The crystal structures of optical resolving agents, (1S,2R)-2-(benzamido) cyclohexanecarboxylic acid (BACO) and its reduction product, (1S,2R)-2-(benzylamino)cyclohexanemethanol (BACH), were determined, and correlated with its physicochemical properties. The molecular structure in BACO is rigidly stabilized by the intramolecular hydrogen bond, but the tweeter-like structure in BACH is flexible. The results from thermal experiments essentially describe that the crystal form of BACO is more stable than that of BACH.

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The title compound, [Mo₃Pd(PPh₃)S₄(Tm)₃]PF₆·0.5CH₃OH·3H₂O (Tm = hydrotris(methimazolyl)borate), crystallized in the triclinic space group P1 with the following unit-cell parameters: a = 14.8578(3)Å, b = 14.9415(3)Å, c = 20.308(2)Å, α = 109.806(8)°, β = 96.546(7)°, γ = 101.774(7)°, V = 4069.5(5)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 0.0574 for 14608 observed reflections. The octahedral coordination geometry of two molybdenum atoms are defined by three sulfur donors from a tridentate Tm ligand and three μ₃S atoms. The distorted trigonalbipyramidal geometry of the remaining molybdenum atom is defined by two sulfur donors from a bidentate Tm ligand and three μ₃S atoms.

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The title compound, 6-methyl-4-[(quinolin-8-yloxy)methyl]-2H-chromen-2-one, crystallizes under a monoclinic system with space group P2₁/c. The unit cell parameters are a = 7.4641(2), b = 12.1483(3) c = 17.1084(4)Å, β = 99.667(1), Z = 4. The molecule is almost planar and the quinoline ring makes a dihedral angle of 2.86(3)° with the coumarin moiety. The molecules are stabilized by intermolecular C-H…O, C-H…π and π…π stacking interactions in the solid state.

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A chain complex of rhodium(II) acetate with 1,4-diazabicyclo[2.2.2]octane (dabco), [Rh₂(CH₃CO₂)₄(dabco)], was prepared, and 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 = 10.274(6)Å, b = 15.689(10)Å, c = 11.547(7)Å, β = 97.202(13)°, V = 1847(2)ų, D_x = 1.993 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0642 and 0.1598, respectively, for all 2174 independent reflections. The complex is a linear chain molecule with an alternating arrangement of Rh₂(CH₃CO₂)₄ [Rh-Rh 2.3598(15)Å] and dabco. The adsorption property was confirmed for N₂ with a specific surface area of 190.1 m²/g.

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The title compound, 2-(2-methyl-4-nitro-1H-imidazol-1-yl)-N′-[(1E)-1-phenylethylidene]acetohydrazide, C₁₄H₁₅N₅O₃, crystallizes in the monoclinic space group P2₁/n with unit-cell parameters: a = 10.8689(4), b = 10.5644(3), c = 12.9608(4)Å, β = 94.606(3)°, Z = 4. In the molecule, the mean plane of the imidazole ring forms a dihedral angle of 64.46(7)° with the benzene ring. The crystal structure was refined to a final R-value of 0.0474 for 2112 observed reflections. In the crystal, N-H…O intermolecular hydrogen bonds link the molecules into dimmers.

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The manganese(II) complex [Mn(DMF)₆](BPh₄)₂ [DMF = N,N-dimethylformamide] [hexakis(N,N-dimethylformamide-κO)manganese(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 = 1 with cell parameters: a = 10.0628(16)Å, b = 12.1027(19)Å, c = 14.881(2)Å, α = 112.191(3)°, β = 93.081(3)°, γ = 108.055(3)°, V = 1565.1(4)ų. Six DMF molecules coordinate to a manganese(II) center to form a [Mn(DMF)₆]²⁺ cation, somehow approximated to an S₆ symmetry; however, the coordination geometry is apparently compressed along a pseudo-trigonal axis different from the pseudo-S₆ axis.

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Halogen bonding in a 1-methyl-2,4,5-triiodoimidazole crystal was investigated. This compound crystallizes in a monoclinic, space group C2/c, with cell parameters: a = 16.7627(17)Å, b = 14.8566(14)Å, c = 22.350(2)Å, β = 101.2380(10)°, V = 5459.0(9)ų, and Z = 24. The crystal structure was solved by a direct method and refined by full-matrix least-squares to a final R value 0.0316 with I > 2σ(I). The three molecules formed a triangular trimer through three intermolecular halogen bonds between the 2-iodide groups and the 3-nitrogens.

