Powder diffraction data are presented for Ivabradine hydrochloride (pure and solvated forms), a drug marketed worldwide for symptomatic treatment of angina pectoris and inappropriate sinus tachycardia. [Ivrabradine: 3-[3-({[(7S)-3,4-dimethoxy bicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}(methyl)amino)propyl]-7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one]. Many are the different (polymorphic or solvated) phases claimed in the scientific or forensic literature. We have here prepared monophasic samples of six different ivabradine hydrochloride species. Exposure to water vapours, at room temperature, of the anhydrous δ-d form generated pure powders of the tetrahydrate form (the β-form). Two different anhydrous forms (β-d and α) were prepared by gentle, or extensive, heating of the β and δ-d forms, respectively. Acetonitrile and acetone solvates (hereafter called δ1- and δ2-forms) were obtained by precipitation methods from concentrated solutions. Diffraction data were collected on laboratory equipment with Ni-filtered CuKα radiation; cell parameters and space groups were determined from ab initio indexing procedures using the SVD algorithm.

Accurate minor and trace element analysis via micro-XRF can be more difficult to accomplish in single crystal and polycrystalline materials due to diffraction phenomena which obscure elemental peaks and distort the spectral background. A primary-beam filter is commonly used to eliminate diffractive artifacts as well as tube characteristic lines, but this dramatically reduces the sensitivity to lighter elements. One way around this is to collect a spectrum with unfiltered excitation to obtain the low-energy region, i.e., Na, Mg, Al, and Si, and then collect other portions of the spectrum under more optimized conditions. The fundamental parameter method is capable of using multiple spectra to quantify the complete element suite of the sample. By unifying the quantification for several spectra taken under different excitation conditions, the overall results can be improved. We have applied this method to selected cases for geological and metallurgical samples. The combined method gives better results for all elements than the single spectrum quantification as judged by agreement with the values from the supplier.

In the “double-Voigt” approach, an exact Voigt function describes both size- and strainbroadened profiles. The lattice strain is defined in terms of physically credible mean-square strain averageid over a distance in the diffracting domains. Analysis of Fourier coefficients in a harmonic approximation for strain coefficients leads to the Warren-Averbach method for the separation of size and strain contributions to diffraction line broadening. The model is introduced in the Rietveld refinement program in the foliowing way: Line widths are modeled with only four parameters in the isotropic case. Varied parameters are both surface- and volumeweighted domain sizes and root-mean-square strains averaged over two distances. Refined parameters determine the physically broadened Voigt line profile. Instrumental Voigt line profile parameters are added to obtain the observed (Voigt) line profile. To speed computation, the corresponding pseudo-Voigt function is calculated and used as a fitting function in refinement. This approach allows for both fast computer code and accurate modeling in terms of physically identifiable parameters.

Nanocrystalline powders of Fe and W were prepared by mechanical working in a highenergy Spex 8000 mixer/mill. The diffraction patterns were recorded with Co Kα radiation and the line profiles were subjected to a Fourier analysis. The size 〈D〉 of the coherently diffracting domains (x-ray particle size) and the root-mean square strains 〈ε2L〉1/2 were determined with the Warren-Averbach method. In addition, the integral breadths were evaluated and corrected for instrumental broadening assuming Cauchy line profiles. In order to separate particle size and strains, the corrected breadths β(s) = βcosθ/λ were plotted as a function of s = 2sinθ/λ, i.e., β(s) =(1/D) + 2ε s, where D = 〈D2/〈D〉 and ε is a strain averaged over the domain size D.

X-ray fluorescence analysis indicated that the W powders contained an iron and chromium contamination due to the abrasion of the stainless steel balls reaching a value of 24 at% Fe+Cr after 20h of milling. Since W is elastically isotropic, all available (hkl) reflections can be used in the Warren-Averbach and line breaddi analyses. After 20 h of milling, the W powder exhibited a particle size 〈D〉 = 35 Å and a strain 〈ε2〉1/2 = 0.52% at L = 30 Å. The integral breadths yielded the particle size D1 = 70 Å and the strain ε = 0.38%. in the case of Fe powder, also milled for 20 h, the (110) - (220) pair of reflections was used to calculate the particle size and strains. The Fourier analysis yielded the values 〈D〉 = 105 Å and 〈ε2〉1/2 = 0.59% at L = 30 Å. The corresponding integral breadth values are D1 = 280 Å and ε1 = 0.7%. The sum of the particle size Fourier coefficients is equal to the integral breadth particle size D1 = 125 Å, which is very close to value 〈D〉 = 105 Å indicating that the particle or domain sizes have a very narrow size distribution.

