Synthesis and Structure of a Silver(I) Complex {[Ag5(L)2(NO3)4](NO3)(CHCl3)2}n [L?=?2,3-bis(pyrimidine-2-thiomethyl)quinoxaline]

Abstract  The reaction of the dithioether ligand, 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline (L) with AgNO₃, leads to the formation of a novel complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}n 1, which has been characterized by single-crystal X-ray diffraction analysis: monoclinic, space group C2/c, with a = 34.741(7), b = 9.930(2), c = 17.004(4) ?, β = 106.497(6)° and V = 5625(2) ?³.Complex 1 consists of 2D {[Ag₅(L)₂(NO₃)₄]⁺}n cations, uncoordinated anions and CHCl₃ solvent molecules. In 1, there exist three crystallographic independent Ag^I centers, which adopt different coordination geometries. There exist π–π stacking interactions in the complex and these weak interactions further stabilize the crystal structure in the solid state. The coordination feature of the ligand has been investigated by DFT calculations. Index Abstract  Synthesis and Structure of a Silver(I) Complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}_n [L = 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline] Chao-Yan Zhang, Qian Gao, Ya-Bo Xie*, and Jian-Bo Feng The crystal structure of complex {[Ag₅(L)₂(NO₃)₄](NO₃)(CHCl₃)₂}n (L = 2,3-bis(pyrimidine-2-thiomethyl)quinoxaline) consists of 2D {[Ag₅(L)₂(NO₃)₄]⁺}n cations, uncoordinated anions and CHCl₃ solvent molecules. There exist three crystallographic independent Ag^I centers, which adopt different coordination geometries. The coordination feature of the ligand has been investigated by DFT calculations.      

Synthesis and crystal structure of the copper(I) complex with 2-[(o-pyridyl)-sulfanylmethyl]-pyrimidine ligand

The reaction of a flexible monothioether ligand, 2-[(o-pyridyl)-sulfanylmethyl]-pyrimidine (L), with CuI leads to the formation of a novel complex [Cu₄I₄(L)₂] (1), which has been characterized by elemental analyses, IR spectroscopy, and single-crystal X-ray diffraction analysis: monoclinic, space group P2₁/n, with a = 10.921(5), b = 10.824(5), c = 13.128(6) Å, β = 109.333(5)° and Z = 2. Single-crystal X-ray analyses show that complex 1 is tetranuclear structure with a distorted chair-like Cu₄I₄ skeleton. Cu···Cu interactions are found to exist in this tetranuclear molecule. In the packing mode of complex 1, there exist N⋯⋯⋯I weak interactions and intermolecular π–π contacts. These weak interactions not only stabilize the structure of complex, but also further link the tetranuclear molecules into a high-dimensional supramolecular architecture.     

The co-crystal of iron(II) complex hydrate with hydroxybenzoic acid: [Fe(Phen)<Subscript>3</Subscript>]Cl(p-hydroxybenzoate).2(p-hydroxybenzoic acid).7H<Subscript>2</Subscript>O

Crystal of [Fe(Phen)₃]Cl(PHB).2(PHBH).7H₂O (1) is triclinic, space group P-1 with a = 12.0388(11) ?, b = 15.5286(14) ?, c = 15.7794(14) ?, α = 89.759(2)°, β = 75.818(2)°, γ = 71.900(2)° and Z = 2, (phen = phenanthroline, PHBH = p-hydroxybenzoic acid, PHB = p-hydroxybenzoate anion). The phen in adjacent Fe(phen)₃ ²⁺ cations are π–π interacted forming offset face to face (OFF) motifs. Juxtaposition of four phen ligands from two cations encapsulate an R₂ ²(8) dimeric unit of H-bonded PHBH molecules within a centrosymmetric box froming a filled aryl box motif (FAB). Alternation of OFF and FAB motifs form {OFF⋯FAB}∞ strands. The Fe(phen)₃ ²⁺ cation engages its phen ligands in π–π and/or CH–π interactions with two crystalographically different PHBH molecules and one PHB anion. Seven water molecules and a chloride anion per iron(II) trisphenanthroline cation fill empty spaces in the structure forming a hydrophilic cluster. Extensive intermolecular H-bond interactions occur between water molecules, chloride anions, PHBH molecules, and PHB anions. Thermal analysis of (1) was done under N_2(g). The TG, and dTG curves revealed the expected mass losses. All associated processes are endothermic as shown in the DSC curve.     

