Coordination Compounds of Lanthanide Nitrates with Dimorpholido-N-trichloroacetylphosphorylamide. The Structure of Di(dimorpholido-N-trichloroacetylphosphorylamide)- diaqua Neodymium(III)trinitrate

2000 ◽  
Vol 55 (3-4) ◽  
pp. 262-268 ◽  
Author(s):  
Vladimir A. Ovchynnikov ◽  
Taras P. Timoshenko ◽  
Vladimir M. Amirkhanov ◽  
Joachim Sieler ◽  
Viktor V. Skopenko
Keyword(s):  
Molecular Structure ◽  
Coordination Compounds ◽  
Methanol Solution ◽  
Acetone Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Data ◽  
Weak Electrolytes ◽  
Phosphoryl Oxygen ◽  
Lanthanide Nitrates

Abstract Lanthanide, Carbacylamidophosphate The coordination compounds of the general formula Ln(NO3)3(HL)2(H2O)2 H2O , where Ln = La, Ce -Nd, Sm -Dy, HL = CCl3C(O)NHP(O)[N(CH2CH2)2O]2, dimorpholido-N-tri-chloroacetylphosphorylamide, have been synthesized. The complexes were studied by IR, 1H and 31P NMR and UV-VIS absorption spectroscopies. X-ray diffraction analyses indicate that all synthesized compounds are isostructural. The crystal structure of Nd(NO3)3(HL)2(H2O)2 H2O was solved (monoclinic, a = 11.0467(3), b = 15.9080(5), c = 24.1921(7) Å, β = 96.4080(10)°, space group P21/n, V = 4224.7(2) Å3, Z = 4, R = 0.049, wR = 0.0915). The complex has a molecular structure. The monodentate neutral phosphorictriamide ligands are coordinated to the metal atom via the phosphoryl oxygen atom. The coordination polyhedron of Nd is a sphenocorona; C.N. = 10(60[NO3-], 20[HL], 20[H2O]). It was shown that these compounds in methanol solution are 1:1 electrolytes, and in acetone solution weak electrolytes. According to NMR data in acetone solution the complexes of the lanthanides with the ligand {HL} have axial symmetry.

1,2-Hydroboration of Alkyn-1-yldichlorosilanes using Triethylborane

2008 ◽  
Vol 63 (11) ◽  
pp. 1267-1275 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Ezzat Khan ◽  
Wolfgang Milius
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Hydrogen Transfer ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ethyl Group ◽  
Nmr Data

Abstract Triethylborane, BEt3, can act as a 1,2-hydroborating reagent towards alkyn-1-ylsilanes, depending on the nature of the silane. A mechanism is proposed invoking hydrogen transfer from the β -carbon of one ethyl group, quite different from the 1,2-hydroboration mechanism using tri-n-propylborane, BnPr3. The structure of the products has been confirmed by comparison with that obtained using 9-borabicyclo[3.3.1]nonane, 9-BBN, as a well established 1,2-hydroborating reagent. All products have been characterized by a consistent set of NMR data (1H, 11B, 13C and 29Si NMR). The molecular structure of (Z)-1-dichlorosilyl-1-[9-(9-borabicyclo[3.3.1]nonyl)]-2-phenylethene has been determined by single crystal X-ray diffraction.

Synthese und Eigenschaften einiger Silylethinylsilane; Molekülstruktur von Tetrakis(trimethylsilylethinyl)silan / Synthesis and Properties of Some Silylethynylsilane; Molecular Structure of Tetrakis(trimethylsilylethynyl)silane

1988 ◽  
Vol 43 (1) ◽  
pp. 49-52 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Jan Ebenhöch
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Silicon Atom ◽  
Grignard Reagent ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Nmr Data

Abstract Trimethylsilylethine (1) has been prepared from C2H2, sodium and Me3SiCl in anisole. The product can be converted into a Grignard reagent Me3SiC≡CMgCl using iPrMgCl. This reagent yields the compounds Me3SiC≡CSiH3, (Me3SiC≡C)2SiH2, (Me3SiC≡C)3SiH, and (Me3SiC≡C)4Si (2-5) when treated with equivalent amounts of H3SiBr, H2SiBr2, HSiCl3, or SiCl4. respectively. The new silanes have been characterized by NMR data. The crystal structure of (Me3SiC≡C)4Si has been determined by single crystal X-ray diffraction. It shows the expected tetrahedral geometry at he central silicon atom with four linear SiC≡CSi linkages.

