Experimental
Data collection
Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) Tmin = 0.745, Tmax = 0.842 6717 measured reflections 3073 independent reflections 2888 reflections with I > 2σ(I) Rint = 0.015
|
Co1—N3 | 2.109 (2) | Co1—N1 | 2.1697 (18) | Co1—O1 | 2.1838 (16) | | N3—Co1—N1 | 86.99 (7) | N3—Co1—O1 | 90.67 (7) | N1—Co1—O1 | 89.79 (6) | | |
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | O1—H15⋯O4i | 0.85 | 1.94 | 2.775 (3) | 167 | O1—H16⋯O2ii | 0.85 | 2.09 | 2.930 (3) | 171 | Symmetry codes: (i) -x+1, -y+1, -z; (ii) x-1, y, z. | |
Data collection: RAPID-AUTO (Rigaku, 1998
); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002
); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008
); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008
); molecular graphics: SHELXTL (Sheldrick, 2008
); software used to prepare material for publication: SHELXL97.
Supporting information
1,1'-Butane-1,4-diyldiimidazole ligand was prepared from imidazole and 1,4-dibromobutane in DMSO (Ma et al., 2003a). 1,1'-Butane-1,4-diyldiimidazole (0.76 g, 4 mmol) and cobalt dinitrate (0.73 g, 4 mmol) were dissolved in hot aqua solution (10 ml) to give a clear solution. The resulting solution was allowed to stand in a desiccator at room temperature for a week, pink crystals of (I) were obtained.
H atoms bound to C atoms were placed in calculated positions and treated as riding on their parent atoms, with C—H = 0.93 Å (aromatic), C—H = 0.97 Å (methylene), and with Uiso(H) = 1.2Ueq(C). Water H atoms were initially located in a difference Fourier map, but they were treated as riding on their parent atoms with O—H = 0.85 Å and with with Uiso(H) = 1.5Ueq(O).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
Poly[[[diaquacobalt(II)]-bis[µ
2-1,1'-(butane-1,4-diyl)diimidazole-
κ2N3:
N3']] dinitrate]
top Crystal data top [Co(C10H14N4)2(H2O)2](NO3)2 | Z = 1 |
Mr = 599.49 | F(000) = 313 |
Triclinic, P1 | Dx = 1.468 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.574 (7) Å | Cell parameters from 6295 reflections |
b = 8.692 (6) Å | θ = 3.0–27.5° |
c = 9.666 (5) Å | µ = 0.70 mm−1 |
α = 104.71 (2)° | T = 291 K |
β = 97.14 (3)° | Block, brown |
γ = 98.89 (3)° | 0.45 × 0.28 × 0.26 mm |
V = 678.2 (8) Å3 | |
Data collection top Rigaku R-AXIS RAPID diffractometer | 3073 independent reflections |
Radiation source: fine-focus sealed tube | 2888 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −11→11 |
Tmin = 0.745, Tmax = 0.842 | k = −11→11 |
6717 measured reflections | l = −12→12 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0539P)2 + 0.1966P] where P = (Fo2 + 2Fc2)/3 |
