K_4Na_2{Cu[C(CH_3)(OH)(PO_3)_2]_2}·12H_2O络合物的晶体结构研究

K_4Na_2{Cu[C(CH_3)(OH)(PO_3)_2]_2}·_(12)H_2O络合物晶体属三斜晶系,空间群为C~1_i-P;a=11.951(3),b=6。220(1),c=11.789(2)A;a=113.166(11)°,β=108.944(15)°,γ=97.563(14)°;V=727.4A~3;D_c=2.02g/cm~3;μ_(MoKa)=16.9cm~(-1)。结构分析证实Cu~( 2)与2个HEDP配体形成了六啮六环的螫合离子,6个Cu—O配住键包含有键距为2.667A2个长键。R=0.0413。     

三岔共轭体系的结构研究——2-苯甲酰噻吩的晶体结构和构象

用X射线单晶衍射法测定了标题化合物的晶体结构,并用PCILO方法进行了构象分析。C_(11)H_8OS属于正交晶系,空间群P2_12_12_1,a=11.945(4),b=10.236(7),c=7.649(4),Z=4,Dc=1.37g/cm~3。由于分子内存在空间位阻,分子骨架不呈平面状。噻吩环与羰基骨架平面的二面角(θ_1)为21°,苯环与其的二面角(θ_2)为32°。计算得到的最低能量构象与晶态构象一致。文中讨论了分子的形状、空间位阻、基团共轭能力对构象的影响和孤立态分子在整个构象空间的势能变化。     

中药白头翁配基G(C_(30)H_(48)O_4)的晶体和分子结构

白头翁配基G(C_(30)H_(48)O_4)晶体的空间群是P2_12_12_1,晶胞参数为:a=12.5925(2),b=13.245(2),c=15.923(2);Z=4(Dobs=1.12,Dcalc=1.182g·cm~(-3))。晶体结构用直接法和电子密度函数解出。在这个不对称分子中,四个六元环构型均属椅式,并且彼此间通过ee键稠合。晶体中存在三种O-H…O分子间氢键。     

绵毛马兜铃“结晶K”(C_(15)H_(20)O_2)的分子及晶体结构

本文报导从绵毛马兜铃(Aristolochia Mollissima Hance)中提取的一种结晶体K,C_(15)H_(20)O_2的分子及晶体结构。晶体属于正交晶系,晶胞参数为:a=6.543(2),b=13.972(3),c=14.732(2),空间群为P2_12_12_1,Z=4,d_(cal)=1.15g/cm~3。结构模型由SHELXTL程序解出,经最小二乘修正,最后的一致性因子R=0.055。 结构测定表明,分子内存在一个10员二烯环和一个5员内酯环,它们共有一个碳—碳双键。5员内酯环呈平面构型,且与10员环的最小二乘平面相互垂直。     

红霉素A6，9-亚胺醚的合成及晶体结构测定

通过红霉素A9（E）-肟（1）的Beckmann重排合成了红霉素A6，9-亚胺醚（2） ，并对2乾地了波谱表征。红霉素A6，9-亚胺醚（2）的X射线衍射单晶结构测定表 明，其结构为正交晶系，P2_12_12_1空间群，晶胞参数：a=1.0646(2) nm, b=1. 7896(4) nm, c=2.3755(5) nm; α=β=γ=90.00(0)°，V=4.5257(16) nm~3， D_c=1.187 g/cm~3，Z=4，F（000）=1776，μ=0.091 mm~(-1), R_1=0.0399, ω R_2=0.0482。     

5-取代丙二酸亚异丙酯的结构研究 Ⅱ.5-(α-异丙基)-2,2-二甲基-1,3-二氧杂环己烷-4,6-二酮的晶体结构及量子化学计算

5-(α-异丙基)-2,2-二甲基-1,3-二氧杂环己烷-4,6-二酮C_9H_(14)O_4,M_r=186.21,正交晶系,空间群为P2_12_12_1,晶胞参数为:a=5.228(1),b=11.079(4),c=16.955A。V=892.1(5)A~3,D_c=1.286g·cm~(-3),Z=4,μ(MoK_a)=0.92cm~(-1)。用直接法解出结构,经最小二乘法修正,最后的偏离因子R=0.062。结构测定表明,分子内六元环具有扭曲船式结构。对5-(α-苯乙基)-2,2-二甲基-1,3-二氧杂环己烷-4,6-二酮的CNDO/2计算表明,最稳定构型是扭曲船式结构,与X射线晶体分析结果相一致。     

