Alkinol- und Alkindiol-substituierte Titanocen-Komplexe; Synthese, Reaktionsverhalten und Strukturmerkmale / Alkyne-ol and Alkyne-diol Substituted Titanocene Complexes; Synthesis, Reaction Behaviour and Structural Features

1995 ◽  
Vol 50 (6) ◽  
pp. 923-930 ◽  
Author(s):  
Heinrich Lang ◽  
Katrin Köhler ◽  
Mathias Herres ◽  
Christiane Emmerich
Keyword(s):  
Spectroscopic Data ◽  
Structural Features ◽  
Synthesis Reaction ◽  
Addition Compound ◽  
X Ray ◽  
C Nmr

The reaction of (η5-C5H4SiMe3)2TiCl2 (1) with HO(CH2)nC ≡ CR (2a: n = 1, R = H; 2b: n = 1, R = CH3; 2c: n = 1, R = CH2OH ; 3: n = 2, R = H; 4: n = 4, R = H) affords in toluene at 25 °C in the presence of NEt3 the monoalkyne-ol substituted titanocenes (η5-C5H4SiMe3)2Ti(Cl)[O(CH2)nC ≡ CR] (5a: n = 1. R = H; 5b: n = 1, R = CH3; 5c: n = 1, R = C H2OH; 6: n = 2, R = H; 7: n = 4. R = H ). Compound 5c reacts with one equivalent of 1 in the presence of NEt3 to yield (η5-C5H4SiMe3)2(Cl)Ti-OCH2C ≡ CCH2O -Ti(Cl)(η5-C5H4SiMe3)2 (8). In addition, compound 8 can be synthesized directly by treatment of (η5- C5H4SiMe3)2TiCl2 (1) with 0.5 equivalents of HOCH9C≡CCH2OH (2c) in the presence of NEt3. The reaction of (η5-C5H4SiMe3)2Ti(Cl)(OCH2C ≡ CCH3) (5b) with Co2(CO)8 (9) yields (η5-C5H4SiMe3)2Ti(Cl)[(η2-OCH2C ≡ CCH3)Co2(CO)6] (10). Treatment of 5b or 10 with HCl(aq) (11) leads to the formation of (η5-C5H4SiMe3)2TiCl2 (1) and HOCH2C ≡ CCH3 (2b) (reaction of 5b with 11) or (η5-C5H4SiMe3)2TiCl2 (1) and [(η2-HOCH2C ≡ CCH3)Co2(CO)6] (12) (reaction of 10 with 11). All compounds have been characterized by analytical and spectroscopic data (IR , 1H, 13C NMR, MS) and (η5-C5H4SiMe3)2Ti(Cl)(OCH2C ≡ CCH3) (5b) by X -ray analysis.

A New Bis-Tröger's Base: Synthesis, Spectroscopy, Crystal Structure and Isomerization

2006 ◽  
Vol 71 (9) ◽  
pp. 1278-1302 ◽  
Author(s):  
Martin Valík ◽  
Pavel Matějka ◽  
Eberhardt Herdtweck ◽  
Vladimír Král ◽  
Bohumil Dolensky
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Data ◽  
The Other ◽  
X Ray Diffraction ◽  
One Pot ◽  
Molecular Tweezers ◽  
X Ray ◽  
Troger's Base ◽  
Ir And Raman ◽  
C Nmr

A new bis-Tröger's base was prepared from a tetraamine precursor as a mixture of two diastereoisomers. One of the isomers has a chair-like geometry, and the other possesses a boat-like geometry, embodying molecular tweezers. A one-pot preparation of bis-TB isomers and their interconversion under acid conditions was also studied. Structures of both isomers were confirmed by single-crystal X-ray diffraction. Extensive spectroscopic data, including 1H and 13C NMR, IR and Raman spectra of the isomers, are given.

scholarly journals Solid State Structure and Absolute Configuration of Filifolinol Acetate

2011 ◽  
Vol 6 (6) ◽  
pp. 1934578X1100600
Author(s):  
Marcelo A. Muñoz ◽  
Alejandro Urzúa ◽  
Javier Echeverría ◽  
Brenda Modak ◽  
Pedro Joseph-Nathan
Keyword(s):  
Density Functional Theory ◽  
Solid State ◽  
Absolute Configuration ◽  
Spectroscopic Data ◽  
Density Functional ◽  
Vibrational Circular Dichroism ◽  
State Structure ◽  
Functional Theory ◽  
X Ray ◽  
C Nmr

Careful reevaluation of the 1H and 13C NMR spectroscopic data of filifolinol acetate (4) led to the reassignment of the C-10 and C-11 signals, as well as the gem-dimethyl signals. Single crystal X-ray analysis provided an independent structural confirmation of 4, and comparison of the experimental vibrational circular dichroism spectrum with calculations performed using density functional theory provided the absolute configuration of this 3H-spiro-1-benzofuran-2,1′-cyclohexane and related molecules.

