Electronic and structural properties of a reactive metalloporphyrin with N-oxide axial ligands. Crystal and molecular structure of bis(2,6-lutidine N-oxide)(tetraphenylporphinato)manganese(III) perchlorate

1985 ◽  
Vol 24 (19) ◽  
pp. 3024-3030 ◽  
Author(s):  
Craig L. Hill ◽  
Michael W. Williamson
Keyword(s):  
Molecular Structure ◽  
Structural Properties ◽  
Crystal And Molecular Structure ◽  
Axial Ligands ◽  
Electronic And Structural Properties

Synthesis and Electrochemistry of Aluminum Porphycenes: Crystal and Molecular Structure of Methyl-σ-Bonded Aluminum Etioporphycene

1997 ◽  
Vol 01 (02) ◽  
pp. 109-119 ◽  
Author(s):  
ROGER GUILARD ◽  
VIRGINIE PICHON-PESME ◽  
HASSANE LACHEKAR ◽  
CLAUDE LECOMTE ◽  
ALLY M. AUKAULOO ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Axial Ligands ◽  
Uv Visible

The synthesis and characterization of three monomeric aluminum porphycenes with anionic or σ-bonded axial ligands is reported. The investigated compounds are represented as ( EtioPc ) Al ( CH 3) and ( EtioPc ) AlX where EtioPc represents the dianion of etioporphycene and X = Cl − or OH −. Each synthesized complex was characterized by mass spectrometry. 1 H NMR, IR and UV-visible spectroscopies as well as by electrochemistry. Comparisons are made between the properties of complexes in the aluminum etioporphycene series and related chloro- or methyl σ-bonded Al ( III ) porphyrins containing octaethylporphyrin ( OEP ) or tetraphenylporphyrin ( TPP ) macrocycles. Comparisons are also made between the currently investigated compounds and a previously reported Al ( III ) μ-oxo dimer, [( EtioPc ) Al ]2 O . In addition, the crystal and molecular structure of ( EtioPc ) Al ( CH 3) was determined by X-ray diffraction. The molecular structure of this methyl-σ-bonded aluminum etioporphycene provides the first structural data for an aluminum porphycene compound. The aluminum(III) atom in ( EtioPc ) Al ( CH 3) is pentacoordinated and is located 0.54 Å from the plane of the four N -nitrogens.

Kristall-und Molekülstruktur von N-(TricHorgermyl)-trimethylphosphinimin [Cl3Ge-N=PMe3]n, n = 1 und 2 / Crystal and Molecular Structure of N-(Trichlorogermyl)-trimethylphosphinimine [Cl3Ge-N=PMe3]n, n= 1 and 2

1978 ◽  
Vol 33 (5) ◽  
pp. 493-497 ◽  
Author(s):  
W. S. Sheldrick ◽  
D. Schomburg ◽  
W. Wolfsberger
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Centrosymmetric Dimer ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
Axial Ligands ◽  
Trigonal Bipyramidal ◽  
Coordinate Bond

Abstract N-(Trichlorogermyl)trimethylphosphinimine crystallizes in the triclinic space group P1̅ with a = 12.49(2), b = 12.54(3), c = 6.66(1) Å,a = 100.96(10),β = 91.45(14), γ = 102.77(15)°. The structure was solved by Patterson and difference syntheses and refined to R = 0.063 for 2867 independent reflections. In the unit cell there are two symmetry related monomers containing tetracoordinated Ge and one crystallographically centrosymmetric dimer with a planar four-membered [GeN]2 ring exhibiting trigonal-bipyramidal pentacoordinated Ge and trigonal N. Significant differences are observed in the bond lengths from pentacoordinated Ge to its equatorial and axial ligands: Ge-Neq 1.837(7), Ge-Nax 1.972(7), Ge-Cleq 2.176(2) and 2.170(2), Ge-Clax 2.345(3) Å. The Ge-Neq distance is similar to that observed in tetracoordinated derivatives [1.81-1.87 Å], whereas the Ge-Nax distance is 0.22 Å shorter than that observed for the axial N→Ge coordinate bond in hitherto known pentacoordinated derivatives [2.19-2.24 Å]. The very short Ge-N bond length of 1.737(8) Å in the monomer which is 0.07 Å shorter than in other tetracoordinated derivatives may be indicative of the involvement of a (p→d)π component.

Crystal and Molecular Structure of the N-Methyldiethanolaminogallane Dimer, [CH3N(CH2CH2O)2GaH]2

1974 ◽  
Vol 52 (12) ◽  
pp. 2206-2215 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Experimental Error ◽  
Crystal And Molecular Structure ◽  
Fourier Synthesis ◽  
Full Matrix ◽  
Axial Ligands ◽  
Trigonal Bipyramidal ◽  
The Mean ◽  
Distorted Trigonal Bipyramidal

Crystals of the N-methyldiethanolaminogallane dimer are orthorhombic, a = 19.112(4), b = 9.947(2), c = 7.709(2) Å, Z = 4, space group P212121. The structure was determined by Patterson and Fourier synthesis and was refined by full-matrix least-squares procedures to a final R of 0.056 for 1477 observed reflections. The structure provides the first1 known crystallographic example of pentacoordinate gallium, the dimerization of MeN(CH2CH2O)2GaH occurring via the formation of a four-membered Ga2O2 ring. The coordination about the gallium is distorted trigonal bipyramidal with an angle of 151.2(4)° between the axial substituents. The mean bond distances are: Ga—N, 2.192(5), and Ga—O, 2.018(2) for axial ligands; Ga—O, 1.847(2), 1.960(8), and Ga—H, 1.41(4) for equatorial ligands; O—C, 1.419(14), C—N, 1.470(7), C—C, 1.520(12), and C—H, 1.00(13) Å. The molecule has C2 symmetry to within experimental error. There are possible [Formula: see text] hydrogen bonds ([Formula: see text] 3.13(1)–3.44(1) Å) in the structure.

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