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ANEXO II
DATOS CRISTALOGRÁFICOS (RAYOS X)
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Difracción de Rayos X del paladaciclo 7
Tabla 1. Datos del cristal y del refinamiento de la estructura para 25.
Fórmula empírica C26.50 H23 Cl N2 O6.50 Pd2 S2
Peso molecular 785.84
Temperatura 296(2) K
Longitud de onda 0.71073 Å
Sistema cristalino y Monoclinic
Grupo espacial C2/c
Dimensiones de la celda a = 23.0429(6) Å; α= 90°.
b = 19.2530(5) Å; β= 05.9220(10)°.
c = 15.1462(4) Å; γ = 90°.
Volumen 6461.7(3) Å3
Z 8
densidad calculada 1.616 Mg/m3
Coeficiente de absorción 1.366 mm-1
F(000) 3112
Tamaño del cristal (mm) 0.21 x 0.12 x 0.09 mm3
Rango de θ (°) 1.40 to 28.28°.
Índices h, k, l -30 ≤ h ≤ 30, -25 ≤ k ≤ 25, -20 ≤ l ≤ 20
Reflexiones recogidas 69707
Reflexiones observadas 8004 (R(int) = 0.0294)
Método de refinamiento Refinamiento por mínimos cuadrados con matriz completa
Datos/restricciones/parámetros 8004 / 0 / 364 Bondad de ajuste en F2 1.218
Factores finales de acuerdo [I>2σ(I)] R1 = 0.0322, wR2 = 0.1161 Factores de acuerdo (todos los
datos) R1 = 0.0466, wR2 = 0.1377
Mayor diferencia pico y agujero 1.575 and -0.706 e.Å-3
Tabla 2. Coordenadas atómicas (x 10^4) y parámetros de desplazamiento isotrópico equivalentes (Å^2 x 10^3) para 7. U(eq) está definido como un tercio de la traza del tensor Uij ortogonalizado.
x y z U(eq)
Pd(1) 1872(1) 1899(1) 7028(1) 37(1)
Pd(2) 2440(1) 757(1) 8394(1) 38(1)
S(1) 1180(1) 2534(1) 5077(1) 53(1)
S(2) 1709(1) -208(1) 6676(1) 50(1)
C(1) 2586(2) 1273(2) 5872(3) 53(1)
C(2) 2758(2) 1162(3) 5089(4) 64(1)
C(3) 2464(3) 1464(3) 4296(4) 67(1)
C(4) 1970(2) 1884(2) 4263(3) 60(1)
C(5) 1802(2) 1968(2) 5070(3) 46(1)
C(6) 760(2) 1899(2) 5524(3) 44(1)
C(7) 177(2) 1731(2) 5025(3) 54(1)
C(8) -139(2) 1270(3) 5412(4) 64(1)
C(9) 120(2) 1001(3) 6271(4) 60(1)
C(10) 701(2) 1186(2) 6763(3) 50(1)
C(11) 1030(2) 1640(2) 6380(2) 37(1)
C(12) 1544(2) 100(2) 9192(3) 44(1)
C(13) 1070(2) -323(2) 9232(3) 50(1)
C(14) 786(2) -731(2) 8484(3) 50(1)
C(15) 991(2) -709(2) 7708(3) 45(1)
C(16) 1472(2) -279(2) 7711(2) 38(1)
C(17) 2480(2) -446(2) 7188(3) 51(1)
C(18) 2724(3) -1003(3) 6856(5) 76(2)
C(19) 3321(3) -1145(3) 7256(7) 110(3)
C(20) 3664(3) -730(3) 7921(7) 101(3)
C(21) 3405(2) -168(3) 8222(5) 73(2)
C(22) 2807(2) -17(2) 7860(3) 43(1)
C(23) 3202(2) 1945(2) 8097(3) 47(1)
C(24) 3802(2) 2308(3) 8278(4) 70(1)
C(25) 1798(2) 1980(2) 8954(3) 47(1)
C(26) 1615(3) 2365(3) 9703(4) 71(1)
C(27) 10000 2692(8) 7500 280(19)
Cl(1) 9904(2) 3229(3) 6550(4) 252(3)
N(1) 2101(2) 1683(2) 5872(2) 45(1)
N(2) 1752(2) 131(2) 8429(2) 41(1)
O(1) 853(2) 2662(2) 4098(2) 80(1)
O(2) 1423(2) -793(2) 6071(2) 73(1)
O(3) 2755(1) 2258(2) 7626(2) 55(1)
O(4) 3196(1) 1347(2) 8430(2) 57(1)
O(5) 2140(2) 1483(2) 9184(2) 58(1)
O(6) 1585(2) 2188(2) 8150(2) 56(1)
O(7) 5000 2944(3) 7500 85(2)
Tabla 3. Longitudes de enlace (Å) y ángulos (º) para 7.
Pd(1)-C(11) 1.984(3) N(1)-C(1)-H(1) 119.2 Pd(1)-N(1) 2.006(3) C(3)-C(2)-C(1) 120.9(5) Pd(1)-O(6) 2.061(3) C(3)-C(2)-H(2) 119.5 Pd(1)-O(3) 2.105(3) C(1)-C(2)-H(2) 119.5
Pd(1)-Pd(2) 3.0557(4) C(2)-C(3)-C(4) 119.7(4) Pd(2)-C(22) 1.992(4) C(2)-C(3)-H(3) 120.2 Pd(2)-N(2) 2.005(3) C(4)-C(3)-H(3) 120.2 Pd(2)-O(4) 2.067(3) C(3)-C(4)-C(5) 117.4(5) Pd(2)-O(5) 2.077(3) C(3)-C(4)-H(4) 121.3
S(1)-O(1) 1.487(3) C(5)-C(4)-H(4) 121.3
S(1)-C(6) 1.802(4) N(1)-C(5)-C(4) 123.5(4) S(1)-C(5) 1.803(5) N(1)-C(5)-S(1) 117.0(3) S(2)-O(2) 1.487(3) C(4)-C(5)-S(1) 119.3(4) S(2)-C(17) 1.791(5) C(11)-C(6)-C(7) 123.4(4) S(2)-C(16) 1.801(4) C(11)-C(6)-S(1) 116.9(3) C(1)-C(2) 1.366(6) C(7)-C(6)-S(1) 119.5(3) C(1)-N(1) 1.368(6) C(8)-C(7)-C(6) 117.7(4)
C(1)-H(1) 0.9300 C(8)-C(7)-H(7) 121.2
C(2)-C(3) 1.340(8) C(6)-C(7)-H(7) 121.2
C(2)-H(2) 0.9300 C(9)-C(8)-C(7) 120.2(4)
C(3)-C(4) 1.385(8) C(9)-C(8)-H(8) 119.9
C(3)-H(3) 0.9300 C(7)-C(8)-H(8) 119.9
C(4)-C(5) 1.390(6) C(8)-C(9)-C(10) 121.1(4)
C(4)-H(4) 0.9300 C(8)-C(9)-H(9) 119.5
C(5)-N(1) 1.339(5) C(10)-C(9)-H(9) 119.5 C(6)-C(11) 1.370(5) C(11)-C(10)-C(9) 119.6(4) C(6)-C(7) 1.387(6) C(11)-C(10)-H(10) 120.2 C(7)-C(8) 1.378(7) C(9)-C(10)-H(10) 120.2 C(7)-H(7) 0.9300 C(6)-C(11)-C(10) 118.0(4) C(8)-C(9) 1.374(8) C(6)-C(11)-Pd(1) 120.3(3) C(8)-H(8) 0.9300 C(10)-C(11)-Pd(1) 121.7(3) C(9)-C(10) 1.388(6) N(2)-C(12)-C(13) 122.0(4)
C(9)-H(9) 0.9300 N(2)-C(12)-H(12) 119.0
C(10)-C(11) 1.384(5) C(13)-C(12)-H(12) 119.0 C(10)-H(10) 0.9300 C(12)-C(13)-C(14) 120.0(4) C(12)-N(2) 1.369(5) C(12)-C(13)-H(13) 120.0 C(12)-C(13) 1.376(6) C(14)-C(13)-H(13) 120.0 C(12)-H(12) 0.9300 C(15)-C(14)-C(13) 118.9(4) C(13)-C(14) 1.386(6) C(15)-C(14)-H(14) 120.5 C(13)-H(13) 0.9300 C(13)-C(14)-H(14) 120.5 C(14)-C(15) 1.382(6) C(16)-C(15)-C(14) 118.4(4) C(14)-H(14) 0.9300 C(16)-C(15)-H(15) 120.8 C(15)-C(16) 1.382(5) C(14)-C(15)-H(15) 120.8 C(15)-H(15) 0.9300 N(2)-C(16)-C(15) 123.8(3)
C(16)-N(2) 1.356(5) N(2)-C(16)-S(2) 117.6(3) C(17)-C(22) 1.365(6) C(15)-C(16)-S(2) 118.5(3) C(17)-C(18) 1.370(6) C(22)-C(17)-C(18) 123.3(5) C(18)-C(19) 1.371(10) C(22)-C(17)-S(2) 116.6(3) C(18)-H(18) 0.9300 C(18)-C(17)-S(2) 119.9(4) C(19)-C(20) 1.356(11) C(17)-C(18)-C(19) 117.1(6) C(19)-H(19) 0.9300 C(17)-C(18)-H(18) 121.4 C(20)-C(21) 1.374(8) C(19)-C(18)-H(18) 121.4 C(20)-H(20) 0.9300 C(20)-C(19)-C(18) 121.4(5) C(21)-C(22) 1.366(7) C(20)-C(19)-H(19) 119.3 C(21)-H(21) 0.9300 C(18)-C(19)-H(19) 119.3 C(23)-O(3) 1.236(5) C(19)-C(20)-C(21) 119.6(6) C(23)-O(4) 1.258(5) C(19)-C(20)-H(20) 120.2 C(23)-C(24) 1.505(6) C(21)-C(20)-H(20) 120.2 C(24)-H(24A) 0.9600 C(22)-C(21)-C(20) 121.0(6) C(24)-H(24B) 0.9600 C(22)-C(21)-H(21) 119.5 C(24)-H(24C) 0.9600 C(20)-C(21)-H(21) 119.5 C(25)-O(5) 1.228(5) C(17)-C(22)-C(21) 117.5(4) C(25)-O(6) 1.249(5) C(17)-C(22)-Pd(2) 123.0(3) C(25)-C(26) 1.508(6) C(21)-C(22)-Pd(2) 119.3(4) C(26)-H(26A) 0.9600 O(3)-C(23)-O(4) 125.4(4) C(26)-H(26B) 0.9600 O(3)-C(23)-C(24) 117.2(4) C(26)-H(26C) 0.9600 O(4)-C(23)-C(24) 117.5(4) C(27)-Cl(1)#1 1.736(10) C(23)-C(24)-H(24A) 109.5 C(27)-Cl(1) 1.736(10) C(23)-C(24)-H(24B) 109.5 C(27)-H(27A) 0.9700 H(24A)-C(24)-H(24B) 109.5 C(27)-H(27B) 0.9700 C(23)-C(24)-H(24C) 109.5 C(11)-Pd(1)-N(1) 88.40(14) H(24A)-C(24)-H(24C) 109.5 C(11)-Pd(1)-O(6) 89.10(14) H(24B)-C(24)-H(24C) 109.5 N(1)-Pd(1)-O(6) 174.83(14) O(5)-C(25)-O(6) 125.2(4) C(11)-Pd(1)-O(3) 174.33(13) O(5)-C(25)-C(26) 117.4(4) N(1)-Pd(1)-O(3) 89.36(13) O(6)-C(25)-C(26) 117.4(4) O(6)-Pd(1)-O(3) 92.71(13) C(25)-C(26)-H(26A) 109.5 C(11)-Pd(1)-Pd(2) 109.47(10) C(25)-C(26)-H(26B) 109.5 N(1)-Pd(1)-Pd(2) 105.98(10) H(26A)-C(26)-H(26B) 109.5 O(6)-Pd(1)-Pd(2) 79.13(9) C(25)-C(26)-H(26C) 109.5 O(3)-Pd(1)-Pd(2) 76.17(9) H(26A)-C(26)-H(26C) 109.5 C(22)-Pd(2)-N(2) 89.25(14) H(26B)-C(26)-H(26C) 109.5 C(22)-Pd(2)-O(4) 88.54(14) Cl(1)#1-C(27)-Cl(1) 106.9(9) N(2)-Pd(2)-O(4) 175.28(13) Cl(1)#1-C(27)-H(27A) 110.3
C(22)-Pd(2)-O(5) 169.30(15) Cl(1)-C(27)-H(27A) 110.3 N(2)-Pd(2)-O(5) 89.92(13) Cl(1)#1-C(27)-H(27B) 110.3 O(4)-Pd(2)-O(5) 91.48(13) Cl(1)-C(27)-H(27B) 110.3 C(22)-Pd(2)-Pd(1) 114.52(12) H(27A)-C(27)-H(27B) 108.6 N(2)-Pd(2)-Pd(1) 104.83(9) C(5)-N(1)-C(1) 117.0(4) O(4)-Pd(2)-Pd(1) 79.88(9) C(5)-N(1)-Pd(1) 120.9(3) O(5)-Pd(2)-Pd(1) 75.97(9) C(1)-N(1)-Pd(1) 122.0(3) O(1)-S(1)-C(6) 108.0(2) C(16)-N(2)-C(12) 116.9(3) O(1)-S(1)-C(5) 106.3(2) C(16)-N(2)-Pd(2) 122.3(3) C(6)-S(1)-C(5) 95.79(18) C(12)-N(2)-Pd(2) 120.8(3) O(2)-S(2)-C(17) 107.0(2) C(23)-O(3)-Pd(1) 129.9(3) O(2)-S(2)-C(16) 106.86(19) C(23)-O(4)-Pd(2) 126.4(3) C(17)-S(2)-C(16) 96.02(18) C(25)-O(5)-Pd(2) 130.6(3) C(2)-C(1)-N(1) 121.5(5) C(25)-O(6)-Pd(1) 126.1(3) C(2)-C(1)-H(1) 119.2
Tabla 4. Parámetros de desplazamiento anisotrópico (Å2 x 103) para 7. El factor exponencial del desplazamiento anisotrópico tiene la siguiente forma: -2 2 [ h2 a*2 U11 + ... + 2 h k a* b* U12 ].
