phw1114

Table 1 Crystal data and structure refinement for phw1114

Identification code

phw1114

Empirical formula

C45H63Cl9N12

Formula weight

1091.12

Temperature/K

109.9

Crystal system

triclinic

Space group

P-1

a/Å

14.3898(12)

b/Å

14.5637(14)

c/Å

15.0840(10)

α/°

88.276(7)

β/°

63.722(8)

γ/°

71.729(9)

Volume/Å3

2669.5(4)

Z

2

ρcalcmg/mm3

1.357

m/mm‑1

0.516

F(000)

1140.000

Crystal size/mm3

0.2245 × 0.06 × 0.0362

Theta range for data collection

5.76 to 58.06°

Index ranges

-19 ≤ h ≤ 19, -18 ≤ k ≤ 19, -19 ≤ l ≤ 20

Reflections collected

17691

Independent reflections

11923[R(int) = 0.0254]

Data/restraints/parameters

11923/0/647

Goodness-of-fit on F2

1.019

Final R indexes [I>2σ (I)]

R1 = 0.0565, wR2 = 0.1016

Final R indexes [all data]

R1 = 0.0895, wR2 = 0.1161

Largest diff. peak/hole / e Å-3

0.642/-0.481


Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1114. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.

Atom

x

y

z

U(eq)

C1

8823.3(19)

1590.9(18)

1418.6(17)

12.9(5)

C2

9797.1(19)

1343.3(18)

367.1(17)

13.7(5)

C3

10903.1(19)

1214.4(18)

346.7(17)

14.8(5)

C4

11104.6(19)

537.3(19)

1086.4(17)

16.7(5)

C5

10147.5(19)

867.1(18)

2137.4(17)

14.4(5)

C6

9096(2)

886.5(18)

2111.9(18)

15.8(5)

C7

7434(2)

2164.7(19)

795.9(18)

16.3(5)

C8

6353(2)

2137.7(18)

925.4(18)

16.1(5)

C9

6124(2)

1604.0(19)

363.5(18)

17.8(5)

C10

4964(2)

1821(2)

820.6(19)

20.5(6)

C11

4528(2)

2478.9(19)

1646.0(19)

20.0(6)

C12

12815(2)

992(2)

-927.0(18)

21.4(6)

C13

13597(2)

654.0(19)

-2004.0(18)

18.2(5)

C14

13850(2)

1159(2)

-2814.5(19)

21.9(6)

C15

14587(2)

477(2)

-3674.6(19)

24.2(6)

C16

14772(2)

-430(2)

-3373.2(19)

24.4(6)

C17

9604(2)

456.5(19)

3883.6(18)

18.3(5)

C18

9404(2)

1446(2)

4335.0(17)

19.0(6)

C19

10009(2)

1771(2)

4660.0(18)

21.7(6)

C20

9443(2)

2778(2)

5022.8(19)

27.9(7)

C21

8507(2)

3032(2)

4912(2)

30.2(7)

N1

7786.4(17)

1557.0(17)

1465.4(15)

14.7(4)

N2

5368.6(17)

2664.9(17)

1714.2(16)

17.3(5)

N3

11775.9(17)

813.5(16)

-678.7(15)

16.6(5)

N4

14170.8(19)

-312.0(18)

-2360.5(17)

22.4(5)

N5

10379.1(18)

176.0(16)

2807.0(15)

16.4(5)

N6

8491(2)

2226.4(19)

4489.8(17)

26.6(6)

C22

4641(2)

4037.7(19)

-1068.1(18)

18.4(5)

C23

4324(2)

4957.8(19)

-1522.7(17)

18.0(5)

C24

5175(2)

4861.6(19)

-2605.5(18)

17.4(5)

C25

6312(2)

4661.5(19)

-2668.2(18)

18.5(5)

C26

6645(2)

3740.7(19)

-2215.8(18)

17.6(5)

C27

5781(2)

3828.9(19)

-1138.1(17)

17.9(5)

C28

2788(2)

4083(2)

147(2)

28.8(7)

C29

2171(2)

3895(2)

1189(2)

22.6(6)

C30

1828(2)

3121(2)

1545(2)

25.9(6)

C31

1347(2)

3279(2)

2593(2)

27.6(7)

C32

1420(2)

