scholarly journals Synthesis and crystal structures of two new tin bis(carboranylamidinate) complexes

2017 ◽  
Vol 73 (10) ◽  
pp. 1443-1448 ◽  
Author(s):  
Nicole Harmgarth ◽  
Phil Liebing ◽  
Philipp Hillebrand ◽  
Sabine Busse ◽  
Frank T. Edelmann
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Structure Analysis ◽  
Lone Pair ◽  
Main Reaction ◽  
Similar Reaction ◽  
Main Reaction Product ◽  
X Ray ◽  
Trigonal Bipyramidal Coordination ◽  
Trigonal Bipyramidal

Reaction of 2 equiv. of the lithium carboranylamidinate Li[o-(C2H10B10)C(NCy)(NHCy)] with SnCl2in THF afforded the stannylene compound bis(N,N′-dicyclohexylamidinatocarboranate)tin(II), SnII[o-(C2H10B10)C(NCy)(NHCy)]2(1). A similar reaction of SnCl4with 2 equiv. of Li[o-(C2H10B10)C(NiPr)(NHiPr)] unexpectedly afforded the known solvated pentachloridostannate(IV) salt [Li(THF)4][SnCl5(THF)] as the main reaction product. Small amounts of the new chlorido-tin(IV) bis(carboranylamidinate) bis(N,N′-diisopropylamidinatocarboranate)chloridotin(IV), SnIVCl[o-(C2H10B10)C(NiPr)(NHiPr)][o-(C2H10B10)C(NiPr)2] (2), were isolated as a by-product. Single-crystal X-ray structure analysis revealed aκC,κN-chelating coordination of the carboranylamidinate ligands in both1and2. The Sn atom in1adopts a pseudo-trigonal–bipyramidal coordination under participation of a stereoactive lone pair. In2, a trigonal–bipyramidal coordination of Sn is completed by a chlorido ligand.

Die neuen Oxobismutate(III) Cs6Bi4O9, K9Bi5O13 und A2Bi4O7 (A = Rb, Cs) / The New Oxobismutates(III) Cs6Bi4O9, K9Bi5O13 and A2Bi4O7 (A = Rb, Cs)

2002 ◽  
Vol 57 (10) ◽  
pp. 1090-1100
Author(s):  
Franziska Emmerling ◽  
Caroline Röhr
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Alkali Metals ◽  
Mixed Valence ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Mixed Valence Compound

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.

scholarly journals Darstellung und Kristallstrukturen von (PH4P)4Sb8I28 und (Ph4P)Sb3I10(Ph = C6H5) / Synthesis and Crystal Structures of (PH4P)4Sb8I28 and (Ph4P)Sb3I10(Ph = C6H5)

1987 ◽  
Vol 42 (12) ◽  
pp. 1493-1499 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Detlev Haase
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Lone Pair ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Polymeric Chains ◽  
Bond Strengths

AbstractThe compounds (Pn4P)4Sb8I28 (1) and (Ph4P)Sb3I10 (2) were prepared by the reaction of SbI3 and Ph4PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data.1 crystallizes in the triclinic space group P1̄ with a - 1321.7(5). b = 1346.7(5), c = 2201.8(8) pm, α = 104.18(2). β = 99.92(2), γ = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, β = 100.75(1)°.Whereas 1 exhibits isolated Sb8I284- ions, the anions of 2 are built up of polymeric chains [Sb3I10- ]∞. In both compounds the distorted Sbl6 octahedra are linked by common edges. The Sb-I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry, the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb-I bond strengths and the different bridges formed by iodine.The lone pair of Sb(III) seems to be predominantly 5 s2.

