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Crystals of hexa-
tert-butyldisilane, C
24H
54Si
2, undergo a reversible phase transition at 179 (2) K. The space group changes from
Ibca (high temperature) to
Pbca (low temperature), but the lattice constants
a,
b and
c do not change significantly during the phase transition. The crystallographic twofold axis of the molecule in the high-temperature phase is replaced by a noncrystallographic twofold axis in the low-temperature phase. The angle between the two axes is 2.36 (4)°. The centre of the molecule undergoes a translation of 0.123 (1) Å during the phase transition, but the conformation angles of the molecule remain unchanged. Between the two tri-
tert-butylsilyl subunits there are six short repulsive intramolecular C—H
H—C contacts, with H
H distances between 2.02 and 2.04 Å, resulting in a significant lengthening of the Si—Si and Si—C bonds. The Si—Si bond length is 2.6863 (5) Å and the Si—C bond lengths are between 1.9860 (14) and 1.9933 (14) Å. Torsion angles about the Si—Si and Si—C bonds deviate by approximately 15° from the values expected for staggered conformations due to intramolecular steric H
H repulsions. A new polymorph is reported for the crystal structure of 1,1,2,2-tetra-
tert-butyl-1,2-diphenyldisilane, C
28H
46Si
2. It has two independent molecules with rather similar conformations. The Si—Si bond lengths are 2.4869 (8) and 2.4944 (8) Å. The C—Si—Si—C torsion angles deviate by between −3.4 (1) and −18.5 (1)° from the values expected for a staggered conformation. These deviations result from steric interactions. Four Si—C(
t-Bu) bonds are almost staggered, while the other four Si—C(
t-Bu) bonds are intermediate between a staggered and an eclipsed conformation. The latter Si—C(
t-Bu) bonds are about 0.019 (2) Å longer than the staggered Si—C(
t-Bu) bonds.
Supporting information
CCDC references: 1007691; 1007692
For both compounds, data collection: SMART (Siemens, 1995); cell refinement: SMART (Siemens, 1995); data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
(I) Hexa-
tert-butyldisilane
top
Crystal data top
C24H54Si2 | F(000) = 1808 |
Mr = 398.85 | Dx = 1.015 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 371 reflections |
a = 11.2923 (8) Å | θ = 3–26° |
b = 29.204 (3) Å | µ = 0.14 mm−1 |
c = 15.8321 (16) Å | T = 147 K |
V = 5221.1 (8) Å3 | Rod, colorless |
Z = 8 | 0.75 × 0.27 × 0.14 mm |
Data collection top
Siemens SMART 1K CCD diffractometer | 7483 independent reflections |
Radiation source: normal-focus sealed tube | 4986 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
ω scans | θmax = 30.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −15→15 |
Tmin = 0.856, Tmax = 0.980 | k = −41→41 |
58910 measured reflections | l = −21→20 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.05P)2 + 0.8P] where P = (Fo2 + 2Fc2)/3 |
7483 reflections | (Δ/σ)max = 0.001 |
253 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.24 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Si1 | 0.17754 (3) | 0.124481 (12) | 0.56117 (2) | 0.01561 (10) | |
Si2 | 0.34409 (3) | 0.127976 (12) | 0.44019 (2) | 0.01567 (10) | |
C1 | 0.01469 (12) | 0.13043 (5) | 0.51447 (10) | 0.0243 (3) | |
C2 | −0.08188 (13) | 0.11645 (7) | 0.57885 (11) | 0.0399 (4) | |
H2A | −0.1602 | 0.1234 | 0.5555 | 0.060* | |
H2B | −0.0705 | 0.1335 | 0.6315 | 0.060* | |
H2C | −0.0761 | 0.0835 | 0.5903 | 0.060* | |
C3 | −0.01244 (13) | 0.18029 (5) | 0.48846 (11) | 0.0329 (4) | |
H3A | −0.0930 | 0.1821 | 0.4657 | 0.049* | |
H3B | 0.0442 | 0.1901 | 0.4452 | 0.049* | |
H3C | −0.0057 | 0.2003 | 0.5379 | 0.049* | |
C4 | −0.00989 (13) | 0.10131 (5) | 0.43568 (10) | 0.0311 (4) | |
H4A | −0.0910 | 0.1068 | 0.4163 | 0.047* | |
H4B | −0.0002 | 0.0688 | 0.4496 | 0.047* | |
H4C | 0.0459 | 0.1097 | 0.3909 | 0.047* | |
C5 | 0.18333 (13) | 0.06576 (5) | 0.62495 (9) | 0.0247 (3) | |
C6 | 0.30907 (14) | 0.05040 (5) | 0.64885 (10) | 0.0318 (4) | |
H6A | 0.3053 | 0.0209 | 0.6783 | 0.048* | |
H6B | 0.3452 | 0.0733 | 0.6860 | 0.048* | |
H6C | 0.3569 | 0.0472 | 0.5975 | 0.048* | |
C7 | 0.11442 (15) | 0.06725 (6) | 0.70932 (10) | 0.0369 (4) | |
H7A | 0.1138 | 0.0367 | 0.7348 | 0.055* | |
H7B | 0.0329 | 0.0772 | 0.6987 | 0.055* | |
H7C | 0.1529 | 0.0888 | 0.7479 | 0.055* | |
C8 | 0.12939 (16) | 0.02598 (5) | 0.57365 (11) | 0.0371 (4) | |
H8A | 0.1357 | −0.0025 | 0.6062 | 0.056* | |
H8B | 0.1724 | 0.0227 | 0.5202 | 0.056* | |
H8C | 0.0458 | 0.0325 | 0.5620 | 0.056* | |
C9 | 0.19898 (12) | 0.17452 (5) | 0.64523 (9) | 0.0225 (3) | |
C10 | 0.08987 (14) | 0.18213 (6) | 0.70264 (10) | 0.0352 (4) | |
H10A | 0.1092 | 0.2047 | 0.7462 | 0.053* | |
H10B | 0.0678 | 0.1531 | 0.7295 | 0.053* | |
H10C | 0.0235 | 0.1933 | 0.6685 | 0.053* | |
C11 | 0.30305 (13) | 0.16440 (5) | 0.70498 (10) | 0.0286 (3) | |
H11A | 0.3143 | 0.1903 | 0.7435 | 0.043* | |
H11B | 0.3753 | 0.1597 | 0.6718 | 0.043* | |
H11C | 0.2859 | 0.1367 | 0.7378 | 0.043* | |
C12 | 0.22530 (14) | 0.22154 (5) | 0.60588 (11) | 0.0318 (4) | |
H12A | 0.2375 | 0.2441 | 0.6509 | 0.048* | |
H12B | 0.1583 | 0.2310 | 0.5706 | 0.048* | |
H12C | 0.2969 | 0.2195 | 0.5711 | 0.048* | |
C13 | 0.31336 (12) | 0.17872 (5) | 0.35889 (9) | 0.0229 (3) | |
C14 | 0.27842 (14) | 0.22426 (5) | 0.40074 (11) | 0.0310 (4) | |
H14A | 0.2625 | 0.2472 | 0.3570 | 0.047* | |
H14B | 0.3433 | 0.2349 | 0.4369 | 0.047* | |
H14C | 0.2071 | 0.2197 | 0.4350 | 0.047* | |
C15 | 0.21142 (13) | 0.16659 (5) | 0.29861 (10) | 0.0285 (3) | |
H15A | 0.1950 | 0.1927 | 0.2616 | 0.043* | |
H15B | 0.1404 | 0.1593 | 0.3315 | 0.043* | |
H15C | 0.2338 | 0.1400 | 0.2643 | 0.043* | |
C16 | 0.42090 (14) | 0.19045 (6) | 0.30226 (11) | 0.0348 (4) | |
H16A | 0.3971 | 0.2129 | 0.2595 | 0.052* | |
H16B | 0.4491 | 0.1626 | 0.2743 | 0.052* | |
H16C | 0.4845 | 0.2033 | 0.3371 | 0.052* | |
C17 | 0.34969 (13) | 0.07047 (5) | 0.37334 (9) | 0.0251 (3) | |
C18 | 0.22682 (15) | 0.05198 (5) | 0.34840 (10) | 0.0329 (4) | |
