Synthesis and Crystal Structure of a Copper(Ⅱ) Complex with a Tab-Tab Disulfide Ligand (Tab-Tab)[CuBr4] (Tab = Trimethylammoniumphenyl-4-thiolate)

Reaction of CuBr2 with TabHPF6/Et3N in methanol followed by dissolving the resulting precipitate in hydrobromic acid yielded purple blocks of the title complex [Tab-Tab][CuBr4] 1 (C18H26CuBr4N2S2). 1 crystallizes in the monoclinic system, space group P21/n with a = 9.686(3),b = 19.257(5), c = 13.399(4) (A), β= 93.610(9)°, V= 2494.2(13) (A)3, Z= 4, Dc = 1.911 g/cm3, T=193(2) K, Mr = 717.71, F(000) = 1396, μ = 74.58 cm-1, S = 1.126, R = 0.0748 and wR = 0.1736 for 2921 observed reflections with I ＞ 2σ(Ⅰ). The structure of 1 contains a discrete [CuBr4]2- dianion and a [Tab-Tab]2+ dication. In the dianion, the Cu atom is coordinated to four Br atoms forming a distorted tetrahedral coordination geometry. The bromides of the dianion interact with the H atoms of the phenyl and methyl groups of the dications to form a 1D hydrogen-bonded chain.     

Synthesis and Structure of { (Tab-Tab) [Ag2(μ-Cl)4]·2MeCN}n (Tab = 4-(Trimethylammonio)benzenethiolate)

In the presence of Et4NCl?H2O,reaction of AgCl with TabHPF6 in MeCN afforded the title complex {(Tab-Tab)[Ag2(μ-Cl)4]·2MeCN}n 1.1 crystallizes in the orthorhombic space group Pbcn with a=16.782(3),b=6.8358(14),c=26.194(5) ,V=3004.9(10) 3,Z=8,μ= 1.817 mm-1,Dc=1.711 g/cm3,T=223 K,C11H16AgCl2N2S,Mr=387.10,F(000)=1544,S=1.160,R=0.0528 and wR=0.0896 for 2732 observed reflections with I > 2σ(I).1 contains a 1D linear [Ag2Cl4]n2n-chain coupled with the [Tab-Tab]2+ dications.Intermolecular hydrogen bonding interac-tions between the protons of methyl groups from the Tab-Tab dications and the chlorides result in the formation of a 2D hydrogen-bonded network.     

Construction of symmetric and asymmetric Mo/S/Cu clusters from a cluster precursor [Et4N]2[(edt)2Mo2S2(mu-S)2] (edt = ethanedithiolate)

Treatment of [Et 4N] 2[(edt) 2Mo 2S 2(mu-S) 2] ( 1) (edt = ethanedithiolate) with equimolar CuBr afforded an anionic hexanuclear cluster [Et 4N] 2[(edt) 2Mo 2(mu-S) 3(mu 3-S)Cu] 2.2CH 2Cl 2 ( 2.2CH 2Cl 2). On the other hand, reactions of 1 with 2 equiv of CuBr in the presence of 1,2-bis(diphenylphosphino)methane (dppm) and pyridine (Py) ligands gave rise to two neutral tetranuclear clusters [(edt) 2Mo 2O 2(mu-S) 2Cu 2(dppm) 2] ( 3) and [(edt) 2Mo 2O(mu 3-S)(mu-S) 2Cu 2(Py) 4] ( 4), respectively. The reaction of 1 with 2 equiv of CuBr followed by the addition of a mixture of dppm and Py (molar ratio = 1:2) yielded another neutral tetranuclear cluster [(edt) 2Mo 2(mu-S) 2(mu 3-S) 2Cu 2(dppm)(Py)].Py ( 5.Py). Compounds 2- 5 have been characterized by elemental analysis, UV-vis spectra, IR spectra, (1)H NMR, and X-ray analysis. The structure of the dianion of 2 can be viewed as having a [Mo 4S 8Cu 2] core in which two chemically equivalent [Mo 2(mu-S) 3(mu 3-S)(edt) 2Cu] (-) anions are linked by two extra Cu-S edt bonds. The molecular structure of 3 may be visualized as being built of one [(edt) 2Mo 2X 2(mu-S) 2] (2-) dianion and one [Cu 2(dppm) 2] (2+) dication that are connected by a pair of M-mu-S edt bonds. Compound 4 is formed by the affiliation of two Cu(I) atoms only at one end of the [(edt) 2Mo 2S 2(mu-S) 2] moiety, connecting with the S t atoms and the S edt atom. Cluster 5.Py can be viewed as being constructed from the addition of one Cu atom onto the incomplete cubanelike [Mo 2S 4Cu] framework through one terminal sulfur and one edt sulfur. Among the four clusters, 3 and 4 have internal mirror symmetry or pseudo mirror symmetry, respectively, while 2 and 5 are asymmetric clusters with racemic formation.     

