NMR Crystallography for Structural Characterization of Oxovanadium(V) Complexes: Deriving Coordination Geometry and Detecting Weakly Coordinated Ligands at Atomic Resolution in the Solid State

2015 ◽  
Vol 54 (4) ◽  
pp. 1363-1374 ◽  
Author(s):  
Mingyue Li ◽  
Jenna Yehl ◽  
Guangjin Hou ◽  
Pabitra B. Chatterjee ◽  
Amir Goldbourt ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Atomic Resolution ◽  
Coordination Geometry ◽  
Nmr Crystallography

Synthesis and structural characterization of bis(tropolonatodimethylgallium), [(C7H5O2)Ga(CH3)2]2

1984 ◽  
Vol 62 (9) ◽  
pp. 1705-1708 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Solid State ◽  
Physical Properties ◽  
Least Squares ◽  
Structural Characterization ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
State Structure ◽  
Full Matrix ◽  
Trigonal Bipyramidal

Details of the synthesis, physical properties, and solid-state structure of [(C7H5O2)Ga(CH3)2]2 are reported. Crystals of bis(tropolonatodimethylgallium) are monoclinic, a = 10.2669(9), b = 9.3237(3), c = 10.8671(10) Å, β = 112.896(4)°, Z = 2, space group P21/n (22°C, λ = 0.70930 Å). The structure was solved by conventional heavy-atom techniques and was refined by full-matrix least-squares procedures to R = 0.034 and Rw = 0.037 for 1746 reflections with I ≥ 3σ(I). The centrosymmetric binuclear dimer features five-coordinate gallium atoms having irregular trigonal bipyramidal coordination geometry and a planar four-membered Ga2O2 ring. Important bond lengths (corrected for libration) are Ga—O(equatorial) = 1.972(2), Ga—O(axial) = 2.025(2) and 2.551(2) Å, and Ga—C = 1.951(4) and 1.954(4) Å.

A Methyl Group Bridging on Three Metal Atoms. Solid-State and Solution Structural Characterization of the [Re3(μ-H)3(μ3-CH3)(CO)9]-Anion

1999 ◽  
Vol 121 (10) ◽  
pp. 2307-2308 ◽  
Author(s):  
T. Beringhelli ◽  
G. D'Alfonso ◽  
M. Panigati ◽  
F. Porta ◽  
P. Mercandelli ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Methyl Group ◽  
Metal Atoms

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Manganese(i) poly(mercaptoimidazolyl)borate complexes: spectroscopic and structural characterization of Mn⋯H–B interactions in solution and in the solid state

2005 ◽  
pp. 171-180 ◽  
Author(s):  
Leigh A. Graham ◽  
Alison R. Fout ◽  
Karl R. Kuehne ◽  
Jennifer L. White ◽  
Bhaskar Mookherji ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Borate Complexes
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