Studies in the Cycloproparene Series: Formation of a New Dimer of 1H-Cyclopropa[b]naphthalene

1999 ◽  
Vol 52 (4) ◽  
pp. 285 ◽  
Author(s):  
Brian Halton ◽  
Carissa S. Jones ◽  
Peter T. Northcote ◽  
Roland Boese
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
Size Exclusion ◽  
The Novel ◽  
Methyl Derivative ◽  
X Ray ◽  
Pure Compounds

1-(Trimethylsilyl)-1H-cyclopropa[b]naphthalene (10) and its 1-methyl derivative (11) have been isolated as pure compounds from use of a lipophilic size exclusion gel. Acylation of the 1H-cyclopropa[b]naphthalenyl anion (2) is effected with N,N -dimethyl-benzamide and -acetamide to give (5) and (6), respectively. Analogous reactions with the 1-(trimethylsilyl)-1H-cyclopropa[b]naphthalenyl anion (9) do not yield the 1-acyl-1-(trimethylsilyl)-1H-cyclopropa[b]naphthalenes (12) and (13); instead the novel 6-methyl- 7H-dibenzo[b,g]fluorene (15) results from attempted acetylation. Compound (15), a formal dimer of 1H-cyclopropa[b]naphthalene (1), is formed also from anion (9) both in toluene and from addition of hydrocarbon (1); its structure is assigned from spectroscopic data and confirmed by single-crystal X-ray analysis.

scholarly journals New Piperazine Derivatives Synthesized from Thio-Substituted Polyhalogeno-2-nitro-1,3-butadienes

2010 ◽  
Vol 7 (4) ◽  
pp. 1498-1506 ◽  
Author(s):  
S. Goksin Aydinli ◽  
Cemil Ibis
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
The Novel ◽  
X Ray ◽  
Piperazine Derivatives ◽  
Bioactive Heterocycles ◽  
New Compounds

It is known that polyhalogeno-nitro-1,3-butadienes are important starting materials for the synthesis of polyfunctionalized bioactive heterocycles. NovelN,S-substituted nitrobutadienes (4a-j) were synthesized from the reaction of the monothio-substituted nitrodiene derivatives (2a) and (2b) with some piperazine derivatives. These new compounds are stable and the structures of these products were characterized by spectroscopic data. The structure of the novelN,S-substituted nitrodiene compound (4g) synthesized in this study was also elucidated by single crystal x-ray analysis.

(+)-Iforrestine: a Novel Heterocyclic Nephrotoxin From Isotropis forrestii

1989 ◽  
Vol 42 (8) ◽  
pp. 1249 ◽  
Author(s):  
SM Colegate ◽  
PR Dorling ◽  
CR Huxtable ◽  
TJ Shaw ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Spectroscopic Data ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tubular Necrosis ◽  
Proximal Tubular ◽  
Renal Proximal Tubular ◽  
Heterocyclic Structure

A compound that reproduces the acute renal proximal tubular necrosis associated with ingestion of Isotropis forrestii, by animals, has been isolated from the plant. The novel heterocyclic structure was determined by a single-crystal X-ray diffraction study. The spectroscopic data are presented and rationalized with respect to the assigned structure.

New iboga-type alkaloids from Ervatamia hainanensis

RSC Advances ◽  
2016 ◽  
Vol 6 (36) ◽  
pp. 30277-30284 ◽  
Author(s):  
Zhi-Wen Liu ◽  
Xiao-Jun Huang ◽  
Han-Lin Xiao ◽  
Guo Liu ◽  
Jian Zhang ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
X Ray Diffraction ◽  
X Ray

The structures and absolute configurations of seven new iboga-type alkaloids 1–7 were determined by spectroscopic data, Mosher's method, single crystal X-ray diffraction and ECD analyses.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

1,3-Dipolar Cycloadditions of a Chiral Oxazolidinone With Nitrones and Nitrile Oxides

