CRYSTAL STRUCTURE OF (NH_4)_(11)[Na(H_2O)_2P_4W_(14)O_(58)] ·12H_2O

<正> (NH4)11[Na(H2O)2P4W14O58)·12H2O, Mr = 4099. 39, triclinic, space group P1, a = 14. 376(2), b = 19.861(9), c=13. 010(3)(?) , α=104. 68(2), β=91. 37(1), γ= 104. 05(2)°, V = 3471. 1 (?)3, Z = 2, Dc=3. 922g/cm3, μ (MoKα) = 238. 274cm-1, F(000) = 3664, R = 0.0510, Rw = 0. 0665 for 9260 observed reflections with I> 3σ(I). The polyanion [Na(H2O)2P4W14O58]11- consists of two PW7O29 subunits anisostructurally, two linkage phosphorous atoms and one sodium ion with two water ligands as well. The geometries of tungsten atoms within these two subunits are almost the same as those in K12P4W14O58· 21H2O[2]. The four phosphorous atoms are in PO4 coordinations. The sodium ion locates nearly at the center of the polyanion, and is coordinated by two water molecules, five oxygen atoms of the anion and one phosphorous atom with Na-P = 3. 053(3) (?). Due to the presence of the sodium atom, the interactions between oxygen and tungsten atoms in the polyanion are somewhat weakened.     

SYNTHESIS, STRUCTURE AND PROPERTIES OF Na_3[V_2O_3(nta)_2]·5H_2O

<正> Compound Na3 [V2O3 (nta )2 ]·5H2O (1) (ntaH3 = N (CH2CO2H)3) has been prepared by reduction of a mixture of (NH4)2[VO(O2)2Cl] and H3(nta) in H2O with Na2S2O4. The compound crystallizes in the triclinic system, space group P1 with Mr = 685. 2, a = 11. 050(6), b=12. 179(4), c=9. 792 (3)A,α=111.71(2),β= 98. 23(3), γ= 89. 36(2)°, Z=2, V = 1210. 5A3,λ(MoKa) = 0. 71069 A, F(000) = 694 and DC = 1. 880g/cm3. The structure was solved by direct methods and refined by full-matrix least squares to final R and Rw values of 0. 055 and 0. 065, respectively.The structure of the anion can be considered as two [VO(nta)] fragments connected by one μ2-O atom. Each vanadium atom in the fragment is coordinated by one vanadyl oxygen atom, one bridging-oxygen atom, three oxygen atoms and one nitrogen atom from (nta) ligand in a distorted octahedral geometry. In this paper, we have studied the conversion of compound 1 to mononuclear compound Na2[VO(O2) (nta)]·5H2O (2) by oxidation with hydrogen peroxide, as well as thei     

CRYSTAL STRUCTURE OF (Et_4N)_2[Mo_6O(μ-O)_(12)O_5]

<正> Mr= 1140.4, tetragonal,P4/mnc,a=10.726(2), c=14.208(3)A, Z=2,Dc=2.316 g.cm-3,V=1634.5(9)A3,final R=0.050 for 1457 independent reflections. The anion [Mo6O19]2- has its No atoas in octahedral configuration with one oxygen atom situated in the center of the octahedron, twelve bridging oxygen atoms,and six terminal oxygen atoms. The average bond lengths of the three types of Mo-O bonds are 1.678 A (Mo=0), 1.919A [Mo-(μ-O)], and 2.310 A [Mo-(μs-O)], respectively.     

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) .     

CRYSTAL STRUCTURE OF UO_2(PMBP)_2(H_2O) THF

<正> C34H28N407U·C4H4O Mr=910.7, monoclinic, Cc, a=12.999(1), b=15.448(2), c=18.481(2) A, β=100.18(2)°, Z=4, DC=1.656 g/cm-3, V=3652.3 A3, final R = 0.035 for 3457 observable reflections. Uranyl ion is coordinated equatorially by four oxygen atoms of PMBP and one oxygen atom of water in a distorted pentagonal bi-pyramid.     

CRYSTAL STRUCTURE OF CK(C_(12)H_(24)O_6)]_2Pd(SCN)_4(H_2O)

<正> [K(C_12H_24O_6)]_2Pd(SCN)_4(H_2O),MT=963.59,monoclinic, P21/n,a= 11. 075(1),b= 12. 231(1),c= 15. 863(2) A ,β=93. 25(1)°,V=2145. 3A3,Z=2, Dc=1. 492gcm-3,λ(MoKa) = 0. 71073A μ=8. 64cm-1,F(000) = 996,final R=0. 045 for 1835 observable reflections. The Pd2+ ion coordinates with four S atoms from SCN- groups forming a regular square planar configuration. The K+ ion is surrounded by six ether oxygen atoms,one O atom from water molecule coordinated to two K+ions and one N atom from SCN- group to form a distorted hexagonal bipyramid. Two K atoms are linked with one Pd atom by two bridging SCN- groups forming a chain molecular array in the crystal.     

