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Acta Crystallogr Sect E Struct Rep Online. 2008 October 1; 64(Pt 10): m1350.
Published online 2008 September 30. doi:  10.1107/S1600536808030882
PMCID: PMC2959305

Diaqua­bis[2-(2-pyridylmeth­oxy)pyrazine-κN 4]bis­(thio­cyanato-κN)cobalt(II)

Abstract

In the title complex, [Co(NCS)2(C10H9N3O)2(H2O)2], the CoII ion is located on a crystallographic twofold rotation axis and is in a slightly distorted octa­hedral CoN4O2 coordination environment. The dihedral angle between the pyridine and pyrazine rings is 85.86 (10)°. In the crystal structure, inter­molecular O—H(...)N and O—H(...)S hydrogen bonds link complex mol­ecules into a three-dimensional network.

Related literature

For the isostructural Mn complex, see: Li (2007 [triangle]). For a related structure, see: Zhao et al. (2007 [triangle]).

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Object name is e-64-m1350-scheme1.jpg

Experimental

Crystal data

  • [Co(NCS)2(C10H9N3O)2(H2O)2]
  • M r = 585.53
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1350-efi2.jpg
  • a = 19.954 (4) Å
  • b = 10.044 (2) Å
  • c = 13.650 (3) Å
  • β = 110.749 (3)°
  • V = 2558.2 (10) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.88 mm−1
  • T = 298 (2) K
  • 0.41 × 0.31 × 0.16 mm

Data collection

  • Bruker SMART APEX CCD diffractometer
  • Absorption correction: multi-scan SADABS (Sheldrick, 1996 [triangle]) T min = 0.714, T max = 0.872
  • 7123 measured reflections
  • 2768 independent reflections
  • 2361 reflections with I > 2σ(I)
  • R int = 0.032

Refinement

  • R[F 2 > 2σ(F 2)] = 0.039
  • wR(F 2) = 0.108
  • S = 1.09
  • 2768 reflections
  • 168 parameters
  • 1 restraint
  • H-atom parameters constrained
  • Δρmax = 0.75 e Å−3
  • Δρmin = −0.37 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

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

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808030882/lh2698sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808030882/lh2698Isup2.hkl

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

Acknowledgments

This work was supported by the Doctors’ Foundation of Binzhou University.

supplementary crystallographic information

Comment

Molecules containing both pyridyl and pyrazinyl groups are useful multi-dentate ligands and a number of complexes have been published dealing with these ligands (e.g. Zhao et al., 2007; Li, 2007). Herein the crystal structure of the title complex, (I), with 2-((pyridin-2-yl)methoxy)pyrazine as ligand, is reported.

The molecular structure of (I) is shown in Fig. 1. In the mono-nuclear complex, atom Co1 lies on a twofold rotation axis and its coordination geometry is slightly distorted octahedral (Table 1). In the crystal structure, complex molecules are linked via intermolecular O—H···S and O—H···N hydrogen bonds as shown in Fig. 2 and Table 2, to form a three-dimensional network. The diheral angle between pyridine and pyrazine rings is 85.86 (10)°. The title compound is isostructural with the MnII complex (Li, 2007).

Experimental

A 5 ml methanol solution of 2-[(pyridin-2-yl)methoxy]pyrazine (0.0526 g, 0.281 mmol) was added into 10 ml H2O solution containing Co(ClO4)2.6H2O (0.1032 g, 0.282 mmol) and NaSCN (0.0457 g, 0.564 mmol), and the mixture was stirred for a few minutes. Red single crystals were obtained after the solution had been allowed to stand at room temperature for two weeks.

Refinement

The H atoms bonded to O atoms were located in a difference Fourier map, and included in their 'as found' positions. The C-bound H atoms were placed in calculated positions, C—H = 0.93–0.97 Å. All H atoms were refined as riding, with Uiso(H) = 1.2–1.5Ueq(C,O).

Figures

Fig. 1.
View of complex (I), showing the the asymmetric atom numbering scheme with thermal ellipsoids drawn at the 30% probability level. (symmetry code: (i) -x, y, -z + 3/2)
Fig. 2.
Part of the crystal structure of (I). Hydrogen bonds are shown as dashed lines.

Crystal data

[Co(NCS)2(C10H9N3O)2(H2O)2]F(000) = 1204
Mr = 585.53Dx = 1.520 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3335 reflections
a = 19.954 (4) Åθ = 2.3–27.5°
b = 10.044 (2) ŵ = 0.88 mm1
c = 13.650 (3) ÅT = 298 K
β = 110.749 (3)°Block, red
V = 2558.2 (10) Å30.41 × 0.31 × 0.16 mm
Z = 4

Data collection

Bruker SMART APEX CCD diffractometer2768 independent reflections
Radiation source: fine-focus sealed tube2361 reflections with I > 2σ(I)
graphiteRint = 0.032
[var phi] and ω scansθmax = 27.0°, θmin = 2.2°
Absorption correction: multi-scan SADABS (Sheldrick, 1996)h = −25→21
Tmin = 0.714, Tmax = 0.872k = −11→12
7123 measured reflectionsl = −9→17

