Structural Correlations in High-Spin Complexes of [Fe{HC(3,5-Me2pz)3}2]2+: Solid State Structure of [Fe{HC(3,5-Me2pz)3}2][Fe2OCl6]

Abstract  The cation in the solid state structure of [Fe{HC(3,5-Me₂pz)₃}₂][Fe₂OCl₆] (pz = pyrazolyl ring) contains an octahedral iron(II) center with an average Fe–N bond distance of 2.17 Å, indicating that the iron(II) is in the high-spin form. While M–N bond distances of this length with κ³-[HC(3,5-Me₂pz)₃] ligands generally cause tilting of pz to open up the “bite” angle, in this structure the average tilting angle is only 3.1°, a much lower value than observed in earlier structures of this same cation paired with different anions. The crystals are monoclinic, space group P2₁/n, with a = 11.1671(12) Å, b = 10.8091(11) Å, c = 17.4385(17) Å, α = γ = 90°, β = 95.685(2)°, and Z = 2. Graphical Abstract  The cation in the solid state structure of [Fe{HC(3,5-Me₂pz)₃}₂][Fe₂OCl₆] (pz = pyrazolyl ring) contains an octahedral iron(II) center in the high-spin form with unusual orientations of the pyrazolyl rings.      

Synthesis,Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl<Subscript>2</Subscript> · 3.5H<Subscript>2</Subscript>O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane)

Abstract The reaction of the potentially tetradentate ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl₂(CH₃CN)₂] yields a mixture of complexes, where the ligand acts as bidentate SS, or tetradentate 2NS or NSSN. This mixture of complexes SS, 2NS, and NSSN was crystallized with dichloromethane/n-pentane (1:1) and crystals of [Pt(bddn)]Cl₂ (isomer NSSN) were obtained. The complex has been characterized by elemental analyses, mass spectrometry, conductivity, IR, ¹H, ¹³C{¹H}, ¹H{¹⁹⁵Pt}, ¹⁹⁵Pt{¹H}NMR, HSQC and NOESY spectroscopies, and X-ray diffraction. Compound [PtCl₂(bddn)] · 3.5H₂O crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 15.430(7) ?, b = 17.405(4) ?, c = 18.887(7) ?, β = 91.24(2)°, V = 5071(3) ?³, Z = 4, R ₁ = 0.0354, wR₂ = 0.1034. This compound consist of discrete cations [Pt(bddn)]²⁺, Cl⁻ anions and water molecules of crystallization. The platinum(II) is tetracoordinated by two azine nitrogen atoms and two sulfur atoms of the thioether-pyrazole ligand, in a distorted square planar geometry. Graphical Abstract Synthesis, Structural Characterization and Spectroscopic Properties of [Pt(bddn)]Cl ₂ · 3.5H ₂ O (bddn = 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane) Antonio de Leon, Josefina Pons*, Jordi García-Antón, Xavier Solans, Mercè Font-Bardia, Josep Ros* Reaction of the ligand 1,9-bis(3,5-dimethyl-1-pyrazolyl)-3,7-dithianonane (bddn) with [PtCl₂(CH₃CN)₂], yields a mixture of complexes. The mixture was crystallized with dichloromethane/pentane (1:1) and crystals of [Pt(bddn)]Cl₂ · 3.5 H₂O was obtained. Electronic supplementary material The online version of this article contains supplementary material, which is available to authorized users.     

Synthesis, Structure and Properties of (H2NCH2CH2NH3)3 {(VO)6 [B10O16 (OH)6]2} · 11H2O

Abstract A new polyoxovanadoborate cluster (H₂NCH₂CH₂NH₃)₃ {(VO)₆[B₁₀O₁₆(OH)₆]₂} · 11H₂O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA. The crystal of the new compound belongs to monoclinic system, space group C2/c with a = 20.198(1) ?, b = 13.4476(8) ?, c = 21.602(1) ?, β = 97.067(1)°, V = 5822.8(5) ?³, Z = 4, D _c = 1.956 g cm⁻³, M = 1714.4, μ = 1.066 mm⁻¹, S = 1.905, R = 0.059, R _w = 0.0966. Index Abstract A new polyoxovanadoborate cluster (H2NCH2CH2NH3)3{(VO)6 [B10O16(OH)6]2} · 11H2O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA.      

Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane

Abstract The title complex [Co₂(bte)₃(NCS)₄(H₂O)₂] _n (bte = 1,2-bis(triazol-1-yl)ethane) has been prepared. Single-crystal X-ray analysis reveals that the complex crystallizes in space group P ī with a = 7.7962(2), b = 8.3407(4), c = 14.7735(5) ?, α = 86.835(2), β = 76.2031(9), γ = 80.583(3)°. The crystal consists of two discrete complexes, [Co(bte)(NCS)₂(H₂O)₂] and [Co(bte)₂(NCS)₂]. The structure of [Co(bte)(NCS)₂(H₂O)₂] consists of neutral chain containing Co(II) bridged by bte molecules. The six-co-ordination of Co²⁺ is achieved by means of two trans NCS⁻ ions and water molecules. The structure of [Co(bte)₂(NCS)₂] demonstrates a one-dimensional neutral chain through bte-bridge, in which the Co(II) atom is in a distorted octahedral environment formed by four nitrogen atoms of the triazoles and two nitrogen atoms from two trans thiocyanato liagnds. Index abstract Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane This paper reports the synthesis and crystal structure of complex [Co₂(bte)₃(NCS)₄(H₂O)₂]_n (bte = 1,2-bis(triazol-1-yl)ethane), which consists two different neutral chains containing Co(II) bridged by bte molecules.      

A Unique Example of a Co-crystal of [Co(AMTTO)2(H2O)2](NO3)2 and [Co(AMTTO)2(CH3CN)2](NO3)2 (AMTTO = 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione)

A co-crystal of cobalt(II) complexes, Co(AMTTO)₂(CH₃CN)₂]²⁺(NO₃)₂. [Co(AMTTO)₂(H₂O)₂]²⁺(NO₃)₂, compound (1) was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P2₁/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R₁?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)₂(CH₃CN)₂]²⁺ and [Co(AMTTO)₂(H₂O)₂]²⁺ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

     

Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt<Subscript>2</Subscript>(μ<Subscript>2</Subscript>-S)<Subscript>2</Subscript>] Core Structures

Abstract Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were synthesized from mononuclear starting materials, and characterized. Complex [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] has phospine ligands arranged trans and presents a planar [Pt₂(μ₂-S)₂] core structure, imposed by symmetry. In contrast, the almost isoformular complex [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)] revealed to be a butterfly molecule with phosphine ligands in a cis configuration. In both complexes, two pentafluorobenzenethiolate ligands bridge metal centers in an anti conformation. Both compounds have been X-ray characterized. Trans complex: a = 11.8576(13) ?, b = 12.3237(14) ?, c = 13.4644(16) ?, α = 90.528(9)°, β = 113.866(9)°, γ = 107.698(9)°, ; cis complex: a = 24.368(2) ?, b = 15.043(2) ?, c = 37.596(7) ?, β = 93.69(1)°, C2/c. Index Abstract Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt ₂ (μ ₂ -S ) ₂ ] Core Structures Sylvain Bernès, Luis Villanueva & Hugo Torrens Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were X-ray characterized, [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] and [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)]. The [Pt₂(μ₂-S)₂] core is constrained by symmetry to be planar in the former complex, affording a trans arrangement for non-bridging ligands, whereas the latter is a butterfly molecule with a cis configuration. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

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.      

Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions

Abstract The synthesis and crystal structure of a new Ni(II) complex of stoichiometry [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O, where phen is phenanthroline and H₂Or is oratate monoanion, are reported. The complex [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O crystallizes in the monoclinic system with space group C2/c and cell parameters a = 16.1661(8) ?, b = 12.5669(7) ? and c = 16.4752(7) ?. The coordination around Ni(II) is a distorted octahedron with two phen ligands perpendicular to each other and two aqua ligands in cis- position. Orotate ions locate themselves out of the coordination sphere and bridge the [Ni(phen)₂(H₂O)₂]²⁺ moieties through hydogen bonding with aqua ligands. The FT-IR spectrum of the complex and thermal decomposition behaviour are also briefly discussed. Graphical Abstract Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions Dursun Ali K?se, Birgül Zümreoglu-Karan, Başak Koşar, Orhan Büyükgüng?r A new complex where Vitamin B13 monoanions act as counter ions and bridge the [Ni(phen)₂(H₂O)₂]²⁺ units by hydrogen bonds is described CCDC deposition number is 606339.     

