Métodos de funcionalización de compuestos tipo pinza para- hidroxisustituidos

Esquema 58. Métodos de funcionalización de compuestos tipo pinza para-

Anexos

Anexos

Longitud de

enlace (Å) Ángulo (°)

Ni-Cl 2.2110(9) Cl Ni P1 99.25(3) Ni -P1 2.1844(7) Cl Ni P2 97.21(3) Ni -P2 2.1823(7) C2 Ni P1 81.49(6) Ni –C2 1.882(2) P2 Ni C2 82.06(6)

Anexos

Figura 43 Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 3a, las elipsoides son mostradas al 30%.

Longitud de

enlace (Å) Ángulo

(°) Ni-Cl 2.1853(16) Cl Ni P1 98.76(5) Ni -P1 2.1818(11) Cl Ni P2 96.82(5) Ni -P2 2.1720(11) C2 Ni P1 81.98(11) Ni-C2 1.878(4) P2 Ni C2 82.46(11)

Anexos

Longitud de

enlace (Å) Ángulo (°)

Ni-Cl1 2.1988(10) Cl1 Ni P1 98.05(3) Ni -P1 2.1757(8) Cl1 Ni P2 98.45(3) Ni -P2 2.1821(8) C2 Ni P1 81.76(8) Ni -C2 1.879(3) P2 Ni C2 81.81(8)

Figura 44. Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 9, las elipsoides son mostradas al 30%.

Anexos

Longitud de enlace (Å)

Àngulo (°)

Ni-Br1 2.304(3) Br1 Ni P1 98.12(7) Ni-Cl1 2.303(11) Br1 Ni P2 98.17(7) Ni -P1 2.1863(9)

Ni -P2 2.1854(8) C2 Ni P1 81.84(5) Ni –C2 1.8823(18) P2 Ni C2 81.92(5)

Figura 45. Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 10, las elipsoides son mostradas al 30%.

Anexos

Longitud de

enlace (Å) Àngulo (°)

Ni1-Br1 2.3210(12) Br1 Ni1P1 98.26(4) Ni1-Cl1 2.343(10) Br1 Ni1P2 97.97(4) Ni1 -P1 2.1909(8) C2 Ni1P1 81.61(8) Ni1-P2 2.1840(8) P2 Ni1C2 82.17(8) Ni1-C2 1.887(3)

Figura 46. Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 11, las elipsoides son mostradas al 30%.

Anexos

Longitud de

enlace (Å) Àngulo (°)

Ni-Cl1 2.1894(12) Cl1 Ni P1 97.62(4) Ni -P1 2.1868(10) Cl1 Ni P2 98.53(4) Ni -P2 2.1806(10) C2 Ni P1 81.62(11) Ni –C2 1.882(3) P2 Ni C2 82.30(11)

Figura 47. Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 13, las elipsoides son mostradas al 30%.

Anexos

Longitud de

enlace (Å) Àngulo (°)

Pd1-Cl1 2.306(3) Cl1Pd1P1 99.74(8) Pd1-P1 2.2612(18) Cl1Pd1P2 99.63(8) Pd1-P2 2.2716(19) C1Pd1P1 79.88(18)

Pd1-C1 1.973(7) P2Pd1C1 80.84(18)

Figura 48. Estructura molecular y valores de distancia y ángulos de enlace seleccionados del compuesto 14, las elipsoides son mostradas al 30%.

Anexos

Tabla 19. Datos cristalográficos de los compuestos 3a, 8, 9, 9', 10, 11, 13y 14.

3a 8 9 9' 10 11 13 14

Formula empírica

C22H39ClN iO3P2

C33H47ClFe NiO4P2

C31H47ClN iO3P2

C31H47ClNi O3P2, 0.5(C9H10O

) C25H43Br0.65Cl0.3 5NiO3P2

C25H41Br0.74Cl0.2 6NiO3P2

C25H38Cl3N3

NiO3P2

C25H38Cl3N3

O3P2Pd Peso

molecular

507.63

719.66 623.78 690.87 576.59 578.69 655.58 703.27

Temperat ura/K

298

298(2) 298(2) 298 298(2) 298(2) 298(2) 298(2)

Sistema cristalino

monoclínic

o monoclinic monoclínic

o triclínico triclínico monoclínico monoclínico monoclínico Grupo

espacial

P21/n

P21/c P21/n P-1 P-1 C2/c P21/n P21/n

a/Å 9.7190(1) 20.3566(5) 8.4358(3) 8.1630(4) 8.111(2) 32.7941(8) 8.0717(9) 8.1646(10) b/Å 20.1518(2) 10.8879(3) 19.0495(7) 14.8826(8) 13.123(4) 8.5806(2) 28.421(3) 28.713(4) c/Å 14.0221(1) 16.0417(4) 20.4390(7) 16.3974(9) 14.654(4) 25.0327(6) 13.6670(14) 13.7242(17)

