Facile Synthesis of Pentamethylcyclopentadienyl Ruthenium Half-Sandwich Complexes by Naphthalene Displacement

2018 ◽  
Vol 71 (4) ◽  
pp. 289 ◽  
Author(s):  
Jeremy Stone ◽  
David Jago ◽  
Alexandre Sobolev ◽  
Mark Spackman ◽  
George Koutsantonis
Keyword(s):  
Single Crystal ◽  
Organometallic Chemistry ◽  
Synthetic Methods ◽  
Sandwich Complexes ◽  
Facile Synthesis ◽  
X Ray ◽  
Wide Range ◽  
Structure Determinations ◽  
Half Sandwich

Ruthenium half-sandwich complexes are central in a wide range of diverse applications in the field of organometallic chemistry. As such, exploration of their preparation and reactivity is crucial for development of their chemistry. Herein, we present alternative synthetic methods for the preparation of Cp*Ru(dppm)Cl, Cp*Ru(dppe)Cl, Cp*Ru(dppf)Cl, [Cp*Ru(COD)(MeCN)]BF4, and [Cp*Ru(bpy)(MeCN)]BF4 (dppm = 1,2-bis(diphenylphosphino)methane; dppe = 1,2-bis(diphenylphosphino) ethane; dppf = 1,2-bis(diphenylphosphino)ferrocene; COD = 1,5-cyclooctadiene; bpy= 2,2′-bipyridine), starting from the easily accessible [Cp*Ru(η6-C10H8)]BF4. The single-crystal X-ray structure determinations for [Cp*Ru(COD)(MeCN)]BF4, and [Cp*Ru(bpy)(MeCN)]BF4 are also presented.

Comparative Structural Studies on Three-Coordinate Copper(I) Halide Complexes With Tertiary Phosphines. Crystal Structures of [(PPh2Mes)CuX]2 and [(PPhMes2)CuX]2 (Mes = Mesityl X = Cl, Br, I)

1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Atom ◽  
Structural Studies ◽  
Coordination Environment ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Structure Determinations ◽  
Halide Complexes ◽  
The Subject

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.

Approaches to the Synthesis of Lincosamine, a Derived Portion of the Antibiotic Lincomycin

1990 ◽  
Vol 43 (10) ◽  
pp. 1657 ◽  
Author(s):  
LM Engelhardt ◽  
BW Skelton ◽  
RV Stick ◽  
DMG Tilbrook ◽  
AH White
Keyword(s):  
Nitrogen Atom ◽  
Single Crystal ◽  
Structure Elucidation ◽  
X Ray ◽  
Structure Determinations

A variety of approaches towards the synthesis of lincosamine, a derived portion of the antibiotic lincomycin , are reported. Initial approaches involved the intramolecular delivery of a nitrogen atom ( trichloroacetimidate , trichloroacetylcarbamate , carbamate, 2-amino-2- phenylacetate ) attached to O4 onto C6 of a 6,7-anhydrooctoside. Later approaches, albeit more direct but again largely unsuccessful, involved the Sharpless titanium(IV)-mediated nucleophilic opening of a suitable 6,7-anhydrooctose, and the Sharpless oxyamination and the aziridination of suitable octenoses . As an aid to the structure elucidation of several compounds encountered in this work, single-crystal X-ray structure determinations are reported for methyl 6,7-anhydro-2,3-di-O-benzyl-8-deoxy-α-D-threo-D-galacto-octopyranoside , methyl 6,7-anhydro-2,3-di-O-benzyl-8-deoxy-α-D-threo-D-gluco-octopyranoside and 7-azido-7-deoxy-1,2:3,4-di-O-isopropylidene-β-L-erythro-Dgalacto-octose.

Catalyst-Free Synthesis of Diastereomerically Pure 3-Sulfonyl­azetidin-2-ones via Microwave-Assisted Tandem Wolff Rearrangement–Staudinger Cycloaddition

Synthesis ◽  
2020 ◽  
Author(s):  
Mikhail Krasavin ◽  
Judith Synofzik ◽  
Olga Bakulina ◽  
Olga Balabas ◽  
Dmitry Dar’in
Keyword(s):  
Drug Design ◽  
Single Crystal ◽  
Wolff Rearrangement ◽  
X Ray ◽  
Design And Optimization ◽  
X Ray Crystallography ◽  
Microwave Assisted ◽  
Catalyst Free ◽  
Relative Stereochemistry ◽  
Wide Range

A wide range of α-diazo-β-ketosulfones have been applied to thermally promoted tandem Wolff rearrangement – Staudinger [2+2] cycloaddition with imines to give polysubstituted β-lactam sulfones. Dia­stereomerically pure syn-diastereomers were obtained in good yields and the relative stereochemistry was confirmed by single-crystal X-ray crystallography. These findings significantly expand the scope of this transformation, in contrast to substantial limitations reported previously. Moreover, this methodology enables flexible exploration of new substitution patterns around the privileged β-lactam core for drug design and optimization.

