Daten Röntgenkristallstrukturanalyse 136a
Table 1. Crystal data and structure refinement for 136a.
|
1.1.159. Empirical formula |
1.1.160. C21 H26 N2 O2 |
|
|
1.1.161. Formula weight |
1.1.162. 338.44 |
|
|
1.1.163. Temperature |
1.1.164. 100(2) K |
|
|
1.1.165. Wavelength |
1.1.166. 0.71073 A |
|
|
1.1.167. Crystal system, space group |
1.1.168. Monoclinic, P 21 |
|
|
1.1.169. Unit cell dimensions |
1.1.170. a = 8.462 A |
1.1.171. alpha = 90 deg. |
|
1.1.172. |
1.1.173. b = 19.757 A |
1.1.174. beta = 102.02 deg. |
|
1.1.175. |
1.1.176. c = 11.404 A |
1.1.177. gamma = 90 deg. |
|
1.1.178. Volume |
1.1.179. 1864.7 A^3 |
|
|
1.1.180. Z, Calculated density |
1.1.181. 4, 1.206 Mg/m^3 |
|
|
1.1.182. Absorption coefficient |
1.1.183. 0.078 mm^-1 |
|
|
1.1.184. F(000) |
1.1.185. 728 |
|
|
1.1.186. Crystal size |
1.1.187. 0.40 x 0.20 x 0.04 mm |
|
|
1.1.188. Theta range for data collection |
1.1.189. 3.36 to 28.00 deg. |
|
|
1.1.190. Limiting indices |
1.1.191. -11<=h<=10, -24<=k<=26, 0<=l<=15 |
|
|
1.1.192. Reflections collected / unique |
1.1.193. 7976 / 7976 [R(int) = 0.0000] |
|
|
1.1.194. Completeness to theta = 28.00 |
1.1.195. 99.5 % |
|
|
1.1.196. Max. and min. transmission |
1.1.197. 0.9969 and 0.9696 |
|
|
1.1.198. Refinement method |
1.1.199. Full-matrix least-squares on F^2 |
|
|
1.1.200. Data / restraints / parameters |
1.1.201. 7976 / 1 / 473 |
|
|
1.1.202. Goodness-of-fit on F^2 |
1.1.203. 0.916 |
|
|
1.1.204. Final R indices [I>2sigma(I)] |
1.1.205. R1 = 0.0548, wR2 = 0.0904 |
|
|
1.1.206. R indices (all data) |
1.1.207. R1 = 0.0863, wR2 = 0.0985 |
|
|
1.1.208. Absolute structure parameter |
1.1.209. 0.2(13) |
|
|
1.1.210. Extinction coefficient |
1.1.211. 0.0054(7) |
|
|
1.1.212. Largest diff. peak and hole |
1.1.213. 0.208 and -0.205 e.A^-3 |
|
Table 2. Atomic coordinates (x104) and equivalent isotropic displacement parameters (A2x103) for 136a. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
|
x |
y |
z |
U(eq) |
|
|
C(1) |
-2994(4) |
-604(2) |
-599(2) |
14(1) |
|
C(2) |
-3481(4) |
-111(2) |
1241(3) |
16(1) |
|
C(3) |
-5179(4) |
151(2) |
760(3) |
20(1) |
|
C(4) |
-6024(4) |
302(2) |
1796(3) |
21(1) |
|
C(5) |
-7743(5) |
546(2) |
1336(3) |
33(1) |
|
C(6) |
-5987(4) |
-319(2) |
2591(3) |
21(1) |
|
C(7) |
-4274(4) |
-581(2) |
3032(2) |
19(1) |
|
C(8) |
-3448(3) |
-757(1) |
1991(2) |
14(1) |
|
C(9) |
-1747(4) |
-1054(1) |
2403(2) |
17(1) |
|
C(10) |
-604(4) |
-615(2) |
3305(3) |
27(1) |
|
C(11) |
-1846(4) |
-1771(2) |
2893(3) |
24(1) |
|
C(12) |
-781(4) |
-60(1) |
-1332(2) |
17(1) |
|
C(13) |
356(4) |
-110(2) |
-1969(3) |
19(1) |
|
C(14) |
464(4) |
-698(2) |
-2715(2) |
18(1) |
|
C(15) |
1810(4) |
-832(2) |
-3199(3) |
22(1) |
|
C(16) |
1881(4) |
-1409(2) |
-3865(3) |
21(1) |
|
C(17) |
623(4) |
