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)Å3, Dx = 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)Å3. 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)Å3, Dcalcd = 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)Å3. 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)Å3. 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 [NCP]P(O)[NP][NP] configuration where two angles, O=P–NP, are the largest ones at the P atom, while the NP–P–NP angle is the smallest one (NCP and NP 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)Å3, Dcalcd = 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)Å3, Dx = 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)Å3. 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].
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