Home Crystal structure of poly[(μ7-4-(3,5-dicarboxylatophenoxy)phthalato)-(1,10-phenanthroline-κ2N,N′)dizinc(II)], C28H14N2O9Zn2
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Crystal structure of poly[(μ7-4-(3,5-dicarboxylatophenoxy)phthalato)-(1,10-phenanthroline-κ2N,N′)dizinc(II)], C28H14N2O9Zn2

  • Tao Sun EMAIL logo and Ke Li
Published/Copyright: August 23, 2019

Abstract

C28H14N2O9Zn2, triclinic, P1̄ (no. 2), a = 9.6870(5) Å, b = 10.1849(9) Å, c = 12.7338(9) Å, α = 95.202(6)°, β = 107.027(5)°, γ = 91.896(5)°, V = 1193.97(14) Å3, Z = 2, Rgt(F) = 0.0516, wRref(F2) = 0.1267, T = 293(2) K.

CCDC no.: 1946294

A part of the 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:Colorless block
Size:0.43 × 0.32 × 0.29 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:2.07 mm−1
Diffractometer, scan mode:SuperNova, ω-scans
θmax, completeness:25.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:25935, 4433, 0.088
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3738
N(param)refined:370
Programs:CrysAlisPRO [1], SHELX [2], [3]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.80005(5)0.87012(5)0.39316(4)0.02366(17)
Zn21.09938(5)0.77784(5)0.61098(4)0.02333(17)
N10.7728(4)0.7336(4)0.2530(3)0.0259(8)
N20.6048(4)0.9252(4)0.2878(3)0.0272(9)
O10.7421(3)0.7299(3)0.4781(3)0.0322(8)
O20.9303(3)0.6692(3)0.6101(3)0.0400(9)
O30.2688(3)0.7182(4)0.5571(3)0.0434(9)
O40.2619(3)0.6486(4)0.7112(3)0.0439(9)
O50.6993(3)0.3809(3)0.8225(2)0.0305(8)
O61.1044(5)−0.0972(4)0.8557(3)0.0592(12)
O71.0988(3)−0.0458(3)0.6881(2)0.0285(7)
O80.7932(3)0.0029(3)0.5239(2)0.0262(7)
O90.9799(3)0.1467(3)0.5430(2)0.0214(6)
C10.8503(5)0.6316(5)0.2414(4)0.0351(12)
H10.92560.61290.30160.042*
C20.8231(6)0.5513(5)0.1420(4)0.0427(13)
H20.87910.48010.13630.051*
C30.7145(6)0.5781(6)0.0542(5)0.0478(14)
H30.69680.5260−0.01270.057*
C40.6271(5)0.6846(5)0.0627(4)0.0364(12)
C50.6614(5)0.7582(5)0.1663(4)0.0276(10)
C60.5069(6)0.7177(6)−0.0238(4)0.0463(14)
H60.48520.6704−0.09320.056*
C70.4241(6)0.8160(6)−0.0073(4)0.0432(14)
H70.34650.8353−0.06560.052*
C80.4526(5)0.8915(5)0.0975(4)0.0338(12)
C90.5707(5)0.8628(4)0.1847(4)0.0266(10)
C100.3677(5)0.9920(5)0.1222(5)0.0429(14)
H100.28911.01650.06720.052*
C110.4002(5)1.0526(5)0.2252(5)0.0438(13)
H110.34311.11850.24140.053*
C120.5185(5)1.0178(5)0.3084(4)0.0369(12)
H120.53801.05990.37950.044*
C130.7976(4)0.6758(4)0.5625(4)0.0240(10)
C140.6968(4)0.6116(4)0.6162(3)0.0212(9)
C150.5552(4)0.6478(4)0.5930(3)0.0226(9)
H150.51970.70380.53890.027*
C160.4666(4)0.6002(4)0.6507(4)0.0225(9)
C170.5149(4)0.5069(4)0.7240(4)0.0238(10)
H170.45330.47090.75930.029*
C180.6546(4)0.4678(4)0.7442(3)0.0207(9)
C190.7474(4)0.5239(4)0.6927(4)0.0251(10)
H190.84340.50200.70990.030*
C200.7935(4)0.2849(4)0.8079(4)0.0233(9)
C210.8803(5)0.2402(5)0.9018(4)0.0282(10)
H210.87960.27770.97100.034*
C220.9689(5)0.1388(4)0.8926(4)0.0260(10)
H221.02640.10670.95600.031*
C230.9732(4)0.0837(4)0.7886(3)0.0222(9)
C240.8864(4)0.1332(4)0.6954(3)0.0208(9)
C250.7932(4)0.2320(4)0.7047(4)0.0226(9)
H250.73160.26180.64190.027*
C261.0673(5)−0.0290(5)0.7809(4)0.0270(10)
C270.8866(4)0.0867(4)0.5799(3)0.0194(9)
C280.3225(4)0.6560(4)0.6383(4)0.0254(10)

Source of material

A mixture of Zn(NO3)2⋅6H2O (0.1 mmol, 0.0297 g), 1,10-phenanthroline (0.1 mmol, 0.0180 g), 4-(3,5-dicarboxyphenoxy)phthalic acid (0.1 mmol, 35 mg), was dissolved in 10 mL H2O. The solution was heated in a 25 mL Teflon-lined autoclave under autogenous pressure at 423 K for 5 days. After cooling to room temperature colourless block crystals were obtained.

Experimental details

All H atoms were positioned geometrically (N—H = 0.86 Å and C—H = 0.93 Å) and refined using a riding model, with Uiso(H) = 1.2Ueq(C, N).

Discussion

Research on metal-organic coordination polymers (CPs) have made considerable progress in the fields of supramolecular chemistry and crystal engineering, owing to their intriguing architectures and applications [4], [5], [6], [7], [8]. Among the various ligands, the organic carboxylate ligands have been proven to be good candidates for the construction of CPs [7], [8]. Moreover, N-donor ligands have been proved to be efficient and typical building blocks in the assembly of CPs [9]. In addition, various aromatic N-donors also play an important role and frequently serve as ancillary ligands to adjust the supramolecular structure of the resulting network.

The asymmetric unit of the title structure contains two Zn(II) metal center, one 4-(3,5-dicarboxylatophenoxy)phthalato and one 1,10-phenanthroline ligand to construct a coordination polymer. The zinc atom 1 is six-coordinated [ZnN2O4], whereas the zinc atom 2 is penta-coordinated [ZnO5] (cf. the figure). The Zn—O bond lengths range from 1.928(7)–2.473(7) Å. The Zn—N bond lengths range from 2.103(9) Å, 2.108(10) Å, respectively. The bond angles of O—Zn—O are in the range of 60.5(3)° to 172.1(3)°. In addition, there is a complex network of intermolecular hydrogen bonds. These interactions result in a three dimensional architecture.

References

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Received: 2019-06-16
Accepted: 2019-08-09
Published Online: 2019-08-23
Published in Print: 2019-11-26

©2019 Tao Sun et al., published by De Gruyter, Berlin/Boston

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

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  64. Crystal structure of (2,2′-bipyridyl)bis(4-bromobenzyl)dibromidotin(IV), C24H20Br4N2Sn
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