The synthesis and characterization of 1,1-bis(aminomethyl)cyclohexaneplatinum(II) compounds and the crystal structure determination of 1,1-bis(aminomethyl)-cyclohexaneaquosulphatoplatinum(II) monohydrate

Harry A. Meinema, François Verbeek, Jan W. Marsman, Eric J. Bulten, James C. Dabrowiak, Bala S. Krishnan, Anthony L. Spek

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Abstract

The synthesis and characterization of a number of 1,1-bis(aminomethylcyclohexane)platinum(II) complexes is described. Reaction of 1,1-bis(aminomethyl- cyclohexane)dichloroplatinum(II) (LPtCl2) with silver sulphate and silver nitrate in water results in the isolation of the corresponding aquosulphato·monohydrate, LPt(H2O)SO4·H2O and dinitratoplatinum- (II), LPt(NO3)2, complexes. Treatment of aqueous solutions of these compounds with an equimolar amount of sodium hydroxide results in the formation of mixtures of hydroxo-bridged dimers and trimers. The less soluble cyclic trimeric species [LPt(μ-OH)]3(NO3)3·2H2O and {[LPt(μ-OH)]3}2(SO4)3ṡ8H2O have been isolated. The 1H, 13C and 195Pt NMR spectra of the various compounds have been studied in D2O. In particular, 195Pt NMR is a valuable tool for identification of the various platinum complexes present in aqueous solution. IR spectral data are reported. The IR spectra of LPt(SO4)ṡxH2O containing varying amounts of water of crystallization and/or coordination are discussed. In LPt(H2O)SO4ṡH2O the symmetry of the monodentate SO4 ligand appears to be lowered as a result of strong hydrogen bonding to the water molecules. The crystal structure of this compound has been determined by single-crystal X-ray diffraction. The monoclinic crystal, space group P21/c, has cell dimensions a = 13.615(9), b = 7.372(1), c = 14.702(2) Å, β = 109.26(4)° and has four formula units in the unit cell. The structure was solved by standard methods and refined to R = 0.0337 based on 2671 reflections. The coordination of the metal atom is square planar with two nitrogen atoms, one oxygen of a water molecule and one oxygen of the sulfate anion being bound to platinum(II). There is extensive inter- and intramolecular hydrogen bonding.

Original languageEnglish (US)
Pages (from-to)127-135
Number of pages9
JournalInorganica Chimica Acta
Volume114
Issue number2
DOIs
StatePublished - Apr 15 1986

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Crystal structure
Platinum
crystal structure
platinum
Water
Hydrogen Bonding
synthesis
water
Sulfates
sulfates
Hydrogen bonds
Silver
Nuclear magnetic resonance
Oxygen
aqueous solutions
Silver Nitrate
Atoms
Sodium Hydroxide
silver nitrates
nuclear magnetic resonance

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

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The synthesis and characterization of 1,1-bis(aminomethyl)cyclohexaneplatinum(II) compounds and the crystal structure determination of 1,1-bis(aminomethyl)-cyclohexaneaquosulphatoplatinum(II) monohydrate. / Meinema, Harry A.; Verbeek, François; Marsman, Jan W.; Bulten, Eric J.; Dabrowiak, James C.; Krishnan, Bala S.; Spek, Anthony L.

In: Inorganica Chimica Acta, Vol. 114, No. 2, 15.04.1986, p. 127-135.

Research output: Contribution to journalArticle

Meinema, Harry A. ; Verbeek, François ; Marsman, Jan W. ; Bulten, Eric J. ; Dabrowiak, James C. ; Krishnan, Bala S. ; Spek, Anthony L. / The synthesis and characterization of 1,1-bis(aminomethyl)cyclohexaneplatinum(II) compounds and the crystal structure determination of 1,1-bis(aminomethyl)-cyclohexaneaquosulphatoplatinum(II) monohydrate. In: Inorganica Chimica Acta. 1986 ; Vol. 114, No. 2. pp. 127-135.
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abstract = "The synthesis and characterization of a number of 1,1-bis(aminomethylcyclohexane)platinum(II) complexes is described. Reaction of 1,1-bis(aminomethyl- cyclohexane)dichloroplatinum(II) (LPtCl2) with silver sulphate and silver nitrate in water results in the isolation of the corresponding aquosulphato·monohydrate, LPt(H2O)SO4·H2O and dinitratoplatinum- (II), LPt(NO3)2, complexes. Treatment of aqueous solutions of these compounds with an equimolar amount of sodium hydroxide results in the formation of mixtures of hydroxo-bridged dimers and trimers. The less soluble cyclic trimeric species [LPt(μ-OH)]3(NO3)3·2H2O and {[LPt(μ-OH)]3}2(SO4)3ṡ8H2O have been isolated. The 1H, 13C and 195Pt NMR spectra of the various compounds have been studied in D2O. In particular, 195Pt NMR is a valuable tool for identification of the various platinum complexes present in aqueous solution. IR spectral data are reported. The IR spectra of LPt(SO4)ṡxH2O containing varying amounts of water of crystallization and/or coordination are discussed. In LPt(H2O)SO4ṡH2O the symmetry of the monodentate SO4 ligand appears to be lowered as a result of strong hydrogen bonding to the water molecules. The crystal structure of this compound has been determined by single-crystal X-ray diffraction. The monoclinic crystal, space group P21/c, has cell dimensions a = 13.615(9), b = 7.372(1), c = 14.702(2) {\AA}, β = 109.26(4)° and has four formula units in the unit cell. The structure was solved by standard methods and refined to R = 0.0337 based on 2671 reflections. The coordination of the metal atom is square planar with two nitrogen atoms, one oxygen of a water molecule and one oxygen of the sulfate anion being bound to platinum(II). There is extensive inter- and intramolecular hydrogen bonding.",
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T1 - The synthesis and characterization of 1,1-bis(aminomethyl)cyclohexaneplatinum(II) compounds and the crystal structure determination of 1,1-bis(aminomethyl)-cyclohexaneaquosulphatoplatinum(II) monohydrate

