Hexacarbonyldieisen-stabilisierte Sulfimid-Derivate, Fe2(CO)6(μ-SNR) / Hexacarbonyl Diiron Stabilized Sulfimide Derivatives, Fe2(CO)6(μ-SNR)

1995 ◽  
Vol 50 (8) ◽  
pp. 1252-1256 ◽  
Author(s):  
Max Herberhold ◽  
Uwe Bertholdt ◽  
Wolfgang Milius
Keyword(s):  
Molecular Structure ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
X Ray ◽  
C Nmr

Hexacarbonyl diiron complexes of N-substituted sulfimides (SNR) have been obtained from the parent tetrahedrane, Fe2(CO)6(μ-SNH) (1), by deprotonation to give the anion Fe2(CO)6(μ-SN-) (2) and subsequent reaction with either trialkyloxonium or carbenium tetrafluoroborates. The new aza-diferra-thia-tetrahedranes, Fe2(CO)6(μ-SNR) (R = CH3 (3a), C2H5 (3b), CPh3 (3c), cyclo-C3Ph3 (3d), cyclo-C7H7 (3e), and cyclo-(C7H7)M (CO)3 with M = Cr (3f), Mo (3g), W (3h)) were characterized by their 1H and 13C NMR as well as their IR and MS spectra. The molecular structure of Fe2(CO)6[SN-cyclo-C7H7Mo(CO)3] (3g) has been determined by X-ray diffraction.

Structure cristalline et moléculaire d'un composé tricyclique contenant le cycle à dix chaînons dioxo diaza diphosphécine

1992 ◽  
Vol 70 (3) ◽  
pp. 809-816 ◽  
Author(s):  
Brigitte Duthu ◽  
Karim El Abed ◽  
Douraid Houalla ◽  
Robert Wolf ◽  
Joël Jaud
Keyword(s):  
Molecular Structure ◽  
Comparative Analysis ◽  
Double Bond ◽  
Mass Spectroscopy ◽  
Crystal And Molecular Structure ◽  
Accurate Information ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Parameters ◽  
C Nmr

The sulfuration of the tricyclic organophosphorous dimer 2 leads easily to the dithiotricyclic derivative 3, which has been characterized by 31P, 1H, and 13C NMR, elemental analysis, and mass spectroscopy. Its crystal and molecular structure has been established by X-ray diffraction and compared to that of 2, which was previously determined. The comparative analysis of X-ray diffraction and NMR parameters gives accurate information about the molecular structure of both compounds. A numerical value of the anistropy cone of the P=S double bond is proposed. Keywords: phosphecine, NMR, X-ray, tricycle.

Synthesis of Rhodium Complexes with Novel Perfluoroalkyl Substituted Cyclopentadienyl Ligands

2001 ◽  
Vol 66 (2) ◽  
pp. 382-396 ◽  
Author(s):  
Jan Čermák ◽  
Kateřina Auerová ◽  
Huong Thi Thu Nguyen ◽  
Vratislav Blechta ◽  
Pavel Vojtíšek ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Chemical Shifts ◽  
Rhodium Complexes ◽  
Carbonyl Complexes ◽  
X Ray Diffraction ◽  
Metal Catalysis ◽  
Chloro Complexes ◽  
X Ray ◽  
Cyclopentadienyl Ligands ◽  
C Nmr

Mixtures of isomers of (perfluoroalkyl)tetramethylcyclopenta-1,3-dienes (CH3)4C5H(CF2)nCF3 (n = 3, 5, 7, 9) were synthesized as precursors of new cyclopentadienyl ligands for organotransition metal catalysis in fluorous biphase media and characterized by combination of GC-MS and 13C NMR spectroscopy. Rhodium(III) chloro complexes [Rh{(CH3)4C5(CF2)nCF3}Cl2]2 and rhodium(I) carbonyl complexes [Rh{(CH3)4C5(CF2)nCF3}(CO)2] were prepared from the cyclopentadienes and molecular structure of [Rh{(CH3)4C5(CF2)5CF3}Cl2]2 was determined by X-ray diffraction. The ligands are electronically close to the unsubstituted cyclopentadienyl as shown by values of carbonyl stretching frequencies in the carbonyl complexes. Neither carbonyl frequencies nor NMR chemical shifts of the complexes are substantially affected by the length of the perfluoroalkyl chain.

