Intramolecular Mobility in the Complexes 2SbCl3· p-C6H4(CH3)2and SbCl3· C6H5COCH3according to 35Cl NQR Data

Temperature dependences of the ³⁵Cl and ¹²¹Sb spin-lattice relaxation time ₁in antimony trichloride complexes with p-xylene and acetophenone were studied using NQR spectroscopy. The activation energies of the retarded motion (similar to that discovered in some v complexes of SbCl₃) of chlorine atoms were determined from the ³⁵Cl ₁(T) function. New data on the shape of the ¹²¹Sb ₁(T) function are discussed.     

Synthesis and structure of nalidixium tetrachloroantimonate monohydrate, (C12H13N2O3)SbCl4 · H2O

Nalidixium tetrachloroantimonate monohydrate, (C₁₂H₁₃N₂O₃)SbCl₄ · H₂O, has been synthesized and its crystal structure has been determined. The structure is built of the [Sb₂Cl₈]^2? anions, C₁₂H₁₃N₂O ₃ ⁺ nalidixium cations, and H₂O molecules joint by hydrogen bonds and π-π-and Cl?Cl interactions. The [Sb₂Cl₈]^2? anion is a dimer of the SbCl₅ E distorted octahedra sharing common Cl?Cl edge (E is the lone electron pair). The Sb polyhedra contain two short Sb-Cl bonds (2.387 and 2.395 Å), one bond of a medium length (2.508 Å), and two long bridging bonds (2.745 and 3.054 Å).     

Crystal structure,DSC and Raman studies in CH3C6H4NH(CH3)2·SbCl4

The salt para methyl phenyl dimethyl ammonium tetrachloroantimonate (III) crystallizes in the monoclinic system with space group Cc. The unit cell dimensions are: a=13.780(1) Å, b=14.943(2) Å, c=8.192(1) Å, β=113.39(1)°, with Z=4. The structure consists of ammonium cations and polynuclear anions in which distorted SbCl₅ square pyramids sharing a common Cl atom are held together in infinite chains parallel to the c axis. These chains are themselves interconnected by means of the NH⋯Cl hydrogen bonds. Differential scanning calorimetry study was carried out. The Raman of polycrystalline samples have been recorded at different temperatures between 77 and 300 K. A low-temperature phase transition at 230 K of order-disorder type was found.     

Synthesis,crystal structure,and catalytic performance of two 3-D supramolecular compounds: (C7N2H7)3(C7N2H6) · PMo12O40 · 2H2O and (C7N2H7)3(C7N2H6)2 · AsMo12O40 · 3H2O

Two organic–inorganic compounds based on Keggin building blocks have been synthesized by hydrothermal methods, (C₇N₂H₇)₃(C₇N₂H₆)?·?PMo₁₂O_40?·?2H₂O (1) and (C₇N₂H₇)₃(C₇N₂H₆)_2?·?AsMo₁₂O_40?·?3H₂O (2) (C₇N₂H₆?=?benzimidazole). Single-crystal X-ray analysis revealed that 1 crystallized in the triclinic system, P-1 space group with a?=?9.8980(4)?Å, b?=?11.2893(4)?Å, c?=?25.8933(9)?Å, α?=?93.307(2)°, β?=?90.630(2)°, γ?=?108.330(2)°, V?=?2740.68(18)?ų, Z?=?2, R ₁(F)?=?0.0740, ωR ₂(F ²)?=?0.1511, and S?=?1.037; 2 crystallized in the triclinic system, P-1 space group with a?=?12.3353(4)?Å, b?=?13.2649(4)?Å, c?=?20.2878(6)?Å, α?=?95.6630(10)°, β?=?100.1720(10)°, γ?=?99.3940(10)°, V?=?3195.72(17)?ų, Z?=?2, R ₁(F)?= 0.0329, ωR₂ (F ²)?=?0.1236, and S?=?1.088. The two compounds show a layer framework constructed from Keggin-polyoxoanion clusters and benzimidazole via hydrogen bonds and π–π stacking interactions, resulting in a 3-D supramolecular network. Both have high catalytic activity for oxidation of methanol. When the initial concentration of the methanol is 5.37?g?m^?3 in air and the flow velocity is 4.51?mL?min^?1, methanol is completely eliminated at 150°C for 1 (160°C for 2).     

