[Zr2F8(dmso)2(H2O)2], a dehydration product of [ZrF4(dmso)(H2O)2]⋅2H2O, crystallizes in the orthorhombic symmetry [space group Cmca, a=7.8266(3) Å, b=13.5847(5) Å, c=15.6119(6) Å, and Z=4]. The structure, solved ab initio in direct space from X-ray powder diffraction data, is built up from [Zr2F8O4] bipolyhedra formed by edge sharing of [ZrF5O2] pentagonal bipyramids (condensed from isolated [ZrF4O3] pentagonal bipyramids in the precursor). Difficulties associated with a fortuitous hexagonal pseudosymmetry were surmounted. The dmso departure at 220 °C leads to an amorphous phase.

This paper describes a method to determine the equilibrium transformation temperatures in low C steels using the in situ high-temperature X-ray diffraction technique. The samples were heated and then cooled from 1000 to 720 °C in a stepwise manner decreasing to −10 °C. Austenite and ferrite fractions were determined by a quantitative method using the integrated intensities of austenite (111)γ and ferrite (110)α peaks from X-ray diffraction patterns. The effect of the temperature on interplanar d spacings of (111) and (110) crystallographic planes was determined using 2θ maximum positions of the austenite (111)γ and ferrite (110)α peaks. The equilibrium transformation temperatures were determined to be Ae1=720 °C and Ae3=950 °C. The results are in excellent agreement with those obtained by dilatometric analysis and Thermo-Calc phase diagram simulation software. In addition, the results were supported by microstructural observations: the formation of thin ferrite films (5–10 μm) was observed at temperatures near to experimental Ae3.

The structure of a high-pressure polymorph of glycine (the β′-polymorph formed reversibly at 0.8 GPa from the β-polymorph) was determined from high-resolution X-ray powder diffraction data collected in situ in a diamond anvil cell at nine pressure points up to 2.6 GPa. X-ray powder diffraction study gave a structural model of at least the same quality as that obtained from a single-crystal diffraction experiment. The difference between the powder-diffraction and the single-crystal models is related to the orientation of the NH3-tails and the structure of the hydrogen-bonds network. The phase transition between the β- and β′-polymorphs is reversible and preserves a single crystal intact. No transformations were observed between the β-, α-, and β′-polymorphs on compression and decompression, although the α- and β′-polymorphs belong to the same space group (P21/c). The instability of the β- and γ-forms with pressure can be predicted easily when considering the densities of their structures versus pressure. The direction of the transformation (i.e., which of the high-pressure polymorphs is formed) is determined by structural filiation between the parent and the high-pressure phases because of the kinetic control of the transformations.

Tibolone is used for hormone reposition of postmenopause women and isotibolone is considered the major degradation product of tibolone. Isotibolone can also be present in tibolone API raw materials due to some inadequate synthesis. Its presence is then necessary to be identified and quantified in the quality control of both API and drug products. In this work we present the indexing of an isotibolone X-ray diffraction pattern measured with synchrotron light (λ=1.2407 Å) in the transmission mode. The characterization of the isotibolone sample by IR spectroscopy, elemental analysis, and thermal analysis are also presented. The isotibolone crystallographic data are a=6.8066 Å, b=20.7350 Å, c=6.4489 Å, β=76.428°, V=884.75 Å3, and space group P21, ρo=1.187 g cm−3, Z=2.

X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze form I of atorvastatin. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.3771 Å. Form I of atorvastatin was found to be triclinic with space group P1 and unit cell parameters a=5.4568(2) Å, b=9.8887(4) Å, c=30.3091(9) Å, α=76.801(3)°, β=99.177(5)°, γ=105.318(5)°, V=1527.1(1) Å3, Z=1, and M=1209.41 g mol−1 Alternatively, another unit cell dimension can be used to describe the same P1 crystal with a=5.4564(2) Å, b=9.8883(4) Å, c=29.6555(8) Å, α=95.745(3)°, β=94.297(5)°, γ=105.327(5)°, and V=1526.8(1) Å3.

A lattice thermal expansion study on Li2NiMn3O8, a high-voltage cathode material for lithium-ion batteries, was carried out by high-temperature X-ray diffraction from room temperature to 973 K. Rietveld refinement of a high-quality room-temperature diffraction pattern confirmed that Li2NiMn3O8 has the cubic Al2MgO4 spinel type of crystal structure. The analysis of the high-temperature X-ray diffraction patterns showed that the Li2NiMn3O8 structure remained stable and no phase transition was detected over the temperature range from 298 to 973 K. As expected, the value of lattice parameter a or unit cell volume V increases with increasing temperature. The increase in a or V is linear only in the low-temperature region and nonlinear over the entire temperature range from 298 to 973 K. Least-squares analysis of the data for a or V showed the thermal expansion of a or V for Li2NiMn3O8 can best be fitted by a 3-degree polynomial function of temperature. The linear thermal expansion coefficients for a and V averaged over the entire temperature range from 298 to 973 K were also calculated, and αTa=1.10×10−5 K−1; αTV=3.29×10−5 K−1.

