STRUCTURE OF 3-(N-METHYL- β-NAPHTHYLAMINO)-ACROLEIN,C_(14)H_(13)NO

<正> M=211.28, monoclinic, P21/c, a=10.268(2), b=11.581(2), c=9.605(2)A, β=100.40(2)°, V=1123.5(4)A3, 2=4, Dx=1.25 g/cm3, λ=0.71069A, u=0.73 cm-1, F(000)=448, room temperature, R=0.041. The planes of the formylvinyl groupand the naphthyl ring are tilted with respect to the plane of nitrogen frameN by 8.6 and 33.6 , respectively. The O atom and the methyl group are in Z position.     

MOLECULAR STRUCTURES AND SINGLE CRYSTAL ESR SPECTRA OF IMIDAZO-LATE-BRIDGED Co(Ⅲ)-Cu(Ⅱ)-Co(Ⅲ)AND Co(Ⅲ)-Zn(Ⅲ)-Co(Ⅲ) COMPLEXES

The structures of the heterotrinuclear complexes, [(NH_3)_5ColmCu(dien)ImCo(NH_3)_5]-(C10_4)_6·4H_20 and [(NH_3)_5CoImZn(dien)ImCo(NH_3)_5]-(ClO_4)_6·4H_2O, are reported. Co--Cu--Cocrystallizes in the monoclinic space group C2/c with a =32.414(4), b= 9.421(1), c=15.167(5)?,β= 90.91(2)°, Z=4 and Co--Zn--Co in the same space group with a = 32.578(2), b = 9.419(1), c = 15.125(3)?, β=91.10(1)°Z=4. The Cu(Ⅱ) and Zn(Ⅱ) geometriesare intermediate between a trigonal bipyramid and a square pyramid,the Co(Ⅲ) is a-hexagonal coordination and the dien ligand shows a disordered contribution in the respectivestructure.The magnetic properties of Co--Cu--Co are investigated. From the single crystalESR spectra studies, the anisotropic g and A tensors and electronic spin-density of Co--Cu--Co are obtained and the nature of the bonding for Cu~(2+) is discussed.     

CRYSTAL STRUCTURE OF GdCl_3(DIMETHOXYETHANK)_2

<正> C8H2oCl3GdO4,Mr=443.80,monoclinic, space group P21/c, a=11.442 (3),b= 8.849(2), c= 15.575(5)A,β=104.8l(2)° ,V=1521.9(7)A3,Z= 4, DC = 1.94 g/cm3,λ(MoKα) =0.71069A,F(000)=860. The structure was solved by Patterson and Fourier techniques and refined by least-squares nethod to a final conventional lvalue of 0.051 (Rw=0.054). The central ion Gd(III) is bonded to three chlorine atoms and four oxygen atoms froa two dimethoxye-thane molecules to form a distorted pentagonal bipyramid. The Qd-Cl distances are in the range of 2.460-2.628A (average 2.571A). The Gd-O distances are in the range of 2.408-2.493A (average 2.458A).     

OXO-CENTERED HETEROTRINUCLEAR TRANSITION METAL CARBOXYLATE COMPLEXES 3, SYNTHESES AND X-RAY STRUCTURAL CHARACTERISTICS OF COMPOUNDS Fe_2MO(O_2CCCl_3)_6(THF)_3 (1,M = Mn;2,M=Co;3, M = Ni;THF=TETRAHYDROFURAN)

<正> The title compounds have been synthesized and characterized by x-ray analysis. They are isomorphous, belonging to trigonal space group R3m,with crystallo-graphic parameters; (1)α =b =c= 13. 713(5) A ;α= β=γ=83. 66(3)°;V = 2535A3;Z = 2;DC=1. 80gcm-3;F(000) = 1358;M= 1373. 23;(2)α= b = c=13. 687(2) A;α = β = γ = 84. 27(1)°/;V = 2528. 0A3;Z = 2; Dc = 1. 81gcm-3; F (000)= 1362; M = 1377. 23;(3)α = b=c=13. 671(6) A ;α = β = γ=84. 12(3)°;V=2518A3;Z=2;DC = 1. 82 gcm-3;F(000)= 1364;Mr= 1376. 99.The structure of comp ound 2 has been determined with the final R= 0. 061 for 845 reflections with I≥3σ(Ⅰ).The three metal atoms are crystallographically equivalent because of the arbitrariness of orientation of the molecules,and in the sense of crystallography the molecule Fc2CoO(O2CCCl3)6(THF)3 is of C3vsymmetry with centered oxygen atom on the 3-fold axis. The atoms M,C(1~4),C1(1) and O(1) lie on the mirror. Three CC13 groups on one side the Fe2CoO plane and three terminal THF ligands are dynamically     

