Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate（Ⅲ） [C4HgNH3]2Sb4S7

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 P with a = 7.0124(11), b = 11.919(2), c = 14.879(3) (A), α = 108.791(3), β = 102.441(3), γ = 92.846(2)o, V = 1140.1(3) (A)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.     

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, Nano-particle Morphology and Interaction with ATP of[NH3CH2CH(NH2)CH3]2[M(Ⅵ)O2(OC6H4O)2] (M=Mo0.6W0.4) and Its Activity to Promote DNA Cleavage

The title complex[NH3CH2CH(NH2)CH3]2[M(Ⅵ)O2(OC6H4O)2](M=Mo0.6W0.4)was synthesized via a simple solution-phase chemical route. The determination of single crystal X-ray diffraction revealed that the title compound is crystallized in a monoclinic system with P2(1)/n space group, a=1.0913(10) nm, b=1. 0442(10) nm,c=1.8842(19) nm, α=90°, β=96.530(17)°, γ=90°,Z=4, and V=2. 133(4) nm3. The mononuclear anionic unit [M(Ⅵ)O2(OC6H4O)2]2- displays chiral pseudo-octahedral [MO6] coordination geometry and is ges show that the title complex is comprised of nano-particles with diameters ranging from 20 to 50 nm. The NMR study shows the 1 H downfield chemical shifts of [NH3CHaHbCH(NH2)CH3] cations in the title complex when it is mixed with adenosine-triphosphate(ATP), and the chemical shift difference between Ha and Hb is increased greatly,and most of the catecholate ligands dissociate from the central metal atoms. The DNA cleavage activity experiment reveals that DNA cleavage promoted by the title complex is lower than that by Na2MoO4 which possesses antitumor property, but higher than that by Na2WO4.     

The Crystal and Electronic Structure of A Reticular Type Mo-Fe-S Cluster Compound [Et_4N]_4[Mo2Fe_4S_9(SCH_2CH_2S)_2]

The single crystal of [Et4N]4 [MO2Fe4S9(SCH2CH2S)2] was obtainedby reaction of (NH4)2HoS4, FeCl3 , HSCH2CH2SH and Et4 NBr in CH3CN and MeOH-MeONa. Cluster compound [Et4N]4 [Mo2Fe4S9(SCH2CH2S)2] crystal -Lized in the monoclinic space group C2/c with unit cell parameters:a = 17. 672(2)A, b = 33. 851(4)A, c = l3. 900(3)A, β=135.11(4)°, V=5868.8 (3.9)A3 and Z = 4. On the basis of 3514 unique data (I>2σ(I)) the structure was refined to R = 0.0575. The anion [Mo2Fe4S9(SCH2CH2S)2]4-of the cluster compound includes doubly bridging (μ2-S), triply bridging (μ3-S) and quadruply bridging (μ4 -S) . The structrue analysis gives a rule with bond lengths decreasing in the order of Fe-(μ4-S)> Fe-(μ3-s)> Fe-(μ2 -s) and EHMO calculation gives the other rule with bond order increasing in the order of Fe-(μ4-S)< Fe-(μ3-S)相似文献   

Synthesis and characterization of a new open-framework zinc phosphite (4,4′-(C5H4N)2(CH2)3)·[Zn3(HPO3)4]

Employing 4,4-trimethylenedipyridine as a template,a new two-dimensional zinc phosphite (4,4-(C5H4N)2(CH2)3)· [Zn3(HPO3)4 ] has been prepared at room temperature and characterized by single-crystal X-ray diffraction,FTIR,elemental analysis,powder X-ray diffraction,and thermogravimetric analysis.The compound crystallizes in the monoclinic space group P2 1 /c,with cell parameters,a=9.3309(19),b=14.798(3),c=33.637(7),β=91.11(3),V=4643.8(16) nm 3 and Z=4.The connectivity of the ZnO4 tetrahedra and HPO 3 pseudo pyramids results in infinite corner-sharing 4-membered ring chains as second building units which are further linked by Zn O P bonds to form a 2-D layer that with interesting 8-membered ring channels along the [100] direction.The diprotonated 4,4-trimethylenedipyridine molecules sit in the middle of the layers along the [100] direction and interact with the framework via hydrogen bonds.     

