Dicaesium cobalt(II) dioxalate tetrahydrate [tetraaquabis(μ-oxalato)cobalt(II)dicaesium(I)], Cs2CoII(C2O4)2·4H2O, has a layered structure and is isotypic with Cs2Mg(C2O4)2·4H2O. The unique Co atom shows octahedral coordination, with a mean Co—O bond length of 2.084 Å. The Cs atom is irregularly coordinated by nine O atoms. Layers of CoO4(H2O)2 octahedra, whose non-water O ligands belong to nearly planar bidentate oxalate groups, are separated by corrugated layers of Cs atoms. Medium-strong hydrogen bonds provide connections within the layer planes. All atoms are in general positions except the Co atom, which lies on a twofold axis.
Supporting information
CCDC reference: 239248
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.017
- wR factor = 0.042
- Data-to-parameter ratio = 23.3
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.338 0.545
Tmin and Tmax expected: 0.293 0.545
RR = 1.153
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.17
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.55 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C4 H8 Co1 Cs2 O12
Atom count from _chemical_formula_moiety:H800 Co400 Cs800 O800
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 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
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 2003); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL SCALEPACK and DENZO (Otwinowski & Minor, 1997); 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); software used to prepare material for publication: SHELXL97.
Dicaesium cobalt(II) dioxalate tetrahydrate
top
Crystal data top
Cs2Co(C2O4)2(H2O)4 | F(000) = 1060 |
Mr = 572.85 | Dx = 2.859 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2582 reflections |
a = 16.949 (3) Å | θ = 2.0–32.6° |
b = 7.368 (1) Å | µ = 6.74 mm−1 |
c = 13.540 (3) Å | T = 293 K |
β = 128.09 (3)° | Irregular, dark pink |
V = 1330.8 (7) Å3 | 0.19 × 0.18 × 0.09 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 2423 independent reflections |
Radiation source: fine-focus sealed tube | 2290 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.008 |
ψ and ω scans | θmax = 32.6°, θmin = 3.1° |
Absorption correction: multi-scan (HKL SCALEPACK; Otwinowski & Minor, 1997) | h = −25→25 |
Tmin = 0.338, Tmax = 0.545 | k = −11→11 |
4679 measured reflections | l = −20→20 |
Refinement top
Refinement on F2 | Primary atom site location: isomorphous structure methods |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.017 | w = 1/[σ2(Fo2) + (0.015P)2 + 2.66P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.042 | (Δ/σ)max = 0.001 |
S = 1.08 | Δρmax = 0.87 e Å−3 |
2423 reflections | Δρmin = −0.93 e Å−3 |
104 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00154 (10) |
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 | |
Cs | 0.152947 (9) | 0.315208 (16) | 0.108849 (10) | 0.03098 (5) | |
Co | 0.0000 | 0.33315 (4) | 0.2500 | 0.02028 (7) | |
C1 | 0.12908 (12) | 0.1857 (2) | 0.49770 (15) | 0.0226 (3) | |
C2 | 0.15826 (11) | 0.0875 (2) | 0.42282 (14) | 0.0219 (3) | |
O1 | 0.06240 (10) | 0.30724 (17) | 0.43929 (12) | 0.0262 (2) | |
O2 | 0.17079 (11) | 0.1360 (3) | 0.60733 (12) | 0.0386 (3) | |
