Synthesis, Structure Determination, and Magnetic Properties of [Cr3(dpa)4Cl2][CuCl2], a Compound Comprising a Trinuclear Chain Cation

2012 ◽  
Vol 67 (8) ◽  
pp. 759-764 ◽  
Author(s):  
Dilahan Aydin-Cantürk ◽  
Hanne Nuss Max-Planck
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Partial Oxidation ◽  
Ethyl Ether ◽  
Structure Determination ◽  
Magnetic Moment ◽  
Effective Magnetic Moment ◽  
X Ray ◽  
Weiss Constant ◽  
Paramagnetic Behavior

The new compound [Cr3(dpa)4Cl2][CuCl2] (1) (dpa = di-2,2'-pyridylamido) was synthesized by reacting Cr2(dpa)4 and anhydrous CuCl2 in dry tetrahydrofuran. Partial oxidation of Cr2(dpa)4 by Cu(II) forms Cr3+ ions, which coordinate to the free N donor atoms of the dpa ligands, and led to the formation of a trinuclear chain cation [Cr3(dpa)4Cl2]+. Recrystallization from CH2Cl2/ethyl ether yielded dark-brown, block-shaped crystals suitable for X-ray structure determination (Pccn (no. 56), a=1246:8(5), b=1487:3(3), c=2184:8(1) pm, V =4051.6(8) ·106 pm3, Z =4). The crystal structure is composed of discrete [Cr3(dpa)4Cl2]+ cations and [CuCl2]- anions. The Cr3 chain comprises quadruply-bonded diamagnetic (Cr2)4+ dimers and a pseudo-octahedrally coordinated, paramagnetic Cr3+ ion, manifesting itself in the effective magnetic moment μeff of 3:54μB (d3, S = 3=2) and the almost ideal Curie-paramagnetic behavior observed between 2 and 300 K with a Weiss constant θ = -0:25(4)K and χ0 = 4:9(7)×10-4 emu mol-1

Crystal Structure and Magnetic Properties of (2,2'-Dipyridyl)-(2-acetylphenolato)copper(II) Perchlorate

2002 ◽  
Vol 57 (10) ◽  
pp. 1129-1132 ◽  
Author(s):  
A. Elmali ◽  
Y. Elerman ◽  
I. Svoboda
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Magnetic Moment ◽  
Basal Plane ◽  
Effective Magnetic Moment ◽  
Mixed Ligand ◽  
Magnetic Susceptibility Data ◽  
Susceptibility Data ◽  
Dimeric Unit

The mixed-ligand dinuclear complex (2,2'-dipyridyl)-(2-acetylphenolato)copper(II) perchlorate was synthesized and its crystal structures determined. The structure consists of a dimeric unit involving a planar Cu2O2 group. The coordination sphere of the Cu atom can be described as an alongated octahedron where the basal plane is formed by the two N atoms of the 2,2'-dipyridyl molecule and the two O atoms of the acetophenon anion. Two apical Cu - O contacts complete the 4+2 coordination of the Cu atoms. They correspond to one of the O atoms of the perchlorate anion and to the O atom of the second unit. Magnetic susceptibility data obey the Curie-Weiss law with θ = -8.1(2) K. The decreasing of the effective magnetic moment from 1.94(8) μB at 300 K to 1.86(8) μB at 70 K and the negative Weiss constant indicate weak antiferromagnetic interactions between the two copper atoms in the dimeric units.

Structure and Magnetic Properties of a Dinuclear Complex with Iron(III) in Octahedral and Pyramidal Coordination

1994 ◽  
Vol 49 (9) ◽  
pp. 1239-1242 ◽  
Author(s):  
Ayhan Elmali ◽  
Yalcin Elerman ◽  
Ingrid Svoboda ◽  
Hartmut Fuess ◽  
Klaus Griesar ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Magnetic Moment ◽  
Effective Magnetic Moment ◽  
Dinuclear Complex ◽  
Monoclinic Space Group ◽  
Temperature Dependent ◽  
Space Group ◽  
Binuclear Unit

