一种新的生物分离方法——混合模式吸附层析

混合模式吸附层析是一种新型的生物分离方法,其功能配基兼有两种或两种以上的作用模式,主要为静电和疏水相互作用。在低盐和高盐条件下,都可以实现对目标物的有效吸附,具有明显的耐盐吸附的特性,可避免对料液的额外预处理,从而提高分离效率,减少分离成本,已获得一定的应用。本文对混合模式吸附技术的发展历程、类型及应用现状等进行综述,以推动该技术的发展和进一步应用。

Integrated Assembly Structure Design Within Concurrent Engineering

Taking a microwave product as an example, a system of integrated assembly structure design is presented. Getting design constraints from the upstream design section through product data management(PDM), the system generates the assembly scheme using the case? based method, then assigns the design requirements into each component of the assembly. The detail design for each component can be performed under these design constraints. In order to practise concurrent design, the system sends the final design result to the upstream section and downstream section through PDM to achieve information sharing and integration.

Synthesis and Structure of bis(μ-2-aminopyridine N-oxide)-bis[dichlorocopper(II)]

The complex [Cu2（apo）4Cl4]·2H2O （apo=2-aminopyridine N-oxide） was obtained. A single- crystal X-ray study shows that the complex is a binuclear compound （Cu2C20H28Cl4N8O6）. The coordination geometry about each copper atom is best described as a distorted square pyramid. The compound [Cu2（apo）4Cl4]·2H2O belongs to the triclinic system with space group P, lattice constants: a = 7.8550（7）, b = 8.5378（7）, c = 12.082（1） ?, α = 72.807（1）, β = 77.641（1）, γ = 70.800（1）(, V =724.85（11） ?3, Z=1, Mr =745.38, Dc=1.708 g/cm3, μ =1.886mm-1, F（000） =378, R=0.0359, wR2=0.0884 for 2220 reflections with I >2σ（I）. The distances between Cu（II） and O atoms are in the range from 1.934（2） to 2.042（2）?. The distance between two copper atoms Cu-Cu（A） is 3.2978（8） ?. The distances of Cu-Cl（1） and Cu-Cl（2） are 2.2322（9）, 2.5095（10） ?, respectively. There is no evident hydrogen bond between N and Cl.

Synthesis and Structure of the Manganese Complexwith 2-Aminopyridine N-oxide

The complex Mn(apo)6Cl2 (apo=2-aminopyridine N-oxide) was obtained by the reaction of MnCl2(4H2O with apo(HCl and NaOH in ethanol. A single-crystal X-ray study shows that the complex is mononuclear with octahedral coordination environment (MnC30H36N12O6Cl2). The oxygen atoms from apo ligands coordinate to the manganese atom forming Mn(apo)6Cl2. The compound Mn(apo)6Cl2 is hexagonally symmetric with space group R3, lattice constants: a = 12.010(2), b = 12.010(2), c = 20.232(4) ?, ( = 120(, V= 2527.4(7) ?3, Z=3, Mr =786.55, Dc=1.550 g/cm3, (= 0.614mm-1, F(000) = 1221, R = 0.0541, Rw = 0.0580 for 1229 reflections with I>2((I). The distances between Mn(II) and O atoms are in the range from 2.171(5) to 2.184(5) ?, and the distance between the chlorine anion and N atom of amido group is 3.3 ?. The dihedral angle between two adjacent pyridine ring planes is 59.19 (0.17)°.

