Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805033088/lh6519sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805033088/lh6519Isup2.hkl |
CCDC reference: 289806
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.002 Å
- Disorder in main residue
- R factor = 0.056
- wR factor = 0.166
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.33 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.22 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Si1 PLAT301_ALERT_3_B Main Residue Disorder ......................... 28.00 Perc.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.51 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.22 PLAT371_ALERT_2_C Long C(sp2)-C(sp1) Bond C5 - C9 ... 1.44 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.36 Ratio
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEX-II (Bruker, 2004); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: XCIF (Bruker, 2001).
C26H32N2Si2 | Z = 2 |
Mr = 428.72 | F(000) = 460 |
Triclinic, P1 | Dx = 1.039 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.5351 (3) Å | Cell parameters from 7708 reflections |
b = 11.4008 (3) Å | θ = 2.3–27.2° |
c = 11.8287 (4) Å | µ = 0.14 mm−1 |
α = 80.458 (2)° | T = 193 K |
β = 78.076 (2)° | Prism, colorless |
γ = 89.318 (2)° | 0.48 × 0.34 × 0.18 mm |
V = 1370.47 (7) Å3 |
Bruker Kappa/APEX-II CCD diffractometer | 6809 independent reflections |
Radiation source: fine-focus sealed tube | 5162 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
Profile data from φ and ω scans | θmax = 28.3°, θmin = 1.8° |
Absorption correction: integration (SHELXTL/XPREP; Bruker, 2001) | h = −14→14 |
Tmin = 0.948, Tmax = 0.975 | k = −15→15 |
38376 measured reflections | l = −15→15 |
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)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.166 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0772P)2 + 0.4863P] where P = (Fo2 + 2Fc2)/3 |
6809 reflections | (Δ/σ)max = 0.031 |
460 parameters | Δρmax = 0.55 e Å−3 |
913 restraints | Δρmin = −0.61 e Å−3 |
Experimental. One distinct cell was identified using APEX2 (Bruker, 2004). Ten frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2001) then corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001) before using SAINT/SADABS (Bruker, 2001) to sort, merge, and scale the combined data. No decay correction was applied. |
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. Systematic conditions suggested the ambiguous space group. Structure was phased by direct methods. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F2. A final analysis of variance between observed and calculated structure factors showed little dependence on amplitude or resolution. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
N1 | 0.01955 (9) | 0.89466 (8) | 0.90737 (8) | 0.0507 (2) | |
C1 | 0.04545 (10) | 0.98707 (9) | 0.94551 (9) | 0.0461 (3) | |
