A new compound NH4Co2OH(MoO4)2⋅H2O was prepared by precipitation of aqueous solutions of cobalt nitrate and ammonium heptamolybdate at pH = 7.5. The crystal structure was identified by X-ray powder diffraction (XRPD) and Rietveld refinement as a known polymorph of layered molybdates (Φy) with general formula AT2OH(MoO4)2⋅H2O (A = NH4+, Na+, K+ and T = Zn2+, Co2+, Cu2+, Ni2+) and refined from a model based on that structure. The lattice parameters were refined with R-3 space group (148) a = 6.1014(2) Å, b = 6.1014(2) Å, c = 21.826(1) Å, α = 90°, β = 90°, and γ = 120°.

X-ray powder diffraction data, including unit cell parameters and space group assignment, for the ESP15228 species of C19H34O5 formula, are here reported [a = 6.0434(6), b = 12.2543(6), c = 14.0285(8) Å, α = 86.584(3), β = 85.707(10), γ = 78.801(5)°, V = 1015.2(1) Å3, Z = 2, ρcalc = 1.152 g cm−3, and space group P-1]. All measured lines were indexed and no detectable impurities were observed.

The dichloro-dioxide-(4,4′-dimethyl-2,2′-bipyridyl)-molybdenum (VI) complex was prepared from molybdenum(VI)-dichloride-dioxide and 4,4′-dimethyl-2,2′-bipyridyl in CH2Cl2 obtaining a clear green solution. The molybdenum complex was precipitated using ethyl ether, separated by filtration and the light green solid washed with ethyl ether. The XRPD pattern for the new compound showed that the crystalline compound belongs to the monoclinic space group P21/n (No.14) with refined unit-cell parameters a = 12.0225(8) Å, b = 10.3812(9) Å, c = 11.7823(9) Å, β = 103.180(9)°, unit-cell volume V = 1431.79 Å3, and Z = 4.

A new ternary compound Al0.931Ni1.069Sc5 has been synthesized and studied by means of the X-ray powder diffraction technique. Al0.931Ni1.069Sc5 crystallizes in the hexagonal crystal system with the Al5Co2 structure type, space group P63/mmc, with a = 8.8287(3) Å, c = 8.6959(4) Å, Z = 4 and V = 587.00 Å3, ρcalc = 3.538 g/cm3.

X-ray powder diffraction data for the two new polymorphs of 1-methylhydantoin, C4H6N2O2, are reported. The polymorph II (MH-II) crystallizes in the orthorhombic system with space group Pna21 [a = 19.0323(7) Å, b = 3.91269(8) Å, c = 6.8311(7) Å, Z′ = 1, Z = 4, unit cell volume V = 508.70(3) Å3. Polymorph III (MH-III) crystallizes in the orthorhombic system with space group P212121 [a = a = 7.82427(5), b = 9.8230(5), c = 20.2951(4), Z′ = 3, Z = 12, unit cell volume V = 1563.5(1) Å3]. All measured lines, in each case, were indexed and are consistent with the space group.

Nicotine 2,6-dihydroxybenzoate is a nicotine salt that can be used as the nicotine source in tobacco products. X-ray powder diffraction data, unit-cell parameters, and space group for nicotine 2,6-dihydroxybenzoate, C10H15N2⋅C7H5O4, are reported [a = 7.726(8) Å, b = 11.724(3) Å, c = 9.437(1) Å, α = 90°, β = 109.081(3)°, γ = 90°, unit-cell volume V = 802.902 Å3, Z = 2, ρcal = 1.309 g cm−3, and space group P21] at room temperature. All measured lines were indexed and were consistent with the P21 space group.

Quantitative phase analysis is one of the major applications of X-ray powder diffraction. The essential principle of quantitative phase analysis is that the diffraction intensity of a component phase in a mixture is proportional to its abundance. Nevertheless, the diffraction intensities of the component phases cannot be compared with each other directly since the coherent scattering power per unit cell (or chemical formula) of each component phase is usually different. The coherent scattering power per unit cell of a crystal is well represented by the sum of the squared structure factors, which cannot be calculated directly when the crystal structure data is unavailable. Presented here is a way to approximate the coherent scattering power per unit cell based solely on the unit cell parameters and the chemical contents. This approximation is useful when the atomic coordinates for one or more of the phases in a sample are unavailable. An assessment of the accuracy of the approximation is presented. This assessment indicates that the approximation will likely be within 10% when X-ray powder diffraction data is collected over a sufficient portion of the measurable pattern.

