Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100008775/fr1269sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100008775/fr1269Isup2.hkl |
CCDC reference: 150769
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
[Sm(C9H9F5NSi)3(C4H8O)] | F(000) = 1956 |
Mr = 985.24 | Dx = 1.675 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 17.447 (3) Å | Cell parameters from 31 reflections |
b = 10.467 (2) Å | θ = 13.0–13.5° |
c = 21.934 (4) Å | µ = 1.70 mm−1 |
β = 102.77 (1)° | T = 203 K |
V = 3906.5 (12) Å3 | Block, yellow |
Z = 4 | 0.45 × 0.33 × 0.25 mm |
Siemens P4/PC diffractometer | 5303 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.041 |
Graphite monochromator | θmax = 25.0°, θmin = 2.6° |
ω scans | h = −20→20 |
Absorption correction: empirical (using intensity measurements) (XSCANS; Siemens, 1994) | k = −12→1 |
Tmin = 0.46, Tmax = 0.65 | l = −1→26 |
8237 measured reflections | 3 standard reflections every 97 reflections |
6811 independent reflections | intensity decay: 13 (linear) |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0451P)2 + 4.7821P] where P = (Fo2 + 2Fc2)/3 |
6811 reflections | (Δ/σ)max = 0.001 |
487 parameters | Δρmax = 0.99 (1.0Å from Sm1) e Å−3 |
0 restraints | Δρmin = −1.02 (1.0Å from Sm1) e Å−3 |
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. Hydrogen atom positions were idealized; C—H distances were fixed at 0.93 Å for aromatic, 0.96 Å for methyl, and 0.98 Å for methylene. The hydrogen atom positions were refined using the riding model, with their isotropic temperature factors set to 1.5 (methyl) or 1.2 (methylene, aromatic) times the equivalent isotropic U of the atom they were bonded to. |
x | y | z | Uiso*/Ueq | ||
Sm1 | 0.249096 (13) | 0.01041 (2) | 0.754458 (10) | 0.03195 (9) | |
Si1 | 0.22618 (8) | −0.21384 (13) | 0.63541 (7) | 0.0430 (3) | |
Si2 | 0.07850 (8) | 0.20103 (14) | 0.67863 (7) | 0.0418 (3) | |
Si3 | 0.43041 (8) | 0.14615 (14) | 0.83873 (6) | 0.0418 (3) | |
O1 | 0.3140 (2) | −0.1701 (3) | 0.81568 (16) | 0.0507 (9) | |
N1 | 0.2762 (2) | −0.0728 (4) | 0.66120 (17) | 0.0355 (9) | |
N2 | 0.1329 (2) | 0.1269 (4) | 0.74634 (17) | 0.0372 (9) | |
N3 | 0.3290 (2) | 0.1381 (4) | 0.82706 (18) | 0.0377 (9) | |
