CRYSTAL STRUCTURE OF THE METHYL 4—（N—（1—OXYPROPYL）—N—PHENYLAMINO]—1—[2—（2—THIENYL）ETHYL]—4—PIPERIDINECARBOXYLATE（R31826）HYDROCHLORIDE

<正> C22H28N2O3S.HCl, Mr = 436.9, triclinic,P1;a=8.557(3),b= 10.299(2),c= 13.894(2)A;α= 99.25(1),β=86.64(2),γ= 107.68(2)°;V= 1151.2(3)A3,Z= 2, DC = 1.27g/cm3,R=0.064. The torsion angle C(14)-C(1)-N(2)-0(19) in the title compound is 137.5 being much larger than that (106°) in R30730. The dihedral angle between mean planes of the thiophene ring and piperidine ring is about 83 .     

Crystal Structure of cis—2—[P,P—Diethoxy） phosphono（m—nitro）benzyloxy]

The crystal structure of the title compound cis-2-[(P, P-Diethoxy)phosphono(m-nitro)benzyloxy]-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide, C22H29NO8P2S, was determined by single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with Mr=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, Dx=1.338 g/cm3, λ=0.71073, μ=0.2796 mm-1 and F(000)=556. The structure was solved by direct methods. The final R factor is 0.052 and Rw is 0.057 for 1793 unique observed reflections [I≥3σ(I)]. A cis-configuration and a preferred chair conformation for the molecule have been established by X-ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C4-H and 31P NMR.     

Crystal Structure of 5—（l—Menthyloxy）—3—chloro—4— Pyrrolidinyl—2（5H0—f

The molecular structure of the title compound 5-(l-menthyloxy)-3-chloro-4-pyrrolidinyl-2(5H)-furanone, C18H28ClNO3(Ⅰ), has been determined by X-ray diffraction at 296(1)K. The crystal is monoclinic with space group P21, a=9.457(3), b=10.413(3), c=9.525(2), β=95.19(2)°, V=934(1) 3, Z=2, Mr=341.88, Dx=1.22 g/cm3, μ=2.15 cm-1, F(000)=368. The final R factor is 0.059, and Rw is 0.065 for 1020 observed reflections with I≥3σ(I). The absolute configuration at C(14) of the acetal carbon was proved to be S, taking into account the known configuration of 1R, 2S, 5R-menthyl moiety. There are three rings in the molecule of this compound: the furanone ring, the pyrrolidine ring and the mentholoxy group ring. The franone ring is connected with the pyrrolidine ring and the mentholoxy ring by N atom and μ2-O bridge atom respectively.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1，2，3，4—TETRAKIS（6‘,7’—DIMETHYL）BENZOXAZOLYL CYCLOBUTANE

<正> 1,2,3,4-Tetrakis(6',7'--dimethyl)benzoxazolyl cyclobutane was obtained by irradiation of E-l,2-bis(6',7'-dimethyl-1',3'-benzoxazolyly-2')-ethene in ethanol with a 450-watt high pressure mercury lamp. Its crystal and molecular structure has been determined by X-ray diffraction method. The crystal is triclinic, space group A with a = 7.008(2), b=9.586(1), c = 13.174(2)A,α= 104.08(1),β= 98.56(2),γ=99.97(2)°,V= 828.4A3, Mr= 636.76, (C40H36N4O4), Z =1, Dx =1.28g/cm3,μ= 0.78 cm-1 and F(OOO)=336.     

The Molybdenum（0）Complex [Et4N]2[Mo2（CO）6（pys）2]（pys=Pyrindine—2—thiol

The title compound tetraethylammonium hexacarbonylbis(μ-pyridine-2-thiolato-S∶S) dimolybdenum [Et4N]2[Mo2(CO)6(pys)2] crystallizes in the monoclinic, space group, P21/c with a=13.217(2), b=21.648(2), c=27.193(6)(), β=82.52(2)°, V=7714.6()3, Z=8, Mr=840.77, Dc=1.45 g/cm3, μ=7.8 cm-1, R=0.038 and Rw=0.040 for 6082 reflections with I≥3σ(I). X-ray crystal structure study reveals that the asymmetric unit of the title compound is comprised of two independent formulations of the molecular formula. Each dianion has approximate C2 symmetry and the dimetallic Mo2S2 core adopts a "butterfly" conformation with a dihedral angle between the halves of 139.3(1)° for the first independent anion and 142.8(1)° for the second one. The two pyridine rings lie on the same side of the molecule in a cis arrangement and the Mo...Mo separations are 3.76(1) and 3.838(1)().     

