共查询到20条相似文献,搜索用时 15 毫秒
1.
Mohammad R. Hasan Michael B. Hursthouse Shariff E. Kabir K.M. Abdul Malik Edward Rosenberg Tasneem A. Siddiquee 《Journal of chemical crystallography》1999,29(5):597-602
The reaction of [Ru3(CO)10(-dppm)] 1 with PPhCl2 in refluxing CHCl3 results in the isolation of [(-H)Ru3(CO)8(-Cl)(-dppm)] 3 in 10% yield. Compound 3, which has been structurally characterized by crystallographic methods, is also formed from the reaction of 1 with H2 in refluxing CCl4. The compound crystallizes in the monoclinic space group P21/c with a = 16.814(2), b = 18.7590(12), c = 11.486(2) Å, = 97.745(11)°, V = 3589.8(8) Å3, and Z = 4. The hydride and chloride ligands bridge the same edge of the triruthenium cluster as the dppm ligand. 相似文献
2.
William H. Watson Miguel A. Mendez-Rojas Yuxin Zhao Michael G. Richmond 《Journal of chemical crystallography》2003,33(10):765-774
Treatment of the azavinylidene-bridged cluster Ru3(-H)(-N=CPh2)(CO)10 (1) with the diphosphine ligand bis(dimethylphosphino)ethane (dmpe) gives Ru3( -H)(-N=CPh2)(CO)8(dmpe) (2) in moderate yield, while the ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) reacts with Ru3( -H)(-N=CPh2)(CO)10 in the presence of Me3NO to furnish Ru3( -H)(-N=CPh2)(CO)8(bpcd) (3) in low yield. Each new cluster has been isolated and characterized in solution by IR and NMR (1H and 31P) spectroscopies, and the coordination mode exhibited by the ancillary diphosphine ligand in 2 and 3 has been established by X-ray crystallography. Ru3( -H)(-N=CPh2)(CO)8(dmpe) crystallizes in the monoclinic space group P2(1)/c, a = 10.791(1) Å, b = 16.377(1) Å, c = 18.148(1) Å, = 96.675(2)°, V = 3185.3(4) Å3, Z = 4, D
cacl = 1.791 Mg/m3; R = 0.0360, R
w
= 0.0866 for 7522 observed reflections with I > 2(I). Ru3(-H)(-N=CPh2)(CO)8(bpcd) crystallizes, as the CH2Cl2 solvate, in the triclinic space group
, a = 11.956(1) Å, b = 14.228(1) Å, c = 31.409(3) Å, = 89.377(2)°, = 79.344(2)°, = 77.235(2)°, V = 5118.4(8) Å3, Z = 2, D
calc = 1.670 Mg/m3; R = 0.0557, R
w
= 0.1069 for 10977 observed reflections with I > 2(I). The structural details of clusters 2 and 3 are contrasted with Ru3(-H)(-N=CPh2)(CO)7(-dppm)(-dppm), which is the only known structurally characterized phosphine-substituted cluster of this genre. 相似文献
3.
Khandakar M. Hanif Mohammad S. Islam Shariff E. Kabir K. M. Abdul Malik Md. Arzu Miah Nathan Wakelin 《Journal of chemical crystallography》2003,33(11):859-865
Treatment of Ru3(CO)12 with 2-mercaptobenzothiazole at 68°C gave the known compound [(-H)Ru3(3-2-C7H4NS2)(CO)9] 1 and the new compound [(-H)2Ru3(-2-C
7H4NS2) (3-2-C7H4NS2)(CO)7] 2 in 15 and 10% yields respectively. Compound 2 has been characterized by elemental analysis, infrared, 1H NMR and mass spectroscopic data together with single crystal X-ray crystallography. It crystallizes in the monoclinic space group C2/c with a = 31.662(6), b = 14.577(3), c = 11.602(2) Å, = 104.15(3)°, Z = 8, and V = 5192.4(2) Å3. The compound consists of a Ru3 triangle with three different Ru-Ru bond lengths [2.75264, 2.79084, 2.97604 Å] and the two 2-mercaptobenzothiazole ligands are differently attached to the metal atoms. Compound 2 is also obtained by the reaction of 1 with excess 2-mercaptobenzothiazole at 68°C. 相似文献
4.