H18A | 0.2361 | 0.0230 | 0.3180 | 0.049* | |
H18B | 0.1868 | 0.0743 | 0.3120 | 0.049* | |
H18C | 0.1794 | 0.0469 | 0.3994 | 0.049* | |
C19 | 0.41818 (15) | 0.07537 (6) | 0.28926 (10) | 0.0372 (4) | |
H19A | 0.4261 | 0.0452 | 0.2626 | 0.056* | |
H19B | 0.4970 | 0.0880 | 0.3005 | 0.056* | |
H19C | 0.3749 | 0.0960 | 0.2514 | 0.056* | |
C20 | 0.41077 (15) | 0.03161 (5) | 0.42263 (10) | 0.0355 (4) | |
H20A | 0.4088 | 0.0034 | 0.3890 | 0.053* | |
H20B | 0.3692 | 0.0266 | 0.4762 | 0.053* | |
H20C | 0.4932 | 0.0401 | 0.4341 | 0.053* | |
C21 | 0.50546 (12) | 0.13774 (5) | 0.48782 (9) | 0.0240 (3) | |
C22 | 0.53571 (13) | 0.10779 (5) | 0.56483 (10) | 0.0299 (4) | |
H22A | 0.6143 | 0.1161 | 0.5861 | 0.045* | |
H22B | 0.5355 | 0.0755 | 0.5482 | 0.045* | |
H22C | 0.4766 | 0.1127 | 0.6092 | 0.045* | |
C23 | 0.52267 (13) | 0.18761 (5) | 0.51742 (11) | 0.0335 (4) | |
H23A | 0.6032 | 0.1915 | 0.5393 | 0.050* | |
H23B | 0.4654 | 0.1946 | 0.5621 | 0.050* | |
H23C | 0.5103 | 0.2084 | 0.4697 | 0.050* | |
C24 | 0.60486 (13) | 0.12825 (6) | 0.42309 (11) | 0.0392 (4) | |
H24A | 0.6814 | 0.1369 | 0.4475 | 0.059* | |
H24B | 0.5905 | 0.1462 | 0.3718 | 0.059* | |
H24C | 0.6057 | 0.0956 | 0.4089 | 0.059* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.01472 (17) | 0.01753 (17) | 0.0146 (2) | −0.00121 (13) | 0.00001 (14) | −0.00181 (15) |
Si2 | 0.01544 (18) | 0.01680 (17) | 0.0148 (2) | 0.00162 (13) | 0.00021 (14) | 0.00224 (15) |
C1 | 0.0155 (7) | 0.0341 (8) | 0.0232 (8) | −0.0015 (6) | −0.0008 (6) | −0.0032 (6) |
C2 | 0.0167 (7) | 0.0689 (12) | 0.0343 (10) | −0.0051 (7) | 0.0029 (7) | −0.0034 (9) |
C3 | 0.0217 (7) | 0.0410 (9) | 0.0360 (10) | 0.0110 (7) | −0.0062 (7) | −0.0053 (8) |
C4 | 0.0246 (8) | 0.0420 (9) | 0.0267 (9) | −0.0084 (6) | −0.0055 (7) | −0.0046 (7) |
C5 | 0.0310 (8) | 0.0237 (7) | 0.0194 (8) | −0.0057 (6) | 0.0018 (6) | 0.0041 (6) |
C6 | 0.0418 (9) | 0.0258 (7) | 0.0278 (9) | 0.0021 (7) | 0.0003 (7) | 0.0086 (7) |
C7 | 0.0421 (10) | 0.0425 (9) | 0.0262 (10) | −0.0071 (8) | 0.0076 (8) | 0.0113 (8) |
C8 | 0.0523 (10) | 0.0229 (7) | 0.0359 (11) | −0.0147 (7) | 0.0008 (8) | 0.0045 (7) |
C9 | 0.0224 (7) | 0.0248 (7) | 0.0204 (8) | 0.0039 (5) | −0.0027 (6) | −0.0077 (6) |
C10 | 0.0311 (8) | 0.0481 (10) | 0.0265 (9) | 0.0087 (7) | 0.0023 (7) | −0.0161 (8) |
C11 | 0.0304 (8) | 0.0339 (8) | 0.0216 (9) | 0.0010 (6) | −0.0077 (6) | −0.0082 (7) |
C12 | 0.0376 (9) | 0.0222 (7) | 0.0355 (10) | 0.0023 (6) | −0.0063 (7) | −0.0096 (7) |
C13 | 0.0241 (7) | 0.0244 (7) | 0.0201 (8) | −0.0009 (6) | −0.0012 (6) | 0.0086 (6) |
C14 | 0.0365 (9) | 0.0210 (7) | 0.0355 (10) | −0.0007 (6) | −0.0060 (7) | 0.0081 (7) |
C15 | 0.0304 (8) | 0.0326 (8) | 0.0225 (9) | 0.0007 (6) | −0.0067 (7) | 0.0087 (7) |
C16 | 0.0313 (8) | 0.0432 (9) | 0.0299 (10) | −0.0051 (7) | 0.0027 (7) | 0.0183 (8) |
C17 | 0.0336 (8) | 0.0240 (7) | 0.0178 (8) | 0.0080 (6) | 0.0030 (6) | −0.0025 (6) |
C18 | 0.0464 (10) | 0.0260 (8) | 0.0264 (9) | −0.0011 (7) | −0.0014 (7) | −0.0081 (7) |
C19 | 0.0458 (10) | 0.0431 (9) | 0.0226 (9) | 0.0116 (8) | 0.0090 (8) | −0.0064 (7) |
C20 | 0.0504 (10) | 0.0252 (8) | 0.0310 (10) | 0.0160 (7) | 0.0034 (8) | −0.0035 (7) |
C21 | 0.0156 (7) | 0.0332 (7) | 0.0233 (8) | 0.0011 (6) | 0.0010 (6) | 0.0066 (6) |
C22 | 0.0217 (7) | 0.0416 (9) | 0.0264 (9) | 0.0056 (6) | −0.0032 (6) | 0.0060 (7) |
C23 | 0.0236 (8) | 0.0383 (9) | 0.0386 (10) | −0.0127 (6) | −0.0069 (7) | 0.0080 (8) |
C24 | 0.0182 (7) | 0.0663 (12) | 0.0329 (10) | 0.0034 (7) | 0.0030 (7) | 0.0115 (9) |
Geometric parameters (Å, º) top
Si1—C1 | 1.9895 (14) | C12—H12A | 0.9800 |
Si1—C5 | 1.9911 (14) | C12—H12B | 0.9800 |
Si1—C9 | 1.9913 (14) | C12—H12C | 0.9800 |
Si1—Si2 | 2.6863 (5) | C13—C15 | 1.537 (2) |
Si2—C17 | 1.9860 (14) | C13—C14 | 1.537 (2) |
Si2—C21 | 1.9926 (14) | C13—C16 | 1.548 (2) |
Si2—C13 | 1.9933 (14) | C14—H14A | 0.9800 |
C1—C4 | 1.535 (2) | C14—H14B | 0.9800 |
C1—C3 | 1.544 (2) | C14—H14C | 0.9800 |
C1—C2 | 1.548 (2) | C15—H15A | 0.9800 |
C2—H2A | 0.9800 | C15—H15B | 0.9800 |
C2—H2B | 0.9800 | C15—H15C | 0.9800 |
C2—H2C | 0.9800 | C16—H16A | 0.9800 |
C3—H3A | 0.9800 | C16—H16B | 0.9800 |
C3—H3B | 0.9800 | C16—H16C | 0.9800 |
C3—H3C | 0.9800 | C17—C20 | 1.5404 (19) |
C4—H4A | 0.9800 | C17—C18 | 1.540 (2) |
C4—H4B | 0.9800 | C17—C19 | 1.546 (2) |
C4—H4C | 0.9800 | C18—H18A | 0.9800 |
C5—C6 | 1.536 (2) | C18—H18B | 0.9800 |
C5—C8 | 1.543 (2) | C18—H18C | 0.9800 |
C5—C7 | 1.546 (2) | C19—H19A | 0.9800 |
C6—H6A | 0.9800 | C19—H19B | 0.9800 |
C6—H6B | 0.9800 | C19—H19C | 0.9800 |
C6—H6C | 0.9800 | C20—H20A | 0.9800 |
C7—H7A | 0.9800 | C20—H20B | 0.9800 |
C7—H7B | 0.9800 | C20—H20C | 0.9800 |
C7—H7C | 0.9800 | C21—C22 | 1.539 (2) |
C8—H8A | 0.9800 | C21—C23 | 1.542 (2) |
C8—H8B | 0.9800 | C21—C24 | 1.545 (2) |
C8—H8C | 0.9800 | C22—H22A | 0.9800 |
C9—C12 | 1.537 (2) | C22—H22B | 0.9800 |
C9—C11 | 1.5373 (19) | C22—H22C | 0.9800 |
C9—C10 | 1.547 (2) | C23—H23A | 0.9800 |
C10—H10A | 0.9800 | C23—H23B | 0.9800 |
C10—H10B | 0.9800 | C23—H23C | 0.9800 |
C10—H10C | 0.9800 | C24—H24A | 0.9800 |
C11—H11A | 0.9800 | C24—H24B | 0.9800 |
C11—H11B | 0.9800 | C24—H24C | 0.9800 |
C11—H11C | 0.9800 | | |
| | | |
C1—Si1—C5 | 107.10 (6) | C9—C12—H12A | 109.5 |
C1—Si1—C9 | 107.26 (6) | C9—C12—H12B | 109.5 |
C5—Si1—C9 | 106.80 (6) | H12A—C12—H12B | 109.5 |
C1—Si1—Si2 | 112.26 (5) | C9—C12—H12C | 109.5 |
C5—Si1—Si2 | 111.80 (5) | H12A—C12—H12C | 109.5 |
C9—Si1—Si2 | 111.32 (5) | H12B—C12—H12C | 109.5 |
C17—Si2—C21 | 107.07 (6) | C15—C13—C14 | 105.96 (12) |
C17—Si2—C13 | 106.87 (6) | C15—C13—C16 | 106.19 (13) |
C21—Si2—C13 | 107.29 (6) | C14—C13—C16 | 105.04 (12) |
C17—Si2—Si1 | 111.72 (5) | C15—C13—Si2 | 111.10 (9) |
C21—Si2—Si1 | 112.08 (5) | C14—C13—Si2 | 114.18 (10) |
C13—Si2—Si1 | 111.51 (4) | C16—C13—Si2 | 113.70 (10) |
C4—C1—C3 | 105.65 (12) | C13—C14—H14A | 109.5 |
C4—C1—C2 | 105.17 (12) | C13—C14—H14B | 109.5 |
C3—C1—C2 | 106.54 (12) | H14A—C14—H14B | 109.5 |
C4—C1—Si1 | 114.88 (10) | C13—C14—H14C | 109.5 |
