Reaction products of diorganotin(IV) oxides, R2SnO, with nitric acid. Part 1: R = methyl, ethyl, and isopropyl

2014 ◽  
Vol 92 (6) ◽  
pp. 471-483 ◽  
Author(s):  
Hans Reuter ◽  
Martin Reichelt
Keyword(s):  
Nitric Acid ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Primary Reaction ◽  
One Dimensional ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Special Respect ◽  
Oxalate Ion ◽  
Tin Coordination

The reaction of diorganotin(IV) oxides, R2SnO with R = Me, Et, and i-Pr, with nitric acid in different stoichiometric ratios resulted in the formation of different products depending on the organic groups. The diorganotin(IV) nitrate hydroxides Me2Sn(NO3)(OH) (1a) Et2Sn(NO3)(OH), α-1b, β-1b, i-Pr2Sn(NO3)(OH) (1c), the diisopropyltin(IV) dinitrate dihydrate, i-Pr2Sn(NO3)2·2H2O (2c) and the diisopropyltin(IV) nitrate oxalate dihydrate, [i-Pr2Sn(NO3)]2Ox·2H2O (3) as side-product. On examination of the solubility of the primary reaction products in different solvents, the two additional compounds Me2Sn(NO3)(OH)·DMSO (4) and 2i-Pr2Sn(NO3)2·3DMSO = [i-Pr2Sn(NO3)(dmso)3] [i-Pr2Sn(NO3)3] (5) have been isolated. All compounds have been structurally characterized by single crystal X-ray diffraction with special respect to dimensionality (1a, α-1b, 1c = dimeric molecules hydrogen bonded to one-dimensional chains; β-1b = two-dimensional coordination polymer; 2c = monomeric; 3 = monomeric, tin atoms linked via a double side-on chelating oxalate ion; 4 = dimeric, 5 = monomeric anion/cation), tin coordination (trigonal-bipyramidal = 1a, α-1b, 1c; six-fold = β-1b; seven-fold = 3, 4, 5-cation; eight-fold = 2c, 5-anion) and nitrate bonding modes (monodentate = 1a, α-1b, 1c; unsymmetrical bidentate = 3, symmetrical bidentate = 3, 4, 5-cation, 5-anion; syn-anti bridging = β-1b), the latter one being analysed using both, Sn–O and N–O distances.

Reaction products of diorganotin(IV) oxides, R2SnO, with nitric acid. Part 2 – R = n-butyl and t-butyl

2014 ◽  
Vol 92 (6) ◽  
pp. 484-495 ◽  
Author(s):  
Hans Reuter ◽  
Martin Reichelt
Keyword(s):  
Nitric Acid ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Primary Reaction ◽  
Dimeric Molecule ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Solvent Molecules ◽  
Hydroxide Hydrate ◽  
Hydrogen Bonded

The reaction of diorganotin(IV) oxides, R2SnO with R = n-butyl and t-butyl, with nitric acid in different stoichiometric ratios resulted in the formation of different products depending on the organic groups attached to the tin atom: the diorganotin(IV) dinitrate dihydrates, n-Bu2Sn(NO3)2·2H2O (2d) and t-Bu2Sn(NO3)2·2H2O (2e), the mixed diorganotin(IV) nitrate methoxide oxide n-Bu2Sn(NO3)(n-Bu2SnOMe)O (6), and the diorganotin(IV) nitrate hydroxide hydrate t-Bu2Sn(NO3)(OH)·H2O = [t-Bu2Sn(OH)(H2O)][NO3] (7). On examination of the solubility of the primary reaction products in different solvents, the three additional compounds t-Bu2Sn(NO3)(OH)·DMSO (8), t-Bu2Sn(NO3)(OH)·THF, and 2-t-Bu2Sn(NO3)(OH)·DMF = [t-Bu2Sn(OH)dmf]2[NO3]2·[t-Bu2Sn(NO3)OH]2 (9) could be isolated. All compounds have been structurally characterized by single crystal X-ray diffraction (primary results for 7) with special attention paid to dimensionality (2d and 2c = monomeric, hydrogen bonded molecules; 6 = dimeric molecules of ladder-type structure; 7 = dimeric cation; 8 = dimeric molecule with hydrogen bonded solvent molecules; 9 = both components dimeric), tin coordination (6, 7, 8, and 9 = trigonal bipyramidal; 2d and 2e = eightfold), and nitrate bonding modes (7 and 9 = isolated, hydrogen bonded; 6, 8, and 9 (component 2) = monodentate; 2d and 2e = symmetrical bidentate), the latter one being analyzed using both Sn–O and N–O distances.