Michael P. Castellani William G. Smith Nimish G. Patel Simon G. Bott Michael G. Richmond 《Journal of chemical crystallography》1999,29(5):609-617
The reaction between the tricobalt cluster Co3(CO)9(3-CCl) (1) and AlCl3, followed by treatment with ethyl diazoacetate, N2CHCO2Et, affords a complex mixture of products in low yields. Column chromatography has allowed the isolation of the four cluster compounds Co3(CO)9(3-CH) (2), Co3(CO)9(3-CCO2Et) (3), Co3(CO)9(3-CCH2CO2Et) (4), and [Co3(CO)9(3-CCHCO2Et)]2 (5). Clusters 4 and 5 are new and have been fully characterized in solution by IR and 1H NMR spectroscopy. The molecular structures of clusters 3–5 have also been determined by single-crystal X-ray diffraction analysis. Co3(CO)9(3-CCO2Et) crystallizes in the triclinic space group P
, a = 8.8393(5), b = 14.727(1), c = 15.272(1) Å, = 93.361(6), = 105.509(5)°, = 100.336(6)°, V = 1872.6(2) Å3, Z = 4, and d
calc = 1.823 g/cm3. Co3(CO)9(3-CCH2CO2Et) crystallizes in the monoclinic space group P21/n, a = 9.3806(7), b = 9.2617(8), c = 22.455(2) Å, = 94.483(7)°, V = 1944.9(3) Å3, Z = 4, and d
calc = 1.803 g/cm3. [Co3(CO)9(3-CCHCO2Et)]2 crystallizes in the monoclinic space group C2/c, a = 21.585(2), b = 8.7977(7), c = 20.784(1) Å, = 104.807(6)°, V = 3815.8(5) Å3, Z = 4, and d
calc = 1.835 g/cm3. Plausible pathways leading to the formation of clusters 2,
4, and 5 are discussed. 相似文献
5.
Kazi A. Azam Mohitosh Bhowmick Golam Mohammad Golzar Hossain Shariff E. Kabir Kalipada Kundu Khalifa Mohammad Abdul Malik Salina Perven 《Journal of chemical crystallography》2001,31(1):63-68
Treatment of [Ru3(CO)10(-dppm)] (1) with the ditelluride Te2(C6H4OEt-4)2 in refluxing toluene afforded the new aryltellurol bridged complex [Ru2(CO)4(-TeC6H4OEt-4)2 (-dppm)] (2) together with three known complexes [Ru4(CO)8(-CO)(4-Te)2(-dppm)] (3), [Ru2(CO)6{-CH2PPh(C6H4)PPh}] (4), and [Ru2(CO)6{-C6H4PPh(CH2)PPh}] (5). All the four complexes were characterized by spectroscopic methods, including an X-ray structure determination for 5. Complex 5 crystallizes in the monoclinic space group P21/c with a = 13.650(2), b = 9.995(2), c = 18.929(3) Å, = 97.49(2)°, V = 2560.4(8) Å3, and Z = 4. In this complex the two ruthenium atoms are bridged by the phosphino-phosphide ligand C6H4PPh(CH2)PPh which is attached to one Ru by the C6H4 group and a P atom while to the other Ru by both the two P atoms. Both the ruthenium atoms show distorted octahedral geometry. The Ru—Ru bond length is 2.8719(7) Å. 相似文献
6.