杂芳核对(N-N-二烃基胺基)二氯硼烷的三烃基化反应, 二乙胺合三(2-苯并噻唑基)硼烷的合成及其晶体结构

本文报道(N,N-二烃基胺基)二氯硼烷的反常三烃化反应。2-苯并噻唑基Grignard剂与(N,N-二乙胺基)二氯硼烷反应,得到二乙胺合三(2-苯并嚷唑基)硼烷,并讨论了反应机理。分子结构经X单晶结构分析确证。晶体结构属正交晶系,空间群为P2_12_12_1,晶胞参数a=11.570(3),b=12.496(4),c=16.577(4)nm;Z=4,V=2397.3nm~3,D_0=1.348g/cm~3,μ(MoK_a)=3.167cm~(-1)。     

THE MOLECULAR AND CRYSTAL STRUCTURE OF [Et4N]2[Fe2S2（NO）4]

<正> The compound [Et_4N]_2[Fe_2S_2(NO)_4] (M_r=556.36) crystallizes in the monoclinic,space group P 2_1/n with a=9. 688(3), b=10. 882(2), c=12. 625(2), β=97. 86(3)°, Z=2, V=1318. 4, D_c=1. 40g/cm~3, ;μ(MoK_a)=12. 8cm~(-1) and F(000)=588. The final R=0. 028 and R_w=0. 029 for 2041 reflections (I≥3σ(I)).The crystals of [Et_4N]_2[Fe_2S_2(NO)_4] consist of discrete cations [Et_4N]~+ and anions     

1-苯基-3-甲基-4-苯甲酰基-吡唑啉酮-5(HPMBP)的金属离子配合物的结构研究——Ⅰ.HPMBP及其配合物Cu(PMBP)_2的晶体结构

本文研究了Cu(PMBP)_2和HPMBP的单晶体结构,晶体学参数为:(1)HPMBP,C_(17)H_(14)0_2N_2,M=278.31,单斜晶系,空间群P2_1/a,a=11.406(5),b=9.087(1),c=13.467(3)(?),β=90.76(3)°,V=1395.7(?)~3,Z=4,D_c=1.324g cm~(-3),μ=0.95cm~(-1).(2)Cu(PMBP)_2,C_(34)H_(26)O_4N_4Cu,M=618.16,单斜晶系,空间群P_2_1/c,a=6.809(3),b=23.722(8),c=9.102(3)(?),β=108.94(4)°,V=1390.7(?)~3,Z=2,D_c=1.476g cm~(-3) μ=8.67cm~(-1).结果表明,HPMBP具有烯醇式结构,其中两个给体氧原子处于有利于形成六元螯合环的几何位置;在配合物Cu(PMBP)_2中,Cu原子为对称中心,两个配体中的四个氧原子形成以Cu为中心的近似平面正方形的配位结构,Cu-O距离分别为1.906和1.896(?).     

具有生物活性的金属配合物研究——Ⅴ.3,6-二-[二甲氨基]-二苯并碘六环镝二氨三乙酸配合物的晶体结构及分子结构

合成了标题化合物并测定了它的晶体及分子结构。晶体属正交晶系,空间群P2_12_12_1。晶胞参数a=15.154(3),b=18.234(3),c=24.010(3)A;V=6634.5A~3,Z=4,D_c=1.751,D_o=1.756g/cm~3,F(000)=3468e,μ=172.8cm~(-1).配位阴离子组成为[Dy(NTA)_2)~(3-),镝的配位数为8;阳离子为三个[IC_(17)N_2H(20)]~ 。阴、阳离子间除静电相互作用外,尚有一定键合作用。     

2,2,7,7-四甲基-5,6-二氧代-9-(2-氯苯基)-10-(4-甲基苯基)-9,10-二氢-2H-吖啶的合成和晶体结构

标题化合物2,2,7,7-四甲基-5,6-二氧代-9-(2-氯苯基)-10-(4-甲基苯基)-9,10-二氢-2H-吖啶(C30H32ClNO2,Mr=474.02)是由邻氯苯甲醛和5,5-二甲基-1,3-环己二酮和对甲基苯胺以乙二醇作溶剂在微波辐射下而得到的。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群P21/c,a=12.048(3),b=11.044(2),c=19.989(5)?b=101.42(2),Z=4,V=2607(1)3,Dc=1.208g/cm3,m(MoKa)=0.173mm-1,F(000)=1008,R=0.0450,wR=0.0869。X-射线衍射分析表明:原子C(8),C(13),C(14),C(15),C(20)和N形成1个六员环,采用船式构象,六员环C(8)~C(13)和C(15)~C(20)采用半椅式构象。     