4131(2)

2842(2)

28.5(7)

C33

3912(2)

5934.8(19)

-3202.7(18)

17.9(5)

C34

3872(2)

6684.8(19)

-3887.1(18)

18.0(5)

C35

4188(2)

6578(2)

-4896.0(19)

23.7(6)

C36

4091(2)

7512(2)

-5212(2)

27.6(7)

C37

3714(2)

8162(2)

-4394.3(19)

23.4(6)

C38

8102(2)

2768(2)

-1793(2)

27.6(7)

C39

9284(2)

2526.5(19)

-2031.5(19)

21.2(6)

C40

9833(2)

3068(2)

-1880(2)

27.7(6)

C41

10942(2)

2464(2)

-2230(2)

26.8(6)

C42

11037(2)

1575(2)

-2591(2)

23.8(6)

N7

3853.7(18)

4125.5(18)

-16.3(16)

20.7(5)

N8

1912.9(19)

4513.4(19)

1986.8(17)

24.5(5)

N9

4902.9(18)

5756.1(16)

-3054.4(16)

17.4(5)

N10

3591.0(18)

7650.8(17)

-3591.8(17)

18.9(5)

N11

7741.2(18)

3598.4(16)

-2281.4(17)

18.9(5)

N12

10023.6(18)

1619.1(17)

-2470.6(16)

20.8(5)

C43

7836(2)

6826(2)

-5456(2)

30.6(7)

Cl1

6556.5(6)

6880.1(8)

-5345.7(6)

47.0(2)

Cl2

7653.5(7)

7556.6(7)

-4446.5(6)

46.0(2)

Cl3

8642.0(9)

5623.8(7)

-5518.2(8)

69.4(3)

C44

6461(2)

10390(2)

-2725.3(19)

25.1(6)

Cl4

7478.0(6)

10802.2(6)

-3651.5(6)

40.7(2)

Cl5

5735.3(7)

11233.8(7)

-1643.1(6)

43.6(2)

Cl6

7081.9(6)

9230.9(6)

-2478.8(6)

34.04(18)

C45

9170(3)

4527(2)

1725(2)

36.3(8)

Cl7

8082.5(8)

5631.5(6)

1980.3(7)

52.3(2)

Cl8

9524.6(8)

3909.2(6)

570.6(6)

48.0(2)

Cl9

8776.9(6)

3810.5(6)

2692.5(6)

34.47(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1114. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]

Atom

U11

U22

U33

U23

U13

U12

C1

13.5(12)

12.1(12)

14.5(12)

2.2(9)

-8.3(10)

-3.3(10)

C2

14.8(12)

15.3(13)

12.2(12)

4.6(10)

-7.8(10)

-4.5(10)

C3

12.5(12)

17.3(13)

11.4(12)

0.9(10)

-3.6(10)

-3.5(10)

C4

10.0(12)

21.5(14)

16.6(13)

1(1)

-6.3(10)

-2.2(11)

C5

14.5(12)

14.7(13)

14.0(12)

3.1(10)

-8.2(10)

-2.3(10)

C6

14.9(12)

17.0(13)

14.8(13)

4.3(10)

-7.5(11)

-3.5(11)

C7

14.0(12)

19.4(14)

15.6(13)

7.9(10)

-7.9(11)

-4.4(11)

C8

15.9(12)

16.1(13)

17.4(13)

6.5(10)

-9.8(11)

-3.6(11)

C9

16.6(13)

19.9(14)

14.3(13)

3.4(10)

-6.7(11)

-3.5(11)

C10

18.7(13)

25.7(15)

23.6(14)

8.2(11)

-13.2(12)

-10.7(12)

C11

14.2(13)

23.8(15)

23.4(14)

9.0(11)

-10.0(11)

-6.7(11)

C12

17.4(13)

27.3(16)

18.7(14)

2.7(11)

-5.9(11)

-9.9(12)

C13

13.5(12)

22.3(15)

20.9(14)

5.0(11)

-8.4(11)

-7.9(11)

C14

16.4(13)

24.8(15)

25.9(15)

7.8(12)

-10.8(12)

-7.1(12)

C15

20.4(14)

37.2(18)

15.5(14)

7.6(12)

-7.4(12)

-12.0(13)

C16

18.2(14)

