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.      

Novel Assembly of a Cyanide-Bridged Copper(II)–Nickel(II) Binuclear Complex with a Copper(II) Macrocyclic Ligand

Abstract  

A mononuclear fragment [Cu(L)Cl]ClO₄ (1) and a cyano-bridged Cu^II–Ni^II binuclear complex [CuL][Ni(CN)₄]·0.25H₂O (2) (L = 1,3,6,8,11,14-hexaazatricyclo[12.2.1.18,11]-octadecane), have been prepared and characterized. X-ray single crystal analyses indicate that the both complexes crystallize in the monoclinic crystalline system. The complex of 1 in P1n1 space group with unit cell constants a = 6.1176(6) ?, b = 11.9147(10) ?, c = 12.2041(12) ?, β = 98.816(5)° and 2 in the P2₁/n space group with unit cell constants a = 8.1419(13) ?, b = 14.695(2) ?, c = 16.863(3) ?, β = 98.375(2)° have been revealed. The complex 2 assumes a binuclear structure in which the nickel(II) ion is in a square planar environment and the copper(II) is in a square-prism geometry environment.     

Two-Dimensional Hydrogen-Bonded Polymer from Nickel(II) Tetraaza Macrocyclic Complex and Succinate Ligand

Abstract  

The reaction of [Ni(L)]Cl₂·2H₂O (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12] docosane) with succinic acid (C₄H₆O₄) yields a 2D hydrogen-bonded polymer with formula [Ni(L)(C₄H₅O₄)₂] (1). This polymer complex has been characterized by X-ray crystallography, spectroscopy and cyclic voltammetry. The complex has a center of symmetry. The crystal structure of 1 exhibits a distorted octahedral geometry about Ni atom with four nitrogen atoms of the macrocycle and two oxygen atoms of the succinate ligand at the trans position. Compound 1 crystallizes in the monoclinic system C2/c with a = 14.8203(11), b = 12.3070(8), c = 17.4164(12) ?, β = 107.356(6)°, V = 3032.1(4) ?³, Z = 4. Electronic spectrum of 1 reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes two waves of a one-electron transfer corresponding to Ni^II/Ni^III and Ni^II/Ni^I processes.     

Synthesis and Crystal Structure of a New Mo(V) Complex of Cyano Ligands

Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, (teta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene), has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction: monoclinic, space group P2(1)/c with a = 10.8553(8) ?, b = 12.4854(8) ?, c = 22.6348(15) ?, α = 90.00°, β = 97.3080(10)°, γ = 90.00°, Mr = 609.63, v = 3042.8(4), Z = 4. There are one [H₃teta]³⁺, one [Mo(CN)₈]³⁻ and one water molecule in the asymmetric unit. The complex is interconnected through hydrogen bond and formed into a 3D porous network. Graphical Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction. And it shows a 3D porous network through hydrogen bonds.      

Synthesis,Crystal Structure and Thermal Properties of <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline and <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline

Abstract  

Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, ¹H-NMR, ¹³C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C₁₉H₁₈N₂O₂Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C₁₉H₁₈N₂OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions.     

Dihydrogen Phosphate and Hydrogen Sulphate of 1,4-Dimethyl-1,4-diazabicyclo[2.2.2]octane-1,4-diium: Crystal Structures, Hydrogen Bonding and Infrared Spectra

