Novel binuclear doubly vinyl-bridged iridium complexes formed by olefinic C—H activation

1995 ◽  
Vol 73 (7) ◽  
pp. 1050-1057 ◽  
Author(s):  
Helmut Werner ◽  
Justin Wolf ◽  
Angelika Nessel ◽  
Arno Fries ◽  
Bernd Stempfle ◽  
...  
Keyword(s):  
Structure Analysis ◽  
Binuclear Complex ◽  
Iridium Complexes ◽  
Heterometallic Complex ◽  
Metal Compounds ◽  
X Ray ◽  
Compound C

Treatment of [C5H5IrX2]n (2: X = Cl; 3: X = Br) with CH2=CHtBu in the presence of Na2CO3–iPrOH gives, besides the bis(olefin) complex [C5H5Ir(CH2=CHtBu)2] (4), the doubly vinyl-bridged iridium(II) compound {[C5H5Ir(μ-η1,η2-CH=CHtBu)]2} (5). The related binuclear complex {[CH2(C5H4)2][Ir2(μ-η1,η2-CH=CHtBu)2]} (9) was obtained from {[CH2(C5H4)2][IrBr2]2}n (8) and CH2=CHtBu–Na2CO3 in ethanol and characterized by an X-ray structure analysis (monoclinic, C2/c (No. 15), a = 20.050(8), b = 8.843(1), c = 24.25(1) Å, β = 99.53(2)°, V = 4241 Å3, Z = 8, R = 0.032, Rw = 0.041). Protonation of both 5 and 9 with HBF4•OEt2 yields the BF4 salts of the unsymmetrical hydridometal cations 10 and 11 in which the vinyl bridges are still intact. The reaction of the binuclear bis(cyclooctene)metal compounds {[CH2(C5H4)2][Rh(C8H14)2]2} (14) and {[CH2(C5H4)2][Rh(C8H14)2][Ir(C8H14)2]} (17) with bromine yields almost quantitatively the polymeric (or oligomeric) dibromo derivatives 16 and 18, which could, however, not be converted to vinyl bridged complexes by treatment with CH2=CHtBu–Na2CO3–ROH. Keywords: iridium complexes, C-H activation, bridging vinyl ligands, cationic hydridometal complexes, heterometallic complex.

4-(Bromomethyl)benzophenone

2007 ◽  
Vol 63 (3) ◽  
pp. o1188-o1189 ◽  
Author(s):  
Wei-Jian Xu ◽  
Yang-Ling Zang ◽  
Guo-Liang Wu ◽  
Sheng-Pei Su ◽  
De-Yue Qiu
Keyword(s):  
Crystal Structure ◽  
Carbon Tetrachloride ◽  
Dihedral Angle ◽  
Structure Analysis ◽  
Title Compound ◽  
Crystal Packing ◽  
Crystal Structure Analysis ◽  
X Ray ◽  
Compound C ◽  
Phenyl Rings

The title compound, C14H11BrO, was synthesized by the reaction of 4-methylbenzophenone and bromine in carbon tetrachloride. X-ray crystal structure analysis reveals that the benzene and phenyl rings form a dihedral angle of 59.53 (6)°, and the crystal packing is stabilized by intermolecular C—H...π interactions.

Boron Chelates and Boron-Metal Chelates, X [1]. 3-(2-Hydroxyphenyl)-2,2-diphenyl-1-oxa-3-azonia-2-borata-naphthalene-methanol (1/1): Synthesis, Spectroscopic Investigations and Crystal Structure

1982 ◽  
Vol 37 (11) ◽  
pp. 1450-1455 ◽  
Author(s):  
Rudolf Allmann ◽  
Eberhard Hohaus ◽  
Stanislaw Olejnik
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Analysis ◽  
Title Compound ◽  
Chelate Ring ◽  
Boron Chelates ◽  
X Ray ◽  
Membered Chelate Ring ◽  
Compound C ◽  
Overall Ratio

The title compound, C25H20BNO2 · CH3OH, was examined by UV, IR, 1H, and 13C NMK spectroscopy as well as by thermogravimetry and X-ray structure analysis (Pbnb, a = 8.815, b = 17.309, c=28.992 Å, R= 5.5%). These investigations show the six-membered chelate ring (chelate A) to exist as formulated in [2] and not as a five-membered chelate ring B. One methanol molecule connects two chelate molecules by hydrogen bonds, resulting in an overall ratio of chelate to methanol of 1 : 1.

