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Acta Crystallogr Sect E Struct Rep Online. 2008 March 1; 64(Pt 3): m446.
Published online 2008 February 6. doi:  10.1107/S1600536808003140
PMCID: PMC2960768

Tetra­aqua­bis(4-formyl­benzoato-κO)cobalt(II) tetra­hydrate

Abstract

The CoII atom in the title compound, [Co(C8H5O3)2(H2O)4]·4H2O, which exists in an all-trans octa­hedral coordination geometry, lies on a center of inversion. The coordinated and uncoordinated water mol­ecules engage in extensive hydrogen-bonding inter­actions, forming a three-dimensional hydrogen-bonded network.

Related literature

Hexaaqua­cobalt(II) bis­(4-formyl­benzoate) dihydrate was isolated from the reaction of cobalt(II) acetate and 4-formyl­benzoic acid in the presence of sodium hydroxide; see Deng et al. (2006b [triangle]). The reaction with pyridine in place of sodium hydroxide yielded the formylbenzoate-coordinated title compound. This is isostructural with the nickel analog; see Deng et al. (2006a [triangle]).

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Object name is e-64-0m446-scheme1.jpg

Experimental

Crystal data

  • [Co(C8H5O3)2(H2O)4]·4H2O
  • M r = 501.30
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m446-efi1.jpg
  • a = 7.1472 (3) Å
  • b = 7.4759 (4) Å
  • c = 11.5720 (6) Å
  • α = 77.114 (2)°
  • β = 77.905 (2)°
  • γ = 63.839 (1)°
  • V = 536.61 (5) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 0.87 mm−1
  • T = 295 (2) K
  • 0.30 × 0.26 × 0.22 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.666, T max = 0.832
  • 5294 measured reflections
  • 2426 independent reflections
  • 2270 reflections with I > 2σ(I)
  • R int = 0.015

Refinement

  • R[F 2 > 2σ(F 2)] = 0.027
  • wR(F 2) = 0.080
  • S = 1.03
  • 2426 reflections
  • 174 parameters
  • 12 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.35 e Å−3
  • Δρmin = −0.27 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 [triangle]); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 [triangle]); method used to solve structure: atomic coordinates taken from the isostructural nickel analog; program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2008 [triangle]).

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808003140/bt2668sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808003140/bt2668Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We thank the Heilongjiang Province Natural Science Foundation (No. B200501), the Scientific Fund for Remarkable Teachers of Heilongjiang Province (No. 1054G036), Heilongjiang University and the University of Malaya for supporting this work.

supplementary crystallographic information

Comment

Hexaaquacobalt(II) bis(4-formylbenzoate) dihydrate was isolated from the reaction of cobalt(II) acetate and 4-formylbenzoic acid in the presence of sodium hydroxide (Deng et al., 2006b). The reaction with pyridine in place of sodium hydroxide yielded the formybenzoate-coordinated title compound.

Experimental

Cobalt diacetate dihydrate (2.32 g, 10 mmol) was added to an aqueous solution of 4-formylbenzoic acid (3.0 g, 20 mmol) that was earlier been treated with 1 ml pyridine to give a pH of 6. The solution was allowed to evaporate at room temperature; pink prismatic crystals separated from the filtered solution after several days. C&H elemental analysis. Calc. for C16H26O14Co: C 38.33, H 5.23%. Found: C 38.36, H 5.24%.

Refinement

The carbon-bound H atoms were placed in calculated positions [C–H 0.93 Å and Uiso(H) 1.2Ueq(C)], and were included in the refinement in the riding-model approximation. The water H-atoms were located in a difference Fourier map, and were refined with distance restraints of O–H 0.85±0.01 Å and H···H 1.39±0.01 Å; their displacement parameters were freely refined.

Figures

Fig. 1.
Anisotropic displacement parameter plot of (I). Displacement ellipsoids are drawn at the 50% probability level and H atoms as spheres of arbitrary radius.

Crystal data

[Co(C8H5O3)2(H2O)4]·4H2OZ = 1
Mr = 501.30F000 = 261
Triclinic, P1Dx = 1.551 Mg m3
Hall symbol: -P 1Mo Kα radiation λ = 0.71073 Å
a = 7.1472 (3) ÅCell parameters from 4983 reflections
b = 7.4759 (4) Åθ = 3.1–27.5º
c = 11.5720 (6) ŵ = 0.87 mm1
α = 77.114 (2)ºT = 295 (2) K
β = 77.905 (2)ºPrism, pink
γ = 63.839 (1)º0.30 × 0.26 × 0.22 mm
V = 536.61 (5) Å3