U11 U22 U33 U23 U13 U12
Pd(1) 38(1) 38(1) 32(1) -1(1) 6(1) -4(1) Pd(2) 44(1) 31(1) 35(1) -3(1) 8(1) -4(1)
S(1) 60(1) 47(1) 45(1) 9(1) 3(1) -6(1)
S(2) 66(1) 50(1) 32(1) -3(1) 12(1) -10(1) C(1) 50(2) 50(2) 60(3) -8(2) 21(2) -8(2) C(2) 67(3) 60(3) 74(3) -16(2) 35(3) -9(2) C(3) 80(3) 71(3) 62(3) -26(2) 39(3) -32(3) C(4) 77(3) 66(3) 37(2) -10(2) 15(2) -37(2) C(5) 49(2) 48(2) 40(2) -2(2) 10(2) -19(2) C(6) 42(2) 46(2) 40(2) -1(2) 6(2) -1(2)
C(7) 42(2) 64(2) 48(2) -5(2) 1(2) 4(2)
C(8) 38(2) 81(3) 69(3) -15(3) 8(2) -10(2) C(9) 47(2) 64(3) 70(3) -5(2) 20(2) -13(2)
C(10) 46(2) 52(2) 52(2) -1(2) 14(2) -2(2) C(11) 34(2) 37(2) 39(2) -3(1) 8(1) -1(1) C(12) 52(2) 42(2) 38(2) -3(2) 14(2) 3(2)
C(13) 55(2) 51(2) 51(2) 5(2) 25(2) 5(2)
C(14) 43(2) 47(2) 61(3) 6(2) 16(2) -3(2) C(15) 42(2) 42(2) 48(2) -1(2) 5(2) -4(2)
C(16) 45(2) 35(2) 31(2) 1(1) 6(1) 1(1)
C(17) 64(3) 40(2) 56(2) -4(2) 30(2) -7(2) C(18) 94(4) 50(3) 98(4) -26(3) 53(3) -14(3) C(19) 97(5) 61(3) 191(9) -33(4) 73(6) 8(3) C(20) 63(4) 68(4) 173(8) -20(4) 32(4) 14(3) C(21) 53(3) 57(3) 108(5) -8(3) 23(3) 1(2)
C(22) 45(2) 33(2) 56(2) 0(2) 21(2) 1(1)
C(23) 47(2) 52(2) 41(2) -10(2) 10(2) -13(2) C(24) 52(3) 79(3) 75(3) -6(3) 13(2) -25(2) C(25) 52(2) 46(2) 44(2) -9(2) 16(2) -12(2) C(26) 89(4) 71(3) 58(3) -19(2) 30(3) 3(3) C(27) 260(30) 82(10) 600(60) 0 290(30) 0
Cl(1) 184(4) 231(4) 371(8) -107(5) 124(5) -101(4) N(1) 48(2) 45(2) 42(2) -6(1) 14(1) -13(1)
N(2) 49(2) 37(1) 36(2) 2(1) 9(1) 1(1)
O(1) 87(3) 86(3) 53(2) 28(2) -5(2) -8(2) O(2) 93(3) 81(2) 42(2) -22(2) 15(2) -29(2)
O(3) 50(2) 56(2) 53(2) 1(1) 3(1) -16(1)
O(4) 46(2) 49(2) 71(2) -3(1) 8(1) -11(1) O(5) 78(2) 46(2) 50(2) -10(1) 19(2) 0(2) O(6) 66(2) 61(2) 41(2) -8(1) 15(1) 4(2)
O(7) 79(4) 85(4) 83(4) 0 8(3) 0
Tabla 5. Coordenadas de átomos de hidrógeno ( x 104) y parámetros de desplazamiento isotrópico(Å2 x 103) para 7.
x y z U(eq)
H(1) 2802 1064 6416 63
H(2) 3085 874 5108 77
H(3) 2589 1392 3770 80
H(4) 1760 2102 3722 72
H(7) 6 1923 4449 64
H(8) -529 1140 5092 77
H(9) -98 690 6526 72
H(10) 868 1005 7348 59
H(12) 1727 373 9698 53
H(13) 940 -335 9762 60
H(14) 464 -1015 8504 60
H(15) 809 -977 7196 55
H(18) 2494 -1274 6379 91
H(19) 3495 -1533 7067 131
H(20) 4071 -827 8172 121
H(21) 3640 116 8680 87
H(24A) 3995 2177 7816 104
H(24B) 4052 2176 8871 104
H(24C) 3741 2801 8260 104
H(26A) 1674 2071 10232 106
H(26B) 1197 2493 9488 106
H(26C) 1857 2775 9865 106
H(27A) 9649 2398 7433 337
H(27B) 10351 2398 7567 337
Tabla 6. Torsión de ángulos (º) para 7.
C(11)-Pd(1)-Pd(2)-C(22) 85.93(16) N(1)-Pd(1)-Pd(2)-C(22) -8.12(15)
O(6)-Pd(1)-Pd(2)-C(22) 171.06(15) O(3)-Pd(1)-Pd(2)-C(22) -93.38(15) C(11)-Pd(1)-Pd(2)-N(2) -10.16(14) N(1)-Pd(1)-Pd(2)-N(2) -104.20(13) O(6)-Pd(1)-Pd(2)-N(2) 74.98(13) O(3)-Pd(1)-Pd(2)-N(2) 170.54(13) C(11)-Pd(1)-Pd(2)-O(4) 169.61(15) N(1)-Pd(1)-Pd(2)-O(4) 75.57(13) O(6)-Pd(1)-Pd(2)-O(4) -105.25(13) O(3)-Pd(1)-Pd(2)-O(4) -9.69(13) C(11)-Pd(1)-Pd(2)-O(5) -96.27(15) N(1)-Pd(1)-Pd(2)-O(5) 169.68(14) O(6)-Pd(1)-Pd(2)-O(5) -11.14(14) O(3)-Pd(1)-Pd(2)-O(5) 84.42(14) N(1)-C(1)-C(2)-C(3) 1.2(7) C(1)-C(2)-C(3)-C(4) -1.1(7) C(2)-C(3)-C(4)-C(5) -0.5(6) C(3)-C(4)-C(5)-N(1) 2.3(6) C(3)-C(4)-C(5)-S(1) 177.7(3) O(1)-S(1)-C(5)-N(1) -168.8(3) C(6)-S(1)-C(5)-N(1) -58.1(3) O(1)-S(1)-C(5)-C(4) 15.4(4) C(6)-S(1)-C(5)-C(4) 126.1(3) O(1)-S(1)-C(6)-C(11) 171.3(3) C(5)-S(1)-C(6)-C(11) 62.1(3) O(1)-S(1)-C(6)-C(7) -12.7(4) C(5)-S(1)-C(6)-C(7) -122.0(4) C(11)-C(6)-C(7)-C(8) -1.0(7) S(1)-C(6)-C(7)-C(8) -176.7(3) C(6)-C(7)-C(8)-C(9) 1.0(7) C(7)-C(8)-C(9)-C(10) 0.0(8) C(8)-C(9)-C(10)-C(11) -1.0(7) C(7)-C(6)-C(11)-C(10) 0.1(6) S(1)-C(6)-C(11)-C(10) 175.9(3) C(7)-C(6)-C(11)-Pd(1) 178.9(3) S(1)-C(6)-C(11)-Pd(1) -5.4(4) C(9)-C(10)-C(11)-C(6) 1.0(6) C(9)-C(10)-C(11)-Pd(1) -177.8(3) N(1)-Pd(1)-C(11)-C(6) -48.0(3) O(6)-Pd(1)-C(11)-C(6) 127.5(3)
O(3)-Pd(1)-C(11)-C(6) 18.8(15) Pd(2)-Pd(1)-C(11)-C(6) -154.4(3) N(1)-Pd(1)-C(11)-C(10) 130.8(3) O(6)-Pd(1)-C(11)-C(10) -53.8(3) O(3)-Pd(1)-C(11)-C(10) -162.5(12) Pd(2)-Pd(1)-C(11)-C(10) 24.4(3) N(2)-C(12)-C(13)-C(14) -0.5(6) C(12)-C(13)-C(14)-C(15) 0.6(6) C(13)-C(14)-C(15)-C(16) 0.0(6) C(14)-C(15)-C(16)-N(2) -0.8(6) C(14)-C(15)-C(16)-S(2) -176.2(3) O(2)-S(2)-C(16)-N(2) 169.5(3) C(17)-S(2)-C(16)-N(2) 59.7(3) O(2)-S(2)-C(16)-C(15) -14.8(4) C(17)-S(2)-C(16)-C(15) -124.7(3) O(2)-S(2)-C(17)-C(22) -172.1(3) C(16)-S(2)-C(17)-C(22) -62.4(3) O(2)-S(2)-C(17)-C(18) 12.6(4) C(16)-S(2)-C(17)-C(18) 122.3(4) C(22)-C(17)-C(18)-C(19) 2.9(8) S(2)-C(17)-C(18)-C(19) 177.8(5) C(17)-C(18)-C(19)-C(20) -3.2(12) C(18)-C(19)-C(20)-C(21) 1.9(13) C(19)-C(20)-C(21)-C(22) -0.1(12) C(18)-C(17)-C(22)-C(21) -1.2(7) S(2)-C(17)-C(22)-C(21) -176.3(4) C(18)-C(17)-C(22)-Pd(2) -176.2(4) S(2)-C(17)-C(22)-Pd(2) 8.7(5) C(20)-C(21)-C(22)-C(17) -0.2(8) C(20)-C(21)-C(22)-Pd(2) 175.0(6) N(2)-Pd(2)-C(22)-C(17) 42.7(3) O(4)-Pd(2)-C(22)-C(17) -141.4(4) O(5)-Pd(2)-C(22)-C(17) 128.3(7) Pd(1)-Pd(2)-C(22)-C(17) -63.3(4) N(2)-Pd(2)-C(22)-C(21) -132.2(4) O(4)-Pd(2)-C(22)-C(21) 43.7(4) O(5)-Pd(2)-C(22)-C(21) -46.6(9) Pd(1)-Pd(2)-C(22)-C(21) 121.8(4) C(4)-C(5)-N(1)-C(1) -2.2(5) S(1)-C(5)-N(1)-C(1) -177.8(3)
C(4)-C(5)-N(1)-Pd(1) 174.4(3) S(1)-C(5)-N(1)-Pd(1) -1.1(4) C(2)-C(1)-N(1)-C(5) 0.5(6) C(2)-C(1)-N(1)-Pd(1) -176.1(3) C(11)-Pd(1)-N(1)-C(5) 52.4(3) O(6)-Pd(1)-N(1)-C(5) -8.7(16) O(3)-Pd(1)-N(1)-C(5) -122.4(3) Pd(2)-Pd(1)-N(1)-C(5) 162.2(3) C(11)-Pd(1)-N(1)-C(1) -131.1(3) O(6)-Pd(1)-N(1)-C(1) 167.8(13) O(3)-Pd(1)-N(1)-C(1) 54.2(3) Pd(2)-Pd(1)-N(1)-C(1) -21.3(3) C(15)-C(16)-N(2)-C(12) 1.0(5) S(2)-C(16)-N(2)-C(12) 176.3(3) C(15)-C(16)-N(2)-Pd(2) -179.0(3) S(2)-C(16)-N(2)-Pd(2) -3.6(4) C(13)-C(12)-N(2)-C(16) -0.3(5) C(13)-C(12)-N(2)-Pd(2) 179.6(3) C(22)-Pd(2)-N(2)-C(16) -45.5(3) O(4)-Pd(2)-N(2)-C(16) -107.5(16) O(5)-Pd(2)-N(2)-C(16) 145.2(3) Pd(1)-Pd(2)-N(2)-C(16) 69.7(3) C(22)-Pd(2)-N(2)-C(12) 134.6(3) O(4)-Pd(2)-N(2)-C(12) 72.6(16) O(5)-Pd(2)-N(2)-C(12) -34.7(3) Pd(1)-Pd(2)-N(2)-C(12) -110.2(3) O(4)-C(23)-O(3)-Pd(1) -10.6(7) C(24)-C(23)-O(3)-Pd(1) 168.7(3) C(11)-Pd(1)-O(3)-C(23) -159.2(12) N(1)-Pd(1)-O(3)-C(23) -92.5(4) O(6)-Pd(1)-O(3)-C(23) 92.2(4) Pd(2)-Pd(1)-O(3)-C(23) 14.1(4) O(3)-C(23)-O(4)-Pd(2) -6.1(6) C(24)-C(23)-O(4)-Pd(2) 174.6(3) C(22)-Pd(2)-O(4)-C(23) 127.1(4) N(2)-Pd(2)-O(4)-C(23) -170.8(14) O(5)-Pd(2)-O(4)-C(23) -63.6(4) Pd(1)-Pd(2)-O(4)-C(23) 11.9(3) O(6)-C(25)-O(5)-Pd(2) -6.0(7) C(26)-C(25)-O(5)-Pd(2) 173.4(3)
C(22)-Pd(2)-O(5)-C(25) -177.5(7) N(2)-Pd(2)-O(5)-C(25) -92.0(4) O(4)-Pd(2)-O(5)-C(25) 92.5(4) Pd(1)-Pd(2)-O(5)-C(25) 13.4(4) O(5)-C(25)-O(6)-Pd(1) -13.2(6) C(26)-C(25)-O(6)-Pd(1) 167.4(3) C(11)-Pd(1)-O(6)-C(25) 126.4(4) N(1)-Pd(1)-O(6)-C(25) -172.4(13) O(3)-Pd(1)-O(6)-C(25) -58.9(4) Pd(2)-Pd(1)-O(6)-C(25) 16.4(3)
Difracción de Rayos X del paladaciclo 20a
Tabla 1. Datos del cristal y refinamiento de estructura para 20a
Fórmula empírica C19H24N2O6S
Peso molecular 408.46
Temperatura 298(2) K
Longitud de onda 1.54178 Å
Sistema cristalino y Ortorrómbico
Grupo espacial P212121
Dimensiones de la celda a = 9.8306(5) Å; α= 90°.
b = 24.3215(12) Å; β= 90°.
c = 17.0929(8) Å; γ = 90°.
