scholarly journals Structural Studies of [(py)2CdFe(CO)4]3 and {(THF)5[CdFe(CO)4]3}

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Bryce Anderson ◽  
Atta M. Arif ◽  
Richard D. Ernst
Keyword(s):  
Membered Ring ◽  
Coordination Geometry ◽  
Structural Studies ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
Complex Versus ◽  
Amine Ligands ◽  
Basic Amine

The structures of [(py)2CdFe(CO)4]3 and {(THF)5[CdFe(CO)4]3} have been determined (py = pyridine; THF = tetrahydrofuran). Each is composed of a six-membered ring having alternating cadmium and iron centers. The presence of the more strongly basic amine ligands in the former led to a greater contribution of an ionic resonance form, which resulted in overall longer Cd–Fe bonds and a greater contribution of a bicapped tetrahedral coordination geometry about iron. Thus, the Cd–Fe distances range from 2.5679(4) to 2.6501(1) Å for the THF complex versus 2.6445(8) to 2.6833(7) Å for the py complex. Similarly, the Fe–Cd–Fe and Cd–Fe–Cd angles for the THF complex fell in respective ranges of 139.03(2)–157.27(2)° and 84.41(1)–99.79(1)°, as compared to 135.31(3)–139.51(4)° and 102.52(3)–104.62(4)° for the py complex. The space group for the former compound is Pbcn, with a = 12.2678(2), b = 22.4601(5), and c = 17.0039(4) Å, while for the THF complex, the space group is P21/c, with a = 10.7297(2), b = 20.4961(2), c = 18.7464(3) Å, and β = 94.2715(6)°.

Anionic pyrazolyl-bridged nickel nitrosyl complexes. Synthesis, structure, and reactivity

1979 ◽  
Vol 57 (23) ◽  
pp. 3099-3106 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Ion Pair ◽  
Sodium Ion ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
Nitrosyl Complexes ◽  
Pyrazolyl Group ◽  
The Mean ◽  
Distorted Tetrahedral Coordination ◽  
Molecular Unit

A series of anionic pyrazolyl-bridged nickel nitrosyl complexes, M+[(ON)Ni(μ-L2)(μ-X)Ni(NO)]− (where L = pyrazolyl, N2C3H3, or 3,5-dimethylpyrazolyl, N2C5H7; X = Cl, Br, I, or N2C5H7; and M = Na, (CH3)4N, or (C2H5)4N) is described. Crystallographic analyses have been carried out on two of these complexes. Crystals of [(C2H5)4N]+[(ON)Ni(μ-I)(μ- N2C5H7)2Ni(NO)]− are orthorhombic, a = 19.910(1), b = 14.0330(7), c = 9.3195(9) Å, Z = 4, space group Pn21a and crystals of [(C4H8O)2Na][(ON)Ni(μ-N2C5 H7)3Ni(NO)] are orthorhombic, a = 19.897(2), b = 19.529(3), c = 15.894(2) Å, Z = 8, space group Pbca. Both structures were solved by Patterson and Fourier syntheses and were refined by full-matrix least-squares procedures to R = 0.027 and 0.057 for 2572 and 2168 reflections with I ≥ 3σ(I) respectively. The structure of [(C2H5)4N]+[(ON)Ni(μ-I)(μ-N2C5H7)2Ni(NO)]− consists of discrete cations and binuclear anions which have approximate C2v symmetry. The nickel atoms have distorted tetrahedral coordination geometry. Important mean molecular dimensions (distances corrected for libration) are: Ni—I—Ni, 73.67(2)°, Ni—I, 2.765(3), Ni—NO, 1.649(5), Ni—N(pyrazolyl), 1.980(14) Å, and Ni—N—O, 172.5(18)°. The structure of [(C4H8O)2Na][(ON)Ni(μ-N2C5 H7)3Ni(NO)] consists of discrete ion-pair units in which the two NiNO moieties are bridged by three N2C5H7 ligands, two of which are coordinated to the sodium ion via a novel η2(N,N) π-interaction (mean Na—N = 2.61(3) Å). The sodium is also coordinated to two tetrahydrofuran oxygen atoms to give a distorted tetrahedral coordination geometry about the sodium (Na—O = 2.301(6) and 2.266(5) Å). Except for disordered tetrahydrofuran carbon atoms, the molecular unit has approximate C2v symmetry. The nickel atoms have distorted tetrahedral coordination geometry, the mean distances being Ni—NO, 1.591(6), Ni—N(pyrazolyl), 1.985(2) for the unique pyrazolyl group and 2.016(5) Å for the pyrazolyl nitrogen atoms coordinated to Na. The mean Ni—N—O angle is 176.9(11)°.

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.

