Home The 1-N amides 1∞[Eu2(Pyr)4(PyrH)2(NH3)] · PyrH and [Yb2(Cbz)4(NH2)2(NH3)4] · 3CbzH: Distinctions in the crystal structures, thermal properties and ammonolysis tendency
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The 1-N amides 1∞[Eu2(Pyr)4(PyrH)2(NH3)] · PyrH and [Yb2(Cbz)4(NH2)2(NH3)4] · 3CbzH: Distinctions in the crystal structures, thermal properties and ammonolysis tendency

  • Klaus Müller-Buschbaum and Caterina C. Quitmann
Published/Copyright: September 25, 2009
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Zeitschrift für Kristallographie - Crystalline Materials
From the journal Zeitschrift für Kristallographie - Crystalline Materials Volume 220 Issue 2-3

Abstract

The low-temperature oxidation of the rare earth metals europium and ytterbium with the 1-N amines pyrrole and carbazole in liquid ammonia gave the pyrrolate 1∞[Eu2(Pyr)4(PyrH)2(NH3)] · PyrH (1) (Pyr– = C4H4N–, pyrrolate anion; PyrH = C4H4NH, pyrrole) and the carbazolate [Yb2(Cbz)4(NH2)2(NH3)4] · 3CbzH (2) (Cbz– = C12H8N–, carbazolate; CbzH = C12H8NH), respectively. Though both compounds are ammine complexes, the course through the redox potentials ELn(II/III) as well as the growing steric demand of the ligand result in various differences in the properties of the products. 1 shows a 1-dimensional structure of pyrrolate, pyrrole groups and one equivalent of ammonia coordinating and bridging divalent europium centers. This includes η5 – π-interactions between the metal centers and pyrrolate and pyrrole rings. The resulting polymer shows a rather high thermal stability and melts at 445 °C prior to decomposition under release of ammonia at 475 °C. Contrary to this, 2 contains dimeric units around trivalent ytterbium consisting of carbazolate, ammonia and NH–2 amide groups. No π-interactions are observed. Instead ammonolysis of liquid ammonia results in formation of an amide that contains two different amide groups. The thermal stability of 2 is lower than of 1. The building units of complex 2 decompose at 310 °C without melting. Both compounds were investigated by low-temperature single crystal X-ray analysis, Mid IR, Far IR and Raman spectroscopy as well as simultaneous DTA/TG.

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Published Online: 2009-9-25
Published in Print: 2005-3-1

© 2005 Oldenbourg Wissenschaftsverlag GmbH

Articles in the same Issue

  1. Editorial: Hans-Jörg Deiseroth zum 60. Geburtstag
  2. The coloring problem in intermetallics: bonding and properties of Tb3Zn3.6Al7.4 with the La3Al11 structure type
  3. On the crystal structure of γ-AgMg4
  4. Metallic barrelane: crystal structure, physical properties and bonding analysis of La16Al13
  5. Structural phase transition of CeAuGe at high pressure
  6. Incommensurately modulated CeSi1.82
  7. Cs6[Fe2O6] and Rb4[Fe2O5]: New oxoferrates(III) with edge sharing FeO4 tetrahedra
  8. Crystal structures of M2[B10H10] (M = Na, K, Rb) via real-space simulated annealing powder techniques
  9. The Lewis acid-base adducts of bismuth and aluminium trihalides — crystal structures of [Bi2X4][AlX4]2 (X = Cl, Br)
  10. Solvothermal synthesis, phase transition and crystal structure of β- and γ-CuPb3Br7
  11. The 1-N amides 1∞[Eu2(Pyr)4(PyrH)2(NH3)] · PyrH and [Yb2(Cbz)4(NH2)2(NH3)4] · 3CbzH: Distinctions in the crystal structures, thermal properties and ammonolysis tendency
  12. Tetranuclear [Zr4(OH)8(H2O)16] units in the crystal structure of ZrOI2 · 8 H2O
  13. Single crystal structure refinement of tetramethylammonium-hectorite
  14. Crystal structures of Gd2(Cl3CCOO)6(bipy)2(H2O)2 · 4 bipy, Pr(Cl3CCOO)3(bipy)2, Nd(Cl3CCOO)3(bipy)2 and Er(Cl3CCOO)3(bipy)2(H2O)
  15. [Ba2(C2H6O2)4][Ge2(C2H4O2)6] · 2.5 C2H6O2 – an ethanediolato complex of germanium. Synthesis, thermal decomposition and crystal structure
  16. Synthesis and crystal structure of {[Li(NH3)4]2[18-crown-6]}[Li(NH3)4]2(Sn3ph6)2 · 4 NH3
  17. Nd(NH2SO3)(SO4) · 1.5 H2O: a non-centrosymmetric amidosulfate-sulfate of neodymium
  18. Synthesis of InxGa1–xN solid solutions
  19. Chemical analyses and X-ray diffraction investigations of human hydroxyapatite minerals from aortic valve stenoses
  20. M4,667Ch[SiO4]3 (M = Nd, Sm; Ch = O, S): structural comparison of two apatite-type lanthanoid chalcogenide ortho-oxosilicates
  21. Neutron powder diffraction study on Li1.8Na0.2MgCl4
  22. On the crystal structure of a new modification of 2-amino-4,6-dichloro-1,3,5-triazine
  23. In-situ investigation of oxygen diffusion in Sr, Mg-doped LaGaO3 superionic conductors with a simultaneously applied electric field
  24. Surface dynamics of III—V semiconductors studied by in situ X-ray diffraction during molecular beam epitaxy
  25. The real structure of Na3BiO4 by electron microscopy, HR-XRD and PDF analysis
  26. High-pressure phase transition of the oxonitridosilicate chloride Ce4[Si4O3+xN7–x]Cl1–xOx with x = 0.12 and 0.18
  27. Noncentrosymmetric coordination networks based on nitrate and acetylenedicarboxylate anions
  28. The crystal structure of γ-P4, a low temperature modification of white phosphorus
  29. Phosphorus-rich phosphorus selenides P14+xSe (x = 1, 5)
  30. Crystal structure and optical properties of the new 8O polytype of Ca2Ta2O7
  31. Photoluminescence of ZnGa2S4 : Eu2+
  32. A structural differentiation of quaternary copper argyrodites: Structure — property relations of high temperature ion conductors
  33. In situ bulk structural study on solid-state dynamics and catalytic activity correlations of a H4[PNbMo11O40] partial oxidation catalyst
  34. Structural study of β-Ni(OH)2 and α-Ni(OH)2 variants for electrode applications
https://doi.org/10.1524/zkri.220.2.158.59117

