PREPARATION AND CRYSTAL STRUCTURE OF CYCLOPENTADI-ENYL TETRAMETHYLETHENE-BRIDGED DICYCLOPENTA-DIENYLSAMARIUM(Ⅲ) TETRAHYDROFURANATE

<正> (CH3)4C2(C5H4)2Sm(C5H5)(OC4H8),Mr=499.4,orthorhom-bic,Cc2a,a=11.696(6),b=12.539(5),c=29.432(15)A,V=4316(4)A3,Z=8,Dc=1.54g/cm3,μ(MoKa)=27.8cm-1,F(000)=2024,R=0.077 for 1833 observed reflections.The samarium atom in the molecule is bonded to three cyclopen-tadienyl rings and one oxygen atom of tetrahydrofuran(THF)to form a tetrahedral configuration.The average Sm-C(η5-Cp)distances for the three cyclopentadienyl groups are 2.72(3),2.76(3)and 2.78(3)A,respectively,and the Sm-O bond is 2.53(1)A.     

CRYSTAL STRUCTURE OF Ce(ClO_4)_3 COMPLEX WITH 3,3-R,R''''-16-C-5(R=CH_3;R''''=CH_3O(CH_2)_2OCH~-_2)

<正> The title compound C18H37O20NCeCl3, Mr = 834. 25, orthorhom-bic, P212121, a = 11.836(4), b = 13.899(6), c= 19. 401(6) A ; V=3192(2)A3; Z = 4; Dc=1. 74gcm-3, F (000) = 1684,μ= 17. 8cm-1 (MoKa). The final R = 0. 080, Rw = 0. 081. The Ce(Ⅲ) ion is coordinated to one O atom of one C1O4- ion, a CH3CN molecule, a water molecule and seven O atoms from a crown ether molecule. The other two C1O4- ions are not coordinated to the metal. The bond lengths of Ce-N(CH3CN), Ce -O(ClO4-), Ce -O(H2O) and Ce-O(crown) are 2. 61,2. 82,2. 53, and 2. 56A, respectively.     

CRYSTAL AND MOLECULAR STRUCTURE OF 2-PHBNYLQUINOXALINE

<正> C14H10N2,Mr =206.24, space group P21/n, a =5.861(3), b =10.230 (5), c =17.440(11) A,β=92.07(5)°,V= 1045(1) A3,Z=4, Dx=1.31 g.cm-3, MoKa radiation,u=0.73 cm-1,F(000)=432,R=0.063 for 1054 observed reflections. 2-Phenylquinoxaline molecule is approximately planar. The dihedral angle between the quinoxaline ring and the substituted phenyl ring is 7.0°. The C-C bond distance connecting these two rings is 1.495(4) A. The whole molecule is a conjugation system.     

MOLECULAR AND CRYSTAL STRUCTURE OF (μ-4,4'-DIPYRIDYL)-BIS [DIAQUA-IMINODIACETATO-COBALT(Ⅱ)] TETRAHYDRATE {[CoNH(CH_2COO)_2(H_2O)_2]_2C_10H_8N_2}·4H_2O

<正> Mr=679.8,monoclinic, C2/m,a = 21.146(3), b = 12.613(1), c = 5.202(3)A,β= 93.26(2) ,V= 1385.1A3,Z = 2,Dx=1.63,Dm=1.64 g.cm-3 λ(MoKα)=0.71073A,μ=13.3cm-1,final R=0.036 for 1427 observed reflections. Bach cobalt atom in the title complex is in six-coordination environment with one bridging dipy ligand, two terminal H2O ligands and one tridentate ininodiacetic acid ligand. The "facial configuration" of the coaplex is compared with "the meridional one" found in corresponding Cu(II) complex.The bridge ligand dipy is tilted out of the coordination plane (N(1)-N(2)-O(1)-O(2) or N(1)-N(2)-0(1')-0(2')) by 47°,which may provide a spin-spin exchange pathway. Another possible magnetic exchange pathway is in the hydrogen-bonding linkage.     

SYNTHESIS AND CRYSTAL STRUCTURE OF BaGa_4

<正> BaGa4,tetragonal space group I4/mmm with lattice parameters a=b=4.5650(8), c=10.786(2)A, V=224.77(7)A3,Dc=6.15 gcm-3,and Z=2,λ(MoKα)=0.71069A,μ=335.93cm-1,F(OOO) =360. The final R = 0.045, Rw=0.069.The distribution of valence electrons in crystal Ba6a4 is described and a suggestion that two different types of gallium atoms form covalent bonds by utilizing sp3 and dsp3 hybrid orbitals respectively is proposed.     

