A tetranuclear heterometal complex, [MnNi(L1-H)₂(OAc)]₂·2CH₃OH [H₂L1-H = N-(2-oxymethylphenyl)-salicylideneimine], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in a monoclinic system, spaces group P2₁/n and Z = 4 with cell parameters a = 10.638(2)Å, b = 11.483(2)Å, c = 23.538(4)Å, β = 95.505(3)°, V = 2862.1(9)ų. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0682 and 0.1200, respectively, for all 6514 independent reflections. The tetranuclear hetero-metal arrangement is represented as defected double-cubane.

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The structure of 3-bromo-7-(dimethylamino)-4-methylcoumarin (1) was determined by X-ray crystallography. It crystallizes in the space group P2₁/n (#14) with cell parameters a = 9.000(3)Å, b = 11.561(3)Å, c = 10.591(3)Å, β = 96.5568(14)°, Z = 4, and V = 1094.8(5)ų. The molecule is almost planar. Intermolecular C=O…Br, C-H…O, C-H…π, and π…π interactions were observed in the crystal lattice.

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The title compound, potassium ethylenediaminetetraacetatocobaltate(III) dihydrate, K[Co(edta)]·2H₂O, was prepared. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 6.432(3)Å, b = 10.098(5)Å, c = 22.740(11)Å, V = 1477.0(12)ų, D_x = 1.899 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0283 and 0.0722, respectively, for all 3416 independent reflections. The cobalt atom is coordinated by two ethylenediamine-nitrogen and four glycinato-oxygen atoms in an octahedral geometry, whereas the potassium ion is coordinated by four glycinato-oxygen and two water-oxygen atoms in a distorted octahedron.

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The crystal structure of epalrestat dimethanol-solvate (C₁₅H₁₃NO₃S₂·2CH₃OH) was determined by X-ray crystallography. The crystal is a pseudopolymorphic form of the previously reported monomethanol solvate. The compound crystallized in a monoclinic system, and was characterized as follows: P1, a = 7.8868(2)Å, b = 8.1577(3)Å, c = 16.1069(5)Å, α = 85.5626(19)°, β = 77.790(2)°, γ = 67.5381(18)°, Z = 2, V = 936.00(5)ų. The pattern of the hydrogen bonds is designated by the graph-set R₆⁶(16), composed of two epalrestat and four methanol molecules. The planarity of the epalrestat molecules is lower than that of all other reported polymorphic forms of epalrestat.

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The crystal structure of o-carboxyphenylfluorone (denoted OCPF) was determined by X-ray diffraction. This compound crystallizes in triclinic, space group P1 with a = 8.738(2), b = 9.394(2), c = 11.712(2)Å, α = 107.747(3)°, β = 93.435(3)°, γ = 91.447(3)°, V = 913.0(3)ų, Z = 2. The final R value is 0.0730. The structure takes a dihedral formation consisting of xanthene and benzene carboxylic rings and tautomers. They exist with a zwitterionic character; the dihedral angle between the xanthene and benzene rings systems is 69.22(5)°, and the end of the rings of xanthene are inclined to each other at an angle of about 6.6(1)°.

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Erratum: X-ray Structure Analysis Online, 2015, Vol. 31, No. 11, p. 55On page 55, the surname of the first author should read MIKURIYA.

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The dinuclear zinc(II) complex [Zn₂(L)(MeCO₂)₂]BPh₄ [HL = 1:2 condensation product of 2,6-diformyl-4-methylphenol and 2-methoxyethylamine] was prepared, and characterized by a single-crystal X-ray method. The compound crystallized in the monoclinic space group P2₁/n and Z = 4 with the following cell parameters: a = 14.9150(18)Å, b = 10.2522(12)Å, c = 26.964(4)Å, β = 103.127(3)°, V = 4015.4(9)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values were 0.0351 and 0.0631, respectively, for all 8747 independent reflections. In the complex cation, [Zn₂(L)(MeCO₂)₂]⁺, two zinc(II) ions are bridged by the phenolate oxygen of the dinucleating ligand, L⁻, and two acetate ions. Both zinc(II) ions have trigonal bipyramidal coordination geometry.