We report the dielectric properties of ACu3Ti4O12 (A = Eu2/3, Tb2/3, and Na1/2Eu1/2) (ACTO) in the frequency range of 40 Hz–2.5 MHz and in the temperature range of 293–473 K. The experimental results show that substituting for Ca improves the loss tangent of CaCu3Ti4O12 (CCTO). Although the dielectric constants largely decrease, they remain at a high level of 103. To identify the observed dielectric performances of ACTO, scanning electron microscopy and complex impedance measurements were conducted. The conducting mechanism for the grain of ACTO was found to be ion jumping rather than electron hopping (for the grain of CCTO). The results show that the decreased dielectric constant may be related to the decreased grain size, the different carrier in the grain, the different grain boundary properties, or a combination of these factors. All these factors are associated with the deficiency of oxygen vacancies in the samples of ACTO. The decreased loss tangent may be due to the increase in the grain boundary resistance.

X-ray powder diffraction data, unit-cell parameters, and space group for the holmium nitrate pentahydrate Ho(NO3)3•5H2O are reported [a = 6.642(8) Å, b = 9.55(2) Å, c = 10.56(2) Å, α = 63.672(1)°, β = 84.622(2)°, γ = 76.085(2)°, unit-cell volume V = 582,74 Å3, Z = 2, space group P-1]. Ho(NO3)3•5H2O is isostructural with ytrium nitrate pentahydrate (PDF 01-75-2104) (ICDD, 2011). All measured lines were indexed and are consistent with the P-1 space group. No detectable impurities were observed.

Structures of [Cd(C2H8N2)Cl2]n(1) and [Cd(C2H8N2)Br2]n(2) were solved from powder diffraction data. Compound (1) crystallizes in the space group Pbam (No. 55), a = 9.9021(7) Å, b = 7.8186(6) Å, c = 4.0705(3) Å, V = 315.13(3) Å3, Z = 2. (2) is isostructural: space group Pbam (No. 55), a = 10.405(2) Å, b = 7.8634(8) Å, c = 4.2079(5) Å, V = 344.28(6) Å3, Z = 2. The investigated compounds are examples of two-dimensional hybrid coordination polymers, in which neighboring metal centers are bridged via both organic and inorganic moieties: ethylenediamine molecules and halide anions. Both crystal structures were solved ab initio from powder data using direct methods.

There has been some confusion in the published literature concerning the structure of Metastudtite (UO2)O2(H2O)2 where differing unit cells and space groups have been cited for this compound. Owing to the absence of a refined structure for Metastudtite, Weck et al. (2012) have documented a first-principles study of Metastudtite using density functional theory (DFT). Their model presents the structure of Metastudtite as an orthorhombic (space group Pnma) structure with lattice parameters of a = 8.45, b = 8.72, and c = 6.75 Å. A Powder Diffraction File (PDF) database entry has been allocated for this hypothetical Metastudtite phase based on the DFT modeling (see 01-081-9033) and aforementioned Dalton Trans. manuscript. We have obtained phase pure powder X-ray diffraction data for Metastudtite and have confirmed the model of Weck et al. via Rietveld refinement (see Figure 1). Structural refinement of this powder diffraction dataset has yielded updated refined parameters. The new cell has been determined as a = 8.411(1), b = 8.744(1), and c = 6.505(1) Å; cell volume = 478.39 Å3. There are only subtle differences between the refined structure and that of the first-principles model derived from DFT. Notably, the b-axis is significantly contracted in the final refinement as compared with DFT. There were also subtle changes to the U1, O1, and O3 atom positions. Tabulated powder diffraction data (d's and I's) for the Metastudtite have been derived from the refined model and these new values can serve to augment the PDF entry 01-081-9033 with a more updated entry based on observed X-ray powder diffraction data.

