具有三维超分子结构的单核Ni(Ⅱ)配合物[Ni(nas)2(phen)2]的合成、表征及晶体结构

水热合成了镍(Ⅱ)-2-萘胺-1-磺酸-邻菲哕啉三元配合物[Ni(nas)2 (phen)2],并用红外、元素分析、热重、固体紫外和X-射线单晶衍射法对配合物的晶体结构进行了表征.结果表明,该配合物属于四方晶系,空间群P41212,晶胞参数a=1.24321(4) nm,b=1.24321(4) nm,c =2.45032(16) nm,α=90.00°,β=90.00°,γ=90.00°,V=3.7871(3) nm3.     

新的NLO化合物Ce(MoO2)(OH)(IO3)4的合成和晶体结构

新的NLO化合物Ce(MoO2)(OH)(IO3)4由水热法在170℃下制备得到.X射线单晶结构分析表明,该化合物以极性空间群P21结晶,晶体学参数为:a=0.70144(8)nm,b=1.41554(10)nm,c=0.70969(6)nm,β=115.318(7)°,V=0.6369(1)nm3,Z=2.Ce(MoO2)(OH)(IO3)4的晶体结构是由八配位的Ce3+阳离子,高度畸变的MoO66-八面体,和碘酸根阴离子基团组成的复杂三维网所构成.分析其结构表明,含有Ⅰ(3)和Ⅰ(4)的碘酸根基团的孤电子对的合成方向指向极化轴b,从而导致晶体结构具有非中心对称性.此外,红外光谱进一步证实了MoO66-,IO3-基团和Mo-OH作用的存在.     

基于柔性芳香羧酸配体的三维镉(Ⅱ)配位聚合物的合成、晶体结构及荧光性质

以Cd(NO3)2·4H2O和5-(4-羧基苯氧基)烟酸(H2L)为原料,用水-DMF溶剂热合成法合成了一个新型三维配位聚合物[Cd(L) (H2O)2]n,并采用红外光谱、元素分析、热重分析和X射线粉末衍射对其进行了表征.晶体结构由X射线单晶衍射仪分析确定,该配合物属于单斜晶系,P21/n空间群,晶胞参数为a=0.6201(2) nm,b=0.8225(3) nm,c=2.6361 (10) nm,α=90.00°,β=90.101 (7)°,γ=90.00°,V=1.3444(9) nm3,Z=4.在该配合物中,每个Cd(Ⅱ)的配位环境为六配位的八面体构型,金属Cd(Ⅱ)通过配体离子L2-连接形成一个三维的框架结构.室温固态荧光测试结果表明,该配合物具有一定的荧光性.     

基于4-(1H-吡唑-3-基)-吡啶构筑的新型Zn(Ⅱ)配位聚合物的合成、晶体结构和性质研究

采用水热法,合成了一个Zn(Ⅱ)配位聚合物[Zn3(4-PP)4(OH)2(SO4)2(H2O)2]n(1,4-PP=4-(1H-pyrazol-3-yl) pyridine),并用元素分析、红外光谱和X-射线单晶衍射对其进行了表征,测定了其热重性质和荧光性质.该配位聚合物1属于单斜晶系,P21/c群,其晶胞参数为:a=12.303(3) nm,b =6.0083(12) nm,c=25.308(5) nm,β=101.40(3)°,F(000)=1056,Dc=1.882 g/cm3,V=1833.8(6) nm3,Mr=1038.94,Z=2,μ(MoKα)=2.140 mm-1,R1=0.0672,wR2 =0.1300.在该配位聚合物1中,金属锌(Ⅱ)与SO24-以及OH-形成纯无机的二维层状结构,而4-PP配体仅作为端基配体;二维结构进一步通过氢键的作用形成三维超分子结构.     

新型链状化合物Mn3（dap）2（AsS3）2的溶剂热合成与表征

用溶剂热方法合成了一种新型链状化合物Mn3(dap)2(AsS3)2(dap=1,2-丙二胺),通过单晶X-射线衍射技术对其进行了晶体结构分析,该化合物属于单斜晶系,空间群C2/c。晶胞参数a=2.0869(14)nm,b=0.8745(6)nm,c=1.2496(8)nm,β=121.141(10)°,Z=4。标题化合物由两个相对称的[AsS3]3-三角锥与两个对称的过渡金属胺螯合物[Mn(dap)]2+通过共用S原子连接形成{[Mn(dap)]2(AsS3)2}2-原子簇,这些原子簇之间由四配位的Mn1进一步连接,形成沿c轴延伸的{Mn3(dap)2(AsS3)2}n一维链。紫外-可见漫反射光谱研究表明,化合物为宽带半导体,带隙Eg=2.5 eV。同时对该化合物进行了IR、XRD、XPS等表征。     

