Synthesis and structural study of aminals derived from 8-aminoquinoline and 1-aminonaphtalene

1987 ◽  
Vol 65 (4) ◽  
pp. 687-692 ◽  
Author(s):  
Enrique Galvez ◽  
Isabel Iriepa ◽  
Antonio Lorente ◽  
Jose Miguel Mohedano ◽  
Feliciana Florencio ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Carbon Atom ◽  
Mass Spectra ◽  
The Other ◽  
Reaction Conditions ◽  
Schiff’S Base ◽  
Triclinic Space Group ◽  
X Ray ◽  
H Nmr ◽  
Cell Dimensions

Reaction of 8-aminoquinoline with pyridine-2-carboxaldehyde (2), pyridine-3-carboxaldehyde (3), pyridine-4-carboxaldehyde (4), and benzaldehyde (5) yields the corresponding aminals or Schiff's bases according to reaction conditions; analogous results are obtained from the reaction of 1-amino-naphtalene with pyridine-2-carboxaldehyde (6). On the other hand, reaction of 8-aminoquinoline with thiophene-2-carboxaldehyde or pyrrole-2-carboxaldehyde yields neither the aminal nor the Schiff's base. Crystals of 4 (C24H19N5) belong to the triclinic space group [Formula: see text]. Cell dimensions are a = 11.547(3), b = 11.759(2), c = 15.687(5) Å, α = 98.50(2)°, β = 101.61(2)°, γ = 107.28(2)°, V = 1942.6(9) Å3. Final R = 0.077 and Rw = 0.064; 3160 reflections were observed. The ir, 1H nmr of 2–6, the mass spectra of 4 and 5 and the X-ray analysis of 4 are described and discussed. Preparative features, ir, 1H nmr, analyses and crystal structure indicate that the formation of 2–6 are governed mainly by the nucleophilicity at the aldehyde carbon atom and the existence of the hydrogen bonds in the aminal.

scholarly journals Chemie polyfunktioneller Moleküle, 106. Kupfer(I)halogenid — Komplexe des Bis(diphenylphosphino)amins / Chemistry of Polyfunctional Molecules, 106. Copper(I) Halide Complexes of Bis(diphenylphosphino)amine

1990 ◽  
Vol 45 (12) ◽  
pp. 1657-1668 ◽  
Author(s):  
Jochen Ellermann ◽  
Falk A. Knoch ◽  
Klaus J. Meier
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Conductivity Data ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr ◽  
Nmr Data ◽  
Halide Complexes

Reaction of Copper(I) halides CuX (X = Cl, Br, I) in methanol with bis(diphenylphosphino)amine (dppa, 1) yields complexes [Cu3X2(dppa)3]X (X = Cl, Br, I: 2a–c). The derivates [Cu3X2(dppa)3]PF6 (2a′–c′) have been synthesized by metatheses of 2a–c with NH4PF6. The IR, Raman, 31P{1H} NMR, 1H{31Ρ} NMR, 13C{1H} NMR spectra, and FD mass spectra as well as the conductivity data are reported and discussed together with the X-ray crystal structure of 2a · 5 CH3OH. The structure consists of the trinuclear cations [Cu3Cl2(dppa)3]+, distorted tetrahedral anions [Cl( · · · HOCH3)4]- and molecules of methanol of crystallization, hydrogen bridged to the solvated anions. The Cu3Cl2 core of the cations corresponds closely to a trigonal bipyramid with the copper atoms in the equatorial and the chlorine atoms in the axial positions. The colourless prisms of 2a · 5 CH3OH crystallize in the triclinic space group P1̅, with the lattice constants a = 1368.0(4); b = 1486.7(4); c = 2036.8(10) pm; α = 74.52(3); β = 74.73(3); γ = 82.26(2)°. Raman and 31P{1H} NMR data of the complexes [Cu(X)dppm]4 (dppm = (C6H5)2PCH2P(C6H5)2; X = Br, I) described earlier suggest that these compounds should also be formulated as [Cu3X2(dppm)3]X (4b, c).The Raman spectra of the cations of 2a–c, 2a′–c′ and 4a–c show bands at 165 (X = Cl), 145 (X = Br) and 125 (X = I) cm-1, which can be assigned to the symmetric (XCu3X) stretching mode of the XCu3X unit.

