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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

October 2017 issue

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Cover illustration: Carboranylamidinate ligands are a special class of amidinates ions of the general formula [RC(NR')2]- in which the R and R' substituents can be the chemically versatile carboranyl moiety ortho-C2H11B10. The presence of this bulky subsitutent influences the coordination mode of the ligand in metal-amidinate complexes, adopting a specific [kappa]C,[kappa]N-chelating mode instead of the more common [kappa]N,[kappa]N'-chelating behaviour. Reaction of lithium carboranylamidinates Li[o-(C2H10B10)C(NCy)(NHCy)] and Li[o-(C2H10B10)C(NiPr)(NHiPr)] with SnCl2 and SnCl4, respectively, afforded the two new compounds SnII[o-(C2H10B10)C(NCy)(NHCy)]2 (1) and SnIVCl[o-(C2H10B10)C(NiPr)(NHiPr)][o-(C2H10B10)C(NiPr)2] (2), the latter isolated as a by-product. Compound 2, illustrated here, is the first carboranylamidinate complex containing both mono- and dianionic carboranylamidinate ligands in a single molecule. See: Harmgarth, Liebing, Hillebrand, Busse & Edelmann [Acta Cryst. (2017). E73, 1443-1448].

research communications


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The characteristic structural feature of a new two-dimensional Zn coordination polymer is an infinite polymeric layer parallel to the crystallographic (132) plane.

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Accurate structural parameters (bond lengths and angles) of dimethyl sulfoxide, DMSO, have been obtained from the redetermination of its crystal structure by single-crystal X-ray diffraction at 100 K using CCD data in order to get a reference point for the deformation of the chemically bonded mol­ecule. In addition, the new data show that mol­ecule approximates Cs symmetry in the solid state where all atoms occupy general positions.

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The syntheses and crystal structures of the title dioxane hemisolvates of N-(7-bromo­methyl-1,8-naphthyridin-2-yl)acetamide and bis­[N-(7-di­bromo­methyl-1,8-naphthyridin-2-yl)acetamide] are described.

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The title compound, 7β-hy­droxy­royleanone, an abietane-type diterpene, was isolated from Taxodium ascendens (B.).

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The crystal structure of the enanti­opure sulfoxide of a 2,3,5,6-tetra­hydro-1,3-thia­zin-4-one exhibits a twisted half-chair pucker for the thia­zine ring. Inter­molecular N—H ⋯O hydrogen-bonding inter­actions form a two-dimensional layered structure lying parallel to (001).

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Tranexamic acid is an anti­fibrinolytic amino acid that exists as a zwitterion [trans-4-(ammonio­meth­yl)cyclo­hexane-1-carboxyl­ate] in the solid state. Its reaction with copper chloride lead to the formation of a copper(II) paddle-wheel structure.

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The new polymorph of lithium tetra­chlorido­aluminate, LiAlCl4, adopts a defect wurtz-stannite-type of structure and is metastable.

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The title compounds are monomeric models for a polythio­noester and a poly(ester-co-thio­noester). The mol­ecules adopt all-trans structures with inter­molecular C⋯S close contacts and C—H⋯π inter­actions. Both crystals have almost the same mol­ecular packing in space group P21/c.

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The synthesis and structures of three manganese(II) pyridine N-oxide complexes are presented.

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The title compound, C18H22FN5O8S, is used as a herbicide. The crystal structure is stabilized by N/C—H⋯O hydrogen bond, C—H⋯F and C—H⋯π inter­actions with weak π–π inter­actions contacts to form a three-dimensional architecture.

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Tin forms mononuclear chelate complexes with κC,κN-coordinated carboranylamidinate ligands, in which the Sn atom exhibits a trigonal–bipyramidal (SnIV) or pseudo-trigonal–bipyramidal (SnII) coordination.

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The title Schiff base was synthesized via the condensation reaction of 3,5-di-tert-butyl-4-hy­droxy­benzaldehyde and 2-hydrazinyl­pyridine and crystallized with a single mol­ecule in the asymmetric unit. The conformation about the C=N bond is E. In the crystal, N—H⋯N hydrogen bonds connect pairs of mol­ecules into dimers. In addition, weak C—H⋯O hydrogen bonds and C—H⋯π inter­actions are observed.

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A new organic perchlorate (C9H22N2)[ClO4]2 was synthesized by slow evaporation at room temperature and its crystal structure was determined. This compound was characterized by TGA–DSC and Hirshfeld surface analysis.

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The mononuclear title compound features a Zn2+ ion coordinated by two symmetrically binding di­thio­carbamate ligands and one end of a 4-pyridine­aldazine mol­ecule with the resulting NS4 donor set tending towards a square-pyramidal geometry.

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A linear SP coordination geometry for the gold atom is found in the title structure, which also features a short intra­molecular Au⋯O inter­action, in contrast to a Au⋯π inter­action found in the first polymorph.

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The mol­ecular and crystal structure of the insecticide fipronil is reported. In the crystal, N—H⋯N, N—H⋯O, C—H⋯F hydrogen bonds, C—N⋯π and C—Cl⋯π inter­actions link adjacent mol­ecules, forming a three-dimensional network. In addition, there are short F⋯F inter­actions present.

