| Literature DB >> 29755509 |
Ting Liu1, Rong-Gui Yang1, Guo-Qing Zhong1.
Abstract
The novel 3D edta-linked heterometallic complex [Sb2Er(edta)2(H2O)4]NO3·4H2O (H4edta = ethylenediaminetetraacetic acid) was synthesized and characterized by elemental analyses, single-crystal X-ray diffraction, powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and thermal analysis. The complex crystallizes in the monoclinic system with space group Pm. In the complex, each erbium(III) ion is connected with antimony(III) ions bridging by four carboxylic oxygen atoms, and in each [Sb(edta)]- anion, the antimony(III) ion is hexacoordinated by two nitrogen atoms and four oxygen atoms from the edta4- ions, together with a lone electron pair at the equatorial position. The erbium(III) ion is octacoordinated by four oxygen atoms from four different edta4- ions and four oxygen atoms from the coordinated water molecules. The carboxylate bridges between antimony and erbium atoms form a planar array, parallel to the (1 0 0) plane. There is an obvious weak interaction between antimony atom and oxygen atom of the carboxyl group from the adjacent layer. The degradation of the complex proceeds in several steps and the water molecules and ligands are successively emitted, and the residues of the thermal decomposition are antimonous oxide and erbium(III) oxide. The complex was evaluated for its antimicrobial activities by agar diffusion method, and it has good activities against the test bacterial organisms.Entities:
Year: 2018 PMID: 29755509 PMCID: PMC5884401 DOI: 10.1155/2018/4313197
Source DB: PubMed Journal: Bioinorg Chem Appl Impact factor: 7.778
Figure 1Thermal ellipsoid representation (at 50% probability) of molecular structure unit of the complex. All the H atoms are omitted for clarity. Symmetry codes: A x − 1/2, −y, z − 1/2; B x + 1/2, −y + 1, z − 1/2.
Crystallographic data and structure refinement parameters of the title complex.
| Empirical formula | C20H40N5O27ErSb2 |
| 2.278 |
| Formula weight (g·mol−1) | 1193.33 | Absorption coefficient (mm−1) | 4.043 |
|
| 289(2) |
| 1162 |
| Crystal system | Monoclinic | Crystal size (mm3) | 0.48 × 0.44 × 0.20 |
| Space group |
| Theta range for data collection (°) | 1.84 to 26.00 |
|
| 7.3790(10) | Limiting indices | −9 ≤ |
|
| 22.116(5) | Reflections collected/unique | 7847/6826 [ |
|
| 10.661(3) | Goodness-of-fit (GOF) on | 1.002 |
|
| 90.55(2) | Final |
|
|
| 1739.7(7) |
|
|
|
| 2 | Largest diff. peak and hole (e·Å−3) | 1.767 and −1.676 |
Selected bond lengths (Å) and angles (°) of the title complex.
| Er(1)–O(16)#1 | 2.285(7) | Er(1)–O(10) | 2.290(7) |
| Er(1)–O(2) | 2.290(7) | Er(1)–O(8)#2 | 2.298(7) |
| Er(1)–O(20) | 2.347(9) | Er(1)–O(17) | 2.375(8) |
| Er(1)–O(19) | 2.421(7) | Er(1)–O(18) | 2.432(7) |
| Sb(1)–O(5) | 2.127(8) | Sb(1)–O(3) | 2.215(8) |
| Sb(1)–N(1) | 2.315(8) | Sb(1)–N(2) | 2.332(8) |
| Sb(1)–O(1) | 2.459(7) | Sb(1)–O(7) | 2.564(7) |
| Sb(2)–O(13) | 2.124(8) | Sb(2)–O(11) | 2.218(9) |
| Sb(2)–N(3) | 2.318(8) | Sb(2)–N(4) | 2.322(8) |
| Sb(2)–O(9) | 2.438(7) | Sb(2)–O(15) | 2.541(8) |
| O(16)#1–Er(1)–O(10) | 85.6(3) | O(16)#1–Er(1)–O(2) | 102.7(3) |
| O(10)–Er(1)–O(2) | 150.5(3) | O(16)#1–Er(1)–O(8)#2 | 148.0(3) |
