Crystal structures of acid ethylenediaminetetraacetates [Cd(H2 Edta)(H2O)] · 2H2O and [Mn(H2O)4][Mn(HEdta)(H2O)]2 · 4H2O

The crystal structures of [Cd(H₂ Edta)(H₂O)] · 2H₂O (I) and [Mn(H₂O)₄][Mn(HEdta)(H₂O)]₂ · 4H₂O (II) are studied by X-ray diffraction [R ₁ = 0.0209 (0.0272), wR ₂ = 0.0571 (0.0730) for 2551 (4025) reflections with I > 2σ(I) in I (II), respectively]. Structure I contains mononuclear [Cd(H₂ Edta)(H₂O)] complexes with the C ₂ symmetry, and structure II contains centrosymmetric trinuclear [Mn(H₂O)₄][Mn(HEdta)(H₂O)]₂ complexes. In I and II, the protonated ligands are hexadentate (2N + 4O), and the water molecule increases the coordination number of the metal atom to seven. The acid protons participate in short intermolecular hydrogen bonds, which are symmetric in II and asymmetric in I.     

BaBPO5和(H3O)Zn(H2O)2BP2O8·H2O的低温溶剂热合成及表征

以乙醇为溶剂,在低温条件下合成出了两种手性硼磷酸盐化合物BaBPO5(1)(T=120℃,t=5d)和(H3O)Zn(H2O)2BP2O8·H2O (2)(T=80℃,t=5d).XRD单晶衍射仪测定了化合物的结构,结果表明:(1)属三方晶系,P3221空间群,a=b=7.1162(3)(A),c=6.9979(6),(A)=3,该晶体含有一维线性链状阴离子结构;(2)属六方晶系,P6122空间群,a=b =9.513(2)(A),c=15.906(8),(A)=6.该晶体具有三维骨架结构.实验结果表明使用乙醇作溶剂可以极大降低硼磷酸盐的合成温度,进而有助于获得手性硼磷酸盐化合物,这为手性硼磷酸盐的合成提供了一种新思路.     

[Co(H2O)6](C18H15O4SO3)2·4H2O的合成和晶体结构

以芒柄花素为先导化合物,合成了水溶性的[Co(H2O)6](C18H15O4SO3)2·4H2O,并采用IR, 1H NMR, TG-DTA, XRD和单晶X射线衍射法对其结构进行了表征.单晶X射线衍射结果表明:[Co(H2O)6]2+、C18H15O4SO 3和H2O之间存在多种氢键,形成晶体结构中的亲水区.异黄酮骨架间反平行排列,面对面和边对面芳香堆积作用同时存在于其中,构成晶体结构中的疏水区.磺酸根是连接亲水区和疏水区的桥梁.氢键、芳香堆积作用以及阴阳离子之间的静电引力共同将标题化合物组装成具有三维网络结构的超分子.     

Synthesis and crystal structure of [Ni(H2O)6](C19H17O9S)2·2H2O

A water soluble flavonoid sulfate, [Ni(H₂O)₆](C₁₉H₁₇O₉S)₂·2H₂O was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. The crystal of it belongs to triclinic crystal system, space group P–1. The results show that the title compound consists of [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and H₂O. Ni(II) is located on the symmetry center and octahedrally coordinated by six water molecules. A variety of hydrogen bonds among [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and the lattice water molecules build a hydrophilic region. Aromatic π–π stacking interactions assemble isoflavone skeletons into a column and the columns form a hydrophobic region of the title compound. The sulfo-groups bridge the hydrophilic regions and the hydrophobic regions as well as the inorganic components and organic components. Hydrogen bonds, stacking interactions and the electrostatic interactions between cation [Ni(H₂O)₆]²⁺ and anion sulfonate C₁₉H₁₇O₆SO₃ ⁻ lead the moieties to a three-dimensional structure.     

Structure of progesterone hydroquinone monohydrate (1∶1∶1), C21H30O2·C6H6O2·H2O

The crystal structure of progesterone hydroquinone monohydrate was determined by means of X-ray diffraction methods:M _r=442.6, orthorhombic,P2₁2₁2₁,a=14.680(2),b=22.725(3),c=7.334(1) Å,V _a=2446.6(6) ų,Z=4,D _x=1.190 M gm^–3, MoK radiation ,(MoK)=0.75 cm^–1,F(000)=948. The structure was solved usingMultan;R=0.059,R _w=0.059 for 2736 reflections. This progesterone molecule has the most flattenedA ring, relative to the rest of the skeleton, of all progesterone molecules studied so far. Steroid, hydroquinone, and water molecules form, by means of hydrogen bonds, two parallel chains connected with each other by hydrogen bonds.The authors thank Dr. A. Szyczewski for supplying crystals. This research was supported by the project RP.II.10 from the Polish Ministry of National Education and by PHS Grant No. DK26546.     

Structure of 17α-methyl-testosterone semihydrate,C20H30O2·1/2 H2O

The crystal structure of 17-methyltestosterone hemihydrate, C₂₀H₃₀O₂·1/2H₂O, has been determined:M _r =312.5, space groupP2₁2₁2₁2₁,a=6.374(2),b=12.807(2),c=43.398(5)Å,V _c =3543(2)ų,Z=8,D _x =1.172 mg^–3, CuK radiation ( = 1.54184 Å),(CuK)=5.5 cm^–1,F(000)=1376. The structure was solved usingMultan. The final conventionalR=0.053 (R _w =0.052) for 3634 reflections. The structure contains two crystallographically independent molecules in the asymmetric part of the unit cell that have almost identical geometry.     

Structure of 17β-hydroxy-1,4-androstadien-3-one monohydrate C19H26O2·H2O

The structure of the title compound, C₁₉H₂₆O₂·H₂O, was determined by X-rays.M _r=304.4, space groupP2₁,a=10.3113(6),b=10.3978(21),c=7.8710(9) Å, =89.527(9)°,V _c=844(1) ų,Z=2,D _x=1.194 Mg m^–3. CuK radiation ,(CuK)=5.9 cm^–,F(000)=332. FinalR factor=0.046 (R _w=0.047) for 1002 unique reflections. The structure was solved usingMultan. The water molecule is the hydrogen donor to O(3) and a hydrogen acceptor from the O(17) hydroxyl group. RingA is rather flat relative to the rest of the steroid backbone and the O(3)-plane distance is 1.99 Å.     

Preparation and X-ray structure of [H3O+·18-crown-6]-[(H5O 2 + )(Cl−)2], a compound containing both H3O+ and H5O 2 + crystallized from aromatic solution

The title compound was synthesized by the reaction of [H₃O⁺·18-crown-6][Cl-H-Cl^–]·3.8 C₆H₅Me with two equivalents of H₂O. Colorless crystals, which slowly deposited from the corresponding liquid clathrate, belong to the monoclinic space group P2₁/n witha=10.648(6),b=9.571(2),c=20.801(6) Å,=98.67(5)°, andD _c=1.24 g cm^–3 forZ=4. Refinement based on 1609 observed reflections led to a finalR value of 0.072. In the crystal structure the [H₃O⁺·18-crown-6]⁺ cations are packed in layers separated by puckered sheets of [(H₅O ₂ ⁺ )(Cl^–)₂]^–.     

CoC2O4·2H2O纳米晶形貌可控合成

通过简单调节反应介质热塑性酚醛树脂与乙二醇配比,选择性地制备了CoC2O4·2H2O纳米棒和纳米片晶体或其两种形貌晶体混合物.样品热重和差示扫描量热(TG-DSC)、X射线粉体衍射(XRD)、场发射扫描电镜( FESEM)实验表明:以热塑性酚醛树脂为反应介质得到了COC2O4·2H2O纳米棒;以乙二醇为反应介质得到了CoC2O4·2H2O纳米片;逐渐增大乙二醇和酚醛树脂质量比,实现了CoC2O4·2H2O形貌由纳米棒形貌转变为纳米片形貌.基于不同晶体形貌和实验结果,提出了棒状和片状COC2O4·2H2O可能的形成机理模型以解释两种形貌COC2O4·2H2O纳米晶的生长行为.     

Structure of 6β-hydroxy-4-androsten-3,17-dione monohydrate,C19H27O3·H2O

The structure of the title compound was determined by X-rays:M _r =319.4,P2₁2₁2₁,a=7.753(3),b=10.566(8),c=20.997(10) Å,Z=4 andD _x =1.171 M gm^–3. FinalR=0.042 (R _w =0.041) for 1814 unique reflections. The water molecule is the hydrogen donor to O3 and O17 and an hydrogen acceptor from the O17 hydroxyl group.     

[Mn(H2O)6][Bi(edta)2.2H2O的合成与晶体结构

以MnCO3与多胺羧酸铋反应,合成了含铋多金属配合物[Mn(H2O)6][Bi(edta)]2.2H2O,通过元素分析和红外光谱对配合物的组成和结构进行了表征.用热重-差热手段研究了配合物的热分解过程,用x射线单晶衍射法测定了其晶体结构.[Mn(H2O)6][Bi(edta)]2·2H2O属单斜晶系,C2/c空间群,晶胞参数:a=2.37013(4)nm,b=0.87111(2)nm,c=1.61082(3)nm,β=97.273(1).,Z=4,Mr=1193.46,V=3.299.01(11)nm3,Dc=2.403g.cm-3,μ=11.123mm-1,F(000)=2284,R1=:0.0210,wR2=0.0567.大量分子间氢键将整个连接起来形成无限3-D结构.     

水热合成三维超分子配位聚合物[Cd(C2O4)(H2O)2]·H2O及晶体结构

在水热条件下,制备了二维层状配位聚合物 [Cd(C2O4)(H2O)2] ·H2O(1)的单晶体,对其进行了X射线粉末衍射、元素分析、红外光谱、热重分析和X射线单晶衍射测定.单晶结构分析表明,该晶体属于三斜晶系,P-1空间群,晶胞参数a=0.60109(12)nm, b=0.66607(13)nm,c=0.84987(17)nm,α=74.72(3)°,β=74.33(3)°,γ=81.07(3)°,V=0.31473(11)nm3,Z=2,R1=0.015,ωR2=0.0368.草酸镉单晶结构由两个2D层构成,每一个2D层是由[Cd2(C2O4)2(H2O)4]·2H2O的重复单元形成,每个单元是由一个七配位独立镉原子配位而成(五个草酸氧原子和两个水分子氧原子).2D层与层之间通过不同层草酸分子与配位水分子之间及草酸与客体水分子之间形成的氢键将2D层状化合物连成一个3D超分子结构.热重分析表明该配位聚合物在340℃下稳定.     

[Gd(BMBCP)(H2O)4][PMo12O40]·2.75H2O配位聚合物的合成及表征

以-Keggin型多金属氧酸盐[PMo12O40]3-作为模板,采用水热法成功合成一例新型二维Gd(Ⅲ)配位聚合物[Gd(BMBCP)(H2O)4][PMo12O40]·2.75H2O (HNU-13) (H2BMBCP·Cl2=1,4-双(3-羧酸吡啶基-1-亚甲基)苯二氯).通过单晶X-射线衍射仪确定其结构,并通过X-射线粉末衍射 (PXRD),傅里叶红外光谱 (IR)和热重分析仪(TG)对其进行表征.结果表明,化合物结构结晶于单斜晶系,P2(1)/n空间群,晶胞参数为a =1.4291 nm ,b=1.3772 nm,c=2.8430 nm,α=90.00°,β =91.154°, γ=90.00°,Z =4.值得注意的是,由于[PMo12O40]3-与H2BMBCP·Cl2配体的静电作用,从而形成左右手螺旋链,进一步的构筑为层状4,4-网格结构.     

Synthesis and crystal structure of hexaaquamagnesium hydrogen phosphododecatungstate tetrahydrate [Mg(H2O)6][HPW12O40]·4H2O

Crystals suitable for X-ray structure analysis were obtained after the slow evaporation of the reaction mixture containing equimolar quantities of magnesium chloride and dodecatungstophosphoric acid aqueous solution insuring pH of the solution between 1.0 and 1.2. This simple synthetic route yielded stability of Keggin anion and high quality [Mg(H₂O)₆][HPW₁₂O₄₀]·4H₂O single crystals. The obtained compound belongs to the group of heteropoly compounds and its structure is composed of Keggin [PW₁₂O₄₀]^3– anions, [Mg(H₂O)₆]²⁺ cations and lattice water molecules. Zigzag arrangement of Keggin anions along c-axis creates irregular channels occupied by [Mg(H₂O)₆]²⁺ cations and lattice H₂O molecules. The calculation of the total potential solvent volume indicated the presence of 4.1 lattice H₂O lattice molecules per formula unit, which is in agreement with the here presented structural model. The position of one lattice water molecule is well defined, while each of three other molecules is statistically distributed over two locations. Hydrogen bonds involve all coordinated and lattice H₂O molecules, as well as some oxygen atoms from the Keggin anion. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Metal-hydroxycarboxylate interactions: syntheses and structures of K2[VO2(C6H6O7)]2·4H2O and (NH4)2[VO2(C6H6O7)]2·2H2O