-1868(2) |
-4042(3) |
21(1) |
|
C(18) |
-729(4) |
-1746(2) |
-3563(2) |
17(1) |
|
C(19) |
-815(4) |
-1158(2) |
-2918(2) |
15(1) |
|
C(20) |
-2317(4) |
-1003(2) |
-2443(2) |
16(1) |
|
C(21) |
-3575(4) |
-677(2) |
-3392(3) |
20(1) |
|
C(22) |
-5326(4) |
-2757(1) |
-3252(2) |
14(1) |
|
C(23) |
-4733(4) |
-3154(2) |
-5084(2) |
17(1) |
|
C(24) |
-3289(4) |
-3609(2) |
-4707(3) |
19(1) |
|
C(25) |
-2247(4) |
-3621(2) |
-5647(3) |
22(1) |
|
C(26) |
-785(4) |
-4084(2) |
-5268(3) |
28(1) |
|
C(27) |
-3295(4) |
-3842(2) |
-6842(2) |
20(1) |
|
C(28) |
-4785(4) |
-3401(2) |
-7215(2) |
20(1) |
|
C(29) |
-5825(4) |
-3372(1) |
-6256(2) |
16(1) |
|
C(30) |
-7339(4) |
-2926(2) |
-6615(2) |
19(1) |
|
C(31) |
-8512(4) |
-3216(2) |
-7700(3) |
29(1) |
|
C(32) |
-6966(4) |
-2182(2) |
-6825(3) |
25(1) |
|
C(33) |
-7502(4) |
-3342(2) |
-2555(2) |
16(1) |
|
C(34) |
-8643(4) |
-3325(1) |
-1924(2) |
18(1) |
|
C(35) |
-8808(4) |
-2740(1) |
-1173(2) |
15(1) |
|
C(36) |
-10196(4) |
-2619(2) |
-729(2) |
17(1) |
|
C(37) |
-10325(4) |
-2040(2) |
-69(2) |
17(1) |
|
C(38) |
-9079(4) |
-1575(2) |
148(2) |
17(1) |
|
C(39) |
-7703(4) |
-1686(1) |
-299(2) |
16(1) |
|
C(40) |
-7567(4) |
-2262(1) |
-948(2) |
14(1) |
|
C(41) |
-6034(4) |
-2394(1) |
-1403(2) |
15(1) |
|
C(42) |
-4765(4) |
-2711(2) |
-463(2) |
19(1) |
|
N(1) |
-1981(3) |
-556(1) |
-1395(2) |
15(1) |
|
N(2) |
-4545(4) |
-419(2) |
-4102(2) |
32(1) |
|
N(3) |
-6335(3) |
-2835(1) |
-2464(2) |
13(1) |
|
N(4) |
-3774(3) |
-2959(2) |
240(2) |
28(1) |
|
O(1) |
-2543(3) |
-165(1) |
301(2) |
17(1) |
|
O(2) |
-4111(3) |
-999(1) |
-723(2) |
19(1) |
|
O(3) |
-5726(3) |
-3180(1) |
-4174(2) |
17(1) |
|
O(4) |
-4236(3) |
-2353(1) |
-3109(2) |
20(1) |
Table 3. Bond lengths [A] and angles [deg] for 136a.
|
C(1)-O(2) |
1.210(3) |
C(9)-C(11)-H(11A) |
109.5 |
|
C(1)-O(1) |
1.338(3) |
C(9)-C(11)-H(11B) |
109.5 |
|
C(1)-N(1) |
1.374(3) |
H(11A)-C(11)-H(11B) |
109.5 |
|
C(2)-O(1) |
1.464(3) |
C(9)-C(11)-H(11C) |
109.5 |
|
C(2)-C(3) |
1.518(5) |
H(11A)-C(11)-H(11C) |
109.5 |
|
C(2)-C(8) |
1.533(4) |
H(11B)-C(11)-H(11C) |
109.5 |
|
C(2)-H(2) |
0.97(3) |
C(13)-C(12)-N(1) |
121.4(3) |
|
C(3)-C(4) |
1.533(4) |
C(13)-C(12)-H(12) |
119.3 |
|
C(3)-H(3A) |
0.9900 |
N(1)-C(12)-H(12) |
119.3 |
|
C(3)-H(3B) |
0.9900 |
C(12)-C(13)-C(14) |
121.4(3) |
|
C(4)-C(5) |
1.519(5) |
C(12)-C(13)-H(13) |
119.3 |
|
C(4)-C(6) |
1.522(4) |
C(14)-C(13)-H(13) |
119.3 |
|
C(4)-H(4) |
0.98(3) |
C(15)-C(14)-C(19) |
118.8(3) |
|
C(5)-H(5A) |
0.9800 |
C(15)-C(14)-C(13) |
122.7(3) |
|
C(5)-H(5B) |
0.9800 |
C(19)-C(14)-C(13) |
118.4(3) |
|
C(5)-H(5C) |
0.9800 |
C(16)-C(15)-C(14) |
120.6(3) |
|
C(6)-C(7) |
1.522(4) |
C(16)-C(15)-H(15) |
119.7 |
|
C(6)-H(6A) |
0.9900 |
C(14)-C(15)-H(15) |
119.7 |
|
C(6)-H(6B) |
0.9900 |
C(15)-C(16)-C(17) |
