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Title: high-order harmonic generation from laser induced plasma comprising cdse/v2o5 core/shell quantum dots embedded on mos2 nanosheets.

Abstract: Research of the nonlinear optical characteristics of transition metal dichalcogenides in the presence of photoactive particles, plasmonic nanocavities, waveguides, and metamaterials is still in its early stages. This investigation delves into the high-order harmonic generation (HHG) from laser induced plasma of MoS2 nanosheets in the presence of semiconductor photoactive medium such as CdSe and CdSe/V2O5 core/shell quantum dots. Our comprehensive findings shed light on the counteractive coupling impact of both bare and passivated quantum dots on MoS2 nanosheets, as evidenced by the emission of higher-order harmonics. Significantly, the intensity of harmonics and their cut-off were notably enhanced in the MoS2-CdSe and MoS2-V-CdSe configurations compared to pristine MoS2 nanosheets. These advancements hold promise for applications requiring the emission of coherent short-wavelength radiation.

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• Published: 16 February 2024

Developing high-power Li||S batteries via transition metal/carbon nanocomposite electrocatalyst engineering

• Huan Li   ORCID: orcid.org/0000-0003-0662-6939 1   na1 ,
• Rongwei Meng 2   na1 ,
• Chao Ye 1 ,
• Anton Tadich 3 ,
• Wuxing Hua   ORCID: orcid.org/0000-0003-0385-3773 2 ,
• Qinfen Gu   ORCID: orcid.org/0000-0001-9209-4208 3 ,
• Bernt Johannessen   ORCID: orcid.org/0000-0002-3027-0816 3 , 4 ,
• Xiao Chen   ORCID: orcid.org/0000-0003-1104-6146 5 ,
• Kenneth Davey 1 &
• Shi-Zhang Qiao   ORCID: orcid.org/0000-0002-4568-8422 1  

Nature Nanotechnology ( 2024 ) Cite this article

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The activity of electrocatalysts for the sulfur reduction reaction (SRR) can be represented using volcano plots, which describe specific thermodynamic trends. However, a kinetic trend that describes the SRR at high current rates is not yet available, limiting our understanding of kinetics variations and hindering the development of high-power Li||S batteries. Here, using Le Chatelier’s principle as a guideline, we establish an SRR kinetic trend that correlates polysulfide concentrations with kinetic currents. Synchrotron X-ray adsorption spectroscopy measurements and molecular orbital computations reveal the role of orbital occupancy in transition metal-based catalysts in determining polysulfide concentrations and thus SRR kinetic predictions. Using the kinetic trend, we design a nanocomposite electrocatalyst that comprises a carbon material and CoZn clusters. When the electrocatalyst is used in a sulfur-based positive electrode (5 mg cm −2 of S loading), the corresponding Li||S coin cell (with an electrolyte:S mass ratio of 4.8) can be cycled for 1,000 cycles at 8 C (that is, 13.4 A g S −1 , based on the mass of sulfur) and 25 °C. This cell demonstrates a discharge capacity retention of about 75% (final discharge capacity of 500 mAh g S −1 ) corresponding to an initial specific power of 26,120 W kg S −1 and specific energy of 1,306 Wh kg S −1 .

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Acknowledgements

This research was financially supported by the Australian Research Council (ARC) through the Discovery Project Program (grant numbers FL170100154 and DP220102596). Density functional theory computations were undertaken with the assistance of the National Computational Infrastructure (NCI), supported by the Australian Government. B.J. is supported by a Fellowship at the University of Wollongong. Part of this research was undertaken on the X-ray Absorption Spectroscopy (XAS), Powder Diffraction (PD) and Soft X-ray Spectroscopy (SXR) Beamlines at the Australian Synchrotron, part of ANSTO.

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These authors contributed equally: Huan Li, Rongwei Meng.

Authors and Affiliations

School of Chemical Engineering, The University of Adelaide, Adelaide, South Australia, Australia

Huan Li, Chao Ye, Kenneth Davey & Shi-Zhang Qiao

School of Chemical Engineering and Technology, Tianjin University, Tianjin, China

Rongwei Meng & Wuxing Hua

Australian Synchrotron, ANSTO, Clayton, Victoria, Australia

Anton Tadich, Qinfen Gu & Bernt Johannessen

Institute for Superconducting and Electronic Materials, University of Wollongong, Wollongong, New South Wales, Australia

Bernt Johannessen

Beijing Key Laboratory of Green Reaction Engineering and Technology, Department of Chemical Engineering, Tsinghua University, Beijing, China

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Contributions

S.-Z.Q. conceived and supervised this research. H.L. designed and carried out experiments and density functional theory computations. R.M. carried out the synthesis of the cluster catalysts and electrochemical tests. C.Y. assisted with the design of the sulfur positive electrode. A.T. assisted with soft X-ray spectroscopy and related data analyses. W.H. tested the Li−S battery performance. Q.G. assisted with the in situ synchrotron X-ray diffraction measurements. B.J. carried out X-ray adsorption spectroscopy and data analyses. X.C. captured scanning transmission electron microscope images. S.-Z.Q. and K.D. revised the paper. All authors discussed the results and commented on the paper.