AU - Meinema, Harry A.

AU - Verbeek, François

AU - Marsman, Jan W.

AU - Bulten, Eric J.

AU - Dabrowiak, James C.

AU - Krishnan, Bala S.

AU - Spek, Anthony L.

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N2 - The synthesis and characterization of a number of 1,1-bis(aminomethylcyclohexane)platinum(II) complexes is described. Reaction of 1,1-bis(aminomethyl- cyclohexane)dichloroplatinum(II) (LPtCl2) with silver sulphate and silver nitrate in water results in the isolation of the corresponding aquosulphato·monohydrate, LPt(H2O)SO4·H2O and dinitratoplatinum- (II), LPt(NO3)2, complexes. Treatment of aqueous solutions of these compounds with an equimolar amount of sodium hydroxide results in the formation of mixtures of hydroxo-bridged dimers and trimers. The less soluble cyclic trimeric species [LPt(μ-OH)]3(NO3)3·2H2O and {[LPt(μ-OH)]3}2(SO4)3ṡ8H2O have been isolated. The 1H, 13C and 195Pt NMR spectra of the various compounds have been studied in D2O. In particular, 195Pt NMR is a valuable tool for identification of the various platinum complexes present in aqueous solution. IR spectral data are reported. The IR spectra of LPt(SO4)ṡxH2O containing varying amounts of water of crystallization and/or coordination are discussed. In LPt(H2O)SO4ṡH2O the symmetry of the monodentate SO4 ligand appears to be lowered as a result of strong hydrogen bonding to the water molecules. The crystal structure of this compound has been determined by single-crystal X-ray diffraction. The monoclinic crystal, space group P21/c, has cell dimensions a = 13.615(9), b = 7.372(1), c = 14.702(2) Å, β = 109.26(4)° and has four formula units in the unit cell. The structure was solved by standard methods and refined to R = 0.0337 based on 2671 reflections. The coordination of the metal atom is square planar with two nitrogen atoms, one oxygen of a water molecule and one oxygen of the sulfate anion being bound to platinum(II). There is extensive inter- and intramolecular hydrogen bonding.

AB - The synthesis and characterization of a number of 1,1-bis(aminomethylcyclohexane)platinum(II) complexes is described. Reaction of 1,1-bis(aminomethyl- cyclohexane)dichloroplatinum(II) (LPtCl2) with silver sulphate and silver nitrate in water results in the isolation of the corresponding aquosulphato·monohydrate, LPt(H2O)SO4·H2O and dinitratoplatinum- (II), LPt(NO3)2, complexes. Treatment of aqueous solutions of these compounds with an equimolar amount of sodium hydroxide results in the formation of mixtures of hydroxo-bridged dimers and trimers. The less soluble cyclic trimeric species [LPt(μ-OH)]3(NO3)3·2H2O and {[LPt(μ-OH)]3}2(SO4)3ṡ8H2O have been isolated. The 1H, 13C and 195Pt NMR spectra of the various compounds have been studied in D2O. In particular, 195Pt NMR is a valuable tool for identification of the various platinum complexes present in aqueous solution. IR spectral data are reported. The IR spectra of LPt(SO4)ṡxH2O containing varying amounts of water of crystallization and/or coordination are discussed. In LPt(H2O)SO4ṡH2O the symmetry of the monodentate SO4 ligand appears to be lowered as a result of strong hydrogen bonding to the water molecules. The crystal structure of this compound has been determined by single-crystal X-ray diffraction. The monoclinic crystal, space group P21/c, has cell dimensions a = 13.615(9), b = 7.372(1), c = 14.702(2) Å, β = 109.26(4)° and has four formula units in the unit cell. The structure was solved by standard methods and refined to R = 0.0337 based on 2671 reflections. The coordination of the metal atom is square planar with two nitrogen atoms, one oxygen of a water molecule and one oxygen of the sulfate anion being bound to platinum(II). There is extensive inter- and intramolecular hydrogen bonding.

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