Crystal Structure and Molecular Absolute Configuration of （＋）－Isocedranol （C_（15）H_（26）O）

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＭｏｌｅｃｕｌａｒＡｂｓｏｌｕｔｅＣｏｎｆｉｇｕｒａｔｉｏｎｏｆ（＋）－Ｉｓｏｃｅｄｒａｎｏｌ（Ｃ_（１５）Ｈ_（２６）Ｏ）￥ＬｉｕＪｉｅ；ＣｈｅｎＭｉｎ－Ｑｉｎ（ＣｅｎｔｅｒｏｆＡｎａｌｙｓｉｓ＆Ｍｅａｓｕｒｅｍ...     

Structure of Copper（Ⅱ）Bis（piperidyldithiocarbamate）

ＳｔｒｕｃｔｕｒｅｏｆＣｏｐｐｅｒ（Ⅱ）Ｂｉｓ（ｐｉｐｅｒｉｄｙｌｄｉｔｈｉｏｃａｒｂａｍａｔｅ）ＬａｎｇＪｉａｎ－ｐｉｎｇ；ＬｕＪｉａｎ－Ｍｅｉ；ＢｉａｎＧｕｏ－Ｑｉｎｇ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＳｕｚｈｏｕＵｎｉｖｅｒｓｉｔｙ...     

Crystal and Molecular Structure of Di－chloro－bis（р－methylphenylbutylsulfide） Palladium（Ⅱ）

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＤｉ－ｃｈｌｏｒｏ－ｂｉｓ（р－ｍｅｔｈｙｌｐｈｅｎｙｌｂｕｔｙｌｓｕｌｆｉｄｅ）Ｐａｌｌａｄｉｕｍ（Ⅱ）￥ＧｕｏＳｏｎｇ－Ｓｈａｎ；ＣｕｉＬｉ；ＷａｎｇＨａｎｇ－Ｚｈａｎｇ；ＱｉａｎＰｕ（...     

Preparation and Crystal Structure of Bis（2－thenoyltrifluoroacetone）Copper（Ⅱ）

ＰｒｅｐａｒａｔｉｏｎａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（２－ｔｈｅｎｏｙｌｔｒｉｆｌｕｏｒｏａｃｅｔｏｎｅ）Ｃｏｐｐｅｒ（Ⅱ）ＷａｎｇＤｏｎｇ－Ｍｅｉ；ＹａｎｇＲｕｉ－Ｎａ；ＨｕＹｉ－Ｍｉｎ；ＪｉｎＤｏｕ－Ｍａｎ（ＨｅｎａｎＩｎｓｔｉ...     

Crystal Structure and Spectrum Properties of a Manganese Complex with Schiff Base Ligand，Mn（bzacen）（pyrimidine）（NCS）

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＳｐｅｃｔｒｕｍＰｒｏｐｅｒｔｉｅｓｏｆａＭａｎｇａｎｅｓｅＣｏｍｐｌｅｘｗｉｔｈＳｃｈｉｆｆＢａｓｅＬｉｇａｎｄ，Ｍｎ（ｂｚａｃｅｎ）（ｐｙｒｉｍｉｄｉｎｅ）（ＮＣＳ）￥ＦｅｎｇＹｕｎ－Ｌｏｎｇ；ＬｉｕＳｈｉ－...     

Spectral Analysis and Crystal Structure of Tris（benzoyl－trifluoroacetonate）bis（triphenyl－phosphine oxide）Europium（Ⅲ）

ＳｐｅｃｔｒａｌＡｎａｌｙｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＴｒｉｓ（ｂｅｎｚｏｙｌ－ｔｒｉｆｌｕｏｒｏａｃｅｔｏｎａｔｅ）ｂｉｓ（ｔｒｉｐｈｅｎｙｌ－ｐｈｏｓｐｈｉｎｅｏｘｉｄｅ）Ｅｕｒｏｐｉｕｍ（Ⅲ）ＬｅｉＨｅｎｇ－Ｙｉ；ＹａｎｇＹ...     

Crystal Structure of Ethyl Ester N－（Isopropylcarbamoyl－Methoxyphosphonyl）－（1）－α－Phenylalanine

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＥｔｈｙｌＥｓｔｅｒＮ－（Ｉｓｏｐｒｏｐｙｌｃａｒｂａｍｏｙｌ－Ｍｅｔｈｏｘｙｐｈｏｓｐｈｏｎｙｌ）－（１）－α－ＰｈｅｎｙｌａｌａｎｉｎｅＣｈｅｎＲｕ－Ｙｕ；ＬｉＨｕｉ－Ｙｉｎｇ（ＩｎｓｔｉｔｕｔｅｏｆＥｌｅｍｅ...     

