新磺酰脲类化合物的合成、结构及构效关系研究(Ⅵ)1—N-〔2-(4-甲基)嘧啶基〕-2-甲酸甲酯-苄基磺酰脲的晶体及分子结构

合成了标题化合物 C6H4 (CO2 CH3 ) CH2 SO2 NHCONHC4 N2 H2 CH3 (C15H16N4 O5S,Mr=36 4 .38) ,用 X-射线晶体衍射法测定了其晶体结构。它属单斜晶系 ,空间群为P2 1/ c,a=10 .2 2 0 (1) ,b=9.938(1) ,c=17.2 4 6 (2 ) ,β=10 6 .2 6 (2 )°,V=16 81.6(3) 3 ,Z=4 ,Dc=1.4 39Mg/ m3 ,μ=0 .2 2 7mm-1,F (0 0 0 ) =76 0。结构由直接法解出 ,全矩阵最小二乘法修正 ,最终偏离因子 R=0 .0 4 98,w R=0 .132 7(I>2 σ(I) ) ,独立可观测点数为 3448。分子中的嘧啶磺酰脲、苯环及酯基分别形成 3个独立的平面共轭体系。     

吡啶-2-甲醛缩水杨酰腙锌(Ⅱ)和镍(Ⅱ)配合物的合成及晶体结构

利用水热法合成2种吡啶-2-甲醛缩水杨酰腙配合物[Zn(C13H10N3O2)2]·H2O(1)和[Ni(C13H11N3O2)2]2(CH3CH2OH)(SO4)2·3H2O(2),并测定了晶体结构.结果表明1属单斜晶系,空间群P21/c,其晶胞参数为:a=12.4352(14),b=17.878(2),c=13.8...     

Crystal Structure of catena-[(Tetrakis-μ2-acetato-μ2-4,4'-bipyridine) dicopper(Ⅱ)] Acetonitrile Solvate

The title compound,[Cu2(CH3COO)4(C8H10N2)]n·nCH3CN1 (C8H10N2,4,4'-bipy = 4,4'-bipyridine),has been solvothermally synthesized in CH3CN and characterized by X-ray diffraction.The crystal is of monoclinic,space group Cc with a = 22.626(6),b = 14.012(4),c =15.106(4) (A),β = 107.610(3)°,V = 4565(2) (A)3,C20H23Cu2N3O8,Mr = 560.49,Z = 8,Dc = 1.631 g/cm3,μ = 1.914 mm-1,Flack parameter = 0.48(1),F(000) = 2288,R = 0.042 and wR = 0.)98 for 8887 observed reflections (I ＞ 2σ(I)).It consists of nearly linear one-dimensional chains [Cu2(CH3COO)4(C8H10N2)]n derived from paddle-wheel [Cu2(CH3COO)4] unit linked by 4,4'-bipy,and CH3CN as guest molecule regularly decorates between the chains.     

新磺酰脲类化合物N-[2-(4-甲基)嘧啶基]-N''''-2-甲氧羰基苯磺酰脲的合成及其二聚体结构

合成并用X-射线晶体衍射法测定了标题化合物 (C14H14N4O5S, Mr = 350.35)的结构。晶体属正交晶系, 空间群为Pna21, 晶胞参数a = 13.242(4), b = 9.478(3), c = 24.889(8) ? V = 3123.7(17) 3, Z = 8, Dc = 1.490 g/cm3, m = 0.241 mm-1, F(000) = 1456。独立可观测点数为3268。最终偏离因子R = 0.0592, wR = 0.1217 (I > 2s(I) 2153), S = 1.122。X-射线衍射证实标题化合物分子晶体中存在2种构型, 分子中苯环所在的位置同嘧啶磺酰脲平面的取向相反。每种构型中嘧啶磺酰脲、苯环及甲氧羰基分别形成3个独立的平面共轭体系。除此之外, 经由O(1)N(6)和N(2)O(6)形成的分子间氢键以及苯环平面间的p-p 相互作用将2个分子结合在一起从而形成二聚结构。     