(1aR,2aS,5aS,5bS)-Perhydro-4H-oxireno[3,4]cyclopenta[1,2-b]furan-4-one

2007 ◽  
Vol 63 (3) ◽  
pp. o1359-o1360
Author(s):  
Christian Peifer ◽  
Melanie Tschertsche ◽  
Dieter Schollmeyer ◽  
Stefan Laufer
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Title Compound ◽  
Crystal Structure Analysis ◽  
Epoxide Group ◽  
X Ray ◽  
Compound C ◽  
Lactone Group

The structure of the title compound, C7H8O3, was determined in the course of our studies of the synthesis of cyclopenta[1,2-b]furan-4-one derivatives. The molecule has four chiral C atoms. The X-ray crystal structure analysis shows the compound to possess an epoxide group with an endo orientation with respect to the lactone group.

scholarly journals 7-Isopropylidene-N2,N3,N5,N6-tetramethoxy-N2,N3,N5,N6-tetramethylbicyclo[2.2.1]hepta-2,5-diene-2,3,5,6-tetracarboxamide

2014 ◽  
Vol 70 (4) ◽  
pp. o438-o438
Author(s):  
Benjamin Sahlmann ◽  
Christian Näther ◽  
Rainer Herges
Keyword(s):  
Molecular Structure ◽  
Structure Analysis ◽  
Title Compound ◽  
Methyl Groups ◽  
X Ray ◽  
Compound C ◽  
Methoxy Groups

Although the molecular structure of the title compound, C22H32N4O8, displays a twofold symmetry of the molecule including the methoxy and methyl substituents, no crystallographic twofold symmetry is observed in the X-ray structure analysis. The carbonyl O atoms alternately point to different sides of the plane defined by the carbonyl C atoms. Two methoxy groups are oriented inside the molecules cavity. The H atoms of two methyl groups are disordered over two orientations and were refined using a split model.

Tetraphenylarsonium diisothiocyanatodibromonickelate(II)

2006 ◽  
Vol 62 (5) ◽  
pp. m1014-m1015
Author(s):  
S. S. Singh ◽  
R. S. Prasad ◽  
Shailesh Upreti ◽  
N. K. Jha ◽  
A. Ramanan
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Title Compound ◽  
Crystal Structure Analysis ◽  
Mixed Ligand ◽  
Asymmetric Unit ◽  
X Ray ◽  
Twofold Axis ◽  
Compound C

Use of mixed-ligand (bromide and thiocyanate ions) coordination with nickel has led to the crystallization of the title compound, (C24H20As)2[Ni(NCS)2Br2]. X-ray crystal structure analysis reveals that the asymmetric unit contains one (C6H5)4As+ cation and one half [Ni(NCS)2Br2]2− anion, the latter lying on a crystallographic twofold axis.

Absolute Stereochemistry of (-)-Wieland-Miescher Ketone as Established by the X-ray Crystallographic and CD Exciton Chirality Methods

1992 ◽  
Vol 57 (7) ◽  
pp. 1459-1465 ◽  
Author(s):  
Nobuyuki Harada ◽  
Tatsuo Sugioka ◽  
Hisashi Uda ◽  
Takeo Kuriki
Keyword(s):  
Structure Analysis ◽  
Absolute Configuration ◽  
X Ray ◽  
The Absolute ◽  
Absolute Stereochemistry

The 8aR absolute stereochemistry of Wieland-Miescher ketone (-)-I was established by the X-ray structure analysis of its bis(4-bromobenzoate) derivatives (1R,6R,8aR)-(+)-IV and (1R,6S,8aR)-(-)-V. The absolute configuration of (-)-I was corroborated further by the application of the CD exciton chirality method to bis(4-bromobenzoates) (+)-IV and (-)-V.

Diphosphinoazine Rhodium(I) and Iridium(I) Complexes

2006 ◽  
Vol 71 (2) ◽  
pp. 197-206 ◽  
Author(s):  
Martin Pošta ◽  
Jan Čermák ◽  
Pavel Vojtíšek ◽  
Ivana Císařová
Keyword(s):  
Rhodium Complexes ◽  
Iridium Complexes ◽  
X Ray ◽  
First Time

The first rhodium complexes of diphosphinoazines [{RhCl(1,2-η:5,6-η-CH=CHCH2CH2CH=CHCH2CH2)}2 {μ-R2PCH2C(But)=NN=C(But)CH2PR2] (R = Ph, Cy, Pri) were prepared by cleavage of the bridge in chloro(cycloocta-1,5-diene)rhodium(I) dimer, the analogous iridium(I) complexes were also prepared for the first time. The X-ray structures of isostructural rhodium and iridium complexes with bis(dicyclohexylphosphino)pinacoloneazine were determined. Diphosphinoazine ligands in the complexes remained in (Z,Z) configuration bridging two RhCl(C8H12) units.

scholarly journals Preparative-scale HPLC Resolution of Metallacyclic η3-Allyltricarbonyliron Complexes and Determination of the Absolute Configuration by X-Ray Crystal Structure Analysis

1999 ◽  
Vol 23 (9) ◽  
pp. 578-579
Author(s):  
Rainer Schobert ◽  
Hermann Pfab ◽  
Jutta Böhmer ◽  
Frank Hampel ◽  
Andreas Werner
Keyword(s):  
Crystal Structure ◽  
Silica Gel ◽  
Structure Analysis ◽  
Absolute Configuration ◽  
Crystal Structure Analysis ◽  
Preparative Scale ◽  
X Ray ◽  
The Absolute

Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.

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