Combination of Pyridinium and Isoquinolinium Ylides with Phenylisocyanate and Isothiocyanates: Synthesis, Characterisation, and X-Ray Crystal Structures of Mesoionic Monosubstituted 3-Oxo-Propanamides or Thioamides

2015 ◽  
Vol 68 (10) ◽  
pp. 1577
Author(s):  
Mohammad Seifi ◽  
S. Yousef Ebrahimipour ◽  
Jim Simpson ◽  
Michal Dusek ◽  
Vaclav Eigner ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Similar Reaction ◽  
X Ray ◽  
Pyridinium Ylides

Pyridinium ylides derived from 2-bromoacetophenone or methyl bromoacetate have been reacted with phenylisocyanate, phenyl- or methylisothiocyanate to afford mesoionic monosubstituted 3-oxo-propanamides or thioamides, via self-protonation of the intermediate N-anion. A similar reaction under the same conditions of isoquinolinium ylides with phenylisocyanate or phenyisothiocyante also produced the corresponding mesoionic compounds. In order to establish the exact structure of the mesoionic compounds, single crystal X-ray structures were obtained for three of the pyridinium ylides.

Halogeno-und Pseudohalogeno-tris(pentahaptocyclopentadienyl)uran(IV)- Komplexe als Lewis-Säuren: Darstellung und Struktur trigonal-bipyramidaler Uran-Organyle des Typs [(η5 -C5H5)3UXL] / Tris(pentahaptocyclopentadienyl)uranium(IV) Halides and Pseudohalides as Lewis-Acids: Preparation and Structure of Uranium Organyls [(η5 -C5H5)3UXL] with Trigonal-Bipyramidal Coordination

1978 ◽  
Vol 33 (12) ◽  
pp. 1393-1397 ◽  
Author(s):  
R. D. Fischer ◽  
E. Klähne ◽  
J. Kopf
Keyword(s):  
Structure Analysis ◽  
Lewis Acids ◽  
Lewis Base ◽  
Lewis Acidity ◽  
X Ray ◽  
Trigonal Bipyramidal Coordination ◽  
Trigonal Bipyramidal ◽  
Linear Alignment ◽  
Specific Reactions

Abstract The first two examples of a novel series of organo-actinide complexes, [Cp3UXL] (Cp = η5 -C5H5, X = halide or pseudohalide anion, L = uncharged Lewis base), are described. The X-ray structure analysis of the system with X = NCS and L = CH3CN confirms an almost linear alignment (H3)CCNUNCS along with the coplanarity of the three Cp ring normals. The remarkable Lewis acidity of certain Cp3UX-compounds appears to be essential for the formation of oligomeric species [Cp3UX]∞ as well as for specific reactions of monomeric CP3UX.

Solid-state reaction of Pt thin film with single-crystal (001) β–SiC

1994 ◽  
Vol 9 (3) ◽  
pp. 648-657 ◽  
Author(s):  
J.S. Chen ◽  
E. Kolawa ◽  
M-A. Nicolet ◽  
R.P. Ruiz ◽  
L. Baud ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Single Crystal ◽  
Atomic Scale ◽  
Solid State Reactions ◽  
Main Reaction ◽  
Main Reaction Product ◽  
X Ray Diffraction ◽  
X Ray ◽  
Amorphous Interlayer

Thermally induced solid-state reactions between a 70 nm Pt film and a single-crystal (001) β-SiC substrate at temperatures from 300 °C to 1000 °C for various time durations are investigated by 2 MeV He backscattering spectrometry, x-ray diffraction, secondary ion mass spectrometry, scanning electron microscopy, and cross-sectional transmission electron microscopy. Backscattering spectrometry shows that Pt reacts with SiC at 500 °C. The product phase identified by x-ray diffraction is Pt3Si. At 600–900 °C, the main reaction product is Pt2Si, but the depth distribution of the Pt atoms changes with annealing temperature. When the sample is annealed at 1000 °C, the surface morphology deteriorates with the formation of some dendrite-like hillocks; both Pt2Si and PtSi are detected by x-ray diffraction. Samples annealed at 500–900 °C have a double-layer structure with a silicide surface layer and a carbon-silicide mixed layer below in contact with the substrate. The SiC—Pt interaction is resolved at an atomic scale with high-resolution electron microscopy. It is found that the grains of the sputtered Pt film first align themselves preferentially along an orientation of {111}Pt//{001}SiC without reaction between Pt and SiC. A thin amorphous interlayer then forms at 400 °C. At 450 °C, a new crystalline phase nucleates discretely at the Pt-interlayer interface and projects into or across the amorphous interlayer toward the SiC, while the undisturbed amorphous interlayer between the newly formed crystallites maintains its thickness. These nuclei grow extensively down into the substrate region at 500 °C, and the rest of the Pt film is converted to Pt3Si. Comparison between the thermal reaction of SiC-Pt and that of Si–Pt is discussed.

