Seven isotopic molybdates MIIUMo4O16 have been synthesized by solid state reaction with MII = Mg, Mn, Cd, Ca, Hg, Sr, Pb. Single crystals of CaUMo4O16 were obtained. Previously reported as triclinic, this compound is monoclinic, space group P2/n. Unit-cell parameters for the seven compounds are:

MgUMo4O16: a = 11.393(2), b = 6.505(1), c = 7.918(2) Å, β = 89.81(3)°, V = 586.8(5) Å3, Z = 2, Dx = 5.12 Mg m−3;

MnUMo4O16: a = 11.413(2), b = 6.555(1), c = 8.023(1) Å, β = 89.86(2)°, V = 600.2(4)Å3, Z = 2, Dx = 5.18 Mg m−3;

CdUMo4O16: a = 11.427(2), b = 6.607(1), c = 8.144(2) Å3, β = 90.40(2)°, V = 614.8(5)Å3, Z = 2, Dx = 5.37 Mg m−3;

CaUMo4O16: a = 11.443(3), b = 6.653(2), c = 8.239(2)Å, β = 90.51(3)°, V = 627.2(6)Å3, Z = 2, Dm = 4.83(5), Dx = 4.88 Mg m−3;

HgUMo4O16: a = 11.439(3), b = 6.643(1), c = 8.257(2)Å, β = 90.53(3)°, V = 627.4(6)Å3, Z = 2, Dx = 5.73 Mg m−3;

SrUMo4O16: 11.465(3), b = 6.768(2), c = 8.492(2) Å, β = 90.86(3)°, V = 658.8(6)Å3, Z = 2, Dx = 4.88 Mg m−3;

PbUMo4O16: a = 11.470(4), b = 6.813(2), c = 8.557(2)Å, β = 90.88(4)°, V = 668.7(8)Å3, Dx = 5.41 Mg m−3;

Powder diffraction data for each phase are reported.

X-ray powder diffraction data for 1-(4-Nitrophenyl)-2-piperidinone, C11H12N2O3, are reported [a = 9.514(3) Å, b = 12.308(6) Å, c = 9.175(1) Å, α = 90°, β = 91.811(2)°, γ = 90°, V = 1073.94 Å3, Z = 4, ρcal = 1.362 g cm−3 and space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

The “hook effect” observed in the Warren-Averbach analysis of X-ray diffraction peaks from multiple layer thin films of copper has been investigated theoretically and experimentally. The strengths of the “hook effect” for films of different layer thicknesses were analyzed. The results showed definite correlation between the strengths of the “hook effect” and the grain size distributions in 1, 4, and 19-layer copper films.

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°.

The crystal structure of ipratropium bromide monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Ipratropium bromide monohydrate crystallizes in the space group P21/c (#14) with a = 8.21420(7) Å, b = 10.54617(13) Å, c = 24.0761(39) Å, β = 99.9063(7) °, V = 2054.574(22) Å3, and Z = 4. Both hydrogen atoms of the water molecule act as donors to the bromide cation, forming a ring with the graph set R2,4(8). The hydroxyl group also acts as a donor to Br. Several C–H⋯Br hydrogen bonds are present. The water molecule acts as an acceptor in two C–H⋯O hydrogen bonds from methyl groups. The ketone acts as an acceptor in C–H⋯O hydrogen bonds from methyl groups, a methylene group, and a methyne group. The hydroxyl group acts as an acceptor in a C–H⋯O hydrogen bond from a phenyl carbon atom. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1611.

The crystal structure of pantoprazole sodium sesquihydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Pantoprazole sodium sesquihydrate crystallizes in space group Pbca (#61) with a = 33.4862(6), b = 17.29311(10), c = 13.55953(10) Å, V = 7852.06(14) Å3, and Z = 16. The crystal structure is characterized by layers parallel to the bc-plane. One layer contains the Na coordination spheres. The two independent sodium ions are trigonal bipyramidal and octahedral. The NaO3N2 and NaO4N2 coordination spheres share an edge to form pairs. The sodium bond valence sums are 1.17 and 1.15. The difluoromethyl groups are probably disordered. Two water molecules act as hydrogen bond donors to pyridine nitrogen atoms and sulfoxide oxygen atoms. The third water molecule participates in bifurcated hydrogen bonds, but one of its hydrogen atoms does not participate in hydrogen bonds. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1424.

X-ray powder diffraction data, unit-cell parameters and space group for methoxmetamine (C14H20ClNO2) are reported [a = 6.5768(7) Å, b = 14.0830(10) Å, c = 15.0530(10) Å, β = 90.975(2)°, unit-cell volume V = 1394.0(2) Å3, and Z = 4, and space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

The crystallite size distribution is an important parameter affecting the processing and properties of materials or products containing crystallites. The X-ray diffraction pattern collected with a two-dimensional detector may contain one or several spotty diffraction rings when an appropriate X-ray beam size is used. The spottiness of the diffraction ring is related to the size, size distribution, and orientation distribution of the crystallites. The intensity of a diffraction spot may represent its volume or size of a crystallite when a perfect Bragg condition is met. This paper introduces the algorithms and procedure to evaluate crystallite size distribution from a 2D diffraction pattern by rocking scan.