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Acta Cryst. (2007). E63, m2186-m2187    [ doi:10.1107/S1600536807034708 ]

Pentaaqua(1-vinyl-1H-imidazole-[kappa]N3)cobalt(II) sulfate

G.-Y. Liu, W.-L. Liu, F.-Q. Liu, R.-X. Li and S.-Y. Huang

Abstract top

In the title compound, [Co(C5H6N2)(H2O)5]SO4, each CoII ion is coordinated by one N atom from a 1-vinyl-1H-imidazole ligand and five water molecules in a distorted octahedral geometry. In the crystal structure, the cations and anions are linked by O-H...O hydrogen bonds into two-dimensional layers parallel to the ab plane, with the 1-vinyl-1H-imidazole ligands protruding.

Comment top

In the title compound, (I) (Fig. 1), the local coordination geometry around the Co centre can be described as a distorted octahedron, formed by one N atom from one N-vinylimidazole ligand and five O atoms from five water molecules. The Co—N bond distance is 2.069 (3) Å, compared with a value of 2.097 (2) Å in [Co(viz)4SiF6] {viz is N-vinylimidazole; Driessen et al., 1982}. The Co—O bond distances range from 2.067 (3) to 2.199 (2) Å, compared to the similar Co—O(water) bond distances of 2.087 (3), 2.062 (2) and 2.087 (4) Å in [(pyz)Co2(H2O)10](SO4)2(H2O)2 (pyz is pyrazine; Xie et al., 2004).

In the crystal, the cations and anions are linked by O—H···O hydrogen bonds into two-dimensional layers parallell to ab-plane with the protruding N-vinylimidazole ligands.

Related literature top

In the corresponding binuclear cobalt compound [(pyz)Co2(H2O)10](SO4)2(H2O)2 (Xie et al., 2004), the two CoII ions have a distorted octahedral environment formed by five water molecules and one N atom from pyz (= pyrazine). In [Co(viz)4SiF6] (viz = N-vinylimidazole), the CoII ions also have a distorted octahedral environment (Driessen et al., 1982).

Experimental top

The title compound was prepared by the reaction of N-ethylimidazole (0.48 g, 5 mmol) with CoSO4.7H2O(1.40 g, 5 mmol) by means of hydrothermal synthesis in a stainless-steel reactor with a Teflon liner at 383 K for 24 h. Single crystals suitable for X-ray measurements were obtained by recrystallization from ethanol at room temperature.