3073 reflections | (Δ/σ)max < 0.001 |
178 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.22 e Å−3 |
Crystal data top [Co(C10H14N4)2(H2O)2](NO3)2 | γ = 98.89 (3)° |
Mr = 599.49 | V = 678.2 (8) Å3 |
Triclinic, P1 | Z = 1 |
a = 8.574 (7) Å | Mo Kα radiation |
b = 8.692 (6) Å | µ = 0.70 mm−1 |
c = 9.666 (5) Å | T = 291 K |
α = 104.71 (2)° | 0.45 × 0.28 × 0.26 mm |
β = 97.14 (3)° | |
Data collection top Rigaku R-AXIS RAPID diffractometer | 3073 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2888 reflections with I > 2σ(I) |
Tmin = 0.745, Tmax = 0.842 | Rint = 0.015 |
6717 measured reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 1.16 | Δρmax = 0.35 e Å−3 |
3073 reflections | Δρmin = −0.22 e Å−3 |
178 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 | 0.1755 (2) | 0.2246 (2) | 0.53022 (19) | 0.0325 (4) | |
H1 | 0.2106 | 0.2822 | 0.6272 | 0.039* | |
C2 | 0.0680 (2) | 0.1572 (2) | 0.30656 (19) | 0.0336 (4) | |
H2 | 0.0131 | 0.1605 | 0.2184 | 0.040* | |
C3 | 0.1346 (2) | 0.0324 (2) | 0.3277 (2) | 0.0372 (4) | |
H3 | 0.1343 | −0.0642 | 0.2586 | 0.045* | |
C4 | 0.2858 (2) | −0.0192 (3) | 0.5505 (2) | 0.0424 (5) | |
H4 | 0.2518 | −0.1333 | 0.4989 | 0.051* | |
H5 | 0.2548 | −0.0033 | 0.6455 | 0.051* | |
C5 | 0.4672 (2) | 0.0257 (2) | 0.5695 (2) | 0.0386 (4) | |
H6 | 0.4997 | 0.1423 | 0.6092 | 0.046* | |
H7 | 0.5142 | −0.0241 | 0.6393 | 0.046* | |
C6 | 0.2528 (2) | 0.6569 (2) | 0.77832 (18) | 0.0304 (3) | |
H8 | 0.1736 | 0.6650 | 0.8359 | 0.036* | |
C7 | 0.3724 (2) | 0.6120 (2) | 0.59375 (19) | 0.0315 (3) | |
H9 | 0.3904 | 0.5825 | 0.4985 | 0.038* | |
C8 | 0.4887 (2) | 0.6696 (2) | 0.7135 (2) | 0.0352 (4) | |
H10 | 0.5989 | 0.6866 | 0.7159 | 0.042* | |
C9 | 0.4832 (3) | 0.7684 (3) | 0.9839 (2) | 0.0437 (5) | |
H11 | 0.5643 | 0.7091 | 1.0092 | 0.052* | |
H12 | 0.4018 | 0.7584 | 1.0441 | 0.052* | |
C10 | 0.5592 (2) | 0.9465 (3) | 1.0135 (2) | 0.0449 (5) | |
H13 | 0.6130 | 0.9868 | 1.1137 | 0.054* | |
H14 | 0.6398 | 0.9550 | 0.9523 | 0.054* | |
Co1 | 0.0000 | 0.5000 | 0.5000 | 0.02274 (11) | |
N1 | 0.09324 (17) | 0.27910 (17) | 0.43482 (15) | 0.0296 (3) | |
N2 | 0.20264 (17) | 0.07610 (18) | 0.47097 (17) | 0.0318 (3) | |
N3 | 0.22398 (16) | 0.60381 (16) | 0.63499 (15) | 0.0273 (3) | |
N4 | 0.41025 (18) | 0.69767 (19) | 0.83026 (16) | 0.0329 (3) | |
N5 | 0.8937 (2) | 0.6642 (2) | 0.02300 (18) | 0.0456 (4) | |
O1 | 0.08701 (16) | 0.57801 (16) | 0.32103 (13) | 0.0362 (3) | |
H15 | 0.1299 | 0.5143 | 0.2619 | 0.054* | |
H16 | 0.0215 | 0.6177 | 0.2734 | 0.054* | |