Platin in seiner ungewöhnlichen Oxidationsstufe + III: Diplatin(III)-Komplexe der Modellnukleobase 1-Methyluracil / Platinum in its Unusual Oxidation State + III: Diplatinum(III) Complexes with the Model Nucleobase 1-Methyluracil

1983 ◽  
Vol 38 (11) ◽  
pp. 1441-1445 ◽  
Author(s):  
Bernhard Lippert ◽  
Helmut Schöllhorn ◽  
Ulf Thewalt
Keyword(s):  
Crystal Structure ◽  
Nitric Acid ◽  
Ir Spectra ◽  
Oxidation State ◽  
Structural Similarity ◽  
Single Bond ◽  
Triclinic Space Group ◽  
H Nmr ◽  
Axial Ligands ◽  
Cell Dimensions

Oxidation of the head-tail dimer cis-[(NH3)2Pt(1-MeU)]2(NO3)2 (1-MeU = 1-methyl - uracilato anion, C5H5N2O2) with a mixture of nitrous and nitric acid yields three crystalline species, [(NO2)(NH3)2Pt(C5H5N2O2)2Pt(]SrH3)2(NO2)](NO3)2 · 3 H2O (1), [(H2O)(NH3)2Pt(C5H5N2O2)2Pt(]SrH3)2(NO2)](NO3)2 · 5 H2O (2) and [(NO3)(NH3)2Pt(C5H5N2O2)2Pt(]SrH3)2(NO3)](NO3)2 · 4.5 H2O (3). The crystal structure of 2 has been determined. 2 crystallizes in the triclinic space group P1̄ with cell dimensions a= 11.959(4), b= 11.560(3), c= 11.261(2) Å, α = 89.16(2), β= 104.36(2), γ = 99.61(2)° and Z = 2. The structure was refined to R = 0.056, Rw = 0.061 on 4311 reflections. The Pt-Pt distance within the dinuclear cation of 2 is 2.574(1) Å and cor­responds to a Pt-Pt single bond. The axial ligands are N̲O2 (Ptl) and O̲H2 (Pt2), the equatorial ligands two NH3 groups, N 3 and O4 of 1-MeU for both Pt atoms. The oxidation state of Pt in 2 is +III. 1H NMR and IR spectra of 1, 2, and 3 reveal a close structural similarity of the three compounds.

scholarly journals Chemie polyfunktioneller Moleküle, 114 [1]. Synthese und Struktur eines ionischen und nichtionischen, cyclischen Carbaphosphazens und eines Cobalt(III)phosphazen-Komplexes / Chemistry of Polyfunctional Molecules, 114 [1]. Synthesis and Structure of an Ionic and Non Ionic Cyclic Carbaphosphazene and of a Cobalt(III)phosphazene Complex

1994 ◽  
Vol 49 (12) ◽  
pp. 1763-1773 ◽  
Author(s):  
Jochen Ellermann ◽  
Jörg Sutter ◽  
Falk A. Knoch ◽  
Matthias Moll ◽  
Walter Bauer
Keyword(s):  
Mass Spectra ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr

Reaction of (1) in CH2Cl2 with benzimidazole yields . The salt [4]+BPh4- has been prepared in THF by metathesis of [4]+Cl- with NaBPh4. Deprotonation of the cationic ring in [4]+BPh4- was accomplished using 1,8-diazabicyclo[5.4.01,7]undec-7-ene and resulted in the six-membered carbacyclophosphazene (6). Treating 1 with 8 -hydroxyquinoline in CH2Cl2 yields the octahedral cis-complex = 8-oxyquinolinate group). The com pounds [4]+BPh4-, 6 and 7 are characterized by their IR, Raman, 31P{1H} NMR, 13C{1H} NMR, 1H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4- and 7×0.5 CH2Cl2. The colourless plates of [4]+BPh4- crystallize in the triclinic space group P1̄, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; α = 100.79(2), β = 103.71(3), γ = 108.18(2)°. The black blocks of 7×0.5 CH2Cl2 crystallize in the monoclinic space group P 21/c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; β = 105.86(5)°.

Molecular conformation of 2′-deoxy-3′,5′-di-O-acetyl guanosine. Crystal structure and high resolution proton nuclear magnetic resonance investigations

1988 ◽  
Vol 66 (10) ◽  
pp. 2634-2639 ◽  
Author(s):  
Leo H. Koole ◽  
Henk M. Buck ◽  
Jan A. Kanters ◽  
Arie Schouten
Keyword(s):  
Molecular Conformation ◽  
Proton Nuclear Magnetic Resonance ◽  
Solution Conformation ◽  
Planar System ◽  
Equal Distribution ◽  
Triclinic Space Group ◽  
X Ray ◽  
H Nmr ◽  
Conformational Preferences ◽  
Cell Dimensions

