Hydrothermal Synthesis and Structure Characterization of Diamine-templated Two-dimenisional Cerium Sulfate,[C_6N_2H_(14)][Ce(SO_4)_2(H_2O)_2]·0·5SO_4·2·5H_2O

Open-framework materials are of great interestfrom both the theoretical and practical points of viewdue to their catalytic, absorbent, and ion-exchangeproperties[1]. In the past decade, the study of structur-ally and chemically diverse open framework solids hasbeen flourishing[2—7]. A large variety of silicates[2],phosphates[3]and carboxylates[4]with open-frameworkstructures have been synthesized with organic amines astemplates. Ithas also been demonstrated thatother oxy-salts such as selenat…     

Synthesis, Spectroscopic Properties and Crystal Structures of Dibenzyltin（IV） Dithiobenzoate and Chlorodibenzyltin（IV） Thiobenzoate

Two dibenzyltin(IV) complexes with thiobenzoate ligand, (PhCH2)2Sn(SOCPh)2 (1) and (PhCH2)2Sn(C1)SOCPh (2), have been synthesized by the reaction of dibenzyltin(IV) dichloride with thiobenzoic acid in the presence of organic base Et3N and characterized by IR, ^1H NMR spectroscopy and elemental analysis. Their crystal structures were determined by X-ray single crystal diffraction analysis. In the crystals of 1, the tin atom is six-coordinated in a distorted octahedron configuration. In the crystals of 2, the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other to form a dimer with intermolecular Sn…C1 distances of 0.3591 (2) nm and the tin atom is five-coordinated in a distorted trigonal bipyramid configuration.     

Synthesis,Characterization and Crystal Structure of (PhCH2)2Sn(S2CENt2) and (PhCH2)2Sn(S2CNC4H8)2

Two new dibenzyltin bisditiocarbamates(PhCH2)2 Sn(S2CNEt2)2(1) and (PhCH2)2 Sn(S2CNC4H8)2(2) were synthesized by the reaction of dibenzyltin dichloride with dithiocarbamates and characterized by elemental analysis ,IR,^1H NMR and MS spectra.The crystal structures were determined by X-ray single crystal diffraction analysis.In both complexes,the tin atom is six-coordinated in a distorted octahedral configuration.In the crystals of 1,the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other in dimers by two Sn S interactions of 0.3816nm.In the crystals of 2,the molecules are packed in the unit cell in one-dimensional chain structure linked by weaker intermolecular S S conmtacts.     

Synthesis and Crystal Structure of the Organotin Complex [(o-Cl-PhCH_2)_3SnOCOC_(10)H_8N]·0.5C_6H_6

1 INTRODUCTION There is increasing interest in the study of orga-notin carboxylic ester compounds due to their insec-ticidal, fungicidal and antibiotic activities[1, as well 2]as structure diversity. In recent years many organo-tin carboxylic ester compounds with good biologi-cal activity have been synthesized[3, . Previous stu- 4]dies show that the coordination geometry of centralatom Sn …     

Synthesis and characterization of a new Mo-Fe-S cluster compound containing MoO_3S_3 unit and mixed-valent Mo atoms [Et_4N]_2[Mo_2Fe(CO)_4(S,O-C_6H_4-1,2)_3Cl_2]

Reaction of [Mo3(CO)7(S,O-C6H4-1,2)3]2- with FeCl2 in MeCN at 60℃ affords a new Mo-Fe-S cluster complex containing MoO3S3 unit and mixed-valeut Mo atoms, [Et4N]2[Mo2Fe-(CO)4(O,S-C6H4-1,2)aCl2] (1). 1 is characterized by elemental analysis, IR, Mossbauer spectra, X-ray photoelectron spectra and mass spectra. And the structure of 1 is suggested as the structure which contains a [Mo(S,O-C6H4-1,2)3] unit of which the two of three sulfur atoms link to a Mo(CO)4-moiety and the three oxygen atoms are coordinated to a FeCl2 ligand.     

