Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805036445/er6026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805036445/er6026IIsup2.hkl |
CCDC reference: 293888
Key indicators
- Single-crystal X-ray study
- T = 225 K
- Mean (C-C) = 0.003 Å
- R factor = 0.057
- wR factor = 0.173
- Data-to-parameter ratio = 14.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N1 C14 N1 C12 C11 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 C16 C1 C12 N13 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 SI C1 C12 N13 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N1 C12 N1 C14 O14 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N1 C12 N1 C14 C15 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O1 C17 O1 C14 N13 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O1 C17 O1 C14 C15 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 N13 C1 C15 C16 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 O14 C1 C15 C16 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 C14 C1 C16 C11 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 C12 C1 C16 C15 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C1 SI C1 C16 C15 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N2 C24 N2 C22 C21 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 C26 C2 C22 N23 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 SI C2 C22 N23 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N2 C22 N2 C24 O24 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N2 C22 N2 C24 C25 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O2 C27 O2 C24 N23 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O2 C27 O2 C24 C25 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 N23 C2 C25 C26 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 O24 C2 C25 C26 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 C24 C2 C26 C21 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 C22 C2 C26 C25 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C2 SI C2 C26 C25 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N3 C34 N3 C32 C31 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 C36 C3 C32 N33 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 SI C3 C32 N33 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N3 C32 N3 C34 O34 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N3 C32 N3 C34 C35 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O3 C37 O3 C34 N33 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O3 C37 O3 C34 C35 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 N33 C3 C35 C36 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 O34 C3 C35 C36 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 C34 C3 C36 C31 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 C32 C3 C36 C35 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C3 SI C3 C36 C35 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N4 C44 N4 C42 C41 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 