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 AND MOLECULAR STRUCTURE OF [K(C_(14)H_(20)O_5)_2]_2[Co(NCS)_4]

<正> The title complex (Mr= 1442.6) crystallizes in the monoclinic, space group PC, with a =14.515(7),b =15.773(5), c =16.287(11)51,β=95.13(5)°,Z=2,V=3713.8A3,Dc=1.29 g·cm-3. The structure was solved by Patterson method and the final R=0.068. The potassium atom in the cation lies between the two planes of the oxygen atoms from two benzo-15-crown-5 molecules.     

SYNTHESIS AND STRUCTURE OF A NEW TYPE OF COORDINA-TION COMPOUND OF Gd(Ⅲ) WITH H_2 CCH_2CH_2C(~+NH_2)C-HCOO-

<正> The crystal structure of gadolinium L-proline (Pro) complex [Gd2-(C5H9NO2)6 (H2O)6] (ClO4)6 has been determined. The complex crystallizes in the triclinic space group PI with following crystal data: a = 9. 906(3), b=13. 052(5), c = 13.703(5) A. α=109. 63(3), β=110.31(2), γ=100. 73(3)°, V=1470.3(9) A3.Mr=1710. 1, F(000) = 854,μ=26. 30 cm-1, Dc = 1. 931 g/cm3, Z=1.The structure was refined to the final R of 0. 048 for 3804 reflections. The structure is of one-dimensional chain, in which each gadolinium ion lies at the center of a distorted square antiprism of the eight oxygen atoms provided by four bridging carboxylate groups from four Pro ligands, a terminal carboxylate group from one terminal Pro ligand and three water molecules and the two neighbouring gadolinium ions are linked to each other through the two bridging carboxylate groups from the two Pro ligands. The prolines exist in the form of H2 CCH2CH2(+NH2)CHCOO-, and the complexions in the crystal are linked together by the net of hydrogen bo     

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 AND MOLECULAR STRUCTURE OF BINUCLEAR Ni(Ⅱ) COMPLEX--CNi(OC_6H_4CHNCH_2CH_2OH) (CH_3COO) (H_2O)_2

<正> The title complex crystallizes in the monoclinic space group P21/n,with a = 9. 509(2),b=17. 614(6),c=15. 013(3)A ,β=95. 21(1)°,V = 2504. lA3,Mr = 599.91,Z = 4, Dx= 1. 59g/cm3, μ= 15. 66cm-1F (000) = 1248. The structure was solved by direct method and the final R=0. 060. The crystal consists of discrete molecules with symmetric center at the center of the four-member ring consisting of two Ni atoms and two 0 atoms.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

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.     

OXIDATION DECARBONYLATION OF NH_4[Mo(CO)_5I]: SYNTHE-SES AND CRYSTAL STRUCTURES OF CMo(S_2CNC_4H_8)_4]I_3 · C_7H_8 and Mo_2S_2O_2(S_2CNC4H_8)_2

<正> Both of the title complexes were produced by oxidative decarbony-lation of NH4 CMO (CO)5I]. The complexes CMo(S2CNC4H8)4]I3 ?C7H8(1) and Mo2S2O2 (S2CNC4H8)2(2) both crystallize in triclinic, space group P1 with cell dimensions for (1) : a=13. 554(4), b=13. 620(4), c= 13. 058 (4) A , α=95. 58 (3), β=105. 38(2), γ=115. 49(2)°,V = 2035(1) A3, Z=2, Dc=1. 89 g. cm-3, final R=0. 054 and Rw = 0. 062 for 2926 observed reflections; and for (2): a = 8.730(2), b=16.592(6), c = 6. 688(2)A, α=97. 67(3), β=98. 10(2), γ=80. 26(2)% V = 939. 2(5) A3, Z = 2, Dc = 2. 05 g. cm-3, final R = 0. 038 and Rw = 0. 046 for 2248 observed reflections. The Mo(V) atom is bonded to eight S atoms in distorted dodecahedron for (1). The Mo atoms in compound (2) are bridged by two S atoms and each Mo atom is coordinated by two S atoms from S2CNC4H8 and one O atom to form distorted tetragonal pyramid.     

