Synthesis, characterization, and X-ray structural analysis of the Cu(I) derivative, [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu• PPh3

1981 ◽  
Vol 59 (3) ◽  
pp. 518-523 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Structural Analysis ◽  
Copper Atom ◽  
Direct Methods ◽  
Carbonyl Complex ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Full Matrix ◽  
X Ray ◽  
Complex Crystals ◽  
Distorted Tetrahedral Coordination

The Cu(I) complex [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu•PPh3 has been synthesized and its fluxional behavior in solution probed. Attempts have been made to isolate the analogous Cu(I) carbonyl complex. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl)(N,N-dimethylethanolamino)gallato (N(2),O,N(3))](triphenylphosphine)copper(I) are monoclinic, a = 18.871(2), b = 9.464(1), c = 18.374(2) Ā, β = 109.62(1)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.028 and Rw = 0.035 for 2729 reflections with I ≥ 3σ(I). The copper atom is bonded to the phosphine and to the tridentate Me2Ga(OCH2CH2NMe2)N2C5H7− ligand resulting in a distorted tetrahedral coordination geometry. The Cu—P distance of 2.156(1) Å is unusually short. Other important bond distances (corrected for libration) are: Cu—O, 2.163(2), Cu—N(pyrazolyl), 2.025(3), Cu—N(amino), 2.144(3), Ga—O, 1.896(3), Ga—N, 2.005(3), and Ga—C, 1.972(5) and 1.987(5) Å.

Crystal and molecular structure of bis[methyltris(1-pyrazolyl)gallato]nickel(II)

1979 ◽  
Vol 57 (14) ◽  
pp. 1823-1825 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Nickel Atom ◽  
Exact Formula ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Gallium Atom ◽  
Full Matrix ◽  
Distorted Tetrahedral Coordination

Crystals of bis[methyltris(1-pyrazolyl)gallato]nickel(II) are rhombohedral, a = 9.6670(5), c = 23.893(1) Å, Z = 3, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.030 and Rw = 0.035 for 925 reflections with I ≥ 3σ (I). The crystal structure consists of well separated molecules of [MeGa-(N2C3H3)3]2Ni having exact [Formula: see text] (S6) symmetry and approximate D3d symmetry. The coordination geometry about the nickel atom is octahedral with Ni—N = 2.109(2) Å, N—Ni—N = 90.65(6) and 89.35(6)°. The gallium atom has distorted tetrahedral coordination geometry with Ga—N = 1.939(2), Ga—C = 1.940(4) Å, N—Ga—N = 99.55(6), and N—Ga—C = 118.16(5)°.

N,N-Ethylenebis(salicylideneimine) derivatives of gallium trimethyl: crystal and molecular structure of N,N-ethylenebis(salicylideneiminato) bis(dimethylgallium)

1977 ◽  
Vol 55 (13) ◽  
pp. 2540-2546 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Weighted Mean ◽  
Full Matrix ◽  
Derivatives Of ◽  
Distorted Tetrahedral Coordination

Crystals of N,N-ethylenebis(salicylideneiminato)bis(dimethylgallium) are orthorhombic, a = 22.781(1), b = 9.4869(6), c = 19.700(2) Å, Z = 8, space group Pbca. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.036 and Rw of 0.029 for 2248 reflections with I ≥ 3σ(I). Details of the preparation and physical properties of (C16H14N2O2)(GaMe2)2 and (C16H15N2O2)(GaMe2) are given. The (C16H14N2O2)(GaMe2)2 molecule is approximately centrosymmetric in the solid state. A "GaMe2" unit is coordinated to each of the two salicylideneiminato moieties of the N,N-ethylenebis(salicylideneiminato) ligand. The gallium atoms have a distorted tetrahedral coordination geometry, with bond angles at gallium ranging from 92.7(1) to 124.6(3)°. Important bond lengths (corrected for libration) are: Ga—O, 1.886(2) and 1.884(2), Ga—N, 2.033(3) and 2.042(3), and weighted mean Ga—C, 1.959(9) Å.