A Pyridine-copper Inclusion Complex of a New Tripodal Ligand

A pyridine-copper inclusion complex with [Cu(py)4Cl]+ core was prepared in the presence of tripodal ligand tbst {tbst = 1,3,5-tris(2-benzimidazol)sulfanylmethyl-2,4,6-trimethyl- benzene}, and its structure has been determined. It crystallizes in triclinic, space group P with a = 9.0822(2), b = 17.6026(4), c = 18.7156(4) ? a = 93.40, b = 91.2980(1), g = 91.5560(1), V = 2984.81(1) 3, C58H63Cl2CuN11O4S3, Mr = 1208.81, Z = 2, F(000) = 1262, Dc = 1.345 g/cm3, m = 0.615 mm-1, R = 0.0713 and wR = 0.1307 for 7798 observed reflections (I > 2s(I)). X-ray analysis reveals that the uncoordinated tbst and pyridine as guest molecules are included in the complex with formula {[Cu(py)4Cl]Cl}(tbst)(py)4H2O. The tbst, pyridine, aqua and Cl- anion in the com- plex form extensive hydrogen-bonding interactions, building up a quasi-dinuclear structure.

Synthesis and Structural Characterization of a New One-dimensional Infinite Chain of Silver(I) Complex with Triphenylphosphine

The reaction of triphenylphosphine with AgNO3 yielded an unusual nitrate anion bridging one-dimensional infinite chain [Ag(PPh3)NO3] in which the silver(I) atom is three-coordinated by one P atom of triphenylphosphine and two O atoms of two bridging nitrate anions to form a scalene triangle. The complex [Ag(PPh3)NO3] crystallizes in the monoclinic system, space group P21/c with a = 10.281(2), b = 18.596(5), c = 9.180(2) , = 90.60(1), V = 1755.1(7) 3, Z = 4, Mr = 432.15, Dc = 1.635 g/cm3, F(000) = 864 and = 1.254 mm-1. The final R = 0.0606 and wR = 0.1400 for 2188 observed reflections with I > 2(I) out of 3057 unique ones (Rint = 0.0539). IR and elemental analysis of the complex are characterized.

Synthesis and Crystal Structure of Dicyanamide (5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclo- tetradecane) Copper(II) Percholatehydrate

The copper(II) complex [Cu(teta)N(CN)2](ClO4)H2O (teta = 5,7,7,12,14,14- hexamethyl-1,4,8,11-tetraazacyclotetradecane) has been synthesized and the crystal structure was determined by single-crystal X-ray diffraction. Crystal data: C18H38ClCuN7O5, monoclinic, space group P21/n, a = 8.796(3), b = 11.885(4), c = 23.054(9) , b = 97.540(4)o, V = 2389.3(15) 3, Mr = 531.54, Z = 4, Dc = 1.478 g/cm3, F(000) = 1124, ?= 1.070 mm-1, the final R = 0.0566 and wR = 0.1162 for 4749 observed reflections (I > 2s(I)). The center copper ion is coordinated by five nitrogen atoms in a square pyramidal geometry, with four from the macrocyclic ligand teta and the other one from a nitrile nitrogen atom of dicyanamide which is coordinated to the metal atoms as uni-dentate manner via nitrile nitrogen atom.

Chiral Phosphine Ligands Derived from Sugars8. Crystal and Molecular Structure of Diphenyl (methyl 4', 6'-O-benzylidene-2'-deoxy-α-D-altropyranoside-2-)phosphine Oxide

The crystal structure of the title compound, C26H27O6P, has been determined by single--crystal X-ray diffraction. The crystal is monoclinic with space groupP21, a=16. 193(l), b=5. 804(1), c=12. 512(2) A, β=93. 187(5)°, V=1174. 13A3, Dc=1. 319 g/cm3, F(000) =492, μ= 13. 52 cm-1, Z= 2, and final R= 0. 042and Rw= 0. 040 for 2349 reflections (I≥3σ(I)). Structure analysis revealed that thepyranose and 4, 6-O-benzylidene ring of the title compound adopts a distorted chair conformation.

