Space Group Pbca Research Articles

Crystal structure, optical and electronic properties studies on an hybrid multifunctional MnCl4-based material

In this research, the multifunctional organic-inorganic hybrid PEA-MnCl4 [PEA = (C6H5–C2H4–NH3)2] was subjected to single-crystal X-ray diffraction, X-ray diffraction powder, UV-visible spectroscopy, scanning electron microscopy (SEM), and density functional theory, using projector augmented wave (PAW), based on U-Hubbard Hamiltonian (DFT+U) investigations. At 293(2) K, PEA-MnCl4 crystallizes in Orthorhombic system, Pbca space group (a = 7.202(5) A, b = 7.293(5) A, c = 39.386(5) A, and Z = 8). The optical study reveals that the compound undergoes an indirect optical transition with phonon-assisted Mn2+ d-d transitions in the visible region with an energy gap of about 2.14 eV, due to the internal transition of metal (orbital d). The implementation of the Hubbard U term in the calculation using (GGA+U) approximation allows more comprehension on the material behavior and shows that it keeps the antiferromagnetic state. The energy gap calculated (2.07 eV) is in good agreement with the experimental value. The electronic densities of states were computed and analyzed.

Hydrothermal Synthesis of Co(II) Complex, a Precursor for the Synthesis of Octahedral Co3O4 Nanoparticles :An Active Catalyst for the Removal of Cr(VI)

This work presents the hydrothermal synthesis of [Co(2,2′-bipyridine)2(NCS)2] (1) (150 °C, 48 h). The structure of 1 was characterized step by step by elemental analysis CHN, atomic absorption spectroscopy, Fourier transform infrared spectroscopy, thermal gravimetric analysis, differential thermal analysis and single crystal X-ray diffraction. Complex 1 crystallizes in orthorhombic structure with space group Pbca of expected composition. The full geometry optimization and energy values of the highest occupied molecular orbital and the lowest unoccupied molecular orbital were performed using GAUSSIAN 09. Magnetic characterization of complex 1 revealed a paramagnetic behavior at room temperature. Complex 1 was used as a significant precursor to prepare nanoparticles of Co3O4 by thermal decomposition process. The obtained Co3O4 was characterized by various techniques such as FT-IR spectroscopy, powder X-ray diffraction, nitrogen adsorption–desorption isotherms, scanning electron microscope and vibrating sample magnetometer. Co3O4 nanoparticles revealed a ferromagnetic behavior at room temperature. The SEM images of Co3O4 nanoparticles showed an octahedral morphology with a particle size of about 25 nm. Complex 1, commercial, and synthetic Co3O4 nanoparticles were used for the removal of Cr(VI) ions from the aqueous solution. The results showed that Co3O4 nanoparticles which obtained through thermal decomposition of inorganic complex could be employed as an efficient adsorbent for the removal of Cr(VI). Batch adsorption studies were conducted to find the optimal adsorption conditions such as contact time and pH. The results indicate that the adsorption kinetics data followed a pseudo-second-order model.

Synthesis, characterizations, crystal structures, BSA-binding, molecular docking, and cytotoxic activities of nickel(II) and copper(II) coordination complexes with bidentate N,S-chelating ligand

In the present investigation, we report the synthesis and characterization of three novel nickel(II) [Ni(L)2] (1) and copper(II) [Cu(L)2] (2a) and [Cu(L)2] (2b) complexes, which are made through the coordination of (E)-1-(2-methoxybenzylidine)-4-phenylethiosemicarbazone (HL) as bidentate N,S-ligand. Several modern techniques including experimental electronic and fluorescence spectroscopy, single-crystal X-ray crystallography, molecular docking and BSA-binding are used to characterize the isolated coordination compounds. X-ray crystallography, FT-IR and UV–visible spectra agree with the observed crystal structures. The crystallographic and spectroscopic studies confirmed that these complexes display four-coordinate square-planar trans-[MN2S2] coordination geometry, whose central metal(II) atom lies on the center of symmetry. Complexes 1 and 2a crystallized in the orthorhombic system of the space group Pbca whereas 2b crystallized in the monoclinic system of P21/c. The binding affinity of complexes towards bovine serum albumin (BSA) was determined by UV–visible and fluorescence spectrophotometric methods. The cytotoxic/antiproliferative potential of the synthesized compounds on human cell lines was also investigated by MTT assay.