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A μ-alkoxido-bridged tetranuclear oxidovanadium(IV) complex with 2,6-bis(hydroxymethyl)-4-methylphenol (H₃bhmp), [Et₃NH]₂[(VO)₄(Hbhmp)₂(EtO)₂(SO₄)₂] (1), was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. Compound 1 crystallizes in the triclinic space group P1 with a = 10.799(5)Å, b = 11.339(5)Å, c = 11.703(5)Å, α = 109.294(9)°, β = 114.158(7)°, γ = 102.452(9)°, V = 1127.0(8) ų, D_x = 1.601 g/cm³, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0548 and 0.1126, respectively. Compound 1 consists of triethylammonium cations and the di-μ-sulfato-di-μ-ethoxido-di-μ-alkoxido-di-μ-phenoxido-bridged tetranuclear oxidovanadium(IV) complex anion [(VO)₄(Hbhmp)₂(EtO)₂(SO₄)₂]²⁻ with a parallelogram array of four vanadium atoms.

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The structure of N,N′-bis(4-hexyloxybenzoyl)piperazine was determined by X-ray crystallography. It crystallizes in the space group P2₁/c (#14) with cell parameters a = 27.234(7)Å, b = 7.496(2)Å, c = 6.820(2)Å, β = 93.80(2)°, Z = 2, and V = 1389.3(6)ų. The molecule sits on a center of symmetry, such that the two benzoyl groups are in an anti conformation with respect to one another across the piperazine ring. Intermolecular C–H···O and C–H···π interactions were observed in the crystal lattice.

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The zinc(II) complex [Zn(DMF)₆](BPh₄)₂ [hexakis(N,N-dimethylformamide-κO)zinc(II) bis(tetraphenylborate)] was prepared, and characterized by a single-crystal X-ray method. The compound crystallizes in the orthorhombic space group Pca2₁ and Z = 4 with cell parameters a = 30.231(5)Å, b = 9.2503(14)Å, c = 22.083(3)Å, V = 6175.2(16)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values are 0.0365 and 0.0744, respectively, for all 14167 independent reflections. Six N,N-dimethylformamide (DMF) molecules coordinate to a zinc(II) ion to form a complex cation, [Zn(DMF)₆]²⁺, approximately belonging to an S₆ symmetry. The coordination geometry is trigonally compressed along the pseudo-S₆ axis. Among the six coordination bonds, one of them is 1.5% (0.031 Å) longer than the average (2.093 Å); another is 2.1% (0.044 Å) shorter than the average.

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The X-ray crystal structure of (E)-1-(3,4-methylenedioxy-6-fluorophenyl)-2-nitropropene, a potential antibacterial agent, was established. It crystallizes in the triclinic space group P-1 with cell parameters a = 6.716(1)Å, b = 8.323(2)Å, c = 9.453(2)Å, α = 82.75(2), β = 86.17(1), γ = 68.75(1), V = 488.4(1)ų and Z = 2. The crystal structure was refined to final values of R1 = 0.0439 and wR2 = 0.1340. The molecules pack to form a 2D network with head-to-tail short hydrogen bonding like contacts between the methylenedioxy and nitro groups, and between fluor and hydrogen of the aromatic rings of neighbouring molecules.

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The crystal structure of trans(Cl),cis(S)-dichlorobis(dimethyl sulfoxide-S)(N,N,N′,N′-tetramethylethylenediamine)ruthenium(II) was determined by X-ray crystallography. Single crystals were obtained from the reaction mixture after being left standing at 275 K. The complex crystallized in a monoclinic system, and was characterized as: P2₁/n, a = 8.616(5), b = 22.925(12), c = 8.991(5)Å, β = 94.415(6)°, Z = 4, V = 1770.7(16)ų. The R1 and wR2 values were 0.0540 and 0.1359, respectively, for 4045 reflections.

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The magnesium(II) complex [Mg(DMF)₆](BPh₄)₂ [hexakis(N,N-dimethylformamide-κO)magnesium(II)bis(tetraphenylborate)] was prepared, and characterized by single-crystal X-ray method. The compound crystallized in the orthorhombic space group Fddd and Z = 8 with cell parameters a = 17.107(4)Å, b = 20.585(5)Å, c = 35.776(8)Å, V = 12599(5)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values were 0.0583 and 0.1569, respectively, for all 3621 independent reflections. Six N,N-dimethylformamide (DMF) molecules coordinate to a magnesium(II) ion to form a complex cation, [Mg(DMF)₆]²⁺. Crystallographically, the cation seems to belong to the D₂ point group as the result of disorder; however, we have concluded that each cation must belong to the C₂ point group based on the DFT computation.

