The crystal structure of an epalrestat methanol solvate (C₁₅H₁₃NO₃S₂·CH₃OH) was determined by X-ray crystallography. The compound crystallized in a monoclinic system and was characterized as follows: P2/c, a = 14.1757(3)Å, b = 8.2338(2)Å, c = 28.6476(6)Å, β = 102.0075(7)°, Z = 8, V = 3270.6(1)ų. The epalrestat molecules formed hydrogen bonds with methanol solvent molecules between the carboxyl group of one epalrestat, the hydroxyl group of the methanol, and the carbonyl group of the rhodanine ring in another epalrestat.

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A rhenium(VII) complex with 2-[(2-pyridylmethyl)amino]ethanethiol (Hpmaet), [Re(pmaet)O₃], was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 123 K. It crystallizes in the monoclinic space group P2₁/n with a = 10.054(5)Å, b = 8.466(4)Å, c = 12.924(7)Å, β = 108.552(9)°, V = 1043.0(10)ų, D_x = 2.557 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0195 and 0.0545, respectively, for all 2401 independent reflections. The compound consists of an octahedral molecule of rhenium(VII) with facial pmaet and three oxido oxygens.

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The structure of 4-hydroxy-3-methoxybenzaldehyde-4-methylthiosemicarbazone (VAMTSC) was determined by X-ray crystallography. The molecular structure matches the asymmetric unit, and the compound crystallizes in a monoclinic system. It was characterized thus: P2₁/c, a = 8.4960(3), b = 8.5040(2), c = 17.2236(6)Å, β = 111.513(2)°, Z = 4, V = 1157.71(6)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0403 and wR2 = 0.078.

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The cobalt(II) complex [Co(NMF)₆](BPh₄)₂ [NMF = N-methylformamide] [hexakis(N-methylformamide-κO)cobalt(II) bis(tetraphenylborate)] was prepared, and characterized by a single-crystal X-ray method. The compound crystallizes in the triclinic space group P1 and Z = 4 with cell parameters: a = 10.9801(15)Å, b = 22.581(3)Å, c = 23.805(3)Å, α = 72.198(2)°, β = 87.088(2)°, γ = 88.497(3)°, V = 5612.0(13)ų. Two types of [Co(NMF)₆]²⁺ cations are found in a crystal, and six NMF molecules coordinate to a cobalt(II) center in each cation. Interestingly, one has a pseudo-S₆ symmetry, and the other has a pseudo-C₂ symmetry.

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C₂₂H₃₂O₃ (1) and C₂₄H₃₆O₃ (2) are orthorhombic, P2₁2₁2₁. The unit-cell dimensions for 1 and 2 at 298(2)K are a = 8.9849(11), b = 12.5300(15), c = 17.441(2)Å, V = 1963.5(4)ų, D_x = 1.165 g/cm³, and Z = 4; a = 8.9457(17), b = 12.447(2), c = 19.242(4)Å, V = 2142.6(7)ų, D_x = 1.155 g/cm³, and Z = 4, respectively. The R values for molecules 1 and 2 are R = 0.0607 for 3598 reflections and R = 0.0445 for 3981 reflections, respectively. The A, B, C, and D rings for molecule 1 are chair, half-chair, chair, half-chair (for molecule 2: chair, half-chair, chair, half-chair) conformations. In both structures, the molecules are linked by C-H…O interactions and van der Waals forces.

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The title compound 3,3′-ethanediylidenebis(1-ethylindoline-2-one) was isolated as a byproduct through the reaction of isatin and sodium hydride with iodoethane in tetrahydrofurane. It crystallizes in the space group P2₁/c (#14) with the cell parameters a = 8.7451(9)Å, b = 15.1964(13)Å, c = 6.9425(6)Å, β = 113.561(2)°, Z = 2, and V = 845.70(14)ų. The 3,3′-ethanediylidenebis(indoline-2-one) core is planar, adopting an s-trans conformation with regard to the ethanediylidene moiety. The crystal structure is stabilized by intermolecular C=O…HC and N…HC hydrogen bonds as well as by π-π interactions.