Crystal structure of the skutterudite-related phase has been refined by the Rietveld method from X-ray powder diffraction data. Refined crystallographic data for CoSn1.5Te1.5 are a=12.9063(2) Å, c=15.7837(3) Å, V=2276.89(4) Å3, space group R3 (No. 148), Z=24, and Dx=7.50 g/cm3. The crystal structure of the title compound can be viewed as a modification of the skutterudite structure (CoAs3)—it is isostructural with CoGe1.5Te1.5 and IrSn1.5Te1.5. In the structure of CoSn1.5Te1.5, the Sn and Te atoms exhibit long-range ordering, which results in lowering of the original cubic symmetry of the skutterudite structure to the trigonal one.

SrBi2OB4O9 is a novel centrosymmetric borate oxide forming in the SrO–Bi2O3–B2O3 system. Its crystal structure has been determined ab initio from high-resolution X-ray and neutron powder diffraction data with the help of 11B MAS-NMR data. SrBi2OB4O9 crystallizes with a triclinic unit-cell with a=6.8657(1) Å, b=9.7976(1) Å, c=6.8148(1) Å, α=109.1270(8)°, β=101.8971(8)°, γ=96.1445(8)°, V=416.17(1) Å3, Z=2, space group P-1. Its structure consists of Bi2O4+ layers alternating along the b axis with SrB4O94− layers containing isolated B4O96− (〈2Δ〉Δ) tetraborate anions.

Four new derivatives of N-aryl-2,4-dichlorophenoxyacetamide, 2-(2,4-dichlorophenoxy)-N-(4-fluorophenyl)acetamide, N-(4-bromophenyl)-2-(2,4-dichlorophenoxy)acetamide, N-[4-chloro-3-(trifluoromethyl)phenyl]-2-(2,4-dichlorophenoxy)acetamide, and N-(3-chloro-4-fluorophenyl)-2-(2,4-dichlorophenoxy)acetamide, and two of N-alkyl-2,4-dichlorophenoxyacetamide, N-dodecyl-2,4-dichlorophenoxy-acetamide and 2-(2,4-dichlorophenoxy)-N-hexadecylacetamide, have been characterized by X-ray powder diffraction. These organic compounds are potential pesticides. Experimental 2θ peaks positions, relative peak intensities, values of d and Miller indices, and unit cell parameters are presented.

Co(II) complexes with benzoic acid and ternary complexes with ligands benzoic acid and histidine/aspartic acid have been synthesized and characterized using various spectroscopic methods. On the basis of infrared, UV-visible spectra, and magnetic data the complexes were found to be having octahedral polymeric geometry. X-ray powder diffraction results show that the crystal systems of Co(II)-Ben and Co(II)-Ben-Hist complexes are triclinic with lattice constants a=15.58 Å, b=11.92 Å, c=4.33 Å, α=96.08°, β=104.68°, γ=88.46°, and V=774.15 Å3 and a=18.88 Å, b=17.01 Å, c=15.13 Å, α=93.15°, β=89.41°, γ=100.71°, and V=4768.75 Å3, respectively. The Co(II)-Ben-Asp complex is orthorhombic with lattice constants a=21.57 Å, b=15.06 Å, c=11.40 Å. α=β=γ=90°, and V=3703.38 Å3.

This paper reports a reference X-ray powder diffraction pattern for a high-pressure phase, CaCo2O4, which has been reported recently to have a large Seebeck coefficient. The structure of CaCo2O4 is orthorhombic with space group Pnma, a=8.789(2) Å, b=2.9006(7) Å, c=10.282(3) Å, V=262.43 Å3, and Dc=5.62 g/cm3. This phase crystallizes in the CaFe2O4-type structure and consists of an edge- and corner-shared CoO6 octahedral network. The reference pattern has been submitted to the Powder Diffraction File (PDF).

Two ternary phases, designated τ4 and τ5, were revealed in Al–Ti–Pt. The τ4-phase with equiatomic composition (i.e., AlTiPt) was found to have a hexagonal structure with a=4.3908(9) Å and c=5.4823(10) Å (space group P63/mmc), and the τ5-phase, forming in a compositional range between ∼Al14Ti58Pt28 and Al21Ti63Pt16, has a tetragonal structure (possible space groups P42nm, P-4n2, and P42/mnm). The refined lattice parameters for Al15Ti60Pt25 are a=9.7019(20) Å and c=5.0231(13)Å.