The title compound, N,N′-bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2-ethanediamine, 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 C2/c with a = 17.319(3)Å, b = 9.7041(17)Å, c = 13.352(2)Å, β = 114.032(3)°, V = 2049.4(6)ų, D_x = 1.155 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0524 and 0.1629, respectively, for all 2432 independent reflections. The molecule is twisted at the ethylendiamine moiety of the ligand with a dihedral angle between the two phenolate planes of 13.58(7)°.

The compound of (Z)-1-[4-(trifluoromethyl)benzylidene]thiosemicarbazide crystallizes in the triclinic space group P1 and Z = 2 with cell parameters a = 7.0109(8)Å, b = 11.7862(13)Å, c = 14.9095(16)Å, α = 111.814(2)°, β = 91.720(2)°, γ = 101.036(2)° and V = 1115.7(2)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0438 and wR2 = 0.1078. In the crystal, each molecule is linked by intermolecular N–H···S hydrogen bonds.

A dinuclear nickel(II) complex with N,N′-disalicylidene-2,2′-(ethylenedioxy)bis(ethylamine) (H₂dee), [Ni₂(dee)₂(μ-H₂O)]·2EtOH (1), was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallizes in the monoclinic space group C2/c with a = 18.321(8), b = 13.543(6), c = 18.649(9)Å, β = 108.372(8)°, V = 4391(3)ų, D_calcd = 1.416 g/cm³, Z = 4. The R₁ [I > 2σ(I)] and wR2 (all data) values are 0.0347 and 0.0736, respectively, for all 5014 independent reflections. The complex is composed of a dinuclear molecule with di-μ-phenolato-bridges of dee²⁻ and the μ-aqua-bridge, and crystal ethanol molecules. The electronic spectral feature is consistent with the octahedral geometry of the nickel(II) ions.

A methanesulfonate salt of 3-(N-methyl)quinolinium boronic acid, [3-(N-Me)QnB(OH)₂]CH₃SO₃, was structurally determined by X-ray analysis. The boronic acid salt was crystalized as: P2₁/c, a = 8.57927(17), b = 6.99494(16), c = 21.0760(4)Å, β = 99.4787(19)°, Z = 4, V = 1247.53(4)ų. In the single crystal, hydrogen-bonded 1D-array structures of asymmetric cation-anion units were observed.

The crystal structure of the title complex, [Ru(pic)(bpy)₂]Cl·CH₃CN·1.5H₂O (pic = 2-picolinato; bpy = 2,2′-bipyridine), was determined by X-ray crystallography. Single crystals were obtained by the vapor diffusion of diethyl ether into an acetonitrile solution of [Ru(pic)(bpy)₂]Cl. The complex crystallized in a monoclinic system, and was characterized as: I2/a, a = 15.40850(14), b = 13.07370(14), c = 27.3830(3)Å, β = 98.0922(9)°, Z = 8, V = 5461.27(10)ų. The R1 and wR2 values were 0.0267 and 0.0714, respectively, for 5008 reflections.

The crystal structure of the title compound, (C₁₇H₂₈N)[Ni(dmit)₂] (dmit = 2-thioxo-1,3-dithiole-4,5-dithiolato, C₃S₅²⁻) is characterized by its unusually bent molecular structure in which two ligands, C₃S₅²⁻ in [Ni(dmit)₂]⁻, have a gradient of 19.01(6)° to one another, and [Ni(dmit)₂]⁻ anions are found to form a one-dimensional network in the direction of the a axis by intermolecular S–S contacts between the adjoining anions located almost vertically. Among these vertically arranged anions, the dihedral angle between the adjacent planes of the anions (S–S–Ni–S–S) is 69.51(2)°.

The crystal structure of CCl₃C(O)NHP(O)[(R)-(+)-NHCH(CH₃)(C₆H₅)]₂·0.25H₂O has been determined; it belongs to the chiral space group P1. In all four phosphoric triamide molecules of the asymmetric unit, the P atom has a distorted tetrahedral [N_CP]P(O)[N_P][N_P] configuration where two angles, O=P–N_P, are the largest ones at the P atom, while the N_P–P–N_P angle is the smallest one (N_CP and N_P denote the nitrogen atoms of the C(O)NHP(O) part and the two other nitrogen atoms bonded to phosphorus, respectively). In the crystal structure, two symmetry-independent one-dimensional chains extended along the b axis can be distinguished, each composed of alternating two symmetry independent phosphoric triamide molecules connected through N–H···O interactions. The chains are interconnected through hydrogen bonds of water molecules, and the resulting assembly is a ribbon running along the b axis.

