Coordination Chemistry of Polynitriles, I. Syntheses and Crystal Structures of [Ag(PCC)(DMF)], [Ni(DMF)6](PCC)2 and [Co(DMF)6](PCC)2 (PCC = [C5(CN)5]-, DMF = N,N-Dimethylformamide) [1]

2013 ◽  
Vol 68 (5-6) ◽  
pp. 546-550 ◽  
Author(s):  
Karlheinz Sünkel ◽  
Dietmar Reimann
Keyword(s):  
Coordination Chemistry ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pentagonal Symmetry

Recrystallization of silver pentacyanocyclopentadienide Ag[C5(CN)5] from N,N-dimethylformamide (DMF) gives the polymeric 1:1 complex [Ag{C5(CN)5}(DMF)] (1). The Ag+ cation is coordinated by three N atoms of three different [C5(CN)5]- anions and two O atoms of two DMF molecules. Each [C5(CN)5]- is coordinated via three neighboring CN groups to three different Ag+ ions, while each DMF molecule bridges two Ag+ ions via its O atom. Treatment of NiCl2 6H2O, CoCl2 6H2O or ZnCl2 with Ag[C5(CN)5] in DMF gives the DMF complexes [M(DMF)6][C5(CN)5]2 (M=Ni, 2; Co, 3; Zn, 4). The complexes 2 and 3 were characterized by X-ray diffraction and show octahedral [M(DMF)6]2+ cations with O-coordinated DMF molecules. The [C5(CN)5]- anions show ideal pentagonal symmetry

New Insights into Hexacoordinated Silicon Complexes with 8- Oxyquinolinato Ligands: 1,3-Shift of Si-Bound Hydrocarbyl Substituents and the Influence of Si-Bound Halides on the 8-Oxyquinolinate Coordination Features

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1402-1418 ◽  
Author(s):  
Erik Wächtler ◽  
Alexander Kämpfe ◽  
Katrin Krupinski ◽  
Daniela Gerlach ◽  
Edwin Kroke ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
Quantum Chemical ◽  
Poor Response ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Torsion Angles ◽  
X Ray ◽  
Cp Mas Nmr

Abstract The transsilylation reaction between allyltrichlorosilane and 8-trimethylsiloxyquinoline in the molar ratio 1 : 3 yields the hexacoordinated silicon tris-chelate (oxinate)2Si(adho) (“oxinate” = 8- oxyquinolinate, “adho” = di-anion of 2-allyl-1,2-dihydro-8-oxyquinoline) comprising an SiO3N3 skeleton. The identity of this complex was established by single-crystal X-ray diffraction analysis and 29Si CP=MAS NMR spectroscopy of its chloroform solvate. Benzyltrichlorosilane and dibenzyldichlorosilane, comprising benzyl (Bn) as an “aromatically stabilized allyl moiety” did not undergo such rearrangement. Instead, the complexes (oxinate)2SiBnCl and (oxinate)2SiBn2 were obtained even upon using three molar equivalents of 8-trimethylsiloxyquinoline. We determined the crystal structure of a non-disordered bis-chelate (oxinate)2SiBnCl with Sibound hydrocarbyl and halogen substituents (the previously published (oxinate)2SiMeCl was disordered with alternative Me=Cl site occupancies). (Oxinate)2SiBnCl exhibits surprisingly poor response of the N-Si bonds to the different trans-disposed Si-X (X=Bn, Cl) bonds. For comparison and deeper insights into the coordination chemistry of oxinato silicon complexes with halide substituents, we determined the crystal structures of (oxinate)2SiPhCl·CHCl3, (oxinate)2SiCl2, (oxinate)2SiF2·1.5(CHCl3), and (8-oxyquinaldinate)2SiF2. Furthermore, the crystal structures of BnSiCl3 and Bn2SiCl2 (and its dibromo analog) are reported. The influence of the Si-C-C-C torsion angles of the benzyl group on the 29Si NMR shift of benzylsilanes (which is noticeably upfield with respect to analogous methyl silanes) was analyzed by quantum-chemical calculations.

