The crystal structure of Li2LaTa2O6N was determined from laboratory X-ray powder diffraction data (Cu Kα1) using the Rietveld method. The title compound is tetragonal with space group I4/mmm, Z=2, and unit-cell dimensions a=0.395 049(4) nm, c=1.850 97(3) nm, and V=0.288 869(6) nm3. The initial structural model was successfully derived by the direct methods and further refined by the Rietveld method, with the anisotropic atomic displacement parameters being assigned for all atoms. The final reliability indices were Rwp=5.73%, S=1.46, Rp=4.33%, RB=1.13%, and RF=0.53%. Li2LaTa2O6N has a layered perovskite structure similar to that of Li2LaTa2O7.

The subsolidus phase relations of the Dy-Fe-Al system have been investigated by means of X-ray powder diffraction. There are 5 ternary compounds, 10 binary compounds, and 21 three-phase regions in this system. The solid-solution regions of Dy(Fe1−xAlx)2, DyFe3−xAlx, Dy2(Fe1−xAlx)17, and DyFe12−xAlx have been determined based on the dependence of their unit-cell parameters on the Al content.

An orthorhombic fully ordered structural model is proposed for vaterite [space group Ama2, a=8.4721(5) Å, b=7.1575(7) Å, c=4.1265(4) Å, Z=4, and V=250.23(4) Å3]. It is based on a microtwinning hypothesis, with three domains rotated by 120° along the orthorhombic a axis, regenerating a pseudohexagonal habit. The solution came from direct space ab initio calculations applied to the powder diffraction data. However, five weak superstructure reflections seen in single-crystal and powder diffraction experiments, leading to a six times larger unit cell, are still unexplained.

Two selected members of the homologous series An+2BBn′O3n+3 (A=Sr and Ca; B and B′=Co) have been investigated for their crystal structures because of their potential applications as thermoelectric materials. A combined Rietveld refinement and spin-polarized magnetic geometry optimization technique was employed for the structural studies. Both the n=3 member, (Sr0.8Ca0.2)5Co4O12, and the n=4 member, Sr6Co5O15, have distorted hexagonal perovskite-related structures that possess one-dimensional cobalt oxide chains separated by alkaline-earth cations. The linear chains consist of one unit of CoO6 trigonal prism alternating with n units of CoO6 octahedra. Crystal structures and reference powder X-ray diffraction patterns of (Sr0.8Ca0.2)5Co4O11 [P3c1, a=9.4196(2) Å, c=19.9857(6) Å, V=825.83 Å3, and Dx=5.358 g/cm3] and Sr6Co5O15 [R32, a=9.497 64(12) Å, c=12.3956(2) Å, V=968.34 Å3, and Dx=5.455 g/cm3] are reported.

A suitable external standard method which was first described by O’Connor and Raven (1988) (“Application of the Rietveld refinement procedure in assaying powdered mixtures,” Powder Diffr. 3, 2–6) was used to determine the quantitative phase composition of a commonly used Ordinary Portland Cement (OPC). The method was also applied in order to determine amorphous contents in OPC. Also investigated were the impact of atomic displacement parameters and the microstrain on the calculated amorphous content. The investigations yielded evidence that said parameters do indeed exert an influence on the calculated amorphous content. On the basis of the data produced we can conclude that the method used is entirely to be recommended for the examination of OPC. No significant amorphous content could be proven in the OPC used.

The compound NH4Fe[Fe(CN)6]·xH2O—a commercially available “Prussian blue” pigment—crystallizes in the Fm3m space group, a=10.232(1) Å, based on X-ray powder diffraction (XRPD) data. XRPD investigations of other commercially available “Prussian blue” pigments and oil paints were undertaken. Results for the pigments showed that the XRPD techniques were able to differentiate several different Prussian blue phases that differed only slightly in chemical compositions. Results for the oil paints allowed for the determination of the major crystalline phases used as fillers. However, on the basis of XRPD investigations of oil paints prepared in our laboratory containing a mixture of true Prussian blue Fe4[Fe(CN)6]3·14H2O and BaSO4 (a common filler), the pigment was detectable only in concentrations higher than 2%. This result suggests that XRPD may not be a preferred technique for the identification of Prussian blue in paintings and other works of art because the concentration of this pigment in such materials is commonly less than 2%.

Gemstones are pieces of materials that once cut and polished are used as jewels or adornments. Gemstones may be single crystal (such as diamonds), polycrystalline (such as lapis lazuli), or amorphous (such as amber). In any case, gems may have inclusions that may yield a variety of optic effects. It is also important to unravel the crystal structure of the inclusion(s) in order to determine the origin of the gem and to help to understand their formation mechanism. Here, we expand the use of powder diffraction to identify crystalline inclusions in bulk gemstones highlighting Mo Kα radiation to penetrate within compact gems. Initially, rock crystal quartz with rutile needles was investigated and rutile diffraction peaks were more conspicuous in the Mo pattern than in the Cu pattern. Next, rock crystal quartz with beetle legs was characterized and the red iron oxide inclusion was identified as hematite. The study of a fake gem, glass showing aventurine effect, gave the diffraction peaks of metallic copper. Later, polycrystalline gems, moss agate, and aventurine quartz were also studied. The powder patterns of these compact gemstones could be successfully fitted using the Rietveld method. Finally, we discuss opportunities for further improvements in laboratory powder diffraction to characterize inclusions in compact gems.

