The electrochemical synthesis of β-diketonato complexes of cadmium(II), and their adducts; the crystal and molecular structure of Cd(acac)2phen

1983 ◽  
Vol 61 (9) ◽  
pp. 2141-2146 ◽  
Author(s):  
Luis Bustos ◽  
James H. Green ◽  
J. Lawrence Hencher ◽  
Masood A. Khan ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Good Yield ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Electrolytic Solution ◽  
X Ray ◽  
Subsequent Addition

The cadmium β-diketonate complexes Cd(RCOCHCOR′)2 (R = CH3, R′ = CH3; R = CF3 R′ = CH3, i-C3H7, i-C4H9, t-C4H9, C6H5, 2-naphthyl) can be prepared in good yield by the direct room temperature electrochemical oxidation of the metal into a solution of the parent diketone in acetonitrile. Adducts of the type Cd(RCOCHCOR′)2L (L = 2,2′-bipyridine, 1,10-phenanthroline, N,N,N′,N′-tetramethylethylenediamine) can be prepared insitu, or by subsequent addition of the ligand to the electrolytic solution. X-ray studies show that the molecular structure of both Cd(acac)2phen and Cd(CF3COCHCOC6H5)2phen is based on a CdO4N2 kernel, distorted from octahedral stereochemistry by the bite of the ligands.

Spaltung von S4N4 zu S2N2 bei Raumtemperatur: Darstellung und Struktur von S2N2 • 2AlBr3 / Cleavage of S4N4 to S2N2 at Room Tem perature: Preparation and Structure of S2N2 • 2AlBr3

1984 ◽  
Vol 39 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl
Keyword(s):  
Molecular Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

The compound S2N2 • 2AlBr3 has been prepared by reaction of S4N4 with AlBr3 in 1,2-dibromoethane at room temperature. Its crystal and molecular structure have been determined by X-ray diffraction; R = 0.068. Crystal data: monoclinic, P 21/n, a = 9.594(5), b = 9.975(4), c = 7.528(4) Å , β = 111.36(5)°. The S2N2 ring of the centrosymmetrical complex is bonded via its nitrogen atoms to two AlBr3 units thus completing coordination tetrahedra around the Al atoms. Bond distances and angles within the S2N2 ring are d(S-N) = 1.629(13) and 1.651(13) Å, ∢ (S-N-S) = 95.8, and ∢ (N-S-N) - 84.2°. Whereas the S-N bond lengths agree closely with those of free S2N2, the angle at N is enlarged by ca. 5° and the angle at S is decreased by ca. 5°. The sulfur atoms form two close S···Br contacts of length 3.149 (intramolecular) and 3.193 (intermolecular) Å , respectively. The intermolecular attractive nonbonded S···Br interactions tie the complexes together in a way that leads to infinite chains which run parallel to the crystallographic z axis

Synthesis and Crystal and Molecular Structure of trans-Dichloro(ethanedial dioximato(1—)-N,N')(ethanedial dioxime-N,N')rhodium(III)

1989 ◽  
Vol 44 (1) ◽  
pp. 5-8
Author(s):  
Michel Mégnamisi-Bélombé
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystallographic Direction ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cl Atoms

Abstract trans-Dichloro(ethanedial-dioximato)(ethanediaI-dioxime)rhodium (III), RhCl2(GH)(GH2), has been synthesized and its structure determined by single crystal X-ray diffraction at room temperature. C4H7Cl2N4O4Rh, Mr = 348.94. monoclinic space group P21/ɑ; a = 10.543(3), b = 8.363(2), c = 11.512(3)Å ; β = 92.79(2)°; V = 1024Å3; Z = 4; Dc = 2.26 Mg m-3. Final Rw = 0.075 for 2035 reflections and 139 parameters. The coordination geometry around Rh is a dis­torted (4+2) octahedron, with four chelating N atoms lying in the equatorial plane and the two Cl atoms in the apical positions. The H atoms of the oxime groups are involved in relatively weak intramolecular O-H-O bridgings, as well as in very strong intermolecular bridgings which extend throughout the crystal structure and propagate nearly parallel to the [101] crystallographic direction.

Crystal and Molecular Structure of Di-μ-phenoxido-bis-[N-{(2-hydroxybenzyl)-(S)-alaninato-κ3-O,O',N}copper(II)]. A Simple Homodimetallic Model for N-terminal Tyrosine Coordination with (S)-Alanine as a Second Amino Acid Residue

1998 ◽  
Vol 63 (3) ◽  
pp. 356-362 ◽  
Author(s):  
Svetlana Pakhomova ◽  
Jan Ondráček ◽  
František Jursík
Keyword(s):  
Molecular Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Carbonyl Oxygen ◽  
Antiferromagnetic Coupling ◽  
X Ray Diffraction ◽  
Apical Position ◽  
X Ray ◽  
Pyramidal Geometry ◽  
Square Pyramidal Geometry

