A novel three-dimensional coordination polymer [Cd2(C3H2O4)2(H2O)2(μ 2-hmt)] n (hmt = hexamethylenetetramine): synthesis and crystal structure

The self-assembly of the Cd^II ion, hexamethylenetetramine (hmt) and malonate ligand yields a three-dimensional (3D) coordination polymer [Cd₂(C₃H₂O₄)₂(H₂O)₂( ₂-hmt)] _n with channels. The Cd^II ion is located in a octahedral coordination environment, composed of four oxygen atoms from three malonates, one oxygen atom of water and one nitrogen atom of hmt. Two oxygen atoms of each malonate coordinate to the same Cd^II ion and the other two oxygen atoms connect to adjacent two Cd^II ions respectively to form a two-dimensional infinite network, these networks are bridged by ₂-hmt coordinated to Cd^II ions to product a 3D architecture.     

Synthesis and Crystal Structure of Mixed-Ligand Ni(II) Complex of N-(1-Phenyl-3-methyl-4-benzylidene-5-pyrazolone) p-Nitrobezoylhydrazide and Pyridine

A novel mixed-ligand nickel complex, [Ni(PMBP—PNH) (Py)₃], [PMBP—PNH=N-(1-phenyl-3-methyl-4-benzylidene-5-pyrazolone) p-nitrobezoylhydrazide; Py = pyridine], has been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectrum, thermal analysis, and single-crystal X-ray diffraction. The X-ray diffraction reveals that the nickel (II) ion in the title complex is in a slightly distorted octahedral arrangement of the ONO donor atoms of primary ligand PMBP-PNH and three N-donor atoms in the secondary ligand pyridine.     

Crystal structures of the complexes of rare earth picrates with N, N, N′, N′-tetraphenyl-3, 6-dioxaoctanediamide

The complexes of rare earth picrate with N, N, N′, N′-tetraphenyl-3, 6-dioxaoctanediamide (TDD), [Eu(pic)₃(TDD)]-2CH₃CN and [Y(pic)₃(TDD)], have been synthesized. The crystal structures reveal that TDD acts as a tetradentate ligand, forming a ring-like coordination structure with its oxygen atoms together with one oxygen atom of the bidentate picrate. In the Eu (III) complex, the europium ion with a larger ionic radius lies out of the ring, while in the Y (III) complex, the yttrium ion with a smaller ionic radius enters the cavity of the ligand. The structures of the complexes are greatly affected by the ionic radii due to participation of the picrates in coordination. Project supported by the National Natural Science Foundation of China, the Doctoral Foundation of the State Education Commission of China, and the Climb Plan Foundation of the State Science and Technology Commission of China.     

三核苯甲酸铁配合物[Fe3O(OBZ)6(H2O)3](NO3)(acetone)5(OBZ-=苯甲酸根)的结构和磁性

合成了三核苯甲酸铁配合物［Ｆｅ３Ｏ（ＯＢＺ）６（Ｈ２Ｏ）３］（ＮＯ３）（ａｃｅｔｏｎｅ）５。测定了其晶体结构，其中三个铁形成等边三角形结构。配合物的变温磁化率表明，分子内三个铁之间有弱的反应磁性交换作用，Ｊ＝－３３．１８ｃｍ＾－１。分子之间则有更弱的反铁磁性交换作用，ＺＪ＾＇＝－１．１４ｃｍ＾－１。     

含能配合物[Zn(CHZ)3](C1O4)2的晶体结构、热行为及感度性能研究

通过碳酰肼水溶液与高氯酸锌水溶液反应制得含能配合物[zn(cHZ)3](CIO4)2.培养获得了配合物的单晶,用x射线单晶衍射法测定了晶体结构,该晶体属于单斜晶系、P2(1)/n空间群,晶胞参数a=1.0005(2)nm,b=0.8428(1)nm,c=2.1218(4)nm,β=100.948(3)°,y=1.756...     

Facile optical resolution of tert-butanethiosulfinate by molecular complexation with (R)-BINOL and study of chiral discrimination of the diastereomeric complexes

An important synthon, tert-butanethiosulfinate (2), has been effectively resolved by forming molecular complexes with (R)-2,2'-dihydroxy-1,1'-binaphthyl (BINOL, 3) in high enantioselectivity (>99 % ee). The present procedure represents the first example of the resolution of thiosulfinate. The mechanism of chiral discrimination is discussed in terms of molecular recognition based on IR and Xray analyses of the diastereomeric complexes during the resolution. In the less-soluble complex, (R)-3 and (R)-2 self-assembled as a linear supramolecule; however, in the more-soluble complex, (R)-3 and (S)-2 formed a simple bimolecular complex by one stronger hydrogen bond. Hydrogen bonding is the major driving force for effective resolution.     