C2 | 0.15807 (13) | 1.07129 (11) | 0.89381 (12) | 0.0738 (4) | |
H2A | 0.2019 | 1.0859 | 0.9558 | 0.089* | |
H2B | 0.1270 | 1.1466 | 0.8572 | 0.089* | |
H2C | 0.2191 | 1.0365 | 0.8346 | 0.089* | |
C3 | 0.09603 (10) | 0.86547 (9) | 0.80228 (9) | 0.0443 (2) | |
C4 | 0.17379 (9) | 0.76641 (8) | 0.80748 (9) | 0.0415 (2) | |
H4A | 0.1788 | 0.7206 | 0.8812 | 0.050* | |
C5 | 0.24499 (9) | 0.73405 (8) | 0.70378 (9) | 0.0406 (2) | |
C6 | 0.23529 (10) | 0.79990 (10) | 0.59612 (9) | 0.0477 (3) | |
H6A | 0.2830 | 0.7780 | 0.5257 | 0.057* | |
C7 | 0.15597 (12) | 0.89746 (11) | 0.59178 (10) | 0.0553 (3) | |
H7A | 0.1488 | 0.9421 | 0.5182 | 0.066* | |
C8 | 0.08681 (11) | 0.93032 (10) | 0.69442 (10) | 0.0546 (3) | |
H8A | 0.0329 | 0.9976 | 0.6908 | 0.066* | |
C9 | 0.32899 (10) | 0.63382 (9) | 0.70895 (9) | 0.0465 (3) | |
C10 | 0.39983 (11) | 0.55055 (11) | 0.71202 (11) | 0.0564 (3) | |
Si1 | 0.50989 (3) | 0.42393 (3) | 0.71837 (4) | 0.07298 (12) | |
C11 | 0.66450 (13) | 0.46886 (13) | 0.61633 (14) | 0.0755 (4) | |
H11A | 0.7021 | 0.5375 | 0.6388 | 0.091* | |
H11B | 0.6493 | 0.4904 | 0.5366 | 0.091* | |
H11C | 0.7246 | 0.4026 | 0.6192 | 0.091* | |
C12 | 0.4354 (2) | 0.29712 (15) | 0.6733 (3) | 0.1497 (13) | |
H12A | 0.4198 | 0.3210 | 0.5939 | 0.180* | |
H12B | 0.3528 | 0.2735 | 0.7278 | 0.180* | |
H12C | 0.4941 | 0.2298 | 0.6744 | 0.180* | |
C13 | 0.5360 (2) | 0.3887 (3) | 0.86961 (19) | 0.1760 (10) | |
H13A | 0.5736 | 0.4586 | 0.8900 | 0.211* | |
H13B | 0.5955 | 0.3223 | 0.8755 | 0.211* | |
H13C | 0.4528 | 0.3666 | 0.9237 | 0.211* | |
N2 | 0.06823 (12) | 0.54102 (11) | 0.11004 (11) | 0.0514 (3) | 0.7145 (7) |
C14 | −0.01537 (14) | 0.53784 (12) | 0.04745 (13) | 0.0439 (4) | 0.7145 (7) |
C15 | −0.13882 (16) | 0.60520 (14) | 0.05539 (15) | 0.0555 (4) | 0.7145 (7) |
H15A | −0.2100 | 0.5520 | 0.0524 | 0.067* | 0.7145 (7) |
H15B | −0.1293 | 0.6714 | −0.0104 | 0.067* | 0.7145 (7) |
H15C | −0.1581 | 0.6363 | 0.1294 | 0.067* | 0.7145 (7) |
C16 | 0.04877 (7) | 0.60886 (6) | 0.20147 (6) | 0.0487 (4) | 0.7145 (7) |
C17 | 0.12388 (8) | 0.71130 (7) | 0.18969 (8) | 0.0416 (3) | 0.7145 (7) |
H17A | 0.1820 | 0.7395 | 0.1176 | 0.050* | 0.7145 (7) |
C18 | 0.11402 (11) | 0.77250 (8) | 0.28336 (10) | 0.0393 (3) | 0.7145 (7) |
C19 | 0.02905 (13) | 0.73126 (10) | 0.38879 (8) | 0.0568 (5) | 0.7145 (7) |
H19A | 0.0223 | 0.7731 | 0.4528 | 0.068* | 0.7145 (7) |
C20 | −0.04606 (11) | 0.62882 (10) | 0.40057 (7) | 0.0659 (5) | 0.7145 (7) |
H20A | −0.1041 | 0.6006 | 0.4726 | 0.079* | 0.7145 (7) |
C21 | −0.03620 (8) | 0.56762 (8) | 0.30690 (7) | 0.0624 (5) | 0.7145 (7) |
H21A | −0.0875 | 0.4976 | 0.3149 | 0.075* | 0.7145 (7) |
C22 | 0.19669 (14) | 0.87487 (13) | 0.27352 (13) | 0.0442 (4) | 0.7145 (7) |
C23 | 0.26183 (15) | 0.96201 (14) | 0.26846 (13) | 0.0509 (4) | 0.7145 (7) |
Si2 | 0.35560 (5) | 1.09963 (5) | 0.25912 (5) | 0.06618 (15) | 0.7145 (7) |
C24 | 0.2423 (4) | 1.2259 (3) | 0.2334 (5) | 0.0882 (12) | 0.3102 (1) |
