Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804019592/hg6086sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804019592/hg6086IIsup2.hkl |
CCDC reference: 251617
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX6a (McArdle, 1995); software used to prepare material for publication: SHELXL97.
[Al(C29H30Cl4O5P)3]·0.25C6H6 | Dx = 1.313 Mg m−3 |
Mr = 1940.41 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 8257 reflections |
Hall symbol: -R 3 | θ = 2.7–20.4° |
a = 22.4062 (7) Å | µ = 0.46 mm−1 |
c = 33.854 (2) Å | T = 298 K |
V = 14718.8 (12) Å3 | Cube, colourless |
Z = 6 | 0.55 × 0.50 × 0.50 mm |
F(000) = 6027 |
Siemens SMART CCD area-detector diffractometer | 5770 independent reflections |
Radiation source: fine-focus sealed tube | 4591 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −26→26 |
Tmin = 0.633, Tmax = 0.831 | k = −26→26 |
28911 measured reflections | l = −26→40 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.142 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.09P)2 + 7.037P] where P = (Fo2 + 2Fc2)/3 |
5770 reflections | (Δ/σ)max < 0.001 |
365 parameters | Δρmax = 0.61 e Å−3 |
2 restraints | Δρmin = −0.30 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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Al1 | 0.6667 | 0.3333 | 0.02082 (3) | 0.0274 (2) | |
Cl1 | 0.58283 (4) | 0.19848 (5) | −0.08099 (2) | 0.0735 (3) | |
Cl2 | 0.47533 (6) | 0.19316 (7) | −0.14047 (3) | 0.1003 (4) | |
Cl3 | 0.38766 (5) | 0.26220 (5) | −0.11918 (3) | 0.0815 (3) | |
Cl4 | 0.40678 (4) | 0.33054 (4) | −0.03574 (2) | 0.0599 (2) | |
P1 | 0.52966 (3) | 0.30862 (3) | 0.053209 (17) | 0.03336 (17) | |
O1 | 0.48796 (8) | 0.22857 (8) | 0.05706 (5) | 0.0447 (4) | |
O2 | 0.49675 (8) | 0.33638 (9) | 0.08292 (5) | 0.0407 (4) | |
O3 | 0.50720 (8) | 0.32560 (8) | 0.01313 (5) | 0.0387 (4) | |
O4 | 0.58999 (7) | 0.26903 (8) | −0.00650 (4) | 0.0346 (4) | |
O5 | 0.60504 (7) | 0.34225 (8) | 0.05772 (4) | 0.0333 (4) | |
C1 | 0.44366 (14) | 0.18954 (13) | 0.08864 (9) | 0.0518 (7) | |
C2 | 0.37717 (15) | 0.13459 (14) | 0.07889 (11) | 0.0666 (9) | |
C3 | 0.34052 (18) | 0.09436 (18) | 0.11106 (14) | 0.0844 (12) | |
H3 | 0.2968 | 0.0570 | 0.1063 | 0.101* | |
C4 | 0.3639 (2) | 0.1055 (2) | 0.14921 (15) | 0.0879 (13) | |
C5 | 0.42776 (19) | 0.16154 (19) | 0.15693 (11) | 0.0761 (10) | |
H5 | 0.4436 | 0.1711 | 0.1828 | 0.091* | |
