Home Crystal structure of di-μ2-aqua-tetraaqua-bis(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)disodium(I) C18H24N6Na2O10
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Crystal structure of di-μ2-aqua-tetraaqua-bis(4-(1H-1,2,4-triazol-1-yl)benzoato-κN)disodium(I) C18H24N6Na2O10

  • Xiaonan Gao EMAIL logo , Cun-Lan Zhang and Ai-Yun Fu
Published/Copyright: August 1, 2018

Abstract

C18H24N6Na2O10, triclinic, P1̄, a = 6.223(2) Å, b = 7.385(2) Å, c = 14.295(4) Å, α = 75.491(6)°, β = 77.953(6)°, γ = 70.523(6)°, V = 593.9(3) Å3, Z = 1, Rgt(F) = 0.0517, wRref(F2) = 0.1533, T = 296(2) K.

CCDC no.: 1855536

A part of the 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, colorless
Size:0.2 × 0.2 × 0.2 mm
Wavelength:Mo Kα radiation (λ = 0.71073 Å)
μ:0.151 mm−1
Diffractometer, scan mode:Bruker APEX-II CCD, Φ and ω-scans
θmax, completeness:28.8°, >99%
N(hkl)measured, N(hkl)unique, Rint:4678, 3075, 0.0253
Criterion for Iobs, N(hkl)gt:Iobs > 2σ(Iobs), 1837
N(param)refined:173
Programs:Bruker programs [1], SHELX [2], [3], [4]
Table 2:

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

AtomxyzUiso*/Ueq
Na10.32484(14)0.71525(15)0.94416(6)0.0573(3)
O10.7263(9)0.822(4)0.1605(3)0.070(3)
O1A0.736(3)0.733(8)0.1628(14)0.045(6)
N10.3680(3)0.7611(2)0.61720(11)0.0380(4)
C10.8401(4)0.7252(4)0.23146(15)0.0465(5)
O21.0516(3)0.6408(2)0.22396(11)0.0521(4)
C20.7111(3)0.7384(3)0.33250(13)0.0377(5)
N20.1350(3)0.8255(3)0.63609(13)0.0523(5)
O3−0.0731(2)0.8101(2)0.97557(10)0.0432(4)
H3A−0.1401180.7950451.0343050.052
H3B−0.1667690.9191380.9549860.052
C30.4739(4)0.7912(4)0.35125(16)0.0608(7)
H30.3892190.8215220.2999840.073
N30.2907(4)0.7324(3)0.77516(13)0.0581(6)
O50.7205(2)0.5765(2)0.92465(11)0.0509(4)
H5A0.8170560.5183820.8820990.061
H5B0.7999860.6378380.9369530.061
C50.4833(3)0.7568(3)0.52000(13)0.0340(4)
O40.3425(3)0.8182(2)1.09180(11)0.0488(4)
H4A0.4456780.8111791.1229650.059
H4B0.2622660.7595021.1354560.059
C40.3594(4)0.7997(4)0.44502(16)0.0552(6)
H40.1995760.8344760.4566180.066
C70.8308(4)0.7001(4)0.40855(15)0.0495(6)
H70.9906100.6651920.3972090.059
C60.7191(4)0.7120(4)0.50228(16)0.0542(6)
H60.8029470.6899080.5529220.065
C80.4557(4)0.7055(4)0.70096(15)0.0543(6)
H80.6118950.6547780.7062540.065
C90.1001(4)0.8050(4)0.73174(16)0.0538(6)
H9−0.0465060.8386910.7667120.065

Source of material

The ligand, 4-(1H-1,2,4-triazol-1-yl)benzoic acid, was purchased from alfa aesar company. Sodium hydrate (0.004 g, 0.1 mmol), Hbpt24 (0.0189 g, 0.1 mmol) and distilled water (20 mL) were placed in a 20.0 mL Teflon-lined stainless steel autoclave. It was heated at 383 K for 2 days. After cooling to room temperature, colourless block crystals of the title complex were obtained.

Experimental details

The carbon H-atoms were placed in calculated positions (C—Hphenyl or triazolyl = 0.93 Å) using a riding model (AFIX 43 or AFIX 137 option of the SHELX program [11], [12], [13], and were included with Uiso(H) = 1.2Ueq(C). The water H-atoms were placed in calculated positions (O⋯H = 0.85 Å), and were included with Uiso(H) = 1.2Ueq(O).

Comment

The exploration of alkali-metal complexes has attracted significant interest, due to its potential application in catalysts [5], [6], [7], [8]. The exo-multidentate compounds are often employed as ligands to produce polymeric networks due to their rich coordination sites and various coordination modes [9], [10], [11], [12]. Recently, our group studied the reactions of 4-(1H-1,2,4-triazol-1-yl)benzoic acid (HL) with silver, obtaining a series of coordination compounds [13], [14]. As a follow up study, we report the title complex.

The title complex consists of two Na(I) ion, two L ligands and six coordinated water molecules. Each Na(I) is five-coordinated by one N atom from L and four O atoms from four water molecules. The Na–N distance is 2.437(2) Å and Na–O bond lengths are in the range of 2.3158(17) − 2.530(2) Å. The coordination environment is a distorted trigonal bipyramid, since the N—Na—O and N—Na—O bond angles in the trigonal plane are in the range of 78.13 − 160.18°. The water O5 atom acts as a μ2-bridge linking the Na(I) centers into a the dinuclear complex. Intermolecular hydrogen bonds link dinuclear complexes into a three-dimensional supramolecular framework.

Acknowledgements

We are grateful for financial support from the NSF of China (Grants 21671031, 21705098); Shandong Provincial Science and Technology Department Project (Grants ZR201702200428); Shandong Provincial Higher Education Research Project(J17KA116)).

References

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Received: 2018-03-17
Accepted: 2018-07-12
Published Online: 2018-08-01
Published in Print: 2018-11-27

©2018 Xiaonan Gao 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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  1. Cover and Frontmatter
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