Crystal Structures, Mössbauer Spectra and Reactivity of Sn,II Salicylideneimines

1990 ◽  
Vol 43 (9) ◽  
pp. 1559 ◽  
Author(s):  
AM Vandenbergen ◽  
JD Cashion ◽  
GD Fallon ◽  
BO West

Single-crystal X-ray diffraction studies have been carried out on the tetradentate SnII complex N,N′-(4,5-dimethyl-1,2-phenylene ) bis ( salicylideneiminato )tin(II) [ Sn ( saldph )] and the tetradentate complex N-(2-oxidophenyl) salicylideneiminatotin (II) [ Sn ( salop )]. Sn ( saldph ) is a monomer and has the SnII ion 1.126(1)Ǻ above the plane of the O2N2 donors while Sn ( salop ) is dimeric with bridging between SnII ions by the oxygens of the oxidophenyl groups. SnII ions are raised above the O3N donor planes by 1.109(7)Ǻ while the molecules are bent along the bridging O-O axis with a dihedral angle between the chelate planes of 92.1°. The Mossbauer spectra of the complexes are reported. The SnII salicylideneimines react with H2O and oxygen but are inert to alkyl halides.

Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(


1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.


Author(s):  
Amel Kaibi ◽  
Abderrahim Guittoum ◽  
Nassim Souami ◽  
Mohamed Kechouane

Nanocrystalline Ni75Fe25 (Ni3Fe) powders were prepared by mechanical alloying process using a vario-planetary high-energy ball mill. The intermetallic Ni3Fe formation and different physical properties were investigated, as a function of milling time, t, (in the range 6 to 96 h range), using X-Ray Diffraction (XRD) and Mössbauer Spectroscopy techniques. X-ray diffraction were performed on the samples to understand the structural characteristics and get information about elements and phases present in the powder after different time of milling. The refinement of XRD spectra revealed the complete formation of fcc Ni (Fe) disordered solid solution after 24 h of milling time, the Fe and Ni elemental distributions are closely correlated. With increasing the milling time, the lattice parameter increases and the grains size decreases. The Mössbauer experiments were performed on the powders in order to follow the formation of Ni3Fe compound as a function of milling time. From the adjustment of Mössbauer spectra, we extracted the hyperfine parameters. The evolution of hyperfine magnetic field shows that the magnetic disordered Ni3Fe phase starts to form from 6 h of milling time and grow in intensity with milling time. For the milling time more than 24 h, only the Ni3Fe disordered phase is present with a mean hyperfine magnetic field of about 29.5 T. The interpretation of the Mossbauer spectra confirmed the results obtained by XRD.


Mineralogia ◽  
2013 ◽  
Vol 44 (1-2) ◽  
pp. 3-12 ◽  
Author(s):  
Kamaleldin M. Hassan ◽  
Julius Dekan

AbstractOlivine basalts from southern Egypt were studied by 57Fe Mössbauer spectroscopy at 297 and 77 K, and by optical microscopy and X-ray diffraction. The 57Fe Mössbauer spectra show three-magnetic sextets, three doublets of ferrous (Fe2+), and a weak ferric (Fe3+) doublet that is attributable to a nanophase oxide (npOx). The magnetic sextets relate to titanomagnetite and the Fe2+ doublets to olivine, pyroxene, and ulvöspinel. Variations in the hyperfine parameters of the various Fe components are attributed to changes in the local crystal chemistry. The intensity of oxidation (Fe3+/ΣFe) in the rocks varies from 20-27% with the oxidized iron largely residing in the titanomagnetite.


1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.