C6 | 0.46924 (15) | 0.20426 (15) | 0.12658 (10) | 0.0574 (8) | |
C7 | 0.53892 (15) | 0.26440 (16) | 0.13705 (9) | 0.0587 (8) | |
H7A | 0.5571 | 0.2514 | 0.1594 | 0.070* | |
H7B | 0.5699 | 0.2734 | 0.1150 | 0.070* | |
C8 | 0.53922 (14) | 0.32994 (16) | 0.14715 (8) | 0.0528 (7) | |
C9 | 0.52281 (12) | 0.36663 (14) | 0.12027 (7) | 0.0431 (6) | |
C10 | 0.52512 (14) | 0.42884 (14) | 0.12798 (8) | 0.0493 (6) | |
C11 | 0.54368 (17) | 0.45292 (18) | 0.16662 (9) | 0.0684 (9) | |
H11 | 0.5463 | 0.4944 | 0.1735 | 0.082* | |
C12 | 0.55829 (19) | 0.4181 (2) | 0.19509 (9) | 0.0755 (10) | |
C13 | 0.55689 (17) | 0.3578 (2) | 0.18522 (9) | 0.0703 (9) | |
H13 | 0.5680 | 0.3351 | 0.2043 | 0.084* | |
C14 | 0.3209 (3) | 0.0579 (3) | 0.18231 (16) | 0.130 (2) | |
H14A | 0.3104 | 0.0832 | 0.2012 | 0.195* | |
H14B | 0.3462 | 0.0391 | 0.1950 | 0.195* | |
H14C | 0.2788 | 0.0210 | 0.1717 | 0.195* | |
C15 | 0.5777 (3) | 0.4478 (3) | 0.23708 (11) | 0.1252 (19) | |
H15A | 0.5477 | 0.4647 | 0.2452 | 0.188* | |
H15B | 0.6245 | 0.4849 | 0.2373 | 0.188* | |
H15C | 0.5728 | 0.4123 | 0.2549 | 0.188* | |
C16 | 0.34609 (16) | 0.12223 (16) | 0.03721 (13) | 0.0734 (10) | |
C17 | 0.33743 (18) | 0.18299 (18) | 0.02580 (13) | 0.0888 (12) | |
H17A | 0.3813 | 0.2247 | 0.0272 | 0.133* | |
H17B | 0.3058 | 0.1860 | 0.0437 | 0.133* | |
H17C | 0.3198 | 0.1767 | −0.0006 | 0.133* | |
C18 | 0.38978 (19) | 0.11096 (17) | 0.00687 (12) | 0.0813 (11) | |
H18A | 0.3701 | 0.1063 | −0.0189 | 0.122* | |
H18B | 0.3909 | 0.0698 | 0.0133 | 0.122* | |
H18C | 0.4358 | 0.1497 | 0.0071 | 0.122* | |
C19 | 0.27360 (18) | 0.05800 (19) | 0.03606 (16) | 0.1098 (16) | |
H19A | 0.2557 | 0.0512 | 0.0097 | 0.165* | |
H19B | 0.2437 | 0.0644 | 0.0537 | 0.165* | |
H19C | 0.2763 | 0.0183 | 0.0441 | 0.165* | |
C20 | 0.50849 (15) | 0.46843 (14) | 0.09732 (8) | 0.0520 (7) | |
C21 | 0.43355 (17) | 0.42648 (18) | 0.08421 (12) | 0.0766 (10) | |
H21A | 0.4243 | 0.3821 | 0.0751 | 0.115* | |
H21B | 0.4253 | 0.4501 | 0.0632 | 0.115* | |
H21C | 0.4039 | 0.4208 | 0.1061 | 0.115* | |
C22 | 0.5188 (2) | 0.53596 (19) | 0.11392 (11) | 0.0874 (12) | |
H22A | 0.4874 | 0.5266 | 0.1354 | 0.131* | |
H22B | 0.5103 | 0.5606 | 0.0936 | 0.131* | |
H22C | 0.5653 | 0.5633 | 0.1232 | 0.131* | |
C23 | 0.55677 (18) | 0.48616 (16) | 0.06171 (9) | 0.0653 (8) | |
H23A | 0.6038 | 0.5118 | 0.0705 | 0.098* | |
