Crystal structure of [Co(Ox)(NH3)4][Bi(Edta)] ⋅ 3H2O

The crystal structure of [Co(Ox)(NH₃)₄][Bi(Edta)] ? 3H₂O is determined. The crystals are monoclinic, a = 9.291 Å, b = 22.275 Å, c = 11.402 Å, β = 105.79°, V = 2270.7 ų, Z = 4, and space group P2₁/c. The [Bi(Edta)]^? anionic complexes are linked into polymeric chains through two Bi-O bonds with the neighboring complexes.     

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.     

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.     

[Co(dmg)2Cl2]3·[Co(dmg)2Cl(OH)]·[Co(dmg)(phen)]·(H2O)4的合成和晶体结构

本文合成了一个复杂的单核配合物 [Co(H2dmg)2Cl2]3·[Co(H2dmg)2Cl(OH)]·[Co(Hdmg)(phen)]·(H2O)4 (H2dmg＝dimethylglyoxime, phen＝1,10-Phenanthroline).通过X射线衍射技术获得其单晶结构.在单晶结构中,每五个单核钴(II)的配位结构形成一个重复单元,是一个较为复杂的单晶.其空间群为P-1,晶胞参数为a＝1.3738nm;b＝1.4396nm;c＝1.8656nm.本文中我们将讨论该化合物的分子结构及相关光谱性质.     

Synthesis and crystal structure of [Cu(azpy)(H2O)4][Cu2(nta)2(azpy)]····6H2O: A two-dimensional network solid

The copper(II) complex [Cu(azpy)(H₂O)₄][Cu₂(nta)₂(azpy)]····6H₂O (nta = nitrilotriacetate, azpy = 4,4-azobispyridine) has been synthesized and structurally characterized. It crystallizes in the triclinic space group P , a = 8.6985(3) Å, b = 9.4776(3) Å, c = 14.6544(5) Å, = 71.5360(10)°, = 85.7600(10)°, = 88.1420(10)°, V = 1142.74(7) ų, Z = 1. The crystal structure consists of one-dimensional linear chain cations and dimeric anions. The copper centers in the anion possess distorted trigonal bipyramidal geometry, while Cu(2) has a distorted octahedral geometry in the cation. Coordinated water molecules in the one-dimensional chain form interionic hydrogen bonds with the oxygen atoms of the carboxylate of nta of the dimmer anion. These hydrogen bonds result in the formation of a two-dimensional network.     

Crystal structure of strontium aqua(ethylenediaminetetraacetato)cobaltate(II) tetrahydrate Sr[CoEdta(H2O)] · 4H2O

The complex Sr[Co^II Edta] · 5H₂O (I) (where Edta ^4? is the ethylenediaminetetraacetate ion) has been synthesized. The crystal structure of this compound is determined by X-ray diffraction. Crystals are monoclinic, a = 7.906(2) Å, b = 12.768(2) Å, c = 18.254(3) Å, β = 95.30(3)°, V = 1834.8 ų, space group P2₁/n, Z = 4, and R = 0.036. The structure is built up of the binuclear complex fragments {Sr(H₂O)₃[CoEdta(H₂O)]}, which consist of the anionic [CoEdta(H₂O)]^2? and cationic [Sr(H₂O)₃]²⁺ units linked by the Sr-O bonds into a three-dimensional framework. The coordination polyhedra of the Co and Sr atoms are mono-and bicapped trigonal prisms. The coordination sphere of the Co atom (the coordination number is equal to 6 + 1) involves six donor atoms (2N and 4O) of the Edta ^4? ligand and the O_w atom of water molecule. One of the Co-O distances (2.718 Å) is considerably longer than the other Co-O_lig distances (2.092–2.190 Å) and the Co-O_w(1) distance (2.079 Å). The Sr coordination polyhedron (the coordination number is eight) contains three water molecules, three carbonyl O atoms of the three different anionic complexes, and two O atoms of one acetate group of the fourth anionic complex. The Sr-O distances fall in the range 2.535–2.674 Å. The structural formula of the compound is {Sr(H₂O)₃[CoEdta(H₂O)]}_3∞ · H₂O.     