SYNTHESIS AND STRUCTURE OF Ni_2(PBu_3~n)_2(SC_7H_6S)_2

<正> The nickel(Ⅱ) complex Ni2(PBu3n)2(tdt)2(tdt = SC7H6S2-) containing dithiolato and phosphino ligands has been prepared and characterized by X-ray diffraction. The complex crystallizes in triclinic system, space group P1, with a = 14. 423(4), b = 15. 053(3), c=10. 648(3)(?), α=93.,95(2), β=100. 31(3), γ = 84. 16(2)°; V =2259.6 (?)3; Z = 2, Dc= 1. 22 gem-3, Mr = 830. 57; μ = 11. 076cm-1, F (000) = 888. In the complex, the Nickel atoms are linked by two bridging sulfur atoms from the two tdt ligands with the Ni-Ni distance of 2. 679 (?) . and each nickel atom is four coordinated by one phosphorus and three sulfur atoms with a square-planar geometry, the average length of Ni -S bond is 2. 193(?) and that of Ni-P bond 2.186(?).     

CRYSTAL STRUCTURE OF TRIGALLIUM TRIS(OBTHOPHOSPHATE) 2-ETHANOLANINE HYDRATE, Ga_3(PO_4)_3·H_2NCH_2CH_2OH·H_2O

<正> Trigallium tris(orthophosphate) hydrate-2-ethanolamine was synthesized from the ethanolamine(EAN)-Ga2O3-P2O5-H2O system. The compound crystallizes in monoclinic system, space group P21/n, with a = 8.669(2), b = 17.932(4), c = 9.097(2) A,β= 108.32(1)°,V=1342.4 A3, Z = 4. The structure was solved by direct methods and refined to final R of 0.048. For the three gallium atoms in an asymmetric unit, the coordination tetrahedron of Ga(3) is nearly regular, while Ga(l) and Ga(2) are each coordinated by five oxygen atoms and their coordination polyhedra show some distortion from a trigonal bipyramid. The three-dimensional net in the crystal lattice is built of two-dimensional nets which are composed of irregular triangles, quadrilaterals, pentagons and octagons formed by Ga and P atoms. Moreover, the corrugated 2D nets running along [101] are linked together by two double-crank-shaft chains of GaPO4, one of which runs along [101] while the other along [101]. The ethanolamine molecule, so called the template,     

CRYSTAL STRUCTURE OF A LINEAR TETRANUCLEAR Mo-Fe-S CLUSTER, (Et_4N)_4C(MoS_4)_2Fe_2S_2D·(CH_3OH)_2

<正> C_34H_88O_2N_4Mo_2Fe_2S_10, Mt= 1209. 25,monoclinic, P2_1/a,a= 17. 722 (7) ,b= 11. 857(5),c= 13. 743(5) A .β= 112. 29 (3)°, V= 2672. 0A3,Z = 2,Dc = 1. 503 g·cm-33,μ(Moka) = 14. 0 cm-1,T=193 K. Final R=0. 045 for 1943 observed reflections (I≥3σ(I)). In the anion [(MoS4)_2Fe2S2]4- ,the two Fe atoms, each attached with a chelating MoS42- unit, are bridged by two sulfur atoms. The metal atoms are arranged in a linear fashion with Mo-Fe-Fe angle of 179. 1(1)°, and Fe-Fe and Fe-Mo distances of 2. 746(2) and 2. 801(2) A, respectively. The long Fe-S distances (average 2. 246A) in Fe2S2 ring could be a result of the hydrogen-bonding interaction between the sulfur atom and the methanolic hydrogen atom.     

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.     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.     

CRYSTAL STRUCTURE OF TRIS(2-THENOYLTRIFLUOROACETONATO)BIS(TRIPHENYLPHOSPHINE OXIDE)EUROPIUM(Ⅲ), Eu(TTA)_3.(Ph_3PO)_2

<正> C60H42O8F9S3P2Eu,Mr=1372.07 triclinic, space group Pl,a = 11.191(1), b = 12.121(2), c = 23.529(3) A,α=80.08(1),β=76.51(1),γ=70.46(1)°,V=2909.3(6)A3, Dm(flotation in CCl4/BrCH2CH2Br) = 1.566, Dx(Z=2) = 1.562 g cm-3,λ(MoKα) =0.71073 A,μ=13.16 cm-1, F(OOO)=1376, T =295 °K, final RF=0.033 for 9104 observed reflections with |Fσ|>3σ(|Fσ|).The compound is isostructural with the known neodymium(Ⅲ) complex. The metal atom in the monomeric molecule is coordinated dodecahedrally by the eight 0 atoms of the surrounding ligands with Eu-0 bond distances in the range 2.361(2)-2.457(3) A.     

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.     