C3—C1—Si1 | 111.40 (9) | H14A—C14—H14C | 109.5 |
C2—C1—Si1 | 112.56 (11) | H14B—C14—H14C | 109.5 |
C1—C2—H2A | 109.5 | C13—C15—H15A | 109.5 |
C1—C2—H2B | 109.5 | C13—C15—H15B | 109.5 |
H2A—C2—H2B | 109.5 | H15A—C15—H15B | 109.5 |
C1—C2—H2C | 109.5 | C13—C15—H15C | 109.5 |
H2A—C2—H2C | 109.5 | H15A—C15—H15C | 109.5 |
H2B—C2—H2C | 109.5 | H15B—C15—H15C | 109.5 |
C1—C3—H3A | 109.5 | C13—C16—H16A | 109.5 |
C1—C3—H3B | 109.5 | C13—C16—H16B | 109.5 |
H3A—C3—H3B | 109.5 | H16A—C16—H16B | 109.5 |
C1—C3—H3C | 109.5 | C13—C16—H16C | 109.5 |
H3A—C3—H3C | 109.5 | H16A—C16—H16C | 109.5 |
H3B—C3—H3C | 109.5 | H16B—C16—H16C | 109.5 |
C1—C4—H4A | 109.5 | C20—C17—C18 | 105.95 (13) |
C1—C4—H4B | 109.5 | C20—C17—C19 | 106.28 (12) |
H4A—C4—H4B | 109.5 | C18—C17—C19 | 105.20 (13) |
C1—C4—H4C | 109.5 | C20—C17—Si2 | 111.55 (10) |
H4A—C4—H4C | 109.5 | C18—C17—Si2 | 113.86 (10) |
H4B—C4—H4C | 109.5 | C19—C17—Si2 | 113.36 (10) |
C6—C5—C8 | 105.94 (13) | C17—C18—H18A | 109.5 |
C6—C5—C7 | 105.10 (13) | C17—C18—H18B | 109.5 |
C8—C5—C7 | 106.09 (12) | H18A—C18—H18B | 109.5 |
C6—C5—Si1 | 114.00 (10) | C17—C18—H18C | 109.5 |
C8—C5—Si1 | 111.63 (10) | H18A—C18—H18C | 109.5 |
C7—C5—Si1 | 113.41 (10) | H18B—C18—H18C | 109.5 |
C5—C6—H6A | 109.5 | C17—C19—H19A | 109.5 |
C5—C6—H6B | 109.5 | C17—C19—H19B | 109.5 |
H6A—C6—H6B | 109.5 | H19A—C19—H19B | 109.5 |
C5—C6—H6C | 109.5 | C17—C19—H19C | 109.5 |
H6A—C6—H6C | 109.5 | H19A—C19—H19C | 109.5 |
H6B—C6—H6C | 109.5 | H19B—C19—H19C | 109.5 |
C5—C7—H7A | 109.5 | C17—C20—H20A | 109.5 |
C5—C7—H7B | 109.5 | C17—C20—H20B | 109.5 |
H7A—C7—H7B | 109.5 | H20A—C20—H20B | 109.5 |
C5—C7—H7C | 109.5 | C17—C20—H20C | 109.5 |
H7A—C7—H7C | 109.5 | H20A—C20—H20C | 109.5 |
H7B—C7—H7C | 109.5 | H20B—C20—H20C | 109.5 |
C5—C8—H8A | 109.5 | C22—C21—C23 | 105.54 (13) |
C5—C8—H8B | 109.5 | C22—C21—C24 | 105.20 (12) |
H8A—C8—H8B | 109.5 | C23—C21—C24 | 106.23 (12) |
C5—C8—H8C | 109.5 | C22—C21—Si2 | 114.93 (10) |
H8A—C8—H8C | 109.5 | C23—C21—Si2 | 111.43 (9) |
H8B—C8—H8C | 109.5 | C24—C21—Si2 | 112.81 (11) |
C12—C9—C11 | 105.86 (12) | C21—C22—H22A | 109.5 |
C12—C9—C10 | 105.29 (12) | C21—C22—H22B | 109.5 |
C11—C9—C10 | 105.96 (13) | H22A—C22—H22B | 109.5 |
C12—C9—Si1 | 114.09 (10) | C21—C22—H22C | 109.5 |
C11—C9—Si1 | 111.29 (9) | H22A—C22—H22C | 109.5 |
C10—C9—Si1 | 113.66 (10) | H22B—C22—H22C | 109.5 |
C9—C10—H10A | 109.5 | C21—C23—H23A | 109.5 |
C9—C10—H10B | 109.5 | C21—C23—H23B | 109.5 |
H10A—C10—H10B | 109.5 | H23A—C23—H23B | 109.5 |
C9—C10—H10C | 109.5 | C21—C23—H23C | 109.5 |
H10A—C10—H10C | 109.5 | H23A—C23—H23C | 109.5 |
H10B—C10—H10C | 109.5 | H23B—C23—H23C | 109.5 |
C9—C11—H11A | 109.5 | C21—C24—H24A | 109.5 |
C9—C11—H11B | 109.5 | C21—C24—H24B | 109.5 |
H11A—C11—H11B | 109.5 | H24A—C24—H24B | 109.5 |
C9—C11—H11C | 109.5 | C21—C24—H24C | 109.5 |
H11A—C11—H11C | 109.5 | H24A—C24—H24C | 109.5 |
H11B—C11—H11C | 109.5 | H24B—C24—H24C | 109.5 |
| | | |
C1—Si1—Si2—C17 | −74.14 (7) | Si2—Si1—C9—C11 | −75.23 (11) |
C5—Si1—Si2—C17 | 46.25 (7) | C1—Si1—C9—C10 | 42.06 (12) |
C9—Si1—Si2—C17 | 165.61 (6) | C5—Si1—C9—C10 | −72.48 (12) |
C1—Si1—Si2—C21 | 165.69 (7) | Si2—Si1—C9—C10 | 165.23 (10) |
C5—Si1—Si2—C21 | −73.92 (7) | C17—Si2—C13—C15 | 47.20 (12) |
C9—Si1—Si2—C21 | 45.43 (7) | C21—Si2—C13—C15 | 161.76 (10) |
C1—Si1—Si2—C13 | 45.38 (7) | Si1—Si2—C13—C15 | −75.16 (11) |
C5—Si1—Si2—C13 | 165.77 (6) | C17—Si2—C13—C14 | 166.96 (10) |
C9—Si1—Si2—C13 | −74.87 (7) | C21—Si2—C13—C14 | −78.48 (11) |
C5—Si1—C1—C4 | −77.84 (12) | Si1—Si2—C13—C14 | 44.60 (11) |
C9—Si1—C1—C4 | 167.82 (11) | C17—Si2—C13—C16 | −72.53 (12) |
Si2—Si1—C1—C4 | 45.24 (11) | C21—Si2—C13—C16 | 42.04 (13) |
C5—Si1—C1—C3 | 162.08 (10) | Si1—Si2—C13—C16 | 165.12 (10) |
C9—Si1—C1—C3 | 47.74 (12) | C21—Si2—C17—C20 | 47.24 (12) |
Si2—Si1—C1—C3 | −74.84 (11) | C13—Si2—C17—C20 | 161.95 (11) |
C5—Si1—C1—C2 | 42.49 (12) | Si1—Si2—C17—C20 | −75.82 (11) |
C9—Si1—C1—C2 | −71.85 (12) | C21—Si2—C17—C18 | 167.10 (11) |
Si2—Si1—C1—C2 | 165.57 (10) | C13—Si2—C17—C18 | −78.19 (12) |
C1—Si1—C5—C6 | 167.25 (11) | Si1—Si2—C17—C18 | 44.03 (12) |
C9—Si1—C5—C6 | −78.10 (12) | C21—Si2—C17—C19 | −72.68 (12) |
Si2—Si1—C5—C6 | 43.88 (12) | C13—Si2—C17—C19 | 42.03 (12) |
C1—Si1—C5—C8 | 47.25 (12) | Si1—Si2—C17—C19 | 164.26 (9) |
C9—Si1—C5—C8 | 161.90 (11) | C17—Si2—C21—C22 | −77.39 (12) |
Si2—Si1—C5—C8 | −76.11 (11) | C13—Si2—C21—C22 | 168.19 (11) |
C1—Si1—C5—C7 | −72.52 (12) | Si1—Si2—C21—C22 | 45.46 (12) |
C9—Si1—C5—C7 | 42.13 (12) | C17—Si2—C21—C23 | 162.61 (10) |
Si2—Si1—C5—C7 | 164.11 (9) | C13—Si2—C21—C23 | 48.19 (12) |
C1—Si1—C9—C12 | −78.69 (11) | Si1—Si2—C21—C23 | −74.54 (11) |
C5—Si1—C9—C12 | 166.77 (10) | C17—Si2—C21—C24 | 43.22 (12) |
Si2—Si1—C9—C12 | 44.48 (11) | C13—Si2—C21—C24 | −71.21 (12) |
C1—Si1—C9—C11 | 161.60 (10) | Si1—Si2—C21—C24 | 166.06 (10) |
C5—Si1—C9—C11 | 47.06 (12) | | |
(II) 1,1,2,2-Tetra-
tert-butyl-1,2-diphenyldisilane
top
Crystal data top
C28H46Si2 | Z = 4 |
Mr = 438.83 | F(000) = 968 |
Triclinic, P1 | Dx = 1.089 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.0240 (11) Å | Cell parameters from 165 reflections |
b = 17.566 (2) Å | θ = 3–26° |
c = 18.961 (3) Å | µ = 0.15 mm−1 |
α = 116.476 (6)° | T = 157 K |
β = 95.018 (7)° | Block, colorless |
γ = 90.263 (10)° | 0.30 × 0.26 × 0.25 mm |
V = 2676.8 (6) Å3 | |
Data collection top
Siemens SMART 1K CCD diffractometer | 12352 independent reflections |
Radiation source: normal-focus sealed tube | 7513 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
ω scans | θmax = 28.0°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −11→11 |
Tmin = 0.873, Tmax = 0.964 | k = −23→23 |
31180 measured reflections | l = −25→25 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.116 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.051P)2] where P = (Fo2 + 2Fc2)/3 |
12352 reflections | (Δ/σ)max = 0.001 |
565 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.27 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Si1 | 0.40260 (6) | 0.21134 (3) | 0.83084 (3) | 0.02539 (14) | |