Results from Monte Carlo simulations of two-dimensional projections for a simple real sample (an aluminium cube with a cylindrical hole filled by air or steel) in a realistic experimental environment are presented. A meaningful comparison with measurements was therefore possible. Coherent and incoherent scattering as well as excitation of fluorescent radiation are accounted for; multiple sequences of these interactions are followed up to a selectable order. Such simulations are important aids to modern metrological applications of computed tomography where the dimensional accuracy of hidden or inaccessible components of work pieces is determined. The complex process requires a high level of optimization of the instrumental parameters for each sample type whereby the accurate simulation of the physical interactions between X-rays and the sample material is a supplement and alternative to time consuming measurements.

In the framework of the study of the relationship between crystal packing of solid dyes and their visible reflectance spectra, the crystal structure of 3-methoxy-7H-benz[de]anthracen-7-one (Disperse Yellow 13, C18H12O2) has been determined using a combined set of Bragg–Brentano diffractometer and Guinier–Johannson photographic data with the grid search procedure. Parameters of the orthorhombic cell (P212121, No.19, Z=4) at 295 K are a=15.265(9) Å, b=20.524(9) Å, c=3.990(2) Å. Rietveld refinement gave Rp=0.085, Rb=0.135. The molecules form stacks along [001] with an interplanar spacing of 3.46 Å.

The X-ray powder diffraction pattern of the room temperature phase of Cd4GeSe6, a II4 □ IV VI6 semiconducting material, has been recorded and evaluated. This material crystallizes in the monoclinic space group Cc [No. 9] with a=12.847(3), b=7.407(2), c=12.854(2) Å, β=109.82(1)°, and Z=4. The powder diffraction pattern was also used to refine the crystal structure of this material employing the Rietveld method. The refinement of 56 parameters led to RWP=13.2%, RP=9.95% for 3751 step intensities and RB=7.05% and RF=5.20% for 833 reflections. Cd4GeSe6 can be considered a defect “adamantane-structure” material with a sphalerite-related superstructure.

As complementary metal oxide semiconductor devices continue to scale along the rapid pace of Moore’s law, gate dielectric materials with significantly higher dielectric constant (k=10–25) are being evaluated as replacements for conventional silicon dioxide, SiO2 (k=3.9), and silicon oxynitride. This allows for the introduction of a physically thicker film with lower leakage current and with capacitance equivalent to a thinner (1.0 nm and below) SiO2 layer (Schlom and Haeni, 2002; Wilk et al., 2001; Kingon et al., 2001). Although binary metal oxide films such as HfO2 and ZrO2 exhibit higher permittivity than their corresponding silicates and aluminates, alloyed with various molecular percents of SiO2 or Al2O3, respectively, they are compromised by lower onset of crystallization temperature which contributes a higher degree of interfacial microroughness and increased gate leakage current due to dislocations and oxygen vacancies generated along grain boundaries. Accordingly, development of hafnium silicate has been the subject of intense investigation as an advanced gate dielectric thin film designed to meet the device manufacturing requirements of thermal stability in direct contact with substrate silicon and metal gate electrode materials. In this paper, we present results corresponding to the utilization of total reflection X-ray fluorescence spectroscopy (TXRF) as a quick, accurate, nondestructive technique for hafnium silicate composition determination based on detection of the Hf:Si ratio of (HfO2)x(SiO2)1−x, where x varies over the range 0.2–1.0.

The versatility of confocal micro X-ray fluorescence (MXRF) in analyzing thin films on semiconductor wafers is demonstrated. Unlike conventional MXRF, confocal MXRF can depth profile sample layers and reduce spectral background. Nondestructive quantification of the silicon dioxide concentration in hafnium silicate thin films is an example of one application demonstrating the advantage of confocal MXRF. Additionally, the growth of titanium nitride films on various high-k gate dielectric substrates was analyzed with confocal MXRF due to its ability to detect sub-nm film thickness changes.

Accurate, digitized, spectral distribution data are given for CuKα radiation, comprising the profiles of CuKα1, CuKα2 and CuKα3,4. Three consistent analytical procedures are detailed for locating the peak of an X-ray emission line and are found to be superior to the conventional graphical centerline method.