THE CRYSTAL STRUCTURE OF NEOTRIPTOPHENOLIDE

<正> M=342.44, monoclinic, P21, a=8.100(2), b=20.493(2), c=10.830(2) A, β=90.78(2)°,V=1797.5 A3, Dc=1.265 g.cm-3, Z=4. There are two molecules per asymmetric unit. Final R = 0.036 for 1936 observed reflections. The rings A and B take semi-chair conformations and trans-fusion in the title molecule. The 5-H is α-axial and 20-CH3 is β-axial.     

CRYSTAL STRUCTURE OF Mo_3(μ3-S)(μ-S)_3 (μ-C_2H_5COO)(dtp)_3Py

<正> C20H40Mo3NO8P3S10, Mr=1123.93, triclinic, P1,a=12.972(3), b=13.763(2), c= 14.515(7)A,α=66.22(3),β=101.72(3),γ=118.90(1)° , V= 2076(2) A3, Z=2,Dc=1.798 g.cm-3, MoKa radiation, final R= 0.040 and Rw=0.056 for 5645 observed reflections. The molecule contains three Mo atoms arranged in a triangle with one capping-S atom, three (μ-S) atoms, one (μ-EtCOO) ligand, one chelate ligand dtp on each Mo atom, and one terminal Py on atom Mo(1). The coordination of Mo atoms is of distorted octahedron.     

SYNTHESIS AND CRYSTAL STRUCTURE OF SODIUM ETHYLENEDIAME-TETRAACETATOVANADYL(IV) TETRAHYDRATE Na[VO(C_(10)H_(13)N_2O_8)]·4H_2O

<正> Mr=451,orthorhombic,P212121, a=6.524(2), b=13.910(2),c= 19.694(5)A,V=1787.4A3,Z=4,Dx=1.670 g·cm-3,MoKd,λ=0.71073A,μ=6.270 cm-1,F(000)=928, room temperature, final R=0.052 for 1643 unique reflections.The VO2+ ion is coordinated by three O and two N atoms of one ethylenediaminetetraacetate (EDTA) ligand, which acts in quinquedentate chelate fasion. The coordination geometry of V atom is roughly octahedral.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF STEMOTININE

<正> C18H25NO5, Mr = 335.40, tetragonal, P41212, a = 15.578(4), c =14.723(3) A, V =3573(2) A3, Z = 8, D = 1.247 g cm-3, MoKα,λ= 0.71069 A, μ = 0.;85 cm-1, T = 293K, final R .= 0.100 and RW (on F2) = 0.080 for 1095 observed data [|FO| > 2σ(|FO|)]. The structure confirms the spectrbscopic assignment of a pentacyclic skeleton containing two α-methyl-γ-lactone rings, one ether and one tertiary amine.     

DETERMINATION OF CRYSTAL STRUCTURE OF C6H5GdCl2（THF）4

<正> By X-ray (λ=0. 71069A) diffraction of single crystal,we have determined the crystal structure of C6H5GdCl2 (THF)4,C22H37Cl2O4Gd, MT=593. 2,or-thorhombic space group Ccm2;with lattice parameters a=12. 776(6),b=12. 954(6), c=15. 802(3)A ;V=2615. 4(1. 8)A3;Z=4,Dc=2. 43gcm-3,μ=29. 3cm-1,F(000) = 1120. The structure was solved by heavy-atom method and Fourier techniques and refined by least-squares to a final R=0. 051 ,Rw = 0. 049 for 839 reflections with I≥1. 5σ (I). The results revealed that the bond length of Gd-C is 2. 437(22) A ,the average bond lengths of Gd-Cl 2. 678(6) A ,Gd-O 2. 499(12) A, C-C from phenyl group 1. 376(40)A. This crystal structure is the first organolanthanide complex with only one Ln-C bond in the molecule.     

THE CRYSTAL STRUCTURE OF PSEUDOLARIC ACID D

<正> Mr=318.46, orthorhombic, P212121, a=6.921(2), b=10.175(2), c= 25.036(5) A, Z=4, Dc=1.200 g.cm-3, V=1763.0 A3, final R=0.057 for 1451 observed reflections. The rings A and B take chair conformations, so is the ring C approximately. The ring D takes envelop conformation. The rings A and B are trans-fused in the structure.     

SYNTHESIS AND CRYSTAL STRUCTURE OF S-BENZYL-N-(FERRO-CENYL) METHYLIDENEDITHIOCARBAZATE

<正> C_19H_18N_2S_2Fe, Mt = 394. 33, monoclinic, P2_1/c,a = 7. 726 ( 7) , b = 11. 098(1 ),c= 21. 300(6) A ,β=100. 40(7)°,V= 1796. 2 A3,Z = 4,DC = 1. 458g·cm-3;MoKa,(λ=0. 71073A),μ=10. 635cm-1,F(000) = 816,room temperature,final R=0. 098,Rw=0. 121 for 3250 unique reflections,2306 reflections with I>3σ(I). The title compound is a new Schiff base which is made by condensation of formoylferrocene, FC-CHO and S-benzyldithiocarbazate. The mean Fe-C distance is 2. 04 A. The mean C-C distances in the cyclopentadienyl rings with and without side chain are 1. 43 and 1. 38 A,respectively. Electron migration from cyclopentadienyl ring to side chain is evident. A substantial Kekule-type distortion of the phenyl ring on the side chain is indicated.     