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Correspondence to Shi-Zhang Qiao .

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Nature Nanotechnology thanks Bing Joe Hwang and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Supplementary Figs. 1–32, Tables 1 and 2, Notes 1–6 and References.

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Li, H., Meng, R., Ye, C. et al. Developing high-power Li||S batteries via transition metal/carbon nanocomposite electrocatalyst engineering. Nat. Nanotechnol. (2024). https://doi.org/10.1038/s41565-024-01614-4

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DOI : https://doi.org/10.1038/s41565-024-01614-4

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Structural, magnetic, and magnetocaloric properties of triangular-lattice transition-metal phosphates

Chuandi zhang, junsen xiang, quanliang zhu, longfei wu, shanfeng zhang, juping xu, wen yin, peijie sun, wei li, gang su, and wentao jin, phys. rev. materials 8 , 044409 – published 26 april 2024.

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• INTRODUCTION
• RESULTS AND DISCUSSIONS
• ACKNOWLEDGMENTS

The recent discovery of the spin supersolid candidate Na 2 BaCo ( PO 4 ) 2 has stimulated a great deal of research on triangular-lattice transition-metal phosphates. Here we report a comprehensive study on the structural, magnetic, and magnetocaloric properties of polycrystalline Na 2 A T ( PO 4 ) 2 ( A = Ba,Sr; T = Co,Ni,Mn). X-ray and neutron diffraction measurements confirm that Na 2 Ba T ( PO 4 ) 2 ( NB T P ) crystallizes in a trigonal structure, while Na 2 Sr T ( PO 4 ) 2 ( NS T P ) forms a monoclinic structure with a slight distortion of the triangular network of T 2 + ions. The dc magnetization data show that all six compounds order antiferromagnetically below 2 K, and the Néel temperatures of NS T P are consistently higher than those of NB T P for T = Co, Ni, and Mn, due to the release of geometrical frustration by monoclinical distortions. Furthermore, magnetocaloric measurements show that trigonal NB T P can reach a lower temperature in the quasiadiabatic demagnetization process and thus it demonstrates a better performance in the magnetic refrigeration, compared with monoclinic NS T P . Our findings highlight the outstanding magnetocaloric performances of the trigonal transition-metal phosphates and disclose two necessary ingredients for a superior magnetic coolant that can reach an ultralow temperature, including a perfect geometrically frustrated lattice and a small effective spin number associated with the magnetic ions.

• Received 17 January 2024
• Accepted 1 April 2024

DOI: https://doi.org/10.1103/PhysRevMaterials.8.044409

©2024 American Physical Society

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• Physical Systems

Authors & Affiliations

• 1 School of Physics, Beihang University, Beijing 100191, China
• 2 Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, 100190 Beijing, China
• 3 Spallation Neutron Source Science Center, Dongguan 523803, China
• 4 CAS Key Laboratory of Theoretical Physics, Institute of Theoretical Physics, Chinese Academy of Sciences, Beijing 100190, China
• 5 CAS Center for Excellence in Topological Quantum Computation, University of Chinese Academy of Sciences, Beijing 100190, China
• 6 Peng Huanwu Collaborative Center for Research and Education, Beihang University, Beijing 100191, China
• 7 Kavli Institute for Theoretical Sciences, and School of Physical Sciences, University of Chinese Academy of Sciences, Beijing 100049, China
• * These authors contributed equally to this work.
• † [email protected]

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Room-temperature XRD and NPD patterns of NBNP (a), (e), NBMP (b), (f), NSNP (c), (g), and NSMP (d), (h) and corresponding Rietveld refinements. The circles represent the observed intensities, and the solid lines are the calculated patterns. The differences between the observed and calculated intensities are shown at the bottom. The short vertical bars correspond to the expected nuclear Bragg reflections.

The monoclinic unit cell of NS T P (a) with the in-plane structure viewed along the c axis illustrated in (b), where the angle enclosed by the dashed line marks the in-plane T − T − T bond angle in the isosceles triangular network of the T 2 + layers.

dc magnetic susceptibility ( χ , filled circles) and inverse susceptibility (1/ χ , empty squares) of the polycrystalline NBCP (a), NBNP (b), NBMP (c), NSCP (d), NSNP (e), and NSMP (f), respectively, measured in a magnetic field of 0.1 T. The black solid lines represent the CW fittings to 1/ χ in the low-temperature paramagnetic state from 2 to 20 K. The insets are enlarged plots of χ ( T ) in the temperature range from 0.4 to 1.8 K, in which the arrows mark the AFM ordering temperatures.

