The title compound, dicaesium trichromium(VI) oxide, is the orthorhombic (space group Pbca) modification of Cs2Cr3O10. The compound is isotypic with its NH4 and Rb trichromate analogues. The structure contains discrete [Cr3O10]2− anions [Cr—O—Cr = 136.58 (11) and 140.30 (12)°] linked via two non-equivalent irregularly 11-coordinated Cs+ cations [dav(Cs—O) = 3.224 and 3.272 Å]. 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 = 0.019
- wR factor = 0.052
- Data-to-parameter ratio = 29.7
checkCIF/PLATON results
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Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Cr1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Cr2
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Cr3
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2003); 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); ORTEP-3 for Windows (Farrugia, 1997).
dicesium trichromium(VI) oxide
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Crystal data top
Cs2Cr3O10 | F(000) = 2096 |
Mr = 581.82 | Dx = 3.449 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 4564 reflections |
a = 11.887 (2) Å | θ = 2.0–32.6° |
b = 9.671 (2) Å | µ = 9.29 mm−1 |
c = 19.493 (4) Å | T = 293 K |
V = 2240.9 (8) Å3 | Tabular, orange |
Z = 8 | 0.10 × 0.10 × 0.05 mm |
Data collection top
Nonius KappaCCD diffractometer | 4071 independent reflections |
Radiation source: fine-focus sealed tube | 3587 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.011 |
ψ and ω scans | θmax = 32.6°, θmin = 2.7° |
Absorption correction: multi-scan HKL SCALEPACK (Otwinowski & Minor, 1997) | h = −17→17 |
Tmin = 0.457, Tmax = 0.654 | k = −14→14 |
7678 measured reflections | l = −29→29 |
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)] = 0.019 | w = 1/[σ2(Fo2) + (0.028P)2 + 1.72P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.053 | (Δ/σ)max = 0.002 |
S = 1.05 | Δρmax = 0.59 e Å−3 |
4071 reflections | Δρmin = −0.87 e Å−3 |
137 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00197 (7) |
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 | |
Cs1 | 0.551246 (12) | 0.646114 (15) | 0.416422 (7) | 0.02978 (5) | |
Cs2 | 0.225573 (12) | 0.774086 (15) | 0.320165 (8) | 0.03163 (5) | |
Cr1 | 0.31124 (3) | 0.50625 (4) | −0.024272 (17) | 0.02531 (7) | |
Cr2 | 0.37664 (3) | 0.69456 (4) | 0.112922 (17) | 0.02531 (7) | |
Cr3 | 0.49513 (3) | 0.50362 (4) | 0.232628 (18) | 0.02427 (7) | |
O1 | 0.3544 (3) | 0.3499 (2) | −0.02371 (13) | 0.0629 (7) | |
O2 | 0.18390 (17) | 0.5129 (2) | −0.05239 (11) | 0.0441 (5) | |
O3 | 0.38996 (17) | 0.6022 (2) | −0.07125 (10) | 0.0439 (4) | |
O4 | 0.31084 (17) | 0.5724 (2) | 0.06318 (9) | 0.0395 (4) | |
O5 | 0.28273 (17) | 0.7574 (3) | 0.16140 (11) | 0.0491 (5) | |
O6 | 0.42874 (19) | 0.8151 (2) | 0.06763 (11) | 0.0442 (4) | |
O7 | 0.48350 (16) | 0.6242 (2) | 0.16099 (9) | 0.0368 (4) | |
O8 | 0.62195 (16) | 0.5187 (2) | 0.26009 (11) | 0.0413 (4) | |
O9 | 0.40740 (15) | 0.54400 (19) | 0.29248 (9) | 0.0345 (4) | |
