S 2´-(Hexadeylmercapto)uridin OK 268

Identification code

d:\x-data\kacz1

Empirical formula

C25 H44 N2 O5 S

Formula weight

484.68

Temperature

100(2) K

Wavelength

0.71073 A

Crystal system, space group

Monoclinic, P 21

Unit cell dimensions

a = 7.4662(15) A alpha = 90 deg

b = 5.5675(7) A beta = 92.569(18) deg

c = 33.317(9) A gamma = 90 deg.

Volume

1383.5(5) A³

Z, Calculated density

2, 1.163 Mg/m³

Absorption coefficient

0.152 mm^-1

F(000)

528

Crystal size

0.60 x 0.20 x 0.05 mm

Theta range for data collection

3.22 to 23.78 deg.

Limiting indices

-8<=h<=8, -5<=k<=6, -37<=l<=37

Reflections collected / unique

12447 / 4014 [R(int) = 0.2407]

Completeness to theta

= 23.78 98.3 %

Max. and min. transmission

0.9925 and 0.9145

Refinement method

Full-matrix least-squares on F²

Data / restraints / parameters

4014 / 1 / 161

Goodness-of-fit on F²

1.658

Final R indices [I>2sigma(I)]

R1 = 0.2331, wR2 = 0.5058

R indices (all data)

R1 = 0.3132, wR2 = 0.5508

Absolute structure parameter

0.0(6)

Largest diff. peak and hole

1.099 and -0.622 e.A^-3

X

Y

Z

U(eq)

C(1)

-5150(30)

-1700(40)

-8585(6)

72(6)

C(2)

-7030(30)

-1780(40)

-8406(6)

56(5)

C(3)

-8110(20)

-2230(40)

-8770(5)

48(4)

C(4)

-5290(30)

-3620(40)

-8911(5)

52(5)

C(5)

-9080(30)

70(40)

8948(7)

74(7)

C(6)

-2740(30)

-5070(40)

-9307(6)

54(5)

C(7)

-1890(20)

-2770(30)

-9895(5)

46(5)

C(8)

-3360(30)

-1000(40)

-9825(6)

54(5)

C(9)

-4290(30)

-1330(40)

-9504(6)

54(5)

C(10)

-2770(30)

520(40)

-8062(6)

61(5)

C(11)

-1120(30)

430(40)

-7773(6)

68(6)

C(12)

-360(30)

2810(50)

-7618(6)

65(5)

C(13)

1330(30)

2760(50)

-7391(6)

62(5)

C(14)

1940(30)

5180(50)

-7242(7)

85(7)

C(15)

3970(30)

5140(40)

-7051(6)

62(6)

C(16)

4780(30)

7620(60)

-6944(7)

88(7)

C(17)

6460(30)

7450(50)

-6738(7)

76(6)

C(18)

7190(30)

9820(40)

-6615(7)

69(6)

C(19)

9210(40)

9790(50)

-6390(8)

86(7)

C(20)

9810(40)

12130(60)

-6270(8)

94(8)

C(21)

11790(40)

12110(60)

-6068(9)

109(10)

C(22)

12380(40)

14630(50)

-5934(8)

89(8)

C(23)

14420(50)

14550(70)

-5725(10)

115(10)

C(24)

15080(60)

17060(110)

-5546(14)

189(19)

C(25)

17260(50)

17340(90)

-5367(10)

141(12)

N(1)

-4153(18)

-3220(30)

-9246(4)

41(3)

N(2)

-1780(20)

-4530(30)

-9626(4)

53(4)

O(1)

-7118(16)

-3240(20)

-9084(3)

53(3)

O(2)

-7055(16)

-3800(30)

-8146(5)

83(5)

O(3)

-7675(18)

1780(20)

-8983(6)

82(5)

O(4)

-2553(17)

-6640(20)

-9087(4)

61(4)

O(5)

-1026(16)

-2670(30)

-10196(4)

66(4)

S(1)

-3178(7)

-2385(10)

-8260(2)

67(2)

Tabelle 8: Atomic coordinates ( x 10⁴) and equivalent isotropic displacement parameters A² x 10³) for OK-268. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor

C(1)-C(4)

1.52(3)

C(1)-C(2)

1.55(3)

C(1)-S(1)

1.83(2)

C(1)-H(1)

1.0000

C(2)-O(2)

1.42(2)

C(2)-C(3)

1.45(3)

C(2)-H(2)

1.0000

C(3)-O(1)

1.42(2)

C(3)-C(5)

1.58(3)

C(3)-H(3)

1.0000

C(4)-N(1)

1.45(2)

C(4)-O(1)

1.47(2)

C(4)-H(4)

1.0000

C(5)-O(3)

1.42(3)

C(5)-H(5A)

0.9900

C(5)-H(5B)

0.9900

C(6)-O(4)

1.14(2)

C(6)-N(2)

1.34(2)

C(6)-N(1)

1.49(2)

C(7)-O(5)

1.216(19)

C(7)-N(2)

1.33(2)

C(7)-C(8)

1.50(3)

C(8)-C(9)

1.32(3)

C(8)-H(8)

0.9500

C(9)-N(1)

1.36(2)

C(9)-H(9)

0.9500

C(10)-C(11)

1.53(3)

C(10)-S(1)

1.77(2)

C(10)-H(10A)

0.9900

C(10)-H(10B)

0.9900

C(11)-C(12)

1.52(3)

C(11)-H(11A)

0.9900

C(11)-H(11B)

0.9900

C(12)-C(13)

1.44(3)

C(12)-H(12A)

0.9900

C(12)-H(12B)

0.9900

C(13)-C(14)

1.50(4)

C(13)-H(13A)

0.9900

C(13)-H(13B)

0.9900

C(14)-C(15)

1.62(3)

C(14)-H(14A)

0.9900

C(14)-H(14B)

0.9900

C(15)-C(16)

1.54(4)

C(15)-H(15A)

0.9900

C(15)-H(15B)