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The title compound, 2-(p-anilinophenyl)-2-phenylindan-1,3-dione, was isolated by reacting 2-phenylindan-1,3-dione with N,N-diphenylhydrazine. This compound crystallizes in the monoclinic crystal system in the space group P2₁/n (#14) with the cell parameters a = 9.837(4)Å, b = 13.221(3)Å, c = 16.325(6)Å, β = 107.914(15)°, Z = 4, and V = 2020.2(12)ų. The five-membered ring of the indan-1,3-dione core is slightly bent, forming an envelope-like conformation. The crystal structure is stabilized by the N-H…O=C hydrogen bond with a carbonyl oxygen and by the weak C-H…O=C interaction with another carbonyl oxygen.

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The title compound, (5,10,15,20-tetrakis(2,3,5,6-tetrafluoro-4-(dimethylamino)phenyl)porphyrinato)palladium(II)-dichloromethane (1/1), crystallized in the triclinic space group P1 with the following unit-cell parameters: a = 10.100(2)Å, b = 14.544(3)Å, c = 17.861(4)Å, α = 83.619(10)°, β = 85.295(10)°, γ = 73.839(8)°, V = 2500.7(9)ų and Z = 2. The crystal structure was solved by direct methods, and refined by full-matrix least-squares procedures to a final R-value of 0.0494 for 11445 observed reflections. A porphyrin ligand coordinated to palladium atom, and four 2,3,5,6-tetrafluoro-4-(dimethylamino)phenyl groups bonded to the meso position of the porphyrin skeleton.

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The title compound, (4S)-4-[(2S)-butan-2-yl]-1,3-oxazolidine-2,5-dione, C₇H₁₁NO₃ was synthesized and the crystal structure was determined by the single-crystal X-ray diffraction method at 123 K. It crystallizes in an orthorhombic space group, P2₁2₁2₁, with unit-cell parameters: a = 6.4713(3)Å, b = 6.7196(3)Å, c = 17.9369(7)Å, and Z = 4. The oxazolidine ring in this compound is planar with a maximum deviation of 0.037(4)Å.

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The nickel(II) complex [Ni{H₂(ide)}₂](BPh₄)₂·BPh(ide)·(CH₃)₂CHOH (H₂(ide) = 2,2′-iminodiethanol) was prepared, and characterized by a single-crystal X-ray method. The compound crystallizes in the triclinic space group, P1 and Z = 2, with cell parameters a = 11.8846(12)Å, b = 14.5812(11)Å, c = 20.235(2)Å, α = 73.031(5)°, β = 84.561(6)°, γ = 66.297(5)°, V = 3069.9(5)ų. In the complex cation, two H₂(ide) ligands work as tridentate ligands in the fac-forms, and the amino nitrogen atoms are at the cis-positions. The crystal contains an organoboron coordination complex, BPh(ide), and the complex cation is hydrogen-bonded to both BPh(ide) and 2-propanol molecules.

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p-Nitrophenyl[36]trithiononaphyrin(1.0.0.1.0.0.1.0.0), C₇₅H₆₉N₉O₆S₃, was isolated. The crystal structure was determined by single-crystal X-ray diffraction at 200(2)K and belonged to the monoclinic space group Cc. The lattice parameters are a = 24.986(4)Å, b = 23.548(4)Å, c = 13.762(7)Å, β = 101.358(2)°, V = 7939(2)ų, Dx = 1.078 g/cm³, and Z = 4; R1 [I > 2σ(I)] and wR2 are 0.0656 and 0.1368, respectively, for 17971 independent reflections. The results of a ¹H NMR study suggested that the title compound has a weak antiaromatic character because of a slight distortion of its large macrocyclic ring, as determined by single-crystal X-ray analysis. Single-crystal X-ray analysis also revealed that the 2,5-substituted thiophene rings are inverted in the title compound.

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The X-ray crystal structure of 6-fluoro-3,4-methylenedioxyamphetamine hydrochloride, a fluoro analogue of 3,4-(methylenedioxy)amphetamine, was established. It crystallizes in the orthorhombic space group Pbac with cell parameters a = 24.679(4)Å, b = 9.873(4)Å, c = 9.253(5)Å, V = 2254.5(16)ų and Z = 8. The crystal structure was refined to final values of R1 = 0.0601 and wR2 = 0.1479. An X-ray crystal structure analysis revealed that each molecule features strong intermolecular N-H…Cl hydrogen bonds.