H23B | 0.5480 | 0.5134 | 0.0433 | 0.098* | |
H23C | 0.5488 | 0.4444 | 0.0491 | 0.098* | |
C24 | 0.50208 (11) | 0.29390 (11) | −0.02323 (7) | 0.0360 (5) | |
C25 | 0.54506 (11) | 0.26732 (11) | −0.03194 (7) | 0.0338 (5) | |
C26 | 0.53388 (13) | 0.23530 (13) | −0.06877 (8) | 0.0448 (6) | |
C27 | 0.48599 (15) | 0.23320 (15) | −0.09556 (8) | 0.0547 (7) | |
C28 | 0.44644 (14) | 0.26289 (15) | −0.08604 (8) | 0.0518 (7) | |
C29 | 0.45466 (12) | 0.29305 (13) | −0.04938 (8) | 0.0430 (6) | |
C1S | 0.6218 (15) | 0.3535 (19) | 0.3346 (7) | 0.215 (8)* | 0.50 |
H1S | 0.5898 | 0.3678 | 0.3384 | 0.258* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.0262 (3) | 0.0262 (3) | 0.0297 (6) | 0.01308 (17) | 0.000 | 0.000 |
Cl1 | 0.0764 (5) | 0.1012 (7) | 0.0717 (5) | 0.0659 (5) | −0.0310 (4) | −0.0463 (5) |
Cl2 | 0.1177 (8) | 0.1487 (10) | 0.0720 (6) | 0.0947 (8) | −0.0561 (6) | −0.0626 (6) |
Cl3 | 0.0811 (6) | 0.1019 (7) | 0.0794 (6) | 0.0593 (5) | −0.0460 (5) | −0.0241 (5) |
Cl4 | 0.0568 (4) | 0.0676 (5) | 0.0740 (5) | 0.0450 (4) | −0.0078 (3) | 0.0017 (4) |
P1 | 0.0309 (3) | 0.0329 (3) | 0.0388 (3) | 0.0179 (3) | 0.0061 (2) | 0.0047 (2) |
O1 | 0.0391 (9) | 0.0345 (9) | 0.0585 (11) | 0.0170 (8) | 0.0130 (8) | 0.0092 (8) |
O2 | 0.0390 (9) | 0.0464 (10) | 0.0425 (9) | 0.0258 (8) | 0.0085 (7) | 0.0047 (7) |
O3 | 0.0426 (9) | 0.0408 (9) | 0.0408 (9) | 0.0269 (8) | −0.0014 (7) | −0.0009 (7) |
O4 | 0.0314 (8) | 0.0326 (8) | 0.0396 (9) | 0.0157 (7) | −0.0078 (7) | −0.0046 (6) |
O5 | 0.0325 (8) | 0.0358 (8) | 0.0329 (8) | 0.0180 (7) | 0.0045 (6) | 0.0004 (6) |
C1 | 0.0442 (15) | 0.0407 (14) | 0.077 (2) | 0.0258 (12) | 0.0236 (14) | 0.0244 (13) |
C2 | 0.0419 (15) | 0.0378 (15) | 0.121 (3) | 0.0209 (13) | 0.0270 (17) | 0.0277 (16) |
C3 | 0.0529 (19) | 0.057 (2) | 0.143 (4) | 0.0277 (16) | 0.038 (2) | 0.045 (2) |
C4 | 0.072 (2) | 0.073 (2) | 0.129 (4) | 0.044 (2) | 0.056 (2) | 0.058 (2) |
C5 | 0.081 (2) | 0.081 (2) | 0.084 (2) | 0.054 (2) | 0.0389 (19) | 0.0428 (19) |
C6 | 0.0550 (17) | 0.0533 (17) | 0.074 (2) | 0.0344 (15) | 0.0248 (15) | 0.0276 (15) |
C7 | 0.0621 (18) | 0.079 (2) | 0.0517 (16) | 0.0474 (17) | 0.0153 (13) | 0.0283 (15) |
C8 | 0.0480 (15) | 0.0696 (19) | 0.0441 (15) | 0.0319 (14) | 0.0157 (12) | 0.0145 (13) |
C9 | 0.0393 (13) | 0.0555 (16) | 0.0359 (13) | 0.0247 (12) | 0.0120 (10) | 0.0058 (11) |
C10 | 0.0444 (15) | 0.0559 (16) | 0.0473 (15) | 0.0249 (13) | 0.0164 (12) | 0.0019 (12) |
