Powder diffraction

The crystal structure of valganciclovir hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Valganciclovir hydrochloride crystallizes in space group P2 1 2 1 2 1 (#19) with a = 7.07758(23), b = 11.34599(27), c = 49.3041(22) Å, V = 3,959.22(22) Å 3 , and Z = 8. Solution and refinement of the structure were made difficult by the limited data range, the relatively large size of the structure, the broad diffraction peaks, the relatively low crystallinity, and the significant preferred orientation. The two independent cations are protonated at the N atoms of the valine side chains. The crystal structure is dominated by alternating layers of ring systems and protonated side chains/anions along the c -axis. In addition to the ammonium–Cl hydrogen bonds, the ring systems and side chains are linked into a three-dimensional network by hydrogen bonds. The two independent cations have very different conformations. N–H···Cl, N–H···O, O–H···N, O–H···O, and O–H···Cl, as well as C–H···Cl, C–H···N, and C–H···O hydrogen bonds, are prominent in the structure. The powder pattern is included in the Powder Diffraction File ™ (PDF ® ) as entry 00-071-1641.

The crystal structure of trametinib dimethyl sulfoxide has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Trametinib dimethyl sulfoxide crystallizes in space group P-1 (#2) with a = 10.7533(4), b = 12.6056(5), c = 12.8147(6) Å, α = 61.2830(8), β = 69.9023(11), γ = 77.8038(10)°, V = 1,428.40(3) Å 3 , and Z = 2 at 298 K. The crystal structure contains hydrogen-bonded trametinib and dimethyl sulfoxide (DMSO) molecules. These are arranged into layers parallel to the (101) plane. There are two strong classical hydrogen bonds in the structure. One links the trametinib and DMSO molecules. Another is an intramolecular hydrogen bond. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File™.

The crystal structure of flumethasone has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Flumethasone crystallizes in space group P2 1 (#4) with a = 6.46741(5), b = 24.91607(20), c = 12.23875(11) Å, β = 90.9512(6)°, V = 1971.91(4) Å 3 , and Z = 4 at 298 K. The crystal structure consists of O–H⋯O hydrogen-bonded double layers of flumethasone molecules parallel to the ac -plane. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of delamanid has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Solution and refinement of the structure presented significant difficulties, and the result should be considered proposed or approximate. Delamanid crystallizes in the space group P2 1 2 1 2 1 (#19) with a = 67.3701(18), b = 12.86400(9), c = 5.65187(12) Å, V = 4,898.19(14) Å 3 , and Z = 8 at 295 K. There are two independent delamanid molecules, with different conformations, which are essentially identical in energy. The crystal structure consists of layers of delamanid molecules perpendicular to the a -axis. The imidazooxazole ring systems stack along the b -axis, and the trifluoromethyl groups make up the boundaries of the corrugated layers. There are no classical hydrogen bonds in the crystal structure. Eight C–H···O and one C–H···N hydrogen bonds contribute to the lattice energy. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of sparsentan has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Sparsentan crystallizes in space group P-1 (#2) with a = 11.4214(8), b = 12.0045(9), c = 14.1245(12) Å, α = 97.6230(22), β = 112.4353(16), γ = 110.2502(11)°, V = 1599.20(6) Å 3 , and Z = 2 at 298 K. The crystal structure consists of an isotropic packing of dimers of sparsentan molecules, linked by N–H···O=S hydrogen bonds. Several intra- and intermolecular C–H···O and C–H···N hydrogen bonds also link the molecules. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).

This work reports the X-ray powder diffraction (XRPD) data recorded at room temperature (293 K) of dibromidodioxido-[(4,4′-di-tert-butyl)-2,2′-bipyridine]molybdenum(VI). The analysis of the powder diffraction pattern led to an orthorhombic united cell with parameters a = 17.9205(23) Å, b = 13.4451(16) Å, c = 18.1514(19) Å, V = 4,373.5(11) Å 3 , and values of Z = 8 and Z’ = 2. The crystal structure of this material corresponds to the structure of entry IFUJEC of the Cambridge Structural Database (CSD), determined at 90 K. The excellent Rietveld refinement, carried out with General Structure and Analysis Software II (GSAS-II), showed the single-phase nature of the material and the good quality of the data. This material was also characterized by elemental analysis, UV–vis, Fourier transform infrared spectroscopy (FTIR), and proton nuclear magnetic resonance ( 1 H-NMR) techniques.

