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The structure of the title compound, catena-poly[[[diaquacobalt(II)]-μ-oxydiacetato-κ4O,O′,O′′:O′′′)cobalt(II)] monohydrate], {[Co(C4H4O5)(H2O)2]·H2O}n, (I), was first determined and reported by Hatfield et al. [Proc. Indian Acad. Sci. Chem. Sci. (1987), 98, 23–31]. We present here a redetermination, with appreciably improved accuracy and successful location of H atoms. In the crystal structure, oxydiacetate plays the role of both chelating and bridging ligand, resulting in he formation of polymeric chains of complex molecules along the crystallographic b axis. Water molecules occupy the apical positions, thus completing the coordination octahedron of the CoII atom. The polymeric chains are interlinked via intermolecular hydrogen bonding between carboxylate and water molecules, forming the three-dimensional supramolecular structure.
Supporting information
CCDC reference: 200725
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.003 Å
- R factor = 0.022
- wR factor = 0.064
- Data-to-parameter ratio = 13.8
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Data collection: MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1985); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997).
Crystal data top
[Co(C4H4O5)(H2O)2]·H2O | F(000) = 500 |
Mr = 245.05 | Dx = 1.977 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
a = 7.1220 (12) Å | Cell parameters from 20 reflections |
b = 10.3935 (7) Å | θ = 5.0–10.3° |
c = 11.1259 (10) Å | µ = 2.10 mm−1 |
β = 91.529 (10)° | T = 298 K |
V = 823.27 (17) Å3 | Prism, red |
Z = 4 | 0.40 × 0.32 × 0.32 mm |
Data collection top
Rigaku AFC-7S diffractometer | 1458 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.019 |
Graphite monochromator | θmax = 26.0°, θmin = 2.7° |
ω/2θ scans | h = 0→8 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→12 |
Tmin = 0.451, Tmax = 0.511 | l = −13→13 |
1757 measured reflections | 3 standard reflections every 150 reflections |
1624 independent reflections | intensity decay: 0.7% |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + 0.4775P] where P = (Fo2 + 2Fc2)/3 |
1624 reflections | (Δ/σ)max = 0.001 |
118 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.33 e Å−3 |
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 | |
Co | 0.42776 (4) | 0.39268 (2) | 0.19689 (2) | 0.02063 (11) | |
O1 | 0.20534 (19) | 0.28219 (12) | 0.26287 (13) | 0.0241 (3) | |
O2 | 0.0990 (2) | 0.08756 (13) | 0.30293 (13) | 0.0263 (3) | |
O3 | 0.5174 (2) | 0.20294 (14) | 0.18300 (17) | 0.0409 (4) | |
