Study of structure of bis(triphenylstannyl) chromate(VI) by infrared, Mössbauer, and 1H, 13C and 119Sn NMR spectra

1984 ◽  
Vol 49 (6) ◽  
pp. 1497-1504 ◽  
Author(s):  
Karel Handlíř ◽  
Jaroslav Holeček ◽  
Milan Nádvorník ◽  
Antonín Lyčka ◽  
Milan Hucl
Keyword(s):  
Solid State ◽  
Molecular Complex ◽  
Equatorial Plane ◽  
Nmr Spectra ◽  
Three Dimensional ◽  
119Sn Nmr ◽  
Bridge Oxygen ◽  
The Common ◽  
Ester Molecule ◽  
Oxygen Atoms

The infrared, Mössbauer, and 1H, 13C and 119 Sn NMR spectra have been used to study the structure of bis(triphenylstannyl) chromate(VI) in solid state and in solvents of both noncoordinating and coordinating types. In solid state the compound forms a three-dimensional polymer: the tetrahedral CrO4 group and trans-trigonally bipyramidal (C6H5)3SnO2 grouping are connected mutually symmetrically by bridges represented by the common oxygen atoms. The three phenyl groups in the (C6H5)3SnO2 grouping are located in the equatorial plane of the trigonal bipyramide which is completed by two bridge oxygen atoms in axial positions. Solutions in noncoordinating solvents contain monomeric bis(triphenylstannyl) chromate(VI). The ester molecule contain two tetrahedral, (C6H5)3SnO groups bound by oxygen bridges to a CrO4 group which shows the C2v symmetry. In coordinating solvents the title compound forms a molecular complex having the coordination number 5 at the central tin atom.

119Sn, 13C and 1H NMR Spectra of Tris(1-butyl)stannyl D-Glucuronate

1997 ◽  
Vol 62 (8) ◽  
pp. 1169-1176 ◽  
Author(s):  
Antonín Lyčka ◽  
Jaroslav Holeček ◽  
David Micák
Keyword(s):  
Chemical Shift ◽  
Carbonyl Group ◽  
1H Nmr ◽  
Equatorial Plane ◽  
Title Compound ◽  
Nmr Spectra ◽  
Hydroxyl Groups ◽  
Carboxylic Group ◽  
H Nmr ◽  
Oxygen Atoms

The 119Sn, 13C and 1H NMR spectra of tris(1-butyl)stannyl D-glucuronate have been measured in hexadeuteriodimethyl sulfoxide, tetradeuteriomethanol and deuteriochloroform. The chemical shift values have been assigned unambiguously with the help of H,H-COSY, TOCSY, H,C-COSY and 1H-13C HMQC-RELAY. From the analysis of parameters of 119Sn, 13C and 1H NMR spectra of the title compound and their comparison with the corresponding spectra of tris(1-butyl)stannyl acetate and other carboxylates it follows that in solutions of non-coordinating solvents (deuteriochloroform) the title compound is present in the form of more or less isolated individual molecules with pseudotetrahedral environment around the central tin atom and with monodentately bound carboxylic group. The interaction of tin atom with oxygen atoms of carbonyl group and hydroxyl groups of the saccharide residue - if they are present at all - are very weak. In solutions in coordinating solvents (hexadeuteriodimethyl sulfoxide or tetradeuteriomethanol), the title compound forms complexes with one molecule of the solvent. Particles of these complexes have a shape of trigonal bipyramid with the 1-butyl substituents in equatorial plane and the oxygen atoms of monodentate carboxylic group and coordinating solvent in axial positions.

IR and 13C, 17O, and 119Sn NMR spectra of some bis(1-butyl)tin(IV) carboxylates of dicarboxylic acids

1991 ◽  
Vol 56 (9) ◽  
pp. 1908-1915 ◽  
Author(s):  
Jaroslav Holeček ◽  
Antonín Lyčka ◽  
Milan Nádvorník ◽  
Karel Handlíř
Keyword(s):  
Infrared Spectroscopy ◽  
Nmr Spectroscopy ◽  
Dicarboxylic Acid ◽  
Nmr Spectra ◽  
Dicarboxylic Acids ◽  
119Sn Nmr ◽  
Carboxylic Groups ◽  
Cyclic Oligomers ◽  
The Media ◽  
Oxygen Atoms

