Main group (IIIA or 13) complexes of benzohydroxamic acid and the crystal structure of tris(benzohydroxamato)indium(III)

1988 ◽  
Vol 66 (8) ◽  
pp. 1809-1813 ◽  
Author(s):  
Carey A. Matsuba ◽  
Steven J. Rettig ◽  
Chris Orvig
Keyword(s):  
Crystal Structure ◽  
High Yield ◽  
Acetohydroxamic Acid ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Full Matrix ◽  
X Ray ◽  
Benzohydroxamic Acid ◽  
Ethanol Solvate ◽  
Indium Complex

A series of tris(benzohydroxamato)metal(III) complexes has been prepared and characterized wherein the metals are aluminum, gallium, and indium. The complexes are synthesized in high yield from aqueous solution. The indium complex, as its ethanol solvate In(C7H6NO2)3•C2H5OH, has been studied by single crystal X-ray diffraction. The crystals are monoclinic with a = 11.091(2), b = 18.065(3), c = 12.861(2) Å, β = 105.55(1)°, Z = 4, and space group P21/n. The structure was solved by Patterson and Fourier methods and was refined by full-matrix least-squares procedures to R = 0.038 and Rw = 0.037 for 2579 reflections with I ≥ 3σ(I). Bond lengths and angles in the compound were normal, although there is a strong In—O(C) interaction; the arrangement of the three ligands is mer. There is extensive hydrogen bonding involving all possible donors. All three complexes have been studied by mass spectrometry, and by infrared and nuclear magnetic resonance (1H, 27Al) spectroscopies. Parallel studies have been attempted with acetohydroxamic acid.

Crystal structure of Tetracyclo[5,3,1,12,6,04,9]dodecane (iceane)

1977 ◽  
Vol 30 (8) ◽  
pp. 1837 ◽  
Author(s):  
DPG Hamon ◽  
CL Raston ◽  
GF Taylor ◽  
JN Varghese ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rigid Body ◽  
Least Squares ◽  
Title Compound ◽  
Molecular Geometry ◽  
Thermal Motion ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Hexagonal Close Packed

The crystal structure of the title compound, C12H18, has been determined at 295 K by X-ray diffraction and refined by full-matrix least squares to a residual of 0.049 for 216 ?observed? reflections; molecular geometry has been corrected for the effects of thermal motion using a rigid body approximation. Crystals are hexagonal, P63/m, a = 6.582(1), c = 11.843(3) Ǻ, Z = 2, the molecules occupying a hexagonal close- packed array.

Pentamethylcyclopentadienyl-Vanadium Complexes Containing Halogeno- and Oxo-Ligands

1987 ◽  
Vol 42 (12) ◽  
pp. 1520-1526 ◽  
Author(s):  
Max Herberhold ◽  
Walter Kremnitz ◽  
Markus Kuhnlein ◽  
Manfred L. Ziegler ◽  
Karl Brunn
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
High Yield ◽  
Vanadium Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Oxygen Bond ◽  
Single Bonds ◽  
Oxo Ligands

AbstractA simple and high-yield preparation of the pentamethylcyclopentadienyl vanadium(IV) trihalides Cp*VX3 (X = CL, Br, I) from Cp*V(CO)4 as well as their conversion into the oxo-vanadium(V) compounds Cp*VOX2 (X = CL, Br) and [Cp*VOX]2(μ-O) (X = CL, Br, I) are described. The equilibrium between the two fluoride species Cp*VOF2 and [Cp*VOF]2(μ-O) has also been investigated. The complexes are characterized by their NMR (51V, l3C, 1H), IR, and mass spectra. The crystal structure of the binuclear chloro-oxo complex [Cp*VOCl]2(μ-O) has been determined by X-ray diffraction. The molecules contain two [Cp*VOCl] units combined via a bent oxo bridge (V-O-V angle of 142.2(2)°). The vanadium-oxygen bond lengths are 157.6(8) and 179.4(1) pm for the terminal and the bridging oxo ligands, respectively, corresponding to double and single bonds.

Synthesis and X-ray crystal structure of the 3,5-dimethylpyrazolato copper(I) trimer, [Cu(pz″)]3

1990 ◽  
Vol 68 (8) ◽  
pp. 1444-1449 ◽  
Author(s):  
Martin K. Ehlert ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Heavy Atom ◽  
High Yield ◽  
Asymmetric Unit ◽  
Temperature Synthesis ◽  
Full Matrix ◽  
X Ray ◽  
Unit Space ◽  
High Temperature Synthesis

A moderately high-yield, high temperature synthesis of the title compound is reported. Crystals of tris[(3,5-dimethylpyrazolato-N1,N2)copper(I)] are triclinic, a = 12.360(4), b = 14.637(4), c = 12.358(4) Å, α = 105.29(2), β = 119.83(2), γ = 93.99(3)°, Z = 4 (trimers, two per asymmetric unit), space group [Formula: see text]. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.034 and Rw = 0.038 for 3877 reflections with I ≥ 3σ(I). The structure consists of trimeric molecules with an unusually short average Cu—N distance of 1.852 Å. The central Cu3N6 nine-membered rings are planar to within 0.07 Å. The trimer units are linked in pairs about centres of symmetry by weak [Formula: see text] interactions averaging 2.946 Å. Keywords: pyrazolato copper (I) timer, copper (I) pyrazolate.

