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KCrO3Cl, potassium trioxochlorochromate(VI), has been redetermined from room-temperature single-crystal X-ray data. The Cr atom is tetrahedrally coordinated by three O atoms (average Cr-O bond length 1.597 Å) and one Cl atom at 2.1916 (8) Å, with nearly ideal tetrahedral angles. The K ion is coordinated by eight O and three Cl atoms. Isolated CrO3Cl tetrahedra and K ions are connected via common ligands. All atoms are in general positions.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Cr-O) = 0.002 Å
- R factor = 0.028
- wR factor = 0.079
- Data-to-parameter ratio = 19.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Data collection: COLLECT (Nonius, 2001); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Shape Software, 1999) and ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
potassium trioxochloro(I)chromate(VI)
top
Crystal data top
KCrO3Cl | F(000) = 336 |
Mr = 174.55 | Dx = 2.528 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1435 reflections |
a = 7.838 (2) Å | θ = 2.0–30.0° |
b = 7.493 (1) Å | µ = 3.84 mm−1 |
c = 7.812 (2) Å | T = 293 K |
β = 91.40 (3)° | Tabular, brown–orange |
V = 458.66 (18) Å3 | 0.20 × 0.10 × 0.02 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 1102 independent reflections |
Radiation source: fine-focus sealed tube | 924 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
ω scans | θmax = 27.9°, θmin = 2.6° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | h = −10→10 |
Tmin = 0.514, Tmax = 0.927 | k = −9→9 |
2117 measured reflections | l = −10→10 |
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)] = 0.028 | w = 1/[σ2(Fo2) + (0.04P)2 + 0.08P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.079 | (Δ/σ)max = 0.001 |
S = 1.16 | Δρmax = 0.57 e Å−3 |
1102 reflections | Δρmin = −0.38 e Å−3 |
56 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.015 (2) |
Special details top
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 | |
K | 0.30127 (8) | 0.63961 (7) | 0.86872 (6) | 0.03601 (19) | |
Cr | 0.28241 (5) | 0.12435 (4) | 0.87486 (4) | 0.02481 (16) | |
Cl | 0.04765 (8) | 0.28306 (8) | 0.85952 (8) | 0.0406 (2) | |
O1 | 0.4366 (2) | 0.2626 (2) | 0.8906 (3) | 0.0479 (5) | |
O2 | 0.2965 (2) | 0.0072 (2) | 0.7049 (2) | 0.0457 (5) | |
O3 | 0.2764 (3) | −0.0052 (2) | 1.0374 (2) | 0.0493 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K | 0.0489 (4) | 0.0303 (3) | 0.0287 (3) | −0.0019 (2) | −0.0029 (3) | −0.00078 (18) |
Cr | 0.0256 (3) | 0.0236 (2) | 0.0252 (2) | −0.00018 (13) | 0.00016 (17) | −0.00001 (12) |
Cl | 0.0309 (3) | 0.0416 (4) | 0.0491 (4) | 0.0069 (2) | −0.0001 (3) | −0.0004 (3) |
O1 | 0.0342 (10) | 0.0367 (10) | 0.0724 (13) | −0.0082 (8) | −0.0048 (9) | −0.0026 (9) |
O2 | 0.0501 (12) | 0.0480 (11) | 0.0388 (9) | 0.0106 (9) | −0.0010 (8) | −0.0146 (8) |
O3 | 0.0530 (12) | 0.0519 (12) | 0.0435 (10) | 0.0119 (9) | 0.0096 (9) | 0.0195 (9) |