Synthesis and Crystal Structure of （Et4N）2[Pd2（mp）2（mpH）2]

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（Ｅｔ_４Ｎ）_２［Ｐｄ_２（ｍｐ）_２（ｍｐＨ）_２］ＳｈｉＪｉ－Ｃｈｅｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ；ＷｅｎＴｉｎｇ－Ｂｉｎ；ＤｅｎｇＹｕ－Ｈｅｎｇ；ＣｈｅｎｇＣｈａｎｇ－Ｎｅｎｇ；Ｌｉ?..     

THE REACTION OF（μ_3－CPh）Co_3（CO）_9 WITH TRANSITION METAL CARBONYL ANION M（CO）_3（RCOCp）AND CHARACTERIZATION OF CLUSTERS（μ_3－CPh）CO_2M（CO）_8（RCOCPp）（M＝Mo，W；R＝H，CH_3．C_2H_5O）

ＴＨＥＲＥＡＣＴＩＯＮＯＦ（μ_３－ＣＰｈ）Ｃｏ_３（ＣＯ）_９ＷＩＴＨ　ＴＲＡＮＳＩＴＩＯＮＭＥＴＡＬＣＡＲＢＯＮＹＬＡＮＩＯＮＭ（ＣＯ）_３（ＲＣＯＣｐ）ＡＮＤＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦＣＬＵＳＴＥＲＳ（μ_３－ＣＰｈ）ＣＯ_２Ｍ（ＣＯ）_８（ＲＣＯＣＰｐ）（Ｍ＝Ｍｏ，Ｗ；Ｒ＝Ｈ，ＣＨ_３．Ｃ_２Ｈ_５Ｏ）Ａｕｔｈｏｒｔｏｗｈｏｍｃｏｒｍｓｐｏｎｄｅｎｃｅｓｈｏｕｌｄａｄｄｒｅｓｓｅｄ．ＥｘｐｅｒｉｍｅｎｔａｌｓｅｃｔｉｏｎＧｅｎｅｒａｌｐｒｏｃｅｄｕｒｅａｎｄｍａｔｅｒｉａｌＡｌｌｏｐｅｒａｔｉｏｎｗａｓｃａｒｒｉｅｄｏｕｔｕｎｄｅｒｈｉｇｈｌｙｐｕｒｅｎｉｔｒｏｇｅｎａｔｍｏｓｐｈｅｒｅｕｓｉｎｇｓｈａｄａｒｄＳｃｈｌｅｎｌｃａｎｄｖａｃｕｕｍｔｅｃｈｎｉｑｕｅｓ．Ｈｅ－ｃａｎｅ，ｂｅｎｚｅｎｅａｎｄｔｅｔｒａｈｙｄｒｏｆｕｒａｎｗｅｒｅｐｒｅｄｒｉｅｄｏｖｅｒｓｏｄｉｕｍｗｉｒｅａｎｄｄｉｓｔｉｌｌｅｄｆｒｏｍｓｏｄｉｕｍ－ｂｅｎｚｏｐｈｅｎｏｎｅｕｎｄｅｒｎｉｔｒｏｇｅｎ．ＮａＭ（ＣＯ）３（ＲＣＯＣＰ）ａｎｄＰｈＣＣｏ３（ＣＯ），ｗｅｒｅｐｒｅｐａｒｅｄａｃｃｏｒｄｉｎｇｔｏｌｉｔｅｒａｔＵｒｅ     

Crystal Structure of Co（S2CPh）3

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣｏ（Ｓ_２ＣＰｈ）_３ＬｕＳｈａｏ－Ｆａｎｇ；ＣｈｅｎＨｏｎｇ－Ｂｉｎ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＦｕｊｉａｎＩｎｓｔｉｔｕｔｅｏｆＲｅｓｅａｒｃｈｏｎｔｈｅＳｔｒｕｃｔｕｒｅｏｆＭａｔｔｅｒ，Ａｃａｄｅｍｉａ...     

