H1B—C1—H1C109.5Oi—Al—O91.52 (4)
S—C2—H2A109.5Oii—Al—O88.48 (4)
S—C2—H2B109.5Oiii—Al—O91.52 (4)
H2A—C2—H2B109.5Oiv—Al—O88.48 (4)
S—C2—H2C109.5Oi—Al—Ov88.48 (4)
H2A—C2—H2C109.5Oii—Al—Ov91.52 (4)
H2B—C2—H2C109.5Oiii—Al—Ov88.48 (4)
O—S—C2102.99 (5)Oiv—Al—Ov91.52 (4)
O—S—C1103.89 (6)O—Al—Ov180.0
C2—S—C198.81 (6)S—O—Al125.42 (5)
Oi—Al—Oii180.0
Symmetry codes: (i) x+y, x+1, z; (ii) xy+2/3, x+1/3, z+1/3; (iii) y+1, xy+1, z; (iv) y1/3, x+y+1/3, z+1/3; (v) x+2/3, y+4/3, z+1/3.
 

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