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) [C4H9NH3]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.     

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.     

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.     

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   

Ba2SbGaS5: Solid-state Synthesis, Crystal and Electronic Structures, and Property Characterization

Single crystal of Ba2SbGaS5 has been synthesized by the high temperature solidstate reaction method. The compound crystallizes in the orthorhombic space group Pnma with a = 12.177(4), b = 8.880(3), c = 8.982(3), V = 971.4(6)3 , Z = 4, Dc = 4.284 g/cm3 , = 14.487 mm-1 , F(000) = 1096, the final R = 0.0171 and wR = 0.0384 for all data. The structure comprises an infinite one-dimensional 1∞SbGaS54- anionic chain constructed from the GaS4 tetrahedra and the SbS5 polyhedra via sharing edge alternately. The paralleled 1∞SbGaS54- anionic chains engage with each other and form the two-dimensional Sb-Ga-S layer perpendicular to a-axis with the isolated Ba2+ cations arranged between layers. The IR spectrum and the UV-Vis spectrum have been investigated. Also, the first-principles band structure and density of states calculations indicate that the compound belongs to indirect semiconductor with the band gap of 2.1 eV, which is supported by the UV-Vis diffuse reflectance results.     

Synthesis and Crystal Structure of an Unusual Dodecacoordinated Lanthanum Complex by Phenanthroline and Nitrate （phenH）_2[La（NO_3）_5（phen）]·CH_3OH

Lanthanum complex (phenH)2[La(NO3)5(phen)]·CH3OH (1, phen=phenanthroline) was synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a=20.3040(3), b=10.7091(1), c=19.0771(2), β=102.090(1)°, V=4056.07(8)3, Z=4, Dc=1.676 g/cm3, μ= 1.142 mm-1, F(000)=2056, the final R=0.0346 and wR=0.0793 for 9981 (Rint=0.0358) independent reflections. The mononuclear complex 1 consists of four parts: two phenH+ cations formed by the protonation of phen, one complex anion [La(NO3)5(phen)]2-, and one solvent methanol molecule. The complex anion contains one phen and five nitrate ligands which both chelate the center La(III) ion, adopting a distorted twelve-coordinated icosahedral geometry. The cations, anion and solvent molecule are linked together by hydrogen bonds. One of the protonated phenanthrolines (phenH+) acting as cation connects to the anion via N–H…O hydrogen bond directly, and the other one links to the anion through an intermediate solvent CH3OH via N–H…O and O–H…O hydrogen bonds. By the plentiful additional weak C–H…O intermolecular hydrogen bonds, the compound molecules construct a two-dimensional layer structure.     

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 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.     

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 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.     

Two Polymorphs of the Inclusion Compound [（n-C4H9）4N] ＋（C13H9O3）-H2O

Two polymorphs of the inclusion compound [(n-C4H9)4N]+·(C13H9O3)-·H2O havebeen prepared and characterized by X-ray crystallography. Polymorph 1: triclinic P 1 , a =13.4982(2), b = 13.5743(2), c = 17.1996(2) , α = 67.045(1), β = 77.845(1), γ = 88.762(1)°, V =2830.43(7)3, Z = 4, R = 0.0491, wR = 0.1276; Polymorph 2: tetragonal P43, a = b = 13.53690(1) , c = 30.8491(8) , V = 5653.02(16)3, Z = 8, R = 0.0448, wR = 0.0984. In these two crystalstructures, the hydrogen-bonded ribbons built of 4,4 -dihydroxybenzophenone (DHBP, C13H10O3)anions and water molecules are orderly arranged to generate two-dimensional host layers, withtetrabutylammonium cations contained between the layers to form the sandwich-like inclusioncompounds. The structures of 1 and 2, which exist as two polymorphs, both display the similarpacking pattern and hydrogen-bond linking model.     

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, 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.     

Syntheses, Crystal Structures and Thermal and Optical Properties of Two Organic Templated Gallium Antimony Sulfides

Two new gallium antimony sulfides,[enH2][Ga2Sb2S7]·en(1) and [puH]2[Ga2Sb2S7](2)(en = ethylenediamine,pu = propyleneurea),have been solvothermally synthesized.In the pre-paration of compound 2,the protonated propyleneurea cation as counterion and template was in situ synthesized by the reaction of 1,3-diaminopropane with CO2 in pyridine.Both structures contain a two-dimensional network composed of novel heterometallic clusters of {Ga2Sb2S9} as the second-dary building unit.The thermal and optical properties of compounds 1 and 2 were characterized by TGA and UV-Vis,respectively.     