Infrared spectroscopy and multinuclear (13C, 17O, and 119Sn NMR spectroscopy have been used to study the structure of bis(1-butyl)tin(IV) carboxylates of dicarboxylic acids (1-C4H9)2. Sn(X(COO)2), where X = (CH2)n (n = 0-8), CH=CH (cis and trans) and C6H4 (ortho and para).The crystalline compounds are formed by linear or cyclic oligomers or polymers whose basic building units represent a grouping composed of the central tin atom substituted by two 1-butyl groups and coordinated with both oxygen atoms of two anisobidentate carboxylic groups derived from different molecules of a dicarboxylic acid. The environment of the tin atom has a shape of a trapezoidal bipyramid. When dissolvet in non-coordinating solvents, the compounds retain the oligomeric character with unchanged structure of environment of the central tin atom. In the media of coordinating solvents the bis(1-butyl)tin(IV) carboxylates of dicarboxylic acids form complexes whose central hexacoordinated tin atom binds two molecules of the solvent trough their donor atoms. Carboxylic groups form monodenate linkages in these complexes.

On the assignment of 119Sn resonances of bis[dicarboxylatotetraorganodistannoxanes] in solution and solid state 119Sn NMR spectra

1998 ◽  
Vol 552 (1-2) ◽  
pp. 177-186 ◽  
Author(s):  
François Ribot ◽  
Clément Sanchez ◽  
Abdelkrim Meddour ◽  
Marcel Gielen ◽  
Edward R.T Tiekink ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
119Sn Nmr

scholarly journals Single-crystal Structure and Solid-state NMR of Ga2–xScxO3 (x = 0.83)

2011 ◽  
Vol 66 (1) ◽  
pp. 14-20
Author(s):  
Hamdi Ben Yahia ◽  
Leo van Wüllen ◽  
Sarkarainadar Balamurugan ◽  
Ute Ch. Rodewald ◽  
Hellmut Eckert ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Growth ◽  
Solid State ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Three Dimensional ◽  
Crystal Data ◽  
X Ray ◽  
Nmr Data

Colorless needles of Ga2−xScxO3 (x = 0.83) were isolated during the crystal growth of La3Ga3Sc2O12 in a K2WO4 flux. The structure was refined from X-ray single-crystal data: β -Ga2O3 type,C2/m, Z = 4, a = 12.716(4), b = 3.1566(6), c = 5.928(5) Å , β = 102.57(3)◦,V = 232.2 Å3, wR2 = 0.0618, 429 F2 values, 32 variables. The structure is based on infinite double chains of edge-sharing Sc/GaO6 octahedra running along the b axis. The GaO4 tetrahedra connect these chains by sharing corners and form a three-dimensional framework. The oxygen atoms form a distorted ccp pattern. The 45Sc NMR spectra confirm the presence of a single scandium site, while 71Ga NMR data clearly prove the partial occupancy of the scandium site by gallium atoms. The nuclear electric quadrupolar parameters of 45Sc and 71Ga are discussed in relation to the crystallographic atomic environments

Synthesis of a Novel Lanthanide Oxide Nitrate Compound with 3D Structure

2014 ◽  
Vol 809-810 ◽  
pp. 218-221
Author(s):  
Hua Li ◽  
Yan Min Yu ◽  
Zhao Yuan Gong ◽  
Hui Ying Chen ◽  
Wen Zhong Wang
Keyword(s):  
3D Structure ◽  
Three Dimensional ◽  
Lanthanide Ions ◽  
Dimensional Structure ◽  
X Ray Diffraction ◽  
Lanthanide Oxide ◽  
X Ray ◽  
Open Framework ◽  
Bridge Oxygen ◽  
Oxygen Atoms

One lanthanide nitrate (Ln = Tb) with a novel three dimensional structure have been prepared through hydrothermal method. Single crystal X-ray diffraction structures were obtained. The compound crystallizes in the orthorhombic,Pnmaspace group. The lanthanide ions are eight-coordinate with six oxygen atoms coming from nitrate ions and two from bridge oxygen atoms. If the bridge oxygen atoms could be ignored, the compound can be described as a rare microporous 3D Lanthanide nitride with the open framework.