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A six-coordinated Ni(II) complex, bis(O-propylxanthato)bis(3-chloropyridine)nickel(II), [Ni(C₅H₄NCl)₂(S₂COC₃H₇)₂], has been synthesized by the reaction of bis(O-propylxanthato)nickel(II) with 3-chloropyridine in acetone. The structure of the title compound was elucidated by a single-crystal X-ray diffraction method. The compound crystallizes in the monoclinic space group P2₁/c with unit-cell parameters: a = 9.4079(1), b = 10.7323(2), c = 11.7498(2)Å and β = 96.443(1)°. The crystal structure was solved by direct methods and refined by full-matrix least-squares procedures to a final R-value of 0.023 for 2064 observed reflections. The asymmetric unit comprises half a molecule and the nickel(II) cation lies on an inversion centre. The pyridine ring is coplanar, and is held almost perpendicular to the dithiocarbonato group. Molecules in the crystal are packed together to form layers, which appear to extend diagonally along the ac-plane.

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The nickel(II) complex [Ni(DMSO)₆](BPh₄)₂ (DMSO = dimethylsulfoxide) [hexakis(dimethylsulfoxide-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 = 1 with cell parameters a = 12.4224(17)Å, b = 12.5588(18)Å, c = 12.9099(18)Å, α = 61.745(2)°, β = 89.999(2)°, γ = 63.942(2)°, V = 1537.8(4)³. Six DMSO molecules coordinate to a nickel(II) center to form a [Ni(DMSO)₆]²⁺ cation. In the present crystal, the DMSO molecules are disordered, and two conformers of [Ni(DMSO)₆]²⁺ were found to be superimposed. The NiO₆S₆ units in both conformers are approximated by an S₆-propeller-like structure; however, in conformer A, the Ni(DMSO)₄ unit in the complex cation is approximated by an S₄-propeller-like structure, and tetragonal elongation is observed along the pseudo-S₄ axis; while in conformer B, the whole structure is approximated as an S₆-propeller-like structure, and a trigonal compression is observed along the pseudo-S₆ axis.

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Single crystals of complex of Ni(II), bis(O-propyldithiocarbonato-κ²S,S′)(3,5-lutidine-κN)nickel(II) [Ni(S₂COCH₂CH₂CH₃)_2-(C₇H₉N)₂] have been synthesized by the reaction of bis(O-propyldithiocarbonato)nickel(II) with 3,5-lutidine in acetone, and its structure elucidated by the single-crystal X-ray diffraction method. The complex crystallizes in the triclinic space group P1 with unit-cell parameters: a = 7.008(5), b = 9.546(5), c = 10.621(5)Å, α = 87.484(5)°, β = 72.927(5)° and γ = 75.686(5)°. The crystal structure was solved by direct methods and refined by full-matrix least-squares procedures to a final R-value of 0.0371 for 2074 observed reflections. The two pyridine rings are coplanar, and are held almost perpendicular to the dithiocarbonato groups. The compound has a trans octahedral geometry.

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The title compound, an adduct of rhodium(II) benzoate [Rh₂(bz)₄] with piperazine (pip), catena(tetrakis(μ-benzoato-O,O′)(μ-piperazine-N,N′)dirhodium(II)-acetonitrile (1/2)) [Rh₂(bz)₄(pip)]_n·2nCH₃CN, 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 = 10.812(2)Å, b = 11.393(3)Å, c = 15.331(3)Å, α = 71.014(5)°, β = 87.063(5)°, γ = 76.451(5)°, V = 1734.4(8)ų, D_x = 1.644 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0558 and 0.1367, respectively, for all 6986 independent reflections. The crystal contains zigzag chain molecules with an alternating arrangement of Rh₂(bz)₄ [Rh-Rh 2.4010(10), 2.4066(10)Å] and piperadine, and acetonitrile molecules. The adsorption property was confirmed for N₂ with a specific surface area of 52.7 m²/g.

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The crystal structure of epalrestat non-solvate (C₁₅H₁₃NO₃S₂) was determined by X-ray crystallography. The compound crystallized in a triclinic system and was characterized as follows: P1, a = 8.20888(15)Å, b = 11.6639(2)Å, c = 16.3107(3)Å, α = 96.5985(8)°, β = 93.8393(8)°, γ = 104.6780(8)°, Z = 4, V = 1493.22(5)ų. Neighboring epalrestat molecules formed intermolecular hydrogen bonds between the carboxyl group and the carbonyl group of the rhodanine ring and the cyclic structure from four molecules.