Refinement top

H atoms bonded to O atoms were located in a difference map and were refined with bonds restraints O—H=0.85 (3) Å, H···H 1.37 (2) Å, and with Uiso(H) = 0.1. The C-bound H atoms were positioned geometrically (C—H = 0.93 Å) and allowed to ride on their parent atoms with Uiso(H) = 1.2 times Ueq(C).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and local programs.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing 50% probability displacement ellipsoids and the atom-numbering scheme.
Pentaaqua(1-vinyl-1H-imidazole-κN3)cobalt(II) sulfate top
Crystal data top
[Co(C5H6N2)(H2O)5]SO4Z = 2
Mr = 339.19F(000) = 350
Triclinic, P1Dx = 1.735 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.2070 (12) ÅCell parameters from 25 reflections
b = 8.0820 (16) Åθ = 4–14°
c = 13.409 (3) ŵ = 1.52 mm−1
α = 83.42 (3)°T = 293 K
β = 77.67 (3)°Block, pink
γ = 82.67 (3)°0.40 × 0.30 × 0.10 mm
V = 649.1 (2) Å3
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer		2486 independent reflections
Radiation source: fine-focus sealed tube2322 reflections with I > 2σ(I)
graphiteRint = 0.032
thin–slice ω scansθmax = 26.0°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)		h = −7→7
Tmin = 0.581, Tmax = 0.863k = −9→9
2546 measured reflectionsl = 0→16
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0813P)2 + 0.8585P]
where P = (Fo2 + 2Fc2)/3
2486 reflections(Δ/σ)max = 0.001
193 parametersΔρmax = 0.65 e Å−3
15 restraintsΔρmin = −0.46 e Å−3
Crystal data top
[Co(C5H6N2)(H2O)5]SO4γ = 82.67 (3)°
Mr = 339.19V = 649.1 (2) Å3
Triclinic, P1Z = 2
a = 6.2070 (12) ÅMo Kα radiation
b = 8.0820 (16) ŵ = 1.52 mm−1
c = 13.409 (3) ÅT = 293 K
α = 83.42 (3)°0.40 × 0.30 × 0.10 mm
β = 77.67 (3)°
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer		2486 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2004)		2322 reflections with I > 2σ(I)
Tmin = 0.581, Tmax = 0.863Rint = 0.032
2546 measured reflectionsθmax = 26.0°
Refinement top
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.129Δρmax = 0.65 e Å−3
S = 1.06Δρmin = −0.46 e Å−3
2486 reflectionsAbsolute structure: ?
193 parametersFlack parameter: ?
15 restraintsRogers parameter: ?
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
xyzUiso*/Ueq
Co0.43720 (6)0.70331 (5)0.68120 (3)0.02540 (18)
S−0.07835 (12)1.21755 (9)0.65627 (6)0.0268 (2)
O10.3863 (4)0.4501 (3)0.6951 (2)0.0382 (6)
O20.7417 (4)0.6427 (3)0.7345 (2)0.0389 (6)
O30.6202 (4)0.6508 (3)0.5351 (2)0.0405 (6)
O40.5035 (5)0.9498 (3)0.6461 (3)0.0453 (7)
O50.1416 (4)0.7796 (3)0.61441 (19)0.0317 (5)
O6−0.2029 (5)1.0888 (4)0.7207 (3)0.0533 (8)
O7−0.0249 (4)1.3356 (3)0.7205 (2)0.0438 (7)
O80.1284 (4)1.1339 (3)0.5985 (2)0.0455 (7)
O9−0.2087 (5)1.3086 (3)0.5828 (2)0.0454 (7)
N10.2553 (5)0.7268 (4)0.8283 (2)0.0366 (7)
N2−0.0162 (6)0.7876 (5)0.9575 (3)0.0474 (8)
C10.0593 (6)0.8068 (5)0.8561 (3)0.0417 (9)
H1A−0.01930.87000.81050.050*