C11 | 0.068 (2) | 0.072 (2) | 0.0573 (19) | 0.0289 (17) | 0.0156 (15) | −0.0115 (16) |
C12 | 0.073 (2) | 0.106 (3) | 0.0447 (18) | 0.043 (2) | 0.0043 (15) | −0.0080 (18) |
C13 | 0.066 (2) | 0.102 (3) | 0.0433 (16) | 0.042 (2) | 0.0081 (14) | 0.0127 (17) |
C14 | 0.114 (4) | 0.117 (4) | 0.164 (5) | 0.062 (3) | 0.089 (3) | 0.095 (4) |
C15 | 0.150 (5) | 0.160 (5) | 0.054 (2) | 0.069 (4) | −0.011 (2) | −0.025 (3) |
C16 | 0.0413 (16) | 0.0452 (17) | 0.124 (3) | 0.0147 (14) | −0.0069 (18) | 0.0115 (18) |
C17 | 0.0540 (19) | 0.057 (2) | 0.148 (4) | 0.0222 (17) | −0.009 (2) | 0.021 (2) |
C18 | 0.067 (2) | 0.0508 (19) | 0.108 (3) | 0.0157 (17) | −0.014 (2) | 0.0024 (19) |
C19 | 0.052 (2) | 0.058 (2) | 0.194 (5) | 0.0083 (18) | 0.000 (3) | 0.020 (3) |
C20 | 0.0567 (16) | 0.0462 (15) | 0.0581 (17) | 0.0295 (13) | 0.0192 (13) | 0.0040 (12) |
C21 | 0.062 (2) | 0.073 (2) | 0.106 (3) | 0.0417 (18) | 0.0079 (19) | 0.022 (2) |
C22 | 0.131 (3) | 0.065 (2) | 0.082 (2) | 0.061 (2) | 0.028 (2) | 0.0007 (18) |
C23 | 0.080 (2) | 0.0604 (18) | 0.0627 (18) | 0.0409 (17) | 0.0254 (16) | 0.0145 (15) |
C24 | 0.0339 (12) | 0.0300 (11) | 0.0410 (13) | 0.0137 (10) | −0.0024 (10) | −0.0008 (10) |
C25 | 0.0281 (11) | 0.0294 (11) | 0.0394 (13) | 0.0109 (9) | −0.0043 (9) | −0.0017 (9) |
C26 | 0.0409 (13) | 0.0455 (14) | 0.0508 (15) | 0.0238 (12) | −0.0096 (11) | −0.0103 (11) |
C27 | 0.0538 (16) | 0.0631 (18) | 0.0494 (16) | 0.0309 (14) | −0.0206 (13) | −0.0187 (13) |
C28 | 0.0458 (15) | 0.0557 (16) | 0.0555 (16) | 0.0266 (13) | −0.0204 (12) | −0.0085 (13) |
C29 | 0.0344 (13) | 0.0391 (13) | 0.0565 (15) | 0.0191 (11) | −0.0055 (11) | 0.0012 (11) |
Al1—O4i | 1.8461 (15) | C13—H13 | 0.9300 |
Al1—O4 | 1.8461 (15) | C14—H14A | 0.9600 |
Al1—O4ii | 1.8461 (15) | C14—H14B | 0.9600 |
Al1—O5i | 1.9448 (15) | C14—H14C | 0.9600 |
Al1—O5ii | 1.9448 (16) | C15—H15A | 0.9600 |
Al1—O5 | 1.9448 (15) | C15—H15B | 0.9600 |
Cl1—C26 | 1.720 (3) | C15—H15C | 0.9600 |
Cl2—C27 | 1.720 (3) | C16—C17 | 1.518 (5) |
Cl3—C28 | 1.724 (3) | C16—C18 | 1.524 (5) |
Cl4—C29 | 1.724 (2) | C16—C19 | 1.540 (4) |
P1—O5 | 1.4736 (16) | C17—H17A | 0.9600 |
P1—O2 | 1.5494 (16) | C17—H17B | 0.9600 |
P1—O3 | 1.5588 (16) | C17—H17C | 0.9600 |
P1—O1 | 1.5594 (17) | C18—H18A | 0.9600 |
O1—C1 | 1.423 (3) | C18—H18B | 0.9600 |
O2—C9 | 1.415 (3) | C18—H18C | 0.9600 |