Abstract  

The crystal structures of the title compounds consist of 1,4-dimethyl-1,4-diazabicyclo[2.2.2]octane-1,4-diium cation [C₈H₁₈N₂]²⁺ and [H₂PO₄]⁻ or [HSO₄]⁻ anions. Both crystal structures are monoclinic, the structure of the dihydrogen phosphate (I) is non-centrosymmetric (P2₁) with a = 6.4090(2) ?, b = 13.6920(5) ?, c = 7.6140(3) ?, β = 94.620(2)°, V = 665.97(4) ?³, Z = 2; whereas the unit cell of the hydrogen sulphate (II) is centrosymmetric (P2₁/c) with a = 13.8460(2) ?, b = 12.6610(2) ?, c = 8.0360(2) ?, β = 99.5800(12)°, V = 1389.10(5) ?³, Z = 4. Both the structures are formed by the different bonding patterns of the anions interlinked by strong and moderate O–H···O hydrogen bonds. While the structure of (I) consists of a two-dimensional network of the hydrogen bonded dihydrogen phosphates, the infinite chains of the hydrogen bonded hydrogen sulphates are the basic building unit of the structure (II). In addition to the dominant electrostatic interaction the divalent cations stabilize themselves in the structures by forming several C–H···O hydrogen bonds to the oxygen atoms of the anions. The IR spectra of both the compounds are strongly affected by the hydrogen bonds whose influence on OH stretching vibrations is analysed by means of the DFT calculations in the solid state.     

Synthesis and Crystal Structure of [Na(H<Subscript>2</Subscript>O)<Subscript>1.5</Subscript>][Na(H<Subscript>2</Subscript>O)<Subscript>3.5</Subscript>] X<Subscript>2</Subscript>·2H<Subscript>2</Subscript>O (X = 4′-Methoxy-7-Hydroxyisoflavone-3′-Sulfonate)

Abstract  

Water-soluble derivative of formononetin, [Na(H₂O)_1.5][Na(H₂O)_3.5] X₂·2H₂O(X = 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate) was synthesized by sulfonation reaction. It was characterized by IR, ¹H NMR and single-crystal X-ray diffraction analysis. Single-crystal X-ray diffraction analysis showed that the title compound crystallized in a triclinic space group P-1 with cell parameters a = 6.9642(15) ?, b = 13.343(3) ?, c = 20.634(5) ?, α = 107.115(3)˚, β = 93.121(4)˚, γ = 91.911(3)˚, V = 1827.3(7) ?⁻³, D _c  = 1.575 Mg m ⁻³, Z = 2. There are two conformers of 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate anions, two kinds of sodium cations, five coordinated water molecules and two lattice water molecules in the crystal structure. The sodium atoms coordinated with the oxygen atoms from water molecules, hydroxyl groups and sulfo-groups to form a Na–O coordinated network. Aromatic π···π stacking interactions and hydrogen bonding existed in the crystal structure of title compound, which together with coordinated interactions and electrostatic interactions between sodium cations and anions sulfonates C₁₆H₁₀O₄SO₃ ⁻ lead to the moieties into a three-dimensional network.     

Structure and Antibacterial Activity of 3-(3,4-Dimethoxyphenyl)furan-2(5<Emphasis Type="Italic">H</Emphasis>)-ones

Abstract  

Crystalline hydrate of the title compound (5), C₁₉H₂₆N₂O₅·2(H₂O), was structurally characterized by single crystal X-ray diffraction. It crystallizes in monoclinic system space group P 21/c with a = 7.3987(7) ?, b = 17.8691(16) ?, c = 17.0022(13) ?, β = 112.944(3)°, V = 2070.0(3) ?³, Z = 4, R ₁ = 0.0592, wR ₂ = 0.1016, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with 3,4-dimethoxybenzene ring, making a dihedral angle of 0.860(69)°. Two kinds of centrosymmetric tetramers characterized by graph-set motifs of R ₇⁸(36) and R ₄⁶(32) are formed through O–H···O, O–H···N and C–H···O hydrogen bonding interactions, which generate a sheet of edge-fused rings parallel to the (011) plane. These sheets are further linked into a three dimensional network by C–H···π interactions. Nine 3-(3,4-dimethoxyphenyl)furan-2(5H)-ones were synthesized and fully characterized by elemental analysis, MS and ¹H NMR. All of them were evaluated for antimicrobial activities against three Gram-positive organisms and a Gram-negative organism, and compound 5 was the most active against Staphylococcus aureus ATCC 25923.     