Composite topological nodal lines penetrating the Brillouin zone in orthorhombic AgF2

It has recently been found that nonsymmorphic symmetries can bring many exotic band crossings. Here, based on symmetry analysis, we predict that materials with time-reversal symmetry in the space group of Pbca (No. 61) possess rich symmetry-enforced band crossings, including nodal surfaces, fourfold degenerate nodal lines and hourglass Dirac loops, which appear in triplets as ensured by the cyclic permutation symmetry. We take Pbca AgF2 as an example in real systems and studied its band structures with ab initio calculations. Specifically, in the absence of spin-orbit coupling (SOC), besides the above-mentioned band degeneracies, this system features a nodal chain and a nodal armillary sphere penetrating the Brillouin zone (BZ). While with SOC, we find a new configuration of the hourglass Dirac loop/chain with the feature traversing the BZ, which originates from the splitting of a Dirac loop confined in the BZ. Furthermore, guided by the bulk-surface correspondence, we calculated the surface states to explore these bulk nodal phenomena. The evolution of these interesting nodal phenomena traversing the BZ under two specific uniaxial strains is also discussed.

Tris(μ2-2-meth-oxy-6-{[(2-sulfido-eth-yl)imino]meth-yl}phenolato)trinickel(II) di-methyl-formamide monosolvate: crystal structure, spectroscopic characterization and anti-bacterial activity.

The title trinuclear nickel(II) complex, [Ni3(C10H11NO2S)3]·C3H7NO, with a Schiff base ligand formed in situ from 2-amino-ethane-thiol and o-vanillin crystallizes in the ortho-rhom-bic space group Pbca. Its asymmetric unit consists of one neutral Ni3 L 3 mol-ecule and one DMF solvent mol-ecule. The solid-state organization of the complex can be described as an insertion of the solvent mol-ecules within the crystallographically independent trinuclear NiII species. Several C-H⋯π edge-to-face inter-actions and π-π stacking inter-actions link the components in the crystal. A first example of a short inter-molecular C-H⋯Ni contact is found. Anti-bacterial in vitro screening revealed that the title compound has anti-bacterial activity, the best effect being against Acinetobacter baumannii.

Synthesis and Characterization of the Tin Iodide Borate Sn3[B3O7]I.

The tin iodide borate Sn3[B3O7]I was synthesized via a hydrothermal synthesis and crystallizes in the centrosymmetric space group Pbca (no. 61) possessing lattice parameters of a = 1071.8(3), b = 852.3(2), and c = 2016.8(5) pm and Z = 8. Characteristic for the structure are infinite chains along the b axis, built up of three membered B3O8 rings consisting of one BO3 unit and two corner-sharing BO4 tetrahedra. The three tin cations are oriented differently: one cation is located layer-like between the infinite chains, and the other two cations show an orientation in a row with the infinite chain. In this structure, only one of the three tin cations exhibits a coordination to the halogen anion. The new centrosymmetric tin iodide borate Sn3[B3O7]I was investigated by single-crystal diffraction, vibrational spectroscopy, powder X-ray diffraction data, thermogravimetry, differential scanning calorimetry, and DFT calculations.

Dinuclear platinum(II) complexes of imidazophenanthroline-based bridging ligands as potential anticancer agents: synthesis, characterization, and in vitro cytotoxicity studies.

