Nuclear magnetic resonance studies on the anions [M(SnCl3)5Cl]4− (M = Ru, Os) and [Ru(SnCl3)5(MeCN)]3−: the X-ray crystal structure of [N(C2H5)4]4[Ru(SnCl3)5Cl]

1982 ◽  
Vol 60 (11) ◽  
pp. 1304-1316 ◽  
Author(s):  
Louis J. Farrugia ◽  
Brian R. James ◽  
Claude R. Lassigne ◽  
Edward J. Wells
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Octahedral Geometry ◽  
Coupling Constants ◽  
Order Effects ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Crystallographic Study

The octahedral anions [M(SnCl3)5Cl]4− (M = Ru, Os) have been fully characterized by 119Sn FT nmr spectroscopy. For M = Ru, 117Sn and 115Sn nmr spectra were also recorded, and an X-ray crystallographic study was carried out on the tetraethylammonium salt, isolated as a disolvate from acetonitrile. The Ru—Sn bond lengths indicate some degree of dπ–dπ interactions. The slight distortions from octahedral geometry are discussed in connection with the packing of the chlorine atoms. The Sn nmr spectra reveal the first observed coupling to a 99Ru nucleus (I = 5/2, 12.7% natural abundance), very large 2J(119Sn—117Sn) coupling constants, and the first observed second-order effects on a heteronuclear system. The octahedral anion [Ru(SnCl3)5(MeCN)]3− was also synthesized as the tetraethylammonium salt and characterized spectroscopically.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

sHigh resolution 1H nuclear magnetic resonance studies of a flavine and its product with MoCl4

1977 ◽  
Vol 55 (4) ◽  
pp. 575-582 ◽  
Author(s):  
T. Roberie ◽  
N. S. Bhacca ◽  
J. Selbin
Keyword(s):  
Aqueous Solution ◽  
Nuclear Magnetic Resonance ◽  
Binding Sites ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
Side Chain ◽  
Magnetic Resonance Studies ◽  
H Nmr ◽  
Metal Atoms ◽  
1H Nuclear Magnetic Resonance

The high resolution 1H nmr spectra of the substituted flavine, 3-N-methyltetraacetylriboflavine (3-Me-TARF), and its non-aqueous solution complexes with Gd(fod)3, Eu(fod)3, MoCl4, and MoCl4•2CH3(CH2)2CN, were studied in order to try to discern the binding sites of the flavine as it attaches to the molybdenum. Evidence was found that all three metal atoms, Gd(III), Eu(III), and Mo(IV), are attached in solution not only by the primary binding (chelating) sites of the flavine, viz., the O-4 and N-5 atoms, but also by an acetyl oxygen atom, at the C-4′ site of the ribityl side chain. 300 MHz spectra of the 3-Me-TARF have permitted the coupling constants for the side chain methine and methylene protons to be obtained.

Metal Tetrahydroborates and Tetrahydroborato Metalates, 15 [1]. An 11B and 113Cd NMR Study of MBH4–CdCl2 Systems in Dimethylformamide and the X-Ray Structure of CdCl2 · 2 DMF

1990 ◽  
Vol 45 (11) ◽  
pp. 1463-1471 ◽  
Author(s):  
Gerald Linti ◽  
Heinrich Nöth ◽  
Martina Thomann
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Coordination Polymer ◽  
Ambient Temperature ◽  
Nmr Spectra ◽  
Carbonyl Oxygen ◽  
X Ray ◽  
Rapid Exchange ◽  
Nmr Study ◽  
In Cis

CdCl2 dissociates in dimethylformamide into the species Cd(DMF)62+, CdCl(DMF)5+ and CdCl3- as determined by 113Cd NMR spectroscopy. 11B and 113Cd NMR spectra of MBH4/CdCl2 solutions in this solvent show the presence of complexes [CdCl2-n(BH4)n+1]- with rapid exchange of BH4- and Cl- at ambient temperature. There is no evidence that Cd(BH4)2 is formed in a metathetical reaction.The crystal structure of CdCl2 · 2 DMF has been determined. It is a coordination polymer containing hexacoordinated Cd atoms with the DMF molecules in cis-position. Coordination of DMF occurs via the carbonyl oxygen atoms.

scholarly journals Palladium(II) complexes with R2edda derived ligands, Part III: Diisobutyl (s,s)-2,2'-(1,2-ethanediyldiimino)di(4-methylpentanoate) and its palladium(II) complex: Synthesis and characterization

2009 ◽  
Vol 74 (11) ◽  
pp. 1249-1258 ◽  
Author(s):  
Bojana Zmejkovski ◽  
Goran Kaludjerovic ◽  
Santiago Gómez-Ruiz ◽  
Tibor Sabo
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Nmr Spectra ◽  
Symmetry Axis ◽  
Layer Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

A new R2edda-type ester, diisobutyl (S,S)-2,2'-(1,2-ethane-diyldiimino) di(4-methylpentanoate) dihydrochloride, [(S,S)-H2iBu2eddl]Cl2, 1, and its palladium(II) complex, dichloro(diisobutyl (S,S)-2,2'-(1,2-ethanediyldiimino) di(4-methylpentanoate))palladium(II), [PdCl2{(S,S)-iBu2eddl}], 2, were synthesized and characterized by elemental analysis, as well as IR and NMR spectroscopy. It was found that complex 2 was obtained as mixture of two diastereoisomers, observed in NMR spectra. The crystal structure of compound 1 was determined by X-ray diffraction studies and is described. The isolated crystals consisted of one dicationic species [(S,S)-H2iBu2eddl]2+ and two Cl-. The crystal system was tetragonal with the space group P42. Hydrogen bonds significant for the manner of packing are N-H1N???Cl, 3.049(3) ?, 159(3)? and N-H2N???Cl, 3.100(3) ?, 164(3)?. An infinite chain was formed building a one layer structure, usual for these types of compounds. The C2 symmetry axis of the compound passes through the C1-C1i bond vector and lies perpendicular to the plane N2Cl2.

15N and 77Se Nuclear Magnetic Resonance Study of Selenium Diimides and Aminoselenanes

1993 ◽  
Vol 48 (10) ◽  
pp. 1307-1314 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Berthold Distler ◽  
Silke Gerstmann ◽  
Max Herberhold
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectra ◽  
Decomposition Product ◽  
Nuclear Magnetic Resonance Study ◽  
Coupling Constants ◽  
Magnetic Resonance Study ◽  
Nmr Data ◽  
Cp Mas Nmr ◽  
Membered Heterocycle

Selenium diimides R(NSeN)R [R = tBu (1a), tOct (1b)], the eight-membered heterocycle tBuN(SeSeSe)2NtBu (2) and the aminoselenanes of the type [R(Cl3Si)N]2Se (4a,b) and [(Me3Si)2N]2Se (5) were studied by multinuclear NMR with emphasis on 15N NMR for detection of coupling constants J(77Se15N). The selenium diimides possess the largest values of 1J(77Se15N) observed so far (1a: 158.4 and 163.5 Hz; 1 b: 158.6 and 162.8 Hz). Compound 1 b was found to be much more stable than 1a, the heterocycle 2 being the major decomposition product of 1a. The selenium diimides (1a,b) react readily with hexachlorodisilane to give the bis[alkyl(trichlorosilyl)amino]selenanes 4a,b. The solid state 13C, 15N, 29Si and 77Se CP/MAS NMR spectra of bis[bis(trimethylsilyl)amino]selenane (5) gave results in accord with the known crystal structure, and there is agreement with the solution state NMR data

Structural and spectral study of coordination of 4,4′-dimethoxy-2,2′-bipyridine toward Zn(II) and Cd(II) containing thiocyanato or azido ligands

2016 ◽  
Vol 71 (9) ◽  
pp. 959-965 ◽  
Author(s):  
Farzin Marandi ◽  
Keyvan Moeini ◽  
Hadi Amiri Rudbari
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
New Compounds ◽  
C Nmr

AbstractThree new compounds of zinc(II) and cadmium(II) with the ligand 4,4′-dimethoxy-2,2′-bipyridine (4,4′-dmo-2,2′-bpy), including cis-[Zn(4,4′-dmo-2,2′-bpy)2(SCN)2] (1), cis-[Cd(4,4′-dmo-2,2′-bpy)2(SCN)2] (2), and [Cd3(4,4′-dmo-2,2′-bpy)3(N3)5(OAc)]n (3), have been obtained as white single crystals by the branched tube method and characterized by elemental analysis, FT-IR and 1H, 13C NMR spectroscopy, and X-ray crystallography. Single-crystal structure analyses of the isostructural complexes 1 and 2 showed distorted octahedral geometry for zinc(II) and cadmium(II) with ZnN6 and CdN6 environments. Complex 3 reveals a rare coordination polymer containing octahedrally coordinated cadmium(II) expanding to chains by two different bridging modes, including Cd‒O‒C‒O‒Cd and Cd‒N‒Cd.

Sign in / Sign up

Export Citation Format

Share Document