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1.
The C,N-(trimethylsilyliminodiphenylphosphoranyl)silylmethylmetal complexes [Fe(L)2] (3), [Co(L)2] (4), [ZrCl3(L)]·0.83CH2Cl2 (5), [Fe(L)3] (6), [Fe(L′)2] (7) and [Co(L′)2] (8) have been prepared from the lithium compound Li[CH(SiMe2R)P(Ph)2NSiMe3] [1a, (R = Me) {≡ Li(L)}; 1b, (R = NEt2) {≡ Li(L′)}] and the appropriate metal chloride (or for 7, FeCl3). From Li[N(SiMe3)C(Ph)C(H)P(Ph)2NSiMe3] [≡ Li(L″)] (2), prepared in situ from Li(L) (1a) and PhCN, and CoCl2 there was obtained bis(3-trimethylsilylimino- diphenylphosphoranyl-2-phenyl-N-trimethylsilyl-1-azaallyl-N,N′)cobalt(II) (9). These crystalline complexes 3-9 were characterised by their mass spectra, microanalyses, high spin magnetic moments (not 5) and for 5 multinuclear NMR solution spectra. The X-ray structure of 3 showed it to be a pseudotetrahedral bis(chelate), the iron atom at the spiro junction. 相似文献
2.
Falguni Basuli 《Journal of organometallic chemistry》2011,696(1):235-243
A series of reactivity studies of the carboamination pre-catalyst [Ti(NMe2)3(NHMe2)][B(C6F5)4] as well as the preparation of other catalysts are reported in this work. Treatment of [Ti(NMe2)3(NHMe2)][B(C6F5)4] with the aldimines Ar′NCHtol (Ar′ = 2,6-Me2C6H3, tol = 4-MeC6H4), and depending on the reaction conditions, results in isolation of [Me2NCHR′][B(C6F5)4] (1) or (Me2N)2CHtol, as well as the asymmetric titanium dimer [(Me2N)2(HNMe2)Ti(μ2-N[2,6-Me2C6H3])2Ti(NHMe2)(NMe2)][B(C6F5)4] (2). Protonation of CpTi(NMe2)3 and Cp∗Ti(NMe2)3 results in isolation of the salts, [CpTi(NMe2)2(NHMe2)][B(C6F5)4] (3) and [Cp∗Ti(NMe2)2(NHMe2)][B(C6F5)4] (4), respectively. Treatment of compounds 3 or 4 with H2N[2,6-iPr2C6H3] results in formation of the imido salts [CpTi(N[2,6-iPr2C6H3])(NHMe2)2][B(C6F5)4] (5) (58% yield) or [Cp∗Ti(N[2,6-iPr2C6H3])(NHMe2)2][B(C6F5)4] (6). When Ti(NMe2)4 is treated with [Et3Si][B(C6F5)4], the salt [Ti(NMe2)3(N[SiEt3]Me2)][B(C6F5)4] (7) is obtained, and treatment of the latter with [2,6-iPr2C6H3]NCHtol produces the imine adduct [Ti(NMe2)3(κ1-[2,6-iPr2C6H3]NCHtol)][B(C6F5)4] (8). The carboamination catalytic activity of complexes 2-7 was investigated and compared to [Ti(NMe2)3(NHMe2)][B(C6F5)4]. Likewise, a proposed mechanism to the active carboamination catalyst stemming from [Ti(NMe2)3(NHMe2)][B(C6F5)4] is described. 相似文献
3.
Nallasamy Palanisami 《Journal of organometallic chemistry》2006,691(15):3260-3266
Aminosilanes bearing bulky substituents on nitrogen centers, [(ArNH)2SiPhMe] (Ar = 2,6-iPr2C6H3 (1), 2,4,6-Me3C6H2 (2)) and half-sandwich lithium silylamide [(2,6-Et2C6H3NLi)(2,6-Et2C6H3NH)SiPh2] (3) have been prepared and characterized by elemental analysis, IR, EI mass and NMR (1H and 29Si) spectroscopic studies. The solid state structures of 2 and 3 have been determined by single crystal X-ray diffraction studies. The molecule 2 has a C1 symmetry due to the steric crowding, and the two N-H protons are approximately trans to each other. The amido nitrogen atoms in 2 show significant deviation from trigonal-planar geometry, and as a result, the observed Si-N bonds are marginally longer than those observed in aminosilanes with planar nitrogen atoms. The molecule 3 exists as discrete dimer with an inversion center. The Li ion in 3 forms intramolecular π-complex with the neighboring aryl (2,6-Et2C6H3) group, to form a half-sandwich lithium silylamide. 相似文献
4.
