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1.
In the system PbF 2/AsF 5/anhydrous hydrogen fluoride (aHF) two new lead(II) hexafluoroarsenates(V) Pb(HF)(AsF 6) 2 and PbFAsF 6 were isolated. Pb(HF)(AsF 6) 2 is formed when the molar ratio AsF 5:PbF 2 is 2 or higher. It crystallizes in the space group Pbcn with a=1058.3(3) pm, b=1520.9(6) pm, c=1079.4(3) pm, V=1.7374(10) nm 3 and Z=8. The HF molecule is directly connected to the Pb center, eight fluorine atoms from three different AsF 6− ions (Pb–F distances ranging from 248(4) to 276(2) pm) and one further fluorine at 306(3) pm complete the coordination sphere. PbFAsF 6 is obtained when equimolar amounts of PbF 2 and AsF 5 react in aHF. PbFAsF 6 crystallizes in the space group P
with: a=466.10(10) pm, b=723.70(10) pm, c=747.40(10) pm, =105.930(10)°, β=101.49(2)°, γ=90.660(10)°, V=0.23698(7) nm 3 and Z=2. The basic unit in the structure of PbF(AsF 6) consists of a four-membered ring of two Pb and two F atoms. The Pb atoms in the ring are further connected by two AsF 6− units via cis-fluorine bridges, thus forming a [PbF(AsF 6)] 2 cluster, which interacts by additional Pb–F bonds thus forming a ribbon-like polymer. 相似文献
2.
Nest-shaped cluster [MoOICu 3S 3(2,2′-bipy) 2] (1) was synthesized by the treatment of (NH 4) 2MoS 4, CuI, ( n-Bu) 4NI, and 2,2′-bipyridine (2,2′-bipy) through a solid-state reaction. It crystallizes in monoclinic space group P2 1/ n, a=9.591(2) Å, b=14.820(3) Å, c=17.951(4) Å, β=91.98(2)°, V=2549.9(10) Å 3, and Z=4. The nest-shaped cluster was obtained for the first time with a neutral skeleton containing 2,2′-bipy ligand. The non-linear optical (NLO) property of [MoOICu 3S 3(2,2′-bipy) 2] in DMF solution was measured by using a Z-scan technique with 15 ns and 532 nm laser pulses. The cluster has large third-order NLO absorption and the third-order NLO refraction, its 2 and n2 values were calculated as 6.2×10 −10 and −3.8×10 −17 m 2 W −1 in a 3.7×10 −4 M DMF solution. 相似文献
3.
The XeOSeF 5+ cation has been synthesized for the first time and characterized in solution by 19F, 77Se and 129Xe NMR spectroscopy and in the solid state by X-ray crystallography and Raman spectroscopy with AsF 6− as its counter anion. The X-ray crystal structures of the tellurium analogue and of the Xe(OChF 5) 2 derivatives have also been determined: [XeOChF 5][AsF 6] crystallize in tetragonal systems, P4/ n, a=6.1356(1) Å, c=13.8232(2) Å, V=520.383(14) Å 3, Z=2 and R1=0.0453 at −60°C (Te) and a=6.1195(7) Å, c=13.0315(2) Å, V=488.01(8) Å 3, Z=2 and R1=0.0730 at −113°C (Se); Xe(OTeF 5) 2 crystallizes in a monoclinic system, P2 1/ c, a=10.289(2) Å, b=9.605(2) Å, c=10.478(2) Å, β=106.599(4)°, V=992.3(3) Å 3, Z=4 and R1=0.0680 at −127°C; Xe(OSeF 5) 2 crystallizes in a triclinic system,
, a=8.3859(6) Å, c=12.0355(13) Å, V=732.98(11) Å 3, Z=3 and R1=0.0504 at −45°C. The energy minimized geometries and vibrational frequencies of the XeOChF 5+ cations and Xe(OChF 5) 2 were calculated using density functional theory, allowing for definitive assignments of their experimental vibrational spectra. 相似文献
4.