钼铁硫原子簇化合物的合成与结构化学研究II: 以Fe(SR)6为桥的双类立方烷化合物的合成及(Et4N)4[Mo2Fe7S8(SC6H4CH3-m)12].2THF的晶体结构

在乙腈溶液中(Et4N)2[Fe4(SR)10]与(Et4N)2[MoS4]反应半小时生成对氧极为敏感的系列黑色晶状化合物(Et4N)4[Mo2Fe7S8(SR)12](R=C6H5,1;R=C6H4CH3-m, 2;R=C6H4CH3-o, 3;R=C6H4CH3-ρ,4). 2.2THF晶体的分子量为2982.8, 属单斜晶系;空间群为P21/n; a=18.022(2), b=18.375(2), c=22.254(3)A; β=71.04(1)°;V=6969(2)A^3;Dc=1.424g.cm^-^3;Z=2;F(000)=3108.晶体结构用直接法解出,修正至R=0.064. 2.2THF中Mo...Mo'距离为7.234A.     

STRUCTURAL STUDIES OF trans-1,2 CYCLOHEXANEDIA-MINETETRAACETIC ACID HYDRATE]·C_(14)H_(22)N_2O_8·H_2O

<正> C14H22N2O8. H2O,Mr = 364. 4, monoclinic,P21/n,a =11.536(2),b= 10. 744(2),c=13. 271(3)A,B=99. 87(2) ,V=1620.5A3,Z=4,Do=1. 47,Dc= 1. 493gcm-3,F(000) = 776,u(MoKa) = 1. 17cm-1.The structure was solved by direct methods and refined to R=0. 059 for 2743 observed reflections with I>3 o(I).The molecule of trans-1,2-cyclohexanediaminetetraacetic acid exists in the crystal in a zwitte-rionic form -OOCCH2N+H(CH2COOH) C6H10N(CH2COOH)2. There is no intramolecular hydrogen bond,but intermolecular hydrogen bonds exist between water molecule and car-boxyl group as well as between the carboxyl groups.     

CRYSTAL STRUCTURE OF 3-NITRO-2, 6-BIS(4''''-BENZO-15-CROWN-5)-AMINOPYRIDINE POTASSIUM PICRATE HYDRATE METHANOL, (C_(33)H_(42)N_4o_(12)K)C_6H_2N_3o_7·H_2O ·CH_3OH

<正> The title compound, (C33H42N4O12K)C6H2N3O7·H2O·CH3OH,Mr = 1003. 98,space group P1,a=11. 458(2) ,b= 14. 565(6) ,c=15. 828(3) A ;α=63. 34 (2),β=74. 06(1),γ=81. 03(2)°,V=2268. 1 A3;Z = 2,Dx = l. 47g/cm3,λ=0. 71069 A (MoKa).The final R = 0. 041 for 1700 observed reflections (I≥3σ(I)). The molecule is sandwich-like, and the cation K+ is sandwiched between the two crown rings.     

新磺酰脲类化合物的合成、结构及构效关系研究(I)——N-(2''''-嘧啶基)-2-甲酸乙酯-苯磺酰脲的晶体及分子结构

本文在合成标题化合物的基础上,测定了其晶体结构.晶体属单斜晶系,空间群为P2_1/a.晶胞参数a=0.7348(2)nm,b=2.1496(4)nm,c=0.9973(2)nm,β=90.19(2)°,V=1.576nm~3,Z=4.晶体结构由直接法解出,进行全矩阵最小二乘法修正,R=0.059.分子中的嘧啶磺酰脲、苯环及酯基三部分分别形成3个独立的平面共轭体系.S-N原子间形成d-pπ键并参加到第一个共轭体系中.分子中还存在着N与H原子间的分子内氢键.     