CRYSTAL AND MOLECULAR STRUCTURE OF 1-PHENYLAMINOMETHYL-3,7,10-TRIMETHYL-2,8,9-TRIOXA-5-AZA-1-SILITRICYCLO(3,3,3,0~(1,5)) UNDECANE

<正> The transparent colourless crystal of the title compound crystallized in monoclinic system with space group P21/c and cell dimensions a=9.857(7), b=11.128(4), c=16.036(7) A, β=103.31(5)°, V=1711.7A3, Z=4, Dc= 1.25 g.cm-3, λ =-1.5418 A, μ= 13.067 cm-1. The structure was solved by direct methods and refined by full matrix least-squares, the final discrepancy factor R=0.061 and Rw=0.060. The skeleton of the molecule is composed of three five-membered rings with a common edge N(l)-Si(l), and the dihedral angles between each two of the three rings are 110.5°, 107.9° and 105.0° respectively. The N(l)-Si(l) coordination bond length is 2.143(3) A. In comparison with the structures of other related compounds, it was found the N-Si bond length varies with the electronegativities of the substitute groups R at Si atom.     

BINUCLBAB COPPER(Ⅱ) COMPLEXES OF SOME PLANT GROWTH-STIMULATING SUBSTANCES.Ⅰ.SYNTHESIS AND STRUCTURE OF BIS(N,N-DIMETHYLFORMAMIDE)-TETHAKIS(μ-INDOLYL-3-ACETOXY) DICOPPER(Ⅱ)

<正> The structure of the title compound (Mr = 969.99) has been determined by X-ray analysis. The crystals are monoclinic, space group P21/n with a =14.746(2),b= 10.782(7), c = 15.531(3) A,β=113.74(2)°,Z=2,and DC=1.425g·cm-3. The final refinement converged with R = 0.067 and Hw=0.080 for 4491 observed reflections with I>3σ(I).     

THE CRYSTAL STRUCTURE OF TR1S (μ-SULFJDO)-(U3-SULFJDO)-TETRAKTS (O,O-DIETHYLPHOSPHORODITHIOATO-S,S)-OXAZOLE-TRI-MOLYBDENUM-ANTIMONOUSCHLORID {Mo_3(U3-S)[u-S)_3·SbCl_3][S_2P(OEt)_2]_4·(C_3H_3ON)}

<正> Mr = 1445.67, triclinic. The space group is P1 with the unit cell parameters: a = 10.342(3), b = 11.994(3), c = 21.352(4) A; (?)= 76.27(2), β - 88.55(2)°, r = 73.26(2)°; V = 246lA3, Z = 2, DC = 1.959 g.cm-3. The final R factor is 0.068 based on 4053 reflectioons with I≥3(?)(Ⅰ). The title compound may be regarded as the result of that a molecule of trinuclear Mo cluster {Mo3S4[S2P(OEt)2]4·(C3H3ON)}[1] connects with a molecule of SbCl3 by three bridging S atoms. The skeleton {Mo3SbS4} is a distorted cube. The distances of Mo-Mo bonds are 2.728(2), 2,743(2) and 2.751(2) A, respectively, and the distances between Sb and Mo atoms are 3.814(2), 3.815(2) and 3.847(2) A, respectively.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A CUBANE-LIKE MOLYBDENUM-COPPER-SULFUR CLUSTER {Mo3CuS4[S2P(OC2H5)2]3(I)(μ-CCl3(00)CH3CN}

<正> The synthesis and crystal structure of the cubane-like cluste with [Mo3CuS4] core is reported herein. The title compound crystallizes i triclinic space group Pl with the following unit cell dimensions: a 11.723(3), b = 14.353(6), c = 15.533(4)A;α= 75.40(3)°,β=69.13(2)°,γ 64.93(3)°; Z = 2; V = 2196 A3; DC = 2.033 g·cm-3.7704 independent reflec tions were collected on CAM four-circle diffractoneter with MoKa radiatio in the range of 1 < <25°, with only 2083 reflections having intensitie I > 3σ(I). The structure was determined by direct methods and refined b the least-squares method to a final R index of 0.091. There are some distortion in the cubane-like [Mo3CuS4] core, with three Mo-Mo bonds and thre weak Mo-Cu bonds.     

CRYSTAL STRUCTURE OF 2-(PHENYLAMINO THIOFORMYD-3,4,5,6-TETRAHYDROPYRIMIDINE

<正> The title compound 2-(phenylamino thioformyl)-3,4,5,6-tetrahy-dropyrimidine(C11H13N3S,Mr=219)was synthesized by the reaction of N,N'-diphenyl dithiooxamide with 1,3-diamine trimethylene.The crystal is monoclinic,space group P21,with unit cell constants a=6.253(1),b=7.304(1),c=12.027(2)A,β=102.71(1)°,Z=2,V=535.9(2)A3,Dc=1.35.g/cm3.The final deviation factor R=0.025.The result reveals that the dihedral angle between the thio-formyl group [S,C(7),C(8),N(1)]and the phenyl ring is 33.4°,and the thio-formyl group and the mean plane of the atoms [N(3),C(8),N(2),C(9)]are nearly coplanar.     

