CRYSTAL STRUCTURES OF Ln(o-HOC_6H_4CO_2)_3 (H_2O)_2·2H_2O [Ln =Tb,Ho]

<正> Ln(o-HOC6H4CO2)3(H2O)2·2H2O [Ln = Tb, Ho], Mr = 642. 32 (648. 33 )**,monoclinic, space group Cc,a=16. 280(4)(16. 217 (2)) ,b= 14. 889(3) (14. 877(2)),c = 9.867(1)(9. 835(2)) A,β=101.49(1)(101. 46(1))°,Z= 4,V= 2343. 8(7)(2325. 3(6)) A3,Dc=1. 8(1. 85)g·cm-3,μ=31. 6(36. 1)cm-1(MoKa), F(000) = 1272(1280).The final R=0. 031(0. 031),Rw = 0. 029(0. 031). There is no discrete molecules of the compounds in the crystal structures. The compounds are in linear polymeric arrangements, each metal ion is bridged to the next by two bridging carboxyl groups from salicylato ions.     

PREPARATION AND CRYSTAL STRUCTURES OF Ln_2(S0_4)_3(H_2O)_4 (Ln=La COMPOUND Ⅰ;Nd,COMPOUND Ⅱ)

<正> The title crystal structures have been determined by X-ray diffraction. They crystallize in the monoclinic, space group P21/n, Z=4 with diaensions a= 12.388(1), b= 7.140(1), c= 14.302(1) A,β=90.65(1)° for compound Ⅰ, and a=12.987(2), b= 7.190(1), c=13.284(2) A,β=92.40(2)° for compound Ⅱ. The structures were solved by direct methods, and refined by full matrix least-squares to consistence factors R=0.026 for Ⅰ and R=0.031 for Ⅱ.     

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.     

CRYSTAL STRUCTURE OF [Tm_4(p-NO_2C_6H_4CO_2)_(12)(H_2O)_(10)·2H_2O

<正> [Tm4 (p-NO2C6H4CO2)12 (H2O)10]·2H2O, Mr = 2885. 28, triclinic, space group P1 with a=14. 109(4) ,b= 14. 594(3) ,c= 13. 638(3) A ,α= 107. 04 (2), β=103. 36(2),γ= 93. 93(2)°, Z=1,V = 2584(1) A3.F(000) = l416,μ = 36. 4cm-1(Moka) ,Dc=1. 85g·cm3. The final R factor is 0. 034. The crystal structure is composed of tetrameric units in which four metal ions are bridged by carboxyl groups in chain form.     

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.     

CRYSTAL STRUCTURE OF Co(H_2O)_3SO_4(phen)

<正> PRELIMINARY INFORMATION. The title compound is a member of a series of cobalt complexes of polydentate ligands currently being investigated. It was prepared by the reaction of CoSO_4·7H_2O with phenanthroline in the equimolar ratio.     

CRYSTAL STRUCTURE OF Ba[Co(EDTA)]_2·6H_2O

<正> INTRODUCTION. The crystal structures of a number of metal complexes of ethlenediaminetetraacetic acid (EDTA) have been reported. As a versatile ligand, EDTA molecule is known to have several different coordination forms.     

CRYSTAL STRUCTURE OF [Eu_2(Met)_3(Gly)(H_2O)_3](ClO_4)_6

<正> The crystal structure of [Eu2(Met)3(Gly)(H2O)2](ClO4)6(Met=CH3-S(CH2)2CHNH2COOH, Gly=NH2CH2COOH) belongs to monoclinic system with space group P21/n.The final R is 0.060. The Met and Gly are bonded as bidentate bridging ligands to Eu(III) atoms.     

稀土配位聚合物{(H_2prz)[Ln_2(pzdc)_4(H_2O)_2]·5H_2O}_n(Ln=Eu,Tb)的合成、结构和性质

以Ln(NO3)3、H2pzdc(2,3-吡嗪-二羧酸)和prz(哌嗪)为原料,在水热条件下得到了2个结构新颖的稀土配位聚合物{(H2prz)[Ln2(pzdc)4(H2O)2]·5H2O}n(Ln=Eu(1),Tb(2))。对它们进行了元素分析、红外光谱、粉末X-射线衍射、热重等分析,并用X-射线衍射测定了它们的单晶结构。2个配合物的晶系都属于三斜晶系,P1空间群。研究了它们的荧光性质,固体荧光实验测试结果表明,2个配合物在室温下均表现出相应稀土离子的特征荧光发射。     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

CRYSTAL STRUCTURE OF COMPLEX OF ERBIUM(Ⅲ) AND QLYCINE,[Er(GLy)_2(H_2O)_4]_2(ClO_4)_6·4(C_4H_8O_2)

<正> The crystal structure of [Er(Gly)2 (HaO)4]2(ClO4)6.4(Dio) (Gly= NH2CH2COOH; Dio=dioxane) has been determined belonging to triclinic system with space group P1.The final R was 0.055. The carboxyl groups of Gly are associated to Er(Ⅲ) atoms to act as the bidentate bridging ligands.     

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.     

