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metal-organic compounds
Diaquabis(2-oxo-2H-chromene-3-carboxylato)zinc(II)
aCollege of Environmental and Energy Engineering, Beijing University of Technology, Beijing 100124, People's Republic of China
*Correspondence e-mail: xieyabo@bjut.edu.cn
In the title compound, [Zn(C10H5O4)2(H2O)2], the ZnII atom lies on a crystallographic inversion center and is six-coordinated by two O atoms from water molecules in the axial positions and four O atoms from two deprotonated coumarin-3-carboxylate ligands in the equatorial plane, forming a slightly distorted octahedral coordination geometry. O—H⋯O hydrogen-bonding interactions involving the water molecules form infinite chains parallel to [010].
Related literature
For related structures, see: Chu et al. (2010). For hydrogen-bond motifs, see: Bernstein et al. (1995
); Etter (1990
).
Experimental
Crystal data
|
Refinement
|
|
Data collection: APEX2 (Bruker, 2005); cell SAINT (Bruker, 2005
); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008
); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008
); molecular graphics: ORTEPIII (Burnett & Johnson, 1996
), ORTEP-3 for Windows (Farrugia, 1997
) and PLATON (Spek, 2009
); software used to prepare material for publication: SHELXTL (Sheldrick, 2008
).
Supporting information
https://doi.org/10.1107/S1600536810050865/dn2633sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810050865/dn2633Isup2.hkl
The title complex was synthesized by carefully layering a solution of ZnSO4.7H2O (28.8 mg, 0.1 mmol) in ethanol solution (10 ml) on top of a solution of coumarin-3-carboxylic acid (19.0 mg, 0.1 mmol) and LiOH (8.4 mg, 0.2 mmol) in H2O (10 ml) in a test-tube. After about one month at room temperature, colorless block-shaped single crystals suitable for X-ray investigation appeared at the boundary between ethanol solution and water with a yield of 27%.
The H atoms were placed geometrically (C—H = 0.93 Å) and treated as riding with Uiso(H) = 1.2eq(C) . H atoms of water molecule were located in difference Fourier maps and included in the subsequent
using restraints (O-H= 0.85 (1)Å and H···H= 1.40 (2)Å) with Uiso(H) = 1.5Ueq(O). In the last cycle of they were treated as riding on their parent O atom.In the past decades, numerous papers dealing with mononuclear zinc complexes have been published (Chu et al. 2010). Herein, we report the synthesis and
of a new mononuclear zinc complex.In the title compound, [Zn(C10H5O4)2(H2O)2], each ZnII atom lies on a crystallographic inversion center and is six-coordinated by two O atoms from water molecules in the axial positions and four O atoms from two deprotonated coumarin-3-carboxylic acid ligands in the equatorial plane, forming an octahedral coordination geometry (Fig. 1). O—H···O hydrogen bonds involving the water molecules build up chain parllel to the [0 1 0] axis (Table 1, Fig. 2). The O-H···O interactions results in the formation of R42(8) rings (Etter, 1990; Bernstein et al., 1995).
For related structures, see: Chu et al. (2010). For hydrogen-bond motifs, see: Bernstein et al. (1995); Etter (1990).
