Titan(IV)-Fulvalenkomplexe. Darstellung und Struktur von [CpTiPh2l2(C10H8) / Titanium(IV) Fulvalene Complexes. Preparation and Structure of [CpTiPh2]2(C10H8)

1993 ◽  
Vol 48 (5) ◽  
pp. 603-607 ◽  
Author(s):  
Ulf Thewalt ◽  
Thomas Wöhrle
Keyword(s):  
Structure Analysis ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The green insoluble TiIV compound which is obtained by treating titanocene with HC1 reacts with PhLi to yield the fulvalene-bridged compound [CpTiPh2]2(C10Hg) 3(Ph). An X-ray structure analysis of 3(Ph) shows, that the Ti atoms are in a trans arrangement with respect to the fulvalene group. Crystal data for 3(Ph) are as follows: C44H38Ti2, orthorhombic, space group P212,1 21, with a = 11,385(2), b = 14,510(2), c = 19,489(4) Å, Z = 4. The crystals exhibit enantiomorphism.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

Die Röntgenstrukturanalyse von (CO)9Co3CΟΒΒr2Ν(C5)3. X-ray Structure Analysis of (CO)9Co3COBBr2N(C2H5)3

1976 ◽  
Vol 31 (3) ◽  
pp. 342-344 ◽  
Author(s):  
Volker Bätzel
Keyword(s):  
Least Squares ◽  
Structure Analysis ◽  
Reliability Index ◽  
Three Dimensional ◽  
Diagonal Matrix ◽  
Crystal Data ◽  
Block Diagonal Matrix ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray

Using three dimensional X-ray data collected on a four circle diffractometer, the structure of (CO)9Co3COBBr2N(C2H5)3 was solved by Patterson and Fourier methods. Least squares refinement with a block-diagonal matrix leads to a reliability index of R = 10.7%. Crystal data: α = 13.277(6) Å, b = 10.17(1) Å, c = 9.22(2) Å; α = 91.12(6)°, β = 87.61(4)°, γ = 98.79(2)°; space group P1̅; Z = 2; V = 1229,7 Å3; Dx = 1.97 gcm-3.

Vanadiumkomplexe mit dreizähnigen diaciden Liganden. Bis[2-(2′-hydroxyphenyl)-chinolin-8-olato]dimethoxo-dioxo-divanadium(V) -ein neuer Strukturtyp/Vanadium Complexes with Tridentate Diacidic Ligands. Bis[2-(2′-hydroxyphenyl)-8-quinolinolato)dimethoxo-dioxo-divanadium (V) - a New Structure Type

1997 ◽  
Vol 52 (6) ◽  
pp. 693-695 ◽  
Author(s):  
Heike Hefele ◽  
Erhard Uhlemann ◽  
Frank Weller
Keyword(s):  
Molecular Structure ◽  
Structure Analysis ◽  
Sulfate Solution ◽  
Structure Type ◽  
Vanadium Complexes ◽  
Crystal Data ◽  
Space Group ◽  
X Ray

A new binuclear vanadium( V) complex was synthesized by reaction of an aqueous oxovanadium(IV) sulfate solution with 2-(2′-hydroxyphenyl)-8-quinolinol dissolved in methanol. The molecular structure of the complex was determined by X-ray structure analysis. Crystal data: a = 10.004(3), b = 9.325(2), c = 15.089(3) Å; β = 91.95(2)°; space group P21/n, Z = 4.

The selective complexation of adamantane nitriles by tungsten pentacarbonyl

1996 ◽  
Vol 74 (1) ◽  
pp. 107-113 ◽  
Author(s):  
Valerie J. Jefford ◽  
Melbourne J. Schriver ◽  
Michael J. Zaworotko
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pure Compounds ◽  
Semi Empirical ◽  
Oxygen Atoms ◽  
Selective Complexation

Adamantyl-1,3,4-oxathiazol-2-one is usually prepared as a mixture with 1-adamantanecarbonitrile. To separate these two compounds the mixture is reacted with thf•W(CO)5, which selectively forms a complex with the nitrile. The resulting mixture can then be readily separated into pure compounds by sublimation. Characterization data are presented, including the X-ray crystal structure of the nitrile complex, which can be prepared directly from the reaction of the adamantyl nitrile and thf•W(CO)5. (Crystal data for C16H15NO5W: orthorhombic, space group Pmcn, a = 10.5869(19) Å, b = 14.0622(22) Å, c = 23.342(4) Å, V = 3475.0(11) Å, Z = 8, R = 0.042.) The nitrile can be recovered from the complex by reaction with P(C6H5)3 followed with separation by sublimation. The reaction of the related 1-cyano-3-(1,3,4-oxathiazol-2-on-5-yl)-adamantane with thf•W(CO)5 yields a complex in which the site of coordination is shown spectroscopically to be the nitrile moiety. Semi-empirical calculations at the PM3 level indicate that the oxathiazolone heterocycle may be a poor ligand due to the influence of the exo- and endo-cyclic oxygen atoms. Key words: oxathiazolone, nitrile, tungsten, complexation, selectivity, adamantane.not available

