Molecular and crystal structure of bis-quinolizidine immonium salts, II:. delta. /sup 1(6)/-dehydrosparteinium monoperchlorate
..delta../sup 1(6)/-Dehydrosparteinium monoperchlorate, (C/sub 15/H/sub 25/N/sub 2/)/sup +/ x ClO/sub 4//sup -/, is orthorhombic: P2/sub 1/2/sub 11/, a = 12.473(2), b = 24.292(3), c = 10.835(1) A, V/sub c/ = 3353.7(9) A/sup 3/, Z = 8, D/sub x/ = 1.32, D/sub m/ = 1.32 g cm/sup -3/, ..mu..(Cu K..cap alpha..) = 20.7 cm/sup -1/. The final R was 0.097 for 2091 observed counter reflections. A partial disorder of the crystal structure has been observed. The two independent perchlorate anions are orientationally disordered, and the peripheral atoms in the cation skeletons have large temperature factors due both to conformational disorder of rings A and to disordered orientations of the whole cations alike. In rings A, atoms C(3) and C(4), trans-annular to the immonium bond, are disordered to a different extent in each of the two independent cations. Rings B, C, and D have sofa (distorted towards half-chair), chair, and chair conformations, respectively. The quinolizidinium and quinolizidine moieties have planar and cis configurations, respectively. The title compound was obtained from ..delta../sup 5/-dehydrosparteine, the product of mercuric acetate dehydrogenation of sparteine at room temperature. From /sup 13/C NMR measurements in /sup 2/H/sub 2/O and in DMSO/sup 2/H/sub 6/ it is evident that, in solution, the molecular geometry with chair/chair cis-ring fusion within the quinolizidine moiety is present, as was in the crystalline state by X-ray analysis.
- Research Organization:
- Adam Mickiewicz Univ., Poznan, Poland
- OSTI ID:
- 6321396
- Journal Information:
- J. Crystallogr. Spectrosc. Res.; (United States), Vol. 16:2
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
36 MATERIALS SCIENCE
74 ATOMIC AND MOLECULAR PHYSICS
PERCHLORATES
MOLECULAR STRUCTURE
NMR SPECTRA
ORTHORHOMBIC LATTICES
ALKALOIDS
BOND ANGLE
BOND LENGTHS
CARBON 13
CHEMICAL SHIFT
CONFORMATIONAL CHANGES
DEUTERIUM COMPOUNDS
DMSO
ELECTRON SPECTRA
HYPERFINE STRUCTURE
INFRARED SPECTRA
ISOTOPIC EXCHANGE
MASS SPECTRA
ORDER PARAMETERS
ORDER-DISORDER TRANSFORMATIONS
QUINOLINES
SPIN
STRUCTURAL CHEMICAL ANALYSIS
SYNTHESIS
X-RAY DIFFRACTION
ANGULAR MOMENTUM
AROMATICS
AZAARENES
AZINES
CARBON ISOTOPES
CHLORINE COMPOUNDS
COHERENT SCATTERING
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DIFFRACTION
DIMENSIONS
EVEN-ODD NUCLEI
HALOGEN COMPOUNDS
HETEROCYCLIC COMPOUNDS
HYDROGEN COMPOUNDS
ISOTOPES
LENGTH
LIGHT NUCLEI
NUCLEI
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
OXYGEN COMPOUNDS
PARTICLE PROPERTIES
PHASE TRANSFORMATIONS
PYRIDINES
SCATTERING
SPECTRA
STABLE ISOTOPES
SULFOXIDES
400201* - Chemical & Physicochemical Properties
360602 - Other Materials- Structure & Phase Studies
640302 - Atomic
Molecular & Chemical Physics- Atomic & Molecular Properties & Theory