Si2 | 0.47108 (6) | 0.21499 (3) | 0.70812 (3) | 0.02498 (14) | |
Si3 | 1.09848 (6) | 0.27363 (3) | 0.32339 (3) | 0.02468 (14) | |
Si4 | 0.98576 (6) | 0.30935 (3) | 0.21761 (3) | 0.02642 (14) | |
C1 | 0.3063 (2) | 0.31601 (12) | 0.88451 (11) | 0.0272 (5) | |
C2 | 0.1696 (2) | 0.32745 (13) | 0.85030 (12) | 0.0317 (5) | |
H2 | 0.1244 | 0.2814 | 0.8035 | 0.038* | |
C3 | 0.0976 (2) | 0.40332 (14) | 0.88205 (13) | 0.0395 (6) | |
H3 | 0.0056 | 0.4088 | 0.8566 | 0.047* | |
C4 | 0.1599 (3) | 0.47119 (14) | 0.95088 (14) | 0.0421 (6) | |
H4 | 0.1127 | 0.5239 | 0.9724 | 0.051* | |
C5 | 0.2910 (3) | 0.46087 (14) | 0.98744 (13) | 0.0409 (6) | |
H5 | 0.3332 | 0.5064 | 1.0355 | 0.049* | |
C6 | 0.3627 (2) | 0.38501 (13) | 0.95518 (12) | 0.0325 (5) | |
H6 | 0.4531 | 0.3797 | 0.9820 | 0.039* | |
C7 | 0.5738 (2) | 0.20840 (13) | 0.89947 (12) | 0.0328 (5) | |
C8 | 0.5272 (3) | 0.22161 (15) | 0.98063 (12) | 0.0441 (6) | |
H8A | 0.6154 | 0.2209 | 1.0144 | 0.066* | |
H8B | 0.4557 | 0.1757 | 0.9728 | 0.066* | |
H8C | 0.4811 | 0.2765 | 1.0061 | 0.066* | |
C9 | 0.6912 (2) | 0.27865 (14) | 0.91287 (13) | 0.0414 (6) | |
H9A | 0.7700 | 0.2821 | 0.9533 | 0.062* | |
H9B | 0.6439 | 0.3334 | 0.9307 | 0.062* | |
H9C | 0.7342 | 0.2652 | 0.8632 | 0.062* | |
C10 | 0.6553 (3) | 0.12405 (14) | 0.86656 (13) | 0.0427 (6) | |
H10A | 0.7530 | 0.1326 | 0.8967 | 0.064* | |
H10B | 0.6684 | 0.1061 | 0.8107 | 0.064* | |
H10C | 0.5961 | 0.0800 | 0.8714 | 0.064* | |
C11 | 0.2503 (2) | 0.12310 (13) | 0.81337 (12) | 0.0326 (5) | |
C12 | 0.1494 (3) | 0.15552 (15) | 0.88080 (14) | 0.0474 (6) | |
H12A | 0.0823 | 0.1087 | 0.8752 | 0.071* | |
H12B | 0.0907 | 0.2013 | 0.8786 | 0.071* | |
H12C | 0.2108 | 0.1773 | 0.9317 | 0.071* | |
C13 | 0.1507 (3) | 0.09454 (14) | 0.73465 (13) | 0.0428 (6) | |
H13A | 0.0707 | 0.0550 | 0.7316 | 0.064* | |
H13B | 0.2108 | 0.0661 | 0.6902 | 0.064* | |
H13C | 0.1074 | 0.1444 | 0.7321 | 0.064* | |
C14 | 0.3180 (3) | 0.04165 (13) | 0.81117 (14) | 0.0463 (6) | |
H14A | 0.2382 | −0.0016 | 0.7993 | 0.069* | |
H14B | 0.3721 | 0.0549 | 0.8627 | 0.069* | |
H14C | 0.3869 | 0.0199 | 0.7701 | 0.069* | |
C15 | 0.2882 (2) | 0.19813 (12) | 0.64157 (11) | 0.0275 (5) | |
C16 | 0.2425 (2) | 0.12230 (13) | 0.57392 (12) | 0.0336 (5) | |
H16 | 0.3035 | 0.0748 | 0.5601 | 0.040* | |
C17 | 0.1115 (3) | 0.11409 (15) | 0.52636 (13) | 0.0395 (6) | |
H17 | 0.0838 | 0.0614 | 0.4814 | 0.047* | |
C18 | 0.0222 (2) | 0.18165 (15) | 0.54406 (13) | 0.0395 (6) | |
H18 | −0.0667 | 0.1764 | 0.5111 | 0.047* | |
C19 | 0.0620 (2) | 0.25712 (14) | 0.60982 (13) | 0.0363 (5) | |
H19 | 0.0002 | 0.3042 | 0.6224 | 0.044* | |
C20 | 0.1924 (2) | 0.26516 (13) | 0.65815 (12) | 0.0313 (5) | |
H20 | 0.2171 | 0.3177 | 0.7038 | 0.038* | |
C21 | 0.6013 (2) | 0.12466 (13) | 0.64978 (12) | 0.0308 (5) | |
C22 | 0.5377 (3) | 0.03894 (13) | 0.64132 (12) | 0.0371 (5) | |
H22A | 0.5958 | −0.0074 | 0.6064 | 0.056* | |
H22B | 0.4336 | 0.0299 | 0.6186 | 0.056* | |
H22C | 0.5433 | 0.0399 | 0.6935 | 0.056* | |
C23 | 0.7628 (2) | 0.13488 (14) | 0.68858 (13) | 0.0403 (6) | |
H23A | 0.8105 | 0.0803 | 0.6643 | 0.060* | |
H23B | 0.7616 | 0.1529 | 0.7454 | 0.060* | |
H23C | 0.8187 | 0.1779 | 0.6806 | 0.060* | |
C24 | 0.6153 (3) | 0.11856 (14) | 0.56669 (12) | 0.0414 (6) | |
H24A | 0.6778 | 0.0714 | 0.5376 | 0.062* | |
H24B | 0.6608 | 0.1720 | 0.5722 | 0.062* | |
H24C | 0.5162 | 0.1085 | 0.5376 | 0.062* | |
C25 | 0.5534 (2) | 0.32644 (13) | 0.72476 (12) | 0.0305 (5) | |
C26 | 0.4964 (2) | 0.40077 (12) | 0.79587 (12) | 0.0372 (5) | |
H26A | 0.5338 | 0.4547 | 0.7988 | 0.056* | |
H26B | 0.5317 | 0.3971 | 0.8446 | 0.056* | |
H26C | 0.3873 | 0.3981 | 0.7897 | 0.056* | |
C27 | 0.7245 (2) | 0.33340 (15) | 0.73911 (15) | 0.0496 (7) | |
H27A | 0.7600 | 0.3916 | 0.7529 | 0.074* | |
H27B | 0.7663 | 0.2935 | 0.6909 | 0.074* | |
H27C | 0.7561 | 0.3196 | 0.7827 | 0.074* | |
C28 | 0.5140 (3) | 0.34103 (14) | 0.65083 (12) | 0.0420 (6) | |
H28A | 0.5652 | 0.3937 | 0.6581 | 0.063* | |
H28B | 0.4061 | 0.3457 | 0.6435 | 0.063* | |
H28C | 0.5456 | 0.2930 | 0.6040 | 0.063* | |
C29 | 0.9328 (2) | 0.26410 (12) | 0.37612 (11) | 0.0251 (4) | |
C30 | 0.8354 (2) | 0.19223 (13) | 0.33837 (11) | 0.0291 (5) | |
H30 | 0.8535 | 0.1503 | 0.2872 | 0.035* | |
C31 | 0.7137 (2) | 0.17930 (14) | 0.37208 (12) | 0.0332 (5) | |
H31 | 0.6518 | 0.1288 | 0.3446 | 0.040* | |
C32 | 0.6825 (2) | 0.23985 (14) | 0.44557 (12) | 0.0342 (5) | |
H32 | 0.5983 | 0.2319 | 0.4688 | 0.041* | |
C33 | 0.7748 (2) | 0.31192 (14) | 0.48487 (12) | 0.0353 (5) | |
H33 | 0.7536 | 0.3542 | 0.5353 | 0.042* | |
C34 | 0.8987 (2) | 0.32337 (13) | 0.45148 (12) | 0.0310 (5) | |
H34 | 0.9624 | 0.3729 | 0.4805 | 0.037* | |
C35 | 1.2398 (2) | 0.36089 (13) | 0.40154 (12) | 0.0338 (5) | |
C36 | 1.2779 (3) | 0.34527 (14) | 0.47485 (12) | 0.0455 (6) | |
H36A | 1.3436 | 0.3923 | 0.5144 | 0.068* | |
H36B | 1.3283 | 0.2916 | 0.4592 | 0.068* | |
H36C | 1.1860 | 0.3420 | 0.4975 | 0.068* | |
C37 | 1.1728 (2) | 0.44891 (13) | 0.42790 (13) | 0.0391 (6) | |
H37A | 1.2391 | 0.4922 | 0.4711 | 0.059* | |
H37B | 1.0750 | 0.4477 | 0.4462 | 0.059* | |
H37C | 1.1619 | 0.4628 | 0.3831 | 0.059* | |
C38 | 1.3904 (2) | 0.36823 (15) | 0.37169 (14) | 0.0484 (6) | |
H38A | 1.4421 | 0.4228 | 0.4080 | 0.073* | |
H38B | 1.3730 | 0.3651 | 0.3187 | 0.073* | |
H38C | 1.4519 | 0.3215 | 0.3694 | 0.073* | |
C39 | 1.1830 (2) | 0.16089 (12) | 0.28358 (12) | 0.0299 (5) | |
C40 | 1.1651 (3) | 0.12264 (14) | 0.34199 (13) | 0.0418 (6) | |
H40A | 1.2189 | 0.0700 | 0.3254 | 0.063* | |
H40B | 1.0593 | 0.1101 | 0.3422 | 0.063* | |
H40C | 1.2058 | 0.1636 | 0.3954 | 0.063* | |
C41 | 1.1103 (2) | 0.09643 (12) | 0.20167 (12) | 0.0357 (5) | |
H41A | 1.1469 | 0.0398 | 0.1890 | 0.053* | |
H41B | 1.1359 | 0.1137 | 0.1615 | 0.053* | |
H41C | 1.0019 | 0.0948 | 0.2024 | 0.053* | |
C42 | 1.3507 (2) | 0.16282 (15) | 0.27521 (14) | 0.0455 (6) | |
H42A | 1.3830 | 0.1044 | 0.2482 | 0.068* | |
H42B | 1.4057 | 0.1920 | 0.3279 | 0.068* | |
