Synthesis and Characterization of N-Methyl-Substituted Germocanes. Crystal Structure of MeN(CH2CH2O)2GeBr2

2003 ◽  
Vol 58 (12) ◽  
pp. 1165-1170 ◽  
Author(s):  
Sergey S. Karlov ◽  
Elmira Kh. Yakubova ◽  
Ekaterina V. Gauchenova ◽  
Anastasia A. Selina ◽  
Andrei V. Churakov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structural Data ◽  
Closed Shell ◽  
Bond Critical Point ◽  
Composition And Structure ◽  
Elemental Analyses ◽  
Laplacian Of Charge Density ◽  
Good Agreement ◽  
C Nmr

The reaction of GeHal4 with MeN(CH2CH2OSiMe3)2 affords dihalogermocanes MeN(CH2 CH2O)2GeHal2 (1, Hal = Br; 2, Hal = Cl). Treatment of Me2Ge(NMe2)2 with MeN(CH2CH2OH)2 leads to dimethylgermocane MeN(CH2CH2O)2GeMe2 (3). The composition and structure of 1-3 were established by elemental analyses, 1H, 13C NMR spectroscopy, and mass spectrometry. The crystal structure of 1 is reported; structural data obtained from geometry DFT optimization on 1 are in good agreement with experimental results. Values of the electron density in the N→Ge bond critical point and the Laplacian of charge density for 1-3 indicate a closed-shell interaction between the Ge and N atoms.

Synthesis and Characterization of Chromium Tricarbonyl Complexes of 1-Phenylgermatrane and 1-Phenylazagermatrane. Crystal Structure of [N(CH2CH2O)3GeC6H5]Cr(CO)3

2002 ◽  
Vol 57 (9) ◽  
pp. 993-998 ◽  
Author(s):  
Sergey S. Karlov ◽  
Denis A. Sorokin ◽  
Yuri F. Oprunenko ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Chromium Tricarbonyl ◽  
Elemental Analyses ◽  
Chromium Tricarbonyl Complexes ◽  
C Nmr

The reaction of 1-phenylgermatrane (1) and 1-phenylazagermatrane (2) with Cr(CO)6 affords chromium tricarbonyl complexes [N(CH2CH2O)3GeC6H5]Cr(CO)3 (6) and [N(CH2- CH2NH)3GeC6H5]Cr(CO)3 (7). In contrast, the same reaction of Cr(CO)6 with 1-(9-anthracenyl) germatrane (3) does not proceed. Composition and structures of the 6 and 7 were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry. The crystal structure of 6 is reported

Synthesis and characterization of N-glucosylated dithiadiazepine derivatives through carbon-sulfur bond formation

2015 ◽  
Vol 21 (5) ◽  
pp. 269-272 ◽  
Author(s):  
Snehal A. Chavan ◽  
Avinash G. Ulhe ◽  
Baliram N. Berad
Keyword(s):  
Bond Formation ◽  
Synthesis And Characterization ◽  
Mass Spectral ◽  
H Nmr ◽  
Chemical Structures ◽  
Elemental Analyses ◽  
New Compounds ◽  
Sulfur Bond ◽  
C Nmr

AbstractNew 4,7-bis(arylamino)-2-tetra-O-acetyl-β-d-glucopyranosylimino-1,3,5,6-dithiadiazepines were synthesized via reaction of N-tetra-O-acetyl-β-d-glucopyranosyl isocyanodichloride with 1,6-diaryl-2,5-dithio-bis-ureas without using any catalyst. Thus, the synthesis of 7-membered heterocycles containing two sulfur and two nitrogen atoms through carbon-sulfur bond formation was explored. The chemical structures of these new compounds were elucidated by IR, 1H NMR, 13C NMR, mass spectral, and elemental analyses.

scholarly journals Beiträge zur Chemie der Schwefelhalogenide, 9 [1]. Trifhiormethyldichlorsulfonium(IV)-hexafluoroarsenat(V) / Contributions to the Chemistry of Sulfur Halides, 9 [1] Trifluoromethyldichlorosulfonium(IV) Hexafluoroarsenate(V )