The methylgallium-2-carboxylatobenzimidazolato hexamer, [MeGa·C8H4N2O2]6·C6H6·(Me2C6H4)2; synthesis and X-ray crystal structure

1999 ◽  
Vol 77 (4) ◽  
pp. 434-438 ◽  
Author(s):  
Steven J Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Room Temperature ◽  
Direct Methods ◽  
Membered Ring ◽  
Coordination Geometry ◽  
Temperature Reaction ◽  
Full Matrix ◽  
X Ray ◽  
Solvent Molecules

The room-temperature reaction of Me3Ga with benzimidazole 2-carboxylic acid in xylene solvent has yielded a novel crystalline hexameric gallium compound with "MeGa" moieties bridged by the doubly depronotated ligand precursor. Crystals of [MeGa(4,5-benzimidazolato-2-carboxylato)]6·(C6H6)·(m-Me2C6H4)2 are monoclinic, a = 18.091(2), b = 17.094(2), c = 13.2215(5) Å, Z = 2, space group C2/m. The structure was solved by direct methods and refined by full-matrix least-squares procedures to R (F, I [Formula: see text] 3σ(I)) = 0.064 (Rw (F2, all data) = 0.134). The hexameric Ga complex contains a six-membered ring of Ga atoms, bridged by the benzimidazolate ligands with the benzo rings projecting alternately above and below the Ga plane, thus forming a ball-shaped molecule. The complex could have ideal D3d symmetry, but it contains an encapsulated molecule of benzene, which distorts the regularity of the Ga6 hexagon, and reduces the symmetry of the complex to the crystallographically observed C2h. The coordination geometry at each of the two independent GaO2N2C centres approximates a trigonal bipyramid, with a N2C trigonal plane, and the O atoms above and below; average dimensions are Ga-O = 2.176(2), Ga-N = 1.973(3), Ga-C = 1.927(5) Å, O-Ga-O = 165°. The unit cell also contains four m-xylene solvent molecules (outside the molecular cage).Key words: gallium, crystal structure, benzene intercalate, benzimidazolecarboxylic acid.

Synthesis, structure, and properties of poly-bis(μ-diethylphosphinato)copper(II)

1982 ◽  
Vol 60 (15) ◽  
pp. 2017-2022 ◽  
Author(s):  
Katherine W. Oliver ◽  
Steven J. Rettig ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Infrared Spectra ◽  
Field Model ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Structure And Properties ◽  
Tetrahedral Coordination ◽  
Full Matrix

The preparation, magnetic properties, electronic and infrared spectra, and molecular structure of poly-bis(μ-diethylphosphinato)copper(II) are described. Crystals of poly-bis(μ-diethylphosphinato)copper(II) are triclinic, a = 7.700(1), b = 9.807(1), c = 10.101(1) Å, α = 90.48(1), β = 104.77(1), γ = 112.21(1)°, Z = 2, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.025 and Rw = 0.032 for 3491 reflections with I ≥ 3σ(I). The polymeric structure consists of Cu atoms with flattened tetrahedral coordination geometry linked by double phosphinate bridges. Mean bond lengths (corrected for libration) are: Cu—O, 1.924(3), P—O, 1.526(4), and P—C, 1.807(4) Å. Assignment of the electronic spectrum using a crystal field model gives Dq = 1665 cm−1 and Cp = 1800 cm−1. Magnetic susceptibility studies give no evidence for magnetic concentration over the temperature range 80 to 300 K.

scholarly journals Synthesis and Characterisation of Zinc(II) Complex With 2-Amino-5-bromopyridine Ligand

2017 ◽  
Author(s):  
Fitriani
Keyword(s):  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Visible Absorption ◽  
X Ray ◽  
X Ray Crystallography ◽  
Uv Visible ◽  
Cl Atoms ◽  
Distorted Tetrahedral Coordination

The synthesis and characterisation of zinc(II) complex with 2-amino-5-bromopyridine (C5H5BrN2) ligand have been described. The complex was structurally characterised via X-ray crystallography, in the title compound, (2-amino-5-bromopyridinium) [ZnCl¬3(2-amino-5-bromopyridine)] or which is also called (C5H6BrN2) [ZnCl3(C5H5BrN2)]¬. The Zn(II) atom is four-coordinated by three Cl atoms and one imine N-atom of 2-amino-5-bromopyridine ligand, forming a distorted tetrahedral coordination geometry. The complex was also investigated by elemental analysis, 1H NMR, IR spectroscopy and UV-Visible absorption. The protonation behaviour upon coordination is discussed.

