Two new organic-selenate salts: syntheses and crystal structures of bis(di-iso-propylammonium) selenate and di-n-butylammonium hydrogenoselenate

2017 ◽  
Vol 72 (6) ◽  
pp. 425-432
Author(s):  
Waly Diallo ◽  
Libasse Diop ◽  
Cheikh Abdoul Khadir Diop ◽  
Laurent Plasseraud ◽  
Hélène Cattey

AbstractTwo new dialkyammonium selenate salts [i-Pr2NH2]2[SeO4] (1) and [n-Bu2NH2][HSeO4] (2) have been isolated and characterized by single-crystal X-ray diffraction. Salt 1 crystallizes in the monoclinic system, space group P21/n with a=8.7190(5), b=8.8500(4), c=22.5953(9) Å, β=94.6290(17)°, V=1737.84(14) Å3 and Z=4. Salt 2 crystallizes in the monoclinic system space group P21/n with a=10.9328(9), b=8.1700(6), c=13.8095(11) Å, β=97.130(3)°, V=1223.94(17) Å3 and Z=4. In both salts, dialkylammonium cations and selenate anions are connected through NH···O and OH···O hydrogen bonds. In the crystal structure, 1 and 2 are organized in layer-like arrangements. Structural characterizations were completed by infrared and 1H, 13C{1H} and 77Se NMR spectroscopy and elemental analysis which corroborate the X-ray elucidations.

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.


1996 ◽  
Vol 61 (9) ◽  
pp. 1335-1341 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová

The crystal structure of [(η4-C8H12)PdBr2] has been determined by a single crystal X-ray diffraction with R = 3.82% for 2 147 independent diffractions. The compound crystallizes with the symmetry of orthorhombic space group P212121 (No. 19) within the following parameters: a = 7.0785(5) Å, b = 11.1896(9) Å, c = 12.514(1) Å, V = 991.2(1) Å3, Z = 4. The square planar arrangement of ligands around Pd(II) is distorted due to the steric requirements of 1,5-cyclooctadiene in a twisted boat conformation. Formula units are joined by the weak C2-H2...Br1(1 + x, y, z) hydrogen bonds.


1998 ◽  
Vol 53 (2) ◽  
pp. 131-134 ◽  
Author(s):  
Willi Buchmeier ◽  
Bernward Engelen ◽  
Holger Müller

Abstract The crystal structure of MgSO3·H2O , space group P21 /ln, Z = 4, Dx = 2.415 g·cm-3 , a = 4.699(1), b = 12.751(3), c = 5.618(1) Å, β = 90.49(3)°, was determined by single crystal X-ray diffraction. MgSO3·H2O crystallizes in the MnSO3·H2O type. The structure consists of buckled trans layers ∞[MgSO3·H2O], which are built up from strongly distorted MgO5(H2O) octahedra sharing four equatorial vertices, and of trigonal pyramidal SO32- ions. It is close­ly related to the structures of orthorhombic MnSeO3·D2O and monoclinic ZnSeO3·H2O . The Mg-O distances range from 2.051(3) to 2.175(4) Å. The S-O distances (1.543(3), 1.547(3) and 1.493(3) Å) and the O-S-O angles (98.4(2) and 2x 106.0(2)°) correspond to those in MnSO3·H2O . The distortion of the MO5(H2O) octahedra (M = Mg, Mn) and of the SO32- ions is smaller in MgSO3·H2O , but with greater deviations from m symmetry. The distances between the H-connected ∞2[MSO3·H2O] layers are greater in MgSO3·H2O , indicating weaker inter-layer hydrogen bonds. The lateral arrangement of the ∞2[MSO3·H2O] layers is nearly the same in both sulfite monohydrates.


Author(s):  
M. Akkurt ◽  
E. Sarıpınar ◽  
S. Öztürk ◽  
C. Yılmaz ◽  
H.-K. Fun

AbstractThe crystal structure of (4-methoxy-phenyl)-[4-(4-methoxy-phenyl)-1-(1-phenylethylideneamino)-2-thioxo-1,2-dihydro-pyrimidin-5-yl]-methanone, has beeen determined by single-crystal X-ray diffraction at 183(2) K. The compound crystallizes in the monoclinic system, space group


1992 ◽  
Vol 47 (4) ◽  
pp. 460-464 ◽  
Author(s):  
Klaus Brodersen ◽  
Jürgen Hofmann

