Startseite Structure Determination for the Crystalline Phase of Triphenyl Phosphite by Means of Multi-Dimensional Solid-State NMR and X-Ray Diffraction
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Structure Determination for the Crystalline Phase of Triphenyl Phosphite by Means of Multi-Dimensional Solid-State NMR and X-Ray Diffraction

  • Jürgen Senker EMAIL logo und Jens Lüdecke
Veröffentlicht/Copyright: 2. Juni 2014
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Zeitschrift für Naturforschung B
Aus der Zeitschrift Zeitschrift für Naturforschung B Band 56 Heft 11

The crystalline phase of triphenyl phosphite P(OC6H5)3 was investigated by means of 31P solid-state NMR and X-ray diffraction in a temperature range between 170 K and its melting point (Tm = 293 K). ID MAS NMR spectra exhibit one sharp central resonance indicating only one crystallographically unique molecule in the unit cell. A theoretical analysis concerning the shape of 2D exchange spectra for 1 = 1 /2 nuclei is presented. It is shown that if the exchange is caused by radio-frequency driven spin-diffusion, this technique allows to discriminate rotational symmetry elements in crystalline solids. Used on crystalline triphenyl phosphite, 3-fold symmetry could be revealed clearly. Structure determination based on X-ray single crystal diffraction data collected at 191 K shows that triphenyl phosphite crystallises in hexagonal metric with space group R3̅(wR2= 8.3%, Z = 18) and one molecule in the asymmetric unit. This result is in excellent agreement with the NMR spectroscopic data. The lattice parameters at 200 K were determined to a = 37.887(1) and c = 5.7567(2) Å (V = 7156(1) Å3) by refining an X- ray powder-diffraction pattern. The structure of triphenylphosphite can be described as a close rod packing. The rods are formed by ecliptically arranged triphenylphosphite molecules. Due to the 3-fold rotoinversion axis the orientation of molecules in neighboured rods is antiparallel.

Keywords: Triphenyl Phosphite; Structure Determination; Solid-State NMR
Received: 2001-7-18
Published Online: 2014-6-2
Published in Print: 2001-11-1

© 1946 – 2014: Verlag der Zeitschrift für Naturforschung

Artikel in diesem Heft

  1. Structure Determination for the Crystalline Phase of Triphenyl Phosphite by Means of Multi-Dimensional Solid-State NMR and X-Ray Diffraction
  2. Amido-tert-butylimido-vanadium(V)-Verbindungen. Darstellung, Reaktionen und 51V-NMR-spektroskopische Untersuchungen / Amido-tert-butylimidovanadium(V) Compounds. Synthesis, Reactions and 51V NMR Spectroscopic Studies
  3. peri-Interactions in Naphthalenes, 5 [1]. On the Impact of peri-Stress and Trityl-Stress upon the Length of N+-C Bonds in 1-Azonia-acenaphthene Cations
  4. [Co(NH3)6]C1C03 - ein Hexaammincobalt(III)-Komplex mit einer ‘idealen’ Carbonat-Gruppe / [Co(NH3)6]C1C03 - a Hexaamminecobalt(III) Complex with an ‘Ideal’ Carbonate Group
  5. Crystal Structure and Magnetic Properties of an Oxygen-Bridged Trinuclear Copper(II) Complex
  6. Importance of Orbital Complementarity in Spin Coupling through Two Different Bridging Groups. Synthesis, Crystal Structure, Magnetic Properties and Magneto-Structural Correlations in a Dicopper(II) Complex of Endogenous Alkoxo Bridging Ligand with Exogenous Pyrazolate
  7. Thermal Catalytic Hydrosilylation of Conjugated Dienes with Triethylsilane in the Presence of Tricarbonyl(o-xylene)Metal (Metal = Cr, Mo, W) Complexes
  8. Preparation, Properties, and Crystal Structure of Quaternary Silicide Carbides RCr2Si2C (R = Y, La - Nd, Sm, Gd - Ho)
  9. CsCu3Dy2S5 und CsCu3Er2S5 : Zwei isotype quaternäre Sulfide der Lanthanoide mit Kanalstrukturen / CsCu3Dy2S5 and CsCu3Er2S5: Two Isotypic Quaternary Sulfides of the Lanthanides with Channel Structures
  10. Donor-Acceptor Complexes between Simple Phosphines. First Structural Data for an Almost Forgotten Class of Compounds
  11. Donor-Acceptor Complexes between Organoamines and Phosphorus Tribromide
  12. Orthoamides, LVI [1]. A New Method of Wide Scope for the Preparation of Aryl Formates
  13. Orthoamide, LVII [1]. Lassen sich aromatische Aldehyde nach Fries aus Arylformiaten hersteilen? / Orthoamides, LVII [1]. Can Aromatic Aldehydes be Prepared from Aryl Formates via the Fries Rearrangement?
  14. Polysulfonylamine, CXLVII [1]. Die ersten N,N-disulfonylierten Thioharnstoffe: Synthese von (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) und Kristallstruktur der Ditosylverbindung / Polysulfonylamines, CXLVII [1]. The First N,N-Disulfonylated Thioureas: Synthesis of (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) and Crystal Structure of the Ditosyl Compound
  15. Einige Umsetzungen von Inhydrazinen mit Isocyanaten: [2+2]- und [4+2]Cycloadditionen, (Hydrazinoethinyl)metallierung / Some Reactions of Ynehydrazines with Isocyanates: [2+2]- and [4+2]Cycloadditions, (Hydrazinoethynyl)metallation
  16. Structural Influence of Hydrogen Bonding and π-Stacking in trans-Diazido-tetrakis( pyrazole)nickel(II) and trans-Diazido-tetrakis(3-methylpyrazoIe)nickel(II)
  17. 7-Azoniafluorenonderivate durch elektrostatisch aktivierte SNAr-Reaktionen / 7-Azoniafluorenone Derivatives by Electrostatically Activated SNAr-Reactions
  18. Palladium(II) and Platinum(II) Complexes of N-3-Pyridinylmethanesulfonamide
  19. Facile Approach to Versatile Chiral Intermediates for Fused Cyclopentanoid Natural Products
  20. Nukleophile Aromatische Substitution an 2-Fluoroimidazolium-Ionen: Synthese und Kristallstruktur eines dikationischen 2,2-Biimidazolyl- Derivates [1] / Nucleophilic Aromatic Substitution at 2-Fluoroimidazolium Ions: Synthesis and Crystal Structure of a Dicationic 2,2′-Biimidazolyl Derivative [1]
  21. Interpenetrierende Clusterstränge in der Kristallstruktur von K0,77Nb6Cl15 / Interpenetrating Cluster Chains in the Structure of K0.77Nb6Cl15
  22. Synthesis and Structure of RE2Rh2Cd (RE = La, Ce, Pr, Nd, Sm)
https://doi.org/10.1515/znb-2001-1101
Schlagwörter für diesen Artikel
Triphenyl Phosphite; Structure Determination; Solid-State NMR

Artikel in diesem Heft

  1. Structure Determination for the Crystalline Phase of Triphenyl Phosphite by Means of Multi-Dimensional Solid-State NMR and X-Ray Diffraction
  2. Amido-tert-butylimido-vanadium(V)-Verbindungen. Darstellung, Reaktionen und 51V-NMR-spektroskopische Untersuchungen / Amido-tert-butylimidovanadium(V) Compounds. Synthesis, Reactions and 51V NMR Spectroscopic Studies
  3. peri-Interactions in Naphthalenes, 5 [1]. On the Impact of peri-Stress and Trityl-Stress upon the Length of N+-C Bonds in 1-Azonia-acenaphthene Cations
  4. [Co(NH3)6]C1C03 - ein Hexaammincobalt(III)-Komplex mit einer ‘idealen’ Carbonat-Gruppe / [Co(NH3)6]C1C03 - a Hexaamminecobalt(III) Complex with an ‘Ideal’ Carbonate Group
  5. Crystal Structure and Magnetic Properties of an Oxygen-Bridged Trinuclear Copper(II) Complex
  6. Importance of Orbital Complementarity in Spin Coupling through Two Different Bridging Groups. Synthesis, Crystal Structure, Magnetic Properties and Magneto-Structural Correlations in a Dicopper(II) Complex of Endogenous Alkoxo Bridging Ligand with Exogenous Pyrazolate
  7. Thermal Catalytic Hydrosilylation of Conjugated Dienes with Triethylsilane in the Presence of Tricarbonyl(o-xylene)Metal (Metal = Cr, Mo, W) Complexes
  8. Preparation, Properties, and Crystal Structure of Quaternary Silicide Carbides RCr2Si2C (R = Y, La - Nd, Sm, Gd - Ho)
  9. CsCu3Dy2S5 und CsCu3Er2S5 : Zwei isotype quaternäre Sulfide der Lanthanoide mit Kanalstrukturen / CsCu3Dy2S5 and CsCu3Er2S5: Two Isotypic Quaternary Sulfides of the Lanthanides with Channel Structures
  10. Donor-Acceptor Complexes between Simple Phosphines. First Structural Data for an Almost Forgotten Class of Compounds
  11. Donor-Acceptor Complexes between Organoamines and Phosphorus Tribromide
  12. Orthoamides, LVI [1]. A New Method of Wide Scope for the Preparation of Aryl Formates
  13. Orthoamide, LVII [1]. Lassen sich aromatische Aldehyde nach Fries aus Arylformiaten hersteilen? / Orthoamides, LVII [1]. Can Aromatic Aldehydes be Prepared from Aryl Formates via the Fries Rearrangement?
  14. Polysulfonylamine, CXLVII [1]. Die ersten N,N-disulfonylierten Thioharnstoffe: Synthese von (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) und Kristallstruktur der Ditosylverbindung / Polysulfonylamines, CXLVII [1]. The First N,N-Disulfonylated Thioureas: Synthesis of (RSO2)2N-C(S)-NMe2 (R = Me, 4-Me-C6H4) and Crystal Structure of the Ditosyl Compound
  15. Einige Umsetzungen von Inhydrazinen mit Isocyanaten: [2+2]- und [4+2]Cycloadditionen, (Hydrazinoethinyl)metallierung / Some Reactions of Ynehydrazines with Isocyanates: [2+2]- and [4+2]Cycloadditions, (Hydrazinoethynyl)metallation
  16. Structural Influence of Hydrogen Bonding and π-Stacking in trans-Diazido-tetrakis( pyrazole)nickel(II) and trans-Diazido-tetrakis(3-methylpyrazoIe)nickel(II)
  17. 7-Azoniafluorenonderivate durch elektrostatisch aktivierte SNAr-Reaktionen / 7-Azoniafluorenone Derivatives by Electrostatically Activated SNAr-Reactions
  18. Palladium(II) and Platinum(II) Complexes of N-3-Pyridinylmethanesulfonamide
  19. Facile Approach to Versatile Chiral Intermediates for Fused Cyclopentanoid Natural Products
  20. Nukleophile Aromatische Substitution an 2-Fluoroimidazolium-Ionen: Synthese und Kristallstruktur eines dikationischen 2,2-Biimidazolyl- Derivates [1] / Nucleophilic Aromatic Substitution at 2-Fluoroimidazolium Ions: Synthesis and Crystal Structure of a Dicationic 2,2′-Biimidazolyl Derivative [1]
  21. Interpenetrierende Clusterstränge in der Kristallstruktur von K0,77Nb6Cl15 / Interpenetrating Cluster Chains in the Structure of K0.77Nb6Cl15
  22. Synthesis and Structure of RE2Rh2Cd (RE = La, Ce, Pr, Nd, Sm)
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