The crystal structure of a heterobimetallic crown ether complex: [Na(dibenzo-18-crown-6)][FeCl4]

Slow evaporation of a solution of ferric chloride and dibenzo-18-crown-6 in 31 CH₃CNCH₃OH produced single crystals of the title complex. This heterobimetallic crown ether complex, [Na(dibenzo-18-crown-6)][FeCl₄], crystallizes in the monoclinic space group P2_t/n with cell parameters (at 22°C)a=14.608(6),b=10.466(9),c=17.276(9)Å, =91.47(6)°, andD _calc=1.46 g cm^–3 for Z=4. The structure consists of discrete ions with the shortest Na ... Cl distance a lengthy contact of 3.56(1)Å. The average Na...O separation is 2.69(3)Å. The [FeCl₄]^– anion exhibits a distorted tetrahedral geometry with an average Fe–Cl bond length of 2.16(2)Å.     

Crystal structure of [Pb(cis-anti-cis-dicyclohexyl-18-crown-6)(OH2)2][ClO4]2

[Pb(cis-anti-cis-dicyclohexyl-18-crown-6)(OH₂)₂][ClO₄]₂ was crystallized using a slightly modified literature method for the separation of dicyclohexyl-18-crown-6 isomers. It crystallizes in the monoclinic space groupP2₁/n witha=8.415(5),b=20.993(9),c=8.973(5) Å, β=111.56(6)^o, andD _calc=1.84 g/cm³ for Z=2. The Pb²⁺ ion resides on a crystallographic center of inversion and is coordinated to the six crown ether donors and two axial water molecules in a hexagonal bipyramidal geometry. The Pb-O(etheric) distances range from 2.694(4) to 2.743(4) Å while the Pb?OH₂ distance is 2.522(6) Å.     

Synthesis and crystal structure of catena-poly[aqua(cis-syn-cis-dicyclohexyl-18-crown-6) tetra(thiocyanato)barium(II) platinum(II)]: [BaPt(NCS)4(C20H36O6)(H2O)] n

An organic–inorganic hybrid polymeric complex, [BaPt(NCS)₄(C₂₀H₃₆O₆)(H₂O)] _n or [[Ba(DC18C6-A)(H₂O)][Pt(SCN)₄]] _n (1) (DC18C6-A = cis-syn-cis-dicyclohexyl-18-crown-6) has been synthesized by the reaction of cis-syn-cis-dicyclohexyl-18-crown-6 with Ba(SCN)₂, BaCO₃ and H₂PtCl₄, and characterized by elementary analysis, FT-IR spectra and X-ray single-crystal diffraction. It crystallizes as monoclinic, space group P 2₁/n with crystallographic data: a = 14.275(6) ?, b = 13.165(5) ?, c = 18.971(8) ?, β = 106.294(6)°, V = 3422(2) ?³, Z = 4, D _calcd = 1.854 g/cm³, F(000) = 1856, R ₁ = 0.0491, wR ₂ = 0.0709. The asymmetric unit of complex 1 contains one [Ba(DC18C6-A)(H₂O)]²⁺ complex cation and one [Pt(SCN)₄]²⁻ complex anion, which are assembled into an infinite polymeric chain via the bridging SCN groups. The coordinated water molecule gives two different intrachain and interchain hydrogen bonds.     

Synthesis and Crystal Structure of Chiral Substituted (<Emphasis Type="Italic">S</Emphasis>)-2-[(<Emphasis Type="Italic">4</Emphasis>-Methoxyphenoxy) Methyl]-15-Crown-5 Ether with Sodium Perchlorate Complex

