13986-26-0Relevant articles and documents
Synthesis and structure of an infinite-chain form of ZrI2 (α)
Guthrie, Dennis H.,Corbett, John D.
, p. 256 - 263 (1981)
The synthesis of a second polymorph of ZrI2 has been achieved by a transport reaction between ZrI4 and zirconium metal under a 750 850°C gradient in a sealed tantalum tube. The black lath-like crystals produced in the 775°C region occur in space group P21 m with a = 6.821(2) A, b = 3.741(1) A, c = 14.937(3) A, β = 95.66(3)°, Z = 4. A total of 669 independent reflections with 2θ ≤ 50° and I > 3σ(I) were measured at room temperature on a four-circle automated diffractometer with monochromatized MoKα radiation and were corrected for absorption (μ = 190 cm-1). The structure was solved by direct methods and full-matrix least-squares refinement of all atoms with anisotropic thermal parameters to give final residuals R = 0.064 and Rw = 0.079. This phase is isoelectronic and isostructural with β-MoTe2, a distorted CdI2-type structure in which the zirconium atoms are displaced 0.440 A from the octahedral centers along a to form infinite zigzag metal chains (dZrZr = 3.182(3) A) parallel to b. The phase is a diamagnetic semiconductor at room temperature (Eg ～ 0.1 eV).
New Double Salts with Boron-Centered Zirconium Clusters: Syntheses and Structures of Cs[ZrCl5]·Cs2[(Zr6B)X 15] (X = Cl or Cl+I), and Anion Distribution in the Mixed Halide Phase
Rohm, Henning W.,K?ckerling, Martin
, p. 2356 - 2362 (2003)
Two new members of a double salt containing halide supported zirconium octahedra were obtained from solid state reactions. Single-crystal X-ray data refinements established the isotypic compounds as Cs[ZrCl5] ·Cs2[(Zr6B)Cl15] (I) (R?c, Z = 6, a = 12.765(2), c = 34.652(6) A?, R1(F) = 0.0339, wR2(F2) = 0.0770) and the mixed halide Cs[ZrCl5]·Cs2[(Zr 6B)Cl14.57(2)I0.43] (II) (R3?c, Z = 6, a = 12.777(2), c = 34.668(7) A?, R1(F) = 0.0459, wR2(F2) = 0.1279), respectively. The structure contains a network of boron centered [(Zr 6B)Cli12] clusters interbridged three-dimensionally by 6/2 Xa-a atoms at all zirconium vertices (X = Cl, or Cl+1, respectively). Within voids of the cluster network [ZrCl 5]- anions and Cs+ cations are located, allowing for the description as a double salt. The [ZrCl5] - anion (D3h-symmetry) has been found so far only in this structure type. The space requirement of a variety of transition metal complexes is estimated and compared with the volume of the [ZrCl 5]- anion in order to see if other double salts are geometrically possible. Besides the unusual [ZrCl5]- ion the mixed chloride-iodide structure reveals another interesting feature. Contrary to many other structures an ordered chlorine atom substitution by iodine is observed on the cluster interconnecting site. The phase width for Cs[ZrCl5]·Cs2[(Zr6B)Cl 15-XIX] has been found to cover 0 ≤ x ≤ 1.
KINETICS OF FORMATION OF SOLID IODIDES ON ZIRCONIUM.
Cubicciotti,Scott
, p. 241 - 250 (1981)
The reaction of zirconium with gaseous ZrI//4 was studied in the temperature range 300-500 degree C. Specimens of zirconium were heated in sealed glass tubes with solid ZrI//4 which was kept at a lower temperature to maintain a fixed ZrI//4 pressure. The solid zirconium iodides that formed on the zirconium surface were examined by scanning electron microscopy. Initially, isolated clusters of ZrI crystals formed which subsequently coalesced into a layer of ZrI. A layer of diiodide formed on top of the layer of monoiodide in later stages. The amount of iodide on the surface was determined by chemical analysis.
THERMODYNAMICS OF VAPORIZATION OF ZrI4 IN THE UNIVARIANT REGION: ZIRCONIUM MONOIODIDE/ZIRCONIUM.
Cubicciotti,Lau
, p. 196 - 199 (1981)
The pressures of gaseous ZrI//4 over solid zirconium iodides in the composition range ZrI to Zr were measured by a torsion-effusion method. A univariant region was observed between solids of composition ZrI//1//. //0//5 and Zr. The results extend literature information on the thermodynamics of vaporization in the ZrI//4/Zr region of the Zr-I system.
Arene Derivatives of Zirconium(II) and Hafnium(II)
Calderazzo, Fausto,Pallavicini, Piersandro,Pampaloni, Guido
, p. 1813 - 1818 (2007/10/02)
The anhydrous tetrahalides MX4 (M = Zr or Hf, X = Br or I) were prepared by treating M(BH4)4 with dry HX in n-heptane as solvent, followed by sublimation under reduced pressure.The reaction of ZrCl4 with Al-AlCl3-aromatic hydrocarbon systems led to soluti