1995 ◽  
Vol 48 (9) ◽  
pp. 1511 ◽  
Author(s):  
SG Pyne ◽  
J Safaei-G ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Hydrogen Atmosphere ◽  
Dipolar Cycloaddition ◽  
Cycloaddition Reactions ◽  
The Novel ◽  
X Ray ◽  
Dipolar Cycloadditions ◽  
Nitrile Oxides ◽  
Exocyclic Methylene

The 1,3-dipolar cycloaddition reactions of the chiral oxazolidinone (1) and nitrones are highly regioselective and only 5,5-disubstituted isoxazolidine adducts are formed. These reactions occur under equilibrating conditions to give the more stable adducts that result from addition to the exocyclic methylene of (1) from the sterically more hindered π-face. The endo adducts are generally thermodynamically favoured. In one case the novel azetidine (21) was formed from the treatment of the adduct (4a) with palladium hydroxide on carbon under a hydrogen atmosphere. The major adducts from the reaction of (1) and nitrile oxides (16a,b) had the expected stereochemistry, addition of the 1,3-dipole having occurred from the less hindered π-face of the exocyclic methylene of (1). The stereochemistry of many of these products has been elucidated by single-crystal X-ray structural determinations.

Studies of Australian soft corals. IX. A novel nor-diterpene from the soft coral Sinularia leptoclados

1978 ◽  
Vol 31 (9) ◽  
pp. 2049 ◽  
Author(s):  
BF Bowden ◽  
JC Coll ◽  
SJ Mitchell ◽  
J Mulder ◽  
GJ Stokie
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
Soft Coral ◽  
Parent Compound ◽  
Soft Corals ◽  
X Ray

The structure of a novel nor-cembranoid diterpene of formula C19H24O6 (1) is reported. The compound was extracted from the soft coral Sinularia leptoclados, and spectroscopic data were collected on the parent compound (1) and a series of derivatives. It was not possible to assign an unambiguous structure on purely spectroscopic grounds, and so single-crystal X-ray analysis was used to prove the structure (1): (4R*,8S*,11R*,13S*,14R*)-14-hydroxy-4-isopropenyl-11-methyl-6,9-dioxo-8,11-epoxycyclotetradec-1-ene-1,13-carbolactone.

scholarly journals The structure of fusarochromanone: new mycotoxin from Fusariumroseum, "Graminearum"

1986 ◽  
Vol 64 (7) ◽  
pp. 1258-1261 ◽  
Author(s):  
Sadanand V. Pathre ◽  
William B. Gleason ◽  
Yin-Wan Lee ◽  
Chester J. Mirocha
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
Ring Structure ◽  
Toxic Principle ◽  
X Ray ◽  
Tibial Dyschondroplasia ◽  
Toxic Cultures

An isolate of Fusariumroseum "Graminearum" obtained from overwintered oats in Alaska produced toxic cultures when grown on rice. The toxic principle called fusarochromanone isolated from these cultures reproduced the signs of tibial dyschondroplasia in poultry and also reduced hatchability of fertile eggs. Spectroscopic data (nmr, ir, and ms) indicated the mycotoxin to be a chromanone derivative. The chromanone ring structure was also confirmed by single crystal X-ray.

Kristallstruktur und Schwingungsspektren von Li5CrCl8 / Crystal Structure and Vibrational Spectra of Li5CrCl8

1992 ◽  
Vol 47 (12) ◽  
pp. 1687-1692 ◽  
Author(s):  
Heinz Dieter Lutz ◽  
Peter Kuske ◽  
Arno Pfitzner ◽  
Hermann-Josef Steiner
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Structure Type ◽  
The Novel ◽  
X Ray ◽  
Symmetry Coordinates ◽  
Unknown Structure ◽  
Ir And Raman

