In the title complex, [Co(NCS)
2(C
10H
9N
3O)
2(H
2O)
2], the Co
II ion is located on a crystallographic twofold rotation axis and is in a slightly distorted octahedral CoN
4O
2 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.
Supporting information
CCDC reference: 706007
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean
(C-C) = 0.003 Å
- R factor = 0.039
- wR factor = 0.108
- Data-to-parameter ratio = 16.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.02
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 -- N4 .. 5.04 su
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C12
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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.
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).
Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Diaquabis[2-(2-pyridylmethoxy)pyrazine-
κN
4]bis(thiocyanato-
κN)cobalt(II)
top
Crystal data top
[Co(NCS)2(C10H9N3O)2(H2O)2] | F(000) = 1204 |
Mr = 585.53 | Dx = 1.520 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3335 reflections |
a = 19.954 (4) Å | θ = 2.3–27.5° |
b = 10.044 (2) Å | µ = 0.88 mm−1 |
c = 13.650 (3) Å | T = 298 K |
β = 110.749 (3)° | Block, red |
V = 2558.2 (10) Å3 | 0.41 × 0.31 × 0.16 mm |
Z = 4 | |
Data collection top
Bruker SMART APEX CCD diffractometer | 2768 independent reflections |
Radiation source: fine-focus sealed tube | 2361 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ϕ and ω scans | θmax = 27.0°, θmin = 2.2° |
Absorption correction: multi-scan SADABS (Sheldrick, 1996) | h = −25→21 |
Tmin = 0.714, Tmax = 0.872 | k = −11→12 |
7123 measured reflections | l = −9→17 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0638P)2 + 0.3122P] where P = (Fo2 + 2Fc2)/3 |
2768 reflections | (Δ/σ)max = 0.008 |
168 parameters | Δρmax = 0.75 e Å−3 |
1 restraint | Δρmin = −0.37 e Å−3 |
Crystal data top
[Co(NCS)2(C10H9N3O)2(H2O)2] | V = 2558.2 (10) Å3 |
Mr = 585.53 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 19.954 (4) Å | µ = 0.88 mm−1 |
b = 10.044 (2) Å | T = 298 K |
c = 13.650 (3) Å | 0.41 × 0.31 × 0.16 mm |
β = 110.749 (3)° | |
Data collection top
Bruker SMART APEX CCD diffractometer | 2768 independent reflections |
Absorption correction: multi-scan SADABS (Sheldrick, 1996) | 2361 reflections with I > 2σ(I) |
Tmin = 0.714, Tmax = 0.872 | Rint = 0.032 |
7123 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.039 | 1 restraint |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.75 e Å−3 |
2768 reflections | Δρmin = −0.37 e Å−3 |
168 parameters | |
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 | |