Synthesis and Crystal Structure of [NdCl5(THF)]2-[HO-4,6-di-tBu-C6H2-2-CH2{CH(iPrNCHCHN)}]2+·THF

The title complex 1·THF has been synthesized by the reaction of [HO-4,6-di-tBu-C6H2-2-CH2{CH(iprNCHCHN)}]Cl with NdCl3 in a 2:1 molar ratio in THF, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a =9.6501(14), b = 16.393(2), c = 36.745(6) (A), β = 97.444(4)°, V = 5763.7(15)(A)3, Mr= 1124.69, Z =4, Dc= 1.296 g/cm3, μ(MoKa) = 1.175 mm-1, F(000) = 2348, the final R = 0.0729 and wR =0.1762 for 8735 observed reflections with I ＞ 2σ(1). Complex 1 consists of an anion [NdCl5(THF)]2- and two cations [HO-4,6-di-tBu-C6H2-2-CH2{CH(iprNCHCHN)}]2 to form a layer structure by the interconnection of anions and cations via hydrogen bonding. The central metal Nd in the anionic unit is coordinated by five Cl atoms and one oxygen atom from solvated THF molecule assuming a distorted octahedral geometry.     

Synthesis and Structure of a New Gadolinium Porous Complex Assembled from 2,3-Pyrazinedicarboxylic Acid and Ammonia

A new gadolinium porous complex,(NH_4)_2[Gd2(pzdc)4(H_2O)2], was synthesized through hydrothermal reaction of 2,3-pyrazinedicarboxylic acid and Gd(NO3)3·6 H_2O with the pH value adjusted by ammonia. It was characterized by elemental analysis, FT-IR, TGA and further by single-crystal X-ray crystallography. It crystallizes in monoclinic, space group P21/c with a = 14.249(7), b = 15.889(8), c = 12.846(7) ?, β = 95.724(10)°, V = 2894(3) ?3, Z = 4, Dc = 2.385 g/cm3, μ(Mo Ka) = 4.65 mm–1 and F(000) = 1976. 1976 reflections were measured and 6446 independent reflections(Rint = 0.0985) were used in further refinement. The complex exhibits a 3D framework constructed from the [Gd2(pzdc)4(H_2O)2]2-building blocks. It is scarce that the NH4+ cations are located in the channels and balance the charge of anion framework. Furthermore, the ion exchange property of this complex has also been studied. The NH4+ cations can be replaced by Na+ cations, which is an uncommon phenomenon for gadolinium-containing porous complex.     

THE CRYSTAL STRUCTURE OF TR1S (μ-SULFJDO)-(U3-SULFJDO)-TETRAKTS (O,O-DIETHYLPHOSPHORODITHIOATO-S,S)-OXAZOLE-TRI-MOLYBDENUM-ANTIMONOUSCHLORID {Mo_3(U3-S)[u-S)_3·SbCl_3][S_2P(OEt)_2]_4·(C_3H_3ON)}

<正> Mr = 1445.67, triclinic. The space group is P1 with the unit cell parameters: a = 10.342(3), b = 11.994(3), c = 21.352(4) A; (?)= 76.27(2), β - 88.55(2)°, r = 73.26(2)°; V = 246lA3, Z = 2, DC = 1.959 g.cm-3. The final R factor is 0.068 based on 4053 reflectioons with I≥3(?)(Ⅰ). The title compound may be regarded as the result of that a molecule of trinuclear Mo cluster {Mo3S4[S2P(OEt)2]4·(C3H3ON)}[1] connects with a molecule of SbCl3 by three bridging S atoms. The skeleton {Mo3SbS4} is a distorted cube. The distances of Mo-Mo bonds are 2.728(2), 2,743(2) and 2.751(2) A, respectively, and the distances between Sb and Mo atoms are 3.814(2), 3.815(2) and 3.847(2) A, respectively.     

THE CRYSTAL STRUCTURE OF BAYLEYITE

The bayleyite crystallizes in monoclinic space group C_2~5h-P2_1/c with a=6.499(1), b=15.235(5), c=26.513(6), β= 92.92(2)°, Z=4. Intensities of 3430 independent reflections are collected with diffractometer using MoKα radiation. The crystal structure has been solved by the Patterson method and refined by block least square refinement for positional parameters and isotropic temperature factor of non-hydrogen atoms. The final R factor is 0.038.The result of crystal structure analysis shows that the structure consists of discrete [UO_2(CO_3)_3]~(4-) ions and Mg~(2 ) cations are between slab-like units, but they are not in a slablike unit. Its crystal struture is different from that of liebigite which was determined by Appleman. Complexes and cations between slab-like units and in a slab-like unit are connected by hydrogen bonds formed by water molecules.     

