A laboratory-scale X-ray diffractometer for obtaining high X-ray intensity data was developed. The apparatus, equipped with 600 W CuKα radiation with a Ni filter, incorporates technology that dramatically improves the quality of X-ray diffraction. The system comprises of a low-noise one-dimensional silicon strip detector, a variable slit, and a goniometer with a radius as small as 150 mm. A variable knife edge was used as a countermeasure for unwanted scattering, particularly in the low angle range. With this system, cement may be analyzed within 5 min. NIST 2686 standard reference material was analyzed using the newly developed diffractometer, and the quantitative analysis results for the major phases are in agreement with the certified values of the reference material.

A series of iron-doped lead titanate PbTi(1−x)FexO(3−δ) samples in the x = 0–1 composition range was prepared using sol–gel synthesis at a calcination temperature of 700 °C. The room temperature CuKα powder diffraction data collected from x = 0, 0.005, 0.01, 0.025, 0.05, 0.075, 0.1, 0.125, 0.15, 0.175, 0.2, and 0.3 samples were analyzed using the Rietveld method. Magnetoplumbite (PbFe12O19) secondary phase formation was observed at compositions x = 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, and 1. Fe-composition dependent decrease of tetragonal distortion has been observed. According to Vegard's law, the B-site iron solubility limit in the lead titanate host was found to be approximately 10 mol% (x = 0.1). Homogeneous distribution of dopants below the solubility limit was evidenced by the linear behavior of unit-cell parameters. The absence of a cubic phase and the persistence of distorted oxygen octahedra indicated the existence of ferroelectric properties even at the x = 0.3 composition. Beyond x = 0.3, the P4mm tetragonal model was determined to be invalid possibly because of oxygen defect driven structural changes, mainly tilting Fe-polyhedra.

Polycrystalline Sr3Sm2(BO3)4 borate has been synthesized through a solid-state reaction, and the title compound is stable in air and water. Its crystal structure was investigated from powder X-ray diffraction data using the Rietveld method. The fundamental building units of the crystal Sr3Sm2(BO3)4 are isolated BO3 anionic groups, distorted Sm–O polyhedra, and irregular Sr–O polyhedra, with the crystal structure isostructural to Sr3Nd2(BO3)4. The infrared spectrum of Sr3Sm2(BO3)4 has been measured, which is consistent with the crystallographic study. According to diffuse reflection measurement of Sr3Sm2(BO3)4 powders, the absorption edge is in the deep UV range and UV-vis transmittance is very high. Phosphor Sr3Sm2(BO3)4 exhibits an orange-red emission.

Twenty-seven scapolite samples from various localities and with compositions between Me6–93 were obtained using electron microprobe analysis (EMPA). Their unit-cell parameters were obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinements using space group P42/n. The EMPA data show the well-known discontinuity at Me75. In addition, the unit-cell parameters, especially c, show a discontinuity at Me75 (=five Al atoms per formula unit, apfu), ideally NaCa3[Al5Si7O24](CO3), where the scapolite solid solution is divided into two (Me% = [Ca/(Ca + Na + K)] × 100). A maximum c parameter value occurs at Me37.5 (=four Al apfu ideally), where complete Al–Si, Na–Ca, and Cl–CO3 order occurs. The unit-cell volume, V, varies smoothly with Me% and Al apfu across the series.

We conducted in-situ high-temperature neutron and X-ray diffraction studies on tetragonal PbTiO3. Using a combination of Rietveld analysis and Maximum Entropy Method, the nuclear and charge density distributions were determined as a function of temperature up to 460 °C. The ionic states obtained from charge density distributions reveal that the covalency of Pb–O2 bonds gradually weakens with increasing temperature. The spontaneous polarizations calculated from the contributions of ionic state, ionic displacement, and nuclear polarization, are in good agreement with the experimental measurements. This method provides an effective approach to determine spontaneous polarizations in multiferroics with high-current leakage and low resistance.

The cause of birefringence in several garnet-group minerals with general chemical formula, [8]X3[6]Y2[4]Z3[4]O12, which was observed over 100 years ago, is unknown, although many different reasons were proposed, including symmetry lower than cubic. In this study, electron microprobe analyses (EMPA) were obtained for a Ti-rich andradite, ideally Ca3(Fe23+)Si3O12, from Magnet Cove, Arkansas, USA, and the results show that the sample is inhomogeneous with two distinct compositions. The crystal structure was refined by the Rietveld method, cubic space group $Ia\overline 3 d$, and monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data, which shows a mixture of three distinct cubic phases that are intergrown together and cause birefringence because of strain arising from small structural mismatch. This mixture of three cubic phases was not observed by any other experimental technique. These results have many implications, including garnet phase transitions from cubic to lower symmetry in the mantle, which has important geophysical consequences.

