Synthesis and crystal structure of a new zinc diphosphonate

A new zinc diphosphonate [NH₃CH(CH₃)CH₂NH₃]₂Zn₂(edbbp)₂(HNO₃)₂·4H₂O [eddbp?= O₃PCH(Ph)NH(CH₂)₂NHCH(Ph)PO₃] was hydrothermally synthesized with Zn(NO₃)₂·6H₂O, ethane-1,2-diamino-N,N′-bis(benzylphosphonic acid) (H₄edbbp) and 1,2-propyldiamine. It consists of a centro-symmetric dimeric unit [Zn₂(edbbp)₂], in which each zinc ion adopts a distorted square-pyramidal coordination geometry. Hydrogen bonds formed between phosphonate groups and protonated 1,2-propyldiamine molecules link the dimeric units into one-dimensional chains. The doubly protonated 1,2-propyldiamine molecules serve not only as charge compensating counter ions, but also as bridging groups. Hydrogen-bonding interactions among the phosphonate oxygen atoms, water molecules, nitric acid molecules and protonated 1,2-propyldiamine result in the formation of a three-dimensional supramolecular network.     

Anion recognition by a disiloxane-1,3-diol in organic solvents

To explore the anion recognition ability of silanol derivatives, ESI-MS and ¹H NMR titrations of a 1,3-disiloxanediol 1 with anions were studied in CDCl₃ and MeCN-d₃. The results indicate that 1 showed strong binding to anions such as AcO⁻ and halides.     

Silver(Ⅱ) 5,10,15,20-tetra(ethoxycarbonyl) porphyrin:An unexpected six-coordinate linear assembled structure

A novel six-coordinated silver porphyrin linear assembly was observed in silver(II) 5,10,15,20-tetra(ethoxycarbonyl) porphyrin crystal.     

PM3 semiempirical study and its comparison with X-ray crystal structure of 2-methyl-4-(4-methoxyphenylazo)phenol

The crystal and molecular structure of 2-methyl-4-(4-methoxyphenylazo)phenol have been determined by X-ray single crystal diffraction technique. The compound crystallizes in the monoclinic space group P2₁/c with a=9.7763(8) Å, b=11.3966(8) Å, c=11.9531(8) Å and β=108.752(6)°. In addition to the molecular geometry from X-ray experiment, its optimized molecular structure has been obtained with the aid of PM3 semiempirical quantum mechanical method, and then the corresponding geometric parameters were compared with those of X-ray crystallography. To determine conformational flexibility and crystal packing effects on the molecules, molecular energy profile of the title compound was obtained with respect to two selected degrees of torsional freedom, which were varied from ?180° to +180° in steps of 10°. Crystal structure of the title compound is a fibroid structure constructed by C–H···O and O–H···N type intermolecular hydrogen bonds. The most favorable conformer of the title compound has been determined by the crystal packing effects and there is no steric hindrance during rotation around the selected torsion angles.     

Synthesis and crystal structure of diferrocenylmethoxyethylamine

The reaction of diethanolamine with diferrocenylmethyl carbonium (2) that was generated by diferrocenylmethanol (1) treated with BF₃ in CH₂Cl₂ provided the synthesis of title compound diferrocenylmethoxyethylamine (3). The structure of 3 was determined by the X-ray diffraction (XRD) with crystal data: monoclinic P2₁/n space group and a=5.8419(14) Å, b=13.572(3) Å, c=23.839(6) Å, α=90°, β=91.827(5)°, γ=90°, V=1889.2(8) Å³, Z=4, D _c =1.558 mg·m^?3, μ=1.548 mm^?1, F(000)=920. The intra- and inter-molecular H bonding modes in 3 were demonstrated both in molecular crystal structure and IR spectral characterization.     