Juri Ugolotti 《Journal of organometallic chemistry》2011,696(6):1184-1188
Treatment of R2Si(CC-SiMe3)2 [1a (Me), 1b (Ph)] with HB(C6F5)2 at low temperature (253 K (a), 273 K (b)) gives the -B(C6F5)2 substituted silacyclobutene products (4a,b) under kinetic control. Upon warming to room temperature they disappear to form the thermodynamically favoured isomeric silole derivatives (2a,b). Similar treatment of Me2Si(CC-R1)2 [5a (R1 = Ph), 5b (R1 = tert-butyl) with HB(C6F5)2 at room temperature gave the stable -B(C6F5)2 substituted silacyclobutene derivatives 6 and 7, respectively. Subsequent photolysis resulted in a Z- to E-isomerization of the substituted exocyclic CC double bonds in these products. The silacyclobutene derivative E-6 was characterized by an X-ray crystal structure analysis. 相似文献
5.
Sergey A. Belov Dmitrii P. Krut’ko Dmitrii A. Lemenovskii Judith A.K. Howard 《Journal of organometallic chemistry》2008,693(10):1912-1918
Novel half-sandwich [C9H5(SiMe3)2]ZrCl3 (3) and sandwich [C9H5(SiMe3)2](C5Me4R)ZrCl2 (R = CH3 (1), CH2CH2NMe2 (2)) complexes were prepared and characterized. The reduction of 2 by Mg in THF lead to (η5-C9H5(SiMe3)2)[η5:η2(C,N)-C5Me4CH2CH2N(Me)CH2]ZrH (7). The structure of 7 was proved by NMR spectroscopy data. Hydrolysis of 2 resulted in the binuclear complex ([C5Me4CH2CH2NMe2]ZrCl2)2O (6). The crystal structures of 1 and 6 were established by X-ray diffraction analysis. 相似文献
6.
Franc Perdih 《Journal of fluorine chemistry》2006,127(10):1289-1293
[Na{Ti2(C5Me5)2F7}] (1) was prepared from sodium fluoride and [{Ti(C5Me5)F3}2] [H.W. Roesky, et al., Angew. Chem. Int. Ed. Engl. 31 (1992) 864-866]. The solid-state 1 consists of a polymeric chain of two rows of dititanate anions [Ti2(C5Me5)2F7]− connected by sodium ions in the middle of the chain. Each sodium ion is coordinated by five fluorine atoms from three [Ti2(C5Me5)2F7]− anions. The variable-temperature 19F NMR of CD3CN solution of 1 revealed interconversions of monomeric species [Na(CD3CN)n{Ti2(C5Me5)2F7}] (1solv) with different number of CD3CN ligands on the sodium ion. The addition of HMPA to the CD3CN solution of 1 allows 19F NMR observation of 1·HMPA (1a) and 1·HMPA·CD3CN (1b) in the slow exchange. The solid-state structure of [NaTi6(C5Me5)5F20(H2O)]·(THF) (2·THF) reveals the sodium ion coordinated by four fluorine atoms from the anion [Ti2(C5Me5)2F7]− and by three fluorine atoms from the cluster [Ti4(C5Me5)3F13(H2O)]. 相似文献
7.
[2-(Me2NCH2)C6H4]HgCl (1) was prepared by reacting HgCl2 with [2-(Me2NCH2)C6H4]Li in diethyl ether. The reactions of 1 with the sodium or ammonium salt of the appropriate thiophosphinato ligand, in 1:1 molar ratio, afford the isolation of [2-(Me2NCH2)C6H4]Hg[S(S)PR2] [R=Me (2), Et (3), Ph (4)], [2-(Me2NCH2)C6H4]Hg[S(O)PPh2] (5) and [2-(Me2NCH2)C6H4]Hg[S(S)P(OiPr)2] (6). The compounds were investigated by IR and multinuclear NMR (1H, 13C and 31P) spectroscopy. The molecular structures of 1 and 4 were determined by single-crystal X-ray diffraction. Due to the strong intramolecular coordination of the N atom of the pendant CH2NMe2 arm [Hg(1)-N(1) 2.764(6) and 2.725(4) Å in 1 and 4, respectively] both compounds exhibit a T-shaped (C,N)HgX core in the molecular unit, with almost linear arrangement of the covalent bonds [C(1)-Hg(1)-Cl(1) 176.93(18)° in 1, and C(1)-Hg(1)-S(1) 169.54(16)° in 4]. The crystals of 1 contain discrete monomeric molecules, while the crystals of 4 contain dimer associations built through asymmetric bridging dithiophosphinato ligands [Hg(1)-S(1) 2.3911(16) Å, Hg(1)?S(2a) 3.102(2) Å], thus resulting in an overall pseudo-trigonal bipyramidal (or seesaw) (C,N)HgS2 core, with the nitrogen atom and the weekly bonded sulfur atom in equatorial positions [N(1)-Hg(1)?S(2a) 82.01(10)°]. 相似文献
8.