(3E)-5-Hydroxy-3-[5-(hydroxymethyl)furan-2-ylmethylene]-1-benzofuran-2(3H)-one

2007 ◽  
Vol 63 (11) ◽  
pp. o4354-o4354
Author(s):  
Hong-Yan Ma ◽  
Ji Shi ◽  
Chang-Hong Wang ◽  
Zheng-Tao Wang
Keyword(s):  
Hydrogen Bonds ◽  
Spectroscopic Data ◽  
Furan Ring ◽  
Crystallographic Analysis ◽  
Relative Configuration ◽  
X Ray ◽  
H Nmr ◽  
Compound C ◽  
A Chain ◽  
C Nmr

The title compound, C14H10O5, was isolated from Senecio cannabifolius Less var. integrifolius aqueous extract. The structure was elucidated on the basis of spectroscopic data, including MS, 1H NMR and 13C NMR, and the relative configuration was confirmed by X-ray crystallographic analysis. The benzofuran ring is almost coplanar with the furan ring [dihedral angle = 10.47 (15)°]. A chain is formed through supramolecular R 2 2(10) synthons and three-centre hydrogen bonds.

Selektive Additionsreaktionen an bifunktionalen neutralen Phosphenium-Ion-Komplexen / Selective Addition Reactions of Bifunctional Neutral Phosphenium Ion Complexes

1991 ◽  
Vol 46 (12) ◽  
pp. 1650-1658 ◽  
Author(s):  
Heinrich Lang ◽  
Michael Leise ◽  
Wolfgang Imhof
Keyword(s):  
Triple Bond ◽  
Spectroscopic Data ◽  
Multiple Bond ◽  
Addition Reactions ◽  
X Ray ◽  
Higher Temperature ◽  
New Compounds ◽  
Selective Addition ◽  
C Nmr ◽  
Membered Heterocyclic Compound

The reaction of bifunctional neutral phosphenium ion complexes, containing a carbon-carbon triple bond next to a phosphorus-molybdenum multiple bond, with carbenes and to carbene isolobal organometallic fragments is discussed.So, the reaction of (R)(PhC=C)P=MoCp′(CO), (R = 2,4,6-′Bu3C6H2O; Cp′ = η5-C5H5: la; Cp′ = η5-C5Me5: 1b) with CH2,Ν2 (2) yields the three membered heterocyclic compound (3). 3 reacts with Co2(CO)8 to afford complex (5) in which the phenylethynyl building block is η2-side-on coordinated to a Co2(CO)6 fragment. Similar to the reaction of 1 with 2, 1 forms with Fe2(CO)9 (6), compound (7). In 7 the PMo double bond is coordinated in a η2 fashion to the 16-electron organometallic fragment Fe(CO)4. Using an excess of 6 and a higher temperature, the phosphorus-alkynyl-carbon σ-bond is cleaved, and cluster MoCp*Fe3(CO)8η3-PR)(C≡CPh) (8) is formed.The reaction of 1 with Cr(CO)5(THF) yields 10, a complex, in which the PhC≡C ligand is η2-coordinated to Cp′(CO)2Mo, and the Cr(CO)5 group forms a dative bond with the phosphorus atom.All new compounds have been characterized by analytical as well as by spectroscopic data (IR, 1H, 31P, 13C NMR, MS), compound 10 by an X-ray analysis.