Synthesis and Crystal Structure of Salicylyl-4-phenyl Thiosemicarbazide Lead with a Two-dimensional Network

A two-dimensional lead complex, [Pb(C14N3O2H12S)(NO3)]n·nH2O, was prepared by the reaction of salicylyl-4-phenyl thiosemicarbazide and lead nitrate. The compound (C14H13N4O6PbS, Mr=572.53) crystallizes in the monoclinic space group P21/c with a=11.2984(2), b=15.6628(7), c=11.1118(2), β= 113.564(2)n, V=1802.43(10)3, Dc=2.110 g/cm3, Z=4, μ(MoKα)= 9.515 mm·1, F(000)=1084, the final R=0.0394 and wR=0.0701 for 2552 observed reflections with I > 2σ(I). The Pb(II) ion displays a distorted octahedron in which the hypothesized stereochemically active lone pair occupies the apex. The compound exhibits a two-dimensional network structure formed by the zigzag one-dimensional chains joined by two μ-O of two nitrate groups in overlapping. A large ring exists in the two-dimensional layers. The TGA of the title compound has been studied.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]~(2 )·[SbCl_5]~(2-)}_2

A new supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2,was synthesized by the hydrothermal reaction of o-diaminobenzene,2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution,and characterized by chemical analysis,elemental analysis,IR spectra,thermogravimetric analysis and fluorescence spectra. The crystal structure was deter-mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c,with a=16.0397(13),b=14.3189(12),c=15.6370(13),β=105.8980(10)°,V=3454.0(5)3,Z=4,C24H22Cl10N6Sb2,Mr=992.48,Dc=1.909 g/cm3,μ=2.366 mm-1,S=1.010,F(000)=1920,R=0.0254 and wR=0.0555. The coordination anion,[SbCl5]2-which is a distorted tetragonal pyramid,is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2-form a biquaternion ring structure through the secondary bonding of Sb···Cl. Moreover,the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridyl)benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

CRYSTAL AND MOLECULAR STRUCTURE OF GUANIDINIUM BIS (o-AMINOPHENYLARSENIC) HEXAMOLYBDATE (CN_3H_6)_4[(o NH_2C_6H_4 As)_2Mo_6O_(24)]

<正> Guanidinium bis (o - aminophenylarsenic) hexamolybdate belongs to monoclinic space group P21/c,with a=10. 217(2),b= 18. 870(2),c= 10. 939(2)A,β = 102. 82(3)°,Z = 2,V=2056. 4A3,and Dc=2. 477 g·cm-3. Each molecule contains one [(o-NH2C6H4As)2Mo6O24]4- anion and four CN3H6+ cations. In the anion,six distorted MoO6 octahedra are connected with edges-sharing to form a six-membered Mo ring which is capped above and below by two o - aminophenylarsenic groups. There is half a molecule in an asymmetric unit. It is interesting that both phenyl planes are almost perpendicular to the plane of the Mo atoms. The structure of the anion is similar to that of [ (CH3 As)2Mo6O24]4-,[(n-C3H7As)2Mo6O24]4- or [(C6H5CH2As)2Mo6O24]4-. This is the first example of this type of compounds in which the As atom is directly connected to a substituted phenyl group.     

A Novel Two-dimensional Lead(Ⅱ) Coordination Polymer Based on Dinuclear Lead(Ⅱ) Unit Containing(5-Chloro-quinolin-8-yloxy) Acetate

A novel two-dimensional lead(II) coordination polymer 1, [C11H7Cl2NO3Pb]n, has been prepared by solvothermal reaction of new bridging ligand(5-chloro-quinolin-8-yloxy)acetic acid(HL) with PbCl2, and its structure was characterized by IR, elemental analysis, TG-DTA and single-crystal X-ray diffraction analysis. The crystal is of monoclinic system, space group P21/c with a = 16.7603(7), b = 8.6907(4), c = 8.4745(3), β = 101.1110(11)°, C11H7Cl2NO3 Pb, Mr = 479.27, V = 1211.25(9)3, Z = 4, Dc = 2.628 g/cm3, F(000) = 880, μ = 14.367 mm-1, R = 0.0173 and wR = 0.0508. The asymmetric unit contains one lead(II) cation, one(5-chloro-quinolin-8-yloxy)acetate(L) ligand and a chloride ion. The PbII center is hepta-coordinated in a distorted pentagonal bipyramidal geometry. The coordination sphere of the Pb atom is completed by two oxygen atoms and one nitrogen atom of the same L ligand, two bridging chloride ions and two bridging oxygen atoms of two adjacent L ligands. Two PbII centers are linked by the two L ligands to form a C2-symmetric dimer unit with a planar [Pb2O2] ring. Each dimer unit acts as a secondary building unit(SBU) and links adjacent four dimer units by the chloride atoms and oxygen atoms of carboxylate groups of L, forming a two-dimensional array. Such two-dimensional layers are packed through intermolecular C–H···Cl hydrogen bonds into a three-dimensional supramolecular structure. When the dimer unit is viewed as a 4-connected node, 1 is simplified as a 4-nodal 2-D network with square lattices of the diagonal lengths to be 6.079(1). The fluorescence emission peak of complex 1 appears near 407 nm.     

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.