13C NMR investigations of carbon monoxide adsorbed in zeolites

¹³C NMR spectra of CO and CO₂ molecules adsorbed in zeolites of A, X, Y type were measured as a function of temperature and pore filling. In contrast to other systems, strong resonance shifts to lower fields appear when CO is adsorbed in decationated zeolites. These shifts can be interpteted by an interaction with adsorption sites of Lewis type.     

13C NMR of pterocarpans

¹³CNMR spectra of eight pterocarpans are reported Assignments are based on multiplicities and second-order features in off-resonance decoupled spectra and on chemical shifts in model compounds. Comparison of the degree of long-range (C, H) coupling in ¹H-coupled spectra is found useful     

Raman scattering study of the ferroelectric phase transition in tris-sarcosine calcium chloride (tscc)

We obtained Raman scattering spectra of normal and deuterated TSCC crystals and one TSCC_I-xB_x mixed crystal (c_I-x = Cl, B_x = Br). The soft-mode behaviour is studied in the temperature range from 80 K to the Curie point. The L and T component of the soft mode are overdamped near 100 K while the oblique component can be observed all over the temperature range we studied. For both normal TSCC and mixed TSCC_I-xB_x crystals the critical exponent β = $\text{1}\text{3}$ is in agreement with dielectric measurements and theoretical calculations.     

13C NMR spectrum of coumarin

Summary The positions of the signals from the C₃, C₅, C₆, and C₇ carbon atoms in the¹³C NMR spectrum of coumarin have been established with the aid of information obtained from the¹³C NMR spectra of [3-D]-, [4-D]-, and 7-methoxycoumarins and by the use of an additive calculation based on the increments of the methoxy group in the¹³C NMR spectrum of anisole.M. V. Lomonosov Moscow State University Scientific-Research Institute of Pharmacology, Academy of Medical Sciences of the USSR. Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 458–462, July–August, 1975.     

Fourier 13C NMR and PMR including 13C satellites of oriented cyanopropyne

Fourier ¹³C and proton NMR spectra of cyanopropyne partially oriented by a nematic phase have been recorded and interpreted. It is shown that more accurate measurements are obtained much more rapidly by observing ¹³C satellites by Fourier PMR than by direct observation of the ¹³C spectrum. The geometry has been extracted from direct couplings; a small but systematic discrepancy with microwave spectroscopy is observed for the carboncarbon bond lengths.     

13C NMR investigations of the nucleoside antibiotic hikizimycin and its constituents

Confirmation of the structure of the nucleoside antibiotic hikizimycin was obtained by comparing the ¹³C NMR chemical shift data of selected model compounds with hikizimycin and its constituents.     

13C NMR spectroscopy of cyclopentenpoliols

The ¹³C NMR spectral parameters of eleven cyclopentenpoliols are discussed. Chemical shift criteria to distinguish isomeric 3' and 4' monodeoxy eucommiols have been clearly established.     

13C NMR study of the 1-isopropyl-indanyl-ion in methylene chloride solution

¹³C NMR study of the reaction between 3-isopropyl indene and trifluoromethane sulfonic acid in methylene chloride solution at ?70° shows the presence of 1-isopropyl indanyl cation. Proposed assignments of the chemical shifts show charge delocalisation due to the aromatic ring.     

Fourier transform NMR investigations of 13C labeled silyl and stannyl acetylenes

The ¹³C NMR spectra of ¹³C labeled mono- and di-substituted silyl- and stannyl-acetylenes have been studied. It was found that the values of ¹J(CC) coupling constants between acetylenic carbons decrease very sharply in the series Alk₃SiCCH, Alk₃SnCCH, Alk₃SiCCSiAlk₃ and Alk₃SnCCSnAlk₃. These results and the observed changes in the geminal hetero-atom β-acetylenic carbon couplings suggest a very strong p_πd_π interaction between the π-electrons of the triple bond and the vacant d orbitals of silicon and tin.     

13C NMR spectra of some furocoumarins

¹³C NMR spectra of some naturally occurring furocoumarins and derivatives have been examined. The assignment of chemical shifts for all the C atoms has been achieved by using techniques recently reported by Bose et al.     

