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The title compound, GaCl3·C4H8O, is isostructural with AlCl3·C4H8O. The mol­ecule is located on a mirror plane, passing through the Ga atom, the O atom and one of the Cl atoms. All other atoms occupy general positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016100/cf6203sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016100/cf6203Isup2.hkl
Contains datablock I

CCDC reference: 198316

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.035
  • wR factor = 0.093
  • Data-to-parameter ratio = 28.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
Author response: The data were measured on an area-detector.
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.
Author response: The data were measured on an area-detector.

2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Comment top

We report here the X-ray crystal structure analysis of GaCl3.thf (thf = C4H8O). The halides of Ga(I), Ga(II), and Ga(III) have been used in the synthesis of new gallium clusters (Donchev et al., 2001). The synthesis of these clusters depends on the oxidation state of Ga in the halides on the one hand and the solvent on the other. GaCl3 features a cyclic, dimeric arrangement in non-donor solvents such as alkanes and benzene. By contrast, monomeric adducts of GaCl3 are formed in the presence of Lewis bases. Given this background, we became interested in the reaction of GaCl3.thf with the bulky siloxides tBu3SiONa and tBu2PhSiONa (Lerner et al., 2002). Therefore, we prepared a solution of GaCl3.thf in pentane. Colourless crystals of the title compound, (I), were grown from this solution at 267 K. GaCl3.C4H8O is isostructural with AlCl3.C4H8O (Engelhardt et al., 1996). The molecule is located on a mirror plane; the Ga atom, the O atom and one of the Cl atoms lie in this plane. All other atoms occupy general positions.

Experimental top

Colourless crystals of the title compound were obtained from a solution of 0.07 g (0.4 mmol) GaCl3 and 0.5 ml tetrahydrofuran in 20 ml pentane at 267 K. The NMR spectra were recorded on a Bruker AM 250 spectrometer. GaCl3.thf: 1H-NMR (C6D6, internal TMS): δ 0.82 (m; CH2), 3.42 (m; OCH2). 13C{1H}NMR (C6D6, internal TMS): δ 24.6 (s; CH2), 71.8 (s; OCH2).

Refinement top

All H atoms were located in a difference Fourier synthesis. They were refined with fixed individual displacement parameters [U(H) = 1.2 Ueq(C)], using a riding model with C—H = 0.99 Å.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. Perspective view of the molecule, with the atom numbering; displacement ellipsoids are drawn at the 50% probability level. Symmetry operator for generating equivalent atoms: (i) x, −y + 1/2, z.
top
Crystal data top
[Ga(C4H8O)Cl3]F(000) = 244
Mr = 248.17Dx = 1.819 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 7266 reflections
a = 6.2048 (9) Åθ = 3.8–29.8°
b = 10.3980 (11) ŵ = 3.85 mm1
c = 7.3089 (10) ÅT = 173 K
β = 106.085 (11)°Plate, colourless
V = 453.09 (10) Å30.30 × 0.20 × 0.10 mm
Z = 2
Data collection top
STOE IPDS II two-circle
diffractometer
1356 independent reflections
Radiation source: fine-focus sealed tube1200 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
ω scansθmax = 29.8°, θmin = 3.8°
Absorption correction: multi-scan
(MULABS; Spek, 1990; Blessing, 1995)
h = 87
Tmin = 0.392, Tmax = 0.700k = 1414
6794 measured reflectionsl = 1010
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.093 w = 1/[σ2(Fo2) + (0.0482P)2 + 0.2393P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
1356 reflectionsΔρmax = 0.66 e Å3
47 parametersΔρmin = 1.01 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.051 (6)
Crystal data top
[Ga(C4H8O)Cl3]V = 453.09 (10) Å3
Mr = 248.17Z = 2
Monoclinic, P21/mMo Kα radiation
a = 6.2048 (9) ŵ = 3.85 mm1
b = 10.3980 (11) ÅT = 173 K
c = 7.3089 (10) Å0.30 × 0.20 × 0.10 mm
β = 106.085 (11)°
Data collection top
STOE IPDS II two-circle
diffractometer
1356 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 1990; Blessing, 1995)
1200 reflections with I > 2σ(I)
Tmin = 0.392, Tmax = 0.700Rint = 0.070
6794 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0350 restraints
wR(F2) = 0.093H-atom parameters constrained
S = 1.04Δρmax = 0.66 e Å3
1356 reflectionsΔρmin = 1.01 e Å3
47 parameters
Special details top

Experimental.