C1 | 0.1609 (3) | −0.2361 (5) | 0.6925 (2) | 0.0498 (13) | |
H1A | 0.1927 | −0.2425 | 0.7341 | 0.075* | |
H1B | 0.1306 | −0.3129 | 0.6824 | 0.075* | |
H1C | 0.1261 | −0.1643 | 0.6900 | 0.075* | |
C2 | 0.1636 (3) | −0.2011 (6) | 0.5553 (2) | 0.0565 (15) | |
H2A | 0.1964 | −0.1901 | 0.5258 | 0.085* | |
H2B | 0.1291 | −0.1290 | 0.5531 | 0.085* | |
H2C | 0.1330 | −0.2776 | 0.5455 | 0.085* | |
C3 | 0.2872 (4) | −0.3622 (5) | 0.6381 (3) | 0.0676 (17) | |
H3A | 0.3204 | −0.3713 | 0.6791 | 0.101* | |
H3B | 0.3191 | −0.3559 | 0.6077 | 0.101* | |
H3C | 0.2533 | −0.4352 | 0.6289 | 0.101* | |
C4 | 0.1043 (4) | 0.3715 (5) | 0.6694 (3) | 0.0654 (16) | |
H4A | 0.0935 | 0.4205 | 0.7036 | 0.098* | |
H4B | 0.0734 | 0.4040 | 0.6307 | 0.098* | |
H4C | 0.1591 | 0.3781 | 0.6691 | 0.098* | |
C5 | −0.0286 (3) | 0.1805 (6) | 0.6742 (3) | 0.0560 (14) | |
H5A | −0.0428 | 0.2240 | 0.7087 | 0.084* | |
H5B | −0.0405 | 0.0912 | 0.6761 | 0.084* | |
H5C | −0.0579 | 0.2156 | 0.6356 | 0.084* | |
C6 | 0.1013 (3) | 0.1145 (6) | 0.6110 (2) | 0.0578 (15) | |
H6A | 0.1563 | 0.1229 | 0.6117 | 0.087* | |
H6B | 0.0710 | 0.1499 | 0.5729 | 0.087* | |
H6C | 0.0885 | 0.0257 | 0.6135 | 0.087* | |
C7 | 0.4835 (3) | 0.0813 (7) | 0.9157 (2) | 0.0627 (17) | |
H7A | 0.4675 | −0.0055 | 0.9198 | 0.094* | |
H7B | 0.4713 | 0.1320 | 0.9488 | 0.094* | |
H7C | 0.5391 | 0.0838 | 0.9181 | 0.094* | |
C8 | 0.4598 (3) | 0.0492 (7) | 0.7763 (3) | 0.0673 (18) | |
H8A | 0.4430 | −0.0375 | 0.7790 | 0.101* | |
H8B | 0.5159 | 0.0517 | 0.7817 | 0.101* | |
H8C | 0.4355 | 0.0837 | 0.7361 | 0.101* | |
C9 | 0.4641 (3) | 0.3132 (6) | 0.8341 (4) | 0.092 (3) | |
H9A | 0.4377 | 0.3502 | 0.7950 | 0.138* | |
H9B | 0.5198 | 0.3140 | 0.8369 | 0.138* | |
H9C | 0.4524 | 0.3619 | 0.8680 | 0.138* | |
C10 | 0.3139 (3) | 0.0041 (5) | 0.6258 (2) | 0.0381 (11) | |
C11 | 0.3228 (3) | 0.1342 (5) | 0.6382 (2) | 0.0374 (11) | |
C12 | 0.3599 (3) | 0.2202 (5) | 0.6082 (2) | 0.0474 (13) | |
C13 | 0.3920 (3) | 0.1776 (6) | 0.5605 (3) | 0.0539 (15) | |
C14 | 0.3857 (3) | 0.0526 (7) | 0.5447 (2) | 0.0518 (14) | |
C15 | 0.3478 (3) | −0.0345 (5) | 0.5765 (2) | 0.0466 (12) | |
C16 | 0.1067 (3) | 0.1293 (5) | 0.8016 (2) | 0.0397 (11) | |
