NCO-Chelated organoantimony(III) and organobismuth(III) dichlorides: Syntheses and structures

2010 ◽  
Vol 75 (10) ◽  
pp. 1041-1050 ◽  
Author(s):  
Jan Vrána ◽  
Roman Jambor ◽  
Aleš Růžička ◽  
Jaroslav Holeček ◽  
Libor Dostál
Keyword(s):  
Solid State ◽  
Good Yield ◽  
Solution Nmr ◽  
Molar Ratio ◽  
Organolithium Compound ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chelating Ligand

The novel NCO chelating ligand L, 1-CH2N(CH3)2-3-CH2OCH3-C6H4, was prepared in four steps from commercially available m-tolunitrile in a good yield. Successful lithiation of this ligand was achieved by the reaction with n-BuLi in hexane. Using of this in situ prepared organolithium compound LLi in the reactions with MCl3 (M = Sb, Bi) in 1:1 molar ratio led to isolation of the desired mono-organocompounds MLCl2 (M = Sb (1), Bi (2)). Their structures were studied both in solution (NMR) and in the solid state (X-ray diffraction), and were compared with those of the NCN- and OCO-chelating analogues.

scholarly journals Formation and structure of the first metal complexes comprising amidinoguanidinate ligands

2016 ◽  
Vol 72 (11) ◽  
pp. 1526-1531 ◽  
Author(s):  
Farid M. Sroor ◽  
Phil Liebing ◽  
Cristian G. Hrib ◽  
Daniel Gräsing ◽  
Liane Hilfert ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Metal Complexes ◽  
Solid State Reaction ◽  
The Novel ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray

The first metal complexes comprising amidinoguanidinate ligands have been prepared and structurally characterized, namely bis[μ-N,N′,N′′,N′′′-tetraisopropyl-1-(1-butylamidinato)guanidinato-κ3N1,N2:N2]bis[(tetrahydrofuran)lithium], [Li2(C18H37N4)2(C4H8O)2], (2), and [bis(tetrahydrofuran)lithium]-di-μ-chlorido-{(N,N′-dicyclohexyl-1-butylamidinato-κ2N1,N2)[N,N′,N′′,N′′′-tetracyclohexyl-1-(1-butylamidinato)guanidinato-κ2N1,N2]holmate(III)}, [HoLiCl2(C4H8O)2(C17H31N2)(C30H53N4)], (3). The novel lithium amidinoguanidinate precursors Li[nBuC(=NR)(NR)C(NR)2] [1:R= Cy (cyclohexyl),2:R=iPr) were obtained by treatment ofN,N′-diorganocarbodiimides,R—N=C=N—R(R=iPr, Cy), with 0.5 equivalents ofn-butyllithium under well-defined reaction conditions. An X-ray diffraction study of2revealed a ladder-type dimeric structure in the solid state. Reaction of anhydrous holmium(III) chloride within situ-prepared2afforded the unexpected holmium `ate' complex [nBuC(=NCy)(NCy)C(NCy)2]Ho[nBuC(NCy)2](μ-Cl)2Li(THF)2(3) in 71% yield. An X-ray crystal structure determination of3showed that this complex contains both an amidinate ligand and the new amidinoguanidinate ligand.

On the Solid-State Isomerization of Terpinolene Tetrabromide

2010 ◽  
Vol 63 (3) ◽  
pp. 458
Author(s):  
Paul V. Bernhardt ◽  
Raymond M. Carman ◽  
Tri T. Le
Keyword(s):  
Solid State ◽  
Solid State Reaction ◽  
Bulk Material ◽  
Solution Nmr ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
Compound A ◽  
X Ray

The isomerization of terpinolene tetrabromide from the cis-2,4- (diaxial) dibromo isomer (A) to the more stable trans-2,4- (equatorial–axial) compound (B) has been investigated in the solid state. The progress of the solid-state reaction as a function of time was followed by solution NMR analysis, and, more effectively, by micropowder X-ray diffraction of the bulk material in situ. Characterization of the solid-state reaction mixture is facilitated by the existence of X-ray crystal structures of both compounds A (monoclinic) and B (reported previously) in addition to a new triclinic polymorph of compound A reported herein, all three forms being observed by powder X-ray diffraction.

