Synthesis, Characterisation, and X-Ray Crystal Structures of 8-Hydroxyquinoline Complexes of Group IV Metal Alkoxides

2013 ◽  
Vol 66 (12) ◽  
pp. 1587
Author(s):  
Mahsa Armaghan ◽  
Mahdi Mirzaee ◽  
Mahmood Norouzi ◽  
Mostafa M. Amini ◽  
Hamid Reza Khavasi
Keyword(s):  
Metal Ion ◽  
Room Temperature ◽  
Group Iv ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Nitrogen ◽  
Distorted Octahedral ◽  
Stoichiometric Reaction ◽  
Alkoxy Groups

Stoichiometric reaction of 8-hydroxyquinoline with titanium tetraethoxide, and zirconium and hafnium tetra-2-propoxide in toluene at room temperature resulted in formation of [M2-μ-(OR)2-(C9H6NO)2(OR)2] (1: M = Ti, R = Et; 2: M = Zr, R = iPr; 3: M = Hf, R = iPr). All complexes were characterised by infrared, ultraviolet-visible, and NMR spectroscopy, and mass spectrometry. The molecular structures of 1, 2, and 3 were determined by single-crystal X-ray diffraction. The coordination geometries around the metal ions are distorted octahedral, which share an edge through bridged alkoxy groups. Each anionic 8-quinolinolate ligand is also chelated to one metal ion through its pyridine nitrogen and phenolate oxygen atoms.

The structure of monoclinic NaNiO2 as determined by powder X-ray and neutron scattering

1997 ◽  
Vol 12 (4) ◽  
pp. 239-241 ◽  
Author(s):  
Stefan Dick ◽  
Michaela Müller ◽  
Franziska Preissinger ◽  
Thomas Zeiske
Keyword(s):  
Neutron Scattering ◽  
Room Temperature ◽  
Scattering Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Jahn Teller ◽  
Na Ions ◽  
Starting Model

The crystal structure of low temperature NaNiO2 has been refined by Rietveld methods using powder X-ray diffraction and neutron scattering data. The starting model was based on parameters that had been obtained earlier by X-ray film methods. At room temperature NaNiO2 is monoclinic, C2/m, a=0.53192(2), b=0.28451(1), c=0.55826(4) nm, β=110.449(2)°. NaNiO2 has a layered structure. The Ni–O layer is formed by edge sharing of Jahn–Teller elonganted NiO6 octahedra with Ni–O distances of 0.1911(2) nm and 0.2144(4) nm. The Na ions between these layers also exhibit a distorted octahedral coordination with Na–O distances of 0.2328(2) nm and 0.2369(4) nm. The final R values were Rwp=0.069, RI=0.059, Rexp=0.059 for the neutron and Rwp=0.032, RI=0.034, Rexp=0.017 for the X-ray data.

Synthesis, IR and X-Ray Studies of Tetra(N,N′-tetraethyl-N″-benzoyl- phosphorictriamide)-tetra(μ-3-methoxo)-tetra(methanol)tetra-NickeI(II)

1998 ◽  
Vol 53 (8) ◽  
pp. 836-840 ◽  
Author(s):  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Anatoliy A. Kapshuk ◽  
Tatyana Yu. Sliva ◽  
Tadeusz Glowiak ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Metal Ion ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Methoxy Groups ◽  
Oxygen Atoms

Abstract A new nickel(II) complex with N,N′-tetraethyl-N″-benzoylphosphortriamide (HL = C6H5C(O)N(H)P(O)(NEt2)2) of composition Ni4L4(OCH3)4·(HOCH3)4 (1) has been synthe­ sized. The crystal and molecular structure of 1 has been determined from the X-Ray diffraction data (tetragonal, space group P4̄21c with a = 17.000(2) Å, c = 15.338(3) Å, Z = 2; R = 0.0399 for 1412 unique reflections). The structure is made up of cubane-like tetramers. In the corners of a cube there are 4 atoms of nickel and 4 atoms of oxygen of methoxy groups. The nickel atoms are characterized by a slightly distorted octahedral environment, which consists of three oxygen atoms of methoxy groups, carbonylic and phosphorylic oxygen atoms of the ligand L-, and an oxygen atom of a methanol molecule. The ligands L- coordinate to the metal ion forming a chelate via the oxygen atoms of carbonylic and phosphorylic groups.

Synthesis, crystal structures, and thermal and spectroscopic properties of two Cd(II) metal-organic frameworks with a versatile ligand

2016 ◽  
Vol 71 (8) ◽  
pp. 909-917 ◽  
Author(s):  
Jia-Ming Li ◽  
Kun-Huan He ◽  
Zhong-Feng Shi ◽  
Hui-Yuan Gao ◽  
Yi-Min Jiang
Keyword(s):  
Room Temperature ◽  
Metal Organic Frameworks ◽  
Spectroscopic Properties ◽  
Supramolecular Architecture ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Hydrogen Bond Interactions ◽  
Distorted Octahedral ◽  
Metal Organic

AbstractTwo new metal-organic frameworks, namely, [Cd(L)(H2O)]n (1) and {[Cd0.5(L)(4,4′-bipy)0.5][Cd0.5(H2O)(4,4′-bipy)0.5]·H2O}n (2), where H2L = N-pyrazinesulfonyl-glycine and 4,4′-bipy = 4,4′-bipyridine, have been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental, thermogravimetric, and photoluminescent analysis. X-ray diffraction crystallographic analyses indicate that 1 displays a distorted octahedral metal coordination in a 3-connected (4, 82) topology, while the molecular structure of 2 has a 4-connected (4, 4) topology with two perfectly octahedrally coordinated Cd centers. The L2– ligand serves as a N,N,O-tridentate, μ2-pyrazine-bridging, and μ2-carboxylate-bridging ligand in 1, and as a N,O-bidentate and μ2-carboxylate-bridging ligand in 2. In the crystal, a 3D supramolecular architecture is formed by O–H···O hydrogen bond interactions in 1, but through O–H···O as well as π···π stacking in 2. The two compounds show intense fluorescence in the solid state at room temperature.

Structures of Energetic Acetylene Derivatives HC≡CCH2ONO2, (NO2)3CCH2C≡CCH2C(NO2)3 and Trinitroethane, (NO2)3CCH3

2013 ◽  
Vol 68 (5-6) ◽  
pp. 719-731 ◽  
Author(s):  
Thomas M. Klapötke ◽  
Burkhard Krumm ◽  
Richard Moll ◽  
Alexander Penger ◽  
Stefan M. Sproll ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Gas Phase ◽  
Quantum Chemical ◽  
Room Temperature ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Polar Solvents ◽  
X Ray ◽  
Nmr Study ◽  
Acetylene Derivatives

The molecular structures and relative ratios of the two conformers (anti and gauche) of HCCCH2ONO2 detected in the gas phase at room temperature have been determined by electron diffraction. The results are discussed on the basis of quantum chemical calculations. The molecular structures of (NO2)3CCH2C≡CCH2C(NO2)3 and (NO2)3CCH3 have been determined by X-ray diffraction. A109Ag NMR study was performed for silver trinitromethanide Ag[C(NO2)3] in various polar solvents.

scholarly journals Preparation and Structures of Ternary Copper(II) Complexes of ADP and ATP Models for Enzyme-Metal Ion-Nucleoside Polyphosphate Complexes

1982 ◽  
Vol 37 (7) ◽  
pp. 863-871 ◽  
Author(s):  
William S. Sheldrick
Keyword(s):  
Metal Ion ◽  
Basic Structure ◽  
Axial Position ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
Bidentate Coordination ◽  
X Ray ◽  
Ph Values ◽  
Distorted Octahedral ◽  
The Third Terminal

AbstractThe stable ternary copper(II) complexes of ATP and ADP, [Cu(H2ATP)(phen)]2 · 7 H2O (2) and [Cu4(HADP)2(bipy)4(H2O)2(NO3)2] · 2 NO3 (3), have been isolated from aqueous solution at respective pH values of 2.8 and 4.0. Their structures have been established by single crystal X-ray diffraction. Tridentate coordination of each of the Cu atoms by ono α-, one β- and one γ-phosphate O atom of one ATP molecule is observed in 2. The binding Oα atoms occupy axial positions in a distorted octahedral geometry at Cu and the Cu- Oα interactions are weak. The other axial position is occupied by a γ-phosphate O atom of the second ATP molecule, leading to a dimeric structure. The basic structure of 3 is similar with, in this case, bidentate coordination of each of the central Cu atoms by one α- and one β-phosphate O atom of ono ADP molecule. In this case, however, the third terminal β-phosphate O atoms each bind a further Cu atom. All four Cu atoms in 3 display square pyramidal coordination. The structures of 2 and 3 are stabilised by intramolecular stacking of adenine and phenanthroline/bipyridyl systems. The significance of these structures as models for enzyme-metal ion-nucleoside polyphosphate complexes is discussed.