120.3(3) |
|
C(7)-C(8) |
1.537(3) |
C(15)-C(16)-H(16) |
119.9 |
|
C(7)-H(7A) |
0.9900 |
C(17)-C(16)-H(16) |
119.9 |
|
C(7)-H(7B) |
0.9900 |
C(16)-C(17)-C(18) |
120.0(3) |
|
C(8)-C(9) |
1.535(4) |
C(16)-C(17)-H(17) |
120.0 |
|
C(8)-H(8) |
1.0000 |
C(18)-C(17)-H(17) |
120.0 |
|
C(9)-C(10) |
1.527(4) |
C(19)-C(18)-C(17) |
119.6(3) |
|
C(9)-C(11) |
1.531(4) |
C(19)-C(18)-H(18) |
120.2 |
|
C(9)-H(9) |
1.0000 |
C(17)-C(18)-H(18) |
120.2 |
|
C(10)-H(10A) |
0.9800 |
C(18)-C(19)-C(14) |
120.6(3) |
|
C(10)-H(10B) |
0.9800 |
C(18)-C(19)-C(20) |
120.1(3) |
|
C(10)-H(10C) |
0.9800 |
C(14)-C(19)-C(20) |
119.3(3) |
|
C(11)-H(11A) |
0.9800 |
N(1)-C(20)-C(21) |
108.6(2) |
|
C(11)-H(11B) |
0.9800 |
N(1)-C(20)-C(19) |
112.3(2) |
|
C(11)-H(11C) |
0.9800 |
C(21)-C(20)-C(19) |
110.6(2) |
|
C(12)-C(13) |
1.325(4) |
N(1)-C(20)-H(20) |
108.4 |
|
C(12)-N(1) |
1.402(4) |
C(21)-C(20)-H(20) |
108.4 |
|
C(12)-H(12) |
0.9500 |
C(19)-C(20)-H(20) |
108.4 |
|
C(13)-C(14) |
1.454(4) |
N(2)-C(21)-C(20) |
178.7(3) |
|
C(13)-H(13) |
0.9500 |
O(4)-C(22)-O(3) |
125.8(2) |
|
C(14)-C(15) |
1.390(4) |
O(4)-C(22)-N(3) |
123.4(2) |
|
C(14)-C(19) |
1.395(4) |
O(3)-C(22)-N(3) |
110.8(2) |
|
C(15)-C(16) |
1.378(4) |
O(3)-C(23)-C(24) |
109.1(2) |
|
C(15)-H(15) |
0.9500 |
O(3)-C(23)-C(29) |
106.2(2) |
|
C(16)-C(17) |
1.381(5) |
C(24)-C(23)-C(29) |
113.0(2) |
|
C(16)-H(16) |
0.9500 |
O(3)-C(23)-H(23) |
109.5 |
|
C(17)-C(18) |
1.388(4) |
C(24)-C(23)-H(23) |
109.5 |
|
C(17)-H(17) |
0.9500 |
C(29)-C(23)-H(23) |
109.5 |
|
C(18)-C(19) |
1.385(4) |
C(23)-C(24)-C(25) |
111.2(2) |
|
C(18)-H(18) |
0.9500 |
C(23)-C(24)-H(24A) |
109.4 |
|
C(19)-C(20) |
1.513(4) |
C(25)-C(24)-H(24A) |
109.4 |
|
C(20)-N(1) |
1.466(3) |
C(23)-C(24)-H(24B) |
109.4 |
|
C(20)-C(21) |
1.497(4) |
C(25)-C(24)-H(24B) |
109.4 |
|
C(20)-H(20) |
1.0000 |
H(24A)-C(24)-H(24B) |
108.0 |
|
C(21)-N(2) |
1.145(4) |
C(24)-C(25)-C(27) |
108.6(3) |
|
C(22)-O(4) |
1.204(3) |
C(24)-C(25)-C(26) |
111.3(3) |
|
C(22)-O(3) |
1.332(3) |
C(27)-C(25)-C(26) |
111.4(3) |
|
C(22)-N(3) |
1.372(4) |
C(24)-C(25)-H(25) |
108.5 |
|
C(23)-O(3) |
1.466(3) |
C(27)-C(25)-H(25) |
108.5 |
|
C(23)-C(24) |
1.506(4) |
C(26)-C(25)-H(25) |
108.5 |
|
C(23)-C(29) |
1.520(4) |
C(25)-C(26)-H(26A) |
109.5 |
|
C(23)-H(23) |
1.0000 |
C(25)-C(26)-H(26B) |
109.5 |
|
C(24)-C(25) |
1.523(4) |
H(26A)-C(26)-H(26B) |
109.5 |
|
C(24)-H(24A) |
0.9900 |
C(25)-C(26)-H(26C) |
109.5 |
|
C(24)-H(24B) |
0.9900 |
H(26A)-C(26)-H(26C) |
109.5 |
|
C(25)-C(27) |
1.527(4) |
H(26B)-C(26)-H(26C) |
109.5 |
|
C(25)-C(26) |
1.528(5) |
C(28)-C(27)-C(25) |
112.3(2) |
|
C(25)-H(25) |
1.0000 |
C(28)-C(27)-H(27A) |
109.1 |
|
C(26)-H(26A) |
0.9800 |
C(25)-C(27)-H(27A) |
109.1 |
|
C(26)-H(26B) |
0.9800 |
C(28)-C(27)-H(27B) |
109.1 |
|
C(26)-H(26C) |
0.9800 |
