Molecular and Supramolecular Structures of a Nickel（Ⅱ） Complex with a Macrocyclic Ligand

1 INTRODUCTION The knowledge of all non-covalent interactions, such as strong and weak hydrogen bonds and p…p interactions, is important to the supramolecular chemistry, biochemistry, crystal engineering and material science[1～7]. Several mononuclear complexes of macrocyclic oxamido Schiff base ligands with phenyls have been used as 揷omplex ligands?to design polynuclear complexes[8～11]. Herein we report the molecular and crystal structures, CH贩稯 hy- drogen bonding and p…p stacki…     

Synthesis and Crystal Structure of Macrocyclic Cavitand Cucurbit[5]uril and Its Supramolecular Adduct with Cu（Ⅱ）

The first supramolecular adduct (H₃O)₂[Cu(H₂O)₄](SO₄)₂·2(C₃₀H₃₀N₂₀O₁₀)·₂₄(H₂O) based on cucurbit[5]uril was synthesized and characterized by single crystal X‐ray diffraction analysis. In the adduct, copper ion is coordinated by four oxygen atoms from H₂O. The latter links two cucurbit[5]uril molecules due to a complicated hydrogen bonding containing lattice water molecules.     

Syntheses and Crystal Structures of Three Palladium（Ⅱ） Complexes with Isonitrosobenzoylacetoneimine Ligand

Three palladium (II) complexes with the isonitrosobenzoylacetoneimine (HIBI) ligand, Pd (p‐CH₃C₆H₄IBI)₂ (1), Pd (C₆H₅IBI)₂ (2) and Pd₂Cl₂ (C₆H₅CH₂IBI)₂ · CHCl₃ (3), were prepared and characterized by IR, Raman and X‐ray diffraction studies. The geometries around the palladium atoms in the complexes 1 and 2 are distorted trans‐PdN₄ square planes, and the Schiff base ligands RIBI^? are coordinated through their oximo‐nitrogen atoms and imino‐nitrogen atoms. The week Pd…H? C agostic interactions [Pd…H = 0.2764 nm] complete the hexacoordinate environment around palladium in the complex 1. The octahedral deformation of the classical square planar environment of the Pd atom is due to the week Pd…O (1b) interactions [Pd? O (1b) = 0.3157 (9) nm] in the complex 2. The complex 3 is a first example of binuclear complex with isonitrosoketoimine ligands, in which one of oximo groups is coordinated through oximo‐nitrogen and oximo‐oxygen atoms.     

Synthesis, Characterization and Crystal Structure of the First Tri-nuclear MFe2（M = Cu and Ni） Complexes Based on Nitroprusside

IntroductionSince 184 8,whenPlayfairpublishedthefirstpaperrelatedtonitroprussides ,1thetransitionmetalpenta cyanonitrosylmetallatehydrateshavebeenwidelystudiedbecauseoftheirimportantrolesinmolecularsieves ,cationexchangers,electronscavengersandradionuclidesor bents .2 4 Thenitroprussides ,regardlessofthecationicmetal,arecurrentlyemployedasreversibleinhibitorsofagroupofenzymesknownassuperoxidedismutases .5Recently ,using [Fe(CN ) 5(NO) ]2 - asabuildingblock ,somenitroprusside bridgedpolymeri…     

Synthesis,Crystal Structures and Properties of Two Novel Co（Ⅱ） and Cd（Ⅱ） Complexes of N-AcetyI-L-glutamic Acid and Imidazole Ligands

Two novel complexes {[Co（A-glu）（Im）2]·0.5H2O}n （1） and [Cd（A-glu）（Im）3]n （2） （H2A-glu=N-acetyl-L-glutamic acid, Im=imidazole） have been synthesized from the reaction of H2A-glu with Co（CH3COO）2·4H2O or Cd（CH3COO）2·2H2O in the presence of Im. Both of the complexes display different coordination environment and similar one-dimensional chain structure. The magnetic susceptibility measurements for 1 show a weak antiferromagnetic interaction between two cobalt（Ⅱ） ions bridged by A-glu ligand. The complex 2 exhibits an intense fluorescent emission in solid state at room temperature.     

