The structure of 2,2-dibutyl-1,3,2-dioxastannane in the solid state and in solution

1992 ◽  
Vol 70 (1) ◽  
pp. 197-204 ◽  
Author(s):  
T. Bruce Grindley ◽  
Rasiah Thangarasa ◽  
Pradip K. Bakshi ◽  
T. Stanley Cameron
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Carbon Atom ◽  
Low Temperature ◽  
Nmr Spectra ◽  
Monomer Unit ◽  
The Other ◽  
Mirror Plane ◽  
X Ray ◽  
X Ray Crystallography

Crystals of 2,2-dibutyl-1,3,2-dioxastannane (1) are orthorhombic, of space group Pnma, with a = 7.663(3), b = 18.437(2), c = 9.277(4) Å, Z = 4, R = 0.0568 (Rw = 0.0551) for 1183 independent reflections with I > 3σ(I). Compound 1 is a polymer in which each monomer unit is joined to the next by a four-membered (SnO)2 ring. The Sn—O bond lengths inside the monomer units average 2.04 Å while those between monomers average 2.57 Å. The mirror plane of the crystal contains the atoms in the four-membered rings and the other oxygen atoms. Two of the three remaining carbon atoms in the six-membered rings of the monomer units are close to the mirror plane. The other carbon atom is disordered above and below the plane. It was shown by 119Sn NMR spectroscopy that solutions of 1 contain mixtures of oligomers that consist mainly of dimers, trimers, and tetramers in chloroform-d. ΔG0 values for dimmer–trimer equilibria and dimmer–tetramer equilibria of −2.5 and −1.5 kcal mol−1 were obtained from integration of low temperature 119Sn NMR spectra. These values favour the higher oligomers slightly less than those for 2,2-dibutyl-1,3,2-dioxastannolane. Keywords: 1,3,2-dioxastannanes, stannylene acetals. X-ray crystallography, 119Sn NMR spectroscopy.

Triferrocenylborane – Molecular Structure in Solution and in the Solid State

1995 ◽  
Vol 50 (2) ◽  
pp. 201-204 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Udo Dörfler ◽  
Wolfgang Milius ◽  
Max Herberhold
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Low Temperature ◽  
Single Crystal ◽  
Nmr Spectra ◽  
The Other ◽  
X Ray ◽  
Single Diastereomer ◽  
Structure In Solution ◽  
C Nmr

According to a single crystal X-ray structure determination all three ferrocenyl substituents of triferrocenylborane (1) adopt the same orientation with respect to the BC3-plane [P21/c monoclinic; Z = 4; a = 1353.5(3), b = 1695.6(3), c = 1056.4(2) pm, β = 109.27(3)°]. The simulated X-ray powder pattern of the single crystal is identical with the powder diagram of a macroscopic sample, indicating the presence of a single diastereomer (1a) in the solid state. However, at low temperature (< - 95 °C) in solution, the 13C NMR spectra suggest the presence of the second diastereomer (1b) in which one ferrocenyl group is oriented opposite to the other two with respect to the central BC3-plane.

ChemInform Abstract: DYNAMIC INTERMOLECULAR TAUTOMERISM OF 3,5-DIMETHYLPYRAZOLE IN THE SOLID STATE BY CARBON-13 CP/MAS NMR SPECTROSCOPY AND X-RAY CRYSTALLOGRAPHY

1985 ◽  
Vol 16 (51) ◽  
Author(s):  
A. BALDY ◽  
J. ELGUERO ◽  
R. FAURE ◽  
M. PIERROT ◽  
E.-J. VINCENT
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Mas Nmr ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cp Mas Nmr

Molecular structure and dynamics of C-1-adamantyl substituted N-unsubstituted pyrazoles studied by solid state NMR spectroscopy and X-ray crystallography

1997 ◽  
pp. 1867-1876 ◽  
Author(s):  
Rosa María Claramunt ◽  
María Dolores Santa María ◽  
Isabelle Forfar ◽  
Francisco Aguilar-Parrilla ◽  
María Minguet-Bonvehí ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
X Ray ◽  
Solid State Nmr Spectroscopy ◽  
X Ray Crystallography ◽  
Structure And Dynamics

