Synthesis, Characterization and Crystal Structure of Palladium(II) Complexes Containing EDTA Tetraalkyl Ester Ligands

2007 ◽  
Vol 72 (4) ◽  
pp. 560-568 ◽  
Author(s):  
Goran N. Kaluđerović ◽  
Harry Schmidt ◽  
Christoph Wagner ◽  
Kurt Merzweiler ◽  
Dirk Steinborn
Keyword(s):  
Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Nitrogen Donor ◽  
C Nmr

The reaction of solutions of tetraalkyl ethylenediamine-N,N,N',N'-tetraacetate esters (alkyl = Me, 1a; Et, 1b) with H2[PdCl4] led to the complexes [PdCl2(R4EDTA)] (R = Me, 2a; Et, 2b). The coordination of R4EDTA ligands to palladium(II) ions occurs through the two nitrogen donor atoms, as confirmed by IR, 1H and 13C NMR spectroscopies and X-ray crystallography.

Triazene derivatives of (1,x-)diazacycloalkanes. Part VI. 3-({5,5-Dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines — Synthesis, characterization, and X-ray crystal structure

2006 ◽  
Vol 84 (10) ◽  
pp. 1294-1300 ◽  
Author(s):  
Keith Vaughan ◽  
Shasta Lee Moser ◽  
Reid Tingley ◽  
M Brad Peori ◽  
Valerio Bertolasi
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Ion Trapping ◽  
Published Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diazonium Ion ◽  
Derivatives Of ◽  
C Nmr

Reaction of a series of diazonium salts with a mixture of formaldehyde and 1,2-diamino-2-methylpropane affords the 3-({5,5-dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines (1a–1f) in excellent yield. The products have been characterized by IR and NMR spectroscopic analysis, elemental analysis, and X-ray crystallography. The X-ray crystal structure of the p-methoxycarbonyl derivative (1c) establishes without question the connectivity of these novel molecules, which can be described as linear bicyclic oligomers with two imidazolidinyl groups linked together by a one-carbon spacer. This is indeed a rare molecular building block. The molecular structure is corroborated by 1H and 13C NMR data, which correlates with the previously published data of compounds of types 5 and 6 derived from 1,3-propanediamine. The triazene moieties in the crystal of 1c display significant π conjugation, which gives the N—N bond a significant degree of double-bond character. This in turn causes restricted rotation around the N—N bond, which leads to considerable broadening of signals in both the 1H and 13C NMR spectra. The molecular ion of the p-cyanophenyl derivative (1b) was observed using electrospray mass spectrometry (ES + Na). The mechanism of formation of molecules of type 1 is proposed to involve diazonium ion trapping of the previously unreported bisimidazolidinyl methane (13).Key words: triazene, bistriazene, imidazolidine, synthesis, X-ray crystallography, NMR spectroscopy.

The crystal structure of Tetraisothiocyanatotetrakis(tetramethylurea)thorium(IV)

1980 ◽  
Vol 33 (5) ◽  
pp. 1161 ◽  
Author(s):  
CEF Rickard ◽  
DC Woollard
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Coordination Polyhedron ◽  
Title Complex ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Nitrogen Donor

The structure of the title complex has been determined by single- crystal X-ray crystallography. The crystals are monoclinic, a 13.954(1), b 20.334(2), c 14.138(1) Ǻ, β 98.06(3)°, space group P21/c. The structure was refined to a residual of 0.044 by using 3875 structure amplitudes. The molecules are eight-coordinate, the coordination polyhedron being a slightly distorted dodecahedron with the oxygen and nitrogen donor atoms equally distributed between the A and B sites.