William H. Watson Krzysztof Ejsmont Jie Liu Michael G. Richmond 《Journal of chemical crystallography》2003,33(10):775-785
The heterometallic complex CoRu(CO)7(μ-PPh2) (1) reacts with the diphosphine ligand (Z)-Ph2PCH=CHPPh2 under both thermolysis and Me3NO activation to furnish CoRu(CO)5[(Z)-Ph2PCH=CHPPh2](μ-PPh2) (2) in good yield. Treatment of 2 with dimethyl acetylenedicarboxylate (DMAD) at elevated temperature leads to the formal insertion of the DMAD ligand into the Co–phosphido bond and formation of the metallocyclic compound CoRu(CO)3(μ-CO)[(Z)-Ph2PCH=CHPPh2][μ,η3-Ph2PC(CO2Me)C(CO2Me)] (3) that contains a 5e? alkenylphosphine moiety. These new CoRu compounds have been isolated by chromatography and fully characterized in solution by IR and NMR (1H and 31P) spectroscopies, and the solid-state structures of both 2 and 3 have been determined by X-ray diffraction analysis. CoRu(CO)5[(Z)-Ph2PCH=CHPPh2](μ-PPh2) crystallizes in the monoclinic space group P2 1/n, a = 11.493(8), b = 20.24(1), c = 17.04(1) Å, β = 91.03(1)°, V = 3964(5) Å3, Z = 4, D calc = 1.477 Mg/m3; R = 0.0475, R w = 0.1054 for 5120 observed reflections with I > 2σ (I). CoRu(CO)3(μ-CO)(Z)-Ph2PCH=CHPPh2][μ,η3-Ph2PC(CO2Me)C(CO2Me)], as the CH2Cl2 solvate, crystallizes in monoclinic space group P2 1/c, a = 17.0307(9) Å, b = 11.2124(6) Å, c = 24.083(1) Å, β = 97.755(1)°, V = 4556.8(4) Å3, Z = 4, D calc = 1.579 Mg/m3; R = 0.0379, R w = 0.0609 for 10774 observed reflections with I > 2σ(I). The regioselective coordination of the (Z)-Ph2PCH=CHPPh2 ligand to the two equatorial sites of the ruthenium center in 2 and the presence of the metallocyclic alkenylphosphine ligand in 3 are confirmed by the structural studies. The regiochemistry found in the coordination of (Z)-Ph2PCH=CHPPh2 to 1 is contrasted with the related diphosphine ligands bma and bpcd, while the DMAD insertion reactivity with 2 is discussed relative to alkyne reactions reported for the parent compound CoRu(CO)7(μ-PPh2). 相似文献
7.
Arnold L. Rheingold Mark E. Fountain James R. Harper 《Journal of chemical crystallography》1987,17(1):121-126
The X-ray crystallographic structure determination of Mo2(CO)8[-As(C6F5)2]2 reveals that the compound crystallizes in the tetragonal space groupP421
c witha=14.915(3),c=16.732(3) Å,V=3722(1) Å3, andZ=4. Least-squares refinement based on 1474 independent observed data [(F
obs)3(F
obs)] resulted in a finalR value of 0.038. The Mo-Mo distance of 3.132(1) Å is longer than found in analogous phosphido-bridged molybdenum systems. The central Mo2As2 rhombus is nearly flat and the coordination geometry of the Mo atoms is essentially octahedral. An unusual staggering of the Mo(CO)4 groups by 15.8° and short intramolecular C6F5CO contacts support the presence of a strong steric interaction between the Mo(CO)4 and As(C6F5)2 groups. 相似文献
8.
Simon G. Bott Huafeng Shen Michael G. Richmond 《Journal of chemical crystallography》1998,28(5):385-399
Thermal and Me3NO-assisted activation of the donor–acceptor complex Ru2(CO)6(bpcd) (1) [where bpcd = 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione] with PMe3 or tBuNC affords the mono-substituted complexes Ru2(CO)5L(bpcd), as a result of regiospecific ligand attack at the diphosphine-substituted ruthenium center. Solution NMR measurements (1H and 31P) reveal that the PMe3 derivative exists as a noninterconverting mixture of axial (3a) and equatorial (3e) isomers, with the only the equatorial isomer being observed for Ru2(CO)5(tBuNC)(bpcd) (5). Near-UV irradiation of 1 in the presence of added ligand yields Ru2(CO)5L(bpcd), in addition to the known 2-phosphido complex Ru2(CO)6 [-C=C(PPh2)C(O)CH2C(O)](2-PPh2) (2) and the corresponding phosphido-substituted complexes Ru2(CO)5L[-{C =C(PPh2)C(O)CH2C}(O)]2-PPh2)[4 (L = PMe3); 6 (L = tBuNC)]. As with compounds 3a, 3e, and 5, both 4 and 6 exhibit ligand attachment at the diphosphine-substituted ruthenium center. The molecular structures of 3e, 4, 5, and 6 were determined by X-ray crystallography. 3e, as the 1/2 C6H6 solvate, crystallizes in the monoclinic space group C2/c: a = 40.573(3) Å, b = 10.2663(9) Å, c = 18.347(1) Å, = 95.371(6)°, V = 7609(1) Å3 and Z = 8; 4, crystallizes in the monoclinic space group P21/n: a = 10.8241(8) Å, b = 18.074(1) Å, c = 19.194(1) Å, = 96.968(6)°, V = 3727.3(5) Å3, and Z = 4; 5, as the 1/2CH2Cl2 solvate, crystallizes in the monoclinic space group C2/c: a = 40.955(3) Å, b = 9.7230(6) Å, c = 20.542(1) Å, = 106.596(5)°, V = 7839.2(9) Å3, and Z = 8; 6, as the 1/2C5H12 solvate, crystallizes in the monoclinic space group P21/c: a = 21.773(2) Å, b = 10.907(3) Å, c = 18.744(4) Å, = 114.68(1)°, V = 4045(1) Å3, and Z = 4. The site occupied by the PMe3 and tBuNC ligands in these compounds is discussed relative to the steric size/electronic properties of the ancillary ligand and its interaction with the bpcd ligand. 相似文献
9.