1985 ◽  
Vol 40 (9) ◽  
pp. 1123-1129 ◽  
Author(s):  
Rolf Minkwitz ◽  
Ulrike Naß ◽  
Armin Radünz ◽  
Hans Preut
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
Structural Data ◽  
Normal Coordinate Analysis ◽  
Vibrational Assignment ◽  
Normal Coordinate ◽  
Sulfonium Salt ◽  
C Nmr

The synthesis of CF3SCl2+AsF6- is reported. The sulfonium salt is characterised by IR, Raman, 19F and 13C NMR spectroscopy. The vibrational assignment is based on a Cs model for the cation and assisted by a normal coordinate analysis. The crystal structure has been determined from three-dimensional diffractometer data at -133 K. The structural data for the cation are: C-F = 128.8(5) pm, C-S = 197,8(3) pm, S-Cl = 195,9(1) pm and F-C-F = 111,8(3)°, Cl-S-Cl = 104,22(5)°, C-S-Cl = 99,8(1)°.

scholarly journals Synthesis, crystal structure, and theoretical studies of a macrocyclic silver(I) complex of imino-pyridyl Schiff base ligand

2021 ◽  
Vol 12 (3) ◽  
pp. 248-255
Author(s):  
Jahangir Mondal ◽  
Meman Sahu ◽  
Bhaskar Sharma ◽  
Rakesh Ganguly ◽  
Shubhamoy Chowdhury ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Complex I ◽  
Average Distance ◽  
Spectroscopic Techniques ◽  
Triclinic Space Group ◽  
X Ray ◽  
Elemental Analyses ◽  
Photophysical Studies ◽  
Pyridyl Ligand

The synthesis and characterization of an imino-pyridyl ligand N,N'-(butane-1,4-diyl)bis(1-(pyridin-2-yl)methanimine) (L) and its Ag(I)ClO4 complex (I) by various spectroscopic techniques and elemental analyses is presented in this study. X-ray single crystal structure of complex I revealed that in complex I, each Ag(I) ion is tetra coordinated with two pyridine N-atoms and two imine N-atoms of the ligand L, forming a macrocyclic dimeric Ag(I) grid. In the macrocyclic dimer complex I, Ag-Ag separation along the chain is 5.318 Å. The Ag-Npy average distance is 2.396 Å and that of the Ag-Nim is 2.257 Å. The macrocyclic dimer complex I is supramolecularly arranged by π-stacking interactions. Computational, Hirshfeld surface analysis and photophysical studies on ligand L and complex I have also been performed. Crystal data for C32H36Ag2Cl2N8O8 (M =947.33 g/mol): Triclinic, space group P-1 (no. 2), a = 9.1714(12) Å, b = 10.4373(14) Å, c = 10.8297(14) Å, α = 112.317(3)°, β = 91.391(3)°, γ = 92.353(3)°, V = 957.3(2) Å3, Z = 1, T = 293.15 K, μ(MoKα) = 1.220 mm-1, Dcalc = 1.643 g/cm3, 10248 reflections measured (4.07° ≤ 2Θ ≤ 53.098°), 3966 unique (Rint = 0.0280, Rsigma = 0.0331) which were used in all calculations. The final R1 was 0.0722 (I > 2σ(I)) and wR2 was 0.2229 (all data).

On Attempts to Synthesize Lanthanide Complexes of the Dianionic Fluorenyl-alkoxo Ligand [C13H8-cyclo-C6H10-O]2-. Crystal Structure of (C13H9-cyclo-C6H10-O)LaI2(DME)2

2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectra ◽  
Single Crystal ◽  
Lanthanide Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.