Synthesis,halogenation and structural characterization of (Z)-1-[2-(triphenylstannyl)vinyl]-l-cyclododecanol

Synthesis and characterization of (Z)-1-[2-(triphenylstannyl)vinylj-l-cyclododecanol,c-(CH2)11C(OH)CH=CHSnPh3,are reported,together with its halogenation by I2,Br2 and IC1 to yield derivatives of the types c-(CH2)11C(OH)CH=CHSnPh3_nXn (n=1,2; X=I,Br,Cl,respectively).The molecular structures of two compounds have been determined by X-ray diffraction analysis.The tin atom exhibits a distorted tetrahedral geometry in the crystal of (Z)-1-[2-(triphenylstannyl)vinyl]-1-cyclododecanol,but a trigonal bipyramidal geometry in the monoiodo-derivative (Z)-1-[2-(diphenyliodo-stannyl)vinyl]-l-cyclododecanol and other derivatives,in which significant intramolecular coordinative interaction HO→Sn is observed.And the formation of a five-membered tin containing ring is significant for their antitumour activities.     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Synthesis, Structure and Characterization of Bis(ethylene-1,2-dithiolate)(μ_2-di-2-pyridyl-ketone p-phenyldiamine-N,N'''')-tin(IV) Dichloromethane

1 INTRODUCTION Sn(edt)2:[Sn(edt)2L]?CH2Cl2 through a one-pot reac- tion of Sn(edt)2, bis(2-pyridyl)ketone and p-phenyl- In recent years, the researches on tin sulfide mate- diamine in CH2Cl2. Herein we report the synthesis, rials draw increasing attention of chemists owning to crystal structure and characterization of the title com- their potential applications as photovoltaic materials, pound. holographic recording system[1, , solar control devi- 2] ces[3 and semiconductor materials. …     

[Co_3(1,2-S2C6H4)_3(PPh_3)_3]+, A basic triangle unit of some polynuclear molecules

[Co3(1,2-S2C6H4)3(PPh3)3][CoBr3(DMF)].sol (1, sol=CHCl3,O(C2H5)2,H2O) was obtained from the reaction of CoBr(PPh3)3 with Na2(S2C6H4) in chloroform. The Co3 core in the cation of 1 exhibits a metal-metal bonded isosceles triangle, in which the two longer Co-Co bonds are both bridged by S2C6H4 ligands on two sides of the triangle plane respectively, while the bottom short Co-Co bond is bridged by the third bidentate S2C6H4 ligand. A series of polynu-clear cobalt cluster compounds with phosphine, thiolate and/or sulphur ligands were prepared by low oxidation state Co+ with thiolates in organic solvents. These tri-, tetra-, hexa-, heptanuclear cluster compounds 1-8 with various types of crystal structures can be viewed as the condensed polynuclear cobalt complexes that the cobalt atom frameworks with sulphur bridged were built through the small triangular units of [Co3S3nL3] (n=1,2) with or without [CoL] (L=PR3, Br, Cl, 5-C5H5) fragments.     

Synthesis,Structure and Biological Activities of a Novel Anionic Organotin(Ⅳ) Complex {[(pClC_6H_4CH_2)Sn(H_2O)(Cl)_2OCOCH(O)CH(O)CO_2Sn(H_2O)(Cl)_2(p-ClC_6H_4CH_2)]·2(HNEt_3)}

A novel anionic organotin(Ⅳ) complex {[(pClC_6H_4CH_2)Sn(H_2O)(Cl)_2OCOCH(O)CH(O)CO_2Sn(H_2O)(Cl)_2(p-ClC_6H_4CH_2)]·2(HNEt_3)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.     