Benito Flores-Chávez José G. Alvarado-Rodríguez Noemí Andrade-López Verónica García-Montalvo Eliazar Aquino-Torres 《Polyhedron》2009
Treatment of RnGeCl4−n with {S(C6H3SH)2O} (1) afforded the stable phenoxathiin-4,6-dithiolate compounds [{S(C6H3S)2O}GeR2] [n = 2; R = Et (2), Ph (3)] and [{S(C6H3S)2O}GeRCl] [n = 1; R = Et (4), Ph (5)]. Treatment of GeCl4 with 1 in benzene afforded the dichloro compound [{S(C6H3S)2O}GeCl2] (8) at 7 °C. Bromo compounds [{S(C6H3S)2O}GeRBr] [R = Et (6), Ph (7)] and [{S(C6H3S)2O}GeBr2] (9) were synthesized by halogen exchange from the appropriate chloro derivative using KBr/HBr. X-ray structure determinations of diorganyl dithiolate compounds 2 and 3 revealed that germanium atom is contained in a boat–chair-shaped eight-membered central ring and displays a tetrahedral geometry. In contrast, compounds 4–6 display a boat–boat-shaped central ring with a significant intramolecular transannular O···Ge interaction. The geometry of the pentacoordinate Ge atom in these last complexes may be described as distorted trigonal bipyramidal with a 62–65% distortion displacement. 相似文献
9.
Wen-Yi Lee Jia-Wei Hsu Yu-Chun Lin Ting-Yu Lee 《Journal of organometallic chemistry》2011,696(23):3816-3821
A series of zirconium and hafnium alkoxide and amide complexes containing symmetrical tridentate pyrrolyl ligand, [C4H2NH(2,5-CH2NMe2)2] have been synthesized conveniently by treatment of 2,6-di-tert-butylphenol, tert-butanol or pyrrole in pentane and their reactivity over ring opening polymerization of ε-caprolactone have been carried out. Reactions of [C4H2NH(2,5-CH2NMe2)2] with M(NEt2)4 (M = Zr or Hf) originate [C4H2N(2,5-CH2NMe2)2]M(NEt2)3 (1, M = Zr; 2, M = Hf). Furthermore, reactions of [C4H2N(2,5-CH2NMe2)2]M(NEt2)3 with 2,6-di-tert-butylphenol, tert-butanol or pyrrole afford [C4H2N(2,5-CH2NMe2)2]M(OC6H3-2,6-tBu2)(NEt2)2 (3, M = Zr; 4, M = Hf), [C4H2N(2,5-CH2NMe2)2]M(OtBu)3 (5, M = Zr; 6, M = Hf) and [C4H2N(2,5-CH2NMe2)2]M(C4H4N)3 (7, M = Zr; 8, M = Hf), respectively, in satisfactory yield. All the complexes have been characterized by NMR spectra as well 3, 4 and 6 subjected to the X-ray diffraction analysis. Complexes 3-8 have been used as initiators for the ring-opening polymerization of ε-caprolactone and observed broad PDI values (1.84-2.75) representing multiple reactivity centers of these complexes. 相似文献
10.