Two nickel (imidazole) complexes, Ni(im) 6Cl 2·4H 2O (1) and Ni(im) 6(NO 3) 2 (2) (im=imidazole) have been synthesized and characterized by elemental analysis, IR, UV, TG and single crystal X-ray diffraction. 1 crystallizes in the triclinic space group P-1 with a=8.800(6) Å, b=9.081(6) Å, c=10.565(7) Å, =75.058(9)°, β=83.143(8)°, γ=61.722(8)°, V=718.3(8) Å 3, Z=1 and R1 ( wR2)=0.0469 (0.1497). 2 crystallizes in the trigonal space group R-3 with a=12.370(6) Å, b=12.370(6) Å, c=14.782(14) Å, =90.00°, β=90.00°, γ=120.00°, V=1959(2) Å 3, Z=3 and R1 ( wR2)=0.0358 (0.0955). 1 and 2 exhibit different supramolecular network due to their different counter anions and different hydrogen bonding connection. In compound 1, [Ni(im) 6] 2+ cation and counter anions Cl − alternatively array in an ABAB fashion via N–HCl hydrogen bonding. In compound 2, the plane of each NO 32− is almost parallel and each NO 32− connect three different [Ni(im) 6] 2+ cations via N–HO hydrogen bonding. 相似文献
5.
The compound [Zn(H 2O) 4] 2[H 2As 6V 15O 42(H 2O)]·2H 2O (1) has been synthesized and characterized by elemental analysis, IR, ESR, magnetic measurement, third-order nonlinear property study and single crystal X-ray diffraction analysis. The compound 1 crystallizes in trigonal space group R3, a= b=12.0601(17) Å, c=33.970(7) Å, γ=120°, V=4278.8(12) Å 3, Z=3 and R1( wR2)=0.0512 (0.1171). The crystal structure is constructed from [H 2As 6V 15O 42(H 2O)] 4− anions and [Zn(H 2O) 4] 2+ cations linked through hydrogen bonds into a network. The [H 2As 6V 15O 42(H 2O)] 6− cluster consists of 15 VO 5 square pyramids linked by three As 2O 5 handle-like units. 相似文献
6.
Excitation of solutions of Fe(bipy) 2(CN) 2 by a 266-nm laser pulse produces a hydrated electron and the oxidized complex, Fe(bipy) 2 (CN) 2+, in the primary photochemical step, in homogeneous aqueous solution as well as in aqueous solutions containing cetyltrimethylammonium bromide (CTAB) or sodium dodecyl sulfate (SDS) micelles. In all cases nascent hydrated electrons react with ground state Fe(bipy) 2(CN) 2 to form Fe(bipy) 2(CN) 2−, and comparison of the decay constants in the three media (H 2O: k = 2.8 × 10 10 M −1 s −1; CTAB: k = 2.9 × 10 10 M −1 s −1; SDS: k = 5.5 × 10 9 M −1 s −1), shows that the reaction is essentially unaffected by CTAB micelles but is much slower in SDS solution. Similar micellar effects were found for the back reaction between e aq− and Fe(bpy) 2(CN) 2+. Rate constants for the scavenging of the photogenerated hydrated electrons by methyl viologen (MV 2+) cations and NO 3− anions were measured in the three systems, and the results indicate that for scavenging by MV 2+ the rate constants are decreased in the micelle systems ( k in H 2O, 8.4 × 10 10; CTAB, 3.5 × 10 10 and SDS, 1.58 × 10 10 M −1 s −1), whereas for NO 3− the CTAB micelle decreases while the SDS micelle enhances the scavenging compared to water solution ( k in H 2O, 8.3 × 10 9; CTAB, 7 × 10 8; and SDS, 2.05 × 10 10 M −1 s −1). For the comproportionation reaction between Fe(bipy) 2(CN) 2+ and Fe(bipy) 2(CN) 2− both micelles reduce the rate ( k in H 2O, 3.3 × 10 10; CTAB, 2.3 × 10 10; and SDS, 1.05 × 10 10 M −1s −1), but while the reaction of Fe(bipy) 2(CN) 2+ with MV + is increased in CTAB compared to water, it is slowed in SDS ( k in H 2O, 2.4 × 10 10; CTAB, 8.9 × 10 10; and SDS, 1.8 × 10 10 M −1s −1). All effects observed in these microheterogeneous systems can be uniformly interpreted in terms of Coulombic interactions between the actual reactants and the charged surface of the micelles. 相似文献
7.