C46 C4 C42 N43 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 SI C4 C42 N43 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N4 C42 N4 C44 O44 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... N4 C42 N4 C44 C45 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O4 C47 O4 C44 N43 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... O4 C47 O4 C44 C45 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 N43 C4 C45 C46 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 O44 C4 C45 C46 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 C44 C4 C46 C41 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 C42 C4 C46 C45 PLAT713_ALERT_1_C TORSION Unknown or Inconsistent Label .......... C4 SI C4 C46 C45
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 48 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 48 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: modified versions of NRC-2/NRC2A (Ahmed et al., 1973); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: enCIFer (Allen et al., 2004).
C24H24N4O4Si | Z = 2 |
Mr = 460.56 | F(000) = 484 |
Triclinic, P1 | Dx = 1.342 Mg m−3 |
Hall symbol: -P 1 | Cu Kα radiation, λ = 1.54178 Å |
a = 9.661 (3) Å | Cell parameters from 25 reflections |
b = 10.364 (4) Å | θ = 15.0–30.0° |
c = 12.230 (6) Å | µ = 1.24 mm−1 |
α = 107.74 (4)° | T = 225 K |
β = 94.68 (3)° | Block, colorless |
γ = 99.22 (3)° | 0.52 × 0.48 × 0.18 mm |
V = 1140.1 (9) Å3 |
Enraf–Nonius CAD-4 diffractometer | 3964 reflections with I > 2σ(I) |
Radiation source: X-ray sealed tube | Rint = 0.078 |
Graphite monochromator | θmax = 69.8°, θmin = 3.8° |
ω/2θ scans | h = −11→11 |
Absorption correction: analytical (ABSORP in NRCVAX; Gabe et al., 1989) | k = −12→12 |
Tmin = 0.570, Tmax = 0.810 | l = −14→14 |
8614 measured reflections | 6 standard reflections every 60 min |
4319 independent reflections | intensity decay: 0.1% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.057 | H-atom parameters constrained |
wR(F2) = 0.173 | w = 1/[σ2(Fo2) + (0.1135P)2 + 0.4013P] where P = (Fo2 + 2Fc2)/3 |
S = 1.11 | (Δ/σ)max < 0.001 |
4319 reflections | Δρmax = 0.43 e Å−3 |
302 parameters | Δρmin = −0.53 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0133 (15) |
Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using an Enraf–Nonius CAD4 diffractometer equipped with FR590 generator, a Kappa goniometer, a standard scintillation counter and a locally modified low temperature device. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of 25 strong reflections. The intensity of some selected strong reflections was monitored during the course of the data collection. Data were corrected for absorption, Lorentz and polarization effects |
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. |
x | y | z | Uiso*/Ueq | ||
Si | 0.28028 (5) | 0.24267 (5) | 0.32296 (5) | 0.0327 (2) | |
O14 | 0.53201 (18) | 0.13402 (16) | 0.73881 (14) | 0.0463 (4) | |