C17 | 0.1221 (3) | 0.0257 (5) | 0.8431 (2) | 0.0407 (11) | |
C18 | 0.1025 (3) | 0.0177 (6) | 0.9008 (2) | 0.0509 (14) | |
C19 | 0.0642 (3) | 0.1192 (7) | 0.9203 (3) | 0.0585 (16) | |
C20 | 0.0481 (3) | 0.2240 (6) | 0.8827 (3) | 0.0580 (16) | |
C21 | 0.0682 (3) | 0.2288 (5) | 0.8251 (3) | 0.0494 (13) | |
C22 | 0.2919 (3) | 0.2302 (5) | 0.8569 (2) | 0.0437 (12) | |
C23 | 0.2681 (3) | 0.3491 (5) | 0.8300 (3) | 0.0482 (13) | |
C24 | 0.2297 (3) | 0.4386 (6) | 0.8576 (3) | 0.0610 (16) | |
C25 | 0.2111 (3) | 0.4146 (7) | 0.9136 (3) | 0.0670 (18) | |
C26 | 0.2323 (3) | 0.3008 (7) | 0.9421 (3) | 0.0618 (18) | |
C27 | 0.2722 (3) | 0.2101 (6) | 0.9146 (2) | 0.0499 (13) | |
C28 | 0.3181 (4) | −0.1862 (6) | 0.8824 (3) | 0.0669 (17) | |
H28A | 0.2684 | −0.2165 | 0.8898 | 0.080* | |
H28B | 0.3316 | −0.1064 | 0.9047 | 0.080* | |
C29 | 0.3823 (5) | −0.2848 (9) | 0.9025 (4) | 0.103 (3) | |
H29A | 0.4205 | −0.2545 | 0.9387 | 0.123* | |
H29B | 0.3600 | −0.3642 | 0.9136 | 0.123* | |
C30 | 0.4210 (5) | −0.3060 (8) | 0.8485 (3) | 0.097 (3) | |
H30A | 0.4670 | −0.2521 | 0.8519 | 0.117* | |
H30B | 0.4363 | −0.3946 | 0.8460 | 0.117* | |
C31 | 0.3600 (4) | −0.2707 (7) | 0.7949 (3) | 0.077 (2) | |
H31A | 0.3270 | −0.3437 | 0.7799 | 0.093* | |
H31B | 0.3831 | −0.2399 | 0.7612 | 0.093* | |
F11 | 0.29054 (17) | 0.1796 (3) | 0.68553 (12) | 0.0474 (7) | |
F12 | 0.3651 (2) | 0.3433 (3) | 0.62406 (16) | 0.0712 (10) | |
F13 | 0.4288 (2) | 0.2583 (4) | 0.52848 (16) | 0.0775 (11) | |
F14 | 0.4171 (2) | 0.0078 (4) | 0.49793 (17) | 0.0827 (12) | |
F15 | 0.3460 (2) | −0.1572 (3) | 0.55994 (16) | 0.0681 (10) | |
F17 | 0.16267 (16) | −0.0759 (3) | 0.82515 (13) | 0.0473 (7) | |
F18 | 0.1222 (2) | −0.0855 (4) | 0.93621 (15) | 0.0728 (10) | |
F19 | 0.0450 (2) | 0.1159 (4) | 0.97605 (16) | 0.0884 (13) | |
F20 | 0.0137 (2) | 0.3270 (4) | 0.90206 (16) | 0.0765 (11) | |
F21 | 0.05249 (19) | 0.3380 (3) | 0.79252 (15) | 0.0616 (9) | |
F23 | 0.28367 (18) | 0.3790 (3) | 0.77441 (15) | 0.0585 (8) | |
F24 | 0.2080 (2) | 0.5515 (4) | 0.8286 (2) | 0.0846 (12) | |
F25 | 0.1728 (2) | 0.5006 (4) | 0.9410 (2) | 0.1028 (16) | |
F26 | 0.21367 (19) | 0.2698 (5) | 0.99720 (15) | 0.0878 (13) | |