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A dinuclear cobalt(II) complex with N,N,N′,N′-tetrakis(3,5-dimethyl-1-pyrazolyl)methyl-1,4-phenylenediamine (tpmp), [Co₂(tpmp)Cl₄], was isolated. The crystal structure was determined by a single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinic space group P2₁/n with a = 12.4671(16)Å, b = 10.1719(13)Å, c = 29.292(4)Å, β = 101.260(3)°, V = 3643.1(8)ų, D_x = 1.459 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0589 and 0.1203, respectively, for all 8453 independent reflections. The complex consists of two tetrahedral cobalt(II) chromophores with two pyrazolato-nitrogen atoms of tpmp and two chloride atoms that are connected to the phenylenediamine moiety of tpmp with a Co…Co separation of 11.522(1)Å.

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The title compound, [Co(NCS)₂(C₅H₆N₂)₂], crystalized in the Pmmn space group; a = 13.029(5)Å, b = 14.551(6)Å, c = 4.1463(16)Å, V = 786.1(5)ų, D_x = 1.535 g/cm³, and Z = 2. The R1 [I > 2σ(I)]; the wR₂ (all 978 independent reflections) values are 0.0570 and 0.1489, respectively. The Co complex has mm2 crystallographic symmetry, and also has a compressed tetrahedral coordination geometry. The complexes are stacked so as to form a characteristic one-dimensional chain structure; weak interactions exist between adjacent pyridine rings, and NCS and pyridine rings are observed.

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The structure of 7-bromo-4-isopropyl-2-[[(4-methylphenyl)-sulfonyl]oxy]tropone was determined by X-ray crystallography. It crystallizes in the space group P2₁/c (#14) with cell parameters a = 9.4884(6)Å, b = 9.5235(6)Å, c = 18.1540(13)Å, β = 95.203(2)°, Z = 4, and V = 1633.7(2)ų. The tropone and benzene rings in 1 adopt a syn conformation with respect to each other. Intramolecular C-H…π and intermolecular C-H…O, C-H…Br, and π…π interactions were observed in the crystal lattice.

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The title compound of a lantern-type rhodium(II) dinuclear complex, cis-[Rh₂(3,5-Me₂-pf)₂(O₂CCF₃)₂(H₂O)₂]·0.5C₆H₁₄ (3,5-Me₂-pf^- = N,N′-bis(3,5-dimethylphenyl)formamidinate anion), was isolated and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the triclinic space group P1 with a = 11.4725(16)Å, b = 12.4679(17)Å, c = 16.113(2)Å, α = 77.391(2)°, β = 75.265(2)°, γ = 85.548(2)°, V = 2174.6(5)ų, D_x = 1.548 g/cm3, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0275 and 0.0625, respectively, for all 9465 independent reflections. The cis-(2:2) arrangement of the 3,5-Me₂-pf and trifluoroacetato ligands within the dinuclear core was confirmed, the axial sites of the dimer being occupied by the water molecules. The Rh-Rh distance is 2.4538(4)Å and the axial Rh-O (H₂O) distances are 2.3309(16) and 2.3196(16)Å.

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μ-Alkoxido-bridged dinuclear dioxidovanadium(V) and tetranuclear oxidovanadium(IV) complexes with 2,6-bis(hydroxymethyl)-4-methylphenol (H₃bhmp), [Et₃NH]₂[(VO₂)₂(Hbhmp)₂] (1) and [Et₃NH]₂[(VO)₄(Hbhmp)₂(MeO)₂(SO₄)₂] (2) were synthesized. The crystal structures were determined by the single-crystal X-ray diffraction method at 293 K. Compound 1 crystallizes in the triclinic space group P1 with a = 8.5059(15)Å, b = 9.8815(17)Å, c = 11.3339(19)Å, α = 82.916(3)°, β = 83.819(3)°, γ = 65.595(3)°, V = 859.2(3)ų, D_x = 1.358 g/cm³, D_m (floatation) = 1.358 g/cm³, and Z = 1. However, compound 2 crystallizes in the triclinic space group P1 with a = 10.731(14)Å, b = 11.373(15)Å, c = 11.558(15)Å, α = 104.28(3)°, β = 112.76(2)°, γ = 108.23(2)°, V = 1121(3)ų, D_x = 1.568 g/cm³, D_m (floatation) = 1.554 g/cm³, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0409 and 0.1166 for 1 and 0.0514 and 0.1454 for 2, respectively. Compound 1 consists of triethylammonium cations and the di-μ-alkoxido-bridged dinuclear dioxidovanadium(V) complex anion [(VO₂)₂(Hbhmp)₂]^2-, whereas compound 2 consists of triethylammonium cations and the di-μ-sulfato-di-μ-methoxido-di-μ-alkoxido-di-μ-phenoxido-bridged tetranuclear oxidovanadium(IV) complex anion [(VO)₄(Hbhmp)₂(MeO)₂(SO₄)₂]^2- with a parallelogram array of four vanadium atoms.

