Penta­aqua­(1-vinyl-1H-imidazole-κN³)cobalt(II) sulfate

In the title compound, [Co(C₅H₆N₂)(H₂O)₅]SO₄, each Co^II 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.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.041
• wR factor = 0.129
• Data-to-parameter ratio = 12.9

checkCIF/PLATON results

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Alert level C
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal  (x 10000)       3000 Deg.
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for          S
PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...          8
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         10
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              O4 S

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT794_ALERT_5_G Check Predicted Bond Valency for Co          (2)       1.90
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         15

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   4 ALERT level G = General alerts; check

   3 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
   1 ALERT type 5 Informative message, check

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S1. Comment

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

In the corresponding binuclear cobalt compound [(pyz)Co₂(H₂O)₁₀](SO₄)₂(H₂O)₂ (Xie et al., 2004), the two Co^II 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 Co^II ions also have a distorted octahedral environment (Driessen et al., 1982).

S2. Experimental

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.

S3. Refinement

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 U_iso(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 U_iso(H) = 1.2 times U_eq(C).

Computing details

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

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

Crystal data

[Co(C5H6N2)(H2O)5]SO4	Z = 2
Mr = 339.19	F(000) = 350
Triclinic, P1	Dx = 1.735 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.2070 (12) Å	Cell parameters from 25 reflections
b = 8.0820 (16) Å	θ = 4–14°
c = 13.409 (3) Å	µ = 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) Å^3

