Crystal structure of L-leucinium tetrafluoroantimonate(III)

The crystal structure of L-leucinium tetrafluoroantimonate(III) of the composition (C₆H₁₄NO₂)SbF₄ (orthorhombic symmetry: a = 6.1459(6) Å, b = 14.994(1) Å, c = 24.789(2) Å, Z = 8, P 2₁2₁2₁ space group) synthesized for the first time is determined. The (C₆H₁₄NO₂)SbF₄ structure represents a new structure type of tetrafluoroantimonate(III). It is formed by (C₆H₁₄NO₂)+ cations and chain complex [Sb₂F₈]_n ²ⁿ anions composed of Sb₂F₈ dimers linked into chains by bridging F atoms. The Sb₂F₈ dimers consist of SbF₃ and SbF₅ groups bound by bridging fluoride atoms of the SbF₅ group. Chains in the structure are linked by N-H…F, N-H…O, and O-H…F hydrogen bonds into a three-dimensional framework.     

Ribbon structure of the coordination polymer of silver trifluoroacetate with 2-pyrimidinecarboxamide

Complex [Ag(CF₃CO₂)(C₅H₅N₃O)] (I) was synthesized, and its structure was determined. Crystals of complex I are triclinic, space group P \(\bar 1\),,a = 7.325(1) Å, b = 7.554(1) Å, c = 10.527(1) Å, α = 94.25(1)°, β = 96.19(1)°, γ = 117.75(1)°, V = 507.4(1) ų, ρ_calcd = 2.252 g/cm³, Z = 2. Structure I contains dimeric silver carboxylates Ag₂(C₅H₅N₃O) ₂ ²⁺ , formed by 2-pyrimidinecarboxamide. Adjacent dimers Ag₂(C₅H₅N₃O) ₂ ²⁺ are linked by carboxylate dimers to form infinite ribbons along the x axis. The ribbons are arranged in the structure so that cavities are formed between them in the [001] direction. Trifluoroacetate CF₃ groups and carboxamide NH₂ groups are directed into the inside of these cavities.     

Synthesis and molecular structure of salicylaldehydeS-methyl-isothiosemicarbazone,C9H11N3OS

The crystal structure of salicylaldehyde S-methylisothiosemicarbazone together with the synthesis applied are reported: C₉H₁₁N₃OS, monoclinic, P2₁/n,a=5.169(4),b=16.853 (10),c=11.367(5)Å, β=92.48(1)°,V=989.3(18)ų,Z=4,d _x =1.405g cm^?3. The structure was solved by the heavy atom method and refined anisotropically to a residualR=0.046. The molecule is practically co-planar. There is only one basic difference between the title compound H₂ L and its deprotonated and complexed forms reported hitherto: the nearly 180° difference in rotation about the formal double bond C1—N2. The molecules form hydrogen bonded dimers around \(\bar 1\) .     

Synthesis and structure of a binuclear ruthenium 4-chlorobenzamidato complex

The compound Ru₂Cl(4-Cl-C₆H₄CONH)₄ was prepared by reaction of Ru₂Cl(O₂CCH₃)₄ with 4-Cl-C₆H₄CONH₂ at 180°C. Crystals of the composition Ru₂Cl(4-Cl-C₆H₄CONH)₄CH₃OH were obtained by slow diffusion of CH₃OH containing Et₄NCl into a Me₂SO solution of the compound. The structure of the crystalline product, which loses solvent of crystallization on removal from the mother liquor, was solved by X-ray crystallography by mounting a single crystal in a capillary containing the mother liquor. The crystals belong to the space group P1? (triclinic crystal system) with a = 12.731(3) Å, b = 14.389(3) Å, c = 12.604(3) Å, α = 103.41(2)°, β = 106.43(2)°, γ = 64.90(2)°, V = 1988.6(8) ų and Z = 2. There are two half ruthenium dimers linked by a Cl atom and an uncoordinated solvent CH₃OH molecule per asymmetric unit. The ruthenium dimers lie on two centers of inversion at 0, 0, 0 and 1/2, 0, 0. The chloride ions bridge dinuclear cations in the crystal, forming infinite zigzag chains. The average Ru-Ru distance is 2.296[1] Å and each ruthenium atom has a RuClN₂O₂ coordination sphere where the average Ru′-Ru-Cl angle is virtually linear (175.68[6]°). The metal oxidation states in the complex are + 2 and + 3, giving an average value of + 2.5. The arrangement of four bridging 4-Cl-benzamidato ligands is of the 2 : 2 type. The average Ru-N, Ru-O, Ru-Cl distances and Ru(1)-Cl(1)-Ru(2) angle are 2.036[6] Å, 2.044[5] Å, 2.583[2] Å and 117.26(8)°, respectively. The IR spectrum of the compound shows two N-H stretches at 3380 and 3340 cm^?1. The electronic spectrum of the compound in Me₂SO exhibits bands at 558 nm (ε = 340 M^?1 cm^?1), 425 nm (1000) and 320 nm (22,700).     