CRYSTAL STRUCTURES OF TWO DITHIOLATO-COPPER COMPLEXES (Ph_4P)Cu(BDT)_2 AND (Ph_4P)Cu(TDT)_2

<正> [(C6H5)4P]Cu(S2C6H4)2(Ⅰ),Mr = 683. 39,monoclinic,space group C2/c,a=16. 099 (4),b= 11. 913(3) ,c = 16: 715(9) A ,β=97. 13(4)°, v = 3180. 7 A3,z=4.MoKa radiation,λ= 0. 71069A ,Dc= 1. 427g/cm3,μ= 10. 1cm-1,F(000) = 1400,R=0. 061 and Rw = 0. 068 for 2189 reflections with Ⅰ>3σ(Ⅰ). [(C6H5)4P]Cu (S2C7H6)2(Ⅰ),Mr = 711. 45,monoclinic,space group C2/c,a=16. 501(6),b = 37. 461 (15),c=16. 684(4)A,β=96. 70(4)°, v= 10248. 8(46) A3,z= 12. MoKa radiation, λ= 0. 71069A,Dc=1.383g/cm3,μ=9. 45cm-1,F(000).= 4416,R= 0. 074 and Rw= 0. 078 for 2085 reflections with I>2σ(I)(1). The copper atom in the complexes is surrounded by four sulfur atoms from two dithiolato ligands in an approximate, square-plane. The average Cu-S distances of the copmplexes(Ⅰ) and (Ⅱ) are 2. 179 and 2. 178 A, respectively.     

Structure of a Discrete 8:6 La(Iii): P-Sulfonatocalix[4]Arene Complex

Abstract

The crystal structure of a complex formed between La(III) and p-sulfonatocalix[4]arene is reported. The complex cristallizes in the monoclinic space group P2₁/n, a = 15.091(1), b = 28.550(3), c = 30.167(3) Å, β = 90.008(2)°, V = 12997(2) ų, ρ_calc. (g cm^?3) = 1.792, Z = 2. Refinement led to R₁ value of 0.0961 for 13930 unique reflections. It forms discrete units with 8 La(III) cations coordinated by 6 calixarene ligands. The calixarenes are organized in an up-down configuration, bridged by La(III), forming layers of 3 repeating calixarene units and channels along the a axis. The units are linked by hydrogen-bonds.     

Crystal Structure of a Uranyl/p-tert-Butylcalix[5]arene Complex

The synthesis and crystal structure of the inclusion complex between uranyl and p-tert-butylcalix[5]arene are reported. [UO2 (p-tert-butylcalix[5]arene-4H]2- · &·2MeOH(1) crystallizes in the monoclinic space group C2/c, a = 30.06(2), b = 18.20(3), c = 31.35(2) Å, = 128.51(6)°, V = 13423(40) Å3, Z = 8. Refinement led to a final conventional R value of 0.043 for 4155 reflections. The uranyl ion is bonded, in its equatorial plane, to the five oxygen atoms of the calixarene, four of which are deprotonated. A protonated triethylamine molecule is located inside the calixarene cavity and hydrogen bonded to a uranyl oxygen atom, and another one outside and hydrogen bonded to a calixarene oxygen atom. The calixarene conformation is the usual cone one.     

Extraannular fluorinated calixarenes: regiospecificity of the deoxofluorination reactions of bis(spirodienol) derivatives

A new route for the partial displacement of OH groups of p-tert-butylcalixarene via spirodienol derivatives is described. NaBH(4) reduction of the bis(spirodienone) calixarene derivatives 2a-2c afforded the corresponding bis(spirodienols) 3a-3c in stereospecific fashion. (1)H NMR NOESY spectroscopy indicated that in the case of 2a, the reaction proceeds by attack at the exo face of the two carbonyls (the face located anti to the spiro C-O bond). The spirodienols readily revert to p-tert-butylcalix[4]arene when heated. The reaction of 3a with the deoxofluorinating agent DAST (Et(2)NSF(3)) afforded a mixture of extraannular substituted calixarenes possessing one or two fluoro-substituted dehydroxylated rings. The bisfluorinated calixarene 6a adopts in the crystal a conformation (1,3-alternate) similar to that adopted in solution by the di-dehydroxylated calixarene 6b. An experiment conducted with a selectively deuterated spirodienol derivative indicated that the deoxofluorination reaction involves regiospecific nucleophilic attack at the gamma position of the pentadienol subunit.     

