Crystal structure and single crystal EPR of (NH_4)_2(15-crown-5)_3[Cu(mnt)_2] and (NH_4)_2(benzo-15-crown-5)_4[Cu(mnt)_2]·0.5H_2O

The X-ray crystal structures of (NH4)2(15-crown-5)3[Cu(mnt)2] (1) and (NH4)2(benzo-15-crown-5)4- [Cu(mnt)2]·0.5H2O (2) were determined. Two single crystals are composed of distinct structures of ammonium-crown ether supramolecular cation and [Cu(mnt)2]2? anion. The triple-decker dication in complex 1 and a sandwich dimmer in complex 2 were observed. X-Band EPR studies on the single crystals of both complex 1 and complex 2 have been carried out at room temperature, which revealed that complex 2 showed a perfect hyperfine structure of Cu whereas that of complex 1 could not be observed. The principal values and direction cosines of the principal axes of the g and A tensors were computed by a least-squares fitting procedure. The spin density of Cu(II) was estimated according to the principal values of the A tensors and compared well with the results calculated based on DFT method.     

Synthesis and Crystal Structure of a Copper(II) Complex with α-Hydroxylated Acid, [Cu(C_(14)H_8O_3)(C_5H_(13)NO)(H_2O)].0.5H_2O

1 INTRODUCTION There has been considerable interest of copper(II) -hydroxylate complexes in the structural chemistry and biochemistry. There are two structural types in copper(II) -hydroxylate com- plexes: mononuclear[1~6] and dinuclear structure[7~9]. The present work is a part of our study on the copper complexes of -hydroxylated acid and reports the synthesis and structure of a mononuclear copper(II) complex with 9-hydroxy- fluorene-9-carboxylato acid, [Cu(C14H8O3)(C5H13- NO)(H…     

STRUCTURE STUDIES OF [Et_4N]_4[Cu_8(i-mnt)_6] (i-mnt=S_2C=C(CN)_2) AND [Me_4N]_4[Cu_5Ag_3(i-mnt)_6]·H_2O

<正> [Me4N]6[Ag6(i-mnt)6].H2O(1),[Et4N]4[Cu8(i-mnt)6](2) and [Me4N]4-[Cu5Ag3(i-mnt)6].H2O(3)(i-mnt=S2C=C(CN)2) were synthesized. The crystal and molecular structure of the complex 1 was reported by us.The structure of the complex 2 was determined from single crystal X-ray diffraction data. [Et4N]4[Cu8(i-mnt)s] 2, Mr=1870.46, monoclinic, P21/n, a=14.724(6), b = 17.228(3), c=15.59(1)A,β= 100.75(7)°,V=3886.3A3;Z = 2,Dc= 1.598 g/cm3. Complex 3 has been characterized by ICP elemental analyses and IR spectrum.     

HETERONUCLEAR COMPLEX CONTAINING COPPER-LANTHANIDE ARRAYS: THE SYNTHESIS AND CRYSTAL STRUCTURE OF Ln_2Cu_4L_8 (HL)_4(OH)_2(CIO_4)_4(H_2O)_(10)·2CH_3COCH_3 (Ln = Tb (1), Y (2); HL = 2-Pyridone C_5H_5NO)

Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the moleratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10)2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and thestructure was determined by four-circle diffractometer. Data showed that the crystal is in space groupC2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A~3. Thestructure was solved by a combination of Patterson method and Fourier technique. The final R value is0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form anessentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atomsare five-coordinate.     

Synthesis,Crystal Structure and Property of a Binuclear Copper Complex [Cu_2L_2(pht)_2]_2·H_2O

A new binuclear copper complex, [Cu2L2(pht)2]2·H2O(Hpht = 5,5-diphenylhydantoin, i.e. phenytoin; L = 2-diethylaminoethanol), has been synthesized by the solvothermal method, and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 31.918(3), b = 12.9222(15), c = 19.868(2) , β = 98.762(2)o, V = 8098.8(16) 3, Dc = 1.429 Mg/m3, Z = 4, F(000) = 3640, μ = 1.107 mm-1, R = 0.0560 and wR = 0.1276(I 2(I)). Each copper(Ⅱ) in a molecule is coordinated with N and O atoms from ligand L and N atom from ligand Hpht in a tetradentate manner. Moreover, two copper(Ⅱ) centers are bridged by two O atoms of hydroxyl groups from two L ligands to form a slightly distorted binuclear {Cu2O2} diamond configuration. In addition, the interaction of this complex with calf thymus DNA(CT-DNA) was investigated by UV-vis spectrum and viscometry, and the complex may bind to DNA through intercalation.     