O10 | 0.4713 (2) | 0.34858 (19) | 0.20758 (11) | 0.0480 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cs1 | 0.03058 (8) | 0.03135 (8) | 0.02740 (7) | −0.00003 (5) | −0.00390 (5) | 0.00029 (5) |
Cs2 | 0.03385 (8) | 0.02909 (8) | 0.03193 (8) | 0.00131 (5) | −0.00477 (5) | −0.00476 (5) |
Cr1 | 0.03152 (17) | 0.02517 (16) | 0.01923 (15) | 0.00092 (13) | −0.00251 (12) | −0.00123 (11) |
Cr2 | 0.02894 (16) | 0.02843 (16) | 0.01856 (14) | −0.00166 (13) | −0.00057 (12) | −0.00149 (12) |
Cr3 | 0.02743 (16) | 0.02293 (15) | 0.02244 (15) | −0.00145 (12) | 0.00058 (12) | −0.00026 (11) |
O1 | 0.100 (2) | 0.0376 (11) | 0.0507 (13) | 0.0266 (12) | −0.0015 (13) | 0.0015 (9) |
O2 | 0.0371 (9) | 0.0575 (12) | 0.0377 (10) | −0.0115 (9) | −0.0107 (8) | 0.0051 (9) |
O3 | 0.0414 (10) | 0.0545 (12) | 0.0359 (9) | −0.0095 (9) | 0.0059 (8) | 0.0033 (9) |
O4 | 0.0481 (10) | 0.0456 (10) | 0.0247 (8) | −0.0112 (9) | −0.0030 (7) | −0.0082 (7) |
O5 | 0.0398 (11) | 0.0665 (15) | 0.0411 (11) | 0.0041 (9) | 0.0071 (8) | −0.0213 (10) |
O6 | 0.0536 (11) | 0.0353 (9) | 0.0436 (11) | −0.0017 (9) | 0.0020 (9) | 0.0123 (8) |
O7 | 0.0379 (9) | 0.0442 (10) | 0.0282 (8) | −0.0016 (8) | −0.0045 (7) | 0.0089 (7) |
O8 | 0.0302 (8) | 0.0461 (10) | 0.0476 (11) | 0.0011 (8) | −0.0061 (7) | 0.0127 (9) |
O9 | 0.0373 (9) | 0.0359 (9) | 0.0304 (8) | −0.0005 (7) | 0.0070 (7) | −0.0031 (7) |
O10 | 0.0753 (14) | 0.0296 (9) | 0.0393 (10) | −0.0112 (9) | 0.0108 (10) | −0.0103 (7) |
Geometric parameters (Å, º) top
Cs1—O1i | 3.084 (2) | Cs2—O2ii | 3.265 (2) |
Cs1—O3ii | 3.108 (2) | Cs2—O10vi | 3.289 (2) |
Cs1—O9 | 3.1203 (19) | Cs2—O8i | 3.366 (2) |
Cs1—O10i | 3.1222 (19) | Cs2—O1v | 3.406 (3) |
Cs1—O4iii | 3.192 (2) | Cs2—O10i | 3.714 (3) |
Cs1—O6iv | 3.225 (2) | Cr1—O1 | 1.597 (2) |
Cs1—O2v | 3.2479 (19) | Cr1—O3 | 1.605 (2) |
Cs1—O6ii | 3.309 (2) | Cr1—O2 | 1.6111 (19) |
Cs1—O5iii | 3.321 (2) | Cr1—O4 | 1.8209 (18) |
Cs1—O2iii | 3.342 (2) | Cr2—O5 | 1.584 (2) |
Cs1—O8 | 3.393 (2) | Cr2—O6 | 1.588 (2) |
Cs2—O9vi | 3.0990 (19) | Cr2—O4 | 1.7168 (18) |
Cs2—O3ii | 3.119 (2) | Cr2—O7 | 1.7190 (18) |
Cs2—O9 | 3.1487 (18) | Cr3—O10 | 1.6021 (18) |
Cs2—O8vii | 3.172 (2) | Cr3—O8 | 1.6063 (19) |
Cs2—O5 | 3.173 (2) | Cr3—O9 | 1.6128 (17) |
Cs2—O7vii | 3.2430 (19) | Cr3—O7 | 1.8243 (18) |
| | | |
O1—Cr1—O3 | 111.36 (13) | O6—Cr2—O7 | 107.79 (10) |
O1—Cr1—O2 | 110.01 (14) | O4—Cr2—O7 | 111.84 (10) |
O3—Cr1—O2 | 109.30 (11) | O10—Cr3—O8 | 110.63 (12) |
O1—Cr1—O4 | 109.09 (11) | O10—Cr3—O9 | 109.45 (10) |
O3—Cr1—O4 | 109.42 (10) | O8—Cr3—O9 | 110.10 (11) |
O2—Cr1—O4 | 107.58 (10) | O10—Cr3—O7 | 110.57 (10) |
O5—Cr2—O6 | 108.96 (13) | O8—Cr3—O7 | 105.56 (9) |
O5—Cr2—O4 | 106.26 (11) | O9—Cr3—O7 | 110.48 (9) |
O6—Cr2—O4 | 111.63 (11) | Cr2—O4—Cr1 | 140.30 (12) |
O5—Cr2—O7 | 110.34 (11) | Cr2—O7—Cr3 | 136.58 (11) |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) x, −y+3/2, z+1/2; (iii) x+1/2, y, −z+1/2; (iv) −x+1, y−1/2, −z+1/2; (v) −x+1/2, −y+1, z+1/2; (vi) −x+1/2, y+1/2, z; (vii) x−1/2, y, −z+1/2. |