Pd(II) and Pt(II) Complexes of 1,2-Bis(pyridin-2-yl)ethane-N,N'

1994 ◽  
Vol 49 (6) ◽  
pp. 844-848 ◽  
Author(s):  
A. McFarlane ◽  
J. R. Lusty ◽  
J. J. Fiol ◽  
A. Terrón ◽  
E. Molins ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Spectroscopic Data ◽  
Low Energy ◽  
X Ray ◽  
H Nmr ◽  
Direct Bond ◽  
Structures And Properties ◽  
C Nmr

X-ray crystal structures and properties of the two Pd(II) and Pt(II) complexes [bpeH2][PdCl4] and [Pt(bpe)Cl2], [bpe = 1,2-bis(pyridin-2-yl)ethane] are described and correlated with the IR and 1H NMR/13C NMR spectroscopic data. In the case of the Pt(II) complex, the 1,2-bis(pyridin-2-yl)ethane is bound to the metal by the heterocycle nitrogen atoms but no direct bond is found in the case of the Pd(II) complex. The ligand exhibits low energy geometries in both compounds: the cis-conformation in the Pt(II) complex, and the transconformation in the Pd(II) complex

scholarly journals Polymerization of Propene with Modified Constrained Geometry Complexes. Double-Bond Isomerization in Pendant Alkenyl Groups Attached to Cyclopentadienyl Ligands

2003 ◽  
Vol 68 (6) ◽  
pp. 1119-1130 ◽  
Author(s):  
Oetze K. B. Staal ◽  
Dirk J. Beetstra ◽  
Andries P. Jekel ◽  
Bart Hessen ◽  
Jan H. Teuben ◽  
...  
Keyword(s):  
Double Bond ◽  
Spectroscopic Data ◽  
Catalyst Activity ◽  
X Ray ◽  
X Ray Crystallography ◽  
Molecular Weights ◽  
Constrained Geometry ◽  
Internal Position ◽  
Moderate Effect ◽  
C Nmr

Polymerization of propene with dimethylsilylene-bridged (amidocyclopentadienyl)dichlorotitanium(IV) complexes [TiCl2{η5-1-(t-BuSiMe2N-κN)-2,3,4-Me3-5-R-C5}], where R = Me (1), H (2), Ph (3), 4-fluorophenyl (4), but-2-en-2-yl (5), and butyl (6), combined with excess methylaluminoxane revealed a moderate effect of the substituent R on the catalyst activity and the molecular weight of polypropene. The asymmetric substitution in the position adjacent to the bridging carbon atom resulted in polymer yields decreasing in the order 1 > 6 > 3 ≈ 5 > 4 > 2 while polymers with the molecular weights (Mw) close to 2.5 × 105 for 1, 3, and 4, 1.5 × 105 for 5 and 6, and 7.5 × 104 for 2 were obtained. The 13C NMR analysis of the polymers has shown that atactic polypropene is slightly enriched with syndiotactic triads for all the catalysts. Investigation of the crystal structure of 5 by X-ray crystallography revealed that the double bond in but-3-en-2-yl had shifted to an internal position to give the isomeric, but-2-en-2-yl-substituted complex. Likewise, the spectroscopic data for complex 7 prepared from the ligand containing but-3-en-1-yl substituent, indicate the absence of terminal double bond.

Azide und Cyanamide – ähnlich und doch anders/Azides and Cyanamides – Similar and Yet Different

2003 ◽  
Vol 58 (11) ◽  
pp. 1097-1104 ◽  
Author(s):  
Olaf Reckeweg ◽  
Arndt Simon
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystals ◽  
Crystal Structures ◽  
Spectroscopic Data ◽  
Structural Features ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Time ◽  
Raman And Ir Spectroscopy

Abstract The crystal structures of LiN3*H2O (P63/mcm (No. 193), Z = 6; 924.01(13); 560.06(7) pm); NH4N3 (Pmna (No. 53), Z =4; a=889.78(18), b=380,67(8), c=867.35(17) pm); Ca(N3)2 (Fddd (No. 70), Z = 8; a=595.4(2), b=1103.6(5), c=1133.1(6) pm), Sr(N3)2 (Fddd (No. 70), Z =8; a= 612.02(9), b = 1154.60(18), c = 1182.62(15) pm); Ba(N3)2 (P21/m (No. 11), Z = 2; a = 544.8(1), b = 439.9(1), c = 961.3(2) pm, β = 99.64(3)°) and TlN3 (I4/mcm (No. 140), Z = 2; 618.96(9); 732.71(15) pm) have been either determined for the first time or redetermined by X-ray diffraction on single crystals. The afore mentioned compounds, AN3 (A = Na, K, Rb, Cs), M(N3)2 · 2.5 H2O (M = Mg, Zn) and the cyanamides Li2CN2, CdCN2 and CuCN2 were investigated by Raman and IR spectroscopy (KBr technique). Structural features and spectroscopic data of azides and cyanamides from this work and from literature are listed and compared.

