Additionen an die Si=N-Doppelbindung – Kristallstruktur eines (SiNCO)-Vierringes / Additions to the Si=N-Double Bond - Crystal Structure of a (SiNCO)-Four Membered Ring

1991 ◽  
Vol 46 (6) ◽  
pp. 709-713 ◽  
Author(s):  
Susanne Vollbrecht ◽  
Uwe Klingebiel ◽  
Dieter Schmidt-Bäse
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Single Crystals ◽  
Membered Ring ◽  
Thermal Cleavage

In the reaction with benzophenone and phenylaldehyde lithiated aminofluorosilanes behave like iminosilanes. Four membered rings are formed in (2+2) cycloadditions. The oxaazasilacyclobutane ((CMe3)2Si—NCMe3—C6H5CH—O—) was purified by destillation. Single crystals were obtained by recrystallization from hexane. The thermal cleavage of the (SiNCO)-rings leads to carboimines and cyclosiloxanes. The lithium derivate of di-tert-butylfluorosilyl-2.6-diisopropylphenylamine reacts with 2-methyl-propenal-2 in two competing ways. In a (2+4) cycloaddition an 1-oxa-3-aza-2-sila-5-cyclohexene is formed, and in a (2+2) cycloaddition 2-methyl-2-propenyl-N-(2.6-diisopropylphenyl)imine is generated via an (SiNCO)-ring intermediate.

ChemInform Abstract: Additions to the Si=N Double Bond - Crystal Structure of a (SiNCO) Four-Membered Ring.

ChemInform ◽  
2010 ◽  
Vol 22 (35) ◽  
pp. no-no
Author(s):  
S. VOLLBRECHT ◽  
U. KLINGEBIEL ◽  
D. SCHMIDT-BAESE
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Membered Ring

scholarly journals Synthesis and crystal structure of ABW-type SrFe1.40V0.60O4

2020 ◽  
Vol 76 (5) ◽  
pp. 664-667
Author(s):  
Thomas Gstir ◽  
Volker Kahlenberg ◽  
Hannes Krüger ◽  
Simon Penner
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Three Dimensional ◽  
Charge Compensation ◽  
Membered Ring ◽  
Side Product ◽  
Double Perovskites ◽  
Tetrahedral Framework ◽  
Synthesis And Crystal Structure ◽  
Zeolite Type

Single crystals of SrFe1.40V0.60O4, strontium tetraoxidodi[ferrate(III)/vanadate(III)], have been obtained as a side product in the course of sinter experiments aimed at the synthesis of double perovskites in the system SrO–Fe2O3–V2O5. The crystal structure can be characterized by layers of six-membered rings of TO4-tetrahedra (T: FeIII, VIII) perpendicular to [100]. Stacking of the layers along [100] results in a three-dimensional framework enclosing tunnel-like cavities in which SrII cations are incorporated for charge compensation. The sequence of directedness of up (U) and down (D) pointing vertices of neighboring tetrahedra in a single six-membered ring is UUUDDD. The topology of the tetrahedral framework belongs to the zeolite-type ABW.

scholarly journals Pseudo-polymorphism of Halogen Substituted Tetraaza[14]annulene Complexes

2014 ◽  
Vol 70 (a1) ◽  
pp. C1004-C1004
Author(s):  
Shuhei Ichimura ◽  
Masahiro Saeki ◽  
Yoshinori Tamaki ◽  
Kazuo Miyamura
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Single Crystals ◽  
Membered Ring ◽  
Space Group ◽  
X Ray ◽  
Coordination Sites ◽  
The Difference

6,8,15,17-tetramethyldibenzo-5,9,14,18-tetraazacyclotetradecinatonickel (II) (tmtaa) bears strain within its 14-membered ring and is known to adopt saddle-shaped structure. As a consequence, tmtaa has an asymmetric apical coordination sites at both sides of the saddle. Our previous study revealed that the chlorine substituted complex, [Ni(tmtaa-4Cl)] shown in Figure (X = Cl), exhibited pseudo-polymorphism with dichloromethane and chloroform. This behaviour is due to the good affinity between halogen substituents and halomethane solvent. In this study, we grew single crystals of [Ni(tmtaa-4Br)] using various halomethane solvent as crystallization solvents and elucidated the role of the solvents related to the generation of pseudo-polymorprhism. We have succeeded in obtaining two kinds of single crystals 1 and 2 from the same vial container using bromoform. From X-ray structural analysis, 1 and 2 formed twist dimer as with previous report, and are found to include bromoform in their crystal structure. Note that these complexes adopted more distorted saddle-shaped structure than normal tmtaa complexes. The Ni-N4 planes were not planar. The difference of 1 and 2 was the degree of distortion around Ni-N4 plane, and 1 was more distorted than 2. The space group of these complexes were Aba2 and C2/c respectively. The interactions that led to the difference in packing of dimers were CH...π interaction in 1 and π...π interaction in 2.

