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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

October 2021 issue

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Cover illustration: Conformational flexibility within molecules of the serine protease inhibitor nafamostat influences its therapeutic characteristics. In the dimesylate salt of nafamostat, the divalent cation is twisted to give screw-like motifs, which pack via extensive hydrogen bonding into columnar structures. See: Fujii [Acta Cryst. (2021). E77, 999–1002].

Jerry P. Jasinski tribute


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The reported mol­ecule contains a number of unusual features, the most notable being a finite yet exceptionally long cyclic metal-azido chain. These rare features are the consequence of both sterically protecting Cp* ligands and highly bridging oxide and hydroxide ligands in the same system and illustrate the inter­esting new possibilities that can arise from combining organometallic and solvothermal f-block element chemistry.

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(E)-1-(4-Meth­oxy­phen­yl)-3-[4-(prop-2-yn­yloxy)phen­yl]prop-2-en-1-one undergoes a cyclo­condensation reaction with thio­semicarbazide to form the corresponding 4,5-di­hydro­pyrazole-1-arbo­thio­amide, which in turn undergoes further cyclo­addition with phenacyl bromides to form 4,5-di­hydro-1-(thia­zol-2-yl)pyrazoles. The mol­ecules adopt an overall T-shape structure. Different combinations of hydrogen bonds link the mol­ecules into ribbons or sheets.

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The crystal structures of two manganese(II) complexes have been determined. The manganese(II) centers of each structure are six-coordinate with a distorted octa­hedral geometry. Although the bis­(quinolin-2-ylmeth­yl)ethanamine ligands differ only by a methyl group, the structure of one complex is dimeric with bridging acetate ligands and exhibits a trans coordination and coplanarity of the quinolyl moieties, while the second complex is monomeric with a cis coordination of the quinolyl groups.

research communications


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6-Nitro­quinazolin-4(3H)-one (C8H5N3O3), 6-amino­quinazolin-4(3H)-one (C8H7N3O) and 4-amino­quinazoline hemi­hydro­chloride dihydrate (C16H19N6O2) were synthesized and their structures were determined by single-crystal X-ray analysis.

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C—H⋯N inter­actions, C—Cl⋯π inter­actions, and π-π stacking inter­actions link mol­ecules in the crystal, forming mol­ecular layers approximately parallel to the (002) plane. The three-dimensional packing is strengthened by additional weak van der Waals inter­actions between the layers.

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The crystal structure of nafamostat mesylate is reported, which is a serine protease inhibitor, and has been applied clinically as an anti­coagulant and anti-inflammatory agent.

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The title compounds Fe4(C7H4O3)O(C2H3O2)6(C5H5N)3X where X is either Cl or F were synthesized using a self-assembly reaction in methanol and pyridine with stoicometric addition of salicyl­hydroxamic acid (H3shi), acetic acid (HOAc), and the appropriate ferric halide salt. The compound is remeniscent of hydroximate binding in metallacrown structures.

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In the racemic title compound, the [Co(en)3]3+ and [Na(H2O)6]+cations exist in distorted octa­hedral coordination environments and charge neutrality in the salt is furnished by Cl anions. Structural cohesion is maintained by an array of C—HO, N—HCl and O—HCl hydrogen bonds.

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The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetra­kis­(1,3-di­methyl­imidazolium-2-yl­idene)palladium(II) hexa­deca­carbonyl­tetra­rhenium diethyl ether disolvate, [Pd(C5H8N2)4][Re4(CO)16]·2C4H10O or [Pd(IMe)4][Re4(CO)16]·2C4H10O, (1), and di­carbonyl­octa-μ-carbonyl-tetra­kis­(tri­phenyl­phosphane)palladiumdirhenium, [Pd4Re2(C18H15P)4(CO)10] or Pd4Re2(PPh3)4(μ-CO)8(CO)2, (2), from the reaction of Pd(PPh3)4 with 1,3-di­methyl­imidazolium-2-carboxyl­ate and Re2(CO)10 in a toluene–aceto­nitrile mixture.

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The polymer contains Li+ cations coordinated via oxygen to two cyanuranate anions and three water mol­ecules in a trigonal–bipyramidal geometry and to three water mol­ecules and an oxygen from the cyanuric anion in a tetra­hedral geometry. A three-dimensional network of hydrogen bonds serves to hold the structure together.

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A tris­ilver complex stabilized by two monoanionic bis­phosphinimine ligands is reported. Noteworthy asymmetry at the cluster core is observed. This is the first example of a tris­ilver complex supported by monoanionic bis­phosphinimine ligands.

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The fluorene skeleton of the title mol­ecule is nearly planar and the crystal structure is composed of mol­ecular layers extending parallel to the 302 plane. A Hirshfeld surface analysis indicated that the most important contributions to the overall surface are from H⋯H, O⋯H and C⋯H inter­actions.

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Octa­hedral [Fe(DMF)6]3+ and tetra­hedral-based [Cd2Cl7]3− ions stack alternately along the c-axis direction in this rare example of a [Fe(DMF)6]3+-containing ionic salt.

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The phenyl-quinoxaline moiety in the title compound is not planar. In the crystal, C—H⋯O hydrogen bonds between neighboring quinoxaline rings form chains along the a axis direction.

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The title compound was obtained via a two-step synthesis (Dimroth reaction and amidation) for anti­cancer activity screening and was selected from a 1H-1,2,3-triazole-4-carboxamide library. The cyclo­propyl ring is oriented almost perpendicular to the benzene ring [dihedral angle = 87.9 (1)°], while the dihedral angle between the mean plane of the cyclo­propyl ring and that of the triazole ring is 55.6 (1)°. In the crystal, the mol­ecules are linked by O—H⋯O and C—H⋯N inter­actions into infinite ribbons propagating in the [001] direction, which are inter­connected by weak C—H⋯O inter­actions into layers.

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In the crystal, mol­ecules are linked by C—H⋯O hydrogen bonds, forming layers parallel to the (001) plane. These layers of mol­ecules are connected by C—H⋯π inter­actions along the c-axis direction. Inter­layer van der Waals and inter­halogen inter­actions stabilize the packing.

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In this O-alkyl­ated sulfonyl­pyrazolone, the sulfur atom lies 0.558 (1) Å out of the pyrazole ring plane. The NH2 group is involved in an intra­molecular hydrogen bond to a sulfonyl oxygen atom and in a three-centre system with the two oxygen atoms of the side chain at C3, forming a ribbon structure.

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A supra­molecular two-dimensional polymer structure of caesium tetra­methyl­dithio­imidodiphosphinate is reported.

Research communications

Research communications are designed to help authors bring out the science behind their structure determinations. Authors are encouraged to report more than one structure in the same communication and also to include the results of investigations with other techniques. The Research communications format makes Acta E the natural home for structure determinations with interesting science to report.

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