Synthesis and Crystal Structure of Methyl(7,7-Dimethyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl)Carboxylate

<正>The title compound methyl (7,7-dimemyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl) carboxylate (C19H20ClNO4, Mr = 361.81) was synthesized and crystallized. The crystal belongs to triclinic, space group P 1 with a = 8.519(2), b = 10.346(2), c = 11.481(3) A, α = 108.16(1), β = 107.78(2), γ= 91.83(2)°, Z = 2, V = 906.5(3) A3, Dc = 1.326 g/cm3, μ(MoKα) = 0.234 mm-1, F(000) = 380, R = 0.0467 and wR = 0.1270 for 3142 observed reflections (I > 2σ(I)). X-ray analysis reveals that the C(7), C(8), C(9), O(1), C(10) and C(11) atoms form a six-membered ring which adopts a boat conformation. In the ring, the distances of C(8)-C(9) and C(10)-C(11) are 1.332(3) and 1.357(3) A, respectively, which indicates that they are C=C double bonds. Another six-membered ring (C(8)-C(9)-C(15)-C(14)-C(13)-C(12)) adopts the half-chair confonnation. In addition, there are intermolecular hydrogen bonds in the crystal structure.     

Synthesis and X-ray Crystal Structure of a New Molecular Clip

The synthesis and X-ray crystal structure of a new molecular clip 2 was reported. It （C24H24N4O2, Mr = 400.47） crystallizes in the space group C2/c with a = 15.587（2）, b = 8.5805（12）, c = 15.259（2） A, β = 102.448（3）°, V= 1992.9 （5）A63, Z = 4, Dc = 1.335 g/cm63,μ = 0.087 mm^-1 and F（000） = 848. It remains monomeric in the crystal and a tape-like structure is formed in the crystal structure of molecular clip. The most unusual structural feature of 2 is the boat conformation of its cyclohexyl ring imposed by the ring fusion at C（9）-C（9a）.     

Synthesis and Crystal Structure of 3,7,7-Trimethyl- 1-phenyl-4-（3-nitrophenyl）- 4,5,6,7,8,9-hexahydro-1H-pyrazolo [3,4-b]quinoline-5（6H）-one

The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-l-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a=16.3331(10), b=13.8329(9), c=19.4163(12) A, V= 4386.8(5)A3, Z=8, Dc=1.298g/cm^3,μ=0.087 mm^-1, F(000)=1808, Mr=428.48, the final R=0.0519 and wR=0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.     

CRYSTAL AND MOLECULAR STRUCTURES OF THE DERIVA-TIVES OF ( + )- 1K, 3K(S) , 5S-2,4,3-DIAZAPHOSPHABICYCLO-[3. 2. 1]OCTANE

<正> Compound C9H19N2OPS (1) , Mr = 234. 3, monoclinic, space group P21, a = 7. 5637(2), b = 7. 704(2), c=10. 258(1) (?) ,β = 98. 66(2)°, V = 590. 9(?)3, Z =2, Dc=1. 317g/cm3, F(000) = 252. The final R = 0. 063 and Rw = 0. 080 with unit weight for 870 observed reflections (I≥3σ(I)). Compound C10H22 N3PS(2), Mr = 247. 34, monoclinic, space group P21, a = 7. 656(1), b = 8. 248 (1), c=10.750(l)(?), β=91.31(1)°, 7 = 678.73(?)3, Z = 2, Dc=1. 21g/cm3, final R = 0. 066 and Rw = 0. 081 with unit weight for 813 observed reflections (I≥3σ (I)), F(000) = 268. Both skeletons of (1) and (2) have similar geometry, which is composed of three rings : a seven-membered ring in a boat form, a six-membered ring in a chair conformation, and a five-membered ring in envelope form. The configura-tions of the chiral phosphorus atoms are assigned as 3R for (1) and as 3S for (2).     

X-ray Structure of 1- (3' -Phenyl-4' -morpholinyl-2' 5' - dithiole-1' - ylidene)-3, 4-biscarboethoxy-2-thionaphthalene

1INTR0DUCTIONa-Thiocarbonylthioformamideshavebeensynthesizedsince1980[l-23,however,thereisn0reP0rtofthesecomP0undsrelatedtheirpropertiesandreactivities(3).Ac-cordingtothepublishedpapers('-",adithioketone,adithioesterandadithioth-ioesteraresnitablefort4 2JcycloadditionwithalkenicandacetylenicdienophileS.Wewanttoknowwhethera-thiocarbonylthioformamideshavethesamecharacters,thereforethereactionofathiobenzoylthioformmorpholine(1)withdiethylacetylenedicarboxylate(2)wasexplored.Theredultsshowth…     

螺〔1-溴-4-l-孟氧基-5-氧杂-6-氧代双环〔3.1.0〕己烷2,3’-(4’-甲氧基5’孟氧基丁内酯)〕的晶体结构

本文报道了利用新手性源合成的标题化合物C2 9H45 BrO7(Mr=5 85 .5 6 )的晶体结构 ,该晶体属正交晶系 ,空间群为P2 1 2 1 2 1 ,晶胞参数a =9.748(4) ,b =12 .5 37(5 ) ,c =2 5 .85 1(9) ,V =315 9(2 ) 3,Z =4,Dx=1.2 31g/cm3,μ =1.341mm- 1 ,F(0 0 0 ) =12 40 ,偏离因子R =0 .0 475 ,Rw=0 .0 6 0 9;分子中共有 5个环 ,12个手性中心 ,2个六元环呈椅式构象 ,2个五元内酯环呈信封式构象 ,并分别与环丙烷形成〔2 .4〕螺环和〔3 .1.0〕稠环 ,4个新生成的手性中心的绝对构型为C(13) (S) ,C(14 ) (S) ,C(15 ) (R) ,C(16 (R) ,无任何对称因素     

Crystal Structure of 1，6：3，4－Dianhydro－β－D－galactopyranose－2－O－p－tolylsulfonate（C_13H_14O_6S）

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ１，６：３，４－Ｄｉａｎｈｙｄｒｏ－β－Ｄ－ｇａｌａｃｔｏｐｙｒａｎｏｓｅ－２－Ｏ－ｐ－ｔｏｌｙｌｓｕｌｆｏｎａｔｅ（Ｃ_１３Ｈ_１４Ｏ_６Ｓ）ＷａｎｇＡｎ－Ｌａｉ；ＬｕＳｈｉ－Ｊｉｅ；ＦｕＨｏｎｇ－Ｘｉａｎｇ；Ｗａ?..     

Crystal Structure and Conformation of [1-(β-D-lyxofuranosyl)uracil]-2′-spiro-5″-[4″-(S)-(diethoxyphosphinyl)-2″-oxazoline]

The title compound, C15H22N3O9P·2H2O, Mr=455.36, crystallizes in orthorhombic, space group P212121, with a =9.193(2), b =14.681(3), c =15.201(3)A, V =2501(1)A3, Z =4, Dx=1.474g/cm3, λ(MoKα)=0.71073A, μ=0.1894mm-1, T=299±1K, F(000)=960, R=0.061 and Rw=0.068 for 1899 observed reflections with I≥3σ(I). The analysis results indicate that the title compound is of lyxo-configuration and the configuration at C4″ is S. In the crystal state the molecule has anti conformation about glycosidic bond with the torsion angle-151.7°, the sugar ring is puckered with C3′-endo-C2′-exo, and the conformation of the C4′-C5′ bond is-sc.     

Synthesis and Crystal Structure of N-methyl- 9- （4-bromophenyl）-1,2,3,4,5,6,7,8,9,10- decahydroacridine- 1,8-dione under Microwave Irradiation

1 INTRODUCTION Since the discovery of pharmacological effectsof 1,4-dihydropyridine (1,4-DHPs) as calcium mo-dulators[1], a great deal of work has been directedtowards the synthesis of 1,4-DHPs acting as cal-cium antagonists[2]. The chemical modifications onthe DHP ring, such as the introduction of differentsubstituents on heteroatoms[3], have allowed theexpansion of researches on structure-activity rela-tionship to have new insight into the molecularinteractions at the receptor l…