(Acetonitrile-κN)trichloridogallium(III)

In the title complex, [GaCl₃(CH₃CN)], the Ga^III atom shows a slightly distorted tetra­hedral coordination, with three Cl atoms and one N atom of the acetonitrile as ligands. The Ga atom, one Cl atom, the N atom, both C atoms and one H atom of the acetonitrile mol­ecule are situated on a mirror plane. The crystal packing is stabilized by several weak inter­molecular C—H...Cl hydrogen-bonding contacts.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.017
• wR factor = 0.042
• Data-to-parameter ratio = 21.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT480_ALERT_4_B Long H...A H-Bond Reported H1     ..  CL2     ..       3.34 Ang.
PLAT480_ALERT_4_B Long H...A H-Bond Reported H2     ..  CL1     ..       3.44 Ang.
PLAT480_ALERT_4_B Long H...A H-Bond Reported H2     ..  CL2     ..       3.23 Ang.

Alert level C
PLAT031_ALERT_4_C Refined Extinction Parameter within Range ......       2.57 Sigma
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.73 mm
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct...          2
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Ga1
PLAT390_ALERT_3_C Deviating Methyl C2      X-C-H Bond Angle ......     117.00 Deg.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1     ..  CL1     ..       3.01 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2     ..  CL2     ..       2.90 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            CL1 -GA1 -N1  -C1      0.00  0.03   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          2
            CL2 -GA1 -N1  -C1   -119.72  0.04   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          3
            CL2 -GA1 -N1  -C1    119.72  0.03   7.565   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          4
            GA1 -N1  -C1  -C2     18.00  0.00   1.555   1.555   1.555   1.555

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
  11 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
   1 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
  11 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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S1. Comment

In the title adduct, the coordination of the Ga atom by the three Cl atoms and the N atom of the acetonitrile ligand can be considered as slightly distorted tetrahedral, with Cl—Ga—N bond angles in the range 104.68 (6)–105.14 (3) ° and Cl—Ga—Cl bond angles in the range 113.371 (17)–113.93 (3) ° (Fig. 1).

The C_s-symmetric molecule exhibits an almost linear Ga—N1—C1—C2 unit (C1—N1—Ga1 = 179.22 (19) °, N1—C1—C2 = 179.9 (3) °), and the H atoms of the methyl group adopt a staggered conformation relative to the Cl atoms.

In the crystal structure, the GaCl₃^.CH₃CN adducts are linked by very weak intermolecular C—H···Cl interactions (Fig. 2, Table).

Related literature

For related literature, see: Herler et al. (2005).

S2. Experimental

The title compound was unintentionally obtained as a by-product of an attempted reaction of 4-bis(trimethylsilyl)-amino-1,2,4,3,5-triazadiphosphole GaCl₃ adduct (Herler et al., 2005) with Cr(CH₃CN)₃(CO)₃ in CH₂Cl₂. Recrystallization from a saturated CH₂Cl₂/Et₂O solution at ambient temperature gave colourless needle-like crystals of GaCl₃^.CH₃CN.

S3. Refinement

All Hydrogen atoms were found from difference Fourier maps and were refined freely.

Computing details

Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2 (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures

	Fig. 1. Molecular structure of (I), showing the atomic numbering scheme and displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (i) x, -y + 1/2, z.]
	Fig. 2. Part of the packing diagram of (I). Unique C—H···Cl interactions represented by dashed lines are shown for one molecule of (I). Colour code as in Fig. 1. [Symmetry codes: (i) x + 1, y, z; (ii) x + 1/2, y, -z + 1/2; (iii) -x + 1, y - 1/2, -z + 1; (iv) -x + 3/2, -y, z + 1/2; (v) -x + 1, -y, -z + 1.]