Crystal data and X-ray powder-diffraction data for ferrimolybdite, Fe2(MoO4)36.8(H2O)

1995 ◽  
Vol 10 (2) ◽  
pp. 101-103 ◽  
Author(s):  
Ernst Horn ◽  
Masayasu Kurahashi ◽  
Dianhao Huang ◽  
Chengyu Wu
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Crystal Data ◽  
Powder Diffraction Data ◽  
Orthorhombic Space Group ◽  
Chinese Sample ◽  
Space Group ◽  
X Ray

Powder-diffraction data were collected for a Chinese sample of ferrimolybdite. This mineral is orthorhombic, space group Pmmn or Pm21n, with a = 6.665(2), b = 15.423(5), c = 29.901(8), and V = 3074(1) Å3.

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Structure and conformation of hydroxylubimin, a sesquiterpenoid phytoalexin

1977 ◽  
Vol 55 (10) ◽  
pp. 1619-1623 ◽  
Author(s):  
George I. Birnbaum
Keyword(s):  
Structure Analysis ◽  
Direct Methods ◽  
Membered Ring ◽  
Side Chain ◽  
Equatorial Position ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Independent Molecules ◽  
Chiral Centers

In order to determine the orientation of the isopropenyl group and confirm the stereochemistry at other chiral centers in lubimin (1) and hydroxylubimin (2), two antifungal sesquiterpenes, an X-ray structure analysis of 2 was carried out. Crystals of 2 are orthorhombic, space group P212121, a = 6.190, b = 7.210, c = 63.082 Å, Z = 8. The structure was solved by direct methods and refined to R = 0.045. In both independent molecules the six-membered ring is chair-shaped with all four substituents equatorially oriented. The five-membered ring, attached by a spiro junction, is a half-chair with the isopropenyl substituent in an equatorial position. This side-chain is trans to the methyl-bearing carbon in the six-membered ring.

scholarly journals Indole alkaloids from Vinca erecta type of sarpagine and ajmaline

2019 ◽  
Vol 10 (4) ◽  
pp. 409-416 ◽  
Author(s):  
Shahobiddin Adizov ◽  
Bakhodir Tashkhodjaev
Keyword(s):  
Conformational Changes ◽  
Absolute Configuration ◽  
Indole Alkaloids ◽  
Diffraction Method ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The single crystal X-ray diffraction method established the absolute configuration of the Vinca erecta indole alkaloids of the akuammidine sarpagine type (3S, 5S, 15R, 16R) and its o-acyl derivative, as well as the type of ajmaline, quebrachidine (2S, 3S, 5S, 7R, 15S, 16R, 17S) and majoridine (2R, 3S, 5S, 7R, 15R, 16S, 17R). Crystal data for C21H24N2O3 (1): orthorhombic, space group P212121 (no. 19), a = 6.3949(5) Å, b = 13.5009(10) Å, c = 22.461(3) Å, Z = 4, 7694 reflections measured (7.64° ≤ 2Θ ≤ 152.294°), 3813 unique (Rint = 0.0798) which were used in all calculations. The final R1 was 0.0680 (I > 2σ(I)) and wR2 was 0.1650 (all data). Crystal data for C23H26N2O4 (2): orthorhombic, space group P212121 (no. 19), a = 9.9730(13) Å, b = 10.2090(10) Å, c = 20.409(3) Å, Z = 4, 7959 reflections measured (8.666° ≤ 2Θ ≤ 151.998°), 4212 unique (Rint = 0.0386) which were used in all calculations. The final R1 was 0.0477 (I > 2σ(I)) and wR2 was 0.1171 (all data). Crystal data for C42H48N4O6 (3): monoclinic, space group P21 (no. 4), a = 8.9320(10) Å, b = 21.515(5) Å, c = 9.5420(10) Å, β = 97.103(10)°, Z = 2, 16677 reflections measured (9.34° ≤ 2Θ ≤ 151.836°), 7393 unique (Rint = 0.0278) which were used in all calculations. The final R1 was 0.0366 (I > 2σ(I)) and wR2 was 0.1037 (all data). Crystal data for C23H28N2O3 (4): orthorhombic, space group P212121 (no. 19), a = 10.636(2) Å, b = 11.208(12) Å, c = 16.725(13) Å, Z = 4, 1650 reflections measured (9.498° ≤ 2Θ ≤ 119.97°), 1650 unique (Rint = 0.0436) which were used in all calculations. The final R1 was 0.0608 (I > 2σ(I)) and wR2 was 0.1720 (all data). In alkaloids such as sarpagine and ajmaline exo, the substituents of alkaloids do not lead to conformational changes of a stable polycyclic framework. In the series of sarpagine, alkaloids form mono-salts in the tetrahedral nitrogen N4, and in indolines of the ajmaline type, the tetrahedral hybridization of the N1 and N4 atoms favors the formation of disols. In V. erecta alkaloids, the exomethylene fragment (C18-C19=C20-C21) of the polycyclic backbone always takes on the E-state.