Isothermal magnetization [ M ( H ) , filled circles] of polycrystalline NBCP (a), NBNP (b), NBMP (c), NSCP (d), NSNP (e), and NSMP (f), respectively, measured at 0.4 K and their first derivatives ( d M / d H , solid lines). Dashed lines in (a), (b), and (d) correspond to the contribution from the Van-Vleck paramagnetism. The shaded zones in (b) and (c) mark the region of the slope change of the M ( H ) curve, for which a dip appears in d M / d H for NBNP and NBMP. The green arrows in (a), (b), and (d) mark the critical field ( H s ) corresponding to the moment saturation for NBCP, NBNP, and NSCP, respectively.

The cooling curve of polycrystalline Na 2 A T ( PO 4 ) 2 samples in the adiabatic demagnetization process starting from an initial temperature of T 0 = 2 K and an initial magnetic field of H 0 = 4 T (a) and 6 T (b), respectively. The cooling performances of the commercial sub-Kelvin magnetic coolant GGG in similar conditions are also shown, in dashed lines, for comparison.

The zero-field molar specific heat ( C , filled circles) and magnetic entropy ( S , solid lines) of NBCP and GGG single crystals, respectively, at low temperatures. The specific-heat data of single-crystal GGG are from Refs. [ 46, 47 ]. S is obtained by integrating C / T . The horizontal dashed lines mark the maximal magnetic entropy of R  ln2 and R  ln8 as expected for the J eff = 1/2 and J = 7/2 systems, respectively.

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Recent developments in transition metal-based nanomaterials for supercapacitor applications

• FOCUS ISSUE: Transition Metal-based Nanomaterials
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• Rahul Singhal   ORCID: orcid.org/0000-0002-5017-9091 1 ,
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In the recent years the demand of high energy density, high power density energy storage device with long cycle stability increased because of their vast applications from portable electronics devices to power tolls and hybrid electric vehicles. Also, the developments in renewable energy sources also created immediate demand for high energy density energy storage devices. Supercapacitors are found to be suitable to fulfill the current demand of energy storage devices. Transition metal nanomaterials are considered to store high charge because of their large surface area and variable oxidation states. In the present review, we discussed the recent advances in the area of supercapacitors using transition metal oxides, nitride, sulfides, diselenides, phosphides, and ferrites. The effect of surface morphology, synthesis process, and various doping/composites on specific capacitance of supercapacitors were discussed in detail.

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Singhal, R., Chaudhary, M., Tyagi, S. et al. Recent developments in transition metal-based nanomaterials for supercapacitor applications. Journal of Materials Research 37 , 2124–2149 (2022). https://doi.org/10.1557/s43578-022-00598-y

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The mechanism of water oxidation using transition metal-based heterogeneous electrocatalysts.

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a Key Laboratory of Applied Surface and Colloid Chemistry, Ministry of Education, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi’an 710119, P. R. China E-mail: [email protected] , [email protected] , [email protected]

The water oxidation reaction, a crucial process for solar energy conversion, has garnered significant research attention. Achieving efficient energy conversion requires the development of cost-effective and durable water oxidation catalysts. To design effective catalysts, it is essential to have a fundamental understanding of the reaction mechanisms. This review presents a comprehensive overview of recent advancements in the understanding of the mechanisms of water oxidation using transition metal-based heterogeneous electrocatalysts, including Mn, Fe, Co, Ni, and Cu-based catalysts. It highlights the catalytic mechanisms of different transition metals and emphasizes the importance of monitoring of key intermediates to explore the reaction pathway. In addition, advanced techniques for physical characterization of water oxidation intermediates are also introduced, for the purpose of providing information for establishing reliable methodologies in water oxidation research. The study of transition metal-based water oxidation electrocatalysts is instrumental in providing novel insights into understanding both natural and artificial energy conversion processes.

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Synthesis, characterization, and biological studies of some biometal complexes

• Vinay Kumar Srivastava 1  

Future Journal of Pharmaceutical Sciences volume  7 , Article number:  51 ( 2021 ) Cite this article

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Metal complexes Cu[C 13 H 8 O 4 N] 2 2, Ni[C l3 H 8 O 4 N] 2 3, and Co[C 13 H 8 O 4 N] 2 4 of bioinorganic relevance have been synthesized with the Schiff base ligand 2-furylglyoxal–anthranilic acid (FGAA) [C 13 H 9 O 4 N] 1 .

All the complexes are well characterized by various spectral and physical methods. The antimicrobial activity of the complexes has been studied against some of the pathogenic bacteria and fungi.

Results indicate that complexes have higher antimicrobial activity than the free ligand. This would suggest that chelation reduces considerably the polarity of the metal ions in the complexes which in turn increases the hydrophobic character of the chelate and thus enables permeation, through the lipid layer of microorganisms. All the complexes were assessed for their anticancer studies against a panel of selected cancer cells HOP62 and BT474 respectively. Results showed that the complexes are promising chemotherapeutic alternatives in the search of anticancer agents. The fluorescence quenching phenomenon is observed in the Schiff base metal complexes.