STRUCTURE OF 1，2，4—TRIPHENYLCYCLOPENTA—1，3—DIENE

<正> C23H18, Mr = 294. 40, orthorhombic, Pbca, a = 20. 927(9), b = 20. 695(9), c = 7. 570(2)(?), V = 3278(2)(?)3, Z = 8, Dc=1.19gcm-3, μ(MoKα) = 0. 63cm-1, F(000) = 1248, R = 0. 057 for 1109 observed reflections with I>2. 5* (I). The dihedral angles between a given phenyl ring and the cyclopentadienyl plane are 28. 2, 50. 2 and 21. 8°, respectively. The structure is stabilized through weak stacking of the cyclopentadiene moieties in crystals.     

RESEARCH ON CRYSTAL STRUCTURE OF 4—AMINOBENZOPHENONE（ABP）

<正> 4-aminobenzophenone(ABP), (C6H5)CO(C6H4NH2),Mr= 197. 23, monoelinic, space group P21,a= 12. 036 (3), b = 5. 450 (7), c= 8. 299(2) A,β = 97. 86°,V = 539. 32(3) A3,Z = 2,DC = 2. 215,Dm = 1. 209g/cm3,λ(MoKa) = 0. 71073 A,F(000)= 208,μ=0. 722cm-1,R=0. 083,Rw = 0. 084 for 721 observed reflections. There exists a cleavage plane (100) in the crystal ABP.     

Synthesis and Structural Invstigation of {CpEu[CH（COOC2H5）2][μ—CH（CO

The title complex {CpEu[CH(COOC2H5)2][μ-CH(COOC2H5)2]}2 crystallizes in the triclinic system, space group P with unit cell constants a=9.108(1), b=11.580(2), c=11.705(2) , α=70.42(1)°, β=73.83(1)°, γ=78.60(1)°, Dc=1.602 g/cm3, Mr=1070.76, V=1109.7(3)3, Z=1, μ(MoKα)=28.66 cm-1 and F(000)=536, T=296K, R=0.028, Rw=0.037. The geometry around the Eu ion can be described as a pentagonal bipyramid.     

CRYSTAL STRUCTURE OF ERBIUM（Ⅲ）COMPLEX WITH 1，3，5—BENZENETRICARBOXYLIC ACID

<正> The crystal structure of erbium (Ⅲ) complex of 1,3,5-benzenetricar-boxylic acid is reported. The title compound crystallizes in triclinic space group of P1 and cell parameters a = 7. 649(3) ,b= 9. 859(2) ,c= 11. 171 (3) A ;α= 106. 90(2),β= 104. 40(3),γ=107. 20(3)°;Z = 2;V = 716. 5A3.The final R and Rw are 0. 0328 and 0. 0338 respectively. The rare earth ion is nine-coordinated by four oxygen atoms from two carboxylato groups in two 1, 3, 5- benzenetricarboxylato groups and five aqua molecules, forming a distorted monocapped square antiprism. The Er-O distances fall in the range of 2. 327-2. 627A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A NEW BINUCLEAR CUPRUM COMPLEX, [(CuCl)_2(η~2-dppe)_2(μ-dppe)]·2CH_2C1_2

<正> C80H76Cl6Cu2P6,Mr=1563.13,monoclinic,P21/n,a=12.608(9),b=21.729(7),c=14.473(8)A.,β=105.34(5)°,V=3823.6A3,Z=2,Dc=1.28 g.cm-3,F(000)=1528,μ=8.6 cm-1,The final R and Rw are 0.076 and 0.083 respectively for 4418 observed reflections with I≥3σ(I).There is a center of inversion in the molecule.     

CRYSTAL STRUCTURE OF MIXED-METAL CLUSTER(η~5-C_5H_5)_2Mo_2Fe_2(μ3-S)_2(μ-CO)_2(CO)_6

<正> Mr= 721.98,monoclinic, P21/n,a= 9.773(1), b = 6.641(3), c = 16.258(1)A,β=92.25(1)°,V=1054.4(7)A3,Dx = 2.274g/cm3,Z=2,λ(MoKα)=0.7107A.Final R= 0.024,Rw= 0.036 for 1554 observed reflections. The cluster core Fe2Mo2 is a rhombic plane with Mo-No distance of 2.827A and average Mo-Fe distance of 2.773A.     

