Crystal Structure and Thermal Decomposition Mechanism of [K（DNP）（H2O）0.5]n

Introduction As developing high-energy, low toxicity and envi-ronment friendly primary explosive has been becoming a new and important investigation field, much attention has been paid to nitrogen-rich potassium coordination compounds for the sake of their low toxicity and little pollutions.1-11 In order to make good use of potassium compounds, the reaction of 2,4-dinitrophenol (DNP) and potassium hydroxide was designed, and the title compound potassium 2,4-dinitrophenate (KDNP) was obtained…     

Synthesis and Crystal Structure of a Two-dimensional Coordination Polymer [Cd（dym）（H2O）2（H2O）]n with Cd6 Hexagonal Macrometallocycle

1 INTRODUCTION The investigation of coordination polymers has rapidly been expanded in last decade owing to their potential applications such as catalysis, molecular absorption, non-linear and magnetic materials. Among the varieties of such coordination polymers, the po- lymers of cadmium with dicarboxylates having fas- cinating structural topologies and good photolumi- nescence constitute a new family. Many reports are concerned about cadmium dicarboxylate polymers with 1D helix structu…     

Interactions with ATP, DNA Cleavage and Anti-tumor Activities of Complexes with Anions [Mo（V）O2（O2CeH4）2]^3-, [Mo（Ⅴ）0.5W（Ⅵ）0.5O2（O2C6H4）2]^2.5- and [W（Ⅵ）O2（O2C6H4）2]^2-

(NH3CH2CH2NH2)3[Mo(Ⅴ)O2(O2C6H4)2] (1), (NH3CH2CH2NH2)2.5[Mo(Ⅴ)o.sW(Ⅵ)o.502(O2C6H4)2] (2) and(NH3CH2CH2NH2)2[VC(Ⅵ)O2(O2C6H4)2] (3) were synthesized, structurally characterized by X-ray diffraction analysis, and studied on their interactions with ATP, their DNA cleavage activities and antitumor properties. The redox state of molybdenum was not changed on going from crystal to aqueous solutions in complexes 1 and 2, while tungsten underwent reduction from W(VI) to W(V) in complexes 2 and 3. ATP promoted the oxidation of both molybdenum and tungsten from M(Ⅴ) to M(Ⅵ) and the hydrolysis of catecholate ligands in solution consisting of ATP and the complexes. Complex 1 possesses fairly good activity to DNA cleavage and against tumor S180 in mice, and is more effective than the control drug cyclophosphamide under the identical conditions. However, complexes 2 and 3 exhibited marginal effectiveness. The effectiveness of anti-tumor of the complexes was related positively to their DNA cleavage activities and their hydrolysis of catecholate ligands.     

Crystal Structure of Hydrochlorate of 1,1＇-Bis[（4-pyridylamino）carbonyl]ferrocene

The hydrochlorate of 1,1?-bis[(4-pyridylamino)carbonyl]ferrocene (C23H23O3N4ClFe, Mr = 494.75) was structurally characterized by means of X-ray single-crystal diffraction. It crystallizes in triclinic, space group P1 with a = 9.5299(19), b = 12.792(3), c = 9.2644(19) ?, α = 91.56(3), β = 101.97(3), γ = 74.71(3)°, V = 1065.2(4) ?3, Z = 2, Dc = 1.542 g/cm3, F(000) = 512, μ(MoKα) = 0.868 mm-1, T = 291(2) K, the final R = 0.0596 and wR = 0.1531 for 2842 observed reflections with I > 2σ(I). Interestingly, two 1,1?- bis[(4-pyridylamino)carbonyl]ferrocenes (4-BPFA) join shoulder-to-shoulder through intermolecular hydrogen bonds N–H…N, forming an unexpected macrocycle with dimensions of 3.385 ? × 15.778 ?.     

Synthesis and Crystal Structure of Drum Organooxotin Clusters from Heteroaromatic Carboxylic Acid [PhCH2Sn（O）（O2CC5H4N）]6 and[PhCh2Sn）（O）（O2CC4H3O）]6

IntroductionRecentlywehaveinvestigatedthestructuralchemistryofanumberofdi ortri organotinheteroaromaticcarboxyl ates.1 5Thesestudieshaveshownthatthestructureoforgan otinheteroaromaticcarboxylatesisdependentonboththena tureofthealkylorarylsubstituentboundtothetinatomandthetypeofcarboxylateligand .Inparticular,majorstructuralvariationsareobservedwhencarboxylateligandcontainsanadditionaldonoratom ,suchasapyridineNatom ,availableforcoordinationtotheSnatom .1 3,5 8Wehavenowturnedtothemonoorganotin…     

Crystal Structure of Bis (O,O’-diisopropyl dithiophosphate):[(C3H7O)2PS2]2

The crystal and molecular structures of [(C3H7O)2PS2]2 (CCDC No. 217201) were determined by means of X-ray crystallography. It crystallized in a triclinic system with space group P(-1) and lattice parameters a=0.82794(3) nm, b=0.84764(2) nm, c=0.85034(3) nm, α=97.78(3)°, β=110.77(3)°, γ= 94. 95 (3)°,V= 0. 54701(9) nm3, Z= 1. In this molecule, the two diisopropyl dithiophosphate groups, [(C3H7O)2PS2]2,which are parallel to each other, are linked by an S-S bond and there exist inversion centers in the molecule.In the structure, the P = S bonds in the two dithiophosphate units are trans-oriented to each other.     

In[(C2H5O)2PS2]3配合物的合成及晶体结构研究

稀散元素材料已成为当代高新技术领域的重要支撑材料,其中铟应用于液晶材料(ITO)的研究与开发^[1,2].烷基二硫代磷酸酯具有优良的配位性能,可用作石油添加剂和高聚物防老化剂^[3,4].因此,目前对稀散元素烷基硫代配合物研究十分活跃.     

Crystal Structure and Luminescence of a Europium Coordination Polymer {[Eu(p-MOBA)_3·2H_2O]·0.5H_2O· 0.5(4,4′-bipy)}_∞

ＩｎｔｒｏｄｕｃｔｉｏｎＭｏｎｏｎｕｃｌｅａｒ ,ｄｉｎｕｃｌｅａｒａｎｄｐｏｌｙｍｅｒｉｃｔｙｐｅｓｏｆｃｒｙｓ ｔａｌｓｔｒｕｃｔｕｒｅｓｆｏｒｌａｎｔｈａｎｉｄｅｃｏｍｐｌｅｘｅｓｗｉｔｈｂｅｎｚｏｉｃａｃｉｄａｎｄｉｔｓｄｅｒｉｖａｔｉｖｅｓｈａｖｅｂｅｅｎｏｂｔａｉｎｅｄｂｅｃａｕｓｅｏｆｔｈｅｖａｒｉ ａｔｉｏｎｏｆｂｒｉｄｇｉｎｇｆｏｒｍｓｆｏｒｃａｒｂｏｘｙｌａｔｅｇｒｏｕｐａｎｄｃｏｏｒｄｉｎａ ｔｉｏｎａｂｉｌｉｔｙｏｆｄｉａｍｍｉｎｅｌｉｇａｎｄｓ ,ｓｕｃｈａｓ 1,10 ｐｈｅｎａ…     

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）2]

Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).     

三环己基锡O，O＇－二（4－氯苯基）二硫代磷酸酯和二丁基锡双［O，O＇－二（4－甲基苯基）二硫代磷酸酯］的分子和晶体结构

三环己基锡Ｏ，Ｏ＇－二（４－氯苯基）二硫代磷酸酯（Ⅰ），Ｃ＿（３０）Ｈ＿（４１）Ｃｌ＿２Ｏ＿２ＰＳ＿２Ｓｎ，Ｍ＿ｒ＝７１８．３６，单斜晶系，Ｐ２＿１／ｎ，ａ＝１６．１５１（２），ｂ＝９．４１５（１），ｃ＝２２．９８７（３），β＝１０５．６９（１）°，Ｚ＝４，Ｄｃ＝１．４１８ｇ·ｃｍ￣（－３），Ｒ＝０．０６３；二丁基锡双［Ｏ，Ｏ＇－二（４－甲基苯基）二硫代磷酸酯］（Ⅱ），Ｃ＿（３６）Ｈ＿（４６）Ｏ＿４Ｐ＿２Ｓ＿４Ｓｎ，Ｍ＿ｒ＝８５１．６６，单斜晶系，Ｐ２＿１／ｃ，ａ＝１２．２８４（４），ｂ＝９．８０７（１），ｃ＝３４．４７１（８），β＝９９．０２（２）°，Ｚ＝４，Ｄ＿ｃ＝１．３７９ｇ·ｃｍ（－３），Ｒ＝０．０４２。化合物Ⅰ具有单分子的四配位变形四面体结构。其Ｓｎ－Ｓ（１）键长为２．５０１（２）；而Ｓｎ与Ｓ（２）的原子间距则为３．５９７；化合物Ⅱ具有单分子的六配位变形八面体结构，其Ｓｎ－Ｓ（１），Ｓｎ－Ｓ（２），Ｓｎ－Ｓ（３）和Ｓｎ－Ｓ（４）的键长分别为２．４９５（３），２．４９３（２），３．２４４（４）和３．２２８（３）。     

