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  • Amide hydrolysis  (1)
  • Pentathionates  (1)
  • X-ray crystallography  (1)
  • 1
    Electronic Resource
    Electronic Resource
    The phenomenon of conglomerate crystallization in coordination compounds. XXIII: The crystallization behavior of [cis-Co(en)2(N3)(SO3)] · 2H2O (I) and of [cis-Co(en)2(NO2)(SO3)] · H2O (II) (1993)
    Springer
    Structural chemistry 4 (1993), S. 235-245 
    Details
    ISSN: 1572-9001
    Keywords: Conglomerate crystallization ; cobalt complexes ; X-ray crystallography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A room temperature water solution of (I) crystallizes as a racemate, space groupP2 1/n with lattice constantsa=7.737(6),b=10.694(5),c=15.097(6) Å, andβ=102.83(5)°;V=1218.05 Å3 andd (calc; M.W.=337.24, Z=4) = 1.642 g cm−3. A total of 2381 data were collected over the range 4° ≤ 2θ 〈 50°; of these, 1452 (independent and withI ≥ 3σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 15.76 cm−1), and the relative transmission coefficients ranged from 0.8976 to 0.9984. Refinement led to the finalR(F) andR w(F) residuals of 0.0858 and 0.1116. A room temperature water solution of (II) crystallizes as a racemate in space group P21/c with lattice constantsa=6.638(3),b=11.425(8),c=15.147(16) Å, andβ=93.27(6)°; F=1146.8 Å andd (calc; M.W.=323.2,Z=4) = 1.872 g cm−3. A total of 2200 data were collected over the range 4° ≤ 2θ 〈 50°; of these, 1918 (independent and withI ≥ 3σ(I)) were used in the structural analysis. Data were corrected for absorption (μ=16.94 cm−1), and the relative transmission coefficients ranged from 0.9049 to 0.9967. Refinement led to the finalR(F) andR w(F) residuals of 0.0231 and 0.0279. The chirality symbol for the particular enantiomer of (I) refined here is ∧ (δδ), while for (II) the chirality symbol is ∧(δλ), which means that in the latter compound one of the en rings is in a higher energy conformation. We attribute this result to competitive intramolecular hydrogen-bonded interactions between the — NH2 hydrogens of the en ligands and the oxygens of the -NO2 and -SO3 ligands, strengths which are enhanced by coercing a change in sign of the torsional angle of one en ringa motion which permits both oxo ligands to form stronger hydrogen bonds while retaining proper O ⋯ O contacts. This phenomenon is not observed in (I) since the azide ligand does not compete with -SO3 for such hydrogen-bonded interactions, and nonbonded pair repulsions can be minimized without affecting the ability of — SO3 oxygens to form strong intramolecular hydrogen bonds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00673698
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    Syntheses of K[Co(tren)(NH3)(SO4)](S4O6)·2(H2O) and of [cis-α-Co(trien)(NH3)Cl](S5O6) - Compounds Produced by Hydrolytic Cleavage of Sulfur-Sulfur Bonds of the Tetrathionate Anion (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 717-722 
    Details
    ISSN: 1434-1948
    Keywords: Tetrathionates ; Pentathionates ; Sulfato ligands ; Cobalt(III) complexes ; Thiobacillus ferrooxidans ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: K[Co(tren)(NH3)(SO4)](S4O6)·2(H2O) (1) and [cis-α-Co-(trien)(NH3)Cl](S5O6) (2) have been prepared unexpectedly while attempting to obtain crystals suitable for X-ray diffraction of [Co(tren)(NH3)Cl](S4O6) (3) and of [cis-Co(trien)(NH3)Cl](S4O6) (4), respectively. 1 is derived from 3 by hydrolysis of the tetrathionate anion resulting in a sulfato moiety which displaces the chloro ligand from the coordination sphere of the metal center. 2 is derived from 4 by hydrolysis of the tetrathionate anion followed by reformation into pentathionate anion and H2S, as described in previous chromatographic work by Steudel. Compounds 1 and 2 have been characterized by elemental analyses and by single-crystal X-ray diffraction studies.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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    Paper (German National Licenses)
  • 3
    Electronic Resource
    Electronic Resource
    Crystal Structures of Oxalato and Oxamido Polyaminecobalt(III) Complexes Produced by Hydrolysis of Monooxamide (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 723-728 
    Details
    ISSN: 1434-1948
    Keywords: Monooxamide ; Amide hydrolysis ; Cobalt(III) ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of sodium monooxamide (H2NCOCO2Na) with trans-[Co(en)2Cl2]Cl, trans-[Co(3,2,3-tet)Cl2]Cl (3,2,3-tet = 1,5,8,12-tetraazadodecane), cis-α-[Co(trien)Cl2]Cl and [Co(tren)Cl2]Cl result in the formation of [Co(en)2(ox)]Cl · 4H2O (1), cis-β-[Co(3,2,3-tet)(ox)]Cl· 4 H2O (2), cis-α-[Co(trien)(ox)]Cl · 2 H2O (3), and [Co(tren)(ox)](ClO4) · 0.5 H2O (4) respectively, implying a hydrolytic cleavage of the amide bond. [Co(tren)(O,O′-oxam)]Cl2 · 2 H2O (5) (oxam = H2NCOCO2-) and p-[Co(tren)(NH3)(O-oxam)]Cl2 (6) have also been prepared in order to give mechanistic information for the hydrolysis of monooxamide. Crystal structures of the products are reported and possible pathways for the hydrolysis reactions are discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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    Paper (German National Licenses)
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