Two ZnIImononuclear coordination compounds with pyridinedicarboxylate and auxiliaryN-(pyridin-4-ylmethylidene)hydroxylamine ligands

2014 ◽  
Vol 70 (12) ◽  
pp. 1101-1104 ◽  
Author(s):  
Eduard B. Coropceanu ◽  
Ana Dreab ◽  
Lilia Croitor
Keyword(s):  
Single Crystal ◽  
Coordination Compounds ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Water Molecules ◽  
Coordination Geometry ◽  
X Ray ◽  
Trigonal Bipyramidal Coordination ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral

Two new mononuclear coordination compounds, bis{4-[(hydroxyimino)methyl]pyridinium} diaquabis(pyridine-2,5-dicarboxylato-κ2N,O2)zincate(II), (C6H7N2O)2[Zn(C7H3NO4)2(H2O)2], (1), and (pyridine-2,6-dicarboxylato-κ3O2,N,O6)bis[N-(pyridin-4-ylmethylidene-κN)hydroxylamine]zinc(II), [Zn(C7H3NO4)(C6H6N2O)2], (2), have been synthesized and characterized by single-crystal X-ray diffractometry. The centrosymmetric ZnIIcation in (1) is octahedrally coordinated by two chelating pyridine-2,5-dicarboxylate ligands and by two water molecules in a distorted octahedral geometry. In (2), the ZnIIcation is coordinated by a tridentate pyridine-2,6-dicarboxylate dianion and by twoN-(pyridin-4-ylmethylidene)hydroxylamine molecules in a distortedC2-symmetric trigonal bipyramidal coordination geometry.

Neue Oxopnictate AI3MVO4: Darstellung und Kristallstruktur von A3AsO4 (A = K, Rb, Cs) und K3BiO4 / New Oxopnictates AI3MVO4: Synthesis and Crystal Structure of A3AsO4 (A = K, Rb, Cs) and K3BiO4

2002 ◽  
Vol 57 (6) ◽  
pp. 599-604 ◽  
Author(s):  
Franziska Emmerling ◽  
Mamdouh Idilbi ◽  
Caroline Röhr
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Close Packing ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds have been synthesized via oxidation of the elemental pnicogenes (M = As, Bi) with the hyperoxides AO2 (A = K, Rb, Cs) and their crystal structures were determined on the basis of single crystal X-ray data. In K3AsO4 (orthorhombic, Cccm, a = 1060:1(1), b = 1135:2(1), c = 1694:0(2) pm, Z = 16) and Cs3AsO4(orthorhombic, Pnma, a = 1254:3(2), b = 902:9(2), c = 658:5(3) pm, Z = 4) isolated tetrahedra [AsO4]3- with distances As-O between 167.0 and 170.5 pm are present, which are arranged in a nearly cubic close packing. The structure of K3BiO4 (triclinic, P1̄, a = 643:18(6), b = 657:27(6), c = 762:41(7) pm, α = 101:724(2)°, β = 96:472(2)°, γ = 105:465(2)°, Z = 2) contains centrosymmetric dimers [O3BiO2BiO3]6-, in which the Bi(V) atoms are surrounded by five O atoms in a distorted trigonal bipyramidal geometry with distances Bi-O in the range of 199.5 to 233.1 pm.

Zur Stereochemie des freien Elektronenpaares in AX6E-Systemen, VIII. Statisch verzerrte Anionen in [H3N(CH2)3NH3]3(BiX6)2(H2O)2 mit X = Cl, Br/ On the Stereochemistry of the Lone-Pair Electrons in AX6E-Systems, VIII Statically Distorted Anion in [H3N(CH2)3NH3]3(BiX6)2(H2O)2 with X = Cl, Br

1988 ◽  
Vol 43 (8) ◽  
pp. 1003-1009 ◽  
Author(s):  
André du Bois ◽  
Walter Abriel
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Coordination Polyhedron ◽  
Lone Pair ◽  
Structural Data ◽  
Octahedral Coordination ◽  
Intensity Data ◽  
Space Group ◽  
X Ray ◽  
Lone Pair Electrons