scholarly journals Solid-State 17O NMR Study of α-D-Glucose: Exploring New Frontiers in Isotopic Labeling, Sensitivity Enhancement, and NMR Crystallography

2022 ◽  
Author(s):  
Jiahui Shen ◽  
Victor Terskikh ◽  
Jochem Struppe ◽  
Alia Hassan ◽  
Martine Monette ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Isotopic Labeling ◽  
Sensitivity Enhancement ◽  
17O Nmr ◽  
Nmr Study ◽  
Nmr Characterization ◽  
Nmr Crystallography ◽  
Oxygen Atoms

We report synthesis and solid-state 17O NMR characterization of α-D-glucose for which all six oxygen atoms are site-specifically 17O-labeled. Solid-state 17O NMR spectra were recorded for α-D-glucose/NaCl/H2O (2/1/1) cocrystals under...

scholarly journals Solid-state 119Sn NMR and M¨ossbauer Spectroscopic Studies of the Intermediate-valent Stannide CeRuSn

2012 ◽  
Vol 67 (5) ◽  
pp. 473-478 ◽  
Author(s):  
Falko M. Schappacher ◽  
Panchanana Khuntia ◽  
Anakot K. Rajarajan ◽  
Michael Baenitz ◽  
John A. Mydosh ◽  
...  
Keyword(s):  
Solid State ◽  
Magnetic Anisotropy ◽  
Ground State ◽  
Nmr Spectra ◽  
Spectroscopic Studies ◽  
Hyperfine Fields ◽  
Local Site ◽  
119Sn Nmr ◽  
Intermediate Valent ◽  
Absolute Shift

The ternary stannide CeRuSn is a static mixed-valent cerium compound with an ordering of trivalent and intermediate-valent cerium on two distinct crystallographic sites. 119Sn Mössbauer spectra showed two electronically almost identical tin atoms at 323 K, while at 298 K and below (77 and 4:2 K) two tin sites can clearly be distinguished. Solid-state 119Sn NMR experiments were performed to probe the local hyperfine fields at the two different Sn sites. Powder 119Sn NMR spectra are nicely fitted with two Sn sites with nearly the same magnetic anisotropy, but with different absolute shift values. Both Sn sites are strongly affected by crossover-like transitions between 100 and 280 K. This local-site study confirms the superstructure modulations found in previous investigations. Towards lower temperatures the powder NMR spectra are broadened giving strong precursor evidence for the antiferromagnetically ordered ground state.

The reaction of thiourea and 1,3-dimethylthiourea towards organoiodines: oxidative bond formation and halogen bonding

2021 ◽  
Vol 77 (10) ◽  
pp. 599-609
Author(s):  
Andrew J. Peloquin ◽  
Arianna C. Ragusa ◽  
Colin D. McMillen ◽  
William T. Pennington
Keyword(s):  
Solid State ◽  
Halogen Bond ◽  
Bond Formation ◽  
Three Dimensional ◽  
Halogen Bonding ◽  
Donor Molecule ◽  
The Common