Synthesis, structure and properties of a two-dimensional iron(II) metal-organic framework

Reaction of FeSO₄·7H₂O with 5-(isonicotinamido)isophthalic acid (H₂INAIP) in the presence of NaOH results in the formation of a two-dimensional network [Fe(INAIP)(H₂O)]_n·2nH₂O. In the complex, each INAIP^2? ligand links three Fe(II) atoms to give a double-chain structure using its two carboxylate groups in ?? ₁?C?? ¹:?? ¹ and ?? ₂?C?? ¹:?? ¹ coordination modes. The chains are interlinked to form a layer structure through Fe?CN interactions, which it is extended to a three-dimensional supramolecular structure by H-bonding interactions. The thermal and magnetic properties of the complex were investigated, and antiferromagnetic interactions were observed. Moreover, the adsorption behavior shows that the title complex has obviously selective adsorption of CO₂ over N₂ after the removal of the solvent molecules within the pores.     

Crystal structure and magnetic properties of the binuclear copper(II) complex with 2,6-diformyl-4-tert-butylphenol bis(imidazolinylhydrazone)

The binuclear copper(II) complex with 2,6-diformyl-4-tert-butylphenol bis(imidazolinylhydrazone) (H₃L), [Cu₂(H₂L)Br₂]ClO₄ (I), was synthesized. The structure of complex I was determined by X-ray diffraction analysis. The antiferromagnetic exchange interaction (2J = ?108 cm^?1) translated through the phenoxide oxygen atom is observed between the copper(II) ions. The exchange parameter was calculated by the quantum-chemical “broken symmetry” method.     

Crystal and molecular structure of the monoclinic modification of Mn(S2CO-i-C3H7)2(2,2’-bipy)

The crystal and molecular structure of modification II of the Mn(S₂CO-i-C₃H₇)₂(2,2’-Bipy) complex was determined from X-ray diffraction data (“Syntex P2₁” diffractometer, CuK_α radiation, 1603 F(hkl), R = 0.0446). The crystals are monoclinic,a = 23350(3),b = 9.325(1),c = 22.030(2) å, Β = 106.98(1)?,V = 4587.7 å³, Z =8, d _calc = 1.394 g/cm³, space group C2/c. The structure consists of monomeric molecules in which the manganese atom has a distorted octahedral environment (4S + 2N). The orthorhombic and monoclinic modifications of the complex are compared with respect to the molecular geometry and packing.     

The crystal structure of tetrabutylammonium trichlorocarbonylplatinate(II)

Crystals of [C₁₆H₃₆N]⁺[Cl₃COPt]^? are monoclinic, space group P2₁/n, with a 14.949(8), b 8.892(7), c 18.232(10) Å, β 105.5(3)°, Z 4. The structure has been refined by least-squares to a final R of 0.042 for 2358 counter intensities. The PtCl bond lengths in the square-planar anion are not significantly different (mean value 2.291 Å) and the PtC (carbonyl) bond length is 1.82 Å.Conclusions are drawn on the factors affecting the trans influence in this complex and a number of related square planar Pt^II chloro-complexes.     