Monika Kulcsar Cristian Silvestru John E. Drake Michael E. Hursthouse 《Journal of organometallic chemistry》2005,690(13):3217-3228
The cleavage of the Se-Se bond in [2-(Me2NCH2)C6H4]2Se2 (1) was achieved by treatment with SO2Cl2 (1:1 molar ratio) or elemental halogens to yield [2-(Me2NCH2)C6H4]SeX [X = Cl (2), Br (3), I (4)]. Oxidation of 1 with SO2Cl2 (1:3 molar ratio) gave [2-(Me2NCH2)C6H4]SeCl3 (5). [2-(Me2NCH2)C6H4]SeS(S)CNR2 [R = Me (6), Et (7)] were prepared by reacting [2-(Me2NCH2)C6H4]SeBr with Na[S2CNR2] · nH2O (R = Me, n = 2; R = Et, n = 3). The reaction of 3 with K[(SPMe2)(SPPh2)N] resulted in isolation of [2-(Me2NCH2)C6H4]Se-S-PMe2N-PPh2S (8). The compounds were characterized by solution NMR spectroscopy (1H, 13C, 31P, 77Se, 2D experiments). The solid-state molecular structures of 2, 4-8 were established by single crystal X-ray diffraction. All compounds are monomeric, with the N atom of the pendant CH2NMe2 arm involved in a three-center-four-electron N?Se-X (X = halogen, S) bond. This results in a T-shaped coordination geometry for the Se(II) atom in 2, 4, 6-8. In 5, the Se(IV) atom achieves a square pyramidal coordination in the mononuclear unit. Loosely connected dimers are formed through intermolecular Se?Cl interactions (3.40 Å); the overall coordination geometry being distorted octahedral. In all compounds hydrogen bonds involving halide or sulfur atoms generate supramolecular associations in crystals. 相似文献
11.
Grant D.W. Anderson Malcolm L.H. Green Ino C. Vei 《Journal of organometallic chemistry》2004,689(24):4407-4419
Reactions between [Fe(η-C5H5)(MeCO)(CO)(L)], L = PPh3 (1), PMe3 (2), PPhMe2 (3), PCy3 (4), CO (5), and B(C6F5)3 give new complexes [Fe(η-C5H5){MeCOB(C6F5)3}(CO)(L)] L = PPh3 (7), PMe3 (8), PPhMe2 (9), PCy3 (10), CO (11), where B(C6F5)3 coordinates selectively to the O-acyl groups. Hydrolysis of 7 gives [Fe(η-C5H5){HOB(C6F5)3}(CO)(PPh3)] (6). The X-ray structures of 6, 8 and 11 have been determined. Calculations, using density functional theory, demonstrate that the charge transfer to the acyl group on Lewis acid coordination is more significant in the σ than the π system. Both effects lead to a lengthening of the acyl C-O bond thus π populations cannot be inferred from the distance changes. 相似文献
12.
Robert K. Thomson 《Journal of organometallic chemistry》2011,696(25):3966-3973
Reaction of (C5Me5)2Lu(Me)(μ-Me)Li(THF)3 (2) with excess 12-crown-4 affords the new separated ion pair complex, [Li(12-crown-4)2][(C5Me5)2LuMe2] (3), in excellent yield. This complex reacts with 2,6-diisopropylaniline and phenylacetylene to give the methyl amide complex [Li(12-crown-4)2][(C5Me5)2Lu(Me)(NH-2,6-iPr2C6H3)] (4) and the bis(acetylide) complex [Li(12-crown-4)2][(C5Me5)2Lu(C≡C-Ph)2] (5), respectively. Attempts to promote methane loss from complexes 3 and 4 to generate a lutetium methylidene or imido complex, respectively, were unsuccessful. The ability of the bis(acetylide) complex 5 to act as a π-tweezer complex was also explored. Reaction between [Li(12-crown-4)2][(C5Me5)2Lu(C≡C-Ph)2] (5) and CuSPh gave only intractable lutetium products and the copper(I) species [Li(12-crown-4)2][Cu(C≡C-Ph)2] (8). The new lutetium complexes have been characterized by elemental analysis and NMR spectroscopy. Finally, the X-ray crystal structures of (C5Me5)2Lu(Me)(μ-Me)Li(THF)3 (2), [Li(12-crown-4)2][(C5Me5)2LuMe2] (3), [Li(12-crown-4)2][(C5Me5)2Lu(Me)(NH-2,6-iPr2C6H3)] (4), [Li(12-crown-4)2][(C5Me5)2Lu(C≡C-Ph)2] (5), and [Li(12-crown-4)2][Cu(C≡C-Ph)2] (8) are also reported. 相似文献
13.