The title calixarene, dimanganese thiacalix[4]arene tetrasulfonate, was prepared and its crystal structure was determined. [Mn(H 2O) 6] 2[thiacalix[4]arene tetrasulfonate]·0.5H 2O crystallizes in the monoclinic system, P2(1)/ m space group, with a=13.014 (6), b=14.146 (9), c=13.184 (7) Å, β=113.307 (10)°, V=2229 (2) Å 3 and Dc=1.710 gcm −3, Z=2. The title calixarene exists in the solid state as bilayer structure. The hydrophobic organic layer consists of thiacalix[4]arene tetrasulfonate in an up-down fashion, whereas, the hydrophilic inorganic layer consists of hexaaquamanganese (II) which is linked to the former through a second-sphere coordination. 相似文献
8.
Structures of the following compounds have been obtained: N-(2-pyridyl)- N′-2-thiomethoxyphenylthiourea, PyTu2SMe, monoclinic, P2 1/ c, a=11.905(3), b=4.7660(8), c=23,532(6) Å, β=95.993(8)°, V=1327.9(5) Å 3 and Z=4; N-2-(3-picolyl)- N′-2-thiomethoxyphenyl-thiourea, 3PicTu2SeMe, monoclinic, C2/ c, a=22.870(5), b=7.564(1), c=16.941(4) Å, β=98.300(6)°, V=2899.9(9) Å 3 and Z=8; N-2-(4-picolyl)- N′-2-thiomethoxyphenylthiourea, 4PicTu2SMe, monoclinic P2 1/ a, a=9.44(5), b=18.18(7), c=8.376(12) Å, β=91.62(5)°, V=1437(1) Å 3 and Z=4; N-2-(5-picolyl)- N′-2-thiomethoxyphenylthiourea, 5PicTu2SMe, monoclinic, C2/ c, a=21.807(2), b=7.5940(9), c=17.500(2) Å, β=93.267(6)°, V=2893.3(5) Å 3 and Z=8; N-2-(6-picolyl)- N′-2-thiomethoxyphenylthiourea, 6PicTu2SMe, monoclinic, P2 1/ c, a=8.499(4), b=7.819(2), c=22.291(8) Å, β=90.73(3)°, V=1481.2(9) Å 3 and Z=4 and N-2-(4,6-lutidyl)- N′-2-thiomethoxyphenyl-thiourea, 4,6LutTu2SMe, monoclinic, P2 1/ c, a=11.621(1), b=9.324(1), c=14.604(1) Å, β=96.378(4)°, V=1572.4(2) Å 3 and Z=4. Comparisons with other N-2-pyridyl- N′-arylthioureas having substituents in the 2-position of the aryl ring are included. 相似文献
9.
Syntheses and crystal structures of 1,2:5,6:9,10:13,14:17,18:21,22-hexabenzo-3,7,11,15,19,23-hexadehydro[24]annulene (HBC), 1,2:5,6:9,10:13,14-tetrabenzo-3,7,11,15-tetradehydro[16]annulene (QBC) and a tetracobalt complex of QBC. The first example of a transition metal complex of QBC
1,2:5,6:9,10:13,14-Tetrabenzo-3,7,11,15-tetradehydro[16]annulene, or tetrabenzocyclyne (QBC) and 1,2:5,6:9,10:13,14:17,18:21,22-hexabenzo-3,7,11,15,19,23-hexadehydro[24]annulene (HBC) have been structurally characterized by X-ray. crystallography. QBC crystallizes in two different space groups; P2 1/ c with a = 10.652(3) Å, b = 10.624(2) Å, c = 19.549(4) Å, β = 93.83(2)°, V = 2207.4(8) Å 3, and Z = 4 and P4 12 12 with a = 9.330(1) Å, c = 25.497(8) Å, V = 2219.6(12) Å, and Z = 4. HBC crystallizes in monoclinic P2 1/ n with a = 14.763(3) Å, b = 10.296(2) Å, c = 22.057(4) Å, β = 108.61(3), V = 3177.4(11) Å 3, T = 133 K, and Z = 4. Reaction of QBC with dicobaltoctacarbonyl has produced a tetracobalt complex which has been characterized by X-ray crystallography. This complex crystallizes in monoclinic P2 1/ c with a = 14.699(3) Å, b = 17.188(3) Å, c = 17.254(3) Å, β = 112.63(3)°, V = 4023.5(13) Å 3, and Z = 4. Only two of the four C---C triple bonds of QBC bind to dicobalthexacarbonyl moieties even when excess dicobaltoctacarbonyl is used. 相似文献
10.
One-dimensional Co(dien) 2(VO 3) 3·(H 2O) was prepared from the hydrothermal reaction of NH 4VO 3, Co 2O 3, diethylenetriamine (dien) and H 2O at 130 °C. The compound crystallizes in the monoclinic system, space group P2 1/ c with a=16.1581(6) Å, b=8.7006(3) Å, c=13.9893(4) Å, β=103.1483(11)°, V=1915.13(11) Å 3, Z=4, and R1=0.0268 for 3060 observed reflections. Single crystal X-ray diffraction revealed that the structure is composed of infinite one-dimensional chains formed by corner-sharing VO 4 tetrahedra with Co(dien) 3+ complex cations and crystallization water molecules occupying the interchain positions, which are held together to a three-dimensional network via extensive hydrogen-bonding interactions. The compound, with a new zig-zag conformation of metavanadate chains, is the first example of vanadium oxides incorporating trivalent transition metal coordination groups. Other characterizations by elemental analysis, IR and thermal analysis are also described. 相似文献
11.
The crystal structures of pharmaceutical product mesalazine (marketed also under different proprietary names as Salofalk, Asacol, Asacolitin, and Claversal) and its hydrochloride are reported. In the crystal mesalazine is in zwitterion form as 5-ammoniosalicylate (1) whereas mesalazine hydrochloride crystallizes in an ionized form as 5-ammoniosalicylium chloride (2). Compound 1 (C 7H 7O 3N) crystallizes in the monoclinic space group P2 1/ n with a = 3.769(1) Å, b = 7.353(2) Å, c = 23.475(5) Å, β = 94.38(2)°, V = 648.7(8) Å 3, Z = 4, Dc = 1.568 g cm −3 and μ( MoK) = 1.2 cm −1. Compound 2 (C 7H 8O 3NCl) crystallizes in the triclinic space group P
with a = 4.4839(2) Å, b = 5.7936(2) Å, c = 15.6819(5) Å, = 81.329(3)°, β = 88.026(3)°, γ = 79.317(4)°, V = 395.74(3) Å 3, Z = 2, Dc = 1.591 g cm −3 and μ(CuK) = 40.8 cm −1. The crystal structures were solved by direct methods and refined to R = 0.041 for 1 and 0.028 for 2, using 607 and 1374 observed reflections, respectively. The configuration of both molecules, with the ortho hydroxyl to a carboxyl group, favours the intramolecular hydrogen bonds. Very complex systems of intermolecular hydrogen bonds were observed in both crystal packings. They are discussed in terms of graph-set notation. The mesalazine crystal structure is characterized by two-dimensional network of hydrogen bonds in the ab plane. The crystal structure pattern of mesalazine hydrochloride is a three-dimensional network significantly supported by N +---HCl − interactions. 相似文献
12.
