Synthesis and characterization of O, O-alkylene dithiophosphate derivatives of dimethyl-and trimethylgermane. Crystal structure of

1994 ◽  
Vol 72 (8) ◽  
pp. 1830-1838 ◽  
Author(s):  
John E. Drake ◽  
Anil G. Mislankar ◽  
Raju Ratnani
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Distorted Tetrahedron ◽  
Dithiophosphoric Acid ◽  
Cell Parameters ◽  
Intramolecular Distance ◽  
Derivatives Of ◽  
C Nmr ◽  
Identical Fashion

The O, O-alkylene dithiophosphate derivatives of dimethyl- and trimethylgermane [Formula: see text], [Formula: see text], [Formula: see text],[Formula: see text], [Formula: see text], and Me3Ge[S2POCH2CEt2CH2O] have been prepared in 70–85% yields by reaction of the salts of the appropriate O,O-alkylene dithiophosphoric acid with dichlorodimethyl-and chlorotrimethylgermane. The compounds were characterized by infrared, Raman, and 1H, 13C, and 31P NMR spectroscopy. The crystal structure of [Formula: see text], was determined and it crystallizes as monoclinic in the space group P21/a (No. 14) with the cell parameters a = 12.368(6) Å, b = 6.897(2) Å, c = 17.923(3) Å, β = 99.00(3)°, V = 2450(2) Å3, Z = 4, R = 0.0455, and Rw = 0.0394. The environment about germanium is essentially that of a distorted tetrahedron resulting in a S—Ge—S angle of 89.9(1)° and a C—Ge—C angle of 121.6(5)°. In contrast with analogous non-cyclic diorganodithiophosphatogermanes, the terminal sulfur atoms are oriented towards germanium rather than away from it to give an average [Formula: see text] intramolecular distance of 3.49(3) Å. The spectra are interpreted as indicating that the dithiophosphate groups are linked in identical fashion in all compounds 1–6. The 1H and 13C NMR spectra are of particular interest in that, unlike the spectra reported previously for related species, the substituents on the atoms in both the five- and six-membered rings maintain their non-equivalence in solution.

scholarly journals Synthesis and Characterization of Zinc(II)-Complexes with S-Alkyl Derivatives of Thiosalicylic Acid

2018 ◽  
Vol 19 (2) ◽  
pp. 113-117 ◽  
Author(s):  
Milos V. Nikolic ◽  
Marina Z. Mijajlovic ◽  
Dusan Lj. Tomovic ◽  
Andriana M. Bukonjic ◽  
Verica V. Jevtic ◽  
...  
Keyword(s):  
Nmr Spectra ◽  
Ethanol Solution ◽  
Alkyl Halides ◽  
Synthesis And Characterization ◽  
Direct Reaction ◽  
Thiosalicylic Acid ◽  
Alkyl Derivatives ◽  
Derivatives Of ◽  
C Nmr

Abstract New zinc(II)-complexes with S-alkyl derivatives of thiosalicylic acid (alkyl = benzyl-(L1), methyl-(L2), ethyl-(L3), propyl-(L4), butyl-(L5)) have been synthesized and characterized by elemental microanalysis, IR spectroscopy, and 1H and 13C NMR spectroscopy. The S-alkyl derivatives of thiosalicylic acid were prepared by alkylation of thiosalicylic acid by adding alkyl halides to an alkaline water-ethanol solution, while the corresponding zinc(II)-complexes were obtained via the direct reaction of ZnCl2 with S-alkyl derivatives of thiosalicylic acid in water. Based on the microanalysis results and the IR and NMR spectra of the S-alkyl derivatives of thiosalicylic acid and the corresponding zinc(II)-complexes, we concluded that the ligands are bidentately coordinated to the zinc(II)-ion.