The di-μ-phenolato-μ-methanol-bridged dinuclear nickel(II) complex with N,N′-disalicylidene-2,2′-(ethylenedioxy)bis(ethylamine) (H₂dee), [Ni₂(dee)₂(μ-CH₃OH)]·2CH₃OH, was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallizes in the monoclinic space group Cc with a = 18.157(2), b = 13.1691(17), c = 18.880(3)Å, β = 110.483(2)°, V = 4229.0(10)ų, D_calcd = 1.449 g/cm³, Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0532 and 0.1455, respectively, for all 7392 independent reflections. The temperature dependence of the magnetic susceptibility showed a ferromagnetic interaction between the two nickel(II) ions (g = 2.23, J = 6.50 cm⁻¹, D = 8.96 cm⁻¹, and Nα = 697 × 10⁻⁶ cm³ mol⁻¹ or g = 2.21, J = 7.27 cm⁻¹, D = –6.88 cm⁻¹, and Nα = 765 × 10⁻⁶ cm³ mol⁻¹).

The title complex of a six-coordinated (2,3,7,8,12,13,17,18-octaethylporphyrinato)iron(III) complex with two 4-methylpyridine N-oxides, [Fe(OEP)(4-MePyNO)₂]BF₄ (BF₄: tetrafluoroborate), was isolated, and the crystal structure was determined by the single-crystal X-ray diffraction method at 100(2)K. It crystallizes in the triclinic space group P-1 with a = 7.9064(2)Å, b = 13.7091(4)Å, c = 20.7535(6)Å, α = 90.870(2)°, β = 92.579(2)°, γ = 93.419(2)°V = 2242.83(11)ų, D_x = 1.323 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0517 and 0.1167, respectively, for all 10829 independent reflections. The average Fe–N and Fe–O distances are 2.045(2)Å and 2.093(1)Å. The porphyrin ring is a perfectly planar structure. We will determine the magnetic behaviors by SQUID and ESR measurements.

A tetracoordinate organoboron coordination compound dimethylformamide-triphenylborane complex (DMF-BPh₃) was prepared, and characterized by single-crystal X-ray method. The compound crystallized in the orthorhombic space group Pna2₁ and Z = 4 with cell parameters a = 16.6818(12)Å, b = 11.5428(8)Å, c = 9.2234(6)Å, V = 1776.0(2)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values were 0.042 and 0.1020, respectively, for all 4299 independent reflections. Three phenyl groups and one dimethylformamide (DMF) bound to the central boron atom, forming a tetrahedral geometry. The B–O(DMF) distance [1.601(3)Å] was found to be shorter than the B–C distances [1.616(3) – 1.626(3)Å].

A tetranuclear nickel(II) complex with 1-acetylacetoneimine-3-salicylideneamino-2-propanol (H₃asp), [Ni₄(asp)₂(CH₃O)₂(CH₃OH)₂], was synthesized, and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the monoclinic space group P2₁/c with a = 12.154(3)Å, b = 11.821(3)Å, c = 15.945(4)Å, β = 112.214(3)°, V = 2120.9(9)ų, D_x = 1.421 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0363 and 0.1022, respectively, for all 5069 independent reflections. The complex has a centrosymmetric di-μ₃-methoxido-di-μ-alkoxido-di-μ-phenoxido-bridged tetranuclear nickel(II) structure with a defective double-cubane core, having two octahedral Ni and two five-coordinate Ni atoms with two unsymmetrical Schiff-base ligands and two methanol molecules. The temperature dependence of the magnetic susceptibility showed a ferromagnetic interaction between the nickel(II) ions. The spectral and magnetic properties are consistent with the crystal structure.

A crystal of trisaccharide, β-D-galactopyranosyl-(1↔6)-β-D-fructofuranosyl-(2↔1)-2-acetamido-2-deoxy-α-D-glucopyranoside, was prepared and its crystal structure was determined at the orthorhombic space group P2₁2₁2₁ with cell parameters a = 8.7221(2), b = 9.6970(3), c = 31.8548(10)Å, Z = 4. A bent structure was observed, where β-D-galactopyranoside and 2-acetamido-2-deoxy-α-D-glucopyranoside rings made close contacts.

A μ-dioxido-bridged dinuclear oxidomolybdenum(V) complex with 2(2-aminoethyl)aminoethanethiol (Haeaet), [(MoO)₂O₂(aeaet)₂], was prepared. 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 = 13.975(3)Å, b = 12.475(3)Å, c = 12.158(3)Å, β = 100.091(4)°, V = 2086.8(8)ų, D_x = 1.573 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0373 and 0.0975, respectively, for all 2384 independent reflections. The two molybdenum atoms are bridged by two oxido-O atoms in a distorted octahedral geometry with oxido-O and facial NNS-donor atoms of aeaet⁻. The DFT calculation showed that the absorption bands at 228, 332, and 461 nm in the UV-vis spectra can be ascribed to LMCT bands from S(3p) to Mo(4d).