F27 | 0.29100 (18) | 0.0969 (4) | 0.94379 (14) | 0.0640 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sm1 | 0.02942 (13) | 0.03382 (14) | 0.03350 (14) | 0.00116 (11) | 0.00887 (9) | 0.00208 (11) |
Si1 | 0.0450 (8) | 0.0370 (7) | 0.0479 (8) | −0.0036 (6) | 0.0122 (6) | −0.0064 (6) |
Si2 | 0.0359 (7) | 0.0403 (7) | 0.0475 (8) | 0.0035 (6) | 0.0056 (6) | 0.0071 (6) |
Si3 | 0.0324 (7) | 0.0507 (8) | 0.0425 (7) | 0.0001 (6) | 0.0083 (6) | −0.0018 (6) |
O1 | 0.051 (2) | 0.049 (2) | 0.051 (2) | 0.0137 (17) | 0.0090 (17) | 0.0088 (17) |
N1 | 0.036 (2) | 0.035 (2) | 0.037 (2) | −0.0013 (17) | 0.0114 (17) | −0.0016 (17) |
N2 | 0.032 (2) | 0.042 (2) | 0.039 (2) | 0.0045 (18) | 0.0103 (17) | 0.0027 (18) |
N3 | 0.033 (2) | 0.043 (2) | 0.038 (2) | 0.0000 (18) | 0.0109 (17) | −0.0022 (18) |
C1 | 0.047 (3) | 0.047 (3) | 0.056 (3) | −0.007 (3) | 0.012 (3) | 0.001 (3) |
C2 | 0.056 (3) | 0.066 (4) | 0.047 (3) | −0.013 (3) | 0.011 (3) | −0.016 (3) |
C3 | 0.073 (4) | 0.046 (3) | 0.086 (5) | 0.004 (3) | 0.024 (4) | −0.010 (3) |
C4 | 0.068 (4) | 0.046 (3) | 0.079 (4) | 0.002 (3) | 0.009 (3) | 0.011 (3) |
C5 | 0.041 (3) | 0.062 (4) | 0.061 (4) | 0.004 (3) | 0.004 (3) | 0.001 (3) |
C6 | 0.056 (3) | 0.068 (4) | 0.047 (3) | 0.012 (3) | 0.006 (3) | 0.011 (3) |
C7 | 0.044 (3) | 0.101 (5) | 0.040 (3) | 0.010 (3) | 0.004 (2) | −0.002 (3) |
C8 | 0.040 (3) | 0.108 (5) | 0.054 (3) | 0.013 (3) | 0.010 (3) | −0.012 (4) |
C9 | 0.036 (3) | 0.062 (4) | 0.179 (8) | −0.008 (3) | 0.024 (4) | 0.020 (5) |
C10 | 0.032 (2) | 0.048 (3) | 0.033 (2) | −0.001 (2) | 0.0052 (18) | −0.002 (2) |
C11 | 0.036 (3) | 0.045 (3) | 0.032 (2) | −0.001 (2) | 0.008 (2) | 0.004 (2) |
C12 | 0.043 (3) | 0.052 (3) | 0.044 (3) | −0.007 (3) | 0.003 (2) | 0.008 (2) |
C13 | 0.043 (3) | 0.072 (4) | 0.045 (3) | −0.016 (3) | 0.005 (2) | 0.015 (3) |
C14 | 0.032 (3) | 0.092 (4) | 0.035 (3) | −0.002 (3) | 0.013 (2) | −0.003 (3) |
C15 | 0.039 (3) | 0.053 (3) | 0.049 (3) | 0.002 (2) | 0.012 (2) | −0.008 (3) |
C16 | 0.027 (2) | 0.047 (3) | 0.045 (3) | −0.004 (2) | 0.008 (2) | −0.002 (2) |
C17 | 0.029 (2) | 0.048 (3) | 0.047 (3) | −0.007 (2) | 0.010 (2) | −0.001 (2) |
C18 | 0.040 (3) | 0.070 (4) | 0.043 (3) | −0.015 (3) | 0.009 (2) | 0.005 (3) |