Structural Modulation in Lanthanide Tetracyanoplatinates Incorporating Terpyridine: Synthesis and Structures of Four Distinct One-Dimensional Variants

Abstract  

The synthesis of four different lanthanide tetracyanoplatinates all incorporating 2,2′:6′,2″-terpyridine have been carried out in acetonitrile/water mixtures by reaction of an appropriate Ln³⁺ salt with 2,2′:6′,2″-terpyridine and potassium tetracyanoplatinate. The use of different Ln³⁺ salts as reactants results in the isolation of {La(tpy)(H₂O)₃}₂[Pt(CN)₄]₃·2CH₃CN·2H₂O (La-1) space group P[`1] P\bar{1} , a = 9.3862(15) ?, b = 12.186(1) ?, c = 13.493(1) ?, α = 88.082(7)°, β = 80.22(1)°, γ = 74.88(1)°, {Pr(tpy)(H<sub>2</sub>O)<sub>3</sub>}<sub>2</sub>[Pt(CN)<sub>4</sub>]<sub>3</sub>·2H<sub>2</sub>O (Pr-2) space group P[`1] P\bar{1} , a = 9.2458(15) ?, b = 10.8068(9) ?, c = 13.6178(14) ?, α = 84.554(8)°, β = 74.905(10)°, γ = 79.490(9)°, Ho(tpy)(H₂O)₂(NO₃)[Pt(CN)₄] · CH₃CN (Ho-3) space group P2₁/c, a = 12.867(1) ?, b = 15.1046(15) ?, c = 13.651(4) ?, β = 105.39(1)°, or Yb(tpy)(H₂O)₂(NO₃)[Pt(CN)₄]·0.5CH₃CN·1.5H₂O (Yb-4) space group Pbcn, a = 13.226(7) ?, b = 15.870(2) ?, c = 24.276(3) ? under quite similar reaction conditions. All four of these compounds have been isolated as single crystals and X-ray diffraction has been used to investigate their structural features. None of these compounds are isostructural with one another, but all contain one-dimensional, polymeric structures that contain tris chelation of the Ln³⁺ cations by terpyridine and bridging of the Ln³⁺ ions by tetracyanoplatinate. La-1 and Pr-2 contain both cis- and trans-bridging of Ln³⁺ cations by tetracyanoplatinate resulting in double chains with a ladder-type structure. Ho-3 and Yb-4 are similar in that they contain chelation of Ln³⁺ by both terpyridine and a nitrate anion and both structure types only contain cis-bridging by tetracyanoplatinate. All four structures contain Pt–Pt interactions in the form of dimeric units.     

Two Metal Complexes Supported by {VO<Subscript>3</Subscript>}<Subscript>n</Subscript><Superscript>n−</Superscript> Chains: Hydrothermal Syntheses and Crystal Structures of [M(dpa)V<Subscript>2</Subscript>O<Subscript>6</Subscript>] (M = Zn(II) and Cu(II); dpa = 2,2′-dipyridylamine)

Abstract  

Two new metal complexes supported by {VO₃}_n ⁿ⁻ chains, [M(dpa)V₂O₆] (1, M = Zn²⁺; 2·H₂O, M = Cu²⁺; dpa = 2,2′-dipyridylamine), have been synthesized hydrothermally and characterized by elemental analysis, TG analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal data: [Zn(dpa)V₂O₆] 1, Triclinic, P-1, a = 9.663(7) ?, b = 10.617(7) ?, c = 15.114(10) ?, α = 105.678(10)°, β = 104.772(9)°, γ = 94.021(10)°, Z = 2; [Cu(dpa)V₂O₆]·H₂O 2·H₂O, Monoclinic, C2, a = 20.543(3) ?, b = 7.2460(9) ?, c = 10.4853(13) ?, β = 111.318(2)°, Z = 4. Complex 1 is constructed from sinusoidal {VO₃}_n ⁿ⁻ chains with {Zn(dpa)}²⁺ fragments spanning the adjacent troughs and crests into an 1D ribbon-like structure. Complex 2 is built up by linking {VO₃}_n ⁿ⁻ chains via pairs of symmetrical {Cu(dpa)}²⁺ fragments into a 2D layered structure. The Zn(II) and Cu(II) ions exhibit tetrahedral and square pyramidal coordination environments, respectively. The formation of the two isomers is attributed to the flexibility of {VO₃}_n ⁿ⁻ chains and the different coordination configurations of the two metal ions. There exist significant π–π stacking and hydrogen bonding interactions in complexes 1 and 2.     

Absence of Platinophilic Interactions in a Series of Tetracyanoplatinates Incorporating Cyclic Amines

Abstract  

Three novel compounds have been synthesized and structurally characterized: [1,10-Hphen]₂Pt(CN)₄·2H₂O (1a) space group P2₁/n, a = 8.73070(17) ?, b = 15.4609(2) ?, c = 9.82661(19) ?, β = 103.252(2)°; [2,2′-Hbipy]₂Pt(CN)₄·2H₂O (1b) space group P2₁/n, a = 7.0859(14) ?, b = 12.940(2) ?, c = 13.7486(19) ?, β = 100.708(16)°; K₂[Pt(CN)₄]·2phen (phen = 1,10-phenanthroline) (2) space group P2₁/c, a = 8.1393(4) ?, b = 20.4050(9) ?, c = 8.4085(4) ?, β = 105.284°. All three structures contain isolated [Pt(CN)₄]²⁻ ions and they all illustrate the absence of Pt⋯Pt interactions due to the presence of bulky cyclic amines or ammoniums. The structures of 1a and 1b contain large organic cations, 2,2′-bipyridinium and 1,10-phenanthrolinium, respectively while compound 2 contains neutral 1,10-phenanthroline molecules co-crystallized between the potassium tetracyanoplatinate framework.     

Syntheses and Crystal Structures of Two CuII Coordination Isomers [Cu(pmt)2] · 4H2O (1) and {[Cu(pmt)2] · 2H2O} n (2)

Abstract  A pair of Cu^II coordination isomers [Cu(pmt)₂] · 4H₂O (1) and {[Cu(pmt)₂] · 2H₂O} _n (2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl₂ · 2H₂O and Hpmt but with different experimental methods in water–methanol mixed solution, and were characterized by X-ray diffraction, elemental analysis, IR spectrum. X-ray analysis indicates that complex (1) is a mononuclear complex in which two deprotonated pmt ligands coordinate in a facial tridentate arrangement about the Cu^II atom. While complex (2) is a coordination polymer, in which four N atoms of pmt ligands coordinate to one Cu^II atom but its sulfonate O atoms bond to adjacent Cu^II atom. Thus 12-membered rings (–Cu–N–C–C–S–O–)₂ are obtained between two neighbouring Cu^II atoms and they connect one another to form this new polymer. Crystal data: [Cu(pmt)₂] · 4H₂O (1), Mr = 566.10, monoclinic, P2 ₁/c, a = 9.1950(8) ?, b = 11.5093(10) ?, c = 11.2304(10) ?, β  = 105.5550(10)°, Z = 2, V = 1144.96(17) ?³, R ₁  = 0.0407, wR ₂  = 0.1242 [I > 2σ (I)]; {[Cu(pmt)₂] · 2H₂O} _n (2), Mr = 530.07, triclinic, P-1, a = 7.6165(19) ?, b = 8.806(2) ?, c = 9.592(4) ?, α = 104.933(4)°, β = 106.732(4)°, γ = 109.503(3)°, Z = 1, V = 534.2(3) ?³, R ₁ = 0.0470, wR ₂ = 0.1082 [I > 2σ(I)]. Index Abstract  A pair of Cu^II coordination isomers [Cu(pmt)₂] · 4H₂O (1) and {[Cu(pmt)₂] · 2H₂O} _n (2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl₂ · 2H₂O and Hpmt but with different experimental methods in water–methanol mixed solution.      

The Synthesis and Crystal Structure of (Hpy)<Subscript>3</Subscript>[PMo<Subscript>12</Subscript>O<Subscript>40</Subscript>]·2(py)

Abstract  

The novel supramolecular networks based on Keggin-type polyoxoanion, formulated (Hpy)₃[PMo₁₂O₄₀]·2(py) has been synthesized hydrothermally and determined by X-ray diffraction. The compound crystallize in Monoclinic, system with space groups and cell parameters, P2 ₁ /n, a = 10.9370(2) ?, b = 19.586(3) ?, c = 12.5500(2) ?, β = 98.618(2)°, V = 2657.8(6) ?³. Organic fragments and Keggin anions are connected via N–H···N, N–H···O contacts to form interesting 1D zigzag chain. The molecule is stabilized in solid state by electrostatic forces and intermolecular hydrogen-bonding interactions to give the confirmation of guest [PMo₁₂O₄₀]³⁻ inserting in organic host.     

Synthesis and Crystal Structure of Three New Metal-Organic Frameworks in the Ln(III)/2,6-Pyridinedicarboxylate System

Abstract  

In this paper, three new metal-organic frameworks, synthesized by hydrothermal technique, are described. The compounds crystallize in triclinic space group P − 1 with cell parameters, respectively equal to (1) [La(H₂O)₃(dipic)]₂(C₂O₄) · 2H₂O a = 7.9990(1) ?, b = 8.3380(4) ?, c = 9.6180(5) ?, α = 98.194(5)°, β = 100.438(3)°, γ = 102.437(3)°, (2) [Eu(H₂O)₂(C₂O₄)]₂(dipic) · 3H₂O a = 8.2170(6) ?, b = 10.5900(8) ?, c = 13.0670(3) ?, α = 93.951(3)°, β = 103.393(5)°, γ = 107.797(6)°, and (3) [Ce₃(dipic)₃(Hdipic)(SO₄)(H₂O)₃] · 4H₂O a = 11.655(1) ?, b = 12.886(1) ?, c = 16.139(2) ?, α = 106.369(8)°, β = 92.90(1)°, γ = 115.787(7)°. They differ by their dimensionality mono-dimensional for (1), tri-dimensional for (2) and bi-dimensional for (3).     

The Zolmitriptan-Pyridine (1:1) and Zolmitriptan-Propiophenone (3:2) Inclusion Complex

Abstract  

The crystal structures of zolmitriptan with pyridine (I) and propiophenone (II) solvates have been determined by single crystal X-ray diffraction studies. Compound (I) crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 8.5610(5) ?, b = 12.2709(7) ?, c = 19.6201(12) ?, V = 2061.1(2) ?³, and Z = 4, while compound (II) crystallizes in the monoclinic space group P2₁ with a = 15.085(1) ?, b = 19.656(12) ?, c = 21.0860(13) ?, β = 92.068(1)°, V = 6248(4) ?³ and Z = 4. The asymmetric unit of (I), C₁₆H₂₁N₃O₂·C₅H₅N, contains one zolmitriptan molecule and one pyridine solvate, while the asymmetric unit of (II), 3(C₁₆H₂₁N₃O₂)·2(C₉H₁₀O) comprises six zolmitriptan molecules and four propiophenone solvates. In both structures, the N–H···N hydrogen bonds, form an infinite helical chain and generate a C(11)-type motif in (I) and a D₂²(13)-type motif in (II). Both the complexes have layer structures, the layers being constructed from rings (cavity) of four zolmitriptan molecules, hydrogen bonded through N–H···N and N–H···O bonds, where the pyridine (I) and propiophenone (II) solvates are included in an R₄⁴(33) ring.     

