Crystal structure from X-ray powder diffraction data, DFT-D calculation, Hirshfeld surface analysis, and energy frameworks of (RS)-trichlormethiazide

The structure of racemic (RS)-trichlormethiazide [systematic name: (RS)-6-chloro-3-(dichloromethyl)-1,1-dioxo-3,4-dihydro-2H-1λ6,2,4-benzothiadiazine-7-sulfonamide], C8H8Cl3N3O4S2 (RS-TCMZ), a diuretic drug used in the treatment of oedema and hypertension, was determined from laboratory X-ray powder diffraction data using DASH [David et al. (2006). J. Appl. Cryst. 39, 910–915.], refined by the Rietveld method with TOPAS-Academic [Coelho (2018). J. Appl. Cryst. 51, 210–218], and optimized using DFT-D calculations. The extended structure consists of head-to-tail dimers connected by π–π interactions which, in turn, are connected by C—Cl...π interactions. They form chains propagating along [101], further connected by N—H...O hydrogen bonds to produce layers parallel to the ac plane that stack along the b-axis direction, connected by additional N—H...O hydrogen bonds. The Hirshfeld surface analysis indicates a major contribution of H...O and H...Cl interactions (32.2 and 21.7%, respectively). Energy framework calculations confirm the major contribution of electrostatic interactions (E elec) to the total energy (E tot). A comparison with the structure of S-TCMZ is also presented.

X-ray powder diffraction data for rivaroxaban, C19H18ClN3O5S

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.

Crystal structures and X-ray powder diffraction data for Cs2NiSi5O12, RbGaSi2O6, and CsGaSi2O6 synthetic leucite analogues

Leucites are tetrahedrally coordinated silicate framework structures with some of the silicon framework cations partially replaced by divalent or trivalent cations. These structures have general formulae A2BSi5O12 and ACSi2O6; where A is a monovalent alkali metal cation, B is a divalent cation, and C is a trivalent cation. In this paper, we report the Rietveld refinements of three more synthetic leucite analogues with stoichiometries of Cs2NiSi5O12, RbGaSi2O6, and CsGaSi2O6. Cs2NiSi5O12 is Ia $\bar{3}$ d cubic and is isostructural with Cs2CuSi5O12. RbGaSi2O6 is I41/a tetragonal and is isostructural with KGaSi2O6. CsGaSi2O6 is $I\bar{4}3d$ cubic and is isostructural with RbBSi2O6.

X-ray powder diffraction data for tetrazene nitrate monohydrate, C2H9N11O4

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.

Continuous series of symmetric peak profile functions determined by standard deviation and kurtosis

A mathematical system for modeling the effects of symmetrized instrumental aberrations has been developed. The system is composed of the truncated Gaussian, sheared Gaussian, and Rosin-Rammler-type functions. The shape of the function can uniquely be determined by the standard deviation and kurtosis. A practical method to evaluate the convolution with the Lorentzian function and results of application to the analysis of experimental powder diffraction data are briefly described.

The crystal chemistry and electrical properties of Fe doped Ca12Al14O33 (Mayenite)

X-ray and neutron powder diffraction have been used to study the crystal chemistry of Fe doped mayenite (Ca12Al14-xFexO33). Solid- state synthesis was used to prepare Ca12Al14-xFexO33 where x = 0, 0.1, 0.2, 0.5 and 0.6 and the citrate gel route was used to prepare Ca12Al14-xFexO33 where x = 0, 0.05, 0.1, 0.2, 0.3 and 0.4. X-ray powder diffraction data indicate that samples with the same composition but synthesized by the citrate gel route were more likely to be phase pure than samples obtained by traditional solid-state synthesis. The refined lattice parameters were observed to increase with increasing Fe concentration, irrespective of the synthesis method. Refined neutron powder data confirm that Fe is going into Al site rather than Ca site. A 2-point probe was used to measure the electrical properties of the Fe doped citrate gel synthesized samples and showed that the resistivity increases for the Fe doped samples compared to the undoped mayenite.

Crystal structure of brigatinib Form A (Alunbrig®), C29H39ClN7O2P

The crystal structure of brigatinib Form A has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Brigatinib Form A crystallizes in space group P-1 (#2) with a = 9.59616(20), b = 10.9351(3), c = 14.9913(6) Å, α = 76.1210(13), β = 79.9082(11), γ = 74.0802(6)°, V = 1458.497(15) Å3, and Z = 2. Structure solution was complicated by the lowest cost factor solution having an unreasonable conformation of the dimethylphosphoryl group. The second-best structure yielded a better refinement. The crystal structure is characterized by alternating layers of aliphatic and aromatic portions of the molecules along the b-axis. Strong N–H⋯N hydrogen bonds link the molecules into pairs, with a graph set R2,2(8). There is a strong intramolecular N–H⋯O hydrogen bond to the phosphoryl group, which determines the orientation of this group. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

Locating hydrogen positions in the autunite mineral metatorbernite [Cu(UO2)2(PO4)2·8H2O]: a combined approach using neutron powder diffraction and computational modelling

Metatorbernite [Cu(UO2)2(PO4)2·8H2O] is a promising remediation material for environmental uranium contamination. Previous X-ray diffraction studies have been unable to definitively locate hydrogen positions within metatorbernite, which are key to determining the hydrogen-bond network that helps to stabilize the structure. Here, hydrogen positions have been determined using a combination of neutron powder diffraction and the computational modelling technique ab initio random structure searching (AIRSS). Atomic coordinates determined through Rietveld analysis of neutron powder diffraction data are in excellent agreement with the minimum energy configuration predicted by AIRSS; thus, simulations confirm that our proposed model likely represents the global minimum configuration. Two groups of water molecules exist within the metatorbernite structure: free water and copper-coordinating water. Free water molecules are held within the structure by hydrogen bonding only, whilst the coordinating water molecules bond to copper in the equatorial positions to produce a 4 + 2 Jahn–Teller octahedra. The successful agreement between neutron powder diffraction data and AIRSS suggests that this combined approach has excellent potential for the study of other (trans)uranium materials in which hydrogen bonding plays a key role in phase stability.