Cyano-Bridged Bimetallic Complexes of Copper(II) with Nitroprusside. Crystal Structure of [Cu(H2NCH2CH(NH2)CH3)2Fe(CN)5NO] . H2O

2000 ◽  
Vol 53 (3) ◽  
pp. 225 ◽  
Author(s):  
Zdenek Smékal ◽  
Zdenek Trávnícek ◽  
Jaromír Marek ◽  
Milan Nádvornik

Five new complexes of compositions [Cu(1,2-pn)2Fe(CN)5NO]·H2O (1,2-pn = propane-1,2-diamine) and [Cu(L)Fe(CN)5NO]·xH2O (L = tmen (N,N,N′,N′-tetramethylethane-1,2-diamine), x = 0.5; L = trimeen (N,N,N′-trimethylethane-1,2-diamine), x = 1; L = dien (N-(2-aminoethyl)ethane-1,2-diamine), x = 0; L = medpt (N-(3-aminopropyl)-N-methylpropane-1,3-diamine), x = 2) have been isolated from the reaction mixture of Cu(ClO4)2·6H2O (or CuCl2·2H2O), the amine and Na2 [Fe(CN)5NO]·2H2O in water. The complexes have been characterized by infrared and ultraviolet–visible spectroscopies, and magnetic measurements. Single-crystal X-ray structural analysis revealed that the [Cu(1,2-pn)2Fe(CN)5NO]·H2O complex assumes a cyanide-bridged binuclear structure in which iron(II) is six-coordinated by five cyanide ligands and one nitrosyl group (the nitrosyl group lies cis to the bridging cyanide group), while copper(II) is five-coordinated by two propane-1,2-diamine ligands and a bridging cyanide ligand in a distorted tetragonal pyramidal arrangement.

1995 ◽  
Vol 73 (1) ◽  
pp. 95-99 ◽  
Author(s):  
Frank E. Smith ◽  
Rosemary C. Hynes ◽  
John Tierney ◽  
Ying Z. Zhang ◽  
George Eng

The title compound was synthesized as part of an effort to produce a more effective fungicide to combat Dutch Elm Disease (DED), which is caused by the fungus Ceratocystisulmi. A full X-ray structural analysis of the 1:1 adduct has been carried out and the results are reported along with the Mössbauer data for the compound. The crystals are monoclinic, space group P21/a with a = 19.240(3) Å, b = 9.1463(24) Å, c = 19.3512(24) Å, β = 118.874(8)°, V = 2982.0(10) Å3, z = 4, and Dcalc = 1.427 Mg m−3. The final discrepancy factors are RF = 0.056 and Rw = 0.058 for 1915 significant reflections. The QS and IS values in the Mössbauer spectrum of the complex are 3.08 mm s−1 and 1.28 mm s−1, respectively. The 2,3-diphenylthiazolidin-4-one behaves as a monodentate ligand and coordinates to the tin through the oxygen atom. The complex exhibits a trigonal bipyramidal configuration with the three phenyl groups in equatorial positions and the chloride and ligand oxygen occupying the apical sites. Keywords: triorganotin, fungicide, Dutch Elm Disease, thiazolidin-4-one.


2017 ◽  
Vol 73 (10) ◽  
pp. 1497-1500
Author(s):  
Khamid U. Khodjaniyazov ◽  
Utkir S. Makhmudov ◽  
Kambarali K. Turgunov ◽  
Burkhon Z. Elmuradov

Selective C-formylation of 8,9,10,11-tetrahydropyrido[2′,3′:4,5]pyrimido[1,2-a]-azepin-5(7H)-one has been studied for the first time. It was revealed that formylation proceeds by the formation of an intermediate salt, which due to the re-amination process on treatment with aqueous ammonia transformed into the corresponding (E)-11-(aminomethylene)-8,9,10,11-tetrahydropyrido[2′,3′:4,5]-pyrimido[1,2-a]azepin-5(7H)-one, C13H14N4O, as anE-isomer. Formylation was carried out by Vilsmeier–Haack reagent and the structure of the synthesized compound was confirmed by X-ray structural analysis, spectroscopic and LC–MS methods. In the molecule, the seven-membered pentamethylene ring adopts a twist-boat conformation.


