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, Crystal Structure of a New Co(II) Complex with Pyrazine-2,3,5,6-tetracarboxylic Acid

Abstract A new complex [Co(H₂pztc)(bpy)H₂O] (H₄pztc = pyrazine-2,3,5,6-tetracarboxylic acid, bpy = 2,2′-bipyridine) has been synthesized by hydrothermal reactions of Co(NO₃)₂ · 6H₂O with H₄pztc and bpy and characterized by IR and X-ray diffraction single crystal structure analysis. It belongs to monoclinic system, P2₁/c space group with a = 13.454(2) ?, b = 12.939(2) ?, c = 11.4993(19) ?, α = 90°, β = 111.640(3)°, γ = 90°. This complex is assembled into 3D supramolecular architecture by hydrogen bonds (O–H···O, C–H···O). Index Abstract A new complex of cobalt(II) with pyrazine-2,3,5,6-tetracarboxylic acid and 2,2′-bipyridine is assembled by intermolecular hydrogen bonds forming 2D layer and 3D supramolecular network.      

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 Structures of Ternary Copper(II) Complex Containing Salicylaldehyde Schiff Base and 4,4′-Bipyridine

Abstract  A new ternary mixed-ligand complex [Cu₂(sal-glu)₂(bipy)(H₂O)₂] · (H₂O) (bipy = 4,4′-bipyridine and sal-glu = salicylaldehyde l-glutamic Schiff base) has been synthesized and characterized by X-ray diffraction. It crystallizes in the triclinic system, space group P-1 with a = 9.6199(13) ?, b = 9.9111(13) ?, c = 9.9167(13) ?. The amino acid Schiff base coordinates to the Cu(II) ion in a tridentate mode including phenol-hydroxyl oxygen, carboxyl oxygen and amide nitrogen atom, while the bipy coordinates in bidentate bridging mode linking two Cu(II) ions. The [Cu₂(sal-glu)₂(bipy)(H₂O)₂] units are linked into 1-D chain structure and the bipy molecules are interspersed into parallel sheets via intermolecular hydrogen bonds. The carboxyl oxygen atoms, phenolic oxygen atoms and water oxygen atoms are involved in the extensive intermolecular hydrogen bond network between the water molecules and phenol-hydroxyl oxygen atoms from salicylaldehyde derived ligand. Graphical Abstract  A new ternary mixed-ligand complex [Cu₂(sal-glu)₂(bipy)(H₂O)₂]·(H₂O) (bipy = 4, 4′-bipyridine and sal-glu = salicylaldehyde l-glutamic Schiff base) crystallizes in the triclinic system, space group P-1 with a = 9.6199(13) ?, b = 9.9111(13) ?, c = 9.9167(13) ?. The amino acid Schiff base coordinates to the Cu(II) ion in a tridentate mode including phenol-hydroxyl oxygen, carboxyl oxygen and amide nitrogen atom, while the bipy coordinates in bidentate bridging mode linking two Cu(II) ions. The [Cu₂(sal-glu)₂(bipy)(H₂O)₂] units are linked into 1-D chain structure and the bipy molecules are interspersed into parallel sheets via intermolecular hydrogen bonds. The carboxyl oxygen atoms, phenolic oxygen atoms and water oxygen atoms are involved in the extensive intermolecular hydrogen bond network between the water molecules and phenol-hydroxyl oxygen atoms from salicylaldehyde derived ligand.      

Two new CrIII(bpb)(H2O)X complexes derived from [Cr(bpb)(N3)2]− or [Cr(bpb)(CN)2]− (bpb2− = 1,2-bis(pyridine-2-carboxamido)benzenate, X− = hydroxo or azide)