Data collection

Rigaku R-AXIS RAPID diffractometer2426 independent reflections
Radiation source: fine-focus sealed tube2270 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.016
Detector resolution: 10.000 pixels mm-1θmax = 27.5º
T = 295(2) Kθmin = 3.1º
ω scansh = −9→9
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)k = −9→9
Tmin = 0.666, Tmax = 0.832l = −15→14
5294 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.080  w = 1/[σ2(Fo2) + (0.0481P)2 + 0.1724P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
2426 reflectionsΔρmax = 0.36 e Å3
174 parametersΔρmin = −0.27 e Å3
12 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Co10.50000.50000.50000.02806 (11)
O10.45499 (18)0.39037 (19)0.36093 (10)0.0359 (3)
O20.0927 (2)0.2392 (2)−0.11561 (12)0.0492 (3)
O30.76754 (19)0.3176 (2)0.25021 (12)0.0460 (3)
O1W0.19780 (18)0.52308 (19)0.58061 (11)0.0381 (3)
H1W10.192 (3)0.570 (3)0.6429 (14)0.057 (7)*
H1W20.091 (3)0.602 (3)0.5461 (19)0.071 (8)*
O2W0.3680 (2)0.79054 (18)0.40003 (12)0.0408 (3)
H2W10.329 (4)0.893 (3)0.434 (2)0.067 (8)*
H2W20.271 (3)0.807 (4)0.362 (2)0.069 (8)*
O3W0.2016 (3)1.1588 (2)0.48800 (14)0.0544 (4)
H3W10.152 (3)1.158 (3)0.5610 (10)0.051 (6)*
H3W20.282 (4)1.218 (4)0.470 (2)0.096 (11)*
O4W−0.0173 (2)1.1045 (2)0.71542 (13)0.0534 (4)
H4W10.001 (4)1.159 (3)0.767 (2)0.076 (8)*
H4W20.048 (5)0.9775 (14)0.731 (3)0.096 (11)*
C10.2664 (3)0.2311 (2)−0.11986 (15)0.0384 (4)
H10.35630.2070−0.19100.046*
C20.3455 (2)0.2570 (2)−0.01950 (13)0.0311 (3)
C30.2157 (2)0.3005 (3)0.08787 (15)0.0351 (3)
H30.07790.31390.09670.042*
C40.2921 (2)0.3237 (3)0.18106 (14)0.0344 (3)
H40.20520.35370.25250.041*
C50.4989 (2)0.3026 (2)0.16869 (13)0.0279 (3)
C60.6284 (2)0.2574 (2)0.06149 (14)0.0321 (3)
H60.76680.24200.05280.039*
C70.5514 (3)0.2353 (2)−0.03205 (14)0.0334 (3)
H70.63800.2059−0.10370.040*
C80.5803 (2)0.3383 (2)0.26758 (13)0.0297 (3)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Co10.02531 (16)0.03279 (16)0.02910 (16)−0.01180 (12)−0.00411 (10)−0.01027 (11)
O10.0324 (5)0.0492 (6)0.0324 (6)−0.0187 (5)−0.0014 (4)−0.0167 (5)
O20.0491 (8)0.0561 (8)0.0500 (8)−0.0196 (6)−0.0160 (6)−0.0179 (6)
O30.0315 (6)0.0714 (9)0.0433 (7)−0.0231 (6)−0.0004 (5)−0.0248 (6)
O1W0.0298 (6)0.0469 (7)0.0409 (7)−0.0161 (5)−0.0034 (5)−0.0134 (5)
O2W0.0431 (7)0.0362 (6)0.0432 (7)−0.0124 (5)−0.0143 (5)−0.0063 (5)
O3W0.0666 (9)0.0547 (8)0.0556 (9)−0.0350 (8)−0.0125 (7)−0.0084 (7)
O4W0.0528 (8)0.0562 (9)0.0547 (9)−0.0140 (7)−0.0207 (6)−0.0204 (7)
C10.0468 (9)0.0372 (8)0.0326 (8)−0.0149 (7)−0.0078 (7)−0.0104 (6)
C20.0378 (8)0.0278 (7)0.0290 (7)−0.0132 (6)−0.0063 (6)−0.0055 (5)
C30.0300 (7)0.0459 (9)0.0341 (8)−0.0184 (7)−0.0029 (6)−0.0102 (6)
C40.0325 (8)0.0448 (8)0.0276 (7)−0.0171 (7)0.0008 (6)−0.0106 (6)
C50.0300 (7)0.0268 (6)0.0278 (7)−0.0114 (6)−0.0048 (5)−0.0056 (5)
C60.0292 (7)0.0348 (7)0.0331 (8)−0.0137 (6)−0.0007 (6)−0.0084 (6)
C70.0379 (8)0.0340 (7)0.0273 (7)−0.0143 (6)0.0017 (6)−0.0093 (6)
C80.0295 (7)0.0297 (7)0.0305 (7)−0.0110 (6)−0.0050 (6)−0.0071 (5)

Geometric parameters (Å, °)

