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1.
《结构化学》1990,(3)
<正> 2 - acetyldiferrocenylmethane, C5H5FeC5H4CH2C5H3 (COCH3) FeC5H5 ( I ),Mr=426. 1,violet-red prism-like crystal,m. p. 163. 7~166. 3℃,obtained from benzene-ligroin solution (benzene : ligroin=1 : 3). A crystal of approximate dimensions 0. 20×0. 40×0. 45 mm was selected for data collection from a CAD4 diffractometer with graphite monochromated MoKa radiation (λ=0. 71069A). Compound Ⅰ crystallized in the triclinic space group P1 with unit cell dimensions;a = 9. 597(2),b=9. 768 (2),c=11.540(1) A ,α= 111-93(1),β=111. 42(1),γ= 92. 46(2)°,V = 913. 9 A3, Z= 2, and Dc= 1. 548 g/cm3. 3' - Acetyldiferrocenylmethane, C5H5FeC5H4CH2C5H4FeC5 H4-COCH3(Ⅱ) ,is an isomer of compound Ⅰ ,yellow needle-like crystal,m. p. 110. 5~ 111. 0℃ ,obtained by the same method. A crystal of approximate dimensions 0. 025×0. 01×0. 45 mm was selected for data collection. Compound Ⅱ crystallized in monoclinic space group P21/c with a = 10. 930 (2), b= 5. 907(6) ,c= 27. 729(5) A ,β= 92. 64 (1)°,V=1788. 4A3,Z=4,Dc=1. 583 g/cm3. 相似文献
2.
<正> (C6H5COCHCOC6H5)SmI2(THF)3,Mr= 843. 75,triclinic space group P1,a=13. 274(3),b=9. 886(3),c= 12. 526(4)A,a= 110. 89(3),B=93. 98(2),y=85. 16(2) ,V=1528. 9(8)A3,Z=2,Dc=1. 83g/cm3, (MoKa) = 0. 71069A,u= 40. 3cm-1,F(000) - 810. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0.082(Rw= 0. 083). The central Sm(III) ion is coordinated by two iodine ions, two oxygen atoms from C6H5COCHCOC6H5 and three oxygen atoms from three THF molecules to form a distorted pentagonal bipyramid. The Sm-I distances are 3. 103 and 3. 092 A ,The Sm-O (O atom from C6H5COCHCOC6H5) distances are 2. 273 and 2. 307 A and the average Sm -O(THF) distance is 2. 500A. 相似文献
3.
Reaction of benzyl chloride with η5-CH3COC5H4W(CO)2Na formed in situ from η6-CH3CO C6H4Na and W(CO)2 gives η6-CH3COC6H4W(CO)3CH2C5H5.The single crystal structure of the product was determined by X-ray diffraction method. It crystallizes in the triclinlc space group P1 with unit cell parameters a= 10.199(5),b=12.116(7), c=14.207(6)A;a=69.47(5),β=72. 38(3),γ= 85.89(4);V= 1569. 9A3, Dc= 1.98 g/cm2; Z=4. Least-square refinement led to final R value of 0. 0539 and Rw value of 0. 0553, based on 3548 independent observed reflections. 相似文献
4.
《结构化学》1990,(3)
<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group. 相似文献
5.
《结构化学》1991,(3)
<正> [(C6H5)4P]Cu(S2C6H4)2(Ⅰ),Mr = 683. 39,monoclinic,space group C2/c,a=16. 099 (4),b= 11. 913(3) ,c = 16: 715(9) A ,β=97. 13(4)°, v = 3180. 7 A3,z=4.MoKa radiation,λ= 0. 71069A ,Dc= 1. 427g/cm3,μ= 10. 1cm-1,F(000) = 1400,R=0. 061 and Rw = 0. 068 for 2189 reflections with Ⅰ>3σ(Ⅰ). [(C6H5)4P]Cu (S2C7H6)2(Ⅰ),Mr = 711. 45,monoclinic,space group C2/c,a=16. 501(6),b = 37. 461 (15),c=16. 684(4)A,β=96. 70(4)°, v= 10248. 8(46) A3,z= 12. MoKa radiation, λ= 0. 71069A,Dc=1.383g/cm3,μ=9. 45cm-1,F(000).= 4416,R= 0. 074 and Rw= 0. 078 for 2085 reflections with I>2σ(I)(1). The copper atom in the complexes is surrounded by four sulfur atoms from two dithiolato ligands in an approximate, square-plane. The average Cu-S distances of the copmplexes(Ⅰ) and (Ⅱ) are 2. 179 and 2. 178 A, respectively. 相似文献
6.