无机-有机杂化晶体[C_(12)H_(11)N_2O_2][Cd(SCN)_3]的合成和晶体结构(英文)

合成了无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3],并采用元素分析、红外光谱表征和单晶X射线衍射分析和热重分析研究.红外光谱分析表明SCN-采用1,3-μ模式.结构分析表明,相邻的Cd(II)原子通过三个1,3-μ-SCN- 阴离子桥连形成无限的[Cd(SCN)-3]∞之字链结构,固体结构中[C12H11N2O2]+阳离子和[Cd(SCN)-3]∞配阴离子形成了分离柱状堆积.该晶体属于单斜晶系P2(1)/c空间群,晶胞参数分别为:a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3 , T = 293(2) K, μ = 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)]. 热分析结果在180-305 ℃化合物失去一个有机分子,305 ℃以上伴随着镉升华失去三个SCN-阴离子.     

Na3La2(BO3)3的晶体结构

以Na2CO3-H3BO3-NaF为助熔剂,使用顶部籽晶法生长出Na3La2(BO3)3透明单晶.测定了Na3La2(BO3)3的晶体结构,该晶体属正交晶系,空间群:mm2(No.38),晶胞参数为a＝0.51580(10)nm,b=1.1350(2)nm,c=0.73230(15)nm,α＝β＝γ＝90°,V＝0.42871(15)nm3,密度:.053g/cm3.晶体结构中的硼氧基团是平面的BO3基团,BO3基团相互独立,且与Na(1)O6、Na(2)O8、Na(3)O6和La(1)O9配位多面体连结形成三维网络骨架结构.讨论了Na3La2(BO3)3的晶体结构与倍频效应的关系.     

锌(Ⅱ)配位聚合物{[Zn(CPGA)(DPPP)]H2O}n的合成和晶体结构

采用水热法合成了一个锌的新型配位聚合物{[Zn(CPGA)(DPPP)]·H2O｝n(1),[CPGA=3-(4-氯苯基)戊二酸根,DPPP=l,3-二(4-吡啶基)丙烷],用元素分析、红外光谱和X-射线单晶结构等进行了表征.结果表明该配位聚合物属于单斜晶系,P21/n空间群.晶胞参数为:a=1.3775(2) nm,b=1.20745(19) nm,c=1.4854(2) nm,F(000)=1080,Dc=1.419 g·cm-3,V=2.4446(7) nm3,Mr=522.28,Z=4,μ=1.151 mm-1,月1=0.0389,ωR2=0.1253.该配位聚合物晶体中,Zn(Ⅱ)与配体3-(4-氯苯基)戊二酸根和DPPP连接形成一维波浪面结构,水分子和3-(4-氯苯基)戊二酸根中未参与配位的氧原子形成的氢键将相邻的两层连接形成双层结构,双层结构没有进一步连接.     

锌（Ⅱ）配位聚合物[Zn（HCPGA）2（H2O）2]n的合成和晶体结构

以3-(4-氯苯基)戊二酸(H2CPGA)为主要配体采用微波合成法合成了一个锌的新型配位聚合物[Zn(HCPGA)2(H2O)2]n(1),用元素分析仪、荧光光谱仪、红外光谱仪、热重分析仪和单晶衍射仪等对其进行了表征。结果表明该配位聚合物属于单斜晶系,空间群是C2/c。晶胞参数:a=2.9922(12)nm,b=0.7370(3)nm,c=1.0924(4)nm,β=98.008(6)°,F(000)=1200,Dc=1.628 g·cm-3,V=2.3855(16)nm3,Mr=584.68,Z=4,μ=1.309 mm-1,R1=0.0352,wR2=0.1124。     

二2-(2'-吡啶基)苯并咪唑一水合锌(Ⅱ)配合物的合成和结构表征

采用水热法合成了新配合物二2-(2'-吡啶基)苯并咪唑一水合锌(Ⅱ)配位聚合物{[Zn(L)2·H2O]}n(1),[L=2-(2'-吡啶基)苯并咪唑],用元素分析、红外光谱和X射线单晶结构等进行了表征,结果表明该配位聚合物属于单斜晶系,P21/c空间群.晶胞参数为:a=1.25188(19) nm,b =1.30095(19) nm,c=1.3300(2) nm,β =102.676(3)°,F(000) =968,Dc=1.483 g · cm-3,V=2.1133(5) nm3,Mr=471.81,Z=4,μ=1.192 mm-1,R1=0.0539,wR2=0.0819.该配位聚合物晶体是由配位水与苯并咪唑上的氮原子形成氢键以及配体2-(2'-吡啶基)苯并咪唑之间的π-π堆积作用连接而成的无限延伸的一维链状结构.     