| O(10)–Er(1)–O(8)#2 | 102.5(3) | O(2)–Er(1)–O(8)#2 | 85.4(3) |
| O(16)#1–Er(1)–O(20) | 70.8(3) | O(10)–Er(1)–O(20) | 80.9(3) |
| O(2)–Er(1)–O(20) | 75.5(3) | O(8)#2–Er(1)–O(20) | 140.7(3) |
| O(16)#1–Er(1)–O(17) | 138.7(3) | O(10)–Er(1)–O(17) | 74.5(3) |
| O(2)–Er(1)–O(17) | 81.1(3) | O(8)#2–Er(1)–O(17) | 72.8(3) |
| O(20)–Er(1)–O(17) | 70.5(3) | O(16)#1–Er(1)–O(19) | 78.6(2) |
| O(10)–Er(1)–O(19) | 69.4(3) | O(2)–Er(1)–O(19) | 139.7(3) |
| O(8)#2–Er(1)–O(19) | 75.6(3) | O(20)–Er(1)–O(19) | 138.7(3) |
| O(17)–Er(1)–O(19) | 124.6(3) | O(16)#1–Er(1)–O(18) | 76.3(3) |
| O(10)–Er(1)–O(18) | 139.0(3) | O(2)–Er(1)–O(18) | 70.2(3) |
| O(8)#2–Er(1)–O(18) | 77.6(3) | O(20)–Er(1)–O(18) | 125.0(3) |
| O(17)–Er(1)–O(18) | 140.0(3) | O(19)–Er(1)–O(18) | 71.1(3) |
| O(5)–Sb(1)–O(3) | 146.1(3) | O(5)–Sb(1)–N(1) | 79.4(3) |
| O(3)–Sb(1)–N(1) | 73.3(3) | O(5)–Sb(1)–N(2) | 75.4(3) |
| O(3)–Sb(1)–N(2) | 79.2(3) | N(1)–Sb(1)–N(2) | 77.0(3) |
| O(5)–Sb(1)–O(1) | 82.5(3) | O(3)–Sb(1)–O(1) | 105.2(3) |
| N(1)–Sb(1)–O(1) | 68.7(3) | N(2)–Sb(1)–O(1) | 142.0(3) |
| O(5)–Sb(1)–O(7) | 99.1(3) | O(3)–Sb(1)–O(7) | 91.1(3) |
| N(1)–Sb(1)–O(7) | 142.9(3) | N(2)–Sb(1)–O(7) | 67.0(3) |
| O(1)–Sb(1)–O(7) | 148.3(3) | O(13)–Sb(2)–O(11) | 146.9(3) |
| O(13)–Sb(2)–N(3) | 81.3(3) | O(11)–Sb(2)–N(3) | 72.4(3) |
| O(13)–Sb(2)–N(4) | 75.5(3) | O(11)–Sb(2)–N(4) | 79.5(3) |
| N(3)–Sb(2)–N(4) | 77.6(3) | O(13)–Sb(2)–O(9) | 80.4(3) |
| O(11)–Sb(2)–O(9) | 107.0(3) | N(3)–Sb(2)–O(9) | 68.3(3) |
| N(4)–Sb(2)–O(9) | 140.7(3) | O(13)–Sb(2)–O(15) | 96.1(3) |
| O(11)–Sb(2)–O(15) | 93.6(3) | N(3)–Sb(2)–O(15) | 143.6(3) |
Symmetry transformations used to generate equivalent atoms: #1 x − 1/2, −y, z − 1/2; #2 x + 1/2, −y + 1, z − 1/2; #3 x − 1/2, −y + 1, z + 1/2; #4 x + 1/2, −y, z + 1/2.
Figure 2Coordination polyhedron structure of Er(III).
Figure 3A view of the two-dimensional layer of the complex parallel to the (1 0 0) plane.
Figure 4Packing diagram of the title complex viewed along the a axis.
Figure 5FTIR spectrum of the title complex.
Figure 6TG curve of the title complex.
Thermal decomposition data of the title complex.
| Reaction | Temperature (°C) | Mass loss (%) | |
|---|---|---|---|
|
|
| ||
| [Sb2(edta)2- | |||
| ↓ −8H2O | 70–220 | 12.00 | 12.08 |
| [Sb2(edta)2Er]NO3 | |||
| ↓ −NO2, −1/4O2 | 220–310 | 4.28 | 4.53 |
| [Sb2(edta)2Er]O0.5 | |||
| ↓ −2(CH2)2NCH2COO, −1/4O2 | 310–360 | 18.05 | 17.45 |
| (Sb–Sb)[N(CH2COO)3]2(Er–Er)0.5 | |||
| ↓ −2N(CH2)3, –2CO | 360–430 | 14.69 | 14.09 |
| (OSbO–OSbO)(CO)4(OErO–OErO)0.5 | |||
| ↓ −4CO, –3/4O2 | 430–510 | 11.36 | 11.40 |
| Sb2O3 + 0.5Er2O3 | 39.62a | 40.45b | |
aThe experimental mass percent of the residue in the sample; bthe calculated mass percent of the residue in the sample.
Figure 7XRD pattern of the pyrolysis residue.
Antibacterial activities of the title complex.
| Compound | Concentration (mg·mL−1) | Inhibition zone diameter (mm) | ||||
|---|---|---|---|---|---|---|
|
|
|
|
|
| ||
| DMSO | — | — | — | — | — | — |
| [Sb(Hedta)]·2H2O | 1.0 | 14 | 17 | 13 | 14 | 12 |
| [Sb2(edta)2- | 1.0 | 17 | 26 | 16 | 22 | 16 |
| Penicillin | 1.0 | 15 | 18 | 17 | 19 | 18 |
| Furacilinum | 1.0 | 14 | 23 | 19 | 16 | 20 |