Metal pyrazolate polymers. Part 1. Synthesis, structure, and magnetic properties of the [Cu(pz)2]x polymer

1989 ◽  
Vol 67 (11) ◽  
pp. 1970-1974 ◽  
Author(s):  
M. K. Ehlert ◽  
S. J. Rettig ◽  
A. Storr ◽  
R. C. Thompson ◽  
J. Trotter
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Magnetic Data ◽  
Coordination Geometry ◽  
Antiferromagnetic Exchange ◽  
Chain Polymer ◽  
X Ray ◽  
Linear Chains ◽  
Polymeric Chains ◽  
Distorted Tetrahedral Coordination

A novel and reliable method for the synthesis of polybis(μ-pyrazolato-N,N′)copper(II), [Cu(pz)2]x(where pz = N2C3H3), is presented. Single crystals of the polymer suitable for X-ray study have been grown under carefully controlled conditions. Crystals of polybis(μ-pyrazolato-N,N′)copper(II) are orthorhombic, a = 7.917(1), b = 11.491(2), c = 7.778(1) Å, Z = 4, space group Ibam. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.029 and Rw = 0.038 for 507 reflections with I ≥ 3σ(I). The crystal structure consists of infinite double-bridged polymeric chains. The Cu atom has a D2 distorted tetrahedral coordination geometry with Cu—N = 1.957(2) Å and N—Cu—N = 94.3(1)–139.5(1)°. Magnetic susceptibility studies (4.2 to 299 K) on this material reveal very strong antiferromagnetic exchange between copper(II) centres in the extended linear chains. The magnetic data have been successfully analyzed according to the isotropic Heisenberg model for linear chains with −J = 78 cm−1 and g = 2.12. Keywords: crystal structure, copper(II) pyrazolate chain polymer, antiferromagnetic exchange.

Thiophenophane–metal complexes. I. Preparation, X-ray structure, and cyclic voltammetry of 2,5,8-trithia[9](2,5)thiophenophane, L, and of its metalcomplexcation bis(2,5,8-trithia[9](2,5)thiophenophane-S2,S3]copper(I),[CuL2]+1

1988 ◽  
Vol 66 (6) ◽  
pp. 1506-1512 ◽  
Author(s):  
C. Robert Lucas ◽  
Liu Shuang ◽  
Michael J. Newlands ◽  
Jean-Pierre Charland ◽  
Eric J. Gabe
Keyword(s):  
Cyclic Voltammetry ◽  
Reference Electrode ◽  
Molecular Structures ◽  
Saturated Calomel Reference Electrode ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Distorted Tetrahedral Coordination

Preparation of the thiophenophane C10H14S4, (L), and syntheses of its copper(I) complex [CuL2]ClO4 or [CuL2]BF4 are described. The 13C and 1H nmr spectra of L and the ir spectra (4000–200 cm−1) of [CuL2]ClO4 and [CuL2]BF4 are reported. The molecular structures of L and [CuL2]ClO4 have been determined. For L: space group P21/a, a = 7.9347(2) Å, b = 18.7479(3) Å, c = 8.8596(2) Å, β = 108.446(2)°, Z = 4, Rf = 0.048, and Rw = 0.034. For [CuL2]ClO4: space group P21/c, a = 9.4363(1) Å, b = 18.2768(3) Å, c = 16.2157(3) Å, β = 96.520(2)°, Z = 4, Rf = 0.056, and Rw = 0.037. The Cu(I) complex has distorted tetrahedral coordination geometry; its perchlorate anion is non-coordinating and disordered. The Cu—S bond lengths lie in the range 2.301–2.392 Å and the S—Cu—S angles in the range 92.43—150.26°. Cyclic voltammetry of [CuL2]ClO4 (10−3 mol/L in dimethylsulfoxide, 0.1 mol/L Et4NClO4, glassy carbon working electrode, platinum counter electrode, aqueous saturated calomel reference electrode against which the ferrocenium/ferrocene potential under similar conditions was 400 mV) shows a quasi-reversible oxidation (E1/2 = 0.150 V, ΔEp = 170 mV at 50 mV/s). Thiophene's effect as a sub-unit in a small macrocycle upon properties of the latter is discussed.