Assembly of a new family of mercury(II) zwitterionic thiolate complexes from a preformed compound [Hg(Tab)2](PF6)2 [Tab = 4-(trimethylammonio)benzenethiolate

Reactions of Hg(OAc)2 with 2 equiv of TabHPF6 [TabH = 4-(trimethylammonio)benzenethiol] in MeCN/MeOH afforded a mononuclear linear complex [Hg(Tab)2](PF6)2 (1). By using 1 as a precursor, a new family of mercury(II) zwitterionic thiolate complexes, [Hg2(Tab)6](PF6)4.2MeCN (2.2MeCN), [Hg(Tab)2(SCN)](PF6) (3), [Hg(Tab)2(SCN)2] (4), [Hg(Tab)I2] (5), {[Hg(Tab)2]4[HgI2][Hg2I6]}(PF6)2(NO3)4 (6), [Hg(Tab)2][HgI4] (7), [Hg(Tab)2][HgCl2(SCN)2] (8), [Tab-Tab]2[Hg3Cl10] (9), and [Hg2(Tab)6]3(PF6)Cl11 (10), were prepared and characterized by elemental analysis, IR spectra, UV-vis spectra, 1H NMR, and single-crystal X-ray crystallography. The [Hg2(Tab)6]4+ tetracation of 2 or 10 contains an asymmetrical Hg2S2 rhomb with an inversion center lying on the midpoint of the Hg...Hg line. The Hg atom of the [Hg(Tab)2]2+ dication of 3 is coordinated to one SCN-, forming a rare T-shaped coordination geometry, while in 4, the Hg atom of [Hg(Tab)2]2+ is coordinated to two SCN-, forming a seesaw-shaped coordination geometry. Through weak secondary Hg...S coordinations, each cation in 3 is further linked to afford a one-dimensional zigzag chain. The trigonal [Hg(Tab)I2] molecules in 5 are held together by weak secondary Hg...I and Hg...S interactions, forming a one-dimensional chain structure. In 6, the four [Hg(Tab)2]2+ dications, one HgI2 molecule, one [Hg2I6]2- dianion, one PF6-, and four NO3- anions are interconnected by complicated secondary Hg...I and Hg...O interactions, forming a scolopendra-like chain structure. The secondary Hg...I interactions, [Hg(Tab)2]2+ and [HgI4]2- in 7, are combined to generate a one-dimensional chain structure, while [Hg(Tab)2]2+ and [HgCl2(SCN)2]2- in 8 are interconnected by secondary Hg...N interactions to form a one-dimensional zigzag chain structure. Compound 9 consists of two [Tab-Tab]2+ dications and one [Hg3Cl10]4- tetraanion. The facile approach to the construction of 2-8 and 10 from 1 may be applicable to the mimicking of a coordination sphere of the Hg sites of metallothioneins.     

Reaction of Mo(CO)_6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et_4N]_3[Mo_2(CO)_6(μ-OC_6H_4OCH_2C_6H_5)_3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a = 15.359(2), b = 18.378(3), c = 24.952(2), β = 102.268(4)°, V = 6882.3(16) 3, Mr = 1348.34, Z = 4, Dc = 1.301 g/cm3, F(000) = 2832 and μ = 0.424 mm-1. The final R = 0.0606 and wR = 0.1552 for 9396 observed reflections (I > 2σ(I)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) , indicating no metal- metal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

Synthesis and Structural Characterization of [Cu(DMF)_6][(η~5-C_5Me_5)WS_3(CuBr)_3]_2·Et_2O

1 INTRODUCTION In the last decade, we have been interested in the synthesis of [PPh4][(h5-C5Me5)MS3] (M = Mo, W)[1, 2] , Whose organometallic trisulfido anions show high reactivity towards various transition metals[3~6] . We once reported that the reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CH3CN afforded a double incomplete-cubane cluster [PPh4]2[(h5-C5Me5)WS3(CuBr)3]2[3], while the analogous reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CHCl3 gave rise to a 揻our-…     

Synthesis and Structural Characterization of a Salt{[Co(Phen)3][Mo2S2(μ-S)2(edt)2]}2·(DMSO)2·(Et2O)(Phen = 1,10-Phenanthroline,edt = Ethane-1,2-dithiolate)

