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 Structure of a Pure Inorganic Network Based Tetra-Sodium Capped Sandwich-Type Polyanion

Abstract  

The synthesis and single-crystal structure of a Na-salt compound Na₁₀[Co₄(OH₂)₂(AsW₉O₃₄)₂]·32H₂O (1) was reported. Compound 1 crystallizes in triclinic system, space group P−1, with the lattice parameters: a = 11.6040(10) ?, b = 12.9361(13) ?, c = 17.396(2) ?, α = 97.4120(10)°, β = 106.8590(10)°, γ = 111.867(2)° and Z = 1. Compound 1 consists of a pure inorganic network based on tetra-sodium capped sandwich-type anionic clusters [Co₄(OH₂)₂(AsW₉O₃₄)₂]¹⁰⁻ bridged through Na–OH₂ subunits. The thermogravimetric and electrochemistry measurements had also been studied.     

Crystal Structure and Photoluminescent Properties of Two Cadmium(II) Complexes with Orotic Acid

Abstract  

Assembly of orotic acid (2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylic acid, H₃dtpc) and Cd(OAc)₂·2H₂O gave rise to two complexes [Cd₂(H₂dtpc)₂(H₂O)₆] (I) and [Cd(H₂dtpc)(bpy)(H₂O)]_n (II) (bpy = 2,2′-bipyridine). Complex (I) and (II) have been characterized by X-ray single crystal diffraction, IR, PXRD, TGA and fluorescence spectra. Structural analyses reveal that (I) is a binuclear structure, and complex (II) possesses a one-dimensional infinite zig-zag chain architecture and the chains are further assembled into 2D supramolecular network by strong hydrogen bonding interactions. Crystal data for (I): Monoclinic, space group P2(1)/n, a = 9.3221(19) ?, b = 6.6315(13) ?, c = 15.322(3) ?, β = 102.31(3)°, V = 925.4(3) ?³, Z = 4, R1 = 0.0269, and wR2 = 0.0604; for (II): Monoclinic, space group P2(1)/c, a = 9.9880(2) ?, b = 14.5085(2) ?, c = 11.6957(2) ?, β = 107.976(2)°, V = 1612.10(5) ?³, Z = 4, R1 = 0.0234 and wR2 = 0.0554.     

Synthesis,Crystal Structure and IR Spectra of Complexes of Mn(II) by Indole-2-Carboxylic or Isoquinoline-1-Carboxylic Acids and 1,10-Phenanthroline

Abstract  

Two ternary complexes of manganese(II) indole-2-carboxylate (2-IC⁻) or isoquinolinecarboxylate (IQC⁻) with 1,10-phenanthroline (phen) in methanol or in dimethylacetamide (DMA) were synthesized and studied by X-ray diffraction and IR spectra. [Mn(C₉H₆NO₂)₂(C₁₂H₈N₂)₂]·CH₄O (1) crystallizes in the triclinic space group P-1 with cell parameters of a = 10.548(2) ?, b = 14.168(3) ?, c = 14.580(3) ?, α = 62.35(2)°, β = 69.16(2)°, γ = 78.61(2)°, V = 1802.4(6) ?³ and Z = 2; [Mn(C₁₀H₆NO₂)₂(C₁₂H₈N₂)].C₄H₉NO (2) crystallizes in the monoclinic space group P2₁/a with cell parameters of a = 15.304(5) ?, b = 12.871(5) ?, c = 17.421(5) ?, β = 114.39(1), V = 3125(2) ?³ and Z = 4. In 1, Mn is six-coordinate by two bidentate phen ligands and two 2-IC⁻ ligands and exhibits a very distorted octahedral geometry. This complex is solvated by methanol involved in hydrogen bonding. In 2, Mn atom is surrounded by one bidentate phen ligand and two bidentate IQC⁻ ligands. The complex exhibits a distorted octahedral geometry around the Mn^II atom. The crystal structure is completed by a disordered DMA solvate molecule. The IR spectra of both compounds are slightly different in the range 4000–2400 cm⁻¹ which may be attributed to hydrogen bond lack in 2.     