The syntheses and structural determination of Nd III and Er III complexes with nitrilotriacetic acid (nta) were reported in this paper. Their crystal and molecular structures and compositions were determined by single-crystal X-ray structure analyses and elemental analyses, respectively. The crystal of K 3[Nd III(nta) 2(H 2O)]·6H 2O complex belongs to monoclinic crystal system and C2/ c space group. The crystal data are as follows: a=1.5490(11) nm, b=1.3028(9) nm, c=2.6237(18) nm, β=96.803(10)°, V=5.257(6) nm 3, Z=8, M=763.89, Dc=1.930 g cm −3, μ=2.535 mm −1 and F(000)=3048. The final R1 and wR1 are 0.0390 and 0.0703 for 4501 ( I>2σ( I)) unique reflections, R2 and wR2 are 0.0758 and 0.0783 for all 10474 reflections, respectively. The Nd IIIN 2O 7 part in the [Nd III(nta) 2(H 2O)] 3− complex anion has a pseudo-monocapped square antiprismatic nine-coordinate structure in which the eight coordinate atoms (two N and six O) are from the two nta ligands and a water molecule coordinate to the central Nd III ion directly. The crystal of the K 3[Er III(nta) 2(H 2O)]·5H 2O complex also belongs to monoclinic crystal system and C2/ c space group. The crystal data are as follows: a=1.5343(5) nm, b=1.2880(4) nm, c=2.6154(8) nm, b=96.033(5)°, V=5.140(3) nm 3, Z=8, M=768.89, Dc=1.987 g cm −3, μ=3.833 mm −1 and F(000)=3032. The final R1 and wR1 are 0.0321 and 0.0671 for 4445 ( I>2σ( I)) unique reflections, R2 and wR2 are 0.0432 and 0.0699 for all 10207 reflections, respectively. The Er IIIN 2O 7 part in the [Er III(nta) 2(H 2O)] 3− complex anion has the same structure as Nd IIIN 2O 7 part in which the eight coordinate atoms (two N and six O) are from the two nta ligands and a water molecule coordinate to the central Nd III ion directly. 相似文献
13.
Upon UV irradiation in hexane at 243 K tricarbonyl-η 5-cyclohexadienyl-manganese (1) and two equivalents of 2-butyne (2) or diphenylacetylene (4) yield in successive [5 + 2, 3 + 2] cycloadditions tricarbonyl-η 2:2:1-1,2,3,10-tetramethyl-tricyclo[5.2.1.0 4,9]-deca-2,5-dien-10-yl-manganese (6), or tricarbonyl-η 2:2:1-1,2,3,10-tetraphenyl-tricyclo[5.2.1.0 4,9]-deca-2,5-dien-10-yl-manganese (8), respectively. 3-Hexyne (3) reacts with 1 under the same conditions by successive [5 + 2, 3 + 2] cycloadditions and 1,4-H-shift to tricarbonyl-η 2:2:1-1,2,3-triethyl-10-ethylidene-tricyclo[5.2.1.0 4,9]dec-2-en-5-yl-manganse (7). Identical products are also obtained when 1 is first irradiated in THF at 208 K and the thermolabile intermediate, dicarbonyl-η 5-cyclohexadienyl-tetrahydrofurane-manganese (11), is treated with an excess of the alkynes 2–4. In contrast, bis(trimethylsily)acetylene (5) substitutes photochemically in 1 only a CO ligand to yield dicarbonyl-η 5-cyclohexadienyl-η 2-bis(trimethylsily)Acetylene-manganese (9). The crystal and molecular structure of 7 was determined by an X-ray diffraction analysis. Complex 7 crystallizes in the triclinic space group
, a = 822.6(2) pm, B = 882.5(2) pm, C = 1344.6(2) pm, = 92.36(2)°, β = 107.13(2)°, γ = 99.71(2)°, V = 0.9152(3) nm 3, Z = 2. The complexes 6–9 were studied in solution by IR and NMR spectroscopy. The structures of 6,8 and 9 were elucidated from the NMR spectra. A possible formation mechanism for the complexes 6–9 will be discussed. 相似文献
14.