Four New Cu（Ⅱ） Complexes with Benzotriazole-based Ligands： Syntheses,Crystal Structures and Theoretical Investigations

Four new Cu（Ⅱ） complexes with two benzotriazole-based ligands, [Cu2（L^1）2（NO3）2]· 2H2O （1）, [Cu2（L^1）2]·2ClO4·2H2O （2）, [Cu2（HL^2）2（NO3）4]·2CH3COCH3 （3） and [Cu（HL^2）2（Cl）]·Cl·2CH2Cl2 （4）, where HL^1 = 1,3-bis（benzotriazol-2-yl）-2-propanol and HL^2 = 1,3-bis（benzotriazol-1-yl）-2-propanol, were synthesized and structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction analyses. It is revealed that complexes 1～3 have dinuclear structures, while 4 possesses a one-dimensional （1-D） chain structure, which extends in two orthogonal orientations. In 1～4, the coordination numbers of Cu（Ⅱ） centers range from four to six, which may be attributed to the different geometries and coordination abilities of the ligands and anions. The L^1 ligand in complexes 1 and 2 adopts a tridentate di-chelating coordination mode, whereas ligand HL^2 in complexes 3 and 4 has a bidentate bridging coordination mode. The different coordination modes of these two ligands may be explained by the different charges of nitrogen donor atoms in the benzotriazole ring, which has been investigated by density functional theory （DFT） calculations.     

Syntheses and Crystal Structures of Ternary Complexes of Zinc（Ⅱ） and Cadmium（Ⅱ） with 3-Aminobenzoic Acid and 1,10-Phenanthroline

1 INTRODUCTION Benzoic acids with substituent of amino are a class of rigid ligands possessing several functional groups. When they coordinate to metal ions, versa- tile coordination modes will be presented with pre- sence of not only coordinate-covalent bonds but also hydrogen bonds. Besides, diverse coordination modes of carboxyl and rigid frame of benzene ring gua- rantee the stability of multi-dimensional structures of the synthesized metal complexes. Thus ligands of this class are o…     

Crystal Structures and Characterizations of Bis(pyrrolidinedithiocarbamato)Cu（Ⅱ） and Zn(Ⅱ） Complexes

The structures of [Cu (S₂CN (CH₂)₄)₂] (1) and [Zn₂(S₂CN‐(CH₂)₄)₄] (2) have been determined by X‐ray crystallography analysis. They are all isomorphous and triclinic, space group of P1^?, with Z = 1. The lattice parameters of compound 1 is: a = 0.63483(2) nm, b = 0.74972(3) nm, c=0.78390(1) mn, α = 75.912(2)°, β = 78.634(2)° and γ = 86.845(2)°; compound 2: a = 0.78707(6) nm, b=0.79823(6) nm, c = 1.23246(9) nm, α = 74.813(2)°, β = 73.048(2)° and γ = 88.036(2)°. The copper atom is located on a crystallographic inversion center and zinc atom lies across centers of symmetry. The Cu(II) ion has a square‐planar geometry while Zn(II) has a distorted tetrahedral geometry. The thermal gravity (TG) data indicate that no structural transitions in the two compounds were abserved and the decomposition products can adsorb gas. Also they all have a high thermal stability.     

Synthesis and Crystal Structures of Two Di-Cu(Ⅱ) Complexes Based on an Asymmetric Dinucleating Ligand

Two new dicopper(II) complexes [Cu2L(OAc)2](ClO4)·H2O(1) and [Cu2L(BPP)2]-(ClO4)(2) using an asymmetric dinucleating ligand HL and auxiliary ligands such as acetate(OAc) and bisphenyl phosphate(BPP) have been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. Complex 1 crystallizes as blue single crystals that belong to the triclinic crystal system and P1 space group, while complex 2 crystallizes in a monoclinic P21/c space group. Single-crystal X-ray diffraction analysis reveals that the two copper ions in complexes 1 and 2 reside within the adjacent ligand compartments and are bridged by the endogenous phenoxo-O from ligand L and the introduction of two desired exogenous carboxylates or phosphates in the bidentate μ-1,3-bridged mode. The coordination geometries of Cu(1) and Cu(2) are both distorted square pyramids.     

Crystal Structures of Fluoride and Chloride Complexes of Tris[（2-benzimidazolyl）methyl]amine

The crystal structures of fluoride and chloride complexes of tris[（2-benzimidazolyl）methyl]amine 1 were characterized by X-ray crystallography. 1 adopts （73 symmetrical geometry and cone-like conformation so as to allow its three NHs to associate with the anions through hydrogen bonds. Despite the different sizes of the anions, the two crystals are unexpectedly isostructural. The binding ability of the anions of 1 in solution was also studied by using of UV-vis spectroscopy.     