Abstract  The crystal and molecular structure of chiral crown ether, (S)-2-[(4-methoxyphenoxy)methyl]-15-crown-5 · NaClO₄, has been determined by single-crystal X-ray diffraction. The complex crystallizes in the orthorombic space group Pbca with Z = 8. Lattice parameters are a = 11.451(2), b = 12.842(3), c = 31.330(7) ?. The structure was refined to R factor of 0.0547. The Na ion is heptacoordinated. The Na–O_ether distances range from 2.363(4) to 2.433(4) ? and average 2.404(5) ?. Perchlorate anion is bounded to sodium ion asymmetrically; the Na–O8 and Na–O9 distances are 2.444(5) ? and 2.607(5) ?. The C–O and C–C distances of the 15-membered ring average 1.419(9) and 1.478(12) ? while the O–C–C and C–O–C angles average 108.2(6)˚ and 115.4(6)˚. Index Abstract  In the molecule, the sodium ion is seven coordinated by the five ring oxygen atoms and two oxygen atoms of the perchlorate anion. The macrocyclic strand of the molecule displays ag-a, ag+a, ag−a, ag+a, ag−g-set of torsion angles.      

Synthesis and crystal structure of a mixed-ligand lanthanum complex of phenanthroline H-bonded with benzo-15-crown-5

A mixed ligand lanthanum complex H-bonded with a crown ether benzo-15-crown-5 (B15C5), [La(NO₃)₃(H₂O)₂phen]B15C5 (phen = phenanthroline), was synthesized and characterized by elemental analysis, infrared spectrum, and X-ray crystal structure analysis. The crystals of the title compound are monoclinic, P2₁, with a = 18.879(6) Å, b = 20.110(5) Å, c = 19.358(4) Å, V = 6623.4 ų, = 115.68(3)°, Z = 8, D _calc = 1.623 g/cm³. In this complex, two nitrogen atoms from phen and eight oxygen atoms, six from NO₃ ^– and two from H₂O, coordinate to La(III), forming a 10-coordination structural unit. The two H₂O molecules are located in opposite directions of the unit, each H₂O is H-bonded with two O atoms of the B15C5, and each B15C5 molecule is H-bonded with two H₂O molecules on opposite sides, thus an infinite supramolecular chain forms. The title compound has a layered structure, and in each unit cell there exists one 3D channel.     

Crystal structure and electrochemical property of one‐dimensional complex: [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]2[Cu(mnt)2]

One metalorganic complex [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]₂[Cu(mnt)₂] (mnt = maleonitriledithiolate) has been obtained by the reaction of dicyclohexyl‐18‐crown‐6 with K₂mnt and CuCl₂·2H₂O. The title complex has been characterized by elementary analysis, FT‐IR, UV‐Vis spectroscopy and x‐ray single crystal diffraction. The title complex crystallizes in the triclinic space group P1 with crystallographic data: a = 10.870(6) Å, b = 11.536(6) Å, c = 12.904(7) Å, α = 101.541(10)°, β = 110.573(9)°, γ = 99.441(9)°, V = 1435.2(13) ų, Z = 1, D_calcd = 1.350 g/cm³, F(000) = 615, R₁ = 0.0641, wR₂ = 0.1475. It displays one‐dimensional chain‐like structure formed by [K(cis‐syn‐cis‐ dicyclohexyl‐18‐crown‐6)]⁺ complex cations and [Cu(mnt)₂]^2‐ complex anions through N‐K‐N interactions. Its electrochemical behavior has also been studied by the cyclic voltammetry. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Single Crystal X-Ray Structure of [Na(H2O)2(C18H15O6SO3)]2

Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. Single-crystal X-ray diffraction study indicates that it is a dimeric centrosymmetric species. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Graphical Abstract  [Na(H₂O)₂(C₁₈H₁₅O₆SO₃)]₂ was synthesized by sulfated 5-hydroxy-6,7,4′-trimethoxyisoflavone with concentrated sulfuric acid. The coordination polyhedron of each Na(I) atom exhibits a distorted trigonal bipyramidal geometry. The dimeric centrosymmetric units are linked by intermolecular hydrogen bonds C–H⋯π, C–H⋯O and O–H⋯O to result in a three-dimensional framework. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and crystal structure of a novel 3D supramolecular complex [Na(DC18C6-B)][Ni(mnt)<Subscript>2</Subscript>]