The crystal structure of potassium trichloro(2,6-lutidine)platinum(II)

1976 ◽  
Vol 54 (6) ◽  
pp. 1002-1006 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon
Keyword(s):  
Crystal Structure ◽  
Complex Salt ◽  
Platinum Atom ◽  
Potassium Ions ◽  
Distorted Tetrahedron ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Salt Forms ◽  
Coordination Plane

The molecular and crystal structure of potassium trichloro(2,6-lutidine)platinum(II) has been determined by X-ray diffraction. The complex salt forms monoclinic crystals, a = 6.941, b = 24.301, c = 11.168 Å, β = 141.58°, Z = 4, and space group P21/c. Positional and anisotropic thermal parameters were refined by full matrix least squares calculations to R = 0.038 and Rw = 0.034.The coordination around the platinum atom is planar. The Pt—Cl bond lengths are 2.301, 2.299, and 2.302 Å and the Pt—N bond length is 2.011 Å. The 2,6-lutidine ring lies almost perpendicular to the coordination plane of the platinum atom (81.6°). The PtCl3 moieties are packed around the potassium ions, which are surrounded by four chlorine atoms at distances smaller than 3.15 Å forming a distorted tetrahedron.

Preparation and Crystal Structure of Genistein Benzenesulfonate Prodrugs

2008 ◽  
Vol 2008 (10) ◽  
pp. 555-558 ◽  
Author(s):  
You Peng ◽  
Zeyuan Deng ◽  
Shaojie Lang ◽  
Yawei Fan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Sulfonic Acid ◽  
Nmr Spectra ◽  
High Yield ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
H Nmr ◽  
Ester Prodrugs

In order to improve bioavailability and anticancer activity of genistein, a series of novel sulfonic acid ester prodrugs of the isoflavone genistein were synthesised in high yield with excellent regioselectivity. Their structures were characterised by IR, MS, elemental analysis and 1H NMR spectra. The crystal structure was examined by X-ray diffraction. X-ray structure determination revealed that all the aromatic rings in the compound are not coplanar. In the crystal structure, molecules are linked through intermolecular C-H···O hydrogen bonds, forming layers parallel to the ab plane.

Structure, Stereochemistry and Novel 'Hydrogen Bonding' in Two Bipyridinium Salts of the B10H102- Anion

1987 ◽  
Vol 40 (12) ◽  
pp. 2097 ◽  
Author(s):  
DJ Fuller ◽  
DL Kepert ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Charge Transfer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Structure Determinations ◽  
Positively Charged

Crystal structure determinations of (LH)2(B10H10), (1), and (LH2)(B10H10), (2), L = 2,2'- bipyridine , have been carried out by single-crystal X-ray diffraction methods at 295 K, being refined by full-matrix least squares to residuals of 0.041, 0.047 for 1758, 1771 'observed' independent reflections respectively. Crystals of (1) are monoclinic, P21/n, a 12.040(7), b 17.71(1), c 11.142(4) �, β 101.78(4)�, Z 4. Crystals of (2) are monoclinic, P21/c, a 9.937(4), b 10.837(3), c 14.856(5) �, β 109 2l(3)�, Z 4. The colour of the compounds is accounted for by charge-transfer interactions of a novel type, namely between the positively charged cationic acid hydrogen atoms and the negatively charged non-apical hydrogen atoms of the anion. In yellow (1), these distances are 2.26(5) �, while in red (2), they are much shorter, being 1.89(4), 1.97(3) �.

Synthesis of Triferrocenylbenzenes by Tantalum(V)-Catalyzed Cyclotrimerization of Ethynylferrocene. The Crystal Structure of 1,3,5-Triferrocenylbenzene

1997 ◽  
Vol 62 (10) ◽  
pp. 1577-1584 ◽  
Author(s):  
Petr Štěpnička ◽  
Ivana Císařová ◽  
Jan Sedláček ◽  
Jiří Vohlídal ◽  
Miroslav Polášek
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
High Yield ◽  
Isomer Mixture ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Yield Formation

Exclusive, high-yield formation of the cyclotrimers of ethynylferrocene (1) was observed when TaCl5 in benzene was employed as catalyst. Analysis of the resulting isomer mixture by means of HPLC and 1H NMR revealed the presence of 1,3,5-triferrocenylbenzene (sym-2) and 1,2,4-triferrocenylbenzene (asym-2) in the ratio of 4 : 6. A small amount of pure sym-2 isomer was isolated, and its solid-state structure was established by single-crystal X-ray diffraction. The molecules of sym-2 possess a distorted up-up-down arrangement of the ferrocenyl groups attached to the benzene ring.