By varying the halogen-bond-donor molecule, 11 new halogen-bonding cocrystals involving thiourea or 1,3-dimethylthiourea were obtained, namely, 1,3-dimethylthiourea–1,2-diiodo-3,4,5,6-tetrafluorobenzene (1/1), C6F4I2·C3H8N2S, 1, thiourea–1,3-diiodo-2,4,5,6-tetrafluorobenzene (1/1), C6F4I2·CH4N2S, 2, 1,3-dimethylthiourea–1,3-diiodo-2,4,5,6-tetrafluorobenzene (1/1), C6F4I2·C3H8N2S, 3, 1,3-dimethylthiourea–1,3-diiodo-2,4,5,6-tetrafluorobenzene–methanol (1/1/1), C6F4I2·C3H8N2S·CH4O, 4, 1,3-dimethylthiourea–1,3-diiodo-2,4,5,6-tetrafluorobenzene–ethanol (1/1/1), C6F4I2·C3H8N2S·C2H6O, 5, 1,3-dimethylthiourea–1,4-diiodo-2,3,5,6-tetrafluorobenzene (1/1), C6F4I2·C3H8N2S, 6, 1,3-dimethylthiourea–1,3,5-trifluoro-2,4,6-triiodobenzene (1/1), C6F3I3·C3H8N2S, 7, 1,3-dimethylthiourea–1,1,2,2-tetraiodoethene (1/1), C6H16N4S2·C2I4, 8, [(dimethylamino)methylidene](1,2,2-triiodoethenyl)sulfonium iodide–1,1,2,2-tetraiodoethene–acetone (1/1/1), C5H8I3N2S+·I−·C3H6O·C2I4, 9, 2-amino-4-methyl-1,3-thiazol-3-ium iodide–1,1,2,2-tetraiodoethene (2/3), 2C4H7N2S+·2I−·3C2I4, 10, and 4,4-dimethyl-4H-1,3,5-thiadiazine-3,5-diium diiodide–1,1,2,2-tetraiodoethene (2/3), 2C5H12N4S2+·4I−·3C2I4, 11. When utilizing the common halogen-bond-donor molecules 1,2-, 1,3-, and 1,4-diiodotetrafluorobenzene, as well as 1,3,5-trifluoro-2,4,6-triiodobenzene, bifurcated I...S...I interactions were observed, resulting in the formation of isolated rings, chains, and sheets. Tetraiodoethylene (TIE) provided I...S...I cocrystals as well, but further yielded a sulfonium-containing product through the reaction of the S atom with TIE. This particular sulfonium motif is the first of its kind to be structurally characterized, and is stabilized in the solid state through a three-dimensional I...I halogen-bonding network. Thiourea reacted with acetone in the presence of TIE to provide two novel heterocyclic products, again stabilized in the solid state through I...I halogen bonding.

Si(Li) detector for microanalysis cooled by thermoelectric device

1992 ◽  
Vol 50 (2) ◽  
pp. 1736-1737
Author(s):  
Shaul Barkan
Keyword(s):  
Solid State ◽  
Liquid Nitrogen ◽  
Thermoelectric Device ◽  
Peltier Cooler ◽  
Complicated Process ◽  
The Common

Cooling down solid state detecors, with other different way then liquid Nitrogen, is a goal of many vendors and customers since the invention of these detectors. THe disadvantage of the common way of liquid Nitrogen is first the inavailibility of the LN in many uses (like space military and any other applications that are not done inside a well organize Laboratory). The use of LN also considers as a Labor consumer in addition to the big dewar that has to be added to any detector for storing the LN, the boiling of the LN, may cause microphonics problesm and the refiling of the dewar in many Labs is a complicated process due to inconvenience location of the microscope.In this paper I will show a spectra result of 10mm2 SiLi detector for microanalysis use, cooled by peltier cooler. The peltier cooler has the advantage of non-microphonics and non-labor needed (like adding LN to the dewar).

A Free Energy Perturbation Approach to Estimate the Intrinsic Solubilities of Drug-like Small Molecules

2019 ◽  
Author(s):  
Sayan Mondal ◽  
Gary Tresadern ◽  
Jeremy Greenwood ◽  
Byungchan Kim ◽  
Joe Kaus ◽  
...  
Keyword(s):  
Solid State ◽  
Small Molecules ◽  
Three Dimensional ◽  
Aqueous Solubility ◽  
Computational Approach ◽  
Free Energy Perturbation ◽  
Perturbation Approach ◽  
Energy Perturbation ◽  
State Form ◽  
Good Agreement

<p>Optimizing the solubility of small molecules is important in a wide variety of contexts, including in drug discovery where the optimization of aqueous solubility is often crucial to achieve oral bioavailability. In such a context, solubility optimization cannot be successfully pursued by indiscriminate increases in polarity, which would likely reduce permeability and potency. Moreover, increasing polarity may not even improve solubility itself in many cases, if it stabilizes the solid-state form. Here we present a novel physics-based approach to predict the solubility of small molecules, that takes into account three-dimensional solid-state characteristics in addition to polarity. The calculated solubilities are in good agreement with experimental solubilities taken both from the literature as well as from several active pharmaceutical discovery projects. This computational approach enables strategies to optimize solubility by disrupting the three-dimensional solid-state packing of novel chemical matter, illustrated here for an active medicinal chemistry campaign.</p>

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