Reaction of [Et4N]2[Mo2S2(μ-S)2(edt)2] with CoCl2(6H2O and Phen in MeCN followed by recrystallization in DMSO/Et2O gave rise to dark-red block crystals of {[Co(Phen)3]- [Mo2S2(μ-S)2(edt)2]}2·(DMSO)2·(Et2O) 1 (C88H86Co2Mo4N12O3S18). 1 crystallizes in the monoclinic system, space group P21/c with a = 24.631(4), b = 16.117(3), c = 24.791(4) (A), β = 92.835°, V = 9829.3(3) (A)3, Z = 4, Mr = 2438.57, Dc = 1.648 g/cm3, F(000) = 4928, μ = 12.61 cm-1, R = 0.0936 and wR = 0.1682 for 12998 observed reflections with I > 2.0σ(I). In the structure of 1, the Co atom of the [Co(Phen)3]2+ dication is octahedrally coordinated by three Phen ligands. The Mo atom of the [Mo2S2(μ-S)2(edt)2]2- dianion is coordinated by two μ-S, one terminal S and two S atoms from edt, forming a distorted square pyramidal geometry. The mean Co-N and Mo…Mo bond distances are 2.139 and 2.872 (A), respectively.     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group─Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2 (C18H22Cl4Cu2N6), has been synthe- sized and characterized by X-ray structure determination. It crystallizes in the triclinic P1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3) , α = 117.214(10), β = 108.251(9), γ = 91.560(6)o, V = 562.3(4) 3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(II) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(II)-Cu(II) binuclear entity with the distance between two copper(II) atoms of 3.398 .     

A New Two-dimensional Copper（II） Complex with p-PhDTA Bridges

A new p-PhDTA bridged Cu（II） complex [Cu2（p-PhDTA）（DMSO）2]·4DMSO （p-PhDTA = p-phenylenediamine-N,N,N,N＇-tetraacetic acid） has been synthesized and structurally characterized. The crystal belongs to orthorhombic, space group Pca21 with a = 19.572（4）, b = 19.552（4）, c = 10.156（2）A, C26H48N2O14CU2S6, Mr = 932.10, V = 3886.4（13）A3, Z = 4, Dc = 1.593 g/cm^3, F（000） = 1936, λ（MoKa） = 0.71073A,μ = 1.480, R = 0.0487 and wR = 0.1151 for 8464 observed reflections （I 〉2σ（I））. In the complex, the oxygen atoms of carboxylate of p-PhDTA connect the Cu atoms in a syn-anti type, giving one-dimensional chains which are further linked by the benzene groups ofp-PhDTA to form a novel two-dimensional structure.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…     

Synthesis and Crystal Structure of exo-4-（3,4-Dichlorophenyl）-8-ethyl-3,3a,4,5,8, 12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline

The title compound exo-4-(3,4-dichlorophenyl)-8-ethyl-3,3a,4,5,8,12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline (C25H22Cl2N2O, Mr = 437.35) was synthesized and crystallized. The crystal belongs to tetragonal, space group I4(1)/a with a = 17.4903(3), b = 17.4903(3), c = 28.3403(5) , Z = 16, V = 8669.6(3) 3, Dc = 1.340 g·cm-3, μ(MoKɑ) = 0.319 mm-1, F(000) = 3648, R = 0.0429 and wR = 0.711 for 2714 observed reflections I > 2σ(I). X-ray analysis reveals that atoms C(1), C(2), C(3), C(4), C(5) and N(1) on the new pyridine ring are slightly distorted, forming a distorted boat conformation.     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C_(13)H_9N_2O)Cl]_2·(CH_3CN)_2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .     

Syntheses and Crystal Structures of Two New Nickel（Ⅱ） Complexes with Salicylidene-2-ethanolamine

Two new Schiff base complexes of nickle(Ⅱ) [C18H20NiN2O4]·1.5H2O(1) and [C18H20N2NiO4]·H2O(2) were synthesized and characterized by elemental analysis,IR,UV-Vis and X-ray crystal structure analysis.Both 1 and 2 crystallize in the orthorhombic system.Crystal 1:space group Pbcn with a = 12.8591(19),b = 14.779(2),c = 19.749(3) ,V = 3753.3(10) 3,C18H23N2NiO5.5,Mr = 414.07,Z = 8,Dc = 1.445 g/cm3,μ = 1.067 mm-1,F(000) = 1712,S = 1.037,the final R = 0.0741 and wR = 0.2101 for 4353 observed reflections(I > 2σ(I)) and R = 0.1157 and wR = 0.2380 for all data.Crystal 2:space group P21 with a = 9.4673(17),b = 11.559(2),c = 16.347(3) ,V = 1788.9(6) 3,C18H22N2NiO5,Mr = 405.07,Z = 4,Dc = 1.497 g/cm3,μ = 1.116 mm-1,F(000) = 840,S = 1.085,the final R = 0.0330 and wR = 0.0869 for 3151 observed reflections(I > 2σ(I)) and R = 0.0362 and wR = 0.0887 for all data.Each Ni atom of 1 and 2 is six-coordinated with two nitrogen atoms and four oxygen atoms from two salicylidene-2-ethanolamine ligands yielding a distorted octahedral geometry.Dimer structure is observed in the packing diagram of 1.The thermal stability of complex 2 is also studied.     