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

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

THE PREPARATION AND CRYSTAL STRUCTURE OF IMIDAZOLATE BRIDGED HETEROTRINUCLEAR COMPLEX [ (NH_3)_5 RhlmZn ( dien )-ImRh(NH_3)_5(C10_4)_6·4H_2O

<正> The imidazolate bridged heterotrinuclear complex [(NH3)5RhImZn(dien)-ImRh(NH3)5](ClO4)6·/4H2O,Mr= 1347. 56,was prepared and crystallized in the mono-clinic space group C2/c with unit cell constants, a = 32. 972 (4) , b = 9. 482 ( 1) , c = 15. 250(3) A ,β = 91. 26(1)°,V = 4766. 6A3 and Z=4. The structure was determined from 9043 independent reflections and refined to R=0. 049 for 3051 observed MoKa reflections. The Zn atom showed a distorted trigonal bipyramid coordination, being bonded to three nitrogen atoms of dien and two of imidazole. Each imidazole anion bridged one Zn atom and one Rh atom. The Rh atom was coordinated by six nitrogen atoms,one of which is from imidazole and the five others from NH3 forming a regular octahedral coordination.     

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex:[Co2(2,2'-bpy)_2(μ-L)_2(L)_2(μ-H_2O)](HL=4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2'-bpy)2(μ-L)2(L)2(μ-H2O)] (HL=4-chlorobenzoic acid) has been obtained by hydrothermal synthesis,and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system,space group C2/c with a=22.537(5),b=16.212(3),c=15.306(3) ,β=124.37(3)°,V=4616.1(16) 3,Mr=1070.45,Dc=1.540 g/cm3,Z=4,μ=1.012 mm-1,F(000)=2176,the final R=0.0338 and wR=0.0810. The title complex is composed of dinuclear [Co2(2,2'-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand,three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS [4,4,4-TRIFLUOR-1-(2-THIENYL) Butandion-1,3] COPPER (Ⅱ) WITH DIMETHYLFORMAMIDE, [Cu(TTA)_2(DMF)]

<正> [Cu(C8H4F3O2S)2(C3H7NO)], Mr = 579. 0, monoclinic, P21/c, a = 9. 4851(6), b = 26. 6574(6), c=9.2619(6) A ,β=96.08(3)°, V = 2328.7A3, Z=4, Dc=1. 65gcm-3, μ(MoKa) = 7. 2cm-1, F (000) = 1172, MoKa radiation, final R = 0. 074 and Rw = 0. 068 for 1841 reflections with I≥3σ(Ⅰ). The Cu(Ⅱ) atom is coordinated by five oxygen atoms, one of which from DMF is in the axial position, to form a square pyramidal geometry. That the thenoyl groups in the ligands take the cis-form around the Cu(Ⅱ) atom is explained by the hydrogen bonding effect.     

SYNTHESIS AND STRUCTURE OF DIAQUO-μ-TRIETHYLENETE-TRA AMINOHEX A ACETATODI ANTIMONY ( Ⅲ) , C(H_2O)Sb(ttha)Sb-(H_2O)]

<正> C_18H_28N_4O_14Sb_2, MT = 767. 94, monoclinic, space group P2_1/c, a = 13. 847(2),b=6.866(2),c=13. 846(2) A,β=116. 46(1)°,V=1180. 3A3,Z=2,Dc = 2. 161g/cm3, F(000) = 756,μ(MoKa) = 23. 83cm-1. R and Rw were 0.054 and 0. 060, respectively, for 1357 observed reflections at room temperature. Each binuclear complexes arranged so that the centre of the carbon-carbon bond in the ethylenediamine group lies on a crystallographic centre of inversion. The ethylenediamine group forms a bridge between the two halves of the title molecule. Each antimony atom is ψ-heptacoordi-nated by a lone electron pair,one O atom from a water molecucle,one O atom from an ac-etato group and two amino N atoms at the equatorial plane as well as two O atoms from the acetato groups at the axial positions forming a pentagonal bipyramid.     