A supramolecular complex [Na(DC18C6-B)][Ni(mnt)₂] (1) (DC18C6-B = cis-anti-cis-dicyclohexyl-18-crown-6, isomer B; mnt = maleonitriledithiolate) has been prepared and characterized by elementary analysis, FT-IR spectroscopy and X-ray single crystal diffraction. It crystallizes in triclinic, space group P1 with crystallographic data: a = 7.974(4) Å, b = 14.343(7) Å, c = 15.559(8) Å, α = 96.230(8)^∘, β = 100.361(8)^∘, γ = 93.849(9)^∘, V = 1733.2(15) ų, Z = 2, D_calcd = 1.408 g/cm³, F(000) = 766, R₁ = 0.0491, wR₂ = 0.1018. The formula unit contains one [Na(DC18C6-B)]⁺ complex cation and one [Ni(mnt)₂]⁻ complex anion, which are constructed into an infinite chain-like structure through Na–N bonds. The resulting chains crisscross on the [Ni(mnt)₂]⁻ complex anions and further assemble into an unusual 3D supramolecular framework via the weak interactions.     

Synthesis and Crystal Structure Analysis of One Dimensional Supramolecular [Cd (Glu) (Tu)2]n

The complex of [Cd (C₅H₆O₄) (CH₄N₂S)₂]_n ( I ) has been synthesized and its X‐ray crystal structure determined at room temperature, M = 394.74, monoclinic, space group Pc (No. 7), with lattice parameters a = 7.683(3), b = 11.566, c = 16.00(1) Å, β = 100.32 (4)°, and Z = 4. There are two different Cd sites in this complex. Cd (1) coordinates to four oxygen atoms from Glutaric anion and two sulfide atoms from thiourea. Cd (2) coordinates to three oxygen and two sulfide atoms. The Cd atoms are linked by glutaric anion to form one‐dimensional chains. The adjacent chains are held together by hydrogen bonds to form a three dimensional network.     

Crystal Structure of bis(18-Crown-6)-bis(formato-O) dicaesium dihydrate

Abstract  The crystal structure of the title compound, [2Cs⁺(C₁₂H₂₄O₆)₂(CHO₂ ⁻)₂(H₂O)₂], was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁ /n with cell parameters a = 10.4278(7) ?, b = 10.0183(5) ?, c = 18.2383(12) ?, β = 93.723(5)°, V = 1910.3(2) ?³ and Z = 2. The Cs cations are bonded to each of the six O atoms of a crown ether ring, two water molecules, and one O atom of a formato anion. As a result of that, a centrosymmetric dimeric dinuclear complex is formed. The two halves of the dimer are connected by a ring of formato anions and water molecules which are linked by O–H···O hydrogen bonds. Index Abstract  The title compound, bis(18-crown-6)-bis(formato-O), caesium dihydrate, features a centrosymmetric dimeric dinuclear complex where two Cs cations are coordinated by six O atoms of a crown ether ring. The two halves of this complex are held together by a ring of formato anions and water molecules which are linked by hydrogen bonds.      

有机锡配合物{[nBu2Sn(OOCC5H3(NO2)2)]2O}2的合成、谱学表征和晶体结构

以3,5-二硝基苯甲酸和二丁基氧化锡为原料,合成了一种新的有机锡配合物{[~nBu_2Sn(OOCC_5H_3(NO_2)_2)]_2O}_2,并对其进行了元素分析、红外光谱表征和X射线单晶衍射.结果表明:该配合物属三斜晶系,P_ī空间群,a=1.0705(2) nm,b=1.3333(3) nm,c=1.4360(3) nm,α=68.892(3) °,β=78.297(3) °,γ=80.285(3) °, V=1.8620(7) nm~3 , Z=1, dc=1.613 g/cm~3 , μ=1.406 mm~(-1), F(000) =908, R_1=0.0408, wR_2=0.0948.该化合物分子是以Sn_2O_2四元环为中心,对称的二聚体结构,内外环锡原子均为五配位的畸变三角双锥构型.     

Macrocycle complexation chemistry 30: Comparison of the crystal structures of [La(NO3)3(15-crown-5)] and [La(NO3)3(monoaza-15-crown-5)]

For part 29, see Rogerset al. (1989).     