H24A | 0.2736 | 1.2968 | 0.2572 | 0.106* | 0.3102 (1) |
H24B | 0.1551 | 1.2035 | 0.2796 | 0.106* | 0.3102 (1) |
H24C | 0.2394 | 1.2431 | 0.1500 | 0.106* | 0.3102 (1) |
C25 | 0.4941 (4) | 1.1140 (5) | 0.1317 (4) | 0.0851 (12) | 0.3102 (1) |
H25A | 0.5303 | 1.1953 | 0.1150 | 0.102* | 0.3102 (1) |
H25B | 0.4640 | 1.0964 | 0.0631 | 0.102* | 0.3102 (1) |
H25C | 0.5611 | 1.0577 | 0.1496 | 0.102* | 0.3102 (1) |
C26 | 0.4082 (4) | 1.1070 (5) | 0.3951 (3) | 0.0873 (11) | 0.3102 (1) |
H26A | 0.4773 | 1.1678 | 0.3806 | 0.105* | 0.3102 (1) |
H26B | 0.4410 | 1.0296 | 0.4245 | 0.105* | 0.3102 (1) |
H26C | 0.3347 | 1.1277 | 0.4535 | 0.105* | 0.3102 (1) |
N3 | −0.0388 (3) | 0.6000 (3) | 0.0981 (3) | 0.0545 (8) | 0.2855 (7) |
C27 | 0.0198 (4) | 0.5168 (3) | 0.0524 (4) | 0.0549 (10) | 0.2855 (7) |
C28 | 0.1262 (4) | 0.4455 (4) | 0.0964 (4) | 0.0718 (12) | 0.2855 (7) |
H28A | 0.0930 | 0.3653 | 0.1330 | 0.086* | 0.2855 (7) |
H28B | 0.1563 | 0.4845 | 0.1543 | 0.086* | 0.2855 (7) |
H28C | 0.1987 | 0.4404 | 0.0306 | 0.086* | 0.2855 (7) |
C29 | −0.00799 (19) | 0.63682 (17) | 0.19780 (17) | 0.0507 (9) | 0.2855 (7) |
C30 | 0.0819 (2) | 0.7294 (2) | 0.1821 (2) | 0.0456 (8) | 0.2855 (7) |
H30A | 0.1300 | 0.7600 | 0.1059 | 0.055* | 0.2855 (7) |
C31 | 0.1016 (3) | 0.7772 (2) | 0.2780 (3) | 0.0453 (9) | 0.2855 (7) |
C32 | 0.0313 (4) | 0.7325 (3) | 0.3896 (2) | 0.0564 (11) | 0.2855 (7) |
H32A | 0.0447 | 0.7652 | 0.4552 | 0.068* | 0.2855 (7) |
C33 | −0.0587 (3) | 0.6400 (3) | 0.40527 (17) | 0.0680 (12) | 0.2855 (7) |
H33A | −0.1067 | 0.6094 | 0.4815 | 0.082* | 0.2855 (7) |
C34 | −0.0783 (2) | 0.5921 (2) | 0.30937 (18) | 0.0588 (10) | 0.2855 (7) |
H34A | −0.1398 | 0.5288 | 0.3201 | 0.071* | 0.2855 (7) |
C35 | 0.1921 (3) | 0.8766 (3) | 0.2602 (4) | 0.0436 (9) | 0.2855 (7) |
C36 | 0.2687 (3) | 0.9588 (3) | 0.2440 (3) | 0.0493 (10) | 0.2855 (7) |
Si3 | 0.38282 (14) | 1.08391 (12) | 0.23218 (12) | 0.0632 (4) | 0.2855 (7) |
C37 | 0.2954 (6) | 1.2245 (4) | 0.2088 (8) | 0.0864 (15) | 0.1579 (1) |
H37A | 0.3559 | 1.2920 | 0.1984 | 0.104* | 0.1579 (1) |
H37B | 0.2253 | 1.2278 | 0.2769 | 0.104* | 0.1579 (1) |
H37C | 0.2588 | 1.2282 | 0.1386 | 0.104* | 0.1579 (1) |
C38 | 0.5165 (5) | 1.0754 (8) | 0.1039 (5) | 0.0816 (16) | 0.1579 (1) |
H38A | 0.5777 | 1.1423 | 0.0934 | 0.098* | 0.1579 (1) |
H38B | 0.4804 | 1.0792 | 0.0334 | 0.098* | 0.1579 (1) |
H38C | 0.5617 | 1.0004 | 0.1173 | 0.098* | 0.1579 (1) |
C39 | 0.4466 (6) | 1.0664 (8) | 0.3681 (4) | 0.0819 (16) | 0.1579 (1) |
H39A | 0.5084 | 1.1316 | 0.3630 | 0.098* | 0.1579 (1) |
H39B | 0.4904 | 0.9903 | 0.3783 | 0.098* | 0.1579 (1) |
H39C | 0.3747 | 1.0681 | 0.4352 | 0.098* | 0.1579 (1) |
C40 | 0.2401 (5) | 1.2043 (4) | 0.3265 (6) | 0.0988 (15) | 0.2366 (1) |
H40A | 0.2740 | 1.2860 | 0.2985 | 0.119* | 0.2366 (1) |
H40B | 0.2290 | 1.1863 | 0.4120 | 0.119* | 0.2366 (1) |
H40C | 0.1562 | 1.1962 | 0.3048 | 0.119* | 0.2366 (1) |
C41 | 0.4345 (6) | 1.1611 (5) | 0.1093 (4) | 0.0877 (14) | 0.2366 (1) |