Synthesis and crystal structure of [Co(phen)(H2O)4](SO4)⋅2(H2O)

The title complex, [Co(phen)(H₂O)₄](SO₄)2(H₂O) (phen = 1,10-phenanthroline) was prepared in aqua tert-butylperoxohydrogen solution. X-ray single crystal structure determination reveals that the complex consists of a phenanthrolinatocobalt(II)tetrahydrate dication, two uncoordinated water molecules and a sulfate anion. It crystallizes in the orthorhombic space group Pbca with a = 8.856(1), b = 18.318(3), c =21.918(5) Å, V = 3555.6(11) ų. The coordination geometry at each cobalt(II) atom is a slightly distorted octahedron.     

Crystal structure of {NH2C(NHC6H5)2}3[UO2(C2O4)2(NCS)] · 1.25H2O

Synthesis and X-ray diffraction study of {NH₂C(NHC₆H₅)₂}₃[UO₂(C₂O₄)₂(NCS)] · 1.25H₂O single crystals have been performed. This compound is crystallized in the orthorhombic system, with the unit-cell parameters a = 45.2646(8) Å, b = 57.7359(11) Å, c = 7.9244(3) Å, sp. gr. Fdd2, Z = 16, V = 20 709.6(10) ų, and R = 0.0477. The uranium-containing structural units of the crystals are one-core groups of the [UO₂(C₂O₄)₂(NCS)]^3? composition, belonging to the crystallochemical group AB ₂ ⁰¹ M ¹ (A = UO ₂ ⁺² , B ⁰¹ = C₂O ₄ ^2? , M ¹ = NCS^?) of uranyl complexes. The uranium-containing complexes are connected into a three-dimensional framework owing to the electrostatic interactions with the outer-sphere cations and a system of hydrogen bonds.     

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)     

Synthesis and structure of (NH4)3[UO2(C3H2O4)2(NCS)] · 2H2O

Malonate-thiocyanate complex (NH₄)₃[UO₂(C₃H₂O₄)₂(NCS)] · 2H₂O is synthesized and studied by X-ray diffraction. The compound crystallizes in the monoclinic system: a = 13.9983(4) Å, b = 8.1947(2) Å, c = 16.4678(4) Å, β = 100.846(1)°, space group Cc, Z = 4, and R = 0.0158. The main structural units of the crystal are mononuclear [UO₂(C₃H₂O₄)₂(NCS)]^3? groups belonging to the AB ₂ ⁰¹ M ₁ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₂O ₄ ^2? , M ¹ = NCS^?). Discrete uranium-containing groups are connected by electrostatic interactions with ammonium ions and by hydrogen bonds. Some specific structural features of crystals containing [UO₂(L)₂(NCS)]^3? complexes, where L is the oxalate or malonate ion, are discussed.     

Crystal structure of calcium trans-N-(nitrilotriacetato)(pyridine-2-carboxylato)cobaltate(III) hexahydrate, Ca[Co(Nta)(Pic)]2] · 6H2O

Crystals of Ca[Co^III (Nta)(Pic)]₂ · 6H₂O (I) (where Nta ^3? and Pic ^? are the nitrilotriacetate and picolinate ions, respectively) are prepared and characterized by the X-ray diffraction technique. Crystals I are monoclinic, a = 18.599(4) Å, b = 12.556(3) Å, c = 14.042(3) Å, β = 102.90(3)°, V = 3196(1) ų, Z = 4, space group P2₁/c, R1 = 0.0278, wR2 = 0.0716, and Goof = 1.054 for 4982 reflections with I > 2σ(I). Structure I is built of the { Ca(H₂O)₄[Co(Nta)(Pic)]₂{ _1∞ polymer ribbons and molecules of crystallization water. One of the two symmetrically independent anionic complexes (B) is included in the chain and alternates with cationic units, whereas the other anionic complex (A) forms a branch of this chain. The cationic and anionic units are interlinked via the interactions of the Ca²⁺ cations with the carbonyl atoms of the main (Nta ^3?) and additional (Pic ^?1) ligands. The octahedral environment of the Co(III) atoms consists of donor atoms of the Nta ^3? (N + 3O) and Pic ^? (N + O) ligands. The coordination polyhedron of the Ca atom (pentagonal bipyramid) includes two carbonyl O atoms of two Nta ^3? ligands, one O_Pic atom, and four O_w atoms of water molecules.     