The structure of bis(m-aminobenzonitrile)dimercury(I) dinitrate, [Hg2(m -NH2C6H4CN)2](NO3)2 has been determined by single crystal X-ray diffraction techniques and refined to an Rw-value of 0.022. The crystals are triclinic, space group P1 with a = 5.4878(1) Å, b = 8.4085(1) Å, c = 9.6062(1) Å, α = 92.599(3)°, β = 94.763(3)°, γ = 89.614(3)° and Z = 1.The Hg22+-ion [Hg-Hg 2.524(1) Å] is approximately axially coordinated to amino nitrogen atoms [Hg - N 2.209(4) Å, Hg - Hg - N 169.5(3)°]. Additional amino hydrogen bonds to oxygen are building chains along the b-axis containing units of L - Hg - Hg - L groups.


2009 ◽  
Vol 64 (10) ◽  
pp. 1208-1212
Author(s):  
Patrick Bösing ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel

The reduction of a partially deprotonated bishydroxylamine complex {(tBu2Ga)2[cyclo-ON(Me)(CH2)2- (Me)NO][HON(Me)(CH2)2(Me)(H)NO]} with a reagent composed of titanium tetrachloride and methyllithium leads to the reduction of one of the N-O groups to an amine function affording the salt {(tBu2Ga)[cyclo- ON(H)(Me)(CH2)2NHMe]}+ {tBu2GaCl2}−. This has been characterised by 1H and 13C NMR spectroscopy, by elemental analysis and by single crystal X-ray diffraction, showing the neutral amine/hydroxylamine ligand to be present in its tautomeric aminoxide form. The molecules form hexameric cyclic aggregates by N-H···Cl hydrogen bonds.


2015 ◽  
Vol 34 (1) ◽  
pp. 101
Author(s):  
Alparslan Karadogan ◽  
Ahmet Karadag ◽  
Veysel T. Yilmaz

A new nickel(II) saccharinate (sac) complex containing <em>N</em>,<em>N</em>′-bis(2-hydroxyethyl)ethylenediamine (bishydeten), [Ni(bishydeten)<sub>2</sub>](sac)<sub>2</sub>, has been synthesized and characterized by elemental analysis, FTIR and single crystal X-ray diffraction. The title complex consists of a [Ni(bishydeten)<sub>2</sub>]<sup>2+</sup> cation and two sac anions. In the complex cation, the nickel(II) ion is coordinated by two neutral bishydeten ligands, leading to a distorted octahedral NiN<sub>4</sub>O<sub>2</sub> coordination, while both sac anions remain outside the coordination sphere. In the crystal, the complex cations and sac anions are connected by an extensive network of N–H∙∙∙N, N–H∙∙∙O, O–H∙∙∙O and C–H∙∙∙O hydrogen bonds into a three-dimensional supramolecular lattice.


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group


2020 ◽  
Vol 75 (8) ◽  
pp. 765-768
Author(s):  
Bohdana Belan ◽  
Dorota Kowalska ◽  
Mariya Dzevenko ◽  
Mykola Manyako ◽  
Roman Gladyshevskii

AbstractThe crystal structure of the phase Ce5AgxGe4−x (x = 0.1−1.08) has been determined using single-crystal X-ray diffraction data for Ce5Ag0.1Ge3.9. This phase is isotypic with Sm5Ge4: space group Pnma (No. 62), Pearson code oP36, Z = 4, a = 7.9632(2), b = 15.2693(5), c = 8.0803(2) Å; R1 = 0.0261, wR2 = 0.0460, 1428 F2 values and 48 variables. The two crystallographic positions 8d and 4c show Ge/Ag mixing, leading to a slight increase in the lattice parameters as compared to those of the pure binary compound Ce5Ge4.


2017 ◽  
Vol 72 (12) ◽  
pp. 983-988 ◽  
Author(s):  
Martin K. Schmitt ◽  
Hubert Huppertz

Abstractβ-Y(BO2)3 was synthesized in a Walker-type multianvil module at 5.9 GPa/1000°C. The crystal structure has been elucidated through single-crystal X-ray diffraction. β-Y(BO2)3 crystallizes in the orthorhombic space group Pnma (no. 62) with the lattice parameters a=15.886(2), b=7.3860(6), and c=12.2119(9) Å. Its crystal structure will be discussed in the context of the isotypic lanthanide borates β-Ln(BO2)3 (Ln=Nd, Sm, Gd–Lu).


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