共查询到20条相似文献,搜索用时 15 毫秒
1.
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
2.
Kazi A. Azam Anjoli R. Das Michael B. Hursthouse Shariff E. Kabir K. M. Abdul Malik 《Journal of chemical crystallography》1998,28(4):283-288
The reaction of [Os3(CO)10(MeCN)2] with 2-ethylpyridine at ambient temperature leads to the isolation of the cluster [(-H)Os3(CO)10(-2-N=CCH=CHCH=CC2H5)][3 (65% yield) which has been structurally characterized by crystallographic methods. The compound crystallizes in the triclinic space group
with a = 9.334(2), b = 9.918(2), c = 11.767(1) Å, = 92.13(2), = 99.93(1), = 99.88(2)°, V = 1054.7(3) Å3 and Z = 2. The same edge of the osmium triangle in the cluster is bridged by both the hydrido and the heterocyclic ligands, the latter through the nitrogen and the carbon atoms of the C=N bond. 相似文献
3.
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
4.
Chun-Gu Xia Simon G. Bott Michael G. Richmond 《Journal of chemical crystallography》2003,33(9):681-687
The triruthenium cluster ( -H)Ru3( 3–3-CHCHCMe)(CO)9 reacts with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) in the presence of Me3NO to afford ( -H)Ru3( 3– 3-CHCHCMe)(CO)7(bpcd) in moderate yield. This new cluster has been isolated and characterized in solution by IR and NMR (1H, 31P) spectroscopies, and the solid-state structure has been established by X-ray crystallography. ( -H)Ru3( 3– 3-CHCHCMe)(CO)7(bpcd) MeOH crystallizes in the triclinic space group P
, a = 11.2426(8) Å, b = 11.7141(8) Å, c = 16.195(1) Å, = 102.041(5)°, = 95.128(5)°, = 102.553(6)°, V = 2008.4(3) Å3, Z = 2, d
calc. = 1.733 g/cm3; R = 0.0488, R
w = 0.0546 for 2212 observed reflections with I > 3 (I). The X-ray structure reveals that the bpcd ligand is bound exclusively to the Ru3 core at the ruthenium center coordinated by the terminal CH unit of the -allylic 3– 3-CHCHCMe moiety. 相似文献
5.
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
6.
C. Niamh McMahon Julie A. Francis Andrew R. Barron 《Journal of chemical crystallography》1997,27(3):191-194
The crystal and molecular structure of [(tBu)2Al(μ-Cl)]2 has been determined. The bond lengths and geometry about aluminum are similar to that in [Me2Al(μ-Cl)]2 and [(Mes)2Al(μ-Cl)]2 suggesting that the geometry about the aluminum is defined by the steric repulsion between the alkyl groups on adjacent aluminum centers and not steric congestion between ligands on individual aluminum centers. Crystal data: Triclinic, $P\bar 1$ ,a=6.514(1),b=8.628(2),c-11.236(2)c=11.236(2) Å, α=102.05(3), β=105.32(3), γ=103.47(3)°,V=567.2(3) Å3,Z=1,R=0.063,R w =0.067. 相似文献
7.
Jakia Akter G.M. Golzar Hossain Shariff E. Kabir K.M. Abdul Malik 《Journal of chemical crystallography》2000,30(12):773-776
Decacarbonyl--hydrido--1,8-2-quinoline-triosmium crystallizes in the triclinic space group P
with a = 7.8551(6), b = 9.1283(8), c = 16.7915(8) Å, = 74.788(2), = 88.086(2), = 66.392(3)°, V = 1062.22(13)° Å3, T = 150 K, and Z = 2. The molecule consists of an Os3 triangle with the hydride and the heterocyclic ligand bridging the same Os—Os edge. The heterocyclic ligand is coordinated through the C(8) carbon and nitrogen atoms in a new -1,8-2-bonding mode. The Os—Os distances lie in the close range 2.8837(4)–2.9034(4) Å with an average value of 2.892(7) Å. 相似文献
8.
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
9.