The relative stabilities of PhE(NH-t-Bu)2 and PhE(μ-N-t-Bu)2EPh (E = As, Sb, and Bi): X-ray structures of {Li2[PhAs(N-t-Bu)2]}2 and PhE(μ-N-t-Bu)2EPh (E = Sb, Bi)

2003 ◽  
Vol 81 (2) ◽  
pp. 169-174 ◽  
Author(s):  
Glen G Briand ◽  
Tristram Chivers ◽  
Masood Parvez
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Phenyl Group ◽  
Synthetic Approach ◽  
Relative Stabilities ◽  
X Ray ◽  
X Ray Crystallography ◽  
In Trans ◽  
C Nmr

The reaction of PhECl2 with 2 equiv of LiHN-t-Bu has been studied for the series E = As, Sb, and Bi to determine the effect of the phenyl group on subsequent amine condensation processes. For PhAsCl2, the metathesis product PhAs(NH-t-Bu)2 4 was obtained as a colourless oil. Similar reactions involving PhECl2, where E = Sb or Bi, yielded the cyclodipnict(III)azanes PhE(μ-N-t-Bu)2EPh 5 (E = Sb) and 6 (E = Bi), respectively. Treatment of 4 with 2 equiv of n-BuLi produced the dilithium salt Li2[PhAs(N-t-Bu)2] 7a. Products 4, 5, 6, and 7a were characterized by 1H, 7Li (7a), and 13C NMR spectra, while 5, 6, and 7a were also structurally characterized by X-ray crystallography. Compound 7a is dimeric in the solid state via intermolecular Li···N and η6-Li···Ph interactions. The cyclodipnict(III)azanes 5 and 6 have similar structures, with the exocyclic phenyl groups in trans positions relative to the E2N2 ring. This synthetic approach provides a new route to the four-membered rings RE(μ-N-t-Bu)2ER (E = Sb, Bi) and the first example of a bis(organyl)cyclodibism(III)azane.Key words: arsenic, antimony, bismuth, amides, imides.

Encapsulation of L-Valine, D-Leucine and D-Methionine by Cucurbit[8]uril

CrystEngComm ◽  
2022 ◽  
Author(s):  
Zenghui Zhang ◽  
Rui-Lian Lin ◽  
Xiangyun Yu ◽  
Li-Xia Chen ◽  
Zhu Tao ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Binding Interactions ◽  
X Ray ◽  
X Ray Crystallography

The binding interactions of cucurbit[8]uril (Q[8]) with L-Valine, D-Leucine, and D-Methionine, both in aqueous solution and solid state, have been studied by 1H NMR spectroscopy and X-ray crystallography. 1H NMR...

Interactions de l'ion Ag+ avec la glutarimide

1984 ◽  
Vol 62 (7) ◽  
pp. 1287-1291 ◽  
Author(s):  
Johanne Perron ◽  
André L. Beauchamp
Keyword(s):  
Infrared Spectroscopy ◽  
Infrared Spectrum ◽  
Nmr Spectra ◽  
The Other ◽  
Mirror Plane ◽  
Bond Orders ◽  
X Ray Diffraction ◽  
Complex Species ◽  
X Ray ◽  
C Nmr

The 1:1 complex formed between Ag+ ions and glutarimide was investigated by X-ray diffraction, infrared spectroscopy, and 1H and 13C nmr. The crystals are monoclinic, C2/c, a = 13.497(3) Å, b = 9.503(2) Å, c = 9.600(4) Å, β = 92.30(3)°, Z = 4 molecules per cell. The structure was refined on 1086 nonzero [Formula: see text] reflections to R = 0.027. One half of the Ag atoms are linearly coordinated to the N atoms of two deprotonated glutarimide ligands, whereas the other half are surrounded by an approximate tetrahedron of four carbonyl oxygens belonging to two adjacent [Glu–Ag–Glu]− units. The [Glu–Ag–Glu]− groups are joined by tetrahedrally coordinated Ag atoms into infinite chains along the c axis. Complexation introduces a number of changes in the infrared spectrum of glutarimide. They can be related to the disappearance of the N—H vibrator and the change of bond orders in the —C(O)—N—C(O)— portion of the ligand. The nmr spectra show that coordinated glutarimide retains a mirror plane when the Ag complex is dissolved in DMSO. This suggests that the O-bonded Ag atoms dissociate to a large extent in solution, leaving the linear [Glu–Ag–Glu]− ions as the major glutarimide complex species.

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