0.9900

C(16)-C(17)

1.41(3)

C(16)-H(16A)

0.9900

C(16)-H(16B)

0.9900

C(17)-C(18)

1.48(3)

C(17)-H(17A)

0.9900

C(17)-H(17B)

0.9900

C(18)-C(19)

1.66(3)

C(18)-H(18A)

0.9900

C(18)-H(18B)

0.9900

C(19)-C(20)

1.42(4)

C(19)-H(19A)

0.9900

C(19)-H(19B)

0.9900

C(20)-C(21)

1.60(4)

C(20)-H(20A)

0.9900

C(20)-H(20B)

0.9900

C(21)-C(22)

1.53(4)

C(21)-H(21A)

0.9900

C(21)-H(21B)

0.9900

C(22)-C(23)

1.65(4)

C(22)-H(22A)

0.9900

C(22)-H(22B)

0.9900

C(23)-C(24)

1.59(6)

C(23)-H(23A)

0.9900

C(23)-H(23B)

0.9900

C(24)-C(25)

1.72(5)

C(24)-H(24A)

0.9900

C(24)-H(24B)

0.9900

C(25)-H(25A)

0.9800

C(25)-H(25B)

0.9800

C(25)-H(25C)

0.9800

N(2)-H(2N)

0.8800

O(2)-H(2O)

0.8400

O(3)-H(3O)

0.8400

C(4)-C(1)-C(2)

102.7(17)

C(4)-C(1)-S(1)

107.7(15)

C(2)-C(1)-S(1)

118.9(15)

C(4)-C(1)-H(1)

109.0

C(2)-C(1)-H(1)

109.0

S(1)-C(1)-H(1)

109.0

O(2)-C(2)-C(3)

110.7(17)

O(2)-C(2)-C(1)

107.0(17)

C(3)-C(2)-C(1)

99.3(15)

O(2)-C(2)-H(2)

113.0

C(3)-C(2)-H(2)

113.0

C(1)-C(2)-H(2)

113.0

O(1)-C(3)-C(2)

113.4(15)

O(1)-C(3)-C(5)

106.7(14)

C(2)-C(3)-C(5)

113.6(18)

O(1)-C(3)-H(3)

107.6

C(2)-C(3)-H(3)

107.6

C(5)-C(3)-H(3)

107.6

N(1)-C(4)-O(1)

103.9(13)

N(1)-C(4)-C(1)

114.7(17)

O(1)-C(4)-C(1)

102.3(15)

N(1)-C(4)-H(4)

111.7

O(1)-C(4)-H(4)

111.7

C(1)-C(4)-H(4)

111.7

O(3)-C(5)-C(3)

104.5(17)

O(3)-C(5)-H(5A)

110.8

C(3)-C(5)-H(5A)

110.8

O(3)-C(5)-H(5B)

110.8

C(3)-C(5)-H(5B)

110.8

H(5A)-C(5)-H(5B)

108.9

O(4)-C(6)-N(2)

128(2)

O(4)-C(6)-N(1)

120.5(17)

N(2)-C(6)-N(1)

111.1(17)

O(5)-C(7)-N(2)

125.1(17)

O(5)-C(7)-C(8)

120.8(17)

N(2)-C(7)-C(8)

113.7(15)

C(9)-C(8)-C(7)

116.7(19)

C(9)-C(8)-H(8)

121.6

C(7)-C(8)-H(8)

121.6

C(8)-C(9)-N(1)

126.6(19)

C(8)-C(9)-H(9)

116.7

N(1)-C(9)-H(9)

116.7

C(11)-C(10)-S(1)

108.9(16)

C(11)-C(10)-H(10A)

109.9

S(1)-C(10)-H(10A)

109.9

C(11)-C(10)-H(10B)

109.9

S(1)-C(10)-H(10B)

109.9

H(10A)-C(10)-H(10B)

108.3

C(12)-C(11)-C(10)

117.6(19)

C(12)-C(11)-H(11A)

107.9

C(10)-C(11)-H(11A)

107.9

C(12)-C(11)-H(11B)

107.9

C(10)-C(11)-H(11B)

107.9

H(11A)-C(11)-H(11B)

107.2

C(13)-C(12)-C(11)

118(2)

C(13)-C(12)-H(12A)

107.8

C(11)-C(12)-H(12A)

107.8

C(13)-C(12)-H(12B)

107.8

C(11)-C(12)-H(12B)

107.8

H(12A)-C(12)-H(12B)

107.2

C(12)-C(13)-C(14)

114(2)

C(12)-C(13)-H(13A)

108.8

C(14)-C(13)-H(13A)

108.8

C(12)-C(13)-H(13B)

108.8

C(14)-C(13)-H(13B)

108.8

H(13A)-C(13)-H(13B)

107.7

C(13)-C(14)-C(15)

112(2)

C(13)-C(14)-H(14A)

109.1

C(15)-C(14)-H(14A)

109.1

C(13)-C(14)-H(14B)

109.1

C(15)-C(14)-H(14B)

109.1

H(14A)-C(14)-H(14B)

107.8

C(16)-C(15)-C(14)

115.4(19)

C(16)-C(15)-H(15A)

108.4

C(14)-C(15)-H(15A)

108.4

C(16)-C(15)-H(15B)

108.4

C(14)-C(15)-H(15B)

108.4

H(15A)-C(15)-H(15B)

107.5

C(17)-C(16)-C(15)

112(3)

C(17)-C(16)-H(16A)

109.1

C(15)-C(16)-H(16A)

109.1

C(17)-C(16)-H(16B)

109.1

C(15)-C(16)-H(16B)

109.1

H(16A)-C(16)-H(16B)

107.8

C(16)-C(17)-C(18)

112(2)

C(16)-C(17)-H(17A)

109.1

C(18)-C(17)-H(17A)

109.1

C(16)-C(17)-H(17B)

109.1

C(18)-C(17)-H(17B)

109.1

H(17A)-C(17)-H(17B)