CRYSTAL STRUCTURE OF A HETERONUCLEAR LANTHANIDE COMPLEX OF ERBIUM-YTTRIUM AND GLYCINE[ErY(GlY)_6(H_2O)_4](ClO_4)_65H_2O

The title complex [ErY(Gly)_6(H_2O)_4](ClO_4)_6 5H_2O has been synthesized.Its crystalstructure has been determined by X-ray diffraction method.The crystal is triclinic with space groupP1.The unit cell parameters are as follows:a=11.518(4),b=14.105(7),c=15.530(6) ,α=96.61(3),β=102.74(3),γ=105.70(3)°,V=2327.7(17) ~3,Z=2,Dc=2.091g/cm~3.The structure has been refinedto a final R of 0.0785.The crystal is an infinite chain complex,in which four carboxyl groups fromglycine molecules bridge the Er(Ⅲ)and Y(Ⅲ)ion,other two carboxyl groups bridge two adjacentEr(Ⅲ)or two Y(Ⅲ)ions.     

CRYSTAL STRUCTURE OF ERBIUM (HI) COMPLEX WITH 5-SUL-FOSALICYLIC ACID[Er (SO_3C_8H_3(OH)CO_2) (H_2O)_7] [Er (SO_3C_6H_3-(OH)CO_2)_2(H_2O)_6]·8H_2O

<正> [Er(SSA)(H2O)7][Er(SSA)2(H2O)6]·8H2O (H2SSA = 5-sul-fosalicylic acid), Mr=1361.3, monoclinic,P21/c, a = 21.459(7), b = 10.125(2), c = 22. 033(5)(?), β=109. 07(2)°, V = 4524(2)(?)3, Z = 4, D,= 1. 998g/cm3, μ (MoKa) = 40. 6cm-1, F(000)=2704, R = 0. 038 for 5805 observed reflections. The Er(Ⅲ) ions in-both complex cation and anion are coordinated by unidentate SSA ligand(s) and water molecules in a trigondodecahedral geometry. The coordination polyhedra are connected with each other by hydrogen bonds involving the uncoordinated carboxylato oxygen atoms and the coordinated water molecules. Stacking interactions between the phenyl rings further stabilize the structure.     

CRYSTAL STRUCTURE OF [Eu(μ-CH_3COC-O)(CH3COO)_2(H_2O)_2]_2·4H_2O

<正> C12H34O20Eu2,Mr=802.30 triclinic, space group P1, a= 8.955(2), b=9.328(1), c=10.536(2) A,α= 91.74(2),β=113.87(2),γ=118.23(2), V=681.7(2)A,Dm(flotation in CC14/ BrCH2CH2Br)=1.95,DX(Z=1) =1.954g cm-3,λ(MoKα)=0.71069 A,μ=6.41 cm-1,F(OOO)=391.92, T =. 295°K,final RF= 0.032 for 7483 observed reflections with |F0|>3a(|Fo|). The compound is isostructural with the known erbium complex,the basic unit being a centrosymmetric dimer composed of two nine-coordinate polyhedra sharing a common edge. An O atom in one or the three bidentate acetato groups about each europium atom serves as a bridge between the metal centars. The dimeric units are linked by hydrogen bonds involving both ligand and lattice water molecules to form a three-dimensional network.     

Syntheses and Crystal Structures of(H_3O)(C_3H_5N_2)[Mn(OH)_6Mo_6O_(18)]·3.5H_2O and (H_3O)_3[Co(OH)_6Mo_6O_(18)]·7H_2O

1 INTRODUCTION Polyoxometalates, a rich and remarkable classof inorganic cluster system[1], exhibit diverse appli-cation possibilities due to their topological and elec-tronic properties, ranging from their well-known roleas reagents in analytical, b…     

CRYSTAL STRUCTURE OF RhCl(dppm)_2·H_2O

<正> C50H46OP4ClRh, RhCl(dppm)2 · H2O, Mr = 922. 2, monoclinic, P21/2, a=10. 532(3), b=22.574(8), c=18. 641(8) A, β=93. 41(3)°, V = 4424 (3) A3, Z = 4, Dc=1. 386 g. cm-3, λ(MoKα) = 0. 71073A , F(000) = 1904. The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares to final R = 0. 037 and Rw = 0. 036 for 3432 (F> 6. 0σ(F) ) observed reflections. The structure of the title compound contains RhCl-(dppm)2 and non-coordinated H2O molecules. The rhodium atom is coordinated by one chlorine atom and four phosphorus atoms of two DPPM ligands forming a tetragonal pyramidal configuration.     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

CRYSTAL STRUCTURE OF DI(α-HYDROXYISOBUTYRATE)DIAQUO NEODYMIUM NITRATE Nd(C_4H_7O_3)_2NO_32H_2O

The crystal structure of di(-hydroxyisobutyrate)diaquo neodymiumnitrate Nd(C_4H_7O_3)_2NO_32H_2O was determined by X-ray diffraction analysis.It belongs to monoclinic,space group C2/C,with cell dimensionsa=8.996(1),b=8.601(1),c=21.111(3),β=92.38°,V=1632.O,Z=4,D_c=1.83g/cm~3.Crystalstructure has been refined by full-matrix least-square techniques giving afinal R value of 0.036.The neodymium atom is coordinated to eight oxygenatoms.The nitrate group in complex is not bonded to neodymium,each twoneodymium atoms are linked by bridging carboxyl group forming a chainpolymeric molecule.