Synthesis, structural characterization and cytotoxic activity of two new organoruthenium(II) complexes

Two new p-cymene ruthenium(II) complexes containing as additional ligands N-methylpiperazine ([(?6-p-cymene)RuCl2(CH3NH(CH2)4NH)]PF6, complex 1) or vitamin K3-thiosemicarbazone ([(?6-p-cymene)RuCl2(K3tsc)], complex 2) were synthesized starting from [(?6-p-cymene)2RuCl2]2 and the corresponding ligand. The complexes were characterized by elemental analysis, IR, electronic absorption and NMR spectroscopy. The X-ray crystal structure determination of complex 1 revealed ?piano-stool? geometry. The differences in the cytotoxic activity of the two complexes are discussed in terms of the ligand present.

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THE NMR SPECTROSCOPY AND X-RAY CRYSTAL STRUCTURE DETERMINATION OF TWO ISOMERIC FORMS OF THE DIOXODIPHOSPHORUS MACROCYCLE 5,13-DIPHENYL-1,9-DIOXA-5,13-DIPHOSPHACYCLOHEXADECANE-5,13-DIOXIDE

Phosphorus Sulfur and Silicon and the Related Elements ◽

10.1080/10426509408036925 ◽

1994 ◽

Vol 88 (1-4) ◽

pp. 225-231 ◽

Cited By ~ 1

Author(s):

Henri J. Cristau ◽

Patrick Mouchet ◽

Wan-Sheung Li ◽

Mary McPartlin ◽

Ian J. Scowen

Keyword(s):

Crystal Structure ◽

Nmr Spectroscopy ◽

Structure Determination ◽

Crystal Structure Determination ◽

X Ray

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A simple molecule with a complex crystal structure: interplay of31P solid-state NMR spectroscopy and single-crystal x-ray diffraction in the structure determination of a ruthenium diphosphine diamine complex

Magnetic Resonance in Chemistry ◽

10.1002/mrc.1433 ◽

2004 ◽

Vol 42 (9) ◽

pp. 807-813 ◽

Cited By ~ 9

Author(s):

Klaus Eichele ◽

Christiane Nachtigal ◽

Susanne Jung ◽

Hermann A. Mayer ◽

Ekkehard Lindner ◽

...

Keyword(s):

Crystal Structure ◽

Solid State ◽

Nmr Spectroscopy ◽

Structure Determination ◽

Solid State Nmr ◽

X Ray Diffraction ◽

X Ray ◽

Complex Crystal Structure ◽

Complex Crystal

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The protonation of the ethylenediphosphinetetraacetate anion and the crystal structure of the bis (hydrogen bromide) of ethylenediphosphinetetraacetic acid

Collection of Czechoslovak Chemical Communications ◽

10.1135/cccc19813063 ◽

1981 ◽

Vol 46 (12) ◽

pp. 3063-3073 ◽

Cited By ~ 5

Author(s):

Jana Podlahová ◽

Bohumil Kratochvíl ◽

Vratislav Langer ◽

Josef Šilha ◽

Jaroslav Podlaha

Keyword(s):

Crystal Structure ◽

Hydrogen Bonds ◽

Structure Determination ◽

Free Acid ◽

Hydrogen Bromide ◽

Carboxyl Groups ◽

Spectroscopic Methods ◽

X Ray ◽

Partial Formation

The equilibria and mechanism of addition of protons to the ethylenediphosphinetetraacetate anion (L4-) were studied in solution by the UV, IR, 1H and 31P NMR spectroscopic methods. A total of six protons can be bonded to the anion. They are added stepwise, first with partial formation of zwitterions containing P-H bonds, which then dissociate with formation of the free acid, H4L, where all four protons are bonded in carboxyl groups. The formation of zwitterions is strongly dependent on the concentration. In the final stage, the acid bonds two additional protons to form the bis-phosphonium cation, H6L2+. A number of isostructural salts containing this cation, H4L.2 HX (X = Cl, Br, I), have been prepared. The X-ray crystal structure determination of the bromide confirmed the expected arrangement. The bromide crystals are monoclinic, a = 578.2, b = 1 425.0, c = 1 046.7 pm, β = 103.07° with a space group of P21/c, Z = 2. The final R factor was 0.059 based on 1 109 observed reflections. The structure consists of H6L2+ cations containing protons bonded to phosphorus atoms (P-H distance 134 pm) and of bromide anions, located in gaps which are also sufficiently large for I- anions in the isostructural iodide. The interbonding of phosphonium cations proceeds through hydrogen bonds, C-OH...O=C, in which the O...O distance is 275.3 pm.

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