Synthesis and Crystal Structure of Bi（Hsal）3（1,10- phenanthroline） （Hsal = O2CC6H4-2-OH）

A new bismuth compound Bi（Hsal）3（1,10-phenanthroline） （Hsal = O2CC6H4-2-OH） has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1, with a = 10.243（2）, b = 11.905（3）, c = 12.934（3） A, α= 76.780（6）, β= 68.683（6）,γ= 80.930（7）°, V = 1425.6（5） A^3, Dc = 1.865 g/cm^3, Mr = 800.51, F（000） = 780, μ= 6.247 mm^-1, Z = 2, R = 0.0456 and wR = 0.1131 for 5612 observed reflections （I 〉 2σ（I））. In this compound, three salicylate ligands coordinate to the Bi atom through the carboxylate groups to form a four-membered chelate ring, and phenanthroline ligand chelates the metal through two N atoms. The structure of the title compound manifests a possible coordination mode between bismuth subsalicylate and N atom containing amino acid in the biological system.     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

Synthesis and Structural Characterization of [Cu(DMF)_6][(η~5-C_5Me_5)WS_3(CuBr)_3]_2·Et_2O

1 INTRODUCTION In the last decade, we have been interested in the synthesis of [PPh4][(h5-C5Me5)MS3] (M = Mo, W)[1, 2] , Whose organometallic trisulfido anions show high reactivity towards various transition metals[3~6] . We once reported that the reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CH3CN afforded a double incomplete-cubane cluster [PPh4]2[(h5-C5Me5)WS3(CuBr)3]2[3], while the analogous reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CHCl3 gave rise to a 揻our-…     

K3Eu5(PO4)6: hydrothermal synthesis,crystal structure and photoluminescence properties

An anhydrous orthophosphate, K₃Eu₅(PO₄)₆ (tripotassium pentaeuropium hexaphosphate), has been prepared by a high‐temperature solid‐state reaction combined with hydrothermal synthesis, and its crystal structure was determined by single‐crystal X‐ray diffraction analysis (SC‐XRD). The results show that the compound crystallizes in the monoclinic space group C2/c and the structure features a three‐dimensional framework of [Eu₅(PO₄)₆]_∞, with the tunnel filled by K⁺ ions. The IR spectrum, UV–Vis spectrum and luminescence properties of polycrystalline samples of K₃Eu₅(PO₄)₆, annealed at temperatures of 650, 700, 750, 800 and 850 °C, were investigated. Although with a full Eu³⁺ concentration (9.96 × 10²¹ ions cm^?3), the self‐activated phosphor K₃Eu₅(PO₄)₆ shows s strong luminescence emission intensity with a quantum yield of 37%. Under near‐UV light excitation (393 nm), the series of samples shows the characteristic emissions of Eu³⁺ ions in the visible region from 575 to 715 nm. The sample sintered at 800 °C gives the strongest emission and its lifetime sintered at 800 °C (1.88 ms) is also the longest of all.     

Studies on Selena-Macrocyclic Amides Synthesis and Structural Characterization of 7-Phenyl-5, 9-dioxo-1-selena-4, 7, 10-triazacyclododecane and 6-(4-Nitrobenzyl )-5, 9-dioxo-1, 4, 7, 10-selenatriazacyclododecane

lmTR0DUCTI0NSincetheseleniumcoronandswereachivevedin1989tli,thesynthesisandcoor-dinationchemistrystudyofthismacrocycliccomPOundshavereceivedwideattentionowingtotheirstrongcomplexingabilitiestowardssoft.transiti0nandheavymetals.InourprevibuspaPer,wereP0rtedthecrystalstructureoftw0selenacrownethers(2'3)andaPd(1)complexwith10'selenabenzo-15-crown-5t4i.Duetothedifficultyofthepreparationsofselenium-nitr0genmixeddonorc0n-..tainingmacrocycles,thestudyontheseligandsisconsiderablyscarce.Thesynthes…     

Electrochemical-hydrothermal Synthesis and Structural Characterization of Zn2(OH)VO4