Synthesis,Crystal Structure and Magnetic Properties of a Ni（Ⅱ） Supramolecular Complex Based on Aromatic Polycarboxylate Ligand

A Ni(Ⅱ) supramolecular complex,[Ni 2 (btec)(3py) 2 (H 2 O) 8 ](H 2 O) 4 (1),has been synthesized by Ni(ClO 4) 2 ·6H 2 O,benzene-1,2,4,5-tetracarboxylic acid (H 4 btec) and terminal ligand 3-hydroxypyridine (3py) in aqueous solution.The title compound crystallizes in triclinic system,space group P1,with a=8.5637(12),b=9.4138(13),c=10.3611(14),α=67.9540(10),β=85.1740(10),γ=76.9890(10)°,V=754.33(18) 3,Z=2,M r=386.96,D c=1.704 Mg/m 3,μ=1.345 mm-1,F(000)=402,the final R=0.0222 and wR=0.0563 for 2675 observed reflections with I > 2σ(Ⅰ).The adjacent discrete molecules are further self-assembled by intermolecular π-π and O-H···O hydrogen bonding interactions to construct a 3D supramolecular framework.Magnetic measurement shows weak ferromagnetic interaction in the range of 2～300 K.     

Synthesis and Crystal Structure of a New Dinuclear Manganese （Ⅱ） Manganese （Ⅲ） Complex of a Macrocyclic Ligand

IntroductionIn recentyears many efforts have been devotedto the preparation and characterization of pendant-arm macrocyclic complexes due to the fact that theligating groups attaching to the macrocyclic skele-ton can offer additional donor groups to maintainthe coordination sphere of metal centers in themacrocycles[1,2 ] .In this way,functionalised pen-dant- arm macrocyclic complexes have been de-signed and prepared so as to mimic the structureand properties of certain metalloenzymes and met-a…     

Crystal Structures of Co（II） and Cu（II） Complexes and Ammonium Salt Involving Ethylenediamine

The Co（II） complex I and ammonium salt II were synthesized from the direct reaction of 1,2-ethylenediamine and cobaltous acetate tetrahydrate and manganese acetate tetrahydrate in anhydrous ethanol. Treatment of N,N＇-bis（salicylidene）ethylenediamine with Cu（OAc）2·H2O results in the formation of Cu（II） complex III. C14H37CoNaO8 （I）： triclinic, space group P1, a = 8.6296（12）, b = 12.0291（17）, c = 12.1108（17） A, α = 75.335（2）, β = 69.991（2）, γ = 72.248（2）°, V= 1109.4（3） A3, Z = 2, ρcaloa = 1.342 g/cm3, the final R= 0.0342 for 4817 observed reflections with I 〉 2σ（I） and Rw = 0.1263 for all data. C6H16N204 （II）： space group P1, a = 5.5513（10）, b = 5.5589（11）, c = 7.4437（14） A, α = 94.332（4）, β = 104.497（4）, γ = 103.487（4）°,V= 214.06（7） A3, Z = 1, ρcalcd = 1.398 g/cm3, the final R = 0.0431 for 829 observed reflections with I〉 2σ（I） and Rw = 0.1263 for all data. C14H37CuN40 （III）, space group P21/n, a = 9.050（9）, b = 18.434（17）, c = 11.659（11） A, β = 107.134（19）°, V= 1859（3） A3, Z = 4, ρcalcd =1.443 g/cm3, the final R = 0.0616 for 3308 observed reflections （O 〉 2σ（I）） and Rw = 0.1229 for all data. Their structures were all determined by X-ray diffraction, elemental analysis and IR.     

Crystal Structure, Thermal Analysis and Theoretical Calculation of a One-dimensional Chain Complex [Zn（dafo）2（H2O）2]（NO3）2

Introduction Molecular recognition and molecular self-assemblycarried out by cooperation of the weak interactions(electrostatic reaction, hydrogen bonds, van der Waalsforce, short-range repulsive force, etc) are the commonphenomena in nature. In recent years, the research onsupramolecular complex has been a crossing focus ofseveral subjects such as chemistry, physics, biology,material and information.1 Supramolecular complex hasa wide application foreground in material, catalysis,conductor,…     

Synthesis and Crystal Structure of Dissymmetrical Double Schiff Base Cu（Ⅱ） Homobinuclear and Cu（Ⅱ）-Mg（Ⅱ）-Cu（Ⅱ） Heterotrinuclear Complexes

