The Crystal Structures of Two Hydro-closo-Borates with Divalent Tin in Comparison: Sn(H2O)3[B10H10] · 3 H2O and Sn(H2O)3[B12H12] · 4 H2O

Single crystals of Sn(H2O)3[B10H10] · 3 H2O and Sn(H2O)3[B12H12] · 4 H2O are easily accessible by reactions of aqueous solutions of the acids (H3O)2[B10H10] and (H3O)2[B12H12] with an excess of tin metal powder after isothermal evaporation of the clear brines. Both compounds crystallize with similar structures in the triclinic system with space group P$$\bar{1 }$$ 1 ¯ and Z = 2. The crystallographic main features are electroneutral $${}_{\infty }^{1} \{$$ ∞ 1 { Sn(H2O)3/1[B10H10]3/3} and $${}_{\infty }^{1} \{$$ ∞ 1 { Sn(H2O)3/1[B12H12]3/3} double chains running along the a-axes. Each Sn2+ cation is coordinated by three water molecules of hydration (d(Sn–O) = 221–225 pm for the B10 and d(Sn–O) = 222–227 pm for the B12 compound) and additionally by hydridic hydrogen atoms of the three nearest boron clusters (d(Sn–H) = 281–322 pm for the B10 and d(Sn–H) = 278–291 pm for the B12 compound), which complete the coordination sphere. Between these tin(II)-bonded water and the three or four interstitial crystal water molecules, classical bridging hydrogen bonds are found, connecting the double chains to each other. Furthermore, there is also non-classical hydrogen bonding between the anionic [BnHn]2− (n = 10 and 12) clusters and the crystal water molecules pursuant to B–Hδ−$$\cdots$$ ⋯ δ+H–O interactions often called dihydrogen bonds.

N,N-bis(2-quinolinylmethyl)benzylamine

N,N-bis(2-quinolinylmethyl)benzylamine (1) was synthesized under basic conditions from a pseudo-three-component reaction between benzylamine and two molecules of 2-(quinolinylmethyl)chloride, resulting in the formation of two N–C bonds in a single step. Compound (1) crystallizes in the triclinic system of the P-1 space group. The unit cell comprises a dimer of 1, in which the monomers are linked by two complementary hydrogen bonds between N1 and H′1–C′1 of another molecule. The dimers form chains along the a-axis through intermolecular interactions between the N′2 acceptor atoms and C″17 donors from molecules in the nearest neighboring dimer. These interactions form extended sheets of the dimers of 1, along the ab plane. The quinolinylmeth-2-yl groups of 1 lie in almost orthogonal planes and their N1/2(q) donor atoms are away from the apical amino N3 atom.

Crystal Structure of Novel Terephthalate Salt of Antiarrhythmic Drug Disopyramide

1:1 salt of Disopyramide (DPA) with Terephthalic acid (TA) was obtained by the slow solvent evaporation and the slurry crystallization methods. X-ray single crystal diffraction of DPA:TA confirmed the formation of salt by the transfer of an acidic proton from one of the carboxylic acidic groups of TA to the tertiary amino group of the chain moiety (N3-nitrogen atom) of the DPA molecules. DPA:TA salt crystals crystalize in the triclinic system with space group P-1. The asymmetric unit, comprising one protonated DPA and one TA anion, are linked by a strong charge assisted N+–H∙∙∙O¯ hydrogen bond and a C–H∙∙∙O¯ hydrogen bond. Moreover, structural characterization of DPA:TA salt was carried out using Fourier transform infrared spectroscopy, differential scanning calorimeter, thermogravimetric analysis, and powder X-ray diffraction techniques

N,N-bis(2-quinolinylmethyl)benzylamine

The compound, C27H23N3 (1), crystallizes in the triclinic system of the P-1 space group. The unit cell comprises a dimer of 1, in which the monomers are linked by two complementary hydrogen bonds between N1 and H1-C1 of another molecule. The dimers form chains along the a-axis through intermolecular interactions between the N2 acceptor atoms and C17 donors from molecules in the nearest neighbouring dimer. These interactions form extended sheets of the dimers of 1, along the ab plane. The quinolinylmeth-2-yl groups of 1 lie in almost orthogonal planes and their N1/2(q) donor atoms being away from the apical amino N3 atom.

Synthesis, structure and magnetic properties of two new spin-chain compounds Ca2Ni(HSeO3)2(SeO3)2 and Na2Cu(SeO3)2·2H2O

Two new selenite compounds Ca2Ni(HSeO3)2(SeO3)2 (CaNi) and Na2Cu(SeO3)2·2H2O (NaCu) were obtained by a hydrothermal method. Both compounds crystallize in the triclinic system of space group P-1, featuring a selenite-bridged one-dimensional...