丙酰皮考林酰肼(C_9H_(11)N_3O_2 )的合成和晶体结构

合成了标题化合物(C9H11N3O2,Mr=193.21),晶体属于单斜晶系,空间群为C2/c, a=13.703(1),b = 9.142(1), c = 16.437(2)?, ( = 105.547(3)(,V = 1983.8(4)?,Z = 8, Dc=1.294g/cm3, F(000)= 816,(??o?α)=0.094 mm-1,R=0.0527, wR=0.1517,I(2((I)的可观察衍射点1596个。有机分子间以氢键相联并形成网状结构,N(2)-H...N(1a)(a: -x+1, y, -z+1/2)和N(3)-H…O(2b)(b: -x+1/2, y-1/2, -z+1/2)键键长分别为3.007(2)和2.786(2)?。     

Synthesis and Crystal Structure of a New Tetracopper Complex [Cu(H_2O)_3Cu(HCDTA)]_2(ClO_4)_2·H_2O

A new tetracopper complex [Cu(H2O)3Cu(HCDTA)]2(ClO4)2·H2O (CDTA = transcyclohexane-1,2-diamine-N,N,N′,N′-tetraacetate) has been prepared and characterized by singlecrystal X-ray diffraction analysis. The crystal adopts space group C2/c with a = 16.990(10), b = 9.150(5), c = 29.318(17) , β = 104.289(9)°, V = 4417(4) 3, Z = 4, C28H52Cl2Cu4N4O31, Mr = 1265.80, Dc = 1.904 g/cm3, μ = 2.130 mm-1, F(000) = 2584, T = 293(2) K, the final R = 0.0328 and wR = 0.0809 for 4938 observed reflections (I 2σ(I)). The tetracopper units are interconnected by weak covalent bonds into a layered structure.     

2-(甲苯-4-磺酰胺基)-苯甲酸的晶体结构、光谱及热性质

报道了2-(甲苯-4-磺酰胺基)-苯甲酸(I)的元素分析和红外、核磁共振光谱性质并通过单晶X射线衍射确定了其晶体结构. 晶体属单斜晶系, 空间群为C2/c,晶胞参数为, a=2.7320(3) nm, b=0.85441(8) nm, c=1.17607(11) nm, α=90°, β=98.728(3)°, γ=90°, V=2.7135(5) nm3, Z=8. 晶体中分子单体通过N—H…O 和O—H…O氢键作用形成具有中心对称的二聚体, 且进一步通过两种不同的C—H…O 氢键和π…π作用形成超分子结构. 在不同的溶剂中, 化合物I的紫外吸收表现出明显的溶剂效应, 此外, 荧光光谱与DSC-TGA热重分析表明, 该化合物是一种耐热的荧光材料.     

N,N,N'''',N''''-四[2-(1-乙基苯并咪唑)甲基]乙二胺及其高氯酸盐的晶体结构

本文通过单晶X-射线衍射法测定了EtEDTB1.4C2H5OH5H2O 1和H4EtEDTB(ClO4)4 C2H5OH 2的晶体结构。晶体学数据如下:1的分子式为C44.8H66.4N10O6.4, Mr = 847.48, 属三斜晶系, 空间群P, a = 11.489 (2), b = 11.866(3), c = 12.002(3) , = 97.47(2), ?= 114.564(13), ?= 114.11(2)? V = 1266.6(5) 3, Z = 1, Dc = 1.111 g/cm3, F(000) = 456, m(MoK? = 0.076 mm-1。共收集衍射数据5207条, 其中独立衍射数据4323条(Rint = 0.0257), 1318条可观测衍射数据(I > 2(I))用于结构计算。结构由直接法解出, 并用全矩阵最小二乘法修正, 最终偏离因子R = 0.0706, wR = 0.1802。分子具有对称中心, 4个苯并咪唑基团围绕中心呈螺旋桨状均匀排布。在1的晶体中, EtEDTB分子通过水和乙醇的氢键相连形成二维网状结构。2的分子式为C44H58Cl4N10O17, Mr = 1140.80, 属单斜晶系, 空间群C2/c, a = 24.260(5), b = 13.040(3), c = 17.680(4) , ?= 97.50(3)? V = 5545.2(2) 3, Z = 4, Dc = 1.366 g/cm3, F(000) = 2384, m(MoK? = 0.289 mm-1。共收集衍射数据12055条, 其中独立衍射数据6360条(Rint = 0.0408), 2875条可观测衍射数据(I > 2(I))用于结构计算。结构由直接法解出, 并用全矩阵最小二乘法修正, 最终偏离因子R = 0.0692     