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.09w = 1/[σ2(Fo2) + (0.0638P)2 + 0.3122P] where P = (Fo2 + 2Fc2)/3
2768 reflections(Δ/σ)max = 0.008
168 parametersΔρmax = 0.75 e Å3
1 restraintΔρmin = −0.37 e Å3

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 (Å2)

xyzUiso*/Ueq
C10.23226 (11)−0.20768 (19)1.25209 (19)0.0415 (5)
H10.1927−0.25831.21360.050*
C20.25719 (13)−0.2109 (2)1.3601 (2)0.0473 (5)
H20.2351−0.26431.39550.057*
C30.31522 (12)−0.1337 (2)1.41439 (17)0.0471 (5)
H30.3328−0.13261.48720.057*
C40.34682 (12)−0.0580 (2)1.35887 (17)0.0474 (5)
H40.3863−0.00621.39610.057*
C50.26655 (10)−0.12879 (17)1.20171 (15)0.0336 (4)
C60.24197 (11)−0.1258 (2)1.08505 (16)0.0431 (5)
H6A0.2825−0.11381.06250.052*
H6B0.2184−0.20891.05620.052*
N20.17307 (9)−0.09050 (15)0.88100 (13)0.0385 (4)
C80.15889 (10)−0.00579 (18)0.94509 (15)0.0349 (4)
C90.13592 (11)−0.0711 (2)0.77904 (16)0.0425 (5)
H90.1426−0.13010.73080.051*
C100.08838 (10)0.0321 (2)0.74250 (16)0.0398 (5)
H100.06460.04210.67080.048*
C110.10991 (10)0.09863 (18)0.91016 (15)0.0341 (4)
H110.10120.15450.95870.041*
C120.02714 (11)0.28829 (18)0.53206 (17)0.0365 (4)
Co10.00000.28266 (3)0.75000.02902 (14)
N40.02348 (10)0.29084 (16)0.61484 (15)0.0394 (4)
N30.07579 (8)0.11899 (15)0.80922 (13)0.0330 (3)
N10.32395 (9)−0.05466 (17)1.25423 (13)0.0402 (4)
O10.19253 (8)−0.01598 (14)1.04945 (11)0.0455 (4)
O20.07922 (7)0.43031 (14)0.82323 (11)0.0425 (3)
H50.06370.49160.85320.064*
H80.10790.45990.79690.064*
S10.03352 (5)0.28165 (7)0.41650 (6)0.0722 (2)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.0319 (10)0.0342 (10)0.0538 (13)0.0006 (7)0.0096 (10)0.0005 (9)
C20.0484 (13)0.0442 (11)0.0552 (14)0.0083 (9)0.0257 (11)0.0133 (10)
C30.0505 (13)0.0511 (12)0.0351 (11)0.0126 (10)0.0096 (10)0.0053 (10)
C40.0409 (11)0.0471 (12)0.0439 (12)−0.0040 (9)0.0022 (10)−0.0025 (10)
C50.0296 (9)0.0283 (9)0.0380 (10)0.0092 (7)0.0059 (8)0.0013 (7)
C60.0425 (11)0.0390 (10)0.0387 (11)0.0150 (9)0.0032 (9)0.0006 (9)
N20.0362 (9)0.0342 (8)0.0403 (9)0.0070 (7)0.0075 (7)−0.0012 (7)
C80.0310 (9)0.0330 (9)0.0339 (10)0.0013 (7)0.0032 (8)−0.0014 (8)
C90.0439 (11)0.0420 (11)0.0367 (11)0.0094 (9)0.0082 (9)−0.0046 (9)
C100.0362 (10)0.0425 (10)0.0347 (10)0.0066 (8)0.0051 (9)−0.0033 (9)
C110.0294 (9)0.0315 (9)0.0354 (10)0.0028 (7)0.0040 (8)−0.0028 (8)
C120.0364 (10)0.0331 (9)0.0404 (9)0.0018 (7)0.0140 (9)0.0011 (8)
Co10.0249 (2)0.0302 (2)0.0284 (2)0.0000.00494 (15)0.000
N40.0405 (10)0.0391 (9)0.0397 (9)−0.0016 (7)0.0152 (8)0.0003 (7)
N30.0257 (7)0.0328 (8)0.0354 (8)0.0009 (6)0.0045 (6)−0.0013 (6)
N10.0346 (9)0.0398 (9)0.0419 (9)−0.0016 (7)0.0083 (8)0.0039 (8)
O10.0514 (9)0.0385 (7)0.0343 (8)0.0187 (6)−0.0002 (7)−0.0015 (6)
O20.0415 (8)0.0437 (8)0.0417 (8)−0.0125 (6)0.0137 (7)−0.0072 (6)
S10.1124 (7)0.0671 (5)0.0530 (4)0.0083 (4)0.0491 (4)0.0012 (3)

Geometric parameters (Å, °)

