Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803020464/br6120sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803020464/br6120Isup2.hkl |
CCDC reference: 225683
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (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
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.
[Al(C2H6OS)6]Cl3 | Dx = 1.461 Mg m−3 |
Mr = 602.14 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 1340 reflections |
Hall symbol: -R 3 | θ = 3.0–30.0° |
a = 10.3760 (6) Å | µ = 0.85 mm−1 |
c = 22.0210 (12) Å | T = 150 K |
V = 2053.2 (2) Å3 | Fragment, colourless |
Z = 3 | 0.25 × 0.20 × 0.15 mm |
F(000) = 948 |
Nonius KappaCCD diffractometer | 1340 independent reflections |
Radiation source: fine-focus sealed tube, KappaCCD | 1266 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
φ and ω scans | θmax = 30.0°, θmin = 3.9° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997)' | h = −12→12 |
Tmin = 0.816, Tmax = 0.883 | k = −14→14 |
2680 measured reflections | l = −30→30 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-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 = 1.11 | Δρmax = 0.50 e Å−3 |
1340 reflections | Δρmin = −0.43 e Å−3 |
44 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0018 (3) |
Primary atom site location: structure-invariant direct methods |
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 | ||
Cl1 | 0.0000 | 0.0000 | 0.0000 | 0.02766 (17) | |
Cl2 | 0.0000 | 0.0000 | 0.2509 | 0.03096 (14) | |
C1 | 0.24971 (17) | 0.24361 (15) | 0.12848 (6) | 0.0321 (3) | |
H1A | 0.1855 | 0.1497 | 0.1093 | 0.039* | |
H1B | 0.2216 | 0.2394 | 0.1703 | 0.039* | |
H1C | 0.3508 | 0.2647 | 0.1262 | 0.039* | |
C2 | 0.30666 (14) | 0.37757 (14) | 0.01919 (6) | 0.0271 (3) | |
H2A | 0.3154 | 0.4569 | −0.0061 | 0.032* | |
H2B | 0.2411 | 0.2837 | 0.0003 | 0.032* | |
H2C | 0.4030 | 0.3874 | 0.0246 | 0.032* | |
S | 0.23359 (3) | 0.38616 (3) | 0.090813 (13) | 0.01964 (11) | |
Al | 0.3333 | 0.6667 | 0.1667 | 0.01667 (17) | |
O | 0.35982 (9) | 0.53114 (9) | 0.11850 (4) | 0.02161 (18) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cl1 | 0.0216 (3) | 0.022 | 0.0398 (4) | 0.011 | 0.000 | 0.000 |
Cl2 | 0.0334 (3) | 0.033 | 0.0260 (3) | 0.017 | 0.000 | 0.000 |
C1 | 0.0406 (7) | 0.0220 (6) | 0.0334 (7) | 0.0154 (5) | 0.0013 (5) | 0.0055 (5) |
C2 | 0.0277 (6) | 0.0240 (6) | 0.0246 (6) | 0.0094 (5) | 0.0027 (4) | −0.0024 (4) |
S | 0.01714 (15) | 0.01628 (14) | 0.02438 (16) | 0.00753 (10) | 0.00040 (9) | −0.00070 (9) |
Al | 0.0149 (2) | 0.0149 (2) | 0.0201 (4) | 0.00747 (11) | 0.000 | 0.000 |
O | 0.0181 (4) | 0.0184 (4) | 0.0278 (4) | 0.0088 (3) | −0.0010 (3) | −0.0051 (3) |
C1—S | 1.7751 (13) | S—O | 1.5427 (8) |
C1—H1A | 0.9600 | Al—Oi | 1.8880 (8) |
C1—H1B | 0.9599 | Al—Oii | 1.8880 (8) |
C1—H1C | 0.9601 | Al—Oiii | 1.8880 (8) |
C2—S | 1.7715 (12) | Al—Oiv | 1.8880 (8) |
C2—H2A | 0.9600 | Al—O | 1.8880 (8) |
C2—H2B | 0.9599 | Al—Ov | 1.8880 (8) |
C2—H2C | 0.9600 | ||
S—C1—H1A | 109.5 | Oi—Al—Oiii | 91.52 (4) |
S—C1—H1B | 109.5 | Oii—Al—Oiii | 88.48 (4) |
H1A—C1—H1B | 109.5 | Oi—Al—Oiv | 88.48 (4) |
S—C1—H1C | 109.5 | Oii—Al—Oiv | 91.52 (4) |
H1A—C1—H1C | 109.5 | Oiii—Al—Oiv | 180.0 |
H1B—C1—H1C | 109.5 | Oi—Al—O | 91.52 (4) |
S—C2—H2A | 109.5 | Oii—Al—O | 88.48 (4) |
S—C2—H2B | 109.5 | Oiii—Al—O | 91.52 (4) |
H2A—C2—H2B | 109.5 | Oiv—Al—O | 88.48 (4) |
S—C2—H2C | 109.5 | Oi—Al—Ov | 88.48 (4) |
H2A—C2—H2C | 109.5 | Oii—Al—Ov | 91.52 (4) |
H2B—C2—H2C | 109.5 | Oiii—Al—Ov | 88.48 (4) |
O—S—C2 | 102.99 (5) | Oiv—Al—Ov | 91.52 (4) |
O—S—C1 | 103.89 (6) | O—Al—Ov | 180.0 |
C2—S—C1 | 98.81 (6) | S—O—Al | 125.42 (5) |
Oi—Al—Oii | 180.0 |
Symmetry codes: (i) −x+y, −x+1, z; (ii) x−y+2/3, x+1/3, −z+1/3; (iii) −y+1, x−y+1, z; (iv) y−1/3, −x+y+1/3, −z+1/3; (v) −x+2/3, −y+4/3, −z+1/3. |