Acta Crystallographica Section E: Crystallographic Communications最新文献

The crystal structure of a one-dimensional anionic bis-muth(III) iodide coordination polymer, catena-poly[[tri-iodido-bis-muth(III)]-di-μ-iodido-[tri-iodido-bis-muth(III)]-μ-4,7-bis-(pyridin-4-yl)benzo[c][1,2,5]thia-diazole], {(C₁₆H₃₆N)₂[Bi₂I₈(C₁₆H₁₀N₄S)]} _n , constructed from μ₂-iodido-bridged dinuclear [Bi₂I₈]^2- units and the π-conjugated N-donor ligand 4,7-bis-(pyridin-4-yl)benzo[c][1,2,5]thia-diazole (dpbt) is reported. Each Bi^III centre adopts a distorted octa-hedral geometry with five iodido ligands and one nitro-gen donor atom. The dinuclear units are linked by dpbt to form infinite chains, with charge balance provided by tetra-n-butyl-ammonium cations. The crystal packing is governed by C-H⋯I hydrogen bonds and C-H⋯π inter-actions, while π-π stacking is suppressed by steric effects. Anionic iodido-bis-muth polymers of this type are rare.

The cocrystal formed between 2,3-di-amino-pyrazine and 2,3,5,6-tetra-fluoro-phthalic acid, crystallizes as the solvated salt bis-(2,3-di-amino-pyrazin-1-ium) 2,3,5,6-tetra-fluoro-phthalate-2,3,5,6-tetra-fluoro-phthalic acid (1/1), 2C₄H₇N₄ ⁺·C₈F₄O₄ ^2-·C₈H₂F₄O₄, in the triclinic space group P1 with one unique protonated 2,3-di-amino-pyrazinium cation, one half a tetra-fluoro-phthalic acid mol-ecule and one half of a tetra-fluoro-phthalate anion. The cocrystal forms a supra-molecular network with cooperative neutral and charge-assisted hydrogen bonding. In this, the linear network of alternating pyrazinium and tetra-fluoro-phenyl moieties is crosslinked through bifurcated hydrogen bonds of two amino H atoms and a carboxyl oxygen to form a corrugated two-dimensional network.

Crystals of the title compound, [Cu(NCS)(C₆H₈N₂)] _n (C₆H₈N₂ = 2,6-di-methyl-pyrazine), were prepared by the reaction of CuNCS and 2,6-di-methyl-pyrazine in aceto-nitrile. The asymmetric unit consists of one Cu^I cation, one thio-cyanate anion and one 2,6-di-methyl-pyrazine ligand with all atoms lying on general positions. The copper cations are tetra-hedrally coordinated by two S- and one N-bonded thio-cyanate anions and one 2,6-di-methyl-pyrazine ligand, which s coordinated to the metal center with the N atom that is not adjacent to the methyl groups. The copper cations are linked by the μ-1,3,3 (N,S,S) bridging thio-cyanate anions into layers that lie parallel to the ac plane. The layers are stacked perpendicular to the b-axis direction and are separated by the 2,6-di-methyl-pyrazine ligands. The title crystal structure is compared with those of related CuNCS compounds with isomeric di-methyl-pyrazine ligands.

The crystal structure of the nickel(II) macrocyclic title complex, trans- [Ni(ClO₄)₂(C₁₆H₃₈N₆)], was analyzed using synchrotron radiation. The coordination environment consists of four nitro-gen atoms from the ligand [Ni-N = 1.9382 (16), 1.9378 (17) Å] and two perchlorate oxygen atoms [Ni-O = 2.878 (3) Å], adopting an octa-hedral geometry with slight tetra-gonal distortion. The structural comparison with its Cu^II analogue reveals a notable elongation in the axial Ni-O bonds, which is attributed to the steric hindrance of the macrocyclic ligand and weak axial coordination. Supra-molecular inter-actions involving hydrogen bonding further consolidate the three-dimensional crystal packing.

The title compounds, [ZnCl₂(C₄H₅N₃)₂] (1) and [ZnI₂(C₄H₅N₃)₂] (2) (C₄H₅N₃ = 2-amino-pyrimidine), were prepared from a solvent mixture of tri-chloro-methane and methanol and structurally characterized. The asymmetric unit of 1 consists of one Zn^II cation that is situated on a twofold rotation axis and one chloride anion as well as one 2-amino-pyrimidine ligand in general positions. The asymmetric unit of 2 is built up of one Zn^II cation, two iodide anions and two 2-amino-pyrimidine ligands, all of them located in general positions. In both compounds, the metal cations are tetra-hedrally coordinated by two halide anions and two 2-amino-pyrimidine ligands. In compound 1, the discrete complexes are linked by N-H⋯Cl hydrogen bonds into layers that are further connected by weak C-H⋯Cl inter-actions. In compound 2, the complexes are connected via N-H⋯I hydrogen bonds into layers that are further linked by a number of N-H⋯I and C-H⋯I hydrogen bonds. Compound 1 represents a second polymorphic modification of ZnCl₂(C₄H₅N₃)₂ that crystallizes in the ortho-rhom-bic non-centrosymmetric space group Pba2, whereas the known form crystallizes in the monoclinic, centrosymmetric space group C2/c [Lin & Zeng (2007 ▸). Acta Cryst. E63, m1597].

The title compound (E)-2-(benzo[d]thia-zol-2-yl)-N'-(1-(4-bromo-phen-yl)ethyl-idene)acetohydrazide, C₁₇H₁₄BrN₃OS, crystallizes in space group P2₁/c with Z = 4. The configuration across the formal N=C double bond at the hydrazide moiety is E; the atom sequence C-C-C(= O)-N-N=C-(bromo-phen-yl) is very approximately planar (r.m.s. deviation 0.17 Å, when all carbon atoms of the bromo-phenyl group are included), being synperiplanar around the C(=O)-N bond and anti-periplanar (choosing the appropriate final atom C_Ar) elsewhere. The inter-planar angle to the benzo-thia-zole unit (r.m.s. deviation 0.01 Å) is 69.75 (2)°. The main packing feature is a classical inversion-symmetric dimer with hydrogen bonds of the type N-H⋯O=C. This combines with a rather long N_thia-zole⋯Br halogen bond to form a thick layer structure parallel to the bc plane.

The title compound, (C₃H₅N₂)₄[Co(C₃H₄N₂)₆](C₉H₃O₆)₂·2H₂O (1), was synthesized by slow evaporation of mixed ethano-lic solutions of CoCl₂, benzene-1,3,5-tri-carb-oxy-lic acid (H₃btc) and imidazole (Im) at room temperature. The crystal structure comprises [Co(Im)₆]²⁺ cations, btc^3- anions, Im⁺ cations and water mol-ecules in a 1:2:4:2 ratio. The crystal packing shows alternating layers stacked along the c-axis direction, linked primarily by hydrogen bonds of the types N-H⋯O (between cations and anions) and O-H⋯O (between anions and water mol-ecules).

The title coordination complex, bis-(μ-pyridin-1-ium-3-carboxyl-ato-κ² O:O')bis-[di-aqua-bis-(nitrato-κ² O,O')calcium(II)], [Ca₂(C₆H₅NO₂)₂(NO₃)₄(H₂O)₄], was prepared from calcium nitrate and nicotinic acid in a water-ethanol solvent mixture. The asymmetric unit contains a half mol-ecule of the complex, with the calcium atom exhibiting a coordination number of eight, forming a distorted dodeca-hedral geometry with a mixed-ligand environment. The μ₂-O,O' bridging zwitterionic nicotinic acid mol-ecules generate a centrosymmetric dinuclear complex. The extended structure features N-H⋯O, O-H⋯O and C-H⋯O hydrogen bonds, which generate a three-dimensional network. Hirshfeld surface and two-dimensional fingerprint plot analyses were performed to qu-antify and visualize the inter-molecular inter-actions contributing to the overall cohesion of the structure.

In the title salt, (C₂H₄N₃S)₂[MnCl₂(C₃H₂O₄)(H₂O)₂], the central Mn^II atom of the complex anion adopts a distorted octa-hedral coordination environment, defined by two aqua, two chlorido, and one bidentate malonato ligands. The anion is charge balanced by two thia-diazole moieties protonated at one of the heterocyclic N atoms. In the crystal, the cations and anions engage in extensive hydrogen-bonding inter-actions and short S⋯Cl contacts; additional π-π stacking inter-actions are present between adjacent cations. Hirshfeld surface analysis was used to qu-antify the inter-molecular inter-actions of the complex anion, revealing that H⋯O, H⋯Cl, and H⋯H inter-actions contribute most to the crystal packing.

We report the single-crystal X-ray diffraction structures of the azo-benzene-bridged aza-18-crown-6 cryptand 7,16-[3,3'-(diazene-1,2-di-yl)bis-(1,3-phenyl-enecarbon-yl)]-1,4,10,13-tetra-oxa-7,16-di-aza-cyclo-octa-decane, C₂₆H₃₂N₄O₆, 1, and its sodium complex poly[[{μ-7,16-[3,3'-(diazene-1,2-di-yl)bis-(1,3-phenyl-enecarbon-yl)]-1,4,10,13-tetra-oxa-7,16-di-aza-cyclo-octa-deca-ne}bis-{tetra-kis-[3,5-bis-(tri-fluoro-meth-yl)phen-yl]borato}disodium] benzene disolvate], {[Na₂(C₃₂H₁₂F₂₄B)₂(C₂₆H₃₂N₄O₆)]·2C₆H₆} _n . The free ligand 1 crystallizes in space group P2₁/n and adopts an elongated strain-distorted crown conformation with a slightly twisted azo-benzene unit. In contrast, 2 [obtained with sodium tetra-kis-3,5-bis-(tri-fluoro-meth-yl)phenyl borate (NaBArF)] crystallizes in space group P1 and features multiple Na⁺ centers that assemble into a three-dimensional network in the solid state. Hirshfeld surface analysis was used to provide a complementary, qu-anti-tative description of the dominant inter-molecular contacts governing the crystal packing.