phw 1301
Table
1 Crystal data and structure refinement for |
|
Identification
code |
|
Empirical
formula |
C35H48N6O
|
Formula
weight |
568.79
|
Temperature/K
|
110.00(10)
|
Crystal
system |
monoclinic
|
Space
group |
P21/n
|
a/Å
|
11.6014(5)
|
b/Å
|
9.7929(4)
|
c/Å
|
29.2781(12)
|
α/°
|
90.00
|
β/°
|
90.850(4)
|
γ/°
|
90.00
|
Volume/Å3
|
3326.0(2)
|
Z |
4 |
ρcalcmg/mm3 |
1.136
|
m/mm‑1
|
0.070
|
F(000)
|
1232.0
|
Crystal
size/mm3 |
0.2369
× 0.1651 × 0.0437 |
2Θ
range for data collection |
5.6
to 56° |
Index
ranges |
-15
≤ h ≤ 15, -10 ≤ k ≤ 12, -38 ≤ l ≤ 23 |
Reflections
collected |
12634
|
Independent
reflections |
6771[R(int) = 0.0346] |
Data/restraints/parameters
|
6771/4/410
|
Goodness-of-fit
on F2 |
1.049
|
Final
R indexes [I>=2σ (I)] |
R1
= 0.0598, wR2 = 0.1260 |
Final
R indexes [all data] |
R1
= 0.0888, wR2 = 0.1413 |
Largest
diff. peak/hole / e Å-3 |
0.21/-0.24
|
Table
2 Fractional Atomic Coordinates (×104) and Equivalent
Isotropic Displacement Parameters (Å2×103) for . Ueq is defined
as 1/3 of of the trace of the orthogonalised
UIJ tensor. |
||||
Atom |
x |
y |
z |
U(eq) |
C1 |
1375.5(16) |
7091.2(19) |
3052.1(6) |
17.3(4) |
C2 |
2242.4(16) |
7853.7(19) |
2760.5(6) |
19.1(4) |
C3 |
3228.7(16) |
6933.9(19) |
2615.3(6) |
17.9(4) |
C4 |
3821.3(17) |
6303(2) |
3033.0(6) |
20.4(4) |
C5 |
2959.4(16) |
5544.7(19) |
3328.5(6) |
18.2(4) |
C6 |
1979.0(16) |
6486.0(19) |
3471.5(6) |
18.6(4) |
C7 |
-529.6(17) |
7849.8(19) |
2994.0(6) |
19.8(4) |
C8 |
-1519.3(17) |
8743.5(19) |
3058.3(6) |
18.6(4) |
C9 |
-1387.8(18) |
10053(2) |
3240.0(7) |
23.2(5) |
C10 |
-2313.9(17) |
10918(2) |
3280.6(7) |
24.5(5) |
C11 |
-3430.0(17) |
10505(2) |
3147.5(7) |
22.2(5) |
C12 |
-3567.4(17) |
9174(2) |
2979.8(7) |
23.2(5) |
C13 |
-2620.3(17) |
8340(2) |
2928.6(7) |
23.5(5) |
C14 |
-4164(2) |
12759(2) |
3342.4(9) |
39.2(6) |
C15 |
-5521.8(18) |
10902(2) |
3140.7(8) |
33.1(5) |
C16 |
4163.7(16) |
7456.9(19) |
1938.0(6) |
19.2(4) |
C17 |
4930.0(17) |
8188.9(19) |
1629.4(6) |
20.2(4) |
C18 |
4946.8(18) |
7871(2) |
1168.2(7) |
25.4(5) |
C19 |
5656.2(19) |
8543(2) |
869.4(7) |
30.6(5) |
C20 |
6402.3(19) |
9578(2) |
1023.5(7) |
30.0(5) |
C21 |
6392.9(19) |
