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.

  1. O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341.
  2. SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790
  3. SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122

Crystal structure determination of []

Crystal Data for C35H48N6O (=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)°, = 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.