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1.
Mari Sasaki Genta Sakane Tadashi Ouchi Takashi Shibahara 《Journal of Cluster Science》1998,9(1):25-43
Sulfur/oxygen-bridged incomplete cubane-type triphenylphosphine molybdenum and tungsten-clusters [Mo3S4Cl4(H2O)2(PPh3)3]·3THF (1A), [Mo3S4Cl4(H2O)2(PPh3)3]·2THF (2A), [Mo3OS3Cl4(H2O)2(PPh3)3]·2THF (1B), and [W3S4Cl4(H2O)2(PPh3)3]·2THF (1C) were prepared from the corresponding aqua clusters and PPh3 in THF/MeOH. On recrystallization from THF, procedures with and without addition of hexane to the solution gave 1A and 2A, respectively, while the procedures gave no effect on the formation of 1B and 1C. Crystallographic results obtained are as follows: 1A: monoclinic, P21/n, a=17.141(4) Å, b=22.579(5) Å, c=19.069(4) Å, =96.18(2)°, V=7337(3) Å3, Z=4, R(R
w)=0.078(0.102); 1C: monoclinic, P2
1/c, a=12.635(1) Å, b=20.216(4) Å, c=27.815(3) Å, =96.16(1)°, V=7062(2) Å3, Z=4, R(R
w)=0.071(0.083). If the phenyl groups are ignored, the molecule [Mo3S4Cl4(H2O)2(PPh3)3] in 2A has idealized CS symmetry with the mirror plane perpendicular to the plane determined by the metal atoms, while the molecule in 1A does not have the symmetry. The tungsten compound 1C is isomorphous with the molybdenum compound 2A. 31P NMR spectra of 1A, 2A, and 1C were obtained and compared with similar clusters with dmpe (1,2-bis(dimethylphosphino)ethane) ligands. 相似文献
2.
J. V. Brenčič L. Golič I. Leban P. Šegedin 《Monatshefte für Chemie / Chemical Monthly》1979,110(5):1221-1228
Mo2Cl4
Pic
4·CHCl3 (A) (Pic=4-methylpyridine) and Mo2Br4
Pic
4 (B) crystallize in the monoclinic space group.A inC2/c (No. 15) witha=15.175 (4),b=10.847 (2),c=19.946 (6) and =104.52 (2)°;D
o=1.71 (2),D
c
=1.72 gcm–3 forZ=4.B inP2l/n
(No. 14) witha=9.270 (3),b=16.614 (5),c=9.305 (3) and =91.96 (5)°;D
o=2.03 (3),D
c
=2.05 gcm–3 forZ=2.Two halogens and 4-methylpyridines of the MoX
2
Pic
2 group are in the trans position. Mo–Mo bond lengths are 2.153 96) forA and 2.150 92) forB. Both molecules are situated on the inversion center resulting in the eclipsed configuration of the ligands around the molybdenum pair. The structure ofB has been refined to the conventionalR factors of 0.08 and 0.098. Disorder on the part of 4-methylpyridines and chloroform molecules stopped the refinement ofA at the endR value of 0.175.Mean Mo–X and Mo–N bonding distances are 2.40 (2), 2.25 (5) forA and 2.53 (3), 2.25 (1) forB. 相似文献
3.
《Journal of Coordination Chemistry》2012,65(7):1198-1206
Two new compounds, [Zn(phen)3]2[γ-As8V14O42(H2O)]?·?4H2O (1) and [Cd(phen)3]2[γ-As8V14O42(H2O)]?·?2H2O (2) (phen?=?1,10′-phenanthroline), have been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, infrared spectrum, and thermogravimetric analysis. Compound 1 crystallizes in the triclinic space group P 1 with a?=?11.429(4)?Å, b?=?15.760(5)?Å, c?=?15.952(5)?Å, α?=?108.825(5)°, β?=?92.194(5)°, γ?=?104.155(5)°, V?=?2615.6(15)?Å3, Z?=?1; 2 crystallizes in the triclinic space group P 1 with a?=?11.450(4)?Å, b?=?15.629(6)?Å, c?=?16.302(6)?Å, α?=?109.177(5)°, β?=?92.628(5)°, γ?=?104.251(4)°, V?=?2644.8(17)?Å3, Z?=?1. Single-crystal structural analysis shows that both 1 and 2 consist of a new type of [γ-As8V14O42(H2O)]4? cluster anion. 相似文献
4.