2′-Deoxy-3′,5′-di-O-acetyl guanosine crystallizes in the triclinic space group [Formula: see text], and the cell dimensions are a = 8.643(1) Å, b = 10.122(1) Å, c = 10.391(1) Å, α = 87.04(1)°, β = 73.58(1)°, γ = 72.37(1)°, V = 830.4(2) Å3; Z = 2 molecules per cell. Least-squares refinement converged at R = 0.031 for 3450 observed reflections. The asymmetric unit consists of two independent molecules. The guanine bases are linked via N(1)—H … N(7) and N(2)—H … O(6) hydrogen bonds to form a virtually planar system. Moreover, the conformational preferences of the title compound in DMSO-d6 solution have been determined with 300 MHz 1H NMR. It is found that the X-ray structure and the solution conformation are essentially similar. The C(4′)—C(5′) linkage resides in the gauche+ (g+) or trans (t) rotamers in the solid state, while an approximately equal distribution over g+, t, and gauche− is found in solution.

Reactions of the tetrasulfur pentanitride(-1) ion with halogens: synthesis, spectroscopic characterization, and crystal structure of pentasulfur hexanitride

1979 ◽  
Vol 57 (11) ◽  
pp. 1286-1293 ◽  
Author(s):  
T. Chivers ◽  
J. Proctor
Keyword(s):  
Crystal Structure ◽  
Thionyl Chloride ◽  
Mass Spectra ◽  
Methylene Chloride ◽  
Spectroscopic Characterization ◽  
The Other ◽  
X Ray ◽  
Yellow Orange ◽  
Uv Visible ◽  
Single Bonds

Pentasulfur hexanitride, S5N6, has been prepared in good yield by the reaction of [n-Bu4N+][S4N5−] with bromine (or iodine) in methylene chloride at 0 °C. In contrast, the tetrasulfur pentanitride(−1) ion reacts smoothly with chlorine to give S4N5Cl, while the reaction with sulfuryl chloride produces S4N5Cl and S5N6 and the reaction with thionyl chloride produces a mixture of S3N2O, S3N2O2, S4N4, and S5N6. Pentasulfur hexanitride is an air-sensitive, explosive, yellow-orange solid which sublimes at ca. 45 °C/10−2 Torr without significant decomposition. It has been characterised by infrared, Raman, uv–visible, and mass spectra and by a single crystal X-ray structure determination. The crystals are monoclinic and belong to the space group C2/c, a = 8.787(2), b = 11.190(2), c = 7.427(2) Å, β = 106.46(2)°, V = 700.3(5) Å3, Z = 4, Dc = 2.317 g cm−3. The refined structure (Rw = 0.040) has twofold symmetry and resembles a basket in which an —N=S=N— unit (d(S—N) = 1.54 Å) is the handle which bridges an S4N4 cradle via S—N single bonds (d(S—N) = 1.70 Å). The introduction of this bridge widens one of the [Formula: see text] transannular separations in S4N4 to 3.94 Å while the other is shortened to 2.43 Å. Thus, the S4N4 cradle can be viewed as two five-membered rings fused at the S—S bond.

Cluster Chemistry. XLVII. X-Ray Crystal Structure of OsPt2(μ-CO)3(CO)2(PPh3)3

1986 ◽  
Vol 39 (12) ◽  
pp. 2145 ◽  
Author(s):  
MI Bruce ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
Metal Metal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Triphenylphosphine Ligand

The crystal structure of OsPt2(μ-CO)3(CO)2(PPh3)3 has been determined by single-crystal X-ray diffraction techniques. Crystals are triclinic, space group Pī with unit cell dimensions a 13.593(4), b 15.839(4), c 12.633(8) Ǻ, α 102.97(3), β 108.18(2), γ 84.86(3)° with Z2. The structure was refined by a full-matrix least-squares procedure on 5896 reflections [I ≥ 2.5σ(I)] to final R 0.028 and Rw 0.034. A triphenylphosphine ligand binds each of the metal atoms disposed at the corners of a triangle. Each metal-metal bond is spanned by a bridging carbonyl group. The coordination about the osmium atom is completed by two terminal carbonyl groups.

Molecular conformation of 2′-deoxy-3′,5′-di-O-acetyl adenosine. Crystal structure and high resolution proton nuclear magnetic resonance investigations

1987 ◽  
Vol 65 (2) ◽  
pp. 326-331 ◽  
Author(s):  
Leo H. Koole ◽  
Henk M. Buck ◽  
Jan A. Kanters ◽  
Arie Schouten
Keyword(s):  
Crystal Structure ◽  
Molecular Conformation ◽  
Proton Nuclear Magnetic Resonance ◽  
Solution Conformation ◽  
Orthorhombic Space Group ◽  
One Dimensional ◽  
X Ray ◽  
H Nmr ◽  
Conformational Preferences ◽  
Cell Dimensions

