Synthesis and Characterization of Diorganotin(IV) Complexes Bearing Binary Schiff‐Bases and Crystal Structure of nBu2SnL1

Four novel diorganotin(IV) complexes with general formula R₂SnL (R = nBu, PhCH₂) were synthesized from diorganotin dichlorides and binary Schiff‐bases (H₂L) containing N₂O₂ donor atoms in the presence of sodium ethoxide. The Schiff bases were prepared by reactions of o‐phenylenediamine with 3‐tert‐butyl‐2‐hydroxy‐5‐methylbenzaldehyde (H₂L¹) and salicylaldehyde (H₂L²) respectively. The compounds were characterized by elemental analyses, IR, and NMR spectroscopy. The solid‐state crystal structure of the compound nBu₂SnL¹ was determined by single‐crystal structural analysis.     

A New Chair‐shaped Conformation Containing HgHgOHgHgO: Synthesis and Structure of Hg4(L2)2(NO3)4 (L2 = morpholin‐4‐ylpyridin‐2‐ylmethyleneamine)

. The complex Hg₄(L²)₂(NO₃)₄ ( 1 ) (L² = morpholin‐4‐ylpyridin‐2‐ylmethyleneamine) has been synthesized and characterized by CHN analysis, IR, and UV/Vis spectroscopy. The crystal structure of 1 was determined using single‐crystal X‐ray diffraction. The crystal structure of 1 contains four mercury atoms, four nitrate anions (two terminal and two bridge ones) and two L² ligand molecules. A chair shape, six‐membered ring is formed with the sequence OHgHgOHgHg built from Hg–Hg dumbbells and oxygen atoms from the nitrate co‐ligands. In the crystal structure, the asymmetric unit of the compound is built up by one‐half of the molecule. It contains the Hg₂²⁺ moiety with a mercury–mercury bonded core, in which one diimine ligand is coordinated to one of the mercury atoms. The nitrate anions act as anisobidentate and bidentate ligands.     

Synthesis, Structure and Biological Activities of S-[α-（ 4-Methoxyphenylcarbonyl ）-2-（1,2,4-triazole-l-yl） ethyl-N, N-dime-thyldithiocarbamate

The title compound was prepared by reaction of N, N‐dimethyldithiocarbamate sodium with l‐bromo‐l‐(4‐methoxyphenylcarbonyl)‐2‐(1, 2, 4‐triazole‐l‐yl) ethane. Its crystal structure has been determined by X‐ray diffraction analysis. The crystal belongs to triclinic with space group Pī, a = 0.7339(2) nm, b = 1.1032(2) nm, c = 1.1203(2) nm, a = 90.27(3)°, β = 102.03(3)°, γ = 104.91(3)°, Z=2, V = 0.8556(3) nm³, D_c = 1.360 g/cm³, μ =0.325 mm^?1, F(000)=368, final R₁ =0.0475. The planes of 4‐methoxybenzyl group and triazole ring are nearly perpendicular to each other. The dihedral angle is 83.97°. There is an obvious π‐π stacking interaction between the molecules in the crystal lattice. The results of biological test show that the title compound has fungicidal and plant growth regulating activities.     

A Supermolecule Assembled by Sodium Cation,Crown Ether and α‐Dawson Heteropolyanion

The supermolecular based on sodium molybdate(VI) and sulfate, dibenzo‐18‐crown‐6 was synthesized in acetonitrile and characterized by elemental analysis, IR, ¹H NMR, single crystal X‐ray diffraction, indicating that it contains [S₂Mo₁₈O₆₂]⁴⁺ and [Na(DB18C6)(H₂O)]⁺, where each sodium ion is deviated from the plane defined by the oxygen atoms in the corresponding crown ether. The compound crystallizes in the monoclinic space group C2/c with a=3.29332(10) nm, b=1.90917(6) nm, c=2.63132(7) nm, β=121.6630(10)°, V=14081.8(7) nm³, Z=8, T=293(2) K, and R₁ (wR₂)=0.0177 (0.1525). The compound exhibits a novel organic‐inorganic structure, in which the crown ether‐sodium complexes are coordinated to the terminal oxygen atoms of Mo₁₈O₅₄ and the oxygen atoms of water molecule.     