The crystal structure of the novel pink Li5CrCl8 oC28 has been determined by both single crystal X-ray and neutron powder studies. The title compound crystallizes in a hitherto unknown structure type (space group C mmm, Z = 2). The final R values are R = 3.4% (715 independent reflections with I > 3aI) and Rwp = 11.5%, respectively (a = 1019.79(3), b = 723.94(2) and c = 726.16(3) pm). The structure consists of edge-connected Li(l)Cl6 and alternating edge-connected Li(2)Cl6 and CrCl6 octahedra, respectively. It is related to the NaCl super structure SnMn2S4 type. IR and Raman spectra as well as symmetry coordinates are given and discussed in terms of CrCl6 and LiCl6 breathing modes.

scholarly journals Übergangsmetall-Carben-Komplexe, CXXXIV [1]. Synthese neuer Mono- und Biscarben-Komplexe der VI. Nebengruppe; Röntgenstruktur des ersten Bis[amino(alkoxy)carben]-Komplexes / Transition Metal Carbene Complexes, CXXXIV [1]. Synthesis of New Mono- and Bis-Carbene Complexes of Group VIb Elements; Structure of the First Bis[amino(alkoxy)carbene]-Complex

1984 ◽  
Vol 39 (5) ◽  
pp. 668-674 ◽  
Author(s):  
Ernst Otto Fischer ◽  
Rudolf Reitmeier ◽  
Klaus Ackermann
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Spectroscopic Data ◽  
The Novel ◽  
Nucleophilic Agent ◽  
Reaction Conditions ◽  
Carbene Complexes ◽  
X Ray ◽  
X Ray Crystallography ◽  
New Compounds

The hexacarbonyl compounds of chromium, molybdenum and tungsten react with the highly nucleophilic agent Li NiPr2 and in a subsequent alkylation with (Et3O)BF4 to give the carbene complexes (CO)5M[C(N′Pr2)OEt] (1, 3, 4). In case of W(CO)6 and Mo(CO)6 the novel biscarbene complexes cis(CO)4M[C(NiPr2)OEt]2 (2, 5) are additionally obtained. Reaction conditions, properties and spectroscopic data of the new compounds are reported. The molecular structure of cis(CO)4W[C(NiPr2)OEt]2 (4) was determined by X-ray crystallography

Crystal-Structures of 2 3-Substituted 10,11-Dimethoxy-1,2,3,4,5,6-Hexahydro-7,9-etheno-3-benzazecine Derivatives

1989 ◽  
Vol 42 (2) ◽  
pp. 321
Author(s):  
XY Jia ◽  
JB Bremner ◽  
BW Skelton ◽  
AH White ◽  
KN Winzenberg
Keyword(s):  
Hydrogen Atom ◽  
Chemical Shift ◽  
Single Crystal ◽  
Crystal Structures ◽  
Naphthalene Ring ◽  
Methyl Derivative ◽  
X Ray ◽  
Structure Determinations

The title compounds are 3-aza[6](1,7)-naphthalenophanes with 3-Me and 3-CO2Me substituents, C18H23NO2 and C19H23NO4; in the former the chemical shift of the naphthalene hydrogen enclosed by the medium nitrogen-containing ring is the highest yet observed in a derivative of this type ( σ 9.33). In order to examine the environment of this hydrogen atom and the expected associated naphthalene ring distortions in both compounds, single-crystal X-ray structure determinations have been carried out at 295 K showing the transannular H…N distance in the methyl derivative to be remarkably short at 2.08(2) � . Crystals are triclinic, P1, a 11.683(3), b 10.846(3), c 6.729(2) �, α 90.08(2), β 93.33(2), γ 112.88 Z 2; R was 0.041 for 1378 'observed' reflections. Crystals of the 3-CO2Me derivative are also triclinic, P1, a 12.587(9), b 10.650(4), c 6.758(3) � , a 91.91(3), β 100.51(4), γ 104.74(5)° Z 2; R 0.067 for 1267 'observed' reflections.

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