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The title compound of N,N′-bis(3,5-dichlorophenyl)formamidine, which is abbreviated as H(3,5-Cl₂-pf), 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 = 7.9265(13)Å, b = 9.3588(15)Å, c = 10.4003(17)Å, α = 76.579(3)°, β = 72.529(2)°, γ = 74.249(2)°, V = 698.7(2)ų, D_x = 1.588 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0276 and 0.0771, respectively, for all 3046 independent reflections. The C-N (amine) single bond (1.3486(18)Å) and C=N (imine) double bond (1.2836(18)Å) within the H(3,5-Cl₂-pf) molecule were confirmed. Two H(3,5-Cl₂-pf) molecules are associated with a set of hydrogen bonds through each amine and imine nitrogen atoms with a N^amine...N^imine distance of 3.0264(17)Å.

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The crystal structure of a copper(II) complex with 2-pyridinecarboxylic acid anhydride ([Cu₂(2-Py)₂(H₂O)(OH)₂(SO₄)]) was determined by single-crystal X-ray diffractometry. [Cu₂(2-Py)₂(H₂O)(OH)₂(SO₄)] crystallized in the orthorhombic system, space group Cmc2₁, with a = 16.046(2), b = 12.8608(8), c = 12.8905(9)Å, V = 2660.2(4)ų, Z = 4. The crystal structure was solved by direct methods and refined by full-matrix least squares on F² to final values of R1 = 0.0613. The complex would produce a π-π interaction between [Cu(2-Py)(OH)₂] and [Cu(2-Py)(H₂O)(SO₄)] in cooperation with a weak coordination of the sulfate ion to the copper(II).

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The title compound, a chain adduct of rhodium(II) acetate with 1,2-bis(4-pyridyl)ethane (bpe), catena(tetrakis(μ-acetao-O,O′)(μ-1,2-bis(4-pyridyl)ethane-N,N′)dirhodium(II)-water (1/2)), [Rh₂(CH₃CO₂)₄(bpe)]_n·2nH₂O, 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 = 24.937(5)Å, b = 13.211(3)Å, c = 8.8480(19)Å, β = 94.189(3)°, V = 2907.0(11)ų, D_x = 1.513 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0356 and 0.0863, respectively, for all 3324 independent reflections. The molecule has a linear chain with an alternating arrangement of Rh₂(CH₃CO₂)₄ [Rh-Rh 2.3990(8)Å] and bpe. The specific surface area estimated from a N₂ adsorption isotherm was 65.6 m² g^-1.

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The title compound, a chain adduct of molybdenum(II) acetate with 1,2-bis(4-pyridyl)ethane (bpe), catena(tetrakis(μ-acetato-O,O′)(μ-1,2-bis(4-pyridyl)ethane-N,N′)dimolybdenum(II)), [Mo₂(CH₃CO₂)₄(bpe)]_n, was synthesized, and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the triclinic space group P1 with a = 7.8313(12)Å, b = 8.5393(13)Å, c = 9.9498(14)Å, α = 73.412(3)°, β = 68.894(2)°, γ = 73.198(3)°, V = 581.86(15)ų, D_x = 1.747 g/cm³, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0309 and 0.0680, respectively, for all 2580 independent reflections. The molecule has a zigzag chain structure with an alternating arrangement of Mo₂(CH₃CO₂)₄ [Mo-Mo 2.0984(5)Å] and bpe. The adsorption isotherm was investigated, and no adsorption property was found for N₂.

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The title compound, a chain adduct of molybdenum(II) acetate with trans-1,2-bis(4-pyridyl)ethylene (bpel), catena(tetrakis(μ-acetato-O,O′)(μ-trans-1,2-bis(4-pyridyl)ethylene-N,N′)dimolybdenum(II)), [Mo₂(CH₃CO₂)₄(bpel)]_n, was synthesized, 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 = 7.6144(15)Å, b = 8.4800(16)Å, c = 9.7140(19)Å, α = 99.026(3)°, β = 112.749(3)°, γ = 103.210(3)°, V = 541.72(18)ų, D_x = 1.871 g/cm³, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0336 and 0.0898, respectively, for all 2324 independent reflections. The molecule has a zigzag chain structure with an alternating arrangement of Mo₂(CH₃CO₂)₄ and bpel [Mo-Mo 2.1038(5)Å, Mo-N 2.591(3)Å]. The adsorption isotherm was investigated and no adsorption property was found for N₂.

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The crystal structure of N-[4-hydroxy-3-nitro-5-(trifluoromethyl)phenyl]-2-methylpropaneamide was determined by X-ray crystallography. The title compound crystal, a monoclinic system, was characterized as follows: P2₁/c, a = 4.9578(4), b = 12.2784(12), c = 21.4038(19)Å, β = 93.308(2)°, Z = 4, V = 1300.8(2)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to the final value of R = 0.0604.