Crystalline [Li{N(SiMe2OMe)C(tBu)C(H)(SiMe3)}]2 (5), [Li{N(SiMe2OMe)C(Ph)C(H)(SiMe3)}]2 (6), [C(C6H3Me2-2,5)C(H)(SiMe3)}(TMEDA)](7), [Li{N(SiMe(OMe)2)C(tBu)C(H)(SiMe3)}(THF)]2 (8), Li{N(SiMe(OMe)2)C(Ph)C(H)(SiMe3)}(TMEDA) (9) and [Li{N(SiMe2OMe)C(tBu)C(H)(SiMe2OMe)}]2 (10) were readily obtained at ambient temperature from (i) [Li{CH(SiMe3)(SiMe2OMe)}]8 (1) and an equivalent portion of RCN (R=tBu (5), Ph (6) or 2,5-Me2C6H3 (7)); (ii) [Li{CH(SiMe3)(SiMe(OMe)2)}]∞ (2) and an equivalent portion of tBuCN (8) or PhCN (9); and (iii) [Li{CH(SiMe2OMe)2}]∞ (3) and one equivalent of tBuCN (10). Reactions (i) and (ii) were regiospecific with SiMe3−n(OMe)n>SiMe3 in 1,3-migration from C (in 1 or 2)→N. The 1-azaallyl ligand was bound to the lithium atom as a terminally bound κ1-enamide (8 and 10), a bridging η3-1-azaallyl (6), or a bridging κ1-enamide (5). The stereochemistry about the CC bond was Z for 5, 8 and 10 and E for 7. X-ray data are provided for 5, 6, 7, 8 and 10 and multinuclear NMR spectra data in C6D6 or C6D5CD3 for each of 5-10. 相似文献
14.
H.J. Breunig T. Borrmann O. Moldovan R.P. Wagner 《Journal of organometallic chemistry》2009,694(3):427-91
Syntheses of [Me3SbM(CO)5] [M = Cr (1), W (2)], [Me3BiM(CO)5] [M = Cr (3), W (4)], cis-[(Me3Sb)2Mo(CO)4] (5), [tBu3BiFe(CO)4] (6), crystal structures of 1-6 and DFT studies of 1-4 are reported. 相似文献
15.
Lenka Dastychová Marie Sotolářová Dalibor Dastych Jan Taraba Marek Nečas Jiří Příhoda 《Polyhedron》2007
The reaction of P4S10 (1) with N,N′-diphenylurea (PhNH)2CO (2) results in new heterocyclic compounds: the pyridinium salt of 1,3-diphenyl-2-sulfido-2-thioxo-1,3-diaza-2λ5-phosphetidine (3) (with a P–N–C–N cycle) and the pyridinium salt of 1,4-diphenyl-2,5-disulfido-2,5-dithioxo-1,4-dithiadiaza-2λ5,5λ5-diphosphinane (4), containing the (P–S–N)2 cycle and the cyclic thiophosphates [pyH]2[P2S8] (5), [pyH]2[P2S7] (6) and [pyH]3[P3S9] (7). A similar reaction, but carried out with N,N′-diphenylthiourea (PhNH)2CS (8), leads to the formation of 4 and 6. pyPS2Cl (9), used as an alternative starting material, also yields compounds 3, 4, 5, and further [pyH][PS2Cl2] (10) and S8 after reaction with 2. Compound 3 reacts with Pd(CH3COO)2, with the formation of the complex [Pd(Ph2N2COPS2)2] (11). The crystal structures of 3 and 7 were determined by single-crystal X-ray diffraction. 相似文献
16.
The complexes of the type (ArCH2)2SnO were catalytic-oxygenated by Ag+ and yielded mixed-ligand organotin(IV) complexes (ArCH2)(2-C5H4NCO2)2(ArCOO)tin(IV) (Ar = C6H5 (1), 2-ClC6H4 (2), 2-CNC6H4 (3), 4-ClC6H4 (4), 4-CNC6H4 (5), 2-FC6H4 (6)). The complexes 1-6 are characterized by elemental analyses, IR and NMR (1H, 13C, 119Sn) spectroscopies. Single X-ray crystal structure analysis has been determined, which reveals that the center tin atom of complex 2 is seven-coordinated geometry. 相似文献
17.
Eight ionic organotin compounds [R2SnCl2(2-quin)]−(HNEt3)+ have been synthesized by reactions of 2-quinH with R2SnCl2 (R = PhCH21, 2-Cl-C6H4CH22, 4-Cl-C6H4CH23, 2-F-C6H4CH24, 4-F-C6H4CH25, 4-CN-C6H4CH26, Ph 7, 2,4-Cl2-C6H3CH28) in the presence of organic base NEt3, and their structures have been characterized by elemental analysis, IR and multinuclear NMR (1H, 13C, 119Sn) spectroscopies. The structure of [(2,4-Cl2-C6H3CH2)2SnCl2(2-quin)]−(NEt3)+ (8) has been determined by X-ray diffraction study. Studies show that compound 8 has a monomeric structure with the central tin atom six-coordinate in a distorted octahedral configuration and the nitrogen atoms of the 2-quin ligands are coordinating to the tin atom in all the eight compounds. 相似文献
18.