(Acetonitrile-κN)trichloridogallium(III)

Crystal data

[GaCl3(C2H3N)]	F(000) = 416
Mr = 217.12	Dx = 1.928 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 4237 reflections
a = 9.1760 (18) Å	θ = 5.8–56.4°
b = 7.5100 (15) Å	µ = 4.64 mm^−1
c = 10.857 (2) Å	T = 173 K
V = 748.2 (3) Å^3	Needle, colourless
Z = 4	0.73 × 0.12 × 0.09 mm

Data collection

Bruker–Nonius Apex X8 CCD diffractometer	1011 independent reflections
Radiation source: sealed tube	878 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.037
ω scans	θmax = 28.5°, θmin = 2.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −12→12
Tmin = 0.130, Tmax = 0.660	k = −10→9
11546 measured reflections	l = −14→14

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.017	All H-atom parameters refined
wR(F^2) = 0.042	w = 1/[σ^2(Fo^2) + (0.0212P)^2 + 0.2025P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max < 0.001
1011 reflections	Δρmax = 0.28 e Å^−3
48 parameters	Δρmin = −0.38 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0018 (7)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ga1	0.41273 (2)	0.2500	0.356223 (19)	0.02617 (9)
Cl1	0.25406 (7)	0.2500	0.50041 (6)	0.04725 (17)
Cl2	0.41187 (5)	0.01076 (6)	0.24861 (4)	0.04570 (13)
N1	0.60162 (19)	0.2500	0.44199 (18)	0.0359 (4)
C1	0.7096 (2)	0.2500	0.4926 (2)	0.0331 (5)
C2	0.8469 (3)	0.2500	0.5568 (3)	0.0437 (6)
H1	0.926 (5)	0.2500	0.511 (6)	0.13 (2)*
H2	0.861 (3)	0.159 (4)	0.605 (3)	0.106 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ga1	0.02312 (12)	0.02984 (13)	0.02554 (13)	0.000	0.00012 (8)	0.000
Cl1	0.0414 (3)	0.0532 (3)	0.0472 (3)	0.000	0.0204 (3)	0.000
Cl2	0.0555 (3)	0.0393 (2)	0.0424 (2)	−0.00081 (19)	0.00219 (17)	−0.01284 (17)
N1	0.0290 (9)	0.0415 (10)	0.0372 (10)	0.000	−0.0038 (8)	0.000
C1	0.0296 (10)	0.0345 (11)	0.0352 (11)	0.000	−0.0010 (8)	0.000
C2	0.0288 (11)	0.0513 (15)	0.0512 (16)	0.000	−0.0133 (11)	0.000

Geometric parameters (Å, º)

Ga1—N1	1.9676 (18)	N1—C1	1.133 (3)
Ga1—Cl1	2.1379 (7)	C1—C2	1.440 (3)
Ga1—Cl2	2.1432 (5)	C2—H1	0.88 (5)
Ga1—Cl2^i	2.1432 (5)	C2—H2	0.87 (3)
N1—Ga1—Cl1	104.68 (6)	C1—N1—Ga1	179.22 (19)
N1—Ga1—Cl2	105.14 (3)	N1—C1—C2	179.9 (3)
Cl1—Ga1—Cl2	113.371 (17)	C1—C2—H1	116 (4)
N1—Ga1—Cl2^i	105.14 (3)	C1—C2—H2	115 (2)
Cl1—Ga1—Cl2^i	113.371 (17)	H1—C2—H2	103 (3)
Cl2—Ga1—Cl2^i	113.93 (3)
Cl1—Ga1—N1—C1	0.00 (3)	Cl2^i—Ga1—N1—C1	119.72 (3)
Cl2—Ga1—N1—C1	−119.72 (4)	Ga1—N1—C1—C2	180 (100)

Symmetry code: (i) x, −y+1/2, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C2—H1···Cl1^ii	0.88 (5)	3.01 (5)	3.786 (3)	147 (5)
C2—H1···Cl2^iii	0.88 (5)	3.34 (5)	3.818 (3)	117 (3)
C2—H2···Cl1^iv	0.87 (3)	3.44 (3)	3.9172 (10)	117 (2)
C2—H2···Cl2^v	0.87 (3)	2.90 (3)	3.615 (2)	141 (2)
C2—H2···Cl2^vi	0.87 (3)	3.23 (3)	3.733 (3)	119 (2)

Symmetry codes: (ii) x+1, y, z; (iii) x+1/2, y, −z+1/2; (iv) −x+1, y−1/2, −z+1; (v) −x+3/2, −y, z+1/2; (vi) −x+1, −y, −z+1.