Synthesis and Structure Investigation of a Novel 3-Dimensional Potassium Supermolecular Compound Based on 2,4-Dinitro Resorcinol

A novel 3‐dimensional potassium supermolecular compound [K(HDNR)(H₂DNR)(H₂O)]_n (H₂DNR?2,4‐dinitro resorcinol) was synthesized and characterized by elemental analysis and FT‐IR spectroscopy. The crystal structure investigated by X‐ray single crystal diffraction shows that [K(HDNR)(H₂DNR)(H₂O)]_n crystallizes with a monoclinic unit cell in the space group P2(1)/c with unit cell dimensions of a=17.648(5) Å, b=12.527(3) Å, c=7.735(2) Å, β=94.33(2)°, V=1705.00(73) ų, Z=4. The structure was refined to the final R=0.0670 and wR=0.0722 for 2022 observed reflections with I>2σ(I). In the compound, potassium cation is assembled into one‐dimensional chains along c‐axis through oxygen atoms from water molecules, and the chains were connected by the bridged HDNR^? anions to form a two‐dimensional net structure. The two‐dimensional nets constructed a three‐dimensional supramolecular architecture via intermolecular hydrogen bonds and N–O···π interaction. Density functional theory (DFT) B3LYP was employed to optimize the structure and calculate energies for three tautomers of HDNR^? univalent anion. Three stable tautomers were located. It was found that the structure (I) with O(1) losing hydrogen atom is more stable than the structure (II) also with O(1) losing hydrogen atom and the structure (III) with O(4) losing hydrogen atom.     

Synthesis of homoleptic lanthanide amides and the crystal structure of [Li(THF)4][Y(NPh2)4]

Anhydrous LnCl₃ reacted with three equivalents of LiNPh₂ in THF to give the unexpected homoleptic lanthanide amides [Li(THF)₄][Ln(NPh₂)₄] (Ln = Sm (1), Y (2)) in high yield. The crystal structure of complex 2 has been determined by X-ray diffraction methods. It crystallizes in the orthorhombic space group Pbcn with a = 17.522(3) Å, b = 16.321(3) Å, c = 19.947(3) Å, V = 5704.4(17) ų, and D _calc = 1.231 mg/m³ for Z = 4. Complex 2 is composed of discrete [Li(THF)₄]⁺ cations and [Y(NPh₂)₄]^– anions, both of which have crystallographically imposed two-fold symmetry. To achieve steric saturation of the metal center, there are interactions between the yttrium atom and one -carbon atom of each amide ligand. The yttrium and lithium atoms both exhibit distorted tetrahedral coordination geometry.     

The crystal and computed structures of 1,2,4‐triazol‐5‐one (TO)

1,2,4‐Triazol‐5‐one (TO) was synthesized by reacting semicarbazide hydrochloride with formic acid and its single crystal was grown by the slow evaporation method. Its molecular structure and crystal structure were determined by X‐ray single crystal diffraction technique. The obtained results show that the crystal belongs to Crystal system of Monoclinic, space group Pn. It was characterized by elemental microanalysis and FT‐IR techniques. Based on the crystal data, we had also carried quantum chemistry calculations on the title compound using the B3LYP and MP2 method with cc‐pVTZ basis set. The calculation results further demonstrate the crystal structure of title compound and its other related properties.     

含吡唑啉酮酰肼类衍生物的合成与结构

报道了PMBP-NTH(NTH为烟酰肼)与PMBP-PAH(PAH为对甲氧基苯甲酰肼)的合成、表征和晶体结构分析,PMBP-NTH晶体属三斜晶系,具有P1空间群,a=0.9024(2)nm,b=1.0953(2)nm,c=1.1635(2)nm,α67.070(10)°,β=68.220(10)°,γ=84.770(10)°,V=0.9816(3)nm^3,Z=2,Dc=1.345g/cm^3,μ=0.090mm^-1,F(000)=416,R=0.0363,ωR=0.0870.PMBP-PAH属单斜晶系,具有P21/c空间群,a=1.2715(4)nm,b=0.91710(10)nm,c=1.8979(3)nm,β=106.890(10)°,V=2.1177(8)nm^3,Z=4,Dc=1.338g/cm^3,μ=0.090mm^-1,F(000)=896,R=0.0414,ωR=0.0972.这两个化合物在分子内都形成了大的共轭体系,由于分子间氢键力的作用,又使它们在晶体中以二聚体形式存在.