H41A | 0.5039 | 1.2171 | 0.1103 | 0.105* | 0.2366 (1) |
H41B | 0.3707 | 1.2026 | 0.0685 | 0.105* | 0.2366 (1) |
H41C | 0.4715 | 1.0965 | 0.0684 | 0.105* | 0.2366 (1) |
C42 | 0.4770 (4) | 1.0564 (5) | 0.3526 (4) | 0.0827 (13) | 0.2366 (1) |
H42A | 0.5108 | 1.1279 | 0.3733 | 0.099* | 0.2366 (1) |
H42B | 0.5486 | 1.0154 | 0.3093 | 0.099* | 0.2366 (1) |
H42C | 0.4353 | 1.0032 | 0.4242 | 0.099* | 0.2366 (1) |
C43 | 0.5276 (4) | 1.0698 (7) | 0.2029 (7) | 0.0898 (15)* | 0.1677 (1) |
H43A | 0.5807 | 1.1410 | 0.1987 | 0.108* | 0.1677 (1) |
H43B | 0.5378 | 1.0487 | 0.1246 | 0.108* | 0.1677 (1) |
H43C | 0.5558 | 1.0037 | 0.2557 | 0.108* | 0.1677 (1) |
C44 | 0.3335 (8) | 1.1421 (6) | 0.4063 (4) | 0.0859 (17)* | 0.1677 (1) |
H44A | 0.3836 | 1.2153 | 0.4011 | 0.103* | 0.1677 (1) |
H44B | 0.3637 | 1.0781 | 0.4599 | 0.103* | 0.1677 (1) |
H44C | 0.2413 | 1.1553 | 0.4357 | 0.103* | 0.1677 (1) |
C45 | 0.2936 (6) | 1.2190 (5) | 0.1609 (5) | 0.0920 (16)* | 0.1677 (1) |
H45A | 0.3426 | 1.2931 | 0.1550 | 0.110* | 0.1677 (1) |
H45B | 0.2016 | 1.2305 | 0.1924 | 0.110* | 0.1677 (1) |
H45C | 0.3038 | 1.1969 | 0.0829 | 0.110* | 0.1677 (1) |
C46 | 0.4960 (5) | 1.0338 (9) | 0.3315 (5) | 0.0885 (17) | 0.1276 (1) |
H46A | 0.5602 | 1.0973 | 0.3254 | 0.106* | 0.1276 (1) |
H46B | 0.5406 | 0.9627 | 0.3089 | 0.106* | 0.1276 (1) |
H46C | 0.4469 | 1.0151 | 0.4125 | 0.106* | 0.1276 (1) |
C47 | 0.2916 (7) | 1.2129 (4) | 0.2757 (8) | 0.0940 (16) | 0.1276 (1) |
H47A | 0.3516 | 1.2808 | 0.2655 | 0.113* | 0.1276 (1) |
H47B | 0.2472 | 1.1937 | 0.3582 | 0.113* | 0.1276 (1) |
H47C | 0.2274 | 1.2333 | 0.2268 | 0.113* | 0.1276 (1) |
C48 | 0.4818 (8) | 1.1179 (9) | 0.0816 (4) | 0.0919 (18) | 0.1276 (1) |
H48A | 0.5407 | 1.1856 | 0.0758 | 0.110* | 0.1276 (1) |
H48B | 0.4247 | 1.1379 | 0.0258 | 0.110* | 0.1276 (1) |
H48C | 0.5326 | 1.0484 | 0.0633 | 0.110* | 0.1276 (1) |
U11 | U22 | U33 | U12 | U13 | U23 | |
N1 | 0.0487 (4) | 0.0489 (4) | 0.0525 (4) | 0.0030 (4) | 0.0056 (4) | −0.0228 (4) |
C1 | 0.0426 (5) | 0.0438 (5) | 0.0498 (5) | 0.0059 (4) | 0.0028 (4) | −0.0180 (4) |
C2 | 0.0614 (7) | 0.0694 (6) | 0.0840 (7) | −0.0147 (6) | 0.0245 (6) | −0.0422 (5) |
C3 | 0.0398 (4) | 0.0448 (5) | 0.0484 (5) | 0.0011 (4) | 0.0006 (4) | −0.0204 (4) |
C4 | 0.0391 (4) | 0.0416 (4) | 0.0431 (4) | −0.0017 (4) | −0.0007 (4) | −0.0146 (4) |
C5 | 0.0320 (4) | 0.0425 (4) | 0.0487 (5) | 0.0001 (4) | −0.0025 (4) | −0.0189 (4) |
C6 | 0.0454 (5) | 0.0572 (5) | 0.0426 (5) | 0.0061 (4) | −0.0030 (4) | −0.0225 (4) |
C7 | 0.0617 (6) | 0.0610 (6) | 0.0465 (5) | 0.0142 (5) | −0.0137 (5) | −0.0161 (5) |
C8 | 0.0555 (6) | 0.0533 (5) | 0.0577 (6) | 0.0177 (5) | −0.0100 (5) | −0.0199 (5) |
C9 | 0.0376 (4) | 0.0475 (5) | 0.0515 (5) | 0.0002 (4) | 0.0020 (4) | −0.0145 (4) |
C10 | 0.0442 (5) | 0.0545 (6) | 0.0630 (7) | 0.0067 (5) | 0.0048 (5) | −0.0087 (5) |
Si1 | 0.05134 (17) | 0.06101 (19) | 0.0858 (3) | 0.02001 (15) | 0.01242 (17) | 0.01272 (18) |
