Complexes of divalent platinum with diphenylphosphineacetic acid

1981 ◽  
Vol 46 (5) ◽  
pp. 1222-1228 ◽  
Author(s):  
Jiří Pangrác ◽  
Jana Podlahová
Keyword(s):  
Nmr Spectra ◽  
Square Planar ◽  
Divalent Platinum

Diphenylphosphineacetic acid (HA) acts as a monodentate P-donor towards divalent platinum; the anion acts as a bidentate P,O-donor. Three types of complexes have been prepared, PtX2(HA)2, PtXA(HA) and PtA2 (X = Cl, Br, I, SCN), whose formation is determined primarily by the type of X, the acidity of the medium and the polarity of the solvent. It follows from electronic, infrared and 31P-NMR spectra that all the prepared complexes are cis-square planar in structure.

Purine complexes of platinum: synthesis, nmr, and crystal and molecular structures of cis-chloro(caffeine)bis(triethylphosphine)platinum(II) fluoroborate and cis-bis(isocaffeine)bis(triethylphosphine)platinum (II) fluoroborate

1983 ◽  
Vol 61 (6) ◽  
pp. 1132-1141 ◽  
Author(s):  
Gordon William Bushnell ◽  
Roderick James Densmore ◽  
Keith Roger Dixon ◽  
Arthur Charles Ralfs
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Molecular Structures ◽  
Platinum Drugs ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Antitumour Agents ◽  
Crystal And Molecular Structures ◽  
Square Planar

Synthesis and 31P nmr spectra of the complex cations, cis-[PtCl(L)(PEt3)2]+, L= theophylline, caffeine, or isocaffeine, and cis[Pt(isocaff)2(PEt3)2]2+ are reported. The crystal structure of cis-[PtCl(caffeine)(PEt3)2][BF4] is determined, space group [Formula: see text], a = 1.1766(6), b = 1.4428(5), c = 0.9002(4) nm, α = 97.28(4)°, β = 97.69(4)°, γ = 100.96(5)°, Dm = 1.649 g cm−1, the bond lengths are Pt—Cl= 233.4(4) pm, Pt—N = 215(1) pm, Pt—P = 225.4(5) pm (mean), and the residual R = 0.071. The crystal structure of cis-[Pt(isocaffeine)2(PEt3)2][BF4]2 is orthorhombic, space group Pbca, a = 2.317(3), b = 1.717(3), c = 2.130(3) nm, Dm = 1.574 g cm−3, with an opposing isocaffeine conformation, bond lengths Pt—N = 211(2) pm, Pt—P = 227.6(9) pm (mean), and R = 0.073. Both crystal structures contain approximately square planar Pt(II) coordination with the purine coordinated via an imidazole nitrogen. The structures are discussed as models for the possible involvement of [Formula: see text] chelation of guanine to platinum when platinum drugs act as antitumour agents, but there is no evidence that isocaffeine acts as an [Formula: see text] chelate.

Darstellung und Kristallstrukturen einiger Übergangsmetall-Komplexverbindungen mit Liganden mit dem 4,5-Benzo-3-methyl-1,3,2-oxazaphosphorinan-6-on-Gerüst / Synthesis and X-Ray Crystal Structures of Some Transition-Metal Complexes Involving Ligands with the 4,5-Benzo-3-methyl-1,3,2-oxazaphosphorinan-6-one Framework

1994 ◽  
Vol 49 (11) ◽  
pp. 1481-1493 ◽  
Author(s):  
Axel Fischer ◽  
Ion Neda ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Transition Metal ◽  
Single Crystal ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Coordination Geometry ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Envelope Conformation ◽  
Square Planar ◽  
Distorted Octahedral

