Synthesis and Crystal Structure of Bis(cyclopentadienyl) Ytterbium Complex Supported by β-Diketiminate

Treatment of the β-diketiminate-supported ytterbium dichloride LYbCl2(THF)2 1 (L = N,N'-bis(2,6-dimethylphenyl)-2,4-pentanediiminate) with 2 equiv of C5H5Na gave rise to the title complex LYb(C5H5)2 2 (C31H35N2Yb, Mr = 608.65), and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 14.417(2), b = 10.432(2), c = 18.040(4)(A),β= 95.73(2)°, V = 2699.6(9)(A)3, Dc = 1.498 g/cm3, Z = 4,λ(MoKα) = 0.71073(A), μ = 3.485 mm(1, F(000) = 1220, the final R = 0.0304 and wR = 0.0703 for 3962 observed reflections with I > 2σ(I). In the molecular structure of the title complex, the central metal atom Yb is eight-coordinated by two cyclopentadienyl groups and two nitrogen atoms of β- diketiminate group to form a distorted tetrahedral geometry.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cobalt（Ⅱ） Complex

A metal-organic coordination polymer [Co2(cbba)4(bix)2]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid,bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,TG,and single-crystal X-ray diffraction.Pink crystals crystallize in the monoclinic system,space group P21/n with a = 21.148(4),b = 15.728(3),c = 23.879(4) ,β = 102.148(3)°,V = 7764(2)3,C316H232Cl15Co8N32O48,Mr = 6248.53,Dc = 1.336 g/cm3,F(000) = 3207,Z = 1,μ(MoKα) = 0.621 mm-1,the final R = 0.0567 and wR = 0.1280 for 8510 observed reflections(I > 2σ(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Synthesis and Crystal Structure of β-Diketiminate Ytterbium Dichloride

1 TRODUCTIINON The monoanionic b-diketiminato ligands, [ArNC(R)CHC(R)NAr]- [1], are ideal for use with metals and have been applied for early[2] and late[3] transition metals and group 13 metal complexes[4]. These ligands have several attractive feature…     

Synthesis and Crystal Structure of β-Diketiminate Ytterbium Dichloride

The reaction of anhydrous YbCl3 with lithium β-diketiminate, LLi (L=N,Ndiphenyl-2,4-pentanediimine anion), in 1:1 molar ratio in THF gave rise to the title complex LYbCl2(THF)2 1 which has been characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pna21(#33) with a=19.657(8), b=9.581(4), c=14.107(6) A,V=2656.8(18) A3, Z=4, C25H33N2O2Cl2Yb, Mr= 637.49, Dc=1.594 g/cm3, F(000)=1268.00 and μ (MoKα)=3.744mm- 1. The final R and wR are 0.031 and 0.073 for 2596 observed reflections with I ＞ 2σ(I), respectively. The X-ray crystal structure analysis revealed that the center ytterbium(Ⅲ) is bonded to two chloride anions, two oxygen atoms from two tetrahydrofuran molecules and one chelate ligand β-diketiminate to form a six-coordinate distorted octahedral geometry.     

Synthesis and Crystal Structure of O,O-Dimethyl-N-(β-triphenylgermanyl)propionyl-α- aminobenzylphosphonates

1 INTRODUCTION Both β-triphenylgermanyl propionic acid and its derivatives have recently attracted a great deal of attention due to their strong anti-inflammatory as well as antibiotic properties[1~3]. α-aminobenzyl- phosphonates are also reported to exhibit diverse biological activities[4~6].It is conceivable that the incorporation of the two moieties into one structural unit might produce an unexpected effect on the activity of such a compound, and the studies on this type of novel s…     

Synthesis and Crystal Structure of a New μ-Oxamide Trimeric Hetero-tetranuclear Complex

1 INTRODUCTION The study of spin exchange interaction between metal centers through extended bridges is an active subject in the field of coordination chemistry[1～3]. Polynuclear complexes with extended ligand bri- dges are currently of considerable interest[4～6]. One of the best strategies to design and synthesize poly- nuclear species is ‘complex as ligand’ approach[4, 7]. The oxamide group is proved to be an interesting multiatomic bridge, linking metals in polynuclear complexes[8…     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

Synthesis and Crystal Structure of 2-Nitro-9,9-bis（methylpropionate）fluorine

The title compound of 2-nitro-9,9-bis(methylpropionate)fluorine (C21H21NO6 , Mr=383.39) was synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P21/c with a=11.4581(15), b=10.3624(14), c=16.573(2) , β=96.629(2) o , V=1954.6(5) 3 , Z=4, Dc=1.303 g/cm 3 , μ=0.096 mm -1 , F(000) = 808, R =0.0493 and wR=0.1499 for 3107 observed reflections with I > 2σ(I). X-ray analysis reveals that three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system. Weak C-H O hydrogen bonding connects the molecules into centrosymmetric dimmers.     

