新型杂多蓝化合物[NH_3(CH_2)_2NH_3]_5[Cd(H_2O)][CdMo_(12)~ⅤO_(30)(HPO_4)_6(H_2PO_4)_2]·5H_2O的合成与晶体结构

利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMo12ⅤO30(HPO4)6(H2PO4)2].5H2O.通过元素分析I、CP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.564 2(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.030 0,wR2=0.071 6.     

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system,space group P1 with a=7.0124(11),b=11.919(2),c=14.879(3),α=108.791(3),β=102.441(3),γ=92.846(2)o,V=1140.1(3)3,Mr=859.71,Z=2,Dc=2.504 g/cm3,μ =5.324 mm-1,F(000)=804,S=1.013,the final R=0.0297 and wR=0.0618 for 3534 observed reflections with I > 2σ(I). 1 consists of [C4H9NH3]+ cations and two-dimensional [Sb4S7]n2n- anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]+ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.     

Crystal Structure of Binuclear Bridging Complex[(dppf)_2Pd_2 (Ⅱ) (μ-Cl)_2] [PF_6]_2

1INTRODUCTIoNFerrocenecontainingtransitionmeta1complexeshasarousedtheinterestofchemistsbecauseofitsnovelstructureandproperties"',Huangetal[2'3isynthesizedsomechainandbridgeformcomplexesandstudiedtheirIRandCV.Linetal[4isyn-thesizedthecrystalof[(dppf)PdCl,jO.5[(CH3),COj(dppf=1,11-(diphenylphosphine)-ferrocene)anddeterminedthestructurebyX-raydiffraction.Inthisarticlewereportthesynthesisandcrystalstructureof[(dppf),Pd,(ll)(p-Cl),j[PF,j2.2EXPERIMENTAL2.1PreparationAsolutionofO.86mm…     

铂氢化物trans-[PtH(tu)(PPh_3)_2]Cl(tu)(THF)_2(tu=SC(NH_2)_2)的结构

制得含硫脲配体的铂氢化物单晶trans-[PtH(tu)(PPh_3)_2]Cl(tu)(THF)_2,其结构测定结果为:C_(46)H_(55)N_4O_2P_2S_2ClPt M=1052.6,单斜晶系,空间群为 P2_1/c,a=12.103(1),b=21.619(3),c=20.189(4)(?),β=103.31(0)°,V=5140(2)(?)~3,Z=4,D_c=1.360g·cm~(-3),F(000)=2128,R=0.050,R_w=0.063.Pt(Ⅱ)与两个磷、一个硫脲分子的硫和一个氢相配合,形成四边形配位。     

Syntheses and Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)_2Cl]·ClO_4 and [Zn(bipy)_2Cl]·BF_4

Two new transition metal complexes, [Ni(bipy)2Cl]·ClO4 (bipy = 2,2'-bipyridine) 1 and [Zn(bipy)2Cl]·BF4 2, have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 crystallize in monoclinic space group P21/n with Z = 4. For 1, a = 10.776(1), b = 12.067(1), c = 16.146(2) , β = 93.021(2)o, V = 2031.9(4) 3, Mr = 505.98, Dc = 1.654 g/cm3, μ = 1.255 mm–1, F(000) = 1032, the final R = 0.0406 and wR = 0.1002 for 3983 observed reflections with I > 2σ(I). For 2, a = 10.758(4), b = 12.058(4), c = 16.135(5) , β = 104.57(1)o, V = 2025.7(12) 3, Mr = 500.00, Dc = 1.639 g/cm3, μ = 1.396 mm–1, F(000) = 1008, the final R = 0.0470 and wR = 0.1237 for 3759 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. A one-dimen-sional zigzag double hydrogen-bonding-chain is generated by the intermolecular M-bipy ···anion···bipy- M hydrogen bonding interactions between the chelating ligands of bipy and anion.     

CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

CRYSTAL AND MOLECULAR STRUCTURE OF AuCSC(NH_2)_2]_2CiO_4 CONTAINING TWO-COORDINATE COMPLEX CATION

<正> Au [SC(NH2)2]2C1O4, Mr,= 448. 66, orthorhombic, Pcca, α= 17. 873 (2),b = 8. 2933(7), c = 7. 196(2) A V=1066. 6A3,Z=4,DC = 2. 794g·cm-3,R= 0. 049,Rw=0. 068 for 807 observed reflections. The structure consists of complex cation Au[SC(NH2)2]2+ and perchlorate ion ClO4-. The gold atom( I ) in the cation has a slightly bent linear coordination geometry.     

THE PREPARATION AND CRYSTAL STRUCTURE OF IMIDAZOLATE BRIDGED HETEROTRINUCLEAR COMPLEX [ (NH_3)_5 RhlmZn ( dien )-ImRh(NH_3)_5(C10_4)_6·4H_2O

<正> The imidazolate bridged heterotrinuclear complex [(NH3)5RhImZn(dien)-ImRh(NH3)5](ClO4)6·/4H2O,Mr= 1347. 56,was prepared and crystallized in the mono-clinic space group C2/c with unit cell constants, a = 32. 972 (4) , b = 9. 482 ( 1) , c = 15. 250(3) A ,β = 91. 26(1)°,V = 4766. 6A3 and Z=4. The structure was determined from 9043 independent reflections and refined to R=0. 049 for 3051 observed MoKa reflections. The Zn atom showed a distorted trigonal bipyramid coordination, being bonded to three nitrogen atoms of dien and two of imidazole. Each imidazole anion bridged one Zn atom and one Rh atom. The Rh atom was coordinated by six nitrogen atoms,one of which is from imidazole and the five others from NH3 forming a regular octahedral coordination.     

具有螺旋结构的新型硼磷酸盐化合物:(NH_4)_(0.5)(H_3O)_(0.5)Mg(H_2O)_2BP_2O_8

利用水热方法合成新型硼磷化合物 (NH4) 0 .5(H3 O) 0 .5Mg(H2 O) 2 BP2 O8,单晶X射线衍射分析证明化合物属六方晶系 ,空间群为P652 2 ,a =0 .945 0 7( 19)nm ,c=1.5 80 3 ( 5 )nm ,γ =12 0° ,V =1.2 2 2 4( 5 )nm3 ,Mr=2 79.0 6,Dc=2 .2 5 8g/cm3 ,Z =6,F( 0 0 0 ) =83 4,μ =0 .663mm-1.结构中BO4,PO4基团形成1∞{[BP2 O8] 3 -}的螺旋带与MgO6相连构成八面体 -四面体空间骨架 ,元素分析、IR光谱、热重差热分析和电荷平衡计算证明晶体中含有NH+ 4 和质子 .NH+ 4 占据螺旋带螺旋纹内 ,质子化的水分子靠近螺旋带通道的内侧 ,两者均起到平衡电荷和稳定骨架的作用     

CRYSTAL STRUCTURE OF (Br(μ-Met)(μ-Gly)(H_2O)_4]_2[Er(μ-Net)_2(H_2O)_4]_2(ClO_4)_(12)

<正> [Er(u-Met)(u-Gly)(H2O)4]2[Er(u-Met)2(HaO)4]2(ClO4)12(NMet=CH3S-(CH2)2CH(NH2)COOH,Gly=NH2CH2COOH), Mr=3194, trilinic, space group P1, a = 12.375(6),b= 14.041(13), c=19.074(13)A,α=80.85(6),β=80.72(6).γ=62.82(6)° ,Z=1,V= 2896A3,Dc=1.83 g/cm3,R=0.091. The carboxyl groups of Met and Gly in the title complex are bonded to Er atoms as bidentate bridging ligands.There are two different cations located at crystallographic symmetry centers in one unit cell.     