A new zinc vanadate Zn₂(OH)VO₄ has been synthesized by an electrochemical-hydrothermal method and characterized by single crystal X-ray diffraction. The compound crystallizes in the orthorhombic system, space group Pnma, a = 14.645(1) Å, b = 6.0215(5) Å, c = 8.8757(8) Å, V = 782.7(1) ų, Z = 4, measured at 223 K. In the structure, rutile-type [ZnO₆] octahedral chains are interconnected by [VO₄] tetrahedra to form a framework of composition [Zn(OH)VO₄], the voids of which are filled by Zn cations with trigonal bipyramidal and octahedral coordination. The structure is closely related to that of the adamite-type phases and the minerals descloizite PbZn(OH)VO₄ and tsumcorite Pb_0.5Zn(H₂O)AsO₄.     

7,7-二甲基-2-对溴苯基-4-苯基-5-氧代-1,4,5,6,7,8-六氢化-6H-喹啉的合成及晶体结构

标题化合物C23H22BrNO是由1-(4-溴苯基)-3-苯基-2-丙烯-1-酮与5,5-二甲基-1, 3-环己二酮在N, N-二甲基甲酰胺(DMF)中在NH4OAc催化下反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群C2/C, a = 19.678(4),b = 13.571(2),c = 17.311(3) 牛琤 = 118.74(1),Mr = 408.33, V = 4055(1) ?,Dc = 1.338 g/cm3, Z = 8, m (MoKa) = 2.038 mm-1, F(000) = 1680, R = 0.0539,wR = 0.1369。X-衍射分析表明,六元环C(10)C(13)C(16)C(17)采用半椅式构象:原子C(10),C(11),C(12),C(16)和C(17)在同一个平面内,而原子C(13)远离平面为0.3282 牛闷矫嬗?个苯环的夹角分别为41.09, 81.97,2个苯环的夹角为75.87。另外在晶体结构中,存在1个分子间氢键。     

Synthesis and Structure Characterization of Mn2（CO）6（μ—S2CP^iPr3）

1INTRODUCTIONThechemistryofhomobinuclearcomplexeshasbeenaveryactivefieldofresearchinthepastdecadesbecauseoftheirnovelstructuresandapplicationsinorganicsynthesis[1,2].Atthesametimephosphine-carbondisulfideadducts,S2CPR3,areveryversatileligandswithavarietyofcoo-rdinationmodestotransitionmetalcenters.Itisabletoformallydonatefrom2to8etoametalormetals[3].AlthoughMn2(CO)6(m-S2CPiPr3)hasbeensynthesizedbyMiguelD.etal.[4,5],nocrystallo-graphicdatatillnowareavailableforit.Inthispaperwewilldesc…     

MZr2（AsO4）3（M=Na,K,Rb,Cs）的水热合成与结构表征

用水热晶化法合成了MZr_2(ASO_4)_3(M=Na,K,Rb,Cs)系列化合物。研究了反应物浓度、配比及不同砷源等水热晶化条件对产物物相的影响。用XRD、IR和Raman光谱对产物进行了表征。4种晶体的振动光谱由钠到铯呈现出规律性变化。     

层状MAgTeS3 (M＝K, Rb)的溶剂热合成与表征

以硫醇为螯合剂, 在溶剂热条件下合成了两种层状硫代亚碲酸盐KAgTeS₃ (1)和RbAgTeS₃ (2). X射线单晶解析表明, 1和2是类质同晶化合物. 在晶体结构中, 银硫四面体通过共用顶点形成无限的平行链, 在相邻链中银硫四面体取向相反, 这些链与链由三角锥配位的碲互相连接形成阴离子层状结构, 阳离子在阴离子层间. 1的结晶学数据为: M_r＝370.75, P2₁/c, a＝0.73639(6) nm, b＝1.06468(8) nm, c＝0.85203(6) nm, β＝106.4640(10)°, V＝0.64062(8) nm³, Z＝4, R(F)＝4.44%, wR(F²)＝11.66%. 2的结晶学数据: M_r＝417.12, P2₁/c, a＝0.75531(12) nm, b＝1.07076(7) nm, c＝0.8583(2) nm, β＝106.497(6)°, V＝0.66558(19) nm³, Z＝4, R(F)＝6.00%, wR(F²)＝15.43%. DSC及紫外-可见漫反射光谱研究表明, 这两种化合物为半导体, 并具有很好的热稳定性.     