混合三烃基锡有机酸酯化合物构效关系 （Ⅰ）二环己基－甲基－2，4－二溴－β－甲基苯氧乙酸锡酯 及二环己基－甲基－2－甲氧基－4－丙烯基苯氧乙酸锡酯的晶体结构和分子结构

报道２，４－Ｂｒ２Ｃ６Ｈ３ＯＣＨ（ＣＮ３）ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＵ３（１）和２－ＯＣＨ３－４－ＣＨ３ＣＨ＝ＣＨＣ６Ｈ３ＯＣＨ２ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＨ３（Ｈ２Ｏ）（Ⅱ）的晶体结构和分子结构。（Ⅰ）单斜晶系，空间群Ｐ２１／ｃ，ａ＝１３．０６７（３），ｂ＝１０．５９４（３），ｃ＝１８．１５７（４），β＝１０６．９９（２）°，Ｚ＝４，Ｄｃ＝１．６７２ｇ／ｃｍ３，Ｖ＝２４０３．７３，μ＝４３．７３１ｃｍ－１，Ｍｒ＝６２２．９９，Ｆ（０００）＝１２３２；（Ⅱ）单斜晶系，空间群Ｐ２１／ｎ，ａ＝１０．４０９（１），ｂ＝　１２．５７０（２），ｃ＝２０．６６４（２），β＝８３．５１（１）°，Ｚ＝４，Ｄｃ＝１．２８１ｇ／ｃｍ３，Ｖ＝２６８６．４Ａ３，μ＝９．７６１ｃｍ－１，Ｍｒ＝５３９．２８，Ｆ（０００）＝１１２０．最后的偏离因子，化合物（Ⅰ）Ｒ＝０．０４６，Ｒω＝０．０４６；化合物（Ⅱ）Ｒ＝０．０４９，Ｒω＝０．０４７。晶体结构解析表明，化合物（Ⅰ）和（Ⅱ）中的锡均被配体的３个碳和２个氧原子配位，配位原子呈畸变三角双锥构型；化合物中的环己基均为椅式构象；化合物（Ⅱ）中，配位水分子和另一分子的羰基氧与芳环上的甲基氧?     

Syntheses,Crystal Structures and IR Spectra of Two Mixed Metal Complexes:〔Cr_nFe_(3-n)(μ_3-O)-(μ-O_2CC_2H_5)_6 Py_3〕Cl(n=1,2)

1INTR0DUCTI0NTrinuclearoxo-carboxylatocomplexescontainingmixedmetalionshavebeenofintenseinterestsincethefirststructuredeterminedbyX-raydiffractioninl965t1i,Theimportanceofthesecompoundsshowsinservingasmodelstotesttheoriesforthepotentialmagneticcoupllngbetweenmetalionsinmultinuclearsystem,asempha-sizedbyCANNONDetal.t2i.However,inrecentyears,wehavefoundthatthiskindofcompoundsmayactasaprecursorofthecatalystfortheadditi0nreactionofacetylenewitheitherH,O0rH,,andf0rtheketonizationofacidbydec…     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

Synthesis and Crystal Structure of an Ionic Compound [Fe(CN)_6(phCH_2NC_5H_5)3]·(H_2O)_4

A novel ionic compound [Fe(CN)6(phCH2NC5H5)3]·(H2O)4(Mr = 794.71) has been synthesized and its structure was characterized by IR, elemental analysis and X-ray diffraction. The compound crystallizes in monoclinic, space group P21/c with a = 10.837(2), b = 16.551(3), c = 23.402(5) , β = 97.531(4)o, V = 4161.0(15) A3, Z = 4, Dc = 1.269 g/cm3, F(000) = 1668, μ = 0.414 mm-1, R = 0.0479 and wR = 0.1232. The building unit of the title compound consists of three (phCH2N+C5H5) ions, one [Fe(CN)6]3- anion and four water molecules. According to the structural analysis, [Fe(CN)6]3- are linked together by O–H···N and O–H···O hydrogen bonds, but [Fe(CN)6]3- and [(phCH2N+C5H5)3] ions are bound by electrostatic force to form an ionic compound.     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

Crystal Structure of Tris（m—nitrobenzoato）Samarium Dihydrate

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＴｒｉｓ（ｍ－ｎｉｔｒｏｂｅｎｚｏａｔｏ）ＳａｍａｒｉｕｍＤｉｈｙｄｒａｔｅＭａＪｉａｎ－Ｆａｎｇ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ；ＮｉＪｉａ－Ｚｕａｎ（ＬａｂｏｒａｔｏｒｙｏｆＲａｒｅＥａｒｔｈＣｈｅｍｉｓｔｒｙａ...