配合物Nd(C7H7N2O2)3(H2O)3的合成及其晶体结构

用水热法合成了3,5-二氨基苯甲酸与Nd(Ⅲ)的配合物Nd(C7H7N2O2)3(H2O)3(1),其结构经IR,元素分析和X-射线单晶衍射仪表征。1为单核结构,属六方晶系,R3空间群,晶胞参数:a=1.887 29(18)nm,b=1.887 29(18)nm,c=0.603 53(12)nm,β=90,°γ=120°,V=1.861 7(4)nm3,Z=3,μ=2.154 mm-1,Dc=1.744 g.cm-3,R1=0.014 3,wR2=0.033 2。1中Nd(Ⅲ)与来自3个3,5-二氨基苯甲酸的6个氧原子及3个配位水的氧原子进行配位,形成9配位化合物。     

Synthesis,Crystal Structure,and NMR Spectroscopy of a New P-Phenylenediamonium Diphosphate [p-NH3C6H4NH3]H2P2O7

Crystal growth and characterization by X-ray diffraction and NMR spectroscopy of a new p-phenylenediamonium diphosphate [p-NH₃ C ₆ H ₄ NH ₃]H ₂ P ₂ O ₇ are reported. This compound crystallizes in a triclinic unit cell P1 with the parameters a = 7.130(3), b = 9.047(3), c = 9.350(2) Å, α = 133.44(2)°, β = 95.02(2)°, γ = 107.11(4)°, Z = 2, V = 514.3(15) ų, and D _x = 1.848 g.cm^{? 3}. The crystal structure has been solved and refined to R = 0.0273, using 3678 independent reflections. The atomic arrangement is build up by infinite ribbons of [H₂ P ₂ O ₇] ^2? anions, extending along the a-direction at y = 1/2. Between these ribbons are located the p-phenylenediammonium entities, which form hydrogen bonds N─H…O with some external oxygen atoms of phosphoric groups. Crystallographic results are correlated with that of the solid state ¹³C and ³¹P MAS NMR spectroscopy.     

Xenon Trioxide Adducts of O-Donor Ligands; [(CH3)2CO]3XeO3, [(CH3)2SO]3(XeO3)2, (C5H5NO)3(XeO3)2, and [(C6H5)3PO]2XeO3

Xenon trioxide (XeO₃) forms adducts with triphenylphosphine oxide, dimethylsulfoxide, pyridine-N-oxide, and acetone by coordination of the ligand oxygen atoms to the Xe^VI atom of XeO₃. The crystalline adducts were characterized by low-temperature, single-crystal X-ray diffraction, and Raman spectroscopy. Unlike solid XeO₃, which detonates when mechanically or thermally shocked, solid (C₅H₅NO)₃(XeO₃)₂, [(C₆H₅)₃PO]₂XeO₃, and [(CH₃)₂SO]₃(XeO₃)₂ are insensitive to mechanical shock. The [(CH₃)₂SO]₃(XeO₃)₂ adduct slowly decomposes over several days to (CH₃)₂SO₂, Xe, and O₂. All three complexes undergo rapid deflagration when ignited by a flame. Both [(C₆H₅)₃PO]₂XeO₃ and (C₅H₅NO)₃(XeO₃)₂ are room-temperature stable and the [(CH₃)₂CO]₃XeO₃ complex dissociates at room temperature to form a stable solution of XeO₃ in acetone. The xenon coordination sphere of [(C₆H₅)₃PO]₂XeO₃, a distorted square-pyramid, provides the first example of a five-coordinate XeO₃ complex with only two Xe- - -O adduct bonds. The xenon coordination spheres of the remaining adducts are distorted octahedra, comprised of three Xe- - -O secondary bonds that are approximately trans to the primary Xe−O bonds of XeO₃. Quantum-chemical calculations were used to assess the nature of the Xe- - -O adduct bonds, which are described as predominantly electrostatic bonds between the nucleophilic oxygen atoms of the bases and the σ-holes of the electrophilic xenon atoms.