Hydrothermal Synthesis and Crystal Structure of a Square Grid Coordination Copper(II) Polymer from 1,4-Bis(imidazole-1-ylmethyl)benzene

1INTRODUCTION The employment of transition metal ions and ap-propriate bridging ligands has become a dominant theme in the construction of some interesting ar-rays[1,2],especially for the large square grid net-works.Recently,considerable research effort has been focused on the studies of polymeric frame-works with the ligands based on imidazole.These polymers are of great interest not only due to their intriguing topologies but also the potential applications in ion exchange,magnetic and e…     

Synthesis and Structural Characterization of a New Cadmium(II) Complex with a Double Betaine

1 INTRODUCTION The construction of supramolecular aggregates has received much attention due to their intriguing network topologies and potential functions as new classes of materials[1, 2]. Multiple noncovalent interac- tions, such as hydrogen bonds, π-π stacking and host- guest ionic interactions, play important roles in the supramolecular assembly of metal ions and organic ligands[3, 4]. In this context the multidentate ligands with conjugated groups are employed as building blocks in…     

Synthesis and Crystal Structure of α-（1,2,4-Triazol-1H-yl）-ρ-chloro Acetophenone, [ClC6H4COCH2（C2H2N3）]

1 INTRODUCTION Triazole nuclei appear frequently in the struc- tures of various natural products and biologically active compounds, notably thiamine (vitamin B), penicillins, antibiotics such as micrococcin[1], and many metabolic products of fungi and primitive marine animals, including 2-(aminoalky)triazole-4- carboxylic acids[2]. Numerous triazole derivatives exhibit pharmacological activity[3], e.g., 4-amino-N- (triazole-2-yl)benzenesulfonamide is a commercial drug. We report herein …     

Disilver(I) rectangular-shaped metallacycles: X-ray crystal structure and dynamic behavior in solution

Reaction of the ditopic semirigid ligand 1,2-bis(imidazolylmethyl)benzene (1,2-bImb) or the flexible ligand 1,4-bis(2-benzimidazolyl)butane (C4BIm) with AgX (X = ClO4-, BF4-, CF3CO2-) afforded five new complexes, namely, [Ag2(1,2-bImb)2](ClO4)2 (1), [Ag2(1,2-bImb)2](BF4)2 (2), [Ag2(1,2-bImb)2](CF3CO2)2.2CH3OH (3.2CH3OH), [Ag2(C4BIm)2](ClO4)2.2DMF (4.2DMF), and [Ag2(C4BIm)2](CF3CO2)2.2H2O (5.2H2O), all of which contain a centrosymmetric, rectangular-shaped cationic disilver(I) metallacycle [Ag2(L)2]2+. In 1-3, a pair of 1,2-bImb ligands takes on the syn conformation to connect two Ag(I) ions to give a compressed rectangle with a transannular Ag...Ag separation of 3.27-3.36 angstroms, whereas in 4 and 5, the pair of planar C4BIm ligands acts in the cis conformation to connect two Ag(I) ions to yield a normal rectangle with a transannular Ag...Ag separation of 7.67-7.91 angstroms. The anions form Ag...O or Ag...F weak interactions in 1-3 and O-H...O or N-H...O hydrogen bonds in 4 and 5 in crystal packing but exhibit no significant influence on the formation of the disilver(I) macrocycles. The solution structure and dynamic behavior of the complexes studied by electrospray ionization mass spectrometry, 1H NMR, and variable-temperature NMR indicated that the dynamic equilibrium between the [Ag2(L)2]2+ cation and the open-ring oligomers or other potential species occurs via solvent-assisted dissociative exchange. The metal-ligand exchange barrier was estimated to be 54.5 kJ mol(-1).     

Synthesis and Crystal Structure of a New Lead Coordination Polymer： [Pb（L）（1,4-ndc）]

The title coordination polymer, [Pb(L)(1,4-ndc)] 1 (L = 2-(4-fluorophenyl)-1Himidazo[4,5f1,10]phenanthroline, 1,4-ndc = naphthalene-1,4-dicarboxylic acid), has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR and singlecrystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 10.1043(11), b = 14.3162(15), c = 17.6061(18), β = 95.3990(10)°, V = 2535.5(5)3, Z = 4, C31H17FN4O4Pb, Mr = 735.68, Dc = 1.927 g/cm3, F(000) = 1416, μ(MoKa) = 6.709 mm-1, R = 0.0201 and wR = 0.0489. The 1,4-ndc dianions link neighboring Pb(II) atoms in a bis-chelating mode, yielding a one-dimensional chain structure along the c axis. The C–H···π interactions between the carbon atom of L ligand and the benzene ring of 1,4-ndc lead the one-dimensional chains to form a two-dimensional supramolecular layer. The π-π interactions between L ligand and 1,4-ndc ligand make the two-dimensional layers generate a three-dimensional supramolecular architecture. Additionally, the N–H···O hydrogen bonds further stabilize the structure of 1.     