CRYSTAL AND MOLECULAR STRUCTURE OF(μ-PhCH_2S)(μ-CH_3C(0)CH_2S)Fe_2(CO)_6

<正> The crystal and molecular structures of (μ-PhCH2S)(μ-CH3C(O)CH2S)-Fe2(CO)6 have been determined by X-ray diffraction technique. The complex has chemical formula of C16H12O7S2Fe2 and Mr=492.08. The crystals are tri-clinic, space group P1,with a=8.461(5), b=10.937(5), c=ll.419(4)A,α=81.61 (3), β=78.21(4),γ=71.04(4)°,V=974.5A3, Dc=1.68 gcm-3,μ(MoKα)=17.3cm-1, Z=2,F(000)=495.93. The final R was 0.038 for 2874 independent reflections.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF CHLORO(BIS-2,2''''-DIPYRIDYL) COPPER7,7'''',8,8''''-TETRACYANOQUINODIMETHANE [Cu(bipy)_2Cl]·TCNQ_2

The crystals of title compound are prepared by the electrochemical method and its structure has been determined by X-ray diffractions method. The crystals are triclinic with space group P(?). a=7.920, b=13.140, c=19.126; a=100.77°, β=94.45° and γ=101.08° ; Z=2, Calculating of electronic structure of TCNQ and its packing mode are discussed.     

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 TETRAKIS(THIPHENYLPHOSPHINE OXIDE)-DICHLORO-GADOLINIUM(Ⅲ)TRICHLOHO-COPPER(Ⅱ)

<正> The crystal of tetrakis(triphenylphosphine oxide)-dichloro-gadolinium trichloro-copper belongs to triclinic, space group Pl with unit cell parameters of a = 19.395(2), b = 19.708(5), c = 20.609(4)A,α= 63.32(2)° ,β=88.74(1)°,γ=81.49(1)°,V=6943.8A3,and Z=4. The final refinement converges with R=0.072 and Rw = 0.077 for 7870 observed independent reflections.     

CRYSTAL AND MOLECULAR STRUCTURES OF SCHIFF BASE COM-PLEXES WITH TRANSITION METAL IONS Ⅱ . BIS-( N-( 4-CHLQRO-PHENYL)-SALICYLALDIMINATO)COBALT (Ⅱ)

<正> The crystal and molecular structure of the title compound was determined by means of Patterson and Fourier synthesis based on three-dimensional X-ray data. The crystallographic parameters are as follows; (C13H8NOCl)2Co, monoclinic, space group A2/a,a = 11. 722 (8) , b = 8. 726 (5) , c = 21. 810 (8) A ,β= 95. 90 (6)°, V = 2219. OA3,Z= 4, Dc=1.55g/cm3,μ= 10. 71cm-1, F(000) = 1052, R= 0.042, Rw = 0. 051. Two iminato ligands are attached to the center atom Co through their donor atoms N(1),O(1),N(1)* ,and O(1)* to form a distorted tetrahedral configuration. The bond lengths of Co-O and Co-N are 1. 891 and 1. 988 A , respectively.     

THE STRUCTURE OF N-METHYL-CINNOLINE TCNQ_2 II.THE STRUCTURE OF IN-METHYL-CINNOLINE TCNQ_2

<正> M =553.6, triclinic,Pl, a=6.5157(22), b=7.7153(14), c=13.9146(28)A; α=88.394(16)°, β=84.288(22)°, γ=78.749(22)°, V=682.62(30)A3, Z=1; μ(MoKα)= 0.80cm-1, F(000)=284.92, room temperature. The final R=0.0537 for 1230 independent reflections. Planar tetracyanoquinodimethane(TCNQ). stacks along a axis with the molecular planes parallel to each other. The separations between TCNQs are 3.2698 and 3.2448. The overlaps of TCNQs are of the ring-external bond type. This mode of TCNQ stacking is used to explain the conductivity of the title compound. The D.C. conductivity along needle axis is σ(RT)=10(Ωcm)-1 1.     

