Thermodynamics Research Center / ThermoML | Journal of Chemical and Engineering Data

Synthesis, Crystal Structure, and Thermal Properties of a Holmium(III) Benzoate Complex with 1,10-Phenanthroline

Wang, J.-F.[Juan-Fen], Ren, N.[Ning], Zhang, J.-J.[Jian-Jun], Wu, K.-Z.[Ke-Zhong], Wang, S.-P.[Shu-Ping]
J. Chem. Eng. Data 2010, 55, 11, 4982-4989
ABSTRACT
A binuclear holmium(III) benzoate 1,10-phenanthroline ternary complex, [Ho(BA)3phen]2, was synthesized and characterized by elemental analysis, IR and UV spectroscopy, molar conductance, single crystal X-ray diffraction, and thermogravimetric/differential thermogravimetric (TG-DTG) techniques. The crystal of the complex is in a triclinic crystal system, space group p with a = 10.7162(18) A, b = 11.845(3) A, c = 12.227(2) A, a = 105.141(11)deg , ss = 93.845(8)deg , ? = 112.880(5)deg , and Z = 1. Each Ho(III) cation in the crystal is eight-coordinated including two O atoms of one chelating bidentate carboxylate group, four O atoms of four bridging bidentate carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule, yielding a distorted square antiprismatic comformation. The thermal analysis of [Ho(BA)3phen]2 has been performed by simultaneous TG/DSC-FTIR techniques. By the Malek method, SB(m,n) was defined as a kinetic model for the second-step thermal decomposition. The activation energy E of this step is 296.99 kJ*mol-1, and the pre-exponential factor ln A is 39.99 s-1. The thermodynamic parameters, Gibbs energy (?G?), enthalpy (?H?), and entropy (?S?) of activation, at the peak temperatures were also calculated. The heat capacity of [Ho(BA)3phen]2 was measured by differential scanning calorimetry (DSC) over the temperature range from (254 to 470) K. In addition, the values of the experimental heat capacities were fitted to a polynomial equation with the least-squares method.
Compounds
# Formula Name
1 C66H46Ho2N4O12 tetrakis[.mu.-(benzoato-.kappa.O:.kappa.O')]bis(benzoato-.kappa.O,.kappa.O')bis(1,10-phenanthroline-.kappa.N1,.kappa.N10)diholmium
Datasets
The table above is generated from the ThermoML associated json file (link above). POMD and RXND refer to PureOrMixture and Reaction Datasets. The compound numbers are included in properties, variables, and phases, if specificied; the numbers refer to the table of compounds on the left.
Type Compound-# Property Variable Constraint Phase Method #Points
  • POMD
  • 1
  • Molar heat capacity at constant pressure, J/K/mol ; Crystal
  • Temperature, K; Crystal
  • Pressure, kPa; Crystal
  • Crystal
  • Small sample (50 mg) DSC
  • 73