30.1(16)

19.8(14)

-4.0(12)

-4.3(12)

-7.6(12)

C17

18.4(13)

23.4(15)

16.6(13)

7.4(11)

-10.7(11)

-7.8(11)

C18

18.0(13)

24.2(15)

9.9(12)

5.2(10)

-3.4(11)

-5.6(12)

C19

20.2(14)

27.4(16)

18.7(14)

4.9(11)

-8.5(12)

-10.3(12)

C20

32.7(16)

31.1(17)

18.3(14)

-1.5(12)

-6.6(13)

-15.7(14)

C21

31.6(17)

25.9(17)

22.0(15)

-6.4(12)

-7.9(13)

-1.0(13)

N1

14.5(11)

15.7(12)

15.8(11)

5.2(9)

-9.2(9)

-4.5(9)

N2

14.6(11)

17.1(12)

18.1(11)

0.8(9)

-7.5(9)

-2.6(9)

N3

12.9(11)

22.4(12)

12.7(11)

2.6(9)

-4.9(9)

-5.0(9)

N4

21.6(12)

23.3(13)

18.9(12)

7.4(10)

-6.7(10)

-7.3(11)

N5

12.9(11)

21.3(12)

14.9(11)

3.4(9)

-8.7(9)

-2.4(9)

N6

20.9(13)

30.7(15)

24.1(13)

-1.5(10)

-11.5(11)

-1.2(11)

C22

19.8(13)

19.3(14)

15.7(13)

5(1)

-8.1(11)

-6.4(11)

C23

16.0(13)

20.6(14)

16.0(13)

4.1(10)

-8.3(11)

-2.9(11)

C24

19.1(13)

16.4(14)

15.5(13)

3.4(10)

-9.3(11)

-2.5(11)

C25

16.8(13)

19.9(14)

15.9(13)

4.8(10)

-7.1(11)

-3.2(11)

C26

16.9(13)

17.2(14)

16.4(13)

2.2(10)

-7.8(11)

-2.5(11)

C27

19.0(13)

18.5(14)

16.4(13)

4.8(10)

-10.1(11)

-3.8(11)

C28

23.1(15)

44.2(19)

24.0(15)

12.6(13)

-12.8(13)

-15.1(14)

C29

15.3(13)

30.1(16)

23.1(14)

7.8(12)

-9.3(12)

-7.9(12)

C30

19.6(14)

29.5(17)

31.6(16)

5.4(13)

-13.7(13)

-9.3(13)

C31

20.3(14)

34.0(18)

29.5(16)

14.1(13)

-10.0(13)

-13.3(13)

C32

20.3(14)

37.1(18)

20.0(15)

6.1(13)

-5.6(12)

-5.3(13)

C33

15.4(13)

17.5(14)

19.8(13)

3.2(10)

-9.5(11)

-1.9(11)

C34

14.1(12)

21.3(14)

18.7(13)

4.1(11)

-10.0(11)

-2.3(11)

C35

19.1(14)

29.6(16)

21.4(14)

1.4(12)

-12.8(12)

-1.2(12)

C36

20.4(15)

39.4(19)

16.9(15)

10.1(13)

-9.2(12)

-1.9(13)

C37

15.0(13)

27.1(16)

26.3(15)

13.6(12)

-9.9(12)

-4.8(12)

C38

23.1(15)

24.3(16)

40.9(18)

16.8(13)

-19.4(14)

-8.8(13)

C39

20.0(14)

18.2(14)

26.2(15)

9.7(11)

-13.2(12)

-4.1(11)

C40

31.2(16)

18.9(15)

38.0(17)

6.3(12)

-20.1(14)

-8.5(13)

C41

26.8(15)

26.6(16)

37.2(17)

16.1(13)

-21.0(14)

-13.5(13)

C42

19.0(14)

23.8(15)

26.4(15)

8.7(12)

-9.8(12)

-5.8(12)

N7

20.0(12)

24.8(13)

19.2(12)

12(1)

-10.7(10)

-8.1(10)

N8

21.5(12)

21.7(14)

28.2(13)

7.5(11)

-10.2(11)

-6.6(11)

N9

14.0(11)

21.2(12)

15.5(12)

6.6(9)

-7.6(10)

-3.2(10)

N10

18.9(12)

20.6(13)

14.0(12)

3.6(9)

-7.2(10)

-3.1(10)

N11

14.5(11)

19.7(12)

17.0(12)

4.9(9)

-6.2(10)

-0.6(9)

N12

20.8(12)

18.9(13)

26.6(13)

6(1)

-14.1(10)

-7.3(10)

C43

22.3(15)

37.3(19)

27.0(16)

2.4(13)

-9.3(13)

-6.3(14)

Cl1

25.9(4)

81.0(7)

36.3(5)

2.0(4)

-15.4(4)

-18.3(4)

Cl2

41.0(5)

44.3(5)

54.1(5)

-10.5(4)

-26.8(4)

-6.6(4)

Cl3

73.9(7)

41.0(6)

90.3(8)

-21.7(5)

-57.1(6)

16.6(5)

C44

20.1(14)

33.4(17)

21.2(14)

0.6(12)

-10.4(12)

-6.4(13)

Cl4

31.6(4)

48.0(5)

37.5(4)

23.8(4)

-14.5(4)

-10.3(4)

Cl5

43.6(5)

46.6(5)

35.3(4)

-12.6(4)

-17.0(4)

-8.5(4)

Cl6

32.7(4)

31.1(4)

42.1(4)

11.8(3)

-17.6(4)

-15.3(3)

C45

34.3(18)

29.4(18)

46(2)

0.6(15)

-17.0(16)

-14.1(15)

Cl7

66.3(6)

22.4(4)

64.3(6)

-1.9(4)

-30.1(5)

-8.7(4)

Cl8

68.6(6)

28.2(5)

36.7(5)

4.2(3)

-18.3(4)

-11.3(4)

Cl9

34.7(4)

37.3(5)

38.0(4)

2.7(3)

-21.7(4)

-12.6(4)

 

Table 4 Bond Lengths for phw1114.

Atom

Atom

Length/Å

 

Atom

Atom

Length/Å

C1

C2

1.536(3)

 

C24

N9

1.473(3)

C1

C6

1.532(3)

 

C25

C26

1.525(3)

C1

N1

1.479(3)

 

C26

C27

1.525(3)

C2

C3

1.529(3)

 

C26

N11

1.484(3)

C3

C4

1.530(3)

 

C28

C29

1.492(4)

C3

N3

1.478(3)

 

C28

N7

1.463(3)

C4

C5

1.529(3)

 

C29

C30

1.370(4)

C5

C6

1.521(3)

 

C29

N8

1.363(4)

C5

N5

1.473(3)

 

C30

C31

1.409(4)

C7

C8

1.492(3)

 

C31

C32

1.356(4)

C7

N1

1.476(3)

 

C32

N8

1.368(3)

C8

C9

1.371(3)

 

C33

C34

1.486(3)

C8

N2

1.376(3)

 

C33

N9

1.483(3)

C9

C10

1.423(3)

 

C34

C35

1.380(3)

C10

C11

1.366(4)

 

C34

N10

1.365(3)

C11

N2

1.365(3)

 

C35

C36

1.414(4)

C12

C13

1.493(3)

 

C36

C37

1.367(4)

C12

N3

1.479(3)

 

C37

N10

1.375(3)

C13

C14

1.374(3)

 

C38

C39

1.496(4)

C13

N4

1.369(3)

 

C38

N11

1.472(3)

C14

C15

1.412(4)

 

C39

C40

1.364(4)

C15

C16

1.368(4)

 

C39

N12

1.366(3)

C16

N4

1.365(3)

 

C40

C41

1.415(4)

C17

C18

1.500(4)

 

C41

C42

1.362(4)

C17

N5

1.483(3)

 

C42

N12

1.368(3)

C18

C19

1.368(4)

 

C43

Cl1

1.750(3)

C18

N6

1.371(3)

 

C43

Cl2

1.757(3)

C19

C20

1.421(4)

 

C43

Cl3

1.749(3)

C20

C21

1.364(4)

 

C44

Cl4

1.773(3)

C21

N6

1.364(4)

 

C44

Cl5

1.753(3)

C22

C23

1.520(3)

 

C44

Cl6

1.760(3)

C22

C27

1.527(3)

 

C45

Cl7

1.763(3)

C22

N7

1.465(3)

 

C45

Cl8

1.766(3)

C23

C24

1.524(3)

 

C45

Cl9

1.757(3)

C24

C25

1.528(3)

 

 

 

 

 

Table 5 Bond Angles for phw1114.

Atom

Atom

Atom

Angle/˚

 

Atom

Atom

Atom

Angle/˚

C6

C1

C2

110.5(2)

 

N9

C24

C23

111.3(2)

N1

C1

C2

114.59(19)

 

N9

C24

C25

108.7(2)

N1

C1

C6

107.21(19)

 

C26

C25

C24

111.4(2)

C3

C2

C1

114.05(19)

 

C25

C26

C27

109.9(2)

C2

C3

C4

112.08(19)

 

N11

C26

C25

108.8(2)

N3

C3

C2

107.85(19)

 

N11

C26

C27

111.4(2)

N3

C3

C4

110.1(2)

 

C26

C27

C22

111.2(2)

C5

C4

C3

111.5(2)

 

N7

C28

C29

110.0(2)

C6

C5

C4

109.03(19)

 

C30

C29

C28

130.8(3)

N5

C5

C4

108.9(2)

 

N8

C29

C28

121.3(2)

N5

C5

C6

110.12(19)

 

N8

C29

C30

107.8(2)

C5

C6

C1

112.14(19)

 

C29

C30

C31

107.5(3)

N1

C7

C8

111.00(19)

 

C32

C31

C30

107.2(2)

C9

C8

C7

129.9(2)

 

C31

C32

N8

108.6(3)

C9

C8

N2

107.3(2)

 

N9

C33

C34

109.8(2)

N2

C8

C7

122.7(2)

 

C35

C34

C33

130.0(3)

C8

C9

C10

107.8(2)

 

N10

C34

C33

122.2(2)

C11

C10

C9

106.9(2)

 

N10

C34

C35

107.4(2)

N2

C11

C10

108.5(2)

 

C34

C35

C36

107.6(3)

N3

C12

C13

110.0(2)

 

C37

C36

C35

107.4(2)

C14

C13

C12

131.1(3)

 

C36

C37

N10

107.9(3)

N4

C13

C12

122.1(2)

 

N11

C38

C39

111.8(2)

N4

C13

C14

106.7(2)

 

C40

C39

C38

131.6(3)

C13

C14

C15

107.9(2)

 

C40

C39

N12

107.7(2)

C16

C15

C14

107.5(2)

 

N12

C39

C38

120.8(2)

N4

C16

C15

107.4(2)

 

C39

C40

C41

107.5(3)

N5

C17

C18

117.0(2)

 

C42

C41

C40

107.5(2)

C19

C18

C17

131.0(2)

 

C41

C42

N12

107.7(3)

C19

C18

N6

107.1(2)

 

C28

N7

C22

114.2(2)

N6

C18

C17

121.9(2)

 

C29

N8

C32

108.9(2)

C18

C19

C20

107.9(3)

 

C24

N9

C33

113.9(2)

C21

C20

C19

107.0(3)

 

C34

N10

C37

109.7(2)

N6

C21

C20

108.0(3)

 

C38

N11

C26

113.1(2)

C7

N1

C1

114.09(19)

 

C39

N12

C42

109.6(2)

C11

N2

C8

109.5(2)

 

Cl1

C43

Cl2

110.00(16)

C3

N3

C12

114.21(19)

 

Cl3

C43

Cl1

110.98(17)

C16

N4

C13

110.5(2)

 

Cl3

C43

Cl2

110.36(17)

C5

N5

C17

115.9(2)

 

Cl5

C44

Cl4

109.19(16)

C21

N6

C18

110.0(3)

 

Cl5

C44

Cl6

110.87(15)

C23

C22

C27

110.8(2)

 

Cl6

C44

Cl4

109.96(15)

N7

C22

C23

111.3(2)

 

Cl7

C45

Cl8

109.13(19)

N7

C22

C27

108.3(2)

 

Cl9

C45

Cl7

109.90(17)

C22

C23

C24

110.3(2)

 

Cl9

C45

Cl8

111.13(17)

C23

C24

C25

110.0(2)

 

 

 

 

 

 

Table 6 Torsion Angles for phw1114.

A

B

C

D

Angle/˚

C1

C2

C3

C4

48.8(3)

C1

C2

C3

N3

170.20(19)

C2

C1

C6

C5

55.2(3)

C2

C1

N1

C7

-54.2(3)

C2

C3

C4

C5

-53.3(3)

C2

C3

N3

C12

157.8(2)

C3

C4

C5

C6

58.6(3)

C3

C4

C5

N5

178.8(2)

C4

C3

N3

C12

-79.6(3)

C4

C5

C6

C1

-60.2(3)

C4

C5

N5

C17

172.3(2)

C6

C1

C2

C3

-49.1(3)

C6

C1

N1

C7

-177.2(2)

C6

C5

N5

C17

-68.3(3)

C7

C8

C9

C10

178.2(2)

C7

C8

N2

C11

-178.7(2)

C8

C7

N1

C1

-176.8(2)

C8

C9

C10

C11

-0.1(3)

C9

C8

N2

C11

-0.8(3)

C9

C10

C11

N2

-0.4(3)

C10

C11

N2

C8

0.8(3)

C12

C13

C14

C15

-175.8(3)

C12

C13

N4

C16

176.1(2)

C13

C12

N3

C3

-174.1(2)

C13

C14

C15

C16

0.0(3)

C14

C13

N4

C16

-0.4(3)

C14

C15

C16

N4

-0.2(3)

C15

C16

N4

C13

0.3(3)

C17

C18

C19

C20

180.0(2)

C17

C18

N6

C21

179.6(2)

C18

C17

N5

C5

-53.2(3)

C18

C19

C20

C21

0.4(3)

C19

C18

N6

C21

-0.4(3)

C19

C20

C21

N6

-0.6(3)

C20

C21

N6

C18

0.7(3)

N1

C1

C2

C3

-170.4(2)

N1

C1

C6

C5

-179.27(19)

N1

C7

C8

C9

-99.6(3)

N1

C7

C8

N2

77.8(3)

N2

C8

C9

C10

0.5(3)

N3

C3

C4

C5

-173.35(19)

N3

C12

C13

C14

98.9(3)

N3

C12

C13

N4

-76.6(3)

N4

C13

C14

C15

0.2(3)

N5

C5

C6

C1

-179.6(2)

N5

C17

C18

C19

-80.4(3)

N5

C17

C18

N6

99.5(3)

N6

C18

C19

C20

0.0(3)

C22

C23

C24

C25

-57.8(3)

C22

C23

C24

N9

-178.3(2)

C23

C22

C27

C26

-57.0(3)

C23

C22

N7

C28

72.5(3)

C23

C24

C25

C26

58.0(3)

C23

C24

N9

C33

-69.0(3)

C24

C25

C26

C27

-56.8(3)

C24

C25

C26

N11

-178.9(2)

C25

C24

N9

C33

169.7(2)

C25

C26

C27

C22

56.0(3)

C25

C26

N11

C38

175.5(2)

C27

C22

C23

C24

57.6(3)

C27

C22

N7

C28

-165.5(2)

C27

C26

N11

C38

54.3(3)

C28

C29

C30

C31

176.0(3)

C28

C29

N8

C32

-175.8(2)

C29

C28

N7

C22

164.0(2)

C29

C30

C31

C32

-0.6(3)

C30

C29

N8

C32

0.6(3)

C30

C31

C32

N8

1.0(3)

C31

C32

N8

C29

-1.0(3)

C33

C34

C35

C36

-173.8(3)

C33

C34

N10

C37

174.8(2)

C34

C33

N9

C24

-165.2(2)

C34

C35

C36

C37

-0.3(3)

C35

C34

N10

C37

0.5(3)

C35

C36

C37

N10

0.6(3)

C36

C37

N10

C34

-0.7(3)

C38

C39

C40

C41

178.5(3)

C38

C39

N12

C42

-178.7(2)

C39

C38

N11

C26

169.3(2)

C39

C40

C41

C42

0.5(3)

C40

C39

N12

C42

0.6(3)

C40

C41

C42

N12

-0.1(3)

C41

C42

N12

C39

-0.3(3)

N7

C22

C23

C24

178.1(2)

N7

C22

C27

C26

-179.3(2)

N7

C28

C29

C30

-116.4(3)

N7

C28

C29

N8

59.1(4)

N8

C29

C30

C31

0.0(3)

N9

C24

C25

C26

-179.9(2)

N9

C33

C34

C35

98.4(3)

N9

C33

C34

N10

-74.5(3)

N10

C34

C35

C36

-0.1(3)

N11

C26

C27

C22

176.5(2)

N11

C38

C39

C40

58.8(4)

N11

C38

C39

N12

-122.1(3)

N12

C39

C40

C41

-0.6(3)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1114.

Atom

x

y

z

U(eq)

H1

8689

2265

1687

15

H2A

9849

734

46

16

H2B

9650

1870

-33

16

H3

10916

1867

518

18

H4A

11203

-134

864

20

H4B

11790

528

1098

20

H5

10066

1534

2377

17

H6A

8479

1084

2795

19

H6B

9179

222

1884

19

H7A

7995

1925

95

20

H7B

7371

2846

941

20

H9A

6647

1167

-226

21

H10A

4568

1559

595

25

H11A

3769

2760

2097

24

H12A

13148

639

-511

26

H12B

12663

1697

-783

26

H14

13576

1846

-2799

26

H15

14899

621

-4341

29

H16

15233

-1031

-3791

29

H17A

9882

-34

4255

22

H17B

8887

419

3990

22

H19

10687

1390

4646

26

H20

9673

3195

5292

34

H21

7963

3661

5097

36

H22

4651

3476

-1442

22

H23A

4276

5525

-1139

22

H23B

3593

5070

-1488

22

H24

5195

4303

-2992

21

H25A

6860

4588

-3375

22

H25B

6306

5224

-2310

22

H26

6694

3170

-2607

21

H27A

5767

4362

-735

21

H27B

5981

3215

-861

21

H28A

2901

3557

-328

35

H28B

2357

4708

28

35

H30

1902

2578

1156

31

H31

1030

2866

3042

33

H32

1171

4416

3501

34

H33A

3243

6160

-2553

22

H33B

3933

5321

-3488

22

H35

4429

5984

-5304

28

H37

3564

8846

-4383

28

H38A

7996

2191

-2013

33

H38B

7641

2926

-1062

33

H40

9527

3730

-1592

33

H41

11516

2645

-2217

32

H42

11690

1024

-2876

29

H43

8227

7086

-6085

37

H44

5937

10342

-2975

30

H45

9821

4676

1678

44

H1A

7840(20)

1000(20)

1330(20)

30(9)

H2

5300(20)

3080(20)

2130(20)

32(9)

H3A

11540(20)

1096(19)

-1080(19)

14(7)

H4

14170(20)

-750(20)

-2010(20)

20(8)

H5A

11040(20)

112(19)

2744(18)

17(7)

H6

7990(20)

2190(20)

4430(20)

29(9)

H7

4090(20)

3670(20)

235(19)

18(8)

H8

2070(30)

5010(20)

1980(20)

37(10)

H9

5420(20)

5740(20)

-3580(20)

34(9)

H10

3300(20)

7900(20)

-3010(20)

23(8)

H11

8200(30)

3470(20)

-2880(20)

40(10)

H12

9840(20)

1140(20)

-2600(20)

25(8)

H36

4260(20)

7650(20)

-5840(20)

30(8)


[RSC Journal Format]

Experimental

Single crystals of C45H63Cl9N12 [phw1114] were []. A suitable crystal was selected and mounted on a Oxford Diffraction SuperNova diffractometer. The crystal was kept at 109.9 K. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the XL [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] XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
[3] XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122

Crystal structure determination of [phw1114]

Crystal Data. C45H63Cl9N12, =1091.12, triclinic, a = 14.3898(12) Å, b = 14.5637(14) Å, c = 15.0840(10) Å, α = 88.276(7)°, β = 63.722(8)°, γ = 71.729(9)°, = 2669.5(4) Å3, T = 109.9, space group P-1 (no. 2), Z = 2, μ(Mo Kα) = 0.516, 17691 reflections measured, 11923 unique (Rint = 0.0254) which were used in all calculations. The final wR(F2) was 0.1161 (all data).

This report has been created with Olex2, compiled on 2011.08.18 svn.r1932. Please let us know if there are any errors or if you would like to have additional featrues.