| Literature DB >> 30906785 |
Fatima A I Al-Khodir1, Hana M A Abumelha1, Tarfah Al-Warhi1, S A Al-Issa1.
Abstract
New Pd(II) and Pt(IV) triazine complexes [Pt3(L 1 )2(Cl)9(H2O)3].3Cl.3H2O (1), [Pt3(L 2 )2(Cl)9(H2O)3].3Cl (2), [Pt3(L 3 )2(Cl)9(H2O)3].3Cl (3), [Pt2(L 4 )2(Cl)6(H2O)2] .2Cl.4H2O (4), [Pd3(L 1 )2(H2O)6] .3Cl2 (5), [Pd3(L 2 )2(H2O)6].3Cl2 (6), [Pd3(L 3 )2(H2O)6].3Cl2 (7), and [Pd2(L 4 )2(H2O)4].2Cl2 (8) were synthesized and well characterized using elemental analyses, molar conductance, IR, UV-Vis, magnetic susceptibility, 1H, 13C-NMR spectra, and thermal analyses. These analyses deduced that the L 1 , L 2 , and L 3 ligands act as tridentate forming octahedral geometry with Pt(IV) metal ions and square planar geometry in case of Pd(II) complexes but the L 4 ligand acts as bidentate chelate. The molar conductance values refer to the fact that all the prepared s-triazine complexes have electrolyte properties which are investigated in DMSO solvent. Surface morphology behaviors of prepared complexes have been scanned using TEM. The crystalline behavior of triazine complexes has been checked based on X-ray powder diffraction patterns. The antimicrobial activity of the free ligands and their platinum(IV) and palladium(II) complexes against the species Staphylococcus aureus (G+), Escherichia coli (G-), Aspergillus flavus, and Candida albicans has been carried out and compared with the standard one. The coordination of ligands towards metal ions makes them stronger bacteriostatic agents, thus inhibiting the growth of bacteria and fungi more than the free ligands. The cytotoxic assessment IC50 of the free ligands and its platinum(IV) complexes in vitro against human colon and lung cancer cell lines introduced a promising efficiency.Entities:
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Year: 2019 PMID: 30906785 PMCID: PMC6398043 DOI: 10.1155/2019/9835745
Source DB: PubMed Journal: Biomed Res Int Impact factor: 3.411
Figure 1Structures of prepared triazine ligands [29].= N-(4-chlorophenyl)-N,N-di(pyrimidin-2-yl)-1,3,5-triazine-2,4,6-triamine.= N-(4-chlorophenyl)-N,N-di(pyrimidin-2-yl)-1,3,5-triazine-2,4,6-triamine.=6-chloro-N-(pyrimidin-2-yl)-N-(1H-1,2,4-triazol-3-yl)-1,3,5-triazine-2,4-diamine.= 6-chloro-N-(4-chlorophenyl)-N-(pyrimidin-2-yl)-1,3,5-triazine-2,4-diamine).
Figure 2Synthesis of trisubstituted triazine derivatives.
Microanalytical and physicochemical data of ligands and their complexes.