C(25)-C(27)-H(27B) |
109.1 |
|
C(27)-C(28) |
1.519(4) |
H(27A)-C(27)-H(27B) |
107.9 |
|
C(27)-H(27A) |
0.9900 |
C(27)-C(28)-C(29) |
112.7(2) |
|
C(27)-H(27B) |
0.9900 |
C(27)-C(28)-H(28A) |
109.1 |
|
C(28)-C(29) |
1.540(4) |
C(29)-C(28)-H(28A) |
109.1 |
|
C(28)-H(28A) |
0.9900 |
C(27)-C(28)-H(28B) |
109.1 |
|
C(28)-H(28B) |
0.9900 |
C(29)-C(28)-H(28B) |
109.1 |
|
C(29)-C(30) |
1.539(4) |
H(28A)-C(28)-H(28B) |
107.8 |
|
C(29)-H(29) |
1.0000 |
C(23)-C(29)-C(30) |
113.0(2) |
|
C(30)-C(31) |
1.528(4) |
C(23)-C(29)-C(28) |
107.6(2) |
|
C(30)-C(32) |
1.532(4) |
C(30)-C(29)-C(28) |
113.5(2) |
|
C(30)-H(30) |
1.0000 |
C(23)-C(29)-H(29) |
107.5 |
|
C(31)-H(31A) |
0.9800 |
C(30)-C(29)-H(29) |
107.5 |
|
C(31)-H(31B) |
0.9800 |
C(28)-C(29)-H(29) |
107.5 |
|
C(31)-H(31C) |
0.9800 |
C(31)-C(30)-C(32) |
110.7(3) |
|
C(32)-H(32A) |
0.9800 |
C(31)-C(30)-C(29) |
111.4(2) |
|
C(32)-H(32B) |
0.9800 |
C(32)-C(30)-C(29) |
113.8(3) |
|
C(32)-H(32C) |
0.9800 |
C(31)-C(30)-H(30) |
106.8 |
|
C(33)-C(34) |
1.320(4) |
C(32)-C(30)-H(30) |
106.8 |
|
C(33)-N(3) |
1.394(4) |
C(29)-C(30)-H(30) |
106.8 |
|
C(33)-H(33) |
0.9500 |
C(30)-C(31)-H(31A) |
109.5 |
|
C(34)-C(35) |
1.462(4) |
C(30)-C(31)-H(31B) |
109.5 |
|
C(34)-H(34) |
0.9500 |
H(31A)-C(31)-H(31B) |
109.5 |
|
C(35)-C(36) |
1.394(4) |
C(30)-C(31)-H(31C) |
109.5 |
|
C(35)-C(40) |
1.395(4) |
H(31A)-C(31)-H(31C) |
109.5 |
|
C(36)-C(37) |
1.385(4) |
H(31B)-C(31)-H(31C) |
109.5 |
|
C(36)-H(36) |
0.9500 |
C(30)-C(32)-H(32A) |
109.5 |
|
C(37)-C(38) |
1.383(4) |
C(30)-C(32)-H(32B) |
109.5 |
|
C(37)-H(37) |
0.9500 |
H(32A)-C(32)-H(32B) |
109.5 |
|
C(38)-C(39) |
1.382(4) |
C(30)-C(32)-H(32C) |
109.5 |
|
C(38)-H(38) |
0.9500 |
H(32A)-C(32)-H(32C) |
109.5 |
|
C(39)-C(40) |
1.376(4) |
H(32B)-C(32)-H(32C) |
109.5 |
|
C(39)-H(39) |
0.9500 |
C(34)-C(33)-N(3) |
121.9(3) |
|
C(40)-C(41) |
1.517(4) |
C(34)-C(33)-H(33) |
119.1 |
|
C(41)-N(3) |
1.469(3) |
N(3)-C(33)-H(33) |
119.1 |
|
C(41)-C(42) |
1.489(4) |
C(33)-C(34)-C(35) |
120.6(3) |
|
C(41)-H(41) |
1.0000 |
C(33)-C(34)-H(34) |
119.7 |
|
C(42)-N(4) |
1.142(4) |
C(35)-C(34)-H(34) |
119.7 |
|
C(36)-C(35)-C(40) |
118.4(3) |
||
|
O(2)-C(1)-O(1) |
126.7(3) |
C(36)-C(35)-C(34) |
122.6(3) |
|
O(2)-C(1)-N(1) |
123.2(3) |
C(40)-C(35)-C(34) |
118.9(3) |
|
O(1)-C(1)-N(1) |
110.1(3) |
C(37)-C(36)-C(35) |
120.4(3) |
|
O(1)-C(2)-C(3) |
112.1(2) |
C(37)-C(36)-H(36) |
119.8 |
|
O(1)-C(2)-C(8) |
113.5(2) |
C(35)-C(36)-H(36) |
119.8 |
|
C(3)-C(2)-C(8) |
113.0(3) |
C(38)-C(37)-C(36) |
120.2(3) |
|
O(1)-C(2)-H(2) |
105.6(19) |
C(38)-C(37)-H(37) |
119.9 |
|
C(3)-C(2)-H(2) |
104(2) |
C(36)-C(37)-H(37) |
119.9 |
|
C(8)-C(2)-H(2) |
107.6(19) |
C(39)-C(38)-C(37) |
119.8(3) |
|
C(2)-C(3)-C(4) |
110.3(2) |
C(39)-C(38)-H(38) |
120.1 |
|
C(2)-C(3)-H(3A) |
109.6 |
C(37)-C(38)-H(38) |