Monomere und dimere Oxotrihalogenoselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]SeOCl3 und [N(C2H5)4]SeOCl3 / Monomerie and Dimeric Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of [As(C6H5)4]SeOCl3 and [N(C2H5)4]SeOCl3

1983 ◽  
Vol 38 (1) ◽  
pp. 20-29 ◽  
Author(s):  
Bernt Krebs ◽  
Marita Hucke ◽  
Michael Hein ◽  
Andreas Schäffer
Keyword(s):  
Polymer Chains ◽  
Monoclinic Space Group ◽  
Structure And Properties ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers

Abstract The monomeric SeOCl3- ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6H5)4Cl, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6H5)4]SeOCl3 is monoclinic, space group P21/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) Å, β = 110,97(3)° (at -135 °C), Z = 4; it contains a novel type of ψ-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Å) and by one Cl(Se-Cl 2,234(1) Å), the axial Se-Cl bonds (2,430(1) and 2,475(1) Å) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P1̄, with a = 10,607(3), b = 8,950(2), c = 8,862(2) Å, α = 119,79(2)°, β = 101,07(2)°, γ = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se2O2Cl62- like in the [P(C6H5)4]+ salt, with two tetragonal SeOCl4 pyramids linked through a Cl···Cl edge and the lone pairs trans to the axial Se-O bonds (1,589(4) Å). Se-Cl bond lengths are 2.270(1) and 2,351(2) Å (terminal); 2,698(1) and 2,920(1) Å (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed.

Na+/H+ Topotactic Exchange on NaNbWO6 with TTB-like Structure: The series HxNa1-xNbWO6

2002 ◽  
Vol 755 ◽  
Author(s):  
A. Kuhn ◽  
F. García-Alvarado ◽  
H. Bashir ◽  
A. L. Dos Santos ◽  
J. L. Acosta
Keyword(s):  
Nitric Acid ◽  
Thermogravimetric Analysis ◽  
Chemical Analysis ◽  
Exchange Reaction ◽  
Proton Exchange ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Exchange Reactions ◽  
X Ray ◽  
Sodium Proton Exchange

ABSTRACTTTB-type NaNbWO6 has been used to perform sodium-proton exchange reactions by using nitric acid as an exchanging agent. The characterisation of the exchange reaction products, performed by means of chemical analysis, X-ray diffraction and thermogravimetric analysis, indicate that the exchange reaction takes place topotactically. The following formula is proposed for the obtained phase of variable composition: Na1-xHxNbWO6 (0<x<0.46).

Isostructural organic–inorganic hybrid compounds: triethylcholine tribromidocadmate and triethylcholine tribromidomercurate

2015 ◽  
Vol 71 (8) ◽  
pp. 728-732
Author(s):  
Dong-Yan Wang ◽  
Xue-Li Hou ◽  
Xue-Nan Li
Keyword(s):  
Hydrogen Bonding ◽  
Hybrid Materials ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
One Dimensional ◽  
X Ray ◽  
Hybrid Compounds ◽  
Trigonal Bipyramidal ◽  
Hydrogen Bonding Interactions ◽  
Distorted Trigonal Bipyramidal

In order to search for new anionic architectures and develop useful organic–inorganic hybrid materials in halometallate systems, two new crystalline organic–inorganic hybrid compounds have been prepared,i.e. catena-poly[triethyl(2-hydroxyethyl)azanium [[bromidocadmate(II)]-di-μ-bromido]], {(C8H20NO)[CdBr3]}n, (1), andcatena-poly[triethyl(2-hydroxyethyl)azanium [[bromidomercurate(II)]-di-μ-bromido]], {(C8H20NO)[HgBr3]}n, (2), and the structures determined by X-ray diffraction analysis. The compounds are isostructural, crystallizing in the space groupP21/n. The metal centres are five-coordinated by bromide anions, giving a slightly distorted trigonal–bipyramidal geometry. The crystal structures consist of one-dimensional edge-sharing chains ofMBr5trigonal bipyramids, between which triethylcholine counter-cations are intercalated. O—H...Br hydrogen-bonding interactions are present between the cations and anions.

Synthesis and Structure Characterization of some Triorganotin Esters of Heteroaromatic Carboxlic Acid and Crystal Structure of Triphenyltin Esters 5-Chloro-6-Hydroxynicotinic Acid

2012 ◽  
Vol 466-467 ◽  
pp. 463-468
Author(s):  
Hong Tao Gao
Keyword(s):  
Structure Characterization ◽  
Linear Polymers ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Ir And Nmr Spectroscopy ◽  
Bipyramidal Structure ◽  
Adjacent Molecule

Reactions of (R3Sn)2O (R=Ph, 2-ClC6H4CH2, 2-FC6H4CH2, 4-CNC6H4CH2) with 5-chloro-6-hydroxynicotinic acid in 1/2 stoichiometry yielded eight triorganotin compounds. These compounds have been characterized by elemental analysis, IR and NMR spectroscopy. The crystal structures of triphenyltin esters of 5-chloro-6-hydroxynicotinic acid were determined by single crystal X-ray diffraction. In the compound, the tin atoms are rendered five-coordinated in a trigonal bipyramidal structure by coordinating though the three phenyl carbon atoms and two oxygen atoms one from carboxylate and other from the phenolic hydroxide. The resulting structure is one-dimensional linear polymers through an interaction between the O atoms of phenolic hydroxide and tin atoms of an adjacent molecule.