STRUCTURE OF PENTAAQUO PYROMEL DIZINE (Ⅱ)-DIHYDROUS [C_6H_2(COO)_4Zn_2(H_2O)_5]·2H_2O

Crystal and molecular structure of [C6H2(COO)4Zn2(H2O)5]·2H2O has been determined by X-ray diffraction technique, Mr = 507. 0,monoclinic,space group P21/n,a = 5. 925(1), 6 = 23. 613(9) ,c= 11. 790(5) A ,β= 96. 36 (3)°, V=1639. 3 (1. 0) A3,Z=4,DC = 2. 05g/cm3,λ=0. 71069 A,μ(MoKa) = 30. 9/cm-1,F(000) = 1024e. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0. 055(Re = 0. 059)for 1557(I>3σ(I))reflections. Both atoms Zn(1) and Zn(2) are bridged by the Z,E-type of the car-boxyl group, in addition, Zn (1) is monodentate-bonded to the three remaining carboxyl and Zn(2) is bonded to five water molecules. The crystal structure shows a 2-dimensional polymeric network along(010)face. The Zn(l) -O distances are in the range of 1. 94~ 2. 01 A (average 1. 98 A ). The Zn(2) -O distances are in the range of 2. 06~2. 21 A (average 2. 12A).     

STRUCTURE OF TRANS-SYN-BIS-[(η-(CH_3)_2CHC_5H_4)Mo (μ-S)(μ-SC(CH_3)_3)]

<正> Mr = 648.75, triclinic, space group P1 , a = 10.087(4), b = 12.686(5), c = 14.222(6) A, α= 104.83(3)°, β = 124.61(4)°, γ = 90.98(3)°, V = 1417.22A3, Z = 2, De = 1.520 Mg.m-3, (MoKα)= 0.71069A, μ(MoKα) = 11.597 cm-1, F(000) = 664, room temperature. Final R=0.0424 for 5705 observed reflections. In the molecule two metal atoms are bonded togetherin a cavity surrounded by Ugands. Pour sulphur atoms are in bridging positions and in the same plane perpendicular to the metal-metal vector with the two t-butylthiolato ligands being in mutu-syn positions.     

THE CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR SILVER CLUSTER COMPLEX Ag_4(α-C_(10)H_7CS_2)_4(Py)_4·2Py

The title compound has been synthesized by the reaction of α-dithionaphthoic acidwith AgNO_3 in an organic solvent. The single crystals were obtained by recrystallizingfrom pyridine. We obtained two kinds of crystal with different colours (A and B), usingdifferent ratios of silver nitrate and α-dithionaphthoic acid (1:2,1:4) in the reactions. The structures of the two kinds of crystal were determined by a single-crystal X-raydiffraction analysis. The crystal (A) belongs to monoclinic space group C_(2h)~5-P2_1/a withunit cell parameters: a = 22.822(4) A, b = 12.803 (4) A, c = 24.444 (7) A, β = 103.90 (2)°V = 6933.14 A~3, Z = 4. The crystal (B) belongs to monoclinic space group C_(2h)~6-C2/c witha = 29.150 (2) A, b = 12.799 (3) A, c = 24.413 (2) A, β = 130.56 (4)°, V = 6914.38 A~3,Z = 4. Both crystals (A) and (B) have the same molecular configuration, but they havedifferent symmetry. In crystal (B), the molecule possesses a C_2 symmetry. This paperreports the structure determination and parameters o     

THE CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM)(μ-OXO)BIS[TRIPHENYL-THIOLATO-IRON(Ⅲ)],(Et_4N)_2[Fe_2O(SPh)_6]

<正> Fe_2OSsN_2C_(52)H_(70),Mr=1043.23,monoclinic, P21/a, a=18.121(3), b=15.249(3), c=20.369(4)A,β=102.49(8)°,V=5495(1)A3, Z=4, Dc=1.261g.cm-3,MoKα(λ =0.710691), μ=17.816mm-1, F(000)=2208. R=0.073 for 4374 observed reflections with I≥3.0σ(I). The structure of the anion contains a linear Fe-O-Fe unit, with mean Fe-O distance of 1.766(2)A. The coordination geometry about each iron atom is close to tetrahedral with the angles O-Fe-S and S-Fe-S being 115.3° and 103.1°, respectively.     

STRUCTURE OF 3-(IMIDAZOLIDIN-2-YLIDENE)-4,5-DIMETHYL-4,5-DIHYDRO-2(3H)-FURANONE, C_9H_(14)O_2N_2

<正> Mr=182.25, Orthorhombic, Pna21, a=10.698(4), b=9.779(4), c=8.872(5)A, Z=4, V=928.1(7)A3, Dx=1.3 Mgm-3, λ(MoKα)=0 . 71069A, μ(MoKα) = 1.0cm-1, F(000)=392, room temperature, R=0.034 for 637 reflections. The lactone ring and imidazolidine ring are twisted mutually by 12.3°. The two methyl groups are in cis positions relative to the lactone ring. There exist intramolecular and intermolecular hydrogen bonds in the structure.