Synthesis and Structure of [Fe<Subscript>3</Subscript>O(O<Subscript>2</Subscript>CCH<Subscript>2</Subscript>OMe)<Subscript>6</Subscript>(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][FeCl<Subscript>4</Subscript>]

Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined. The three iron atoms and the μ₃-oxo are coplanar. Each carboxylic ligand is bidentate and links two iron atoms in the cluster. The clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration. The [FeCl₄]⁻ anion is intercalated between the hydrogen-bonded sheets. Crystal data: space group P2₁/n, a = 10.276(2), b = 22.793(5), c = 17.091(3) ?, β = 96.66(3)°, V = 3976(1) ?³, Z = 4, R = 0.0837, wR ₂ = 0.1836. Graphical Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined in which the clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration.      

Synthesis,Properties, and Crystal Structures of Copper(II) Di-(2-picolyl)amine Complexes Containing Inorganic Salts

Abstract These complexes have been characterized by X-ray crystallography, spectroscopic, and cyclic voltammetry. In 1, the copper(II) ion has a distorted square-pyramidal geometry with three nitrogen atoms of the dpa ligand and two oxygen atoms of the nitrate anions. The crystal structure of 2 shows that the copper(II) ions are bridged by tp anion to form a dinuclear complex, in which each copper(II) ion exhibits a distorted square-pyramid with three nitrogen atoms of the dpa ligand, water molecule, and the oxygen atom of the bridging tp ligand. Cyclic voltammetric data indicate that 1 undergoes irreversible one-electron oxidation to the Cu^III and reversible one-electron reduction to the Cu^I, while 2 gives one reversible oxidation and two reversible and irreversible reduced processes. The electronic spectra and redox potentials of the complexes are influenced significantly by the anionic ligands. Graphical Abstract The reaction of [Cu(dpa)Cl₂] with K(NO₃)₂ and Na₂tp yields mononuclear and dinuclear copper(II) complexes [Cu(dpa)(NO₃)₂] (1) and [Cu₂(dpa)₂(H₂O)₂(μ-tp)](tp)·6H₂O (2) (dpa = di-(2-picolyl)amine, tp = terephthalate).      

Crystal Structure of Tetrakis Imidazole Copper(II) Diadipate Complex

Abstract  The title compound, [Cu(C₃H₄N₂)₄(COO–(CH₂)₄–COOH)₂] is a neutral complex and exist as a monomeric unit. The Cu atom occupies at the center of symmetry (0, 0.5, 0) with a distorted octahedral geometry. Imidazole nitrogens N1 and N6 (Cu1–N1 = 1.993(3) ?; Cu1–N6 = 2.008(3) ?) from two different imidazole group which are symmetrically disposed provides the square base and the long carboxylate oxygens (Cu1–O2 = 2.582(3) ?) from the protonated end of symmetrically oriented dibasic acid at the trans axial position. The adipate monoanion is in weak coordination with the metal center via monodentate fashion. The strong carboxylate-carboxylic acid intermolecular O–H…O interaction between the adjacent molecules is present in this structure as observed in the crystal structure of hexanedioic acid is noteworthy. In addition to the O–H…O H-bonding other molecular interactions such as N–H…O and C–H…O in packing generates a 3-D hydrogen bond network. Graphical Abstract  The title compound tetrakis imidazole Cu(II) diadipate is a neutral complex and exist as a monomeric unit with the metal atom occupies at the center of symmetry. Strong inter and intramolecular H-bonding interactions such as O–H…O, N–H…O and C–H…O in packing generates a 3-D hydrogen bond network.     

Synthesis and Crystal Structure of Pivalamidate-Bridged Trinuclear Platinum–Copper Complex with a Linear Pt–Cu–Pt Core

Abstract The heterotrimetallic complex [Cu{trans-Pt(NH₃)₂(NHCO^tBu)₂}₂](NO₃)₂ was synthesized and structurally characterized by X-ray crystallography. The cationic complex consists two trans-[Pt(NH₃)₂(NHCO^tBu)₂] units and one Cu²⁺ ion, which are linearly held together by four bridging pivalamidate ligands. The compound crystallizes in the monoclinic space group P2₁/c with a = 13.18(1) ?, b = 13.12(1) ?, c = 21.38(2) ?, β = 116.88(3)°?, V = 3674(5) ?³, and Z = 4. The trimeric Pt–Cu–Pt cation further aggregates into a dimer of trimer via a weak Pt···Pt interaction. Graphical abstract Synthesis and crystal structure of pivalamidate-bridged trinuclear platinum–copper complex with a linear Pt–Cu–Pt core Chao Chen, Huayu Qiu*, Fenghui Liu and Wanzhi Chen* A heterotrimetallic complex [Cu{trans-Pt(NH3)₂(NHCO^tBu)₂}₂](NO₃)₂ was synthesized and structurally characterized by X-ray crystallography.      