scholarly journals Guaiol - A Naturally Occurring Insecticidal Sesquiterpene

2013 ◽  
Vol 8 (10) ◽  
pp. 1934578X1300801 ◽  
Author(s):  
Tao Liu ◽  
Chun-Juan Wang ◽  
Hui-Qin Xie ◽  
Qing Mu
Keyword(s):  
Musca Domestica ◽  
Plutella Xylostella ◽  
Spectroscopic Data ◽  
Significant Inhibition ◽  
X Ray ◽  
Naturally Occurring ◽  
Mythimna Separate ◽  
Good Contact ◽  
Main Component ◽  
C Nmr

The dichloromethane fraction of Ferula ferulaeoides was analyzed by GC and GC-MS, and thirty-four compounds were identified. The main component in the fraction, guaiol (37.0%) was separated by chromatographic methods and identified from spectroscopic data, including 1H and 13C NMR, and X-ray crystallographic diffraction. Guaiol showed significant inhibition of aphids at a concentration of 70 mg/L. It also showed good contact activities against the 4th instar larvae of Mythimna separate and 3rd instar larvae of Plutella xylostella, with LD50 values of 0.07 and 8.9 mg/larva, as well as fumigation activity against the 4th instar larvae of M. separata and adult Musca domestica, with LC50 values of 3.5 μL/L and 16.9 μL/L, respectively.

scholarly journals Preparation of anthracene-based tetraperimidine hexafluorophosphate and selective recognition of chromium(III) ions

2019 ◽  
Vol 15 ◽  
pp. 2847-2855
Author(s):  
Qing-Xiang Liu ◽  
Feng Yang ◽  
Zhi-Xiang Zhao ◽  
Shao-Cong Yu ◽  
Yue Ding
Keyword(s):  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Selective Recognition ◽  
Addition Compound ◽  
X Ray ◽  
H Nmr ◽  
C Nmr

A novel anthracene-based tetraperimidine hexafluorophosphate 3 was prepared, and its structure was determined through X-ray analysis, HRMS as well as 1H and 13C NMR spectroscopy. In the cationic moiety of 3, two (N-ethylperimidinyl–C2H4)2NCH2– arms were attached to the 9- and 10-positions of anthracene. In addition, compound 3 was used as a chemosensor to research the ability to recognize Cr3+ through fluorescence and UV titrations, HRMS, as well as 1H NMR and IR spectroscopy. The results indicate that 3 is an effective chemosensor for Cr3+.

Synthese, Struktur und Reaktivität von 2-Amino- und 2-Imino-2,3-dihydro-1H-1,3,2-diazaborolen / Synthesis, Structure and Reactivity of 2-Amino- and 2-Imino-2,3-dihydro-1H-1,3,2-diazaboroles

1999 ◽  
Vol 54 (3) ◽  
pp. 363-371 ◽  
Author(s):  
Lothar Weber ◽  
Eckhard Dobbert ◽  
Andreas Rausch ◽  
Hans-Georg Stammler ◽  
Beate Neumann
Keyword(s):  
Diffraction Analysis ◽  
Spectroscopic Data ◽  
Ethylene Diamine ◽  
Gaseous Ammonia ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

The 2-halo-2,3-dihydro-1H-1,3,2-diazaboroles (1a′: R = tBu, X = Br; 1b: R = 2,6-Me2C6H3; X = I) were converted into the 2-amino-2,3-dihydro-1H-1,3,2- diazaboroles (2a: R = tBu; 2b: 2,6-Me2C6H3) by treatment with dry gaseous ammonia. Similarly reaction of 1a′ with 2,6-dimethylaniline or tBuNH2 afforded the corresponding derivates (3; R1 = 2,6-Me2C6H3; 4; R1 = tBu). The treatment of 1a′ with the ethylene diamine adduct of lithium acetylide led to the formation of (5). Lithiation of 2 a and subsequent silylation gave 6 (R1 = SiMe3), which was transformed to the diborolylamine (7) upon exposure to 1a′. Borolylketimine (8 ) and borolylcarbodiimide (9) resulted from 1a′ and Ph2C=NSiMe3 or Me3SiN=C=NSiMe3, respectively. All the new compounds were characterized by elemental analyses as well as spectroscopic data (IR, 1H, 11B, 13C NMR, MS). Heterocycle 5 was also subjected to an X-ray diffraction analysis.

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