Synthesis and Structural Characterization of a Salt {[Co(Phen)_3][Mo_2S_2(μ-S)_2(edt)_2]}_2·(DMSO)_2·(Et_2O)(Phen = 1,10-Phenanthroline,edt=Ethane-1,2-dithiolate)

1 INTRODUCTION Dinuclear sulfido-bridged complexes with M2S2(μ-S)2 unit serving as building blocks for the construction of mixed-metal clusters are well docu- mented due to their rich structure diversities[1～3] as well as their potential applications in catalytic sys- tems and eletro/photonic materials[4, 5]. For example, reaction of [CpEt2Mo2S2(μ-S)2] with 2 equiv. of Co- (CO)3(NO) gave rise to a cubane-like cluster com- pound [CpEt2Mo2S2(μ-S)2Co2(CO)2][6]. In the case of[Mo…     

Solvothermal Synthesis,Crystal Structure and Optical Property of Lanthanide Selenidostannate [{Tb（en）_3}_2（μ-OH）_2]Sn_2Se_6 with a 3-D H-bonded Network

An inorganic-organic hybrid lanthanide selenidostannate [{Tb(en)3}2(μ-OH)2]Sn2Se6(1) was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120(2),b=11.781(3),c=15.403(3),β=99.534(5)°,V=1811.1(7)3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F(000)=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ> 2σ(Ⅰ).1 consists of a [Sn2Se6]4-and a [{Tb(en)3}2(μ-OH)2]4+ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb(en)3}2(μ-OH)2]4+ complex is composed of two [Tb(en)3]3+ ions joined by two μ-OH bridging ligands.The Tb3+ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb(en)3}2(μ-OH)2]4+ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.     

Solid state synthesis and structure of two novel polyoxometalates [(n-Bu)_4N]_4[M_6o_(19)][Ag_21_4](M=Mo,W)

The reaction of [NH4]2[MO2S2],AgI and (n-Bu)4NBr in solid state produced the polyoxometalates [(n-Bu)4N]4[M6O19][Ag2l4] (1,M=Mo;2,M=W) which were structurally determined.The crystals of 1 and 2 are isomorphous,monoclinic,space group P221/c.1,a=1.6624(2),6=1.6699(3),c=1.7217(2) nm,(8=98.29(1)°,V =4.729(1) nm3,Z=2,R=0.040,Rw=0.037;2,a= 1.6636(3),6=1.6733(3),c=1.7190(3) nm,β=98.25(1)°,V=4.736(1) nm3,Z=2,R=0.038,Rw=0.047.The results of the structure determination showed that the two compounds had the same structures whose skeletons are composed of [Ag2I4]2-and [M6O19]2-The difference of them and heteropolymetalate compounds synthesized in solution is that the title compounds contain cluster ion,heteropolymetalate and organic cations,while the latter is only composed of heteropolymetalate and organic cations.     

Syntheses and Crystal Structures of Two New Metal Phosphonates:[Mn(H_2O)_2(C_(12)H_8N_2)(HO_3PCH_2CH_2CO_2)] and [Co(H_2O)_4(C_(10)H_8N_2)]·(HO_3PCH_2CH_2CO_2)

By the reactions of manganese(II) acetate, 2-sulfoethylphosphonic acid, 1,10-phen (1,10-phen = 1, 10-phenanthroline) or cobalt(II) acetate, 4,4'-bipy and 2-carboxyethylphosphonic acid, two novel compounds of [Mn(H2O)2(C12H8N2)(HO3PCH2CH2CO2)] (1) and[Co(H2O)4 (C10H8N2)]· (HO3PCH2CH2CO2) (2) have been synthesized and characterized by IR spectroscopy, elemental analyses and single-crystal X-ray diffraction. Compound 1 has a 0D structure. Two Mn(II) ions are linked by two 2-carboxyethylphosphonic acid ligands, forming a centrosymmetric dimer. These dimers are further interlinked into a 2D layer structure by π-π stacking interactions and hydrogen bonds. Compound 2 has a 1D chain structure. The 2-carbo- xyethylphosphonic acid remains uncoor- dinated and acts as the organic template. By the bridge of 4,4'-bipy, the [Co(4,4'-bipy)]2+ chains are formed.     