Synthesis and Crystal Structure of Lead(II) Thenoyltrifluoroacetonate Complexes with Substituted 2,2' -Bipyridines: Interplay of Intermolecular Interactions in Crystals

2010 ◽  
Vol 65 (2) ◽  
pp. 128-134 ◽  
Author(s):  
Farzin Marandi ◽  
Zahra Nikpey ◽  
Jia Hao Goh ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Nmr Spectroscopy ◽  
Intermolecular Interactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Three substituted 2,2'-bipyridine adducts of lead(II) thenoyltrifluoroacetonate, [Pb(4,4'-dm-2,2’- bpy)(ttfa)2]2, 1, [Pb(5,5' -dm-2,2’-bpy)(ttfa)2]2, 2, and [Pb(4,4'-dmo-2,2’-bpy)(ttfa)2], 3, (4,4’ -dm- 2,2’-bpy, 5,5’-dm-2,2’-bpy, 4,4’-dmo-2,2’-bpy and ttfa are the abbreviations for 4,4’-dimethyl-, 5,5’-dimethyl-, and 4,4’-dimethoxy-2,2’-bipyridine, and thenoyltrifluoroacetonate, respectively) have been synthesized, characterized by elemental and thermal analysis, IR and 1H- and 13C-NMR spectroscopy, and studied by X-ray crystallography. The supramolecular features in these complexes are guided/controlled by weak directional intermolecular interactions.

2,2'-Bipyridine Mercury(II) Complexes [Hg(bpy)(NO2)X] (X = NO2 –, SCN– , CH3COO–); Π-Π Stacking In The Crystal Structure Of [Hg(bpy)(NO2)2]

2005 ◽  
Vol 60 (3) ◽  
pp. 289-293 ◽  
Author(s):  
Ali Ramazani ◽  
Ali Morsali ◽  
Leila Dolatyari ◽  
Bijan Ganjeie
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Aromatic Rings ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Coordinate Geometry ◽  
C Nmr

The mercury(II) complexes of 2,2′-bipyridine (bpy), [Hg(bpy)(NO2)2], [Hg(bpy)(NO2) (CH3COO)], and [Hg(bpy)(NO2)(NCS)] have been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The structure of [Hg(bpy)(NO2)2] has been confirmed by X-ray crystallography. The complex is a monomer and the Hg atom has an unsymmetrical six-coordinate geometry, formed by two nitrogen atoms of the bpy ligand and four oxygen atoms of the two nitrite anions. There is a short intermolecular π-π stacking interaction between parallel aromatic rings

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.

Negative hyperconjugation in hexachloro-3-cyclopentenylaminosulphenyl halides: Preparation and X-ray structure of C5Cl6NSBr and synthesis of C5Cl6NS+AsF6−

1991 ◽  
Vol 69 (6) ◽  
pp. 1022-1027 ◽  
Author(s):  
Allen Apblett ◽  
Tristram Chivers ◽  
James F. Fait ◽  
Rainer Vollmerhaus
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Good Yield ◽  
Variable Temperature ◽  
Triclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Compound C ◽  
Negative Hyperconjugation ◽  
C Nmr

The reaction of hexachlorocyclopentadiene with (NSCl)3 at 65 °C in the absence of a solvent produced hexachloro-3-cyclopentenylidenaminosulfenyl chloride, C5Cl6NSCl, in good yield. The derivatives C5Cl6NSX(X = Br, I, C5Cl6N, NPr2i, Ph) were prepared by treatment of C5Cl6NSCl with Me3SiBr, Me3SiI, Ph3Sb, iPr2NH, and Ph2Hg, respectively. The crystal structure of C5Cl6NSBr was determined by X-ray crystallography. Crystals of C5Cl6NSBr are triclinic, space group [Formula: see text] with a = 9.626(2), b = 9.810(2), c = 13.736(2) Å, α = 79.68(1), β = 88.62(1), γ = 74.73(1)°, Z = 4, final R and Rw values were0.075 and 0.063, respectively, for 4850 unique observed reflections. The > C=NSBr moiety adopts a syn conformation and there are two different molecules of C5Cl6NSBr in the asymmetric units. The bond lengths are d(C=N) = 1.278(8) and 1.253(8), d(N—S) = 1.560(6) and 1.569(6), and d(S—Br) = 2.229(2) and2.235(2) Å. The bond angles at nitrogen are 146.7(4) and 148.6(4) and those at sulfur are 116.8(2) and 116.5(2)°. The unusual geometry of the < C=NSBr moiety is explained in terms of negative hyperconjugation (nN → σSBr*). A variable temperature 13C NMR of C5Cl6NSCl provides evidence for a fiuxional process (ΔG*298 = 68.1 ± 1.2 kJ mol−1) in solution. The dark purple compound C5Cl6NS+AsF6− was synthesized from the reaction of C5Cl6NSCl and AgAsF6 in SO2. Key words: hexachloro-3-cyclopentenylidenamino sulfides, crystal structure, hexachloro-3-cyclopentenylidenaminosulfenyl bromide.