2005 ◽  
Vol 473-474 ◽  
pp. 117-122 ◽  
Author(s):  
A.C. Kis ◽  
Th. Leventouri ◽  
J.R. Thompson

Structure and magnetic properties of ferrimagnetic bioceramics in the system {0.45(CaO, P2O5) ySiO2 xFe2O3 0.03Na2O}, x=0.05, 0.10, 0.15, 0.20, were studied by x-ray powder diffraction and magnetic measurements. Magnetite and calcium phosphate, crystallizing in the hexagonal and monoclinic crystal systems, are the major phases in the compounds. Phase development, crystal structure, and magnetic properties of the composites are determined by the specific starting composition of oxides and the heat-treatment temperature.


2001 ◽  
Vol 56 (10) ◽  
pp. 1025-1034 ◽  
Author(s):  
Markus Ströbele ◽  
H.-Jtirgen Meyer

The title compounds were prepared through reactions of Li2Nb6Cl16 with the corresponding crown ethers in acetone. All three compounds were obtained as dark brown crystals. Their structures were solved with the means of single-crystal X-ray diffraction.[Li(12-crown-4)2][Li(12-crown-4)(OH2)]2[Nb6Cl18]: space group P21/n, Z =2, a = 1320.4(1), b = 1879.1(1), c = 1321.7(1) pm, ß = 92.515(6)°, R1 = 0.0297 (I>2σ(I)). The crystal structure contains Li+ sandwiched by two 12-crown-4-ethers plus Li+ coordinated by one 12-crown-4- ether and one water molecule.[Li(15-crown-5)2(OH2)]3[Nb6Cl18]: space group R3̅, Z = 3, a = b = 2081.7(1), c = 1991.7(1) pm, R1 = 0.0395 (I > 2σ(I)). In the crystal structure Li+ and one water molecule are sandwiched by two 15-crown-5-ethers.[(18-crown-6)2(O2H5)]3[Nb6Cl18]: space group P1̅, Z = 1 ,a = 1405.1(1), b = 1461.1(2), c = 1492.2(2) pm; α = 98.80(1)°, ß = 98.15(1)°, γ = 97.41(1)°, R1 = 0.0538 (I > 2σ(I)). H5O2+ was found in the structure refinement sandwiched between two 18-crown-6-ethers.All compounds reported contain [Nb6Cl18] clusters with Nb-Nb distances between 299 and 301 pm. The paramagnetic behaviour expected for [Nb6Cl18]3- in all three compounds was confirmed by magnetic measurements.


ChemInform ◽  
2010 ◽  
Vol 28 (48) ◽  
pp. no-no
Author(s):  
O. OLEKSYN ◽  
P. SCHOBINGER-PAPAMANTELLOS ◽  
J. RODRIGUEZ-CARVAJAL ◽  
E. BRUECK ◽  
K. H. J. BUSCHOW

1992 ◽  
Vol 47 (6) ◽  
pp. 814-818 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred Dirk Bacher ◽  
Gertraude Koellner ◽  
Birgit Siewert ◽  
Ulrich Müller

Reaction of VC14 with (Me3Si)2S in CH2C12 yields an insoluble product with the approximate composition VSC12. Its reaction with PPh4Cl in CH2Cl2 affords (PPh4)3[V2Cl9] · 7 CH2Cl2, whereas PPh4[VOCl4] is formed in the presence of oxygen. According to an X-ray crystal structure analysis, (PPh4)3[V2Cl9] · 7 CH2Cl2 contains [V2C19]3- ions having two face-sharing coordination octahedra but no significant metal-metal bonding (V-V distance 327.5 pm). Crystal data: a = 1386.4(7), b = 1405.6(7), c = 2710(2) pm, α = 95.800(5), β = 95.370(5), γ = 118.11(3)°, triclinic, Ρ 1̄, Ζ = 2; R = 0.066 for 8779 observed reflexions. PPh4[VOCl4] is isotypic with AsPh4[VOCl4] and contains tetragonal-pyramidal [VOCl4]- ions; tetragonal, P4/n, Z = 2, a = 1264.5(2), c = 772.0(2) pm; R = 0.050 for 654 observed reflexions.


