Home Physical Sciences Crystal structure of catena-poly[diaqua(μ3-pyrazine-2,3-dicarboxylato-κ4O,N:O′:O′′)zinc(II)] 1.25 hydrate, C6H8.5N2O7.25Zn
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Crystal structure of catena-poly[diaqua(μ3-pyrazine-2,3-dicarboxylato-κ4O,N:O′:O′′)zinc(II)] 1.25 hydrate, C6H8.5N2O7.25Zn

  • Deng Linxin , Li Song and Li Xingyu EMAIL logo
Published/Copyright: December 28, 2017

Abstract

C6H8.5N2O7.25Zn, triclinic, P1̅ (no. 2), a = 6.4463(5) Å, b = 8.4180(7) Å, c = 9.8370(8) Å, α = 66.130(1)°, β = 79.537(1)°, γ = 81.153(2)°, V = 478.11(7) Å3, Z = 2, Rgt(F) = 0.0292, wRref(F2) = 0.0782, T = 298 K.

CCDC no.:: 912097

A part of the polymeric title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Block, colourless
Size:0.39 × 0.21 × 0.17 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:2.6 mm−1
Diffractometer, scan mode:Bruker SMART, φ and ω-scans
2θmax, completeness:50°, >98%
N(hkl)measured, N(hkl)unique, Rint:2410,1656, 0.021
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1486
N(param)refined:154
Programs:Bruker programs [1], SHELX [2], DIAMOND [3], PLATON [4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Zn10.28894(5)0.78200(4)0.20990(3)0.02068(14)
N10.3025(4)0.5054(3)0.3352(3)0.0195(5)
N20.2821(4)0.1631(3)0.5368(3)0.0227(5)
O10.2511(3)1.0530(2)0.1242(2)0.0243(5)
H1C0.27881.10370.02960.029*
H1D0.12741.09080.15150.029*
O20.3660(3)0.7615(3)0.0012(2)0.0301(5)
H2C0.47800.8143−0.03370.036*
H2D0.29410.7865−0.07030.036*
O30.2344(3)0.7712(2)0.4266(2)0.0232(5)
O40.1821(4)0.5881(3)0.6664(2)0.0279(5)
O50.0316(3)0.2140(3)0.8200(2)0.0249(5)
O60.3757(3)0.1995(3)0.8206(2)0.0254(5)
O70.8652(3)0.1530(3)0.2348(2)0.0307(5)
H7C0.84850.23290.26880.037*
H7D0.82060.06070.30460.037*
O8a0.074(3)0.478(3)1.005(2)0.094(6)
H8Ca0.09550.49210.91290.112*
H8Da0.01630.38341.05550.112*
C10.2228(4)0.6221(4)0.5302(3)0.0186(6)
C20.2156(4)0.2362(3)0.7541(3)0.0181(6)
C30.2607(4)0.4669(4)0.4834(3)0.0182(6)
C40.2537(4)0.2948(3)0.5846(3)0.0177(6)
C50.3209(5)0.2041(4)0.3893(3)0.0281(7)
H50.33970.11550.35360.034*
C60.3341(5)0.3749(4)0.2878(3)0.0262(7)
H60.36520.39880.18570.031*
  1. aOccupancy: 0.25.

Source of material

A mixture of pyrazine-2,3-dicarboxylic acid (0.1 mmol), Zn(NO3)2⋅H2O(0.1 mmol), H2O (10 mL) and methanol 2 mL was stirred for 20 min and then sealed in a 25 mL Teflon-lined stainless steel autoclave and heated at 170° for 72 h. White block crystals of the title compound were obtained, which were washed with water and dried in air with a 72% yield.

Experimental details

The H atoms of the solvent water molecule were located from the difference Fourier map and then allowed to ride on their parent O atom in the final cycles of refinement with d(O—H) = 0.850 Å and Uiso(H) = 1.5 Ueq(O).

Discussion

In this paper, we choose the pyrazine-2,3-dicarboxylate (PDC) a ligands to synthesized a new compound. This compound crystallizes in the P-1 space group, and possesses an extended one-dimensional framework. Each Zn(II) is coordinated by five O and one N atoms. Two oxygen atoms come from two individual H2O molecules, one O atom and the N atom come from one PDC ligand, the remaining two O atoms are from two adjacent PDC ligands, as shown in the figure. The Zn2+, 2 H2O and 1 PDC ligand form a plane, two Zn—O bonds spread out combining the other two planes and extending to a one-dimensional chain.

The analogous monohydrate of the title compound is known for decades [5]. The structure is similar to the structure reported in this manuscript. Results indicate that especially the number of water molecules is not the same.

Acknowledgements

We acknowledge support for the publication fee by the Scientific Research Foundation of Yunnan Provincial Education Department no. 2017zzx299 and Innovation Research Fund of Criminal Science and Technology Key Lab of Yunnan Province no. YJXK117001.

References

1. Bruker: APEX2, SAINT and SADABS. Brucker AXS Inc., Madison, WI, USA (2009).Search in Google Scholar

2. Sheldrick, G. M.: Crystal structure refinement with SHELXL. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Search in Google Scholar PubMed PubMed Central

3. Brandenburg, K.: DIAMOND. Visual Crystal Structure Information System. Ver. 4.0. Crystal Impact, Bonn, Germany (2015).Search in Google Scholar

4. Spek, A. L.: Single-crystal structure validation with the program PLATON. J. Appl. Crystallogr. 36 (2003) 7–13.10.1107/S0021889802022112Search in Google Scholar

5. Richard, P.; Tran Qui, D.; Bertaut, E. F.: Structure cristalline du polychelate Zn-2,3-PYD⋅3H2O. Acta Crystallogr. B30 (1974) 628–633.10.1107/S0567740874003438Search in Google Scholar

Received: 2017-8-29
Accepted: 2017-11-25
Published Online: 2017-12-28
Published in Print: 2018-1-26

©2018 Deng Linxin et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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