Zinc 3,5-dimethylpyrazolate complexes: synthesis and structural studies. The crystal and molecular structure of [Zn2(dmpz)4(Hdmpz)2]

1990 ◽  
Vol 68 (9) ◽  
pp. 1494-1498 ◽  
Author(s):  
Martin K. Ehlert ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
High Yield ◽  
Coordination Geometry ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group

Zinc metal reacts with excess 3,5-dimethylpyrazole (Hdmpz) in the presence of O2 to produce materials of composition Zn(dmpz)2(Hdmpz)y. Thermolysis of these materials results in the loss of Hdmpz and the formation of the [Zn(dmpz)2]x polymer. Under appropriate conditions the pure dimer [Zn2(dmpz)4(Hdmpz)2] can be obtained in high yield. Crystals of bis[μ-(3,5-dimethylpyrazolyl-N1,N2)]bis[(3,5-dimethylpyrazolyl)(3,5-dimethylpyrazole)zinc(II)] are orthorhombic, a = 17.009(2), b = 29.239(2), c = 13.590(2) Å, Z = 8, space group Fddd. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.037 and Rw = 0.042 for 913 reflections with I ≥ 3σ(I). The structure of [Zn2(dmpz)4(Hdmpz)2] contains nearly planar doubly dmpz bridged Zn2 units capped at each end by strongly hydrogen-bonded [Formula: see text] units. The zinc atoms display pseudotetrahedral coordination geometry with Zn—N = 1.991(3) (bridging) and 2.025(3) Å (terminal), and N—Zn—N = 99.6(2)–113.8(2)°. Keywords: zinc 3,5-dimethylpyrazolate complexes, crystal structure.

scholarly journals Tetrakis(dimethoxyboryl)methane

IUCrData ◽  
2016 ◽  
Vol 1 (8) ◽  
Author(s):  
Sumeng Liu ◽  
Gregory S. Girolami
Keyword(s):  
Title Compound ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Occupancy Factor ◽  
Bond Lengths ◽  
Methoxy Groups ◽  
Synthetic Intermediate ◽  
Distorted Tetrahedral Coordination

The title compound, tetrakis(dimethoxyboryl)methane (systematic name: octamethyl methanetetrayltetraboronate), C9H24B4O8or C[B(OMe)2]4, is a useful synthetic intermediate. Crystals of this compound at 102 K conform to the orthorhombic space groupPbcn. The molecules, which reside on sites of crystallographic twofold symmetry, have idealized -4 point symmetry like most other CX4molecules in which eachXgroup bears two non-H substituents at the 1-position. The central C atom has a slightly distorted tetrahedral coordination geometry, with C—B bond lengths of 1.5876 (16) and 1.5905 (16) Å. One of the methoxy groups is disordered over two sets of sites; the major component has an occupancy factor of 0.676 (8).

Synthesis and structural studies of rhodium complexes of phosphorus—sulfur ligands

1986 ◽  
Vol 64 (9) ◽  
pp. 1870-1875 ◽  
Author(s):  
David G. Dick ◽  
Douglas W. Stephan
Keyword(s):  
Single Crystal ◽  
Planar Geometry ◽  
Methyl Groups ◽  
Rhodium Complexes ◽  
Coordination Geometry ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Square Planar

Rhodium complexes of the phosphorus—sulfur ligands, 2-diphenylphosphinoethyl methyl sulfide (MeSP), 1, and 2-diphenylphosphinothiophene (PTH), 2, have been prepared and studied by single crystal X-ray diffraction methods. [Rh(MeSP)2]BF4•H2O, 3, crystallizes in the space group P21/n with a = 16.939(6) Å, b = 17.152(5) Å, c = 12.049(9) Å, β = 106.50(4)°, and Z = 4. The MeSP ligands chelate to Rh yielding a distorted square-planar geometry. The disposition of the methyl groups on the cis sulfur atoms is transoid. Average Rh—P and Rh—S bond distances were found to be 2.225(3) and 2.347(3) Å, respectively. [Rh(PTH)2(COD)]BF4, 4, crystallizes in the space group Cc with a = 15.862(2) Å, b = 15.112(3) Å, c = 16.029(3) Å, β = 103.32(1)°, and Z = 4. The Rh atom in 4 also has essentially a square-planar coordination geometry. 2 does not chelate but rather is monohapto through phosphorus. Rh—P distances of 2.319(3) and 2.378(3) Å and Rh—C distances of 2.17(1), 2.22(1), 2.24(1), and 2.27(1) Å were found. The small variations in the Rh—P and Rh—C bonds distances appear to be a result of steric interactions between 2 and the COD ligand.

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.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

Structural studies of organoboron compounds. XX.(Salicylaldoximato-O,N)diphenylboron

1984 ◽  
Vol 62 (7) ◽  
pp. 1363-1368 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Hydrogen Bonds ◽  
Least Squares ◽  
Chelate Ring ◽  
Direct Methods ◽  
Structural Studies ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Phenolic Oxygen

Crystals of (salicylaldoximato-O,N)diphenylboron are triclinic, a = 10.125(2), b = 10.797(1), c = 14.760(2) Å, α = 89.05(1), β = 86.98(1), γ = 83.18(1)°, Z = 4, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.048 for4145 reflections with I ≥ 3σ(I). The structure consists of two crystallographically independent, but essentially identical, molecules linked by strong [Formula: see text] hydrogen bonds to form continuous spirals along the a axis. The Ph2B moiety is chelated by the phenolic oxygen and oxime nitrogen atoms of the ligand resulting in the formation of a non-planar six-membered chelate ring. Important libration-corrected mean bond lengths are O—B = 1.516(1), N—B = 1.609(2), and C—B = 1.613(2) 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).

Sign in / Sign up

Export Citation Format

Share Document