C11 | 0.0562 (7) | 0.0771 (8) | 0.0812 (9) | 0.0202 (6) | 0.0076 (6) | −0.0076 (7) |
C12 | 0.0901 (12) | 0.0519 (8) | 0.287 (3) | 0.0099 (9) | 0.0051 (17) | −0.0259 (14) |
C13 | 0.1220 (12) | 0.267 (2) | 0.0874 (13) | 0.1098 (14) | 0.0227 (11) | 0.0540 (14) |
N2 | 0.0484 (6) | 0.0505 (6) | 0.0597 (6) | −0.0039 (5) | −0.0118 (5) | −0.0209 (5) |
C14 | 0.0436 (6) | 0.0364 (6) | 0.0503 (7) | −0.0102 (5) | −0.0040 (6) | −0.0099 (5) |
C15 | 0.0550 (8) | 0.0529 (8) | 0.0613 (8) | 0.0041 (7) | −0.0097 (7) | −0.0207 (7) |
C16 | 0.0447 (7) | 0.0517 (7) | 0.0532 (7) | −0.0034 (6) | −0.0110 (6) | −0.0174 (6) |
C17 | 0.0364 (6) | 0.0458 (7) | 0.0440 (6) | 0.0002 (5) | −0.0110 (5) | −0.0082 (5) |
C18 | 0.0341 (5) | 0.0412 (6) | 0.0478 (6) | 0.0041 (5) | −0.0167 (5) | −0.0120 (5) |
C19 | 0.0511 (8) | 0.0706 (9) | 0.0522 (7) | −0.0082 (7) | −0.0063 (6) | −0.0254 (7) |
C20 | 0.0567 (9) | 0.0820 (10) | 0.0543 (8) | −0.0203 (8) | 0.0067 (7) | −0.0188 (8) |
C21 | 0.0591 (8) | 0.0629 (8) | 0.0649 (9) | −0.0204 (7) | −0.0016 (7) | −0.0225 (7) |
C22 | 0.0430 (6) | 0.0489 (7) | 0.0441 (6) | 0.0034 (6) | −0.0148 (5) | −0.0106 (6) |
C23 | 0.0537 (7) | 0.0583 (8) | 0.0453 (7) | −0.0061 (7) | −0.0176 (6) | −0.0122 (6) |
Si2 | 0.0725 (3) | 0.0670 (3) | 0.0610 (3) | −0.0286 (2) | −0.0146 (2) | −0.0129 (2) |
C24 | 0.095 (2) | 0.064 (2) | 0.106 (2) | −0.0184 (18) | −0.0241 (19) | −0.0105 (19) |
C25 | 0.081 (2) | 0.082 (2) | 0.0831 (19) | −0.0206 (18) | −0.0087 (18) | 0.0037 (19) |
C26 | 0.090 (2) | 0.100 (2) | 0.0773 (18) | −0.0416 (18) | −0.0317 (16) | −0.0097 (18) |
N3 | 0.0559 (14) | 0.0535 (14) | 0.0614 (14) | −0.0058 (13) | −0.0214 (12) | −0.0185 (12) |
C27 | 0.0519 (18) | 0.0511 (18) | 0.0666 (19) | −0.0079 (16) | −0.0203 (16) | −0.0132 (16) |
C28 | 0.077 (2) | 0.076 (2) | 0.078 (2) | 0.008 (2) | −0.0407 (18) | −0.0262 (19) |
C29 | 0.0470 (15) | 0.0506 (16) | 0.0604 (16) | −0.0046 (14) | −0.0199 (13) | −0.0151 (13) |
C30 | 0.0412 (14) | 0.0501 (16) | 0.0502 (15) | 0.0011 (13) | −0.0185 (12) | −0.0106 (13) |
C31 | 0.0391 (14) | 0.0471 (16) | 0.0520 (16) | 0.0027 (13) | −0.0130 (13) | −0.0103 (14) |
C32 | 0.0502 (18) | 0.066 (2) | 0.0552 (19) | −0.0077 (17) | −0.0071 (16) | −0.0209 (17) |
C33 | 0.065 (2) | 0.074 (2) | 0.063 (2) | −0.0187 (19) | −0.0020 (18) | −0.0207 (18) |
C34 | 0.0525 (17) | 0.0578 (18) | 0.0638 (19) | −0.0139 (16) | −0.0021 (16) | −0.0145 (16) |
C35 | 0.0416 (15) | 0.0507 (17) | 0.0468 (15) | 0.0029 (14) | −0.0243 (12) | −0.0127 (14) |
C36 | 0.0574 (18) | 0.0515 (18) | 0.0429 (16) | −0.0073 (16) | −0.0192 (14) | −0.0075 (14) |
Si3 | 0.0768 (7) | 0.0500 (6) | 0.0657 (7) | −0.0164 (6) | −0.0283 (6) | 0.0001 (5) |
C37 | 0.093 (3) | 0.069 (2) | 0.089 (2) | −0.009 (2) | −0.004 (2) | −0.008 (2) |
C38 | 0.075 (3) | 0.080 (3) | 0.083 (2) | −0.006 (2) | −0.012 (2) | 0.001 (3) |
C39 | 0.080 (3) | 0.090 (3) | 0.078 (2) | −0.030 (2) | −0.020 (2) | −0.011 (2) |