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
Ga10.43452 (6)0.25000.62919 (5)0.03059 (16)
Cl10.75135 (17)0.25000.56595 (16)0.0540 (3)
Cl20.37313 (15)0.07687 (9)0.76462 (13)0.0619 (3)
O10.2102 (5)0.25000.3882 (4)0.0391 (6)
C10.1263 (7)0.3663 (3)0.2771 (5)0.0587 (9)
H1A0.04080.42060.34370.070*
H1B0.25200.41740.25620.070*
C20.0193 (9)0.3195 (4)0.0959 (5)0.0785 (13)
H2A0.17380.35180.07810.094*
H2B0.03550.35180.01060.094*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ga10.0276 (2)0.0329 (2)0.0286 (2)0.0000.00337 (14)0.000
Cl10.0355 (5)0.0812 (8)0.0482 (5)0.0000.0165 (4)0.000
Cl20.0547 (5)0.0619 (5)0.0611 (5)0.0124 (4)0.0028 (4)0.0292 (4)
O10.0415 (14)0.0309 (12)0.0357 (12)0.0000.0047 (10)0.000
C10.067 (2)0.0387 (14)0.0530 (17)0.0087 (15)0.0128 (15)0.0144 (12)
C20.106 (3)0.064 (2)0.0430 (16)0.031 (2)0.0179 (18)0.0066 (15)
Geometric parameters (Å, º) top
Ga1—O11.919 (3)C1—H1A0.990
Ga1—Cl22.1388 (8)C1—H1B0.990
Ga1—Cl12.1405 (11)C2—C2i1.446 (9)
O1—C11.469 (3)C2—H2A0.990
C1—C21.464 (5)C2—H2B0.990
O1—Ga1—Cl2104.36 (5)C2—C1—H1B110.7
Cl2—Ga1—Cl2i114.63 (6)O1—C1—H1B110.7
O1—Ga1—Cl1106.13 (10)H1A—C1—H1B108.8
Cl2—Ga1—Cl1113.08 (3)C2i—C2—C1109.4 (2)
C1—O1—C1i110.8 (3)C2i—C2—H2A109.8
C1—O1—Ga1124.27 (16)C1—C2—H2A109.8
C2—C1—O1105.2 (3)C2i—C2—H2B109.8
C2—C1—H1A110.7C1—C2—H2B109.8
O1—C1—H1A110.7H2A—C2—H2B108.2
Cl2—Ga1—O1—C1155.4 (3)C1i—O1—C1—C22.0 (6)
Cl1—Ga1—O1—C185.0 (3)Ga1—O1—C1—C2173.1 (3)
Cl2—Ga1—O1—C1i34.7 (3)O1—C1—C2—C2i1.2 (4)
Symmetry code: (i) x, y+1/2, z.

Experimental details

Crystal data
Chemical formula[Ga(C4H8O)Cl3]
Mr248.17
Crystal system, space groupMonoclinic, P21/m
Temperature (K)173
a, b, c (Å)6.2048 (9), 10.3980 (11), 7.3089 (10)
β (°) 106.085 (11)
V3)453.09 (10)
Z2
Radiation typeMo Kα
µ (mm1)3.85
Crystal size (mm)0.30 × 0.20 × 0.10
Data collection
DiffractometerSTOE IPDS II two-circle
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 1990; Blessing, 1995)
Tmin, Tmax0.392, 0.700
No. of measured, independent and
observed [I > 2σ(I)] reflections
6794, 1356, 1200
Rint0.070
(sin θ/λ)max1)0.699
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.093, 1.04
No. of reflections1356
No. of parameters47
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.66, 1.01

Computer programs: X-AREA (Stoe & Cie, 2001), X-AREA, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991), SHELXL97.

Selected geometric parameters (Å, º) top
Ga1—O11.919 (3)Ga1—Cl12.1405 (11)
Ga1—Cl22.1388 (8)
O1—Ga1—Cl2104.36 (5)O1—Ga1—Cl1106.13 (10)
Cl2—Ga1—Cl2i114.63 (6)Cl2—Ga1—Cl1113.08 (3)
Symmetry code: (i) x, y+1/2, z.
 

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