Synthesis, Crystal Structure and Magnetic Properties of a Copper(II) p-Formylbenzoate Complex

2012 ◽  
Vol 67 (11) ◽  
pp. 1185-1190 ◽  
Author(s):  
Jin-Li Qi ◽  
Wei Xu ◽  
Yue-Qing Zheng

A new Cu(II) complex was prepared at room temperature from the reaction of p-formylbenzoic acid, phenanthroline, CuCl2⋅2H2O, and NaOH under ethanolic aqueous conditions. The complex has been characterized by X-ray diffraction, IR spectroscopy, TG-DTA analyses, and magnetic measurements. Single-crystal X-ray diffraction analysis indicated that the complex crystallizes in the triclinic space group P1̄ with the cell dimensions a=7.875(2), b=10.724(2), c=15.317(3) Å , α =102.65(3), β =93.71(3), γ =107:64(3)°. The Cu atoms are in the environment of distorted CuN2O3 tetragonal pyramids. These discrete complex molecules are packed through intermolecular π...π-stacking interactions and C-H...O hydrogen bonds forming a supramolecular structure. The title complex obeys the Curie-Weiss law with a Curie constant C=0:53 cm3 K mol-1 and a Weiss constant θ = -0:27 K. The shape of the xmT curve is characteristic of weak ferromagnetic interactions between the Cu(II) centers from 300 to 7 K, while there are weak antiferromagnetic interactions below 7 K.

2007 ◽  
Vol 62 (10) ◽  
pp. 1267-1270 ◽  
Author(s):  
Xian-Wen Wang ◽  
Fu-Ping Chen ◽  
Liang Chen ◽  
Jing-Zhong Chen

A new ternary mixed ligand dinuclear samarium(III) complex, Sm2(C3H3O2)6(phen)2 (1) (C3H3O2 = acrylate; phen = 1,10-phenathroline), has been synthesized and characterized by microanalysis, IR and UV/vis spectra and single crystal X-ray diffraction. Compound 1 crystallizes in the triclinic space group P1̅ with cell parameters: a = 9.6687(19), b = 10.690(2), c = 10.799(2) Å , α = 105.50(3), β = 106.67(3), γ = 91.59(3)°, V = 1023.8(3) Å3. The Sm(III) cations are bridged by four acrylate anions into a dinuclear molecular unit. The nine-coordinate Sm(III) atoms adopt a significantly distorted monocapped anti-square-prismatic geometry. Within the crystal structure, the complex molecules are associated via π-π stacking interactions into one-dimensional supramolecular chains along the [011] direction. Compound 1 exhibits intense fluorescence in the solid state at room temperature.


2019 ◽  
Vol 74 (6) ◽  
pp. 485-489
Author(s):  
Yuan Huang ◽  
Xiu-feng Yu ◽  
Zhen Rong ◽  
Yi-chun Ai ◽  
Kun Qian ◽  
...  

AbstractA new complex [Pr3NH]+ [Mn(dca)3]− · H2O (dicyanamide = dca−) was synthesized, in which the Mn2+ cations are bridged by end-to-end dca anions to form three-dimensional [Mn(dca)3]nn− networks and tripropylammonium cations reside in the cavities of these networks. The complex has been characterized by single-crystal X-ray diffraction, infrared spectroscopy, elemental analysis, and magnetic measurements. Magnetic susceptibility data indicate ferromagnetic interactions among the MnII ions.


1965 ◽  
Vol 9 ◽  
pp. 170-189 ◽  
Author(s):  
M. Stammler ◽  
R. Bruenner ◽  
W. Schmidt ◽  
D. Orcutt

AbstractThe thermal transformations which take place in solid methyl-substituted ammonium perchlorates have been studied using high-temperature X-ray diffraction and differential thermal analysis techniques. In the temperature range from 20°C to their decomposition temperature (above 300°C), ammonium perchlorate and tetramethyl ammonium perchlorate undergo only one enantiomorphic phase transition, namely at 240 and 340°C (with decomposition), respectively. This I—II transition is ascribed to the beginning of the free rotation of the ClO4− ions. The rotation of the cations, however, begins below room temperature. If the symmetry of the cation is lowered by having both methyl groups and hydrogens arranged around the nitrogen (as in monomethyl, dimethyl, and trimethyl ammonium perchlorates), there is an additional enantiomorphic phase transition. This I—II transformation is ascribed to the rotation of the cations which have, in the partially substituted ions, two sets of non-equivalent symmetry axes (different moments of inertia). The temperatures of transformation are discussed in terms of the space requirements for rotation. Symmetries and cell dimensions of some modifications were determined.


