Structural Properties of a Dimeric Phenylcyanamidocopper(I) Complex, [{Cu(PPh3)2(C6H5NCN)}2]

2000 ◽  
Vol 53 (12) ◽  
pp. 971 ◽  
Author(s):  
Eric W. Ainscough ◽  
Andrew M. Brodie ◽  
Peter C. Healy ◽  
Joyce M. Waters
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Properties ◽  
Structure Determination ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
X Ray ◽  
Angle Spinning

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

Lewis-Base Adducts of Group I Metal(I) Compounds. XXVI. Solid-State Cross-Polarization Magic-Angle-Spinning 31P N.M.R. and Structural Studies on 1:1 Adducts of Triphenylphosphine With Gold(I) Salts

1987 ◽  
Vol 40 (9) ◽  
pp. 1545 ◽  
Author(s):  
PF Barron ◽  
LM Engelhardt ◽  
PC Healy ◽  
J Oddy ◽  
AH White
Keyword(s):  
Solid State ◽  
Magic Angle Spinning ◽  
Lewis Base ◽  
Magic Angle ◽  
Molecular Formula ◽  
Cross Polarization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Group I ◽  
Angle Spinning

Linear, two-coordinate compounds of molecular formula (PPh3) AuX have been characterized by solid-state and solution 31P n.m.r. spectroscopy, and single-crystal X-ray diffraction techniques. The solid state n.m.r. spectra reveal single, broad resonance lines for X = NO3 (chemical shift 19 ppm , ref. 85% H3PO4), CH3C02 (24 ppm), SCN (36ppm), CN (37 ppm ) and CH3 (47 ppm ) and doublets for X = Cl (27, 33 ppm ), Br (28, 36 ppm ) and I (34, 38 ppm ), the latter three spectra being recorded at 121.47 MHz and 161.96 MHz. Solution spectra show relatively sharp single resonances for each compound with 6 values generally slightly higher than in the solid state. Crystal data are reported for X = NO3, space gro )p P21/c, a 8 895(9), b 10.117(8), c 19.57(2) �; β 97.43(8)�, Au-P,O = 2.199(5), 2.02(1) �. Crystals of compounds with X = Br, I and SCN are isomorphous with the AuCl compound, belonging to space group 212121. For X = Br, a 12.479(5), b 13.45(1), c 10.0!2(8) �; Au-P, Br = 2.252(6), 2.407(2) �. For X = I, a 12.529(8), b 13.870(5), c 10.188(4) �; Au-P, I = 2.254(5), 2.556(2) �. For X = SCN, a 12.257(5), b 13.776(8), c 10.754(6) �; Au-P, S = 2.252(7), 2.304(7) �.

Structure determination of aligned systems by solid-state NMR magic angle spinning methods

2005 ◽  
Vol 176 (2) ◽  
pp. 223-233 ◽  
Author(s):  
Benjamin J. Gross ◽  
Joseph M. Tanski ◽  
Ann E. McDermott
Keyword(s):  
Solid State ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Angle Spinning

Determination of the location of naphthalene in the zeolite ZSM-5 host framework by solid-state 1H/29Si CP MAS NMR spectroscopy

2006 ◽  
Vol 84 (2) ◽  
pp. 345-355 ◽  
Author(s):  
Colin A Fyfe ◽  
Darren H Brouwer
Keyword(s):  
Solid State ◽  
Structure Determination ◽  
Dipolar Coupling ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Magic Angle ◽  
Cross Polarization ◽  
Nmr Structure Determination ◽  
Nmr Data ◽  
Angle Spinning

The location of naphthalene in the zeolite ZSM-5 has been determined from solid-state 1H/29Si cross-polarization (CP) magic-angle-spinning (MAS) NMR data alone. With the peaks in the 29Si spectrum assigned to the inequivalent Si sites in the zeolite from a two-dimensional INADEQUATE spectrum, the rates of cross polarization between the 1H nuclei of the guest sorbate molecules and the 29Si nuclei of the zeolite framework were used to determine the location of the naphthalene molecules by exploiting the proportional relationship between cross-polarization rate constants and 1H/29Si dipolar coupling second moments. The NMR structure determination was carried out on three different selectively deuterium-labeled naphthalene molecules (naphthalene-d0, α-naphthalene-d4, and β-naphthalene-d4). The average of the molecule locations in agreement with all three sets of NMR data was found to be in excellent agreement with an existing single crystal XRD structure of the naphthalene–ZSM-5 complex.Key words: solid-state NMR, cross polarization, zeolites, host–guest complexes, structure determination.

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