Two new Cr(III) complexes, [Cr(bpb)(H₂O)(OH)]·3H₂O (1) and [Cr(bpb)(H₂O)(N₃)]·H₂O (2) have been synthesized and structurally characterized. Both complexes were unexpectedly obtained as single crystals during the reactions of [Cr(bpb)(CN)₂]⁻ or [Cr(bpb)(N₃)₂]⁻ with [Ni(L)](ClO₄)₂ (L = 3,10-dimethyl-1,3,6,8,10,12-hexaazacyclotetradecane) or MX₂·nH₂O (M = Cu, Ni and Mn, X = Cl⁻ and ClO₄ ⁻). Complex 1 crystallizes in the triclinic system, space group P-1, formula CrC₁₈H₂₁N₄O₇ with a = 7.1543(17) ?, b = 12.420(3) ?, c = 12.955(3) ?, α = 115.021(5)°, β = 95.544(5)°, and γ = 101.575(5)°. Complex 2 crystallizes in the monoclinic system, space group P2₁/c, formula CrC₁₈H₁₆N₇O₄ with a = 11.7171(9) ?, b = 9.4999(7) ?, c = 16.8799(13) ?, and β = 97.449(2)°. Both complexes exhibit distorted octahedral coordination environment with four nitrogen atoms of bpb²⁻ situated at the equatorial plane (Cr–N bond distances range from 1.961(3) to 2.1088(15) ?), and the remaining two trans-positions occupied by terminal ligands H₂O/HO and H₂O/N₃ in 1 and 2, respectively. It is noteworthy that a hydrogen-bonded folded ladder-like structure involving twelve O atoms in 1 and a chair-like hexagonal hydrogen-bonded cluster containing six O atoms are formed.     

Synthesis,Characterization and Fluorescent Property of Two Mixed Ligand Coordination Polymers Constructed from 4-Cyclohexene-1,2-dicarboxylate and Nitrogen-Containing Ligands

Abstract  

Two new coordination polymers [Cd(1,2′-cy)(btx)_0.5H₂O]_n 1 and {[Ni(1,2-cy)(2,2′-bipy)(H₂O)₂]·3H₂O}_n 2 (1,2′-cy=4-cyclohexene-1,2-dicarboxylate, btx=1,4-bis(triazol-1-ylmethyl)benzene, 2,2′-bipy=2,2′-bipyridine) had been synthesized. Their structures were characterized by elemental analysis, IR, TG and X-ray single-crystal diffraction analysis. Crystal data for complex 1: Triclinic, space group P-1, a = 6.4303(13) ?, b = 10.399(2) ?, c = 11.713(2), α = 83.04(3)°, β = 81.87(3)°, γ = 83.84(3)°, and Z = 2. For complex 2: Orthorhombic, space group Pbcn, a = 15.613(3) ?, b = 13.970(3) ?, c = 21.290(4) ?, and Z = 4. Complex 1 exhibits an interesting two-dimensional wavelike covalent layer structure. When Ni salt was replaced by Cd salt, and reacts with 1,2′-cy and 2,2′-bipy, one-dimensional chain-like complex 2 was obtained. Furthermore, the fluorescent property of complex 1 was reported.     

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.     

Syntheses and Crystal Structures of Two New Cadmium(II) and Nickel(II) Complexes with 1,4-Phenylenediacetate and 2,2′-Bipyridyl-Like Ligands

Abstract  

Two new complexes, namely [Cd(PDA)_0.5(2,2′-bpy)Cl](H₂PDA) (1) and [Ni(PDA)(phen)(H₂O)]₂ (2) (H₂PDA = 1,4-phenylenediacetic acid, 2,2′-bpy = 2,2′-bipyridine, phen = 1,10-phenanthroline), have been synthesized and characterized by elemental analysis, IR spectra and X-ray crystal diffraction. Single-crystal X-ray diffraction analysis shows that complex 1 crystallizes in the triclinic space group P-1 with unit cell dimensions a = 8.760 (4) ?, b = 11.190 (5) ?, c = 13.917 (7) ?, α = 110.383 (5)°, β = 101.736 (5)°, γ = 100.612 (5)°, V = 1202.8 (10) ?³, Z = 2, R ₁ = 0.0314 and wR ₂ = 0.0898. Complex 2 crystallizes in the monoclinic space group P2(1)/n with unit cell dimensions a = 9.911 (3) ?, b = 17.924 (6) ?, c = 10.638 (4) ?, β = 94.998 (5)°, V = 1882.7 (11) ?³, Z = 2, R ₁ = 0.0397 and wR ₂ = 0.1150. In complex 1, Cd(II) ions are alternately bridged by PDA ligands and chloride ions into 1D chains and the PDA ligands display trans-configuration. Complex 2 is a dimer and two Ni(II) ions are linked by two PDA ligands with cis-configuration, resulting in a cyclic structure. In spite of these differences, both in complexes 1 and 2 there are π–π stacking interactions and hydrogen bonding to make them 3D supramolecular frameworks.     