Solvothermal Synthesis and Crystal Structure of a 18-Membered Macrocycle Schiff Base Dinuclear Copper(II) Complex: Cu2(NO3)4(APTY)4 (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one)

Abstract  A new 18-membered macrocycle Schiff base dinuclear copper(II) complex: Cu₂(NO₃)₄(APTY)₄ (1) (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one), has been successfully synthesized by solvothermal treatment of Cu(NO₃)₂ · 6H₂O with APTY. Compound 1 crystallizes in the triclinic space group P-1 with cell parameters: a = 10.556(2) ?, b = 12.075(2) ?, c = 15.230(3) ?, α = 74.75(3), β = 81.50(3), γ = 70.60(3)°, V = 1762.7(6) ?³, R1 = 0.0493, wR2 = 0.1400, Z = 1, D _calc = 1.455 g/cm³, F(000) = 798, S = 1.009. In the compound molecules, each of the six-coordinated Cu^II atoms are bridged by APTY ligands into 18-membered macrocycle, and each the Cu²⁺ atoms exhibits a significantly distorted octahedral geometry. The crystal packing is stabilized by C–H···O hydrogen-bonding interactions into a three-dimensional supramolecular framework. Index Abstract  A new 18-membered macrocycle Schiff base dinuclear copper(II) complex: Cu₂(NO₃)₄(APTY)₄ (1), has been successfully synthesized by solvothermal treatment (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one). The six-coordinated Cu²⁺ atom exhibit significantly distorted octahedral geometry. The crystal packing is stabilized by C–H···O hydrogen-bonding interactions into a three-dimensional supramolecular framework.     

Synthesis and Structural Characterization of [2-(2-1H-Imidazoly)-1H-imidazolium nitrate] and [2-(2-1H-Imidazoly)-2H-imidazolium phthalyl glycinate] Based on the 2,2′-bi-1H-Imidazole Molecule

Abstract  

Two new compounds (H₃biim)(NO₃)(1) and (H₄biim)(phthgly)₂ (2) (H₂biim=biimidazole; Hphthgly=N-phthaloylglycine) have been synthesized and characterized by luminescence and single crystal X-ray diffraction study. Compound 1 crystallizes in the monoclinic space group C2/c, where a = 14.8078(15), b = 5.9233(6), c = 20.028(2) ?, β = 92.7910(10)°, V = 1754.6(3) ?³ and Z = 8. Compound 2 crystallizes in the monoclinic space group P2(1)/n, where a = 15.3775(14), b = 5.3200(6), c = 6.4689(18)?, β = 115.418(2)° V = 1216.9(2)?³ and Z = 4. In 1, the N–H groups of H₃biim⁺ and the oxygen atoms of NO₃ ⁻ are linked by hydrogen bonds leading to H₃biim⁺(N,N)–R₂²(10) and N–H···O interactions forming infinite 1D helical chains along the b-axis. Compound 2 consists of a planar diprotonated biimidazole moiety and two phthgly anions which connect to the dication by hydrogen bonds phthgly⁻(O,O)–R₂²(9).     

Synthesis, Spectroscopic Studies and X-ray Crystal Structures of New Pyrazoline and Pyrazole Derivatives

Abstract  

The synthesis and characterization of some pyrazoline compounds of 1,3-diketones with hydrazine derivatives, namely, 1-(S-benzyldithiocarbazate)-3-methyl-5-phenyl-5-hydroxypyrazoline (1); 1-(2-thiophenecarboxylic)-3-methyl-5-phenyl-5-hydroxypyrazoline (2); 1-(2-thiophenecarboxylic)-3,5-dimethyl-5-hydroxypyrazoline (3); 1-(S-benzyldithiocarbazato)-3-methyl-5-phenylpyrazole (4); 1-(2-thiophenecarboxylic)-3-methyl-5-phenylpyrazole (5) and 1-(S-benzyldithiocarbazate)-3,5-dimethylpyrazole (6) are reported. Studies by IR, (¹H, ¹³C)-NMR spectroscopies and single crystal X-ray diffraction revealed that compounds (1)_, (2) and (3) are formed as pyrazoline, whereas (4) and (5) are formed as pyrazole derivatives only under acidic conditions. Compound (1) crystallizes in orthorhombic P2₁2₁2₁, a = 6.38960(10) ?, b = 12.9176(3) ?, c = 21.2552(5) ?, (2) crystallizes in monoclinic, P2₁/n, a = 11.3617(2) ?, b = 8.4988(2) ?, c = 92.8900(10) ? and β = 92.8900(5)°, (3) crystallizes in monoclinic, C2/c, a = 15.9500(5) ?, b = 9.3766(3) ?, c = 16.6910(5) ? and β = 113.825(2)°, (4) crystallizes in monoclinic, P2₁/c, a = 15.228(4) ?, b = 5.5714(13) ?, c = 19.956(5) ? and β = 91.575(7)° and (6) crystallizes in orthorhombic, P2₁2₁2₁, a = 5.3920(2) ?, b = 11.2074(5) ?, c = 21.885(1) ?. The (3) derivative represents the first pyrazoline compound prepared from 2,4-pentanedione and characterized crystallographically.     