Co1—O12.098 (1)O4W—H4W10.847 (10)
Co1—O1i2.098 (1)O4W—H4W20.849 (10)
Co1—O1Wi2.113 (1)C1—C21.475 (2)
Co1—O1w2.113 (1)C1—H10.9300
Co1—O2w2.116 (1)C2—C71.388 (2)
Co1—O2Wi2.116 (1)C2—C31.393 (2)
O1—C81.2630 (18)C3—C41.381 (2)
O2—C11.207 (2)C3—H30.9300
O3—C81.2543 (19)C4—C51.395 (2)
O1W—H1W10.858 (9)C4—H40.9300
O1W—H1W20.844 (9)C5—C61.393 (2)
O2W—H2W10.849 (9)C5—C81.507 (2)
O2W—H2W20.848 (9)C6—C71.382 (2)
O3W—H3W10.845 (9)C6—H60.9300
O3W—H3W20.838 (10)C7—H70.9300
O1—Co1—O1i180.0O2—C1—C2124.23 (16)
O1—Co1—O1Wi93.12 (5)O2—C1—H1117.9
O1i—Co1—O1Wi86.88 (5)C2—C1—H1117.9
O1—Co1—O1W86.88 (5)C7—C2—C3119.95 (14)
O1i—Co1—O1W93.12 (5)C7—C2—C1119.56 (14)
O1Wi—Co1—O1W180.0C3—C2—C1120.49 (14)
O1—Co1—O2W86.82 (5)C4—C3—C2119.79 (14)
O1i—Co1—O2W93.18 (5)C4—C3—H3120.1
O1Wi—Co1—O2W89.23 (5)C2—C3—H3120.1
O1W—Co1—O2W90.77 (5)C3—C4—C5120.42 (14)
O1—Co1—O2Wi93.18 (5)C3—C4—H4119.8
O1i—Co1—O2Wi86.82 (5)C5—C4—H4119.8
O1Wi—Co1—O2Wi90.77 (5)C6—C5—C4119.52 (14)
O1W—Co1—O2Wi89.23 (5)C6—C5—C8119.64 (13)
O2W—Co1—O2Wi180.0C4—C5—C8120.77 (13)
C8—O1—Co1127.37 (10)C7—C6—C5120.04 (14)
Co1—O1W—H1W197.7 (16)C7—C6—H6120.0
Co1—O1W—H1W2120.0 (19)C5—C6—H6120.0
H1W1—O1W—H1W2108.3 (14)C6—C7—C2120.27 (14)
Co1—O2W—H2W1118.7 (17)C6—C7—H7119.9
Co1—O2W—H2W2113.8 (17)C2—C7—H7119.9
H2W1—O2W—H2W2108.9 (15)O3—C8—O1124.60 (14)
H3W1—O3W—H3W2110.9 (15)O3—C8—C5117.39 (13)
H4W1—O4W—H4W2109.2 (15)O1—C8—C5118.00 (13)
O1i—Co1—O1—C80(100)C4—C5—C6—C70.5 (2)
O1Wi—Co1—O1—C8−0.75 (13)C8—C5—C6—C7−176.45 (13)
O1W—Co1—O1—C8179.25 (13)C5—C6—C7—C2−0.4 (2)
O2W—Co1—O1—C888.31 (13)C3—C2—C7—C6−0.2 (2)
O2Wi—Co1—O1—C8−91.69 (13)C1—C2—C7—C6−179.45 (14)
O2—C1—C2—C7176.99 (16)Co1—O1—C8—O310.4 (2)
O2—C1—C2—C3−2.3 (3)Co1—O1—C8—C5−168.27 (9)
C7—C2—C3—C40.6 (2)C6—C5—C8—O3−2.7 (2)
C1—C2—C3—C4179.83 (15)C4—C5—C8—O3−179.67 (15)
C2—C3—C4—C5−0.4 (2)C6—C5—C8—O1176.00 (14)
C3—C4—C5—C6−0.1 (2)C4—C5—C8—O1−0.9 (2)
C3—C4—C5—C8176.80 (15)

Symmetry codes: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O3i0.86 (1)1.77 (1)2.611 (2)166 (2)
O1W—H1W2···O3Wii0.84 (1)2.11 (1)2.925 (2)161 (2)
O2W—H2W1···O3W0.85 (1)1.97 (1)2.808 (2)168 (2)
O2W—H2W2···O4Wii0.85 (1)1.97 (1)2.808 (2)169 (2)
O3W—H3W1···O4W0.85 (1)2.00 (1)2.810 (2)159 (2)
O3W—H3W2···O1iii0.84 (1)2.19 (1)2.992 (2)159 (2)
O4W—H4W1···O2iv0.85 (1)1.93 (1)2.771 (2)169 (3)
O4W—H4W2···O3i0.85 (1)2.00 (1)2.841 (2)172 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+2, −z+1; (iii) x, y+1, z; (iv) x, y+1, z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT2668).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Deng, Z.-P., Gao, S. & Ng, S. W. (2006a). Acta Cryst. E62, m2904–m2905.
  • Deng, Z.-P., Gao, S. & Ng, S. W. (2006b). Acta Cryst. E62, m3423–m3424.
  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Rigaku (1998). RAPID-AUTO Rigaku Corporation, Tokyo, Japan.
  • Rigaku/MSC (2002). CrystalStructure Rigaku/MSC, The Woodlands, Texas, USA.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2008). publCIF In preparation.

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