X-ray powder diffraction data, unit-cell parameters, and space group for rivaroxaban, C19H18ClN3O5S, are reported [a = 9.010(3) Å, b = 10.986(6) Å, c = 11.230(1) Å, α = 63.439(5)°, β = 74.355(4)°, γ = 78.133(3)°, unit-cell volume V = 952.87 Å3, Z = 2, ρcal = 1.519 g cm−3, and space group P1]. All measured lines were indexed and are consistent with the P1 space group. No detectable impurities were observed.

X-ray powder diffraction data, unit-cell parameters, and space group for tetrazene nitrate monohydrate, C2H9N11O4, are reported [a = 5.205(1) Å, b = 13.932(3) Å, c = 14.196(4) Å, β = 97.826(3)°, unit-cell volume V = 1019.8(4) Å3, Z = 4, and space group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurities were observed.

The direct derivation (DD) method is a technique for quantitative phase analysis (QPA). It can be characterized by the use of the total sums of scattered/diffracted intensities from individual components as the observed data. The crystal structure parameters are required when we calculate the intensities of reflections or diffraction patterns. Intensity can, however, be calculated only with the chemical composition data if it is not of individual reflections but of a total sum of diffracted/scattered intensities for that material. Furthermore, it can be given in a form of the scattered intensity per unit weight. Therefore, we can calculate the weight proportion of a component material by dividing the total sum of observed scattered/diffracted intensities by the scattered intensity per unit weight. The chemical composition data of samples under investigation are known in almost all cases at the stage of QPA. Thus, a technical problem is how to separate the observed diffraction pattern of a mixture into individual component patterns. Various pattern decomposition techniques currently available can be used for separating the pattern of a mixture. In this report, the theoretical background of the DD method and various techniques for pattern decompositions are reviewed along with the examples of applications.

The structure of the anticancer drug carmustine (1,3-bis(2-chloroethyl)-1-nitrosourea, C5H9Cl2N3O2) was successfully determined from laboratory X-ray powder diffraction data recorded at 278 K and at 153 K. Carmustine crystallizes in the orthorhombic space group P212121 with Z = 4. The lattice parameters are a = 19.6935(2) Å, b = 9.8338(14) Å, c = 4.63542(6) Å, V = 897.71(2) ų at 153 K, and a = 19.8522(2) Å, b = 9.8843(15) Å, c = 4.69793(6) Å, V = 921.85(2) ų at 278 K. The Rietveld fits are very good, with low R-values and smooth difference curves of calculated and experimental powder data. The molecules form a one-dimensional hydrogen bond pattern. At room temperature, the investigated commercial sample of carmustine was amorphous.

X-ray powder diffraction data, unit-cell parameters, and space group for N,N-dimethyl-1H-benzo[d]imidazol-2-amine, C9H11N3, are reported [a = 11.379(3) Å, b = 10.227(5) Å, c = 7.151(1) Å, α = 90°, β = 90°, γ = 90°, unit-cell volume V = 832.318 Å3, Z = 4, ρcal = 1.286 g cm−3, and space group P21212]. All measured lines were indexed and were consistent with the P21212 space group. No detectable impurities were observed.

Nicotine 3,5-dihydroxybenzoate dihydrate is a nicotine salt and can be used as compositions in tobacco products. X-ray powder diffraction data, unit-cell parameters, and space group for nicotine 3,5-dihydroxybenzoate, C10H15N2⋅C7H5O4⋅2H2O, are reported [a = 8.424(1) Å, b = 13.179(8) Å, c = 8.591(1) Å, α = 90°, β = 102.073(8)°, γ = 90°, unit-cell volume V = 932.765(3) Å3, Z = 2, ρcal = 1.256 g⋅cm−3, and space group P21] at room temperature. All measured lines were indexed and are consistent with the P21 space group.

X-ray powder diffraction data, unit-cell parameters, and space group for norethisterone enanthate, C27H38O3, are reported [a = 6.191(4) Å, b = 12.711(3) Å, c = 31.396(2) Å, α = 90°, β = 90°, γ = 90°, unit-cell volume V = 2471.16 Å3, Z = 4, ρcal = 1.104 g cm−3, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed.