铋(Ⅲ)四氢吡咯氨荒酸配合物[Bi(S2CNC4H8)3]2的合成和晶体结构

The novel bismuth(Ⅲ) complex with dithiotetrahydropyrrolocarbamate, [Bi(S₂CNC₄H₈)₃]₂ has been synthe-sized. The crystal structure has been determined by X-ray single crystal diffraction. The crystal belongs to mono-clinic with space group C2/c, a=1.6356(9) nm, b=1.1875(6) nm, c=2.3954(13) nm, β=100.741(8)°, Z=4, V=4.571(4) nm³, D_x=1.882g·cm^-3,μ=8.267mm^-1, F(000)=2512, R=0.0404, wR=0.0622. In this binuclear complex, each Bi(Ⅲ) is seven coordinate with a distorted pentagonal bipyramidal geometry. CCDC: 179924.     

3,3,6,6-四甲基-9-邻氯苯基-1,8-二氧代-3,4,5,6,7,9-六氧化氧杂蒽的合成和晶体结构

标题化合物C23H25对O3Cl是由邻氯苯甲醛与5，5-二甲基1，3-环己二酮在N，N-二甲基甲酸腹中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单科晶系，空间群=1632。晶体结构用直接法解出，使用全矩阵最小二乘法对原子参数进行修正，最后的偏离因子为R=0．054，Rw一0．063。在晶体结构中，吡喃环与苯环之间的两面角为92．43°。     

Synthesis and Structure of 4，5－bis（2，4－Dinitrophenylthio）－1，3－Dithiole－2－Thione

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ４，５－ｂｉｓ（２，４－Ｄｉｎｉｔｒｏｐｈｅｎｙｌｔｈｉｏ）－１，３－Ｄｉｔｈｉｏｌｅ－２－ＴｈｉｏｎｅＱｕＺｈｅｎｇ；ＣａｉＪｉｎｇ－Ｈｕａ；ＦａｎｇＱｉ；ＹｏｕＸｉａｏ－Ｚｅｎｇ（Ｃｏｏｒｄｉｎａｔｉ...     

Synthesis and Structural Characterization of Pd[CH3O（O）C6H3CHNNC（S）NH2]（C5H5N）

1 INTRODUCTION Palladium (Ⅱ) coordination and organometallic compounds usually show square planar environments at the metal center[1], and have experienced an im- portant development in the past years due to their acting as intermediates in different types of catalytic reactions and numerous applications in organic synthesis[2]. Although palladium plays an increase- ingly recognized role as a biometal[3], little is known about the structure and function of palladium compounds in living …     

3,3,6,6-四甲基-4a-羟基-9-邻甲氧基苯基-1,8-二氧代-2,3,4,4a,5,6,7,8,9,9a-十氢化-1H-氧杂蒽的合成和晶体结构

标题化合物C24H30O5是由邻甲氧基苯甲醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单斜晶系，空间群C2／c，a=33．942（6），b=7273（1），c=22667（4）A，β=128．989（9）°，Mr=398．50，V=4349（1）A3，Dc=1．2179·cm-3，Z=8，μ（MoKa）=840mm－1，F（000）=1712。晶体结构用直接法解出，经用全矩阵最小二乘法对原子参数进行修正，最后的偏离因子为R=0.043，Rw=0．052。在晶体结构中，存在一个分子间氢键。     

Synthesis and Crystal Structure of the Mixed-quadriligand Bismuth Complex [Bi(S_2CNEt_2)_2(NO_3)]·[1,10-Phen]

1 INTRODUCTION Some reports on the syntheses and crystal struc-tures of organotin(IV) dithiocarbamate complexes haveappeared in the previous literatures[1～3], but the bis-muth(Ⅲ) complexes with dithiocarbamate have beenscarcely studied[4]. Due to the n…     

Synthesis,Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(IV) Complex with 5-Bromonicotinic Acid

1 INTRODUCTION Organotin esters of carboxylic acids are widely used as biocides, fungicides and homogeneous ca- talysts in industry[1～3]. Recently, pharmaceutical pro- perties of organotin esters of carboxylic acids have been investigated for their antitumour activity[4, 5]. Studies on organotin compounds containing car- boxylate ligands with additional donor atoms (e.g. N, O or S) that are available for coordination to the tin atom have revealed that new structural types may lead to di…     

Synthesis,Crystal Structure,and Characterization of Na7Cu4(AsO4)5

Abstract

Sodium copper (II) arsenate Na₇Cu₄(AsO₄)₅ has been grown by conventional high-temperature, solid-state methods in molten-salt media. It was characterized by single crystal X-ray diffraction (XRD), thermal analysis (DTA–TGA), scanning electron microscopy (SEM), semiquantitative energy dispersive spectroscopy analysis (EDS), and vibrational spectroscopy. Na₇Cu₄(AsO₄)₅ exhibits a three-dimensional framework built up of CuO₅, CuO₄, and AsO₄ polyhedra, with intersecting channels in which the Na⁺ cations are located. The three-dimensional cohesion of the framework results from Cu–O–As bridges. CuO₅ and CuO₄ polyhedra are elongated due to the Jahn–Teller effect, whereas AsO₄ tetrahedra are almost regular. This new structural model is validated by the charge distribution (CD) analysis. The infrared and Raman spectra confirmed the presence of AsO₄ tetrahedra.

[Supplementary materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfer, and Silicon and the Related Elements for the following free supplemental files: Additional tables and figures.]     

Crystallographic report: Bi(S2CNC5H10)2(NO3)(1,10‐phenanthroline)

The structure of Bi(S₂CNC₅H₁₀)₂(NO₃)(1,10‐Phen) features an eight‐coordinated distorted square antiprismatic geometry around bismuth, defined by an N₂O₂S₄ donor set, with Bi? S distances ranging from 2.641(2) to 2.824(2) Å. Copyright © 2004 John Wiley & Sons, Ltd.     

BiVO_4/Bi_6O_6(OH)_3(NO_3)_3复合光催化剂的制备及光催化性能研究

以Bi(NO_3)_3·5H_2O和NH_4VO_3为原料,控制水溶液介质p H及反应时间,采用水热合成法制备钒酸铋(BiVO_4)及其复合物(BiVO_4/Bi_6O_6(OH)_3(NO_3)_3).利用X-射线粉末衍射、扫描电子显微镜和紫外-可见漫反射吸收光谱等手段对制备的样品进行了物理表征,结果表明,在控制反应时间为1 h,介质p H值在1.14~9.01之间时,制备的样品为BiVO_4/Bi_6O_6(OH)_3(NO_3)_3复合物,当p H值增加至10.92时为纯BiVO_4;控制介质p H为7.17,反应时间在1~12 h之间时得到BiVO_4/Bi_6O_6(OH)_3(NO_3)_3复合光催化剂,反应时间为18 h时为纯BiVO_4.在可见光(λ≥400 nm)照射下,以有机染料罗丹明B(Rhodamine B,Rh B)为底物,研究不同条件制备的BiVO_4或者复合物为光催化剂的光催化特性,发现p H=7.17,水热反应12 h得到的催化剂(BiVO_4/Bi_6O_6(OH)_3(NO_3)_3)光催化降解活性高于对照制备的纯BiVO_4.同时在可见光照射下,BiVO_4/Bi_6O_6(OH)_3(NO_3)_3亦可以有效降解无色小分子2,4-二氯苯酚(2,4-Dichlorophenol,2,4-DCP),说明氧化过程涉及到光催化过程.分析BiVO_4/Bi_6O_6(OH)_3(NO_3)_3复合光催化剂对Rh B光催化降解过程中活性物种,表明在降解过程中主要涉及空穴和超氧氧化,O_2·~-起主要作用.