Articles in the same Issue

  1. Editorial: Hans-Jörg Deiseroth zum 60. Geburtstag
  2. The coloring problem in intermetallics: bonding and properties of Tb3Zn3.6Al7.4 with the La3Al11 structure type
  3. On the crystal structure of γ-AgMg4
  4. Metallic barrelane: crystal structure, physical properties and bonding analysis of La16Al13
  5. Structural phase transition of CeAuGe at high pressure
  6. Incommensurately modulated CeSi1.82
  7. Cs6[Fe2O6] and Rb4[Fe2O5]: New oxoferrates(III) with edge sharing FeO4 tetrahedra
  8. Crystal structures of M2[B10H10] (M = Na, K, Rb) via real-space simulated annealing powder techniques
  9. The Lewis acid-base adducts of bismuth and aluminium trihalides — crystal structures of [Bi2X4][AlX4]2 (X = Cl, Br)
  10. Solvothermal synthesis, phase transition and crystal structure of β- and γ-CuPb3Br7
  11. The 1-N amides 1∞[Eu2(Pyr)4(PyrH)2(NH3)] · PyrH and [Yb2(Cbz)4(NH2)2(NH3)4] · 3CbzH: Distinctions in the crystal structures, thermal properties and ammonolysis tendency
  12. Tetranuclear [Zr4(OH)8(H2O)16] units in the crystal structure of ZrOI2 · 8 H2O
  13. Single crystal structure refinement of tetramethylammonium-hectorite
  14. Crystal structures of Gd2(Cl3CCOO)6(bipy)2(H2O)2 · 4 bipy, Pr(Cl3CCOO)3(bipy)2, Nd(Cl3CCOO)3(bipy)2 and Er(Cl3CCOO)3(bipy)2(H2O)
  15. [Ba2(C2H6O2)4][Ge2(C2H4O2)6] · 2.5 C2H6O2 – an ethanediolato complex of germanium. Synthesis, thermal decomposition and crystal structure
  16. Synthesis and crystal structure of {[Li(NH3)4]2[18-crown-6]}[Li(NH3)4]2(Sn3ph6)2 · 4 NH3
  17. Nd(NH2SO3)(SO4) · 1.5 H2O: a non-centrosymmetric amidosulfate-sulfate of neodymium
  18. Synthesis of InxGa1–xN solid solutions
  19. Chemical analyses and X-ray diffraction investigations of human hydroxyapatite minerals from aortic valve stenoses
  20. M4,667Ch[SiO4]3 (M = Nd, Sm; Ch = O, S): structural comparison of two apatite-type lanthanoid chalcogenide ortho-oxosilicates
  21. Neutron powder diffraction study on Li1.8Na0.2MgCl4
  22. On the crystal structure of a new modification of 2-amino-4,6-dichloro-1,3,5-triazine
  23. In-situ investigation of oxygen diffusion in Sr, Mg-doped LaGaO3 superionic conductors with a simultaneously applied electric field
  24. Surface dynamics of III—V semiconductors studied by in situ X-ray diffraction during molecular beam epitaxy
  25. The real structure of Na3BiO4 by electron microscopy, HR-XRD and PDF analysis
  26. High-pressure phase transition of the oxonitridosilicate chloride Ce4[Si4O3+xN7–x]Cl1–xOx with x = 0.12 and 0.18
  27. Noncentrosymmetric coordination networks based on nitrate and acetylenedicarboxylate anions
  28. The crystal structure of γ-P4, a low temperature modification of white phosphorus
  29. Phosphorus-rich phosphorus selenides P14+xSe (x = 1, 5)
  30. Crystal structure and optical properties of the new 8O polytype of Ca2Ta2O7
  31. Photoluminescence of ZnGa2S4 : Eu2+
  32. A structural differentiation of quaternary copper argyrodites: Structure — property relations of high temperature ion conductors
  33. In situ bulk structural study on solid-state dynamics and catalytic activity correlations of a H4[PNbMo11O40] partial oxidation catalyst
  34. Structural study of β-Ni(OH)2 and α-Ni(OH)2 variants for electrode applications
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