InAlCl4 crystallizes in the baryte (BaSO4) structure type. The structure is characterized by AlCl4 tetrahedra and isolated InI cations.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (l-Al) = 0.003 Å
- R factor = 0.051
- wR factor = 0.174
- Data-to-parameter ratio = 38.7
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Al
| Author Response: aluminium is coordinated by a tetrahedron of iodine anions
compared to them is it considerably more confined in space
|
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
0 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
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.
indium(I) tetrachloroaluminate
top
Crystal data top
InAlCl4 | Dx = 2.636 Mg m−3 |
Mr = 283.60 | Melting point: not measured K |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 4273 reflections |
a = 10.937 (2) Å | θ = 2.8–28.3° |
b = 7.0519 (12) Å | µ = 4.80 mm−1 |
c = 9.2671 (19) Å | T = 298 K |
V = 714.7 (2) Å3 | Irregular, pale yellow |
Z = 4 | 0.3 × 0.2 × 0.1 mm |
F(000) = 520 | |
Data collection top
Stoe IPDS-II diffractometer | 1353 independent reflections |
Radiation source: fine-focus sealed tube | 720 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
2° φ scans | θmax = 32.2°, θmin = 2.9° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)] | h = −16→16 |
Tmin = 0.353, Tmax = 0.609 | k = −8→10 |
22140 measured reflections | l = −13→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.051 | w = 1/[σ2(Fo2) + (0.0685P)2 + 0.8739P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.174 | (Δ/σ)max < 0.001 |
S = 1.09 | Δρmax = 1.01 e Å−3 |
1353 reflections | Δρmin = −0.95 e Å−3 |
35 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.017 (2) |
Special details top
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope
and mounted in a glass capillary. The scattering intensities were collected
with an imaging plate diffractometer (Stoe IPDS-II) equipped with a
fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 30 mA. Intensity data were collected at 298 K by φ scans in 180 frames
(0 < φ < 200° exposure time of 6 min) in the 2Θ range 2.86 - 64.80
°·Structure solution and refinement were carried out using the program
SHELXL97 (Sheldrick, 1997). A numerical absorption correction
(X-RED (Stoe & Cie, 2001) was applied after optimization of the crystal
shape (X-SHAPE (Stoe & Cie, 1999)). The final difference maps were free
of any chemically significant features. The refinement was based on F2 for
ALL reflections. |
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 | x | y | z | Uiso*/Ueq | |
In | 0.31448 (8) | 0.2500 | 0.68576 (12) | 0.1199 (6) | |
Cl1 | 0.7228 (3) | 0.7500 | 0.9474 (3) | 0.0952 (9) | |
Al | 0.56727 (19) | 0.7500 | 0.8111 (2) | 0.0477 (5) | |
Cl2 | 0.57498 (15) | 0.9936 (2) | 0.67625 (16) | 0.0780 (5) | |
Cl3 | 0.4017 (3) | 0.7500 | 0.9276 (4) | 0.1233 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
In | 0.0668 (5) | 0.1646 (11) | 0.1284 (10) | 0.000 | 0.0027 (4) | 0.000 |
Cl1 | 0.0991 (18) | 0.1020 (18) | 0.0847 (16) | 0.000 | −0.0494 (14) | 0.000 |
Al | 0.0510 (10) | 0.0473 (10) | 0.0449 (9) | 0.000 | −0.0017 (8) | 0.000 |
Cl2 | 0.0799 (10) | 0.0670 (8) | 0.0872 (10) | −0.0059 (7) | −0.0122 (7) | 0.0294 (7) |
Cl3 | 0.097 (2) | 0.155 (3) | 0.118 (2) | 0.000 | 0.0568 (18) | 0.000 |
Geometric parameters (Å, º) top
Al—Cl1 | 2.119 (3) | Al—Cl2 | 2.1256 (17) |
Al—Cl2i | 2.1256 (17) | Al—Cl3 | 2.108 (3) |
| | | |
Cl3—Al—Cl1 | 112.59 (16) | Cl3—Al—Cl2 | 109.58 (10) |
Cl3—Al—Cl2i | 109.58 (10) | Cl1—Al—Cl2 | 108.58 (9) |
Cl1—Al—Cl2i | 108.58 (9) | Cl2i—Al—Cl2 | 107.81 (12) |
Symmetry code: (i) x, −y+3/2, z. |