Spectroscopic studies of triphenyltin azide and of its adducts with O- and N-donor ligands; the crystal and molecular structures of triphenyltin azide and of azido(hexamethylphosphoramide)triphenyltin(IV)

1998 ◽  
Vol 76 (12) ◽  
pp. 1827-1835 ◽  
Author(s):  
Ivor Wharf ◽  
Ryszard Wojtowski ◽  
Carol Bowes ◽  
Anne-Marie Lebuis ◽  
Mario Onyszchuk
Keyword(s):  
Solid State ◽  
Spectroscopic Studies ◽  
Triphenylphosphine Oxide ◽  
Molecular Structures ◽  
The Other ◽  
Donor Ligands ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Nmr Data ◽  
Ir And Raman

Complete far-IR and Raman data (<400 cm-1) are reported for triphenyltin azide (1) as well as for adducts Ph3SnN3·L (L = hexamethylphosphoramide (HMPA), triphenylphosphine oxide, pyridine-N-oxide, 4-picoline-N-oxide, or pyridine). The small changes in v(Sn-N3) noted on going from (1) to the adducts, as well as solid-state 119Sn nmr data, indicate that (1), like the adducts, has five-coordinate tin atoms. X-ray analysis shows that (1) crystallizes with two different chains of five-coordinate Ph3Sn units joined by 1,3-azide bridges. In one unit, the geometry around tin is similar to that found for the monomeric HMPA adduct (2), which has trans-axial HMPA and azide ligands. The other unit in (1) has nonplanar -SnC3- groups connected by less symmetric 1,3-azide bridges and thus resembles the structure of isoelectronic triphenyltin isocyanate.Key words: triphenyltin azide, O- and N-donor adducts, far-IR/Raman, crystal structures.

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

Experimental and computational structural study of two hindered aminoanthraquinones in crystals and solutions

2000 ◽  
Vol 215 (9) ◽  
Author(s):  
A.V. Yatsenko ◽  
K.A. Paseshnichenko ◽  
S.I. Popov
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Electronic Spectra ◽  
Molecular Structures ◽  
Amino Group ◽  
Single Crystal Diffraction ◽  
Molecular Conformations ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Visible Spectra

The crystal and molecular structures of 2-methyl-1-methylamino-anthraquinone (I) and 1-methylphenylamino-anthraquinone (II) were studied by the X-ray single-crystal diffraction and the visible spectra of crystalline specimens and their solutions were recorded. The molecule I is closely planar, whereas in the molecule II the amino group is 58° rotated out of the plane of the anthraquinone skeleton. In both structures the molecules pack in stacks. The comparison of experimental and calculated (on the DFT and AM1 levels) molecular structures, together with the comparison of experimental and INDO/S-calculated electronic spectra, give the evidence that molecular conformations (especially for II) change upon transfer from the solid state to solutions, and the π-delocalisation throughout the whole molecule enhances in the solid state.

Tetra(alkynyl)silanes, a 3,6-Disila-triyne, a 3,6,9-Trisila-tetrayne, a 1,3,4,6-Tetrasiladiyne, and Bis(trimethylstannyl)ethyne. Molecular Structures and Solid-state NMR Studies

2010 ◽  
Vol 65 (2) ◽  
pp. 119-127 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Ezzat Khan ◽  
Amin Badshah ◽  
Elias Molla ◽  
Peter Thoma ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Mas Nmr ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Solution State ◽  
Nmr Data

The molecular structures of three alkynylsilanes, tetrakis(ethynyl-p-tolyl)silane, 3,3,6,6,-tetramethyl- 3,6-disila-triyne, 3,3,6,6,9,9,-hexamethyl-3,6,9-trisila-tetrayne, and of bis(trimethylstannyl)- ethyne have been determined by X-ray diffraction. The same alkynylsilanes, and in addition 1,2- bis(trimethylsilylethynyl)-1,1,2,2-tetramethyldisliane, were studied by solid-state 13C and 29Si MAS NMR spectroscopy. The results of these measurements were compared with crystallographic evidence and also with relevant solution-state NMR data.