Synthesis and Crystal Structure of 3,3＇-Bis（2-benzimidazolyl）-2,2＇-dipyridine with Hydrated Zinc（Ⅱ） Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(II) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr = 1259.38) belongs to the monoclinic system, space group C2/c with a = 20.874(2), b = 14.9953(16), c = 20.462(3) , β = 101.553(2)°, V = 6274.8(13) 3, Z = 4, Dc = 1.333 g/cm3, F (000) = 2608, μ(MoKα) = 0.548 mm–1, R = 0.0682 and wR = 0.1931 for 4984 observed reflections with I > 2σ(I). The Zn(II) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2+ cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

Synthesis and Crystal Structure of a Molybdenum Carbonyl Compound with Thiolate and Dithiocarbamate Ligands,[Bu4N][(OC)4Mo(μ-SC6H5)2Mo(C5H10CNS2)(CO)2]

A di-molybdenum carbonyl compound containing thiolate and dithiocarbamate li- gands, [Bu4N][(CO)4Mo(μ-SC6H5)2Mo(C5H10dtc)(CO)2] 1 (C5H10dtc = S2CNC5H10), has been pre- pared by reaction of [Mo2(SC6H5)2(CO)8] with C5H10dtcNa and [NBu4]Br in acetone. It crystallizes in monoclinic, space group P21/n with a = 13.162(3), b = 17.466(2), c = 20.453(4)(A),β = 100.77(1)°, Z = 4, V = 4619(2)(A)3, C40H56Mo2N2O6S4, Mr = 980.95, Dc = 1.389 g/cm3, μ= 7.66 cm-1, F(000) = 1988 and R = 0.0746 for 5161 observed reflections with I > 2σ(I). The complex contains a [Mo2S2]2- planar core in which one Mo atom is chelated by a C5H10dtc ligand, leading to different coordination environments of the two Mo atoms. 95Mo NMR measurement indicates that the two Mo atoms are in different oxidation states.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis and Crystal Structure of a Novel 1D Magnesium(II) Coordination Polymer Constructed by L-Cysteic Acid

A novel coordination polymer [Mg(L)(H2O)2]·H2O] (LH2 = L-cysteic acid) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal crystallizes in orthorhombic system, space group P212121, with a = 5.962(3), b = 11.224(6), c = 13.664(7) , V = 914.3(8) 3, Z = 4, Mr = 245.50, Dc = 1.783 g/cm3, μ = 0.445 mm–1, flack parameter = 0.32(16), F(000) = 512, the final R = 0.0458 and wR = 0.1172 for 1578 observed reflections with I > 2σ(I). The Mg(II) atom shows an octahedral geometry defined by two carboxyl O atoms from two different L-cysteic acid ligands, one carboxyl O atom and one amino N atom from the adjacent ligand, and two aqua ligands. The Mg(II) atoms are bridged by L-cysteic acid ligands, leading to a 1D infinite zigzag chain. In the structure there are extensive hydrogen bonds, through which the complex completes its 3D framework structure.     

Synthesis and Crystal Structure of catena-Poly[bis-(benzimidazole)cobalt(II) μ-Phthalato]

1 INTRODUCTION Chemists have recognized that intermolecular inter- actions are the basis of functional properties for most molecular assembles, and detailed understan- ding of non-covalent chemistry is therefore funda- mental to interpreting and predicting the relation- ship between structure and function. Among intermo- lecular interactions, the π-π stacking between aro- matic rings is correlated with the electron transfer process in some biological systems[1], and the nature of π-π s…     

Syntheses and Crystal Structure of [Cu（pyr）3].Hg2I6

1INTRODUCTIONThepolynucleard10metalcomplexesarepotentialluminescentsensormaterialsduetotheirattractivephotochemicalandphotophysicalpro-perties[1,2].Lowdimensionalmetal-organichalidecomplexeshavereceivedever-interestingattentioninrecentyearsfortheirpotentialapplicationsaselectronicandcatalyticmaterials[3,4].RecentlyHomo-metaloligomersandthechainsofcopperhavebeenreportedbyZubietaandthecoworkersviahydrothermalsyntheses[5,6].Theexistingexamplesofcopperwithmercuryareextremelyrare[7].Intherece…     

From Chain to Layer Structure: Zn~(II) Coordination Polymers Derived from Diphenic Acid

1 INTRODUCTION The rational design and synthesis of metal-organic coordination polymers have generated considerable interest in supramolecular chemistry and material science owing to their intriguing structural diver- sities and potential applications as functional mate- rials[1～3]. Up to now, some structural motifs with specific topologies and functions have been con- structed through rational combination of organic li- gands containing appropriate coordination sites and metal ions beari…