C19 | 0.049 (3) | 0.085 (4) | 0.046 (3) | −0.015 (3) | 0.019 (3) | −0.014 (3) |
C20 | 0.035 (3) | 0.077 (4) | 0.061 (4) | 0.003 (3) | 0.009 (3) | −0.028 (3) |
C21 | 0.032 (3) | 0.054 (3) | 0.060 (3) | −0.003 (2) | 0.005 (2) | −0.005 (3) |
C22 | 0.030 (2) | 0.056 (3) | 0.044 (3) | −0.009 (2) | 0.005 (2) | −0.008 (2) |
C23 | 0.033 (3) | 0.053 (3) | 0.058 (3) | −0.005 (2) | 0.008 (2) | −0.013 (3) |
C24 | 0.041 (3) | 0.056 (4) | 0.084 (5) | 0.002 (3) | 0.009 (3) | −0.011 (3) |
C25 | 0.040 (3) | 0.079 (5) | 0.081 (5) | 0.002 (3) | 0.012 (3) | −0.037 (4) |
C26 | 0.033 (3) | 0.109 (5) | 0.044 (3) | −0.014 (3) | 0.011 (2) | −0.028 (3) |
C27 | 0.037 (3) | 0.070 (4) | 0.040 (3) | −0.009 (3) | 0.004 (2) | −0.011 (3) |
C28 | 0.079 (4) | 0.071 (4) | 0.046 (3) | 0.016 (4) | 0.002 (3) | 0.017 (3) |
C29 | 0.087 (5) | 0.133 (7) | 0.076 (5) | 0.012 (5) | −0.008 (4) | 0.037 (5) |
C30 | 0.094 (6) | 0.109 (6) | 0.080 (5) | 0.059 (5) | 0.002 (4) | 0.005 (5) |
C31 | 0.083 (5) | 0.074 (5) | 0.073 (4) | 0.027 (4) | 0.011 (4) | 0.003 (4) |
F11 | 0.0637 (19) | 0.0403 (16) | 0.0415 (15) | −0.0056 (14) | 0.0189 (14) | −0.0020 (13) |
F12 | 0.091 (3) | 0.051 (2) | 0.073 (2) | −0.0200 (19) | 0.0223 (19) | 0.0110 (17) |
F13 | 0.064 (2) | 0.106 (3) | 0.066 (2) | −0.025 (2) | 0.0213 (18) | 0.025 (2) |
F14 | 0.066 (2) | 0.130 (4) | 0.064 (2) | −0.012 (2) | 0.0396 (19) | −0.014 (2) |
F15 | 0.067 (2) | 0.071 (2) | 0.075 (2) | −0.0028 (18) | 0.0354 (18) | −0.0224 (19) |
F17 | 0.0515 (18) | 0.0441 (16) | 0.0513 (17) | 0.0030 (14) | 0.0221 (14) | 0.0107 (14) |
F18 | 0.088 (3) | 0.082 (3) | 0.053 (2) | −0.010 (2) | 0.0253 (18) | 0.0175 (19) |
F19 | 0.090 (3) | 0.128 (4) | 0.059 (2) | −0.019 (3) | 0.042 (2) | −0.018 (2) |
F20 | 0.064 (2) | 0.094 (3) | 0.075 (2) | 0.012 (2) | 0.0208 (18) | −0.035 (2) |
F21 | 0.061 (2) | 0.0525 (19) | 0.069 (2) | 0.0169 (16) | 0.0099 (16) | −0.0093 (17) |
F23 | 0.0566 (19) | 0.0543 (19) | 0.066 (2) | 0.0047 (16) | 0.0160 (16) | 0.0056 (16) |
F24 | 0.063 (2) | 0.059 (2) | 0.129 (3) | 0.0154 (19) | 0.015 (2) | −0.013 (2) |
F25 | 0.063 (2) | 0.133 (4) | 0.112 (3) | 0.018 (2) | 0.019 (2) | −0.070 (3) |
F26 | 0.053 (2) | 0.166 (4) | 0.0476 (19) | −0.011 (2) | 0.0183 (16) | −0.032 (2) |