Data collection

Bruker SMART 1K CCD area-detector diffractometer	2486 independent reflections
Radiation source: fine-focus sealed tube	2322 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
thin–slice ω scans	θmax = 26.0°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −7→7
Tmin = 0.581, Tmax = 0.863	k = −9→9
2546 measured reflections	l = 0→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.129	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0813P)^2 + 0.8585P] where P = (Fo^2 + 2Fc^2)/3
2486 reflections	(Δ/σ)max = 0.001
193 parameters	Δρmax = 0.65 e Å^−3
15 restraints	Δρmin = −0.46 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Co	0.43720 (6)	0.70331 (5)	0.68120 (3)	0.02540 (18)
S	−0.07835 (12)	1.21755 (9)	0.65627 (6)	0.0268 (2)
O1	0.3863 (4)	0.4501 (3)	0.6951 (2)	0.0382 (6)
O2	0.7417 (4)	0.6427 (3)	0.7345 (2)	0.0389 (6)
O3	0.6202 (4)	0.6508 (3)	0.5351 (2)	0.0405 (6)
O4	0.5035 (5)	0.9498 (3)	0.6461 (3)	0.0453 (7)
O5	0.1416 (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)
O8	0.1284 (4)	1.1339 (3)	0.5985 (2)	0.0455 (7)
O9	−0.2087 (5)	1.3086 (3)	0.5828 (2)	0.0454 (7)
N1	0.2553 (5)	0.7268 (4)	0.8283 (2)	0.0366 (7)
N2	−0.0162 (6)	0.7876 (5)	0.9575 (3)	0.0474 (8)
C1	0.0593 (6)	0.8068 (5)	0.8561 (3)	0.0417 (9)
H1A	−0.0193	0.8700	0.8105	0.050*
C2	0.1479 (10)	0.6906 (8)	0.9986 (4)	0.0736 (17)
H2A	0.1466	0.6570	1.0674	0.088*
C3	0.3118 (9)	0.6545 (7)	0.9172 (4)	0.0680 (15)
H3A	0.4448	0.5893	0.9215	0.082*
C4	−0.2297 (9)	0.8587 (8)	1.0087 (4)	0.0685 (15)
H4A	−0.3243	0.9171	0.9685	0.082*
C5	−0.2983 (10)	0.8469 (8)	1.1060 (4)	0.0807 (18)
H5A	−0.2079	0.7893	1.1484	0.097*
H5B	−0.4387	0.8959	1.1342	0.097*
H5WA	0.165 (11)	0.741 (7)	0.556 (5)	0.1*
H4WA	0.597 (8)	1.002 (7)	0.664 (6)	0.1*
H2WA	0.787 (10)	0.540 (5)	0.730 (6)	0.1*
H5WB	0.139 (11)	0.886 (5)	0.604 (5)	0.1*
H2WB	0.839 (8)	0.699 (6)	0.695 (5)	0.1*
H4WB	0.389 (6)	1.018 (6)	0.642 (6)	0.1*
H1WA	0.254 (3)	0.427 (8)	0.700 (6)	0.1*
H1WB	0.471 (8)	0.378 (7)	0.659 (5)	0.1*
H3WA	0.703 (9)	0.559 (4)	0.533 (6)	0.1*
H3WB	0.691 (9)	0.723 (6)	0.494 (5)	0.1*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co	0.0185 (3)	0.0206 (3)	0.0371 (3)	0.00043 (16)	−0.00718 (18)	−0.00281 (17)
S	0.0177 (4)	0.0223 (4)	0.0407 (5)	0.0007 (3)	−0.0093 (3)	−0.0006 (3)
O1	0.0260 (12)	0.0251 (12)	0.0621 (17)	−0.0017 (10)	−0.0049 (12)	−0.0067 (11)
O2	0.0256 (12)	0.0338 (13)	0.0601 (17)	0.0028 (10)	−0.0165 (12)	−0.0071 (12)
O3	0.0371 (14)	0.0331 (14)	0.0460 (15)	0.0013 (11)	0.0001 (11)	−0.0035 (11)
O4	0.0359 (14)	0.0225 (12)	0.083 (2)	−0.0034 (10)	−0.0257 (14)	−0.0012 (13)
O5	0.0255 (11)	0.0267 (12)	0.0442 (14)	0.0024 (9)	−0.0124 (10)	−0.0045 (10)
O6	0.0424 (16)	0.0540 (18)	0.0659 (19)	−0.0204 (14)	−0.0153 (14)	0.0098 (15)
O7	0.0356 (14)	0.0362 (14)	0.0644 (18)	0.0008 (11)	−0.0208 (13)	−0.0100 (13)
O8	0.0306 (13)	0.0355 (14)	0.0631 (18)	0.0112 (11)	−0.0033 (12)	−0.0019 (12)
O9	0.0458 (16)	0.0413 (15)	0.0507 (16)	0.0193 (12)	−0.0253 (13)	−0.0082 (12)
N1	0.0316 (15)	0.0393 (17)	0.0374 (16)	0.0030 (13)	−0.0070 (13)	−0.0042 (13)
N2	0.0397 (18)	0.055 (2)	0.0436 (18)	−0.0001 (16)	−0.0024 (15)	−0.0039 (16)
C1	0.036 (2)	0.047 (2)	0.042 (2)	0.0025 (17)	−0.0082 (16)	−0.0093 (16)
C2	0.073 (4)	0.092 (4)	0.040 (2)	0.018 (3)	−0.002 (2)	0.009 (2)
C3	0.055 (3)	0.083 (4)	0.053 (3)	0.026 (3)	−0.009 (2)	0.008 (3)
C4	0.050 (3)	0.091 (4)	0.056 (3)	0.017 (3)	−0.005 (2)	−0.010 (3)
C5	0.063 (3)	0.094 (4)	0.065 (3)	0.018 (3)	0.009 (3)	0.004 (3)

Geometric parameters (Å, º)