Synthesis and Structural Characterization of {[Mn(phen)_2(OAc)(H_2O)]ClO_4}_2H_2O

1 INTRODUCTION Chemistry of manganese cluster has become an attractive research field because of the involvement of manganese in several biological redox-active sys- tems[1,2], especially in the oxygen-evolving complex (OEC) of photosystem Ⅱ (PSⅡ) in green plants[3]. It was thought that the coordination environment of Mn in OEC contains O and N donors, and the bind- ing of aqua to the Mn site may be important to the oxidation of aqua for the evolution of dioxygen[4, 5]. In recent …     

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) .     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex[La(betaine)_2(H_2O)_6Fe(CN)_6]·2H_2O

1 INTRODUCTION In the last decade, cyano-bridged Prussian Blueanalogues[1] have been intensively studied from theviewpoint of application as functionalized molecule-based magnets[2], chemical sensor materials[3], fluo-rescent materials[4] and zeolitic-type materials[5, , 6]etc. In 1976, a series of cyano-bridged three-dimen-sional rare earth hexacyanometalates(IIILnM(CN)6?nH2O (M = Fe or Cr, n = 4 or 5) were crystallized andsubjected to single-crystal X-ray analysis[7]. …     

Synthesis and Structural Characterization of Mononuclear Mn~(II) Picolilato Complex Mn(2-C_5H_4NCOO)_2(H_2O)_2.1/2CH_3CN

1 INTRODUCTION Manganese has been implicated as an essential part of the active center in various manganese enzymes. Various nuclearities have been observed from mononuclear atom in superoxide dismutase [1] to the tetranuclear atom of oxygen evolution in photosystem II[2]. The manganese active centers in biological systems are surrounded by O and N coordination sphere[3, 4]. Synthetic efforts have produced a great variety of Mn clusters with varying nuclearity and oxidation states. Si…     

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 and Structure of a Novel Macrocyclic Complex [Cd_2(phen)_4(phth)_2]·4H_2O

1 INTRODUCTION In recent years, extensively attention has been fo- cused on the design and synthesis of d10 metal- based complexes[1, 2]. A series of d10 metal-organic frame- works have been described not only because of their intriguing structures but also due to their ptential ap- plications in photoluminescent fields[3～7]. Although phthalate ligand was successfully used to design and synthesize a wide variety of metal complexes, those containing Cd(II) complex are less considered[8～…     

New Dimeric Selenidoarsenate(III):Solvothermal Synthesis and Crystal Structure of [Co(en)_3]_2As_2Se_5

1 INTRODUCTION The mild solvothermal synthesis with the presence of a structure-directing agent is proved to be a versa- tile route for the preparation of chalcogenidometa- lates of the heavier group (14 and 15) elements[1～3]. Templated by the transition metal complex cations, a large number of chalcogenidoantimonates containing transition metal complex ions have been synthesized by solvothermal method, such as Mn2(en)2Sb2S5[4], [Co(en)3]CoSb4S8[5], [M(en)3]Sb2S4 (M = Co, Ni)[6], [N…     

Synthesis and Crystal Structure of [Cu_2(DMF)(H_2O)(C_7H_4NO_4)_2(C_7H_3NO_4)]_2·3.5DMF

A new copper(II) complex [Cu2(DMF)(H2O)(C7H4NO4)2(C7H3NO4)]2·3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 10.722(3),b = 18.170(4),c = 20.923(7),α = 105.297(9),β = 101.701(10),γ = 105.74(1)°,V = 3615(1) 3,Z = 2,C58.50H64.50Cu4N11.50O31.50,Mr = 1686.90,Dc = 1.550 g/cm3,μ = 1.255 mm-1,F(000) = 1728.00,T = 150(2) K,the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I > 2σ(I).In the crystal,each formular unit consists of two dinuclear copper(II) compounds,between which the O-H···O hydrogen bonds exist.Each CuII cation is six-coordinated in an octahedral geometry.The intermolecular hydrogen-bonding interaction leads to a 3-D framework of the title compound.     

Synthesis,Crystal Structure and Thermal Stability Properties of a Binuclear Copper(Ⅱ) Coordination Polymer {[Cu_2(4,4'-bipy)_2(o-ABA)_4(H_2O)_2][(H_2O)_2]}_n

One-dimensional chain copper(Ⅱ) coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4'-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756(10),b= 1.57756(10),c=2.1438(3)nm,V=5.3352(8) nm3,Dc=1.524 g/cm3,Z=4,F(000)=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper(1) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry;the copper(2) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.     