Volumen 4086.8(3) Å3
Z 8
densidad calculada 1.328 mgm-3 Coeficiente de absorción 1.735 mm-1
F(000) 1728
Tamaño del cristal (mm) 0.15 x 0.10 x 0.08
Rango de θ (°) 3.63 a 66.56
Índices h, k, l -11 ≤ h ≤ 11, -19 ≤ k ≤ 15, -26 ≤ l ≤ 28 Reflexiones recogidas 19517
Reflexiones observadas 6646 (R(int) = 0.0551)
Método de refinamiento Refinamiento por mínimos cuadrados con matriz completa
Datos/restricciones/parámetros 6646 / 0 / 529 Bondad de ajuste en F2 1.042
Factores finales de acuerdo [I>2σ(I)] R1 = 0.0546, wR2 = 0.1401 Factores de acuerdo (todos los
datos) R1 = 0.0753, wR2 = 0.1548
Mayor diferencia pico y agujero 0.369 y -0.480 Å-3
Tabla 2. Coordenadas atómicas (x 104) y parámetros de desplazamiento isotrópico equivalentes (Å2 x 103) para 20a. U(eq) está definido como un tercio de la traza del tensor Uij ortogonalizado.
x y z U(eq)
S(1) 2120(1) 9912(1) 2169(1) 48(1)
O(1) 3236(4) 10448(2) 4939(1) 77(1)
O(2) 204(4) 12957(2) 5656(1) 89(1)
O(3) 2388(4) 8719(2) 3484(2) 96(1)
O(4) 4224(3) 9255(2) 3849(1) 65(1)
O(5) 825(3) 10058(2) 1912(1) 65(1)
O(6) 3265(3) 10364(2) 2019(1) 60(1)
N(1) 1898(3) 9991(2) 2823(1) 47(1)
N(2) 3749(4) 8701(2) 2171(2) 68(1)
C(1) 2561(4) 11149(3) 4904(2) 57(1)
C(2) 2631(5) 11727(3) 5306(2) 63(1)
C(3) 1924(5) 12420(3) 5241(2) 65(1)
C(4) 1098(5) 12533(3) 4798(2) 73(1)
C(5) 1052(5) 11938(3) 4397(2) 71(1)
C(6) 1772(4) 11258(2) 4431(2) 55(1)
C(7) 1745(4) 10655(2) 3978(2) 54(1)
C(8) 2967(5) 10722(2) 3589(2) 52(1)
C(9) 2962(6) 11468(2) 3262(2) 83(2)
C(10) 3045(4) 10008(2) 3202(2) 45(1)
C(11) 3153(4) 9248(2) 3515(2) 52(1)
C(12) 4381(5) 8588(3) 4212(2) 82(2)
C(13) 2500(4) 8908(2) 2045(2) 52(1)
C(14) 4076(5) 7942(3) 2122(2) 83(2)
C(15) 3135(6) 7398(3) 1955(2) 85(2)
C(16) 1850(6) 7614(3) 1838(2) 77(1)
C(17) 1506(5) 8388(3) 1878(2) 67(1)
C(18) 3949(7) 10284(3) 5436(2) 100(2)
C(19) 1321(7) 13653(3) 5637(3) 112(2)
S(1') 2258(1) 5077(1) 2136(1) 49(1)
O(1') 3288(4) 5473(2) 4922(1) 78(1)
O(2') 2320(4) 7968(2) 5697(1) 80(1)
O(3') 2087(4) 3844(2) 3397(2) 93(1)
O(4') 4004(3) 4198(2) 3815(1) 67(1)
O(5') 1195(3) 5488(2) 1859(1) 63(1)
O(6') 3649(3) 5257(2) 2002(1) 59(1)
N(1') 2057(3) 5216(2) 2784(1) 49(1)
N(2') 3085(5) 3568(2) 1991(2) 90(1)
C(1') 2694(4) 6194(2) 4903(2) 51(1)
C(2') 2815(4) 6751(2) 5318(2) 58(1)
C(3') 2151(4) 7456(3) 5268(2) 58(1)
C(4') 1360(5) 7613(3) 4823(2) 65(1)
C(5') 1279(4) 7054(3) 4401(2) 61(1)
C(6') 1939(4) 6348(2) 4429(2) 50(1)
C(7') 1880(4) 5771(2) 3964(2) 52(1)
C(8') 3186(4) 5760(2) 3609(2) 48(1)
C(9') 3446(5) 6531(2) 3325(2) 73(1)
C(10') 3147(4) 5085(2) 3183(2) 46(1)
C(11') 2987(5) 4301(2) 3465(2) 56(1)
C(12') 4001(6) 3498(3) 4154(2) 94(2)
C(13') 1985(4) 4057(2) 2023(2) 49(1)
C(14') 2765(6) 2760(3) 1931(2) 80(2)
C(15') 1420(5) 2530(3) 1917(2) 70(1)
C(16') 434(5) 3088(3) 1958(2) 71(1)
C(17') 701(3) 3851(2) 2007(2) 42(1)
C(18') 3979(7) 5259(3) 5410(3) 106(2)
C(19') 1543(7) 8667(3) 5692(3) 106(2)
Tabla 3. Longitudes de enlace (Å) y ángulos (º) para 20a.
S(1)-O(5) 1.440(3) C(7)-C(8)-C(10) 110.9(3)
S(1)-N(1) 1.610(3) C(9)-C(8)-H(8) 106(4)
S(1)-C(13) 1.782(4) C(7)-C(8)-H(8) 110(5)
O(1)-C(1) 1.373(5) C(10)-C(8)-H(8) 107(4) O(1)-C(18) 1.424(5) C(8)-C(9)-H(9A) 109.5
O(2)-C(3) 1.375(5) C(8)-C(9)-H(9B) 109.5
O(2)-C(19) 1.418(7) H(9A)-C(9)-H(9B) 109.5 O(3)-C(11) 1.178(5) C(8)-C(9)-H(9C) 109.5 O(4)-C(11) 1.329(5) H(9A)-C(9)-H(9C) 109.5 O(4)-C(12) 1.451(5) H(9B)-C(9)-H(9C) 109.5 N(1)-C(10) 1.457(4) N(1)-C(10)-C(11) 110.9(3)
N(1)-H(1) 0.8600 N(1)-C(10)-C(8) 111.3(3)
N(2)-C(13) 1.314(5) C(11)-C(10)-C(8) 112.1(3) N(2)-C(14) 1.341(6) N(1)-C(10)-H(10) 104(2) C(1)-C(2) 1.391(6) C(11)-C(10)-H(10) 111(2) C(1)-C(6) 1.399(6) C(8)-C(10)-H(10) 107(2) C(2)-C(3) 1.382(6) O(3)-C(11)-O(4) 123.5(4)
C(2)-H(2) 0.9300 O(3)-C(11)-C(10) 125.6(4)
C(3)-C(4) 1.364(6) O(4)-C(11)-C(10) 110.8(3) C(4)-C(5) 1.409(7) O(4)-C(12)-H(12A) 109.5
C(4)-H(4) 0.9300 O(4)-C(12)-H(12B) 109.5
C(5)-C(6) 1.363(6) H(12A)-C(12)-H(12B) 109.5
C(5)-H(5) 0.9300 O(4)-C(12)-H(12C) 109.5
C(6)-C(7) 1.509(6) H(12A)-C(12)-H(12C) 109.5 C(7)-C(8) 1.534(6) H(12B)-C(12)-H(12C) 109.5 C(7)-H(7A) 0.9700 N(2)-C(13)-C(17) 123.7(4)
C(7)-H(7B) 0.9700 N(2)-C(13)-S(1) 114.6(3)
C(8)-C(9) 1.502(6) C(17)-C(13)-S(1) 121.4(3) C(8)-C(10) 1.544(6) N(2)-C(14)-C(15) 121.4(5)
C(8)-H(8) 0.71(5) N(2)-C(14)-H(14) 119.3
C(9)-H(9A) 0.9600 C(15)-C(14)-H(14) 119.3 C(9)-H(9B) 0.9600 C(16)-C(15)-C(14) 120.6(5) C(9)-H(9C) 0.9600 C(16)-C(15)-H(15) 119.7 C(10)-C(11) 1.510(5) C(14)-C(15)-H(15) 119.7 C(10)-H(10) 0.99(4) C(15)-C(16)-C(17) 118.8(5) C(12)-H(12A) 0.9600 C(15)-C(16)-H(16) 120.6 C(12)-H(12B) 0.9600 C(17)-C(16)-H(16) 120.6 C(12)-H(12C) 0.9600 C(16)-C(17)-C(13) 117.9(5) C(13)-C(17) 1.383(6) C(16)-C(17)-H(17) 121.1 C(14)-C(15) 1.372(7) C(13)-C(17)-H(17) 121.1 C(14)-H(14) 0.9300 O(1)-C(18)-H(18A) 109.5 C(15)-C(16) 1.347(7) O(1)-C(18)-H(18B) 109.5 C(15)-H(15) 0.9300 H(18A)-C(18)-H(18B) 109.5
C(16)-C(17) 1.368(7) O(1)-C(18)-H(18C) 109.5 C(16)-H(16) 0.9300 H(18A)-C(18)-H(18C) 109.5 C(17)-H(17) 0.9300 H(18B)-C(18)-H(18C) 109.5 C(18)-H(18A) 0.9600 O(2)-C(19)-H(19A) 109.5 C(18)-H(18B) 0.9600 O(2)-C(19)-H(19B) 109.5 C(18)-H(18C) 0.9600 H(19A)-C(19)-H(19B) 109.5 C(19)-H(19A) 0.9600 O(2)-C(19)-H(19C) 109.5 C(19)-H(19B) 0.9600 H(19A)-C(19)-H(19C) 109.5 C(19)-H(19C) 0.9600 H(19B)-C(19)-H(19C) 109.5 S(1')-O(5') 1.428(3) O(5')-S(1')-O(6') 118.90(17) S(1')-O(6') 1.439(3) O(5')-S(1')-N(1') 107.49(18) S(1')-N(1') 1.607(3) O(6')-S(1')-N(1') 107.92(17) S(1')-C(13') 1.785(4) O(5')-S(1')-C(13') 107.30(17) O(1')-C(1') 1.364(5) O(6')-S(1')-C(13') 108.48(18) O(1')-C(18') 1.416(6) N(1')-S(1')-C(13') 106.07(17) O(2')-C(3') 1.373(5) C(1')-O(1')-C(18') 117.9(4) O(2')-C(19') 1.418(7) C(3')-O(2')-C(19') 117.8(4) O(3')-C(11') 1.192(5) C(11')-O(4')-C(12') 118.2(4) O(4')-C(11') 1.325(5) C(10')-N(1')-S(1') 122.5(2) O(4')-C(12') 1.453(5) C(10')-N(1')-H(1') 118.8 N(1')-C(10') 1.462(5) S(1')-N(1')-H(1') 118.8 N(1')-H(1') 0.8600 C(13')-N(2')-C(14') 115.1(4) N(2')-C(13') 1.370(5) O(1')-C(1')-C(2') 123.8(4) N(2')-C(14') 1.424(6) O(1')-C(1')-C(6') 115.3(3) C(1')-C(2') 1.393(5) C(2')-C(1')-C(6') 120.9(4) C(1')-C(6') 1.397(5) C(3')-C(2')-C(1') 119.6(4) C(2')-C(3') 1.376(6) C(3')-C(2')-H(2') 120.2 C(2')-H(2') 0.9300 C(1')-C(2')-H(2') 120.2 C(3')-C(4') 1.358(6) C(4')-C(3')-O(2') 123.2(4) C(4')-C(5') 1.406(6) C(4')-C(3')-C(2') 121.0(4) C(4')-H(4') 0.9300 O(2')-C(3')-C(2') 115.7(4) C(5')-C(6') 1.371(6) C(3')-C(4')-C(5') 118.6(4) C(5')-H(5') 0.9300 C(3')-C(4')-H(4') 120.7 C(6')-C(7') 1.502(5) C(5')-C(4')-H(4') 120.7 C(7')-C(8') 1.548(5) C(6')-C(5')-C(4') 122.4(4) C(7')-H(7'1) 0.9700 C(6')-C(5')-H(5') 118.8 C(7')-H(7'2) 0.9700 C(4')-C(5')-H(5') 118.8 C(8')-C(9') 1.509(6) C(5')-C(6')-C(1') 117.3(4) C(8')-C(10') 1.551(5) C(5')-C(6')-C(7') 121.5(4) C(8')-H(8') 0.93(5) C(1')-C(6')-C(7') 121.2(4)