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 and Crystal Structure of the Coordination Polymer [Cu(ppca′)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)(HgI<Subscript>2</Subscript>)](H<Subscript>2</Subscript>O) (ppca′ = 3,4′-bipyridine-6-carboxylic acid)

Abstract  

The coordination complex Cu(ppca′)₂(H₂O)₂ (1) was synthesized hydrothermally using the ligand 3,4′-bipyridine-6-carboxylic acid (ppca′). Complex 1 consists of pseudo-octahedral copper (II) units hydrogen bonded into a three-dimensional network that crystallizes in the monoclinic P2₁/n space group. In complex 1, a = 5.3429(4) ?, b = 29.343(2) ?, c = 6.7940(5) ?, and β = 110.635(2)°.     

Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium Perchlorate Dihydrate

Abstract The crystal structure of 4,4′-bipyridin-1-ium perchlorate dihydrate, [C₁₀H₉N₂](ClO₄) · 2H₂O, is determined by room temperature X-ray diffraction. The compound crystallizes in the triclinic space group P-1 with a = 8.122(3) ?, b = 9.726(3) ?, c = 17.648(6) ?, α = 78.181(4)°, β = 82.797(5)°, γ = 67.439(4)°, Z = 2, V = 1258.4(7) ?³. In the compound, monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds in a head-to-tail fashion. The chains are stacked via π–π stacking interactions to create two-dimensional sheets. The interlayer space is occupied by the hydrogen-bonded water chains that are linked to the organic sheets via C–H···O interactions and the perchlorate anions that are linked to the water chains and the organic sheets via O–H···O and C–H···O hydrogen bonds, respectively, thus generating a three-dimensional supramolecular architecture. Index Abstract Supramolecular Network via Hydrogen Bonding and π–π Stacking in 4,4′-Bipyridin-1-ium perchlorate dihydrate Jian-Yong Zhang, Ai-Ling Cheng and En-Qing Gao* Monoprotonated 4,4′-bipyridin-1-ium cations are self-assembled into supramolecular chains along the a-axis through N–H···N hydrogen bonds, and these chains are stacked via π–π stacking and hydrogen bond interactions involving water molecules and perchlorate anions.      

Supramolecular Cobalt(II), Copper(II) and Cadmium(II) Complexes Obtained from a Proton Transfer Compound including Pyridine-2,6-dicarboxylate and Propane-1,3-diaminium Ions; Synthesis,Characterization and Crystal Structure

Abstract The three complexes (pnH₂)[Co(pydc)₂]·4H₂O 1, (pnH₂)[Cu(pydc)₂]·4H₂O 2, and (pnH₂)[Cd(pydc)₂]·3.5H₂O 3 (pn: propane-1,3-diamine, pydc: pyridine-2,6-dicarboxylate) were prepared using a proton transfer compound (pnH₂)(pydc)·(pydcH₂)·2.5H₂O, LH ₂ and corresponding metallic salts. The characterization was carried out using elemental analysis, IR and NMR spectroscopy, and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in space group P , but complex 3 crystallizes in space group P2/c. Cell parameters of the complexes are a = 8.449(1) ?, b = 11.668(1) ?, c = 12.801(1) ?, α = 115.748(2)°, β = 93.038(2)°, γ = 97.867(2)° for 1; a = 7.973(2) ?, b = 16.632(2) ?, c = 25.280(5) ?, α = 94.178(6)°, β = 95.186(6)°, γ = 91.603(5)° for 2 and a = 20.055(1) ?, b = 13.8161(9) ?, c = 8.2418(5) ?, β = 100.086(1)° for 3. The three crystal structures illustrate that the metal ion is six-coordinated by two pydc’s. In structures of 2 and 3, it can be seen that propane-1,3-diaminium fragments have different conformations. The complexes have ion-pairing interactions, O–H···O, N–H···O and C–H···O hydrogen bonds, π–π stacking as well as van der Waals forces as the main factors in formation of their supramolecular structures. Index Abstract Supramolecular Cobalt(II), Copper(II) and Cadmium(II) Complexes Obtained from a Proton Transfer Compound including Pyridine-2,6-dicarboxylate and Propane-1,3-diaminium Ions; Synthesis, Characterization and Crystal Structure Hossein Aghabozorg, Mohammad Ghadermazi,Bahar Nakhjavan, Faranak Manteghi The synthesis, characterization, crystal structure and non-covalent interactions of three supramolecular complexes of Co(II), Cu(II) and Cd(II) obtained by the reaction of a proton transfer compound i.e. (pnH₂)(pydc)·(pydcH₂)·2.5H₂O with the corresponding metallic salts are reported. 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 Double-Chain Coordination Polymer [Zn<Subscript>2</Subscript>(bipy)<Subscript>2</Subscript>(btec)(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>]<Subscript>n</Subscript> (bipy = 2,2′-bipyridine; btec = 1,2,4,5-benzenetetracarboxylate)