《结构化学》1985,(1)
<正> The crystal and molecular structures of (C12H8N2)Mo(CO)4 and (C12H8N2)Cr(CO)4 are reported. They crystallize in the space group C2/m and are isomorphous with each other. The unit cell dimensions for (C12H8N2 Cr(CO)4 are a=15.404(2), b=12.091(2), c=8.223(2) A, 3=108.70(2)0, and V=1450.6(9) A3, while for (C12H8N2)Mo(CO)4 are a=15.546(6), b=12.086(4), c=8.269(1.) A, β= 107.37(2)0 and V=1482.9(l.5) A3, and both Z=4. Final R=0.040 Rw=0.050 for (C12H8N2)Cr(CO)4 and R=0.034 Rw=0.053 for (C12H8N2)Mo(CO)4. 相似文献
7.
The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a=15.359(2), b=18.378(3), c=24.952(2)(A), β=102.268(4)°, V=6882.3(16) (A)3, Mr=1348.34, Z=4, Dc=1.301 g/cm3, F(000)=2832 and μ= 0.424 mm-1. The final R=0.0606 and wR=0.1552 for 9396 observed reflections (Ⅰ > 2σ(Ⅰ)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) (A), indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed. 相似文献
8.
《结构化学》1992,(1)
<正> BrC6H4C2H2COC6H4OCH3, Mr = 317. 19, is monoclinic, space group PC with unit cell of a = 15. 869(3), b = 7. 146(2), c=5. 991(1) (?); β=82.85 (1)°; Z = 2, Dc=1. 56g/cm3; V = 674. 1(?)3; λ(MoKa) = 0. 71073A, μ= 30. 1 cm-1, F(000) = 320e, final R = 0. 040, Rw = 0. 041 for 993 observed reflections with I>3σ(I). As the two phenyl planes and the C2H2CO group are non-coplanar, the conjugated system was disturbed. This will produce a large hypsochromic shift of cutoff wavelength of transmission. 相似文献
9.
<正> By X-ray (λ=0. 71069A) diffraction of single crystal,we have determined the crystal structure of C6H5GdCl2 (THF)4,C22H37Cl2O4Gd, MT=593. 2,or-thorhombic space group Ccm2;with lattice parameters a=12. 776(6),b=12. 954(6), c=15. 802(3)A ;V=2615. 4(1. 8)A3;Z=4,Dc=2. 43gcm-3,μ=29. 3cm-1,F(000) = 1120. The structure was solved by heavy-atom method and Fourier techniques and refined by least-squares to a final R=0. 051 ,Rw = 0. 049 for 839 reflections with I≥1. 5σ (I). The results revealed that the bond length of Gd-C is 2. 437(22) A ,the average bond lengths of Gd-Cl 2. 678(6) A ,Gd-O 2. 499(12) A, C-C from phenyl group 1. 376(40)A. This crystal structure is the first organolanthanide complex with only one Ln-C bond in the molecule. 相似文献
10.
《结构化学》1993,(4)
<正> (CH3)4C2(C5H4)2Sm(C5H5)(OC4H8),Mr=499.4,orthorhom-bic,Cc2a,a=11.696(6),b=12.539(5),c=29.432(15)A,V=4316(4)A3,Z=8,Dc=1.54g/cm3,μ(MoKa)=27.8cm-1,F(000)=2024,R=0.077 for 1833 observed reflections.The samarium atom in the molecule is bonded to three cyclopen-tadienyl rings and one oxygen atom of tetrahydrofuran(THF)to form a tetrahedral configuration.The average Sm-C(η5-Cp)distances for the three cyclopentadienyl groups are 2.72(3),2.76(3)and 2.78(3)A,respectively,and the Sm-O bond is 2.53(1)A. 相似文献
11.