Co—N1	2.069 (3)	O4—H4WB	0.85 (3)
Co—O1	2.092 (3)	O5—H5WA	0.85 (3)
Co—O2	2.141 (3)	O5—H5WB	0.85 (3)
Co—O3	2.103 (3)	N1—C1	1.303 (5)
Co—O4	2.067 (3)	N1—C3	1.361 (6)
Co—O5	2.199 (2)	N2—C1	1.338 (5)
S—O6	1.463 (3)	N2—C2	1.376 (6)
S—O7	1.467 (3)	N2—C4	1.437 (6)
S—O8	1.476 (3)	C1—H1A	0.9300
S—O9	1.479 (3)	C2—C3	1.354 (7)
O1—H1WA	0.85 (3)	C2—H2A	0.9300
O1—H1WB	0.85 (3)	C3—H3A	0.9300
O2—H2WA	0.85 (3)	C4—C5	1.279 (7)
O2—H2WB	0.86 (3)	C4—H4A	0.9300
O3—H3WA	0.85 (3)	C5—H5A	0.9300
O3—H3WB	0.85 (3)	C5—H5B	0.9300
O4—H4WA	0.85 (3)
O4—Co—N1	97.60 (13)	H3WA—O3—H3WB	107 (6)
O4—Co—O1	172.04 (12)	Co—O4—H4WA	130 (5)
N1—Co—O1	90.19 (12)	Co—O4—H4WB	114 (4)
O4—Co—O3	88.68 (13)	H4WA—O4—H4WB	108 (5)
N1—Co—O3	173.68 (11)	Co—O5—H5WA	108 (5)
O1—Co—O3	83.56 (11)	Co—O5—H5WB	104 (5)
O4—Co—O2	90.23 (11)	H5WA—O5—H5WB	107 (6)
N1—Co—O2	92.21 (12)	C1—N1—C3	105.0 (4)
O1—Co—O2	91.12 (11)	C1—N1—Co	128.0 (3)
O3—Co—O2	86.96 (11)	C3—N1—Co	126.9 (3)
O4—Co—O5	85.84 (10)	C1—N2—C2	106.7 (4)
N1—Co—O5	91.87 (11)	C1—N2—C4	124.2 (4)
O1—Co—O5	92.29 (10)	C2—N2—C4	129.1 (4)
O3—Co—O5	89.36 (11)	N1—C1—N2	112.4 (4)
O2—Co—O5	174.67 (10)	N1—C1—H1A	123.8
O6—S—O7	109.97 (19)	N2—C1—H1A	123.8
O6—S—O8	108.12 (19)	C3—C2—N2	105.1 (4)
O7—S—O8	109.66 (17)	C3—C2—H2A	127.4
O6—S—O9	110.33 (18)	N2—C2—H2A	127.4
O7—S—O9	109.81 (16)	C2—C3—N1	110.7 (4)
O8—S—O9	108.92 (17)	C2—C3—H3A	124.6
Co—O1—H1WA	117 (5)	N1—C3—H3A	124.6
Co—O1—H1WB	123 (5)	C5—C4—N2	124.4 (5)
H1WA—O1—H1WB	107 (6)	C5—C4—H4A	117.8
Co—O2—H2WA	110 (5)	N2—C4—H4A	117.8
Co—O2—H2WB	108 (5)	C4—C5—H5A	120.0
H2WA—O2—H2WB	107 (6)	C4—C5—H5B	120.0
Co—O3—H3WA	115 (5)	H5A—C5—H5B	120.0
Co—O3—H3WB	123 (5)
O4—Co—N1—C1	68.8 (4)	C2—N2—C1—N1	1.7 (6)
O1—Co—N1—C1	−109.5 (4)	C4—N2—C1—N1	−178.5 (4)
O2—Co—N1—C1	159.3 (3)	C1—N2—C2—C3	−1.3 (7)
O5—Co—N1—C1	−17.2 (3)	C4—N2—C2—C3	178.9 (5)
O4—Co—N1—C3	−114.5 (4)	N2—C2—C3—N1	0.6 (7)
O1—Co—N1—C3	67.1 (4)	C1—N1—C3—C2	0.4 (7)
O2—Co—N1—C3	−24.0 (4)	Co—N1—C3—C2	−176.8 (4)
O5—Co—N1—C3	159.4 (4)	C1—N2—C4—C5	−176.7 (6)
C3—N1—C1—N2	−1.3 (5)	C2—N2—C4—C5	3.1 (10)
Co—N1—C1—N2	175.9 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5WA···O9^i	0.85 (3)	1.90 (7)	2.750 (4)	171 (6)
O4—H4WA···O6^ii	0.85 (3)	1.83 (4)	2.673 (5)	171 (6)
O2—H2WA···O7^iii	0.85 (3)	1.90 (5)	2.714 (4)	161 (5)
O5—H5WB···O8	0.85 (3)	1.99 (4)	2.839 (3)	173 (6)
O2—H2WB···O5^ii	0.85 (3)	2.10 (5)	2.926 (4)	163 (6)
O4—H4WB···O8	0.85 (3)	1.93 (5)	2.752 (4)	162 (7)
O1—H1WA···O7^iv	0.85 (3)	1.92 (4)	2.765 (4)	169 (6)
O1—H1WB···O9^iii	0.85 (3)	2.07 (5)	2.818 (4)	146 (6)
O3—H3WB···O8^v	0.85 (3)	1.88 (5)	2.730 (6)	174 (5)
O3—H3WA···O9^iii	0.85 (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.