H42C | 1.3703 | 0.1933 | 0.2442 | 0.068* | |
C43 | 0.8722 (2) | 0.20731 (12) | 0.14458 (11) | 0.0278 (5) | |
C44 | 0.9149 (3) | 0.14953 (13) | 0.07113 (12) | 0.0352 (5) | |
H44 | 1.0032 | 0.1622 | 0.0538 | 0.042* | |
C45 | 0.8329 (3) | 0.07415 (14) | 0.02248 (12) | 0.0400 (6) | |
H45 | 0.8672 | 0.0360 | −0.0264 | 0.048* | |
C46 | 0.7024 (3) | 0.05449 (14) | 0.04462 (14) | 0.0436 (6) | |
H46 | 0.6466 | 0.0029 | 0.0116 | 0.052* | |
C47 | 0.6542 (3) | 0.11096 (14) | 0.11563 (13) | 0.0394 (6) | |
H47 | 0.5632 | 0.0988 | 0.1311 | 0.047* | |
C48 | 0.7374 (2) | 0.18521 (13) | 0.16448 (12) | 0.0317 (5) | |
H48 | 0.7021 | 0.2227 | 0.2133 | 0.038* | |
C49 | 1.1329 (3) | 0.33361 (14) | 0.16055 (13) | 0.0394 (6) | |
C50 | 1.2526 (3) | 0.26657 (15) | 0.13856 (14) | 0.0467 (6) | |
H50A | 1.3185 | 0.2754 | 0.1042 | 0.070* | |
H50B | 1.2042 | 0.2094 | 0.1107 | 0.070* | |
H50C | 1.3110 | 0.2723 | 0.1869 | 0.070* | |
C51 | 1.2196 (3) | 0.42041 (15) | 0.20862 (15) | 0.0602 (8) | |
H51A | 1.3059 | 0.4228 | 0.1816 | 0.090* | |
H51B | 1.2534 | 0.4270 | 0.2617 | 0.090* | |
H51C | 1.1543 | 0.4664 | 0.2130 | 0.090* | |
C52 | 1.0594 (3) | 0.33549 (16) | 0.08456 (14) | 0.0545 (7) | |
H52A | 1.1366 | 0.3444 | 0.0554 | 0.082* | |
H52B | 0.9909 | 0.3820 | 0.0990 | 0.082* | |
H52C | 1.0042 | 0.2812 | 0.0512 | 0.082* | |
C53 | 0.8392 (2) | 0.39848 (13) | 0.25250 (12) | 0.0332 (5) | |
C54 | 0.7624 (2) | 0.40245 (14) | 0.32286 (13) | 0.0398 (6) | |
H54A | 0.6838 | 0.4434 | 0.3345 | 0.060* | |
H54B | 0.8357 | 0.4205 | 0.3693 | 0.060* | |
H54C | 0.7187 | 0.3460 | 0.3098 | 0.060* | |
C55 | 0.9048 (3) | 0.48959 (13) | 0.27858 (14) | 0.0490 (6) | |
H55A | 0.8292 | 0.5308 | 0.3025 | 0.074* | |
H55B | 0.9351 | 0.4945 | 0.2324 | 0.074* | |
H55C | 0.9915 | 0.5012 | 0.3174 | 0.074* | |
C56 | 0.7172 (3) | 0.38147 (14) | 0.18397 (13) | 0.0447 (6) | |
H56A | 0.6510 | 0.4292 | 0.1999 | 0.067* | |
H56B | 0.6595 | 0.3289 | 0.1714 | 0.067* | |
H56C | 0.7639 | 0.3756 | 0.1372 | 0.067* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0280 (3) | 0.0240 (3) | 0.0237 (3) | 0.0013 (2) | 0.0014 (2) | 0.0105 (2) |
Si2 | 0.0252 (3) | 0.0255 (3) | 0.0241 (3) | 0.0043 (2) | 0.0014 (2) | 0.0112 (3) |
Si3 | 0.0225 (3) | 0.0245 (3) | 0.0239 (3) | 0.0045 (2) | 0.0048 (2) | 0.0076 (2) |
Si4 | 0.0292 (3) | 0.0248 (3) | 0.0268 (3) | 0.0037 (2) | 0.0072 (3) | 0.0122 (3) |
C1 | 0.0271 (12) | 0.0286 (11) | 0.0265 (11) | −0.0005 (9) | 0.0048 (9) | 0.0127 (9) |
C2 | 0.0316 (13) | 0.0310 (12) | 0.0288 (11) | 0.0016 (10) | 0.0055 (10) | 0.0097 (10) |
C3 | 0.0312 (13) | 0.0414 (14) | 0.0460 (14) | 0.0073 (11) | 0.0074 (11) | 0.0191 (12) |
C4 | 0.0438 (15) | 0.0304 (13) | 0.0509 (15) | 0.0107 (11) | 0.0183 (12) | 0.0145 (12) |
C5 | 0.0460 (15) | 0.0321 (13) | 0.0354 (13) | −0.0003 (11) | 0.0069 (11) | 0.0065 (11) |
C6 | 0.0344 (13) | 0.0303 (12) | 0.0301 (12) | 0.0005 (10) | 0.0016 (10) | 0.0114 (10) |
C7 | 0.0352 (13) | 0.0335 (12) | 0.0276 (11) | 0.0066 (10) | 0.0015 (10) | 0.0122 (10) |
C8 | 0.0527 (16) | 0.0494 (15) | 0.0318 (13) | 0.0075 (12) | −0.0009 (11) | 0.0205 (12) |
C9 | 0.0343 (14) | 0.0474 (15) | 0.0381 (13) | 0.0023 (11) | −0.0061 (11) | 0.0169 (12) |
C10 | 0.0480 (15) | 0.0452 (14) | 0.0372 (13) | 0.0116 (12) | −0.0011 (11) | 0.0215 (12) |
C11 | 0.0352 (13) | 0.0291 (12) | 0.0356 (12) | −0.0034 (10) | 0.0040 (10) | 0.0165 (10) |
C12 | 0.0492 (16) | 0.0443 (15) | 0.0547 (16) | −0.0050 (12) | 0.0159 (13) | 0.0255 (13) |
C13 | 0.0383 (14) | 0.0371 (13) | 0.0485 (15) | −0.0138 (11) | −0.0044 (11) | 0.0170 (12) |
C14 | 0.0583 (17) | 0.0299 (13) | 0.0550 (15) | −0.0034 (11) | 0.0048 (13) | 0.0231 (12) |
C15 | 0.0289 (12) | 0.0303 (12) | 0.0251 (11) | 0.0034 (9) | 0.0011 (9) | 0.0142 (10) |
C16 | 0.0376 (13) | 0.0296 (12) | 0.0306 (12) | 0.0066 (10) | −0.0029 (10) | 0.0120 (10) |
C17 | 0.0403 (14) | 0.0409 (14) | 0.0318 (12) | −0.0020 (11) | −0.0071 (11) | 0.0134 (11) |
C18 | 0.0273 (13) | 0.0563 (16) | 0.0382 (13) | −0.0009 (11) | −0.0057 (10) | 0.0256 (12) |
C19 | 0.0285 (13) | 0.0446 (14) | 0.0430 (14) | 0.0130 (11) | 0.0067 (11) | 0.0253 (12) |
C20 | 0.0313 (13) | 0.0333 (12) | 0.0293 (11) | 0.0051 (10) | 0.0040 (10) | 0.0138 (10) |
C21 | 0.0307 (12) | 0.0309 (12) | 0.0279 (11) | 0.0085 (10) | 0.0027 (9) | 0.0105 (10) |
C22 | 0.0429 (14) | 0.0317 (12) | 0.0343 (12) | 0.0122 (10) | 0.0030 (10) | 0.0127 (10) |
C23 | 0.0317 (13) | 0.0442 (14) | 0.0427 (14) | 0.0126 (11) | 0.0060 (11) | 0.0170 (12) |
C24 | 0.0436 (15) | 0.0431 (14) | 0.0345 (13) | 0.0138 (11) | 0.0111 (11) | 0.0134 (11) |
C25 | 0.0298 (12) | 0.0287 (12) | 0.0354 (12) | −0.0001 (9) | 0.0047 (10) | 0.0163 (10) |
C26 | 0.0423 (14) | 0.0275 (12) | 0.0389 (13) | −0.0058 (10) | 0.0036 (11) | 0.0124 (10) |
C27 | 0.0372 (15) | 0.0415 (14) | 0.0751 (18) | −0.0055 (11) | 0.0040 (13) | 0.0307 (14) |
C28 | 0.0497 (16) | 0.0397 (14) | 0.0447 (14) | 0.0056 (11) | 0.0157 (12) | 0.0241 (12) |
C29 | 0.0245 (11) | 0.0278 (11) | 0.0265 (11) | 0.0092 (9) | 0.0048 (9) | 0.0148 (9) |
C30 | 0.0297 (12) | 0.0332 (12) | 0.0245 (11) | 0.0081 (10) | 0.0037 (9) | 0.0127 (10) |
C31 | 0.0260 (12) | 0.0398 (13) | 0.0369 (13) | 0.0001 (10) | 0.0012 (10) | 0.0203 (11) |
C32 | 0.0260 (12) | 0.0497 (14) | 0.0366 (13) | 0.0081 (11) | 0.0087 (10) | 0.0269 (12) |
C33 | 0.0387 (14) | 0.0400 (13) | 0.0305 (12) | 0.0146 (11) | 0.0129 (10) | 0.0171 (11) |
C34 | 0.0323 (13) | 0.0298 (12) | 0.0300 (12) | 0.0058 (10) | 0.0073 (10) | 0.0119 (10) |
C35 | 0.0290 (12) | 0.0318 (12) | 0.0322 (12) | −0.0011 (10) | 0.0030 (10) | 0.0067 (10) |
C36 | 0.0416 (15) | 0.0456 (15) | 0.0350 (13) | 0.0008 (12) | −0.0093 (11) | 0.0076 (11) |
C37 | 0.0381 (14) | 0.0284 (12) | 0.0395 (13) | −0.0039 (10) | 0.0045 (11) | 0.0050 (10) |
C38 | 0.0318 (14) | 0.0479 (15) | 0.0495 (15) | −0.0061 (11) | 0.0050 (12) | 0.0073 (12) |
C39 | 0.0270 (12) | 0.0291 (12) | 0.0301 (12) | 0.0086 (9) | 0.0030 (9) | 0.0099 (10) |
C40 | 0.0479 (15) | 0.0381 (13) | 0.0408 (14) | 0.0160 (11) | 0.0002 (11) | 0.0194 (11) |