Coordination Chemistry of Lipoic Acid and Related Compounds, Part 1 Syntheses and Crystal Structures of the UV- and Light-Sensitive Lipoato Complexes [M(lip)2(H2O)2] (M = Zn, Cd)

1997 ◽  
Vol 52 (1) ◽  
pp. 17-24 ◽  
Author(s):  
Henry Strasdeit ◽  
Angelika von Döllen ◽  
Anne-Kathrin Duhme
Keyword(s):  
Coordination Chemistry ◽  
Crystal Structures ◽  
Metal Nitrate ◽  
X Ray Diffraction ◽  
Carboxylate Ligands ◽  
X Ray ◽  
Layer Structures ◽  
Network Of Hydrogen Bonds ◽  
Related Compounds ◽  
Nm Range

The rac-lipoato (lip-) complexes [Zn(lip)2(H2O)2] (1) and [Cd(lip)2(H2O)2] (2) were obtained in good yields from solutions of sodium lipoate and the respective metal nitrate in methanol/water. 1 and 2 form pale yellow, moderately light-sensitive crystals.Both compounds were structurally characterized by single-crystal X-ray diffraction. 1: C2/c, a = 39.958(6), b = 5.360(1), c = 10.794(1) Å, β = 95.76(1)°, Z = 4, wR2 = 0.150 (all data). 2: C2/c, a = 38.200(2), b = 5.472(1), c = 11.179(1) Å, β = 92.72(1)°, Z = 4, wR2 = 0.090 (all data). The metal ions are hexacoordinated by the oxygen atoms of two chelating carboxylate ligands and two aqua ligands. The crystal structures are very similar but not isotypic. They are layer structures, in which the complexes within a layer are interconnected by a network of hydrogen bonds. Adjacent layers have contacts via the 1,2-dithiolanyl rings of their lipoato ligands.Crystals of 1 and 2 decompose on exposure to visible light or ultraviolet radiation in the 280-390 nm range. Photopolymerization by formation of intermolecular S-S bonds is very probably involved. Furthermore, the infrared spectra reveal the transformation of COO- into COOH groups

Transmission electron microscope studies in special ceramics

1978 ◽  
Vol 36 (1) ◽  
pp. 268-269
Author(s):  
A. Zangvil ◽  
L.J. Gauckler ◽  
G. Schneider ◽  
M. Rühle
Keyword(s):  
Phase Diagrams ◽  
Crystal Structures ◽  
Thin Foil ◽  
Limited Extent ◽  
Complex Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Electron Microscopes ◽  
Lattice Resolution

The use of high temperature special ceramics which are usually complex materials based on oxides, nitrides, carbides and borides of silicon and aluminum, is critically dependent on their thermomechanical and other physical properties. The investigations of the phase diagrams, crystal structures and microstructural features are essential for better understanding of the macro-properties. Phase diagrams and crystal structures have been studied mainly by X-ray diffraction (XRD). Transmission electron microscopy (TEM) has contributed to this field to a very limited extent; it has been used more extensively in the study of microstructure, phase transformations and lattice defects. Often only TEM can give solutions to numerous problems in the above fields, since the various phases exist in extremely fine grains and subgrain structures; single crystals of appreciable size are often not available. Examples with some of our experimental results from two multicomponent systems are presented here. The standard ion thinning technique was used for the preparation of thin foil samples, which were then investigated with JEOL 200A and Siemens ELMISKOP 102 (for the lattice resolution work) electron microscopes.

scholarly journals Crystal Chemical Relations in the Shchurovskyite Family: Synthesis and Crystal Structures of K2Cu[Cu3O]2(PO4)4 and K2.35Cu0.825[Cu3O]2(PO4)4

Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Complexity ◽  
Crystal Chemical ◽  
X Ray Diffraction ◽  
Complexity Measures ◽  
X Ray ◽  
The Family ◽  
Similarities And Differences ◽  
Related Compounds

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.

scholarly journals Building crystal structures of conjugated polymers through X‐ray diffraction and molecular modeling

