Synthesis and Characterization of Cobalt(II)/(III), Nickel(II) and Copper(II) Complexes of New 14, 15 and 16-Membered Macrocyclic Ligands

El-Tabl, Abdou Saad Korean Chemical Society 2004 Bulletin of the Korean Chemical Society Vol.25 No.12

A new series of nickel(II), cobalt(II)/(III) and copper(II) complexes of 14, 15 and 16-membered of macrocyclic ligands have been prepared and characterized by elemental analyses, IR, UV-VIS and $^1H-NMR$ spectra, magnetic susceptibilities, conductivities, DTA and ESR measurements. Molar conductances in DMF solution indicate that, the complexes are nonelectrolytes except (9-12) complexes. The electronic spectra show that, all complexes are square planar or distorted octahedral geometry. The ESR spectra of solid complexes (4), (8) and (11) show square planar of axial type symmetry $(d_{x2-y2})$ with considerable covalent bond character. However, complex (12) shows a spectrum of octahedral geometry with $d_{z2}$ ground state. Complex (12) shows exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Synthesis, Characterization and ESR Studies of New Copper(II) Complexes of Vicinal Oxime Ligands

El-Tabl, Abdou S.,Shakdofa, Mohamad M.E.,El-Seidy, Ahmed M.A. Korean Chemical Society 2011 대한화학회지 Vol.55 No.4

Ethoxylacetyl oxime ligands [HL, (1) and $H_2L^1$, (3)] react with copper(II) acetate monohydrate yield octahedral and square planar complexes, respectively. The complexes have been postulated due to elemental analyses, IR, UVVis. spectra, magnetic susceptibility, conductivity and ESR spectra. Molar conductance of the complexes in DMF indicates a non-ionic character. The ESR spectra of [$(L)_2Cu(H_2O)_2$], (2) complex at room temperature and 77K are characteristic of an axial symmetry ($d_{x2-y2}$) with covalent bond character and have a large line width typical of dipolar interactions. However, [$(L^1)Cu$], (4) complex in the solid state showed spectra of marked broadening and loss of hyperfine splitting confirming spinexchange interactions between the copper(II) sites. The spectrum of the doped copper(II) complex at room temperature showed super-hyperfine splitting from coordinated nitrogen atoms and it has an axial type ($d_{x2-y2}$) with covalent bond character and an essentially square-planar arrangement around the copper(II) ion. The spectrum of [$(L^1)Cu$], (4) in frozen methanol at 77K was characteristic of the triplet state of a dimer species and the distance found between the two copper(II) centers was calculated and is equal to 4.8 ${\AA}$. Ethoxylacetyl oxime 리간드 [HL, (1) 및 $H_2L^1$, (3)]와 아세트산 구리(II) 일수화물을 반응시켜 팔면체 및 사각평면착물을 각각 얻었다. 이들 착물을 원소분석, IR 및 UV-Vis 스펙트럼, 자기수자율, 전기전도도 및 ESR 스펙트럼으로 조사하였다. DMF에서 이들 착물의 몰전기전도도 측정한 결과 비이온성을 보였다. 실온 및 77 K에서 [$(L)_2Cu(H_2O)_2$], (2) 착물의 ESR 스펙트럼은 배위결합성을 갖는 축대칭($d_{x2-y2}$)의 특성을 보이며, 또한 전형적인 쌍극자 상호작용에 의해 큰 띠나비를 갖는다. 그러나 착물 [$(L^1)Cu$], (4)는 고체상태에서 큰 띠넓임으로 인해 초미세 갈라짐이 관찰되지 않았는데, 이는 구리(II) 결합자리들 사이의 스핀-교환 상호작용에 의한 것으로 확인되었다. 실온에서 도포된 구리(II) 착물의 스펙트럼은 배위된 질소원자로 인해 극초미세 갈라짐을 보였다. 또한 이 물질은 공유 결합성을 갖는 축형태($d_{x2-y2}$)의 특성을 보이고, 구리(II) 이온의 환경은 기본적으로 사각-평면 배열을 갖는다. 77 K의 얼어있는 메탄올에서 [$(L_1)Cu$], (4)의 스펙트럼은 이합체 화합물의 삼중항 상태의 특성을 보이며, 두 구리(II) 이온 중심 사이의 거리를 계산한 결과 4.8 이다.