The structure of the dithionite ion

The Raman spectra of aqueous and solid sodium dithionite have been recorded. Differences in the location, intensity, and number of observed bands are attributed to conformational changes in the dithionite ion. The structure of the aqueous ion is non-planar with a C_2h symmetry with an SS bond distance estimated to be 0.220–0.226 nm, as opposed to the dithionite structure in the Na₂S₂O₄·2H₂O salt which is known to have C_2ν structure with a bond distance of 0.2389 nm. The Raman spectra of aqueous dithionite are assigned to A_g (SO) = 997 cm^?1; B_g (SO) at 912 cm^?1, B_g SO₂ twist at 324 cm^?1. The remaining bands are a strong A_g, the SO₂ wag, the SO₂ scissor, and the SS stretch at 584, 461, and 232 cm^?1, respectively, but due to coupling all three motions are expected to exhibit substantial SS character. The variation of the spectra of the solid and aqueous sodium dithionite indicate strong environmental effect on the structure of the anion.     

Synthesis and crystal structure of the complex N,N-dimethylanilinium dicitratoborate monohydrate

N,N-Dimethylanilinium dicitratoborate monohydrate [C₆H₅NH(CH₃)₂][(C₆H₆O₇)₂B]·H₂O (I) was synthesized for the first time. Single crystals were obtained in an aqueous solution; the crystal structure was studied by X-ray crystallography. Crystals of I are triclinic, space group $P\bar 1$ , a = 9.7017(2) ?, b = 11.0475(2) ?, c = 12.6282(2) ?, ?? = 106.595(2)°, ?? = 106.931(1)°, ?? = 103.568(1)°, V = 1163.97(4) ?³, Z = 2, ??_calc = 1.516 g/cm³. The structural units of compound 1 are large complex dicitratoborate anions with a spiran structure, N,N-dimethylanilinium cations, and crystal water molecules. The crystal packing is a three-dimensional framework. A hydrogen-bond system is formed by seven independent contacts O(N)-H??O.     

Crystal and molecular structure and vibrational spectra of 2,6-bis(diphenylphosphorylmethyl)-4-methylphenol and its complex with cerium(III) nitrate

The structure of 2,6-bis(diphenylphosphorylmethyl)-4-methylphenol 2,6-[Ph₂P(O)CH₂]₂-4-MeC₆H₂OH(L¹) and its 1: 1 complex with cerium(III) nitrate were studied by X-ray diffraction. A rather strong intramolecular hydrogen bond P=O…H-O (O…O, 2.646(1) Å) exists in the L¹ molecules. In the crystal, the molecules are combined into centrosymmetric dimers through the stacking interaction between the central phenol rings; the distance between the ring planes is 3.39 Å. In the complex molecule, [Ce(L¹)(NO₃)₃ · Me₂C(O)], the neutral ligand L¹ is tridentate and the three nitrate ions are bidentate, and the tenth coordination site is occupied by acetone oxygen. No intramolecular H-bonds are present. In the crystal, the complex molecules are combined into centrosymmetric dimers through intermolecular hydrogen bonds O-H…O-NO₂ (O…O, 2.713(8) Å). The vibrational (IR, Raman) spectra of the ligand and the complex were studied and the principal bands were assigned. According to IR spectroscopy, the P=O…H-O intramolecular hydrogen bond is retained in both the ligand and the complex molecules.     

The crystal and molecular structure of η5-cyclopentadienyliodomethyl(methylthio)carbene-(triphenylphosphine)iridium(III) iodide

The crystal and molecular structure of η⁵-cyclopentadienyliodomethyl(methylthio)carbene(triphenylphosphine)iridium(III) iodide [IrI{C(Me)SMe}(η⁵-C₅H₅)(PPh₃)]I has been determined from three dimensional X-ray data in order to clarify the contribution of the α-sulphur atom to the bonding in this carbenoid complex.The compound crystallizes in space group Pbc2₁ with four formula units in a cell of dimensions a 9.745(6), b 15.201(8), and c 17.364(10) Å. Least-squares refinement of the structure has led to the final discrepancy index R = 0.047 for the 1655 symmetry-independent observable reflections. The coordination geometry about the iridium atom is approximately tetrahedral; the coordination positions are occupied by the η⁵-C₅H₅ ring center, the phosphorus, the iodide I(1) and the carbon C(6) of the C(Me)SMe ligand (IrRc 1.89, IrP 2.280(7), Ir(1) 2.651(2) and IrC(6) 2.03(3) Å).The bonding of the C(Me)SMe group indicates that this complex must be formulated as a C(Me)SMe complex of iridium(III).     