Effect of Mn3+ doping on crystal structure, point defects, and optical properties in green Ca3(VO4)2 single crystals

2021 ◽  
pp. 111300
Author(s):  
Galina M. Kuz’micheva ◽  
Liudmila. I. Ivleva ◽  
Irina A. Kaurova ◽  
Evgeny V. Khramov ◽  
Victor B. Rybakov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Optical Properties ◽  
Single Crystals ◽  
Point Defects

scholarly journals Some Novel Cobalt Diphenylphosphine Complexes: Synthesis, Characterization, and Behavior in the Polymerization of 1,3-Butadiene

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 4067
Author(s):  
Giovanni Ricci ◽  
Giuseppe Leone ◽  
Giorgia Zanchin ◽  
Benedetta Palucci ◽  
Alessandra Forni ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
And Behavior

Some novel cobalt diphenylphosphine complexes were synthesized by reacting cobalt(II) chloride with (2-methoxyethyl)diphenylphosphine, (2-methoxyphenyl)diphenylphosphine, and 2-(1,1-dimethylpropyl)-6-(diphenylphosphino)pyridine. Single crystals suitable for X-ray diffraction studies were obtained for the first two complexes, and their crystal structure was determined. The novel compounds were then used in association with methylaluminoxane (MAO) for the polymerization of 1,3-butadiene, and their behavior was compared with that exhibited in the polymerization of the same monomer by the systems CoCl2(PnPrPh2)2/MAO and CoCl2(PPh3)2/MAO. Some significant differences were observed depending on the MAO/Co ratio used, and a plausible interpretation for such a different behavior is proposed.

Zum Mineral Johillerit verwandte Oxovanadate RbCd4V3O12 und TlCd4V3O12 / Oxovanadates RbCd4V3O12 and TlCd4V3 O12 Related to the Mineral Johillerite

1997 ◽  
Vol 52 (5) ◽  
pp. 663-668 ◽  
Author(s):  
B. Mertens ◽  
Hk. Müller-Buschbaum
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystals ◽  
Solid State Reactions ◽  
Space Group ◽  
Related Compounds

Abstract Single crystals of I RbCd4V3O12 and TlCd4V3O12 II have been prepared by solid state reactions in closed iron tubes. The compounds crystallize closely related to the Johillerite structure in the space group C62h- C2/c with I: a = 13.058(3); b - 13.528(3), c = 7 .0 6 0 (2 )Å , β = 114.88(2)°; II: a = 12.999(6), b = 13.527(7), c = 7.055(3) Å , β = 114.88(4)°, Z = 4. Special features are the loss of Cu2+ in order to gain an additional Cd2+ position. The crystal structure is discussed with respect to related compounds of the Johillerite type.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Calcium Carbodiimide Compounds Revisited – Syntheses, Single Crystal Structure Determination and Vibrational Spectra of Ca11N6[CN2]2, Ca4N2[CN2] and Ca[CN2]

2008 ◽  
Vol 63 (5) ◽  
pp. 530-536 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
X Ray ◽  
Characteristic Features ◽  
Reported Data ◽  
Correct Data

Single crystals of Ca11N6[CN2]2 (dark red needles, tetragonal, P42/mnm (no. 136), a = 1456.22(5), and c = 361.86(2) pm, Z = 2), Ca4N2[CN2] (transparent yellow needles, orthorhombic, Pnma (no. 62), a = 1146.51(11), b = 358.33(4), and c = 1385.77(13) pm, Z = 4) and Ca[CN2] (transparent, colorless, triangular plates, rhombohedral, R3̅m (no. 166), a = 369.00(3), and c = 1477.5(3) pm, Z = 3) were obtained by the reaction of Na2[CN2], CaCl2 and Ca3N2 (if demanded by stoichiometry) in arc-welded Ta ampoules at temperatures between 1200 - 1400 K. Their crystal structures were re-determined by means of single crystal X-ray structure analyses. Additionally, the Raman spectra were recorded on these same single crystals, whereas the IR spectra were obtained with the KBr pellet technique. The title compounds exhibit characteristic features for carbodiimide units with D∞h symmetry (d(C-N) = 121.7 - 123.8 pm and ∡ (N-C-N) = 180°). The vibrational frequencies of these units are in the expected range (Ca11N6[CN2]2: νs = 1230, νs = 2008; δ = 673/645/624 cm−1; Ca4N2[CN2]: νs = 1230, νs = 1986; δ = 672/647 cm−1; Ca[CN2]: νs = 1274, νs = 2031, δ = 668 cm−1). The structural results are more precise than the previously reported data, and with the newly attained Raman spectrum of Ca11N6[CN2]2 we correct data reported earlier.

scholarly journals Crystal structure of (3E)-3-(2,4-dinitrophenoxymethyl)-4-phenylbut-3-en-2-one

2014 ◽  
Vol 70 (9) ◽  
pp. o1051-o1052 ◽  
Author(s):  
Ignez Caracelli ◽  
Stella H. Maganhi ◽  
Paulo J. S. Moran ◽  
Bruno R. S. de Paula ◽  
Felix N. Delling ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Nitro Group ◽  
Benzene Ring ◽  
Torsion Angle ◽  
Title Compound ◽  
Phenyl Ring ◽  
Aromatic Rings ◽  
Compound C ◽  
The One

In the title compound, C17H14N2O6, the conformation about the C=C double bond [1.345 (2) Å] isE, with the ketone moiety almost coplanar [C—C—C—C torsion angle = 9.5 (2)°] along with the phenyl ring [C—C—C—C = 5.9 (2)°]. The aromatic rings are almost perpendicular to each other [dihedral angle = 86.66 (7)°]. The 4-nitro moiety is approximately coplanar with the benzene ring to which it is attached [O—N—C—C = 4.2 (2)°], whereas the one in theorthoposition is twisted [O—N—C—C = 138.28 (13)°]. The molecules associateviaC—H...O interactions, involving both O atoms from the 2-nitro group, to form a helical supramolecular chain along [010]. Nitro–nitro N...O interactions [2.8461 (19) Å] connect the chains into layers that stack along [001].

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