α/° 90 90 90 102.301(1) 72.956(4) 90 90 90

β/°

103.238(1)

99.011(1) 90.406(1) 102.241(1) 88.668(5) 125.1748(10) 94.878(2) 95.542(2)

γ/° 90 90 90 97.727(1) 72.497(4) 90 90 90

Volumen/

ų 2673.33(4)

3511.61(16) 3284.4(2) 1868.12(17

) 1418.6(7) 5757.8(2) 3123.9(6) 3202.3(7)

Z 4 4 4 2 2 8 4 4

ρ calcg/cm 1.261

1.361 1.262 1.228 1.35 1.335 1.394 1.459

Anexos

μ/mm^-1 0.964 1.15 0.798 0.709 1.768 1.862 1.01 0.959

Continuación Tabla 20. Datos cristalográficos de los compuestos 3a, 8, 9, 9', 10, 11, 13y 14.

3a 8 9 9' 10 11 13 14

F(000) 1080 1512 1328 736 607 2427 1368 1440

Tamaño del cristal /mm³

0.10 x 0.11 x

0.40 0.28 × 0.22 ×

0.12 0.18 x 0.34

x 0.41 0.09 x 0.29 x 0.33

0.447 × 0.345 × 0.218

0.466 × 0.418 ×

0.320 0.04 x 0.14

x 0.27 0.03 x 0.13 x 0.44

Radiación MoKα (λ

= 0.71073) MoKα (λ =

0.71073) MoKa

0.71073 MoKa

0.71073 MoKα (λ =

0.71073) MoKα (λ =

0.71073) MoKα (λ =

0.71073) MoKα (λ = 0.71073) rango de 2Θ para

la colección/°

4.042 to

50.634 4.06 to 50.7 2.0, 25.3 1.7, 25.3 3.412 to

55.128 4.984 to

55.046 1.7, 25.4 2.1, 25.6

Index ranges

-11 ≤ h ≤ 11, -24 ≤ k

≤ 24, -16 ≤ l ≤ 16

-24 ≤ h ≤ 21, -12 ≤ k ≤ 13, -19 ≤ l ≤ 19

-10: 10 ; - 22: 22 ; -24:

24 -9: 9 ; -17:

17 ; -19: 19

-10 ≤ h ≤ 10, -17 ≤ k

≤ 16, -19 ≤ l ≤ 19

-37 ≤ h ≤ 42, -7 ≤ k ≤ 11, - 32 ≤ l ≤ 32

-9 ≤ h ≤ 9, - 34 ≤ k ≤ 34, - 16 ≤ l ≤ 16

-9 ≤ h ≤ 9, - 34 ≤ k ≤ 33, -15 ≤ l ≤ 16 Reflexiones

colectadas 24236

20422 32864 16358 19518 18956 25776 15756

Continuación Tabla 21. Datos cristalográficos de los compuestos 3a, 8, 9, 9', 10, 11, 13y 14.

Anexos

3a 8 9 9' 10 11 13 14

Reflexiones independientes

4872 [Rint = 0.0669, Rsigma =

0.0473] 6374 [Rint = 0.0382]

5992 [Rint = 0.0463, Rsigma = 0.0337]

6815 [Rint = 0.0331, Rsigma = 0.0456]

6536 [Rint = 0.0242, Rsigma = 0.0266]

6603 [Rint = 0.0559, Rsigma =

0.0592] 5717 [Rint = 0.0738]

5932, R(int)

=0.090 Datos/restriccione

s /parámetros

4872/1/27

7 6374/182/43

7 5992/40/37

4 6815/793/61

7 6536/24/33

2 6603/102/37

3 5717/192/39

6 5932/60/38

8

Goodness-of-fit

on F2 0.981

1.04 1.025 1.033 1.016 0.918 0.811 1.014

Final R indexes

R1 = 0.0335, wR2 = 0.0751

R1 = 0.0484, wR2 = 0.1170

R1 = 0.0391, wR2 = 0.0886

R1 = 0.0429, wR2 = 0.1082

R1 = 0.0281, wR2 = 0.0678

R1 = 0.0376, wR2 = 0.0855

R1 = 0.0445, wR2 = 0.0657

R1 = 0.0704, wR2 =

0.1594

Final R indexes [all data]

R1 = 0.0500, wR2 = 0.0828

R1 = 0.0787, wR2 = 0.1378

R1 = 0.0588, wR2 = 0.1015

R1 = 0.0623, wR2 = 0.1205

R1 = 0.0379, wR2 = 0.0726

R1 = 0.0638, wR2 = 0.0919

R1 = 0.0843, wR2 = 0.0729

R1 = 0.1339, wR2 =

0.1943 Largest diff.

peak/hole / e Å^-3

0.29/-0.33

0.67/-0.53 0.28/-0.29 0.57/-0.30 0.33/-0.25 0.66/-0.37 0.58/-0.32 0.67/-1.11

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