Monosubstituierte Derivate des Halbsandwich-Komplexes Cp*Ta(CO)4 - Vergleich mit den analogen Vanadiumverbindungen Cp*V(CO)3L und Röntgenstrukturanalyse des γ-Picolin-Komplexes Cp*V(CO)3(NC5H4-Me(4)) / Monosubstituted Derivatives of the Halfsandwich Complex Cp*Ta(CO)4 - Comparison with the Analogous Vanadium Compounds Cp*V(CO)3L and X-Ray Structural Analysis of the γ-Picoline Complex Cp*V(CO)3(NC5H4-Me(4))

2000 ◽  
Vol 55 (12) ◽  
pp. 1188-1194 ◽  
Author(s):  
Max Herberhold ◽  
Gudrun Frohmader ◽  
Jürgen Peukert ◽  
Wolfgang Milius
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Cyclic Ethers ◽  
Vanadium Complex ◽  
Vanadium Compounds ◽  
X Ray ◽  
Derivatives Of ◽  
C Nmr

The photo-induced substitution of a CO ligand in Cp*Ta(CO)4 (1) has been used to prepare a series of Cp*Ta(CO)3L (2) complexes, in which the two-electron ligand L includes, e.g., isonitriles, sulfanes, cyclic ethers, phosphanes and pyridines. The complexes (2a-y) were characterized by their v(CO) frequencies and their 1H and 13C NMR spectra, and were compared - if possible - with the corresponding vanadium complex, Cp*V(CO)4 (3) and its derivatives, Cp*V(CO)3L (4). The molecular structure of the 4-picoline complex Cp*V(CO)3(NC5H4-Me(4)) (4r) has been determined by X-ray crystal structure analysis.

scholarly journals Heteroleptic [Cu(P^P)(N^N)][PF6] Complexes: Effects of Isomer Switching from 2,2′-biquinoline to 1,1′-biisoquinoline

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 185
Author(s):  
Nina Arnosti ◽  
Marco Meyer ◽  
Alessandro Prescimone ◽  
Edwin C. Constable ◽  
Catherine E. Housecroft
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Nmr Spectra ◽  
Phenyl Ether ◽  
Quantum Yields ◽  
Dynamic Processes ◽  
Electrochemical Behaviors ◽  
Ambient Temperatures ◽  
Π Stacking

The preparation and characterization of [Cu(POP)(biq)][PF6] and [Cu(xantphos)(biq)][PF6] are reported (biq = 1,1′-biisoquinoline, POP = bis(2-(diphenylphosphanyl)phenyl)ether, and xantphos = (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane). The single crystal structure of [Cu(POP)(biq)][PF6] 0.5Et2O was determined and compared to that in three salts of [Cu(POP)(bq)]+ in which bq = 2,2′-biquinoline. The P–C–P angle is 114.456(19)o in [Cu(POP)(biq)]+ compared to a range of 118.29(3)–119.60(3)o [Cu(POP)(bq)]+. There is a change from an intra-POP PPh2-phenyl/(C6H4)2O-arene π-stacking in [Cu(POP)(biq)]+ to a π-stacking contact between the POP and bq ligands in [Cu(POP)(bq)]+. In solution and at ambient temperatures, the [Cu(POP)(biq)][PF6]+ and [Cu(xantphos)(biq)]+ cations undergo several concurrent dynamic processes, as evidenced in their multinuclear NMR spectra. The photophysical and electrochemical behaviors of the heteroleptic copper (I) complexes were investigated, and the effects of changing from bq to biq are described. Short Cu···O distances within the [Cu(POP)(biq)]+ and [Cu(xantphos)(biq)]+ cations may contribute to their very low photoluminescent quantum yields.

Preparation of 2,3-Dideoxy-2,3-epimino and 3,4-Dideoxy-3,4-epimino Derivatives of 1,6-Anhydro-β-D-hexopyranoses by Mitsunobu Reaction

1998 ◽  
Vol 63 (6) ◽  
pp. 813-825 ◽  
Author(s):  
Jiří Kroutil ◽  
Tomáš Trnka ◽  
Miloš Buděšínský ◽  
Miloslav Černý
Keyword(s):  
Nmr Spectra ◽  
Mitsunobu Reaction ◽  
Derivatives Of ◽  
C Nmr

A series of new 2-, 3- and 4-benzylamino-2-, 3- and 4-deoxy derivatives of 1,6-anhydro-β-D-hexopyranoses were prepared from 1,6:2,3- and 1,6:3,4-dianhydro-β-D-hexopyranoses by treatment with benzylamine and converted into 2,3-(N-benzylepimino)-2,3-dideoxy- and 3,4-(N-benzylepimino)-3,4-dideoxy-β-D-hexopyranoses of the D-allo, D-galacto and D-talo configuration by Mitsunobu reaction. The structures of benzylamino and benzylimino derivatives were confirmed by 1H and 13C NMR spectra.