SmartMat ◽  
2021 ◽  
Author(s):  
Ze‐Fan Yao ◽  
Qi‐Yi Li ◽  
Hao‐Tian Wu ◽  
Yi‐Fan Ding ◽  
Zi‐Yuan Wang ◽  
...  
Keyword(s):  
Molecular Modeling ◽  
Conjugated Polymers ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals A Versatile Approach to Access Trimetallic Complexes Based on Trisphosphinite Ligands

Molecules ◽  
2020 ◽  
Vol 25 (3) ◽  
pp. 593
Author(s):  
Juan Miranda-Pizarro ◽  
Macarena G. Alférez ◽  
M. Dolores Fernández-Martínez ◽  
Eleuterio Álvarez ◽  
Celia Maya ◽  
...  
Keyword(s):  
Coordination Chemistry ◽  
Late Transition Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Full Characterization ◽  
Metal Precursors ◽  
Straightforward Method ◽  
One Step ◽  
Late Transition

A straightforward method for the preparation of trisphosphinite ligands in one step, using only commercially available reagents (1,1,1-tris(4-hydroxyphenyl)ethane and chlorophosphines) is described. We have made use of this approach to prepare a small family of four trisphosphinite ligands of formula [CH3C{(C6H4OR2)3], where R stands for Ph (1a), Xyl (1b, Xyl = 2,6-Me2-C6H3), iPr (1c), and Cy (1d). These polyfunctional phosphinites allowed us to investigate their coordination chemistry towards a range of late transition metal precursors. As such, we report here the isolation and full characterization of a number of Au(I), Ag(I), Cu(I), Ir(III), Rh(III) and Ru(II) homotrimetallic complexes, including the structural characterization by X-ray diffraction studies of six of these compounds. We have observed that the flexibility of these trisphosphinites enables a variety of conformations for the different trimetallic species.

scholarly journals The crystal structures and mechanical properties of the uranyl carbonate minerals roubaultite, fontanite, sharpite, widenmannite, grimselite and čejkaite

2020 ◽  
Vol 7 (21) ◽  
pp. 4197-4221 ◽  
Author(s):  
Francisco Colmenero ◽  
Jakub Plášil ◽  
Jiří Sejkora
Keyword(s):  
Mechanical Properties ◽  
Hydrogen Bonding ◽  
Diffraction Pattern ◽  
Crystal Structures ◽  
First Principles ◽  
X Ray Diffraction ◽  
Carbonate Minerals ◽  
X Ray ◽  
Uranyl Carbonate

The structure, hydrogen bonding, X-ray diffraction pattern and mechanical properties of six important uranyl carbonate minerals, roubaultite, fontanite, sharpite, widenmannite, grimselite and čejkaite, are determined using first principles methods.

Crystal structures of (S)- and (R,S)-2,2′-bipyridine-3,3′-dicarboxylic acid 1,1′-dioxides and of their barium salts: absolute configuration and molecular distortion enforced by supramolecular self-assembly

1997 ◽  
Vol 212 (3) ◽  
Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  
Keyword(s):  
Single Crystal ◽  
Dicarboxylic Acid ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Self Assembly ◽  
Barium Salt ◽  
X Ray Diffraction ◽  
X Ray

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(

Synthesis and Crystal Structures of the P,N-Substituted Ferrocenes [Fe{η5-C5H4–P(S)Ph2}(η5-C5H4–NHCH2tBu)] and [Fe(η5-C5H4– PPh2)(η5-C5H4–NHCH2tBu)]

2014 ◽  
Vol 69 (8) ◽  
pp. 906-912 ◽  
Author(s):  
Michael Ritte ◽  
Clemens Bruhn ◽  
Ulrich Siemeling
Keyword(s):  
Crystal Structures ◽  
Raney Nickel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bromo Derivative

The P,N-substituted ferrocene [Fe{η5-C5H4-P(S)Ph2}(η5-C5H4-NHCH2tBu)] was prepared in six steps from the bromo derivative [Fe{η5-C5H4-PPh2}(η5-C5H4-Br)]. Its reductive desulfurisation with Raney nickel afforded the corresponding phosphino-substituted derivative [Fe(η5-C5H4- PPh2)(η5-C5H4-NHCH2tBu)]. Both compounds have been structurally characterised by singlecrystal X-ray diffraction studies.

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