Lead thiolates. The formation of water-soluble lead(II) thiolates and the crystal structure of 2-(Morpholin-4-yl)ethanethiolatolead(II) nitrate

1981 ◽  
Vol 34 (1) ◽  
pp. 57 ◽  
Author(s):  
IG Dance ◽  
PJ Guerney

The solubilized thiolate ligand 2-(morpholin-4-yl)ethanethiolate, mes, and its ammonium conjugate acid, Hmes, form crystalline complexes Pb2(Hmes)3(N03)4, Pb(mes)2, Pb(mes)(N03), Pb(mes)- (O2CCH3) and Pb(mes)(O2CCF3). These lead(II) thiolate complexes are soluble in aqueous media. Crystals of Pb(mes)(NO3) contain chains of alternating lead and bridging thiolate sulfur atoms [Pb-S 2.646(4), 2.793(4) �], with the lead coordinated also by the tertiary nitrogen atom [Pb-N 2.61(1) �]. The nitrate ions weakly bridge lead atoms along the chain [Pb-O 2.69(2), 2.88(2), 2.98(2), 3.03(2) �]. Crystal data: Pbca, a l3.396(2), b 21.900(3), c 7.348(1) �, Z 8(x PbSN2O4- C6H12), 1602 observed data, R 0.057.

1959 ◽  
Vol 12 (1) ◽  
pp. 90 ◽  
Author(s):  
E Gellert

A new alkaloid pleurospermine, C14Hl9O3N, has been isolated from the leaves of Cryptocarya pleurosperma. Pleurospermine contains a methoxyl group, a phenolic hydroxyl group, and a tertiary nitrogen atom. The third oxygen atom is possibly present as an alcoholic hydroxyl group. On heating with palladium-charcoal the alkaloid yields 4-hydroxy-3-methoxyacetophenone (I), while methylation followed by oxidation gives veratric acid.


1988 ◽  
Vol 43 (12) ◽  
pp. 1616-1620 ◽  
Author(s):  
Abderraouf Khabou ◽  
Kurt Dehnicke

Abstract [MONCl3 · NC - C2Cl3]2 has been prepared by the reaction of MONCl3 with trichloromethyl isocyanidedichloride, CCl3NCCl2 , in CH2Cl2 suspension. The compound forms redbrown. mois-ture sensitive crystals, which were characterized by their IR spectrum as well as by a crystal structure determination (2482 independent observed reflexions, R = 0.048). Crystal data (-70 °C): Space group P21/c, Z = 2, a = 674.2(2); b = 2128.2(11); c = 786.0(4) pm: β = 102.81(3)°. [MONCl3 • NC-C2Cl3]2 forms centrosymmetric dimeric molecules via chloro bridges with Mo-Cl bond lengths of 240.7 and 276.0 pm. The longer MoCl bond of the MOCl2MO ring is caused by the trans influence of the nitride ligand; the MoN bond length of 167 pm corresponds with a triple bond. The 2,3,3-trichloroacrylnitrile ligand is bonded by its nitrogen atom with a bond length of Mo -N = 216 pm; the Mo-N≡C-C sequence is almost linear with a remarkable short C-C bond of 143.0 pm.


1964 ◽  
Vol 42 (11) ◽  
pp. 2584-2594 ◽  
Author(s):  
W. A. Szarek ◽  
K. A. H. Adams ◽  
M. Curcumelli-Rodostamo ◽  
D. B. MacLean

Annotine, C16H21O3N, is shown to be pentacyclic and to contain a tertiary hydroxyl group, a lactone function, a tertiary nitrogen atom, and a dialkylated double bond. The position of the double bond and the tertiary hydroxyl group relative to the nitrogen atom has been established by Emde degradation of annotine methiodide. The presence of a lactone function is inferred from the reduction of annotine to dihydroannotinol, a hemiacetal, which reacts with 1 mole of ethyl mercaptan. The reduction of the lactone to a diol in an annotine derivative has been carried out. The chemical studies and the examination of annotine and its derivatives by modern instrumental methods allow the assignment of a plausible structure to the alkaloid.


1955 ◽  
Vol 8 (1) ◽  
pp. 129 ◽  
Author(s):  
WD Crow ◽  
M Michael

The bark and leaves of the rain-forest tree Kopsia longiflora Merrill (Apocynaceae) contain four new alkaloids ; kopsinine, C21H26O2N2, (0.2 per cent.), kopsilongine, C24H30O6N2 (0.06 per cent.), and kopsamine, C25H30O7N2 (0.02 per cent.) occurring in the bark ; and kopsilongine (0.07 per cent.), kopsamine (0.3 per cent.), and kopsiflorine, C23H28O5N2, (0.04 per cent.) in the leaves. The bark also contains β-amyrin (0.35 per cent.) while the leaves afford a mixture of paraffin hydrocarbons, mainly n-hentri- acontane, β-sitosterol, a sterol, C29H50O2, and a triterpene alcohol acetate, C32H52O2. Kopsamine, kopsilongine, and kopsiflorine each contain two methoxyl groups, while kopsinine contains only one ; kopsamine and kopsilongine also contain methylene-dioxy-groups. No reactive carbonyl groups were detected. The alkaloids all titrated as monoacid bases and formed monomethiodides: while the ultraviolet spectra recorded in acid and neutral media show that the basic (tertiary) nitrogen atom does not contribute to the chromophoric system.


1985 ◽  
Vol 19 (6) ◽  
pp. 430-434
Author(s):  
A. Z. Abyshev ◽  
V. G. Klimov ◽  
S. S. Krylov ◽  
E. V. Semenov ◽  
I. P. Sidorova

2018 ◽  
Vol 9 (3) ◽  
pp. 178-181 ◽  
Author(s):  
Leslaw Sieron ◽  
Agnieszka Czylkowska ◽  
Bartlomiej Rogalewicz

A new gadolinium(III) complex with 4,4’-bipyridine (4-bpy) and dibromoacetate ligand of general formula [Gd(4-bpy)(CBr2HCOO)3(H2O)]n, has been synthesized, crystallized and characterized by a single-crystal X-ray diffraction analysis. The gadolinium atom has an unsymmetrical eight-coordinate geometry, being coordinated by six oxygen atoms of dibromoacetate anions, one nitrogen atom of 4-bpy and one water molecule. The complex is a one-dimensional polymer as a result of dibromoacetate ligand bridging with the repeating monomeric units. There are π...π stacking interactions between the 4-bpy rings as well as O–H...O and O–H...N hydrogen bonds. Crystal Data for C16H13Br6GdN2O7 (Mw = 981.99 g/mol): triclinic, space group P-1 (no. 2), a = 9.7368(4) Å, b = 11.5416(4) Å, c = 11.7634(4) Å, α = 104.2750(10)°, β = 94.060(2)°, γ = 92.6900(10)°, V = 1275.08(8) Å3, Z = 2, T = 90 K, μ(CuKα) = 28.190 mm-1, Dcalc = 2.558 g/cm3, 8399 reflections measured (7.782° ≤ 2Θ ≤ 133.18°), 4006 unique (Rint = 0.0409, Rsigma = 0.0639) which were used in all calculations. The final R1 was 0.0527 (I > 2σ(I)) and wR2 was 0.1396 (all data).


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