New salts of barium with dicarboxylic acids (glutaric, adipic, pimelic, suberic, sebacic, and dodecanedioic) were synthesized and characterized by powder diffraction techniques. In addition to the basic crystallographic data and chemical analyses of barium glutarate hexahydrate {1}, barium adipate {2}, barium pimelate {3}, barium disuberate {4}, barium sebacate {5}, and barium dodecanedioate {6}, the processes of their thermal decomposition were investigated by XRPD. All the compounds decompose to barium carbonate at temperatures between 400 and 500 °C.

X-ray powder diffraction data, unit cell parameters, and space group for a new platinum-based anticancer complex cis-[bis(acetonitrile)]-[(1R,2R)-1,2-diaminocyclohexane-κN, κN′]platinum (II)nitrate (1:2) monohydrate, cis-[Pt(C2H3N)2(C6H14N2)](NO3)2·H2O, are presented [a=12.638(3) Å, b=12.153(2) Å, c=11.881(3) Å, β=95.145(4)°, space group P21, cell volume=1817.5 Å3, and Z=4]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurities were observed.

Ternary Al-Cu-W alloys were investigated. The previously reported Al3Ti-type phase (space group I4/mmm) with the average composition Al67Cu11.5W21.5 was found to have a=3.7296(4) Å and c=8.3797(10) Å. The ternary phase forming around Al67Cu21W12 has a hexagonal structure with a=8.6594(13) Å and c=15.2677(21) Å.

The 1-[N-(methyl)-(3,5-dimethylphenylamino)]methylnaphthalene (chemical formula C20H21N) was prepared by means of a condensation between alpha-naphthylaldehyde and 3,5-dimethylaniline in anhydrous ethanol to obtain the aldimine (1) which was reduced with NaBH4 to afford the 1-[N-(3,5-dimethylphenylamino)]methylnaphtalene (2), and finally, the compound (3) was obtained by N-alkylation reaction of (2) with methyl iodine (CH3I) and potassium carbonate (K2CO3) in acetone. Final compound (3) was purified by chromatographic column. The XRPD pattern for the new compound, 1-[N-(methyl)-(3,5-dimethylphenylamino)]methylnaphthalene, was obtained. This compound crystallizes in monoclinic system with space group P21/a (No. 14) and refined unit-cell parameters a=13.260(4) Å, b=15.495(5) Å, c=7.719(5) Å, β=90.19(6), and V=1586(1) Å3.

Methods of chemical preparation and XRD data are reported for a new triphosphate CuNa3P3O10 and two cyclotriphosphates SrRbP3O9·3H2O and SrRbP3O9. SrRbP3O9·3H2O was prepared by the method of ion-exchange resin, while CuNa3P3O10 and SrRbP3O9 were obtained by total dehydration of CuNa3P3O10·12H2O and SrRbP3O9·3H2O, respectively. CuNa3P3O10 crystallizes in the hexagonal system, with space group P-31c, Z=2, and the following unit-cell dimensions: a=b=7.022(1) Å, c=9.217(1) Å, M(20)=81, F(20)=117(0.003 419, 50), and V=393.24(2) Å3. SrRbP3O9·3H2O is orthorhombic, with Z=4, space group Pnma, and the following unit-cell dimensions: a=9.120(1) Å, b=8.141(1) Å, c=15.234(1) Å, M(20)=5.1, F(20)=5.8(0.0173,199), and V=1131.1(3) Å3. SrRbP3O9 is monoclinic, with space group P21/m or P21, Z=4, and the following unit-cell dimensions: a=14.958(3) Å, b=8.503(2) Å, c=7.898(2) Å, β=122.19(2)°, M(20)=9.9, F(20)=16.5(0.0189, 64), and V=850.2(8) Å3.

The mixed ligand complexes of manganese(II), nickel(II), copper(II), zinc(II), and cadmium(II) involving aspartic acid and benzoic acid have been synthesized. The complexes were studied by various spectroscopic techniques such as infrared, electronic, X-ray diffraction, and magnetic measurements. The complexes were found to have octahedral geometry. The X-ray powder diffraction results show that the crystal systems of Mn(II)-Asp-Ben complex are hexagonal, and Ni(II)-Asp-Ben, Cu(II)-Asp-Ben, Zn(II)-Asp-Ben, and Cd(II)-Asp-Ben complexes are found to be triclinic. The value of unit-cell parameters and XRD data for the five mixed ligand complexes are reported.

GSAS instrument parameters are tabulated for a variety of laboratory and synchrotron diffractometers to give users an idea of the typical ranges of profile parameters when they generate their own instrument parameter files. For modern high-resolution laboratory diffractometers, the parameters fall in the ranges 0<U<3, V=0, 0<W<4, 1<X<3, 0<Y<3, 1<asym<3, and 0<S/L<0.03. For synchrotron diffractometers, the parameters fall in the ranges 0<U<1.2, −1<V<0, 0<W<1, 0<X<1, 0<Y<1, 0<asym<0.5, 0<S/L<0.001, and 0<H/L<0.007. FULLPROF equivalents are also reported. The factors which are convoluted together to generate the instrument profile are described.