Homobinuclear complex （HCuL）2 （1） （H3L： N-3-carboxylsalicylidene-N＇-salicylaldehyde-1,2-diaminoethane） was obtained from self-organization of the reported complex HCuL, and its crystal structure was determined through X-ray diffraction at room temperature. The crystal of complex 1 belongs to monolinic system, the space group Cc, a=2.5326（5） nm, b=0.88861（18） nm, c=1.3738（3） nm, β=96.95（3）°, Z=4, R1=0.0520, wR2=0.1185. （HCuL）2 is a dimeric molecule and has extended phenolic oxygen-bridged structure. In addition, using mononuclear complex HCuL as building blocks, Cu（Ⅱ）-Mg（Ⅱ）-Cu（Ⅱ） heterotrinuclear complex 2 was synthesized, and its crystal structure also has been determined by X-ray analysis. The crystal of complex 2 is of monoclinic system, space group Pc, a=1.1816（2） nm, b=1.5599（3） nm, c=1.9642 （4） nm, β=98.22°, Z=2, R1=0.0701, wR2=0.1498. Each dissymmetricai cell unit of complex 2 contains two heterotrinucler neutral molecules： {[CuL（H2O）]Mg[CuL（CH3OH）]} and {[CuL]Mg[CuL（H2O）]}.     

Syntheses,Crystal Structures and Properties of Co（Ⅱ） and Cu（Ⅱ） Complexes with 5-Nitro-1,2,3-benzenetricarboxylic Acid

Two new coordination polymers,{[Co(O2N-Hbtb)(phen)(H2O)3]·2H2O}n 1 and {[Cu3(O2N-btb)2(bipy)2(H2O)4]·4H2O}n 2(O2N-H3btb=5-nitro-1,2,3-benzenetricarboxylic acid,phen=1,10-phenanthroline,bipy=2,2'-bipyridine),were prepared through hydrothermal reactions of Co(Ⅱ) or Cu(Ⅱ) salt with O2N-H3btb in the presence of different auxiliary N-donor ligands.Their crystal structures were determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectroscopy.In the two complexes,O2N-H3btb ligand acts as monodentate and bis-monodentate modes,respectively.Complex 1 displays a two-dimensional layered structure through the inter-and intramolecular hydrogen bonding interactions while complex 2 has an O2N-btb bridged one-dimensional chain which is extended into a three-dimensional network by hydrogen bonding interactions.The magnetic properties of complex 2 are investigated over the temperature range of 2～300 K and ferromagnetic interactions are observed.     

Synthesis, Crystal Structure, Properties and Thermoanalysis of Complexes of Cu（Ⅱ） and Ni（Ⅱ） with Taurine-5-chlorosalicylaldelyde Schiff Base

The reactions of transition metal salts with taurine 5‐chlorosalicylaldelyde Schiff base gave two complexes [Ni(TCSSB)(H₂O)₃].H₂O (1) and [Cu(TCSSB)(H₂O)₂]₂[Cu(TCSSB)₂].6H₂O (2) (TCSSB=taurine‐5‐chlorosalicylaldelyde Schiff base), which were characterized by elemental analysis and X‐ray diffraction analysis. The complex 1 crystallized in monoclinic system with space group P2 ₁/c, and a=1.4816(2) nm, b=1.3953(2) nm, c= 0.7466(1) nm, β= 100.499(3)°, V=1.5176(4) nm³, Z=4, and an infinite 3‐D network structure was formed by hydrogen bonds among sulfo group, crystal water and coordinated water. Complex 2 crystallized in triclinic system with space group P1 , with the cell parameters: a = 0.6413(2) nm, b= 1.4596(3) nm, c= 1.6188(4) nm, a= 102.473(5)°, β= 98.979(4)°, γ=101.739°, V=1.4165(6) nm³, Z=1. The coordination environment between Cu(1) and Cu(2) is different. Cu(1) is slightly distorted square pyramidal while Cu(2) is distorted square‐plane. The complex 1 is mononuclear while the complex 2 is made up of two coordinated subunits, namely [Cu(TCSSB)₂] and [CU(TCSSB)(H₂O)₂]₂. Besides that the TG‐DTG of the complex 1 was analyzed, the thermal decomposition reaction of the complex was studied under a non‐isothermal condition by TG‐DTG. The TG and DTG curves indicate that the complex was decomposed in three stages: .