A modified method for polynomial smoothing and the calculation of derivatives of equally spaced step scan powder diffraction data is presented. The algorithm takes the angular dependence of the full width at half maximum (FWHM) of diffraction peaks into account, is very effective, and easy to code.

Mixed lead chloride oxalate, Pb2Cl2(C2O4), has been obtained in a polycrystalline form in the course of a study on precursors of nanocrystalline PZT-type oxides. Its crystal structure has been solved ab initio from powder diffraction data collected using a monochromatic radiation from a conventional X-ray source. The symmetry is monoclinic, space group C2/m, the cell dimensions are a=5.9411(3) Å, b=5.8714(4) Å, c=9.4212(4) Å, β=95.232(4)° and Z=2. The structure consists of a stacking of complex double sheets, built from lead polyhedra, parallel to (001) and connected together through oxalate groups. The lead atom is nine-fold coordinated by four O atoms from one bidentate and two monodentate oxalate groups and five Cl atoms. The polyhedron can be described as a highly distorted square antiprism mono-capped by a Cl atom. The thermal behavior of lead chloride oxalate, in vacuum and in air, is carefully described from temperature-dependent powder diffraction and thermogravimetric measurements. It is shown that reaction pathways are complicated by the identification of various oxide chloride phases.

The crystal structure of anhydrous δ-D-mannitol (C6H14O6) was solved from high-resolution synchrotron X-ray powder diffraction data collected on a mixture containing 20% and 80% w/w of β- and δ-D-mannitol, respectively. The direct space simulated annealing program PSSP, and Rietveld analysis employing GSAS were used to determine and refine the structure. The polymorph has monoclinic symmetry, space group P21 with a=5.089 41(5) Å, b=18.2504(2) Å, c=4.917 02(5) Å, and β=118.303(2)°. There is one molecule in the irreducible volume of the unit cell. The pattern of hydrogen bonding is significantly different than the previously known α and β forms.

Zn7Sb2O12 is known to adopt an inverse spinel crystal structure, in which Zn2+ occupies the eight tetrahedral positions and Sb5+ and Zn2+ randomly occupy the 16 octahedral positions. Samples of Zn7−xNixSb2O12 (x=0, 1, 2, 3, and 4) were synthesized using a modified polymeric precursor method, known as the Pechini method. The crystal structure of the powders was characterized by Rietveld refinement with X-ray diffraction data. The results show that for x=0, 1, and 2 Ni substitutes for Zn2+ in the octahedral sites, and that for x=3 and 4 it is assumed that Ni2+ replaces Zn2+ ions in both the octahedral and tetrahedral positions. It is also observed for x=3 and 4 the formation of two spinel phases.

Methods of chemical preparation and crystal data are reported for two new anhydrous cyclotriphosphates MIIK4(P3O9)2 (MII=Co2+ and Mn2+). These anhydrous cyclotriphosphates CoK4(P3O9)2 and MnK4(P3O9)2 were obtained by total dehydration of corresponding hydrated cyclotriphosphates CoK4(P3O9)2.7H2O and MnK4(P3O9)2.2H2O. CoK4(P3O9)2 is triclinic, space group P−1, Z=1 with the following unit-cell dimensions: a=6.29(3) Å, b=8.00(1)Å, c=13.05(8)Å, α=86.03(5)°, β=98.00(1)°, γ=68.11(2)°. MnK4(P3O9)2 crystallizes in the rhombohedral system, space group P−31c, Z=2 with the following unit-cell dimensions: a=b=7.337(3)Å, c=19.920(1)Å.

A new cobalt molybdate with the formula NaCo2OH(H2O)(MoO4)2 was synthesized by hydrothermal reaction at 200 °C and was found to possess the Φx type structure. The crystalline system of this material is monoclinic and its cell parameters are a=9.3792 (2), b=6.3331 (1), c=7.6281 (2) Å and β=115.832°, obeying the C2/m space group symmetry.

Calcium sodium iminodisulphonate trihydrate was first described by Divers and Haga [J. Chem. Soc. 943–968, (1892)]. It has recently been found as one of several crystalline products resulting from the removal of sulphur dioxide from flue gas. It has not so far been included in the ICCD powder diffraction file.