Potassium and ammonium dimeric (citrato)dioxovanadium(V) hydrate K₂[VO₂(H₂cit)]₂·4H₂O1 and (NH₄)₂[VO₂(H₂cit)]₂·2H₂O2 (H₄cit=citric acid) have been prepared and characterized by X-ray structure analyses. Vanadate1 crystallizes in the monoclinic space groupP2₁/n (No. 14) with unit cell parameters:a=9.304(2),b=11.756(2),c=11.911(2)Å, =111.72(3)°, andD _c=1.911 g/cm³,Z=2; Vanadate2 also crystallizes in the monoclinic space groupP2₁/n with unit cell parameters:a=9.719(2),b=11.111(3),c=11.294(2)Å, =109.03(2)°, andD _c=1.781 g/cm³,Z=2. Each dimer contains a centro-symmetric planar four-member V₂O₂ ring with two exocyclic citrate entities coordinated by the oxygen atoms of the hydroxy-and -carboxylate ligands, while the other two -carboxylate groups remain uncomplexed. Principal dimensions of the V–O bonds are 1.986(4)_av (hydroxy) and 1.980(3)Å(-carboxyl) for vanadate1, 1.988(2)_av (hydroxy) and 1.974(3)Å(-carboxyl) for vanadate2.     

Crystal structure and hydrogen-bonding system of cholic acid hemihydrate,C24H40O5·1/2H2O

Crystals of the hemihydrate of this bile acid are hexagonal, space groupP6₅22, a=b=13.736(8)Å,c=85.06(6)Å,V=13,899ų. The asymmetric unit contains two independent steroid molecules and one water molecule, the latter disordered over two nonequivalent positions.Z=12[2(C₂₄H₄₀O₅)·1(H₂O)],F(000)=5496. Structure solution by direct methods; refinement by least-squares, toR=0.072. The complex hydrogen-bond system comprises: (a) three standard ordered O-HO hydrogen-bonds; (b) what is probably a symmetrically hydrogen-bonded carboxylic acid dimer, with a twofold rotation axisin the plane of the two carboxyl groups; (c) helical hydrogen-bonding chains about each 6₅ axis, disordered over four possible arrangements. In these helical chains, the six independent hydrogen-bonds can as a group be in either of two systems of nearly equivalent flip-flop arrangements: O-HO OH-O. Each helical system includes water, which can occupy either of two sites; thus, there is further disorder involving two sets of nonequivalent hydrogen-bonds with water as donor and acceptor. Many aggregation features here differ markedly from those in the crystal structures of either anhydrous cholic acid or cholic acid monohydrate.     

配合物[Co(phendione)(SO4)(H2O)]·5H2O的合成及表征

在水和甲醇的混合液中合成了标题配合物[Co(phendione)(SO4)(H2O)]·5H2O (phendione=1,10-菲啰啉-5,6-二酮),通过元素分析,红外光谱和热分析对配合物进行了表征.结果表明,配合物中Co(Ⅱ)与2个N原子和2个O原子形成4配位结构,其中2个N原子来自配体1,10-菲啰啉-5,6 -二酮,2个O原子分别来自1个水分子和1个硫酸根离子.根据热分解曲线,初步探讨了该配合物的热分解机理,热分解最终产物为CoO.     

Synthesis and X-ray structure of [(H3O)(C14H20O5)2][Me2NH2]2 [PMo12O40] · 2C14H20O5 (C14H20O5 = benzo-15-crown-5; Me2NH = dimethylamine)

[(H₃O)(C₁₄H₂₀O₅)₂][Me₂NH₂]₂ [PMo₁₂O₄₀] · 2C₁₄H₂₀O₅ 1 was synthesized from benzo-15-crown-5 and H₃PMo₁₂O₄₀·24H₂O in N,N-dimethylformamide for the first time. 1 crystallizes in the monoclinic space group C2/c with a = 18.583(4), b = 25.510(5), c = 19.904(4) Å, = 94.66(3)° D _c = 2.124 mg/m³ for Z = 4. Refinement based on 7358 observed reflections led to a R1(wR2) = 0.0378(0.0761). The complex cation, [(H₃O)(C₁₄H₂₀O₅)₂]⁺, exhibits a sandwich structure by hydrogen-bonding in the mean distance of 2.955 Å. The anion, PMo₁₂O₄₀ ^3–, is a -Keggin structure.