29Si and 13C NMR spectra of permethylpolysilanes

²⁹Si, ¹³C and ¹H NMR spectra are reported for the series of linear permethylpolysilanes Me(SiMe₂)_nMe where n = 1 to 6, for the cyclic permethylpolysilanes (Me₂Si)_n where n = 5 to 8, and for a few related compounds. For linear polysilanes the ²⁹Si and ¹³C chemical shifts can be accurately calculated from simple additivity relationships based on the number of silicon atoms in α, β, γ and δ positions. Adjacent (α) silicon atoms lead to upfield shifts in the ²⁹Si and ¹³C resonances, whereas more remote silicon atoms lead to downfield shifts. The ²⁹Si chemical shifts of the polysilane chains are linearly related to the ¹³C shifts of the carbon atoms attached to the silicon. The ²⁹Si and ¹³C resonances of the cyclic silanes deviate from this relationship. Ring current effects arising from σ delocalization are suggested as an explanation for the deviations. Proton-coupled ²⁹Si NMR spectra are reported for Me₃SiSiMe₃ and for (Me₂Si)_n, n = 5 to 7.     

13C high-resolution NMR study of undoped polyacetylene

¹³C NMR spectra of undoped polyacetylene,(CH)_x, have been measured. The existence of 3.4 mol% methylene moieties as defects in the (CH)_x chains has been observed in trans-(CH)_x. Measurements of partially cis-to-trans isomerized (CH)_x suggest the existence of isolated cis regions.     

NMR 13C study of the structure of polyethyleneimine

The NMR ¹³C (CMR) spectrum of high molecular weight (M = 20,000) branched polyethyleneimine (PEI) obtained by polymerization of ethyleneimine (EI) in aqueous and alcoholic solutions at 50° with 1,3-dichloropropanol as initiator, contains 8 lines. The lines were identified using CMR spectra of model compounds, i.e. linear PEI, regularly branched PEI, diethylenetriamine and ethyleneimine pentamer. It has been shown that the deshielding effect of the nitrogen atoms on the α-atoms of carbon decreases in the folowing order: N_tert > N_sec > N_prim; with the atoms of carbon in the β-position, the effect increases in the opposite order.A quantitative estimation has been made of the distribution of the diads of elementary units containing the same and different nitrogen atoms. The data have been used to draw some conclusions about the structure of the PEI macromolecule.     

13C NMR investigation of the structure of cationic carbonyls in transition metal zeolites

¹³C NMR spectroscopy was used to investigate the nature of carbon monoxide adsorbed on transition metal ions hosted in a synthetic faujasite type zeolite. The adsorbed CO species was characterised by a highly shielded carbon nucleus. Using the Pople approximation for the paramagnetic shielding term, the observed chemical shift was rationalised assuming the formation of a cationic carbonyl species with an appreciable electronic transfer from the carbon lone pair to the transition metal ion and negligible π back-bonding if at all.     

13C NMR substituent effects in tetracyclic diterpenoids

The ¹³C NMR chemical shifts of ent-beyer-15-ene, and one hydroxy and four acetoxy derivatives are reported. The substituent effects of the acetoxy groups upon the saturated and olefinic carbon atoms are discussed. Conformational aspects of the molecules are considered in the light of these effects.     

14N and 13C NMR of tautomeric systems of hydroxy-pyridines

¹⁴N NMR is shown to be an efficient method of investigation of the tautomeric equilibria in hydroxy-and related substituted pyridines. Large relative ¹⁴N chemical shifts within tautomeric pairs estimated from N-Me and O-Me derivatives make possible quantitative determinations of the equilibria. Qualitative conclusions may be drawn from ¹⁴N line widths as well as from ¹³C and proton chemical shifts.     

29Si and 13C NMR Studies of organofunctional di- and trisilanes

A series of di- and trisilanes of general structure Ph₃SiSiMe₂R and (Ph₃Si)₂SiR′R″ were synthesized, and the ²⁹Si and ¹³C chemical shifts and one-bond siliconsilicon coupling constants (¹J_SiSi) were measured. The coupling constants of the disilanes were found to be primarily dependent upon the inductive effect of the alkyl group, R, as measured by the Taft o^★ constant. In both series of compounds, increasing alkyl substitution at silicon led to a decrease in ¹J_SiSi.