120.1 |
|
C(4)-C(3)-H(3A) |
109.6 |
C(40)-C(39)-C(38) |
120.1(3) |
|
C(2)-C(3)-H(3B) |
109.6 |
C(40)-C(39)-H(39) |
120.0 |
|
C(4)-C(3)-H(3B) |
109.6 |
C(38)-C(39)-H(39) |
120.0 |
|
H(3A)-C(3)-H(3B) |
108.1 |
C(39)-C(40)-C(35) |
121.0(3) |
|
C(5)-C(4)-C(6) |
111.2(3) |
C(39)-C(40)-C(41) |
120.0(3) |
|
C(5)-C(4)-C(3) |
111.3(3) |
C(35)-C(40)-C(41) |
119.0(2) |
|
C(6)-C(4)-C(3) |
110.3(2) |
N(3)-C(41)-C(42) |
108.6(2) |
|
C(5)-C(4)-H(4) |
109.0(19) |
N(3)-C(41)-C(40) |
111.7(2) |
|
C(6)-C(4)-H(4) |
110.2(18) |
C(42)-C(41)-C(40) |
111.4(2) |
|
C(3)-C(4)-H(4) |
104.7(18) |
N(3)-C(41)-H(41) |
108.3 |
|
C(4)-C(5)-H(5A) |
109.5 |
C(42)-C(41)-H(41) |
108.3 |
|
C(4)-C(5)-H(5B) |
109.5 |
C(40)-C(41)-H(41) |
108.3 |
|
H(5A)-C(5)-H(5B) |
109.5 |
N(4)-C(42)-C(41) |
178.5(3) |
|
C(4)-C(5)-H(5C) |
109.5 |
C(1)-N(1)-C(12) |
124.0(2) |
|
H(5A)-C(5)-H(5C) |
109.5 |
C(1)-N(1)-C(20) |
117.1(2) |
|
H(5B)-C(5)-H(5C) |
109.5 |
C(12)-N(1)-C(20) |
118.5(2) |
|
C(4)-C(6)-C(7) |
111.7(3) |
C(22)-N(3)-C(33) |
124.1(2) |
|
C(4)-C(6)-H(6A) |
109.3 |
C(22)-N(3)-C(41) |
116.6(2) |
|
C(7)-C(6)-H(6A) |
109.3 |
C(33)-N(3)-C(41) |
119.1(2) |
|
C(4)-C(6)-H(6B) |
109.3 |
C(1)-O(1)-C(2) |
119.8(2) |
|
C(7)-C(6)-H(6B) |
109.3 |
C(22)-O(3)-C(23) |
116.6(2) |
|
H(6A)-C(6)-H(6B) |
107.9 |
C(10)-C(9)-C(11) |
110.8(3) |
|
C(6)-C(7)-C(8) |
112.2(2) |
C(10)-C(9)-C(8) |
114.3(2) |
|
C(6)-C(7)-H(7A) |
109.2 |
C(11)-C(9)-C(8) |
110.2(2) |
|
C(8)-C(7)-H(7A) |
109.2 |
C(10)-C(9)-H(9) |
107.1 |
|
C(6)-C(7)-H(7B) |
109.2 |
C(11)-C(9)-H(9) |
107.1 |
|
C(8)-C(7)-H(7B) |
109.2 |
C(8)-C(9)-H(9) |
107.1 |
|
H(7A)-C(7)-H(7B) |
107.9 |
C(9)-C(10)-H(10A) |
109.5 |
|
C(2)-C(8)-C(9) |
113.3(2) |
C(9)-C(10)-H(10B) |
109.5 |
|
C(2)-C(8)-C(7) |
106.5(2) |
H(10A)-C(10)-H(10B) |
109.5 |
|
C(9)-C(8)-C(7) |
113.5(2) |
C(9)-C(10)-H(10C) |
109.5 |
|
C(2)-C(8)-H(8) |
107.8 |
H(10A)-C(10)-H(10C) |
109.5 |
|
C(9)-C(8)-H(8) |
107.8 |
H(10B)-C(10)-H(10C) |
109.5 |
|
C(7)-C(8)-H(8) |
107.8 |
Table 4. Anisotropic displacement parameters (A^2 x 10^3) for 136a. The anisotropic displacement factor exponent takes the form: -2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ]
|
U11 |
U22 |
U33 |
U23 |
U13 |
U12 |
|
|
C(1) |
16(2) |
15(2) |
11(1) |
3(1) |
2(1) |
1(1) |
|
C(2) |
19(2) |
15(2) |
16(1) |
-6(1) |
6(1) |
-2(1) |
|
C(3) |
25(2) |
15(2) |
19(2) |
-1(1) |
4(1) |
4(1) |
|
C(4) |
14(2) |
18(2) |
29(2) |
-9(1) |
4(1) |
-2(1) |
|
C(5) |
31(2) |
29(2) |
38(2) |
-7(2) |
4(2) |
7(2) |
|
C(6) |
18(2) |
24(2) |
24(2) |
-8(1) |
9(1) |
-3(1) |
|
C(7) |
20(2) |
23(2) |
16(1) |
-3(1) |
6(1) |
1(1) |
|
C(8) |
15(2) |
15(1) |
13(1) |
-4(1) |
4(1) |
-4(1) |
|
C(9) |
16(2) |
19(2) |
18(1) |
-3(1) |
5(1) |
-1(1) |
|
C(10) |
19(2) |
28(2) |
31(2) |
-3(1) |
-1(1) |
2(2) |
|
C(11) |
20(2) |
27(2) |
25(2) |
1(1) |
5(1) |
2(1) |
|
C(12) |
23(2) |
11(1) |
16(1) |
2(1) |
3(1) |
-2(1) |
|
C(13) |
20(2) |
16(2) |
23(2) |
3(1) |
7(1) |
0(1) |
|
C(14) |
18(2) |
21(2) |
16(1) |
5(1) |
5(1) |
1(1) |
|
C(15) |
18(2) |
28(2) |
21(2) |
8(1) |
5(1) |
-1(1) |
|
C(16) |
20(2) |
28(2) |
19(2) |
8(1) |
10(1) |
11(2) |
|
C(17) |
24(2) |
21(2) |
18(1) |
4(1) |
5(1) |
6(1) |
|
C(18) |
15(2) |
20(2) |
15(1) |
1(1) |
3(1) |
3(1) |
|
C(19) |
14(2) |
20(2) |
11(1) |
6(1) |
4(1) |
4(1) |
|
C(20) |
14(2) |
20(2) |
14(1) |
-3(1) |
2(1) |
-2(1) |
|
C(21) |
16(2) |
29(2) |
16(1) |
-4(1) |
8(1) |
3(1) |
|
C(22) |
16(2) |
13(1) |
13(1) |
1(1) |
5(1) |
4(1) |
|
C(23) |
23(2) |
15(2) |
15(1) |
-1(1) |
11(1) |
-4(1) |
|
C(24) |
24(2) |
20(2) |
13(1) |
-1(1) |
1(1) |
0(1) |
|
C(25) |
23(2) |
23(2) |
19(2) |
0(1) |
6(1) |
2(1) |
|
C(26) |
24(2) |
32(2) |
27(2) |
-2(1) |
5(2) |
9(2) |
|
C(27) |
24(2) |
26(2) |
13(1) |
-2(1) |
8(1) |
8(1) |
|
C(28) |
26(2) |
24(2) |
11(1) |
-1(1) |
6(1) |
2(1) |
|
C(29) |
22(2) |
14(1) |
13(1) |
-4(1) |
8(1) |
-2(1) |
|
C(30) |
22(2) |
21(2) |
16(1) |
-1(1) |
6(1) |
2(1) |
|
C(31) |
26(2) |
33(2) |
25(2) |
-3(1) |
0(1) |
4(2) |
|
C(32) |
23(2) |
20(2) |
31(2) |
1(1) |
4(1) |
4(1) |
|
C(33) |
19(2) |
15(2) |
14(1) |
-6(1) |
5(1) |
-2(1) |
|
C(34) |
20(2) |
12(2) |
23(2) |
-1(1) |
6(1) |
-6(1) |
|
C(35) |
18(2) |
14(2) |
13(1) |
1(1) |
5(1) |
-3(1) |
|
C(36) |
17(2) |
16(2) |
17(1) |
1(1) |
4(1) |
-3(1) |
|
C(37) |
16(2) |
21(2) |
16(1) |
0(1) |
6(1) |
3(1) |
|
C(38) |
21(2) |
17(2) |
14(1) |
-4(1) |
5(1) |
2(1) |
|
C(39) |
19(2) |
15(2) |
14(1) |
1(1) |
2(1) |
-3(1) |
|
C(40) |
14(2) |
17(2) |
11(1) |
6(1) |
2(1) |
4(1) |
|
C(41) |
19(2) |
17(2) |
11(1) |
-3(1) |
3(1) |
-4(1) |
|
C(42) |
20(2) |
25(2) |
13(1) |
-6(1) |
8(1) |
-6(1) |
|
N(1) |
17(1) |
17(1) |
14(1) |
-1(1) |
5(1) |
-1(1) |
|
N(2) |
24(2) |
52(2) |
20(1) |
-4(1) |
4(1) |
9(2) |
|
N(3) |
13(1) |
17(1) |
10(1) |
-2(1) |
2(1) |
-1(1) |
|
N(4) |
20(2) |
45(2) |
18(1) |
3(1) |
3(1) |
3(1) |
|
O(1) |
19(1) |
19(1) |
16(1) |
-5(1) |
8(1) |
-6(1) |
|
O(2) |
19(1) |
21(1) |
19(1) |
-4(1) |
8(1) |
-6(1) |
|
O(3) |
23(1) |
19(1) |
11(1) |
-3(1) |
7(1) |
-4(1) |
|
O(4) |
20(1) |
22(1) |
22(1) |
-7(1) |
9(1) |
-7(1) |
Table 5. Hydrogen coordinates (x104) and isotropic displacement parameters (A2x103) for 136a
|
x |
y |
z |
U(eq) |
|
|
H(2) |
-2960(40) |
246(16) |
1770(30) |
29(9) |
|
H(3A) |
-5805 |
-192 |
222 |
24 |
|
H(3B) |
-5128 |
568 |
289 |
24 |
|
H(4) |
-5390(40) |
670(16) |
2250(30) |
24(9) |
|
H(5A) |
-7741 |
918 |
769 |
40 |
|
H(5B) |
-8196 |
705 |
2011 |
40 |
|
H(5C) |
-8401 |
173 |
931 |
40 |
|
H(6A) |
-6657 |
-681 |
2134 |
26 |
|
H(6B) |
-6460 |
-203 |
3289 |
26 |
|
H(7A) |
-4305 |
-989 |
3529 |
23 |
|
H(7B) |
-3629 |
-232 |
3543 |
23 |
|
H(8) |
-4128 |
-1104 |
1482 |
26(9) |
|
H(9) |
-1267 |
-1093 |
1675 |
10(7) |
|
H(10A) |
-568 |
-158 |
2979 |
32 |
|
H(10B) |
482 |
-813 |
3459 |
32 |
|
H(10C) |
-992 |
-593 |
4056 |
32 |
|
H(11A) |
-2280 |
-1751 |
3625 |
29 |
|
H(11B) |
-764 |
-1972 |
3077 |
29 |
|
H(11C) |
-2557 |
-2048 |
2291 |
29 |
|
H(12) |
-782 |
319 |
-821 |
20 |
|
H(13) |
1118 |
246 |
-1938 |
23 |
|
H(15) |
2689 |
-522 |
-3070 |
26 |
|
H(16) |
2799 |
-1491 |
-4202 |
26 |
|
H(17) |
683 |
-2269 |
-4493 |
25 |
|
H(18) |
-1590 |
-2063 |
-3678 |
20 |
|
H(20) |
-2761 |
-1439 |
-2203 |
12(8) |
|
H(23) |
-4360 |
-2679 |
-5161 |
7(7) |
|
H(24A) |
-3661 |
-4074 |
-4585 |
23 |
|
H(24B) |
-2635 |
-3448 |
-3935 |
23 |
|
H(25) |
-1851 |
-3151 |
-5740 |
26 |
|
H(26A) |
-166 |
-3942 |
-4483 |
33 |
|
H(26B) |
-100 |
-4057 |
-5861 |
33 |
|
H(26C) |
-1153 |
-4552 |
-5218 |
33 |
|
H(27A) |
-2646 |
-3823 |
-7470 |
24 |
|
H(27B) |
-3636 |
-4318 |
-6775 |
24 |
|
H(28A) |
-5449 |
-3580 |
-7970 |
24 |
|
H(28B) |
-4443 |
-2936 |
-7373 |
24 |
|
H(29) |
-6198 |
-3843 |
-6143 |
8(7) |
|
H(30) |
-7906 |
-2936 |
-5929 |
10(7) |
|
H(31A) |
-8059 |
-3161 |
-8418 |
35 |
|
H(31B) |
-9546 |
-2976 |
-7810 |
35 |
|
H(31C) |
-8685 |
-3698 |
-7568 |
35 |
|
H(32A) |
-6271 |
-1997 |
-6100 |
30 |
|
H(32B) |
-7977 |
-1924 |
-7013 |
30 |
|
H(32C) |
-6411 |
-2149 |
-7497 |
30 |
|
H(33) |
-7474 |
-3710 |
-3087 |
19 |
|
H(34) |
-9364 |
-3696 |
-1957 |
22 |
|
H(36) |
-11060 |
-2935 |
-879 |
20 |
|
H(37) |
-11273 |
-1963 |
235 |
21 |
|
H(38) |
-9168 |
-1179 |
603 |
20 |
|
H(39) |
-6850 |
-1364 |
-158 |
19 |
|
H(41) |
-5615 |
-1951 |
-1633 |
21(9) |
Table 6. Torsion angles [deg] for 136a
|
O(1)-C(2)-C(3)-C(4) |
-171.3(2) |
C(28)-C(29)-C(30)-C(31) |
64.8(3) |
|
|
C(8)-C(2)-C(3)-C(4) |
58.9(3) |
C(23)-C(29)-C(30)-C(32) |
61.7(3) |
|
|
C(2)-C(3)-C(4)-C(5) |
-178.4(3) |
C(28)-C(29)-C(30)-C(32) |
-61.3(3) |
|
|
C(2)-C(3)-C(4)-C(6) |
-54.6(3) |
N(3)-C(33)-C(34)-C(35) |
5.2(5) |
|
|
C(5)-C(4)-C(6)-C(7) |
178.5(2) |
C(33)-C(34)-C(35)-C(36) |
163.9(3) |
|
|
C(3)-C(4)-C(6)-C(7) |
54.6(3) |
C(33)-C(34)-C(35)-C(40) |
-12.3(4) |
|
|
C(4)-C(6)-C(7)-C(8) |
-57.7(3) |
C(40)-C(35)-C(36)-C(37) |
-0.7(4) |
|
|
O(1)-C(2)-C(8)-C(9) |
46.7(3) |
C(34)-C(35)-C(36)-C(37) |
-176.9(3) |
|
|
C(3)-C(2)-C(8)-C(9) |
175.8(2) |
C(35)-C(36)-C(37)-C(38) |
0.4(4) |
|
|
O(1)-C(2)-C(8)-C(7) |
172.1(2) |
C(36)-C(37)-C(38)-C(39) |
0.2(4) |
|
|
C(3)-C(2)-C(8)-C(7) |
-58.8(3) |
C(37)-C(38)-C(39)-C(40) |
-0.6(4) |
|
|
C(6)-C(7)-C(8)-C(2) |
57.4(3) |
C(38)-C(39)-C(40)-C(35) |
0.4(4) |
|
|
C(6)-C(7)-C(8)-C(9) |
-177.3(3) |
C(38)-C(39)-C(40)-C(41) |
-178.1(2) |
|
|
C(2)-C(8)-C(9)-C(10) |
67.2(3) |
C(36)-C(35)-C(40)-C(39) |
0.3(4) |
|
|
C(7)-C(8)-C(9)-C(10) |
-54.4(3) |
C(34)-C(35)-C(40)-C(39) |
176.6(3) |
|
|
C(2)-C(8)-C(9)-C(11) |
-167.3(2) |
C(36)-C(35)-C(40)-C(41) |
178.7(2) |
|
|
C(7)-C(8)-C(9)-C(11) |
71.1(3) |
C(34)-C(35)-C(40)-C(41) |
-4.9(4) |
|
|
N(1)-C(12)-C(13)-C(14) |
-3.3(5) |
C(39)-C(40)-C(41)-N(3) |
-155.0(2) |
|
|
C(12)-C(13)-C(14)-C(15) |
-166.7(3) |
C(35)-C(40)-C(41)-N(3) |
26.5(3) |
|
|
C(12)-C(13)-C(14)-C(19) |
11.1(4) |
C(39)-C(40)-C(41)-C(42) |
83.3(3) |
|
|
C(19)-C(14)-C(15)-C(16) |
-0.2(4) |
C(35)-C(40)-C(41)-C(42) |
-95.2(3) |
|
|
C(13)-C(14)-C(15)-C(16) |
177.6(3) |
N(3)-C(41)-C(42)-N(4) |
36(13) |
|
|
C(14)-C(15)-C(16)-C(17) |
-1.1(5) |
C(40)-C(41)-C(42)-N(4) |
160(13) |
|
|
C(15)-C(16)-C(17)-C(18) |
0.8(5) |
O(2)-C(1)-N(1)-C(12) |
173.6(3) |
|
|
C(16)-C(17)-C(18)-C(19) |
0.7(4) |
O(1)-C(1)-N(1)-C(12) |
-7.0(4) |
|
|
C(17)-C(18)-C(19)-C(14) |
-1.9(4) |
O(2)-C(1)-N(1)-C(20) |
0.9(4) |
|
|
C(17)-C(18)-C(19)-C(20) |
177.1(3) |
O(1)-C(1)-N(1)-C(20) |
-179.7(2) |
|
|
C(15)-C(14)-C(19)-C(18) |
1.6(4) |
C(13)-C(12)-N(1)-C(1) |
166.9(3) |
|
|
C(13)-C(14)-C(19)-C(18) |
-176.2(3) |
C(13)-C(12)-N(1)-C(20) |
-20.5(4) |
|
|
C(15)-C(14)-C(19)-C(20) |
-177.3(3) |
C(21)-C(20)-N(1)-C(1) |
84.2(3) |
|
|
C(13)-C(14)-C(19)-C(20) |
4.8(4) |
C(19)-C(20)-N(1)-C(1) |
-153.2(3) |
|
|
C(18)-C(19)-C(20)-N(1) |
155.1(3) |
C(21)-C(20)-N(1)-C(12) |
-88.9(3) |
|
|
C(14)-C(19)-C(20)-N(1) |
-26.0(4) |
C(19)-C(20)-N(1)-C(12) |
33.7(3) |
|
|
C(18)-C(19)-C(20)-C(21) |
-83.5(3) |
O(4)-C(22)-N(3)-C(33) |
-173.7(3) |
|
|
C(14)-C(19)-C(20)-C(21) |
95.5(3) |
O(3)-C(22)-N(3)-C(33) |
6.6(4) |
|
|
N(1)-C(20)-C(21)-N(2) |
-15(17) |
O(4)-C(22)-N(3)-C(41) |
0.1(4) |
|
|
C(19)-C(20)-C(21)-N(2) |
-139(16) |
O(3)-C(22)-N(3)-C(41) |
-179.7(2) |
|
|
O(3)-C(23)-C(24)-C(25) |
177.9(2) |
C(34)-C(33)-N(3)-C(22) |
-166.9(3) |
|
|
C(29)-C(23)-C(24)-C(25) |
60.0(3) |
C(34)-C(33)-N(3)-C(41) |
19.5(4) |
|
|
C(23)-C(24)-C(25)-C(27) |
-56.7(3) |
C(42)-C(41)-N(3)-C(22) |
-84.8(3) |
|
|
C(23)-C(24)-C(25)-C(26) |
-179.8(3) |
C(40)-C(41)-N(3)-C(22) |
151.9(2) |
|
|
C(24)-C(25)-C(27)-C(28) |
55.2(3) |
C(42)-C(41)-N(3)-C(33) |
89.3(3) |
|
|
C(26)-C(25)-C(27)-C(28) |
178.2(3) |
C(40)-C(41)-N(3)-C(33) |
-34.0(3) |
|
|
C(25)-C(27)-C(28)-C(29) |
-55.9(3) |
O(2)-C(1)-O(1)-C(2) |
-2.5(4) |
|
|
O(3)-C(23)-C(29)-C(30) |
57.9(3) |
N(1)-C(1)-O(1)-C(2) |
178.1(2) |
|
|
C(24)-C(23)-C(29)-C(30) |
177.5(2) |
C(3)-C(2)-O(1)-C(1) |
-65.0(3) |
|
|
O(3)-C(23)-C(29)-C(28) |
-175.9(2) |
C(8)-C(2)-O(1)-C(1) |
64.6(3) |
|
|
C(24)-C(23)-C(29)-C(28) |
-56.3(3) |
O(4)-C(22)-O(3)-C(23) |
0.7(4) |
|
|
C(27)-C(28)-C(29)-C(23) |
54.0(3) |
N(3)-C(22)-O(3)-C(23) |
-179.5(2) |
|
|
C(27)-C(28)-C(29)-C(30) |
179.8(3) |
C(24)-C(23)-O(3)-C(22) |
86.3(3) |
|
|
C(23)-C(29)-C(30)-C(31) |
-172.3(2) |
C(29)-C(23)-O(3)-C(22) |
-151.6(2) |
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