Manwarul Islam Caroline A. Johns Shariff E. Kabir Kalipada Kundu K.M. Abdul Malik S.M. Bashir Ullah 《Journal of chemical crystallography》1999,29(9):1001-1007
The dimeric complex [Mn2(-pyS)2(CO)6] (1) reacted with 2 M equivalents of both PPh3 and PHPh2 to give the respective monomeric phosphine complexes [Mn(pyS)(L)(CO)3][L = PPh3 (2) and PHPh2 (3)]; with 4 M equivalents of dppm, it yielded the complex [Mn(pyS)(1-dppm)2(CO)2](4). An X-ray structure determination of 4 shows that it crystallizes in the monoclinic space group P21/n with a = 11.027(3), b = 24.984(7), c = 18.379(5) Å, = 99.870(8)°, V = 4988(2) Å3, and Z = 4. The complex has an octahedral geometry with the chelating pyS ligand and two CO groups occupying the equatorial sites and the two monodentate dppm ligands lying in the trans positions. 相似文献
10.
Peter Johnston Louis Denner Charles F. Marais Jan C. A. Boeyens Neil J. Coville 《Journal of chemical crystallography》1988,18(4):403-428
The crystal and molecular structures of three derivatives of [(
5-C5H4Me)Fe(CO)(L)I] [L=2,6-Me2C6H3NC, P(OMe)3, and P(C6H11)3] have been determined. [(
5-C5H4Me)Fe(CO)(CNC6H3Me2-2,6)I] (1): Space groupP¯1,Z=2,a=13.193(7),b=8.183(5),c=7.465(4) Å,=95.13(5),=94.39(5), =91.09(5)°. [(
5-C5H4Me)Fe(CO)[P(OMe)3]I] (2): Space groupP21/c,Z=4,a=7.296(3),b=24.471(6),c=8.877(3) Å,=111.92(4)°. [(
5-C5H4Me)Fe(CO)[P(C6H11)3]I] (3): Space groupP21/c,Z=4,a=9.809(3),b=14.147(2),c=8.276(3) Å,=103.07(2)°. The structures were refined toR values of 0.045, 0.070, and 0.061, respectively. Disorder was observed in the P(OMe)3 ligands on2. Structural data for1 and3 reveal (i) a small movement of the Fe atom away from the ringC atom containing the methyl group, (ii) a larger movement of ring C atoms away from the ring least-squares plane for3 than for1, and (iii) a shift toward an allyl-ene bond length variation in the ring distances for3. Molecular mechanics calculations performed on2 produce a low-energy conformation similar to that found in the crystal structure determination of2 with an energy barrier to ring rotation of ±5 kcal mol–1. A correlation of the structural and molecular mechanics data with the nmr spectra of complexes1 to3 indicates that the steric influence ofL on the ring rotation could be due to ring distortion and/or interaction with the ring methyl group. 相似文献
11.
