Oct 26, 1994 - ... M. G., Medina, A. & Dfaz-Gonz~ilez, M. C. (1987). Acta Cryst. C43, 134-136. Sheldrick, G. M. (1976). SHELX76. Program for Crystal Structure.
1018
C28H24N204S2
Rodrfguez, M. L., Medina de la Rosa, E., Gili, P., Martfn-Zarza, P., Martfn-Reyes, M. G., Medina, A. & Dfaz-Gonz~ilez,M. C. (1987). Acta Cryst. C43, 134-136. Sheldrick, G. M. (1976). SHELX76. Programfor Crystal Structure Determination. Univ. of Cambridge, England. West, D. X. & Pannell, L. K. (1989). TransitionMet. Chem. 14, 457460.
C34. 2o-(/)1
1019
Refinement Refinement on F 2
R[F 2 > 2o-(F2)] = 0.0400 wR(F 2) = 0.0919 S = 0.635 5420 reflections 450 parameters H atoms were refined using a riding model, refining Uiso in groups
w = 1/[cr2(Fo2) + (0.1000P) 2] where P = (F 2 + 2Fc2)/3 ( m / o ' ) m a x -- 0 . 0 5 8 mpmax = 0.193 e /~,- 3 mpmin = -0.171 e ,~-s Extinction correction: none Atomic scattering factors from International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
Table 1. Fractional atomic coordinates and equivalent
isotropic displacement parameters (~ 2) x
Ueq = (1/3)EiEjUoa~ aTai.aj. y z
Ueq
C1 Ol C2 C3 03 C4 C5 05 C6 06 Cll Ci2 C13 C14 C15 C16 C17 N 18 C19 020 C21 C22 023 C24
0.8320 (3) 0.9069 (2) 0.7924 (3) 0.7113 (3) 0.6668 (2) 0.6308 (2) 0.6797 (3) 0.7541 (2) 0.6079 (3) 0.5440 (2) 0.9601 (3) 1.0689 (3) 1.1178 (3) i.2192(3) !.2725 (4) !.2258 (4) 1.1241 (4) 0.8722 (2) 0.9056 (4) 0.8639(3) 0.9973 (5) 0.6609 (3) 0.6904 (2) 0.6142 (3)
0.8224 (3) 0.8163 (2) 0.8789 (3) 0.8824 (2) 0.9313 (2) 0.7772 (2) 0.7254 (3) 0.7238 (2) 0.6196 (3) 0.5605 (2) 0.7795 (4) 0.8300 (3) 0.7752 (3) 0.8204(4) 0.9201 (4) 0.9761 (3) 0.9312 (3) 0.9776 (2) 1.13019 (3) 0.9451 (2) 1.1044 (4) 1.13069 (2) 1.0338 (2) 1.0513 (2)
-0.0194 (1) -0.0458 (!) -0.0498 (1) -0.0186 (1) -0.0454 (1) -0.0048 (1) 0.0223 (1) -0.0087 (1) 0.0386 (1) -0.13003 (1) -0.0165 (1) -0.0319 (1) -0.0323 (1) -0.0443 (i) -0.0556 (2) -0.0546 (2) -0.0433 (1) - 0.0628 (!) -0.1085 (2) -0.1431 (1) -0.1147 (2) -0.0222 (2) 0.0187 (1) -0.0532 (1)
0.0399 (9) 0.0517 (7) 0.0368 (8) 0.0338 (8) 0.0381 (5) 0.0352 (8) 0.0397 (8) 0.0418 (6) 0.0458 (9) 0.0473 (6) 0.0582 (12) 0.0433 (9) 0.0455 (9) 0.0616(11) 0.0711 (13) 0.0747 (14) 0.0609 (11) 0.0388 (7) 0.0594 (12) 0.0836(il) 0.096 (2) 0.0381 (8) 0.0550 (7) 0.0405 (9)
c25
0.5964 (3)
1.0302(3)
-0.1022(2)
0.0558 (11)
C26 C27 C28 C29 Si30 C31 C32 C33 C34 C35 C36 C37 C38 C39 C40 C41 C42 C43 C44 C45 C46 N47 N48 N49
0.5593 (4) 0.5404 (3) 0.5556 (3) 0.5929 (3) 0.49074 (7) 0.4225 (3) 0.3583 (3) 0.4994 (4) 0.3537 (4) 0.5958 (2) 0.5986 (3) 0.6828 (4) 0.7656 (4) 0.7659 (3) 0.6841 (3) 0.3986 (3) 0.3686 (4) 0.2968 (4) 0.2552 (4) 0.2822 (5) 0.3537 (3) 0.5572 (2) 0.4700 (3) 0.3856 (4)
1.0813 (4) 1.1515 (3) 1.1703 (3) 1.1209 (3) 0.43650 (7) 0.3885 (3) 0.2735 (3) 0.4187 (4) 0.4331 (4) 0.4096 (2) 0.3441 (3) 0.3329 (4) 0.3863 (4) 0.4532 (4) 0.4654 (3) 0.3934 (3) 0.3068 (4) 0.2811 (5) 0.3439 (7) 0.4241 (6) 0.4497 (4) 0.7827 (2) 0.7349 (3) 0.6910 (5)
-0.1297 (2) -0.1071 (2) -0.0590 (2) -0.0319 (2) 0.130251(3) -0.0573 (1) -0.0564 (2) -0.0995 (1) -0.0660 (2) 0.0117 (1) 0.0452 (1) 0.0506 (2) 0.0233 (2) -0.0096 (2) -0.0151 (2) 0.0544 (1) 0.0829 (2) 0.1203 (2) 0.1279 (2) 0.1009 (3) 0.0659 (2) 0.0285 (1) 0.0164 (1) 0.0097 (2)
0.0748 (14) 0.0685 (13) 0.0625 (12) 0.0540 (10) 0.0385 (2) 0.0491 (9) 0.0582(11) 0.0753 (14) 0.095 (2) 0.0357 (8) 0.0626 (12) 0.0700 (! 3) 0.0686 (12) 0.0794 (14) 0.0592 (11) 0.0487 (10) 0.0756 (14) 0.105 (2) 0.107 (3) 0.I 12 (2) 0.0807 (15) 0.0446 (8) 0.0636 (10) 0.120 (2)
Riot = 0.0914
0max ---- 25.09 °
h = - 9 - - - * 16 k = - 1 6 - - - * 14 l = - 2 2 ---* 29
Table 2. Selected geometric parameters (,~, o) C 1---O1 C I------O5 C 1~C2
1.395 (4) !.406 (4) i.526 (4)
C5---O5 C5----C6 C6---4)6
1.429 (4) 1.498 (5) 1.423 (4)
1020 0 1 - - c 11 C2--N18 C2---C3 C3---O3 C 3---C4 O3---C22 C4---N47 C4---C5 O1---C1---O5 O1---C1---C'2 O5----C1---C'2 C1----O1----Cll N18----C2----C1 N18----C2----C3 C1---C2---C3 O3---C3-----C4 O3----C3----C2 C4----~3----C2 C22---O3----C3 N47----C4----C3 N47---C4---C5 C3--C4---C5 O5----C5----C6 C3----C4---N47--N48 C5----C6---