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A μ-ethoxido-bridged tetranuclear oxidovanadium(IV) complex with 2,6-bis(hydroxymethyl)-4-methylphenol (H₃bhmp), (Et₃NH)₂[(VO)₄(Hbhmp)₂(EtO)₂(SO₄)₂]·H₂O (1) was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. Compound 1 crystallizes in the trigonal space group R3 with a = 45.690(8)Å, c = 12.589(2)Å, V = 22758(9)ų, D_x = 1.451 g/cm³, and Z = 18. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0614 and 0.1701, respectively. Compound 1 consists of triethylammonium cations and the di-μ-sulfato-di-μ-ethoxido-di-μ-alkoxido-di-μ-phenoxido-bridged tetranuclear oxidovanadium(IV) complex anion [(VO)₄(Hbhmp)₂(EtO)₂(SO₄)₂]²⁻ with a parallelogram array of four vanadium atoms, and water molecules. The adsorption property was studied for N₂ gas with a specific surface area of 1.37 m² g⁻¹, estimated from an N₂ adsorption isotherm.

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The two independent molecules in a single crystal of the title compound, 3-amino-2-benzyl-6-bromo-1,2,4-triazin-5(2H)-one (C₁₀H₉BrN₄O), was determined by X-ray crystallography. The compound was grown from a protic polar solvent, EtOH, and crystallized in an orthorhombic system. It was characterized as follows: Pbca, a = 23.6829(13)Å, b = 7.5558(4)Å, c = 24.1777(13)Å, V = 4326.4(4)ų and Z = 16, resulting in a density, D_calc, of 1.726 g/cm³. The hydrogen-bonding systems assemble with N-H···O [graph set C¹₁(6)], N-H···N [graph set R²₂(8)], and N-H···N combine with N-H···O [graph set R⁴₄(12)].

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The germanium-boron compound, Ph₃GeBpin (pin = 1,2-O₂C₂Me₄), was isolated and the molecular structure was determined by a single crystal X-ray diffraction study at 188 K. The compound crystallizes in an orthorhombic system, space group Pca2₁ and Z = 8 with cell parameters of a = 16.669(4)Å, b = 9.933(2)Å, c = 26.907(6)Å, V = 4455.0(17)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values are 0.0463 and 0.1196, respectively, for all 9468 independent reflections. The molecular structure analysis reveals the boron atom lies in a roughly trigonal environment that contains one pinacolato group. The asymmetric unit contains two independent molecules and the B–Ge bond distances for the two molecules are 2.073(10) and 2.051(14)Å.

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The structure of N,N′-bis(5-butoxytropon-2-yl)piperazine was determined by X-ray crystallography. It crystallizes in the space group P1 (#2) with cell parameters a = 6.819(2)Å, b = 9.204(3)Å, c = 10.178(3)Å, α = 108.65(3)°, β = 106.23(2)°, γ = 92.71(3)°, Z = 1, and V = 574.6(3)ų. The molecule sits on a center of symmetry, such that the two tropone rings are in an anti conformation with respect to one another across the piperazine ring. Intermolecular C–H···O and π···π interactions were observed in the crystal lattice.

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The structure of the drug-drug multi-component crystal of acedoben–dimepranol (2:1) was determined by single-crystal X-ray crystallography. The compound crystallizes in a monoclinic system with space group P2₁/n resulting in the following unit cell: a = 7.78174(14)Å, b = 9.71395(18)Å, c = 63.5236(12)Å, β = 92.4271(7)°, Z = 4, V = 4797.53(15)ų. The final values were R₁ = 0.0443 and wR₂ = 0.1241. Two acedoben molecules share a hydrogen atom between the COOH and COO– groups forming a mono cationic dimer unit. A counter charge is on NH⁺ of the dimepranol molecule.

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A square-planar platinum(II) complex, cis-bis(3-tert-butyl-o-diiminobenzosemiquinonato)platinum(II), was synthesized and characterized by single-crystal X-ray diffraction. It crystalizes in the monoclinic space group P2₁/n and Z = 4 with the following cell parameters: a = 19.748(2)Å, b = 5.9608(7)Å, c = 22.948(3)Å, β = 113.4550(10)°, V = 2478.2(5)ų. The aromatic ring of the ligand is distorted into two shorter and four longer C–C bonds, which are representative of a o-diiminobenzosemiquinonate radical ligand.