C(9')-H(9'1) 0.9600 C(6')-C(7')-C(8') 113.3(3) C(9')-H(9'2) 0.9600 C(6')-C(7')-H(7'1) 108.9 C(9')-H(9'3) 0.9600 C(8')-C(7')-H(7'1) 108.9 C(10')-C(11') 1.515(6) C(6')-C(7')-H(7'2) 108.9 C(10')-H(10') 0.99(4) C(8')-C(7')-H(7'2) 108.9 C(12')-H(12D) 0.9600 H(7'1)-C(7')-H(7'2) 107.7 C(12')-H(12E) 0.9600 C(9')-C(8')-C(7') 112.7(4) C(12')-H(12F) 0.9600 C(9')-C(8')-C(10') 110.4(3) C(13')-C(17') 1.311(5) C(7')-C(8')-C(10') 111.1(3) C(14')-C(15') 1.379(7) C(9')-C(8')-H(8') 109(3) C(14')-H(14') 0.9300 C(7')-C(8')-H(8') 113(3) C(15')-C(16') 1.364(6) C(10')-C(8')-H(8') 100(3) C(15')-H(15') 0.9300 C(8')-C(9')-H(9'1) 109.5 C(16')-C(17') 1.335(6) C(8')-C(9')-H(9'2) 109.5 C(16')-H(16') 0.9300 H(9'1)-C(9')-H(9'2) 109.5 C(17')-H(17') 0.9300 C(8')-C(9')-H(9'3) 109.5 C(18')-H(18D) 0.9600 H(9'1)-C(9')-H(9'3) 109.5 C(18')-H(18E) 0.9600 H(9'2)-C(9')-H(9'3) 109.5 C(18')-H(18F) 0.9600 N(1')-C(10')-C(11') 111.1(3) C(19')-H(19D) 0.9600 N(1')-C(10')-C(8') 110.3(3) C(19')-H(19E) 0.9600 C(11')-C(10')-C(8') 110.9(3) C(19')-H(19F) 0.9600 N(1')-C(10')-H(10') 107(2) O(6)-S(1)-O(5) 119.82(17) C(11')-C(10')-H(10') 109(2) O(6)-S(1)-N(1) 108.58(17) C(8')-C(10')-H(10') 108(2) O(5)-S(1)-N(1) 107.09(16) O(3')-C(11')-O(4') 124.2(4) O(6)-S(1)-C(13) 108.37(18) O(3')-C(11')-C(10') 126.5(4) O(5)-S(1)-C(13) 106.14(18) O(4')-C(11')-C(10') 109.3(4) N(1)-S(1)-C(13) 106.04(18) O(4')-C(12')-H(12D) 109.5 C(1)-O(1)-C(18) 117.5(4) O(4')-C(12')-H(12E) 109.5 C(3)-O(2)-C(19) 117.8(4) H(12D)-C(12')-H(12E) 109.5 C(11)-O(4)-C(12) 116.6(3) O(4')-C(12')-H(12F) 109.5 C(10)-N(1)-S(1) 121.4(2) H(12D)-C(12')-H(12F) 109.5 C(10)-N(1)-H(1) 119.3 H(12E)-C(12')-H(12F) 109.5 S(1)-N(1)-H(1) 119.3 C(17')-C(13')-N(2') 126.4(4) C(13)-N(2)-C(14) 117.7(4) C(17')-C(13')-S(1') 114.3(3) O(1)-C(1)-C(2) 123.5(4) N(2')-C(13')-S(1') 119.1(3) O(1)-C(1)-C(6) 115.9(4) C(15')-C(14')-N(2') 119.4(4) C(2)-C(1)-C(6) 120.6(4) C(15')-C(14')-H(14') 120.3 C(3)-C(2)-C(1) 120.3(4) N(2')-C(14')-H(14') 120.3 C(3)-C(2)-H(2) 119.8 C(16')-C(15')-C(14') 118.7(4)
C(1)-C(2)-H(2) 119.8 C(16')-C(15')-H(15') 120.6 C(4)-C(3)-O(2) 124.2(4) C(14')-C(15')-H(15') 120.6 C(4)-C(3)-C(2) 120.6(4) C(17')-C(16')-C(15') 123.3(4) O(2)-C(3)-C(2) 115.2(4) C(17')-C(16')-H(16') 118.3 C(3)-C(4)-C(5) 117.6(4) C(15')-C(16')-H(16') 118.3 C(3)-C(4)-H(4) 121.2 C(13')-C(17')-C(16') 117.0(3) C(5)-C(4)-H(4) 121.2 C(13')-C(17')-H(17') 121.5 C(6)-C(5)-C(4) 123.8(4) C(16')-C(17')-H(17') 121.5 C(6)-C(5)-H(5) 118.1 O(1')-C(18')-H(18D) 109.5 C(4)-C(5)-H(5) 118.1 O(1')-C(18')-H(18E) 109.5 C(5)-C(6)-C(1) 116.8(4) H(18D)-C(18')-H(18E) 109.5 C(5)-C(6)-C(7) 122.0(4) O(1')-C(18')-H(18F) 109.5 C(1)-C(6)-C(7) 121.2(4) H(18D)-C(18')-H(18F) 109.5 C(6)-C(7)-C(8) 112.8(3) H(18E)-C(18')-H(18F) 109.5 C(6)-C(7)-H(7A) 109.0 O(2')-C(19')-H(19D) 109.5 C(8)-C(7)-H(7A) 109.0 O(2')-C(19')-H(19E) 109.5 C(6)-C(7)-H(7B) 109.0 H(19D)-C(19')-H(19E) 109.5 C(8)-C(7)-H(7B) 109.0 O(2')-C(19')-H(19F) 109.5 H(7A)-C(7)-H(7B) 107.8 H(19D)-C(19')-H(19F) 109.5 C(9)-C(8)-C(7) 112.8(4) H(19E)-C(19')-H(19F) 109.5 C(9)-C(8)-C(10) 110.4(4)
Tabla 4. Parámetros de desplazamiento anisotrópico (Å2 x 103) para 20a. El factor exponencial del desplazamiento anisotrópico tiene la siguiente forma: -2
2 [ h2 a*2 U11 + ... + 2 h k a* b* U12 ].
U11 U22 U33 U23 U13 U12
S(1) 41(1) 58(1) 46(1) 6(1) 1(1) 3(1)
O(1) 88(2) 84(2) 58(2) 0(2) -14(2) 25(2) O(2) 107(3) 94(2) 65(2) -25(2) 0(2) 2(2) O(3) 95(3) 73(2) 119(3) 29(2) -49(2) -28(2) O(4) 48(2) 74(2) 73(2) 20(2) -17(2) 1(1) O(5) 44(2) 98(2) 53(2) 9(2) -8(1) 19(2) O(6) 52(2) 63(2) 65(2) 13(1) 8(1) -4(1)
N(1) 33(1) 66(2) 42(2) -3(2) 0(1) 1(1)
N(2) 59(2) 64(2) 81(3) -6(2) -5(2) 14(2)
C(1) 50(2) 72(2) 48(2) 0(2) -1(2) 4(2)
C(2) 58(3) 82(3) 49(2) -7(2) -6(2) 2(2)
C(3) 59(3) 79(3) 55(2) -15(2) 4(2) -4(3) C(4) 73(3) 82(3) 63(3) -8(3) -2(2) 15(3) C(5) 70(3) 84(3) 59(3) -9(2) -13(2) 12(3)
C(6) 46(2) 68(2) 51(2) -4(2) 0(2) 2(2)
C(7) 45(2) 66(2) 50(2) -4(2) 0(2) -3(2) C(8) 44(3) 57(2) 54(2) -2(2) -3(2) -11(2) C(9) 116(4) 57(2) 76(3) 3(2) 12(3) -21(3) C(10) 34(2) 54(2) 48(2) 3(2) -1(2) -4(2) C(11) 40(2) 57(2) 59(2) 2(2) -7(2) -3(2) C(12) 78(3) 87(3) 83(4) 28(3) -16(3) 14(3) C(13) 43(2) 65(2) 48(2) -2(2) 0(2) 1(2) C(14) 86(4) 66(3) 96(4) -11(3) -8(3) 22(3) C(15) 117(5) 62(3) 76(3) -7(2) -7(3) 9(3) C(16) 90(4) 71(3) 70(3) -15(2) 1(3) -11(3) C(17) 66(3) 82(3) 53(3) -2(2) -6(2) -5(2) C(18) 116(5) 99(4) 86(4) 18(3) -54(4) 14(3) C(19) 139(6) 91(4) 105(5) -37(3) 10(4) 17(4) S(1') 39(1) 63(1) 46(1) -2(1) -2(1) -1(1) O(1') 99(2) 77(2) 59(2) 1(2) -9(2) 36(2) O(2') 85(2) 90(2) 66(2) -32(2) 6(2) -3(2) O(3') 94(3) 66(2) 118(3) 19(2) -32(2) -33(2) O(4') 58(2) 68(2) 74(2) 10(2) -12(2) 4(1) O(5') 49(2) 78(2) 63(2) 8(1) -15(1) 9(1) O(6') 39(1) 77(2) 63(2) 5(1) 6(1) -11(1) N(1') 38(2) 64(2) 45(2) -9(2) 1(1) 0(1) N(2') 85(3) 94(3) 92(3) -1(2) 3(3) 20(2) C(1') 45(2) 63(2) 46(2) -1(2) 1(2) 7(2) C(2') 51(2) 74(3) 47(2) -6(2) -2(2) 1(2) C(3') 52(2) 66(2) 54(2) -14(2) 11(2) -9(2) C(4') 68(3) 57(3) 71(3) -1(2) 6(2) 13(2) C(5') 58(3) 68(2) 56(3) -2(2) -11(2) 13(2) C(6') 44(2) 58(2) 48(2) -6(2) 2(2) -3(2) C(7') 45(2) 58(2) 53(2) -4(2) 3(2) -6(2) C(8') 43(2) 53(2) 46(2) -6(2) -2(2) -11(2) C(9') 89(4) 58(2) 70(3) 1(2) 10(3) -20(2) C(10') 38(2) 54(2) 46(2) -4(2) -2(2) -5(2) C(11') 57(3) 56(2) 55(2) -7(2) -4(2) 5(2) C(12') 113(5) 74(3) 94(4) 28(3) -20(4) 10(3) C(13') 40(2) 60(2) 47(2) -10(2) 0(2) 6(2) C(14') 83(4) 71(3) 86(4) -13(2) 1(3) 26(3)
C(15') 71(3) 58(2) 80(3) -14(2) -8(2) 3(3) C(16') 58(3) 74(3) 81(3) -16(3) -6(2) -2(2) C(17') 24(2) 43(2) 59(2) -11(2) -6(2) 1(1) C(18') 134(5) 87(3) 95(4) 16(3) -53(4) 25(4) C(19') 140(5) 76(3) 101(5) -41(3) 24(4) -1(4)
Tabla 5. Coordenadas de átomos de hidrógeno (x 104) y parámetros de desplazamiento isotrópico (Å2 x 103) para 20a.
X y z U(eq)
H(1) 1084 10024 2951 56
H(2) 3155 11647 5619 75
H(4) 582 12986 4761 87
H(5) 499 12014 4092 85
H(7A) 914 10716 3768 65
H(7B) 1737 10137 4141 65
H(9A) 2151 11492 3042 124
H(9B) 3746 11482 3026 124
H(9C) 2985 11907 3507 124
H(12A) 3518 8461 4374 124
H(12B) 5021 8713 4497 124
H(12C) 4707 8148 4005 124
H(14) 4957 7782 2202 99
H(15) 3388 6876 1924 102
H(16) 1208 7245 1732 92
H(17) 631 8558 1795 80
H(18A) 4669 10658 5483 150
H(18B) 4325 9767 5419 150
H(18C) 3332 10318 5741 150
H(19A) 1612 13968 5332 167
H(19B) 1444 13941 5973 167
H(19C) 377 13523 5594 167
H(1') 1278 5373 2901 59
H(2') 3342 6647 5627 69
H(4') 882 8081 4799 78
H(5') 759 7166 4091 73
H(7'1) 1109 5896 3731 62
H(7'2) 1731 5252 4114 62
H(9'1) 2702 6649 3084 109
H(9'2) 4273 6498 3116 109
H(9'3) 3530 6937 3596 109
H(12D) 3144 3455 4341 141
H(12E) 4722 3531 4420 141
H(12F) 4136 3046 3926 141
H(14') 3456 2390 1902 96
H(15') 1191 2005 1881 84
H(16') 471 2930 1950
H(17') 7 4219 2028 51
H(18D) 4620 5660 5506 159
H(18E) 4452 4774 5353 159
H(18F) 3333 5197 5703 159
H(19D) 1836 8993 5393 159
H(19E) 1669 8940 6033 159
H(19F) 598 8541 5646 159
H(8) 3580(50) 10720(30) 3740(20) 76(19), H(10) 3840(40) 10090(20) 2961(16) 49(10), H(8') 3960(50) 5620(30) 3800(20) 75(15), H(10') 4010(40) 5090(20) 2979(15) 44(9),
Difracción de Rayos X del paladaciclo 25
Tabla 1. Datos del cristal y refinamiento de estructura para 25
Fórmula empírica 2(C24H32N4O8Pd2S2)·CH2Cl2
Peso molecular 1647.88
Temperatura 100(2) K
Longitud de onda 0.7107 Å
Sistema cristalino y Ortorrómbico
Grupo espacial P212121
Dimensiones de la celda a = 8.4525 (4) Å; α= 90°.
b = 15.486 (1) Å; β= 90°.
c = 46.184 (3) Å; γ = 90°.