Data collection: APEX2 (Bruker, 2005); cell
SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).[Zn(C10H5O4)2(H2O)2] | Z = 1 |
Mr = 479.70 | F(000) = 244 |
Triclinic, P1 | Dx = 1.860 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.6113 (13) Å | Cell parameters from 2271 reflections |
b = 6.8404 (14) Å | θ = 3.4–28.4° |
c = 10.392 (2) Å | µ = 1.50 mm−1 |
α = 85.64 (3)° | T = 293 K |
β = 89.47 (3)° | Block, colourless |
γ = 66.09 (3)° | 0.2 × 0.2 × 0.2 mm |
V = 428.27 (18) Å3 |
Bruker APEXII CCD diffractometer | 1808 independent reflections |
Radiation source: fine-focus sealed tube | 1793 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.013 |
φ and ω scans | θmax = 27.1°, θmin = 3.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2008) | h = −8→8 |
Tmin = 0.741, Tmax = 0.748 | k = −8→8 |
2642 measured reflections | l = 0→13 |
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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0216P)2 + 0.2757P] where P = (Fo2 + 2Fc2)/3 |
1808 reflections | (Δ/σ)max < 0.001 |
142 parameters | Δρmax = 0.42 e Å−3 |
0 restraints | Δρmin = −0.28 e Å−3 |
[Zn(C10H5O4)2(H2O)2] | γ = 66.09 (3)° |
Mr = 479.70 | V = 428.27 (18) Å3 |
Triclinic, P1 | Z = 1 |
a = 6.6113 (13) Å | Mo Kα radiation |
b = 6.8404 (14) Å | µ = 1.50 mm−1 |
c = 10.392 (2) Å | T = 293 K |
α = 85.64 (3)° | 0.2 × 0.2 × 0.2 mm |
β = 89.47 (3)° |
Bruker APEXII CCD diffractometer | 1808 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2008) | 1793 reflections with I > 2σ(I) |
Tmin = 0.741, Tmax = 0.748 | Rint = 0.013 |
2642 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 0 restraints |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.42 e Å−3 |
1808 reflections | Δρmin = −0.28 e Å−3 |
142 parameters |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 | ||
Zn1 | 0.5000 | 0.5000 | 0.5000 | 0.01047 (10) | |
O1 | 0.30343 (17) | 0.68964 (17) | 0.87151 (10) | 0.0127 (2) | |
O1W | 0.49536 (17) | 0.22209 (17) | 0.59641 (10) | 0.0133 (2) | |
H1 | 0.3972 | 0.1951 | 0.5649 | 0.020* | |
H2 | 0.6183 | 0.1022 | 0.5763 | 0.020* | |
O2 | 0.45061 (18) | 0.64366 (18) | 0.68157 (10) | 0.0141 (2) | |
O3 | −0.17320 (17) | 0.86870 (17) | 0.50573 (10) | 0.0134 (2) | |
O4 | 0.16868 (17) | 0.63230 (18) | 0.47583 (10) | 0.0132 (2) | |
C1 | −0.2479 (3) | 0.7880 (2) | 0.99672 (15) | 0.0146 (3) | |
H1A | −0.3880 | 0.8073 | 0.9679 | 0.018* | |
C2 | −0.2071 (3) | 0.7889 (3) | 1.12660 (15) | 0.0168 (3) | |
H3A | −0.3203 | 0.8111 | 1.1850 | 0.020* | |
C3 | 0.0042 (3) | 0.7564 (2) | 1.17064 (15) | 0.0161 (3) | |
H2A | 0.0305 | 0.7567 | 1.2584 | 0.019* | |
C4 | 0.1753 (3) | 0.7237 (2) | 1.08507 (15) | 0.0148 (3) | |
H11A | 0.3160 | 0.7015 | 1.1143 | 0.018* | |
C5 | 0.1306 (2) | 0.7250 (2) | 0.95493 (14) | 0.0119 (3) | |
C6 | −0.0780 (2) | 0.7579 (2) | 0.90792 (14) | 0.0122 (3) | |
C7 | −0.1088 (2) | 0.7641 (2) | 0.77180 (14) | 0.0120 (3) | |
H7A | −0.2480 | 0.7893 | 0.7385 | 0.014* | |
C8 | 0.0600 (2) | 0.7342 (2) | 0.68973 (14) | 0.0109 (3) | |
C9 | 0.2798 (2) | 0.6861 (2) | 0.74172 (14) | 0.0113 (3) | |