Intermolecular interactions involved in the crystal structure of 2-amino-5-methylpyridinium hexabromostannate (IV), (C<Subscript>6</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>[SnBr<Subscript>6</Subscript>]

The salt bis(2-amino-5-methylpyridinium) hexabromostannate(IV) (C₆H₉N₂)₂[SnBr₆] is monoclinic, P2 ₁ /c, with the following cell parameters: a=9.1636(18) ?, b=28.767(7) ?, c=16.956(17) ?, β=101.008(5)°, V=4387.5(17) ?³, Z=8, formula units. X-ray crystallography revealed that the structure can be regarded as a semi-regular three-dimensional array of anions, with pairs of cations forming layers perpendicular to b axis in the cavities between the anions. The cohesion forces that connects molecules in the organic layers are hydrophilic N⋯HCH₂ and HN⋯HN hydrogen bonding as well as hydrophobic π-π stacking and CH₃⋯π interactions. Cations and anions are connected via strong Br⋯H hydrogen bonding. Supplementary material CCDC 276493 contains the supplementary crystallographic data. These data can be obtained free of charge via www.ccdc. cam.ac.uk/data_request/cif, by e-mailing data_ request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033.     

Hydrogen Bonded 3D Supramolecular Architectures of Three Saccharinate Salts

Abstract  

Three saccharinate salts (2-aminopyrimidine): (saccharin) (1), (4-phenylthiazol-2-amine): (saccharin) (2), and (2-methylquinoline): (saccharin) (3) were prepared and structurally characterized by X-ray crystallography. Salt 1 crystallizes in the monoclinic, space group P2(1)/c, with a = 7.1782(9) ?, b = 13.5105(16) ?, c = 12.2251(12) ?, β = 93.3410(10)°, V = 1183.6(2) ?³, Z = 4. Compound 2 crystallizes in the triclinic, space group P-1, with a = 7.4584(7) ?, b = 8.6930(9) ?, c = 12.9179(14) ?, α = 108.952(2)°, β = 91.7510(10)°, γ = 97.2280(10)°, V = 783.57(14) ?³, Z = 2. Compound 3 crystallizes in the monoclinic, space group P2(1)/c, with a = 7.781(8) ?, b = 19.4209(19) ?, c = 10.9719(12) ?, β = 107.7390(10)°, V = 1579.2(16) ?³, Z = 4. The different hydrogen bonding interaction modes of the saccharinate anions and the cations lead to 3D network structure, 3D staircase structure, and 3D ABAB layer structure for 1, 2, and 3 respectively. Despite variations in the cation shape on the aromatic N–heterocyclic compounds, there all existed strong intermolecular N–H⋯O(carbonyl) hydrogen bonds. In compounds 1, and 3 the N⁺–H⋯O interaction between the N⁺–H group of the cation and the C=O group of the saccharinate anion is the most important interaction in this family of salts. However, in 2, there was a N–H⋯O interaction between the amino proton and the C=O group of the saccharinate anion. At the next level, the aromatic C–H proton interacts with the sulfonyl O atom. There are also π–π interactions in compounds 1–2, there is CH₃–π interaction in 3. Under these interactions the three compounds exhibit synthons I–III respectively. These interactions are responsible for the high-yielding supramolecular assembly of N-containing aromatic bases and the saccharinate into salts.     