Abstract  A novel aromatic polycarboxylate polymer, [Zn₂(bipy)₂(btec)(H₂O)₂]_n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. Compound 1 belongs to the triclinic crystal system, space group P-1; a = 7.7449(6) ?, b = 8.9286(8) ?, c = 10.7422(8) ?, α = 80.95(1)°, β = 70.21(1)°, γ = 78.14(1)°, V = 680.93(10) ?³, Z = 2. The coordination geometry of Zn(II) atom is distorted trigonal bipyramidal with two nitrogen atoms of one 2,2′-bipy group, two oxygen atoms from two different btec ligands, and one water. The 16-membered rings are alternately arranged forming an infinite 1-D double-chain structure. A 3-D network was constructed by interlayer C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state. Graphical Abstract  A 1-D double-chain aromatic polycarboxylate polymer, [Zn₂(bipy)₂(btec)(H₂O)₂]_n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. A 3-D network was constructed by intermolecular C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.      

Syntheses and crystal structures of an organometallic thiosemicarbazone and an organometallic enehydrazide

Reactions of ferrocenoylacetone with thiosemicarbazide and isonicotinic acid hydrazide generate an organometallic thiosemicarbazone 1 and enehydrazide 2, respectively. The complexes 1 and 2, which can be formulated as [C₅H₅FeC₅H₄C(O)CH₂C(=NNHCSNH₂)CH₃] and [C₅H₅FeC₅H₄C(O)CH=C(NHNHCOC₅H₄N-4)CH₃], have been characterized by elemental analyses, IR, NMR, UV and were structurally characterized by single-crystal X-ray crystallography. Complex 1 (C₁₅H₁₇FeN₃OS) crystallizes in the monoclinic space group P2₁/c, with lattice constants: a = 13.939(3) ?, b = 8.2600(17) ?, c = 13.176(3) ?, β = 94.83(3)°, V = 1511.7(6) ?³, Z = 4, D _c = 1.508 g cm⁻³, F(000) = 712, R ₁ = 0.0602, wR ₂ = 0.1526. Two intermolecular hydrogen bonds N–H···S (N···S = 3.356(8) and 3.499(7) ?, N–H···S = 168 and 170°) form a chain in the [010] direction. The intermolecular hydrogen bond C–H···O (C···O = 3.432(10) ?, C–H···O = 151°) leads to a [010] double-chain through each unit cell. The intermolecular hydrogen bond C–H···O (C···O = 3.359(10) ?, C–H···O = 173°) makes the [010] double-chain pack along the c axis to result in a two-dimensional network. Complex 2 (C₂₀H₁₉FeN₃O₂) crystallizes in the monoclinic space group P2₁/c, with lattice constants: a = 14.091(2) ?, b = 10.024(2) ?, c = 13.806(2) ?, β = 112.41(2)°, V = 1802.8(6) ?³, Z = 4, D _c = 1.434 g cm⁻³, F(000) = 808, R ₁ = 0.0576, wR ₂ = 0.1593. The strong intramolecular hydrogen bond N–H···O from the enamine N atom and carbonyl O atom stabilizes the enehydrazide. The intermolecular hydrogen bonds N–H···O and C–H···O (N···O = 2.906(6) ?, N–H···O = 155° C···O = 3.364(6) ?, C–H···O = 153°) generate a [010] chain. The intermolecular hydrogen bond N–H···O (N···O = 2.989(6) ?, N–H···O = 128°) forms a [010] double-chain through each unit cell. The π···π stacking interation involving the pyridyl groups makes the [010] double-chain pack along the c axis to lead to a two-dimensional network.     