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The crystal structure of the triterpene lactone ochraceolide A (3-oxolup-20 (29)-en-30,21α-olide) isolated from Elaeodendron trichotomum (Turcz.) Lundell is reported.

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The title complex contains a central octa­hedrally coordinated MnIII cation with to two bidentate Schiff base ligands occupying the equatorial positions and two dimethyl sulfoxide ligands occupying the axial positions. In addition, disordered perchlorate anions and solvent mol­ecules with a site-occupancy factor corresponding to that of the major fraction of the anions.

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The 1:1, 2-methyl­pyridium and 4-methyl­pyridinium salts of the chiral 4-methyl­benzo­yloxy-substituted succinic acid form, respectively one- and two-dimensional hydrogen-bonded crystal structures,

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The mol­ecule of the neutral title compound and the cation in the title salt both exhibit a similar kind of disorder, even though their overall conformations are different. There are no direction-specific inter­actions between the mol­ecules of the neutral compound, but the ions in the salt are linked into hydrogen-bonded sheets.

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De­oxy­uridine substituted by dibenzo­furanyl at the carbon atom in base position C5 was synthesized and structurally characterized. The coupling was achieved by a Suzuki–Miyaura reaction utilizing the PTABS ligand and palladium(II) acetate.

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Unusual formation of (E)-11-(amino­methyl­ene)-8,9,10,11-tetra­hydro-pyrido[2′,3′:4,5]pyrimido[1,2-a]azepin-5(7H)-one was found at formyl­ation of 8,9,10,11-tetra­hydro­pyrido[2′,3′:4,5]pyrimido[1,2-a]-azepin-5(7H)-one, which was explained by re-amination of firstly formed inter­mediate.

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The ZnII atom is each of the title compounds is coordinated by two di­thio­carbamate ligands and a pyridyl-N atom. The resultant NS4 donor set approximates a square-pyramid and trigonal-bipyramid, for the solvated and unsolvated structures, respectively. In the solvate, amide-N—H⋯O(di­methyl­formamide) hydrogen-bonds define a three-mol­ecule aggregate while in the unsolvated structure, amide⋯amide hydrogen-bonding leads to a supra­molecular chain.

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The title structure, 4-amino­benzoic acid 4-methyl­pyridine/4-methyl­pyridinium 4-amino­benzoate 0.58/0.42, has been redetermined from the data published by Kumar et al. (2015). Acta Cryst. E71, o125-o126. The motivation for this redetermination follows from negligence of important features of the difference electron-density maps as well as from wrongly applied constraints, which significantly affect the structural model. The corrections affect mainly the positions of the H atoms involved in the hydrogen bonds (centered on the primary amine group for which the H atom turned out to be disordered over two positions about the centre of an N⋯H⋯O hydrogen bond) and the methyl group, which is disordered and has now been remodelled.

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In the cation of the title mol­ecular salt, one of the non-H substituents on the piperidine ring occupies an equatorial site and the other an axial site. The ions are linked into sheets by a combination of one N—H⋯O and two C—H⋯O hydrogen bonds.

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The crystal structure of the centrosymmetric title compound features short N—H⋯π inter­actions.

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The crystal structure of Na(H2AsO4) is isotypic with that of Na(H2PO4). The two structures are compared with the aid of the COMPSTRU program.

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The mol­ecular and crystal structures of a monoclinic polymorph of 1,2-bis­[(1-methyl-1H-tetra­zol-5-yl)sulfan­yl]ethane (BMTTE) are described.

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The title compound crystallizes as a methanol disolvate and exhibits short hydrogen bonds and a disordered perfluoro­alkyl chain.

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In the title benzoyl­thio­urea derivative (MPiCB), the piperidine ring has a chair conformation and its mean plane is inclined to the 4-meth­oxy­benzene ring by 63.0 (3)°.

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The copper(II) complex of the non-symmetric, bidentate ligand 2-{[6-(di­methyl­amino)­pyrimidin-4-yl]sulfan­yl}pyrimidine-4,6-di­amine exhibits distorted square pyramidal geometry around the metal centre, with disorder in the axial position, occupied by chloride or water. The six-membered metal–chelate ring is in a boat-conformation, and short inter­molecular S⋯S inter­actions are observed.

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The mol­ecular structure of {[1′-(di­phenyl­phosphino)ferrocen­yl]meth­yl}di­methyl­ammonium chloride monohydrate is presented. Individual ions and the solvating water mol­ecule assemble into dimeric units located around crystallographic inversion centers via N—H⋯Cl and O—H⋯Cl hydrogen bonds.

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The AgI atom in the title compound is two-coordinate, being bound to two pyridine N atoms from two N-(pyridin-3-ylmeth­yl)pyridin-3-amine ligands in a slightly distorted linear fashion. Each AgI ion bridges the dipyridyl-type ligands to form polymeric zigzag chains. The chains are connected via Ag⋯Ag and π–π inter­actions, forming a corrugated layer parallel to (\overline{1}01). Aceto­nitrile solvent mol­ecules and PF6 anions are inter­calated between these layers. Several inter­molecular N/C—H⋯F hydrogen bonds lead to formation of a three-dimensional supra­molecular network.