Addition der schweren Chalkogen-Atome und Halogenonium-Ionen an Carbodiphosphorane / Addition of the Heavy Chalkogen Atoms and Halogenonium Ions to Carbodiphosphoranes

1985 ◽  
Vol 40 (10) ◽  
pp. 1293-1300 ◽  
Author(s):  
H. Schmidbaur ◽  
Chr. Zybill ◽  
D. Neugebauer ◽  
G. Müller
Keyword(s):  
Room Temperature ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Structure Factors ◽  
Elemental Iodine

Hexaphenylcarbodiphosphorane Ph3P=C=PPh3 (1) forms deeply coloured, crystalline 1:1 ad- ducts with elemental sulfur, selenium and tellurium (2, 3 and 7, respectively). A superior method of synthesis for 7 is the reaction of Na2Te with (Ph3P)2CCl⊕Cl⊖. All three compounds are thermally unstable and decompose at or below room temperature. A selenium adduct 5 was also obtained with Me3P = C = PPh, (4). The compounds 2 and 3 can be alkylated at the chalkogen atoms using MeOSO2F or PhCH2Cl. Oxydation of 3 leads to Se - Se coupling.Addition of elemental iodine to 1 in molar ratios 1:1. 2:3 and 1:2 affords salt-like products composed of the (Ph2P)2Cl⊕ cation associated with I⊖ and/or I3⊖ anions (8a-c).The crystal and molecular structures of 3 and 8b have been determined by single crystal X-ray diffraction. 3′, containing one half equivalent of disordered tetrahydrofuran, crystallizes in the monoclinic space group P21/n (a = 10.848(6), b = 17.433(8). c = 16.848(9) Å, β = 91.51(5)°. V = 3185.07 Å3, ϱx = 1359 gcm-3, Z = 4). Based on 3488 structure factors, the final R value was 0.103. The selenium is attached to the ylidic carbon atom without major changes of the Ph3P=C=PPh3 skeleton (C - Se = 1.99 Å). 8b crystallizes in the triclinic space group P1̄ (a = 9.935(2). b = 11.507(2), c = 16.646(3) Å, α = 90.91(1), β = 112.00(1), γ = 96.60(1)°, V = 1749.15 A3, ϱx = 1.741 gcm-3, Z = 2). Refinement of 382 parameters on 5096 structure factors converged at R = 0.043. The molecular structure shows close similarities to the selenium adduct 3 (C-I = 2.12 Å).

scholarly journals Structural and Spectroscopic Properties of Two New Isostructural Complexes of Lapacholate with Cobalt and Copper

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
R. A. Farfán ◽  
J. A. Espíndola ◽  
M. I. Gomez ◽  
M. C. L. de Jiménez ◽  
M. A. Martínez ◽  
...  
Keyword(s):  
Electronic Absorption Spectra ◽  
Spectroscopic Properties ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Phenol Oxygen ◽  
Oxygen Atoms

The molecular structures of two isostructural complexes of lapacholate (Lap) anion and dimethylformamide (DMF), M(Lap)2(DMF)2 with M: Co Cu, were determined by X-ray diffraction methods. The substances crystallize in the triclinic space group P1¯ with one molecule per unit cell and cell constants a=7.7591(3), b=10.3560(3), c=11.2224(4) Å, α=95.110(2), β=94.310(2), and γ=107.704(2)° for the Co complex and a=7.9308(2), b=10.0033(4), c=10.7508(4), α=97.387(2), β=93.621(2), and γ=103.980(2)° for the Cu complex. The structures were solved from 2933 (Co) and 2888 (Cu) reflections with I>2σ (I) and refined by full matrix least squares to agreement R1-factors of 0.041 (Co) and 0.033 (Cu). The metal M(II) ion is sited on a crystallographic inversion center in a MO6 distorted octahedral environment. This ion is coordinated equatorially to two lapacholate anions through their adjacent carbonyl and phenol oxygen atoms [M–O bond distances of 2.134(1) and 2.008(1) Å (Co) and 2.301(1) and 1.914(1) Å (Cu)] and axially to two DMF molecules through oxygen atoms [M–O bond lengths of 2.143(1) Å (Co) and 2.069(1) Å (Cu)]. The solid state IR transmittance and solution electronic absorption spectra of both Co and Cu compounds are also reported and compared to each other and to the corresponding spectra of other members of the lapacholate metal family of complexes.