Synthesis and Crystal Structure of (C_6N_3H_(18))_2Ti_4O_4(C_2O_4)_7·4H_2O

The title compound (C6N3H18)2Ti4O4(C2O4)74H2O 1 (C13H22N3O18Ti2, Mr = 604.14) was synthesized by the reaction of Ti(SO4)2, H2C2O42H2O and N-(2-ammonioethyl)- piperazinium (AEPP) in aqueous solution. The single-crystal X-ray analysis has revealed that 1 crystallizes in the triclinic system, space group Pi with a = 9.1437(6), b = 11.4991(10), c = 11.6975(8) ? a = 96.2915(18), ?= 107.998(3), ? = 104.276(4), V = 1110.35(14) ?, Z = 2, Dc = 1.807 g/cm3, F(000) = 618, ?= 0.815 mm-1, the final R = 0.0463 and wR = 0.1264 for 3718 observed reflections with I > 2s(I). X-ray crystal-structure analysis suggests that compound 1 consists of [Ti4O4(C2O4)7]6- anion and two protonated N-(2-ammonioethyl)piperazinium cations. The anions are linked into an infinite chain through Ti4O4(C2O4)8 by sharing the oxalates as bridging ligands.

Mononuclear Carbonyl Anion Complexes of GroupsⅣandⅤMetals

The anionic carbonyl complexes of groupsⅣandⅤmetals TM(CO)6,7(TM=Ti,Zr,Hf,V,Nb,Ta)are prepared in the gas phase using a laser vaporation-supersonic expansion ion source.The infrared spectra of TM(CO)_(6,7)-anion complexes in the carbonyl stretching frequency region are measured by mass-selected infrared photodissociation spectroscopy.The six-coordinated TM(CO)_(6)-anions are determined to be the coordination saturate complexes for both the groupⅣand groupⅤmetals.The TM(CO)_(6)-complexes of groupⅣmetals(TM=Ti,Zr,Hf)are 17-electron complexes having a~2A1gground state with D3dsymmetry,while the TM(CO)_(6)-complexes of groupⅤmetals(TM=Ⅴ,Nb,Ta)are 18-electron species with a closed-shell singlet ground state possessing Ohsymmetry.The energy decomposition analyses indicate that the metal-CO covalent bonding is dominated by TM-(d)→(CO)6π-backdonation and TM-(d)←(CO)6σ-donation interactions.

SYNTHESES OF TUNGSTEN COMPLEXES WITH o-MERCAP-TOPHENOL.CRYSTAL STRUCTURE OF (Ph_4P)[WO(OMe)(mp)_2]

Reaction of WCl6, mpH2 o-mercaptophenol) and MeONa in the presence of Ph4PBr gave complexes (Ph4P)[W(mp)3] (1) and (Ph4P) CWO(OMe) (mp)2] (2). Crystal data complex (2), C37H31O4PS2W, Mr = 818. 61, monoclinic, space group P2/a, a=26. 555(3), b=9. 634(1), c=13. 523(7) A. β=94. 68 (2)°, V=3448. 1 A3. A=1. 58 g/cm3, Z = 4. λ(MoKα)=0. 71073 A , μ= 36. 2 cm-1, F(000) = 1624, T=296K, final R(Rw) = 0. 068(0. 070) for 3929 observed reflections. The WO4S2 core is arranged in a distorted octahedral geometry.

Synthesis and Crystal Structure of (Et_4N)_2[Pd_2 (mp)_2 (mpH)_2]

Dinuclear palladium complex (Et_4N)_2[Pd_2(mp)_2 (mpH)_2 (mpH=_2-SC_6H_4OH ) (M_r = 971. 95 ) is prepared in a reaction of sodium 2-mercaptophenolate (Na_2mp) with PdCl_2. It crystallizes in monoclinic with space group P2_1/n, a=9. 088(1),b=17. 851 (4), c=12. 932(2) , β= 93. 21 (1)°, V=2094. 7(7), D_c=1. 54 g/cm￣3, F(000) = 1000, Z=2, and final R= 0. 044 and R_w= 0. 055 for 3090 reflections (I≥3σ(I)). Structure analysis revealed the multifunction chelating character of mp functions as S_tO_t(t for terminal) and S_bOH (b for bridging) in the complex.