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.     

Syntheses, Crystal Structures and Antibacterial Activities of Two Antipyrine Derivatives

Abstract  

Two new antipyrine derivatives, 4-{[1-(5-bromo-2-methoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₁₉H₁₈BrN₃O₂, 1) and 4-{[1-(2-hydroxy-3-ethoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₂₀H₂₁N₃O₃, 2), were synthesized and structurally characterized by elemental analysis, IR and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a = 6.987(1) ?, b = 27.930(2) ?, c = 9.483(1) ?, β = 109.36(2)°, V = 1745.9(4) ?³, Z = 4, R ₁ = 0.0430, and wR ₂ = 0.0870. Compound 2 crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 19.523(2) ?, b = 7.466(1) ?, c = 12.954(2) ?, β = 108.797(1)°, V = 1787.5(4) ?³, Z = 4, R ₁ = 0.0421, and wR ₂ = 0.1032. X-ray structure determinations revealed that the molecules of both compounds display trans configurations about the C=N double bonds. In the crystal structures, molecules are linked together by intermolecular C–H···O hydrogen bonds. Both compounds show strong antibacterial activities.     

Synthesis and Crystal Structure of a 3D Er(III) Coordination Polymer Based on Tripodal Flexible Ligand

Abstract  

Solvothermal reaction of Er(NO₃)₃·6H₂O and tri(2-carboxyethyl)isocyanurate (H₃tci) in DMF/H₂O (DMF = dimethylformamide) medium leads to the generation of one new 3D coordination polymer, [Er(tci)(H₂O)] DMF·2H₂O (1), which was characterized by the elemental analysis, IR spectroscopy and single crystal X-ray diffraction. X-ray diffraction analysis reveals that 1 crystallizes in triclinic space group P-1, features an interesting 3D coordination framework constructed from the flexible tridentate ligand H₃tci. Unit cell parameters for 1: a = 7.853(2) ?, b = 12.186(3) ?, c = 13.222(2) ?, α = 112.156(14)°, β = 105.457(15)°, γ = 91.541(18)° and Z = 2.     

Synthesis, Characterization and Crystal Structure of a New One-Dimensional Heterobimetallic Coordination Polymer Based on [(Tp)Fe(CN)3]?

Abstract  

By using a pre-designed anionic precursor [TpFe^III(CN)₃]⁻ (Tp = hydrotris(pyrazolyl)borate) as a structural building block, a new cyanide-bridged one-dimensional heterobimetallic coordination polymer, [(Tp)₂Fe₂^III(CN)₆Zn·2H₂O] _n (I) has been prepared and characterized by X-ray single crystal diffraction, M?ssbauer and magnetic experiments. Complex I crystallizes in the orthorhombic Ibam space group with a = 14.4094(8) ?, b = 18.3003(10) ?, c = 12.9855(7) ? and consists of rhombic chains, in which the [TpFe^III(CN)₃]⁻ unit acts as a bridging bidentate ligand toward two Zn²⁺ atoms through two of its three cyanide groups.     

Hydrothermal Synthesis, Structural Characterization and Luminescent Property of a New 1-D Chain-like [Er(NC6H4O2)3(H2O)2]n

Abstract  

Erbium (III) coordination compound with the formula [Er(IN)₃(H₂O)₂]_n 1 (HIN = isonicotinic acid) was synthesized by mixing Er₂O₃ with isonicotinic acid under hydrothermal condition. The structure of the title compound was determined by single crystal X-ray diffraction analysis, which reveals that the 1-D chain-like structure is formed by the erbium polyhedra through the carboxyl groups of IN. It crystallizes in the monoclinic system, possesses space group C2/c, with lattice parameters: a = 20.229(10) ?, b = 11.594(6) ?, c = 9.871(5) ?, α = γ=90°, β = 115.509(6)°, V = 2089.3(18) ?³, and D _calc = 1.811 mg/cm³ for Z = 4, F(000) = 1108, GOF = 1.109, R1 = 0.0675. Compound 1 has been characterized by IR absorption spectroscopy, ultraviolet excitation and emission spectrum.     

