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Jose M Goicoechea - One of the best experts on this subject based on the ideXlab platform.
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heteroatomic molecular clusters derived from group 15 zintl ion cages synthesis and isolation of m2 hp7 2 2 m ag au two novel cluster anions exhibiting metallophilic interactions
Inorganic Chemistry, 2011Co-Authors: Caroline M Knapp, Charlotte S Jackson, Joseph S Large, Amber L Thompson, Jose M GoicoecheaAbstract:Ethylenediamine (en) solutions of K3P7 and 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) were reacted with the homoleptic group 11 complexes [M(nbe)3][SbF6] (M = Ag, Au; nbe = norbornene) yielding two novel cluster anions, [M2(HP7)2]2−, both of which were isolated in low crystalline yields as [K(2,2,2-crypt)]2[M2(HP7)2] (M = Ag (1) and Au (2)). Optimization of the reaction conditions by incorporation of a proton source (ammonium tetraphenylborate) and the replacement of the light-sensitive nbe adducts of silver and gold with the chloride salts MCl (M = Ag, Au) was found to greatly increase the yield and purity in which 1 and 2 were isolated. Compounds 1 and 2 were characterized by single crystal X-ray diffraction, electrospray ionization mass-spectrometry (ESI− MS), elemental analysis, and 1H and 31P NMR spectroscopy. Density functional theory (DFT) calculations on the cluster anions were also conducted.
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experimental and computational study of the structural and electronic properties of fe ii 2 2 bipyridine mes 2 and fe ii 2 2 bipyridine mes 2 a complex containing a 2 2 bipyridyl radical anion
Inorganic Chemistry, 2010Co-Authors: Mark Irwin, Mark S Denning, Rhiannon K Jenkins, Tobias Kramer, Fernande Grandjean, Gary J Long, Radovan Herchel, John E Mcgrady, Jose M GoicoecheaAbstract:Addition of potassium metal and 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) to a tetrahydrofuran (THF) solution of Fe(2,2′-bipyridine)(mes)2 (1; mes = 2,4,6-Me3C6H2) yielded the anionic complex [Fe(2,2′-bipyridine)(mes)2]− which was isolated as [K(2,2,2-crypt)][Fe(2,2′-bipyridine)(mes)2] (2) alongside the side-product [K(2,2,2-crypt)][Fe(mes)3]·C6H12 (3). A compositionally pure sample of 2 was obtained by dissolving a mixture of 2 and 3 in dry pyridine and layering the resulting solution with toluene. Solid state magnetic susceptibility measurements on 1 reveal Curie−Weiss paramagnetic behavior with a molar magnetic moment of 5.12(1) μB between 20 and 300 K, a value which is in line with the expected iron(II) spin-only value of 4.90 μB. The magnetic measurements carried out on 2 reveal more complex temperature dependent behavior consistent with intramolecular antiferromagnetic coupling (J = −46 cm−1) between the unpaired electrons of the iron(II) ion (SFe = 2) and a π* orbital...
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synthesis and isolation of fe ge 10 3 a pentagonal prismatic zintl ion cage encapsulating an interstitial iron atom
Journal of the American Chemical Society, 2009Co-Authors: Binbin Zhou, Mark S Denning, Deborah L Kays, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K4Ge9 with FeAr2 (Ar = 2,6-Mes2C6H3) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge10]3− (1) which was crystallographically characterized as a [K(2,2,2-crypt)]+ salt in [K(2,2,2-crypt)]3[Fe@Ge10]•2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
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Synthesis and isolation of [Fe@Ge(10)](3-): a pentagonal prismatic Zintl ion cage encapsulating an interstitial iron atom.
'American Chemical Society (ACS)', 2009Co-Authors: Zhou B, Deborah L Kays, Denning Ms, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K(4)Ge(9) with FeAr(2) (Ar = 2,6-Mes(2)C(6)H(3)) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge(10)](3-) (1) which was crystallographically characterized as a [K(2,2,2-crypt)](+) salt in [K(2,2,2-crypt)](3)[Fe@Ge(10)]*2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry
Mark S Denning - One of the best experts on this subject based on the ideXlab platform.
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experimental and computational study of the structural and electronic properties of fe ii 2 2 bipyridine mes 2 and fe ii 2 2 bipyridine mes 2 a complex containing a 2 2 bipyridyl radical anion
Inorganic Chemistry, 2010Co-Authors: Mark Irwin, Mark S Denning, Rhiannon K Jenkins, Tobias Kramer, Fernande Grandjean, Gary J Long, Radovan Herchel, John E Mcgrady, Jose M GoicoecheaAbstract:Addition of potassium metal and 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) to a tetrahydrofuran (THF) solution of Fe(2,2′-bipyridine)(mes)2 (1; mes = 2,4,6-Me3C6H2) yielded the anionic complex [Fe(2,2′-bipyridine)(mes)2]− which was isolated as [K(2,2,2-crypt)][Fe(2,2′-bipyridine)(mes)2] (2) alongside the side-product [K(2,2,2-crypt)][Fe(mes)3]·C6H12 (3). A compositionally pure sample of 2 was obtained by dissolving a mixture of 2 and 3 in dry pyridine and layering the resulting solution with toluene. Solid state magnetic susceptibility measurements on 1 reveal Curie−Weiss paramagnetic behavior with a molar magnetic moment of 5.12(1) μB between 20 and 300 K, a value which is in line with the expected iron(II) spin-only value of 4.90 μB. The magnetic measurements carried out on 2 reveal more complex temperature dependent behavior consistent with intramolecular antiferromagnetic coupling (J = −46 cm−1) between the unpaired electrons of the iron(II) ion (SFe = 2) and a π* orbital...