Stefanus Otto 《Journal of chemical crystallography》2001,31(4):185-190
The chloro-bridged dimeric complex, trans-[Pd(-Cl)(CH3)(PPh2Fc)]2, was prepared by reaction of [Pd(Cl)(CH3)(COD)] (COD = cis,cis-1,5-cyclooctadiene) with 1 equivalent of PPh2Fc (PPh2Fc = ferrocenyldiphenylphosphine) in acetone medium. The complex was characterized by 1H and 31P NMR spectroscopy and a single crystal X-ray diffraction study revealed a trans geometry. The compound crystallizes in the triclinic space group P1, a = 11.476(2) Å, b = 14.059(3) Å, c = 14.658(3) Å and = 82.34(3)°, = 75.09(3)°, and = 68.48(3)° with Z = 2. Most important geometrical parameters include bond lengths Pd(1)–P(1) 2.2165(10), Pd(2)–P(2) 2.2290(10), Pd(1)–C(1) 2.157(3), Pd(2)–C(2) 2.079(4), Pd(1)–Cl(1) 2.4329(13), Pd(1)–Cl(2) 2.4106(11), Pd(2)–Cl(1) 2.4169(10), and Pd(2)–Cl(2) 2.4414(13) Å and bond angles P(1)–Pd(1)–C(1) 87.47(8), P(1)–Pd(1)–Cl(2) 176.88(4), C(1)–Pd(1)–Cl(1) 173.93(7), P(2)–Pd(2)–C(2) 89.03(11), P(2)–Pd(2)–Cl(1) 174.18(4), and C(2)–Pd(2)–Cl(2) 173.50(11)°. The effective and Tolman cone angles for P(1) were calculated as 170 and 167° and that for P(2) as 179 and 177°, respectively. 相似文献
10.
Kazi A. Azam Michael B. Hursthouse Shariff E. Kabir K.M. Abdul Malik M. Abdul Mottalib 《Journal of chemical crystallography》1999,29(7):813-818
Decacarbonyl--bis(diphenylphosphino)methane triosmium crystallizes in the monoclinic space group P21/c with a = 24.422(5), b = 12.381(2), c = 24.788(5) Å, = 103.69(3)°, V = 7282 (2) Å3, and Z = 8. The molecule consists of a triangular arrangement of osmium atoms with the organic ligand bridging two adjacent osmium atoms at equatorial sites. The Os—Os distances lie in the close range 2.8563(9)–2.8895(11) Å with an average value of 2.87(1) Å. 相似文献
11.
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
12.
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
13.
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
14.
Luigi Pietro Battaglia Anna Bonamartini Corradi Maria Antonietta Zoroddu 《Journal of chemical crystallography》1990,20(2):161-164
The synthesis, magnetic, and structural properties of the title compound are reported. The crystals are triclinic, space groupP¯1, witha=15.084(2),b=11.820(1),c=7.5253(7) Å, =71.50(1),=77.61(1), =68.68(1)° andZ=1; the structure was solved by Patterson and Fourier methods and refined toR 0.0351 for 4147 observed reflections. The content of the unit cell consists of a centrosymmetrical copper acetate-like molecule in which each copper can be described as square-pyramidally surrounded by four carboxylic oxygens in the basal plane [1.955(2)–1.970(2) Å], one methanolic oxygen in the apical site [2.206(2) Å] and a CuCu interaction of 2.612(5) Å at a sixth position of a distorted octahedron. The dimers are packed by means of hydrogen bonds formed between the methanolic OH group and the carboxylic O(2) atom of one adjacent complex and by normal Van der Waals contacts. The subnormal magnetic moment, characteristic of exchange interactions between the two copper(II) ions, and the energy of the d-d band observed are consistent with the reported dinuclear copper(II) acetate-like structure. 相似文献
15.
Gerard A. van Albada Nora Veldman Anthony L. Spek Jan Reedijk 《Journal of chemical crystallography》2000,30(1):69-72
The title compound, catena-[bis(azido-N)-copper(II)-(bis(2-benzimidazolyl)butane), [Cu(C18H18N4)(N3)2]n, was obtained from the reaction of the ligand bis(2-benzimidazolyl)butane and Cu(N3)2. The x-ray crystal structure is reported. The compound crystallizes in the monoclinic space group P21/c with a = 8.2524(10), b = 12.765(5), c = 9.1125(15) Å, = 106.423(12)°, Z = 2. The Cu(II) ions are square-planar coordinated with trans-oriented end-on binding azido ligands. The structure is a polynuclear chain with the benzimidazole bridging at each end. In addition a N(ligand)-H···N(azido) H-bridge [N(ligand)···N(azido) = 2.994(7) Å] is present, resulting in a pseudo 2-dimensional lattice. The characteristic azido infrared vibrations are found at 2060 and 2077 cm–1 (as(N3)) and 1284 and 1297 cm–1 ((N3)). 相似文献
16.