A new heteroleptic cuprous complex with strong yellow photoluminescence

2014 ◽  
Vol 70 (9) ◽  
pp. 858-861 ◽  
Author(s):  
Kaijie Xu ◽  
Mingwei Hong ◽  
Yicheng Zhang ◽  
Li Song ◽  
Wenxiang Chai
Keyword(s):  
Yellow Emission ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Acetonitrile Molecule ◽  
X Ray ◽  
Emission Signal ◽  
Ligand Charge Transfer ◽  
Distorted Tetrahedral Coordination ◽  
Cuprous Complex

In the title heteroleptic cuprous complex, (acetonitrile-κN)({2-[2-(diphenylphosphanyl)phenoxy]phenyl}diphenylphosphane-κ2P,P′)[2-(pyridin-4-yl-κN)-1,3-benzoxazole]copper(I) hexafluoridophosphate, [Cu(C36H28OP2)(CH3CN)(C12H8N2O)]PF6, conventionally abbreviated [Cu(POP)(CH3CN)(4-PBO)]PF6, where POP is the diphosphane ligand {2-[2-(diphenylphosphanyl)phenoxy]phenyl}diphenylphosphane and 4-PBO is the N-containing ligand 2-(pyridin-4-yl)-1,3-benzoxazole, the asymmetric unit consists of a hexafluoridophosphate anion and a whole mononuclear cation, where the CuIcentre is coordinated by two P atoms from the POP ligand, by one N atom from the 4-PBO ligand and by the N atom of the coordinated acetonitrile molecule, giving rise to a CuP2N2distorted tetrahedral coordination geometry. The electronic absorption, photoluminescence and thermal stability properties of this complex have been studied on as-synthesized samples, which had previously been examined by powder X-ray diffraction. A yellow emission signal is attributed to an excited state arising from metal-to-ligand charge transfer (MLCT).

Bis(2,9-dimethyl-1,10-phenanthroline)copper(I) tetraphenylborate dichloromethane solvate

2007 ◽  
Vol 63 (3) ◽  
pp. m800-m802 ◽  
Author(s):  
William T. Eckenhoff ◽  
Tomislav Pintauer
Keyword(s):  
Bond Length ◽  
Dihedral Angle ◽  
Title Compound ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Π Stacking ◽  
Distorted Tetrahedral Coordination

In the title compound, [Cu(C14H12N2)2]C24H20B·CH2Cl2, CuI is chelated by two 2,9-dimethyl-1,10-phenanthroline (2,9-Me2phen) ligands, in a distorted tetrahedral coordination geometry. The average Cu—N bond length is 2.032 Å, and the interligand dihedral angle is 77.60 (6)°. The complexes form π–π stacking interactions between 2,9-Me2phen ligands, with a perpendicular interplanar separation of 3.652 (5) Å.

scholarly journals Bis[μ-1,3-bis(1H-imidazol-1-yl)propane-κ2N3:N3′]bis(dichloridozinc) dihydrate

2014 ◽  
Vol 70 (5) ◽  
pp. m184-m184
Author(s):  
Xiao-Juan Wang ◽  
Yun-Long Feng
Keyword(s):  
Zinc Complex ◽  
Complex Molecule ◽  
Dimensional Structure ◽  
Water Molecules ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Lattice Water ◽  
Bridging Ligand ◽  
Cl Atoms ◽  
Distorted Tetrahedral Coordination

The title hydrated complex, [Zn2Cl4(C9H12N4)2]·2H2O, is a discrete dinuclear zinc complex with 1,3-bis(1H-imidazol-1-yl)propane as the bridging ligand. The complex molecule lies about a crystallographic inversion centre. The ZnIIatom exhibits a distorted tetrahedral coordination geometry defined by two imidazole N atoms and two Cl atoms. O—H...Cl hydrogen bonding between the lattice water molecules and the terminal Cl atoms of the molecule lead to a two-dimensional structure extending parallel to (100).

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