The Synthesis of the Arene Clusters Ru6C(CO)14(η6-Arene) (Arene = C6H5CHMe2, C6H5C4H9, C6H5C3H7, and C6H5C3H5)

On reaction with Ru₃(CO)₁₂, isopropenylbenzene and 4-phenyl-l-butene undergo hydrogenation, to yield the clusters, Ru₆C(CO)₁₄(⁶-C₆H₅CHMe₂) 1 and Ru₆C(CO)₁₄(⁶-C₆H₅C₄H₉) 2, respectively. With allylbenzene, both hydrogenation and isomerization occurs affording Ru₆C(CO)₁₄(⁶-C₆H₅C₃H₇) 3 and Ru₆C(CO)14(⁶-C₆H₅C₃H₅) 4. The structures of 1 and 2 have been established by single crystal X-ray diffraction. One of the Ru–Ru bond lengths in 2 is unusually long and extended Hückel molecular orbital calculations have been used in an attempt to rationalize this feature.     

Rb[C6H3(COOH)2(COO–)] · [C6H3(COOH)3] · 2H2O: Synthesis,Crystal Structure,and Properties

The salt Rb[C₆H₃(COO)₂(^–)] · [C₆H₃(COOH)₃] · 2H₂O (I) of trimesic acid was synthesized and its thermal stability and conductivity (10^–11 ohm^–1 cm^–1 at 298 K) were measured. Molecular and crystal structures of I were established by X-ray diffraction analysis. Hydrogen bonding system in complex I was detected by IR and Raman spectroscopies. X-ray diffraction data agree with vibration spectroscopy data.     

Thermochemical study of [Sm(C7H5O3)2·(C4H6NO2S)]·2H2O

The product from reaction of samarium chloride hexahydrate with salicylic acid and Thioproline, [Sm(C₇H₅O₃)₂·(C₄H₆NO₂S)]·2H₂O, was synthesized and characterized by IR, elemental analysis, molar conductance, and thermogravimetric analysis. The standard molar enthalpies of solution of [SmCl₃·6H₂O(s)], [2C₇H₆O₃(s)], [C₄H₇NO₂S(s)] and [Sm(C₇H₅O₃)₂·(C₄H₇NO₂S)·H₂O(s)] in a mixed solvent of absolute ethyl alcohol, dimethyl sulfoxide(DMSO) and 3 mol L^?1 HCl were determined by calorimetry to be Δ_s H _m ^Φ [SmCl₃ δ6H₂O (s), 298.15 K]= ?46.68±0.15 kJ mol^?1 Δ_s H _m ^Φ [2C₇H₆O₃ (s), 298.15 K]= 25.19±0.02 kJ mol^?1, Δ_s H _m ^Φ [C₄H₇NO₂S (s), 298.15 K]=16.20±0.17 kJ mol^?1 and Δ_s H _m ^Φ [Sm(C₇H₅O₃)₂·(C₄H₆NO₂S)]·2H₂O (s), 298.15 K]= ?81.24±0.67 kJ mol^?1. The enthalpy change of the reaction (1) $$ SmCl_3 \cdot 6H_2 O(s) + 2C_7 H_6 O_3 (s) + C_4 H_7 NO_2 S(s) = Sm(C_7 H_5 O_3 )_2 \cdot (C_4 H_6 NO_2 S) \cdot 2H_2 O(s) + 3HCl(g) + 4H_2 O(1) $$ was determined to be Δ_s H _m ^Φ =123.45±0.71 kJ mol^?1. From date in the literature, through Hess’ law, the standard molar enthalpy of formation of Sm(C₇H₅O₃)₂(C₄H₆NO₂S)δ2H₂O(s) was estimated to be Δ_s H _m ^Φ [Sm(C₇H₅O₃)₂·(C₄H₆NO₂S)]·2H₂O(s), 298.15 K]= ?2912.03±3.10 kJ mol^?1.     

Structure of (C3H5NH3)2H2P2O7·H2O

The bis(cyclopropylammonium)dihydrogenodiphosphate monohydrate is a new diphosphate associated with the organic molecule C₃H₅NH₂. We report the chemical preparation and the crystal structure of this organic cation diphosphate. (C₃H₅NH₃)₂H₂P₂O₇.H₂O is orthorhombic (S.G. : P2₁2₁2₁), with Z = 4 and the following unit-cell parameters : a = 4.828(1) Å, b = 11.011(1) Å, c = 25.645(2) Å. The P₂O₇ groups and H₂O water molecules form a succession of bidimensional layers perpendicular to the c axis. The organic cations ensure the three-dimensional cohesion by NH-O hydrogen bonds.     