The synthesis and characterization of the dinucleating ligands 1,2-bis(2-(1H-imidazo[4,5-f][1,10]phenanthrolin-2-yl)phenoxy)ethane (L1) and 1,2-bis(2-(1H-imidazo[4,5-f][1, 10]phenanthrolin-2-yl)phenoxy)hexane (L2) and their dinuclear complexes [Pt2(L1)Cl4] (1) and [Pt2(L2)Cl4] (2) and the in vitro cytotoxicity of the complexes against HeLa, HepG2, and MCF-7 cell lines are reported. Ligand L1 crystallizes in the orthorhombic system with the space group Pbca. The complexes 1 and 2 undergo aquation following first-order kinetics. The MTT and trypan blue assays indicate higher cytotoxicity of the complexes towards the HepG2 and MCF-7 cell lines compared to cisplatin. The AO/EB assay and flow cytometry by Annexin V alexa fluor®488/PI double staining assay demonstrate distinct morphological changes of apoptosis in a dose dependent manner. The cell cycle analysis shows a marked decrease in the DNA content in the G0/G1 phase with an increase in the G2/M phase on increasing the concentration of the complexes. The potential of the complexes as anticancer agents is demonstrated by their antiproliferative activity on the cell lines. The complexes interact with the major groove of DNA through H-bonding between the imidazole N-H protons and the nucleotide residues DC`21/N4 (cytosine) for complex 1 and DT`7/O2 (thymine) and DT`19/O2 (thymine) for complex 2, with the binding energy of - 1.98 and - 4.45kcal/mol, respectively. Dinuclear Pt(II) complexes of imidazophenanthroline-based dinucleating ligands exhibit antiproliferative activity against HeLa, HepG2, and MCF-7 cell lines.

Synthesis and Structural Characterization of 2-(2-Aminophenyl) Benz imidazole

A Benz imidazole derivative, 2-(2-aminophenyl) Benz imidazole, was synthesized by simple one-pot synthesis method. Its structure was characterized by X-ray single-crystal structural analysis. The results of crystal analysis are C13H11N3, Mr = 209.25, orthorhombic, space group Pbca, a = 7.7679 (16) Å, b = 11.855(2) Å, c = 22.552(5) Å, α = β = γ = 90°, V = 2076.7(7) Å3, Z = 8, Dc = 1.339 g·cm−3, μ = 0.083 mm−1, F (000) = 880, and final R1 = 0.0365, ωR2 = 0.0947. The 2-(2-aminophenyl) Benz imidazole molecule is co-planar. The title compound molecules form 1D chained structure and 2D layered structure by the interaction of intermolecular N-H.N hydrogen bonds.

Study on structure and properties of two metal coordination polymers prepared by 3,5-Bis (4-carboxy-phenoxy)benzoic acid

Two new metal-organic frameworks (MOFs) [Zn(HBCPBA)(tpim)]·H2O (1) and [Co(HBCPBA)(tpim)] (2) were achieved by reactions of corresponding metal salt with mixed organic ligand of 3,5-Bis(4-carboxy-phenoxy)benzoic acid(H3BCPBA) and 2,4,5-tris(4-pyridyl)imidazole (tpim). These crystals were clearly characterized by elemental analysis, IR spectra, X-ray powder diffraction (PXRD) as well as X-ray single-crystal diffraction. The crystal structures showed that the compound 1 crystallizes in the monoclinic system, with P21/c space group, displays a two-dimensional network structure, the compound 2 crystallizes in the orthorhombic system, with Pbca space group, also exhibits a two-dimensional network structure, which has a zero-dimensional ring structure link Co(II) ion by N-containing ligand tpim. Remarkably, 1 can act as fluorescence probe for sensing Fe3+ ion and 2 has electrochemically active substances with good electrochemical reversibility.