Zinc-containing chainlike polymer {Cs_2[Zn(S_2C=C(CN)_2)_2]}_n,the second example of bridging [S_2C=C(CN)_2]

The title compound {Cs2[Zn(S2C=C(CN)2)2]}n(2),Catena-poly {dicesium [bis(l,l-dicyanoethene-2,2-dithiolato-S,S':N)-Zinc(Ⅱ)]},is the second example of bridging [S2C=C(CN)2] (hereafter referred to as i-mnt) for metal-containing polymer.It crystallizes in the non-centrosymmetric space group Ia (alt.Cc,No.9).There are two coordination modes of i-mnt in this compound:μ-η1-η1-i-mnt,bridging two Zn moieties with two S atoms and terminal i-mnt.A characteristic feature of the structure is the infinite-Zn(η2-i-mnt)(η1-η1-i-mnt)-Zn(η1-η1-i-mnt)(η2-i-mnt)-wave-like chain.Cs atoms are located between the chains to form three-dimensional network-like packing.An efficient second harmonic generation from the crystal has been observed on the irradiation with the 1064 nm output of a Nd:YAG laser.     

A Valuable Synthetic Route to the Enantiopure Functionalized N-Substituted Aziridines

Chiral butyrolacto[3,4-b]-2(S)-6(R)-1-N-akylaziridines 7 were synthesized in enantiopure form utilizing racemic 5-methoxy-3-bromo-2(5H)-furanone (5) and available amines (6) as key precursors. After highly effective reduction of 7, the functionaiized 2(S),3(R)-dihyroxymethyl-N-alkylaziridines (8) were obtained in good yields with ≥98% ee. This is a simple and pratical method for the preparation of enantiopure aziridines which are important intermediates in the synthesis of biologic active molecules.     

Syntheses and Single-crystal Structures of Ln_3Sn_(0.25)GeS_7 (Ln=La,Sm)

Two new quaternary sulfides,La3Sn0.25GeS71 and Sm3 Sn0.25GeS72,have been synthesized by a facile solid-state reaction,and their crystal structures were determined by singlecrystal X-ray diffraction analysis.The two compounds crystallize in the P6 3 space group,and the crystal data are as follows-La3Sn0.25GeS7:a=10.3335(7),c=5.8455(7),Z=2;Sm3Sn0.25GeS7:a=9.999(3),c=5.787(2),Z=2.Single-crystal analysis indicated that the two compounds consist of three types of building blocks:LnS 8 anti-tetragonal prism,SnS 6 octahedron,and GeS 4 tetrahedron.     

Layered Lanthanum Complex with 3-Nitrophthalic Acid Assembled via Hydrogen Bonds-Synthesis, Structure and Characterization of [LaL(HL)(H_2O)_3]_2·2H_2O (H_2L=3-NO_2C_6H_3(CO_2H)_2)

A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2·2H2O (H2L = 3-nitro- phthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1 with a = 8.1549(16), b = 8.8856(18), c = 15.277(3) , α = 100.93(3), β = 90.81(3), γ = 104.56(3)°, V = 1049.8(4) 3, Z = 1, μ = 2.125 mm-1, Dc = 1.994 g/cm3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates(2-) coordinate with the La3+ ions in a bridging mode, and two monohydrogen- 3-nitrophthates(1-) and three waters in terminal ways, respectively. Each La3+ ion is nine- coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C–H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.     

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system,space group P1 with a=7.0124(11),b=11.919(2),c=14.879(3),α=108.791(3),β=102.441(3),γ=92.846(2)o,V=1140.1(3)3,Mr=859.71,Z=2,Dc=2.504 g/cm3,μ =5.324 mm-1,F(000)=804,S=1.013,the final R=0.0297 and wR=0.0618 for 3534 observed reflections with I > 2σ(I). 1 consists of [C4H9NH3]+ cations and two-dimensional [Sb4S7]n2n- anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]+ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.     

The Inorganic-free Organic Conductor α''''-(ET)_2C_6H_4(SO_3)_2 : Its Synthesis, Structure, and Conductivity

Having more than twenty years?glory, ET series still keep the most promising family in various kinds of organic conductors. Most of ET based molecular conductors consist of organic cationic ET+0.5 radical and certain anionic inorganic component such as the superconductor k-(ET)2Cu[N(CN)2]Cl (TC = 12.8K, 0.3kbar)1. Recently, the first purely organic superconductor b-(ET)2SF5CH2CF2SO3 (TC = 5.2K)2 has been reported, which aroused our interest on this kind of inorganic-free organic c…