The First Aziridinylguanidinates: New Precursors for Potentially Volatile Metal Guanidinates

2014 ◽  
Vol 67 (7) ◽  
pp. 1110 ◽  
Author(s):  
Peter Tutacz ◽  
Ronny Syre ◽  
Cristian G. Hrib ◽  
Liane Hilfert ◽  
Nancy Frenzel ◽  
...  
Keyword(s):  
Solid State ◽  
Diethyl Ether ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray

The first lithium-aziridinylamidinates, Li[(C2H4N)C(NR)2]·THF (R = iPr (3), Cy (4); iPr = isopropyl, Cy = cyclohexyl), have been prepared by addition of N-aziridinyllithium, C2H4NLi (2), to either N,N′-diisopropylcarbodiimide or N,N′-dicyclohexylcarbodiimide. The cyclohexyl derivative 4 was crystallised from both diethyl ether (Et2O) and THF to afford the crystalline solvent adducts {Li[(C2H4N)C(NR)2]·S}2 (4: S = THF; 4a: S = Et2O) which were structurally characterised by X-ray diffraction. In the solid state, these lithium-aziridinylamidinates comprise ladder-type dimeric molecular structures.

Tetra(alkynyl)silanes, a 3,6-Disila-triyne, a 3,6,9-Trisila-tetrayne, a 1,3,4,6-Tetrasiladiyne, and Bis(trimethylstannyl)ethyne. Molecular Structures and Solid-state NMR Studies

2010 ◽  
Vol 65 (2) ◽  
pp. 119-127 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Ezzat Khan ◽  
Amin Badshah ◽  
Elias Molla ◽  
Peter Thoma ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Mas Nmr ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Solution State ◽  
Nmr Data

The molecular structures of three alkynylsilanes, tetrakis(ethynyl-p-tolyl)silane, 3,3,6,6,-tetramethyl- 3,6-disila-triyne, 3,3,6,6,9,9,-hexamethyl-3,6,9-trisila-tetrayne, and of bis(trimethylstannyl)- ethyne have been determined by X-ray diffraction. The same alkynylsilanes, and in addition 1,2- bis(trimethylsilylethynyl)-1,1,2,2-tetramethyldisliane, were studied by solid-state 13C and 29Si MAS NMR spectroscopy. The results of these measurements were compared with crystallographic evidence and also with relevant solution-state NMR data.

scholarly journals Transition metal complexes with pyrazole based ligands, part 27: Structural and thermal characterization of cobalt(II) halide and pseudohalide complexes with 4-acetyl-3-amino-5-methylpyrazole

2007 ◽  
Vol 72 (12) ◽  
pp. 1281-1293 ◽  
Author(s):  
Vukadin Leovac ◽  
Zoran Tomic ◽  
Katalin Mészáros-Szécsényi ◽  
Ljiljana Jovanovic ◽  
Milan Joksovic
Keyword(s):  
Thermal Decomposition ◽  
Solid State ◽  
Transition Metal Complexes ◽  
Thermal Characterization ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Vis Spectroscopy

The crystal and molecular structures of four tetrahedral structurally similar [Co(aamp)2X2] complexes (aamp = 4-acetyl-3-amino-5-methylpyrazole, X = Cl, Br, I and NCS) were determined by X-ray diffraction analysis and are discussed in detail. It was found that the different capacity of the ligand X (NCS vs. Cl, Br, I) for the formation of non-bonding contacts influence the mode of molecular association in the solid state. The complexes were characterized by UV-Vis spectroscopy. The first step of the thermal decomposition of the compounds was checked and is discussed in the view of the IR spectrum of the intermediate isolated from [Co(aamp)2Br2] by the quasi-isothermal technique.

Molecular structures of various alkyldichlorosilanes in the solid state

2017 ◽  
Vol 46 (27) ◽  
pp. 8875-8882
Author(s):  
Jörg Wagler ◽  
Robert Gericke
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray

A series of organodichlorosilanes RR′SiCl2 (R,R′ = (CH2)3; (CH2)4; (CH2)5; Me,Me; Me,H; Me,Cl) was studied by single-crystal X-ray diffraction analyses.

Synthesis and solid-state molecular structures of bis- and mono-nitrosobenzene complexes of ruthenium porphyrins

2002 ◽  
Vol 80 (9) ◽  
pp. 1252-1258 ◽  
Author(s):  
Jonghyuk Lee ◽  
Brendan Twamley ◽  
George B Richter-Addo
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Ir Spectra ◽  
Single Crystal ◽  
Binding Mode ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Parallel Arrangement ◽  
Ruthenium Porphyrin

Bis-nitrosobenzene complexes of the form (por)Ru(PhNO)2 (por = TPP, TTP; TPP = tetraphenylporphyrinato dianion, TTP = tetratolylporphyrinato dianion) have been prepared in good yields from the reaction of the (por)Ru(CO) precursor with excess PhNO in dichloromethane. The IR spectra of the complexes (as KBr pellets) displayed new bands at ~1348 cm–1, due to υNO. The solid-state molecular structure of (TPP)Ru(PhNO)2 was determined by single-crystal X-ray diffraction, and revealed that the PhNO ligands are bound to the Ru center via the N-binding mode. Reactions of the (por)Ru(PhNO)2 complexes with excess 1-methylimidazole gave the mono-nitrosobenzene complexes (por)Ru(PhNO)(1-MeIm). The IR spectra revealed a lowering of υNO in these mononitrosobenzene derivatives by ~27 cm–1, a feature consistent with the replacement of one π-acid PhNO ligand with the more basic 1-MeIm ligand. The solid-state molecular structure of (TPP)Ru(PhNO)(1-MeIm) reveals, in addition to the N-binding of the PhNO ligand, an essentially parallel arrangement of the C-N-O (of PhNO) and imidazole planes; this is in contrast with the (TPP)Ru(PhNO)2 complex, in which the C-N-O planes (of PhNO) are essentially perpendicular.Key words: nitroso, X-ray, ruthenium, porphyrin, imidazole.