Geometric parameters (Å, º) top
K—O3i | 2.7798 (18) | Cr—O3 | 1.5997 (17) |
K—O1ii | 2.847 (2) | Cr—Cl | 2.1916 (8) |
K—O2iii | 2.8485 (18) | Cr—Kviii | 3.6356 (8) |
K—O3iv | 2.979 (2) | Cr—Kix | 3.8191 (14) |
K—O1 | 3.0210 (19) | Cl—Kx | 3.4023 (13) |
K—O2iv | 3.037 (2) | Cl—Kvii | 3.5505 (14) |
K—O1v | 3.063 (2) | O1—Kii | 2.847 (2) |
K—Cl | 3.3297 (9) | O1—Kix | 3.063 (2) |
K—O2v | 3.368 (2) | O2—Ki | 2.8485 (18) |
K—Clvi | 3.4023 (13) | O2—Kviii | 3.037 (2) |
K—Clvii | 3.5505 (14) | O2—Kix | 3.368 (2) |
K—Criv | 3.6356 (8) | O3—Kiii | 2.7798 (18) |
Cr—O1 | 1.5938 (18) | O3—Kviii | 2.979 (2) |
Cr—O2 | 1.5977 (16) | | |
| | | |
O3i—K—O1ii | 137.83 (6) | O3iv—K—Clvi | 83.64 (4) |
O3i—K—O2iii | 135.75 (6) | O1—K—Clvi | 126.99 (4) |
O1ii—K—O2iii | 61.06 (6) | O2iv—K—Clvi | 59.42 (4) |
O3i—K—O3iv | 137.05 (6) | O1v—K—Clvi | 95.86 (4) |
O1ii—K—O3iv | 62.07 (5) | Cl—K—Clvi | 76.72 (2) |
O2iii—K—O3iv | 86.26 (5) | O2v—K—Clvi | 138.37 (4) |
O3i—K—O1 | 74.35 (6) | O3i—K—Clvii | 125.34 (5) |
O1ii—K—O1 | 87.52 (5) | O1ii—K—Clvii | 96.73 (5) |
O2iii—K—O1 | 66.37 (6) | O2iii—K—Clvii | 58.94 (5) |
O3iv—K—O1 | 146.86 (6) | O3iv—K—Clvii | 61.97 (4) |
O3i—K—O2iv | 86.36 (5) | O1—K—Clvii | 113.16 (4) |
O1ii—K—O2iv | 92.64 (5) | O2iv—K—Clvii | 95.87 (4) |
O2iii—K—O2iv | 137.60 (5) | O1v—K—Clvii | 152.32 (4) |
O3iv—K—O2iv | 51.37 (5) | Cl—K—Clvii | 71.08 (2) |
O1—K—O2iv | 150.77 (6) | O2v—K—Clvii | 152.64 (4) |
O3i—K—O1v | 61.70 (6) | Clvi—K—Clvii | 68.95 (2) |
O1ii—K—O1v | 82.78 (5) | O1—Cr—O2 | 110.70 (11) |
O2iii—K—O1v | 138.61 (6) | O1—Cr—O3 | 111.70 (11) |
O3iv—K—O1v | 94.36 (5) | O2—Cr—O3 | 109.29 (10) |
O1—K—O1v | 94.50 (4) | O1—Cr—Cl | 106.59 (7) |
O2iv—K—O1v | 56.63 (5) | O2—Cr—Cl | 109.13 (7) |
O3i—K—Cl | 70.18 (4) | O3—Cr—Cl | 109.38 (7) |
O1ii—K—Cl | 129.92 (4) | K—Cl—Kvii | 108.92 (2) |
O2iii—K—Cl | 71.87 (4) | Kx—Cl—Kvii | 75.16 (3) |
O3iv—K—Cl | 132.93 (5) | Cr—O1—Kii | 138.75 (11) |
O1—K—Cl | 57.28 (4) | Cr—O1—K | 109.81 (9) |
O2iv—K—Cl | 135.84 (4) | Kii—O1—K | 92.48 (5) |
O1v—K—Cl | 129.57 (4) | Cr—O1—Kix | 105.85 (9) |
O3i—K—O2v | 77.22 (6) | Kii—O1—Kix | 91.67 (6) |
O1ii—K—O2v | 61.64 (6) | K—O1—Kix | 118.96 (6) |
O2iii—K—O2v | 94.42 (6) | Cr—O2—Ki | 168.85 (10) |
O3iv—K—O2v | 114.22 (6) | Cr—O2—Kviii | 98.54 (8) |
O1—K—O2v | 53.52 (5) | Ki—O2—Kviii | 92.17 (5) |
O2iv—K—O2v | 101.37 (4) | Cr—O2—Kix | 93.68 (8) |
O1v—K—O2v | 47.90 (5) | Ki—O2—Kix | 85.58 (6) |
Cl—K—O2v | 108.71 (4) | Kviii—O2—Kix | 109.70 (6) |
O3i—K—Clvi | 65.76 (5) | Cr—O3—Kiii | 162.97 (12) |
O1ii—K—Clvi | 145.35 (4) | Cr—O3—Kviii | 100.80 (8) |
O2iii—K—Clvi | 125.22 (5) | Kiii—O3—Kviii | 94.83 (5) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+2; (iii) x, −y+1/2, z+1/2; (iv) x, y+1, z; (v) −x+1, y+1/2, −z+3/2; (vi) −x, y+1/2, −z+3/2; (vii) −x, −y+1, −z+2; (viii) x, y−1, z; (ix) −x+1, y−1/2, −z+3/2; (x) −x, y−1/2, −z+3/2. |
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