9886(2) |
1491.2(7) |
27.3(5) |
C22 |
5668.6(18) |
9211.7(19) |
1782.7(7) |
23.7(5) |
C23 |
7081(2) |
9977(3) |
250.2(8) |
53.2(8) |
C24 |
7908(2) |
11279(3) |
913.2(9) |
55.1(8) |
C25 |
3193.9(17) |
3853(2) |
3872.5(6) |
21.6(5) |
C26 |
3646.7(17) |
3156.4(19) |
4280.0(6) |
20.8(4) |
C27 |
3101.8(18) |
1980(2) |
4436.4(7) |
26.0(5) |
C28 |
3460.3(19) |
1338(2) |
4831.9(7) |
26.5(5) |
C29 |
4411.8(18) |
1823(2) |
5086.5(6) |
23.2(5) |
C30 |
4973.2(19) |
3002(2) |
4920.0(7) |
24.2(5) |
C31 |
4591.4(18) |
3640(2) |
4530.1(7) |
23.3(5) |
C32 |
4091(2) |
139(2) |
5684.0(8) |
38.1(6) |
C33 |
5764(2) |
1726(2) |
5733.0(8) |
42.4(7) |
N1 |
458.0(14) |
8031.7(16) |
3181.6(5) |
18.9(4) |
N2 |
4055.0(14) |
7745.0(16) |
2356.4(5) |
19.6(4) |
N3 |
3549.2(14) |
4998.4(16) |
3734.4(5) |
19.9(4) |
N4 |
-4348.1(15) |
11390.6(18) |
3171.7(6) |
31.1(4) |
N5 |
7121.8(19) |
10259(2) |
734.8(7) |
43.7(6) |
N6 |
4788.1(17) |
1191.6(17) |
5477.1(6) |
30.9(4) |
C34A |
872(14) |
8885(12) |
4386(2) |
48(4) |
C34B |
267(4) |
9390(6) |
4314.9(14) |
54.2(15) |
C35A |
-514(9) |
8850(20) |
4399(4) |
88(7) |
C35B |
228(7) |
8014(5) |
4488.4(17) |
87(3) |
O1 |
1122.0(15) |
9597.4(16) |
3975.0(6) |
38.9(4) |
Table
3 Anisotropic Displacement Parameters (Å2×103)
for . The Anisotropic displacement factor exponent
takes the form: -2π2[h2a*2U11+...+2hka×b×U12] |
||||||
Atom |
U11 |
U22 |
U33 |
U23 |
U13 |
U12 |
C1 |
15.8(10) |
16.6(9) |
19.4(10) |
-1.9(8) |
1.4(8) |
-0.2(8) |
C2 |
19.2(11) |
18.1(10) |
20(1) |
1.9(8) |
0.4(8) |
0.9(8) |
C3 |
16.1(10) |
18(1) |
19.6(10) |
1.1(8) |
2.2(8) |
-1.0(8) |
C4 |
18.9(11) |
22(1) |
20.4(10) |
1.7(8) |
0.3(8) |
3.6(9) |
C5 |
19.9(11) |
17.2(10) |
17.4(10) |
-0.2(8) |
0.2(8) |
1.8(8) |
C6 |
17.8(10) |
19.2(10) |
18.9(10) |
-0.9(8) |
1.5(8) |
-0.4(8) |
C7 |
23.2(12) |
15.4(10) |
20.8(10) |
-0.8(8) |
1.3(8) |
-1.2(9) |
C8 |
17.0(11) |
19.7(10) |
19.2(10) |
2.7(8) |
0.1(8) |
-0.2(8) |
C9 |
14.1(11) |
22.5(10) |
33.0(12) |
0.0(9) |
-1.3(8) |
-1.9(9) |
C10 |
20.3(11) |
19.1(10) |
34.1(12) |
0.2(9) |
1.2(9) |
1.0(9) |
C11 |
18.1(11) |
25.6(11) |
23(1) |
6.6(9) |
1.7(8) |
1.9(9) |
C12 |
15.6(11) |
29.2(11) |
24.6(11) |
3.9(9) |
-3.5(8) |
