Acta Cryst. (2008). E64, m1517 [ doi:10.1107/S1600536808035903 ]
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N)cadmium(II)The title compound, [Cd(C6H4NO3)2(H2O)4], was obtained by the reaction of cadmium chloride with 5-hydroxynicotinic acid. The CdII atom is located on an inversion centre and is coordinated by two N atoms from two 5-hydroxynicotinic acid ligands and four water molecules in a distorted octahedral geometry. The structure is stabilized by intermolecular O-H
O hydrogen bonds, forming a three-dimensional network.
A mixture of 0.5 mmol 5-hydroxynicotinic acid and 0.5 mmol of cadmium chloride in 10 ml distilled water was stirred for 30 min at 323 K, then the reaction mixture was filtered and well shaped colourless crystals of the title compound was obtained from the mother liquor by slow evaporation at room temperature for several days.
The H atoms bonded to C atoms were positioned geometrically [aromatic C—H = 0.93 Å and aliphatic C—H = 0.97 Å, Uiso(H) = 1.2Ueq(C)]. The H atoms bonded to O atoms were located in a difference Fourier maps and refined with O—H distance restraints of 0.85 and Uiso(H) = 1.5Ueq(O).
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: XPREP (Bruker, 2004); 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).
![[Figure 1]](./at2660fig1thm.gif)
| Fig. 1. A view of the molecule of (I), showing the atom-labelling scheme, displacement ellipsoids are shown at the 30% probability level. [Symmetry code: (A) -x + 1, -y + 1, -z + 2]. |
![[Figure 2]](./at2660fig2thm.gif)
| Fig. 2. A view of the three dimensional framework of the title compound. The O—H···O interactions are depicted by dashed lines. |
| [Cd(C6H4NO3)2(H2O)4] | Z = 1 |
| Mr = 460.68 | F(000) = 230 |
| Triclinic, P1 | Dx = 1.982 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
| a = 7.2190 (1) Å | Cell parameters from 5615 reflections |
| b = 7.2510 (1) Å | θ = 2.5–27.5° |
| c = 8.9260 (1) Å | µ = 1.48 mm−1 |
| α = 70.377 (1)° | T = 296 K |
| β = 68.154 (1)° | Sheet, colourless |
| γ = 65.717 (1)° | 0.27 × 0.17 × 0.07 mm |
| V = 385.97 (1) Å3 |
| Bruker APEXII diffractometer | 1759 independent reflections |
| Radiation source: fine-focus sealed tube | 1754 reflections with I > 2σ(I) |
| graphite | Rint = 0.017 |
| ω scans | θmax = 27.5°, θmin = 2.5° |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
| Tmin = 0.667, Tmax = 0.903 | k = −9→9 |
| 6067 measured reflections | l = −11→11 |
| 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)] = 0.016 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
