Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t)

Bott SG.; Richmond MG.; Shen HF.

首页> 外文期刊>Journal of chemical crystallography >Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t)

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Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t)

机译：区域特异性配体添加到供体-受体化合物Ru-2（CO）（6）（bpcd）：Ru-2（CO）（5）L（bpcd）和Ru-2（CO）的合成和X射线衍射结构（5）L [mu-C = C（PPh2）C（O）CH2C（O）]（mu（2）-PPh2）（其中L = PMe3和（BuNC）-Bu-t）

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Thermal and Me3NO-assisted activation of the donor-acceptor complex Ru-2(CO)(6)(bpcd) (1) [where bpcd = 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione] with PMe3 or (BuNC)-Bu-1 affords the mono-substituted complexes Ru-2(CO)(5)L(bpcd), as a result of regiospecific ligand attack at the diphosphine-substituted ruthenium center. Solution NMR measurements (H-1 and P-31) 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 Ru-2(CO)(5)((BuNC)-Bu-1)(bpcd) (5). Near-UV irradiation of 1 in the presence of added ligand yields Ru2(CO)SL(bpcd), in addition to the known mu(2)-phosphido complex Ru-2(CO)(6)[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (2) and the corresponding phosphido-substituted complexes Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) [4 (L = PMe3); 6 (L = (BuNC)-Bu-t)]. 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) Angstrom, b = 10.2663(9) Angstrom, c = 18.347(1) Angstrom, beta = 95.371(6)degrees, V = 7609(1) Angstrom(3) and Z = 8; 4, crystallizes in the monoclinic space group P2(1): a = 10.8241(8) Angstrom, b = 18.074(1) Angstrom, c = 19.194(1) Angstrom, beta = 96.968(6)degrees, V = 3727.3(5) Angstrom(3), and Z = 4; 5, as the 1/2CH(2)Cl(2) solvate, crystallizes in the monoclinic space group C2/c: a = 40.955(3) Angstrom, b = 9.7230(6) Angstrom, c = 20.542(1) Angstrom, beta = 106.596(5)degrees, V = 7839.2(9) Angstrom(3), and Z = 8; 6, as the 1/2C(5)H(12) solvate, crystallizes in the monoclinic space group P2(1)/c: a = 21.773(2) Angstrom, b = 10.907(3) Angstrom, c = 18.744(4) Angstrom, beta = 114.68(1)degrees, V = 4045(1) Angstrom(3), and Z = 4. The site occupied by the PMe3 and (BuNC)-Bu-1 ligands in these compounds is discussed relative to the steric size/electronic properties of the ancillary ligand and its interaction with the bpcd ligand. [References: 21]

机译：供体-受体复合物Ru-2（CO）（6）（bpcd）（1）的热和Me3NO辅助活化[其中，bpcd = 4,5-双（二苯基膦基）-4-环戊烯-1,3-二酮]与PMe3或（BuNC）-Bu-1配合使用时，由于在二膦取代的钌中心发生了区域特异性配体的攻击，因此提供了单取代的复合物Ru-2（CO）（5）L（bpcd）。溶液NMR测量（H-1和P-31）显示，PMe3衍生物以轴向（3a）和赤道（3e）异构体的非互变混合物形式存在，仅观察到Ru-2（CO）的赤道异构体（ 5）（（（BuNC）-Bu-1）（bpcd）（5）。除已知的mu（2）-磷复合物Ru-2（CO）（6）[mu-C = C（ PPh2）C（O）CH2C（O）]（mu（2）-PPh2）（2）和相应的磷取代的络合物Ru-2（CO）（5）L [mu-C = C（PPh2）C（ O）CH 2 C（O）]（mu（2）-PPh2）[4（L = PMe3）; 6（L =（BuNC）-Bu-t）]。与化合物3a，3e和5一样，4和6都在二膦取代的钌中心显示配体连接。通过X射线晶体学确定3e，4、5和6的分子结构。 3e作为1/2 C6H6的溶剂化物在单斜空间群C2 / c中结晶：a = 40.573（3）埃，b = 10.2663（9）埃，c = 18.347（1）埃，beta = 95.371（6）度，V = 7609（1）埃（3），Z = 8; 4，在单斜空间群P2（1）/ n中结晶：a = 10.8241（8）埃，b = 18.074（1）埃，c = 19.194（1）埃，beta = 96.968（6）度，V = 3727.3 （5）埃（3），Z = 4;如图5所示，当1 / 2CH（2）Cl（2）溶剂化物在单斜空间群C2 / c中结晶时：a = 40.955（3）埃，b = 9.7230（6）埃，c = 20.542（1）埃， beta = 106.596（5）度，V = 7839.2（9）埃（3），Z = 8;如图6所示，当1 / 2C（5）H（12）溶剂化物在单斜空间群P2（1）/ c中结晶时：a = 21.773（2）埃，b = 10.907（3）埃，c = 18.744（4）），β= 114.68（1）度，V = 4045（1）埃（3），Z =4。讨论了这些化合物中由PMe3和（BuNC）-Bu-1配体占据的位点辅助配体的空间大小/电子性质及其与bpcd配体的相互作用。 [参考：21]

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《Journal of chemical crystallography》 |1998年第5期|共15页
作者
Bott SG.; Richmond MG.; Shen HF.;
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正文语种 eng
中图分类晶体学;
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Ruthenium compounds; Donor-acceptor complex; 2; 3-bis(diphenylphosphino)maleic anhydride bma; Molecular-orbital properties; Carbonyl-complexes; Cluster chemistry; Metal-carbonyls; Substitution; Bond; Reactivity;

机译：钌化合物;给体-受体配合物;2;3-双（二苯基膦基）马来酸酐bma;分子轨道性质;羰基配合物;簇化学;金属羰基;取代;键;反应性;

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1. Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t) [J] . Bott SG., Richmond MG., Shen HF. Journal of chemical crystallography . 1998,第5期

机译：区域特异性配体添加到供体-受体化合物Ru-2（CO）（6）（bpcd）：Ru-2（CO）（5）L（bpcd）和Ru-2（CO）的合成和X射线衍射结构（5）L [mu-C = C（PPh2）C（O）CH2C（O）]（mu（2）-PPh2）（其中L = PMe3和（BuNC）-Bu-t）
2. Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t) [J] . Bott SG., Richmond MG., Shen HF. Journal of chemical crystallography . 1998,第5期

机译：区域特异性配体添加到供体-受体化合物Ru-2（CO）（6）（bpcd）：Ru-2（CO）（5）L（bpcd）和Ru-2（CO）的合成和X射线衍射结构（5）L [mu-C = C（PPh2）C（O）CH2C（O）]（mu（2）-PPh2）（其中L = PMe3和（BuNC）-Bu-t）
3. Photochemically mediated alkyne metalation in the donor-acceptor complexes Ru-2(CO)(6)(mu-P-P) [where P-P = bpcd, (Z)-Ph2PCH=CHPPh2]. X-ray diffraction structure of the zwitterionic compound Ru-2(CO)(6)[mu-(Z)-MeO2CC=CCO2Me](mu-bpcd) [J] . Bott SG., Richmond MG., Shen HF. Inorganica Chimica Acta . 2000,第0期

机译：供体-受体配合物Ru-2（CO）（6）（mu-P-P）[其中P-P = bpcd，（Z）-Ph2PCH = CHPPh2]中的光化学介导的炔烃金属化。两性离子化合物Ru-2（CO）（6）[mu-（Z）-MeO2CC = CCO2Me]（mu-bpcd）的X射线衍射结构
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）
6. Chemistry of Polynuclear Metal Complexes with Bridging Carbene or Carbyne Ligands. Part 89. (1) Tetra- and Penta-nuclear Tungsten-Rhodium Complexes: Crystal Structures of (W3Rh2(mu-CO)2(mu-CMe)(mu-C(Me)C(O))(Mu-PPh2)2-(Mu3-CMe)(CO)2(eta- C5H5)3) and (W3Rh2(mu-CO)3(mu-CMe)(mu-C(Me)PPh2)(mu3-CMe)-(CO)2(mu-C5H5)3). [R] . Davies, S. J., Stone, F. G., Howard, J. A., 1989

机译：具有桥接卡宾或卡宾配体的多核金属配合物的化学。第89部分。（1）四核和五核钨铑配合物：（W3Rh2（mu-CO）2（mu-Cme）（μ-C（me）C（O））（mu-pph2）的晶体结构2-（mu3-Cme）（CO）2（eta-C5H5）3）和（W3Rh2（mu-CO）3（mu-Cme）（μ-C（me）pph2）（mu3-Cme） - （CO） 2（mU-C5H5）3）。

Regiospecific ligand addition to the donor-acceptor compound Ru-2(CO)(6)(bpcd): syntheses and X-ray diffraction structures of Ru-2(CO)(5)L(bpcd) and Ru-2(CO)(5)L[mu-C=C(PPh2)C(O)CH2C(O)](mu(2)-PPh2) (where L = PMe3 and (BuNC)-Bu-t)

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