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Crystal structures of hydrogen-bonded 1:2 compounds of chloranilic acid with 2-pyridone, 3-hy­droxy­pyridine and 4-hyroxypyridine have been determined at 120 K. In each crystal structure, the acid and base mol­ecules are linked by short O—H⋯O and N—H⋯O hydrogen bonds.

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Mol­ecules of the complex fac-[ReCl(4-pyOH)2(CO)3] (4-pyOH is 4-hy­droxy­pyridine) and 4-pyridone are associated in ladder chains by hydrogen and coordination bonds.

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In the title indole derivatives, the sulfonyl-bound phenyl rings are almost orthogonal to the indole ring system, subtending dihedral angles of 88.33 (10) and 87.58 (16)°, respectively. The mol­ecules of both (I) and (II) feature intra­molecular C—H⋯O hydrogen bonds that generate S(6) ring motifs with the sulfone O atom. In the crystals, mol­ecules of (I) are linked by C—H—O hydrogen bonds, forming R_{4}^{4}(18) ring motifs while mol­ecules of (II) are linked by C—H—O and C—H—S hydrogen bonds, forming R_{2}^{2}(12) ring motifs.

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A new polymorph of di(thio­phen-3-yl) ketone differing from the previous structure by the mol­ecular assembly is reported and comparatively discussed.

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It is shown that tridentate imine ligands can control the nuclearity of copper(II) complexes based on the donor atoms present in the ligand. While the N,N′,N′′-donating imine ligand led to a mononuclear compound, the N,N′,O-donating imine ligand produced a binuclear metal complex.

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The structure of aceto­nitrile­aqua­[1,2-bis­(pyridin-2-ylmeth­yl)ethane-1,2-di­amine]­zinc(II) perchlorate contains a six-coordinate cation consisting of the tetra­dentate bis­picen ligand, coordinated water, and coordinated aceto­nitrile with the latter two ligands adopting a cis configuration.

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The natural diterpene known as pulcherrin J was isolated from stem barks of medicinally important Caesalpinia pulcherrima (L.). The mol­ecule is composed of a central core of three trans-fused cyclo­hexane rings and a near planar five-membered furan ring, along with an axially oriented cinnamate moiety and a­hydroxyl substituent attached to the C-8 and C-9 positions of the steroid ring system, respectively. Hirshfeld surface analysis indicates that the most significant contacts in packing are H⋯H (67.5%), followed by C⋯H (19.6%) and H⋯O (12.9%).

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The dominant resonance form of the title compound was identified from bond lengths and may correlate with a short intra­molecular O⋯O contact.

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KIn(HAsO4)2 adopts the KSc(HAsO4)2 structure type (space group C2/c), while RbIn(HAsO4)2 and CsIn(HAsO4)2 crystallize in the space group R-3c and are the first arsenate representatives of the RbFe(HPO4)2 structure type. All three compounds have tetra­hedral–octa­hedral framework topologies. The M+ cations, located in voids of the respective framework, are slightly disordered in RbIn(HAsO4)2. In KIn(HAsO4)2, there is a second K-atom position with a very low occupancy, which may suggest that the K atom can easily move in the channels extending along [101].

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The reaction of AgI with the tridentate ligand bis­(pyridin-3-ylmeth­yl)sulfane afforded a one-dimensional double-stranded chain polymeric structure with the charge balanced by a nitrate anion that is disordered over two sites. The AgI cation adopts a highly distorted trigonal–planar geometry coordinated by two pyridine N atoms and one S atom from three individual ligands. Each ligand bridges the AgI atoms to form a zigzag chain. Two adjacent chains are connected by an Ag—S bond, resulting in the formation of a twisted-ribbon type double-stranded chain. These chains are linked by π–π inter­actions, generating a three-dimensional supra­molecular network.

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In the crystal structure of the title compound, C23H19N5O3·0.58C2H6OS·0.42C2H3N, prepared by the azo coupling of the 4-nitro­phenyl­diazo­nium salt with 3a-(p-tol­yl)-2,3,3a,4-tetra­hydro-1H-benzo[d]pyrrolo­[1,2-a]imidazol-1-one, the azo mol­ecules are linked by N—H⋯O hydrogen bonds into chains along the a-axis direction, and by the π–π inter­action into [101] chains.

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The structure of the substituted 2-amino­pyrimidine salt of isophthalic acid comprises an almost planar unit in which the two pyrimidinium cations are cyclically hydrogen-bonded to the succinate dianion and further extended through hydrogen bonds into a one-dimensional supra­molecular structure.

Research communications

The first papers in this new format were published in July 2014. Research communications are longer papers with new text sections designed to help authors bring out the science behind their structure determinations. Figures are included in the published paper and, for the first time in Acta E, individual reports are not limited to single structure determinations. The Research communications format will make Acta E the natural home for structure determinations with interesting science to report.

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Acta E is now included in the Thomson Reuters Emerging Sources Citation Index.

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