An X-ray powder-diffraction pattern for boracite, Mg3B7O13Cl, is reported. Boracite is orthorhombic, space group Pca21, and the refined unit-cell parameters are a=8.557(6), b=8.553(8), c= 12.09(1) Å. X-ray powder-diffraction patterns have been calculated for the boracite-group minerals boracite, ericaite, trembathite and congolite. The calculated pattern for boracite is in good agreement with the observed pattern reported here, but the PDF entry (5-710) for boracite is missing several intense peaks. The calculated pattern for ericaite is in poor agreement with the PDF entry (29-697) for ericaite, and PDF 29-697 is for congolite, not ericaite. The calculated powder patterns presented here for these four minerals will facilitate their identification via X-ray powder diffraction. © 1995 International Centre for Diffraction Data.

The Debye-Scherrer technique and filtered Cu Kα, radiation were used to obtain powder data for reflections to an angle of 2θ = 155°; a vertical scanning diffractometer was used to obtain intensity data to an angle of 2θ = 99°. The space group is with Z = 4. The lattice parameters of the tetragonal unit cell were measured to be a = 6.189 (1) Å and c = 12.391 (1) Å with c/a = 2.002 The unit cell volume was calculated as U = 474.6 (2) Å3 and the X-ray density as Dx = 6.07 ± 0.003 gm cm−3. By comparing measured and theoretical intensity values, the sublattice distortion parameter x was estimated to be x = 0.227 (12).

Gallium iron oxide GaFeO3 and the substituted GaFeO3 with Cr and Mn, i.e., Ga(Fe0.95Me0.05)O3, and (Ga0.95Me0.05)FeO3; Me=Cr and Mn, have been synthesized and investigated by X-ray powder diffraction. The refined structural parameters of the considered samples using the Rietveld technique showed a considerable distortion in the polyhedron around different cations, which may have an effect on the piezoelectricity of the studied samples. There are also changes in the interatomic distances between different cations, which may have a direct influence on the ferromagnetic properties of the samples. Crystallite size and microstrain are anisotropic and the largest along the b axis, which may be responsible for the piezoelectricity. The correlations between all these changeable parameters will be discussed.

An ordered oxygen-deficient tetragonal perovskite compound La1.67Sr0.33Cu205 has been synthesized by solid state reaction. X-ray powder diffraction was used to characterize the material. Unit cell parameters least-squares refined from non-overlapping diffraction peaks are a = 10.8696(9)Å, c = 3.8612(6)Å and V = 456.2(1)Å3. X-ray powder data have been obtained for the experimentally observed peak positions corrected for systematic errors, the relative intensities, values of dexp and the Miller indices of both resolved and overlapping reflections. The experimental diffraction pattern was compared to computer simulated patterns calculated from the neutron crystal structure parameters and the non-oxygen-deficient LaCuO3 compound. The figure of merit is F30 = 33.8 (0.018, 48).

Two homeotypical phases occur at the mole fraction xAl≈0.75 in the ternary system Co-Ni-Al: the pseudoternary intermetallic compound (Co, Ni)4Al13(h) (space group C2/m, Pearson code mC(34-1.8)) [Notation, according to Parthé et al. (1993). TYPIX, Standardized Data and Crystal Chemical Characterization of Inorganic Structure Types (Springer, Berlin), Vol. 2, p. 269, Vol. 3, p. 1055]. For structures with partly occupied sites, the hybrid Pearson code is given as (the sum of the multiplicities of all, fully or partly occupied sites in the unit cell)−(number of structural vacancies in the unit cell)], and the ternary compound Co2NiAl9 (Immm, oI96). Powder diffraction data are reported for these materials or phases—from the viewpoint of phase equilibria—immediately neighboring phases.

An iterative external standard method of X-ray diffraction is presented to overcome the difficulties of preferred orientation and peak overlap encountered in quantitative phase analysis. Instead of using only a single line intensity in the traditional external standard technique, all the reflection data are used in the calculation. The accuracy and applicability of this method was tested on a series of two-phase powder mixtures with known composition. The results show markedly good agreement with the actual values. As an example, the analysis was applied to the data collected from an as plated electrodeposited Zn-Fe coating. The determined phase composition of the coating was found to be 88.2 +/− 5.3 wt % δ-phase and 11.8 +/− 0.7 wt % η -phase.