STUDIES ON SYNTHESIS, STRUCTURE AND PROPERTIES OF THE CRYSTAL OF TRIADIC COMPLEX {Mo[S_2CN(C_2H_5)_2]_4}~( 1){FeCl_4}~(-1){C_6H_5CH_2SSCH_2C_6H_5}

In this paper, a new complex {Mo[S_2CN(C_2H_5)_2]_4}~( 1){FeCl}~(-1){C_6H_5CH_2SSCH_2C_6H_5} is syn-thesized by the reaction of MoCl_5, FeCl_3, PhCH_2SH and diethyldithiocarbamate (DTC)in MeOH. The complex is characterized by X-ray, IR, UV-visible, reflection spectra, themeasurements of magnetic susceptibility, differential thermal and elemental analyses. The crystal of triadic complex containing multi-bond species is quite stable and rare.     

INVESTIGATION ON SYNTHESIS, STRUCTURE AND PROPERTIES OF THE CLUSTER COMPLEX,[(MoS_4)Fe(MoS_4O)] [(C_4H_9)_4N]_3

In this paper, we report a new Mo-Fe-S cluster complex containing an oxygen ligand. Itwas synthesized by the reaction of (NH_4)_2 MoS_4, FeCl_3 in the solution of sodium glycol. The chemical formula of the crystal, [(MoS_4) Fe (MoS_4O)] [(C_4H_9)_4N]_3, was characterized byX-ray. This complex was determined by IR, UV/Vis and Mossbauer spectra as well. The re-suits from Mossbauer spectra of the complex show an isomer shift, δ_m = 0.2263mm/s and aquadrupole splitting, E_q = 0.4527mm/s. The complex has some activity for the reduetion of aectylene to ethylene in the presenceof KBH_4.     

Synthesis and Crystal Structure of Na_(10)[LaSiW_(11)O_(39)(H_2O)_4]_2·22H_2O

1 INTRODUCTION The pseudoliquid character of heteropoly compounds as catalysts is determined by their crystallographic properties. Study on the crystal structures of the heteropoly compounds could provide interesting information to enrich heteropoly acid and catalytic chemistry[1]. In the past, Zhuo Ying-Li抯 group has synthesized the carbamidine salts of 1:1 LnL(Ln=lanthanide, L=[SiW11O39]n－)[2], and Pope抯 group has reported that -SiW11O39 units are connected by lanthanide catio…     

Crystal structure and single crystal EPR of (NH4)2(15-crown-5)3[Cu(mnt)2] and (NH4)2(benzo-15-crown-5)4[Cu(mnt)2]·0.5H2O

The X-ray crystal structures of (NH4)2(15-crown-5)3[Cu(mnt)2] (1) and (NH4)2(benzo-15-crown-5)4- [Cu(mnt)2]·0.5H2O (2) were determined. Two single crystals are composed of distinct structures of ammonium-crown ether supramolecular cation and [Cu(mnt)2]2- anion. The triple-decker dication in complex 1 and a sandwich dimmer in complex 2 were observed. X-Band EPR studies on the single crystals of both complex 1 and complex 2 have been carried out at room temperature, which revealed that complex 2 showed a perfect hyperfine structure of Cu whereas that of complex 1 could not be observed. The principal values and direction cosines of the principal axes of the g and A tensors were computed by a least-squares fitting procedure. The spin density of Cu(Ⅱ) was estimated according to the principal values of the A tensors and compared well with the results calculated based on DFT method.     

Synthesis,Structure and Characterization of a New Complex: [Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O

A novel complex,[Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O,was synthesized and hexagonal single crystals with centimeter-scale sizes were obtained by the method of solvent evaporation.It was characterized by elemental analysis,infrared spectrum,thermogravimetric analysis and X-ray single-crystal diffraction.The complex belongs to triclinic crystal system,space group P■ with a=9.3390(8),b=13.3520(13),c=16.3207(13)?,α=100.7160(3)°,β=90.1020(10)°,γ=109.9490(5)°,V=1874.9(3)?~3,Z=2,D_c=1.542 g/cm~3,M_r=870.64,μ=0.876 mm~(-1),T=293(2) K,F(000)=916 and S=0.990.The crystal structure determination displayed a distorted octahedral geometry around the manganese atom,which is bound to two nitrogen atoms from hexamethylenetetramine,acting as monodentate ligands,and to four aqua ligands.Variable-temperature magnetic measurements of the complex indicate the presence of weak antiferromagnetic interaction between manganese centers.     

Synthesis and Crystal Structure of a Novel Zinc Complex [Zn(OH_2)(HDPA)_2]·3H_2O

1INTRODUCTION In recent years,dicarboxylic acids have been wide-ly used as poly-dentate ligands involved in various metal chelation reactions to form transition or rare earth metal complexes with interesting properties in material science[1~3]and biological systems[4~7].For example,Kim,Y.and his coworkers focus on the syn-theses of copper(II)complexes containing ligands of malonate and pyrazine to study their electronic con-ductivity and magnetic property[8].The importance of Tr(II)/dic…