Crystal structures of 3-[1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl]-1-[4-(methyl (I)/methoxy (II) phenyl)]-2-phenyl-propane-1-one

The compounds 3-(1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl)-1-[4-methyl (I)/methoxy (II)phenyl)]-2-phenyl-propane-1-one crystallize in triclinic space group P . The details are: compound I a = 11.941(6) ?, b = 12.154(7) ?, c = 13.006(7) ?, α = 63.124(8)°, β = 84.464(9)°, γ = 64.810(8)°, V = 1519.7(14) ?³, Z = 2, D _cal = 1.284 Mg m⁻³, and R = 0.0382 (wR = 0.0978); compound II a = 11.897(6) ?, b = 12.268(6) ?, c = 13.001(7) ?, α = 61.919(8)°, β = 83.480(8)°, γ = 64.676(7)°, V = 1504.0(14) ?³, Z = 2, D _cal = 1.333 Mg m⁻³, and R = 0.0422 (wR = 0.1049). The indole ring system in both the molecules I and II are not strictly planar and the dihedral angles formed by the pyrrole and benzo planes are 4.0(7)° and 3.5(8)°, respectively. The C–HO, C–Hπ and ππ types of interactions stabilize the molecules in the unit cell in addition to van der Waal's forces in I and II.     

Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid

Abstract  The Ni(II) complex, [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O, H₂biim being 2,2′-biimidazole, PABA being 4-aminobenzoic acid has been synthesized and the crystal structure determined using X-ray crystallography. The complex crystallizes in triclinic system, space group P − 1 with unit cell parameters a = 8.3920(9) ?, b = 9.8436(11) ?, c = 9.8874(11) ?, α = 94.862(2)°, β = 109.142(2)°, γ = 90.992(2)°, V = 767.95(15) ?³ and Z = 1. The molecules of the complex in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure. Index Abstract  Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid Yanping Li and Pin Yang* The molecules of the title complex [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure.      

Structures of Three Chalcones Derived from 6-Methoxy-2-naphthaldehyde

Abstract  In the molecular structures of three new structurally related chalcone derivatives, namely (2E)-1-(2-hydroxyphenyl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one, C₂₀H₁₆O₃, I, (2E)-1-(2-chloropyridin-4-yl)-3-(6-methoxy-2-naphthyl)prop-2-en-1-one, C₁₉H₁₄ClNO₂, II, and (2E)-3-(6-methoxy-2-naphthyl)-1-pyridin-4-ylprop-2-en-1-one, III, C₁₉H₁₅NO₂, the configuration of the keto group is syn with respect to the olefinic double bond. In all three structures the molecules pack with weak intermolecular C–H···O interactions utilizing both the methoxy and keto oxygen’s in I, the methoxy oxygen in II and the keto oxygen in III. These interactions link the molecules into chains diagonally along the (011) plane of the unit cell in I and III and along the (010) plane in II. The dihedral angle between the phenyl and 2-napthyl rings in I is 31.7(3)°. In II and III the dihedral angle between the pyridyl and 2-naphthyl rings is 14.4(9)° and 1.8(9)°, respectively. C–H···O hydrogen bonding interactions influence these twist angles of these rings in I–III while weak π–π stacking interactions between naphthyl rings in I and III and also between pyridyl and naphthyl rings in II help stabilize crystal packing. [I: P2 ₁ /c, a = 7.6635(4) ?, b = 11.8047(6) ?, c = 16.7584(7) ?, β = 99.271(5)°, V = 1496.25(13) ?³; II: Pbca, a = 14.1424(4) ?, b = 6.0957(2) ?, c = 33.1458(11) ?, V = 2857.43(16) ?³; III: P2 ₁ /c, a = 11.5155(4) ?, b = 6.0020(2) ?, c = 22.4645(8) ?, β = 103.002(4)°, V = 1512.85(9) ?³]. Index Abstract  Crystal structures from three Chalcones derived from 6-methoxy-2-naphthaldehyde are reported and their geometric and packing parameters described.     