C1 | 0.23226 (11) | −0.20768 (19) | 1.25209 (19) | 0.0415 (5) | |
H1 | 0.1927 | −0.2583 | 1.2136 | 0.050* | |
C2 | 0.25719 (13) | −0.2109 (2) | 1.3601 (2) | 0.0473 (5) | |
H2 | 0.2351 | −0.2643 | 1.3955 | 0.057* | |
C3 | 0.31522 (12) | −0.1337 (2) | 1.41439 (17) | 0.0471 (5) | |
H3 | 0.3328 | −0.1326 | 1.4872 | 0.057* | |
C4 | 0.34682 (12) | −0.0580 (2) | 1.35887 (17) | 0.0474 (5) | |
H4 | 0.3863 | −0.0062 | 1.3961 | 0.057* | |
C5 | 0.26655 (10) | −0.12879 (17) | 1.20171 (15) | 0.0336 (4) | |
C6 | 0.24197 (11) | −0.1258 (2) | 1.08505 (16) | 0.0431 (5) | |
H6A | 0.2825 | −0.1138 | 1.0625 | 0.052* | |
H6B | 0.2184 | −0.2089 | 1.0562 | 0.052* | |
N2 | 0.17307 (9) | −0.09050 (15) | 0.88100 (13) | 0.0385 (4) | |
C8 | 0.15889 (10) | −0.00579 (18) | 0.94509 (15) | 0.0349 (4) | |
C9 | 0.13592 (11) | −0.0711 (2) | 0.77904 (16) | 0.0425 (5) | |
H9 | 0.1426 | −0.1301 | 0.7308 | 0.051* | |
C10 | 0.08838 (10) | 0.0321 (2) | 0.74250 (16) | 0.0398 (5) | |
H10 | 0.0646 | 0.0421 | 0.6708 | 0.048* | |
C11 | 0.10991 (10) | 0.09863 (18) | 0.91016 (15) | 0.0341 (4) | |
H11 | 0.1012 | 0.1545 | 0.9587 | 0.041* | |
C12 | 0.02714 (11) | 0.28829 (18) | 0.53206 (17) | 0.0365 (4) | |
Co1 | 0.0000 | 0.28266 (3) | 0.7500 | 0.02902 (14) | |
N4 | 0.02348 (10) | 0.29084 (16) | 0.61484 (15) | 0.0394 (4) | |
N3 | 0.07579 (8) | 0.11899 (15) | 0.80922 (13) | 0.0330 (3) | |
N1 | 0.32395 (9) | −0.05466 (17) | 1.25423 (13) | 0.0402 (4) | |
O1 | 0.19253 (8) | −0.01598 (14) | 1.04945 (11) | 0.0455 (4) | |
O2 | 0.07922 (7) | 0.43031 (14) | 0.82323 (11) | 0.0425 (3) | |
H5 | 0.0637 | 0.4916 | 0.8532 | 0.064* | |
H8 | 0.1079 | 0.4599 | 0.7969 | 0.064* | |
S1 | 0.03352 (5) | 0.28165 (7) | 0.41650 (6) | 0.0722 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0319 (10) | 0.0342 (10) | 0.0538 (13) | 0.0006 (7) | 0.0096 (10) | 0.0005 (9) |
C2 | 0.0484 (13) | 0.0442 (11) | 0.0552 (14) | 0.0083 (9) | 0.0257 (11) | 0.0133 (10) |
C3 | 0.0505 (13) | 0.0511 (12) | 0.0351 (11) | 0.0126 (10) | 0.0096 (10) | 0.0053 (10) |
C4 | 0.0409 (11) | 0.0471 (12) | 0.0439 (12) | −0.0040 (9) | 0.0022 (10) | −0.0025 (10) |
C5 | 0.0296 (9) | 0.0283 (9) | 0.0380 (10) | 0.0092 (7) | 0.0059 (8) | 0.0013 (7) |
C6 | 0.0425 (11) | 0.0390 (10) | 0.0387 (11) | 0.0150 (9) | 0.0032 (9) | 0.0006 (9) |
N2 | 0.0362 (9) | 0.0342 (8) | 0.0403 (9) | 0.0070 (7) | 0.0075 (7) | −0.0012 (7) |
C8 | 0.0310 (9) | 0.0330 (9) | 0.0339 (10) | 0.0013 (7) | 0.0032 (8) | −0.0014 (8) |
C9 | 0.0439 (11) | 0.0420 (11) | 0.0367 (11) | 0.0094 (9) | 0.0082 (9) | −0.0046 (9) |
C10 | 0.0362 (10) | 0.0425 (10) | 0.0347 (10) | 0.0066 (8) | 0.0051 (9) | −0.0033 (9) |