The crystal and molecular structure of [ZnCl2(N4-trzCH2COPh)2] (trz = 1,2,4-triazole) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 26.7892(4) Å, b = 4.9392(2) Å, c = 20.7872(1) Å, = 127.517 (1), and z = 4. The complex has C
2 symmetry. The coordination geometry of each Zn atom is distorted tetrahedral formed by two Cl atoms and two tertiary N atoms of the -(1,2,4-triazole-1-yl)-acetophenone ligands. The two equivalent Zn–Cl and Zn–N bonds form bond angles around the Zn(II) atom in the range 101.4(1)–120.8(1). C–H O intermolecular interactions link the molecules in infinite chains in the [101] direction. 相似文献
12.
Shishir Ghosh Shariff E. Kabir Mansura Khatun Daniel T. Haworth Sergey V. Lindeman Tasneem A. Siddiquee Dennis W. Bennett 《Journal of chemical crystallography》2009,39(9):632-637
Abstract The thermal reaction of [Os3(CO)10(μ-H)(μ-SN2C4H5)] (1) at 110 °C afforded the new compound [Os3(CO)9(μ-H)(μ
3-η
2-SN2C4H5)] (2) in 84% yield. Compound 2 exists as two isomers, which differ in the disposition of the bridging hydride ligand. Both of the isomers of 2 have been characterized by a combination of elemental analysis, infrared and 1H NMR spectroscopic data together with single crystal X-ray crystallography. The isomers crystallize together in the triclinic
space group P-1 with a = 10.4775(2), b = 13.3056(3), c = 15.0325(3) ?, α = 110.8890(10), β = 99.3880(10), γ = 96.1620(10)°, Z = 2 and V = 1900.31(7) ?3.
Index Abstract The synthesis and the molecular structures of the two isomers of [Os3(CO)9(μ-H)(μ
3-η
2-SN2C4H5)] are described. The isomers differ in the disposition of the hydride ligand.
相似文献
13.
William H. Watson Jie Liu Michael G. Richmond 《Journal of chemical crystallography》2005,35(3):249-258
The reaction of the terminal alkyne methyl propiolate with the heterometallic dimers CoRu(CO)7(μ-PPh2) (1) and CoRu(CO)5[(Z)-Ph2PCH=CHPPh2](μ-PPh2) (2) has been investigated at 65°C in toluene. In the reaction of 1, chromatographic purification afforded a minor band, from which the two species RuCo(CO)4(μ-CO)[μ-PPh2C(O)CHC(CO2Me)] and RuCo(CO)4(μ-CO)[μ-PPh2CHC(CO2Me)] were observed by 1H NMR spectroscopy, and one major band, whose 1H NMR spectrum revealed the presence of multiple species. The identity of one of the compounds in the major component has been established as that of CoRu(CO)4(μ-CO)[μ-PPh2C(O)CH(CCO2Me)C(O)CHC(CO2Me)] (3) by X-ray diffraction analysis. The solid-state structure of 3 confirms the double insertion of CO and head-to-head coupling of the methyl propiolate that accompanies the formation of this product. Compound 3 crystallizes in the triclinic space group P-1, a = 8.4035(4), b = 9.6721(5), c = 17.678(1) Å, α = 94.135(2), β = 103.318(2), γ = 101.336(2)°, V = 1360.5(1) Å3, Z = 2, D calc = 1.732 Mg/m3; R = 0.0300, R w = 0.0760 for 8630 reflections with I > 2σ(I). The ruthenium-bound diphosphine ligand in 2 exerts a controlling influence on the reaction with added alkyne insomuch as only the mono-insertion product CoRu(CO)3(μ-CO)[(Z)-Ph2PCH=CHPPh2][μ-PPh2C(O)C(CO2Me)CH] (4) is formed as a single regioisomer. The molecular structure of 4 was established by X-ray diffraction analysis and 4 was found to crystallize in the monoclinic space group P21/c, a = 19.483(7), b = 11.905(4), c = 20.131(7) Å, β = 110.455(6)°, V = 4375(3) Å3, Z = 4, D calc = 1.466 Mg/m3; R = 0.0961, R w = 0.1683 for 6262 reflections with I > 2σ(I). The reactivity of methyl propiolate with 1 and 2 is compared with the known reactivity that has been reported for other alkynes. 相似文献
14.