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The X-ray crystal structure of 7-amino-4-iodo-3-propyl-1H-isochromen-1-one, a potential inhibitor in the production of amyloid β-peptide, was established. It crystallizes in the monoclinic space group P2₁/c with cell parameters a = 8.4258(8)Å, b = 25.4258(18)Å, c = 5.5515(6)Å, α = 90, β = 103.301(4), γ = 90, V = 1157.41(19)ų and Z = 4. The crystal structure was refined to final values of R₁ = 0.0623 and wR₂ = 0.1725. An X-ray crystal structure analysis revealed that each molecule features intermolecular N–H···O hydrogen bonds and halogen halogen interactions.

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The crystal structure of diphenyl (2-butylamido) phosphonate has been determined. This crystal belongs to the space group P2₁/c, and the asymmetric unit of the structure is composed of one complete molecule. The P atom has a distorted tetrahedral configuration with the O–P–O angle as the minimum bond angle at the P atom (97.74(18)°) and one of the O=P–O angles as the maximum angle (115.2(2)°). The oxygen atom of the P–O–C₆H₅ moiety may be ascribed with the sp² character, reflected in the P–O–C angles (120.8(3)° and 125.4(3)°). In the crystal structure, the molecules are aggregated through the N–H···O=P hydrogen bond (N1···O1 = 2.971(5)Å) in a one-dimensional chain along the b axis.

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The title complex crystallizes in a triclinic space group P-1, with unit-cell parameters of a = 4.8079(2)Å, b = 10.8505(3)Å, c = 11.7609(4)Å, α = 107.2057(13)°, β = 96.8425(13)°, γ = 102.2061(16)°, V = 561.89(3)ų, and Z = 2. The structure revealed C–H···O associations as well as π···π interactions between the zwitterionic quinaldic acid molecules, while other intermolecular associations between zwitterionic quinaldic acid and chloranilic acid molecules involve N⁺–H···O_carboxyl, and O–H···O_carboxyl interactions.

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The structure of diiodobis(1-(6-methylpyridine-2-yl)thiourea-kS)mercury(II) was determined by X-ray crystallography. This complex crystallizes in the space group P2₁/c, with cell parameters a = 10.3151(7)Å, b = 16.8739(10)Å, c = 13.7609(7)Å, β = 113.614(4)°, Z = 4, and V = 2194.6(2)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0381 and wR2 = 0.0666. Two molecules of 1-(6-methylpyridin-2-yl)thiourea are coordinated to the mercury ions through monodentate sulfur atoms which leads to the formation of a distorted tetrahedral environment complex.

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On page 47, Table 1, the 9th line,

    D_x = 1.333 g/m³

should read

    D_x = 1.333 g/cm³.

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Two dinuclear cobalt(III) complexes with 1,3-bis(5-nitrosalicylideneamino)-2-propanol (H₃b5nsalpr) and 1,3-bis(3-nitrosalicylideneamino)-2-propanol (H₃b3nsalpr), [Co₂(b5nsalpr)₂(CH₃OH)] and [Co₂(b3nsalpr)₂(CH₃OH)] were synthesized, and the crystal structures were determined by the single-crystal X-ray diffraction method at 90 K. The former crystallizes in the monoclinic space group C2/c with a = 31.560(19)Å, b = 17.013(10)Å, c = 18.888(12)Å, β = 124.334(9)°, V = 8375(9)ų, D_x = 1.612 g/cm³, and Z = 8. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0500 and 0.1376, respectively, for all 10031 independent reflections. The latter crystallizes in the triclinic space group P1 with a = 10.816(2)Å, b = 12.803(2)Å, c = 15.812(2)Å, α = 109.245(3), β = 95.243(4)°, γ = 92.303(3)°, V = 2052.8(7)ų, D_x = 1.613 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0469 and 0.1207, respectively, for all 8755 independent reflections. Both of the molecules are dinuclear cobalt(III) complexes with octahedral geometries, having two tridentate chelates of the two Schiff-base ligands for one cobalt atom and didentate and tridentate chelates of the two Schiff-base ligands and monodentate methanol molecule for the other cobalt atom. The spectral and electochemical features are consistent with the crystal structures.

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The crystal structure of (R)-2-(4-methylimidazolin-2-yl)phenol was determined by X-ray crystallography. Single crystals were obtained by slow evaporation of a methanol solution. The compound crystallized in the monoclinic space group P2₁ and Z = 2 with cell parameters a = 6.345(2)Å, b = 9.631(4)Å, c = 7.805(3)Å, V = 440.8(3)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values are 0.0346 and 0.0787, respectively, for all 1436 independent reflections. In the crystal, the compound exists as twitter-ions to form hydrogen-bonds with neighboring molecules. This intermolecular hydrogen-bonding interaction resulted in the construction of a 1D chain structure.

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