| Compounds | Color | Λ( | Elemental analyses found(Calc.) | Yield, % | |||
|---|---|---|---|---|---|---|---|
| %C | %H | %N | %M | ||||
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| Yellow | 126.8 | (21.44) | (2.01) | (14.71) | (30.73) | 77 |
| 21.32 | 1.96 | 14.57 | 30.66 | ||||
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| Brown | 70.6 | (20.66) | (1.63) | (13.55) | (31.46) | 72 |
| 20.54 | 1.54 | 13.50 | 31.32 | ||||
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| Green | 64.7 | (13.13) | (1.22) | (17.02) | (35.55) | 71 |
| 13.09 | 1.18 | 17.00 | 35.50 | ||||
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| Pale yellow | 95.6 | (22.64) | (2.19) | (14.22) | (28.29) | 69 |
| 22.56 | 2.13 | 14.16 | 28.11 | ||||
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| Dark brown | 139.3 | (28.64) | (2.69) | (19.65) | (22.39) | 75 |
| 28.56 | 2.57 | 19.54 | 22.31 | ||||
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| Red brown | 82 | (26.77) | (2.53) | (17.56) | (22.24) | 70 |
| 26.71 | 2.51 | 17.49 | 22.19 | ||||
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| Brownish green | 106.7 | (17.70) | (2.15) | (22.94) | (26.14) | 74 |
| 17.65 | 2.09 | 22.90 | 26.11 | ||||
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| Brown | 122.3 | (30.49) | (2.56) | (19.15) | (20.78) | 71 |
| 30.41 | 2.49 | 19.12 | 20.69 | ||||
∗ [Pt3(L)2(Cl)9(H2O)3].3Cl.3H2O (1), [Pt3(L)2(Cl)9(H2O)3].3Cl (2), [Pt3(L)2(Cl)9(H2O)3].3Cl (3), [Pt2(L)2(Cl)6(H2O)2] .2Cl.4H2O (4), [Pd3(L)2(H2O)6].3Cl2 (5), [Pd3(L)2(H2O)6].3Cl2 (6), [Pd3(L)2(H2O)6] .3Cl2 (7) and [Pd2(L)2(H2O)4].2Cl2 (8).
Figure 3Suggested structures of Pt(IV) and Pd(II) complexes.
FT-IR spectral band assignments of L, L, L, and L ligands and their complexes.
| Compounds | FTIR spectral assignments (cm−1) | ||||
|---|---|---|---|---|---|
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| 3249-3112 | 1623 | 1559 | 1488 | - |
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| 3260-3142 | 1619 | 1555 | 1485 | - |
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| 3251-3156 | 1621 | 1586 | 1510 | - |
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| 3244-3150 | 1619 | 1574 | 1484 | - |
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| 3200 | 1679 | 1560 | 1385 | 545, 447 |
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| - | 1667 | 1537 | 1383 | 536, 441 |
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| - | 1698 | 1585 | 1382 | 570, 470 |
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| - | 1695 | 1567 | 1390 | 530, 469 |
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| - | 1689 | 1530 | 1394 | 537, 440 |
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| - | 1695 | 1557 | 1396 | 540, 463 |
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| - | 1698 | 1550 | 1391 | 537, 467 |
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| - | 1691 | 1537 | 1393 | 537, 463 |
Figure 4FT-IR spectra of (a) [Pt2(L)2(Cl)6(H2O)2].2Cl.4H2O (4) and (b) [Pd3(L)2 (H2O)6].3Cl2 (6).
Figure 5TGA-DTG curves of Pt(IV) complexes 1–4.
Figure 6TGA-DTG curves of Pd(II) complexes 5–8.
Thermo gravimetric data of Pt(IV) and Pd(II) triazine complexes.
| Complexes | DTGmax | Total weight loss | Total residual | ||
|---|---|---|---|---|---|
| Weight loss, % | Assignments | Residue, % | Assignments | ||
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| 100 | 74 | 3H2O uncoord | 26 | PtO2 + Few carbons |
| 300, 380, 600 | 2 | ||||
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| 100 | 70 | 3H2O coord | 30 | PtO2 + Few carbons |
| 310, 380, 580 | 2 | ||||
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| 100 | 68 | 3H2O coord | 32 | PtO2 + Few carbons |
| 370, 580, 700 | 2 | ||||
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| 100 | 72 | 4H2O uncoord | 28 | PtO2 + Few carbons |
| 280, 380, 700 | 2 | ||||
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| 230, 360, 620 | 75 | 2 | 25 | PdO + Few carbons |
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| 360, 420, 800 | 75 | 2 | 25 | PdO + Few carbons |
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| 300, 360, 650 | 78 | 2 | 22 | PdO + Few carbons |
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| 380, 620, 800 | 82 | 2 | 18 | PdO + Few carbons |
Figure 7
Figure 8SEM photos of Pt(IV) and Pd(II) complexes 1–8.