Daniel L. Reger Terri D. Wright Mark D. Smith Arnold L. Rheingold Brain Rhagitan 《Journal of chemical crystallography》2000,30(10):665-670
[HB(3,4,5-Me3pz)3]2Zn (1) and [H2B(3,4,5-Me3pz)2]Zn(-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2] (2) are present in equal amounts in a crystal in the triclinic space group, P-1 with a = 11.5924(11) Å, b = 12.7799(12) Å, c = 15.7317(14) Å = 107.905(2)° = 96.796(2)°, = 105.786(2)°, and Z = 1. The structure of 1 is a trigonally distorted octahedron and is very similar to the structure of [HB(3,5-Me2pz)3]2Zn showing that the introduction of the third methyl group on the pyrazolyl ring does not impact on structure. [H2B(pz)2]2Zn (3) is orthorhombic, Pca2(1) with a = 10.1473(3) Å, b = 11.1117(2) Å, c = 14.1831(5) Å, = = = 90° and Z = 4. The zinc(II) centers in both 2 and 3 are similar and have pseudotetrahedral structures. 相似文献
15.
William H. Watson Srikanth Kandala Michael G. Richmond 《Journal of chemical crystallography》2006,36(12):813-822
The tetraruthenium cluster H4Ru4(CO)12 (1) has been studied for its reactivity with the unsaturated diphosphine ligands (Z)–Ph2PCH–CHPPh2 and 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) under thermal, near-UV photolysis, and Me3NO-assisted activation. All three cluster activation methods promote loss of CO and furnish the anticipated substitution products H4Ru4(CO)10[(Z)–Ph2PCH–CHPPh2] (2) and H4Ru4(CO)10(bpcd) (3) that possess a chelating diphosphine ligand. Clusters 2 and 3 have been characterized in solution by IR and NMR spectroscopies, and these data are discussed with respect to the crystallographically determined structure for both new cluster compounds. The 31P NMR spectral data and the solid-state structures confirm the presence of a chelating diphosphine ligand in clusters 2 and 3. Cluster 2 crystallizes in the monoclinic space P21/c, a=11.768(6) ?, b=18.521(9) ?, c=20.48(1) ?, β=102.291(8)°, V=4361(4) A3, Z=4, and d
calc=1.726 Mg/m3; R=0.0225, R
w=0.0491 for 6798 reflections with I > 2σ(I). The four bridging hydrides were located in H4Ru4(CO)10[(Z)–Ph2PCH–CHPPh2] and their adopted positions are discussed relative to the solution 1H NMR spectrum. H4Ru4(CO)10(bpcd) crystallizes in the orthorhombic space Pbca, a=19.072(3) ?, b=20.169(3) ?, c=22.774(3) ?, V=8760(2) A3, Z=8, and d
calc=1.870 Mg/m3; R=0.0428, R
w=0.0896 for 10296 reflections with I > 2σ(I). Sealed NMR tubes containing clusters 2 and 3 were found to be exceeding stable towards near-UV light and temperatures up to ca. 125 °C. The surprisingly robust behavior of 2 and 3 is contrasted with the related cluster Ru3(CO)10(bpcd) that undergoes fragmentation to the donor-acceptor compound Ru2(CO)6(bpcd) and the phosphido-bridged compound Ru2(CO)6(μ–PPh2)[μ–C–C(PPh2)C(O)CH2C(O)] under mild conditions. The electrochemical properties of each substituted cluster have been investigated by cyclic voltammetry, and our findings are discussed with respect to the reported electrochemical data on the parent cluster H4Ru4(CO)12.
相似文献
Michael G. Richmond (Corresponding author)Email: |
16.
Simon G. Bott Kaiyuan Yang Michael G. Richmond 《Journal of chemical crystallography》2004,34(2):127-133
Treatment of the diphosphine ligand 1,2-bis(diphenylphosphino)cyclobutenedione (bpcbd) with the THF adduct fac-BrRe(CO)3(THF)2 at room temperature furnishes the new dirhenium compound [BrRe(CO)3]2(bpcbd) instead of the expected mononuclear compound fac-BrRe(CO)3(bpcbd). [BrRe(CO)3]2(bpcbd) was characterized in solution by IR spectroscopy, and the solid-state structure was solved by X-ray crystallography. [BrRe(CO)3]2(bpcbd), as the CH2Cl2 solvate, crystallizes in the space group P
, a = 11.173(1), b = 13.362(1), c = 15.250(1) Å, = 108.973(7)°, = 99.477(8)°, = 110.466(7)°, V = 1915.0(3) Å3, Z = 2, and d
calc = 2.143 g-cm–3. The structure of [BrRe(CO)3]2(bpcbd) consists of two rhenium centers that are six-coordinate and possess nearly ideal octahedral geometry. The two Re(CO)3 units are linked together by the bridging diphosphine ligand and two bridging bromide groups. 相似文献
17.