Notizen: Einkristall-Strukturdaten einiger Fluoride und Cyanide A2IBIMIIIX6 der Elpasolithfamilie / Single Crystal Structural Data of Some Fluorides and Cyanides A2IBIMIIIX6 of the Elpasolite Family

1975 ◽  
Vol 30 (5-6) ◽  
pp. 462-464 ◽  
Author(s):  
R. Haegele ◽  
W. Verscharen ◽  
D. Babel
Keyword(s):  
Single Crystal ◽  
Structural Data ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Structure Determinations ◽  
Crystal Structural Data ◽  
Crystal Structural

The parameters of complete X-ray structure determinations are given for the fluoridesRb2NaFeF6 and Rb2KFeF6 (cubic), Cs2NaCrF6 and Cs2NaFeF6 (hexagonal-rhom-bohedral) and Cs2LiGaF6 (hexagonal). Space group and lattice constants of the monoclinic cyanides Cs2BFe(CN)6 (B = Na, K, Rb) are reported as well.

On the Reaction of ortho-Diphenoquinone Valence Isomers with Primary and Secondary Amines. X-Ray Structure Analysis of a 2,3-Dihydro-1H-azepinone and its Photochemical and Oxidative Conversion Products

1979 ◽  
Vol 32 (9) ◽  
pp. 1931 ◽  
Author(s):  
H Becker ◽  
K Gustafsson ◽  
CL Raston ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Secondary Amines ◽  
Reaction Products ◽  
Oxidative Conversion ◽  
X Ray Diffraction ◽  
X Ray ◽  
Primary And Secondary Amines ◽  
Diffraction Structure ◽  
Structure Determinations ◽  
Photochemical Isomerization

Single-crystal X-ray diffraction structure determinations are reported for three reaction products and photoisomers formed from reactions between an o-diphenoquinone valence isomer and primary and secondary amines, namely: 3,5-di-t-butyl-7-(3,5-di-t-butyl-2-hydroxyphenyl)-1-methyl-2,3-dihydro-1H-azepin-2-one (8; R1 = R2 = But, R3 = Me), its photochemical isomerization product 4,6-di-t-butyl-1-(3,5-di-t-butyl-2-hydroxyphenyl)-2-methyl-2-azabicyclo[3,2,0]hept-6-en-3-one (9; R1 = R2 = But, R3 = Me) and 4',5,7-tri-t-butyl-3'-(2,2-dimethylpropionyl)-1'-methylspiro[benzofuran-3(2H)-2'- pyrrolidinel-2,5'-dione (12; R1 = R2 = But, R3 = Me).

scholarly journals Applications with a brighter X-ray source and new detectors from Agilent

2014 ◽  
Vol 70 (a1) ◽  
pp. C1734-C1734
Author(s):  
Zoltan Gal ◽  
Tadeusz Skarzynski ◽  
Fraser White ◽  
Oliver Presly ◽  
Adrian Jones ◽  
...  
Keyword(s):  
Data Quality ◽  
Single Crystal ◽  
Measurement System ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Vacuum Technology ◽  
Intelligent Measurement ◽  
Wide Range

Agilent Technologies develop and supply X-ray systems for single-crystal diffraction research, including the SuperNova; a compact, highly reliable and very low maintenance instrument providing X-ray data of the highest quality; and the PX Scanner for testing and characterization of protein crystals in their original crystallization drops (in-situ). The SuperNova and PX Scanner are constantly improving, with recent enhancements including a new range of detectors using an Intelligent Measurement System. The Eos S2, Atlas S2 and Titan S2 detector range employs a smart sensitivity control of the electronic gain and is capable of instantaneously switching its binning modes thus providing unprecedented flexibility in tuning every exposure to provide the highest data quality for a wide range of experiments. We have also developed a completely new micro-focus X-ray source based on Gradient Vacuum technology, with novel filament and target designs. This novel source is an integral part of the new Agilent GV1000 X-ray diffractometer, which has been designed for applications that require even higher brightness of the X-ray beam.

The Conformation of Some 1,6-Disulfide-Bridged D-Hexopyranoses

2005 ◽  
Vol 58 (3) ◽  
pp. 199 ◽  
Author(s):  
Ethan D. Goddard-Borger ◽  
Brian W. Skelton ◽  
Robert V. Stick ◽  
Allan H. White
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Similar Investigation ◽  
X Ray ◽  
X Ray Crystallography ◽  
Structure Determinations ◽  
Derivatives Of

The use of 1H NMR spectroscopy, in tandem with X-ray crystallography, has cast light on the conformation of the 1,6-disulfide-bridged derivatives of d-gluco-, d-manno-, d-allo-, d-galacto-, and d-talo-pyranose. A similar investigation was performed on the thiosulfinate derived from the d-gluco disulfide. Single-crystal X-ray structure determinations are reported for (1S,5S,6S,7S,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, (1S,5S,6S,7R,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, and (1S,2S,5S,6S,7S,8R)-6,7,8-triacetoxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane 2-oxide.

Crystal structures of some eriostyl/nitrobenzoate derivatives

1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.

Sign in / Sign up

Export Citation Format

Share Document