4,5-Benzo-2-diethylamino-3-methyl-1,3,2-oxazaphosphorinan-6-one 1 and 4,5-benzo-2-[bis- (2-chlorethyl)amino]-3-methyl-1,3,2-oxazaphosphorinan-6-one 3 reacted with dichloro- (cycloocta-1,5-diene)platinum(II) [(COD)PtCl2] to give the ds-dichloro-platinum(II) com­plexes 2 and 4, respectively. The reaction of 1 with tricarbonyl(cycloheptatriene)molybdenum(0) led to a mixture of isomers including fac-tris-(4,5-benzo-2-diethylamino-3-methyl- 1,3,2-oxazaphosphorinan-6-one)tricarbonylmolybdenum(0) 5. The reaction of 4,5-benzo- 2-acetylamino-3-methyl-1,3,2-oxazaphosphorinan-6-one 6 with dichloro(cycloocta-1,5-diene)- platinum(II) furnished the cis-complex 7. 4,5-Benzo-2-fluoro-3-methyl-1,3,2-oxazaphosphorinan-6-one 8 reacted with both tetracarbonyl(norbornadiene)molybdenum(0) and dichloro- (cycloocta-1,5-diene)platinum(II) to form the cis-complexes 9 and 10. 31P-31P coupling con­stants from the 31P NMR spectra for the complexes 2, 4 and 9 are reported. The structures of 5, 7, 9 and 10 were established by single crystal X-ray analysis. All ligands coordinate via phosphorus only. The structure of 5 shows strongly distorted octahedral coordination geome­try associated with the presence of three bulky ligands. The Mo-P bond lengths in 5 are, for the same reason, significantly longer than in 9. The heterocycles of the ligands in 5 do not show the expected envelope conformation but are almost planar. The platinum(II) complex 7 shows crystallographic C2-symmetry, the coordination geometry at platinum being almost ideally square-planar. The same coordination geometry is observed for 10, the ligands of which possess the expected envelope conformation with phosphorus out of the plane.

scholarly journals Synthesis, Characterization, and Antimicrobial Activity Studies of Ni(II) Complex with Pyridine as a Ligand

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Faridul Islam ◽  
Md. Amran Hossain ◽  
Nur Mostaq Shah ◽  
Hridika Talukder Barua ◽  
Md. Alamgir Kabir ◽  
...  
Keyword(s):  
Antimicrobial Activity ◽  
Nmr Spectra ◽  
Conductivity Measurement ◽  
Molar Conductivity ◽  
Molecular Formula ◽  
H Nmr ◽  
Square Planar ◽  
Elemental Analyses ◽  
Prepared Complex ◽  
C Nmr

We represent a metal complex which has been synthesized by the simple reaction with Ni(II) chloride and pyridine (as a lignd) affording a complex having the molecular formula [NiC5H5N2Cl2], characterized on the basis of elemental analyses, electronic, infrared,1H NMR,13C NMR spectra, magnetic susceptibility, and also aid of molar conductivity measurement. Conductivity measurement reveals nonelectrolytic nature of the complex. IR and13C NMR spectra reveal the presence ofcis- andtrans-structure. On the basis of above analyses the square planarcis- andtrans-structures are proposed for the prepared complex.

Fluxional behaviour of potentially bidentate phenanthroline, naphthyridine, and phthalazine ligands in palladium complexes

1978 ◽  
Vol 56 (7) ◽  
pp. 950-953 ◽  
Author(s):  
J. Bradley Brandon ◽  
Michael Collins ◽  
Keith R. Dixon
Keyword(s):  
Nmr Spectra ◽  
Variable Temperature ◽  
Palladium Complexes ◽  
Exchange Mechanism ◽  
Heterocyclic Ligands ◽  
Planar Structures ◽  
Square Planar ◽  
Intramolecular Process

The synthesis of a series of palladium complexes, cis-[PdCl(PEt3)2L][Y]; L = 1,10-phenanthroline, 1,8-naphthyridine, or phthalazine; Y = BF4− or ClO4−; is reported. Variable temperature 1H and 31P nmr spectra are discussed in terms of square planar structures in which the heterocyclic ligands are essentially monodentate and fluxional with the palladium exchanging between the two nitrogen atoms. Above ca. −10 °C a dissociative exchange mechanism operates in all three complexes and, when L = 1,10-phenanthroline or 1,8-naphthyridine, exchange continues at lower temperatures by an intramolecular process.

