Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804016198/bt6484sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804016198/bt6484Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Ta-Cl) = 0.003 Å
- R factor = 0.020
- wR factor = 0.042
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level B CHEMS01_ALERT_1_B The sum formula contains elements in the wrong order. Ta precedes Cl Sequence must be C, H, then alphabetical.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 K0.04
Alert level G ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.127 0.240 Tmin' and Tmax expected: 0.246 0.263 RR' = 0.564 Please check that your absorption correction is appropriate.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 4 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); 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: DIAMOND (Brandenburg, 1996) and XP in SHELXTL-Plus (Sheldrick, 1991).
K2TaCl6 | Melting point: unknown K |
Mr = 471.85 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, Fm3m | Cell parameters from 1314 reflections |
Hall symbol: -F 423 | θ = 1.9–28.2° |
a = 9.9935 (16) Å | µ = 13.37 mm−1 |
V = 998.1 (3) Å3 | T = 293 K |
Z = 4 | Cube, black |
F(000) = 852 | 0.1 × 0.1 × 0.1 mm |
Dx = 3.140 Mg m−3 |
Stoe IPDS-I diffractometer | 89 independent reflections |
Radiation source: fine-focus sealed tube | 89 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: not measured pixels mm-1 | θmax = 27.8°, θmin = 3.5° |
φ scans | h = −13→12 |
Absorption correction: numerical the absorption correction (X-RED; Stoe & Cie, 2002) was performed after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999) | k = −13→12 |
Tmin = 0.127, Tmax = 0.240 | l = −13→13 |
2354 measured reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.020 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.042 | w = 1/[σ2(Fo2) + 21.1812P] where P = (Fo2 + 2Fc2)/3 |
S = 1.23 | (Δ/σ)max < 0.001 |
89 reflections | Δρmax = 0.59 e Å−3 |
6 parameters | Δρmin = −0.87 e Å−3 |
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 (IPDS I, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA. Intensity data for K2TaCl6 were collected at 293 K by φ-scans in 100 frames (0 < φ < 200°; Δφ = 2°, exposure time of 5 min) in the 2 Θ range 3.80 to 56.30°. 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. |
x | y | z | Uiso*/Ueq | ||
Ta | 0.0000 | 0.0000 | 0.0000 | 0.0274 (3) | |
Cl | 0.0000 | −0.2399 (3) | 0.0000 | 0.0639 (10) | |
K | 0.2500 | −0.2500 | 0.2500 | 0.0614 (14) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta | 0.0274 (3) | 0.0274 (3) | 0.0274 (3) | 0.000 | 0.000 | 0.000 |
Cl | 0.0832 (15) | 0.0252 (13) | 0.0832 (15) | 0.000 | 0.000 | 0.000 |
K | 0.0614 (14) | 0.0614 (14) | 0.0614 (14) | 0.000 | 0.000 | 0.000 |
Ta—Cli | 2.397 (3) | K—Clx | 3.5347 (6) |
Ta—Clii | 2.397 (3) | K—Clxi | 3.5347 (6) |
Ta—Cl | 2.397 (3) | K—Clxii | 3.5347 (6) |
Ta—Cliii | 2.397 (3) | K—Clxiii | 3.5347 (6) |
Ta—Cliv | 2.397 (3) | K—Clxiv | 3.5347 (6) |
Ta—Clv | 2.397 (3) | K—Clviii | 3.5347 (6) |