Volumen 6045.2 (6) Å3
Z 4
densidad calculada 1.811 Mgm-3 Coeficiente de absorción 1.47 mm-1
F(000) 3304
Tamaño del cristal (mm) 0.2 × 0.11 × 0.04
Rango de θ (°) 0.9 a 26.4
Índices h, k, l -10 ≤ h ≤ 10, 0 ≤ k ≤ 19, 0 ≤ l ≤ 57 Reflexiones recogidas 45187
Reflexiones observadas 12387 (R(int) = 0.100)
Método de refinamiento Refinamiento por mínimos cuadrados con matriz completa
Datos/restricciones/parámetros 12387 / 732 / 765 Bondad de ajuste en F2 0.159
Mayor diferencia pico y agujero 1.16 y -1.49 Å-3
Tabla 2. Coordenadas atómicas (x 104) y parámetros de desplazamiento isotrópico equivalentes (Å2 x 103) para 25. U(eq) está definido como un tercio de la traza del tensor Uij ortogonalizado.
x y z U(eq) Pd1 0.35460 (10) 1.02625 (6) 0.084950 (19) 0.01186 (19) Pd2 0.50993 (10) 0.84907 (5) 0.069175 (18) 0.01161 (19) N1 0.4023 (10) 0.8147 (6) 0.0310 (2) 0.0136 (13) C2 0.3440 (13) 0.7363 (8) 0.0243 (3) 0.0172 (16)
H2 0.3476 0.6917 0.0384 0.021*
C3 0.2805 (13) 0.7190 (8) −0.0019 (2) 0.0186 (17)
H3 0.2446 0.6621 −0.0060 0.022*
C4 0.2666 (13) 0.7811 (8) −0.0229 (3) 0.0201 (17)
H4 0.2181 0.7688 −0.0410 0.024*
C5 0.3263 (12) 0.8637 (8) −0.0167 (2) 0.0162 (16)
H5 0.3232 0.9088 −0.0307 0.019*
C6 0.3897 (12) 0.8765 (7) 0.0106 (2) 0.0132 (14) S7 0.4704 (3) 0.97993 (18) 0.02118 (6) 0.0137 (6) O8 0.5019 (10) 1.0231 (5) −0.00545 (15) 0.0181 (13) O9 0.6058 (8) 0.9544 (5) 0.03856 (16) 0.0135 (12) N10 0.3537 (10) 1.0274 (6) 0.04084 (19) 0.0134 (12) C11 0.2006 (13) 1.0608 (7) 0.0279 (2) 0.0137 (13)
H11 0.1842 1.0335 0.0085 0.016*
C12 0.0666 (13) 1.0320 (8) 0.0485 (2) 0.0158 (14) C13 0.1231 (12) 1.0464 (8) 0.0797 (2) 0.0155 (16)
H13A 0.0640 1.0071 0.0927 0.019*
H13B 0.0980 1.1064 0.0855 0.019*
C14 0.0319 (13) 0.9349 (7) 0.0433 (2) 0.0168 (19)
H14A −0.0014 0.9261 0.0232 0.025*
H14B −0.0526 0.9160 0.0564 0.025*
H14C 0.1277 0.9011 0.0471 0.025*
C15 −0.0856 (13) 1.0843 (8) 0.0429 (3) 0.0175 (19)
H15A −0.0687 1.1445 0.0486 0.026*
H15B −0.1725 1.0598 0.0543 0.026*
H15C −0.1124 1.0817 0.0223 0.026*
C16 0.2116 (14) 1.1577 (8) 0.0242 (3) 0.0173 (14) O17 0.2732 (10) 1.2074 (5) 0.04151 (18) 0.0223 (16)
O18 0.1397 (9) 1.1828 (5) 0.00008 (17) 0.0207 (15) C19 0.1356 (16) 1.2749 (8) −0.0045 (3) 0.027 (2)
H19A 0.0559 1.3008 0.0082 0.040*
H19B 0.1084 1.2868 −0.0248 0.040*
H19C 0.2396 1.2996 −0.0002 0.040*
N20 0.3466 (11) 1.0229 (6) 0.12934 (19) 0.0113 (13) C21 0.2250 (13) 1.0433 (7) 0.1469 (2) 0.0140 (16)
H21 0.1252 1.0547 0.1382 0.017*
C22 0.2357 (14) 1.0484 (7) 0.1758 (2) 0.0151 (17)
H22 0.1474 1.0663 0.1870 0.018*
C23 0.3780 (13) 1.0273 (7) 0.1892 (2) 0.0151 (16)
H23 0.3865 1.0285 0.2097 0.018*
C24 0.5070 (15) 1.0044 (6) 0.1725 (2) 0.0160 (15)
H24 0.6060 0.9911 0.1811 0.019*
C25 0.4875 (14) 1.0016 (6) 0.1428 (2) 0.0125 (14) S26 0.6426 (3) 0.97311 (19) 0.11889 (6) 0.0130 (5) O27 0.6221 (8) 1.0322 (5) 0.09480 (16) 0.0133 (12) O28 0.7848 (9) 0.9785 (5) 0.13567 (16) 0.0170 (14) N29 0.6080 (10) 0.8789 (6) 0.1076 (2) 0.0125 (12) C30 0.6348 (14) 0.8076 (7) 0.1272 (2) 0.0157 (13)
H30 0.6301 0.8306 0.1475 0.019*
C31 0.4936 (16) 0.7444 (7) 0.1231 (2) 0.0172 (13) C32 0.4575 (13) 0.7385 (7) 0.0904 (2) 0.0160 (16)
H32A 0.3439 0.7251 0.0877 0.019*
H32B 0.5195 0.6905 0.0819 0.019*
C33 0.7982 (15) 0.7677 (8) 0.1227 (3) 0.0209 (15) O34 0.8937 (10) 0.7546 (5) 0.14220 (19) 0.0243 (17) O35 0.8312 (9) 0.7532 (5) 0.09493 (18) 0.0234 (15) C36 0.9953 (15) 0.7296 (8) 0.0894 (3) 0.027 (2)
H36A 1.0639 0.7792 0.0935 0.041*
H36B 1.0072 0.7128 0.0690 0.041*
H36C 1.0252 0.6811 0.1019 0.041*
C37 0.5286 (14) 0.6533 (7) 0.1343 (2) 0.0165 (19)
H37A 0.5750 0.6571 0.1537 0.025*
H37B 0.6031 0.6245 0.1213 0.025*
H37C 0.4300 0.6201 0.1352 0.025*
C38 0.3501 (14) 0.7835 (8) 0.1383 (2) 0.0179 (19)
H38A 0.2628 0.7419 0.1382 0.027*
H38B 0.3175 0.8363 0.1282 0.027*
H38C 0.3779 0.7975 0.1584 0.027*
Pd41 0.70092 (10) 0.20590 (6) 0.20323 (2) 0.0141 (2) Pd42 1.00080 (11) 0.32515 (5) 0.201411 (18) 0.01338 (19)
N41 0.5847 (12) 0.2297 (6) 0.1655 (2) 0.0179 (14) C42 0.4296 (15) 0.2353 (8) 0.1602 (3) 0.0208 (17)
H42 0.3605 0.2349 0.1765 0.025*
C43 0.3624 (16) 0.2416 (8) 0.1335 (3) 0.0235 (18)
H43 0.2513 0.2485 0.1315 0.028*
C44 0.4566 (14) 0.2377 (8) 0.1096 (3) 0.0238 (18)
H44 0.4130 0.2432 0.0907 0.029*
C45 0.6168 (14) 0.2257 (8) 0.1134 (3) 0.0215 (17)
H45 0.6842 0.2179 0.0972 0.026*
C46 0.6797 (14) 0.2252 (8) 0.1417 (3) 0.0196 (15) S47 0.8839 (4) 0.2103 (2) 0.14818 (6) 0.0181 (6) O48 0.8914 (9) 0.1508 (5) 0.17251 (16) 0.0174 (12) O49 0.9497 (10) 0.1815 (5) 0.12124 (17) 0.0228 (15) N50 0.9610 (11) 0.2988 (6) 0.1587 (2) 0.0186 (13) C51 0.9271 (17) 0.3755 (8) 0.1404 (3) 0.0274 (14)
H51 0.8091 0.3805 0.1402 0.033*
C52 0.9816 (18) 0.4509 (8) 0.1562 (3) 0.0308 (16) C53 0.9422 (17) 0.4431 (8) 0.1872 (3) 0.0284 (18)
H53A 0.8275 0.4529 0.1900 0.034*
H53B 1.0004 0.4874 0.1983 0.034*
C54 0.9729 (18) 0.3642 (9) 0.1099 (3) 0.0359 (17) O55 1.1032 (12) 0.3516 (7) 0.1008 (2) 0.042 (2) O56 0.8474 (13) 0.3767 (7) 0.0914 (2) 0.0432 (19) C57 0.876 (2) 0.3633 (11) 0.0607 (3) 0.048 (3)
H57A 0.9262 0.4146 0.0525 0.073*
H57B 0.7746 0.3529 0.0508 0.073*
H57C 0.9448 0.3131 0.0580 0.073*
C58 0.9160 (17) 0.5369 (9) 0.1435 (3) 0.034 (2)
H58A 0.9547 0.5443 0.1236 0.051*
H58B 0.9520 0.5855 0.1554 0.051*
H58C 0.8001 0.5352 0.1434 0.051*
C59 1.1731 (17) 0.4557 (9) 0.1523 (3) 0.036 (2)
H59A 1.2210 0.4027 0.1599 0.054*
H59B 1.2144 0.5055 0.1630 0.054*
H59C 1.1991 0.4618 0.1317 0.054*
N60 1.0384 (10) 0.3602 (6) 0.2442 (2) 0.0133 (13) C61 1.0713 (12) 0.4398 (8) 0.2545 (3) 0.0139 (10)
H61 1.0835 0.4860 0.2412 0.017*
C62 1.0877 (12) 0.4565 (8) 0.2833 (2) 0.0138 (10)
H62 1.1116 0.5137 0.2894 0.017*
C63 1.0707 (12) 0.3929 (7) 0.3040 (3) 0.0136 (10)
H63 1.0811 0.4045 0.3241 0.016*
C64 1.0361 (11) 0.3080 (7) 0.2932 (2) 0.0133 (10)
H64 1.0247 0.2609 0.3062 0.016*
C65 1.0200 (12) 0.2953 (7) 0.2643 (2) 0.0130 (10) S66 0.9853 (3) 0.19160 (17) 0.24911 (6) 0.0132 (5) O67 1.0726 (8) 0.1925 (5) 0.22191 (16) 0.0119 (12) O68 1.0364 (9) 0.1309 (5) 0.27124 (16) 0.0150 (14) N69 0.8020 (11) 0.1844 (6) 0.24153 (19) 0.0148 (12) C70 0.6892 (13) 0.1823 (7) 0.2667 (3) 0.0167 (13)
H70 0.7454 0.1974 0.2851 0.020*
C71 0.5656 (14) 0.2493 (8) 0.2598 (3) 0.0184 (14) C72 0.5174 (14) 0.2385 (7) 0.2283 (2) 0.0156 (16)
H72A 0.4711 0.2932 0.2212 0.019*
H72B 0.4350 0.1932 0.2269 0.019*
C73 0.6243 (15) 0.0927 (8) 0.2683 (3) 0.0217 (15) O74 0.5896 (10) 0.0445 (6) 0.24877 (18) 0.0250 (17)
O75 0.5940 (10) 0.0725 (6) 0.2966 (2) 0.0316 (16) C76 0.5098 (19) −0.0100 (8) 0.3005 (3) 0.039 (2)
H76A 0.4215 −0.0131 0.2867 0.059*
H76B 0.4691 −0.0138 0.3203 0.059*
H76C 0.5828 −0.0580 0.2969 0.059*
C77 0.4218 (14) 0.2418 (8) 0.2795 (3) 0.0185 (19)
H77A 0.3824 0.1823 0.2792 0.028*
H77B 0.3386 0.2810 0.2727 0.028*
H77C 0.4519 0.2573 0.2993 0.028*
C78 0.6333 (14) 0.3393 (8) 0.2641 (3) 0.0204 (19)
H78A 0.6703 0.3455 0.2841 0.031*
H78B 0.5511 0.3824 0.2602 0.031*
H78C 0.7222 0.3481 0.2508 0.031*
C1W 0.290 (2) 0.4550 (15) 0.0527 (5) 0.089 (8)
H1W1 0.2436 0.4397 0.0337 0.107*
H1W2 0.2811 0.4044 0.0657 0.107*
H1W3 0.3025 0.4652 0.0316 0.107*
H1W4 0.2215 0.4037 0.0550 0.107*
Cl1A 0.4975 (11) 0.4857 (9) 0.0483 (3) 0.150 (6) Cl1B 0.492 (5) 0.428 (4) 0.0674 (14) 0.150 (6) Cl2 0.1906 (7) 0.5447 (3) 0.06771 (12) 0.0781 (15)
Tabla 3. Longitudes de enlace (Å) y ángulos (º) para 25.