Synthesis and Crystal Structures of the Five-Coordinate Diorganotin(IV) Complex [Ph<Subscript>2</Subscript>Sn(L)]·DMF and its 5-Hydroxypyrazoline Ligand (H<Subscript>2</Subscript>L)

Abstract  

A five-coordinate diorganotin(IV) complex [Ph₂Sn(L)]·DMF and its ligand, 5-hydroxy-3-methyl-5-phenyl-(N ⁴-phenylthiosemicarbazone)pyrazoline (H₂L), were synthesized and characterized by elemental analysis, IR, NMR (¹H, ¹³C) spectroscopies and X-ray crystallography techniques. Our studies revealed that H₂L has formed as 5-hydroxy-4,5-dihydropyrazoline derivative in orthorhombic, Pbca space group with a = 15.4330(3) ?, b = 11.5427(2) ?, c = 18.1440(3) ? whereas [Ph₂Sn(L)]·DMF crystallizes with two independent molecules (a and b) in the asymmetric unit in triclinic system, Pī space group with a = 9.2795(1) ?, b = 15.8315(2) ?, c = 19.9895(3) ?, α = 100.855(1)°, β = 92.985(1)°, γ = 102.243(1)°. In molecule a, the central Sn(IV) atom adopts a distorted tetragonal–pyramidal (TTP) geometry with N2 atom at apical position, while in molecule b the Sn(IV) occupies the centre of a trigonal-bipyramid (TBP) with N2 atom of the ONS-tridentate ligand and both Ph groups occupying equatorial positions. One molecule of DMF (crystallization solvent) helps in stabilizing the crystal structure.     

Synthesis and Structure of cis-Dioxo(3-Methoxysalicylaldehyde 4-Methylthiosemicarbazonato-N,O,S)(γ-Picoline-N)Molybdenum(VI)

Abstract  Red crystals of cis-dioxo(3-methoxysalicylaldehyde 4-methylthiosemicarbazonato-N,O,S)(γ-picoline-N)molybdenum(VI), [MoO₂L(γ-pic)], [L²⁻=CH₃OC₆H₄(O)CH=NN=C(S)NHCH₃, 3-methoxysalicylaldehyde 4-methylthiosemicarbazonato] were prepared by the reaction of [MoO₂L] _n with γ-picoline in dry methanol. The title compound crystallized in the monoclinic space group P2₁/n, a = 6.7984(7) ?, b = 15.9760(12) ?, c = 17.1466(14) ?, β = 93.613(8)°, V = 1858.6(3) ?³, Z = 4. The coordination geometry around the molybdenum center is distorted octahedral with the tridentate thiosemicarbazonato ligand (L²⁻) bonded meridionally to the [MoO₂]²⁺ core. The sixth coordination site is occupied by a weakly bound γ-picoline molecule. The adjacent molecules are joined by the N–H···O hydrogen bonds between their amino and methoxy groups thus forming infinite molecular chains. The three-dimensional solid-state structure is achieved by the additional C–H···O, C–H···π and van der Waals interactions. Graphical Abstract  In the title compound, [MoO₂L(γ-pic)], the tridentate thiosemicarbazonato ligand (L²⁻) is meridionally bound to the [MoO₂]²⁺ core, while a molecule of γ-picoline completes the distorted octahedral coordination around the metal atom.      