Field-Induced Single-Ion Magnet Phenomenon in Hexabromo- and Hexaiodorhenate(IV) Complexes

Two mononuclear ReIV complexes of general formula (PPh4)2[ReX6] [PPh4+ = tetraphenylphosphonium cation, X = Br (1) and I (2)] have been prepared and structurally and magnetically characterised. Both compounds crystallise in the triclinic system with space group Pī. Their structures are made up of hexahalorhenate(IV), [ReX6]2−, anions, and bulky PPh4+ cations. Each ReIV ion in 1 and 2 is six-coordinate and bonded to six halide ions in a quasi regular octahedral geometry. In their crystal packing, the [ReX6]2− anions are well separated from each other through the organic cations, generating alternated anionic and cationic layers, and no intermolecular Re−X···X−Re interactions are present. Variable-temperature dc magnetic susceptibility measurements performed on microcrystalline samples of 1 and 2 show a very similar magnetic behaviour, which is typical of noninteracting mononuclear ReIV complexes with S = 3/2. Ac magnetic susceptibility measurements reveal the slow relaxation of the magnetisation in the presence of external dc fields for 1 and 2, hence indicating the occurrence of the field-induced single-ion magnet (SIM) phenomenon in these hexabromo- and hexaiodorhenate(IV) complexes.

Synthesis, structure and hydrogen sorption properties of a pyrazine-bridged copper(I) nitrate metal-organic framework

A new copper(I) pyrazine-bridged coordination polymer [Cu2(pyz)3(NO3)2]·2DMF] (pyz = pyrazine) (1) has been synthesized and characterized by FT-IR, TG/DTG, DSC and single crystal X-ray diffraction techniques. The X-ray crystallographic result reveals a two-dimensional network structure containing hexagonal pores. Thermal analysis of compound 1 reveals it is stable to 380 °C, and gas sorption studies showed that it adsorbs 1.04 wt% hydrogen at 1 atm and 77 K. Compound 1 crystallizes in a triclinic system, space group P-1 (no. 2), a = 7.9550(2) Å, b = 7.9810(2) Å, c = 11.0660(3) Å, α = 76.328(1)°, β = 71.115(1)°, γ = 84.577(1)°, V = 645.79(3) Å3, Z = 2, T = 150(2) K, μ(MoKα) = 1.709 mm-1, Dcalc = 1.639 g/cm3, 11111 reflections measured (7° ≤ 2Θ ≤ 54.96°), 2951 unique (Rint = 0.0539) which were used in all calculations. The final R1 was 0.0346 (>2σ(I)) and wR2 was 0.0727 (all data).

About the crystalline structure of vanadates Ca1.5±0.1Mn0.5±0.1V2O7 and Ca1.5Cd0.5V2O7

The crystal structures of Ca1.5Mn0.5V2O7 (I) and Ca1.5Cd0.5V2O7 (II) synthesized by the citrate method and by a conventional solid-state reaction, respectively, were determined using X-ray powder diffraction data. It was found that the compound I has a monoclinic crystal structure a = 4.88563(9) Å, b = 11.21279(22) Å, c = 5.69643(11 Å), β = 96.376(7)°, V = 310.132(10) Å3 (space group P21/c), Z = 2). Compound I has a narrow homogeneity region Ca1.5±0.1Mn0.5±0.1V2O7. The vanadate Ca1.5Cd0.5V2O7 crystallizes in the triclinic system with the parameters a = 6.66139(6) Å, b = 6.93019(7) Å, c = 7.02211(6) Å, α = 85.4404(9)°, β = 63.7505(7)°, γ = 82.5515(10)° и V = 288.201(5) Å3 (space group P$\bar 1$, Z = 2). It is one of the formulations of the primary solid solution, formed as a result of the substitution of part of the calcium cations for cadmium cations in Ca2V2O7.

Synthesis, structural characterization, and hydrogen bonds of Co9(OH)14[SO4]2

The new compound Co9(OH)14[SO4]2 was synthesized using a hydrothermal method from LiF, Na2SO3, and Co(CH3COO)2·4H2O in a molar ratio of 1:1:1 in the presence of atmospheric oxygen. Its crystal structure was determined from single crystal X-ray diffraction data. Co9(OH)14[SO4]2 crystallizes in the triclinic system, space group P1̅ with a=7.693(2) Å, b=8.318(2) Å, c=8.351(2) Å, α=82.375(5)°, β=77.832(4)°, γ=68.395(4)°, V=484.8(2) Å3, and Z=2. Its structure is composed of cobalt-containing sheets interconnected by SO4 tetrahedra. Bent and symmetrically trifurcated hydrogen bonds have been observed. Furthermore, structural similarities with hydrozincite and brucite minerals have been noticed.

Synthesis and Crystal Structure of 3-3’-Diaminomethyldipropylammonium Hexachlorobismuthate (III)

Synthesis and crystal structure of 3-3’-diamino-N-methyldipropylammonuim hexachlorobismuthate (III) are reported. The compound crystallizes in the triclinic system with space group P1. The unit cell dimensions are: a = 7.5580(5), b =7.8710(6), c = 8.3709(7) Å with Z=1. The crystal is built up of separated [BiCl6]3- octahedral anions and 3-3’-diamino-N- methyldipropylammonium cations. The organic layers are arranged in sandwich between the anionic ones. The crystal packing is governed by means of the ionic N–H···Cl hydrogen bonds, forming a three dimensional network.