Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807043516/wm2142sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807043516/wm2142Isup2.hkl |
CCDC reference: 667186
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (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
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.
All Hydrogen atoms were found from difference Fourier maps and were refined freely.
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 Cs-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).
For related literature, see: Herler et al. (2005).
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).
[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) Å3 | Needle, colourless |
Z = 4 | 0.73 × 0.12 × 0.09 mm |
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 on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.017 | All H-atom parameters refined |
wR(F2) = 0.042 | w = 1/[σ2(Fo2) + (0.0212P)2 + 0.2025P] where P = (Fo2 + 2Fc2)/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+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0018 (7) |
[GaCl3(C2H3N)] | V = 748.2 (3) Å3 |
Mr = 217.12 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 9.1760 (18) Å | µ = 4.64 mm−1 |
b = 7.5100 (15) Å | T = 173 K |
c = 10.857 (2) Å | 0.73 × 0.12 × 0.09 mm |
Bruker–Nonius Apex X8 CCD diffractometer | 1011 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) | 878 reflections with I > 2σ(I) |
Tmin = 0.130, Tmax = 0.660 | Rint = 0.037 |
11546 measured reflections |
R[F2 > 2σ(F2)] = 0.017 | 0 restraints |
wR(F2) = 0.042 | All H-atom parameters refined |
S = 1.04 | Δρmax = 0.28 e Å−3 |
1011 reflections | Δρmin = −0.38 e Å−3 |
48 parameters |
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. |
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)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
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 |
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—Cl2i | 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—Cl2i | 105.14 (3) | C1—C2—H2 | 115 (2) |
Cl1—Ga1—Cl2i | 113.371 (17) | H1—C2—H2 | 103 (3) |
Cl2—Ga1—Cl2i | 113.93 (3) | ||
Cl1—Ga1—N1—C1 | 0.00 (3) | Cl2i—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. |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H1···Cl1ii | 0.88 (5) | 3.01 (5) | 3.786 (3) | 147 (5) |
C2—H1···Cl2iii | 0.88 (5) | 3.34 (5) | 3.818 (3) | 117 (3) |
C2—H2···Cl1iv | 0.87 (3) | 3.44 (3) | 3.9172 (10) | 117 (2) |
C2—H2···Cl2v | 0.87 (3) | 2.90 (3) | 3.615 (2) | 141 (2) |
C2—H2···Cl2vi | 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. |
Experimental details
Crystal data | |
Chemical formula | [GaCl3(C2H3N)] |
Mr | 217.12 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 173 |
a, b, c (Å) | 9.1760 (18), 7.5100 (15), 10.857 (2) |
V (Å3) | 748.2 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.64 |
Crystal size (mm) | 0.73 × 0.12 × 0.09 |
Data collection | |
Diffractometer | Bruker–Nonius Apex X8 CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2004) |
Tmin, Tmax | 0.130, 0.660 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11546, 1011, 878 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.671 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.017, 0.042, 1.04 |
No. of reflections | 1011 |
No. of parameters | 48 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 0.28, −0.38 |
Computer programs: APEX2 (Bruker, 2003), SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2005), SHELXL97 (Sheldrick, 1997).
Ga1—N1 | 1.9676 (18) | Ga1—Cl2 | 2.1432 (5) |
Ga1—Cl1 | 2.1379 (7) | ||
N1—Ga1—Cl1 | 104.68 (6) | Cl1—Ga1—Cl2 | 113.371 (17) |
N1—Ga1—Cl2 | 105.14 (3) | Cl2—Ga1—Cl2i | 113.93 (3) |
Symmetry code: (i) x, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H1···Cl1ii | 0.88 (5) | 3.01 (5) | 3.786 (3) | 147 (5) |
C2—H1···Cl2iii | 0.88 (5) | 3.34 (5) | 3.818 (3) | 117 (3) |
C2—H2···Cl1iv | 0.87 (3) | 3.44 (3) | 3.9172 (10) | 117 (2) |
C2—H2···Cl2v | 0.87 (3) | 2.90 (3) | 3.615 (2) | 141 (2) |
C2—H2···Cl2vi | 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. |
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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 Cs-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).