Metal carbonyl derivatives of 1,4-quinone and 1,4-hydroquinone

CpMoMn(CO)5(mu-S2), 1 reacts with 1,4-benzoquinone to yield CpMoMn(CO)5(mu-S2C6H2O2), 2 containing a 1,4-quinonedithiolato ligand formed by replacing two of the hydrogen atoms on one of the C-C double bonds of 1,4-benzoquinone with sulfur atoms from the disulfido ligand in 1. Compound 2 was reduced with hydrogen to yield CpMoMn(CO)5[mu-S2C6H2(OH)2], 3 which contains a 1,4-hydroquinonedithiolato ligand. Compound 3 was reoxidized to 2 with ferrocenium hexafluorophosphate.     

Hydrothermal Synthesis and Crystal Structure of a New 2D Mn（Ⅱ） Coordination Polymer with 4,4′-Sulfonyldi Benzoic Acid and 1,4-Bis（imidazol-1-ylmethyl）benzene Ligands

A novel manganese coordination polymer [Mn2(sfdb)2(biyb)2(H2O)2]n (1, H2sfdb=4,4′-sulfonyldibenzoic acid, biyb=1,4-bis(imidazol-1-ylmethyl)benze) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray determination, IR and thermogravimetric analysis (TGA). Complex 1 crystallizes in the triclinic system, space group P with a=10.138(4), b=11.187(5), c=13.582(6) γ, α=69.146(7), β=89.628(7), γ=77.076(7)°, Mn2C56H48N8O14S2, Mr=1231.02, V=1398.5(10) ·3, Dc=1.462 g/cm3, F(000)=634, μ=0.600 mm-1, S=1.088 and Z =1. The final refinement gave R=0.0570 and wR=0.1229 for 4889 observed reflections with I > 2σ(I). Interestingly, in complex 1, the sfdb2- and biyb ligands connect the Mn(II) ions into two-dimensional 2-fold interpenetrating layers, and such layers are further connected with each other to generate a 3D supramolecular structure through hydrogen bonding interaction.     

Halogenometallate von Übergangselementen mit Kationen stickstoffhaltiger heterocyclischer Basen. I. Die Kristallstrukturen von 1,4-Dimethylpiperazinium-tetrachlorocobaltat(II) und -zinkat(II), (dmpipzH2)[MIICl4] (M = Co,Zn)

Halogenometalates of Transition Elements with N-heterocyclic Base Cations. I. The Crystal Structures of 1,4-Dimethylpiperazinium Tetrachlorocobaltate(II) and -zincate(II), (dmpipzH₂)[M^IICl₄] (M = Co, Zn) The compounds (dmpipzH₂)[M^IICl₄] crystallize in the monoclinic space group P2₁/m with a = 6.133(1), b = 14.306(1), c = 6.902(1) Å, β = 90.54(2)°, Z = 2 for M = Co and with a = 6.141(1), b = 14.282(1), c = 6.907(1) Å, β = 90.60(2)°, Z = 2 for M = Zn. The structures consist of tetrahedra [MCl₄]^2? and centrosymmetric cations (dmpipzH₂)²⁺ in the chair form. Bifurcated hydrogen bridging bonds of the N? H …? Cl type connect the nitrogen atom to two chloride ions. Two short distances C …? Cl are interpreted in terms of C? H …?Cl hydrogen bridges.     

Structural and spectral investigation on the Co complexes with 1,4-diazacycloheptane (DACH) functionalized by heterocyclic pendants

A series of penta-coordinated Co^II complexes of 1,4-diazacycloheptane (DACH) functionalized by additional imidazole or pyridine donor pendants, [CoL¹Cl](ClO₄)·H₂O (1), [CoL²Cl](ClO₄) (2) and [CoL³Cl](ClO₄)·CH₃OH (3), where L¹=1,4-bis(imidazole-4-ylmethyl)-DACH, L²=1,4-bis(N-1-methylimidazol-2-ylmethyl)-DACH and L³=1,4-bis(pyridyl-2-ylmethyl)-DACH have been synthesized and characterized by elemental analyses, IR and UV–Vis spectra. In all the mononuclear complexes, each Co^II center is penta-coordinated to four nitrogen donors of the ligand and one axial chloride anion. The crystal structure of complex 2 has been determined by X-ray diffraction analysis, which forms a one-dimensional linear structure through inter-molecular C–HCl and C–HO hydrogen-bonding.     

Synthesis and Structural Characterization of a New Cadmium(Ⅱ) Complex with a Double Betaine

A new flexible double betaine L (L =1,4-bis(pyridinio-4-carboxylato-N-methyl)and its crystal structure was determined by single-crystal X-ray diffraction analysis.Crystallo13.7854(3), b = 14.2820(3), c = 14.9188(4)(。A), β = 116.418(1)°, V = 2630.5(1)(。A)3, Z = 4, Dc = 1.704g/cm3, μ(MoKα) = 0.911 mm-1, F(000) = 1368, the final R = 0.0315 and wR = 0.0768 for 3637observed reflections with I ＞ 2σ(I).In complex 1, L acts as a monodentate ligand to link a Cd(Ⅱ) ion in a novel coordination mode of double betaines.The mononuclear [Cd(H2O)4L(NO3)] units are connected through intermolecular hydrogen bonds and π-π stacking reactions to generate a 3D network.     

Synthesis and Crystal Structure of N,N''''-Diphenyl-3, 6-diethyl-1,4-dihydro-s-tetrazine-1,4-dicarbonamide

1INTRODUCTIONIthasbeenarousedmoreandmoreinterestsinces-tetrazinewasfirstsynthesizedbyHautgschin1900[1].Thesynthesisofdihydroderivativeof3,6-dimethyl-s-tetrazinewasreportedindetailbySkorianetz[2].UsingX-ray,Jennison[3]foundthat1,6-dihydro-s-tetrazinehashom…     

Synthesisand Crystal Structure of a Cu（II） Complex with Reduced Schiff-base N-（2-Hydroxybenzyl）-D,L-alanine and 4,4＇-Bipyridine

A new complex [Cu2(sala)2(H2O)2(4,4'-bipy)]·H2O (sala = N-(2-hydroxybenzyl)- D,L-alaninate, 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in monoclinic system, space group C2/c with a = 42.44(3), b = 10.416(8), c = 15.487(13), β = 97.455(14)o, C30H36Cu2N4O9, Mr = 723.71, V = 6789(9)3, Dc = 1.416 g/cm3, Z = 8, F(000) = 2992, μ(MoKα) = 1.308 mm-1, R = 0.0493 and wR = 0.1004 for 4878 observed reflections (I > 2σ(I)). Structural analysis shows that each copper(II) atom displays a distorted square-based pyramidal coordination geometry with two oxygen atoms and one nitrogen atom from one N-(2-hydroxybenzyl)-D,L-alaninate, one nitrogen atom from 4,4'-bipyridine ligand and one water molecule. 4,4'-Bipyridine ligand bridges two Cu(II) ions to form a dinuclear compound. The molecular structure is extended into a one-dimensional wavy chain through hydrogen bonds. These 1D chains are further expanded into 2D networks through hydrogen bonds.     

Synthesis and Crystal Structure of [Ca（DMF）6][Mo6Br8Cl6]

1INTRODUCTION Molybdenum(II)halide clusters containing[Mo6-X8]4 cores have been the subject of interest for over five decades[1].This octahedral cluster-type comple-xes comprise an important,and in a sense archetypal,class of higher nuclearity transition metal cluster com-plexes.Their high symmetry,photochemical and pho-tophysical properties as well as structural relation-ships to cluster complexes of other elements exhibit significant interest[2].In addition,there is a structural simila…     

Synthesis, Crystal Structure and Electrochemistry Properties of a (N,N'-Ethylene-bis(salicylaldiminato)) Nickel(II) Complex, [Ni_2(salen)_2]·NCS·NH_4