Sylvie Le Stang 《Journal of fluorine chemistry》2003,119(2):141-149
The aldehydic benzyl ethers PhCH2OC6H4CHO (2; a/b = para/meta series) are readily available from the corresponding phenols and react with Wittig reagents derived from [Ph3PCH2CH2Rf8]+I− (Rf8=(CF2)7CF3) to give PhCH2OC6H4CHCHCH2Rf8 (86-93%, Z major). Reactions with H2 over Pd/C give the fluorous phenols HOC6H4(CH2)3Rf8(4a,b; 87-91%). Condensations with PCl3 and NEt3 (3.0:1.0:3.3 mol ratio) give the fluorous phosphites P[OC6H4(CH2)3Rf8]3(5a,b; 92-94%), but traces of 4a,b are difficult to remove. The phthalate-based benzyl ethers PhCH2OC6H3(COOR)2 (7; ,5/3,4 OC6H3-3,n-(R)2 series) are easily accessed and reduced with LiAlH4 to the diols PhCH2OC6H3(CH2OH)2(8c,d; 89-90%). Diol 8c and the Dess-Martin periodinane react to give the dialdehyde PhCH2OC6H3(CHO)2 (9c; 95%). This is elaborated by a sequence analogous to 2→4→5 to the fluorous phenol HOC6H3((CH2)3Rf8)2 (11c; 97%/96%, two steps) and phosphite P[OC6H3((CH2)3Rf8)2]3 (12c, 92%), from which traces of 11c are difficult to remove. Diol 8d can be similarly elaborated to 11d, but the dialdehyde 9d is labile and the combined yield of the Dess-Martin/Wittig steps is 32%. The CF3C6F11/toluene partition coefficients of 11c,d, and 12c (two pony tails; 70:30, 72:28, 92:8) are much higher than those of 4a and b (one pony tail; 12:88, 14:86). 相似文献
19.
Lee D. Henderson 《Journal of organometallic chemistry》2007,692(21):4661-4668
The thermodynamics of ion pair symmetrization in a series of metallocenium species generated from were studied using a variety of solution dynamic techniques including line broadening, 2D-EXSY, and 1D-DPFGSE-NOE. Ion pairs were generated by methide abstraction using the corresponding trityl salts [1-A] to yield (A = {C6F4-1,2-[B(C6F5)2]2(μ-O(C6F5))}−, 2-O(C6F5); {C6F4-1,2-[B(C6F5)2]2(μ-OPh)}−, 2-OPh; {C6F4-1,2-[B(C6F5)2]2(μ-OMe)}−, 2-OMe; and [B(C6F5)4]−, 2-B(C6F5)4). The observed activation parameters were interpreted on the basis of a solvent-assisted mechanism of ion pair symmetrization. 相似文献
20.
Maribel Arroyo Sylvain Bernès Norma Calixto Carina Gómez 《Journal of fluorine chemistry》2006,127(1):22-28
A series of three new trithioether compounds containing fluorinated phenyl moieties, 1,3,5-(CH2SRf)3-2,4,6-(CH3)3C6, Rf = C6F5 (1), 4-HC6F4 (2), or 2-FC6H4 (3), were prepared by treatment of 1,3,5-(CH2Br)3-2,4,6-(CH3)3C6 with the corresponding Pb(SC6F5)2 or NaSRf. The new structures were verified by elemental analyses, IR, 1H NMR, 19F NMR spectroscopies, and mass spectra. The single crystal X-ray diffraction studies of 1-3 show a similar cis,trans,trans-conformation for the three fluorophenylthiomethyl groups attached to the central benzene ring with all dihedral angles between planes of central ring and external rings close to 0°, giving flat molecules. Comparing, 1-3 with closely related tripodal molecules built-up on 2,4,6-trimethylbenzene, arrangement of one SR group respect to others seems to be defined by the nature of the R substituent. Then in the case of 1-3, a parallel arrangement of rings is favored over an orthogonal one, which would bring the ortho-F atoms close to H atoms of the methylene groups. 相似文献