Manwarul Islam Shariff E. Kabir Kalipada Kundu K.M. Abdual Malik S.M. Bashir Ullah 《Journal of chemical crystallography》2000,30(6):379-383
The dimeric complex [Mn2(-pyS)2(CO)6] (1) reacted with 2 molar equivalents of Ph2P(CH2)3PPh2 (dppp) and Ph2P(CH2)2PPh2 (dppe) to give the respective monomeric chelate complexes [Mn(2-pyS)(2-dppp)(CO)2] (2) and [Mn(2-pyS)(2-dppe)(CO)2] (3). In contrast, with 2 molar equivalents of Ph2P(CH2)5PPh2 (dpppe), 1 gave the highly insoluble polymeric complex [Mn(2-pyS)(-dpppe)(CO)2]n (4). An X-ray structure determination shows that 2 crystallizes in the monoclinic space group P21/n with a = 10.721(2) Å, b = 19.712(5) Å, c = 14.846(4) Å, = 109.06(2)°, V = 2965.5(14) Å3, and Z = 4. The complex has a distorted octahedral geometry with the dppp ligand, one CO group and the N atom of the chelating pyS ligand occupying equatorial sites, and one CO group and the S atom of the pyS ligand lying in the axial positions. 相似文献
18.
Luigi R. Nassimbeni Margaret L. Niven Johannes J. Cruywagen J. Bernard B. Heyns 《Journal of chemical crystallography》1987,17(3):373-382
The X-ray structure of the tetrameric complex [Mo4O11(C6H5O7)2]-(Me3N(CH2)6NMe3)2·12H2O has been determined. Crystals are monoclinic,C2/c, witha=19.886(8),b=11.773(6),c=26.97(1) Å,=90.69(4)°,V=6313 Å3,Z=4. FinalR=0.050,R
w
=0.053,w=(2
F)–1 for 4451 reflections withI
rel>2I
rel. The configuration of the Mo(VI) complex is similar to that previously reported for a Mo(VI)-malate anion [Mo4O11(mal)2]4– but differs from that proposed previously for a Mo(VI)-citrate complex. 相似文献
19.
Paul K. Baker Michael G.B. Drew Latifah A. Latif 《Journal of chemical crystallography》1999,29(8):907-911
The complex [WI(CO)(cis-dppen)(2-MeC2Me)2]I·CH2Cl2(1) is prepared as a by-product from the reaction of equimolar quantities of [WI2(CO)(NCMe)(2-MeC2Me)2] and cisdppen {dppen = bis(diphenylphosphino)ethene}. Complex 1, [WI(CO)(cis-dppen)(2-MeC2Me)2]I·CH2Cl2 crystallizes in the triclinic space group
with a = 11.189(13), b = 12.331(14), c = 15.395(17) Å, = 83.61(1), = 86.06(1), = 64.48(1)°, U = 1904 Å3, and Z = 2. The metal environment in the cation can best be considered as a distorted octahedron with the two but-2-yne groups taking up individual sites trans to phosphorus atoms of the dppen ligand. The coordination sphere is completed by mutually trans-carbonyl and iodide groups. 相似文献
20.
Ewa Gaŀdecka Zdzisŀaw Gaŀdecki Katarzyna Wajda-Hermanowicz Florian P. Pruchnik 《Journal of chemical crystallography》1995,25(11):717-723
The structure of the title tetranuclear cluster, C59H42N3O8P3Ir4, was determined by X-ray analysis. It crystallizes in the monoclinic space groupC2/c. The unit cell parameters are:a =47.277(6),b=10.519(3),c=23.025(4) Å, =105.77(1)°. The iridium atoms form a nearly regular tetrahedron. Between Ir4 and N336 atoms exists a relatively strong bond, thus one of the phosphine ligands is bridging one coordinatingvia P and N atoms. 相似文献