Alvin A. Holder Robert T. Stibrany Nadejda Bolotina Martin Hall Vince C.R. Payne Kristin Kirschbaum A. Alan Pinkerton Anthony M. Newton 《Journal of chemical crystallography》2004,34(6):383-386
The synthesis and molecular structure of the title compound, [(nitrito-O,O) (dpa)2Cu(II)] (NO2), 1, is reported. Compound 1 crystallized in the orthorhombic space group Pccn with a = 11.397(5) Å, b = 12.256(6) Å, c = 14.876(8) Å, and V = 2077.9(17) Å3 with Z = 4. The distorted octahedral copper(II) cations are linked through a hydrogen-bonded polymer network. The polymer network is formed through the amine N–H of the cations and hydrogen bonded to the N–HO nitrite anions. 相似文献
17.
Simon G. Bott Jian Cheng Wang Michael G. Richmond 《Journal of chemical crystallography》1999,29(5):587-595
Thermolysis of the cluster Ru3(CO)12 with the bis(phosphanyl)hydrazine ligand (MeO)2PN (Me)N(Me)P(OMe)2 (dmpdmh) in toluene at 75°C furnishes the known clusters Ru4(CO)12 [-N(Me)N(Me)] (2) and Ru3(CO)11[P(OMe)3] (3), in addition to the new cluster Ru3 (CO)10(dmpdmh) (1) and the phosphite-tethered cluster Ru3(CO)9[-P(OMe)3] (4). The simple substitution product Ru3(CO)10(dmpdmh), a logical intermediate to clusters 2–4, was synthesized by treating Ru3(CO)12 with Me3NO in CH2Cl2 at room temperature, and independent thermolysis reactions using cluster 1 was shown to yield clusters 2–4. The solid-state structure of clusters 2 and 4 were unequivocally established by X-ray diffraction analysis. Ru4(CO)12[-N(Me)N(Me)] crystallizes in the orthorhombic space group Pnna (#52), a = 12.913(1), b = 13.3238(6), c = 12.5690(8) Å, V = 2162.5(2) Å3, Z = 4, and d
calc = 2.452 g/cm3. Ru3(CO)9[-P(OMe)3] crystallizes in the triclinic space group P
a = 9.586(1), b = 14.354(1), c = 14.997(2) Å, = 89.82(1)°, = 98.36(1)°, = 92.010(8)°, V = 2040.4(4) Å3, Z = 4, and d
calc = 2.212 g/cm3. The coordination of the dimethylazo linkage to the four ruthenium atoms in 2 and the phosphorus atom and one of the oxygen atoms of the methoxy groups to the three ruthenium centers in 4 are confirmed by X-ray analysis. 相似文献
18.
L. Renee Olano Hien T. Tran Joel T. Mague D. Andrew Knight 《Journal of chemical crystallography》2003,33(5-6):497-501
The chiral, racemic, arene phosphonate complex, [t6-1,2-C6H4(OCH3t)(P(O)(OCH2CH3t)2)t] Cr(CO)3 (1), was prepared via the reaction of 1,2-C6H4(OCH3)(P(O)(OCH2CH3)2) with Cr(CO)6 in refluxing dioxane/THF. The title complex crystallized in P1 with the cell dimensions: a = 8.4893(4) Å, b = 11.0638(9) Å, c = 11.2135(8) Å, and = 62.151(8), = 105.154(5), = 112.426(6), giving a volume of 856.34(10) Å3. The conformation of 1 is described as eclipsed (E) in which the methoxy substituent eclipses a carbonyl ligand of the tripod, and the phosphonate substituent is staggered. 相似文献
19.
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
20.
The molecular structure of [(tBu)2Al(-OPh)]2 has been determined. The intramolecular steric interaction between the phenyl groups and thetert-butyl ligands results in the geometry about aluminum being significantly distorted from tetrahedral, with the AlC2 planes are pitched 62° with respect to the Al2O2 plane. The greater distortion from tetrahedral about aluminum, and the orientation of the phenoxide ring more nearly perpendicular to the M2O2 core as compared to that in [(tBu)2Ga(-OPh)]2 are all consistent with increasedtBu...Ph steric interaction as a consequence of the smaller M2O2 core for [(tBu)2Al(-OPh)]2. Crystal data: tetragonal, I41/acd,a=16.44(1),c=21.41(1) Å,V=5788(7) Å3,Z=8,R=0.047,R
w=0.045. 相似文献