Mono- and Di-Lanthanide Derivatives of 19-Tungsto-2-Arsenate(III)

2010 ◽  
Vol 65 (3) ◽  
pp. 383-r392 ◽  
Author(s):  
Amal H Ismail ◽  
Bassem S Bassil ◽  
Isabella Römer ◽  
Nils C. Redeker ◽  
Ulrich Kortz

Two types of lanthanide-containing derivatives of the 19-tungsto-2-arsenate(III) [As2W19O67- (H2O)]14− (As2W19) have been synthesized in mildly acidic aqueous media and characterized in the solid state. The ytterbium(III)-containing anion [Yb(H2O)2K(H2O)2As2W19O67(H2O)]10− (1) was formed by reaction of Yb3+ with the potassium salt of As2W19, while the lanthanum(III) derivative [La2(H2O)6As2W19O67(H2O)]8− (2) was formed by reaction of La3+ with the sodium salt of the trilacunary precursor [B-α-AsW9O33]9− (AsW9). The polyanions 1 and 2 crystallize as hydrated salts in the triclinic system, space group P1̄: K9.5Na0.5[Yb(H2O)2K(H2O)2As2W19O67(H2O)]·25H2O (KNa-1) with cell dimensions a = 12.4730(5), b = 17.4630(9), c = 21.1990(10) Å, α = 72.568(3)◦, β = 85.442(2)◦, γ = 89.147(3)◦, Z = 2; Na8[La2(H2O)8As2W19O67(H2O)]·17H2O (Na-2) with cell dimensions a = 14.929(2), b = 17.769(3), c = 20.754(4) Å, α = 77.203(10)◦, β = 80.273(9)◦, γ = 72.670(9)◦, Z = 2. Both compounds KNa-1 and Na-2 were characterized in the solid state by FTIR spectroscopy, TGA and single-crystal X-ray diffraction analyses. In polyanion 1, the As2W19 unit sandwiches one ytterbium and one potassium ion leading to a structure with idealized Cs symmetry, whereas polyanion 2 incorporates two lanthanum ions leading to a structure with idealized C2v symmetry. Compositional analogs of polyanions 1 (Ln = La, Ce, Eu, Gd and Lu) and 2 (Ce) were also synthesized and identified by FTIR spectroscopy.

2022 ◽  
Vol 1049 ◽  
pp. 218-223
Author(s):  
Aleksandr S. Kazachenko ◽  
Yuriy N. Malyar ◽  
Anna S. Kazachenko

Sulfated derivatives of polysaccharides have anticoagulant, hypolipedimic and other biological activity. In this work, a complex mixed ester of galactomannan, its sulfate-citrate, was obtained for the first time. The introduction of citrate and sulfate groups was proved by FTIR spectroscopy by the appearance of corresponding absorption bands. It was shown by X-ray diffraction that the introduction of the citrate group leads to the amorphization of the galactomannan structure.


Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5745
Author(s):  
Sergey A. Anufriev ◽  
Sergey V. Timofeev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
Igor B. Sivaev

Complexation of the 8,8′-bis(methylsulfanyl) derivatives of cobalt and iron bis(dicarbollides) [8,8′-(MeS)2-3,3′-M(1,2-C2B9H10)2]− (M = Co, Fe) with copper, silver, palladium and rhodium leads to the formation of the corresponding chelate complexes, which is accompanied by a transition from the transoid to the cisoid conformation of the bis(dicarbollide) complex. This transition is reversible and can be used in design of coordination-driven molecular switches based on transition metal bis(dicarbollide) complexes. The solid-state structures of {(Ph3P)ClPd[8,8′- (MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} and {(COD)Rh[8,8′-(MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} were determined by single crystal X-ray diffraction.


2014 ◽  
Vol 2014 ◽  
pp. 1-9
Author(s):  
Hamadi Hamza ◽  
Mohamed Faouzi Zid ◽  
Ahmed Driss

LiNa5K3Mo11As3O45 is a new inorganic compound. It was synthesized by a solid state method. The crystal structure has been studied by single crystal X-ray analysis. The R-values reached 2.8%. The title compound crystallizes in the triclinic system, space group P-1, with a = 10.550 (2) Å, b = 11.723 (2) Å, c = 17.469 (3) Å, α = 102.35 (3)°, β = 87.61 (2)°, and γ = 111.03 (3)°. The anionic unit [Mo11As3O45]9− is formed by nine MoO6 octahedra, two MoO5 trigonal bipyramids, and three AsO4 tetrahedra. The association of [Mo11As3O45]9− units, running along [010], leads to a one-dimensional framework. Li, K, and Na are located in the space surrounding the anionic ribbons. This material was characterized by SEM microscopy, IR spectroscopy, and powder X-ray diffraction. The electrical conductivity was investigated from 528 K to 673 K by impedance complex followed by DSC spectroscopy.


2009 ◽  
Vol 344 (13) ◽  
pp. 1734-1744 ◽  
Author(s):  
Tomasz Gubica ◽  
Andrzej Temeriusz ◽  
Katarzyna Paradowska ◽  
Andrzej Ostrowski ◽  
Paulina Klimentowska ◽  
...  