Darstellung und Struktur eines zweikernigen Vanadium(V)-Komplexes mit den terminal gebundenen Stickstoffliganden NtC4H9, NHtC4H9 und NH2tC4H9: [ VCl(μ-Cl)(NtC4H9)(NHtC4H9) (NH2tC4H9) ]2 / Synthesis and Molecular Structure of a Binuclear Vanadium(V) Complex Containing the Terminal Nitrogen Ligands NtC4H9, NHtC4H9, NH2tC4H9: [VCl(μ-Cl)(NtC4H9)(NHtC4H9)(NH2tC4H9)]2

1985 ◽  
Vol 40 (3) ◽  
pp. 363-367 ◽  
Author(s):  
Fritz Preuss ◽  
Edith Fuchslocher ◽  
William S. Sheldrick
Keyword(s):  
Molecular Structure ◽  
Diffraction Analysis ◽  
Vanadium Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nitrogen Ligands ◽  
Nmr Data ◽  
Distorted Octahedral ◽  
Tert Butylamine ◽  
Cl Atoms

tC4H9N = VCl2(NHtC4H9) and the tert-butylamine complex [tC4H9N=VCl2(NHtC4H9)(NH2tC4H9)] have been prepared by reaction of tC4H9N=VCl3 with NH2tC4H9. 1H and 51V NMR data of these compounds are reported. The complex was investigated by X-ray diffraction analysis; the structure has been found to be a binuclear vanadium complex bridged by two Cl-atoms with a distorted octahedral arrangement of the ligands.

[(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.

Alkynylsilanes and Alkynyl(vinyl)silanes. Synthesis,Molecular Structures and Multinuclear Magnetic Resonance Study

2010 ◽  
Vol 65 (6) ◽  
pp. 725-744 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Stefan Bayer ◽  
Oleg L. Tok ◽  
Elena V. Klimkina ◽  
Wolfgang Milius ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Magnetic Resonance Study ◽  
X Ray ◽  
Nmr Data ◽  
Vinyl Silanes ◽  
Methyl Phenyl

Alkynylsilanes bearing one to four alkynyl groups at silicon, with organyl groups (Me, Ph, Vin), H, Cl at silicon, and with substituents H, nBu, tBu, Ph, C6H4-4-Me, 3-thienyl, CH2NMe2 at the C≡C bond, were prepared, and their 13C and 29Si NMR data are reported. The results of X-ray structure analyses of three representative derivatives [di(phenylethynyl)dimethylsilane, di(phenylethynyl) methyl(phenyl)silane, and tri(phenylethynyl)methylsilane] are presented. The chemistry of mono- and dialkynylsilanes was further developed to prepare compounds with alternating Si atoms and C≡C bonds, affording new dialkynylsilanes as well as numerous new vinylsilanes which have also been characterized by 13C and 29Si NMR spectroscopy in solution. In the case of ethynyl(triphenylsilylethynyl) dimethylsilane, the molecular structure was determined 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.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

Reactions of (η5-C9H7)Rh(η2-C2H4)2 with quinones: molecular structure of [(η5-C9H7)Rh(2,3,5,6-C6O2(CH3)4)]

1999 ◽  
Vol 77 (2) ◽  
pp. 199-204
Author(s):  
Stephen A Westcott ◽  
Nicholas J Taylor ◽  
Todd B Marder
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Ground State ◽  
Slip Parameter ◽  
X Ray Diffraction ◽  
X Ray ◽  
A Value ◽  
Hinge Angle

Reactions of (η5-C9H7)Rh(η2-C2H4)2 (1) with quinones were investigated. Substitution of the labile ethylene ligands was observed upon addition of either duroquinone (2,3,5,6-tetramethyl-1,4-benzoquinone) or 1,4-benzoquinone to complex 1. The molecular structure of neutral (η5-C9H7)Rh(2,3,5,6-C6O2(CH3)4) (3), determined by X-ray diffraction, shows that the duroquinone ligand lies in a plane nearly parallel to the indenyl group. The carbonyl moieties of duroquinone lie in a plane incorporating Rh, C2, and the midpoint between C3a and C7a of the indenyl ring. The slip parameter (Δ= d(average Rh-C3a,7a) -d(average Rh-C1,3)) was calculated to be 0.112(2) Å; whereas a value of ca. 0.05 Å had been obtained previously from film data. Values for the hinge angle (HA = angle between normals to the least-squares planes defined by C1, C2, C3 and C1, C7a, C3a, C3) and fold angle (FA = angle between normals to the least-squares planes defined by C1, C2, C3 and C3a, C4, C5, C7, C7a) are 7.2° and 4.0°, respectively.Key words: indenyl, rhodium, quinones, ring-slippage, ground-state distortion.

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