O24 | 0.05137 (19) | 0.76165 (16) | 0.45700 (14) | 0.0488 (4) | |
O34 | −0.18124 (16) | −0.21736 (16) | 0.03363 (13) | 0.0464 (4) | |
O44 | 0.79059 (17) | 0.35816 (18) | 0.10007 (16) | 0.0517 (4) | |
N13 | 0.5264 (2) | 0.26889 (18) | 0.62133 (16) | 0.0410 (4) | |
N23 | 0.0789 (2) | 0.56330 (19) | 0.31729 (16) | 0.0413 (4) | |
N33 | −0.10641 (19) | −0.01673 (19) | 0.18841 (16) | 0.0409 (4) | |
N43 | 0.5946 (2) | 0.42981 (18) | 0.17707 (16) | 0.0393 (4) | |
C11 | 0.3500 (2) | 0.1973 (2) | 0.45052 (18) | 0.0343 (4) | |
C12 | 0.4638 (2) | 0.2871 (2) | 0.52634 (19) | 0.0402 (5) | |
H12 | 0.5006 | 0.3677 | 0.5100 | 0.048* | |
C14 | 0.4734 (2) | 0.1558 (2) | 0.64314 (18) | 0.0368 (5) | |
C15 | 0.3609 (2) | 0.0552 (2) | 0.5738 (2) | 0.0427 (5) | |
H15 | 0.3278 | −0.0251 | 0.5922 | 0.051* | |
C16 | 0.2997 (2) | 0.0778 (2) | 0.47714 (19) | 0.0400 (5) | |
H16 | 0.2233 | 0.0120 | 0.4285 | 0.048* | |
C17 | 0.6353 (3) | 0.2466 (3) | 0.8163 (2) | 0.0569 (7) | |
H17A | 0.5950 | 0.3293 | 0.8376 | 0.085* | |
H17B | 0.7177 | 0.2624 | 0.7783 | 0.085* | |
H17C | 0.6630 | 0.2245 | 0.8855 | 0.085* | |
C21 | 0.2040 (2) | 0.4026 (2) | 0.37185 (17) | 0.0346 (4) | |
C22 | 0.1313 (3) | 0.4464 (2) | 0.29208 (19) | 0.0420 (5) | |
H22 | 0.1174 | 0.3901 | 0.2141 | 0.050* | |
C24 | 0.0992 (2) | 0.6409 (2) | 0.42661 (18) | 0.0374 (5) | |
C25 | 0.1683 (2) | 0.6080 (2) | 0.51605 (19) | 0.0422 (5) | |
H25 | 0.1795 | 0.6664 | 0.5933 | 0.051* | |
C26 | 0.2193 (2) | 0.4882 (2) | 0.48796 (18) | 0.0377 (5) | |
H26 | 0.2651 | 0.4626 | 0.5467 | 0.045* | |
C27 | −0.0282 (3) | 0.7912 (3) | 0.3666 (2) | 0.0525 (6) | |
H27A | −0.0518 | 0.8817 | 0.3970 | 0.079* | |
H27B | −0.1145 | 0.7220 | 0.3374 | 0.079* | |
H27C | 0.0279 | 0.7898 | 0.3041 | 0.079* | |
C31 | 0.1398 (2) | 0.0977 (2) | 0.22623 (17) | 0.0348 (4) | |
C32 | 0.0024 (2) | 0.0850 (2) | 0.24998 (18) | 0.0405 (5) | |
H32 | −0.0172 | 0.1530 | 0.3145 | 0.049* | |
C34 | −0.0767 (2) | −0.1118 (2) | 0.09871 (17) | 0.0368 (5) | |
C35 | 0.0568 (2) | −0.1119 (2) | 0.06465 (19) | 0.0414 (5) | |
H35 | 0.0730 | −0.1822 | 0.0001 | 0.050* | |
C36 | 0.1645 (2) | −0.0056 (2) | 0.12877 (19) | 0.0398 (5) | |
H36 | 0.2558 | −0.0018 | 0.1072 | 0.048* | |
C37 | −0.3191 (3) | −0.2177 (3) | 0.0694 (2) | 0.0569 (7) | |
H37A | −0.3143 | −0.2198 | 0.1484 | 0.085* | |
H37B | −0.3849 | −0.2986 | 0.0185 | 0.085* | |
H37C | −0.3512 | −0.1350 | 0.0656 | 0.085* | |
C41 | 0.4374 (2) | 0.2765 (2) | 0.24831 (17) | 0.0339 (4) | |
C42 | 0.4786 (2) | 0.3985 (2) | 0.22550 (18) | 0.0366 (5) | |
H42 | 0.4213 | 0.4651 | 0.2453 | 0.044* | |
C44 | 0.6736 (2) | 0.3348 (2) | 0.15048 (18) | 0.0375 (5) | |
C45 | 0.6449 (2) | 0.2081 (2) | 0.1696 (2) | 0.0422 (5) | |
H45 | 0.7046 | 0.1438 | 0.1489 | 0.051* | |
C46 | 0.5270 (2) | 0.1803 (2) | 0.21969 (19) | 0.0396 (5) | |
H46 | 0.5057 | 0.0963 | 0.2351 | 0.047* | |
C47 | 0.8219 (3) | 0.4862 (3) | 0.0766 (3) | 0.0610 (7) | |
H47A | 0.8175 | 0.4680 | −0.0063 | 0.092* | |