SYNTHESES AND CRYSTAL STRUCTURES, REACTION OF α -THIOPI-COLIN-o-TOLUIDIDE AND ITS ORGANOTIN COMPLEX

<正> α-thiopicolin-o-toluidide and its organotin complex have been synthesized, and both crystal structures have been determined by X-ray analysis. The ligand:C13 H12N2S,Mr = 228. 3,monoclinic,P21/n,a=16. 387(1),b = 7. 752(2),c=18. 334(1) A ,β=95. 52(1),V = 2324. 8A3,Z = 8,DC=1. 305g·cm-3,F(000) = 960e. The final R= 0. 053 for 3291 observed unique reflections. There are two molecules in the asymmetric unit,which are confirmed to exist as the keto,cis-N configuration in the solid state. The complex:C17H21N2SClSn,Mr = 439. 6,orthorhombic,P212121,a = 8. 801(3),b = 9. 188 (2),c=24. 087(6) A,V=1947. 9A3,Z = 4,DC=1. 499g·cm-3,F(000) = 880e. The final R = 0. 041 for 1694 observed unique reflections. The tin atom is surrounded by an irregular (5 + 1) coordination geometry with five normal bonds and one weak bond [Sn....C1]. The molecules join each other through the weak bonds to form infinite polymeric chains parallel to the a axis. In addition, the possible reaction mechanism in coordination is discussed.     

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.     

STUDIES ON THE MOLECULAR STRUCTURE OF WT-12 DERIVATIVE OF PYRAZOLO [3,4-d] - 1,3,2-DIAZAPHOSPHORIN-6-ONE

<正> The title compound was obtained by reaction of 1-phenyl-5-benzy-lamino-pyrazole-4-(N-methyl) carboxamide with p-fluorophenyl phosphorus dichloride and its molecular structure determined by X-ray diffraction method. The crystal is mono-clinic,space group P21/c,with a=11. 874(2),b= 12. 986(2),c=14. 587(2) A ,β= 106. 21(1)°,V=2159. 6A3,Mr = 430. 43(C24H20N4OFP),Z=4, Dx = 1. 324g/cm-3,μ(MoKa) = 1. 53cm-1 ,and F(000) = 896. The atoms in the pyrazolo[3,4-d] - 1,3,2-di-azaphosphorin-6-one are coplanar except the P atom.     

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 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 Mo_3(μ3-S)(μ-S)_2[S_2P(OEt)_2]_3][SOP(OEt)_2](0)_2

<正> M=1140.85, monoclinic, P21/c. a=12.748(2), b=14.320(2), c=23.118 (3)A,β=101.07(1)°, V=4141(2)A3, Z=4, Dc=1.830 g.cm-3. Final R=0.039 for 4160 reflections.The title compound is a rather irregular trinuclear molybdenum cluster having only two M-M bonds with two shorter Mo-Mo distances of 2.808(1), 2.839(1), and one longer Mo-Mo distance of 3.337(1)8. The existence of two Mo-Mo bonds is coincident with the electron counting for {Mo3} cluster core, and may be regarded as a result of the oxidation of a compound Mo3(μ3-S)(μ-S)2 (μ-L)[S2P(OEt)2]4(L') (L'=neutral ligands)1 characterized by us previously.     

STRUCTURE OF A Cu (Ⅱ) COMPLEX WITH MIXED LIGANDS, DIETHYLENETRIAMINE ETH YLENEDIAMINE COPPER (Ⅱ) DIPERCHLORATE

<正> CuC6H21N5O8Cl2, Mr = 425. 5, monoclinic, P21/n, a = 8. 418 (2), b = 14.450(4), c= 12. 940(3)A, β=98. 13(2)% V = 1572. 9A3,Z = 4, Dx= 1. 797g. cm-3,μ(MoKa) = 18. 3cm-1. The crystal structure consists of discrete complex cations and perchlorate anions. The coordination geometry around Cu(Ⅱ) atom is a distorted square pyramid. The complex cations are disordered in the crystal,the ethylenediamine ligand chelates to the Cu(Ⅱ ) atom in δ arid λ conformation in different cells. The average Cu-N distance is 2. 03 A in the equatorial plane while the Cu -N distance is 2. 25 A in the axial direction.