[FeL(MeOH)Cl]2 (L = N-(2-hydroxyphenyl)salicylaldimine) was synthesized and its crystal structure determined, [C27H20N 2O5Cl2Fe2], monoclinic, space group P21/c, a = 9.528(1), b = 7.684(1), c = 18.365(2) Å, β = 109.83(1)°, V = 1264.8 Å3, Z = 2. Two identical [FeL(MeOH)Cl] fragments, related by an inversion centre, are combined by the two bridging O atoms, to form a binuclear unit. The iron(III) centers are separated by 3.163(2) Å and weakly antiferromagnetically coupled (J = -8 .0 (1 ) cm-1), which follows from temperature - dependent magnetic susceptibility measurements in the range 4.2 to 288 K. The effective magnetic moment per iron(III) is μeff = 7.4 μB at 288 K

Preparation and Magnetic Properties of Nanocrystalline (Fe,Cr)-N

2012 ◽  
Vol 625 ◽  
pp. 222-225
Author(s):  
Wen Jiang Feng ◽  
Chuan Yin Wang ◽  
Hao Hua Zhang
Keyword(s):  
Crystal Structure ◽  
Solid Solution ◽  
Magnetic Properties ◽  
Magnetic Moment ◽  
Single Phase ◽  
Nitrogen Atmosphere ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nano Crystalline ◽  
Intrinsic Magnetic Moment

The nano-crystalline (Fe,Cr)N was prepared as a single phase by milling Fe80Cr20 in a nitrogen atmosphere. Its crystal structure is determined to be the cubic rock salt-type CrN by X-ray diffraction measurements. The nano-crystalline is stable up to above 773 K and decomposes into (Fe,Cr)N and Fe-Cr solid solution. Due to the combination of Fe atoms and N ones, the intrinsic magnetic moment of Fe atoms is reduced, which is confirmed by our measurements.

Darstellung, Eigenschaften und Kristallstruktur von Rhenium(VII)-Nitridchlorid, ReNCl4 / Preparation, Properties and Crystal Structure of Rhenium(VII) Nitride Chloride, ReNCl4

1979 ◽  
Vol 34 (5) ◽  
pp. 693-696 ◽  
Author(s):  
Werner Liese ◽  
Kurt Dehnicke ◽  
Ingeborg Walker ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Mass Spectrum ◽  
Magnetic Moment ◽  
Effective Magnetic Moment ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Molecular Ion ◽  
Bond Lengths ◽  
Nitrogen Trichloride

Abstract Rhenium(VII) nitride chloride, ReNCl4, is prepared by the reaction of ReCl5 with nitrogen trichloride. It forms metallic glazing, hygroscopic needles with an effective magnetic moment of 0.23 B.M. In the mass spectrum only the molecular ion ReNCl4⊕ is present, followed by ReNCl3⊕. The crystal structure was determined by X-ray diffraction methods (space group Il, 265 independent reflexions, R = 0.071). The structure consists of ReNCl4 units, which are linked by strongly alternated Re ≡ N-Re chains with different bond lengths of r Re ≡ N = 158 pm and r Re-N = 248 pm. The structure is very similar to that of WOCl4.

Synthese und Kristallstruktur von MoCl4(DME) · 15-Krone-5 und MoCl4(DME) (DME = 1,2-Dimethoxyethan) / Synthesis and Crystal Structure of MoCl4(DME) · 15-Crown-5 and MoCl4(DME) (DME = 1,2-Dimethoxyethane)

1991 ◽  
Vol 46 (3) ◽  
pp. 307-314 ◽  
Author(s):  
Evamarie Hey-Hawkins ◽  
Hans Georg von Schnering
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Work Up

NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME)· 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P212121 (No. 19), Z = 4, 2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2) Å. 2, space group I4̄2d (No. 122), Z = 8, 558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.562(2), c = 23.777(6)Å. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.

Synthesis, crystal structure and magnetic characterization of a cyanide-bridged Mo–Ni nanosized molecular wheel

2015 ◽  
Vol 70 (8) ◽  
pp. 527-531 ◽  
Author(s):  
Daopeng Zhang ◽  
Lingqian Kong ◽  
Hongyan Zhang ◽  
Ping Wang
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Building Blocks ◽  
Antiferromagnetic Coupling ◽  
X Ray Diffraction ◽  
Magnetic Characterization ◽  
X Ray