The effect of organic linkers on the supramolecular structures of two new Ni(II) cyclen complexes (cyclen = 1,4,7,10-tetraazadodecane)

Two new nickel(II)(cyclen) coordination polymers, {[Ni(cyclen)·(bipy)]·(ClO₄)₂}_n (1) and [Ni(cyclen)]₂·(squa)·(ClO₄)₂ (2) have been synthesized and characterized structurally, where cyclen is 1,4,7,10-tetraazadodecane. Compound 1 crystallizes in the monoclinic system, space group C2/c, with a = 10.5339(17) ?, b = 14.565(2) ?, c = 16.133(3) ?, β = 102.799(2)°, V = 2413.4(7) ?³. Compound 2 crystallizes in the orthorhombic system, space group P _{nm a} with a = 25.722(3) ?, b = 11.1168(12) ?, c = 11.4580(13) ?, V = 3276.3(6) ?³. In both compounds, each Ni^II center is in a distorted octahedral coordinated environment with four N_cyclen atoms and two N_pyridine atoms from 4,4′-bipyridine linker for 1 and two O_aqueou atoms from the coordinated water for 2, respectively. The complex 1 exhibits infinite zigzag 1D chains by linking of 4,4′-bipyridine coordinated. In complex 2, 2D sheet supramolecule generated through self-assembling by hydrogen bond.     

Synthesis and crystal structure of Mn(II) and Zn(II) complexes with 1,3,5-tris(carboxymethoxyl)benzene ligand

Two complexes (H₂bipy)[M₂(TB)₂(H₂O)₈]·5H₂O (M = Mn 1, Zn 2) (bipy = 4,4′-bipyridine, H₃TB = 1,3,5-tris(carboxymethoxyl)benzene) were synthesized by the reaction of the corresponding metal salt with ligand H₃TB and 4,4′-bipy in an aqueous methanol solution at room temperature, respectively. Their structures were determined by single crystal X-ray diffraction analysis. Both complexes 1 and 2 crystallize in the triclinic space group with the crystal parameters of 1: a = 9.725(12) ?, b = 10.651(13) ?, c = 10.882(13) ?, α = 91.72(2)°, β = 96.41(2)°, γ = 97.72(2)°, V = 1109(2) ?³, Z = 1 and 2: a = 9.610(10) ?, b = 10.55(2) ?, c = 10.83(2) ?, α = 91.60(4)°, β = 95.32(2)°, γ = 97.73(4)°, V = 1082(3) ?³, Z = 1. Complexes 1 and 2 have the same dinuclear structure, in which each metal atom is six coordinated with distorted octahedral geometry by two oxygen atoms from two different TB³⁻ ligands and four ones from four coordinated water molecules. The dinuclear units are further linked by hydrogen bonding and π–π interactions to form the three-dimensional framework structure.     

Synthesis,characterization, and crystal structure of <Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">p</Emphasis>-nitrobenzoyl-<Emphasis Type="Italic">N</Emphasis>′-<Emphasis Type="Italic">p</Emphasis>-chlorophenylthiourea

N-p-nitrobenzoyl-N′-p-chlorophenylthiourea was synthesized and characterized by elemental analysis, IR and ¹H NMR etc. Single crystal structure of the title compound was determined on X-ray diffraction instrument. It is confirmed that the title compound crystallizes in monoclinic space group P2(1)/c, with a=8.5985(14) ?, b=12.1537(19) ?, c=14.972(2) ?, β=105.886(2)°, and D _calc=1.482 g/cm³ for Z=4. Intermolecular N–H⋯O H-bonds link pairs of two molecules. H-bonds and π-π stacking are the main non-bonding interactions in the molecular structure.     

Two Isostructural Complexes Constructed from Mixed Ligands of Dipyrido[3,2-d:2′,3′-f]quinoxaline and Phthalate with Novel Oxygen Clusters

Abstract Two isostructural dinuclear complexes [M₂(Dpq)₂(phth)₂(H₂O)₄] · 2H₂O [M = Zn(1), Ni(2), Dpq = dipyrido[3,2-d:2′,3′-f]quinoxaline, phth = phthalate] have been synthesized and characterized. Crystal data: (1), Mr = 1031.55, monoclinic, C2/c, a = 27.7948(11), b = 10.5196(4), c = 15.0390(5) ?, β = 110.818(1), Z = 4, V = 4110.2 ?³, R ₁ = 0.0277, wR ₂ = 0.0718 [I > 2σ(I)]; (2), Mr = 1018.19, monoclinic, C2/c, a = 27.675(4), b = 10.3601(15), c = 15.082(2) ?, β = 110.954(2), Z = 4, V = 4038.3 ?³, R ₁ = 0.0248, wR ₂ = 0.0668 [I > 2σ(I)]. The dinuclear units are connected into 2-D supramolecular net through O–H···O hydrogen bonding. Moreover, the 2-D networks are ultimately packed into a 3-D supramolecular structure via interlayer π···π stacking interaction between the aromatic rings of Dpq ligands. Furthermore, the photoluminescence property of compound 1 is also studied. Graphical Abstract Two isostructural dinuclear complexes [M₂(Dpq)₂(phth)₂(H₂O)₄] · 2H₂O [M = Zn(1), Ni(2), Dpq = dipyrido[3,2-d:2′,3′-f]quinoxaline, phth = phthalate] have been synthesized, and the structure study reveals that each dinuclear complex is connected with six other dinuclear units through the O–H···O hydrogen bonding to form 2-D supramolecular networks.      

Reaction of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne with Co(II) generates coordination monomers not polymers: Crystal structure of 4-(2,6-dicarboxypyridin-4-yl)ethynylpyridine-2,6-dicarboxylatotriaqua cobalt(II) monohydrate

Reaction and crystallization of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne with Co(II) produces crystals containing monomers of 4-(2,6-dicarboxypyridin-4-yl)ethynylpyridine-2,6-dicarboxylatotriaqua cobalt(II) monohydrate complex (1), [Co(C₁₆H₆N₂O₈)(H₂O)₃]·H₂O, instead of a rigid 1-D metal–organic framework consisting of a linear coordination polymer. This complex crystallizes in the monoclinic space group C2/c with a=6.8028(9) ?, b=36.781(5) ?, c=7.5135(9) 2.474(2)° and Z=4. The complex sits on a symmetry axis such that the two halves of the molecule are related by two-fold rotation symmetry. The molecules form layers in which the molecules are joined by intermolecular O–H⋯O interactions involving hydrogen bonds between CO₂H⋯CO₂ ⁻, H₂O⋯CO₂ ⁻, H₂O⋯CO₂H and H₂O⋯H₂O groups.Supplementary material CCDC-289569 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data request/cif, by e-mailing data request@ccdc.cam.ac.uk or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 IEZ, UK; fax: +44(0)1223-336033.     

Solvent-controlled structures. Synthesis and characterization of complexes Cu(L)2(CH3COO)2 and [Cu2(μ-CH3COO)4(L)2](L)2 [L = N-(4′-methylaniline)-4-pyridinecarboxamide]

Two complexes Cu(L)₂(CH₃COO)₂ (1) and [Cu₂(μ-CH₃COO)₄(L)₂](L)₂ (2) (L = N-(4′-methylaniline)-4-pyridinecarboxamide) have been prepared and their crystal structures have been determined by single-crystal X-ray diffraction. The complexes are obtained by using the same raw materials and reaction conditions except solvents. The presence or absence of water controls the coordination mode to give rise to different structures. The structure of 1 has a triclinic space group P-1 with a = 8.381(3) ?, b = 8.545(4) ?, c = 11.357(5) ?, α = 110.654(6)°, β = 102.388(7)°, γ = 97.889(7)°, V = 722.9(5) ?³, and Z = 1. The structure of 2 has a triclinic space group P-1 with a = 9.121(3) ?, b = 9.454(3) ?, c = 17.233(5) ?, α = 77.374(5)°, β = 89.827(6)°, γ = 74.342(6)°, V = 1393.8(7) ?³, and Z = 1. Supramolecular assemblies have also been found via noncovalent bonds such as hydrogen bonds, π–π stacking interactions.     

Synthesis, Crystal Structure and Magnetic Behaviour of {[Yb(1,4-BDC)1.5(H2O)4]·H2O}n (1,4-BDC?=?1,4-benzenedicarboxylate)

Abstract  

The title complex {[Yb(1,4-BDC)_1.5(H₂O)₄]·H₂O}_n (1) (1,4-BDC = 1,4-benzenedicarboxylate) has been hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. Crystals of compound 1 belongs to the triclinic crystal system, space group P-1; a = 7.549(3) ?, b = 10.072(4) ?, c = 10.470(4) ?, α = 87.810(4)°, β = 82.531(4)°, γ = 86.306(4)°, V = 787.3(5) ?³, Z = 2. The Yb(III) atoms are linked by the deprotonated 1,4-BDC ligands in two kinds of bridging modes. Four Yb(III) atoms at each corner (nodes) and four 1,4-BDC ligands at each edge (spacers) form a edge–sharing 36-membered rings. The rhombohedral Yb₄(1,4-BDC)₄ arranged in an alternating fashion to construct a 1D ladder-like chain along the c axis. Two neighboring chains are linked to each other in a parallel fashion to construct 3D supramolecular structure by O–H···O hydrogen bonds and π–π stacking interactions. In addition, the properties of thermogravimetric analysis and magnetic behaviors of the complex have been also discussed.     

Synthesis and crystal structure of a 2D (6,3) coordination network, {[Ag(L)1.5]NO3} n [L = 1,3-bis(benzylthio)propane]

A new dithioether silver(I) complex, {[Ag(L)_1.5]NO₃} _n (1) has been prepared by the reaction of AgNO₃ with 1,3-bis(benzylthio)propane (L) in methanol/chloroform. The structure was characterized by single-crystal X-ray diffraction analysis: rhombohedral system, space group R –3c, with a =b = 15.651(7), c = 39.26(4) Å, V = 8328(1) ų, and Z = 6. The crystal structure consists of [Ag(L)_1.5]⁺ cations and NO₃ ^– anions. In 1, each silver(I) center is coordinated equivalently to three sulfur donors from three different ligands to give a trigonal-planar coordination geometry. Each L links two adjacent silver(I) centers in bis-monodentate bridging mode to form a 2D (6,3) network sheet. Furthermore, these 2D sheets are linked by the weak coordination interactions between nitrate ions and silver(I) atoms to form a 3D brick-wall framework.     

X-ray diffraction study of R2[UO2(C3H2O4)2] ·H2O (R = K or Rb)

Compounds K₂[UO₂(C₃H₂O₄)₂] · H₂O (I) and Rb₂[UO₂(C₃H₂O₄)₂] · H₂O (II) are synthesized and their crystal structures are determined by X-ray diffraction. The compounds crystallize in the monoclinic crystal system; for I, a = 7.1700(2) ?, b =12.3061(3) ?, c = 14.3080(4) ?, β = 95.831(2)°, space group P2₁/n, Z = 4, and R = 0.0275; for II, a = 7.1197(2) ?, b = 12.6433(4) ?, c = 14.6729(6) ?, β = 96.353(2)°, space group P2₁/n, Z = 4, and R = 0.0328. It is found that I and II are isostructural. The main structural units of the crystals are the [UO₂(C₃H₂O₄)₂]²⁻ chains, which belong to the AT ¹¹ B ⁰¹ (A = UO₂²⁺, T ¹¹, and B ⁰¹ = C₃H₂O₄²⁻) crystal chemical group of uranyl complexes. The chains and alkali metal ions R (R = K or Rb) are connected by electrostatic interactions and hydrogen bonds. Some specific structural features of [UO₂(C₃H₂O4)₂]²⁻ complex groups are discussed.     

Reaction of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne and imidazole with Cu(II) generates a discrete complex not a coordination polymer: crystal structure of [μ-4,4′-(1,2-ethynediyl)-bis(pyridine-2,6-dicarboxylato)-N,O, O′-μ-N′, O′′, O′′′]-diaqua-bis(imidazole)-dicopper(II)

Reaction of 1,2-bis(2,6-dicarboxypyridin-4-yl)ethyne and imidazole with Cu(II) produces crystals containing a discrete complex of [μ-4,4′-(1,2-ethynediyl)-bis(pyridine-2,6-dicarboxylato)-N, O, O′-μ-N′, O′′, O′′′]-diaqua-bis(imidazole)-dicopper(II) complex (1), [(C₁₆H₄N₂O₈)(C₃H₄N₂)₂(H₂O)₂Cu₂] instead of a linear coordination polymer. The complex crystallizes in the monoclinic space group P2₁/n with a = 5.3763(8) ?, b = 18.522(3) ?, c = 11.4827(7) ?, β = 93.705(3) ° and Z = 2. The complex sits on a center of symmetry such that the two halves of the molecule are related by inversion symmetry. The molecules pack in layers in which the molecules are joined by intermolecular N–H⋯O hydrogen bonds between imidazole and carboxylate groups and O–H⋯O hydrogen bonds between carboxylate groups and water.     

Synthesis and crystal structure of Cu3(Bipy)2(L1)2(L2)2? 4H2O(Bipy = 2,2′-bipyridine, L1 =1-((2-sulfonateethylimino)methyl)-2-naphthol), L2 = 2-hydroxy-1-naphthaldehyde)

The title compound, Cu₃(Bipy)₂(L¹)₂(L²)₂⋅4H₂O, was synthesized in the methanol solution of Bipy and Cu(II) in the presence of 1-((2-sulfonate-ethylimino)-methyl)-2-naphthol (L¹), which was condensation compound of taurine and 2-hydroxy-1-naphthaldehyde. This complex crystallized in the space group P-1 with a = 9.825(2) ?, b = 12.626(2) ?, c = 14.342(3) ?, α = 90.29(1)^∘, β = 100.67(1)^∘, γ = 101.67(2)^∘, and Z = 2. In the trinuclear Cu(II) complex, there are two type Cu atoms which have square and square pyramid geometries, respectively. The Cu–N distances vary from 1.965(3) to 2.000(4) ?, while the Cu–O distances are between 1.896(3) and 2.337(4) ?.     

Structures and Characterization of [Zn(n-chlorosalicylato)2(N-methylnicotinamide)2(H2O)2] (n?=?4 or 5) Ligand Isomers

Abstract  

Two ligand isomers [Zn{4-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (I) and [Zn{5-ClC₆H₃-2-(OH)COO}₂(Menia)₂(H₂O)₂] (II) (Menia = N-methylnicotinamide) were prepared and characterized by elemental analysis, IR spectroscopy and thermal analysis. The X-ray crystal structures of complexes (I) and (II) were determined. Compound (I) crystallizes in the triclinic space group P[`1] P\bar{1} with a = 8.105(1) ?, b = 10.036(2) ?, c = 10.545(2) ?, α = 109.088(9)°, β = 91.416(8)°, γ = 102.757(9)°, V = 786.2(2) ?<sup>3</sup>, Z = 1. Compound (II) crystallizes in the triclinic space group P[`1] P\bar{1} . Its cell parameters are: a = 8.133(1) ?, b = 10.119(2) ?, c = 10.428(1) ?, α = 66.44(1)°, β = 74.32(1)°, γ = 80.16(1)°, V = 755.5(2) ?³, Z = 1. The molecular structure of both isomers is monomeric. Each Zn(II) atom is hexacoordinated by three pairs of unidentate ligands in trans-positions (ZnO₄N₂). The 5-Clsal complex is somewhat less distorted than 4-Clsal complex (Cl-sal = chlorosalicylate). The structural data are compared with those found in similar [Zn(RCOO)₂(NL)₂(H₂O)₂].