The X-ray crystal structure of N-(7-{[2-(dimethylamino)ethyl]amino}-1-methyl-2-oxo-1,2-dihydro-1,6-naphthyridin-3-yl)-3,4,5-trimethoxybenzamide, a potential anticancer agent targeting Hsp90, was established. It crystallizes in the triclinic space group P-1 with cell parameters a = 9.3554(4)Å, b = 11.4450(5)Å, c = 11.5629(4)Å, α = 87.140(2), β = 78.8070(19), γ = 69.2119(19), V = 1135.21(8)ų and Z = 2. The crystal structure was refined to final values of R1 = 0.0492 and wR2 = 0.1386. An X-ray crystal structure analysis revealed that each molecule features intermolecular N–H···N hydrogen bonds to form dimers.

A nickel(II) complex with α-(2-hydroxy-3-salicylideneaminopropyl)iminopropionic acid (H₃hsaip), [Ni(Hhsaip)], was isolated, and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the monoclinic space group P2₁/c with a = 9.364(3)Å, b = 17.725(5)Å, c = 7.753(2)Å, β = 105.004(5)°, V = 1242.8(6)ų, D_x = 1.715 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0601 and 0.1444, respectively, for all 2950 independent reflections. The complex is a mononuclear nickel(II) complex with Hhsaip, which was derived from the degradation of 1-acetylacetoneimine-3-salicylideneamino-2-propanol, having a square-planar geometry. In the crystal, the nickel atom is close to the neighboring molecule’s one with a distance of 3.265(1)Å. A DFT calculation suggested that the S = 0 state without metal–metal bonding is more stable compared with an S = 1 state with the metal–metal bonding.

The title complex of a six-coordinated [5,10,15,20-tetrakis(2,4,6-trimethylphenyl)-porphyrinato-k⁴N]iron(III) complex with two 3,5-dimethylpyridine N-oxides, [Fe(TMP)(3,5-Me₂PyNO)₂]ClO₄ (ClO₄: perchlorate), was prepared, and characterized by a single-crystal X-ray diffraction method at 100(2)K. The title complex crystallizes in the triclinic space group P-1 with a = 15.2889(4)Å, b = 15.8587(4)Å, c = 16.2403(5)Å, α = 84.596(2)°, β = 63.769(3)°, γ = 84.162(2)°, V = 3508.49(19)ų, D_x = 1.345 g/cm³, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0628 and 0.1517, respectively, for all 16923 independent reflections. The average Fe–N and Fe–O distances are 2.041(3)Å and 2.033(3)Å. The porphyrin ring is a completely planar structure. We will determine the magnetic behaviors by SQUID and ESR measurements.

The structure of 4-(bis(4-hydroxy-2-oxo-2H-chromen-3-yl)methyl)benzoic acid (1) was determined by X-ray crystallography. Compound 1 · THF crystallizes in the monoclinic system, space group P2₁/n (#14) with cell parameters a = 10.676(2)Å, b = 10.017(2)Å, c = 24.438(6)Å, β = 100.890(10)°, V = 2566.4(10)ų and Z = 4. The molecular configuration/conformation is stabilized by two intramolecular hydrogen bonds formed between the carbonyl group of one 4-hydroxycoumarin unit and the hydroxyl group of the second one and the opposite (C=O···H–O).

The title compound, C₉H₁₂N₂S₃, was obtained from a condensation reaction between S-methyldithiocarbazate and 1-(2-thienyl)-1-propane. The compound crystallized in the monoclinic space group P2₁/n with cell parameters a = 10.178(3), b = 13.357(4), c = 8.845(3)Å, β =98.613(5)°, Z = 4 and V = 1188.9(6)ų. The compound was nearly planar with intermolecular N–H···S hydrogen bonding observed in the crystal lattice.

A nickel(II) complex with 1,3-bis(pyrrole-2-methylideneamino)-2-propanol (H₃bpmp), [Ni(Hbpmp)]·0.5CH₃OH, was prepared, and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the triclinic space group P1 with a = 9.6947(12)Å, b = 12.0269(15)Å, c = 13.2626(18)Å, α = 94.036(2)°, β = 108.801(2)°, γ = 104.820(2)°, V = 1395.3(3)ų, D_x = 1.509 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0401 and 0.0955, respectively, for all 6384 independent reflections. The complex is a mononuclear nickel(II) complex with Hbpmp, having a square-planar geometry. The spectral feature is consistent with the crystal structure.