The rich crystal chemistry of the AMM′(PO4)2 morphotropic series: NaZnAl(PO4)2, the first Na representative with a new structure type

A novel phosphate, sodium zinc aluminium bis(phosphate), NaZnAl(PO₄)₂, was obtained under mild‐temperature hydrothermal conditions at 553 K. The crystal structure has been studied using single‐crystal X‐ray experimental data. The pseudo‐hexagonal phase NaZnAl(PO₄)₂ crystallizes in the monoclinic space group P2₁/c. Its unique crystal structure is based on a three‐dimensional (3D) framework built by Zn‐, Al‐ and P‐centred tetrahedra sharing vertices. Channels parallel to the [101] and [01] directions are limited by six‐ and eight‐membered windows, and incorporate Na atoms. The new compound is discussed as a member of the morphotropic series AMM′PO₄, where A = Na, K, Rb or NH₄, M = Cu, Ni, Co, Fe, Zn or Mg and M′ = Fe, Al or Ga. The title compound is the first Na representative within the series and is characterized by a 3D architecture of tetrahedra populated in an ordered manner by Zn²⁺, Al³⁺ and P⁵⁺ ions.     

Hydrothermal Synthesis and Characterization of a One—Dimen—sional Copper（Ⅰ） Halide Cluster with 1,10—Phenanthroline

The title compound Cu₂Cl₂phen (phen = 1,10‐phenanthroline, C₁₂H₈N₂) 1 was synthesized from CuCl₂·2H₂O, CuCl and phen by hydrothermal method and its structure was determined by single crystal X‐ray analysis. With phen, CuG forms one‐dimensional chains, which comprise two zigzag chains based on fused Cu‐X units and connected via covalent bonds. The compound contains two crystallographically unique monovalent copper ions, Cu(1) and Cu(2). The Cu(1) atom in the tetrahedral site, is coordinated to two bridging Cl^? and two N atoms in phen. The Cu(2) atom with a slightly distorted triangular planar geometry, is coordinated to three Cl^?. The compound 1 was crystallized in monoclinic, space group P2₁/n with a = 0.37338(4), b = 1.9510(2), c = 1.68008(19) nm, β = 95.605 (3)°, R = 0.0458, and was characterized by elemental analysis, IR spectrum and TGA analysis.     

Synthesis,Characterization, and Energetic Properties of Nitroso Compounds

Sodium and potassium methyl(nitroso)amide (M[CH₃N₂O], M = Na ( 1 ), K ( 2 )) were prepared by the reaction of monomethylhydrazine with iso‐pentyl nitrite or n‐butyl nitrite and a suitable metal ethoxide (M[CH₃CH₂O], M = Na, K) in an ethanol‐ether mixture. The reaction of monomethylhydrazine with a small excess of iso‐pentyl nitrite or n‐butyl nitrite and in the absence of a metal ethoxide led to the formation of N‐nitroso‐N‐methylhydrazine (CH₃(NO)N–NH₂, ( 3 )). Alternatively, compound 3 was prepared by the amination reaction of 1 or 2 using the sodium salt of HOSA in ethanol solution. Compounds 1–3 were characterized using elemental analysis, differential scanning calorimetry, mass spectrometry, vibrational (infrared and Raman) and UV spectroscopy and multinuclear (¹H, ¹³C and ¹⁵N) NMR spectroscopy. For compounds 1–3 , several physical and chemical properties of interest and sensitivity data were measured and for compound 3 thermodynamic and explosive properties are also given. Additionally, the solid‐state structure of compound 3 was determined by single‐crystal X‐ray analysis and the structures of the cis‐ and trans‐[CH₃N₂O]^– anions and that of 3 were optimized using DFT calculations and used to calculate the NBO charges.     

Crystal Structure and Theoretical Calculation of 1,4-Bis-(1-ferrocenesulfonyl-2-benzimidazolyl) Butane

A N,N′‐bisferrocenesulfonyl bisbenzimidazole compound 1,4‐bis(1‐ferrocenesulfonyl‐2‐benzimidazolyl) butane was prepared. Its crystal structure was determined. The crystal belongs to triclinic with space group P‐1 and a=0.87241(13) nm, b=0.97553(15) nm, c=1.4120(2) nm, and α=83.041(2) °, β=72.454(2)°, γ=69.732(2)°, the unit cell volume V=1.0746(3) nm³, the molecule number in one unit cell Z=1, the absorption coefficient μ=1.191 mm^?1, the calculated density D_c=1.584 g/cm³. The theoretical investigation of the compound as a structure unit was fully optimized by B3LYP/6‐31G method in Gaussian 03 package, and the most stable structure of the compound in theory was obtained. The two results were compared. The optimized structure was in accordance with the crystal structure in the main, suggesting that the molecular geometry optimization of the structures was reliable and the calculation method used was reliable. The distribution of atomic charges and the energy, and composition of frontier molecular orbits were analyzed. Thermal analysis indicated that it is stable before melting.     

Synthesis and Characterization of a New Thallium(I) Coordination Polymer of Tetrazolate Ligand as Precursor for Preparation of Thallium(III) Oxide Nanoparticles

A new thallium(I) coordination polymer, [Tl₂L · H₂O]_n ( 1 ) [H₂L = 5‐(4‐hydroxyphenyl)tetrazole], was synthesized and characterized by IR spectroscopy, elemental analysis, and X‐ray crystallography. The single‐crystal X‐ray diffraction data of compound 1 show the existence of two different Tl^I ions with differing coordination numbers. The coordination number of Tl^I(1) is four and that of Tl^I(2) is two. This coordination polymer was used as a precursor for the preparation of Tl^III oxide nanoparticles. Thallium(III) oxide was characterized by powder X‐ray diffraction and the morphology of nanoparticles characterized by scanning electron microscope (SEM).     

3,5-二羟基-2,4,6-三硝基苯酚氨基脲铵盐半水合物的合成、晶体结构和热分解特性

A new compound, semicarbazidium 3,5-dihydroxy-2,4,6-trinitrophenolate hemihydrate （SCDHTNP·0.5H2P）, was synthesized by the reaction of the aqueous solutions of semicarbazide with trinitrophloroglucinol. Its structure was determined by single-crystal X-ray diffraction analysis and characterized by elemental analysis, FTIR, DSC and TG-DTG techniques. The crystal is monoclinic with space group P21/n and the empirical formula C7H9N6O10.50. The unit cell parameters are： a= 1.3791（3） nm, b=0.9256（2） nm, c=2.0468（4） nm,β= 106.93（3）°, V=2.4995（9）nm^3, Z=8, Dc= 1.835 g/cm^3, Mr=345.20, F（000）= 1416, s=0.945,μ（Mo Ka）=0.174 mm^-1. The final R and wR are 0.0401 and 0.0896. Its structure consists of two semicarbazidium cations, two 3,5-dihydroxy-2,4,6-trinitrophenolate anions and one crystal water molecule, which are interconnected by electrostatic forces and hydrogen bonds into layer structure, making the title compound very stable. Under a linear heating rate, the thermal decomposition processes of SCDHTNP·0.5H2O have one endothermal dehydration stage and two intensive exothermic decomposition stages at 178-241℃ to evolve abundant gas products.     

Synthese und Charakterisierung von Natriumcyanamid

Synthesis and Characterization of Sodium Cyanamide The synthesis of Na₂CN₂ was carried out by reaction of sodium amide with sodium hydrogen cyanamide at 200 °C, in vacuum. Single crystals were obtained while heating the product (500 °C, 8 days) in silver crucibles. The title compound was characterised by single crystal X‐ray diffraction and IR‐spectroscopy (C2/m; Z = 2, a = 5.0456(3), b = 5.0010(3), c = 5.5359(3) Å; β = 110.078(5)°; R1 = 3.18%, wR2 = 6.35%, GOF = 1.078). The CN₂^2– units are linear exhibiting a C–N bond length of 1.236(1) Å, while sodium is coordinated by five nitrogen atoms forming a square pyramid. The structural relationships to aristotypic Na₂HgO₂ are pointed out.     