(Z)-1-苯基-1-对氟苯基-2-对甲苯磺酰基-1,4-戊二烯的合成及其晶体结构

通过1-苯基-2-对甲苯磺酰基乙炔、对氟苯基氯化锌及烯丙基溴的三组分串联反应,合成了(Z)-1-苯基-1-对氟苯基-2-对甲苯磺酰基-1,4-戊二烯(1),其结构经1H NMR, 13C NMR, IR, HR-MS和XRD表征.1为Z-构型,属单斜晶系,空间群P21/c, a=9.899 1(20)(A), b=9.621 9(20)(A), c=21.812 9(15)(A), β=95.575(10)°, V=2067.8(6)(A)3, Z=4, Dc=1.254 g·cm3, μ=0.181 mm-1, λ=0.710 73(A), F(000)=816, R=0.046 3, wR=0.134 1.共收集到3 684个独立衍射点,其中I>2σ(I)的可观察点为2 989.     

[Ni(C_5H_5N)_2(C_7·H_6O_2N)_2]H_2O三元配合物的合成及晶体结构

合成了标题化合物。该化合物的分子式[Ni(C5H5N)2(C7H6O2N)2]H2O(C24H24N4NiO3),分子量475.18,采用单色的MoKα (λ = 0.71073 )射线测定,共收集7408个数据,其中独立衍射点2567个(Rint = 0.0272),I > 2s(I)可观测点数1926个,结果表明该化合物属单斜晶系, 空间群C2/c其晶胞参数为: a = 14.466(2),b = 12.193(2),c = 14.072(2) ;β = 116.229(2)°,V = 2226.6(5) 3,Z = 4,Dc = 1.418 g/cm3 ,μ = 0.905 mm-1,F(000) = 992. 2个水杨醛亚胺各提供2个配位原子参与配位,2个吡啶各提供1个配位原子参与配位,该配合物是六配位的八面体构型,同时讨论了该体系中不同配位原子的配位能力的差异。     

Reaction of Mo(CO)_6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et_4N]_3[Mo_2(CO)_6(μ-OC_6H_4OCH_2C_6H_5)_3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a = 15.359(2), b = 18.378(3), c = 24.952(2), β = 102.268(4)°, V = 6882.3(16) 3, Mr = 1348.34, Z = 4, Dc = 1.301 g/cm3, F(000) = 2832 and μ = 0.424 mm-1. The final R = 0.0606 and wR = 0.1552 for 9396 observed reflections (I > 2σ(I)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) , indicating no metal- metal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

2D氢键网络镉配合物Cd(pyridine-2-sulfonato)2(H2O)2和锌配合物Zn(pyridine-2-sulfonato)2(H2O)2的合成和晶体结构

合成了镉的吡啶-2-磺酸配合物Cd(C5H4NSO3)2(H2O)2 1和锌的吡啶-2-磺酸配合物Zn(C5H4NSO3)2(H2O)2 2。 研究表明, 2个化合物属异质同晶, 均属单斜晶系, 空间群为C2/c. 化合物1晶胞参数为:a = 13.7671(5), b = 7.2778(3), c = 16.1559(9) ? b = 106.656(3)? V = 1550.8(1) 3, Z = 4, Dc = 1.990 g/cm3, m =1.719 mm-1, F(000) = 920, R = 0.0225, wR = 0.0584, 共收集到1759个独立衍射点, 其中I≥2(I)的可观测点为1681个;化合物2晶胞参数为:a = 13.711(1), b = 7.1451(9), c = 15.972(1) , b =107.079(5)? V = 1495.7(3) 3, Z = 4, Dc = 1.855 g/cm3, m = 1.964 mm-1, F(000) = 848, R = 0.0310, wR = 0.0831, 共收集到1707个独立衍射点, 其中I≥2(I)的可观测点为1592个。在2个标题配合物中, Cd2+离子(或Zn2+离子)由2个吡啶-2-磺酸中的2个氮和2个氧以及2个水分子中的2个氧配位形成畸变的N2O4八面体配位构型。每个配合物分子具有晶体学2次旋转轴对称性。配合物分子之间通过许多OH(配位水分子)LO(未配位磺酸根)氢键联结成二维结构网络。     