A crystal of disaccharide, β-D-fructofuranosyl-[2↔1]-6-amido-6-deoxy-α-D-glucopyranoside, was prepared and its crystal structure was determined at the triclinic space group P1 with cell parameters a = 6.9140(5), b = 7.7202(5), c = 8.7383(7)Å, Z = 1, R1 [I > 2σ(I)] = 0.0235, wR2 (all data) = 0.0645. In comparison with the crystal structure of sucrose, the configuration around the glycosidic bond is similar.

A dinuclear Cu(II) complex, [Cu₂(OAc)₂(BF₄)(tphn)(H₂O)]BF₄·CH₂Cl₂ [tphn = N,N,N′,N′-tetrakis(2-pyridylmethyl)-1,6-hexanediamine], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in the monoclinic space group P2₁/c with a = 8.4305(16), b = 27.302(5), c = 19.131(4)Å, β = 102.724(2)°, V = 4295.2(14)ų, D_calcd = 1.550 g/cm³, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0694 and 0.1976, respectively, for all 9131 independent reflections. The complex contains two square pyramidal Cu(II) ions that are bound to both terminal tridentate sites of tphn.

A copper(II) complex with 1,3-bis(pyrrole-2-methylideneamino)-2-propanol (H₃bpmp), [Cu(Hbpmp)]·0.5C₂H₅OH, was prepared, and the crystal structure at 293 K was elucidated by the single-crystal X-ray diffraction method. The complex crystallized in the monolinic space group C2/c with a = 17.975(2)Å, b = 18.894(2)Å, c = 9.2081(11)Å, β = 113.728(2)°, V = 2863.0(6)ų, D_m = 1.48 g/cm³, D_c = 1.526 g/cm³, and Z = 8. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0320 and 0.0991, respectively, for all 3378 independent reflections. The complex is essentially a square-planar copper(II) complex with partially deprotonated Hbpmp²⁻; this mononuclear unit is loosely connected by the axial semi-coordination of the alcohol group of the Hbpmp²⁻ ligand of the neighboring mononuclear unit to form a dinuclear assembly. The temperature dependence of the magnetic susceptibility (4.5 – 300 K) follows the Curie–Weiss law with θ = –1.2 K, showing a weak antiferromagnetic interaction between the copper(II) ions, consistent with the crystal structure.

The structure of the bis[bis(p-methoxyphenyl)glyoximato]nickel(II) complex was determined by X-ray crystallography. The symmetry operation (–x+1, –y, –z+0.5) generates the whole molecule. The compound crystallizes in a monoclinic system, which was characterized as follows: C2/c, a = 17.6548(12), b = 19.0788(13), c = 9.2011(9)Å, β = 103.547(2)°, Z = 4, V = 3013.0(4)ų. The crystal structure was solved using a dual-space algorithm and refined by a full-matrix least-squares method on F² to final values of R₁ = 0.0683 and wR₂ = 0.1454. The para-methoxy group substitution brings about a molecular cuboid stemming from Ni(II)···π contact and moderate hydrogen bonding, instead of Ni–Ni interactions.

The structure of 2,2′-(((2,2-dimethylpropane-1,3-diyl)bis(azanylylidene))bis(methanylylidene))bis(4-methoxyphenol)palladium(II) was determined by X-ray crystallography analysis. It crystallizes in the space group P2₁/n, with cell parameter a = 12.5115(7)Å, b = 10.5337(6)Å, c = 15.0080(9)Å, β = 94.0547(19)°, Z = 4, and V = 1973.0(2)ų. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F² to final values of R1 = 0.0415 and wR2 = 0.1251. The Schiff-base ligand was found to coordinate to the palladium(II) through tetradentate ONNO atoms forming a slightly distorted square-planar complex. Two intermolecular hydrogen bonds, C–H···O, stabilized two molecules forming dimers.

A dinuclar magnesium(II) complex, [Mg₂(sym-hcp)₂](BPh₄)₂·2acetone·2H₂O, was synthesized with a dinucleating ligand, 4-chloro-2,6-bis[(2-hydroxyethyl)methylaminomethyl]phenolate [(sym-hcp)⁻], and characterized by a single-crystal X-ray method. The compound crystallized in the monoclinic space group C2/c and Z = 4 with cell parameters a = 22.7667(13)Å, b = 19.1628(11)Å, c = 17.3218(10)Å, β = 96.1500(10)°, V = 7513.6(7)ų. The R₁ [I > 2σ(I)] and wR₂ (all data) values were 0.0418 and 0.1023, respectively, for all 8618 independent reflections. The analysis revealed a bis-μ-phenolato-dimagnesium(II) core structure containing two distorted octahedral magnesium(II) ions.