Synthesis and crystal structure of two novel nickel (imidazole) complexes having hydrogen-bonded networks

Two nickel (imidazole) complexes, Ni(im)₆Cl₂·4H₂O (1) and Ni(im)₆(NO₃)₂ (2) (im=imidazole) have been synthesized and characterized by elemental analysis, IR, UV, TG and single crystal X-ray diffraction. 1 crystallizes in the triclinic space group P-1 with a=8.800(6) Å, b=9.081(6) Å, c=10.565(7) Å, =75.058(9)°, β=83.143(8)°, γ=61.722(8)°, V=718.3(8) Å³, Z=1 and R₁ (wR₂)=0.0469 (0.1497). 2 crystallizes in the trigonal space group R-3 with a=12.370(6) Å, b=12.370(6) Å, c=14.782(14) Å, =90.00°, β=90.00°, γ=120.00°, V=1959(2) Å³, Z=3 and R₁ (wR₂)=0.0358 (0.0955). 1 and 2 exhibit different supramolecular network due to their different counter anions and different hydrogen bonding connection. In compound 1, [Ni(im)₆]²⁺ cation and counter anions Cl⁻ alternatively array in an ABAB fashion via N–HCl hydrogen bonding. In compound 2, the plane of each NO₃²⁻ is almost parallel and each NO₃²⁻ connect three different [Ni(im)₆]²⁺ cations via N–HO hydrogen bonding.     

Synthesis, crystal structure and theoretical investigation of two infinite two-dimensional supra-molecular compounds

Two supra-molecular compounds: (1,1′-biphenyl)-4,4′-diammonium bis(3,5-dinitrobenzoate) (1) and 4,4′-methylene bis(benzenammonium) bis(3,5-dinitrobenzoate) monohydrate (2) were synthesized and characterized by IR spectrum, UV spectrum and element analysis. The single crystal structure analysis indicates that these compositions in two compounds are linked through N–HO and O–HO hydrogen bonds into infinite two-dimensional structure. Moreover, theoretical investigation was performed by using RHF/6-31G(d) method, and their stabilities, frontier molecular orbital composition and Mulliken charge distribution were discussed.     

Facile syntheses, structural characterizations, and isomerization of disiloxane-1,3-diols

In the hydrolysis reaction of dichlorosilanes having an intramolecular coordinating atom, dcisiloxane-1,3-diols, [(OH){o-(CH₃)₂NCH₂-C₆H₄}RSi]₂O(R=CH₂CH (1), C₆H₅ (2), o-(CH₃)₂NCH₂C₆H₄ (3), Me (4)), were obtained in high yields. The results of the crystal structure analyses of meso-2, rac-2a, rac-2b and 3 are reported. They showed strong intramolecular hydrogen bondings between the hydroxy group and the nitrogen atom. We have also found that the diastereomeric isomerization of meso-2 to rac-2 in CDCl₃ solvent containing moisture occurred to result in the 55:45 equilibrium mixtures of the isomers and vice versa.     

Synthesis, crystal structure, hydrogen bonding and spectroscopy of transition-metal complexes with the ligand (N,N′-bis(2-pyridylmethyl)-1,3-propanediamine)

Six mononuclear complexes are reported with the tetradentate ligand N,N′-bis(2-pyridylmethyl)-1,3-propanediamine, (abbreviated as pypn) i.e. [Cu(pypn)(ClO₄)₂](H₂O)_1/2 (1), [Fe(pypn)Cl₂](NO₃) (2), [Zn(pypn)Cl](ClO₄) (3), [Co(pypn)(NCS)₂](ClO₄) (4), [Co(pypn)(N₃)₂](ClO₄) (5), [Zn(pypn)(NCS)₂] (6). The synthesis and X-ray crystal structures of all six compounds and their spectroscopic properties are presented.The geometry of the Cu²⁺, Co³⁺, Zn²⁺, Fe³⁺ ions is essentially octahedrally based, with the mm conformation (for Cu) and m_sf conformations for the other 3 metal ions; in compound 3 the geometry around the Zn²⁺ is distorted trigonal bipyramidal. The stabilisation of the crystal lattices is maintained by interesting, relative strong hydrogen bonds.     