Abstract Using 293 K diffractometer intensity data, the crystal structures of [H3N(CH2)3NH3]3(BiX6)2(H2O)2 with X - Cl, Br have been determined by single crystal X-ray technique and refined to a final Rw of 0.027 and 0.043, respectively. The structures are isotypic, space group P21/c, Z = 2 with a = 14.415(1). b = 9.7401(7), c = 12.4609(9)Å, β = 105.997(8)°for X - Cl and a = 14.794(2), b = 10.127(2), c = 12.853(2)Å, β = 105.68(2)° for X - Br. Statically distorted BiX63- octahedra confirm the symmetry rules for the stereochemistry of the lone pair electrons in AX6E-systems. Basic structural data for all compounds containing BiX63- and SbXh3 ions (X = Cl, Br, I) known to date are given including the ⊿-values as a measure for the distortion of the octahedral coordination polyhedron.

Stereospecific reactions of aryltellurium(IV) trichlorides with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol: the X-ray crystal structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride

1995 ◽  
Vol 73 (2) ◽  
pp. 255-263 ◽  
Author(s):  
Bozena Borecka ◽  
T. Stanley Cameron ◽  
M. Azad Malik ◽  
Barry C. Smith
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lone Pair ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Compound C ◽  
Stereospecific Reactions

Aryltellurium(IV) trichlorides react with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol to give aryl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides and aryl(cis-1-hydroxymethyl-trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides. The structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride has been determined by single crystal X-ray analysis. The compound C15H20Cl2O3Te, Mr = 446.8, crystallizes in the monoclinic space group P21/c with a = 9.626(2) Å, b = 15.768(5) Å, c = 11.176(3) Å, β = 92.08(1)°, V = 1695.2(5) Å3 and D(calc) = 1.751 for Z = 4. Tellurium is bonded axially to two chlorines and equatorially to aryl carbon and carbon from the cyclohexyl portion of oxabicyclo[3.2.1]oct-4-yl in a pseudo-trigonal-bipyramidal arrangement having an equatorial lone pair of electrons. Bond lengths are Te—Cl(1) = 2.492(3) Å, Te—Cl(2) = 2.539(3) Å, Te—C(4) = 2.175(10) Å, and Te—C(9) = 2.090(10) Å. Keywords: organotellurium(IV), 3-cyclohexene-1-methanol, 3-cyclohexene-1, 1-dimethanol.

Darstellung und Kristallstrukturen von Chloro- und Bromophenylantimonaten(III) [Ph2SbX2] - und [Ph2Sb2X7]3- (X=Cl, Br) / Preparation and Crystal Structures of Chloro- and Bromophenylantimonates(III) [Ph2SbX2]- and [Ph2Sb2X7]3- (X=Cl, Br)

1992 ◽  
Vol 47 (7) ◽  
pp. 919-924 ◽  
Author(s):  
W. S. Sheldrick ◽  
C. Martin
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Halogen Atoms ◽  
Trigonal Bipyramidal ◽  
The Individual

The halophenylantimonates(III) [Ph4P][Ph2SbCl2] (1), [Ph4P][Ph2SbBr2] (2), [Me3NH]3[Ph2Sb2Cl7] (3) and [Me3NH]3[Ph2Sb2Br7] (4) have been prepared and their structures established by single crystal X-ray diffraction. The anions [Ph2SbCl2]- and [Ph2SbBr2]- display w-trigonal bipyramidal geometries with axial halogen atoms. Sb-Cl [2.618(4), 2.601(4)Å] and Sb-Br distances [2.779(3), 2.794(2)A] are very similar to one another in the individual anions of 1 and 2. The anions [Ph2Sb2Cl7]3- and [Ph2Sb2Br7]3- both contain two square pyramidal coordination polyhedra which are vertex-linked to one another via Sb-X-Sb (X=Cl, Br) angles of respectively 152.9(1) and 152.3(1)°; the latter anion displays crystallographic C2-symmetry. trans-Sited Sb-Cl or Sb-Br bond distances in 3 and 4 are structurally correlated to one another.

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