Aren‐Stapelung in den Kanälen eines dreidimensionalen Koordinationspolymers: Kristallstruktur des Natriumkomplexes [Na{C6H4(SO2)2N}(H2O)] und supramolekulare Verwandtschaft mit dem analogen Silberkomplex

Metal Salts of Benzene‐1,2‐di(sulfonyl)amine. 5. Arene Stacking in the Channels of a Three‐Dimensional Coordination Polymer: Crystal Structure of the Sodium Complex [Na{C₆H₄(SO₂)₂N}(H₂O)] and its Supramolecular Relationship to the Analogous Silver Complex The sodium compound NaZ · H₂O, derived from HZ = ortho‐benzenedisulfonimide, has been characterized by single crystal X‐ray diffraction at –100 °C (orthorhombic, space group Pna2₁, Z = 4). The five‐membered 1,3,2‐dithiazolide heterocycle possesses an envelope conformation, the N atom lying 30.3(1) pm outside the mean plane of the S–C–C–S moiety. The sodium ion attains a severely distorted octahedral coordination via Na⁺…O^δ– interactions with four anions and one water molecule. In contrast to the previously reported lamellar layer structures of CsZ, RbZ · H₂O and KZ · H₂O, the present crystal displays a three‐dimensional coordination assembly consisting of sodium ions, (SO₂)₂N groups and water molecules. This polar framework is pervaded by parallel channels approximately 800 × 800 pm² in profile, into which the lipophilic benzo rings are stacked at intercentroid distances of 402 pm. Re‐examination of AgZ · H₂O (Z. Anorg. Allg. Chem. 1993 , 619, 1441) discloses a striking supramolecular relationship to the sodium congener. In the crystal packing of the silver complex, one‐dimensional strands comprising pentacoordinate cations are associated by O–H…O(S) hydrogen bonds into a three‐dimensional polar framework, which again accommodates stacks of benzo groups within parallel channels.     

Synthesis, Structure and Biological Activities of Novel Triazole Compounds Containing N,N-Dialkyldithiocarbamate Moiety

Introduction As an important type of fungicides, triazole compounds are highly efficient, low poisonous and inward absorbent.1-3 At present, the studies on triazole derivatives are mainly concentrated on compounds with triazole as the only active group. The report of triazole compounds that contain both triazole group and other active group in a single molecule has rarely been found. Dialkyl-substituted dithiocarbamate salts have also shown interesting biological effects.4 N,N-Dialkyldithio-…     

The 1:1 cocrystals of the proton‐transfer compound dilituric acid–phenyl­biguanide monohydrate

A proton‐transfer compound, 1‐phenyl­biguanidium 5‐nitro‐2,6‐dioxo‐1,2,3,6‐tetra­hydro­pyrimidin‐4‐olate monohydrate, C₈H₁₂N₅⁺·C₄H₂N₃O₅⁻·H₂O, has been synthesized by a reaction between dilituric acid (5‐nitro‐2,4,6‐trihydroxy­pyrimi­dine, Dilit) and phenyl­biguanide (N‐phenyl­imido­carbonimidic diamide, Big). This compound cocrystallized as a 1:1 adduct, and the asymmetric unit consists of two dilituric amino–oxo planar tautomeric anions (Dilit⁻), two monoprotonated phenyl­biguanidium cations (BigH⁺) and two water mol­ecules of crystallization (Z′ = 2). Protonation occurs at the N atom attached to the phenyl ring of Big as a result of the proton‐transfer process from the acidic hydr­oxy group of Dilit. In the crystal structure, the hydrated 1:1 adduct is stabilized by 25 two‐ and three‐center hydrogen bonds.     