C40 | 0.107 (3) | 0.072 (2) | 0.109 (3) | −0.015 (2) | 0.002 (2) | −0.022 (2) |
C41 | 0.098 (2) | 0.078 (2) | 0.079 (2) | −0.017 (2) | −0.010 (2) | 0.004 (2) |
C42 | 0.073 (2) | 0.094 (3) | 0.087 (2) | −0.0482 (19) | −0.0336 (18) | −0.006 (2) |
C46 | 0.077 (3) | 0.090 (3) | 0.087 (3) | −0.014 (3) | −0.011 (2) | 0.010 (3) |
C47 | 0.097 (3) | 0.074 (3) | 0.092 (3) | −0.001 (2) | 0.009 (2) | 0.003 (2) |
C48 | 0.087 (3) | 0.083 (3) | 0.082 (2) | 0.006 (3) | 0.007 (3) | 0.024 (3) |
N1—C1 | 1.2662 (14) | C25—H25C | 0.9800 |
N1—C3 | 1.4220 (13) | C26—H26A | 0.9800 |
C1—C2 | 1.4954 (16) | C26—H26B | 0.9800 |
C1—C1i | 1.5083 (19) | C26—H26C | 0.9800 |
C2—H2A | 0.9800 | N3—C27 | 1.262 (5) |
C2—H2B | 0.9800 | N3—C29 | 1.413 (4) |
C2—H2C | 0.9800 | C27—C27ii | 1.495 (9) |
C3—C8 | 1.3858 (15) | C27—C28 | 1.506 (5) |
C3—C4 | 1.3878 (14) | C28—H28A | 0.9800 |
C4—C5 | 1.4024 (13) | C28—H28B | 0.9800 |
C4—H4A | 0.9500 | C28—H28C | 0.9800 |
C5—C6 | 1.3895 (14) | C29—C30 | 1.3900 |
C5—C9 | 1.4380 (14) | C29—C34 | 1.3900 |
C6—C7 | 1.3837 (16) | C30—C31 | 1.3900 |
C6—H6A | 0.9500 | C30—H30A | 0.9500 |
C7—C8 | 1.3871 (16) | C31—C32 | 1.3900 |
C7—H7A | 0.9500 | C31—C35 | 1.449 (4) |
C8—H8A | 0.9500 | C32—C33 | 1.3900 |
C9—C10 | 1.2010 (16) | C32—H32A | 0.9500 |
C10—Si1 | 1.8423 (12) | C33—C34 | 1.3900 |
Si1—C11 | 1.8370 (13) | C33—H33A | 0.9500 |
Si1—C13 | 1.844 (2) | C34—H34A | 0.9500 |
Si1—C12 | 1.856 (2) | C35—C36 | 1.208 (4) |
C11—H11A | 0.9800 | C36—Si3 | 1.846 (3) |
C11—H11B | 0.9800 | Si3—C47 | 1.834 (5) |
C11—H11C | 0.9800 | Si3—C39 | 1.848 (5) |
C12—H12A | 0.9800 | Si3—C37 | 1.848 (5) |
C12—H12B | 0.9800 | Si3—C48 | 1.851 (5) |
C12—H12C | 0.9800 | Si3—C38 | 1.859 (5) |
C13—H13A | 0.9800 | Si3—C46 | 1.863 (5) |
C13—H13B | 0.9800 | C37—H37A | 0.9800 |
C13—H13C | 0.9800 | C37—H37B | 0.9800 |
N2—C14 | 1.267 (2) | C37—H37C | 0.9800 |
N2—C16 | 1.4112 (15) | C38—H38A | 0.9800 |
C14—C15 | 1.497 (2) | C38—H38B | 0.9800 |
C14—C14ii | 1.508 (3) | C38—H38C | 0.9800 |
C15—H15A | 0.9800 | C39—H39A | 0.9800 |
C15—H15B | 0.9800 | C39—H39B | 0.9800 |
C15—H15C | 0.9800 | C39—H39C | 0.9800 |
C16—C17 | 1.3900 | C40—H40A | 0.9800 |
C16—C21 | 1.3900 | C40—H40B | 0.9800 |
C17—C18 | 1.3900 | C40—H40C | 0.9800 |
C17—H17A | 0.9500 | C41—H41A | 0.9800 |
C18—C19 | 1.3900 | C41—H41B | 0.9800 |
C18—C22 | 1.4393 (16) | C41—H41C | 0.9800 |
C19—C20 | 1.3900 | C42—H42A | 0.9800 |
C19—H19A | 0.9500 | C42—H42B | 0.9800 |
C20—C21 | 1.3900 | C42—H42C | 0.9800 |
C20—H20A | 0.9500 | C43—H43A | 0.9800 |
C21—H21A | 0.9500 | C43—H43B | 0.9800 |
C22—C23 | 1.200 (2) | C43—H43C | 0.9800 |
C23—Si2 | 1.8396 (16) | C44—H44A | 0.9800 |
Si2—C41 | 1.821 (4) | C44—H44B | 0.9800 |
Si2—C26 | 1.821 (4) | C44—H44C | 0.9800 |
Si2—C45 | 1.843 (5) | C45—H45A | 0.9800 |
Si2—C43 | 1.845 (4) | C45—H45B | 0.9800 |
Si2—C40 | 1.849 (4) | C45—H45C | 0.9800 |
Si2—C44 | 1.851 (4) | C46—H46A | 0.9800 |
Si2—C25 | 1.856 (4) | C46—H46B | 0.9800 |
Si2—C42 | 1.868 (4) | C46—H46C | 0.9800 |