Synthesis, Characterization of Mn2＊, Co2＊, Ni2＊, Cu2＊ and Zn2. Complex Salts with 2,3,5-（Triphenyl） Tetrazolium Chloride and the Crystal Structure of [C N4（ C6H5）3]2[C uC 14]

A series of new complex salts of the type [R]2[MC14] where R =[Ph-C=n-N-Ph N=N-Ph],M = Mn2＋, Co2＋, Ni2＋, Cu2＋ and Zn2＋ wereprepared and characterized by elemental analysis, molar conductance, IR and UVNis is spectral studies and magnetic measurements.The crystal structure of[Ph-C=n-N-Ph N=N-Ph]2[CuCl4] was determined by single crystal X-ray crystallography. The structure consisted of anion part and a 2,3,5-（triphenyl） tetrazolium cation as counter ions. The copper complex has a distorted tetrahedral geometry, the CI（1）-Cu-CI（2） [124.33 （2°）] and Cl（3）-Cu-Cl（4） [131.03 （2°）] angles are significantly larger than the ideal tetrahedral. The [CuCI4] anion and its counter ions are connected through a hydrogen bonds between C1 of the dianion and hetero aromatic rings by Cl-π, π-π and C-H … π, interactions.

Hydrothermal Synthesis and Structure of a New Two-dimensional Zincophosphite: Zn_2(HPO_3)_3·H_2DACH(DACH = 1,2-diaminocyclohexane)

A new open-framework zincophosphite, Zn2(HPO3)3H2DACH 1, was hydro- thermally synthesized in the presence of 1,2-diaminocyclohexane (DACH) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Crystal data for 1: Mr = 486.88, monoclinic, space group P21/c with a = 10.2287(11), b = 9.7624(11), c = 16.1686(18) , b = 92.573(2), V = 1612.9(3) 3, Z = 4, Dc = 2.005 g/cm3, F(000) = 984, = 3.314 mm-1 and S = 1.152. The final R = 0.0473 and wR = 0.1121 for 2456 observed reflections with I > 2s(I). The inorganic layer consisting of four- and eight-membered rings is constructed of alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertices. The organic template molecules reside in the interlayer region and interact with the inorganic network through H-bonds.

Crystal Structure of Copper（Ⅱ） Complex with 3－Hydroxyl－1，5－diazacyclooctane

Crystal structure of copper(Ⅱ) complex with a new mesocyclic diamine ligand 3-hydroxyl-1, 5-diazacyclooctane, Cu [C_(12)H_(28)N_4O_2]Br_2, M_r= 483. 7 is reported. It crystallizes in orthorhombic Pbca with a= 16. 201 (5), b=10. 513 (4), c=9. 992(4) A, V=1701. 8(7) A￣3, Z=4, D_c=1. 888 g/cm￣3, μ=49. 5 cm￣(-1) (MoKa),F(000) = 972. The final R and Rto are 0. 039 and 0. 047 for 1052 observed reflections with I≥3σ(I). The result of X-ray structure determination shows that 3hydroxyl-1,5-diazacyclooctane forms a 2 :1 complex with CuBr_2 in which the central copper ion is sandwiched between the two ligands.

Chiral Phosphine Ligands Derived fro m Sugars .14 . Crystal Structure of Diphenyl( m ethyl4’,6’-O-benzylidene-3’-deoxy-α- D-altropyranoside-3-)phosphine Oxide

The crystal structure of the title compound, C 26 H 27 O 6P, has been determined by single crystal X ray diffraction analysis. The crystal is orthorhombic with space group P2 12 12 1, a=6.154(4), b=17.199(8), c=22.180(3) , V=2347.6 3, D c=1.32 g/cm 3, F(000)=984, μ=1.5 cm -1 , Z =4, and final R =0.075 and R w =0.080 for 1417 reflections (I≥3σ(I)) . The X ray diffraction analysis revealed that the structure of the title compound s similar to that of its parent phosphine and the pyranose and 4, 6 O benzylidene rings remain distorted chair conformations.

