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含相当大体积三（吡唑基）硼氢配体的铜（I）配合物的合成与表征。探究由该配体形成的含金属口袋的灵活性。

Synthesis and Characterization of Copper(I) Complexes with a Fairly Bulky Tris(pyrazolyl)hydroborate Ligand. Probing the Flexibility of the Metal-Containing Pocket Formed by the Ligand.

作者信息

Conry Rebecca R., Ji Guanzhen, Tipton A. Alex

机构信息

Department of Chemistry/216, University of Nevada, Reno, Nevada, 89557.

出版信息

Inorg Chem. 1999 Mar 8;38(5):906-913. doi: 10.1021/ic980851w.

DOI:10.1021/ic980851w
PMID:11670862
Abstract

Four copper(I) tris(pyrazolyl)hydroborate complexes are reported with the fairly bulky tris[3-(p-tert-butylphenyl)-5-methylpyrazol-1-yl]hydroborate ligand (Tp()t(Bu-)(Ph,Me)). Tp()t(Bu-)(Ph,Me)Cu(CH(3)CN) (1) was synthesized from CuCl and Tp()t(Bu-)(Ph,Me)Li(CH(3)CN). The acetonitrile ligand in 1 was easily replaced by CO, PPh(3), and P(t)()Bu(3), forming Tp()t(Bu-)(Ph,Me)Cu(CO) (2), Tp()t(Bu-)(Ph,Me)Cu(PPh(3)) (3), and Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(3)) (4), respectively. Complexes 1-4 have been crystallographically characterized. 1.4CH(3)CN, 173 K: C(52)H(67)BCuN(11), triclinic, P&onemacr;, a = 13.4201(10) Å, b= 15.132(2) Å, c = 15.2125(13) Å, alpha = 60.743(6) degrees, beta = 73.211(4) degrees, gamma = 74.839(5) degrees, Z = 2, R1 = 6.81% (wR2 = 18.91%). 2, 296 K: C(43)H(52)BCuN(6)O, monoclinic, C2/c, a = 25.592(4) Å, b = 12.434(2) Å, c = 28.044(3) Å, beta = 104.073(9) degrees, Z = 8, R1 = 7.47% (wR2 = 22.08%). 3.CH(2)Cl(2), 173 K: C(61)H(69)BCl(2)CuN(6)P, triclinic, P&onemacr;, a= 12.5080(13) Å, b = 15.159(3) Å, c = 17.151(2) Å, alpha = 64.271(10) degrees, beta = 79.073(7) degrees, gamma = 86.572(8) degrees, Z = 2, R1 = 5.13% (wR2 = 13.28%). 4.0.5 hexane, 298 K: C(57)H(86)BCuN(6)P, triclinic, P&onemacr;, a = 13.337(2) Å, b = 13.435(2) Å, c = 17.386(2) Å, alpha = 88.371(7) degrees, beta = 71.863(8) degrees, gamma = 80.223(9) degrees, Z = 2, R1 = 6.96% (wR2 = 18.62%). The Tp()t(Bu-)(Ph,Me) ligands in 1, 2, and 3 bind in a tridentate fashion; the CH(3)CN and CO ligands fit comfortably within the pocket formed by the tert-butylphenyl substituents and the PPh(3) ligand interleaves between the pyrazole arms. The flexibility of the pocket was probed by calculating the area of the triangle created by connecting the midpoints of the 3-phenyl groups; this parameter increases by 15% for 3 (the largest) over 1 (the smallest). Thus, the pocket exhibits some flexibility, found to be due to both steric and electronic factors. Complex 4 features a bidentate Tp()t(Bu-)(Ph,Me) ligand as the P(t)()Bu(3) apparently exceeds the pocket's flexibility.

摘要

报道了四种含相当庞大的三[3-(对叔丁基苯基)-5-甲基吡唑-1-基]硼氢配体（Tp()t(Bu-)(Ph,Me)）的铜(I)配合物。Tp()t(Bu-)(Ph,Me)Cu(CH(3)CN)（1）由CuCl和Tp()t(Bu-)(Ph,Me)Li(CH(3)CN)合成。1中的乙腈配体很容易被CO、PPh(3)和P(t)()Bu(3)取代，分别形成Tp()t(Bu-)(Ph,Me)Cu(CO)（2）、Tp()t(Bu-)(Ph,Me)Cu(PPh(3))（3）和Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(3))（4）。配合物1 - 4已通过晶体学表征。1.4CH(3)CN，173 K：C(52)H(67)BCuN(11)，三斜晶系，P&onemacr;，a = 13.4201(10) Å，b = 15.132(2) Å，c = 15.2125(13) Å，α = 60.743(6)°，β = 73.2(2) Å，c = 28.044(3) Å，β = 104.073(9)°，Z = 8，R1 = 7.47%（wR2 = 22.08%）。3.CH(2)Cl(2)，173 K：C(61)H(69)BCl(2)CuN(6)P，三斜晶系，P&onemacr;，a = 12.508(CH(3)CN)（1）由CuCl和Tp()t(Bu-)(Ph,Me)Li(CH(3)CN)合成。1中的乙腈配体很容易被CO、PPh(3)和P(t)()Bu(3)取代，分别形成Tp()t(Bu-)(Ph,Me)Cu(CO)（2）、Tp()t(Bu-)(Ph,Me)Cu(PPh(3))（3）和Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(3))（4）。配合物1 - 4已通过晶体学表征。1.4CH(3)CN，173 K：C(52)H(67)BCuN(11)，三斜晶系，P&onemacr;，a = 13.4201(10) Å，b = 15.132(2) Å，c = 15.2125(13) Å，α = 60.743(6)°，β = 73.211(CH(3)CN)（1）由CuCl和Tp()t(Bu-)(Ph,Me)Li(CH(3)CN)合成。1中的乙腈配体很容易被CO、PPh(3)和P(t)()Bu(3)取代，分别形成Tp()t(Bu-)(Ph,Me)Cu(CO)（2）、Tp()t(Bu-)(Ph,Me)Cu(PPh(3))（3）和Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(3))（4）。配合物1 - 4已通过晶体学表征。1.4CH(3)CN，173 K：C(52)H(67)BCuN(11)，三斜晶系，P&onemacr;，a = 13.4201(10) Å，b = 15.132(2) Å，c = 15.2125(13) Å，α = 60.743(6)°，β = 73.211(4)°，γ = 74.839(5)°，Z = 2，R1 = 6.81%（wR2 = 18.91%）。2，296 K：C(43)H(52)BCuN(6)O，单斜晶系，C2/c，a = 25.592(4) Å，b = 12.434(2) Å，c = 28.044(3) Å，β = 104.073(9)°，Z = 8，R1 = 7.47%（wR2 = 22.08%）。3.CH(2)Cl(2)，173 K：C(61)H(69)BCl(2)CuN(6)P，三斜晶系，P&onemacr;，a =F1 = 7.47%（wR2 = 22.08%）。3.CH(2)Cl(2)，173 K：C(61)H(69)BCl(2)CuN(6)P，三斜晶系，P&onemacr;，a = 12.5080(13) Å，b = 15.159(3) Å，c = 17.151(2) Å，α = 64.271(10)°，β = 79.073(7)°，γ = 86.572(8)°，Z = 2，R1 = 5.13%（wR2 = 13.28%）。4.0.5己烷，298 K：C(57)H(86)BCuN(FF1 = 7.47%（wR2 = 22.08%）。3.CH(2)Cl(2)，173 K：C(61)H(69)BCl(2)CuN(6)P，三斜晶系, a = 12.5080(13) Å, b =CH(3)CN)（1）由CuCl和Tp()t(Bu-)(Ph,Me)Li(CH(3)CN)合成。1中的乙腈配体很容易被CO、PPh(3)和P(t)()Bu(3)取代，分别形成Tp()t(Bu-)(Ph,Me)Cu(CO)（2）、Tp()t(Bu-)(Ph,Me)Cu(PPh(3))（3）和Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(Ch,Me)Cu(CO)（2）、Tp()t(Bu-)(Ph,Me)Cu(PPh(3))（3）和Tp()t(Bu-)(Ph,Me)Cu(P(t)()Bu(3))（4）。配合物1 F1 = 7.47%（wR2 = 22.

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