CRYSTAL STEOCTURE OF [Cu(HCOO)_2(HCOOH)_2]n

<正> Mr=245.6, monoclinic, V2l/c, a=7.778(4), b=7.946(4), c=8.008(4) X, B=115.31(4)? V=447.483, Z=2, Dx=1.82 g/cm3, X(Mokct)=0.710698, y=25.5cm~1 F(000)=245.96, T=293 K. The final R=0.059 for 423 unique observed reflections. Cu2-' is coordinated by six oxygen atoms to form a distorted octahedron. Cu2^ ions are linked together by formate groups in an anti-anti bridging arrangement to form a two dimensional polymer. Two oxygen atoms in a formate group are equivalent with C(l)-0(l)=l.25(1) and C(l)-0(2) = l. 2.5(1)8.     

Crystal structure and single crystal EPR of (NH_4)_2(15-crown-5)_3[Cu(mnt)_2] and (NH_4)_2(benzo-15-crown-5)_4[Cu(mnt)_2]·0.5H_2O

The X-ray crystal structures of (NH4)2(15-crown-5)3[Cu(mnt)2] (1) and (NH4)2(benzo-15-crown-5)4- [Cu(mnt)2]·0.5H2O (2) were determined. Two single crystals are composed of distinct structures of ammonium-crown ether supramolecular cation and [Cu(mnt)2]2? anion. The triple-decker dication in complex 1 and a sandwich dimmer in complex 2 were observed. X-Band EPR studies on the single crystals of both complex 1 and complex 2 have been carried out at room temperature, which revealed that complex 2 showed a perfect hyperfine structure of Cu whereas that of complex 1 could not be observed. The principal values and direction cosines of the principal axes of the g and A tensors were computed by a least-squares fitting procedure. The spin density of Cu(II) was estimated according to the principal values of the A tensors and compared well with the results calculated based on DFT method.     

[Et_4N]_2[Zn_2(OPh)_2Cl_4]的合成和晶体结构

ZnCl2, PhONa和Et4NCl稨2O在乙腈溶剂中反应合成了一种二核锌配合物[Et4N]2[Zn2(OPh)2Cl4]。X射线衍射结果表明,晶体属单斜晶系,C2/m空间群,晶胞参数 a = 14.1366(2), b=13.6985(5), c=9.3308(3)牛?107.851(2)o, V=1719.92(9)?,C28H50O2N2Zn2Cl4,Mr=721.24,Z=2,Dx=1.393g/cm3,μ(MoKα)=1.732mm—1,F(000)=756, R=0.0552, wR=0.1534, S=1.027。 配合物是由2个阳离子Et4N+和1个阴离子[Zn2(OPh)2Cl4]2—组成。阴离子[Zn2(OPh)2Cl4]2—包含着1个中心Zn2O2菱形平面。配合物中的2个锌原子通过2个苯酚中的氧原子桥连,每个锌原子还与2个氯原子配位形成变形四面体结构。     

THE SYNTHESIS AND STRUCTURE OF THE IMIDAZOLATE-BRIDGED HETEROTRINUCLEAR COMPLEX (en)_2Ni[(Im)Co-(NH_3)_5]_2(CIO_4)_6·5H_2O

<正> (H2NC2H4NH2)2Ni [(C3H3N2) Co (NH3)5]2 (CIO4)6 · 5H2O,NiCo2Cl6O29N18C10H62, Mr = 1288. 00, monoclinic, C2/c, a = 31. 832(4), b = 9. 691 (1), c=15. 425(4)(?),β=90. 71(2)°, Z = 4, V = 4758. 0(?)3, Dc=1. 798g/cm3, μ (MoKa) = 15. 22cm-1, F(000)=2656. The three metal nuclei, one Ni( Ⅱ ) and two Co( Ⅲ ), bridged by two imidazolyl anions (Im = C3H3N2), form an isosceles triangle. The Ni( Ⅱ ) atom is situated on the two-fold axis and coordinated by six nitrogen atoms to form a distorted octahedron with two nitrogen atoms from two Im in cis-positions. The two Co( Ⅲ ) atoms are related by C2 symmetry and each Co( Ⅲ ) is coordinated by six nitrogen atoms to form an octahedral configuration.     