C41 | 0.0422 (14) | 0.0245 (11) | 0.0360 (12) | 0.0098 (10) | 0.0066 (11) | 0.0092 (10) |
C42 | 0.0309 (14) | 0.0443 (15) | 0.0517 (15) | 0.0148 (11) | 0.0077 (11) | 0.0123 (12) |
C43 | 0.0325 (12) | 0.0282 (11) | 0.0253 (11) | 0.0058 (9) | 0.0002 (9) | 0.0148 (9) |
C44 | 0.0393 (14) | 0.0357 (13) | 0.0310 (12) | 0.0064 (10) | 0.0031 (10) | 0.0153 (10) |
C45 | 0.0518 (16) | 0.0351 (13) | 0.0263 (12) | 0.0101 (11) | −0.0015 (11) | 0.0087 (10) |
C46 | 0.0519 (16) | 0.0323 (13) | 0.0431 (14) | −0.0039 (12) | −0.0105 (12) | 0.0167 (12) |
C47 | 0.0399 (14) | 0.0383 (13) | 0.0453 (14) | −0.0054 (11) | −0.0024 (11) | 0.0247 (12) |
C48 | 0.0363 (13) | 0.0314 (12) | 0.0315 (12) | 0.0050 (10) | 0.0023 (10) | 0.0180 (10) |
C49 | 0.0431 (15) | 0.0394 (13) | 0.0423 (14) | −0.0002 (11) | 0.0136 (11) | 0.0225 (11) |
C50 | 0.0392 (15) | 0.0562 (16) | 0.0448 (14) | 0.0000 (12) | 0.0177 (12) | 0.0203 (13) |
C51 | 0.0635 (19) | 0.0490 (16) | 0.0722 (19) | −0.0130 (14) | 0.0216 (15) | 0.0285 (15) |
C52 | 0.0659 (19) | 0.0632 (17) | 0.0527 (16) | 0.0070 (14) | 0.0207 (14) | 0.0396 (14) |
C53 | 0.0366 (13) | 0.0282 (12) | 0.0355 (12) | 0.0100 (10) | 0.0047 (10) | 0.0147 (10) |
C54 | 0.0412 (14) | 0.0367 (13) | 0.0419 (14) | 0.0189 (11) | 0.0129 (11) | 0.0162 (11) |
C55 | 0.0593 (17) | 0.0307 (13) | 0.0570 (16) | 0.0059 (12) | 0.0065 (13) | 0.0196 (12) |
C56 | 0.0491 (16) | 0.0412 (14) | 0.0491 (15) | 0.0155 (12) | 0.0030 (12) | 0.0252 (12) |
Geometric parameters (Å, º) top
Si1—C1 | 1.916 (2) | C26—H26C | 0.9800 |
Si1—C7 | 1.947 (2) | C27—H27A | 0.9800 |
Si1—C11 | 1.961 (2) | C27—H27B | 0.9800 |
Si1—Si2 | 2.4869 (8) | C27—H27C | 0.9800 |
Si2—C15 | 1.924 (2) | C28—H28A | 0.9800 |
Si2—C21 | 1.950 (2) | C28—H28B | 0.9800 |
Si2—C25 | 1.969 (2) | C28—H28C | 0.9800 |
Si3—C29 | 1.916 (2) | C29—C30 | 1.398 (3) |
Si3—C35 | 1.949 (2) | C29—C34 | 1.405 (3) |
Si3—C39 | 1.963 (2) | C30—C31 | 1.384 (3) |
Si3—Si4 | 2.4944 (8) | C30—H30 | 0.9500 |
Si4—C43 | 1.924 (2) | C31—C32 | 1.379 (3) |
Si4—C49 | 1.942 (2) | C31—H31 | 0.9500 |
Si4—C53 | 1.971 (2) | C32—C33 | 1.376 (3) |
C1—C6 | 1.397 (3) | C32—H32 | 0.9500 |
C1—C2 | 1.400 (3) | C33—C34 | 1.388 (3) |
C2—C3 | 1.386 (3) | C33—H33 | 0.9500 |
C2—H2 | 0.9500 | C34—H34 | 0.9500 |
C3—C4 | 1.385 (3) | C35—C37 | 1.542 (3) |
C3—H3 | 0.9500 | C35—C38 | 1.543 (3) |
C4—C5 | 1.372 (3) | C35—C36 | 1.544 (3) |
C4—H4 | 0.9500 | C36—H36A | 0.9800 |
C5—C6 | 1.385 (3) | C36—H36B | 0.9800 |
C5—H5 | 0.9500 | C36—H36C | 0.9800 |
C6—H6 | 0.9500 | C37—H37A | 0.9800 |
C7—C9 | 1.539 (3) | C37—H37B | 0.9800 |
C7—C10 | 1.546 (3) | C37—H37C | 0.9800 |
C7—C8 | 1.548 (3) | C38—H38A | 0.9800 |
C8—H8A | 0.9800 | C38—H38B | 0.9800 |
C8—H8B | 0.9800 | C38—H38C | 0.9800 |
C8—H8C | 0.9800 | C39—C42 | 1.538 (3) |
C9—H9A | 0.9800 | C39—C41 | 1.540 (3) |
C9—H9B | 0.9800 | C39—C40 | 1.549 (3) |
C9—H9C | 0.9800 | C40—H40A | 0.9800 |
C10—H10A | 0.9800 | C40—H40B | 0.9800 |
C10—H10B | 0.9800 | C40—H40C | 0.9800 |
C10—H10C | 0.9800 | C41—H41A | 0.9800 |
C11—C12 | 1.532 (3) | C41—H41B | 0.9800 |
C11—C13 | 1.543 (3) | C41—H41C | 0.9800 |
C11—C14 | 1.543 (3) | C42—H42A | 0.9800 |
C12—H12A | 0.9800 | C42—H42B | 0.9800 |
C12—H12B | 0.9800 | C42—H42C | 0.9800 |
C12—H12C | 0.9800 | C43—C44 | 1.398 (3) |
C13—H13A | 0.9800 | C43—C48 | 1.407 (3) |
C13—H13B | 0.9800 | C44—C45 | 1.391 (3) |
C13—H13C | 0.9800 | C44—H44 | 0.9500 |
C14—H14A | 0.9800 | C45—C46 | 1.376 (3) |
C14—H14B | 0.9800 | C45—H45 | 0.9500 |
C14—H14C | 0.9800 | C46—C47 | 1.379 (3) |
C15—C20 | 1.400 (3) | C46—H46 | 0.9500 |
C15—C16 | 1.403 (3) | C47—C48 | 1.384 (3) |
C16—C17 | 1.388 (3) | C47—H47 | 0.9500 |
C16—H16 | 0.9500 | C48—H48 | 0.9500 |
C17—C18 | 1.368 (3) | C49—C50 | 1.542 (3) |
C17—H17 | 0.9500 | C49—C51 | 1.547 (3) |
C18—C19 | 1.373 (3) | C49—C52 | 1.547 (3) |
C18—H18 | 0.9500 | C50—H50A | 0.9800 |
C19—C20 | 1.392 (3) | C50—H50B | 0.9800 |
C19—H19 | 0.9500 | C50—H50C | 0.9800 |
C20—H20 | 0.9500 | C51—H51A | 0.9800 |
C21—C22 | 1.544 (3) | C51—H51B | 0.9800 |
C21—C23 | 1.546 (3) | C51—H51C | 0.9800 |
C21—C24 | 1.547 (3) | C52—H52A | 0.9800 |
C22—H22A | 0.9800 | C52—H52B | 0.9800 |
C22—H22B | 0.9800 | C52—H52C | 0.9800 |
C22—H22C | 0.9800 | C53—C54 | 1.531 (3) |
C23—H23A | 0.9800 | C53—C56 | 1.546 (3) |
C23—H23B | 0.9800 | C53—C55 | 1.546 (3) |
C23—H23C | 0.9800 | C54—H54A | 0.9800 |
C24—H24A | 0.9800 | C54—H54B | 0.9800 |
C24—H24B | 0.9800 | C54—H54C | 0.9800 |
C24—H24C | 0.9800 | C55—H55A | 0.9800 |
C25—C26 | 1.531 (3) | C55—H55B | 0.9800 |
C25—C27 | 1.539 (3) | C55—H55C | 0.9800 |
C25—C28 | 1.546 (3) | C56—H56A | 0.9800 |
C26—H26A | 0.9800 | C56—H56B | 0.9800 |
C26—H26B | 0.9800 | C56—H56C | 0.9800 |
| | | |
C1—Si1—C7 | 108.90 (9) | C25—C27—H27A | 109.5 |
C1—Si1—C11 | 104.10 (9) | C25—C27—H27B | 109.5 |
C7—Si1—C11 | 111.05 (9) | H27A—C27—H27B | 109.5 |
C1—Si1—Si2 | 103.91 (6) | C25—C27—H27C | 109.5 |
C7—Si1—Si2 | 113.40 (7) | H27A—C27—H27C | 109.5 |
C11—Si1—Si2 | 114.65 (7) | H27B—C27—H27C | 109.5 |
C15—Si2—C21 | 107.90 (9) | C25—C28—H28A | 109.5 |
C15—Si2—C25 | 104.01 (9) | C25—C28—H28B | 109.5 |
C21—Si2—C25 | 110.74 (9) | H28A—C28—H28B | 109.5 |
C15—Si2—Si1 | 106.51 (6) | C25—C28—H28C | 109.5 |
C21—Si2—Si1 | 112.90 (7) | H28A—C28—H28C | 109.5 |
C25—Si2—Si1 | 114.11 (6) | H28B—C28—H28C | 109.5 |
C29—Si3—C35 | 108.11 (9) | C30—C29—C34 | 115.21 (18) |
C29—Si3—C39 | 104.08 (9) | C30—C29—Si3 | 118.89 (14) |
C35—Si3—C39 | 110.91 (9) | C34—C29—Si3 | 125.90 (15) |
C29—Si3—Si4 | 104.41 (6) | C31—C30—C29 | 123.06 (19) |
C35—Si3—Si4 | 114.20 (7) | C31—C30—H30 | 118.5 |
C39—Si3—Si4 | 114.21 (6) | C29—C30—H30 | 118.5 |
C43—Si4—C49 | 107.94 (9) | C32—C31—C30 | 119.9 (2) |
C43—Si4—C53 | 104.91 (9) | C32—C31—H31 | 120.1 |
C49—Si4—C53 | 111.19 (9) | C30—C31—H31 | 120.1 |
C43—Si4—Si3 | 104.13 (6) | C33—C32—C31 | 119.16 (19) |
C49—Si4—Si3 | 113.16 (8) | C33—C32—H32 | 120.4 |
C53—Si4—Si3 | 114.68 (7) | C31—C32—H32 | 120.4 |
C6—C1—C2 | 115.55 (19) | C32—C33—C34 | 120.6 (2) |