Synthesis,Structure and Reaction of a New BitungstenCompound:(Et_4N)_2W_2S_4 (tdt)_2

The new binuclear tungsten compound (Et4N)2W2S4(tdt)2 (H2tdt=H2S2C6H3CH3) (I) with Mr=1067. 97 has been prepared and characterized by IR andX-ray single crystal analysis. Compound (I) has been synthesized by two routes, ofwhich one was from the reaction of (NH4)WS4 with H2tdt, and the other is from lig-and substitution reaction of W2S4 (dip)2 by H2tdt. The compound contains a typical[W2S4j2+ moiety with a W-W bond of 2. 862(2) A. Its crystallographic data are: or-thorhombic, space group Pbca, a=23. 995 (9), b=31. 496 (7), c=10. 537 (5) A, V=7950(8) A3, Z=8, Dc= 1. 78 g·cm-3, p(MoKa)= 63. 37 cm-1 and R=0. 062 for1926 reflections with I≥3d(I). Synthesis, structure and reaction of the compound arediscussed in this paper.

Solid Synthesis and Crystal Structure of Compound[ (PPh_3 )_3,Cu_2MoOS_3]

A brown-red compound [( PPh_3 )_2Cu_2MoOS_3] was synthesized through a solid state reaction. The crystal is monoclinic, space group P2_1/c with α =19. 316(5), b=10. 46(1), c=24. 738(8) A, β=97. 01(2)°, V=4946(9) A￣3, Z=4. The unique Mo atom has a distorted tetrahedral coordination geometry, one Cu atom has a distorted tetrahedral coordination geometry, too, but the other has a trigonal planar environment. The core , Cu_2MoOS_3, shows a butterfly-like structure.

The Synthesis and Crystallographic Characterization of Heterotrimetallic Linear Complex of [Et_4N][ (Ph_3P)_2{CuS_2WS_2Fe} Br_2]

The complex [Et4N][(Ph3P)2{CuS2WS2Fe} Br2] (1 ), C44, H50NBr2CuFeP2S4W, M4= 1246. 13, has been obtained by reaction of [Et4N]2[WS4] andFeBr2 with Cu (Ph3P )3I in MeCN/CH2Cl2. Crystal data for [Et4N][(Ph3P)2{CuS2WS2Fe) Br2] (1): triclinic, P1, Z = 2, a= 13. 495 (7), b = 15. 322 (5), c =12. 361 (4), a=105. 32(3), β=93. 19(4), γ=101. 35(4) and V=2401. 2 The bond lengths of W-Fe bond and the W-Cu distance are 2. 793(2) A and 2. 823(2), respectively. Three kind metal atoms of the title structure [Et4N][(Ph3P)2{CuS2WS2Fe}Br2] (1) are nearly distributed along a line, and along which three metalatoms (W, Cu, Fe) are approximately tetrahedral coordination.

Crystal Structure of Trinitratotri(Butylcaprolactam) Terbium(Ⅲ) Tb[■C_4H_9]_3(NO_3)_3

Tb[CH_2(CH_2)_4CONC_4H_9]_3(NO_3)_3,Mr=821.92. It is monoclinic,space group P2_1/c,a=18.604(2), b=9.768(1),c=21.887(3),β=96. 06(1)°,V=3955. 4(8),Z=4,Dc=1.43 g/cm￣3, MoKα radiation,μ=23.19 cm-1,F(000)=1760, R=0.039 for 2982 reflections with I>3σ(I).Tb(Ⅲ) is coordinated by three carbonyls of the three organic ligands and three bidentate nitrate groups. So each Tb(Ⅲ) is coordinated by nine oxygen atoms to form a distorted tricapped trigonal prism.