F-type or T-type Aromatic–Aromatic Interaction in Two Isoflavone Derivatives

Abstract Two isoflavone derivatives, 5,6,7,4′-tetramethoxyisoflavone (I) and 6,4′-dimethoxy- 7-ethoxy-5-hydroxylisoflavone (II), have been synthesized and their crystal structures were determined by ¹H NMR and single crystal X-ray diffraction studies. I is triclinic, space group P-1 with a = 7.828(1) ?, b = 10.285(2) ?, c = 11.608(2) ?, α = 104.90(2)°, β = 110.546(9)°, γ = 99.54(1)° and Z = 2. II is orthorhombic, space group Pna2 ₁ with a = 7.0244(6) ?, b = 15.0104(15) ?, c = 15.7538(15) ?, and Z = 4. Molecules of I are linked into two-dimensional structure by a combination of C–H···O hydrogen bond and F-type aromatic–aromatic interactions. II shows some discrepancies with I and the molecules are linked into columns by T-type aromatic-aromatic interaction. Graphical Abstract F-type or T-type Aromatic–Aromatic Interaction in Two Isoflavone Derivatives Zun-Ting Zhang,* Xue-Ling Zhang Molecules of 5,6,7,4′-tetramethoxyisoflavone are linked into two-dimensional structure by a combination of C–H···O hydrogen bond and F-type aromatic–aromatic interactions; 6,4′-dimethoxy-7-ethoxy-5-hydroxylisoflavone shows some discrepancies with 5,6,7,4′-tetramethoxyisoflavone and the molecules are linked into columns by T-type aromatic–aromatic interaction.      

Histamine Molecule and Dianion Oxalate are Efficient Blocks for Building 2D Supramolecular Networks

Abstract  

One salt and two Cu(II) complexes (H₂hsm)(ox), 1, [Cu(hsm)(ox)], 2, and [Cu(hsm)(ox)H₂O], 3, have been synthesized and X-ray characterized (hsm is histamine and ox²⁻ is the oxalate dianion). Starting from the prochiral tetracoordinated complex 2, pentacoordinated complex 3 crystallizes as a racemic mixture of the enantiomeric Δ and Λ isomers, in space group P2₁/c. In all cases, the side chain of the hsm group is gauche, allowing the formation of strong hydrogen bonds in the salt 1, and to chelate the metal center in complexes 2 and 3. The combination hsm/ox seems to favor the formation of 2D supramolecular structures (planes or wavy planes), through efficient networks of N–H···O hydrogen bonds. Cell parameters: 1, P2₁/c, a = 6.260 (2) ?, b = 11.500 (4) ?, c = 12.525 (4) ?, β = 104.047 (17)o; 2, C2/c, a = 10.7966 (13) ?, b = 15.5622 (16) ?, c = 11.3996 (15) ?, β = 106.261 (11)o; 3, P2₁/c, a = 7.0627 (6) ?, b = 7.1323 (6) ?, c = 20.0296 (19) ?, β = 91.529 (7)o.     

Synthesis and structural characterization of the dinuclear bis(glutarato)bis(urea)copper(II)complex, dihydrate

The complex [Cu(OOC-(CH₂)₃-COO)(O=C(NH₂)₂]₂·2H₂O has been synthesized and characterized by X-ray crystallography. It crystallizes in the triclinic system P-1 with a = 8.003(2) ?, b = 8.611(2) ?, c = 8.620(2) ?, α = 96.14(3)°, β = 116.66(2)°, γ = 105.66(4)° and V = 492.9(3) ?³. The structure consists of discrete centrosymmetric binuclear units and water molecules. The Cu(II) ions adopt a square-pyramidal coordination with four oxygen atoms of four bridging carboxylate and one carbonyl oxygen of the monodentate urea ligand. There is a very strong interaction between the two copper centers in binuclear entities (CuCu: 2.6266(15) ?).     