二维配位聚合物[Cd(C8H7NO2)2]n 的水热合成与晶体结构

在中温水热条件下,利用醋酸镉和3-(3-吡啶基)丙烯酸反应,合成了一种新型的二维配位聚合物[Cd(C8H7NO2)2]n.对其进行了元素分析、红外光谱表征和X射线单晶衍射测定.该配位聚合物属三斜晶系,P-1空间群,晶胞参数为:a=0.5031(2)nm,b=0.8109(3)nm,c=0.9531(4)nm,α=69.411(6)°,β=80.554(6)°,γ=76.020(7)°,V=0.3519(2)nm3,Z=1,dc=1.929g/cm3,μ=1.575 mm-1,F(000)=202,R1=0.0313,wR2=0.0641.     

The Crystal Structure of [La(NO3)6{Cu(2,2′-bipy)2}2][La(NO3)6Cu(2,2′-bipy)2]CH3CN with the Most Profuse Modes of Nitrate Coordination

The title compound [La(NO₃)₆{Cu(2,2′-bipy)₂}₂][La(NO₃)₆Cu(2,2′-bipy)₂] CH₃CN was synthesized, the crystal and molecular structures were determined at room temperature. The complex formed monoclinic crystals, space group P21/n (No.14), a = 10.354 (3) A, b = 23.440 (9) A, c = 32.817 (9) A, b = 90.39 (2)°, Z = 4. The crystal structure consisted of a discrete [La(NO₃)₆{Cu(2,2′-bipy)₂}₂]⁺ cation and [La(NO₃)₆Cu(2,2′-bipy)₂]^- anion and a non-coordinated CH₃CN molecule. Each La(III) ion was 12-coordinate with twelve oxygen atoms from six chelating nitrate ligands. There were four modes of nitrate coordination and the coordination geometry of all three copper ions was different in the crystal structure.     

新型配位聚合物[Ni(C6H4NO2)2(H2O)4]n的水热合成和晶体结构

以NiCl2·6H2O和4-氰基吡啶为原料,在中温水热反应条件下,合成了一种新型配位聚合物[Ni(C6H4NO2)2(H2O)4]n单晶体,并对其进行了元素分析、红外光谱表征和X射线单晶衍射测定.该配位聚合物属三斜晶系,P-1空间群,a=0.6298(4)nm,b=0.6907(4)nm,c=0.9243(5)nm,α=96.437(8)°,β=105.184(9)°,γ=113.314(9)°,V=0.3456(3)nm3,Z=2,dc=1.802 g/cm3,μ=1.452mm-1,F(000)=194,R1=0.0309,R2=0.0753.该晶体通过配位键的连接和分子间氢键相互作用形成三维的网状结构.     

Synthesis, structure and characterization of a new inorganic-organic hybrid complex (C3H5N2)2[Cd(C3H4N2)2Nb2O3F8]·2H2O

(C₃H₅N₂)₂[Cd(C₃H₄N₂)₂Nb₂O₃F₈]·2H₂O (C₃H₄N₂=imidazole) (1) was prepared from the hydrothermal reaction of Nb₂O₅, 3CdSO₄·8H₂O, C₃H₄N₂, HF and H₂O at 403 K, and characterized by single crystal X-ray diffraction and IR spectra. 1 crystallizes in the orthorhombic system, space group Pba2, with a=11.0192(9), b=16.8012(14), c=6.8717(6) ?, and Z=2. The crystal is made up of [Cd(C₃H₄N₂)₂Nb₂O₃F₈]²⁻ anions, [C₃H₅N₂]⁺ complex cations and H₂O molecules of crystallization. And the backbone of the compound is a one dimension coordination polymeric chain containing the anions. The complex cations and anions are linked through hydrogen bonding interactions. Co-crystallized water molecules fill in the pores and hydrogen bond to the host. Bond valence sums show that O1, O3 and F3 have much more negative charge, which are in agreement with the crystal structure that they act as bridging atoms.Supplementary material CCDC-606794 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdc.cam.ac.uk/ const/retrieving.html or from the Cambridge Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and crystal structure of [Tb4(H2O)2](C2O4)2(C5H6O4)4

