Acta Cryst. (2008). E64, m645 [ doi:10.1107/S1600536808009422 ]
In the cation of the title compound, [Co(H2O)6](C13H10NO4S)2, the Co atom lies on a centre of symmetry and its coordination geometry is octahedral. The crystal structure is stabilized by water-anion O-H
O hydrogen bonds. An intramolecular O-HN hydrogen bond occurs in the anion.
1 mmol of Cobalt acetate was added to a solution of salicylaldehyde-4-aminobenzene sulfonic acid (1 mmol) in 10 ml of 95% ethanol. The mixture was stirred for 2 h at refluxing temperature. Evaporating some ethanol, clear blocks of (I) were obtained after one weeks.
The H atoms were placed geometrically [C—H = 0.93 Å, O—H = 0.82 for hydroxy group and O—H = 0.85 Å for water molecules] and refined as riding with Uiso(H) = 1.2Ueq(carrier).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); 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: SHELXTL (Sheldrick, 2008).
![[Figure 1]](./at2558fig1thm.gif)
| Fig. 1. The molecular structure of (I) showing 30% displacement ellipsoids. [Symmetry code: (a) -x +2, -y, -z]. |
| [Co(H2O)6](C13H10NO4S)2 | F000 = 746 |
| Mr = 719.59 | Dx = 1.535 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation λ = 0.71073 Å |
| Hall symbol: -P 2yn | Cell parameters from 2380 reflections |
| a = 6.3216 (13) Å | θ = 2.4–25.3º |
| b = 35.211 (3) Å | µ = 0.76 mm−1 |
| c = 6.9924 (15) Å | T = 298 (2) K |
| β = 90.186 (2)º | Block, light purple |
| V = 1556.4 (5) Å3 | 0.40 × 0.35 × 0.15 mm |
| Z = 2 |
| Bruker SMART CCD area-detector diffractometer | 2749 independent reflections |
| Radiation source: fine-focus sealed tube | 2171 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.040 |
| T = 298(2) K | θmax = 25.0º |
| φ and ω scans | θmin = 2.3º |
| Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −5→7 |
| Tmin = 0.752, Tmax = 0.895 | k = −41→37 |
| 7328 measured reflections | l = −8→8 |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.071 | H-atom parameters constrained |
| wR(F2) = 0.141 | w = 1/[σ2(Fo2) + (0.0118P)2 + 5.6103P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.17 | (Δ/σ)max < 0.001 |
| 2749 reflections | Δρmax = 0.34 e Å−3 |
| 205 parameters | Δρmin = −0.69 e Å−3 |
| Primary atom site location: structure-invariant direct methods | Extinction correction: none |
| [Co(H2O)6](C13H10NO4S)2 | V = 1556.4 (5) Å3 |
| Mr = 719.59 | Z = 2 |
| Monoclinic, P21/n | Mo Kα |
| a = 6.3216 (13) Å | µ = 0.76 mm−1 |
| b = 35.211 (3) Å | T = 298 (2) K |
| c = 6.9924 (15) Å | 0.40 × 0.35 × 0.15 mm |
| β = 90.186 (2)º |
| Bruker SMART CCD area-detector diffractometer | 2749 independent reflections |
| Absorption correction: multi-scan (SADABS; Bruker, 2000) | 2171 reflections with I > 2σ(I) |
| Tmin = 0.752, Tmax = 0.895 | Rint = 0.040 |
| 7328 measured reflections |
| R[F2 > 2σ(F2)] = 0.071 | 205 parameters |
| wR(F2) = 0.141 | H-atom parameters constrained |
| S = 1.17 | Δρmax = 0.34 e Å−3 |
| 2749 reflections | Δρmin = −0.69 e Å−3 |
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. |
| x | y | z | Uiso*/Ueq | ||
| Co1 | 1.0000 | 0.0000 | 0.0000 | 0.0332 (3) | |
| N1 | 0.4234 (9) | 0.23121 (15) | 0.5063 (8) | 0.0585 (14) | |
| O1 | 0.5135 (6) | 0.05103 (11) | 0.3289 (6) | 0.0480 (10) | |
| O2 | 0.5140 (6) | 0.05158 (12) | 0.6754 (6) | 0.0504 (11) | |
| O3 | 0.8400 (5) | 0.06145 (11) | 0.5055 (5) | 0.0418 (9) | |
| O4 | 0.1496 (8) | 0.28449 (14) | 0.5667 (7) | 0.0772 (15) | |
| H4 | 0.1993 | 0.2632 | 0.5809 | 0.116* | |
| O5 | 0.7065 (5) | 0.02585 (12) | 0.0016 (6) | 0.0496 (10) | |
| H5A | 0.6839 | 0.0392 | −0.0978 | 0.060* | |
| H5B | 0.6850 | 0.0389 | 0.1020 | 0.060* | |
| O6 | 1.1038 (6) | 0.03462 (13) | 0.2207 (6) | 0.0571 (12) | |
| H6A | 1.2332 | 0.0310 | 0.2484 | 0.069* | |
| H6B | 1.0279 | 0.0325 | 0.3203 | 0.069* | |
| O7 | 1.1055 (6) | 0.03864 (12) | −0.2024 (6) | 0.0575 (12) | |
| H7A | 1.0260 | 0.0392 | −0.3007 | 0.069* | |
| H7B | 1.2326 | 0.0344 | −0.2355 | 0.069* | |
| S1 | 0.61081 (19) | 0.06622 (4) | 0.50249 (19) | 0.0345 (3) | |
| C1 | 0.5625 (8) | 0.11545 (15) | 0.4991 (7) | 0.0349 (12) | |
| C2 | 0.3648 (9) | 0.12848 (17) | 0.4446 (9) | 0.0471 (15) | |
| H2 | 0.2605 | 0.1115 | 0.4059 | 0.056* | |
| C3 | 0.3241 (10) | 0.16694 (17) | 0.4483 (10) | 0.0542 (17) | |
| H3 | 0.1907 | 0.1758 | 0.4140 | 0.065* | |
| C4 | 0.4787 (10) | 0.19236 (17) | 0.5021 (10) | 0.0522 (15) | |
| C5 | 0.6758 (10) | 0.17953 (18) | 0.5569 (9) | 0.0545 (17) | |
| H5 | 0.7794 | 0.1967 | 0.5950 | 0.065* | |
| C6 | 0.7197 (9) | 0.14085 (17) | 0.5552 (8) | 0.0471 (15) | |
| H6 | 0.8527 | 0.1320 | 0.5911 | 0.056* | |
| C7 | 0.5616 (11) | 0.25709 (18) | 0.4752 (10) | 0.0571 (17) | |
| H7 | 0.6992 | 0.2500 | 0.4448 | 0.069* | |
| C8 | 0.5093 (11) | 0.29731 (17) | 0.4862 (10) | 0.0542 (16) | |
| C9 | 0.3064 (12) | 0.3093 (2) | 0.5366 (10) | 0.0624 (19) | |
| C10 | 0.2661 (13) | 0.34768 (19) | 0.5538 (10) | 0.067 (2) | |
| H10 | 0.1313 | 0.3557 | 0.5881 | 0.080* | |
| C11 | 0.4190 (14) | 0.3740 (2) | 0.5216 (10) | 0.071 (2) | |
| H11 | 0.3882 | 0.3997 | 0.5362 | 0.085* | |
| C12 | 0.6230 (15) | 0.3628 (2) | 0.4664 (12) | 0.080 (2) | |
| H12 | 0.7268 | 0.3808 | 0.4399 | 0.095* | |
| C13 | 0.6654 (12) | 0.32435 (19) | 0.4525 (10) | 0.0661 (19) | |
| H13 | 0.8009 | 0.3164 | 0.4199 | 0.079* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Co1 | 0.0218 (5) | 0.0452 (6) | 0.0327 (5) | −0.0015 (5) | −0.0018 (4) | −0.0005 (5) |
| N1 | 0.063 (4) | 0.047 (3) | 0.066 (4) | 0.009 (3) | −0.001 (3) | −0.008 (3) |
| O1 | 0.032 (2) | 0.060 (3) | 0.051 (3) | 0.0021 (18) | −0.0070 (18) | −0.011 (2) |
| O2 | 0.035 (2) | 0.065 (3) | 0.051 (3) | 0.0022 (19) | 0.0071 (18) | 0.018 (2) |
| O3 | 0.0233 (18) | 0.057 (2) | 0.045 (2) | 0.0035 (17) | 0.0008 (16) | 0.0017 (19) |
| O4 | 0.081 (4) | 0.063 (3) | 0.087 (4) | 0.014 (3) | 0.020 (3) | 0.006 (3) |
| O5 | 0.037 (2) | 0.075 (3) | 0.037 (2) | 0.013 (2) | −0.0008 (17) | 0.001 (2) |
| O6 | 0.028 (2) | 0.095 (3) | 0.048 (3) | −0.002 (2) | −0.0009 (18) | −0.023 (2) |
| O7 | 0.028 (2) | 0.090 (3) | 0.055 (3) | −0.002 (2) | −0.0028 (18) | 0.026 (2) |
| S1 | 0.0233 (6) | 0.0456 (8) | 0.0348 (7) | 0.0022 (6) | −0.0004 (5) | 0.0012 (6) |
| C1 | 0.028 (3) | 0.047 (3) | 0.030 (3) | 0.002 (2) | −0.002 (2) | −0.001 (2) |
| C2 | 0.033 (3) | 0.051 (4) | 0.058 (4) | 0.002 (3) | −0.016 (3) | −0.002 (3) |
| C3 | 0.041 (3) | 0.049 (4) | 0.072 (5) | 0.011 (3) | −0.005 (3) | −0.001 (3) |
| C4 | 0.053 (4) | 0.048 (3) | 0.056 (4) | 0.012 (3) | 0.001 (3) | −0.003 (3) |
| C5 | 0.061 (4) | 0.045 (4) | 0.057 (4) | −0.004 (3) | −0.014 (3) | −0.009 (3) |
| C6 | 0.038 (3) | 0.057 (4) | 0.046 (4) | −0.001 (3) | −0.014 (3) | −0.003 (3) |
| C7 | 0.061 (4) | 0.053 (4) | 0.057 (4) | 0.012 (3) | −0.001 (3) | −0.007 (3) |
| C8 | 0.065 (4) | 0.049 (4) | 0.049 (4) | 0.002 (3) | −0.003 (3) | −0.013 (3) |
| C9 | 0.084 (5) | 0.057 (4) | 0.047 (4) | 0.007 (4) | 0.008 (4) | −0.002 (3) |
| C10 | 0.104 (6) | 0.045 (4) | 0.051 (4) | 0.017 (4) | 0.008 (4) | −0.003 (3) |
| C11 | 0.107 (6) | 0.046 (4) | 0.059 (5) | 0.019 (4) | −0.010 (4) | −0.002 (4) |
| C12 | 0.105 (7) | 0.045 (4) | 0.089 (6) | 0.000 (4) | −0.009 (5) | 0.001 (4) |
| C13 | 0.067 (5) | 0.057 (4) | 0.075 (5) | 0.003 (4) | −0.005 (4) | −0.007 (4) |
| Co1—O5 | 2.067 (3) | C1—C6 | 1.392 (7) |
| Co1—O5i | 2.067 (3) | C2—C3 | 1.379 (8) |
| Co1—O6 | 2.072 (4) | C2—H2 | 0.9300 |
| Co1—O6i | 2.072 (4) | C3—C4 | 1.377 (8) |
| Co1—O7i | 2.075 (4) | C3—H3 | 0.9300 |
| Co1—O7 | 2.075 (4) | C4—C5 | 1.379 (8) |
| N1—C7 | 1.281 (8) | C5—C6 | 1.390 (8) |
| N1—C4 | 1.412 (7) | C5—H5 | 0.9300 |
| O1—S1 | 1.460 (4) | C6—H6 | 0.9300 |
| O2—S1 | 1.452 (4) | C7—C8 | 1.456 (8) |
| O3—S1 | 1.458 (3) | C7—H7 | 0.9300 |
| O4—C9 | 1.338 (8) | C8—C13 | 1.392 (9) |
| O4—H4 | 0.8200 | C8—C9 | 1.397 (9) |
| O5—H5A | 0.8501 | C9—C10 | 1.381 (9) |
| O5—H5B | 0.8500 | C10—C11 | 1.359 (10) |
| O6—H6A | 0.8500 | C10—H10 | 0.9300 |
| O6—H6B | 0.8500 | C11—C12 | 1.404 (10) |
| O7—H7A | 0.8500 | C11—H11 | 0.9300 |
| O7—H7B | 0.8500 | C12—C13 | 1.384 (9) |
| S1—C1 | 1.760 (5) | C12—H12 | 0.9300 |
| C1—C2 | 1.384 (7) | C13—H13 | 0.9300 |
| O5—Co1—O5i | 180.0 (2) | C3—C2—H2 | 120.4 |
| O5—Co1—O6 | 91.09 (15) | C1—C2—H2 | 120.4 |
| O5i—Co1—O6 | 88.91 (15) | C4—C3—C2 | 120.8 (6) |
| O5—Co1—O6i | 88.91 (15) | C4—C3—H3 | 119.6 |
| O5i—Co1—O6i | 91.09 (15) | C2—C3—H3 | 119.6 |
| O6—Co1—O6i | 180.0 (2) | C3—C4—C5 | 120.2 (6) |
| O5—Co1—O7i | 89.69 (15) | C3—C4—N1 | 117.4 (6) |
| O5i—Co1—O7i | 90.31 (15) | C5—C4—N1 | 122.4 (6) |
| O6—Co1—O7i | 88.81 (17) | C4—C5—C6 | 119.9 (6) |
| O6i—Co1—O7i | 91.19 (17) | C4—C5—H5 | 120.0 |
| O5—Co1—O7 | 90.31 (15) | C6—C5—H5 | 120.0 |
| O5i—Co1—O7 | 89.69 (15) | C5—C6—C1 | 119.3 (5) |
| O6—Co1—O7 | 91.19 (17) | C5—C6—H6 | 120.3 |
| O6i—Co1—O7 | 88.81 (17) | C1—C6—H6 | 120.3 |
| O7i—Co1—O7 | 180.0 (3) | N1—C7—C8 | 121.8 (6) |
| C7—N1—C4 | 121.1 (6) | N1—C7—H7 | 119.1 |
| C9—O4—H4 | 109.5 | C8—C7—H7 | 119.1 |
| Co1—O5—H5A | 112.8 | C13—C8—C9 | 119.2 (6) |
| Co1—O5—H5B | 112.9 | C13—C8—C7 | 119.7 (6) |
| H5A—O5—H5B | 110.4 | C9—C8—C7 | 121.1 (6) |
| Co1—O6—H6A | 112.5 | O4—C9—C10 | 119.2 (7) |
| Co1—O6—H6B | 112.4 | O4—C9—C8 | 121.6 (6) |
| H6A—O6—H6B | 110.2 | C10—C9—C8 | 119.2 (7) |
| Co1—O7—H7A | 112.2 | C11—C10—C9 | 121.5 (7) |
| Co1—O7—H7B | 112.2 | C11—C10—H10 | 119.3 |
| H7A—O7—H7B | 110.0 | C9—C10—H10 | 119.3 |
| O2—S1—O3 | 111.6 (2) | C10—C11—C12 | 120.5 (7) |
| O2—S1—O1 | 112.6 (2) | C10—C11—H11 | 119.7 |
| O3—S1—O1 | 112.7 (2) | C12—C11—H11 | 119.7 |
| O2—S1—C1 | 106.7 (2) | C13—C12—C11 | 118.2 (8) |
| O3—S1—C1 | 106.6 (2) | C13—C12—H12 | 120.9 |
| O1—S1—C1 | 106.1 (2) | C11—C12—H12 | 120.9 |
| C2—C1—C6 | 120.5 (5) | C12—C13—C8 | 121.3 (7) |
| C2—C1—S1 | 119.1 (4) | C12—C13—H13 | 119.3 |
| C6—C1—S1 | 120.4 (4) | C8—C13—H13 | 119.3 |
| C3—C2—C1 | 119.3 (5) | ||
| O2—S1—C1—C2 | −77.9 (5) | C2—C1—C6—C5 | 0.4 (9) |
| O3—S1—C1—C2 | 162.7 (4) | S1—C1—C6—C5 | −178.0 (5) |
| O1—S1—C1—C2 | 42.4 (5) | C4—N1—C7—C8 | −177.6 (6) |
| O2—S1—C1—C6 | 100.5 (5) | N1—C7—C8—C13 | 179.6 (7) |
| O3—S1—C1—C6 | −18.9 (5) | N1—C7—C8—C9 | 1.8 (11) |
| O1—S1—C1—C6 | −139.2 (5) | C13—C8—C9—O4 | 178.6 (6) |
| C6—C1—C2—C3 | −0.7 (9) | C7—C8—C9—O4 | −3.6 (11) |
| S1—C1—C2—C3 | 177.7 (5) | C13—C8—C9—C10 | −0.7 (10) |
| C1—C2—C3—C4 | 1.2 (10) | C7—C8—C9—C10 | 177.1 (6) |
| C2—C3—C4—C5 | −1.3 (11) | O4—C9—C10—C11 | −178.9 (7) |
| C2—C3—C4—N1 | −178.6 (6) | C8—C9—C10—C11 | 0.4 (11) |
| C7—N1—C4—C3 | −150.6 (7) | C9—C10—C11—C12 | 1.1 (11) |
| C7—N1—C4—C5 | 32.2 (10) | C10—C11—C12—C13 | −2.2 (11) |
| C3—C4—C5—C6 | 0.9 (11) | C11—C12—C13—C8 | 2.0 (11) |
| N1—C4—C5—C6 | 178.2 (6) | C9—C8—C13—C12 | −0.5 (11) |
| C4—C5—C6—C1 | −0.5 (10) | C7—C8—C13—C12 | −178.3 (7) |
| Symmetry codes: (i) −x+2, −y, −z. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H4···N1 | 0.82 | 1.88 | 2.588 (7) | 143 |
| O5—H5A···O2ii | 0.85 | 1.96 | 2.736 (6) | 151 |
| O5—H5B···O1 | 0.85 | 1.97 | 2.744 (6) | 151 |
| O6—H6A···O1iii | 0.85 | 1.99 | 2.757 (5) | 150 |
| O6—H6B···O3 | 0.85 | 2.03 | 2.768 (5) | 144 |
| O7—H7A···O3ii | 0.85 | 1.96 | 2.759 (5) | 157 |
| O7—H7B···O2iv | 0.85 | 1.98 | 2.761 (5) | 152 |
| C6—H6···O3 | 0.93 | 2.56 | 2.918 (7) | 104 |
| Symmetry codes: (ii) x, y, z−1; (iii) x+1, y, z; (iv) x+1, y, z−1. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O4—H4···N1 | 0.82 | 1.88 | 2.588 (7) | 143 |
| O5—H5A···O2i | 0.85 | 1.96 | 2.736 (6) | 151 |
| O5—H5B···O1 | 0.85 | 1.97 | 2.744 (6) | 151 |
| O6—H6A···O1ii | 0.85 | 1.99 | 2.757 (5) | 150 |
| O6—H6B···O3 | 0.85 | 2.03 | 2.768 (5) | 144 |
| O7—H7A···O3i | 0.85 | 1.96 | 2.759 (5) | 157 |
| O7—H7B···O2iii | 0.85 | 1.98 | 2.761 (5) | 152 |
| C6—H6···O3 | 0.93 | 2.56 | 2.918 (7) | 104 |
| Symmetry codes: (i) x, y, z−1; (ii) x+1, y, z; (iii) x+1, y, z−1. |
The authors thank the National Natural Science Foundation of China (20671073), the National Natural Science Foundation of Shandong (Y2007B60), the Science and Technology Foundation of Weifang and Weifang University for research grant.
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As part of our ongoing studies of the coordination chemistry of Schiff base ligands (Xi-Shi & Yi-Min, 2008; Tai, Feng & Zhang, 2008; Tai, Yin & Feng, 2007; Tai, Yin, Feng & Kong, 2007; Tai, Yin & Hao, 2007; Wang et al., 2007; Tai et al., 2003), we now report the synthesis and structure of the title compound, (I), (Fig. 1).
In the molecule of (I), the Co (II) centre is six-coordinate with six O donors of the water molecules. The C7—N1 bond length of 1.281 (8) Å is close to double-bond. Otherwise, the geometrical parameters for (I) are in normal range (Allen et al., 1987). The dihedral angle between the two benzene ring is 33.5°, indicating that the molecule is non-planar, which perhaps correlates with the intramolecular and intermolecular hydrogen bonds (Table 1).