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The asymmetric unit of the title hydrated salt contains one [(C₆H₅CH₂)₂NH₂]⁺ cation, one [(C₆H₅)₂P(O)(O)]^- anion and one solvent water molecule. In the anion, the P atom is in a distorted tetrahedral [C]₂P[O][O] environment with the highest angle of 116.38(9)° for the O-P-O angle and the lowest angle of 102.74(10)° for the C-P-C angle. The most characteristic feature of the cation is the open C-N-C angle (of 113.50(17)°). In the crystal structure, the cations, anions and water molecules are hydrogen-bonded to each other, through O-H…O (O…O = 2.904(3)Å and 2.921(2)Å) and N-H…O (N…O = 2.731(2)Å and 2.766(3)Å) hydrogen bonds, building a linear arrangement along the b axis. In this hydrogen-bond pattern, the PO groups act as a double hydrogen-bond acceptor.

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4-Carboxybenzylidene-4′-hexylaniline (1) exhibits enantiotropic smectic F, smectic C, and nematic phases. It crystallizes in the space group P1 (#2) with cell parameters a = 6.4250(18)Å, b = 8.495(2)Å, c = 16.665(5)Å, α = 93.09(2)°, β = 98.399(17)°, γ = 110.373(14)°, Z = 2, and 838.2(4)ų. The molecule contains intermolecular hydrogen bonds, resulting in centrosymmetric dimers. The two benzene rings are nearly coplanar. The molecules form a tilted layer structure via intermolecular O-H…O, C-H…O, C-H…π and π…π interactions.

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The structure of [Cu(II)(bqdmpn)](NO₃)₂ [BQDMPN = N,N′-bis(2-methylquinolyl)dimethyl-1,3-propanediamine] was determined by the single-crystal X-ray diffraction method at 93 K. The compound crystallized in a orthorhombic system and was characterized thus: Pbcn, a = 12.666(2), b = 12.687(2), c = 15.113(3)Å, Z = 4, V = 2428.7(7)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values are 0.0356 and 0.0994, respectively, for all 3907 independent reflections. The geometry around the copper center is distorted square planar with BQDMPN.

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The structure of N,N′-bis(5-octyloxytropon-2-yl)piperazine was determined by X-ray crystallography. It crystallizes in the space group C2/c (#15) with cell parameters a = 31.61(2)Å, b = 7.686(5)Å, c = 12.807(8)Å, β = 97.643(19)°, Z = 4, and V = 3084(4)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 C-H…π interactions were observed in the crystal lattice.

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The nickel(II) complex [Ni(NMF)₆](BPh₄)₂ [NMF = N-methylformamide] [hexakis(N-methylformamide-κO)nickel(II) bis(tetraphenylborate)] was prepared, and characterized by a single-crystal X-ray method. The compound crystallizes in the triclinic space group P1 and Z = 2 with the following cell parameters: a = 10.680(2)Å, b = 13.271(3)Å, c = 19.960(4)Å, α = 86.043(6)°, β = 84.483(6)°, γ = 87.335(7)°, V = 2807.0(10)ų. Two types of [Ni(NMF)₆]²⁺ cations are found in a crystal, but both have a pseudo-S₆ symmetry.