Synthesis and Crystal Structure of a Three-dimensional Manganese(Ⅱ)Complex Constructed via Covalent and Hydrogen Bonds

1INTRODUCTIONCrystalengineeringofone-,two-andthree-dimensionalsupramolecularcomplexesiscurrentlyofgreatinterestowingtothefascinatingstructuraldiversityandpotentialapplicationsinmaterials,suchaselectricconductivity,magnetism,host-guestapplication,molecularrecognitionandcatalysis[1,2].Severaltypesofinteractions,suchascoordinationcovalentbond,hydrogenbond,p-pstackingandelectrostaticinteractionscanbeusedtoconstructextendedsupramolecularframeworks[3~6],butcoordinationbondingandhydrogenbondingin…     

Synthesis and Crystal Structure of a Novel Fe(Ⅲ) Schiff Base Complex

A novel Fe(Ⅲ) Schiff base complex,FeⅢ(HL) {H4L = 1,1,1,1-tetrakis[(salicylaldimino)methyl]methane},has been prepared and characterized by elemental analyses,IR spectrum,and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P21/n with a = 12.569(3),b = 12.955(3),c = 17.647(4) ,β = 91.896(9)°,V = 2871.9(1) 3,Z = 4,Dc = 1.391 g/cm3,F(000) = 1252.0,Mr = 601.45,R = 0.0383 and wR = 0.1025.The structural analysis reveals that the Fe(Ⅲ) ions are six-coordinated by imine nitrogen atoms and phenolic oxygen atoms form three pendant arms of Schiff base ligands,and one of the salicylaldimine chelating units remains uncoordinated.Discrete complex molecules were further assembled into 1D supramolecular aggregations by C-H…O hydrogen bonding and C-H…π interactions.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Synthesis,Crystal Structure and Fluorescent Property of a Lanthanum(Ⅲ) Complex Coordinated with Quinolinyloxy Acetamide Ligand

A novel lanthanum(Ⅲ) complex, [LaL2(NO3)3]·H2O(1) based on L(L = N-(naphthalene-1-yl)-2-(quinolin-8-yloxy)acetamide), was synthesized and characterized by X-ray diffraction. The crystal of 1 belongs to the monoclinic system, space group C2 c with Mr = 1017.69, a = 25.1438(17), b = 13.5950(9), c = 18.2349(12) A, β = 132.4980(10)°, V = 4595.8(5) A3, Z = 4, Dc = 1.471 Mg/m3, F(000) = 2056, μ = 1.004 mm-1, R = 0.0588 and wR = 0.1402. The central La(Ⅲ) ion is coordinated to four oxygen atoms, two nitrogen atoms from two independent acetamide ligands and six oxygen atoms from three nitrate anions, possessing a distorted icosahedron coordination geometry. In the crystal of 1, intermolecular N–H···O hydrogen bonds linked the molecules into chains along the c axis. In solid state and CH3 CN solution, complex 1 exhibits stronger fluorescent emission than the ligand L.     

Synthesis and Crystal Structure of a New Zn(Ⅱ) Coordination Polymer Constructed by 1,2,4,5-Benzenetetracarboxylate

A new Zn(Ⅱ) coordination polymer [Zn3(btec)(OH)2(H2O)2]n (1, btec = 1,2,4,5- benzenetetracarboxylate) has been synthesized by hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in mono- clinic, space group C2/c, with a = 19.580(3), b = 5.0137(8), c = 15.975(3), β = 121.629(2)°, V = 1335.3(4)3, C10H8O12Zn3, Mr = 516.27, Z = 4, Dc = 2.568g/cm3, μ = 5.419 mm-1, F(000) = 1016, R = 0.0590 and Rw = 0.1279 for 1110 observed reflections (I > 2σ(I)). X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn(Ⅱ) atoms which are connected through the bridging carboxylate oxygen atoms of the btec ligands and μ2-bridging oxygen atoms of water molecules to generate an infinite one-dimensional chain. The adjacent chains are linked together through the benzene rings of the btec ligands to form a two-dimensional polymeric network. The adjacent two-dimensional layers are further connected together by the benzene rings of btec ligands to give the final three-dimensional structure. The benzene rings act as pillars between two layers.     

Synthesis and Crystal Structure of Bis（barbiturato） triwater Complex of Copper（Ⅱ）

1 INTRODUCTION A variety of transition metal complexes with barbiturates have been prepared owing to their important roles in clinical detection and identi- fication of drug[1～5]. They have the general formula of M(Ⅱ)(barb)2L2, where M is a transition metal (Co, Cr, Zn, Cu etc), barb the anion of a substituted barbituratic acid and L an organic base, usually pyridine. In these complexes, the donor atom in the barbiturate anion is a deprotonated nitrogen atom and, the coordination …     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Synthesis and Crystal Structure of Glycin·3,5-Dihydroxybenzoic Acid

1 INTRODUCTION In the last two decades, the extended field of non-linear optical (NLO) applications (frequency conver-sion, optical parametric amplification and oscillationetc) has stimulated search for highly nonlinear opticalmaterials[1~3]. Especially, organic NLO materials arerapidly investigated due to their large nonlinear sus-ceptibility, inherent synthetic flexibility, high opticaldamage thresholds and intrinsic tailorability[4~6]. It isknown that the solution growth technique a…     

Synthesis, Crystal Structure and Hydrogenation Catalysis of a CF3-BINAP（O）-Rh-COD Complex

The complex [(CF3-BINAP(O))Rh(COD)][ClO4]·Et2O(2,CF3-BINAP(O)=2-{bis[3,5-bis(trifluoromethyl)phenyl]phosphino}-2-{bis[3,5-bis(trifluoromethyl)phenyl]phosphinyl}-1,1-binaphthyl, COD=1,5-cyclooctadiene) was obtained directly from the reaction of CF 3-BINAP(O) ligand with [Rh(COD)][ClO4]. Complex 2 has been characterized by single-crystal X-ray diffraction. The crystal adopts space group P21/n with a=19.0727(4), b=15.6275(4), c=22.3039(6), β=112.3570(10)°, V=6148.2(3)3 , Z=4, Dc=1.693 g/cm3 , F(000)=3144, μ(MoKα)=0.500 mm-1 , the final R=0.0947 and wR=0.2501. Structural studies reveal that Rh(I) is coordinated by one oxygen and one phosphorus in the same ligand. Asymmetric hydrogenation of acetami- docinnamic acid with compound 2 was also evaluated.     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).