A hydrothermal reaction of 1,3-dicyanobenzene and Ca(OH) 2 yielded a triple helical calcium-based coordination polymer of the formula, C 20H 25Ca 2.50O 18.50 (1). The 1,3-benzenecarboxylate anion, found in the final product was generated in situ during the synthesis by the hydrolysis of 1,3-dicyanobenzene. X-ray diffraction study shows that the complex 1 crystallizes in the monoclinic system, C2/c space group, a=15.5701(5), b=21.4445(7), c=17.1601(6) Å, β=111.7400(7)°, V=5322.1(3) Å 3, Z=8, Dc=1.651 Mg/m 3. The calcium atoms show differences in the coordination environments. Complex 1 emits strong blue fluorescent light ( λem(max)=419 nm) when it is excited by UV light ( λex(max)=316 nm) in the solid state at room temperature. 相似文献
15.
The crystal structure of N-(2-hydroxy-5-chlorophenyl) salicylaldimine (C 13H 10NO 2Cl) was determined by X-ray analysis. It crystallizes orthorhombic space group P2 12 12 1 with a=12.967(2) Å, b=14.438(3) Å, c=6.231(3) Å, V=1166.5(6) Å 3, Z=4, Dc=1.41 g cm −3 and μ(MoK )=0.315 mm −1. The title compound is thermochromic and the molecule is nearly planar. Both tautomeric forms (keto and enol forms in 68(3) and 32(3)%, respectively) are present in the solid state. The molecules contain strong intramolecular hydrogen bonds, N1–H1O1/O2 (2.515(1) and 2.581(2) Å) for the keto form and O1–H01N1 for the enol one. There is also strong intermolecular O2–HO1 hydrogen bonding (2.599(2) Å) between neighbouring molecules. Minimum energy conformations AM1 were calculated as a function of the three torsion angles, θ1(N1–C7–C6–C5), θ2(C8–N1–C7–C6) and θ3(C9–C8–N1–C7), varied every 10°. Although the molecule is nearly planar, the AM1 optimized geometry of the title compound is not planar. The non-planar conformation of the title compound corresponding to the optimized X-ray structure is the most stable conformation in all calculations. 相似文献
16.
The molecular structure of the title complex [ZnBr 2(C 7H 6N 2) 2] was investigated by X-ray diffraction and IR spectroscopy methods. Molecules of zinc(II) complex crystallize in the triclinic crystal system with cell constants a=7.526(2) Å, b=7.8971(8) Å, c=13.431(1) Å, Z=2 and V=791.3(2) Å 3. In the molecular structure, the Zn atom is coordinated tetrahedrally by two Br − anions and two benzimidazole ligands. Intramolecular steric repulsions between Br − anions and benzimidazole groups have been caused to cis configuration around the central metal atom. 相似文献
17.
A tetrasilver(I) phosphonitocavitand was synthesized and structurally characterized. The compound crystallizes in the monoclinic space group P2 1/ n with a=15.0151(13), b=39.832(4), c=15.2479(14) Å, β=95.1000(2)°, V=9083.3(14) Å 3 and Z=4. The structure contains four coplanar silver atoms bridged by four μ-Cl and one central trapped μ 4-Cl atoms in the inside of the closing bowl-shaped cavitand. Nonlinear optical properties of this metal-cavitand were investigated. Optical limiting effect with threshold of 0.6 J cm −2 was observed with the laser pulses of 7 ns at 532 nm. 相似文献
18.