Stereochemical Assignment of Substituted 2-Aminobicyclo[3.1.0]hexane and 2-Aminobicyclo[5.1.0]octane Derivatives via Single Crystal X-ray Diffraction

Abstract  

Crystals of benzyl (RS,RS,RS)-7-phenylbicyclo[5.1.0]octan-2-ylcarbamate 9 and (RS,RS,RS)-N-[3′-(4″-methylpiperazin-1″-yl)propyl]-N-{5-(4′′′-cyanophenyl)bicyclo[3.1.0]hexan-2-yl}amine dihydrochloride 10·2HCl were synthesised and single crystal X-ray diffraction was used to establish unambiguously the relative configurations within these structures. Compound 9 crystallizes in the orthorhombic space group P2 ₁ 2 ₁ 2 ₁ with cell parameters of a = 6.85340(10) ?, b = 9.8732(2) ?, c = 27.5407(6) ?, V = 1863.54(6) ?³ and Z = 4. In the crystal structure adjacent molecules are linked by N–H···O=C hydrogen bonds. Compound 10·2HCl crystallizes as the corresponding monohydrate in the monoclinic space group P2 ₁/n with cell parameters of a = 7.1540(17) ?, b = 39.763(12) ?, c = 8.163(3) ?, β = 91.062(7)°, V = 2321.7(11) ?³ and Z = 4. In the crystal structure adjacent molecules are linked by a series of hydrogen bonds between the ammonium groups, chloride ions and adventitious water molecules.     

Synthesis and Crystal Structures of Two Binuclear Lanthanide [Ln = Pr,Dy] Complexes with 4-Quinolineacarboxylate

Abstract  

The reaction of the organic ligand, 4-quinolineacarboxylate (L) with Pr(ClO₄)₃·6H₂O and Dy(ClO₄)₃·6H₂O, leads to the formation of two novel complexes [Pr₂(L)₆(H₂O)₄]2H₂O 1 and [Dy₂(L)₆(H₂O)₄]2H₂O 2, which have been characterized by elemental analysis, IR and single-crystal X-ray diffraction analysis (monoclinic system, space group P2(1)/n, with a = 11.805(2), b = 16.645(3), c = 15.367(3) ?, β = 106.78(3)°, V = 2891.1(10) ?³, Z = 4 for 1, monoclinic system, space group P2(1)/n, with a = 11.629(2), b = 16.478(3), c = 5.336(3) ?, β = 105.83°, V = 2827.4(10) ?³, Z = 4). The two isostructure complexes are binuclear and possess an inversion center which is at the midpoint of the linkage of two symmetrical La(III) centers. In two complexes, each metal center adopts nine-coordinated mode coordinated by nine O atoms from two H₂O molecules and three carboxyls of three ligands, and L displays three different coordination modes. Hydrogen bonds join the binuclear complexes into 3D networks.     

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).     

Preparation, Crystal Structure and Spectroscopic Properties of Dimeric [Zn(2-bromobenzoato)2(phenazone)]2 and Monomeric [Zn(2-bromobenzoato)2(thiourea)2]·2H2O

Abstract  

The binuclear zinc complex bis(2-bromobenzoato-O)-bis(μ ₂ -2-bromobenzoato-O,O′)-bis(phenazone-O)-dizinc(II) (I) and the mononuclear dihydrate bis(2-bromobenzoato-O)-bis(thiourea-S)-zinc(II) (II) have been synthesized and characterized by means of elemental analysis and spectroscopic methods (IR, ¹H and ¹³C NMR, EDS). The solid state structures of both compounds were determined by single-crystal X-ray diffractometry. Compound [Zn(2-BrC₆H₄COO)₂(phen)]₂ (phen—phenazone) (I) crystallized as a dimeric compound with a triclinic lattice (space group P − 1), where both zinc atoms, interconnected by two carboxylate groups, possess a distorted tetrahedral coordination environment. The crystallographic data of complex I: a = 9.9410(3) ?, b = 10.7309(3) ?, c = 12.9237(4) ?, α = 93.6004(17)°, β = 92.5898(11)°, γ = 116.2192(16)°, V = 1230.26(6) ?³, Z = 1. Complex [Zn(2-BrC₆H₄COO)₂(tu)₂]·2H₂O (tu—thiourea) (II) crystallized with an orthorhombic lattice (space group Aba2) as a monomeric compound, where the coordination environment of the central zinc atom is a distorted tetrahedron. The crystallographic data of complex II are: a = 9.8595(3) ?, b = 19.7052(5) ?, c = 12.5908(3) ?, V = 2446.18(11) ?³, Z = 4. The modes of the carboxylate binding were assigned from the IR spectra using the magnitude of the separation between the carboxylate stretches (Δ), which correlated well with the crystal structures. The computed theoretical IR spectrum agreed well with the experimental data.     