F27 | 0.0529 (19) | 0.095 (3) | 0.0438 (17) | −0.0060 (19) | 0.0109 (14) | 0.0067 (18) |
Sm1—N3 | 2.299 (4) | C9—H9A | 0.9600 |
Sm1—N2 | 2.338 (4) | C9—H9B | 0.9600 |
Sm1—N1 | 2.365 (4) | C9—H9C | 0.9600 |
Sm1—O1 | 2.446 (3) | C10—C11 | 1.391 (7) |
Sm1—F11 | 2.536 (3) | C10—C15 | 1.402 (7) |
Sm1—F17 | 2.555 (3) | C11—C12 | 1.361 (7) |
Sm1—Si1 | 3.4678 (15) | C11—F11 | 1.371 (5) |
Si1—N1 | 1.744 (4) | C12—F12 | 1.332 (6) |
Si1—C2 | 1.858 (5) | C12—C13 | 1.366 (8) |
Si1—C3 | 1.876 (6) | C13—F13 | 1.349 (6) |
Si1—C1 | 1.884 (5) | C13—C14 | 1.351 (8) |
Si2—N2 | 1.757 (4) | C14—F14 | 1.351 (6) |
Si2—C6 | 1.854 (6) | C14—C15 | 1.398 (8) |
Si2—C5 | 1.863 (5) | C15—F15 | 1.333 (6) |
Si2—C4 | 1.862 (6) | C16—C21 | 1.397 (7) |
Si3—N3 | 1.732 (4) | C16—C17 | 1.404 (7) |
Si3—C9 | 1.855 (6) | C17—F17 | 1.382 (6) |
Si3—C8 | 1.864 (6) | C17—C18 | 1.384 (7) |
Si3—C7 | 1.865 (5) | C18—F18 | 1.331 (6) |
O1—C31 | 1.457 (7) | C18—C19 | 1.372 (8) |
O1—C28 | 1.459 (6) | C19—F19 | 1.338 (6) |
N1—C10 | 1.382 (6) | C19—C20 | 1.363 (9) |
N2—C16 | 1.388 (6) | C20—F20 | 1.347 (6) |
N3—C22 | 1.401 (6) | C20—C21 | 1.386 (8) |
C1—H1A | 0.9600 | C21—F21 | 1.344 (6) |
C1—H1B | 0.9600 | C22—C27 | 1.398 (7) |
C1—H1C | 0.9600 | C22—C23 | 1.400 (8) |
C2—H2A | 0.9600 | C23—F23 | 1.344 (6) |
C2—H2B | 0.9600 | C23—C24 | 1.369 (8) |
C2—H2C | 0.9600 | C24—F24 | 1.356 (7) |
C3—H3A | 0.9600 | C24—C25 | 1.361 (9) |
C3—H3B | 0.9600 | C25—F25 | 1.339 (7) |
C3—H3C | 0.9600 | C25—C26 | 1.358 (9) |
C4—H4A | 0.9600 | C26—F26 | 1.359 (7) |
C4—H4B | 0.9600 | C26—C27 | 1.391 (8) |
C4—H4C | 0.9600 | C27—F27 | 1.353 (7) |
C5—H5A | 0.9600 | C28—C29 | 1.515 (9) |
C5—H5B | 0.9600 | C28—H28A | 0.9700 |
C5—H5C | 0.9600 | C28—H28B | 0.9700 |
C6—H6A | 0.9600 | C29—C30 | 1.506 (10) |
C6—H6B | 0.9600 | C29—H29A | 0.9700 |
C6—H6C | 0.9600 | C29—H29B | 0.9700 |
C7—H7A | 0.9600 | C30—C31 | 1.449 (9) |
C7—H7B | 0.9600 | C30—H30A | 0.9700 |
C7—H7C | 0.9600 | C30—H30B | 0.9700 |
C8—H8A | 0.9600 | C31—H31A | 0.9700 |
C8—H8B | 0.9600 | C31—H31B | 0.9700 |
C8—H8C | 0.9600 | ||
N3—Sm1—N2 | 97.60 (13) | H7A—C7—H7C | 109.5 |
N3—Sm1—N1 | 127.35 (13) | H7B—C7—H7C | 109.5 |
N2—Sm1—N1 | 117.50 (13) | Si3—C8—H8A | 109.5 |
N3—Sm1—O1 | 86.14 (14) | Si3—C8—H8B | 109.5 |