Synthesis and Molecular Structure of 2-(4-Chlorophenyl)-3-(phenyl-amino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one

Crystallography Reports - 2-(4-Chlorophenyl)-3-(phenylamino)-5-(thiophen-2-ylmethylidene)-3,5-dihydro-4H-imidazol-4-one, C20H14N3OSCl was synthesized and its crystal structure was determined by...     

Synthesis and X-ray structure of 3-(4-methyl phenyl)-2-(4-biphenyl)-1,3-thiazolidin-4-one

The title compound (C₂₂H₁₉NOS) was synthesized, characterized and structure was determined by X-ray diffraction method. It crystallizes in the monoclinic space group P2₁/c with cell parameters a = 22.181(2) Å, b = 6.0760(4) Å, c = 13.349(3) Å, = 95.615(3)^, and {Z = 4}. The final residual factor is 0.0625 for 1724 reflections with I > 2(I). 4-thiazolidinone ring moiety shows twisted conformation.     

Synthesis and Crystal Structures of 4-(3-Nitropyridin-2-ylamino)phenol and 4-(3-Aminopyridin-2-ylamino)phenol

Abstract  

The title compounds, 4-(3-nitropyridin-2-ylamino)phenol (I) and 4-(3-aminopyridin-2-ylamino)phenol (II), are two intermediates for the synthesis of a potential antitumor agent ABT-751. The reaction of 4-aminophenol with 2-chloro-3-nitropyridine yielded I which was converted into II by reduction. Instead of the Pd/C catalytic hydrogenation described in many literature, reduction with cheap sodium sulfide in aqueous media was utilized for shorting the reaction time and simplifying the operation. The crystal structures of the resultant compounds were determined by single-crystal X-ray diffraction. The compound I is crystallized in P2₁/c space group of monoclinic system, with a = 11.5236(19) ?, b = 8.7389(17) ?, c = 10.684(3) ? and α = 90.00°, β = 107.76(3)°, γ = 90.00°. The compound II is crystallized in Cc space group of monoclinic system, with a = 10.688(2) ?, b = 14.2181(18) ?, c = 7.9836(15) ? and α = 90.00°, β = 125.801(7)°, γ = 90.00°. In both crystal structures, the intermolecular N–H–O and O–H–N hydrogen bonds link the molecules, which effectively stabilize the structures.     

Synthesis,Crystal Structure,Spectroscopic and Electronic Properties of (E)-Trans-2-(2-(Biphenyl-4-ylmethylene)Hydrazinyl)-4-(3-Methyl-3-Phenylcyclobutyl)Thiazole

Abstract  

A new compound of (C₂₇H₂₅N₃S) has been synthesized and characterized by ¹H NMR, ¹³C NMR, IR, UV-Visible spectroscopy, and single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P2₁/c and crystals of (I) were found approximately 0.5:0.5 ratio to be twinned. The crystal structure is stabilized by N–H···N inter molecular hydrogen bonding. In addition to the molecular geometry and dimeric structure from X-ray experiment, the optimized molecular geometry for monomer and dimer, vibrational frequencies, atomic charges distribution, and total energies of the title compound in the ground state have been calculated using ab initio method. Density Functional Theory (B3LYP) and Hartree-Fock (HF) methods with basis sets 6-31G(d, p) and 3-21G were used in the calculations. Calculated frequencies are in good agreement with the corresponding experimental data. UV-Vis absorption spectra of the compound have been ascribed to their corresponding molecular structure and electrons orbital transitions.     

Synthesis, characterization, and structural analysis of ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate

Ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate was prepared by reacting the lithium salt of ethyl cyanoacetate with (Z)-O-methyl-4-chloroben-zohydroximoyl fluoride. This compound crystallizes in space group Pbca,with lattice constants a=7.5740(15) ?, b=11.337(2) ?, and c=30.424(5) ? at 110 K. Characterizations include spectrometric identifications employing IR, UV, and ¹H and ¹³C NMR. The compound exists in the solid as the enamine tautomer, with the cyano group cis to the 4-chlorophenyl group (the Z configuration). The C=C and C–N bond distances are 1.3930(16) ? and 1.3278(16) ?, respectively. The N–H group forms a bifurcated hydrogen bond with acceptors C=O (intramolecular) and C≡N (intermolecular).Supplementary material CCDC-289444 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; Fax: +44(0)1223-336033.     