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The title compound, a chain complex of copper(II) pivalate with 1,2-bis(4-pyridyl)ethane (bpe), catena(tetrakis(μ-pivalato-O,O′)(μ-1,2-bis(4-pyridyl)ethane-N,N′)dicopper(II)) [Cu₂(piv)₄(bpe)]_n, was isolated. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinic space group C2/c with a = 21.267(3)Å, b = 18.250(2)Å, c = 10.1715(13)Å, β = 99.716(3)°, V = 3891.2(9)ų, D_x = 1.222 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0509 and 0.1360, respectively, for all 4516 independent reflections. The crystal contains zigzag chain molecules with an alternating arrangement of Cu₂(piv)₄ [Cu…Cu 2.6207(8)Å] and dpe. The adsorption isotherm measurement showed no adsorption property for N₂.

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Tetranuclear nickel(II) and cobalt(II) complexes with μ₃-O-3,5-dimethyl-1-pyrazylmethanolato (dmpm) and μ-O,O′-acetato, [M₄(dmpm)₄(O₂CCH₃)₄]·2CH₃CN (M = Ni, Co), were isolated. The crystal structures were determined by the single-crystal X-ray diffraction method at 90 K. Both of the structures are isomorphous in the tetragonal space group P4₂/n with a = 11.5812(11)Å, c = 16.580(2)Å, V = 2223.8(4)ų, D_x = 1.459 g/cm³, and Z = 2 for the nickel(II) complex; these values are a = 11.608(2)Å, c = 16.717(4)Å, V = 2252.4(7)ų, D_x = 1.555 g/cm³, and Z = 2 for the cobalt(II) complex. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0288 and 0.0842, and 0.1046 and 0.2786, for the former and the latter, respectively. Each complex has a cubane-like tetranuclear M₄O₄ core with octahedral NO₅ geometry; the closest Ni…Ni separation is 2.9750(4)Å, or the Co…Co separation of 3.0433(19)Å.

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The solid-state structure of bis(acetone-κO)-1,4,8,11-tetraazacyclotetradecane copper(II) ditetraphenylborate acetone disolvate was determine by single-crystal X-ray diffraction analysis. Single crystals of the title compound were obtained from acetone and diethyl ether. The compound crystallizes in a triclinic system, space group P1. The unit-cell parameters were determined to be a = 12.2123(15), b = 12.5684(16), c = 12.9841(16)Å, α = 100.526(2)°, β = 107.4237(19)°, γ = 116.1558(19)°, Z = 1, V = 1587.4(3)ų. The crystal includes two acetone molecules. One of which shows a conformational disorder. The crystal structure was solved by dual space methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0392 and wR2 = 0.0999 for I > 2σ(I) and all data, respectively.

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The title compound, 1,3-bis(5-nitrosalicylideneamino)-2-propanol, was synthesized and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the monoclinic space group C2/c with a = 18.388(5)Å, b = 10.355(3)Å, c = 19.159(5)Å, β = 113.596(6)°, V = 3343.1(15)ų, D_x = 1.543 g/cm³, and Z = 8. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0909 and 0.1730, respectively, for all 3867 independent reflections. The molecule is folded at the central carbon atom with a dihedral angle between the two approximate planes of 11.21°.

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The structure of 4,4′-bi(3-(1-methylethoxy)-3-cyclobutene-1,2-dione) was determined by X-ray crystallography. A symmetry operation (-x+1, -y+1, -z+2) generated the whole molecule. The compound crystallised in a monoclinic system and was characterised as follows: P2₁/c, a = 5.6929(5)Å, b = 13.3409(13)Å, c = 9.5865(9)Å, β = 106.414(2)°, Z = 2, V = 698.41(11)ų. The crystal structure was solved by a direct method and refined by full-matrix least-squares on F² to obtain final values of R₁ = 0.0423 and wR₂ = 0.00894. The carbon-carbon (C-C) bond lengths suggested that not only the cyclic-linker C-C bond, but also adjacent C-C bonds, are involved in two kinds of delocalised electron systems.

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The title compound, 1,4,7-tris(2-mercaptoethyl)-1,4,7-triazacyclononane (H₃tmtacn), was synthesized and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinic space group P2₁/n with a = 9.9553(13)Å, b = 13.7164(19)Å, c = 14.724(2)Å, β = 102.528(2)°, V = 1962.7(5)ų, D_x = 1.355 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0538 and 0.1436, respectively, for all 4528 independent reflections. The triazacyclononane moiety is protonated at the two nitrogen atoms with hydrogen-bonded chloride ions and water molecules as H₃tmtacn·2HCl·H₂O.

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