O4 | 0.6875 (2) | 0.40311 (12) | 0.11159 (14) | 0.0263 (3) | |
O5 | 0.9161 (2) | 0.29292 (15) | 0.02577 (14) | 0.0316 (3) | |
O6 | 0.2728 (2) | 0.38931 (13) | 0.03141 (13) | 0.0276 (3) | |
O7 | 0.5339 (2) | 0.40441 (15) | 0.37293 (15) | 0.0342 (4) | |
O8 | 0.8955 (2) | 0.33566 (17) | 0.40516 (16) | 0.0405 (4) | |
C1 | 0.2223 (3) | 0.16117 (18) | 0.26487 (17) | 0.0207 (4) | |
C2 | 0.3996 (3) | 0.10239 (18) | 0.2181 (2) | 0.0286 (5) | |
H2A | 0.4615 | 0.0512 | 0.2804 | 0.034* | |
H2B | 0.3702 | 0.0469 | 0.1501 | 0.034* | |
C3 | 0.6921 (3) | 0.17443 (19) | 0.1315 (2) | 0.0268 (4) | |
H3A | 0.6750 | 0.1136 | 0.0660 | 0.032* | |
H3B | 0.7771 | 0.1369 | 0.1914 | 0.032* | |
C4 | 0.7718 (3) | 0.29967 (19) | 0.08539 (17) | 0.0223 (4) | |
H61 | 0.2847 | 0.4578 | −0.0147 | 0.080* | |
H62 | 0.1588 | 0.3667 | 0.0392 | 0.080* | |
H71 | 0.4852 | 0.3395 | 0.4235 | 0.080* | |
H72 | 0.6524 | 0.3906 | 0.3648 | 0.080* | |
H81 | 0.8712 | 0.2601 | 0.4395 | 0.080* | |
H82 | 0.9911 | 0.3221 | 0.3577 | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.02085 (16) | 0.01253 (15) | 0.02889 (17) | 0.00075 (9) | 0.00784 (11) | 0.00096 (9) |
O1 | 0.0251 (7) | 0.0135 (6) | 0.0340 (8) | −0.0004 (5) | 0.0083 (6) | 0.0024 (6) |
O2 | 0.0259 (7) | 0.0159 (7) | 0.0374 (9) | −0.0051 (6) | 0.0079 (6) | 0.0018 (6) |
O3 | 0.0331 (8) | 0.0140 (7) | 0.0772 (12) | 0.0005 (6) | 0.0335 (8) | 0.0020 (7) |
O4 | 0.0273 (8) | 0.0177 (7) | 0.0343 (8) | 0.0008 (5) | 0.0100 (6) | 0.0029 (6) |
O5 | 0.0214 (7) | 0.0352 (8) | 0.0387 (8) | −0.0023 (6) | 0.0109 (6) | −0.0056 (7) |
O6 | 0.0265 (7) | 0.0247 (8) | 0.0317 (8) | −0.0055 (6) | 0.0017 (6) | 0.0063 (6) |
O7 | 0.0343 (9) | 0.0346 (9) | 0.0337 (8) | −0.0038 (7) | 0.0025 (7) | 0.0056 (6) |
O8 | 0.0353 (9) | 0.0370 (9) | 0.0498 (10) | 0.0034 (7) | 0.0122 (8) | 0.0075 (8) |
C1 | 0.0229 (9) | 0.0180 (9) | 0.0213 (9) | −0.0028 (7) | 0.0002 (7) | 0.0007 (7) |
C2 | 0.0300 (11) | 0.0150 (10) | 0.0412 (12) | −0.0016 (8) | 0.0113 (9) | 0.0032 (8) |
C3 | 0.0215 (10) | 0.0197 (9) | 0.0397 (11) | 0.0053 (8) | 0.0082 (8) | −0.0004 (9) |
C4 | 0.0180 (9) | 0.0254 (10) | 0.0235 (9) | −0.0011 (8) | 0.0003 (7) | −0.0009 (8) |
Geometric parameters (Å, º) top
Co—O1 | 2.1045 (14) | O6—H61 | 0.883 |
Co—O2i | 2.0345 (14) | O6—H62 | 0.852 |
Co—O3 | 2.0798 (15) | O7—H71 | 0.950 |
Co—O4 | 2.1041 (15) | O7—H72 | 0.863 |
Co—O6 | 2.1213 (15) | O8—H81 | 0.892 |
Co—O7 | 2.0841 (17) | O8—H82 | 0.884 |
O1—C1 | 1.264 (2) | C1—C2 | 1.508 (3) |
O2—C1 | 1.247 (2) | C2—H2A | 0.970 |
O3—C2 | 1.402 (2) | C2—H2B | 0.970 |
O3—C3 | 1.415 (2) | C3—C4 | 1.515 (3) |
O4—C4 | 1.269 (2) | C3—H3A | 0.970 |