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

Bromo-di(silyl)methanes - Precursors to Disilylcarbanionic Ligands

1995 ◽  
Vol 50 (5) ◽  
pp. 821-827 ◽  
Author(s):  
Sebastian Bommers ◽  
Holger Beruda ◽  
Martin Paul ◽  
Hubert Schmidbaur
Keyword(s):  
Single Crystal ◽  
Diethyl Ether ◽  
Molecular Structures ◽  
Triflic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Halogen Free

Abstract The reaction of the series of methyl/phenylchlorosilanes Me2PhSiCl, MePh2SiCl and Ph3SiCl with CHBr3/n-BuLi to give the corresponding bromo-di(silyl)methanes has been investigated. The selectivity of the reaction proved to be strongly influenced by the number of phenyl groups bound to silicon. As already established for Me3SiCl, Si-C coupling readily occurs with Me2PhSiCl to give (Me2PhSi)2CHBr (1) in good yields, whereas MePh2SiCl affords (MePh2Si)2CHBr (2) in lower yields. The molecular structures of 2 and the by-product (MePh2Si)2CBr2 have been determ ined by single crystal X-ray diffraction. In the case of the fully arylated species, Ph3SiCl, only the monosilylated compound (Ph-Si)CH2Br (3) is generated. (HMe2Si)2CHBr (5) can be obtained starting from 1 by treatment with triflic acid to give (CF3SO3Me2Si)2CHBr (4), followed by reduction of 4 with LiAlH4 in diethyl ether. In situ metalation of 5 with n-BuLi affords (HMe2)2CHLi, which reacts instantaneously with a second equivalent of 5 to give the halogen-free dimer [(HMe2Si)2CH]SiMe2CH2SiMe2H (6).

Arylimido zirconium and titanium complexes: characteristic structures and application in ethylene polymerization

2016 ◽  
Vol 71 (10) ◽  
pp. 1019-1023 ◽  
Author(s):  
Shifang Yuan ◽  
Lijing Wang ◽  
Yupeng Hua ◽  
Jing Zhang ◽  
Wen-Hua Sun
Keyword(s):  
Solid State ◽  
Ethylene Polymerization ◽  
Titanium Tetrachloride ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Zirconium Tetrachloride ◽  
Titanium Complexes ◽  
Titanium Complex ◽  
X Ray ◽  
Catalytic Activities

AbstractDimeric anilidolithium (ArHNLi·Et2O)2 (Ar=2,6-iPr2C6H3) reacted with zirconium tetrachloride in THF to give the heterometallic zirconium–lithium complex [(Et2O)2Li(μ-Cl)2(ArHN)(ArN=)Zr(μ-Cl)]2 (C1) and with titanium tetrachloride in toluene to give the titanium complex [(ArN=)TiCl2·(Et2O)2] (C2) each in good isolated yields. Their molecular structures in the solid state were confirmed by X-ray diffraction analysis. Upon activation with methylaluminoxane, both arylimido zirconium and titanium complexes exhibited good catalytic activities toward ethylene polymerization.

The synthesis and structural characterization of linear and macrocyclic bis(dinitrosyliron) complexes supported by bis(phosphine) bridging ligands

2003 ◽  
Vol 81 (6) ◽  
pp. 468-475 ◽  
Author(s):  
Lijuan Li ◽  
Nada Reginato ◽  
Michael Urschey ◽  
Mark Stradiotto ◽  
John D Liarakos
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Mononuclear Complex ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
X Ray ◽  
Phosphine Complexes

Reactions involving Fe(NO)2(CO)2 and the bis(phosphine) ligands bis(diphenylphosphino)methane (DPPM), bis(diphenylphosphino)acetylene (DPPA), 1,6-bis(diphenylphosphino)hexane (DPPH), and 1,4-bis(diphenyl phosphino)benzene (DPPB) have been examined. From these reactions, the mononuclear complex, Fe(κ1-DPPM)(NO)2(CO) 3, linear dinuclear species of the type Fe2(µ-L)(NO)4(CO)2 (L = Ph2PCH2PPh2 4, Ph2PC[Formula: see text]CPPh2 5, Ph2PCH2(CH3)4CH2PPh2 6, and Ph2P(p-C6H4)PPh2 7), and macrocyclic dinuclear species of the type Fe2(µ-L)2(NO)4 (L = Ph2PCH2PPh2 8 and Ph2PC[Formula: see text]CPPh2 9) were isolated and spectroscopically characterized. For 4, 5, 8, and 9, the solid-state molecular structures of the products were determined by use of single-crystal X-ray diffraction techniques. Key words: dinitrosyliron, iron nitrosyls, dinuclear macrocycles, bis(phosphine) complexes.

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