Pd1-C13 1.997 (11) Pd41-Pd42 3.1373 (12)
Pd1-N10 2.037 (9) Pd42-C53 2.004 (12)
Pd1-N20 2.052 (9) Pd42-N50 2.041 (9)
Pd1-O27 2.308 (7) Pd42-N60 2.072 (9)
Pd1-Pd2 3.1276 (12) Pd42-O67 2.341 (7)
Pd2-N29 2.011 (9) N41-C42 1.337 (14)
Pd2-C32 2.022 (11) N41-C46 1.364 (16)
Pd2-N1 2.056 (9) C42-C43 1.362 (17)
Pd2-O9 2.306 (8) C42-H42 0.9500
N1-C2 1.347 (14) C43-C44 1.363 (18)
N1-C6 1.347 (14) C43-H43 0.9500
C2-C3 1.350 (16) C44-C45 1.378 (17)
C2-H2 0.9500 C44-H44 0.9500
C3-C4 1.370 (17) C45-C46 1.408 (17)
C3-H3 0.9500 C45-H45 0.9500
C4-C5 1.403 (17) C46-S47 1.767 (12)
C4-H4 0.9500 S47-O49 1.434 (8)
C5-C6 1.384 (15) S47-O48 1.454 (8)
C5-H5 0.9500 S47-N50 1.594 (10)
C6-S7 1.809 (12) N50-C51 1.486 (15)
S7-O8 1.425 (7) C51-C52 1.451 (18)
S7-O9 1.452 (8) C51-C54 1.471 (19)
S7-N10 1.529 (9) C51-H51 1.0000
N10-C11 1.517 (14) C52-C53 1.474 (18)
C11-C16 1.513 (16) C52-C58 1.557 (17)
C11-C12 1.544 (16) C52-C59 1.63 (2)
C11-H11 1.0000 C53-H53A 0.9900
C12-C13 1.536 (15) C53-H53B 0.9900
C12-C15 1.541 (15) C54-O55 1.196 (17)
C12-C14 1.551 (16) C54-O56 1.377 (16)
C13-H13A 0.9900 O56-C57 1.453 (17)
C13-H13B 0.9900 C57-H57A 0.9800
C14-H14A 0.9800 C57-H57B 0.9800
C14-H14B 0.9800 C57-H57C 0.9800
C14-H14C 0.9800 C58-H58A 0.9800
C15-H15A 0.9800 C58-H58B 0.9800
C15-H15B 0.9800 C58-H58C 0.9800
C15-H15C 0.9800 C59-H59A 0.9800
C16-O17 1.225 (14) C59-H59B 0.9800
C16-O18 1.328 (13) C59-H59C 0.9800
O18-C19 1.442 (14) N60-C61 1.351 (14)
C19-H19A 0.9800 N60-C65 1.379 (14)
C19-H19B 0.9800 C61-C62 1.362 (15)
C19-H19C 0.9800 C61-H61 0.9500
N20-C21 1.347 (14) C62-C63 1.379 (16)
N20-C25 1.385 (14) C62-H62 0.9500
C21-C22 1.342 (15) C63-C64 1.437 (15)
C21-H21 0.9500 C63-H63 0.9500
C22-C23 1.392 (15) C64-C65 1.354 (15)
C22-H22 0.9500 C64-H64 0.9500
C23-C24 1.383 (16) C65-S66 1.777 (11)
C23-H23 0.9500 S66-O68 1.454 (8)
C24-C25 1.378 (14) S66-O67 1.457 (8)
C24-H24 0.9500 S66-N69 1.593 (10)
C25-S26 1.771 (11) N69-C70 1.505 (14)
S26-O28 1.433 (8) C70-C73 1.495 (17)
S26-O27 1.451 (8) C70-C71 1.507 (16)
S26-N29 1.577 (9) C70-H70 1.0000
N29-C30 1.447 (14) C71-C72 1.518 (16)
C30-C33 1.528 (16) C71-C78 1.520 (16)
C30-C31 1.555 (17) C71-C77 1.524 (16)
C30-H30 1.0000 C72-H72A 0.9900
C31-C37 1.533 (15) C72-H72B 0.9900
C31-C38 1.529 (16) C73-O74 1.207 (14)
C31-C32 1.543 (15) C73-O75 1.369 (15)
C32-H32A 0.9900 O75-C76 1.473 (14)
C32-H32B 0.9900 C76-H76A 0.9800
C33-O34 1.228 (14) C76-H76B 0.9800
C33-O35 1.330 (14) C76-H76C 0.9800
O35-C36 1.457 (14) C77-H77A 0.9800
C36-H36A 0.9800 C77-H77B 0.9800
C36-H36B 0.9800 C77-H77C 0.9800
C36-H36C 0.9800 C78-H78A 0.9800
C37-H37A 0.9800 C78-H78B 0.9800
C37-H37B 0.9800 C78-H78C 0.9800
C37-H37C 0.9800 C1W-Cl2 1.767 (19)
C38-H38A 0.9800 C1W-Cl1A 1.83 (2)
C38-H38B 0.9800 C1W-Cl1B 1.89 (6)
C38-H38C 0.9800 C1W-H1W1 0.9900
Pd41-N69 1.992 (9) C1W-H1W2 0.9900
Pd41-C72 2.001 (11) C1W-H1W3 0.9900
Pd41-N41 2.034 (10) C1W-H1W4 0.9900
Pd41-O48 2.309 (8)
C13-Pd1-N10 82.7 (4) O48-Pd41-Pd42 68.8 (2) C13-Pd1-N20 95.3 (4) C53-Pd42-N50 79.9 (5) N10-Pd1-N20 177.7 (4) C53-Pd42-N60 96.4 (5) C13-Pd1-O27 167.9 (4) N50-Pd42-N60 176.3 (4) N10-Pd1-O27 101.6 (3) C53-Pd42-O67 175.2 (4) N20-Pd1-O27 80.6 (3) N50-Pd42-O67 104.9 (3) C13-Pd1-Pd2 121.4 (3) N60-Pd42-O67 78.7 (3) N10-Pd1-Pd2 77.1 (3) C53-Pd42-Pd41 110.2 (4) N20-Pd1-Pd2 103.0 (2) N50-Pd42-Pd41 77.0 (3) O27-Pd1-Pd2 70.72 (19) N60-Pd42-Pd41 104.6 (2) N29-Pd2-C32 81.9 (4) O67-Pd42-Pd41 71.48 (17)
N29-Pd2-N1 177.3 (4) C42-N41-C46 115.7 (11) C32-Pd2-N1 95.7 (4) C42-N41-Pd41 129.9 (9) N29-Pd2-O9 103.5 (3) C46-N41-Pd41 113.5 (8) C32-Pd2-O9 166.7 (4) N41-C42-C43 125.3 (13)
N1-Pd2-O9 79.2 (3) N41-C42-H42 117.3
N29-Pd2-Pd1 76.5 (3) C43-C42-H42 117.3
C32-Pd2-Pd1 122.6 (3) C42-C43-C44 119.2 (12)
N1-Pd2-Pd1 104.0 (3) C42-C43-H43 120.4
O9-Pd2-Pd1 70.71 (18) C44-C43-H43 120.4 C2-N1-C6 116.8 (10) C43-C44-C45 118.4 (12)
C2-N1-Pd2 126.3 (8) C43-C44-H44 120.8
C6-N1-Pd2 116.8 (7) C45-C44-H44 120.8
N1-C2-C3 122.0 (11) C44-C45-C46 119.4 (13)
N1-C2-H2 119.0 C44-C45-H45 120.3
C3-C2-H2 119.0 C46-C45-H45 120.3
C2-C3-C4 121.8 (12) N41-C46-C45 121.6 (11)
C2-C3-H3 119.1 N41-C46-S47 116.4 (9)
C4-C3-H3 119.1 C45-C46-S47 121.8 (10)
C3-C4-C5 117.8 (11) O49-S47-O48 117.2 (5)
C3-C4-H4 121.1 O49-S47-N50 111.9 (5)
C5-C4-H4 121.1 O48-S47-N50 106.9 (5)
C6-C5-C4 117.0 (11) O49-S47-C46 105.8 (5)
C6-C5-H5 121.5 O48-S47-C46 104.9 (5)
C4-C5-H5 121.5 N50-S47-C46 109.8 (5)
N1-C6-C5 124.4 (11) S47-O48-Pd41 102.1 (4) N1-C6-S7 114.2 (8) C51-N50-S47 115.8 (8) C5-C6-S7 121.3 (9) C51-N50-Pd42 114.9 (8) O8-S7-O9 117.2 (5) S47-N50-Pd42 122.3 (6) O8-S7-N10 114.1 (5) C52-C51-C54 119.5 (12) O9-S7-N10 108.1 (5) C52-C51-N50 107.3 (10) O8-S7-C6 104.6 (5) C54-C51-N50 113.5 (11)
O9-S7-C6 101.9 (5) C52-C51-H51 105.1
N10-S7-C6 110.1 (5) C54-C51-H51 105.1
S7-O9-Pd2 104.7 (4) N50-C51-H51 105.1
C11-N10-S7 118.7 (7) C51-C52-C53 110.4 (11) C11-N10-Pd1 113.6 (7) C51-C52-C58 112.7 (11) S7-N10-Pd1 125.9 (5) C53-C52-C58 110.9 (11) C16-C11-N10 109.3 (9) C51-C52-C59 107.3 (12) C16-C11-C12 113.6 (10) C53-C52-C59 109.6 (11) N10-C11-C12 106.5 (8) C58-C52-C59 105.9 (11)
C16-C11-H11 109.1 C52-C53-Pd42 109.7 (9)
N10-C11-H11 109.1 C52-C53-H53A 109.7
C12-C11-H11 109.1 Pd42-C53-H53A 109.7
C13-C12-C15 109.9 (10) C52-C53-H53B 109.7 C13-C12-C11 107.9 (9) Pd42-C53-H53B 109.7 C15-C12-C11 111.0 (9) H53A-C53-H53B 108.2
C13-C12-C14 110.1 (10) O55-C54-O56 120.8 (13) C15-C12-C14 109.0 (9) O55-C54-C51 126.9 (13) C11-C12-C14 108.9 (10) O56-C54-C51 112.1 (13) C12-C13-Pd1 113.3 (7) C54-O56-C57 117.5 (12)
C12-C13-H13A 108.9 O56-C57-H57A 109.5
Pd1-C13-H13A 108.9 O56-C57-H57B 109.5
C12-C13-H13B 108.9 H57A-C57-H57B 109.5
Pd1-C13-H13B 108.9 O56-C57-H57C 109.5
H13A-C13-H13B 107.7 H57A-C57-H57C 109.5
C12-C14-H14A 109.5 H57B-C57-H57C 109.5
C12-C14-H14B 109.5 C52-C58-H58A 109.5
H14A-C14-H14B 109.5 C52-C58-H58B 109.5
C12-C14-H14C 109.5 H58A-C58-H58B 109.5
H14A-C14-H14C 109.5 C52-C58-H58C 109.5
H14B-C14-H14C 109.5 H58A-C58-H58C 109.5
C12-C15-H15A 109.5 H58B-C58-H58C 109.5
C12-C15-H15B 109.5 C52-C59-H59A 109.5
H15A-C15-H15B 109.5 C52-C59-H59B 109.5
C12-C15-H15C 109.5 H59A-C59-H59B 109.5
H15A-C15-H15C 109.5 C52-C59-H59C 109.5
H15B-C15-H15C 109.5 H59A-C59-H59C 109.5
O17-C16-O18 123.9 (11) H59B-C59-H59C 109.5 O17-C16-C11 125.2 (11) C61-N60-C65 116.7 (10) O18-C16-C11 110.9 (10) C61-N60-Pd42 127.5 (8) C16-O18-C19 115.1 (9) C65-N60-Pd42 115.8 (7)
O18-C19-H19A 109.5 N60-C61-C62 122.7 (11)
O18-C19-H19B 109.5 N60-C61-H61 118.6
H19A-C19-H19B 109.5 C62-C61-H61 118.6
O18-C19-H19C 109.5 C61-C62-C63 121.9 (11)
H19A-C19-H19C 109.5 C61-C62-H62 119.0
H19B-C19-H19C 109.5 C63-C62-H62 119.0
C21-N20-C25 116.2 (9) C62-C63-C64 115.8 (11)
C21-N20-Pd1 128.4 (7) C62-C63-H63 122.1
C25-N20-Pd1 115.3 (7) C64-C63-H63 122.1 C22-C21-N20 124.2 (11) C65-C64-C63 119.7 (10)
C22-C21-H21 117.9 C65-C64-H64 120.2
N20-C21-H21 117.9 C63-C64-H64 120.2
C21-C22-C23 119.2 (11) C64-C65-N60 123.2 (10)
C21-C22-H22 120.4 C64-C65-S66 122.4 (9)
C23-C22-H22 120.4 N60-C65-S66 114.2 (8)
C24-C23-C22 119.5 (11) O68-S66-O67 117.5 (5)
C24-C23-H23 120.3 O68-S66-N69 113.5 (5)
C22-C23-H23 120.3 O67-S66-N69 107.7 (5)
C25-C24-C23 118.0 (11) O68-S66-C65 104.9 (5)
C25-C24-H24 121.0 O67-S66-C65 104.4 (5)
C23-C24-H24 121.0 N69-S66-C65 108.1 (5)
C24-C25-N20 122.8 (10) S66-O67-Pd42 103.1 (4) C24-C25-S26 122.7 (9) C70-N69-S66 116.6 (7) N20-C25-S26 114.5 (8) C70-N69-Pd41 114.8 (7) O28-S26-O27 118.6 (5) S66-N69-Pd41 126.9 (5) O28-S26-N29 112.8 (5) C73-C70-N69 106.8 (9) O27-S26-N29 107.9 (5) C73-C70-C71 113.3 (10) O28-S26-C25 105.6 (5) N69-C70-C71 105.0 (9)
O27-S26-C25 103.5 (5) C73-C70-H70 110.5
N29-S26-C25 107.5 (5) N69-C70-H70 110.5
S26-O27-Pd1 104.1 (4) C71-C70-H70 110.5
C30-N29-S26 117.9 (8) C70-C71-C72 108.3 (10) C30-N29-Pd2 116.3 (7) C70-C71-C78 110.0 (10) S26-N29-Pd2 125.5 (5) C72-C71-C78 109.2 (10) N29-C30-C33 111.3 (9) C70-C71-C77 111.9 (10) N29-C30-C31 106.4 (9) C72-C71-C77 110.5 (10) C33-C30-C31 115.0 (10) C78-C71-C77 106.9 (10)
N29-C30-H30 108.0 C71-C72-Pd41 111.9 (8)
C33-C30-H30 108.0 C71-C72-H72A 109.2
C31-C30-H30 108.0 Pd41-C72-H72A 109.2
C37-C31-C38 111.1 (10) C71-C72-H72B 109.2
C37-C31-C32 108.4 (9) Pd41-C72-H72B 109.2 C38-C31-C32 108.6 (10) H72A-C72-H72B 107.9 C37-C31-C30 112.9 (10) O74-C73-O75 121.8 (11) C38-C31-C30 107.6 (9) O74-C73-C70 128.8 (12) C32-C31-C30 108.1 (9) O75-C73-C70 109.1 (10) C31-C32-Pd2 112.3 (8) C73-O75-C76 113.8 (10)
C31-C32-H32A 109.1 O75-C76-H76A 109.5
Pd2-C32-H32A 109.1 O75-C76-H76B 109.5
C31-C32-H32B 109.1 H76A-C76-H76B 109.5
Pd2-C32-H32B 109.1 O75-C76-H76C 109.5
H32A-C32-H32B 107.9 H76A-C76-H76C 109.5
O34-C33-O35 122.8 (11) H76B-C76-H76C 109.5 O34-C33-C30 124.1 (11) C71-C77-H77A 109.5 O35-C33-C30 113.0 (10) C71-C77-H77B 109.5 C33-O35-C36 114.3 (9) H77A-C77-H77B 109.5
O35-C36-H36A 109.5 C71-C77-H77C 109.5
O35-C36-H36B 109.5 H77A-C77-H77C 109.5
H36A-C36-H36B 109.5 H77B-C77-H77C 109.5