O5—C4 | 1.240 (2) | C3—H3B | 0.970 |
| | | |
O2i—Co—O3 | 166.65 (6) | H61—O6—H62 | 112.81 |
O2i—Co—O7 | 88.42 (6) | Co—O7—H71 | 112.70 |
O3—Co—O7 | 91.20 (7) | Co—O7—H72 | 102.89 |
O2i—Co—O4 | 91.86 (6) | H71—O7—H72 | 108.52 |
O3—Co—O4 | 74.94 (6) | H81—O8—H82 | 106.06 |
O7—Co—O4 | 96.87 (6) | O2—C1—O1 | 123.29 (19) |
O2i—Co—O1 | 118.14 (6) | O2—C1—C2 | 118.19 (17) |
O3—Co—O1 | 75.16 (6) | O1—C1—C2 | 118.52 (17) |
O7—Co—O1 | 87.81 (6) | O3—C2—C1 | 107.87 (16) |
O4—Co—O1 | 149.81 (5) | O3—C2—H2A | 110.1 |
O2i—Co—O6 | 88.32 (6) | C1—C2—H2A | 110.1 |
O3—Co—O6 | 94.21 (7) | O3—C2—H2B | 110.1 |
O7—Co—O6 | 169.69 (6) | C1—C2—H2B | 110.1 |
O4—Co—O6 | 93.01 (6) | H2A—C2—H2B | 108.4 |
O1—Co—O6 | 85.11 (6) | O3—C3—C4 | 107.37 (16) |
C1—O1—Co | 118.49 (13) | O3—C3—H3A | 110.2 |
C1—O2—Coii | 132.67 (14) | C4—C3—H3A | 110.2 |
C2—O3—C3 | 119.72 (16) | O3—C3—H3B | 110.2 |
C2—O3—Co | 119.93 (13) | C4—C3—H3B | 110.2 |
C3—O3—Co | 120.24 (12) | H3A—C3—H3B | 108.5 |
C4—O4—Co | 119.14 (12) | O5—C4—O4 | 125.08 (18) |
Co—O6—H61 | 115.82 | O5—C4—C3 | 117.12 (17) |
Co—O6—H62 | 113.04 | O4—C4—C3 | 117.79 (16) |
| | | |
O2i—Co—O1—C1 | −178.86 (13) | O7—Co—O4—C4 | 92.98 (15) |
O3—Co—O1—C1 | 0.00 (14) | O1—Co—O4—C4 | −4.5 (2) |
O7—Co—O1—C1 | −91.82 (14) | O6—Co—O4—C4 | −89.97 (15) |
O4—Co—O1—C1 | 8.1 (2) | Coii—O2—C1—O1 | 173.05 (13) |
O6—Co—O1—C1 | 95.67 (14) | Coii—O2—C1—C2 | −6.5 (3) |
O2i—Co—O3—C2 | 176.6 (2) | Co—O1—C1—O2 | 179.55 (14) |
O7—Co—O3—C2 | 88.42 (18) | Co—O1—C1—C2 | −0.9 (2) |
O4—Co—O3—C2 | −174.79 (19) | C3—O3—C2—C1 | −177.86 (18) |
O1—Co—O3—C2 | 1.01 (17) | Co—O3—C2—C1 | −1.6 (2) |
O6—Co—O3—C2 | −82.80 (18) | O2—C1—C2—O3 | −178.82 (18) |
O2i—Co—O3—C3 | −7.2 (4) | O1—C1—C2—O3 | 1.6 (3) |
O7—Co—O3—C3 | −95.37 (17) | C2—O3—C3—C4 | 171.17 (19) |
O4—Co—O3—C3 | 1.41 (16) | Co—O3—C3—C4 | −5.0 (2) |
O1—Co—O3—C3 | 177.21 (18) | Co—O4—C4—O5 | 173.12 (15) |
O6—Co—O3—C3 | 93.40 (17) | Co—O4—C4—C3 | −7.7 (2) |
O2i—Co—O4—C4 | −178.39 (15) | O3—C3—C4—O5 | −172.72 (18) |
O3—Co—O4—C4 | 3.59 (15) | O3—C3—C4—O4 | 8.0 (3) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x+1/2, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H61···O4iii | 0.88 | 1.82 | 2.700 (2) | 179 |
O6—H62···O5iv | 0.85 | 1.89 | 2.730 (2) | 167 |
O7—H71···O5v | 0.95 | 1.86 | 2.807 (2) | 174 |
O7—H72···O8 | 0.86 | 1.87 | 2.687 (2) | 158 |
O8—H81···O6vi | 0.89 | 2.00 | 2.876 (2) | 168 |
O8—H82···O1vii | 0.88 | 1.92 | 2.806 (2) | 176 |
Symmetry codes: (iii) −x+1, −y+1, −z; (iv) x−1, y, z; (v) x−1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x+1, y, z. |
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