O2 | 0.8432 (2) | 0.6759 (3) | 0.13902 (17) | 0.0653 (5) | |
O3 | 1.0374 (3) | 0.7011 (3) | 0.0241 (2) | 0.0777 (6) | |
O4 | 0.7986 (3) | 0.6117 (3) | −0.09384 (18) | 0.0784 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0368 (9) | 0.0342 (9) | 0.0280 (8) | 0.0154 (7) | 0.0043 (6) | 0.0069 (6) |
C2 | 0.0329 (9) | 0.0340 (9) | 0.0296 (8) | 0.0099 (7) | −0.0003 (6) | 0.0018 (7) |
C3 | 0.0351 (9) | 0.0295 (8) | 0.0410 (10) | 0.0095 (7) | 0.0044 (7) | −0.0016 (7) |
C4 | 0.0378 (10) | 0.0439 (10) | 0.0616 (12) | 0.0199 (8) | 0.0163 (9) | 0.0325 (9) |
C5 | 0.0347 (9) | 0.0401 (10) | 0.0481 (11) | 0.0173 (8) | 0.0071 (8) | 0.0188 (8) |
C6 | 0.0275 (8) | 0.0326 (8) | 0.0281 (8) | 0.0071 (6) | 0.0016 (6) | 0.0040 (6) |
C7 | 0.0294 (8) | 0.0352 (9) | 0.0289 (8) | 0.0104 (7) | 0.0043 (6) | 0.0050 (6) |
C8 | 0.0252 (8) | 0.0408 (9) | 0.0361 (9) | 0.0074 (7) | 0.0022 (7) | 0.0052 (7) |
C9 | 0.0417 (10) | 0.0535 (12) | 0.0264 (9) | 0.0104 (9) | −0.0092 (7) | 0.0006 (8) |
C10 | 0.0347 (10) | 0.0518 (12) | 0.0331 (10) | 0.0069 (8) | −0.0095 (7) | −0.0068 (8) |
Co1 | 0.02260 (16) | 0.02296 (16) | 0.02042 (16) | 0.00763 (11) | −0.00069 (10) | 0.00224 (11) |
N1 | 0.0317 (7) | 0.0279 (7) | 0.0289 (7) | 0.0123 (6) | 0.0024 (5) | 0.0046 (5) |
N2 | 0.0292 (7) | 0.0300 (7) | 0.0415 (8) | 0.0124 (6) | 0.0095 (6) | 0.0137 (6) |
N3 | 0.0256 (7) | 0.0269 (7) | 0.0267 (7) | 0.0074 (5) | −0.0003 (5) | 0.0034 (5) |
N4 | 0.0286 (7) | 0.0367 (8) | 0.0273 (7) | 0.0071 (6) | −0.0034 (5) | 0.0017 (6) |
N5 | 0.0577 (11) | 0.0593 (11) | 0.0302 (8) | 0.0315 (9) | 0.0132 (7) | 0.0166 (7) |
O1 | 0.0396 (7) | 0.0424 (7) | 0.0261 (6) | 0.0096 (5) | 0.0033 (5) | 0.0091 (5) |
O2 | 0.0727 (12) | 0.0991 (15) | 0.0351 (8) | 0.0308 (11) | 0.0235 (8) | 0.0233 (9) |
O3 | 0.0612 (12) | 0.1029 (17) | 0.0649 (12) | 0.0139 (11) | 0.0261 (10) | 0.0096 (11) |
O4 | 0.0786 (13) | 0.1321 (19) | 0.0324 (8) | 0.0623 (13) | 0.0048 (8) | 0.0143 (10) |
Geometric parameters (Å, º) top C1—N1 | 1.318 (2) | C8—N4 | 1.373 (2) |
C1—N2 | 1.341 (2) | C8—H10 | 0.9300 |
C1—H1 | 0.9300 | C9—N4 | 1.470 (2) |
C2—C3 | 1.350 (3) | C9—C10 | 1.523 (3) |
C2—N1 | 1.379 (2) | C9—H11 | 0.9700 |
C2—H2 | 0.9300 | C9—H12 | 0.9700 |
C3—N2 | 1.366 (3) | C10—C10ii | 1.521 (4) |
C3—H3 | 0.9300 | C10—H13 | 0.9700 |
C4—N2 | 1.469 (2) | C10—H14 | 0.9700 |
C4—C5 | 1.519 (3) | Co1—N3 | 2.109 (2) |
C4—H4 | 0.9700 | Co1—N3iii | 2.109 (2) |
C4—H5 | 0.9700 | Co1—N1iii | 2.1697 (18) |
C5—C5i | 1.510 (4) | Co1—N1 | 2.1697 (18) |
C5—H6 | 0.9700 | Co1—O1iii | 2.1838 (16) |
C5—H7 | 0.9700 | Co1—O1 | 2.1838 (16) |