Methods of chemical preparation and crystal data are reported for four new condensed phosphates: two hydrated cyclotriphosphates with a general formula SrMIP3O9⋅3H2O (MI=K+,Tl+) and their corresponding anhydrous cyclotriphosphates SrMIP3O9 (MI=K+,Tl+). The two hydrated condensed phosphates, SrKP3O9⋅3H2O and SrTlP3O9⋅3H2O, belong to previously investigated structure types. SrKP3O9⋅3H2O and SrTlP3O9⋅3H2O are orthorhombic, Z=4, space group Pnma, with respectively the following unit-cell dimensions: a=9.082(2) Å, b=8.133(2) Å, c=15.009(2) Å, M(20)=49, F(25)=61(0.0052;79) and a=9.115(7) Å, b=8.139(7) Å, c=15.221(2) Å, M(20)=285, F(30)=522(0.000 411;140). SrKP3O9 and SrTlP3O9 are monoclinic, space group P21/m or P21, Z=4, with, respectively, the following unit-cell dimensions: a=14.957(1) Å, b=8.372(1) Å, c=7.909(1) Å, β=102.27(1)°, M(20)=81, F(24)=95(0.000 025;92) and a=14.544(2) Å, b=8.639(1) Å, c=7.727(1) Å, β=102.05(1)°, M(20)=66, F(30)=78(0.003 098;125).

The new heteropoly blue compound (MoO2)0.5PMo14O42, which is relevant in the context of catalytic activity of heteropoly-molybdates, was prepared by controlled thermolysis of (NH4)3PMo12O40 at 730 K in a nitrogen atmosphere. Powder X-ray diffraction analysis showed that this compound has a cubic unit cell, space group Pn3m (No. 224), with ao=11.795(2) Å, Z=2 and DXR=4.2466 g cm−3. Computer modeling and Rietveld analysis of powder diffraction patterns led to a proposed structure of the corresponding Keggin-cage unit PMo14O42.

Five new aliphatic-aromatic thiodiols: 1,2-bis[4-(2′-hydroxyethylthio)phenyl]ethane (C18H22O2S2), 1,2-bis[4-(3′-hydroxypropylthio)phenyl]ethane (C20H26O2S2), 1,2-bis[4-(6′-hydroxyhexylthio)phenyl]ethane (C26H38O2S2), 1,2-bis[4-(10′-hydroxydecylthio)phenyl]ethane (C34H54O2S2), 1,2-bis[4-(11′-hydroxyundecylthio)phenyl]ethane (C36H58O2S2) have been characterized by X-ray powder diffraction. These thiodiols can be used for synthesis of thermoplastic nonsegmented polyurethanes. Experimental 2θ peaks positions, relative peak intensities, values of d and Miller indices as well as unit cell parameters are reported.

The X-ray powder diffraction pattern for a new precursor in the synthesis of pyridyl tetrahydroquinolines was determined. 4-N-(4-methylphenyl)amine-4-(3′-pyridyl)-1-butene is monoclinic with refined unit cell parameters a=16.554(5), b=7.204(2), c=12.257(3) Å, β=99.76(2)°, V=1440.5(4) Å3, Z=4, and Dx=1.098 g/cm3, with space group P21/n (No. 14).

The potassium μ-Oxo-bis(oxodiperoxovanadate)(4-) hydrate K4[O{VO(O2)2}2]*H2O was prepared, and its X-ray powder diffraction patterns have been recorded at room temperature. The unit cell parameters were refined to a=6.7097(1) Å, b=9.9574(1) Å, c=15.8250(3) Å, β=93.69(6)°, space group P21/c (14). The sample of K4V2O11*H2O was characterized by IR spectroscopy and analytical investigation. Results of crystal structure refinement by Rietveld method are presented; final RF and Rwp are 13 and 16%, respectively.

PLZT of the compositions 0≤L≤12, and 0≤T≤10 was studied in order to describe the structure of the phases as a function of composition. This range contains a mixed region with PLZT+La2Zr2O7, an orthorhombic, a rhombohedral (hexagonal) phase, a tetragonal phase, and a mixture of different PLZT phases. Each phase pure composition is described by X-ray diffraction.

Quaternary compound CuZnGa3Te6 was synthesized by the melt and anneal technique. The defect-tetrahedral structure compound crystallized in the tetragonal unit cell with possible space group I4 and Z=4/3. Complete powder diffraction data were obtained and unit cell parameters a and c, and X-ray density were calculated. These were a=0.5946(2) nm, c=1.1891(5) nm, and Dx=5.81×103 kg/m3.

The X-ray powder diffraction patterns of two liquid aniline derivatives o-chloroaniline, and m-chloroaniline were measured at 250 °K in a low temperature chamber. Both compounds crystallize in the orthorhombic system with the unit cell parameters refined to a=1.8391(3) nm, b=1.0357(2) nm, c=0.6092(1) nm, space group Pmmm(47) and a=0.450 39(9) nm, b=1.9820(4) nm, c=1.2699(4) nm, space group Pcca(54) for o-chloroaniline and m-chloroaniline, respectively. Investigated at room temperature, 2,6-dichloroaniline crystallizes in the monoclinic system, space group P21/c(14), a=1.1329(2) nm, b=0.41093(8) nm, c=1.5445(3) nm, α=γ=90° β=99.96(2)°.