The crystal structure of tamsulosin hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Tamsulosin hydrochloride crystallizes in space group P21 (#4) with a = 7.62988(2), b = 9.27652(2), c = 31.84996(12) Å, β = 93.2221(2)°, V = 2250.734(7) Å3, and Z = 4. In the crystal structure, two arene rings are connected by a carbon chain oriented roughly parallel to the c-axis. The crystal structure is characterized by two slabs of tamsulosin hydrochloride molecules perpendicular to the c-axis. As expected, each of the hydrogens on the protonated nitrogen atoms makes a strong hydrogen bond to one of the chloride anions. The result is to link the cations and anions into columns along the b-axis. One hydrogen atom of each sulfonamide group also makes a hydrogen bond to a chloride anion. The other hydrogen atom of each sulfonamide group forms bifurcated hydrogen bonds to two ether oxygen atoms. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1415.

The crystal structure of pimecrolimus Form B has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Pimecrolimus crystallizes in the space group P21 (#4) with a = 15.28864(7), b = 13.31111(4), c = 10.95529(5) Å, β = 96.1542(3)°, V = 2216.649(9) Å3, and Z = 2. Although there are an intramolecular six-ring hydrogen bond and some larger chain and ring patterns, the crystal structure is dominated by van der Waals interactions. There is a significant difference between the conformation of the Rietveld-refined and the DFT-optimized structures in one portion of the macrocyclic ring. Although weak, intermolecular interactions are apparently important in determining the solid-state conformation. The powder pattern is included in the Powder Diffraction File™ (PDF®) as entry 00-066-1619. This study provides the atomic coordinates to be added to the PDF entry.

The crystal structure of (E)-doxepin hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. (E)-doxepin hydrochloride crystallizes in space group P21/a (#14) with a = 13.78488(7), b = 8.96141(7), c = 14.30886(9) Å, β = 96.5409(5)°, V = 1756.097(12) Å3, and Z = 4. There is a strong discrete hydrogen bond between the protonated nitrogen atom and the chloride anion. There are six C–H⋯Cl hydrogen bonds between the methyl groups and the chloride, as well as additional hydrogen bonds from methylene groups and the vinyl proton. The hydrogen bonds are important in determining the solid-state conformation of the cation. The compound is essentially isostructural to amitriptyline hydrochloride. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1613.

Commercial fluorometholone, CAS #426-13-1, crystallizes in the monoclinic space group P21 (#4) with a = 6.40648(2), b = 13.43260(5), c = 11.00060(8) Å, β = 92.8203(5)°, V = 945.517(5) Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded one previous structure determination, using single-crystal data at 292 K. In this work, the sample was ordered from the United States Pharmacopeial Convention (Lot # R032K0) and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using density functional theory (DFT) techniques. Hydrogen positions were included as a part of the structure and were re-calculated during the refinement. The diffraction data were collected on beamline 11-BM at the Advanced Photon Source, Argonne National Laboratory, and the powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™. The agreement of the Rietveld-refined and DFT-optimized structures is excellent; the root-mean-square Cartesian displacement is 0.060 Å. In addition to the O–H⋯O hydrogen bonds observed by Park et al. (Park, Y. J., Lee, M. Y., and Cho, S. I. (1992). “Fluorometholone,” J. Korean Chem. Soc. 36, 812–817), C–H⋯O hydrogen bonds contribute to the crystal energy.

Trimethoprim crystallizes in the triclinic space group P-1 (#2) with a = 10.5085(3), b = 10.5417(2), c = 8.05869(13) Å, α = 101.23371(21), β = 112.1787(3), γ = 112.6321(4)°, V = 743.729 Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded three previous structure determinations, using data collected at 100 K, 173 K, and room temperature. In this work, the sample was ordered from the United States Pharmacopeial Convention (USP) and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using density functional theory techniques. We found similar hydrogen bonding patterns with the previous determinations. In addition, we identified two C–H⋯O hydrogen bonds, which also contribute to the crystal energy. When comparing the previously reported trimethoprim structure determinations, the unit cell length lattice parameters were found to contract at lower temperatures, particularly 100 K. All structures show reasonable agreement, with unit cell length differences ranging between 0.05 and 0.15 Å. The diffraction data for this study were collected on beamline 11-BM at the Advanced Photon Source, and the powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

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.

