Home Physical Sciences Crystal structure of catena-poly[aqua-(μ4-4,4′-(pyridine-3,5-diyl)dibenzoato-κ4O,O′:O′′:O′′′)zinc(II)], C19H13NO5Zn
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Crystal structure of catena-poly[aqua-(μ4-4,4′-(pyridine-3,5-diyl)dibenzoato-κ4O,O′:O′′:O′′′)zinc(II)], C19H13NO5Zn

  • Hui-Long Fang , Li-Zhi Zhu , Biao Li and Jun-Jie Wang ORCID logo EMAIL logo
Published/Copyright: June 17, 2020

Abstract

C19H13NO5Zn, monoclinic, P2/c (no. 13), a = 16.7294(5) Å, b = 6.4985(2) Å, c = 7.1414(2) Å, β = 100.449(3)°, V = 763.51(4) Å3, Z = 2, Rgt(F) = 0.0297, wRref(F2) = 0.0732, T = 293(2) K.

CCDC no.: 2007140

A part of the coordination polymer title structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Colorless needle
Size:0.12 × 0.09 × 0.08 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.64 mm−1
Diffractometer, scan mode:Xcalibur, ω
θmax, completeness:26.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:3268, 1553, 0.026
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1342
N(param)refined:124
Programs:CrysAlisPRO [1], Olex2 [2], SHELX [3], [4]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.5000000.68318(6)0.7500000.02041(14)
O10.45174(9)0.3049(3)0.5156(2)0.0215(4)
O20.39483(10)0.5794(3)0.6225(2)0.0269(4)
O30.5000000.9896(4)0.7500000.0333(7)
H30.484(2)1.067(5)0.659(4)0.049(10)*
N10.000000−0.2777(5)0.2500000.0277(7)
C10.39022(13)0.4068(4)0.5404(3)0.0187(5)
C20.07251(13)0.0450(4)0.3011(3)0.0191(5)
C30.0000000.1528(5)0.2500000.0199(7)
H3A0.0000000.2958840.2500000.024*
C40.22312(14)0.0447(4)0.3250(3)0.0233(5)
H40.218499−0.0822240.2638580.028*
C50.16155(14)0.3390(4)0.4429(3)0.0209(5)
H50.1155570.4106620.4618750.025*
C60.30729(13)0.3198(4)0.4741(3)0.0188(5)
C70.29909(14)0.1301(4)0.3842(3)0.0229(6)
H70.3451020.0596390.3634900.027*
C80.15305(13)0.1467(4)0.3558(3)0.0188(5)
C90.23772(13)0.4249(4)0.5017(3)0.0207(5)
H90.2424920.5533940.5599450.025*
C100.06804(14)−0.1686(4)0.3024(3)0.0238(5)
H100.116031−0.2409750.3428660.029*

Source of material

A mixture of 4,4′-pyridine-3,5-diyldibenzoic acid (0.0319 g, 0.1 mmol), zinc nitrate hexahydrate (0.0298 g, 0.1 mmol) and deionized water (10 mL) was added to a 25 mL Teflon-lined stainless steel autoclave, heated at 393 K in an oven for 72 h, then cooled to room temperature automatically. Colorless block crystals were obtained, filtered, washed with deionized water, and dried in air (yield 35.2%, based on 4,4′-pyridine-3,5-diyldibenzoic acid).

Experimental details

The structure was solved by direct methods with the SHELXS-2018 program. All H-atoms from C atoms were positioned with idealized geometry and refined using a riding model with C—H = 0.93 Å with Uiso(H) = 1.2Ueq(C). The H-atom from O was located with Q peak and refined freely.

Comment

Known as a famous N-heterocyclic aromatic dicarboxylic acid ligand, 4,4′-pyridine-3,5-diyldibenzoic acid and its deprotonated forms have been used to build various metal coordination polymers or metal-organic frameworks. Due to variable coordination numbers (usually 4, 5 or 6) of zinc cations and the flexible coordination modes of 4,4′-pyridine-3,5-diyldibenzoic acid, some examples of 4,4′-pyridine-3,5-diyldibenzoate- or its N-oxide-based Zn(II) complexes have been reported [5], [6], [7], [8], [9]. We herein report a new two-dimensional Zn(II) complex based on this ligand.

As shown in the figure, the asymmetric unit of the title complex consists of a half five-coordinated Zn(II) cation, a half 4,4′-pyridine-3,5-diyldibenzoate and a half coordination water molecule. The N atom from the ligand is not involved in coordination, which is different from similar complexes [5], [6], [7], [8], [9]. The bond lengths of Zn(II)—O in the complex are 1.991, 1.949, and 2.193 Å, respectively, all of which are comparable with similar complexes [5], [6], [7], [8], [9].

Acknowledgements

Key scientific research projects of general colleges and universities in Hunan Province (18A458), Natural Science Foundation of Hunan Province (2016JJ6141), Key R & D and technological innovation projects of science and Technology Bureau of Chenzhou (zdyf201916).

References

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Received: 2020-04-22
Accepted: 2020-06-02
Published Online: 2020-06-17
Published in Print: 2020-08-26

©2020 Hui-Long Fang et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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