一个新的二氮六元杂环化合物的合成、结构及表征

二氮杂环化合物及其衍生物在配合物的自组装和生物无机等领域中具有诱人的研究前景,因而引起各国化学家的广泛关注．这类化合物的合成可以追溯到60年前,Buhle等首次合成了1,5-二氮环辛烷(DACO)．随后,其一系列衍生物也被合成出来,并应用于配位化学及相关领域的研     

Synthesis and Crystal Structure of a Complex of Melamine with Benzoic Acid

A new complex of melamine（MA） with benzoic acid（HBA） was prepared, affording [（HMA＋）（BA-）]-2H2O. Each HBA molecule is deprotonated and one triazine nitrogen atom of MA is protonated. The adjacent HMA＋ cations are related via an inverse center to form ribbons with a pair of N--H…N hydrogen bonds. COO- groups of BA- anions are hydrogen bonded to alternate sides of the （HMA＋）∞ ribbons to generate indention ID tapes, which are extended into a 3D structure via N--H…O- and N--H…OW hydrogen bonds and π-π stacking interactions. Predominant patterns of the hydrogen bond present in the complex are anion/water and amino/water tape structures. The hydrogen-bonding patterns consist of alternate 6, 10-membered rings sharing two edges. Infrared（IR） spectroscopy conforms that proton transfer has taken place in the complex.     

Benzamidinium acetylsalicylate: crystal structure of the first salt with acetylsalicylate anion

The first crystal structure of a non-coordinating acetylsalicylate anion containing salt was determined by X-ray crystallography. Benzamidinium acetylsalicylate crystallizes in the triclinic space group $ P\bar{1} The first crystal structure of a non-coordinating acetylsalicylate anion containing salt was determined by X-ray crystallography. Benzamidinium acetylsalicylate crystallizes in the triclinic space group (a = 9.8885(5), b = 10.2769(5), c = 15.2656(7) ?, α = 87.219(4), β = 78.261(4) and γ = 72.589(4) Z = 4, V = 1449.17(12) ?³, R1 = 0.0346 and wR2 = 0.0697). The structure comprises pairs of hydrogen bonded benzamidinium cations and acetylsalicylate anions connected into infinite chains through further N–H···O hydrogen bonds.     

Synthesis,crystal structure and magnetic property of an octacyanometalate-bridged complex

An octacyanometalate-bridged complex, [Ni(en)₂(H₂O)W(CN)₈][Ni(en)₃] · 2H₂O, has been prepared and characterized and the magnetic properties studied. The complex was characterized using IR, elemental analysis and UV-Vis. The magnetic susceptibility measured over the range 1.8–300 K shows antiferromagnetic interaction.     

Synthesis and structure of fluorosilicic acid compounds with 4-aminobenzoic acid and with 4-aminobenzenesulfonamide: The role of H-bonding in crystal structure formation

Preparation and characterization of the ammonium hexafluorosilicate salts, 2[R]⁺[SiF₆]²⁻ (R = 4-(aminosulfonyl)benzenammonium) (1), and 2[R]⁺[SiF₆]²⁻.4H₂O (R = 4-carboxybenzenammonium), (2), are described. These salts, prepared from the reaction of the 4-aminobenzenesulfonamide or the 4-aminobenzoic acid with fluorosilicic acid, were characterized by IR, mass spectrometry and X-ray diffraction. 1 and 2 crystallize in monoclinic crystal system (space group P2₁/c and P2₁/n, respectively), with Z = 2 in both cases. Compounds exhibit an extensive system of hydrogen bonding.     

Synthesis,Structures and Properties of Four Coordination Polymers Constructed from 5‐Nitroisophthalate and Benzimidazole Ligand

Four coordination polymers, [Cu(NIPH)(Bim)₂]_n ( 1 ), [Co(NIPH)(Bim)₂]_n ( 2 ), [Zn(NIPH)(Bim)]_n ( 3 ), and [Cd(NIPH)(Bim)(H₂O)]_n ( 4 ) (NIPH = 5‐nitroisophthalate and Bim = benzimidazole) have been synthesized and characterized by elemental analysis, IR, TGA and single‐crystal X‐ray diffraction. The crystal structural analyses reveal that 1 and 2 are composed of zig‐zag chains and straight line chains, respectively. 3 and 4 are constructed by double‐stranded loop‐like chains. All these chain‐like structures are finally packed into three‐dimensional networks through hydrogen bonds. Thermogravimetic analyses (TGA) of 1 – 4 and temperature‐dependent magnetic susceptibilities of 1 have been performed.     