C11 | 0.0294 (9) | 0.0315 (9) | 0.0354 (10) | 0.0028 (7) | 0.0040 (8) | −0.0028 (8) |
C12 | 0.0364 (10) | 0.0331 (9) | 0.0404 (9) | 0.0018 (7) | 0.0140 (9) | 0.0011 (8) |
Co1 | 0.0249 (2) | 0.0302 (2) | 0.0284 (2) | 0.000 | 0.00494 (15) | 0.000 |
N4 | 0.0405 (10) | 0.0391 (9) | 0.0397 (9) | −0.0016 (7) | 0.0152 (8) | 0.0003 (7) |
N3 | 0.0257 (7) | 0.0328 (8) | 0.0354 (8) | 0.0009 (6) | 0.0045 (6) | −0.0013 (6) |
N1 | 0.0346 (9) | 0.0398 (9) | 0.0419 (9) | −0.0016 (7) | 0.0083 (8) | 0.0039 (8) |
O1 | 0.0514 (9) | 0.0385 (7) | 0.0343 (8) | 0.0187 (6) | −0.0002 (7) | −0.0015 (6) |
O2 | 0.0415 (8) | 0.0437 (8) | 0.0417 (8) | −0.0125 (6) | 0.0137 (7) | −0.0072 (6) |
S1 | 0.1124 (7) | 0.0671 (5) | 0.0530 (4) | 0.0083 (4) | 0.0491 (4) | 0.0012 (3) |
Geometric parameters (Å, º) top
C1—C5 | 1.379 (3) | C8—C11 | 1.397 (2) |
C1—C2 | 1.380 (3) | C9—C10 | 1.373 (3) |
C1—H1 | 0.9300 | C9—H9 | 0.9300 |
C2—C3 | 1.372 (3) | C10—N3 | 1.348 (2) |
C2—H2 | 0.9300 | C10—H10 | 0.9300 |
C3—C4 | 1.374 (3) | C11—N3 | 1.319 (2) |
C3—H3 | 0.9300 | C11—H11 | 0.9300 |
C4—N1 | 1.337 (3) | C12—N4 | 1.158 (3) |
C4—H4 | 0.9300 | C12—S1 | 1.628 (2) |
C5—N1 | 1.341 (2) | Co1—N4 | 2.0597 (19) |
C5—C6 | 1.491 (3) | Co1—N4i | 2.0597 (19) |
C6—O1 | 1.445 (2) | Co1—O2 | 2.1394 (13) |
C6—H6A | 0.9700 | Co1—O2i | 2.1394 (13) |
C6—H6B | 0.9700 | Co1—N3i | 2.1856 (15) |
N2—C8 | 1.321 (2) | Co1—N3 | 2.1856 (15) |
N2—C9 | 1.339 (3) | O2—H5 | 0.8552 |
C8—O1 | 1.346 (2) | O2—H8 | 0.8316 |
| | | |
C5—C1—C2 | 119.44 (19) | C9—C10—H10 | 119.6 |
C5—C1—H1 | 120.3 | N3—C11—C8 | 120.83 (17) |
C2—C1—H1 | 120.3 | N3—C11—H11 | 119.6 |
C3—C2—C1 | 118.7 (2) | C8—C11—H11 | 119.6 |
C3—C2—H2 | 120.7 | N4—C12—S1 | 178.7 (2) |
C1—C2—H2 | 120.7 | N4—Co1—N4i | 175.43 (9) |
C2—C3—C4 | 118.6 (2) | N4—Co1—O2 | 91.49 (6) |
C2—C3—H3 | 120.7 | N4i—Co1—O2 | 85.34 (6) |
C4—C3—H3 | 120.7 | N4—Co1—O2i | 85.34 (6) |
N1—C4—C3 | 123.60 (19) | N4i—Co1—O2i | 91.49 (6) |
N1—C4—H4 | 118.2 | O2—Co1—O2i | 92.24 (8) |
C3—C4—H4 | 118.2 | N4—Co1—N3i | 92.63 (6) |
N1—C5—C1 | 122.21 (19) | N4i—Co1—N3i | 90.81 (6) |
N1—C5—C6 | 117.08 (18) | O2—Co1—N3i | 173.74 (6) |
C1—C5—C6 | 120.69 (18) | O2i—Co1—N3i | 92.79 (6) |
O1—C6—C5 | 107.55 (16) | N4—Co1—N3 | 90.81 (6) |
O1—C6—H6A | 110.2 | N4i—Co1—N3 | 92.63 (6) |
C5—C6—H6A | 110.2 | O2—Co1—N3 | 92.79 (6) |
O1—C6—H6B | 110.2 | O2i—Co1—N3 | 173.74 (6) |
C5—C6—H6B | 110.2 | N3i—Co1—N3 | 82.45 (8) |
H6A—C6—H6B | 108.5 | C12—N4—Co1 | 170.41 (18) |
C8—N2—C9 | 115.14 (16) | C11—N3—C10 | 117.06 (16) |
N2—C8—O1 | 120.55 (16) | C11—N3—Co1 | 122.44 (12) |
N2—C8—C11 | 123.07 (17) | C10—N3—Co1 | 120.49 (13) |
O1—C8—C11 | 116.38 (17) | C4—N1—C5 | 117.44 (17) |