Synthesis, characterization and properties of lanthanide complexes with different ancillary ligands

By introducing different ancillary ligands and solvent molecules, four lanthanide complexes [Yb2(L)2(acac)2(CH3OH)2]·CH3OH·H2O (1), [Lu2(L)2(acac)2(CH3OH)2]·2CH3OH (2), [Yb2(L)2(dbm)2(CH3OH)2]·CH3OH (3), and [Lu2(L)2(dbm)2(C2H5OH)2] (4) (where H2L = 2-(hydroxyimino)-2-[(5-methyl-2-hydroxyphenyl)methylene]hydrazide, Hacac = acetylacetonate and Hdbm = 1,3-diphenyl-1,3-propanedione) have been synthesized and characterized. The X-ray structural analyses show that complexes 1 and 2 are isostructural in the Triclinic system, space group Pī, complex 3 crystallizes in Monoclinic system, space group P21/c, and complex 4 crystallizes in Orthorhombic system, space group Pbca. The metal ions in complexes 1–4 are all eight-coordinated and show a similar distorted triangular dodecahedron coordination geometry. The fluorescence properties of complexes 1–4 were also investigated. Complexes 1 and 3 showed characteristic emission peaks of Yb(III) ion, while complexes 2 and 4 exhibited emission peaks consistent with that of the ligand when they were excited at the same wavelength.

Crystal structure of strontium perchlorate anhydrate, Sr(ClO4)2, from laboratory powder X-ray diffraction data.

The crystal structure of strontium perchlorate anhydrate, Sr(ClO4)2, was determined and refined from laboratory powder X-ray diffraction data. The material was obtained by dehydration of Sr(ClO4)2·3H2O at 523 K for two weeks. It crystallizes in the ortho-rhom-bic space group Pbca and is isotypic with Ca(AlD4)2 and Ca(ClO4)2. The asymmetric unit contains one Sr, two Cl and eight O sites, all on general positions (Wyckoff position 8c). The crystal structure consists of Sr2+ cations and isolated ClO4 - tetra-hedra. The Sr2+ cation is coordinated by eight O atoms from eight ClO4 - tetra-hedra. The validity of the crystal structure model for Sr(ClO4)2 anhydrate was confirmed by the bond valence method.

Contributions to the stereochemistry of zirconium oxysalts—part II: syntheses and crystal structures of Zr(SeO3)(SeO4), Zr4(SeO3)(SeO4)7, and Zr3(SeO3)(SeO4)5·2H2O

Three new compounds Zr(SeO3)(SeO4), Zr4(SeO3)(SeO4)7, and Zr3(SeO3)(SeO4)5·2H2O were synthesized at low-hydrothermal conditions (Teflon-lined steel vessels, 220 °C) from mixtures of Zr2O2(CO3)(OH)2, H2SeO4, and minor contents of water. Colorless single crystals up to several tenth of a mm in size, obtained within 1 week, were studied by single crystal X-ray techniques. Zr(SeO3)(SeO4) crystallizes in the orthorhombic space group Pbca (No. 61), with a = 8.291 (2) A, b = 9.458 (2) A, c = 15.357 (3) A, V = 1204.2 (5) A3, Z = 8, R1 = 0.0322. Zr4(SeO3)(SeO4)7 is monoclinic, space group P21/n (No. 14), with a = 5.313 (1) A, b = 10.704 (2) A, c = 10.484 (2) A, β = 104.13 (1)°, V = 578.2 (1) A3, Z = 1, R1 = 0.0172. Two independent selenium atoms are present in this structure: one forming a SeO4 tetrahedron, and the other one exhibiting mixed occupation by ¾ Se6+ and ¼ Se4+; its coordination is, therefore, partially disordered. Zr3(SeO3)(SeO4)5·2H2O crystallizes in the triclinic space group P1 (No. 1), with a = 5.273 (1) A, b = 8.079 (2) A, c = 11.959 (2) A, α = 82.60 (1)°, β = 88.27 (1)°, γ = 89.87 (1)°, V = 505.1 (1) A3, Z = 1, R1 = 0.0235, but exhibits strong centrosymmetric pseudosymmetry; the inversion center is violated only by replacement of one selenate(VI) tetrahedron by a trigonal pyramidal selenite(IV) group as pseudo-centric counterpart. Hydrogen bonds in this compound show donor–acceptor distances within the range of 2.67–2.81 A. All three framework structures are unique and built up from corner-sharing polyhedra. In all three compounds, mean cation-oxygen bond lengths (Zr[6]: 2.062 and 2.067 A; Zr[7]: 2.132, 2.137 and 2.139 A; Se4+[3]: 1.675 and 1.680 A, excluding the disordered group; Se6+[4]: 1.621–1.641 A) are comparatively short, resulting in rather high bond valence sums.