Synthesen und Kristallstrukturen von Bis(N-lithiumtrimethylsilylamino)- bis(dimethylamino)silan und 1,1-Dichloro-2,4-bis(trimethylsilylamino)- 3,3-bis(dimethylamino)siladiazatitanacyclobutan / Syntheses and Crystal Structures of Bis(N-lithio-trimethylsilylamino)bis(dimethylamino)- silane and 1,1-Dichloro-2,4-bis(trimethylsilylamino)-3,3-bis(dimethylamino)siladiazatitanacyclobutane

2002 ◽  
Vol 57 (9) ◽  
pp. 976-982
Author(s):  
Josef Engering ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Titanium Tetrachloride ◽  
Solution Nmr ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Nmr Spectroscopy

Bis(N-lithio-trimethylsilylamino)bis(dimethylamino)silane (1) is formed in the reaction of silicon tetrachloride with excess hexamethyldisilazane, followed by halogen substitution using two equivalents of LiN(CH3)2, and treatment with two equivalents of n-butyllithium in hexane. 1, found to be dimeric in the solid state, was characterised by single crystal X-ray diffraction (monoclinic, C2/c, a = 1925.2(4), b = 1501.7(2), c = 1389.7(3) pm, β= 101.98(2), Z = 4, C20H60Li4N8Si6), and by solid state and solution NMR spectroscopy and mass spectrometry. Further reaction with titanium tetrachloride (molar ratio 1:1) yields orange crystals of the dimer [TiClf(μ2-NSi(CH3)3)2Si(N(CH3)2)μ2-Cl]2 (2) characterised by single crystal X-ray diffraction (triclinic, P1, a = 942.1(4), b = 991.7(4), c = 1222.6(5) pm, α= 90.12(1), β= 94.42(2), γ= 107.64(1)°, Z = 1, C20H60Cl4N8Si6Ti2)

Solid state synthesis of LiFePO4 studied by in situ high energy X-ray diffraction

2011 ◽  
Vol 21 (15) ◽  
pp. 5604 ◽  
Author(s):  
Zonghai Chen ◽  
Yang Ren ◽  
Yan Qin ◽  
Huiming Wu ◽  
Shengqian Ma ◽  
...  
Keyword(s):  
Solid State ◽  
High Energy ◽  
Solid State Synthesis ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer
Keyword(s):  
Diffraction Analysis ◽  
Room Temperature ◽  
31P Nmr ◽  
Spectroscopic Studies ◽  
Iron Complex ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phosphenium Ions

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.

scholarly journals In situ X-ray diffraction computed tomography studies examining the thermal and chemical stabilities of working Ba0.5Sr0.5Co0.8Fe0.2O3−δ membranes during oxidative coupling of methane

2020 ◽  
Vol 22 (34) ◽  
pp. 18964-18975
Author(s):  
Dorota Matras ◽  
Antonis Vamvakeros ◽  
Simon D. M. Jacques ◽  
Vesna Middelkoop ◽  
Gavin Vaughan ◽  
...  
Keyword(s):  
Computed Tomography ◽  
Solid State ◽  
Oxidative Coupling ◽  
Structural Changes ◽  
Oxidative Coupling Of Methane ◽  
Membrane Reactors ◽  
Solid State Chemistry ◽  
X Ray Diffraction ◽  
X Ray

In situ XRD-CT and post-reaction SEM/EDX were used to study the solid-state chemistry and structural changes of Ba0.5Sr0.5Co0.8Fe0.2O3−δ membrane reactors during the oxidative coupling of methane reaction.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.

Tautomeric polymorphism of the neuroactive inhibitor kynurenic acid

2019 ◽  
Vol 75 (6) ◽  
pp. 793-805
Author(s):  
Dorota Pogoda ◽  
Jan Janczak ◽  
Sylwia Pawlak ◽  
Michael Zaworotko ◽  
Veneta Videnova-Adrabinska
Keyword(s):  
Solid State ◽  
Kynurenic Acid ◽  
Variable Temperature ◽  
Neurological Diseases ◽  
Crystal Form ◽  
Phase Behaviour ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

Kynurenic acid (KYN; systematic name: 4-hydroxyquinoline-2-carboxylic acid, C10H7NO3) displays a therapeutic effect in the treatment of some neurological diseases and is used as a broad-spectrum neuroprotective agent. However, it is understudied with respect to its solid-state chemistry and only one crystal form (α-KYN·H2O) has been reported up to now. Therefore, an attempt to synthesize alternative solid-state forms of KYN was undertaken and six new species were obtained: five solvates and one salt. One of them is a new polymorph, β-KYN·H2O, of the already known KYN monohydrate. All crystal species were further studied by single-crystal and powder X-ray diffraction, thermal and spectroscopic methods. In addition to the above methods, differential scanning calorimetry (DSC), in-situ variable-temperature powder X-ray diffraction and Raman microscopy were applied to characterize the phase behaviour of the new forms. All the compounds display a zwitterionic form of KYN and two different enol–keto tautomers are observed depending on the crystallization solvent used.

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