H47B | 0.9162 | 0.5351 | 0.1145 | 0.092* | |
H47C | 0.7533 | 0.5423 | 0.1059 | 0.092* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si | 0.0312 (3) | 0.0295 (3) | 0.0318 (3) | −0.0033 (2) | 0.0037 (2) | 0.0067 (2) |
O14 | 0.0557 (10) | 0.0404 (8) | 0.0414 (8) | 0.0029 (7) | 0.0009 (7) | 0.0162 (7) |
O24 | 0.0571 (10) | 0.0375 (9) | 0.0465 (9) | 0.0100 (7) | 0.0096 (7) | 0.0048 (7) |
O34 | 0.0394 (8) | 0.0413 (9) | 0.0419 (8) | −0.0101 (7) | 0.0022 (7) | −0.0004 (7) |
O44 | 0.0424 (9) | 0.0508 (10) | 0.0590 (10) | 0.0000 (7) | 0.0216 (8) | 0.0145 (8) |
N13 | 0.0429 (10) | 0.0332 (9) | 0.0418 (10) | −0.0051 (7) | −0.0003 (8) | 0.0127 (8) |
N23 | 0.0429 (10) | 0.0380 (10) | 0.0377 (9) | 0.0049 (8) | 0.0044 (7) | 0.0063 (8) |
N33 | 0.0334 (9) | 0.0393 (10) | 0.0389 (9) | −0.0033 (7) | 0.0062 (7) | 0.0018 (8) |
N43 | 0.0409 (10) | 0.0328 (9) | 0.0400 (9) | −0.0017 (7) | 0.0108 (7) | 0.0090 (7) |
C11 | 0.0330 (10) | 0.0318 (10) | 0.0342 (10) | −0.0017 (8) | 0.0066 (8) | 0.0086 (8) |
C12 | 0.0398 (11) | 0.0338 (10) | 0.0430 (11) | −0.0085 (8) | −0.0019 (9) | 0.0164 (9) |
C14 | 0.0424 (11) | 0.0316 (10) | 0.0362 (10) | 0.0056 (8) | 0.0102 (9) | 0.0104 (8) |
C15 | 0.0475 (12) | 0.0324 (10) | 0.0469 (12) | −0.0037 (9) | 0.0076 (10) | 0.0161 (9) |
C16 | 0.0391 (11) | 0.0315 (10) | 0.0417 (11) | −0.0070 (8) | 0.0036 (9) | 0.0080 (8) |
C17 | 0.0597 (16) | 0.0553 (15) | 0.0486 (14) | −0.0023 (12) | −0.0110 (12) | 0.0181 (12) |
C21 | 0.0304 (10) | 0.0323 (10) | 0.0350 (10) | −0.0029 (7) | 0.0051 (8) | 0.0062 (8) |
C22 | 0.0493 (12) | 0.0354 (11) | 0.0330 (10) | 0.0028 (9) | 0.0035 (9) | 0.0022 (8) |
C24 | 0.0346 (10) | 0.0313 (10) | 0.0401 (11) | −0.0004 (8) | 0.0083 (8) | 0.0055 (8) |
C25 | 0.0435 (12) | 0.0396 (11) | 0.0322 (10) | −0.0011 (9) | 0.0055 (9) | 0.0001 (9) |
C26 | 0.0338 (10) | 0.0390 (11) | 0.0338 (10) | −0.0024 (8) | 0.0033 (8) | 0.0077 (8) |
C27 | 0.0553 (15) | 0.0437 (13) | 0.0582 (15) | 0.0133 (11) | 0.0101 (12) | 0.0135 (11) |
C31 | 0.0371 (10) | 0.0303 (10) | 0.0322 (10) | −0.0016 (8) | 0.0054 (8) | 0.0070 (8) |
C32 | 0.0379 (11) | 0.0369 (11) | 0.0352 (10) | −0.0010 (8) | 0.0054 (8) | −0.0009 (8) |
C34 | 0.0393 (11) | 0.0316 (10) | 0.0315 (10) | −0.0038 (8) | 0.0016 (8) | 0.0052 (8) |
C35 | 0.0408 (12) | 0.0357 (11) | 0.0381 (11) | 0.0018 (9) | 0.0077 (9) | 0.0002 (9) |
C36 | 0.0354 (11) | 0.0386 (11) | 0.0395 (11) | 0.0011 (9) | 0.0093 (9) | 0.0062 (9) |
C37 | 0.0374 (12) | 0.0565 (15) | 0.0576 (15) | −0.0106 (11) | 0.0013 (11) | 0.0019 (12) |
C41 | 0.0340 (10) | 0.0312 (10) | 0.0315 (9) | −0.0010 (8) | 0.0023 (8) | 0.0071 (8) |
C42 | 0.0356 (10) | 0.0316 (10) | 0.0385 (10) | 0.0015 (8) | 0.0077 (8) | 0.0074 (8) |
C44 | 0.0326 (10) | 0.0382 (11) | 0.0333 (10) | −0.0028 (8) | 0.0063 (8) | 0.0040 (8) |
C45 | 0.0381 (11) | 0.0380 (11) | 0.0469 (12) | 0.0063 (9) | 0.0077 (9) | 0.0086 (9) |
C46 | 0.0401 (11) | 0.0318 (10) | 0.0442 (11) | 0.0004 (8) | 0.0058 (9) | 0.0118 (9) |