Synthesis, Characterization and Biological Studies of New Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide

El-Tabl, Abdou S.,Shakdofa, Mohamad M.E.,El-Seidy, Ahmed M.A.,Al-Hakimi, Ahmed N. Korean Chemical Society 2011 대한화학회지 Vol.55 No.1

2-(Benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide 에대한새로운일련의 Mn(II), Ni(II), Co(II), Cu(II) 및 Zn(II) 착물을 합성하여 그 특성을 원소분석, IR, UV-vis, $^1H$-NMR, 질량분석, ESR, 자기수자율 및 몰 전기전도도 측정에 의하여 조사하였다. 이들 착물의 기하구조가 사각평면 또는 팔면체임을 분광학적 데이터 및 자기적 측정으로부터 알았다. 이 리간드와 해당착물의 세균에(Aspergillus nigar 및 Fusarium oxysporium) 대한생물학적활성을 조사하였다. 그 결과, 금속착물들은 리간드 및 금속이온 모두에 비해 더 큰 활성을 나타내었다. New series of Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of the 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene) acetohydrazide have been synthesized and characterized by elemental analysis, IR, UV-vis, $^1H$-NMR, mass and ESR spectra, magnetic susceptibility and molar conductivity measurements. The spectral data and magnetic measurements of the complexes indicate that, the geometries are either square planar or octahedral. The biological activity of the ligand and its complexes against fungi (Aspergillus nigar and Fusarium oxysporium) were investigated. The metal complexes exhibited higher activity than both the parent ligand and the corresponding metal ion.

Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

El-Tabl, Abdou S.,Shakdofa, Mohamad M.E.,El-Seidy, Ahmed M.A. Korean Chemical Society 2011 대한화학회지 Vol.55 No.6

A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Synthesis and Characterization of Cobalt(II)/(III), Nickel(II) and Copper(II) Complexes of New 14, 15 and 16-Membered Macrocyclic Ligands

Abdou Saad El-Tabl 대한화학회 2004 Bulletin of the Korean Chemical Society Vol.25 No.12

A new series of nickel(II), cobalt(II)/(III) and copper(II) complexes of 14, 15 and 16-membered of macrocyclic ligands have been prepared and characterized by elemental analyses, IR, UV-VIS and 1H-NMR spectra, magnetic susceptibilities, conductivities, DTA and ESR measurements. Molar conductances in DMF solution indicate that, the complexes are nonelectrolytes except (9-12) complexes. The electronic spectra show that, all complexes are square planar or distorted octahedral geometry. The ESR spectra of solid complexes (4), (8) and (11) show square planar of axial type symmetry (dx2-y2) with considerable covalent bond character. However, complex (12) shows a spectrum of octahedral geometry with dz2 ground state. Complex (12) shows exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.

Synthesis, Characterization and Biological Studies of New Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide

Abdou S. El-Tabl,Mohamad M. E. Shakdofa,Ahmed N. Al-Hakimi,Ahmed M. A. El-Seidy 대한화학회 2011 대한화학회지 Vol.55 No.1

New series of Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of the 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide have been synthesized and characterized by elemental analysis, IR, UV-vis, ^1H-NMR, mass and ESR spectra, magnetic susceptibility and molar conductivity measurements. The spectral data and magnetic measurements of the complexes indicate that, the geometries are either square planar or octahedral. The biological activity of the ligand and its complexes against fungi (Aspergillus nigar and Fusarium oxysporium) were investigated. The metal complexes exhibited higher activity than both the parent ligand and the corresponding metal ion.