O3 | 0.22512 (11) | −0.0284 (2) | 0.47609 (13) | 0.0366 (3) | |
O4 | 0.10792 (10) | 0.13303 (18) | 0.30847 (11) | 0.0266 (2) | |
OW5 | 0.10313 (10) | 0.5237 (2) | 0.28168 (14) | 0.0331 (3) | |
OW6 | −0.03449 (12) | 0.1640 (2) | −0.15203 (15) | 0.0336 (3) | |
H1 | 0.090 (3) | 0.627 (5) | 0.258 (3) | 0.059 (9)* | |
H2 | 0.159 (2) | 0.534 (4) | 0.356 (3) | 0.049 (8)* | |
H3 | −0.072 (2) | 0.164 (4) | −0.135 (3) | 0.039 (7)* | |
H4 | −0.054 (3) | 0.082 (5) | −0.196 (3) | 0.065 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cs | 0.02999 (7) | 0.03478 (7) | 0.02809 (7) | −0.00206 (4) | 0.01787 (5) | −0.00132 (4) |
Co | 0.02094 (13) | 0.01943 (13) | 0.01884 (13) | 0.000 | 0.01145 (11) | 0.000 |
C1 | 0.0205 (6) | 0.0273 (7) | 0.0192 (6) | −0.0008 (5) | 0.0119 (5) | −0.0006 (5) |
C2 | 0.0202 (6) | 0.0223 (6) | 0.0221 (6) | 0.0000 (5) | 0.0125 (5) | −0.0011 (5) |
O1 | 0.0275 (6) | 0.0293 (6) | 0.0222 (5) | 0.0058 (4) | 0.0156 (5) | −0.0003 (4) |
O2 | 0.0348 (7) | 0.0578 (9) | 0.0203 (6) | 0.0124 (7) | 0.0155 (5) | 0.0082 (6) |
O3 | 0.0314 (6) | 0.0408 (8) | 0.0308 (6) | 0.0163 (6) | 0.0158 (6) | 0.0046 (6) |
O4 | 0.0314 (6) | 0.0268 (6) | 0.0222 (5) | 0.0057 (5) | 0.0168 (5) | 0.0006 (4) |
OW5 | 0.0248 (6) | 0.0273 (6) | 0.0326 (7) | −0.0037 (5) | 0.0104 (5) | 0.0058 (5) |
OW6 | 0.0395 (8) | 0.0311 (7) | 0.0333 (7) | −0.0043 (6) | 0.0240 (6) | −0.0048 (5) |
Geometric parameters (Å, º) top
Cs—O2i | 3.108 (2) | Co—O4 | 2.0881 (13) |
Cs—O3ii | 3.1391 (15) | Co—O1iii | 2.0927 (14) |
Cs—OW6 | 3.157 (2) | Co—O1 | 2.0927 (14) |
Cs—O1iii | 3.2887 (15) | C1—O2 | 1.242 (2) |
Cs—OW5 | 3.3146 (17) | C1—O1 | 1.265 (2) |
Cs—O1iv | 3.3193 (14) | C1—C2 | 1.554 (2) |
Cs—O2v | 3.3396 (19) | C2—O3 | 1.235 (2) |
Cs—O3v | 3.4503 (17) | C2—O4 | 1.268 (2) |
Cs—O4 | 3.4978 (14) | OW5—H1 | 0.80 (4) |
Co—OW5 | 2.0701 (14) | OW5—H2 | 0.86 (3) |
Co—OW5iii | 2.0701 (14) | OW6—H3 | 0.81 (3) |
Co—O4iii | 2.0881 (13) | OW6—H4 | 0.77 (4) |
| | | |
OW5—Co—OW5iii | 94.59 (9) | O2—C1—O1 | 125.88 (16) |
OW5—Co—O4iii | 171.00 (5) | O2—C1—C2 | 117.82 (15) |
OW5iii—Co—O4iii | 88.29 (6) | O1—C1—C2 | 116.27 (14) |
OW5—Co—O4 | 88.29 (6) | O3—C2—O4 | 125.44 (16) |
OW5iii—Co—O4 | 171.00 (5) | O3—C2—C1 | 119.19 (15) |
O4iii—Co—O4 | 90.15 (8) | O4—C2—C1 | 115.36 (14) |
OW5—Co—O1iii | 92.28 (6) | Co—OW5—H1 | 125 (2) |
OW5iii—Co—O1iii | 94.81 (6) | Cs—OW5—H1 | 107 (2) |
O4iii—Co—O1iii | 78.96 (5) | Co—OW5—H2 | 119 (2) |
O4—Co—O1iii | 93.59 (6) | Cs—OW5—H2 | 106.3 (19) |
OW5—Co—O1 | 94.81 (6) | H1—OW5—H2 | 102 (3) |
OW5iii—Co—O1 | 92.28 (6) | Cs—OW6—H3 | 96 (2) |
O4iii—Co—O1 | 93.59 (6) | Cs—OW6—H4 | 143 (3) |
O4—Co—O1 | 78.96 (5) | H3—OW6—H4 | 101 (3) |
O1iii—Co—O1 | 169.53 (7) | | |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) −x+1/2, y+1/2, −z+1/2; (iii) −x, y, −z+1/2; (iv) x, −y+1, z−1/2; (v) x, −y, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW5—H1···OW6vi | 0.80 (4) | 1.91 (4) | 2.685 (2) | 162 (4) |
OW5—H2···O3i | 0.86 (3) | 1.88 (3) | 2.730 (2) | 172 (3) |
OW6—H3···O2iii | 0.81 (3) | 1.93 (3) | 2.733 (2) | 173 (3) |
OW6—H4···O4vii | 0.77 (4) | 1.99 (4) | 2.752 (2) | 177 (4) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (iii) −x, y, −z+1/2; (vi) −x, −y+1, −z; (vii) −x, −y, −z. |