STRUCTURE OF TARAXER-9,12,17-TRIENE-3β,23-DIOL,C_(29)H_(44)O_2

<正> The structure of the title compound, a pentacyclic triterpenoid isolated from Clinopodium Polycephalum (Vant.) C. Y. Wu et Hsuan, has been determined by X-ray crystallographic analysis. C29H44O2,Mr=424.67, monocli-nic, P21,a=10.753(2), b=7.705(2), c=15.336(2)A,β=101.47(1)°, V=1245.2(7) A3,Z=2, Dx=1.133gcm-3,μ(Mo-Kα)=0.64cm-1, F(000)=468, 294K. Ths structure was solved by direct methods and refined to R=0.050 for 2269 observed MoKd reflections.     

Crystal Structure of Di-μ-bromo-tris(triphenylphosphine) Di-silver(Ⅰ)

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＤｉ－μ－ｂｒｏｍｏ－ｔｒｉｓ（ｔｒｉｐｈｅｎｙｌｐｈｏｓｐｈｉｎｅ）Ｄｉ－ｓｉｌｖｅｒ（Ⅰ）ＺｈｕＹｏｎｇ－Ｂａｏ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＳｔｒｕｃｔｕｒａｌＣｈｅｍｉｓｔｒｙａｎｄＦｕｊｉａｎ...     

CRYSTAL STRUCTURE OF COMPLEX OF p-METHOXY-ARYLDIAZONIUM SALT WITH DTBENZO-24-CROWN-8

<正> Mr=448.5, monoclinic P21/c, a=8.531(3), B=12.076(4), C=33.309(13) A, β=95.41(1)°, V=3416.2(2) A3, Z=4, μ(MoKα)= 1.2 cm-1, F(000)=1408, room temperature, R=0.086, Rw=0.084 (W=1/(σ2(F) + 0.0001 x F2)) for 1759 independent reflections with I > 3σ(I).     

CRYSTAL STRUCTURE OF Mo_3(μ_3-O) (μ-S_2)_ 3 [S_2P(OEt)_2]_3I

<正> Mr=1178.9, monoclinic, P21/n, a=16.570(2), b=12.370(1), c=20.007(2) A,β=99.97(1)°, V=4039.0A3, Z=4, Dx=1.938 Mgm-3, λ(MoKα)=0.7107A, μ(MoKα)=23.96 F(000)=2296, room temperature. Final R value=0.047 for 4387 unique observed reflections. It consists of neutral mono-oxo-capped trinuclear molybdenum cluster molecules with an average Mo-Mo bond length of 2.626(4)A and an average Mo-0 bond length of 2.036(2)8.     

THE CRYSTAL STRUCTURE OF BEDT-TTF[Pd(dmit)_2] (H_2dmit=4,5-dimercapto-1,3-dithiole-2-thione)

<正> C16H8PdS18, Mr=984.6, triclinic, Pl, a=6.6889(20), b=7.3824(21), c=15.0945(38)A; α=92.098(23)°,β=97.958(22)°, r=109.269(22)°, V=694.14(33)A3, Z=1; μ(MoKα)=19.68 cm-1. F(000)=437.98, room temperature, R=0.042, Rw=0.041 for 1865 independent diffractions. Planar BEDT-TTF and Pd(dmit)a stack along b axis separately. The separation between BEDT-TTFs is 6.74A, that between Pd(dimt)a planes 6.53A. This feature of BEDT-TTF[Pd(dimt)2] stacking may be used to explain the semiconducting character of the title compound.     

Schiff碱(C7H7NO)钯(Ⅱ)配合物的合成与晶体结构

合成了N—H水杨醛Sch iff碱的钯(Ⅱ)配合物.X射线单晶衍射表明,配合物晶体属于单斜晶系,Pī空间群,分子式为C48H50N8O8Pd3,晶体学参数:a=0.945 8(19)nm,b=1.059 9(2)nm,c=1.396 5(3)nm,α=74.61(3),°β=75.18(3)°,γ=68.49(3)°,V=1.236(4)nm3,Dc=1.594 Mg/m3,Mr=1 186.16,Z=1,F(000)=596,R1=0.029 9,wR2=0.073 4.晶体结构表明,钯原子为四配位,位于配合物的中心与配体的氮原子和氧原子结合形成六元环.     

Crystal Structures of O－Vanillin－semicarbazide and Salicylaldehyde－semicarbazide

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｓｏｆＯ－Ｖａｎｉｌｌｉｎ－ｓｅｍｉｃａｒｂａｚｉｄｅａｎｄＳａｌｉｃｙｌａｌｄｅｈｙｄｅ－ｓｅｍｉｃａｒｂａｚｉｄｅ￥ＬｉＳｈｕ－Ｌａｎ；ＬｉｕＤｅ－Ｘｉｎ；ＺｈｏｕＪｉａｎ－Ｈｕａ；ＭｅｎｇＦａｎ－Ｑｉｎ（Ｄｅｐａ...     

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.