The octahedral transition metal complexes 2, 3, and 4 have been obtained by treatment of ligand 2-furylglyoxal-anthranilic acid (FGAA) 1 with metal acetate. Complexes under investigations have shown antimicrobial, potential anticancer, and the DNA binding studies.

Graphical abstract

The chemistry of transition metal complexes has received considerable attention largely due to their catalytic and bioinorganic relevance. Such complexes are also important due to their potential biological activities such as antibacterial, antifungal, antimalarial, and antitumor [ 1 , 2 , 3 , 4 ]. Medicinal inorganic chemistry is comparatively a new discipline which developed after the serendipitous discovery of the antitumor activity of cisplatin [ 5 , 6 , 7 ]. The clinical success of this platinum complex has stimulated considerable interest in the search for new metal complexes as modern therapeutics, diagnostic, and radiopharmaceutical agents. Copper, nickel, and cobalt complexes are used in the treatment of many diseases including cancer and as potential hypoxia-activated prodrugs [ 8 , 9 , 10 , 11 , 12 , 13 , 14 ]. Coordination compounds which form coordinate bonds via the sulfur, oxygen, and nitrogen donor atoms are well known and have a long history. The interest in preparation of new metal complexes gained the tendency of studying the interactions of metal complexes with DNA for their applications in biotechnology and medicine.

Deoxyribonucleic acid (DNA) is the primary target molecule for most anticancer and antiviral therapies according to cell biologists. Investigation on the interaction of DNA with small molecules is important in the design of new type of pharmaceutical molecule. Schiff base constitutes an important class of nitrogen donor ligands and occupy a prominent position among the recent achievement in the field of coordination chemistry. The azomethine which is the functional group of Schiff base is aided in forming a stable complex. The chemistry of Schiff base metal complexes is exploited in industries, technologies, and in medicinal fields. The present investigations deal with the synthesis, characterization, antimicrobial, anticancer, and DNA cleavage studies of Cu(II), Ni(II), and Co(II) metal complexes containing Schiff base ligand 2-furylglyoxal-anthranilic acid (FGAA).

All reagents used were of analytical grade and used as purchased commercially; however, the solvents were purified by the standard procedure [ 15 ]. The ligand 2-furylglyoxal-anthranilic acid (FGAA) was prepared by the reported procedure [ 16 , 17 , 18 , 19 , 20 ]. C, H, and N were analyzed on Carlo-Erba microanalyzer. Metal contents were estimated by standard procedure [ 21 ]. FTIR was recorded on Thermo Nicolet Avater 370. Electronic spectra on Shimadzu UV-160A spectrophotometer. The conductance measurements were carried out on a metal CM-180 Eliodigital conductivity meter. Magnetic studies were done by a Guoy balance using Hg [Co (SCN) 4 ] as the calibrant.

1 H and 13 C NMR spectra in dimethyl sulfoxide (DMSO) were recorded on a Brucker WH 300 (200 MHz) and Varian Gemini (200 MHz) spectrometers using tetramethylsilane (TMS) as an internal reference.

The in vitro antimicrobial screening effects of the investigated compounds were tested against the bacterial species: Escherichia coli , ( E. coli ) and Klbsiella pneumoniae ( K. pneumoniae ), and fungal species: Aspergillus niger ( A. niger ) and Candida albicans ( C. albicans ) by using Kirby Bauer Disk diffusion method [ 22 , 23 , 24 ]. Chloramphenicol and nystatin were used as the standard antibacterial and antifungal agents. The tested compounds were dissolved in DMF solution (which has no inhibition activity) and solution soaked in filter paper disk of 5 mm diameter and 1 mm thickness. The disks were incubated 24 h for bacterial and 72 h for fungal species at 37 °C. The minimum inhibitory concentration (MIC) value of the compounds was determined by the serial dilution method [ 25 , 26 , 27 ].

The in vitro cancer studies of all the compounds were assessed for their anti-proliferation test against a panel of selected human cancer cell lines such as HOP62 (lung) and BT 474 (breast) by using SRB (sulforhodamine B) assay [ 28 , 29 , 30 , 31 , 32 , 33 , 34 , 35 , 36 , 37 ] concentration of drug used 10, 20, 40, and 80 μg/mL ADR (adrimycin) was used as a positive control which controls cells with definite structure and clear cell wall without degeneration. Each drug was assayed inducing 50% growth inhibition (GI 50 ), total growth inhibition (TGI), and 50% cytotoxicity (LC 50 ) after a 48 h incubation period were calculated by linear interpolation from the observed data points. Fluorescence measurements were recorded on an F-7000 FL spectrophotometer at room temperature.