Synthesis and Characterization of Acetone Hydrazones

1‐Isopropylidene‐2‐methylhydrazine ( 1 ), 1‐isopropylidene‐2‐hydroxyethylhydrazine ( 2 ) and 1‐isopropylidene‐2‐formylhydrazine ( 3 ) were synthesized by reaction of the corresponding hydrazine with an excess of acetone in the presence of a drying agent (anhydrous sodium sulfate or barium oxide). All compounds 1 – 3 were characterized by elemental analysis, coupled gas chromatography‐mass spectrometry (GC–MS), multinuclear NMR spectroscopy (¹H, ¹³C and ¹⁵N) and vibrational spectroscopy (infrared and Raman). Compounds 1 and 2 are liquid at room conditions and their density was measured by means of a picnometer, however, (at room conditions) compound 3 is a solid and its crystal density and structure were determined by low temperature X‐ray diffraction techniques (monoclinic, P2₁/n, Z = 4, a = 5.666(1) Å, b = 6.254(1) Å, c = 15.277(4) Å, β = 91.30(2)°, V = 541.2(2) ų). The structure of hydrazone 3 is discussed in detail and compared to that of monoformylhydrazine. Finally, the (gas phase) structure of compound 3 was optimized using DFT calculations (B3LYP/6‐31+G(d, p)) and its NBO charges are reported.     

The Crystal Structure of Disodium Phosphonate,Na2HPO3

Anhydrous disodium phosphonate, Na₂HPO₃, was prepared by dehydration of its pentahydrate. The crystal structure of Na₂HPO₃ was solved from high resolution X‐ray powder diffraction data (P2₁/n; Z = 4; a = 9.6987(1), b = 6.9795(1), c = 5.0561(1) Å, β = 92.37(1)°; V = 341.97(1) ų). The crystal structure consists of two types of sodium‐oxygen polyhedra, which are connected via common edges and vertices forming layers perpendicular to [100]. These Na(1)‐ and Na(2)‐layers are interlinked via common edges, forming in a 3D‐framework. The resulting topology is providing oxygen arrangements that please the coordinative requirement of phosphorus(III).     

Experimental and Theoretical Studies of 4‐(1‐benzyl‐5‐methyl‐1H‐1,2,3‐triazol‐4‐yl)‐6‐(2,4‐dichlorophenyl)pyrimidin‐2‐amine: A Potential Antibacterial Agent

The title compound ( 1 ), 4‐(1‐benzyl‐5‐methyl‐1H‐1,2,3‐triazol‐4‐yl)‐6‐(2,4‐dichlorophenyl)pyrimidin‐2‐amine (C₂₀H₁₆Cl₂N₆), was synthesized and structurally characterized by elemental analysis, ¹H NMR and ¹³C NMR and single crystal X‐ray diffraction. The compound crystallizes as a colourless needle shaped in the triclinic system, space group P‐1 with cell constants: a = 10.7557(11) Å, b = 12.7078(17) Å, c = 15.511(2) Å, α = 68.029(4)0, β = 86.637(5)0, γ = 87.869(4)0; V = 1962.4 (4) ų, Z = 4. There are two structurally similar but crystallographically independent molecules (A and B) in the asymmetric unit of the title compound, which is linked via N‐H…Cl hydrogen bond. An intramolecular C‐H…N hydrogen also occurs in each molecule. In the crystal, each of independent molecules forms a centrosymmetric dimer with an R²₂(8) ring motifs through a pair of N‐H…N hydrogen bonds. These dimers are further connected by intermolecular N‐H…Cl and C‐H…Cl hydrogen bonds, forming an infinite two dimensional supramolecular network lying parallel to the [010] plane. The molecular geometry was also optimized using density functional theory (DFT/B3LYP) method with the 6‐311G (d, p) basis set and compared with the experimental data. Mulliken population analyses on atomic charges, HOMO‐LUMO energy levels, Molecular electrostatic potential and chemical reactivity of the title compound were investigated by theoretical calculations. The thermo dynamical properties of the title compound at different temperature have been calculated and corresponding relations between the properties and temperature have also been obtained. The in vitro antibacterial activity has been screened against Gram‐positive (Bacillus cerus and Staphylococcus epidermidis) and Gram‐Negative (Escherichia coli, Acinetobacter baumannii and Proteus vulgaris). The results revealed that the compound exhibited good to moderate antibacterial activity.     