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.

Flucytosine, CAS #2022-85-7, crystallizes in the tetragonal space group P41212 (#94) with a = 6.643768(27), c = 23.89009(10) Å, V = 1054.500(7) Å3, and Z = 8. In this work, the sample was obtained from the United States Pharmacopeial Convention (USP) Lot #R03100 and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using the density functional theory (DFT). When looking down the a-axis, the crystal structure consists of multiple ribbon-like structures stacked into columns. The powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®). The agreement of the Rietveld-refined and DFT-optimized structures is good, with the largest difference in the external amine group with an overall root mean displacement of 0.056 Å. There is also evidence of unit cell expansion at higher temperatures, as the volume of the unit cell at 298 K was 1.6–1.9% greater than the two unit cells obtained at 150 K. A N–H⋯O hydrogen bond exists in the inter-ribbon region between the flucytosine molecules, resulting in a 3D hydrogen bond network.

Herbicide-resistant Amaranthus spp. continue to cause management difficulties in soybean. New soybean technologies under development, including resistance to various combinations of glyphosate, glufosinate, dicamba, 2,4-D, isoxaflutole, and mesotrione, will make possible the use of additional herbicide sites of action in soybean than is currently available. When this research was conducted, these soybean traits were still regulated and testing herbicide programs with the appropriate soybean genetics in a single experiment was not feasible. Therefore, the effectiveness of various herbicide programs (PRE herbicides followed by POST herbicides) was evaluated in bare-ground experiments on glyphosate-resistant Palmer amaranth and glyphosate-resistant waterhemp (both tall and common) at locations in Arkansas, Illinois, Indiana, Missouri, Nebraska, and Tennessee. Twenty-five herbicide programs were evaluated; 5 of which were PRE herbicides only, 10 were PRE herbicides followed by POST herbicides 3 to 4 wks after (WA) the PRE application (EPOST), and 10 were PRE herbicides followed by POST herbicides 6 to 7 WA the PRE application (LPOST). Programs with EPOST herbicides provided 94% or greater control of Palmer amaranth and waterhemp at 3 to 4 WA the EPOST. Overall, programs with LPOST herbicides resulted in a period of weed emergence in which weeds would typically compete with a crop. Weeds were not completely controlled with the LPOST herbicides because weed sizes were larger (≥ 15 cm) compared with their sizes at the EPOST application (≤ 7 cm). Most programs with LPOST herbicides provided 80 to 95% control at 3 to 4 WA applied LPOST. Based on an orthogonal contrast, using a synthetic-auxin herbicide LPOST improves control of Palmer amaranth and waterhemp over programs not containing a synthetic-auxin LPOST. These results show herbicides that can be used in soybean and that contain auxinic- or HPPD-resistant traits will provide growers with an opportunity for better control of glyphosate-resistant Palmer amaranth and waterhemp over a wide range of geographies and environments.

In North America, terrestrial records of biodiversity and climate change that span Marine Oxygen Isotope Stage (MIS) 5 are rare. Where found, they provide insight into how the coupling of the ocean–atmosphere system is manifested in biotic and environmental records and how the biosphere responds to climate change. In 2010–2011, construction at Ziegler Reservoir near Snowmass Village, Colorado (USA) revealed a nearly continuous, lacustrine/wetland sedimentary sequence that preserved evidence of past plant communities between ~140 and 55 ka, including all of MIS 5. At an elevation of 2705 m, the Ziegler Reservoir fossil site also contained thousands of well-preserved bones of late Pleistocene megafauna, including mastodons, mammoths, ground sloths, horses, camels, deer, bison, black bear, coyotes, and bighorn sheep. In addition, the site contained more than 26,000 bones from at least 30 species of small animals including salamanders, otters, muskrats, minks, rabbits, beavers, frogs, lizards, snakes, fish, and birds. The combination of macro- and micro-vertebrates, invertebrates, terrestrial and aquatic plant macrofossils, a detailed pollen record, and a robust, directly dated stratigraphic framework shows that high-elevation ecosystems in the Rocky Mountains of Colorado are climatically sensitive and varied dramatically throughout MIS 5.