Synthesis and Crystal Structure of a New Complex Zn(Ⅱ)L_2·2CH_3OH(H_2L = 4-Chloro-2-(2,3-dihydro-1H-benzoimidazol-2-yl)-phenol)

A new complex Zn(Ⅱ)L2·2CH3OH(H2L = 4-chloro-2-(2,3-dihydro-1H-ben-zoimi-dazol-2-yl)-phenol) has been prepared and characterized by single-crystal X-ray diffraction analysis and elemental analysis.The crystal is of triclinic system,space group P1 with a = 9.2905(10),b = 10.3555(13),c = 14.9590(14) ,α = 101.0340(10),β = 101.261(2),γ = 99.1660(10)o,V = 1356.1(3) 3,Z = 2,C28H24Cl2N4O4Zn,Mr = 616.78,Dc = 1.510 g/cm3,μ = 1.145 mm·1,F(000) = 632,the final R = 0.0379 and wR = 0.0830 for 3606 observed reflections with I 2σ(I).The Zn(Ⅱ) atom presents a distorted square pyramidal coordination involving two H2L ligands.The hydrogen bonds and π···π stacking interactions extend the complex into a two-dimensional framework.     

Synthesis and Crystal Structure of 3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)- pyrrol-2-yl)pentane·2CH_3OH

3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)pyrrol-2-yl)pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·(CH3OH)2, belongs to the orthorhombic system, space group Pccn with a = 18.094(2), b = 11.6890(16), c = 13.3629(19) , V = 2826.3(7) 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F(000) = 1080 and μ(MoKα) = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ(I), and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.     

Synthesis,Crystal Structure and Neuroprotection of Methyl 2-（（4-（2-（2-Methylphenoxy）acetyl）- piperazin-1-yl）-methyl）benzoate①

A new phenoxyacetamide derivative, methyl 2-((4-(2-(2-methylphenoxy)acetyl)piperazin-1-yl)methyl)benzoate(C22H26N2O4, Mr = 382.45), has been synthesized and characterized by 1H NMR, 13 C NMR, H RMS and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a = 11.145(2), b = 13.667(3), c = 13.998(3)A, β = 112.01(3)o, V = 1976.8(7)A3, Z = 4, Dc = 1.285 g/cm3, F(000) = 816, μ = 0.089 mm-1, MoKα radiation(λ = 0.71073 A), the final R = 0.0602 and wR = 0.1533 for 2343 observed reflections with I 2σ(I). Intramolecular C–H···O interactions as well as intermolecular C–H···O hydrogen bonds help to stabilize the crystal structure. The preliminary bioassay results show that the title compound exhibits potent neuroprotective activity.     

Synthesis, Crystal Structure, and Photoluminescent and Semiconductive Properties of [La(C6NO2H5)3-(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O)

A new heterometallic 4f-5d inorganic-organic metal-isonicotinic acid complex [La(C6NO2H5)3(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydro-thermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell: α= 24.140(7), b = 20.884(7), c = 15.462(2) (A), β = 127.46(1)°,V = 6187(3) (A)3, C36H47Cl13Hg3La2N6O20, Mr = 2224.24, Dc = 2.388 g/cm3, Z = 4, T = 293(2) K, μ(MoKα) = 9.401 mm-1, F(000) = 4160 and R/wR = 0.0376/0.0636 for 4130 observed reflections (I > 2σ(I)) and 5617 unique reflections. Complex 1 is characteristic of a one-dimensional polycationic chain-like structure. Photoluminescent investigation reveals that the title complex displays interesting emissions in violet and orange regions. The luminescence spectra show stronger orange emission than violet emission. Optical absorption spectra of 1 reveal the presence of a wide optical bandgap of 3.41 eV.