The crystal and molecular structure of tetrabenzocyclodecan-1,6-dione

1980 ◽  
Vol 58 (8) ◽  
pp. 777-779 ◽  
Author(s):  
T. Stanley Cameron ◽  
Christine Chan ◽  
David G. Morris ◽  
Alistair G. Shepherd
Keyword(s):  
Molecular Structure ◽  
Diffraction Analysis ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Nmr Spectrum ◽  
X Ray ◽  
C Nmr

The crystals belong to the orthorhombic space group C222, with a = 9.226, b = 12.092, c = 16.513 Å, Z = 4. A single crystal X-ray diffraction analysis has shown that the title compound, in which all carbon atoms are sp2 hybridized, exists with the ten membered ring in a slightly twisted tub conformation. The 13C nmr spectrum is also reported.

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.

[(Dimethylamino)methyl]ferrocene as an Amine Ligand: Study of the Bonding and X-Ray Crystal and Molecular Structure of the Pentacarbonyl{[(dimethylamino)methyl]ferrocene}tungsten Complex

2002 ◽  
Vol 67 (2) ◽  
pp. 228-234 ◽  
Author(s):  
Axel Fischer ◽  
Frank T. Edelmann ◽  
Klaus Jacob ◽  
Ivan Pavlík ◽  
Martin Pavlišta
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Amine Nitrogen ◽  
X Ray ◽  
Nmr Data ◽  
Amine Ligand ◽  
C Nmr

The heterodinuclear complex [W(CO)5(Me2NCH2Fc)] (Fc = ferrocenyl) (1) resulting from the reaction of [(dimethylamino)methyl]ferrocene (2) and [W(CO)6] was studied by single-crystal X-ray diffraction. Its molecular structure confirms the coordination of the amine nitrogen in 2 to tungsten (d(W-N) = 2.359(5) Å) and reveals its trans-influence in the W(CO)5 moiety. The structure is discussed in relation to several previously referred spectroscopic (IR, UV-VIS, 13C NMR) data.

Synthesis and Crystal Structure of 13-cis-Retinoate Aryl Derivatives

2011 ◽  
Vol 236-238 ◽  
pp. 3037-3040
Author(s):  
Wei Guo Yi ◽  
Dong Yan ◽  
Long Yong Xie ◽  
Jian Nan Xiang ◽  
Zhong Cao
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Retinoic Acid ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
C Nmr

A series of 13-cis-retinoate aryl derivatives were synthesized from 13-cis-retinoic acid and phenols or arylalcohol with dicyclohexylcarbodiimide (DCC) as reagent and 4-dimethylaminopyridine (DMAP) as catalyst. Their structures were characterized by1H,13C NMR, IR and MS. The crystal of 3a has been determined by single crystal X-ray diffraction analysis and its molecular structure has been confirmed. Compound 3a belongs to monoclinic system with space group P2 (1)/c, a = 22.235 (3) Å, b = 7.4117 (10) Å, c = 15.990 (2) Å, β = 109.253 (3) °, V = 2487.7 (6) Å3, Z = 4, R = 0.0613, ωR = 0.01437.