C47 | 0.0563 (16) | 0.0574 (16) | 0.0664 (17) | −0.0080 (12) | 0.0243 (13) | 0.0214 (13) |
Si—C11 | 1.867 (2) | C21—C22 | 1.383 (3) |
Si—C31 | 1.871 (2) | C21—C26 | 1.408 (3) |
Si—C21 | 1.872 (2) | C22—H22 | 0.94 |
Si—C41 | 1.874 (2) | C24—C25 | 1.392 (3) |
O14—C14 | 1.354 (3) | C25—C26 | 1.367 (3) |
O14—C17 | 1.433 (3) | C25—H25 | 0.94 |
O24—C24 | 1.360 (3) | C26—H26 | 0.94 |
O24—C27 | 1.432 (3) | C27—H27A | 0.97 |
O34—C34 | 1.354 (3) | C27—H27B | 0.97 |
O34—C37 | 1.435 (3) | C27—H27C | 0.97 |
O44—C44 | 1.354 (3) | C31—C32 | 1.377 (3) |
O44—C47 | 1.433 (3) | C31—C36 | 1.405 (3) |
N13—C14 | 1.315 (3) | C32—H32 | 0.94 |
N13—C12 | 1.344 (3) | C34—C35 | 1.388 (3) |
N23—C24 | 1.313 (3) | C35—C36 | 1.373 (3) |
N23—C22 | 1.347 (3) | C35—H35 | 0.94 |
N33—C34 | 1.319 (3) | C36—H36 | 0.94 |
N33—C32 | 1.348 (3) | C37—H37A | 0.97 |
N43—C44 | 1.320 (3) | C37—H37B | 0.97 |
N43—C42 | 1.349 (3) | C37—H37C | 0.97 |
C11—C12 | 1.384 (3) | C41—C42 | 1.381 (3) |
C11—C16 | 1.398 (3) | C41—C46 | 1.407 (3) |
C12—H12 | 0.94 | C42—H42 | 0.94 |
C14—C15 | 1.391 (3) | C44—C45 | 1.392 (3) |
C15—C16 | 1.379 (3) | C45—C46 | 1.368 (3) |
C15—H15 | 0.94 | C45—H45 | 0.94 |
C16—H16 | 0.94 | C46—H46 | 0.94 |
C17—H17A | 0.97 | C47—H47A | 0.97 |
C17—H17B | 0.97 | C47—H47B | 0.97 |
C17—H17C | 0.97 | C47—H47C | 0.97 |
C11—SI—C31 | 110.28 (10) | C21—C26—H26 | 119.7 |
C11—SI—C21 | 110.38 (10) | O24—C27—H27A | 109.5 |
C31—SI—C21 | 109.15 (10) | O24—C27—H27B | 109.5 |
C11—SI—C41 | 105.43 (10) | H27A—C27—H27B | 109.5 |
C31—SI—C41 | 111.96 (10) | O24—C27—H27C | 109.5 |
C21—SI—C41 | 109.59 (10) | H27A—C27—H27C | 109.5 |
C14—O14—C17 | 116.00 (18) | H27B—C27—H27C | 109.5 |
C24—O24—C27 | 116.65 (18) | C32—C31—C36 | 115.50 (19) |
C34—O34—C37 | 116.28 (18) | C32—C31—SI | 120.23 (15) |
C44—O44—C47 | 117.65 (19) | C36—C31—SI | 124.25 (16) |
C14—N13—C12 | 116.36 (18) | N33—C32—C31 | 125.43 (19) |
C24—N23—C22 | 116.7 (2) | N33—C32—H32 | 117.3 |
C34—N33—C32 | 116.43 (19) | C31—C32—H32 | 117.3 |
C44—N43—C42 | 116.22 (19) | N33—C34—O34 | 119.4 (2) |
C12—C11—C16 | 115.35 (19) | N33—C34—C35 | 124.32 (19) |
C12—C11—SI | 118.50 (15) | O34—C34—C35 | 116.31 (19) |
C16—C11—SI | 126.13 (16) | C36—C35—C34 | 117.5 (2) |
N13—C12—C11 | 125.67 (19) | C36—C35—H35 | 121.3 |
N13—C12—H12 | 117.2 | C34—C35—H35 | 121.3 |
C11—C12—H12 | 117.2 | C35—C36—C31 | 120.8 (2) |
N13—C14—O14 | 118.39 (19) | C35—C36—H36 | 119.6 |
N13—C14—C15 | 124.4 (2) | C31—C36—H36 | 119.6 |
O14—C14—C15 | 117.20 (19) | O34—C37—H37A | 109.5 |
C16—C15—C14 | 117.36 (19) | O34—C37—H37B | 109.5 |
C16—C15—H15 | 121.3 | H37A—C37—H37B | 109.5 |
C14—C15—H15 | 121.3 | O34—C37—H37C | 109.5 |
C15—C16—C11 | 120.8 (2) | H37A—C37—H37C | 109.5 |
C15—C16—H16 | 119.6 | H37B—C37—H37C | 109.5 |
C11—C16—H16 | 119.6 | C42—C41—C46 | 115.94 (19) |
O14—C17—H17A | 109.5 | C42—C41—SI | 123.22 (16) |
O14—C17—H17B | 109.5 | C46—C41—SI | 120.69 (16) |
H17A—C17—H17B | 109.5 | N43—C42—C41 | 125.2 (2) |
O14—C17—H17C | 109.5 | N43—C42—H42 | 117.4 |