Formalism for the determination of intermediate stress gradients using X-ray diffraction

2009 ◽  
Vol 42 (2) ◽  
pp. 192-197 ◽  
Author(s):  
Thomas Gnäupel-Herold
Keyword(s):  
Lattice Strain ◽  
Narrow Line ◽  
X Ray Diffraction ◽  
Beam Spot ◽  
Strain Measurements ◽  
One Dimensional ◽  
X Ray ◽  
Stress Gradients ◽  
Shaped Beam

A method is outlined that allows the determination of one-dimensional stress gradients at length scales greater than 0.2 mm. By using standard four-circle X-ray diffractometer equipment and simple aperture components, length resolutions down to 0.05 mm in one direction can be achieved through constant orientation of a narrow, line-shaped beam spot. Angle calculations are given for the adjustment of goniometer angles, and for the effective azimuth and tilt of the scattering vector for general angle settings in a four-circle goniometer. The latter is necessary for the computation of stresses from lattice strain measurements.

scholarly journals Hydrogen bonding in melamine compounds of amino acids

2014 ◽  
Vol 70 (a1) ◽  
pp. C534-C534
Author(s):  
Nasreddine Ghouari ◽  
Nourreedine Benali-Cherif
Keyword(s):  
Amino Acids ◽  
Hydrogen Bonding ◽  
Nitric Acid ◽  
Organic Cation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hybrid Compounds ◽  
Amino Butyric Acid ◽  
3D Network ◽  
Bonding Electron

The theme of this work is part of the study of intermolecular interactions that hold the crystal structures of hybrid compounds based sulphuric acid, nitric acid, Melamine, Diethylamine, L-(+) - glutamic acid, DL-2-amino butyric acid. The aim of this work is to enlarge our laboratory researches [1-3] and methods in synthesis of new hybrid compounds consisting in organic cation(s) and mineral anion(s). We have obtained single crystals of a few samples after several trials and we plan to synthesize and characterize these crystals by X-ray diffraction, FTIR and Raman. The crystals structures allow us to study the 3D network hydrogen bonding, electron density and collect several other informations useful in FTIR and Raman studies of these hybrid compounds.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

Polysulfonylamine, CXXV [1]. Neue Komplexe von Disulfonylaminen mit Kronenethern - im voraus entworfen oder zufällig entdeckt / Polysulfonylamines, CXXV [1]. New Complexes of Disulfonylam ines with Crown Ethers - Preconceived or Discovered by Serendipity

2000 ◽  
Vol 55 (3-4) ◽  
pp. 299-316 ◽  
Author(s):  
Dagmar Henschel ◽  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bonds ◽  
X Ray Diffraction ◽  
Ladder Structure ◽  
Triclinic Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Bonding System ◽  
Supramolecular Aggregate ◽  
Guest Species ◽  
The One

Abstract In a study aim ed at the „deconstruction“ of the supramolecular aggregate 3(18C6) · 2HN( SO2Me)2 (1,18C6 = 18-crown-6), which is known to display a ladder structure with two isotactic [18C6 - Me SO2N(H)SO2Me···)∞ polymers forming the uprights and symmetrically N - H···O bonded 18C6 rings providing the rungs, the following crystalline complexes were isolated and (except for 2b) characterized by low-temperature X-ray diffraction: 18C6-ClN (SO2Me)2 (2a, triclinic, space group P1̅, Z = 2), 18C6-PhN (SO2Me)2 (2b), 18C6 -MeN(SO2Me)2 (3, monoclinic, P21/c, Z = 8), Bz18C6-HN(SO2Me)2 (4, Bz18C6 = benzo-18-crown-6, monoclinic, P21/n, Z = 4), 18C6-2 MeN (SO2Me)2 (5, triclinic, P1̅, Z = 1), 18C6-Me2SO- HN( SO2Me) (SO2Ph) (13, triclinic, P1̅, Z = 2), and 18C6-H2OMe2SO·2HN(SO2Me)2 (14, triclinic, P1̅, Z = 2). Each of the one-dimensional polymers 2a (syndiotactic), 3 (disyndiotactic) and 4 (isotactic) mimics a single upright of 1; in contrast to 1 and 2a, where the intra-catemer connectivity solely relies on S - Me ··· crow n and crown ··· O = S hydrogen bonds, this bonding system is reinforced in 3 by N -Me ··· crown and in 4 by N - H ··· crown hydrogen bonds. Complex 5 is monomeric and matches a fragment formally extruded from the catemer 3; moreover, 3 and 5 represent a rare case of two structurally characterized 18C6 complexes containing the same uncharged guest species in distinct molecular ratios. The surprising structure of the quaternary adduct 14 exhibits an [18C6 ··· MeSO2N(H)SO2Me ··· ]∞ chain, which can be regarded both as an isolated, though unmodified upright from the ladder 1 and, being syndiotactic, as a stereochemical analogue of 2a; the potentially rung-forming *NH functions in the chain are blocked by hydrogenbonded side chains of the type * N - H ··· water ··· sulfoxide ··· H - N (SO2Me)2. The ternary complex 13 consists of chains [18C6 ··· Me2SO ··· H - N (SO2Ph)SO2Me···]∞ and is not closely related to the other structures

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