Cation movement and phase transitions in KTP isostructures; X-ray study of sodium-doped KTP at 10.5 K

2003 ◽  
Vol 59 (3) ◽  
pp. 353-360 ◽  
Author(s):  
Stefan T. Norberg ◽  
Alexander N. Sobolev ◽  
Victor A. Streltsov
Keyword(s):  
Metal Ion ◽  
Room Temperature ◽  
Second Harmonic ◽  
Temperature Data ◽  
Potassium Titanyl Phosphate ◽  
Structure Model ◽  
Alkaline Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Framework

An accurate structure model of sodium-doped potassium titanyl phosphate, (Na0.114K0.886)K(TiO)2(PO4)2, has been determined at 10.5 K by single-crystal X-ray diffraction. In addition to the low-temperature data, X-ray intensities have been collected at room temperature. When the temperature was decreased from room temperature to 10.5 K, both potassium cations moved 0.033 (2) Å along the c-axis, i.e. in the polar direction within the rigid Ti—O—P network. This alkaline metal ion displacement can be related to the Abrahams–Jamieson–Kurtz T C criteria for oxygen framework ferroelectrics. Potassium titanyl phosphate (KTP) is a well known material for second harmonic generation (SHG), and the influence of sodium dopant on the TiO6 octahedral geometry and SHG is discussed. The material studied crystallizes in the space group Pna21 with Z = 4, a = 12.7919 (5), b = 6.3798 (4), c = 10.5880 (7) Å, V = 864.08 (9) Å3, T = 10.5 (3) K and R = 0.023.

Phase transitions in KTP isostructures: correlation between structure and T c in germanium-doped RbTiOPO4

2003 ◽  
Vol 59 (5) ◽  
pp. 588-595 ◽  
Author(s):  
Stefan T. Norberg ◽  
Joacim Gustafsson ◽  
Bengt-Erik Mellander
Keyword(s):  
Phase Transition ◽  
Transition Temperature ◽  
Room Temperature ◽  
Dielectric Measurements ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
The Relationship ◽  
Germanium Concentration

Crystals of germanium-doped rubidium titanyl phosphate, Rb2(Ti)(Ge0.121Ti0.879)O2(PO4)2 (GeRTP#1) and Rb2(Ge0.125Ti0.875)(Ge0.225Ti0.775)O2(PO4)2 (GeRTP#2), have been structurally characterized from X-ray diffraction data at room temperature. In addition, a third structure, Rb2(TiO)2(PO4)2 (RTP), has been reinvestigated. The exchange of titanium for germanium results in a less distorted octahedral coordination around the two crystallographically independent titanium sites. Additionally, rubidium split-cation positions have been found in these doped RTP crystals. Dielectric measurements show that the phase-transition temperature, T c , decreases with increasing germanium concentration, and a direct correlation between the room-temperature split of the rubidium cations and T c has been discovered. General trends regarding the relationship between the room-temperature structures of KTP-like compounds and their T c values are discussed.

X-Ray Diffraction Studies on Ti-Pd Shape Memory Alloys

2014 ◽  
Vol 783-786 ◽  
pp. 2517-2522
Author(s):  
Raju Arockiakumar ◽  
Madoka Takahashi ◽  
Satoshi Takahashi ◽  
Yoko Yamabe-Mitarai
Keyword(s):  
Phase Transformation ◽  
Shape Memory ◽  
Low Temperatures ◽  
Periodic Table ◽  
Room Temperature ◽  
Group Iv ◽  
X Ray Diffraction ◽  
Transformation Behavior ◽  
X Ray ◽  
B2 Phase

The phase transformation behavior of Ti-50Pd-5x (x =Zr, Hf, V, Nb, Ta, Cr, Mo, W) (at.%) alloys was studied by X-ray diffraction measurements from room temperature to 800 oC. In all the alloys, B19 martensite was observed at room temperature and it transformed to B2 phase upon heating. In addition, peaks corresponding to formation of (Ti, x)2Pd3 phase was seen for all the alloys. However, the temperature of formation of (Ti, x)2Pd3, interestingly, varied with respect to the elements group from the periodic table. Elements except from group IV (Zr and Hf) have been identified to accelerate the formation of (Ti, x)2Pd3 phase even at low temperatures (~400 oC).

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