Crystal structure of [Co(bipy)(maleato) (H2O)3]·H2O (bipy = 2,2′-bipyridine)

Preparation of the mononuclear cobalt(II) complex, [Co(bipy)(maleato) (H₂O)₃]·H₂O (1) where bipy = 2,2-bipyridine, were accomplished by reaction of an aqueous solution containing sodium maleate and an ethanolic solution of Co(NO₃)₂·6H₂O and bipy. The crystal structure of complex (1) was determined by X-ray crystallography. The complex crystallizes in the monoclinic space group P2₁/n with a = 9.477(3), b = 7.660(2), c =23.526 (3) Å, = 97.64(2)°, V = 1692.6(6) ų, and Z = 4. The structure consists of discrete mononuclear cobalt molecules. The cobalt atom is six-coordinate and presents a slightly distorted octahedral geometry, which consists of the two imine N atoms of bipy, a terminal carboxylate O atom from maleato ligand, and a water O atom in the basal plane with Co—N bond distances of 2.116(2) and 2.124(3) Å and Co—O distances of 2.075(2) and 2.088(2) Å, respectively. The relatively shorter Co—O distances are due to the trans effect of the bipy ligand. The octahedral coordination is completed the other two water molecules. The coordinate and the lattice water molecules were identified by TG study.     

Synthesis and structural characterization of [Co(tren)(Tsal)]ClO4·H2O and [Ni(pn)(py)2(NCS)2]

Complexes [Co(tren)(Tsal)]ClO₄·H₂O 1 and [Ni(pn)(py)₂(NCS)₂] 2, (tren = tris(2-aminoethyl)amine, Tsal = thiosalicylate ion, pn = 1, 2-diamino propane and py = pyridine) have been synthesized and structurally characterized. Both complexes crystallize in the monoclinic space group C2/c with a = 21.3340(6), b = 11.7754(2), c = 14.8076(5) Å, = 100.3831(10)°, Z = 8 (1), and a = 7.2573(8), b = 17.8810(11), c = 15.2681(12) Å, = 101.170(2)°, Z = 4 (2). The metal atoms in both cases have distorted octahedral geometry. In 1, the tren ligand is quadridentate and Tsal is bidentate chelate. In 2, the pn ligand forms a bidentate chelate with the NCS ligands in trans positions. Complex 1 is diamagnetic whereas 2 shows paramagnetism with a magnetic moment of 3.10 B. M.     

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.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

[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.     

Eightfold-coordinated diethylenetriaminepentaacetates: Crystal structures of K[M(Dtpa)] ⋅3H2O (M = Zr or Hf) and NH4[Sn(Dtpa)] ⋅ H2O

The crystal structures of K[M(Dtpa)] ? 3H₂O (M = Zr or Hf) and NH₄[Sn(Dtpa)] ? H₂O are studied by X-ray diffraction. The coordination number of the metal atom in all the compounds is eight. The NH₄[Sn(Dtpa)] ? H₂O complex is isostructural to the (H₅O₂)[M(Dtpa)] ? H₂O (M = Sn or Hf) compounds studied earlier.     

Complexation between molybdenum(VI) and oxalate: Crystal and molecular structure of [(−)Co(en)3][MoO3(C2O4)OH2]I·2 H2O

The crystal structure of the product of the reaction between [(–)Co(en)₃]I₃ and a mixture of Na₂MoO₄ and NaHC₂O₄ in aqueous solution is reported: [(–)Co(en)₃][MoO₃(C₂O₄)OH₂]I·2H₂O, space groupP2₁2₁2₁,a=8.131(2),b=14.590(4),c=17.509(4) Å;Z=4. FinalR=0.048,R _w=0.050,w=( ² F)^–1 for 1899 reflections. The configuration of the Mo(VI) oxalate complex differs notably from that proposed previously on the basis of chemical analysis and equilibrium studies.     

Synthesis, Structure and Properties of (H2NCH2CH2NH3)3 {(VO)6 [B10O16 (OH)6]2} · 11H2O

Abstract A new polyoxovanadoborate cluster (H₂NCH₂CH₂NH₃)₃ {(VO)₆[B₁₀O₁₆(OH)₆]₂} · 11H₂O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA. The crystal of the new compound belongs to monoclinic system, space group C2/c with a = 20.198(1) ?, b = 13.4476(8) ?, c = 21.602(1) ?, β = 97.067(1)°, V = 5822.8(5) ?³, Z = 4, D _c = 1.956 g cm⁻³, M = 1714.4, μ = 1.066 mm⁻¹, S = 1.905, R = 0.059, R _w = 0.0966. Index Abstract A new polyoxovanadoborate cluster (H2NCH2CH2NH3)3{(VO)6 [B10O16(OH)6]2} · 11H2O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA.