CRYSTAL AND MOLECULAR STRUCTURE OF BENZO-15-CROWN-5 POTASSIUM TETRACHLOROAURATE K(C_(14)H_(20)O_5)_2-AuCl_4

<正> The crystal and molecular structure of the title compound K(C14 H20O5)2AuCl4 has been determined by X-ray diffraction method.The crystallographic data are as follows;Mr=914.51,triclinic,space group P1,a=10.988(2),b=13.472(4),c=13.696(2)A,α=77.72(1),β=79.02(2),γ=64.92(2)°,V=1782.6(4)A3,Z=2,Dc=1.704 g.cm-3,μ=45.858 cm-1,F(000)=454,R=0.019,Rw=0.018 for 5697 observed reflections with I≥3σ(I).X-ray structure determination shows that benzo-15-crown-5(B15C5)forms a 2:1 complex with KAu-C14 in which K+is sandwiched between two crown rings.The dihedral angle between these two ether oxygen planes is 11.9°.The anion AuCl4-has a planar square configuration which is bound with the complex cation K(B15C5)2+by electrostatic force to form an ion-pair.     

Crystal Structure of 3-methyl-1, 2, 3, 4, 4a, 4b, 9a, 15, 15a,15b-decahydro-(4,5);(4a,15)-dimethano-tricyclo(4, 3, 1, 0~(2,7)) deca 〔8, 9, 1, 10-a,b, c〕pyrido〔4,3-a〕-acridin-6-en-9-ol-8-one

1INTRODUCTIONIntheO-demethyIationof7a-o-amino-phenyl-6,14-endo-ethenotetrahydrothe-baine,catalyzedbyhydrobromicacid,ifinhightemperatureandprolongedtime,anewcomPoundwithyie1dof17.9%wasfound,whosestructurecannotbedeferredfromthepreviousacid-catalyzedrearrangementof6,14-endo-ethnotetrahydrothe-baines(1-33.ItwascrystallizedfromanhydrousethanolsolutionanditsstructurewasdeterminedbyX-raycrystallography.2EXPERmENTALAcrystalwithdimensionsofO.3mmXO.4mmXO.5mmwasmountedonanEnraf-NoniusCAD4d…     

Synthesis and Crystal Structure of 13-Phenyl-1,10- dithia-4,7-dioxa-13-aza-15-Crown-5

1　ＩＮＴＲＯＤＵＣＴＩＯＮＣｒｏｗｎａｎｄａｚａｃｒｏｗｎｅｔｈｅｒｈａｖｅｂｅｅｎｕｓｅｄｗｉｄｅｌｙａｓｈｏｓｔｓｆｏｒｒｅｃｏｇｎｉｚｉｎｇｇｕｅｓｔｍｅｔａｌｉｏｎｓ.[1～ 4] Ｔｈｉａｃｒｏｗｎｅｔｈｅｒｓｉｎｃｏｒｐｏｒａｔｉｎｇｏｎｌｙｓｕｌｆｕｒａｔｏｍｓｉｎｒｉｎｇａｌｓｏｈａｖｅｂｅｅｎｓｔｕｄｉｅｄａｓｅｘｔｒａｃｔｉｎｇｒｅａｇｅｎｔｓｆｏｒｓｏｍｅｓｏｆｔｍｅｔａｌｉｏｎｓ.[5] Ｏｎ ｌｙｆｅｗｓｔｕｄｉｅｓｏｎｍｉｘｅｄ ｄｏｎｏｒｃｒｏｗｎｅｔｈｅｒｃｏｎｔａｉｎ ｉｎｇ…     

Crystal Structure of 3, 4-trans-4, 5-trans-2-Amino-3-cyano-1, 3-diethyloxy carbonyl- 4, 5-di (4-chlorophenyl)cyclopentene

1INTRoDUCT1oNThechemistriesofsamariumdiiodideandlow-valenttitaniumareofcurrentin--.terestinorganicSynthesis.Theyhavebeenwidelyusedinsyntheticreactions(l.2i.Thereactivityofthereagentstowardsvariousnitrogen-containingcomPOundshasal-readybeenexamined.Thereare,toourknowledge,noliteratureexamplesforthereductionofafylidenecyanoacetatederivativeswiththesereagents.Recently,wefoundthatthetitlecompoundisobtainedbycyclodimerizationreactionofpchlorObenzylidenecyanoacetatewithsamariumdiiodideorlow-va…     

Crystal Structure of 4, 5-trans-2-Amino-1, 3, 3-tricyano-4, 5-di (4-chlorophenyl)cyclopentene. Ethanol. Monohydrate

1mTRODUCT10NSincethetimeKaganhasdem0nstratedasimplepreparationofsamariumdiio-didefromsamariummetaland1,2-diiodoethanet1),SmI2hasbeenwidelyusedinsyntheticreactionst23.Thereactivityofsamariumdiiodidetowardsvariousnitrogen-containingcomP0undshasalreadybeenexamined.Thereare,toourknowledge,noliteratureexamplesforthereductionofcyanogrouptoproduceaminowiththisreagent.Inthispaper,wediscussedthecrystalstructureofthetitlecomP0undsyn-thesizedbythereactionofsamariumdii0didereagentwithp-chloroben-zyli…     

Structure and properties of dinuclear manganese(III) complexes with pentaanionic pentadentate ligands including alkoxo, amido, and phenoxo donors

Doubly bridged mu-alkoxo-mu-X (X = pyrazolato or acetato) dinuclear MnIII complexes of 2-hydroxy-N-{2-hydroxy-3-[(2-hydroxybenzoyl)amino]propyl}benzamide) (H5L1) and 2-hydroxy-N-{2-hydroxy-4-[(2-hydroxybenzoyl)amino]butyl}benzamide (H5L2), [Mn2(L)(pz)(MeOH)4].xMeOH (1, L = L1, x = 0.5; 2, L = L2, x = 0; Hpz = pyrazole) and [Mn2(L1)(OAc)(MeOH)4] (3), have been prepared, and their structure and magnetic properties have been studied. The X-ray diffraction analysis of 1 (C24.5H34Mn2N4O9.5, triclinic, P, a = 12.2050(7) A, b = 12.7360(8) A, c = 19.2780(10) A, alpha = 99.735(5) degrees , beta = 96.003(4) degrees , gamma = 101.221(5) degrees , V = 2867.6(3) A3, Z = 4), 2 (C25H34Mn2N4O9, triclinic, P, a = 9.4560(5) A, b = 11.0112(5) A, c = 13.8831(6) A, alpha = 90.821(4) degrees , beta = 92.597(4) degrees , gamma = 93.403(4) degrees , V = 1441.29(12) A3, Z = 2), and 3 (C23H32Mn2N2O11, triclinic, P, a = 10.511(5) A, b = 11.713(5) A, c = 13.135(5) A, alpha = 64.401(5) degrees , beta = 74.000(5) degrees , gamma = 66.774(5) degrees , V = 1329.3(10) A3, Z = 2) revealed that all complexes consist of dinuclear units which are further extended into 1D (1 and 3) and 2D (2) supramolecular networks via hydrogen-bonding interactions. Magnetic susceptibility data evidence antiferromagnetic interactions for all three complexes: J = -3.6 cm-1, D approximately 0 cm-1, g = 1.93 (1); J = -2.7 cm-1, D = 0.8 cm-1, g = 1.93 (2); J = -4.9 cm-1, D = 3.8 cm-1, g = 1.95 (3).     

The Crystal Structure of 1, 4, 7, 10- Tetraazacyclododecane Hydrate Triperchlorate

1=mTRODUCTIONMacroazacyclicligandisofwideinterestbecauseofitsstructuralsimilaritywiththeskeletonofPOrphyrinringinsomebibectivesubstancessuchaschlorophyllandhemeetc.tl1.Asametalsimulationenzyme,macroazacyclicligandcoordinatedwithtransitionmetalhasbeeninvestigatedthoroghlyinkinetic,dynamicandstructuralcharactert2.3).Butthere'isnorePOrtaboutthecrystalstructureof1,4,7,1o-tetraaza-cyclododecanehydratetriperchlorate.2EXPERIMENTAL2-lSynthesisoftheTitleComplexTetraazacycldodecanewassynthes…     

CRYSTAL STRUCTURE OF BENZO-15-CROWN-5-POTASSIUM TETRAIODOINDATE(Ⅲ)

<正> K(C14H2oO5)2InI4, Mr =1198.16, triclinic,P1,a=ll.839(3), b=12.993(4), c= 14.774(6)A,α=107.87(3),β=109.25(3),γ=95.08(2)°,V=1996.1A3, Z=2, Dc=1.993g.cm-3, MoKa radiation, =0.71073A, F(000)=1136e, R=0.049 for 4381 observable reflections. The structure consists of complex cation K(B15C5)2+ and complex anion InI4-. In the cation, potassium ion lies between two ether oxygen planes of two benzo-15-crown-5 molecules. In the an-ion, indium atom is tetrahedrally coordinated by four iodine atoms.     

7,7-二甲基-2-对溴苯基-4-苯基-5-氧代-1,4,5,6,7,8-六氢化-6H-喹啉的合成及晶体结构

标题化合物C23H22BrNO是由1-(4-溴苯基)-3-苯基-2-丙烯-1-酮与5,5-二甲基-1, 3-环己二酮在N, N-二甲基甲酰胺(DMF)中在NH4OAc催化下反应而得。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C2/C, a = 19.678(4),b = 13.571(2),c = 17.311(3) 牛琤 = 118.74(1),Mr = 408.33, V = 4055(1) ?,Dc = 1.338 g/cm3, Z = 8, m (MoKa) = 2.038 mm-1, F(000) = 1680, R = 0.0539,wR = 0.1369。X-衍射分析表明,六元环C(10)C(13)C(16)C(17)采用半椅式构象:原子C(10),C(11),C(12),C(16)和C(17)在同一个平面内,而原子C(13)远离平面为0.3282 牛闷矫嬗?个苯环的夹角分别为41.09, 81.97,2个苯环的夹角为75.87。另外在晶体结构中,存在1个分子间氢键。     

2,11,14-三氮-5,8-二氧-3,4,9,10-双(4,4'-三氟甲苯并)-13,15-(2’,6’)吡啶环十五-1,12-二烯酮的合成和晶体结构

合成并测定了2，11，14-三氯-5，8-二氧-3，4，9，10－双（4，4’-三氟甲苯并）-13，15－（2’，6’）吡啶环十五-1，12-二烯酮的单晶结构。晶体分子式C23H15F6N3O4，Mr=511．38，晶体属单斜晶系，空间群P21/c，晶胞参数a=6.732（2），b=15.751（4），c=20．420（8）A，β=96．54（3）°，V=2151．6A3，Z=4，Dc=1．579g／cm3，μ（MOKO）=1．360cm－1，F（000）=1040。分子含有A、B、C、D四个环，D、C苯环对称连有2个三氟甲基，中间A环为含氧、氮的十五员王冠大杂环，整个分子为近平面结构。     

Na_3Fe（C_2O_4）_3·5H_2O的合成、晶体结构及谱学表征

合成并测定三价铁乙二酸配合物Ｎａ_３Ｆｅ（Ｃ_２Ｏ_４）_３．５Ｈ_２Ｏ的单晶结构。晶体属单斜晶系，空间群为Ｃ２／ｃ，晶胞参数ａ＝１７．３８０（１），ｂ＝１２．６９３（５），ｃ＝１５．１９６（６），β＝１００．４７（６）°，Ｖ＝３２９７（３），Ｚ＝８，Ｄ_ｃ＝１．７４ｇ／ｃｍ￣（－３）．Ｍ_ｒ＝４７８．９８，μ＝１０．５１ｃｍ￣（－１）。结构的偏离因子Ｒ＝０．０３６，Ｒ_ｗ＝０．０５６。此外，还测定了化合物的红外、拉曼、紫外一可见吸收光谱、穆斯堡尔谱及磁化率等。并通这有关信息讨论了该化合物的结构。     

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2的晶体和分子结构

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2(分子量900.8)晶体属单斜晶系,空间群P21/n,晶胞参数a=21.319(2),b=20.844(2),c=10.130(3),β=91.255(2)°,V=4500.4,Z=4,D_c=1.15g·cm~(-3),F(000)=1864,μ(CuKα)=44.97cm~(-1)。共收集独立衍射点数7636个,其I>3σ(1)的衍射点数6810个。最终的R=0.045,R_w=0.050(W=1/σ~2(F)+(F)+g|F|~2)。其分子结构呈畸变的三角双锥构型。     

THE CRYSTAL STRUCTURE AND SECOND-HARMONIC EFFECT OF COMPOUND C_9H_9N_3O_6· C_5H_5N

<正> The title compound (PAP) with excellent nonlinear optical prpper-ties has been synthesized. CHCHSCOO , monoclinic with space group P21, a = 4. 521(1), b = 9.601(6), c=17. 892(2)(?) , β=96. 12(1)°, V =772.8(?)3, Z = 2, Dc=1.44g · cm-3, F(000)-348, μ= 1.24cm-1. The second-harmonic intensities of PAP, MAP and NaAP HAP were measured,with the values which are 100, 50, 5. 0 times as large as that of KDP, respectively, Indicating that PAP is a new NLO crystal.     

Crystal Structure of 3, 7-Dihydroxy1-1, 5-diazacyclooctane Dihydrobromide C_6H_(14)N_2O_2. 2HBr. EtOH

1I7NTRODUCT1ONAsequenceofnovelhydroxylmesocyclicdiaminesLl-3Jweresynthesizedinourlaboratoryandemployedtobindtransitionmetalions.Wehavepreviouslyreported[']thatoneofthesemesocycles,3-hydroxyL1,5-diazacycloheptane,adoptstranschair-chairconformationinthecomplexes,whereasitlookslikeacrownintheabsenceofguests.Here,wereportthemolecularstructureofthetitlemesocyclicdiaminewhichbearsdoublehydroxylgroups.2EXPERIMENTALThetitlecompound['Jwasheatedtobedissolvedinalittlewater,followedbyad-ditiono…     

Synthesis, structural characterization, and Monte Carlo simulation of the magnetic properties of two new alternating MnII azide 2-D honeycombs. Study of the ferromagnetic ordered phase below 20 K

Reaction of MnII and pyridine derivatives such as 4-methylpyridine (4-Mepy) and 4-ethylpyridine (4-Etpy) led to the new two-dimensional systems trans-[Mn(4-Mepy)2(N3)2]n (1) and trans-[Mn(4-Etpy)2(N3)2]n (2). Compound 1 crystallizes in the triclinic system, P1 group (a = 9.269(2) A, b = 9.635(3) A, c = 18.860(4) A, Z = 4), and compound 2 crystallizes in the monoclinic system, P2(1)/c group (a = 14.416(3) A, b = 8.515(2) A, c = 15.728(4) A, Z = 4). The two compounds show honeycomb structures based on dinuclear Mn-(mu-N3)2-Mn subunits linked to the four nearest-neighbor similar subunits by four end-to-end single azido bridges, but whereas the subunits of compound 1 show the end-to-end Mn-(mu 1,3-N3)2-Mn kind of bridges, compound 2 prefers the end-on Mn-(mu 1,1-N3)2-Mn fragment. Magnetically, compound 1 is an alternating 2-D system with two different antiferromagnetic interactions, whereas compound 2 corresponds to a two-dimensional ferro-antiferromagnetic system showing spin canting and permanent magnetization below 20 K. The coupling constant parameters J1 = -10.1 cm-1, J2 = -4.7 cm-1, and g = 2.019 for 1 and J1 = -5.3 cm-1, J2 = 2.9 cm-1, and g = 2.016 for 2 have been obtained from calculations using the Monte Carlo method based on the Metropolis algorithm.     

STRUCTURE OF 5-(N-METHYL-β-NAPHTHYLAMINO)-PENTA-2,4-DIENAL,C_(16)H_(15)NO

<正> M=237.31, orthorhombic, Pbca, a=8.342(2), b=15.675(3), c=19.779 (4)A3, Z=8, Dx=1.21 g/cm3, λ(MoKα)=0.71069A, μ=0.71 cm-1, F(000)=1008, room temperture, R=0.046. The planes of the formyl butadienyl group and the naph-thyl ring are tilted with respect to the plane of the nitrogen frame N by 2.8° and 31.4° , respectively. The O atom and the methyl group are in Z position.     

Synthesis and Crystal Structure of a Molybdenum Carbonyl Compound with Thiolate and Dithiocarbamate Ligands,[Bu4N][(OC)4Mo(μ-SC6H5)2Mo(C5H10CNS2)(CO)2]

A di-molybdenum carbonyl compound containing thiolate and dithiocarbamate li- gands, [Bu4N][(CO)4Mo(μ-SC6H5)2Mo(C5H10dtc)(CO)2] 1 (C5H10dtc = S2CNC5H10), has been pre- pared by reaction of [Mo2(SC6H5)2(CO)8] with C5H10dtcNa and [NBu4]Br in acetone. It crystallizes in monoclinic, space group P21/n with a = 13.162(3), b = 17.466(2), c = 20.453(4)(A),β = 100.77(1)°, Z = 4, V = 4619(2)(A)3, C40H56Mo2N2O6S4, Mr = 980.95, Dc = 1.389 g/cm3, μ= 7.66 cm-1, F(000) = 1988 and R = 0.0746 for 5161 observed reflections with I > 2σ(I). The complex contains a [Mo2S2]2- planar core in which one Mo atom is chelated by a C5H10dtc ligand, leading to different coordination environments of the two Mo atoms. 95Mo NMR measurement indicates that the two Mo atoms are in different oxidation states.     

Crystal Structure and Molecular Structure of Binuclear Copper（Ⅱ）Complex，［Cu（C_5H_5NO）（C_6H_5COO）_2］_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＢｉｎｕｃｌｅａｒＣｏｐｐｅｒ（Ⅱ）Ｃｏｍｐｌｅｘ，［Ｃｕ（Ｃ_５Ｈ_５ＮＯ）（Ｃ_６Ｈ_５ＣＯＯ）_２］_２￥ＹａｎｇＲｕｉ－Ｎａ；ＨｏｕＹｉ－Ｍｉｎ；ＸｕｅＢａｏ－Ｙｕ；Ｊｉ...     

Synthesis and Crystal Structure of (CO)5ReSnMe2Re(CO)5

１ＩＮＴＲＯＤＵＣＴＩＯＮＨｏｍｏ ｄｉｎｕｃｌｅａｒｍｅｔａｌｃａｒｂｏｎｙｌｃｌｕｓｔｅｒｓｈａｖｅｂｅｎｓｔｕｄｉｅｄｗｉｄｅｌｙｆｏｒｔｈｅｉｒｎｏｖｅｌｓｔｒｕｃｔｕｒｅｓａｎｄｕｓｅｓｉｎｏｒｇａｎｉｃｓｙｎｔｈｅｓｉｓ〔１〕．Ｅｘａｍｐ...     

CRYSTAL AND MOLECULAR STRUCTURE OF { CNa(15-crown-5)]_n [Cd(SCN)_3]}_n

<正> The complex [Na(15-crown-5)] [Cd(SCN)3] (15-crown-5 = C10H20 O5) crysializes in monoclinic space group P21/c with a=10. 219(2) ,b= 10. 575(2) ,c= 20. 572(2) A ,β=98. 45(1)°,V= 2198. 7A3,Mr=529. 89,Z = 4,Dx=1. 600g/cm3,F (000) -1052,μ= 15. 708cm-1. The structure was solved by direct methods with the final R=0. 064. Results of structure analysis indicate that the Na ion is bonded by 15-crown-5 to form a complex cation and the Cd(Ⅱ) is bonded by six SCN ion to form an anion chain with a distorted octahedral coordination.