Si2—C24 | 1.885 (4) | C47—H47A | 0.9800 |
C24—H24A | 0.9800 | C47—H47B | 0.9800 |
C24—H24B | 0.9800 | C47—H47C | 0.9800 |
C24—H24C | 0.9800 | C48—H48A | 0.9800 |
C25—H25A | 0.9800 | C48—H48B | 0.9800 |
C25—H25B | 0.9800 | C48—H48C | 0.9800 |
C1—N1—C3 | 120.71 (9) | C27—N3—C29 | 122.0 (3) |
N1—C1—C2 | 126.21 (10) | N3—C27—C27ii | 118.3 (4) |
N1—C1—C1i | 116.44 (11) | N3—C27—C28 | 125.2 (4) |
C2—C1—C1i | 117.34 (12) | C27ii—C27—C28 | 116.4 (4) |
C1—C2—H2A | 109.5 | C27—C28—H28A | 109.5 |
C1—C2—H2B | 109.5 | C27—C28—H28B | 109.5 |
H2A—C2—H2B | 109.5 | H28A—C28—H28B | 109.5 |
C1—C2—H2C | 109.5 | C27—C28—H28C | 109.5 |
H2A—C2—H2C | 109.5 | H28A—C28—H28C | 109.5 |
H2B—C2—H2C | 109.5 | H28B—C28—H28C | 109.5 |
C8—C3—C4 | 119.78 (9) | C30—C29—C34 | 120.0 |
C8—C3—N1 | 120.48 (9) | C30—C29—N3 | 119.00 (16) |
C4—C3—N1 | 119.59 (9) | C34—C29—N3 | 120.48 (16) |
C3—C4—C5 | 119.89 (9) | C31—C30—C29 | 120.0 |
C3—C4—H4A | 120.1 | C31—C30—H30A | 120.0 |
C5—C4—H4A | 120.1 | C29—C30—H30A | 120.0 |
C6—C5—C4 | 119.83 (9) | C30—C31—C32 | 120.0 |
C6—C5—C9 | 120.11 (9) | C30—C31—C35 | 119.5 (2) |
C4—C5—C9 | 120.06 (9) | C32—C31—C35 | 120.4 (2) |
C7—C6—C5 | 119.84 (9) | C31—C32—C33 | 120.0 |
C7—C6—H6A | 120.1 | C31—C32—H32A | 120.0 |
C5—C6—H6A | 120.1 | C33—C32—H32A | 120.0 |
C6—C7—C8 | 120.31 (10) | C34—C33—C32 | 120.0 |
C6—C7—H7A | 119.8 | C34—C33—H33A | 120.0 |
C8—C7—H7A | 119.8 | C32—C33—H33A | 120.0 |
C3—C8—C7 | 120.33 (10) | C33—C34—C29 | 120.0 |
C3—C8—H8A | 119.8 | C33—C34—H34A | 120.0 |
C7—C8—H8A | 119.8 | C29—C34—H34A | 120.0 |
C10—C9—C5 | 179.28 (12) | C36—C35—C31 | 179.1 (4) |
C9—C10—Si1 | 179.04 (13) | C35—C36—Si3 | 175.3 (4) |
C11—Si1—C10 | 108.41 (6) | C47—Si3—C36 | 109.3 (3) |
C11—Si1—C13 | 109.98 (9) | C36—Si3—C39 | 108.3 (3) |
C10—Si1—C13 | 107.50 (9) | C36—Si3—C37 | 108.5 (2) |
C11—Si1—C12 | 109.68 (10) | C39—Si3—C37 | 112.0 (4) |
C10—Si1—C12 | 108.76 (8) | C47—Si3—C48 | 112.0 (4) |
C13—Si1—C12 | 112.40 (13) | C36—Si3—C48 | 110.2 (3) |
Si1—C11—H11A | 109.5 | C36—Si3—C38 | 107.2 (3) |
Si1—C11—H11B | 109.5 | C39—Si3—C38 | 110.4 (3) |
H11A—C11—H11B | 109.5 | C37—Si3—C38 | 110.3 (3) |
Si1—C11—H11C | 109.5 | C47—Si3—C46 | 110.9 (4) |
H11A—C11—H11C | 109.5 | C36—Si3—C46 | 107.2 (3) |
H11B—C11—H11C | 109.5 | C48—Si3—C46 | 107.1 (3) |
Si1—C12—H12A | 109.5 | Si3—C37—H37A | 109.5 |
Si1—C12—H12B | 109.5 | Si3—C37—H37B | 109.5 |
H12A—C12—H12B | 109.5 | H37A—C37—H37B | 109.5 |
Si1—C12—H12C | 109.5 | Si3—C37—H37C | 109.5 |
H12A—C12—H12C | 109.5 | H37A—C37—H37C | 109.5 |
H12B—C12—H12C | 109.5 | H37B—C37—H37C | 109.5 |
Si1—C13—H13A | 109.5 | Si3—C38—H38A | 109.5 |
Si1—C13—H13B | 109.5 | Si3—C38—H38B | 109.5 |
H13A—C13—H13B | 109.5 | H38A—C38—H38B | 109.5 |
Si1—C13—H13C | 109.5 | Si3—C38—H38C | 109.5 |
H13A—C13—H13C | 109.5 | H38A—C38—H38C | 109.5 |
H13B—C13—H13C | 109.5 | H38B—C38—H38C | 109.5 |
C14—N2—C16 | 121.08 (12) | Si3—C39—H39A | 109.5 |
N2—C14—C15 | 126.51 (14) | Si3—C39—H39B | 109.5 |