C20.1479 (10)0.6906 (8)0.9986 (4)0.0736 (17)
H2A0.14660.65701.06740.088*
C30.3118 (9)0.6545 (7)0.9172 (4)0.0680 (15)
H3A0.44480.58930.92150.082*
C4−0.2297 (9)0.8587 (8)1.0087 (4)0.0685 (15)
H4A−0.32430.91710.96850.082*
C5−0.2983 (10)0.8469 (8)1.1060 (4)0.0807 (18)
H5A−0.20790.78931.14840.097*
H5B−0.43870.89591.13420.097*
H5WA0.165 (11)0.741 (7)0.556 (5)0.1*
H4WA0.597 (8)1.002 (7)0.664 (6)0.1*
H2WA0.787 (10)0.540 (5)0.730 (6)0.1*
H5WB0.139 (11)0.886 (5)0.604 (5)0.1*
H2WB0.839 (8)0.699 (6)0.695 (5)0.1*
H4WB0.389 (6)1.018 (6)0.642 (6)0.1*
H1WA0.254 (3)0.427 (8)0.700 (6)0.1*
H1WB0.471 (8)0.378 (7)0.659 (5)0.1*
H3WA0.703 (9)0.559 (4)0.533 (6)0.1*
H3WB0.691 (9)0.723 (6)0.494 (5)0.1*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.0185 (3)0.0206 (3)0.0371 (3)0.00043 (16)−0.00718 (18)−0.00281 (17)
S0.0177 (4)0.0223 (4)0.0407 (5)0.0007 (3)−0.0093 (3)−0.0006 (3)
O10.0260 (12)0.0251 (12)0.0621 (17)−0.0017 (10)−0.0049 (12)−0.0067 (11)
O20.0256 (12)0.0338 (13)0.0601 (17)0.0028 (10)−0.0165 (12)−0.0071 (12)
O30.0371 (14)0.0331 (14)0.0460 (15)0.0013 (11)0.0001 (11)−0.0035 (11)
O40.0359 (14)0.0225 (12)0.083 (2)−0.0034 (10)−0.0257 (14)−0.0012 (13)
O50.0255 (11)0.0267 (12)0.0442 (14)0.0024 (9)−0.0124 (10)−0.0045 (10)
O60.0424 (16)0.0540 (18)0.0659 (19)−0.0204 (14)−0.0153 (14)0.0098 (15)
O70.0356 (14)0.0362 (14)0.0644 (18)0.0008 (11)−0.0208 (13)−0.0100 (13)
O80.0306 (13)0.0355 (14)0.0631 (18)0.0112 (11)−0.0033 (12)−0.0019 (12)
O90.0458 (16)0.0413 (15)0.0507 (16)0.0193 (12)−0.0253 (13)−0.0082 (12)
N10.0316 (15)0.0393 (17)0.0374 (16)0.0030 (13)−0.0070 (13)−0.0042 (13)
N20.0397 (18)0.055 (2)0.0436 (18)−0.0001 (16)−0.0024 (15)−0.0039 (16)
C10.036 (2)0.047 (2)0.042 (2)0.0025 (17)−0.0082 (16)−0.0093 (16)
C20.073 (4)0.092 (4)0.040 (2)0.018 (3)−0.002 (2)0.009 (2)
C30.055 (3)0.083 (4)0.053 (3)0.026 (3)−0.009 (2)0.008 (3)
C40.050 (3)0.091 (4)0.056 (3)0.017 (3)−0.005 (2)−0.010 (3)
C50.063 (3)0.094 (4)0.065 (3)0.018 (3)0.009 (3)0.004 (3)
Geometric parameters (Å, °) top
Co—N12.069 (3)O4—H4WB0.85 (3)
Co—O12.092 (3)O5—H5WA0.85 (3)
Co—O22.141 (3)O5—H5WB0.85 (3)
Co—O32.103 (3)N1—C11.303 (5)
Co—O42.067 (3)N1—C31.361 (6)
Co—O52.199 (2)N2—C11.338 (5)
S—O61.463 (3)N2—C21.376 (6)
S—O71.467 (3)N2—C41.437 (6)
S—O81.476 (3)C1—H1A0.9300
S—O91.479 (3)C2—C31.354 (7)
O1—H1WA0.85 (3)C2—H2A0.9300
O1—H1WB0.85 (3)C3—H3A0.9300
O2—H2WA0.85 (3)C4—C51.279 (7)
O2—H2WB0.86 (3)C4—H4A0.9300
O3—H3WA0.85 (3)C5—H5A0.9300
O3—H3WB0.85 (3)C5—H5B0.9300
O4—H4WA0.85 (3)
O4—Co—N197.60 (13)H3WA—O3—H3WB107 (6)
O4—Co—O1172.04 (12)Co—O4—H4WA130 (5)
N1—Co—O190.19 (12)Co—O4—H4WB114 (4)
O4—Co—O388.68 (13)H4WA—O4—H4WB108 (5)
N1—Co—O3173.68 (11)Co—O5—H5WA108 (5)
O1—Co—O383.56 (11)Co—O5—H5WB104 (5)
O4—Co—O290.23 (11)H5WA—O5—H5WB107 (6)
N1—Co—O292.21 (12)C1—N1—C3105.0 (4)
O1—Co—O291.12 (11)C1—N1—Co128.0 (3)
O3—Co—O286.96 (11)C3—N1—Co126.9 (3)
O4—Co—O585.84 (10)C1—N2—C2106.7 (4)