UV irradiation of tricarbonyl-η 5-2,4-dimethyl-2,4-pentadien-1-yl-manganese (2) in THF at 208 K yields solvent-stabilized dicarbonyl-η 5-2,4-dimethyl-2,4-pentadien-1-yl-tetrahydrofurane-manganese (3), which reacts in situ with two equivalents of 1-dimethylamino-2-propyne (4) to dicarbonyl-1–5-η-2,4-dimethyl-(6-dimethylaminomethyl- N)-10-dimethylamino-deca-2,4,6,8- tetraen-1-yl-manganese (5). The crystal and molecular structure was determined by an X-ray diffraction analysis. Complex 5 crystallizes in the monoclinic space group P2 1/ c, A = 1109.9(2) pm, B = 836.0(2) pm, C = 2156.9(4) pm, β = 93.23(3)°, V = 1.9982(7) nm 3, Z = 4. Complex 5 was also studied in solution by IR and NMR spectroscopy. A possible formation mechanism of 5 will be discussed. ZusammenfassungUV-Bestrahlung von Tricarbonyl-η5-2,4-dimethyl-2,4-pentadien-1-yl-mangan (2) in THF bei 208 K liefert solvenstabilisiertes Dicarbonyl-η5-2,4-dimethyl-2, 4-pentadien-1-yl-tetrahydrofuran-mangan (3), welches in situ mit zwei Äquivalenten 1-Dimethylamino-2-propin (4) zu Dicarbonyl-1–5-η-2,4-dimethyl-(6-dimethylaminomethyl-N)-10-dimethylamino-deca-2,4,6,8-tetraen-1-yl-mangan (5) reagiert. Seine Kristall- und Molekülstruktur wurde durch eine Röntgenbeugungsanalye bestimmt. Komplex 5 kristallisiert in der monoclinen Raumgruppe P21/c, A = 1109.9(2) pm, B = 836.0(2) pm, C = 2156.9(4) pm, β = 93.23(3)°, V = 1.9982(7)_ nm3, Z = 4. Komplex 5 wurde auch in Lösung IR- und NMR-spektroskopisch untersucht. Ein möglicher Bildungsmechanismus von 5 wird diskutiert. 相似文献
19.
The photocatalytic removal of the insecticide fenitrothion (IUPAC name: O, O-dimethyl O-4-nitro- m-tolyl phosphorothioate), C 9H 12NO 5PS, from water suspension of TiO 2, was investigated by following the disappearance of the original substance along with the formation and disappearance of intermediates via recording NMR ( 1H and 31P) and UV spectra, as well as by pH measurements. Based on the obtained data, a possible reaction mechanism was proposed. It was found that 31P-NMR spectrometry can be successfully used to follow the kinetics of transforming organic into inorganic phosphorus in the course of the degradation ( ka=9.2×10 −7 mol dm −3 min −1, r=0.980 for the illumination period after 15 h). The rate of fenitrothion aromatic ring decomposition was followed by UV spectrometry during the illumination ( ka=3.1×10 −6 mol dm −3 min −1, r=0.989). The complete mineralization was attained after about 66 h of irradiation. 相似文献
20.
Condensation of thiosemicarbazide or N(4)-ethylthiosemicarbazide with 1,2,8,9-tetraphenyl-3,7-diazanona-1,9-dione in the presence of copper(II) acetate in 96% ethanol leads to Δ 6-5,6-diphenyl-5-methoxy-1,2,4-triazacyclohexene-3-thione, C 16H 15N 3OS, or Δ 6-4-methyl-5,6-diphenyl-5-ethoxy-1,2,4-triazacyclohexene-3-thione, C 18H 19N 3OS. For C 16H 15N 3OS the crystal data are monoclinic, P2 1/ c, a=9.7780(7), b=8.5120(3), c=18.2210(13) Å, β=100.958(3)°, V=1488.89(16) Å 3, and Z=4 in agreement with an earlier report. For C 18H 19N 3OS the crystal data are orthorhombic, P2 12 12 1, a=8.6940(3), b=12.9946(3), c=15.5139(5) Å, V=1752.68(9) Å 3, and Z=4. 相似文献
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