Preparation and structure of 2-chloro-1,3-dimethyldiaza-2-arsenane, 1,3-dimethyldiaza-2-arsenanium tetrachlorogallate, and butadiene cycloadducts of diazarsenium cations

1996 ◽  
Vol 74 (11) ◽  
pp. 2209-2216 ◽  
Author(s):  
Neil Burford ◽  
Charles L.B. Macdonald ◽  
Trenton M. Parks ◽  
Gang Wu ◽  
Borzena Borecka ◽  
...  
Keyword(s):  
Solid State ◽  
Chloride Ion ◽  
2D Nmr ◽  
Diels Alder ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
State Structure ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

1,3-Dimethyldiaza-2-arsenanium tetrachlorogallate (crystal data: C5H12AsCl4GaN2, M = 386.61, orthorhombic, space group Pca21, a = 14.432(3) Å, b = 6.7580(14) Å, c = 13.905(3) Å, V = 1356.2(5) Å3) is synthesized by the routine chloride ion abstraction procedure from 2-chloro-1,3-dimethyldiaza-2-arsenane (crystal data: C5H12AsClN2, M = 210.54, monoclinic, space group P21/n, a = 7.206(1) Å, b = 9.650(1) Å, c = 13.021(2) Å, β = 99.61(2)°, V = 892.8(2) Å3). X-ray crystallographic studies of both compounds are described together with that for 2-chloro-1,3-dimethyldiaza-2-arsolidine (crystal data: C4H10AsClN2, M = 196.51, monoclinic, space group P21/n, a = 6.959(7) Å, b = 9.23(2) Å, c = 12.14(2) Å, β = 95.4(1)°, V = 777(4) Å3) providing useful structural comparisons. In contrast to the closely related arsolidinium salts, the diazarsenanium gallate exhibits a monomeric solid state structure. Rapid and quantitative cycloaddition reactions of the diazarsolidinium and diazarsenanium cations with 2,4-dimethylbutadiene give similar cycloadducts. The Diels–Alder type arsolidinium adduct is structurally characterized (crystal data: C10H20AsCl4GaN2, M = 454.73, orthorhombic, space group Pca21, a = 18.471(2) Å, b = 7.000(2) Å, c = 13.738(1) Å, V = 1776.2(8) Å3), and the related structure of the arsenanium cycloadduct is confirmed by 2D NMR. Key words: arsenium, cycloadditions, arsenanium, Diels–Alder, cyclochloroarsines.

X-ray analysis of the structure and correlation with the spectra of haplophytine

1976 ◽  
Vol 54 (5) ◽  
pp. 726-732 ◽  
Author(s):  
P.-T. Cheng ◽  
S. C. Nyburg ◽  
F. N. MacLachlan ◽  
Peter Yates
Keyword(s):  
Magnetic Resonance ◽  
Structure Analysis ◽  
Proton Magnetic Resonance ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Magnetic Resonance Spectra

Haplophytine crystallizes as the methanolate in the orthorhombic space group P212121 with a = 13.874(4), b = 10.628(4), c = 22.890(9) Å, Z = 4. X-Ray structure analysis confirms that the previously assigned structure 3 is correct and that haplophytine undergoes reversible rearrangement on conversion to its dihydrobromide 1. The dimensions of 3 provide evidence supporting previous interpretations of unusual features of the infrared and proton magnetic resonance spectra of haplophytine.

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