Synthesis and Properties of Triphenylgermanium Heteroaromatic Carboxylates and Crystal Structure of Triphenylgermanium 2‐Furoate

Ten triphenylgermanium heteroaromatic carboxylates Ph₃GeO₂CR (where R=2‐furanyl, 2‐furanvinyl, 2‐(5‐tertbutyl) furanyl, 2‐thiophenyl, 2‐pyridinyl, 3‐pyridinyl, 4‐pyridinyl, 3‐indolyl, 3‐indolylmethyl, 3‐indolylpropyl) were synthesized by the reaction of sodium heteroaromatic carboxylates with the triphenylgermanium chloride. All compounds were characterized by elemental analysis, ¹H NMR and MS spectra. The compounds were tested against two human tumour cell lines: MCF‐7 and WiDr. The results showed that they had high activities. The crystal structure of triphenylgermanium 2‐furoate was determined by X‐ray single crystal diffraction. The crystal belongs to monoclinic with space group P2₁/c, a = 1.1545(4), b=0.9934(3), c = 1.6284(5) nm, β= 91.59(5), Z = 4. In this crystal, the structure consists of discrete molecule containing four‐coordinate germanium atom in a distored tetrahedron.     

Synthesis,Structure, and Properties of a New Calcium(II) Complex of 1,10‐Phenanthroline, 1,2,4,5‐Benzenetetracarboxylic Acid,and a New Precursor to Produce Pure Phase Micro‐crystalline Calcite Particles

The self‐assembly of 1, 0‐phenanthroline (phen) and 1,2,4,5‐benzenetetracarboxylic acid(H₄btc) with Ca(NO₃)₂ gives rise to a two‐dimensional network structure coordination polymer, [Ca(phen)(btc)_0.5(H₂O)] ( 1 ), which was characterized by elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction. This compound is monoclinic, space group C2/c, with Z = 8 in a unit cell with dimensions a = 21.744(3) Å, b = 10.0151(12) Å, c = 14.7122(17) Å, β = 110.2850(10)°. The structure contains one crystallographic unique Ca^II atom, one phen coordinated molecule and a half of btc^4– anion. The phen molecule acts as a didentate ligand chelating with a Ca^II atom, whereas the btc^4– anion acts as a μ₆‐bridge linking six different Ca^II atoms to form a two‐dimensional network with (4, 4) topological structure. The three dimensional stacking structures are formed by C–H ··· O hydrogen bonding and π–π interaction. The thermal stability and fluorescent properties of 1 were investigated. Calcite particles are produced by calcination of compound 1 at 580 °C. The obtained calcite was characterized by XRD and SEM analyses.     

Conformation and tautomerism of methoxy‐substituted 4‐phenyl‐4‐thiazoline‐2‐thiones: a combined crystallographic and ab initio investigation

4‐Phenyl‐4‐thiazoline‐2‐thiol is an active pharmaceutical compound, one of whose activities is as a human indolenamine dioxygenase inhibitor. It has been shown recently that in both the solid state and the gas phase, the thiazolinethione tautomer should be preferred. As part of both research on this lead compound and a medicinal chemistry program, a series of substituted arylthiazolinethiones have been synthesized. The molecular conformations and tautomerism of 4‐(2‐methoxyphenyl)‐4‐thiazoline‐2‐thione and 4‐(4‐methoxyphenyl)‐4‐thiazoline‐2‐thione, both C₁₀H₉NOS₂, are reported and compared with the geometry deduced from ab initio calculations [PBE/6‐311G(d,p)]. Both the crystal structure analyses and the calculations establish the thione tautomer for the two substituted arylthiazolinethiones. In the crystal structure of the 2‐methoxyphenyl regioisomer, the thiazolinethione unit was disordered over two conformations. Both isomers exhibit similar hydrogen‐bond patterns [R₂²(8) motif] and form dimers. The crystal packing is further reinforced by short S…S interactions in the 2‐methoxyphenyl isomer. The conformations of the two regioisomers correspond to stable geometries calculated from an ab initio energy‐relaxed scan.