Preparation of praseodymium(III) chloranilate and the crystal structures of Pr/sub 2/(C/sub 6/Cl/sub 2/O/sub 4/)/sub 3/. 8C/sub 2/H/sub 5/OH and Na/sub 3/(C/sub 6/H/sub 2/O(OH)(SO/sub 3/)/sub 2/). H/sub 2/O
The crystal structure of Pr/sub 2/(C/sub 6/Cl/sub 2/O/sub 4/)/sub 3/ x 8C/sub 2/H/sub 5/OH (1), a complex obtained by slow hydrolysis of o-chloranil (C/sub 6/Cl/sub 4/O/sub 2/) in acidic ethanol solution, has been determined by single-crystal x-ray diffraction techniques with data collected by counter methods. The structure of Na/sub 3/(C/sub 6/H/sub 2/O(OH)(SO/sub 3/)/sub 2/) x H/sub 2/O (2), the tranion of tiron, has also been determined by x-ray crystallography. Crystals of 1 form in triclinic space group P1 with a = 8.990 (1) Angstrom, b = 10.503 (2) Angstrom, c = 13.598 (1) Angstrom, ..cap alpha.. = 99.02 (1)/sup 0/, ..beta.. = 91.50 (1)/sup 0/, ..gamma.. = 94.44 (1)/sup 0/. The observed density of 1.643 g cm/sup -3/ is in agreement with the calculated value of 1.671 g cm/sup -3/ for one unit of Pr/sub 2/(C/sub 6/Cl/sub 2/O/sub 4/)/sub 3/ x 8C/sub 2/H/sub 5/OH per unit cell. The crystal structure is a three-dimensional network of alternating (C/sub 6/Cl/sub 2/O/sub 4/)/sup 2 -/ and Pr/sup 3 +/ ions in which the chloranilate rings lie about crystallographic inversion centers. Crystals of 2 form from aqueous solution in orthorhombic space group Pnma with a = 16.018 (2) Angstrom, b = 6.972 (2) Angstrom, and c = 9.700 (1) Angstrom. The (C/sub 6/H/sub 2/O(OH)(SO/sub 3/)/sub 2/)/sup 3 -/ species exhibits rigorous C/sub s/ symmetry, with only the two symmetry-related oxygen atoms of each SO/sub 3/ moiety lying out of the plane of the anion. There are no unusual aspects of the molecular geometry of 2. Full-matrix least-squares refinement of the structure has converged with R and R/sub w/ indices (on /F/) of 0.034 and 0.045 with use of the 805 observations with F/sub 0//sup 2/ > 3sigma(F/sub 0//sup 2/0. 5 figures, 10 tables
- Research Organization:
- Univ. of California, Berkeley
- DOE Contract Number:
- AC03-76SF00098
- OSTI ID:
- 5105434
- Journal Information:
- Inorg. Chem.; (United States), Vol. 22:21
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
PRASEODYMIUM COMPLEXES
STRUCTURAL CHEMICAL ANALYSIS
ALCOHOLS
ANISOTROPY
BOND ANGLE
BOND LENGTHS
COMPARATIVE EVALUATIONS
CRYSTALLOGRAPHY
EXPERIMENTAL DATA
HYDRATES
INFRARED SPECTRA
LATTICE PARAMETERS
LEAST SQUARE FIT
LIGANDS
MATHEMATICAL MODELS
MOLECULAR STRUCTURE
MONOCRYSTALS
ORTHORHOMBIC LATTICES
PHENOLATES
SAMPLE PREPARATION
SODIUM COMPLEXES
SPACE GROUPS
TIRON
TRICLINIC LATTICES
X-RAY DIFFRACTION
ALKALI METAL COMPLEXES
ALKALI METAL COMPOUNDS
AROMATICS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
CRYSTALS
DATA
DIFFRACTION
DIMENSIONS
HYDROXY COMPOUNDS
INFORMATION
LENGTH
MAXIMUM-LIKELIHOOD FIT
NUMERICAL DATA
NUMERICAL SOLUTION
ORGANIC ACIDS
ORGANIC COMPOUNDS
ORGANIC SULFUR COMPOUNDS
PHENOLS
POLYPHENOLS
RARE EARTH COMPLEXES
REAGENTS
SCATTERING
SODIUM COMPOUNDS
SPECTRA
SULFONIC ACIDS
400301* - Organic Chemistry- Chemical & Physicochemical Properties- (-1987)
400301 - Organic Chemistry- Chemical & Physicochemical Properties- (-1987)
400104 - Spectral Procedures- (-1987)