C1—C51.379 (3)C8—C111.397 (2)
C1—C21.380 (3)C9—C101.373 (3)
C1—H10.9300C9—H90.9300
C2—C31.372 (3)C10—N31.348 (2)
C2—H20.9300C10—H100.9300
C3—C41.374 (3)C11—N31.319 (2)
C3—H30.9300C11—H110.9300
C4—N11.337 (3)C12—N41.158 (3)
C4—H40.9300C12—S11.628 (2)
C5—N11.341 (2)Co1—N42.0597 (19)
C5—C61.491 (3)Co1—N4i2.0597 (19)
C6—O11.445 (2)Co1—O22.1394 (13)
C6—H6A0.9700Co1—O2i2.1394 (13)
C6—H6B0.9700Co1—N3i2.1856 (15)
N2—C81.321 (2)Co1—N32.1856 (15)
N2—C91.339 (3)O2—H50.8552
C8—O11.346 (2)O2—H80.8316
C5—C1—C2119.44 (19)C9—C10—H10119.6
C5—C1—H1120.3N3—C11—C8120.83 (17)
C2—C1—H1120.3N3—C11—H11119.6
C3—C2—C1118.7 (2)C8—C11—H11119.6
C3—C2—H2120.7N4—C12—S1178.7 (2)
C1—C2—H2120.7N4—Co1—N4i175.43 (9)
C2—C3—C4118.6 (2)N4—Co1—O291.49 (6)
C2—C3—H3120.7N4i—Co1—O285.34 (6)
C4—C3—H3120.7N4—Co1—O2i85.34 (6)
N1—C4—C3123.60 (19)N4i—Co1—O2i91.49 (6)
N1—C4—H4118.2O2—Co1—O2i92.24 (8)
C3—C4—H4118.2N4—Co1—N3i92.63 (6)
N1—C5—C1122.21 (19)N4i—Co1—N3i90.81 (6)
N1—C5—C6117.08 (18)O2—Co1—N3i173.74 (6)
C1—C5—C6120.69 (18)O2i—Co1—N3i92.79 (6)
O1—C6—C5107.55 (16)N4—Co1—N390.81 (6)
O1—C6—H6A110.2N4i—Co1—N392.63 (6)
C5—C6—H6A110.2O2—Co1—N392.79 (6)
O1—C6—H6B110.2O2i—Co1—N3173.74 (6)
C5—C6—H6B110.2N3i—Co1—N382.45 (8)
H6A—C6—H6B108.5C12—N4—Co1170.41 (18)
C8—N2—C9115.14 (16)C11—N3—C10117.06 (16)
N2—C8—O1120.55 (16)C11—N3—Co1122.44 (12)
N2—C8—C11123.07 (17)C10—N3—Co1120.49 (13)
O1—C8—C11116.38 (17)C4—N1—C5117.44 (17)
N2—C9—C10122.97 (19)C8—O1—C6116.04 (15)
N2—C9—H9118.5Co1—O2—H5113.0
C10—C9—H9118.5Co1—O2—H8123.6
N3—C10—C9120.87 (19)H5—O2—H8111.7
N3—C10—H10119.6
C5—C1—C2—C30.8 (3)C9—C10—N3—Co1180.00 (15)
C1—C2—C3—C4−1.0 (3)N4—Co1—N3—C11150.92 (14)
C2—C3—C4—N10.3 (3)N4i—Co1—N3—C11−26.06 (15)
C2—C1—C5—N10.3 (3)O2—Co1—N3—C1159.39 (14)
C2—C1—C5—C6178.48 (17)N3i—Co1—N3—C11−116.53 (16)
N1—C5—C6—O1−88.0 (2)N4—Co1—N3—C10−30.49 (15)
C1—C5—C6—O193.7 (2)N4i—Co1—N3—C10152.53 (15)
C9—N2—C8—O1179.51 (18)O2—Co1—N3—C10−122.02 (14)
C9—N2—C8—C11−1.2 (3)N3i—Co1—N3—C1062.06 (13)
C8—N2—C9—C102.4 (3)C3—C4—N1—C50.7 (3)
N2—C9—C10—N3−1.2 (3)C1—C5—N1—C4−1.0 (3)
N2—C8—C11—N3−1.2 (3)C6—C5—N1—C4−179.25 (17)
O1—C8—C11—N3178.10 (17)N2—C8—O1—C6−1.9 (3)
C8—C11—N3—C102.4 (3)C11—C8—O1—C6178.76 (17)
C8—C11—N3—Co1−178.94 (13)C5—C6—O1—C8−173.42 (17)
C9—C10—N3—C11−1.3 (3)

Symmetry codes: (i) −x, y, −z+3/2.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O2—H5···S1ii0.862.583.4123 (17)164.
O2—H8···N1iii0.831.982.803 (2)172.

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH2698).

References

  • Bruker (2007). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Li, J.-M. (2007). Acta Cryst. E63, m2266.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Zhao, H.-Y., Shi, J.-M. & Liu, L.-D. (2007). Acta Cryst. E63, m441–m442.

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