Synthesis, crystal structure and biological activity of 6-(3-chloropropoxy)-4-(2-fluorophenylamino)-7-methoxyquinazoline

The title compound, 6-(3-chloropropoxy)-4-(2-fluorophenylamino)-7-methoxyquinazoline, was synthesized by selective nucleophilic attack at C-1 of 1-bromo-3-chloropropane by the potassium salt of 4-(2-fluorophenylamino)-7-methoxyquinazolin-6-ol, which was prepared from 7-methoxy-4-oxo-3,4-dihydroquinazolin-6-yl acetate in three steps. The compound crystallized as an ethyl acetate complex (C20H21ClFN3O3, Mr = 405.85), and X-ray crystallography showed that the crystal belongs to the orthorhombic system, space group Pbca with a = 12.7407(4) Å, b = 14.0058(5) Å, c = 21.7726(7) Å, α = 90°, β = 90° and γ = 90°. The whole molecule is stacked into a three-dimensional structure via weak N–H…N hydrogen bonding between molecules. The compound acts as an effective inhibitor on the proliferation of a lung cancer cell line.

Germanium-8-Hydroxyquinoline hydroxides: Synthesis, structure and luminescence properties

A new germanium hydroxide coordinated by 8-Hydroxyquinoline (8-HQ), C18H14GeN2O4 (Hereafter, GeHQ1) was synthesized via either a hydrothermal or common solution approach. Its structure was determined with both powder XRD and single crystal X-ray diffraction techniques. GeHQ1 crystallizes in orthorhombic symmetry, space group Pbca (No. 61) with unit-cell parameters: a = 8.7537(5) Å, b = 13.9817(7) Å, c = 24.8775(13) Å, and V = 3044.8(3) Å3, Z = 8, R = 0.0337 for reflections with I >2 sigma(I) and wR = 0.0803. The structure of GeHQ1 is built up from one germanium metal center octahedrally coordinating with two 8-Hydroxyquinoline anions (8-Q) and two hydroxyl groups and each two adjacent building units are held into a dimer via extensive hydrogen-bonding interaction between two relatively closer hydroxyl groups (2.936 Å) of two adjacent molecules. The crystals were also studied by SEM (scanning electron microscopy), EDS (energy dispersive analysis of X-rays spectroscopy), FT-IR spectrum and TGA (Thermogravimetric analysis). The photoluminescence properties were investigated in room temperature as well as lower temperature (14 K).

Analysis of two novel 1–4 quinolinone structures with bromine and nitrobenzyl ligands

The scientific community has shown particular interest in the study of quinolinones-a class of bicyclic organic compounds. An example of these compounds are the 4-quinolinones, considered to be very useful building blocks, since they can adapt their molecular structures with different ligands for applications in various fields such as pharmacy, medicine, physics and engineering. The compounds (E)-3-(benzylidene)-2-(3-nitrophenyl)-2,3-dihydro-1-(phenylsulfonyl)-quinolin-4-(1H)-one (NFQ) and (E)-3-(benzylidene)-2-(4-bromophenyl)-2,3-dihydro-1-(phenylsulfonyl) quinolin-4-(1H)-one (BFQ) were synthesized and characterized by infrared spectroscopy, 1H and 13C NMR, and melting point. NFQ crystallized in the orthorhombic Pbca space group while BFQ appears in the monoclinic P21/n space group. X-ray diffraction was used to evaluate their crystallographic structures, and Hirshfeld surface evaluates the intermolecular interactions, supramolecular arrangement and packaging. Theoretical vibrational assignments and calculated electronic properties also demonstrate acceptable agreement between experimental and theoretical results.