Crystal structure and properties of H3[PMo12O40] · 3C2H6O

The title compound H₃[PMo₁₂O₄₀]· 3C₂H₆O was prepared and characterized by X-ray crystallography, its i.r. spectrum, cyclic voltammetry and e.s.r. spectra. The anion of the title compound is a Keggin-type heteropoly structure based upon a central PO₄ tetrahedron surrounded by 12 MoO₆ octahedra arranged in four groups of three edge-shared octahedra Mo₃O₁₃. Weak hydrogen bonds exist between the organic solvent molecules and the heteropoly anion. The catalytic activity of the title compound was determined by the synthesis of butyl acetate. The conversion of n-BuOH reached 93.3% and the yield of MeCO₂Bu-n was 92.0% when the ratio of MeCO₂H to n-BuOH, catalyst amount, reaction time, reaction temperature were 2:1, 0.24% of the reactants (50 mg), 2.0 h and 115 120 °C, respectively.     

Synthesis,Crystal structure and Luminescent Property of a New 3D Supramolecular Compound （C6H6NO2）3（C6H5NO2）（PW12O40）·2H2O

A supramolecular compound （C6H6NO2）3（C6H5NO2）（PW12O40）·2H2O including the Keggin-type [PW1O40]3- polyanion, [HC6H5NO2]＋ （protonated pyridine-4-carboxylic acid molecule）, C6H5NO2 （pyridine-4-carboxylic acid molecule） and two free H20 molecules has been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectra, single-crystal X-ray diffraction and powder X-ray diffraction. The crystal belongs to orthorhombic, space group Pnnm with a = 1.0483（3）, b = 1.4368（6）, c = 2.0526（7） nm, V= 3.0918（18） nm3,Z = 2, F（000） = 3004, Mr= 3406.07, Dc= 1.757 g.m-3,μ = 41.241 mm-1, the final R = 0.0387 and wR = 0.1089 for 2091 observed reflections withI〉 2σ（I）. A total of 30431 reflections were collected, of which 3083 were independent （Rint = 0.0605）. S is 1.182. The title compound presents a 3-D structure via intermolecular hydrogen bonds among [PW12O40]3- polyanions and pyridine-4-carboxylic acid ligands. The ultraviolet and luminescence spectra have been studied at room temperature, of which the purple fluorescent emission is located at 363 nm when excited at 264 nm. Fluorescent emission of the compound derives from the π-π＊ transitions in the pyridine-4-carboxylic acid ligands.     

Synthesis, crystal structure, and thermal analysis of hexahydrogen dodecavanadate of composition [NH3 · H2O]6 · H6[Ca4V12O40] · 6H2O

Dihydrogen dodecavanadate of composition [NH₃ · H₂O]₆ · H₆[Ca₄V₁₂O₄₀] · 6H₂O was synthe-sized and studied by X-ray crystallography and TGA analyses. The crystals are cubic, space group I $\bar 4$ 3m;; unit cell parameters: a = 13.518(2) ?, V = 2470.4(3) ?³, ??_calc = 2.2334 g/cm³, Z = 2.     

Critical temperatures,pressures, and densities for the mixtures CO2–C3H8, CO2–nC4H10, C2H6–C3H8, and C3H8–nC4H10

A simple method is developed to estimate mixture critical temperatures (T_c), pressures (P_c), and densities (ρ_c) as a function of overall composition (X) from near critical region experimental coexistence data. This three-step method is applied to four mixtures, CO₂–C₃H₈, CO₂–nC₄H₁₀, C₂H₆–C₃H₈, and C₃H₈–nC₄H₁₀. Isothermal liquid–vapor coexistence data, which includes temperature, vapor pressure, coexisting densities (ρ^ℓ and ρ^v), and coexisting compositions for the more volatile component (x₁^v and x₁^ℓ) are used. In the first step, the difference of the saturated liquid and vapor densities (ρ^ℓ−ρ^v) is fitted to an empirical function in ((P_c−P)/P_c) to obtain P_c. Then P/P_c and ((ρ^ℓ+ρ^v)/2ρ_c) are simultaneously fitted to functions of a polynomial in (X₁−(x₁^v+x₁^ℓ)/2) yielding estimates of ρ_c and X₁. Finally, the discrete estimated critical data points are fitted with an equation to provide a continuous representation of the critical lines. The method is successfully tested for the mixtures, CO₂–C₃H₈ and CO₂–nC₄H₁₀, for which there is a reasonable amount of isothermal data. The procedure is then applied to the mixtures, C₂H₆–C₃H₈ and C₃H₈–nC₄H₁₀, for which there are sparse data. For all four mixtures, the critical temperature line, T_c vs. X₁, matches literature values within ±0.5%. The critical pressure line, P_c vs. X₁, and critical density line, ρ_c vs. X₁, match literature values, in general, within ±2%.     

[Mn3O(O2CC6H5)6(C3H4N2)3]·C6H5CO2·0.5H2O的 合成、晶体结构及磁性质

Mn(O2CMe)2·4H2O、咪唑、苯甲酸和N(n-Bu)4MnO4在无水乙醇溶剂中反应,制备得到锰的三核μ3-O桥联配位化合物[Mn3O(O2CC6H5)6(C3H4N2)3]·C6H5CO2·0.5H2O.该配位化合物的X射线单晶衍射表明,其属于单斜晶系,空间群P21/C,晶胞参数：a=1.52832(19)nm,b=1.9722(2)nm,c=2.1023(3)nm,β=92.597(3)°,Z=4.变温磁化率(5～280K)研究表明,该配位化合物中3个锰离子在低温下存在弱的反铁磁性耦合,交换积分J=-2.34cm^-1。     

Study of the solubility of components in the system Mg(ClO3)2-2NH2C2H4OH · H3C6H5O7-H2O

The solubility of components in the system Mg(ClO₃)₂-2NH₂C₂H₄OH · H₃C₆H₅O₇-H₂O was studied from the complete freezing temperature ?59.4°C to 20.0°C. A polythermal solubility diagram was constructed, in which the crystallization fields were determined for ice, Mg(ClO₃)₂ · 16H₂O, Mg(ClO₃)₂ · 12H₂O, Mg(ClO₃)₂ · 6H₂O, 2NH₂C₂H₄OH · H₃C₆H₅O₇ · H₂O, 2NH₂C₂H₄OH · H₃C₆H₅O₇, and two new compounds, [(HOC(CH₂COOH)₂COO)₂Mg · 2H₂O] and [HOC(CH₂COO)₂MgCOOH · 2H₂O], which were identified by chemical and physicochemical analysis methods.     

The mechanism and kinetics of energy transfer processes in the Xe–CCl4–M (M=CH4, C2H2, C2H4, C2H6 C3H6 and C3H8) mixtures irradiated by xenon resonance light

The mechanism and kinetics of energy transfer from Xe(6s[3/2]₁) resonance state (E=8.44 eV) to selected hydrocarbon molecules have been investigated by XeCl(B–X) (λ_max=308 nm) fluorescence intensity measurements at stationary conditions in Xe–CCl₄–M systems. Steady-state analysis of the fluorescence intensity dependence on the xenon and M pressure at constant CCl₄ concentration shows that these process occur in the two- and three-body reactions: Xe(6s[3/2]₁⁰)+M→products, Xe(6s[3/2]₁⁰+M+Xe→products. The two- and three-body rate constants for these reactions have been found (see Table 1Table 1. Experimental parameters of Eq. (8)found by least square method in Xe–CCl₄–C₂H₂ and Xe–CCl₄–C₂H₄ systems for chosen xenon pressures in the range 25–150 Torr. Linear correlation coefficients (R) are also shown     

16.

Synthesis, characterization and standard molar enthalpy of formation of Nd(C7H5O3)2·(C9H6NO)     

L. Qiang-Guo  H. Yi  L. Xu  Y. Li-Juan  X. Sheng-Xiong  Y. De-Jun  L. Yi 《Journal of Thermal Analysis and Calorimetry》2008,91(2):615-620

The complex from reaction of neodymium chloride six-hydrate with salicylic acid and 8-hydroxyquinoline, Nd(C₇H₅O₃)₂·(C₉H₆NO), was synthesized and characterized by IR, elemental analysis, molar conductance, and thermogravimatric analysis. The standard molar enthalpies of solution of [NdCl₃·6H₂O(s)], [2C₇H₆O₃(s)], [C₉H₇NO(s)] and [Nd(C₇H₅O₃)₂·(C₉H₆NO)(s)] in a mixed solvent of anhydrous ethanol, dimethyl formamide (DMF) and perchloric acid were determined by calorimetry at 298.15 K. Based on Hess’ law, a new chemical cycle was designed, and the enthalpy change of the reaction

Synthesis, characterization and standard molar enthalpy of formation of Nd(C7H5O3)2·(C9H6NO)

The complex from reaction of neodymium chloride six-hydrate with salicylic acid and 8-hydroxyquinoline, Nd(C₇H₅O₃)₂·(C₉H₆NO), was synthesized and characterized by IR, elemental analysis, molar conductance, and thermogravimatric analysis. The standard molar enthalpies of solution of [NdCl₃·6H₂O(s)], [2C₇H₆O₃(s)], [C₉H₇NO(s)] and [Nd(C₇H₅O₃)₂·(C₉H₆NO)(s)] in a mixed solvent of anhydrous ethanol, dimethyl formamide (DMF) and perchloric acid were determined by calorimetry at 298.15 K. Based on Hess’ law, a new chemical cycle was designed, and the enthalpy change of the reaction

Hydrothermal Synthesis and Crystal Structure of a New Phosphonate： {[Cu（1,10-phen）]2-（H2O3PCH2C6H4C6H4CH2PO3H）2-（HO3PCH2C6H4C6H4CH2PO3H） }n

1 INTRODUCTION Metal organophosphonates have attracted considerable attention for over three decades due to their potential or practical applications, include- ing ion exchanges[1, 2], molecular sensors[3] and optics[4, 5]. Recently, a number of porous m…     

Synthesis,spectroscopic, structural and thermal characterizations of [(C7H6NO4)2TeBr6·4H2O]

Tellurium (IV) complexes with pyridine-2,6-dicarboxylate ligand were synthesized by slow evaporation from aqueous solutions yielding a new compound: [(C₇H₆NO₄)₂TeBr₆·4H₂O]. The structure of this compound was solved and refined by single-crystal X-ray diffraction. The compound is centrosymmetric P2₁/c (N°: 14) with the parameters a = 8.875(5) Å, b = 15.174(5) Å, c = 10.199(5) Å, β = 94.271° (5) and Z = 2. The structure consists of isolated H₂O, isolated [TeBr₆]^2? octahedral anions and (pyridine-2,6-dicarboxylate) [C₇H₆NO₄]⁺ cations. The stability of the structure was ensured by ionic and hydrogen bonding contacts (N–H?Br and O–H?Br) and Van-Der Walls interaction. The thermal decomposition of the compound was studied by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The FTIR and Raman spectroscopy at different temperatures confirm the existence of vibrational modes that correspond to the organic, inorganic and water molecular groups. Additionally, the UV–Vis diffuse reflectance spectrum was recorded in order to investigate the band gap nature. The measurements show that this compound exhibits a semiconducting behavior with an optical band gap of 2.66 eV.     

Synthesis and Crystal Structure of a Hydrogen-bonded Supramolecular Compound [(C6H5N2O)3·Cu1.5]·6H2O

A hydrogen-bonded supermolecular compound [(C6H5N2O)3·Cu1.5](6H2O was syn- thesized from picolinamide and Cu(NO3)2·6H2O at the presence of sodium pyrophosphate deca- hydrate. It crystallizes in triclinic, space group P with a = 1.05947(8), b = 1.09130(8), c = 1.11456(8) nm, α = 67.8460(10), β = 84.497(1), γ = 74.6210(10)°, C18H27Cu1.5N6O9, Mr = 566.77, V = 1.15077(15) nm3, Z = 2, Dc = 1.636 g/cm3, F(000) = 585, μ = 1.461 mm-1, R1 = 0.0278 and wR2 = 0.0749. In the complex, the Cu(II) ion reveals a distorted tetradentate plane-tetragonal geometry. The structure consists of neutral two-dimensional layers via hydrogen bonds O-H…O and N-H…O between the molecules, and the layers are connected by weak interactions of the Cu-Cu, Cu-N, π-π and hydrogen bonds to form a three-dimensional network structure.     

Three organic–inorganic hybrid B-Anderson polyoxoanions as building blocks: syntheses,structures, and characterization of [(C6H5NO2)2Ln(H2O)6](CrMo6O24H6)·2C6H5NO2·6H2O (Ln = Sm,Dy, Er)

Three new B-Anderson type polyoxometalates, [(C₆H₅NO₂)₂Ln(H₂O)₆](CrMo₆O₂₄H₆)·2C₆H₅NO₂·6H₂O (Ln?=?Sm 1, Dy 2 and Er 3), have been synthesized in aqueous solution and structurally characterized by single-crystal X-ray diffraction, IR spectra, UV spectroscopy, and fluorescence spectroscopy. Crystal structure analysis reveals that these three compounds have the same composition and are isostructural, assembled by B-Anderson type polyoxoanion [CrMo₆O₂₄H₆]^3?, rare-earth ions, and ligands. UV spectroscopy shows that 1 is stable when pH is 4.50–5.83. The fluorescence spectra of 2 indicate that both rare-earth ions Dy³⁺ and pyridine-4-carboxylic acid ligands function in the charge transition of the compound.