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.     

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.     

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.     

配合物[Cu2(C6H2Cl2OC=N-C3H6COO)2(H2O)2]·3H2O合成与晶体结构

本文以苏氨酸,3,5-二溴水杨醛以及醋酸铜为原料合成了新型配合物[Cu2(C6H2Cl2OC=N-C3H6COO)2(H2O)2]·3H2O,并对其晶体结构经元素分析,红外光谱及X射线单晶衍射表征.结果表明:该晶体属单斜晶体结构,晶胞参数分别为:a=0.6985(2) nm, b=1.0789(2) nm, c=1.9639(3) nm, β=92.182(3) °, Mr=797.34, V=1.4789(6) nm3 , Z=2, Dc=1.790 g/cm3, μ(MoKa) =1.867 mm-1, F(000)=808, R=0.0321, wR= 0.0566.Cu(II)与一个N原子,两个O原子以及一个水分子构成三齿链状席夫碱.不对称单元结构包含两个配合物分子及三个由氢键链接的水分子.     

Crystal structure of aminoguanidinium hexahydro-closo-hexaborate dihydrate, (CN4H7)2B6H6 · 2H2O

The (HAgu)₂B₆H₆ · 2H₂O compound was synthesized and its crystal structure was determined [R = 0.0385 for 2018 reflections with I > 2σ(I)]. The structure consists of HAgu ⁺ cations, centrosymmetric B₆H ₆ ^2? anions, and water molecules. The anions have an almost regular octahedral structure. The bond lengths and angles lie within the following narrow ranges: B-B, 1.715–1.726(2) Å; B-H, 1.08–1.14(2) Å; B-B-B, 59.72°–60.29(9)° and 89.63°–90.20(11)°; and B-B-H, 133.2°–137.0(9)°. The HAgu ⁺ cations and water molecules are involved in the O-H?O, N-H?O, and N-N?N hydrogen bonds and participate in numerous (N, O)-H?H-B specific interactions with the B₆H ₆ ^2? anions, which results in splitting and high-frequency shift of the band of B-H stretching vibrations in the IR spectrum.     

[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.     

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.     

[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.     

Refined crystal structure of lovozerite Na2CaZr[Si6O12(OH,O)6] · H2O

The structure of Na,Ca,Zr-silicate lovozerite, Na₂CaZr[Si₆O₁₂(OH,O)₆] · H₂O, from the Khibiny alkaline massif (the Kola Peninsula) was refined by single-crystal X-ray diffraction analysis (Syntex $P\bar 1$ diffractometer, λMoK _α radiation, 2θ/θ scanning technique). The refinement (R _hkl = 0.077, 1531 independent reflections; anisotropic thermal parameters) confirmed the trigonal system proposed for the mineral earlier (sp. gr. R3; a = 10.18(1) Å, c = 13.13(2) Å, Z = 3) and revealed the presence of two additional positions (C and B) statistically occupied by Ca and Na atoms (and partly by Mn) and H₂O molecules, respectively.     

Silicogermanate Ba2K2In2[(Si0.8Ge0.2)6O18] · 2H2O As an Analogue of the Natural Zirconosilicate Kostylevite K4Zr2[Si6O18] · 2H2O

Crystallography Reports - Crystals of new silicogermanate Ba2K2In2[(Si0.8Ge0.2)6O18] · 2H2O were prepared by the hydrothermal synthesis; sp. gr. P21/n, a = 6.5548(6) Å, b = 11.6946(10)...     

α-NiSO4·6H2O晶体生长与光学性质

用水溶液降温法生长出光学品级的α-NiSO4·6H2O大单晶,对晶体的透过光谱和(001)晶面的X射线衍射性能进行了测试和表征.     

Interferometric study of the growth kinetics of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals

Crystallography Reports - The growth kinetics of the (001) and (110) faces of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals in the kinetic mode has been in situ investigated for the...     

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.     

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.     

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)     

Crystal structure of N-benzylmethylammonium dihydrogen-monophosphate monohydrate, [C6H5CH2NH2CH3]H2PO4·H2O

The salt N-benzylmethylammonium dihydrogenmonophosphate monohydrate is monoclinic with the following unit cell dimensions: a = 6.356(1)Å, b = 8.385(7)Å, c = 11.472(5)Å, = 104.32(1)°, space group P2₁ with Z = 2. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O–H···O and N–H···O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Synthesis and structure determination of a new layered zincophosphate: [H2N2C6H16]0.5[Zn2(PO4)(HPO4)(H2O)]·H2O

The synthesis and crystal structure of a new microporous zincophosphate are described. [H₂N₂C₆H₁₆]_0.5[Zn₂(PO₄)(HPO₄)(H₂O)]·H₂O crystallizes in the triclinic space group P1¯ with a = 8.822(4), b = 9.236(4), c = 8.451(3) Å, = 67.19(3), = 91.32(3), = 111.10(3)°, V = 586.7(4) ų and Z = 2. This new material consists of infinite two-dimensional anionic layers alternated with planes containing organic diprotonated templates, N, N, N, N-tetramethylethylenediamine [H₂N₂C₆H₁₆]²⁺ molecules. The framework structure is built up of ZnO₄, ZnO₃OH₂, PO₄, and PO₃OH tetrahedra, linked through oxygen vertices. The presence of terminal OH₂ and OH groups, leads to an open structure containing four- and eight-rings. The organic molecules are interconnected to the framework through hydrogen bonds.     

A dinuclear cyanide-bridged complex, [(DMF)4(H2O)3LuCo(CN)6]·H2O

The crystal structure of the bimetallic cyanide bridged complex [(DMF)₄(H₂O)₃LuCo(CN)₆]·H₂O (1) was obtained by single-crystal X-ray diffraction. The central lutetium(III) ion is eight coordinate arranged in a square antiprism while the cobalt(III) ion is six coordinate, oriented octahedrally. Molecules in the crystal lattice are held together by a network of hydrogen bonding. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a = 13.875(2), b = 8.8352(9), c = 24.633(2) Å = 96.392(8)° and Z = 4.     

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.