C10 | 0.0171 (2) | 0.7468 (2) | 0.54635 (14) | 0.0105 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.00736 (13) | 0.01189 (14) | 0.01013 (13) | −0.00175 (9) | 0.00122 (8) | −0.00152 (9) |
O1 | 0.0106 (5) | 0.0164 (5) | 0.0101 (5) | −0.0041 (4) | 0.0009 (4) | −0.0028 (4) |
O1W | 0.0105 (5) | 0.0139 (5) | 0.0143 (5) | −0.0036 (4) | 0.0005 (4) | −0.0016 (4) |
O2 | 0.0099 (5) | 0.0185 (5) | 0.0133 (5) | −0.0048 (4) | 0.0021 (4) | −0.0041 (4) |
O3 | 0.0093 (5) | 0.0143 (5) | 0.0138 (5) | −0.0018 (4) | −0.0009 (4) | −0.0012 (4) |
O4 | 0.0091 (5) | 0.0168 (5) | 0.0116 (5) | −0.0026 (4) | 0.0013 (4) | −0.0032 (4) |
C1 | 0.0139 (7) | 0.0135 (7) | 0.0155 (7) | −0.0046 (6) | 0.0028 (6) | −0.0014 (6) |
C2 | 0.0204 (8) | 0.0135 (7) | 0.0147 (7) | −0.0051 (6) | 0.0069 (6) | −0.0015 (6) |
C3 | 0.0247 (8) | 0.0122 (7) | 0.0098 (7) | −0.0059 (6) | 0.0016 (6) | −0.0012 (5) |
C4 | 0.0166 (7) | 0.0133 (7) | 0.0129 (7) | −0.0043 (6) | −0.0009 (6) | −0.0014 (6) |
C5 | 0.0129 (7) | 0.0092 (6) | 0.0117 (7) | −0.0024 (5) | 0.0034 (5) | −0.0017 (5) |
C6 | 0.0133 (7) | 0.0095 (6) | 0.0129 (7) | −0.0036 (5) | 0.0020 (5) | −0.0008 (5) |
C7 | 0.0110 (7) | 0.0108 (7) | 0.0135 (7) | −0.0037 (5) | −0.0002 (5) | −0.0008 (5) |
C8 | 0.0105 (7) | 0.0100 (6) | 0.0113 (6) | −0.0032 (5) | 0.0004 (5) | −0.0016 (5) |
C9 | 0.0123 (7) | 0.0096 (6) | 0.0105 (6) | −0.0026 (5) | 0.0004 (5) | −0.0015 (5) |
C10 | 0.0097 (6) | 0.0108 (6) | 0.0120 (7) | −0.0051 (5) | 0.0006 (5) | −0.0009 (5) |
Zn1—O4 | 2.0122 (12) | C1—C6 | 1.406 (2) |
Zn1—O4i | 2.0122 (12) | C1—H1A | 0.9300 |
Zn1—O1Wi | 2.0918 (12) | C2—C3 | 1.398 (2) |
Zn1—O1W | 2.0918 (12) | C2—H3A | 0.9300 |
Zn1—O2 | 2.1548 (12) | C3—C4 | 1.388 (2) |
Zn1—O2i | 2.1548 (12) | C3—H2A | 0.9300 |
O1—C9 | 1.3623 (18) | C4—C5 | 1.386 (2) |
O1—C5 | 1.3801 (18) | C4—H11A | 0.9300 |
O1W—H1 | 0.8200 | C5—C6 | 1.391 (2) |
O1W—H2 | 0.9269 | C6—C7 | 1.426 (2) |
O2—C9 | 1.2241 (18) | C7—C8 | 1.356 (2) |
O3—C10 | 1.2501 (19) | C7—H7A | 0.9300 |
O4—C10 | 1.2617 (19) | C8—C9 | 1.454 (2) |
C1—C2 | 1.380 (2) | C8—C10 | 1.509 (2) |
O4—Zn1—O4i | 180.0 | C3—C2—H3A | 119.9 |
O4—Zn1—O1Wi | 88.05 (5) | C4—C3—C2 | 120.84 (15) |
O4i—Zn1—O1Wi | 91.95 (5) | C4—C3—H2A | 119.6 |
O4—Zn1—O1W | 91.95 (5) | C2—C3—H2A | 119.6 |
O4i—Zn1—O1W | 88.05 (5) | C5—C4—C3 | 118.17 (15) |
O1Wi—Zn1—O1W | 180.00 (3) | C5—C4—H11A | 120.9 |
O4—Zn1—O2 | 87.20 (5) | C3—C4—H11A | 120.9 |
O4i—Zn1—O2 | 92.80 (5) | O1—C5—C4 | 117.34 (14) |
O1Wi—Zn1—O2 | 90.89 (5) | O1—C5—C6 | 120.25 (13) |
O1W—Zn1—O2 | 89.11 (5) | C4—C5—C6 | 122.41 (14) |
O4—Zn1—O2i | 92.80 (5) | C5—C6—C1 | 118.34 (14) |
O4i—Zn1—O2i | 87.20 (5) | C5—C6—C7 | 118.03 (14) |
O1Wi—Zn1—O2i | 89.11 (5) | C1—C6—C7 | 123.62 (14) |
O1W—Zn1—O2i | 90.89 (5) | C8—C7—C6 | 121.59 (14) |
O2—Zn1—O2i | 180.000 (1) | C8—C7—H7A | 119.2 |
C9—O1—C5 | 122.65 (12) | C6—C7—H7A | 119.2 |
Zn1—O1W—H1 | 109.5 | C7—C8—C9 | 119.36 (14) |
Zn1—O1W—H2 | 110.7 | C7—C8—C10 | 119.39 (13) |
H1—O1W—H3 | 99.9 | C9—C8—C10 | 121.24 (13) |
C9—O2—Zn1 | 122.37 (10) | O2—C9—O1 | 114.78 (13) |