107.9

C(17)-C(18)-C(19)

116(2)

C(17)-C(18)-H(18A)

108.3

C(19)-C(18)-H(18A)

108.3

C(17)-C(18)-H(18B)

108.3

C(19)-C(18)-H(18B)

108.3

H(18A)-C(18)-H(18B)

107.4

C(20)-C(19)-C(18)

113(2)

C(20)-C(19)-H(19A)

109.0

C(18)-C(19)-H(19A)

109.0

C(20)-C(19)-H(19B)

109.0

C(18)-C(19)-H(19B)

109.0

H(19A)-C(19)-H(19B)

107.8

C(19)-C(20)-C(21)

113(2)

C(19)-C(20)-H(20A)

109.1

C(21)-C(20)-H(20A)

109.1

C(19)-C(20)-H(20B)

109.1

C(21)-C(20)-H(20B)

109.1

H(20A)-C(20)-H(20B)

107.8

C(22)-C(21)-C(20)

112(2)

C(22)-C(21)-H(21A)

109.3

C(20)-C(21)-H(21A)

109.3

C(22)-C(21)-H(21B)

109.3

C(20)-C(21)-H(21B)

109.3

H(21A)-C(21)-H(21B)

108.0

C(21)-C(22)-C(23)

111(2)

C(21)-C(22)-H(22A)

109.5

C(23)-C(22)-H(22A)

109.5

C(21)-C(22)-H(22B)

109.5

C(23)-C(22)-H(22B)

109.5

H(22A)-C(22)-H(22B)

108.1

C(24)-C(23)-C(22)

114(3)

C(24)-C(23)-H(23A)

108.8

C(22)-C(23)-H(23A)

108.8

C(24)-C(23)-H(23B)

108.8

C(22)-C(23)-H(23B)

108.8

H(23A)-C(23)-H(23B)

107.7

C(23)-C(24)-C(25)

119(4)

C(23)-C(24)-H(24A)

107.6

C(25)-C(24)-H(24A)

107.6

C(23)-C(24)-H(24B)

107.6

C(25)-C(24)-H(24B)

107.6

H(24A)-C(24)-H(24B)

107.0

C(24)-C(25)-H(25A)

109.5

C(24)-C(25)-H(25B)

109.5

H(25A)-C(25)-H(25B)

109.5

C(24)-C(25)-H(25C)

109.5

H(25A)-C(25)-H(25C)

109.5

H(25B)-C(25)-H(25C)

109.5

C(9)-N(1)-C(4)

125.0(16)

C(9)-N(1)-C(6)

118.7(15)

C(4)-N(1)-C(6)

116.3(15)

C(7)-N(2)-C(6)

133.0(18)

C(7)-N(2)-H(2N)

113.5

C(6)-N(2)-H(2N)

113.5

C(3)-O(1)-C(4)

105.7(12)

C(2)-O(2)-H(2O)

109.5

C(5)-O(3)-H(3O)

109.5

C(10)-S(1)-C(1)

98.6(11)

Tabelle 9: Bond lengths [A] and angles [deg] for OK-268

Symmetry transformations used to generate equivalent atoms:

U11

U22

U33

U23

U13

U12

O(2)

11(6)

117(15)

121(13)

27(11)

3(7)

-8(7)

O(3)

44(8)

9(6)

191(17)

4(8)

-5(9)

7(5)

O(4)

40(7)

33(8)

111(11)

22(7)

22(7)

22(6)

O(5)

50(8)

67(10)

85(9)

9(8)

31(7)

26(8)

S(1)

49(3)

40(3)

113(4)

4(3)

5(3)

28(3)

Tabelle 10: Anisotropic displacement parameters (A²x10³) for OK-268. The anisotropic displacement factor exponent takes the form: -2 pi² [h² a•² U11 + 2 h k a• b• U12]

x

y

z

U(eq)

H(1)

-4980

-97

-8714

87

H(2)

-7359

-247

-8270

68

H(3)

-9063

-3416

-8703

58

H(4)

-5137

-5267

-8796

63

H(5A)

-9668

-271

-9214

89

H(5B)

-9988

668

-8765

89

H(8)

-3599

303

-10004

65

H(9)

-5151

-136

-9447

65

H(10A)

-2564

1659

-8283

73

H(10B)

-3826

1073

-7918

73

H(11A)

-1427

-553

-7538

81

H(11B)

-159

-433

-7909

81

H(12A)

-223

3876

-7852

77

H(12B)

-1256

3552

-7448

77

H(13A)

2259

2088

-7563

74

H(13B)

1225

1674

-7159

74

H(14A)

1120

5736

-7036

101

H(14B)

1861

6335

-7468

101

H(15A)

3999

4144

-6805

75

H(15B)

4748

4347

-7245

75

H(16A)

4908

8555

-7194

105

H(16B)

3945

8503

-6775

105

H(17A)

7318

6645

-6914

91

H(17B)

6349

6434

-6496

91

H(18A)

6348

10573

-6432

83

H(18B)

7230

10844

-6857

83

H(19A)

9197

8747

-6150

104

H(19B)

10078

9101

-6575

104

H(20A)

8975

12793

-6076

112

H(20B)

9783

13191

-6508

112

H(21A)

11828

11025

-5833

131

H(21B)

12635

11481

-6263

131

H(22A)

11539

15265

-5740

106

H(22B)

12360

15714

-6170

106

H(23A)

14454

13350

-5506

138

H(23B)

15264

14024

-5928

138

H(24A)

14294

17476

-5324

227

H(24B)

14870

18286

-5758

227

H(25A)

17495

16178

-5149

169

H(25B)

17465

18968

-5265

169

H(25C)

18070

17017

-5584

169

H(2N)

-913

-5559

-9666

64

H(2O)

-6168

-3731

-7981

125

H(3O)

-8111

3097

-9064

122

Tabelle 11: Hydrogencoordinates (x 10⁴) and isotropic displacement parameters (A²x10³) for OK-268

C(4)-C(1)-C(2)-O(2)

78.5(18)

S(1)-C(1)-C(2)-O(2)

-40(2)

C(4)-C(1)-C(2)-C(3)

-37(2)

S(1)-C(1)-C(2)-C(3)

-155.3(16)

O(2)-C(2)-C(3)-O(1)

-91.2(19)

C(1)-C(2)-C(3)-O(1)

21(2)

O(2)-C(2)-C(3)-C(5)

146.7(17)

C(1)-C(2)-C(3)-C(5)

-101.0(19)

C(2)-C(1)-C(4)-N(1)

151.9(17)

S(1)-C(1)-C(4)-N(1)

-81.8(18)

C(2)-C(1)-C(4)-O(1)

40.1(18)

S(1)-C(1)-C(4)-O(1)

166.4(13)

O(1)-C(3)-C(5)-O(3)

-72(2)

C(2)-C(3)-C(5)-O(3)

53(2)

O(5)-C(7)-C(8)-C(9)

176(2)

N(2)-C(7)-C(8)-C(9)

3(3)

C(7)-C(8)-C(9)-N(1)

-5(3)

S(1)-C(10)-C(11)-C(12)

170.7(16)

C(10)-C(11)-C(12)-C(13)

-171.6(18)

C(11)-C(12)-C(13)-C(14)

-178.2(19)

C(12)-C(13)-C(14)-C(15)

-170.8(17)

C(13)-C(14)-C(15)-C(16)

172.0(19)

C(14)-C(15)-C(16)-C(17)

173.2(19)

C(15)-C(16)-C(17)-C(18)

-176.8(19)

C(16)-C(17)-C(18)-C(19)

-177.2(19)

C(17)-C(18)-C(19)-C(20)

-178(2)

C(18)-C(19)-C(20)-C(21)

-178(2)

C(19)-C(20)-C(21)-C(22)

-179(2)

C(20)-C(21)-C(22)-C(23)

180(2)

C(21)-C(22)-C(23)-C(24)

-175(3)

C(22)-C(23)-C(24)-C(25)

-173(3)

C(8)-C(9)-N(1)-C(4)

-176(2)

C(8)-C(9)-N(1)-C(6)

4(3)

O(1)-C(4)-N(1)-C(9)

47(2)

C(1)-C(4)-N(1)-C(9)

-64(2)

O(1)-C(4)-N(1)-C(6)

-132.3(15)

C(1)-C(4)-N(1)-C(6)

116.9(18)

O(4)-C(6)-N(1)-C(9)

177.5(19)

N(2)-C(6)-N(1)-C(9)

0(2)

O(4)-C(6)-N(1)-C(4)

-3(3)

N(2)-C(6)-N(1)-C(4)

179.4(16)

O(5)-C(7)-N(2)-C(6)

-172(2)

C(8)-C(7)-N(2)-C(6)

1(3)

O(4)-C(6)-N(2)-C(7)

-179(2)

N(1)-C(6)-N(2)-C(7)

-2(3)

C(2)-C(3)-O(1)-C(4)

4(2)

C(5)-C(3)-O(1)-C(4)

129.5(16)

N(1)-C(4)-O(1)-C(3)

-147.1(15)

C(1)-C(4)-O(1)-C(3)

-27.4(18)

C(11)-C(10)-S(1)-C(1)

-179.5(15)

C(4)-C(1)-S(1)-C(10)

157.0(15)

C(2)-C(1)-S(1)-C(10

-86.9(19)

Tabelle 12: Torsion angles [deg] for OK-268

Arabino- O 2, O 2´-Anhydro( O 3´, O 5´-tetraisopropyldisilyl)uridin OK 321

Identification code

d:\x-data\kacz2

Empirical formula

C22 H37 Cl3 N2 O6 Si2

Formula weight

588.07

Temperature

150(2) K

Wavelength

0.71073 A

Crystal system, space group

Monoclinic, P 21

Unit cell dimensions

a = 8.104 A alpha = 90 deg.

b = 10.382 A beta = 91.08 deg.

c = 16.842 A gamma = 90 deg.

Volume

1416.8 A³

Z, Calculated density

2, 1.379 Mg/m³

Absorption coefficient

0.447 mm^-1

F(000)

620

Crystal size

0.52 x 0.32 x 0.24 mm

Theta range for data collection

2.30 to 25.89 deg.

Limiting indices

-9<=h<=9, -12<=k<=12, -20<=l<=20

Reflections collected / unique

10250 / 5476 [R(int) = 0.0161]

Completeness to theta

= 25.89 99.5 %

Absorption correction

None

Max. and min. transmission

0.9004 and 0.8009

Refinement method

Full-matrix least-squares on F²

Data / restraints / parameters

5476 / 1 / 373

Goodness-of-fit on F²

1.044

Final R indices [I>2sigma(I)]

R1 = 0.0289, wR2 = 0.0698

R indices (all data)

R1 = 0.0315, wR2 = 0.0705

Absolute structure parameter

-0.02(5)

Largest diff. peak and hole

0.651 and -0.418 e e.A^-3

X

Y

Z

U(eq)

C(1)

1424(4)

6701(3)

2804(2)

50(1)

C(2)

3126(5)

6644(4)

3065(3)

77(1)

C(3)

941(4)

5785(3)

2132(2)

40(1)

C(4)

-1744(3)

8324(2)

2617(1)

24(1)

C(5)

-2393(4)

7773(3)

3396(2)

46(1)

C(6)

-2466(3)

9666(3)

2454(2)

34(1)

C(7)

817(3)

11824(2)

3928(2)

27(1)

C(8)

-132(4)

11369(3)

4643(2)

44(1)

C(9)

1521(4)

13170(3)

4064(2)

54(1)

C(10)

4030(3)

10118(2)

4245(1)

25(1)

C(11)

3406(4)

9421(3)

4983(2)

47(1)

C(12)

5181(4)

11200(4)

4502(2)

67(1)

C(13)

2307(3)

11670(2)

2096(1)

21(1)

C(14)

2545(3)

10832(2)

1383(1)

20(1)

C(15)

4221(3)

10061(2)

430(1)

18(1)

C(16)

7261(3)

10115(2)

57(1)

19(1)

C(17)

8639(3)

9406(2)

4(1)

19(1)

C(18)

8645(2)

8054(2)

227(1)

17(1)

C(19)

5948(2)

8291(2)

584(1)

15(1)

C(20)

3269(3)

8896(2)

747(1)

20(1)

C(21)

2590(2)

9386(2)

1533(1)

19(1)

C(22)

6468(3)

3193(2)

2003(1)

26(1)

O(1)

1021(2)

8881(2)

1719(1)

23(1)

O(2)

1296(2)

9348(2)

3276(1)

22(1)

O(3)

3266(2)

11257(2)

2770(1)

20(1)

O(4)

4150(2)

11040(1)

1031(1)

19(1)

O(5)

4475(2)

7864(2)

844(1)

21(1)

O(6)

9845(2)

7343(2)

119(1)

24(1)

Si(1)

552(1)

8344(1)

2610(1)

19(1)

Si(2)

2337(1)

10627(1)

3551(1)

17(1)

Cl(1)

5199(1)

4467(1)

1674(1)

49(1)

Cl(2)

7302(1)

3552(1)

2948(1)

45(1)

Cl(3)

8031(1)

2908(1)

1314(1)

32(1)

N(1)

5865(2)

9540(2)

358(1)

17(1)

N(2)

7210(2)

7538(2)

555(1)

17(1)

Tabelle 13: Atomic coordinates ( x 10⁴) and equivalent isotropic displacement parameters A²x 10³ for OK-321. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor

C(1)-C(2)

1.441(4)

C(1)-C(3)

1.524(4)

C(1)-Si(1)

1.872(3)

C(1)-H(1)

1.0000

C(2)-H(2A)

0.9800

C(2)-H(2B)

0.9800

C(2)-H(2C)

0.9800

C(3)-H(3A)

0.9800

C(3)-H(3B)

0.9800

C(3)-H(3C)

0.9800

C(4)-C(5)

1.533(3)

C(4)-C(6)

1.534(4)

C(4)-Si(1)

1.861(2)

C(4)-H(4)

0.94(3)

C(5)-H(5A)

0.9800

C(5)-H(5B)

0.9800

C(5)-H(5C)

0.9800

C(6)-H(6A)

0.9800

C(6)-H(6B)

0.9800

C(6)-H(6C)

0.9800

C(7)-C(8)

1.516(4)

C(7)-C(9)

1.525(4)

C(7)-Si(2)

1.870(2)

C(7)-H(7)

0.83(3)

C(8)-H(8A)

0.9800

C(8)-H(8B)

0.9800

C(8)-H(8C)

0.9800

C(9)-H(9A)

0.9800

C(9)-H(9B)

0.9800

C(9)-H(9C)

0.9800

C(10)-C(12)

1.518(4)

C(10)-C(11)

1.532(3)

C(10)-Si(2)

1.863(2)

C(10)-H(10)

0.95(4)

C(11)-H(11A)

0.9800

C(11)-H(11B)

0.9800

C(11)-H(11C)

0.9800

C(12)-H(12A)

0.9800

C(12)-H(12B)

0.9800

C(12)-H(12C)

0.9800

C(13)-O(3)

1.430(3)

C(13)-C(14)

1.498(3)

C(13)-H(13A)

0.96(2)

C(13)-H(13B)

1.01(3)

C(14)-O(4)

1.456(2)

C(14)-C(21)

1.523(3)

C(14)-H(14)

0.99(2)

C(15)-O(4)

1.437(2)

C(15)-N(1)

1.445(3)

C(15)-C(20)

1.536(3)

C(15)-H(153)

0.93(3)

C(16)-C(17)

1.341(3)

C(16)-N(1)

1.385(3)

C(16)-H(16)

0.96(3)

C(17)-C(18)

1.453(3)

C(17)-H(17)

0.92(3)

C(18)-O(6)

1.238(2)

C(18)-N(2)

1.403(3)

C(19)-N(2)

1.290(3)

C(19)-N(1)

1.353(3)

C(19)-O(5)

1.353(2)

C(20)-O(5)

1.457(3)

C(20)-C(21)

1.531(3)

C(20)-H(20)

0.90(3)

C(21)-O(1)

1.415(2)

C(21)-H(21)

1.00(3)

C(22)-Cl(2)

1.757(2)

C(22)-Cl(1)

1.759(2)

C(22)-Cl(3)

1.759(2)

C(22)-H(22)

0.83(3)

O(1)-Si(1)

1.6524(16)

O(2)-Si(2)

1.6354(16)

O(2)-Si(1)

1.6368(15)

O(3)-Si(2)

1.6611(15)

C(2)-C(1)-C(3)

115.6(3)

C(2)-C(1)-Si(1)

116.5(2)

C(3)-C(1)-Si(1)

110.40(19)

C(2)-C(1)-H(1)

104.2

C(3)-C(1)-H(1)

104.2

Si(1)-C(1)-H(1)

104.2

C(1)-C(2)-H(2A)

109.5

C(1)-C(2)-H(2B)

109.5

H(2A)-C(2)-H(2B)

109.5

C(1)-C(2)-H(2C)

109.5

H(2A)-C(2)-H(2C)

109.5

H(2B)-C(2)-H(2C)

109.5

C(1)-C(3)-H(3A)

109.5

C(1)-C(3)-H(3B)

109.5

H(3A)-C(3)-H(3B)

109.5

C(1)-C(3)-H(3C)

109.5

H(3A)-C(3)-H(3C)

109.5

H(3B)-C(3)-H(3C)

109.5

C(5)-C(4)-C(6)

110.9(2)

C(5)-C(4)-Si(1)

111.64(17)

C(6)-C(4)-Si(1)

111.52(16)

C(5)-C(4)-H(4)

110.2(16)

C(6)-C(4)-H(4)

107.5(16)

Si(1)-C(4)-H(4)

104.9(15)

C(4)-C(5)-H(5A)

109.5

C(4)-C(5)-H(5B)

109.5

H(5A)-C(5)-H(5B)

109.5

C(4)-C(5)-H(5C)

109.5

H(5A)-C(5)-H(5C)

109.5

H(5B)-C(5)-H(5C)

109.5

C(4)-C(6)-H(6A)

109.5

C(4)-C(6)-H(6B)

109.5

H(6A)-C(6)-H(6B)

109.5

C(4)-C(6)-H(6C)

109.5

H(6A)-C(6)-H(6C)

109.5

H(6B)-C(6)-H(6C)

109.5

C(8)-C(7)-C(9)

111.1(2)

C(8)-C(7)-Si(2)

114.20(19)

C(9)-C(7)-Si(2)

114.41(18)

C(8)-C(7)-H(7)

106(2)

C(9)-C(7)-H(7)

105(2)

Si(2)-C(7)-H(7)

105(2)

C(7)-C(8)-H(8A)

109.5

C(7)-C(8)-H(8B)

109.5

H(8A)-C(8)-H(8B)

109.5

C(7)-C(8)-H(8C)

109.5

H(8A)-C(8)-H(8C)

109.5

H(8B)-C(8)-H(8C)

109.5

C(7)-C(9)-H(9A)

109.5

C(7)-C(9)-H(9B)

109.5

H(9A)-C(9)-H(9B)

109.5

C(7)-C(9)-H(9C)

109.5

H(9A)-C(9)-H(9C)

109.5

H(9B)-C(9)-H(9C)

109.5

C(12)-C(10)-C(11)

109.2(2)

C(12)-C(10)-Si(2)

114.2(2)

C(11)-C(10)-Si(2)

113.14(17)

C(12)-C(10)-H(10)

104(2)

C(11)-C(10)-H(10)

111(2)

Si(2)-C(10)-H(10)

104(2)

C(10)-C(11)-H(11A)

109.5

C(10)-C(11)-H(11B)

109.5

H(11A)-C(11)-H(11B)

109.5

C(10)-C(11)-H(11C)

109.5

H(11A)-C(11)-H(11C)

109.5

H(11B)-C(11)-H(11C)

109.5

C(10)-C(12)-H(12A)

109.5

C(10)-C(12)-H(12B)

109.5

H(12A)-C(12)-H(12B)

109.5

C(10)-C(12)-H(12C)

109.5

H(12A)-C(12)-H(12C)

109.5

H(12B)-C(12)-H(12C)

109.5

O(3)-C(13)-C(14)

112.71(18)

O(3)-C(13)-H(13A)

110.4(13)

C(14)-C(13)-H(13A)

105.9(14)

O(3)-C(13)-H(13B)

111.2(16)

C(14)-C(13)-H(13B)

106.1(15)

H(13A)-C(13)-H(13B)

110(2)

O(4)-C(14)-C(13)

111.63(18)

O(4)-C(14)-C(21)

101.25(16)

C(13)-C(14)-C(21)

116.30(18)

O(4)-C(14)-H(14)

108.7(14)

C(13)-C(14)-H(14)

112.6(14)

C(21)-C(14)-H(14)

105.6(15)

O(4)-C(15)-N(1)

111.92(17)

O(4)-C(15)-C(20)

106.61(16)

N(1)-C(15)-C(20)

101.79(17)

O(4)-C(15)-H(153)

109.6(16)

N(1)-C(15)-H(153)

111.7(15)

C(20)-C(15)-H(153)

114.9(16)

C(17)-C(16)-N(1)

118.3(2)

C(17)-C(16)-H(16)

124.5(15)

N(1)-C(16)-H(16)

117.1(15)

C(16)-C(17)-C(18)

120.77(19)

C(16)-C(17)-H(17)

116.8(16)

C(18)-C(17)-H(17)

122.2(16)

O(6)-C(18)-N(2)

119.30(19)

O(6)-C(18)-C(17)

122.51(18)

N(2)-C(18)-C(17)

118.17(17)

N(2)-C(19)-N(1)

127.30(18)

N(2)-C(19)-O(5)

121.25(18)

N(1)-C(19)-O(5)

111.43(17)

O(5)-C(20)-C(21)

113.51(17)

O(5)-C(20)-C(15)

106.10(16)

C(21)-C(20)-C(15)

103.28(17)

O(5)-C(20)-H(20)

109.6(17)

C(21)-C(20)-H(20)

111.5(15)

C(15)-C(20)-H(20)

112.6(16)

O(1)-C(21)-C(14)

112.50(17)

O(1)-C(21)-C(20)

114.06(17)

C(14)-C(21)-C(20)

101.08(17)

O(1)-C(21)-H(21)

114.6(14)

C(14)-C(21)-H(21)

105.1(15)

C(20)-C(21)-H(21)

108.4(15)

Cl(2)-C(22)-Cl(1)

109.81(14)

Cl(2)-C(22)-Cl(3)

111.32(13)

Cl(1)-C(22)-Cl(3)

110.02(13)

Cl(2)-C(22)-H(22)

109.4(18)

Cl(1)-C(22)-H(22)

106.6(18)

Cl(3)-C(22)-H(22)

109.6(18)

C(21)-O(1)-Si(1)

123.28(13)

Si(2)-O(2)-Si(1)

153.14(10)

C(13)-O(3)-Si(2)

119.93(13)

C(15)-O(4)-C(14)

103.26(15)

C(19)-O(5)-C(20)

108.48(16)

O(2)-Si(1)-O(1)

108.61(8)

O(2)-Si(1)-C(4)

111.00(10)

O(1)-Si(1)-C(4)

104.86(9)

O(2)-Si(1)-C(1)

109.13(10)

O(1)-Si(1)-C(1)

111.91(14)

C(4)-Si(1)-C(1)

111.26(14)

O(2)-Si(2)-O(3)

109.56(8)

O(2)-Si(2)-C(10)

108.51(10)

O(3)-Si(2)-C(10)

105.62(9)

O(2)-Si(2)-C(7)

107.25(10)

O(3)-Si(2)-C(7)

108.59(10)

C(10)-Si(2)-C(7)

117.18(11)

C(19)-N(1)-C(16)

118.67(17)

C(19)-N(1)-C(15)

112.10(17)

C(16)-N(1)-C(15)

129.10(18)

C(19)-N(2)-C(18)

116.57(17)

Tabelle 14: Bond lengths [A] and angles [deg] for OK-321

Symmetry transformations used to generate equivalent atoms:

U11

U22

U33

U23

U13

U12

C(1)

62(2)

23(1)

65(2)

-12(1)

-33(2)

16(1)

C(2)

77(3)

43(2)

108(3)

-28(2)

-55(2)

29(2)

C(3)

46(2)

22(1)

52(2)

-11(1)

-8(1)

2(1)

C(4)

22(1)

29(1)

21(1)

-1(1)

0(1)

-8(1)

C(5)

47(2)

51(2)

41(2)

8(1)

16(1)

-16(2)

C(6)

21(1)

42(2)

38(1)

5(1)

-3(1)

4(1)

C(7)

26(1)

26(1)

28(1)

-8(1)

-1(1)

6(1)

C(8)

39(2)

45(2)

48(2)

-13(1)

19(1)

5(1)

C(9)

64(2)

27(2)

73(2)

-19(1)

28(2)

0(1)

C(10)

21(1)

30(1)

25(1)

-3(1)

-4(1)

1(1)

C(11)

41(2)

56(2)

44(2)

26(1)

-10(1)

-5(1)

C(12)

62(2)

76(3)

59(2)

26(2)

-39(2)

-41(2)

C(13)

21(1)

21(1)

22(1)

0(1)

1(1)

6(1)

C(14)

17(1)

24(1)

18(1)

-2(1)

-1(1)

5(1)

C(15)

17(1)

22(1)

15(1)

-3(1)

-1(1)

5(1)

C(16)

25(1)

15(1)

16(1)

3(1)

4(1)

-3(1)

C(17)

20(1)

19(1)

18(1)

-1(1)

4(1)

-4(1)

C(18)

18(1)

17(1)

15(1)

-4(1)

-1(1)

0(1)

C(19)

18(1)

15(1)

13(1)

-4(1)

0(1)

-4(1)

C(20)

15(1)

23(1)

22(1)

-8(1)

-3(1)

1(1)

C(21)

13(1)

25(1)

21(1)

-5(1)

-1(1)

-1(1)

C(22)

26(1)

29(1)

23(1)

2(1)

1(1)

1(1)

O(1)

15(1)

32(1)

21(1)

-7(1)

0(1)

-5(1)

O(2)

24(1)

20(1)

21(1)

-3(1)

-3(1)

-3(1)

O(3)

20(1)

21(1)

19(1)

-4(1)

-1(1)

0(1)

O(4)

20(1)

18(1)

19(1)

-4(1)

3(1)

2(1)

O(5)

17(1)

16(1)

29(1)

-3(1)

6(1)

-3(1)

O(6)

20(1)

22(1)

29(1)

-5(1)

3(1)

3(1)

Si(1)

19(1)

16(1)

21(1)

-4(1)

-5(1)

1(1)

Si(2)

16(1)

18(1)

17(1)

-5(1)

-2(1)

1(1)

Cl(1)

49(1)

59(1)

40(1)

18(1)

8(1)

28(1)

Cl(2)

58(1)

55(1)

23(1)

-1(1)

-8(1)

1(1)

Cl(3)

30(1)

37(1)

31(1)

0(1)

7(1)

3(1)

N(1)

18(1)

14(1)

17(1)

1(1)

0(1)

2(1)

N(2)

19(1)

13(1)

18(1)

-2(1)

2(1)

-1(1)

Tabelle 15: Anisotropic displacement parameters (A²x10³ for OK-321. The anisotropic displacement factor exponent takes the form: -2 pi²[h² a•² U11 + 2 h k a• b• U12]

X

Y

Z

U(eq)

H(1)

796

6379

3269

60

H(2A)

3428

5748

3179

92

H(2B)

3277

7164

3547

92

H(2C)

3831

6981

2647

92

H(3A)

1404

4930

2242

48

H(3B)

1372

6111

1631

48

H(3C)

-265

5725

2092

48

H(4)

-2060(30)

7790(30)

2190(15)

29(7)

H(5A)

-2001

8304

3841

55

H(5B)

-1991

6889

3465

55

H(5C)

-3602

7772

3378

55

H(6A)

-2044

9996

1952

40

H(6B)

-2144

10250

2887

40

H(6C)

-3673

9609

2419

40

H(7)

120(40)

11910(30)

3564(19)

44(9)

H(8A)

621

11299

5103

52

H(8B)

-623

10525

4529

52

H(8C)

-1007

11989

4759

52

H(9A)

639

13750

4230

65

H(9B)

1994

13489

3570

65

H(9C)

2383

13135

4480

65

H(10)

4700(40)

9570(40)

3940(20)

58(10)

H(11A)

2730

8680

4819

56

H(11B)

2738

10014

5296

56

H(11C)

4349

9121

5305

56

H(12A)

4609

11773

4868

80

H(12B)

5517

11688

4034

80

H(12C)

6160

10836

4769

80

H(13A)

1150(30)

11630(20)

2207(13)

13(5)

H(13B)

2620(30)

12570(30)

1930(16)

33(7)

H(14)

1680(30)

10960(20)

971(14)

21(6)

H(153)

3820(30)

10390(30)

-48(15)

23(6)

H(16)

7180(30)

11010(30)

-85(14)

24(6)

H(17)

9540(30)

9800(30)

-218(15)

26(7)

H(20)

2450(30)

8640(30)

411(14)

24(6)

H(21)

3460(30)

9260(30)

1957(14)

24(6)

H(22)

5870(30)

2550(30)

2033(15)

25(7)

Tabelle 16: Hydrogen coordinates ( x 10⁴) and isotropic displacement parameters (A²x 10³) for OK-321

O(3)-C(13)-C(14)-O(4)

-73.0(2)

O(3)-C(13)-C(14)-C(21)

42.5(3)

N(1)-C(16)-C(17)-C(18)

2.5(3)

C(16)-C(17)-C(18)-O(6)

173.3(2)

C(16)-C(17)-C(18)-N(2)

-4.8(3)

O(4)-C(15)-C(20)-O(5)

-115.59(16)

N(1)-C(15)-C(20)-O(5)

1.81(19)

O(4)-C(15)-C(20)-C(21)

4.1(2)

N(1)-C(15)-C(20)-C(21)

121.47(17)

O(4)-C(14)-C(21)-O(1)

-167.21(15)

C(13)-C(14)-C(21)-O(1)

71.6(2)

O(4)-C(14)-C(21)-C(20)

-45.15(18)

C(13)-C(14)-C(21)-C(20)

-166.32(18)

O(5)-C(20)-C(21)-O(1)

-99.9(2)

C(15)-C(20)-C(21)-O(1)

145.67(18)

O(5)-C(20)-C(21)-C(14)

139.12(17)

C(15)-C(20)-C(21)-C(14)

24.70(19)

C(14)-C(21)-O(1)-Si(1)

-110.30(18)

C(20)-C(21)-O(1)-Si(1)

135.32(16)

C(14)-C(13)-O(3)-Si(2)

-110.47(18)

N(1)-C(15)-O(4)-C(14)

-143.44(17)

C(20)-C(15)-O(4)-C(14)

-32.96(19)

C(13)-C(14)-O(4)-C(15)

173.35(17)

C(21)-C(14)-O(4)-C(15)

48.96(18)

N(2)-C(19)-O(5)-C(20)

-175.39(17)

N(1)-C(19)-O(5)-C(20)

3.1(2)

C(21)-C(20)-O(5)-C(19)

-115.75(18)

C(15)-C(20)-O(5)-C(19)

-3.0(2)

Si(2)-O(2)-Si(1)-O(1)

-3.2(3)

Si(2)-O(2)-Si(1)-C(4)

-118.0(2)

Si(2)-O(2)-Si(1)-C(1)

119.0(3)

C(21)-O(1)-Si(1)-O(2)

42.95(18)

C(21)-O(1)-Si(1)-C(4)

161.67(17)

C(21)-O(1)-Si(1)-C(1)

-77.59(19)

C(5)-C(4)-Si(1)-O(2)

-66.1(2)

C(6)-C(4)-Si(1)-O(2)

58.57(18)

C(5)-C(4)-Si(1)-O(1)

176.85(19)

C(6)-C(4)-Si(1)-O(1)

-58.53(18)

C(5)-C(4)-Si(1)-C(1)

55.7(2)

C(6)-C(4)-Si(1)-C(1)

-179.70(18)

C(2)-C(1)-Si(1)-O(2)

-37.9(4)

C(3)-C(1)-Si(1)-O(2)

-172.4(2)

C(2)-C(1)-Si(1)-O(1)

82.3(3)

C(3)-C(1)-Si(1)-O(1)

-52.1(3)

C(2)-C(1)-Si(1)-C(4)

-160.7(3)

C(3)-C(1)-Si(1)-C(4)

64.8(3)

Si(1)-O(2)-Si(2)-O(3)

-6.6(3)

Si(1)-O(2)-Si(2)-C(10)

-121.5(2)

Si(1)-O(2)-Si(2)-C(7)

111.1(2)

C(13)-O(3)-Si(2)-O(2)

59.23(16)

C(13)-O(3)-Si(2)-C(10)

175.91(16)

C(13)-O(3)-Si(2)-C(7)

-57.61(18)

C(12)-C(10)-Si(2)-O(2)

175.6(2)

C(11)-C(10)-Si(2)-O(2)

-58.5(2)

C(12)-C(10)-Si(2)-O(3)

58.2(2)

C(11)-C(10)-S i(2)-O(3)

-175.9(2)

C(12)-C(10)-Si(2)-C(7)

-62.8(3)

C(11)-C(10)-Si(2)-C(7)

63.0(2)

C(8)-C(7)-Si(2)-O(2)

61.4(2)

C(9)-C(7)-Si(2)-O(2)

-168.9(2)

C(8)-C(7)-Si(2)-O(3)

179.75(18)

C(9)-C(7)-Si(2)-O(3)

-50.6(2)

C(8)-C(7)-Si(2)-C(10)

-60.8(2)

C(9)-C(7)-Si(2)-C(10)

68.8(2)

N(2)-C(19)-N(1)-C(16)

0.1(3)

O(5)-C(19)-N(1)-C(16)

-178.28(16)

N(2)-C(19)-N(1)-C(15)

176.46(19)

O(5)-C(19)-N(1)-C(15)

-2.0(2)

C(17)-C(16)-N(1)-C(19)

-0.2(3)

C(17)-C(16)-N(1)-C(15)

-175.78(19)

O(4)-C(15)-N(1)-C(19)

113.46(19)

C(20)-C(15)-N(1)-C(19)

0.0(2)

O(4)-C(15)-N(1)-C(16)

-70.7(3)

C(20)-C(15)-N(1)-C(16)

175.81(19)

N(1)-C(19)-N(2)-C(18)

-2.4(3)

O(5)-C(19)-N(2)-C(18)

175.84(16)

O(6)-C(18)-N(2)-C(19)

-173.66(18)

C(17)-C(18)-N(2)-C(19)

4.6(3)

Tabelle 17: Torsion angles [deg] for OK-321