scholarly journals Transition metal complexes with pyrazole based ligands, part 27: Structural and thermal characterization of cobalt(II) halide and pseudohalide complexes with 4-acetyl-3-amino-5-methylpyrazole

2007 ◽  
Vol 72 (12) ◽  
pp. 1281-1293 ◽  
Author(s):  
Vukadin Leovac ◽  
Zoran Tomic ◽  
Katalin Mészáros-Szécsényi ◽  
Ljiljana Jovanovic ◽  
Milan Joksovic
Keyword(s):  
Thermal Decomposition ◽  
Solid State ◽  
Transition Metal Complexes ◽  
Thermal Characterization ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Vis Spectroscopy

The crystal and molecular structures of four tetrahedral structurally similar [Co(aamp)2X2] complexes (aamp = 4-acetyl-3-amino-5-methylpyrazole, X = Cl, Br, I and NCS) were determined by X-ray diffraction analysis and are discussed in detail. It was found that the different capacity of the ligand X (NCS vs. Cl, Br, I) for the formation of non-bonding contacts influence the mode of molecular association in the solid state. The complexes were characterized by UV-Vis spectroscopy. The first step of the thermal decomposition of the compounds was checked and is discussed in the view of the IR spectrum of the intermediate isolated from [Co(aamp)2Br2] by the quasi-isothermal technique.

Preparative and Vibrational Spectroscopic Studies of Anilinium Salts Containing the [Hg2Cl6]2-, [Hg2Cl4X2]2-, [CdHgI6]2-, [CdHgI4Br2]2- and [CdHgBr4I2]2- Ions (X = Br, I)

1991 ◽  
Vol 46 (11) ◽  
pp. 1532-1538 ◽  
Author(s):  
Theodoros F. Zafiropoulos ◽  
John C. Plakatouras ◽  
S. P. Perlepes
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Raman Spectra ◽  
Spectroscopic Studies ◽  
Ir And Raman Spectra ◽  
X Ray ◽  
Ir And Raman ◽  
Complex Anions

Synthetic procedures are described that allow access to anilinium salts containing the complex anions [Hg2Cl62-, [Hg2Cl4X2]2- (X = Br, I), [CdHgI6]2-, [CdHgI4Br2]2- and [CdHgBr4I2]2--. Isolated dimeric structures are proposed for the new complexes in the solid state, using X-ray powder patterns, Far-IR and Raman spectra. The spectral detail is greatly enhanced in measurements at low temperature (∼100 K).

Bridged calix[4]arenes; X-ray crystal and molecular structures and spectroscopic studies

1990 ◽  
pp. 1769-1775 ◽  
Author(s):  
Volker Böhmer ◽  
Helmut Goldmann ◽  
Walter Vogt ◽  
Erich F. Paulus ◽  
Fred L. Tobiason ◽  
...  
Keyword(s):  
Spectroscopic Studies ◽  
Molecular Structures ◽  
X Ray ◽  
Crystal And Molecular Structures

Crystal and Molecular Structures of Penta-O-acetyl-aldehydo-D-glucose Dimethyl Acetal and of Hepta-O-acetyl-aldehydo-D-glucose Hydrate

1996 ◽  
Vol 49 (3) ◽  
pp. 391 ◽  
Author(s):  
P Koll ◽  
J Kopf
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Dimethyl Acetal ◽  
Molecular Structures ◽  
Carbon Skeleton ◽  
Parallel Orientation ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Solid State Structures

The solid-state structures of the title compounds were determined by conventional single-crystal X-ray crystallography. In both cases a planar zigzag conformation of the carbon skeleton is observed with a resulting 1,3-parallel orientation of O(2) and O(4). In the case of the heptaacetate even a second such arrangement is established between O(3) and one of the oxygens at C(1). These findings substantiate the claim that such conformations are not as unfavourable as previously was assumed by many authors.