The Synthesis and Crystal Determination of 3-Hydroxy-4-(4-methoxyphenyl)-5-(2-nitrophenyl)furan-2(5H)-one

Abstract  

The title compound, C₁₇H₁₃NO₆, was synthesized and structurally characterized by elemental analysis, MS, ¹H NMR and single crystal X-ray diffraction. It crystallizes in monoclinic system space group C 2/c with a = 27.981(6) ?, b = 12.996(3) ?, c = 8.0900(16) ?, β = 91.06(3)°, V = 2941.4(10) ?³, Z = 8, R ₁ = 0.0675, wR ₂ = 0.1626, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with p-methoxybenzene ring and forms a dihedral angle of 87.2(1)° with the nitrobenzene ring. O–H···O Intermolecular hydrogen bonds link pairs of molecules into centrosymmetric dimers, making a graph set motif of R ₂²(10). The dimers are further assembled into a chain of edge-fused R ₄⁴(34) rings running along the [001] direction. The final three-dimensional supramolecular architecture is stabilized by weak π–π interactions.     

X-ray structure analysis of 1-(4-bromophenyl)-3-(4-chlorophenyl)-prop-2-en-1-one

The title compound crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 15.6239(15) ?, b = 14.0537(14) ?, c = 5.8396(5) ?, β = 92.666(3)°, V = 1280.8 (2) ?³, and Z = 4. The final reliability index is 0.0538 for 2921 observed reflections. Two phenyl rings of the title molecule are not coplanar, with a dihedral angle of 46.3(0)°. The molecular planarity of this substituted chalcone is strongly affected by the 4′-bromo group. The crystal cohesion is accentuated by π···π, C–H···Br interactions and R₃ ¹ (11) hydrogen bond.     

Crystal and molecular structures of 1-(2-carboxypropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (1) (C17H21NO4) and 1-(2-carbamoyl propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C17H22N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol containing 2-methylalanine fragment are described in this paper. The space groups and unit-cell parameters are: compound1 (C₁₇H₂₁NO₄): monoclinic, space groupP2₁/n,a=5.787(1),b=18.703(4),c=23.526(5)Å,=96.49(2)°; compound2 (C₁₇H₂₂N₂O₃): triclinic, space groupP¯1,a=8.321(1),b=10.121(1),c=10.368(1)Å,=109.49(1)°,=90.49(1)°, =103.48(1)°. The structures were solved by direct methods and refined with full matrix least-squares techniques toR indices of 0.055 and 0.049, respectively. The molecules of compound1 exist in the crystal as dual ions. The molecules of compound2 are compact and their external chain is twisted in a characteristic way (similar to that found in peptides).     

Synthesis and crystal structures of 2-amino-3-cyano-4-(2-chlorophenyl)-1,4-dihydro-2H-pyrano[3, 2-h]quinoline and 2-amino-3-cyano-4-(2-chlorophenyl)-8-(2-chlorobenzylidene)-1,4,5,6,7,8-hexahydrobenzo[b]pyran

The title compounds 2-amino-3-cyano-4-(2-chlorophenyl)-1,4-dihydro-2H-pyrano[3, 2-h]quinoline 1 (C₁₉H₁₂ClN₃O, M _r = 333.77) and 2-amino-3-cyano-4-(2-chlorophenyl)-8-(2-chlorobenzylidene)-1,4,5,6,7,8-hexahydrobenzo[b]pyran 2 were synthesized and crystallized. The crystals of compound 1 are triclinic, space group P-1, a = 7.488(2), b = 9.127(3), c = 12.252(3) Å, = 73.58(2), = 78.38(2)°, = 75.39(2), Z = 2, V = 769.5(4) ų; The compound 2 crystallizes in space group P2₁/n, with cell parameters a = 13.582(2), b = 8.974(1), c = 16.960(2) Å, = 103.34(1)° and D _calc = 1.352 g/cm^–3 for Z = 4. X-ray analysis reveals that atoms C(1)—C(5) and O form a pyran ring in compound 1, which adopts half-chair conformation. In compound 2 the atoms C(12)—C(16) and O form a pyran ring which adopts boat conformation, another six-membered ring (C(8)—C(13)) adopts a half-chair conformation. In addition, there are intermolecular hydrogen bonds in the crystal structures 1 and 2.