Miyasato M Sagami T Minoura M Yamamoto Y Akiba KY 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(10):2590-2600
A variety of hexaorganotellurium compounds, Ar(6-n)(CH3)nTe [Ar=4-CF3C6H4, n=0 (1a), n=1 (3a), n=2 (trans-4a and cis-4a), n=3 (mer-5a), n=4 (trans-6a); Ph, n=0 (1b), n=1 (3b), n=2 (trans-4b); 4-CH3C6H4, n=0 (1c), n=1 (3c), n=2 (trans-4c), n=4 (trans-6c); 4-BrC6H4, n=0 (1d)] and Ar5(R)Te [Ar=4-CF3C6H4, R=4-CH3OC6H4 (8); Ar=4-CF3C6H4, R=vinyl (9), Ar=Ph, R=vinyl (10), Ar=4-CF3C6H4, R=PhSCH2 (11), Ar=Ph, R=PhSCH2 (12), Ar=4-CF3C6H4, R=nBu (13)] and pentaorganotellurium halides, Ar5TeX [Ar=4-CF3C6H4, X=Cl (2a-Cl), X=Br (2a-Br); Ar=Ph, X=Cl (2b-Cl), X=Br (2b-Br); Ar=4-CH3C6H4, X=Cl (2c-Cl), X=Br (2c-Br); Ar=4-BrC6H4, X=Br (2d-Br)] and (4-CF3C6H4)4(CH3)TeX [X=Cl (trans-7a-Cl) and X=Br (trans-7a-Br)] were synthesized by the following methods: 1) one-pot synthesis of 1 a, 2) the reaction of SO2Cl2 or Br2 with Ar5Te(-)Li+ generated from TeCl4 or TeBr4 with five equivalents of ArLi, 3) reductive cleavage of Ar(6-m)(CH3)(m)Te (m=0 or 2) with KC8 followed by treatment with CH3I, 4) valence expansion reaction from low-valent tellurium compounds by treatment with KC8 followed by reaction with CH3I, 5) nucleophilic substitution of Ar(6-y-z)(CH3)zTeX(y-z) (X=Cl, Br, OTf; z=0, 1; y=1, 2) with organolithium reagents. The scope and limitations and some details for each method are discussed and electrophilic halogenation of the hexaorganotellurium compounds is also described. 相似文献
12.
YAO Tian-Ming YOU Xiao-ZengCoordination Chemistry Institute State Key Laboratory of Coordination Chemistry Nanjing University Nanjing ChinaYANG Qing-ChuanChemistry Department Beijing University Beijing China 《中国化学》1994,12(3):248-257
The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR s 相似文献
13.
Three unusual compounds based on polyoxometalate building blocks, [(H2O)5Na2(C6NO2H4)(C6NO2H5)3Ag2][Ag2IMo6O24(H2O)4] x 6.25H2O (1), [(H2O)4Na2(C6NO2H5)6Ag3][IMo6O24] x 6H2O (2), and (C6NO2H6)2[(C6NO2H5)2Ag][Cr(OH)6Mo6O18] x 4H2O (3), have been synthesized and characterized by elemental analysis; IR, XPS, and ESR spectroscopy; TG analysis; and single-crystal X-ray diffraction. Compound 1 is constructed from the cationic two-dimensional (2D) coordination polymer sheets which are constituted of [(H2O)5Na2(C6NO2H4)(C6NO2H5)3Ag2]3+ and anionic [Ag2IMo6O24(H2O)4]3- chains as pillars, forming a three-dimensional (3D) supramolecular framework via weak Ag-O interactions. Compound 2 is composed of the well-defined [IMo6O24]5- building blocks, which are linked through trinuclear Ag-pyridine-3-carboxylic acid, [(C6NO2H5)6Ag3]3+, fragments into a one-dimensional (1D) hybrid chain; adjacent chains are further connected by sodium cations to yield a novel 2D network. Compound 3 has a 1D chainlike structure constructed from [Cr(OH)6Mo6O18]3- building blocks and Ag-pyridine-4-carboxylic acid coordination units. The crystal data for these compounds are the following: 1, triclinic, P1, a = 13.280(3) A, b = 13.641(3) A, c = 16.356(3) A, alpha = 89.68(3) degrees, beta = 88.31(3) degrees, gamma = 75.87(3) degrees, Z = 2; 2, triclinic, P1, a = 11.978(2) A, b = 12.008(2) A, c = 13.607(3) A, alpha = 116.14(3) degrees, beta = 108.85(3) degrees, gamma = 93.86(3) degrees, Z = 1; 3, triclinic, P1, a = 10.458(2) A, b = 10.644(2) A, c = 12.295(3) A, alpha = 97.40(3) degrees, beta = 112.38(3) degrees, gamma = 113.59(3) degrees, Z = 1. 相似文献
14.
(C5H4CH3)3Ho和(C5H4CH3)2Ho(C5H5)与5-苯基四唑(HN4CPh)在THF中反应,得到复合产物[(C5H4CH3)2HoN4CPh]2·[(C5H4CH3)(C5H5)HoN4CPh]2,该晶体属三斜晶系,P1空间群,晶胞参数为a=9.386(3),b=13.071(3),c=16.571(2)A,a=86.90(1),β=74.61(2),γ=77.30(2)°,V=1912.2(8)A3,Z=1,Dc=1.602g/cm3,Mr=922.61,μ=41.92cm-1,F(000)=896,最终偏离因子R=0.041,Rw=0.056.晶体数据显示,在同一个晶胞里有两个组成不同的分子,每一个分子都是具有对称中心的四唑基桥二聚体结构,其桥环单元-HoN3HoN3-是平面型的。每个钬原子分别被两个茂基和3个四唑基氮原子配位,形成1个边桥变形四面体构型。 相似文献