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synthesis and isolation of fe ge 10 3 a pentagonal prismatic zintl ion cage encapsulating an interstitial iron atom
Journal of the American Chemical Society, 2009Co-Authors: Binbin Zhou, Mark S Denning, Deborah L Kays, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K4Ge9 with FeAr2 (Ar = 2,6-Mes2C6H3) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge10]3− (1) which was crystallographically characterized as a [K(2,2,2-crypt)]+ salt in [K(2,2,2-crypt)]3[Fe@Ge10]•2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
Binbin Zhou - One of the best experts on this subject based on the ideXlab platform.
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synthesis and isolation of fe ge 10 3 a pentagonal prismatic zintl ion cage encapsulating an interstitial iron atom
Journal of the American Chemical Society, 2009Co-Authors: Binbin Zhou, Mark S Denning, Deborah L Kays, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K4Ge9 with FeAr2 (Ar = 2,6-Mes2C6H3) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge10]3− (1) which was crystallographically characterized as a [K(2,2,2-crypt)]+ salt in [K(2,2,2-crypt)]3[Fe@Ge10]•2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
Deborah L Kays - One of the best experts on this subject based on the ideXlab platform.
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synthesis and isolation of fe ge 10 3 a pentagonal prismatic zintl ion cage encapsulating an interstitial iron atom
Journal of the American Chemical Society, 2009Co-Authors: Binbin Zhou, Mark S Denning, Deborah L Kays, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K4Ge9 with FeAr2 (Ar = 2,6-Mes2C6H3) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge10]3− (1) which was crystallographically characterized as a [K(2,2,2-crypt)]+ salt in [K(2,2,2-crypt)]3[Fe@Ge10]•2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry.
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Synthesis and isolation of [Fe@Ge(10)](3-): a pentagonal prismatic Zintl ion cage encapsulating an interstitial iron atom.
'American Chemical Society (ACS)', 2009Co-Authors: Zhou B, Deborah L Kays, Denning Ms, Jose M GoicoecheaAbstract:Reaction of an ethylenediamine (en) solution of the Zintl phase precursor K(4)Ge(9) with FeAr(2) (Ar = 2,6-Mes(2)C(6)H(3)) in the presence of 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) yielded the endohedral Zintl ion [Fe@Ge(10)](3-) (1) which was crystallographically characterized as a [K(2,2,2-crypt)](+) salt in [K(2,2,2-crypt)](3)[Fe@Ge(10)]*2en. This unprecedented Zintl ion exhibits a pentagonal prismatic 10-atom germanium cage with an interstitial iron atom in the central cavity. Confirmation of the existence of the cluster anion in solution was corroborated by positive and negative ion mode electrospray mass spectrometry
Mark Irwin - One of the best experts on this subject based on the ideXlab platform.
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experimental and computational study of the structural and electronic properties of fe ii 2 2 bipyridine mes 2 and fe ii 2 2 bipyridine mes 2 a complex containing a 2 2 bipyridyl radical anion
Inorganic Chemistry, 2010Co-Authors: Mark Irwin, Mark S Denning, Rhiannon K Jenkins, Tobias Kramer, Fernande Grandjean, Gary J Long, Radovan Herchel, John E Mcgrady, Jose M GoicoecheaAbstract:Addition of potassium metal and 2,2,2-crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]Hexacosane) to a tetrahydrofuran (THF) solution of Fe(2,2′-bipyridine)(mes)2 (1; mes = 2,4,6-Me3C6H2) yielded the anionic complex [Fe(2,2′-bipyridine)(mes)2]− which was isolated as [K(2,2,2-crypt)][Fe(2,2′-bipyridine)(mes)2] (2) alongside the side-product [K(2,2,2-crypt)][Fe(mes)3]·C6H12 (3). A compositionally pure sample of 2 was obtained by dissolving a mixture of 2 and 3 in dry pyridine and layering the resulting solution with toluene. Solid state magnetic susceptibility measurements on 1 reveal Curie−Weiss paramagnetic behavior with a molar magnetic moment of 5.12(1) μB between 20 and 300 K, a value which is in line with the expected iron(II) spin-only value of 4.90 μB. The magnetic measurements carried out on 2 reveal more complex temperature dependent behavior consistent with intramolecular antiferromagnetic coupling (J = −46 cm−1) between the unpaired electrons of the iron(II) ion (SFe = 2) and a π* orbital...