scholarly journals Synthesis and Cytotoxicity of Platinum(II) Complexes of 3-Aminocyclopentanespiro- 5-hydantoin and 3-Aminocycloheptanespiro-5-hydantoin

2003 ◽  
Vol 58 (1-2) ◽  
pp. 103-108 ◽  
Author(s):  
Daniel Kushev ◽  
Emilya Naydenova ◽  
Julita Popova ◽  
Liliana Maneva ◽  
Konstantin Grancharov ◽  
...  
Keyword(s):  
Antibacterial Activity ◽  
Cell Growth ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
In Vitro Cytotoxicity ◽  
Bacterial Strains ◽  
Macromolecular Synthesis ◽  
Square Planar ◽  
Murine Erythroleukemia

Four new platinum(II) complexes of 3-aminocyclopentanespiro-5-hydantoin (acpsh) and 3-aminocycloheptanespiro-5-hydantoin (achpsh) were synthesized and characterized by elemental analysis, IR and 1NMR spectra. The spectral analyses indicated a cis-square planar structure of the complexes with ligands coordinated via the NH2 group. The complexes were evaluated for in vitro cytotoxicity in murine erythroleukemia (MEL) cells, clone F4N, using cell-growth and macromolecular synthesis assay. The compounds, with exception of [Pt(NH3)(achpsh)Cl2] (IV), exhibited much lower cytotoxicity than that of cisplatin (DDP). Compound IV was nearly as cytotoxic as DDP. The new complexes exerted low antibacterial activity as assessed by seven bacterial strains

scholarly journals Synthesis of N,O-Chelating Hydrazidopalladium Complexes from 1,2-Bis(trifluoroacetyl)hydrazine

Inorganics ◽  
2021 ◽  
Vol 9 (10) ◽  
pp. 76
Author(s):  
Yoshihito Kayaki ◽  
Tomohiro Hayakawa ◽  
Takao Ikariya
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Nmr Spectra ◽  
Structural Changes ◽  
Variable Temperature ◽  
Palladium Complexes ◽  
Electron Donors ◽  
Crystal Structure Determination ◽  
X Ray ◽  
Square Planar

N,O-chelating dicarbonylhydrazido-palladium complexes were synthesized by treatment of 1,2-bis(trifluoroacetyl)hydrazine with a mixture of a Pd(0) source, [Pd(dba)2] (DBA = dibenzylideneacetone), and four-electron donors including 1,3-bis(diphenylphosphino)propane (DPPP), N,N,N’,N’-tetramethylethylenediamine (TMEDA), and two equivalents of triphenylphosphine. The same products from DPPP and TMEDA could be obtained alternatively by using Pd(OAc)2 through deprotonation of the diacylhydrazine. The five-membered chelate structure was confirmed by NMR spectra and X-ray crystal structure determination. The X-ray structures indicate that the products are formally considered as Pd(II) complexes with a hydrazido(2–) ligand. In the case of the triphenylphosphine-coordinated complex, a fluxional behavior in dichloromethane-d2 was observed by variable temperature NMR experiments, possibly due to structural changes between the square planar and pseudo-tetrahedral geometries.