The crystal structure of fruquintinib Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Fruquintinib Form I crystallizes in space group C2 (#5) with a = 35.4167(22), b = 3.90500(12), c = 26.9370(11) Å, β = 108.0290(22)°, V = 3,542.52(26) Å 3 , and Z = 8 at 298 K. The crystal structure consists of double layers of each of the two independent molecules parallel to the ab -plane. These layers stack along the short b -axis. N–H···N hydrogen bonds link the layers. Most of the C–H···N and C–H···O hydrogen bonds are intramolecular. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of repotrectinib has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Repotrectinib crystallizes in the space group P2 1 2 1 2 1 (#19) with a = 9.27406(5), b = 11.60810(8), c = 15.63623(8) Å, V = 1,683.306(20) Å 3 , and Z = 4 at 298 K. The crystal structure consists of stacks of V-shaped molecules along the b -axis. One amino group acts as a donor to the carbonyl group to link the molecules into chains along the a -axis with a graph set C1,1(8). The second amino group forms two intramolecular hydrogen bonds. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of iprodione has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Iprodione crystallizes in the space group P2 1 /c (#14) with a = 15.6469(3), b = 22.8436(3), c = 8.67226(10) Å, β = 94.1303(7)°, V = 3,091.70(9) Å 3 , and Z = 8 at 298 K. The crystal structure contains clusters of four iprodione molecules. The only two classical N–H···O hydrogen bonds in the structure are both intramolecular. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of quizartinib hydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Quizartinib hydrate crystallizes in space group P-1 (#2) with a = 13.9133(9), b = 17.877(3), c = 19.8459(30) Å, α = 115.080(5), β = 93.768(5), γ = 100.831(5)°, V = 4,332.1(6) Å 3 , and Z = 6 at 298 K. In the complex crystal structure, the molecules are generally oriented parallel to the (110) plane. Two of the independent molecules are linked into dimers by N–H···O or N–H···N hydrogen bonds. Each molecule exhibits a unique pattern of C–H···O, C–H···N, or C–H···S hydrogen bonds. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File ™ (PDF ® ).

Data mining for materials science and structure prediction is growing rapidly. Such an approach relies a lot on the available published and unpublished crystal structure. In this contribution, we are using the experimental pattern reported in the PDF entry 00-058-0728 for the experimental data used to solve the previously unreported crystal structure of RbCdVO 4 . Contrary to the reported literature, the title compound crystallizes in the monoclinic system P2 1 with Z = 4. The lattice parameters are a = 12.53678(16) Å, b = 5.82451(7) Å, c = 12.47733(17) Å, β = 105.6169(10)°, and V = 877.47(2) Å 3 . Its crystal structure type is new and quite complex as it exhibits 28 atoms in the asymmetric unit.

The crystal structure of a new form of racemic reboxetine mesylate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Reboxetine mesylate crystallizes in space group P2 1 /c (#14) with a = 14.3054(8), b = 18.0341(4), c = 16.7924(11) Å, β = 113.4470(17)°, V = 3,974.47(19) Å 3 , and Z = 8 at 298 K. The crystal structure consists of double columns of anions and cations along the a -axis. Strong N–H···O hydrogen bonds link the cations and anions into zig-zag chains along the a -axis. The powder pattern has been submitted to the International Centre for Diffraction Data (ICDD ® ) for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of tafamidis has been independently resolved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Tafamidis crystallizes in space group P2 1 /c (#14) with a = 3.787093(6), b = 14.97910(4), c = 22.93751(7) Å, β = 90.92672(19)°, V = 1,301.012(4) Å 3 , and Z = 4 at 295 K. The crystal structure consists of stacks of molecules along the a -axis. The molecules are inclined to this axis; the mean plane is (−4, 2, 11). Strong centrosymmetric O–H⋅⋅⋅O hydrogen bonds exist between carboxylic acid groups. The molecules are linked along the b -axis by C–H⋅⋅⋅N hydrogen bonds. Two C–H⋅⋅⋅Cl hydrogen bonds also contribute to the lattice energy. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).

BaLa 2 Cu 1− x Ba x Ti 2 O 9 ( x = 0.00, 0.15, and 0.30) ceramics were synthesized in polycrystalline form via the conventional solid-state reaction techniques in air. The crystal structure of the title compositions was characterized by room-temperature X-ray powder diffraction and analyzed using the Rietveld refinement method. All the compositions crystallize in the tetragonal symmetry of space group I 4/ mcm (No. 140) with cell volumes: 249.43(1) Å 3 for x = 0.00, 249.42(1) Å 3 for x = 0.15, and 250.05(1) Å 3 for x = 0.30. The tilt system of the M O 6 octahedra ( M = Cu(Ba2)/Ti) corresponds to the notation a 0 a 0 c − . The M O 6 octahedra share the corners via oxygen atoms in 3 D. Along the c -axis, the octahedra are connected by O(1) atoms of (0, 0, 1/4) positions; while in the ab -plane, they are linked by O(2) atoms of ( x , x + 1/2, 0) positions. The bond angle of M –O2– M is 168.6(7)° for x = 0.00, 168.6(6)° for x = 0.15, and 166.8(6)° for x = 0.30, whereas the bond angle of M –O1– M is constrained to be 180° by space group I 4/ mcm.