Synthesis and characterization of silver(I) complexes of thioureas and thiocyanate: crystal structure of polymeric (1,3-diazinane-2-thione)thiocyanato silver(I)

2015 ◽  
Vol 70 (8) ◽  
pp. 541-546 ◽  
Author(s):  
Muhammad Nawaz Tahir ◽  
Anvarhusein A. Isab ◽  
Fozia Afzal ◽  
Kashif Raza ◽  
Shah Muhammad ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectrum ◽  
Coordination Environment ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Ir And Nmr Spectroscopy ◽  
A Chain ◽  
Distorted Tetrahedral Coordination ◽  
C Nmr

AbstractSilver(I) complexes of thioureas and thiocyanate, [(Tu)AgSCN], [(Metu)AgSCN], [(Dmtu)AgSCN], [(Tmtu)(AgSCN)1.5], [(Imt)AgSCN], and [(Diaz)AgSCN] (where Tu = thiourea, Metu = N-methylthiourea, Dmtu = N,N′-dimethylthiourea, Tmtu = N,N,N′,N′-tetramethylthiourea, Imt = 1,3-imidazolidine-2-thione, and Diaz = 1,3-diazinane-2-thione), have been prepared and characterized by elemental analysis, IR and NMR spectroscopy, and thermal analysis. The crystal structure of one of them, [(Diaz)Ag(SCN)] (1), was determined by X-ray crystallography. The crystal structure of 1 shows that the complex exists in the form of a chain-like polymer comprising [Ag(μ2-Diaz)(μ2-SCN)] units. The silver atoms are bridged by μ2-thione sulfur atoms of Diaz and μ2-thiocyanate sulfur atoms. Thereby each silver atom adopts a distorted tetrahedral coordination environment comprising four sulfur atoms, two from thione and two from thiocyanate ligands. An upfield shift in the >C=S resonance of thiones in 13C NMR and a downfield shift in the N–H resonance in 1H NMR are consistent with the sulfur coordination to silver(I). The appearance of a band around 2100 cm–1 in the IR and a resonance around 125 ppm in the 13C NMR spectrum indicates the binding of thiocyanate to silver(I).

Darstellung und Charakterisierung von einigen unsymmetrischen Chlordiorganophosphanen RR′PCI / Preparation and Characterization of Some Unsymmetrical Chlorodiorganophosphines RR′PCI

1989 ◽  
Vol 44 (4) ◽  
pp. 502-504 ◽  
Author(s):  
Jung Su Han ◽  
Werner Wolfsberger
Keyword(s):  
Spectroscopic Data ◽  
Grignard Reagents ◽  
Elemental Analyses ◽  
C Nmr

Some unsymmetrical chlorophosphines RR′PCI were prepared by the reaction of RPCl2 (R = CH3, C2H5, i-C3H7, C6H5) with Grignard reagents R′MgCl (R′ = c-C5H9, c-C6H11, i-C3H7) and characterized by elemental analyses and spectroscopic data (IR, 31P and 13C NMR).

Darstellung und Kristallstrukturbestimmung von 1,2-Di-t-butyl-1,2-diiodo- diarsan (t-C4H9AsI)2 und Synthese von 1,2,3,4-Tetrakis(t-butyl)tetraarsetan (t-C4H9As)4 über selektive Reduktion von t-Butylarsendiiodid t-C4H9AsI2 Synthesis and Crystal Structure of 1,2-Di-t-butyl-1,2-diiododiarsane (t-C4H9AsI)2 and Synthesis of 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4 via Selective Reduction of t-Butylarsenic Diiodide t-C4H9AsI2

1997 ◽  
Vol 52 (7) ◽  
pp. 790-794 ◽  
Author(s):  
Klaus Megges ◽  
Evgeni V. Avtomonov ◽  
Jörg Lorberth
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
Selective Reduction ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
High Yields ◽  
C Nmr