Synthesis of metal complexes (2-4)

Metal complexes of Cu[C 13 H 8 O 4 N) 2 2, Ni [C 13 H 8 O 4 N] 2 3 , and Co [C 13 H 8 O 4 N] 2 4, were synthesized by the addition of ethanolic solution of ligand 2-furylglyoxal–anthranilic acid 1 (2 mmol) copper acetate/nickel acetate/cobalt acetate (1 mmol). The mixture was magnetically stirred and refluxed for 2 h. The complexes obtained were filtered, washed with ethanol, and dried.

All the metal complexes were colored, non-hygroscopic in nature, and stable at room temp. They were insoluble in common organic solvents but soluble in DMF and DMSO. The results of the elemental analysis are in good agreement with the calculated values. The molar conductance value indicates their non-electrolytic nature. Physical and analytical data of complexes are summarized in Table  1 .

On the basis of analytical and spectral data, octahedral geometry has been assigned to the complexes. The results of antimicrobial activity and anticancer studies indicate metal complexes are much more active as compared to ligand fragments. Fluorescence quenching phenomena are observed in its metal complexes by fluorescence studies.

IR spectral studies

Infrared spectra of free ligand, a sharp band [ 38 , 39 , 40 ] appeared at 1615-1590 cm –1 ascribed to the stretching vibrations of azomethine group and was shifted to lower frequency region after complexation suggesting thereby the participation of imine nitrogen. A strong band appeared at 1735-1690 cm –1 in the IR spectra of ligand (FGAA) which is due to the presence of stretching vibration of carbonyl group coordination through this carbonyl oxygen to the central metal ion is confirmed by a negative shift in this frequency in the spectra of corresponding metal complexes. IR spectra of ligand displays a bond of medium intensity in the region of 3550-3490 cm –1 due to the –OH stretching vibration of free –CO 2 H group. Coordination of ligand as a consequence of deprotonation of – CO 2 H group is evident by the disappearance of the above band in the IR spectra of respective complexes [ 41 , 42 ]. Furthermore, the asymmetrical and symmetrical vibrations of COO – group appeared at 1560-1535 cm –1 and 1340-1325 cm –1 Δν (as–s) value 220-210 cm –1 further indicate the coordination through unidentate carboxylate group. Some new bands appeared in the IR spectra of metal complexes at 550-530 cm –1 , 450-430 cm –1 , and 335-325 cm –1 are probably due to the formation of M–O, M–N, and M–S bonds respectively which further give additional evidences in favor of the coordination of metals through azomethine nitrogen, carbonyl oxygen, and carboxylate group.

Electronic spectral and magnetic studies

Divalent copper having a d 9 configuration give rise to a 2D free ion term which split into a regular octahedral environment into a lower doublet 2 E g and an upper triplet 2 T 2g levels. In electronic spectra [ 43 , 44 , 45 , 46 ] of a true octahedral system, only one band due to 2 E g → 2 T 2g transitions is expected but true octahedral structures are not common. Therefore, instead of a one broad band due to 2 E g → 2 T 2g transition. These transitions from the ground state 2 B 1g → 2 A 1g → 2 B 2g and 2 E g are expected as a consequence of John-Tellers configuration stability. The 2 E g orbitals separate so that one goes up as much as the other goes down.

The T 2g orbitals separate in such a way that the doubly degenerate pair goes down only half as far as the single orbital goes up therefore in case of Cu (II); there is no net energy change for T 2g electrons since four are stabilized while two are destabilized due to which Cu(II) complex shows distortion in an octahedral geometry. The electronic spectra of Cu(II) complex displays three spectral bands in the region 10635, 14850, 16345 cm –1 which are in good agreement with the distorted geometry of complex under investigation. This geometry is further supported by the magnetic moment value 1.98 B.M. of the complex. In the Ni(II) complex, three bands in the range 10750, 1665, 25650 cm –1 corresponding to the transition 3 A 2g → 3 T 2g → 3 T 1g and 3 T 1g (P) are observed which clearly indicate the octahedral geometry. The theoretical value of ν 2 /ν 1 for octahedral Ni(II) complex is found 1.55. The observed value lies 1.60 which is in conformity with the distorted octahedral geometry of the ligand around central Ni(II) ion lowering the ratio of ν 2 /ν 1 may be attributed due to configuration interaction between T 1g (P) and T 1g (F) excited state. The octahedral geometry is further supported by their magnetic value 3.14 B.M. In octahedrally surrounded Co(II) ions, three bands in the region 8000, 15616, 18175 cm –1 are expected which may be assigned to 4 T 1g to 4 T 2g (F) (ν 1 ), 4 A 2g (F) (ν 2 ), and 4 T 1g (P) (ν 3 ) transitions respectively. The 4 A 2g transition is very weak and often appears as shoulder. Cobalt complex possesses an octahedral geometry which is further confirmed by the energy ratio ν 2 /ν 1 lies 1.95 and magnetic moment value 4.60 B.M.