A new Ni(II) complex [Ni2(salen)2]·(NCS)·NH4 (salen = N,N’-bis(salicylidenea- mino)ethanato) has been prepared and structurally characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a = 16.8725(13), b = 19.0046(15), c = 20.0583(16) , Z = 8, V = 6431.8(9) 3, C33H32N6Ni2O4S1, Mr = 726.13, Dc = 1.500 g/cm3, F(000) = 3008, μ = 1.284 mm-1, the final R = 0.0394 and wR = 0.0767 for 4449 observed reflections with I > 2σ(I). The complex involves a N,N’-ethylene-bis(salicylaldiminato) Schiff base, an isothiocyanato anion and an ammonium cation. The nickle(II) ion adopts a distorted square coordination geometry with N2O2 set of Schiff base ligand. The complexes are linked into a dimmer via intermolecular hydrogen bonds and the [Ni(salen)] moieties are connected together to form a 2-D layer structure by intermolecular N–H…O hydrogen bonds and π-π stacking. Cyclic-voltammetry method was used to characterize electrochemically the complex.     

Syntheses and Crystal Structures of Two Coordination Polymers with Aromatic Dioxide as Bridge Ligands

Two coordination polymers, namely, two-dimensional complex 1 {[Cu(μ- L)1.5(ClO4)2(H2O)].(H2O)0.5}n (L = pyrazine-1,4-dioxide) and one-dimensional complex 2 [Co(μ-L)Br2(H2O)2]n, have been synthesized with pyrazine-1,4-dioxide as bridging ligands, and their crystal structures were determined by X-ray crystallography. Crystal data for complex 1: monoclinic system, space group C2/c, with a = 23.310(3), b = 12.2338(17), c = 10.6075(15) , β = 110.487(2)°, V = 2833.6(7) 3, Z = 8, C6H9Cl2CuN3O12.5, Mr = 457.60, Dc = 2.145 g/cm3, F(000) = 1832 and μ = 1.998 mm-1; and those for 2: monoclinic system, space group C2/c, with a = 11.012(3), b = 7.483(2), c = 11.451(3) , β = 101.654(4)°, V = 924.2(4) 3, Z = 4, C4H8Br2CoN2O4, Mr = 366.87, Dc = 2.637 g/cm3, F(000) = 700 and μ = 10.487 mm-1. 1 shows a two-dimensional sheet structure on the ac plane through the coordination of μ-L bridging ligands with Cu(II) ions, while 2 displays a zigzag one-dimensional chain along the c axis via the coordination of μ-L bridging ligand with Co(II) ions. Hydrogen bonds in 1 and 2 make the sheets (or chains) connect each other to form a three-dimensional structure.     

The experimental electron density distribution in the complex of (E)-1,2-bis(4-pyridyl)ethylene with 1,4-diiodotetrafluorobenzene at 90 K

The experimental electron density of the donor-acceptor complex of (E)-1,2-bis(4-pyridyl)ethylene (bpe) with 1,4-diiodotetrafluorobenzene (F(4)DIB) at 90 K has been determined with the aspherical atom formalism and analyzed by means of the topological theory of molecular structure. The bpe and F(4)DIB molecules are connected by intermolecular I.N bonds into infinite 1D chains. F.H bonds link these chains together to form the crystal assembly. The topological analysis reveals that the Cbond;I bond is of the "closed shell" type. Its bond-critical properties run parallel to those found in metal-metal and metal-ligand bonds of organometallic compounds. The integrated net charges show that the I.N halogen bond has an essentially electrostatic nature. F.F, F.C, and C.C intermolecular interactions, for which a bond path was found, contribute to reinforce the crystal structure.     

Syntheses and structures of copper(I) complexes based on Cu(n)X(n) (X = Br and I; n = 1, 2 and 4) units and bis(pyridyl) ligands with longer flexible spacer