Synthesis and Crystal Structure of [NdCl_5(THF)]~(2-) [HO-4,6-di-~tBu-C_6H_2-2-CH_2{CH(~i PrNCHCHN)}]_2~ ·THF

The title complex 1·THF has been synthesized by the reaction of [HO-4,6-di-tBu- C6H2-2-CH2{CH(iPrNCHCHN)}]Cl with NdCl3 in a 2:1 molar ratio in THF, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 9.6501(14), b = 16.393(2), c = 36.745(6) , β = 97.444(4)o, V = 5763.7(15) 3, Mr = 1124.69, Z = 4, Dc = 1.296 g/cm3, μ(MoKα) = 1.175 mm-1, F(000) = 2348, the final R = 0.0729 and wR = 0.1762 for 8735 observed reflections with I > 2σ(I). Complex 1 consists of an anion [NdCl5(THF)]2- and two cations [HO-4,6-di-tBu-C6H2-2-CH2{CH(iPrNCHCHN)}]2 to form a layer structure by the interconnection of anions and cations via hydrogen bonding. The central metal Nd in the anionic unit is coordinated by five Cl atoms and one oxygen atom from solvated THF molecule assuming a distorted octahedral geometry.     

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.     

Synthesis and Crystal Structure of a Magnesium Metal-organic Framework

A magnesium metal organic framework, [NH2(CH3)2][N(CH3)4][Mg5(bpdc)3(O2CH)6]· 3H2O (1, bpdcH2 = 4,4′-biphenyldicarboxylic acid), has been solvothermally synthesized and structurally characterized. 1 crystallizes in the trigonal system, space group R-3, with a = 11.3427(3), c = 41.5662(18) , V = 4631.3(3) 3, Z = 3 and the final R = 0.0457. Its structure features a pillared-layered three-dimensional network with 8.21  cavities, in which cationic [NH2(CH3)2]+ or [N(CH3)4]+ and lattice water molecules are located. Thermal stability of the title compound has also been investigated.     

CRYSTAL STRUCTURE OF 2, 4-DITHIONE-3-AMINO-1, 3, 2-OX-AZAPHOSPHORINEBENZO-2-THIONO PYRIDINIUM

<正> The structure of title compound [C7H6N2OPS3]-·[HNC5H5]+ was determined by x-ray diffraction. It belongs to monoclinic system with space group P21/a, a = 16.745(2), b= 8.563(2), c=21. 050(5)(?), β=93.32(1)°, V= 3013. 6(?)3, Z = 8, Mr = 341. 4, F (000) = 1536, Dc=1. 504 g. cm-3,μ= 53. 0 cm-1. The crystal is composed of discrete cations C5H5NH+ and anions CrH6N2OPS3-. There are two pairs of the cations and the anions in each asymmetric unit. The stability of the anion is increased by the formation of (d-p)π bonding involving the 3d orbital of the P atom and the lone electron pairs of the S atoms.     

Solid state synthesis and structure of two novel polyoxometalates [(n-Bu)_4N]_4[M_6o_(19)][Ag_21_4](M=Mo,W)

The reaction of [NH4]2[MO2S2],AgI and (n-Bu)4NBr in solid state produced the polyoxometalates [(n-Bu)4N]4[M6O19][Ag2l4] (1,M=Mo;2,M=W) which were structurally determined.The crystals of 1 and 2 are isomorphous,monoclinic,space group P221/c.1,a=1.6624(2),6=1.6699(3),c=1.7217(2) nm,(8=98.29(1)°,V =4.729(1) nm3,Z=2,R=0.040,Rw=0.037;2,a= 1.6636(3),6=1.6733(3),c=1.7190(3) nm,β=98.25(1)°,V=4.736(1) nm3,Z=2,R=0.038,Rw=0.047.The results of the structure determination showed that the two compounds had the same structures whose skeletons are composed of [Ag2I4]2-and [M6O19]2-The difference of them and heteropolymetalate compounds synthesized in solution is that the title compounds contain cluster ion,heteropolymetalate and organic cations,while the latter is only composed of heteropolymetalate and organic cations.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-COPPER-SULFUR CLUSTER COMPOUND [(CH_3CH_2 )_4N]_2 [(μs-S)CusS_6(S_2)_6Mo_6O_6].DMF

The synthesis and crystal structure of a novel molybdenum-copper cluster compound with [(μs-S)Cus] core is reported. It was prepared from Cu2Br2 upon reaction with molybdenum sulfur compound [CH3CH2)4N]2[Mo2O2S2-(S2)(S4)]. The title compound crystallizes in the monoclinic system space group Cc with cell dimensions: a=21.320(5), b=21.869(3), c=13.029(5)A,β=118.28(1)°,Z=4, V=5349A3 and Dc=2.48 g.m-3. The structure has been determined by Patterson and Fourier methods and then refined by the least squares method to a final R of 0.053. There are some distortions from octahedron in configuration of the [(μs-S)Cu6]6 core with three weak Cu-Cu bonds.     