Copper(II) and lead(II) complexes of 4,4′-bipyridine-<Emphasis Type="Italic">N,N</Emphasis>′-dioxide

Cu(II) and Pb(II) complexes of 4,4′-bipyridine-N,N′-dioxide have been prepared using a solvent-layering system. [Cu₂Cl₄(bpdo)₃(H₂O)₂] . 2(CH₃)₂SO (1) crystallises in P-1, a=8.731(2), b=8.943(2), c=14.408(3) ?, α=102.85(3), β=97.49(3), γ=109.77(3)°. The Cu(II) complex is a z-shaped discrete molecule with a DMSO molecule hydrogen bonded to the host through coordinated water molecule. Crystallisation of PbCl₂, PbBr₂ and PbI₂ with bpdo afforded isostructural 2D coordination polymers. [PbCl₂(bpdo)]_n is monoclinic, C2/c with a=16.3274(7), b=4.0708(1), c=18.6146(8) ?, β=93.73(1)°; [PbBr₂(bpdo)]_n is monoclinic, C2/c with a=16.403(3), b=4.2412(8), c=18.846(4) ?, β=92.59(3)° and [PbI₂(bpdo)]_n is monoclinic, C2/c with a=16.438(3), b=4.538(1), c=18.973(4) ?, β=91.04(3)°. The adjacent metal centres of these polymers are bridged by coordinated Cl⁻, Br⁻ or I⁻ anions as well as by bpdo ligands. These polymers possess no conventional hydrogen bonds.     

Crystal and Molecular Structure of the 1:2 Adduct Formed Between <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Butylenebis(imidazole) and Carboxylic Acid Derivatives

Abstract  

Two imidazolyl derived complexes [N,N′-butylenebis(imidazole): (fumaric acid)₂ (1), and N,N′-butylenebis(imidazole): (2,4,6-trinitrophenol)₂ (2)] were prepared and structurally characterized by X-ray crystallography. Compound 1 crystallizes in the triclinic, space group P−1, with a = 5.9990(12) ?, b = 8.1772(16) ?, c = 10.419(2) ?, α = 86.88(2)°, β = 84.73(3)°, γ = 77.03(4)°, V = 495.67(17) ?³, Z = 1. For 1, two dimensional network structure is formed through imidazolium moieties forming hydrogen bonds to di-ionic carboxylate groups of fumarate chains. In the same network layers and adjacent layers, C–H···O contact also accompanies the N⁺–H···O⁻ hydrogen bonds, all these lead the extended architecture to show a three-dimensional lamellar structure. Compound 2 crystallizes in the triclinic, space group P − 1, with a = 7.0236(14) ?, b = 8.2831(17) ?, c = 12.053(2) ?, α = 106.05(4)°, β = 99.13(2)°, γ = 98.84(3)°, V = 650.8(2) ?³, Z = 1. In 2, two parallel imidazolium cations and two antiparallel 2,4,6-trinitrophenolate anions formed 32-membered rings through hydrogen bonding interaction, these rings extended along the c axis direction to form one dimensional railway structure. Adjacent parallel railways connect further through C–H···O hydrogen bonds between the 2-CH of the imidazole ring and the NO₂ group O atoms. These weak interactions combined, the complex showed 3D layer structure.     

The crystal structure of a bis(2,6-pyridinedicarboxylato)chromate(III) anion with an elaborate network of hydrogen bonding and π stacking

The synthesis, X-ray crystallography, spectroscopic, and electrochemical properties of the title compound, [Hdpa][Cr(dipic)₂]·3H₂O, 1, are reported. Compound 1 crystallized in the triclinic space group P-1 with a = 7.1057(11) ?, b = 12.965(2) ?, c = 14.269(2) ?, α = 80.306(3)°, β = 82.101(2)°, γ = 83.799(2)°, and V = 1278.6(4) ?³ with Z = 2. The distorted octahedral chromium anions are part of an elaborate network of hydrogen bonding formed by the waters of solvation, the anion, and cation as well as π-stacking interactions.