O35-C36-H36C 109.5 C71-C78-H78A 109.5
H36A-C36-H36C 109.5 C71-C78-H78B 109.5
H36B-C36-H36C 109.5 H78A-C78-H78B 109.5
C31-C37-H37A 109.5 C71-C78-H78C 109.5
C31-C37-H37B 109.5 H78A-C78-H78C 109.5
H37A-C37-H37B 109.5 H78B-C78-H78C 109.5
C31-C37-H37C 109.5 Cl2-C1W-Cl1A 107.2 (12) H37A-C37-H37C 109.5 Cl2-C1W-Cl1B 117.7 (17)
H37B-C37-H37C 109.5 Cl2-C1W-H1W1 110.3
C31-C38-H38A 109.5 Cl1A-C1W-H1W1 110.3
C31-C38-H38B 109.5 Cl1B-C1W-H1W1 128.8
H38A-C38-H38B 109.5 Cl2-C1W-H1W2 110.3
C31-C38-H38C 109.5 Cl1A-C1W-H1W2 110.3
H38A-C38-H38C 109.5 Cl1B-C1W-H1W2 70.9
H38B-C38-H38C 109.5 H1W1-C1W-H1W2 108.5
N69-Pd41-C72 82.0 (4) Cl2-C1W-H1W3 108.0 N69-Pd41-N41 176.3 (4) Cl1A-C1W-H1W3 75.5 C72-Pd41-N41 94.4 (4) Cl1B-C1W-H1W3 107.2 N69-Pd41-O48 100.6 (3) H1W2-C1W-H1W3 137.0 C72-Pd41-O48 171.7 (4) Cl2-C1W-H1W4 108.0 N41-Pd41-O48 82.9 (3) Cl1A-C1W-H1W4 141.6 N69-Pd41-Pd42 77.0 (3) Cl1B-C1W-H1W4 108.1 C72-Pd41-Pd42 119.6 (3) H1W1-C1W-H1W4 70.8 N41-Pd41-Pd42 105.1 (3) H1W3-C1W-H1W4 107.3 C13-Pd1-Pd2-N29 −136.0 (5) O34-C33-O35-C36 −6.5 (17) N10-Pd1-Pd2-N29 151.0 (4) C30-C33-O35-C36 169.7 (10) N20-Pd1-Pd2-N29 −31.4 (4) N69-Pd41-Pd42-C53 −133.3 (5) O27-Pd1-Pd2-N29 43.6 (3) C72-Pd41-Pd42-C53 −60.5 (5) C13-Pd1-Pd2-C32 −65.0 (5) N41-Pd41-Pd42-C53 43.6 (5) N10-Pd1-Pd2-C32 −138.1 (5) O48-Pd41-Pd42-C53 119.6 (5) N20-Pd1-Pd2-C32 39.6 (5) N69-Pd41-Pd42-N50 152.8 (4) O27-Pd1-Pd2-C32 114.6 (4) C72-Pd41-Pd42-N50 −134.4 (5)
C13-Pd1-Pd2-N1 41.2 (5) N41-Pd41-Pd42-N50 −30.3 (4) N10-Pd1-Pd2-N1 −31.8 (4) O48-Pd41-Pd42-N50 45.7 (3) N20-Pd1-Pd2-N1 145.9 (4) N69-Pd41-Pd42-N60 −30.6 (4) O27-Pd1-Pd2-N1 −139.1 (3) C72-Pd41-Pd42-N60 42.2 (4) C13-Pd1-Pd2-O9 114.2 (4) N41-Pd41-Pd42-N60 146.3 (4) N10-Pd1-Pd2-O9 41.2 (3) O48-Pd41-Pd42-N60 −137.7 (3) N20-Pd1-Pd2-O9 −141.1 (3) N69-Pd41-Pd42-O67 41.9 (3) O27-Pd1-Pd2-O9 −66.1 (3) C72-Pd41-Pd42-O67 114.7 (4)
C32-Pd2-N1-C2 −8.9 (10) N41-Pd41-Pd42-O67 −141.2 (3) O9-Pd2-N1-C2 158.7 (9) O48-Pd41-Pd42-O67 −65.2 (3) Pd1-Pd2-N1-C2 −134.5 (9) C72-Pd41-N41-C42 −19.6 (12) C32-Pd2-N1-C6 171.5 (8) O48-Pd41-N41-C42 152.5 (12) O9-Pd2-N1-C6 −20.9 (7) Pd42-Pd41-N41-C42 −141.8 (11) Pd1-Pd2-N1-C6 45.9 (8) C72-Pd41-N41-C46 172.1 (8)
C6-N1-C2-C3 2.2 (16) O48-Pd41-N41-C46 −15.8 (8) Pd2-N1-C2-C3 −177.4 (8) Pd42-Pd41-N41-C46 49.8 (8)
N1-C2-C3-C4 −2.4 (18) C46-N41-C42-C43 −4 (2) C2-C3-C4-C5 2.4 (18) Pd41-N41-C42-C43 −171.9 (9) C3-C4-C5-C6 −2.2 (16) N41-C42-C43-C44 3 (2) C2-N1-C6-C5 −2.2 (16) C42-C43-C44-C45 1.4 (19) Pd2-N1-C6-C5 177.4 (8) C43-C44-C45-C46 −5.4 (18)
C2-N1-C6-S7 179.9 (8) C42-N41-C46-C45 −0.6 (17) Pd2-N1-C6-S7 −0.5 (10) Pd41-N41-C46-C45 169.5 (9) C4-C5-C6-N1 2.3 (16) C42-N41-C46-S47 −175.8 (9) C4-C5-C6-S7 −180.0 (8) Pd41-N41-C46-S47 −5.7 (11) N1-C6-S7-O8 158.1 (8) C44-C45-C46-N41 5.1 (18) C5-C6-S7-O8 −19.9 (10) C44-C45-C46-S47 −179.9 (9) N1-C6-S7-O9 35.5 (9) N41-C46-S47-O49 162.7 (9) C5-C6-S7-O9 −142.4 (9) C45-C46-S47-O49 −12.5 (12) N1-C6-S7-N10 −79.0 (9) N41-C46-S47-O48 38.2 (10) C5-C6-S7-N10 103.0 (9) C45-C46-S47-O48 −137.0 (10) O8-S7-O9-Pd2 −160.4 (4) N41-C46-S47-N50 −76.3 (10) N10-S7-O9-Pd2 69.0 (5) C45-C46-S47-N50 108.5 (11) C6-S7-O9-Pd2 −47.0 (5) O49-S47-O48-Pd41 −161.0 (4) N29-Pd2-O9-S7 −137.2 (4) N50-S47-O48-Pd41 72.5 (5) C32-Pd2-O9-S7 110.4 (16) C46-S47-O48-Pd41 −44.1 (5)
N1-Pd2-O9-S7 42.1 (4) N69-Pd41-O48-S47 −143.4 (4) Pd1-Pd2-O9-S7 −67.0 (4) N41-Pd41-O48-S47 37.3 (5) O8-S7-N10-C11 47.9 (10) Pd42-Pd41-O48-S47 −72.0 (4) O9-S7-N10-C11 −179.8 (8) O49-S47-N50-C51 66.5 (10) C6-S7-N10-C11 −69.2 (9) O48-S47-N50-C51 −163.9 (8) O8-S7-N10-Pd1 −148.1 (6) C46-S47-N50-C51 −50.6 (10) O9-S7-N10-Pd1 −15.8 (8) O49-S47-N50-Pd42 −144.3 (6) C6-S7-N10-Pd1 94.8 (7) O48-S47-N50-Pd42 −14.7 (7) C13-Pd1-N10-C11 12.6 (8) C46-S47-N50-Pd42 98.5 (7) O27-Pd1-N10-C11 −156.0 (7) C53-Pd42-N50-C51 5.0 (9) Pd2-Pd1-N10-C11 137.2 (7) O67-Pd42-N50-C51 −174.8 (8)
C13-Pd1-N10-S7 −152.1 (8) Pd41-Pd42-N50-C51 118.7 (8) O27-Pd1-N10-S7 39.3 (7) C53-Pd42-N50-S47 −144.4 (7)
Pd2-Pd1-N10-S7 −27.5 (6) O67-Pd42-N50-S47 35.8 (7) S7-N10-C11-C16 −104.9 (10) Pd41-Pd42-N50-S47 −30.7 (5) Pd1-N10-C11-C16 89.2 (9) S47-N50-C51-C52 169.7 (9) S7-N10-C11-C12 132.1 (9) Pd42-N50-C51-C52 18.2 (13) Pd1-N10-C11-C12 −33.8 (11) S47-N50-C51-C54 −56.1 (14) C16-C11-C12-C13 −78.0 (12) Pd42-N50-C51-C54 152.4 (10) N10-C11-C12-C13 42.3 (12) C54-C51-C52-C53 −171.7 (12) C16-C11-C12-C15 42.5 (13) N50-C51-C52-C53 −40.8 (15) N10-C11-C12-C15 162.8 (10) C54-C51-C52-C58 63.7 (17) C16-C11-C12-C14 162.5 (9) N50-C51-C52-C58 −165.4 (11) N10-C11-C12-C14 −77.2 (11) C54-C51-C52-C59 −52.4 (16) C15-C12-C13-Pd1 −155.5 (8) N50-C51-C52-C59 78.5 (12) C11-C12-C13-Pd1 −34.4 (12) C51-C52-C53-Pd42 46.4 (14) C14-C12-C13-Pd1 84.4 (10) C58-C52-C53-Pd42 172.0 (9) N10-Pd1-C13-C12 12.6 (8) C59-C52-C53-Pd42 −71.5 (11) N20-Pd1-C13-C12 −166.2 (8) N50-Pd42-C53-C52 −27.2 (10) O27-Pd1-C13-C12 124.2 (16) N60-Pd42-C53-C52 152.7 (10) Pd2-Pd1-C13-C12 −57.5 (9) Pd41-Pd42-C53-C52 −99.1 (10) N10-C11-C16-O17 −39.5 (16) C52-C51-C54-O55 66 (2) C12-C11-C16-O17 79.3 (15) N50-C51-C54-O55 −62 (2) N10-C11-C16-O18 143.0 (9) C52-C51-C54-O56 −108.7 (15) C12-C11-C16-O18 −98.3 (11) N50-C51-C54-O56 123.2 (12) O17-C16-O18-C19 −1.1 (17) O55-C54-O56-C57 7 (2) C11-C16-O18-C19 176.5 (9) C51-C54-O56-C57 −177.1 (12) C13-Pd1-N20-C21 −9.6 (10) C53-Pd42-N60-C61 −21.8 (10) O27-Pd1-N20-C21 158.9 (10) O67-Pd42-N60-C61 158.1 (9) Pd2-Pd1-N20-C21 −133.5 (9) Pd41-Pd42-N60-C61 −134.7 (8) C13-Pd1-N20-C25 174.3 (8) C53-Pd42-N60-C65 154.8 (8) O27-Pd1-N20-C25 −17.2 (7) O67-Pd42-N60-C65 −25.4 (7) Pd2-Pd1-N20-C25 50.3 (7) Pd41-Pd42-N60-C65 41.9 (7) C25-N20-C21-C22 3.9 (16) C65-N60-C61-C62 0.7 (15) Pd1-N20-C21-C22 −172.2 (9) Pd42-N60-C61-C62 177.2 (8) N20-C21-C22-C23 −3.7 (18) N60-C61-C62-C63 −0.4 (17)
C21-C22-C23-C24 2.4 (17) C61-C62-C63-C64 0.6 (16) C22-C23-C24-C25 −1.6 (16) C62-C63-C64-C65 −1.1 (15) C23-C24-C25-N20 2.0 (16) C63-C64-C65-N60 1.5 (16) C23-C24-C25-S26 −179.9 (8) C63-C64-C65-S66 177.4 (8) C21-N20-C25-C24 −3.0 (15) C61-N60-C65-C64 −1.3 (15) Pd1-N20-C25-C24 173.6 (8) Pd42-N60-C65-C64 −178.2 (8) C21-N20-C25-S26 178.7 (8) C61-N60-C65-S66 −177.5 (7) Pd1-N20-C25-S26 −4.7 (10) Pd42-N60-C65-S66 5.6 (10) C24-C25-S26-O28 −14.9 (10) C64-C65-S66-O68 −20.0 (10) N20-C25-S26-O28 163.4 (7) N60-C65-S66-O68 156.2 (8) C24-C25-S26-O27 −140.2 (9) C64-C65-S66-O67 −144.2 (9) N20-C25-S26-O27 38.1 (9) N60-C65-S66-O67 32.1 (9) C24-C25-S26-N29 105.8 (9) C64-C65-S66-N69 101.4 (9) N20-C25-S26-N29 −75.9 (9) N60-C65-S66-N69 −82.4 (9) O28-S26-O27-Pd1 −163.0 (4) O68-S66-O67-Pd42 −162.4 (4) N29-S26-O27-Pd1 67.2 (5) N69-S66-O67-Pd42 67.9 (5) C25-S26-O27-Pd1 −46.5 (5) C65-S66-O67-Pd42 −46.8 (5) C13-Pd1-O27-S26 110.6 (18) N50-Pd42-O67-S66 −137.0 (4) N10-Pd1-O27-S26 −139.6 (4) N60-Pd42-O67-S66 43.2 (4) N20-Pd1-O27-S26 39.5 (4) Pd41-Pd42-O67-S66 −66.6 (3) Pd2-Pd1-O27-S26 −67.9 (4) O68-S66-N69-C70 48.1 (9) O28-S26-N29-C30 41.6 (9) O67-S66-N69-C70 180.0 (7) O27-S26-N29-C30 174.6 (8) C65-S66-N69-C70 −67.8 (9) C25-S26-N29-C30 −74.3 (9) O68-S66-N69-Pd41 −147.7 (6) O28-S26-N29-Pd2 −144.5 (6) O67-S66-N69-Pd41 −15.9 (8) O27-S26-N29-Pd2 −11.5 (7) C65-S66-N69-Pd41 96.3 (7) C25-S26-N29-Pd2 99.5 (7) C72-Pd41-N69-C70 13.3 (7) C32-Pd2-N29-C30 16.1 (8) O48-Pd41-N69-C70 −158.7 (7)
O9-Pd2-N29-C30 −151.5 (7) Pd42-Pd41-N69-C70 136.2 (7) Pd1-Pd2-N29-C30 142.5 (8) C72-Pd41-N69-S66 −151.1 (7) C32-Pd2-N29-S26 −157.9 (7) O48-Pd41-N69-S66 36.9 (7)
O9-Pd2-N29-S26 34.6 (7) Pd42-Pd41-N69-S66 −28.2 (6) Pd1-Pd2-N29-S26 −31.4 (5) S66-N69-C70-C73 −109.2 (9)
S26-N29-C30-C33 −95.7 (10) Pd41-N69-C70-C73 84.7 (9) Pd2-N29-C30-C33 89.8 (10) S66-N69-C70-C71 130.2 (9) S26-N29-C30-C31 138.3 (8) Pd41-N69-C70-C71 −35.9 (10) Pd2-N29-C30-C31 −36.1 (10) C73-C70-C71-C72 −71.3 (13) N29-C30-C31-C37 161.0 (9) N69-C70-C71-C72 44.9 (12) C33-C30-C31-C37 37.4 (13) C73-C70-C71-C78 169.4 (10) N29-C30-C31-C38 −76.0 (11) N69-C70-C71-C78 −74.4 (12) C33-C30-C31-C38 160.4 (10) C73-C70-C71-C77 50.7 (14) N29-C30-C31-C32 41.1 (12) N69-C70-C71-C77 166.9 (9) C33-C30-C31-C32 −82.5 (12) C70-C71-C72-Pd41 −36.8 (11) C37-C31-C32-Pd2 −153.0 (8) C78-C71-C72-Pd41 82.9 (10) C38-C31-C32-Pd2 86.2 (10) C77-C71-C72-Pd41 −159.7 (8) C30-C31-C32-Pd2 −30.3 (11) N69-Pd41-C72-C71 13.3 (8) N29-Pd2-C32-C31 9.2 (8) N41-Pd41-C72-C71 −167.0 (8)
N1-Pd2-C32-C31 −169.6 (8) Pd42-Pd41-C72-C71 −56.8 (9) O9-Pd2-C32-C31 123.9 (15) N69-C70-C73-O74 −37.3 (17) Pd1-Pd2-C32-C31 −59.0 (9) C71-C70-C73-O74 77.8 (16) N29-C30-C33-O34 129.1 (13) N69-C70-C73-O75 148.0 (10) C31-C30-C33-O34 −109.8 (13) C71-C70-C73-O75 −96.8 (12) N29-C30-C33-O35 −47.0 (14) O74-C73-O75-C76 −2.9 (17) C31-C30-C33-O35 74.0 (13) C70-C73-O75-C76 172.2 (10)
Tabla 4. Parámetros de desplazamiento anisotrópico (Å2 x 103) para 25. El factor exponencial del desplazamiento anisotrópico tiene la siguiente forma: -2 2 [ h2 a*2 U11 + ... + 2 h k a* b* U12 ].