N2—C9—C10 | 122.97 (19) | C8—O1—C6 | 116.04 (15) |
N2—C9—H9 | 118.5 | Co1—O2—H5 | 113.0 |
C10—C9—H9 | 118.5 | Co1—O2—H8 | 123.6 |
N3—C10—C9 | 120.87 (19) | H5—O2—H8 | 111.7 |
N3—C10—H10 | 119.6 | | |
| | | |
C5—C1—C2—C3 | 0.8 (3) | C9—C10—N3—Co1 | 180.00 (15) |
C1—C2—C3—C4 | −1.0 (3) | N4—Co1—N3—C11 | 150.92 (14) |
C2—C3—C4—N1 | 0.3 (3) | N4i—Co1—N3—C11 | −26.06 (15) |
C2—C1—C5—N1 | 0.3 (3) | O2—Co1—N3—C11 | 59.39 (14) |
C2—C1—C5—C6 | 178.48 (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—O1 | 93.7 (2) | N4i—Co1—N3—C10 | 152.53 (15) |
C9—N2—C8—O1 | 179.51 (18) | O2—Co1—N3—C10 | −122.02 (14) |
C9—N2—C8—C11 | −1.2 (3) | N3i—Co1—N3—C10 | 62.06 (13) |
C8—N2—C9—C10 | 2.4 (3) | C3—C4—N1—C5 | 0.7 (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—N3 | 178.10 (17) | N2—C8—O1—C6 | −1.9 (3) |
C8—C11—N3—C10 | 2.4 (3) | C11—C8—O1—C6 | 178.76 (17) |
C8—C11—N3—Co1 | −178.94 (13) | C5—C6—O1—C8 | −173.42 (17) |
C9—C10—N3—C11 | −1.3 (3) | | |
Symmetry code: (i) −x, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H5···S1ii | 0.86 | 2.58 | 3.4123 (17) | 164 |
O2—H8···N1iii | 0.83 | 1.98 | 2.803 (2) | 172 |
Symmetry codes: (ii) x, −y+1, z+1/2; (iii) −x+1/2, −y+1/2, −z+2. |
Experimental details
Crystal data |
Chemical formula | [Co(NCS)2(C10H9N3O)2(H2O)2] |
Mr | 585.53 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 19.954 (4), 10.044 (2), 13.650 (3) |
β (°) | 110.749 (3) |
V (Å3) | 2558.2 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.88 |
Crystal size (mm) | 0.41 × 0.31 × 0.16 |
|
Data collection |
Diffractometer | Bruker SMART APEX CCD diffractometer |
Absorption correction | Multi-scan SADABS (Sheldrick, 1996) |
Tmin, Tmax | 0.714, 0.872 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7123, 2768, 2361 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.638 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.108, 1.09 |
No. of reflections | 2768 |
No. of parameters | 168 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.75, −0.37 |
Selected geometric parameters (Å, º) topCo1—N4 | 2.0597 (19) | Co1—N3 | 2.1856 (15) |
Co1—O2 | 2.1394 (13) | | |
| | | |
N4—Co1—N4i | 175.43 (9) | O2—Co1—N3i | 173.74 (6) |
N4—Co1—O2 | 91.49 (6) | N4—Co1—N3 | 90.81 (6) |
N4i—Co1—O2 | 85.34 (6) | O2—Co1—N3 | 92.79 (6) |
O2—Co1—O2i | 92.24 (8) | N3i—Co1—N3 | 82.45 (8) |
N4—Co1—N3i | 92.63 (6) | | |
Symmetry code: (i) −x, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H5···S1ii | 0.86 | 2.58 | 3.4123 (17) | 164.1 |
O2—H8···N1iii | 0.83 | 1.98 | 2.803 (2) | 171.6 |
Symmetry codes: (ii) x, −y+1, z+1/2; (iii) −x+1/2, −y+1/2, −z+2. |
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).