N1—Co—O591.87 (11)C1—N2—C4124.2 (4)
O1—Co—O592.29 (10)C2—N2—C4129.1 (4)
O3—Co—O589.36 (11)N1—C1—N2112.4 (4)
O2—Co—O5174.67 (10)N1—C1—H1A123.8
O6—S—O7109.97 (19)N2—C1—H1A123.8
O6—S—O8108.12 (19)C3—C2—N2105.1 (4)
O7—S—O8109.66 (17)C3—C2—H2A127.4
O6—S—O9110.33 (18)N2—C2—H2A127.4
O7—S—O9109.81 (16)C2—C3—N1110.7 (4)
O8—S—O9108.92 (17)C2—C3—H3A124.6
Co—O1—H1WA117 (5)N1—C3—H3A124.6
Co—O1—H1WB123 (5)C5—C4—N2124.4 (5)
H1WA—O1—H1WB107 (6)C5—C4—H4A117.8
Co—O2—H2WA110 (5)N2—C4—H4A117.8
Co—O2—H2WB108 (5)C4—C5—H5A120.0
H2WA—O2—H2WB107 (6)C4—C5—H5B120.0
Co—O3—H3WA115 (5)H5A—C5—H5B120.0
Co—O3—H3WB123 (5)
O4—Co—N1—C168.8 (4)C2—N2—C1—N11.7 (6)
O1—Co—N1—C1−109.5 (4)C4—N2—C1—N1−178.5 (4)
O2—Co—N1—C1159.3 (3)C1—N2—C2—C3−1.3 (7)
O5—Co—N1—C1−17.2 (3)C4—N2—C2—C3178.9 (5)
O4—Co—N1—C3−114.5 (4)N2—C2—C3—N10.6 (7)
O1—Co—N1—C367.1 (4)C1—N1—C3—C20.4 (7)
O2—Co—N1—C3−24.0 (4)Co—N1—C3—C2−176.8 (4)
O5—Co—N1—C3159.4 (4)C1—N2—C4—C5−176.7 (6)
C3—N1—C1—N2−1.3 (5)C2—N2—C4—C53.1 (10)
Co—N1—C1—N2175.9 (3)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O5—H5WA···O9i0.85 (3)1.90 (7)2.750 (4)171 (6)
O4—H4WA···O6ii0.85 (3)1.83 (4)2.673 (5)171 (6)
O2—H2WA···O7iii0.85 (3)1.90 (5)2.714 (4)161 (5)
O5—H5WB···O80.85 (3)1.99 (4)2.839 (3)173 (6)
O2—H2WB···O5ii0.85 (3)2.10 (5)2.926 (4)163 (6)
O4—H4WB···O80.85 (3)1.93 (5)2.752 (4)162 (7)
O1—H1WA···O7iv0.85 (3)1.92 (4)2.765 (4)169 (6)
O1—H1WB···O9iii0.85 (3)2.07 (5)2.818 (4)146 (6)
O3—H3WB···O8v0.85 (3)1.88 (5)2.730 (6)174 (5)
O3—H3WA···O9iii0.85 (3)2.10 (5)2.885 (4)154 (5)
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) x+1, y−1, z; (iv) x, y−1, z; (v) −x+1, −y+2, −z+1.
Table 1
Selected geometric parameters (Å) top
Co—N12.069 (3)Co—O32.103 (3)
Co—O12.092 (3)Co—O42.067 (3)
Co—O22.141 (3)Co—O52.199 (2)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O5—H5WA···O9i0.85 (3)1.90 (7)2.750 (4)171 (6)
O4—H4WA···O6ii0.85 (3)1.83 (4)2.673 (5)171 (6)
O2—H2WA···O7iii0.85 (3)1.90 (5)2.714 (4)161 (5)
O5—H5WB···O80.85 (3)1.99 (4)2.839 (3)173 (6)
O2—H2WB···O5ii0.85 (3)2.10 (5)2.926 (4)163 (6)
O4—H4WB···O80.85 (3)1.93 (5)2.752 (4)162 (7)
O1—H1WA···O7iv0.85 (3)1.92 (4)2.765 (4)169 (6)
O1—H1WB···O9iii0.85 (3)2.07 (5)2.818 (4)146 (6)
O3—H3WB···O8v0.85 (3)1.88 (5)2.730 (6)174 (5)
O3—H3WA···O9iii0.85 (3)2.10 (5)2.885 (4)154 (5)
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) x+1, y−1, z; (iv) x, y−1, z; (v) −x+1, −y+2, −z+1.
Acknowledgements top

This work was supported by the National Natural Science Foundation of China (grant No. 20601015).

references
References top

Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Driessen, R. A. J., Hulsbergen, F. B., Vermin, W. J. & Reedijk, J. (1982). Inorg. Chem. 21, 3594–3597.

Sheldrick, G. M. (2001). SHELXTL. Version 5.0. Bruker AXS Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.

Xie, L., Wei, Y., Wang, Y., Hou, H., Fan, Y. & Zhu, Y. (2004). J. Mol. Struct. 692, 201–207.