2000 ◽  
Vol 22 (1-2) ◽  
pp. 169-173 ◽  
Author(s):  
E Beregi ◽  
A Watterich ◽  
L Kovács ◽  
János Madarász

2015 ◽  
Vol 93 (3) ◽  
pp. 375-379 ◽  
Author(s):  
Karlee L. Bamford ◽  
Alasdair P.M. Robertson ◽  
Hilary A. Jenkins ◽  
Brian O. Patrick ◽  
Neil Burford

Three series of phosphine chalcogenide complexes of the antimony(III) halides SbX3 (X = F, Cl, Br, or I) have been synthesized and characterized by spectroscopic and crystallographic methods. Complexes of the generic formulae (Cy3PO)SbX3 (X = F (1a), Cl (1b), or Br (1c)), (Cy3PO)2SbX3 (X = F (2a), Cl (2b), or Br (2c)), and (Cy3PS)SbX3 (X = Cl (3b), Br (3c), or I (3d)) were synthesized via the treatment of solutions of SbX3 with OPCy3 and SPCy3, respectively. Derivatives of (Cy3PO)SbX3 were characterized by single crystal X-ray diffraction for 1a and 1b and crystallize as dimers through symmetry related intermolecular Sb–X interactions, providing the first structurally characterized examples of this class of complex. Derivatives of (Cy3PS)SbX3 (3b–3c) adopt analogous dimeric structures in the solid state. The solid-state structure of (Cy3PO)2SbCl3 (2b) is consistent with the previously reported structures of bis-phosphine oxide complexes of antimony(III), with a square pyramidal Sb center and cis-configured OPCy3 ligands. The phosphine chalcogenide complexes of SbX3 display configurations that are consistent with the perceived trans-labilizing properties of the ligands/substituents.


1978 ◽  
Vol 33 (7) ◽  
pp. 753-755 ◽  
Author(s):  
G. Struckmeier ◽  
J. Engel ◽  
U. Thewalt

Abstract The crystal and molecular structure of the title compound has been determined by X-ray diffraction. The compound possesses an (almost) planar Z configuration. The ions form ion pairs in the solid state: each bromide anion is connected via two hydrogen bonds with a cation. The crystal data are: space group P21/n with Z = 4; cell dimensions a = 14.097(2), b = 11.591(2), c = 14.133(3) Å, β = 106,22(2)°.


Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3357
Author(s):  
Catalin Vasile Maftei ◽  
Martin Heiko Franz ◽  
Christian Kleeberg ◽  
Ion Neda

The substance class of the well-known Cinchona alkaloids is widened by 6′-Amino-cinchonine and 6′-Amino-cinchonidine, novel compounds which incorporate a primary amino function in the quinolinic ring system. These key intermediates open the field for a range of fruitful chemistry. Here is described a short and direct pathway for the synthesis of triazole containing derivatives of the above-mentioned substances using the [3 + 2] Huisgen cycloaddition. For this purpose, the amines were first converted into the corresponding azides. Based on this, non-substituted and silyl-protected triazoles were synthesized as examples. Furthermore, didehydrated derivatives of quincorine and quincoridine were used as addition partners, resulting in compounds that carry the quinuclidine ring of the cinchona alkaloids at both ends. Some of these compounds were examined radiographically to investigate the position of the quinuclidine ring to the triazole. The solid-state structures of compounds 10, 11 and 28 were determined by X-ray diffraction analyses.


2010 ◽  
Vol 65 (7) ◽  
pp. 776-782 ◽  
Author(s):  
Gerhard Laus ◽  
Klaus Wurst ◽  
Volker Kahlenberg ◽  
Holger Kopacka ◽  
Christoph Kreutz ◽  
...  

1-Hydroxyimidazole-3-oxide (1) was alkylated with benzyl bromide in the presence of NaHCO3 to give the new 1,3-di(benzyloxy)imidazolium bromide 2a which was converted to the hexafluorophosphate 2b and bis(trifluoromethylsulfonyl)imide 2c. From this cation, pyridine generated a carbene which was trapped by sulfur or selenium to yield the respective 2-thione 3 or 2-selone 4. Bromination afforded the 2-bromo derivative 5. Reaction of the hexafluorophosphate 2b with silver oxide gave the silver-N-heterocyclic carbene complex 6 which was transmetallated with Au(Me2S)Cl to the gold-carbene complex 7. A rhodium-carbene complex 8 was obtained by reaction of the hexafluorophosphate 2b with [Rh(cod)Cl]2 in the presence of triethylamine. Eight crystal structures were determined by X-ray diffraction. The N-benzyloxy groups are twisted out of the plane of the imidazole ring in the solid state. They adopt syn conformations in the cation of the hexafluorophosphate 2b and in the metal-carbene complexes 6 - 8, but anti conformations in the thione 3 and selone 4. Both conformations were observed in two polymorphs of the 2-bromo compound 5.


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