A Tetranuclear Propane-1,3-Dithiolate Complex, [Fe2(CO)5{Ph2P(CH2)3}{(µ-SCH2)2CH2}]2, with a Bridging 1,6-Bis(diphenylphosphino)hexane Ligand

The 2:1 molar reaction of [Fe₂(CO)₆{(µ-SCH₂)₂CH₂}] (1) and a bidentate diphosphine ligand, 1,6-bis(diphenylphosphino)hexane (dpph), in the presence of Me₃NO resulted in the isolation of [Fe₂(CO)₅{Ph₂P(CH₂)₃}{(µ-SCH₂)₂CH₂}]₂ (2) as red crystals in 71?% yield. The dpph ligand in compound 2, coordinates two Fe₂S₂ subunits as bridging mode and hence makes a linkage between two [Fe₂(CO)₅{(µ-SCH₂)₂CH₂}] fragments. Each Fe₂S₂ butterfly of the complex consists of two fused Fe(S-C-C-C-S) six-membered rings, one of which attains a chair conformation, and the other is necessarily in a boat conformation. Compound 2 has unequivocally been characterized by elemental analysis, IR, ¹H NMR and ³¹P NMR spectroscopy together with single crystal X-ray diffraction studies. Crystals of 2 are triclinic, space group P-1, a = 9.918(4) Å, b = 10.347(3) Å, c = 14.581(5) Å, α?=?72.239(12)º, β?=?80.342(12)º, γ?=?68.550(14)º and Z = 1.

Graphic Abstract

A novel tetranuclear propane-1,3-dithiolate complex, [Fe₂(CO)₅{Ph₂P(CH₂)₃}{(μ-SCH₂)₂CH₂}]₂ (2), bearing a bridging bis(diphenylphosphino)hexane (dpph) ligand, was synthesized from the Me₃NO aided room temperature displacement of carbonyls from [Fe₂(CO)₆{(μ-SCH₂)₂CH₂}] (1), and structurally characterized.

     

Synthesis and Crystal Structure of a Mixed-Ligand Cobalt(II) Complex with 2-Aminobenzimidazole

Abstract  The cobalt(II) complex, [Co(abz)₂(SCN)₂] 1, has been synthesized by the reaction of cobalt(II) nitrate with ammonium thiocyanate and abz ligands (abz = 2-aminobenzimidazole), and was fully structurally characterized by elemental analysis, IR spectra, X-ray diffraction and thermogravimetric experiments. It crystallizes in the triclinic P-1 space group with a = 8.6316(10), b = 9.3426(10), c = 13.254(2) ?, α = 95.793(2), β = 95.870(2), γ = 115.7380(10), V = 945.1(2) ?³, and Z = 2. The central cobalt(II) atom is four-coordinated to nitrogen donors from two neutral abz ligands and two isothiocyanate anions respectively, adopting a slightly distorted tetrahedral geometry. In addition, the intermolecular N–H···N and N–H···S hydrogen bonds interactions link the discrete mononuclear units into infinite three-dimensional networks. Index Abstract  The essence sentence of the paper: In the mixed-ligand mononuclear complex, [Co(abz)₂(SCN)₂], the four coordinated cobalt(II) atom exhibits a slightly distort tetrahedron, which is further assembled into 3D infinite network by intermolecular hydrogen interactions.      