Self-assembly of four bis(pyridyl) ligands with longer flexible spacer: 1,4-bis(3-pyridylaminomethyl)benzene (L1), 1,4-bis(2-pyridylaminomethyl)benzene (L2), 1,3-bis(3-pyridylaminomethyl)benzene (L3) and 1,3-bis(2-pyridylaminomethyl)benzene (L4), and CuX (X = Br and I) leads to the formation of eight [Cu(n)X(n)]-based (X = Br and I; n = 1, 2, and 4) complexes, [Cu(2)I(2)L1(PPh(3))(4)] (1), [Cu(4)Cl(2)Br(2)(L4)(2)(PPh(3))(6)]·(CH(3)CN)(2) (2), [Cu(2)I(2)(L3)(2)] (3), {[Cu(2)Br(2)L2(PPh(3))(2)]·(CH(2)Cl(2))(2)}(n) (4), [CuIL1](n)·nCH(2)Cl(2) (5), [CuIL1](n) (6), [CuIL4](n) (7) and [Cu(2)I(2)L4](n) (8), which have been synthesized and characterized by elemental analysis, IR, TG, powder and single-crystal X-ray diffraction. Structural analyses show that the eight complexes possess an increasing dimensionality from 0D (1-3) to 1D (4) to 2D (5-8), in which 1 and 2 contain a CuX unit, 2-7 contain a Cu(2)X(2) unit and 8 contains a Cu(4)X(4) unit. Such evolvement indicates that the conformation of flexible bis(pyridyl) ligands and the participation of triphenylphosphine (PPh(3)) as a second ligand take an essential role in the framework formation of the Cu(i) complexes. Moreover, a pair of symmetry-related L3 ligands in complex 3 coordinate to the rhomboid Cu(2)I(2) dimer to form "handcuff-shaped" dinuclear structures, which are further joined together through intermolecular N-HI hydrogen bonds to furnish a 2D (4,4) layer. Although complexes 5 and 6 exhibit a similar 2D (4,4) layer constructed from L1 ligand bridging [Cu(2)I(2)](n) units, the different packing fashion of the layers leads to the formation of 3D porous frameworks of 5 and dense 3D frameworks of 6. The "twisted-boat" conformation of the Cu(4)I(4) tetramer unit in complex 8 has not been reported so far.     

多齿配体2,5-二羟基-1,4-苯醌缩氨基脲 (C_6H_4O_3NNHCONH_2.CHON(CH3_)_2)的合成及晶体结构

报道了含1个溶剂DMF的多齿配体2,5-二羟基-1,4-苯醌缩氨基脲的合成和晶体结构。该化合物(C10N4O5H14)属正交晶系,其空间群为P212121 a=13.221(6),b=17.709(5),c=5.347(4)?, V=1252.0(1)3,Z=4,F(000)=568, Dx=1.434g/cm3,Mr=270.25, m (MoKα)= 1.16 cm-1, 结构由直接法解出,全矩阵最小二乘法修正,最终的偏离因子R=0.0319,wR=0.0748。结构测定表明溶剂DMF分子和2,5-二羟基-1,4苯醌缩氨基脲间形成很强的氢键,后者可看作是两条共轭链的偶合物。     

Crystal and molecular structure of methyl 2-bis(pentyloxy)phosphoryl-2-phenylsulfonamido-3,3,3-trifluoropropionate

Crystal and molecular structure of methyl 2-bis(pentyloxy)phosphoryl-2-phenylsulfonamido-3,3,3-trifluoropropionate (I) was determined by XRD analysis: space group $P\bar 1$ , a=9.406(3), b=12.068(6), c=14.150(8) Å, α=66.88(5), β=68.61(5), γ=71.33(5)°, Z=2, R=0.090 (CAD-4 automatic diffractometer, λCuK_α, 1950 independent reflections with I≥2σ). The S and P atoms of molecule I have a distorted tetrahedral coordination. The S?N?C?P torsion angle is 159.4°. The two pentyl substituents in structure I have different conformations, and their atoms make rather intense thermal vibrations. In crystal structure I, the molecules are linked into centrosymmetric H-dimers by pairs of intermolecular hydrogen bonds N?H...O=P.     

Solvothermal synthesis and crystal structure of a 1d coordination polymer: [Ni(1,4-BDC)(N-MIM)<Subscript>2</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> (1,4-BDC = 1,4-benzenedicarboxylic acid,N-MIM = <Emphasis Type="Italic">N</Emphasis>-methylimidazole)

A new metal-organic coordination polymer, namely [Ni(1,4-BDC)(N-MIM)₂] _n (I) (1,4-BDC = 1,4-benzenedicarboxylic acid and N-MIM = N-methylimidazole), has been synthesized under solvothermal conditions by using N-MIM as solvent and characterized by elemental analysis, IR, and X-ray single-crystal diffraction. The X-ray diffraction analysis reveals that I crystallizes in the monoclinic system, space group C2/c. The 1,4-BDC ligand adopts a bis(bidentate) chelating mode to connect two adjacent Ni(II) centers to form a one-dimensional (1D) zigzag chain. The adjacent chains are further linked through hydrogen bonds and π-π stacking interactions, forming a three-dimensional (3D) supramolecular framework. The unit cell parameters for I: a = 17.250(10), b = 7.214(4), c = 16.506(7)Å, β = 125.53(4)°, V = 1671.6(15)ų, Z = 4.