The synthesis and structural characterization of a series of pentacoordinate diorganotin(IV) N-arylidene-α-amino acid complexes

1992 ◽  
Vol 70 (4) ◽  
pp. 1114-1120 ◽  
Author(s):  
F. E. Smith ◽  
Rosemary C. Hynes ◽  
T. T. Ang ◽  
L. E. Khoo ◽  
G. Eng
Keyword(s):  
Molecular Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Intermolecular Contacts ◽  
Distorted Trigonal Bipyramidal Coordination ◽  
C Nmr ◽  
Distorted Trigonal Bipyramidal

Eight new diorganotin complexes formulated as R2Sn(OArCR″=NCHR′COO) were prepared and characterized by 1H and 13 C NMR, IR, and elemental analysis. A single crystal X-ray diffraction study of the dibutyltin N-salicylidenevaline complex, Bu2Sn(OC6H4CH=NCH(i-Pr)COO), determines the molecular structure. The crystals are orthorhombic, space group P212121 with a = 9.187(2) Å, b = 10.003(2) Å, c = 23.482(4) Å, V = 2157.8(6) Å3, Z = 4, and Dc = 1.392 g cm−3. The final discrepancy factors are RF = 0.040, and Rw = 0.021 for 1131 significant reflections. The tin atom has a distorted trigonal bipyramidal coordination, with no short intermolecular contacts. The two axial Sn—O bonds of 2.078(10) and 2.151(8) Å and the equatorial Sn—N bond of 2.158(8) Å are among the shortest found in related complexes. The fact that the closest intermolecular Sn—O distance is 4.511(8) Å indicates a nonbridging carbonyl group.

An unusual reaction of a bridged triterpenoid α-diketone with acetic anhydride

1991 ◽  
Vol 56 (12) ◽  
pp. 2917-2935 ◽  
Author(s):  
Eva Klinotová ◽  
Václav Křeček ◽  
Jiří Klinot ◽  
Miloš Buděšínský ◽  
Jaroslav Podlaha ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Acetic Anhydride ◽  
Spectral Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mild Conditions ◽  
Condensation Products ◽  
Unsaturated Lactones ◽  
C Nmr

3β-Acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) reacts with acetic anhydride in pyridine under very mild conditions affording β-lactone IVa and γ-lactones Va and VIIa as condensation products. On reaction with pyridine, lactones Va and VIIa undergo elimination of acetic acid to give unsaturated lactones VIIIa and IXa, respectively. Similarly, the condensation of 20β,28-epoxy-21,22-dioxo-18α,19βH-ursan-3β-yl acetate (IIIb) with acetic anhydride leads to β-lactone IVb and γ-lactone Vb; the latter on heating with pyridine affords unsaturated lactone VIIIb and 21-methylene-22-ketone Xb. The structure of the obtained compounds was derived using spectral methods, particularly 1H and 13C NMR spectroscopy; structure of lactone IVa was confirmed by X-ray diffraction.

scholarly journals Synthesis of Bis(Carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) and Attempt of Synthesis of Gadolinium Bis(Dicarbollide)

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1321
Author(s):  
Yasunobu Asawa ◽  
Aleksandra V. Arsent’eva ◽  
Sergey A. Anufriev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
X Ray Diffraction ◽  
Stable Conformation ◽  
Acyl Chlorides ◽  
X Ray ◽  
Cesium Fluoride ◽  
The Stability

Bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) were prepared by the reactions of the corresponding carboranyl acyl chlorides with ethylenediamine. Crystal molecular structure of 1,1′-μ-(CH2NH(O)C-1,2-C2B10H11)2 was determined by single crystal X-ray diffraction. Treatment of bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 with ammonium or cesium fluoride results in partial deboronation of the ortho-carborane cages to the nido-carborane ones with formation of [7,7′(8′)-μ-(CH2NH(O)C(CH2)n-7,8-C2B9H11)2]2−. The attempted reaction of [7,7′(8′)-μ-(CH2NH(O)CCH2-7,8-C2B9H11)2]2− with GdCl3 in 1,2-dimethoxy- ethane did not give the expected metallacarborane. The stability of different conformations of Gd-containing metallacarboranes has been estimated by quantum-chemical calculations using [3,3-μ-DME-3,3′-Gd(1,2-C2B9H11)2]− as a model. It was found that in the most stable conformation the CH groups of the dicarbollide ligands are in anti,anti-orientation with respect to the DME ligand, while any rotation of the dicarbollide ligand reduces the stability of the system. This makes it possible to rationalize the design of carborane ligands for the synthesis of gadolinium metallacarboranes on their base.

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