2′-Deoxy-3′,5′-di-O-acetyl adenosine crystallizes in the orthorhombic space group P212121, and the cell dimensions are a = 7.768(1) Å, b = 12.890(1) Å, c = 15.495(1) Å; Z = 4 molecules per cell. Least-squares refinement converged at R = 0.054 for 1752 observed reflections. The adenine bases are linked via N6—H … N1 and N6—H … N7 hydrogen bonds, in such a way that infinite one-dimensional chains are formed. Comments are made on the fact that this structure is entirely different from the parallel dimer that was found for 3′,5′-di-O-acetyl thymidine. Furthermore, the conformational preferences of the title compound in aqueous solution have been determined with 300- and 500-MHz 1H nmr. It is found that the X-ray structure and the solution conformation are essentially similar, except for the C4′—C5′ conformation, that is γ− in the solid state, and predominantly γ+ in solution.

Cyclometallated Compounds. IX. Reactions of 2-Benzoylpyridine With Rhodium(III) Trichloride

1995 ◽  
Vol 48 (9) ◽  
pp. 1573 ◽  
Author(s):  
DJ Degeest ◽  
PJ Steel
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Reaction Conditions ◽  
Initial Product ◽  
X Ray ◽  
X Ray Crystallography

X-Ray crystallography and n.m.r. spectroscopy have been used to study the products of reactions between rhodium(III) trichloride and 2-benzoylpyridine under various reaction conditions. X-Ray crystal structures have shown that the initial product of reaction in refluxing ethanol is a centrosymmetric isomer, as previously proposed, but that this undergoes aqueous hydrolysis to a C2-symmetric isomer, rather than the previously proposed C2v isomer. Reaction in refluxing 2-methoxyethanol produces an unusual complex with one C-N cyclometallated ligand and one N-O coordinated ligand. In Me2SO, the non-cyclometallated ligand of this latter compound undergoes solvolysis to produce a complex containing two Me2SO molecules, one coordinated through oxygen and the other through sulfur. The X-ray crystal structure of this compound is also reported.

scholarly journals Crystal structure of (E)-4-nitro-2-(((3-(tetrahydro-8λ4-[1,3,2]oxazaborolo[2,3-b][1,3,2]oxaborol-8-yl)phenyl)imino)methyl)phenol – water (1/2), C17H18BN3O5·2H2O

2016 ◽  
Vol 231 (1) ◽  
pp. 89-91
Author(s):  
Chunhua Ge ◽  
Juanjuan Liu ◽  
Zhe Xü ◽  
Yang Zhang ◽  
Xiangdong Zhang
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Carbon Atom ◽  
Boron Atom ◽  
Crystal Structure Analysis ◽  
Coordination Bond ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Phenol Water

AbstractThe title compound has been synthesized and characterized by IR, 1H NMR, elemental analysis as well as single crystal X-ray diffraction techniques. Crystal structure analysis reveals that the boron atom is tetrahedrally bonding with one carbon atom, one nitrogen atom, and two oxygen atoms. The bond between nitrogen atom and boron atom is a coordination bond.

Darstellung, Reaktivität und Kristallstruktur von [(CO)3Mn(dppm)2(μ-S)Rh(CO)] / Synthesis, Reactivity and Crystal Structure of [(CO)3Mn(dppm)2(μ-S)Rh(CO)]

1992 ◽  
Vol 47 (5) ◽  
pp. 668-674 ◽  
Author(s):  
O. Heyke ◽  
G. Beuter ◽  
I.-P. Lorenz
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Frame Structure ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Group 2

The reaction of [(CO)3Mn(dppm)2Rh(CO)] (1) with H2S in dichloromethane yields [(CO)3Mn(dppm)2(μ-S)Rh(CO)] (2), which is characterized by IR, 31P{1H}, 1H, 13C{1H} nmr and mass spectra. The crystal structure of 2 was determined by X-ray diffraction: space group P21/n, Z = 4, a = 1232.6(3), b = 2558.8(4), c = 1640.8(2) pm, β = 97.74(2)°, R/Rw = 0.048/0.057. The dimeric complex shows A-frame structure possessing a bridging sulfur and a semibridging CO group. 2 cannot be oxidized to the corresponding SO2 bridged complex [(CO)3Mn(dppm)2(μ-SO2)Rh(CO)] (3). The reaction of 2 with SO2, however, yields the SO2 bridged complex [(CO)2Mn(dppm)2(μ-S)(μ-SO2)Rh(CO)] (5); in dichloromethane 2 is readily chlorinated to afford the salt [(CO)3Mn(dppm),(μ-S)RhCl]Cl (4).

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