O3—C24 | 1.397 (3) | C19—H19A | 0.9600 |
O4—C25 | 1.311 (3) | C19—H19B | 0.9600 |
C1—C6 | 1.377 (4) | C19—H19C | 0.9600 |
C1—C2 | 1.418 (4) | C20—C22 | 1.519 (4) |
C2—C3 | 1.390 (5) | C20—C21 | 1.524 (4) |
C2—C16 | 1.536 (5) | C20—C23 | 1.533 (4) |
C3—C4 | 1.369 (6) | C21—H21A | 0.9600 |
C3—H3 | 0.9300 | C21—H21B | 0.9600 |
C4—C5 | 1.377 (6) | C21—H21C | 0.9600 |
C4—C14 | 1.515 (5) | C22—H22A | 0.9600 |
C5—C6 | 1.395 (4) | C22—H22B | 0.9600 |
C5—H5 | 0.9300 | C22—H22C | 0.9600 |
C6—C7 | 1.509 (4) | C23—H23A | 0.9600 |
C7—C8 | 1.504 (4) | C23—H23B | 0.9600 |
C7—H7A | 0.9700 | C23—H23C | 0.9600 |
C7—H7B | 0.9700 | C24—C29 | 1.376 (3) |
C8—C9 | 1.393 (4) | C24—C25 | 1.394 (3) |
C8—C13 | 1.400 (4) | C25—C26 | 1.397 (3) |
C9—C10 | 1.393 (4) | C26—C27 | 1.388 (4) |
C10—C11 | 1.397 (4) | C27—C28 | 1.386 (4) |
C10—C20 | 1.528 (4) | C28—C29 | 1.381 (4) |
C11—C12 | 1.378 (5) | C1S—C1Siii | 1.294 (4) |
C11—H11 | 0.9300 | C1S—C1Siv | 1.294 (4) |
C12—C13 | 1.376 (5) | C1S—H1S | 0.9300 |
C12—C15 | 1.537 (5) | ||
O4i—Al1—O4 | 97.09 (7) | C12—C15—H15B | 109.5 |
O4i—Al1—O4ii | 97.09 (7) | H15A—C15—H15B | 109.5 |
O4—Al1—O4ii | 97.09 (7) | C12—C15—H15C | 109.5 |
O4i—Al1—O5i | 88.31 (6) | H15A—C15—H15C | 109.5 |
O4—Al1—O5i | 90.58 (6) | H15B—C15—H15C | 109.5 |
O4ii—Al1—O5i | 169.98 (8) | C17—C16—C18 | 111.0 (3) |
O4i—Al1—O5ii | 90.58 (6) | C17—C16—C2 | 108.8 (3) |
O4—Al1—O5ii | 169.98 (8) | C18—C16—C2 | 112.2 (3) |
O4ii—Al1—O5ii | 88.31 (6) | C17—C16—C19 | 106.5 (3) |
O5i—Al1—O5ii | 83.18 (7) | C18—C16—C19 | 107.0 (3) |
O4i—Al1—O5 | 169.98 (8) | C2—C16—C19 | 111.3 (3) |
O4—Al1—O5 | 88.31 (6) | C16—C17—H17A | 109.5 |
O4ii—Al1—O5 | 90.58 (6) | C16—C17—H17B | 109.5 |
O5i—Al1—O5 | 83.18 (7) | H17A—C17—H17B | 109.5 |
O5ii—Al1—O5 | 83.18 (7) | C16—C17—H17C | 109.5 |
O5—P1—O2 | 112.42 (9) | H17A—C17—H17C | 109.5 |
O5—P1—O3 | 113.13 (9) | H17B—C17—H17C | 109.5 |
O2—P1—O3 | 100.98 (9) | C16—C18—H18A | 109.5 |
O5—P1—O1 | 116.99 (9) | C16—C18—H18B | 109.5 |
O2—P1—O1 | 106.01 (9) | H18A—C18—H18B | 109.5 |
O3—P1—O1 | 105.83 (9) | C16—C18—H18C | 109.5 |
C1—O1—P1 | 127.04 (17) | H18A—C18—H18C | 109.5 |
C9—O2—P1 | 127.37 (15) | H18B—C18—H18C | 109.5 |
C24—O3—P1 | 126.68 (14) | C16—C19—H19A | 109.5 |
C25—O4—Al1 | 138.90 (14) | C16—C19—H19B | 109.5 |
P1—O5—Al1 | 124.90 (9) | H19A—C19—H19B | 109.5 |
C6—C1—C2 | 123.8 (3) | C16—C19—H19C | 109.5 |