1992 ◽  
Vol 70 (3) ◽  
pp. 792-801 ◽  
Author(s):  
Jagadese J. Vittal ◽  
Philip A. W. Dean ◽  
Nicholas C. Payne

The structures of three tetramethylammonium salts containing anions of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd) were determined by single crystal X-ray diffraction techniques. The Zn salt crystallizes in different space groups depending upon the solvent combination used in the synthesis. Thus crystals of (Me4N)2[Zn4(SePh)10], 1, grown from a mixture of methanol, acetonitrile, and acetone are triclinic, space group [Formula: see text] with cell dimensions a = 13.214(2), b = 23.859(2), c = 13.072(1) Å, α = 91.134(8), β = 113.350(8), γ = 79.865(9)°, and Z = 2. In the absence of acetone, a solvated crystal (Me4N)2[Zn4(SePh)10]•CH3CN, 2, is formed, which belongs to the monoclinic space group P21/n with a = 14.248(1), b = 39.722(2), c = 13.408(1) Å, β = 97.132(5)°, and Z = 4. The Cd salt (Me4N)2[Cd4(SePh)10], 3, crystallizes in the monoclinic space group P21/c, with a = 20.830(2), b = 14.282(1), c = 25.872(1) Å, β = 99.626(6)°, and Z = 4. These three salts are the first examples of homoleptic, tetranuclear selenolatometal(II) anions with (μ-Se)6M4 cages of adamantane-type stereochemistry. In each case the phenyl substituents of the bridging ligands adopt the configuration [aae, aae, aee, aee], which has the minimum number of two 1,3-axial–axial non-bonding substituent interactions. Keywords: selenolate complexes, synthesis, X-ray crystallography, isomerism, adamantane stereochemistry.


2006 ◽  
Vol 61 (10) ◽  
pp. 1217-1221 ◽  
Author(s):  
Zerrin Heren ◽  
Cem Keser ◽  
C. Cüneyt Ersanli ◽  
O. Zafer Yeşilel ◽  
Nazan Ocak

The mixed-ligand picolinato (pic) complex of Cu(II) with 4-methylimidazole (4-MeIm), [Cu(pic)2(4-MeIm)2], was synthesized and characterized by elemental analysis, magnetic susceptibility, spectroscopic methods (UV/vis and FT-IR) and X-ray diffraction. In the slightly distorted octahedral cis-bis(4-methylimidazole)bis(picolinato)copper(II) complex, the pic ligands are coordinated to the Cu(II) ion as bidentate N,O-donors forming chelate rings. The 4-MeIm ligands are N-coordinated in cis positions. The complex crystallizes in the triclinic space group p̅1 with unit cell parameters a = 9.204(5), b = 9.498(5), c = 13.095(5) Å , α = 90.395(5), β = 101.687(5), γ = 112.291(5)° and Z = 2. Hydrogen bondings and C-H ··· π interactions occur between picolinato and methylimidazole ligands of neighboring complex molecules. The thermal decomposition of the complex is described.


2005 ◽  
Vol 475-479 ◽  
pp. 3729-3732
Author(s):  
Cong Mian Zhen ◽  
Xiao Xia Zhai ◽  
Chengfu Pan ◽  
Xiangfu Nie

FePt/C mutilayer films were successfully prepared by using RF and DC magnetron sputtering system. FePt nanoparticles embedded in a C matrix were formed by consequently annealing. X-ray diffraction (XRD) results show the degree of atomic ordering of the L10 structure increases with higher temperature annealing. Room temperature magnetic measurements reveal that in-plane coercivity HC, and squareness Mr/MS depend on the thickness of carbon layer. Relatively High HC (3245.1Oe) and squareness (0.67) were obtained when the thickness of C layer is 2.0 nm. The carbon layer not only isolates the FePt grain, but also suppresses the growth of fct FePt grains. When the thickness of carbon layer is 2.0 nm, the FePt grain size decreases down to ~20 nm measured by Scan Probe Microscope (SPM). Interactions between particles can be tuned to near zero when we select the proper thickness of C layer.


