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.

Thermal enhancement of 2H11/2→4I15/2 up-conversion luminescence of Er3+ doped K2Yb(PO4)(MoO4) phosphors

2021 ◽  
Author(s):  
Hongqiang Cui ◽  
Yongze Cao ◽  
Lei Zhang ◽  
Yuhang Zhang ◽  
Siying Ran ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Reaction ◽  
Solid State Reaction Method ◽  
X Ray Diffraction ◽  
Orthorhombic Crystal ◽  
Orthorhombic Crystal Structure ◽  
Reaction Method ◽  
X Ray ◽  
Thermal Enhancement

Er3+ with different concentrations doped K2Yb(PO4)(MoO4) phosphors were prepared by a solid-state reaction method, and the layered orthorhombic crystal structure of the samples was confirmed by X-ray diffraction (XRD). Under...

Structure determination of fatty acid ester biofuels via in situ cryocrystallisation and single crystal X-ray diffraction

CrystEngComm ◽  
2019 ◽  
Vol 21 (1) ◽  
pp. 41-52 ◽  
Author(s):  
Siriyara Jagannatha Prathapa ◽  
Cara Slabbert ◽  
Manuel A. Fernandes ◽  
Andreas Lemmerer
Keyword(s):  
Crystal Structure ◽  
Fatty Acid ◽  
Fatty Acid Ester ◽  
Structure Determination ◽  
Homologous Series ◽  
Methyl Esters ◽  
X Ray Diffraction ◽  
X Ray

In situ cryocrystallisation enabled the crystal structure determination of a homologous series of low-melting n-alkyl methyl esters Cn−1H2n+1CO2CH3.

The Structure of the Novel Lichen Xanthone Thiomelin and Its Cogenors

1987 ◽  
Vol 40 (7) ◽  
pp. 1169 ◽  
Author(s):  
JA Elix ◽  
KL Gaul ◽  
M Sterns ◽  
MW Binsamsudin
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Ring Opening ◽  
Spectroscopic Data ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lichen Metabolite

The structure determination of thiomelin (2,4-dichloro-1,8-dihydroxy-5-methoxy-6-methyl-9H-xanthen-9-one) (3), an unusual lichen metabolite probably derived biosynthetically by oxidative ring opening of a precursor anthraquinone, is reported. The crystal structure of thiomelin diacetate (4) was determined by X-ray diffraction, while that of the cogenors 8-O-methylthiomelin (5), 4-dechlorothiomelin (7), 4-dechloro-8- O- methylthiomelin (9), 2-dechloro-8- O- methylthiomelin (10) and 2,4-dichloro-l-hydroxy-7-methoxy-6,8-dimethyl-9H-xanthen-9-one (12) were deduced from spectroscopic data.

Ni/GeSn solid-state reaction monitored by combined X-ray diffraction analyses: focus on the Ni-rich phase

2018 ◽  
Vol 51 (4) ◽  
pp. 1133-1140 ◽  
Author(s):  
Andrea Quintero ◽  
Patrice Gergaud ◽  
Joris Aubin ◽  
Jean-Michel Hartmann ◽  
Vincent Reboud ◽  
...  
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Solid State Reaction ◽  
Metastable Phase ◽  
Hexagonal Structure ◽  
X Ray Diffraction ◽  
Rich Phase ◽  
X Ray ◽  
Pole Figures

The Ni/Ge0.9Sn0.1 solid-state reaction was monitored by combining in situ X-ray diffraction, in-plane reciprocal space map measurements and in-plane pole figures. A sequential growth was shown, in which the first phase formed was an Ni-rich phase. Then, at 518 K, the mono-stanogermanide phase Ni(Ge0.9Sn0.1) was observed. This phase was stable up to 873 K. Special attention has been given to the nature and the crystallographic orientation of the Ni-rich phase obtained at low temperature. It is demonstrated, with in-plane pole figure measurements and simulation, that it was the ∊-Ni5(Ge0.9Sn0.1)3 metastable phase with a hexagonal structure.

Low-temperature crystallization and structure determination of N-(trifluoromethyl)formamide, N-(2,2,2-trifluoroethyl)formamide and 2,2,2-trifluoroethyl isocyanide

1999 ◽  
Vol 55 (1) ◽  
pp. 70-77 ◽  
Author(s):  
G. J. Perpétuo ◽  
J. Buschmann ◽  
P. Luger ◽  
D. Lentz ◽  
D. Dreissig
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
Crystal Packing ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Low Temperature Crystallization ◽  
Temperature Crystallization

Crystals of N-(trifluoromethyl)formamide, C2H2F3NO, (I), N-(2,2,2-trifluoroethyl)formamide, C3H4F3NO, (II), and 2,2,2-trifluoroethyl isocyanide, C3H2F3N, (III), were grown in situ on an X-ray diffractometer and analysed by single-crystal X-ray diffraction methods at low temperatures. Crystal data: (I) orthorhombic, P212121, a = 4.547 (2) Å, b = 5.947 (3) Å, c = 14.731 (9) Å, V = 398.3 (4) Å3, Z = 4, M r = 113.05, T = 143 K, D x = 1.885 Mg m−3; (II) monoclinic, P21/n, a = 4.807 (1) Å, b = 16.707 (3) Å, c = 6.708 (1) Å, β = 109.90 (1)°, V = 506.6 (2) Å3, Z = 4, M r = 127.07, T = 141 K, D x = 1.666 Mg m−3; (III) orthorhombic, P212121, a = 5.668 (2) Å, b = 9.266 (3) Å, c = 8.626 (2) Å, V = 453.0 (2) Å3, Z = 4, M r = 109.06, T = 163 K, D x = 1.599 Mg m−3. The results showed that in the crystal both formamides (I) and (II) are exclusively present in the form of the Z isomer, although measurements of solutions of (I) have shown that the E isomer prevails [Lentz et al. (1987). Angew. Chem. 99, 951–953]. In addition ab initio calculations for (I) predicted the E isomer to be the more stable one. In compound (III) the isocyanide group is staggered with respect to the trifluoroethyl group. In the crystal packing of (I) and (II) intermolecular N—H\cdotsO hydrogen bonds generate infinite chains. In (I), these chains are linked to form sheets by C—H\cdotsO contacts. In the crystal structure of (III) each isocyanide dipole is surrounded by four electronegative F atoms with intermolecular C\cdotsF contacts between 3.4 and 3.5 Å.

Synthesis and Crystal Structure of K6Mo10O33

2007 ◽  
Vol 62 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Nachiappan Arumugam ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Molybdenum Oxide ◽  
Solid State Reaction ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

A new potassium molybdenum oxide, K6Mo10O33, was synthesized by solid state reaction from the appropriate quantities of pre-dried MoO3 and K2MoO4, fired at around 650 °C for 2 d. The structure has been solved by using single crystal X-ray diffraction. The compound adopts the space group P1, with the lattice constants a = 7.7100(5), b = 11.9659(8), c = 17.1321(12) A° , α = 86.42 (10), β = 77.18(10), γ = 74.14(10)°. The structure is built up of infinite chains of edge-sharing MoO6 octahedra and groups of four MoO6 octahedra forming Mo4O17 units. These sub-units are connected together by common vertices.

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