| S = 1.09 | w = 1/[σ2(Fo2) + (0.0249P)2 + 0.1253P] where P = (Fo2 + 2Fc2)/3 |
| 1759 reflections | (Δ/σ)max < 0.001 |
| 131 parameters | Δρmax = 0.36 e Å−3 |
| 7 restraints | Δρmin = −0.33 e Å−3 |
| [Cd(C6H4NO3)2(H2O)4] | γ = 65.717 (1)° |
| Mr = 460.68 | V = 385.97 (1) Å3 |
| Triclinic, P1 | Z = 1 |
| a = 7.2190 (1) Å | Mo Kα radiation |
| b = 7.2510 (1) Å | µ = 1.48 mm−1 |
| c = 8.9260 (1) Å | T = 296 K |
| α = 70.377 (1)° | 0.27 × 0.17 × 0.07 mm |
| β = 68.154 (1)° |
| Bruker APEXII diffractometer | 1754 reflections with I > 2σ(I) |
| Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | Rint = 0.017 |
| Tmin = 0.667, Tmax = 0.903 | θmax = 27.5° |
| 6067 measured reflections | Standard reflections: 0 |
| 1759 independent reflections |
| R[F2 > 2σ(F2)] = 0.016 | H atoms treated by a mixture of independent and constrained refinement |
| wR(F2) = 0.042 | Δρmax = 0.36 e Å−3 |
| S = 1.09 | Δρmin = −0.33 e Å−3 |
| 1759 reflections | Absolute structure: ? |
| 131 parameters | Flack parameter: ? |
| 7 restraints | Rogers parameter: ? |
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 | ||
| Cd1 | 0.5000 | 0.5000 | 1.0000 | 0.02626 (6) | |
| O1 | 0.8938 (2) | 0.7990 (2) | 0.32463 (16) | 0.0427 (3) | |
| O1W | 0.2684 (3) | 0.3168 (3) | 1.07212 (17) | 0.0482 (4) | |
| H1WA | 0.287 (5) | 0.249 (4) | 1.009 (3) | 0.072* | |
| H1WB | 0.209 (5) | 0.270 (4) | 1.163 (2) | 0.072* | |
| O2 | 0.6901 (2) | 0.8709 (2) | 0.16430 (15) | 0.0429 (3) | |
| O2W | 0.7595 (2) | 0.2074 (2) | 0.92481 (18) | 0.0478 (4) | |
| H2WA | 0.881 (3) | 0.189 (4) | 0.865 (3) | 0.072* | |
| H2WB | 0.762 (5) | 0.098 (3) | 0.994 (3) | 0.072* | |
| O3 | 0.0066 (2) | 0.7675 (2) | 0.58671 (17) | 0.0400 (3) | |
| H3 | 0.002 (4) | 0.785 (4) | 0.491 (2) | 0.053 (7)* | |
| N1 | 0.4459 (2) | 0.6297 (2) | 0.74305 (16) | 0.0264 (3) | |
| C1 | 0.5945 (2) | 0.6740 (2) | 0.60554 (19) | 0.0267 (3) | |
| H1A | 0.7280 | 0.6483 | 0.6138 | 0.032* | |
| C2 | 0.5560 (2) | 0.7568 (2) | 0.45137 (18) | 0.0245 (3) | |
| C3 | 0.3595 (3) | 0.7885 (2) | 0.43778 (19) | 0.0263 (3) | |
| H3A | 0.3310 | 0.8402 | 0.3354 | 0.032* | |
| C4 | 0.2061 (2) | 0.7415 (2) | 0.5802 (2) | 0.0270 (3) | |
| C5 | 0.2549 (2) | 0.6655 (3) | 0.73035 (19) | 0.0276 (3) | |
| H5A | 0.1507 | 0.6383 | 0.8260 | 0.033* | |
| C6 | 0.7273 (3) | 0.8123 (2) | 0.30121 (19) | 0.0288 (3) |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Cd1 | 0.02499 (9) | 0.03841 (10) | 0.01604 (8) | −0.01493 (7) | −0.00552 (6) | −0.00099 (6) |
| O1 | 0.0313 (6) | 0.0688 (9) | 0.0266 (6) | −0.0259 (6) | −0.0010 (5) | −0.0044 (6) |
| O1W | 0.0589 (9) | 0.0749 (10) | 0.0276 (6) | −0.0484 (8) | −0.0017 (6) | −0.0091 (7) |
| O2 | 0.0587 (8) | 0.0592 (8) | 0.0199 (6) | −0.0385 (7) | −0.0088 (5) | 0.0028 (5) |
| O2W | 0.0368 (7) | 0.0424 (7) | 0.0347 (7) | −0.0075 (6) | 0.0072 (6) | 0.0013 (6) |
| O3 | 0.0285 (6) | 0.0620 (8) | 0.0326 (7) | −0.0220 (6) | −0.0135 (5) | 0.0007 (6) |
| N1 | 0.0258 (6) | 0.0362 (7) | 0.0187 (6) | −0.0141 (5) | −0.0068 (5) | −0.0018 (5) |
| C1 | 0.0252 (7) | 0.0376 (8) | 0.0208 (7) | −0.0155 (6) | −0.0064 (6) | −0.0037 (6) |
| C2 | 0.0278 (7) | 0.0271 (7) | 0.0195 (7) | −0.0128 (6) | −0.0046 (6) | −0.0033 (5) |
| C3 | 0.0312 (7) | 0.0288 (7) | 0.0207 (7) | −0.0120 (6) | −0.0109 (6) | −0.0005 (5) |
| C4 | 0.0249 (7) | 0.0305 (7) | 0.0281 (7) | −0.0112 (6) | −0.0107 (6) | −0.0026 (6) |
| C5 | 0.0254 (7) | 0.0358 (8) | 0.0219 (7) | −0.0143 (6) | −0.0053 (6) | −0.0023 (6) |
| C6 | 0.0340 (8) | 0.0319 (8) | 0.0206 (7) | −0.0166 (6) | −0.0025 (6) | −0.0038 (6) |
| Cd1—O2W | 2.2830 (14) | O3—C4 | 1.3543 (19) |
| Cd1—O2Wi | 2.2830 (14) | O3—H3 | 0.830 (17) |
| Cd1—N1i | 2.2831 (13) | N1—C5 | 1.335 (2) |
| Cd1—N1 | 2.2831 (13) | N1—C1 | 1.3411 (19) |
| Cd1—O1W | 2.3291 (13) | C1—C2 | 1.387 (2) |
| Cd1—O1Wi | 2.3291 (13) | C1—H1A | 0.9300 |
| O1—C6 | 1.255 (2) | C2—C3 | 1.385 (2) |
| O1W—H1WA | 0.809 (17) | C2—C6 | 1.517 (2) |
| O1W—H1WB | 0.794 (17) | C3—C4 | 1.389 (2) |
| O2—C6 | 1.244 (2) | C3—H3A | 0.9300 |
| O2W—H2WA | 0.823 (17) | C4—C5 | 1.386 (2) |
| O2W—H2WB | 0.822 (17) | C5—H5A | 0.9300 |
| O2W—Cd1—O2Wi | 180.0 | C5—N1—C1 | 118.64 (13) |
| O2W—Cd1—N1i | 87.79 (5) | C5—N1—Cd1 | 117.86 (10) |
| O2Wi—Cd1—N1i | 92.21 (5) | C1—N1—Cd1 | 123.49 (10) |
| O2W—Cd1—N1 | 92.21 (5) | N1—C1—C2 | 122.29 (14) |
| O2Wi—Cd1—N1 | 87.79 (5) | N1—C1—H1A | 118.9 |
| N1i—Cd1—N1 | 180.000 (1) | C2—C1—H1A | 118.9 |
| O2W—Cd1—O1W | 85.72 (6) | C3—C2—C1 | 118.97 (14) |
| O2Wi—Cd1—O1W | 94.28 (6) | C3—C2—C6 | 121.06 (14) |
| N1i—Cd1—O1W | 90.57 (5) | C1—C2—C6 | 119.96 (14) |
| N1—Cd1—O1W | 89.43 (5) | C2—C3—C4 | 118.68 (14) |
| O2W—Cd1—O1Wi | 94.28 (6) | C2—C3—H3A | 120.7 |
| O2Wi—Cd1—O1Wi | 85.72 (6) | C4—C3—H3A | 120.7 |
| N1i—Cd1—O1Wi | 89.43 (5) | O3—C4—C5 | 115.78 (14) |
| N1—Cd1—O1Wi | 90.57 (5) | O3—C4—C3 | 125.40 (14) |
| O1W—Cd1—O1Wi | 180.0 | C5—C4—C3 | 118.81 (14) |
| Cd1—O1W—H1WA | 117 (2) | N1—C5—C4 | 122.55 (14) |
| Cd1—O1W—H1WB | 127 (2) | N1—C5—H5A | 118.7 |
| H1WA—O1W—H1WB | 110 (2) | C4—C5—H5A | 118.7 |
| Cd1—O2W—H2WA | 131 (2) | O2—C6—O1 | 125.02 (15) |
| Cd1—O2W—H2WB | 117 (2) | O2—C6—C2 | 117.26 (15) |
| H2WA—O2W—H2WB | 105 (2) | O1—C6—C2 | 117.71 (14) |
| C4—O3—H3 | 108.2 (19) | ||
| O2W—Cd1—N1—C5 | 119.15 (12) | C1—C2—C3—C4 | 1.8 (2) |
| O2Wi—Cd1—N1—C5 | −60.85 (12) | C6—C2—C3—C4 | −177.83 (14) |
| O1W—Cd1—N1—C5 | 33.45 (13) | C2—C3—C4—O3 | 178.81 (15) |
| O1Wi—Cd1—N1—C5 | −146.55 (13) | C2—C3—C4—C5 | 0.2 (2) |
| O2W—Cd1—N1—C1 | −61.78 (13) | C1—N1—C5—C4 | 1.7 (2) |
| O2Wi—Cd1—N1—C1 | 118.22 (13) | Cd1—N1—C5—C4 | −179.16 (12) |
| O1W—Cd1—N1—C1 | −147.47 (13) | O3—C4—C5—N1 | 179.22 (15) |
| O1Wi—Cd1—N1—C1 | 32.53 (13) | C3—C4—C5—N1 | −2.1 (2) |
| C5—N1—C1—C2 | 0.5 (2) | C3—C2—C6—O2 | −5.8 (2) |
| Cd1—N1—C1—C2 | −178.62 (11) | C1—C2—C6—O2 | 174.61 (15) |
| N1—C1—C2—C3 | −2.2 (2) | C3—C2—C6—O1 | 173.06 (16) |
| N1—C1—C2—C6 | 177.42 (14) | C1—C2—C6—O1 | −6.6 (2) |
| Symmetry codes: (i) −x+1, −y+1, −z+2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1W—H1WA···O2ii | 0.81 (2) | 1.94 (2) | 2.742 (2) | 171 (3) |
| O1W—H1WB···O3iii | 0.79 (2) | 2.20 (2) | 2.9728 (19) | 164 (3) |
| O2W—H2WA···O1iv | 0.82 (2) | 1.87 (2) | 2.6556 (18) | 160 (3) |
| O2W—H2WB···O2v | 0.82 (2) | 1.93 (2) | 2.7349 (19) | 165 (3) |
| O3—H3···O1vi | 0.83 (2) | 1.88 (2) | 2.6637 (19) | 157 (3) |
| Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+2; (iv) −x+2, −y+1, −z+1; (v) x, y−1, z+1; (vi) x−1, y, z. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1W—H1WA···O2i | 0.81 (2) | 1.94 (2) | 2.742 (2) | 171 (3) |
| O1W—H1WB···O3ii | 0.79 (2) | 2.20 (2) | 2.9728 (19) | 164 (3) |
| O2W—H2WA···O1iii | 0.82 (2) | 1.87 (2) | 2.6556 (18) | 160 (3) |
| O2W—H2WB···O2iv | 0.82 (2) | 1.93 (2) | 2.7349 (19) | 165 (3) |
| O3—H3···O1v | 0.83 (2) | 1.88 (2) | 2.6637 (19) | 157 (3) |
| Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+2; (iii) −x+2, −y+1, −z+1; (iv) x, y−1, z+1; (v) x−1, y, z. |
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There is intense research on the synthesis of the cadmium metal compounds for their interesting photoluminescent properties. A large number of these compounds have been synthesized (He et al., 2008; Zora et al., 2006; Kang et al.,2007; Zhang et al., 2006).
As illustrated in Fig. 1, the Cd(II) atom is coordinated by two nitrogen atoms from two 5-hydroxynicotinic acid ligands and four water molecules. Four coordinated atoms of O1W, O2W, O1WA and O2WA constitute the base of the octahedral, whereas N1 and N1A atoms occupy the apical position. The intermolecular hydrogen bonds play an important role in the formation of the three-dimensional network. As shown in Fig. 2, the intermolecular O—H···O hydrogen bonds link the neighboring molecules to a three-dimensional network.