NMR spectral studies

In the 1 H NMR spectra of free Schiff base ligand, the signals were appeared in the range of 7.15-7.20 ppm due to (HC=N) proton [ 47 ]. However, in the spectra of Schiff base metal complexes of Cu(II), Ni(II), and Co(II), the signals were observed in the downfield regions of 8.0–9.0 ppm supporting the coordination of iminonitrogen atom to Cu (II)/Ni (II)/Co (II) [ 48 ] while the free ligand NMR spectra has a characteristic NMR signal for carboxyl group proton in the 10.5-12.5 ppm range, the disappearance of this signal in the 1 H NMR spectra of metal complexes indicating the involvement of carboxylate ion oxygen in chelation through deprotonation. There is no appreciable change in the peak position corresponding to NH and aromatic protons. The 13 C–NMR signals for the metal, complexes are assigned by the comparison with the spectra of corresponding free Schiff base ligand. A downfield shift of CH = N group in the range of 150-160 ppm and for 175-182.5 ppm. In the complexes, NMR spectra indicate that the ligand coordinates through both the nitrogen atom of CH = N and the oxygen of COO — ion [ 49 , 50 , 51 , 52 ] (Fig.  1 ).

The proposed structure of metal complex M = Cu(II) or Ni(II) or Co(II)

In vitro antimicrobial studies

The antibacterial and antifungal activity of the ligand and complexes [ 53 , 54 ] were assayed against some of the bacteria and fungi. DMF is used as negative control and chloramphenicol is used as a positive standard for antibacterial and nystatin for antifungal activities (Fig.  2 a and b). The minimum inhibitory concentration (MIC) value of the compounds was determined by the serial dilution method and is given in Table  2 .

a Antibacterial studies of ligand and its metal complex against E. coli and K. pneumoniae . b Antifungal studies of ligand and its metal complex against A. niger and C. albicans

The in vitro antimicrobial activity results revealed that complexes are more microbial toxic than the ligand. The activity order of the synthesized complexes and ligand are as follows 2 > 4 > 3 > 1 .

Such increased activity of the metal chelates can be explained on the basis of Tweedy’s chelation theory on chelation, the polarity of the metal ion will be reduced to a greater extent due to the overlap of the ligand orbital and partial sharing of the positive charge of the metal ion with donor groups. Further, it increases the delocalization of π electrons over the whole chelate ring and enhances the penetration of the metal complexes into lipid membranes and blocking of the metal-binding sites in the enzymes of microogranism. These complexes also disturb the respiration process of the cell and thus block the synthesis of proteins which restricts further growth of the organism. The complex 2 shows higher antimicrobial activity than other complex 3 and 4 complex. The variation in the effectiveness of different compounds against different organisms depends either on the impermeability of the cells of the microbes or on differences in ribosome of microbial cells. Further, lipophilicity which controls the rate of entry of molecules into the cells is modified by coordination so compounds 2 , 3 , and 4 can become more active than compound 1 compared to the standard compounds chloramphenicol and nystatin (Fig.  2 a and b); the present metal complexes are much less active against the representative strains of microorganism [ 55 , 56 ].

In vitro anticancer studies

The data obtained by the SRB assay show that metal complexes 2 and 3 have inhibitory effects on the growth of HOP62 (Tables  3 and 4 ) (Fig.  3 ) and BT474 (Tables  5 and 6 ) (Fig.  4 ). Cancer cells in dose-dependent manner. Complex 4 exhibits cytotoxic effect on BT474 cancer cells but no antiproliferative effect against cell line HOP62. The antiproliferative effect of tested complexes is likely due to the lipophilicity of the complexes that alleviate the transport of metal complexes into the cell and posteriorly into the organelles where metal may possibly contribute to toxicity by inhibitory cellular respiration and metabolism of biomolecules [ 57 , 58 , 59 ]. The pure metals are inactive however the activity of metal cations varies on their bioavailability hence delivery methods/solubility and ionization of metal sources are significant parameters to deal metals in biological system [ 60 , 61 , 62 ] possibly this is the reason that bonding of metal cations (Cu(II)/Ni(II)/Co(II) to biologically compatible ligand (FGAA) enhances the bioavailability and ultimately the activity of metal cations. In contrast, coordination enhances the activity of the metal complexes against BT 474 and HOP 62 cell lines. The compound 1 (ligand) exhibited no cytotoxic effect on both the cell lines. The choice of the coordinated ligand (s) seems to be as important as the choice of metal(s) because besides being the integral part of biologically active complexes. These organic molecules (ligands) can exert a biological activity of their own. The photomicrograph of the cells treated with compounds 1, 2, 3, and 4 revealed the morphological features of apoptosis consist of membrane blebbing, nuclear condensation, cytoplasmic shrinkage, DNA fragmentation, cell wall destruction, and formation of apoptotic bodies (Figs.  5 and 6 ). Morphological images were grabbed using a phase-contrast microscope at × 20 magnifications with a digital camera at 48 h after treatment with the samples. Compound 1 showed negligible cytotoxicity as the cell growth and morphology did not get affected whereas it can be seen clearly that the compounds 2 , 3 , and 4 affected the normal morphology which rendered the cells to lose their viability. The picture revealed that the cells treated with compounds 2 , 3 , and 4 exhibited apoptotic cellular death as the population of cells reduced drastically within the 48 h of treatment. The photomicrograph depicts the treatment of HOP 62 and BT 474 cells treated with complexes 2 , 3 , and 4 showed a significant inhibitory effect on the cellular growth. In all two cell lines, the increase in the number of cells with abnormal morphology was accompanied by an increase in the number of irregular refractive clumps. The majority of the cell appear to be rounded and shrunken due to apoptosis and white spots in the images showing the apoptotic cell. The percentage cell viability in presence of ligand and metal complexes for BT 474 and HOP 62 cell lines are shown in Figs.  3 and 4 . The graphs of percentage control growth versus molar drug concentration showed the effective drug concentration on both cell lines and each point is the mean standard error obtained from three independent experiments. The results showed that complexes 2 , 3 , and 4 were the most potent and strongly inhibited the proliferations of both the two cell lines in a dose-dependent manner with TGI values 17.3, 30.3, and 46.4 μg/ml respectively. It was verified that the increased in concentration of complexes leads to higher cytotoxic activities. Nevertheless, results also proved that ADR showed superior cytotoxic activity against both cell lines.