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Nickel(II) 5,10,15,20-tetraphenyl[1,2-c]pyrrolo-21-ethylcarboxyl-22-dipyrrylmethylporphyrin, C₅₈H₄₁N₇O₂Ni, was synthesized. The crystal structure was determined by single-crystal X-ray diffraction at 150(2)K, and belongs to monoclinic space group P2₁/n with lattice parameters of a = 17.002(5)Å, b = 11.984(3)Å, c = 24.361(7)Å, β = 92.289(4)°, V = 4960(2)ų, D_x = 1.241 g/cm³, and Z = 4. R1 [I > 2σ(I)] and wR2 were 0.0540 and 0.1188, respectively, for 6229 obserbedreflections.

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Nickel(II) 5,10,15,20-tetraphenyl[1,2-c](4′,5′-dimethyl)imidazolylpyrrolo-21-ethylcarboxyl-porphyrin, C₅₄H₃₉N₇Ni·CHCl₃, was isolated. The crystal structure was determined by single-crystal X-ray diffraction at 150 K, and belonged to the triclinic space group P1 with a = 11.746(6)Å, b = 14.006(8)Å, c = 14.915(8)Å, α = 104.878(8)°, β = 98.664(7)°, γ = 100.314(7)°, V = 2283(2)ų, D_x = 1.449 g/cm³, and Z = 2. R1 [I > 2σ(I)] and wR2 were 0.0870 and 0.17032, respectively, for 9067 independent reflections. It contained high-strain molecules having horse-saddle shapes.

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The title compound, (C₂₄H₂₀P)₂(C₆H₄N₂O₆S₂)CuI·0.34H₂O, was obtained by the slow evaporation of a solvent from an acetonitrile solution containing a mixture of (PPh₄)₂N,N′-disulfobenzoquinonediimine and CuI. The structure consists of a one-dimensional metal-organic framework of the dianion and CuI. The anionic chains are surrounded by relatively large counter-cations, and are thus well isolated from each other.

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A crystal of β-D-fructofuranosyl 4-chloro-4-deoxy-α-D-galactopyranoside was prepared, and its crystal structure was determined at the space group P2₁. The cell parameters were a = 8.048(5), b = 8.682(5), c = 12.059(8)Å, β = 107.03(2)° and Z = 2. The crystal structure was solved by a direct method and refined by full-matrix least-squares to a final R value of 0.0529.

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The title compound, a chain adduct of rhodium(II) benzoate with 1,4-diazabicyclo[2.2.2]octane (dabco), catena(tetrakis(μ-benzoato-O,O′)(μ-1,4-diazabicyclo[2.2.2]octane-N,N′)dirhodium(II)-acetonitrile(1/4)), [Rh₂(C₆H₅CO₂)₄(dabco)]_n·4nCH₃CN, was isolated. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the tetragonal space group P4/n with a = 21.3695(18)Å, c = 9.6278(12)Å, V = 4396.6(8)ų, D_x = 1.468 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0417 and 0.0825, respectively, for all 5185 independent reflections. The molecule has a linear chain with an alternating arrangement of Rh₂(C₆H₅CO₂)₄ [Rh-Rh 2.4062(11)Å, 2.4110(11)Å] and dabco. The adsorption property was confirmed for N₂ gas with a specific surface area of 387.8 m² g^-1 estimated from an N₂ adsorption isotherm.

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The title compound is synthesized and characterized using spectral studies and an X-ray diffraction method. It belongs to the monoclinic crystal system with space group P2₁/c, and cell parameters a = 16.184(7)Å, b = 8.5876(13)Å, c = 15.0540(7)Å, β = 114.510(12)° and Z = 4. The molecules are connected by C-H…F and C-H…O hydrogen bonds. In addition, short contacts of the type C-F…π are observed.

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The crystal structure of 2,6-di(ethylurea)pyridine, determined by X-ray diffraction methods, crystallizes in a monoclinic space group, P2₁/c, with the following unit cell parameters: a = 12.6800(5)Å, b = 8.1730(5)Å, c = 12.9490(9)Å, β = 93.602(2)°, V = 1339.30(13)ų and Z = 4. The structure is stabilized by N-H…O, N-H…N, and C-H…O hydrogen bonds. The alteration of alkyl chain length contributes to the formation of different intriguing layered structure, and a slight influence on the hydrogen-bonding network.

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