Palmer amaranth and waterhemp have become increasingly troublesome weeds throughout the United States. Both species are highly adaptable and emerge continuously throughout the summer months, presenting the need for a residual PRE application in soybean. To improve season-long control of Amaranthus spp., 19 PRE treatments were evaluated on glyphosate-resistant Palmer amaranth in 2013 and 2014 at locations in Arkansas, Indiana, Nebraska, Illinois, and Tennessee; and on glyphosate-resistant waterhemp at locations in Illinois, Missouri, and Nebraska. The two Amaranthus species were analyzed separately; data for each species were pooled across site-years, and site-year was included as a random variable in the analyses. The dissipation of weed control throughout the course of the experiments was compared among treatments with the use of regression analysis where percent weed control was described as a function of time (the number of weeks after treatment [WAT]). At the mean (i.e., average) WAT (4.3 and 3.2 WAT for Palmer amaranth and waterhemp, respectively) isoxaflutole + S-metolachlor + metribuzin had the highest predicted control of Palmer amaranth (98%) and waterhemp (99%). Isoxaflutole + S-metolachlor + metribuzin, S-metolachlor + mesotrione, and flumioxazin + pyroxasulfone had a predicted control ≥ 97% and similar model parameter estimates, indicating control declined at similar rates for these treatments. Dicamba and 2,4-D provided some, short-lived residual control of Amaranthus spp. When dicamba was added to metribuzin or S-metolachlor, control increased compared to dicamba alone. Flumioxazin + pyroxasulfone, a currently labeled PRE, performed similarly to treatments containing isoxaflutole or mesotrione. Additional sites of action will provide soybean growers more opportunities to control these weeds and reduce the potential for herbicide resistance.

Synthetic organic pigments (SOPS) find wide use in modern and contemporary works of art. These laboratory-made pigments are used in many fields, including industrial and architectural paints, printing inks, plastics, textiles, and artists’ materials. They have been examined by a variety of techniques including spectroscopic methods such as Fourier transform infrared spectroscopy (FTIR), Raman, and X-ray powder diffraction (XRD) as well as chromatographic or mass spectrometric techniques such as pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and laser desorption ionization mass spectrometry (LDI-MS). Often, a combination of techniques has been used to examine these pigments. Previously, we used a combination of Raman spectroscopy and LDI-MS to characterize commercially available SOPS. However, many pigments, termed “historical” are no longer manufactured, and therefore, may not have been characterized. This paper describes the synthesis of members of several classes of SOPS and their characterization.

The present study sought to explicate the time-course of posttraumatic stress (PTS)-related attentional bias to threat (ABT) by examining differences in attention bias variability (ABV; a measure which accounts for the temporal dynamics of ABT). A dot-probe task with four presentation durations was used to capture both subliminal and supraliminal stages of processing. Task stimuli consisted of neutral and threat images. Attentional control (AC) was examined as a moderator of the relationship between PTSD and ABV. At an experimental session, participants (PTSD = 11, trauma control = 18) completed questionnaires, a modified dot-probe task, and a stimulus-response task measuring AC. Individuals in the PTSD group exhibited greater ABV compared to trauma control participants. AC moderated this relationship, with participants with PTSD and poor AC exhibiting significantly greater ABV than trauma-exposed control participants with poor AC. These effects remained significant after accounting for traditionally calculated ABT scores and variability on trials for which only neutral stimuli were present, thus ensuring that the observed effects were specific to the presence of threat stimuli and not merely a function of general variability in response times. Findings implicate AC as a buffering mechanism against threat-related attentional dyscontrol among those with PTSD. Clinical implications will be discussed.