3D energy frameworks of dimethylbenzophenone tetramorphs

The tetramorphth crystals of 4,4–dimethylbenzophenone (D) were obtained using slow-evaporation crystallization method and the structure is elucidated using single crystal X-ray diffraction technique. D crystallizes in the orthorhombic crystal system (space group Pbca) with cell parameters a = 14.6986 (11) Å, b = 6.1323 (4) Å, c = 26.2730 (18) Å, V = 2368.2 (3) Å3 and Z = 8. In the crystal structure, intermolecular interaction of the type C---H...π stabilizes the crystal packing. This polymorph is the fourth candidate of its kind and second candidate in the orthorhombic crystal system. The structural comparisons and crystal packing of tetramorphs (A, B, C and D) are analyzed using molecular structures, Hirshfeld surfaces, enrichment ratios (E) and energy frameworks. The conformational differences are observed in all the tetramorphs and the intercontacts H⋯H and C⋯H contributes around 85 % to the Hirshfeld surfaces. The E ratio provides evidence of H⋯H, C⋯H and O⋯H intercontacts having high propensity to form contacts in the crystal packing. The average energy (dimer formation) for each polymorph is calculated from energy framework analysis. The systematic comparison of crystal packing in tetramorphs through 3D-topology is visualized. In the energy-frameworks of the crystal packing, dispersion energy dominates over the electrostatic energy. Overall, the molecular packings of the four polymorphic structures are different.

Hydrothermal crystal growth of 2-D and 3-D barium rare earth germanates: BaREGeO4(OH) and BaRE10(GeO4)4O8 (RE = Ho, Er)

Two new structural types of BaREGeO4(OH) and BaRE10(GeO4)4O8 (RE = Ho3+,Er3+) single crystals were synthesized via high-temperature and high-pressure hydrothermal synthesis. The BaREGeO4(OH) compounds were found to crystallize in the orthorhombic space group Pbca. BaHoGeO4(OH) is used as a representative of the family with cell parameters of a = 5.7175(2) Å, b = 10.1556(5) Å, c = 10.6189(9) Å and V = 964.97(8) Å3. The BaREGeO4(OH) structure contains a one-dimensional chain of rare-earth polyhedra linked through edge sharing of oxygen atoms. High density BaRE10(GeO4)4O8 crystals crystallize in the monoclinic space group C2/m and feature a sheet like arrangement of rare-earth oxide polyhedra with Keggin-like features. BaHo10(GeO4)4O8 is used as a representative of this structure type with cell parameters of a = 12.4533(8) Å, b = 7.2008(5) Å, c = 12.0034(8) Å, β = 100.183(2)⁰ and V = 1059.43(12) Å3. Barium polyhedra and isolated GeO4 units aid in connecting the rare earth oxide framework to extend it in three-dimensional (3-D) space. Characterization by single crystal X-ray diffraction and Raman and photoluminescence spectroscopies is reported.

Energetic propane-1,3-diaminium and butane-1,4-diaminium salts of N,N'-dinitroethylenediazanide: syntheses, crystal structures and thermal properties.

The acidity of the amine H atoms and the consequent salt formation ability of ethylenedinitramine (EDNA) were analyzed in an attempt to improve the thermal stability of EDNA. Two short-chain alkanediamine bases, namely propane-1,3-diamine and butane-1,4-diamine, were chosen for this purpose. The resulting salts, namely propane-1,3-diaminium N,N'-dinitroethylenediazanide, C3H12N22+·C2H4N4O42-, and butane-1,4-diaminium N,N'-dinitroethylenediazanide, C4H14N22+·C2H4N4O42-, crystallize in the orthorhombic space group Pbca and the monoclinic space group P21/n, respectively. The resulting salts display extensive hydrogen-bonding networks because of the presence of ammonium and diazenide ions in the crystal lattice. This results in an enhanced thermal stability and raises the thermal decomposition temperatures to 202 and 221 °C compared to 180 °C for EDNA. The extensive hydrogen bonding present also plays a crucial role in lowering the sensitivity to impact of these energetic salts.