MOLECULAR AND CRYSTAL STRUCTURE OF (μ-HOCH_2 CH_2 S)_2 Fe_2 (CO)_4(PPh_3)_2

<正> The molecular and crystal structure of the complex (μ-HOCH2CH2-S)2 Fe2(CO)4(PPh3)2 synthesized by reaction of ethylene epoxide with (μ-Lis)2Fe2(CO)6, followed by EtOH alcoholysis and PPh3 substitution,was determined by X-ray diffraction technique. The crystals are triclinic,space group P 1,with a= 10. 902(2),b=12. 106 (2),c=16. 123(4) A ,V= 2079. 36A3,α=78. 13(1),β=89. 37(2),γ=87. 93(1)°, Z = 2,Dx=1. 44 g/cm3.μ(MoKa) = 9. 149cm-1, F(000) = 940. The final R and Rw equal to 0. 055 and 0. 068,respectively,for 3598 observed independent reflections. In this molecule two PPh3 ligands are trans to the Fe - Fe bond and axially coordinated to two iron atoms. In addition,two hydroxylethyl groups are attached to bridging sulfur atoms by e-type of bond and thus this molecule is an ee conformer.     

Synthesis,Structure and Luminescent Properties of [Zn(btzb)2Cl2]·2H2O[btzb=1,2-Bis(5-tetrazolyl)benzene]

The title compound[Zn(btzb)2Cl2]·2H2O(1·2H2O,btzb=1,2-bis(5-tetrazolyl)benzene)was synthesized in situ by the[2 3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions.1·2H2O crystallizes in the monoclinic system,space group P21/c with a=9.0119(18),b=7.5566(15),c=18.076(5)(A),β=114.67(2)°,V=1118.6(4)(A)3,Z=2,Dc=1.784 g/cm3 T=223(2)K,C16H16N16O2Cl2Zn,Mr=600.74,F(000)=608,μ(MoKα)=1.393 mm-1,S=1.081,R=0.0306 and wR=0.0669 for 1896 observed reflections with Ⅰ ＞2σ(Ⅰ).The Zn2 ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms,forming a distorted octahedral coordination geometry.A number of intermolecular hydrogen bonding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure.The luminescent property of 1·2H2O was also investigated.     

STRUCTURE OF A Fe-S CLUSTER COMPLEX [{(μ-PhCH_2S)Fe_2(CO)_6}_2(μ4-S)]

<正> [{(μ-PhCH2S)Fe2(CO)6}2(u4-S)], Mr = 837.95, triclinic, Pl,a=13.701(3),b=16.542(5), c=17.030(5)A,α=107.69(2),β=90.15(2),γ= 114.49(2)°,V=3309.3A3, Z=4, Dx=1.68 g/cm3,MoKa,λ=0.71069A μ=20.2 cm-1,F(000)=2008, room temperature, final R=0.035 for 4960 independent reflections. The molecule possesses approximate C2 symmetry with the pseudo-twofold axis passing through the unique sulfur atom u4-S(2) and the midpoint of the other two u2-sulfur atoms S(1) and S(3). The unique u4-sulfur atom has a tetrahedral geometry and donates its six valence electrons to the four iron atoms. The average Fe-(μ4-S) distance of 2.247 A is slightly shorter than the average Fe-(μ2-S) distance of 2.265A.     

CRYSTAL STRUCTURE OF CATENA-BIS(NITRILOTRIACETATO) PENTAAQUATRILEAD(Ⅱ), [Pb_3{N(CH_2CO_2)_3}_2(H_2O)_5]_n

<正> The title complex crystallizes in the hexagonal space group P65 (No. 170) with a = 9. 020(1), c=48. 969(6) A , V = 3450. 3(9)A3, Z = 6, Dc= 3. 14 gcm-3 and μ(MoKa) = 21. 99 mm-1. The crystal structure (R = 0. 063 for 2173 observed data) consists of a three-dimehsional network featuring three independent lead(Ⅱ) atoms in 7-, 8-, and 9-coordination environments. The bond lengths of Pb-N are 2. 62(3) and 2. 63(3) A, and those of Pb-O range from 2. 49(4) to 3. 00(3) A.     

CRYSTAL STRUCTURE OF TRIS(DIBENZOYLMETHANE)-(o-PHENANTHROLINE)EUROPIUM ACETONE SOLVATE [Eu(DBM)_3·Phen]·CH_3OCH_3

<正> The crystal of the title compound belongs to triclinic system, space group P1 with cell parameters a=12. 541(2),b=13. 049(2), c=16. 273(2) A ,a=93. 62 (1),B=96. 56(1),y=109. 38(1) ,V=2431.22A3, Z=2,Dc=1.45gcm-3,u(MoKa) = 13. 03cm-1, and F(000) = 1068. Each Eu atom in the molecule is coordinated to six oxygen atoms and two nitrogen atoms arranged in a distorted square antiprism.