Crystal and Molecular Structures of 2-Amino-4-Nitrobenzoic Acid and Its Cocrystals with 2,2′-Bipyridine (2/1) and Bis(pyridin-2-yl)ketone (1/1)

Abstract  

The eight-membered {···HOC=O}₂ synthon featured in the crystal structure of 2-amino-4-nitrobenzoic acid (1) is replaced by carboxylic acid···N-pyridine hydrogen bonds in its cocrystals with 2,2′-bipyridine (2/1; 2) and bis(pyridin-2-yl)ketone (1/1; 3) indicating the robust nature of the latter synthon. Disruption of the three-dimensional architecture based on O–H···O and N–H···O(nitro) hydrogen bonds in (1) is evident in the cocrystals which form supramolecular tubes (2) and chains (3) based on O–H···N and N–H···O hydrogen bonding. Compound (1) crystallizes in the monoclinic space group P2₁/n with a = 3.6291(1) ?, b = 7.7339(3) ?, c = 26.561(1) ?, β = 91.385(2)°, and Z = 4. Compound (2) crystallizes in the monoclinic space group C2/c with a = 27.562(3) ?, b = 6.8300(6) ?, c = 12.923(1) ?, β = 110.593(5)°, and Z = 4. Compound (3) crystallizes in the monoclinic space group P2₁/c with a = 3.795(3) ?, b = 12.024(8) ?, c = 35.65(2) ?, β = 92.131(6)°, and Z = 4 (determined from synchrotron data).     

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.     

The Structure and Fluorescence Property of a 3D Supramolecular Network [Cd2(2-mBIM)2Cl2(C4H4O4)(H2O)2(H2O)]n

Abstract  

A cadmium(II) coordination polymer [Cd₂(2-mBIM)₂Cl₂(C₄H₄O₄)(H₂O)₂(H₂O)] _n (1) (wherein 2-mBIM = bis(2-methylimidazo-1-yl) methane, C₄H₄O₄ = succinate anion) has been synthesized and characterized by X-ray diffraction. Complex 1 crystallizes in the monoclinic space group C2/c with a = 23.5265(15) ?, b = 7.3558(5) ?, c = 17.4771(11) ?, β = 90.3560(10)°, V = 3024.5(3) ?³, Z = 4. Each Cd(II) atom is octahedrally coordinated and connected with two adjacent Cd(II) atoms by two individual 2-mBIM ligands in a trans-configuration to form one-dimensional (1D) helical structure. Such 1D helical chain structures were connected to each other via the succinate anion ligands and result in the formation of a two-dimensional (2D) framework. Meanwhile, an overall three-dimensional (3D) supramolecular network was formed via the weak hydrogen bond interactions between metal-coordination and free water molecules.     

Reactivity of [Re2(CO)8(MeCN)2] With 1-vinylimidazole: X-ray Structures of [Re2(CO)8{η1-NC3H3N(CH=CH2)}2] and [ReCl2(CO)2{η1-NC3H3N(CH=CH2)}2]

Abstract  Treatment of [Re₂(CO)₈(MeCN)₂] with excess 1-vinylimidazole in refluxing benzene gives three new compounds [Re₂(CO)₉{η ¹-NC₃H₃N(CH=CH₂)}] (1), [Re₂(CO)₈{η ¹-NC₃H₃N(CH=CH₂)}₂] (2) and [ReCl₂(CO)₂{η ¹-NC₃H₃N(CH=CH₂)}₂] (3) in 11, 32 and 2% yields, respectively. The solid-state structures of complexes 2 and 3 have been determined by single crystal X-ray diffraction studies. Compound 2 crystallizes in the monoclinic space group C2/c, with lattice parameters a = 13.8378(5) ?, b = 11.8909(5) ?, c = 14.4591(6) ?, β = 116.6470(10)°, Z = 4 and V = 2131.99(15) ?³. Compound 3 crystallizes in the monoclinic space group C2/c, with lattice parameters a = 10.1028(3) ?, b = 13.5640(5) ?, c = 12.5398(4) ?, β = 109.637(2)°, Z = 4 and V = 1618.4(9) ?³. The disubstituted dinuclear compound 2 contains two 1-vinylimidazole ligands coordinated through the imino nitrogen atoms at the equatorial sites, whereas the mononuclear compound 3 contains two carbonyl ligands, two N coordinated η ¹-1-vinylimidazole ligands and two terminal Cl ligands. Graphical Abstract  Two dinuclear complesxes [Re₂(CO)₉{η ¹-NC₃H₃N(CH=CH₂)}] (1) and [Re₂(CO)₈{η ¹-NC₃H₃N(CH=CH₂)}₂] (2) and the mononuclear [ReCl₂(CO)₂{η ¹-NC₃H₃N(CH=CH₂)}₂] (3) were obtained from the reaction of [Re₂(CO)₈(MeCN)₂] with excess 1-vinylimidazole at 80 °C. The X-ray structrures of 2 and 3 are described.