Complexes of dodecamethylcyclohexaphosphazene with palladium(II) chloride and platinum(II) chloride. Crystal and molecular structure of cis-dichloro[η2-dodecamethylcyclohexaphosphazene (N,N′)] palladium(II) sesquihydrate

1981 ◽  
Vol 59 (16) ◽  
pp. 2429-2434 ◽  
Author(s):  
Norman L. Paddock ◽  
T. N. Ranganathan ◽  
Steven J. Rettig ◽  
Rajendra D. Sharma ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Order ◽  
Nmr Spectra ◽  
Crystal And Molecular Structure ◽  
Model Calculations ◽  
Full Matrix ◽  
X Ray ◽  
Square Planar ◽  
The Mean ◽  
C Nmr

Dodecamethylcyclohexaphosphazene N6P6Me12, 1, forms 1:1 complexes with palladium(II) chloride, 2, and platinum(II) chloride, 3. Their 31P, 1H, and 13C nmr spectra show them to be rigid molecules in solution, with an approximate plane of symmetry. Crystals of 2 are orthorhombic, a = 17.4030(3), b = 15.4897(5), c = 10.7417(2) Å, Z = 4, space group P21212. The structure was determined from diffractometer X-ray data and refined by full-matrix least-squares methods to R = 0.031 for 3545 reflections with I ≥ 3σ(I). The metal atom has square planar coordination, and forms 6- and 10-membered chelate rings with the phosphazene ligand. The mean P—N bond length is 1.609 Å; the variation of bond lengths within the ring is consistent with model calculations of changes in bond order arising from the localization of bonding electrons.

Palladium(II) and Platinum(II) Complexes of N-3-Pyridinylmethanesulfonamide

2001 ◽  
Vol 56 (11) ◽  
pp. 1217-1226
Author(s):  
Nicolay I. Dodoff
Keyword(s):  
Nitrogen Atom ◽  
Ir Spectra ◽  
Electric Conductivity ◽  
Elemental Analysis ◽  
Nmr Spectra ◽  
Pyridine Nitrogen Atom ◽  
Normal Coordinate ◽  
H Nmr ◽  
Pyridine Nitrogen ◽  
Square Planar

The complexes cis-[Pd(PMSA)2Cl2] cis-[Pt(PMSA)2X2], trans-[Pt(PMSA)2I2] and [Pt(PMSA)4]Cl2 (PMSA = N-3-pyridinylmethanesulfonamide; X = Cl, Br, I) have been synthesized and characterized by elemental analysis, molar electric conductivity, IR and 1H NMR spectra. A detailed assignment of the IR spectra (4000-150 cm-1) of the complexes, supported by an approximate normal coordinate analysis, has been performed. The complexes are of square-planar type and the PMSA ligand is coordinated via the pyridine nitrogen atom.

scholarly journals [AU(DIEN)Cl]Cl2: Exchange Phenomena Observed by H1 and C13 NMR Spectroscopy

1999 ◽  
Vol 6 (4-5) ◽  
pp. 261-269 ◽  
Author(s):  
Sabine L. Best ◽  
Zijian Guo ◽  
Milos I. Djuran ◽  
Peter J. Sadler
Keyword(s):  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Variable Temperature ◽  
Hydroxo Complex ◽  
Acidic Solutions ◽  
Exchange Effects ◽  
Square Planar ◽  
Ph Range ◽  
Solution Behaviour

The solution behaviour of the square-planar gold(III) complex [Au(dien)Cl]Cl2 (dien = 1,5- diamino-3-azapentane) was investigated by H1 and C13 NMR spectroscopy. We have found that H1 NMR spectra of [Au(dien)Cl]Cl2 are characterised by exchange behaviour over the whole pH range, and some exchange effects are also seen in C13 NMR spectra of the deprotonated hydroxo derivative of the complex in alkaline solution. An exchange rate of > 378 s-1 was determined from H1 NMR spectra at pH∗2 (coalescence temperature 40C° ). In slightly acidic solutions of the complex, H1 chemical shifts are in accordance with the known deprotonation of the central amine group of the complexed diethylenetriamine ligand. In C13 NMR spectra, two separate sets of resonances are observed for the chloro and the hydroxo complex of gold(III) diethylenetriamine. The hydroxo complex [Au(dien-H)OH]+ shows exchange effects in C13 NMR spectra. Variable temperature studies show the carbon atoms next to the central secondary amine to be inequivalent and each present in two different environments that are in intermediate to fast exchange on the NMR time-scale.

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