Single-crystal and powder X-ray diffraction data, collected at room temperature, unit-cell parameters and space group for eluxadoline nitrate monohydrate, C32H35N5O5⋅2HNO3⋅H2O, are reported [a = 11.066(5) Å, b = 13.452(6) Å, c = 24.373(9) Å, unit-cell volume V = 3628.15 Å3, Z = 4, ρcal = 1.344 g⋅cm−3, and space group P212121]. All the diffraction peaks in the experimental pattern have been indexed and are consistent with the P212121 space group.

X-ray powder diffraction data for estra-4,9-diene-3,17-dione, C18H22O2, are reported [a = 9.236(7) Å, b = 10.294(4) Å, c = 15.471(1) Å, unit cell volume V = 1471.11 Å3, Z = 4, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed. The single-crystallographic data of the compound are also reported [a = 9.2392(7) Å, b = 10.2793(5) Å, c = 15.4822(7) Å, unit cell volume V = 1470.37(15) Å3, Z = 4, and space group P212121]. Both single-crystal and powder diffraction methods can get the similar structure data.

X-ray powder diffraction data for new metal-organic compounds: tetrakis(3-ethylanilinium) octamolybdate Mo8O26(C8H12N)4 [a = 10.682(4), b = 16.589(5), c = 7.307(2) Å, α = 92.79(2)°, β = 97.99(3)°, γ = 103.89(3)°, V = 1240.27 Å3, Z = 1, space group P−1]; tetrakis(3-ethylanilinium) octamolybdate tetrahydrate Mo8O26(C8H12N)4·(H2O)4 [a = 18.801(7), b = 17.943(6), c = 7.334(3) Å, β = 98.50(5)°, V = 2446.99 Å3, Z = 2, space group P21/m] and bis(3-ethylanilinium) pentamolybdate Mo5O16(C8H12N)2 [a = 34.643(6), b = 5.5796(7), c = 14.200(3) Å, β = 96.20(2)°, V = 2728.69 Å3, Z = 4, space group I2/a] are reported in this paper. The investigated compounds were synthesized from molybdic acid and 3-ethylaniline in acidic solution. In the first two cases, we obtained octamolybdates, while the last compound crystallized as pentamolybdate.

The crystal and molecular structure of fenspiride, a bronchodilator and anti-inflammatory drug, are reported. Fenspiride crystallizes in the monoclinic system, with two crystallographically independent molecules in the general position of the space group P21/n (No. 14) and Z = 8. Rietveld refined unit cell parameters are a = 11.52013(8) Å, b = 5.614091(31) Å, c = 44.1567(4) Å, α = 90°, β = 93.0885(6)°, γ = 90°, and V = 2851.69(4) Å3.

Laboratory X-ray powder diffraction was used to solve and refine the crystal structures of appended guest molecules within the pores of metal–organic frameworks (MOFs). Herein, we report the crystal structure of 1-propanethiol adsorbed in the pores of Co2(dobdc) (dobdc4– = 2,5-dioxido-1,4-benzenedicarboxylate, MOF-74). Soaking the activated MOF in neat 1-propanethiol resulted in the formation of 1-propanethiol–Co2(dobdc). The thiol appendant MOF maintained the crystal symmetry, with a rhombohedral space group R-3 and unit-cell parameters a = 25.9597(9) Å, c = 6.8623(5) Å, and V = 4005.0(4) Å3. As expected, the thiol sulfur formed a bond with the open cobalt metal site. The alkane chain was directed toward the center of the pore, participating in numerous van der Waals weak interactions with neighboring molecules. For the final Rietveld refinement, soft restrains were applied using bond distances obtained by periodic density functional theory (DFT) geometry optimization.

Ba3−xSrxTb3−xCexO9 (x = 1 and 1.5) ceramics (BSTC) with a relative density of 93% and a grain size distribution of 0.2–3 µm were prepared by the mixed-oxides reaction route. The crystalline structures, microstructures, valence states, and electrical properties of two ceramics were analyzed using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR), and electrical measurements. Rietveld analyses of XRPD patterns show that BSTC1 is indexed as a trigonal structure with the space group R-3c, and BSTC3/2 is indexed as an orthorhombic perovskite structure with the space group Pmcn. The EPR, XPS, and electrical conductivity results confirm that Ce and Tb ions in BSTC exist as Ce4+ and mixed-valence states of Tb4+/Tb3+, respectively. At room temperature, the two BSTC ceramics exhibit a similar semiconducting behavior. The relationships between electrical conductivity and temperature/frequency are provided. The defect chemistry is discussed.