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex: [Co2(2,2(')-bpy)2((-L)2(L)2(μ-H2O)] (HL = 4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ- H2O)] (HL = 4-chlorobenzoic acid) has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537(5), b = 16.212(3),c = 15.306(3)(A), β= 124.37(3)°, V = 4616.1(16) (A)3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, μ = 1.012 mm-1, F(000) = 2176, the final R = 0.0338 and Wr = 0.0810. The title complex is composed of dinuclear [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Unexpected Synthesis and Crystal Structure of Macrocyclic Nickel Complex Involving Rare S-Cl Bond

A novel complex of [NiL(OOCNH2C2H3SClO3)]·H2O was obtained unexpectedly by the reaction of [Ni(rac-L)](ClO4)2 with l-cysteine (L=5,5,7,12,12,14-hexamethyl-1,4,8,11-tetra- azacyclotetradecane), and characterized by EA, IR, ESI-MS and single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121 with a=9.211(12), b=14.942(19), c=19.002(2), Mr=563.80, V=2615.3(6)3 , Z=4, Dc=1.432 g/cm3 , F(000)=1204, μ=0.966 mm-1 , the final R=0.0565 and wR=0.1515. The central nickel(Ⅱ) ion displays a distorted six-coordinate octahedral coordination geometry by coordination with four nitrogen atoms of L, and one oxygen and one nitrogen atoms of l-cysteine. The sulfur atom of l-cysteine instead of oxygen atom links directly with the chlorine atom of perchlorate. The title complex is the first example of perchlorate salt involving the sulfur atom.     

CRYSTAL AND MOLBCULAR STRUCTURE OF MoO_2(Oxine)_2

<正> MoO2(C9H5NOH)2, Mr = 396,monoclinic,space group Cc,a = 13.369 (6), b = 9.408(4), c = 13.560(3)A,°=109.65°,V=1605A3,Z= 4,Dc= 1.639 g/cm3.R=0.027 for 1372 observed reflections [I>3o(I)]. X-ray analysis showed that the coordination sphere around molybdenum atom has a distorted octahedral geometry with two terminal oxygen atoms arranged in cis-form and two oxines act as bidentate ligands connected to the molybdenum through O and N atoms.Therefore, the molecule is not as Atovmyan described that the molybdenum atom is located on two-fold axis with space group C2/c but only approxiaately C2 synmetry.     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRAAQUA TRIM TRATO SAMARIUM(Ⅲ) DIHYDRATE [Sm(H_2O)_4(NO3)_3] ·2H_2O

<正> [Sm(H2O)4(NO3)3]·2H2O,Mr=444. 46,triclinic,space group P1 ,a = 6.747(1),b=9. 156(1),c=11.673(l) A ,α= 69. 90(1),β=88. 88(1),γ=69. 29 (1)°,V = 629.0A3,Z=2,λ(MoKa) = 0. 7107A,F(000) = 430,Dx=2. 346/cm3,final R=0. 032. The Sm atom in the title complex has bicapped square antiprismtic coordination of oxygen atoms from four water molecules and three NO3 groups. The Sm -O(nitrato) and Sm-O(aqua) distances are in the ranges of 2. 517-2. 716 and 2. 407-2. 432A , respectively. The N-O bond lengths vary between 1. 209 and 1. 265 A with the shortest distances being those involving noncoordinated oxygen atoms. The two lattice water molecules are outside the coordination sphere of the Sm atom but participate in the network of intermolecular hydrogen bonds.     

Synthesis and Crystal Structure of a New Complex {[Co~(Ⅲ)L_2]·[Co~(Ⅱ)(H_2O)_6]_(0.5)·2.25H_2O}_4 (H_2L = N-(2-Hydroxyphenyl)salicylidenimine)

The reaction of Co(OAc)2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of {[CoIIIL2]·[CoII(H2O)6]0.5·2.25H2O}4 1 (H2L = N-(2-hydroxyphenyl) sali-cylidenimine). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104H114Co6N8O37, Mr = 2421.61, a = 10.625(3), b = 16.335(4), c = 15.265(4) , β = 102.990(4)o, V = 2581.6(11) 3, Z = 1, Dc = 1.558 g/cm3, μ = 1.034 mm-1, F(000) = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co(III) atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra-molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

SYNTHESIS, CHARACTERIZATION AND STRUCTURE OF [Co(DBP)_2·3Py]_2·2CHCl_3

The mixed ligand complex of cobalt with dibutylphosphate (HDBP) and pyridine has been synthesized. Elemental analysis yields the result that the formula of this compound is Co(DBP)_2·3Py·CHCl_3 (Py=pyridine). The thermal analsyis, visible spectra and magnetic properties of it have been studied as well. Single crystal structural analysis shows that the crystal is triclinic with space group P and the unit cell parameters are as follows:a=14.490(10), α=90.37(4)°,b=15.721(7), β=96.04(5)°,c=20.109(12), γ=105.63(4)°.The final R factor is 0.0773. Two Co atoms are connected by two bridging DBP groups to form a dinuclear molecule [Co(DBP)_2·3Py]_2 which has a C_s, symmetry. Each cell contains two dinuclear molecules and four chloroform molecules. The cobalt is coordinated in an octahedral arrangement by three oxygen atoms and three nitrogen atoms, of which one oxygen atom comes from a monodentate DBP group, two oxygen atoms from two bridging DBP groups, and the three nitrogen atoms from the three pyridi