Synthesis and Crystal Structure of 4,6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde

Abstract The title compound, 3, 6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]- benzene-1,3-dicarbaldehyde was synthesized by Vilslmeier reaction from resveratrol (trans-3,4′,5-trihydroxystilbene). Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with crystallographic parameters: a = 7.2950(15) ?, b = 14.781(3) ?, c = 12.202(2) ?, β = 96.57(3)°, μ = 0.108 mm⁻¹, V = 1307.1(5) ?, Z = 4, Dx = 1.445 g/cm³, F(000) = 592, T = 293(2) K, 2.17°≤ θ ≤ 26.00°. The X-ray results demonstrated that the Vilslmeier reaction of resveratrol with DMF, POCl₃ and CH₃CN yielded 4,6-dhydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde. Graphical Abstract In this article, a resveratrol derivative was prepared and structurally characterized by single crystal X-ray diffraction.      

Syntheses, Spectroscopic Data, and X-ray Diffraction Structures of the Heterometallic RuRe Face-shared Bioctahedral (η6-cymene)Ru(μ-Cl)3Re(CO)3 and MnRu2 Edge-shared Trioctahedral [fac-ClRu(CO)3]2(μ-Cl)4Mn(H2O)2 Complexes

Abstract  Thermolysis of the diruthenium compound [(η⁶-cymene)RuCl₂]₂ (1) with ClRe(CO)₅ (2) leads to the formation of the new confacial bioctahedral compound (η⁶-cymene)Ru(μ-Cl)₃Re(CO)₃ (3) in good yields; the same product has also been isolated when a mixture of 1 and 2 is irradiated with near UV–vis light for an extended period of time. Heating 1 and ClMn(CO)₅ (4) does not furnish the corresponding manganese analogue of 3 but rather the trioctahedral halide-bridged product [fac-ClRu(CO)₃]₂(μ-Cl)₄Mn(H₂O)₂ (5). 3 and 5 have been fully characterized in solution and their molecular structures established by X-ray crystallography. Graphical Abstract  Thermolysis of [(η⁶-cymene)RuCl₂]₂ (1) with the respective pentacarbonyl ClM(CO)₅ [where M = Re (2); Mn(4)] affords the halide-bridged compounds (η⁶-cymene)Ru(μ-Cl)₃Re(CO)₃ (3) and [fac-ClRu(CO)₃]₂(μ-Cl)₄Mn(H₂O)₂ (5). 3 and 5 have been isolated and characterized spectroscopically in solution and their molecular structures established by X-ray crystallography.      

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.     

The Synthesis and Crystal Structure of [BiI2(tpy)2][Bi2I7(tpy)]: A New Metal Halide Material

Abstract [BiI₂(tpy)₂][Bi₂I₇(tpy)] (1) (tpy = 2,2′:6′2′′-terpyridine), a new compound containing a discrete bismuth halide anion, has been synthesized solvothermally and characterized by single crystal X-ray diffraction. The solvothermal reaction between BiI₃, Zn(NO₃)₂ · 6H₂O, and 2,2′:6′2′′-terpyridine in an ethanol/water solvent mixture resulted in the title compound. The anion and cation of this compound both contain bismuth, iodide ligands, and the organic ligand. The anion is composed of two face-sharing bismuth polyhedra, one of which is coordinated in a tridentate fashion to a disordered tpy ligand; and the remaining coordination sites at each Bi center are occupied by iodide ligands. The cation of the compound is a distorted, eight-coordinate polyhedron with a bismuth center, two iodide ligands, and six nitrogen atoms from two, tridentate tpy ligands. [BiI₂(tpy)₂][Bi₂I₇(tpy)] crystallizes in the triclinic space group P with the following lattice parameters: a = 10.0744(5) ?, b = 16.6115(8) ?, c = 18.5333(9) ?, α = 102.6490(10)°, β = 101.0850(10)°, and γ = 93.9160(10)°. Index Abstract The title compound, [BiI₂(tpy)₂][Bi₂I₇(tpy)], was synthesized solvothermally by the reaction between BiI₃ and 2,2′:6′2′′-terpyridine. Single crystal X-ray diffraction analysis reveals that the molecular structure contains one anion and one cation, both of which contain bismuth, iodine, and the tpy ligand, a situation not typically observed in these types of compounds.      

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.      

Synthesis and Crystal Structure of a New Binuclear Samarium Complex with Salicylate

Index Abstract  In the dinuclear compound (HPhen)₂[Sm₂(Hsal)₈(H₂O)₂] · 2H₂O (Hsal = o-HOC₆H₄CO₂ ⁻, Phen = 1,10-phenanthroline), intermolecular hydrogen bonds and π–π stacking interactions between parallel aromatic rings result in the formation of a two-dimensional supramolecular network.