Synthesis and crystal structure of two derivatives of benzodiazepines

Two benzodiazepine derivatives, C₂₃H₂₂N₂O (I), 2-methyl-8-methoxy-2,4-diphenyl-2,3-dihydro-1H-1,5-benzodiazepine, and C₂₂H₁₇N₃O₂Br₂ (II), 2-methyl-7-nitro-2,4-bis(4′-bromophenyl)-2,3-dihydro-1H-1,5-benzodiazepine, were studied by single crystal X-ray diffraction method. Compound (I) crystallizes in the monoclinic system, space group P2₁/c, a = 13.1703(17) Å, b = 11.1990(14) Å, c = 12.9093(16) Å, β = 107.831(2)°, V = 1812.6(3) ų, Z = 4. Compound (II) crystallizes in the monoclinic system, space group P2₁/n, a = 11.7345(12) Å, b = 12.7477(13) Å, c = 13.5965(14) Å, β = 95.221(2)°, V = 2025.4(4) ų, Z = 4. The molecules of (I) and (II) have T-shape form with the diazepine ring at the junction point. The seven membered central benzodiazepine ring in both structures adopt a twist-boat conformation. The crystal packing is stabilized by C-H…π (in I) and C-H…O (in II) interactions.     

Synthesis,structures, catalytic,and anticancer activities of some coordination compounds involving two new triazole derivatives

Five N-heterocyclic carboxylate-based coordination complexes, [Co(L¹)₂(H₂O)₂]·2H₂O (1), [Cd(L¹)₂(H₂O)₂]·2H₂O (2), [Co(L²)(H₂O)₃] (3), [Ni(L²)(H₂O)₃] (4), and [Cu₂(L²)₂(H₂O)₂] (5), have been synthesized and characterized by elemental analysis, IR spectroscopy, Powder X-ray diffraction, thermogravimetric analyses, and single-crystal X-ray crystallography, where HL¹ is 2-((5-amino-1H-1,2,4-triazol-3-yl)thio)acetic acid and H₂L² is 2-((5-amino-1-(carboxymethyl)-1H-1,2,4-triazol-3-yl)thio)acetic acid. In these complexes, the hydrogen bonds (H-bonds) play an important role in their packing structures. Complex 1 has nine H-bonds showing a 3-D sqc38 topology. Complex 2 has 17 H-bonds exhibiting a 3-D hxl network. Complexes 3 and 4 are isomorphic, both of which possess ten H-bonds to present a 3-D btc topology. Complex 5 with eight H-bonds forms a 2-D sq1 structure. In addition, complex 3 catalyzes the decolorization of methyl orange. Meanwhile, 1, 3, and 5 show certain anticancer activities to inhibit the growth of HepG2 cells.     

Synthesis,crystal structure,and fluorescence properties of several schiff-base compounds

Two new Schiff-base compounds, 1,6-bis(4-dimethylaminobenzyl)-2,5-diaza-1,5-hexadiene (bdh), 1,4-bis(4-dimethylaminobenzyl)-2,3-diaza-1,3-butadiene (bdb), and a silver complex of the latter ([Ag₂(bdb)₃(NO₃)₂]·H₂O, 1) have been synthesized and characterized. The crystal structure of complex 1 was determined. 1 is a dinuclear complex, with the silver ions lying in coordination tetrahedra formed by two nitrogen atoms from the bdb ligands and two oxygen atoms from the nitrate anions. The fluorescence properties of bdh and bdb were studied; the fluorescence of bdb was quenched by the addition of silver ions, indicating that it is a potential fluorescent reagent for the analysis of silver.     

Synthesis, crystal structure, and electronic structure of RbVSe2

RbVSe₂ has been synthesized at 773 K through the reaction of V and Se with a Rb₂Se₃ reactive flux. The compound crystallizes in the orthorhombic space group D_2h²⁴-Fddd with 16 formula units in a cell of dimensions , , and at . The structure possesses infinite one-dimensional chains of edge-sharing VSe₄ tetrahedra separated from the Rb⁺ ions. These chains distort slightly to chains. The V-V distance within these chains is 2.8362(4) Å. First-principles total energy calculations indicate that a non-magnetic configuration for the V³⁺ cations is the most stable.