-5.1(9) |
C13 |
23.0(12) |
22(1) |
25.4(11) |
1.1(9) |
-3.0(8) |
-1.5(9) |
C14 |
26.6(14) |
30.6(13) |
60.7(16) |
4.5(12) |
8.3(11) |
12.8(11) |
C15 |
18.8(12) |
49.2(14) |
31.3(12) |
9.9(11) |
0.5(9) |
9.3(11) |
C16 |
15(1) |
19(1) |
23.7(11) |
1.0(9) |
-0.3(8) |
1.7(8) |
C17 |
18.0(11) |
20.5(10) |
22.3(10) |
2.8(9) |
3.0(8) |
4.8(9) |
C18 |
23.1(12) |
27.0(11) |
26.0(11) |
0.2(9) |
1.6(9) |
-1.8(9) |
C19 |
33.3(13) |
37.0(13) |
21.8(11) |
2.6(10) |
6.7(9) |
0.9(11) |
C20 |
31.6(13) |
24.4(11) |
34.2(12) |
5.6(10) |
12.7(10) |
0.3(10) |
C21 |
26.6(12) |
22.1(11) |
33.4(12) |
-0.6(10) |
7.4(9) |
-2.6(9) |
C22 |
26.1(12) |
19.7(10) |
25.5(11) |
-0.1(9) |
5.3(9) |
2.4(9) |
C23 |
63(2) |
58.7(17) |
38.8(15) |
10.1(14) |
24.6(14) |
-9.0(15) |
C24 |
67(2) |
43.4(15) |
56.0(18) |
-0.2(14) |
31.1(15) |
-23.7(15) |
C25 |
21.0(11) |
23.8(11) |
20.1(10) |
-2.6(9) |
1.0(8) |
2.5(9) |
C26 |
24.0(12) |
18.8(10) |
19.6(10) |
-0.8(8) |
2.3(8) |
3.8(9) |
C27 |
25.7(12) |
23.6(11) |
28.6(11) |
1.8(9) |
-3.4(9) |
0.0(9) |
C28 |
31.8(13) |
21.3(11) |
26.4(11) |
3.9(9) |
0.8(9) |
-1.6(10) |
C29 |
30.0(12) |
20.8(10) |
18.8(10) |
-2.0(9) |
-0.7(9) |
7.7(9) |
C30 |
27.4(12) |
20.7(10) |
24.2(11) |
-4.0(9) |
-3.1(9) |
1.9(9) |
C31 |
28.4(12) |
17.8(10) |
23.6(11) |
-1.2(9) |
3.5(9) |
0.2(9) |
C32 |
55.2(17) |
33.9(13) |
25.3(12) |
8.7(10) |
1.8(11) |
7.3(12) |
C33 |
64.4(18) |
31.1(13) |
31.1(13) |
2.1(11) |
-23.3(12) |
4.1(12) |
N1 |
15.9(9) |
18.9(8) |
21.8(9) |
2.4(7) |
1.4(7) |
1.7(7) |
N2 |
17.5(9) |
20.4(8) |
20.9(9) |
2.3(7) |
2.2(7) |
-0.4(7) |
N3 |
21.8(10) |
17.9(8) |
20.0(9) |
1.3(7) |
1.2(7) |
3.8(7) |
N4 |
17.4(10) |
28.1(10) |
47.9(12) |
3.1(9) |
1.7(8) |
6.0(8) |
N5 |
55.3(15) |
42.7(12) |
33.5(11) |
2.4(10) |
20.7(10) |
-15.7(11) |
N6 |
42.0(12) |
24.8(10) |
25.9(10) |
4.9(8) |
-6.6(8) |
1.0(9) |
C34A |
54(9) |
44(8) |
47(7) |
10(6) |
1(5) |
-1(6) |
C34B |
86(4) |
50(3) |
28(2) |
-2.1(19) |
4(2) |
7(3) |
C35A |
35(8) |
170(20) |
60(8) |
27(10) |
-1(6) |
-25(10) |
C35B |
126(7) |
63(3) |
74(4) |
5(3) |
41(4) |
-6(4) |
O1 |
46.8(11) |
34.0(9) |
35.7(10) |
-8.4(8) |
-5.8(8) |
-0.3(8) |
Table
4 Bond Lengths for . |
||||||
Atom |
Atom |
Length/Å |
|
Atom |
Atom |
Length/Å |
C1 |
C2 |
1.524(2) |
|
C17 |
C22 |
1.388(3) |
C1 |
C6 |
1.525(3) |
|
C18 |
C19 |
1.378(3) |
C1 |
N1 |
1.462(2) |
|
C19 |
C20 |
1.403(3) |
C2 |
C3 |
1.522(3) |
|
C20 |
C21 |
1.402(3) |
C3 |
C4 |
1.525(3) |
|
C20 |
N5 |
1.370(3) |
C3 |
N2 |
1.465(2) |
|
C21 |
C22 |
1.375(3) |
C4 |
C5 |
1.525(3) |
|
C23 |
N5 |
1.446(3) |
C5 |
C6 |
1.527(3) |
|
C24 |
N5 |
1.445(3) |
C5 |
N3 |
1.464(2) |
|
C25 |
C26 |
1.465(3) |
C7 |
C8 |
1.458(3) |
|
C25 |
N3 |
1.264(2) |
C7 |
N1 |
1.276(2) |
|
C26 |
C27 |
1.395(3) |
C8 |
C9 |
1.395(3) |
|
C26 |
C31 |
1.392(3) |
C8 |
C13 |
1.385(3) |
|
C27 |
C28 |
1.376(3) |
C9 |
C10 |
1.375(3) |
|
C28 |
C29 |
1.406(3) |
C10 |
C11 |
1.406(3) |
|
C29 |
C30 |
1.415(3) |
C11 |
C12 |
1.401(3) |
|
C29 |
N6 |
1.366(2) |
C11 |
N4 |
1.376(3) |
|
C30 |
C31 |
1.369(3) |
C12 |
C13 |
1.379(3) |
|
C32 |
N6 |
1.449(3) |
C14 |
N4 |
1.445(3) |
|
C33 |
N6 |
1.446(3) |
C15 |
N4 |
1.445(3) |
|
C34A |
C35A |
1.61(2) |
C16 |
C17 |
1.464(3) |
|
C34A |
O1 |
1.425(2) |
C16 |
N2 |
1.265(2) |
|
C34B |
C35B |
1.441(8) |
C17 |
C18 |
1.386(3) |
|
C34B |
O1 |
1.4304(19) |
Table
5 Bond Angles for . |
||||||||
Atom |
Atom |
Atom |
Angle/˚ |
|
Atom |
Atom |
Atom |
Angle/˚ |
C2 |
C1 |
C6 |
110.04(16) |
|
N5 |
C20 |
C19 |
122.1(2) |
N1 |
C1 |
C2 |
109.01(15) |
|
N5 |
C20 |
C21 |
120.8(2) |
N1 |
C1 |
C6 |
111.31(15) |
|
C22 |
C21 |
C20 |
121.1(2) |
C3 |
C2 |
C1 |
111.82(15) |
|
C21 |
C22 |
C17 |
121.72(19) |
C2 |
C3 |
C4 |
110.35(15) |
|
N3 |
C25 |
C26 |
124.0(2) |
N2 |
C3 |
C2 |
108.91(15) |
|
C27 |
C26 |
C25 |
119.55(19) |
N2 |
C3 |
C4 |
110.12(16) |
|
C31 |
C26 |
C25 |
122.67(18) |
C3 |
C4 |
C5 |
111.14(16) |
|
C31 |
C26 |
C27 |
117.75(18) |
C4 |
C5 |
C6 |
111.03(15) |
|
C28 |
C27 |
C26 |
121.4(2) |
N3 |
C5 |
C4 |
109.63(15) |
|
C27 |
C28 |
C29 |
121.12(19) |
N3 |
C5 |
C6 |
109.81(15) |
|
C28 |
C29 |
C30 |
117.06(18) |
C1 |
C6 |
C5 |
110.41(15) |
|
N6 |
C29 |
C28 |
121.97(19) |
N1 |
C7 |
C8 |
124.37(18) |
|
N6 |
C29 |
C30 |
120.97(19) |
C9 |
C8 |
C7 |
121.25(18) |
|
C31 |
C30 |
C29 |
121.0(2) |
C13 |
C8 |
C7 |
121.21(18) |
|
C30 |
C31 |
C26 |
121.70(19) |
C13 |
C8 |
C9 |
117.52(18) |
|
C7 |
N1 |
C1 |
116.94(16) |
C10 |
C9 |
C8 |
121.21(19) |
|
C16 |
N2 |
C3 |
117.10(17) |
C9 |
C10 |
C11 |
121.06(19) |
|
C25 |
N3 |
C5 |
115.68(17) |
C12 |
C11 |
C10 |
117.67(18) |
|
C11 |
N4 |
C14 |
119.46(18) |
N4 |
C11 |
C10 |
120.98(19) |
|
C11 |
N4 |
C15 |
121.18(18) |
N4 |
C11 |
C12 |
121.34(19) |
|
C15 |
N4 |
C14 |
117.57(18) |
C13 |
C12 |
C11 |
120.18(19) |
|
C20 |
N5 |
C23 |
120.1(2) |
C12 |
C13 |
C8 |
122.27(19) |
|
C20 |
N5 |
C24 |
120.0(2) |
N2 |
C16 |
C17 |
123.95(18) |
|
C24 |
N5 |
C23 |
119.9(2) |
C18 |
C17 |
C16 |
120.57(18) |
|
C29 |
N6 |
C32 |
119.93(19) |
C18 |
C17 |
C22 |
117.34(18) |
|
C29 |
N6 |
C33 |
120.53(18) |
C22 |
C17 |
C16 |
122.09(18) |
|
C33 |
N6 |
C32 |
118.57(18) |
C19 |
C18 |
C17 |
121.9(2) |
|
O1 |
C34A |
C35A |
104.3(11) |
C18 |
C19 |
C20 |
120.8(2) |
|
O1 |
C34B |
C35B |
113.8(5) |
C21 |
C20 |
C19 |
117.10(19) |
|
|
|
|
|
Table
6 Hydrogen Bonds for . |
||||||
D |
H |
A |
d(D-H)/Å |
d(H-A)/Å |
d(D-A)/Å |
D-H-A/° |
O1 |
H1A |
N1 |
0.87(3) |
2.01(3) |
2.879(2) |
175(3) |
Table
7 Torsion Angles for . |
||||||||||
A |
B |
C |
D |
Angle/˚ |
|
A |
B |
C |
D |
Angle/˚ |
C1 |
C2 |
C3 |
C4 |
-56.3(2) |
|
C19 |
C20 |
N5 |
C23 |
3.7(4) |
C1 |
C2 |
C3 |
N2 |
-177.24(16) |
|
C19 |
C20 |
N5 |
C24 |
-177.5(2) |
C2 |
C1 |
C6 |
C5 |
-57.1(2) |
|
C20 |
C21 |
C22 |
C17 |
0.9(3) |
C2 |
C1 |
N1 |
C7 |
109.07(19) |
|
C21 |
C20 |
N5 |
C23 |
-177.0(2) |
C2 |
C3 |
C4 |
C5 |
55.3(2) |
|
C21 |
C20 |
N5 |
C24 |
1.9(3) |
C2 |
C3 |
N2 |
C16 |
-113.88(19) |
|
C22 |
C17 |
C18 |
C19 |
-0.6(3) |
C3 |
C4 |
C5 |
C6 |
-56.3(2) |
|
C25 |
C26 |
C27 |
C28 |
-176.34(18) |
C3 |
C4 |
C5 |
N3 |
-177.84(15) |
|
C25 |
C26 |
C31 |
C30 |
177.46(18) |
C4 |
C3 |
N2 |
C16 |
124.99(19) |
|
C26 |
C25 |
N3 |
C5 |
-178.04(17) |
C4 |
C5 |
C6 |
C1 |
57.2(2) |
|
C26 |
C27 |
C28 |
C29 |
-1.8(3) |
C4 |
C5 |
N3 |
C25 |
-144.15(17) |
|
C27 |
C26 |
C31 |
C30 |
-0.8(3) |
C6 |
C1 |
C2 |
C3 |
57.3(2) |
|
C27 |
C28 |
C29 |
C30 |
0.5(3) |
C6 |
C1 |
N1 |
C7 |
-129.37(18) |
|
C27 |
C28 |
C29 |
N6 |
-179.28(19) |
C6 |
C5 |
N3 |
C25 |
93.61(19) |
|
C28 |
C29 |
C30 |
C31 |
0.6(3) |
C7 |
C8 |
C9 |
C10 |
176.92(18) |
|
C28 |
C29 |
N6 |
C32 |
-10.9(3) |
C7 |
C8 |
C13 |
C12 |
-179.04(18) |
|
C28 |
C29 |
N6 |
C33 |
-179.4(2) |
C8 |
C7 |
N1 |
C1 |
-175.56(17) |
|
C29 |
C30 |
C31 |
C26 |
-0.5(3) |
C8 |
C9 |
C10 |
C11 |
1.1(3) |
|
C30 |
C29 |
N6 |
C32 |
169.32(18) |
C9 |
C8 |
C13 |
C12 |
-0.9(3) |
|
C30 |
C29 |
N6 |
C33 |
0.7(3) |
C9 |
C10 |
C11 |
C12 |
1.1(3) |
|
C31 |
C26 |
C27 |
C28 |
1.9(3) |
C9 |
C10 |
C11 |
N4 |
-177.44(19) |
|
N1 |
C1 |
C2 |
C3 |
179.66(15) |
C10 |
C11 |
C12 |
C13 |
-3.2(3) |
|
N1 |
C1 |
C6 |
C5 |
-178.11(15) |
C10 |
C11 |
N4 |
C14 |
-0.9(3) |
|
N1 |
C7 |
C8 |
C9 |
16.2(3) |
C10 |
C11 |
N4 |
C15 |
-165.24(19) |
|
N1 |
C7 |
C8 |
C13 |
-165.75(19) |
C11 |
C12 |
C13 |
C8 |
3.1(3) |
|
N2 |
C3 |
C4 |
C5 |
175.58(15) |
C12 |
C11 |
N4 |
C14 |
-179.34(19) |
|
N2 |
C16 |
C17 |
C18 |
-175.77(19) |
C12 |
C11 |
N4 |
C15 |
16.3(3) |
|
N2 |
C16 |
C17 |
C22 |
4.7(3) |
C13 |
C8 |
C9 |
C10 |
-1.2(3) |
|
N3 |
C5 |
C6 |
C1 |
178.58(15) |
C16 |
C17 |
C18 |
C19 |
179.86(19) |
|
N3 |
C25 |
C26 |
C27 |
172.01(18) |
C16 |
C17 |
C22 |
C21 |
179.41(19) |
|
N3 |
C25 |
C26 |
C31 |
-6.2(3) |
C17 |
C16 |
N2 |
C3 |
178.49(17) |
|
N4 |
C11 |
C12 |
C13 |
175.37(18) |
C17 |
C18 |
C19 |
C20 |
0.5(3) |
|
N5 |
C20 |
C21 |
C22 |
179.6(2) |
C18 |
C17 |
C22 |
C21 |
-0.2(3) |
|
N6 |
C29 |
C30 |
C31 |
-179.56(19) |
C18 |
C19 |
C20 |
C21 |
0.2(3) |
|
C35A |
C34A |
O1 |
C34B |
23.1(11) |
C18 |
C19 |
C20 |
N5 |
179.6(2) |
|
C35B |
C34B |
O1 |
C34A |
-35.6(10) |
C19 |
C20 |
C21 |
C22 |
-1.0(3) |
|
|
|
|
|
|
Table
8 Hydrogen Atom Coordinates (Å×104) and Isotropic
Displacement Parameters (Å2×103) for . |
||||
Atom |
x |
y |
z |
U(eq) |
H1 |
1038 |
6347 |
2871 |
21 |
H2A |
1853 |
8212 |
2491 |
23 |
H2B |
2551 |
8620 |
2933 |
23 |
H3 |
2923 |
6203 |
2420 |
21 |
H4A |
4191 |
7017 |
3212 |
25 |
H4B |
4414 |
5674 |
2935 |
25 |
H5 |
2634 |
4783 |
3152 |
22 |
H6A |
1428 |
5975 |
3649 |
22 |
H6B |
2285 |
7216 |
3662 |
22 |
H7 |
-625 |
7097 |
2804 |
24 |
H9 |
-660 |
10345 |
3335 |
28 |
H10 |
-2200 |
11791 |
3398 |
29 |
H12 |
-4299 |
8853 |
2903 |
28 |
H13 |
-2725 |
7476 |
2803 |
28 |
H14A |
-3962 |
12722 |
3661 |
59 |
H14B |
-4858 |
13283 |
3302 |
59 |
H14C |
-3551 |
13183 |
3177 |
59 |
H15A |
-5612 |
10337 |
2875 |
50 |
H15B |
-6039 |
11666 |
3118 |
50 |
H15C |
-5695 |
10379 |
3408 |
50 |
H16 |
3731 |
6737 |
1819 |
23 |
H18 |
4465 |
7184 |
1057 |
30 |
H19 |
5640 |
8308 |
562 |
37 |
H21 |
6885 |
10557 |
1606 |
33 |
H22 |
5674 |
9447 |
2090 |
28 |
H23A |
7257 |
9032 |
199 |
80 |
H23B |
7635 |
10537 |
98 |
80 |
H23C |
6323 |
10174 |
132 |
80 |
H24A |
7477 |
12018 |
1042 |
83 |
H24B |
8376 |
11619 |
671 |
83 |
H24C |
8393 |
10877 |
1145 |
83 |
H25 |
2609 |
3426 |
3705 |
26 |
H27 |
2483 |
1622 |
4270 |
31 |
H28 |
3066 |
570 |
4932 |
32 |
H30 |
5611 |
3348 |
5078 |
29 |
H31 |
4973 |
4417 |
4430 |
28 |
H32A |
3369 |
523 |
5776 |
57 |
H32B |
4490 |
-225 |
5946 |
57 |
H32C |
3952 |
-579 |
5467 |
57 |
H33A |
6412 |
1814 |
5535 |
64 |
H33B |
5957 |
1113 |
5978 |
64 |
H33C |
5572 |
2604 |
5856 |
64 |
H34A |
1186 |
9364 |
4650 |
58 |
H34B |
1188 |
7968 |
4380 |
58 |
H34C |
-483 |
9620 |
4185 |
65 |
H34D |
418 |
10009 |
4567 |
65 |
H35A |
-809 |
8439 |
4123 |
132 |
H35B |
-806 |
9761 |
4425 |
132 |
H35C |
-755 |
8319 |
4657 |
132 |
H35D |
-2 |
7404 |
4247 |
131 |
H35E |
-318 |
7964 |
4731 |
131 |
H35F |
977 |
7759 |
4602 |
131 |
H1A |
880(20) |
9150(30) |
3734(10) |
66(10) |
Experimental
Single
crystals of C35H48N6O [] were []. A
suitable crystal was selected and [oil on loop]
on a Oxford Diffraction Supernova diffractometer.
The crystal was kept at 110.00(10) K during data collection. Using Olex2 [1],
the structure was solved with the Superflip [2]
structure solution program using Charge Flipping and refined with the ShelXL [3] refinement package using Least Squares minimisation.
Crystal
structure determination of []
Crystal
Data for C35H48N6O
(M =568.79): monoclinic, space group P21/n (no. 14), a =
11.6014(5) Å, b = 9.7929(4) Å, c =
29.2781(12) Å, β = 90.850(4)°, V =
3326.0(2) Å3, Z = 4, T =
110.00(10) K, μ(Mo Kα) = 0.070 mm-1, Dcalc = 1.136 g/mm3, 12634
reflections measured (5.6 ≤ 2Θ ≤ 56), 6771 unique (Rint = 0.0346) which were used in
all calculations. The final R1 was 0.0598 (>2sigma(I)) and wR2 was 0.1413 (all data).
This report has been
created with Olex2, compiled on Dec 5 2012 16:17:34. Please let us know if
there are any errors or if you would like to have additional featrues.