U11 U22 U33 U12 U13 U23 Pd1 0.0079
(4)
0.0146 (4)
0.0131 (4)
0.0020 (4)
−0.0003
(4) 0.0005 (4) Pd2 0.0100
(4) 0.0114
(4) 0.0135
(4) 0.0007
(4) −0.0018
(4) −0.0013 (3) N1 0.007 (3) 0.017 (3) 0.017 (3) 0.000 (3) −0.001 (3) −0.002 (2) C2 0.011 (4) 0.021 (3) 0.019 (3) −0.003
(3) 0.000 (3) −0.005 (3)
C3 0.011 (4) 0.024 (4) 0.021 (4) −0.001
(3) −0.001 (3) −0.009 (3) C4 0.013 (4) 0.027 (4) 0.019 (4) 0.003 (3) −0.005 (3) −0.008 (3) C5 0.009 (4) 0.024 (3) 0.016 (3) 0.006 (3) −0.001 (3) −0.006 (3) C6 0.005 (3) 0.019 (3) 0.015 (3) 0.000 (3) 0.001 (3) −0.002 (2) S7 0.0109
(13) 0.0140
(13) 0.0163
(13) 0.0013
(11) 0.0000
(11) 0.0005 (11) O8 0.016 (3) 0.021 (3) 0.017 (3) −0.001
(3) 0.006 (3) 0.003 (3) O9 0.009 (3) 0.012 (3) 0.020 (3) −0.002
(2) 0.000 (2) 0.000 (2) N10 0.006 (2) 0.019 (3) 0.015 (2) 0.002 (2) 0.001 (2) 0.004 (2) C11 0.009 (3) 0.017 (3) 0.016 (3) 0.001 (2) −0.002 (2) 0.005 (3) C12 0.009 (2) 0.021 (3) 0.018 (3) −0.001
(3) −0.001 (2) 0.006 (3) C13 0.009 (3) 0.020 (4) 0.018 (3) 0.003 (3) 0.001 (2) 0.004 (3) C14 0.012 (4) 0.021 (4) 0.017 (4) −0.002
(3) 0.001 (4) 0.009 (3) C15 0.011 (3) 0.023 (4) 0.019 (4) 0.000 (3) −0.005 (3) 0.005 (4) C16 0.016 (3) 0.017 (3) 0.020 (3) 0.003 (3) −0.002 (3) 0.006 (3) O17 0.024 (4) 0.017 (3) 0.025 (4) 0.001 (3) −0.002 (3) 0.003 (3) O18 0.015 (3) 0.020 (3) 0.026 (3) 0.005 (3) −0.004 (3) 0.010 (3) C19 0.021 (4) 0.025 (4) 0.035 (5) 0.005 (4) −0.004 (4) 0.015 (4) N20 0.013 (3) 0.006 (3) 0.015 (2) 0.004 (3) 0.001 (2) 0.002 (3) C21 0.016 (3) 0.011 (4) 0.015 (3) 0.004 (3) 0.001 (3) 0.002 (3) C22 0.019 (3) 0.012 (4) 0.014 (3) 0.003 (3) 0.003 (3) 0.002 (3) C23 0.020 (4) 0.012 (4) 0.014 (3) 0.004 (3) −0.002 (3) −0.003 (3) C24 0.020 (3) 0.013 (4) 0.015 (3) 0.003 (3) −0.004 (3) 0.001 (3) C25 0.016 (3) 0.008 (3) 0.014 (2) 0.003 (3) 0.000 (2) 0.001 (3) S26 0.0100
(12) 0.0128
(13) 0.0162
(13) 0.0021
(11) −0.0039
(11) −0.0013 (11) O27 0.011 (2) 0.012 (3) 0.017 (3) −0.002
(3) −0.003 (2) −0.001 (2) O28 0.010 (3) 0.018 (3) 0.023 (3) −0.001
(3) −0.009 (2) −0.002 (3) N29 0.012 (3) 0.013 (2) 0.013 (2) 0.002 (2) −0.001 (2) −0.002 (2) C30 0.017 (3) 0.014 (3) 0.016 (3) 0.004 (2) 0.000 (2) 0.002 (2) C31 0.018 (3) 0.015 (3) 0.018 (3) 0.001 (3) 0.001 (3) 0.003 (2) C32 0.014 (4) 0.014 (3) 0.020 (3) 0.001 (3) 0.000 (3) 0.004 (3)
C33 0.017 (3) 0.023 (3) 0.022 (3) 0.007 (3) −0.002 (3) 0.002 (3) O34 0.022 (4) 0.026 (4) 0.025 (3) 0.007 (3) −0.007 (3) 0.001 (3) O35 0.014 (3) 0.032 (4) 0.024 (3) 0.010 (3) −0.002 (3) −0.001 (3) C36 0.015 (4) 0.038 (5) 0.029 (4) 0.010 (4) 0.000 (4) −0.004 (4) C37 0.022 (4) 0.013 (3) 0.015 (4) 0.002 (3) 0.001 (4) 0.001 (3) C38 0.017 (4) 0.018 (4) 0.019 (4) 0.003 (4) 0.000 (4) 0.001 (4) Pd41 0.0114
(4) 0.0125
(4) 0.0185
(5) 0.0018
(4) −0.0043
(4) −0.0005 (4) Pd42 0.0136
(4) 0.0118
(4) 0.0147
(4) 0.0025
(4) −0.0016
(4) −0.0020 (3) N41 0.017 (2) 0.016 (4) 0.021 (3) 0.000 (3) −0.005 (2) 0.002 (3) C42 0.016 (3) 0.021 (4) 0.025 (3) −0.003
(3) −0.008 (3) 0.003 (3) C43 0.019 (3) 0.025 (4) 0.026 (4) −0.003
(4) −0.008 (3) 0.002 (4) C44 0.021 (4) 0.025 (4) 0.026 (3) −0.005
(3) −0.008 (3) 0.005 (4) C45 0.020 (3) 0.022 (4) 0.023 (3) −0.005
(3) −0.005 (3) 0.006 (4) C46 0.018 (3) 0.019 (4) 0.022 (3) −0.002
(3) −0.003 (2) 0.006 (3) S47 0.0209
(14) 0.0177
(14) 0.0157
(14) 0.0079
(12) −0.0041
(11) −0.0041 (12) O48 0.022 (3) 0.015 (3) 0.015 (3) 0.005 (3) −0.004 (2) −0.006 (2) O49 0.027 (3) 0.025 (3) 0.017 (3) 0.009 (3) 0.001 (3) −0.006 (3) N50 0.021 (3) 0.018 (2) 0.017 (2) 0.003 (3) −0.002 (2) 0.000 (2) C51 0.034 (3) 0.023 (3) 0.026 (3) 0.005 (3) −0.004 (3) 0.006 (3) C52 0.038 (4) 0.021 (3) 0.033 (3) 0.001 (3) −0.001 (3) 0.007 (2) C53 0.041 (5) 0.016 (3) 0.029 (3) 0.002 (3) −0.002 (4) 0.005 (3) C54 0.044 (4) 0.037 (3) 0.027 (3) 0.005 (4) −0.006 (3) 0.009 (3) O55 0.049 (4) 0.045 (4) 0.033 (4) 0.008 (4) 0.003 (3) 0.006 (4) O56 0.054 (4) 0.048 (4) 0.028 (3) −0.002
(4) −0.012 (3) 0.011 (3) C57 0.065 (6) 0.054 (6) 0.027 (4) −0.004
(5) −0.010 (5) 0.011 (5) C58 0.046 (5) 0.021 (4) 0.036 (5) 0.003 (4) −0.001 (5) 0.011 (4) C59 0.039 (4) 0.027 (5) 0.042 (5) −0.003
(4) −0.002 (4) 0.009 (4) N60 0.006 (3) 0.013 (2) 0.021 (2) 0.000 (3) −0.004 (3) −0.001 (2) C61 0.007 (2) 0.014 (2) 0.021 (2) 0.002 (2) −0.003 (2) −0.0021
(18)
C62 0.006 (2) 0.014 (2) 0.021 (2) 0.002 (2) −0.002 (2) −0.0020 (18) C63 0.005 (2) 0.014 (2) 0.021 (2) 0.0020
(19) −0.002 (2) −0.0018 (17) C64 0.005 (2) 0.014 (2) 0.021 (2) 0.0024
(19) −0.002 (2) −0.0016 (17) C65 0.005 (2) 0.014 (2) 0.021 (2) 0.003 (2) −0.002 (2) −0.0013
(18) S66 0.0127
(12) 0.0109
(12) 0.0159
(13) 0.0006
(12) −0.0027
(11) −0.0018 (10) O67 0.007 (2) 0.012 (3) 0.017 (3) −0.004
(3) −0.002 (2) −0.001 (2) O68 0.016 (3) 0.009 (3) 0.021 (3) −0.001
(3) −0.007 (3) 0.001 (2) N69 0.011 (2) 0.017 (3) 0.016 (2) 0.000 (2) −0.0010
(19) 0.000 (2) C70 0.013 (3) 0.019 (3) 0.018 (3) 0.001 (2) −0.001 (2) 0.000 (3) C71 0.015 (3) 0.019 (3) 0.022 (3) 0.003 (3) 0.000 (2) −0.003 (3) C72 0.011 (3) 0.016 (4) 0.021 (3) 0.001 (3) −0.002 (3) −0.001 (3) C73 0.021 (3) 0.023 (3) 0.022 (3) −0.004
(3) −0.004 (3) 0.003 (3) O74 0.025 (4) 0.024 (4) 0.026 (4) −0.007
(3) −0.005 (3) 0.002 (3) O75 0.035 (4) 0.034 (4) 0.026 (3) −0.013
(3) −0.003 (3) 0.009 (3) C76 0.049 (5) 0.038 (5) 0.031 (5) −0.019
(4) −0.002 (5) 0.010 (4) C77 0.017 (4) 0.018 (4) 0.020 (4) 0.004 (3) 0.001 (3) −0.003 (4) C78 0.014 (4) 0.021 (4) 0.026 (4) 0.004 (3) −0.005 (4) −0.005 (4) C1W 0.030
(10) 0.13 (2) 0.105
(17) −0.002
(12) 0.025 (11) −0.071 (16) Cl1A 0.068 (5) 0.164
(12) 0.216
(14) −0.037
(7) 0.071 (7) −0.089 (10) Cl1B 0.068 (5) 0.164
(12) 0.216
(14) −0.037
(7) 0.071 (7) −0.089 (10) Cl2 0.076 (4) 0.062 (3) 0.097 (4) −0.005
(3) 0.001 (3) −0.008 (3)