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)