Hydrogen-Bonded Molecular Ladders and Interlaced Networks in Complexes Built of V-Shaped Molecules 4,4′-Isopropylidenediphenol or 4,4′-Oxydibenzoic Acid with 4,4′-Bipyridine

Abstract  

The title compounds, C₁₀H₈N₂·C₁₅H₁₆O₂ (1) and C₁₀H₈N₂·C₁₄H₁₀O₅ (2), were synthesized by 4,4′-bipyridyl and two similar V-shaped molecules. The two complexes both crystallized in the same space group P2₁/n with the crystal cell parameters: a = 16.0536(3) ?, b = 6.42730(1) ?, c = 21.2717(4) ?, β = 102.330°, V = 2144.21(7) ?³, Z = 4 in compound 1 and a = 7.45020(10) ?, b = 10.0784(2) ?, c = 26.9430(5) ?, β = 92.1140(10)°, V = 2021.67(6) ?³, Z = 4 in compound 2. Compound 1 forms regular molecular chains containing alternative 4,4′-bipyridyl and 4,4′-isopropylidenediphenol units; the molecular components are linked by two types of O–H···N hydrogen bonds. Additionally, every two neighboring chains are connected to be a ladder structure by means of weak C–H···O interactions. In compound 2, 4,4′-bipyridyl and 4,4′-oxydibenzoic acid first construct one-dimensional architecture by strong O–H···N hydrogen bonds, which are similar with the interactions in compound 1. Secondly, two types of weak C–H···O contacts formed between 4,4′-bipyridyl and the acid link one-dimensional chains to be interlaced three-dimensional hydrogen-bonded networks.     

Syntheses, Characterization and Crystal Structures of Two Isostructural Hydrazone Compounds N′-(3-Bromo-5-chloro-2-hydroxybenzylidene)-4-chlorobenzohydrazide Methanol Solvate and N′-(3,5-Dichloro-2-hydroxybenzylidene)-4-chlorobenzohydrazide Methanol Solvate

Abstract  

Reactions of 4-chlorobenzohydrazide with 3-bromo-5-chloro-2-hydroxybenzaldehyde and 3,5-dichloro-2-hydroxybenzaldehyde, respectively, afforded two isostructural hydrazone compounds, C₁₄H₉BrCl₂N₂O₂·CH₃OH (1) and C₁₄H₉Cl₃N₂O₂·CH₃OH (2). Both compounds were structurally characterized by X-ray determination. Compound 1 crystallizes in the triclinic space group P − 1 with unit cell dimensions a = 7.462(1) ?, b = 9.281(2) ?, c = 12.626(1) ?, α = 98.451(2)°, β = 98.630(2)°, γ = 100.025(2)°, V = 837.8(2) ?³, Z = 2, R ₁ = 0.0394 and wR ₂ = 0.0967. Compound 2 crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a = 7.485(1) ?, b = 13.389(2) ?, c = 16.693(2) ?, β = 99.754(2)°, V = 1648.7(4) ?³, Z = 4, R ₁ = 0.0375 and wR ₂ = 0.0900. X-ray structural determination revealed that each compound consists of a hydrazone molecule and a methanol molecule of crystallization. In the crystal structures of both compounds, the adjacent molecules are linked by methanol molecules through N–H···O and O–H···O hydrogen bonds, forming dimers.     

Structure of Diaqua 1,10-Phenanthroline Cobalt (II) 2,5-Pyridinedicarboxylate Monohydrate

Abstract  

The coordination complex namely diaqua 1,10-phenanthroline cobalt (II) 2,5-pyridine dicarboxylate monohydrate that is formulated as [Co(H₂O)₂(PHEN)(PDC)] H₂O, (PHEN is the abbreviation of 1,10-phenanthroline and PDC is the abbreviation of 2,5-pyridinedicarboxylate), has been hydrothermally synthesized and characterized via single crystal X-ray diffraction techniques. This compound is monoclinic, space group P21/c, with Z = 4 in a unit cell with dimensions a = 11.7840(5) ?, b = 7.5298(3) ?, c = 21.5238(9) ?, β = 93.124(3)°. The structure contains one crystallographic unique Co atom, two coordinate water molecules, one PHEN species, one PDC fragment and one lattice water molecule. Extensive water O–H···O hydrogen bonding interaction among the adjacent discrete molecules leads to a two dimensional framework. This structure represents the first of cobalt compound in the system of PDC and PHEN that has been reported.