H17A—C17—H17C | 109.5 | C41—C42—H42 | 117.4 |
H17B—C17—H17C | 109.5 | N43—C44—O44 | 119.5 (2) |
C22—C21—C26 | 115.5 (2) | N43—C44—C45 | 124.48 (19) |
C22—C21—SI | 120.47 (16) | O44—C44—C45 | 116.0 (2) |
C26—C21—SI | 124.04 (17) | C46—C45—C44 | 117.7 (2) |
N23—C22—C21 | 125.2 (2) | C46—C45—H45 | 121.2 |
N23—C22—H22 | 117.4 | C44—C45—H45 | 121.2 |
C21—C22—H22 | 117.4 | C45—C46—C41 | 120.5 (2) |
N23—C24—O24 | 119.4 (2) | C45—C46—H46 | 119.8 |
N23—C24—C25 | 124.1 (2) | C41—C46—H46 | 119.8 |
O24—C24—C25 | 116.52 (19) | O44—C47—H47A | 109.5 |
C26—C25—C24 | 117.9 (2) | O44—C47—H47B | 109.5 |
C26—C25—H25 | 121.1 | H47A—C47—H47B | 109.5 |
C24—C25—H25 | 121.1 | O44—C47—H47C | 109.5 |
C25—C26—C21 | 120.6 (2) | H47A—C47—H47C | 109.5 |
C25—C26—H26 | 119.7 | H47B—C47—H47C | 109.5 |
C31—SI—C11—C12 | 174.20 (17) | C11—SI—C31—C32 | 83.4 (2) |
C21—SI—C11—C12 | −65.1 (2) | C21—SI—C31—C32 | −38.1 (2) |
C41—SI—C11—C12 | 53.16 (19) | C41—SI—C31—C32 | −159.57 (17) |
C31—SI—C11—C16 | −4.5 (2) | C11—SI—C31—C36 | −95.0 (2) |
C21—SI—C11—C16 | 116.21 (19) | C21—SI—C31—C36 | 143.55 (19) |
C41—SI—C11—C16 | −125.52 (19) | C41—SI—C31—C36 | 22.0 (2) |
C14—N1—C12—C11 | −0.2 (3) | C34—N3—C32—C31 | 0.5 (4) |
C16—C1—C12—N13 | −0.8 (3) | C36—C3—C32—N33 | 0.3 (3) |
SI—C1—C12—N13 | −179.61 (18) | SI—C3—C32—N33 | −178.21 (18) |
C12—N1—C14—O14 | −179.18 (19) | C32—N3—C34—O34 | 179.60 (19) |
C12—N1—C14—C15 | 1.3 (3) | C32—N3—C34—C35 | −0.6 (3) |
C17—O1—C14—N13 | 8.1 (3) | C37—O3—C34—N33 | −0.6 (3) |
C17—O1—C14—C15 | −172.3 (2) | C37—O3—C34—C35 | 179.5 (2) |
N13—C1—C15—C16 | −1.3 (3) | N33—C3—C35—C36 | −0.2 (4) |
O14—C1—C15—C16 | 179.2 (2) | O34—C3—C35—C36 | 179.6 (2) |
C14—C1—C16—C11 | 0.2 (3) | C34—C3—C36—C31 | 1.1 (3) |
C12—C1—C16—C15 | 0.8 (3) | C32—C3—C36—C35 | −1.1 (3) |
SI—C1—C16—C15 | 179.48 (17) | SI—C3—C36—C35 | 177.33 (17) |
C11—SI—C21—C22 | −172.37 (17) | C11—SI—C41—C42 | −124.20 (18) |
C31—SI—C21—C22 | −51.00 (19) | C31—SI—C41—C42 | 115.86 (18) |
C41—SI—C21—C22 | 71.94 (19) | C21—SI—C41—C42 | −5.4 (2) |
C11—SI—C21—C26 | 9.9 (2) | C11—SI—C41—C46 | 51.09 (19) |
C31—SI—C21—C26 | 131.28 (17) | C31—SI—C41—C46 | −68.85 (19) |
C41—SI—C21—C26 | −105.78 (18) | C21—SI—C41—C46 | 169.89 (16) |
C24—N2—C22—C21 | 0.1 (3) | C44—N4—C42—C41 | −0.2 (3) |
C26—C2—C22—N23 | 1.5 (3) | C46—C4—C42—N43 | 1.2 (3) |
SI—C2—C22—N23 | −176.37 (18) | SI—C4—C42—N43 | 176.66 (16) |
C22—N2—C24—O24 | 178.60 (19) | C42—N4—C44—O44 | 179.05 (19) |
C22—N2—C24—C25 | −1.3 (3) | C42—N4—C44—C45 | −0.3 (3) |
C27—O2—C24—N23 | 4.3 (3) | C47—O4—C44—N43 | −0.7 (3) |
C27—O2—C24—C25 | −175.8 (2) | C47—O4—C44—C45 | 178.7 (2) |
N23—C2—C25—C26 | 0.7 (3) | N43—C4—C45—C46 | −0.2 (3) |
O24—C2—C25—C26 | −179.13 (19) | O44—C4—C45—C46 | −179.54 (19) |
C24—C2—C26—C21 | 1.0 (3) | C44—C4—C46—C41 | 1.2 (3) |
C22—C2—C26—C25 | −2.0 (3) | C42—C4—C46—C45 | −1.6 (3) |
SI—C2—C26—C25 | 175.80 (16) | SI—C4—C46—C45 | −177.23 (17) |
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