C6—N3 | 1.322 (2) | N5—O3 | 1.222 (3) |
C6—N4 | 1.339 (2) | N5—O2 | 1.238 (2) |
C6—H8 | 0.9300 | N5—O4 | 1.243 (3) |
C7—C8 | 1.360 (3) | O1—H15 | 0.8501 |
C7—N3 | 1.377 (2) | O1—H16 | 0.8500 |
C7—H9 | 0.9300 | | |
| | | |
N1—C1—N2 | 112.01 (16) | C9—C10—H13 | 108.7 |
N1—C1—H1 | 124.0 | C10ii—C10—H14 | 108.7 |
N2—C1—H1 | 124.0 | C9—C10—H14 | 108.7 |
C3—C2—N1 | 110.00 (16) | H13—C10—H14 | 107.6 |
C3—C2—H2 | 125.0 | N3—Co1—N3iii | 180.0 |
N1—C2—H2 | 125.0 | N3—Co1—N1iii | 93.01 (7) |
C2—C3—N2 | 106.29 (15) | N3iii—Co1—N1iii | 86.99 (7) |
C2—C3—H3 | 126.9 | N3—Co1—N1 | 86.99 (7) |
N2—C3—H3 | 126.9 | N3iii—Co1—N1 | 93.01 (7) |
N2—C4—C5 | 113.21 (16) | N1iii—Co1—N1 | 180.0 |
N2—C4—H4 | 108.9 | N3—Co1—O1iii | 89.33 (7) |
C5—C4—H4 | 108.9 | N3iii—Co1—O1iii | 90.67 (7) |
N2—C4—H5 | 108.9 | N1iii—Co1—O1iii | 89.79 (6) |
C5—C4—H5 | 108.9 | N1—Co1—O1iii | 90.21 (6) |
H4—C4—H5 | 107.8 | N3—Co1—O1 | 90.67 (7) |
C5i—C5—C4 | 113.9 (2) | N3iii—Co1—O1 | 89.33 (7) |
C5i—C5—H6 | 108.8 | N1iii—Co1—O1 | 90.21 (6) |
C4—C5—H6 | 108.8 | N1—Co1—O1 | 89.79 (6) |
C5i—C5—H7 | 108.8 | O1iii—Co1—O1 | 180.0 |
C4—C5—H7 | 108.8 | C1—N1—C2 | 104.72 (15) |
H6—C5—H7 | 107.7 | C1—N1—Co1 | 121.60 (12) |
N3—C6—N4 | 111.57 (16) | C2—N1—Co1 | 133.01 (12) |
N3—C6—H8 | 124.2 | C1—N2—C3 | 106.97 (15) |
N4—C6—H8 | 124.2 | C1—N2—C4 | 124.90 (17) |
C8—C7—N3 | 109.66 (16) | C3—N2—C4 | 128.10 (16) |
C8—C7—H9 | 125.2 | C6—N3—C7 | 105.41 (14) |
N3—C7—H9 | 125.2 | C6—N3—Co1 | 127.19 (12) |
C7—C8—N4 | 105.97 (16) | C7—N3—Co1 | 126.95 (12) |
C7—C8—H10 | 127.0 | C6—N4—C8 | 107.39 (15) |
N4—C8—H10 | 127.0 | C6—N4—C9 | 125.56 (17) |
N4—C9—C10 | 110.98 (17) | C8—N4—C9 | 126.96 (16) |
N4—C9—H11 | 109.4 | O3—N5—O2 | 119.7 (2) |
C10—C9—H11 | 109.4 | O3—N5—O4 | 120.4 (2) |
N4—C9—H12 | 109.4 | O2—N5—O4 | 119.8 (2) |
C10—C9—H12 | 109.4 | Co1—O1—H15 | 119.0 |
H11—C9—H12 | 108.0 | Co1—O1—H16 | 115.0 |
C10ii—C10—C9 | 114.1 (2) | H15—O1—H16 | 109.0 |
C10ii—C10—H13 | 108.7 | | |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+2, −z+2; (iii) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O1—H15···O4iv | 0.85 | 1.94 | 2.775 (3) | 167 |
O1—H16···O2v | 0.85 | 2.09 | 2.930 (3) | 171 |
Symmetry codes: (iv) −x+1, −y+1, −z; (v) x−1, y, z. |
Experimental details
Crystal data |
Chemical formula | [Co(C10H14N4)2(H2O)2](NO3)2 |
Mr | 599.49 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 291 |
a, b, c (Å) | 8.574 (7), 8.692 (6), 9.666 (5) |
α, β, γ (°) | 104.71 (2), 97.14 (3), 98.89 (3) |
V (Å3) | 678.2 (8) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.70 |
Crystal size (mm) | 0.45 × 0.28 × 0.26 |