A topochemical rearrangement with multiple inversions of configuration

2001 ◽  
Vol 79 (8) ◽  
pp. 1272-1277 ◽  
Author(s):  
Saul Wolfe ◽  
Yih-Huang Hsieh ◽  
Raymond J Batchelor ◽  
Frederick WB Einstein ◽  
Ian D Gay
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Room Temperature ◽  
The Other ◽  
X Ray ◽  
Controlled Processes ◽  
X Ray Crystallography ◽  
Intramolecular Process ◽  
C Nmr ◽  
The Ideal

Crystalline 2-benzyloxypyridine-1-oxide rearranges slowly at room temperature to crystalline 1-benzyloxy-2-pyridone. No intermediates are detected when the process is followed by solid-state 13C NMR. The crystal structure of the pyridine-1-oxide strongly suggests that a topochemically controlled intramolecular process, in which the benzyl group migrates with retention of configuration, is not feasible. On the other hand, although somewhat disfavoured by initial solid-state O···C···O angles significantly less than the ideal 180°, intermolecular topochemically controlled processes can be envisaged that lead, with multiple inversions of configuration, either to net retention of configuration or to net inversion of configuration in the benzyl group. In contrast to the 50–80% inversion observed in solution, in the solid state only inversion is observed experimentally when chirally labelled α-deuteriobenzyloxypyridine-1-oxide is allowed to rearrange.Key words: X-ray crystallography, solid-state 13C NMR, benzyl-α-D-alcohol, 2-benzyloxypyridine-1-oxide, 1-benzyloxy-2-pyridone.

Crystal and solution structure of (E)-1,2-bis(ethylsulphonyl)cyclobutane-1,2-dicarbonitrile

1989 ◽  
Vol 54 (12) ◽  
pp. 3253-3259
Author(s):  
Jaroslav Podlaha ◽  
Miloš Buděšínský ◽  
Jana Podlahová ◽  
Jindřich Hašek
Keyword(s):  
Hydrogen Peroxide ◽  
Solution Structure ◽  
Peroxide Oxidation ◽  
X Ray ◽  
X Ray Crystallography ◽  
Nmr Study ◽  
Hydrogen Peroxide Oxidation ◽  
Unusual Product ◽  
C Nmr

The unusual product of the reaction of 2-chloroacrylonitrile with ethane thiol and following hydrogen peroxide oxidation was found to be (E)-1,2-bis(ethylsulphonyl)cyclobutane-1,2-dicarbonitrile by means of X-ray crystallography. 1H and 13C NMR study of this compound has proven the same conformation of the molecule in solution.

Darstellung, 11B-, 13C-, 29Si-NMR- und Schwingungsspektren von Trimethylsilylmethyl-hexahydro-closo-hexaborat, [B6H6(CH2Si(CH3)3)]- sowie Kristallstruktur von [P(C6H5)4][B6H6(CH2Si(CH3)3)] / Preparation, 11B, 13C, 29Si NMR and Vibrational Spectra of Trimethylsilylmethyl-hexahydro-clo-hexaborate, [B6H6(CH2Si(CH 3)3)]-and the Crystal Structure of [P(C6H5)4] [B6H6(CH2Si(CH3)3)]

1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
29Si Nmr ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Stretching Vibration ◽  
Ir And Raman ◽  
C Nmr

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.

Verfeinerung der Kristallstruktur von Tripalladium-di-tetrathiophospliat Pd3(PS4)2 Refinement of the Crystal Structure of Tripalladium-di-tetrathiophosphate Pda3(PS4)2

1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Type Structure ◽  
Tetrahedral Symmetry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Planar Environment

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.

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