Self-assembly route from a bis-aminal derivative to a new cyclam based macropentacycleElectronic supplementary information (ESI) available: 1H NMR spectrum of 2a and X-ray study of 3b, including views of the asymmetric unit, space-filling models and molecular packing. See http://www.rsc.org/suppdata/nj/b3/b310074j/

2004 ◽  
Vol 28 (2) ◽  
pp. 173 ◽  
Author(s):  
Rapha�l Tripier ◽  
St�phanie Develay ◽  
Michel Le Baccon ◽  
Fran�oise Chuburu ◽  
Fran�ois Michaud ◽  
...  
Keyword(s):  
1H Nmr ◽  
Self Assembly ◽  
Molecular Packing ◽  
Supplementary Information ◽  
Asymmetric Unit ◽  
Space Filling ◽  
Nmr Spectrum ◽  
X Ray ◽  
Unit Space

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

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.

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