Synthesis, Spectroscopic, and Biological Studies of Chromium(III), Manganese(II), Iron(III), Cobalt(II), Nickel(II), Copper(II), Ruthenium(III), and Zirconyl(II) Complexes of N¹,N²-Bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)pr

Al-Hakimi, Ahmed N.,Shakdofa, Mohamad M.E.,El-Seidy, Ahemd M.A.,El-Tabl, Abdou S. Korean Chemical Society 2011 대한화학회지 Vol.55 No.3

[ $N^1,N^2$ ]bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)propyl)phthalamide ($H_4L$, 1) 의 새로운 크롬(III), 망간(II), 철(III), 코발트(II), 니켈(II), 구리(II), 루테늄(III) 및 산화 지르코늄(II) 착물을 합성하여 원소분석, 물리적 성질 및 분광학적으로 특성을 규명하였다. 분광학적 결과를 통해 이 리간드는 $[H_4LMX_2(H_2O)]{\cdot}nH_2O$ (M = Cu(II), Ni(II), Co(II), X = Cl 또는 $NO_3$)의 일반식을 갖는 착물2-5에서는 중성의 삼배위 리간드로 행동한다. 또는 $[H_4L(ZrO)_2Cl_2]{\cdot}8H_2O$ 의 일반식을 갖는 착물 6-9 에서는 이염기성 육배위 리간드로 행동한다. DMF 용액에서의 몰전기전도도 실험결과 이들 착물은 비이온성을 나타낸다. 고체 구리착물 2, 5 및 6 의 ESR 스펙트럼에서 $g_{\parallel}$ >g> $g_e$을 보이는데, 이는 일그러진 팔면체구조와 큰 공유결합성을 갖는 $d{_x}^2{_{-y}}^2$ 오비탈에 비공유 전자쌍이 존재함을 의미한다. 이합체 구리(II) 착물 $[H_2LCu_2Cl_2(H_2O)_4]{\cdot}3H_2O$ (6)에 대해 두 구리원자 사이의 거리를 ESR 스펙트럼으로부터 추정한 parallel component 의 field zero splitting 파라메타를 이용하여 계산하였다. 이들 화합물의 항박테리아 및 항균 활성도를 측정한 결과, 몇가지 금속 착물의 경우 표준시약인 tetracycline (박테리아) 및 Amphotricene B (균류)보다 더 큰 저해효과를 보였다. Novel chromium(III), manganese(II), iron(III), cobalt(II), nickel(II), copper(II), ruthenium(III), and zirconyl(II) complexes of $N^1,N^2$-bis(3-((3-hydroxynaphthalen-2-yl)methylene-amino)propyl)phthalamide ($H_4L$, 1) have been synthesized and characterized by elemental, physical, and spectral analyses. The spectral data showed that the ligand behaves as either neutral tridentate ligand as in complexes 2-5 with the general formula $[H_4LMX_2(H_2O)]{\cdot}nH_2O$ (M=Cu(II), Ni(II), Co(II), X = Cl or $NO_3$), neutral hexadentate ligand as in complexes 10-12 with the general formula $[H_4LM_2Cl_6]{\cdot}nH_2O$ (M=Fe(III), Cr(III) or Ru(III)), or dibasic hexadentate ligand as in complexes 6-9 with the general formula $[H_2LM_2Cl_2(H_2O)_4]{\cdot}nH_2O$ (M = Cu(II), Ni(II), Co(II) or Mn(II), and 13 with general formula $[H_4L(ZrO)_2Cl_2]{\cdot}8H_2O$. Molar conductance in DMF solution indicated the non-ionic nature of the complexes. The ESR spectra of solid copper(II) complexes 2, 5, and 6 showed $g_{\parallel}$ >g> $g_e$, indicating distorted octahedral structure and the presence of the unpaired electron in the $N^1,N^2$ orbital with significant covalent bond character. For the dimeric copper(II) complex $[H_2LCu_2Cl_2(H_2O)_4]{\cdot}3H_2O$ (6), the distance between the two copper centers was calculated using field zero splitting parameter for the parallel component that was estimated from the ESR spectrum. The antibacterial and antifungal activities of the compounds showed that, some of metal complexes exhibited a greater inhibitory effect than standard drug as tetracycline (bacteria) and Amphotricene B (fungi).