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.
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.
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] |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).
| Atom | x | y | z | Uiso*/Ueq |
|---|---|---|---|---|
| Na1 | 0.32484(14) | 0.71525(15) | 0.94416(6) | 0.0573(3) |
| O1 | 0.7263(9) | 0.822(4) | 0.1605(3) | 0.070(3) |
| O1A | 0.736(3) | 0.733(8) | 0.1628(14) | 0.045(6) |
| N1 | 0.3680(3) | 0.7611(2) | 0.61720(11) | 0.0380(4) |
| C1 | 0.8401(4) | 0.7252(4) | 0.23146(15) | 0.0465(5) |
| O2 | 1.0516(3) | 0.6408(2) | 0.22396(11) | 0.0521(4) |
| C2 | 0.7111(3) | 0.7384(3) | 0.33250(13) | 0.0377(5) |
| N2 | 0.1350(3) | 0.8255(3) | 0.63609(13) | 0.0523(5) |
| O3 | −0.0731(2) | 0.8101(2) | 0.97557(10) | 0.0432(4) |
| H3A | −0.140118 | 0.795045 | 1.034305 | 0.052 |
| H3B | −0.166769 | 0.919138 | 0.954986 | 0.052 |
| C3 | 0.4739(4) | 0.7912(4) | 0.35125(16) | 0.0608(7) |
| H3 | 0.389219 | 0.821522 | 0.299984 | 0.073 |
| N3 | 0.2907(4) | 0.7324(3) | 0.77516(13) | 0.0581(6) |
| O5 | 0.7205(2) | 0.5765(2) | 0.92465(11) | 0.0509(4) |
| H5A | 0.817056 | 0.518382 | 0.882099 | 0.061 |
| H5B | 0.799986 | 0.637838 | 0.936953 | 0.061 |
| C5 | 0.4833(3) | 0.7568(3) | 0.52000(13) | 0.0340(4) |
| O4 | 0.3425(3) | 0.8182(2) | 1.09180(11) | 0.0488(4) |
| H4A | 0.445678 | 0.811179 | 1.122965 | 0.059 |
| H4B | 0.262266 | 0.759502 | 1.135456 | 0.059 |
| C4 | 0.3594(4) | 0.7997(4) | 0.44502(16) | 0.0552(6) |
| H4 | 0.199576 | 0.834476 | 0.456618 | 0.066 |
| C7 | 0.8308(4) | 0.7001(4) | 0.40855(15) | 0.0495(6) |
| H7 | 0.990610 | 0.665192 | 0.397209 | 0.059 |
| C6 | 0.7191(4) | 0.7120(4) | 0.50228(16) | 0.0542(6) |
| H6 | 0.802947 | 0.689908 | 0.552922 | 0.065 |
| C8 | 0.4557(4) | 0.7055(4) | 0.70096(15) | 0.0543(6) |
| H8 | 0.611895 | 0.654778 | 0.706254 | 0.065 |
| C9 | 0.1001(4) | 0.8050(4) | 0.73174(16) | 0.0538(6) |
| H9 | −0.046506 | 0.838691 | 0.766712 | 0.065 |
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)).
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©2018 Xiaonan Gao et al., published by De Gruyter, Berlin/Boston
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