Crystal Structure, Nano-particle Morphology and Interaction with ATP of [ NH3 CH2 CH（ NH2 ） CH3 ]2 [ M（ Ⅵ ） O2 （ OC6 H4 O）2 ] （M = Mo0. 6 W0. 4 ） and Its Activity to Promote DNA Cleavage

The title complex [NH_3CH_2CH(NH_2)CH_3]_2 [M(Ⅵ)O_2(OC_6H_4O)_2](M= Mo_(0.6)W_(0.4))was synthesized via a simple solution-phase chemical route.The determination of single crystal X-ray diffraction revealed that the title compound is crystallized in a monoclinic system with P2(1)/n space group,a=1.0913(10)nm,b=1.0442(10)nm,c=1.8842(19)nm,α=90°,β=96.530(17)°,γ=90°,Z=4,and V=2.133(4)nm3.The mononuclear anionic unit [M(Ⅵ)O2(OC6H4O)2]2-displays chiral pseudo-octahedral [MO_6] coordination geometry and is linked by chiral cations via hydrogen bond and π…π stacking interaction.The transmission electron microscopy images show that the title complex is comprised of nano-particles with diameters ranging from 20 to 50 nm.The NMR study shows the 1H downfield chemical shifts of [NH_3CHaHbCH(NH_2)CH_3] cations in the title complex when it is mixed with adenosine-triphosphate(ATP),and the chemical shift difference between Ha and Hb is increased greatly,and most of the catecholate ligands dissociate from the central metal atoms.The DNA cleavage activity experiment reveals that DNA cleavage promoted by the title complex is lower than that by Na_2MoO_4 which possesses antitumor pro-perty,but higher than that by Na_2WO_4.     

Synthesis, Single-crystal Structure, and Optical and Magnetic Properties of CaEr2S4

Brown needle-like crystals of CaEr2S4 were isolated as the major product from a reaction of elements and binary sulfides by a two-step flux technique. CaEr2S4 crystallizes in the orthorhombic space group Pnma with a = 12.845(4), b = 3.862(4), c = 13.001(2) , V = 645.0(7) 3, Z = 4, F(000) = 880, μ(MoKα) = 27.794 mm-1, the final R = 0.0528 and wR = 0.0562 for 1070 observed reflections with I > 3σ(I). The CaEr2S4 structure forms a three-dimensional framework that consists of interconnected tetra-octahedral Er4S18 fragments. Ca2+ cations, in a monocapped trigonal prism geometry, are stuffed in two parallel rows into the one-dimensional channels along the b direction. CaEr2S4 is an infrared-transparent semiconductor with a band gap of 1.81 eV. Magnetic susceptibility measurements over 6～300 K indicate a Curie-Weiss paramagnetic behavior for the phase, with an effective magnetic moment of 9.64(1) μB per Er3+ ion.     

New Dimeric Selenidoarsenate(III):Solvothermal Synthesis and Crystal Structure of [Co(en)_3]_2As_2Se_5

1 INTRODUCTION The mild solvothermal synthesis with the presence of a structure-directing agent is proved to be a versa- tile route for the preparation of chalcogenidometa- lates of the heavier group (14 and 15) elements[1～3]. Templated by the transition metal complex cations, a large number of chalcogenidoantimonates containing transition metal complex ions have been synthesized by solvothermal method, such as Mn2(en)2Sb2S5[4], [Co(en)3]CoSb4S8[5], [M(en)3]Sb2S4 (M = Co, Ni)[6], [N…     

Synthesis and Crystal Structure of [K（2,2,2-crypt）]_3Sb_（11）

The title complex [K(2,2,2-crypt)]3Sb11 has been prepared by the reaction of K3Cd2Sb with Cu-C≡CH in ethylenediamine in the presence of 2,2,2-crypt, and characterized by low temperature X-ray structure analysis. The crystal is of orthorhombic system, space group C2221 with a = 15.475(3), b = 22.807(5), c = 24.834(6), V = 8765(3)3, Dc = 1.960 g/cm3, C54H108K3N6O18Sb11, Mr = 2586.01, F(000) = 4944, μ = 3.531 mm-1, Z = 4, R = 0.0442 and wR = 0.1053 for 10265 observed reflections (I > 2σ(I)). The "naked" Sb113- anion is stable due to the completely sequestered alkali metal cations through ion-ion interactions.     

Syntheses, properties and structures of copper and nickel complexes of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate

The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR s