Homoleptische Methylverbindungen von Elementen der 4. und 5 ...

Praktischer Teil
Fortsetzung Tab. 52
Completeness to theta = 29.89° 100.0 %
Reflctions >2sigma(I)° 348
Refinement method Full-matrix least-squares on F 2
Data / restraints / parameters 350 / 0 / 19
Goodness-of-fit on F 2
1.218
Flack-Parameter 0.15(6)
Final R indices [I>2sigma(I)] R1 = 0.0173, wR 2 = 0.0408
R indices (all data) R1 = 0.0175, wR 2 = 0.0410
Absolute structure parameter 0.15(6)
Largest diff. peak and hole 0.293 and -0.283 e.Å -3
Tab. 53 Atomic coordinates (10 4 ) and equivalent isotropic displacement parameters (10 -1 pm 2 ) for
TiCl(CH ) . U(eq) is defined as one third of the trace of the orthogonalized Uij tensor.
3 3
x y z U(eq)
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Ti(1) 1383(1) 1383(1) 1383(1) 20(1)
C(1) 1238(1) 3329(1) 1238(1) 27(1)
Cl(1) 1113(1) -1113(1) 1113(1) 16(1)
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Tab. 54 Bond lengths [pm] and angles [°] for TiCl(CH 3 ) 3 .
Ti(1)-C(1) 206.05(15)
Ti(1)-C(1)#1 206.05(15)
Ti(1)-C(1)#2 206.05(15)
Ti(1)-Cl(1)#3 265.79(5)
Ti(1)-Cl(1)#4 265.79(5)
Ti(1)-Cl(1) 265.79(5)
C(1)-H(1) 93(3)
C(1)-H(2) 83.1(18)
Cl(1)-Ti(1)#3 265.79(5)
Cl(1)-Ti(1)#4 265.79(5)
C(1)-Ti(1)-C(1)#1 98.15(7)
C(1)-Ti(1)-C(1)#2 98.15(7)
C(1)#1-Ti(1)-C(1)#2 98.15(7)
C(1)-Ti(1)-Cl(1)#3 91.44(5)
C(1)#1-Ti(1)-Cl(1)#3 165.30(6)
Symmetry transformations used to generate equivalent atoms:
#1 y,z,x #2 z,x,y #3 -x,-y,z #4 x,-y,-z
84
C(1)#2-Ti(1)-Cl(1)#3 91.44(5)
C(1)-Ti(1)-Cl(1)#4 91.44(5)
C(1)#1-Ti(1)-Cl(1)#4 91.44(4)
C(1)#2-Ti(1)-Cl(1)#4 165.30(6)
Cl(1)#3-Ti(1)-Cl(1)#4 77.13(2)
C(1)-Ti(1)-Cl(1) 165.30(6)
C(1)#1-Ti(1)-Cl(1) 91.44(5)
C(1)#2-Ti(1)-Cl(1) 91.44(5)
Cl(1)#3-Ti(1)-Cl(1) 77.13(2)
Cl(1)#4-Ti(1)-Cl(1) 77.13(2)
Ti(1)-C(1)-H(1) 106.7(15)
Ti(1)-C(1)-H(2) 113.1(13)
H(1)-C(1)-H(2) 107.3(19)
Ti(1)-Cl(1)-Ti(1)#3 101.528(16)
Ti(1)-Cl(1)-Ti(1)#4 101.528(16)
Ti(1)#3-Cl(1)-Ti(1)#4 101.529(16)
Tab. 55 Anisotropic displacement parameters (10 -1 pm 2 ) for TiCl(CH 3 ) 3 . The anisotropic
displacement factor exponent takes the form: -2π 2 [ h 2 a 2 U11 + ... + 2 h k a* b* U12 ]
U11 U22 U33 U23 U13 U12
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Ti(1) 20(1) 20(1) 20(1) -4(1) -4(1) -4(1)
C(1) 29(1) 22(1) 29(1) -2(1) -2(1) -2(1)
Cl(1) 16(1) 16(1) 16(1) 1(1) -1(1) 1(1)
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