X-ray powder diffraction data, unit-cell parameters and space group for C8H20CuN10O8 are presented [a = 5.262 (2) Å, b = 14.051 (3) Å, c = 12.183 (3) Å, β = 96.912 (5)°, unit-cell volume V = 894.3 Å3, Z = 2, space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

A new compound Er3Co4Al12 was prepared by arc melting under argon atmosphere. The powder X-ray diffraction data of Er3Co4Al12 were successfully indexed, giving a hexagonal structure with a = 8.6185(2) Å, c = 9.2347(3) Å, and unit-cell volume V = 594.04 Å3. Compound Er3Co4Al12 has the Gd3Ru4Al12 type-structure, Z = 2 and space group P63/mmc.

X-ray powder diffraction data, unit-cell parameters, and space group for a new bis(β-diiminato) Cu(II) complex, C44H54CuN4O4, are reported [a = 8.683(3) Å, b = 11.216(3) Å, c = 11.753(4) Å, α = 66.27(3), β = 84.61(3), γ = 78.85(3), unit-cell volume V = 1027.77 Å3, Z = 1, and space group P-1]. All measured lines were indexed and are consistent with the P-1 space group. No detectable impurity was observed.

Crystal and X-ray powder diffraction data are presented for the Al3Ho2Si2 ternary compound. The powder pattern was indexed and refined on a monoclinic cell with the Al3Y2Si2 structure type with space group C12/m1, a = 10.1096(2) Å, b = 4.020(6) Å, c = 6.5734(6) Å, β = 100.848(2)°, V = 262.37 Å3, Z = 2ρx = 5.910 g cm−3, F30 = 142.8(0.006, 35), and RIR = 0.91.

X-ray powder diffraction data, unit-cell parameters, and space group for norandrostenedione, C18H24O2, are reported [a = 26.3955(15) Å, b = 8.0476(4) Å, c = 7.3002(3) Å, α = β = γ = 90°, unit-cell volume V = 1550.71 Å3, Z = 4, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurity was observed.

X-ray powder diffraction data, unit-cell parameters, and space group for potassium erbium fluoride, K0.5Er0.5F2, are reported [a = 5.6862(5) Å, unit-cell volume V = 183.85 Å3, Z = 4, and space group Fm-3m]. Potassium erbium fluoride is isostructural with a large family of fluorides represented by the mineral fluorite CaF2. All of the measured lines of the title compound were indexed and are consistent with the Fm-3m space group. No detectable impurities were observed.

The 2,4-diaryl 1,2,3,4-tetrahydroquinoline derivative (1), described in the title (Chemical formula: C23H22N2O3), was synthesized via the “one-pot” three-component imino Diels–Alder reaction catalyzed by Cu(OTf)2. Molecular characterization was performed by 1H and 13C NMR, Fourier transform-infrared, and gas chromatography-mass spectrometry. The X-ray powder diffraction pattern for the title compound was analyzed and found to be crystallized in an orthorhombic system with space group P212121 (No. 19) and refined unit-cell parameters a = 8.6415(8) Å, b = 12.679(2) Å, c = 17.601(2) Å, and V = 1928.4(2) Å3.

X-ray powder diffraction data, unit-cell parameters and space group for peiminine, C27H43NO3, are reported (a = 30.2026 Å, b = 5.8468 Å, c = 14.4344 Å, β = 96.9456°, unit-cell volume V = 2530.23 Å3, Z = 2 and space group P21). All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

The 4-benzyloxy-1-oxaspiro-[4.6]-undec-3-en-2-one (C17H20O3) was prepared through a domino reaction from benzyl α-hydroxycycloheptanecarboxylate and the cumulated ylide Ph3P=C=C=O by: (i) addition and (ii) intramolecular Wittig Olefination reaction. The reaction was carried out using anhydrous toluene as solvent under an argon atmosphere in a Schlenk flask. Molecular characterization was performed by Fourier transform infrared spectroscopy, gas chromatography-mass spectrometry, (1H,13C – mono and bidimensional) nuclear magnetic resonance spectroscopy; crystallographic characterization was completed by X-ray diffraction of polycrystalline samples (XRPD). The title compound crystallized in a monoclinical system and unit-cell parameters are reported [a = 13.207(3) Å, b = 5.972(1) Å, c = 19.719(4) Å, β = 105.67(2)°, unit-cell volume V = 1497.5 (4) Å3, Z = 4]. All of the measured lines were indexed with the P21/n (No. 14) space group.