2009 ◽  
Vol 1199 ◽  
Author(s):  
Danilo G Barrionuevo ◽  
Surinder P Singh ◽  
Maharaj S. Tomar

AbstractWe synthesized BiFe1-xMnxO3 (BFMO) for various compositions by sol gel process and thin films were deposited by spin coating on platinum Pt/Ti/SiO2/Si substrates. X-ray diffraction shows all the diffraction planes corresponding to rhombohedrally distorted perovskite BiFeO3 structure. The absence of any impurity phase in the films suggests the incorporation Mn ion preferentially to Fe site in the structure for low concentration. Magnetic measurements reveal the formation of ferromagnetic phase at room temperature with increased Mn substitution. On the other hand, ferroelectric polarization decreases with increasing Mn ion concentration. Raman studies suggest the dopant induced structural distortion.


2016 ◽  
Vol 81 (11) ◽  
pp. 1251-1262 ◽  
Author(s):  
Oluwafunmilayo Adekunle ◽  
Ray Butcher ◽  
Oladapo Bakare ◽  
Olusegun Odunola

[Cu(phen)2(CH3COO)](ClO4).2H2O (1) and [Cu(bipy)2(CH3COO)]-(ClO4).H2O (2) {phen = 1,10-phenanthroline, bipy = 2,2?-bipyridine}were synthesized and characterized. The complexes were characterized by employying elemental analyses, infrared and UV-Visible spectroscopy, room temperature magnetic measurements and the crystal structures elucidated using X-ray diffraction experiment. The redox properties of the complexes were also investigated. Both structures have a square pyramidal CuN4O chromophore which exhibit significant distortions due to long Cu-O [2.217(3) ? for (1) and 2.179 (1) for (2)] and Cu-N [2.631(2) ? for (1) and 2.714(1) ? for (2)] bonds. This distortion if further shown by the O-Cu-N bond angles [147.71(8) o for (1) and 153.40(5) o for (2)]. The elemental analyses further support the structural details unveiled by the single crystal X-ray diffraction analysis. The infrared spectra shows the acetate vibrational frequencies at 1587 cm-1,1428 cm-1, 1314 cm-1 for (1) and 1571 cm-1, 1441 cm-1, 1319c m-1 for (2) and the perchlo-rate bands at 1059 cm-1, 720 cm-1 (1) and 1080 cm-1,768 cm-1 (2). The broad d-d bands for the copper ion at 14,514 cm-1(1) and 14,535 cm-1(2) support the adoption of square pyramid geometries. The magnetic moments for the two complexes are 1.83 B.M for (1) and 1.72 B.M for (2). The peak to peak values of the two complexes show that the electrode reactions are quasi-reversibile with ?Ep = 0.023V (1) and 0.025V for (2). In both structures, there are ?-? intermolecular interactions in addition to hydrogen bonding between the units.


1986 ◽  
Vol 39 (12) ◽  
pp. 2145 ◽  
Author(s):  
MI Bruce ◽  
MR Snow ◽  
ERT Tiekink

The crystal structure of OsPt2(μ-CO)3(CO)2(PPh3)3 has been determined by single-crystal X-ray diffraction techniques. Crystals are triclinic, space group Pī with unit cell dimensions a 13.593(4), b 15.839(4), c 12.633(8) Ǻ, α 102.97(3), β 108.18(2), γ 84.86(3)° with Z2. The structure was refined by a full-matrix least-squares procedure on 5896 reflections [I ≥ 2.5σ(I)] to final R 0.028 and Rw 0.034. A triphenylphosphine ligand binds each of the metal atoms disposed at the corners of a triangle. Each metal-metal bond is spanned by a bridging carbonyl group. The coordination about the osmium atom is completed by two terminal carbonyl groups.


1999 ◽  
Vol 52 (10) ◽  
pp. 949 ◽  
Author(s):  
Martin A. Bennett ◽  
Glen B. Robertson ◽  
Pramesh N. Kapoor

Reaction of the cyclohexyne–platinum(0) complex [Pt(η2-C6H8)(Cy2PCH2CH2PCy2)]* with water and CO2 in the presence of triphenylphosphine gives the bicarbonate salt of the (η1-cyclohexenyl)platinum(II) cation, [Pt(η1-C6H9)(Cy2PCH2CH2 PCy2)(PPh3)] [HCO3] · 3H2O, which has been characterized by n.m.r. spectroscopy and single-crystal X-ray diffraction at low temperature. Crystals are triclinic, space group P1– with unit cell dimensions a 20.315(2), b 12.782(1), c 10.694(1) Å, α 66.61(1), β 104.73(1), γ 102.11(1)˚, and Z 2. The structure was refined to a final R value of 0.036 with use of 7553 reflections [I > 3σ(I)]. The cation has the expected, somewhat distorted planar coordination geometry; the anion consists of discrete, hydrogen-bonded dimers [(HCO3)(H2O)3]22-.


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