Author(s):  
William W. Brennessel ◽  
John E. Ellis

The reaction of the [K(18-crown-6)(thf)2]1+ (thf is tetrahydrofuran) salt of bis(anthracene)ferrate(−1), or [Fe(C14H10)2]−, with 2,6-dimethylphenyl isocyanide (CNXyl) in thf resulted in the formation of two new iron isocyanide complexes, namely, [(1,2,3,4-η)-anthracene]tris(2,6-dimethylphenyl isocyanide)iron, [Fe(C14H10)(C9H9N)3] or [Fe(1,2,3,4-η-C14H10)(CNXyl)3], and {5,6-bis(2,6-dimethylanilino)-3-(2,6-dimethylphenyl)-1,2,7-tris[(2,6-dimethylphenyl)imino]-3-azoniahept-3-ene-1,4,7-triido}tris(2,6-dimethylphenyl isocyanide)iron tetrahydrofuran disolvate, [Fe(C54H56N6)(C9H9N)3]·2C4H8O or [Fe(C54H56N6)(CNXyl)3]·2C4H8O, which were characterized by single-crystal X-ray diffraction. The former is likely an intermediate along the path to the known homoleptic [Fe(CNXyl)5], while the latter contains a tridentate ligand that is formed from the `coupling' of six CNXyl ligands. A third crystal structure from this reaction, (7-methylindol-1-ido-κN)(1,4,7,10,13,16-hexaoxacyclooctadecane-κ6 O)potassium, [K(C9H8N)(C12H24O6)] or [K(C9H8N)(18-crown-6)], contains a 7-methylindol-1-ide anion, in which one CNXyl ligand has shed a proton during its reductive cyclization.


1991 ◽  
Vol 10 (4) ◽  
pp. 197-200 ◽  
Author(s):  
S. Musić ◽  
S. Popović ◽  
M. Metikoš-Hukovć ◽  
V. Gvozdić

1985 ◽  
Vol 38 (9) ◽  
pp. 1417 ◽  
Author(s):  
H Becker ◽  
VA Patrick ◽  
BW Skelton ◽  
AH White

The crystal structures of racemic bis [α-(9-anthryl)] ether and its meso form have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.053 and 0.041 for 1868 and 3568 independent 'observed' reflections respectively. Crystals of the racemate are orthorhombic, Pcab, a 23.07(1), b 19.85(2), c 10.241(8) Ǻ, Z 8. Crystals of the meso form are triclinic, Pī , a 19.032(12), b 14.207(11), c 9.451(8) Ǻ, α 79.46(6), β 89.68(6), γ 68.97(5)°, Z 4. In the racemate , the dihedral angle between the methyl groups along the ether bonds is 12°, and the short axes of the anthracene moieties lie at an angle of about 120°. In the meso compound, for the two molecules the dihedral angles between the methyl groups along the ether bonds are 90 and 93°, the angle between the two anthracene moieties is 90°, and the interplanar angles between the partly overlapping aromatic systems are 46 and 43°.


2002 ◽  
Vol 57 (10) ◽  
pp. 1090-1100
Author(s):  
Franziska Emmerling ◽  
Caroline Röhr

AbstractThe title compounds were synthesized at a temperature of 700 °C via oxidation of elemental Bi with the hyperoxides AO2 or via reaction of the elemental alkali metals A with Bi2O3. Their crystal structures have been determined by single crystal x-ray diffraction. They are dominated by two possible surroundings of Bi by O, the ψ-trigonal-bipyramidal three (B) and the ψ-tetrahedral four (T) coordination. Cs6Bi4O9 (triclinic, spacegroup P1̄, a = 813.82(12), b = 991.60(14), c = 1213.83(18) pm, α = 103.658(2), β = 93.694(3), γ = 91.662(3)°, Z = 2) contains centrosymmetric chain segmentes [Bi8O18]12- with six three- (T) and two four-coordinated (B) Bi(III) centers. K9Bi5O13 (monoclinic, spacegroup P21/c, a = 1510.98(14), b = 567.59(5), c = 2685.6(2) pm, β = 111.190(2)°, Z = 4) is a mixed valence compound with isolated [BivO4]3- tetrahedra and chains [BiIII4O9]6- of two T and two B coordinated Bi. In the compounds A2Bi4O7 (A = Rb/Cs: monoclinic, C2/c, a = 2037.0(3) / 2130.6(12), b = 1285.5(2) / 1301.9(7), c = 1566.6(2) / 1605.6(9) pm, β = 94.783(3) / 95.725(9)°, Z = 8) ribbons [Bi4O6O2/2]2- are formed, which are condensed to form a three-dimensional framework.


1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.


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