Substituent Effects and Structure in Substituted Dibenzonaphthyrones

1985 ◽  
Vol 38 (1) ◽  
pp. 97
Author(s):  
H Becker ◽  
CL Raston ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Double Bond ◽  
Substituent Effects ◽  
Molecular Geometry ◽  
Molecular Structures ◽  
The Other ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of [1]benzopyrano[4,3- c][1]benzopyran-5,11-done (dibenzo-naphthyrone) and three of its symmetrically tetrasubstituted derivatives have been determined by single-crystal X-ray diffraction methods. Only the tetra-t-butyl-substituted dibenzonaphthyrone was found to deviate significantly from planarity by having the two carbonyl groups folded and 'syn'-oriented relative to the plane of the connecting ethylene double bond. The dihedral angle between the two aromatic rings was found to be 25. The molecular geometry of all the other dibenzo-naphthyrones in their crystalline states is characterized by planarity, and their structures are centrosymmetric.

Xenon Trioxide Adducts of O-Donor Ligands; [(CH3)2CO]3XeO3, [(CH3)2SO]3(XeO3)2, (C5H5NO)3(XeO3)2, and [(C6H5)3PO]2XeO3

2018 ◽  
Author(s):  
Katherine Marczenko ◽  
James Goettel ◽  
Gary Schrobilgen
Keyword(s):  
Room Temperature ◽  
Triphenylphosphine Oxide ◽  
Donor Ligands ◽  
Mechanical Shock ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Coordination ◽  
Xenon Trioxide ◽  
Distorted Octahedra ◽  
Coordination Spheres

Oxygen coordination to the Xe(VI) atom of XeO<sub>3</sub> was observed in its adducts with triphenylphosphine oxide, dimethylsulfoxide, pyridine-N-oxide, and acetone. The crystalline adducts were characterized by low-temperature, single-crystal X-ray diffraction and Raman spectroscopy. Unlike solid XeO<sub>3</sub>, which detonates when mechanically or thermally shocked, the solid [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub>, [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub>,<sub> </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> adducts are insensitive to mechanical shock, but undergo rapid deflagration when ignited by a flame. Both [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3 </sub>and (C<sub>5</sub>H<sub>5</sub>NO)<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> are air-stable whereas [(CH<sub>3</sub>)<sub>2</sub>SO]<sub>3</sub>(XeO<sub>3</sub>)<sub>2</sub> slowly decomposes over several days and [(CH<sub>3</sub>)<sub>2</sub>CO]<sub>3</sub>XeO<sub>3</sub> undergoes adduct dissociation at room temperature. The xenon coordination sphere of [(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>PO]<sub>2</sub>XeO<sub>3</sub> is a distorted square pyramid which provides the first example of a five-coordinate XeO<sub>3</sub> adduct. The xenon coordination spheres of the remaining adducts are distorted octahedra comprised of three Xe---O secondary contacts that are approximately trans to the primary Xe–O bonds of XeO<sub>3</sub>. Quantum-chemical calculations were used to assess the Xe---O adduct bonds, which are predominantly electrostatic σ-hole bonds between the nucleophilic oxygen atoms of the bases and the σ-holes of the xenon atoms.

Structural and spectroscopic studies of transition metal nitrite complexes. VIII. Crystal structures and spectra of three pentanuclear species with stoichiometry [Ni5(N-substituted ethane-1,2-diamine)4(OH)2(NO2)8]

1981 ◽  
Vol 34 (10) ◽  
pp. 2139 ◽  
Author(s):  
AJ Finney ◽  
MA Hitchman ◽  
CL Raston ◽  
GL Rowbottom ◽  
AH White
Keyword(s):  
Transition Metal ◽  
Crystal Structures ◽  
General Formula ◽  
Infrared Spectra ◽  
Spectroscopic Studies ◽  
Molecular Structures ◽  
Structural Variations ◽  
Crystal And Molecular Structures

The preparation of a series of novel compounds of general formula [Ni5L4(NO2)8(OH)2] formed by ethane-1,2-diamine or one of five N-substituted ethane-1,2-diamines (L) is described. The crystal and molecular structures of the ethane-1,2-diamine, N,N'-diethylethane-1,2-diamine and N,N-dimethylethane-1,2-diamine complexes are reported. Each compound contains a planar, pentameric arrangement of nickel(II) ions, linked by bridging hydroxide and nitrite ligands. The details of the nitrite bridges differ among the complexes, causing differences in their electronic and infrared spectra. The structural variations are probably caused by the differing steric requirements of the amine substituents.

Sign in / Sign up

Export Citation Format

Share Document