2014 ◽  
Vol 644-650 ◽  
pp. 4950-4955 ◽  
Author(s):  
Li Mei Sun ◽  
Song Bai Han ◽  
Yun Tao Liu ◽  
Dong Feng Chen ◽  
Xiang Feng Liu

The synergetic effects of the substitution of Ti and Si for Fe on the crystallographic structure and magnetic properties of Nd2Fe17-x-yTixSiycompounds have been comprehensively investigated by means of x-ray diffraction, neutron diffraction and magnetic measurements. Rietveld refinements of the diffraction data indicate that all the samples crystallize in the rhombohedral Th2Zn17-type structure. For a given Ti content, thea-axis and the unit cell volumeVof Nd2Fe17-x-yTixSiydecrease linearly with increasing silicon content, while thec-axis behaves complicatedly dependent on different Ti content. The site occupancies of Ti and Si in the crystallographic sites significantly change compared to what is observed in the corresponding singly substituted compounds. TheTCof doubly substituted Nd2Fe16.5-yTi0.8Siyand Nd2Fe16.5-yTi0.5Siyis higher than that of singly substituted Nd2Fe16-ySiyfor a lower Si content while the converse behavior is observed for a higher Si content. For a given Ti content, theTCof Nd2Fe17-x-yTixSiycompounds increases with increasing Si content and theMsfirst increases and then decreases. TheMsof Nd2Fe17-x-yTixSiydecreases with the increase of Ti content.


2001 ◽  
Vol 66 (10) ◽  
pp. 1490-1498 ◽  
Author(s):  
Zdeněk Smékal ◽  
Jiří Kameníček ◽  
Ingrid Svoboda ◽  
Albert Escuer

The novel complex [μ-(NC)-Fe(CN)3(NO)-μ-(CN)-Cu(ept)]n·4nH2O (ept = N-(2-aminoethyl)- propane-1,3-diamine) was obtained by the reaction of Cu(ClO4)2·6H2O with N-(2-amino- ethyl)propane-1,3-diamine and Na2[Fe(CN)5NO]·2H2O in water. This compound was characterized by IR, UV-VIS and EPR spectroscopies and magnetic measurement. Single-crystal X-ray structure analysis revealed that the title complex has a one-dimensional polymeric structure containing hexacoordinate iron(II) with five cyanide ligands (two of them, in trans position, bridging) and one nitrosyl group, and pentacoordinate copper(II) with N-(2-aminoethyl)propane-1,3-diamine and two sites occupied by bridging cyanide ligands. Magnetic investigation revealed a very weak antiferromagnetic interaction between the copper atoms (superexchange interaction parameter J = -1.7(1) cm-1; H = -JSiSi+1) within the chain through the diamagnetic [Fe(CN)5NO]2- ions.


ChemInform ◽  
2005 ◽  
Vol 36 (47) ◽  
Author(s):  
Sabir H. Mashraqui ◽  
Mamta B. Patil ◽  
Yogesh Sangvikar ◽  
Mohamed Ashraf ◽  
Hitesh D. Mistry ◽  
...  

1992 ◽  
Vol 47 (7) ◽  
pp. 925-928 ◽  
Author(s):  
Joachim Mündelein ◽  
Hans-Uwe Schuster

Three new ternary compounds MnCuP, MnCuP0.5As0.5 and MnCuAs have been prepared and characterized by X-Ray, DTA and magnetic measurements. They crystallize orthorhombically in the space group P nma (No. 62). The structures were calculated from single crystal data. The melting points were determined by DTA measurements (MnCuP: 1090°C; MnCuP0.5As0.5: 1000 °C; MnCuAs: 950 °C). MnCuAs appears to show an antiferromagnetic ordering up to 295 K.


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