含潜在异构手性双臂配体的螺旋组装和手性聚集

采用具有潜在异构手性的双臂配体，双吡啶二甲基联苯-2，2′-二酰肼，合成了4个双核螺旋配合物。配体与CdI₂和Cu(NO₃)₂反应得到双核单螺旋化合物1和2，在化合物2中，由于C-H…π和π…π的协同相互作用沿ab面形成单一手性的二维平面。双核双螺旋化合物3(Ni(Ⅱ))和4(Co(Ⅱ))中的金属中心表现相同的绝对构型，说明含异构手性的配体能够把金属中心的手性从一个中心传递到另一个中心。     

Synthesis and Crystal Structure of a Mo-S Cluster Compound Coordinated by Isonicotinate

A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophospha- te, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345(2), b = 13.7805(2), c = 14.5400(1) , α = 107.078(1), β = 113.380(1), γ = 96.310(1)o, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75(5) 3, Z = 2, Dc = 1.748 g/cm3, μ = 1.399, F(000) = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections (I > 2σ(I)). 31P NMR spectrum has been measured with the resonance 110.050 and 108.783 (2:1).     

Synthesis and Crystal Structure of 4-[（1E）-（4-Hydroxy-3,5-dimethoxybenzylidene）-amino]-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

The title compound (C20H21N3O4, Mr = 367.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 7.5143(15), b = 13.901(3), c = 18.545(4) , V = 1937.1(7) 3, Z = 4, Dc = 1.260 g/cm3, μ = 0.089 mm-1, F(000) = 776, the final R = 0.0616 and wR = 0.0912. X-ray diffraction reveals that the molecule adopts an E configuration about the central C=N double bond. The intermolecular O–H…O hydrogen bond stabilizes the crystal structure by causing the formation of a supramolecular architecture.     

Synthesis and Crystal Structure of 3-Phenyi- 6-（4-methylphenyi）-1,2,4-triazolo[4,3-b]-1,2,4-triazine

1 INTRODUCTION The fused heterocycles bearing 1,2,4-triazine have attracted considerable attention in recent years owing to their biological and pharmaceutical activi- ties[1～3]. The 1,2,4-triazine core is a versatile synthe- tic platform to access a wide range of condensed heterocyclic ring systems via inter- and intramolecu- lar Diels-Alder reaction with a vast array of dieno- philes[4～6]. IBD (iodobenzene diacetate) is commer- cially available and used as benign non-metallic oxidant…     

Synthesis and Crystal Structure of a 2-D Hydrogen-bonded Supramolecular Network {[Cu4(OH)4(2,2''-bpy)4(bqdc)]·2ClO4}n

The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquinoline-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P-1 with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) (A), α= 80.0480(10), β= 87.7900(10), γ = 74.0800(1)°, V = 1423.65(16) (A)3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm3, μ = 1.651 mm-1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with Ⅰ＞ 2σ(Ⅰ). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]4 are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .     

Synthesis and Crystal Structure of (E)-Ethyl 3-Keto-18β-glycyrrhetinate 3-Oxime

A novel derivative of glycyrrhetinic acid, (E)-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 (Mr = 511.72), was synthesized and structurally characterized by IR, 1H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897(12), b = 7.3190(7), c = 15.9944(14) , β = 94.833(2)o, V = 1456.9(2) 3, Z = 2, Dc = 1.167 g/cm3, μ = 0.075 mm-1, F(000) = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent (Rint = 0.0199) and 2605 were observed with I > 2σ(I). There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H2O)3}·2H2O]n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc=5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a=9.599(3), b=18.699(5), c=7.557(2) (A), β= 108.198(4)°, V=1288.6(6) (A)3, Z=4, Mr=382.60, Dc=1.972 g/cm3, F(000)=760, μ=1.740, the final R=0.0555 and wR=0.0995 for 1732 observed reflections with Ⅰ ＞ 2σ(Ⅰ). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Syntheses and(Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)2Cl]·ClO4 and [Zn(bipy)2Cl]·BF4

Two new transition metal complexes, [Ni(bipy)2Cl]·ClO4 (bipy = 2,2'-bipyridine) 1 and [Zn(bipy)2Cl]·BF4 2, have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 crystallize in monoclinic space group P21/n with Z = 4. For 1, a = 10.776(1), b = 12.067(1), c = 16.146(2)(A), β= 93.021(2)o, V = 2031.9(4)(A)3, Mr = 505.98, Dc = 1.654 g/cm3, μ = 1.255 mm-1, F(000) = 1032, the final R = 0.0406 and wR = 0.1002 for 3983 observed reflections with Ⅰ ＞ 2σ(I). For 2, a = 10.758(4), b = 12.058(4), c = 16.135(5) (A), β = 104.57(1)o, V = 2025.7(12) (A)3, Mr = 500.00, Dc = 1.639 g/cm3, μ = 1.396 mm-1, F(000) = 1008, the final R = 0.0470 and wR = 0.1237 for 3759 observed reflections with Ⅰ ＞ 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. A one-dimen- sional zigzag double hydrogen-bonding-chain is generated by the intermolecular M-bipy …anion…bipy--M hydrogen bonding interactions between the chelating ligands of bipy and anion.     

Synthesis and Structural Characterization of Di(2-amino-5-methyl-1,8-naphthyridin-1- ium-7-carboxylato)dichlorocuprate(Ⅱ) Dihydrate

Di(2-amino-5-methyl-1,8-naphthyridin-1-ium-7-carboxylato)dichlorocuprate(Ⅱ) ditrated hydrochloride acid, and its structure was determined by X-ray diffraction at 298 K. The compound (C20H22Cl2CuN6O6, Mr = 576.88) crystallizes in monoclinic, space group P21/n with a =9.102(9), b = 12.150(12), c = 10.619(10) (A), β = 91.20°, V = 1174.1 (19) (A)3, Z = 2, Dc = 1.632 g/em3,F(000) = 590, μ = 1.208 mm- 1, R = 0.0392 and wR = 0.0984. The Cu2 ion is six-coordinated by two nitrogen and two oxygen atoms from two different naphthyridine ligands at the equatorial positions together with two chloride ions located at the axial positions.     

Synthesis and Crystal Structure of an Ionic Compound [Fe(CN)6(phCH2NC5H5)3]·(H2O)4

A novel ionic compound [Fe(CN)6(phCH2NC5H5)3]·(H2O)4(Mr = 794.71) has been synthesized and its structure was characterized by IR, elemental analysis and X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 10.837(2), b = 16.551(3), c = 23.402(5) (A), β = 97.531(4)°V = 4161.0(15)(A)3, Z = 4, Dc = 1.269 g/cm3, F(000) = 1668, μ = 0.414 mm-1, R = 0.0479 and wR = 0.1232. The building unit of the title compound consists of three (phCH2N C5H5) ions, one [Fe(CN)6]3- anion and four water molecules. According to the structural analysis, [Fe(CN)6]3- are linked together by O-H…N and O-H…O hydrogen bonds, but [Fe(CN)6]3- and [(phCH2N C5H5)3] ions are bound by electrostatic force to form an ionic compound.Keywords: N-benzyl-pyridine, ferricyanic anion, crystal structure, supramolecular, ionic compound.