Abstract 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4(4) has been synthesized by reduction of t-butylarsenic (III) diiodide (1) with equivalent quantities of either Mg, Ca, Zn, Li, or CoCp2 in THF at low temperatures in high yields. Treatment of 1 with CoCp2 in a molar ratio 1:1 in n-pentane at -78 °C leads to the formation of 1,2-di-t-butyl-1,2-diiododiarsine (2) (t-C4H9AsI)2 in 69 % yield. The products have been characterized by spectroscopic methods (H, 13C-NMR, EI-MS) and elemental analyses. The crystal structure of 2 has been determined by X-ray diffraction methods.

scholarly journals Regioselective synthesis and characterization of monovanadium-substituted β-octamolybdate [VMo7O26]5−

2019 ◽  
Vol 75 (7) ◽  
pp. 872-876
Author(s):  
Lukáš Krivosudský ◽  
Alexander Roller ◽  
Annette Rompel
Keyword(s):  
Aqueous Solution ◽  
Hydrogen Peroxide ◽  
The Other ◽  
Synthesis And Characterization ◽  
One Pot ◽  
X Ray ◽  
Composition And Structure ◽  
Elemental Analyses ◽  
Crystallization Solution

The monovanadium-substituted polyoxometalate anion [VMo7O26]5−, exhibiting a β-octamolybdate archetype structure, was selectively prepared as pentapotassium [hexaikosaoxido(heptamolybdenumvanadium)]ate hexahydrate, K5[VMo7O26]·6H2O (VMo7 ), by oxidation of a reduced vanadomolybdate solution with hydrogen peroxide in a fast one-pot approach. X-ray structure analysis revealed that the V atom occupies a single position in the cluster that differs from the other positions by the presence of one doubly-bonded O atom instead of two terminal oxide ligands in all other positions. The composition and structure of VMo7 was also confirmed by elemental analyses and IR spectroscopy. The selectivity of the synthesis was inspected by a 51V NMR investigation which showed that this species bound about 95% of VV in the crystallization solution. Upon dissolution of VMo7 in aqueous solution, the [VMo7O26]5− anion is substantially decomposed, mostly into [VMo5O19]3−, α-[VMo7O26]4− and [V2Mo4O19]4−, depending on the pH.

scholarly journals Synthesis, Crystal Structure and Spectral Properties of Copper(II) 2-Chloronicotinato Complexes with N-Heterocyclic Ligands

2016 ◽  
Vol 15 (2) ◽  
pp. 190-199 ◽  
Author(s):  
Jozef Miklovič ◽  
Dušan Valigura ◽  
Ingrid Svoboda ◽  
Ján Moncol ◽  
Milan Mazúr
Keyword(s):  
Crystal Structure ◽  
Spectral Properties ◽  
Crystal Structure Analysis ◽  
Synthesis And Characterization ◽  
Epr Spectrum ◽  
Heterocyclic Ligands ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Good Agreement

Abstract The synthesis and characterization of nine new copper(II) complexes [Cu(2-Clnic)2L2] (where 2-Clnic is 2-chloronicotinate anion, L is imidazole – Im, benzimidazole – Bim, furo[3,2-c]pyridine – FP, 2-methylfuro[3,2-c]pyridine – MFP, or [1]benzofuro[3,2-c]pyridine – BFP), [Cu(2-Clnic)2(INA)] (where INA is isonicotinamide), [Cu(2-Clnic)2(4-py)]·H2O (where 4-py is 4-methylpyridine) and [Cu2(2-Clnic)4(IQ)2] (where IQ is isoquinoline) are reported. The characterizations were based on elemental analysis, infrared, electronic and EPR spectra. The dimeric character of [Cu2(2-Clnic)4(IQ)2] is assumed on the EPR spectrum and the other spectral methods. The crystal structure of the [Cu(2-Clnic)2(Bim)2] and [Cu(2-Clnic)2(FP)2] complexes have been determined by X-ray crystal structure analysis. Both complexes exhibit the hexacoordination coordination polyhedra around copper atom that lies in the crystallographic center of symmetry. The distorted tetragonal-bipyramidal (4+2) arrangement is in good agreement with spectral data that have suggested an asymmetric chelate coordination of the carboxylic group.

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