Single-crystal X-ray diffraction study established the dimeric [Cu2(ohb-(S)-Ala)2] structure (ohb-(S)-Ala = N-(2-hydroxybenzyl-(S)-alaninate). The complex crystallizes in the tetragonal space group P43212 with a = b = 8.849(1) Å, c = 24.913(2) Å, V = 1950.8(3) Å3, Z = 8. The Cu(II) ion has distorted square-pyramidal geometry with the equatorial positions occupied by three oxygen and one nitrogen atom. Each copper atom is weakly coordinated at the apical position by carbonyl oxygen atom of the neighbouring molecule at the distance 2.329(2) Å. The Cu-Cu separation 3.0204(7) Å and the Cu-O3-Cu angle 100.8(1)° lead to antiferromagnetic coupling (at room temperature μeff = 1.35 μB). The O1-Cu-O3 angle (154.9(1)°) indicates distortion of the square pyramid toward a trigonal bipyramid (t = 0.23).

Die Kristall- und Molekülstruktur von Tris(dimethylamino)boran / The Crystal and Molecular Structure of Tris(dimethylamino)borane

1982 ◽  
Vol 37 (10) ◽  
pp. 1230-1233 ◽  
Author(s):  
Günter Schmid ◽  
Roland Boese ◽  
Dieter Bläser
Keyword(s):  
Molecular Structure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Melting Process ◽  
Single Crystal Growth ◽  
Zone Melting ◽  
X Ray Diffraction ◽  
X Ray

Abstract Tris(dimethylamino)borane, X-ray The crystal and molecular structure of tris(dimethylamino)borane, a liquid at room temperature, has been determined by single-crystal X-ray diffraction methods at - 116°C. The single-crystal growth was accomplished by means of a miniature zone melting process on the diffractometer. The structure data are compared with those of other aminoboranes.

Anion Effects on the Structural Properties of Bis(triphenylphosphine)copper(I) Carboxylate Complexes, [(PPh3)2CuO2CR]

1998 ◽  
Vol 51 (1) ◽  
pp. 67 ◽  
Author(s):  
Robert D. Hart ◽  
Peter C. Healy ◽  
Michelle L. Peake ◽  
Allan H. White
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Structural Properties ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Nitrate Complex ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Anion Coordination

The crystal and molecular structure of the 2 : 1 triphenylphosphine copper(I) benzoate complex [(PPh3)2CuO2CC6H5] have been determined by a room-temperature single-crystal X-ray study. The complex is isomorphous with the dithiobenzoate analogue, crystallizing in the orthorhombic space group P212121 with a 20·094(5), b 16·929(9), c 10·659(8) Å, Z 4; conventional R on |F| was 0·039 for 4261 independent ‘observed’ (I > 3σ(I)) reflections. Comparison of structural data for this and other [(PPh3)2CuO2CR] complexes shows that the P–Cu–P angle and the anion coordination are dependent on both the donor strength of the anion and on steric interactions between the anion and the triphenylphosphine ligands. The structure of the analogous nitrate complex [(PPh3)2CuNO3] has also been redetermined.

The crystal and molecular structure of tris(pentamethylenedithiocarbamate) chromium(III)-chloroform (1 : 2)

1981 ◽  
Vol 46 (1) ◽  
pp. 6-19 ◽  
Author(s):  
Viktor Kettman ◽  
Ján Garaj ◽  
Jaroslav Majer
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Complex Molecules ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Cell Dimensions ◽  
Crustal Density ◽  
Unit Cell Dimensions

The crystal and molecular structure of [Cr(S2CN(CH2)5)3].2 CHCl3 was found by the X-ray structural analysis method. The value R 0.090 was found for 1 131 observed independent reflections. The substance crystallizes in a space group of symmetry P212121 with the following unit cell dimensions: a = 0.8675 (6), b = 1.815(2), c = 2.155(3) nm. The experimentally observed crustal density was 1.48 Mgm-3 and the value calculated for Z = 4 was 1.51 Mgm-3. The CrS6 coordination polyhedron has the shape of a trigonally distorted octahedron, where the D3 symmetry is a approximately retained. The degree of trigonal distortion expressed as the projection of the chelate S-Cr-S angle onto the plane perpendicular to the C3 pseudo axis is Φ = 41.7° (Φ = 60° for an octahedron). The skeleton of the structure formed by the complex molecules contains channels filled with chloroform molecules. The specific type of complex-chloroform interaction consists of the formation of hydrogen bonds of the chloroform protons with the fully occupied pπ-orbitals of the sulphur atoms in the coordination polyhedra. The low stability and crystal decomposition can be explained by loss of chloroform from the channels.

scholarly journals Structural Characterization of Heterodinuclear ZnII-LnIII Complexes (Ln = Pr, Nd) with a Ring-Contracted H2valdien-Derived Schiff Base Ligand

2021 ◽  
Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Structural Characterization ◽  
Schiff Base Ligand ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Imidazoline Ring

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

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