N2—Sm1—O1 | 137.14 (13) | H8A—C8—H8B | 109.5 |
N1—Sm1—O1 | 91.92 (13) | Si3—C8—H8C | 109.5 |
N3—Sm1—F11 | 78.32 (12) | H8A—C8—H8C | 109.5 |
N2—Sm1—F11 | 86.95 (11) | H8B—C8—H8C | 109.5 |
N1—Sm1—F11 | 66.67 (11) | Si3—C9—H9A | 109.5 |
O1—Sm1—F11 | 135.12 (11) | Si3—C9—H9B | 109.5 |
N3—Sm1—F17 | 97.73 (11) | H9A—C9—H9B | 109.5 |
N2—Sm1—F17 | 67.23 (11) | Si3—C9—H9C | 109.5 |
N1—Sm1—F17 | 130.69 (12) | H9A—C9—H9C | 109.5 |
O1—Sm1—F17 | 69.96 (11) | H9B—C9—H9C | 109.5 |
F11—Sm1—F17 | 153.29 (9) | N1—C10—C11 | 120.4 (4) |
N3—Sm1—Si1 | 150.04 (10) | N1—C10—C15 | 126.9 (5) |
N2—Sm1—Si1 | 110.00 (10) | C11—C10—C15 | 112.7 (4) |
N1—Sm1—Si1 | 27.28 (9) | C12—C11—F11 | 117.1 (4) |
O1—Sm1—Si1 | 81.54 (9) | C12—C11—C10 | 126.7 (5) |
F11—Sm1—Si1 | 91.40 (7) | F11—C11—C10 | 116.2 (4) |
F17—Sm1—Si1 | 103.43 (7) | F12—C12—C13 | 120.0 (5) |
N1—Si1—C2 | 113.2 (2) | F12—C12—C11 | 121.7 (5) |
N1—Si1—C3 | 116.8 (2) | C13—C12—C11 | 118.3 (5) |
C2—Si1—C3 | 107.5 (3) | F13—C13—C14 | 119.6 (5) |
N1—Si1—C1 | 102.8 (2) | F13—C13—C12 | 121.1 (6) |
C2—Si1—C1 | 108.8 (2) | C14—C13—C12 | 119.2 (5) |
C3—Si1—C1 | 107.4 (3) | F14—C14—C13 | 120.4 (5) |
N1—Si1—Sm1 | 38.44 (12) | F14—C14—C15 | 117.9 (6) |
C2—Si1—Sm1 | 127.6 (2) | C13—C14—C15 | 121.6 (5) |
C3—Si1—Sm1 | 124.5 (2) | F15—C15—C14 | 118.6 (5) |
C1—Si1—Sm1 | 64.50 (17) | F15—C15—C10 | 119.9 (5) |
N2—Si2—C6 | 106.8 (2) | C14—C15—C10 | 121.5 (5) |
N2—Si2—C5 | 110.0 (2) | N2—C16—C21 | 127.9 (5) |
C6—Si2—C5 | 107.0 (3) | N2—C16—C17 | 119.9 (4) |
N2—Si2—C4 | 114.6 (2) | C21—C16—C17 | 112.1 (4) |
C6—Si2—C4 | 106.4 (3) | F17—C17—C18 | 117.4 (5) |
C5—Si2—C4 | 111.6 (3) | F17—C17—C16 | 116.6 (4) |
N3—Si3—C9 | 111.3 (2) | C18—C17—C16 | 126.0 (5) |
N3—Si3—C8 | 107.6 (2) | F18—C18—C19 | 121.8 (5) |
C9—Si3—C8 | 109.3 (3) | F18—C18—C17 | 119.9 (5) |
N3—Si3—C7 | 113.8 (2) | C19—C18—C17 | 118.3 (5) |
C9—Si3—C7 | 107.0 (3) | F19—C19—C20 | 120.9 (6) |
C8—Si3—C7 | 107.7 (3) | F19—C19—C18 | 120.1 (6) |
C31—O1—C28 | 108.9 (4) | C20—C19—C18 | 119.0 (5) |
C31—O1—Sm1 | 127.3 (3) | F20—C20—C19 | 120.1 (5) |
C28—O1—Sm1 | 123.6 (3) | F20—C20—C21 | 118.6 (6) |
C10—N1—Si1 | 125.2 (3) | C19—C20—C21 | 121.3 (5) |
C10—N1—Sm1 | 118.9 (3) | F21—C21—C20 | 116.9 (5) |