Crystal structure of a new molecular complex of fullerene with tetramethyltetraselenafulvalene: C60·TMTSF·2CS2

A new molecular complex of fullerene with tetramethyltetraselenafulvalene (TMTSF), C₆₀·TMTSF·2CS₂, (1) was synthesized. The structure and composition of the complex were established by X-ray diffraction analysis. The crystals of C₆₀·C₁₀H₁₂Se₄·2CS₂ are monoclinic:a=15.407(2),b=12.934(2),c=12.026(2) Å β=108.39(3)°,V=2274.1(6) ų, space groupCm, Z=2,d _calc=1.929 g cm^?3,R=0.047. The crystal structure of 1 consists of layers. Layers formed by fullerene and CS₂ molecules alternate with layers of TMTSF molecules. Peculiarities of the crystal structure of 1 are the nonplanar conformation of TMTSF molecules and the absence of shortened C…C contacts between adjacent fullerenes molecules. The energy of intermolecular TMTSF…C₆₀ interactions in the crystal was estimated.     

A restudy of the crystal structure of tetraaquastrontium dicitratoborate trihydrate

The crystal structure of Sr(H₂O)₄[(C₁₂H₁₁O₁₄)B] · 3H₂O (I) has been restudied and determined with a higher accuracy. The crystals are monoclinic, space group P2₁/n, a = 11.405(1) Å, b = 18.814(1) Å, c = 11.987(1) Å, β = 110.79(1)°; Z = 4. The structure was refined by full matrix least-squares calculation to R = 0.0547 on 5343 unique reflections with R _int = 0.0419. The structural units of crystal I are the Sr²⁺ cation, seven water molecules, and doubly charged dicitratoborate anion, which is not equivalent to the singly charged complex dicitratoborate anion identified previously in the crystal structures of complexes of boric and citric acids. The coordination polyhedron of the Sr²⁺ cation is a distorted dodecahedron composed of four O atoms of coordinated water molecules and four O atoms of two complex anions. The crystal packing of I is layered. Thirteen independent O-H…O and O-H…, O′ contacts form an intricate system of hydrogen bonds.     

Molecular tapes in the structure of isoguaninium chloride

Isoguanine, an analogue of guanine, is of intrinsic interest as a noncanonical nucleobase. The crystal structure of isoguaninium chloride (systematic name: 6‐amino‐2‐oxo‐1H,7H‐purin‐3‐ium chloride), C₅H₆N₅O⁺·Cl⁻, has been determined by single‐crystal X‐ray diffraction. Structure analysis was supported by electrostatic interaction energy (E_es) calculations based on charge density reconstructed with the UBDB databank. In the structure, two kinds of molecular tapes are observed, one parallel to (010) and the other parallel to (50). The tapes are formed by dimers of isoguaninium cations interacting with chloride anions. E_es analysis indicates that cations in one kind of tape are oriented so as to minimize repulsive electrostatic interactions.     

The crystal structure of tris(triphenylphosphine)gold(I)-[dodecahydrido-6-thia-nido-decaborate(1—)]

The crystal structure of tris(triphenylphosphine)gold(I)[dodecahydrido-6-thia-nido-decaborate(1—)], [(C₆H₅)₃P]₃AuB₉H₁₂S, has been determined using X-ray techniques and counter data. The compound is a salt consisting of [(C₆H₅)₃P]₃Au⁺ cations and B₉H₁₂S^? anions. The cation is trigonal and nearly planar with AuP distances of 2.382(5) Å and PAuP anglés of 119.3(36)°. The B₉H₁₂S^? thiaborane anion is an open icosahedral fragment with the S atom in the 6 position, on the periphery of the decaborane polyhedron. The structure is the same as that found in solution for the isoelectronic B₁₀H₁₄^2? anion. Crystals are triclinic, space group P$\text{1}$, with a = 13.086(12), b = 19.635(32), c = 11.180(8) Å, α = 103.60(16), β = 72.10(9), and γ = 94.76(15)°. The structure was refined by least squares to a conventional R of 0.077.     