C10—O4—Zn1 | 131.42 (10) | O2—C9—C8 | 127.30 (14) |
C2—C1—C6 | 120.10 (15) | O1—C9—C8 | 117.92 (13) |
C2—C1—H1A | 119.9 | O3—C10—O4 | 124.05 (14) |
C6—C1—H1A | 119.9 | O3—C10—C8 | 116.41 (13) |
C1—C2—C3 | 120.13 (15) | O4—C10—C8 | 119.51 (13) |
C1—C2—H3A | 119.9 |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1···O3ii | 0.82 | 1.88 | 2.6950 (17) | 179 |
O1W—H2···O3iii | 0.93 | 1.83 | 2.7473 (19) | 168 |
Symmetry codes: (ii) −x, −y+1, −z+1; (iii) x+1, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [Zn(C10H5O4)2(H2O)2] |
Mr | 479.70 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 6.6113 (13), 6.8404 (14), 10.392 (2) |
α, β, γ (°) | 85.64 (3), 89.47 (3), 66.09 (3) |
V (Å3) | 428.27 (18) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.50 |
Crystal size (mm) | 0.2 × 0.2 × 0.2 |
Data collection | |
Diffractometer | Bruker APEXII CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2008) |
Tmin, Tmax | 0.741, 0.748 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2642, 1808, 1793 |
Rint | 0.013 |
(sin θ/λ)max (Å−1) | 0.641 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.061, 1.12 |
No. of reflections | 1808 |
No. of parameters | 142 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.42, −0.28 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1···O3i | 0.82 | 1.88 | 2.6950 (17) | 179.4 |
O1W—H2···O3ii | 0.93 | 1.83 | 2.7473 (19) | 167.8 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x+1, y−1, z. |
Acknowledgements
This work was supported by the National Natural Science Foundation of China (No. 21075114), the Science and Technology Development Project of Beijing Education Committee and the Special Environmental Protection Fund for Public Welfare project (201009015).
References
Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555–1573. CrossRef CAS Web of Science Google Scholar
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Google Scholar
Chu, W. J., Yao, H. C., Ma, H. C., He, Y., Fan, Y. T. & Hou, H. W. (2010). J Coord. Chem. 63, 3734–3742. Web of Science CSD CrossRef CAS Google Scholar
Etter, M. C. (1990). Acc. Chem. Res. 23, 120–126. CrossRef CAS Web of Science Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
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In the past decades, numerous papers dealing with mononuclear zinc complexes have been published (Chu et al. 2010). Herein, we report the synthesis and crystal structure of a new mononuclear zinc complex.
In the title compound, [Zn(C10H5O4)2(H2O)2], each ZnII atom lies on a crystallographic inversion center and is six-coordinated by two O atoms from water molecules in the axial positions and four O atoms from two deprotonated coumarin-3-carboxylic acid ligands in the equatorial plane, forming an octahedral coordination geometry (Fig. 1). O—H···O hydrogen bonds involving the water molecules build up chain parllel to the [0 1 0] axis (Table 1, Fig. 2). The O-H···O interactions results in the formation of R42(8) rings (Etter, 1990; Bernstein et al., 1995).