C6—C1—Si1 | 125.60 (16) | C32—C33—H33 | 119.7 |
C2—C1—Si1 | 118.82 (15) | C34—C33—H33 | 119.7 |
C3—C2—C1 | 122.6 (2) | C33—C34—C29 | 122.1 (2) |
C3—C2—H2 | 118.7 | C33—C34—H34 | 119.0 |
C1—C2—H2 | 118.7 | C29—C34—H34 | 119.0 |
C4—C3—C2 | 119.9 (2) | C37—C35—C38 | 105.66 (17) |
C4—C3—H3 | 120.0 | C37—C35—C36 | 109.10 (17) |
C2—C3—H3 | 120.0 | C38—C35—C36 | 105.85 (19) |
C5—C4—C3 | 118.8 (2) | C37—C35—Si3 | 109.32 (14) |
C5—C4—H4 | 120.6 | C38—C35—Si3 | 114.99 (14) |
C3—C4—H4 | 120.6 | C36—C35—Si3 | 111.62 (14) |
C4—C5—C6 | 120.9 (2) | C35—C36—H36A | 109.5 |
C4—C5—H5 | 119.5 | C35—C36—H36B | 109.5 |
C6—C5—H5 | 119.5 | H36A—C36—H36B | 109.5 |
C5—C6—C1 | 122.1 (2) | C35—C36—H36C | 109.5 |
C5—C6—H6 | 119.0 | H36A—C36—H36C | 109.5 |
C1—C6—H6 | 119.0 | H36B—C36—H36C | 109.5 |
C9—C7—C10 | 105.93 (18) | C35—C37—H37A | 109.5 |
C9—C7—C8 | 108.92 (17) | C35—C37—H37B | 109.5 |
C10—C7—C8 | 105.95 (17) | H37A—C37—H37B | 109.5 |
C9—C7—Si1 | 110.09 (14) | C35—C37—H37C | 109.5 |
C10—C7—Si1 | 114.67 (14) | H37A—C37—H37C | 109.5 |
C8—C7—Si1 | 110.99 (15) | H37B—C37—H37C | 109.5 |
C7—C8—H8A | 109.5 | C35—C38—H38A | 109.5 |
C7—C8—H8B | 109.5 | C35—C38—H38B | 109.5 |
H8A—C8—H8B | 109.5 | H38A—C38—H38B | 109.5 |
C7—C8—H8C | 109.5 | C35—C38—H38C | 109.5 |
H8A—C8—H8C | 109.5 | H38A—C38—H38C | 109.5 |
H8B—C8—H8C | 109.5 | H38B—C38—H38C | 109.5 |
C7—C9—H9A | 109.5 | C42—C39—C41 | 105.59 (17) |
C7—C9—H9B | 109.5 | C42—C39—C40 | 105.87 (17) |
H9A—C9—H9B | 109.5 | C41—C39—C40 | 107.60 (17) |
C7—C9—H9C | 109.5 | C42—C39—Si3 | 113.47 (14) |
H9A—C9—H9C | 109.5 | C41—C39—Si3 | 113.83 (14) |
H9B—C9—H9C | 109.5 | C40—C39—Si3 | 110.00 (14) |
C7—C10—H10A | 109.5 | C39—C40—H40A | 109.5 |
C7—C10—H10B | 109.5 | C39—C40—H40B | 109.5 |
H10A—C10—H10B | 109.5 | H40A—C40—H40B | 109.5 |
C7—C10—H10C | 109.5 | C39—C40—H40C | 109.5 |
H10A—C10—H10C | 109.5 | H40A—C40—H40C | 109.5 |
H10B—C10—H10C | 109.5 | H40B—C40—H40C | 109.5 |
C12—C11—C13 | 107.98 (19) | C39—C41—H41A | 109.5 |
C12—C11—C14 | 106.66 (17) | C39—C41—H41B | 109.5 |
C13—C11—C14 | 106.06 (17) | H41A—C41—H41B | 109.5 |
C12—C11—Si1 | 110.19 (14) | C39—C41—H41C | 109.5 |
C13—C11—Si1 | 113.09 (14) | H41A—C41—H41C | 109.5 |
C14—C11—Si1 | 112.52 (15) | H41B—C41—H41C | 109.5 |
C11—C12—H12A | 109.5 | C39—C42—H42A | 109.5 |
C11—C12—H12B | 109.5 | C39—C42—H42B | 109.5 |
H12A—C12—H12B | 109.5 | H42A—C42—H42B | 109.5 |
C11—C12—H12C | 109.5 | C39—C42—H42C | 109.5 |
H12A—C12—H12C | 109.5 | H42A—C42—H42C | 109.5 |
H12B—C12—H12C | 109.5 | H42B—C42—H42C | 109.5 |
C11—C13—H13A | 109.5 | C44—C43—C48 | 115.17 (19) |
C11—C13—H13B | 109.5 | C44—C43—Si4 | 124.74 (16) |
H13A—C13—H13B | 109.5 | C48—C43—Si4 | 120.07 (15) |
C11—C13—H13C | 109.5 | C45—C44—C43 | 122.4 (2) |
H13A—C13—H13C | 109.5 | C45—C44—H44 | 118.8 |
H13B—C13—H13C | 109.5 | C43—C44—H44 | 118.8 |
C11—C14—H14A | 109.5 | C46—C45—C44 | 120.5 (2) |
C11—C14—H14B | 109.5 | C46—C45—H45 | 119.8 |
H14A—C14—H14B | 109.5 | C44—C45—H45 | 119.8 |
C11—C14—H14C | 109.5 | C45—C46—C47 | 118.9 (2) |
H14A—C14—H14C | 109.5 | C45—C46—H46 | 120.6 |
H14B—C14—H14C | 109.5 | C47—C46—H46 | 120.6 |
C20—C15—C16 | 115.44 (19) | C46—C47—C48 | 120.5 (2) |
C20—C15—Si2 | 119.92 (15) | C46—C47—H47 | 119.8 |
C16—C15—Si2 | 124.62 (15) | C48—C47—H47 | 119.8 |
C17—C16—C15 | 122.5 (2) | C47—C48—C43 | 122.5 (2) |
C17—C16—H16 | 118.8 | C47—C48—H48 | 118.7 |
C15—C16—H16 | 118.8 | C43—C48—H48 | 118.7 |
C18—C17—C16 | 120.2 (2) | C50—C49—C51 | 105.3 (2) |
C18—C17—H17 | 119.9 | C50—C49—C52 | 109.51 (19) |
C16—C17—H17 | 119.9 | C51—C49—C52 | 106.00 (19) |
C17—C18—C19 | 119.5 (2) | C50—C49—Si4 | 110.51 (14) |
C17—C18—H18 | 120.3 | C51—C49—Si4 | 114.00 (15) |
C19—C18—H18 | 120.3 | C52—C49—Si4 | 111.22 (16) |
C18—C19—C20 | 120.4 (2) | C49—C50—H50A | 109.5 |
C18—C19—H19 | 119.8 | C49—C50—H50B | 109.5 |
C20—C19—H19 | 119.8 | H50A—C50—H50B | 109.5 |
C19—C20—C15 | 122.0 (2) | C49—C50—H50C | 109.5 |
C19—C20—H20 | 119.0 | H50A—C50—H50C | 109.5 |
C15—C20—H20 | 119.0 | H50B—C50—H50C | 109.5 |
C22—C21—C23 | 105.81 (17) | C49—C51—H51A | 109.5 |
C22—C21—C24 | 109.58 (17) | C49—C51—H51B | 109.5 |
C23—C21—C24 | 105.50 (17) | H51A—C51—H51B | 109.5 |
C22—C21—Si2 | 109.43 (14) | C49—C51—H51C | 109.5 |
C23—C21—Si2 | 115.51 (14) | H51A—C51—H51C | 109.5 |
C24—C21—Si2 | 110.77 (14) | H51B—C51—H51C | 109.5 |
C21—C22—H22A | 109.5 | C49—C52—H52A | 109.5 |
C21—C22—H22B | 109.5 | C49—C52—H52B | 109.5 |
H22A—C22—H22B | 109.5 | H52A—C52—H52B | 109.5 |
C21—C22—H22C | 109.5 | C49—C52—H52C | 109.5 |
H22A—C22—H22C | 109.5 | H52A—C52—H52C | 109.5 |
H22B—C22—H22C | 109.5 | H52B—C52—H52C | 109.5 |
C21—C23—H23A | 109.5 | C54—C53—C56 | 107.82 (18) |
C21—C23—H23B | 109.5 | C54—C53—C55 | 105.69 (17) |
H23A—C23—H23B | 109.5 | C56—C53—C55 | 105.91 (17) |
C21—C23—H23C | 109.5 | C54—C53—Si4 | 112.52 (13) |
H23A—C23—H23C | 109.5 | C56—C53—Si4 | 110.01 (14) |
H23B—C23—H23C | 109.5 | C55—C53—Si4 | 114.46 (16) |
C21—C24—H24A | 109.5 | C53—C54—H54A | 109.5 |
C21—C24—H24B | 109.5 | C53—C54—H54B | 109.5 |
H24A—C24—H24B | 109.5 | H54A—C54—H54B | 109.5 |
C21—C24—H24C | 109.5 | C53—C54—H54C | 109.5 |
H24A—C24—H24C | 109.5 | H54A—C54—H54C | 109.5 |
H24B—C24—H24C | 109.5 | H54B—C54—H54C | 109.5 |
C26—C25—C27 | 106.72 (18) | C53—C55—H55A | 109.5 |
C26—C25—C28 | 107.93 (17) | C53—C55—H55B | 109.5 |
C27—C25—C28 | 106.05 (17) | H55A—C55—H55B | 109.5 |
C26—C25—Si2 | 112.75 (13) | C53—C55—H55C | 109.5 |
C27—C25—Si2 | 112.15 (14) | H55A—C55—H55C | 109.5 |
C28—C25—Si2 | 110.89 (14) | H55B—C55—H55C | 109.5 |
C25—C26—H26A | 109.5 | C53—C56—H56A | 109.5 |
C25—C26—H26B | 109.5 | C53—C56—H56B | 109.5 |
H26A—C26—H26B | 109.5 | H56A—C56—H56B | 109.5 |
C25—C26—H26C | 109.5 | C53—C56—H56C | 109.5 |
H26A—C26—H26C | 109.5 | H56A—C56—H56C | 109.5 |
H26B—C26—H26C | 109.5 | H56B—C56—H56C | 109.5 |
| | | |
C1—Si1—Si2—C15 | −71.47 (9) | C15—Si2—C25—C26 | 87.92 (16) |
C7—Si1—Si2—C15 | 170.44 (9) | C21—Si2—C25—C26 | −156.42 (14) |
C11—Si1—Si2—C15 | 41.46 (10) | Si1—Si2—C25—C26 | −27.71 (17) |