Growth curve: human lung cancer cell line HOP 62 compounds 1-4

Growth curve: human breast cancer cell line BT 474 compounds 1 - 4

HOP 62 Cell images compounds 1 - 4

BT474 Cell images compounds 1-4

Fluorescence studies

Emission intensity of the three complexes increases on increasing the conc. of CT DNA. The enhancement of emission intensity is an indication of binding for the complexes to the hydrophobic pockets of DNA and complexes can be protected efficiently by the hydrophobic environment inside the DNA helix [ 63 , 64 ]. The high binding affinities of the metal complexes are probably attributed to the extension of the π system of the intercalated ligand due to the co-ordination of transition metal ions which also leads to a planar area greater than that of the free ligand and the coordinated ligand penetrating more deeply into and stacking more strongly with base pairs of DNA. The quenching plots illustrate that the quenching of ethidium bromide (EtBr) bound to DNA by the complexes are in good agreement with the linear Stern-Volmer equation which proves that the three complexes bind to DNA. The K b (slope/intercept values in graph of F 0 / F vs (conc.) values for complexes 2 , 3 , and 4 are 2.225 × 10 2 M –1 , 1.94 × 10 2 M –1 , and 1.55 × 10 2 M –1 ). Based on the K b values, the order of binding strength of metal complexes 2 > 3 > 4 (Figs.  7 , 8 , 9 ).

a Fluorescence quenching curves of ethidium bromide bound to DNA in presence of Ni (II) complex. b Stern-Volmer plots of the fluorescence titration for Ni (II) complex. Representation of slope and Intercept values. Kb = slope/Intercept value i.e. 1.94 × 10 2 M -1 F0 = Highest emission of DNA+Etbr, F = Highest emission of DNA+Etbr after addition of complexes

a Fluorescence quenching curves of ethidium bromide bound to DNA in presence of Cu (II) Complex. b Stern-Volmer plots of the fluorescence titrations for Cu (II) Complex. Representation of slope and intercept values. Kb = slope/Intercept value i.e. 2.225 × 10 2 M -1

a Fluorescence quenching curves of ethidium bromide bound to DNA in presence of Co (II) complex. b Stern-Volmer plots of the fluorescence titrations for Co (II) Complex. Representation of slope and intercept values. Kb = slope/Intercept value i.e. 1.55 × 10 2 M -1

Conclusions

In the present study, novel metal complexes of Cu(II), Ni(II), and Co(II) were prepared and characterized by physico-chemical methods. Spectral studies demonstrate the ligand coordinating through azomethine nitrogen and carboxylate oxygen atoms and reveal octahedral geometry for Cu(II), Ni(II), and Co(II) complexes. The antibacterial and antifungal data given for the compound presented in this paper allowed us to state that the metal complexes generally have better activity than the ligands and less activity than standards. The metal complexes exerted growth inhibition on the human tumor cell lines showing promise as potential anticancer drugs deserving of further investigation. The Schiff base exhibits a strong fluorescence emission contrast to this partial fluorescence quenching phenomena is observed in its metal complexes.