A terbium complex associating two ligands, oxalate and glutarate, was prepared under hydrothermal conditions at 200°C by treating an aqueous suspension of terbium oxalate decahydrate with glutaric acid and guanidinium carbonate. Its structure was solved by X-ray diffraction on a single crystal. It crystallizes in the monoclinic space group P2₁ with lattice constants, a = 9.514(1) Å, b = 9.0681(8) Å, c = 19.702(2) Å, and = 97.90(1)°. The terbium atoms and the oxalate ligands build dense chains which are connected by one side of the carboxylic group of some glutarate ligands, thus forming a sheet at the c level 0 and 1/2. These sheets are bridged by glutarate groups. The terbium atoms are ninefold coordinate with nine oxygen atoms of the ligands or with one water molecule and eight oxygen atoms of the ligands. Each polyhedron of the terbium atoms share one edge and one face of oxygen atoms with the two neighboring ones. The oxalate ligands are bischelating and bismonodentate. The coordination scheme of glutarate differs: either they are bismonodentate from one side and chelating and monodentate from the other side or they are chelating and monodentate from both sides.     

Synthesis and crystal structure of [Nd(H2O)2]2(C2O4)3

Some crystals of [Nd(H₂O)₂]₂(C₂O₄)₃ were synthesized hydrothermally by heating at 200°C for 8 days an aqueous suspension of neodymium oxalate decahydrate in presence of terephthallic acid and guanidinium carbonate. They crystallize in the orthorhombic system, space group P2₁2₁2₁, with a = 8.6702(7) Å, b = 9.558(2) Å, and c = 17.009(2) Å. The structure of this complex is built up by two independent neodymium atoms, three bischelating oxalate ligands, and four water molecules forming a rectangle building unit of 6-membered ring, [Ln(H₂O)₂(C₂O₄)]₆. The packing of these units leads to a layer parallel to the plane (001). However, the neodymium atoms of two neighbor layers share an edge of oxalato oxygen atoms thus giving a double-layer. The three dimensionality between these double-layers is insured by hydrogen bonds of water molecules which are bound to the neodymium atoms. There is no zeolitic water molecule. The two neodymium atoms are nine-coordinated. In both cases, the coordination polyhedron can be described as a distorted tricapped trigonal prism.     

无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3]的合成和晶体结构

合成了无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3],并采用元素分析、红外光谱表征和单晶X射线衍射分析和热重分析研究.红外光谱分析表明SCN-采用1,3-μ模式.结构分析表明,相邻的Cd(II)原子通过三个1,3-μ-SCN- 阴离子桥连形成无限的[Cd(SCN)-3]∞之字链结构,固体结构中[C12H11N2O2]+阳离子和[Cd(SCN)-3]∞配阴离子形成了分离柱状堆积.该晶体属于单斜晶系P2(1)/c空间群,晶胞参数分别为:a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3 , T = 293(2) K, μ = 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)]. 热分析结果在180-305 ℃化合物失去一个有机分子,305 ℃以上伴随着镉升华失去三个SCN-阴离子.     

Self-assembly in transition metal complexes: structural characterization of a copper histamine nitrate [Cu(II)(him)2(NO3)2]

A new monomeric copper (II) complex with histamine (him), [Cu(II)(him)₂(No₃)₂], has been prepared by the reaction of Cu(NO₃)₂ with histaminium dichloride and its structure was determined by x-ray crystallography. The complex crystallizes in the triclinic system, space group with a = 5.7238(4), b = 8.7094(7), c = 9.2481(11) Å, = 69.693(8), = 73.242(7), = 71.050(7)°, V = 400.84(6) ų, and Z = 1. The structure consists of discrete [Cu(II)(him)₂(NO₃)₂] molecules in which the metal atom is centrosymmetrically coordinated by two histamine ligands forming an equatorial plane with Cu–N(imidazole ring) being 2.032(2) and Cu–N(NH₂ group) being 2.023(2) Å. Two O atoms from nitrate anions coordinate on the elongated axial positions with Cu–O being 2.549(2) Å. In the crystal structure, the molecules are organized by hydrogen bonds forming a two-dimensional network.