C1—Si1—Si2—C21 | 170.29 (9) | C15—Si2—C25—C27 | −151.59 (15) |
C7—Si1—Si2—C21 | 52.20 (10) | C21—Si2—C25—C27 | −35.92 (18) |
C11—Si1—Si2—C21 | −76.78 (10) | Si1—Si2—C25—C27 | 92.78 (15) |
C1—Si1—Si2—C25 | 42.68 (10) | C15—Si2—C25—C28 | −33.23 (17) |
C7—Si1—Si2—C25 | −75.40 (10) | C21—Si2—C25—C28 | 82.43 (16) |
C11—Si1—Si2—C25 | 155.62 (10) | Si1—Si2—C25—C28 | −148.86 (13) |
C29—Si3—Si4—C43 | −68.61 (9) | C35—Si3—C29—C30 | −163.88 (15) |
C35—Si3—Si4—C43 | 173.53 (9) | C39—Si3—C29—C30 | −45.90 (17) |
C39—Si3—Si4—C43 | 44.40 (10) | Si4—Si3—C29—C30 | 74.16 (15) |
C29—Si3—Si4—C49 | 174.44 (9) | C35—Si3—C29—C34 | 15.5 (2) |
C35—Si3—Si4—C49 | 56.58 (10) | C39—Si3—C29—C34 | 133.51 (17) |
C39—Si3—Si4—C49 | −72.56 (10) | Si4—Si3—C29—C34 | −106.43 (17) |
C29—Si3—Si4—C53 | 45.46 (10) | C34—C29—C30—C31 | −0.2 (3) |
C35—Si3—Si4—C53 | −72.41 (10) | Si3—C29—C30—C31 | 179.31 (15) |
C39—Si3—Si4—C53 | 158.46 (10) | C29—C30—C31—C32 | 1.4 (3) |
C7—Si1—C1—C6 | 9.90 (19) | C30—C31—C32—C33 | −1.0 (3) |
C11—Si1—C1—C6 | 128.42 (17) | C31—C32—C33—C34 | −0.6 (3) |
Si2—Si1—C1—C6 | −111.24 (16) | C32—C33—C34—C29 | 1.9 (3) |
C7—Si1—C1—C2 | −172.21 (15) | C30—C29—C34—C33 | −1.5 (3) |
C11—Si1—C1—C2 | −53.69 (17) | Si3—C29—C34—C33 | 179.11 (16) |
Si2—Si1—C1—C2 | 66.65 (16) | C29—Si3—C35—C37 | −69.57 (16) |
C6—C1—C2—C3 | 2.9 (3) | C39—Si3—C35—C37 | 176.92 (13) |
Si1—C1—C2—C3 | −175.23 (16) | Si4—Si3—C35—C37 | 46.15 (15) |
C1—C2—C3—C4 | −0.9 (3) | C29—Si3—C35—C38 | 171.80 (16) |
C2—C3—C4—C5 | −1.6 (3) | C39—Si3—C35—C38 | 58.29 (19) |
C3—C4—C5—C6 | 1.9 (3) | Si4—Si3—C35—C38 | −72.47 (17) |
C4—C5—C6—C1 | 0.2 (3) | C29—Si3—C35—C36 | 51.21 (17) |
C2—C1—C6—C5 | −2.5 (3) | C39—Si3—C35—C36 | −62.30 (17) |
Si1—C1—C6—C5 | 175.42 (16) | Si4—Si3—C35—C36 | 166.94 (13) |
C1—Si1—C7—C9 | −65.46 (16) | C29—Si3—C39—C42 | −152.29 (15) |
C11—Si1—C7—C9 | −179.52 (14) | C35—Si3—C39—C42 | −36.26 (18) |
Si2—Si1—C7—C9 | 49.69 (16) | Si4—Si3—C39—C42 | 94.50 (15) |
C1—Si1—C7—C10 | 175.23 (15) | C29—Si3—C39—C41 | 86.91 (16) |
C11—Si1—C7—C10 | 61.17 (17) | C35—Si3—C39—C41 | −157.05 (14) |
Si2—Si1—C7—C10 | −69.62 (16) | Si4—Si3—C39—C41 | −26.29 (16) |
C1—Si1—C7—C8 | 55.22 (16) | C29—Si3—C39—C40 | −33.92 (16) |
C11—Si1—C7—C8 | −58.84 (16) | C35—Si3—C39—C40 | 82.12 (16) |
Si2—Si1—C7—C8 | 170.36 (12) | Si4—Si3—C39—C40 | −147.12 (13) |
C1—Si1—C11—C12 | −31.94 (17) | C49—Si4—C43—C44 | 16.0 (2) |
C7—Si1—C11—C12 | 85.10 (17) | C53—Si4—C43—C44 | 134.60 (17) |
Si2—Si1—C11—C12 | −144.76 (13) | Si3—Si4—C43—C44 | −104.56 (17) |
C1—Si1—C11—C13 | 89.01 (16) | C49—Si4—C43—C48 | −165.72 (16) |
C7—Si1—C11—C13 | −153.95 (15) | C53—Si4—C43—C48 | −47.08 (17) |
Si2—Si1—C11—C13 | −23.81 (18) | Si3—Si4—C43—C48 | 73.76 (16) |
C1—Si1—C11—C14 | −150.83 (15) | C48—C43—C44—C45 | −2.2 (3) |
C7—Si1—C11—C14 | −33.80 (17) | Si4—C43—C44—C45 | 176.21 (16) |
Si2—Si1—C11—C14 | 96.35 (14) | C43—C44—C45—C46 | 1.6 (3) |
C21—Si2—C15—C20 | −161.85 (15) | C44—C45—C46—C47 | 0.3 (3) |
C25—Si2—C15—C20 | −44.20 (17) | C45—C46—C47—C48 | −1.4 (3) |
Si1—Si2—C15—C20 | 76.66 (16) | C46—C47—C48—C43 | 0.7 (3) |
C21—Si2—C15—C16 | 16.21 (19) | C44—C43—C48—C47 | 1.1 (3) |
C25—Si2—C15—C16 | 133.86 (17) | Si4—C43—C48—C47 | −177.41 (16) |
Si1—Si2—C15—C16 | −105.27 (17) | C43—Si4—C49—C50 | −69.22 (18) |
C20—C15—C16—C17 | 0.2 (3) | C53—Si4—C49—C50 | 176.22 (15) |
Si2—C15—C16—C17 | −177.96 (16) | Si3—Si4—C49—C50 | 45.46 (17) |
C15—C16—C17—C18 | 0.8 (3) | C43—Si4—C49—C51 | 172.40 (17) |
C16—C17—C18—C19 | −1.0 (3) | C53—Si4—C49—C51 | 57.8 (2) |
C17—C18—C19—C20 | 0.2 (3) | Si3—Si4—C49—C51 | −72.91 (18) |
C18—C19—C20—C15 | 0.9 (3) | C43—Si4—C49—C52 | 52.63 (18) |
C16—C15—C20—C19 | −1.0 (3) | C53—Si4—C49—C52 | −61.93 (18) |
Si2—C15—C20—C19 | 177.23 (15) | Si3—Si4—C49—C52 | 167.32 (14) |
C15—Si2—C21—C22 | −69.53 (15) | C43—Si4—C53—C54 | 86.34 (16) |
C25—Si2—C21—C22 | 177.25 (13) | C49—Si4—C53—C54 | −157.22 (15) |
Si1—Si2—C21—C22 | 47.90 (15) | Si3—Si4—C53—C54 | −27.26 (17) |
C15—Si2—C21—C23 | 171.23 (14) | C43—Si4—C53—C56 | −33.90 (16) |
C25—Si2—C21—C23 | 58.01 (17) | C49—Si4—C53—C56 | 82.54 (17) |
Si1—Si2—C21—C23 | −71.34 (16) | Si3—Si4—C53—C56 | −147.50 (13) |
C15—Si2—C21—C24 | 51.39 (16) | C43—Si4—C53—C55 | −152.98 (15) |
C25—Si2—C21—C24 | −61.83 (16) | C49—Si4—C53—C55 | −36.55 (19) |
Si1—Si2—C21—C24 | 168.82 (12) | Si3—Si4—C53—C55 | 93.41 (15) |
Cell parameters a, b and c (Å) of (I) at
different temperatures topThe phase transition occurs at 179 (2) K. |
T (K) | a | b | c | Space group |
294 | 11.3431 (16) | 29.416 (4) | 15.938 (3) | Ibca |
200 | 11.3227 (14) | 29.231 (4) | 15.874 (3) | |
170 | 11.3064 (11) | 29.243 (3) | 15.846 (2) | |
147 | 11.2923 (8) | 29.204 (3) | 15.8321 (16) | Pbca |
Selected M—M and M–C distances (Å) in disilanes
(M = Si), digermanes (M = Ge) and distannanes (M = Sn) topCompound | M—M | M—C(t-Bu) | M—C(phenyl) | M—C(methyl) |
(I): (t-Bu)3SiSi(t-Bu)3 | 2.6863 (5) | 1.986 (1)–1.993 (1) | | |
(II): Ph(t-Bu)2SiSiPh(t-Bu)2 | 2.4869 (8)–2.4944 (8) | 1.942 (2)–1.971 (2) | 1.916 (2)–1.924 (2) | |
(a): (t-Bu)3SiSiPh3 | 2.450 (2) | 1.949 (3)–1.957 (3) | 1.899 (3)–1.907 (3) | |
(b): Ph2(t-Bu)SiSi(t-Bu)Ph2 | 2.3859 (15) | 1.913 (3) | 1.886 (3)–1.894 (3) | |
(c): Me2(t-Bu)SiSiPh3 | 2.360 (2) | 1.893 (4) | 1.862 (4)–1.876 (4) | 1.860 (6)–1.868 (5) |
(d): Ph3SiSiMe3 | 2.355 (1) | | 1.886 (1) | 1.862 (2) |
(e): Me3SiSiMe3 | 2.340 (9) | | | 1.877 (3) |
(f): H3SiSiH3 | 2.331 (3) | | | |
(g): (t-Bu)3GeGe(t-Bu)3 | 2.705 (1)–2.714 (1) | 2.047 (8)–2.123 (6) | | |
(h): Ph3GeGeMe3 | 2.418 (1) | | 1.957 (2) | 1.943 (4) |
(i): (t-Bu)3SnSn(t-Bu)3 | 2.894 (1) | 2.22 (2)–2.26 (2) | | |
(j): Ph3SnSnMe3 | 2.7820 (14) | | 2.152 (4) | 2.138 (5) |
Notes: (a) Wiberg et al. (2000);
(b) Monakhov et al. (2010);
(c) Leigh et al. (1997);
(d) Párkányi & Hengge (1982);
(e) Beagley et al. (1971);
(f) Beagley et al. (1972);
(g) Weidenbruch et al. (1988);
(h) Párkányi et al. (1994);
(i) Puff et al. (1989);
(j) Párkányi et al. (1996). |
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