C6—C1—O1 | 118.3 (2) | H19A—C19—H19C | 109.5 |
C2—C1—O1 | 117.8 (3) | H19B—C19—H19C | 109.5 |
C3—C2—C1 | 113.9 (4) | C22—C20—C21 | 107.1 (3) |
C3—C2—C16 | 122.3 (3) | C22—C20—C10 | 111.5 (3) |
C1—C2—C16 | 123.7 (3) | C21—C20—C10 | 110.7 (2) |
C4—C3—C2 | 124.9 (4) | C22—C20—C23 | 107.2 (3) |
C4—C3—H3 | 117.5 | C21—C20—C23 | 110.4 (3) |
C2—C3—H3 | 117.5 | C10—C20—C23 | 109.8 (2) |
C3—C4—C5 | 118.3 (3) | C20—C21—H21A | 109.5 |
C3—C4—C14 | 121.3 (4) | C20—C21—H21B | 109.5 |
C5—C4—C14 | 120.4 (5) | H21A—C21—H21B | 109.5 |
C4—C5—C6 | 121.2 (4) | C20—C21—H21C | 109.5 |
C4—C5—H5 | 119.4 | H21A—C21—H21C | 109.5 |
C6—C5—H5 | 119.4 | H21B—C21—H21C | 109.5 |
C1—C6—C5 | 117.9 (3) | C20—C22—H22A | 109.5 |
C1—C6—C7 | 123.6 (2) | C20—C22—H22B | 109.5 |
C5—C6—C7 | 118.5 (3) | H22A—C22—H22B | 109.5 |
C8—C7—C6 | 115.0 (2) | C20—C22—H22C | 109.5 |
C8—C7—H7A | 108.5 | H22A—C22—H22C | 109.5 |
C6—C7—H7A | 108.5 | H22B—C22—H22C | 109.5 |
C8—C7—H7B | 108.5 | C20—C23—H23A | 109.5 |
C6—C7—H7B | 108.5 | C20—C23—H23B | 109.5 |
H7A—C7—H7B | 107.5 | H23A—C23—H23B | 109.5 |
C9—C8—C13 | 115.9 (3) | C20—C23—H23C | 109.5 |
C9—C8—C7 | 123.6 (3) | H23A—C23—H23C | 109.5 |
C13—C8—C7 | 120.5 (3) | H23B—C23—H23C | 109.5 |
C10—C9—C8 | 125.4 (3) | C29—C24—C25 | 123.5 (2) |
C10—C9—O2 | 116.5 (2) | C29—C24—O3 | 116.1 (2) |
C8—C9—O2 | 117.9 (2) | C25—C24—O3 | 120.33 (19) |
C9—C10—C11 | 114.6 (3) | O4—C25—C24 | 122.2 (2) |
C9—C10—C20 | 123.8 (2) | O4—C25—C26 | 122.6 (2) |
C11—C10—C20 | 121.6 (3) | C24—C25—C26 | 115.0 (2) |
C12—C11—C10 | 123.0 (3) | C27—C26—C25 | 122.5 (2) |
C12—C11—H11 | 118.5 | C27—C26—Cl1 | 119.6 (2) |
C10—C11—H11 | 118.5 | C25—C26—Cl1 | 117.87 (18) |
C13—C12—C11 | 119.4 (3) | C28—C27—C26 | 120.1 (2) |
C13—C12—C15 | 120.8 (4) | C28—C27—Cl2 | 120.0 (2) |
C11—C12—C15 | 119.8 (4) | C26—C27—Cl2 | 119.9 (2) |
C12—C13—C8 | 121.6 (3) | C29—C28—C27 | 118.9 (2) |
C12—C13—H13 | 119.2 | C29—C28—Cl3 | 120.2 (2) |
C8—C13—H13 | 119.2 | C27—C28—Cl3 | 120.9 (2) |
C4—C14—H14A | 109.5 | C24—C29—C28 | 119.9 (2) |
C4—C14—H14B | 109.5 | C24—C29—Cl4 | 119.0 (2) |
H14A—C14—H14B | 109.5 | C28—C29—Cl4 | 121.06 (19) |
C4—C14—H14C | 109.5 | C1Siii—C1S—C1Siv | 119.5 (5) |
H14A—C14—H14C | 109.5 | C1Siii—C1S—H1S | 120.2 |
H14B—C14—H14C | 109.5 | C1Siv—C1S—H1S | 120.2 |
C12—C15—H15A | 109.5 |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) y+1/3, −x+y+2/3, −z+2/3; (iv) x−y+1/3, x−1/3, −z+2/3. |