Cl—Kvi | 3.5347 (6) | K—Clxv | 3.5347 (6) |
Cl—K | 3.5347 (6) | K—Clv | 3.5347 (6) |
Cl—Kvii | 3.5347 (6) | K—Clvii | 3.5347 (6) |
Cl—Kviii | 3.5347 (6) | K—Cliii | 3.5347 (6) |
K—Clix | 3.5347 (6) | ||
Cli—Ta—Clii | 90.0 | Clix—K—Clviii | 119.973 (2) |
Cli—Ta—Cl | 90.0 | Clx—K—Clviii | 62.68 (8) |
Clii—Ta—Cl | 90.0 | Clxi—K—Clviii | 90.047 (3) |
Cli—Ta—Cliii | 180.0 | Cl—K—Clviii | 90.047 (3) |
Clii—Ta—Cliii | 90.0 | Clxii—K—Clviii | 57.31 (8) |
Cl—Ta—Cliii | 90.0 | Clxiii—K—Clviii | 119.973 (2) |
Cli—Ta—Cliv | 90.0 | Clxiv—K—Clviii | 119.973 (2) |
Clii—Ta—Cliv | 90.0 | Clix—K—Clxv | 119.973 (2) |
Cl—Ta—Cliv | 180.0 | Clx—K—Clxv | 90.047 (3) |
Cliii—Ta—Cliv | 90.0 | Clxi—K—Clxv | 62.68 (8) |
Cli—Ta—Clv | 90.0 | Cl—K—Clxv | 119.973 (2) |
Clii—Ta—Clv | 180.0 | Clxii—K—Clxv | 57.31 (8) |
Cl—Ta—Clv | 90.0 | Clxiii—K—Clxv | 90.047 (3) |
Cliii—Ta—Clv | 90.0 | Clxiv—K—Clxv | 62.68 (8) |
Cliv—Ta—Clv | 90.0 | Clviii—K—Clxv | 57.31 (8) |
Ta—Cl—Kvi | 91.64 (5) | Clix—K—Clv | 62.68 (8) |
Ta—Cl—K | 91.64 (5) | Clx—K—Clv | 90.047 (3) |
Kvi—Cl—K | 176.71 (9) | Clxi—K—Clv | 119.973 (2) |
Ta—Cl—Kvii | 91.64 (5) | Cl—K—Clv | 57.31 (8) |
Kvi—Cl—Kvii | 89.953 (3) | Clxii—K—Clv | 119.973 (2) |
K—Cl—Kvii | 89.953 (3) | Clxiii—K—Clv | 90.047 (3) |
Ta—Cl—Kviii | 91.64 (5) | Clxiv—K—Clv | 119.973 (2) |
Kvi—Cl—Kviii | 89.953 (3) | Clviii—K—Clv | 119.973 (2) |
K—Cl—Kviii | 89.953 (3) | Clxv—K—Clv | 176.71 (9) |
Kvii—Cl—Kviii | 176.71 (9) | Clix—K—Clvii | 62.68 (8) |
Clix—K—Clx | 57.31 (8) | Clx—K—Clvii | 119.973 (2) |
Clix—K—Clxi | 57.31 (8) | Clxi—K—Clvii | 90.047 (3) |
Clx—K—Clxi | 57.31 (8) | Cl—K—Clvii | 90.047 (3) |
Clix—K—Cl | 119.973 (2) | Clxii—K—Clvii | 119.973 (2) |
Clx—K—Cl | 119.973 (2) | Clxiii—K—Clvii | 57.31 (8) |
Clxi—K—Cl | 176.71 (9) | Clxiv—K—Clvii | 57.31 (8) |
Clix—K—Clxii | 176.71 (9) | Clviii—K—Clvii | 176.71 (9) |
Clx—K—Clxii | 119.973 (2) | Clxv—K—Clvii | 119.973 (2) |
Clxi—K—Clxii | 119.973 (2) | Clv—K—Clvii | 62.68 (8) |
Cl—K—Clxii | 62.68 (8) | Clix—K—Cliii | 90.047 (3) |
Clix—K—Clxiii | 119.973 (1) | Clx—K—Cliii | 62.68 (8) |
Clx—K—Clxiii | 176.71 (9) | Clxi—K—Cliii | 119.973 (2) |
Clxi—K—Clxiii | 119.973 (2) | Cl—K—Cliii | 57.31 (8) |
Cl—K—Clxiii | 62.68 (8) | Clxii—K—Cliii | 90.047 (3) |
Clxii—K—Clxiii | 62.68 (8) | Clxiii—K—Cliii | 119.973 (2) |
Clix—K—Clxiv | 90.047 (3) | Clxiv—K—Cliii | 176.71 (9) |
Clx—K—Clxiv | 119.973 (2) | Clviii—K—Cliii | 62.68 (8) |
Clxi—K—Clxiv | 62.68 (8) | Clxv—K—Cliii | 119.973 (2) |
Cl—K—Clxiv | 119.973 (2) | Clv—K—Cliii | 57.31 (8) |
Clxii—K—Clxiv | 90.047 (3) | Clvii—K—Cliii | 119.973 (2) |
Clxiii—K—Clxiv | 57.31 (8) |
Symmetry codes: (i) z, x, y; (ii) y, −x, −z; (iii) −z, −x, −y; (iv) −x, −y, −z; (v) −y, x, z; (vi) x−1/2, y, z−1/2; (vii) −x+1/2, −y−1/2, −z; (viii) −x, −y−1/2, −z+1/2; (ix) z+1/2, x, y+1/2; (x) y+1/2, −x, −z+1/2; (xi) x+1/2, y, z+1/2; (xii) z, x−1/2, y+1/2; (xiii) y+1/2, −x−1/2, −z; (xiv) −z+1/2, −x−1/2, −y; (xv) −y, x−1/2, z+1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register