AbstractBy using K4[Mo(CN)8] and [Ni(L)(H2O)2][ClO4]2 as reagents (L = 2,12-dimethyl-3,7,11,17-tetraazabicyclo [11.3.1]heptadeca-1(17),13,15-triene), a new cyanide-bridged Mo–Ni complex containing the building blocks [Ni(H2O)(L)]2+ and [Ni(L)]2+ bridged by [Mo(CN)8]4− units has been obtained. The complex with the formula {[Ni(H2O)(L)][Ni(L)][Mo(CN)8]}6 · 36H2O · 2CH3OH (1) was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The structure determination reveals an octadecanuclear cluster in the form of a 36-membered macrocycle, in which the largest intramolecular W···W and Ni···Ni distances are 16.5 and 14.4 Å, respectively, indicating that complex 1 is a nanosized molecular wheel. Investigation of its magnetic properties has shown weak antiferromagnetic coupling between the adjacent Ni(II) ions bridged by the diamagnetic [Mo(CN)8]4− ions.

A study on α-RuCl3 crystal structure by scanning tunneling microscopy

1989 ◽  
Vol 47 ◽  
pp. 30-31
Author(s):  
H.-J. Cantow ◽  
H. Hillebrecht ◽  
S. Magonov ◽  
H. W. Rotter ◽  
G. Thiele
Keyword(s):  
Crystal Structure ◽  
Density Distribution ◽  
Scanning Tunneling Microscopy ◽  
Electron Density ◽  
Structure Determination ◽  
Electron Density Distribution ◽  
Scanning Tunneling ◽  
Monoclinic Space Group ◽  
Tunneling Microscopy ◽  
X Ray

From X-ray analysis, the conclusions are drawn from averaged molecular informations. Thus, limitations are caused when analyzing systems whose symmetry is reduced due to interatomic interactions. In contrast, scanning tunneling microscopy (STM) directly images atomic scale surface electron density distribution, with a resolution up to fractions of Angstrom units. The crucial point is the correlation between the electron density distribution and the localization of individual atoms, which is reasonable in many cases. Thus, the use of STM images for crystal structure determination may be permitted. We tried to apply RuCl3 - a layered material with semiconductive properties - for such STM studies. From the X-ray analysis it has been assumed that α-form of this compound crystallizes in the monoclinic space group C2/m (AICI3 type). The chlorine atoms form an almost undistorted cubic closed package while Ru occupies 2/3 of the octahedral holes in every second layer building up a plane hexagon net (graphite net). Idealizing the arrangement of the chlorines a hexagonal symmetry would be expected. X-ray structure determination of isotypic compounds e.g. IrBr3 leads only to averaged positions of the metal atoms as there exist extended stacking faults of the metal layers.

The protonation of the ethylenediphosphinetetraacetate anion and the crystal structure of the bis (hydrogen bromide) of ethylenediphosphinetetraacetic acid

1981 ◽  
Vol 46 (12) ◽  
pp. 3063-3073 ◽  
Author(s):  
Jana Podlahová ◽  
Bohumil Kratochvíl ◽  
Vratislav Langer ◽  
Josef Šilha ◽  
Jaroslav Podlaha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Free Acid ◽  
Hydrogen Bromide ◽  
Carboxyl Groups ◽  
Spectroscopic Methods ◽  
X Ray ◽  
Partial Formation

The equilibria and mechanism of addition of protons to the ethylenediphosphinetetraacetate anion (L4-) were studied in solution by the UV, IR, 1H and 31P NMR spectroscopic methods. A total of six protons can be bonded to the anion. They are added stepwise, first with partial formation of zwitterions containing P-H bonds, which then dissociate with formation of the free acid, H4L, where all four protons are bonded in carboxyl groups. The formation of zwitterions is strongly dependent on the concentration. In the final stage, the acid bonds two additional protons to form the bis-phosphonium cation, H6L2+. A number of isostructural salts containing this cation, H4L.2 HX (X = Cl, Br, I), have been prepared. The X-ray crystal structure determination of the bromide confirmed the expected arrangement. The bromide crystals are monoclinic, a = 578.2, b = 1 425.0, c = 1 046.7 pm, β = 103.07° with a space group of P21/c, Z = 2. The final R factor was 0.059 based on 1 109 observed reflections. The structure consists of H6L2+ cations containing protons bonded to phosphorus atoms (P-H distance 134 pm) and of bromide anions, located in gaps which are also sufficiently large for I- anions in the isostructural iodide. The interbonding of phosphonium cations proceeds through hydrogen bonds, C-OH...O=C, in which the O...O distance is 275.3 pm.

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