Metal-phenoxyalkanoic acid interactions—12: The crystal and molecular structure of μ-aqua-di-μ-[(2-chlorophenoxy)ethanoato-(O,O′)]-bis[(2-chlorophenoxy)-ethanoato-bis(pyridine)nickel(II)]-water (1/1)

The crystal structure of the pyridine adduct of nickel (2-chlorophenoxy)-ethanote, {[Ni₂(2-CPA)₄(py)₄(H₂O)] · H₂O}, has been determined from three dimensional X-ray data at 293 K. Crystals of the complex are triclinic, space group P$\text{1}$, with two dimers in a unit cell of dimensions a = 21.740(5), b = 14.312(7), c = 9.044(2)Å, α = 96.69(4), β = 84.99(4), γ = 101.20(3)°. The structure was solved by direct methods and refined to 0.059 for 2682 ‘observed’ reflections. The dimer consists of two face-to-face NiO₄N₂ octahedra joined at their apical positions by a bridging water molecule [Ni(1)-Ow; 2.14(1)Å; Ni(2)-Ow, 2.10(1)Å; Ni(1)-Ôw-Ni(2), 116.9(4)°]. Two bidentate carboxyl groups of the 2-CPA molecules bridge the other two corners of the triangular face while the other two 2-CPA ligands are unidentate [Ni-O, 2.05(1)Å (mean)]. The coordination about each Ni is completed by two cis-related pyridine nitrogens [Ni-N; 2.11(1)Å (mean)]     

Synthesis and crystal structure of cadmium(II) complex with 2-pyrimidinecarboxamide

The complex [Cd(N₂H₃C₅ONH₂)₂(CH₃COO)₂] (I) was synthesized and its structure was determined. The crystals are monoclinic: space group C2/c, a = 14/416(1), b = 9.410(1), c = 13.708(1) Å, β = 113.82(1)°, V = 1701.0(1) ų, ρ(calcd.) = 1.862 g/cm³, Z = 4. The structure consists of individual complexes I united by the N-H…O hydrogen bonding system into supramolecular framework. The coordination sphere of the cadmium atom (on axis 2) involves two chelate pyrimidinecarboxamide ligands, which form five-membered chelate rings CdOCCN(Cd-N(2) 2.432(4), Cd-O(3) 2.388(4) Å), and two monodentate CH₃COO^? ions (Cd-O(1) 2.280(3) Å). The second O atom of the acetate group is involved in a weak contact with the Cd²⁺ ion (Cd-O 2.670(4) Å). With account for the latter two contacts, the coordination polyhedron of Cd is irregular octahedron.     

Synthesis, structure and luminescence properties of lanthanide complex with a new tetrapodal ligand featuring salicylamide arms

A new tetrapodal ligand 1,1,1-tetrakis{[(2′-(2-furfurylaminoformyl))phenoxyl]methyl}methane (L) has been prepared and their coordination chemistry with Ln^III ions has been investigated. The structure of {[Ln₄L₃(NO₃)₁₂]·H₂O}_∞ (Ln=Nd, Eu)] shows the binodal 4,3-connected three-dimensional interpenetration coordination polymers with topology of a (8⁶)₃(8³)₄ notation. [DyL(NO₃)₃(H₂O)₂]·0.5CH₃OH and [ErL(NO₃)₃(H₂O) (CH₃OH)]·CH₃COCH₃ is a 1:1 mononuclear complex with interesting supramolecular features. The structure of [NdL(H₂O)₆]·3ClO₄·3H₂O is a 2:1 mononuclear complex which further self-assembled through hydrogen bond to form a three-dimensional supramolecular structures. The result presented here indicates that both subtle variation of the terminal group and counter anions can be applied in the modulation of the overall molecular structures of lanthanide complex of salicylamide derivatives due to the structure specialties of this type of ligand. The luminescence properties of the Eu^III complex are also studied in detail.