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Abbreviations

2-Furylglyoxal-anthranilic acid

Tera methyl silane

Dimethyl formamide

Dimethyl sulfoxide

Minimum inhibitory concentration

Sulforhodamine B

50% growth inhibition

Total growth inhibition

Cytotoxic killing of 50% of cells

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Acknowledgements

The author express his gratitude to the STIC, Cochin University, CDRI, Lucknow , S.P Centre for Science and Technology Vallabh Vidhya Nagar, and ACTREC Mumbai for providing facilities of spectral and biological studies.

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Srivastava, V.K. Synthesis, characterization, and biological studies of some biometal complexes. Futur J Pharm Sci 7 , 51 (2021). https://doi.org/10.1186/s43094-021-00191-w

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Organic Synthesis via Transition Metal-Catalysis

In recent years, the development of transition-metal-catalyzed reactions has acquired an increasing importance. In fact, the use of transition metal complexes as catalysts may allow performing important organic transformations in one synthetic step by the assembly of simple units under sustainable conditions [ 1 ]. This Special Issue reports significant contributions in this field. In particular, seven papers have been published: two reviews and five original research articles.

The first review (by Garazi Urgoitia, Maria Teresa Herrero, Fátima Churruca, Nerea Conde, and Raul SanMartin) reports on the use of palladium pincer complexes as catalysts or pre-catalysts for the direct arylation of arenes with aryl halides or pseudo-halides [ 2 ]. This is a particularly important process, which allows aryl–aryl coupling (also intramolecularly) using an arene (or heteroarene) as one coupling partner, with C–H activation.

The second review (by Mieko Arisawa and Masahiko Yamaguchi) concerns the synthesis of a plethora of organosulfur compounds by rhodium-catalyzed S–S bond cleavage of disulfides or elemental sulfur and subsequent transfer of the ensuing organothio groups to organic substrates [ 3 ].

In the first original research article, Jérémy Ternel, Adrien Lopes, Mathieu Sauthier, Clothilde Buffe, Vincent Wiatz, Hervé Bricout, Sébastien Tilloy, and Eric Monflier describe the reductive hydroformylation (performed under 80 bar pressure of a 1:1 CO/H 2 mixture, in toluene at 80 °C) of isosorbide diallyl ether (readily available by allylation of bio-sourced isosorbide). The process is catalyzed by a rhodium/amine catalytic system, [typically, Rh(acac)(CO) 2 /Et 3 N], to give the corresponding high value-added bis-primary alcohols [ 4 ].

The second original research article (by Joanna Palion-Gazda, André Luz, Luis R. Raposo, Katarzyna Choroba, Jacek E. Nycz, Alina Bieńko, Agnieszka Lewińska, Karol Erfurt, Pedro V. Baptista, Barbara Machura, Alexandra R. Fernandes, Lidia S. Shul’pina, Nikolay S. Ikonnikov, and Georgiy B. Shul’pin) reports on the use of methyl-substituted 8-hydroxyquinolines (Hquin) for the preparation of five-coordinated oxovanadium(IV) complexes [VO(2,6-(Me) 2 -quin) 2 , VO(2,5-(Me) 2 -quin) 2 , and VO(2-Me-quin) 2 ]. These complexes were then used as catalysts for the efficient oxidation of hydrocarbons (to alcohols) and alcohols (to ketones), carried out with H 2 O 2 in acetonitrile at 50 °C in the presence of 2-pyrazinecarboxylic acid (PCA) as a cocatalyst [ 5 ].

The subsequent papers report on transition-metal-promoted cyclization processes leading to heterocyclic derivatives. Thus, new polycyclic heterocycles (1 H -benzo[4,5]imidazo[1,2- c ][1,3]oxazin-1-ones) were synthesized by Lucia Veltri, Roberta Amuso, Marzia Petrilli, Corrado Cuocci, Maria A. Chiacchio, Paola Vitale, and Bartolo Gabriele using a ZnCl 2 -promoted deprotective annulation approach starting from N -Boc-2-alkynylbenzimidazoles under mild conditions (CH 2 Cl 2 as the solvent at 40 °C for 3 h) [ 6 ]. N -benzoylindoles were obtained by Zhe Chang, Tong Ma, Yu Zhang, Zheng Dong, Heng Zhao, and Depeng Zhao by Pd(II)-catalyzed oxidative C–H functionalization and annulation of substituted N -(2-allylphenyl)benzamides, carried out with Pd(OAc) 2 as the catalyst in the presence of benzoquinone as the oxidant and dibutyl phosphate as the additive in DMSO at 60–70 °C [ 7 ]. An annulative C–H activation process was also developed by Bao Wang, Xu Han, Jian Li, Chunpu Li, and Hong Liu for the synthesis of fused isochromeno-1,2-benzothiazine derivatives, starting from S -phenylsulfoximides and 4-diazoisochroman-3-imine. The process, catalyzed by [Cp*RhCl 2 ] 2 in the presence of AgOPiv, takes place in trifluoroethanol at room temperature under air [ 8 ].

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