Ligand-induced polyhedral opening in the mixed-metal cluster MeCCo2NiCp(CO)6 by 4,5-Bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray structure of Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2)

William H. Watson; Krzysztof Ejsmont; Jie Liu; Michael G. Richmond

首页> 外文期刊>Journal of Chemical Crystallography >Ligand-induced polyhedral opening in the mixed-metal cluster MeCCo2NiCp(CO)6 by 4,5-Bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray structure of Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2)

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Ligand-induced polyhedral opening in the mixed-metal cluster MeCCo2NiCp(CO)6 by 4,5-Bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray structure of Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2)

机译：4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮（bpcd）配体在混合金属簇MeCCo2 NiCp（CO）6 中诱导的多面体开口：X- Co2 NiCp（CO）4 [μ2，η2，η1 -C（Me）C = C（PPh2 ）的射线结构C（O）CH2 C（O）]（μ2 -PPh2 ）

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The mixed-metal cluster MeCCo2NiCp(CO)6 (1) reacts with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) in refluxing CH2Cl2 to afford the disubstituted cluster MeCCo2NiCp(CO)4(bpcd) (2), which exists as a 1:1 mixture of bridging and chelating bpcd isomers. VT 31P NMR spectroscopy confirms that the two bpcd isomers do not interconvert in solution over the temperature range of 182–298 K. Thermolysis of cluster 2 leads to bpcd/cluster activation and formation of the phosphido-bridged cluster Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2) (3). The ligand-induced polyhedral expansion that accompanies the formation of the title cluster was established by X-ray diffraction analysis. Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2) crystallizes in the triclinic space group P-1, a=9.679(2), b=11.691(2), c=16.653(3) Å, α=85.849(3)°, β=85.456(4)°, γ=66.453(3)°, V=1720.3(6) A3, Z=2, D cacl=1.632 Mg/m3; R=0.0874, R w=0.1998 for 7053 observed reflections with I > 2σ(I).

机译：混合金属簇MeCCo2 NiCp（CO）6 （1）在回流条件下与二膦配体4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮（bpcd）反应CH2 Cl2 提供二取代簇MeCCo2 NiCp（CO）4 （bpcd）（2），该化合物以1：1桥接和螯合bpcd异构体的混合物形式存在。 VT 31 P NMR光谱证实，在182–298 K的温度范围内，这两个bpcd异构体在溶液中不会互变。簇2的热解导致bpcd /簇活化，并形成了磷酸桥联簇Co2 NiCp（CO）4 [μ2，η2，η1 -C（Me）C = C（PPh2 ）C（O）CH2 C（O）]（μ2 -PPh2 ）（3）。通过X射线衍射分析确定了伴随标题簇形成的配体诱导的多面体膨胀。 Co2 NiCp（CO）4 [μ2，η2，η1 -C（Me）C = C（PPh2 ）C（O ）CH2 C（O）]（μ2 -PPh2 ）在三斜空间群P-1中结晶，a = 9.679（2），b = 11.691（2），c = 16.653（3）Å，α= 85.849（3）°，β= 85.456（4）°，γ= 66.453（3）°，V = 1720.3（6）A3 ，Z = 2，D cacl = 1.632 Mg / m3 ; R = 0.0874，R w = 0.1998，观察到了7053个I>2σ（I）的反射。

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《Journal of Chemical Crystallography》 |2006年第12期|823-830|共8页
作者
William H. Watson; Krzysztof Ejsmont; Jie Liu; Michael G. Richmond;
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Department of Chemistry Texas Christian University Fort Worth TX 76129 USA;

Department of Chemistry Texas Christian University Fort Worth TX 76129 USA;

Department of Chemistry University of North Texas Denton TX 76203 USA;

Department of Chemistry University of North Texas Denton TX 76203 USA;

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Tetrahedrane clusters; mixed-metal clusters; diphosphine ligand; CO substitution; polyhedral cluster opening; phosphido-bridged cluster;

机译：四面体簇;混合金属簇;二膦配体;CO取代;多面体簇开口;磷桥簇;

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外文文献

1. Ligand-induced polyhedral opening in the mixed-metal cluster MeCCo2NiCp(CO)(6) by 4,5-Bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray structure of Co2NiCp(CO)(4)[mu(2),eta(2),eta(1)-C(Me)C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) [J] . Watson WH, Ejsmont K, Liu J, Journal of chemical crystallography . 2006,第12期

机译：4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮（bpcd）引起的混合金属簇MeCCo2NiCp（CO）（6）中配体诱导的多面体开口：Co2NiCp（CO）的X射线结构（4）[mu（2），eta（2），eta（1）-C（Me）C = C（PPh2）C（O）CH2C（O）]（mu（2）-PPh2）
2. CO substitution in PhCCo3(CO)(9) by 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd). Ligand fluxionality, kinetics, and X-ray structures of PhCCo3(CO)(7)(bpcd) and Co-3(CO)(6)[mu(2)-eta(2),eta(1)-C(Ph)C=C(PPh2)C(O)CH2C(O)]-(mu(2)-PPh2) [J] . Bott SG., Richmond MG., Shen HF. Structural Chemistry . 2001,第3a4期

机译：PhCCo3（CO）（9）中的CO被4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮（bpcd）取代。 PhCCo3（CO）（7）（bpcd）和Co-3（CO）（6）[mu（2）-eta（2），eta（1）-C（Ph）的配体通量，动力学和X射线结构）C = C（PPh2）C（O）CH2C（O）]-（mu（2）-PPh2）
3. CO Substitution and Cluster-Ligand Reductive Coupling in the Reaction of 2,3-Bis(diphenylphosphino)maleic Anhydride (bma) with the Mixed-metal Clusters PhCCo2MCp(CO)8 (where M = Cr, W): Synthesis and X-ray Diffraction Structures of the Phosphido-bridged Clusters Co2MCp(CO)5[μ2,η2,η1-C(Ph)C=C(PPh2)C(O)OC(O)](μ-PPh2) [J] . Weiqiang Zhang, William H. Watson, Michael G. Richmond Journal of Chemical Crystallography . 2008,第1期

机译：2,3-双（二苯基膦基）马来酸酐（bma）与混合金属簇PhCCo2 MCp（CO）8 （其中M = Cr）反应中的CO取代和簇配体还原偶联，W）：磷酸桥联簇Co2 MCp（CO）5 [μ2，η2，η1-的合成及X射线衍射结构C（Ph）C = C（PPh2 ）C（O）OC（O）]（μ-PPh2）
4. Substitution chemistry of the cobalt complexes R carbon cobalt(3) nonacarbonyl (R = hydrogen, formyl radical) with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): Syntheses, x-ray structures, and reactivity. [D] . Liu, Jie. 2001

机译：用二膦配体4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮（bpcd）取代钴络合物R的碳（9）碳羰基钴（R =氢，甲酰基）：合成，x射线结构和反应性。
5. Diphosphine Isomerization and C-H and P-C Bond Cleavage Reactivity in the Triosmium Cluster Os3(CO)10(bpcd): Kinetic and Isotope Data for Reversible Ortho Metalation and X-ray Structures of the Bridging and Chelating Isomers of Os3(CO)10(bpcd) and the Benzyne-Substituted Cluster HOs3(CO)8(m3-C6H4)m2, h1-PPhCdC(PPh2)C(O)CH2C(O) [O] . -1

机译：二膦异构化和CH和CH和PC粘合切割反应性在TrioSmium簇OS3（CO）10（BPCD）中：动力学和同位素数据，用于桥接的可逆正交和X射线结构和OS3（CO）10（BPCD）的螯合异构体（BPCD）和苯并替代的簇Hos3（CO）8（M3-C6H4）M2，H1-PPHCDC（PPH2）C（O）CH 2 C（O）

Ligand-induced polyhedral opening in the mixed-metal cluster MeCCo2NiCp(CO)6 by 4,5-Bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray structure of Co2NiCp(CO)4[μ2,η2,η1-C(Me)C=C(PPh2)C(O)CH2C(O)](μ2-PPh2)

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