Crystal chemistry and physical properties of the A2M3(H2O)2[B4P6O24(OH)2] (A = Cs, Rb; M = Ni, Cu, (Ni, Fe)) borophosphate family.

Three new transition metal borophosphates, Cs2Cu3(H2O)2[B4P6O24(OH)2] (denoted (I)), Cs2Ni3(H2O)2[B4P6O24(OH)2] (II) and mixed Rb2Ni2.5Fe0.5(H2O)2[B4P6O24(OH)2] (III), were synthesized by a boric acid flux method at 473-493 K. X-ray single-crystal diffraction study confirms their isotipy with (Cs/Rb)2Co3(H2O)2[B4P6O24(OH)2] borophosphates crystallizing in the orthorhombic space group Pbca. The crystal structures of all compounds are based on 3D frameworks made from corrugating borophosphate layers [B4P6O24(OH)2] and trimers of MO4(H2O)2 and two MO6 edge-sharing octahedra. The negative charge of the framework is compensated by alkali metal cations, Rb+ or Cs+. Structural analysis reveals the flexibility of mixed anionic frameworks of the described structural type. The Cu-member demonstrates a strong distortion of the unit cell due to the Jahn-Teller effect of the d9 configuration of the Cu2+ cation. The possibility of a solid solution between different transition metals (Fe and Ni) with the formation of crystals with mixed structural positions is confirmed by an example of the (III) phase. It is shown that Fe2+ cations prefer to occupy the M2 position with more distorted oxygen environment, as compared to the M1O6 octahedra. Magnetic studies of (I), (II) and (III) prove that all compounds are paramagnets down to the lowest temperatures of measurements, 2 K. (I) and (II) compounds are thermally stable up to 500 °C. Different mechanisms of their thermal decomposition are discussed. The possibility of a wide isomorphous substitution at the transition metal sites of the title structure type opens the way to the modification of the properties in the discussed series of borophosphates.

Synthesis and spectroscopic study of transition metal complexes of tridentate ligand formed by direct condensation of o-vanillin and 2-aminophenol: X-ray structural characterization of the zinc(II) complex

The reactions of the Schiff base 2-((2-hydroxyphenylimino)methyl)-6-methoxyphenol (H2L), obtained by direct condensation of 2-aminophenol and 2-hydroxy-3-methoxybenzaldehyde, with some transition metal ions (Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)) afforded complexes of general formulae [M2(L)2(solvent)x] (M: Mn, Co, Ni, Cu or Zn; Solvent: DMSO or H2O). These compounds were characterized by elemental analysis, UV-Vis, IR, 1H- and 13C-NMR spectroscopies, molar conductivity and room temperature magnetic measurements. The structure of zinc(II) complex has been determined by X-ray crystallography. Crystal data for C32H34N2O8S2Zn2 (M =769.47 g/mol): Orthorhombic, space group Pbca (no. 61), a = 16.3176(7) Å, b = 9.1247(3) Å, c = 21.8274(10) Å, V = 3250.0(2) Å3, Z = 4, T = 173(2) K, μ(MoKα) = 1.658 mm-1, Dcalc = 1.573 g/cm3, 28116 reflections measured (4.5° ≤ 2Θ ≤ 60.3°), 4457 unique (Rint = 0.0409, Rsigma = 0.0371) which were used in all calculations. The final R1 was 0.0307(0.0466) and wR2 was 0.0649 (0.0701) (all data). The coordination sphere of the Zn center is best described as a trigonal bipyramid.