The leucite group structures are tetrahedrally coordinated silicate framework structures with some of the silicate framework cations partially replaced by divalent or trivalent cations. These structures have general formulae A 2 B Si 5 O 12 and AC Si 2 O 6 , where A is a monovalent alkali metal cation, B is a divalent cation, and C is a trivalent cation. These leucites can have crystal structures in several different space groups, dependent on stoichiometry, synthesis conditions, and temperature. Phase transitions are known for temperature changes. This paper reports a high-temperature X-ray powder diffraction study on RbGaSi 2 O 6, which shows a phase transition from I 41/ a tetragonal to Ia d cubic on heating from room temperature to 733 K. On cooling to room temperature, the crystal structure reverts to I 4 1 /a tetragonal.

High-energy mixing offers a novel approach to enhancing the efficiency of Portland cements that incorporate supplementary cementitious materials regarding the hydration time and compressive strength formation. This research focused on monitoring the formation and degradation of mineral phases, as well as the compressive strength development and heat flow of mortars, within the first 48 hours, using clinker-efficient Portland composite cements. This study involved mixing Portland cement containing 20 wt% amorphous blast furnace slag and 10 wt% limestone with water using three different high-energy mixing techniques. The results demonstrated that the compressive strength of the Portland composite cements was comparable to that of ordinary Portland cement within a 48-hour period. Rietveld refinement was employed to track the formation of portlandite and the sum of the amorphous phases quartz and tobermorite, as well as the degradation of tricalcium silicate. The decline in tricalcium silicate and the formation of Portlandite showed a significant increase in reaction speed due to high-energy mixing. Additionally, a reduction in calcite content was observed, suggesting that calcium carbonate contributes to the enhanced compressive strength observed within the first 48 hours.

The crystal structure of valganciclovir hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Valganciclovir hydrochloride crystallizes in space group P2(1)2(1)2(1) (#19) with a = 7.07758(23), b = 11.34599(27), c = 49.3041(22) & Aring;, V = 3,959.22(22) & Aring;(3), and Z = 8. Solution and refinement of the structure were made difficult by the limited data range, the relatively large size of the structure, the broad diffraction peaks, the relatively low crystallinity, and the significant preferred orientation. The two independent cations are protonated at the N atoms of the valine side chains. The crystal structure is dominated by alternating layers of ring systems and protonated side chains/anions along the c-axis. In addition to the ammonium-Cl hydrogen bonds, the ring systems and side chains are linked into a three-dimensional network by hydrogen bonds. The two independent cations have very different conformations. N-HCl, N-HO, O-HN, O-HO, and O-HCl, as well as C-HCl, C-HN, and C-HO hydrogen bonds, are prominent in the structure. The powder pattern is included in the Powder Diffraction File (TM) (PDF (R)) as entry 00-071-1641.

The crystal structure of resmetirom heminonahydrate Form CSI has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Form CSI had been described previously as a dihydrate. Resmetirom heminonahydrate Form CSI crystallizes in space group P-1 (#2) with a = 11.3094(23), b = 15.158(6), c = 16.570(7) Å, α = 67.405(13), β = 74.425(7), γ = 69.526(7)°, V = 2,427.2(4) Å 3 , and Z = 4 at 298 K. The crystal structure consists of layers of resmetirom molecules parallel to the bc -plane. These layers are separated by water-rich layers also parallel to the bc -plane. A strong N–H···O links the two resmetirom molecules. The equivalent amino group in the other molecule acts as a donor to a water molecule. A number of C–H···O and C–H···N hydrogen bonds also contribute to the lattice energy. Water molecules act as donors to both O and N in the resmetirom molecules. The structure is more complicated than a hydrogen-bonded framework of resmetirom molecules with water in the pores. The powder pattern has been submitted to the International Centre for Diffraction Data (ICDD) for inclusion in the Powder Diffraction File ™ (PDF ® ).

The crystal structure of fluvoxamine hydrogen maleate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Fluvoxamine maleate crystallizes in space group P2 1 /c (#14) with a = 21.6310(15), b = 5.3180(4), c = 19.5555(15) Å, β = 99.979(5)°, V = 2,215.48(25) Å 3 , and Z = 4 at 298 K. The crystal structure consists of alternating double layers of cations and anions parallel to the bc -plane. Hydrogen bonds link the layers of anions and cations parallel to the bc -plane. The powder pattern has been submitted to the International Centre for Diffraction Data for inclusion in the Powder Diffraction File ™ (PDF ® ).