Si1—N1—Sm1 | 114.28 (18) | F21—C21—C16 | 119.7 (5) |
C16—N2—Si2 | 120.6 (3) | C20—C21—C16 | 123.3 (5) |
C16—N2—Sm1 | 113.0 (3) | C27—C22—C23 | 113.9 (5) |
Si2—N2—Sm1 | 126.32 (19) | C27—C22—N3 | 123.4 (5) |
C22—N3—Si3 | 117.4 (3) | C23—C22—N3 | 122.6 (5) |
C22—N3—Sm1 | 116.8 (3) | F23—C23—C24 | 117.3 (5) |
Si3—N3—Sm1 | 125.0 (2) | F23—C23—C22 | 119.2 (5) |
Si1—C1—H1A | 109.5 | C24—C23—C22 | 123.4 (6) |
Si1—C1—H1B | 109.5 | F24—C24—C25 | 119.2 (6) |
H1A—C1—H1B | 109.5 | F24—C24—C23 | 120.1 (6) |
Si1—C1—H1C | 109.5 | C25—C24—C23 | 120.7 (6) |
H1A—C1—H1C | 109.5 | F25—C25—C26 | 119.7 (7) |
H1B—C1—H1C | 109.5 | F25—C25—C24 | 121.5 (7) |
Si1—C2—H2A | 109.5 | C26—C25—C24 | 118.8 (6) |
Si1—C2—H2B | 109.5 | C25—C26—F26 | 121.6 (6) |
H2A—C2—H2B | 109.5 | C25—C26—C27 | 120.7 (6) |
Si1—C2—H2C | 109.5 | F26—C26—C27 | 117.6 (7) |
H2A—C2—H2C | 109.5 | F27—C27—C26 | 119.0 (5) |
H2B—C2—H2C | 109.5 | F27—C27—C22 | 118.6 (5) |
Si1—C3—H3A | 109.5 | C26—C27—C22 | 122.4 (6) |
Si1—C3—H3B | 109.5 | O1—C28—C29 | 103.9 (5) |
H3A—C3—H3B | 109.5 | O1—C28—H28A | 111.0 |
Si1—C3—H3C | 109.5 | C29—C28—H28A | 111.0 |
H3A—C3—H3C | 109.5 | O1—C28—H28B | 111.0 |
H3B—C3—H3C | 109.5 | C29—C28—H28B | 111.0 |
Si2—C4—H4A | 109.5 | H28A—C28—H28B | 109.0 |
Si2—C4—H4B | 109.5 | C30—C29—C28 | 107.6 (6) |
H4A—C4—H4B | 109.5 | C30—C29—H29A | 110.2 |
Si2—C4—H4C | 109.5 | C28—C29—H29A | 110.2 |
H4A—C4—H4C | 109.5 | C30—C29—H29B | 110.2 |
H4B—C4—H4C | 109.5 | C28—C29—H29B | 110.2 |
Si2—C5—H5A | 109.5 | H29A—C29—H29B | 108.5 |
Si2—C5—H5B | 109.5 | C31—C30—C29 | 103.0 (6) |
H5A—C5—H5B | 109.5 | C31—C30—H30A | 111.2 |
Si2—C5—H5C | 109.5 | C29—C30—H30A | 111.2 |
H5A—C5—H5C | 109.5 | C31—C30—H30B | 111.2 |
H5B—C5—H5C | 109.5 | C29—C30—H30B | 111.2 |
Si2—C6—H6A | 109.5 | H30A—C30—H30B | 109.1 |
Si2—C6—H6B | 109.5 | C30—C31—O1 | 106.7 (6) |
H6A—C6—H6B | 109.5 | C30—C31—H31A | 110.4 |
Si2—C6—H6C | 109.5 | O1—C31—H31A | 110.4 |
H6A—C6—H6C | 109.5 | C30—C31—H31B | 110.4 |
H6B—C6—H6C | 109.5 | O1—C31—H31B | 110.4 |
Si3—C7—H7A | 109.5 | H31A—C31—H31B | 108.6 |
Si3—C7—H7B | 109.5 | C11—F11—Sm1 | 115.3 (3) |
H7A—C7—H7B | 109.5 | C17—F17—Sm1 | 108.0 (2) |
Si3—C7—H7C | 109.5 |
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