Triazene derivatives of (1,x-)diazacycloalkanes. Part VI. 3-({5,5-Dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines — Synthesis, characterization, and X-ray crystal structure

2006 ◽  
Vol 84 (10) ◽  
pp. 1294-1300 ◽  
Author(s):  
Keith Vaughan ◽  
Shasta Lee Moser ◽  
Reid Tingley ◽  
M Brad Peori ◽  
Valerio Bertolasi
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Ion Trapping ◽  
Published Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diazonium Ion ◽  
Derivatives Of ◽  
C Nmr

Reaction of a series of diazonium salts with a mixture of formaldehyde and 1,2-diamino-2-methylpropane affords the 3-({5,5-dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines (1a–1f) in excellent yield. The products have been characterized by IR and NMR spectroscopic analysis, elemental analysis, and X-ray crystallography. The X-ray crystal structure of the p-methoxycarbonyl derivative (1c) establishes without question the connectivity of these novel molecules, which can be described as linear bicyclic oligomers with two imidazolidinyl groups linked together by a one-carbon spacer. This is indeed a rare molecular building block. The molecular structure is corroborated by 1H and 13C NMR data, which correlates with the previously published data of compounds of types 5 and 6 derived from 1,3-propanediamine. The triazene moieties in the crystal of 1c display significant π conjugation, which gives the N—N bond a significant degree of double-bond character. This in turn causes restricted rotation around the N—N bond, which leads to considerable broadening of signals in both the 1H and 13C NMR spectra. The molecular ion of the p-cyanophenyl derivative (1b) was observed using electrospray mass spectrometry (ES + Na). The mechanism of formation of molecules of type 1 is proposed to involve diazonium ion trapping of the previously unreported bisimidazolidinyl methane (13).Key words: triazene, bistriazene, imidazolidine, synthesis, X-ray crystallography, NMR spectroscopy.

scholarly journals STRUCTURAL CHARACTERIZATION OF THE NEW DIAMOND-LIKE SEMICONDUCTOR CuNbGaSe3

2018 ◽  
Vol 15 (29) ◽  
pp. 228-233
Author(s):  
J. A. FLORES-CRUZ ◽  
G. E. DELGADO ◽  
J. E. CONTRERAS ◽  
M. QUINTERO ◽  
L. NIEVES ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Behavior ◽  
Secondary Phase ◽  
Chalcopyrite Structure ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Chalcogenide Compound ◽  
Semiconductor Type

The chalcogenide compound CuNbGaSe3, belonging to the system I-II-III-VI3, has been investigated by means of X-ray powder diffraction and its crystal structure has been refined by the Rietveld method.This is a material of the semiconductor type, which improves the properties of a simple semiconductor like CuGaSe2 because it ads spintronic applications due to its magnetic behavior. The powder pattern was composed by 94.2% of the principal phase CuNbGaSe3 and 5.8% of the secondary phase Cu0.667NbSe2. This material crystallizes with a CuFeInSe3-type structure in the tetragonal space group P4 2c (Nº 112), unit cell parameters a = 5.6199(4) Å, c = 11.0275(2) Å, V = 348.28(4) Å3, with a normal adamantane-structure where occurs a degradation of symmetry from the chalcopyrite structure I4 2d to a related structure P4 2c.

Über Antimon-haltige Heterocyclen, V Antimon(III)-dithiolate mit verbrückten 5-und 8-Ringen/On Heterocyclic Systems Containing Antimony, V Antimony(III) Dithiolates with Bridged 5-and 8 -Membered Rings

1986 ◽  
Vol 41 (11) ◽  
pp. 1455-1460 ◽  
Author(s):  
Harald M. Hoffmann ◽  
Martin Dräger
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Coordination Polyhedra ◽  
Starting Point ◽  
C Nmr

Abstract For diamony(III)-trisdithiolates two constitutions (bicyclic B or two bridged monocycles C) are possible. Two synthetical paths to three examples Sb2(XS2)3 with X = CH2CH2 (1), CH2CH2- O - CH2CH2 (2), CH2CH2- S - CH2CH2 (3) are reported. 13C NMR spectra in CDCl3 solution show the constitution C for 2 and 3, and a possible equilibrium C ⇌ 4:1) for 1. This corresponds to the result of a crystal structure analysis (R = 0.027). The constitution C found in solid 1 exhibits expanded coordination polyhedra around the two antimony atoms which indicate a starting point for rearrangement into the constitution B. The two bridged 5-membered rings have different conformations: envelope and half-chair.

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