A novel selective and sensitive colorimetric receptor 1 (1, 10-phenanthroline-2, 9-dialdehyde bis-(-p-nitrophenylureasemicarbo-hydrazone)) based on urea showing distinctive color fading phenomenon towards H2PO4? ion was reported. Fancifully, the recognition process of receptor 1 to H2PO4? was not interfered by the existence of others anions. We have probed the binding mechanism of 1-H2PO4? that H2PO4? ion induced competitive hydrogen binding process via intramolecular hydrogen-bond by UV–vis, fluorescence, 1H NMR titrations and ESI-MS experiments. 相似文献
5.
《Journal of Coordination Chemistry》2012,65(16-18):2965-2977
AbstractThermal treatment of pyridine-2-ethyl cyclopentadiene (1) with Fe(CO)5 and Ru3(CO)12 gave novel intramolecular C–H activated dinuclear products (3 and 5). In the case of Fe(CO)5, the reaction also afforded the normal bis(cyclopentadienyl) diiron complex (4). However, similar reaction of pyridine-2-methyl cyclopentadiene (2) with Fe(CO)5 and Ru3(CO)12 only afforded the normal bis(cyclopentadienyl) dinuclear metal complexes (7 and 8). For Ru3(CO)12, the reaction also yielded a pendant η1-pyridyl-coordinated product (9). In addition, the reactions of 1 and 2 with Re2(CO)10 formed the corresponding pyridylethyl/pyridylmethyl cyclopentadienyl rhenium tricarbonyl complexes 10 and 11, which further underwent pyridine to rhenium cyclization via photoirradiation to provide the rhenium dicarbonyl complexes 12 and 13. The molecular structures of 3, 5, 6, 7, 8, 9, and 12 were determined by X-ray diffraction. 相似文献
6.
《Journal of Coordination Chemistry》2012,65(7):1167-1176
In thermal reactions of the doubly bridged dicyclopentadienes (C5H3R(SiMe2))(C5H3R(GeMe2)) (R=H (1), tBu (5)) with Mo(CO)6, the bridging GeMe2 is cleaved to give the corresponding degermylated products [(η5-C5H3R)2(SiMe2)]Mo2(CO)6 (3, rac-7), or both GeMe2 and SiMe2 are cleaved to afford the nonbridged products [(η5-C5H4R)Mo(CO)3]2 (2, 6). The reactions also produce germylidyne trimolybdenum clusters [(η5-C5H3R)2(SiMe2)](η5-C5H4R)[Mo(CO)2]3(μ3-GeMe) (4, rac-/meso-7) containing the Mo3(μ3-GeMe) units. Similarly, reaction of the single GeMe2-bridged dicyclopentadienes (C5H5)2GeMe2 (9) with Mo(CO)6 also results in the degermylated 2, as well as the similar trimolybdenum cluster [(η5-C5H5)Mo(CO)2]3(μ3-GeMe) (10). The molecular structures of 4 and trans-5 were determined by X-ray diffraction. 相似文献
7.
C. Hamon J. D. Soilan-Rodriguez H. Kalchhauser W. Reischl 《Monatshefte für Chemie / Chemical Monthly》1997,128(12):1297-1300
Summary When the benzoate of (S)-(Z)-2-(5-(tert-butyldimethylsiloxy)-2-methylencyclohexyliden)-ethanol (5) is treated with 2.5 equivalents of Hg(OOCCF3)2 in dryTHF, a smooth and selective allylic hydroxylation occurs. The C-1 functionalized vitamin D A-ring synthon6 is isolated in 65 to 70% yield in a single step.
Hydroxylierung eines Vitamin D A-Ring-Fragments (Kurze Mitt.)
Zusammenfassung Umsetzung des Benzoats von (S)-(Z)-2-(5-(tert-Butyldimethylsiloxy)-2-methylencyclohexyliden)-ethanol (5) mit 2.5 Äquivalenten Hg(OOCCF3)2 in trockenemTHF führt zu einer selektiven allylischen Hydroxylierung. Damit ist das an C-1 funktionalisierte Vitamin D A-Ring-Fragment6 in einem einzigen Schritt in einer Ausbeute von 65 bis 70% zugänglich.相似文献
8.
D. V. Konarev R. N. Lyubovskaga O. S. Roshchupkina B. P. Tarasov Yu. M. Shulga 《Russian Chemical Bulletin》1997,46(1):32-35
Compounds C60(S4N4)2−x
(C6H6)
x
(1a-d) withx=0.67 (a), 1.0 (b), 1.1 (c), and 1.2 (d), in which isomorphous replacement of S4N4 with benzene takes place, were obtained by the reaction of fullerence C60 with tetrasulfur tetranitride in benzene. Complexes C60·S4N4 (2) and C60(S4N4)2 (3) containing no solvent were isolated from toluene. The compositions of the compounds were established by elemental and thermogravimetric
analyses. The data of IR and X-ray photoelectron (XP) spectroscopies show that in the complexes studied the transfer of electron
density occurs mainly from the nitrogen atoms of S4N4.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 37–40. January 1977. 相似文献
9.
I. Ban L. Golič S. Milićev B. Volavšek 《Monatshefte für Chemie / Chemical Monthly》1995,126(12):1279-1289
Summary Hydroxylammonium fluorozirconates have been investigated. Two new microcristalline phases have been isolated from aqueous solutions: (NH3OH)2ZrF6 (1) and (NH3OH)3ZrF7 (2). The crystals were prepared by slow evaporation of the solution of NH2OH, Zr, and HF. Different compositions of the crystals were achieved by varying the molar ratios of the components. They were characterized by thermal analysis, vibrational spectroscopy, and structure (single crystal x-ray methods). (NH3OH)2ZrF6 (1) crystallizes triclinic, P
(No.: 2),a=7.400(2),b=7.609(2),c=7.887(2) Å, =57.29(3)°, =62.16(3)°, =67.83(2)°. (NH3OH)3ZrF7 (2) crystallizes triclinic, P
(No.: 2),a=7.128(1),b=7.989(1),c=8.888(1) Å, =109.72(1)°, =91.01(1)°, =104.27(1)°. 相似文献
10.
Linyan Yang Yamin Zong Lisha Yang Rui Lv Liyuan Jing Jifei Ma 《Journal of Coordination Chemistry》2017,70(12):2161-2173
One-pot solvothermal treatment of Co(NO3)2·6H2O, H2L (5-(3-methyl-5-(pyridin-4-yl)-4H-1,2,4-triazol-4-yl) isophthalic acid), and 4,4′-bipyridine (4,4′-bipy) in H2O/DMF (V/V = 1?:?1) yielded a cobalt-organic chain, [Co(L)(O)(H2O)2]n·1.25nH2O (1). Compound 1 as raw materials was calcined to obtain Co3O4, which could be confirmed by PXRD and SEM. Via the modification, Co3O4@SiO2-NH2 and Co3O4@SiO2-NH2-FA samples could be obtained. Compared to Co3O4@SiO2-NH2, Co3O4@SiO2-NH2-FA seems to have better peroxidase-mimetic properties. UV–vis results showed that optimal conditions of peroxidase-mimetic experiments were at 50°C in sodium acetate-acetic acid buffer (pH 3.6, 0.2 M), when the concentration of tetramethylbenzidine (TMB) was 0.2 mM. A concentration-dependent manner was shown between the concentration of glucose and absorbance in the measurement experiments for glucose. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(2):306-315
Reactions of 2,4-dihydroxyacetophenone oxime with manganese salts yielded two manganese crowns, [Mn3(μ 3-O)(4-OH-Me-sao)3(HCOO)(MeOH)5]·MeOH (1) and [Mn3(μ 3-O)(4-OH-Me-sao)3(CH3COO)(MeOH)5]·MeOH (2) (4-OH-Me-saoH2=2,4-dihydroxyacetophenone oxime). Both compounds possess [MnIII 3(μ 3-O)]7+ cores which contain 9-MC-3 metallacrown (MC) rings with the repeating pattern [–Mn–N–O–]. However, the difference in the structures of both compounds is coordinated carboxylates. In 1 and 2, the MC molecules are connected with each other through intermolecular hydrogen bonds, generating similar 3-D supramolecular networks. Magnetic properties reveal that in 1 and 2 the metal ions exhibit ferromagnetic exchange coupling. 相似文献
12.
13.
通过溶剂热法合成了2种三维微孔锌金属有机框架材料,其分子式为[Zn3(DBA)(OH)(1,10-phen)2]n (1)和{[Zn2(HDBA)(4,4′-bipy)1.5]·H2O}n (2)(H5DBA=3,5-二(2′,4′-对羧基苯基)苯甲酸;1,10-phen=1,10-菲咯啉;4,4′-bipy=4,4′-联吡啶)。结构分析表明,配合物1为三核锌基金属单元的三维微孔骨架,配合物2为双核锌基的微孔结构。与2相比,配合物1在水中具有较强的发光性能,可作为检测Fe3+、Cr2O72-和丙酮分子的发光传感器,具有较高的选择性和灵敏度。 相似文献
14.
E. Fluck C. M. E. Pavlidou R. Janoschek 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):469-474
Abstract Experimental findings as well as quantum chemical calculations indicate that the P4 molecule has a remarkably low nucleophilicity. The P4H+ ion is predicted to have a ‘proton at apex’ configuration whereas a proton in the centre seems to be metastable. The influence of d orbitals on the stability of P4 against 2 P2 and 1/2 P8, the photoelectron spectrum, and the valence electron density is discussed. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(10):1623-1629
Using 3,5-dimethyl-4-amino-1,2,4-triazole (L) and corresponding Ag(I), K(I) salts under ammonia solution and hydrothermal conditions, a triazole–silver(I)–potassium(I) complex {K[Ag2L2(μ 3-Cl)(μ 2-Cl)2]} n (1) has been isolated. In 1, μ 3-Cl, μ 2-Cl and L bridge AgI ions forming a rare 1-D [Ag2L2(μ 3-Cl)(μ 2-Cl)2]? anion while K+ cations are located between neighboring anion chains. Strong solid-state fluorescence spectrum of 1 was also investigated showing that the excited peak is located at 320 nm while the maximum emission peak is located at 440 nm. 相似文献
16.
The reactions ofo-tosylaminobenzaldehyde (1) withp-aminobenzenesulfonamides (2a-c) yielded 13-(p-RNHSO2C6H4)-6,12-epimino-5,11-ditosyl-5,6,11,12-tetrahydrodibenzo[b f]-1,5-diazocines (3a-c) (R=H (a); 2-thiazolyl (b); or 2,6-dimethoxy-4-pyrimidinyl 2,6-dimethoxy-4-pyrimidinyl (c). The structure of compound3c was confirmed by X-ray diffurction study.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2035–2039, November, 1997. 相似文献
17.
Hui-Bo Zhou Dai-Zheng Liao Li-Xin Deng Jing-Zhong Yu Yang-Ping Gao Xiao-Fang Yang Zong-Hui Jiang Shi-Ping Yan Peng Cheng 《Structural chemistry》2006,17(1):43-47
Two new complexes, [Cu(L1){N(CN)2}]·ClO4 (1) (L1 is 1,8-dimethyl-1,3,6,8,10,13-hexa-azacyclotetradecane) and [Co(L2)(N3)2]·ClO4 (2) (L2 is 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyclotetradecane) have been synthesized and characterized. The compounds crystallize in the monoclinic system P21 space group for 1 and P21/n for 2. Single crystal X-ray analysis reveals that the compound 1 assumes a one-dimensional structure via hydrogen-bonding interactions, in which each Cu(II) ion is coordinated by four nitrogen atoms from ligand L1 and one nitrogen atom from [N(CN)2]− anion. For compound 2, each Co(III) ion is coordinated by four nitrogen atoms of ligand L2 and two nitrogen atoms from N3
− anion. 相似文献
18.
19.
20.
Topological analysis of the crystal structure of Na2ZrSi2O7 (parakeldyshite, space group P1–) with an MT framework, where M are ZrO6 octahedra and T are SiO4 tetrahedra, was carried out by the method of coordination sequences (TOPOS.3.2 program package), and the self-organization of this structure was modeled. The cyclic-type suprapolyhedral cluster precursor Na2M2T4 with the local symmetry 1– was identified by bicolor decomposition of the 4646+664 net. The cluster is composed of six polyhedra with two Na atoms located in the center. The precursors control the evolution of high-level crystal-forming clusters. The cluster coordination number is six. The centers of eight cluster precursors in the superprecursor of the Na2ZrSi2O7 structure are related by translation vectors. 相似文献