SYNTHESIS AND STRUCTURE OF A NEW DINUCLEAR MOLYBDENUM(O) COMPLEX [Et_4N]_2 [Mo_2 (CO)_8 (SCH_2COOEt)_2]

<正> t Reaction of Et^NI, NaSCH2COOEt with Mo(CO)6 in MeCN affords a new dinuclear molybdenum(O) complex, [Eti,N]2 [Mo2(CO) 8(SCH2COOEt)2] (I) . The crystal and molecular structure has been determined from three-dimensional X-ray data. 1_ crystallizes in the triclinic, space group PI with a=10.362(1), b= 10.391(1), c=10.815(2) X, a=91.64(2), 6=100.07(2), Y=H4.46(1)? Z=l, R= 0.048 for 2975 reflections with I?o(I). Noribonding of Mo...Mo distance (3.939(11)A) in _! supports the previous speculation for the two-electron redox properity,of complex anion, [Mo2(CO)g(SR)2J2~.     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates:C_4H_(10)N_2·B_6O_8(OH)_2 and (NH_3CH_2CH_2NH_3)B_5O_8(OH)

Two new borate compounds,C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8-(OH) 2,have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction,IR,elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system,space group P21/c,with a=8.3318(17),b=6.2118(12),c=12.479(3) ,β=108.96(3)o,V=610.8(2) 3,Mr=313.02,Z=2,Dc=1.702 g/cm3,μ=0.150 mm-1,F(000)=320,R =0.0387 and wR =0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system,which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic,space group Cc,with a=6.7207(13),b=11.481(2),c=12.564(3) ,β=95.25(3)o,V=965.4(3) 3,Mr=261.18,Z=4,Dc=1.797 g/cm3,μ= 0.164 mm-1,F(000)=536,R=0.0396 and wR=0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

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.     

固相配位化学反应研究(L)——[(n-Bu)_4N]_2[MoOS_3(CuNCS)_3]的固相合成及其晶体结构

(NH4)2MoOS3、CuSCN、KSCN和(n-Bu)4NBr发生固相反应,产物经DMF/CH2Cl2处理,得暗红色标题化合物晶体[(n-Bu)4N]2[MoOS3(CuNCS)3].晶体属单斜晶系,空间群P21/n,a=1.6672(9)nm,b=1.6278(6)nm,c=1.9608(8)nm,β=110.05(4)°,Z=4.标题化合物是具有网兜骨架的Mo-Cu-S杂核簇合物.Mo-Cu的平均键长为0.2647 nm.     

新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMoV12O30(HPO4)6(H2PO4)2]·5H2O的合成与晶体结构

利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMoV12O30(HPO4)6(H2PO4)2]·5H2O.通过元素分析、ICP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.5642(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.0300,wR3=0.071 6.     

Synthesis and Crystal Structure of a New Charge-assisted Hydrogen-bonded Host Framework [Co(en)_3]_2[Zr_2(C_2O_4)_7]·2H_2O

Using the deep eutectic solvent formed of oxalic acid and choline chloride, a new charge-assisted hydrogen-bonded host framework [Co(en)3]2[Zr2(C2O4)7]·2H2O(1) has been obtained. The title complex crystallizes in the monoclinic, space group P21/n(No. 14) with a = 7.7448(10), b = 14.5683(19), c = 19.375(3), β = 92.124(2)o, V = 2184.5(5) 3, Z = 4, Dc = 1.996 g.cm-3, F(000) = 1332, μ = 1.328 mm-1, R = 0.0353 and w R = 0.0718(Ⅰ 2σ(Ⅰ)). Single-crystal structure analysis reveals that the title complex possesses a 3D network assembled through a multitude of charge-assisted hydrogen bonds between the in situ generated anionic coordination complexes [Zr2(C2O4)7]6- and metal complexes Co(en)33+.