|
Data collection |
Diffractometer | Rigaku R-AXIS RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.745, 0.842 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6717, 3073, 2888 |
Rint | 0.015 |
(sin θ/λ)max (Å−1) | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.096, 1.16 |
No. of reflections | 3073 |
No. of parameters | 178 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.35, −0.22 |
Selected geometric parameters (Å, º) topCo1—N3 | 2.109 (2) | Co1—O1 | 2.1838 (16) |
Co1—N1 | 2.1697 (18) | | |
| | | |
N3—Co1—N1 | 86.99 (7) | N1—Co1—O1 | 89.79 (6) |
N3—Co1—O1 | 90.67 (7) | | |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O1—H15···O4i | 0.85 | 1.94 | 2.775 (3) | 166.6 |
O1—H16···O2ii | 0.85 | 2.09 | 2.930 (3) | 170.7 |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) x−1, y, z. |
Acknowledgements
The authors thank Heilongjiang University for supporting this study.
References
Dong, G.-C. & Zhang, R.-C. (2006). Acta Cryst. E62, m1847–m1849. Web of Science CSD CrossRef IUCr Journals Google Scholar
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Google Scholar
Ma, J.-F., Yang, J., Zheng, G.-L. & Liu, J.-F. (2003). Inorg. Chem. 42, 7531–7534. Web of Science CSD CrossRef PubMed CAS Google Scholar
Rigaku (1998). RAPID-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku/MSC (2002). CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yu, Y.-H., Shi, A.-E., Su, Y., Hou, G.-F. & Gao, J.-S. (2008). Acta Cryst. E64, m628. Web of Science CSD CrossRef IUCr Journals Google Scholar
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The 1,1'-butane-1,4-diyldiimidazole as a flexible ligand exhibit a variety of supramolecular aggregation patterns (Ma et al., 2003; Dong et al., 2006; Yu et al., 2008). In this paper, we report the new title compound, (I), synthssized by the reaction of 1,1'-butane-1,4-diyldiimidazole ligand and cobalt dinitrate in aqua solution.
In (I), each CoII atom is located on a inversion centre and is six-coordinated in an octahedral environment by four N atoms from four different 1,1'-butane-1,4-diyldiimidazole ligands and two O atoms form the two water molecules (Fig. 1). The Co—N and Co—O distances are normal (Table 1). The CoII atoms are bridged by ligands, generating a two-dimensional (4,4)-network (Fig. 2).
In the crystal, a R44(12) motif is built up by O—H···O hydrogen bonding interaction between the uncoordinated nitrate anions and the coordinated water molecules,which linke the adjacent fishnet planes to a three-dimensional supramolecular structure (Fig. 3, Table 2).