N2—C14—C14ii | 116.54 (16) | H39A—C39—H39B | 109.5 |
C15—C14—C14ii | 116.91 (17) | Si3—C39—H39C | 109.5 |
C17—C16—C21 | 120.0 | H39A—C39—H39C | 109.5 |
C17—C16—N2 | 119.61 (6) | H39B—C39—H39C | 109.5 |
C21—C16—N2 | 120.12 (6) | Si2—C40—H40A | 109.5 |
C18—C17—C16 | 120.0 | Si2—C40—H40B | 109.5 |
C18—C17—H17A | 120.0 | H40A—C40—H40B | 109.5 |
C16—C17—H17A | 120.0 | Si2—C40—H40C | 109.5 |
C19—C18—C17 | 120.0 | H40A—C40—H40C | 109.5 |
C19—C18—C22 | 119.81 (9) | H40B—C40—H40C | 109.5 |
C17—C18—C22 | 120.10 (9) | Si2—C41—H41A | 109.5 |
C18—C19—C20 | 120.0 | Si2—C41—H41B | 109.5 |
C18—C19—H19A | 120.0 | H41A—C41—H41B | 109.5 |
C20—C19—H19A | 120.0 | Si2—C41—H41C | 109.5 |
C19—C20—C21 | 120.0 | H41A—C41—H41C | 109.5 |
C19—C20—H20A | 120.0 | H41B—C41—H41C | 109.5 |
C21—C20—H20A | 120.0 | Si2—C42—H42A | 109.5 |
C20—C21—C16 | 120.0 | Si2—C42—H42B | 109.5 |
C20—C21—H21A | 120.0 | H42A—C42—H42B | 109.5 |
C16—C21—H21A | 120.0 | Si2—C42—H42C | 109.5 |
C23—C22—C18 | 177.38 (16) | H42A—C42—H42C | 109.5 |
C22—C23—Si2 | 177.45 (15) | H42B—C42—H42C | 109.5 |
C41—Si2—C23 | 112.6 (2) | Si2—C43—H43A | 109.5 |
C26—Si2—C23 | 111.83 (15) | Si2—C43—H43B | 109.5 |
C23—Si2—C45 | 108.5 (2) | H43A—C43—H43B | 109.5 |
C23—Si2—C43 | 107.4 (3) | Si2—C43—H43C | 109.5 |
C45—Si2—C43 | 112.0 (3) | H43A—C43—H43C | 109.5 |
C41—Si2—C40 | 112.0 (3) | H43B—C43—H43C | 109.5 |
C23—Si2—C40 | 106.22 (18) | Si2—C44—H44A | 109.5 |
C23—Si2—C44 | 109.6 (2) | Si2—C44—H44B | 109.5 |
C45—Si2—C44 | 108.8 (3) | H44A—C44—H44B | 109.5 |
C43—Si2—C44 | 110.6 (4) | Si2—C44—H44C | 109.5 |
C26—Si2—C25 | 112.0 (2) | H44A—C44—H44C | 109.5 |
C23—Si2—C25 | 109.81 (17) | H44B—C44—H44C | 109.5 |
C41—Si2—C42 | 111.4 (2) | Si2—C45—H45A | 109.5 |
C23—Si2—C42 | 104.83 (19) | Si2—C45—H45B | 109.5 |
C40—Si2—C42 | 109.4 (3) | H45A—C45—H45B | 109.5 |
C26—Si2—C24 | 108.2 (2) | Si2—C45—H45C | 109.5 |
C23—Si2—C24 | 106.21 (15) | H45A—C45—H45C | 109.5 |
C25—Si2—C24 | 108.5 (2) | H45B—C45—H45C | 109.5 |
Si2—C24—H24A | 109.5 | Si3—C46—H46A | 109.5 |
Si2—C24—H24B | 109.5 | Si3—C46—H46B | 109.5 |
H24A—C24—H24B | 109.5 | H46A—C46—H46B | 109.5 |
Si2—C24—H24C | 109.5 | Si3—C46—H46C | 109.5 |
H24A—C24—H24C | 109.5 | H46A—C46—H46C | 109.5 |
H24B—C24—H24C | 109.5 | H46B—C46—H46C | 109.5 |
Si2—C25—H25A | 109.5 | Si3—C47—H47A | 109.5 |
Si2—C25—H25B | 109.5 | Si3—C47—H47B | 109.5 |
H25A—C25—H25B | 109.5 | H47A—C47—H47B | 109.5 |
Si2—C25—H25C | 109.5 | Si3—C47—H47C | 109.5 |
H25A—C25—H25C | 109.5 | H47A—C47—H47C | 109.5 |
H25B—C25—H25C | 109.5 | H47B—C47—H47C | 109.5 |
Si2—C26—H26A | 109.5 | Si3—C48—H48A | 109.5 |
Si2—C26—H26B | 109.5 | Si3—C48—H48B | 109.5 |
H26A—C26—H26B | 109.5 | H48A—C48—H48B | 109.5 |
Si2—C26—H26C | 109.5 | Si3—C48—H48C | 109.5 |
H26A—C26—H26C | 109.5 | H48A—C48—H48C | 109.5 |
H26B—C26—H26C | 109.5 | H48B—C48—H48C | 109.5 |
Symmetry codes: (i) −x, −y+2, −z+2; (ii) −x, −y+1, −z. |
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