Figure 9TEM photos of Pt(IV) complexes 1–4.
Inhibition zone diameter of free ligands and its Pt(IV) and Pd(II) complexes.
| Sample | Inhibition zone diameter (mm/mg Sample) | ||||
|---|---|---|---|---|---|
| Bacteria | Fungi | ||||
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| Standard | Ampicillin: Antibacterial agent | 30 | 24 | -- | -- |
| Amphotericin B: Antifungal agent | -- | -- | 16 | 21 | |
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| Control: DMSO | 0.0 | 0.0 | 0.0 | 0.0 | |
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| 11 | 10 | 10 | 0.0 | |
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| 0.0 | 0.0 | 0.0 | 0.0 | |
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| 0.0 | 0.0 | 0.0 | 0.0 | |
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| 15 | 10 | 0.0 | 0.0 | |
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| 19 | 18 | 16 | 0.0 | |
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| 12 | 11 | 0.0 | 0.0 | |
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| 24 | 23 | 12 | 0.0 | |
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| 14 | 12 | 0.0 | 0.0 | |
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| 14 | 15 | 15 | 0.0 | |
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| 11 | 11 | 0.0 | 0.0 | |
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| 16 | 17 | 12 | 0.0 | |
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| 14 | 15 | 11 | 0.0 | |
∗Ampicillin and amphotericin B are standards of antibacterial and antifungal agents.
IC50 activity of the free ligands and its Pt(IV) complexes.
| Against human colon cancer cell lines | ||||||||
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| Concentration ( | Viability (%) | |||||||
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| 100 | 65 | 66 | 61 | 72.7 | 55.3 | 6.4 | 35.5 | 44.6 |
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| 50 | 70 | 67.8 | 64.4 | 81.7 | 60 | 31.8 | 41.4 | 56.6 |
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| 10 | 72 | 70 | 69.3 | 82.5 | 65 | 62.9 | 66.8 | 71.5 |
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| IC50 | 170 | 461 | 277 | 259 | 162.8 | 27 | 50.7 | 79 |
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| Against human lung cancer A549 cell lines | ||||||||
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| Concentration ( | Viability (%) | |||||||
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| 150 | 82.4 | 100 | 96 | 100 | 100 | 44.6 | 100 | 77.7 |
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| 100 | 83.4 | 100 | 98.7 | 100 | 100 | 61.7 | 100 | 100 |
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| 50 | 86 | 100 | 100 | 100 | 100 | 66.5 | 100 | 100 |
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| 10 | 98.7 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
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| IC50 | 431.4 | - | 1305.7 | - | - | 128 | - | 212 |
Figure 10| No. | Type of analysis | Model of the instruments |
| (i) | Elemental analyses | Perkin Elmer CHN 2400 (USA) |
| (ii) | Metal ions | gravimetrically |
| (iii) | Melting point | MPS10–120 |
| (iv) | Molar conductivities | Jenway 4010 conductivity meter |
| (v) | Infrared spectra | Bruker Alpha FTIR Spectrophotometer |
| (vi) | UV-Vis absorption spectra | UV2 Unicam UV/Vis Spectrophotometer |
| (vii) | Magnetic moments | Magnetic Susceptibility Balance, Sherwood Scientific, Cambridge Science Park, Cambridge, England |
| (viii) | 1H,13C-NMR spectra | Oxford YH-300 NMR spectrometer |
| (ix) | Mass spectra | 70 eV using AEI MS 30 mass spectrometer |
| (x) | Thermal studies TG/DTG | Mettler Toledo AG thermogravimetric analyzer |
| (xi) | SEM | Quanta FEG 250 equipment |
| (xii) | XRD | X 'Pert PRO PANanalytical X-ray powder diffraction |
| (xiii) | TEM | JEOL 100s microscopy |