Röntgenstrukturbestimmung von AlCl3-Pyridin-Addukten: Der strukturelle Aufbau im trans-Dichlorotetrakis(pyridin)aluminium(III)- Tetrachloroaluminat(III) und im Trichlorotris(pyridin)aluminium(III) / X-ray Diffraction Study of AICl3-Pyridine Adducts: The Crystal Structure of trans-Dichlorotetrakis(pyridine)aluminium(III)tetrachloroaluminat(III) and of Trichlorotris(pyridine)aluminium(III)

1982 ◽  
Vol 37 (10) ◽  
pp. 1312-1315 ◽  
Author(s):  
Peter Pullmann ◽  
Karl Hensen ◽  
Jan W. Bats
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Diffraction Study ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
The Mean

Abstract Crystals of [Al(C5H5N)4Cl2][AlCl4] are orthorhombic, Pna21, Z = 4, a = 18.522(7), b = 15.141(5), c = 9.593(3) Å, V = 2690(2) Å3 , Dc = 1.440 g/cm3 . The structure has been solved from 5968 diffractometer measured intensities and refined by full-matrix least squares to Rw(F) = 0.032. The crystal structure shows the complex to be trans-dichloro-tetrakis(pyridine)aluminium(III) tetrachloroaluminat(III). The mean trans Al-Cl-and trans Al-N-distances in the octahedron are 2.279(3) and 2.070(4) Å, respectively. Crystals of Al(C5H5N)3Cl3 are monoclinic, P21/c, Z = 4, a = 7.261(2), b = 29.961(4), c = 8.624(1) Å, β = 98.12(2)°, V -1857(1) Å3 , DC = 1.326 g/cm3 . The structure has been solved from 4707 diffractometer measured intensities and refined to Rw(F) = 0.028. The crystal structure shows octahedral complexes AlCl3·3 (C5H5N) with trans geometry. The Al-N-distance trans to chlorine (2.096(2) Å) is significantly longer than the two other Al-N-distances (mean 2.072(2) Å).

scholarly journals Synthesis, Characterization, and Crystal Structure of Negundoside (2′-p-Hydroxybenzoyl Mussaenosidic Acid)

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Suresh Sharma ◽  
B. D. Gupta ◽  
Rajni Kant ◽  
Vivek K. Gupta
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Direct Method ◽  
Monoclinic Crystal System ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Monoclinic Crystal ◽  
Full Matrix ◽  
X Ray ◽  
Cell Parameters

The structure of title compound Negundoside (2′-p-hydroxybenzoyl mussaenosidic acid) was established by spectral and X-ray diffraction studies. The compound crystallizes in the monoclinic crystal system with space group P21 having unit cell parameters: a=11.6201 (5) Å, b=9.2500 (4) Å, c=12.2516 (5) Å, β=97.793 (4)°, and Z=2. The crystal structure was solved by direct method using single crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R value of 0.0520 for 3389 observed reflections.

Ring contraction of 4-substituted 2,6-dichlorophenols. The crystal structure of 2,2,4α,5α-Tetrachloro-1α,3α-dihydroxycyclopentane-1,4-carbolactone

1977 ◽  
Vol 30 (10) ◽  
pp. 2195 ◽  
Author(s):  
RM Christie ◽  
RW Rickards ◽  
KJ Schmalzl ◽  
D Taylor
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Major Product ◽  
X Ray Diffraction ◽  
Ring Contraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Counter Data

Alkaline chlorination of the 4-alkyl-2,6-dichlorophenols (2b) and (2c) proceeds through ring contraction and halolactonization to form the 4α- alkyl-2,2,5α-trichloro-1α,3α-dihydroxycyclopentane-1,4-carbolactones (4b) and (4c). Under similar conditions, 2,4,6-trichlorophenol affords the analogous 2,2,4α,5α-tetrachloro-1α,3α-dihydroxycyclopentane-1,4- carbolactone (4a) in low yield, in addition to the Hantzsch acid (3a) as the major product. The acid (3a) upon further treatment undergoes chloro-lactonization to give the lactone (4a). The structures of the lactones (4b) and (4c) follow from spectroscopic comparison with (4a), the structure of which has been established by X-ray diffraction (C6H4Cl4O4 orthorhombic a 13.485(1), b 12.348(1), c 11.371(1) Ǻ, space group Pccn, Z 8, solved by direct methods and refined by block-diagonal and full-matrix least squares to R 0.031, Rw 0.043 for 1313 unique counter data with I/σ(I) ≥ 3.0).

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